# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound1a-150K

_audit_creation_date             2013-09-13T18:39:34-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;(1-{6-[1,1-di(pyridin-2-yl)ethyl]pyridin-2-yl}-N,N-
dimethylmethanamine)bis(thiocyanato-\kN)iron(II)--chloroform(1/1)
;
_chemical_formula_iupac          '[Fe (C20 H22 N4) (N C S)2].C H Cl3'
_chemical_formula_moiety         'C22 H22 Fe N6 S2, C H Cl3'
_chemical_formula_sum            'C23 H23 Cl3 Fe N6 S2'
_chemical_formula_weight         609.79

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.1455(13)
_cell_length_b                   9.2914(8)
_cell_length_c                   16.4133(13)
_cell_angle_alpha                90
_cell_angle_beta                 104.815(7)
_cell_angle_gamma                90
_cell_volume                     2675.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(10)
_cell_measurement_reflns_used    1497
_cell_measurement_theta_min      3.3436
_cell_measurement_theta_max      32.5384

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248
_exptl_crystal_recrystallization_method 
'precipitation: chloroform, diethyl ether, vapour diffusion, r. t., 3 d'

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.86223
_exptl_absorpt_correction_T_max  1

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_ambient_temperature      150.0(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent Sapphire 3'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_standards_number         0
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_unetI/netI     0.1276
_diffrn_reflns_number            10615
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.35
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_full        26
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             5248
_reflns_number_gt                3319
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
 The chloroform moiety exhibits disorder. It has been modeled in two discrete
 positions using SAME, DELU and tight ISOR restraints. The s.o.f. refined to
 48(3) % and 52(3) %, respectively.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0273P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5248
_refine_ls_number_parameters     356
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.1293
_refine_ls_R_factor_gt           0.0748
_refine_ls_wR_factor_ref         0.1364
_refine_ls_wR_factor_gt          0.1146
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.09
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.089


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.3427(3) -0.0842(6) 0.1700(3) 0.0279(14) Uani 1 1 d . . .
C12 C 0.4030(3) -0.1300(7) 0.1415(3) 0.0352(15) Uani 1 1 d . . .
H12 H 0.4445 -0.1799 0.1774 0.042 Uiso 1 1 calc R . .
C13 C 0.4018(3) -0.1011(7) 0.0578(4) 0.0378(15) Uani 1 1 d . . .
H13 H 0.4444 -0.1256 0.037 0.045 Uiso 1 1 calc R . .
C14 C 0.3386(3) -0.0368(6) 0.0049(3) 0.0309(14) Uani 1 1 d . . .
H14 H 0.3362 -0.0215 -0.0529 0.037 Uiso 1 1 calc R . .
C15 C 0.2787(3) 0.0047(6) 0.0378(3) 0.0232(12) Uani 1 1 d . . .
C16 C 0.2013(3) 0.0603(6) -0.0145(3) 0.0200(12) Uani 1 1 d . . .
C17 C 0.2010(3) 0.0679(6) -0.1080(3) 0.0292(14) Uani 1 1 d . . .
H17A H 0.1513 0.1026 -0.1409 0.044 Uiso 1 1 calc R . .
H17B H 0.2106 -0.0281 -0.1278 0.044 Uiso 1 1 calc R . .
H17C H 0.2409 0.1342 -0.1151 0.044 Uiso 1 1 calc R . .
C21 C 0.0744(3) -0.1417(6) 0.0900(3) 0.0236(12) Uani 1 1 d . . .
H21 H 0.0674 -0.1492 0.1453 0.028 Uiso 1 1 calc R . .
C22 C 0.0247(3) -0.2161(6) 0.0264(3) 0.0258(13) Uani 1 1 d . . .
H22 H -0.0146 -0.2744 0.0374 0.031 Uiso 1 1 calc R . .
C23 C 0.0344(3) -0.2026(6) -0.0542(3) 0.0272(13) Uani 1 1 d . . .
H23 H 0.0018 -0.2532 -0.0997 0.033 Uiso 1 1 calc R . .
C24 C 0.0911(3) -0.1162(6) -0.0682(3) 0.0259(13) Uani 1 1 d . . .
H24 H 0.0974 -0.1056 -0.1236 0.031 Uiso 1 1 calc R . .
C25 C 0.1395(3) -0.0443(6) -0.0015(3) 0.0199(11) Uani 1 1 d . . .
C31 C 0.1554(3) 0.3387(6) 0.1263(3) 0.0271(13) Uani 1 1 d . . .
H31 H 0.1513 0.3421 0.1828 0.033 Uiso 1 1 calc R . .
C32 C 0.1388(3) 0.4612(6) 0.0780(3) 0.0280(13) Uani 1 1 d . . .
H32 H 0.1234 0.5468 0.1007 0.034 Uiso 1 1 calc R . .
C33 C 0.1450(3) 0.4567(6) -0.0038(3) 0.0299(13) Uani 1 1 d . . .
H33 H 0.1337 0.5395 -0.0388 0.036 Uiso 1 1 calc R . .
C34 C 0.1679(3) 0.3299(6) -0.0345(3) 0.0251(13) Uani 1 1 d . . .
H34 H 0.1734 0.326 -0.0905 0.03 Uiso 1 1 calc R . .
C35 C 0.1827(2) 0.2092(6) 0.0162(3) 0.0207(12) Uani 1 1 d . . .
C40 C 0.3328(3) -0.1157(7) 0.2569(3) 0.0332(15) Uani 1 1 d . . .
H40A H 0.359 -0.2067 0.2785 0.04 Uiso 1 1 calc R . .
H40B H 0.3556 -0.0372 0.2961 0.04 Uiso 1 1 calc R . .
C42 C 0.2391(3) -0.1194(7) 0.3380(3) 0.0365(15) Uani 1 1 d . . .
H42A H 0.1852 -0.1328 0.3364 0.055 Uiso 1 1 calc R . .
H42B H 0.2561 -0.025 0.3622 0.055 Uiso 1 1 calc R . .
H42C H 0.2694 -0.1949 0.3728 0.055 Uiso 1 1 calc R . .
C43 C 0.2254(3) -0.2717(6) 0.2171(3) 0.0336(14) Uani 1 1 d . . .
H43A H 0.2578 -0.3448 0.2519 0.05 Uiso 1 1 calc R . .
H43B H 0.2305 -0.2778 0.1592 0.05 Uiso 1 1 calc R . .
H43C H 0.1721 -0.2884 0.2174 0.05 Uiso 1 1 calc R . .
C51 C 0.0673(3) 0.0757(6) 0.2547(3) 0.0250(13) Uani 1 1 d . . .
C61 C 0.3202(3) 0.2615(7) 0.2773(3) 0.0288(14) Uani 1 1 d . . .
N10 N 0.2824(2) -0.0128(5) 0.1208(2) 0.0205(10) Uani 1 1 d . . .
N20 N 0.1322(2) -0.0591(5) 0.0792(2) 0.0189(10) Uani 1 1 d . . .
N30 N 0.1773(2) 0.2141(5) 0.0976(2) 0.0204(10) Uani 1 1 d . . .
N41 N 0.2491(2) -0.1279(5) 0.2515(2) 0.0279(11) Uani 1 1 d . . .
N50 N 0.1199(2) 0.0807(5) 0.2266(2) 0.0270(11) Uani 1 1 d . . .
N60 N 0.2752(2) 0.1745(5) 0.2508(2) 0.0261(11) Uani 1 1 d . . .
S52 S -0.00611(8) 0.0626(2) 0.29444(8) 0.0417(5) Uani 1 1 d . . .
S62 S 0.38393(9) 0.3870(2) 0.31350(11) 0.0506(5) Uani 1 1 d . . .
Fe1 Fe 0.20309(4) 0.04609(8) 0.17162(4) 0.0202(2) Uani 1 1 d . . .
C1A C 0.5686(9) 0.8848(19) 0.3899(13) 0.056(5) Uani 0.48(2) 1 d PDU A 1
H1A H 0.5967 0.886 0.3449 0.068 Uiso 0.48(2) 1 calc PR A 1
Cl2A Cl 0.5091(8) 1.0355(12) 0.3720(10) 0.061(3) Uani 0.48(2) 1 d PDU A 1
Cl3A Cl 0.5173(6) 0.7248(10) 0.3769(7) 0.073(3) Uani 0.48(2) 1 d PDU A 1
Cl4A Cl 0.6367(6) 0.8793(16) 0.4836(8) 0.112(4) Uani 0.48(2) 1 d PDU A 1
C1B C 0.5668(8) 0.922(2) 0.3762(12) 0.061(5) Uani 0.52(2) 1 d PDU A 2
H1B H 0.5735 0.9324 0.3178 0.073 Uiso 0.52(2) 1 calc PR A 2
Cl2B Cl 0.4998(7) 1.0486(13) 0.3913(10) 0.073(3) Uani 0.52(2) 1 d PDU A 2
Cl3B Cl 0.5313(9) 0.7513(15) 0.3884(11) 0.136(4) Uani 0.52(2) 1 d PDU A 2
Cl4B Cl 0.6519(4) 0.956(2) 0.4480(9) 0.138(4) Uani 0.52(2) 1 d PDU A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C11 N10 1.357(6) . ?
C11 C12 1.364(7) . ?
C11 C40 1.511(7) . ?
C12 C13 1.394(8) . ?
C13 C14 1.385(7) . ?
C14 C15 1.386(7) . ?
C15 N10 1.355(6) . ?
C15 C16 1.535(6) . ?
C16 C17 1.535(6) . ?
C16 C35 1.539(7) . ?
C16 C25 1.541(7) . ?
C21 N20 1.349(6) . ?
C21 C22 1.378(6) . ?
C22 C23 1.383(7) . ?
C23 C24 1.370(7) . ?
C24 C25 1.387(6) . ?
C25 N20 1.371(6) . ?
C31 N30 1.347(6) . ?
C31 C32 1.375(7) . ?
C32 C33 1.378(7) . ?
C33 C34 1.386(7) . ?
C34 C35 1.382(7) . ?
C35 N30 1.366(6) . ?
C40 N41 1.504(6) . ?
C42 N41 1.479(6) . ?
C43 N41 1.471(7) . ?
C51 N50 1.163(6) . ?
C51 S52 1.631(5) . ?
C61 N60 1.152(6) . ?
C61 S62 1.644(6) . ?
N10 Fe1 1.918(4) . ?
N20 Fe1 1.978(4) . ?
N30 Fe1 1.959(4) . ?
N41 Fe1 2.114(4) . ?
N50 Fe1 1.972(4) . ?
N60 Fe1 1.988(4) . ?
C1A Cl4A 1.709(14) . ?
C1A Cl3A 1.738(14) . ?
C1A Cl2A 1.746(13) . ?
C1B Cl4B 1.716(12) . ?
C1B Cl3B 1.746(14) . ?
C1B Cl2B 1.752(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N10 C11 C12 123.0(5) . . ?
N10 C11 C40 112.6(5) . . ?
C12 C11 C40 124.3(5) . . ?
C11 C12 C13 117.8(5) . . ?
C14 C13 C12 120.2(5) . . ?
C13 C14 C15 118.8(5) . . ?
N10 C15 C14 121.0(5) . . ?
N10 C15 C16 114.0(4) . . ?
C14 C15 C16 124.8(4) . . ?
C17 C16 C15 110.2(4) . . ?
C17 C16 C35 109.9(4) . . ?
C15 C16 C35 111.4(4) . . ?
C17 C16 C25 110.6(4) . . ?
C15 C16 C25 107.7(4) . . ?
C35 C16 C25 107.0(4) . . ?
N20 C21 C22 124.5(5) . . ?
C21 C22 C23 117.5(5) . . ?
C24 C23 C22 119.9(5) . . ?
C23 C24 C25 120.0(5) . . ?
N20 C25 C24 121.1(5) . . ?
N20 C25 C16 116.8(4) . . ?
C24 C25 C16 122.0(4) . . ?
N30 C31 C32 123.4(5) . . ?
C31 C32 C33 118.5(6) . . ?
C32 C33 C34 119.1(6) . . ?
C35 C34 C33 120.1(5) . . ?
N30 C35 C34 120.7(5) . . ?
N30 C35 C16 115.3(5) . . ?
C34 C35 C16 123.9(4) . . ?
N41 C40 C11 108.7(4) . . ?
N50 C51 S52 178.0(6) . . ?
N60 C61 S62 179.0(5) . . ?
C15 N10 C11 118.8(4) . . ?
C15 N10 Fe1 123.5(3) . . ?
C11 N10 Fe1 117.5(3) . . ?
C21 N20 C25 117.0(4) . . ?
C21 N20 Fe1 123.8(3) . . ?
C25 N20 Fe1 119.1(3) . . ?
C31 N30 C35 118.1(5) . . ?
C31 N30 Fe1 120.9(3) . . ?
C35 N30 Fe1 120.9(4) . . ?
C43 N41 C42 108.7(5) . . ?
C43 N41 C40 106.4(4) . . ?
C42 N41 C40 108.0(4) . . ?
C43 N41 Fe1 115.3(3) . . ?
C42 N41 Fe1 115.4(4) . . ?
C40 N41 Fe1 102.2(3) . . ?
C51 N50 Fe1 167.7(5) . . ?
C61 N60 Fe1 162.2(4) . . ?
N10 Fe1 N30 92.57(17) . . ?
N10 Fe1 N50 172.8(2) . . ?
N30 Fe1 N50 93.66(18) . . ?
N10 Fe1 N20 86.45(16) . . ?
N30 Fe1 N20 85.00(16) . . ?
N50 Fe1 N20 90.44(16) . . ?
N10 Fe1 N60 90.81(17) . . ?
N30 Fe1 N60 86.57(17) . . ?
N50 Fe1 N60 93.22(17) . . ?
N20 Fe1 N60 171.01(18) . . ?
N10 Fe1 N41 80.25(17) . . ?
N30 Fe1 N41 170.91(17) . . ?
N50 Fe1 N41 93.89(18) . . ?
N20 Fe1 N41 100.00(17) . . ?
N60 Fe1 N41 87.95(17) . . ?
Cl4A C1A Cl3A 109.1(10) . . ?
Cl4A C1A Cl2A 116.7(11) . . ?
Cl3A C1A Cl2A 112.1(10) . . ?
Cl4B C1B Cl3B 112.4(10) . . ?
Cl4B C1B Cl2B 108.4(10) . . ?
Cl3B C1B Cl2B 107.6(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N10 C11 C12 C13 0.1(9) . . . . ?
C40 C11 C12 C13 175.6(6) . . . . ?
C11 C12 C13 C14 -4.3(9) . . . . ?
C12 C13 C14 C15 3.3(9) . . . . ?
C13 C14 C15 N10 2.0(8) . . . . ?
C13 C14 C15 C16 -172.3(5) . . . . ?
N10 C15 C16 C17 -176.6(5) . . . . ?
C14 C15 C16 C17 -1.9(7) . . . . ?
N10 C15 C16 C35 61.1(6) . . . . ?
C14 C15 C16 C35 -124.2(6) . . . . ?
N10 C15 C16 C25 -55.9(6) . . . . ?
C14 C15 C16 C25 118.8(6) . . . . ?
N20 C21 C22 C23 -1.2(8) . . . . ?
C21 C22 C23 C24 -0.9(8) . . . . ?
C22 C23 C24 C25 1.0(8) . . . . ?
C23 C24 C25 N20 0.7(8) . . . . ?
C23 C24 C25 C16 -176.7(5) . . . . ?
C17 C16 C25 N20 -178.5(4) . . . . ?
C15 C16 C25 N20 61.0(6) . . . . ?
C35 C16 C25 N20 -58.8(5) . . . . ?
C17 C16 C25 C24 -1.0(7) . . . . ?
C15 C16 C25 C24 -121.4(5) . . . . ?
C35 C16 C25 C24 118.7(5) . . . . ?
N30 C31 C32 C33 -0.2(8) . . . . ?
C31 C32 C33 C34 -0.3(7) . . . . ?
C32 C33 C34 C35 1.3(7) . . . . ?
C33 C34 C35 N30 -2.0(7) . . . . ?
C33 C34 C35 C16 174.3(4) . . . . ?
C17 C16 C35 N30 176.6(4) . . . . ?
C15 C16 C35 N30 -61.0(5) . . . . ?
C25 C16 C35 N30 56.5(5) . . . . ?
C17 C16 C35 C34 0.1(6) . . . . ?
C15 C16 C35 C34 122.6(5) . . . . ?
C25 C16 C35 C34 -120.0(5) . . . . ?
N10 C11 C40 N41 28.1(7) . . . . ?
C12 C11 C40 N41 -147.9(6) . . . . ?
C14 C15 N10 C11 -6.1(8) . . . . ?
C16 C15 N10 C11 168.8(4) . . . . ?
C14 C15 N10 Fe1 178.4(4) . . . . ?
C16 C15 N10 Fe1 -6.7(6) . . . . ?
C12 C11 N10 C15 5.1(8) . . . . ?
C40 C11 N10 C15 -170.9(5) . . . . ?
C12 C11 N10 Fe1 -179.1(5) . . . . ?
C40 C11 N10 Fe1 4.8(6) . . . . ?
C22 C21 N20 C25 2.8(8) . . . . ?
C22 C21 N20 Fe1 -179.7(4) . . . . ?
C24 C25 N20 C21 -2.6(7) . . . . ?
C16 C25 N20 C21 175.0(4) . . . . ?
C24 C25 N20 Fe1 179.9(4) . . . . ?
C16 C25 N20 Fe1 -2.6(6) . . . . ?
C32 C31 N30 C35 -0.4(7) . . . . ?
C32 C31 N30 Fe1 178.0(4) . . . . ?
C34 C35 N30 C31 1.5(7) . . . . ?
C16 C35 N30 C31 -175.1(4) . . . . ?
C34 C35 N30 Fe1 -176.9(3) . . . . ?
C16 C35 N30 Fe1 6.5(5) . . . . ?
C11 C40 N41 C43 78.4(5) . . . . ?
C11 C40 N41 C42 -165.0(5) . . . . ?
C11 C40 N41 Fe1 -42.9(5) . . . . ?
C15 N10 Fe1 N30 -34.6(4) . . . . ?
C11 N10 Fe1 N30 149.9(4) . . . . ?
C15 N10 Fe1 N20 50.2(4) . . . . ?
C11 N10 Fe1 N20 -125.3(4) . . . . ?
C15 N10 Fe1 N60 -121.2(4) . . . . ?
C11 N10 Fe1 N60 63.3(4) . . . . ?
C15 N10 Fe1 N41 151.0(4) . . . . ?
C11 N10 Fe1 N41 -24.5(4) . . . . ?
C31 N30 Fe1 N10 -144.1(4) . . . . ?
C35 N30 Fe1 N10 34.3(4) . . . . ?
C31 N30 Fe1 N50 39.5(4) . . . . ?
C35 N30 Fe1 N50 -142.1(4) . . . . ?
C31 N30 Fe1 N20 129.7(4) . . . . ?
C35 N30 Fe1 N20 -51.9(4) . . . . ?
C31 N30 Fe1 N60 -53.5(4) . . . . ?
C35 N30 Fe1 N60 124.9(4) . . . . ?
C51 N50 Fe1 N30 125.7(19) . . . . ?
C51 N50 Fe1 N20 40.7(19) . . . . ?
C51 N50 Fe1 N60 -147.5(18) . . . . ?
C51 N50 Fe1 N41 -59.4(19) . . . . ?
C21 N20 Fe1 N10 138.9(4) . . . . ?
C25 N20 Fe1 N10 -43.8(4) . . . . ?
C21 N20 Fe1 N30 -128.3(4) . . . . ?
C25 N20 Fe1 N30 49.1(4) . . . . ?
C21 N20 Fe1 N50 -34.6(4) . . . . ?
C25 N20 Fe1 N50 142.8(4) . . . . ?
C21 N20 Fe1 N41 59.4(4) . . . . ?
C25 N20 Fe1 N41 -123.2(4) . . . . ?
C61 N60 Fe1 N10 52.5(14) . . . . ?
C61 N60 Fe1 N30 -40.1(14) . . . . ?
C61 N60 Fe1 N50 -133.5(14) . . . . ?
C61 N60 Fe1 N41 132.7(14) . . . . ?
C43 N41 Fe1 N10 -78.6(4) . . . . ?
C42 N41 Fe1 N10 153.3(4) . . . . ?
C40 N41 Fe1 N10 36.4(3) . . . . ?
C43 N41 Fe1 N50 97.1(4) . . . . ?
C42 N41 Fe1 N50 -31.0(4) . . . . ?
C40 N41 Fe1 N50 -147.9(3) . . . . ?
C43 N41 Fe1 N20 6.0(4) . . . . ?
C42 N41 Fe1 N20 -122.1(4) . . . . ?
C40 N41 Fe1 N20 121.0(3) . . . . ?
C43 N41 Fe1 N60 -169.8(4) . . . . ?
C42 N41 Fe1 N60 62.1(4) . . . . ?
C40 N41 Fe1 N60 -54.8(3) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_database_code_depnum_ccdc_archive 'CCDC 960951'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound1a-273K

_audit_creation_date             2013-09-13T18:35:16-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;(1-{6-[1,1-di(pyridin-2-yl)ethyl]pyridin-2-yl}-N,N-
dimethylmethanamine)bis(thiocyanato-\kN)iron(II)--chloroform(1/1)
;
_chemical_formula_iupac          '[Fe (C20 H22 N4) (N C S)2].C H Cl3'
_chemical_formula_moiety         'C22 H22 Fe N6 S2, C H Cl3'
_chemical_formula_sum            'C23 H23 Cl3 Fe N6 S2'
_chemical_formula_weight         609.79

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.242(8)
_cell_length_b                   9.322(3)
_cell_length_c                   16.786(7)
_cell_angle_alpha                90
_cell_angle_beta                 104.10(4)
_cell_angle_gamma                90
_cell_volume                     2768.5(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    1377
_cell_measurement_theta_min      3.3041
_cell_measurement_theta_max      32.8471

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248
_exptl_crystal_recrystallization_method 
'precipitation: chloroform, diethyl ether, vapour diffusion, r. t., 3 d'

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.009
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.75056
_exptl_absorpt_correction_T_max  1

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_ambient_temperature      273(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent Sapphire 3'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_standards_number         0
_diffrn_reflns_av_R_equivalents  0.0952
_diffrn_reflns_av_unetI/netI     0.1245
_diffrn_reflns_number            13767
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.31
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_full        26
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             5436
_reflns_number_gt                3116
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
 The chloroform moiety exhibits rotational disorder. It has been modeled in
 two discrete positions using SAME, DELU and tight ISOR restraints (for the
 chlorine atoms). The s.o.f. refined to 48(2) % and 52(2) %, respectively.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0602P)²+1.9445P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5436
_refine_ls_number_parameters     347
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.1553
_refine_ls_R_factor_gt           0.0842
_refine_ls_wR_factor_ref         0.2009
_refine_ls_wR_factor_gt          0.1615
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.074

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29934(5) 0.94818(9) 0.32239(5) 0.0424(3) Uani 1 1 d . . .
S52 S 0.51244(12) 0.9466(3) 0.20376(12) 0.0873(7) Uani 1 1 d . . .
S62 S 0.11238(13) 0.6065(3) 0.18688(16) 0.0984(8) Uani 1 1 d . . .
N10 N 0.2190(3) 1.0189(5) 0.3845(3) 0.0438(12) Uani 1 1 d . . .
N20 N 0.3217(3) 0.7773(5) 0.4080(3) 0.0393(11) Uani 1 1 d . . .
N30 N 0.3729(3) 1.0562(5) 0.4274(3) 0.0394(11) Uani 1 1 d . . .
N41 N 0.2420(3) 1.1327(6) 0.2452(3) 0.0597(15) Uani 1 1 d . . .
N50 N 0.3844(3) 0.9278(7) 0.2644(3) 0.0644(16) Uani 1 1 d . . .
N60 N 0.2221(3) 0.8137(6) 0.2434(3) 0.0594(15) Uani 1 1 d . . .
C11 C 0.1588(4) 1.0865(7) 0.3371(4) 0.0528(17) Uani 1 1 d . . .
C12 C 0.0994(4) 1.1266(8) 0.3684(6) 0.075(2) Uani 1 1 d . . .
H12 H 0.0583 1.1749 0.3357 0.09 Uiso 1 1 calc R . .
C13 C 0.1012(4) 1.0949(8) 0.4483(6) 0.080(2) Uani 1 1 d . . .
H13 H 0.0597 1.1154 0.4694 0.095 Uiso 1 1 calc R . .
C14 C 0.1653(4) 1.0319(7) 0.4982(5) 0.0621(19) Uani 1 1 d . . .
H14 H 0.1679 1.0141 0.5534 0.075 Uiso 1 1 calc R . .
C15 C 0.2244(3) 0.9964(6) 0.4650(4) 0.0446(15) Uani 1 1 d . . .
C16 C 0.3005(3) 0.9379(6) 0.5158(3) 0.0398(14) Uani 1 1 d . . .
C17 C 0.2994(4) 0.9307(7) 0.6068(4) 0.0594(18) Uani 1 1 d . . .
H17A H 0.2629 0.8608 0.6141 0.089 Uiso 1 1 calc R . .
H17B H 0.286 1.023 0.6244 0.089 Uiso 1 1 calc R . .
H17C H 0.3485 0.9039 0.6389 0.089 Uiso 1 1 calc R . .
C21 C 0.3411(3) 0.6499(7) 0.3813(4) 0.0522(17) Uani 1 1 d . . .
H21 H 0.3433 0.6422 0.3267 0.063 Uiso 1 1 calc R . .
C22 C 0.3577(4) 0.5311(7) 0.4303(5) 0.0581(19) Uani 1 1 d . . .
H22 H 0.372 0.4453 0.4101 0.07 Uiso 1 1 calc R . .
C23 C 0.3526(4) 0.5433(7) 0.5099(5) 0.0608(19) Uani 1 1 d . . .
H23 H 0.3628 0.4646 0.5449 0.073 Uiso 1 1 calc R . .
C24 C 0.3321(3) 0.6722(7) 0.5379(4) 0.0526(17) Uani 1 1 d . . .
H24 H 0.3285 0.6803 0.592 0.063 Uiso 1 1 calc R . .
C25 C 0.3170(3) 0.7892(6) 0.4866(3) 0.0391(14) Uani 1 1 d . . .
C31 C 0.4294(3) 1.1407(6) 0.4169(4) 0.0447(15) Uani 1 1 d . . .
H31 H 0.437 1.1496 0.3643 0.054 Uiso 1 1 calc R . .
C32 C 0.4765(3) 1.2147(6) 0.4800(4) 0.0542(17) Uani 1 1 d . . .
H32 H 0.5143 1.2738 0.47 0.065 Uiso 1 1 calc R . .
C33 C 0.4667(4) 1.2000(7) 0.5578(4) 0.0564(18) Uani 1 1 d . . .
H33 H 0.4978 1.2483 0.6017 0.068 Uiso 1 1 calc R . .
C34 C 0.4099(4) 1.1122(6) 0.5693(4) 0.0484(16) Uani 1 1 d . . .
H34 H 0.4024 1.1012 0.6219 0.058 Uiso 1 1 calc R . .
C35 C 0.3637(3) 1.0399(5) 0.5047(3) 0.0347(13) Uani 1 1 d . . .
C40 C 0.1632(4) 1.1167(8) 0.2507(4) 0.070(2) Uani 1 1 d . . .
H40A H 0.1397 1.0388 0.2153 0.084 Uiso 1 1 calc R . .
H40B H 0.1356 1.2041 0.2316 0.084 Uiso 1 1 calc R . .
C42 C 0.2460(6) 1.1245(9) 0.1585(4) 0.098(3) Uani 1 1 d . . .
H42A H 0.2098 1.1891 0.126 0.147 Uiso 1 1 calc R . .
H42B H 0.2351 1.0283 0.1387 0.147 Uiso 1 1 calc R . .
H42C H 0.2959 1.1508 0.1543 0.147 Uiso 1 1 calc R . .
C43 C 0.2707(4) 1.2737(7) 0.2798(4) 0.074(2) Uani 1 1 d . . .
H43A H 0.2414 1.3488 0.2479 0.11 Uiso 1 1 calc R . .
H43B H 0.3227 1.2837 0.2783 0.11 Uiso 1 1 calc R . .
H43C H 0.2665 1.28 0.3356 0.11 Uiso 1 1 calc R . .
C51 C 0.4379(4) 0.9349(8) 0.2394(4) 0.0606(19) Uani 1 1 d . . .
C61 C 0.1770(4) 0.7290(8) 0.2203(4) 0.0580(18) Uani 1 1 d . . .
C1A C 0.0690(6) 0.5990(13) 0.3839(7) 0.125(3) Uani 0.48(2) 1 d PDU A 1
H1A H 0.0713 0.5987 0.3262 0.15 Uiso 0.48(2) 1 calc PR A 1
Cl2A Cl 0.0036(8) 0.4664(16) 0.3949(14) 0.134(5) Uani 0.48(2) 1 d PDU A 1
Cl3A Cl 0.0345(13) 0.7528(15) 0.4016(17) 0.263(9) Uani 0.48(2) 1 d PDU A 1
Cl4A Cl 0.1529(5) 0.527(2) 0.4403(9) 0.214(6) Uani 0.48(2) 1 d PDU A 1
C1B C 0.0690(6) 0.5990(13) 0.3839(7) 0.125(3) Uani 0.52(2) 1 d PDU A 2
H1B H 0.098 0.5975 0.3419 0.15 Uiso 0.52(2) 1 calc PR A 2
Cl2B Cl 0.0101(9) 0.4601(13) 0.3631(13) 0.135(5) Uani 0.52(2) 1 d PDU A 2
Cl3B Cl 0.0210(6) 0.7638(10) 0.3721(8) 0.151(4) Uani 0.52(2) 1 d PDU A 2
Cl4B Cl 0.1350(9) 0.6260(19) 0.4774(9) 0.213(8) Uani 0.52(2) 1 d PDU A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N50 2.032(6) . ?
Fe1 N60 2.099(6) . ?
Fe1 N10 2.101(5) . ?
Fe1 N20 2.117(5) . ?
Fe1 N30 2.183(5) . ?
Fe1 N41 2.252(5) . ?
S52 C51 1.617(8) . ?
S62 C61 1.639(8) . ?
N10 C11 1.345(7) . ?
N10 C15 1.347(7) . ?
N20 C21 1.347(7) . ?
N20 C25 1.349(7) . ?
N30 C31 1.342(7) . ?
N30 C35 1.357(7) . ?
N41 C40 1.469(9) . ?
N41 C42 1.477(8) . ?
N41 C43 1.480(8) . ?
N50 C51 1.154(9) . ?
N60 C61 1.138(8) . ?
C11 C12 1.366(10) . ?
C11 C40 1.500(10) . ?
C12 C13 1.367(10) . ?
C13 C14 1.391(10) . ?
C14 C15 1.370(8) . ?
C15 C16 1.541(8) . ?
C16 C25 1.524(8) . ?
C16 C17 1.535(8) . ?
C16 C35 1.540(7) . ?
C21 C22 1.369(9) . ?
C22 C23 1.367(9) . ?
C23 C24 1.374(9) . ?
C24 C25 1.375(8) . ?
C31 C32 1.377(8) . ?
C32 C33 1.366(9) . ?
C33 C34 1.370(9) . ?
C34 C35 1.377(7) . ?
C1A Cl3A 1.622(15) . ?
C1A Cl4A 1.727(14) . ?
C1A Cl2A 1.758(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N50 Fe1 N60 96.6(2) . . ?
N50 Fe1 N10 166.8(2) . . ?
N60 Fe1 N10 93.3(2) . . ?
N50 Fe1 N20 102.2(2) . . ?
N60 Fe1 N20 88.2(2) . . ?
N10 Fe1 N20 86.69(19) . . ?
N50 Fe1 N30 92.2(2) . . ?
N60 Fe1 N30 166.2(2) . . ?
N10 Fe1 N30 79.67(18) . . ?
N20 Fe1 N30 79.64(17) . . ?
N50 Fe1 N41 95.6(2) . . ?
N60 Fe1 N41 86.9(2) . . ?
N10 Fe1 N41 76.3(2) . . ?
N20 Fe1 N41 162.0(2) . . ?
N30 Fe1 N41 102.73(19) . . ?
C11 N10 C15 121.0(5) . . ?
C11 N10 Fe1 114.9(4) . . ?
C15 N10 Fe1 124.0(4) . . ?
C21 N20 C25 118.8(5) . . ?
C21 N20 Fe1 117.4(4) . . ?
C25 N20 Fe1 123.7(4) . . ?
C31 N30 C35 117.9(5) . . ?
C31 N30 Fe1 120.4(4) . . ?
C35 N30 Fe1 121.7(4) . . ?
C40 N41 C42 110.0(6) . . ?
C40 N41 C43 108.8(6) . . ?
C42 N41 C43 109.6(6) . . ?
C40 N41 Fe1 102.2(4) . . ?
C42 N41 Fe1 113.6(5) . . ?
C43 N41 Fe1 112.4(4) . . ?
C51 N50 Fe1 168.8(6) . . ?
C61 N60 Fe1 161.5(6) . . ?
N10 C11 C12 120.8(7) . . ?
N10 C11 C40 115.5(6) . . ?
C12 C11 C40 123.7(7) . . ?
C11 C12 C13 119.0(7) . . ?
C12 C13 C14 119.9(7) . . ?
C15 C14 C13 119.1(7) . . ?
N10 C15 C14 119.9(6) . . ?
N10 C15 C16 116.5(5) . . ?
C14 C15 C16 123.6(6) . . ?
C25 C16 C17 109.4(5) . . ?
C25 C16 C35 108.1(4) . . ?
C17 C16 C35 109.8(5) . . ?
C25 C16 C15 111.5(4) . . ?
C17 C16 C15 109.7(5) . . ?
C35 C16 C15 108.3(4) . . ?
N20 C21 C22 123.5(6) . . ?
C23 C22 C21 117.6(6) . . ?
C22 C23 C24 119.7(6) . . ?
C23 C24 C25 120.6(6) . . ?
N20 C25 C24 119.8(6) . . ?
N20 C25 C16 117.0(5) . . ?
C24 C25 C16 123.1(5) . . ?
N30 C31 C32 123.3(6) . . ?
C33 C32 C31 118.9(6) . . ?
C32 C33 C34 118.3(6) . . ?
C33 C34 C35 121.3(6) . . ?
N30 C35 C34 120.3(5) . . ?
N30 C35 C16 117.1(5) . . ?
C34 C35 C16 122.6(5) . . ?
N41 C40 C11 111.4(5) . . ?
N50 C51 S52 179.3(8) . . ?
N60 C61 S62 179.7(7) . . ?
Cl3A C1A Cl4A 125.1(10) . . ?
Cl3A C1A Cl2A 107.4(11) . . ?
Cl4A C1A Cl2A 101.6(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N50 Fe1 N10 C11 78.5(10) . . . . ?
N60 Fe1 N10 C11 -60.6(4) . . . . ?
N20 Fe1 N10 C11 -148.6(4) . . . . ?
N30 Fe1 N10 C11 131.3(4) . . . . ?
N41 Fe1 N10 C11 25.4(4) . . . . ?
N50 Fe1 N10 C15 -103.4(10) . . . . ?
N60 Fe1 N10 C15 117.5(5) . . . . ?
N20 Fe1 N10 C15 29.5(5) . . . . ?
N30 Fe1 N10 C15 -50.6(5) . . . . ?
N41 Fe1 N10 C15 -156.5(5) . . . . ?
N50 Fe1 N20 C21 -43.2(5) . . . . ?
N60 Fe1 N20 C21 53.2(4) . . . . ?
N10 Fe1 N20 C21 146.6(4) . . . . ?
N30 Fe1 N20 C21 -133.3(4) . . . . ?
N41 Fe1 N20 C21 127.4(6) . . . . ?
N50 Fe1 N20 C25 137.3(4) . . . . ?
N60 Fe1 N20 C25 -126.2(4) . . . . ?
N10 Fe1 N20 C25 -32.8(4) . . . . ?
N30 Fe1 N20 C25 47.3(4) . . . . ?
N41 Fe1 N20 C25 -52.0(8) . . . . ?
N50 Fe1 N30 C31 32.4(4) . . . . ?
N60 Fe1 N30 C31 162.6(8) . . . . ?
N10 Fe1 N30 C31 -137.1(4) . . . . ?
N20 Fe1 N30 C31 134.4(4) . . . . ?
N41 Fe1 N30 C31 -63.8(4) . . . . ?
N50 Fe1 N30 C35 -147.1(4) . . . . ?
N60 Fe1 N30 C35 -17.0(10) . . . . ?
N10 Fe1 N30 C35 43.3(4) . . . . ?
N20 Fe1 N30 C35 -45.2(4) . . . . ?
N41 Fe1 N30 C35 116.6(4) . . . . ?
N50 Fe1 N41 C40 153.8(4) . . . . ?
N60 Fe1 N41 C40 57.4(4) . . . . ?
N10 Fe1 N41 C40 -36.8(4) . . . . ?
N20 Fe1 N41 C40 -17.0(8) . . . . ?
N30 Fe1 N41 C40 -112.6(4) . . . . ?
N50 Fe1 N41 C42 35.4(5) . . . . ?
N60 Fe1 N41 C42 -61.0(5) . . . . ?
N10 Fe1 N41 C42 -155.1(5) . . . . ?
N20 Fe1 N41 C42 -135.3(7) . . . . ?
N30 Fe1 N41 C42 129.0(5) . . . . ?
N50 Fe1 N41 C43 -89.7(5) . . . . ?
N60 Fe1 N41 C43 173.9(5) . . . . ?
N10 Fe1 N41 C43 79.7(5) . . . . ?
N20 Fe1 N41 C43 99.5(7) . . . . ?
N30 Fe1 N41 C43 3.8(5) . . . . ?
N60 Fe1 N50 C51 168(3) . . . . ?
N10 Fe1 N50 C51 29(4) . . . . ?
N20 Fe1 N50 C51 -103(3) . . . . ?
N30 Fe1 N50 C51 -23(3) . . . . ?
N41 Fe1 N50 C51 80(3) . . . . ?
N50 Fe1 N60 C61 138.1(18) . . . . ?
N10 Fe1 N60 C61 -50.5(18) . . . . ?
N20 Fe1 N60 C61 36.1(18) . . . . ?
N30 Fe1 N60 C61 8(2) . . . . ?
N41 Fe1 N60 C61 -126.6(18) . . . . ?
C15 N10 C11 C12 -3.9(9) . . . . ?
Fe1 N10 C11 C12 174.2(5) . . . . ?
C15 N10 C11 C40 174.5(5) . . . . ?
Fe1 N10 C11 C40 -7.4(7) . . . . ?
N10 C11 C12 C13 -1.2(11) . . . . ?
C40 C11 C12 C13 -179.4(7) . . . . ?
C11 C12 C13 C14 4.6(12) . . . . ?
C12 C13 C14 C15 -3.1(11) . . . . ?
C11 N10 C15 C14 5.4(9) . . . . ?
Fe1 N10 C15 C14 -172.6(5) . . . . ?
C11 N10 C15 C16 -171.5(5) . . . . ?
Fe1 N10 C15 C16 10.6(7) . . . . ?
C13 C14 C15 N10 -1.9(10) . . . . ?
C13 C14 C15 C16 174.7(6) . . . . ?
N10 C15 C16 C25 -63.5(6) . . . . ?
C14 C15 C16 C25 119.7(6) . . . . ?
N10 C15 C16 C17 175.2(5) . . . . ?
C14 C15 C16 C17 -1.6(8) . . . . ?
N10 C15 C16 C35 55.3(6) . . . . ?
C14 C15 C16 C35 -121.5(6) . . . . ?
C25 N20 C21 C22 -1.2(9) . . . . ?
Fe1 N20 C21 C22 179.4(5) . . . . ?
N20 C21 C22 C23 1.5(10) . . . . ?
C21 C22 C23 C24 -0.7(10) . . . . ?
C22 C23 C24 C25 -0.2(10) . . . . ?
C21 N20 C25 C24 0.2(8) . . . . ?
Fe1 N20 C25 C24 179.6(4) . . . . ?
C21 N20 C25 C16 175.7(5) . . . . ?
Fe1 N20 C25 C16 -4.9(7) . . . . ?
C23 C24 C25 N20 0.5(9) . . . . ?
C23 C24 C25 C16 -174.8(6) . . . . ?
C17 C16 C25 N20 -178.5(5) . . . . ?
C35 C16 C25 N20 -59.0(6) . . . . ?
C15 C16 C25 N20 60.0(6) . . . . ?
C17 C16 C25 C24 -3.1(8) . . . . ?
C35 C16 C25 C24 116.4(6) . . . . ?
C15 C16 C25 C24 -124.6(6) . . . . ?
C35 N30 C31 C32 -2.2(8) . . . . ?
Fe1 N30 C31 C32 178.3(4) . . . . ?
N30 C31 C32 C33 1.4(9) . . . . ?
C31 C32 C33 C34 -0.3(9) . . . . ?
C32 C33 C34 C35 0.2(9) . . . . ?
C31 N30 C35 C34 2.0(8) . . . . ?
Fe1 N30 C35 C34 -178.5(4) . . . . ?
C31 N30 C35 C16 -177.7(5) . . . . ?
Fe1 N30 C35 C16 1.9(6) . . . . ?
C33 C34 C35 N30 -1.0(9) . . . . ?
C33 C34 C35 C16 178.6(5) . . . . ?
C25 C16 C35 N30 59.7(6) . . . . ?
C17 C16 C35 N30 179.0(5) . . . . ?
C15 C16 C35 N30 -61.2(6) . . . . ?
C25 C16 C35 C34 -119.9(6) . . . . ?
C17 C16 C35 C34 -0.7(7) . . . . ?
C15 C16 C35 C34 119.1(6) . . . . ?
C42 N41 C40 C11 165.3(6) . . . . ?
C43 N41 C40 C11 -74.6(7) . . . . ?
Fe1 N41 C40 C11 44.4(6) . . . . ?
N10 C11 C40 N41 -28.0(8) . . . . ?
C12 C11 C40 N41 150.4(7) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_database_code_depnum_ccdc_archive 'CCDC 960952'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound1b-150K

_audit_creation_date             2013-09-13T18:28:57-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;(1-{6-[1,1-di(pyridin-2-yl)ethyl]pyridin-2-yl}-N,N-
dimethylmethanamine)bis(thiocyanato-\kN)iron(II)--chloroform(1/2)
;
_chemical_formula_iupac          '[Fe (C20 H22 N4) (N C S)2].2C H Cl3'
_chemical_formula_moiety         'C22 H22 Fe N6 S2, 2(C H Cl3)'
_chemical_formula_sum            'C24 H24 Cl6 Fe N6 S2'
_chemical_formula_weight         729.16

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.7750(18)
_cell_length_b                   15.5077(14)
_cell_length_c                   14.5434(19)
_cell_angle_alpha                90
_cell_angle_beta                 91.427(13)
_cell_angle_gamma                90
_cell_volume                     3105.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(2)
_cell_measurement_reflns_used    7503
_cell_measurement_theta_min      3.2307
_cell_measurement_theta_max      32.5898

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1480
_exptl_crystal_recrystallization_method 
'evaporation: chloroform, r. t., 2 weeks'

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.54673
_exptl_absorpt_correction_T_max  1

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_ambient_temperature      150.0(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent Sapphire 3'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_standards_number         0
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_number            24699
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.24
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_full        26
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             6079
_reflns_number_gt                4964
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
 The chloroform moiety centered at C5 exhibits positional disorder. It has
 been modeled in two discrete positions using SAME as well as tight DELU and
 ISOR restraints. The s.o.f. refined to 67(2) % and 33(2) %, respectively.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0555P)²+3.6304P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6079
_refine_ls_number_parameters     392
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0559
_refine_ls_wR_factor_ref         0.1336
_refine_ls_wR_factor_gt          0.1247
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.56
_refine_diff_density_rms         0.082

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.0782(3) 0.5424(2) 0.3489(2) 0.0220(7) Uani 1 1 d . . .
C12 C 0.0010(3) 0.5954(2) 0.3682(3) 0.0252(8) Uani 1 1 d . . .
H12 H -0.0458 0.61 0.3216 0.03 Uiso 1 1 calc R . .
C13 C -0.0071(3) 0.6268(2) 0.4564(3) 0.0267(8) Uani 1 1 d . . .
H13 H -0.0618 0.6604 0.4721 0.032 Uiso 1 1 calc R . .
C14 C 0.0649(3) 0.6091(2) 0.5219(3) 0.0237(8) Uani 1 1 d . . .
H14 H 0.0614 0.6328 0.582 0.028 Uiso 1 1 calc R . .
C15 C 0.1421(2) 0.5565(2) 0.4988(2) 0.0197(7) Uani 1 1 d . . .
C16 C 0.2325(3) 0.5409(2) 0.5600(2) 0.0211(7) Uani 1 1 d . . .
C17 C 0.2242(3) 0.5896(2) 0.6511(2) 0.0297(8) Uani 1 1 d . . .
H17A H 0.168 0.5682 0.6841 0.045 Uiso 1 1 calc R . .
H17B H 0.2161 0.6513 0.6387 0.045 Uiso 1 1 calc R . .
H17C H 0.2834 0.5805 0.6887 0.045 Uiso 1 1 calc R . .
C31 C 0.4208(3) 0.5513(2) 0.3822(3) 0.0260(8) Uani 1 1 d . . .
H31 H 0.4341 0.522 0.3265 0.031 Uiso 1 1 calc R . .
C32 C 0.4868(3) 0.6113(2) 0.4149(3) 0.0288(8) Uani 1 1 d . . .
H32 H 0.544 0.6234 0.3821 0.035 Uiso 1 1 calc R . .
C33 C 0.4683(3) 0.6535(2) 0.4957(3) 0.0296(8) Uani 1 1 d . . .
H33 H 0.5119 0.6962 0.5189 0.035 Uiso 1 1 calc R . .
C34 C 0.3856(3) 0.6329(2) 0.5428(3) 0.0272(8) Uani 1 1 d . . .
H34 H 0.3721 0.661 0.5992 0.033 Uiso 1 1 calc R . .
C35 C 0.3223(2) 0.5712(2) 0.5075(2) 0.0202(7) Uani 1 1 d . . .
C21 C 0.2783(3) 0.3100(2) 0.5129(3) 0.0261(8) Uani 1 1 d . . .
H21 H 0.2891 0.2757 0.4599 0.031 Uiso 1 1 calc R . .
C22 C 0.2817(3) 0.2711(2) 0.5976(3) 0.0331(9) Uani 1 1 d . . .
H22 H 0.2962 0.2114 0.6032 0.04 Uiso 1 1 calc R . .
C23 C 0.2641(3) 0.3197(3) 0.6742(3) 0.0334(9) Uani 1 1 d . . .
H23 H 0.2636 0.2936 0.7333 0.04 Uiso 1 1 calc R . .
C24 C 0.2469(3) 0.4070(2) 0.6643(3) 0.0290(8) Uani 1 1 d . . .
H24 H 0.2356 0.4416 0.7169 0.035 Uiso 1 1 calc R . .
C25 C 0.2462(2) 0.4440(2) 0.5771(3) 0.0224(7) Uani 1 1 d . . .
C40 C 0.0998(3) 0.5080(2) 0.2561(3) 0.0269(8) Uani 1 1 d . . .
H40A H 0.0695 0.4506 0.2475 0.032 Uiso 1 1 calc R . .
H40B H 0.0733 0.5472 0.2079 0.032 Uiso 1 1 calc R . .
C42 C 0.2291(3) 0.4484(3) 0.1671(3) 0.0416(11) Uani 1 1 d . . .
H42A H 0.2033 0.3901 0.175 0.062 Uiso 1 1 calc R . .
H42B H 0.2996 0.4455 0.1601 0.062 Uiso 1 1 calc R . .
H42C H 0.1991 0.4748 0.1122 0.062 Uiso 1 1 calc R . .
C43 C 0.2467(3) 0.5898(2) 0.2343(3) 0.0335(9) Uani 1 1 d . . .
H43A H 0.3169 0.5862 0.2258 0.05 Uiso 1 1 calc R . .
H43B H 0.2337 0.6258 0.288 0.05 Uiso 1 1 calc R . .
H43C H 0.2155 0.6153 0.1795 0.05 Uiso 1 1 calc R . .
C51 C 0.4115(3) 0.3372(2) 0.2956(2) 0.0234(8) Uani 1 1 d . . .
C61 C 0.1128(3) 0.2840(2) 0.3540(3) 0.0277(8) Uani 1 1 d . . .
N10 N 0.1451(2) 0.52080(17) 0.41449(19) 0.0191(6) Uani 1 1 d . . .
N30 N 0.3379(2) 0.53208(17) 0.4258(2) 0.0210(6) Uani 1 1 d . . .
N20 N 0.2600(2) 0.39541(17) 0.5018(2) 0.0215(6) Uani 1 1 d . . .
N41 N 0.2069(2) 0.50134(18) 0.2492(2) 0.0252(7) Uani 1 1 d . . .
N50 N 0.3523(2) 0.37518(19) 0.3278(2) 0.0276(7) Uani 1 1 d . . .
N60 N 0.1551(2) 0.34849(19) 0.3477(2) 0.0265(7) Uani 1 1 d . . .
S52 S 0.50023(7) 0.28238(6) 0.24642(7) 0.0322(2) Uani 1 1 d . . .
S62 S 0.05402(9) 0.19343(6) 0.36687(8) 0.0415(3) Uani 1 1 d . . .
Fe1 Fe 0.24684(4) 0.44440(3) 0.37711(4) 0.02028(14) Uani 1 1 d . . .
C1 C 0.1060(4) 0.8425(3) 0.4265(4) 0.0543(13) Uani 1 1 d . . .
H1 H 0.0621 0.8224 0.4758 0.065 Uiso 1 1 calc R . .
Cl2 Cl 0.22162(13) 0.80309(13) 0.44980(16) 0.1004(6) Uani 1 1 d . . .
Cl3 Cl 0.10573(15) 0.95607(10) 0.42525(14) 0.0941(6) Uani 1 1 d . . .
Cl4 Cl 0.06061(10) 0.80433(7) 0.32011(9) 0.0557(3) Uani 1 1 d . . .
C5A C 0.4450(6) 0.4099(6) 0.8690(6) 0.038(2) Uani 0.670(14) 1 d PDU A 1
H5A H 0.4497 0.3669 0.818 0.046 Uiso 0.670(14) 1 calc PR A 1
Cl6A Cl 0.4529(4) 0.5138(3) 0.8218(4) 0.0368(8) Uani 0.670(14) 1 d PDU A 1
Cl7A Cl 0.5398(4) 0.39129(18) 0.9478(3) 0.0634(13) Uani 0.670(14) 1 d PDU A 1
Cl8A Cl 0.3308(5) 0.3980(3) 0.9202(4) 0.0680(13) Uani 0.670(14) 1 d PDU A 1
C5B C 0.4156(13) 0.4050(13) 0.8791(13) 0.047(5) Uani 0.330(14) 1 d PDU A 2
H5B H 0.4301 0.3592 0.833 0.057 Uiso 0.330(14) 1 calc PR A 2
Cl6B Cl 0.4396(12) 0.5061(9) 0.8302(12) 0.069(4) Uani 0.330(14) 1 d PDU A 2
Cl7B Cl 0.4841(13) 0.3845(4) 0.9791(8) 0.087(4) Uani 0.330(14) 1 d PDU A 2
Cl8B Cl 0.2908(10) 0.3988(7) 0.9056(6) 0.063(2) Uani 0.330(14) 1 d PDU A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C11 N10 1.353(4) . ?
C11 C12 1.378(5) . ?
C11 C40 1.487(5) . ?
C12 C13 1.379(5) . ?
C13 C14 1.385(5) . ?
C14 C15 1.389(5) . ?
C15 N10 1.347(4) . ?
C15 C16 1.531(5) . ?
C16 C17 1.531(5) . ?
C16 C25 1.535(5) . ?
C16 C35 1.544(5) . ?
C31 N30 1.353(4) . ?
C31 C32 1.378(5) . ?
C32 C33 1.374(5) . ?
C33 C34 1.382(5) . ?
C34 C35 1.384(5) . ?
C35 N30 1.356(4) . ?
C21 N20 1.358(4) . ?
C21 C22 1.371(6) . ?
C22 C23 1.371(6) . ?
C23 C24 1.381(5) . ?
C24 C25 1.393(5) . ?
C25 N20 1.347(5) . ?
C40 N41 1.486(5) . ?
C42 N41 1.487(5) . ?
C43 N41 1.495(5) . ?
C51 N50 1.118(4) . ?
C51 S52 1.665(4) . ?
C61 N60 1.163(5) . ?
C61 S62 1.633(4) . ?
N10 Fe1 1.924(3) . ?
N30 Fe1 1.970(3) . ?
N20 Fe1 1.970(3) . ?
N41 Fe1 2.119(3) . ?
N50 Fe1 1.956(3) . ?
N60 Fe1 1.991(3) . ?
C1 Cl2 1.732(6) . ?
C1 Cl4 1.757(5) . ?
C1 Cl3 1.761(5) . ?
C5A Cl7A 1.740(8) . ?
C5A Cl6A 1.757(8) . ?
C5A Cl8A 1.767(8) . ?
C5B Cl7B 1.742(15) . ?
C5B Cl6B 1.758(14) . ?
C5B Cl8B 1.775(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N10 C11 C12 121.3(3) . . ?
N10 C11 C40 113.8(3) . . ?
C12 C11 C40 124.8(3) . . ?
C11 C12 C13 118.7(4) . . ?
C12 C13 C14 119.8(3) . . ?
C13 C14 C15 119.3(3) . . ?
N10 C15 C14 120.2(3) . . ?
N10 C15 C16 114.9(3) . . ?
C14 C15 C16 124.6(3) . . ?
C17 C16 C15 110.4(3) . . ?
C17 C16 C25 110.8(3) . . ?
C15 C16 C25 110.1(3) . . ?
C17 C16 C35 110.8(3) . . ?
C15 C16 C35 108.3(3) . . ?
C25 C16 C35 106.3(3) . . ?
N30 C31 C32 122.9(3) . . ?
C33 C32 C31 118.8(3) . . ?
C32 C33 C34 119.2(3) . . ?
C33 C34 C35 119.6(3) . . ?
N30 C35 C34 121.6(3) . . ?
N30 C35 C16 116.3(3) . . ?
C34 C35 C16 122.1(3) . . ?
N20 C21 C22 122.5(4) . . ?
C23 C22 C21 119.1(3) . . ?
C22 C23 C24 119.2(4) . . ?
C23 C24 C25 119.7(4) . . ?
N20 C25 C24 120.8(3) . . ?
N20 C25 C16 115.8(3) . . ?
C24 C25 C16 123.3(3) . . ?
N41 C40 C11 107.9(3) . . ?
N50 C51 S52 178.8(3) . . ?
N60 C61 S62 177.9(4) . . ?
C15 N10 C11 120.3(3) . . ?
C15 N10 Fe1 123.3(2) . . ?
C11 N10 Fe1 116.2(2) . . ?
C31 N30 C35 117.8(3) . . ?
C31 N30 Fe1 121.4(2) . . ?
C35 N30 Fe1 120.7(2) . . ?
C25 N20 C21 118.6(3) . . ?
C25 N20 Fe1 121.4(2) . . ?
C21 N20 Fe1 119.9(3) . . ?
C40 N41 C42 108.5(3) . . ?
C40 N41 C43 108.3(3) . . ?
C42 N41 C43 107.9(3) . . ?
C40 N41 Fe1 101.9(2) . . ?
C42 N41 Fe1 114.9(2) . . ?
C43 N41 Fe1 114.9(2) . . ?
C51 N50 Fe1 176.7(3) . . ?
C61 N60 Fe1 160.5(3) . . ?
N10 Fe1 N50 173.77(12) . . ?
N10 Fe1 N30 86.27(12) . . ?
N50 Fe1 N30 92.21(12) . . ?
N10 Fe1 N20 91.63(12) . . ?
N50 Fe1 N20 94.23(12) . . ?
N30 Fe1 N20 83.81(12) . . ?
N10 Fe1 N60 93.31(12) . . ?
N50 Fe1 N60 89.12(12) . . ?
N30 Fe1 N60 171.08(13) . . ?
N20 Fe1 N60 87.30(12) . . ?
N10 Fe1 N41 79.43(11) . . ?
N50 Fe1 N41 94.91(12) . . ?
N30 Fe1 N41 100.19(12) . . ?
N20 Fe1 N41 169.87(11) . . ?
N60 Fe1 N41 88.47(13) . . ?
Cl2 C1 Cl4 111.0(3) . . ?
Cl2 C1 Cl3 110.9(3) . . ?
Cl4 C1 Cl3 109.1(3) . . ?
Cl7A C5A Cl6A 110.9(5) . . ?
Cl7A C5A Cl8A 111.5(5) . . ?
Cl6A C5A Cl8A 108.9(5) . . ?
Cl7B C5B Cl6B 113.4(12) . . ?
Cl7B C5B Cl8B 108.5(9) . . ?
Cl6B C5B Cl8B 109.2(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N10 C11 C12 C13 0.2(5) . . . . ?
C40 C11 C12 C13 -176.1(3) . . . . ?
C11 C12 C13 C14 3.9(5) . . . . ?
C12 C13 C14 C15 -3.0(5) . . . . ?
C13 C14 C15 N10 -2.2(5) . . . . ?
C13 C14 C15 C16 171.9(3) . . . . ?
N10 C15 C16 C17 175.9(3) . . . . ?
C14 C15 C16 C17 1.5(5) . . . . ?
N10 C15 C16 C25 -61.5(4) . . . . ?
C14 C15 C16 C25 124.1(3) . . . . ?
N10 C15 C16 C35 54.4(4) . . . . ?
C14 C15 C16 C35 -120.0(3) . . . . ?
N30 C31 C32 C33 0.4(6) . . . . ?
C31 C32 C33 C34 1.6(6) . . . . ?
C32 C33 C34 C35 -0.7(6) . . . . ?
C33 C34 C35 N30 -2.2(5) . . . . ?
C33 C34 C35 C16 175.7(3) . . . . ?
C17 C16 C35 N30 179.4(3) . . . . ?
C15 C16 C35 N30 -59.3(4) . . . . ?
C25 C16 C35 N30 59.0(4) . . . . ?
C17 C16 C35 C34 1.5(5) . . . . ?
C15 C16 C35 C34 122.7(3) . . . . ?
C25 C16 C35 C34 -119.0(3) . . . . ?
N20 C21 C22 C23 1.4(6) . . . . ?
C21 C22 C23 C24 -2.4(6) . . . . ?
C22 C23 C24 C25 1.0(6) . . . . ?
C23 C24 C25 N20 1.5(5) . . . . ?
C23 C24 C25 C16 -177.1(3) . . . . ?
C17 C16 C25 N20 -176.3(3) . . . . ?
C15 C16 C25 N20 61.3(4) . . . . ?
C35 C16 C25 N20 -55.8(4) . . . . ?
C17 C16 C25 C24 2.4(5) . . . . ?
C15 C16 C25 C24 -120.0(4) . . . . ?
C35 C16 C25 C24 122.8(4) . . . . ?
N10 C11 C40 N41 -29.9(4) . . . . ?
C12 C11 C40 N41 146.7(3) . . . . ?
C14 C15 N10 C11 6.4(5) . . . . ?
C16 C15 N10 C11 -168.3(3) . . . . ?
C14 C15 N10 Fe1 -178.1(2) . . . . ?
C16 C15 N10 Fe1 7.2(4) . . . . ?
C12 C11 N10 C15 -5.5(5) . . . . ?
C40 C11 N10 C15 171.3(3) . . . . ?
C12 C11 N10 Fe1 178.7(2) . . . . ?
C40 C11 N10 Fe1 -4.6(4) . . . . ?
C32 C31 N30 C35 -3.2(5) . . . . ?
C32 C31 N30 Fe1 -179.1(3) . . . . ?
C34 C35 N30 C31 4.1(5) . . . . ?
C16 C35 N30 C31 -173.9(3) . . . . ?
C34 C35 N30 Fe1 179.9(3) . . . . ?
C16 C35 N30 Fe1 2.0(4) . . . . ?
C24 C25 N20 C21 -2.5(5) . . . . ?
C16 C25 N20 C21 176.2(3) . . . . ?
C24 C25 N20 Fe1 174.0(3) . . . . ?
C16 C25 N20 Fe1 -7.3(4) . . . . ?
C22 C21 N20 C25 1.0(5) . . . . ?
C22 C21 N20 Fe1 -175.5(3) . . . . ?
C11 C40 N41 C42 166.7(3) . . . . ?
C11 C40 N41 C43 -76.4(3) . . . . ?
C11 C40 N41 Fe1 45.1(3) . . . . ?
C15 N10 Fe1 N30 -49.5(3) . . . . ?
C11 N10 Fe1 N30 126.2(2) . . . . ?
C15 N10 Fe1 N20 34.2(3) . . . . ?
C11 N10 Fe1 N20 -150.1(2) . . . . ?
C15 N10 Fe1 N60 121.6(3) . . . . ?
C11 N10 Fe1 N60 -62.8(2) . . . . ?
C15 N10 Fe1 N41 -150.6(3) . . . . ?
C11 N10 Fe1 N41 25.1(2) . . . . ?
C31 N30 Fe1 N10 -140.8(3) . . . . ?
C35 N30 Fe1 N10 43.5(3) . . . . ?
C31 N30 Fe1 N50 33.2(3) . . . . ?
C35 N30 Fe1 N50 -142.6(3) . . . . ?
C31 N30 Fe1 N20 127.2(3) . . . . ?
C35 N30 Fe1 N20 -48.6(3) . . . . ?
C31 N30 Fe1 N41 -62.2(3) . . . . ?
C35 N30 Fe1 N41 122.0(3) . . . . ?
C25 N20 Fe1 N10 -33.9(3) . . . . ?
C21 N20 Fe1 N10 142.5(3) . . . . ?
C25 N20 Fe1 N50 143.9(3) . . . . ?
C21 N20 Fe1 N50 -39.6(3) . . . . ?
C25 N20 Fe1 N30 52.1(3) . . . . ?
C21 N20 Fe1 N30 -131.4(3) . . . . ?
C25 N20 Fe1 N60 -127.2(3) . . . . ?
C21 N20 Fe1 N60 49.3(3) . . . . ?
C25 N20 Fe1 N41 -61.8(8) . . . . ?
C21 N20 Fe1 N41 114.7(6) . . . . ?
C61 N60 Fe1 N10 -104.5(9) . . . . ?
C61 N60 Fe1 N50 81.2(9) . . . . ?
C61 N60 Fe1 N20 -13.0(8) . . . . ?
C61 N60 Fe1 N41 176.2(9) . . . . ?
C40 N41 Fe1 N10 -38.2(2) . . . . ?
C42 N41 Fe1 N10 -155.3(3) . . . . ?
C43 N41 Fe1 N10 78.7(2) . . . . ?
C40 N41 Fe1 N50 144.5(2) . . . . ?
C42 N41 Fe1 N50 27.4(3) . . . . ?
C43 N41 Fe1 N50 -98.7(2) . . . . ?
C40 N41 Fe1 N30 -122.4(2) . . . . ?
C42 N41 Fe1 N30 120.5(3) . . . . ?
C43 N41 Fe1 N30 -5.5(3) . . . . ?
C40 N41 Fe1 N20 -9.8(8) . . . . ?
C42 N41 Fe1 N20 -126.9(6) . . . . ?
C43 N41 Fe1 N20 107.0(7) . . . . ?
C40 N41 Fe1 N60 55.5(2) . . . . ?
C42 N41 Fe1 N60 -61.6(3) . . . . ?
C43 N41 Fe1 N60 172.4(2) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_database_code_depnum_ccdc_archive 'CCDC 960953'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound1b-273K

_audit_creation_date             2013-09-13T18:41:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;(1-{6-[1,1-di(pyridin-2-yl)ethyl]pyridin-2-yl}-N,N-
dimethylmethanamine)bis(thiocyanato-\kN)iron(II)--chloroform(1/2)
;
_chemical_formula_iupac          '[Fe (C20 H22 N4) (N C S)2].2C H Cl3'
_chemical_formula_moiety         'C22 H22 Fe N6 S2, 2(C H Cl3)'
_chemical_formula_sum            'C24 H24 Cl6 Fe N6 S2'
_chemical_formula_weight         729.16

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.8495(12)
_cell_length_b                   15.7047(11)
_cell_length_c                   14.7310(14)
_cell_angle_alpha                90
_cell_angle_beta                 91.087(8)
_cell_angle_gamma                90
_cell_volume                     3203.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    273.00(14)
_cell_measurement_reflns_used    1444
_cell_measurement_theta_min      3.2927
_cell_measurement_theta_max      32.5343

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1480
_exptl_crystal_recrystallization_method 
'precipitation: chloroform, diethyl ether, vapour diffusion, r. t., 2 weeks'

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.8832
_exptl_absorpt_correction_T_max  1

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_ambient_temperature      273.00(14)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent Sapphire 3'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_standards_number         0
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_unetI/netI     0.115
_diffrn_reflns_number            13334
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.3
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_reflns_number_total             5553
_reflns_number_gt                3285
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
 The chloroform moiety centered at C5 exhibits positional disorder. It has
 been modeled in two discrete positions using SAME as well as tight DELU and
 ISOR restraints. The s.o.f. refined to 0.46(3) and 0.54(3), respectively.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0442P)²+1.9887P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5553
_refine_ls_number_parameters     392
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.149
_refine_ls_R_factor_gt           0.0824
_refine_ls_wR_factor_ref         0.1686
_refine_ls_wR_factor_gt          0.1402
_refine_ls_goodness_of_fit_ref   1.09
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.069


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.0801(4) 0.5453(3) 0.3521(4) 0.0379(15) Uani 1 1 d . . .
C12 C 0.0047(4) 0.5975(3) 0.3726(5) 0.0411(16) Uani 1 1 d . . .
H12 H -0.0411 0.6127 0.3285 0.049 Uiso 1 1 calc R . .
C13 C -0.0018(4) 0.6268(4) 0.4598(5) 0.0476(17) Uani 1 1 d . . .
H13 H -0.0543 0.6599 0.476 0.057 Uiso 1 1 calc R . .
C14 C 0.0687(4) 0.6077(3) 0.5234(4) 0.0409(15) Uani 1 1 d . . .
H14 H 0.0653 0.6293 0.582 0.049 Uiso 1 1 calc R . .
C15 C 0.1451(4) 0.5558(3) 0.4991(4) 0.0327(13) Uani 1 1 d . . .
C16 C 0.2339(4) 0.5378(3) 0.5595(4) 0.0361(14) Uani 1 1 d . . .
C17 C 0.2249(5) 0.5855(4) 0.6497(4) 0.0582(19) Uani 1 1 d . . .
H17A H 0.2821 0.5762 0.6863 0.087 Uiso 1 1 calc R . .
H17B H 0.1696 0.5649 0.6813 0.087 Uiso 1 1 calc R . .
H17C H 0.2175 0.6453 0.638 0.087 Uiso 1 1 calc R . .
C21 C 0.2723(4) 0.3096(4) 0.5142(5) 0.0489(17) Uani 1 1 d . . .
H21 H 0.2816 0.2761 0.4631 0.059 Uiso 1 1 calc R . .
C22 C 0.2750(4) 0.2716(4) 0.5969(6) 0.060(2) Uani 1 1 d . . .
H22 H 0.2871 0.2135 0.6016 0.072 Uiso 1 1 calc R . .
C23 C 0.2601(4) 0.3185(5) 0.6730(6) 0.062(2) Uani 1 1 d . . .
H23 H 0.2602 0.2932 0.7301 0.074 Uiso 1 1 calc R . .
C24 C 0.2446(4) 0.4066(4) 0.6626(5) 0.0534(18) Uani 1 1 d . . .
H24 H 0.234 0.4409 0.7129 0.064 Uiso 1 1 calc R . .
C25 C 0.2452(4) 0.4411(4) 0.5766(4) 0.0376(15) Uani 1 1 d . . .
C31 C 0.4229(4) 0.5497(4) 0.3860(5) 0.0489(17) Uani 1 1 d . . .
H31 H 0.4362 0.522 0.3319 0.059 Uiso 1 1 calc R . .
C32 C 0.4887(4) 0.6096(4) 0.4185(6) 0.0544(19) Uani 1 1 d . . .
H32 H 0.5442 0.6224 0.3867 0.065 Uiso 1 1 calc R . .
C33 C 0.4691(5) 0.6489(4) 0.4984(6) 0.056(2) Uani 1 1 d . . .
H33 H 0.5109 0.6902 0.5218 0.068 Uiso 1 1 calc R . .
C34 C 0.3868(4) 0.6272(4) 0.5444(5) 0.0474(17) Uani 1 1 d . . .
H34 H 0.3737 0.6531 0.5996 0.057 Uiso 1 1 calc R . .
C35 C 0.3240(4) 0.5670(3) 0.5088(4) 0.0371(15) Uani 1 1 d . . .
C40 C 0.0997(4) 0.5119(4) 0.2589(5) 0.0511(18) Uani 1 1 d . . .
H40A H 0.0678 0.4575 0.2504 0.061 Uiso 1 1 calc R . .
H40B H 0.0741 0.5512 0.2136 0.061 Uiso 1 1 calc R . .
C42 C 0.2229(6) 0.4508(5) 0.1647(5) 0.086(3) Uani 1 1 d . . .
H42A H 0.1926 0.3961 0.1699 0.13 Uiso 1 1 calc R . .
H42B H 0.2913 0.4434 0.1585 0.13 Uiso 1 1 calc R . .
H42C H 0.1972 0.4799 0.1123 0.13 Uiso 1 1 calc R . .
C43 C 0.2471(5) 0.5879(4) 0.2332(5) 0.064(2) Uani 1 1 d . . .
H43A H 0.2178 0.6138 0.1804 0.097 Uiso 1 1 calc R . .
H43B H 0.3153 0.5822 0.2245 0.097 Uiso 1 1 calc R . .
H43C H 0.2359 0.6228 0.2854 0.097 Uiso 1 1 calc R . .
C51 C 0.4168(5) 0.3359(4) 0.2884(5) 0.0519(19) Uani 1 1 d . . .
C61 C 0.1105(4) 0.2825(4) 0.3518(5) 0.0508(18) Uani 1 1 d . . .
N10 N 0.1471(3) 0.5219(3) 0.4154(4) 0.0345(12) Uani 1 1 d . . .
N20 N 0.2569(3) 0.3928(3) 0.5027(4) 0.0378(12) Uani 1 1 d . . .
N30 N 0.3417(3) 0.5298(3) 0.4283(4) 0.0389(12) Uani 1 1 d . . .
N41 N 0.2039(4) 0.5019(3) 0.2475(4) 0.0555(15) Uani 1 1 d . . .
N50 N 0.3564(4) 0.3732(3) 0.3204(4) 0.0581(17) Uani 1 1 d . . .
N60 N 0.1528(4) 0.3444(4) 0.3449(4) 0.0545(15) Uani 1 1 d . . .
S52 S 0.50439(14) 0.28252(12) 0.24217(15) 0.0727(6) Uani 1 1 d . . .
S62 S 0.05039(16) 0.19393(13) 0.36518(17) 0.0866(7) Uani 1 1 d . . .
Fe1 Fe 0.24910(6) 0.44020(5) 0.37375(7) 0.0399(3) Uani 1 1 d . . .
C1 C 0.1105(7) 0.8424(6) 0.4260(7) 0.113(3) Uani 1 1 d . . .
H1 H 0.0694 0.8215 0.4747 0.136 Uiso 1 1 calc R . .
Cl2 Cl 0.0635(2) 0.80648(15) 0.3225(2) 0.1265(10) Uani 1 1 d . . .
Cl3 Cl 0.1066(3) 0.9527(2) 0.4254(3) 0.1834(17) Uani 1 1 d . . .
Cl4 Cl 0.2239(3) 0.8055(3) 0.4441(4) 0.217(2) Uani 1 1 d . . .
C5A C 0.5489(14) 0.5994(13) 0.1337(15) 0.094(7) Uani 0.46(2) 1 d PDU A 1
H5A H 0.5457 0.64 0.1842 0.112 Uiso 0.46(2) 1 calc PR A 1
Cl6A Cl 0.6604(14) 0.6064(10) 0.0732(14) 0.136(5) Uani 0.46(2) 1 d PDU A 1
Cl7A Cl 0.4556(13) 0.6118(6) 0.0562(7) 0.113(4) Uani 0.46(2) 1 d PDU A 1
Cl8A Cl 0.5587(12) 0.4904(7) 0.1714(10) 0.092(4) Uani 0.46(2) 1 d PDU A 1
C5B C 0.5781(13) 0.5989(12) 0.1218(12) 0.089(5) Uani 0.54(2) 1 d PDU A 2
H5B H 0.5645 0.6451 0.1644 0.107 Uiso 0.54(2) 1 calc PR A 2
Cl6B Cl 0.7042(10) 0.6012(8) 0.0958(7) 0.102(3) Uani 0.54(2) 1 d PDU A 2
Cl7B Cl 0.5183(16) 0.6193(5) 0.0208(11) 0.144(6) Uani 0.54(2) 1 d PDU A 2
Cl8B Cl 0.5432(12) 0.4999(10) 0.1721(9) 0.109(4) Uani 0.54(2) 1 d PDU A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C11 N10 1.354(7) . ?
C11 C12 1.365(7) . ?
C11 C40 1.499(8) . ?
C12 C13 1.369(8) . ?
C13 C14 1.374(8) . ?
C14 C15 1.388(7) . ?
C15 N10 1.343(7) . ?
C15 C16 1.531(8) . ?
C16 C17 1.532(8) . ?
C16 C35 1.537(8) . ?
C16 C25 1.547(7) . ?
C21 N20 1.335(7) . ?
C21 C22 1.356(9) . ?
C22 C23 1.360(10) . ?
C23 C24 1.407(9) . ?
C24 C25 1.379(8) . ?
C25 N20 1.338(7) . ?
C31 N30 1.334(7) . ?
C31 C32 1.388(8) . ?
C32 C33 1.361(9) . ?
C33 C34 1.380(8) . ?
C34 C35 1.381(7) . ?
C35 N30 1.348(7) . ?
C40 N41 1.465(7) . ?
C42 N41 1.487(8) . ?
C43 N41 1.493(7) . ?
C51 N50 1.132(8) . ?
C51 S52 1.634(8) . ?
C61 N60 1.141(7) . ?
C61 S62 1.634(7) . ?
N10 Fe1 2.013(4) . ?
N20 Fe1 2.041(5) . ?
N30 Fe1 2.057(5) . ?
N41 Fe1 2.179(6) . ?
N50 Fe1 1.994(6) . ?
N60 Fe1 2.050(6) . ?
C1 Cl4 1.691(9) . ?
C1 Cl3 1.734(9) . ?
C1 Cl2 1.740(10) . ?
C5A Cl7A 1.719(16) . ?
C5A Cl6A 1.801(16) . ?
C5A Cl8A 1.804(15) . ?
C5B Cl7B 1.719(14) . ?
C5B Cl8B 1.792(14) . ?
C5B Cl6B 1.796(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N10 C11 C12 121.8(6) . . ?
N10 C11 C40 113.7(5) . . ?
C12 C11 C40 124.4(6) . . ?
C11 C12 C13 118.3(6) . . ?
C12 C13 C14 120.6(6) . . ?
C13 C14 C15 119.2(6) . . ?
N10 C15 C14 119.9(5) . . ?
N10 C15 C16 115.5(5) . . ?
C14 C15 C16 124.5(5) . . ?
C17 C16 C15 109.7(5) . . ?
C17 C16 C35 110.8(5) . . ?
C15 C16 C35 108.2(5) . . ?
C17 C16 C25 110.4(5) . . ?
C15 C16 C25 110.7(5) . . ?
C35 C16 C25 106.9(4) . . ?
N20 C21 C22 123.1(7) . . ?
C21 C22 C23 120.0(6) . . ?
C22 C23 C24 117.9(7) . . ?
C25 C24 C23 118.9(7) . . ?
N20 C25 C24 121.9(5) . . ?
N20 C25 C16 116.0(5) . . ?
C24 C25 C16 122.2(6) . . ?
N30 C31 C32 123.5(7) . . ?
C33 C32 C31 117.7(6) . . ?
C32 C33 C34 119.5(6) . . ?
C33 C34 C35 120.2(6) . . ?
N30 C35 C34 120.5(6) . . ?
N30 C35 C16 117.4(5) . . ?
C34 C35 C16 122.1(6) . . ?
N41 C40 C11 109.8(5) . . ?
N50 C51 S52 179.7(7) . . ?
N60 C61 S62 178.2(7) . . ?
C15 N10 C11 119.9(5) . . ?
C15 N10 Fe1 124.0(4) . . ?
C11 N10 Fe1 116.0(4) . . ?
C21 N20 C25 118.2(6) . . ?
C21 N20 Fe1 118.7(5) . . ?
C25 N20 Fe1 123.0(4) . . ?
C31 N30 C35 118.5(5) . . ?
C31 N30 Fe1 120.2(4) . . ?
C35 N30 Fe1 121.2(4) . . ?
C40 N41 C42 110.0(6) . . ?
C40 N41 C43 108.5(5) . . ?
C42 N41 C43 107.1(6) . . ?
C40 N41 Fe1 102.6(4) . . ?
C42 N41 Fe1 114.1(4) . . ?
C43 N41 Fe1 114.4(4) . . ?
C51 N50 Fe1 178.6(6) . . ?
C61 N60 Fe1 160.1(6) . . ?
N50 Fe1 N10 171.5(2) . . ?
N50 Fe1 N20 98.5(2) . . ?
N10 Fe1 N20 88.50(19) . . ?
N50 Fe1 N60 91.0(2) . . ?
N10 Fe1 N60 94.22(19) . . ?
N20 Fe1 N60 87.0(2) . . ?
N50 Fe1 N30 92.94(19) . . ?
N10 Fe1 N30 83.14(17) . . ?
N20 Fe1 N30 82.17(19) . . ?
N60 Fe1 N30 168.9(2) . . ?
N50 Fe1 N41 95.9(2) . . ?
N10 Fe1 N41 77.6(2) . . ?
N20 Fe1 N41 165.02(19) . . ?
N60 Fe1 N41 88.5(2) . . ?
N30 Fe1 N41 101.3(2) . . ?
Cl4 C1 Cl3 111.8(5) . . ?
Cl4 C1 Cl2 111.0(6) . . ?
Cl3 C1 Cl2 108.0(6) . . ?
Cl7A C5A Cl6A 107.7(12) . . ?
Cl7A C5A Cl8A 111.3(12) . . ?
Cl6A C5A Cl8A 98.6(11) . . ?
Cl7B C5B Cl8B 113.0(11) . . ?
Cl7B C5B Cl6B 105.4(9) . . ?
Cl8B C5B Cl6B 112.1(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N10 C11 C12 C13 0.5(8) . . . . ?
C40 C11 C12 C13 -176.7(6) . . . . ?
C11 C12 C13 C14 3.4(9) . . . . ?
C12 C13 C14 C15 -2.2(9) . . . . ?
C13 C14 C15 N10 -2.9(8) . . . . ?
C13 C14 C15 C16 172.7(5) . . . . ?
N10 C15 C16 C17 175.8(5) . . . . ?
C14 C15 C16 C17 0.0(8) . . . . ?
N10 C15 C16 C35 54.8(6) . . . . ?
C14 C15 C16 C35 -121.0(6) . . . . ?
N10 C15 C16 C25 -62.1(6) . . . . ?
C14 C15 C16 C25 122.1(6) . . . . ?
N20 C21 C22 C23 1.1(9) . . . . ?
C21 C22 C23 C24 -1.5(9) . . . . ?
C22 C23 C24 C25 -0.1(9) . . . . ?
C23 C24 C25 N20 2.4(8) . . . . ?
C23 C24 C25 C16 -176.8(5) . . . . ?
C17 C16 C25 N20 -177.9(5) . . . . ?
C15 C16 C25 N20 60.4(6) . . . . ?
C35 C16 C25 N20 -57.3(6) . . . . ?
C17 C16 C25 C24 1.3(7) . . . . ?
C15 C16 C25 C24 -120.3(6) . . . . ?
C35 C16 C25 C24 122.0(6) . . . . ?
N30 C31 C32 C33 0.9(9) . . . . ?
C31 C32 C33 C34 1.1(9) . . . . ?
C32 C33 C34 C35 -1.1(9) . . . . ?
C33 C34 C35 N30 -0.9(9) . . . . ?
C33 C34 C35 C16 177.3(5) . . . . ?
C17 C16 C35 N30 179.5(5) . . . . ?
C15 C16 C35 N30 -60.2(6) . . . . ?
C25 C16 C35 N30 59.1(6) . . . . ?
C17 C16 C35 C34 1.3(7) . . . . ?
C15 C16 C35 C34 121.6(6) . . . . ?
C25 C16 C35 C34 -119.1(6) . . . . ?
N10 C11 C40 N41 -29.4(7) . . . . ?
C12 C11 C40 N41 148.0(5) . . . . ?
C14 C15 N10 C11 6.7(7) . . . . ?
C16 C15 N10 C11 -169.3(5) . . . . ?
C14 C15 N10 Fe1 -176.2(4) . . . . ?
C16 C15 N10 Fe1 7.8(6) . . . . ?
C12 C11 N10 C15 -5.6(8) . . . . ?
C40 C11 N10 C15 171.8(5) . . . . ?
C12 C11 N10 Fe1 177.1(4) . . . . ?
C40 C11 N10 Fe1 -5.4(6) . . . . ?
C22 C21 N20 C25 1.2(8) . . . . ?
C22 C21 N20 Fe1 -177.4(4) . . . . ?
C24 C25 N20 C21 -2.9(8) . . . . ?
C16 C25 N20 C21 176.4(4) . . . . ?
C24 C25 N20 Fe1 175.7(4) . . . . ?
C16 C25 N20 Fe1 -5.1(6) . . . . ?
C32 C31 N30 C35 -2.9(9) . . . . ?
C32 C31 N30 Fe1 179.8(4) . . . . ?
C34 C35 N30 C31 2.8(8) . . . . ?
C16 C35 N30 C31 -175.4(5) . . . . ?
C34 C35 N30 Fe1 -179.9(4) . . . . ?
C16 C35 N30 Fe1 1.9(7) . . . . ?
C11 C40 N41 C42 167.0(5) . . . . ?
C11 C40 N41 C43 -76.1(6) . . . . ?
C11 C40 N41 Fe1 45.3(5) . . . . ?
C15 N10 Fe1 N20 33.2(4) . . . . ?
C11 N10 Fe1 N20 -149.6(4) . . . . ?
C15 N10 Fe1 N60 120.1(4) . . . . ?
C11 N10 Fe1 N60 -62.7(4) . . . . ?
C15 N10 Fe1 N30 -49.1(4) . . . . ?
C11 N10 Fe1 N30 128.1(4) . . . . ?
C15 N10 Fe1 N41 -152.4(4) . . . . ?
C11 N10 Fe1 N41 24.8(4) . . . . ?
C21 N20 Fe1 N50 -40.8(4) . . . . ?
C25 N20 Fe1 N50 140.6(4) . . . . ?
C21 N20 Fe1 N10 144.1(4) . . . . ?
C25 N20 Fe1 N10 -34.5(4) . . . . ?
C21 N20 Fe1 N60 49.8(4) . . . . ?
C25 N20 Fe1 N60 -128.8(4) . . . . ?
C21 N20 Fe1 N30 -132.6(4) . . . . ?
C25 N20 Fe1 N30 48.8(4) . . . . ?
C21 N20 Fe1 N41 122.6(7) . . . . ?
C25 N20 Fe1 N41 -55.9(9) . . . . ?
C61 N60 Fe1 N50 82.6(16) . . . . ?
C61 N60 Fe1 N10 -104.1(16) . . . . ?
C61 N60 Fe1 N20 -15.9(16) . . . . ?
C61 N60 Fe1 N30 -28(2) . . . . ?
C61 N60 Fe1 N41 178.5(16) . . . . ?
C31 N30 Fe1 N50 32.5(5) . . . . ?
C35 N30 Fe1 N50 -144.7(4) . . . . ?
C31 N30 Fe1 N10 -139.8(4) . . . . ?
C35 N30 Fe1 N10 42.9(4) . . . . ?
C31 N30 Fe1 N20 130.7(4) . . . . ?
C35 N30 Fe1 N20 -46.6(4) . . . . ?
C31 N30 Fe1 N60 143.4(9) . . . . ?
C35 N30 Fe1 N60 -33.9(12) . . . . ?
C31 N30 Fe1 N41 -64.0(4) . . . . ?
C35 N30 Fe1 N41 118.7(4) . . . . ?
C40 N41 Fe1 N50 148.0(4) . . . . ?
C42 N41 Fe1 N50 29.0(5) . . . . ?
C43 N41 Fe1 N50 -94.8(4) . . . . ?
C40 N41 Fe1 N10 -37.6(3) . . . . ?
C42 N41 Fe1 N10 -156.5(5) . . . . ?
C43 N41 Fe1 N10 79.7(4) . . . . ?
C40 N41 Fe1 N20 -15.6(9) . . . . ?
C42 N41 Fe1 N20 -134.6(7) . . . . ?
C43 N41 Fe1 N20 101.6(8) . . . . ?
C40 N41 Fe1 N60 57.1(4) . . . . ?
C42 N41 Fe1 N60 -61.9(5) . . . . ?
C43 N41 Fe1 N60 174.3(4) . . . . ?
C40 N41 Fe1 N30 -117.8(4) . . . . ?
C42 N41 Fe1 N30 123.2(5) . . . . ?
C43 N41 Fe1 N30 -0.6(4) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_database_code_depnum_ccdc_archive 'CCDC 960954'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound2

_audit_creation_date             2013-09-13T18:26:04-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;dichlorido(1-{6-[1,1-di(pyridin-2-yl)ethyl]pyridin-2-yl}-
        N,N-dimethylmethanamine)iron(II)--methanol(1/1)
;
_chemical_formula_iupac          '[Fe (C20 H22 N4) Cl2].C H3 O H'
_chemical_formula_moiety         'C20 H22 Cl2 Fe N4, C H4 O'
_chemical_formula_sum            'C21 H26 Cl2 Fe N4 O'
_chemical_formula_weight         477.21

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.8322(7)
_cell_length_b                   14.7903(7)
_cell_length_c                   15.1031(12)
_cell_angle_alpha                90
_cell_angle_beta                 93.936(8)
_cell_angle_gamma                90
_cell_volume                     2191.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    4771
_cell_measurement_theta_min      3.288
_cell_measurement_theta_max      32.5497

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            'light red'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_crystal_recrystallization_method 
'precipitation (vapour diffusion): methanol, diethyl ether, r. t., 2 weeks'

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.29154
_exptl_absorpt_correction_T_max  1

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent Sapphire 3'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_standards_number         0
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_number            9403
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.29
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_full        26
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             4295
_reflns_number_gt                3400
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
;
_computing_cell_refinement       
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction        
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
        (compiled Apr 28 2010,14:27:37)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0552P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4295
_refine_ls_number_parameters     267
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.0975
_refine_ls_wR_factor_gt          0.0949
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.996
_refine_diff_density_min         -0.74
_refine_diff_density_rms         0.068

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.8134(3) 0.89822(16) -0.04540(15) 0.0234(5) Uani 1 1 d . . .
C12 C 0.8345(3) 0.97140(17) -0.10032(17) 0.0293(6) Uani 1 1 d . . .
H12 H 0.8447 0.9629 -0.1619 0.035 Uiso 1 1 calc R . .
C13 C 0.8404(3) 1.05640(17) -0.06367(17) 0.0315(6) Uani 1 1 d . . .
H13 H 0.8592 1.1072 -0.0993 0.038 Uiso 1 1 calc R . .
C14 C 0.8190(3) 1.06799(16) 0.02535(17) 0.0276(6) Uani 1 1 d . . .
H14 H 0.8191 1.1269 0.0505 0.033 Uiso 1 1 calc R . .
C15 C 0.7972(2) 0.99222(15) 0.07788(16) 0.0205(5) Uani 1 1 d . . .
C16 C 0.7670(3) 0.99841(15) 0.17656(15) 0.0213(5) Uani 1 1 d . . .
C17 C 0.7552(3) 1.09906(15) 0.20267(18) 0.0308(6) Uani 1 1 d . . .
H17A H 0.7362 1.1035 0.2654 0.046 Uiso 1 1 calc R . .
H17B H 0.6809 1.1274 0.166 0.046 Uiso 1 1 calc R . .
H17C H 0.8411 1.1301 0.1932 0.046 Uiso 1 1 calc R . .
C21 C 0.9978(3) 0.82003(16) 0.27342(16) 0.0246(5) Uani 1 1 d . . .
H21 H 1.0129 0.7577 0.2627 0.03 Uiso 1 1 calc R . .
C22 C 1.0745(3) 0.86146(17) 0.34229(17) 0.0289(6) Uani 1 1 d . . .
H22 H 1.1396 0.8283 0.3787 0.035 Uiso 1 1 calc R . .
C23 C 1.0533(3) 0.95277(17) 0.35638(17) 0.0300(6) Uani 1 1 d . . .
H23 H 1.1046 0.9837 0.4026 0.036 Uiso 1 1 calc R . .
C24 C 0.9570(3) 0.99856(17) 0.30269(16) 0.0254(5) Uani 1 1 d . . .
H24 H 0.9425 1.0614 0.3113 0.03 Uiso 1 1 calc R . .
C25 C 0.8813(2) 0.95245(14) 0.23603(15) 0.0193(5) Uani 1 1 d . . .
C31 C 0.5072(3) 0.81526(16) 0.18408(17) 0.0249(6) Uani 1 1 d . . .
H31 H 0.4996 0.754 0.1654 0.03 Uiso 1 1 calc R . .
C32 C 0.4009(3) 0.85279(17) 0.22548(18) 0.0291(6) Uani 1 1 d . . .
H32 H 0.3224 0.8181 0.2362 0.035 Uiso 1 1 calc R . .
C33 C 0.4112(3) 0.94295(17) 0.25142(17) 0.0304(6) Uani 1 1 d . . .
H33 H 0.3398 0.9711 0.2806 0.036 Uiso 1 1 calc R . .
C34 C 0.5260(3) 0.99045(17) 0.23408(16) 0.0266(6) Uani 1 1 d . . .
H34 H 0.5336 1.0524 0.2504 0.032 Uiso 1 1 calc R . .
C35 C 0.6314(2) 0.94878(14) 0.19288(15) 0.0192(5) Uani 1 1 d . . .
C40 C 0.8015(3) 0.80251(16) -0.07918(16) 0.0285(6) Uani 1 1 d . . .
H40A H 0.7648 0.8027 -0.1419 0.034 Uiso 1 1 calc R . .
H40B H 0.8929 0.7741 -0.0765 0.034 Uiso 1 1 calc R . .
C42 C 0.5678(3) 0.77984(18) -0.04405(18) 0.0355(7) Uani 1 1 d . . .
H42A H 0.5416 0.7711 -0.1072 0.053 Uiso 1 1 calc R . .
H42B H 0.56 0.844 -0.029 0.053 Uiso 1 1 calc R . .
H42C H 0.5075 0.7443 -0.0085 0.053 Uiso 1 1 calc R . .
C43 C 0.7203(3) 0.65314(16) -0.04806(17) 0.0339(7) Uani 1 1 d . . .
H43A H 0.6577 0.6181 -0.0137 0.051 Uiso 1 1 calc R . .
H43B H 0.8139 0.6321 -0.0342 0.051 Uiso 1 1 calc R . .
H43C H 0.696 0.6451 -0.1116 0.051 Uiso 1 1 calc R . .
N10 N 0.8003(2) 0.90896(12) 0.04231(12) 0.0193(4) Uani 1 1 d . . .
N20 N 0.9032(2) 0.86357(12) 0.22096(12) 0.0189(4) Uani 1 1 d . . .
N30 N 0.6214(2) 0.86065(12) 0.16853(13) 0.0200(4) Uani 1 1 d . . .
N41 N 0.7104(2) 0.74985(13) -0.02496(13) 0.0240(5) Uani 1 1 d . . .
Cl1 Cl 0.73196(7) 0.64711(4) 0.18216(4) 0.02641(16) Uani 1 1 d . . .
Cl2 Cl 1.02399(7) 0.72141(4) 0.07670(4) 0.03062(16) Uani 1 1 d . . .
Fe1 Fe 0.79341(3) 0.78361(2) 0.11666(2) 0.01687(11) Uani 1 1 d . . .
O1 O 0.3271(3) 0.66676(16) 0.0759(2) 0.0854(10) Uani 1 1 d . . .
H1 H 0.2824 0.7001 0.0394 0.128 Uiso 1 1 calc R . .
C2 C 0.3390(3) 0.58152(19) 0.0401(2) 0.0445(8) Uani 1 1 d . . .
H2A H 0.4221 0.5526 0.066 0.067 Uiso 1 1 calc R . .
H2B H 0.3438 0.5864 -0.0243 0.067 Uiso 1 1 calc R . .
H2C H 0.2596 0.5451 0.0532 0.067 Uiso 1 1 calc R . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C11 N10 1.349(3) . ?
C11 C12 1.388(3) . ?
C11 C40 1.507(3) . ?
C12 C13 1.373(4) . ?
C13 C14 1.386(4) . ?
C14 C15 1.398(3) . ?
C15 N10 1.345(3) . ?
C15 C16 1.542(3) . ?
C16 C17 1.546(3) . ?
C16 C25 1.547(3) . ?
C16 C35 1.557(3) . ?
C21 N20 1.344(3) . ?
C21 C22 1.385(3) . ?
C22 C23 1.385(4) . ?
C23 C24 1.381(4) . ?
C24 C25 1.389(3) . ?
C25 N20 1.354(3) . ?
C31 N30 1.343(3) . ?
C31 C32 1.371(4) . ?
C32 C33 1.392(4) . ?
C33 C34 1.370(4) . ?
C34 C35 1.389(3) . ?
C35 N30 1.356(3) . ?
C40 N41 1.477(3) . ?
C42 N41 1.480(3) . ?
C43 N41 1.477(3) . ?
N10 Fe1 2.1710(18) . ?
N20 Fe1 2.1935(19) . ?
N30 Fe1 2.226(2) . ?
N41 Fe1 2.2913(19) . ?
Cl1 Fe1 2.3455(6) . ?
Cl2 Fe1 2.5570(7) . ?
O1 C2 1.380(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N10 C11 C12 121.6(2) . . ?
N10 C11 C40 115.6(2) . . ?
C12 C11 C40 122.8(2) . . ?
C13 C12 C11 118.5(2) . . ?
C12 C13 C14 120.0(2) . . ?
C13 C14 C15 119.4(2) . . ?
N10 C15 C14 119.9(2) . . ?
N10 C15 C16 116.84(19) . . ?
C14 C15 C16 123.2(2) . . ?
C15 C16 C17 109.05(19) . . ?
C15 C16 C25 110.8(2) . . ?
C17 C16 C25 109.84(18) . . ?
C15 C16 C35 110.41(18) . . ?
C17 C16 C35 109.5(2) . . ?
C25 C16 C35 107.26(18) . . ?
N20 C21 C22 123.4(2) . . ?
C21 C22 C23 117.8(2) . . ?
C24 C23 C22 119.5(2) . . ?
C23 C24 C25 119.8(2) . . ?
N20 C25 C24 121.0(2) . . ?
N20 C25 C16 116.53(19) . . ?
C24 C25 C16 122.5(2) . . ?
N30 C31 C32 123.4(2) . . ?
C31 C32 C33 118.3(2) . . ?
C34 C33 C32 118.8(3) . . ?
C33 C34 C35 120.5(2) . . ?
N30 C35 C34 120.4(2) . . ?
N30 C35 C16 117.2(2) . . ?
C34 C35 C16 122.4(2) . . ?
N41 C40 C11 110.1(2) . . ?
C15 N10 C11 120.4(2) . . ?
C15 N10 Fe1 124.96(16) . . ?
C11 N10 Fe1 114.57(15) . . ?
C21 N20 C25 118.5(2) . . ?
C21 N20 Fe1 116.85(15) . . ?
C25 N20 Fe1 124.62(15) . . ?
C31 N30 C35 118.6(2) . . ?
C31 N30 Fe1 118.07(15) . . ?
C35 N30 Fe1 123.02(16) . . ?
C40 N41 C43 109.1(2) . . ?
C40 N41 C42 109.7(2) . . ?
C43 N41 C42 108.7(2) . . ?
C40 N41 Fe1 102.25(14) . . ?
C43 N41 Fe1 113.98(15) . . ?
C42 N41 Fe1 112.86(15) . . ?
N10 Fe1 N20 83.10(7) . . ?
N10 Fe1 N30 78.24(7) . . ?
N20 Fe1 N30 79.61(7) . . ?
N10 Fe1 N41 74.03(7) . . ?
N20 Fe1 N41 156.06(7) . . ?
N30 Fe1 N41 102.10(7) . . ?
N10 Fe1 Cl1 166.23(6) . . ?
N20 Fe1 Cl1 106.83(5) . . ?
N30 Fe1 Cl1 93.91(5) . . ?
N41 Fe1 Cl1 96.93(5) . . ?
N10 Fe1 Cl2 97.22(6) . . ?
N20 Fe1 Cl2 87.88(6) . . ?
N30 Fe1 Cl2 167.08(5) . . ?
N41 Fe1 Cl2 88.05(6) . . ?
Cl1 Fe1 Cl2 92.76(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N10 C11 C12 C13 -0.7(4) . . . . ?
C40 C11 C12 C13 178.3(2) . . . . ?
C11 C12 C13 C14 -3.1(4) . . . . ?
C12 C13 C14 C15 2.7(4) . . . . ?
C13 C14 C15 N10 1.5(4) . . . . ?
C13 C14 C15 C16 -177.6(2) . . . . ?
N10 C15 C16 C17 -175.0(2) . . . . ?
C14 C15 C16 C17 4.1(3) . . . . ?
N10 C15 C16 C25 64.0(3) . . . . ?
C14 C15 C16 C25 -116.9(2) . . . . ?
N10 C15 C16 C35 -54.7(3) . . . . ?
C14 C15 C16 C35 124.4(2) . . . . ?
N20 C21 C22 C23 -1.0(4) . . . . ?
C21 C22 C23 C24 0.6(4) . . . . ?
C22 C23 C24 C25 0.8(4) . . . . ?
C23 C24 C25 N20 -2.0(4) . . . . ?
C23 C24 C25 C16 176.9(2) . . . . ?
C15 C16 C25 N20 -59.7(3) . . . . ?
C17 C16 C25 N20 179.8(2) . . . . ?
C35 C16 C25 N20 60.9(3) . . . . ?
C15 C16 C25 C24 121.3(2) . . . . ?
C17 C16 C25 C24 0.8(3) . . . . ?
C35 C16 C25 C24 -118.1(2) . . . . ?
N30 C31 C32 C33 1.1(4) . . . . ?
C31 C32 C33 C34 0.4(4) . . . . ?
C32 C33 C34 C35 -1.2(4) . . . . ?
C33 C34 C35 N30 0.6(4) . . . . ?
C33 C34 C35 C16 -176.5(2) . . . . ?
C15 C16 C35 N30 56.2(3) . . . . ?
C17 C16 C35 N30 176.3(2) . . . . ?
C25 C16 C35 N30 -64.6(2) . . . . ?
C15 C16 C35 C34 -126.6(2) . . . . ?
C17 C16 C35 C34 -6.5(3) . . . . ?
C25 C16 C35 C34 112.6(2) . . . . ?
N10 C11 C40 N41 29.9(3) . . . . ?
C12 C11 C40 N41 -149.2(2) . . . . ?
C14 C15 N10 C11 -5.3(3) . . . . ?
C16 C15 N10 C11 173.8(2) . . . . ?
C14 C15 N10 Fe1 172.16(17) . . . . ?
C16 C15 N10 Fe1 -8.7(3) . . . . ?
C12 C11 N10 C15 5.0(4) . . . . ?
C40 C11 N10 C15 -174.1(2) . . . . ?
C12 C11 N10 Fe1 -172.72(19) . . . . ?
C40 C11 N10 Fe1 8.1(3) . . . . ?
C22 C21 N20 C25 -0.1(4) . . . . ?
C22 C21 N20 Fe1 -179.6(2) . . . . ?
C24 C25 N20 C21 1.6(4) . . . . ?
C16 C25 N20 C21 -177.4(2) . . . . ?
C24 C25 N20 Fe1 -178.92(18) . . . . ?
C16 C25 N20 Fe1 2.1(3) . . . . ?
C32 C31 N30 C35 -1.7(4) . . . . ?
C32 C31 N30 Fe1 172.1(2) . . . . ?
C34 C35 N30 C31 0.8(3) . . . . ?
C16 C35 N30 C31 178.1(2) . . . . ?
C34 C35 N30 Fe1 -172.68(17) . . . . ?
C16 C35 N30 Fe1 4.6(3) . . . . ?
C11 C40 N41 C43 -169.5(2) . . . . ?
C11 C40 N41 C42 71.5(2) . . . . ?
C11 C40 N41 Fe1 -48.5(2) . . . . ?
C15 N10 Fe1 N20 -32.21(19) . . . . ?
C11 N10 Fe1 N20 145.38(18) . . . . ?
C15 N10 Fe1 N30 48.56(19) . . . . ?
C11 N10 Fe1 N30 -133.85(18) . . . . ?
C15 N10 Fe1 N41 155.0(2) . . . . ?
C11 N10 Fe1 N41 -27.45(17) . . . . ?
C15 N10 Fe1 Cl1 104.7(3) . . . . ?
C11 N10 Fe1 Cl1 -77.7(3) . . . . ?
C15 N10 Fe1 Cl2 -119.17(18) . . . . ?
C11 N10 Fe1 Cl2 58.42(17) . . . . ?
C21 N20 Fe1 N10 -144.75(19) . . . . ?
C25 N20 Fe1 N10 35.76(19) . . . . ?
C21 N20 Fe1 N30 135.99(19) . . . . ?
C25 N20 Fe1 N30 -43.49(19) . . . . ?
C21 N20 Fe1 N41 -127.6(2) . . . . ?
C25 N20 Fe1 N41 52.9(3) . . . . ?
C21 N20 Fe1 Cl1 45.02(18) . . . . ?
C25 N20 Fe1 Cl1 -134.47(18) . . . . ?
C21 N20 Fe1 Cl2 -47.22(17) . . . . ?
C25 N20 Fe1 Cl2 133.29(19) . . . . ?
C31 N30 Fe1 N10 140.78(18) . . . . ?
C35 N30 Fe1 N10 -45.66(17) . . . . ?
C31 N30 Fe1 N20 -134.19(18) . . . . ?
C35 N30 Fe1 N20 39.37(17) . . . . ?
C31 N30 Fe1 N41 70.17(18) . . . . ?
C35 N30 Fe1 N41 -116.27(17) . . . . ?
C31 N30 Fe1 Cl1 -27.78(17) . . . . ?
C35 N30 Fe1 Cl1 145.78(17) . . . . ?
C31 N30 Fe1 Cl2 -148.70(19) . . . . ?
C35 N30 Fe1 Cl2 24.9(4) . . . . ?
C40 N41 Fe1 N10 39.92(15) . . . . ?
C43 N41 Fe1 N10 157.53(19) . . . . ?
C42 N41 Fe1 N10 -77.80(17) . . . . ?
C40 N41 Fe1 N20 22.2(3) . . . . ?
C43 N41 Fe1 N20 139.8(2) . . . . ?
C42 N41 Fe1 N20 -95.6(2) . . . . ?
C40 N41 Fe1 N30 113.78(15) . . . . ?
C43 N41 Fe1 N30 -128.62(18) . . . . ?
C42 N41 Fe1 N30 -3.94(18) . . . . ?
C40 N41 Fe1 Cl1 -150.69(14) . . . . ?
C43 N41 Fe1 Cl1 -33.09(18) . . . . ?
C42 N41 Fe1 Cl1 91.58(16) . . . . ?
C40 N41 Fe1 Cl2 -58.15(14) . . . . ?
C43 N41 Fe1 Cl2 59.45(18) . . . . ?
C42 N41 Fe1 Cl2 -175.87(16) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 Cl2 0.84 2.66 3.088(3) 113.2 1_455

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_database_code_depnum_ccdc_archive 'CCDC 960955'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound1-cd2cl2

_audit_creation_date             2013-09-13T18:37:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;(1-{6-[1,1-di(pyridin-2-yl)ethyl]pyridin-2-yl}-N,N-
dimethylmethanamine)bis(thiocyanato-\kN)iron(II)--[D₂]dichloromethane(1/1)
;
_chemical_formula_iupac          '[Fe (C20 H22 N4) (N C S)2].C D2 Cl2'
_chemical_formula_moiety         'C22 H22 Fe N6 S2, C D2 Cl2'
_chemical_formula_sum            'C23 H22 Cl2 D2 Fe N6 S2'
_chemical_formula_weight         577.36

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.1440(2)
_cell_length_b                   12.7087(4)
_cell_length_c                   22.2852(7)
_cell_angle_alpha                90
_cell_angle_beta                 107.386(3)
_cell_angle_gamma                90
_cell_volume                     2471.41(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    7067
_cell_measurement_theta_min      3.284
_cell_measurement_theta_max      32.4926

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       coloumn
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1184
_exptl_crystal_recrystallization_method 
'evaporation: [D₂]dichloromethane, r. t., 1 week'

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.85378
_exptl_absorpt_correction_T_max  1

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent Sapphire 3'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_standards_number         0
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_number            20548
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.29
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_full        26
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             4855
_reflns_number_gt                4483
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
 Deuterium atoms have been refined as protium atoms and afterwards been
 assigned the right SFAC type.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0314P)²+2.4293P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4855
_refine_ls_number_parameters     310
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.0875
_refine_ls_wR_factor_gt          0.0853
_refine_ls_goodness_of_fit_ref   1.16
_refine_ls_restrained_S_all      1.16
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.063


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.0178(3) 0.8829(2) 0.70182(11) 0.0203(5) Uani 1 1 d . . .
C12 C 0.0765(3) 0.9164(2) 0.65483(12) 0.0251(6) Uani 1 1 d . . .
H12 H 0.0163 0.9134 0.612 0.03 Uiso 1 1 calc R . .
C13 C 0.2262(3) 0.9546(2) 0.67152(12) 0.0238(5) Uani 1 1 d . . .
H13 H 0.2668 0.983 0.6404 0.029 Uiso 1 1 calc R . .
C14 C 0.3154(3) 0.9507(2) 0.73398(11) 0.0200(5) Uani 1 1 d . . .
H14 H 0.4197 0.9722 0.7456 0.024 Uiso 1 1 calc R . .
C15 C 0.2509(2) 0.91511(18) 0.77920(11) 0.0147(5) Uani 1 1 d . . .
C16 C 0.3389(2) 0.90040(18) 0.84904(11) 0.0148(5) Uani 1 1 d . . .
C17 C 0.5088(3) 0.9278(2) 0.86093(12) 0.0210(5) Uani 1 1 d . . .
H17A H 0.553 0.8814 0.8358 0.032 Uiso 1 1 calc R . .
H17B H 0.5638 0.9184 0.9056 0.032 Uiso 1 1 calc R . .
H17C H 0.518 1.0012 0.849 0.032 Uiso 1 1 calc R . .
C21 C 0.0504(3) 1.0092(2) 0.91890(11) 0.0202(5) Uani 1 1 d . . .
H21 H -0.0517 0.9924 0.9177 0.024 Uiso 1 1 calc R . .
C22 C 0.1221(3) 1.0926(2) 0.95540(11) 0.0235(5) Uani 1 1 d . . .
H22 H 0.0697 1.1332 0.9783 0.028 Uiso 1 1 calc R . .
C23 C 0.2719(3) 1.1162(2) 0.95817(12) 0.0239(5) Uani 1 1 d . . .
H23 H 0.3236 1.174 0.9824 0.029 Uiso 1 1 calc R . .
C24 C 0.3447(3) 1.05400(19) 0.92487(11) 0.0202(5) Uani 1 1 d . . .
H24 H 0.4483 1.0678 0.9271 0.024 Uiso 1 1 calc R . .
C25 C 0.2667(3) 0.97128(18) 0.88810(10) 0.0152(5) Uani 1 1 d . . .
C31 C 0.1572(3) 0.65077(19) 0.87700(12) 0.0223(5) Uani 1 1 d . . .
H31 H 0.0561 0.6256 0.8711 0.027 Uiso 1 1 calc R . .
C32 C 0.2784(3) 0.5842(2) 0.90479(13) 0.0278(6) Uani 1 1 d . . .
H32 H 0.2609 0.5154 0.9178 0.033 Uiso 1 1 calc R . .
C33 C 0.4250(3) 0.6203(2) 0.91303(13) 0.0262(6) Uani 1 1 d . . .
H33 H 0.5109 0.5765 0.9315 0.031 Uiso 1 1 calc R . .
C34 C 0.4450(3) 0.7211(2) 0.89405(11) 0.0209(5) Uani 1 1 d . . .
H34 H 0.5456 0.747 0.8995 0.025 Uiso 1 1 calc R . .
C35 C 0.3198(3) 0.78503(19) 0.86716(10) 0.0156(5) Uani 1 1 d . . .
C40 C -0.1390(3) 0.8357(2) 0.69191(12) 0.0220(5) Uani 1 1 d . . .
H40A H -0.2147 0.8921 0.6902 0.026 Uiso 1 1 calc R . .
H40B H -0.1709 0.7968 0.6516 0.026 Uiso 1 1 calc R . .
C42 C -0.2916(3) 0.7378(2) 0.74528(13) 0.0252(6) Uani 1 1 d . . .
H42A H -0.3476 0.7054 0.7051 0.038 Uiso 1 1 calc R . .
H42B H -0.3433 0.8029 0.751 0.038 Uiso 1 1 calc R . .
H42C H -0.2887 0.689 0.7797 0.038 Uiso 1 1 calc R . .
C43 C -0.0607(3) 0.6640(2) 0.73325(13) 0.0255(6) Uani 1 1 d . . .
H43A H -0.0599 0.6125 0.7661 0.038 Uiso 1 1 calc R . .
H43B H 0.0447 0.6784 0.7334 0.038 Uiso 1 1 calc R . .
H43C H -0.1192 0.6358 0.6922 0.038 Uiso 1 1 calc R . .
C51 C -0.1208(3) 0.7291(2) 0.92054(11) 0.0181(5) Uani 1 1 d . . .
C61 C -0.2338(3) 1.0336(2) 0.78870(11) 0.0179(5) Uani 1 1 d . . .
Fe1 Fe -0.00074(3) 0.84726(3) 0.823771(15) 0.01387(10) Uani 1 1 d . . .
N10 N 0.1011(2) 0.88818(15) 0.76311(9) 0.0147(4) Uani 1 1 d . . .
N20 N 0.1190(2) 0.95022(15) 0.88467(9) 0.0157(4) Uani 1 1 d . . .
N30 N 0.1747(2) 0.74950(15) 0.85778(9) 0.0164(4) Uani 1 1 d . . .
N41 N -0.1325(2) 0.76229(16) 0.74539(10) 0.0204(4) Uani 1 1 d . . .
N50 N -0.0992(2) 0.78704(17) 0.88384(10) 0.0198(4) Uani 1 1 d . . .
N60 N -0.1585(2) 0.95809(16) 0.79693(9) 0.0185(4) Uani 1 1 d . . .
S52 S -0.14563(8) 0.64264(5) 0.97168(3) 0.02608(15) Uani 1 1 d . . .
S62 S -0.33932(7) 1.14070(5) 0.77634(3) 0.02767(16) Uani 1 1 d . . .
C1 C 0.7191(3) 0.2794(2) 0.93229(14) 0.0328(7) Uani 1 1 d . . .
D1A D 0.7359 0.2621 0.8915 0.039 Uiso 1 1 calc R . .
D1B D 0.7973 0.3316 0.954 0.039 Uiso 1 1 calc R . .
Cl2 Cl 0.74047(8) 0.16498(7) 0.97837(4) 0.0415(2) Uani 1 1 d . . .
Cl3 Cl 0.53434(9) 0.33465(7) 0.91857(4) 0.0454(2) Uani 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C11 N10 1.352(3) . ?
C11 C12 1.379(4) . ?
C11 C40 1.508(3) . ?
C12 C13 1.394(4) . ?
C13 C14 1.388(3) . ?
C14 C15 1.387(3) . ?
C15 N10 1.352(3) . ?
C15 C16 1.535(3) . ?
C16 C25 1.532(3) . ?
C16 C17 1.536(3) . ?
C16 C35 1.544(3) . ?
C21 N20 1.350(3) . ?
C21 C22 1.377(4) . ?
C22 C23 1.386(4) . ?
C23 C24 1.383(4) . ?
C24 C25 1.392(3) . ?
C25 N20 1.357(3) . ?
C31 N30 1.351(3) . ?
C31 C32 1.385(4) . ?
C32 C33 1.376(4) . ?
C33 C34 1.379(4) . ?
C34 C35 1.385(3) . ?
C35 N30 1.357(3) . ?
C40 N41 1.501(3) . ?
C42 N41 1.487(3) . ?
C43 N41 1.473(3) . ?
C51 N50 1.160(3) . ?
C51 S52 1.647(3) . ?
C61 N60 1.163(3) . ?
C61 S62 1.644(3) . ?
Fe1 N10 1.9281(19) . ?
Fe1 N20 1.966(2) . ?
Fe1 N50 1.977(2) . ?
Fe1 N60 1.977(2) . ?
Fe1 N30 1.9915(19) . ?
Fe1 N41 2.100(2) . ?
C1 Cl2 1.757(3) . ?
C1 Cl3 1.770(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N10 C11 C12 121.5(2) . . ?
N10 C11 C40 113.1(2) . . ?
C12 C11 C40 125.5(2) . . ?
C11 C12 C13 118.6(2) . . ?
C14 C13 C12 119.4(2) . . ?
C15 C14 C13 119.3(2) . . ?
N10 C15 C14 120.5(2) . . ?
N10 C15 C16 114.87(19) . . ?
C14 C15 C16 124.6(2) . . ?
C25 C16 C15 108.67(18) . . ?
C25 C16 C17 110.71(19) . . ?
C15 C16 C17 110.12(18) . . ?
C25 C16 C35 107.95(18) . . ?
C15 C16 C35 108.35(18) . . ?
C17 C16 C35 110.95(19) . . ?
N20 C21 C22 122.8(2) . . ?
C21 C22 C23 118.9(2) . . ?
C24 C23 C22 118.7(2) . . ?
C23 C24 C25 120.2(2) . . ?
N20 C25 C24 120.6(2) . . ?
N20 C25 C16 116.3(2) . . ?
C24 C25 C16 123.1(2) . . ?
N30 C31 C32 123.7(2) . . ?
C33 C32 C31 118.2(2) . . ?
C32 C33 C34 118.9(2) . . ?
C33 C34 C35 120.6(2) . . ?
N30 C35 C34 121.0(2) . . ?
N30 C35 C16 117.19(19) . . ?
C34 C35 C16 121.8(2) . . ?
N41 C40 C11 108.73(19) . . ?
N50 C51 S52 177.1(2) . . ?
N60 C61 S62 179.3(2) . . ?
N10 Fe1 N20 91.06(8) . . ?
N10 Fe1 N50 172.86(8) . . ?
N20 Fe1 N50 93.59(8) . . ?
N10 Fe1 N60 93.30(8) . . ?
N20 Fe1 N60 86.57(8) . . ?
N50 Fe1 N60 92.39(8) . . ?
N10 Fe1 N30 86.10(8) . . ?
N20 Fe1 N30 86.18(8) . . ?
N50 Fe1 N30 88.80(8) . . ?
N60 Fe1 N30 172.71(8) . . ?
N10 Fe1 N41 80.38(8) . . ?
N20 Fe1 N41 168.27(8) . . ?
N50 Fe1 N41 95.73(8) . . ?
N60 Fe1 N41 85.94(8) . . ?
N30 Fe1 N41 101.11(8) . . ?
C15 N10 C11 120.1(2) . . ?
C15 N10 Fe1 123.06(16) . . ?
C11 N10 Fe1 116.77(16) . . ?
C21 N20 C25 118.8(2) . . ?
C21 N20 Fe1 120.18(16) . . ?
C25 N20 Fe1 120.66(16) . . ?
C31 N30 C35 117.6(2) . . ?
C31 N30 Fe1 122.79(16) . . ?
C35 N30 Fe1 119.37(16) . . ?
C43 N41 C42 108.2(2) . . ?
C43 N41 C40 107.2(2) . . ?
C42 N41 C40 108.82(19) . . ?
C43 N41 Fe1 114.34(15) . . ?
C42 N41 Fe1 115.28(15) . . ?
C40 N41 Fe1 102.56(14) . . ?
C51 N50 Fe1 158.53(19) . . ?
C61 N60 Fe1 168.4(2) . . ?
Cl2 C1 Cl3 111.32(15) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N10 C11 C12 C13 1.1(4) . . . . ?
C40 C11 C12 C13 -177.5(2) . . . . ?
C11 C12 C13 C14 4.8(4) . . . . ?
C12 C13 C14 C15 -4.1(4) . . . . ?
C13 C14 C15 N10 -2.5(4) . . . . ?
C13 C14 C15 C16 176.0(2) . . . . ?
N10 C15 C16 C25 -61.6(3) . . . . ?
C14 C15 C16 C25 119.9(2) . . . . ?
N10 C15 C16 C17 177.0(2) . . . . ?
C14 C15 C16 C17 -1.6(3) . . . . ?
N10 C15 C16 C35 55.5(2) . . . . ?
C14 C15 C16 C35 -123.1(2) . . . . ?
N20 C21 C22 C23 -1.1(4) . . . . ?
C21 C22 C23 C24 -1.0(4) . . . . ?
C22 C23 C24 C25 1.7(4) . . . . ?
C23 C24 C25 N20 -0.3(4) . . . . ?
C23 C24 C25 C16 178.9(2) . . . . ?
C15 C16 C25 N20 63.0(3) . . . . ?
C17 C16 C25 N20 -175.98(19) . . . . ?
C35 C16 C25 N20 -54.4(2) . . . . ?
C15 C16 C25 C24 -116.3(2) . . . . ?
C17 C16 C25 C24 4.8(3) . . . . ?
C35 C16 C25 C24 126.4(2) . . . . ?
N30 C31 C32 C33 -0.3(4) . . . . ?
C31 C32 C33 C34 0.7(4) . . . . ?
C32 C33 C34 C35 0.0(4) . . . . ?
C33 C34 C35 N30 -1.2(4) . . . . ?
C33 C34 C35 C16 176.3(2) . . . . ?
C25 C16 C35 N30 59.9(2) . . . . ?
C15 C16 C35 N30 -57.7(3) . . . . ?
C17 C16 C35 N30 -178.7(2) . . . . ?
C25 C16 C35 C34 -117.8(2) . . . . ?
C15 C16 C35 C34 124.7(2) . . . . ?
C17 C16 C35 C34 3.7(3) . . . . ?
N10 C11 C40 N41 -27.4(3) . . . . ?
C12 C11 C40 N41 151.3(2) . . . . ?
C14 C15 N10 C11 8.4(3) . . . . ?
C16 C15 N10 C11 -170.2(2) . . . . ?
C14 C15 N10 Fe1 -175.63(17) . . . . ?
C16 C15 N10 Fe1 5.7(3) . . . . ?
C12 C11 N10 C15 -7.8(4) . . . . ?
C40 C11 N10 C15 171.0(2) . . . . ?
C12 C11 N10 Fe1 176.03(19) . . . . ?
C40 C11 N10 Fe1 -5.2(3) . . . . ?
N20 Fe1 N10 C15 36.60(19) . . . . ?
N60 Fe1 N10 C15 123.23(19) . . . . ?
N30 Fe1 N10 C15 -49.50(19) . . . . ?
N41 Fe1 N10 C15 -151.47(19) . . . . ?
N20 Fe1 N10 C11 -147.32(18) . . . . ?
N60 Fe1 N10 C11 -60.70(18) . . . . ?
N30 Fe1 N10 C11 126.58(18) . . . . ?
N41 Fe1 N10 C11 24.61(18) . . . . ?
C22 C21 N20 C25 2.5(4) . . . . ?
C22 C21 N20 Fe1 -170.40(19) . . . . ?
C24 C25 N20 C21 -1.8(3) . . . . ?
C16 C25 N20 C21 179.0(2) . . . . ?
C24 C25 N20 Fe1 171.15(17) . . . . ?
C16 C25 N20 Fe1 -8.1(3) . . . . ?
N10 Fe1 N20 C21 137.81(18) . . . . ?
N50 Fe1 N20 C21 -47.61(19) . . . . ?
N60 Fe1 N20 C21 44.57(18) . . . . ?
N30 Fe1 N20 C21 -136.17(19) . . . . ?
N41 Fe1 N20 C21 94.9(4) . . . . ?
N10 Fe1 N20 C25 -35.00(18) . . . . ?
N50 Fe1 N20 C25 139.58(18) . . . . ?
N60 Fe1 N20 C25 -128.24(18) . . . . ?
N30 Fe1 N20 C25 51.02(18) . . . . ?
N41 Fe1 N20 C25 -77.9(4) . . . . ?
C32 C31 N30 C35 -0.8(4) . . . . ?
C32 C31 N30 Fe1 -175.3(2) . . . . ?
C34 C35 N30 C31 1.6(3) . . . . ?
C16 C35 N30 C31 -176.1(2) . . . . ?
C34 C35 N30 Fe1 176.30(17) . . . . ?
C16 C35 N30 Fe1 -1.4(3) . . . . ?
N10 Fe1 N30 C31 -139.5(2) . . . . ?
N20 Fe1 N30 C31 129.17(19) . . . . ?
N50 Fe1 N30 C31 35.50(19) . . . . ?
N41 Fe1 N30 C31 -60.1(2) . . . . ?
N10 Fe1 N30 C35 46.08(17) . . . . ?
N20 Fe1 N30 C35 -45.25(17) . . . . ?
N50 Fe1 N30 C35 -138.93(18) . . . . ?
N41 Fe1 N30 C35 125.47(17) . . . . ?
C11 C40 N41 C43 -78.1(2) . . . . ?
C11 C40 N41 C42 165.2(2) . . . . ?
C11 C40 N41 Fe1 42.6(2) . . . . ?
N10 Fe1 N41 C43 79.33(17) . . . . ?
N20 Fe1 N41 C43 123.0(4) . . . . ?
N50 Fe1 N41 C43 -94.63(18) . . . . ?
N60 Fe1 N41 C43 173.37(18) . . . . ?
N30 Fe1 N41 C43 -4.73(18) . . . . ?
N10 Fe1 N41 C42 -154.38(19) . . . . ?
N20 Fe1 N41 C42 -110.7(4) . . . . ?
N50 Fe1 N41 C42 31.66(19) . . . . ?
N60 Fe1 N41 C42 -60.34(18) . . . . ?
N30 Fe1 N41 C42 121.57(18) . . . . ?
N10 Fe1 N41 C40 -36.30(14) . . . . ?
N20 Fe1 N41 C40 7.4(5) . . . . ?
N50 Fe1 N41 C40 149.74(14) . . . . ?
N60 Fe1 N41 C40 57.75(14) . . . . ?
N30 Fe1 N41 C40 -120.35(14) . . . . ?
N20 Fe1 N50 C51 -98.6(5) . . . . ?
N60 Fe1 N50 C51 174.7(5) . . . . ?
N30 Fe1 N50 C51 -12.5(5) . . . . ?
N41 Fe1 N50 C51 88.6(5) . . . . ?
N10 Fe1 N60 C61 -89.2(9) . . . . ?
N20 Fe1 N60 C61 1.7(9) . . . . ?
N50 Fe1 N60 C61 95.1(9) . . . . ?
N41 Fe1 N60 C61 -169.3(10) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_database_code_depnum_ccdc_archive 'CCDC 960956'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound3

_audit_creation_date             2013-09-13T18:33:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;dichlorido(1-{6-[1,1-di(pyridin-2-yl)ethyl]pyridin-2-yl}-
        N,N-dimethylmethanamine)iron(III) hexafluorophosphate
;
_chemical_formula_iupac          '[Fe (C20 H22 N4) Cl2](P F6)'
_chemical_formula_moiety         'C20 H22 Cl2 Fe N4 1+, F6 P 1-'
_chemical_formula_sum            'C20 H22 Cl2 F6 Fe N4 P'
_chemical_formula_weight         590.14

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.9533(5)
_cell_length_b                   10.8208(7)
_cell_length_c                   12.7219(7)
_cell_angle_alpha                92.040(5)
_cell_angle_beta                 106.526(5)
_cell_angle_gamma                93.255(5)
_cell_volume                     1177.98(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    3783
_cell_measurement_theta_min      3.3389
_cell_measurement_theta_max      32.3926

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            'pale orange'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             598
_exptl_crystal_recrystallization_method 
'precipitation (vapour diffusion): acetonitrile, diethyl ether, r. t., 2 d'

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.78828
_exptl_absorpt_correction_T_max  1

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent Sapphire 3'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_standards_number         0
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.039
_diffrn_reflns_number            9564
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.35
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_full        26
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             4620
_reflns_number_gt                4042
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
 The hexafluorophosphate moiety exhibits rotational disorder. It has been
 modeled in two discrete positions using SAME, DELU and tightened ISOR
 restraints. The s.o.f. refined to 51(2) % and 49(2) %, respectively.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0472P)²+0.4573P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4620
_refine_ls_number_parameters     365
_refine_ls_number_restraints     135
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0376
_refine_ls_wR_factor_ref         0.095
_refine_ls_wR_factor_gt          0.0908
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.063

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#

_restr_special_details           
;
 Additionally, equal-1,2- and equal-1,3-distance restraints (generated using
 SHELXL-97 SAME intructions with standard weights) have been applied to the
 whole hexafluorophosphate moiety in both orientations of disorder.
;
loop_
_restr_U_rigid_atom_site_label_1
_restr_U_rigid_site_symmetry_1
_restr_U_rigid_atom_site_label_2
_restr_U_rigid_site_symmetry_2
_restr_U_rigid_target_weight_param
_restr_U_rigid_U_parallel
_restr_U_rigid_diff
_restr_U_rigid_details
P1 . F1A . 0.01 0 0.0036 'SHELXL DELU'
P1 . F2A . 0.01 0 0.0043 'SHELXL DELU'
P1 . F3A . 0.01 0 0.0091 'SHELXL DELU'
P1 . F4A . 0.01 0 0.0005 'SHELXL DELU'
P1 . F5A . 0.01 0 0.0022 'SHELXL DELU'
P1 . F6A . 0.01 0 0.0042 'SHELXL DELU'
P1 . F1B . 0.01 0 0.0036 'SHELXL DELU'
P1 . F2B . 0.01 0 0.0078 'SHELXL DELU'
P1 . F3B . 0.01 0 0.0017 'SHELXL DELU'
P1 . F4B . 0.01 0 0.0015 'SHELXL DELU'
P1 . F5B . 0.01 0 0.0048 'SHELXL DELU'
P1 . F6B . 0.01 0 0.0035 'SHELXL DELU'

loop_
_restr_U_iso_atom_site_label
_restr_U_iso_weight_param
F1A 0.02
F2A 0.02
F3A 0.02
F4A 0.02
F5A 0.02
F6A 0.02
F1B 0.02
F2B 0.02
F3B 0.02
F4B 0.02
F5B 0.02
F6B 0.02

loop_
_restr_parameter_class_class_id
_restr_parameter_class_parameter_type
_restr_parameter_class_target
_restr_parameter_class_target_weight_param
_restr_parameter_class_details
1 occupancy 1 0 'total s.o.f. of 1'
2 occupancy 1 0 'total s.o.f. of 1'
3 occupancy 1 0 'total s.o.f. of 1'
4 occupancy 1 0 'total s.o.f. of 1'
5 occupancy 1 0 'total s.o.f. of 1'
6 occupancy 1 0 'total s.o.f. of 1'

loop_
_restr_parameter_id
_restr_parameter_class_id
_restr_parameter_atom_site_label
_restr_parameter_atom_coefficient
1 1 F1A 1
2 1 F1B 1
3 2 F2A 1
4 2 F2B 1
5 3 F3A 1
6 3 F3B 1
7 1 F4A 1
8 1 F4B 1
9 2 F5A 1
10 2 F5B 1
11 3 F6A 1
12 3 F6B 1

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C -0.0360(3) 0.0603(2) 0.15180(19) 0.0231(5) Uani 1 1 d . . .
C12 C -0.1519(3) -0.0027(2) 0.0690(2) 0.0263(6) Uani 1 1 d . . .
H12 H -0.1419 -0.086 0.0473 0.032 Uiso 1 1 calc R . .
C13 C -0.2822(3) 0.0572(2) 0.0186(2) 0.0284(6) Uani 1 1 d . . .
H13 H -0.3613 0.0164 -0.0407 0.034 Uiso 1 1 calc R . .
C14 C -0.2987(3) 0.1775(2) 0.0540(2) 0.0261(6) Uani 1 1 d . . .
H14 H -0.3907 0.2181 0.0217 0.031 Uiso 1 1 calc R . .
C16 C -0.1784(3) 0.2368(2) 0.13735(19) 0.0207(5) Uani 1 1 d . . .
C17 C -0.1877(3) 0.3668(2) 0.1888(2) 0.0233(5) Uani 1 1 d . . .
C18 C -0.3531(3) 0.4101(3) 0.1406(2) 0.0324(6) Uani 1 1 d . . .
H18A H -0.374 0.4169 0.0612 0.049 Uiso 1 1 calc R . .
H18B H -0.3606 0.4912 0.175 0.049 Uiso 1 1 calc R . .
H18C H -0.4298 0.3499 0.1551 0.049 Uiso 1 1 calc R . .
C21 C 0.1964(3) 0.5210(2) 0.1934(2) 0.0302(6) Uani 1 1 d . . .
H21 H 0.303 0.5056 0.2244 0.036 Uiso 1 1 calc R . .
C22 C 0.1613(4) 0.6273(2) 0.1375(2) 0.0375(7) Uani 1 1 d . . .
H22 H 0.2417 0.6844 0.1301 0.045 Uiso 1 1 calc R . .
C23 C 0.0075(4) 0.6483(2) 0.0929(2) 0.0370(7) Uani 1 1 d . . .
H23 H -0.02 0.7197 0.0523 0.044 Uiso 1 1 calc R . .
C24 C -0.1083(3) 0.5658(2) 0.1070(2) 0.0315(6) Uani 1 1 d . . .
H24 H -0.2153 0.5805 0.0768 0.038 Uiso 1 1 calc R . .
C25 C -0.0660(3) 0.4608(2) 0.16579(19) 0.0231(5) Uani 1 1 d . . .
C31 C 0.0312(3) 0.3219(2) 0.4802(2) 0.0247(5) Uani 1 1 d . . .
H31 H 0.134 0.3029 0.5188 0.03 Uiso 1 1 calc R . .
C32 C -0.0728(3) 0.3437(2) 0.5396(2) 0.0297(6) Uani 1 1 d . . .
H32 H -0.0428 0.3393 0.6172 0.036 Uiso 1 1 calc R . .
C33 C -0.2218(3) 0.3722(3) 0.4831(2) 0.0339(6) Uani 1 1 d . . .
H33 H -0.297 0.3862 0.5211 0.041 Uiso 1 1 calc R . .
C34 C -0.2601(3) 0.3803(2) 0.3702(2) 0.0306(6) Uani 1 1 d . . .
H34 H -0.3614 0.4017 0.3307 0.037 Uiso 1 1 calc R . .
C35 C -0.1516(3) 0.3573(2) 0.3150(2) 0.0224(5) Uani 1 1 d . . .
C40 C 0.1097(3) 0.0029(2) 0.2159(2) 0.0263(6) Uani 1 1 d . . .
H40A H 0.0836 -0.0842 0.2291 0.032 Uiso 1 1 calc R . .
H40B H 0.1863 0.0033 0.1731 0.032 Uiso 1 1 calc R . .
C42 C 0.3437(3) 0.0399(3) 0.3694(2) 0.0348(7) Uani 1 1 d . . .
H42A H 0.3446 -0.0496 0.3784 0.052 Uiso 1 1 calc R . .
H42B H 0.3896 0.0841 0.4409 0.052 Uiso 1 1 calc R . .
H42C H 0.4048 0.063 0.3194 0.052 Uiso 1 1 calc R . .
C43 C 0.0892(3) 0.0374(2) 0.3999(2) 0.0311(6) Uani 1 1 d . . .
H43A H -0.0197 0.0574 0.3699 0.047 Uiso 1 1 calc R . .
H43B H 0.1348 0.0827 0.471 0.047 Uiso 1 1 calc R . .
H43C H 0.093 -0.0519 0.4097 0.047 Uiso 1 1 calc R . .
N10 N -0.0472(2) 0.17962(17) 0.18176(15) 0.0193(4) Uani 1 1 d . . .
N20 N 0.0851(2) 0.43804(18) 0.20586(16) 0.0224(4) Uani 1 1 d . . .
N30 N -0.0062(2) 0.32603(18) 0.37010(16) 0.0211(4) Uani 1 1 d . . .
N41 N 0.1792(3) 0.07380(19) 0.32283(16) 0.0246(5) Uani 1 1 d . . .
Cl1 Cl 0.36382(7) 0.35182(6) 0.42039(5) 0.02985(16) Uani 1 1 d . . .
Cl2 Cl 0.28903(8) 0.23961(6) 0.15083(5) 0.02975(16) Uani 1 1 d . . .
Fe1 Fe 0.16240(4) 0.27137(3) 0.28414(3) 0.01917(11) Uani 1 1 d . . .
P1 P 0.36780(9) 0.19222(8) 0.74984(6) 0.03539(19) Uani 1 1 d DU . .
F1A F 0.3692(8) 0.2145(6) 0.8734(5) 0.0439(15) Uani 0.510(11) 1 d PDU A 1
F2A F 0.1928(8) 0.2177(12) 0.7121(5) 0.103(4) Uani 0.510(11) 1 d PDU A 1
F3A F 0.4280(14) 0.3271(4) 0.7442(9) 0.091(3) Uani 0.510(11) 1 d PDU A 1
F4A F 0.5447(6) 0.1528(6) 0.7877(4) 0.0484(16) Uani 0.510(11) 1 d PDU A 1
F5A F 0.3186(10) 0.0465(6) 0.7561(6) 0.075(2) Uani 0.510(11) 1 d PDU A 1
F6A F 0.3684(14) 0.1616(12) 0.6270(6) 0.060(3) Uani 0.510(11) 1 d PDU A 1
F1B F 0.4046(14) 0.2618(12) 0.8699(6) 0.111(4) Uani 0.490(11) 1 d PDU A 2
F2B F 0.1878(9) 0.1754(8) 0.7430(10) 0.093(3) Uani 0.490(11) 1 d PDU A 2
F3B F 0.3278(12) 0.3276(5) 0.7030(5) 0.073(2) Uani 0.490(11) 1 d PDU A 2
F4B F 0.5441(8) 0.2139(11) 0.7572(10) 0.115(4) Uani 0.490(11) 1 d PDU A 2
F5B F 0.3978(12) 0.0657(8) 0.7983(6) 0.085(3) Uani 0.490(11) 1 d PDU A 2
F6B F 0.3306(16) 0.1364(11) 0.6288(7) 0.065(3) Uani 0.490(11) 1 d PDU A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C11 N10 1.350(3) . ?
C11 C12 1.378(3) . ?
C11 C40 1.508(3) . ?
C12 C13 1.371(4) . ?
C13 C14 1.392(4) . ?
C14 C16 1.385(3) . ?
C16 N10 1.346(3) . ?
C16 C17 1.547(3) . ?
C17 C18 1.539(3) . ?
C17 C25 1.544(4) . ?
C17 C35 1.554(3) . ?
C21 N20 1.350(3) . ?
C21 C22 1.378(4) . ?
C22 C23 1.368(4) . ?
C23 C24 1.384(4) . ?
C24 C25 1.394(3) . ?
C25 N20 1.344(3) . ?
C31 N30 1.347(3) . ?
C31 C32 1.382(4) . ?
C32 C33 1.381(4) . ?
C33 C34 1.386(4) . ?
C34 C35 1.378(4) . ?
C35 N30 1.359(3) . ?
C40 N41 1.488(3) . ?
C42 N41 1.495(3) . ?
C43 N41 1.486(3) . ?
N10 Fe1 2.1235(19) . ?
N20 Fe1 2.1449(19) . ?
N30 Fe1 2.196(2) . ?
N41 Fe1 2.215(2) . ?
Cl1 Fe1 2.2250(7) . ?
Cl2 Fe1 2.3187(7) . ?
P1 F5B 1.528(6) . ?
P1 F3A 1.538(5) . ?
P1 F2A 1.547(6) . ?
P1 F4B 1.559(6) . ?
P1 F6B 1.570(8) . ?
P1 F1A 1.579(5) . ?
P1 F2B 1.589(7) . ?
P1 F6A 1.587(7) . ?
P1 F4A 1.606(5) . ?
P1 F1B 1.617(7) . ?
P1 F5A 1.624(5) . ?
P1 F3B 1.622(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N10 C11 C12 121.2(2) . . ?
N10 C11 C40 115.2(2) . . ?
C12 C11 C40 123.5(2) . . ?
C13 C12 C11 118.7(2) . . ?
C12 C13 C14 120.2(2) . . ?
C16 C14 C13 118.7(2) . . ?
N10 C16 C14 120.5(2) . . ?
N10 C16 C17 116.1(2) . . ?
C14 C16 C17 123.4(2) . . ?
C18 C17 C16 109.2(2) . . ?
C18 C17 C25 109.8(2) . . ?
C16 C17 C25 110.8(2) . . ?
C18 C17 C35 110.2(2) . . ?
C16 C17 C35 108.25(19) . . ?
C25 C17 C35 108.56(19) . . ?
N20 C21 C22 122.5(3) . . ?
C23 C22 C21 118.3(3) . . ?
C22 C23 C24 120.1(3) . . ?
C23 C24 C25 119.2(3) . . ?
N20 C25 C24 120.5(2) . . ?
N20 C25 C17 117.1(2) . . ?
C24 C25 C17 122.4(2) . . ?
N30 C31 C32 123.2(2) . . ?
C33 C32 C31 118.1(2) . . ?
C32 C33 C34 119.2(3) . . ?
C35 C34 C33 120.2(2) . . ?
N30 C35 C34 120.7(2) . . ?
N30 C35 C17 117.0(2) . . ?
C34 C35 C17 122.3(2) . . ?
N41 C40 C11 110.02(19) . . ?
C16 N10 C11 120.4(2) . . ?
C16 N10 Fe1 123.99(16) . . ?
C11 N10 Fe1 115.14(16) . . ?
C25 N20 C21 119.4(2) . . ?
C25 N20 Fe1 123.57(16) . . ?
C21 N20 Fe1 116.98(17) . . ?
C31 N30 C35 118.6(2) . . ?
C31 N30 Fe1 119.43(16) . . ?
C35 N30 Fe1 121.90(16) . . ?
C40 N41 C43 108.7(2) . . ?
C40 N41 C42 108.8(2) . . ?
C43 N41 C42 108.4(2) . . ?
C40 N41 Fe1 105.17(14) . . ?
C43 N41 Fe1 112.54(15) . . ?
C42 N41 Fe1 113.09(17) . . ?
N10 Fe1 N20 87.25(7) . . ?
N10 Fe1 N30 78.99(8) . . ?
N20 Fe1 N30 78.51(8) . . ?
N10 Fe1 N41 75.01(7) . . ?
N20 Fe1 N41 161.98(8) . . ?
N30 Fe1 N41 100.71(8) . . ?
N10 Fe1 Cl1 167.72(6) . . ?
N20 Fe1 Cl1 99.44(6) . . ?
N30 Fe1 Cl1 92.17(6) . . ?
N41 Fe1 Cl1 98.58(6) . . ?
N10 Fe1 Cl2 91.30(6) . . ?
N20 Fe1 Cl2 87.24(6) . . ?
N30 Fe1 Cl2 163.04(6) . . ?
N41 Fe1 Cl2 89.98(6) . . ?
Cl1 Fe1 Cl2 99.26(3) . . ?
F3A P1 F2A 95.3(4) . . ?
F5B P1 F4B 90.1(5) . . ?
F5B P1 F6B 92.7(6) . . ?
F4B P1 F6B 90.9(6) . . ?
F3A P1 F1A 92.0(3) . . ?
F2A P1 F1A 89.9(4) . . ?
F5B P1 F2B 91.7(4) . . ?
F4B P1 F2B 177.9(6) . . ?
F6B P1 F2B 90.1(6) . . ?
F3A P1 F6A 90.9(5) . . ?
F2A P1 F6A 91.5(5) . . ?
F1A P1 F6A 176.6(5) . . ?
F3A P1 F4A 89.8(4) . . ?
F2A P1 F4A 174.9(5) . . ?
F1A P1 F4A 90.9(3) . . ?
F5B P1 F1B 92.4(4) . . ?
F4B P1 F1B 88.7(5) . . ?
F6B P1 F1B 174.9(6) . . ?
F2B P1 F1B 90.2(5) . . ?
F3A P1 F5A 175.2(4) . . ?
F2A P1 F5A 89.3(5) . . ?
F1A P1 F5A 89.3(3) . . ?
F6A P1 F5A 87.7(5) . . ?
F4A P1 F5A 85.6(3) . . ?
F5B P1 F3B 176.3(4) . . ?
F4B P1 F3B 92.9(5) . . ?
F6B P1 F3B 89.5(5) . . ?
F2B P1 F3B 85.3(4) . . ?
F1B P1 F3B 85.4(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N10 C11 C12 C13 -1.5(4) . . . . ?
C40 C11 C12 C13 177.8(2) . . . . ?
C11 C12 C13 C14 -2.6(4) . . . . ?
C12 C13 C14 C16 2.9(4) . . . . ?
C13 C14 C16 N10 1.1(4) . . . . ?
C13 C14 C16 C17 -175.8(2) . . . . ?
N10 C16 C17 C18 -171.7(2) . . . . ?
C14 C16 C17 C18 5.4(3) . . . . ?
N10 C16 C17 C25 67.2(3) . . . . ?
C14 C16 C17 C25 -115.8(3) . . . . ?
N10 C16 C17 C35 -51.7(3) . . . . ?
C14 C16 C17 C35 125.3(2) . . . . ?
N20 C21 C22 C23 -0.2(4) . . . . ?
C21 C22 C23 C24 1.7(4) . . . . ?
C22 C23 C24 C25 -0.7(4) . . . . ?
C23 C24 C25 N20 -1.8(4) . . . . ?
C23 C24 C25 C17 177.7(2) . . . . ?
C18 C17 C25 N20 178.0(2) . . . . ?
C16 C17 C25 N20 -61.3(3) . . . . ?
C35 C17 C25 N20 57.4(3) . . . . ?
C18 C17 C25 C24 -1.6(3) . . . . ?
C16 C17 C25 C24 119.2(3) . . . . ?
C35 C17 C25 C24 -122.1(2) . . . . ?
N30 C31 C32 C33 -0.6(4) . . . . ?
C31 C32 C33 C34 -1.3(4) . . . . ?
C32 C33 C34 C35 1.4(4) . . . . ?
C33 C34 C35 N30 0.3(4) . . . . ?
C33 C34 C35 C17 -179.1(2) . . . . ?
C18 C17 C35 N30 -176.8(2) . . . . ?
C16 C17 C35 N30 63.9(3) . . . . ?
C25 C17 C35 N30 -56.5(3) . . . . ?
C18 C17 C35 C34 2.7(3) . . . . ?
C16 C17 C35 C34 -116.6(3) . . . . ?
C25 C17 C35 C34 123.0(3) . . . . ?
N10 C11 C40 N41 20.8(3) . . . . ?
C12 C11 C40 N41 -158.5(2) . . . . ?
C14 C16 N10 C11 -5.2(4) . . . . ?
C17 C16 N10 C11 171.9(2) . . . . ?
C14 C16 N10 Fe1 166.46(18) . . . . ?
C17 C16 N10 Fe1 -16.4(3) . . . . ?
C12 C11 N10 C16 5.5(4) . . . . ?
C40 C11 N10 C16 -173.8(2) . . . . ?
C12 C11 N10 Fe1 -166.88(19) . . . . ?
C40 C11 N10 Fe1 13.8(3) . . . . ?
C24 C25 N20 C21 3.3(4) . . . . ?
C17 C25 N20 C21 -176.2(2) . . . . ?
C24 C25 N20 Fe1 -174.03(18) . . . . ?
C17 C25 N20 Fe1 6.4(3) . . . . ?
C22 C21 N20 C25 -2.3(4) . . . . ?
C22 C21 N20 Fe1 175.2(2) . . . . ?
C32 C31 N30 C35 2.3(4) . . . . ?
C32 C31 N30 Fe1 -173.96(19) . . . . ?
C34 C35 N30 C31 -2.1(3) . . . . ?
C17 C35 N30 C31 177.4(2) . . . . ?
C34 C35 N30 Fe1 174.01(18) . . . . ?
C17 C35 N30 Fe1 -6.5(3) . . . . ?
C11 C40 N41 C43 78.5(2) . . . . ?
C11 C40 N41 C42 -163.6(2) . . . . ?
C11 C40 N41 Fe1 -42.2(2) . . . . ?
C16 N10 Fe1 N20 -24.69(19) . . . . ?
C11 N10 Fe1 N20 147.40(17) . . . . ?
C16 N10 Fe1 N30 54.13(19) . . . . ?
C11 N10 Fe1 N30 -133.78(17) . . . . ?
C16 N10 Fe1 N41 158.5(2) . . . . ?
C11 N10 Fe1 N41 -29.42(16) . . . . ?
C16 N10 Fe1 Cl1 98.8(3) . . . . ?
C11 N10 Fe1 Cl1 -89.2(3) . . . . ?
C16 N10 Fe1 Cl2 -111.87(19) . . . . ?
C11 N10 Fe1 Cl2 60.22(16) . . . . ?
C25 N20 Fe1 N10 30.18(19) . . . . ?
C21 N20 Fe1 N10 -147.22(19) . . . . ?
C25 N20 Fe1 N30 -49.14(19) . . . . ?
C21 N20 Fe1 N30 133.45(19) . . . . ?
C25 N20 Fe1 N41 40.2(4) . . . . ?
C21 N20 Fe1 N41 -137.2(3) . . . . ?
C25 N20 Fe1 Cl1 -139.45(18) . . . . ?
C21 N20 Fe1 Cl1 43.14(18) . . . . ?
C25 N20 Fe1 Cl2 121.61(19) . . . . ?
C21 N20 Fe1 Cl2 -55.79(18) . . . . ?
C31 N30 Fe1 N10 135.46(19) . . . . ?
C35 N30 Fe1 N10 -40.66(18) . . . . ?
C31 N30 Fe1 N20 -135.14(19) . . . . ?
C35 N30 Fe1 N20 48.75(18) . . . . ?
C31 N30 Fe1 N41 63.21(18) . . . . ?
C35 N30 Fe1 N41 -112.90(18) . . . . ?
C31 N30 Fe1 Cl1 -35.94(17) . . . . ?
C35 N30 Fe1 Cl1 147.94(18) . . . . ?
C31 N30 Fe1 Cl2 -168.52(15) . . . . ?
C35 N30 Fe1 Cl2 15.4(3) . . . . ?
C40 N41 Fe1 N10 37.76(15) . . . . ?
C43 N41 Fe1 N10 -80.45(17) . . . . ?
C42 N41 Fe1 N10 156.34(18) . . . . ?
C40 N41 Fe1 N20 27.4(3) . . . . ?
C43 N41 Fe1 N20 -90.8(3) . . . . ?
C42 N41 Fe1 N20 146.0(2) . . . . ?
C40 N41 Fe1 N30 113.17(16) . . . . ?
C43 N41 Fe1 N30 -5.03(18) . . . . ?
C42 N41 Fe1 N30 -128.25(17) . . . . ?
C40 N41 Fe1 Cl1 -152.95(15) . . . . ?
C43 N41 Fe1 Cl1 88.84(16) . . . . ?
C42 N41 Fe1 Cl1 -34.37(17) . . . . ?
C40 N41 Fe1 Cl2 -53.59(15) . . . . ?
C43 N41 Fe1 Cl2 -171.80(16) . . . . ?
C42 N41 Fe1 Cl2 64.99(16) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_database_code_depnum_ccdc_archive 'CCDC 960957'
