# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1a
_database_code_depnum_ccdc_archive 'CCDC 1063076'
_audit_update_record             
;
2015-06-17 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
OC-6-22-(acetylacetonato)difluoridobis(pyridine)vanadium(III)
_chemical_formula_iupac          '[V (C5 H5 N)2 (C5 H7 O2) F2]'
_chemical_formula_moiety         'C15 H17 F2 N2 O2 V'
_chemical_formula_sum            'C15 H17 F2 N2 O2 V'
_chemical_formula_weight         346.24

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 0.0000 0.0000 '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'
O O 0.0106 0.0060 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.4170(14)
_cell_length_b                   8.0367(4)
_cell_length_c                   13.1548(12)
_cell_angle_alpha                90
_cell_angle_beta                 113.588(10)
_cell_angle_gamma                90
_cell_volume                     1590.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    2471
_cell_measurement_theta_min      3.5820
_cell_measurement_theta_max      26.9930
_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.5353
_exptl_crystal_size_mid          0.1159
_exptl_crystal_size_min          0.0576
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)

Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)

Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 11 0 0.0353
-10 -1 18 0.2724
12 -4 -17 0.2203
-21 -1 0 0.0593
10 -10 0 0.0140
-2 -8 13 0.1718
-20 0 15 0.2246
9 10 0 0.0360
-9 -10 0 0.0365

_diffrn_orient_matrix_UB_11      0.0418430000
_diffrn_orient_matrix_UB_12      0.0396705000
_diffrn_orient_matrix_UB_13      0.0156436000
_diffrn_orient_matrix_UB_21      0.0199872000
_diffrn_orient_matrix_UB_22      -0.0632293000
_diffrn_orient_matrix_UB_23      0.0398976000
_diffrn_orient_matrix_UB_31      0.0084872000
_diffrn_orient_matrix_UB_32      -0.0470689000
_diffrn_orient_matrix_UB_33      -0.0403267000

_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent Sapphire3'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12389
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.598
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3116
_reflns_number_gt                2613
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_twin_formation_mechanism        gt
_twin_dimensionality             triperiodic
_twin_morphology                 simple
_twin_special_details            
;       
Individuals are twinned by rotation of 180° around [1 0 0] in
reciprocal space.
;

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.709(1) ref 1 0 0 0 1 0 0 0 1
2 0.291(1) mt_II 1 0 1 0 -1 0 0 0 -1

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX (Farrugia, 2012)'

_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0284P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3116
_refine_ls_number_parameters     202
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.0778
_refine_ls_wR_factor_gt          0.0723
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.4475(2) 0.1043(3) 0.5949(3) 0.0279(7) Uani 1 1 d . . . . .
H11 H 0.4480 0.1037 0.5229 0.033 Uiso 1 1 calc R U . . .
C12 C 0.5219(2) 0.0486(4) 0.6829(3) 0.0316(8) Uani 1 1 d . . . . .
H12 H 0.5728 0.0122 0.6717 0.038 Uiso 1 1 calc R U . . .
C13 C 0.5212(2) 0.0467(4) 0.7877(3) 0.0331(8) Uani 1 1 d . . . . .
H13 H 0.5710 0.0063 0.8496 0.040 Uiso 1 1 calc R U . . .
C14 C 0.4468(2) 0.1045(4) 0.8008(3) 0.0312(8) Uani 1 1 d . . . . .
H14 H 0.4447 0.1065 0.8719 0.037 Uiso 1 1 calc R U . . .
C15 C 0.3751(2) 0.1597(4) 0.7079(3) 0.0294(7) Uani 1 1 d . . . . .
H15 H 0.3241 0.1998 0.7172 0.035 Uiso 1 1 calc R U . . .
C21 C 0.1400(2) 0.3449(4) 0.2286(3) 0.0334(7) Uani 1 1 d . . . . .
H21 H 0.1968 0.3715 0.2299 0.040 Uiso 1 1 calc R U . . .
C22 C 0.0662(2) 0.3719(4) 0.1313(3) 0.0362(8) Uani 1 1 d . . . . .
H22 H 0.0722 0.4166 0.0678 0.043 Uiso 1 1 calc R U . . .
C23 C -0.0161(2) 0.3323(4) 0.1290(3) 0.0371(8) Uani 1 1 d . . . . .
H23 H -0.0682 0.3491 0.0635 0.045 Uiso 1 1 calc R U . . .
C24 C -0.0221(2) 0.2679(4) 0.2229(3) 0.0400(8) Uani 1 1 d . . . . .
H24 H -0.0782 0.2394 0.2233 0.048 Uiso 1 1 calc R U . . .
C25 C 0.0550(2) 0.2458(4) 0.3160(3) 0.0360(8) Uani 1 1 d . . . . .
H25 H 0.0507 0.2014 0.3806 0.043 Uiso 1 1 calc R U . . .
C32 C 0.3363(2) 0.7168(4) 0.4096(3) 0.0475(9) Uani 1 1 d . . . . .
H32A H 0.4006 0.7177 0.4540 0.071 Uiso 1 1 calc R U . . .
H32B H 0.3117 0.8269 0.4126 0.071 Uiso 1 1 calc R U . . .
H32C H 0.3249 0.6893 0.3325 0.071 Uiso 1 1 calc R U . . .
C33 C 0.2932(2) 0.5887(4) 0.4554(3) 0.0315(8) Uani 1 1 d . . . . .
C34 C 0.2421(2) 0.6374(4) 0.5121(3) 0.0344(8) Uani 1 1 d . . . . .
H34 H 0.2308 0.7526 0.5160 0.041 Uiso 1 1 calc R U . . .
C35 C 0.2064(2) 0.5236(4) 0.5641(3) 0.0312(7) Uani 1 1 d . . . . .
C36 C 0.1589(2) 0.5839(4) 0.6343(3) 0.0438(9) Uani 1 1 d . . . . .
H36A H 0.0964 0.5500 0.6001 0.066 Uiso 1 1 calc R U . . .
H36B H 0.1625 0.7055 0.6398 0.066 Uiso 1 1 calc R U . . .
H36C H 0.1868 0.5353 0.7087 0.066 Uiso 1 1 calc R U . . .
N10 N 0.37427(15) 0.1593(3) 0.6060(2) 0.0230(5) Uani 1 1 d . . . . .
N20 N 0.13591(16) 0.2836(3) 0.3204(2) 0.0256(6) Uani 1 1 d . . . . .
O30 O 0.31030(13) 0.4366(3) 0.44014(17) 0.0284(5) Uani 1 1 d . . . . .
O31 O 0.21256(14) 0.3667(2) 0.55773(17) 0.0303(5) Uani 1 1 d . . . . .
F1 F 0.19737(11) 0.0459(2) 0.49475(14) 0.0310(4) Uani 1 1 d . . . . .
F2 F 0.30163(11) 0.1215(2) 0.37143(14) 0.0291(4) Uani 1 1 d . . . . .
V1 V 0.25509(4) 0.22387(5) 0.46330(4) 0.02260(13) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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 1.342(4) . ?
C11 C12 1.379(4) . ?
C12 C13 1.384(5) . ?
C13 C14 1.381(4) . ?
C14 C15 1.387(4) . ?
C15 N10 1.335(4) . ?
C21 N20 1.330(4) . ?
C21 C22 1.382(4) . ?
C22 C23 1.378(4) . ?
C23 C24 1.378(4) . ?
C24 C25 1.377(4) . ?
C25 N20 1.341(4) . ?
C32 C33 1.506(4) . ?
C33 O30 1.288(4) . ?
C33 C34 1.382(4) . ?
C34 C35 1.403(4) . ?
C35 O31 1.271(3) . ?
C35 C36 1.508(4) . ?
N10 V1 2.164(2) . ?
N20 V1 2.156(2) . ?
O30 V1 2.015(2) . ?
O31 V1 2.011(2) . ?
F1 V1 1.8515(17) . ?
F2 V1 1.8603(17) . ?

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 123.1(3) . . ?
C11 C12 C13 118.9(3) . . ?
C14 C13 C12 118.7(3) . . ?
C13 C14 C15 118.6(3) . . ?
N10 C15 C14 123.3(3) . . ?
N20 C21 C22 123.7(3) . . ?
C23 C22 C21 118.2(3) . . ?
C22 C23 C24 119.2(3) . . ?
C25 C24 C23 118.4(3) . . ?
N20 C25 C24 123.5(3) . . ?
O30 C33 C34 124.8(3) . . ?
O30 C33 C32 114.8(3) . . ?
C34 C33 C32 120.4(3) . . ?
C33 C34 C35 122.7(3) . . ?
O31 C35 C34 123.7(3) . . ?
O31 C35 C36 115.7(3) . . ?
C34 C35 C36 120.6(3) . . ?
C15 N10 C11 117.4(3) . . ?
C15 N10 V1 120.9(2) . . ?
C11 N10 V1 121.5(2) . . ?
C21 N20 C25 117.0(3) . . ?
C21 N20 V1 121.1(2) . . ?
C25 N20 V1 121.6(2) . . ?
C33 O30 V1 130.0(2) . . ?
C35 O31 V1 131.6(2) . . ?
F1 V1 F2 100.57(8) . . ?
F1 V1 O31 88.15(8) . . ?
F2 V1 O31 171.27(8) . . ?
F1 V1 O30 172.21(8) . . ?
F2 V1 O30 87.17(8) . . ?
O31 V1 O30 84.11(8) . . ?
F1 V1 N20 89.99(9) . . ?
F2 V1 N20 89.85(8) . . ?
O31 V1 N20 89.61(9) . . ?
O30 V1 N20 89.16(9) . . ?
F1 V1 N10 89.24(8) . . ?
F2 V1 N10 89.63(8) . . ?
O31 V1 N10 91.03(8) . . ?
O30 V1 N10 91.69(9) . . ?
N20 V1 N10 178.98(9) . . ?

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 1.0(5) . . . . ?
C11 C12 C13 C14 -1.6(5) . . . . ?
C12 C13 C14 C15 1.0(4) . . . . ?
C13 C14 C15 N10 0.2(5) . . . . ?
N20 C21 C22 C23 -0.4(5) . . . . ?
C21 C22 C23 C24 0.1(5) . . . . ?
C22 C23 C24 C25 0.1(5) . . . . ?
C23 C24 C25 N20 0.0(5) . . . . ?
O30 C33 C34 C35 3.0(5) . . . . ?
C32 C33 C34 C35 -174.7(3) . . . . ?
C33 C34 C35 O31 -4.8(5) . . . . ?
C33 C34 C35 C36 173.9(3) . . . . ?
C14 C15 N10 C11 -0.9(4) . . . . ?
C14 C15 N10 V1 173.7(2) . . . . ?
C12 C11 N10 C15 0.3(4) . . . . ?
C12 C11 N10 V1 -174.3(2) . . . . ?
C22 C21 N20 C25 0.5(5) . . . . ?
C22 C21 N20 V1 174.1(2) . . . . ?
C24 C25 N20 C21 -0.3(5) . . . . ?
C24 C25 N20 V1 -173.9(3) . . . . ?
C34 C33 O30 V1 12.8(4) . . . . ?
C32 C33 O30 V1 -169.3(2) . . . . ?
C34 C35 O31 V1 -9.5(5) . . . . ?
C36 C35 O31 V1 171.7(2) . . . . ?

_refine_diff_density_max         0.295
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.060

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1b
_database_code_depnum_ccdc_archive 'CCDC 1063077'
_audit_update_record             
;
2015-06-17 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'trans-difluoridotetrakis(pyridine)vanadium(III) tetrafluoroborate'
_chemical_formula_iupac          '[V (C5 H5 N)4 F2]B F4'
_chemical_formula_moiety         'C20 H20 F2 N4 V 1+, B F4 1-'
_chemical_formula_sum            'C20 H20 B F6 N4 V'
_chemical_formula_weight         492.15

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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   14.0214(17)
_cell_length_b                   12.8277(10)
_cell_length_c                   13.4718(17)
_cell_angle_alpha                90
_cell_angle_beta                 114.259(14)
_cell_angle_gamma                90
_cell_volume                     2209.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    1009
_cell_measurement_theta_min      4.2010
_cell_measurement_theta_max      26.3370
_exptl_crystal_description       coloumn
_exptl_crystal_colour            blue-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.7001
_exptl_crystal_size_mid          0.1845
_exptl_crystal_size_min          0.1596
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)

Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)

Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-15 -9 0 0.0965
10 -1 -18 0.2805
-11 1 19 0.4158
14 -12 0 0.0726
-14 -10 -3 0.1078
-11 -9 -7 0.1521
-17 -9 3 0.1221
-10 1 19 0.4185
15 9 1 0.0914
-14 12 0 0.0870
0 -7 16 0.3258
-13 12 -2 0.0995
3 5 -18 0.2696
-5 -17 0 0.1011
5 17 0 0.0963
12 8 -16 0.2668
-10 -14 10 0.2235
11 14 1 0.0750
13 13 -3 0.1052
-4 -13 13 0.2531
5 -18 -1 0.0872
-18 1 0 0.0870
-10 1 -11 0.1874
-17 1 -2 0.0995
-9 15 -1 0.0963
18 4 -2 0.1127

_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent Sapphire3'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4570
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.635
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2162
_reflns_number_gt                1487
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX (Farrugia, 2012)'

_refine_special_details          
;
The tetrafluoroborate moiety is disordered over a special position of higher
symmetry. It was thus modelled using PART -1 and enhanced rigid-bond restraints
(RIGU) with standard ESDs.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0516P)²+0.5074P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2162
_refine_ls_number_parameters     165
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.1295
_refine_ls_wR_factor_gt          0.1096
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.5300(2) 0.7355(2) 0.2454(2) 0.0417(7) Uani 1 1 d . . . . .
H11 H 0.5227 0.6824 0.1937 0.050 Uiso 1 1 calc R U . . .
C12 C 0.4462(3) 0.7582(3) 0.2703(3) 0.0521(8) Uani 1 1 d . . . . .
H12 H 0.3828 0.7201 0.2373 0.063 Uiso 1 1 calc R U . . .
C13 C 0.4557(3) 0.8367(3) 0.3436(3) 0.0564(9) Uani 1 1 d . . . . .
H13 H 0.3988 0.8533 0.3620 0.068 Uiso 1 1 calc R U . . .
C14 C 0.5479(3) 0.8907(2) 0.3898(2) 0.0487(8) Uani 1 1 d . . . . .
H14 H 0.5558 0.9458 0.4397 0.058 Uiso 1 1 calc R U . . .
C15 C 0.6293(2) 0.8631(2) 0.3621(2) 0.0410(7) Uani 1 1 d . . . . .
H15 H 0.6933 0.9005 0.3943 0.049 Uiso 1 1 calc R U . . .
C21 C 0.7709(2) 0.5193(2) 0.3169(2) 0.0412(7) Uani 1 1 d . . . . .
H21 H 0.7285 0.5103 0.2415 0.049 Uiso 1 1 calc R U . . .
C22 C 0.8041(3) 0.4326(2) 0.3818(3) 0.0463(8) Uani 1 1 d . . . . .
H22 H 0.7843 0.3651 0.3513 0.056 Uiso 1 1 calc R U . . .
C23 C 0.8660(2) 0.4437(2) 0.4912(3) 0.0469(8) Uani 1 1 d . . . . .
H23 H 0.8897 0.3845 0.5374 0.056 Uiso 1 1 calc R U . . .
C24 C 0.8928(2) 0.5433(2) 0.5317(3) 0.0456(8) Uani 1 1 d . . . . .
H24 H 0.9356 0.5539 0.6068 0.055 Uiso 1 1 calc R U . . .
C25 C 0.8572(2) 0.6268(2) 0.4631(2) 0.0410(7) Uani 1 1 d . . . . .
H25 H 0.8765 0.6948 0.4923 0.049 Uiso 1 1 calc R U . . .
N10 N 0.62207(18) 0.78650(16) 0.29227(18) 0.0355(6) Uani 1 1 d . . . . .
N20 N 0.79627(19) 0.61690(16) 0.35631(19) 0.0356(6) Uani 1 1 d . . . . .
F1 F 0.66707(13) 0.66910(12) 0.14344(13) 0.0479(5) Uani 1 1 d . . . . .
V1 V 0.7500 0.7500 0.2500 0.0435(3) Uani 1 2 d S . P . .
B1 B 0.7500 0.1361(4) 0.5000 0.0444(12) Uani 1 2 d S TU P . .
F2 F 0.7153(6) 0.0984(5) 0.3929(5) 0.092(2) Uani 0.5 1 d . U P A -1
F3 F 0.7258(6) 0.0736(5) 0.5611(6) 0.095(2) Uani 0.5 1 d . U P A -1
F4 F 0.8593(4) 0.1369(7) 0.5353(5) 0.142(2) Uani 0.5 1 d . U P A -1
F5 F 0.7120(5) 0.2306(3) 0.4966(7) 0.099(3) Uani 0.5 1 d . U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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 1.351(4) . ?
C11 C12 1.378(4) . ?
C12 C13 1.379(4) . ?
C13 C14 1.370(5) . ?
C14 C15 1.385(4) . ?
C15 N10 1.335(3) . ?
C21 N20 1.349(3) . ?
C21 C22 1.373(4) . ?
C22 C23 1.376(4) . ?
C23 C24 1.380(4) . ?
C24 C25 1.368(4) . ?
C25 N20 1.344(4) . ?
N10 V1 2.145(2) . ?
N20 V1 2.150(2) . ?
F1 V1 1.7658(16) . ?
V1 F1 1.7659(16) 7_665 ?
V1 N10 2.145(2) 7_665 ?
V1 N20 2.150(2) 7_665 ?
B1 F3 1.290(6) . ?
B1 F5 1.317(6) . ?
B1 F4 1.405(6) . ?
B1 F2 1.406(6) . ?

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 122.0(3) . . ?
C11 C12 C13 119.2(3) . . ?
C14 C13 C12 119.3(3) . . ?
C13 C14 C15 118.5(3) . . ?
N10 C15 C14 123.0(3) . . ?
N20 C21 C22 122.4(3) . . ?
C21 C22 C23 119.9(3) . . ?
C22 C23 C24 117.9(3) . . ?
C25 C24 C23 119.6(3) . . ?
N20 C25 C24 123.0(3) . . ?
C15 N10 C11 117.9(3) . . ?
C15 N10 V1 121.20(19) . . ?
C11 N10 V1 120.89(18) . . ?
C25 N20 C21 117.2(2) . . ?
C25 N20 V1 121.56(18) . . ?
C21 N20 V1 121.05(19) . . ?
F1 V1 F1 180.00(9) . 7_665 ?
F1 V1 N10 89.95(8) . 7_665 ?
F1 V1 N10 90.05(8) 7_665 7_665 ?
F1 V1 N10 90.05(8) . . ?
F1 V1 N10 89.95(8) 7_665 . ?
N10 V1 N10 180.0 7_665 . ?
F1 V1 N20 89.57(8) . . ?
F1 V1 N20 90.43(8) 7_665 . ?
N10 V1 N20 86.97(8) 7_665 . ?
N10 V1 N20 93.03(8) . . ?
F1 V1 N20 90.43(8) . 7_665 ?
F1 V1 N20 89.57(8) 7_665 7_665 ?
N10 V1 N20 93.03(8) 7_665 7_665 ?
N10 V1 N20 86.97(8) . 7_665 ?
N20 V1 N20 180.0 . 7_665 ?
F3 B1 F5 112.7(4) . . ?
F3 B1 F4 109.0(5) . . ?
F5 B1 F4 111.9(6) . . ?
F3 B1 F2 111.7(5) . . ?
F5 B1 F2 108.4(5) . . ?
F4 B1 F2 102.7(4) . . ?

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 1.4(5) . . . . ?
C11 C12 C13 C14 0.2(5) . . . . ?
C12 C13 C14 C15 -0.9(5) . . . . ?
C13 C14 C15 N10 0.1(4) . . . . ?
N20 C21 C22 C23 -0.4(4) . . . . ?
C21 C22 C23 C24 -0.1(4) . . . . ?
C22 C23 C24 C25 0.2(4) . . . . ?
C23 C24 C25 N20 0.1(4) . . . . ?
C14 C15 N10 C11 1.4(4) . . . . ?
C14 C15 N10 V1 178.6(2) . . . . ?
C12 C11 N10 C15 -2.1(4) . . . . ?
C12 C11 N10 V1 -179.3(2) . . . . ?
C24 C25 N20 C21 -0.6(4) . . . . ?
C24 C25 N20 V1 -176.3(2) . . . . ?
C22 C21 N20 C25 0.7(4) . . . . ?
C22 C21 N20 V1 176.4(2) . . . . ?

_refine_diff_density_max         0.314
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.062

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1c
_database_code_depnum_ccdc_archive 'CCDC 1063078'
_audit_update_record             
;
2015-06-17 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'pyridinium trans-difluoridotetrakis(pyridine)vanadium(III)hexafluorosilicate'
_chemical_formula_iupac          '(C5 H6 N)[V (C5 H5 N)4 F2]Si F6'
_chemical_formula_moiety         'C20 H20 F2 N4 V 1+, F6 Si 2-, C5 H6 N 1+'
_chemical_formula_sum            'C25 H26 F8 N5 Si V'
_chemical_formula_weight         627.54

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 0.0000 0.0000 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           127
_space_group_name_H-M_alt        'P 4/m b m'
_space_group_name_Hall           '-P 4 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
'-y-1/2, -x-1/2, z'
'y-1/2, x-1/2, z'

_cell_length_a                   10.8047(2)
_cell_length_b                   10.8047(2)
_cell_length_c                   12.6865(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1481.04(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    149.9(10)
_cell_measurement_reflns_used    2992
_cell_measurement_theta_min      4.0880
_cell_measurement_theta_max      29.1910
_exptl_crystal_description       shard
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.3228
_exptl_crystal_size_mid          0.2993
_exptl_crystal_size_min          0.2357
_exptl_absorpt_coefficient_mu    0.449
_shelx_estimated_absorpt_T_min   0.869
_shelx_estimated_absorpt_T_max   0.901
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.907
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)

Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)

Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 18 0.0868
0 -15 5 0.1388
-5 -12 -9 0.0922
8 -11 -7 0.0683
15 2 3 0.1042
9 -9 10 0.1280
-9 12 -2 0.1403
-1 -2 18 0.0920
13 7 5 0.0954
-2 15 0 0.1141
-9 -12 4 0.1253
-13 0 -9 0.1720
4 13 -9 0.1086
2 15 -4 0.0969

_diffrn_orient_matrix_UB_11      0.0403355000
_diffrn_orient_matrix_UB_12      -0.0107619000
_diffrn_orient_matrix_UB_13      -0.0431473000
_diffrn_orient_matrix_UB_21      0.0386566000
_diffrn_orient_matrix_UB_22      0.0490228000
_diffrn_orient_matrix_UB_23      0.0172991000
_diffrn_orient_matrix_UB_31      0.0345016000
_diffrn_orient_matrix_UB_32      -0.0422982000
_diffrn_orient_matrix_UB_33      0.0310539000

_diffrn_ambient_temperature      149.9(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent Sapphire3'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2574
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_av_R_equivalents  0.139
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.772
_diffrn_reflns_theta_max         25.984
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2574
_reflns_number_gt                1293
_reflns_threshold_expression     'I > 2σ(I)'

_twin_formation_mechanism        gt
_twin_dimensionality             triperiodic
_twin_morphology                 simple
_twin_special_details            
;       
Individuals are twinned by rotation of -90.5869° around [0 0 1] in reciprocal
or (0 0 1) in direct space.
;

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.837(2) ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 0.163(2) nmt -0.0088 0.9947 0.0346 -1.0008 -0.0108 0.0218 0.0316 -0.0460
0.9996

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX (Farrugia, 2012)'

_refine_special_details          
;
Refined as a 2-component twin.

The pyridinium ion is rotationally disordered over a special position with two
symmetry-independent atom positions. It was modelled as an occupationally
disordered species with a C/N ratio of 0.375:0.125 in one position to keep
the stoichiometry correct. The position was chosen because of the possibility
of hydrogen bonding.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0774P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2574
_refine_ls_number_parameters     60
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0508
_refine_ls_wR_factor_ref         0.1325
_refine_ls_wR_factor_gt          0.1201
_refine_ls_goodness_of_fit_ref   0.844
_refine_ls_restrained_S_all      0.844
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.4475(3) 0.2022(3) 0.1619(3) 0.0452(8) Uani 1 1 d . . . . .
H11 H 0.5219 0.2355 0.1339 0.054 Uiso 1 1 calc R U . . .
C12 C 0.3898(3) 0.2637(3) 0.2435(3) 0.0576(10) Uani 1 1 d . . . . .
H12 H 0.4243 0.3377 0.2713 0.069 Uiso 1 1 calc R U . . .
C13 C 0.2828(3) 0.2172(3) 0.2838(4) 0.0616(15) Uani 1 2 d S T P . .
H13 H 0.2411 0.2589 0.3394 0.074 Uiso 1 2 calc R U P . .
N10 N 0.4027(2) 0.0973(2) 0.1207(3) 0.0337(8) Uani 1 2 d S T P . .
F1 F 0.3847(2) -0.1153(2) 0.0000 0.0460(9) Uani 1 4 d S T P . .
V1 V 0.5000 0.0000 0.0000 0.0347(4) Uani 1 8 d S T P . .
F2 F 0.61482(18) 0.60640(18) 0.5000 0.0388(6) Uani 1 2 d S T P . .
F3 F 0.5000 0.5000 0.3675(3) 0.0427(9) Uani 1 4 d S T P . .
Si2 Si 0.5000 0.5000 0.5000 0.0259(5) Uani 1 8 d S T P . .
C20 C 0.5304(5) 0.8792(4) 0.5000 0.0629(15) Uani 0.75 2 d S T P A 1
H20A H 0.5532 0.7943 0.5000 0.075 Uiso 0.75 2 calc R U P A 1
N20 N 0.5304(5) 0.8792(4) 0.5000 0.0629(15) Uani 0.25 2 d S T P A 2
H20B H 0.5516 0.8006 0.5000 0.075 Uiso 0.25 2 calc R U P A 2
C21 C 0.4109(4) 0.9109(4) 0.5000 0.060(2) Uani 1 4 d S T P . .
H21 H 0.3488 0.8488 0.5000 0.072 Uiso 1 4 calc R U P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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 1.339(3) . ?
C11 C12 1.380(5) . ?
C12 C13 1.360(4) . ?
N10 C11 1.339(3) 15_665 ?
N10 V1 2.134(3) . ?
F1 V1 1.762(3) . ?
V1 F1 1.762(3) 9_655 ?
V1 N10 2.134(3) 2_655 ?
F2 Si2 1.691(2) . ?
F3 Si2 1.681(3) . ?
Si2 F3 1.681(3) 9_666 ?
Si2 F2 1.691(2) 3_655 ?
C20 C21 1.335(6) . ?
C20 C20 1.381(10) 15_775 ?
N20 C21 1.335(6) . ?

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 122.5(3) . . ?
C13 C12 C11 119.2(4) . . ?
C12 C13 C12 119.2(5) 15_665 . ?
C11 N10 C11 117.4(4) 15_665 . ?
C11 N10 V1 121.27(19) 15_665 . ?
C11 N10 V1 121.27(19) . . ?
F1 V1 F1 180.00(19) . 9_655 ?
F1 V1 N10 90.0 . 10 ?
F1 V1 N10 90.0 9_655 10 ?
F1 V1 N10 90.0 . 9_655 ?
F1 V1 N10 90.0 9_655 9_655 ?
N10 V1 N10 88.33(18) 10 9_655 ?
F1 V1 N10 90.0 . 2_655 ?
F1 V1 N10 90.0 9_655 2_655 ?
N10 V1 N10 180.0(2) 10 2_655 ?
N10 V1 N10 91.67(18) 9_655 2_655 ?
F1 V1 N10 90.000(1) . . ?
F1 V1 N10 90.0 9_655 . ?
N10 V1 N10 91.67(18) 10 . ?
N10 V1 N10 180.0 9_655 . ?
N10 V1 N10 88.33(18) 2_655 . ?
F3 Si2 F3 180.0 9_666 . ?
F3 Si2 F2 90.000(1) 9_666 9_666 ?
F3 Si2 F2 90.000(1) . 9_666 ?
F3 Si2 F2 90.0 9_666 11_566 ?
F3 Si2 F2 90.0 . 11_566 ?
F2 Si2 F2 90.0 9_666 11_566 ?
F3 Si2 F2 90.0 9_666 3_655 ?
F3 Si2 F2 90.0 . 3_655 ?
F2 Si2 F2 90.0 9_666 3_655 ?
F2 Si2 F2 180.0 11_566 3_655 ?
F3 Si2 F2 90.000(1) 9_666 . ?
F3 Si2 F2 90.0 . . ?
F2 Si2 F2 180.0 9_666 . ?
F2 Si2 F2 90.0 11_566 . ?
F2 Si2 F2 90.000(1) 3_655 . ?
C21 C20 C20 120.1(3) . 15_775 ?
C21 N20 N20 120.1(3) . 15_775 ?
C20 C21 C20 119.7(6) 7_456 . ?
N20 C21 N20 119.7(6) 7_456 . ?

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 -0.4(6) . . . . ?
C11 C12 C13 C12 0.8(7) . . . 15_665 ?
C12 C11 N10 C11 -0.1(6) . . . 15_665 ?
C12 C11 N10 V1 -176.7(3) . . . . ?
C20 C20 C21 C20 0.0 15_775 . . 7_456 ?
N20 N20 C21 N20 0.0 15_775 . . 7_456 ?

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
N20 H20B F2 0.88 2.21 3.086(5) 177.0 .

_refine_diff_density_max         0.509
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.066

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1e
_database_code_depnum_ccdc_archive 'CCDC 1063080'
_audit_update_record             
;
2015-06-17 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'pyridinium trans-tetrafluoridobis(pyridine)vanadate(III)--ethanol (3/2)'
_chemical_formula_iupac          '(C5 H6 N)[V (C5 H5 N)2 F4].0.67C2 H5 O H'
_chemical_formula_moiety         
'3(C10 H10 F4 N2 V 1-), 3(C5 H6 N 1+), 2(C2 H6 O)'
_chemical_formula_sum            'C49 H60 F12 N9 O2 V3'
_chemical_formula_weight         1187.88

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 0.0000 0.0000 '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'
O O 0.0106 0.0060 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.4345(6)
_cell_length_b                   31.4088(12)
_cell_length_c                   10.9799(6)
_cell_angle_alpha                90
_cell_angle_beta                 111.971(7)
_cell_angle_gamma                90
_cell_volume                     2697.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    2992
_cell_measurement_theta_min      3.6880
_cell_measurement_theta_max      31.0650
_exptl_crystal_description       plate
_exptl_crystal_colour            black-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.5856
_exptl_crystal_size_mid          0.3846
_exptl_crystal_size_min          0.1755
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)

Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.

(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 -26 -10 0.2078
0 -24 12 0.1503
0 23 -12 0.1857
-11 0 11 0.0907
11 -3 -11 0.0688
2 44 -1 0.3406
1 4 13 0.1891
2 23 11 0.2058
10 13 -11 0.1424
-8 -24 -4 0.2274
-3 25 -10 0.2053
4 -21 -13 0.1712

_diffrn_special_details          
;
Because the crystal system seemed to be orthorhombic initially, an inappropriate
data-collection strategy was chosen. The completeness is thus too low.
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent Sapphire3'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11455
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.677
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measured_fraction_theta_full 0.891
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_Laue_measured_fraction_full 0.891
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_point_group_measured_fraction_full 0.891
_reflns_number_total             4725
_reflns_number_gt                3538
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX (Farrugia, 2012)'

_refine_special_details          
;
One pyridinium ion is rotationally disordered over a special position with three
symmetry-independent atom positions. It was modelled as an occupationally
disordered species with a C/N ratio of 0.5:0.5 in one position to keep
the stoichiometry correct. The position was chosen because of the possibility
of hydrogen bonding and the found electron density.

The oxygen-borne hydrogen atom was refined with a 1,2-distance restraint
(0.84 Å) and Uiso[H] = 1.2 Ueq[O]. The nitrogen-borne hydrogen atom in
the disordered pyridinium ion was fully constrained to the nitrogen atom. The
one in the ordered pyridinium ion was refined with a 1,2-distance restraint
(0.88 Å), a same-1,3-distance restraint and Uiso[H] = 1.2 Ueq[N].
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0362P)²+2.2766P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4725
_refine_ls_number_parameters     347
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1114
_refine_ls_wR_factor_gt          0.0998
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
_restr_distance_details
O60 H60 0.84 0.02 -0.01 'generated by SHELXL DFIX'
N40 H40 0.88 0.02 0.04 'generated by SHELXL DFIX'
N50 C50 0.0 0.0 0.0 'generated by SHELXL EXYZ'

loop_
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
_restr_equal_distance_class_average
_restr_equal_distance_class_esd
_restr_equal_distance_class_diff_max
_restr_equal_distance_class_details
1 0.02 1.957 0.015 0.008 'generated by SHELXL SADI'

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_class_id
_restr_equal_distance_details
C41 H40 1 'equal C41-H40 and C45-H40'
C45 H40 1 'equal C41-H40 and C45-H40'

loop_
_restr_U_similar_atom_site_label_1
_restr_U_similar_atom_site_label_2
_restr_U_similar_weight_param
N50 C50 0.0

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.0971(5) 0.61363(10) 0.5224(4) 0.0337(9) Uani 1 1 d . . . . .
H11 H 0.0917 0.6112 0.4347 0.040 Uiso 1 1 calc R U . . .
C12 C -0.0309(5) 0.59538(11) 0.5537(4) 0.0411(10) Uani 1 1 d . . . . .
H12 H -0.1234 0.5811 0.4885 0.049 Uiso 1 1 calc R U . . .
C13 C -0.0227(5) 0.59811(11) 0.6813(4) 0.0373(10) Uani 1 1 d . . . . .
H13 H -0.1087 0.5856 0.7061 0.045 Uiso 1 1 calc R U . . .
C14 C 0.1120(5) 0.61929(11) 0.7713(4) 0.0358(9) Uani 1 1 d . . . . .
H14 H 0.1205 0.6217 0.8598 0.043 Uiso 1 1 calc R U . . .
C15 C 0.2359(5) 0.63727(10) 0.7330(3) 0.0286(8) Uani 1 1 d . . . . .
H15 H 0.3289 0.6519 0.7965 0.034 Uiso 1 1 calc R U . . .
C21 C 0.7601(5) 0.69610(10) 0.5429(4) 0.0300(8) Uani 1 1 d . . . . .
H21 H 0.8021 0.6768 0.6144 0.036 Uiso 1 1 calc R U . . .
C22 C 0.8769(5) 0.71591(10) 0.4994(4) 0.0333(9) Uani 1 1 d . . . . .
H22 H 0.9955 0.7098 0.5396 0.040 Uiso 1 1 calc R U . . .
C23 C 0.8185(5) 0.74424(11) 0.3983(4) 0.0363(10) Uani 1 1 d . . . . .
H23 H 0.8952 0.7580 0.3659 0.044 Uiso 1 1 calc R U . . .
C24 C 0.6450(5) 0.75252(11) 0.3439(4) 0.0379(9) Uani 1 1 d . . . . .
H24 H 0.6014 0.7729 0.2754 0.045 Uiso 1 1 calc R U . . .
C25 C 0.5354(5) 0.73104(10) 0.3895(3) 0.0305(8) Uani 1 1 d . . . . .
H25 H 0.4161 0.7363 0.3495 0.037 Uiso 1 1 calc R U . . .
N10 N 0.2289(4) 0.63471(7) 0.6092(3) 0.0238(6) Uani 1 1 d . . . . .
N20 N 0.5926(4) 0.70289(8) 0.4890(3) 0.0237(6) Uani 1 1 d . . . . .
F1 F 0.3530(3) 0.63241(5) 0.39952(18) 0.0276(5) Uani 1 1 d . . . . .
F2 F 0.5866(3) 0.62708(6) 0.6419(2) 0.0390(5) Uani 1 1 d . . . . .
F3 F 0.4786(3) 0.70065(6) 0.70695(19) 0.0370(5) Uani 1 1 d . . . . .
F4 F 0.2419(2) 0.70739(5) 0.45996(19) 0.0275(5) Uani 1 1 d . . . . .
V1 V 0.41388(7) 0.66813(2) 0.55177(5) 0.02027(15) Uani 1 1 d . . . . .
C31 C 0.8066(5) 0.49495(10) 1.1879(3) 0.0299(8) Uani 1 1 d . . . . .
H31 H 0.8996 0.5121 1.2407 0.036 Uiso 1 1 calc R U . . .
C32 C 0.6838(5) 0.48387(11) 1.2362(4) 0.0372(9) Uani 1 1 d . . . . .
H32 H 0.6914 0.4937 1.3200 0.045 Uiso 1 1 calc R U . . .
C33 C 0.5493(5) 0.45832(11) 1.1622(4) 0.0349(9) Uani 1 1 d . . . . .
H33 H 0.4645 0.4497 1.1946 0.042 Uiso 1 1 calc R U . . .
C34 C 0.5414(5) 0.44563(10) 1.0398(4) 0.0318(9) Uani 1 1 d . . . . .
H34 H 0.4495 0.4284 0.9857 0.038 Uiso 1 1 calc R U . . .
C35 C 0.6683(5) 0.45823(9) 0.9966(3) 0.0268(8) Uani 1 1 d . . . . .
H35 H 0.6616 0.4493 0.9121 0.032 Uiso 1 1 calc R U . . .
N30 N 0.8009(4) 0.48255(8) 1.0694(3) 0.0235(6) Uani 1 1 d . . . . .
F5 F 0.8618(3) 0.54555(5) 0.89706(18) 0.0284(5) Uani 1 1 d . . . . .
F6 F 0.9097(2) 0.46207(5) 0.85724(18) 0.0278(4) Uani 1 1 d . . . . .
V2 V 1.0000 0.5000 1.0000 0.02002(19) Uani 1 2 d S . P . .
C41 C 0.7919(5) 0.65098(12) 0.9350(4) 0.0359(9) Uani 1 1 d D . . . .
H41 H 0.7139 0.6418 0.8516 0.043 Uiso 1 1 calc R U . . .
C42 C 0.7905(5) 0.69197(12) 0.9737(4) 0.0384(10) Uani 1 1 d . . . . .
H42 H 0.7110 0.7116 0.9174 0.046 Uiso 1 1 calc R U . . .
C43 C 0.9037(5) 0.70501(10) 1.0941(4) 0.0352(9) Uani 1 1 d . . . . .
H43 H 0.9041 0.7336 1.1222 0.042 Uiso 1 1 calc R U . . .
C44 C 1.0177(5) 0.67534(12) 1.1741(4) 0.0395(10) Uani 1 1 d . . . . .
H44 H 1.0969 0.6836 1.2581 0.047 Uiso 1 1 calc R U . . .
C45 C 1.0162(5) 0.63498(11) 1.1327(4) 0.0374(9) Uani 1 1 d D . . . .
H45 H 1.0949 0.6148 1.1871 0.045 Uiso 1 1 calc R U . . .
N40 N 0.9048(5) 0.62336(9) 1.0157(4) 0.0418(9) Uani 1 1 d D . . . .
H40 H 0.905(3) 0.5957(6) 0.989(2) 0.050 Uiso 1 1 d D U . . .
N50 N 0.5274(4) 0.54199(9) 0.5357(3) 0.0281(7) Uani 0.5 1 d . . P A 1
H50A H 0.5445 0.5689 0.5588 0.034 Uiso 0.5 1 calc R U P A 1
C50 C 0.5274(4) 0.54199(9) 0.5357(3) 0.0281(7) Uani 0.5 1 d . . P A 2
H50B H 0.5459 0.5711 0.5607 0.034 Uiso 0.5 1 calc R U P A 2
C51 C 0.6345(5) 0.51114(11) 0.6124(3) 0.0312(8) Uani 1 1 d . . . . .
H51 H 0.7280 0.5188 0.6899 0.037 Uiso 1 1 calc R U . A 1
C52 C 0.3953(5) 0.53075(11) 0.4243(3) 0.0309(8) Uani 1 1 d . . . . .
H52 H 0.3225 0.5522 0.3711 0.037 Uiso 1 1 calc R U . A 1
C61 C 0.6169(5) 0.63462(12) 0.2260(4) 0.0411(10) Uani 1 1 d . . . . .
H61A H 0.6932 0.6234 0.1835 0.049 Uiso 1 1 calc R U . . .
H61B H 0.6844 0.6545 0.2963 0.049 Uiso 1 1 calc R U . . .
C62 C 0.4724(6) 0.65851(12) 0.1261(4) 0.0496(12) Uani 1 1 d . . . . .
H62A H 0.4088 0.6393 0.0539 0.074 Uiso 1 1 calc R U . . .
H62B H 0.5183 0.6823 0.0919 0.074 Uiso 1 1 calc R U . . .
H62C H 0.3958 0.6694 0.1674 0.074 Uiso 1 1 calc R U . . .
O60 O 0.5592(4) 0.60031(8) 0.2829(3) 0.0429(7) Uani 1 1 d D . . . .
H60 H 0.497(5) 0.6094(11) 0.321(4) 0.051 Uiso 1 1 d D U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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 1.338(4) . ?
C11 C12 1.375(5) . ?
C12 C13 1.379(5) . ?
C13 C14 1.368(5) . ?
C14 C15 1.384(5) . ?
C15 N10 1.341(4) . ?
C21 N20 1.329(4) . ?
C21 C22 1.392(5) . ?
C22 C23 1.363(5) . ?
C23 C24 1.383(5) . ?
C24 C25 1.381(5) . ?
C25 N20 1.346(4) . ?
N10 V1 2.161(3) . ?
N20 V1 2.171(3) . ?
F1 V1 1.9170(18) . ?
F2 V1 1.919(2) . ?
F3 V1 1.8837(19) . ?
F4 V1 1.8832(19) . ?
C31 N30 1.342(4) . ?
C31 C32 1.374(5) . ?
C32 C33 1.378(5) . ?
C33 C34 1.379(5) . ?
C34 C35 1.381(4) . ?
C35 N30 1.343(4) . ?
N30 V2 2.158(3) . ?
F5 V2 1.9229(18) . ?
F6 V2 1.8876(17) . ?
V2 F6 1.8876(18) 3_767 ?
V2 F5 1.9229(18) 3_767 ?
V2 N30 2.158(3) 3_767 ?
C41 N40 1.347(5) . ?
C41 C42 1.357(5) . ?
C42 C43 1.372(5) . ?
C43 C44 1.390(5) . ?
C44 C45 1.345(5) . ?
C45 N40 1.328(5) . ?
N50 C52 1.357(5) . ?
N50 C51 1.376(5) . ?
C50 C52 1.357(5) . ?
C50 C51 1.376(5) . ?
C51 C52 1.371(5) 3_666 ?
C52 C51 1.372(5) 3_666 ?
C61 O60 1.420(4) . ?
C61 C62 1.500(6) . ?

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 123.3(3) . . ?
C11 C12 C13 118.8(4) . . ?
C14 C13 C12 118.5(3) . . ?
C13 C14 C15 119.8(3) . . ?
N10 C15 C14 122.1(4) . . ?
N20 C21 C22 123.2(3) . . ?
C23 C22 C21 119.0(4) . . ?
C22 C23 C24 118.4(3) . . ?
C25 C24 C23 119.7(3) . . ?
N20 C25 C24 122.0(4) . . ?
C11 N10 C15 117.5(3) . . ?
C11 N10 V1 122.0(2) . . ?
C15 N10 V1 120.3(2) . . ?
C21 N20 C25 117.7(3) . . ?
C21 N20 V1 121.8(2) . . ?
C25 N20 V1 120.5(2) . . ?
F4 V1 F3 91.94(9) . . ?
F4 V1 F1 90.87(8) . . ?
F3 V1 F1 176.93(9) . . ?
F4 V1 F2 178.54(9) . . ?
F3 V1 F2 89.47(10) . . ?
F1 V1 F2 87.72(9) . . ?
F4 V1 N10 88.78(9) . . ?
F3 V1 N10 89.77(9) . . ?
F1 V1 N10 89.04(9) . . ?
F2 V1 N10 90.84(9) . . ?
F4 V1 N20 89.32(9) . . ?
F3 V1 N20 90.79(9) . . ?
F1 V1 N20 90.49(9) . . ?
F2 V1 N20 91.05(10) . . ?
N10 V1 N20 178.04(11) . . ?
N30 C31 C32 122.8(4) . . ?
C31 C32 C33 119.6(3) . . ?
C32 C33 C34 118.1(3) . . ?
C33 C34 C35 119.4(4) . . ?
N30 C35 C34 122.6(3) . . ?
C31 N30 C35 117.5(3) . . ?
C31 N30 V2 121.2(2) . . ?
C35 N30 V2 121.3(2) . . ?
F6 V2 F6 180.0 3_767 . ?
F6 V2 F5 90.80(8) 3_767 3_767 ?
F6 V2 F5 89.20(8) . 3_767 ?
F6 V2 F5 89.20(8) 3_767 . ?
F6 V2 F5 90.80(8) . . ?
F5 V2 F5 180.0 3_767 . ?
F6 V2 N30 89.58(9) 3_767 . ?
F6 V2 N30 90.41(9) . . ?
F5 V2 N30 89.09(9) 3_767 . ?
F5 V2 N30 90.91(9) . . ?
F6 V2 N30 90.41(9) 3_767 3_767 ?
F6 V2 N30 89.59(9) . 3_767 ?
F5 V2 N30 90.91(9) 3_767 3_767 ?
F5 V2 N30 89.09(9) . 3_767 ?
N30 V2 N30 180.0 . 3_767 ?
N40 C41 C42 119.4(4) . . ?
C41 C42 C43 120.0(4) . . ?
C42 C43 C44 118.4(3) . . ?
C45 C44 C43 120.1(4) . . ?
N40 C45 C44 120.0(4) . . ?
C45 N40 C41 122.0(3) . . ?
C52 N50 C51 119.9(3) . . ?
C52 C50 C51 119.9(3) . . ?
C52 C51 N50 119.3(3) 3_666 . ?
C52 C51 C50 119.3(3) 3_666 . ?
C50 C52 C51 120.8(3) . 3_666 ?
N50 C52 C51 120.8(3) . 3_666 ?
O60 C61 C62 112.5(3) . . ?

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 -1.2(6) . . . . ?
C11 C12 C13 C14 0.6(6) . . . . ?
C12 C13 C14 C15 -0.1(5) . . . . ?
C13 C14 C15 N10 0.0(5) . . . . ?
N20 C21 C22 C23 1.1(5) . . . . ?
C21 C22 C23 C24 0.8(5) . . . . ?
C22 C23 C24 C25 -2.3(5) . . . . ?
C23 C24 C25 N20 2.0(5) . . . . ?
C12 C11 N10 C15 1.1(5) . . . . ?
C12 C11 N10 V1 -173.9(3) . . . . ?
C14 C15 N10 C11 -0.5(5) . . . . ?
C14 C15 N10 V1 174.6(2) . . . . ?
C22 C21 N20 C25 -1.4(5) . . . . ?
C22 C21 N20 V1 175.9(2) . . . . ?
C24 C25 N20 C21 -0.2(5) . . . . ?
C24 C25 N20 V1 -177.5(3) . . . . ?
N30 C31 C32 C33 1.1(6) . . . . ?
C31 C32 C33 C34 -1.6(6) . . . . ?
C32 C33 C34 C35 1.0(5) . . . . ?
C33 C34 C35 N30 0.1(5) . . . . ?
C32 C31 N30 C35 -0.1(5) . . . . ?
C32 C31 N30 V2 -178.9(3) . . . . ?
C34 C35 N30 C31 -0.5(5) . . . . ?
C34 C35 N30 V2 178.3(2) . . . . ?
N40 C41 C42 C43 0.2(5) . . . . ?
C41 C42 C43 C44 -0.2(5) . . . . ?
C42 C43 C44 C45 0.4(5) . . . . ?
C43 C44 C45 N40 -0.5(5) . . . . ?
C44 C45 N40 C41 0.5(5) . . . . ?
C42 C41 N40 C45 -0.3(5) . . . . ?
C52 N50 C51 C52 -0.8(5) . . . 3_666 ?
C52 C50 C51 C52 -0.8(5) . . . 3_666 ?
C51 C50 C52 C51 0.8(5) . . . 3_666 ?
C51 N50 C52 C51 0.8(5) . . . 3_666 ?

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
N40 H40 F5 0.920(18) 1.829(19) 2.729(3) 165.4(16) .
N50 H50A F2 0.88 2.01 2.884(4) 170.3 .
O60 H60 F1 0.835(18) 1.876(19) 2.710(3) 177(4) .

_refine_diff_density_max         0.565
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.065

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2a
_database_code_depnum_ccdc_archive 'CCDC 1063081'
_audit_update_record             
;
2015-06-17 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
trans-difluoridotetrakis(pyridine)managnese(III)pentafluorido(pyridine)silicate(IV)
_chemical_formula_iupac          '[Mn (C5 H5 N)4 F2][Si (C5 H5 N) F5]'
_chemical_formula_moiety         'C20 H20 F2 Mn N4 1+, C5 H5 F5 N Si 1-'
_chemical_formula_sum            'C25 H25 F7 Mn N5 Si'
_chemical_formula_weight         611.53

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 0.0000 0.0000 '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'
Mn Mn 0.3368 0.7283 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.4549(11)
_cell_length_b                   10.3397(5)
_cell_length_c                   11.9769(7)
_cell_angle_alpha                90
_cell_angle_beta                 98.648(5)
_cell_angle_gamma                90
_cell_volume                     2626.7(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    2335
_cell_measurement_theta_min      3.9600
_cell_measurement_theta_max      31.7500
_exptl_crystal_description       irregular
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.6732
_exptl_crystal_size_mid          0.5117
_exptl_crystal_size_min          0.2753
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)

Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)

Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
30 0 1 0.0883
-8 -14 -1 0.2800
-26 -7 -1 0.1940
-30 -1 -1 0.1794
-29 3 0 0.2065
-22 10 0 0.2928
14 13 1 0.3051
-4 -14 5 0.2501
-11 -9 12 0.2501
-14 0 16 0.1941
10 -11 -10 0.3659
14 -1 -16 0.2712
10 10 -12 0.3157
7 13 -8 0.3319
14 1 -16 0.2625
-3 14 2 0.3545
-23 1 -9 0.1894
-15 -10 -7 0.2744
-21 7 -7 0.2209
19 -9 7 0.2169
23 5 7 0.2021
17 -7 10 0.2283
-26 -5 -4 0.1847
-28 0 -4 0.1777
-6 10 -11 0.2885
-5 -9 -13 0.3226
6 -12 9 0.2368
24 0 -12 0.2256
-7 1 -16 0.2659
21 8 -9 0.2874
-22 -9 6 0.2250
-27 -1 9 0.2022

_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent Sapphire3'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5581
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.441
_diffrn_reflns_theta_max         25.989
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2590
_reflns_number_gt                2331
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX (Farrugia, 2012)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0328P)²+1.9060P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2590
_refine_ls_number_parameters     180
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0324
_refine_ls_wR_factor_ref         0.0768
_refine_ls_wR_factor_gt          0.0743
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.32541(9) 0.10415(17) 0.20947(16) 0.0260(4) Uani 1 1 d . . . . .
H11 H 0.3380 0.0526 0.1511 0.031 Uiso 1 1 calc R U . . .
C12 C 0.35173(9) 0.07887(19) 0.31983(17) 0.0306(4) Uani 1 1 d . . . . .
H12 H 0.3810 0.0101 0.3369 0.037 Uiso 1 1 calc R U . . .
C13 C 0.33470(10) 0.1556(2) 0.40499(17) 0.0348(5) Uani 1 1 d . . . . .
H13 H 0.3529 0.1421 0.4814 0.042 Uiso 1 1 calc R U . . .
C14 C 0.29060(11) 0.25226(19) 0.37670(16) 0.0331(5) Uani 1 1 d . . . . .
H14 H 0.2779 0.3059 0.4336 0.040 Uiso 1 1 calc R U . . .
C15 C 0.26522(9) 0.26992(17) 0.26480(16) 0.0274(4) Uani 1 1 d . . . . .
H15 H 0.2342 0.3351 0.2463 0.033 Uiso 1 1 calc R U . . .
C21 C 0.17013(9) 0.01834(17) -0.08416(15) 0.0264(4) Uani 1 1 d . . . . .
H21 H 0.1997 0.0138 -0.1356 0.032 Uiso 1 1 calc R U . . .
C22 C 0.12282(9) -0.07255(18) -0.09199(17) 0.0302(4) Uani 1 1 d . . . . .
H22 H 0.1191 -0.1370 -0.1492 0.036 Uiso 1 1 calc R U . . .
C23 C 0.08078(9) -0.06847(19) -0.01520(17) 0.0318(5) Uani 1 1 d . . . . .
H23 H 0.0484 -0.1315 -0.0177 0.038 Uiso 1 1 calc R U . . .
C24 C 0.08636(9) 0.02862(19) 0.06564(17) 0.0311(4) Uani 1 1 d . . . . .
H24 H 0.0580 0.0332 0.1193 0.037 Uiso 1 1 calc R U . . .
C25 C 0.13400(9) 0.11845(18) 0.06634(15) 0.0256(4) Uani 1 1 d . . . . .
H25 H 0.1372 0.1864 0.1202 0.031 Uiso 1 1 calc R U . . .
F1 F 0.19999(5) 0.37161(9) 0.04510(9) 0.0262(2) Uani 1 1 d . . . . .
Mn1 Mn 0.2500 0.2500 0.0000 0.01966(11) Uani 1 2 d S . P . .
N10 N 0.28281(7) 0.19836(14) 0.18090(12) 0.0234(3) Uani 1 1 d . . . . .
N20 N 0.17608(7) 0.11352(14) -0.00634(12) 0.0223(3) Uani 1 1 d . . . . .
C31 C -0.01919(9) 0.58933(18) 0.15468(15) 0.0249(4) Uani 1 1 d . . . . .
H31 H -0.0328 0.5428 0.0870 0.030 Uiso 1 1 calc R U . . .
C32 C -0.01992(10) 0.72272(19) 0.15155(17) 0.0317(5) Uani 1 1 d . . . . .
H32 H -0.0339 0.7671 0.0829 0.038 Uiso 1 1 calc R U . . .
C33 C 0.0000 0.7912(3) 0.2500 0.0359(7) Uani 1 2 d S T P . .
H33 H 0.0000 0.8830 0.2500 0.043 Uiso 1 2 calc R U P . .
F2 F 0.02262(7) 0.33613(11) 0.12309(9) 0.0401(3) Uani 1 1 d . . . . .
F3 F -0.07526(6) 0.33906(10) 0.18983(11) 0.0389(3) Uani 1 1 d . . . . .
F4 F 0.0000 0.16708(14) 0.2500 0.0326(4) Uani 1 2 d S T P . .
N30 N 0.0000 0.52281(19) 0.2500 0.0202(4) Uani 1 2 d S T P . .
Si1 Si 0.0000 0.32785(6) 0.2500 0.02244(17) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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 1.344(2) . ?
C11 C12 1.382(3) . ?
C12 C13 1.384(3) . ?
C13 C14 1.383(3) . ?
C14 C15 1.381(3) . ?
C15 N10 1.347(2) . ?
C21 N20 1.348(2) . ?
C21 C22 1.376(3) . ?
C22 C23 1.382(3) . ?
C23 C24 1.387(3) . ?
C24 C25 1.380(3) . ?
C25 N20 1.346(2) . ?
F1 Mn1 1.7884(10) . ?
Mn1 F1 1.7884(10) 7 ?
Mn1 N20 2.1157(15) . ?
Mn1 N20 2.1157(15) 7 ?
Mn1 N10 2.2397(15) 7 ?
Mn1 N10 2.2397(15) . ?
C31 N30 1.343(2) . ?
C31 C32 1.380(3) . ?
C32 C33 1.386(2) . ?
C33 C32 1.387(2) 2 ?
F2 Si1 1.6658(11) . ?
F3 Si1 1.6703(12) . ?
F4 Si1 1.6623(15) . ?
N30 C31 1.343(2) 2 ?
N30 Si1 2.016(2) . ?
Si1 F2 1.6658(11) 2 ?
Si1 F3 1.6703(12) 2 ?

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 123.02(18) . . ?
C11 C12 C13 118.78(19) . . ?
C14 C13 C12 118.71(19) . . ?
C15 C14 C13 119.26(18) . . ?
N10 C15 C14 122.53(18) . . ?
N20 C21 C22 122.53(18) . . ?
C21 C22 C23 118.83(18) . . ?
C22 C23 C24 119.35(18) . . ?
C25 C24 C23 118.50(18) . . ?
N20 C25 C24 122.60(17) . . ?
F1 Mn1 F1 180.0 . 7 ?
F1 Mn1 N20 89.96(5) . . ?
F1 Mn1 N20 90.04(5) 7 . ?
F1 Mn1 N20 90.04(5) . 7 ?
F1 Mn1 N20 89.96(5) 7 7 ?
N20 Mn1 N20 180.0 . 7 ?
F1 Mn1 N10 90.51(5) . 7 ?
F1 Mn1 N10 89.49(5) 7 7 ?
N20 Mn1 N10 89.97(5) . 7 ?
N20 Mn1 N10 90.03(5) 7 7 ?
F1 Mn1 N10 89.49(5) . . ?
F1 Mn1 N10 90.51(5) 7 . ?
N20 Mn1 N10 90.03(5) . . ?
N20 Mn1 N10 89.97(5) 7 . ?
N10 Mn1 N10 180.0 7 . ?
C11 N10 C15 117.66(16) . . ?
C11 N10 Mn1 121.45(12) . . ?
C15 N10 Mn1 120.55(12) . . ?
C25 N20 C21 118.15(16) . . ?
C25 N20 Mn1 121.57(12) . . ?
C21 N20 Mn1 120.28(12) . . ?
N30 C31 C32 122.39(18) . . ?
C31 C32 C33 119.10(19) . . ?
C32 C33 C32 118.6(3) . 2 ?
C31 N30 C31 118.4(2) 2 . ?
C31 N30 Si1 120.80(11) 2 . ?
C31 N30 Si1 120.80(11) . . ?
F4 Si1 F2 92.95(4) . 2 ?
F4 Si1 F2 92.95(4) . . ?
F2 Si1 F2 174.11(9) 2 . ?
F4 Si1 F3 93.98(4) . 2 ?
F2 Si1 F3 89.89(7) 2 2 ?
F2 Si1 F3 89.70(7) . 2 ?
F4 Si1 F3 93.98(4) . . ?
F2 Si1 F3 89.70(7) 2 . ?
F2 Si1 F3 89.89(7) . . ?
F3 Si1 F3 172.04(9) 2 . ?
F4 Si1 N30 180.0 . . ?
F2 Si1 N30 87.05(4) 2 . ?
F2 Si1 N30 87.05(4) . . ?
F3 Si1 N30 86.02(4) 2 . ?
F3 Si1 N30 86.02(4) . . ?

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(3) . . . . ?
C11 C12 C13 C14 1.8(3) . . . . ?
C12 C13 C14 C15 -0.4(3) . . . . ?
C13 C14 C15 N10 -1.6(3) . . . . ?
N20 C21 C22 C23 -1.9(3) . . . . ?
C21 C22 C23 C24 1.6(3) . . . . ?
C22 C23 C24 C25 0.1(3) . . . . ?
C23 C24 C25 N20 -1.7(3) . . . . ?
C12 C11 N10 C15 -0.4(3) . . . . ?
C12 C11 N10 Mn1 172.89(13) . . . . ?
C14 C15 N10 C11 2.0(3) . . . . ?
C14 C15 N10 Mn1 -171.38(14) . . . . ?
C24 C25 N20 C21 1.5(3) . . . . ?
C24 C25 N20 Mn1 -178.33(13) . . . . ?
C22 C21 N20 C25 0.3(3) . . . . ?
C22 C21 N20 Mn1 -179.83(14) . . . . ?
N30 C31 C32 C33 0.2(3) . . . . ?
C31 C32 C33 C32 -0.09(13) . . . 2 ?
C32 C31 N30 C31 -0.11(14) . . . 2 ?
C32 C31 N30 Si1 179.90(14) . . . . ?

_refine_diff_density_max         0.261
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.047

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2b
_database_code_depnum_ccdc_archive 'CCDC 1063082'
_audit_update_record             
;
2015-06-17 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        mer-trifluoridotris(pyridine)manganese(III)
_chemical_formula_iupac          '[Mn (C5 H5 N)3 F3]'
_chemical_formula_moiety         'C15 H15 F3 Mn N3'
_chemical_formula_sum            'C15 H15 F3 Mn N3'
_chemical_formula_weight         349.24

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 0.0000 0.0000 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P c'
_space_group_name_Hall           'P -2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'

_cell_length_a                   15.9240(19)
_cell_length_b                   8.1630(8)
_cell_length_c                   12.4914(13)
_cell_angle_alpha                90
_cell_angle_beta                 102.981(12)
_cell_angle_gamma                90
_cell_volume                     1582.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    2304
_cell_measurement_theta_min      3.6650
_cell_measurement_theta_max      31.4310
_exptl_crystal_description       prism
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.4486
_exptl_crystal_size_mid          0.3308
_exptl_crystal_size_min          0.2634
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)

Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)

Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-16 -8 8 0.2236
23 1 -8 0.1468
-7 11 0 0.1915
16 8 -8 0.2083
-22 0 8 0.1131
-23 0 1 0.0853
-1 9 -11 0.2130
14 -7 7 0.2022
-15 -8 0 0.1824
12 0 -17 0.1465
8 -2 -17 0.1611
-2 0 17 0.1796
7 -11 0 0.1846
21 -3 -7 0.1479
-5 0 -16 0.1556
7 4 -17 0.1744
12 5 10 0.1546
5 3 15 0.1304
-15 8 0 0.1655
-5 11 -4 0.1962

_diffrn_orient_matrix_UB_11      -0.0329125000
_diffrn_orient_matrix_UB_12      0.0421740000
_diffrn_orient_matrix_UB_13      -0.0375873000
_diffrn_orient_matrix_UB_21      0.0017021000
_diffrn_orient_matrix_UB_22      -0.0596938000
_diffrn_orient_matrix_UB_23      -0.0406761000
_diffrn_orient_matrix_UB_31      -0.0317418000
_diffrn_orient_matrix_UB_32      -0.0468849000
_diffrn_orient_matrix_UB_33      0.0180494000

_diffrn_ambient_temperature      150(1)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent Sapphire3'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5530
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_av_R_equivalents  0.083
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.310
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_point_group_measured_fraction_full 0.944
_reflns_number_total             5530
_reflns_number_gt                4185
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.889
_reflns_Friedel_fraction_max     0.890
_reflns_Friedel_fraction_full    0.891

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_twin_formation_mechanism        gt
_twin_dimensionality             triperiodic
_twin_morphology                 simple
_twin_special_details            
;       
Individuals are twinned by rotation of ca. 180° around [-0.25 0 1] in
reciprocal or (0 0 1) in direct space.
;

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.644(3) ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 0.356(3) nmt -0.9968 -0.0039 -0.5648 0.0018 -0.9968 0.0017 0.0020 0.0051
0.9971

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX (Farrugia, 2012)'

_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1136P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.05(3)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         5530
_refine_ls_number_parameters     398
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0596
_refine_ls_wR_factor_ref         0.1737
_refine_ls_wR_factor_gt          0.1612
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.9073(9) -0.0356(19) 0.5112(13) 0.037(4) Uani 1 1 d . . . . .
H11 H 0.8640 -0.1007 0.4659 0.045 Uiso 1 1 calc R U . . .
C12 C 0.9843(10) -0.018(3) 0.4834(14) 0.061(6) Uani 1 1 d . . . . .
H12 H 0.9961 -0.0715 0.4210 0.073 Uiso 1 1 calc R U . . .
C13 C 1.0464(11) 0.084(3) 0.5504(19) 0.067(6) Uani 1 1 d . . . . .
H13 H 1.1004 0.0992 0.5316 0.080 Uiso 1 1 calc R U . . .
C14 C 1.0315(11) 0.159(3) 0.6397(19) 0.068(6) Uani 1 1 d . . . . .
H14 H 1.0735 0.2277 0.6845 0.082 Uiso 1 1 calc R U . . .
C15 C 0.9511(8) 0.132(2) 0.6633(15) 0.050(5) Uani 1 1 d . . . . .
H15 H 0.9387 0.1839 0.7261 0.059 Uiso 1 1 calc R U . . .
C21 C 0.7424(9) 0.2675(18) 0.4352(13) 0.028(3) Uani 1 1 d . . . . .
H21 H 0.7400 0.1667 0.3965 0.034 Uiso 1 1 calc R U . . .
C22 C 0.7415(10) 0.4117(17) 0.3783(13) 0.028(4) Uani 1 1 d . . . . .
H22 H 0.7404 0.4100 0.3019 0.034 Uiso 1 1 calc R U . . .
C23 C 0.7424(10) 0.560(2) 0.4327(16) 0.036(4) Uani 1 1 d . . . . .
H23 H 0.7403 0.6602 0.3937 0.043 Uiso 1 1 calc R U . . .
C24 C 0.7461(11) 0.5600(19) 0.5412(13) 0.033(4) Uani 1 1 d . . . . .
H24 H 0.7478 0.6605 0.5799 0.039 Uiso 1 1 calc R U . . .
C25 C 0.7475(10) 0.4125(17) 0.5961(13) 0.026(3) Uani 1 1 d . . . . .
H25 H 0.7491 0.4144 0.6726 0.031 Uiso 1 1 calc R U . . .
C31 C 0.5513(11) 0.141(2) 0.5561(15) 0.041(5) Uani 1 1 d . . . . .
H31 H 0.5643 0.1246 0.4863 0.050 Uiso 1 1 calc R U . . .
C32 C 0.4701(10) 0.192(2) 0.5591(16) 0.042(5) Uani 1 1 d . . . . .
H32 H 0.4283 0.2133 0.4933 0.050 Uiso 1 1 calc R U . . .
C33 C 0.4513(10) 0.212(2) 0.6578(18) 0.049(5) Uani 1 1 d . . . . .
H33 H 0.3959 0.2510 0.6622 0.058 Uiso 1 1 calc R U . . .
C34 C 0.5117(10) 0.177(2) 0.7530(15) 0.043(4) Uani 1 1 d . . . . .
H34 H 0.4982 0.1872 0.8230 0.051 Uiso 1 1 calc R U . . .
C35 C 0.5926(9) 0.126(2) 0.7429(13) 0.033(4) Uani 1 1 d . . . . .
H35 H 0.6344 0.0996 0.8076 0.040 Uiso 1 1 calc R U . . .
N10 N 0.8904(7) 0.0367(14) 0.6017(10) 0.025(3) Uani 1 1 d . . . . .
N20 N 0.7467(8) 0.2646(13) 0.5454(9) 0.022(3) Uani 1 1 d . . . . .
N30 N 0.6139(7) 0.1128(15) 0.6469(11) 0.029(3) Uani 1 1 d . . . . .
F1 F 0.7096(5) -0.0576(9) 0.5044(6) 0.0244(17) Uani 1 1 d . . . . .
F2 F 0.7567(5) -0.1449(9) 0.7120(7) 0.0295(19) Uani 1 1 d . . . . .
F3 F 0.7934(5) 0.1597(9) 0.7590(7) 0.0287(18) Uani 1 1 d . . . . .
Mn1 Mn 0.75176(10) 0.0460(3) 0.63345(13) 0.0200(6) Uani 1 1 d . . . . .
C41 C 0.4464(9) 0.643(2) 0.5254(13) 0.032(4) Uani 1 1 d . . . . .
H41 H 0.4325 0.6258 0.4482 0.038 Uiso 1 1 calc R U . . .
C42 C 0.5287(12) 0.698(2) 0.5747(17) 0.048(6) Uani 1 1 d . . . . .
H42 H 0.5694 0.7229 0.5320 0.058 Uiso 1 1 calc R U . . .
C43 C 0.5497(11) 0.717(2) 0.6892(18) 0.054(6) Uani 1 1 d . . . . .
H43 H 0.6053 0.7521 0.7267 0.065 Uiso 1 1 calc R U . . .
C44 C 0.4882(11) 0.682(2) 0.7442(18) 0.054(5) Uani 1 1 d . . . . .
H44 H 0.5010 0.6944 0.8218 0.065 Uiso 1 1 calc R U . . .
C45 C 0.4076(9) 0.630(2) 0.6914(12) 0.033(4) Uani 1 1 d . . . . .
H45 H 0.3656 0.6070 0.7326 0.040 Uiso 1 1 calc R U . . .
C51 C 0.2525(9) 0.7615(14) 0.2964(10) 0.017(3) Uani 1 1 d . . . . .
H51 H 0.2547 0.6602 0.2596 0.021 Uiso 1 1 calc R U . . .
C52 C 0.2540(10) 0.9057(18) 0.2387(14) 0.028(3) Uani 1 1 d . . . . .
H52 H 0.2538 0.9036 0.1626 0.033 Uiso 1 1 calc R U . . .
C53 C 0.2558(11) 1.0544(16) 0.2943(12) 0.025(3) Uani 1 1 d . . . . .
H53 H 0.2615 1.1551 0.2585 0.030 Uiso 1 1 calc R U . . .
C54 C 0.2491(12) 1.0516(18) 0.4025(13) 0.033(4) Uani 1 1 d . . . . .
H54 H 0.2481 1.1514 0.4413 0.039 Uiso 1 1 calc R U . . .
C55 C 0.2438(11) 0.9024(19) 0.4552(13) 0.030(4) Uani 1 1 d . . . . .
H55 H 0.2371 0.9011 0.5288 0.036 Uiso 1 1 calc R U . . .
C61 C 0.0987(9) 0.3995(18) 0.2914(12) 0.034(4) Uani 1 1 d . . . . .
H61 H 0.1454 0.3864 0.2563 0.040 Uiso 1 1 calc R U . . .
C62 C 0.0200(10) 0.335(2) 0.2420(13) 0.044(4) Uani 1 1 d . . . . .
H62 H 0.0127 0.2787 0.1740 0.052 Uiso 1 1 calc R U . . .
C63 C -0.0474(10) 0.353(2) 0.2911(16) 0.056(5) Uani 1 1 d . . . . .
H63 H -0.1020 0.3068 0.2589 0.067 Uiso 1 1 calc R U . . .
C64 C -0.0354(11) 0.440(3) 0.3889(19) 0.079(7) Uani 1 1 d . . . . .
H64 H -0.0816 0.4540 0.4247 0.095 Uiso 1 1 calc R U . . .
C65 C 0.0466(10) 0.506(2) 0.4343(14) 0.049(4) Uani 1 1 d . . . . .
H65 H 0.0550 0.5703 0.4992 0.059 Uiso 1 1 calc R U . . .
N40 N 0.3875(7) 0.6126(16) 0.5805(10) 0.027(3) Uani 1 1 d . . . . .
N50 N 0.2482(8) 0.7594(13) 0.4019(9) 0.020(2) Uani 1 1 d . . . . .
N60 N 0.1124(7) 0.4797(13) 0.3868(9) 0.024(3) Uani 1 1 d . . . . .
F4 F 0.2961(5) 0.4426(9) 0.3853(7) 0.0276(19) Uani 1 1 d . . . . .
F5 F 0.2534(6) 0.3490(10) 0.5690(6) 0.032(2) Uani 1 1 d . . . . .
F6 F 0.2044(5) 0.6507(10) 0.5891(6) 0.0271(18) Uani 1 1 d . . . . .
Mn2 Mn 0.24955(10) 0.5402(3) 0.48915(13) 0.0189(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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(16) . ?
C11 C12 1.36(2) . ?
C12 C13 1.41(3) . ?
C13 C14 1.34(3) . ?
C14 C15 1.39(2) . ?
C15 N10 1.342(19) . ?
C21 N20 1.364(17) . ?
C21 C22 1.37(2) . ?
C22 C23 1.39(2) . ?
C23 C24 1.34(2) . ?
C24 C25 1.38(2) . ?
C25 N20 1.362(17) . ?
C31 N30 1.352(19) . ?
C31 C32 1.37(2) . ?
C32 C33 1.34(3) . ?
C33 C34 1.38(3) . ?
C34 C35 1.39(2) . ?
C35 N30 1.323(18) . ?
N10 Mn1 2.331(10) . ?
N20 Mn1 2.088(11) . ?
N30 Mn1 2.304(11) . ?
F1 Mn1 1.811(8) . ?
F2 Mn1 1.834(8) . ?
F3 Mn1 1.815(8) . ?
C41 N40 1.305(18) . ?
C41 C42 1.39(2) . ?
C42 C43 1.40(2) . ?
C43 C44 1.35(3) . ?
C44 C45 1.37(2) . ?
C45 N40 1.358(18) . ?
C51 N50 1.335(15) . ?
C51 C52 1.383(18) . ?
C52 C53 1.396(19) . ?
C53 C54 1.38(2) . ?
C54 C55 1.395(19) . ?
C55 N50 1.353(17) . ?
C61 N60 1.334(17) . ?
C61 C62 1.37(2) . ?
C62 C63 1.36(2) . ?
C63 C64 1.39(3) . ?
C64 C65 1.41(2) . ?
C65 N60 1.332(18) . ?
N40 Mn2 2.313(11) . ?
N50 Mn2 2.094(11) . ?
N60 Mn2 2.323(11) . ?
F4 Mn2 1.816(8) . ?
F5 Mn2 1.845(8) . ?
F6 Mn2 1.815(8) . ?

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(15) . . ?
C11 C12 C13 117.7(16) . . ?
C14 C13 C12 122.1(17) . . ?
C13 C14 C15 116.4(18) . . ?
N10 C15 C14 123.3(16) . . ?
N20 C21 C22 122.0(14) . . ?
C21 C22 C23 119.8(14) . . ?
C24 C23 C22 119.3(16) . . ?
C23 C24 C25 119.4(16) . . ?
N20 C25 C24 122.9(14) . . ?
N30 C31 C32 123.6(18) . . ?
C33 C32 C31 118.1(18) . . ?
C32 C33 C34 120.6(16) . . ?
C33 C34 C35 117.8(16) . . ?
N30 C35 C34 122.7(15) . . ?
C15 N10 C11 118.7(12) . . ?
C15 N10 Mn1 118.1(9) . . ?
C11 N10 Mn1 122.0(9) . . ?
C25 N20 C21 116.6(13) . . ?
C25 N20 Mn1 121.2(10) . . ?
C21 N20 Mn1 122.3(10) . . ?
C35 N30 C31 117.1(14) . . ?
C35 N30 Mn1 121.9(10) . . ?
C31 N30 Mn1 121.0(11) . . ?
F1 Mn1 F3 177.1(4) . . ?
F1 Mn1 F2 92.4(4) . . ?
F3 Mn1 F2 90.5(4) . . ?
F1 Mn1 N20 88.1(4) . . ?
F3 Mn1 N20 88.9(4) . . ?
F2 Mn1 N20 179.4(5) . . ?
F1 Mn1 N30 90.4(4) . . ?
F3 Mn1 N30 89.2(4) . . ?
F2 Mn1 N30 95.1(4) . . ?
N20 Mn1 N30 84.9(4) . . ?
F1 Mn1 N10 90.5(4) . . ?
F3 Mn1 N10 89.3(4) . . ?
F2 Mn1 N10 97.8(4) . . ?
N20 Mn1 N10 82.2(4) . . ?
N30 Mn1 N10 167.0(4) . . ?
N40 C41 C42 123.0(16) . . ?
C41 C42 C43 118.1(17) . . ?
C44 C43 C42 117.7(16) . . ?
C43 C44 C45 122(2) . . ?
N40 C45 C44 120.3(15) . . ?
N50 C51 C52 122.4(13) . . ?
C51 C52 C53 118.8(13) . . ?
C54 C53 C52 118.4(13) . . ?
C53 C54 C55 120.1(14) . . ?
N50 C55 C54 120.4(13) . . ?
N60 C61 C62 122.6(14) . . ?
C63 C62 C61 119.4(15) . . ?
C62 C63 C64 119.0(15) . . ?
C63 C64 C65 118.8(17) . . ?
N60 C65 C64 120.6(16) . . ?
C41 N40 C45 119.0(13) . . ?
C41 N40 Mn2 120.3(10) . . ?
C45 N40 Mn2 120.7(9) . . ?
C51 N50 C55 119.7(12) . . ?
C51 N50 Mn2 121.9(9) . . ?
C55 N50 Mn2 118.5(9) . . ?
C65 N60 C61 119.4(13) . . ?
C65 N60 Mn2 117.2(10) . . ?
C61 N60 Mn2 122.7(9) . . ?
F6 Mn2 F4 176.2(4) . . ?
F6 Mn2 F5 91.1(4) . . ?
F4 Mn2 F5 92.6(3) . . ?
F6 Mn2 N50 88.5(4) . . ?
F4 Mn2 N50 87.8(4) . . ?
F5 Mn2 N50 178.3(4) . . ?
F6 Mn2 N40 90.7(4) . . ?
F4 Mn2 N40 88.2(4) . . ?
F5 Mn2 N40 92.1(4) . . ?
N50 Mn2 N40 86.3(5) . . ?
F6 Mn2 N60 90.9(4) . . ?
F4 Mn2 N60 89.9(4) . . ?
F5 Mn2 N60 91.8(4) . . ?
N50 Mn2 N60 89.8(4) . . ?
N40 Mn2 N60 175.8(4) . . ?

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 -2(3) . . . . ?
C11 C12 C13 C14 1(3) . . . . ?
C12 C13 C14 C15 0(3) . . . . ?
C13 C14 C15 N10 0(3) . . . . ?
N20 C21 C22 C23 -2(2) . . . . ?
C21 C22 C23 C24 2(2) . . . . ?
C22 C23 C24 C25 -1(2) . . . . ?
C23 C24 C25 N20 1(2) . . . . ?
N30 C31 C32 C33 -1(3) . . . . ?
C31 C32 C33 C34 -2(3) . . . . ?
C32 C33 C34 C35 2(3) . . . . ?
C33 C34 C35 N30 1(2) . . . . ?
C14 C15 N10 C11 -1(3) . . . . ?
C14 C15 N10 Mn1 -168.3(16) . . . . ?
C12 C11 N10 C15 2(2) . . . . ?
C12 C11 N10 Mn1 168.8(13) . . . . ?
C24 C25 N20 C21 -1(2) . . . . ?
C24 C25 N20 Mn1 178.6(11) . . . . ?
C22 C21 N20 C25 2(2) . . . . ?
C22 C21 N20 Mn1 -178.2(10) . . . . ?
C34 C35 N30 C31 -4(2) . . . . ?
C34 C35 N30 Mn1 175.5(11) . . . . ?
C32 C31 N30 C35 4(2) . . . . ?
C32 C31 N30 Mn1 -175.2(14) . . . . ?
N40 C41 C42 C43 2(3) . . . . ?
C41 C42 C43 C44 -1(3) . . . . ?
C42 C43 C44 C45 0(3) . . . . ?
C43 C44 C45 N40 0(3) . . . . ?
N50 C51 C52 C53 4(2) . . . . ?
C51 C52 C53 C54 -5(2) . . . . ?
C52 C53 C54 C55 2(3) . . . . ?
C53 C54 C55 N50 2(3) . . . . ?
N60 C61 C62 C63 0(2) . . . . ?
C61 C62 C63 C64 2(3) . . . . ?
C62 C63 C64 C65 0(3) . . . . ?
C63 C64 C65 N60 -3(3) . . . . ?
C42 C41 N40 C45 -2(3) . . . . ?
C42 C41 N40 Mn2 175.2(14) . . . . ?
C44 C45 N40 C41 1(2) . . . . ?
C44 C45 N40 Mn2 -176.3(12) . . . . ?
C52 C51 N50 C55 1(2) . . . . ?
C52 C51 N50 Mn2 -178.3(10) . . . . ?
C54 C55 N50 C51 -4(2) . . . . ?
C54 C55 N50 Mn2 175.3(11) . . . . ?
C64 C65 N60 C61 5(3) . . . . ?
C64 C65 N60 Mn2 -165.7(16) . . . . ?
C62 C61 N60 C65 -3(2) . . . . ?
C62 C61 N60 Mn2 166.6(12) . . . . ?

_refine_diff_density_max         0.488
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.120

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3a
_database_code_depnum_ccdc_archive 'CCDC 1063083'
_audit_update_record             
;
2015-06-19 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        trans-difluoridotetrakis(pyridine)nickel(II)
_chemical_formula_iupac          '[Ni (C5 H5 N)4 F2]'
_chemical_formula_moiety         'C20 H20 F2 N4 Ni'
_chemical_formula_sum            'C20 H20 F2 N4 Ni'
_chemical_formula_weight         413.11

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 0.0000 0.0000 '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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   15.1861(10)
_cell_length_b                   8.4089(4)
_cell_length_c                   15.7527(9)
_cell_angle_alpha                90
_cell_angle_beta                 110.717(7)
_cell_angle_gamma                90
_cell_volume                     1881.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    2219
_cell_measurement_theta_min      3.9710
_cell_measurement_theta_max      32.2720
_exptl_crystal_description       irregular
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_F_000             856
_exptl_crystal_size_max          1.3473
_exptl_crystal_size_mid          0.6201
_exptl_crystal_size_min          0.5443
_exptl_absorpt_coefficient_mu    1.062
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.480
_exptl_absorpt_correction_T_max  0.648
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)

Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)

Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -10 10 0.2902
7 9 9 0.3128
21 -1 -2 0.2561
3 -10 -12 0.3129
-17 -4 -5 0.2889
-1 11 6 0.3021
-3 -8 -13 0.3347
-17 7 4 0.3101
-16 6 -4 0.2870
2 -11 -9 0.2933
12 9 -10 0.3571
-11 8 -7 0.3000
20 2 1 0.2608
20 -1 0 0.2528
-12 10 7 0.3394
-21 -1 2 0.2805
20 1 -1 0.2579
8 11 0 0.2960
20 0 1 0.2573
1 12 -2 0.3037
-5 10 -8 0.3151
4 11 7 0.2986
4 10 -11 0.3524
5 8 -17 0.4266
-1 5 -18 0.4435
3 -12 -2 0.2942
0 -12 -3 0.2984
12 9 2 0.2999
17 -7 0 0.3003
11 -8 8 0.3230
-9 6 -13 0.3795
-9 -9 -6 0.3232
-4 9 -12 0.3595
16 -6 4 0.3050
7 -11 -9 0.3290
10 -10 -1 0.3022
-15 -8 9 0.3995
-21 -2 3 0.2952

_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent Sapphire3'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3859
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_av_R_equivalents  0.0149
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.573
_diffrn_reflns_theta_max         25.990
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             1839
_reflns_number_gt                1706
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX (Farrugia, 2012)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0302P)²+2.1050P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1839
_refine_ls_number_parameters     124
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0247
_refine_ls_wR_factor_ref         0.0654
_refine_ls_wR_factor_gt          0.0642
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.58691(12) 0.1676(2) 0.52435(11) 0.0244(3) Uani 1 1 d . . . . .
H11 H 0.5257 0.1394 0.4844 0.029 Uiso 1 1 calc R U . . .
C12 C 0.65310(13) 0.0485(2) 0.55661(13) 0.0306(4) Uani 1 1 d . . . . .
H12 H 0.6373 -0.0592 0.5400 0.037 Uiso 1 1 calc R U . . .
C13 C 0.74255(13) 0.0891(2) 0.61345(14) 0.0356(4) Uani 1 1 d . . . . .
H13 H 0.7896 0.0099 0.6363 0.043 Uiso 1 1 calc R U . . .
C14 C 0.76243(14) 0.2462(2) 0.63646(16) 0.0436(5) Uani 1 1 d . . . . .
H14 H 0.8236 0.2776 0.6750 0.052 Uiso 1 1 calc R U . . .
C15 C 0.69166(13) 0.3579(2) 0.60249(14) 0.0341(4) Uani 1 1 d . . . . .
H15 H 0.7054 0.4660 0.6196 0.041 Uiso 1 1 calc R U . . .
C21 C 0.37669(12) 0.36935(19) 0.59872(11) 0.0239(3) Uani 1 1 d . . . . .
H21 H 0.3382 0.3392 0.5390 0.029 Uiso 1 1 calc R U . . .
C22 C 0.34744(13) 0.3310(2) 0.66986(13) 0.0291(4) Uani 1 1 d . . . . .
H22 H 0.2898 0.2762 0.6590 0.035 Uiso 1 1 calc R U . . .
C23 C 0.40343(14) 0.3735(2) 0.75705(12) 0.0336(4) Uani 1 1 d . . . . .
H23 H 0.3857 0.3467 0.8074 0.040 Uiso 1 1 calc R U . . .
C24 C 0.48567(15) 0.4557(3) 0.76935(12) 0.0374(5) Uani 1 1 d . . . . .
H24 H 0.5250 0.4880 0.8284 0.045 Uiso 1 1 calc R U . . .
C25 C 0.51010(13) 0.4903(2) 0.69512(12) 0.0286(4) Uani 1 1 d . . . . .
H25 H 0.5668 0.5469 0.7043 0.034 Uiso 1 1 calc R U . . .
N10 N 0.60488(9) 0.32096(16) 0.54677(9) 0.0204(3) Uani 1 1 d . . . . .
N20 N 0.45704(9) 0.44725(16) 0.61045(9) 0.0202(3) Uani 1 1 d . . . . .
F1 F 0.40763(6) 0.33780(11) 0.42626(6) 0.0216(2) Uani 1 1 d . . . . .
Ni1 Ni 0.5000 0.5000 0.5000 0.01669(11) Uani 1 2 d S . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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 1.339(2) . ?
C11 C12 1.382(2) . ?
C12 C13 1.380(3) . ?
C13 C14 1.375(3) . ?
C14 C15 1.384(3) . ?
C15 N10 1.336(2) . ?
C21 N20 1.339(2) . ?
C21 C22 1.382(2) . ?
C22 C23 1.382(3) . ?
C23 C24 1.380(3) . ?
C24 C25 1.377(3) . ?
C25 N20 1.341(2) . ?
N10 Ni1 2.1251(13) . ?
N20 Ni1 2.1102(13) . ?
F1 Ni1 2.0061(9) . ?
Ni1 F1 2.0061(9) 5_666 ?
Ni1 N20 2.1101(13) 5_666 ?
Ni1 N10 2.1251(13) 5_666 ?

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 123.16(16) . . ?
C13 C12 C11 118.69(17) . . ?
C14 C13 C12 118.88(17) . . ?
C13 C14 C15 118.80(18) . . ?
N10 C15 C14 123.15(17) . . ?
N20 C21 C22 122.75(16) . . ?
C21 C22 C23 118.96(17) . . ?
C24 C23 C22 118.50(16) . . ?
C25 C24 C23 119.27(18) . . ?
N20 C25 C24 122.67(17) . . ?
C15 N10 C11 117.30(15) . . ?
C15 N10 Ni1 120.47(11) . . ?
C11 N10 Ni1 122.20(11) . . ?
C21 N20 C25 117.83(14) . . ?
C21 N20 Ni1 121.43(11) . . ?
C25 N20 Ni1 120.73(11) . . ?
F1 Ni1 F1 180.0 . 5_666 ?
F1 Ni1 N20 91.28(4) . 5_666 ?
F1 Ni1 N20 88.72(5) 5_666 5_666 ?
F1 Ni1 N20 88.72(5) . . ?
F1 Ni1 N20 91.28(5) 5_666 . ?
N20 Ni1 N20 180.0 5_666 . ?
F1 Ni1 N10 90.22(5) . . ?
F1 Ni1 N10 89.78(5) 5_666 . ?
N20 Ni1 N10 91.28(5) 5_666 . ?
N20 Ni1 N10 88.72(5) . . ?
F1 Ni1 N10 89.78(5) . 5_666 ?
F1 Ni1 N10 90.22(5) 5_666 5_666 ?
N20 Ni1 N10 88.72(5) 5_666 5_666 ?
N20 Ni1 N10 91.28(5) . 5_666 ?
N10 Ni1 N10 180.0 . 5_666 ?

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(3) . . . . ?
C11 C12 C13 C14 0.5(3) . . . . ?
C12 C13 C14 C15 0.6(3) . . . . ?
C13 C14 C15 N10 -1.3(3) . . . . ?
N20 C21 C22 C23 -0.4(3) . . . . ?
C21 C22 C23 C24 1.3(3) . . . . ?
C22 C23 C24 C25 -1.1(3) . . . . ?
C23 C24 C25 N20 0.0(3) . . . . ?
C14 C15 N10 C11 0.7(3) . . . . ?
C14 C15 N10 Ni1 178.84(17) . . . . ?
C12 C11 N10 C15 0.5(2) . . . . ?
C12 C11 N10 Ni1 -177.60(13) . . . . ?
C22 C21 N20 C25 -0.6(2) . . . . ?
C22 C21 N20 Ni1 178.97(13) . . . . ?
C24 C25 N20 C21 0.9(3) . . . . ?
C24 C25 N20 Ni1 -178.74(15) . . . . ?

_refine_diff_density_max         0.236
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.048

