##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in          #
# Acta Crystallographica Section C. It conforms to the requirements of       #
# Notes for Authors for Acta Crystallographica Section C, and has been       #
# peer reviewed under the auspices of the IUCr Commission on Journals.       #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic.                                       #
#                                                                            #
# Software is freely available for graphical display of the structure(s)     #
# in this CIF. For information consult the CIF software page                 #
# http://www.iucr.org/resources/cif/software.                                #
#                                                                            #
# This file may be used for bona fide research purposes within the           #
# scientific community so long as proper attribution is given to the journal # 
# article from which it was obtained.                                        #
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##############################################################################
data_global
_audit_creation_method     SHELXL-2013
_journal_data_validation_number     ?
_journal_date_recd_electronic     2013-09-17
_journal_date_accepted     2013-10-30
_journal_name_full     'Acta Crystallographica, Section C'
_journal_year     2013
_journal_volume     69
_journal_issue     12
_journal_page_first     1482
_journal_page_last     1484
_journal_paper_category     FM
_journal_paper_doi     10.1107/S0108270113029776
_journal_coeditor_code     EG3138
_publ_contact_author_name     'Dr Dennis Wiedemann'
_publ_contact_author_address
;
Institut für Chemie
Technische Universität Berlin
Strasse des 17 Juni 135
10623 Berlin
Germany
;
_publ_contact_author_email     dennis.wiedemann@chem.tu-berlin.de
_publ_contact_author_fax     '+49 30 314-79656'
_publ_contact_author_phone     '+49 30 314-26178'
_publ_section_title
;
(OC-6--13)-Difluoridooxidobis(propan-2-ol)(propan-2-olato)vanadium(V)
;
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    'Kohl, Julia' .
;
Institut für Chemie
Technische Universität Berlin
Strasse des 17 Juni 135
10623 Berlin
Germany
;
    'Wiedemann, Dennis' .
;
Institut für Chemie
Technische Universität Berlin
Strasse des 17 Juni 135
10623 Berlin
Germany
;
_publ_section_synopsis
;
The crystal structure and NMR data of the title compound are reported. It
crystallizes in the space group P\=1 with Z' = 2, the molecules
forming infinite chains via hydrogen bonds. The chains interact through
dispersive aliphatic contacts.
;
data_I
_database_code_depnum_ccdc_archive     'CCDC 969480'
_chemical_name_systematic
;
(OC-6--13)-Difluoridooxidobis(propan-2-ol)(propan-2-olato)vanadium(V)
;
_chemical_formula_moiety     'C9 H23 F2 O4 V'
_chemical_formula_sum     'C9 H23 F2 O4 V'
_chemical_formula_structural     'F2 O (O (C H (C H3)2)) (O H (C H (C H3)2))2 V'
_chemical_formula_iupac     '[V (C3 H7 O) F2 O (C3 H8 O)2]'
_chemical_formula_weight     284.21
_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.
;
_space_group_crystal_system     triclinic
_space_group_name_H-M_alt     'P -1'
_space_group_name_Hall     '-P 1'
loop_
    _space_group_symop_operation_xyz
    'x, y, z'
    '-x, -y, -z'
_cell_length_a     9.0943(9)
_cell_length_b     9.9151(8)
_cell_length_c     16.4279(13)
_cell_angle_alpha     97.315(7)
_cell_angle_beta     97.690(7)
_cell_angle_gamma     92.324(7)
_cell_volume     1453.5(2)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     2615
_cell_measurement_theta_min     3.4772
_cell_measurement_theta_max     32.5898
_cell_measurement_temperature     150.00(10)
_exptl_crystal_description     coloumn
_exptl_crystal_colour     'clear yellow'
_exptl_crystal_size_max     0.887
_exptl_crystal_size_mid     0.200
_exptl_crystal_size_min     0.137
_exptl_crystal_density_diffrn     1.299
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     600
_exptl_absorpt_coefficient_mu     0.702
_exptl_absorpt_correction_type     analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Agilent, 2012), based on expressions derived by
Clark & Reid (1995)]
;
_shelx_estimated_absorpt_T_min     0.575
_shelx_estimated_absorpt_T_max     0.910
_exptl_absorpt_correction_T_min     0.727
_exptl_absorpt_correction_T_max     0.920
_diffrn_ambient_temperature     150.00(10)
_diffrn_radiation_type     'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Agilent Xcalibur'
_diffrn_measurement_device     'κ-geometry diffractometer'
_diffrn_measurement_method     'ω scans'
_diffrn_detector_area_resol_mean     16.3031
_diffrn_reflns_number     10818
_diffrn_reflns_av_R_equivalents     0.0449
_diffrn_reflns_theta_min     3.477
_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_limit_h_min     -11
_diffrn_reflns_limit_h_max     11
_diffrn_reflns_limit_k_min     -12
_diffrn_reflns_limit_k_max     11
_diffrn_reflns_limit_l_min     -17
_diffrn_reflns_limit_l_max     20
_diffrn_standards_number     0
_diffrn_standards_interval_count     .
_diffrn_standards_interval_time     .
_diffrn_standards_decay_%     ?
_refine_special_details
;
Oxygen-borne hydrogen atoms were refined with restrained 1,2- and 1,3- distances
as given by the _restr_distance_[] items. Their Uiso were constrained
to be 1.2 × Ueq of the bearing atoms.
;
_reflns_number_total     5702
_reflns_number_gt     4505
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0726
_refine_ls_R_factor_gt     0.0515
_refine_ls_wR_factor_gt     0.0989
_refine_ls_wR_factor_ref     0.1073
_refine_ls_goodness_of_fit_ref     1.046
_refine_ls_restrained_S_all     1.047
_refine_ls_number_reflns     5702
_refine_ls_number_parameters     313
_refine_ls_number_restraints     8
_refine_ls_hydrogen_treatment     heteroxyz
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
                      'w=1/[σ²(Fo²)+(0.0393P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.000
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.437
_refine_diff_density_min     -0.528
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     .
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'
    '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'
_computing_data_collection     'CrysAlis PRO (Agilent, 2012)'
_computing_cell_refinement     'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction     'CrysAlis PRO (Agilent, 2012)'
_computing_structure_solution     'SHELXS2013 (Sheldrick, 2008)'
_computing_structure_refinement     'SHELXL2013 (Sheldrick, 2008)'
_computing_molecular_graphics     'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material
;
WinGX (Farrugia, 2012), Mercury (Macrae et al., 2008), PLATON/MOLFIT (Spek,
2009), PLATON/PLUTON (Spek, 2009) and CSM website (Zayit et al., 2011)
;
loop_
    _atom_site_type_symbol
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    C C30 0.8503(4) 0.3139(4) -0.0785(2) 0.0415(9) Uani d 1 . .
    H H30A 0.9509 0.3527 -0.0568 0.062 Uiso calc 1 . .
    H H30B 0.7922 0.3827 -0.1038 0.062 Uiso calc 1 . .
    H H30C 0.8560 0.2352 -0.1204 0.062 Uiso calc 1 . .
    C C31 0.7763(3) 0.2691(3) -0.00849(18) 0.0251(7) Uani d 1 . .
    H H31 0.6740 0.2291 -0.0309 0.030 Uiso calc 1 . .
    C C32 0.7665(4) 0.3851(4) 0.0593(2) 0.0416(9) Uani d 1 . .
    H H32A 0.7269 0.3497 0.1056 0.062 Uiso calc 1 . .
    H H32B 0.7004 0.4519 0.0377 0.062 Uiso calc 1 . .
    H H32C 0.8657 0.4288 0.0787 0.062 Uiso calc 1 . .
    C C40 0.6679(4) -0.3120(4) -0.0916(2) 0.0432(9) Uani d 1 . .
    H H40A 0.6861 -0.3383 -0.0358 0.065 Uiso calc 1 . .
    H H40B 0.7073 -0.3796 -0.1307 0.065 Uiso calc 1 . .
    H H40C 0.5608 -0.3077 -0.1082 0.065 Uiso calc 1 . .
    C C41 0.7441(3) -0.1747(3) -0.09197(17) 0.0257(7) Uani d 1 . .
    H H41 0.8530 -0.1814 -0.0748 0.031 Uiso calc 1 . .
    C C42 0.7232(4) -0.1247(4) -0.17588(18) 0.0363(8) Uani d 1 . .
    H H42A 0.6171 -0.1158 -0.1935 0.054 Uiso calc 1 . .
    H H42B 0.7620 -0.1901 -0.2165 0.054 Uiso calc 1 . .
    H H42C 0.7769 -0.0359 -0.1720 0.054 Uiso calc 1 . .
    C C50 0.5413(4) -0.2150(5) 0.2175(2) 0.0653(15) Uani d 1 . .
    H H50A 0.4750 -0.1436 0.2029 0.098 Uiso calc 1 . .
    H H50B 0.5331 -0.2327 0.2741 0.098 Uiso calc 1 . .
    H H50C 0.5131 -0.2985 0.1788 0.098 Uiso calc 1 . .
    C C51 0.6989(3) -0.1691(3) 0.21226(17) 0.0265(7) Uani d 1 . .
    H H51 0.7284 -0.0867 0.2540 0.032 Uiso calc 1 . .
    C C52 0.8081(4) -0.2747(4) 0.2266(2) 0.0449(10) Uani d 1 . .
    H H52A 0.7798 -0.3562 0.1861 0.067 Uiso calc 1 . .
    H H52B 0.8089 -0.2984 0.2827 0.067 Uiso calc 1 . .
    H H52C 0.9075 -0.2390 0.2202 0.067 Uiso calc 1 . .
    O O12 0.8434(2) 0.0957(2) 0.18653(11) 0.0262(5) Uani d 1 . .
    O O33 0.8619(2) 0.1671(2) 0.02944(12) 0.0215(5) Uani d 1 . .
    H H33 0.910(3) 0.128(3) -0.0003(15) 0.026 Uiso d 1 . .
    O O43 0.6905(2) -0.0755(2) -0.03202(11) 0.0239(5) Uani d 1 . .
    H H43 0.6025(19) -0.070(3) -0.0444(16) 0.029 Uiso d 1 . .
    O O53 0.7037(2) -0.1323(2) 0.13039(11) 0.0236(5) Uani d 1 . .
    F F10 0.95277(16) -0.05790(17) 0.07061(9) 0.0238(4) Uani d 1 . .
    F F11 0.60516(15) 0.09967(18) 0.07997(10) 0.0251(4) Uani d 1 . .
    V V1 0.78003(5) 0.01389(5) 0.09899(3) 0.01807(13) Uani d 1 . .
    C C60 0.7591(4) 0.2460(5) 0.4056(2) 0.0567(12) Uani d 1 . .
    H H60A 0.8345 0.2659 0.4548 0.085 Uiso calc 1 . .
    H H60B 0.7966 0.1817 0.3640 0.085 Uiso calc 1 . .
    H H60C 0.6683 0.2060 0.4212 0.085 Uiso calc 1 . .
    C C61 0.7257(3) 0.3742(4) 0.37068(19) 0.0321(8) Uani d 1 . .
    H H61 0.8204 0.4141 0.3566 0.039 Uiso calc 1 . .
    C C62 0.6148(4) 0.3516(4) 0.2929(2) 0.0488(11) Uani d 1 . .
    H H62A 0.5205 0.3132 0.3053 0.073 Uiso calc 1 . .
    H H62B 0.6530 0.2883 0.2510 0.073 Uiso calc 1 . .
    H H62C 0.5985 0.4387 0.2718 0.073 Uiso calc 1 . .
    C C70 0.9422(3) 0.5670(4) 0.73560(19) 0.0399(9) Uani d 1 . .
    H H70A 1.0157 0.4988 0.7273 0.060 Uiso calc 1 . .
    H H70B 0.9076 0.5630 0.7893 0.060 Uiso calc 1 . .
    H H70C 0.9878 0.6579 0.7346 0.060 Uiso calc 1 . .
    C C71 0.8115(3) 0.5382(3) 0.66699(17) 0.0241(7) Uani d 1 . .
    H H71 0.7383 0.6088 0.6773 0.029 Uiso calc 1 . .
    C C72 0.7339(4) 0.4012(4) 0.6657(2) 0.0515(10) Uani d 1 . .
    H H72A 0.6529 0.3859 0.6192 0.077 Uiso calc 1 . .
    H H72B 0.6934 0.3981 0.7178 0.077 Uiso calc 1 . .
    H H72C 0.8049 0.3302 0.6593 0.077 Uiso calc 1 . .
    C C80 0.9360(4) 1.0323(4) 0.6110(3) 0.0494(10) Uani d 1 . .
    H H80A 0.9445 1.0163 0.6690 0.074 Uiso calc 1 . .
    H H80B 0.9271 1.1297 0.6078 0.074 Uiso calc 1 . .
    H H80C 1.0246 1.0021 0.5876 0.074 Uiso calc 1 . .
    C C81 0.7993(3) 0.9530(3) 0.5622(2) 0.0296(7) Uani d 1 . .
    H H81 0.7887 0.9726 0.5036 0.036 Uiso calc 1 . .
    C C82 0.6575(3) 0.9858(4) 0.5978(2) 0.0423(9) Uani d 1 . .
    H H82A 0.5740 0.9288 0.5653 0.063 Uiso calc 1 . .
    H H82B 0.6391 1.0820 0.5956 0.063 Uiso calc 1 . .
    H H82C 0.6678 0.9678 0.6555 0.063 Uiso calc 1 . .
    O O22 0.6793(2) 0.7502(2) 0.41889(12) 0.0336(6) Uani d 1 . .
    O O63 0.6726(2) 0.4712(3) 0.43103(14) 0.0372(6) Uani d 1 . .
    H H63 0.593(2) 0.442(3) 0.4392(19) 0.045 Uiso d 1 . .
    O O73 0.8580(2) 0.5506(2) 0.58798(12) 0.0260(5) Uani d 1 . .
    H H73 0.918(3) 0.496(3) 0.5773(17) 0.031 Uiso d 1 . .
    O O83 0.8222(2) 0.8103(2) 0.56364(11) 0.0240(5) Uani d 1 . .
    F F20 0.92143(16) 0.62287(18) 0.44693(9) 0.0250(4) Uani d 1 . .
    F F21 0.58303(16) 0.63762(18) 0.53906(10) 0.0277(4) Uani d 1 . .
    V V2 0.75177(5) 0.67038(5) 0.49047(3) 0.02055(14) Uani d 1 . .
_geom_special_details
;
All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes.
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    C30 C31 . 1.512(4) n
    C30 H30A . 0.9800 n
    C30 H30B . 0.9800 n
    C30 H30C . 0.9800 n
    C31 O33 . 1.453(3) n
    C31 C32 . 1.510(4) n
    C31 H31 . 1.0000 n
    C32 H32A . 0.9800 n
    C32 H32B . 0.9800 n
    C32 H32C . 0.9800 n
    C40 C41 . 1.503(5) n
    C40 H40A . 0.9800 n
    C40 H40B . 0.9800 n
    C40 H40C . 0.9800 n
    C41 O43 . 1.448(3) n
    C41 C42 . 1.514(4) n
    C41 H41 . 1.0000 n
    C42 H42A . 0.9800 n
    C42 H42B . 0.9800 n
    C42 H42C . 0.9800 n
    C50 C51 . 1.503(4) n
    C50 H50A . 0.9800 n
    C50 H50B . 0.9800 n
    C50 H50C . 0.9800 n
    C51 O53 . 1.443(3) n
    C51 C52 . 1.492(4) n
    C51 H51 . 1.0000 n
    C52 H52A . 0.9800 n
    C52 H52B . 0.9800 n
    C52 H52C . 0.9800 n
    O12 V1 . 1.581(2) y
    O33 V1 . 2.178(2) y
    O33 H33 . 0.778(16) n
    O43 V1 . 2.2513(19) y
    O43 H43 . 0.804(16) n
    O53 V1 . 1.747(2) y
    F10 V1 . 1.8423(14) y
    F11 V1 . 1.8424(15) y
    C60 C61 . 1.486(5) n
    C60 H60A . 0.9800 n
    C60 H60B . 0.9800 n
    C60 H60C . 0.9800 n
    C61 O63 . 1.437(3) n
    C61 C62 . 1.505(4) n
    C61 H61 . 1.0000 n
    C62 H62A . 0.9800 n
    C62 H62B . 0.9800 n
    C62 H62C . 0.9800 n
    C70 C71 . 1.515(4) n
    C70 H70A . 0.9800 n
    C70 H70B . 0.9800 n
    C70 H70C . 0.9800 n
    C71 O73 . 1.436(3) n
    C71 C72 . 1.502(5) n
    C71 H71 . 1.0000 n
    C72 H72A . 0.9800 n
    C72 H72B . 0.9800 n
    C72 H72C . 0.9800 n
    C80 C81 . 1.516(4) n
    C80 H80A . 0.9800 n
    C80 H80B . 0.9800 n
    C80 H80C . 0.9800 n
    C81 O83 . 1.441(4) n
    C81 C82 . 1.515(4) n
    C81 H81 . 1.0000 n
    C82 H82A . 0.9800 n
    C82 H82B . 0.9800 n
    C82 H82C . 0.9800 n
    O22 V2 . 1.586(2) y
    O63 V2 . 2.139(2) y
    O63 H63 . 0.805(17) n
    O73 V2 . 2.253(2) y
    O73 H73 . 0.800(17) n
    O83 V2 . 1.754(2) y
    F20 V2 . 1.8391(14) y
    F21 V2 . 1.8578(15) y
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    C31 C30 H30A . . 109.5 n
    C31 C30 H30B . . 109.5 n
    H30A C30 H30B . . 109.5 n
    C31 C30 H30C . . 109.5 n
    H30A C30 H30C . . 109.5 n
    H30B C30 H30C . . 109.5 n
    O33 C31 C32 . . 106.8(2) n
    O33 C31 C30 . . 109.9(2) n
    C32 C31 C30 . . 112.4(3) n
    O33 C31 H31 . . 109.2 n
    C32 C31 H31 . . 109.2 n
    C30 C31 H31 . . 109.2 n
    C31 C32 H32A . . 109.5 n
    C31 C32 H32B . . 109.5 n
    H32A C32 H32B . . 109.5 n
    C31 C32 H32C . . 109.5 n
    H32A C32 H32C . . 109.5 n
    H32B C32 H32C . . 109.5 n
    C41 C40 H40A . . 109.5 n
    C41 C40 H40B . . 109.5 n
    H40A C40 H40B . . 109.5 n
    C41 C40 H40C . . 109.5 n
    H40A C40 H40C . . 109.5 n
    H40B C40 H40C . . 109.5 n
    O43 C41 C40 . . 109.7(2) n
    O43 C41 C42 . . 109.0(3) n
    C40 C41 C42 . . 113.7(3) n
    O43 C41 H41 . . 108.1 n
    C40 C41 H41 . . 108.1 n
    C42 C41 H41 . . 108.1 n
    C41 C42 H42A . . 109.5 n
    C41 C42 H42B . . 109.5 n
    H42A C42 H42B . . 109.5 n
    C41 C42 H42C . . 109.5 n
    H42A C42 H42C . . 109.5 n
    H42B C42 H42C . . 109.5 n
    C51 C50 H50A . . 109.5 n
    C51 C50 H50B . . 109.5 n
    H50A C50 H50B . . 109.5 n
    C51 C50 H50C . . 109.5 n
    H50A C50 H50C . . 109.5 n
    H50B C50 H50C . . 109.5 n
    O53 C51 C52 . . 108.4(2) n
    O53 C51 C50 . . 107.8(2) n
    C52 C51 C50 . . 114.0(3) n
    O53 C51 H51 . . 108.9 n
    C52 C51 H51 . . 108.9 n
    C50 C51 H51 . . 108.9 n
    C51 C52 H52A . . 109.5 n
    C51 C52 H52B . . 109.5 n
    H52A C52 H52B . . 109.5 n
    C51 C52 H52C . . 109.5 n
    H52A C52 H52C . . 109.5 n
    H52B C52 H52C . . 109.5 n
    C31 O33 V1 . . 126.82(15) n
    C31 O33 H33 . . 113(2) n
    V1 O33 H33 . . 105(2) n
    C41 O43 V1 . . 133.21(16) n
    C41 O43 H43 . . 109(2) n
    V1 O43 H43 . . 114.6(19) n
    C51 O53 V1 . . 130.57(19) n
    O12 V1 O53 . . 99.80(10) y
    O12 V1 F10 . . 99.20(9) y
    O53 V1 F10 . . 97.45(8) y
    O12 V1 F11 . . 98.62(9) y
    O53 V1 F11 . . 97.01(8) y
    F10 V1 F11 . . 154.73(7) y
    O12 V1 O33 . . 94.30(10) y
    O53 V1 O33 . . 165.77(9) y
    F10 V1 O33 . . 78.23(7) y
    F11 V1 O33 . . 82.71(7) y
    O12 V1 O43 . . 172.37(10) y
    O53 V1 O43 . . 87.31(9) y
    F10 V1 O43 . . 82.49(7) y
    F11 V1 O43 . . 77.61(7) y
    O33 V1 O43 . . 78.72(8) y
    C61 C60 H60A . . 109.5 n
    C61 C60 H60B . . 109.5 n
    H60A C60 H60B . . 109.5 n
    C61 C60 H60C . . 109.5 n
    H60A C60 H60C . . 109.5 n
    H60B C60 H60C . . 109.5 n
    O63 C61 C60 . . 110.6(3) n
    O63 C61 C62 . . 109.6(3) n
    C60 C61 C62 . . 112.8(3) n
    O63 C61 H61 . . 107.9 n
    C60 C61 H61 . . 107.9 n
    C62 C61 H61 . . 107.9 n
    C61 C62 H62A . . 109.5 n
    C61 C62 H62B . . 109.5 n
    H62A C62 H62B . . 109.5 n
    C61 C62 H62C . . 109.5 n
    H62A C62 H62C . . 109.5 n
    H62B C62 H62C . . 109.5 n
    C71 C70 H70A . . 109.5 n
    C71 C70 H70B . . 109.5 n
    H70A C70 H70B . . 109.5 n
    C71 C70 H70C . . 109.5 n
    H70A C70 H70C . . 109.5 n
    H70B C70 H70C . . 109.5 n
    O73 C71 C72 . . 110.5(3) n
    O73 C71 C70 . . 110.6(2) n
    C72 C71 C70 . . 112.5(3) n
    O73 C71 H71 . . 107.7 n
    C72 C71 H71 . . 107.7 n
    C70 C71 H71 . . 107.7 n
    C71 C72 H72A . . 109.5 n
    C71 C72 H72B . . 109.5 n
    H72A C72 H72B . . 109.5 n
    C71 C72 H72C . . 109.5 n
    H72A C72 H72C . . 109.5 n
    H72B C72 H72C . . 109.5 n
    C81 C80 H80A . . 109.5 n
    C81 C80 H80B . . 109.5 n
    H80A C80 H80B . . 109.5 n
    C81 C80 H80C . . 109.5 n
    H80A C80 H80C . . 109.5 n
    H80B C80 H80C . . 109.5 n
    O83 C81 C80 . . 107.4(3) n
    O83 C81 C82 . . 108.7(3) n
    C80 C81 C82 . . 113.2(3) n
    O83 C81 H81 . . 109.2 n
    C80 C81 H81 . . 109.2 n
    C82 C81 H81 . . 109.2 n
    C81 C82 H82A . . 109.5 n
    C81 C82 H82B . . 109.5 n
    H82A C82 H82B . . 109.5 n
    C81 C82 H82C . . 109.5 n
    H82A C82 H82C . . 109.5 n
    H82B C82 H82C . . 109.5 n
    C61 O63 V2 . . 133.84(18) n
    C61 O63 H63 . . 108(2) n
    V2 O63 H63 . . 118(2) n
    C71 O73 V2 . . 126.96(15) n
    C71 O73 H73 . . 111(2) n
    V2 O73 H73 . . 121(2) n
    C81 O83 V2 . . 129.26(19) n
    O22 V2 O83 . . 98.83(11) y
    O22 V2 F20 . . 98.47(9) y
    O83 V2 F20 . . 100.51(8) y
    O22 V2 F21 . . 98.67(9) y
    O83 V2 F21 . . 95.14(8) y
    F20 V2 F21 . . 154.66(8) y
    O22 V2 O63 . . 96.21(11) y
    O83 V2 O63 . . 164.06(10) y
    F20 V2 O63 . . 82.38(7) y
    F21 V2 O63 . . 77.34(7) y
    O22 V2 O73 . . 177.56(9) y
    O83 V2 O73 . . 83.05(9) y
    F20 V2 O73 . . 79.61(7) y
    F21 V2 O73 . . 82.67(7) y
    O63 V2 O73 . . 82.07(9) y
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_site_symmetry_1
    _geom_torsion_site_symmetry_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    C32 C31 O33 V1 . . . . 81.7(3) n
    C30 C31 O33 V1 . . . . -156.1(2) n
    C40 C41 O43 V1 . . . . 98.4(3) n
    C42 C41 O43 V1 . . . . -136.6(2) n
    C52 C51 O53 V1 . . . . -105.7(3) n
    C50 C51 O53 V1 . . . . 130.4(3) n
    C51 O53 V1 O12 . . . . 0.1(2) n
    C51 O53 V1 F10 . . . . 100.8(2) n
    C51 O53 V1 F11 . . . . -100.0(2) n
    C51 O53 V1 O33 . . . . 172.1(3) n
    C51 O53 V1 O43 . . . . -177.1(2) n
    C60 C61 O63 V2 . . . . 118.6(3) n
    C62 C61 O63 V2 . . . . -116.6(3) n
    C72 C71 O73 V2 . . . . 104.5(3) n
    C70 C71 O73 V2 . . . . -130.3(2) n
    C80 C81 O83 V2 . . . . -151.4(2) n
    C82 C81 O83 V2 . . . . 85.8(3) n
    C81 O83 V2 O22 . . . . 8.3(2) n
    C81 O83 V2 F20 . . . . 108.7(2) n
    C81 O83 V2 F21 . . . . -91.4(2) n
    C81 O83 V2 O63 . . . . -152.2(3) n
    C81 O83 V2 O73 . . . . -173.3(2) n
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    _geom_hbond_publ_flag
    O33 H33 F10 2_755 0.778(16) 1.903(17) 2.674(2) 171(3) y
    O43 H43 F11 2_655 0.804(16) 1.900(18) 2.690(2) 168(3) y
    O63 H63 F21 2_666 0.805(17) 1.852(18) 2.655(3) 175(4) y
    O73 H73 F20 2_766 0.800(17) 1.967(17) 2.765(2) 175(3) y
_shelxl_version_number         .2013
