#------------------------------------------------------------------------------
#$Date: 2019-11-23 11:51:13 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233174 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/56/7235609.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7235609
loop_
_publ_author_name
'Ghorai, Samir'
'Mukherjee, Chandan'
_publ_section_title
;
 Synthesis and characterization of a tetraradical-containing octanuclear
 vanadium cluster formed via ligand C--N bond breaking and C--O bond
 making
;
_journal_issue                   47
_journal_name_full               'RSC Advances'
_journal_page_first              24698
_journal_paper_doi               10.1039/c4ra02159b
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C60 H92 O32 S2 V8, 2(C16 H36 N)'
_chemical_formula_sum            'C92 H164 N2 O32 S2 V8'
_chemical_formula_weight         2281.89
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                WGT-CM-517-17
_audit_creation_date             2012-05-11
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.855(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.1675(12)
_cell_length_b                   20.323(2)
_cell_length_c                   20.135(3)
_cell_measurement_reflns_used    181957
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.0995
_cell_measurement_theta_min      2.6923
_cell_volume                     5760.5(12)
_computing_cell_refinement       'DENZO (Bruker AXS, 2006)'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'DENZO (Bruker AXS, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD φ- and ω-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            164119
_diffrn_reflns_theta_full        33.07
_diffrn_reflns_theta_max         33.07
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  0.89215
_exptl_absorpt_correction_T_min  0.71712
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2404
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.898
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         21758
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0489P)²+9.2104P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1411
_reflns_number_gt                15539
_reflns_number_total             21758
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra02159b1.cif
_cod_data_source_block           7804
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'MONOCLINIC' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        5760.5(11)
_cod_original_sg_symbol_Hall     '-p 2yn'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7235609
loop_
_symmetry_equiv_pos_as_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'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.23715(2) 0.079238(18) 0.499157(18) 0.01580(7) Uani 1 1 d . . .
V2 V 0.01034(2) 0.114404(18) 0.400185(18) 0.01586(7) Uani 1 1 d . . .
V3 V 0.08697(3) 0.177203(18) 0.566825(19) 0.01716(7) Uani 1 1 d . . .
V4 V 0.10105(2) 0.027750(18) 0.568060(18) 0.01580(7) Uani 1 1 d . . .
O51 O 0.32885(10) 0.08038(8) 0.57167(8) 0.0208(3) Uani 1 1 d . . .
O52 O -0.06903(11) 0.11749(8) 0.32182(8) 0.0224(3) Uani 1 1 d . . .
O53 O 0.16635(12) 0.18697(9) 0.64471(8) 0.0238(3) Uani 1 1 d . . .
O54 O 0.17807(11) 0.02169(9) 0.64739(8) 0.0228(3) Uani 1 1 d . . .
O55 O 0.02545(10) -0.03700(7) 0.55968(8) 0.0176(3) Uani 1 1 d . . .
O56 O 0.12840(10) 0.10774(7) 0.51903(8) 0.0160(3) Uani 1 1 d . . .
O61 O 0.18219(10) -0.00452(8) 0.51726(8) 0.0175(3) Uani 1 1 d . . .
C62 C 0.24074(17) -0.06123(12) 0.54288(14) 0.0274(5) Uani 1 1 d . . .
H62A H 0.2866 -0.0528 0.5914 0.041 Uiso 1 1 calc R . .
H62B H 0.2749 -0.0708 0.5112 0.041 Uiso 1 1 calc R . .
H62C H 0.2009 -0.0990 0.5437 0.041 Uiso 1 1 calc R . .
O71 O 0.02329(11) 0.09803(8) 0.58428(8) 0.0186(3) Uani 1 1 d . . .
C72 C -0.02651(18) 0.09102(13) 0.63145(14) 0.0272(5) Uani 1 1 d . . .
H72A H -0.0797 0.0604 0.6106 0.041 Uiso 1 1 calc R . .
H72B H -0.0509 0.1340 0.6387 0.041 Uiso 1 1 calc R . .
H72C H 0.0167 0.0738 0.6775 0.041 Uiso 1 1 calc R . .
O1 O 0.29633(10) 0.04725(8) 0.43925(8) 0.0181(3) Uani 1 1 d . . .
C2 C 0.25179(15) 0.03640(11) 0.36965(11) 0.0183(4) Uani 1 1 d . A .
C3 C 0.29785(16) 0.01517(12) 0.32357(12) 0.0227(4) Uani 1 1 d . . .
C4 C 0.23939(18) 0.00231(12) 0.25369(12) 0.0252(4) Uani 1 1 d . A .
H4 H 0.2682 -0.0119 0.2216 0.030 Uiso 1 1 calc R . .
C5 C 0.13979(17) 0.00892(11) 0.22685(12) 0.0229(4) Uani 1 1 d D . .
C6 C 0.09637(16) 0.03302(11) 0.27173(11) 0.0196(4) Uani 1 1 d . A .
H6 H 0.0296 0.0399 0.2542 0.024 Uiso 1 1 calc R . .
C7 C 0.15217(15) 0.04694(10) 0.34295(11) 0.0171(4) Uani 1 1 d . . .
O8 O 0.12007(10) 0.06779(8) 0.39247(8) 0.0174(3) Uani 1 1 d . A .
C9 C 0.40562(18) 0.00608(14) 0.35182(14) 0.0296(5) Uani 1 1 d . . .
C10 C 0.45590(19) 0.07061(16) 0.38397(16) 0.0358(6) Uani 1 1 d . . .
H10A H 0.4385 0.1047 0.3469 0.054 Uiso 1 1 calc R . .
H10B H 0.5248 0.0639 0.4024 0.054 Uiso 1 1 calc R . .
H10C H 0.4365 0.0844 0.4231 0.054 Uiso 1 1 calc R . .
C11 C 0.4337(2) -0.04822(15) 0.40852(16) 0.0364(6) Uani 1 1 d . . .
H11A H 0.4157 -0.0351 0.4486 0.055 Uiso 1 1 calc R . .
H11B H 0.5025 -0.0552 0.4258 0.055 Uiso 1 1 calc R . .
H11C H 0.4009 -0.0891 0.3875 0.055 Uiso 1 1 calc R . .
C12 C 0.4403(2) -0.01436(19) 0.29234(16) 0.0442(8) Uani 1 1 d . . .
H12A H 0.4120 -0.0568 0.2724 0.066 Uiso 1 1 calc R . .
H12B H 0.5096 -0.0183 0.3121 0.066 Uiso 1 1 calc R . .
H12C H 0.4213 0.0190 0.2545 0.066 Uiso 1 1 calc R . .
C13 C 0.0765(5) -0.0114(3) 0.1498(4) 0.0226(6) Uani 0.473(3) 1 d PD A 1
C14 C -0.0310(4) -0.0095(4) 0.1318(3) 0.0393(10) Uani 0.473(3) 1 d PD A 1
H14A H -0.0465 -0.0363 0.1665 0.059 Uiso 0.473(3) 1 calc PR A 1
H14B H -0.0642 -0.0272 0.0835 0.059 Uiso 0.473(3) 1 calc PR A 1
H14C H -0.0511 0.0360 0.1338 0.059 Uiso 0.473(3) 1 calc PR A 1
C15 C 0.1011(5) -0.0827(3) 0.1362(3) 0.0378(9) Uani 0.473(3) 1 d PD A 1
H15A H 0.1678 -0.0850 0.1412 0.057 Uiso 0.473(3) 1 calc PR A 1
H15B H 0.0603 -0.0961 0.0877 0.057 Uiso 0.473(3) 1 calc PR A 1
H15C H 0.0907 -0.1122 0.1711 0.057 Uiso 0.473(3) 1 calc PR A 1
C16 C 0.1016(5) 0.0345(3) 0.0990(3) 0.0345(8) Uani 0.473(3) 1 d PD A 1
H16A H 0.0883 0.0801 0.1080 0.052 Uiso 0.473(3) 1 calc PR A 1
H16B H 0.0634 0.0228 0.0493 0.052 Uiso 0.473(3) 1 calc PR A 1
H16C H 0.1692 0.0299 0.1072 0.052 Uiso 0.473(3) 1 calc PR A 1
C91 C -0.2567(2) 0.11986(18) 0.1440(2) 0.0546(9) Uani 0.637(19) 1 d PD B 1
H91A H -0.3112 0.1436 0.1089 0.066 Uiso 0.637(19) 1 calc PR B 1
H91B H -0.2588 0.1271 0.1920 0.066 Uiso 0.637(19) 1 calc PR B 1
C92 C -0.2688(9) 0.0455(4) 0.1268(10) 0.086(4) Uani 0.637(19) 1 d PD B 1
H92A H -0.2733 0.0381 0.0775 0.129 Uiso 0.637(19) 1 calc PR B 1
H92B H -0.3268 0.0296 0.1321 0.129 Uiso 0.637(19) 1 calc PR B 1
H92C H -0.2139 0.0215 0.1598 0.129 Uiso 0.637(19) 1 calc PR B 1
C13' C 0.0855(5) -0.0088(3) 0.1484(4) 0.0226(6) Uani 0.527(3) 1 d PD A 2
C14' C 0.0011(4) -0.0515(3) 0.1456(3) 0.0393(10) Uani 0.527(3) 1 d PD A 2
H14D H 0.0241 -0.0896 0.1771 0.059 Uiso 0.527(3) 1 calc PR A 2
H14E H -0.0330 -0.0666 0.0964 0.059 Uiso 0.527(3) 1 calc PR A 2
H14F H -0.0420 -0.0256 0.1615 0.059 Uiso 0.527(3) 1 calc PR A 2
C15' C 0.1437(4) -0.0474(3) 0.1129(3) 0.0378(9) Uani 0.527(3) 1 d PD A 2
H15D H 0.1943 -0.0192 0.1095 0.057 Uiso 0.527(3) 1 calc PR A 2
H15E H 0.1020 -0.0613 0.0648 0.057 Uiso 0.527(3) 1 calc PR A 2
H15F H 0.1719 -0.0863 0.1418 0.057 Uiso 0.527(3) 1 calc PR A 2
C16' C 0.0507(4) 0.0550(3) 0.1066(3) 0.0345(8) Uani 0.527(3) 1 d PD A 2
H16D H 0.0078 0.0778 0.1252 0.052 Uiso 0.527(3) 1 calc PR A 2
H16E H 0.0168 0.0448 0.0559 0.052 Uiso 0.527(3) 1 calc PR A 2
H16F H 0.1053 0.0833 0.1120 0.052 Uiso 0.527(3) 1 calc PR A 2
C91' C -0.2567(2) 0.11986(18) 0.1440(2) 0.0546(9) Uani 0.363(19) 1 d P B 2
H91C H -0.3055 0.1547 0.1344 0.066 Uiso 0.363(19) 1 calc PR B 2
H91D H -0.2450 0.1014 0.1920 0.066 Uiso 0.363(19) 1 calc PR B 2
C92' C -0.2937(16) 0.0647(10) 0.0868(13) 0.086(4) Uani 0.363(19) 1 d PD B 2
H92D H -0.3049 0.0829 0.0393 0.129 Uiso 0.363(19) 1 calc PR B 2
H92E H -0.3533 0.0469 0.0877 0.129 Uiso 0.363(19) 1 calc PR B 2
H92F H -0.2464 0.0295 0.0973 0.129 Uiso 0.363(19) 1 calc PR B 2
O21 O -0.00172(11) 0.23924(8) 0.57261(8) 0.0210(3) Uani 1 1 d . . .
C22 C -0.08221(16) 0.25203(11) 0.51883(12) 0.0210(4) Uani 1 1 d . . .
C23 C -0.14850(18) 0.30089(13) 0.52062(13) 0.0270(5) Uani 1 1 d . . .
C24 C -0.22938(18) 0.30663(14) 0.45962(14) 0.0295(5) Uani 1 1 d . . .
H24 H -0.2746 0.3392 0.4591 0.035 Uiso 1 1 calc R . .
C25 C -0.24960(17) 0.26699(13) 0.39727(13) 0.0258(5) Uani 1 1 d . . .
C26 C -0.18353(15) 0.22031(12) 0.39613(12) 0.0211(4) Uani 1 1 d . . .
H26 H -0.1947 0.1936 0.3550 0.025 Uiso 1 1 calc R . .
C27 C -0.10041(15) 0.21326(11) 0.45642(12) 0.0197(4) Uani 1 1 d . . .
O28 O -0.03329(11) 0.16989(8) 0.46197(8) 0.0196(3) Uani 1 1 d . . .
C29 C -0.1284(2) 0.34473(16) 0.58678(15) 0.0374(6) Uani 1 1 d . . .
C30 C -0.1266(2) 0.30168(19) 0.64964(15) 0.0429(7) Uani 1 1 d . . .
H30A H -0.1142 0.3292 0.6921 0.064 Uiso 1 1 calc R . .
H30B H -0.0764 0.2686 0.6595 0.064 Uiso 1 1 calc R . .
H30C H -0.1881 0.2797 0.6375 0.064 Uiso 1 1 calc R . .
C31 C -0.0330(3) 0.38029(16) 0.60474(18) 0.0444(7) Uani 1 1 d . . .
H31A H -0.0349 0.4070 0.5637 0.067 Uiso 1 1 calc R . .
H31B H 0.0181 0.3478 0.6155 0.067 Uiso 1 1 calc R . .
H31C H -0.0214 0.4088 0.6464 0.067 Uiso 1 1 calc R . .
C32 C -0.2068(3) 0.3965(2) 0.5741(2) 0.0651(12) Uani 1 1 d . . .
H32A H -0.2677 0.3743 0.5644 0.098 Uiso 1 1 calc R . .
H32B H -0.2110 0.4239 0.5330 0.098 Uiso 1 1 calc R . .
H32C H -0.1917 0.4241 0.6168 0.098 Uiso 1 1 calc R . .
C33 C -0.33962(18) 0.27929(16) 0.33209(14) 0.0328(6) Uani 1 1 d . . .
C34 C -0.35264(18) 0.22965(15) 0.27227(14) 0.0336(6) Uani 1 1 d . . .
H34A H -0.2982 0.2320 0.2573 0.050 Uiso 1 1 calc R . .
H34B H -0.4110 0.2399 0.2314 0.050 Uiso 1 1 calc R . .
H34C H -0.3571 0.1852 0.2896 0.050 Uiso 1 1 calc R . .
C35 C -0.3333(3) 0.34884(17) 0.30436(17) 0.0460(8) Uani 1 1 d . . .
H35A H -0.3286 0.3811 0.3417 0.069 Uiso 1 1 calc R . .
H35B H -0.3903 0.3578 0.2619 0.069 Uiso 1 1 calc R . .
H35C H -0.2770 0.3520 0.2917 0.069 Uiso 1 1 calc R . .
C36 C -0.4277(2) 0.2744(2) 0.35282(18) 0.0574(11) Uani 1 1 d . . .
H36A H -0.4319 0.2299 0.3701 0.086 Uiso 1 1 calc R . .
H36B H -0.4850 0.2839 0.3108 0.086 Uiso 1 1 calc R . .
H36C H -0.4220 0.3064 0.3906 0.086 Uiso 1 1 calc R . .
S40 S 0.16884(4) 0.22525(3) 0.45106(3) 0.01977(10) Uani 1 1 d . . .
O41 O 0.24503(11) 0.17349(8) 0.47032(8) 0.0203(3) Uani 1 1 d . . .
O42 O 0.08300(11) 0.19759(8) 0.39336(8) 0.0201(3) Uani 1 1 d . . .
O43 O 0.14413(12) 0.23914(8) 0.51527(8) 0.0218(3) Uani 1 1 d . . .
O44 O 0.20099(13) 0.28410(9) 0.42795(10) 0.0276(4) Uani 1 1 d . . .
N80 N -0.06470(14) 0.25610(10) 0.17836(10) 0.0230(4) Uani 1 1 d . . .
C81 C -0.06519(19) 0.27567(14) 0.10497(13) 0.0300(5) Uani 1 1 d . . .
H81A H -0.1277 0.2959 0.0778 0.036 Uiso 1 1 calc R . .
H81B H -0.0167 0.3104 0.1125 0.036 Uiso 1 1 calc R . .
C82 C -0.0474(3) 0.22330(17) 0.05772(18) 0.0502(8) Uani 1 1 d . . .
H82A H -0.1051 0.1961 0.0356 0.060 Uiso 1 1 calc R . .
H82B H 0.0050 0.1941 0.0869 0.060 Uiso 1 1 calc R . .
C83 C -0.0210(2) 0.2565(2) -0.00120(16) 0.0505(9) Uani 1 1 d . . .
H83A H -0.0338 0.2257 -0.0418 0.061 Uiso 1 1 calc R . .
H83B H -0.0611 0.2959 -0.0190 0.061 Uiso 1 1 calc R . .
C84 C 0.0839(4) 0.2766(3) 0.0269(3) 0.095(2) Uani 1 1 d . . .
H84A H 0.0976 0.3048 0.0690 0.143 Uiso 1 1 calc R . .
H84B H 0.0972 0.3007 -0.0105 0.143 Uiso 1 1 calc R . .
H84C H 0.1238 0.2371 0.0400 0.143 Uiso 1 1 calc R . .
C85 C -0.06864(19) 0.32152(12) 0.21462(13) 0.0263(5) Uani 1 1 d . . .
H85A H -0.0157 0.3494 0.2135 0.032 Uiso 1 1 calc R . .
H85B H -0.1285 0.3440 0.1856 0.032 Uiso 1 1 calc R . .
C86 C -0.0631(2) 0.31833(12) 0.29159(13) 0.0281(5) Uani 1 1 d . . .
H86A H -0.0091 0.2902 0.3203 0.034 Uiso 1 1 calc R . .
H86B H -0.1222 0.2988 0.2930 0.034 Uiso 1 1 calc R . .
C87 C -0.0500(3) 0.38755(14) 0.32293(16) 0.0402(7) Uani 1 1 d . . .
H87A H -0.1055 0.4148 0.2949 0.048 Uiso 1 1 calc R . .
H87B H 0.0071 0.4076 0.3186 0.048 Uiso 1 1 calc R . .
C88 C -0.0391(3) 0.38790(16) 0.40141(17) 0.0439(7) Uani 1 1 d . . .
H88A H -0.0963 0.3693 0.4058 0.066 Uiso 1 1 calc R . .
H88B H -0.0303 0.4332 0.4194 0.066 Uiso 1 1 calc R . .
H88C H 0.0163 0.3614 0.4295 0.066 Uiso 1 1 calc R . .
C89 C -0.15266(17) 0.21729(13) 0.17321(15) 0.0301(5) Uani 1 1 d . B .
H89A H -0.1536 0.2143 0.2220 0.036 Uiso 1 1 calc R . .
H89B H -0.2088 0.2435 0.1442 0.036 Uiso 1 1 calc R . .
C90 C -0.1660(2) 0.14940(17) 0.1428(2) 0.0479(8) Uani 1 1 d . . .
H90A H -0.1114 0.1215 0.1711 0.057 Uiso 1 1 calc R B 1
H90B H -0.1687 0.1509 0.0929 0.057 Uiso 1 1 calc R B 1
C93 C 0.02420(16) 0.21784(11) 0.22135(12) 0.0221(4) Uani 1 1 d . . .
H93A H 0.0178 0.2020 0.2659 0.027 Uiso 1 1 calc R . .
H93B H 0.0282 0.1786 0.1934 0.027 Uiso 1 1 calc R . .
C94 C 0.11644(17) 0.25602(12) 0.24132(13) 0.0257(5) Uani 1 1 d . . .
H94A H 0.1206 0.2886 0.2790 0.031 Uiso 1 1 calc R . .
H94B H 0.1174 0.2803 0.1989 0.031 Uiso 1 1 calc R . .
C95 C 0.20166(18) 0.20962(13) 0.26850(14) 0.0291(5) Uani 1 1 d . . .
H95A H 0.2008 0.1800 0.2292 0.035 Uiso 1 1 calc R . .
H95B H 0.1968 0.1821 0.3076 0.035 Uiso 1 1 calc R . .
C96 C 0.2953(2) 0.24762(17) 0.29604(17) 0.0389(6) Uani 1 1 d . . .
H96A H 0.2995 0.2758 0.2578 0.058 Uiso 1 1 calc R . .
H96B H 0.3485 0.2165 0.3110 0.058 Uiso 1 1 calc R . .
H96C H 0.2981 0.2749 0.3369 0.058 Uiso 1 1 calc R . .
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'
S S 0.1246 0.1234 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 -1.00 0.1500
0.00 0.00 1.00 0.1500
1.00 0.00 -1.00 0.1300
-1.00 0.00 1.00 0.1300
0.00 -1.00 1.00 0.1100
0.00 1.00 -1.00 0.1100
1.00 0.00 3.00 0.1700
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
O51 V1 O1 97.53(7) . .
O51 V1 O56 109.10(7) . .
O1 V1 O56 153.32(7) . .
O51 V1 O61 97.27(8) . .
O1 V1 O61 98.94(7) . .
O56 V1 O61 76.66(6) . .
O51 V1 O41 97.15(8) . .
O1 V1 O41 92.89(7) . .
O56 V1 O41 85.49(6) . .
O61 V1 O41 159.95(6) . .
O51 V1 O8 172.16(7) . .
O1 V1 O8 75.14(6) . .
O56 V1 O8 78.18(6) . .
O61 V1 O8 81.35(6) . .
O41 V1 O8 86.17(6) . .
O51 V1 V4 95.45(6) . .
O1 V1 V4 137.66(5) . .
O56 V1 V4 40.18(5) . .
O61 V1 V4 39.32(4) . .
O41 V1 V4 125.15(5) . .
O8 V1 V4 88.36(4) . .
O52 V2 O55 102.70(8) . 3_556
O52 V2 O28 107.23(8) . .
O55 V2 O28 89.38(7) 3_556 .
O52 V2 O8 106.88(8) . .
O55 V2 O8 91.06(6) 3_556 .
O28 V2 O8 144.90(6) . .
O52 V2 O42 97.36(8) . .
O55 V2 O42 159.89(6) 3_556 .
O28 V2 O42 83.42(7) . .
O8 V2 O42 84.28(7) . .
O52 V2 O56 178.76(7) . .
O55 V2 O56 76.06(6) 3_556 .
O28 V2 O56 72.76(6) . .
O8 V2 O56 73.32(6) . .
O42 V2 O56 83.87(6) . .
O53 V3 O21 98.70(8) . .
O53 V3 O56 108.25(8) . .
O21 V3 O56 152.96(7) . .
O53 V3 O71 99.60(8) . .
O21 V3 O71 97.29(7) . .
O56 V3 O71 76.44(6) . .
O53 V3 O43 96.68(8) . .
O21 V3 O43 93.90(7) . .
O56 V3 O43 85.31(6) . .
O71 V3 O43 158.58(7) . .
O53 V3 O28 174.15(8) . .
O21 V3 O28 75.55(6) . .
O56 V3 O28 77.46(6) . .
O71 V3 O28 80.31(6) . .
O43 V3 O28 84.89(6) . .
O53 V3 V4 95.23(7) . .
O21 V3 V4 135.95(5) . .
O56 V3 V4 40.83(4) . .
O71 V3 V4 39.01(5) . .
O43 V3 V4 125.69(5) . .
O28 V3 V4 88.36(4) . .
O54 V4 O55 104.68(8) . .
O54 V4 O71 98.72(8) . .
O55 V4 O71 98.88(7) . .
O54 V4 O61 97.31(8) . .
O55 V4 O61 102.51(7) . .
O71 V4 O61 148.96(7) . .
O54 V4 O56 110.13(8) . .
O55 V4 O56 145.17(7) . .
O71 V4 O56 74.97(6) . .
O61 V4 O56 74.61(6) . .
O54 V4 V3 96.22(6) . .
O55 V4 V3 136.36(5) . .
O71 V4 V3 39.45(5) . .
O61 V4 V3 112.40(5) . .
O56 V4 V3 38.83(4) . .
O54 V4 V1 96.55(6) . .
O55 V4 V1 139.14(5) . .
O71 V4 V1 112.06(5) . .
O61 V4 V1 39.46(5) . .
O56 V4 V1 37.88(4) . .
V3 V4 V1 73.321(13) . .
V4 O55 V2 149.88(9) . 3_556
V1 O56 V3 141.50(8) . .
V1 O56 V4 101.93(7) . .
V3 O56 V4 100.34(7) . .
V1 O56 V2 100.88(6) . .
V3 O56 V2 101.20(6) . .
V4 O56 V2 108.63(6) . .
C62 O61 V4 120.17(14) . .
C62 O61 V1 120.68(13) . .
V4 O61 V1 101.22(7) . .
C72 O71 V4 122.76(15) . .
C72 O71 V3 128.06(14) . .
V4 O71 V3 101.54(7) . .
C2 O1 V1 124.14(13) . .
O1 C2 C7 115.23(18) . .
O1 C2 C3 123.99(19) . .
C7 C2 C3 120.78(19) . .
C4 C3 C2 116.0(2) . .
C4 C3 C9 123.3(2) . .
C2 C3 C9 120.8(2) . .
C3 C4 C5 124.3(2) . .
C6 C5 C4 118.9(2) . .
C6 C5 C13' 123.5(3) . .
C4 C5 C13' 117.6(3) . .
C6 C5 C13 118.6(3) . .
C4 C5 C13 122.4(3) . .
C13' C5 C13 5.8(5) . .
C5 C6 C7 119.1(2) . .
O8 C7 C6 125.65(19) . .
O8 C7 C2 113.52(18) . .
C6 C7 C2 120.76(19) . .
C7 O8 V2 140.09(13) . .
C7 O8 V1 111.85(12) . .
V2 O8 V1 105.47(7) . .
C3 C9 C11 109.1(2) . .
C3 C9 C12 111.8(2) . .
C11 C9 C12 107.8(2) . .
C3 C9 C10 110.4(2) . .
C11 C9 C10 110.2(2) . .
C12 C9 C10 107.5(2) . .
C16 C13 C14 109.5(6) . .
C16 C13 C15 108.5(6) . .
C14 C13 C15 106.6(6) . .
C16 C13 C5 106.9(5) . .
C14 C13 C5 116.0(5) . .
C15 C13 C5 109.1(5) . .
C90 C91 C92 114.7(5) . .
C16' C13' C5 108.1(4) . .
C16' C13' C14' 110.4(5) . .
C5 C13' C14' 107.0(5) . .
C16' C13' C15' 108.5(5) . .
C5 C13' C15' 114.7(5) . .
C14' C13' C15' 108.1(5) . .
C22 O21 V3 123.06(14) . .
O21 C22 C27 115.59(19) . .
O21 C22 C23 124.2(2) . .
C27 C22 C23 120.2(2) . .
C24 C23 C22 116.0(2) . .
C24 C23 C29 123.1(2) . .
C22 C23 C29 120.8(2) . .
C23 C24 C25 124.4(2) . .
C26 C25 C24 118.8(2) . .
C26 C25 C33 121.3(2) . .
C24 C25 C33 119.8(2) . .
C25 C26 C27 118.7(2) . .
O28 C27 C26 124.1(2) . .
O28 C27 C22 113.95(19) . .
C26 C27 C22 121.9(2) . .
C27 O28 V2 139.46(14) . .
C27 O28 V3 111.73(13) . .
V2 O28 V3 106.78(7) . .
C30 C29 C31 110.5(3) . .
C30 C29 C23 108.8(3) . .
C31 C29 C23 110.1(2) . .
C30 C29 C32 107.6(3) . .
C31 C29 C32 108.7(3) . .
C23 C29 C32 111.2(2) . .
C25 C33 C34 112.5(2) . .
C25 C33 C35 107.9(2) . .
C34 C33 C35 109.2(2) . .
C25 C33 C36 110.2(2) . .
C34 C33 C36 107.5(3) . .
C35 C33 C36 109.5(3) . .
O44 S40 O42 111.39(10) . .
O44 S40 O43 110.30(10) . .
O42 S40 O43 108.40(9) . .
O44 S40 O41 110.25(10) . .
O42 S40 O41 107.52(9) . .
O43 S40 O41 108.90(9) . .
S40 O41 V1 128.05(9) . .
S40 O42 V2 126.32(9) . .
S40 O43 V3 128.16(10) . .
C93 N80 C89 110.12(18) . .
C93 N80 C81 111.62(18) . .
C89 N80 C81 112.4(2) . .
C93 N80 C85 110.95(18) . .
C89 N80 C85 107.13(19) . .
C81 N80 C85 104.39(18) . .
C82 C81 N80 119.1(2) . .
C81 C82 C83 109.5(3) . .
C84 C83 C82 111.3(3) . .
C86 C85 N80 116.89(19) . .
C85 C86 C87 109.4(2) . .
C86 C87 C88 112.3(2) . .
C90 C89 N80 119.3(2) . .
C89 C90 C91 110.2(3) . .
C94 C93 N80 115.14(19) . .
C93 C94 C95 110.7(2) . .
C94 C95 C96 111.5(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O51 1.5984(16) .
V1 O1 1.8680(15) .
V1 O56 1.9256(15) .
V1 O61 1.9879(16) .
V1 O41 2.0179(17) .
V1 O8 2.2321(15) .
V1 V4 3.0681(5) .
V2 O52 1.5902(16) .
V2 O55 1.9362(15) 3_556
V2 O28 1.9673(16) .
V2 O8 1.9708(15) .
V2 O42 2.0504(16) .
V2 O56 2.4001(15) .
V3 O53 1.5945(16) .
V3 O21 1.8787(16) .
V3 O56 1.9402(15) .
V3 O71 1.9745(16) .
V3 O43 2.0208(16) .
V3 O28 2.2225(16) .
V3 V4 3.0443(6) .
V4 O54 1.5944(16) .
V4 O55 1.7120(15) .
V4 O71 1.9556(16) .
V4 O61 1.9820(15) .
V4 O56 2.0234(15) .
O55 V2 1.9361(15) 3_556
O61 C62 1.429(3) .
O71 C72 1.424(3) .
O1 C2 1.328(2) .
C2 C7 1.419(3) .
C2 C3 1.420(3) .
C3 C4 1.380(3) .
C3 C9 1.529(3) .
C4 C5 1.409(3) .
C5 C6 1.391(3) .
C5 C13' 1.529(8) .
C5 C13 1.546(8) .
C6 C7 1.396(3) .
C7 O8 1.331(2) .
C9 C11 1.530(4) .
C9 C12 1.533(4) .
C9 C10 1.534(4) .
C13 C16 1.533(7) .
C13 C14 1.534(7) .
C13 C15 1.546(7) .
C91 C90 1.510(5) .
C91 C92 1.547(8) .
C13' C16' 1.528(7) .
C13' C14' 1.530(7) .
C13' C15' 1.542(7) .
O21 C22 1.322(3) .
C22 C27 1.420(3) .
C22 C23 1.423(3) .
C23 C24 1.380(4) .
C23 C29 1.536(4) .
C24 C25 1.426(4) .
C25 C26 1.386(3) .
C25 C33 1.521(3) .
C26 C27 1.394(3) .
C27 O28 1.320(3) .
C29 C30 1.531(5) .
C29 C31 1.535(5) .
C29 C32 1.536(4) .
C33 C34 1.527(4) .
C33 C35 1.536(5) .
C33 C36 1.544(4) .
S40 O44 1.4330(18) .
S40 O42 1.4949(17) .
S40 O43 1.5008(17) .
S40 O41 1.5030(17) .
N80 C93 1.518(3) .
N80 C89 1.520(3) .
N80 C81 1.528(3) .
N80 C85 1.529(3) .
C81 C82 1.517(4) .
C82 C83 1.541(5) .
C83 C84 1.531(6) .
C85 C86 1.522(3) .
C86 C87 1.524(4) .
C87 C88 1.526(4) .
C89 C90 1.493(4) .
C93 C94 1.517(3) .
C94 C95 1.527(3) .
C95 C96 1.528(4) .
