#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:42:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179258 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/78/4317854.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_4317854
loop_
_publ_author_name
'Shyamali Ghosh'
'Kausik K. Nanda'
'Anthony W. Addison'
'Raymond J. Butcher'
_publ_section_title
;
 Mononuclear and Mixed-Valence Binuclear Oxovanadium Complexes with
 Benzimidazole-Derived Chelating Agents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2243
_journal_page_last               2249
_journal_paper_doi               10.1021/ic010945x
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C51 H48 F9 N14 O15 S3 V2'
_chemical_formula_weight         1466.09
_chemical_name_systematic
;
    ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 109.274(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.505(2)
_cell_length_b                   21.376(4)
_cell_length_c                   13.547(2)
_cell_measurement_temperature    293(2)
_cell_volume                     3144.9(10)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_sigmaI/netI    0.1140
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7760
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    0.498
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_F_000             1494
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.028
_refine_ls_goodness_of_fit_obs   1.172
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         7402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_restrained_S_obs      1.172
_refine_ls_R_factor_all          0.2192
_refine_ls_R_factor_obs          0.0942
_refine_ls_shift/esd_max         -0.534
_refine_ls_shift/esd_mean        0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1278P)²+4.7640P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3172
_refine_ls_wR_factor_obs         0.2245
_reflns_number_observed          3000
_reflns_number_total             7406
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010945x_2.cif
_cod_data_source_block           '[(H3ntb)VIVO(m-O)VVO(H3ntb)](CF3SO3)3.2H2O'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1278P)^2^+4.7640P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1278P)^2^+4.7640P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3145.1(10)
_cod_database_code               4317854
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
V V 0.54784(10) 0.50973(5) 0.38393(9) 0.0458(4) Uani 1 d . .
S1 S 0.1492(4) 0.2500 0.2031(3) 0.0941(12) Uani 1 d S .
S2 S 0.6026(5) 0.2500 0.0232(5) 0.125(2) Uani 1 d S .
S3 S 0.9775(6) 0.2500 0.6462(5) 0.137(2) Uani 1 d S .
F11 F -0.0085(16) 0.2500 0.0154(11) 0.207(7) Uani 1 d S .
F12 F 0.1565(12) 0.3002(5) 0.0341(7) 0.208(5) Uani 1 d . .
F21 F 0.7067(16) 0.2500 -0.1190(13) 0.192(6) Uani 1 d S .
F22 F 0.5509(13) 0.1990(7) -0.1590(12) 0.284(7) Uani 1 d . .
F31 F 1.1242(44) 0.2500 0.7988(19) 0.443(25) Uani 1 d S .
F32 F 1.1785(15) 0.1986(8) 0.6774(14) 0.345(9) Uani 1 d . .
O O 0.5000 0.5000 0.5000 0.049(2) Uani 1 d S .
O1 O 0.5547(4) 0.5836(2) 0.3710(4) 0.0556(13) Uani 1 d . .
O1W O 0.7753(13) 0.2500 0.3686(15) 0.195(7) Uani 1 d S .
O2W O 0.8427(43) 0.3026(16) 0.2049(43) 0.740(34) Uani 1 d . .
O11 O 0.2813(11) 0.2500 0.2431(11) 0.154(5) Uani 1 d S .
O12 O 0.0934(7) 0.3066(3) 0.2223(7) 0.128(3) Uani 1 d . .
O21 O 0.4778(18) 0.2500 0.0094(23) 0.280(13) Uani 1 d S .
O22 O 0.6597(12) 0.3056(4) 0.0578(9) 0.186(5) Uani 1 d . .
O31 O 0.9829(40) 0.2500 0.5350(14) 0.414(24) Uani 1 d S .
O32 O 0.9407(12) 0.3058(5) 0.6689(11) 0.212(5) Uani 1 d . .
N N 0.5461(5) 0.3961(2) 0.3774(4) 0.0501(14) Uani 1 d . .
N1A N 0.5977(5) 0.4865(3) 0.2518(4) 0.0468(13) Uani 1 d . .
N2A N 0.6321(5) 0.4208(3) 0.1381(4) 0.057(2) Uani 1 d . .
H2AB H 0.6390(5) 0.3861(3) 0.1085(4) 0.061(22) Uiso 1 calc R .
N1B N 0.3718(5) 0.4857(3) 0.2959(4) 0.0489(13) Uani 1 d . .
N2B N 0.2155(6) 0.4209(3) 0.2436(5) 0.062(2) Uani 1 d . .
H2BB H 0.1745(6) 0.3865(3) 0.2351(5) 0.033(17) Uiso 1 calc R .
N1C N 0.7208(5) 0.4836(3) 0.4749(4) 0.0483(13) Uani 1 d . .
N2C N 0.8536(6) 0.4168(3) 0.5768(5) 0.059(2) Uani 1 d . .
H2CB H 0.8842(6) 0.3821(3) 0.6062(5) 0.051(21) Uiso 1 calc R .
C1 C 0.1095(27) 0.2500 0.0572(16) 0.129(7) Uani 1 d S .
C2 C 0.5848(43) 0.2500 -0.1103(26) 0.206(15) Uani 1 d S .
C3 C 1.1632(33) 0.2500 0.7277(44) 0.240(24) Uani 1 d S .
C1A C 0.6277(6) 0.5210(4) 0.1754(5) 0.048(2) Uani 1 d . .
C2A C 0.6382(7) 0.5846(4) 0.1639(6) 0.061(2) Uani 1 d . .
H2AA H 0.6247(7) 0.6126(4) 0.2115(6) 0.036(16) Uiso 1 calc R .
C3A C 0.6694(8) 0.6057(4) 0.0796(6) 0.074(2) Uani 1 d . .
H3AA H 0.6782(8) 0.6483(4) 0.0704(6) 0.129(40) Uiso 1 calc R .
C4A C 0.6879(8) 0.5628(5) 0.0075(7) 0.078(3) Uani 1 d . .
H4AA H 0.7055(8) 0.5782(5) -0.0502(7) 0.077(25) Uiso 1 calc R .
C5A C 0.6812(7) 0.4993(5) 0.0190(6) 0.072(2) Uani 1 d . .
H5AA H 0.6965(7) 0.4712(5) -0.0278(6) 0.118(37) Uiso 1 calc R .
C6A C 0.6502(6) 0.4793(3) 0.1047(5) 0.053(2) Uani 1 d . .
C7A C 0.6017(7) 0.4270(3) 0.2247(5) 0.053(2) Uani 1 d . .
C8A C 0.5759(9) 0.3737(4) 0.2855(6) 0.067(2) Uani 1 d . .
H8AA H 0.5074(9) 0.3494(4) 0.2409(6) 0.062(22) Uiso 1 calc R .
H8AB H 0.6474(9) 0.3465(4) 0.3085(6) 0.095(30) Uiso 1 calc R .
C1B C 0.2685(6) 0.5191(4) 0.2337(5) 0.052(2) Uani 1 d . .
C2B C 0.2544(8) 0.5818(4) 0.2054(6) 0.064(2) Uani 1 d . .
H2BA H 0.3204(8) 0.6096(4) 0.2266(6) 0.059(22) Uiso 1 calc R .
C3B C 0.1414(9) 0.6009(5) 0.1461(7) 0.080(3) Uani 1 d . .
H3BA H 0.1293(9) 0.6427(5) 0.1264(7) 0.087(30) Uiso 1 calc R .
C4B C 0.0431(10) 0.5603(6) 0.1138(8) 0.093(3) Uani 1 d . .
H4BA H -0.0334(10) 0.5756(6) 0.0732(8) 0.132(41) Uiso 1 calc R .
C5B C 0.0541(8) 0.4984(6) 0.1394(6) 0.082(3) Uani 1 d . .
H5BA H -0.0125(8) 0.4711(6) 0.1168(6) 0.077(27) Uiso 1 calc R .
C6B C 0.1699(7) 0.4782(4) 0.2007(6) 0.062(2) Uani 1 d . .
C7B C 0.3344(7) 0.4278(3) 0.3008(5) 0.053(2) Uani 1 d . .
C8B C 0.4173(7) 0.3803(3) 0.3693(6) 0.055(2) Uani 1 d . .
H8BA H 0.4085(7) 0.3808(3) 0.4381(6) 0.048(18) Uiso 1 calc R .
H8BB H 0.3963(7) 0.3389(3) 0.3397(6) 0.040(16) Uiso 1 calc R .
C1C C 0.8278(6) 0.5172(4) 0.5272(5) 0.051(2) Uani 1 d . .
C2C C 0.8582(7) 0.5795(4) 0.5257(6) 0.062(2) Uani 1 d . .
H2CA H 0.8033(7) 0.6079(4) 0.4827(6) 0.033(16) Uiso 1 calc R .
C3C C 0.9717(8) 0.5980(5) 0.5898(7) 0.076(3) Uani 1 d . .
H3CA H 0.9942(8) 0.6399(5) 0.5912(7) 0.073(25) Uiso 1 calc R .
C4C C 1.0551(8) 0.5547(6) 0.6535(7) 0.084(3) Uani 1 d . .
H4CA H 1.1313(8) 0.5690(6) 0.6966(7) 0.061(22) Uiso 1 calc R .
C5C C 1.0292(7) 0.4925(5) 0.6548(7) 0.074(2) Uani 1 d . .
H5CA H 1.0862(7) 0.4641(5) 0.6956(7) 0.064(24) Uiso 1 calc R .
C6C C 0.9129(7) 0.4742(4) 0.5918(6) 0.057(2) Uani 1 d . .
C7C C 0.7403(7) 0.4249(3) 0.5082(6) 0.051(2) Uani 1 d . .
C8C C 0.6389(7) 0.3766(3) 0.4774(6) 0.062(2) Uani 1 d . .
H8CA H 0.6725(7) 0.3361(3) 0.4693(6) 0.062(21) Uiso 1 calc R .
H8CB H 0.6010(7) 0.3733(3) 0.5314(6) 0.060(21) Uiso 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'
F F 0.0171 0.0103 '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_
_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
O1 V O 104.2(2) . . ?
O1 V N1C 105.3(2) . . ?
O V N1C 87.72(15) . . ?
O1 V N1B 105.1(2) . . ?
O V N1B 87.26(15) . . ?
N1C V N1B 149.6(2) . . ?
O1 V N1A 95.9(2) . . ?
O V N1A 159.9(2) . . ?
N1C V N1A 87.9(2) . . ?
N1B V N1A 86.6(2) . . ?
O1 V N 170.5(2) . . ?
O V N 85.23(14) . . ?
N1C V N 75.1(2) . . ?
N1B V N 74.6(2) . . ?
N1A V N 74.7(2) . . ?
O12 S1 O12 115.2(7) 4_565 . ?
O12 S1 O11 114.4(4) 4_565 . ?
O12 S1 O11 114.4(4) . . ?
O12 S1 C1 102.9(6) 4_565 . ?
O12 S1 C1 102.9(6) . . ?
O11 S1 C1 104.9(11) . . ?
O22 S2 O22 121.2(12) 4_565 . ?
O22 S2 O21 114.0(7) 4_565 . ?
O22 S2 O21 114.0(7) . . ?
O22 S2 C2 103.5(9) 4_565 . ?
O22 S2 C2 103.5(9) . . ?
O21 S2 C2 95.6(19) . . ?
O32 S3 O32 126.5(13) . 4_565 ?
O32 S3 O31 110.3(8) . . ?
O32 S3 O31 110.3(8) 4_565 . ?
O32 S3 C3 103.2(8) . . ?
O32 S3 C3 103.2(8) 4_565 . ?
O31 S3 C3 99.0(20) . . ?
V O V 179.999(1) . 3_666 ?
C8A N C8C 112.4(6) . . ?
C8A N C8B 111.5(6) . . ?
C8C N C8B 113.8(6) . . ?
C8A N V 110.7(4) . . ?
C8C N V 104.7(4) . . ?
C8B N V 103.0(4) . . ?
C7A N1A C1A 105.1(5) . . ?
C7A N1A V 120.2(4) . . ?
C1A N1A V 134.7(5) . . ?
C7A N2A C6A 108.2(6) . . ?
C7B N1B C1B 106.3(6) . . ?
C7B N1B V 118.8(5) . . ?
C1B N1B V 134.5(5) . . ?
C7B N2B C6B 108.5(6) . . ?
C7C N1C C1C 107.0(6) . . ?
C7C N1C V 119.1(5) . . ?
C1C N1C V 133.2(5) . . ?
C7C N2C C6C 107.8(6) . . ?
F11 C1 F12 111.1(15) . 4_565 ?
F11 C1 F12 111.1(15) . . ?
F12 C1 F12 113.1(22) 4_565 . ?
F11 C1 S1 108.6(16) . . ?
F12 C1 S1 106.3(12) 4_565 . ?
F12 C1 S1 106.3(12) . . ?
F22 C2 F22 118.6(36) . 4_565 ?
F22 C2 F21 95.6(20) . . ?
F22 C2 F21 95.6(20) 4_565 . ?
F22 C2 S2 116.7(15) . . ?
F22 C2 S2 116.7(15) 4_565 . ?
F21 C2 S2 107.3(28) . . ?
F31 C3 F32 124.2(17) . . ?
F31 C3 F32 124.2(17) . 4_565 ?
F32 C3 F32 110.8(40) . 4_565 ?
F31 C3 S3 80.3(28) . . ?
F32 C3 S3 90.9(25) . . ?
F32 C3 S3 90.9(25) 4_565 . ?
C2A C1A C6A 120.6(7) . . ?
C2A C1A N1A 130.9(6) . . ?
C6A C1A N1A 108.5(6) . . ?
C1A C2A C3A 118.1(8) . . ?
C2A C3A C4A 120.2(9) . . ?
C5A C4A C3A 122.6(8) . . ?
C4A C5A C6A 116.0(8) . . ?
N2A C6A C5A 131.7(7) . . ?
N2A C6A C1A 105.9(6) . . ?
C5A C6A C1A 122.4(7) . . ?
N1A C7A N2A 112.3(6) . . ?
N1A C7A C8A 123.1(6) . . ?
N2A C7A C8A 124.5(6) . . ?
N C8A C7A 111.2(6) . . ?
C6B C1B C2B 120.8(8) . . ?
C6B C1B N1B 108.3(7) . . ?
C2B C1B N1B 130.9(7) . . ?
C3B C2B C1B 117.2(9) . . ?
C2B C3B C4B 122.0(10) . . ?
C5B C4B C3B 122.2(10) . . ?
C4B C5B C6B 116.5(9) . . ?
N2B C6B C5B 133.2(8) . . ?
N2B C6B C1B 105.5(7) . . ?
C5B C6B C1B 121.3(9) . . ?
N1B C7B N2B 111.3(7) . . ?
N1B C7B C8B 121.2(6) . . ?
N2B C7B C8B 127.3(7) . . ?
N C8B C7B 108.0(6) . . ?
C2C C1C N1C 132.3(7) . . ?
C2C C1C C6C 120.6(7) . . ?
N1C C1C C6C 107.0(7) . . ?
C3C C2C C1C 117.6(9) . . ?
C2C C3C C4C 121.0(9) . . ?
C5C C4C C3C 122.8(9) . . ?
C4C C5C C6C 116.0(9) . . ?
C5C C6C N2C 132.0(8) . . ?
C5C C6C C1C 121.9(8) . . ?
N2C C6C C1C 106.1(7) . . ?
N1C C7C N2C 112.0(6) . . ?
N1C C7C C8C 121.6(6) . . ?
N2C C7C C8C 126.2(7) . . ?
N C8C C7C 108.6(6) . . ?
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
V O1 1.594(5) . ?
V O 1.8412(11) . ?
V N1C 2.043(6) . ?
V N1B 2.048(6) . ?
V N1A 2.111(5) . ?
V N 2.430(5) . ?
S1 O12 1.432(7) 4_565 ?
S1 O12 1.432(7) . ?
S1 O11 1.436(12) . ?
S1 C1 1.88(2) . ?
S2 O22 1.364(9) 4_565 ?
S2 O22 1.364(9) . ?
S2 O21 1.39(2) . ?
S2 C2 1.75(3) . ?
S3 O32 1.334(10) . ?
S3 O32 1.334(10) 4_565 ?
S3 O31 1.53(2) . ?
S3 C3 2.06(4) . ?
F11 C1 1.29(2) . ?
F12 C1 1.286(14) . ?
F21 C2 1.45(4) . ?
F22 C2 1.27(2) . ?
F31 C3 1.19(4) . ?
F32 C3 1.33(3) . ?
O V 1.8413(11) 3_666 ?
N C8A 1.477(9) . ?
N C8C 1.481(9) . ?
N C8B 1.488(8) . ?
N1A C7A 1.330(8) . ?
N1A C1A 1.403(8) . ?
N2A C7A 1.336(8) . ?
N2A C6A 1.369(9) . ?
N1B C7B 1.319(8) . ?
N1B C1B 1.404(9) . ?
N2B C7B 1.339(9) . ?
N2B C6B 1.383(10) . ?
N1C C7C 1.328(8) . ?
N1C C1C 1.399(9) . ?
N2C C7C 1.339(9) . ?
N2C C6C 1.387(10) . ?
C1 F12 1.286(14) 4_565 ?
C2 F22 1.27(2) 4_565 ?
C3 F32 1.33(3) 4_565 ?
C1A C2A 1.379(10) . ?
C1A C6A 1.394(10) . ?
C2A C3A 1.380(10) . ?
C3A C4A 1.405(12) . ?
C4A C5A 1.373(12) . ?
C5A C6A 1.389(10) . ?
C7A C8A 1.493(10) . ?
C1B C6B 1.385(10) . ?
C1B C2B 1.389(11) . ?
C2B C3B 1.346(11) . ?
C3B C4B 1.378(14) . ?
C4B C5B 1.363(13) . ?
C5B C6B 1.386(12) . ?
C7B C8B 1.490(10) . ?
C1C C2C 1.379(10) . ?
C1C C6C 1.416(10) . ?
C2C C3C 1.367(11) . ?
C3C C4C 1.406(13) . ?
C4C C5C 1.363(13) . ?
C5C C6C 1.385(11) . ?
C7C C8C 1.509(10) . ?
