#------------------------------------------------------------------------------
#$Date: 2019-11-23 11:26:54 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233074 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/85/4348550.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_4348550
loop_
_publ_author_name
'Zhang, Yuteng'
'Wang, Xinlong'
'Li, Shuangbao'
'Song, Baiqiao'
'Shao, Kuizhan'
'Su, Zhongmin'
_publ_section_title
;
 Ligand-Directed Assembly of Polyoxovanadate-Based Metal-Organic
 Polyhedra.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8770
_journal_page_last               8775
_journal_paper_doi               10.1021/acs.inorgchem.6b01338
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C89.5 H119 Cl4 N11 O71.5 V20'
_chemical_formula_weight         3653.55
_space_group_crystal_system      cubic
_space_group_IT_number           204
_space_group_name_Hall           '-I 2 2 3'
_space_group_name_H-M_alt        'I m -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   30.062(5)
_cell_length_b                   30.062(5)
_cell_length_c                   30.062(5)
_cell_measurement_reflns_used    7032
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.66
_cell_measurement_theta_min      2.35
_cell_volume                     27168(8)
_computing_cell_refinement       'Bruker SAINT v8.34a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v8.34a'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0890
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            79821
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.122
_diffrn_reflns_theta_max         25.122
_diffrn_reflns_theta_min         1.659
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/4 Bruker AXS Madison WI USA'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       block
_exptl_crystal_F_000             10998
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   0.819
_exptl_transmission_factor_min   0.766
_refine_diff_density_max         1.441
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1500P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1987
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3118
_reflns_number_total             4307
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b01338_si_002.cif
_cod_data_source_block           1435110
_cod_original_cell_volume        27168(14)
_cod_original_formula_sum        'C89.50 H119 Cl4 N11 O71.50 V20'
_cod_database_code               4348550
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.766
_shelx_estimated_absorpt_t_max   0.819
_platon_squeeze_void_probe_radius 1.20
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'z, x, y'
'y, z, x'
'-z, -x, y'
'-y, z, -x'
'z, -x, -y'
'-y, -z, x'
'-z, x, -y'
'y, -z, -x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-x, -y, -z'
'x, y, -z'
'-x, y, z'
'x, -y, z'
'-z, -x, -y'
'-y, -z, -x'
'z, x, -y'
'y, -z, x'
'-z, x, y'
'y, z, -x'
'z, -x, y'
'-y, z, x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, x+1/2'
'-z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, -x+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, z+1/2, x+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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.60251(16) 0.16365(15) 0.39936(15) 0.0429(11) Uani 1 1 d . . .
C2 C 0.6604(2) 0.1096(2) 0.3988(2) 0.104(3) Uani 1 1 d . . .
H2 H 0.6868 0.0986 0.4107 0.125 Uiso 1 1 calc R U .
C3 C 0.6410(2) 0.1465(2) 0.4169(2) 0.081(2) Uani 1 1 d . . .
H3 H 0.6540 0.1602 0.4414 0.097 Uiso 1 1 calc R U .
C4 C 0.6410(2) 0.08859(19) 0.3628(2) 0.082(2) Uani 1 1 d . . .
H4 H 0.6542 0.0634 0.3506 0.098 Uiso 1 1 calc R U .
C5 C 0.60178(16) 0.10520(15) 0.34492(16) 0.0470(12) Uani 1 1 d . . .
C6 C 0.58265(14) 0.14276(14) 0.36322(14) 0.0374(10) Uani 1 1 d . . .
H6 H 0.5564 0.1541 0.3513 0.045 Uiso 1 1 calc R U .
C7 C 0.58046(14) 0.20350(14) 0.42041(13) 0.0344(10) Uani 1 1 d . . .
C8 C 0.58012(14) 0.08175(13) 0.30643(14) 0.0362(10) Uani 1 1 d . . .
O1 O 0.62579(13) 0.0000 0.21826(14) 0.0425(11) Uani 1 2 d S T P
O2 O 0.54153(9) -0.04141(8) 0.21758(9) 0.0318(7) Uani 1 1 d . . .
O3 O 0.5000 0.0000 0.1433(2) 0.0563(18) Uani 1 4 d S T P
O4 O 0.5000 0.12624(13) 0.21507(14) 0.0425(10) Uani 1 2 d S T P
O5 O 0.54548(9) 0.09949(9) 0.29138(9) 0.0375(7) Uani 1 1 d . . .
O6 O 0.59763(9) 0.04609(9) 0.29364(10) 0.0384(7) Uani 1 1 d . . .
O7 O 0.59841(9) 0.21857(9) 0.45474(9) 0.0381(7) Uani 1 1 d . . .
O8 O 0.62561(14) 0.29460(14) 0.5000 0.0435(11) Uani 1 2 d S T P
O9 O 0.54140(9) 0.29454(9) 0.45840(8) 0.0323(7) Uani 1 1 d . . .
O10 O 0.5000 0.36865(19) 0.5000 0.0506(17) Uani 1 4 d S T P
O11 O 0.5000 0.29243(13) 0.37402(13) 0.0421(10) Uani 1 2 d S T P
O12 O 0.54539(9) 0.21761(9) 0.40252(9) 0.0371(7) Uani 1 1 d . . .
V1 V 0.58174(3) 0.0000 0.24786(3) 0.0291(3) Uani 1 2 d S T P
V2 V 0.5000 0.0000 0.19623(4) 0.0333(4) Uani 1 4 d S T P
V3 V 0.5000 0.08260(3) 0.24566(3) 0.0288(3) Uani 1 2 d S T P
V4 V 0.5000 0.26374(3) 0.41835(3) 0.0294(3) Uani 1 2 d S T P
V5 V 0.58209(3) 0.26482(3) 0.5000 0.0307(3) Uani 1 2 d S T P
V6 V 0.5000 0.31553(5) 0.5000 0.0336(4) Uani 1 4 d S T P
Cl1 Cl 0.5000 0.20895(7) 0.5000 0.0380(5) Uani 1 4 d S T P
Cl2 Cl 0.5000 0.0000 0.30416(7) 0.0412(5) Uani 1 4 d S T P
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'
O O 0.0106 0.0060 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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
C3 C1 C6 119.5(4) . .
C3 C1 C7 120.5(4) . .
C6 C1 C7 119.9(4) . .
C3 C2 C4 120.1(5) . .
C3 C2 H2 120.0 . .
C4 C2 H2 120.0 . .
C2 C3 C1 120.9(5) . .
C2 C3 H3 119.6 . .
C1 C3 H3 119.6 . .
C2 C4 C5 119.8(5) . .
C2 C4 H4 120.1 . .
C5 C4 H4 120.1 . .
C6 C5 C4 119.5(4) . .
C6 C5 C8 120.6(4) . .
C4 C5 C8 119.8(4) . .
C5 C6 C1 120.1(4) . .
C5 C6 H6 119.9 . .
C1 C6 H6 119.9 . .
O7 C7 O12 126.4(4) . .
O7 C7 C1 116.4(4) . .
O12 C7 C1 117.2(4) . .
O5 C8 O6 126.9(4) . .
O5 C8 C5 116.0(4) . .
O6 C8 C5 117.0(4) . .
V2 O2 V3 98.24(12) . 2_655
V2 O2 V1 98.50(12) . .
V3 O2 V1 126.68(14) 2_655 .
C8 O5 V3 134.9(3) . .
C8 O6 V1 134.3(3) . .
C7 O7 V5 134.9(3) . .
V6 O9 V4 98.45(13) . .
V6 O9 V5 98.15(12) . .
V4 O9 V5 124.80(14) . .
C7 O12 V4 134.7(3) . .
O1 V1 O2 104.66(15) . 28
O1 V1 O2 104.66(15) . .
O2 V1 O2 78.89(16) 28 .
O1 V1 O6 100.64(14) . .
O2 V1 O6 91.53(11) 28 .
O2 V1 O6 154.47(12) . .
O1 V1 O6 100.64(14) . 28
O2 V1 O6 154.46(12) 28 28
O2 V1 O6 91.53(11) . 28
O6 V1 O6 87.13(17) . 28
O1 V1 V2 113.83(17) . .
O2 V1 V2 39.68(8) 28 .
O2 V1 V2 39.68(8) . .
O6 V1 V2 124.50(8) . .
O6 V1 V2 124.50(8) 28 .
O3 V2 O2 110.01(9) . 28
O3 V2 O2 110.01(9) . 27_655
O2 V2 O2 139.98(18) 28 27_655
O3 V2 O2 110.01(9) . 2_655
O2 V2 O2 83.42(16) 28 2_655
O2 V2 O2 83.13(16) 27_655 2_655
O3 V2 O2 110.01(9) . .
O2 V2 O2 83.13(16) 28 .
O2 V2 O2 83.42(16) 27_655 .
O2 V2 O2 139.98(18) 2_655 .
O3 V2 V3 120.90(3) . 2_655
O2 V2 V3 113.18(9) 28 2_655
O2 V2 V3 41.84(8) 27_655 2_655
O2 V2 V3 113.18(9) 2_655 2_655
O2 V2 V3 41.84(8) . 2_655
O3 V2 V3 120.90(3) . .
O2 V2 V3 41.84(8) 28 .
O2 V2 V3 113.18(9) 27_655 .
O2 V2 V3 41.84(8) 2_655 .
O2 V2 V3 113.18(9) . .
V3 V2 V3 118.20(6) 2_655 .
O3 V2 V1 122.28(3) . 2_655
O2 V2 V1 112.32(9) 28 2_655
O2 V2 V1 41.82(8) 27_655 2_655
O2 V2 V1 41.82(8) 2_655 2_655
O2 V2 V1 112.32(9) . 2_655
V3 V2 V1 74.08(2) 2_655 2_655
V3 V2 V1 74.08(2) . 2_655
O3 V2 V1 122.28(3) . .
O2 V2 V1 41.82(8) 28 .
O2 V2 V1 112.32(9) 27_655 .
O2 V2 V1 112.32(9) 2_655 .
O2 V2 V1 41.82(8) . .
V3 V2 V1 74.08(2) 2_655 .
V3 V2 V1 74.08(2) . .
V1 V2 V1 115.45(6) 2_655 .
O4 V3 O2 105.75(14) . 2_655
O4 V3 O2 105.75(14) . 28
O2 V3 O2 79.59(16) 2_655 28
O4 V3 O5 100.74(14) . 27_655
O2 V3 O5 91.20(11) 2_655 27_655
O2 V3 O5 153.41(12) 28 27_655
O4 V3 O5 100.74(14) . .
O2 V3 O5 153.42(12) 2_655 .
O2 V3 O5 91.20(11) 28 .
O5 V3 O5 86.04(16) 27_655 .
O4 V3 V2 114.06(16) . .
O2 V3 V2 39.92(8) 2_655 .
O2 V3 V2 39.92(8) 28 .
O5 V3 V2 124.72(8) 27_655 .
O5 V3 V2 124.72(8) . .
O11 V4 O9 104.99(14) . .
O11 V4 O9 104.99(14) . 27_655
O9 V4 O9 78.67(16) . 27_655
O11 V4 O12 100.17(14) . 27_655
O9 V4 O12 154.69(12) . 27_655
O9 V4 O12 92.32(11) 27_655 27_655
O11 V4 O12 100.17(14) . .
O9 V4 O12 92.31(11) . .
O9 V4 O12 154.69(12) 27_655 .
O12 V4 O12 85.87(16) 27_655 .
O11 V4 V6 114.71(16) . .
O9 V4 V6 39.62(8) . .
O9 V4 V6 39.62(8) 27_655 .
O12 V4 V6 124.86(8) 27_655 .
O12 V4 V6 124.86(8) . .
O8 V5 O9 104.90(15) . 26_556
O8 V5 O9 104.90(15) . .
O9 V5 O9 79.09(16) 26_556 .
O8 V5 O7 100.92(15) . .
O9 V5 O7 154.06(13) 26_556 .
O9 V5 O7 92.04(11) . .
O8 V5 O7 100.93(15) . 26_556
O9 V5 O7 92.04(11) 26_556 26_556
O9 V5 O7 154.06(13) . 26_556
O7 V5 O7 85.40(17) . 26_556
O8 V5 V6 113.92(17) . .
O9 V5 V6 39.75(8) 26_556 .
O9 V5 V6 39.75(8) . .
O7 V5 V6 124.91(9) . .
O7 V5 V6 124.90(9) 26_556 .
O10 V6 O9 109.68(9) . 27_655
O10 V6 O9 109.68(9) . 26_556
O9 V6 O9 140.64(17) 27_655 26_556
O10 V6 O9 109.68(9) . 4_656
O9 V6 O9 83.73(16) 27_655 4_656
O9 V6 O9 83.25(16) 26_556 4_656
O10 V6 O9 109.68(9) . .
O9 V6 O9 83.25(16) 27_655 .
O9 V6 O9 83.73(16) 26_556 .
O9 V6 O9 140.64(17) 4_656 .
O10 V6 V5 121.70(3) . .
O9 V6 V5 112.84(9) 27_655 .
O9 V6 V5 42.09(8) 26_556 .
O9 V6 V5 112.84(9) 4_656 .
O9 V6 V5 42.09(8) . .
O10 V6 V5 121.70(3) . 27_655
O9 V6 V5 42.09(8) 27_655 27_655
O9 V6 V5 112.84(9) 26_556 27_655
O9 V6 V5 42.09(8) 4_656 27_655
O9 V6 V5 112.84(9) . 27_655
V5 V6 V5 116.59(6) . 27_655
O10 V6 V4 122.38(3) . .
O9 V6 V4 41.93(8) 27_655 .
O9 V6 V4 112.53(9) 26_556 .
O9 V6 V4 112.53(9) 4_656 .
O9 V6 V4 41.93(8) . .
V5 V6 V4 73.65(2) . .
V5 V6 V4 73.65(2) 27_655 .
O10 V6 V4 122.38(3) . 26_556
O9 V6 V4 112.53(9) 27_655 26_556
O9 V6 V4 41.93(8) 26_556 26_556
O9 V6 V4 41.93(8) 4_656 26_556
O9 V6 V4 112.54(9) . 26_556
V5 V6 V4 73.65(2) . 26_556
V5 V6 V4 73.65(2) 27_655 26_556
V4 V6 V4 115.23(6) . 26_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C3 1.370(6) .
C1 C6 1.390(6) .
C1 C7 1.508(6) .
C2 C3 1.368(7) .
C2 C4 1.382(7) .
C2 H2 0.9300 .
C3 H3 0.9300 .
C4 C5 1.389(6) .
C4 H4 0.9300 .
C5 C6 1.382(6) .
C5 C8 1.503(6) .
C6 H6 0.9300 .
C7 O7 1.250(5) .
C7 O12 1.257(5) .
C8 O5 1.254(5) .
C8 O6 1.255(5) .
O1 V1 1.595(4) .
O2 V2 1.876(3) .
O2 V3 1.951(3) 2_655
O2 V1 1.959(3) .
O3 V2 1.591(6) .
O4 V3 1.602(4) .
O5 V3 2.004(3) .
O6 V1 2.011(3) .
O7 V5 2.006(3) .
O8 V5 1.585(4) .
O9 V6 1.874(3) .
O9 V4 1.964(3) .
O9 V5 1.964(3) .
O10 V6 1.597(6) .
O11 V4 1.588(4) .
O12 V4 2.003(3) .
V1 O2 1.959(3) 28
V1 O6 2.011(3) 28
V1 V2 2.9065(13) .
V2 O2 1.876(3) 28
V2 O2 1.876(3) 27_655
V2 O2 1.876(3) 2_655
V2 V3 2.8940(12) 2_655
V2 V3 2.8940(12) .
V2 V1 2.9065(13) 2_655
V3 O2 1.951(3) 2_655
V3 O2 1.951(3) 28
V3 O5 2.004(3) 27_655
V4 O9 1.964(3) 27_655
V4 O12 2.003(3) 27_655
V4 V6 2.9065(13) .
V5 O9 1.964(3) 26_556
V5 O7 2.006(3) 26_556
V5 V6 2.9006(13) .
V6 O9 1.874(3) 27_655
V6 O9 1.874(3) 26_556
V6 O9 1.874(3) 4_656
V6 V5 2.9006(13) 27_655
V6 V4 2.9065(13) 26_556
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.002 -0.003 -0.002 11743 2651 ' '
2 0.500 0.000 0.000 575 116 ' '
3 0.000 0.000 0.500 575 116 ' '
4 0.500 0.000 0.500 575 116 ' '
5 0.000 0.500 0.000 575 116 ' '
6 0.500 0.500 0.000 575 116 ' '
7 0.000 0.500 0.500 575 116 ' '
