#------------------------------------------------------------------------------
#$Date: 2019-11-23 11:26:54 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233074 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/85/4348549.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_4348549
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            'C50 H72.5 Cl3 N7.5 O53 S6 V15'
_chemical_formula_weight         2689.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_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            4
_cell_length_a                   23.209(5)
_cell_length_b                   33.798(5)
_cell_length_c                   14.531(5)
_cell_measurement_reflns_used    9227
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.73
_cell_measurement_theta_min      1.06
_cell_volume                     11398(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0400
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34658
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.728
_diffrn_reflns_theta_min         1.755
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.429
_exptl_absorpt_correction_T_max  0.741
_exptl_absorpt_correction_T_min  0.717
_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    1.567
_exptl_crystal_description       block
_exptl_crystal_F_000             5364
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0653P)²+18.6213P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1229
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4577
_reflns_number_total             5797
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b01338_si_002.cif
_cod_data_source_block           1435109
_cod_original_formula_sum        'C50 H72.50 Cl3 N7.50 O53 S6 V15'
_cod_database_code               4348549
_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.
;
_platon_squeeze_void_probe_radius 1.20
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, 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'
'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, y, z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'-x+1/2, y+1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.18107(14) 0.24760(10) 0.5609(2) 0.0426(8) Uani 1 1 d . . .
C2 C 0.05260(14) 0.10183(10) 0.5669(2) 0.0425(8) Uani 1 1 d . . .
C3 C 0.12777(14) 0.31017(10) 0.5599(2) 0.0417(8) Uani 1 1 d . . .
C4 C 0.10299(15) 0.34810(10) 0.5888(2) 0.0408(8) Uani 1 1 d . . .
C5 C 0.11382(14) 0.09497(10) 0.5924(2) 0.0397(7) Uani 1 1 d . . .
C6 C 0.21798(14) 0.21422(11) 0.5901(2) 0.0418(8) Uani 1 1 d . . .
C7 C 0.11151(18) 0.28541(11) 0.4898(3) 0.0591(10) Uani 1 1 d . . .
H7 H 0.0833 0.2916 0.4467 0.071 Uiso 1 1 calc R U .
C8 C 0.14197(18) 0.24984(12) 0.4904(3) 0.0593(10) Uani 1 1 d . . .
H8 H 0.1364 0.2298 0.4476 0.071 Uiso 1 1 calc R U .
C9 C 0.03025(15) 0.12760(13) 0.5053(3) 0.0562(10) Uani 1 1 d . . .
H9 H 0.0525 0.1436 0.4672 0.067 Uiso 1 1 calc R U .
O1 O 0.35507(15) 0.20874(12) 0.7500 0.0598(10) Uani 1 2 d S T P
O2 O 0.26540(10) 0.11319(8) 0.48815(17) 0.0549(6) Uani 1 1 d . . .
O3 O 0.16312(18) 0.43303(11) 0.7500 0.0620(10) Uani 1 2 d S T P
O4 O 0.05918(10) 0.36051(7) 0.54751(15) 0.0445(5) Uani 1 1 d . . .
O5 O 0.35143(15) 0.07813(12) 0.7500 0.0642(11) Uani 1 2 d S T P
O6 O 0.21232(10) 0.18218(7) 0.54793(16) 0.0452(6) Uani 1 1 d . . .
O7 O 0.15151(9) 0.11390(8) 0.55030(16) 0.0464(6) Uani 1 1 d . . .
O9 O 0.25020(10) 0.22129(7) 0.65761(16) 0.0480(6) Uani 1 1 d . . .
O10 O 0.18896(17) 0.01440(11) 0.7500 0.0619(10) Uani 1 2 d S T P
O11 O 0.12794(10) 0.36421(7) 0.65718(16) 0.0464(6) Uani 1 1 d . . .
O12 O 0.05336(10) 0.42980(6) 0.66406(15) 0.0441(6) Uani 1 1 d . . .
O13 O 0.0000 0.49540(15) 0.7500 0.0649(15) Uani 1 4 d S T P
O14 O 0.12113(10) 0.07052(7) 0.65710(17) 0.0471(6) Uani 1 1 d . . .
O15 O 0.24176(9) 0.08066(7) 0.66367(15) 0.0434(5) Uani 1 1 d . . .
O16 O 0.29670(9) 0.14379(7) 0.83582(16) 0.0453(6) Uani 1 1 d . . .
O8 O 0.0000 0.42742(10) 0.4887(2) 0.0535(9) Uani 1 2 d S T P
S1 S 0.0000 0.07770(4) 0.62653(9) 0.0458(3) Uani 1 2 d S T P
S2 S 0.18066(4) 0.28957(3) 0.62537(6) 0.0468(2) Uani 1 1 d . . .
V1 V 0.10697(4) 0.40559(2) 0.7500 0.0424(2) Uani 1 2 d S T P
V2 V 0.23512(2) 0.12637(2) 0.58089(4) 0.04053(16) Uani 1 1 d . . .
V3 V 0.29301(3) 0.18840(3) 0.7500 0.0432(2) Uani 1 2 d S T P
V4 V 0.18405(3) 0.06116(2) 0.7500 0.0417(2) Uani 1 2 d S T P
V5 V 0.29278(3) 0.10267(3) 0.7500 0.0454(2) Uani 1 2 d S T P
V6 V 0.0000 0.40223(2) 0.58129(5) 0.0402(2) Uani 1 2 d S T P
V7 V 0.0000 0.44893(3) 0.7500 0.0463(3) Uani 1 4 d S T P
Cl1 Cl 0.0000 0.35245(5) 0.7500 0.0439(4) Uani 1 4 d S T P
Cl2 Cl 0.17193(5) 0.15152(4) 0.7500 0.0450(3) Uani 1 2 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'
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'
Cl Cl 0.1484 0.1585 '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'
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
C8 C1 C6 129.8(3) . .
C8 C1 S2 111.2(3) . .
C6 C1 S2 118.8(3) . .
C9 C2 C5 129.2(3) . .
C9 C2 S1 111.7(3) . .
C5 C2 S1 118.9(3) . .
C7 C3 C4 129.7(3) . .
C7 C3 S2 111.4(3) . .
C4 C3 S2 118.7(2) . .
O4 C4 O11 126.9(3) . .
O4 C4 C3 118.3(3) . .
O11 C4 C3 114.8(3) . .
O7 C5 O14 127.4(3) . .
O7 C5 C2 118.0(3) . .
O14 C5 C2 114.6(3) . .
O6 C6 O9 127.6(3) . .
O6 C6 C1 117.3(3) . .
O9 C6 C1 115.1(3) . .
C3 C7 C8 112.4(3) . .
C1 C8 C7 112.8(3) . .
C2 C9 C9 112.6(2) . 11
C4 O4 V6 131.8(2) . .
C6 O6 V2 131.7(2) . .
C5 O7 V2 132.0(2) . .
C6 O9 V3 135.4(2) . .
C4 O11 V1 135.6(2) . .
V7 O12 V1 98.06(10) . .
V7 O12 V6 98.93(11) . .
V1 O12 V6 126.74(12) . .
C5 O14 V4 134.4(2) . .
V5 O15 V4 97.89(10) . .
V5 O15 V2 98.46(11) . .
V4 O15 V2 127.31(11) . .
V5 O16 V3 98.37(11) . .
V5 O16 V2 98.78(11) . 10_557
V3 O16 V2 126.28(11) . 10_557
C2 S1 C2 91.5(2) 11 .
C3 S2 C1 92.14(17) . .
O3 V1 O12 106.12(14) . .
O3 V1 O12 106.12(14) . 10_557
O12 V1 O12 79.97(14) . 10_557
O3 V1 O11 101.93(14) . 10_557
O12 V1 O11 151.91(10) . 10_557
O12 V1 O11 90.96(10) 10_557 10_557
O3 V1 O11 101.93(14) . .
O12 V1 O11 90.96(10) . .
O12 V1 O11 151.91(10) 10_557 .
O11 V1 O11 84.66(14) 10_557 .
O3 V1 V7 114.03(16) . .
O12 V1 V7 40.07(7) . .
O12 V1 V7 40.07(7) 10_557 .
O11 V1 V7 124.34(7) 10_557 .
O11 V1 V7 124.34(7) . .
O2 V2 O16 106.61(12) . 10_557
O2 V2 O15 105.37(12) . .
O16 V2 O15 78.53(10) 10_557 .
O2 V2 O6 100.22(12) . .
O16 V2 O6 93.26(10) 10_557 .
O15 V2 O6 154.38(10) . .
O2 V2 O7 100.31(12) . .
O16 V2 O7 153.00(10) 10_557 .
O15 V2 O7 92.62(10) . .
O6 V2 O7 83.78(10) . .
O2 V2 V5 115.91(10) . .
O16 V2 V5 39.41(7) 10_557 .
O15 V2 V5 39.67(7) . .
O6 V2 V5 125.35(7) . .
O7 V2 V5 124.46(7) . .
O1 V3 O16 106.99(13) . .
O1 V3 O16 106.99(13) . 10_557
O16 V3 O16 79.10(14) . 10_557
O1 V3 O9 102.02(13) . .
O16 V3 O9 150.96(10) . .
O16 V3 O9 91.27(10) 10_557 .
O1 V3 O9 102.02(13) . 10_557
O16 V3 O9 91.27(10) . 10_557
O16 V3 O9 150.96(10) 10_557 10_557
O9 V3 O9 84.00(14) . 10_557
O1 V3 V5 115.63(15) . .
O16 V3 V5 39.67(7) . .
O16 V3 V5 39.67(7) 10_557 .
O9 V3 V5 123.58(8) . .
O9 V3 V5 123.58(8) 10_557 .
O10 V4 O15 106.73(13) . 10_557
O10 V4 O15 106.72(13) . .
O15 V4 O15 80.08(14) 10_557 .
O10 V4 O14 102.06(13) . .
O15 V4 O14 151.19(11) 10_557 .
O15 V4 O14 90.78(10) . .
O10 V4 O14 102.06(13) . 10_557
O15 V4 O14 90.78(10) 10_557 10_557
O15 V4 O14 151.20(11) . 10_557
O14 V4 O14 84.20(14) . 10_557
O10 V4 V5 114.95(15) . .
O15 V4 V5 40.12(7) 10_557 .
O15 V4 V5 40.13(7) . .
O14 V4 V5 123.88(8) . .
O14 V4 V5 123.88(8) 10_557 .
O5 V5 O16 110.19(13) . 10_557
O5 V5 O16 110.20(13) . .
O16 V5 O16 83.67(15) 10_557 .
O5 V5 O15 109.41(13) . 10_557
O16 V5 O15 140.40(10) 10_557 10_557
O16 V5 O15 83.09(10) . 10_557
O5 V5 O15 109.41(13) . .
O16 V5 O15 83.09(10) 10_557 .
O16 V5 O15 140.40(10) . .
O15 V5 O15 83.79(14) 10_557 .
O5 V5 V4 119.57(16) . .
O16 V5 V4 113.82(7) 10_557 .
O16 V5 V4 113.82(7) . .
O15 V5 V4 41.99(7) 10_557 .
O15 V5 V4 41.99(7) . .
O5 V5 V3 121.25(16) . .
O16 V5 V3 41.97(8) 10_557 .
O16 V5 V3 41.96(8) . .
O15 V5 V3 113.39(8) 10_557 .
O15 V5 V3 113.40(8) . .
V4 V5 V3 119.18(3) . .
O5 V5 V2 122.399(19) . 10_557
O16 V5 V2 112.40(8) 10_557 10_557
O16 V5 V2 41.81(7) . 10_557
O15 V5 V2 41.87(7) 10_557 10_557
O15 V5 V2 112.52(7) . 10_557
V4 V5 V2 74.45(2) . 10_557
V3 V5 V2 74.08(2) . 10_557
O5 V5 V2 122.400(19) . .
O16 V5 V2 41.81(7) 10_557 .
O16 V5 V2 112.39(8) . .
O15 V5 V2 112.52(7) 10_557 .
O15 V5 V2 41.87(7) . .
V4 V5 V2 74.45(2) . .
V3 V5 V2 74.08(2) . .
V2 V5 V2 115.20(4) 10_557 .
O8 V6 O12 105.30(12) . 11
O8 V6 O12 105.30(12) . .
O12 V6 O12 78.29(14) 11 .
O8 V6 O4 99.64(11) . .
O12 V6 O4 154.94(10) 11 .
O12 V6 O4 92.93(10) . .
O8 V6 O4 99.64(11) . 11
O12 V6 O4 92.93(10) 11 11
O12 V6 O4 154.94(10) . 11
O4 V6 O4 85.22(14) . 11
O8 V6 V7 114.88(13) . .
O12 V6 V7 39.41(7) 11 .
O12 V6 V7 39.41(7) . .
O4 V6 V7 125.43(7) . .
O4 V6 V7 125.43(7) 11 .
O13 V7 O12 110.18(7) . .
O13 V7 O12 110.19(7) . 11
O12 V7 O12 82.74(14) . 11
O13 V7 O12 110.19(7) . 10_557
O12 V7 O12 83.58(14) . 10_557
O12 V7 O12 139.63(14) 11 10_557
O13 V7 O12 110.19(7) . 4_556
O12 V7 O12 139.63(14) . 4_556
O12 V7 O12 83.58(14) 11 4_556
O12 V7 O12 82.74(14) 10_557 4_556
O13 V7 V1 120.54(3) . 11
O12 V7 V1 113.20(8) . 11
O12 V7 V1 41.88(7) 11 11
O12 V7 V1 113.20(8) 10_557 11
O12 V7 V1 41.88(7) 4_556 11
O13 V7 V1 120.54(3) . .
O12 V7 V1 41.88(7) . .
O12 V7 V1 113.20(8) 11 .
O12 V7 V1 41.88(7) 10_557 .
O12 V7 V1 113.20(8) 4_556 .
V1 V7 V1 118.92(5) 11 .
O13 V7 V6 122.77(3) . .
O12 V7 V6 41.66(7) . .
O12 V7 V6 41.66(7) 11 .
O12 V7 V6 111.93(8) 10_557 .
O12 V7 V6 111.93(8) 4_556 .
V1 V7 V6 74.03(2) 11 .
V1 V7 V6 74.03(2) . .
O13 V7 V6 122.78(3) . 10_557
O12 V7 V6 111.93(8) . 10_557
O12 V7 V6 111.93(8) 11 10_557
O12 V7 V6 41.66(7) 10_557 10_557
O12 V7 V6 41.66(7) 4_556 10_557
V1 V7 V6 74.03(2) 11 10_557
V1 V7 V6 74.03(2) . 10_557
V6 V7 V6 114.45(5) . 10_557
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C8 1.371(5) .
C1 C6 1.479(5) .
C1 S2 1.699(4) .
C2 C9 1.352(5) .
C2 C5 1.487(4) .
C2 S1 1.705(3) .
C3 C7 1.371(5) .
C3 C4 1.467(5) .
C3 S2 1.702(3) .
C4 O4 1.253(4) .
C4 O11 1.272(4) .
C5 O7 1.245(4) .
C5 O14 1.263(4) .
C6 O6 1.251(4) .
C6 O9 1.256(4) .
C7 C8 1.395(5) .
C9 C9 1.404(7) 11
O1 V3 1.596(4) .
O2 V2 1.584(2) .
O3 V1 1.599(4) .
O4 V6 2.029(2) .
O5 V5 1.594(3) .
O6 V2 2.017(2) .
O7 V2 2.035(2) .
O9 V3 2.006(2) .
O10 V4 1.584(4) .
O11 V1 2.003(2) .
O12 V7 1.874(2) .
O12 V1 1.943(2) .
O12 V6 1.962(2) .
O13 V7 1.571(5) .
O14 V4 2.014(2) .
O15 V5 1.879(2) .
O15 V4 1.950(2) .
O15 V2 1.964(2) .
O16 V5 1.870(3) .
O16 V3 1.958(3) .
O16 V2 1.963(2) 10_557
O8 V6 1.592(3) .
S1 C2 1.705(3) 11
V1 O12 1.943(2) 10_557
V1 O11 2.003(2) 10_557
V1 V7 2.8825(12) .
V2 O16 1.963(2) 10_557
V2 V5 2.9105(10) .
V3 O16 1.958(3) 10_557
V3 O9 2.006(2) 10_557
V3 V5 2.8975(13) .
V4 O15 1.950(2) 10_557
V4 O14 2.014(2) 10_557
V4 V5 2.8873(13) .
V5 O16 1.870(3) 10_557
V5 O15 1.878(2) 10_557
V5 V2 2.9104(10) 10_557
V6 O12 1.962(2) 11
V6 O4 2.029(2) 11
V6 V7 2.9158(12) .
V7 O12 1.874(2) 11
V7 O12 1.874(2) 10_557
V7 O12 1.874(2) 4_556
V7 V1 2.8824(12) 11
V7 V6 2.9158(12) 10_557
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 0.000 0.000 -0.019 2708 725 ' '
2 0.500 0.500 -0.143 2681 723 ' '
