A polyoxometalate-based metal‒organic polyhedron constructed from a {V5O9Cl} building unit with rhombicuboctahedral geometry
Gong, Ya-Ru; Su, Zhong-Min; Wang, Xin-Long; Acta Crystallographica Section C Structural Chemistry 74 (2018) –; doi:10.1107/S2053229618010689

data_2021251
_publ_section_title
;
 A polyoxometalate-based metal--organic polyhedron constructed from a
 {V5O9Cl} building unit with rhombicuboctahedral geometry
;
_journal_coeditor_code           JR3007
_journal_issue                   11
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_paper_doi               10.1107/S2053229618010689
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '(C2 H8 N)12 [(V5 O9 Cl)6 (C9 H3 O6)8]'
_chemical_formula_moiety         '12(C2 H8 N1 +), C72 H24 Cl6 O102 V30 12-'
_chemical_formula_sum            'C96 H120 Cl6 N12 O102 V30'
_chemical_formula_weight         4814.93
_chemical_name_systematic
;Dodecakis(dimethylammonium)
octakis(\m-benzene-1,3,5-tricarboxylato)hexa-\m-chlorido-tetracosa-\m-oxido-triacontaoxidotriacontavanadium
;
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.7184(17)
_cell_length_b                   29.7184(17)
_cell_length_c                   29.7184(17)
_cell_measurement_reflns_used    19592
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.031
_cell_measurement_theta_min      3.065
_cell_volume                     26247(3)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
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_computing_publication_material
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OLEX2 (Dolomanov <i>et al.</i>,  2009)
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_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
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_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      296.11
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEXII Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            19592
_diffrn_reflns_theta_full        25.031
_diffrn_reflns_theta_max         25.031
_diffrn_reflns_theta_min         3.065
_exptl_absorpt_coefficient_mu    1.140
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       block
_exptl_crystal_F_000             9552
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
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;
TITL q_a.res in Fm-3m
CELL   29.7184   29.7184   29.7184     90.00     90.00     90.00
SPGR Fm-3m
C101 0.397 0.103 0.103 !       6.70 eA-3
C102 0.127 0.432 0.127 !       2.89 eA-3
C103 0.610 0.109 0.055 !       2.00 eA-3
C104 0.047 0.250 0.250 !       1.62 eA-3
C105 0.750 0.249 0.070 !       1.50 eA-3
C106 0.430 0.430 0.430 !       1.39 eA-3
C107 0.580 0.080 0.080 !       1.36 eA-3
C108 0.409 0.497 0.094 !       1.09 eA-3
C109 0.500 0.429 0.087 !       1.08 eA-3
C110 1.000 0.500 0.000 !       0.86 eA-3
C111 0.919 0.033 0.058 !       0.79 eA-3
C112 0.237 0.263 0.263 !       0.77 eA-3
C113 0.763 0.237 0.237 !       0.77 eA-3
C114 0.237 0.232 0.768 !       0.77 eA-3
C115 0.985 0.279 0.279 !       0.73 eA-3
C116 0.907 0.296 0.244 !       0.72 eA-3
C117 0.593 0.204 0.756 !       0.72 eA-3
C118 0.741 0.798 0.908 !       0.72 eA-3
C119 0.593 0.798 0.760 !       0.72 eA-3
C120 0.500 0.500 0.102 !       0.72 eA-3
C121 0.500 0.484 0.004 !       0.66 eA-3
C122 0.922 0.292 0.236 !       0.62 eA-3
C123 0.578 0.208 0.764 !       0.62 eA-3
C124 0.737 0.789 0.923 !       0.62 eA-3
C125 0.158 0.155 0.251 !       0.61 eA-3
C126 0.671 0.125 0.115 !       0.60 eA-3
C127 0.952 0.227 0.227 !       0.59 eA-3
C128 0.946 0.212 0.255 !       0.59 eA-3
C129 0.784 0.292 0.208 !       0.59 eA-3
C130 0.500 0.087 0.471 !       0.57 eA-3
C131 1.000 0.087 0.971 !       0.57 eA-3
C132 0.530 0.414 0.998 !       0.57 eA-3
C133 0.718 0.216 0.929 !       0.57 eA-3
Q134 0.047 0.414 0.046 !       0.57 eA-3
Q135 0.500 0.250-0.001 !       0.54 eA-3
C136 0.268 0.276 0.261 !       0.53 eA-3
Q137 1.000 0.141-0.004 !       0.53 eA-3
C138 0.219 0.331 0.317 !       0.53 eA-3
C139 0.306 0.303 0.197 !       0.51 eA-3
;
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.302
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         1201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0275
_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/[\s^2^(Fo^2^)+(0.0418P)^2^+74.8854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0798
_reflns_number_gt                1046
_reflns_number_total             1201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jr3007sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        26247(5)
_cod_database_code               2021251
_shelx_hkl_checksum              11182
_shelx_res_checksum              29977
_shelx_fab_checksum              12325
_cod_database_fobs_code 2021251