Ligand-Directed Assembly of Polyoxovanadate-Based Metal-Organic Polyhedra.
Zhang, Yuteng; Wang, Xinlong; Li, Shuangbao; Song, Baiqiao; Shao, Kuizhan; Su, Zhongmin; Inorganic chemistry 55 (2016) 8770–8775; doi:10.1021/acs.inorgchem.6b01338

data_4348549
_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       \w-2\q
_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/[\s^2^(Fo^2^)+(0.0653P)^2^+18.6213P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              28116
_shelx_hkl_checksum              44357
_shelx_fab_checksum              38568