Composite Hybrid Cluster Built from the Integration of Polyoxometalate and a Metal Halide Cluster: Synthetic Strategy, Structure, and Properties.
Li, Xin-Xiong; Ma, Xiang; Zheng, Wen-Xu; Qi, Yan-Jie; Zheng, Shou-Tian; Yang, Guo-Yu; Inorganic chemistry 55 (2016) 8257–8259; doi:10.1021/acs.inorgchem.6b01453

data_4348635
_publ_section_title
;
 Composite Hybrid Cluster Built from the Integration of Polyoxometalate
 and a Metal Halide Cluster: Synthetic Strategy, Structure, and
 Properties.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8257
_journal_page_last               8259
_journal_paper_doi               10.1021/acs.inorgchem.6b01453
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C73 H159 Br Cr Mo6 N5 O25'
_chemical_formula_weight         2214.60
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.3390(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.2547(15)
_cell_length_b                   26.168(2)
_cell_length_c                   22.5135(19)
_cell_measurement_reflns_used    512
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      49.768
_cell_measurement_theta_min      6.373
_cell_volume                     9559.9(14)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker XSCANS'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX II diffractometer'
_diffrn_measurement_method       none
_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  0.0187
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32299
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.48
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.357
_exptl_absorpt_correction_T_max  0.7923
_exptl_absorpt_correction_T_min  0.7278
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4572
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.467
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     995
_refine_ls_number_reflns         16368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0874P)^2^+33.9927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1524
_reflns_number_gt                13671
_reflns_number_total             16368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01453_si_003.cif
_cod_data_source_block           1
_cod_original_cell_volume        9559.8(15)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4348635