Sandwich-Type Polyoxotungstate Consisting of Two Different Trilacunary Keggin-Type Units.
Han, Zhan-Gang; Zhang, Hui-Xia; Zhang, De-Shun; Liu, Chun-Na; Zheng, Ran; Xia, Gui-Bin; Wang, Xiao-Xiao; Inorganic chemistry 55 (2016) 12488–12491; doi:10.1021/acs.inorgchem.6b01848

data_4348965
_publ_section_title
;
 Sandwich-Type Polyoxotungstate Consisting of Two Different Trilacunary
 Keggin-Type Units.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12488
_journal_page_last               12491
_journal_paper_doi               10.1021/acs.inorgchem.6b01848
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C16 H126 Ag8 Mn8 N16 Na O159 Sb2 W32'
_chemical_formula_weight         10539.49
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                110.022(2)
_cell_angle_beta                 91.256(2)
_cell_angle_gamma                91.279(2)
_cell_formula_units_Z            1
_cell_length_a                   14.683(2)
_cell_length_b                   17.033(2)
_cell_length_c                   17.605(3)
_cell_measurement_reflns_used    4520
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.55
_cell_measurement_theta_min      2.35
_cell_volume                     4133.7(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0970
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20107
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.826
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    24.107
_exptl_absorpt_correction_T_max  0.027
_exptl_absorpt_correction_T_min  0.010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.234
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4663
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         6.395
_refine_diff_density_min         -3.897
_refine_diff_density_rms         0.607
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1108
_refine_ls_number_reflns         14395
_refine_ls_number_restraints     2128
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1186P)^2^+159.2540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1807
_refine_ls_wR_factor_ref         0.2169
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9757
_reflns_number_total             14395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01848_si_002.cif
_cod_data_source_block           zds_023_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'none' was changed to
'?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4348965
_shelxl_version_number           2014-3
_shelx_res_checksum              99906
_shelx_hkl_checksum              8905