Self-Sorting of Heteroanions in the Assembly of Cross-Shaped Polyoxometalate Clusters.
Zheng, Qi; Vilà-Nadal, Laia; Lang, Zhongling; Chen, Jia-Jia; Long, De-Liang; Mathieson, Jennifer S.; Poblet, Josep M.; Cronin, Leroy; Journal of the American Chemical Society 140 (2018) 2595–2601; doi:10.1021/jacs.7b11982

data_4131879
_publ_section_title
;
 Self-Sorting of Heteroanions in the Assembly of Cross-Shaped
 Polyoxometalate Clusters.
;
_journal_issue                   7
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2595
_journal_page_last               2601
_journal_paper_doi               10.1021/jacs.7b11982
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C38 H276 As4 N19 Na17 O284 P4 W64'
_chemical_formula_weight         18125.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.453(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   57.258(3)
_cell_length_b                   15.0627(8)
_cell_length_c                   77.278(4)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.36
_cell_volume                     66628(6)
_computing_cell_refinement       Apex2
_computing_data_collection       Apex2
_computing_data_reduction        Apex2
_computing_molecular_graphics    Diamond3
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2008 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Apex II Quazar CCD'
_diffrn_measurement_method       '\w & \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1233
_diffrn_reflns_av_unetI/netI     0.1087
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
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_diffrn_reflns_limit_l_min       -77
_diffrn_reflns_number            238128
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        20.866
_diffrn_reflns_theta_max         20.866
_diffrn_reflns_theta_min         1.421
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    22.538
_exptl_absorpt_correction_T_max  0.0853
_exptl_absorpt_correction_T_min  0.0453
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.614
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             64192
_exptl_crystal_size_max          0.090
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_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.07
_refine_diff_density_min         -1.50
_refine_diff_density_rms         0.37
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3206
_refine_ls_number_reflns         34898
_refine_ls_number_restraints     1756
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1195
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+10954.5957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1804
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22222
_reflns_number_total             34898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b11982_si_002.cif
_cod_data_source_block           qz4381a2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4131879
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.236
_shelx_estimated_absorpt_t_max   0.399
_shelx_res_checksum              84658
_shelx_hkl_checksum              74975