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_4131877
_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            'C26 H168 N13 Na19 O254 P4 Te4 W64'
_chemical_formula_weight         17565.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 103.518(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.2204(6)
_cell_length_b                   37.8175(16)
_cell_length_c                   29.2768(13)
_cell_measurement_reflns_used    9730
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      2.34
_cell_volume                     16384.8(12)
_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 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Apex II Quazar CCD'
_diffrn_measurement_method       '\w & \p scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            232609
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.773
_diffrn_reflns_theta_min         1.431
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    22.848
_exptl_absorpt_correction_T_max  0.0921
_exptl_absorpt_correction_T_min  0.0495
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.560
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             15320
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_refine_diff_density_max         3.06
_refine_diff_density_min         -3.34
_refine_diff_density_rms         0.51
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1628
_refine_ls_number_reflns         31748
_refine_ls_number_restraints     998
_refine_ls_restrained_S_all      1.237
_refine_ls_R_factor_all          0.1198
_refine_ls_R_factor_gt           0.0979
_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^)+(0.0038P)^2^+3093.9070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2011
_refine_ls_wR_factor_ref         0.2140
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25631
_reflns_number_total             31748
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b11982_si_003.cif
_cod_data_source_block           qz432e
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4131877
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.208
_shelx_estimated_absorpt_t_max   0.547
_shelx_res_checksum              28142
_shelx_hkl_checksum              9038