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_4131878
_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            'C30 H188 N15 Na17 O254 P8 W64'
_chemical_formula_weight         17228.93
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   34.7924(17)
_cell_length_b                   34.7924(17)
_cell_length_c                   14.1405(9)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.9
_cell_measurement_theta_min      2.48
_cell_volume                     17117.2(16)
_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 0.998
_diffrn_measured_fraction_theta_max 0.991
_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  0.0997
_diffrn_reflns_av_unetI/netI     0.1168
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            71845
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.834
_diffrn_reflns_theta_min         2.194
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    21.553
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.576
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.343
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             15096
_exptl_crystal_size_max          0.100
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_exptl_crystal_size_min          0.040
_refine_diff_density_max         3.15
_refine_diff_density_min         -2.54
_refine_diff_density_rms         0.47
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         16379
_refine_ls_number_restraints     438
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.1571
_refine_ls_R_factor_gt           0.0855
_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^)+(0.0555P)^2^+1897.4790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1810
_refine_ls_wR_factor_ref         0.2189
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9668
_reflns_number_total             16379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b11982_si_004.cif
_cod_data_source_block           qz1036a2
_cod_original_cell_volume        17117(2)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4131878
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.222
_shelx_estimated_absorpt_t_max   0.479
_shelx_res_checksum              17048
_shelx_hkl_checksum              14743