Anisotropic Polyoxometalate Cages Assembled via Layers of Heteroanion Templates.
Zheng, Qi; Kupper, Manuel; Xuan, Weimin; Oki, Hirofumi; Tsunashima, Ryo; Long, De-Liang; Cronin, Leroy; Journal of the American Chemical Society 141 (2019) 13479–13486; doi:10.1021/jacs.9b04533

data_4128894
_publ_section_title
;
 Anisotropic Polyoxometalate Cages Assembled via Layers of Heteroanion
 Templates.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13479
_journal_page_last               13486
_journal_paper_doi               10.1021/jacs.9b04533
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C22 H119 Mo3 N11 Na O96 Se2 W21'
_chemical_formula_weight         6403.85
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.577(2)
_cell_length_b                   21.446(2)
_cell_length_c                   25.391(3)
_cell_measurement_reflns_used    9768
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2.49
_cell_volume                     11205(2)
_computing_cell_refinement       Apex3
_computing_data_collection       Apex3
_computing_data_reduction        Apex3
_computing_molecular_graphics    Diamond3
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II Quasar'
_diffrn_measurement_method       '\w & \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            168417
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.243
_diffrn_source                   '1uS Microfocus x-ray'
_exptl_absorpt_coefficient_mu    22.548
_exptl_absorpt_correction_T_max  0.062
_exptl_absorpt_correction_T_min  0.012
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.796
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             11420
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         3.37
_refine_diff_density_min         -3.25
_refine_diff_density_rms         0.45
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.258
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         11330
_refine_ls_number_restraints     530
_refine_ls_restrained_S_all      1.242
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0754
_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^)+(0.0567P)^2^+1056.3872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1888
_refine_ls_wR_factor_ref         0.2179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9083
_reflns_number_total             11330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04533_si_006.cif
_cod_data_source_block           qz635e_2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'direct methods' was
changed to 'direct'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        11204.7(19)
_cod_database_code               4128894
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.211
_shelx_estimated_absorpt_t_max   0.399
_shelx_res_checksum              46453
_shelx_hkl_checksum              67210