A square-shaped complex with an electron-acceptor ligand: unique cubic crystal symmetry and similarity to the inorganic mineral katoite
Aoki, Kentaro; Otsubo, Kazuya; Kitagawa, Hiroshi; CrystEngComm 23 (2021) 7691–7697; doi:10.1039/D1CE00994J

data_7243622
_publ_section_title
;
 A square-shaped complex with an electron-acceptor ligand: unique cubic
 crystal symmetry and similarity to the inorganic mineral katoite
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              7691
_journal_page_last               7697
_journal_paper_doi               10.1039/D1CE00994J
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety
'C104 H80 N24 O32 Pt4 S4, 17(C4 H8 O), 68(H2 O)'
_chemical_formula_sum            'C172 H352 N24 O117 Pt4 S4'
_chemical_formula_weight         5537.35
_chemical_properties_physical    Efflorescent
_space_group_crystal_system      cubic
_space_group_IT_number           220
_space_group_name_Hall           'I -4bd 2c 3'
_space_group_name_H-M_alt        'I -4 3 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-09-19
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-09-24 deposited with the CCDC.	2021-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   39.9546(6)
_cell_length_b                   39.9546(6)
_cell_length_c                   39.9546(6)
_cell_measurement_reflns_used    247712
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.489
_cell_measurement_theta_min      3.5329
_cell_volume                     63782.3(17)
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2014)'
_computing_data_collection       'CrysAlisPro (Agilent Technologies, 2014)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku XtaLAB Pro'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.2307
_diffrn_reflns_av_unetI/netI     0.1919
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            239627
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.489
_diffrn_reflns_theta_min         3.533
_exptl_absorpt_coefficient_mu    2.781
_exptl_absorpt_correction_T_max  0.532
_exptl_absorpt_correction_T_min  0.388
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             34368
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 4:1 ratio of water and tetrahydrofuran'
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.260
_refine_diff_density_max         1.264
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 2084 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.026(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         15679
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.2014
_refine_ls_R_factor_gt           0.0664
_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^)+(0.0704P)^2^+269.5207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1466
_refine_ls_wR_factor_ref         0.2012
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.950
_reflns_number_gt                5861
_reflns_number_total             15679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00994j3.cif
_cod_data_source_block           exp_185
_cod_depositor_comments          'Adding full bibliography for 7243622.cif.'
_cod_original_cell_volume        63782(3)
_cod_database_code               7243622
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              27152
_shelx_hkl_checksum              20671
_shelx_fab_checksum              9894