A mesoporous ionic solid with 272 AuI6AgI3CuII3 complex cations in a super huge crystal lattice
Takeda, Hiroto; Kojima, Tatsuhiro; Yoshinari, Nobuto; Konno, Takumi; Chemical Science  (2021) –; doi:10.1039/D1SC02497C

data_1564235
_publ_section_title
;
 A mesoporous ionic solid with 272 AuI6AgI3CuII3 complex cations in a
 super huge crystal lattice
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC02497C
_journal_year                    2021
_chemical_absolute_configuration rmad
_chemical_formula_moiety
'C112 H138 Ag3 Au6 Cu3 N6 O15 P6 S6, 1(C2 F3 O2), 2[C2 F3 O2], 15[H2O]'
_chemical_formula_sum            'C118 H168 Ag3 Au6 Cu3 F9 N6 O36 P6 S6'
_chemical_formula_weight         4491.78
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-06-27 deposited with the CCDC.	2021-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   19.2549(7)
_cell_length_b                   19.2549(7)
_cell_length_c                   74.3872(14)
_cell_measurement_reflns_used    56228
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.137
_cell_measurement_theta_min      0.495
_cell_volume                     23884.2(13)
_computing_cell_refinement       'RAPID-AUTO (Rigaku Corporation)'
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation)'
_computing_data_reduction        'RAPID-AUTO (Rigaku Corporation)'
_computing_molecular_graphics    Mercury
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'RIGAKU 1/4chi goniometer with PILATUS3 X CdTe 1M'
_diffrn_measurement_method       'w scan'
_diffrn_radiation_monochromator  Si(311)
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4281
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       96
_diffrn_reflns_limit_l_min       -85
_diffrn_reflns_number            56228
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        14.884
_diffrn_reflns_theta_max         16.137
_diffrn_reflns_theta_min         0.495
_diffrn_source                   'SPring-8 BL02B1 bending magnet'
_exptl_absorpt_coefficient_mu    2.126
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_description       'rhomboidal plate'
_exptl_crystal_F_000             13050
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.874
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 5145 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         11785
_refine_ls_number_restraints     194
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+64.4083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0695
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.940
_reflns_number_gt                11274
_reflns_number_total             11785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc02497c2.cif
_cod_data_source_block           II'_sq
_cod_original_cell_volume        23884.2(18)
_cod_database_code               1564235
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.785
_shelx_estimated_absorpt_t_max   0.848
_shelx_res_checksum              79252
_shelx_hkl_checksum              44623
_shelx_fab_checksum              5707