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_1564233
_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 N6 O12 P6 S6, 1.5(N O3), 1.5[NO3], 17[H2O]'
_chemical_formula_sum            'C112 H172 Ag3 Au6 N9 O38 P6 S6'
_chemical_formula_weight         4136.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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                90
_cell_formula_units_Z            8
_cell_length_a                   30.1406(4)
_cell_length_b                   32.9119(5)
_cell_length_c                   33.4887(7)
_cell_measurement_reflns_used    347480
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.479
_cell_measurement_theta_min      1.027
_cell_volume                     33220.3(10)
_computing_cell_refinement       HKL3000
_computing_data_collection
'<i>PAL BL2D-SMDC Program</i>(Shin et.al, 2016)'
_computing_data_reduction        HKL3000
_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_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.600
_diffrn_reflns_av_R_equivalents  0.1548
_diffrn_reflns_av_unetI/netI     0.0831
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            347480
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        19.479
_diffrn_reflns_theta_max         19.479
_diffrn_reflns_theta_min         1.027
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    3.585
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_description       stick
_exptl_crystal_F_000             16096
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.113
_refine_diff_density_min         -1.318
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
;
 Flack x determined using 12142 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2755
_refine_ls_number_reflns         47764
_refine_ls_number_restraints     7503
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0505P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0977
_reflns_Friedel_coverage         0.883
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                32767
_reflns_number_total             47764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc02497c2.cif
_cod_data_source_block           '[au6ag3](no3)3_sq'
_cod_database_code               1564233
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.787
_shelx_estimated_absorpt_t_max   0.965
_shelx_res_checksum              23273
_shelx_hkl_checksum              48211
_shelx_fab_checksum              21733