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_1564236
_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_formula_moiety
'C112 H138 Ag3 Au6 Cu3 N6 O15 P6 S6, 3[C2 F3 O2], 12.5[H2O]'
_chemical_formula_sum            'C118 H163 Ag3 Au6 Cu3 F9 N6 O33.5 P6 S6'
_chemical_formula_weight         4446.74
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_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            18
_cell_length_a                   33.804(5)
_cell_length_b                   33.804(5)
_cell_length_c                   81.734(16)
_cell_measurement_reflns_used    235614
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      29.803
_cell_measurement_theta_min      1.257
_cell_volume                     80885(2)
_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      103(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.679
_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     0.62997
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.679
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       110
_diffrn_reflns_limit_l_min       -123
_diffrn_reflns_number            235493
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.679
_diffrn_reflns_theta_full        22.209
_diffrn_reflns_theta_max         29.803
_diffrn_reflns_theta_min         1.257
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    4.016
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       'truncated octahedron'
_exptl_crystal_F_000             38700
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.900
_refine_diff_density_min         -1.747
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         25128
_refine_ls_number_restraints     552
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0566
_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^)+(0.1125P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.1950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13810
_reflns_number_total             25128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc02497c2.cif
_cod_data_source_block           II_sq
_cod_original_cell_volume        80885(28)
_cod_original_formula_sum        'C118 H163 Ag3 Au6 Cu3 F9 N6 O33.50 P6 S6'
_cod_database_code               1564236
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.824
_shelx_estimated_absorpt_t_max   0.824
_shelx_res_checksum              51602
_shelx_hkl_checksum              8866
_shelx_fab_checksum              29527