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_1564234
_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, 3(C2 F3 O2), 8[H2O]'
_chemical_formula_sum            'C118 H154 Ag3 Au6 Cu3 F9 N6 O29 P6 S6'
_chemical_formula_weight         4365.67
_space_group_crystal_system      trigonal
_space_group_IT_number           150
_space_group_name_Hall           'P 3 2"'
_space_group_name_H-M_alt        'P 3 2 1'
_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            2
_cell_length_a                   19.2375(4)
_cell_length_b                   19.2375(4)
_cell_length_c                   27.0608(6)
_cell_measurement_reflns_used    30161
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.9510
_cell_measurement_theta_min      1.5400
_cell_volume                     8673.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Mercury 4.2.0 (Macrae et al. 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.819
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.819
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            44681
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.782
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.146
_diffrn_reflns_theta_min         1.939
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.937
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.75a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             4210
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.115
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Flack x determined using 5214 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         13385
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0240
_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^)+(0.0443P)^2^+0.0127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0644
_reflns_Friedel_coverage         0.764
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.738
_reflns_number_gt                12574
_reflns_number_total             13385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc02497c2.cif
_cod_data_source_block           i'_sq
_cod_original_cell_volume        8673.0(4)
_cod_database_code               1564234
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.383
_shelx_estimated_absorpt_t_max   0.842
_oxdiff_exptl_absorpt_empirical_full_min 0.499
_oxdiff_exptl_absorpt_empirical_full_max 1.906
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              76653
_shelx_hkl_checksum              38521
_shelx_fab_checksum              80135