Unprecedented superstructure in the type I family of clathrates
Yox, Philip; Lebedev, Oleg I.; Donadio, Davide; Kovnir, Kirill; Chemical Communications  (2021) –; doi:10.1039/D1CC05167A

data_7129268
_publ_section_title
;
 Unprecedented superstructure in the type I family of clathrates
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05167A
_journal_year                    2021
_chemical_formula_moiety         'As30 Au16 Ba8'
_chemical_formula_sum            'As30 Au16 Ba8'
_chemical_formula_weight         6497.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-09-13 deposited with the CCDC.	2021-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.502(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.1473(14)
_cell_length_b                   15.2189(14)
_cell_length_c                   10.9542(10)
_cell_measurement_reflns_used    59395
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.0
_cell_measurement_theta_min      1.90
_cell_volume                     2525.1(4)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX II CCD area-detector'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            59395
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_min         1.897
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    71.902
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'metallic silver'
_exptl_crystal_density_diffrn    8.546
_exptl_crystal_description       block
_exptl_crystal_F_000             5404.0
_exptl_crystal_recrystallization_method 'Flux growth: CsBr/CsI'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.182
_refine_diff_density_min         -2.361
_refine_diff_density_rms         0.517
_refine_ls_extinction_coef       0.000063(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         6719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0094P)^2^+27.8222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5386
_reflns_number_total             6719
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05167a2.cif
_cod_data_source_block           p21c_a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7129268
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              27679
_shelx_hkl_checksum              39456