Lone-Pair-Induced Structural Ordering in the Mixed-Valent 0D Metal-Halides Rb23BiIIIxSbIII7‒xSbV2Cl54 (0 ≤ x ≤ 7)
Benin, Bogdan M.; McCall, Kyle M.; Wörle, Michael; Borgeaud, Dominique; Vonderach, Thomas; Sakhatskyi, Kostiantyn; Yakunin, Sergii; Günther, Detlef; Kovalenko, Maksym V.; Chemistry of Materials  (2021) –; doi:10.1021/acs.chemmater.0c04491

data_4003892
_publ_section_title
;
 Lone-Pair-Induced Structural Ordering in the Mixed-Valent 0D
 Metal-Halides Rb23BiIIIxSbIII7--xSbV2Cl54 (0 &#x2264; x &#x2264; 7)
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c04491
_journal_year                    2021
_chemical_formula_moiety         '0.25(Cl216 Rb92 Sb36)'
_chemical_formula_sum            'Cl54 Rb23 Sb9'
_chemical_formula_weight         4975.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_audit_creation_date             2020-08-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.3435(7)
_cell_length_b                   12.9057(4)
_cell_length_c                   37.0625(13)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.596
_cell_measurement_theta_min      3.163
_cell_volume                     10687.3(6)
_computing_data_collection       'SMART v5.630 (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0971
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            56777
_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         27.102
_diffrn_reflns_theta_min         1.648
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.016
_exptl_absorpt_correction_T_max  0.5881
_exptl_absorpt_correction_T_min  0.3861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1352 before and 0.0845 after correction.
The Ratio of minimum to maximum transmission is 0.6565.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.093
_exptl_crystal_description       plate
_exptl_crystal_F_000             8912
_exptl_crystal_recrystallization_method
'Solvothermal reaction in HCl at 160 degrees C'
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         5.088
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.673
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         6429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.1521
_refine_ls_R_factor_gt           0.1322
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1570P)^2^+473.2945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3133
_refine_ls_wR_factor_ref         0.3279
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5012
_reflns_number_total             6429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c04491_si_004.cif
_cod_data_source_block           dp082_4_apex1
_cod_database_code               4003892
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.767
_shelx_estimated_absorpt_t_min   0.420
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.758(4)
 0.242(4)
;
_shelx_res_checksum              45
_shelx_hkl_checksum              48333
_olex2_submission_special_instructions 'No special instructions were received'