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_4003890
_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(Cl24 Rb4 Sb4)'
_chemical_formula_sum            'Cl6 Rb Sb'
_chemical_formula_weight         419.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.905(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0736(4)
_cell_length_b                   6.3321(2)
_cell_length_c                   12.1366(3)
_cell_measurement_reflns_used    5458
_cell_measurement_temperature    293
_cell_measurement_theta_max      41.9900
_cell_measurement_theta_min      1.7200
_cell_volume                     907.90(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_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
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     12.38 132.88   0.50   70.00    --   52.50  73.75-125.75  241
  2  \w    -41.81 151.69   0.50   70.00    --   -5.00  73.75  96.76  387
  3  \f    -24.95 342.78   0.50   69.82  79.26  -7.50  73.75    --   735
  4  \w    -91.74 116.76   0.50   70.00    --  -52.50  73.75 104.26  417
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0525219000
_diffrn_orient_matrix_UB_12      -0.0268344000
_diffrn_orient_matrix_UB_13      0.0142020000
_diffrn_orient_matrix_UB_21      0.0263347000
_diffrn_orient_matrix_UB_22      -0.0853767000
_diffrn_orient_matrix_UB_23      0.0331603000
_diffrn_orient_matrix_UB_31      0.0127600000
_diffrn_orient_matrix_UB_32      0.0670744000
_diffrn_orient_matrix_UB_33      0.0475901000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5049
_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         31.495
_diffrn_reflns_theta_min         3.431
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.040
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.960
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.16b (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.072
_exptl_crystal_description       needle
_exptl_crystal_F_000             760
_exptl_crystal_recrystallization_method
'Crystallized solvothermally from HCl/HNO3 solution'
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.103
_refine_diff_density_max         3.230
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         1504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0647P)^2^+1.3476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0954
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1332
_reflns_number_total             1504
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c04491_si_005.cif
_cod_data_source_block           dp064_2
_cod_database_code               4003890
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Rb Sb Cl6'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
;
_shelx_res_checksum              48372
_shelx_hkl_checksum              44795
_olex2_exptl_crystal_mounting_method Tip-mounted
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.990
_oxdiff_exptl_absorpt_empirical_full_min 0.583