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_4003893
_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(Cl20 O4 Rb8 Sb4)'
_chemical_formula_sum            'Cl5 O Rb2 Sb'
_chemical_formula_weight         485.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-31
_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                   14.0332(6)
_cell_length_b                   10.1091(4)
_cell_length_c                   7.2292(3)
_cell_measurement_reflns_used    8737
_cell_measurement_temperature    300
_cell_measurement_theta_max      31.3950
_cell_measurement_theta_min      2.8710
_cell_volume                     1025.56(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_data_collection       'SMART v5.630 (Bruker, 2003)'
_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      300
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.942
_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      2.18 182.00   0.30   30.07    --   28.00  73.93 -25.82  600
  2  \w      2.18 182.00   0.30   30.07    --   28.00  73.93  94.18  600
  3  \w      2.18 182.00   0.30   30.06    --   28.00  73.93-145.82  600
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0275381000
_diffrn_orient_matrix_UB_12      0.0527614000
_diffrn_orient_matrix_UB_13      0.0362507000
_diffrn_orient_matrix_UB_21      -0.0289087000
_diffrn_orient_matrix_UB_22      -0.0008213000
_diffrn_orient_matrix_UB_23      -0.0804235000
_diffrn_orient_matrix_UB_31      -0.0309969000
_diffrn_orient_matrix_UB_32      -0.0462603000
_diffrn_orient_matrix_UB_33      0.0429140000
_diffrn_radiation_monochromator  Parallel,graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11208
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.520
_diffrn_reflns_theta_min         2.903
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    13.356
_exptl_absorpt_correction_T_max  2.374
_exptl_absorpt_correction_T_min  0.727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.16b (Rigaku Oxford Diffraction, 2018)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    3.147
_exptl_crystal_description       plate
_exptl_crystal_F_000             872
_exptl_crystal_preparation       'Solvothermally crystallized from HCl'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.503
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         1694
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0408P)^2^+3.5647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1520
_reflns_number_total             1694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c04491_si_001.cif
_cod_data_source_block           dp085
_cod_database_code               4003893
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Rb4InSbCl12
_shelx_estimated_absorpt_t_max   0.690
_shelx_estimated_absorpt_t_min   0.157
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
;
_shelx_res_checksum              58527
_shelx_hkl_checksum              12554
_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 2.374
_oxdiff_exptl_absorpt_empirical_full_min 0.727