The synthesis and structural aspects of the perbromo-functionalised thiaboranes <i>closo</i>-SB<sub><i>n</i></sub>Br<sub><i>n</i></sub> (<i>n</i> = 5, 9, 11): the solid-state structure of the octahedral <i>closo</i>-SB<sub>5</sub>Br<sub>5</sub>, governed by strong dihalogen contacts.
Keller, Willi; Ballmann, Joachim; Fanfrlík, Jindřich; Hnyk, Drahomír; Chemical communications (Cambridge, England) 61 (2025) 2528–2531; doi:10.1039/d4cc06334a

data_7134118
_publ_section_title
;
 The synthesis and structural aspects of the perbromo-functionalised
 thiaboranes <i>closo</i>-SB<sub><i>n</i></sub>Br<sub><i>n</i></sub>
 (<i>n</i> = 5, 9, 11): the solid-state structure of the octahedral
 <i>closo</i>-SB<sub>5</sub>Br<sub>5</sub>, governed by strong dihalogen
 contacts.
;
_journal_issue                   12
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2528
_journal_page_last               2531
_journal_paper_doi               10.1039/d4cc06334a
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'B5 Br5 S'
_chemical_formula_sum            'B5 Br5 S'
_chemical_formula_weight         485.66
_chemical_properties_physical
'air-sensitive, moisture-sensitive,Air-sensitive,Moisture-sensitive'
_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'
_atom_sites_solution_primary     dual
_audit_creation_date             2024-12-03
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-11-16 deposited with the CCDC.	2025-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0170(10)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   18.6919(2)
_cell_length_b                   12.52450(10)
_cell_length_c                   13.22370(10)
_cell_measurement_reflns_used    26296
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      33.7710
_cell_measurement_theta_min      3.0640
_cell_volume                     3095.76(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_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    -52.00  28.00   0.50   30.00    --  -30.00  57.00-120.00  160
  2  \w    -18.00   8.00   0.50   30.00    --  -30.00-100.00  39.54   52
  3  \w    -99.00 -73.00   0.50   30.00    --  -30.00 -57.00-150.00   52
  4  \w    -49.00  -9.00   0.50   30.00    --  -30.00 -57.00-150.00   80
  5  \w    -35.00  48.00   0.50   30.00    --   31.72 -57.00  60.00  166
  6  \w     10.00  37.00   0.50   30.00    --   31.72  57.00 -30.00   54
  7  \w     15.00  44.00   0.50   30.00    --   31.72 -57.00 150.00   58
  8  \w     22.00  93.00   0.50   30.00    --   31.72  38.00-180.00  142
  9  \w    -19.00  75.00   0.50   30.00    --   31.72 -99.00  30.00  188
 10  \w      5.00  49.00   0.50   30.00    --   31.72  38.00 -60.00   88
 11  \w     52.00 104.00   0.50   30.00    --   31.72  38.00 -60.00  104
 12  \w      1.00  44.00   0.50   30.00    --   31.72  77.00   0.00   86
 13  \w     68.00 103.00   0.50   30.00    --   31.72  77.00   0.00   70
 14  \w    -20.00  63.00   0.50   30.00    --   31.72 -99.00-180.00  166
 15  \w     49.00 104.00   0.50   30.00    --   31.72  38.00  90.00  110
 16  \w    -20.00  75.00   0.50   30.00    --   31.72 -99.00 -90.00  190
 17  \w      4.00  40.00   0.50   30.00    --   31.72  38.00  90.00   72
 18  \w      4.00  64.00   0.50   30.00    --   31.72  77.00  90.00  120
 19  \w      0.00 101.00   0.50   30.00    --   31.72  77.00-180.00  202
 20  \w     62.00 101.00   0.50   30.00    --   31.72  57.00 -30.00   78
 21  \w      1.00  29.00   0.50   30.00    --   31.72  77.00 -90.00   56
 22  \w    -32.00  36.00   0.50   30.00    --   31.72 -38.00 -90.00  136
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0350624000
_diffrn_orient_matrix_UB_12      0.0203507000
_diffrn_orient_matrix_UB_13      -0.0069683000
_diffrn_orient_matrix_UB_21      -0.0054444000
_diffrn_orient_matrix_UB_22      0.0364245000
_diffrn_orient_matrix_UB_23      0.0403344000
_diffrn_orient_matrix_UB_31      0.0134428000
_diffrn_orient_matrix_UB_32      -0.0383395000
_diffrn_orient_matrix_UB_33      0.0346268000
_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  0.0469
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            102152
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.143
_diffrn_reflns_theta_min         2.491
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    19.600
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.51a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.126
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       0.000206(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         12413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0233
_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^)+(0.0210P)^2^+0.5448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0464
_refine_ls_wR_factor_ref         0.0499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10100
_reflns_number_total             12413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06334a2.cif
_cod_data_source_block           SB5Br5
_cod_depositor_comments          'Adding full bibliography for 7134118.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7134118
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         SB5Br5
_chemical_oxdiff_usercomment     SB5Br5
_shelx_estimated_absorpt_t_max   0.271
_shelx_estimated_absorpt_t_min   0.111
_olex2_refinement_description
;
;
_shelx_res_checksum              63290
_shelx_hkl_checksum              4472
_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
;