Chlorinated polyhedral selenaboranes revisited by joint experimental/computational efforts: the formation of <i>closo</i>-1-SeB<sub>9</sub>Cl<sub>9</sub> and the crystal structure of <i>closo</i>-SeB<sub>11</sub>Cl<sub>11</sub>.
Keller, Willi; Hofmann, Matthias; Wadepohl, Hubert; Enders, Markus; Fanfrlík, Jindřich; Hnyk, Drahomír; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt02987e

data_7714378
_publ_section_title
;
 Chlorinated polyhedral selenaboranes revisited by joint
 experimental/computational efforts: the formation of
 <i>closo</i>-1-SeB<sub>9</sub>Cl<sub>9</sub> and the crystal structure of
 <i>closo</i>-SeB<sub>11</sub>Cl<sub>11</sub>.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt02987e
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'B11 Cl11 Se'
_chemical_formula_sum            'B11 Cl11 Se'
_chemical_formula_weight         587.82
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ex_wk1
_audit_creation_date             2017-05-15
_audit_creation_method
;
Olex2 1.2
(compiled Mar 28 2017 19:34:44 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2023-03-26 deposited with the CCDC.	2023-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.7986(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.85030(9)
_cell_length_b                   26.9786(2)
_cell_length_c                   9.14388(9)
_cell_measurement_reflns_used    67816
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      32.1390
_cell_measurement_theta_min      2.5430
_cell_volume                     1913.24(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_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     -3.00  97.00   0.50    2.00    --   27.02  77.00-180.00  200
  2  \w    -42.00  48.00   0.50    2.00    --   27.02 -57.00  60.00  180
  3  \w      7.00  96.00   0.50    2.00    --   27.02  57.00  30.00  178
  4  \w    -43.00  57.00   0.50    2.00    --   27.02 -77.00 -30.00  200
  5  \w     -3.00  97.00   0.50    2.00    --   27.02  77.00  90.00  200
  6  \w    -43.00  57.00   0.50    2.00    --   27.02 -77.00-120.00  200
  7  \w     -3.00  97.00   0.50    2.00    --   27.02  77.00 -60.00  200
  8  \w    -20.00  69.00   0.50    2.00    --   27.02 -99.00-180.00  178
  9  \w      2.00  99.00   0.50    2.00    --   27.02  38.00 -60.00  194
 10  \w    -17.00 100.00   0.50    2.00    --   27.02  19.00-180.00  234
 11  \w     -3.00  97.00   0.50    2.00    --   27.02  77.00   0.00  200
 12  \w    -20.00  69.00   0.50    2.00    --   27.02 -99.00-120.00  178
 13  \w      7.00  96.00   0.50    2.00    --   27.02  57.00 -90.00  178
 14  \w    -20.00  69.00   0.50    2.00    --   27.02 -99.00  60.00  178
 15  \w      7.00  96.00   0.50    2.00    --   27.02  57.00 -30.00  178
 16  \w    -46.00 100.00   0.50    2.00    --   27.02   0.00-180.00  292
 17  \w    -46.00 100.00   0.50    2.00    --   27.02   0.00-150.00  292
 18  \w    -46.00 100.00   0.50    2.00    --   27.02   0.00-120.00  292
 19  \w    -46.00 100.00   0.50    2.00    --   27.02   0.00 -90.00  292
 20  \w      7.00  96.00   0.50    2.00    --   27.02  57.00-180.00  178
 21  \w    -46.00 100.00   0.50    2.00    --   27.02   0.00 -30.00  292
 22  \w    -46.00  40.00   0.50    2.00    --   27.02   0.00   0.00  172
 23  \w    -46.00 100.00   0.50    2.00    --   27.02   0.00 -60.00  292
 24  \f    -60.00 210.00   0.50    0.10   0.00   0.00   0.00    --   540
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0698392000
_diffrn_orient_matrix_UB_12      -0.0141894000
_diffrn_orient_matrix_UB_13      -0.0599872000
_diffrn_orient_matrix_UB_21      -0.0416928000
_diffrn_orient_matrix_UB_22      0.0016730000
_diffrn_orient_matrix_UB_23      0.0494210000
_diffrn_orient_matrix_UB_31      -0.0418417000
_diffrn_orient_matrix_UB_32      0.0220712000
_diffrn_orient_matrix_UB_33      -0.0423406000
_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  0.0359
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            121819
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.365
_diffrn_reflns_theta_min         2.542
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.479
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.205
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model (Busing & Levy, 1957).
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    2.041
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.391
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 5881 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0035(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         13175
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0190
_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^)+(0.0153P)^2^+0.4254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0384
_refine_ls_wR_factor_ref         0.0387
_reflns_Friedel_coverage         0.927
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                12843
_reflns_number_total             13175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02987e2.cif
_cod_data_source_block           ex_wk1
_cod_database_code               7714378
_audit_block_refno               2883
_audit_block_usercomment         'W. Keller SeB11'
_chemical_oxdiff_formula         'Se1 B11 Cl11'
_chemical_oxdiff_usercomment     'W. Keller SeB11'
_shelx_estimated_absorpt_t_max   0.722
_shelx_estimated_absorpt_t_min   0.722
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_shelxl_version_number           2016/6
_olex2_refinement_description
;
;
_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 1.147
_oxdiff_exptl_absorpt_empirical_full_min 0.866
_shelx_res_checksum              43608
_cell_oxdiff_length_a            8.84944(7)
_cell_oxdiff_length_b            26.97772(16)
_cell_oxdiff_length_c            9.14550(7)
_cell_oxdiff_angle_alpha         90.0118(6)
_cell_oxdiff_angle_beta          118.8034(8)
_cell_oxdiff_angle_gamma         89.9469(6)
_cell_oxdiff_volume              1913.24(2)
_cell_oxdiff_measurement_reflns_used 67816