9,9'-Bis-<i>o</i>-carboranes: synthesis and exploration of properties.
Chen, Feijing; Guo, Wenjing; Ma, Yan-Na; Chen, Xuenian; Chemical communications (Cambridge, England) 60 (2024) 614–617; doi:10.1039/d3cc05041f

data_7132436
_publ_section_title
;
 9,9'-Bis-<i>o</i>-carboranes: synthesis and exploration of properties.
;
_journal_issue                   5
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              614
_journal_page_last               617
_journal_paper_doi               10.1039/d3cc05041f
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C2 H11 B10'
_chemical_formula_sum            'C2 H11 B10'
_chemical_formula_weight         143.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-08
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-06-07 deposited with the CCDC.	2023-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.066(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.9432(3)
_cell_length_b                   10.0433(5)
_cell_length_c                   12.6587(6)
_cell_measurement_reflns_used    3163
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      71.3850
_cell_measurement_theta_min      5.6320
_cell_volume                     876.02(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_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    -74.00 -49.00   1.00    1.00    --  -35.62 -13.00 159.00   25
  2  \w    -46.00 -21.00   1.00    1.00    --  -35.62  13.00 -28.00   25
  3  \w     35.00  96.00   1.00    1.00    --   35.62  13.00 -28.00   61
  4  \w    -18.00  31.00   1.00    1.00    --   35.62 -13.00 159.00   49
  5  \w     97.00 175.00   1.00    2.74    --  107.12  13.00 -28.00   78
  6  \w     37.00  81.00   1.00    2.74    --  107.12 -13.00 159.00   44
  7  \w    -93.00 -43.00   1.00    1.00    --  -35.62-178.00  30.00   50
  8  \w    -98.00 -38.00   1.00    1.00    --  -35.62 -57.00 -30.00   60
  9  \w    -36.00  64.00   1.00    1.00    --   35.62 -19.00 -30.00  100
 10  \w     14.00  72.00   1.00    1.00    --   35.62 -99.00-120.00   58
 11  \w     10.00  74.00   1.00    1.00    --   35.62 -99.00 -30.00   64
 12  \w     59.00  99.00   1.00    1.00    --   35.62-178.00 -90.00   40
 13  \w     10.00  71.00   1.00    1.00    --   35.62 -99.00  90.00   61
 14  \w     57.00 106.00   1.00    2.74    --  107.12 -95.00 -30.00   49
 15  \w     42.00 124.00   1.00    2.74    --  107.12 -45.00   0.00   82
 16  \w     40.00 125.00   1.00    2.74    --  107.12 -45.00 -90.00   85
 17  \w    104.00 171.00   1.00    2.74    --  107.12  77.00  60.00   67
 18  \w     61.00 109.00   1.00    2.74    --  107.12-111.00 150.00   48
 19  \w     40.00  96.00   1.00    2.74    --  107.12-111.00 -60.00   56
 20  \w     90.00 116.00   1.00    2.74    --  107.12  45.00-150.00   26
 21  \w    105.00 174.00   1.00    2.74    --  107.12  77.00   0.00   69
 22  \w    143.00 168.00   1.00    2.74    --  107.12  45.00-150.00   25
 23  \w     66.00 113.00   1.00    2.74    --  107.12 -77.00   0.00   47
 24  \w     64.00 125.00   1.00    2.74    --  107.12 178.00 -90.00   61
 25  \w     43.00  69.00   1.00    2.74    --  107.12 -95.00-120.00   26
 26  \w    122.00 152.00   1.00    2.74    --  107.12 111.00 -90.00   30
 27  \w     44.00 102.00   1.00    2.74    --  107.12 -95.00-150.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0585594000
_diffrn_orient_matrix_UB_12      -0.1478709000
_diffrn_orient_matrix_UB_13      0.0089101000
_diffrn_orient_matrix_UB_21      0.2155049000
_diffrn_orient_matrix_UB_22      0.0406512000
_diffrn_orient_matrix_UB_23      0.0197179000
_diffrn_orient_matrix_UB_31      -0.0115127000
_diffrn_orient_matrix_UB_32      0.0046323000
_diffrn_orient_matrix_UB_33      0.1206647000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5428
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.461
_diffrn_reflns_theta_min         5.640
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.275
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74379
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_description       block
_exptl_crystal_F_000             292
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0659
_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^)+(0.1024P)^2^+0.2531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1841
_refine_ls_wR_factor_ref         0.1896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1474
_reflns_number_total             1685
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05041f2.cif
_cod_data_source_block           20230315-wy_auto
_cod_depositor_comments
'Adding full bibliography for 7132433--7132440.cif.'
_cod_database_code               7132436
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C1 B1 H1'
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.997
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Boron cage BH refined with riding coordinates:
 C4(H4), C5(H5)
;
_shelx_res_checksum              41501
_shelx_hkl_checksum              8732
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.446
_oxdiff_exptl_absorpt_empirical_full_min 0.528