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_7132435
_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         'C4 H22 B20 O2'
_chemical_formula_sum            'C4 H22 B20 O2'
_chemical_formula_weight         318.41
_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_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2023-05-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-06-07 deposited with the CCDC.	2023-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.213(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3573(3)
_cell_length_b                   12.9050(3)
_cell_length_c                   13.1240(3)
_cell_measurement_reflns_used    2865
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.2350
_cell_measurement_theta_min      3.6140
_cell_volume                     1937.57(9)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -104.00 -11.00   1.00    1.00    --  -33.50 -37.00-180.00   93
  2  \w   -108.00 -35.00   1.00    1.00    --  -33.50 178.00-120.00   73
  3  \w    -38.00  21.00   1.00    1.00    --  -33.50  57.00 -60.00   59
  4  \w      3.00  41.00   1.00    1.00    --   36.47 -99.00-180.00   38
  5  \w     40.00  74.00   1.00    1.00    --   36.47 -99.00 -60.00   34
  6  \w     44.00  74.00   1.00    1.00    --   36.47 -99.00-180.00   30
  7  \w     91.00 178.00   1.00    5.00    --  108.00  45.00 -60.00   87
  8  \w     38.00 103.00   1.00    5.00    --  108.00 -94.00  60.00   65
  9  \w    103.00 177.00   1.00    5.00    --  108.00  77.00 150.00   74
 10  \w    117.00 164.00   1.00    5.00    --  108.00  77.00-120.00   47
 11  \w     81.00 109.00   1.00    5.00    --  108.00-111.00-180.00   28
 12  \w     64.00 108.00   1.00    5.00    --  108.00-111.00   0.00   44
 13  \w     56.00 119.00   1.00    5.00    --  108.00 -61.00 150.00   63
 14  \w    125.00 158.00   1.00    5.00    --  108.00 111.00 120.00   33
 15  \w    149.00 175.00   1.00    5.00    --  108.00  61.00 -90.00   26
 16  \w     39.00  72.00   1.00    5.00    --  108.00 -94.00-180.00   33
 17  \w     88.00 113.00   1.00    5.00    --  108.00  61.00 -90.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1245220000
_diffrn_orient_matrix_UB_12      -0.0159638000
_diffrn_orient_matrix_UB_13      0.0026436000
_diffrn_orient_matrix_UB_21      -0.0158677000
_diffrn_orient_matrix_UB_22      -0.1182659000
_diffrn_orient_matrix_UB_23      0.0021705000
_diffrn_orient_matrix_UB_31      -0.0485219000
_diffrn_orient_matrix_UB_32      -0.0022916000
_diffrn_orient_matrix_UB_33      -0.1268227000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7051
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.070
_diffrn_reflns_theta_max         67.070
_diffrn_reflns_theta_min         3.864
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98711
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3457
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0675
_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^)+(0.1342P)^2^+0.1490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1854
_refine_ls_wR_factor_ref         0.2037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2743
_reflns_number_total             3457
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05041f2.cif
_cod_data_source_block           202305123_auto
_cod_depositor_comments
'Adding full bibliography for 7132433--7132440.cif.'
_cod_original_cell_volume        1937.57(8)
_cod_database_code               7132435
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C20H20N2O1B7
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.936
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
2. Restrained distances
 O1-H1
 0.9 with sigma of 0.02
3.a Riding coordinates:
 O2(H2)
3.b Boron cage BH refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3), C4(H4), B1(H1B), B2(H2B), B3(H3A), B5(H5), B6(H6),
 B8(H8), B9(H9), B10(H10), B11(H11), B12(H12), B13(H13), B15(H15), B16(H16),
 B18(H18), B19(H19), B20(H20)
;
_shelx_res_checksum              17299
_shelx_hkl_checksum              59392
_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 1.134
_oxdiff_exptl_absorpt_empirical_full_min 0.946