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_7132433
_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         'C8 H30 B20'
_chemical_formula_sum            'C8 H30 B20'
_chemical_formula_weight         342.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-07-09
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5876(5)
_cell_length_b                   11.2736(5)
_cell_length_c                   10.0616(5)
_cell_measurement_reflns_used    1541
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.6290
_cell_measurement_theta_min      3.9130
_cell_volume                     1087.53(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -62.00  36.00   1.00    2.00    --  -33.50  77.00 -90.00   98
  2  \w   -103.00  -5.00   1.00    2.00    --  -33.50 -77.00  60.00   98
  3  \w    -52.00  35.00   1.00    2.00    --  -33.50  57.00-180.00   87
  4  \w     58.00 110.00   1.00    2.00    --   36.47 178.00  90.00   52
  5  \w     27.00 102.00   1.00    2.00    --   36.47  57.00-120.00   75
  6  \w     61.00 101.00   1.00    2.00    --   36.47  57.00 150.00   40
  7  \w     20.00  53.00   1.00    2.00    --   36.47  57.00 150.00   33
  8  \w     46.00 108.00   1.00    8.00    --  108.00 -45.00   0.00   62
  9  \w     95.00 140.00   1.00    8.00    --  108.00  45.00-150.00   45
 10  \w     37.00 127.00   1.00    8.00    --  108.00 -30.00-180.00   90
 11  \w     38.00 122.00   1.00    8.00    --  108.00 -45.00 -60.00   84
 12  \w     62.00  87.00   1.00    8.00    --  108.00 -94.00  60.00   25
 13  \w     40.00 108.00   1.00    8.00    --  108.00 -94.00 -30.00   68
 14  \w     82.00 146.00   1.00    8.00    --  108.00  30.00   0.00   64
;
_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      -0.0115824000
_diffrn_orient_matrix_UB_12      -0.1325107000
_diffrn_orient_matrix_UB_13      -0.0351723000
_diffrn_orient_matrix_UB_21      -0.0270680000
_diffrn_orient_matrix_UB_22      -0.0293132000
_diffrn_orient_matrix_UB_23      0.1473403000
_diffrn_orient_matrix_UB_31      -0.1580682000
_diffrn_orient_matrix_UB_32      0.0147369000
_diffrn_orient_matrix_UB_33      -0.0226953000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3815
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.045
_diffrn_reflns_theta_max         67.044
_diffrn_reflns_theta_min         5.895
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.289
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.046
_exptl_crystal_description       block
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1033
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0603
_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^)+(0.1314P)^2^+0.1034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.1858
_reflns_Friedel_coverage         0.000
_reflns_number_gt                873
_reflns_number_total             1033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05041f2.cif
_cod_data_source_block           202107200
_cod_depositor_comments
'Adding full bibliography for 7132433--7132440.cif.'
_cod_database_code               7132433
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C30H3O5N2B10
_chemical_oxdiff_usercomment     r
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.958
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2-C1
 1.4 with sigma of 0.02
 C3-C1
 1.55 with sigma of 0.02
3. Others
 Fixed Sof: H3A(0.5) H3B(0.5) H3C(0.5) H4A(0.5) H4B(0.5) H4C(0.5)
4.a Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
4.b Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3), B4(H4), B5(H5)
;
_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 1.471
_oxdiff_exptl_absorpt_empirical_full_min 0.888