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_7132437
_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         '2(C10 H17 B10)'
_chemical_formula_sum            'C20 H34 B20'
_chemical_formula_weight         490.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-04-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-09-11 deposited with the CCDC.	2023-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.014(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2379(7)
_cell_length_b                   7.7225(2)
_cell_length_c                   18.3961(6)
_cell_measurement_reflns_used    3597
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.0790
_cell_measurement_theta_min      4.3570
_cell_volume                     2859.25(16)
_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    'olex2.solve (Bourhis et al., 2015)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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   -106.00   4.00   0.50    3.00    --  -33.50 -19.00  90.00  220
  2  \w   -108.00 -35.00   0.50    3.00    --  -33.50 178.00-150.00  146
  3  \w   -106.00 -73.00   0.50    3.00    --  -33.50 178.00 -30.00   66
  4  \w     54.00  95.00   0.50    3.00    --   36.47-134.00-111.00   82
  5  \w     26.00  54.00   0.50    3.00    --   36.47 -57.00 -60.00   56
  6  \w     44.00 109.00   0.50   19.00    --  108.00-111.00  30.00  130
  7  \w     57.00 107.00   0.50   19.00    --  108.00-111.00 -60.00  100
  8  \w     66.00 109.00   0.50   19.00    --  108.00 178.00   0.00   86
  9  \w    103.00 177.00   0.50   19.00    --  108.00  77.00 150.00  148
 10  \w     48.00 102.00   0.50   19.00    --  108.00 -94.00  60.00  108
 11  \w    115.00 177.00   0.50   19.00    --  108.00  77.00   0.00  124
 12  \w     90.00 143.00   0.50   19.00    --  108.00  61.00  90.00  106
 13  \w    108.00 172.00   0.50   19.00    --  108.00 111.00-150.00  128
 14  \w     57.00  83.00   0.50   19.00    --  108.00 -94.00-120.00   52
 15  \w    101.00 168.00   0.50   19.00    --  108.00  77.00 -60.00  134
;
_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      0.0151748000
_diffrn_orient_matrix_UB_12      -0.1955147000
_diffrn_orient_matrix_UB_13      0.0033143000
_diffrn_orient_matrix_UB_21      -0.0750261000
_diffrn_orient_matrix_UB_22      -0.0395313000
_diffrn_orient_matrix_UB_23      -0.0086302000
_diffrn_orient_matrix_UB_31      0.0002352000
_diffrn_orient_matrix_UB_32      -0.0036490000
_diffrn_orient_matrix_UB_33      -0.0836913000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5083
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.060
_diffrn_reflns_theta_max         67.060
_diffrn_reflns_theta_min         4.394
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.371
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88355
_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    1.140
_exptl_crystal_description       plate
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         5083
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_gt           0.0988
_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^)+(0.1819P)^2^+1.4317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2969
_refine_ls_wR_factor_ref         0.3124
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4003
_reflns_number_total             5083
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05041f2.cif
_cod_data_source_block           20230498_auto_tw
_cod_depositor_comments
'Adding full bibliography for 7132433--7132440.cif.'
_cod_original_cell_volume        2859.23(16)
_cod_database_code               7132437
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C20H20N2O4B10
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.943
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.560(6)
 0.440(6)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C3'(H3'A,H3'B), C4'(H4'A,H4'B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C7'(H7'), C8'(H8'), C9'(H9'), C10'(H10')
3.c Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3), B4(H4), B5(H5), B6(H6), B7(H7A), B8(H8A), B9(H9A),
 B1'(H1'), B2'(H2'), B3'(H3'), B4'(H4'), B5'(H5'), B6'(H6'), B7'(H7'A),
 B8'(H8'A), B9'(H9'A)
;
_shelx_res_checksum              49826
_shelx_hkl_checksum              52953
_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 1.360
_oxdiff_exptl_absorpt_empirical_full_min 0.868