Avenue to novel <i>o</i>-carboranyl boron compounds - reactivity study of <i>o</i>-carborane-fused aminoborirane towards organic azides.
Wang, Junyi; Xiang, Libo; Liu, Xiaocui; Matler, Alexander; Lin, Zhenyang; Ye, Qing; Chemical science 15 (2024) 4839–4845; doi:10.1039/d4sc00489b

data_1571061
_publ_section_title
;
 Avenue to novel <i>o</i>-carboranyl boron compounds - reactivity study of
 <i>o</i>-carborane-fused aminoborirane towards organic azides.
;
_journal_issue                   13
_journal_name_full               'Chemical science'
_journal_page_first              4839
_journal_page_last               4845
_journal_paper_doi               10.1039/d4sc00489b
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C11 H37 B11 N2 Si3'
_chemical_formula_sum            'C11 H37 B11 N2 Si3'
_chemical_formula_weight         400.60
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2023-07-03 deposited with the CCDC.	2024-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.3940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9271(3)
_cell_length_b                   24.7750(6)
_cell_length_c                   10.7243(3)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      24.736
_cell_measurement_theta_min      2.727
_cell_volume                     2487.91(12)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            41430
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.759
_diffrn_reflns_theta_max         24.759
_diffrn_reflns_theta_min         2.325
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1196 before and 0.0643 after correction. The Ratio of minimum to maximum transmission is 0.9219. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4255
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0378P)^2^+1.5971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3856
_reflns_number_total             4255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc00489b2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 1571058--1571061.cif.'
_cod_database_code               1571061
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.927
_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.a Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10B,H10A,H10C), C11(H11A,H11B,
 H11C)
2.b Boron cage BH refined with riding coordinates:
 B2(H2), B3(H3), B4(H4), B5(H5), B6(H6), B7(H7), B8(H8), B9(H9), B10(H10),
 B11(H11)
;
_shelx_res_checksum              20541
_olex2_submission_special_instructions 'No special instructions were received'