Examining the reactivity of tris(<i>ortho</i>-carboranyl)borane with Lewis bases and application in frustrated Lewis pair Si-H bond cleavage.
Vashisth, Kanika; Dutta, Sanjay; Akram, Manjur O.; Martin, Caleb D.; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt01557b

data_7713293
_publ_section_title
;
 Examining the reactivity of tris(<i>ortho</i>-carboranyl)borane with
 Lewis bases and application in frustrated Lewis pair Si-H bond cleavage.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt01557b
_journal_year                    2023
_chemical_formula_moiety         'C6 H34 B31, C9 H24 P Si'
_chemical_formula_sum            'C15 H58 B31 P Si'
_chemical_formula_weight         632.78
_chemical_name_systematic        Triscarborane_trimehtylphosphine_triethylsilane
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-02-02
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-04-28 deposited with the CCDC.	2023-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   13.0069(3)
_cell_length_b                   13.0069(3)
_cell_length_c                   25.8322(8)
_cell_measurement_reflns_used    9793
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.08
_cell_measurement_theta_min      2.40
_cell_volume                     3784.77(17)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0498
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            60697
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.675
_diffrn_reflns_theta_min         2.399
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.8096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0808 before and 0.0643 after correction.
The Ratio of minimum to maximum transmission is 0.9392.
The \l/2 correction factor is Not present.
;
_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    1.111
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_preparation       'Vapour diffusion of Dichloromethane on Hexane'
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.133
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2404
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0716P)^2^+4.8722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1925
_reflns_number_total             2404
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01557b2.cif
_cod_data_source_block           Me3PSiEt3_HBoCb3
_cod_original_cell_volume        3784.8(2)
_cod_database_code               7713293
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.982
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C5(H5A,H5B,H5C)
2.c Boron cage BH refined with riding coordinates:
 B5(H5), B2(H2A), B4(H4), B3(H3), B10(H10), B11(H11), B9(H9), B6(H6), B8(H8),
 B7(H7)
;
_shelx_res_checksum              94971
_olex2_exptl_crystal_mounting_method 'MiTeGen MicroMount'
_olex2_submission_special_instructions 'No special instructions were received'