A Self-Catalyzed Reaction of 1,2-Dibenzoyl o-Carborane with Hydrosilanes ‒ Formation of New Hydrofuranes
Jaiswal, Kuldeep; Volodarsky , Solomon; Kampel, Vladimir; Dobrovetsky, Roman; Chemical Communications  (2019) –; doi:10.1039/C9CC04780H

data_7123959
_publ_section_title
;
 A Self-Catalyzed Reaction of 1,2-Dibenzoyl o-Carborane with Hydrosilanes
 -- Formation of New Hydrofuranes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC04780H
_journal_year                    2019
_chemical_formula_moiety         'C22 H36 B10 O2 Si'
_chemical_formula_sum            'C22 H36 B10 O2 Si'
_chemical_formula_weight         468.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2019-06-18 deposited with the CCDC.    2019-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.4050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7044(5)
_cell_length_b                   16.5597(7)
_cell_length_c                   14.4122(6)
_cell_measurement_reflns_used    11908
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.996
_cell_measurement_theta_min      1.990
_cell_volume                     2738.8(2)
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_collection       'Apex2, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 1.75
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '0.5 deg. \f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11908
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.990
_diffrn_source                   'ImuS micro-focus'
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_description       needle
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.387
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.738
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     387
_refine_ls_number_reflns         4800
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0897
_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^)+(0.1328P)^2^+5.4599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2416
_refine_ls_wR_factor_ref         0.2667
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3584
_reflns_number_total             4800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04780h2.cif
_cod_data_source_block           rom47
_cod_database_code               7123959
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.961
_shelx_estimated_absorpt_t_max   0.992
_shelx_res_checksum              72674