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_7123957
_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         'C16 H20 B10 O2'
_chemical_formula_sum            'C16 H20 B10 O2'
_chemical_formula_weight         352.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                75.207(2)
_cell_angle_beta                 79.295(2)
_cell_angle_gamma                71.188(2)
_cell_formula_units_Z            4
_cell_length_a                   11.2245(3)
_cell_length_b                   11.4449(4)
_cell_length_c                   16.0926(6)
_cell_measurement_reflns_used    18510
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.503
_cell_measurement_theta_min      1.923
_cell_volume                     1879.90(11)
_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      110(2)
_diffrn_detector_area_resol_mean 1.75
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_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  0.0368
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18510
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.503
_diffrn_reflns_theta_min         1.923
_diffrn_source                   'ImuS micro-focus'
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_description       needle
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         7705
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0582P)^2^+0.5153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1354
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5493
_reflns_number_total             7705
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04780h2.cif
_cod_data_source_block           rom66
_cod_database_code               7123957
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.978
_shelx_estimated_absorpt_t_max   0.997
_shelx_res_checksum              24813