Insertion of Cyclic Alkyl(amino) Carbene into the Si-H Bonds of Hydrochlorosilanes.
Mohapatra, Chandrajeet; Samuel, Prinson P.; Li, Bin; Niepötter, Benedikt; Schürmann, Christian J; Herbst-Irmer, Regine; Stalke, Dietmar; Maity, Bholanath; Koley, Debasis; Roesky, Herbert W.; Inorganic chemistry 55 (2016) 1953–1955; doi:10.1021/acs.inorgchem.6b00024

data_4347329
_publ_section_title
;
 Insertion of Cyclic Alkyl(amino) Carbene into the Si-H Bonds of
 Hydrochlorosilanes.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1953
_journal_page_last               1955
_journal_paper_doi               10.1021/acs.inorgchem.6b00024
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         '2(C35 H58 Cl2 N2 Si2), C7 H8'
_chemical_formula_sum            'C38.5 H62 Cl2 N2 Si2'
_chemical_formula_weight         679.98
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 118.24(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.688(3)
_cell_length_b                   11.024(2)
_cell_length_c                   20.330(3)
_cell_measurement_temperature    100(2)
_cell_volume                     3887.2(13)
_computing_data_collection       'APEX2 v2012.2'
_computing_molecular_graphics    'XSHELL in SHELXTL97'
_computing_publication_material  'XSHELL in SHELXTL97'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
'SHELXT (G.M.Sheldrick,Acta Cryst.(2015)A71,3-8)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            84942
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.695
_diffrn_reflns_theta_min         1.174
_diffrn_source                   'INCOATEC Microsource'
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.7198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/4
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       block
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         10040
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0390P)^2^+1.8046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8796
_reflns_number_total             10040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00024_si_002.cif
_cod_data_source_block           p21_c_a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C38.50 H62 Cl2 N2 Si2'
_cod_database_code               4347329
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              71326
_shelx_hkl_checksum              3724