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_4347330
_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_absolute_configuration ad
_chemical_formula_moiety         'C30 H47 Cl2 N Si'
_chemical_formula_sum            'C30 H47 Cl2 N Si'
_chemical_formula_weight         520.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 113.64(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.815(2)
_cell_length_b                   16.427(3)
_cell_length_c                   10.972(2)
_cell_measurement_reflns_used    9122
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.578
_cell_measurement_theta_min      2.218
_cell_volume                     1455.5(5)
_computing_cell_refinement       'SAINT V8.30C'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V8.30C'
_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 0.996
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            60081
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         23.694
_diffrn_reflns_theta_min         1.599
_diffrn_source                   'INCOATEC Microsource'
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.7317
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2015/1
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       block
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.404
_exptl_crystal_size_mid          0.385
_exptl_crystal_size_min          0.245
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 3919 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.027(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         8956
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0263
_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^)+(0.0334P)^2^+0.1626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0632
_reflns_Friedel_coverage         0.936
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                8470
_reflns_number_total             8956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00024_si_004.cif
_cod_data_source_block           p21_a
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4347330
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.941
_shelx_estimated_absorpt_t_max   0.964
_shelx_res_checksum              98837
_shelx_hkl_checksum              42260