Tuning Philicity of Dichlorosilylene: Nucleophilic Behavior of the Dichlorosilylene-NHC Complex Cl<sub>2</sub>Si-IPr.
Lee, Vladimir Ya; Horiguchi, Satoru; Sekiguchi, Akira; Gapurenko, Olga A.; Gribanova, Tatyana N.; Minkin, Vladimir I.; Gornitzka, Heinz; ACS omega 4 (2019) 2902–2906; doi:10.1021/acsomega.8b03429

data_4515121
_publ_section_title
;
 Tuning Philicity of Dichlorosilylene: Nucleophilic Behavior of the
 Dichlorosilylene-NHC Complex Cl<sub>2</sub>Si-IPr.
;
_journal_issue                   2
_journal_name_full               'ACS omega'
_journal_page_first              2902
_journal_page_last               2906
_journal_paper_doi               10.1021/acsomega.8b03429
_journal_volume                  4
_journal_year                    2019
_chemical_formula_sum            'C36 H84 Cl2 Ge Si7'
_chemical_formula_weight         857.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.884(2)
_cell_length_b                   20.255(4)
_cell_length_c                   20.493(4)
_cell_measurement_reflns_used    8254
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.19
_cell_measurement_theta_min      2.22
_cell_volume                     4932.9(16)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.785
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.1262
_diffrn_reflns_Laue_measured_fraction_full 0.785
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9593
_diffrn_reflns_point_group_measured_fraction_full 0.739
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.256
_diffrn_reflns_theta_min         1.414
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.922
_exptl_absorpt_correction_T_max  0.9324
_exptl_absorpt_correction_T_min  0.6530
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            yelllow
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       plate
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.404
_refine_diff_density_min         -1.245
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details
;
 Flack x determined using 1570 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.119(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         6609
_refine_ls_number_restraints     1049
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1403
_refine_ls_R_factor_gt           0.1044
_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^)+(0.1573P)^2^+45.9989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2728
_refine_ls_wR_factor_ref         0.3004
_reflns_Friedel_coverage         0.696
_reflns_Friedel_fraction_full    0.682
_reflns_Friedel_fraction_max     0.868
_reflns_number_gt                4867
_reflns_number_total             6609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b03429_si_003.cif
_cod_data_source_block           GeSi3Cl2_0m
_cod_original_cell_volume        4932.7(17)
_cod_database_code               4515121
_shelxl_version_number           2014-3
_shelx_res_checksum              58362
_shelx_hkl_checksum              16865