Neutral Penta- and Hexacoordinate N-Heterocyclic Carbene Complexes Derived from SiX4(X = F, Br)
Ghadwal, Rajendra S.; Sen, Sakya S.; Roesky, Herbert W.; Tavcar, Gasper; Merkel, Sebastian; Stalke, Dietmar; Organometallics 28 (2009) 6374–; doi:10.1021/om9007696

data_4070380
_publ_section_title
;
 Neutral Penta- and Hexacoordinate N-Heterocyclic Carbene Complexes
 Derived from SiX4(X = F, Br)
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6374
_journal_paper_doi               10.1021/om9007696
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C37.5 H48 F4 N2 Si'
_chemical_formula_weight         630.87
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.188(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.332(5)
_cell_length_b                   14.576(4)
_cell_length_c                   24.406(8)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.507
_cell_measurement_theta_min      2.793
_cell_volume                     7247(4)
_computing_cell_refinement       'SAINT V7.61A (Bruker, 2008)'
_computing_data_collection       'APEX2 v2.2.-0 (Bruker, 2008)'
_computing_data_reduction        'SAINT V7.61A (Bruker, 2008)'
_computing_molecular_graphics    'XSHELL v4.01 (Bruker, 2000)'
_computing_publication_material  'XSHELL v4.01 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart Apex with D8-Goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC Quazar multilayer mirror optics'
_diffrn_radiation_source         'micro-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            76619
_diffrn_reflns_theta_full        26.55
_diffrn_reflns_theta_max         26.55
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.9989
_exptl_absorpt_correction_T_min  0.9460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs-2007/4
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         7534
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+13.8166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1467
_reflns_number_gt                5700
_reflns_number_total             7534
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9007696_si_001.cif
_cod_data_source_block           rajendra5
_cod_original_cell_volume        7247(3)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C37.50 H48 F4 N2 Si'
_cod_database_code               4070380