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_4070382
_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            'C41 H52 Br4 N2 Si'
_chemical_formula_weight         920.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0120(16)
_cell_length_b                   14.9509(15)
_cell_length_c                   17.2127(17)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    99(2)
_cell_measurement_theta_max      28.3155
_cell_measurement_theta_min      2.2075
_cell_volume                     4120.6(7)
_computing_cell_refinement       'Bruker AXS SAINT (v 7.46a, Bruker 2007)'
_computing_data_collection       'APEX2 (v2.2-0, Bruker 2007)'
_computing_data_reduction        'Bruker AXS SAINT (v 7.46a, Bruker 2007)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (v 6.3.1, Bruker 2004)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker TXS with D8-Goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'multilayer Mo mirrors'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0113
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            91720
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    3.966
_exptl_absorpt_correction_T_max  0.5877
_exptl_absorpt_correction_T_min  0.2999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs-2007/4
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0232
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+3.5565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0617
_reflns_number_gt                4667
_reflns_number_total             5286
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9007696_si_001.cif
_cod_data_source_block           rajendra6
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               4070382