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_4070381
_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            'C61 H80 F4 N4 Si'
_chemical_formula_weight         973.38
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.5780(10)
_cell_angle_beta                 85.8090(10)
_cell_angle_gamma                74.8090(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7184(11)
_cell_length_b                   14.6505(11)
_cell_length_c                   20.0103(16)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.593
_cell_measurement_theta_min      2.395
_cell_volume                     3451.5(5)
_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_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            79555
_diffrn_reflns_theta_full        27.12
_diffrn_reflns_theta_max         27.12
_diffrn_reflns_theta_min         1.06
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.9892
_exptl_absorpt_correction_T_min  0.9755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007(5'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.937
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
;
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         15220
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0605P)^2^+0.9230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1362
_reflns_number_gt                11372
_reflns_number_total             15220
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9007696_si_001.cif
_cod_data_source_block           rajendra8-sq
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4070381