Reactions of StableN-Heterocyclic Silylenes with Ketones and 3,5-Di-tert-butyl-o-benzoquinone
Azhakar, Ramachandran; Ghadwal, Rajendra S.; Roesky, Herbert W.; Hey, Jakob; Stalke, Dietmar; Organometallics 30 (2011) 3853–; doi:10.1021/om200388a

data_4064876
_publ_contact_author             'Prof. Dr. D. Stalke'
_publ_section_title
;
 Reactions of StableN-Heterocyclic Silylenes with Ketones and
 3,5-Di-tert-butyl-o-benzoquinone
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3853
_journal_paper_doi               10.1021/om200388a
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C41 H52 Fe N2 O Si'
_chemical_formula_sum            'C41 H52 Fe N2 O Si'
_chemical_formula_weight         672.79
_chemical_name_systematic
; 
 ? 
;
_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                 104.5550(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.2031(5)
_cell_length_b                   10.0796(2)
_cell_length_c                   35.5186(8)
_cell_measurement_reflns_used    5008
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.421
_cell_measurement_theta_min      2.264
_cell_volume                     7347.4(3)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2008.11'
_computing_data_reduction        'SAINT V7.46A'
_computing_molecular_graphics    'XSHELL in SHELXTL-97'
_computing_publication_material  'XSHELL in SHELXTL-97'
_computing_structure_refinement  'SHELXL in SHELXTL Version 2008/3'
_computing_structure_solution    'SHELXS in SHELXTL Version 2008/3'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC mirror optics'
_diffrn_radiation_source         'INCOATEC Mo-microfocus source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            58971
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.476
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/2'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         6648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+13.6534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                5810
_reflns_number_total             6648
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200388a_si_001.cif
_cod_data_source_block           comp4
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4064876