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_4064875
_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         '(C43 H60 N2 O2 Si), 2(C1.25 H3)'
_chemical_formula_sum            'C45.5 H66 N2 O2 Si'
_chemical_formula_weight         701.09
_chemical_name_systematic
; 
 ? 
;
_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                73.1430(10)
_cell_angle_beta                 79.4280(10)
_cell_angle_gamma                88.4660(10)
_cell_formula_units_Z            2
_cell_length_a                   12.9856(9)
_cell_length_b                   12.9963(9)
_cell_length_c                   13.3486(9)
_cell_measurement_reflns_used    9459
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.728
_cell_measurement_theta_min      2.251
_cell_volume                     2118.5(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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX II with D8 goniometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'INCOATEC I\mS microfocus source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            59261
_diffrn_reflns_theta_full        26.75
_diffrn_reflns_theta_max         26.75
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/2'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             766
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8992
_refine_ls_number_restraints     143
_refine_ls_restrained_S_all      1.507
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0489P)^2^+1.3795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1151
_reflns_number_gt                7630
_reflns_number_total             8992
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200388a_si_001.cif
_cod_data_source_block           comp03
_cod_original_formula_sum        'C45.50 H66 N2 O2 Si'
_cod_database_code               4064875