Regiospecific C‒H Bond Activation: Reactivity Study of N-Heterocyclic Silylene toward Ambidentate Phosphorus Ylide
Azhakar, Ramachandran; Sarish, Sankaranarayana Pillai; Roesky, Herbert W.; Hey, Jakob; Stalke, Dietmar; Organometallics 30 (2011) 2897–; doi:10.1021/om200308u

data_4064748
_publ_section_title
;
 Regiospecific C--H Bond Activation: Reactivity Study of N-Heterocyclic
 Silylene toward Ambidentate Phosphorus Ylide
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2897
_journal_paper_doi               10.1021/om200308u
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C50 H59 N2 O P Si, C7 H16'
_chemical_formula_sum            'C57 H75 N2 O P Si'
_chemical_formula_weight         863.25
_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                 98.430(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.976(6)
_cell_length_b                   11.607(3)
_cell_length_c                   35.602(9)
_cell_measurement_reflns_used    2767
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      14.749
_cell_measurement_theta_min      2.308
_cell_volume                     10209(4)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX v2008.11'
_computing_data_reduction        'SAINT V7.66A'
_computing_molecular_graphics    'XP in SHELXTL Version 2008/3'
_computing_publication_material  'XShell in SHEXTL-97'
_computing_structure_refinement  'SHELXL in SHEXTL Version 2008/3'
_computing_structure_solution    'SHELXS in SHEXTL Version 2008/3'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'BRUKER SMART APEX II QUASAR'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC x-ray optics'
_diffrn_radiation_source         'INCOATEC Ag Microfocus Source'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0982
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            96732
_diffrn_reflns_theta_full        20.12
_diffrn_reflns_theta_max         20.12
_diffrn_reflns_theta_min         0.91
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         9827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0733P)^2^+19.4430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1580
_reflns_number_gt                7565
_reflns_number_total             9829
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200308u_si_002.cif
_cod_data_source_block           c2c
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4064748