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_4064747
_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'
_chemical_formula_sum            'C50 H59 Cl0 N2 O P Si'
_chemical_formula_weight         763.05
_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    0.064
_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    0.993
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
 Diffuse residual density in channels through unit cell resulting from
 heavily disordered solvent hexane could not be modeled  satisfyingly.
 Results from refinement with modeled solvent is attached in second entry
 "data_c2c".
;
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         9829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0560P)^2^+5.4483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1222
_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_squeeze
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4064747