Reactivity Studies of a Stable N-Heterocyclic Silylene with Triphenylsilanol and Pentafluorophenol
Azhakar, Ramachandran; Ghadwal, Rajendra S.; Roesky, Herbert W.; Granitzka, Markus; Stalke, Dietmar; Organometallics 31 (2012) 5506–; doi:10.1021/om300476q

data_4078864
_publ_section_title
;
 Reactivity Studies of a Stable N-Heterocyclic Silylene with
 Triphenylsilanol and Pentafluorophenol
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              5506
_journal_paper_doi               10.1021/om300476q
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C65 H72 N2 O2 Si3'
_chemical_formula_sum            'C65 H72 N2 O2 Si3'
_chemical_formula_weight         997.52
_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                77.70(2)
_cell_angle_beta                 82.64(2)
_cell_angle_gamma                84.99(3)
_cell_formula_units_Z            2
_cell_length_a                   13.865(2)
_cell_length_b                   14.152(2)
_cell_length_c                   15.025(3)
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.495
_cell_measurement_theta_min      2.179
_cell_volume                     2851.3(8)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2011.2'
_computing_data_reduction        'SAINT V7.68A'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX II Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            55395
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.9703
_exptl_absorpt_correction_T_min  0.9264
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         13082
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0424P)^2^+1.3140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                11178
_reflns_number_total             13082
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300476q_si_002.cif
_cod_data_source_block           p-1
_cod_database_code               4078864