Synthesis and Structures of Heteroleptic Silylenes
Cheuk-Wai So; Herbert W. Roesky; Prabhuodeyara M. Gurubasavaraj; Rainer B. Oswald; Michael T. Gamer; Peter G. Jones; Steffen Blaurock; Journal of the American Chemical Society 129 (2007) 12049–12054; doi:10.1021/ja074019e

data_4109964
_publ_section_title
;
 Synthesis and Structures of Heteroleptic Silylenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12049
_journal_page_last               12054
_journal_paper_doi               10.1021/ja074019e
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C21 H37 N2 P Si'
_chemical_formula_weight         376.59
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 94.17(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.0623(18)
_cell_length_b                   10.209(2)
_cell_length_c                   12.720(3)
_cell_measurement_reflns_used    1671
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.16
_cell_measurement_theta_min      2.25
_cell_volume                     1173.7(4)
_computing_cell_refinement       'Stoe XAREA'
_computing_data_collection       'Stoe XAREA'
_computing_data_reduction        'Stoe XAREA'
_computing_molecular_graphics    'Bruker SHELXTL PLUS'
_computing_publication_material  'Bruker SHELXTL PLUS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       omega-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6303
_diffrn_reflns_theta_full        29.16
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_T_max  0.9659
_exptl_absorpt_correction_T_min  0.9178
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.066
_exptl_crystal_description       prism
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         6303
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.189
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0683
_reflns_number_gt                5742
_reflns_number_total             6303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja074019esi20070626_040059_2.cif
_cod_data_source_block           compound12
_cod_original_cell_volume        1173.8(4)
_cod_database_code               4109964