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_4109965
_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_moiety         'C26 H46 Cl2 N4 Si5'
_chemical_formula_sum            'C26 H46 Cl2 N4 Si5'
_chemical_formula_weight         626.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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_date             07-06-04
_audit_creation_method           'STOE X-RED'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.016(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.2473(15)
_cell_length_b                   8.9149(5)
_cell_length_c                   18.8561(14)
_cell_measurement_reflns_used    12176
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.55
_cell_measurement_theta_min      2.70
_cell_volume                     3571.7(4)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  'X-STEP32, Microsoft Word'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'area detector'
_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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11434
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    0.371
_exptl_absorpt_correction_T_max  0.9546
_exptl_absorpt_correction_T_min  0.9166
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       prism
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0540P)^2^+0.6303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0857
_reflns_number_gt                2598
_reflns_number_total             3156
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja074019esi20070626_040059_3.cif
_cod_data_source_block           compound4
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4109965