Isolation of a Stable, Acyclic, Two-Coordinate Silylene
Brian D. Rekken; Thomas M. Brown; James C. Fettinger; Heikki M. Tuononen; Philip P. Power; Journal of the American Chemical Society 134 (2012) 6504–6507; doi:10.1021/ja301091v

data_4117839
_publ_section_title
;
 Isolation of a Stable, Acyclic, Two-Coordinate Silylene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6504
_journal_page_last               6507
_journal_paper_doi               10.1021/ja301091v
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C48 H50 Br2 S2 Si'
_chemical_formula_sum            'C48 H50 Br2 S2 Si'
_chemical_formula_weight         878.91
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.7230(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0546(8)
_cell_length_b                   14.7263(8)
_cell_length_c                   18.1452(9)
_cell_measurement_reflns_used    9445
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      32.09
_cell_measurement_theta_min      2.54
_cell_volume                     4288.0(4)
_computing_cell_refinement       'SAINT (7.68A) (Bruker, 2009)'
_computing_data_collection       'Apex2 (2010-11.3) (Bruker, 2010)'
_computing_data_reduction        'SAINT (7.68A) (Bruker, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Duo APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            66955
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    2.048
_exptl_absorpt_correction_T_max  0.7069
_exptl_absorpt_correction_T_min  0.4793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       Block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         12509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0269P)^2^+2.0573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0654
_reflns_number_gt                10243
_reflns_number_total             12509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja301091v_si_003.cif
_cod_data_source_block           bdr177
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4117839