Dispersion Forces and Counterintuitive Steric Effects in Main Group Molecules: Heavier Group 14 (Si-Pb) Dichalcogenolate Carbene Analogues with Sub-90° Interligand Bond Angles
Brian D. Rekken; Thomas M. Brown; James C. Fettinger; Felicitas Lips; Heikki M. Tuononen; Rolfe H. Herber; Philip P. Power; Journal of the American Chemical Society 135 (2013) 10134–10148; doi:10.1021/ja403802a

data_4120073
_publ_section_title
;
 Dispersion Forces and Counterintuitive Steric Effects in Main Group
 Molecules: Heavier Group 14 (Si-Pb) Dichalcogenolate Carbene Analogues
 with Sub-90\% Interligand Bond Angles
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10134
_journal_page_last               10148
_journal_paper_doi               10.1021/ja403802a
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         '(C72 H98 Br2 S2 Si), (C6 H14)'
_chemical_formula_sum            'C78 H112 Br2 S2 Si'
_chemical_formula_weight         1301.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 98.173(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.0349(10)
_cell_length_b                   12.9722(5)
_cell_length_c                   22.5882(9)
_cell_measurement_reflns_used    4098
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      69.88
_cell_measurement_theta_min      5.67
_cell_volume                     7551.2(5)
_computing_cell_refinement       'SAINT (8.27b) (Bruker, 2012)'
_computing_data_collection       'Apex2 (2012.2-0) (Bruker, 2012)'
_computing_data_reduction        'SAINT (8.27b) (Bruker, 2012)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker Duo APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12795
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.243
_diffrn_reflns_theta_min         5.672
_exptl_absorpt_coefficient_mu    2.309
_exptl_absorpt_correction_T_max  0.769955
_exptl_absorpt_correction_T_min  0.548573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS V2012/1 (Sheldrick, 2012)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       Block
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.063
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         6764
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+7.5514P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.0964
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6303
_reflns_number_total             6764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja403802a_si_016.cif
_cod_data_source_block           BDR211F1
_cod_database_code               4120073
_shelx_estimated_absorpt_t_min   0.571
_shelx_estimated_absorpt_t_max   0.868
_shelxl_version_number           2012-6
_shelx_res_checksum              18014