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_4120059
_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         'C84 H122 S2 Sn'
_chemical_formula_sum            'C84 H122 S2 Sn'
_chemical_formula_weight         1314.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.0570(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7861(8)
_cell_length_b                   25.4670(11)
_cell_length_c                   16.9855(7)
_cell_measurement_reflns_used    1530
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.32
_cell_measurement_theta_min      2.66
_cell_volume                     7650.8(6)
_computing_cell_refinement       'SAINT (8.18C) (Bruker, 2012)'
_computing_data_collection       'Apex2 (2012.2-0) (Bruker, 2012)'
_computing_data_reduction        'SAINT (8.18C) (Bruker, 2012)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6928
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  0.9463
_exptl_absorpt_correction_T_min  0.8572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS V2008/4 (Sheldrick, 2008)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       Rod
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         6928
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0296P)^2^+8.5855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0823
_reflns_number_gt                5480
_reflns_number_total             6928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja403802a_si_002.cif
_cod_data_source_block           bdr62tw41
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4120059