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_4120068
_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         'C60 H74 Se3'
_chemical_formula_sum            'C60 H74 Se3'
_chemical_formula_weight         1032.07
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                110.151(3)
_cell_angle_beta                 98.376(2)
_cell_angle_gamma                109.783(2)
_cell_formula_units_Z            1
_cell_length_a                   9.2869(13)
_cell_length_b                   12.812(2)
_cell_length_c                   13.0226(18)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.37
_cell_volume                     1307.1(3)
_computing_cell_refinement       'SAINT (8.27b) (Bruker, 2012)'
_computing_data_collection       'SMART (Version 5.054) (Bruker, 2002)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART1000 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5985
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         1.744
_exptl_absorpt_coefficient_mu    2.147
_exptl_absorpt_correction_T_max  0.6557
_exptl_absorpt_correction_T_min  0.5133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       Plate
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.332
_exptl_crystal_size_mid          0.313
_exptl_crystal_size_min          0.168
_refine_diff_density_max         4.251
_refine_diff_density_min         -1.775
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0605
_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^)+(0.1203P)^2^+0.6726P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1633
_refine_ls_wR_factor_ref         0.1699
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5295
_reflns_number_total             5985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja403802a_si_011.cif
_cod_data_source_block           bdr95f2mi
_cod_database_code               4120068
_shelx_estimated_absorpt_t_min   0.536
_shelx_estimated_absorpt_t_max   0.714
_shelxl_version_number           2012-6
_shelx_res_checksum              35776