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_4120066
_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 Se2'
_chemical_formula_sum            'C60 H74 Se2'
_chemical_formula_weight         953.11
_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                 91.888(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4658(14)
_cell_length_b                   16.1684(15)
_cell_length_c                   20.5084(19)
_cell_measurement_reflns_used    9783
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.63
_cell_measurement_theta_min      2.66
_cell_volume                     5125.5(8)
_computing_cell_refinement       'SAINT (8.27b) (Bruker, 2012)'
_computing_data_collection       'Apex2 (2010-7) (Bruker, 2010)'
_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 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0129
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19548
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.823
_exptl_absorpt_coefficient_mu    1.479
_exptl_absorpt_correction_T_max  0.5553
_exptl_absorpt_correction_T_min  0.4461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2008)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       Block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.710
_exptl_crystal_size_mid          0.520
_exptl_crystal_size_min          0.430
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+3.9560P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0556
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5579
_reflns_number_total             5875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja403802a_si_009.cif
_cod_data_source_block           bdr92fmi
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'refu' changed to 'refU'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               4120066
_shelx_estimated_absorpt_t_min   0.420
_shelx_estimated_absorpt_t_max   0.569
_shelxl_version_number           2012-5
_shelx_res_checksum              99633