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_4120064
_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         'C48 H50 Ge S2'
_chemical_formula_sum            'C48 H50 Ge S2'
_chemical_formula_weight         763.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 95.412(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5253(7)
_cell_length_b                   18.4563(10)
_cell_length_c                   16.0363(9)
_cell_measurement_reflns_used    9802
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.55
_cell_volume                     3985.2(4)
_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 0.997
_diffrn_measurement_device_type  'Bruker Duo 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  0.0325
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33794
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_min         2.549
_exptl_absorpt_coefficient_mu    0.906
_exptl_absorpt_correction_T_max  0.7933
_exptl_absorpt_correction_T_min  0.5232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'
_exptl_crystal_colour            'Pale Yellow'
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    none
_exptl_crystal_description       Rod
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.770
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         9129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0366P)^2^+2.6991P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0837
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7720
_reflns_number_total             9129
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja403802a_si_007.cif
_cod_data_source_block           BDR89FMI
_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               4120064
_shelx_estimated_absorpt_t_min   0.542
_shelx_estimated_absorpt_t_max   0.891
_shelxl_version_number           2012-5
_shelx_res_checksum              92387