Thorium Compounds with Bonds to Sulfur or Selenium: Synthesis, Structure, and Thermolysis.
Rehe, David; Kornienko, Anna Y.; Emge, Thomas J.; Brennan, John G.; Inorganic chemistry 55 (2016) 6961–6967; doi:10.1021/acs.inorgchem.6b00645

data_4347808
_publ_section_title
;
 Thorium Compounds with Bonds to Sulfur or Selenium: Synthesis, Structure,
 and Thermolysis.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6961
_journal_page_last               6967
_journal_paper_doi               10.1021/acs.inorgchem.6b00645
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C39 H15 F20 N3 S4 Th'
_chemical_formula_weight         1265.82
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 103.7361(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9212(10)
_cell_length_b                   16.9796(12)
_cell_length_c                   18.0655(14)
_cell_measurement_reflns_used    4489
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.32
_cell_volume                     4148.1(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_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  0.0395
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11750
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.874
_diffrn_reflns_theta_min         1.925
_exptl_absorpt_coefficient_mu    3.922
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.027
_exptl_crystal_description       lathe
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.932
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4894
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+6.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0795
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4308
_reflns_number_total             4894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00645_si_001.cif
_cod_data_source_block           thscfpy_C2c
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4347808
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.672
_shelx_estimated_absorpt_t_max   0.744
_exptl_absorpt_special_details
; 
Twin Law, Sample 1 of 1 
   Transforms h1.1(1)->h1.2(2) 
    -0.99538 -0.04150  0.01054 
    -0.04788  0.99778  0.04248 
    -0.02060  0.05742 -1.00219 
The relative abundance of the two components was about 3:1 
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_shelx_res_checksum              82591
_shelx_hkl_checksum              15427