Systematic Investigation of Thorium(IV)- and Uranium(IV)-Ligand Bonding in Dithiophosphonate, Thioselenophosphinate, and Diselenophosphonate Complexes
Andrew C. Behrle; Charles L. Barnes; Nikolas Kaltsoyannis; Justin R. Walensky; Inorganic Chemistry 52 (2013) 10623–10631; doi:10.1021/ic401642a

data_4336077
_publ_section_title
;
 Systematic Investigation of Thorium(IV)- and Uranium(IV)-Ligand Bonding
 in Dithiophosphonate, Thioselenophosphinate, and Diselenophosphonate
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10623
_journal_page_last               10631
_journal_paper_doi               10.1021/ic401642a
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C32 H40 O8 P4 S8 Th'
_chemical_formula_sum            'C32 H40 O8 P4 S8 Th'
_chemical_formula_weight         1165.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 112.7790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4771(14)
_cell_length_b                   15.8152(14)
_cell_length_c                   18.3267(16)
_cell_measurement_temperature    173(2)
_cell_volume                     4403.2(7)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega 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  0.1690
_diffrn_reflns_av_sigmaI/netI    0.0833
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            50020
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.41
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    3.956
_exptl_absorpt_correction_T_max  0.3006
_exptl_absorpt_correction_T_min  0.0568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Data were corrected for decay and absorption using the program SADABS
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 G\"ottigen, Germany).
;
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.40
_refine_diff_density_max         3.791
_refine_diff_density_min         -1.986
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         10023
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0648P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1233
_reflns_number_gt                7997
_reflns_number_total             10023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401642a_si_001.cif
_cod_data_source_block           complex1
_cod_database_code               4336077