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_4336079
_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         'C52 H48 O P4 S4 Se4 Th'
_chemical_formula_sum            'C52 H48 O P4 S4 Se4 Th'
_chemical_formula_weight         1488.90
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.9080(10)
_cell_angle_beta                 94.7250(10)
_cell_angle_gamma                97.0610(10)
_cell_formula_units_Z            2
_cell_length_a                   11.0735(12)
_cell_length_b                   13.4793(15)
_cell_length_c                   18.856(2)
_cell_measurement_temperature    173(2)
_cell_volume                     2770.6(5)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32426
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    5.621
_exptl_absorpt_correction_T_max  0.5401
_exptl_absorpt_correction_T_min  0.1654
_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    1.785
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.501
_refine_diff_density_min         -1.563
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         12536
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0311
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1127
_reflns_number_gt                11347
_reflns_number_total             12536
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401642a_si_003.cif
_cod_data_source_block           complex6
_cod_original_cell_volume        2770.7(5)
_cod_database_code               4336079