Dithio- and Diselenophosphinate Thorium(IV) and Uranium(IV) Complexes: Molecular and Electronic Structures, Spectroscopy, and Transmetalation Reactivity.
Behrle, Andrew C.; Kerridge, Andrew; Walensky, Justin R.; Inorganic chemistry 54 (2015) 11625–11636; doi:10.1021/acs.inorgchem.5b01342

data_4346370
_publ_section_title
;
 Dithio- and Diselenophosphinate Thorium(IV) and Uranium(IV) Complexes:
 Molecular and Electronic Structures, Spectroscopy, and Transmetalation
 Reactivity.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11625
_journal_page_last               11636
_journal_paper_doi               10.1021/acs.inorgchem.5b01342
_journal_volume                  54
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C24 H56 P4 S8 U), C7 H8'
_chemical_formula_sum            'C55 H120 P8 S16 U2'
_chemical_formula_weight         2018.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           34
_space_group_name_Hall           'P 2 -2n'
_space_group_name_H-M_alt        'P n n 2'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      34
_symmetry_space_group_name_H-M   'P n n 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.242(4)
_cell_length_b                   36.150(6)
_cell_length_c                   10.995(2)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.4
_cell_volume                     8443(3)
_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, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            96924
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.432
_diffrn_reflns_theta_min         1.112
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    4.411
_exptl_absorpt_correction_T_max  0.41
_exptl_absorpt_correction_T_min  0.35
_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\"ottingen, Germany).
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       prism
_exptl_crystal_F_000             4040
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_refine_diff_density_max         1.699
_refine_diff_density_min         -2.658
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details
;
 Flack x determined using 7162 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0061(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     922
_refine_ls_number_reflns         19181
_refine_ls_number_restraints     1251
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0335P)^2^+22.0759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.893
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                16737
_reflns_number_total             19181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01342_si_003.cif
_cod_data_source_block           U(S2PiPr2)4
_cod_database_code               4346370
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.405
_shelx_estimated_absorpt_t_max   0.405
_shelx_res_checksum              22256
_shelx_hkl_checksum              81325