Synthesis, Structure, and Spectroscopy of Two Ternary Uranium(IV) Thiophosphates: UP2S9 and UP2S7 Containing P2S92- and P2S72- Ligands
Jean-Marie Babo; Laurent Jouffret; Jian Lin; Eric M. Villa; Thomas E. Albrecht-Schmitt; Inorganic Chemistry 52 (2013) 7747–7751; doi:10.1021/ic400942r

data_4335397
_publ_section_title
;
 Synthesis, Structure, and Spectroscopy of Two Ternary Uranium(IV)
 Thiophosphates: UP2S9 and UP2S7 Containing P2S92- and P2S72- Ligands
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7747
_journal_page_last               7751
_journal_paper_doi               10.1021/ic400942r
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'P0.67 S2.33 U0.33'
_chemical_formula_weight         174.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            48
_cell_length_a                   8.921(3)
_cell_length_b                   15.198(4)
_cell_length_c                   30.104(9)
_cell_measurement_temperature    296(2)
_cell_volume                     4082(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0634
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            11215
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    17.580
_exptl_absorpt_correction_T_max  0.5051
_exptl_absorpt_correction_T_min  0.3767
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    3.414
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.840
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.215
_refine_ls_extinction_coef       0.000016(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         1183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0041P)^2^+72.1361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0363
_refine_ls_wR_factor_ref         0.0384
_reflns_number_gt                1016
_reflns_number_total             1183
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400942r_si_001_1.cif
_cod_data_source_block           save]
_cod_original_cell_volume        4081(2)
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               4335397