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_4335398
_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 S3 U0.33'
_chemical_formula_weight         196.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           132
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4c 2c'
_symmetry_space_group_name_H-M   'P 42/m c m'
_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            6
_cell_length_a                   7.7621(11)
_cell_length_b                   7.7621(11)
_cell_length_c                   9.691(3)
_cell_measurement_temperature    296(2)
_cell_volume                     583.9(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6214
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    15.725
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    3.347
_exptl_crystal_F_000             532
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.0007(3)
_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   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0139
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0086P)^2^+0.4129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0245
_refine_ls_wR_factor_ref         0.0259
_reflns_number_gt                346
_reflns_number_total             401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400942r_si_001_2.cif
_cod_data_source_block           UP2S9
_cod_original_sg_symbol_H-M      'P 42/m  c m'
_cod_database_code               4335398