#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:45:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179456 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/53/4335397.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4335397
loop_
_publ_author_name
'Jean-Marie Babo'
'Laurent Jouffret'
'Jian Lin'
'Eric M. Villa'
'Thomas E. Albrecht-Schmitt'
_publ_section_title
;
 Synthesis, Structure, and Spectroscopy of Two Ternary Uranium(IV)
 Thiophosphates: UP2S9 and UP2S7 Containing P2S92- and P2S72- Ligands
;
_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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0041P)²+72.1361P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
U U 0.1250 0.1250 0.515311(8) 0.00838(9) Uani 1 2 d S
P P 0.11837(15) 0.31940(8) 0.56908(4) 0.0093(2) Uani 1 1 d .
S1 S 0.1250 0.40262(10) 0.6250 0.0104(3) Uani 1 2 d S
S2 S 0.31747(14) 0.25662(8) 0.55689(4) 0.0099(2) Uani 1 1 d .
S3 S 0.08807(13) 0.40710(8) 0.51967(4) 0.0115(3) Uani 1 1 d .
S4 S -0.03634(14) 0.22491(8) 0.57642(4) 0.0121(3) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
S4 U S4 97.35(6) 14_445 .
S4 U S3 144.35(4) 14_445 30_556
S4 U S3 71.48(4) . 30_556
S4 U S3 71.48(4) 14_445 29_556
S4 U S3 144.34(4) . 29_556
S3 U S3 135.99(5) 30_556 29_556
S4 U S2 104.54(4) 14_445 30_556
S4 U S2 138.59(4) . 30_556
S3 U S2 70.24(3) 30_556 30_556
S3 U S2 76.71(4) 29_556 30_556
S4 U S2 138.58(4) 14_445 29_556
S4 U S2 104.54(4) . 29_556
S3 U S2 76.71(4) 30_556 29_556
S3 U S2 70.24(3) 29_556 29_556
S2 U S2 81.44(5) 30_556 29_556
S4 U S2 69.34(4) 14_445 14_445
S4 U S2 77.67(4) . 14_445
S3 U S2 75.16(4) 30_556 14_445
S3 U S2 125.28(4) 29_556 14_445
S2 U S2 77.86(4) 30_556 14_445
S2 U S2 149.36(4) 29_556 14_445
S4 U S2 77.67(4) 14_445 .
S4 U S2 69.34(4) . .
S3 U S2 125.28(4) 30_556 .
S3 U S2 75.16(4) 29_556 .
S2 U S2 149.36(4) 30_556 .
S2 U S2 77.86(4) 29_556 .
S2 U S2 129.20(5) 14_445 .
S4 U P 36.47(3) 14_445 14_445
S4 U P 99.77(4) . 14_445
S3 U P 110.38(3) 30_556 14_445
S3 U P 90.68(3) 29_556 14_445
S2 U P 79.46(4) 30_556 14_445
S2 U P 155.65(3) 29_556 14_445
S2 U P 37.17(3) 14_445 14_445
S2 U P 112.62(4) . 14_445
S4 U P 99.77(4) 14_445 .
S4 U P 36.46(3) . .
S3 U P 90.68(3) 30_556 .
S3 U P 110.38(3) 29_556 .
S2 U P 155.65(3) 30_556 .
S2 U P 79.46(4) 29_556 .
S2 U P 112.62(4) 14_445 .
S2 U P 37.17(3) . .
P U P 122.57(4) 14_445 .
S4 P S3 117.58(8) . .
S4 P S2 106.44(8) . .
S3 P S2 106.98(7) . .
S4 P S1 111.19(7) . .
S3 P S1 101.33(7) . .
S2 P S1 113.48(7) . .
S4 P U 55.71(5) . .
S3 P U 103.16(6) . .
S2 P U 59.37(4) . .
S1 P U 155.50(6) . .
P S1 P 106.19(9) . 11_455
P S2 U 89.92(5) . 29_556
P S2 U 83.46(5) . .
U S2 U 102.14(4) 29_556 .
P S3 U 92.27(6) . 29_556
P S4 U 87.82(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U S4 2.7860(13) 14_445
U S4 2.7860(13) .
U S3 2.8104(14) 30_556
U S3 2.8104(14) 29_556
U S2 2.8680(13) 30_556
U S2 2.8680(13) 29_556
U S2 2.9182(13) 14_445
U S2 2.9182(13) .
U P 3.3694(14) 14_445
U P 3.3695(14) .
P S4 2.0040(18) .
P S3 2.0156(17) .
P S2 2.0493(18) .
P S1 2.1063(15) .
S1 P 2.1063(15) 11_455
S2 U 2.8680(13) 29_556
S3 U 2.8104(14) 29_556
