#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:35:37 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179068 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/30/4303022.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_4303022
loop_
_publ_author_name
'Geng Bang Jin'
'Eun Sang Choi'
'James A. Ibers'
_publ_contact_author_address
;
        Department of Chemistry
        Northwestern University
        2145 Sheridan Road
        Evanston, IL 60208-3113, USA
;
_publ_contact_author_email       ibers@chem.northwestern.edu
_publ_contact_author_fax         '+1 847 491 2976'
_publ_contact_author_name        'James A. Ibers'
_publ_contact_author_phone       '+1 847 491 5449'
_publ_section_title
;
Reinvestigation of the Uranium(3.5+) Rare-Earth Oxysulfides "(UO)2LnS3"
(Ln = Yb, Y)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8227
_journal_page_last               8232
_journal_paper_doi               10.1021/ic900860c
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'U Yb2 O2 S3'
_chemical_formula_sum            'O2 S3 U Yb2'
_chemical_formula_weight         712.29
_chemical_name_common            'Uranium Ytterbium Oxysulfide'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           139
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m 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            2
_cell_length_a                   3.7762(9)
_cell_length_b                   3.7762(9)
_cell_length_c                   20.691(5)
_cell_measurement_reflns_used    3468
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.57
_cell_measurement_theta_min      1.97
_cell_volume                     295.05(12)
_computing_cell_refinement       'APEX2 v2.0-2 (Bruker, 2005)'
_computing_data_collection       'SMART version 5.054 (Bruker, 2000)'
_computing_data_reduction        'SAINT version 7.23a (Bruker, 2005)'
_computing_molecular_graphics    'CrystalMaker for Windows ver. 2.0.6 (2008)'
_computing_publication_material  'SHELXTL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '0.3 wide w/ exposures'
_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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0160
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            1758
_diffrn_reflns_theta_full        28.57
_diffrn_reflns_theta_max         28.57
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    59.761
_exptl_absorpt_correction_T_max  0.34821
_exptl_absorpt_correction_T_min  0.04411
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'faces indexed'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    8.018
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'square plate'
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.074
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.016
_refine_diff_density_max         3.932
_refine_diff_density_min         -3.413
_refine_diff_density_rms         0.477
_refine_ls_extinction_coef       0.0003(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   1.893
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     14
_refine_ls_number_reflns         148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.893
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0256
_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 
 [1.00000+0.00000exp(0.00(sinθ/λ)²)]/ 
   [σ²(Fo²)+0.0000+0.0000*P+(0.0321P)²+0.0000sinθ/λ] 
 where P = 1.00000Fo² + 0.00000Fc² 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0760
_reflns_number_gt                144
_reflns_number_total             148
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900860c_si_001_2.cif
_cod_data_source_block           Yb
_cod_original_cell_volume        295.04(12)
_cod_database_code               4303022
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.0000 0.0000 0.18835(4) 0.0069(4) Uani 0.50 8 d SP . .
Yb1 Yb 0.0000 0.0000 0.18835(4) 0.0069(4) Uani 0.50 8 d SP . .
Yb2 Yb 0.0000 0.0000 0.5000 0.0078(4) Uani 1 16 d S . .
S1 S 0.0000 0.0000 0.3728(3) 0.0067(9) Uani 1 8 d S . .
S2 S 0.0000 0.0000 0.0000 0.030(3) Uani 1 16 d S . .
O1 O 0.0000 0.5000 0.2500 0.011(3) Uani 1 8 d S . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
Yb Yb -0.3850 5.5486 '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
_geom_angle_publ_flag
O1 U1 O1 71.737(17) 25 . ?
O1 U1 O1 111.91(4) 25 25_455 ?
O1 U1 O1 71.737(17) . 25_455 ?
O1 U1 O1 71.737(17) 25 1_545 ?
O1 U1 O1 111.91(4) . 1_545 ?
O1 U1 O1 71.737(17) 25_455 1_545 ?
O1 U1 S1 140.29(4) 25 25_445 ?
O1 U1 S1 140.29(4) . 25_445 ?
O1 U1 S1 73.17(8) 25_455 25_445 ?
O1 U1 S1 73.17(8) 1_545 25_445 ?
O1 U1 S1 73.17(8) 25 25 ?
O1 U1 S1 73.17(8) . 25 ?
O1 U1 S1 140.29(4) 25_455 25 ?
O1 U1 S1 140.29(4) 1_545 25 ?
S1 U1 S1 129.3(2) 25_445 25 ?
O1 U1 S1 140.29(4) 25 25_455 ?
O1 U1 S1 73.17(8) . 25_455 ?
O1 U1 S1 73.17(8) 25_455 25_455 ?
O1 U1 S1 140.29(4) 1_545 25_455 ?
S1 U1 S1 79.42(8) 25_445 25_455 ?
S1 U1 S1 79.42(8) 25 25_455 ?
O1 U1 S1 73.17(8) 25 25_545 ?
O1 U1 S1 140.29(4) . 25_545 ?
O1 U1 S1 140.29(4) 25_455 25_545 ?
O1 U1 S1 73.17(8) 1_545 25_545 ?
S1 U1 S1 79.42(8) 25_445 25_545 ?
S1 U1 S1 79.42(8) 25 25_545 ?
S1 U1 S1 129.3(2) 25_455 25_545 ?
O1 U1 Yb1 35.868(9) 25 25 ?
O1 U1 Yb1 35.868(9) . 25 ?
O1 U1 Yb1 92.12(3) 25_455 25 ?
O1 U1 Yb1 92.12(3) 1_545 25 ?
S1 U1 Yb1 161.67(10) 25_445 25 ?
S1 U1 Yb1 69.06(10) 25 25 ?
S1 U1 Yb1 107.22(6) 25_455 25 ?
S1 U1 Yb1 107.22(6) 25_545 25 ?
O1 U1 U1 35.868(9) 25 25 ?
O1 U1 U1 35.868(9) . 25 ?
O1 U1 U1 92.12(3) 25_455 25 ?
O1 U1 U1 92.12(3) 1_545 25 ?
S1 U1 U1 161.67(10) 25_445 25 ?
S1 U1 U1 69.06(10) 25 25 ?
S1 U1 U1 107.22(6) 25_455 25 ?
S1 U1 U1 107.22(6) 25_545 25 ?
Yb1 U1 U1 0.000(17) 25 25 ?
O1 U1 U1 35.868(9) 25 25_545 ?
O1 U1 U1 92.12(3) . 25_545 ?
O1 U1 U1 92.12(3) 25_455 25_545 ?
O1 U1 U1 35.868(9) 1_545 25_545 ?
S1 U1 U1 107.22(6) 25_445 25_545 ?
S1 U1 U1 107.22(6) 25 25_545 ?
S1 U1 U1 161.67(10) 25_455 25_545 ?
S1 U1 U1 69.06(10) 25_545 25_545 ?
Yb1 U1 U1 61.50(2) 25 25_545 ?
U1 U1 U1 61.50(2) 25 25_545 ?
O1 U1 U1 92.12(3) 25 25_455 ?
O1 U1 U1 35.868(9) . 25_455 ?
O1 U1 U1 35.868(9) 25_455 25_455 ?
O1 U1 U1 92.12(3) 1_545 25_455 ?
S1 U1 U1 107.22(6) 25_445 25_455 ?
S1 U1 U1 107.22(6) 25 25_455 ?
S1 U1 U1 69.06(10) 25_455 25_455 ?
S1 U1 U1 161.67(10) 25_545 25_455 ?
Yb1 U1 U1 61.50(2) 25 25_455 ?
U1 U1 U1 61.50(2) 25 25_455 ?
U1 U1 U1 92.61(4) 25_545 25_455 ?
S1 Yb2 S1 180.0 . 17_556 ?
S1 Yb2 S2 90.0 . 9 ?
S1 Yb2 S2 90.0 17_556 9 ?
S1 Yb2 S2 90.0 . 9_445 ?
S1 Yb2 S2 90.0 17_556 9_445 ?
S2 Yb2 S2 180.0 9 9_445 ?
S1 Yb2 S2 90.0 . 9_455 ?
S1 Yb2 S2 90.0 17_556 9_455 ?
S2 Yb2 S2 90.0 9 9_455 ?
S2 Yb2 S2 90.0 9_445 9_455 ?
S1 Yb2 S2 90.0 . 9_545 ?
S1 Yb2 S2 90.0 17_556 9_545 ?
S2 Yb2 S2 90.0 9 9_545 ?
S2 Yb2 S2 90.0 9_445 9_545 ?
S2 Yb2 S2 180.0 9_455 9_545 ?
S1 Yb2 Yb2 90.0 . 1_455 ?
S1 Yb2 Yb2 90.0 17_556 1_455 ?
S2 Yb2 Yb2 135.0 9 1_455 ?
S2 Yb2 Yb2 45.0 9_445 1_455 ?
S2 Yb2 Yb2 45.0 9_455 1_455 ?
S2 Yb2 Yb2 135.0 9_545 1_455 ?
S1 Yb2 Yb2 90.0 . 1_655 ?
S1 Yb2 Yb2 90.0 17_556 1_655 ?
S2 Yb2 Yb2 45.0 9 1_655 ?
S2 Yb2 Yb2 135.0 9_445 1_655 ?
S2 Yb2 Yb2 135.0 9_455 1_655 ?
S2 Yb2 Yb2 45.0 9_545 1_655 ?
Yb2 Yb2 Yb2 180.0 1_455 1_655 ?
S1 Yb2 Yb2 90.0 . 1_545 ?
S1 Yb2 Yb2 90.0 17_556 1_545 ?
S2 Yb2 Yb2 135.0 9 1_545 ?
S2 Yb2 Yb2 45.0 9_445 1_545 ?
S2 Yb2 Yb2 135.0 9_455 1_545 ?
S2 Yb2 Yb2 45.0 9_545 1_545 ?
Yb2 Yb2 Yb2 90.0 1_455 1_545 ?
Yb2 Yb2 Yb2 90.0 1_655 1_545 ?
S1 Yb2 Yb2 90.0 . 1_565 ?
S1 Yb2 Yb2 90.0 17_556 1_565 ?
S2 Yb2 Yb2 45.0 9 1_565 ?
S2 Yb2 Yb2 135.0 9_445 1_565 ?
S2 Yb2 Yb2 45.0 9_455 1_565 ?
S2 Yb2 Yb2 135.0 9_545 1_565 ?
Yb2 Yb2 Yb2 90.0 1_455 1_565 ?
Yb2 Yb2 Yb2 90.0 1_655 1_565 ?
Yb2 Yb2 Yb2 180.0 1_545 1_565 ?
Yb2 S1 Yb1 115.37(10) . 25_445 ?
Yb2 S1 U1 115.37(10) . 25_445 ?
Yb1 S1 U1 0.00(3) 25_445 25_445 ?
Yb2 S1 Yb1 115.37(10) . 25 ?
Yb1 S1 Yb1 129.3(2) 25_445 25 ?
U1 S1 Yb1 129.3(2) 25_445 25 ?
Yb2 S1 U1 115.37(10) . 25 ?
Yb1 S1 U1 129.3(2) 25_445 25 ?
U1 S1 U1 129.3(2) 25_445 25 ?
Yb1 S1 U1 0.00(3) 25 25 ?
Yb2 S1 U1 115.37(10) . 25_455 ?
Yb1 S1 U1 79.42(8) 25_445 25_455 ?
U1 S1 U1 79.42(8) 25_445 25_455 ?
Yb1 S1 U1 79.42(8) 25 25_455 ?
U1 S1 U1 79.42(8) 25 25_455 ?
Yb2 S1 U1 115.37(10) . 25_545 ?
Yb1 S1 U1 79.42(8) 25_445 25_545 ?
U1 S1 U1 79.42(8) 25_445 25_545 ?
Yb1 S1 U1 79.42(8) 25 25_545 ?
U1 S1 U1 79.42(8) 25 25_545 ?
U1 S1 U1 129.3(2) 25_455 25_545 ?
Yb2 S1 Yb1 115.37(10) . 25_545 ?
Yb1 S1 Yb1 79.42(8) 25_445 25_545 ?
U1 S1 Yb1 79.42(8) 25_445 25_545 ?
Yb1 S1 Yb1 79.42(8) 25 25_545 ?
U1 S1 Yb1 79.42(8) 25 25_545 ?
U1 S1 Yb1 129.3(2) 25_455 25_545 ?
U1 S1 Yb1 0.00(3) 25_545 25_545 ?
Yb2 S1 Yb1 115.37(10) . 25_455 ?
Yb1 S1 Yb1 79.42(8) 25_445 25_455 ?
U1 S1 Yb1 79.42(8) 25_445 25_455 ?
Yb1 S1 Yb1 79.42(8) 25 25_455 ?
U1 S1 Yb1 79.42(8) 25 25_455 ?
U1 S1 Yb1 0.00(3) 25_455 25_455 ?
U1 S1 Yb1 129.3(2) 25_545 25_455 ?
Yb1 S1 Yb1 129.3(2) 25_545 25_455 ?
Yb2 S2 Yb2 180.0 9_554 9_444 ?
Yb2 S2 Yb2 90.0 9_554 9_544 ?
Yb2 S2 Yb2 90.0 9_444 9_544 ?
Yb2 S2 Yb2 90.0 9_554 9_454 ?
Yb2 S2 Yb2 90.0 9_444 9_454 ?
Yb2 S2 Yb2 180.0 9_544 9_454 ?
U1 O1 Yb1 108.264(17) . 25 ?
U1 O1 U1 108.264(17) . 25 ?
Yb1 O1 U1 0.00(3) 25 25 ?
U1 O1 U1 111.91(4) . 1_565 ?
Yb1 O1 U1 108.265(17) 25 1_565 ?
U1 O1 U1 108.265(17) 25 1_565 ?
U1 O1 U1 108.264(17) . 25_455 ?
Yb1 O1 U1 111.91(4) 25 25_455 ?
U1 O1 U1 111.91(4) 25 25_455 ?
U1 O1 U1 108.265(17) 1_565 25_455 ?
U1 O1 Yb1 111.91(4) . 1_565 ?
Yb1 O1 Yb1 108.265(17) 25 1_565 ?
U1 O1 Yb1 108.265(17) 25 1_565 ?
U1 O1 Yb1 0.00(3) 1_565 1_565 ?
U1 O1 Yb1 108.265(17) 25_455 1_565 ?
U1 O1 Yb1 108.264(17) . 25_455 ?
Yb1 O1 Yb1 111.91(4) 25 25_455 ?
U1 O1 Yb1 111.91(4) 25 25_455 ?
U1 O1 Yb1 108.265(17) 1_565 25_455 ?
U1 O1 Yb1 0.00(3) 25_455 25_455 ?
Yb1 O1 Yb1 108.265(17) 1_565 25_455 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.2786(6) 25 ?
U1 O1 2.2786(6) . ?
U1 O1 2.2786(6) 25_455 ?
U1 O1 2.2786(6) 1_545 ?
U1 S1 2.955(2) 25_445 ?
U1 S1 2.955(2) 25 ?
U1 S1 2.955(2) 25_455 ?
U1 S1 2.955(2) 25_545 ?
U1 Yb1 3.6931(12) 25 ?
U1 U1 3.6931(12) 25 ?
U1 U1 3.6931(12) 25_545 ?
U1 U1 3.6931(12) 25_455 ?
Yb2 S1 2.631(5) . ?
Yb2 S1 2.631(5) 17_556 ?
Yb2 S2 2.6702(6) 9 ?
Yb2 S2 2.6702(6) 9_445 ?
Yb2 S2 2.6702(6) 9_455 ?
Yb2 S2 2.6702(6) 9_545 ?
Yb2 Yb2 3.7762(9) 1_455 ?
Yb2 Yb2 3.7762(9) 1_655 ?
Yb2 Yb2 3.7762(9) 1_545 ?
Yb2 Yb2 3.7762(9) 1_565 ?
S1 Yb1 2.955(2) 25_445 ?
S1 U1 2.955(2) 25_445 ?
S1 Yb1 2.955(2) 25 ?
S1 U1 2.955(2) 25 ?
S1 U1 2.955(2) 25_455 ?
S1 U1 2.955(2) 25_545 ?
S1 Yb1 2.955(2) 25_545 ?
S1 Yb1 2.955(2) 25_455 ?
S2 Yb2 2.6702(6) 9_554 ?
S2 Yb2 2.6702(6) 9_444 ?
S2 Yb2 2.6702(6) 9_544 ?
S2 Yb2 2.6702(6) 9_454 ?
O1 Yb1 2.2786(6) 25 ?
O1 U1 2.2786(6) 25 ?
O1 U1 2.2786(6) 1_565 ?
O1 U1 2.2786(6) 25_455 ?
O1 Yb1 2.2786(6) 1_565 ?
O1 Yb1 2.2786(6) 25_455 ?
