#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:59:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179357 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/54/4325408.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_4325408
loop_
_publ_author_name
'Richard E. Wilson'
_publ_contact_author_address
;CSE/200 
Argonne national Laboratory
9600 S. Cass Avenue
Argonne, IL 60439
;
_publ_contact_author_email       rewilson@anl.gov
_publ_contact_author_name        'Richard E. Wilson'
_publ_contact_author_phone       630-252-1288
_publ_section_title
;
 Structural Periodicity in Plutonium(IV) Sulfates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5663
_journal_page_last               5670
_journal_paper_doi               10.1021/ic200384h
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'H8 O12 Pu S2'
_chemical_formula_weight         506.18
_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   none
_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            8
_cell_length_a                   5.6011(7)
_cell_length_b                   12.0323(17)
_cell_length_c                   26.525(4)
_cell_measurement_reflns_used    869
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.62
_cell_measurement_theta_min      4.09
_cell_volume                     1787.6(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       '0.3 deg 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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            7093
_diffrn_reflns_theta_full        33.62
_diffrn_reflns_theta_max         33.62
_diffrn_reflns_theta_min         4.09
_exptl_absorpt_coefficient_mu    7.903
_exptl_absorpt_correction_T_max  0.5705
_exptl_absorpt_correction_T_min  0.3304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.762
_exptl_crystal_description       block
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.925
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.305
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         869
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0189
_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/[σ²(Fo²)+(0.0319P)²+1.8186P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0487
_refine_ls_wR_factor_ref         0.0495
_reflns_number_gt                812
_reflns_number_total             869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200384h_si_002_1.cif
_cod_data_source_block           fddd
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               4325408
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
Pu1 Pu 0.1250 0.6250 0.1250 0.00586(7) Uani 1 4 d S
S1 S -0.1250 0.3750 0.18134(4) 0.00774(16) Uani 1 2 d S
O1 O -0.1054(3) 0.6842(2) 0.19404(8) 0.0103(4) Uani 1 1 d .
O2 O -0.0953(3) 0.47340(19) 0.14813(9) 0.0111(4) Uani 1 1 d .
O3 O 0.0879(4) 0.3578(2) 0.21221(9) 0.0120(4) Uani 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pu1 0.00598(10) 0.00507(10) 0.00653(10) 0.000 0.000 0.000
S1 0.0084(4) 0.0071(4) 0.0077(4) 0.000 0.000 -0.0008(3)
O1 0.0096(8) 0.0100(9) 0.0112(9) 0.0041(7) 0.0023(6) -0.0015(6)
O2 0.0118(8) 0.0094(9) 0.0120(9) 0.0029(7) 0.0002(7) -0.0023(7)
O3 0.0119(9) 0.0125(9) 0.0115(9) -0.0006(8) -0.0033(8) 0.0031(7)
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'
H H 0.0000 0.0000 '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'
Pu Pu -9.4100 4.3056 '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
O2 Pu1 O2 148.86(12) 14_455 .
O2 Pu1 O2 114.68(11) 14_455 11_454
O2 Pu1 O2 74.13(11) . 11_454
O2 Pu1 O2 74.13(11) 14_455 8_554
O2 Pu1 O2 114.68(11) . 8_554
O2 Pu1 O2 148.86(12) 11_454 8_554
O2 Pu1 O1 138.34(8) 14_455 8_554
O2 Pu1 O1 70.80(8) . 8_554
O2 Pu1 O1 81.11(7) 11_454 8_554
O2 Pu1 O1 74.71(8) 8_554 8_554
O2 Pu1 O1 74.71(8) 14_455 14_455
O2 Pu1 O1 81.11(7) . 14_455
O2 Pu1 O1 70.80(8) 11_454 14_455
O2 Pu1 O1 138.34(8) 8_554 14_455
O1 Pu1 O1 144.73(11) 8_554 14_455
O2 Pu1 O1 81.11(7) 14_455 .
O2 Pu1 O1 74.71(8) . .
O2 Pu1 O1 138.34(8) 11_454 .
O2 Pu1 O1 70.80(8) 8_554 .
O1 Pu1 O1 113.42(10) 8_554 .
O1 Pu1 O1 77.65(10) 14_455 .
O2 Pu1 O1 70.80(8) 14_455 11_454
O2 Pu1 O1 138.34(8) . 11_454
O2 Pu1 O1 74.71(8) 11_454 11_454
O2 Pu1 O1 81.11(7) 8_554 11_454
O1 Pu1 O1 77.65(10) 8_554 11_454
O1 Pu1 O1 113.42(10) 14_455 11_454
O1 Pu1 O1 144.73(11) . 11_454
O3 S1 O3 111.8(2) . 2_455
O3 S1 O2 108.12(13) . 2_455
O3 S1 O2 110.71(13) 2_455 2_455
O3 S1 O2 110.71(13) . .
O3 S1 O2 108.12(13) 2_455 .
O2 S1 O2 107.25(19) 2_455 .
S1 O2 Pu1 148.86(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pu1 O2 2.286(2) 14_455
Pu1 O2 2.286(2) .
Pu1 O2 2.286(2) 11_454
Pu1 O2 2.286(2) 8_554
Pu1 O1 2.351(2) 8_554
Pu1 O1 2.351(2) 14_455
Pu1 O1 2.351(2) .
Pu1 O1 2.351(2) 11_454
S1 O3 1.461(2) .
S1 O3 1.461(2) 2_455
S1 O2 1.485(2) 2_455
S1 O2 1.485(2) .
