#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/54/4325409.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_4325409
loop_
_publ_author_name
'Richard E. Wilson'
_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 O40 Pu2 S9 na10'
_chemical_formula_weight         1650.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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            4
_cell_length_a                   27.1622(17)
_cell_length_b                   6.8916(4)
_cell_length_c                   17.6460(11)
_cell_measurement_reflns_used    3363
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      3.51
_cell_volume                     3303.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0529
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31772
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         3.51
_exptl_absorpt_coefficient_mu    4.802
_exptl_absorpt_correction_T_max  0.9536
_exptl_absorpt_correction_T_min  0.7000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    3.319
_exptl_crystal_description       block
_exptl_crystal_F_000             3080
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         5.150
_refine_diff_density_min         -2.047
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0490P)²+32.0290P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                3363
_reflns_number_total             4117
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200384h_si_002_2.cif
_cod_data_source_block           sodium
_cod_original_formula_sum        'H8 na10 O40 Pu2 S9'
_cod_database_code               4325409
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'
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
Pu1 Pu 0.601600(8) 0.22263(3) 0.187264(12) 0.01190(9) Uani 1 1 d . . .
S1 S 0.68184(6) 0.1910(2) 0.31040(9) 0.0173(3) Uani 1 1 d . . .
O10 O 0.54324(18) 0.0289(8) 0.2433(3) 0.0295(12) Uani 1 1 d . . .
O3 O 0.68405(18) 0.2738(7) 0.2312(3) 0.0230(10) Uani 1 1 d . . .
O5 O 0.6961(2) 0.3336(8) 0.3661(3) 0.0307(12) Uani 1 1 d . . .
O4 O 0.71431(19) 0.0241(8) 0.3137(3) 0.0305(12) Uani 1 1 d . . .
O9 O 0.55645(18) 0.0598(7) 0.0842(3) 0.0223(10) Uani 1 1 d . . .
O6 O 0.53890(18) 0.3792(7) 0.1157(3) 0.0222(10) Uani 1 1 d . . .
O7 O 0.5309(3) 0.2799(8) -0.0146(3) 0.0394(15) Uani 1 1 d . . .
O8 O 0.4720(2) 0.1754(9) 0.0765(4) 0.0416(16) Uani 1 1 d . . .
O15 O 0.6313(2) -0.0924(7) 0.1760(3) 0.0249(11) Uani 1 1 d . . .
O2 O 0.62880(17) 0.1387(8) 0.3174(3) 0.0212(10) Uani 1 1 d . . .
O13 O 0.6294(3) -0.2810(9) 0.2951(4) 0.0480(18) Uani 1 1 d . . .
O12 O 0.61556(19) -0.4310(7) 0.1743(3) 0.0251(11) Uani 1 1 d . . .
O17 O 0.64824(18) 0.2630(7) 0.0833(3) 0.0221(10) Uani 1 1 d . A .
O11 O 0.4937(2) -0.2179(8) 0.1831(3) 0.0301(12) Uani 1 1 d . . .
O14 O 0.6957(3) -0.3110(10) 0.2003(6) 0.075(3) Uani 1 1 d . . .
O16 O 0.7047(3) 0.3396(10) -0.0160(4) 0.059(2) Uani 1 1 d . A .
O1 O 0.55473(19) 0.4078(8) 0.2813(3) 0.0282(11) Uani 1 1 d . . .
O20A O 0.7103(7) 0.015(3) 0.0567(10) 0.047(3) Uani 0.374(12) 1 d P A 1
O20B O 0.6552(6) 0.064(2) -0.0270(10) 0.076(5) Uani 0.626(12) 1 d P A 1
O21B O 0.7300(4) 0.1405(18) 0.0770(6) 0.047(3) Uani 0.626(12) 1 d P A 2
O21A O 0.8248(12) 0.518(4) -0.0075(18) 0.076(5) Uani 0.374(12) 1 d P . 2
O18 O 0.6096(3) -0.3816(11) -0.0065(4) 0.0539(18) Uani 1 1 d . . .
Na1 na 0.54920(13) -0.2811(4) 0.0854(2) 0.0334(7) Uani 1 1 d . . .
S2 S 0.52289(6) 0.2223(2) 0.06234(10) 0.0184(3) Uani 1 1 d . . .
Na2 na 0.70761(12) -0.3150(5) 0.35645(17) 0.0297(7) Uani 1 1 d . . .
S3 S 0.5000 -0.0995(3) 0.2500 0.0144(4) Uani 1 2 d S . .
Na3 na 0.75153(12) 0.4432(5) 0.1750(2) 0.0364(8) Uani 1 1 d . . .
S4 S 0.64346(8) -0.2798(3) 0.21272(13) 0.0310(4) Uani 1 1 d . . .
Na4 na 0.69670(15) 0.3046(6) 0.5022(2) 0.0480(9) Uani 1 1 d . . .
S5 S 0.68435(7) 0.1826(3) 0.02789(10) 0.0269(4) Uani 1 1 d . . .
Na5 na 0.41858(14) -0.0902(6) 0.1103(2) 0.0499(10) 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
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
H H 0.0000 0.0000 '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
O17 Pu1 O10 144.38(19) . .
O17 Pu1 O15 81.41(18) . .
O10 Pu1 O15 74.5(2) . .
O17 Pu1 O6 85.06(18) . .
O10 Pu1 O6 89.90(19) . .
O15 Pu1 O6 128.80(17) . .
O17 Pu1 O3 73.67(18) . .
O10 Pu1 O3 126.27(18) . .
O15 Pu1 O3 80.85(18) . .
O6 Pu1 O3 140.72(16) . .
O17 Pu1 O12 73.32(18) . 1_565
O10 Pu1 O12 136.07(19) . 1_565
O15 Pu1 O12 148.89(18) . 1_565
O6 Pu1 O12 67.40(17) . 1_565
O3 Pu1 O12 74.92(17) . 1_565
O17 Pu1 O1 141.41(17) . .
O10 Pu1 O1 69.66(19) . .
O15 Pu1 O1 136.41(18) . .
O6 Pu1 O1 75.61(18) . .
O3 Pu1 O1 100.96(18) . .
O12 Pu1 O1 68.48(17) 1_565 .
O17 Pu1 O9 74.60(17) . .
O10 Pu1 O9 73.10(17) . .
O15 Pu1 O9 71.58(17) . .
O6 Pu1 O9 57.22(15) . .
O3 Pu1 O9 140.44(17) . .
O12 Pu1 O9 117.13(16) 1_565 .
O1 Pu1 O9 118.59(18) . .
O17 Pu1 O2 128.08(17) . .
O10 Pu1 O2 70.81(17) . .
O15 Pu1 O2 75.99(17) . .
O6 Pu1 O2 144.15(17) . .
O3 Pu1 O2 57.08(16) . .
O12 Pu1 O2 105.68(17) 1_565 .
O1 Pu1 O2 69.46(17) . .
O9 Pu1 O2 136.48(16) . .
O17 Pu1 S2 78.84(14) . .
O10 Pu1 S2 80.10(13) . .
O15 Pu1 S2 100.33(13) . .
O6 Pu1 S2 28.47(11) . .
O3 Pu1 S2 152.01(12) . .
O12 Pu1 S2 92.39(13) 1_565 .
O1 Pu1 S2 97.18(14) . .
O9 Pu1 S2 28.75(11) . .
O2 Pu1 S2 150.66(11) . .
O17 Pu1 S1 100.69(14) . .
O10 Pu1 S1 98.24(14) . .
O15 Pu1 S1 75.48(13) . .
O6 Pu1 S1 155.72(12) . .
O3 Pu1 S1 28.64(12) . .
O12 Pu1 S1 91.46(13) 1_565 .
O1 Pu1 S1 85.79(13) . .
O9 Pu1 S1 147.06(11) . .
O2 Pu1 S1 28.50(11) . .
S2 Pu1 S1 175.80(4) . .
O5 S1 O4 110.5(3) . .
O5 S1 O2 111.5(3) . .
O4 S1 O2 113.1(3) . .
O5 S1 O3 111.3(3) . .
O4 S1 O3 108.2(3) . .
O2 S1 O3 101.9(3) . .
O5 S1 Pu1 128.4(2) . .
O4 S1 Pu1 120.9(2) . .
O2 S1 Pu1 52.58(18) . .
O3 S1 Pu1 49.45(19) . .
S3 O10 Pu1 158.9(3) . .
S1 O3 Pu1 101.9(2) . .
S2 O9 Pu1 98.8(2) . .
S2 O6 Pu1 102.3(2) . .
S4 O15 Pu1 148.7(3) . .
S1 O2 Pu1 98.9(2) . .
S4 O12 Pu1 137.8(3) . 1_545
S5 O17 Pu1 149.3(3) . .
O7 S2 O8 111.9(4) . .
O7 S2 O9 111.1(3) . .
O8 S2 O9 111.8(3) . .
O7 S2 O6 110.6(3) . .
O8 S2 O6 109.3(3) . .
O9 S2 O6 101.6(3) . .
O7 S2 Pu1 125.1(3) . .
O8 S2 Pu1 122.9(3) . .
O9 S2 Pu1 52.45(19) . .
O6 S2 Pu1 49.18(18) . .
O11 S3 O11 111.2(5) . 3_655
O11 S3 O10 111.5(3) . .
O11 S3 O10 108.1(3) 3_655 .
O11 S3 O10 108.1(3) . 3_655
O11 S3 O10 111.5(3) 3_655 3_655
O10 S3 O10 106.3(5) . 3_655
O14 S4 O12 109.4(4) . .
O14 S4 O15 106.4(4) . .
O12 S4 O15 107.7(3) . .
O14 S4 O13 113.1(5) . .
O12 S4 O13 108.4(4) . .
O15 S4 O13 111.8(4) . .
O21A S5 O16 117.6(18) 8_755 .
O21A S5 O20A 64.7(14) 8_755 .
O16 S5 O20A 127.0(9) . .
O21A S5 O17 120.4(17) 8_755 .
O16 S5 O17 109.0(4) . .
O20A S5 O17 112.8(7) . .
O21A S5 O20B 28.6(12) 8_755 .
O16 S5 O20B 105.4(8) . .
O20A S5 O20B 92.9(13) . .
O17 S5 O20B 106.2(6) . .
O21A S5 O21B 104.9(12) 8_755 .
O16 S5 O21B 97.8(6) . .
O20A S5 O21B 42.1(9) . .
O17 S5 O21B 103.3(4) . .
O20B S5 O21B 133.5(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pu1 O17 2.247(5) .
Pu1 O10 2.296(5) .
Pu1 O15 2.324(5) .
Pu1 O6 2.379(5) .
Pu1 O3 2.396(5) .
Pu1 O12 2.428(5) 1_565
Pu1 O1 2.450(5) .
Pu1 O9 2.464(5) .
Pu1 O2 2.480(5) .
Pu1 S2 3.0709(16) .
Pu1 S1 3.0853(16) .
S1 O5 1.443(5) .
S1 O4 1.451(5) .
S1 O2 1.490(5) .
S1 O3 1.511(5) .
O10 S3 1.475(5) .
O9 S2 1.495(5) .
O6 S2 1.499(5) .
O7 S2 1.432(6) .
O8 S2 1.441(6) .
O15 S4 1.482(5) .
O13 S4 1.503(8) .
O12 S4 1.456(5) .
O12 Pu1 2.428(5) 1_545
O17 S5 1.491(5) .
O11 S3 1.445(5) .
O14 S4 1.452(7) .
O16 S5 1.441(6) .
O20A S5 1.443(17) .
O20B S5 1.494(13) .
O21B S5 1.540(11) .
O21A S5 1.32(2) 8_765
S3 O11 1.445(5) 3_655
S3 O10 1.475(5) 3_655
S5 O21A 1.32(2) 8_755
