#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:10:58 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179097 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/59/4305991.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_4305991
loop_
_publ_author_name
'Richard E. Wilson'
'S. Skanthakumar'
'Karah E. Knope'
'Christopher L. Cahill'
'L. Soderholm'
_publ_section_title
;
An Open-Framework Thorium Sulfate Hydrate with 11.5 Å Voids
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9321
_journal_page_last               9326
_journal_paper_doi               10.1021/ic800931f
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'O30 S6 Th3, O'
_chemical_formula_sum            'O31 S6 Th3'
_chemical_formula_weight         1384.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           137
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4ac 2a'
_symmetry_space_group_name_H-M   'P 42/n m c :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                   25.890(4)
_cell_length_b                   25.890(4)
_cell_length_c                   9.0800(18)
_cell_measurement_reflns_used    69106
_cell_measurement_temperature    295
_cell_measurement_theta_max      29.43
_cell_measurement_theta_min      3.87
_cell_volume                     6086.3(18)
_computing_cell_refinement       'APEX II, SAINT+ (Bruker, 2004)'
_computing_data_collection       'APEX II (Bruker, 2004)'
_computing_data_reduction        'SAINT+ (Bruker, 2004)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXCIF-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       '0.3 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  0.1045
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            69106
_diffrn_reflns_theta_full        29.43
_diffrn_reflns_theta_max         29.43
_diffrn_reflns_theta_min         3.87
_exptl_absorpt_coefficient_mu    15.142
_exptl_absorpt_correction_T_max  0.6193
_exptl_absorpt_correction_T_min  0.3942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.022
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needle
_exptl_crystal_F_000             4912
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.261
_refine_diff_density_min         -2.519
_refine_diff_density_rms         0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         4245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0341
_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)+(0.0458P)²+69.9370P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0990
_reflns_number_gt                3044
_reflns_number_total             4245
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800931f_si_002.cif
_cod_data_source_block           final
_cod_original_cell_volume        6086.3(17)
_cod_original_sg_symbol_H-M      'P 42/n m c'
_cod_database_code               4305991
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z+1/2'
'y, -x+1/2, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y, -z'
'y+1/2, x+1/2, -z+1/2'
'-y, -x, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z-1/2'
'-y, x-1/2, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y, z'
'-y-1/2, -x-1/2, z-1/2'
'y, x, 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
Th1 Th 0.7500 0.600051(15) 0.01571(5) 0.01031(10) Uani 1 2 d S . .
Th2 Th 0.887494(10) 0.525978(10) 0.47635(3) 0.00970(9) Uani 1 1 d . . .
S4 S 0.99081(7) 0.49081(7) 0.7500 0.0097(5) Uani 1 2 d S . .
S2 S 0.86714(7) 0.64526(7) 0.2439(2) 0.0120(4) Uani 1 1 d . . .
S1 S 0.86663(7) 0.51364(7) 0.0626(2) 0.0111(4) Uani 1 1 d . . .
S3 S 0.7500 0.51810(12) 0.3532(4) 0.0163(6) Uani 1 2 d S . .
O1 O 0.8172(2) 0.5391(2) 0.0191(8) 0.0225(14) Uani 1 1 d . . .
O9 O 0.7500 0.5652(4) 0.2615(11) 0.022(2) Uani 1 2 d S . .
O2 O 0.8717(3) 0.4666(3) -0.0244(8) 0.0266(15) Uani 1 1 d . . .
O10 O 0.7958(2) 0.5195(3) 0.4491(8) 0.0226(14) Uani 1 1 d . . .
OW3 O 0.8385(3) 0.4793(3) 0.6874(8) 0.0276(16) Uani 1 1 d . . .
O12 O 0.9423(2) 0.4921(3) 0.6666(7) 0.0229(14) Uani 1 1 d . . .
O5 O 0.8635(2) 0.6928(2) 0.3293(7) 0.0205(14) Uani 1 1 d . . .
OW1 O 0.7500 0.5443(4) -0.2148(12) 0.028(2) Uani 1 2 d S . .
O3 O 0.9095(3) 0.5483(3) 0.0328(9) 0.0333(18) Uani 1 1 d . . .
OW4 O 0.8878(3) 0.4309(3) 0.4379(10) 0.0318(17) Uani 1 1 d . . .
O4 O 0.8655(2) 0.5012(3) 0.2192(7) 0.0219(14) Uani 1 1 d . . .
O13 O 1.0342(2) 0.4936(3) 0.6490(8) 0.0257(15) Uani 1 1 d . . .
O6 O 0.8230(3) 0.6410(3) 0.1478(8) 0.0276(16) Uani 1 1 d . . .
O7 O 0.9153(3) 0.6478(3) 0.1580(9) 0.0357(18) Uani 1 1 d . . .
O8 O 0.8682(3) 0.6013(3) 0.3416(9) 0.0323(17) Uani 1 1 d . . .
O11 O 0.7500 0.4723(4) 0.2657(13) 0.034(2) Uani 1 2 d S . .
OW2 O 0.7500 0.6958(4) 0.0195(15) 0.043(3) Uani 1 2 d S . .
O18 O 0.6546(6) 0.7500 -0.0090(18) 0.062(4) Uani 1 2 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'
Th Th -7.2400 8.8979 '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 Th1 O1 95.6(3) 14_755 . ?
O1 Th1 O9 74.7(2) 14_755 . ?
O1 Th1 O9 74.7(2) . . ?
O1 Th1 O5 79.6(2) 14_755 4_564 ?
O1 Th1 O5 136.0(2) . 4_564 ?
O9 Th1 O5 142.05(16) . 4_564 ?
O1 Th1 O5 136.0(2) 14_755 15_775 ?
O1 Th1 O5 79.6(2) . 15_775 ?
O9 Th1 O5 142.05(16) . 15_775 ?
O5 Th1 O5 74.7(3) 4_564 15_775 ?
O1 Th1 O6 147.8(2) 14_755 . ?
O1 Th1 O6 73.5(2) . . ?
O9 Th1 O6 73.2(2) . . ?
O5 Th1 O6 129.3(2) 4_564 . ?
O5 Th1 O6 73.0(2) 15_775 . ?
O1 Th1 O6 73.5(2) 14_755 14_755 ?
O1 Th1 O6 147.8(2) . 14_755 ?
O9 Th1 O6 73.2(2) . 14_755 ?
O5 Th1 O6 73.0(2) 4_564 14_755 ?
O5 Th1 O6 129.3(2) 15_775 14_755 ?
O6 Th1 O6 99.5(4) . 14_755 ?
O1 Th1 OW2 132.15(16) 14_755 . ?
O1 Th1 OW2 132.15(16) . . ?
O9 Th1 OW2 111.2(4) . . ?
O5 Th1 OW2 67.8(3) 4_564 . ?
O5 Th1 OW2 67.8(3) 15_775 . ?
O6 Th1 OW2 64.2(2) . . ?
O6 Th1 OW2 64.2(2) 14_755 . ?
O1 Th1 OW1 68.3(2) 14_755 . ?
O1 Th1 OW1 68.3(2) . . ?
O9 Th1 OW1 123.4(3) . . ?
O5 Th1 OW1 69.4(2) 4_564 . ?
O5 Th1 OW1 69.4(2) 15_775 . ?
O6 Th1 OW1 129.92(19) . . ?
O6 Th1 OW1 129.92(19) 14_755 . ?
OW2 Th1 OW1 125.4(4) . . ?
O8 Th2 O13 96.2(3) . 9_766 ?
O8 Th2 O10 78.1(2) . . ?
O13 Th2 O10 141.3(2) 9_766 . ?
O8 Th2 O12 143.2(2) . . ?
O13 Th2 O12 76.3(2) 9_766 . ?
O10 Th2 O12 129.4(2) . . ?
O8 Th2 O3 71.5(3) . 15_776 ?
O13 Th2 O3 70.3(3) 9_766 15_776 ?
O10 Th2 O3 139.0(2) . 15_776 ?
O12 Th2 O3 72.1(2) . 15_776 ?
O8 Th2 O7 75.8(3) . 15_776 ?
O13 Th2 O7 141.3(3) 9_766 15_776 ?
O10 Th2 O7 75.0(3) . 15_776 ?
O12 Th2 O7 87.8(3) . 15_776 ?
O3 Th2 O7 71.4(3) 15_776 15_776 ?
O8 Th2 OW4 138.4(3) . . ?
O13 Th2 OW4 73.7(3) 9_766 . ?
O10 Th2 OW4 85.3(2) . . ?
O12 Th2 OW4 74.8(2) . . ?
O3 Th2 OW4 135.5(2) 15_776 . ?
O7 Th2 OW4 135.9(3) 15_776 . ?
O8 Th2 O4 71.1(3) . . ?
O13 Th2 O4 72.0(2) 9_766 . ?
O10 Th2 O4 70.0(2) . . ?
O12 Th2 O4 135.8(2) . . ?
O3 Th2 O4 122.4(3) 15_776 . ?
O7 Th2 O4 135.6(3) 15_776 . ?
OW4 Th2 O4 67.3(3) . . ?
O8 Th2 OW3 131.7(3) . . ?
O13 Th2 OW3 132.1(2) 9_766 . ?
O10 Th2 OW3 63.8(2) . . ?
O12 Th2 OW3 65.7(2) . . ?
O3 Th2 OW3 120.1(3) 15_776 . ?
O7 Th2 OW3 66.8(2) 15_776 . ?
OW4 Th2 OW3 69.2(3) . . ?
O4 Th2 OW3 117.5(2) . . ?
O13 S4 O13 108.8(6) 7_546 . ?
O13 S4 O12 110.6(4) 7_546 . ?
O13 S4 O12 109.6(4) . . ?
O13 S4 O12 109.6(4) 7_546 7_546 ?
O13 S4 O12 110.6(4) . 7_546 ?
O12 S4 O12 107.8(5) . 7_546 ?
O8 S2 O6 109.1(4) . . ?
O8 S2 O5 110.0(4) . . ?
O6 S2 O5 109.6(4) . . ?
O8 S2 O7 110.1(5) . . ?
O6 S2 O7 110.7(5) . . ?
O5 S2 O7 107.4(4) . . ?
O3 S1 O4 109.4(4) . . ?
O3 S1 O2 110.3(5) . . ?
O4 S1 O2 110.3(4) . . ?
O3 S1 O1 109.4(4) . . ?
O4 S1 O1 109.8(4) . . ?
O2 S1 O1 107.6(4) . . ?
O11 S3 O9 111.8(7) . . ?
O11 S3 O10 110.5(4) . . ?
O9 S3 O10 108.3(4) . . ?
O11 S3 O10 110.5(4) . 14_755 ?
O9 S3 O10 108.3(4) . 14_755 ?
O10 S3 O10 107.3(6) . 14_755 ?
S1 O1 Th1 159.3(4) . . ?
S3 O9 Th1 146.4(6) . . ?
S3 O10 Th2 149.6(4) . . ?
S4 O12 Th2 152.4(4) . . ?
S2 O5 Th1 148.9(4) . 3_655 ?
S1 O3 Th2 174.0(5) . 15_775 ?
S1 O4 Th2 148.7(4) . . ?
S4 O13 Th2 161.9(5) . 9_766 ?
S2 O6 Th1 158.5(4) . . ?
S2 O7 Th2 151.1(5) . 15_775 ?
S2 O8 Th2 167.5(5) . . ?
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
Th1 O1 2.349(6) 14_755 ?
Th1 O1 2.349(6) . ?
Th1 O9 2.408(10) . ?
Th1 O5 2.439(6) 4_564 ?
Th1 O5 2.439(6) 15_775 ?
Th1 O6 2.476(6) . ?
Th1 O6 2.476(6) 14_755 ?
Th1 OW2 2.479(10) . ?
Th1 OW1 2.542(10) . ?
Th2 O8 2.355(7) . ?
Th2 O13 2.381(6) 9_766 ?
Th2 O10 2.393(6) . ?
Th2 O12 2.402(6) . ?
Th2 O3 2.411(7) 15_776 ?
Th2 O7 2.422(7) 15_776 ?
Th2 OW4 2.486(7) . ?
Th2 O4 2.487(7) . ?
Th2 OW3 2.597(7) . ?
S4 O13 1.451(6) 7_546 ?
S4 O13 1.451(6) . ?
S4 O12 1.466(6) . ?
S4 O12 1.466(6) 7_546 ?
S2 O8 1.444(7) . ?
S2 O6 1.443(6) . ?
S2 O5 1.458(6) . ?
S2 O7 1.472(7) . ?
S1 O3 1.453(7) . ?
S1 O4 1.458(7) . ?
S1 O2 1.457(7) . ?
S1 O1 1.493(6) . ?
S3 O11 1.426(11) . ?
S3 O9 1.475(10) . ?
S3 O10 1.471(7) . ?
S3 O10 1.471(7) 14_755 ?
O5 Th1 2.439(6) 3_655 ?
O3 Th2 2.411(7) 15_775 ?
O13 Th2 2.381(6) 9_766 ?
O7 Th2 2.422(7) 15_775 ?
