#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/02/4330265.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_4330265
loop_
_publ_author_name
'David D. Schnaars'
'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
;
 Uranium(IV) Sulfates: Investigating Structural Periodicity in the
 Tetravalent Actinides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9481
_journal_page_last               9490
_journal_paper_doi               10.1021/ic301291w
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'H2.5 O17.25 Rb4 S4 U'
_chemical_formula_weight         986.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 109.705(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4780(16)
_cell_length_b                   11.3264(15)
_cell_length_c                   13.4294(18)
_cell_measurement_reflns_used    6066
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.89
_cell_measurement_theta_min      4.08
_cell_volume                     1786.8(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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       '0.5 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  0.0784
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28484
_diffrn_reflns_theta_full        31.89
_diffrn_reflns_theta_max         31.89
_diffrn_reflns_theta_min         4.08
_exptl_absorpt_coefficient_mu    20.458
_exptl_absorpt_correction_T_max  0.2493
_exptl_absorpt_correction_T_min  0.1605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    3.668
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             1778
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.738
_refine_diff_density_min         -1.423
_refine_diff_density_rms         0.328
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         6066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0380
_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)+(0.0359P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0827
_reflns_number_gt                4473
_reflns_number_total             6066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301291w_si_003_4.cif
_cod_data_source_block           4
_cod_original_formula_sum        'H2.50 O17.25 Rb4 S4 U'
_cod_database_code               4330265
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-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
O1 O 0.1673(4) 0.9135(4) 0.2435(3) 0.0117(9) Uani 1 1 d .
O15 O 0.0362(4) 0.1285(4) 0.1162(3) 0.0135(9) Uani 1 1 d .
O14 O 0.0950(4) 0.4635(4) 0.4322(3) 0.0136(9) Uani 1 1 d .
O16 O 0.1393(4) 0.6384(4) 0.3480(4) 0.0179(10) Uani 1 1 d .
O17 O 0.2352(4) 0.6386(4) 0.1250(4) 0.0184(10) Uani 1 1 d .
O11 O 0.5361(4) 0.0017(4) 0.1583(3) 0.0117(9) Uani 1 1 d .
O12 O 0.5537(4) 0.3189(4) 0.4206(4) 0.0144(9) Uani 1 1 d .
U1 U 0.211821(19) 0.048033(19) 0.123199(17) 0.00877(6) Uani 1 1 d .
Rb1 Rb 0.63937(5) 0.21753(5) 0.15751(5) 0.01274(12) Uani 1 1 d .
Rb2 Rb 0.51859(5) 0.07152(5) 0.37733(5) 0.01452(13) Uani 1 1 d .
Rb3 Rb 0.28910(5) 0.34854(5) 0.35146(5) 0.01428(13) Uani 1 1 d .
Rb4 Rb 0.01081(6) 0.72125(6) 0.13711(5) 0.02000(14) Uani 1 1 d .
S1 S 0.79329(13) 0.48626(13) 0.15606(12) 0.0105(3) Uani 1 1 d .
S4 S 0.08584(13) 0.59391(13) 0.41989(12) 0.0096(3) Uani 1 1 d .
S2 S 0.31657(13) 0.28938(13) 0.09904(12) 0.0101(3) Uani 1 1 d .
S3 S 0.56926(13) 0.43484(13) 0.38297(12) 0.0095(3) Uani 1 1 d .
O10 O 0.6246(4) 0.4271(4) 0.2988(3) 0.0110(8) Uani 1 1 d .
O2 O 0.2438(4) 0.0999(4) 0.3034(3) 0.0125(9) Uani 1 1 d .
O3 O -0.1155(4) 0.5076(4) 0.1161(4) 0.0162(9) Uani 1 1 d .
O8 O 0.2851(4) 0.3987(4) 0.1372(4) 0.0154(9) Uani 1 1 d .
O7 O 0.4019(4) 0.3051(4) 0.0494(4) 0.0148(9) Uani 1 1 d .
O6 O 0.2132(4) 0.2274(4) 0.0254(3) 0.0099(8) Uani 1 1 d .
O9 O 0.3431(4) 0.0042(4) 0.0326(3) 0.0110(8) Uani 1 1 d .
O5 O 0.3554(4) 0.2009(4) 0.1887(3) 0.0125(9) Uani 1 1 d .
O4 O 0.6943(4) 0.4306(4) 0.0793(3) 0.0150(9) Uani 1 1 d .
O13 O 0.1417(4) 0.6376(4) 0.5305(3) 0.0123(9) Uani 1 1 d .
O18 O 0.0753(19) 0.370(3) 0.197(2) 0.053(12) Uani 0.25(2) 1 d P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Rb Rb -0.9393 2.9676 '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
S1 O1 U1 100.0(2) 2_655 1_565
S4 O15 U1 138.7(3) 2_545 .
S4 O14 U1 99.4(2) . 4_566
O15 U1 O10 152.83(15) . 2_645
O15 U1 O2 77.29(15) . .
O10 U1 O2 82.56(14) 2_645 .
O15 U1 O9 148.05(14) . .
O10 U1 O9 58.31(14) 2_645 .
O2 U1 O9 130.93(15) . .
O15 U1 O1 81.36(15) . 1_545
O10 U1 O1 72.56(15) 2_645 1_545
O2 U1 O1 58.40(14) . 1_545
O9 U1 O1 123.94(14) . 1_545
O15 U1 O6 80.18(15) . .
O10 U1 O6 123.92(14) 2_645 .
O2 U1 O6 108.28(14) . .
O9 U1 O6 76.58(14) . .
O1 U1 O6 159.40(14) 1_545 .
O15 U1 O5 107.58(15) . .
O10 U1 O5 80.40(14) 2_645 .
O2 U1 O5 66.89(14) . .
O9 U1 O5 77.61(14) . .
O1 U1 O5 120.94(14) 1_545 .
O6 U1 O5 57.34(14) . .
O15 U1 O13 98.30(15) . 4_565
O10 U1 O13 80.60(14) 2_645 4_565
O2 U1 O13 129.41(14) . 4_565
O9 U1 O13 75.66(15) . 4_565
O1 U1 O13 71.06(14) 1_545 4_565
O6 U1 O13 120.71(14) . 4_565
O5 U1 O13 152.61(15) . 4_565
O15 U1 O14 76.38(15) . 4_565
O10 U1 O14 122.60(14) 2_645 4_565
O2 U1 O14 153.65(15) . 4_565
O9 U1 O14 74.29(15) . 4_565
O1 U1 O14 117.93(14) 1_545 4_565
O6 U1 O14 66.06(14) . 4_565
O5 U1 O14 120.93(14) . 4_565
O13 U1 O14 56.40(14) 4_565 4_565
O15 U1 S3 175.83(11) . 2_645
O10 U1 S3 29.29(11) 2_645 2_645
O2 U1 S3 106.63(11) . 2_645
O9 U1 S3 29.12(10) . 2_645
O1 U1 S3 99.40(11) 1_545 2_645
O6 U1 S3 99.68(10) . 2_645
O5 U1 S3 75.61(11) . 2_645
O13 U1 S3 78.15(11) 4_565 2_645
O14 U1 S3 99.72(11) 4_565 2_645
O15 U1 S1 78.70(11) . 2_645
O10 U1 S1 74.83(11) 2_645 2_645
O2 U1 S1 29.32(10) . 2_645
O9 U1 S1 133.09(10) . 2_645
O1 U1 S1 29.11(10) 1_545 2_645
O6 U1 S1 136.18(10) . 2_645
O5 U1 S1 93.75(11) . 2_645
O13 U1 S1 100.09(11) 4_565 2_645
O14 U1 S1 141.99(11) 4_565 2_645
S3 U1 S1 103.98(4) 2_645 2_645
O15 U1 S2 94.27(11) . .
O10 U1 S2 102.95(11) 2_645 .
O2 U1 S2 87.52(10) . .
O9 U1 S2 75.22(10) . .
O1 U1 S2 145.84(10) 1_545 .
O6 U1 S2 28.57(10) . .
O5 U1 S2 28.78(10) . .
O13 U1 S2 142.76(11) 4_565 .
O14 U1 S2 93.42(10) 4_565 .
S3 U1 S2 87.40(4) 2_645 .
S1 U1 S2 116.75(4) 2_645 .
O3 S1 O4 113.5(3) 1_655 .
O3 S1 O1 111.4(3) 1_655 2_645
O4 S1 O1 109.7(3) . 2_645
O3 S1 O2 111.4(3) 1_655 2_655
O4 S1 O2 109.2(3) . 2_655
O1 S1 O2 100.8(2) 2_645 2_655
O3 S1 U1 127.0(2) 1_655 2_655
O4 S1 U1 119.5(2) . 2_655
O1 S1 U1 50.94(17) 2_645 2_655
O2 S1 U1 49.96(16) 2_655 2_655
O16 S4 O15 110.2(3) . 2
O16 S4 O14 112.8(3) . .
O15 S4 O14 109.3(3) 2 .
O16 S4 O13 112.6(3) . .
O15 S4 O13 108.6(3) 2 .
O14 S4 O13 103.1(2) . .
O16 S4 U1 124.11(19) . 4_566
O15 S4 U1 125.68(19) 2 4_566
O14 S4 U1 52.41(17) . 4_566
O13 S4 U1 50.90(17) . 4_566
O8 S2 O7 112.9(3) . .
O8 S2 O6 110.9(3) . .
O7 S2 O6 110.8(3) . .
O8 S2 O5 109.7(3) . .
O7 S2 O5 111.1(3) . .
O6 S2 O5 100.8(2) . .
O8 S2 U1 123.0(2) . .
O7 S2 U1 124.07(19) . .
O6 S2 U1 50.17(16) . .
O5 S2 U1 50.60(17) . .
O12 S3 O11 113.3(3) . 2_655
O12 S3 O9 111.1(3) . 2_655
O11 S3 O9 110.5(2) 2_655 2_655
O12 S3 O10 110.9(3) . .
O11 S3 O10 109.1(2) 2_655 .
O9 S3 O10 101.2(2) 2_655 .
O12 S3 U1 128.33(19) . 2_655
O11 S3 U1 118.32(18) 2_655 2_655
O9 S3 U1 50.91(17) 2_655 2_655
O10 S3 U1 50.53(16) . 2_655
S3 O10 U1 100.2(2) . 2_655
S1 O2 U1 100.7(2) 2_645 .
S2 O6 U1 101.3(2) . .
S3 O9 U1 100.0(2) 2_645 .
S2 O5 U1 100.6(2) . .
S4 O13 U1 100.8(2) . 4_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 S1 1.515(4) 2_655
O1 U1 2.418(4) 1_565
O15 S4 1.486(4) 2_545
O15 U1 2.346(4) .
O14 S4 1.486(4) .
O14 U1 2.491(4) 4_566
O16 S4 1.437(5) .
O11 S3 1.455(4) 2_645
O12 S3 1.444(5) .
U1 O10 2.387(4) 2_645
U1 O2 2.390(4) .
U1 O9 2.399(4) .
U1 O1 2.418(4) 1_545
U1 O6 2.423(4) .
U1 O5 2.432(4) .
U1 O13 2.450(4) 4_565
U1 O14 2.491(4) 4_565
U1 S3 3.0439(15) 2_645
U1 S1 3.0674(16) 2_645
U1 S2 3.0938(15) .
S1 O3 1.433(5) 1_655
S1 O4 1.459(5) .
S1 O1 1.515(4) 2_645
S1 O2 1.529(4) 2_655
S1 U1 3.0674(16) 2_655
S4 O15 1.486(4) 2
S4 O13 1.496(4) .
S4 U1 3.1010(15) 4_566
S2 O8 1.445(4) .
S2 O7 1.445(5) .
S2 O6 1.508(4) .
S2 O5 1.515(4) .
S3 O11 1.455(4) 2_655
S3 O9 1.504(4) 2_655
S3 O10 1.513(5) .
S3 U1 3.0439(15) 2_655
O10 U1 2.387(4) 2_655
O2 S1 1.529(4) 2_645
O3 S1 1.433(5) 1_455
O9 S3 1.504(4) 2_645
O13 U1 2.450(4) 4_566
