#------------------------------------------------------------------------------
#$Date: 2021-03-05 03:45:09 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262567 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/18/7241883.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_7241883
loop_
_publ_author_name
'Kornyakov, Ilya V.'
'Tyumentseva, Olga S.'
'Krivovichev, Sergey V.'
'Tananaev, Ivan G.'
'Gurzhiy, Vladislav V.'
_publ_section_title
;
 Crystal chemistry of the M2+[(UO2)(T6+O4)2(H2O)](H2O)4 (M2+ = Mg, Mn, Fe,
 Co, Ni and Zn; T6+ = S, Se) compounds: the interplay between chemical
 composition, pH and structural architecture
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              1140
_journal_page_last               1148
_journal_paper_doi               10.1039/D0CE01587C
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'H10 O15 S2 U Zn'
_chemical_formula_sum            'H10 O15 S2 U Zn'
_chemical_formula_weight         617.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2020-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-18 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8695(3)
_cell_length_b                   8.28206(15)
_cell_length_c                   11.2920(2)
_cell_measurement_reflns_used    10459
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      36.2010
_cell_measurement_theta_min      2.3650
_cell_volume                     1203.57(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ   -360.00   9.50   0.50   69.99 -98.65 -34.00 -40.00    --   739
  2  ω    -77.02  -1.52   0.50   70.00    --  -34.00 102.00 134.00  151
  3  ω    257.77 283.77   0.50   70.00    --  -34.00-114.00 122.00   52
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0258272000
_diffrn_orient_matrix_UB_12      0.0589577000
_diffrn_orient_matrix_UB_13      -0.0347765000
_diffrn_orient_matrix_UB_21      0.0188389000
_diffrn_orient_matrix_UB_22      0.0615755000
_diffrn_orient_matrix_UB_23      0.0379885000
_diffrn_orient_matrix_UB_31      0.0449027000
_diffrn_orient_matrix_UB_32      0.0080442000
_diffrn_orient_matrix_UB_33      -0.0359684000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10046
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_min         2.400
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    15.859
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.408
_exptl_crystal_description       plate
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.874
_refine_diff_density_min         -1.919
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   1.020(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2881
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0244P)²+5.7347P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0483
_refine_ls_wR_factor_ref         0.0498
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2706
_reflns_number_total             2881
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01587c1.cif
_cod_data_source_block           Compound_12
_cod_depositor_comments
'Adding full bibliography for 7241870--7241883.cif.'
_cod_database_code               7241883
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'Zn1 U1 S2 O15'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.504
_shelx_estimated_absorpt_t_min   0.153
_reflns_odcompleteness_completeness 96.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.04
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: -0.020(11)
 1.020(11)
2. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups, All O(H,H,H) groups
3. Restrained distances
 O12-H12_$1
 0.98 with sigma of 0.02
 H12-H12_$1
 1.54 with sigma of 0.02
 H12_$1-O4_$6
 2 with sigma of 0.02
 O10_$1-H14_$6
 2.1 with sigma of 0.02
 O14-H14_$1
 0.98 with sigma of 0.02
 H14-H14_$1
 1.54 with sigma of 0.02
 H14_$7-O10_$6
 1.9 with sigma of 0.02
 O10_$6-H10B_$6
 0.98 with sigma of 0.02
 H10B_$6-O7_$8
 1.8 with sigma of 0.02
 O10_$6-H10A_$6
 0.98 with sigma of 0.02
 H10B_$6-H10A_$6
 1.54 with sigma of 0.02
 H10A_$6-O4_$9
 1.8 with sigma of 0.02
 O16_$7-H16_$10
 0.98 with sigma of 0.02
 H16_$7-H16_$10
 1.54 with sigma of 0.02
 H16_$7-O3_$9
 1.9 with sigma of 0.02
 O15_$8-H15_$11
 0.98 with sigma of 0.02
 H15_$8-H15_$11
 1.54 with sigma of 0.02
 H15_$11-O5_$2
 1.9 with sigma of 0.02
 H12_$8-O4_$9
 1.8 with sigma of 0.02
 O13-H13_$1
 0.98 with sigma of 0.02
 O19-H19
 0.98 with sigma of 0.02
 H19_$5-H19
 1.54 with sigma of 0.02
 H19-O5_$4
 1.75 with sigma of 0.02
 O17-H17
 0.98 with sigma of 0.02
 H17-H17_$5
 1.54 with sigma of 0.02
 H17-O11_$3
 2.3 with sigma of 0.02
 H13-H13_$1
 1.54 with sigma of 0.02
 O18-H18
 0.98 with sigma of 0.02
 H18-H18_$5
 1.54 with sigma of 0.02
 O3_$5-H18_$5
 2.4 with sigma of 0.02
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.935
_oxdiff_exptl_absorpt_empirical_full_min 0.583
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y, z'
'x+1/2, -y, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.24875(2) 1.11332(2) 0.52540(9) 0.00710(8) Uani 1 1 d . . . . .
Zn1 Zn 0.0000 0.66318(16) 0.71005(12) 0.0104(3) Uani 1 2 d S T P B .
Zn2 Zn 0.5000 0.6817(2) 0.67727(13) 0.0205(4) Uani 1 2 d S T P B .
S1 S 0.27384(17) 1.2386(3) 0.8332(2) 0.0095(4) Uani 1 1 d . . . A 1
S2 S 0.25308(13) 0.7422(3) 0.7138(2) 0.0082(5) Uani 1 1 d . . . B 1
O1 O 0.3788(4) 1.0620(7) 0.4918(5) 0.0145(12) Uani 1 1 d . . . . .
O2 O 0.1186(4) 1.1638(7) 0.5597(5) 0.0147(12) Uani 1 1 d . . . . .
O3 O 0.3126(5) 1.2166(9) 0.7089(5) 0.0210(14) Uani 1 1 d D . . . .
O4 O 0.3246(5) 1.3827(7) 0.8824(6) 0.0211(16) Uani 1 1 d D . . . .
O5 O 0.1607(4) 1.2501(8) 0.8347(5) 0.0176(12) Uani 1 1 d D . . . .
O6 O 0.2302(6) 0.8966(10) 0.6562(9) 0.035(2) Uani 1 1 d . . . . .
O7 O 0.3409(5) 0.6604(9) 0.6549(6) 0.0235(15) Uani 1 1 d D . . . .
O8 O 0.1628(5) 0.6384(7) 0.7088(6) 0.0168(13) Uani 1 1 d . . . . .
O9 O 0.1893(5) 0.9021(7) 0.4043(6) 0.0233(15) Uani 1 1 d . . . . .
O10 O 0.2952(5) 1.4054(7) 0.5080(6) 0.0206(14) Uani 1 1 d D . . . .
H10A H 0.249(6) 1.455(7) 0.451(6) 0.031 Uiso 1 1 d DR . . . .
H10B H 0.301(7) 1.482(7) 0.573(5) 0.031 Uiso 1 1 d DR . . . .
O11 O 0.2145(5) 1.2263(8) 0.3363(6) 0.0195(12) Uani 1 1 d D . . . .
O12 O 0.0000 0.7132(12) 0.5307(11) 0.0248(19) Uani 1 2 d DS T P . .
H12 H 0.0600(11) 0.664(11) 0.485(4) 0.037 Uiso 1 1 d DR . . . .
O13 O 0.0000 0.9122(11) 0.7459(9) 0.022(2) Uani 1 2 d DS T P . .
H13 H 0.0593(11) 0.973(9) 0.713(8) 0.032 Uiso 1 1 d DR . . . .
O14 O 0.0000 0.6423(12) 0.8925(9) 0.019(2) Uani 1 2 d DS T P . .
H14 H 0.0605(11) 0.631(12) 0.942(4) 0.028 Uiso 1 1 d DR . . . .
O15 O 0.0000 0.4141(12) 0.6924(9) 0.019(2) Uani 1 2 d DS T P . .
H15 H 0.0598(11) 0.364(10) 0.738(7) 0.028 Uiso 1 1 d DR . . . .
O16 O 0.5000 0.4156(15) 0.6709(12) 0.032(3) Uani 1 2 d DS T P . .
H16 H 0.4398(11) 0.344(6) 0.700(8) 0.047 Uiso 1 1 d DR . . . .
O17 O 0.5000 0.6429(16) 0.8623(12) 0.041(3) Uani 1 2 d DS T P . .
O18 O 0.5000 0.9288(13) 0.7188(14) 0.047(3) Uani 1 2 d DS T P . .
O19 O 0.5000 0.7095(12) 0.4956(7) 0.017(2) Uani 1 2 d DS T P . .
H17 H 0.4396(11) 0.671(8) 0.911(4) 0.026 Uiso 1 1 d DR . . . .
H18 H 0.4402(11) 1.003(4) 0.735(7) 0.026 Uiso 1 1 d DR . . . .
H19 H 0.4402(11) 0.725(13) 0.441(3) 0.026 Uiso 1 1 d DR . . . .
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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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 O2 179.7(3) . . ?
O1 U1 O3 86.9(2) . . ?
O1 U1 O6 92.7(3) . . ?
O1 U1 O9 90.3(2) . . ?
O1 U1 O10 89.4(2) . . ?
O1 U1 O11 94.4(2) . . ?
O2 U1 O3 92.9(2) . . ?
O2 U1 O6 86.9(3) . . ?
O2 U1 O9 89.7(2) . . ?
O2 U1 O10 90.9(3) . . ?
O2 U1 O11 85.9(2) . . ?
O3 U1 O10 68.8(2) . . ?
O6 U1 O3 76.2(3) . . ?
O6 U1 O9 76.3(3) . . ?
O6 U1 O10 144.8(3) . . ?
O6 U1 O11 148.5(3) . . ?
O9 U1 O3 152.2(3) . . ?
O9 U1 O10 138.9(2) . . ?
O9 U1 O11 73.1(2) . . ?
O11 U1 O3 134.7(2) . . ?
O11 U1 O10 65.9(2) . . ?
O8 Zn1 O8 168.8(3) . 3 ?
O12 Zn1 O8 90.7(2) . . ?
O12 Zn1 O8 90.7(2) . 3 ?
O12 Zn1 O13 89.5(4) . . ?
O12 Zn1 O14 173.2(4) . . ?
O12 Zn1 O15 96.0(4) . . ?
O13 Zn1 O8 95.57(17) . . ?
O13 Zn1 O8 95.57(17) . 3 ?
O14 Zn1 O8 89.9(2) . . ?
O14 Zn1 O8 89.9(2) . 3 ?
O14 Zn1 O13 83.7(4) . . ?
O14 Zn1 O15 90.7(5) . . ?
O15 Zn1 O8 84.39(17) . . ?
O15 Zn1 O8 84.39(17) . 3 ?
O15 Zn1 O13 174.4(4) . . ?
O7 Zn2 O7 162.9(3) 3_655 . ?
O7 Zn2 O16 84.9(2) 3_655 . ?
O7 Zn2 O16 84.9(2) . . ?
O7 Zn2 O17 96.2(2) . . ?
O7 Zn2 O17 96.2(2) 3_655 . ?
O7 Zn2 O18 96.3(2) . . ?
O7 Zn2 O18 96.3(2) 3_655 . ?
O17 Zn2 O16 83.1(5) . . ?
O18 Zn2 O16 169.0(6) . . ?
O18 Zn2 O17 85.8(6) . . ?
O19 Zn2 O7 83.6(2) . 3_655 ?
O19 Zn2 O7 83.6(2) . . ?
O19 Zn2 O16 94.5(4) . . ?
O19 Zn2 O17 177.7(5) . . ?
O19 Zn2 O18 96.5(5) . . ?
O4 S1 O3 107.7(4) . . ?
O4 S1 O9 106.8(4) . 2_575 ?
O5 S1 O3 110.5(4) . . ?
O5 S1 O4 112.8(4) . . ?
O5 S1 O9 111.2(4) . 2_575 ?
O9 S1 O3 107.6(4) 2_575 . ?
O6 S2 O7 110.8(5) . . ?
O6 S2 O11 108.7(5) . 2_575 ?
O8 S2 O6 109.9(4) . . ?
O8 S2 O7 108.9(4) . . ?
O8 S2 O11 111.8(4) . 2_575 ?
O11 S2 O7 106.8(4) 2_575 . ?
S1 O3 U1 137.8(4) . . ?
S2 O6 U1 158.6(6) . . ?
S2 O7 Zn2 131.6(4) . . ?
S2 O8 Zn1 137.8(4) . . ?
S1 O9 U1 142.3(4) 2_574 . ?
S2 O11 U1 149.9(4) 2_574 . ?
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 1.768(5) . ?
U1 O2 1.769(5) . ?
U1 O3 2.388(6) . ?
U1 O6 2.337(7) . ?
U1 O9 2.349(6) . ?
U1 O10 2.500(6) . ?
U1 O11 2.373(7) . ?
Zn1 O8 2.105(6) 3 ?
Zn1 O8 2.105(6) . ?
Zn1 O12 2.067(12) . ?
Zn1 O13 2.102(9) . ?
Zn1 O14 2.068(10) . ?
Zn1 O15 2.073(10) . ?
Zn2 O7 2.070(6) . ?
Zn2 O7 2.070(6) 3_655 ?
Zn2 O16 2.205(12) . ?
Zn2 O17 2.114(14) . ?
Zn2 O18 2.100(11) . ?
Zn2 O19 2.064(8) . ?
S1 O3 1.501(6) . ?
S1 O4 1.470(6) . ?
S1 O5 1.460(5) . ?
S1 O9 1.492(6) 2_575 ?
S2 O6 1.464(7) . ?
S2 O7 1.476(6) . ?
S2 O8 1.446(6) . ?
S2 O11 1.468(7) 2_575 ?
O9 S1 1.492(6) 2_574 ?
O11 S2 1.468(7) 2_574 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 S1 O3 U1 -148.7(5) . . . . ?
O5 S1 O3 U1 -25.1(8) . . . . ?
O6 S2 O7 Zn2 85.4(7) . . . . ?
O6 S2 O8 Zn1 -32.2(8) . . . . ?
O7 S2 O6 U1 -4.6(17) . . . . ?
O7 S2 O8 Zn1 -153.7(6) . . . . ?
O8 S2 O6 U1 -125.0(15) . . . . ?
O8 S2 O7 Zn2 -153.6(6) . . . . ?
O9 S1 O3 U1 96.5(6) 2_575 . . . ?
O11 S2 O6 U1 112.3(16) 2_575 . . . ?
O11 S2 O7 Zn2 -32.8(7) 2_575 . . . ?
O11 S2 O8 Zn1 88.5(7) 2_575 . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 -0.020(11)
2 1.020(11)
