#------------------------------------------------------------------------------
#$Date: 2021-03-05 03:45:09 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262567 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/18/7241872.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_7241872
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 Ni O15 S0.61 Se1.39 U'
_chemical_formula_sum            'H10 Ni O15 S0.61 Se1.39 U'
_chemical_formula_weight         676.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-17 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.931(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3534(3)
_cell_length_b                   11.4839(3)
_cell_length_c                   12.9409(4)
_cell_measurement_reflns_used    12693
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.2360
_cell_measurement_theta_min      1.7590
_cell_volume                     1239.79(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(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   -278.37  -1.37   0.50   59.99 -52.22 -34.00  82.00    --   554
  2  φ   -245.76   8.24   0.50   59.99 -98.65 -34.00 -40.00    --   508
  3  ω    -99.38 -20.38   0.50   60.00    --  -34.00 147.98 -65.98  158
;
_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      0.0632358000
_diffrn_orient_matrix_UB_12      -0.0404931000
_diffrn_orient_matrix_UB_13      -0.0052110000
_diffrn_orient_matrix_UB_21      0.0549442000
_diffrn_orient_matrix_UB_22      0.0466571000
_diffrn_orient_matrix_UB_23      -0.0043621000
_diffrn_orient_matrix_UB_31      0.0148778000
_diffrn_orient_matrix_UB_32      -0.0001265000
_diffrn_orient_matrix_UB_33      0.0544098000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12003
_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         27.499
_diffrn_reflns_theta_min         2.372
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    18.826
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    3.622
_exptl_crystal_description       plate
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.807
_refine_diff_density_min         -1.438
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2851
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0167
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0215P)²+3.1183P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0409
_refine_ls_wR_factor_ref         0.0414
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2728
_reflns_number_total             2851
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01587c1.cif
_cod_data_source_block           Compound_8
_cod_depositor_comments
'Adding full bibliography for 7241870--7241883.cif.'
_cod_database_code               7241872
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'Ni4  O60  S3  Se4  U4  '
_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   0.255
_shelx_estimated_absorpt_t_min   0.065
_reflns_odcompleteness_completeness 94.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.20
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H,H,H,H,H,H,H,H,H) groups
2. Shared sites
{S2, Se2}
{S1, Se1}
3. Restrained distances
 O13-H13A
 0.98 with sigma of 0.02
 H14A-O14
 0.98 with sigma of 0.02
 O14-H14B
 0.98 with sigma of 0.02
 H14A-H14B
 1.5 with sigma of 0.02
 H15B-H15A
 1.5 with sigma of 0.02
 H15A-O15
 0.98 with sigma of 0.02
 H15B-O15
 0.98 with sigma of 0.02
 H10B-O10
 0.98 with sigma of 0.02
 O10-H10A
 0.98 with sigma of 0.02
 H10B-H10A
 1.5 with sigma of 0.02
 H13A-H13B
 1.5 with sigma of 0.02
 H13B-O13
 0.98 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(S2) = Uanis(Se2)
Uanis(S1) = Uanis(Se1)
5. Others
 Sof(Se2)=1-FVAR(1)
 Sof(S2)=FVAR(1)
 Sof(Se1)=1-FVAR(2)
 Sof(S1)=FVAR(2)
;
_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 2.001
_oxdiff_exptl_absorpt_empirical_full_min 0.494
loop_
_space_group_symop_operation_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_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 0.61934(2) 0.40919(2) 0.75201(2) 0.00565(5) Uani 1 1 d . . . . .
Se1 Se 0.26236(4) 0.59981(3) 0.77194(3) 0.00603(13) Uani 0.859(3) 1 d . . P A 4
Se2 Se 0.75583(5) 0.72269(4) 0.75421(3) 0.00509(15) Uani 0.530(3) 1 d . . P B 2
Ni1 Ni 0.83534(5) 0.72852(4) 0.50559(3) 0.00824(9) Uani 1 1 d . . . . .
S1 S 0.26236(4) 0.59981(3) 0.77194(3) 0.00603(13) Uani 0.141(3) 1 d . . P A 3
S2 S 0.75583(5) 0.72269(4) 0.75421(3) 0.00509(15) Uani 0.470(3) 1 d . . P B 1
O1 O 0.6903(3) 0.3756(2) 0.87985(18) 0.0124(5) Uani 1 1 d . . . . .
O2 O 0.5498(3) 0.4437(2) 0.62425(18) 0.0106(5) Uani 1 1 d . . . . .
O3 O 0.4144(3) 0.5218(2) 0.81367(18) 0.0110(5) Uani 1 1 d . . . . .
O4 O 0.1063(3) 0.5482(2) 0.82365(19) 0.0151(5) Uani 1 1 d . . . . .
O5 O 0.2469(3) 0.6012(2) 0.6485(2) 0.0138(5) Uani 1 1 d . . . . .
O6 O 0.7335(3) 0.59398(19) 0.7892(2) 0.0122(5) Uani 1 1 d . . . . .
O7 O 0.8287(3) 0.7943(2) 0.84652(17) 0.0126(5) Uani 1 1 d . . . . .
O8 O 0.8691(3) 0.7303(2) 0.66420(18) 0.0137(5) Uani 1 1 d . . . . .
O9 O 0.2899(3) 0.7317(2) 0.81553(18) 0.0122(5) Uani 1 1 d . . . . .
O10 O 0.8982(3) 0.4301(2) 0.6963(2) 0.0122(5) Uani 1 1 d D . . . .
O11 O 0.5854(3) 0.7717(2) 0.71830(18) 0.0120(5) Uani 1 1 d . . . . .
O12 O 0.8249(4) 0.5538(2) 0.5072(2) 0.0176(6) Uani 1 1 d . . . . .
O13 O 1.0791(3) 0.7210(2) 0.49786(19) 0.0127(5) Uani 1 1 d D . . . .
O14 O 0.8497(4) 0.9040(2) 0.5039(2) 0.0165(6) Uani 1 1 d D . . . .
O15 O 0.5903(3) 0.7371(2) 0.50108(19) 0.0167(5) Uani 1 1 d D . . . .
H10A H 0.971(4) 0.480(3) 0.736(3) 0.025 Uiso 1 1 d DR . . . .
H10B H 0.965(4) 0.368(3) 0.676(3) 0.025 Uiso 1 1 d DR . . . .
H12A H 0.802(6) 0.519(5) 0.459(4) 0.025 Uiso 1 1 d R . . . .
H12B H 0.859(6) 0.523(5) 0.554(4) 0.025 Uiso 1 1 d R . . . .
H13A H 1.125(5) 0.789(3) 0.471(3) 0.025 Uiso 1 1 d DR . . . .
H13B H 1.147(5) 0.700(4) 0.556(2) 0.025 Uiso 1 1 d DR . . . .
H14A H 0.846(5) 0.960(3) 0.558(2) 0.025 Uiso 1 1 d DR . . . .
H14B H 0.781(5) 0.934(4) 0.449(2) 0.025 Uiso 1 1 d DR . . . .
H15A H 0.535(5) 0.667(3) 0.482(3) 0.025 Uiso 1 1 d DR . . . .
H15B H 0.541(5) 0.759(3) 0.564(2) 0.025 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'
Ni Ni 0.3393 1.1124 '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'
Se Se -0.0929 2.2259 '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
_geom_angle_publ_flag
O1 U1 O3 91.00(10) . . ?
O1 U1 O6 83.85(10) . . ?
O1 U1 O9 93.42(10) . 2_646 ?
O1 U1 O10 91.04(10) . . ?
O1 U1 O11 85.04(10) . 2_646 ?
O2 U1 O1 179.47(12) . . ?
O2 U1 O3 89.07(10) . . ?
O2 U1 O6 95.67(10) . . ?
O2 U1 O9 86.77(10) . 2_646 ?
O2 U1 O10 88.56(10) . . ?
O2 U1 O11 95.49(10) . 2_646 ?
O3 U1 O6 74.16(9) . . ?
O3 U1 O9 150.03(9) . 2_646 ?
O3 U1 O10 139.93(8) . . ?
O3 U1 O11 76.37(9) . 2_646 ?
O6 U1 O10 66.30(8) . . ?
O6 U1 O11 148.22(9) . 2_646 ?
O9 U1 O6 135.79(9) 2_646 . ?
O9 U1 O10 69.66(8) 2_646 . ?
O9 U1 O11 74.51(9) 2_646 2_646 ?
O11 U1 O10 143.65(8) 2_646 . ?
O3 Se1 O9 107.68(12) . . ?
O4 Se1 O3 107.14(13) . . ?
O4 Se1 O9 107.59(13) . . ?
O5 Se1 O3 111.10(13) . . ?
O5 Se1 O4 113.22(14) . . ?
O5 Se1 O9 109.88(12) . . ?
O6 Se2 O11 107.72(13) . . ?
O7 Se2 O6 109.10(13) . . ?
O7 Se2 O11 110.52(13) . . ?
O8 Se2 O6 111.14(14) . . ?
O8 Se2 O7 108.68(13) . . ?
O8 Se2 O11 109.69(13) . . ?
O8 Ni1 O7 170.79(10) . 4_575 ?
O12 Ni1 O7 83.39(10) . 4_575 ?
O12 Ni1 O8 90.20(10) . . ?
O12 Ni1 O13 90.13(11) . . ?
O12 Ni1 O14 179.08(13) . . ?
O12 Ni1 O15 90.27(12) . . ?
O13 Ni1 O7 85.53(10) . 4_575 ?
O13 Ni1 O8 87.88(10) . . ?
O13 Ni1 O15 175.55(10) . . ?
O14 Ni1 O7 96.57(10) . 4_575 ?
O14 Ni1 O8 89.73(10) . . ?
O14 Ni1 O13 88.95(11) . . ?
O14 Ni1 O15 90.65(12) . . ?
O15 Ni1 O7 90.11(10) . 4_575 ?
O15 Ni1 O8 96.55(10) . . ?
O3 S1 O9 107.68(12) . . ?
O4 S1 O3 107.14(13) . . ?
O4 S1 O9 107.59(13) . . ?
O5 S1 O3 111.10(13) . . ?
O5 S1 O4 113.22(14) . . ?
O5 S1 O9 109.88(12) . . ?
O6 S2 O11 107.72(13) . . ?
O7 S2 O6 109.10(13) . . ?
O7 S2 O11 110.52(13) . . ?
O8 S2 O6 111.14(14) . . ?
O8 S2 O7 108.68(13) . . ?
O8 S2 O11 109.69(13) . . ?
Se1 O3 U1 140.51(13) . . ?
S1 O3 U1 140.51(13) . . ?
Se2 O6 U1 147.52(15) . . ?
S2 O6 U1 147.52(15) . . ?
Se2 O7 Ni1 133.46(14) . 4_576 ?
S2 O7 Ni1 133.46(14) . 4_576 ?
Se2 O8 Ni1 134.06(15) . . ?
S2 O8 Ni1 134.06(15) . . ?
Se1 O9 U1 135.89(13) . 2_656 ?
S1 O9 U1 135.89(13) . 2_656 ?
Se2 O11 U1 146.74(14) . 2_656 ?
S2 O11 U1 146.74(14) . 2_656 ?
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 1.771(2) . ?
U1 O2 1.769(2) . ?
U1 O3 2.319(2) . ?
U1 O6 2.366(2) . ?
U1 O9 2.358(2) 2_646 ?
U1 O10 2.485(3) . ?
U1 O11 2.373(2) 2_646 ?
Se1 O3 1.624(2) . ?
Se1 O4 1.609(3) . ?
Se1 O5 1.597(3) . ?
Se1 O9 1.629(2) . ?
Se2 O6 1.560(2) . ?
Se2 O7 1.549(2) . ?
Se2 O8 1.540(2) . ?
Se2 O11 1.579(2) . ?
Ni1 O7 2.073(2) 4_575 ?
Ni1 O8 2.058(2) . ?
Ni1 O12 2.008(3) . ?
Ni1 O13 2.046(3) . ?
Ni1 O14 2.019(2) . ?
Ni1 O15 2.047(3) . ?
S1 O3 1.624(2) . ?
S1 O4 1.609(3) . ?
S1 O5 1.597(3) . ?
S1 O9 1.629(2) . ?
S2 O6 1.560(2) . ?
S2 O7 1.549(2) . ?
S2 O8 1.540(2) . ?
S2 O11 1.579(2) . ?
O7 Ni1 2.073(2) 4_576 ?
O9 U1 2.358(2) 2_656 ?
O11 U1 2.373(2) 2_656 ?
