#------------------------------------------------------------------------------
#$Date: 2021-03-05 03:45:09 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262567 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/18/7241878.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_7241878
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 S0.22 Se1.78 U'
_chemical_formula_sum            'H10 Ni O15 S0.22 Se1.78 U'
_chemical_formula_weight         694.54
_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                 93.3090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.39020(10)
_cell_length_b                   11.5601(2)
_cell_length_c                   13.0744(2)
_cell_measurement_reflns_used    13068
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.1980
_cell_measurement_theta_min      2.3150
_cell_volume                     1265.99(3)
_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   -360.00   9.50   0.50   60.01 -98.65 -34.00 -40.00    --   739
  2  ω    -90.88 -53.88   0.50   60.00    --  -34.00 147.98 -65.98   74
  3  φ     67.80 100.80   0.50   59.98 -91.24 -34.00 -88.00    --    66
  4  ω    -77.02  -1.52   0.50   60.00    --  -34.00 102.00 134.00  151
  5  φ    232.07 274.57   0.50   59.99 -95.04 -34.00 -77.99    --    85
;
_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      0.0794084000
_diffrn_orient_matrix_UB_12      -0.0038115000
_diffrn_orient_matrix_UB_13      -0.0156064000
_diffrn_orient_matrix_UB_21      0.0278458000
_diffrn_orient_matrix_UB_22      -0.0099374000
_diffrn_orient_matrix_UB_23      0.0515205000
_diffrn_orient_matrix_UB_31      -0.0095942000
_diffrn_orient_matrix_UB_32      -0.0604136000
_diffrn_orient_matrix_UB_33      -0.0074538000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_av_unetI/netI     0.0109
_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       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11649
_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         27.497
_diffrn_reflns_theta_min         2.353
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    19.500
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18092
_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    3.644
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.662
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2904
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0147
_refine_ls_R_factor_gt           0.0140
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0160P)²+2.5498P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0336
_refine_ls_wR_factor_ref         0.0338
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2817
_reflns_number_total             2904
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01587c1.cif
_cod_data_source_block           Compound_10
_cod_depositor_comments
'Adding full bibliography for 7241870--7241883.cif.'
_cod_database_code               7241878
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'Ni4  O60  S2  Se5  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   0.442
_shelx_estimated_absorpt_t_min   0.094
_reflns_odcompleteness_completeness 94.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.13
_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
 H10B-H10A
 1.5 with sigma of 0.02
 H10B-O10
 0.98 with sigma of 0.02
 H10A-O10
 0.98 with sigma of 0.02
 H15B-H15A
 1.5 with sigma of 0.02
 H15B-O15
 0.98 with sigma of 0.02
 H15A-O15
 0.98 with sigma of 0.02
 H12B-O12
 0.98 with sigma of 0.02
 O12-H12A
 0.98 with sigma of 0.02
 H12B-H12A
 1.5 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
 H13A-H13B
 1.5 with sigma of 0.02
 H13A-O13
 0.98 with sigma of 0.02
 O13-H13B
 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 2.388
_oxdiff_exptl_absorpt_empirical_full_min 0.496
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 0.62091(2) 0.40668(2) 0.75284(2) 0.00485(4) Uani 1 1 d . . . . .
Se1 Se 0.26286(3) 0.59739(2) 0.77183(2) 0.00576(10) Uani 0.974(3) 1 d . . P A 4
Se2 Se 0.75641(3) 0.72119(3) 0.75426(2) 0.00471(11) Uani 0.810(3) 1 d . . P B 2
Ni1 Ni 0.83746(4) 0.72744(3) 0.50599(3) 0.00808(8) Uani 1 1 d . . . . .
S1 S 0.26286(3) 0.59739(2) 0.77183(2) 0.00576(10) Uani 0.026(3) 1 d . . P A 3
S2 S 0.75641(3) 0.72119(3) 0.75426(2) 0.00471(11) Uani 0.190(3) 1 d . . P B 1
O1 O 0.6932(2) 0.37313(19) 0.87970(16) 0.0110(4) Uani 1 1 d . . . . .
O2 O 0.5499(2) 0.44098(18) 0.62609(15) 0.0100(4) Uani 1 1 d . . . . .
O3 O 0.4166(2) 0.51892(18) 0.81423(15) 0.0099(4) Uani 1 1 d . . . . .
O4 O 0.1061(2) 0.54502(19) 0.82337(16) 0.0127(4) Uani 1 1 d . . . . .
O5 O 0.2467(3) 0.59889(17) 0.64765(16) 0.0113(4) Uani 1 1 d . . . . .
O6 O 0.7358(2) 0.59002(17) 0.79214(17) 0.0103(4) Uani 1 1 d . . . . .
O7 O 0.8297(2) 0.79718(18) 0.84785(15) 0.0109(4) Uani 1 1 d . . . . .
O8 O 0.8743(2) 0.72838(19) 0.66314(15) 0.0115(4) Uani 1 1 d . . . . .
O9 O 0.2903(3) 0.72968(17) 0.81576(15) 0.0108(4) Uani 1 1 d . . . . .
O10 O 0.8967(2) 0.42900(18) 0.69548(16) 0.0104(4) Uani 1 1 d D . . . .
O11 O 0.5814(2) 0.76874(18) 0.71529(15) 0.0110(4) Uani 1 1 d . . . . .
O12 O 0.8240(3) 0.5540(2) 0.50847(16) 0.0182(5) Uani 1 1 d D . . . .
O13 O 1.0810(2) 0.71884(19) 0.49804(16) 0.0119(4) Uani 1 1 d D . . . .
O14 O 0.8554(3) 0.90245(18) 0.50431(17) 0.0154(5) Uani 1 1 d D . . . .
O15 O 0.5931(3) 0.7379(2) 0.50084(16) 0.0172(5) Uani 1 1 d D . . . .
H10A H 0.952(4) 0.365(2) 0.671(3) 0.026 Uiso 1 1 d DR . . . .
H10B H 0.970(4) 0.471(3) 0.738(3) 0.026 Uiso 1 1 d DR . . . .
H12A H 0.797(5) 0.505(3) 0.4525(19) 0.026 Uiso 1 1 d DR . . . .
H12B H 0.861(5) 0.506(3) 0.5621(19) 0.026 Uiso 1 1 d DR . . . .
H13A H 1.138(4) 0.692(3) 0.557(2) 0.026 Uiso 1 1 d DR . . . .
H13B H 1.126(5) 0.787(2) 0.477(3) 0.026 Uiso 1 1 d DR . . . .
H14A H 0.851(5) 0.947(3) 0.5654(17) 0.026 Uiso 1 1 d DR . . . .
H14B H 0.814(5) 0.951(3) 0.4516(19) 0.026 Uiso 1 1 d DR . . . .
H15A H 0.548(4) 0.665(2) 0.480(3) 0.026 Uiso 1 1 d DR . . . .
H15B H 0.538(4) 0.762(3) 0.557(2) 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'
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 91.06(8) . . ?
O1 U1 O6 83.11(9) . . ?
O1 U1 O9 93.84(8) . 2_646 ?
O1 U1 O10 91.75(8) . . ?
O1 U1 O11 84.20(9) . 2_646 ?
O2 U1 O1 179.56(10) . . ?
O2 U1 O3 89.03(8) . . ?
O2 U1 O6 96.50(9) . . ?
O2 U1 O9 86.30(8) . 2_646 ?
O2 U1 O10 87.90(8) . . ?
O2 U1 O11 96.24(8) . 2_646 ?
O3 U1 O6 74.08(7) . . ?
O3 U1 O9 149.82(7) . 2_646 ?
O3 U1 O10 139.67(7) . . ?
O3 U1 O11 76.50(7) . 2_646 ?
O6 U1 O10 66.36(7) . . ?
O6 U1 O11 147.62(7) . 2_646 ?
O9 U1 O6 136.07(7) 2_646 . ?
O9 U1 O10 69.96(7) 2_646 . ?
O9 U1 O11 74.41(7) 2_646 2_646 ?
O11 U1 O10 143.78(7) 2_646 . ?
O4 Se1 O3 106.94(10) . . ?
O4 Se1 O9 107.53(11) . . ?
O5 Se1 O3 111.20(10) . . ?
O5 Se1 O4 113.29(11) . . ?
O5 Se1 O9 109.97(10) . . ?
O9 Se1 O3 107.66(11) . . ?
O6 Se2 O11 107.76(11) . . ?
O7 Se2 O6 109.00(11) . . ?
O7 Se2 O11 110.79(11) . . ?
O8 Se2 O6 111.21(11) . . ?
O8 Se2 O7 108.38(11) . . ?
O8 Se2 O11 109.70(10) . . ?
O8 Ni1 O7 169.85(8) . 4_575 ?
O12 Ni1 O7 83.18(8) . 4_575 ?
O12 Ni1 O8 89.69(9) . . ?
O12 Ni1 O13 90.56(10) . . ?
O12 Ni1 O14 178.95(10) . . ?
O12 Ni1 O15 90.11(10) . . ?
O13 Ni1 O7 85.27(8) . 4_575 ?
O13 Ni1 O8 87.61(8) . . ?
O14 Ni1 O7 97.09(9) . 4_575 ?
O14 Ni1 O8 89.92(9) . . ?
O14 Ni1 O13 88.45(10) . . ?
O14 Ni1 O15 90.90(10) . . ?
O15 Ni1 O7 90.08(8) . 4_575 ?
O15 Ni1 O8 97.16(8) . . ?
O15 Ni1 O13 175.19(8) . . ?
O4 S1 O3 106.94(10) . . ?
O4 S1 O9 107.53(11) . . ?
O5 S1 O3 111.20(10) . . ?
O5 S1 O4 113.29(11) . . ?
O5 S1 O9 109.97(10) . . ?
O9 S1 O3 107.66(11) . . ?
O6 S2 O11 107.76(11) . . ?
O7 S2 O6 109.00(11) . . ?
O7 S2 O11 110.79(11) . . ?
O8 S2 O6 111.21(11) . . ?
O8 S2 O7 108.38(11) . . ?
O8 S2 O11 109.70(10) . . ?
Se1 O3 U1 140.24(11) . . ?
S1 O3 U1 140.24(11) . . ?
Se2 O6 U1 145.63(12) . . ?
S2 O6 U1 145.63(12) . . ?
Se2 O7 Ni1 132.24(12) . 4_576 ?
S2 O7 Ni1 132.24(12) . 4_576 ?
Se2 O8 Ni1 132.94(12) . . ?
S2 O8 Ni1 132.94(12) . . ?
Se1 O9 U1 135.30(11) . 2_656 ?
S1 O9 U1 135.30(11) . 2_656 ?
Se2 O11 U1 144.37(12) . 2_656 ?
S2 O11 U1 144.37(12) . 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 1.776(2) . ?
U1 O2 1.773(2) . ?
U1 O3 2.3295(19) . ?
U1 O6 2.3723(19) . ?
U1 O9 2.371(2) 2_646 ?
U1 O10 2.487(2) . ?
U1 O11 2.383(2) 2_646 ?
Se1 O3 1.646(2) . ?
Se1 O4 1.629(2) . ?
Se1 O5 1.621(2) . ?
Se1 O9 1.645(2) . ?
Se2 O6 1.608(2) . ?
Se2 O7 1.600(2) . ?
Se2 O8 1.594(2) . ?
Se2 O11 1.622(2) . ?
Ni1 O7 2.084(2) 4_575 ?
Ni1 O8 2.060(2) . ?
Ni1 O12 2.008(2) . ?
Ni1 O13 2.055(2) . ?
Ni1 O14 2.029(2) . ?
Ni1 O15 2.051(2) . ?
S1 O3 1.646(2) . ?
S1 O4 1.629(2) . ?
S1 O5 1.621(2) . ?
S1 O9 1.645(2) . ?
S2 O6 1.608(2) . ?
S2 O7 1.600(2) . ?
S2 O8 1.594(2) . ?
S2 O11 1.622(2) . ?
O7 Ni1 2.084(2) 4_576 ?
O9 U1 2.371(2) 2_656 ?
O11 U1 2.383(2) 2_656 ?
