#------------------------------------------------------------------------------
#$Date: 2021-03-05 03:45:09 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262567 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/18/7241873.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_7241873
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 S0.43 Se1.57 U'
_chemical_formula_sum            'H10 Ni O15 S0.43 Se1.57 U'
_chemical_formula_weight         684.57
_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             2020-10-05
_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                 93.103(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3752(2)
_cell_length_b                   11.5330(3)
_cell_length_c                   13.0328(3)
_cell_measurement_reflns_used    10517
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.1650
_cell_measurement_theta_min      2.3490
_cell_volume                     1257.01(5)
_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  125.04 -98.65 -34.00 -40.00    --   739
  2  ω    -90.34 -28.84   0.50  125.00    --  -34.00 133.99 116.00  123
  3  φ    117.27 255.77   0.50  125.08-112.09 -34.00 -51.99    --   277
;
_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      -0.0747669000
_diffrn_orient_matrix_UB_12      0.0283672000
_diffrn_orient_matrix_UB_13      -0.0077166000
_diffrn_orient_matrix_UB_21      -0.0003665000
_diffrn_orient_matrix_UB_22      -0.0127846000
_diffrn_orient_matrix_UB_23      -0.0532202000
_diffrn_orient_matrix_UB_31      -0.0400817000
_diffrn_orient_matrix_UB_32      -0.0530818000
_diffrn_orient_matrix_UB_33      0.0086480000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0368
_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       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12242
_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         27.500
_diffrn_reflns_theta_min         2.360
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    19.060
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77521
_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    3.617
_exptl_crystal_description       plate
_exptl_crystal_F_000             1241
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.078
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2882
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0256
_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)+(0.0192P)²+3.0687P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0477
_refine_ls_wR_factor_ref         0.0510
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2380
_reflns_number_total             2882
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01587c1.cif
_cod_data_source_block           Compound_9
_cod_depositor_comments
'Adding full bibliography for 7241870--7241883.cif.'
_cod_database_code               7241873
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'Ni4  O60  S1  Se7  U4  H1  '
_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   0.252
_shelx_estimated_absorpt_t_min   0.064
_reflns_odcompleteness_completeness 95.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.16
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Shared sites
{S2, Se2}
{S1, Se1}
3. Restrained distances
 H10A-H10B
 1.5 with sigma of 0.02
 O10-H10A
 0.98 with sigma of 0.02
 O10-H10B
 0.98 with sigma of 0.02
 O12-H12A
 0.98 with sigma of 0.02
 O12-H12B
 0.98 with sigma of 0.02
 H12B-H12A
 1.5 with sigma of 0.02
 H14B-O14
 0.98 with sigma of 0.02
 O14-H14A
 0.98 with sigma of 0.02
 H14A-H14B
 1.5 with sigma of 0.02
 O13_$1-H13A_$1
 0.98 with sigma of 0.02
 O13_$1-H13B_$1
 0.98 with sigma of 0.02
 H13A_$1-H13B_$1
 1.5 with sigma of 0.02
 H13A_$1-O5_$3
 1.9 with sigma of 0.02
 H13B_$1-O9_$2
 2.3 with sigma of 0.02
 O15-H15B
 0.98 with sigma of 0.02
 O15-H15A
 0.98 with sigma of 0.02
 H15B-H15A
 1.5 with sigma of 0.02
 H15B-O2_$4
 2.1 with sigma of 0.02
 H15A-O11
 1.86 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 1.939
_oxdiff_exptl_absorpt_empirical_full_min 0.769
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 0.62001(2) 0.40756(2) 0.75252(2) 0.00615(6) Uani 1 1 d . . . . .
Se1 Se 0.26259(6) 0.59840(6) 0.77180(4) 0.0065(2) Uani 0.873(5) 1 d . . P A 4
Se2 Se 0.75651(7) 0.72161(6) 0.75440(5) 0.0062(2) Uani 0.697(5) 1 d . . P B 2
Ni1 Ni 0.83692(9) 0.72768(7) 0.50576(5) 0.01087(16) Uani 1 1 d . . . . .
S1 S 0.26259(6) 0.59840(6) 0.77180(4) 0.0065(2) Uani 0.127(5) 1 d . . P A 3
S2 S 0.75651(7) 0.72161(6) 0.75440(5) 0.0062(2) Uani 0.303(5) 1 d . . P B 1
O1 O 0.6902(5) 0.3735(3) 0.8796(3) 0.0108(9) Uani 1 1 d . . . . .
O2 O 0.5510(5) 0.4424(3) 0.6256(3) 0.0108(8) Uani 1 1 d D . . . .
O3 O 0.4150(5) 0.5209(4) 0.8135(3) 0.0115(9) Uani 1 1 d . . . . .
O4 O 0.1065(5) 0.5465(4) 0.8235(3) 0.0155(9) Uani 1 1 d . . . . .
O5 O 0.2461(5) 0.5993(4) 0.6483(3) 0.0148(9) Uani 1 1 d D . . . .
O6 O 0.7338(4) 0.5913(4) 0.7919(3) 0.0127(8) Uani 1 1 d . . . . .
O7 O 0.8298(5) 0.7959(4) 0.8470(3) 0.0139(9) Uani 1 1 d . . . . .
O8 O 0.8722(5) 0.7284(4) 0.6633(3) 0.0133(9) Uani 1 1 d . . . . .
O9 O 0.2900(5) 0.7303(3) 0.8154(3) 0.0118(8) Uani 1 1 d D . . . .
O10 O 0.8966(5) 0.4299(4) 0.6963(3) 0.0117(9) Uani 1 1 d D . . . .
H10A H 0.961(6) 0.364(3) 0.681(4) 0.018 Uiso 1 1 d DR . . . .
H10B H 0.966(6) 0.473(4) 0.744(4) 0.018 Uiso 1 1 d DR . . . .
O11 O 0.5829(5) 0.7704(4) 0.7157(3) 0.0141(9) Uani 1 1 d D . . . .
O12 O 0.8245(6) 0.5537(4) 0.5079(3) 0.0215(10) Uani 1 1 d D . . . .
H12A H 0.867(8) 0.502(4) 0.561(3) 0.032 Uiso 1 1 d DR . . . .
H12B H 0.809(9) 0.504(4) 0.449(3) 0.032 Uiso 1 1 d DR . . . .
O13 O 1.0799(5) 0.7201(4) 0.4978(3) 0.0146(9) Uani 1 1 d D . . . .
H13A H 1.137(6) 0.710(3) 0.561(2) 0.022 Uiso 1 1 d DR . . . .
H13B H 1.138(5) 0.772(3) 0.458(3) 0.022 Uiso 1 1 d DR . . . .
O14 O 0.8537(5) 0.9033(4) 0.5048(3) 0.0171(9) Uani 1 1 d D . . . .
H14A H 0.801(7) 0.949(5) 0.451(3) 0.026 Uiso 1 1 d DR . . . .
H14B H 0.844(8) 0.952(4) 0.564(3) 0.026 Uiso 1 1 d DR . . . .
O15 O 0.5922(5) 0.7369(4) 0.5008(3) 0.0194(10) Uani 1 1 d D . . . .
H15A H 0.564(7) 0.758(4) 0.5713(14) 0.029 Uiso 1 1 d DR . . . .
H15B H 0.537(8) 0.664(3) 0.494(2) 0.029 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 91.08(16) . . ?
O1 U1 O6 83.49(16) . . ?
O1 U1 O9 93.55(16) . 2_646 ?
O1 U1 O10 91.79(16) . . ?
O1 U1 O11 83.88(16) . 2_646 ?
O2 U1 O1 179.57(19) . . ?
O2 U1 O3 88.99(16) . . ?
O2 U1 O6 96.12(16) . . ?
O2 U1 O9 86.61(16) . 2_646 ?
O2 U1 O10 87.89(16) . . ?
O2 U1 O11 96.55(16) . 2_646 ?
O3 U1 O6 73.72(14) . . ?
O3 U1 O9 150.08(14) . 2_646 ?
O3 U1 O10 139.42(14) . . ?
O3 U1 O11 76.50(15) . 2_646 ?
O6 U1 O10 66.43(13) . . ?
O6 U1 O11 147.30(14) . 2_646 ?
O9 U1 O6 136.18(14) 2_646 . ?
O9 U1 O10 69.99(14) 2_646 . ?
O9 U1 O11 74.64(14) 2_646 2_646 ?
O11 U1 O10 144.02(14) 2_646 . ?
O3 Se1 O9 107.6(2) . . ?
O4 Se1 O3 107.1(2) . . ?
O4 Se1 O9 107.5(2) . . ?
O5 Se1 O3 111.2(2) . . ?
O5 Se1 O4 113.1(2) . . ?
O5 Se1 O9 110.2(2) . . ?
O6 Se2 O11 107.7(2) . . ?
O7 Se2 O6 109.0(2) . . ?
O7 Se2 O11 110.9(2) . . ?
O8 Se2 O6 111.5(2) . . ?
O8 Se2 O7 108.7(2) . . ?
O8 Se2 O11 109.1(2) . . ?
O8 Ni1 O7 170.21(17) . 4_575 ?
O12 Ni1 O7 83.38(17) . 4_575 ?
O12 Ni1 O8 89.71(17) . . ?
O12 Ni1 O13 90.6(2) . . ?
O12 Ni1 O14 178.9(2) . . ?
O12 Ni1 O15 90.0(2) . . ?
O13 Ni1 O7 85.38(16) . 4_575 ?
O13 Ni1 O8 87.78(16) . . ?
O13 Ni1 O15 175.25(16) . . ?
O14 Ni1 O7 97.02(16) . 4_575 ?
O14 Ni1 O8 89.77(16) . . ?
O14 Ni1 O13 88.45(18) . . ?
O14 Ni1 O15 91.00(19) . . ?
O15 Ni1 O7 90.01(16) . 4_575 ?
O15 Ni1 O8 96.94(16) . . ?
O3 S1 O9 107.6(2) . . ?
O4 S1 O3 107.1(2) . . ?
O4 S1 O9 107.5(2) . . ?
O5 S1 O3 111.2(2) . . ?
O5 S1 O4 113.1(2) . . ?
O5 S1 O9 110.2(2) . . ?
O6 S2 O11 107.7(2) . . ?
O7 S2 O6 109.0(2) . . ?
O7 S2 O11 110.9(2) . . ?
O8 S2 O6 111.5(2) . . ?
O8 S2 O7 108.7(2) . . ?
O8 S2 O11 109.1(2) . . ?
Se1 O3 U1 140.6(2) . . ?
S1 O3 U1 140.6(2) . . ?
Se2 O6 U1 146.1(2) . . ?
S2 O6 U1 146.1(2) . . ?
Se2 O7 Ni1 132.7(2) . 4_576 ?
S2 O7 Ni1 132.7(2) . 4_576 ?
Se2 O8 Ni1 133.7(2) . . ?
S2 O8 Ni1 133.7(2) . . ?
Se1 O9 U1 135.6(2) . 2_656 ?
S1 O9 U1 135.6(2) . 2_656 ?
Se2 O11 U1 144.9(2) . 2_656 ?
S2 O11 U1 144.9(2) . 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(4) . ?
U1 O2 1.769(4) . ?
U1 O3 2.332(4) . ?
U1 O6 2.369(4) . ?
U1 O9 2.367(4) 2_646 ?
U1 O10 2.480(4) . ?
U1 O11 2.374(4) 2_646 ?
Se1 O3 1.628(4) . ?
Se1 O4 1.617(4) . ?
Se1 O5 1.608(4) . ?
Se1 O9 1.636(4) . ?
Se2 O6 1.595(4) . ?
Se2 O7 1.577(4) . ?
Se2 O8 1.575(4) . ?
Se2 O11 1.615(4) . ?
Ni1 O7 2.084(4) 4_575 ?
Ni1 O8 2.058(4) . ?
Ni1 O12 2.009(4) . ?
Ni1 O13 2.045(4) . ?
Ni1 O14 2.030(4) . ?
Ni1 O15 2.050(4) . ?
S1 O3 1.628(4) . ?
S1 O4 1.617(4) . ?
S1 O5 1.608(4) . ?
S1 O9 1.636(4) . ?
S2 O6 1.595(4) . ?
S2 O7 1.577(4) . ?
S2 O8 1.575(4) . ?
S2 O11 1.615(4) . ?
O7 Ni1 2.084(4) 4_576 ?
O9 U1 2.367(4) 2_656 ?
O11 U1 2.374(4) 2_656 ?
