# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_4
_database_code_depnum_ccdc_archive 'CCDC 2039101'
loop_
_audit_author_name
_audit_author_address
'Ilya Kornyakov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2020-10-18 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_audit_creation_date             2020-10-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'H10 Ni O15 S1.38 Se0.62 U'
_chemical_formula_sum            'H10 Ni O15 S1.38 Se0.62 U'
_chemical_formula_weight         640.02
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ni4  O60  S7  Se1  U4  '
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_H-M_alt        'P m n 21'
_space_group_name_Hall           'P 2ac -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, z+1/2'
'-x, y, z'

_cell_length_a                   12.8182(2)
_cell_length_b                   8.2926(2)
_cell_length_c                   11.3803(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1209.68(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13221
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.2450
_cell_measurement_theta_min      1.8090
_shelx_estimated_absorpt_T_max   0.233
_shelx_estimated_absorpt_T_min   0.087
_exptl_absorpt_coefficient_mu    17.111
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81439
_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_absorpt_special_details   ?
_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    3.514
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1173
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11285
_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         27.491
_diffrn_reflns_theta_min         2.393
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ   -269.75   9.25   0.50   59.98 -98.65 -34.00 -40.00    --   558
  2  φ   -344.73 -10.23   0.50   60.00 -52.22 -34.00  82.00    --   669
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0518744000
_diffrn_orient_matrix_UB_12      0.0221775000
_diffrn_orient_matrix_UB_13      0.0144857000
_diffrn_orient_matrix_UB_21      -0.0075007000
_diffrn_orient_matrix_UB_22      0.0292452000
_diffrn_orient_matrix_UB_23      -0.0579497000
_diffrn_orient_matrix_UB_31      -0.0177410000
_diffrn_orient_matrix_UB_32      -0.0772341000
_diffrn_orient_matrix_UB_33      -0.0178542000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2720
_reflns_number_total             2902
_reflns_odcompleteness_completeness 97.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.05
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.994(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2902
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0208
_refine_ls_R_factor_gt           0.0180
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0218P)²+3.2885P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0414
_refine_ls_wR_factor_ref         0.0437
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.006(9)
 0.994(9)
2. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups, All O(H,H,H) groups
3. Shared sites
{S1, Se1}
{S2, Se2}
4. 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_$8
 2 with sigma of 0.02
 O10_$1-H14_$8
 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_$9-O10_$8
 1.9 with sigma of 0.02
 O10_$8-H10B_$8
 0.98 with sigma of 0.02
 H10B_$8-O7_$10
 1.8 with sigma of 0.02
 O10_$8-H10A_$8
 0.98 with sigma of 0.02
 H10B_$8-H10A_$8
 1.54 with sigma of 0.02
 H10A_$8-O4_$11
 1.8 with sigma of 0.02
 O16_$9-H16_$2
 0.98 with sigma of 0.02
 H16_$9-H16_$2
 1.54 with sigma of 0.02
 H16_$9-O3_$11
 1.9 with sigma of 0.02
 O15_$10-H15_$3
 0.98 with sigma of 0.02
 H15_$10-H15_$3
 1.54 with sigma of 0.02
 H15_$3-O5_$4
 1.9 with sigma of 0.02
 H12_$10-O4_$11
 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_$7-H19
 1.54 with sigma of 0.02
 H19-O5_$6
 1.75 with sigma of 0.02
 O17-H17
 0.98 with sigma of 0.02
 H17-H17_$7
 1.54 with sigma of 0.02
 H17-O11_$5
 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_$7
 1.54 with sigma of 0.02
 O3_$7-H18_$7
 2.4 with sigma of 0.02
5. Uiso/Uaniso restraints and constraints
Uanis(S1) = Uanis(Se1)
Uanis(S2) = Uanis(Se2)
6. Others
 Sof(Se1)=1-FVAR(1)
 Sof(S1)=FVAR(1)
 Sof(Se2)=1-FVAR(2)
 Sof(S2)=FVAR(2)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.24983(2) 1.11435(2) 0.52563(8) 0.00726(7) Uani 1 1 d . . . . .
Se1 Se 0.27610(9) 1.24359(15) 0.83450(9) 0.0087(3) Uani 0.491(6) 1 d . . . A 2
Se2 Se 0.25406(10) 0.7434(2) 0.71549(14) 0.0062(5) Uani 0.130(7) 1 d . . . B .
Ni1 Ni 0.0000 0.66475(15) 0.71224(12) 0.0091(3) Uani 1 2 d S T P B .
Ni2 Ni 0.5000 0.67424(16) 0.67305(13) 0.0105(3) Uani 1 2 d S T P B .
S1 S 0.27610(9) 1.24359(15) 0.83450(9) 0.0087(3) Uani 0.509(6) 1 d . . . A 1
S2 S 0.25406(10) 0.7434(2) 0.71549(14) 0.0062(5) Uani 0.870(7) 1 d . . . B 3
O1 O 0.3794(4) 1.0617(6) 0.4887(4) 0.0133(10) Uani 1 1 d . . . . .
O2 O 0.1205(4) 1.1671(6) 0.5617(4) 0.0154(10) Uani 1 1 d . . . . .
O3 O 0.3193(5) 1.2201(8) 0.7056(5) 0.0258(14) Uani 1 1 d D . . . .
O4 O 0.3297(5) 1.3935(6) 0.8867(6) 0.0243(14) Uani 1 1 d D . . . .
O5 O 0.1558(3) 1.2574(7) 0.8323(5) 0.0157(9) Uani 1 1 d D . . . .
O6 O 0.2340(5) 0.9025(8) 0.6595(7) 0.0282(16) Uani 1 1 d . . . . .
O7 O 0.3418(4) 0.6574(7) 0.6550(5) 0.0171(11) Uani 1 1 d D . . . .
O8 O 0.1600(4) 0.6401(6) 0.7106(5) 0.0161(11) Uani 1 1 d . . . . .
O9 O 0.1881(5) 0.9053(7) 0.4084(5) 0.0209(13) Uani 1 1 d . . . . .
O10 O 0.2982(5) 1.4045(6) 0.5069(5) 0.0173(12) Uani 1 1 d D . . . .
H10A H 0.253(6) 1.461(8) 0.456(6) 0.026 Uiso 1 1 d DR . . . .
H10B H 0.309(7) 1.473(6) 0.576(4) 0.026 Uiso 1 1 d DR . . . .
O11 O 0.2136(4) 1.2272(6) 0.3392(5) 0.0182(10) Uani 1 1 d D . . . .
O12 O 0.0000 0.7089(10) 0.5373(8) 0.0209(17) Uani 1 2 d DS T P . .
H12 H 0.0603(11) 0.679(10) 0.488(4) 0.031 Uiso 1 1 d DR . . . .
O13 O 0.0000 0.9096(9) 0.7435(8) 0.0185(17) Uani 1 2 d DS T P . .
H13 H 0.0594(11) 0.986(5) 0.745(8) 0.028 Uiso 1 1 d DR . . . .
O14 O 0.0000 0.6439(10) 0.8899(7) 0.0173(17) Uani 1 2 d DS T P . .
H14 H 0.0604(11) 0.602(8) 0.930(4) 0.026 Uiso 1 1 d DR . . . .
O15 O 0.0000 0.4225(10) 0.6885(6) 0.0136(16) Uani 1 2 d DS T P . .
H15 H 0.0599(11) 0.366(8) 0.727(6) 0.020 Uiso 1 1 d DR . . . .
O16 O 0.5000 0.4229(10) 0.6646(8) 0.0200(17) Uani 1 2 d DS T P . .
H16 H 0.4400(11) 0.358(5) 0.696(6) 0.030 Uiso 1 1 d DR . . . .
O17 O 0.5000 0.6488(11) 0.8520(7) 0.0188(17) Uani 1 2 d DS T P . .
O18 O 0.5000 0.9213(10) 0.6952(6) 0.0166(17) Uani 1 2 d DS T P . .
O19 O 0.5000 0.7030(10) 0.4956(6) 0.0185(19) Uani 1 2 d DS T P . .
H17 H 0.4396(11) 0.654(8) 0.902(4) 0.028 Uiso 1 1 d DR . . . .
H18 H 0.4399(11) 0.993(4) 0.713(7) 0.028 Uiso 1 1 d DR . . . .
H19 H 0.4399(11) 0.730(10) 0.444(3) 0.028 Uiso 1 1 d DR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.767(5) . ?
U1 O2 1.762(5) . ?
U1 O3 2.400(6) . ?
U1 O6 2.334(6) . ?
U1 O9 2.327(5) . ?
U1 O10 2.494(5) . ?
U1 O11 2.365(6) . ?
Se1 O3 1.580(6) . ?
Se1 O4 1.540(6) . ?
Se1 O5 1.546(4) . ?
Se1 O9 1.563(5) 2_575 ?
Se2 O6 1.488(6) . ?
Se2 O7 1.499(5) . ?
Se2 O8 1.480(6) . ?
Se2 O11 1.488(6) 2_575 ?
Ni1 O8 2.061(5) 4 ?
Ni1 O8 2.061(5) . ?
Ni1 O12 2.024(10) . ?
Ni1 O13 2.062(8) . ?
Ni1 O14 2.029(8) . ?
Ni1 O15 2.027(9) . ?
Ni2 O7 2.043(5) 4_655 ?
Ni2 O7 2.043(5) . ?
Ni2 O16 2.087(8) . ?
Ni2 O17 2.047(8) . ?
Ni2 O18 2.064(8) . ?
Ni2 O19 2.033(7) . ?
S1 O3 1.580(6) . ?
S1 O4 1.540(6) . ?
S1 O5 1.546(4) . ?
S1 O9 1.563(5) 2_575 ?
O9 Se1 1.563(5) 2_574 ?
O9 S1 1.563(5) 2_574 ?
O11 Se2 1.488(6) 2_574 ?
O11 S2 1.488(6) 2_574 ?

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 86.8(2) . . ?
O1 U1 O6 92.9(2) . . ?
O1 U1 O9 90.0(2) . . ?
O1 U1 O10 89.1(2) . . ?
O1 U1 O11 94.0(2) . . ?
O2 U1 O1 179.7(2) . . ?
O2 U1 O3 93.4(2) . . ?
O2 U1 O6 87.3(2) . . ?
O2 U1 O9 89.9(2) . . ?
O2 U1 O10 90.8(2) . . ?
O2 U1 O11 85.8(2) . . ?
O3 U1 O10 68.2(2) . . ?
O6 U1 O3 75.5(3) . . ?
O6 U1 O10 143.5(2) . . ?
O6 U1 O11 150.0(2) . . ?
O9 U1 O3 152.7(2) . . ?
O9 U1 O6 77.5(2) . . ?
O9 U1 O10 139.0(2) . . ?
O9 U1 O11 73.3(2) . . ?
O11 U1 O3 133.9(2) . . ?
O11 U1 O10 65.82(18) . . ?
O4 Se1 O3 107.5(4) . . ?
O4 Se1 O5 113.0(3) . . ?
O4 Se1 O9 107.4(3) . 2_575 ?
O5 Se1 O3 110.1(3) . . ?
O5 Se1 O9 111.1(3) . 2_575 ?
O9 Se1 O3 107.4(3) 2_575 . ?
O6 Se2 O7 110.7(4) . . ?
O8 Se2 O6 110.9(4) . . ?
O8 Se2 O7 108.6(3) . . ?
O8 Se2 O11 110.9(3) . 2_575 ?
O11 Se2 O6 107.9(4) 2_575 . ?
O11 Se2 O7 107.7(3) 2_575 . ?
O8 Ni1 O8 168.6(3) 4 . ?
O8 Ni1 O13 95.70(15) . . ?
O8 Ni1 O13 95.70(15) 4 . ?
O12 Ni1 O8 90.52(18) . 4 ?
O12 Ni1 O8 90.52(18) . . ?
O12 Ni1 O13 89.5(3) . . ?
O12 Ni1 O14 174.5(3) . . ?
O12 Ni1 O15 92.7(3) . . ?
O14 Ni1 O8 90.02(17) . . ?
O14 Ni1 O8 90.02(18) . 4 ?
O14 Ni1 O13 85.0(3) . . ?
O15 Ni1 O8 84.29(15) . . ?
O15 Ni1 O8 84.29(15) . 4 ?
O15 Ni1 O13 177.7(3) . . ?
O15 Ni1 O14 92.8(3) . . ?
O7 Ni2 O7 166.0(3) 4_655 . ?
O7 Ni2 O16 85.83(17) . . ?
O7 Ni2 O16 85.83(17) 4_655 . ?
O7 Ni2 O17 95.35(17) 4_655 . ?
O7 Ni2 O17 95.35(17) . . ?
O7 Ni2 O18 94.59(16) . . ?
O7 Ni2 O18 94.59(16) 4_655 . ?
O17 Ni2 O16 86.7(3) . . ?
O17 Ni2 O18 88.9(3) . . ?
O18 Ni2 O16 175.6(4) . . ?
O19 Ni2 O7 84.72(17) . 4_655 ?
O19 Ni2 O7 84.72(17) . . ?
O19 Ni2 O16 94.1(4) . . ?
O19 Ni2 O17 179.2(4) . . ?
O19 Ni2 O18 90.3(3) . . ?
O4 S1 O3 107.5(4) . . ?
O4 S1 O5 113.0(3) . . ?
O4 S1 O9 107.4(3) . 2_575 ?
O5 S1 O3 110.1(3) . . ?
O5 S1 O9 111.1(3) . 2_575 ?
O9 S1 O3 107.4(3) 2_575 . ?
Se1 O3 U1 135.0(3) . . ?
S1 O3 U1 135.0(3) . . ?
Se2 O6 U1 158.8(5) . . ?
Se2 O7 Ni2 131.8(3) . . ?
Se2 O8 Ni1 138.8(3) . . ?
Se1 O9 U1 142.9(3) 2_574 . ?
S1 O9 U1 142.9(3) 2_574 . ?
Se2 O11 U1 149.3(3) 2_574 . ?
S2 O11 U1 149.3(3) 2_574 . ?
S2 O11 Se2 0.0 2_574 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 Se1 O3 U1 -148.9(5) . . . . ?
O4 S1 O3 U1 -148.9(5) . . . . ?
O5 Se1 O3 U1 -25.4(6) . . . . ?
O5 S1 O3 U1 -25.4(6) . . . . ?
O6 Se2 O7 Ni2 83.3(6) . . . . ?
O6 Se2 O8 Ni1 -31.5(7) . . . . ?
O7 Se2 O6 U1 4.3(14) . . . . ?
O7 Se2 O8 Ni1 -153.4(5) . . . . ?
O8 Se2 O6 U1 -116.3(12) . . . . ?
O8 Se2 O7 Ni2 -154.7(4) . . . . ?
O9 Se1 O3 U1 95.8(5) 2_575 . . . ?
O9 S1 O3 U1 95.8(5) 2_575 . . . ?
O11 Se2 O6 U1 122.0(12) 2_575 . . . ?
O11 Se2 O7 Ni2 -34.5(6) 2_575 . . . ?
O11 Se2 O8 Ni1 88.4(6) 2_575 . . . ?

_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 1.308
_oxdiff_exptl_absorpt_empirical_full_min 0.690
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.006(9)
2 0.994(9)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_7
_database_code_depnum_ccdc_archive 'CCDC 2039107'
loop_
_audit_author_name
_audit_author_address
'Ilya Kornyakov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2020-10-17 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_audit_creation_date             2020-10-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'H10 Ni O15 S0.78 Se1.22 U'
_chemical_formula_sum            'H10 Ni O15 S0.77 Se1.23 U'
_chemical_formula_weight         668.39
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ni4  O60  S6  Se1  U4  '
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   8.35980(10)
_cell_length_b                   11.4808(2)
_cell_length_c                   12.96310(10)
_cell_angle_alpha                90
_cell_angle_beta                 92.8940(10)
_cell_angle_gamma                90
_cell_volume                     1242.58(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    15082
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.2670
_cell_measurement_theta_min      2.3740
_shelx_estimated_absorpt_T_max   0.406
_shelx_estimated_absorpt_T_min   0.114
_exptl_absorpt_coefficient_mu    18.328
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35519
_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_absorpt_special_details   ?
_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    3.573
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_unetI/netI     0.0118
_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       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11402
_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         2.371
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_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   -100.38 -20.38   0.50   70.00    --  -34.00 147.98 -65.98  160
  3  ω    241.05 319.05   0.50   70.00    --  -34.00-169.98-150.01  156
;
_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      0.0481275000
_diffrn_orient_matrix_UB_12      -0.0045674000
_diffrn_orient_matrix_UB_13      -0.0433330000
_diffrn_orient_matrix_UB_21      0.0689287000
_diffrn_orient_matrix_UB_22      -0.0076746000
_diffrn_orient_matrix_UB_23      0.0334952000
_diffrn_orient_matrix_UB_31      -0.0121607000
_diffrn_orient_matrix_UB_32      -0.0611516000
_diffrn_orient_matrix_UB_33      -0.0009386000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2777
_reflns_number_total             2856
_reflns_odcompleteness_completeness 94.29
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.10
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         1.659
_refine_diff_density_min         -1.405
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       .
_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         2856
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0172
_refine_ls_restrained_S_all      1.125
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0209P)²+4.0059P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0413
_refine_ls_wR_factor_ref         0.0416
_refine_special_details          ?
_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
 H15B-O15
 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
 H13A-O13
 0.98 with sigma of 0.02
 H13B-O13
 0.98 with sigma of 0.02
 H13A-H13B
 1.5 with sigma of 0.02
 H12A-O12
 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
 O10-H10A
 0.98 with sigma of 0.02
 H10B-H10A
 1.5 with sigma of 0.02
 H10B-O10
 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
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)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.61857(2) 0.41015(2) 0.75179(2) 0.00521(5) Uani 1 1 d . . . . .
Se1 Se 0.26225(4) 0.60078(3) 0.77204(3) 0.00538(13) Uani 0.785(3) 1 d . . P A 4
Se2 Se 0.75580(5) 0.72315(4) 0.75423(3) 0.00449(16) Uani 0.440(3) 1 d . . P B 2
Ni1 Ni 0.83490(5) 0.72871(4) 0.50538(3) 0.00797(9) Uani 1 1 d . . . . .
S1 S 0.26225(4) 0.60078(3) 0.77204(3) 0.00538(13) Uani 0.215(3) 1 d . . P A 3
S2 S 0.75580(5) 0.72315(4) 0.75423(3) 0.00449(16) Uani 0.560(3) 1 d . . P B 1
O1 O 0.6882(3) 0.3768(2) 0.88045(18) 0.0117(5) Uani 1 1 d . . . . .
O2 O 0.5504(3) 0.4444(2) 0.62363(18) 0.0097(4) Uani 1 1 d . . . . .
O3 O 0.4138(3) 0.5232(2) 0.81342(19) 0.0115(5) Uani 1 1 d . . . . .
O4 O 0.1068(3) 0.5501(2) 0.8241(2) 0.0162(5) Uani 1 1 d . . . . .
O5 O 0.2463(3) 0.6017(2) 0.6491(2) 0.0136(5) Uani 1 1 d . . . . .
O6 O 0.7323(3) 0.5954(2) 0.7884(2) 0.0122(5) Uani 1 1 d . . . . .
O7 O 0.8286(3) 0.7935(2) 0.84556(18) 0.0127(5) Uani 1 1 d . . . . .
O8 O 0.8679(3) 0.7304(2) 0.66426(18) 0.0130(5) Uani 1 1 d . . . . .
O9 O 0.2899(3) 0.7320(2) 0.81528(18) 0.0120(5) Uani 1 1 d . . . . .
O10 O 0.8980(3) 0.4305(2) 0.6969(2) 0.0119(5) Uani 1 1 d D . . . .
O11 O 0.5870(3) 0.7731(2) 0.71904(19) 0.0131(5) Uani 1 1 d . . . . .
O12 O 0.8254(4) 0.5541(2) 0.50690(19) 0.0179(6) Uani 1 1 d D . . . .
O13 O 1.0792(3) 0.7220(2) 0.49768(19) 0.0136(5) Uani 1 1 d D . . . .
O14 O 0.8482(4) 0.9048(2) 0.5042(2) 0.0159(6) Uani 1 1 d D . . . .
O15 O 0.5898(3) 0.7366(2) 0.50129(19) 0.0164(5) Uani 1 1 d D . . . .
H10A H 0.968(5) 0.370(3) 0.679(3) 0.025 Uiso 1 1 d DR . . . .
H10B H 0.965(5) 0.480(3) 0.741(3) 0.025 Uiso 1 1 d DR . . . .
H12A H 0.862(5) 0.501(3) 0.559(2) 0.025 Uiso 1 1 d DR . . . .
H12B H 0.789(6) 0.507(3) 0.450(2) 0.025 Uiso 1 1 d DR . . . .
H13A H 1.137(5) 0.702(4) 0.560(2) 0.025 Uiso 1 1 d DR . . . .
H13B H 1.134(5) 0.788(3) 0.472(3) 0.025 Uiso 1 1 d DR . . . .
H14A H 0.851(6) 0.958(3) 0.560(2) 0.025 Uiso 1 1 d DR . . . .
H14B H 0.793(5) 0.944(4) 0.449(2) 0.025 Uiso 1 1 d DR . . . .
H15A H 0.545(5) 0.765(4) 0.562(2) 0.025 Uiso 1 1 d DR . . . .
H15B H 0.529(5) 0.670(3) 0.483(3) 0.025 Uiso 1 1 d DR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.780(2) . ?
U1 O2 1.773(2) . ?
U1 O3 2.322(2) . ?
U1 O6 2.368(2) . ?
U1 O9 2.365(2) 2_646 ?
U1 O10 2.487(3) . ?
U1 O11 2.374(2) 2_646 ?
Se1 O3 1.618(2) . ?
Se1 O4 1.604(3) . ?
Se1 O5 1.593(3) . ?
Se1 O9 1.620(2) . ?
Se2 O6 1.547(2) . ?
Se2 O7 1.534(2) . ?
Se2 O8 1.535(2) . ?
Se2 O11 1.570(2) . ?
Ni1 O7 2.085(2) 4_575 ?
Ni1 O8 2.064(2) . ?
Ni1 O12 2.006(3) . ?
Ni1 O13 2.051(3) . ?
Ni1 O14 2.024(2) . ?
Ni1 O15 2.049(3) . ?
S1 O3 1.618(2) . ?
S1 O4 1.604(3) . ?
S1 O5 1.593(3) . ?
S1 O9 1.620(2) . ?
S2 O6 1.547(2) . ?
S2 O7 1.534(2) . ?
S2 O8 1.535(2) . ?
S2 O11 1.570(2) . ?
O7 Ni1 2.085(2) 4_576 ?
O9 U1 2.364(2) 2_656 ?
O11 U1 2.374(2) 2_656 ?

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 90.54(10) . . ?
O1 U1 O6 84.06(11) . . ?
O1 U1 O9 93.56(10) . 2_646 ?
O1 U1 O10 91.19(10) . . ?
O1 U1 O11 85.02(10) . 2_646 ?
O2 U1 O1 179.48(12) . . ?
O2 U1 O3 89.47(10) . . ?
O2 U1 O6 95.45(10) . . ?
O2 U1 O9 86.69(10) . 2_646 ?
O2 U1 O10 88.47(10) . . ?
O2 U1 O11 95.48(10) . 2_646 ?
O3 U1 O6 74.02(9) . . ?
O3 U1 O9 150.20(9) . 2_646 ?
O3 U1 O10 139.94(8) . . ?
O3 U1 O11 76.32(9) . 2_646 ?
O6 U1 O10 66.37(9) . . ?
O6 U1 O11 148.20(9) . 2_646 ?
O9 U1 O6 135.75(9) 2_646 . ?
O9 U1 O10 69.53(8) 2_646 . ?
O9 U1 O11 74.67(9) 2_646 2_646 ?
O11 U1 O10 143.68(9) 2_646 . ?
O3 Se1 O9 107.56(13) . . ?
O4 Se1 O3 107.34(13) . . ?
O4 Se1 O9 107.25(14) . . ?
O5 Se1 O3 111.09(13) . . ?
O5 Se1 O4 113.28(14) . . ?
O5 Se1 O9 110.07(12) . . ?
O6 Se2 O11 107.72(14) . . ?
O7 Se2 O6 109.24(13) . . ?
O7 Se2 O8 108.93(14) . . ?
O7 Se2 O11 110.36(14) . . ?
O8 Se2 O6 111.08(14) . . ?
O8 Se2 O11 109.50(13) . . ?
O8 Ni1 O7 171.02(10) . 4_575 ?
O12 Ni1 O7 83.60(10) . 4_575 ?
O12 Ni1 O8 90.16(10) . . ?
O12 Ni1 O13 90.17(11) . . ?
O12 Ni1 O14 179.13(12) . . ?
O12 Ni1 O15 90.24(12) . . ?
O13 Ni1 O7 85.53(10) . 4_575 ?
O13 Ni1 O8 88.04(10) . . ?
O14 Ni1 O7 96.52(10) . 4_575 ?
O14 Ni1 O8 89.62(10) . . ?
O14 Ni1 O13 88.98(12) . . ?
O14 Ni1 O15 90.62(12) . . ?
O15 Ni1 O7 90.28(10) . 4_575 ?
O15 Ni1 O8 96.22(10) . . ?
O15 Ni1 O13 175.72(10) . . ?
O3 S1 O9 107.56(13) . . ?
O4 S1 O3 107.34(13) . . ?
O4 S1 O9 107.25(14) . . ?
O5 S1 O3 111.09(13) . . ?
O5 S1 O4 113.28(14) . . ?
O5 S1 O9 110.07(12) . . ?
O6 S2 O11 107.72(14) . . ?
O7 S2 O6 109.24(13) . . ?
O7 S2 O8 108.93(14) . . ?
O7 S2 O11 110.36(14) . . ?
O8 S2 O6 111.08(14) . . ?
O8 S2 O11 109.50(13) . . ?
Se1 O3 U1 140.56(14) . . ?
S1 O3 U1 140.56(14) . . ?
Se2 O6 U1 148.16(16) . . ?
S2 O6 U1 148.16(16) . . ?
Se2 O7 Ni1 133.75(15) . 4_576 ?
S2 O7 Ni1 133.75(15) . 4_576 ?
Se2 O8 Ni1 134.58(15) . . ?
S2 O8 Ni1 134.58(15) . . ?
Se1 O9 U1 136.09(13) . 2_656 ?
S1 O9 U1 136.09(13) . 2_656 ?
Se2 O11 U1 147.48(15) . 2_656 ?
S2 O11 U1 147.48(15) . 2_656 ?

_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 1.576
_oxdiff_exptl_absorpt_empirical_full_min 0.397
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_8
_database_code_depnum_ccdc_archive 'CCDC 2039108'
loop_
_audit_author_name
_audit_author_address
'Ilya Kornyakov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2020-10-17 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_audit_creation_date             2020-10-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_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
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ni4  O60  S3  Se4  U4  '
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   8.3534(3)
_cell_length_b                   11.4839(3)
_cell_length_c                   12.9409(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.931(3)
_cell_angle_gamma                90
_cell_volume                     1239.79(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12693
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.2360
_cell_measurement_theta_min      1.7590
_shelx_estimated_absorpt_T_max   0.255
_shelx_estimated_absorpt_T_min   0.065
_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_absorpt_special_details   ?
_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_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_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_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2728
_reflns_number_total             2851
_reflns_odcompleteness_completeness 94.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.20
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.807
_refine_diff_density_min         -1.438
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       .
_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_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0167
_refine_ls_restrained_S_all      1.125
_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
_refine_special_details          ?
_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)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 ?

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 ?

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_9
_database_code_depnum_ccdc_archive 'CCDC 2039106'
loop_
_audit_author_name
_audit_author_address
'Ilya Kornyakov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2020-10-17 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_audit_creation_date             2020-10-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_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
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ni4  O60  S1  Se7  U4  H1  '
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   8.3752(2)
_cell_length_b                   11.5330(3)
_cell_length_c                   13.0328(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.103(2)
_cell_angle_gamma                90
_cell_volume                     1257.01(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10517
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.1650
_cell_measurement_theta_min      2.3490
_shelx_estimated_absorpt_T_max   0.252
_shelx_estimated_absorpt_T_min   0.064
_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_absorpt_special_details   ?
_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_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_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_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2380
_reflns_number_total             2882
_reflns_odcompleteness_completeness 95.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.16
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         1.078
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.219
_refine_ls_extinction_coef       .
_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_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0256
_refine_ls_restrained_S_all      1.040
_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
_refine_special_details          ?
_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)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 ?

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 ?

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_1
_database_code_depnum_ccdc_archive 'CCDC 2039104'
loop_
_audit_author_name
_audit_author_address
'Ilya Kornyakov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2020-10-18 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_audit_creation_date             2020-10-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'H10 Ni O15 S2 U'
_chemical_formula_sum            'H10 Ni O15 S2 U'
_chemical_formula_weight         610.94
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ni4  O60  S8  U4  '
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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_H-M_alt        'P m n 21'
_space_group_name_Hall           'P 2ac -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, z+1/2'
'-x, y, z'

_cell_length_a                   12.75060(10)
_cell_length_b                   8.30950(10)
_cell_length_c                   11.29290(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1196.50(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    34708
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      44.7710
_cell_measurement_theta_min      2.3930
_shelx_estimated_absorpt_T_max   0.306
_shelx_estimated_absorpt_T_min   0.069
_exptl_absorpt_coefficient_mu    15.521
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14111
_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_absorpt_special_details   ?
_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    3.392
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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       -11
_diffrn_reflns_number            28646
_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         27.490
_diffrn_reflns_theta_min         2.409
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -114.71 -28.21   0.50   10.00    --  -52.00 166.02 179.99  173
  2  φ      5.23 264.73   0.50   10.00 -39.40 -52.00 102.00    --   519
  3  φ   -295.60 -31.10   0.50   10.00 -34.45 -38.00 161.98    --   529
  4  φ   -200.27   6.73   0.50   10.00 -74.17 -44.00-156.00    --   414
  5  ω    -82.44  -8.44   0.50   10.00    --  -48.00 117.99 132.01  148
  6  φ     16.09 272.09   0.50   10.00 -42.45 -36.00 167.96    --   512
  7  ω    -78.16 -24.16   0.50   10.00    --  -44.00  99.99 -30.00  108
  8  φ    153.84 293.34   0.50   10.00-131.49 -54.00 -93.99    --   279
  9  ω    229.47 302.47   0.50   10.00    --  -46.00 -60.00  70.00  146
 10  φ   -359.99   9.51   0.50   10.00 -63.55 -36.00 137.99    --   739
 11  ω    238.20 278.70   0.50   10.00    --  -44.00 -92.00  46.00   81
 12  ω    -68.48  -6.98   0.50   10.00    --  -52.00 106.00  36.00  123
 13  φ    156.99 260.49   0.50   10.00 -92.21 -44.00-109.99    --   207
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0051957000
_diffrn_orient_matrix_UB_12      0.0849933000
_diffrn_orient_matrix_UB_13      -0.0013552000
_diffrn_orient_matrix_UB_21      -0.0546274000
_diffrn_orient_matrix_UB_22      -0.0081358000
_diffrn_orient_matrix_UB_23      -0.0103285000
_diffrn_orient_matrix_UB_31      -0.0092751000
_diffrn_orient_matrix_UB_32      0.0004482000
_diffrn_orient_matrix_UB_33      0.0618945000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2092
_reflns_number_total             2150
_reflns_odcompleteness_completeness 94.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     44.68
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         1.732
_refine_diff_density_min         -1.337
_refine_diff_density_rms         0.260
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.965(13)
_refine_ls_extinction_coef       0.0013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         2150
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0277
_refine_ls_restrained_S_all      1.165
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0592P)²+0.3756P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0758
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.035(13)
 0.965(13)
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
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.24863(2) 1.11241(2) 0.52510(16) 0.01243(15) Uani 1 1 d . . . . .
Ni1 Ni 0.0000 0.66561(14) 0.71070(11) 0.0160(3) Uani 1 2 d S T P B .
Ni2 Ni 0.5000 0.67104(15) 0.67658(12) 0.0178(3) Uani 1 2 d S T P B .
S1 S 0.27374(15) 1.2392(2) 0.83293(17) 0.0170(3) Uani 1 1 d . . . A 1
S2 S 0.25378(8) 0.7428(3) 0.7147(2) 0.0120(4) Uani 1 1 d . . . B 1
O1 O 0.3805(3) 1.0693(5) 0.4908(4) 0.0256(9) Uani 1 1 d . . . . .
O2 O 0.1170(3) 1.1567(5) 0.5599(5) 0.0250(9) Uani 1 1 d . . . . .
O3 O 0.3128(4) 1.2150(5) 0.7104(4) 0.0280(9) Uani 1 1 d D . . . .
O4 O 0.3266(4) 1.3806(4) 0.8815(5) 0.0354(12) Uani 1 1 d D . . . .
O5 O 0.1607(3) 1.2553(6) 0.8334(5) 0.0335(10) Uani 1 1 d D . . . .
O6 O 0.2366(5) 0.8967(9) 0.6563(13) 0.037(2) Uani 1 1 d . . . . .
O7 O 0.3405(4) 0.6544(7) 0.6588(5) 0.0248(12) Uani 1 1 d D . . . .
O8 O 0.1607(4) 0.6435(7) 0.7079(6) 0.0295(13) Uani 1 1 d . . . . .
O9 O 0.1922(4) 0.9011(5) 0.4028(5) 0.0307(10) Uani 1 1 d . . . . .
O10 O 0.2886(5) 1.4045(5) 0.5112(5) 0.0338(12) Uani 1 1 d D . . . .
H10A H 0.256(5) 1.469(8) 0.449(5) 0.051 Uiso 1 1 d DR . . . .
H10B H 0.290(6) 1.482(6) 0.579(4) 0.051 Uiso 1 1 d DR . . . .
O11 O 0.2161(4) 1.2255(5) 0.3378(5) 0.0283(9) Uani 1 1 d D . . . .
O12 O 0.0000 0.7151(12) 0.5346(9) 0.0383(19) Uani 1 2 d DS T P . .
H12 H 0.0606(10) 0.665(8) 0.489(3) 0.057 Uiso 1 1 d DR . . . .
O13 O 0.0000 0.9099(10) 0.7456(8) 0.0282(19) Uani 1 2 d DS T P . .
H13 H 0.0600(10) 0.982(5) 0.729(9) 0.042 Uiso 1 1 d DR . . . .
O14 O 0.0000 0.6359(13) 0.8895(10) 0.034(2) Uani 1 2 d DS T P . .
H14 H 0.0614(10) 0.624(9) 0.948(4) 0.051 Uiso 1 1 d DR . . . .
O15 O 0.0000 0.4225(13) 0.6885(11) 0.032(2) Uani 1 2 d DS T P . .
H15 H 0.0604(10) 0.359(8) 0.727(6) 0.048 Uiso 1 1 d DR . . . .
O16 O 0.5000 0.4183(12) 0.6668(10) 0.029(2) Uani 1 2 d DS T P . .
H16 H 0.4395(10) 0.346(5) 0.695(7) 0.043 Uiso 1 1 d DR . . . .
O17 O 0.5000 0.6407(14) 0.8563(10) 0.039(2) Uani 1 2 d DS T P . .
O18 O 0.5000 0.9188(12) 0.7042(10) 0.039(3) Uani 1 2 d DS T P . .
O19 O 0.5000 0.7033(11) 0.4972(7) 0.030(2) Uani 1 2 d DS T P . .
H17 H 0.4381(9) 0.646(7) 0.903(4) 0.045 Uiso 1 1 d DR . . . .
H18 H 0.4397(10) 0.996(3) 0.717(9) 0.045 Uiso 1 1 d DR . . . .
H19 H 0.4396(10) 0.716(8) 0.442(3) 0.045 Uiso 1 1 d DR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.762(4) . ?
U1 O2 1.763(4) . ?
U1 O3 2.403(5) . ?
U1 O6 2.330(9) . ?
U1 O9 2.347(4) . ?
U1 O10 2.485(4) . ?
U1 O11 2.351(5) . ?
Ni1 O8 2.057(5) 4 ?
Ni1 O8 2.058(5) . ?
Ni1 O12 2.031(11) . ?
Ni1 O13 2.068(9) . ?
Ni1 O14 2.035(11) . ?
Ni1 O15 2.035(11) . ?
Ni2 O7 2.048(5) . ?
Ni2 O7 2.048(5) 4_655 ?
Ni2 O16 2.103(11) . ?
Ni2 O17 2.045(12) . ?
Ni2 O18 2.082(9) . ?
Ni2 O19 2.043(8) . ?
S1 O3 1.484(5) . ?
S1 O4 1.461(4) . ?
S1 O5 1.447(4) . ?
S1 O9 1.474(5) 2_575 ?
S2 O6 1.456(8) . ?
S2 O7 1.470(5) . ?
S2 O8 1.448(5) . ?
S2 O11 1.466(6) 2_575 ?
O9 S1 1.474(5) 2_574 ?
O11 S2 1.466(6) 2_574 ?

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 179.6(2) . . ?
O1 U1 O3 86.48(19) . . ?
O1 U1 O6 92.6(2) . . ?
O1 U1 O9 90.62(19) . . ?
O1 U1 O10 89.37(19) . . ?
O1 U1 O11 93.0(2) . . ?
O2 U1 O3 93.2(2) . . ?
O2 U1 O6 87.5(2) . . ?
O2 U1 O9 89.75(19) . . ?
O2 U1 O10 90.33(19) . . ?
O2 U1 O11 87.1(2) . . ?
O3 U1 O10 68.81(17) . . ?
O6 U1 O3 75.0(3) . . ?
O6 U1 O9 77.2(3) . . ?
O6 U1 O10 143.6(4) . . ?
O6 U1 O11 150.2(3) . . ?
O9 U1 O3 151.92(18) . . ?
O9 U1 O10 139.2(2) . . ?
O9 U1 O11 73.48(19) . . ?
O11 U1 O3 134.54(16) . . ?
O11 U1 O10 65.73(18) . . ?
O8 Ni1 O8 169.6(3) 4 . ?
O8 Ni1 O13 95.20(16) . . ?
O8 Ni1 O13 95.20(16) 4 . ?
O12 Ni1 O8 90.2(2) . 4 ?
O12 Ni1 O8 90.2(2) . . ?
O12 Ni1 O13 89.3(4) . . ?
O12 Ni1 O14 175.3(4) . . ?
O12 Ni1 O15 94.6(4) . . ?
O14 Ni1 O8 90.3(2) . . ?
O14 Ni1 O8 90.3(2) . 4 ?
O14 Ni1 O13 86.0(4) . . ?
O14 Ni1 O15 90.1(5) . . ?
O15 Ni1 O8 84.80(16) . . ?
O15 Ni1 O8 84.80(16) . 4 ?
O15 Ni1 O13 176.1(5) . . ?
O7 Ni2 O7 166.4(3) 4_655 . ?
O7 Ni2 O16 85.85(17) 4_655 . ?
O7 Ni2 O16 85.85(17) . . ?
O7 Ni2 O18 94.66(17) 4_655 . ?
O7 Ni2 O18 94.66(17) . . ?
O17 Ni2 O7 95.09(17) . . ?
O17 Ni2 O7 95.09(17) . 4_655 ?
O17 Ni2 O16 85.9(4) . . ?
O17 Ni2 O18 88.5(4) . . ?
O18 Ni2 O16 174.4(5) . . ?
O19 Ni2 O7 84.94(17) . . ?
O19 Ni2 O7 84.94(17) . 4_655 ?
O19 Ni2 O16 94.5(4) . . ?
O19 Ni2 O17 179.5(4) . . ?
O19 Ni2 O18 91.1(4) . . ?
O4 S1 O3 107.7(3) . . ?
O4 S1 O9 107.4(3) . 2_575 ?
O5 S1 O3 110.5(3) . . ?
O5 S1 O4 112.6(3) . . ?
O5 S1 O9 111.4(3) . 2_575 ?
O9 S1 O3 107.1(3) 2_575 . ?
O6 S2 O7 110.9(5) . . ?
O6 S2 O11 108.2(6) . 2_575 ?
O8 S2 O6 110.7(4) . . ?
O8 S2 O7 108.0(4) . . ?
O8 S2 O11 111.6(4) . 2_575 ?
O11 S2 O7 107.4(3) 2_575 . ?
S1 O3 U1 138.2(3) . . ?
S2 O6 U1 162.6(7) . . ?
S2 O7 Ni2 132.2(3) . . ?
S2 O8 Ni1 139.9(4) . . ?
S1 O9 U1 144.8(3) 2_574 . ?
S2 O11 U1 151.5(3) 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(4) . . . . ?
O5 S1 O3 U1 -25.4(5) . . . . ?
O6 S2 O7 Ni2 81.2(7) . . . . ?
O6 S2 O8 Ni1 -35.4(10) . . . . ?
O7 S2 O6 U1 4(2) . . . . ?
O7 S2 O8 Ni1 -157.0(6) . . . . ?
O8 S2 O6 U1 -116(2) . . . . ?
O8 S2 O7 Ni2 -157.3(5) . . . . ?
O9 S1 O3 U1 96.0(4) 2_575 . . . ?
O11 S2 O6 U1 122(2) 2_575 . . . ?
O11 S2 O7 Ni2 -36.8(6) 2_575 . . . ?
O11 S2 O8 Ni1 85.1(7) 2_575 . . . ?

_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 3.280
_oxdiff_exptl_absorpt_empirical_full_min 0.521
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.035(13)
2 0.965(13)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_5
_database_code_depnum_ccdc_archive 'CCDC 2039103'
loop_
_audit_author_name
_audit_author_address
'Ilya Kornyakov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2020-10-18 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_audit_creation_date             2020-10-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'H10 Ni O15 S1.2 Se0.8 U'
_chemical_formula_sum            'H10 Ni O15 S1.20 Se0.80 U'
_chemical_formula_weight         648.46
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ni4  O60  S3  Se4  U4  '
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_H-M_alt        'P m n 21'
_space_group_name_Hall           'P 2ac -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, z+1/2'
'-x, y, z'

_cell_length_a                   12.8291(9)
_cell_length_b                   8.2825(5)
_cell_length_c                   11.3826(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1209.48(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7153
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.2980
_cell_measurement_theta_min      2.3190
_shelx_estimated_absorpt_T_max   0.473
_shelx_estimated_absorpt_T_min   0.096
_exptl_absorpt_coefficient_mu    17.624
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76695
_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_absorpt_special_details   ?
_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    3.561
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1186
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0393
_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       -15
_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            11165
_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         27.490
_diffrn_reflns_theta_min         2.392
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_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     71.32 313.32   0.50   59.99 -98.65 -34.00 -40.00    --   484
  2  ω    241.05 319.05   0.50   60.00    --  -34.00-169.98-150.01  156
  3  φ    122.91 300.90   0.50   60.00 -52.22 -34.00  82.00    --   356
  4  ω    -84.29 -25.29   0.50   60.00    --  -34.00 147.98 -65.98  118
;
_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      -0.0415802000
_diffrn_orient_matrix_UB_12      -0.0065128000
_diffrn_orient_matrix_UB_13      -0.0408470000
_diffrn_orient_matrix_UB_21      -0.0301549000
_diffrn_orient_matrix_UB_22      -0.0417861000
_diffrn_orient_matrix_UB_23      0.0424076000
_diffrn_orient_matrix_UB_31      -0.0206118000
_diffrn_orient_matrix_UB_32      0.0743807000
_diffrn_orient_matrix_UB_33      0.0203724000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2347
_reflns_number_total             2905
_reflns_odcompleteness_completeness 97.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.28
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         1.034
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.193
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.170(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2905
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0303
_refine_ls_restrained_S_all      1.057
_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)+(0.0303P)²+2.7920P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0663
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.830(15)
 0.170(15)
2. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups, All O(H,H,H) groups
3. Shared sites
{S1, Se1}
{S2, Se2}
4. 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_$8
 2 with sigma of 0.02
 O10_$1-H14_$8
 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_$9-O10_$8
 1.9 with sigma of 0.02
 O10_$8-H10B_$8
 0.98 with sigma of 0.02
 H10B_$8-O7_$10
 1.8 with sigma of 0.02
 O10_$8-H10A_$8
 0.98 with sigma of 0.02
 H10B_$8-H10A_$8
 1.54 with sigma of 0.02
 H10A_$8-O4_$11
 1.8 with sigma of 0.02
 O16_$9-H16_$2
 0.98 with sigma of 0.02
 H16_$9-H16_$2
 1.54 with sigma of 0.02
 H16_$9-O3_$11
 1.9 with sigma of 0.02
 O15_$10-H15_$3
 0.98 with sigma of 0.02
 H15_$10-H15_$3
 1.54 with sigma of 0.02
 H15_$3-O5_$4
 1.9 with sigma of 0.02
 H12_$10-O4_$11
 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_$7-H19
 1.54 with sigma of 0.02
 H19-O5_$6
 1.75 with sigma of 0.02
 O17-H17
 0.98 with sigma of 0.02
 H17-H17_$7
 1.54 with sigma of 0.02
 H17-O11_$5
 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_$7
 1.54 with sigma of 0.02
 O3_$7-H18_$7
 2.4 with sigma of 0.02
5. Uiso/Uaniso restraints and constraints
Uanis(S1) = Uanis(Se1)
Uanis(S2) = Uanis(Se2)
6. Others
 Sof(Se1)=1-FVAR(1)
 Sof(S1)=FVAR(1)
 Sof(Se2)=1-FVAR(2)
 Sof(S2)=FVAR(2)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.24966(5) 1.11481(4) 0.52562(14) 0.00793(11) Uani 1 1 d . . . . .
Se1 Se 0.27643(15) 1.2439(3) 0.83462(16) 0.0108(6) Uani 0.619(10) 1 d . . . A 2
Se2 Se 0.25436(18) 0.7439(4) 0.7157(3) 0.0072(9) Uani 0.183(12) 1 d . . . B .
Ni1 Ni 0.0000 0.6651(3) 0.7127(2) 0.0105(5) Uani 1 2 d S T P B .
Ni2 Ni 0.5000 0.6736(3) 0.6723(2) 0.0114(5) Uani 1 2 d S T P B .
S1 S 0.27643(15) 1.2439(3) 0.83462(16) 0.0108(6) Uani 0.381(10) 1 d . . . A 1
S2 S 0.25436(18) 0.7439(4) 0.7157(3) 0.0072(9) Uani 0.817(12) 1 d . . . B 3
O1 O 0.3791(7) 1.0622(12) 0.4882(7) 0.012(2) Uani 1 1 d . . . . .
O2 O 0.1213(7) 1.1683(13) 0.5630(8) 0.016(2) Uani 1 1 d . . . . .
O3 O 0.3200(8) 1.2220(16) 0.7052(8) 0.025(3) Uani 1 1 d D . . . .
O4 O 0.3312(9) 1.3955(12) 0.8875(11) 0.024(3) Uani 1 1 d D . . . .
O5 O 0.1548(6) 1.2579(13) 0.8324(9) 0.0150(19) Uani 1 1 d D . . . .
O6 O 0.2331(8) 0.9028(15) 0.6596(12) 0.028(3) Uani 1 1 d . . . . .
O7 O 0.3414(8) 0.6561(13) 0.6533(10) 0.018(2) Uani 1 1 d D . . . .
O8 O 0.1612(8) 0.6403(12) 0.7108(10) 0.017(2) Uani 1 1 d . . . . .
O9 O 0.1863(9) 0.9061(13) 0.4086(10) 0.022(3) Uani 1 1 d . . . . .
O10 O 0.2989(8) 1.4049(11) 0.5066(8) 0.016(2) Uani 1 1 d D . . . .
H10A H 0.242(7) 1.455(10) 0.466(10) 0.024 Uiso 1 1 d DR . . . .
H10B H 0.315(11) 1.474(8) 0.572(7) 0.024 Uiso 1 1 d DR . . . .
O11 O 0.2133(7) 1.2270(13) 0.3388(10) 0.022(2) Uani 1 1 d D . . . .
O12 O 0.0000 0.709(2) 0.5374(16) 0.025(4) Uani 1 2 d DS T P . .
H12 H 0.0601(12) 0.663(15) 0.494(6) 0.038 Uiso 1 1 d DR . . . .
O13 O 0.0000 0.9103(17) 0.7449(12) 0.016(3) Uani 1 2 d DS T P . .
H13 H 0.0599(12) 0.954(15) 0.703(9) 0.024 Uiso 1 1 d DR . . . .
O14 O 0.0000 0.6432(19) 0.8877(14) 0.017(3) Uani 1 2 d DS T P . .
H14 H 0.0604(11) 0.598(11) 0.929(5) 0.025 Uiso 1 1 d DR . . . .
O15 O 0.0000 0.424(2) 0.6879(13) 0.019(4) Uani 1 2 d DS T P . .
H15 H 0.0598(11) 0.376(15) 0.733(9) 0.028 Uiso 1 1 d DR . . . .
O16 O 0.5000 0.4239(19) 0.6607(16) 0.023(4) Uani 1 2 d DS T P . .
H16 H 0.4400(12) 0.360(7) 0.693(8) 0.035 Uiso 1 1 d DR . . . .
O17 O 0.5000 0.6461(19) 0.8497(13) 0.018(3) Uani 1 2 d DS T P . .
O18 O 0.5000 0.9182(17) 0.6957(12) 0.015(3) Uani 1 2 d DS T P . .
O19 O 0.5000 0.7040(19) 0.4960(12) 0.017(4) Uani 1 2 d DS T P . .
H17 H 0.4400(11) 0.656(9) 0.901(4) 0.025 Uiso 1 1 d DR . . . .
H18 H 0.4403(11) 0.997(4) 0.694(11) 0.025 Uiso 1 1 d DR . . . .
H19 H 0.4400(11) 0.726(18) 0.444(4) 0.025 Uiso 1 1 d DR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.769(9) . ?
U1 O2 1.758(9) . ?
U1 O3 2.404(10) . ?
U1 O6 2.336(12) . ?
U1 O9 2.329(10) . ?
U1 O10 2.494(9) . ?
U1 O11 2.367(11) . ?
Se1 O3 1.586(10) . ?
Se1 O4 1.560(12) . ?
Se1 O5 1.565(7) . ?
Se1 O9 1.575(11) 2_575 ?
Se2 O6 1.488(12) . ?
Se2 O7 1.510(10) . ?
Se2 O8 1.472(10) . ?
Se2 O11 1.481(12) 2_575 ?
Ni1 O8 2.078(10) . ?
Ni1 O8 2.078(10) 4 ?
Ni1 O12 2.028(18) . ?
Ni1 O13 2.063(14) . ?
Ni1 O14 2.001(16) . ?
Ni1 O15 2.021(17) . ?
Ni2 O7 2.051(10) . ?
Ni2 O7 2.051(10) 4_655 ?
Ni2 O16 2.073(17) . ?
Ni2 O17 2.032(15) . ?
Ni2 O18 2.043(15) . ?
Ni2 O19 2.023(13) . ?
S1 O3 1.586(10) . ?
S1 O4 1.560(12) . ?
S1 O5 1.565(7) . ?
S1 O9 1.575(11) 2_575 ?
O9 Se1 1.575(11) 2_574 ?
O9 S1 1.575(11) 2_574 ?
O11 Se2 1.481(12) 2_574 ?
O11 S2 1.481(12) 2_574 ?

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 86.7(4) . . ?
O1 U1 O6 93.3(4) . . ?
O1 U1 O9 90.4(4) . . ?
O1 U1 O10 88.8(4) . . ?
O1 U1 O11 93.8(4) . . ?
O2 U1 O1 179.6(5) . . ?
O2 U1 O3 93.0(4) . . ?
O2 U1 O6 86.9(4) . . ?
O2 U1 O9 89.9(4) . . ?
O2 U1 O10 90.9(4) . . ?
O2 U1 O11 86.2(4) . . ?
O3 U1 O10 67.9(4) . . ?
O6 U1 O3 75.9(4) . . ?
O6 U1 O10 143.5(4) . . ?
O6 U1 O11 149.8(4) . . ?
O9 U1 O3 153.0(4) . . ?
O9 U1 O6 77.5(4) . . ?
O9 U1 O10 138.9(4) . . ?
O9 U1 O11 73.0(4) . . ?
O11 U1 O3 133.9(4) . . ?
O11 U1 O10 66.0(3) . . ?
O4 Se1 O3 106.9(6) . . ?
O4 Se1 O5 113.3(6) . . ?
O4 Se1 O9 107.0(6) . 2_575 ?
O5 Se1 O3 110.2(5) . . ?
O5 Se1 O9 111.7(6) . 2_575 ?
O9 Se1 O3 107.4(6) 2_575 . ?
O6 Se2 O7 111.1(7) . . ?
O8 Se2 O6 110.5(6) . . ?
O8 Se2 O7 107.6(6) . . ?
O8 Se2 O11 111.0(6) . 2_575 ?
O11 Se2 O6 108.2(7) 2_575 . ?
O11 Se2 O7 108.4(6) 2_575 . ?
O8 Ni1 O8 168.6(6) 4 . ?
O12 Ni1 O8 90.4(3) . . ?
O12 Ni1 O8 90.4(3) . 4 ?
O12 Ni1 O13 90.0(6) . . ?
O13 Ni1 O8 95.7(3) . 4 ?
O13 Ni1 O8 95.7(3) . . ?
O14 Ni1 O8 90.1(3) . . ?
O14 Ni1 O8 90.1(3) . 4 ?
O14 Ni1 O12 174.9(7) . . ?
O14 Ni1 O13 84.9(6) . . ?
O14 Ni1 O15 92.8(7) . . ?
O15 Ni1 O8 84.3(3) . . ?
O15 Ni1 O8 84.3(3) . 4 ?
O15 Ni1 O12 92.2(7) . . ?
O15 Ni1 O13 177.8(6) . . ?
O7 Ni2 O7 165.4(6) . 4_655 ?
O7 Ni2 O16 85.6(3) 4_655 . ?
O7 Ni2 O16 85.6(3) . . ?
O17 Ni2 O7 95.5(3) . . ?
O17 Ni2 O7 95.5(3) . 4_655 ?
O17 Ni2 O16 87.2(6) . . ?
O17 Ni2 O18 89.0(6) . . ?
O18 Ni2 O7 94.8(3) . 4_655 ?
O18 Ni2 O7 94.8(3) . . ?
O18 Ni2 O16 176.2(7) . . ?
O19 Ni2 O7 84.5(3) . . ?
O19 Ni2 O7 84.5(3) . 4_655 ?
O19 Ni2 O16 93.5(7) . . ?
O19 Ni2 O17 179.3(7) . . ?
O19 Ni2 O18 90.3(6) . . ?
O4 S1 O3 106.9(6) . . ?
O4 S1 O5 113.3(6) . . ?
O4 S1 O9 107.0(6) . 2_575 ?
O5 S1 O3 110.2(5) . . ?
O5 S1 O9 111.7(6) . 2_575 ?
O9 S1 O3 107.4(6) 2_575 . ?
Se1 O3 U1 134.4(6) . . ?
S1 O3 U1 134.4(6) . . ?
Se2 O6 U1 158.2(8) . . ?
Se2 O7 Ni2 130.5(6) . . ?
Se2 O8 Ni1 138.6(6) . . ?
Se1 O9 U1 141.8(6) 2_574 . ?
S1 O9 U1 141.8(6) 2_574 . ?
Se2 O11 U1 149.2(6) 2_574 . ?
S2 O11 U1 149.2(6) 2_574 . ?
S2 O11 Se2 0.0 2_574 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 Se1 O3 U1 -149.7(9) . . . . ?
O4 S1 O3 U1 -149.7(9) . . . . ?
O5 Se1 O3 U1 -26.2(11) . . . . ?
O5 S1 O3 U1 -26.2(11) . . . . ?
O6 Se2 O7 Ni2 84.3(10) . . . . ?
O6 Se2 O8 Ni1 -31.5(13) . . . . ?
O7 Se2 O6 U1 2(2) . . . . ?
O7 Se2 O8 Ni1 -153.0(9) . . . . ?
O8 Se2 O6 U1 -118(2) . . . . ?
O8 Se2 O7 Ni2 -154.6(8) . . . . ?
O9 Se1 O3 U1 95.7(9) 2_575 . . . ?
O9 S1 O3 U1 95.7(9) 2_575 . . . ?
O11 Se2 O6 U1 121(2) 2_575 . . . ?
O11 Se2 O7 Ni2 -34.5(11) 2_575 . . . ?
O11 Se2 O8 Ni1 88.6(11) 2_575 . . . ?

_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 1.496
_oxdiff_exptl_absorpt_empirical_full_min 0.685
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.830(15)
2 0.170(15)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_6
_database_code_depnum_ccdc_archive 'CCDC 2039105'
loop_
_audit_author_name
_audit_author_address
'Ilya Kornyakov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2020-10-17 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_audit_creation_date             2020-10-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'H10 Ni O15 S0.96 Se1.04 U'
_chemical_formula_sum            'H10 Ni O15 S0.96 Se1.04 U'
_chemical_formula_weight         659.83
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ni4  O60  S4  Se3  U4  '
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   8.3202(4)
_cell_length_b                   11.4227(4)
_cell_length_c                   12.8820(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.718(4)
_cell_angle_gamma                90
_cell_volume                     1222.92(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10664
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.2140
_cell_measurement_theta_min      2.3830
_shelx_estimated_absorpt_T_max   0.465
_shelx_estimated_absorpt_T_min   0.098
_exptl_absorpt_coefficient_mu    18.111
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59089
_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_absorpt_special_details   ?
_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    3.584
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1203
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_av_unetI/netI     0.0519
_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            12259
_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         2.384
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_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    -77.02  -1.52   0.50   60.00    --  -34.00 102.00 134.00  151
  3  ω   -100.38 -20.38   0.50   60.00    --  -34.00 147.98 -65.99  160
  4  ω    246.23 278.73   0.50   60.00    --  -34.00-102.00 -54.00   65
;
_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      -0.0476414000
_diffrn_orient_matrix_UB_12      0.0306717000
_diffrn_orient_matrix_UB_13      -0.0381633000
_diffrn_orient_matrix_UB_21      0.0195472000
_diffrn_orient_matrix_UB_22      0.0536453000
_diffrn_orient_matrix_UB_23      0.0253095000
_diffrn_orient_matrix_UB_31      0.0680708000
_diffrn_orient_matrix_UB_32      0.0060885000
_diffrn_orient_matrix_UB_33      -0.0306797000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2306
_reflns_number_total             2814
_reflns_odcompleteness_completeness 95.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.28
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         1.559
_refine_diff_density_min         -1.392
_refine_diff_density_rms         0.282
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2814
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0388
_refine_ls_restrained_S_all      1.065
_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)+(0.0209P)²+12.4148P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0710
_refine_special_details          ?
_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
 H13B-H13A
 1.5 with sigma of 0.02
 O13-H13B
 0.98 with sigma of 0.02
 H13B-O1_$1
 2.6 with sigma of 0.02
 O9_$2-H13B
 2.5 with sigma of 0.02
 O15_$3-H15A_$3
 0.98 with sigma of 0.02
 O15_$3-H15B_$3
 0.98 with sigma of 0.02
 H15A_$3-H15B_$3
 1.5 with sigma of 0.02
 H12B-H12A
 1.5 with sigma of 0.02
 O12-H12B
 0.98 with sigma of 0.02
 O12-H12A
 0.98 with sigma of 0.02
 O14-H14B
 0.98 with sigma of 0.02
 O14-H14A
 0.98 with sigma of 0.02
 H14B-H14A
 1.5 with sigma of 0.02
 H10B-H10A
 1.5 with sigma of 0.02
 O10-H10B
 0.98 with sigma of 0.02
 O10-H10A
 0.98 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(S2) = Uanis(Se2)
Uanis(S1) = Uanis(Se1)
Uanis(O7) = Uanis(O11)
Uanis(O6) = Uanis(O7)
5. Others
 Sof(Se2)=1-FVAR(1)
 Sof(S2)=FVAR(1)
 Sof(Se1)=1-FVAR(2)
 Sof(S1)=FVAR(2)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.61782(4) 0.41119(3) 0.75141(2) 0.00513(9) Uani 1 1 d . . . . .
Se1 Se 0.26197(11) 0.60200(8) 0.77224(7) 0.0050(3) Uani 0.714(7) 1 d . . P A 4
Se2 Se 0.75561(16) 0.72369(11) 0.75433(10) 0.0050(5) Uani 0.328(7) 1 d . . P B
2
Ni1 Ni 0.83432(13) 0.72922(9) 0.50522(8) 0.0073(2) Uani 1 1 d . . . . .
S1 S 0.26197(11) 0.60200(8) 0.77224(7) 0.0050(3) Uani 0.286(7) 1 d . . P A 3
S2 S 0.75561(16) 0.72369(11) 0.75433(10) 0.0050(5) Uani 0.672(7) 1 d . . P B 1
O1 O 0.6860(8) 0.3780(5) 0.8803(4) 0.0136(13) Uani 1 1 d D . . . .
O2 O 0.5500(7) 0.4458(5) 0.6230(4) 0.0094(12) Uani 1 1 d . . . . .
O3 O 0.4117(7) 0.5241(5) 0.8138(5) 0.0123(13) Uani 1 1 d . . . . .
O4 O 0.1065(8) 0.5517(6) 0.8245(5) 0.0157(14) Uani 1 1 d . . . . .
O5 O 0.2478(7) 0.6027(5) 0.6496(4) 0.0139(13) Uani 1 1 d . . . . .
O6 O 0.7312(7) 0.5970(5) 0.7876(4) 0.0117(7) Uani 1 1 d . . . . .
O7 O 0.8294(7) 0.7922(5) 0.8447(4) 0.0117(7) Uani 1 1 d . . . . .
O8 O 0.8662(7) 0.7305(5) 0.6649(4) 0.0117(13) Uani 1 1 d . . . . .
O9 O 0.2886(7) 0.7321(5) 0.8140(4) 0.0121(13) Uani 1 1 d D . . . .
O10 O 0.8983(7) 0.4313(5) 0.6974(5) 0.0115(13) Uani 1 1 d D . . . .
O11 O 0.5870(7) 0.7737(5) 0.7192(4) 0.0117(7) Uani 1 1 d . . . . .
O12 O 0.8260(9) 0.5543(5) 0.5064(5) 0.0184(15) Uani 1 1 d D . . . .
O13 O 1.0780(7) 0.7235(5) 0.4969(5) 0.0124(13) Uani 1 1 d D . . . .
O14 O 0.8464(8) 0.9062(5) 0.5043(4) 0.0177(14) Uani 1 1 d D . . . .
O15 O 0.5882(7) 0.7365(5) 0.5018(5) 0.0133(13) Uani 1 1 d D . . . .
H10A H 0.962(8) 0.363(5) 0.681(7) 0.020 Uiso 1 1 d DR . . . .
H10B H 0.975(8) 0.475(6) 0.741(6) 0.020 Uiso 1 1 d DR . . . .
H12A H 0.869(11) 0.500(5) 0.558(4) 0.020 Uiso 1 1 d DR . . . .
H12B H 0.812(12) 0.506(6) 0.445(4) 0.020 Uiso 1 1 d DR . . . .
H13A H 1.146(8) 0.703(6) 0.557(4) 0.020 Uiso 1 1 d DR . . . .
H13B H 1.128(3) 0.792(2) 0.4710(14) 0.020 Uiso 1 1 d DR . . . .
H14A H 0.769(9) 0.947(7) 0.458(5) 0.020 Uiso 1 1 d DR . . . .
H14B H 0.851(11) 0.958(6) 0.564(4) 0.020 Uiso 1 1 d DR . . . .
H15A H 0.549(10) 0.750(7) 0.571(3) 0.020 Uiso 1 1 d DR . . . .
H15B H 0.534(10) 0.663(5) 0.483(6) 0.020 Uiso 1 1 d DR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.770(6) . ?
U1 O2 1.767(5) . ?
U1 O3 2.320(6) . ?
U1 O6 2.361(6) . ?
U1 O9 2.359(6) 2_646 ?
U1 O10 2.477(6) . ?
U1 O11 2.361(6) 2_646 ?
Se1 O3 1.602(6) . ?
Se1 O4 1.593(6) . ?
Se1 O5 1.578(6) . ?
Se1 O9 1.592(6) . ?
Se2 O6 1.525(6) . ?
Se2 O7 1.509(6) . ?
Se2 O8 1.510(6) . ?
Se2 O11 1.562(6) . ?
Ni1 O7 2.081(6) 4_575 ?
Ni1 O8 2.062(6) . ?
Ni1 O12 1.999(6) . ?
Ni1 O13 2.036(6) . ?
Ni1 O14 2.024(6) . ?
Ni1 O15 2.048(6) . ?
S1 O3 1.602(6) . ?
S1 O4 1.593(6) . ?
S1 O5 1.578(6) . ?
S1 O9 1.592(6) . ?
S2 O6 1.525(6) . ?
S2 O7 1.509(6) . ?
S2 O8 1.510(6) . ?
S2 O11 1.562(6) . ?
O7 Ni1 2.081(6) 4_576 ?
O9 U1 2.359(6) 2_656 ?
O11 U1 2.361(6) 2_656 ?

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 90.2(2) . . ?
O1 U1 O6 84.3(2) . . ?
O1 U1 O9 93.0(2) . 2_646 ?
O1 U1 O10 91.1(3) . . ?
O1 U1 O11 84.8(2) . 2_646 ?
O2 U1 O1 179.5(3) . . ?
O2 U1 O3 89.5(2) . . ?
O2 U1 O6 95.2(2) . . ?
O2 U1 O9 87.4(2) . 2_646 ?
O2 U1 O10 88.8(2) . . ?
O2 U1 O11 95.6(2) . 2_646 ?
O3 U1 O6 74.1(2) . . ?
O3 U1 O9 150.2(2) . 2_646 ?
O3 U1 O10 140.12(19) . . ?
O3 U1 O11 76.3(2) . 2_646 ?
O6 U1 O10 66.4(2) . . ?
O6 U1 O11 148.3(2) . 2_646 ?
O9 U1 O6 135.6(2) 2_646 . ?
O9 U1 O10 69.4(2) 2_646 . ?
O9 U1 O11 74.5(2) 2_646 2_646 ?
O11 U1 O10 143.46(19) 2_646 . ?
O4 Se1 O3 107.0(3) . . ?
O5 Se1 O3 110.9(3) . . ?
O5 Se1 O4 113.6(3) . . ?
O5 Se1 O9 109.7(3) . . ?
O9 Se1 O3 108.1(3) . . ?
O9 Se1 O4 107.2(3) . . ?
O6 Se2 O11 107.4(3) . . ?
O7 Se2 O6 109.2(3) . . ?
O7 Se2 O8 108.7(3) . . ?
O7 Se2 O11 111.2(3) . . ?
O8 Se2 O6 111.0(3) . . ?
O8 Se2 O11 109.3(3) . . ?
O8 Ni1 O7 171.1(2) . 4_575 ?
O12 Ni1 O7 83.8(2) . 4_575 ?
O12 Ni1 O8 90.1(2) . . ?
O12 Ni1 O13 90.2(3) . . ?
O12 Ni1 O14 179.1(3) . . ?
O12 Ni1 O15 90.3(3) . . ?
O13 Ni1 O7 85.2(2) . 4_575 ?
O13 Ni1 O8 88.4(2) . . ?
O13 Ni1 O15 175.7(3) . . ?
O14 Ni1 O7 96.3(2) . 4_575 ?
O14 Ni1 O8 89.7(2) . . ?
O14 Ni1 O13 89.0(3) . . ?
O14 Ni1 O15 90.5(3) . . ?
O15 Ni1 O7 90.6(2) . 4_575 ?
O15 Ni1 O8 95.9(2) . . ?
O4 S1 O3 107.0(3) . . ?
O5 S1 O3 110.9(3) . . ?
O5 S1 O4 113.6(3) . . ?
O5 S1 O9 109.7(3) . . ?
O9 S1 O3 108.1(3) . . ?
O9 S1 O4 107.2(3) . . ?
O6 S2 O11 107.4(3) . . ?
O7 S2 O6 109.2(3) . . ?
O7 S2 O8 108.7(3) . . ?
O7 S2 O11 111.2(3) . . ?
O8 S2 O6 111.0(3) . . ?
O8 S2 O11 109.3(3) . . ?
Se1 O3 U1 140.2(3) . . ?
S1 O3 U1 140.2(3) . . ?
Se2 O6 U1 148.7(3) . . ?
S2 O6 U1 148.7(3) . . ?
Se2 O7 Ni1 133.9(4) . 4_576 ?
S2 O7 Ni1 133.9(4) . 4_576 ?
Se2 O8 Ni1 135.0(4) . . ?
S2 O8 Ni1 135.0(4) . . ?
Se1 O9 U1 137.0(3) . 2_656 ?
S1 O9 U1 137.0(3) . 2_656 ?
Se2 O11 U1 147.4(3) . 2_656 ?
S2 O11 U1 147.4(3) . 2_656 ?

_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 1.873
_oxdiff_exptl_absorpt_empirical_full_min 0.489
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_14
_database_code_depnum_ccdc_archive 'CCDC 2039111'
loop_
_audit_author_name
_audit_author_address
'Ilya Kornyakov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2020-10-18 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_audit_creation_date             2020-10-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'H10 Mn O15 S2 U'
_chemical_formula_sum            'H10 Mn O15 S2 U'
_chemical_formula_weight         607.17
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Mn1 U1 S2 O15'
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'
Mn Mn 0.3368 0.7283 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   6.51140(10)
_cell_length_b                   11.3829(2)
_cell_length_c                   8.3439(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.773(2)
_cell_angle_gamma                90
_cell_volume                     618.38(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10264
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      36.5390
_cell_measurement_theta_min      1.7820
_shelx_estimated_absorpt_T_max   0.275
_shelx_estimated_absorpt_T_min   0.061
_exptl_absorpt_coefficient_mu    14.515
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43201
_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_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.261
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             558
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0164
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8215
_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         29.988
_diffrn_reflns_theta_min         2.441
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_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  ω      8.21 192.21   0.50   60.00    --   34.00  73.86 -25.79  368
  2  ω      8.21 192.21   0.50   60.00    --   34.00  73.86  64.21  368
  3  ω      8.21 192.21   0.50   60.00    --   34.00  73.86 154.21  368
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1085739000
_diffrn_orient_matrix_UB_12      -0.0049776000
_diffrn_orient_matrix_UB_13      -0.0032756000
_diffrn_orient_matrix_UB_21      0.0067559000
_diffrn_orient_matrix_UB_22      -0.0306072000
_diffrn_orient_matrix_UB_23      -0.0737062000
_diffrn_orient_matrix_UB_31      0.0062680000
_diffrn_orient_matrix_UB_32      -0.0541021000
_diffrn_orient_matrix_UB_33      0.0420813000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3495
_reflns_number_total             3600
_reflns_odcompleteness_completeness 96.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.27
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details 
;
 Flack x determined using 1629 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(5)
_refine_ls_extinction_coef       0.0075(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3600
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0171
_refine_ls_R_factor_gt           0.0163
_refine_ls_restrained_S_all      1.043
_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)+(0.0283P)²+0.1753P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0398
_refine_ls_wR_factor_ref         0.0401
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All H(H) groups, All O(H,H,H,H,H,H,H,H) groups
2. Restrained distances
 H3A-H3B
 1.54 with sigma of 0.02
 O3-H3B
 0.98 with sigma of 0.02
 O3-H3A
 0.98 with sigma of 0.02
 O6_$1-H3B
 1.65 with sigma of 0.02
 O14_$1-H14B_$1 = O14_$1-H14A_$1
 0.98 with sigma of 0.02
 H14B_$1-H14A_$1
 1.54 with sigma of 0.02
 O5_$2-H14B_$1
 2.1 with sigma of 0.02
 H14A_$1-O7_$3
 2.1 with sigma of 0.02
 O15-H15B = O15-H15A
 0.9 with sigma of 0.02
 H15A-H15B
 1.45 with sigma of 0.02
 H15A-O7_$4
 2.1 with sigma of 0.02
 H15B-O6
 2.1 with sigma of 0.02
 O13-H13A = O13-H13B
 0.9 with sigma of 0.02
 H13A-H13B
 1.45 with sigma of 0.02
 H13A-O1_$2
 2.1 with sigma of 0.02
 O13-H13B
 0.9 with sigma of 0.02
 H13B-H13A
 1.54 with sigma of 0.02
 H13B-O3_$3
 2.2 with sigma of 0.02
 O2_$3-H12A
 2.5 with sigma of 0.02
 O12-H12A
 0.9 with sigma of 0.02
 H12B-H12A
 1.54 with sigma of 0.02
 O12-H12B
 0.9 with sigma of 0.02
 H12A-O2_$3
 2.41 with sigma of 0.02
 H12B-O1
 2.2 with sigma of 0.02
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.00250(2) 0.24499(3) 0.11186(2) 0.01308(6) Uani 1 1 d . . . . .
Mn1 Mn -0.49975(12) 0.06796(8) -0.33123(12) 0.02129(17) Uani 1 1 d . . . . .
S1 S -0.0167(2) 0.43881(13) -0.2355(2) 0.0160(3) Uani 1 1 d . . . . .
S2 S 0.0038(2) 0.05660(13) -0.25657(19) 0.0130(3) Uani 1 1 d . . . . .
O1 O -0.2596(6) 0.2163(3) 0.1489(6) 0.0265(9) Uani 1 1 d D . . . .
O2 O 0.2638(6) 0.2728(4) 0.0741(6) 0.0300(11) Uani 1 1 d D . . . .
O3 O 0.0808(9) 0.2555(6) 0.4010(5) 0.0388(12) Uani 1 1 d D . . . .
O4 O -0.0978(8) 0.3659(5) -0.1035(7) 0.0314(12) Uani 1 1 d . . . . .
O5 O -0.1034(7) 0.5591(4) -0.2147(6) 0.0290(9) Uani 1 1 d D . . . .
O6 O -0.1054(9) 0.3915(5) -0.3829(6) 0.0362(12) Uani 1 1 d D . . . .
O7 O 0.2061(6) 0.4419(4) -0.2314(7) 0.0362(11) Uani 1 1 d D . . . .
O8 O -0.0320(10) 0.1154(6) -0.1043(7) 0.0413(16) Uani 1 1 d . . . . .
O9 O 0.1790(6) 0.1082(4) -0.3370(6) 0.0303(10) Uani 1 1 d . . . . .
O10 O -0.1758(6) 0.0670(6) -0.3598(6) 0.0337(12) Uani 1 1 d . . . . .
O11 O 0.0491(8) -0.0673(4) -0.2243(6) 0.0327(10) Uani 1 1 d . . . . .
O12 O -0.5006(9) 0.0286(6) -0.0706(7) 0.0464(14) Uani 1 1 d D . . . .
O13 O -0.5125(10) -0.1205(7) -0.3671(9) 0.0451(18) Uani 1 1 d D . . . .
H13A H -0.605(12) -0.167(9) -0.316(14) 0.18(10) Uiso 1 1 d D . . . .
H12A H -0.468(13) -0.046(4) -0.046(14) 0.268 Uiso 1 1 d DR . . . .
O14 O -0.5079(7) 0.0843(7) -0.5950(7) 0.0345(15) Uani 1 1 d D . . . .
O15 O -0.4785(7) 0.2582(6) -0.2870(8) 0.0449(15) Uani 1 1 d D . . . .
H3A H 0.110(15) 0.181(5) 0.453(10) 0.067 Uiso 1 1 d DR . . . .
H3B H 0.017(17) 0.302(7) 0.489(9) 0.067 Uiso 1 1 d DR . . . .
H12B H -0.434(16) 0.085(8) -0.004(12) 0.067 Uiso 1 1 d DR . . . .
H13B H -0.400(7) -0.164(7) -0.396(11) 0.067 Uiso 1 1 d DR . . . .
H14A H -0.391(7) 0.037(7) -0.612(8) 0.067 Uiso 1 1 d DR . . . .
H14B H -0.628(7) 0.048(6) -0.642(10) 0.067 Uiso 1 1 d DR . . . .
H15A H -0.593(7) 0.301(5) -0.277(14) 0.067 Uiso 1 1 d DR . . . .
H15B H -0.371(8) 0.310(6) -0.287(10) 0.067 Uiso 1 1 d DR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.769(4) . ?
U1 O2 1.763(4) . ?
U1 O3 2.462(4) . ?
U1 O4 2.349(5) . ?
U1 O5 2.373(4) 2_545 ?
U1 O8 2.338(6) . ?
U1 O11 2.359(4) 2 ?
Mn1 O9 2.141(4) 1_455 ?
Mn1 O10 2.126(4) . ?
Mn1 O12 2.220(6) . ?
Mn1 O13 2.168(8) . ?
Mn1 O14 2.209(6) . ?
Mn1 O15 2.201(7) . ?
S1 O4 1.482(5) . ?
S1 O5 1.492(4) . ?
S1 O6 1.455(5) . ?
S1 O7 1.451(4) . ?
S2 O8 1.458(6) . ?
S2 O9 1.455(4) . ?
S2 O10 1.448(5) . ?
S2 O11 1.465(5) . ?
O5 U1 2.373(4) 2 ?
O9 Mn1 2.141(4) 1_655 ?
O11 U1 2.359(4) 2_545 ?

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 91.5(2) . . ?
O1 U1 O4 89.02(19) . . ?
O1 U1 O5 92.02(17) . 2_545 ?
O1 U1 O8 86.3(2) . . ?
O1 U1 O11 87.42(18) . 2 ?
O2 U1 O1 179.6(2) . . ?
O2 U1 O3 88.8(2) . . ?
O2 U1 O4 90.98(19) . . ?
O2 U1 O5 87.79(18) . 2_545 ?
O2 U1 O8 93.3(2) . . ?
O2 U1 O11 92.94(19) . 2 ?
O4 U1 O3 140.6(2) . . ?
O4 U1 O5 150.7(2) . 2_545 ?
O4 U1 O11 74.6(2) . 2 ?
O5 U1 O3 68.7(2) 2_545 . ?
O8 U1 O3 143.4(2) . . ?
O8 U1 O4 75.9(2) . . ?
O8 U1 O5 74.9(2) . 2_545 ?
O8 U1 O11 149.9(2) . 2 ?
O11 U1 O3 66.1(2) 2 . ?
O11 U1 O5 134.76(17) 2 2_545 ?
O9 Mn1 O12 92.9(2) 1_455 . ?
O9 Mn1 O13 100.0(2) 1_455 . ?
O9 Mn1 O14 87.09(19) 1_455 . ?
O9 Mn1 O15 81.52(17) 1_455 . ?
O10 Mn1 O9 165.7(2) . 1_455 ?
O10 Mn1 O12 97.1(2) . . ?
O10 Mn1 O13 90.9(2) . . ?
O10 Mn1 O14 84.21(18) . . ?
O10 Mn1 O15 87.9(2) . . ?
O13 Mn1 O12 86.3(3) . . ?
O13 Mn1 O14 86.9(3) . . ?
O13 Mn1 O15 177.8(3) . . ?
O14 Mn1 O12 173.0(3) . . ?
O15 Mn1 O12 92.0(3) . . ?
O15 Mn1 O14 94.9(3) . . ?
O4 S1 O5 106.7(3) . . ?
O6 S1 O4 106.2(3) . . ?
O6 S1 O5 107.0(3) . . ?
O7 S1 O4 111.2(3) . . ?
O7 S1 O5 110.8(3) . . ?
O7 S1 O6 114.5(3) . . ?
O8 S2 O11 108.4(4) . . ?
O9 S2 O8 110.6(4) . . ?
O9 S2 O11 108.4(3) . . ?
O10 S2 O8 110.1(4) . . ?
O10 S2 O9 108.9(3) . . ?
O10 S2 O11 110.3(3) . . ?
S1 O4 U1 143.0(3) . . ?
S1 O5 U1 139.2(3) . 2 ?
S2 O8 U1 161.3(5) . . ?
S2 O9 Mn1 132.5(3) . 1_655 ?
S2 O10 Mn1 136.7(3) . . ?
S2 O11 U1 156.3(3) . 2_545 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3A O9 0.97(3) 1.98(7) 2.822(7) 143(8) 1_556
O3 H3B O6 1.00(2) 1.68(2) 2.679(7) 172(9) 1_556

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 O5 U1 100.3(5) . . . 2 ?
O5 S1 O4 U1 -123.7(6) . . . . ?
O6 S1 O4 U1 122.4(6) . . . . ?
O6 S1 O5 U1 -146.3(4) . . . 2 ?
O7 S1 O4 U1 -2.8(7) . . . . ?
O7 S1 O5 U1 -20.9(6) . . . 2 ?
O8 S2 O9 Mn1 90.7(5) . . . 1_655 ?
O8 S2 O10 Mn1 -36.0(7) . . . . ?
O8 S2 O11 U1 50.1(9) . . . 2_545 ?
O9 S2 O8 U1 0.5(14) . . . . ?
O9 S2 O10 Mn1 -157.5(5) . . . . ?
O9 S2 O11 U1 170.2(7) . . . 2_545 ?
O10 S2 O8 U1 -119.9(13) . . . . ?
O10 S2 O9 Mn1 -148.2(4) . . . 1_655 ?
O10 S2 O11 U1 -70.6(9) . . . 2_545 ?
O11 S2 O8 U1 119.3(13) . . . . ?
O11 S2 O9 Mn1 -28.1(5) . . . 1_655 ?
O11 S2 O10 Mn1 83.6(6) . . . . ?

_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 1.581
_oxdiff_exptl_absorpt_empirical_full_min 0.680
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_10
_database_code_depnum_ccdc_archive 'CCDC 2039109'
loop_
_audit_author_name
_audit_author_address
'Ilya Kornyakov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2020-10-17 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_audit_creation_date             2020-10-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_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
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ni4  O60  S2  Se5  U4  '
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   8.39020(10)
_cell_length_b                   11.5601(2)
_cell_length_c                   13.0744(2)
_cell_angle_alpha                90
_cell_angle_beta                 93.3090(10)
_cell_angle_gamma                90
_cell_volume                     1265.99(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13068
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.1980
_cell_measurement_theta_min      2.3150
_shelx_estimated_absorpt_T_max   0.442
_shelx_estimated_absorpt_T_min   0.094
_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_absorpt_special_details   ?
_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_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_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_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2817
_reflns_number_total             2904
_reflns_odcompleteness_completeness 94.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.662
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       .
_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_R_factor_all          0.0147
_refine_ls_R_factor_gt           0.0140
_refine_ls_restrained_S_all      1.144
_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
_refine_special_details          ?
_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)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 ?

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 ?

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_2
_database_code_depnum_ccdc_archive 'CCDC 2039102'
loop_
_audit_author_name
_audit_author_address
'Ilya Kornyakov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2020-10-18 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_audit_creation_date             2020-10-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'H10 Ni O15 S1.85 Se0.15 U'
_chemical_formula_sum            'H10 Ni O15 S1.85 Se0.15 U'
_chemical_formula_weight         617.86
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ni2 U2 S3 O12'
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_H-M_alt        'P m n 21'
_space_group_name_Hall           'P 2ac -2'
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'

_cell_length_a                   12.7808(3)
_cell_length_b                   8.2806(2)
_cell_length_c                   11.3074(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1196.69(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8702
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.2650
_cell_measurement_theta_min      2.3910
_shelx_estimated_absorpt_T_max   0.568
_shelx_estimated_absorpt_T_min   0.127
_exptl_absorpt_coefficient_mu    15.942
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37498
_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_absorpt_special_details   ?
_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    3.429
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1139
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0169
_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       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10729
_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         27.498
_diffrn_reflns_theta_min         2.405
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_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      0.10 332.60   0.50   70.01 -98.65 -34.00 -40.00    --   665
  2  ω   -100.38 -20.38   0.50   70.00    --  -34.00 147.98 -65.98  160
  3  ω    -77.02  -1.52   0.50   70.00    --  -34.00 102.00 134.00  151
  4  ω    241.02 268.02   0.50   70.00    --  -34.00 -89.99 -60.00   54
;
_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      0.0427600000
_diffrn_orient_matrix_UB_12      -0.0541046000
_diffrn_orient_matrix_UB_13      -0.0051994000
_diffrn_orient_matrix_UB_21      -0.0313512000
_diffrn_orient_matrix_UB_22      -0.0631903000
_diffrn_orient_matrix_UB_23      0.0231901000
_diffrn_orient_matrix_UB_31      -0.0164210000
_diffrn_orient_matrix_UB_32      -0.0205022000
_diffrn_orient_matrix_UB_33      -0.0580261000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2575
_reflns_number_total             2756
_reflns_odcompleteness_completeness 96.04
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.19
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         1.430
_refine_diff_density_min         -1.619
_refine_diff_density_rms         0.197
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.068(12)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2756
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0240
_refine_ls_restrained_S_all      1.061
_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)+(0.0419P)²+2.6982P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0645
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.932(12)
 0.068(12)
2. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups, All O(H,H,H) groups
3. Shared sites
{S1, Se1}
{S2, Se2}
4. 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_$10
 2 with sigma of 0.02
 O10_$1-H14_$10
 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_$11-O10_$10
 1.9 with sigma of 0.02
 O10_$10-H10B_$10
 0.98 with sigma of 0.02
 H10B_$10-O7_$2
 1.8 with sigma of 0.02
 O10_$10-H10A_$10
 0.98 with sigma of 0.02
 H10B_$10-H10A_$10
 1.54 with sigma of 0.02
 H10A_$10-O4_$3
 1.8 with sigma of 0.02
 O16_$11-H16_$4
 0.98 with sigma of 0.02
 H16_$11-H16_$4
 1.54 with sigma of 0.02
 H16_$11-O3_$3
 1.9 with sigma of 0.02
 O15_$2-H15_$5
 0.98 with sigma of 0.02
 H15_$2-H15_$5
 1.54 with sigma of 0.02
 H15_$5-O5_$6
 1.9 with sigma of 0.02
 H12_$2-O4_$3
 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_$9-H19
 1.54 with sigma of 0.02
 H19-O5_$8
 1.75 with sigma of 0.02
 O17-H17
 0.98 with sigma of 0.02
 H17-H17_$9
 1.54 with sigma of 0.02
 H17-O11_$7
 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_$9
 1.54 with sigma of 0.02
 O3_$9-H18_$9
 2.4 with sigma of 0.02
5. Uiso/Uaniso restraints and constraints
Uanis(S1) = Uanis(Se1)
Uanis(S2) = Uanis(Se2)
6. Others
 Sof(Se1)=1-FVAR(1)
 Sof(S1)=FVAR(1)
 Sof(Se2)=1-FVAR(2)
 Sof(S2)=FVAR(2)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.25030(2) 1.11309(3) 0.52564(12) 0.00747(11) Uani 1 1 d . . . . .
Se1 Se 0.27412(16) 1.2420(2) 0.83393(17) 0.0089(5) Uani 0.140(8) 1 d . . . A 2
Se2 Se 0.25378(12) 0.7415(3) 0.7150(2) 0.0073(8) Uani 0.008(9) 1 d . . . B .
Ni1 Ni 0.0000 0.66400(18) 0.71108(14) 0.0084(3) Uani 1 2 d S T P B .
Ni2 Ni 0.5000 0.67405(18) 0.67546(14) 0.0094(3) Uani 1 2 d S T P B .
S1 S 0.27412(16) 1.2420(2) 0.83393(17) 0.0089(5) Uani 0.860(8) 1 d . . . A 1
S2 S 0.25378(12) 0.7415(3) 0.7150(2) 0.0073(8) Uani 0.992(9) 1 d . . . B 3
O1 O 0.3810(4) 1.0618(7) 0.4905(5) 0.0128(12) Uani 1 1 d . . . . .
O2 O 0.1197(4) 1.1643(7) 0.5596(5) 0.0126(11) Uani 1 1 d . . . . .
O3 O 0.3152(5) 1.2196(8) 0.7084(6) 0.0232(15) Uani 1 1 d D . . . .
O4 O 0.3267(5) 1.3850(7) 0.8842(7) 0.0203(15) Uani 1 1 d D . . . .
O5 O 0.1586(4) 1.2562(7) 0.8323(6) 0.0134(11) Uani 1 1 d D . . . .
O6 O 0.2343(5) 0.8980(9) 0.6580(9) 0.0220(18) Uani 1 1 d . . . . .
O7 O 0.3408(5) 0.6558(8) 0.6561(6) 0.0154(13) Uani 1 1 d D . . . .
O8 O 0.1610(5) 0.6402(7) 0.7107(7) 0.0152(13) Uani 1 1 d . . . . .
O9 O 0.1918(5) 0.9034(7) 0.4045(6) 0.0190(14) Uani 1 1 d . . . . .
O10 O 0.2981(5) 1.4044(7) 0.5071(6) 0.0155(13) Uani 1 1 d D . . . .
H10A H 0.256(6) 1.464(9) 0.451(6) 0.023 Uiso 1 1 d DR . . . .
H10B H 0.306(8) 1.476(6) 0.575(5) 0.023 Uiso 1 1 d DR . . . .
O11 O 0.2141(5) 1.2272(7) 0.3381(6) 0.0160(11) Uani 1 1 d D . . . .
O12 O 0.0000 0.7069(10) 0.5348(11) 0.0167(18) Uani 1 2 d DS T P . .
H12 H 0.0603(11) 0.670(11) 0.487(4) 0.025 Uiso 1 1 d DR . . . .
O13 O 0.0000 0.9104(11) 0.7419(8) 0.0148(19) Uani 1 2 d DS T P . .
H13 H 0.0599(11) 0.979(7) 0.717(9) 0.022 Uiso 1 1 d DR . . . .
O14 O 0.0000 0.6416(12) 0.8904(9) 0.015(2) Uani 1 2 d DS T P . .
H14 H 0.0601(11) 0.609(10) 0.934(4) 0.023 Uiso 1 1 d DR . . . .
O15 O 0.0000 0.4216(12) 0.6893(9) 0.015(2) Uani 1 2 d DS T P . .
H15 H 0.0601(11) 0.359(9) 0.726(6) 0.023 Uiso 1 1 d DR . . . .
O16 O 0.5000 0.4224(12) 0.6677(10) 0.018(2) Uani 1 2 d DS T P . .
H16 H 0.4397(11) 0.351(6) 0.693(8) 0.028 Uiso 1 1 d DR . . . .
O17 O 0.5000 0.6477(12) 0.8565(9) 0.018(2) Uani 1 2 d DS T P . .
O18 O 0.5000 0.9232(11) 0.6978(8) 0.015(2) Uani 1 2 d DS T P . .
O19 O 0.5000 0.7033(11) 0.4969(8) 0.015(2) Uani 1 2 d DS T P . .
H17 H 0.4393(11) 0.658(8) 0.907(4) 0.022 Uiso 1 1 d DR . . . .
H18 H 0.4398(11) 0.997(4) 0.712(8) 0.022 Uiso 1 1 d DR . . . .
H19 H 0.4398(11) 0.718(11) 0.442(3) 0.022 Uiso 1 1 d DR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.769(5) . ?
U1 O2 1.764(6) . ?
U1 O3 2.395(7) . ?
U1 O6 2.335(8) . ?
U1 O9 2.334(6) . ?
U1 O10 2.497(6) . ?
U1 O11 2.367(7) . ?
Se1 O3 1.525(7) . ?
Se1 O4 1.476(6) . ?
Se1 O5 1.482(5) . ?
Se1 O9 1.509(6) 2_575 ?
Se2 O6 1.469(8) . ?
Se2 O7 1.478(6) . ?
Se2 O8 1.454(6) . ?
Se2 O11 1.474(7) 2_575 ?
Ni1 O8 2.067(6) 3 ?
Ni1 O8 2.067(6) . ?
Ni1 O12 2.024(12) . ?
Ni1 O13 2.070(9) . ?
Ni1 O14 2.036(10) . ?
Ni1 O15 2.022(10) . ?
Ni2 O7 2.052(6) . ?
Ni2 O7 2.053(6) 3_655 ?
Ni2 O16 2.086(10) . ?
Ni2 O17 2.058(11) . ?
Ni2 O18 2.079(9) . ?
Ni2 O19 2.033(9) . ?
S1 O3 1.525(7) . ?
S1 O4 1.476(6) . ?
S1 O5 1.482(5) . ?
S1 O9 1.509(6) 2_575 ?
O9 Se1 1.509(6) 2_574 ?
O9 S1 1.509(6) 2_574 ?
O11 Se2 1.474(7) 2_574 ?
O11 S2 1.474(7) 2_574 ?

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 87.4(2) . . ?
O1 U1 O6 92.5(3) . . ?
O1 U1 O9 89.6(2) . . ?
O1 U1 O10 89.0(2) . . ?
O1 U1 O11 94.5(2) . . ?
O2 U1 O1 179.6(3) . . ?
O2 U1 O3 92.9(2) . . ?
O2 U1 O6 87.8(3) . . ?
O2 U1 O9 90.2(2) . . ?
O2 U1 O10 91.0(2) . . ?
O2 U1 O11 85.1(2) . . ?
O3 U1 O10 68.4(2) . . ?
O6 U1 O3 76.0(3) . . ?
O6 U1 O10 144.3(3) . . ?
O6 U1 O11 149.5(3) . . ?
O9 U1 O3 153.0(2) . . ?
O9 U1 O6 77.3(3) . . ?
O9 U1 O10 138.4(2) . . ?
O9 U1 O11 73.1(2) . . ?
O11 U1 O3 133.9(2) . . ?
O11 U1 O10 65.6(2) . . ?
O4 Se1 O3 107.4(4) . . ?
O4 Se1 O5 113.2(4) . . ?
O4 Se1 O9 107.7(4) . 2_575 ?
O5 Se1 O3 110.0(4) . . ?
O5 Se1 O9 111.0(4) . 2_575 ?
O9 Se1 O3 107.2(4) 2_575 . ?
O6 Se2 O7 110.7(5) . . ?
O6 Se2 O11 107.8(5) . 2_575 ?
O8 Se2 O6 110.9(4) . . ?
O8 Se2 O7 108.8(4) . . ?
O8 Se2 O11 111.1(4) . 2_575 ?
O11 Se2 O7 107.5(4) 2_575 . ?
O8 Ni1 O8 169.1(4) . 3 ?
O8 Ni1 O13 95.41(18) . . ?
O8 Ni1 O13 95.42(18) 3 . ?
O12 Ni1 O8 90.8(2) . 3 ?
O12 Ni1 O8 90.8(2) . . ?
O12 Ni1 O13 89.6(4) . . ?
O12 Ni1 O14 175.1(4) . . ?
O14 Ni1 O8 89.6(2) . . ?
O14 Ni1 O8 89.6(2) . 3 ?
O14 Ni1 O13 85.5(4) . . ?
O15 Ni1 O8 84.55(18) . . ?
O15 Ni1 O8 84.55(18) . 3 ?
O15 Ni1 O12 93.1(4) . . ?
O15 Ni1 O13 177.3(4) . . ?
O15 Ni1 O14 91.8(4) . . ?
O7 Ni2 O7 165.1(4) . 3_655 ?
O7 Ni2 O16 85.52(19) . . ?
O7 Ni2 O16 85.52(19) 3_655 . ?
O7 Ni2 O17 95.6(2) . . ?
O7 Ni2 O17 95.6(2) 3_655 . ?
O7 Ni2 O18 94.94(19) 3_655 . ?
O7 Ni2 O18 94.94(19) . . ?
O17 Ni2 O16 86.3(4) . . ?
O17 Ni2 O18 89.1(4) . . ?
O18 Ni2 O16 175.4(4) . . ?
O19 Ni2 O7 84.4(2) . . ?
O19 Ni2 O7 84.4(2) . 3_655 ?
O19 Ni2 O16 94.4(4) . . ?
O19 Ni2 O17 179.2(4) . . ?
O19 Ni2 O18 90.1(4) . . ?
O4 S1 O3 107.4(4) . . ?
O4 S1 O5 113.2(4) . . ?
O4 S1 O9 107.7(4) . 2_575 ?
O5 S1 O3 110.0(4) . . ?
O5 S1 O9 111.0(4) . 2_575 ?
O9 S1 O3 107.2(4) 2_575 . ?
Se1 O3 U1 136.8(4) . . ?
S1 O3 U1 136.8(4) . . ?
Se2 O6 U1 159.9(6) . . ?
Se2 O7 Ni2 131.5(4) . . ?
Se2 O8 Ni1 139.2(4) . . ?
Se1 O9 U1 144.2(4) 2_574 . ?
S1 O9 U1 144.2(4) 2_574 . ?
Se2 O11 U1 149.5(4) 2_574 . ?
S2 O11 U1 149.5(4) 2_574 . ?
S2 O11 Se2 0.0 2_574 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 Se1 O3 U1 -150.3(5) . . . . ?
O4 S1 O3 U1 -150.3(5) . . . . ?
O5 Se1 O3 U1 -26.6(7) . . . . ?
O5 S1 O3 U1 -26.6(7) . . . . ?
O6 Se2 O7 Ni2 83.1(7) . . . . ?
O6 Se2 O8 Ni1 -31.3(9) . . . . ?
O7 Se2 O6 U1 1.8(17) . . . . ?
O7 Se2 O8 Ni1 -153.2(7) . . . . ?
O8 Se2 O6 U1 -119.0(15) . . . . ?
O8 Se2 O7 Ni2 -154.9(5) . . . . ?
O9 Se1 O3 U1 94.1(6) 2_575 . . . ?
O9 S1 O3 U1 94.1(6) 2_575 . . . ?
O11 Se2 O6 U1 119.1(16) 2_575 . . . ?
O11 Se2 O7 Ni2 -34.5(7) 2_575 . . . ?
O11 Se2 O8 Ni1 88.6(8) 2_575 . . . ?

_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 2.409
_oxdiff_exptl_absorpt_empirical_full_min 0.579
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.932(12)
2 0.068(12)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_11
_database_code_depnum_ccdc_archive 'CCDC 2039113'
loop_
_audit_author_name
_audit_author_address
'Ilya Kornyakov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2020-10-17 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_audit_creation_date             2020-10-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'H10 Ni O15 Se2 U'
_chemical_formula_sum            'H10 Ni O15 Se2 U'
_chemical_formula_weight         704.74
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ni1 U1 Se2 O15'
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'
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   8.3912(2)
_cell_length_b                   11.5652(3)
_cell_length_c                   13.1209(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.533(2)
_cell_angle_gamma                90
_cell_volume                     1270.91(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.2470
_cell_measurement_theta_min      2.3520
_shelx_estimated_absorpt_T_max   0.335
_shelx_estimated_absorpt_T_min   0.068
_exptl_absorpt_coefficient_mu    20.012
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43705
_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_absorpt_special_details   ?
_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    3.683
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0175
_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       5
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12401
_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         2.349
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_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   -338.61 -27.11   0.50   35.01 -52.22 -34.00  82.00    --   623
  2  φ   -306.49   4.01   0.50   35.00-114.28 -34.00 -88.00    --   621
  3  ω    -77.02  -1.52   0.50   35.00    --  -34.00 102.00 134.00  151
;
_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      0.0439251000
_diffrn_orient_matrix_UB_12      -0.0015791000
_diffrn_orient_matrix_UB_13      -0.0444940000
_diffrn_orient_matrix_UB_21      0.0723131000
_diffrn_orient_matrix_UB_22      -0.0027782000
_diffrn_orient_matrix_UB_23      0.0309366000
_diffrn_orient_matrix_UB_31      -0.0044817000
_diffrn_orient_matrix_UB_32      -0.0611861000
_diffrn_orient_matrix_UB_33      -0.0001905000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2643
_reflns_number_total             2919
_reflns_odcompleteness_completeness 94.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.944
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.178
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         2919
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0166
_refine_ls_restrained_S_all      1.033
_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)+(0.0227P)²+3.0421P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0396
_refine_ls_wR_factor_ref         0.0412
_refine_special_details          ?
_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. 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
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.62214(2) 0.40445(2) 0.75324(2) 0.00345(5) Uani 1 1 d . . . . .
Se1 Se 0.26333(4) 0.59525(3) 0.77115(3) 0.00387(7) Uani 1 1 d . . . A 4
Se2 Se 0.75711(4) 0.72018(3) 0.75454(2) 0.00327(7) Uani 1 1 d . . . B 2
Ni1 Ni 0.83915(5) 0.72687(4) 0.50653(3) 0.00531(9) Uani 1 1 d . . . . .
O1 O 0.6956(3) 0.3711(2) 0.87918(19) 0.0078(5) Uani 1 1 d . . . . .
O2 O 0.5497(3) 0.4384(2) 0.62702(19) 0.0076(5) Uani 1 1 d . . . . .
O3 O 0.4178(3) 0.5169(2) 0.81351(19) 0.0079(5) Uani 1 1 d . . . . .
O4 O 0.1064(3) 0.5424(2) 0.8225(2) 0.0106(5) Uani 1 1 d . . . . .
O5 O 0.2466(3) 0.5968(2) 0.6471(2) 0.0102(5) Uani 1 1 d . . . . .
O6 O 0.7381(3) 0.58698(19) 0.7941(2) 0.0069(5) Uani 1 1 d . . . . .
O7 O 0.8301(3) 0.7986(2) 0.84958(19) 0.0076(5) Uani 1 1 d . . . . .
O8 O 0.8785(3) 0.7283(2) 0.66311(19) 0.0086(5) Uani 1 1 d . . . . .
O9 O 0.2903(3) 0.7277(2) 0.81527(19) 0.0084(5) Uani 1 1 d . . . . .
O10 O 0.8963(3) 0.4274(2) 0.6951(2) 0.0082(5) Uani 1 1 d D . . . .
O11 O 0.5793(3) 0.7673(2) 0.71328(19) 0.0071(5) Uani 1 1 d . . . . .
O12 O 0.8236(3) 0.5540(2) 0.5093(2) 0.0150(6) Uani 1 1 d D . . . .
O13 O 1.0822(3) 0.7169(2) 0.4981(2) 0.0098(5) Uani 1 1 d D . . . .
O14 O 0.8589(3) 0.9018(2) 0.5044(2) 0.0109(5) Uani 1 1 d D . . . .
O15 O 0.5949(3) 0.7389(2) 0.5007(2) 0.0133(6) Uani 1 1 d D . . . .
H10A H 0.956(4) 0.366(3) 0.670(3) 0.020 Uiso 1 1 d DR . . . .
H10B H 0.971(4) 0.473(3) 0.737(3) 0.020 Uiso 1 1 d DR . . . .
H12A H 0.807(5) 0.501(3) 0.453(2) 0.020 Uiso 1 1 d DR . . . .
H12B H 0.854(5) 0.505(3) 0.566(2) 0.020 Uiso 1 1 d DR . . . .
H13A H 1.141(5) 0.695(3) 0.558(2) 0.020 Uiso 1 1 d DR . . . .
H13B H 1.126(5) 0.787(2) 0.477(3) 0.020 Uiso 1 1 d DR . . . .
H14A H 0.859(5) 0.950(3) 0.5639(19) 0.020 Uiso 1 1 d DR . . . .
H14B H 0.803(5) 0.946(3) 0.453(2) 0.020 Uiso 1 1 d DR . . . .
H15A H 0.542(5) 0.669(2) 0.482(3) 0.020 Uiso 1 1 d DR . . . .
H15B H 0.546(5) 0.766(3) 0.559(2) 0.020 Uiso 1 1 d DR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.770(3) . ?
U1 O2 1.773(3) . ?
U1 O3 2.329(2) . ?
U1 O6 2.372(2) . ?
U1 O9 2.368(2) 2_646 ?
U1 O10 2.482(3) . ?
U1 O11 2.379(2) 2_646 ?
Se1 O3 1.650(2) . ?
Se1 O4 1.634(2) . ?
Se1 O5 1.625(3) . ?
Se1 O9 1.649(2) . ?
Se2 O6 1.636(2) . ?
Se2 O7 1.631(2) . ?
Se2 O8 1.624(2) . ?
Se2 O11 1.648(2) . ?
Ni1 O7 2.077(2) 4_575 ?
Ni1 O8 2.061(2) . ?
Ni1 O12 2.004(3) . ?
Ni1 O13 2.052(3) . ?
Ni1 O14 2.030(2) . ?
Ni1 O15 2.051(3) . ?
O7 Ni1 2.077(2) 4_576 ?
O9 U1 2.368(2) 2_656 ?
O11 U1 2.379(2) 2_656 ?

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 179.62(12) . . ?
O1 U1 O3 91.49(10) . . ?
O1 U1 O6 82.47(10) . . ?
O1 U1 O9 93.89(10) . 2_646 ?
O1 U1 O10 91.97(10) . . ?
O1 U1 O11 83.85(10) . 2_646 ?
O2 U1 O3 88.65(10) . . ?
O2 U1 O6 97.24(10) . . ?
O2 U1 O9 86.16(10) . 2_646 ?
O2 U1 O10 87.69(10) . . ?
O2 U1 O11 96.53(10) . 2_646 ?
O3 U1 O6 74.13(9) . . ?
O3 U1 O9 149.68(9) . 2_646 ?
O3 U1 O10 139.50(8) . . ?
O3 U1 O11 76.31(9) . 2_646 ?
O6 U1 O10 66.38(8) . . ?
O6 U1 O11 146.94(9) . 2_646 ?
O9 U1 O6 136.17(9) 2_646 . ?
O9 U1 O10 70.14(8) 2_646 . ?
O9 U1 O11 74.65(9) 2_646 2_646 ?
O11 U1 O10 144.16(8) 2_646 . ?
O4 Se1 O3 106.98(13) . . ?
O4 Se1 O9 107.43(13) . . ?
O5 Se1 O3 111.16(13) . . ?
O5 Se1 O4 113.27(14) . . ?
O5 Se1 O9 110.06(12) . . ?
O9 Se1 O3 107.71(13) . . ?
O6 Se2 O11 108.14(12) . . ?
O7 Se2 O6 108.71(12) . . ?
O7 Se2 O11 110.91(12) . . ?
O8 Se2 O6 111.48(13) . . ?
O8 Se2 O7 108.05(13) . . ?
O8 Se2 O11 109.56(13) . . ?
O8 Ni1 O7 169.54(10) . 4_575 ?
O12 Ni1 O7 82.99(10) . 4_575 ?
O12 Ni1 O8 89.79(11) . . ?
O12 Ni1 O13 90.61(11) . . ?
O12 Ni1 O14 179.03(12) . . ?
O12 Ni1 O15 90.14(12) . . ?
O13 Ni1 O7 85.11(10) . 4_575 ?
O13 Ni1 O8 87.42(10) . . ?
O14 Ni1 O7 97.23(10) . 4_575 ?
O14 Ni1 O8 89.86(10) . . ?
O14 Ni1 O13 88.47(11) . . ?
O14 Ni1 O15 90.81(12) . . ?
O15 Ni1 O7 89.84(10) . 4_575 ?
O15 Ni1 O8 97.76(10) . . ?
O15 Ni1 O13 174.76(11) . . ?
Se1 O3 U1 140.53(14) . . ?
Se2 O6 U1 144.39(14) . . ?
Se2 O7 Ni1 131.94(14) . 4_576 ?
Se2 O8 Ni1 131.82(14) . . ?
Se1 O9 U1 135.07(14) . 2_656 ?
Se2 O11 U1 143.04(14) . 2_656 ?

_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 2.493
_oxdiff_exptl_absorpt_empirical_full_min 0.556
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_13
_database_code_depnum_ccdc_archive 'CCDC 2039114'
loop_
_audit_author_name
_audit_author_address
'Ilya Kornyakov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2020-10-18 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_audit_creation_date             2020-10-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Co H10 O15 S2 U'
_chemical_formula_sum            'Co H10 O15 S2 U'
_chemical_formula_weight         611.16
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Co4  O60  S8  U4  '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_H-M_alt        'P m n 21'
_space_group_name_Hall           'P 2ac -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, z+1/2'
'-x, y, z'

_cell_length_a                   12.9160(3)
_cell_length_b                   8.2960(2)
_cell_length_c                   11.2937(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1210.13(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6214
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      36.2760
_cell_measurement_theta_min      2.3770
_shelx_estimated_absorpt_T_max   0.582
_shelx_estimated_absorpt_T_min   0.135
_exptl_absorpt_coefficient_mu    15.161
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53548
_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_absorpt_special_details   ?
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.355
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_unetI/netI     0.0214
_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       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6561
_diffrn_reflns_point_group_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.396
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_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     73.32 318.32   1.00   30.00 -98.65 -34.00 -40.00    --   245
  2  ω    -90.14 -21.14   1.00   30.00    --  -34.00 133.99 116.00   69
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II DUO'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0372948000
_diffrn_orient_matrix_UB_12      -0.0166600000
_diffrn_orient_matrix_UB_13      0.0444421000
_diffrn_orient_matrix_UB_21      0.0398309000
_diffrn_orient_matrix_UB_22      0.0280642000
_diffrn_orient_matrix_UB_23      -0.0380318000
_diffrn_orient_matrix_UB_31      -0.0062994000
_diffrn_orient_matrix_UB_32      0.0790118000
_diffrn_orient_matrix_UB_33      0.0228551000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.774
_reflns_Friedel_fraction_full    0.840
_reflns_Friedel_fraction_max     0.856
_reflns_number_gt                2363
_reflns_number_total             2704
_reflns_odcompleteness_completeness 95.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.866
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details 
;
 Flack x determined using 909 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2704
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0212
_refine_ls_restrained_S_all      1.072
_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)+(0.0227P)²+1.9347P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0457
_refine_ls_wR_factor_ref         0.0479
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups, All O(H,H,H) groups
2. 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_$8
 2 with sigma of 0.02
 O10_$1-H14_$8
 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_$9-O10_$8
 1.9 with sigma of 0.02
 O10_$8-H10B_$8
 0.98 with sigma of 0.02
 H10B_$8-O7_$10
 1.8 with sigma of 0.02
 O10_$8-H10A_$8
 0.98 with sigma of 0.02
 H10B_$8-H10A_$8
 1.54 with sigma of 0.02
 H10A_$8-O4_$11
 1.8 with sigma of 0.02
 O16_$9-H16_$2
 0.98 with sigma of 0.02
 H16_$9-H16_$2
 1.54 with sigma of 0.02
 H16_$9-O3_$11
 1.9 with sigma of 0.02
 O15_$10-H15_$3
 0.98 with sigma of 0.02
 H15_$10-H15_$3
 1.54 with sigma of 0.02
 H15_$3-O5_$4
 1.9 with sigma of 0.02
 H12_$10-O4_$11
 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_$7-H19
 1.54 with sigma of 0.02
 H19-O5_$6
 1.75 with sigma of 0.02
 O17-H17
 0.98 with sigma of 0.02
 H17-H17_$7
 1.54 with sigma of 0.02
 H17-O11_$5
 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_$7
 1.54 with sigma of 0.02
 O3_$7-H18_$7
 2.4 with sigma of 0.02
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.24824(2) 1.11288(2) 0.52536(10) 0.01182(8) Uani 1 1 d . . . . .
Co1 Co 0.0000 0.6634(2) 0.70999(15) 0.0167(4) Uani 1 2 d S T P B .
Co2 Co 0.5000 0.6758(2) 0.67733(16) 0.0213(4) Uani 1 2 d S T P B .
S1 S 0.27403(18) 1.2383(3) 0.8329(2) 0.0160(4) Uani 1 1 d . . . A 1
S2 S 0.25301(13) 0.7425(3) 0.7139(2) 0.0121(5) Uani 1 1 d . . . B 1
O1 O 0.3778(4) 1.0666(7) 0.4909(5) 0.0251(14) Uani 1 1 d . . . . .
O2 O 0.1185(4) 1.1599(7) 0.5593(5) 0.0237(14) Uani 1 1 d . . . . .
O3 O 0.3129(5) 1.2144(8) 0.7097(5) 0.0272(15) Uani 1 1 d D . . . .
O4 O 0.3255(6) 1.3818(7) 0.8813(7) 0.0313(18) Uani 1 1 d D . . . .
O5 O 0.1615(4) 1.2507(9) 0.8344(7) 0.0342(15) Uani 1 1 d D . . . .
O6 O 0.2328(6) 0.8968(9) 0.6562(9) 0.039(2) Uani 1 1 d . . . . .
O7 O 0.3395(5) 0.6597(8) 0.6572(7) 0.0306(16) Uani 1 1 d D . . . .
O8 O 0.1624(5) 0.6413(8) 0.7089(7) 0.0298(17) Uani 1 1 d . . . . .
O9 O 0.1912(5) 0.9006(7) 0.4044(6) 0.0290(16) Uani 1 1 d . . . . .
O10 O 0.2910(6) 1.4053(7) 0.5112(7) 0.0334(17) Uani 1 1 d D . . . .
H10A H 0.249(7) 1.468(9) 0.458(7) 0.050 Uiso 1 1 d DR . . . .
H10B H 0.297(8) 1.475(7) 0.582(5) 0.050 Uiso 1 1 d DR . . . .
O11 O 0.2168(5) 1.2250(8) 0.3367(6) 0.0278(13) Uani 1 1 d D . . . .
O12 O 0.0000 0.7103(13) 0.5319(12) 0.045(3) Uani 1 2 d DS T P . .
H12 H 0.0595(11) 0.665(11) 0.483(5) 0.068 Uiso 1 1 d DR . . . .
O13 O 0.0000 0.9140(11) 0.7427(11) 0.035(3) Uani 1 2 d DS T P . .
H13 H 0.0596(11) 0.975(8) 0.716(9) 0.052 Uiso 1 1 d DR . . . .
O14 O 0.0000 0.6394(14) 0.8906(10) 0.034(3) Uani 1 2 d DS T P . .
H14 H 0.0608(11) 0.620(12) 0.947(4) 0.050 Uiso 1 1 d DR . . . .
O15 O 0.0000 0.4175(12) 0.6927(12) 0.038(3) Uani 1 2 d DS T P . .
H15 H 0.0595(11) 0.368(11) 0.740(7) 0.057 Uiso 1 1 d DR . . . .
O16 O 0.5000 0.4195(13) 0.6669(12) 0.035(3) Uani 1 2 d DS T P . .
H16 H 0.4396(11) 0.347(6) 0.696(8) 0.052 Uiso 1 1 d DR . . . .
O17 O 0.5000 0.6387(14) 0.8609(10) 0.038(3) Uani 1 2 d DS T P . .
O18 O 0.5000 0.9263(12) 0.7126(12) 0.044(3) Uani 1 2 d DS T P . .
O19 O 0.5000 0.7130(13) 0.4971(8) 0.031(3) Uani 1 2 d DS T P . .
H17 H 0.4401(11) 0.677(7) 0.905(4) 0.046 Uiso 1 1 d DR . . . .
H18 H 0.4403(11) 1.000(4) 0.710(10) 0.046 Uiso 1 1 d DR . . . .
H19 H 0.4404(11) 0.726(12) 0.441(3) 0.046 Uiso 1 1 d DR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.760(5) . ?
U1 O2 1.762(5) . ?
U1 O3 2.397(6) . ?
U1 O6 2.331(8) . ?
U1 O9 2.348(6) . ?
U1 O10 2.493(6) . ?
U1 O11 2.360(7) . ?
Co1 O8 2.105(6) 4 ?
Co1 O8 2.105(6) . ?
Co1 O12 2.048(14) . ?
Co1 O13 2.112(9) . ?
Co1 O14 2.049(11) . ?
Co1 O15 2.049(10) . ?
Co2 O7 2.090(6) 4_655 ?
Co2 O7 2.090(6) . ?
Co2 O16 2.130(11) . ?
Co2 O17 2.096(12) . ?
Co2 O18 2.116(10) . ?
Co2 O19 2.059(9) . ?
S1 O3 1.492(6) . ?
S1 O4 1.468(6) . ?
S1 O5 1.458(5) . ?
S1 O9 1.477(6) 2_575 ?
S2 O6 1.461(7) . ?
S2 O7 1.459(6) . ?
S2 O8 1.442(7) . ?
S2 O11 1.466(7) 2_575 ?
O9 S1 1.477(6) 2_574 ?
O11 S2 1.466(7) 2_574 ?

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 179.8(3) . . ?
O1 U1 O3 86.4(2) . . ?
O1 U1 O6 93.1(3) . . ?
O1 U1 O9 90.3(3) . . ?
O1 U1 O10 89.3(3) . . ?
O1 U1 O11 92.9(3) . . ?
O2 U1 O3 93.7(2) . . ?
O2 U1 O6 87.2(3) . . ?
O2 U1 O9 89.7(3) . . ?
O2 U1 O10 90.5(3) . . ?
O2 U1 O11 86.9(2) . . ?
O3 U1 O10 68.7(2) . . ?
O6 U1 O3 75.5(3) . . ?
O6 U1 O9 76.4(3) . . ?
O6 U1 O10 143.9(3) . . ?
O6 U1 O11 149.4(3) . . ?
O9 U1 O3 151.5(2) . . ?
O9 U1 O10 139.7(3) . . ?
O9 U1 O11 73.5(2) . . ?
O11 U1 O3 134.9(2) . . ?
O11 U1 O10 66.2(2) . . ?
O8 Co1 O8 170.0(4) . 4 ?
O8 Co1 O13 94.98(18) 4 . ?
O8 Co1 O13 94.98(18) . . ?
O12 Co1 O8 90.6(2) . . ?
O12 Co1 O8 90.6(2) . 4 ?
O12 Co1 O13 89.1(5) . . ?
O12 Co1 O14 174.6(5) . . ?
O12 Co1 O15 95.5(5) . . ?
O14 Co1 O8 89.8(2) . . ?
O14 Co1 O8 89.8(2) . 4 ?
O14 Co1 O13 85.5(5) . . ?
O14 Co1 O15 89.9(6) . . ?
O15 Co1 O8 85.00(18) . . ?
O15 Co1 O8 85.00(18) . 4 ?
O15 Co1 O13 175.4(5) . . ?
O7 Co2 O7 165.5(4) . 4_655 ?
O7 Co2 O16 86.0(2) 4_655 . ?
O7 Co2 O16 86.0(2) . . ?
O7 Co2 O17 95.6(2) . . ?
O7 Co2 O17 95.6(2) 4_655 . ?
O7 Co2 O18 94.77(19) . . ?
O7 Co2 O18 94.78(19) 4_655 . ?
O17 Co2 O16 84.7(5) . . ?
O17 Co2 O18 87.6(5) . . ?
O18 Co2 O16 172.3(5) . . ?
O19 Co2 O7 84.4(2) . 4_655 ?
O19 Co2 O7 84.4(2) . . ?
O19 Co2 O16 95.4(5) . . ?
O19 Co2 O17 179.8(4) . . ?
O19 Co2 O18 92.2(5) . . ?
O4 S1 O3 107.6(4) . . ?
O4 S1 O9 106.9(4) . 2_575 ?
O5 S1 O3 110.9(4) . . ?
O5 S1 O4 112.9(4) . . ?
O5 S1 O9 110.6(4) . 2_575 ?
O9 S1 O3 107.7(4) 2_575 . ?
O6 S2 O11 108.0(5) . 2_575 ?
O7 S2 O6 110.7(5) . . ?
O7 S2 O11 107.4(4) . 2_575 ?
O8 S2 O6 110.4(4) . . ?
O8 S2 O7 109.3(4) . . ?
O8 S2 O11 111.1(4) . 2_575 ?
S1 O3 U1 137.7(4) . . ?
S2 O6 U1 160.3(6) . . ?
S2 O7 Co2 133.0(4) . . ?
S2 O8 Co1 139.3(4) . . ?
S1 O9 U1 143.9(4) 2_574 . ?
S2 O11 U1 151.8(4) 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 -147.7(5) . . . . ?
O5 S1 O3 U1 -23.7(7) . . . . ?
O6 S2 O7 Co2 84.0(7) . . . . ?
O6 S2 O8 Co1 -32.5(10) . . . . ?
O7 S2 O6 U1 -0.4(17) . . . . ?
O7 S2 O8 Co1 -154.5(7) . . . . ?
O8 S2 O6 U1 -121.5(15) . . . . ?
O8 S2 O7 Co2 -154.2(6) . . . . ?
O9 S1 O3 U1 97.4(6) 2_575 . . . ?
O11 S2 O6 U1 116.9(16) 2_575 . . . ?
O11 S2 O7 Co2 -33.6(8) 2_575 . . . ?
O11 S2 O8 Co1 87.2(8) 2_575 . . . ?

_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 1.553
_oxdiff_exptl_absorpt_empirical_full_min 0.585
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_3
_database_code_depnum_ccdc_archive 'CCDC 2039112'
loop_
_audit_author_name
_audit_author_address
'Ilya Kornyakov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2020-10-18 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_audit_creation_date             2020-10-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'H10 Ni O15 S1.64 Se0.36 U'
_chemical_formula_sum            'H10 Ni O15 S1.64 Se0.35 U'
_chemical_formula_weight         627.59
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ni4  O60  S8 U4  '
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_H-M_alt        'P m n 21'
_space_group_name_Hall           'P 2ac -2'
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'

_cell_length_a                   12.7830(4)
_cell_length_b                   8.2863(3)
_cell_length_c                   11.3033(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1197.28(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14065
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.3430
_cell_measurement_theta_min      1.5730
_shelx_estimated_absorpt_T_max   0.351
_shelx_estimated_absorpt_T_min   0.099
_exptl_absorpt_coefficient_mu    16.528
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57148
_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_absorpt_special_details   ?
_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    3.482
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1154
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_av_unetI/netI     0.0107
_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       -11
_diffrn_reflns_number            11259
_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         27.493
_diffrn_reflns_theta_min         2.405
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_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   -320.82   6.18   0.50   60.00 -98.65 -34.00 -40.00    --   654
  2  φ   -169.47   9.03   0.50   59.99 -52.22 -34.00  82.00    --   357
  3  ω    -90.77 -14.77   0.50   60.00    --  -34.00 133.99 116.00  152
;
_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      -0.0449325000
_diffrn_orient_matrix_UB_12      0.0499900000
_diffrn_orient_matrix_UB_13      -0.0041736000
_diffrn_orient_matrix_UB_21      -0.0325697000
_diffrn_orient_matrix_UB_22      -0.0682634000
_diffrn_orient_matrix_UB_23      0.0089935000
_diffrn_orient_matrix_UB_31      0.0017701000
_diffrn_orient_matrix_UB_32      0.0134188000
_diffrn_orient_matrix_UB_33      0.0618723000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2611
_reflns_number_total             2669
_reflns_odcompleteness_completeness 96.44
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.18
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.152
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.991(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2669
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0165
_refine_ls_R_factor_gt           0.0159
_refine_ls_restrained_S_all      1.139
_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)+(0.0231P)²+2.5252P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0419
_refine_ls_wR_factor_ref         0.0422
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.009(8)
 0.991(8)
2. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups, All O(H,H,H) groups
3. Shared sites
{S1, Se1}
{S2, Se2}
4. 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_$10
 2 with sigma of 0.02
 O10_$1-H14_$10
 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_$11-O10_$10
 1.9 with sigma of 0.02
 O10_$10-H10B_$10
 0.98 with sigma of 0.02
 H10B_$10-O7_$2
 1.8 with sigma of 0.02
 O10_$10-H10A_$10
 0.98 with sigma of 0.02
 H10B_$10-H10A_$10
 1.54 with sigma of 0.02
 H10A_$10-O4_$3
 1.8 with sigma of 0.02
 O16_$11-H16_$4
 0.98 with sigma of 0.02
 H16_$11-H16_$4
 1.54 with sigma of 0.02
 H16_$11-O3_$3
 1.9 with sigma of 0.02
 O15_$2-H15_$5
 0.98 with sigma of 0.02
 H15_$2-H15_$5
 1.54 with sigma of 0.02
 H15_$5-O5_$6
 1.9 with sigma of 0.02
 H12_$2-O4_$3
 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_$9-H19
 1.54 with sigma of 0.02
 H19-O5_$8
 1.75 with sigma of 0.02
 O17-H17
 0.98 with sigma of 0.02
 H17-H17_$9
 1.54 with sigma of 0.02
 H17-O11_$7
 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_$9
 1.54 with sigma of 0.02
 O3_$9-H18_$9
 2.4 with sigma of 0.02
5. Uiso/Uaniso restraints and constraints
Uanis(S1) = Uanis(Se1)
Uanis(S2) = Uanis(Se2)
6. Others
 Sof(Se1)=1-FVAR(1)
 Sof(S1)=FVAR(1)
 Sof(Se2)=1-FVAR(2)
 Sof(S2)=FVAR(2)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.25011(2) 1.11353(2) 0.52542(8) 0.00681(7) Uani 1 1 d . . . . .
Se1 Se 0.27526(9) 1.24288(13) 0.83426(10) 0.0080(3) Uani 0.319(5) 1 d . . . A 2
Se2 Se 0.25380(8) 0.7424(2) 0.71520(15) 0.0060(5) Uani 0.037(6) 1 d . . . B .
Ni1 Ni 0.0000 0.66480(12) 0.71175(10) 0.0078(2) Uani 1 2 d S T P B .
Ni2 Ni 0.5000 0.67475(13) 0.67465(10) 0.0089(2) Uani 1 2 d S T P B .
S1 S 0.27526(9) 1.24288(13) 0.83426(10) 0.0080(3) Uani 0.681(5) 1 d . . . A 1
S2 S 0.25380(8) 0.7424(2) 0.71520(15) 0.0060(5) Uani 0.963(6) 1 d . . . B 3
O1 O 0.3804(3) 1.0613(5) 0.4894(4) 0.0123(8) Uani 1 1 d . . . . .
O2 O 0.1197(3) 1.1653(5) 0.5607(4) 0.0132(8) Uani 1 1 d . . . . .
O3 O 0.3174(4) 1.2197(6) 0.7066(4) 0.0230(11) Uani 1 1 d D . . . .
O4 O 0.3286(4) 1.3897(5) 0.8855(5) 0.0216(11) Uani 1 1 d D . . . .
O5 O 0.1571(3) 1.2575(5) 0.8324(4) 0.0153(8) Uani 1 1 d D . . . .
O6 O 0.2346(4) 0.9008(7) 0.6589(6) 0.0261(14) Uani 1 1 d . . . . .
O7 O 0.3411(3) 0.6575(6) 0.6554(4) 0.0161(9) Uani 1 1 d D . . . .
O8 O 0.1609(3) 0.6409(5) 0.7103(4) 0.0146(9) Uani 1 1 d . . . . .
O9 O 0.1905(4) 0.9040(5) 0.4063(4) 0.0206(10) Uani 1 1 d . . . . .
O10 O 0.2982(3) 1.4049(5) 0.5068(4) 0.0153(9) Uani 1 1 d D . . . .
H10A H 0.250(4) 1.454(6) 0.452(5) 0.023 Uiso 1 1 d DR . . . .
H10B H 0.304(6) 1.477(5) 0.574(4) 0.023 Uiso 1 1 d DR . . . .
O11 O 0.2144(3) 1.2276(5) 0.3384(4) 0.0177(8) Uani 1 1 d D . . . .
O12 O 0.0000 0.7090(8) 0.5351(7) 0.0177(13) Uani 1 2 d DS T P . .
H12 H 0.0608(11) 0.676(9) 0.488(4) 0.026 Uiso 1 1 d DR . . . .
O13 O 0.0000 0.9101(7) 0.7442(6) 0.0149(13) Uani 1 2 d DS T P . .
H13 H 0.0596(11) 0.987(5) 0.736(7) 0.022 Uiso 1 1 d DR . . . .
O14 O 0.0000 0.6424(8) 0.8892(6) 0.0145(13) Uani 1 2 d DS T P . .
H14 H 0.0605(11) 0.601(7) 0.928(4) 0.022 Uiso 1 1 d DR . . . .
O15 O 0.0000 0.4236(8) 0.6887(6) 0.0135(14) Uani 1 2 d DS T P . .
H15 H 0.0603(11) 0.363(7) 0.724(5) 0.020 Uiso 1 1 d DR . . . .
O16 O 0.5000 0.4239(9) 0.6659(7) 0.0193(14) Uani 1 2 d DS T P . .
H16 H 0.4398(11) 0.356(5) 0.696(6) 0.029 Uiso 1 1 d DR . . . .
O17 O 0.5000 0.6482(9) 0.8538(6) 0.0183(14) Uani 1 2 d DS T P . .
O18 O 0.5000 0.9213(8) 0.6965(5) 0.0147(14) Uani 1 2 d DS T P . .
O19 O 0.5000 0.7037(8) 0.4966(5) 0.0137(15) Uani 1 2 d DS T P . .
H17 H 0.4396(10) 0.657(7) 0.905(4) 0.021 Uiso 1 1 d DR . . . .
H18 H 0.4395(11) 0.991(4) 0.719(6) 0.021 Uiso 1 1 d DR . . . .
H19 H 0.4397(11) 0.721(8) 0.445(3) 0.021 Uiso 1 1 d DR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 1.769(4) . ?
U1 O2 1.767(4) . ?
U1 O3 2.389(5) . ?
U1 O6 2.329(5) . ?
U1 O9 2.325(4) . ?
U1 O10 2.500(4) . ?
U1 O11 2.360(5) . ?
Se1 O3 1.552(5) . ?
Se1 O4 1.510(5) . ?
Se1 O5 1.516(4) . ?
Se1 O9 1.528(4) 2_575 ?
Se2 O6 1.479(5) . ?
Se2 O7 1.482(4) . ?
Se2 O8 1.456(4) . ?
Se2 O11 1.472(5) 2_575 ?
Ni1 O8 2.066(4) . ?
Ni1 O8 2.066(4) 3 ?
Ni1 O12 2.030(9) . ?
Ni1 O13 2.065(6) . ?
Ni1 O14 2.015(7) . ?
Ni1 O15 2.015(7) . ?
Ni2 O7 2.048(4) . ?
Ni2 O7 2.048(4) 3_655 ?
Ni2 O16 2.081(7) . ?
Ni2 O17 2.037(7) . ?
Ni2 O18 2.058(7) . ?
Ni2 O19 2.027(6) . ?
S1 O3 1.552(5) . ?
S1 O4 1.510(5) . ?
S1 O5 1.516(4) . ?
S1 O9 1.528(4) 2_575 ?
O9 Se1 1.528(4) 2_574 ?
O9 S1 1.528(4) 2_574 ?
O11 Se2 1.472(5) 2_574 ?
O11 S2 1.472(5) 2_574 ?

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 87.06(17) . . ?
O1 U1 O6 92.54(18) . . ?
O1 U1 O9 89.56(18) . . ?
O1 U1 O10 89.18(17) . . ?
O1 U1 O11 94.24(17) . . ?
O2 U1 O1 179.7(2) . . ?
O2 U1 O3 93.23(17) . . ?
O2 U1 O6 87.53(19) . . ?
O2 U1 O9 90.18(18) . . ?
O2 U1 O10 90.92(17) . . ?
O2 U1 O11 85.56(17) . . ?
O3 U1 O10 68.16(16) . . ?
O6 U1 O3 75.8(2) . . ?
O6 U1 O10 143.7(2) . . ?
O6 U1 O11 150.1(2) . . ?
O9 U1 O3 152.76(18) . . ?
O9 U1 O6 77.4(2) . . ?
O9 U1 O10 138.85(17) . . ?
O9 U1 O11 73.57(17) . . ?
O11 U1 O3 133.63(16) . . ?
O11 U1 O10 65.52(15) . . ?
O4 Se1 O3 107.4(3) . . ?
O4 Se1 O5 113.0(3) . . ?
O4 Se1 O9 107.9(3) . 2_575 ?
O5 Se1 O3 110.0(3) . . ?
O5 Se1 O9 110.9(2) . 2_575 ?
O9 Se1 O3 107.3(3) 2_575 . ?
O6 Se2 O7 110.5(3) . . ?
O8 Se2 O6 111.1(3) . . ?
O8 Se2 O7 108.8(3) . . ?
O8 Se2 O11 111.0(3) . 2_575 ?
O11 Se2 O6 107.6(3) 2_575 . ?
O11 Se2 O7 107.7(3) 2_575 . ?
O8 Ni1 O8 169.0(3) 3 . ?
O12 Ni1 O8 90.56(15) . . ?
O12 Ni1 O8 90.56(15) . 3 ?
O12 Ni1 O13 89.8(3) . . ?
O13 Ni1 O8 95.50(13) . 3 ?
O13 Ni1 O8 95.50(13) . . ?
O14 Ni1 O8 89.93(15) . . ?
O14 Ni1 O8 89.93(15) . 3 ?
O14 Ni1 O12 174.9(3) . . ?
O14 Ni1 O13 85.1(3) . . ?
O14 Ni1 O15 92.1(3) . . ?
O15 Ni1 O8 84.48(13) . 3 ?
O15 Ni1 O8 84.48(13) . . ?
O15 Ni1 O12 93.0(3) . . ?
O15 Ni1 O13 177.2(3) . . ?
O7 Ni2 O7 165.4(3) . 3_655 ?
O7 Ni2 O16 85.71(14) . . ?
O7 Ni2 O16 85.71(14) 3_655 . ?
O7 Ni2 O18 94.70(13) 3_655 . ?
O7 Ni2 O18 94.70(13) . . ?
O17 Ni2 O7 95.62(14) . 3_655 ?
O17 Ni2 O7 95.62(14) . . ?
O17 Ni2 O16 86.5(3) . . ?
O17 Ni2 O18 89.3(3) . . ?
O18 Ni2 O16 175.8(3) . . ?
O19 Ni2 O7 84.43(14) . 3_655 ?
O19 Ni2 O7 84.43(14) . . ?
O19 Ni2 O16 94.1(3) . . ?
O19 Ni2 O17 179.4(3) . . ?
O19 Ni2 O18 90.1(3) . . ?
O4 S1 O3 107.4(3) . . ?
O4 S1 O5 113.0(3) . . ?
O4 S1 O9 107.9(3) . 2_575 ?
O5 S1 O3 110.0(3) . . ?
O5 S1 O9 110.9(2) . 2_575 ?
O9 S1 O3 107.3(3) 2_575 . ?
Se1 O3 U1 135.9(3) . . ?
S1 O3 U1 135.9(3) . . ?
Se2 O6 U1 159.4(4) . . ?
Se2 O7 Ni2 131.7(3) . . ?
Se2 O8 Ni1 139.1(3) . . ?
Se1 O9 U1 144.0(3) 2_574 . ?
S1 O9 U1 144.0(3) 2_574 . ?
Se2 O11 U1 149.5(3) 2_574 . ?
S2 O11 U1 149.5(3) 2_574 . ?
S2 O11 Se2 0.0 2_574 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 Se1 O3 U1 -149.6(4) . . . . ?
O4 S1 O3 U1 -149.6(4) . . . . ?
O5 Se1 O3 U1 -26.2(5) . . . . ?
O5 S1 O3 U1 -26.2(5) . . . . ?
O6 Se2 O7 Ni2 83.1(5) . . . . ?
O6 Se2 O8 Ni1 -31.6(6) . . . . ?
O7 Se2 O6 U1 4.7(12) . . . . ?
O7 Se2 O8 Ni1 -153.5(4) . . . . ?
O8 Se2 O6 U1 -116.2(11) . . . . ?
O8 Se2 O7 Ni2 -154.6(4) . . . . ?
O9 Se1 O3 U1 94.6(4) 2_575 . . . ?
O9 S1 O3 U1 94.6(4) 2_575 . . . ?
O11 Se2 O6 U1 122.0(11) 2_575 . . . ?
O11 Se2 O7 Ni2 -34.2(5) 2_575 . . . ?
O11 Se2 O8 Ni1 88.2(5) 2_575 . . . ?

_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 1.651
_oxdiff_exptl_absorpt_empirical_full_min 0.434
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.009(8)
2 0.991(8)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_12
_database_code_depnum_ccdc_archive 'CCDC 2039110'
loop_
_audit_author_name
_audit_author_address
'Ilya Kornyakov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2020-10-18 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_audit_creation_date             2020-10-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'H10 O15 S2 U Zn'
_chemical_formula_sum            'H10 O15 S2 U Zn'
_chemical_formula_weight         617.60
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Zn1 U1 S2 O15'
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_H-M_alt        'P m n 21'
_space_group_name_Hall           'P 2ac -2'
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'

_cell_length_a                   12.8695(3)
_cell_length_b                   8.28206(15)
_cell_length_c                   11.2920(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1203.57(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10459
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      36.2010
_cell_measurement_theta_min      2.3650
_shelx_estimated_absorpt_T_max   0.504
_shelx_estimated_absorpt_T_min   0.153
_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_absorpt_special_details   ?
_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_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_ambient_temperature      296(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_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_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_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_odcompleteness_completeness 96.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.04
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_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_coef       .
_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_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0205
_refine_ls_restrained_S_all      1.047
_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
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_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
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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_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_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 . . . ?

_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_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 -0.020(11)
2 1.020(11)

