# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_ui_36_thinplate150816_auto
_database_code_depnum_ccdc_archive 'CCDC 2332264'
loop_
_audit_author_name
_audit_author_address
'Mohammad Shohel'
;Oregon State University
United States of America
;
_audit_update_record             
;
2024-02-11 deposited with the CCDC.	2024-05-06 downloaded from the CCDC.
;
_audit_creation_date             2023-07-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H6 Na O14 Re U2'
_chemical_formula_sum            'C4 H6 Na O14 Re U2'
_chemical_formula_weight         963.34
_chemical_melting_point          ?
_chemical_oxdiff_formula         'U Re2 O12'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   15.2417(5)
_cell_length_b                   8.1267(2)
_cell_length_c                   15.0583(5)
_cell_angle_alpha                90
_cell_angle_beta                 113.798(4)
_cell_angle_gamma                90
_cell_volume                     1706.60(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6401
_cell_measurement_temperature    223.00(10)
_cell_measurement_theta_max      77.1190
_cell_measurement_theta_min      3.2010
_shelx_estimated_absorpt_T_max   0.553
_shelx_estimated_absorpt_T_min   0.174
_exptl_absorpt_coefficient_mu    67.259
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.749
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1669
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.236
_diffrn_reflns_theta_min         3.208
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      223.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -68.00 -33.00   0.50    6.00    --  -47.14 125.00 120.00   70
  2  ω    -70.00   1.00   0.50    6.00    --  -47.14  77.00 -60.00  142
  3  ω   -119.00 -93.00   0.50    6.00    --  -47.14-125.00-180.00   52
  4  ω    -26.00  25.00   0.50    6.00    --  -47.14  19.00  60.00  102
  5  ω    -41.00  25.00   0.50    6.00    --  -47.14  37.00-180.00  132
  6  ω   -119.00 -79.00   0.50    6.00    --  -47.14-125.00 -30.00   80
  7  ω     48.00  84.00   0.50    6.00    --   47.14-125.00-180.00   72
  8  ω     84.00 114.00   0.50    6.00    --   47.14  57.00 -90.00   60
  9  ω     33.00  66.00   0.50    6.00    --   47.14  57.00 -90.00   66
 10  ω     94.00 119.00   0.50    6.00    --   47.14  77.00-150.00   50
 11  ω     89.00 117.00   0.50    6.00    --   47.14  77.00 150.00   56
 12  ω     41.00 105.00   0.50    8.00    --  107.75 -77.00  60.00  128
 13  ω     36.00  70.00   0.50    8.00    --  107.75 -88.00  58.18   68
 14  ω     95.00 131.00   0.50    8.00    --  107.75  45.00 120.00   72
 15  ω     99.00 178.00   0.50    8.00    --  107.75  15.00  60.00  158
 16  ω    124.00 177.00   0.50    8.00    --  107.75  15.00 150.00  106
 17  ω     87.00 134.00   0.50    8.00    --  107.75 -87.00 -43.15   94
 18  ω     35.00  70.00   0.50    8.00    --  107.75 -88.00 168.77   70
 19  ω     36.00  66.00   0.50    8.00    --  107.75 -61.00   0.00   60
 20  ω     94.00 120.00   0.50    8.00    --  107.75  15.00 150.00   52
 21  ω     45.00 103.00   0.50    8.00    --  107.75 -77.00 -90.00  116
 22  ω     65.00  91.00   0.50    8.00    --  107.75 -77.00   0.00   52
 23  ω     37.00  70.00   0.50    8.00    --  107.75 -61.00-180.00   66
 24  ω    103.00 175.00   0.50    8.00    --  107.75  45.00 -90.00  144
 25  ω     44.00  71.00   0.50    8.00    --  107.75 -61.00 150.00   54
 26  ω     39.00  65.00   0.50    8.00    --  107.75 -61.00 -90.00   52
 27  ω     38.00  64.00   0.50    8.00    --  107.75 -87.00 -43.15   52
 28  ω     95.00 151.00   0.50    8.00    --  107.75 125.00 120.00  112
 29  ω     37.00  68.00   0.50    8.00    --  107.75 -61.00 120.00   62
 30  ω    145.00 171.00   0.50    8.00    --  107.75  45.00 120.00   52
 31  ω     44.00  70.00   0.50    8.00    --  107.75 -61.00 -60.00   52
 32  ω     50.00 102.00   0.50    8.00    --  107.75 -77.00 120.00  104
 33  ω    143.00 169.00   0.50    8.00    --  107.75  15.00  90.00   52
 34  ω    107.00 133.00   0.50    8.00    --  107.75  15.00  90.00   52
 35  ω    101.00 177.00   0.50    8.00    --  107.75  45.00   0.00  152
 36  ω     37.00  62.00   0.50    8.00    --  107.75 -61.00  60.00   50
 37  ω     67.00 109.00   0.50    8.00    --  107.75-125.00-120.00   84
 38  ω     78.00 122.00   0.50    8.00    --  107.75 -88.00  58.18   88
 39  ω     85.00 130.00   0.50    8.00    --  107.75 -88.00 168.77   90
 40  ω     91.00 139.00   0.50    8.00    --  107.75  61.00-120.00   96
 41  ω     98.00 136.00   0.50    8.00    --  107.75 -88.00-124.15   76
 42  ω     50.00 103.00   0.50    8.00    --  107.75 -77.00 -30.00  106
 43  ω     49.00 108.00   0.50    8.00    --  107.75-125.00 -90.00  118
 44  ω     60.00  94.00   0.50    8.00    --  107.75 -88.00-124.15   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0718701000
_diffrn_orient_matrix_UB_12      0.0981859000
_diffrn_orient_matrix_UB_13      -0.0274936000
_diffrn_orient_matrix_UB_21      0.0045721000
_diffrn_orient_matrix_UB_22      -0.1430442000
_diffrn_orient_matrix_UB_23      -0.0651208000
_diffrn_orient_matrix_UB_31      -0.0837444000
_diffrn_orient_matrix_UB_32      0.0764085000
_diffrn_orient_matrix_UB_33      -0.0866439000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1546
_reflns_number_total             1669
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         6.709
_refine_diff_density_min         -8.171
_refine_diff_density_rms         0.618
_refine_ls_extinction_coef       0.00012(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1669
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0698
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1277P)²+100.4844P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.1941
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.514(6)
 0.486(6)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 Fixed Sof: Re4(0.25) O13(0.25) H16A(0.5) H16B(0.5) H16C(0.5) O12(0.5)
 Re3(0.25) H17A(0.5) H17B(0.5) H17C(0.5) O1(0.25)
4.a Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_atom_sites_solution_hydrogens   geom
_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 0.62195(5) 0.500000 0.49937(6) 0.0194(4) Uani 1 2 d S T P . .
U2 U 0.39990(6) 0.500000 0.25008(6) 0.0279(4) Uani 1 2 d S T P . .
O9 O 0.6252(10) 0.283(2) 0.5005(12) 0.040(4) Uani 1 1 d . . . . .
O7 O 0.4629(15) 0.500000 0.4073(14) 0.032(4) Uiso 1 2 d S . P . .
O6 O 0.3995(13) 0.719(2) 0.2470(10) 0.049(5) Uani 1 1 d . . . . .
O18 O 0.2759(16) 0.500000 0.3133(16) 0.036(5) Uiso 1 2 d S . P . .
Re4 Re 0.1658(2) 0.500000 -0.0071(2) 0.0300(7) Uiso 0.5 2 d S . P . .
O11 O 0.250(2) 0.500000 0.113(2) 0.056(6) Uiso 1 2 d S . P . .
O13 O 0.228(4) 0.500000 -0.079(4) 0.050(12) Uiso 0.5 2 d S . P . .
O8 O 0.5711(16) 0.500000 0.3108(15) 0.036(5) Uiso 1 2 d S . P . .
O10 O 0.7217(14) 0.500000 0.3991(14) 0.036(5) Uani 1 2 d S T P . .
O19 O 0.1966(13) 0.500000 0.4028(14) 0.033(5) Uani 1 2 d S T P . .
C15 C 0.193(2) 0.500000 0.314(2) 0.037(7) Uiso 1 2 d S . P . .
O5 O 0.437(2) 0.500000 0.1033(19) 0.076(10) Uani 1 2 d S T P . .
C14 C 0.659(2) 0.500000 0.322(2) 0.043(9) Uani 1 2 d S T P . .
C16 C 0.108(4) 0.500000 0.229(4) 0.082(15) Uiso 1 2 d S . P . .
H16A H 0.061709 0.573760 0.236550 0.123 Uiso 0.5 1 calc R U P A -1
H16B H 0.081791 0.389517 0.215900 0.123 Uiso 0.5 1 calc R U P A -1
H16C H 0.122126 0.536723 0.174422 0.123 Uiso 0.5 1 calc R U P A -1
O12 O 0.105(4) 0.290(7) -0.020(4) 0.078(14) Uiso 0.5 1 d . . P . .
O21 O 0.5471(17) 0.000000 0.6216(17) 0.040(5) Uani 1 2 d S T P . .
Re3 Re 0.1724(3) 0.4311(6) -0.0066(3) 0.0400(9) Uiso 0.25 1 d . . P . .
Na20 Na 0.3872(7) 0.000000 0.4990(8) 0.026(2) Uani 1 2 d S T P . .
C17 C 0.680(4) 0.500000 0.229(3) 0.073(13) Uiso 1 2 d S . P . .
H17A H 0.743936 0.458860 0.244406 0.110 Uiso 0.5 1 calc R U P B -1
H17B H 0.674338 0.611281 0.203977 0.110 Uiso 0.5 1 calc R U P B -1
H17C H 0.633516 0.429859 0.180264 0.110 Uiso 0.5 1 calc R U P B -1
O1 O 0.087(4) 0.355(7) -0.039(4) 0.022(10) Uiso 0.25 1 d . . P . .


_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 U1 3.7253(15) 5_666 ?
U1 U2 3.9106(11) . ?
U1 U2 3.9192(12) 5_666 ?
U1 O9 1.763(18) 6_565 ?
U1 O9 1.763(18) . ?
U1 O7 2.26(2) 5_666 ?
U1 O7 2.25(2) . ?
U1 O18 2.62(2) 5_666 ?
U1 O8 2.62(2) . ?
U1 O10 2.54(2) . ?
U1 O19 2.555(18) 5_666 ?
U1 C14 2.94(3) . ?
U2 O7 2.167(19) . ?
U2 O6 1.78(2) . ?
U2 O6 1.78(2) 6_565 ?
U2 O18 2.44(2) . ?
U2 O11 2.38(3) . ?
U2 O8 2.39(2) . ?
U2 O5 2.49(3) . ?
O9 Na20 2.309(17) 5_656 ?
O18 C15 1.27(4) . ?
Re4 O11 1.74(3) . ?
Re4 O13 1.70(5) . ?
Re4 O12 1.91(5) 6_565 ?
Re4 O12 1.91(5) . ?
Re4 Re3 0.568(5) 6_565 ?
Re4 Re3 0.568(5) . ?
Re4 O1 1.61(5) 6_565 ?
Re4 O1 1.61(5) . ?
O11 Re3 1.80(3) . ?
O11 Re3 1.80(3) 6_565 ?
O13 Re3 1.72(5) 6_565 ?
O13 Re3 1.72(5) . ?
O8 C14 1.29(4) . ?
O10 C14 1.17(4) . ?
O10 Na20 2.36(2) 3 ?
O19 C15 1.32(4) . ?
O19 Na20 2.31(2) 7_556 ?
C15 C16 1.41(6) . ?
C14 C17 1.56(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
O12 Re3 1.50(5) . ?
O12 Re3 2.46(6) 6_565 ?
O12 O1 0.60(6) . ?
O21 Na20 2.39(3) . ?
O21 Na20 2.40(2) 5_656 ?
Re3 Re3 1.120(10) 6_565 ?
Re3 O1 2.10(5) 6_565 ?
Re3 O1 1.34(5) . ?
Na20 Na20 3.425(19) 5_656 ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 H17C 0.9700 . ?

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
U1 U1 U2 61.71(3) 5_666 . ?
U1 U1 U2 61.47(3) 5_666 5_666 ?
U2 U1 U2 123.18(2) . 5_666 ?
O9 U1 U1 91.4(5) 6_565 5_666 ?
O9 U1 U1 91.4(5) . 5_666 ?
O9 U1 U2 91.1(5) 6_565 . ?
O9 U1 U2 90.2(5) 6_565 5_666 ?
O9 U1 U2 91.1(5) . . ?
O9 U1 U2 90.2(5) . 5_666 ?
O9 U1 O9 177.1(9) 6_565 . ?
O9 U1 O7 90.9(5) 6_565 5_666 ?
O9 U1 O7 91.4(5) 6_565 . ?
O9 U1 O7 91.4(5) . . ?
O9 U1 O7 90.9(5) . 5_666 ?
O9 U1 O18 89.3(5) . 5_666 ?
O9 U1 O18 89.3(5) 6_565 5_666 ?
O9 U1 O8 90.3(5) 6_565 . ?
O9 U1 O8 90.3(5) . . ?
O9 U1 O10 89.1(5) 6_565 . ?
O9 U1 O10 89.1(5) . . ?
O9 U1 O19 88.6(5) . 5_666 ?
O9 U1 O19 88.6(5) 6_565 5_666 ?
O9 U1 C14 89.6(5) 6_565 . ?
O9 U1 C14 89.6(5) . . ?
O7 U1 U1 34.4(5) 5_666 5_666 ?
O7 U1 U1 34.5(5) . 5_666 ?
O7 U1 U2 96.1(5) 5_666 . ?
O7 U1 U2 27.1(5) 5_666 5_666 ?
O7 U1 U2 96.0(5) . 5_666 ?
O7 U1 U2 27.2(5) . . ?
O7 U1 O7 68.9(8) . 5_666 ?
O7 U1 O18 64.6(7) 5_666 5_666 ?
O7 U1 O18 133.4(8) . 5_666 ?
O7 U1 O8 132.7(7) 5_666 . ?
O7 U1 O8 63.9(7) . . ?
O7 U1 O10 112.8(7) . . ?
O7 U1 O10 178.3(6) 5_666 . ?
O7 U1 O19 177.6(7) . 5_666 ?
O7 U1 O19 113.5(7) 5_666 5_666 ?
O7 U1 C14 89.8(8) . . ?
O7 U1 C14 158.6(9) 5_666 . ?
O18 U1 U1 98.9(5) 5_666 5_666 ?
O18 U1 U2 160.7(5) 5_666 . ?
O18 U1 U2 37.5(5) 5_666 5_666 ?
O18 U1 O8 162.7(6) 5_666 . ?
O18 U1 C14 136.8(8) 5_666 . ?
O8 U1 U1 98.4(5) . 5_666 ?
O8 U1 U2 159.8(5) . 5_666 ?
O8 U1 U2 36.7(5) . . ?
O8 U1 C14 25.9(8) . . ?
O10 U1 U1 147.3(4) . 5_666 ?
O10 U1 U2 85.6(4) . . ?
O10 U1 U2 151.2(4) . 5_666 ?
O10 U1 O18 113.8(7) . 5_666 ?
O10 U1 O8 48.9(7) . . ?
O10 U1 O19 64.8(6) . 5_666 ?
O10 U1 C14 23.0(8) . . ?
O19 U1 U1 147.9(4) 5_666 5_666 ?
O19 U1 U2 150.4(4) 5_666 . ?
O19 U1 U2 86.4(4) 5_666 5_666 ?
O19 U1 O18 48.9(6) 5_666 5_666 ?
O19 U1 O8 113.7(7) 5_666 . ?
O19 U1 C14 87.9(8) 5_666 . ?
C14 U1 U1 124.2(7) . 5_666 ?
C14 U1 U2 174.3(7) . 5_666 ?
C14 U1 U2 62.5(7) . . ?
U1 U2 U1 56.82(2) . 5_666 ?
O7 U2 U1 28.4(6) . . ?
O7 U2 U1 28.4(6) . 5_666 ?
O7 U2 O18 69.2(7) . . ?
O7 U2 O11 142.7(9) . . ?
O7 U2 O8 69.4(8) . . ?
O7 U2 O5 144.2(8) . . ?
O6 U2 U1 91.4(5) . 5_666 ?
O6 U2 U1 91.0(5) . . ?
O6 U2 U1 91.0(5) 6_565 . ?
O6 U2 U1 91.4(5) 6_565 5_666 ?
O6 U2 O7 91.4(5) 6_565 . ?
O6 U2 O7 91.4(5) . . ?
O6 U2 O6 177.1(10) . 6_565 ?
O6 U2 O18 90.9(6) . . ?
O6 U2 O18 90.9(6) 6_565 . ?
O6 U2 O11 89.2(5) 6_565 . ?
O6 U2 O11 89.2(5) . . ?
O6 U2 O8 90.1(6) . . ?
O6 U2 O8 90.1(6) 6_565 . ?
O6 U2 O5 88.6(6) . . ?
O6 U2 O5 88.6(6) 6_565 . ?
O18 U2 U1 40.8(5) . 5_666 ?
O18 U2 U1 97.6(5) . . ?
O18 U2 O5 146.6(8) . . ?
O11 U2 U1 114.3(7) . 5_666 ?
O11 U2 U1 171.1(7) . . ?
O11 U2 O18 73.5(9) . . ?
O11 U2 O8 147.9(9) . . ?
O11 U2 O5 73.1(9) . . ?
O8 U2 U1 40.9(5) . . ?
O8 U2 U1 97.8(5) . 5_666 ?
O8 U2 O18 138.6(7) . . ?
O8 U2 O5 74.8(8) . . ?
O5 U2 U1 115.7(6) . . ?
O5 U2 U1 172.6(6) . 5_666 ?
U1 O9 Na20 173.8(9) . 5_656 ?
U1 O7 U1 111.1(8) . 5_666 ?
U2 O7 U1 124.4(10) . . ?
U2 O7 U1 124.5(10) . 5_666 ?
U2 O18 U1 101.7(8) . 5_666 ?
C15 O18 U1 98.8(19) . 5_666 ?
C15 O18 U2 159(2) . . ?
O11 Re4 O12 103.5(16) . . ?
O11 Re4 O12 103.5(16) . 6_565 ?
O13 Re4 O11 107(2) . . ?
O13 Re4 O12 107.8(17) . 6_565 ?
O13 Re4 O12 107.8(17) . . ?
O12 Re4 O12 126(3) . 6_565 ?
Re3 Re4 O11 86.1(7) 6_565 . ?
Re3 Re4 O11 86.1(7) . . ?
Re3 Re4 O13 82.5(7) . . ?
Re3 Re4 O13 82.5(7) 6_565 . ?
Re3 Re4 O12 36.8(17) . . ?
Re3 Re4 O12 162.7(18) . 6_565 ?
Re3 Re4 O12 162.7(18) 6_565 . ?
Re3 Re4 O12 36.8(17) 6_565 6_565 ?
Re3 Re4 Re3 160.4(12) 6_565 . ?
Re3 Re4 O1 52(2) 6_565 6_565 ?
Re3 Re4 O1 146(2) . 6_565 ?
Re3 Re4 O1 146(2) 6_565 . ?
Re3 Re4 O1 52(2) . . ?
O1 Re4 O11 117.1(19) 6_565 . ?
O1 Re4 O11 117.1(19) . . ?
O1 Re4 O13 111(2) . . ?
O1 Re4 O13 111(2) 6_565 . ?
O1 Re4 O12 17(2) 6_565 6_565 ?
O1 Re4 O12 110(3) . 6_565 ?
O1 Re4 O12 110(3) 6_565 . ?
O1 Re4 O12 17(2) . . ?
O1 Re4 O1 94(4) . 6_565 ?
Re4 O11 U2 161.2(16) . . ?
Re4 O11 Re3 18.4(3) . 6_565 ?
Re4 O11 Re3 18.4(3) . . ?
Re3 O11 U2 151.9(12) 6_565 . ?
Re3 O11 U2 151.9(12) . . ?
Re3 O11 Re3 36.3(6) 6_565 . ?
Re4 O13 Re3 19.1(6) . 6_565 ?
Re4 O13 Re3 19.1(6) . . ?
Re3 O13 Re3 37.9(12) 6_565 . ?
U2 O8 U1 102.4(8) . . ?
C14 O8 U1 91.2(17) . . ?
C14 O8 U2 166(2) . . ?
C14 O10 U1 98.5(19) . . ?
C14 O10 Na20 150(2) . 3 ?
Na20 O10 U1 111.3(8) 3 . ?
C15 O19 U1 100.3(17) . 5_666 ?
C15 O19 Na20 147.4(19) . 7_556 ?
Na20 O19 U1 112.3(8) 7_556 5_666 ?
O18 C15 O19 112(3) . . ?
O18 C15 C16 123(4) . . ?
O19 C15 C16 125(4) . . ?
O8 C14 U1 63.0(15) . . ?
O8 C14 C17 117(3) . . ?
O10 C14 U1 58.5(16) . . ?
O10 C14 O8 121(3) . . ?
O10 C14 C17 121(3) . . ?
C17 C14 U1 180(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Re4 O12 Re3 3.9(4) . 6_565 ?
Re3 O12 Re4 13.1(7) . . ?
Re3 O12 Re3 17.0(10) . 6_565 ?
O1 O12 Re4 51(7) . . ?
O1 O12 Re3 63(8) . . ?
O1 O12 Re3 48(7) . 6_565 ?
Na20 O21 Na20 91.3(9) . 5_656 ?
Re4 Re3 O11 75.5(7) . . ?
Re4 Re3 O13 78.4(9) . . ?
Re4 Re3 O12 13.4(14) . 6_565 ?
Re4 Re3 O12 130(2) . . ?
Re4 Re3 Re3 9.8(6) . 6_565 ?
Re4 Re3 O1 108(2) . . ?
Re4 Re3 O1 25.1(16) . 6_565 ?
O11 Re3 O12 83.3(13) . 6_565 ?
O11 Re3 O1 93.9(15) . 6_565 ?
O13 Re3 O11 103.8(18) . . ?
O13 Re3 O12 86.7(14) . 6_565 ?
O13 Re3 O1 90.0(17) . 6_565 ?
O12 Re3 O11 121(2) . . ?
O12 Re3 O13 130(2) . . ?
O12 Re3 O12 117(3) . 6_565 ?
O12 Re3 O1 106(3) . 6_565 ?
Re3 Re3 O11 71.8(3) 6_565 . ?
Re3 Re3 O13 71.0(6) 6_565 . ?
Re3 Re3 O12 140(2) 6_565 . ?
Re3 Re3 O12 23.1(13) 6_565 6_565 ?
Re3 Re3 O1 118(2) 6_565 . ?
Re3 Re3 O1 34.3(15) 6_565 6_565 ?
O1 Re3 O11 131(2) . . ?
O1 Re3 O13 125(3) . . ?
O1 Re3 O12 12.2(19) 6_565 6_565 ?
O1 Re3 O12 95(3) . 6_565 ?
O1 Re3 O12 24(3) . . ?
O1 Re3 O1 83(4) . 6_565 ?
U1 Na20 U1 87.89(14) 3_445 5_666 ?
U1 Na20 U1 87.89(14) 3_445 5_656 ?
U1 Na20 U1 175.7(3) 5_666 5_656 ?
O9 Na20 U1 2.7(4) 2_656 5_666 ?
O9 Na20 U1 173.1(5) 2_656 5_656 ?
O9 Na20 U1 173.1(5) 5_656 5_666 ?
O9 Na20 U1 85.2(4) 5_656 3_445 ?
O9 Na20 U1 85.2(4) 2_656 3_445 ?
O9 Na20 U1 2.7(4) 5_656 5_656 ?
O9 Na20 O9 170.4(9) 5_656 2_656 ?
O9 Na20 O10 86.2(4) 2_656 3_445 ?
O9 Na20 O10 86.2(4) 5_656 3_445 ?
O9 Na20 O19 86.0(5) 2_656 7_556 ?
O9 Na20 O19 86.0(5) 5_656 7_556 ?
O9 Na20 O21 93.6(5) 5_656 5_656 ?
O9 Na20 O21 93.2(5) 2_656 . ?
O9 Na20 O21 93.2(5) 5_656 . ?
O9 Na20 O21 93.6(5) 2_656 5_656 ?
O9 Na20 Na20 94.8(4) 5_656 5_656 ?
O9 Na20 Na20 94.8(4) 2_656 5_656 ?
O10 Na20 U1 35.8(5) 3_445 3_445 ?
O10 Na20 U1 88.47(14) 3_445 5_656 ?
O10 Na20 U1 88.47(14) 3_445 5_666 ?
O10 Na20 O21 100.5(9) 3_445 5_656 ?
O10 Na20 O21 170.7(9) 3_445 . ?
O10 Na20 Na20 144.8(8) 3_445 5_656 ?
O19 Na20 U1 88.10(15) 7_556 5_666 ?
O19 Na20 U1 35.7(5) 7_556 3_445 ?
O19 Na20 U1 88.10(15) 7_556 5_656 ?
O19 Na20 O10 71.5(7) 7_556 3_445 ?
O19 Na20 O21 172.1(9) 7_556 5_656 ?
O19 Na20 O21 99.2(8) 7_556 . ?
O19 Na20 Na20 143.7(7) 7_556 5_656 ?
O21 Na20 U1 91.75(15) 5_656 5_666 ?
O21 Na20 U1 91.27(14) . 5_656 ?
O21 Na20 U1 91.27(14) . 5_666 ?
O21 Na20 U1 135.0(7) . 3_445 ?
O21 Na20 U1 91.75(15) 5_656 5_656 ?
O21 Na20 U1 136.3(7) 5_656 3_445 ?
O21 Na20 O21 88.7(9) . 5_656 ?
O21 Na20 Na20 44.5(6) . 5_656 ?
O21 Na20 Na20 44.2(6) 5_656 5_656 ?
Na20 Na20 U1 92.11(14) 5_656 5_656 ?
Na20 Na20 U1 179.4(5) 5_656 3_445 ?
Na20 Na20 U1 92.11(14) 5_656 5_666 ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Re4 O1 Re3 8.6(6) . 6_565 ?
O12 O1 Re4 112(9) . . ?
O12 O1 Re3 93(9) . . ?
O12 O1 Re3 120(9) . 6_565 ?
Re3 O1 Re4 19.6(8) . . ?
Re3 O1 Re3 28.2(12) . 6_565 ?

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
U1 O18 C15 O19 0.000(4) 5_666 . . . ?
U1 O18 C15 C16 180.000(6) 5_666 . . . ?
U1 O8 C14 O10 0.000(4) . . . . ?
U1 O8 C14 C17 180.000(5) . . . . ?
U1 O10 C14 O8 0.000(5) . . . . ?
U1 O10 C14 C17 180.000(6) . . . . ?
U1 O19 C15 O18 0.000(4) 5_666 . . . ?
U1 O19 C15 C16 180.000(6) 5_666 . . . ?
U2 O18 C15 O19 180.000(12) . . . . ?
U2 O18 C15 C16 0.000(17) . . . . ?
U2 O11 Re3 Re4 -137(2) . . . . ?
U2 O11 Re3 O13 -64(2) . . . . ?
U2 O11 Re3 O12 94(4) . . . . ?
U2 O11 Re3 O12 -149(3) . . . 6_565 ?
U2 O11 Re3 Re3 -128(2) . . . 6_565 ?
U2 O11 Re3 O1 -155(3) . . . 6_565 ?
U2 O11 Re3 O1 121(4) . . . . ?
U2 O8 C14 U1 180.00(2) . . . . ?
U2 O8 C14 O10 180.000(19) . . . . ?
U2 O8 C14 C17 0.000(15) . . . . ?
Re4 O11 Re3 O13 73.9(12) . . . . ?
Re4 O11 Re3 O12 -11.1(14) . . . 6_565 ?
Re4 O11 Re3 O12 -128(3) . . . . ?
Re4 O11 Re3 Re3 9.5(6) . . . 6_565 ?
Re4 O11 Re3 O1 -17.1(16) . . . 6_565 ?
Re4 O11 Re3 O1 -102(3) . . . . ?
Re4 O13 Re3 O11 -71.7(10) . . . . ?
Re4 O13 Re3 O12 10.5(14) . . . 6_565 ?
Re4 O13 Re3 O12 133(3) . . . . ?
Re4 O13 Re3 Re3 -6.8(7) . . . 6_565 ?
Re4 O13 Re3 O1 104(3) . . . . ?
Re4 O13 Re3 O1 22.3(16) . . . 6_565 ?
Re4 O12 Re3 O11 97(3) . . . . ?
Re4 O12 Re3 O13 -112(4) . . . . ?
Re4 O12 Re3 O12 -1.5(11) . . . 6_565 ?
Re4 O12 Re3 Re3 -1.5(11) . . . 6_565 ?
Re4 O12 Re3 O1 -25(9) . . . . ?
Re4 O12 Re3 O1 -8(2) . . . 6_565 ?
Re4 O12 O1 Re3 7(3) . . . . ?
Re4 O12 O1 Re3 -2.0(13) . . . 6_565 ?
Re4 Re3 O1 O12 -160(8) . . . . ?
Re4 Re3 O1 Re3 3.0(8) . . . 6_565 ?
O11 Re4 O13 Re3 83.6(7) . . . . ?
O11 Re4 O13 Re3 -83.6(7) . . . 6_565 ?
O11 Re4 Re3 O13 -108(2) . . . . ?
O11 Re4 Re3 O12 119(3) . . . . ?
O11 Re4 Re3 O12 124(6) . . . 6_565 ?
O11 Re4 Re3 Re3 -67(4) . . . 6_565 ?
O11 Re4 Re3 O1 129(2) . . . . ?
O11 Re4 Re3 O1 136(4) . . . 6_565 ?
O11 Re4 O1 O12 -39(10) . . . . ?
O11 Re4 O1 Re3 -61(2) . . . . ?
O11 Re4 O1 Re3 129(4) . . . 6_565 ?
O11 Re3 O1 Re4 86(2) . . . . ?
O11 Re3 O1 O12 -74(9) . . . . ?
O11 Re3 O1 Re3 89(2) . . . 6_565 ?
O13 Re4 O11 U2 0.000(1) . . . . ?
O13 Re4 O11 Re3 -81.0(6) . . . . ?
O13 Re4 O11 Re3 81.0(6) . . . 6_565 ?
O13 Re4 Re3 O11 108(2) . . . . ?
O13 Re4 Re3 O12 -128(6) . . . 6_565 ?
O13 Re4 Re3 O12 -134(3) . . . . ?
O13 Re4 Re3 Re3 41(4) . . . 6_565 ?
O13 Re4 Re3 O1 -123(3) . . . . ?
O13 Re4 Re3 O1 -116(4) . . . 6_565 ?
O13 Re4 O1 O12 84(10) . . . . ?
O13 Re4 O1 Re3 -108(4) . . . 6_565 ?
O13 Re4 O1 Re3 62(2) . . . . ?
O13 Re3 O1 Re4 -88(2) . . . . ?
O13 Re3 O1 O12 112(8) . . . . ?
O13 Re3 O1 Re3 -85(2) . . . 6_565 ?
O12 Re4 O11 U2 113.6(17) . . . . ?
O12 Re4 O11 U2 -113.6(17) 6_565 . . . ?
O12 Re4 O11 Re3 -32.7(17) 6_565 . . 6_565 ?
O12 Re4 O11 Re3 -165.4(18) . . . 6_565 ?
O12 Re4 O11 Re3 165.4(18) 6_565 . . . ?
O12 Re4 O11 Re3 32.7(17) . . . . ?
O12 Re4 O13 Re3 -165.7(19) 6_565 . . . ?
O12 Re4 O13 Re3 -27.1(19) . . . . ?
O12 Re4 O13 Re3 165.7(19) . . . 6_565 ?
O12 Re4 O13 Re3 27.1(19) 6_565 . . 6_565 ?
O12 Re4 Re3 O11 -124(6) 6_565 . . . ?
O12 Re4 Re3 O11 -119(3) . . . . ?
O12 Re4 Re3 O13 128(6) 6_565 . . . ?
O12 Re4 Re3 O13 134(3) . . . . ?
O12 Re4 Re3 O12 -6(4) 6_565 . . . ?
O12 Re4 Re3 O12 6(4) . . . 6_565 ?
O12 Re4 Re3 Re3 174(4) . . . 6_565 ?
O12 Re4 Re3 Re3 169(8) 6_565 . . 6_565 ?
O12 Re4 Re3 O1 17(5) . . . 6_565 ?
O12 Re4 Re3 O1 5(7) 6_565 . . . ?
O12 Re4 Re3 O1 10(4) . . . . ?
O12 Re4 Re3 O1 12(7) 6_565 . . 6_565 ?
O12 Re4 O1 O12 -157(10) 6_565 . . . ?
O12 Re4 O1 Re3 -21(8) . . . . ?
O12 Re4 O1 Re3 168(7) . . . 6_565 ?
O12 Re4 O1 Re3 -179(2) 6_565 . . . ?
O12 Re4 O1 Re3 11(3) 6_565 . . 6_565 ?
O12 Re3 O1 Re4 160(8) . . . . ?
O12 Re3 O1 Re4 1.1(16) 6_565 . . . ?
O12 Re3 O1 O12 -159(9) 6_565 . . . ?
O12 Re3 O1 Re3 4.1(17) 6_565 . . 6_565 ?
O12 Re3 O1 Re3 163(7) . . . 6_565 ?
Re3 Re4 O11 U2 81.0(6) . . . . ?
Re3 Re4 O11 U2 -81.0(6) 6_565 . . . ?
Re3 Re4 O11 Re3 -162.0(12) 6_565 . . . ?
Re3 Re4 O11 Re3 162.0(12) . . . 6_565 ?
Re3 Re4 O13 Re3 167.2(14) 6_565 . . . ?
Re3 Re4 O13 Re3 -167.2(14) . . . 6_565 ?
Re3 Re4 Re3 O11 67(4) 6_565 . . . ?
Re3 Re4 Re3 O13 -41(4) 6_565 . . . ?
Re3 Re4 Re3 O12 -169(8) 6_565 . . 6_565 ?
Re3 Re4 Re3 O12 -174(4) 6_565 . . . ?
Re3 Re4 Re3 O1 -157(6) 6_565 . . 6_565 ?
Re3 Re4 Re3 O1 -164(4) 6_565 . . . ?
Re3 Re4 O1 O12 21(8) . . . . ?
Re3 Re4 O1 O12 -168(7) 6_565 . . . ?
Re3 Re4 O1 Re3 -170(3) . . . 6_565 ?
Re3 Re4 O1 Re3 170(3) 6_565 . . . ?
Re3 O11 Re3 Re4 -9.5(6) 6_565 . . . ?
Re3 O11 Re3 O13 64.4(10) 6_565 . . . ?
Re3 O11 Re3 O12 -138(3) 6_565 . . . ?
Re3 O11 Re3 O12 -20.6(13) 6_565 . . 6_565 ?
Re3 O11 Re3 O1 -26.6(15) 6_565 . . 6_565 ?
Re3 O11 Re3 O1 -111(3) 6_565 . . . ?
Re3 O13 Re3 Re4 6.8(7) 6_565 . . . ?
Re3 O13 Re3 O11 -65.0(10) 6_565 . . . ?
Re3 O13 Re3 O12 17.3(13) 6_565 . . 6_565 ?
Re3 O13 Re3 O12 140(3) 6_565 . . . ?
Re3 O13 Re3 O1 29.1(16) 6_565 . . 6_565 ?
Re3 O13 Re3 O1 111(3) 6_565 . . . ?
Re3 O12 Re3 Re4 1.5(10) 6_565 . . . ?
Re3 O12 Re3 O11 99(3) 6_565 . . . ?
Re3 O12 Re3 O13 -110(4) 6_565 . . . ?
Re3 O12 Re3 O12 0.003(1) 6_565 . . 6_565 ?
Re3 O12 Re3 O1 -6(3) 6_565 . . 6_565 ?
Re3 O12 Re3 O1 -24(10) 6_565 . . . ?
Re3 O12 O1 Re4 -7(3) . . . . ?
Re3 O12 O1 Re4 2.0(13) 6_565 . . . ?
Re3 O12 O1 Re3 -9(4) . . . 6_565 ?
Re3 O12 O1 Re3 9(4) 6_565 . . . ?
Re3 Re3 O1 Re4 -3.0(8) 6_565 . . . ?
Re3 Re3 O1 O12 -163(7) 6_565 . . . ?
Na20 O10 C14 U1 180.000(12) 3 . . . ?
Na20 O10 C14 O8 180.000(7) 3 . . . ?
Na20 O10 C14 C17 0.000(13) 3 . . . ?
Na20 O19 C15 O18 180.000(6) 7_556 . . . ?
Na20 O19 C15 C16 0.000(12) 7_556 . . . ?
O1 Re4 O11 U2 125(2) . . . . ?
O1 Re4 O11 U2 -125(2) 6_565 . . . ?
O1 Re4 O11 Re3 -44(2) 6_565 . . 6_565 ?
O1 Re4 O11 Re3 44(2) . . . . ?
O1 Re4 O11 Re3 -154(2) . . . 6_565 ?
O1 Re4 O11 Re3 154(2) 6_565 . . . ?
O1 Re4 O13 Re3 148(2) . . . 6_565 ?
O1 Re4 O13 Re3 45(2) 6_565 . . 6_565 ?
O1 Re4 O13 Re3 -148(2) 6_565 . . . ?
O1 Re4 O13 Re3 -45(2) . . . . ?
O1 Re4 Re3 O11 -129(2) . . . . ?
O1 Re4 Re3 O11 -136(4) 6_565 . . . ?
O1 Re4 Re3 O13 123(3) . . . . ?
O1 Re4 Re3 O13 116(4) 6_565 . . . ?
O1 Re4 Re3 O12 -10(4) . . . . ?
O1 Re4 Re3 O12 -12(7) 6_565 . . 6_565 ?
O1 Re4 Re3 O12 -17(5) 6_565 . . . ?
O1 Re4 Re3 O12 -5(7) . . . 6_565 ?
O1 Re4 Re3 Re3 164(4) . . . 6_565 ?
O1 Re4 Re3 Re3 157(6) 6_565 . . 6_565 ?
O1 Re4 Re3 O1 -7.1(19) 6_565 . . . ?
O1 Re4 Re3 O1 7.1(19) . . . 6_565 ?
O1 Re4 O1 O12 -162(8) 6_565 . . . ?
O1 Re4 O1 Re3 176.1(10) 6_565 . . . ?
O1 Re4 O1 Re3 5.6(15) 6_565 . . 6_565 ?
O1 O12 Re3 Re4 25(9) . . . . ?
O1 O12 Re3 O11 122(8) . . . . ?
O1 O12 Re3 O13 -87(9) . . . . ?
O1 O12 Re3 O12 24(10) . . . 6_565 ?
O1 O12 Re3 Re3 24(10) . . . 6_565 ?
O1 O12 Re3 O1 17(8) . . . 6_565 ?
O1 Re3 O1 Re4 -3.0(8) 6_565 . . . ?
O1 Re3 O1 O12 -163(7) 6_565 . . . ?
O1 Re3 O1 Re3 0.002(4) 6_565 . . 6_565 ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 3.008
_oxdiff_exptl_absorpt_empirical_full_min 0.507
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.514(6)
2 0.486(6)

# start Validation Reply Form
_vrf_PLAT201_ui_36_thinplate150816_auto 
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          7 Report
RESPONSE: Those sites are disordered and aniosotropic refinement could not be done with good refinement parameters. 
;
_vrf_PLAT342_ui_36_thinplate150816_auto 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.06 Ang.  
RESPONSE: This is due to the fact that those sites are disordered which resulted low bond precision.  
;
_vrf_PLAT430_ui_36_thinplate150816_auto 
;
PROBLEM: Short Inter D...A Contact  O5       ..O12      .       2.63 Ang.  
RESPONSE: This is due to the presence of hydrogen bonding.  
;
# end Validation Reply Form

####################################################################### 
# 
# 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_utc_3_thinplate_150815_auto
_database_code_depnum_ccdc_archive 'CCDC 2332265'
loop_
_audit_author_name
_audit_author_address
'Mohammad Shohel'
;Oregon State University
United States of America
;
_audit_update_record             
;
2024-02-11 deposited with the CCDC.	2024-05-06 downloaded from the CCDC.
;
_audit_creation_date             2023-07-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H12 Na2 O30 Tc2 U4'
_chemical_formula_sum            'C8 H12 Na2 O30 Tc2 U4'
_chemical_formula_weight         1782.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         'U2 Tc O15 C4 Na H6'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc 0.0057 3.0049 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   15.2356(8)
_cell_length_b                   8.1216(3)
_cell_length_c                   15.0053(7)
_cell_angle_alpha                90
_cell_angle_beta                 114.061(6)
_cell_angle_gamma                90
_cell_volume                     1695.39(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5109
_cell_measurement_temperature    223.00(10)
_cell_measurement_theta_max      76.8850
_cell_measurement_theta_min      3.2210
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    60.650
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.491
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1678
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         3.225
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      223.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -23.00  28.00   0.50    8.00    --  -47.14  19.00-180.00  102
  2  ω   -120.00 -52.00   0.50    8.00    --  -47.14 -19.00   0.00  136
  3  ω   -119.00 -85.00   0.50    8.00    --  -47.14 -77.00  90.00   68
  4  ω    -70.00  25.00   0.50    8.00    --  -47.14  77.00 120.00  190
  5  ω    -10.00  24.00   0.50    8.00    --  -47.14  19.00  30.00   68
  6  ω   -119.00 -93.00   0.50    8.00    --  -47.14 -77.00  60.00   52
  7  ω    -27.00  -2.00   0.50    8.00    --   47.14 -19.00 -90.00   50
  8  ω     55.00  94.00   0.50    8.00    --   47.14-125.00-150.00   78
  9  ω   -157.00-116.00   0.50   10.50    --  -86.25-125.00-120.00   82
 10  ω   -157.00-102.00   0.50   10.50    --  -86.25 -45.00 120.00  110
 11  ω     35.00 105.00   0.50   10.50    --  107.75 -77.00 150.00  140
 12  ω     98.00 177.00   0.50   10.50    --  107.75  15.00  30.00  158
 13  ω    100.00 178.00   0.50   10.50    --  107.75  30.00-150.00  156
 14  ω     80.00 105.00   0.50   10.50    --  107.75 -77.00 -90.00   50
 15  ω     40.00  67.00   0.50   10.50    --  107.75 -61.00-120.00   54
 16  ω     73.00 105.00   0.50   10.50    --  107.75 -77.00  30.00   64
 17  ω    135.00 178.00   0.50   10.50    --  107.75  30.00  60.00   86
 18  ω     38.00  66.00   0.50   10.50    --  107.75 -61.00  60.00   56
 19  ω     36.00  70.00   0.50   10.50    --  107.75 -61.00-150.00   68
 20  ω     36.00  77.00   0.50   10.50    --  107.75 -77.00 -30.00   82
 21  ω     77.00 105.00   0.50   10.50    --  107.75 -94.00-120.00   56
 22  ω     36.00  66.00   0.50   10.50    --  107.75 -77.00  30.00   60
 23  ω     79.00 106.00   0.50   10.50    --  107.75 -94.00 -30.00   54
 24  ω     35.00  66.00   0.50   10.50    --  107.75 -61.00 -90.00   62
 25  ω     42.00  75.00   0.50   10.50    --  107.75 -94.00 -30.00   66
 26  ω    111.00 175.00   0.50   10.50    --  107.75  15.00 -30.00  128
 27  ω     43.00  70.00   0.50   10.50    --  107.75 -61.00-180.00   54
 28  ω     46.00  76.00   0.50   10.50    --  107.75 -77.00 -90.00   60
 29  ω     45.00  72.00   0.50   10.50    --  107.75 -77.00-120.00   54
 30  ω    116.00 176.00   0.50   10.50    --  107.75  15.00 -90.00  120
 31  ω     60.00  86.00   0.50   10.50    --  107.75 -77.00-180.00   52
 32  ω     84.00 131.00   0.50   10.50    --  107.75 -88.00 139.01   94
 33  ω     37.00  99.00   0.50   10.50    --  107.75 -77.00  90.00  124
 34  ω     38.00  71.00   0.50   10.50    --  107.75 -61.00 150.00   66
 35  ω     74.00 105.00   0.50   10.50    --  107.75 -94.00 -90.00   62
 36  ω     41.00  78.00   0.50   10.50    --  107.75 -87.00  21.89   74
 37  ω     86.00 122.00   0.50   10.50    --  107.75 -87.00  21.89   72
 38  ω     37.00  64.00   0.50   10.50    --  107.75 -61.00 120.00   54
 39  ω     35.00  69.00   0.50   10.50    --  107.75 -61.00  30.00   68
 40  ω     67.00 105.00   0.50   10.50    --  107.75 -94.00 120.00   76
 41  ω    110.00 161.00   0.50   10.50    --  107.75  45.00 120.00  102
 42  ω    127.00 167.00   0.50   10.50    --  107.75  45.00-180.00   80
 43  ω     85.00 112.00   0.50   10.50    --  107.75 -88.00   4.91   54
 44  ω     76.00 106.00   0.50   10.50    --  107.75 -94.00   0.00   60
 45  ω     39.00  64.00   0.50   10.50    --  107.75 -88.00   4.91   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0935481000
_diffrn_orient_matrix_UB_12      0.0445351000
_diffrn_orient_matrix_UB_13      0.0105937000
_diffrn_orient_matrix_UB_21      -0.0122421000
_diffrn_orient_matrix_UB_22      0.1523208000
_diffrn_orient_matrix_UB_23      -0.0652621000
_diffrn_orient_matrix_UB_31      -0.0579356000
_diffrn_orient_matrix_UB_32      -0.1040059000
_diffrn_orient_matrix_UB_33      -0.0909437000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1538
_reflns_number_total             1678
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         9.150
_refine_diff_density_min         -5.439
_refine_diff_density_rms         0.667
_refine_ls_extinction_coef       0.00016(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1678
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0678
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1341P)²+30.9071P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1884
_refine_ls_wR_factor_ref         0.1926
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.485(6)
 0.515(6)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H5C(0.5) O00G(0.375) H1A(0.5) H1B(0.5) H1C(0.5)
 O2(0.125)
4.a Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_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
U001 U -0.12190(5) 0.500000 0.50063(6) 0.0208(4) Uani 1 2 d S T P . .
U002 U 0.10166(6) 0.500000 0.75127(5) 0.0297(4) Uani 1 2 d S T P . .
Tc03 Tc 0.3339(2) 0.500000 1.0078(2) 0.0857(14) Uani 1 2 d S T P . .
C5 C 0.612(4) 0.500000 0.234(4) 0.090(16) Uiso 1 2 d S . P . .
H5A H 0.569295 0.582959 0.240464 0.135 Uiso 0.5 1 calc R U P A -1
H5B H 0.582042 0.392580 0.226090 0.135 Uiso 0.5 1 calc R U P A -1
H5C H 0.625275 0.524461 0.177340 0.135 Uiso 0.5 1 calc R U P A -1
O00B O 0.0370(13) 0.500000 0.5927(14) 0.038(4) Uani 1 2 d S T P . .
O00C O 0.2205(15) 0.500000 0.3983(14) 0.040(5) Uani 1 2 d S T P . .
O00D O 0.3039(14) 0.500000 0.5979(14) 0.034(4) Uani 1 2 d S T P . .
O00E O -0.1269(9) 0.281(2) 0.4986(11) 0.042(4) Uani 1 1 d . . . . .
O00F O 0.2201(12) 0.500000 0.6883(12) 0.043(6) Uani 1 2 d S T P . .
O00G O 0.070(3) 0.500000 0.312(3) 0.041(9) Uiso 0.75 2 d S . P . .
O00H O 0.1038(12) 0.719(3) 0.7558(10) 0.057(5) Uani 1 1 d . . . . .
O00I O -0.5473(13) 0.500000 0.3779(13) 0.034(4) Uani 1 2 d S T P . .
O00J O 0.2524(15) 0.500000 0.8872(15) 0.056(6) Uani 1 2 d S T P . .
O00K O 0.0639(18) 0.500000 0.8950(16) 0.060(6) Uani 1 2 d S T P . .
C00M C 0.158(2) 0.500000 0.322(2) 0.042(7) Uiso 1 2 d S . P . .
O1 O 0.406(2) 0.317(4) 1.027(2) 0.132(10) Uiso 1 1 d . . . . .
O13 O 0.272(4) 0.500000 1.079(4) 0.143(17) Uiso 1 2 d S . P . .
C3 C 0.304(2) 0.500000 0.684(2) 0.034(6) Uiso 1 2 d S . P . .
C1 C 0.179(3) 0.500000 0.228(3) 0.067(11) Uiso 1 2 d S . P . .
H1A H 0.135940 0.422806 0.181040 0.101 Uiso 0.5 1 calc R U P B -1
H1B H 0.244801 0.467600 0.245325 0.101 Uiso 0.5 1 calc R U P B -1
H1C H 0.168123 0.609594 0.200045 0.101 Uiso 0.5 1 calc R U P B -1
Na4 Na 0.3853(7) 0.500000 0.4989(7) 0.029(2) Uiso 1 2 d S . P . .
O2 O 0.068(7) 0.500000 0.282(8) 0.04(2) Uiso 0.25 2 d S . P . .


_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
U001 U001 3.7223(13) 5_566 ?
U001 U002 3.9116(11) . ?
U001 O00B 2.245(18) . ?
U001 O00B 2.26(2) 5_566 ?
U001 O00C 2.53(2) 5_566 ?
U001 O00D 2.56(2) 5_566 ?
U001 O00E 1.781(18) 6_565 ?
U001 O00E 1.781(18) . ?
U001 O00F 2.611(16) 5_566 ?
U001 O00G 2.59(4) 5_566 ?
U001 C00M 2.93(3) 5_566 ?
U001 C3 3.02(3) 5_566 ?
U002 O00B 2.17(2) . ?
U002 O00F 2.354(18) . ?
U002 O00G 2.39(4) 5_566 ?
U002 O00H 1.78(2) 6_565 ?
U002 O00H 1.78(2) . ?
U002 O00J 2.369(19) . ?
U002 O00K 2.45(2) . ?
U002 O2 2.42(10) 5_566 ?
Tc03 O00J 1.73(2) . ?
Tc03 O1 1.80(3) . ?
Tc03 O1 1.80(3) 6_565 ?
Tc03 O13 1.68(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C5 C3 1.36(6) 5_666 ?
O00C C00M 1.16(4) . ?
O00C Na4 2.34(2) . ?
O00D C3 1.30(3) . ?
O00D Na4 2.29(2) . ?
O00E Na4 2.288(18) 3_445 ?
O00F C3 1.30(3) . ?
O00G C00M 1.29(5) . ?
O00I Na4 2.41(2) 5_566 ?
O00I Na4 2.42(2) 1_455 ?
C00M C1 1.56(5) . ?
C00M O2 1.25(10) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 H1C 0.9700 . ?
Na4 Na4 3.483(19) 5_666 ?

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
U001 U001 U002 61.66(3) 5_566 . ?
O00B U001 U001 34.2(5) 5_566 5_566 ?
O00B U001 U001 34.5(5) . 5_566 ?
O00B U001 U002 27.2(5) . . ?
O00B U001 U002 95.8(5) 5_566 . ?
O00B U001 O00B 68.6(8) . 5_566 ?
O00B U001 O00C 178.7(6) 5_566 5_566 ?
O00B U001 O00C 112.7(7) . 5_566 ?
O00B U001 O00D 113.7(6) 5_566 5_566 ?
O00B U001 O00D 177.7(7) . 5_566 ?
O00B U001 O00F 63.1(6) 5_566 5_566 ?
O00B U001 O00F 131.7(7) . 5_566 ?
O00B U001 O00G 63.6(10) . 5_566 ?
O00B U001 O00G 132.2(10) 5_566 5_566 ?
O00B U001 C00M 158.3(8) 5_566 5_566 ?
O00B U001 C00M 89.6(8) . 5_566 ?
O00B U001 C3 157.1(8) . 5_566 ?
O00B U001 C3 88.5(7) 5_566 5_566 ?
O00C U001 U001 147.1(5) 5_566 5_566 ?
O00C U001 U002 85.5(5) 5_566 . ?
O00C U001 O00D 65.0(6) 5_566 5_566 ?
O00C U001 O00F 115.6(6) 5_566 5_566 ?
O00C U001 O00G 49.1(9) 5_566 5_566 ?
O00C U001 C00M 23.0(8) 5_566 5_566 ?
O00C U001 C3 90.2(7) 5_566 5_566 ?
O00D U001 U001 147.8(4) 5_566 5_566 ?
O00D U001 U002 150.5(4) 5_566 . ?
O00D U001 O00F 50.6(6) 5_566 5_566 ?
O00D U001 O00G 114.1(9) 5_566 5_566 ?
O00D U001 C00M 88.1(7) 5_566 5_566 ?
O00D U001 C3 25.2(7) 5_566 5_566 ?
O00E U001 U001 92.1(4) 6_565 5_566 ?
O00E U001 U001 92.1(4) . 5_566 ?
O00E U001 U002 91.8(4) . . ?
O00E U001 U002 91.8(4) 6_565 . ?
O00E U001 O00B 92.2(4) 6_565 . ?
O00E U001 O00B 91.2(4) . 5_566 ?
O00E U001 O00B 91.2(4) 6_565 5_566 ?
O00E U001 O00B 92.2(4) . . ?
O00E U001 O00C 88.8(4) 6_565 5_566 ?
O00E U001 O00C 88.8(4) . 5_566 ?
O00E U001 O00D 87.8(4) . 5_566 ?
O00E U001 O00D 87.8(4) 6_565 5_566 ?
O00E U001 O00E 175.5(8) 6_565 . ?
O00E U001 O00F 88.8(5) . 5_566 ?
O00E U001 O00F 88.8(5) 6_565 5_566 ?
O00E U001 O00G 90.6(5) . 5_566 ?
O00E U001 O00G 90.6(5) 6_565 5_566 ?
O00E U001 C00M 89.6(5) 6_565 5_566 ?
O00E U001 C00M 89.6(5) . 5_566 ?
O00E U001 C3 88.1(4) 6_565 5_566 ?
O00E U001 C3 88.1(4) . 5_566 ?
O00F U001 U001 97.2(4) 5_566 5_566 ?
O00F U001 U002 158.9(4) 5_566 . ?
O00F U001 C00M 138.7(7) 5_566 5_566 ?
O00F U001 C3 25.4(7) 5_566 5_566 ?
O00G U001 U001 98.0(8) 5_566 5_566 ?
O00G U001 U002 36.3(8) 5_566 . ?
O00G U001 O00F 164.8(9) 5_566 5_566 ?
O00G U001 C00M 26.1(10) 5_566 5_566 ?
O00G U001 C3 139.4(10) 5_566 5_566 ?
C00M U001 U001 124.1(6) 5_566 5_566 ?
C00M U001 U002 62.4(6) 5_566 . ?
C00M U001 C3 113.3(7) 5_566 5_566 ?
C3 U001 U001 122.6(5) 5_566 5_566 ?
C3 U001 U002 175.7(5) 5_566 . ?
U001 U002 U001 56.79(2) . 5_566 ?
O00B U002 U001 28.2(5) . . ?
O00B U002 U001 28.6(5) . 5_566 ?
O00B U002 O00F 68.9(6) . . ?
O00B U002 O00G 68.3(10) . 5_566 ?
O00B U002 O00J 142.2(8) . . ?
O00B U002 O00K 143.1(8) . . ?
O00B U002 O2 79(3) . 5_566 ?
O00F U002 U001 97.1(4) . . ?
O00F U002 U001 40.3(4) . 5_566 ?
O00F U002 O00G 137.2(10) . 5_566 ?
O00F U002 O00J 73.3(7) . . ?
O00F U002 O00K 148.0(7) . . ?
O00F U002 O2 148(3) . 5_566 ?
O00G U002 U001 96.9(9) 5_566 5_566 ?
O00G U002 U001 40.1(9) 5_566 . ?
O00G U002 O00K 74.9(11) 5_566 . ?
O00G U002 O2 10(2) 5_566 5_566 ?
O00H U002 U001 91.8(4) . . ?
O00H U002 U001 91.8(4) 6_565 . ?
O00H U002 U001 91.7(5) . 5_566 ?
O00H U002 U001 91.7(5) 6_565 5_566 ?
O00H U002 O00B 92.0(4) 6_565 . ?
O00H U002 O00B 92.0(4) . . ?
O00H U002 O00F 90.6(6) 6_565 . ?
O00H U002 O00F 90.6(6) . . ?
O00H U002 O00G 90.9(6) 6_565 5_566 ?
O00H U002 O00G 90.9(6) . 5_566 ?
O00H U002 O00H 176.0(9) 6_565 . ?
O00H U002 O00J 88.3(5) 6_565 . ?
O00H U002 O00J 88.3(5) . . ?
O00H U002 O00K 88.5(6) 6_565 . ?
O00H U002 O00K 88.5(6) . . ?
O00H U002 O2 90.5(6) 6_565 5_566 ?
O00H U002 O2 90.5(6) . 5_566 ?
O00J U002 U001 170.4(6) . . ?
O00J U002 U001 113.6(6) . 5_566 ?
O00J U002 O00G 149.5(11) . 5_566 ?
O00J U002 O00K 74.6(8) . . ?
O00J U002 O2 139(3) . 5_566 ?
O00K U002 U001 171.7(6) . 5_566 ?
O00K U002 U001 114.9(6) . . ?
O2 U002 U001 107(2) 5_566 5_566 ?
O2 U002 U001 50(2) 5_566 . ?
O2 U002 O00K 64(3) 5_566 . ?
O00J Tc03 O1 107.4(11) . 6_565 ?
O00J Tc03 O1 107.4(11) . . ?
O1 Tc03 O1 112(2) . 6_565 ?
O13 Tc03 O00J 108(2) . . ?
O13 Tc03 O1 111.0(13) . . ?
O13 Tc03 O1 111.0(14) . 6_565 ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C5 H5A 109.5 5_666 . ?
C3 C5 H5B 109.5 5_666 . ?
C3 C5 H5C 109.5 5_666 . ?
U001 O00B U001 111.4(8) . 5_566 ?
U002 O00B U001 124.0(8) . 5_566 ?
U002 O00B U001 124.6(10) . . ?
C00M O00C U001 98(2) . 5_566 ?
C00M O00C Na4 151(2) . . ?
Na4 O00C U001 110.8(8) . 5_566 ?
C3 O00D U001 97.8(16) . 5_566 ?
C3 O00D Na4 150.4(18) . . ?
Na4 O00D U001 111.8(8) . 5_566 ?
U001 O00E Na4 173.2(7) . 3_445 ?
U002 O00F U001 104.0(6) . 5_566 ?
C3 O00F U001 95.1(15) . 5_566 ?
C3 O00F U002 160.8(17) . . ?
U002 O00G U001 103.6(14) 5_566 5_566 ?
C00M O00G U001 92(2) . 5_566 ?
C00M O00G U002 164(3) . 5_566 ?
Na4 O00I Na4 92.3(7) 5_566 1_455 ?
Tc03 O00J U002 158.8(14) . . ?
O00C C00M U001 58.7(17) . 5_566 ?
O00C C00M O00G 121(3) . . ?
O00C C00M C1 120(3) . . ?
O00C C00M O2 141(6) . . ?
O00G C00M U001 62(2) . 5_566 ?
O00G C00M C1 119(3) . . ?
C1 C00M U001 179(2) . 5_566 ?
O2 C00M U001 82(5) . 5_566 ?
O2 C00M O00G 20(5) . . ?
O2 C00M C1 99(6) . . ?
C5 C3 U001 178(3) 5_666 5_566 ?
O00D C3 U001 57.0(14) . 5_566 ?
O00D C3 C5 121(3) . 5_666 ?
O00D C3 O00F 116(2) . . ?
O00F C3 U001 59.4(13) . 5_566 ?
O00F C3 C5 123(3) . 5_666 ?
C00M C1 H1A 109.5 . . ?
C00M C1 H1B 109.5 . . ?
C00M C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
U001 Na4 U001 176.6(3) 3_545 3 ?
U001 Na4 U001 88.31(13) 5_566 3_545 ?
U001 Na4 U001 88.31(13) 5_566 3 ?
O00C Na4 U001 88.83(13) . 3_545 ?
O00C Na4 U001 88.83(13) . 3 ?
O00C Na4 U001 36.1(5) . 5_566 ?
O00C Na4 O00I 100.8(8) . 1_655 ?
O00C Na4 O00I 171.5(9) . 5_566 ?
O00C Na4 Na4 144.4(7) . 5_666 ?
O00D Na4 U001 88.45(14) . 3_545 ?
O00D Na4 U001 88.45(14) . 3 ?
O00D Na4 U001 36.2(5) . 5_566 ?
O00D Na4 O00C 72.4(7) . . ?
O00D Na4 O00I 99.2(8) . 5_566 ?
O00D Na4 O00I 173.1(8) . 1_655 ?
O00D Na4 Na4 143.2(7) . 5_666 ?
O00E Na4 U001 85.4(4) 3 5_566 ?
O00E Na4 U001 173.7(5) 8 3 ?
O00E Na4 U001 85.4(4) 8 5_566 ?
O00E Na4 U001 3.0(3) 3 3 ?
O00E Na4 U001 173.7(5) 3 3_545 ?
O00E Na4 U001 3.0(3) 8 3_545 ?
O00E Na4 O00C 86.2(4) 8 . ?
O00E Na4 O00C 86.2(4) 3 . ?
O00E Na4 O00D 86.4(4) 8 . ?
O00E Na4 O00D 86.4(4) 3 . ?
O00E Na4 O00E 170.8(8) 8 3 ?
O00E Na4 O00I 93.3(4) 3 1_655 ?
O00E Na4 O00I 93.4(4) 3 5_566 ?
O00E Na4 O00I 93.3(4) 8 1_655 ?
O00E Na4 O00I 93.4(4) 8 5_566 ?
O00E Na4 Na4 94.6(4) 8 5_666 ?
O00E Na4 Na4 94.6(4) 3 5_666 ?
O00I Na4 U001 90.98(14) 5_566 3_545 ?
O00I Na4 U001 91.45(14) 1_655 3 ?
O00I Na4 U001 90.98(14) 5_566 3 ?
O00I Na4 U001 91.45(14) 1_655 3_545 ?
O00I Na4 U001 135.4(6) 5_566 5_566 ?
O00I Na4 U001 136.9(5) 1_655 5_566 ?
O00I Na4 O00I 87.7(7) 5_566 1_655 ?
O00I Na4 Na4 43.7(5) 1_655 5_666 ?
O00I Na4 Na4 44.0(5) 5_566 5_666 ?
Na4 Na4 U001 91.69(13) 5_666 3 ?
Na4 Na4 U001 91.69(13) 5_666 3_545 ?
Na4 Na4 U001 179.4(5) 5_666 5_566 ?
C00M O2 U002 165(8) . 5_566 ?

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
U001 O00C C00M O00G 0.000(7) 5_566 . . . ?
U001 O00C C00M C1 180.000(5) 5_566 . . . ?
U001 O00C C00M O2 0.00(2) 5_566 . . . ?
U001 O00D C3 C5 180.000(18) 5_566 . . 5_666 ?
U001 O00D C3 O00F 0.000(7) 5_566 . . . ?
U001 O00F C3 C5 180.000(18) 5_566 . . 5_666 ?
U001 O00F C3 O00D 0.000(8) 5_566 . . . ?
U001 O00G C00M O00C 0.000(5) 5_566 . . . ?
U001 O00G C00M C1 180.000(6) 5_566 . . . ?
U001 O00G C00M O2 180.00(4) 5_566 . . . ?
U001 C00M O2 U002 0.00(4) 5_566 . . 5_566 ?
U002 O00F C3 U001 180.00(3) . . . 5_566 ?
U002 O00F C3 C5 0.00(3) . . . 5_666 ?
U002 O00F C3 O00D 180.000(15) . . . . ?
U002 O00G C00M U001 180.000(19) 5_566 . . 5_566 ?
U002 O00G C00M O00C 180.000(17) 5_566 . . . ?
U002 O00G C00M C1 0.00(2) 5_566 . . . ?
U002 O00G C00M O2 0.00(3) 5_566 . . . ?
O00C C00M O2 U002 0.00(6) . . . 5_566 ?
O00G C00M O2 U002 0.000(17) . . . 5_566 ?
O1 Tc03 O00J U002 119.9(11) . . . . ?
O1 Tc03 O00J U002 -119.9(11) 6_565 . . . ?
O13 Tc03 O00J U002 0.000(14) . . . . ?
C1 C00M O2 U002 180.00(3) . . . 5_566 ?
Na4 O00C C00M U001 180.000(12) . . . 5_566 ?
Na4 O00C C00M O00G 180.000(8) . . . . ?
Na4 O00C C00M C1 0.000(12) . . . . ?
Na4 O00C C00M O2 180.000(17) . . . . ?
Na4 O00D C3 U001 180.000(17) . . . 5_566 ?
Na4 O00D C3 C5 0.00(2) . . . 5_666 ?
Na4 O00D C3 O00F 180.000(11) . . . . ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.201
_oxdiff_exptl_absorpt_empirical_full_min 0.465
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.485(6)
2 0.515(6)

# start Validation Reply Form
_vrf_PLAT201_utc_3_thinplate_150815_auto 
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          8 Report
RESPONSE: Those sites are partially occupied and disordered and couldn't be anisotropically refined with good parameters. 
;
_vrf_PLAT342_utc_3_thinplate_150815_auto 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.06 Ang.  
RESPONSE: This low bond precision is due to disorder in C sites.
;
_vrf_PLAT430_utc_3_thinplate_150815_auto 
;
PROBLEM: Short Inter D...A Contact  O1       ..O00K     .       2.79 Ang.  
RESPONSE: This is due to the presence of H bond in between this two sites. 
;
_vrf_PLAT780_utc_3_thinplate_150815_auto 
;
PROBLEM: Coordinates do not Form a Properly Connected Set     Please Do !  
RESPONSE: This is due to the disordered and partially ocuupied site in the structure. Also, least square was used for the refinement, thus this alert can be ignored. 
;
# end Validation Reply Form
####################################################################### 
# 
# 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_ui_36_ms_mo_auto
_database_code_depnum_ccdc_archive 'CCDC 2332266'
loop_
_audit_author_name
_audit_author_address
'Mohammad Shohel'
;Oregon State University
United States of America
;
_audit_update_record             
;
2024-02-11 deposited with the CCDC.	2024-05-06 downloaded from the CCDC.
;
_audit_creation_date             2023-10-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H18 O32 Re2 U5'
_chemical_formula_sum            'C4 H18 O32 Re2 U5'
_chemical_formula_weight         2140.73
_chemical_melting_point          ?
_chemical_oxdiff_formula         UReO16C2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Re Re -1.0185 7.2310 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.7354(3)
_cell_length_b                   8.4717(3)
_cell_length_c                   12.7820(4)
_cell_angle_alpha                94.029(3)
_cell_angle_beta                 99.086(3)
_cell_angle_gamma                109.920(3)
_cell_volume                     770.66(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    6641
_cell_measurement_temperature    149.98(10)
_cell_measurement_theta_max      30.9270
_cell_measurement_theta_min      2.8480
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    34.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.613
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cube
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9602
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.861
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00 -17.00   0.50   70.00    --    4.12 -64.00 -71.00   98
  2  ω     -4.00  72.00   0.50   70.00    --    4.12  64.00  65.00  152
  3  ω    -70.00   5.00   0.50   70.00    --    4.12 -19.00 150.00  150
  4  ω    -12.00  22.00   0.50   70.00    --    4.12 -64.00 -71.00   68
  5  ω    -14.00  25.00   0.50   70.00    --    4.12 -99.00 -90.00   78
  6  ω    -15.00  23.00   0.50   70.00    --    4.12 -99.00  60.00   76
  7  ω    -14.00  11.00   0.50   70.00    --   -6.08 -99.00 -60.00   50
  8  ω    -39.00  14.00   0.50   70.00    --   -6.08 -77.00-120.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0099248000
_diffrn_orient_matrix_UB_12      -0.0538909000
_diffrn_orient_matrix_UB_13      -0.0418572000
_diffrn_orient_matrix_UB_21      0.0926588000
_diffrn_orient_matrix_UB_22      0.0567269000
_diffrn_orient_matrix_UB_23      0.0019995000
_diffrn_orient_matrix_UB_31      0.0346377000
_diffrn_orient_matrix_UB_32      -0.0441894000
_diffrn_orient_matrix_UB_33      0.0382038000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2840
_reflns_number_total             3149
_reflns_odcompleteness_completeness 94.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.309
_refine_diff_density_min         -1.420
_refine_diff_density_rms         0.237
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3149
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0197
_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)+(0.0177P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0443
_refine_ls_wR_factor_ref         0.0455
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 U3-H16A \\sim U3-H16B
 with sigma of 0.02
 U2-H12A \\sim U2-H12B
 with sigma of 0.02
3.a Free rotating group:
 O16(H16A,H16B), O12(H12A,H12B)
3.b Rotating group:
 O15(H15A,H15B)
3.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
;
_atom_sites_solution_hydrogens   mixed
_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 0.500000 0.500000 0.500000 0.01076(8) Uani 1 2 d S . P . .
U2 U 0.50188(3) 0.35030(3) 0.78630(2) 0.00940(6) Uani 1 1 d D . . . .
U3 U 0.24547(3) 0.64361(3) 0.71340(2) 0.00975(6) Uani 1 1 d D . . . .
Re4 Re 0.84721(3) 0.09694(3) 0.87975(2) 0.01274(7) Uani 1 1 d . . . . .
O17 O 0.6895(6) 0.1757(6) 0.8098(3) 0.0183(10) Uani 1 1 d . . . . .
O15 O 0.0884(6) 0.8362(6) 0.6481(3) 0.0167(9) Uani 1 1 d . . . . .
H15A H 0.144055 0.939908 0.685931 0.025 Uiso 1 1 d R U . . .
H15B H -0.029106 0.804028 0.660585 0.025 Uiso 1 1 d R U . . .
O18 O 0.7670(6) 0.0066(6) 0.9882(3) 0.0193(10) Uani 1 1 d . . . . .
O7 O 0.5927(6) 0.2956(6) 0.6155(3) 0.0165(9) Uani 1 1 d . . . . .
O10 O 0.7132(6) 0.5267(6) 0.8363(3) 0.0178(10) Uani 1 1 d . . . . .
O5 O 0.4141(6) 0.4948(5) 0.6617(3) 0.0133(9) Uani 1 1 d . . . . .
O9 O 0.2922(6) 0.1679(5) 0.7454(3) 0.0162(9) Uani 1 1 d . . . . .
O11 O 0.3296(6) 0.5015(5) 0.8558(3) 0.0134(9) Uani 1 1 d . . . . .
O16 O 0.0932(6) 0.7052(6) 0.8549(3) 0.0176(9) Uani 1 1 d G . . . .
H16A H -0.025292 0.685298 0.832196 0.026 Uiso 1 1 d DG U . . .
H16B H 0.139633 0.811852 0.881427 0.026 Uiso 1 1 d DG U . . .
O13 O 0.0322(6) 0.4734(6) 0.6614(3) 0.0180(9) Uani 1 1 d . . . . .
O14 O 0.4452(6) 0.8235(6) 0.7715(3) 0.0174(9) Uani 1 1 d . . . . .
O12 O 0.4974(6) 0.2807(6) 0.9666(3) 0.0158(9) Uani 1 1 d G . . . .
H12A H 0.553338 0.352390 1.024177 0.024 Uiso 1 1 d DG U . . .
H12B H 0.403818 0.204756 0.985566 0.024 Uiso 1 1 d DG U . . .
O20 O 0.8884(7) -0.0465(6) 0.7958(3) 0.0258(11) Uani 1 1 d . . . . .
O6 O 0.7156(6) 0.6690(6) 0.5572(3) 0.0176(9) Uani 1 1 d . . . . .
O8 O 0.6834(6) 0.3051(6) 0.4633(3) 0.0169(10) Uani 1 1 d . . . . .
C22 C 0.7392(9) 0.0992(9) 0.5680(4) 0.0203(14) Uani 1 1 d . . . . .
H22A H 0.658445 0.021565 0.608527 0.030 Uiso 1 1 calc R U . . .
H22B H 0.868130 0.144331 0.608763 0.030 Uiso 1 1 calc R U . . .
H22C H 0.735620 0.038139 0.499245 0.030 Uiso 1 1 calc R U . . .
O19 O 1.0538(7) 0.2633(7) 0.9279(4) 0.0259(11) Uani 1 1 d . . . . .
C21 C 0.6737(9) 0.2363(8) 0.5499(4) 0.0158(13) Uani 1 1 d . . . . .


_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 U2 3.9558(2) . ?
U1 U2 3.9558(2) 2_666 ?
U1 O7 2.562(4) 2_666 ?
U1 O7 2.562(4) . ?
U1 O5 2.267(4) 2_666 ?
U1 O5 2.267(4) . ?
U1 O6 1.791(5) . ?
U1 O6 1.791(5) 2_666 ?
U1 O8 2.580(4) . ?
U1 O8 2.580(4) 2_666 ?
U1 C21 3.030(7) 2_666 ?
U1 C21 3.030(7) . ?
U2 U3 3.7518(3) . ?
U2 O17 2.403(4) . ?
U2 O7 2.458(4) . ?
U2 O10 1.785(5) . ?
U2 O5 2.235(4) . ?
U2 O9 1.790(4) . ?
U2 O11 2.363(4) . ?
U2 O12 2.421(4) . ?
U3 O15 2.461(4) . ?
U3 O5 2.237(4) . ?
U3 O11 2.378(4) . ?
U3 O16 2.427(4) . ?
U3 O13 1.772(5) . ?
U3 O14 1.771(5) . ?
U3 O8 2.441(4) 2_666 ?
Re4 O17 1.739(4) . ?
Re4 O18 1.728(4) . ?
Re4 O20 1.708(4) . ?
Re4 O19 1.718(5) . ?
O15 H15A 0.8989 . ?
O15 H15B 0.8998 . ?
O7 C21 1.293(7) . ?
O16 H16A 0.8698 . ?
O16 H16B 0.8700 . ?
O12 H12A 0.8692 . ?
O12 H12B 0.8698 . ?
O8 C21 1.287(7) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C22 C21 1.435(9) . ?

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
U2 U1 U2 180.0 . 2_666 ?
O7 U1 U2 142.93(9) 2_666 . ?
O7 U1 U2 37.07(9) . . ?
O7 U1 U2 37.07(9) 2_666 2_666 ?
O7 U1 U2 142.93(9) . 2_666 ?
O7 U1 O7 180.00(12) 2_666 . ?
O7 U1 O8 49.86(12) 2_666 2_666 ?
O7 U1 O8 130.14(12) . 2_666 ?
O7 U1 O8 130.14(12) 2_666 . ?
O7 U1 O8 49.86(12) . . ?
O7 U1 C21 24.98(13) 2_666 2_666 ?
O7 U1 C21 155.03(13) . 2_666 ?
O7 U1 C21 155.02(13) 2_666 . ?
O7 U1 C21 24.98(13) . . ?
O5 U1 U2 28.31(10) . . ?
O5 U1 U2 151.69(10) . 2_666 ?
O5 U1 U2 151.69(10) 2_666 . ?
O5 U1 U2 28.31(10) 2_666 2_666 ?
O5 U1 O7 114.90(13) 2_666 . ?
O5 U1 O7 114.90(13) . 2_666 ?
O5 U1 O7 65.10(13) 2_666 2_666 ?
O5 U1 O7 65.10(13) . . ?
O5 U1 O5 180.0 2_666 . ?
O5 U1 O8 114.94(12) 2_666 2_666 ?
O5 U1 O8 65.06(12) 2_666 . ?
O5 U1 O8 114.94(12) . . ?
O5 U1 O8 65.06(12) . 2_666 ?
O5 U1 C21 90.08(14) 2_666 2_666 ?
O5 U1 C21 89.92(14) 2_666 . ?
O5 U1 C21 90.08(14) . . ?
O5 U1 C21 89.92(14) . 2_666 ?
O6 U1 U2 92.66(13) 2_666 . ?
O6 U1 U2 87.34(13) . . ?
O6 U1 U2 92.66(13) . 2_666 ?
O6 U1 U2 87.34(13) 2_666 2_666 ?
O6 U1 O7 91.27(17) 2_666 2_666 ?
O6 U1 O7 88.73(17) . 2_666 ?
O6 U1 O7 91.27(17) . . ?
O6 U1 O7 88.73(17) 2_666 . ?
O6 U1 O5 90.22(17) . 2_666 ?
O6 U1 O5 89.78(17) 2_666 2_666 ?
O6 U1 O5 89.78(17) . . ?
O6 U1 O5 90.22(17) 2_666 . ?
O6 U1 O6 180.0 . 2_666 ?
O6 U1 O8 90.03(18) . . ?
O6 U1 O8 89.97(18) 2_666 . ?
O6 U1 O8 89.97(18) . 2_666 ?
O6 U1 O8 90.03(18) 2_666 2_666 ?
O6 U1 C21 91.58(19) 2_666 2_666 ?
O6 U1 C21 88.42(19) 2_666 . ?
O6 U1 C21 91.58(19) . . ?
O6 U1 C21 88.42(19) . 2_666 ?
O8 U1 U2 86.73(8) . . ?
O8 U1 U2 93.27(8) 2_666 . ?
O8 U1 U2 86.73(8) 2_666 2_666 ?
O8 U1 U2 93.27(8) . 2_666 ?
O8 U1 O8 180.0 2_666 . ?
O8 U1 C21 155.08(13) 2_666 . ?
O8 U1 C21 155.08(13) . 2_666 ?
O8 U1 C21 24.92(13) . . ?
O8 U1 C21 24.92(13) 2_666 2_666 ?
C21 U1 U2 118.02(10) 2_666 . ?
C21 U1 U2 61.98(10) . . ?
C21 U1 U2 118.02(10) . 2_666 ?
C21 U1 U2 61.98(10) 2_666 2_666 ?
C21 U1 C21 180.0 . 2_666 ?
U3 U2 U1 61.715(5) . . ?
O17 U2 U1 109.66(9) . . ?
O17 U2 U3 171.04(10) . . ?
O17 U2 O7 71.41(13) . . ?
O17 U2 O12 74.91(14) . . ?
O7 U2 U1 38.93(10) . . ?
O7 U2 U3 100.29(9) . . ?
O10 U2 U1 89.14(13) . . ?
O10 U2 U3 90.62(14) . . ?
O10 U2 O17 86.65(18) . . ?
O10 U2 O7 93.89(17) . . ?
O10 U2 O5 90.62(18) . . ?
O10 U2 O9 175.79(17) . . ?
O10 U2 O11 89.69(18) . . ?
O10 U2 O12 89.01(17) . . ?
O5 U2 U1 28.75(10) . . ?
O5 U2 U3 32.99(10) . . ?
O5 U2 O17 138.40(13) . . ?
O5 U2 O7 67.38(14) . . ?
O5 U2 O11 70.82(13) . . ?
O5 U2 O12 146.60(14) . . ?
O9 U2 U1 95.03(13) . . ?
O9 U2 U3 91.87(14) . . ?
O9 U2 O17 91.38(18) . . ?
O9 U2 O7 89.01(17) . . ?
O9 U2 O5 93.32(18) . . ?
O9 U2 O11 90.20(18) . . ?
O9 U2 O12 86.88(17) . . ?
O11 U2 U1 99.51(9) . . ?
O11 U2 U3 37.83(9) . . ?
O11 U2 O17 150.51(13) . . ?
O11 U2 O7 138.06(13) . . ?
O11 U2 O12 75.78(14) . . ?
O12 U2 U1 174.95(11) . . ?
O12 U2 U3 113.61(11) . . ?
O12 U2 O7 145.95(14) . . ?
U2 U3 U1 61.678(5) . . ?
O15 U3 U1 112.46(9) . . ?
O15 U3 U2 174.13(9) . . ?
O5 U3 U1 28.73(9) . . ?
O5 U3 U2 32.96(9) . . ?
O5 U3 O15 141.18(13) . . ?
O5 U3 O11 70.51(13) . . ?
O5 U3 O16 144.87(14) . . ?
O5 U3 O8 67.95(13) . 2_666 ?
O11 U3 U1 99.20(10) . . ?
O11 U3 U2 37.55(10) . . ?
O11 U3 O15 148.30(14) . . ?
O11 U3 O16 74.54(14) . . ?
O11 U3 O8 138.09(14) . 2_666 ?
O16 U3 U1 173.44(10) . . ?
O16 U3 U2 111.99(10) . . ?
O16 U3 O15 73.88(14) . . ?
O16 U3 O8 147.18(14) . 2_666 ?
O13 U3 U1 91.90(14) . . ?
O13 U3 U2 92.60(14) . . ?
O13 U3 O15 87.72(18) . . ?
O13 U3 O5 91.79(19) . . ?
O13 U3 O11 93.20(17) . . ?
O13 U3 O16 86.58(18) . . ?
O13 U3 O8 93.40(18) . 2_666 ?
O14 U3 U1 93.51(14) . . ?
O14 U3 U2 91.57(15) . . ?
O14 U3 O15 88.53(18) . . ?
O14 U3 O5 93.83(19) . . ?
O14 U3 O11 87.74(17) . . ?
O14 U3 O16 88.24(17) . . ?
O14 U3 O13 174.3(2) . . ?
O14 U3 O8 89.64(17) . 2_666 ?
O8 U3 U1 39.25(10) 2_666 . ?
O8 U3 U2 100.81(10) 2_666 . ?
O8 U3 O15 73.32(14) 2_666 . ?
O18 Re4 O17 111.5(2) . . ?
O20 Re4 O17 109.8(2) . . ?
O20 Re4 O18 110.7(2) . . ?
O20 Re4 O19 109.0(3) . . ?
O19 Re4 O17 108.2(2) . . ?
O19 Re4 O18 107.6(2) . . ?
Re4 O17 U2 155.9(2) . . ?
U3 O15 H15A 110.6 . . ?
U3 O15 H15B 111.1 . . ?
H15A O15 H15B 103.1 . . ?
U2 O7 U1 104.00(15) . . ?
C21 O7 U1 98.2(3) . . ?
C21 O7 U2 157.2(4) . . ?
U2 O5 U1 122.95(18) . . ?
U2 O5 U3 114.05(15) . . ?
U3 O5 U1 122.95(16) . . ?
U2 O11 U3 104.62(14) . . ?
U3 O16 H16A 112.3 . . ?
U3 O16 H16B 112.1 . . ?
H16A O16 H16B 104.5 . . ?
U2 O12 H12A 124.6 . . ?
U2 O12 H12B 124.4 . . ?
H12A O12 H12B 104.6 . . ?
U3 O8 U1 103.98(14) 2_666 . ?
C21 O8 U1 97.5(4) . . ?
C21 O8 U3 158.4(4) . 2_666 ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
O7 C21 U1 56.8(3) . . ?
O7 C21 C22 123.5(5) . . ?
O8 C21 U1 57.6(3) . . ?
O8 C21 O7 114.3(6) . . ?
O8 C21 C22 122.1(5) . . ?
C22 C21 U1 174.4(5) . . ?

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
U1 O7 C21 O8 3.4(6) . . . . ?
U1 O7 C21 C22 -173.4(6) . . . . ?
U1 O8 C21 O7 -3.4(6) . . . . ?
U1 O8 C21 C22 173.4(5) . . . . ?
U2 O7 C21 U1 -167.2(11) . . . . ?
U2 O7 C21 O8 -163.8(8) . . . . ?
U2 O7 C21 C22 19.5(15) . . . . ?
U3 O8 C21 U1 -174.2(12) 2_666 . . . ?
U3 O8 C21 O7 -177.7(8) 2_666 . . . ?
U3 O8 C21 C22 -0.8(16) 2_666 . . . ?
O18 Re4 O17 U2 59.3(7) . . . . ?
O20 Re4 O17 U2 -177.6(6) . . . . ?
O19 Re4 O17 U2 -58.8(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
;
_oxdiff_exptl_absorpt_empirical_full_max 3.096
_oxdiff_exptl_absorpt_empirical_full_min 0.531

# start Validation Reply Form
_vrf_PLAT430_ui_36_ms_mo_auto    
;
PROBLEM: Short Inter D...A Contact  O11      ..O19      .       2.72 Ang.  
RESPONSE: Thi is due to the presence of hydrogen bond which is described in the manuscript. 
;
# end Validation Reply Form
####################################################################### 
# 
# 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_utc_10_070812_ms_auto
_database_code_depnum_ccdc_archive 'CCDC 2332267'
loop_
_audit_author_name
_audit_author_address
'Mohammad Shohel'
;Oregon State University
United States of America
;
_audit_update_record             
;
2024-02-11 deposited with the CCDC.	2024-05-06 downloaded from the CCDC.
;
_audit_creation_date             2023-09-06
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H6 O32 Tc2 U5'
_chemical_formula_sum            'C4 H6 O32 Tc2 U5'
_chemical_formula_weight         1952.24
_chemical_melting_point          ?
_chemical_oxdiff_formula         'U5 Tc2 O32 C4 H20'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc 0.0057 3.0049 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.7451(3)
_cell_length_b                   8.4501(2)
_cell_length_c                   12.7565(5)
_cell_angle_alpha                93.982(3)
_cell_angle_beta                 99.211(3)
_cell_angle_gamma                109.708(3)
_cell_volume                     768.96(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    8377
_cell_measurement_temperature    172.97(10)
_cell_measurement_theta_max      76.8720
_cell_measurement_theta_min      3.5520
_shelx_estimated_absorpt_T_max   0.294
_shelx_estimated_absorpt_T_min   0.140
_exptl_absorpt_coefficient_mu    81.160
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.216
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10031
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.170
_diffrn_reflns_theta_min         3.541
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.97(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -38.00   7.00   0.50    6.00    --  -47.14  36.00 -34.00   90
  2  ω   -116.00 -41.00   0.50    6.00    --  -47.14 -36.00 169.00  150
  3  ω     -7.00  33.00   0.50    6.00    --   47.14 -36.00 169.00   80
  4  ω     37.00 120.00   0.50    6.00    --   47.14  36.00 -34.00  166
  5  ω   -125.00-100.00   0.50    8.00    --  -86.25 -36.00 169.00   50
  6  ω    -41.00 -14.00   0.50    8.00    --  -86.25  36.00 -34.00   54
  7  ω    138.00 178.00   0.50    8.00    --  107.75  36.00 -34.00   80
  8  ω   -118.00 -89.00   0.50    6.00    --  -47.14 -77.00  60.00   58
  9  ω   -118.00 -93.00   0.50    6.00    --  -47.14 -77.00-180.00   50
 10  ω   -118.00 -79.00   0.50    6.00    --  -47.14-125.00 -60.00   78
 11  ω     42.00  78.00   0.50    6.00    --   47.14-125.00  30.00   72
 12  ω     85.00 115.00   0.50    6.00    --   47.14  77.00  30.00   60
 13  ω     65.00  93.00   0.50    6.00    --   47.14-125.00-150.00   56
 14  ω     42.00  74.00   0.50    6.00    --   47.14 -99.00-180.00   64
 15  ω     35.00  61.00   0.50    6.00    --   47.14-125.00-150.00   52
 16  ω     46.00 106.00   0.50    8.00    --  107.75 -77.00 -60.00  120
 17  ω     87.00 112.00   0.50    8.00    --  107.75-125.00   0.00   50
 18  ω     36.00  71.00   0.50    8.00    --  107.75 -61.00 120.00   70
 19  ω     49.00 105.00   0.50    8.00    --  107.75 -77.00  30.00  112
 20  ω     58.00 110.00   0.50    8.00    --  107.75-125.00-150.00  104
 21  ω     35.00  66.00   0.50    8.00    --  107.75 -85.00-148.01   62
 22  ω     35.00  70.00   0.50    8.00    --  107.75 -61.00 -30.00   70
 23  ω    100.00 136.00   0.50    8.00    --  107.75  30.00 -60.00   72
 24  ω    126.00 176.00   0.50    8.00    --  107.75  77.00 -90.00  100
 25  ω    100.00 125.00   0.50    8.00    --  107.75  61.00-180.00   50
 26  ω     59.00 100.00   0.50    8.00    --  107.75 -94.00 -90.00   82
 27  ω    102.00 156.00   0.50    8.00    --  107.75  45.00 120.00  108
 28  ω     95.00 160.00   0.50    8.00    --  107.75  15.00  60.00  130
 29  ω     38.00  71.00   0.50    8.00    --  107.75-125.00   0.00   66
 30  ω    104.00 148.00   0.50    8.00    --  107.75  45.00   0.00   88
 31  ω     73.00 129.00   0.50    8.00    --  107.75 -88.00 117.48  112
 32  ω     65.00 101.00   0.50    8.00    --  107.75 -94.00  90.00   72
 33  ω     35.00  80.00   0.50    8.00    --  107.75-125.00 150.00   90
 34  ω    107.00 132.00   0.50    8.00    --  107.75  45.00-180.00   50
 35  ω    139.00 167.00   0.50    8.00    --  107.75  45.00-180.00   56
 36  ω     66.00 117.00   0.50    8.00    --  107.75 -87.00  53.68  102
 37  ω     35.00  81.00   0.50    8.00    --  107.75 -77.00   0.00   92
 38  ω     35.00  62.00   0.50    8.00    --  107.75 -61.00  60.00   54
 39  ω     51.00  77.00   0.50    8.00    --  107.75 -94.00-120.00   52
 40  ω    101.00 155.00   0.50    8.00    --  107.75  45.00 150.00  108
 41  ω     44.00  69.00   0.50    8.00    --  107.75 -61.00 -90.00   50
 42  ω     88.00 132.00   0.50    8.00    --  107.75 -85.00-148.01   88
 43  ω     50.00 105.00   0.50    8.00    --  107.75 -94.00-150.00  110
 44  ω    100.00 126.00   0.50    8.00    --  107.75 125.00-150.00   52
 45  ω     94.00 163.00   0.50    8.00    --  107.75  15.00 -90.00  138
 46  ω     35.00  73.00   0.50    8.00    --  107.75 -94.00 120.00   76
 47  ω    107.00 150.00   0.50    8.00    --  107.75  45.00  60.00   86
 48  ω     38.00  64.00   0.50    8.00    --  107.75 -86.00-108.13   52
 49  ω     97.00 122.00   0.50    8.00    --  107.75 -86.00-108.13   50
 50  ω     49.00 101.00   0.50    8.00    --  107.75 -94.00  30.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1094387000
_diffrn_orient_matrix_UB_12      0.1924887000
_diffrn_orient_matrix_UB_13      0.0218605000
_diffrn_orient_matrix_UB_21      -0.1563367000
_diffrn_orient_matrix_UB_22      0.0257902000
_diffrn_orient_matrix_UB_23      0.0522167000
_diffrn_orient_matrix_UB_31      0.0999757000
_diffrn_orient_matrix_UB_32      -0.0214361000
_diffrn_orient_matrix_UB_33      0.1096929000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2699
_reflns_number_total             2797
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.047
_refine_diff_density_min         -1.923
_refine_diff_density_rms         0.336
_refine_ls_extinction_coef       0.00033(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2797
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0260
_refine_ls_restrained_S_all      1.109
_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)+(0.0404P)²+6.9353P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0681
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
;
_atom_sites_solution_hydrogens   geom
_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 0.75649(3) 0.35701(3) 0.28710(2) 0.00895(11) Uani 1 1 d . . . . .
U2 U 0.49818(3) 0.65048(3) 0.21322(2) 0.00847(11) Uani 1 1 d . . . . .
U3 U 0.500000 0.500000 0.500000 0.00932(12) Uani 1 2 d S . P . .
Tc4 Tc 0.15375(9) 0.90270(9) 0.11929(5) 0.01601(16) Uani 1 1 d . . . . .
O7 O 0.5861(8) 0.5065(8) 0.3374(4) 0.0151(12) Uani 1 1 d . . . . .
O9 O 0.9109(9) 0.2974(8) 0.1459(5) 0.0215(13) Uani 1 1 d . . . . .
O13 O 0.5032(9) 0.7195(8) 0.0314(5) 0.0184(13) Uani 1 1 d . . . . .
O10 O 0.9138(8) 0.1625(8) 0.3518(5) 0.0177(13) Uani 1 1 d . . . . .
O16 O 0.3160(9) 0.6948(8) 0.5354(5) 0.0186(13) Uani 1 1 d . . . . .
O8 O 0.6726(8) 0.4995(7) 0.1447(4) 0.0123(11) Uani 1 1 d . . . . .
O18 O 0.2364(10) 0.9901(9) 0.0105(5) 0.0236(14) Uani 1 1 d . . . . .
O17 O 0.3102(9) 0.8243(8) 0.1901(5) 0.0200(13) Uani 1 1 d . . . . .
O14 O 0.4069(9) 0.7041(8) 0.3845(4) 0.0164(12) Uani 1 1 d . . . . .
O20 O 0.1128(11) 1.0467(10) 0.2016(6) 0.0322(17) Uani 1 1 d . . . . .
C21 C 0.3280(12) 0.7626(11) 0.4512(7) 0.0165(17) Uani 1 1 d . . . . .
O19 O -0.0518(10) 0.7387(11) 0.0716(6) 0.0337(17) Uani 1 1 d . . . . .
C22 C 0.2605(14) 0.9020(12) 0.4302(7) 0.0198(19) Uani 1 1 d . . . . .
H22A H 0.259631 0.962618 0.498318 0.030 Uiso 1 1 calc R U . . .
H22B H 0.133441 0.856207 0.387156 0.030 Uiso 1 1 calc R U . . .
H22C H 0.343302 0.980283 0.391066 0.030 Uiso 1 1 calc R U . . .
O11 O 0.7074(9) 0.8329(8) 0.2549(5) 0.0179(13) Uani 1 1 d . . . . .
O12 O 0.2889(9) 0.4758(8) 0.1631(5) 0.0173(13) Uani 1 1 d . . . . .
O5 O 0.5577(9) 0.1783(9) 0.2285(5) 0.0201(14) Uani 1 1 d . . . . .
O6 O 0.9669(9) 0.5255(9) 0.3399(5) 0.0217(14) Uani 1 1 d . . . . .
O15 O 0.2854(9) 0.3319(8) 0.4419(5) 0.0183(13) Uani 1 1 d . . . . .


_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 U2 3.7560(4) . ?
U1 U3 3.9589(3) . ?
U1 O7 2.243(6) . ?
U1 O9 2.429(6) . ?
U1 O10 2.466(6) . ?
U1 O16 2.452(6) 2_666 ?
U1 O8 2.372(6) . ?
U1 O5 1.765(7) . ?
U1 O6 1.757(7) . ?
U2 U3 3.9551(3) . ?
U2 O7 2.222(6) . ?
U2 O13 2.434(6) . ?
U2 O8 2.366(6) . ?
U2 O17 2.394(6) . ?
U2 O14 2.460(6) . ?
U2 O11 1.792(6) . ?
U2 O12 1.772(6) . ?
U3 O7 2.277(6) . ?
U3 O7 2.277(6) 2_666 ?
U3 O16 2.574(6) 2_666 ?
U3 O16 2.574(6) . ?
U3 O14 2.554(6) . ?
U3 O14 2.554(6) 2_666 ?
U3 C21 3.001(9) . ?
U3 C21 3.001(9) 2_666 ?
U3 O15 1.788(6) . ?
U3 O15 1.788(6) 2_666 ?
Tc4 O18 1.729(6) . ?
Tc4 O17 1.731(6) . ?
Tc4 O20 1.695(7) . ?
Tc4 O19 1.706(7) . ?
O16 C21 1.254(11) . ?
O14 C21 1.285(11) . ?
C21 C22 1.465(13) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

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
U2 U1 U3 61.615(6) . . ?
O7 U1 U2 32.54(14) . . ?
O7 U1 U3 29.09(14) . . ?
O7 U1 O9 144.4(2) . . ?
O7 U1 O10 141.9(2) . . ?
O7 U1 O16 68.20(19) . 2_666 ?
O7 U1 O8 70.05(19) . . ?
O9 U1 U2 111.91(15) . . ?
O9 U1 U3 173.24(16) . . ?
O9 U1 O10 73.7(2) . . ?
O9 U1 O16 147.4(2) . 2_666 ?
O10 U1 U2 174.42(14) . . ?
O10 U1 U3 112.83(14) . . ?
O16 U1 U2 100.63(14) 2_666 . ?
O16 U1 U3 39.15(14) 2_666 . ?
O16 U1 O10 73.8(2) 2_666 . ?
O8 U1 U2 37.51(13) . . ?
O8 U1 U3 99.10(13) . . ?
O8 U1 O9 74.5(2) . . ?
O8 U1 O10 148.0(2) . . ?
O8 U1 O16 137.89(19) . 2_666 ?
O5 U1 U2 91.1(2) . . ?
O5 U1 U3 93.3(2) . . ?
O5 U1 O7 93.4(3) . . ?
O5 U1 O9 88.7(3) . . ?
O5 U1 O10 88.6(3) . . ?
O5 U1 O16 89.7(3) . 2_666 ?
O5 U1 O8 87.5(3) . . ?
O6 U1 U2 92.8(2) . . ?
O6 U1 U3 91.8(2) . . ?
O6 U1 O7 91.9(3) . . ?
O6 U1 O9 86.5(3) . . ?
O6 U1 O10 87.8(3) . . ?
O6 U1 O16 93.1(3) . 2_666 ?
O6 U1 O8 93.4(3) . . ?
O6 U1 O5 174.6(3) . . ?
U1 U2 U3 61.717(6) . . ?
O7 U2 U1 32.90(15) . . ?
O7 U2 U3 28.84(15) . . ?
O7 U2 O13 146.2(2) . . ?
O7 U2 O8 70.5(2) . . ?
O7 U2 O17 138.2(2) . . ?
O7 U2 O14 67.3(2) . . ?
O13 U2 U1 113.30(15) . . ?
O13 U2 U3 174.62(15) . . ?
O13 U2 O14 146.4(2) . . ?
O8 U2 U1 37.62(13) . . ?
O8 U2 U3 99.31(13) . . ?
O8 U2 O13 75.7(2) . . ?
O8 U2 O17 151.02(19) . . ?
O8 U2 O14 137.68(19) . . ?
O17 U2 U1 170.79(15) . . ?
O17 U2 U3 109.39(15) . . ?
O17 U2 O13 75.5(2) . . ?
O17 U2 O14 71.3(2) . . ?
O14 U2 U1 100.13(14) . . ?
O14 U2 U3 38.76(14) . . ?
O11 U2 U1 91.6(2) . . ?
O11 U2 U3 94.9(2) . . ?
O11 U2 O7 93.1(3) . . ?
O11 U2 O13 87.2(3) . . ?
O11 U2 O8 89.9(3) . . ?
O11 U2 O17 91.6(3) . . ?
O11 U2 O14 89.0(3) . . ?
O12 U2 U1 90.9(2) . . ?
O12 U2 U3 89.2(2) . . ?
O12 U2 O7 90.8(3) . . ?
O12 U2 O13 88.8(2) . . ?
O12 U2 O8 90.1(3) . . ?
O12 U2 O17 86.4(3) . . ?
O12 U2 O14 93.8(3) . . ?
O12 U2 O11 175.9(3) . . ?
U2 U3 U2 180.0 2_666 . ?
O7 U3 U2 28.08(14) 2_666 2_666 ?
O7 U3 U2 151.92(14) . 2_666 ?
O7 U3 U2 151.92(14) 2_666 . ?
O7 U3 U2 28.08(14) . . ?
O7 U3 O7 180.0 . 2_666 ?
O7 U3 O16 65.54(19) 2_666 . ?
O7 U3 O16 114.46(19) . . ?
O7 U3 O16 65.54(19) . 2_666 ?
O7 U3 O16 114.46(19) 2_666 2_666 ?
O7 U3 O14 64.89(19) 2_666 2_666 ?
O7 U3 O14 115.11(19) 2_666 . ?
O7 U3 O14 115.11(19) . 2_666 ?
O7 U3 O14 64.89(19) . . ?
O7 U3 C21 90.0(2) . 2_666 ?
O7 U3 C21 90.0(2) 2_666 2_666 ?
O7 U3 C21 90.0(2) . . ?
O7 U3 C21 90.0(2) 2_666 . ?
O16 U3 U2 86.48(13) 2_666 2_666 ?
O16 U3 U2 93.52(13) . 2_666 ?
O16 U3 U2 86.48(13) . . ?
O16 U3 U2 93.52(13) 2_666 . ?
O16 U3 O16 180.0 . 2_666 ?
O16 U3 C21 24.5(2) 2_666 2_666 ?
O16 U3 C21 155.5(2) 2_666 . ?
O16 U3 C21 155.5(2) . 2_666 ?
O16 U3 C21 24.5(2) . . ?
O14 U3 U2 37.09(13) 2_666 2_666 ?
O14 U3 U2 142.91(13) 2_666 . ?
O14 U3 U2 37.09(13) . . ?
O14 U3 U2 142.91(13) . 2_666 ?
O14 U3 O16 49.59(19) 2_666 2_666 ?
O14 U3 O16 49.59(19) . . ?
O14 U3 O16 130.41(19) . 2_666 ?
O14 U3 O16 130.41(19) 2_666 . ?
O14 U3 O14 180.0 2_666 . ?
O14 U3 C21 25.1(2) . . ?
O14 U3 C21 154.9(2) 2_666 . ?
O14 U3 C21 154.9(2) . 2_666 ?
O14 U3 C21 25.1(2) 2_666 2_666 ?
C21 U3 U2 117.81(16) . 2_666 ?
C21 U3 U2 117.81(16) 2_666 . ?
C21 U3 U2 62.19(16) . . ?
C21 U3 U2 62.19(16) 2_666 2_666 ?
C21 U3 C21 180.00(15) . 2_666 ?
O15 U3 U2 93.0(2) 2_666 . ?
O15 U3 U2 93.0(2) . 2_666 ?
O15 U3 U2 87.0(2) . . ?
O15 U3 U2 87.0(2) 2_666 2_666 ?
O15 U3 O7 90.4(3) . 2_666 ?
O15 U3 O7 90.4(3) 2_666 . ?
O15 U3 O7 89.6(3) . . ?
O15 U3 O7 89.6(3) 2_666 2_666 ?
O15 U3 O16 90.2(3) 2_666 . ?
O15 U3 O16 89.8(3) . . ?
O15 U3 O16 90.2(3) . 2_666 ?
O15 U3 O16 89.8(3) 2_666 2_666 ?
O15 U3 O14 90.9(3) 2_666 2_666 ?
O15 U3 O14 89.1(3) . 2_666 ?
O15 U3 O14 90.9(3) . . ?
O15 U3 O14 89.1(3) 2_666 . ?
O15 U3 C21 88.5(3) . 2_666 ?
O15 U3 C21 88.5(3) 2_666 . ?
O15 U3 C21 91.5(3) . . ?
O15 U3 C21 91.5(3) 2_666 2_666 ?
O15 U3 O15 180.0(4) . 2_666 ?
O18 Tc4 O17 110.7(3) . . ?
O20 Tc4 O18 111.2(4) . . ?
O20 Tc4 O17 109.8(3) . . ?
O20 Tc4 O19 108.7(4) . . ?
O19 Tc4 O18 107.7(3) . . ?
O19 Tc4 O17 108.6(4) . . ?
U1 O7 U3 122.3(2) . . ?
U2 O7 U1 114.6(2) . . ?
U2 O7 U3 123.1(3) . . ?
U1 O16 U3 103.9(2) 2_666 . ?
C21 O16 U1 158.8(6) . 2_666 ?
C21 O16 U3 97.2(5) . . ?
U2 O8 U1 104.9(2) . . ?
Tc4 O17 U2 155.3(3) . . ?
U2 O14 U3 104.1(2) . . ?
C21 O14 U2 158.1(5) . . ?
C21 O14 U3 97.3(5) . . ?
O16 C21 U3 58.3(5) . . ?
O16 C21 O14 115.7(8) . . ?
O16 C21 C22 122.6(8) . . ?
O14 C21 U3 57.6(4) . . ?
O14 C21 C22 121.6(7) . . ?
C22 C21 U3 175.0(6) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

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
U1 O16 C21 U3 172.5(18) 2_666 . . . ?
U1 O16 C21 O14 177.1(12) 2_666 . . . ?
U1 O16 C21 C22 -2(2) 2_666 . . . ?
U2 O14 C21 U3 168.3(17) . . . . ?
U2 O14 C21 O16 163.7(11) . . . . ?
U2 O14 C21 C22 -17(2) . . . . ?
U3 O16 C21 O14 4.6(8) . . . . ?
U3 O16 C21 C22 -174.2(8) . . . . ?
U3 O14 C21 O16 -4.6(8) . . . . ?
U3 O14 C21 C22 174.2(7) . . . . ?
O18 Tc4 O17 U2 -57.7(9) . . . . ?
O20 Tc4 O17 U2 179.1(8) . . . . ?
O19 Tc4 O17 U2 60.3(9) . . . . ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 3.004
_oxdiff_exptl_absorpt_empirical_full_min 0.336

# start Validation Reply Form
_vrf_PLAT430_utc_10_070812_ms_auto 
;
PROBLEM: Short Inter D...A Contact  O8       ..O13      .       2.66 Ang.  
RESPONSE: This is due to the presence of hydrogen bond which has been discussed in the manuscript. 
;
# end Validation Reply Form
####################################################################### 
# 
# 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_utc_3_rod_131414_cu_auto
_database_code_depnum_ccdc_archive 'CCDC 2332268'
loop_
_audit_author_name
_audit_author_address
'Mohammad Shohel'
;Oregon State University
United States of America
;
_audit_update_record             
;
2024-02-11 deposited with the CCDC.	2024-05-06 downloaded from the CCDC.
;
_audit_creation_date             2023-06-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H20 O25 Tc U4, 0.75(O)'
_chemical_formula_sum            'C8 H20 O25.75 Tc U4'
_chemical_formula_weight         1578.36
_chemical_melting_point          ?
_chemical_oxdiff_formula         'U Tc O C'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc 0.0057 3.0049 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 '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           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   14.3710(3)
_cell_length_b                   13.8231(3)
_cell_length_c                   14.8033(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2940.70(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    16660
_cell_measurement_temperature    222.99(10)
_cell_measurement_theta_max      76.5190
_cell_measurement_theta_min      2.9920
_shelx_estimated_absorpt_T_max   0.559
_shelx_estimated_absorpt_T_min   0.077
_exptl_absorpt_coefficient_mu    65.775
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.565
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2740
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0847
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36295
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         4.438
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      222.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_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    -58.00  21.00   0.50    5.00    --  -47.14  57.00-150.00  158
  2  ω   -119.00 -89.00   0.50    5.00    --  -47.14 -77.00 -30.00   60
  3  ω    -61.00  24.00   0.50    5.00    --  -47.14  57.00  90.00  170
  4  ω   -119.00 -92.00   0.50    5.00    --  -47.14 -77.00   0.00   54
  5  ω    -25.00  22.00   0.50    5.00    --   47.14 -19.00   0.00   94
  6  ω     88.00 115.00   0.50    5.00    --   47.14  77.00  60.00   54
  7  ω    -25.00 119.00   0.50    5.00    --   47.14   0.00  30.00  288
  8  ω    -80.00 -38.00   0.50    8.00    --  -86.25 125.00 -60.00   84
  9  ω     99.00 171.00   0.50    8.00    --  107.75  30.00  30.00  144
 10  ω     50.00 106.00   0.50    8.00    --  107.75 -94.00 120.00  112
 11  ω     35.00  70.00   0.50    8.00    --  107.75 -61.00 150.00   70
 12  ω     99.00 170.00   0.50    8.00    --  107.75  15.00  90.00  142
 13  ω     59.00 105.00   0.50    8.00    --  107.75 -94.00-180.00   92
 14  ω     35.00  69.00   0.50    8.00    --  107.75 -77.00 -90.00   68
 15  ω     35.00  73.00   0.50    8.00    --  107.75 -87.00-110.33   76
 16  ω     39.00  64.00   0.50    8.00    --  107.75 -61.00-180.00   50
 17  ω    130.00 162.00   0.50    8.00    --  107.75  45.00-120.00   64
 18  ω     41.00  97.00   0.50    8.00    --  107.75 -77.00  30.00  112
 19  ω     43.00  69.00   0.50    8.00    --  107.75 -61.00  30.00   52
 20  ω     42.00  70.00   0.50    8.00    --  107.75 -77.00 120.00   56
 21  ω     38.00  63.00   0.50    8.00    --  107.75 -61.00 -90.00   50
 22  ω    110.00 178.00   0.50    8.00    --  107.75  30.00   0.00  136
 23  ω     95.00 167.00   0.50    8.00    --  107.75  45.00 -30.00  144
 24  ω     49.00  92.00   0.50    8.00    --  107.75-125.00 -90.00   86
 25  ω    103.00 131.00   0.50    8.00    --  107.75  45.00  90.00   56
 26  ω    144.00 178.00   0.50    8.00    --  107.75  45.00  90.00   68
 27  ω     35.00  60.00   0.50    8.00    --  107.75 -61.00-120.00   50
 28  ω     40.00  65.00   0.50    8.00    --  107.75 -61.00   0.00   50
 29  ω     40.00  71.00   0.50    8.00    --  107.75 -61.00 120.00   62
 30  ω     71.00 105.00   0.50    8.00    --  107.75 -77.00 -90.00   68
 31  ω    145.00 172.00   0.50    8.00    --  107.75 125.00  90.00   54
 32  ω     95.00 122.00   0.50    8.00    --  107.75 125.00  90.00   54
 33  ω     77.00 103.00   0.50    8.00    --  107.75 -94.00  90.00   52
 34  ω     41.00  71.00   0.50    8.00    --  107.75 -94.00  90.00   60
 35  ω     36.00 105.00   0.50    8.00    --  107.75 -94.00-150.00  138
 36  ω     37.00  62.00   0.50    8.00    --  107.75-125.00-120.00   50
 37  ω    108.00 175.00   0.50    8.00    --  107.75  30.00 120.00  134
 38  ω     97.00 123.00   0.50    8.00    --  107.75  45.00-120.00   52
 39  ω     88.00 115.00   0.50    8.00    --  107.75 -87.00-110.33   54
 40  ω     67.00 106.00   0.50    8.00    --  107.75 -94.00 150.00   78
 41  ω     55.00 105.00   0.50    8.00    --  107.75 -77.00 -30.00  100
 42  ω     68.00  95.00   0.50    8.00    --  107.75 -77.00  60.00   54
 43  ω     74.00 122.00   0.50    8.00    --  107.75 -87.00 -10.88   96
 44  ω     81.00 106.00   0.50    8.00    --  107.75 -77.00-120.00   50
 45  ω     76.00 105.00   0.50    8.00    --  107.75 -94.00-120.00   58
 46  ω     92.00 134.00   0.50    8.00    --  107.75 -88.00 -65.47   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0140774000
_diffrn_orient_matrix_UB_12      0.0590811000
_diffrn_orient_matrix_UB_13      -0.0872043000
_diffrn_orient_matrix_UB_21      -0.1043525000
_diffrn_orient_matrix_UB_22      -0.0256910000
_diffrn_orient_matrix_UB_23      0.0007717000
_diffrn_orient_matrix_UB_31      -0.0202587000
_diffrn_orient_matrix_UB_32      0.0909364000
_diffrn_orient_matrix_UB_33      0.0567442000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2488
_reflns_number_total             2695
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.393
_refine_diff_density_min         -2.572
_refine_diff_density_rms         0.272
_refine_ls_extinction_coef       0.000061(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2695
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0383
_refine_ls_restrained_S_all      1.066
_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)+(0.0529P)²+40.1766P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1013
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O21(0.25) O22(0.125)
3.a Rotating group:
 O14(H14A,H14B), O12(H12A,H12B)
3.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   mixed
_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 0.44329(3) 0.67681(3) 0.04850(2) 0.03781(16) Uani 1 1 d . . . . .
U2 U 0.29637(2) 0.66859(3) 0.30576(3) 0.03968(17) Uani 1 1 d . . . . .
Tc3 Tc 0.500000 0.77793(10) 0.250000 0.0411(3) Uani 1 2 d S T P . .
O4 O 0.4210(5) 0.7950(6) 0.0064(5) 0.0457(18) Uani 1 1 d . . . . .
O9 O 0.5606(5) 0.7314(6) 0.1456(5) 0.0416(17) Uani 1 1 d . . . . .
O16 O 0.4213(7) 0.6734(6) 0.5411(6) 0.053(2) Uani 1 1 d . . . . .
O6 O 0.2469(6) 0.7836(7) 0.3246(6) 0.055(2) Uani 1 1 d . . . . .
O10 O 0.3916(5) 0.7294(6) 0.1914(5) 0.0418(18) Uani 1 1 d . . . . .
O14 O 0.1408(6) 0.6034(8) 0.3499(7) 0.064(3) Uani 1 1 d . . . . .
H14A H 0.117981 0.638456 0.392449 0.096 Uiso 1 1 d R U . . .
H14B H 0.102557 0.610436 0.305617 0.096 Uiso 1 1 d R U . . .
O7 O 0.3439(6) 0.5518(6) 0.2874(6) 0.050(2) Uani 1 1 d . . . . .
O5 O 0.4642(6) 0.5590(6) 0.0882(6) 0.052(2) Uani 1 1 d . . . . .
O8 O 0.500000 0.8977(10) 0.250000 0.062(3) Uani 1 2 d S T P . .
O15 O 0.2977(6) 0.6323(8) 0.4592(6) 0.059(2) Uani 1 1 d . . . . .
O12 O 0.4002(7) 0.6131(7) -0.1008(6) 0.062(2) Uani 1 1 d . . . . .
H12A H 0.419852 0.550660 -0.108300 0.092 Uiso 1 1 d R U . . .
H12B H 0.430521 0.644230 -0.146760 0.092 Uiso 1 1 d R U . . .
O11 O 0.2833(6) 0.6444(8) 0.0503(6) 0.057(2) Uani 1 1 d . . . . .
O13 O 0.2028(6) 0.6471(7) 0.1765(6) 0.054(2) Uani 1 1 d . . . . .
C19 C 0.2114(8) 0.6291(9) 0.0913(8) 0.046(3) Uani 1 1 d . . . . .
C17 C 0.3387(8) 0.6415(9) 0.5343(8) 0.041(2) Uani 1 1 d . . . . .
C18 C 0.2894(8) 0.6146(9) 0.6172(8) 0.046(3) Uani 1 1 d . . . . .
H18A H 0.304507 0.548340 0.633036 0.069 Uiso 1 1 calc R U . . .
H18B H 0.222822 0.620279 0.607563 0.069 Uiso 1 1 calc R U . . .
H18C H 0.308077 0.657331 0.665895 0.069 Uiso 1 1 calc R U . . .
C20 C 0.1300(9) 0.5857(11) 0.0436(10) 0.060(3) Uani 1 1 d . . . . .
H20A H 0.134225 0.599676 -0.020502 0.090 Uiso 1 1 calc R U . . .
H20B H 0.072942 0.613072 0.067553 0.090 Uiso 1 1 calc R U . . .
H20C H 0.129839 0.516225 0.052705 0.090 Uiso 1 1 calc R U . . .
O21 O 0.000000 0.7076(19) 0.250000 0.056(6) Uiso 0.5 2 d S . P . .
O22 O 0.500000 0.582(3) -0.250000 0.049(11) Uiso 0.25 2 d S . P . .


_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 Tc3 3.3935(7) . ?
U1 O4 1.778(9) . ?
U1 O9 2.341(7) . ?
U1 O16 2.356(9) 3_655 ?
U1 O10 2.356(7) . ?
U1 O5 1.757(8) . ?
U1 O12 2.459(9) . ?
U1 O11 2.342(8) . ?
U2 Tc3 3.3955(7) . ?
U2 O9 2.344(7) 3_655 ?
U2 O6 1.763(9) . ?
U2 O10 2.334(7) . ?
U2 O14 2.497(8) . ?
U2 O7 1.774(8) . ?
U2 O15 2.327(9) . ?
U2 O13 2.358(9) . ?
Tc3 O9 1.887(7) . ?
Tc3 O9 1.887(7) 3_655 ?
Tc3 O10 1.905(7) . ?
Tc3 O10 1.905(7) 3_655 ?
Tc3 O8 1.656(14) . ?
O16 C17 1.270(14) . ?
O14 H14A 0.8607 . ?
O14 H14B 0.8608 . ?
O15 C17 1.265(14) . ?
O12 H12A 0.9145 . ?
O12 H12B 0.9156 . ?
O11 C19 1.216(14) . ?
O13 C19 1.292(15) . ?
C19 C20 1.492(17) . ?
C17 C18 1.465(16) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?

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
O4 U1 Tc3 88.5(3) . . ?
O4 U1 O9 92.8(3) . . ?
O4 U1 O16 88.3(3) . 3_655 ?
O4 U1 O10 88.5(3) . . ?
O4 U1 O12 88.2(4) . . ?
O4 U1 O11 90.2(4) . . ?
O9 U1 Tc3 32.27(17) . . ?
O9 U1 O16 76.0(3) . 3_655 ?
O9 U1 O10 64.9(2) . . ?
O9 U1 O12 148.1(3) . . ?
O9 U1 O11 139.6(3) . . ?
O16 U1 Tc3 107.8(2) 3_655 . ?
O16 U1 O10 140.5(3) 3_655 . ?
O16 U1 O12 72.2(3) 3_655 . ?
O10 U1 Tc3 32.83(18) . . ?
O10 U1 O12 146.9(3) . . ?
O5 U1 Tc3 92.7(3) . . ?
O5 U1 O4 178.8(4) . . ?
O5 U1 O9 88.3(3) . . ?
O5 U1 O16 91.6(4) . 3_655 ?
O5 U1 O10 92.3(4) . . ?
O5 U1 O12 90.7(4) . . ?
O5 U1 O11 89.2(4) . . ?
O12 U1 Tc3 176.7(2) . . ?
O11 U1 Tc3 107.7(2) . . ?
O11 U1 O16 144.4(3) . 3_655 ?
O11 U1 O10 74.9(3) . . ?
O11 U1 O12 72.2(3) . . ?
O9 U2 Tc3 32.26(18) 3_655 . ?
O9 U2 O14 146.9(3) 3_655 . ?
O9 U2 O13 142.8(3) 3_655 . ?
O6 U2 Tc3 89.1(3) . . ?
O6 U2 O9 88.3(4) . 3_655 ?
O6 U2 O10 91.5(4) . . ?
O6 U2 O14 85.6(4) . . ?
O6 U2 O7 178.8(4) . . ?
O6 U2 O15 92.5(4) . . ?
O6 U2 O13 90.7(4) . . ?
O10 U2 Tc3 32.64(18) . . ?
O10 U2 O9 64.9(3) . 3_655 ?
O10 U2 O14 147.6(3) . . ?
O10 U2 O13 77.9(3) . . ?
O14 U2 Tc3 174.7(2) . . ?
O7 U2 Tc3 92.1(3) . . ?
O7 U2 O9 92.7(4) . 3_655 ?
O7 U2 O10 89.5(3) . . ?
O7 U2 O14 93.2(4) . . ?
O7 U2 O15 87.2(4) . . ?
O7 U2 O13 88.9(4) . . ?
O15 U2 Tc3 109.0(2) . . ?
O15 U2 O9 76.9(3) . 3_655 ?
O15 U2 O10 141.4(3) . . ?
O15 U2 O14 71.0(3) . . ?
O15 U2 O13 140.4(3) . . ?
O13 U2 Tc3 110.5(2) . . ?
O13 U2 O14 69.9(3) . . ?
U1 Tc3 U1 131.35(4) . 3_655 ?
U1 Tc3 U2 79.825(19) . . ?
U1 Tc3 U2 79.046(18) 3_655 . ?
U1 Tc3 U2 79.045(18) . 3_655 ?
U1 Tc3 U2 79.826(19) 3_655 3_655 ?
U2 Tc3 U2 127.14(4) . 3_655 ?
O9 Tc3 U1 41.5(2) . . ?
O9 Tc3 U1 118.0(2) 3_655 . ?
O9 Tc3 U1 118.0(2) . 3_655 ?
O9 Tc3 U1 41.5(2) 3_655 3_655 ?
O9 Tc3 U2 116.4(2) . . ?
O9 Tc3 U2 116.4(2) 3_655 3_655 ?
O9 Tc3 U2 41.5(2) . 3_655 ?
O9 Tc3 U2 41.5(2) 3_655 . ?
O9 Tc3 O9 140.2(5) . 3_655 ?
O9 Tc3 O10 83.4(3) . . ?
O9 Tc3 O10 83.4(3) 3_655 3_655 ?
O9 Tc3 O10 82.9(3) . 3_655 ?
O9 Tc3 O10 82.9(3) 3_655 . ?
O10 Tc3 U1 42.1(2) 3_655 3_655 ?
O10 Tc3 U1 116.9(2) . 3_655 ?
O10 Tc3 U1 42.1(2) . . ?
O10 Tc3 U1 116.9(2) 3_655 . ?
O10 Tc3 U2 115.9(2) . 3_655 ?
O10 Tc3 U2 41.4(2) . . ?
O10 Tc3 U2 41.4(2) 3_655 3_655 ?
O10 Tc3 U2 115.9(2) 3_655 . ?
O10 Tc3 O10 138.8(5) . 3_655 ?
O8 Tc3 U1 114.32(2) . . ?
O8 Tc3 U1 114.32(2) . 3_655 ?
O8 Tc3 U2 116.43(2) . . ?
O8 Tc3 U2 116.43(2) . 3_655 ?
O8 Tc3 O9 109.9(3) . . ?
O8 Tc3 O9 109.9(3) . 3_655 ?
O8 Tc3 O10 110.6(3) . . ?
O8 Tc3 O10 110.6(3) . 3_655 ?
U1 O9 U2 134.5(4) . 3_655 ?
Tc3 O9 U1 106.3(3) . . ?
Tc3 O9 U2 106.2(3) . 3_655 ?
C17 O16 U1 137.2(8) . 3_655 ?
U2 O10 U1 136.5(4) . . ?
Tc3 O10 U1 105.1(3) . . ?
Tc3 O10 U2 106.0(3) . . ?
U2 O14 H14A 109.2 . . ?
U2 O14 H14B 109.4 . . ?
H14A O14 H14B 104.5 . . ?
C17 O15 U2 147.2(8) . . ?
U1 O12 H12A 111.7 . . ?
U1 O12 H12B 112.3 . . ?
H12A O12 H12B 101.9 . . ?
C19 O11 U1 150.7(8) . . ?
C19 O13 U2 139.6(8) . . ?
O11 C19 O13 122.3(11) . . ?
O11 C19 C20 120.0(12) . . ?
O13 C19 C20 117.6(12) . . ?
O16 C17 C18 118.3(11) . . ?
O15 C17 O16 122.7(11) . . ?
O15 C17 C18 119.0(10) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

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
U1 Tc3 O9 U1 121.9(2) 3_655 . . . ?
U1 Tc3 O9 U2 -147.7(6) . . . 3_655 ?
U1 Tc3 O9 U2 -25.7(4) 3_655 . . 3_655 ?
U1 O16 C17 O15 -28(2) 3_655 . . . ?
U1 O16 C17 C18 152.2(9) 3_655 . . . ?
U1 O11 C19 O13 15(3) . . . . ?
U1 O11 C19 C20 -163.1(14) . . . . ?
U2 Tc3 O9 U1 30.6(4) . . . . ?
U2 Tc3 O9 U1 147.7(6) 3_655 . . . ?
U2 Tc3 O9 U2 -117.1(2) . . . 3_655 ?
U2 O15 C17 O16 -13(2) . . . . ?
U2 O15 C17 C18 166.6(12) . . . . ?
U2 O13 C19 O11 -22(2) . . . . ?
U2 O13 C19 C20 157.0(10) . . . . ?
O9 Tc3 O9 U1 75.4(3) 3_655 . . . ?
O9 Tc3 O9 U2 -72.2(3) 3_655 . . 3_655 ?
O10 Tc3 O9 U1 5.0(4) . . . . ?
O10 Tc3 O9 U1 146.0(4) 3_655 . . . ?
O10 Tc3 O9 U2 -1.6(4) 3_655 . . 3_655 ?
O10 Tc3 O9 U2 -142.7(4) . . . 3_655 ?
O8 Tc3 O9 U1 -104.6(3) . . . . ?
O8 Tc3 O9 U2 107.8(3) . . . 3_655 ?

_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
;
_oxdiff_exptl_absorpt_empirical_full_max 3.566
_oxdiff_exptl_absorpt_empirical_full_min 0.405

# start Validation Reply Form
_vrf_PLAT972_utc_3_rod_131414_cu_auto 
;
PROBLEM: Check Calcd Resid. Dens.  0.92Ang From U1             -2.53 eA-3  
RESPONSE: This site is slightly disordered. Also Cu source may create some absorption artifacts that could be related to this negative residual e density. 
;
# end Validation Reply Form
