#------------------------------------------------------------------------------
#$Date: 2024-07-05 16:37:17 +0300 (Fri, 05 Jul 2024) $
#$Revision: 292828 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/30/7133064.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7133064
loop_
_publ_author_name
'Shohel, Mohammad'
'Nyman, May'
_publ_section_title
;
 Uranyl-Tc(VII)/Tc(V) hybrid clusters.
;
_journal_issue                   45
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5820
_journal_page_last               5823
_journal_paper_doi               10.1039/d4cc01726a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C4 H6 O32 Tc2 U5'
_chemical_formula_sum            'C4 H6 O32 Tc2 U5'
_chemical_formula_weight         1952.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-02-11 deposited with the CCDC.	2024-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                93.982(3)
_cell_angle_beta                 99.211(3)
_cell_angle_gamma                109.708(3)
_cell_formula_units_Z            1
_cell_length_a                   7.7451(3)
_cell_length_b                   8.4501(2)
_cell_length_c                   12.7565(5)
_cell_measurement_reflns_used    8377
_cell_measurement_temperature    172.97(10)
_cell_measurement_theta_max      76.8720
_cell_measurement_theta_min      3.5520
_cell_volume                     768.96(5)
_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)'
_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_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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_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_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_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
_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_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0260
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2699
_reflns_number_total             2797
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc01726a2.cif
_cod_data_source_block           utc_10_070812_ms_auto
_cod_depositor_comments
'Adding full bibliography for 7133061--7133065.cif.'
_cod_database_code               7133064
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'U5 Tc2 O32 C4 H20'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.294
_shelx_estimated_absorpt_t_min   0.140
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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)
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 . . . . .
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'
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_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_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) . . . . ?
