#------------------------------------------------------------------------------
#$Date: 2024-07-05 16:37:17 +0300 (Fri, 05 Jul 2024) $
#$Revision: 292828 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/30/7133061.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_7133061
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 Na O14 Re U2'
_chemical_formula_sum            'C4 H6 Na O14 Re U2'
_chemical_formula_weight         963.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-14
_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                90
_cell_angle_beta                 113.798(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2417(5)
_cell_length_b                   8.1267(2)
_cell_length_c                   15.0583(5)
_cell_measurement_reflns_used    6401
_cell_measurement_temperature    223.00(10)
_cell_measurement_theta_max      77.1190
_cell_measurement_theta_min      3.2010
_cell_volume                     1706.60(10)
_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)'
_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_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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_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_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_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
_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_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0698
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1546
_reflns_number_total             1669
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc01726a2.cif
_cod_data_source_block           ui_36_thinplate150816_auto
_cod_depositor_comments
'Adding full bibliography for 7133061--7133065.cif.'
_cod_database_code               7133061
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'U Re2 O12'
_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   0.553
_shelx_estimated_absorpt_t_min   0.174
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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)
;
_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_
_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'
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 . .
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'
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_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_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 ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.514(6)
2 0.486(6)
