#------------------------------------------------------------------------------
#$Date: 2020-06-13 03:55:56 +0300 (Sat, 13 Jun 2020) $
#$Revision: 253137 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/82/1558297.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_1558297
loop_
_publ_author_name
'Cowie, Bradley E.'
'Douair, Iskander'
'Laurent, Maron'
'Love, Jason'
'Arnold, Polly Louise'
_publ_section_title
;
 Selective Oxo Ligand Functionalisation and Substitution Reactivity in an
 Oxo/Catecholate-Bridged UIV/UIV Pacman Complex
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC02297G
_journal_year                    2020
_chemical_formula_moiety         'C74 H62 Cl2 N10 O2 U2'
_chemical_formula_sum            'C74 H62 Cl2 N10 O2 U2'
_chemical_formula_weight         1670.29
_chemical_name_common            'Compound 6.solvent'
_chemical_name_systematic        '[{(py)U(Cl)2U(O2C6H4)(py)}(LA)]'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-02-18 deposited with the CCDC.	2020-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.395(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.0058(3)
_cell_length_b                   21.7361(5)
_cell_length_c                   14.7736(3)
_cell_measurement_reflns_used    11270
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      26.7980
_cell_measurement_theta_min      3.4130
_cell_volume                     4336.17(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_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    -25.00  21.00   1.00   55.00    --  -17.88 -99.00 150.00   46
  2  ω    -87.00   1.00   1.00   55.00    --  -17.88 -37.00  30.00   88
  3  ω    -85.00  -1.00   1.00   55.00    --  -17.88 -57.00   0.00   84
  4  ω    -35.00  49.00   1.00   55.00    --  -17.88  57.00-150.00   84
  5  ω    -48.00  36.00   1.00   55.00    --   19.60 -57.00  60.00   84
  6  ω    -48.00  36.00   1.00   55.00    --   19.60 -57.00-120.00   84
  7  ω    -35.00  32.00   1.00   55.00    --  -17.88  57.00   0.00   67
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            47380
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.857
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.833
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       plate
_exptl_crystal_F_000             1620
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pyridine/hexanes'
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.095
_refine_diff_density_max         1.658
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         9110
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0382
_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)+(0.0369P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0814
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6549
_reflns_number_total             9110
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc02297g2.cif
_cod_data_source_block           compound6
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               1558297
_shelx_shelxl_version_number     2018/3
_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.
;
_exptl_absorpt_special_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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 0.47537(2) 0.34588(2) 0.75403(2) 0.02654(6) Uani 1 1 d . . . . .
Cl1 Cl 0.36273(12) 0.250000 0.80373(11) 0.0277(4) Uani 1 2 d S T P A .
Cl2 Cl 0.44265(13) 0.250000 0.62201(11) 0.0319(4) Uani 1 2 d S T P A .
O1 O 0.6115(2) 0.31165(14) 0.8331(2) 0.0295(8) Uani 1 1 d . . . . .
N4 N 0.4769(3) 0.36813(17) 0.9269(3) 0.0277(9) Uani 1 1 d . . . . .
N2 N 0.3916(3) 0.39732(18) 0.6076(3) 0.0327(10) Uani 1 1 d . . . . .
N1 N 0.5957(3) 0.36815(18) 0.6511(3) 0.0348(10) Uani 1 1 d . . . . .
N5 N 0.538(3) 0.4562(18) 0.804(3) 0.032(3) Uani 0.16(3) 1 d G U P A 1
C63 C 0.636(3) 0.4575(18) 0.857(3) 0.037(2) Uani 0.16(3) 1 d G U P A 1
H63 H 0.667022 0.421458 0.883186 0.045 Uiso 0.16(3) 1 calc R U P A 1
C62 C 0.688(3) 0.513(3) 0.870(3) 0.039(2) Uani 0.16(3) 1 d G U P A 1
H62 H 0.753835 0.513564 0.904589 0.046 Uiso 0.16(3) 1 calc R U P A 1
C61 C 0.642(5) 0.5665(19) 0.830(3) 0.041(2) Uani 0.16(3) 1 d G U P A 1
H61 H 0.676462 0.603448 0.838529 0.050 Uiso 0.16(3) 1 calc R U P A 1
C60 C 0.543(4) 0.5652(17) 0.778(3) 0.0441(19) Uani 0.16(3) 1 d G U P A 1
H60 H 0.512275 0.601227 0.751064 0.053 Uiso 0.16(3) 1 calc R U P A 1
C59 C 0.491(3) 0.510(2) 0.765(3) 0.046(2) Uani 0.16(3) 1 d G U P A 1
H59 H 0.425460 0.509121 0.729660 0.055 Uiso 0.16(3) 1 calc R U P A 1
N3 N 0.3241(3) 0.39810(17) 0.7654(3) 0.0299(9) Uani 1 1 d . . . . .
C57 C 0.7021(5) 0.250000 0.6719(4) 0.0279(16) Uani 1 2 d S T P . .
H57 H 0.633444 0.249999 0.649845 0.034 Uiso 1 2 calc R U P . .
C28 C 0.5518(5) 0.250000 1.0144(4) 0.0251(15) Uani 1 2 d S T P . .
H28 H 0.496366 0.249999 0.963171 0.030 Uiso 1 2 calc R U P . .
C56 C 0.7508(4) 0.3067(2) 0.6876(3) 0.0313(12) Uani 1 1 d . . . . .
C1 C 0.5534(4) 0.3976(2) 0.5742(4) 0.0412(14) Uani 1 1 d . . . . .
H1 H 0.592276 0.409846 0.535252 0.049 Uiso 1 1 calc R U . . .
C15 C 0.3967(4) 0.3946(2) 0.9350(3) 0.0293(11) Uani 1 1 d . . . . .
H15 H 0.391938 0.405137 0.994643 0.035 Uiso 1 1 calc R U . . .
C16 C 0.5551(4) 0.3645(2) 1.0110(3) 0.0291(11) Uani 1 1 d . . . . .
C29 C 0.5913(4) 0.3065(2) 1.0509(3) 0.0275(11) Uani 1 1 d . . . . .
C11 C 0.2365(3) 0.4160(2) 0.7071(3) 0.0303(11) Uani 1 1 d . . . . .
C64 C 0.6953(3) 0.2817(2) 0.8817(3) 0.0288(11) Uani 1 1 d . . . . .
C5 C 0.3007(4) 0.4187(2) 0.5637(3) 0.0353(12) Uani 1 1 d . . . . .
C14 C 0.3164(4) 0.4081(2) 0.8572(3) 0.0314(12) Uani 1 1 d . . . . .
C55 C 0.7016(4) 0.3642(2) 0.6747(3) 0.0314(12) Uani 1 1 d . . . . .
C17 C 0.5983(4) 0.4178(2) 1.0526(3) 0.0382(13) Uani 1 1 d . . . . .
H17 H 0.575851 0.455459 1.025079 0.046 Uiso 1 1 calc R U . . .
C7 C 0.1767(4) 0.3404(3) 0.5789(4) 0.0426(13) Uani 1 1 d . . . . .
H7AA H 0.154388 0.336617 0.511121 0.051 Uiso 0.468(11) 1 calc R U P B 1
H7AB H 0.233955 0.313894 0.600066 0.051 Uiso 0.468(11) 1 calc R U P B 1
H7BC H 0.227626 0.312949 0.614233 0.051 Uiso 0.532(11) 1 calc R U P B 2
H7BD H 0.117633 0.333687 0.600061 0.051 Uiso 0.532(11) 1 calc R U P B 2
C2 C 0.4513(4) 0.4118(2) 0.5469(3) 0.0378(13) Uani 1 1 d . . . . .
C6 C 0.2124(4) 0.4091(2) 0.6025(3) 0.0368(12) Uani 1 1 d . . . . .
C21 C 0.7091(5) 0.250000 1.1743(4) 0.0386(19) Uani 1 2 d S T P . .
H21 H 0.760175 0.250000 1.229413 0.046 Uiso 1 2 calc R U P . .
C54 C 0.7549(4) 0.4174(3) 0.6864(4) 0.0412(13) Uani 1 1 d . . . . .
H54 H 0.721849 0.454893 0.677174 0.049 Uiso 1 1 calc R U . . .
C13 C 0.2237(4) 0.4319(2) 0.8547(4) 0.0386(13) Uani 1 1 d . . . . .
H13 H 0.199917 0.442343 0.905712 0.046 Uiso 1 1 calc R U . . .
C65 C 0.7791(4) 0.3133(3) 0.9297(4) 0.0410(13) Uani 1 1 d . . . . .
H65 H 0.778713 0.356098 0.930627 0.049 Uiso 1 1 calc R U . . .
C18 C 0.6755(4) 0.4167(3) 1.1357(4) 0.0476(15) Uani 1 1 d . . . . .
H18 H 0.701943 0.453514 1.163471 0.057 Uiso 1 1 calc R U . . .
C12 C 0.1737(4) 0.4368(2) 0.7599(4) 0.0386(13) Uani 1 1 d . . . . .
H12 H 0.109515 0.451448 0.735978 0.046 Uiso 1 1 calc R U . . .
C20 C 0.6724(4) 0.3057(2) 1.1348(3) 0.0324(12) Uani 1 1 d . . . . .
C51 C 0.8568(4) 0.3063(2) 0.7139(3) 0.0351(12) Uani 1 1 d . . . . .
C19 C 0.7116(4) 0.3627(2) 1.1756(3) 0.0399(14) Uani 1 1 d . . . . .
H19 H 0.762833 0.362770 1.230545 0.048 Uiso 1 1 calc R U . . .
C9 C 0.1288(4) 0.4540(3) 0.5553(4) 0.0561(17) Uani 1 1 d . . . . .
H9A H 0.111753 0.447107 0.488006 0.067 Uiso 1 1 calc R U . . .
H9B H 0.070761 0.444273 0.576619 0.067 Uiso 1 1 calc R U . . .
C66 C 0.8632(4) 0.2817(2) 0.9762(4) 0.0448(14) Uani 1 1 d . . . . .
H66 H 0.919877 0.303075 1.007451 0.054 Uiso 1 1 calc R U . . .
C50 C 0.9073(6) 0.250000 0.7263(5) 0.0404(19) Uani 1 2 d S T P . .
H50 H 0.976186 0.250001 0.743251 0.048 Uiso 1 2 calc R U P . .
C52 C 0.9085(4) 0.3634(3) 0.7260(4) 0.0459(15) Uani 1 1 d . . . . .
H52 H 0.977327 0.363544 0.743803 0.055 Uiso 1 1 calc R U . . .
C4 C 0.3017(4) 0.4450(3) 0.4773(4) 0.0521(17) Uani 1 1 d . . . . .
H4 H 0.247821 0.461929 0.433530 0.063 Uiso 1 1 calc R U . . .
C10 C 0.1524(5) 0.5221(3) 0.5736(5) 0.074(2) Uani 1 1 d . . . . .
H10A H 0.177746 0.528820 0.639889 0.111 Uiso 1 1 calc R U . . .
H10B H 0.093239 0.545900 0.550339 0.111 Uiso 1 1 calc R U . . .
H10C H 0.201137 0.534408 0.542165 0.111 Uiso 1 1 calc R U . . .
C53 C 0.8599(4) 0.4166(3) 0.7123(4) 0.0495(15) Uani 1 1 d . . . . .
H53 H 0.894956 0.453391 0.719703 0.059 Uiso 1 1 calc R U . . .
C3 C 0.3956(4) 0.4412(3) 0.4692(4) 0.0553(18) Uani 1 1 d . . . . .
H3 H 0.418064 0.456024 0.419538 0.066 Uiso 1 1 calc R U . . .
C8 C 0.0973(8) 0.3162(5) 0.6181(9) 0.048(4) Uani 0.468(11) 1 d . . P B 1
H8A H 0.120970 0.314006 0.685297 0.071 Uiso 0.468(11) 1 calc R U P B 1
H8B H 0.078639 0.275806 0.593377 0.071 Uiso 0.468(11) 1 calc R U P B 1
H8C H 0.040906 0.342987 0.601220 0.071 Uiso 0.468(11) 1 calc R U P B 1
C8A C 0.1550(11) 0.3241(6) 0.4799(8) 0.083(5) Uani 0.532(11) 1 d . . P B 2
H8AA H 0.104714 0.351084 0.443957 0.125 Uiso 0.532(11) 1 calc R U P B 2
H8AB H 0.131928 0.282388 0.471447 0.125 Uiso 0.532(11) 1 calc R U P B 2
H8AC H 0.213942 0.328182 0.458902 0.125 Uiso 0.532(11) 1 calc R U P B 2
N5A N 0.5369(6) 0.4576(4) 0.7830(8) 0.0322(17) Uani 0.84(3) 1 d . U P A 2
C63A C 0.6263(7) 0.4706(5) 0.8368(7) 0.0351(17) Uani 0.84(3) 1 d . U P A 2
H63A H 0.665547 0.438035 0.866244 0.042 Uiso 0.84(3) 1 calc R U P A 2
C62A C 0.6652(8) 0.5293(5) 0.8522(7) 0.0394(17) Uani 0.84(3) 1 d . U P A 2
H62A H 0.729059 0.535946 0.889790 0.047 Uiso 0.84(3) 1 calc R U P A 2
C61A C 0.6068(11) 0.5773(4) 0.8104(8) 0.0425(17) Uani 0.84(3) 1 d . U P A 2
H61A H 0.630898 0.617399 0.818074 0.051 Uiso 0.84(3) 1 calc R U P A 2
C60A C 0.5140(10) 0.5659(4) 0.7579(8) 0.0473(16) Uani 0.84(3) 1 d . U P A 2
H60A H 0.473353 0.598605 0.731084 0.057 Uiso 0.84(3) 1 calc R U P A 2
C59A C 0.4788(7) 0.5076(5) 0.7437(8) 0.0456(16) Uani 0.84(3) 1 d . U P A 2
H59A H 0.414685 0.500989 0.706841 0.055 Uiso 0.84(3) 1 calc R U P A 2
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 N2 144.16(13) . . ?
O1 U1 N3 143.54(12) . . ?
N2 U1 N3 68.10(13) . . ?
O1 U1 N5A 91.6(2) . . ?
N2 U1 N5A 77.1(3) . . ?
N3 U1 N5A 79.0(2) . . ?
O1 U1 N5 88.9(10) . . ?
N2 U1 N5 82.9(9) . . ?
N3 U1 N5 77.5(12) . . ?
O1 U1 N4 75.42(12) . . ?
N2 U1 N4 131.57(13) . . ?
N3 U1 N4 68.12(12) . . ?
N5A U1 N4 75.2(3) . . ?
N5 U1 N4 68.3(11) . . ?
O1 U1 N1 75.88(12) . . ?
N2 U1 N1 68.28(13) . . ?
N3 U1 N1 131.41(12) . . ?
N5A U1 N1 71.4(2) . . ?
N5 U1 N1 76.9(13) . . ?
N4 U1 N1 134.79(13) . . ?
O1 U1 Cl2 94.61(9) . . ?
N2 U1 Cl2 76.88(9) . . ?
N3 U1 Cl2 114.02(10) . . ?
N5A U1 Cl2 143.3(2) . . ?
N5 U1 Cl2 150.0(12) . . ?
N4 U1 Cl2 141.22(9) . . ?
N1 U1 Cl2 75.12(9) . . ?
O1 U1 Cl1 94.68(9) . . ?
N2 U1 Cl1 113.44(10) . . ?
N3 U1 Cl1 76.78(9) . . ?
N5A U1 Cl1 146.9(2) . . ?
N5 U1 Cl1 140.9(12) . . ?
N4 U1 Cl1 74.99(9) . . ?
N1 U1 Cl1 141.55(9) . . ?
Cl2 U1 Cl1 68.51(4) . . ?
U1 Cl1 U1 95.03(5) . 4_565 ?
U1 Cl2 U1 95.86(5) 4_565 . ?
C64 O1 U1 172.4(3) . . ?
C15 N4 C16 115.4(4) . . ?
C15 N4 U1 113.1(3) . . ?
C16 N4 U1 130.7(3) . . ?
C5 N2 C2 105.0(4) . . ?
C5 N2 U1 139.0(3) . . ?
C2 N2 U1 116.0(3) . . ?
C1 N1 C55 116.4(4) . . ?
C1 N1 U1 112.8(3) . . ?
C55 N1 U1 129.5(3) . . ?
C63 N5 C59 120.0 . . ?
C63 N5 U1 113(2) . . ?
C59 N5 U1 125(2) . . ?
N5 C63 C62 120.0 . . ?
N5 C63 H63 120.0 . . ?
C62 C63 H63 120.0 . . ?
C61 C62 C63 120.0 . . ?
C61 C62 H62 120.0 . . ?
C63 C62 H62 120.0 . . ?
C62 C61 C60 120.0 . . ?
C62 C61 H61 120.0 . . ?
C60 C61 H61 120.0 . . ?
C61 C60 C59 120.0 . . ?
C61 C60 H60 120.0 . . ?
C59 C60 H60 120.0 . . ?
C60 C59 N5 120.0 . . ?
C60 C59 H59 120.0 . . ?
N5 C59 H59 120.0 . . ?
C11 N3 C14 106.2(4) . . ?
C11 N3 U1 138.1(3) . . ?
C14 N3 U1 115.3(3) . . ?
C56 C57 C56 123.7(6) . 4_565 ?
C56 C57 H57 118.2 . . ?
C56 C57 H57 118.2 4_565 . ?
C29 C28 C29 123.4(6) 4_565 . ?
C29 C28 H28 118.3 4_565 . ?
C29 C28 H28 118.3 . . ?
C57 C56 C55 123.9(5) . . ?
C57 C56 C51 117.7(5) . . ?
C55 C56 C51 118.3(5) . . ?
N1 C1 C2 123.2(5) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
N4 C15 C14 122.8(4) . . ?
N4 C15 H15 118.6 . . ?
C14 C15 H15 118.6 . . ?
C17 C16 N4 119.2(4) . . ?
C17 C16 C29 119.6(4) . . ?
N4 C16 C29 121.2(4) . . ?
C28 C29 C16 123.8(4) . . ?
C28 C29 C20 117.6(5) . . ?
C16 C29 C20 118.6(4) . . ?
N3 C11 C12 109.7(4) . . ?
N3 C11 C6 122.9(4) . . ?
C12 C11 C6 127.3(5) . . ?
O1 C64 C64 118.4(2) . 4_565 ?
O1 C64 C65 121.7(4) . . ?
C64 C64 C65 119.8(3) 4_565 . ?
N2 C5 C4 110.0(5) . . ?
N2 C5 C6 122.3(4) . . ?
C4 C5 C6 127.6(5) . . ?
C13 C14 N3 110.0(4) . . ?
C13 C14 C15 129.7(5) . . ?
N3 C14 C15 120.3(4) . . ?
C54 C55 C56 120.1(5) . . ?
C54 C55 N1 118.5(5) . . ?
C56 C55 N1 121.4(4) . . ?
C16 C17 C18 121.4(5) . . ?
C16 C17 H17 119.3 . . ?
C18 C17 H17 119.3 . . ?
C8A C7 C6 114.8(7) . . ?
C8 C7 C6 118.4(6) . . ?
C8 C7 H7AA 107.7 . . ?
C6 C7 H7AA 107.7 . . ?
C8 C7 H7AB 107.7 . . ?
C6 C7 H7AB 107.7 . . ?
H7AA C7 H7AB 107.1 . . ?
C8A C7 H7BC 108.6 . . ?
C6 C7 H7BC 108.6 . . ?
C8A C7 H7BD 108.6 . . ?
C6 C7 H7BD 108.6 . . ?
H7BC C7 H7BD 107.5 . . ?
C3 C2 C1 130.7(5) . . ?
C3 C2 N2 109.6(5) . . ?
C1 C2 N2 119.6(4) . . ?
C11 C6 C5 113.3(4) . . ?
C11 C6 C9 109.8(4) . . ?
C5 C6 C9 110.0(4) . . ?
C11 C6 C7 107.0(4) . . ?
C5 C6 C7 106.8(4) . . ?
C9 C6 C7 109.9(4) . . ?
C20 C21 C20 122.3(6) . 4_565 ?
C20 C21 H21 118.8 . . ?
C20 C21 H21 118.8 4_565 . ?
C55 C54 C53 121.2(5) . . ?
C55 C54 H54 119.4 . . ?
C53 C54 H54 119.4 . . ?
C14 C13 C12 105.9(5) . . ?
C14 C13 H13 127.1 . . ?
C12 C13 H13 127.1 . . ?
C66 C65 C64 120.3(5) . . ?
C66 C65 H65 119.9 . . ?
C64 C65 H65 119.9 . . ?
C19 C18 C17 120.6(5) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C13 C12 C11 108.2(5) . . ?
C13 C12 H12 125.9 . . ?
C11 C12 H12 125.9 . . ?
C21 C20 C19 121.7(5) . . ?
C21 C20 C29 119.5(5) . . ?
C19 C20 C29 118.7(5) . . ?
C50 C51 C52 121.5(5) . . ?
C50 C51 C56 119.5(5) . . ?
C52 C51 C56 119.0(5) . . ?
C18 C19 C20 121.0(5) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 H19 119.5 . . ?
C10 C9 C6 115.5(5) . . ?
C10 C9 H9A 108.4 . . ?
C6 C9 H9A 108.4 . . ?
C10 C9 H9B 108.4 . . ?
C6 C9 H9B 108.4 . . ?
H9A C9 H9B 107.5 . . ?
C66 C66 C65 119.9(3) 4_565 . ?
C66 C66 H66 120.0 4_565 . ?
C65 C66 H66 120.0 . . ?
C51 C50 C51 121.7(7) . 4_565 ?
C51 C50 H50 119.1 . . ?
C51 C50 H50 119.1 4_565 . ?
C53 C52 C51 121.1(5) . . ?
C53 C52 H52 119.5 . . ?
C51 C52 H52 119.5 . . ?
C3 C4 C5 107.5(5) . . ?
C3 C4 H4 126.2 . . ?
C5 C4 H4 126.2 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C52 C53 C54 120.3(6) . . ?
C52 C53 H53 119.9 . . ?
C54 C53 H53 119.9 . . ?
C4 C3 C2 107.8(5) . . ?
C4 C3 H3 126.1 . . ?
C2 C3 H3 126.1 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C8A H8AA 109.5 . . ?
C7 C8A H8AB 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
C7 C8A H8AC 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C63A N5A C59A 116.1(6) . . ?
C63A N5A U1 121.5(5) . . ?
C59A N5A U1 122.4(5) . . ?
N5A C63A C62A 124.4(6) . . ?
N5A C63A H63A 117.8 . . ?
C62A C63A H63A 117.8 . . ?
C61A C62A C63A 117.9(6) . . ?
C61A C62A H62A 121.1 . . ?
C63A C62A H62A 121.1 . . ?
C60A C61A C62A 119.3(7) . . ?
C60A C61A H61A 120.4 . . ?
C62A C61A H61A 120.4 . . ?
C61A C60A C59A 121.0(7) . . ?
C61A C60A H60A 119.5 . . ?
C59A C60A H60A 119.5 . . ?
C60A C59A N5A 121.3(7) . . ?
C60A C59A H59A 119.4 . . ?
N5A C59A H59A 119.4 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.091(3) . ?
U1 N2 2.441(4) . ?
U1 N3 2.448(4) . ?
U1 N5A 2.574(7) . ?
U1 N5 2.59(4) . ?
U1 N4 2.594(4) . ?
U1 N1 2.598(4) . ?
U1 Cl2 2.8077(10) . ?
U1 Cl1 2.8260(11) . ?
O1 C64 1.367(5) . ?
N4 C15 1.296(6) . ?
N4 C16 1.424(6) . ?
N2 C5 1.349(6) . ?
N2 C2 1.414(6) . ?
N1 C1 1.301(6) . ?
N1 C55 1.433(6) . ?
N5 C63 1.3900 . ?
N5 C59 1.3900 . ?
C63 C62 1.3900 . ?
C63 H63 0.9300 . ?
C62 C61 1.3900 . ?
C62 H62 0.9300 . ?
C61 C60 1.3900 . ?
C61 H61 0.9300 . ?
C60 C59 1.3900 . ?
C60 H60 0.9300 . ?
C59 H59 0.9300 . ?
N3 C11 1.356(6) . ?
N3 C14 1.407(6) . ?
C57 C56 1.398(6) . ?
C57 C56 1.398(6) 4_565 ?
C57 H57 0.9300 . ?
C28 C29 1.395(5) 4_565 ?
C28 C29 1.395(5) . ?
C28 H28 0.9300 . ?
C56 C55 1.415(7) . ?
C56 C51 1.431(6) . ?
C1 C2 1.414(7) . ?
C1 H1 0.9300 . ?
C15 C14 1.409(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.375(6) . ?
C16 C29 1.426(6) . ?
C29 C20 1.442(6) . ?
C11 C12 1.397(7) . ?
C11 C6 1.500(7) . ?
C64 C64 1.378(9) 4_565 ?
C64 C65 1.382(6) . ?
C5 C4 1.402(7) . ?
C5 C6 1.509(7) . ?
C14 C13 1.388(7) . ?
C55 C54 1.362(7) . ?
C17 C18 1.404(7) . ?
C17 H17 0.9300 . ?
C7 C8A 1.457(12) . ?
C7 C8 1.481(11) . ?
C7 C6 1.584(7) . ?
C7 H7AA 0.9700 . ?
C7 H7AB 0.9700 . ?
C7 H7BC 0.9700 . ?
C7 H7BD 0.9700 . ?
C2 C3 1.363(7) . ?
C6 C9 1.542(7) . ?
C21 C20 1.383(6) . ?
C21 C20 1.383(6) 4_565 ?
C21 H21 0.9300 . ?
C54 C53 1.418(7) . ?
C54 H54 0.9300 . ?
C13 C12 1.393(7) . ?
C13 H13 0.9300 . ?
C65 C66 1.381(7) . ?
C65 H65 0.9300 . ?
C18 C19 1.351(7) . ?
C18 H18 0.9300 . ?
C12 H12 0.9300 . ?
C20 C19 1.422(6) . ?
C51 C50 1.401(6) . ?
C51 C52 1.425(7) . ?
C19 H19 0.9300 . ?
C9 C10 1.524(8) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C66 C66 1.376(10) 4_565 ?
C66 H66 0.9300 . ?
C50 H50 0.9300 . ?
C52 C53 1.328(7) . ?
C52 H52 0.9300 . ?
C4 C3 1.353(7) . ?
C4 H4 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C53 H53 0.9300 . ?
C3 H3 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C8A H8AA 0.9600 . ?
C8A H8AB 0.9600 . ?
C8A H8AC 0.9600 . ?
N5A C63A 1.323(7) . ?
N5A C59A 1.389(8) . ?
C63A C62A 1.383(8) . ?
C63A H63A 0.9300 . ?
C62A C61A 1.368(9) . ?
C62A H62A 0.9300 . ?
C61A C60A 1.349(9) . ?
C61A H61A 0.9300 . ?
C60A C59A 1.356(10) . ?
C60A H60A 0.9300 . ?
C59A H59A 0.9300 . ?
