# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_rf76b
_database_code_depnum_ccdc_archive 'CCDC 1842376'

_audit_update_record             
;
2018-05-09 deposited with the CCDC.
2018-08-01 downloaded from the CCDC.
;
# publcif _publ_body_element loop end

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H28 N4 O5 U, C5 H5 N'
_chemical_formula_sum            'C32 H33 N5 O5 U'
_chemical_formula_weight         805.66

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'
N N 0.0311 0.0180 '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'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3182(3)
_cell_length_b                   12.47104(19)
_cell_length_c                   12.8143(3)
_cell_angle_alpha                82.2874(17)
_cell_angle_beta                 68.197(3)
_cell_angle_gamma                79.3609(17)
_cell_volume                     1500.76(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100.01(10)
_cell_measurement_reflns_used    9156
_cell_measurement_theta_min      4.6560
_cell_measurement_theta_max      75.7620

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear intense orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_F_000             784
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.121
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -8 0 0.1712
-3 4 3 0.1261
-3 4 -6 0.1091
-3 0 -8 0.0947
3 3 -5 0.0891
2 -5 -4 0.1324
-4 5 0 0.1303
-4 -4 -8 0.1280
-6 -2 0 0.1080
6 0 -1 0.0410
1 7 -3 0.1449
-6 -3 -4 0.1308
2 0 8 0.0532
7 0 4 0.0242
-6 -2 -5 0.0972
-6 1 -5 0.0952
1 8 1 0.1426
-7 0 -3 0.0951
2 8 2 0.1404
2 -4 6 0.1143
-1 -8 -1 0.1748
-6 1 0 0.1008
-1 -1 7 0.0765
0 8 1 0.1408
1 0 -7 0.0892
_exptl_absorpt_coefficient_mu    15.630
_shelx_estimated_absorpt_T_min   0.082
_shelx_estimated_absorpt_T_max   0.254
_exptl_absorpt_correction_T_min  0.074
_exptl_absorpt_correction_T_max  0.406
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      100.01(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_detector_area_resol_mean 5.2817
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -65.00  31.00   1.00    5.00    --  -40.91  57.00 -30.00   96
  2  ω    -96.00  -2.00   1.00    5.00    --  -40.91 125.00   0.00   94
  3  ω   -108.00 -19.00   1.00    5.00    --  -40.91 -38.00  90.00   89
  4  ω     53.00  97.00   1.00    5.00    --   40.91-125.00-180.00   44
  5  ω     54.00 107.00   1.00   15.00    --  111.85 -94.00-120.00   53
  6  ω     90.00 116.00   1.00   15.00    --  111.85-125.00-120.00   26
  7  ω     36.00 135.00   1.00   15.00    --  111.85 -30.00  30.00   99
  8  ω     91.00 175.00   1.00   15.00    --  111.85  45.00  60.00   84
  9  ω    108.00 140.00   1.00   15.00    --  111.85 -61.00 150.00   32
 10  ω     97.00 122.00   1.00   15.00    --  111.85-125.00  60.00   25
 11  ω     49.00  76.00   1.00   15.00    --  111.85-125.00  60.00   27
 12  ω     49.00 108.00   1.00   15.00    --  111.85 -94.00  90.00   59
 13  ω     49.00 124.00   1.00   15.00    --  111.85 -30.00 120.00   75
 14  ω     42.00 114.00   1.00   15.00    --  111.85 -61.00 120.00   72
 15  ω     36.00 141.00   1.00   15.00    --  111.85 -77.00 -60.00  105
 16  ω     30.00 149.00   1.00   15.00    --  111.85 -15.00-120.00  119
 17  ω   -112.00 -23.00   1.00    5.00    --  -40.91 -38.00-180.00   89
;
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            10197
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.616
_diffrn_reflns_theta_max         75.995
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6064
_reflns_number_gt                6044
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 3.10 (CCDC, 2017)'
_computing_publication_material  'CIFTAb (Sheldrick, 2015)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0425P)²+3.0872P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00075(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6064
_refine_ls_number_parameters     390
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0256
_refine_ls_wR_factor_ref         0.0674
_refine_ls_wR_factor_gt          0.0673
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_restrained_S_all      1.148
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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 0.42024(2) 0.26736(2) 0.44456(2) 0.01296(6) Uani 1 1 d . . . . .
O1 O 0.5178(3) 0.3871(2) 0.3052(2) 0.0210(6) Uani 1 1 d . . . . .
O2 O 0.3036(3) 0.2408(2) 0.3358(2) 0.0189(5) Uani 1 1 d . . . . .
O3 O 0.2865(3) 0.3727(2) 0.5157(2) 0.0197(6) Uani 1 1 d . . . . .
O4 O 0.5553(3) 0.1560(2) 0.3887(2) 0.0185(6) Uani 1 1 d . . . . .
O5 O 0.4599(3) 0.2164(3) 0.9880(3) 0.0272(6) Uani 1 1 d . . . . .
H5 H 0.454749 0.182966 0.937220 0.041 Uiso 1 1 calc R U . . .
N1 N 0.6057(4) 0.3470(3) 0.4901(3) 0.0189(7) Uani 1 1 d . . . . .
N2 N 0.4309(3) 0.1949(3) 0.6437(3) 0.0151(6) Uani 1 1 d . . . . .
N3 N 0.2336(3) 0.1397(3) 0.5555(3) 0.0179(6) Uani 1 1 d . . . . .
N4 N 0.5432(4) 0.0768(3) 0.8322(3) 0.0221(7) Uani 1 1 d . . . . .
C1 C 0.6313(4) 0.4342(3) 0.2532(3) 0.0177(8) Uani 1 1 d . . . . .
C2 C 0.6557(4) 0.4863(4) 0.1453(4) 0.0230(8) Uani 1 1 d . . . . .
H2 H 0.589359 0.487516 0.109786 0.028 Uiso 1 1 calc R U . . .
C3 C 0.7744(5) 0.5361(4) 0.0895(4) 0.0288(10) Uani 1 1 d . . . . .
H3 H 0.788522 0.571259 0.016392 0.035 Uiso 1 1 calc R U . . .
C4 C 0.8739(5) 0.5352(4) 0.1397(4) 0.0297(10) Uani 1 1 d . . . . .
H4 H 0.957017 0.567348 0.100240 0.036 Uiso 1 1 calc R U . . .
C5 C 0.8501(4) 0.4872(4) 0.2471(4) 0.0237(8) Uani 1 1 d . . . . .
H5A H 0.915900 0.488783 0.282461 0.028 Uiso 1 1 calc R U . . .
C6 C 0.7300(4) 0.4357(3) 0.3057(4) 0.0182(8) Uani 1 1 d . . . . .
C7 C 0.7061(4) 0.3955(3) 0.4222(4) 0.0201(8) Uani 1 1 d . . . . .
H7 H 0.774264 0.406902 0.451450 0.024 Uiso 1 1 calc R U . . .
C8 C 0.6039(5) 0.3249(4) 0.6068(4) 0.0226(8) Uani 1 1 d . . . . .
H8A H 0.616626 0.391981 0.633105 0.027 Uiso 1 1 calc R U . . .
H8B H 0.683465 0.267324 0.608452 0.027 Uiso 1 1 calc R U . . .
C9 C 0.4655(5) 0.2878(3) 0.6860(4) 0.0222(8) Uani 1 1 d . . . . .
H9A H 0.472064 0.265112 0.761113 0.027 Uiso 1 1 calc R U . . .
H9B H 0.388216 0.350072 0.694698 0.027 Uiso 1 1 calc R U . . .
C10 C 0.2848(4) 0.1769(4) 0.7168(4) 0.0220(8) Uani 1 1 d . . . . .
H10A H 0.220680 0.247285 0.723411 0.026 Uiso 1 1 calc R U . . .
H10B H 0.283200 0.148710 0.793247 0.026 Uiso 1 1 calc R U . . .
C11 C 0.2337(4) 0.0953(4) 0.6677(4) 0.0211(8) Uani 1 1 d . . . . .
H11A H 0.296754 0.024414 0.661728 0.025 Uiso 1 1 calc R U . . .
H11B H 0.137198 0.082975 0.717504 0.025 Uiso 1 1 calc R U . . .
C12 C 0.1243(4) 0.1279(3) 0.5348(4) 0.0188(8) Uani 1 1 d . . . . .
H12 H 0.055256 0.092128 0.593579 0.023 Uiso 1 1 calc R U . . .
C13 C 0.0935(4) 0.1627(3) 0.4326(3) 0.0175(7) Uani 1 1 d . . . . .
C14 C -0.0342(4) 0.1393(3) 0.4303(4) 0.0222(8) Uani 1 1 d . . . . .
H14 H -0.096135 0.104263 0.495278 0.027 Uiso 1 1 calc R U . . .
C15 C -0.0712(4) 0.1660(4) 0.3361(4) 0.0251(9) Uani 1 1 d . . . . .
H15 H -0.157781 0.150212 0.336069 0.030 Uiso 1 1 calc R U . . .
C16 C 0.0212(5) 0.2169(4) 0.2404(4) 0.0228(8) Uani 1 1 d . . . . .
H16 H -0.002734 0.235197 0.174722 0.027 Uiso 1 1 calc R U . . .
C17 C 0.1466(4) 0.2409(3) 0.2404(4) 0.0204(8) Uani 1 1 d . . . . .
H17 H 0.208431 0.274548 0.174333 0.024 Uiso 1 1 calc R U . . .
C18 C 0.1842(4) 0.2164(3) 0.3361(3) 0.0178(7) Uani 1 1 d . . . . .
C19 C 0.5342(5) 0.0923(4) 0.6378(4) 0.0217(8) Uani 1 1 d . . . . .
H19A H 0.630211 0.112957 0.604134 0.026 Uiso 1 1 calc R U . . .
H19B H 0.524689 0.046118 0.584675 0.026 Uiso 1 1 calc R U . . .
C20 C 0.5255(5) 0.0217(4) 0.7459(4) 0.0235(8) Uani 1 1 d . . . . .
H20A H 0.432633 -0.004432 0.777448 0.028 Uiso 1 1 calc R U . . .
H20B H 0.599010 -0.043291 0.727230 0.028 Uiso 1 1 calc R U . . .
C21 C 0.6469(5) 0.0368(4) 0.8649(4) 0.0229(8) Uani 1 1 d . . . . .
H21 H 0.709681 -0.025035 0.830593 0.028 Uiso 1 1 calc R U . . .
C22 C 0.6707(4) 0.0838(4) 0.9530(4) 0.0221(8) Uani 1 1 d . . . . .
C23 C 0.7904(5) 0.0413(4) 0.9812(4) 0.0266(9) Uani 1 1 d . . . . .
H23 H 0.853510 -0.018868 0.943702 0.032 Uiso 1 1 calc R U . . .
C24 C 0.8177(5) 0.0858(4) 1.0627(4) 0.0273(9) Uani 1 1 d . . . . .
H24 H 0.898412 0.055727 1.081591 0.033 Uiso 1 1 calc R U . . .
C25 C 0.7265(5) 0.1746(4) 1.1170(4) 0.0259(9) Uani 1 1 d . . . . .
H25 H 0.746973 0.206703 1.171253 0.031 Uiso 1 1 calc R U . . .
C26 C 0.6062(5) 0.2168(4) 1.0928(3) 0.0228(8) Uani 1 1 d . . . . .
H26 H 0.542793 0.275873 1.132246 0.027 Uiso 1 1 calc R U . . .
C27 C 0.5780(4) 0.1726(3) 1.0102(3) 0.0206(8) Uani 1 1 d . . . . .
N5 N 0.0588(4) 0.7106(3) 0.2799(4) 0.0313(9) Uani 1 1 d . . . . .
C28 C 0.0568(5) 0.6309(4) 0.3614(4) 0.0248(9) Uani 1 1 d . . . . .
H28 H -0.008737 0.643541 0.435222 0.030 Uiso 1 1 calc R U . . .
C29 C 0.1433(4) 0.5318(4) 0.3453(4) 0.0233(8) Uani 1 1 d . . . . .
H29 H 0.137018 0.478034 0.406253 0.028 Uiso 1 1 calc R U . . .
C30 C 0.2402(5) 0.5119(4) 0.2378(4) 0.0287(9) Uani 1 1 d . . . . .
H30 H 0.301531 0.444353 0.223639 0.034 Uiso 1 1 calc R U . . .
C31 C 0.2449(5) 0.5920(4) 0.1532(4) 0.0303(10) Uani 1 1 d . . . . .
H31 H 0.310712 0.581727 0.078982 0.036 Uiso 1 1 calc R U . . .
C32 C 0.1518(5) 0.6889(4) 0.1775(4) 0.0324(10) Uani 1 1 d . . . . .
H32 H 0.154499 0.743094 0.117450 0.039 Uiso 1 1 calc R U . . .


_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 O3 1.783(3) . ?
U1 O4 1.787(3) . ?
U1 O1 2.222(3) . ?
U1 O2 2.240(3) . ?
U1 N1 2.584(3) . ?
U1 N3 2.599(3) . ?
U1 N2 2.625(3) . ?
O1 C1 1.316(5) . ?
O2 C18 1.321(5) . ?
O5 C27 1.355(5) . ?
O5 H5 0.8400 . ?
N1 C7 1.271(6) . ?
N1 C8 1.479(5) . ?
N2 C10 1.490(5) . ?
N2 C9 1.493(5) . ?
N2 C19 1.497(5) . ?
N3 C12 1.288(5) . ?
N3 C11 1.469(5) . ?
N4 C21 1.284(6) . ?
N4 C20 1.459(5) . ?
C1 C2 1.399(6) . ?
C1 C6 1.417(6) . ?
C2 C3 1.381(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.398(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.377(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.409(6) . ?
C5 H5A 0.9500 . ?
C6 C7 1.454(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.525(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.526(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.452(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.413(6) . ?
C13 C18 1.416(6) . ?
C14 C15 1.379(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.400(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.382(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.398(6) . ?
C17 H17 0.9500 . ?
C19 C20 1.520(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.455(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.406(6) . ?
C22 C27 1.409(6) . ?
C23 C24 1.381(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.391(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.384(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.397(6) . ?
C26 H26 0.9500 . ?
N5 C32 1.334(6) . ?
N5 C28 1.339(6) . ?
C28 C29 1.375(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.391(7) . ?
C29 H29 0.9500 . ?
C30 C31 1.365(7) . ?
C30 H30 0.9500 . ?
C31 C32 1.389(7) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?

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
O3 U1 O4 173.47(12) . . ?
O3 U1 O1 90.94(13) . . ?
O4 U1 O1 93.89(12) . . ?
O3 U1 O2 93.31(12) . . ?
O4 U1 O2 91.51(12) . . ?
O1 U1 O2 84.62(10) . . ?
O3 U1 N1 90.24(12) . . ?
O4 U1 N1 87.23(12) . . ?
O1 U1 N1 70.58(11) . . ?
O2 U1 N1 155.00(11) . . ?
O3 U1 N3 84.13(12) . . ?
O4 U1 N3 93.34(12) . . ?
O1 U1 N3 154.37(10) . . ?
O2 U1 N3 70.64(10) . . ?
N1 U1 N3 134.36(11) . . ?
O3 U1 N2 86.20(12) . . ?
O4 U1 N2 87.27(11) . . ?
O1 U1 N2 137.85(10) . . ?
O2 U1 N2 137.52(10) . . ?
N1 U1 N2 67.40(11) . . ?
N3 U1 N2 67.06(10) . . ?
C1 O1 U1 144.5(3) . . ?
C18 O2 U1 144.7(3) . . ?
C27 O5 H5 109.5 . . ?
C7 N1 C8 115.4(3) . . ?
C7 N1 U1 127.9(3) . . ?
C8 N1 U1 116.4(2) . . ?
C10 N2 C9 107.7(3) . . ?
C10 N2 C19 111.7(3) . . ?
C9 N2 C19 113.7(3) . . ?
C10 N2 U1 106.3(2) . . ?
C9 N2 U1 105.2(2) . . ?
C19 N2 U1 111.7(2) . . ?
C12 N3 C11 114.9(3) . . ?
C12 N3 U1 127.4(3) . . ?
C11 N3 U1 116.1(2) . . ?
C21 N4 C20 117.6(4) . . ?
O1 C1 C2 120.6(4) . . ?
O1 C1 C6 121.0(4) . . ?
C2 C1 C6 118.4(4) . . ?
C3 C2 C1 121.3(4) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C2 C3 C4 120.5(4) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C5 C4 C3 119.2(4) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C6 121.3(4) . . ?
C4 C5 H5A 119.4 . . ?
C6 C5 H5A 119.4 . . ?
C5 C6 C1 119.2(4) . . ?
C5 C6 C7 117.9(4) . . ?
C1 C6 C7 122.6(4) . . ?
N1 C7 C6 128.4(4) . . ?
N1 C7 H7 115.8 . . ?
C6 C7 H7 115.8 . . ?
N1 C8 C9 111.2(3) . . ?
N1 C8 H8A 109.4 . . ?
C9 C8 H8A 109.4 . . ?
N1 C8 H8B 109.4 . . ?
C9 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
N2 C9 C8 112.2(3) . . ?
N2 C9 H9A 109.2 . . ?
C8 C9 H9A 109.2 . . ?
N2 C9 H9B 109.2 . . ?
C8 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
N2 C10 C11 110.5(3) . . ?
N2 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
N3 C11 C10 108.8(3) . . ?
N3 C11 H11A 109.9 . . ?
C10 C11 H11A 109.9 . . ?
N3 C11 H11B 109.9 . . ?
C10 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
N3 C12 C13 128.0(4) . . ?
N3 C12 H12 116.0 . . ?
C13 C12 H12 116.0 . . ?
C14 C13 C18 118.9(4) . . ?
C14 C13 C12 117.1(4) . . ?
C18 C13 C12 124.0(4) . . ?
C15 C14 C13 121.6(4) . . ?
C15 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C14 C15 C16 118.8(4) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?
C17 C16 C15 120.7(4) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C16 C17 C18 121.1(4) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
O2 C18 C17 120.7(4) . . ?
O2 C18 C13 120.5(4) . . ?
C17 C18 C13 118.8(4) . . ?
N2 C19 C20 118.8(3) . . ?
N2 C19 H19A 107.6 . . ?
C20 C19 H19A 107.6 . . ?
N2 C19 H19B 107.6 . . ?
C20 C19 H19B 107.6 . . ?
H19A C19 H19B 107.1 . . ?
N4 C20 C19 114.6(4) . . ?
N4 C20 H20A 108.6 . . ?
C19 C20 H20A 108.6 . . ?
N4 C20 H20B 108.6 . . ?
C19 C20 H20B 108.6 . . ?
H20A C20 H20B 107.6 . . ?
N4 C21 C22 121.7(4) . . ?
N4 C21 H21 119.2 . . ?
C22 C21 H21 119.2 . . ?
C23 C22 C27 118.6(4) . . ?
C23 C22 C21 119.6(4) . . ?
C27 C22 C21 121.8(4) . . ?
C24 C23 C22 121.0(4) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C23 C24 C25 119.7(4) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C26 C25 C24 120.6(4) . . ?
C26 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
C25 C26 C27 120.0(4) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
O5 C27 C26 118.5(4) . . ?
O5 C27 C22 121.5(4) . . ?
C26 C27 C22 120.0(4) . . ?
C32 N5 C28 115.7(4) . . ?
N5 C28 C29 124.3(4) . . ?
N5 C28 H28 117.8 . . ?
C29 C28 H28 117.8 . . ?
C28 C29 C30 118.6(4) . . ?
C28 C29 H29 120.7 . . ?
C30 C29 H29 120.7 . . ?
C31 C30 C29 118.3(4) . . ?
C31 C30 H30 120.9 . . ?
C29 C30 H30 120.9 . . ?
C30 C31 C32 118.8(4) . . ?
C30 C31 H31 120.6 . . ?
C32 C31 H31 120.6 . . ?
N5 C32 C31 124.2(4) . . ?
N5 C32 H32 117.9 . . ?
C31 C32 H32 117.9 . . ?

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 O1 C1 C2 162.1(3) . . . . ?
U1 O1 C1 C6 -19.4(7) . . . . ?
O1 C1 C2 C3 -180.0(4) . . . . ?
C6 C1 C2 C3 1.5(6) . . . . ?
C1 C2 C3 C4 0.2(7) . . . . ?
C2 C3 C4 C5 -2.1(7) . . . . ?
C3 C4 C5 C6 2.3(7) . . . . ?
C4 C5 C6 C1 -0.6(6) . . . . ?
C4 C5 C6 C7 -174.7(4) . . . . ?
O1 C1 C6 C5 -179.8(4) . . . . ?
C2 C1 C6 C5 -1.3(6) . . . . ?
O1 C1 C6 C7 -6.0(6) . . . . ?
C2 C1 C6 C7 172.5(4) . . . . ?
C8 N1 C7 C6 -174.8(4) . . . . ?
U1 N1 C7 C6 11.5(6) . . . . ?
C5 C6 C7 N1 180.0(4) . . . . ?
C1 C6 C7 N1 6.1(7) . . . . ?
C7 N1 C8 C9 168.7(4) . . . . ?
U1 N1 C8 C9 -16.8(4) . . . . ?
C10 N2 C9 C8 -171.3(3) . . . . ?
C19 N2 C9 C8 64.4(4) . . . . ?
U1 N2 C9 C8 -58.2(3) . . . . ?
N1 C8 C9 N2 52.1(5) . . . . ?
C9 N2 C10 C11 171.1(3) . . . . ?
C19 N2 C10 C11 -63.4(4) . . . . ?
U1 N2 C10 C11 58.7(3) . . . . ?
C12 N3 C11 C10 -137.1(4) . . . . ?
U1 N3 C11 C10 29.6(4) . . . . ?
N2 C10 C11 N3 -60.5(4) . . . . ?
C11 N3 C12 C13 -180.0(4) . . . . ?
U1 N3 C12 C13 15.0(6) . . . . ?
N3 C12 C13 C14 179.5(4) . . . . ?
N3 C12 C13 C18 0.4(7) . . . . ?
C18 C13 C14 C15 1.0(6) . . . . ?
C12 C13 C14 C15 -178.1(4) . . . . ?
C13 C14 C15 C16 0.4(7) . . . . ?
C14 C15 C16 C17 -0.5(7) . . . . ?
C15 C16 C17 C18 -0.8(6) . . . . ?
U1 O2 C18 C17 160.9(3) . . . . ?
U1 O2 C18 C13 -20.6(7) . . . . ?
C16 C17 C18 O2 -179.2(4) . . . . ?
C16 C17 C18 C13 2.3(6) . . . . ?
C14 C13 C18 O2 179.1(4) . . . . ?
C12 C13 C18 O2 -1.8(6) . . . . ?
C14 C13 C18 C17 -2.3(6) . . . . ?
C12 C13 C18 C17 176.7(4) . . . . ?
C10 N2 C19 C20 -44.1(5) . . . . ?
C9 N2 C19 C20 78.0(5) . . . . ?
U1 N2 C19 C20 -163.0(3) . . . . ?
C21 N4 C20 C19 -119.5(4) . . . . ?
N2 C19 C20 N4 -59.7(5) . . . . ?
C20 N4 C21 C22 -178.0(4) . . . . ?
N4 C21 C22 C23 -176.2(4) . . . . ?
N4 C21 C22 C27 2.7(7) . . . . ?
C27 C22 C23 C24 -0.4(7) . . . . ?
C21 C22 C23 C24 178.5(4) . . . . ?
C22 C23 C24 C25 -0.7(7) . . . . ?
C23 C24 C25 C26 2.1(7) . . . . ?
C24 C25 C26 C27 -2.3(7) . . . . ?
C25 C26 C27 O5 -179.5(4) . . . . ?
C25 C26 C27 C22 1.1(6) . . . . ?
C23 C22 C27 O5 -179.2(4) . . . . ?
C21 C22 C27 O5 2.0(6) . . . . ?
C23 C22 C27 C26 0.2(6) . . . . ?
C21 C22 C27 C26 -178.7(4) . . . . ?
C32 N5 C28 C29 0.4(7) . . . . ?
N5 C28 C29 C30 0.2(7) . . . . ?
C28 C29 C30 C31 0.1(7) . . . . ?
C29 C30 C31 C32 -0.9(7) . . . . ?
C28 N5 C32 C31 -1.4(8) . . . . ?
C30 C31 C32 N5 1.7(8) . . . . ?

_refine_diff_density_max         1.890
_refine_diff_density_min         -2.137
_refine_diff_density_rms         0.144




_publcif_funding_html            
;
;
####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1842378'
_audit_update_record             
;
2018-05-09 deposited with the CCDC.
2018-08-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C64 H64 Fe N10 O10 U2'
_chemical_formula_sum            'C64 H64 Fe N10 O10 U2'
_chemical_formula_weight         1665.16

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'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   46.746(5)
_cell_length_b                   13.2744(3)
_cell_length_c                   24.296(3)
_cell_angle_alpha                90
_cell_angle_beta                 145.84(3)
_cell_angle_gamma                90
_cell_volume                     8465(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.01(10)
_cell_measurement_reflns_used    18539
_cell_measurement_theta_min      3.7100
_cell_measurement_theta_max      75.8310

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear pale red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_F_000             3232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.025
_exptl_absorpt_coefficient_mu    12.408
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.395
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-7 5 -4 0.0496
-17 7 5 0.0443
-19 3 14 0.0595
15 -7 -3 0.0339
18 -4 -13 0.0527
4 8 1 0.0073
12 6 -10 0.0330
-4 -8 -1 0.0173
17 -3 -1 0.0325
3 -7 3 0.0407
-12 -2 -3 0.0488
-21 0 3 0.0495
-28 1 9 0.0608
27 -4 -12 0.0495

_diffrn_ambient_temperature      100.01(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_detector_area_resol_mean 5.2817
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -65.00  32.00   1.00    3.74    --  -40.91  38.00 -30.00   97
  2  ω     71.00 103.00   1.00    3.74    --   40.91 162.00 -41.00   32
  3  ω    109.00 178.00   1.00   14.96    --  111.85  61.00-150.00   69
  4  ω    128.00 165.00   1.00   14.96    --  111.85 -15.00  30.00   37
  5  ω     89.00 171.00   1.00   14.96    --  111.85  77.00  90.00   82
  6  ω    152.00 178.00   1.00   14.96    --  111.85 125.00  30.00   26
  7  ω     95.00 124.00   1.00   14.96    --  111.85 125.00  30.00   29
  8  ω     86.00 159.00   1.00   14.96    --  111.85  45.00 150.00   73
  9  ω     77.00 108.00   1.00   14.96    --  111.85 -94.00 120.00   31
 10  ω     77.00 122.00   1.00   14.96    --  111.85-125.00  30.00   45
 11  ω     58.00 138.00   1.00   14.96    --  111.85 -45.00 -90.00   80
 12  ω     71.00 109.00   1.00   14.96    --  111.85 -94.00-180.00   38
 13  ω     43.00  97.00   1.00    3.74    --   40.91-125.00-180.00   54
 14  ω     42.00  93.00   1.00   14.96    --  111.85 -94.00 -60.00   51
 15  ω     43.00 138.00   1.00   14.96    --  111.85 -61.00  60.00   95
 16  ω     48.00 138.00   1.00   14.96    --  111.85 -45.00 150.00   90
 17  ω     44.00 120.00   1.00   14.96    --  111.85-125.00  90.00   76
 18  ω     23.00  97.00   1.00    3.74    --   40.91-125.00  30.00   74
 19  ω    -75.00  39.00   1.00    3.74    --  -40.91  19.00-150.00  114
 20  ω   -115.00 -35.00   1.00    3.74    --  -40.91 -38.00  30.00   80
;
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            30689
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.368
_diffrn_reflns_theta_max         76.184
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8737
_reflns_number_gt                8306
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;

_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2016)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0260P)²+6.8282P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8737
_refine_ls_number_parameters     394
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0192
_refine_ls_R_factor_gt           0.0182
_refine_ls_wR_factor_ref         0.0484
_refine_ls_wR_factor_gt          0.0480
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

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 0.25447(2) 0.57406(2) 0.70373(2) 0.01573(3) Uani 1 1 d . . . . .
Fe1 Fe 0.500000 0.500000 1.000000 0.01842(10) Uani 1 2 d S . P . .
O1 O 0.20292(7) 0.44472(13) 0.60308(13) 0.0234(3) Uani 1 1 d . . . . .
O2 O 0.18588(6) 0.67120(13) 0.58661(13) 0.0232(3) Uani 1 1 d . . . . .
O3 O 0.24380(7) 0.56463(12) 0.75930(13) 0.0220(3) Uani 1 1 d . . . . .
O4 O 0.27029(7) 0.58443(13) 0.65770(13) 0.0228(3) Uani 1 1 d . . . . .
O5 O 0.51436(7) 0.56690(13) 0.94998(13) 0.0240(4) Uani 1 1 d . . . . .
N1 N 0.30685(8) 0.40843(15) 0.79162(15) 0.0200(4) Uani 1 1 d . . . . .
N2 N 0.34994(7) 0.59933(15) 0.88143(14) 0.0177(4) Uani 1 1 d . . . . .
N3 N 0.28223(7) 0.75854(15) 0.75340(14) 0.0187(4) Uani 1 1 d . . . . .
N4 N 0.46003(7) 0.63512(16) 0.95737(15) 0.0204(4) Uani 1 1 d . . . . .
N5 N 0.42736(8) 0.43033(17) 0.85043(16) 0.0257(4) Uani 1 1 d . . . . .
C1 C 0.20523(10) 0.36173(18) 0.57766(18) 0.0218(5) Uani 1 1 d . . . . .
C2 C 0.16357(11) 0.3326(2) 0.4783(2) 0.0286(5) Uani 1 1 d . . . . .
H2 H 0.134235 0.374355 0.429651 0.034 Uiso 1 1 calc R U . . .
C3 C 0.16506(12) 0.2436(2) 0.4509(2) 0.0315(6) Uani 1 1 d . . . . .
H3 H 0.137134 0.225937 0.383521 0.038 Uiso 1 1 calc R U . . .
C4 C 0.20742(12) 0.1790(2) 0.5218(2) 0.0296(5) Uani 1 1 d . . . . .
H4 H 0.208306 0.118171 0.502583 0.035 Uiso 1 1 calc R U . . .
C5 C 0.24755(10) 0.20505(18) 0.6191(2) 0.0250(5) Uani 1 1 d . . . . .
H5 H 0.275493 0.160084 0.667374 0.030 Uiso 1 1 calc R U . . .
C6 C 0.24804(10) 0.29678(17) 0.64868(19) 0.0216(5) Uani 1 1 d . . . . .
C7 C 0.29373(9) 0.32215(17) 0.75251(18) 0.0211(5) Uani 1 1 d . . . . .
H7 H 0.316404 0.268118 0.796186 0.025 Uiso 1 1 calc R U . . .
C8 C 0.35787(9) 0.41263(18) 0.89814(18) 0.0222(5) Uani 1 1 d . . . . .
H8A H 0.384172 0.405276 0.911081 0.027 Uiso 1 1 calc R U . . .
H8B H 0.361784 0.356082 0.930601 0.027 Uiso 1 1 calc R U . . .
C9 C 0.36559(9) 0.51162(18) 0.94043(17) 0.0202(4) Uani 1 1 d . . . . .
H9A H 0.345457 0.511093 0.942838 0.024 Uiso 1 1 calc R U . . .
H9B H 0.401975 0.518691 1.008384 0.024 Uiso 1 1 calc R U . . .
C10 C 0.35237(9) 0.69131(18) 0.91990(18) 0.0211(5) Uani 1 1 d . . . . .
H10A H 0.388036 0.703253 0.988234 0.025 Uiso 1 1 calc R U . . .
H10B H 0.331551 0.681382 0.920290 0.025 Uiso 1 1 calc R U . . .
C11 C 0.33285(9) 0.78261(18) 0.85740(18) 0.0220(5) Uani 1 1 d . . . . .
H11A H 0.330101 0.841117 0.878118 0.026 Uiso 1 1 calc R U . . .
H11B H 0.356887 0.800112 0.865765 0.026 Uiso 1 1 calc R U . . .
C12 C 0.25906(9) 0.83348(18) 0.69490(19) 0.0217(5) Uani 1 1 d . . . . .
H12 H 0.275849 0.896799 0.723471 0.026 Uiso 1 1 calc R U . . .
C13 C 0.20975(9) 0.83180(18) 0.58929(18) 0.0214(5) Uani 1 1 d . . . . .
C14 C 0.19545(11) 0.91743(19) 0.5365(2) 0.0266(5) Uani 1 1 d . . . . .
H14 H 0.218418 0.972544 0.570456 0.032 Uiso 1 1 calc R U . . .
C15 C 0.14882(11) 0.92337(19) 0.4365(2) 0.0293(6) Uani 1 1 d . . . . .
H15 H 0.139657 0.982102 0.401832 0.035 Uiso 1 1 calc R U . . .
C16 C 0.11505(10) 0.8419(2) 0.38629(19) 0.0281(5) Uani 1 1 d . . . . .
H16 H 0.083118 0.844986 0.317111 0.034 Uiso 1 1 calc R U . . .
C17 C 0.12782(10) 0.75742(19) 0.43654(18) 0.0240(5) Uani 1 1 d . . . . .
H17 H 0.104306 0.703194 0.401565 0.029 Uiso 1 1 calc R U . . .
C18 C 0.17518(9) 0.75019(18) 0.53896(19) 0.0216(5) Uani 1 1 d . . . . .
C19 C 0.38007(9) 0.60934(17) 0.87799(17) 0.0193(4) Uani 1 1 d . . . . .
H19A H 0.362995 0.659451 0.826918 0.023 Uiso 1 1 calc R U . . .
H19B H 0.379190 0.543898 0.857064 0.023 Uiso 1 1 calc R U . . .
C20 C 0.43600(9) 0.64083(18) 0.97377(17) 0.0209(4) Uani 1 1 d . . . . .
H20A H 0.438122 0.710379 0.991683 0.025 Uiso 1 1 calc R U . . .
H20B H 0.453538 0.595127 1.027729 0.025 Uiso 1 1 calc R U . . .
C21 C 0.45285(9) 0.71307(18) 0.91501(18) 0.0222(5) Uani 1 1 d . . . . .
H21 H 0.433525 0.766715 0.899559 0.027 Uiso 1 1 calc R U . . .
C22 C 0.47137(9) 0.72676(19) 0.88873(18) 0.0235(5) Uani 1 1 d . . . . .
C23 C 0.45902(10) 0.8185(2) 0.84310(19) 0.0263(5) Uani 1 1 d . . . . .
H23 H 0.438062 0.865637 0.828527 0.032 Uiso 1 1 calc R U . . .
C24 C 0.47652(10) 0.8416(2) 0.81913(19) 0.0284(5) Uani 1 1 d . . . . .
H24 H 0.467481 0.903444 0.787636 0.034 Uiso 1 1 calc R U . . .
C25 C 0.50795(10) 0.7721(2) 0.84208(18) 0.0276(5) Uani 1 1 d . . . . .
H25 H 0.521173 0.788186 0.827803 0.033 Uiso 1 1 calc R U . . .
C26 C 0.51992(9) 0.6815(2) 0.88479(18) 0.0249(5) Uani 1 1 d . . . . .
H26 H 0.540727 0.635498 0.898083 0.030 Uiso 1 1 calc R U . . .
C27 C 0.50221(9) 0.65383(19) 0.90991(17) 0.0215(5) Uani 1 1 d . . . . .
C28 C 0.39153(10) 0.4875(2) 0.76905(19) 0.0274(5) Uani 1 1 d . . . . .
H28 H 0.400149 0.554178 0.772117 0.033 Uiso 1 1 calc R U . . .
C29 C 0.34258(11) 0.4531(3) 0.6809(2) 0.0334(6) Uani 1 1 d . . . . .
H29 H 0.317920 0.496178 0.625396 0.040 Uiso 1 1 calc R U . . .
C30 C 0.33018(11) 0.3549(3) 0.6751(2) 0.0393(7) Uani 1 1 d . . . . .
H30 H 0.296860 0.329575 0.615613 0.047 Uiso 1 1 calc R U . . .
C31 C 0.36716(12) 0.2946(2) 0.7574(2) 0.0362(6) Uani 1 1 d . . . . .
H31 H 0.360105 0.226327 0.755210 0.043 Uiso 1 1 calc R U . . .
C32 C 0.41484(10) 0.3358(2) 0.8435(2) 0.0291(5) Uani 1 1 d . . . . .
H32 H 0.439882 0.294555 0.900376 0.035 Uiso 1 1 calc R U . . .


_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 O4 1.7851(18) . ?
U1 O3 1.7892(18) . ?
U1 O2 2.223(2) . ?
U1 O1 2.2321(18) . ?
U1 N3 2.558(2) . ?
U1 N1 2.595(2) . ?
U1 N2 2.604(3) . ?
Fe1 O5 2.0164(18) 5_667 ?
Fe1 O5 2.0165(18) . ?
Fe1 N4 2.140(2) . ?
Fe1 N4 2.140(2) 5_667 ?
Fe1 N5 2.274(3) . ?
Fe1 N5 2.274(3) 5_667 ?
O1 C1 1.310(3) . ?
O2 C18 1.316(3) . ?
O5 C27 1.299(3) . ?
N1 C7 1.275(3) . ?
N1 C8 1.474(3) . ?
N2 C10 1.484(3) . ?
N2 C19 1.484(3) . ?
N2 C9 1.487(3) . ?
N3 C12 1.279(3) . ?
N3 C11 1.480(3) . ?
N4 C21 1.292(3) . ?
N4 C20 1.472(3) . ?
N5 C32 1.335(4) . ?
N5 C28 1.345(4) . ?
C1 C2 1.411(4) . ?
C1 C6 1.418(4) . ?
C2 C3 1.385(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.406(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.375(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.404(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.457(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.516(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.521(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.452(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.402(3) . ?
C13 C18 1.418(3) . ?
C14 C15 1.377(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.400(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.378(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.409(4) . ?
C17 H17 0.9500 . ?
C19 C20 1.535(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.451(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.410(4) . ?
C22 C27 1.433(3) . ?
C23 C24 1.375(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.402(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.370(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.425(3) . ?
C26 H26 0.9500 . ?
C28 C29 1.386(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.385(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.382(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.388(4) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?

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 O3 175.52(8) . . ?
O4 U1 O2 93.43(8) . . ?
O3 U1 O2 89.95(8) . . ?
O4 U1 O1 90.25(8) . . ?
O3 U1 O1 92.90(7) . . ?
O2 U1 O1 86.43(8) . . ?
O4 U1 N3 84.85(7) . . ?
O3 U1 N3 93.46(7) . . ?
O2 U1 N3 71.33(7) . . ?
O1 U1 N3 156.84(7) . . ?
O4 U1 N1 89.02(7) . . ?
O3 U1 N1 88.98(7) . . ?
O2 U1 N1 157.53(6) . . ?
O1 U1 N1 71.21(8) . . ?
N3 U1 N1 131.13(7) . . ?
O4 U1 N2 89.92(7) . . ?
O3 U1 N2 85.61(7) . . ?
O2 U1 N2 136.50(7) . . ?
O1 U1 N2 136.96(7) . . ?
N3 U1 N2 65.81(6) . . ?
N1 U1 N2 65.75(7) . . ?
O5 Fe1 O5 180.00(9) 5_667 . ?
O5 Fe1 N4 93.91(7) 5_667 . ?
O5 Fe1 N4 86.09(7) . . ?
O5 Fe1 N4 86.09(7) 5_667 5_667 ?
O5 Fe1 N4 93.90(7) . 5_667 ?
N4 Fe1 N4 180.0 . 5_667 ?
O5 Fe1 N5 88.99(8) 5_667 . ?
O5 Fe1 N5 91.01(8) . . ?
N4 Fe1 N5 90.93(8) . . ?
N4 Fe1 N5 89.07(8) 5_667 . ?
O5 Fe1 N5 91.01(8) 5_667 5_667 ?
O5 Fe1 N5 88.99(8) . 5_667 ?
N4 Fe1 N5 89.06(8) . 5_667 ?
N4 Fe1 N5 90.94(8) 5_667 5_667 ?
N5 Fe1 N5 180.0 . 5_667 ?
C1 O1 U1 136.70(16) . . ?
C18 O2 U1 133.16(15) . . ?
C27 O5 Fe1 133.30(16) . . ?
C7 N1 C8 115.1(2) . . ?
C7 N1 U1 127.10(17) . . ?
C8 N1 U1 117.81(15) . . ?
C10 N2 C19 112.35(18) . . ?
C10 N2 C9 108.48(18) . . ?
C19 N2 C9 113.06(18) . . ?
C10 N2 U1 106.45(13) . . ?
C19 N2 U1 108.81(14) . . ?
C9 N2 U1 107.37(14) . . ?
C12 N3 C11 114.6(2) . . ?
C12 N3 U1 126.01(17) . . ?
C11 N3 U1 118.83(14) . . ?
C21 N4 C20 114.9(2) . . ?
C21 N4 Fe1 127.17(16) . . ?
C20 N4 Fe1 117.92(15) . . ?
C32 N5 C28 117.5(2) . . ?
C32 N5 Fe1 120.21(19) . . ?
C28 N5 Fe1 121.08(18) . . ?
O1 C1 C2 120.1(2) . . ?
O1 C1 C6 121.4(2) . . ?
C2 C1 C6 118.4(2) . . ?
C3 C2 C1 120.6(3) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 120.8(3) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 119.1(2) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C6 121.3(3) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C6 C1 119.7(2) . . ?
C5 C6 C7 117.8(2) . . ?
C1 C6 C7 122.5(2) . . ?
N1 C7 C6 127.6(2) . . ?
N1 C7 H7 116.2 . . ?
C6 C7 H7 116.2 . . ?
N1 C8 C9 110.8(2) . . ?
N1 C8 H8A 109.5 . . ?
C9 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
N2 C9 C8 111.96(19) . . ?
N2 C9 H9A 109.2 . . ?
C8 C9 H9A 109.2 . . ?
N2 C9 H9B 109.2 . . ?
C8 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
N2 C10 C11 110.91(19) . . ?
N2 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.0 . . ?
N3 C11 C10 108.86(19) . . ?
N3 C11 H11A 109.9 . . ?
C10 C11 H11A 109.9 . . ?
N3 C11 H11B 109.9 . . ?
C10 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
N3 C12 C13 126.7(2) . . ?
N3 C12 H12 116.6 . . ?
C13 C12 H12 116.6 . . ?
C14 C13 C18 119.4(2) . . ?
C14 C13 C12 117.5(2) . . ?
C18 C13 C12 123.1(2) . . ?
C15 C14 C13 121.4(2) . . ?
C15 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C14 C15 C16 119.3(2) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C17 C16 C15 120.5(3) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C17 C18 121.0(2) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
O2 C18 C17 120.4(2) . . ?
O2 C18 C13 121.2(2) . . ?
C17 C18 C13 118.4(2) . . ?
N2 C19 C20 116.37(19) . . ?
N2 C19 H19A 108.2 . . ?
C20 C19 H19A 108.2 . . ?
N2 C19 H19B 108.2 . . ?
C20 C19 H19B 108.2 . . ?
H19A C19 H19B 107.3 . . ?
N4 C20 C19 107.43(18) . . ?
N4 C20 H20A 110.2 . . ?
C19 C20 H20A 110.2 . . ?
N4 C20 H20B 110.2 . . ?
C19 C20 H20B 110.2 . . ?
H20A C20 H20B 108.5 . . ?
N4 C21 C22 126.4(2) . . ?
N4 C21 H21 116.8 . . ?
C22 C21 H21 116.8 . . ?
C23 C22 C27 120.1(2) . . ?
C23 C22 C21 116.7(2) . . ?
C27 C22 C21 123.2(2) . . ?
C24 C23 C22 121.7(2) . . ?
C24 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
C23 C24 C25 118.7(3) . . ?
C23 C24 H24 120.7 . . ?
C25 C24 H24 120.7 . . ?
C26 C25 C24 121.1(2) . . ?
C26 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
C25 C26 C27 122.2(2) . . ?
C25 C26 H26 118.9 . . ?
C27 C26 H26 118.9 . . ?
O5 C27 C26 120.1(2) . . ?
O5 C27 C22 123.8(2) . . ?
C26 C27 C22 116.2(2) . . ?
N5 C28 C29 122.8(3) . . ?
N5 C28 H28 118.6 . . ?
C29 C28 H28 118.6 . . ?
C30 C29 C28 119.0(3) . . ?
C30 C29 H29 120.5 . . ?
C28 C29 H29 120.5 . . ?
C31 C30 C29 118.8(3) . . ?
C31 C30 H30 120.6 . . ?
C29 C30 H30 120.6 . . ?
C30 C31 C32 118.6(3) . . ?
C30 C31 H31 120.7 . . ?
C32 C31 H31 120.7 . . ?
N5 C32 C31 123.4(3) . . ?
N5 C32 H32 118.3 . . ?
C31 C32 H32 118.3 . . ?

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 O1 C1 C2 -136.5(2) . . . . ?
U1 O1 C1 C6 46.6(3) . . . . ?
O1 C1 C2 C3 -178.2(2) . . . . ?
C6 C1 C2 C3 -1.3(4) . . . . ?
C1 C2 C3 C4 1.9(4) . . . . ?
C2 C3 C4 C5 0.3(4) . . . . ?
C3 C4 C5 C6 -3.0(4) . . . . ?
C4 C5 C6 C1 3.6(4) . . . . ?
C4 C5 C6 C7 -175.2(2) . . . . ?
O1 C1 C6 C5 175.5(2) . . . . ?
C2 C1 C6 C5 -1.4(3) . . . . ?
O1 C1 C6 C7 -5.8(4) . . . . ?
C2 C1 C6 C7 177.3(2) . . . . ?
C8 N1 C7 C6 -174.1(2) . . . . ?
U1 N1 C7 C6 4.7(4) . . . . ?
C5 C6 C7 N1 162.8(2) . . . . ?
C1 C6 C7 N1 -15.9(4) . . . . ?
C7 N1 C8 C9 -168.9(2) . . . . ?
U1 N1 C8 C9 12.1(2) . . . . ?
C10 N2 C9 C8 172.83(19) . . . . ?
C19 N2 C9 C8 -61.9(3) . . . . ?
U1 N2 C9 C8 58.2(2) . . . . ?
N1 C8 C9 N2 -47.5(3) . . . . ?
C19 N2 C10 C11 58.6(3) . . . . ?
C9 N2 C10 C11 -175.64(18) . . . . ?
U1 N2 C10 C11 -60.4(2) . . . . ?
C12 N3 C11 C10 171.8(2) . . . . ?
U1 N3 C11 C10 -16.1(2) . . . . ?
N2 C10 C11 N3 51.6(2) . . . . ?
C11 N3 C12 C13 178.4(2) . . . . ?
U1 N3 C12 C13 6.9(3) . . . . ?
N3 C12 C13 C14 -168.1(2) . . . . ?
N3 C12 C13 C18 14.8(4) . . . . ?
C18 C13 C14 C15 -1.0(4) . . . . ?
C12 C13 C14 C15 -178.3(2) . . . . ?
C13 C14 C15 C16 -0.3(4) . . . . ?
C14 C15 C16 C17 1.3(4) . . . . ?
C15 C16 C17 C18 -0.9(4) . . . . ?
U1 O2 C18 C17 135.4(2) . . . . ?
U1 O2 C18 C13 -47.4(3) . . . . ?
C16 C17 C18 O2 176.7(2) . . . . ?
C16 C17 C18 C13 -0.5(4) . . . . ?
C14 C13 C18 O2 -175.7(2) . . . . ?
C12 C13 C18 O2 1.4(4) . . . . ?
C14 C13 C18 C17 1.5(4) . . . . ?
C12 C13 C18 C17 178.6(2) . . . . ?
C10 N2 C19 C20 53.4(3) . . . . ?
C9 N2 C19 C20 -69.8(3) . . . . ?
U1 N2 C19 C20 170.98(16) . . . . ?
C21 N4 C20 C19 82.7(2) . . . . ?
Fe1 N4 C20 C19 -95.09(19) . . . . ?
N2 C19 C20 N4 173.76(19) . . . . ?
C20 N4 C21 C22 -178.9(2) . . . . ?
Fe1 N4 C21 C22 -1.3(4) . . . . ?
N4 C21 C22 C23 -179.8(2) . . . . ?
N4 C21 C22 C27 -1.9(4) . . . . ?
C27 C22 C23 C24 -1.1(4) . . . . ?
C21 C22 C23 C24 176.9(2) . . . . ?
C22 C23 C24 C25 -0.8(4) . . . . ?
C23 C24 C25 C26 2.0(4) . . . . ?
C24 C25 C26 C27 -1.4(4) . . . . ?
Fe1 O5 C27 C26 177.84(17) . . . . ?
Fe1 O5 C27 C22 -1.9(4) . . . . ?
C25 C26 C27 O5 179.8(2) . . . . ?
C25 C26 C27 C22 -0.5(4) . . . . ?
C23 C22 C27 O5 -178.6(2) . . . . ?
C21 C22 C27 O5 3.5(4) . . . . ?
C23 C22 C27 C26 1.7(3) . . . . ?
C21 C22 C27 C26 -176.2(2) . . . . ?
C32 N5 C28 C29 2.1(4) . . . . ?
Fe1 N5 C28 C29 -165.4(2) . . . . ?
N5 C28 C29 C30 -1.9(4) . . . . ?
C28 C29 C30 C31 -0.2(4) . . . . ?
C29 C30 C31 C32 1.9(4) . . . . ?
C28 N5 C32 C31 -0.3(4) . . . . ?
Fe1 N5 C32 C31 167.3(2) . . . . ?
C30 C31 C32 N5 -1.7(4) . . . . ?

_refine_diff_density_max         1.461
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.076



####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1842382'
_audit_update_record             
;
2018-05-09 deposited with the CCDC.
2018-08-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C32 H32 N5 O3 U), C5 H5 N, 2(I)'
_chemical_formula_sum            'C69 H69 I2 N11 O6 U2'
_chemical_formula_weight         1878.21

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'
I I -0.4742 1.8119 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.3842(6)
_cell_length_b                   14.1543(8)
_cell_length_c                   16.8027(7)
_cell_angle_alpha                90
_cell_angle_beta                 93.045(4)
_cell_angle_gamma                90
_cell_volume                     3416.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100.01(10)
_cell_measurement_reflns_used    10860
_cell_measurement_theta_min      3.0910
_cell_measurement_theta_max      29.2540

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear intense yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_F_000             1796
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.064
_exptl_absorpt_coefficient_mu    5.697
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.513
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-14 7 15 0.0787
-8 -15 13 0.0287
13 -12 -13 0.0940
13 7 -17 0.0926
-1 20 -5 0.0743
-17 -5 -10 0.0322
17 5 10 0.0322
4 19 4 0.0639
-12 -14 -9 0.0582
-10 5 -19 0.0758
5 -4 22 0.0403
-10 17 0 0.0888
-11 12 -13 0.0783
19 -3 8 0.0480
-6 -18 -8 0.0703
10 -18 0 0.0703
_diffrn_ambient_temperature      100.01(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_detector_area_resol_mean 5.2817
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     44.00  99.00   1.00   37.16    --   11.50 178.00-180.00   55
  2  ω    -35.00  15.00   1.00   37.16    --  -11.97  38.00 -60.00   50
  3  ω    -16.00  17.00   1.00   37.16    --  -11.97 -99.00 120.00   33
  4  ω    -18.00  27.00   1.00   37.16    --  -11.97 -99.00 -30.00   45
  5  ω    -29.00  52.00   1.00   37.16    --  -11.97  38.00 -30.00   81
  6  ω    -31.00  58.00   1.00   37.16    --  -11.97  77.00-180.00   89
;
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            29812
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.822
_diffrn_reflns_theta_max         29.669
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8463
_reflns_number_gt                6666
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2016)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0299P)²+20.0071P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8463
_refine_ls_number_parameters     421
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.0977
_refine_ls_wR_factor_gt          0.0900
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.60859(2) 0.22907(2) 0.31243(2) 0.01662(7) Uani 1 1 d . . . . .
I1 I 0.10003(3) 0.29980(3) 0.37067(2) 0.02312(10) Uani 1 1 d . . . . .
O1 O 0.7454(3) 0.2207(3) 0.2612(2) 0.0209(9) Uani 1 1 d . . . . .
O2 O 0.6125(3) 0.2047(3) 0.4418(2) 0.0215(9) Uani 1 1 d . . . . .
O3 O 0.5448(3) 0.3651(3) 0.2809(3) 0.0222(9) Uani 1 1 d . . . . .
N1 N 0.5900(4) 0.2215(4) 0.1610(3) 0.0210(11) Uani 1 1 d . . . . .
N2 N 0.6657(4) 0.0643(4) 0.3451(3) 0.0220(11) Uani 1 1 d . . . . .
N3 N 0.4374(3) 0.2278(4) 0.3443(3) 0.0187(10) Uani 1 1 d . . . . .
N4 N 0.4971(4) 0.0786(4) 0.2463(3) 0.0229(12) Uani 1 1 d . . . . .
N5 N 0.7156(4) 0.3593(4) 0.3849(3) 0.0196(11) Uani 1 1 d . . . . .
C1 C 0.7940(4) 0.2391(4) 0.1975(4) 0.0188(12) Uani 1 1 d . . . . .
C2 C 0.8907(4) 0.2495(4) 0.2053(4) 0.0221(14) Uani 1 1 d . . . . .
H2 H 0.922142 0.242769 0.256145 0.026 Uiso 1 1 calc R U . . .
C3 C 0.9410(5) 0.2696(5) 0.1393(4) 0.0263(14) Uani 1 1 d . . . . .
H3 H 1.006635 0.276975 0.145337 0.032 Uiso 1 1 calc R U . . .
C4 C 0.8964(5) 0.2790(5) 0.0641(4) 0.0277(15) Uani 1 1 d . . . . .
H4 H 0.931303 0.293263 0.019222 0.033 Uiso 1 1 calc R U . . .
C5 C 0.8019(5) 0.2676(5) 0.0552(4) 0.0263(14) Uani 1 1 d . . . . .
H5 H 0.771922 0.272634 0.003579 0.032 Uiso 1 1 calc R U . . .
C6 C 0.7482(4) 0.2484(4) 0.1211(4) 0.0218(13) Uani 1 1 d . . . . .
C7 C 0.6498(5) 0.2333(5) 0.1072(4) 0.0228(13) Uani 1 1 d . . . . .
H7 H 0.626529 0.231881 0.053226 0.027 Uiso 1 1 calc R U . . .
C8 C 0.4959(5) 0.1910(5) 0.1337(4) 0.0282(15) Uani 1 1 d . . . . .
H8A H 0.486512 0.198595 0.075264 0.034 Uiso 1 1 calc R U . . .
H8B H 0.448148 0.228651 0.159882 0.034 Uiso 1 1 calc R U . . .
C9 C 0.4896(5) 0.0879(5) 0.1569(4) 0.0271(15) Uani 1 1 d . . . . .
H9A H 0.429576 0.061294 0.135843 0.032 Uiso 1 1 calc R U . . .
H9B H 0.540516 0.051981 0.133434 0.032 Uiso 1 1 calc R U . . .
C10 C 0.6688(4) 0.1659(5) 0.4989(4) 0.0214(13) Uani 1 1 d . . . . .
C11 C 0.6798(5) 0.2084(5) 0.5747(4) 0.0265(15) Uani 1 1 d . . . . .
H11 H 0.650171 0.266862 0.584559 0.032 Uiso 1 1 calc R U . . .
C12 C 0.7332(5) 0.1652(6) 0.6342(4) 0.0329(17) Uani 1 1 d . . . . .
H12 H 0.738479 0.193895 0.685414 0.039 Uiso 1 1 calc R U . . .
C13 C 0.7801(5) 0.0806(6) 0.6220(4) 0.0345(17) Uani 1 1 d . . . . .
H13 H 0.818121 0.052576 0.663458 0.041 Uiso 1 1 calc R U . . .
C14 C 0.7697(5) 0.0388(5) 0.5479(4) 0.0295(16) Uani 1 1 d . . . . .
H14 H 0.800808 -0.019102 0.538805 0.035 Uiso 1 1 calc R U . . .
C15 C 0.7144(4) 0.0795(5) 0.4854(4) 0.0230(14) Uani 1 1 d . . . . .
C16 C 0.7035(5) 0.0298(5) 0.4088(4) 0.0243(14) Uani 1 1 d . . . . .
H16 H 0.726382 -0.033078 0.406604 0.029 Uiso 1 1 calc R U . . .
C17 C 0.6474(4) -0.0017(5) 0.2777(4) 0.0250(14) Uani 1 1 d . . . . .
H17A H 0.677471 -0.063434 0.289179 0.030 Uiso 1 1 calc R U . . .
H17B H 0.671972 0.024338 0.228322 0.030 Uiso 1 1 calc R U . . .
C18 C 0.5422(5) -0.0131(5) 0.2682(4) 0.0273(15) Uani 1 1 d . . . . .
H18A H 0.526563 -0.060396 0.226216 0.033 Uiso 1 1 calc R U . . .
H18B H 0.518312 -0.036273 0.318768 0.033 Uiso 1 1 calc R U . . .
C19 C 0.4757(4) 0.4253(4) 0.2939(4) 0.0210(13) Uani 1 1 d . . . . .
C20 C 0.4843(5) 0.5206(5) 0.2750(4) 0.0241(14) Uani 1 1 d . . . . .
H20 H 0.539513 0.542809 0.252527 0.029 Uiso 1 1 calc R U . . .
C21 C 0.4123(5) 0.5834(5) 0.2888(4) 0.0267(15) Uani 1 1 d . . . . .
H21 H 0.418970 0.648400 0.276053 0.032 Uiso 1 1 calc R U . . .
C22 C 0.3311(5) 0.5519(5) 0.3210(4) 0.0268(15) Uani 1 1 d . . . . .
H22 H 0.281956 0.595036 0.329479 0.032 Uiso 1 1 calc R U . . .
C23 C 0.3217(5) 0.4584(5) 0.3406(4) 0.0256(14) Uani 1 1 d . . . . .
H23 H 0.266245 0.437072 0.363160 0.031 Uiso 1 1 calc R U . . .
C24 C 0.3934(4) 0.3941(4) 0.3276(4) 0.0207(13) Uani 1 1 d . . . . .
C25 C 0.3779(4) 0.2948(5) 0.3464(3) 0.0199(13) Uani 1 1 d . . . . .
H25 H 0.317462 0.278243 0.361842 0.024 Uiso 1 1 calc R U . . .
C26 C 0.4043(5) 0.1307(5) 0.3574(4) 0.0257(14) Uani 1 1 d . . . . .
H26A H 0.341376 0.131677 0.378565 0.031 Uiso 1 1 calc R U . . .
H26B H 0.447045 0.097243 0.395993 0.031 Uiso 1 1 calc R U . . .
C27 C 0.4020(4) 0.0818(5) 0.2770(4) 0.0249(14) Uani 1 1 d . . . . .
H27A H 0.377883 0.016682 0.282271 0.030 Uiso 1 1 calc R U . . .
H27B H 0.359593 0.116298 0.238792 0.030 Uiso 1 1 calc R U . . .
C28 C 0.8064(4) 0.3457(5) 0.4011(4) 0.0232(13) Uani 1 1 d . . . . .
H28 H 0.834424 0.290756 0.380506 0.028 Uiso 1 1 calc R U . . .
C29 C 0.8624(5) 0.4081(5) 0.4467(4) 0.0286(15) Uani 1 1 d . . . . .
H29 H 0.926440 0.394811 0.458085 0.034 Uiso 1 1 calc R U . . .
C30 C 0.8226(5) 0.4899(5) 0.4751(4) 0.0312(16) Uani 1 1 d . . . . .
H30 H 0.858867 0.534516 0.505429 0.037 Uiso 1 1 calc R U . . .
C31 C 0.7289(6) 0.5045(5) 0.4580(4) 0.0332(16) Uani 1 1 d . . . . .
H31 H 0.699358 0.559642 0.476704 0.040 Uiso 1 1 calc R U . . .
C32 C 0.6779(5) 0.4382(5) 0.4131(4) 0.0281(15) Uani 1 1 d . . . . .
H32 H 0.613384 0.449258 0.401978 0.034 Uiso 1 1 calc R U . . .
N6 N 0.5184(12) 0.3996(12) 0.0195(9) 0.034(4) Uani 0.5 1 d G U P A -1
C33 C 0.4909(11) 0.4357(11) -0.0550(8) 0.031(4) Uani 0.5 1 d G U P A -1
H33 H 0.479900 0.394195 -0.098903 0.037 Uiso 0.5 1 calc R U P A -1
C34 C 0.4794(11) 0.5325(12) -0.0652(8) 0.026(4) Uani 0.5 1 d G U P A -1
H34 H 0.460541 0.557196 -0.116102 0.031 Uiso 0.5 1 calc R U P A -1
C35 C 0.4954(13) 0.5933(12) -0.0009(9) 0.040(6) Uani 0.5 1 d G U P A -1
H35 H 0.487585 0.659431 -0.007901 0.048 Uiso 0.5 1 calc R U P A -1
C36 C 0.5230(14) 0.5572(13) 0.0736(9) 0.056(7) Uani 0.5 1 d G U P A -1
H36 H 0.533989 0.598666 0.117499 0.067 Uiso 0.5 1 calc R U P A -1
C37 C 0.5345(13) 0.4603(14) 0.0838(8) 0.043(6) Uani 0.5 1 d G U P A -1
H37 H 0.553350 0.435665 0.134699 0.052 Uiso 0.5 1 calc R U P A -1


_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 O3 2.185(4) . ?
U1 O1 2.193(4) . ?
U1 O2 2.199(4) . ?
U1 N2 2.523(5) . ?
U1 N1 2.546(5) . ?
U1 N3 2.548(5) . ?
U1 N5 2.655(5) . ?
U1 N4 2.855(5) . ?
O1 C1 1.335(7) . ?
O2 C10 1.340(8) . ?
O3 C19 1.337(7) . ?
N1 C7 1.292(8) . ?
N1 C8 1.470(8) . ?
N2 C16 1.272(8) . ?
N2 C17 1.481(8) . ?
N3 C25 1.279(8) . ?
N3 C26 1.474(8) . ?
N4 C27 1.488(8) . ?
N4 C18 1.489(9) . ?
N4 C9 1.506(8) . ?
N5 C28 1.334(8) . ?
N5 C32 1.339(8) . ?
C1 C2 1.399(8) . ?
C1 C6 1.416(9) . ?
C2 C3 1.385(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.393(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.369(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.410(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.439(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.515(10) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.409(9) . ?
C10 C15 1.413(9) . ?
C11 C12 1.372(10) . ?
C11 H11 0.9500 . ?
C12 C13 1.395(11) . ?
C12 H12 0.9500 . ?
C13 C14 1.379(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.406(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.469(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.520(9) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.392(9) . ?
C19 C24 1.410(9) . ?
C20 C21 1.394(9) . ?
C20 H20 0.9500 . ?
C21 C22 1.388(9) . ?
C21 H21 0.9500 . ?
C22 C23 1.373(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.401(9) . ?
C23 H23 0.9500 . ?
C24 C25 1.460(9) . ?
C25 H25 0.9500 . ?
C26 C27 1.517(9) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.397(9) . ?
C28 H28 0.9500 . ?
C29 C30 1.387(10) . ?
C29 H29 0.9500 . ?
C30 C31 1.380(10) . ?
C30 H30 0.9500 . ?
C31 C32 1.388(10) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
N6 C33 1.3900 . ?
N6 C37 1.3900 . ?
C33 C34 1.3900 . ?
C33 H33 0.9500 . ?
C34 C35 1.3900 . ?
C34 H34 0.9500 . ?
C35 C36 1.3900 . ?
C35 H35 0.9500 . ?
C36 C37 1.3900 . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?

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
O3 U1 O1 109.05(16) . . ?
O3 U1 O2 111.49(16) . . ?
O1 U1 O2 113.78(16) . . ?
O3 U1 N2 173.94(16) . . ?
O1 U1 N2 75.33(16) . . ?
O2 U1 N2 69.46(16) . . ?
O3 U1 N1 76.94(16) . . ?
O1 U1 N1 69.80(16) . . ?
O2 U1 N1 167.69(17) . . ?
N2 U1 N1 101.19(17) . . ?
O3 U1 N3 70.10(16) . . ?
O1 U1 N3 168.47(16) . . ?
O2 U1 N3 76.41(16) . . ?
N2 U1 N3 104.74(17) . . ?
N1 U1 N3 99.10(16) . . ?
O3 U1 N5 74.07(16) . . ?
O1 U1 N5 72.97(15) . . ?
O2 U1 N5 70.83(16) . . ?
N2 U1 N5 111.59(16) . . ?
N1 U1 N5 121.01(16) . . ?
N3 U1 N5 116.86(16) . . ?
O3 U1 N4 110.02(16) . . ?
O1 U1 N4 107.72(15) . . ?
O2 U1 N4 104.60(16) . . ?
N2 U1 N4 64.21(16) . . ?
N1 U1 N4 63.42(16) . . ?
N3 U1 N4 63.07(16) . . ?
N5 U1 N4 174.98(15) . . ?
C1 O1 U1 145.4(4) . . ?
C10 O2 U1 139.0(4) . . ?
C19 O3 U1 145.9(4) . . ?
C7 N1 C8 117.1(5) . . ?
C7 N1 U1 130.9(4) . . ?
C8 N1 U1 111.7(4) . . ?
C16 N2 C17 116.9(6) . . ?
C16 N2 U1 131.1(4) . . ?
C17 N2 U1 112.0(4) . . ?
C25 N3 C26 117.7(5) . . ?
C25 N3 U1 131.0(4) . . ?
C26 N3 U1 111.2(4) . . ?
C27 N4 C18 109.7(5) . . ?
C27 N4 C9 109.0(5) . . ?
C18 N4 C9 109.2(5) . . ?
C27 N4 U1 110.5(4) . . ?
C18 N4 U1 109.0(4) . . ?
C9 N4 U1 109.4(4) . . ?
C28 N5 C32 117.3(6) . . ?
C28 N5 U1 122.1(4) . . ?
C32 N5 U1 120.4(4) . . ?
O1 C1 C2 120.4(6) . . ?
O1 C1 C6 120.5(5) . . ?
C2 C1 C6 119.2(6) . . ?
C3 C2 C1 120.4(6) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C2 C3 C4 120.7(6) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 119.7(6) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 121.2(6) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C1 118.8(6) . . ?
C5 C6 C7 118.4(6) . . ?
C1 C6 C7 122.6(6) . . ?
N1 C7 C6 126.3(6) . . ?
N1 C7 H7 116.9 . . ?
C6 C7 H7 116.9 . . ?
N1 C8 C9 105.6(5) . . ?
N1 C8 H8A 110.6 . . ?
C9 C8 H8A 110.6 . . ?
N1 C8 H8B 110.6 . . ?
C9 C8 H8B 110.6 . . ?
H8A C8 H8B 108.8 . . ?
N4 C9 C8 109.7(5) . . ?
N4 C9 H9A 109.7 . . ?
C8 C9 H9A 109.7 . . ?
N4 C9 H9B 109.7 . . ?
C8 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
O2 C10 C11 120.5(6) . . ?
O2 C10 C15 120.6(5) . . ?
C11 C10 C15 118.9(6) . . ?
C12 C11 C10 120.1(7) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 122.0(6) . . ?
C11 C12 H12 119.0 . . ?
C13 C12 H12 119.0 . . ?
C14 C13 C12 118.2(6) . . ?
C14 C13 H13 120.9 . . ?
C12 C13 H13 120.9 . . ?
C13 C14 C15 121.9(7) . . ?
C13 C14 H14 119.1 . . ?
C15 C14 H14 119.1 . . ?
C14 C15 C10 119.0(6) . . ?
C14 C15 C16 119.2(6) . . ?
C10 C15 C16 121.8(6) . . ?
N2 C16 C15 125.1(6) . . ?
N2 C16 H16 117.5 . . ?
C15 C16 H16 117.5 . . ?
N2 C17 C18 106.4(5) . . ?
N2 C17 H17A 110.4 . . ?
C18 C17 H17A 110.4 . . ?
N2 C17 H17B 110.4 . . ?
C18 C17 H17B 110.4 . . ?
H17A C17 H17B 108.6 . . ?
N4 C18 C17 110.6(5) . . ?
N4 C18 H18A 109.5 . . ?
C17 C18 H18A 109.5 . . ?
N4 C18 H18B 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
O3 C19 C20 120.3(6) . . ?
O3 C19 C24 120.9(6) . . ?
C20 C19 C24 118.9(6) . . ?
C19 C20 C21 120.2(6) . . ?
C19 C20 H20 119.9 . . ?
C21 C20 H20 119.9 . . ?
C22 C21 C20 120.6(6) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C23 C22 C21 119.9(6) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 120.4(6) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
C23 C24 C19 120.0(6) . . ?
C23 C24 C25 118.0(6) . . ?
C19 C24 C25 122.0(6) . . ?
N3 C25 C24 126.8(6) . . ?
N3 C25 H25 116.6 . . ?
C24 C25 H25 116.6 . . ?
N3 C26 C27 106.5(5) . . ?
N3 C26 H26A 110.4 . . ?
C27 C26 H26A 110.4 . . ?
N3 C26 H26B 110.4 . . ?
C27 C26 H26B 110.4 . . ?
H26A C26 H26B 108.6 . . ?
N4 C27 C26 110.2(5) . . ?
N4 C27 H27A 109.6 . . ?
C26 C27 H27A 109.6 . . ?
N4 C27 H27B 109.6 . . ?
C26 C27 H27B 109.6 . . ?
H27A C27 H27B 108.1 . . ?
N5 C28 C29 123.4(6) . . ?
N5 C28 H28 118.3 . . ?
C29 C28 H28 118.3 . . ?
C30 C29 C28 118.7(6) . . ?
C30 C29 H29 120.7 . . ?
C28 C29 H29 120.7 . . ?
C31 C30 C29 118.0(6) . . ?
C31 C30 H30 121.0 . . ?
C29 C30 H30 121.0 . . ?
C30 C31 C32 119.6(7) . . ?
C30 C31 H31 120.2 . . ?
C32 C31 H31 120.2 . . ?
N5 C32 C31 123.0(7) . . ?
N5 C32 H32 118.5 . . ?
C31 C32 H32 118.5 . . ?
C33 N6 C37 120.0 . . ?
C34 C33 N6 120.0 . . ?
C34 C33 H33 120.0 . . ?
N6 C33 H33 120.0 . . ?
C33 C34 C35 120.0 . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C34 C35 C36 120.0 . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C37 C36 C35 120.0 . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 N6 120.0 . . ?
C36 C37 H37 120.0 . . ?
N6 C37 H37 120.0 . . ?

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 O1 C1 C2 156.9(5) . . . . ?
U1 O1 C1 C6 -23.1(10) . . . . ?
O1 C1 C2 C3 -179.4(6) . . . . ?
C6 C1 C2 C3 0.6(9) . . . . ?
C1 C2 C3 C4 -0.5(10) . . . . ?
C2 C3 C4 C5 -0.5(10) . . . . ?
C3 C4 C5 C6 1.4(10) . . . . ?
C4 C5 C6 C1 -1.3(10) . . . . ?
C4 C5 C6 C7 -177.5(6) . . . . ?
O1 C1 C6 C5 -179.8(6) . . . . ?
C2 C1 C6 C5 0.2(9) . . . . ?
O1 C1 C6 C7 -3.7(9) . . . . ?
C2 C1 C6 C7 176.3(6) . . . . ?
C8 N1 C7 C6 -169.8(6) . . . . ?
U1 N1 C7 C6 4.6(10) . . . . ?
C5 C6 C7 N1 -174.9(6) . . . . ?
C1 C6 C7 N1 9.0(11) . . . . ?
C7 N1 C8 C9 105.8(6) . . . . ?
U1 N1 C8 C9 -69.7(5) . . . . ?
C27 N4 C9 C8 91.2(6) . . . . ?
C18 N4 C9 C8 -148.9(5) . . . . ?
U1 N4 C9 C8 -29.8(6) . . . . ?
N1 C8 C9 N4 64.4(7) . . . . ?
U1 O2 C10 C11 141.0(5) . . . . ?
U1 O2 C10 C15 -42.2(9) . . . . ?
O2 C10 C11 C12 176.1(6) . . . . ?
C15 C10 C11 C12 -0.7(9) . . . . ?
C10 C11 C12 C13 1.8(11) . . . . ?
C11 C12 C13 C14 -1.7(11) . . . . ?
C12 C13 C14 C15 0.5(11) . . . . ?
C13 C14 C15 C10 0.5(10) . . . . ?
C13 C14 C15 C16 -177.8(6) . . . . ?
O2 C10 C15 C14 -177.2(6) . . . . ?
C11 C10 C15 C14 -0.4(9) . . . . ?
O2 C10 C15 C16 1.1(9) . . . . ?
C11 C10 C15 C16 177.9(6) . . . . ?
C17 N2 C16 C15 -170.3(6) . . . . ?
U1 N2 C16 C15 7.0(10) . . . . ?
C14 C15 C16 N2 -170.4(6) . . . . ?
C10 C15 C16 N2 11.3(10) . . . . ?
C16 N2 C17 C18 110.4(6) . . . . ?
U1 N2 C17 C18 -67.5(6) . . . . ?
C27 N4 C18 C17 -150.8(5) . . . . ?
C9 N4 C18 C17 89.8(6) . . . . ?
U1 N4 C18 C17 -29.6(6) . . . . ?
N2 C17 C18 N4 63.3(7) . . . . ?
U1 O3 C19 C20 158.2(5) . . . . ?
U1 O3 C19 C24 -21.1(10) . . . . ?
O3 C19 C20 C21 -179.8(6) . . . . ?
C24 C19 C20 C21 -0.4(9) . . . . ?
C19 C20 C21 C22 -0.4(10) . . . . ?
C20 C21 C22 C23 1.0(10) . . . . ?
C21 C22 C23 C24 -0.6(10) . . . . ?
C22 C23 C24 C19 -0.2(10) . . . . ?
C22 C23 C24 C25 -177.4(6) . . . . ?
O3 C19 C24 C23 -179.9(6) . . . . ?
C20 C19 C24 C23 0.7(9) . . . . ?
O3 C19 C24 C25 -2.8(9) . . . . ?
C20 C19 C24 C25 177.8(6) . . . . ?
C26 N3 C25 C24 -173.6(6) . . . . ?
U1 N3 C25 C24 2.2(9) . . . . ?
C23 C24 C25 N3 -174.2(6) . . . . ?
C19 C24 C25 N3 8.7(10) . . . . ?
C25 N3 C26 C27 107.0(6) . . . . ?
U1 N3 C26 C27 -69.6(5) . . . . ?
C18 N4 C27 C26 94.7(6) . . . . ?
C9 N4 C27 C26 -145.8(6) . . . . ?
U1 N4 C27 C26 -25.5(6) . . . . ?
N3 C26 C27 N4 61.3(7) . . . . ?
C32 N5 C28 C29 1.3(9) . . . . ?
U1 N5 C28 C29 -172.7(5) . . . . ?
N5 C28 C29 C30 -1.8(10) . . . . ?
C28 C29 C30 C31 1.2(10) . . . . ?
C29 C30 C31 C32 -0.3(10) . . . . ?
C28 N5 C32 C31 -0.3(10) . . . . ?
U1 N5 C32 C31 173.8(5) . . . . ?
C30 C31 C32 N5 -0.2(11) . . . . ?
C37 N6 C33 C34 0.0 . . . . ?
N6 C33 C34 C35 0.0 . . . . ?
C33 C34 C35 C36 0.0 . . . . ?
C34 C35 C36 C37 0.0 . . . . ?
C35 C36 C37 N6 0.0 . . . . ?
C33 N6 C37 C36 0.0 . . . . ?

_refine_diff_density_max         2.413
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.188

####################################################################### 
# 
# 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_rf309
_database_code_depnum_ccdc_archive 'CCDC 1842377'

_audit_update_record             
;
2018-05-09 deposited with the CCDC.
2018-08-01 downloaded from the CCDC.
;
# publcif _publ_body_element loop end

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H63 K N6 O11 U, C18 H36 K N2 O6'
_chemical_formula_sum            'C63 H99 K2 N8 O17 U'
_chemical_formula_weight         1556.73

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'
K K 0.2009 0.2494 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.542(6)
_cell_length_b                   13.779(10)
_cell_length_c                   23.86(3)
_cell_angle_alpha                81.55(6)
_cell_angle_beta                 78.59(5)
_cell_angle_gamma                86.58(4)
_cell_volume                     3997(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    42
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_F_000             1598
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.111
_exptl_absorpt_coefficient_mu    2.196
_shelx_estimated_absorpt_T_min   0.526
_shelx_estimated_absorpt_T_max   0.793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3835
_exptl_absorpt_correction_T_max  0.6477
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker, 2008) was used for absorption correction.
wR2(int) was 0.1390 before and 0.1143 after correction.
The Ration of minimum to maximum transmission is 0.5921.
The λ/2 correction factor is 0.0015.
;
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37059
_diffrn_reflns_av_unetI/netI     0.1064
_diffrn_reflns_av_R_equivalents  0.1127
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.495
_diffrn_reflns_theta_max         21.899
_diffrn_reflns_theta_full        21.899
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             9507
_reflns_number_gt                6908
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 3.10 (CCDC, 2017)'
_computing_publication_material  'CIFTab (Sheldrick, 2015)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1482P)²+108.2740P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9507
_refine_ls_number_parameters     820
_refine_ls_number_restraints     1001
_refine_ls_R_factor_all          0.1506
_refine_ls_R_factor_gt           0.1088
_refine_ls_wR_factor_ref         0.3156
_refine_ls_wR_factor_gt          0.2739
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.78659(7) 0.61835(6) 0.23567(4) 0.0413(3) Uani 1 1 d . . . . .
K1 K 0.6887(5) 0.3712(4) 0.3880(2) 0.0575(14) Uani 1 1 d . . . . .
O1 O 0.9316(12) 0.6411(13) 0.2822(7) 0.066(4) Uani 1 1 d . . . . .
O2 O 0.6812(12) 0.7268(11) 0.2956(7) 0.058(4) Uani 1 1 d . . . . .
O3 O 0.7393(13) 0.5051(10) 0.2852(6) 0.057(3) Uani 1 1 d . . . . .
O4 O 0.8299(11) 0.7224(10) 0.1808(6) 0.049(3) Uani 1 1 d . . . . .
O5 O 0.6223(11) 0.5744(11) -0.1347(6) 0.048(3) Uani 1 1 d . . . . .
O6 O 0.4527(16) 0.4507(12) 0.4116(8) 0.076(4) Uani 1 1 d . . . . .
O7 O 0.6439(13) 0.5492(11) 0.4234(7) 0.062(4) Uani 1 1 d . . . . .
O8 O 0.7467(16) 0.2401(11) 0.3048(6) 0.070(4) Uani 1 1 d . . . . .
O9 O 0.9072(15) 0.3043(13) 0.3597(7) 0.075(4) Uani 1 1 d . . . . .
O10 O 0.576(2) 0.1800(15) 0.4523(10) 0.111(6) Uani 1 1 d . . . . .
O11 O 0.719(2) 0.2827(16) 0.5066(8) 0.100(5) Uani 1 1 d . . . . .
N1 N 0.9604(16) 0.5128(13) 0.1915(8) 0.056(4) Uani 1 1 d . . . . .
N2 N 0.7537(13) 0.5183(11) 0.1517(7) 0.042(3) Uani 1 1 d . . . . .
N3 N 0.5856(14) 0.6399(13) 0.2180(8) 0.049(4) Uani 1 1 d . . . . .
N4 N 0.8124(15) 0.5920(12) -0.0123(8) 0.052(4) Uani 1 1 d . . . . .
N5 N 0.8512(18) 0.4555(18) 0.4416(9) 0.078(5) Uani 1 1 d . . . . .
N6 N 0.498(2) 0.2783(18) 0.3487(11) 0.093(5) Uani 1 1 d . . . . .
C1 C 1.038(2) 0.622(2) 0.2812(12) 0.071(7) Uani 1 1 d . . . . .
C2 C 1.091(2) 0.6637(19) 0.3158(11) 0.066(6) Uani 1 1 d . . . . .
H2 H 1.052278 0.707327 0.340385 0.079 Uiso 1 1 calc R U . . .
C3 C 1.202(2) 0.644(2) 0.3160(11) 0.072(7) Uani 1 1 d . . . . .
H3 H 1.236665 0.678374 0.338886 0.086 Uiso 1 1 calc R U . . .
C4 C 1.260(2) 0.5787(19) 0.2847(10) 0.065(6) Uani 1 1 d . . . . .
H4 H 1.332176 0.559384 0.289677 0.077 Uiso 1 1 calc R U . . .
C5 C 1.2147(18) 0.5404(19) 0.2456(9) 0.062(6) Uani 1 1 d . . . . .
H5 H 1.257756 0.500882 0.219607 0.074 Uiso 1 1 calc R U . . .
C6 C 1.104(2) 0.5595(18) 0.2439(10) 0.063(6) Uani 1 1 d . . . . .
C7 C 1.059(2) 0.5031(19) 0.2048(10) 0.064(6) Uani 1 1 d . . . . .
H7 H 1.106167 0.454831 0.187592 0.077 Uiso 1 1 calc R U . . .
C8 C 0.9393(19) 0.4459(17) 0.1510(10) 0.056(5) Uani 1 1 d . . . . .
H8A H 0.965310 0.476515 0.110763 0.067 Uiso 1 1 calc R U . . .
H8B H 0.981040 0.383339 0.157375 0.067 Uiso 1 1 calc R U . . .
C9 C 0.8215(19) 0.4249(15) 0.1590(10) 0.051(5) Uani 1 1 d . . . . .
H9A H 0.796773 0.388731 0.197991 0.061 Uiso 1 1 calc R U . . .
H9B H 0.811160 0.382743 0.130363 0.061 Uiso 1 1 calc R U . . .
C10 C 0.6348(18) 0.4918(17) 0.1646(10) 0.058(5) Uani 1 1 d . . . . .
H10A H 0.619147 0.460373 0.132458 0.069 Uiso 1 1 calc R U . . .
H10B H 0.620583 0.443738 0.200128 0.069 Uiso 1 1 calc R U . . .
C11 C 0.5599(18) 0.5806(17) 0.1723(10) 0.052(5) Uani 1 1 d . . . . .
H11A H 0.483851 0.559096 0.183988 0.063 Uiso 1 1 calc R U . . .
H11B H 0.566160 0.623855 0.134876 0.063 Uiso 1 1 calc R U . . .
C12 C 0.5110(18) 0.6980(17) 0.2317(8) 0.050(5) Uani 1 1 d . . . . .
H12 H 0.450093 0.697181 0.213646 0.060 Uiso 1 1 calc R U . . .
C13 C 0.5034(16) 0.7700(16) 0.2733(9) 0.046(4) Uani 1 1 d . . . . .
C14 C 0.4100(19) 0.8328(19) 0.2818(10) 0.064(6) Uani 1 1 d . . . . .
H14 H 0.351556 0.823721 0.263291 0.076 Uiso 1 1 calc R U . . .
C15 C 0.400(2) 0.905(2) 0.3151(13) 0.082(7) Uani 1 1 d . . . . .
H15 H 0.335561 0.944639 0.321977 0.099 Uiso 1 1 calc R U . . .
C16 C 0.493(2) 0.9197(18) 0.3395(11) 0.067(6) Uani 1 1 d . . . . .
H16 H 0.490352 0.974727 0.359556 0.081 Uiso 1 1 calc R U . . .
C17 C 0.584(2) 0.8606(16) 0.3363(10) 0.060(5) Uani 1 1 d . . . . .
H17 H 0.638878 0.869856 0.357210 0.072 Uiso 1 1 calc R U . . .
C18 C 0.5961(18) 0.7833(16) 0.3002(9) 0.051(5) Uani 1 1 d . . . . .
C19 C 0.7864(17) 0.5788(15) 0.0920(9) 0.042(4) Uani 1 1 d . . . . .
H19A H 0.861263 0.601507 0.088089 0.051 Uiso 1 1 calc R U . . .
H19B H 0.737431 0.637663 0.089684 0.051 Uiso 1 1 calc R U . . .
C20 C 0.782(2) 0.5230(17) 0.0406(10) 0.063(6) Uani 1 1 d . . . . .
H20A H 0.834131 0.465832 0.040517 0.076 Uiso 1 1 calc R U . . .
H20B H 0.708369 0.499204 0.043499 0.076 Uiso 1 1 calc R U . . .
C21 C 0.7475(16) 0.5904(14) -0.0480(9) 0.039(4) Uani 1 1 d . . . . .
H21 H 0.690665 0.544752 -0.038426 0.047 Uiso 1 1 calc R U . . .
C22 C 0.7591(15) 0.6581(14) -0.1039(9) 0.039(4) Uani 1 1 d . . . . .
C23 C 0.6910(16) 0.6379(16) -0.1446(9) 0.044(4) Uani 1 1 d . . . . .
C24 C 0.7083(18) 0.7065(16) -0.1993(9) 0.052(5) Uani 1 1 d . . . . .
H24 H 0.664410 0.702590 -0.227071 0.062 Uiso 1 1 calc R U . . .
C25 C 0.7893(19) 0.7777(17) -0.2109(10) 0.055(5) Uani 1 1 d . . . . .
H25 H 0.797711 0.821290 -0.246104 0.066 Uiso 1 1 calc R U . . .
C26 C 0.8570(18) 0.7858(16) -0.1722(9) 0.050(5) Uani 1 1 d . . . . .
H26 H 0.914012 0.831310 -0.182427 0.060 Uiso 1 1 calc R U . . .
C27 C 0.8419(17) 0.7289(15) -0.1199(9) 0.047(4) Uani 1 1 d . . . . .
H27 H 0.887341 0.736460 -0.093464 0.056 Uiso 1 1 calc R U . . .
C28 C 0.437(4) 0.371(3) 0.3377(17) 0.125(12) Uani 1 1 d . . . . .
H28A H 0.487795 0.419727 0.314366 0.150 Uiso 1 1 calc R U . . .
H28B H 0.382907 0.359933 0.314083 0.150 Uiso 1 1 calc R U . . .
C29 C 0.381(3) 0.411(2) 0.3864(15) 0.101(9) Uani 1 1 d . . . . .
H29A H 0.327877 0.462547 0.374721 0.122 Uiso 1 1 calc R U . . .
H29B H 0.340254 0.359416 0.414271 0.122 Uiso 1 1 calc R U . . .
C30 C 0.476(2) 0.5511(17) 0.3907(11) 0.066(5) Uani 1 1 d . . . . .
H30A H 0.407100 0.589161 0.389234 0.079 Uiso 1 1 calc R U . . .
H30B H 0.519203 0.555864 0.350934 0.079 Uiso 1 1 calc R U . . .
C31 C 0.538(2) 0.5956(19) 0.4278(11) 0.067(6) Uani 1 1 d . . . . .
H31A H 0.544958 0.666930 0.414787 0.081 Uiso 1 1 calc R U . . .
H31B H 0.499387 0.586027 0.468453 0.081 Uiso 1 1 calc R U . . .
C32 C 0.718(2) 0.603(2) 0.4462(14) 0.086(8) Uani 1 1 d . . . . .
H32A H 0.694974 0.598590 0.488604 0.103 Uiso 1 1 calc R U . . .
H32B H 0.716855 0.672557 0.429187 0.103 Uiso 1 1 calc R U . . .
C33 C 0.827(2) 0.559(2) 0.4316(13) 0.088(7) Uani 1 1 d . . . . .
H33A H 0.852296 0.579856 0.389811 0.106 Uiso 1 1 calc R U . . .
H33B H 0.873373 0.590848 0.451919 0.106 Uiso 1 1 calc R U . . .
C34 C 0.560(3) 0.235(2) 0.2990(14) 0.099(8) Uani 1 1 d . . . . .
H34A H 0.578548 0.288755 0.266774 0.119 Uiso 1 1 calc R U . . .
H34B H 0.510453 0.191674 0.286959 0.119 Uiso 1 1 calc R U . . .
C35 C 0.663(3) 0.176(2) 0.3056(13) 0.090(7) Uani 1 1 d . . . . .
H35A H 0.650327 0.131241 0.342464 0.108 Uiso 1 1 calc R U . . .
H35B H 0.683603 0.136165 0.273686 0.108 Uiso 1 1 calc R U . . .
C36 C 0.844(3) 0.192(2) 0.3076(13) 0.092(8) Uani 1 1 d . . . . .
H36A H 0.867116 0.154273 0.274544 0.110 Uiso 1 1 calc R U . . .
H36B H 0.839099 0.145254 0.343840 0.110 Uiso 1 1 calc R U . . .
C37 C 0.923(3) 0.268(2) 0.3057(12) 0.087(7) Uani 1 1 d . . . . .
H37A H 0.998209 0.240316 0.296419 0.105 Uiso 1 1 calc R U . . .
H37B H 0.913989 0.322734 0.274904 0.105 Uiso 1 1 calc R U . . .
C38 C 0.965(2) 0.3881(19) 0.3561(11) 0.070(6) Uani 1 1 d . . . . .
H38A H 0.935839 0.440563 0.329594 0.084 Uiso 1 1 calc R U . . .
H38B H 1.041729 0.374549 0.338586 0.084 Uiso 1 1 calc R U . . .
C39 C 0.962(2) 0.428(2) 0.4154(11) 0.076(7) Uani 1 1 d . . . . .
H39A H 0.991556 0.376305 0.442229 0.091 Uiso 1 1 calc R U . . .
H39B H 1.008403 0.485510 0.408711 0.091 Uiso 1 1 calc R U . . .
C40 C 0.449(4) 0.198(3) 0.3914(17) 0.142(11) Uani 1 1 d . . . . .
H40A H 0.370230 0.200675 0.391791 0.171 Uiso 1 1 calc R U . . .
H40B H 0.478550 0.135538 0.377261 0.171 Uiso 1 1 calc R U . . .
C41 C 0.463(3) 0.191(3) 0.4498(16) 0.129(12) Uani 1 1 d . . . . .
H41A H 0.423809 0.134110 0.473235 0.155 Uiso 1 1 calc R U . . .
H41B H 0.432288 0.251123 0.465938 0.155 Uiso 1 1 calc R U . . .
C42 C 0.595(3) 0.155(2) 0.5097(14) 0.109(7) Uani 1 1 d . . . . .
H42A H 0.582798 0.084482 0.522185 0.131 Uiso 1 1 calc R U . . .
H42B H 0.540948 0.192081 0.535590 0.131 Uiso 1 1 calc R U . . .
C43 C 0.706(3) 0.177(2) 0.5161(14) 0.108(8) Uani 1 1 d . . . . .
H43A H 0.717650 0.150445 0.555390 0.130 Uiso 1 1 calc R U . . .
H43B H 0.761158 0.146186 0.487873 0.130 Uiso 1 1 calc R U . . .
C44 C 0.811(4) 0.308(3) 0.5206(13) 0.119(10) Uani 1 1 d . . . . .
H44A H 0.874022 0.272625 0.499364 0.142 Uiso 1 1 calc R U . . .
H44B H 0.808403 0.288022 0.562420 0.142 Uiso 1 1 calc R U . . .
C45 C 0.826(3) 0.418(3) 0.5055(12) 0.103(8) Uani 1 1 d . . . . .
H45A H 0.758229 0.452413 0.523007 0.123 Uiso 1 1 calc R U . . .
H45B H 0.885310 0.436614 0.523327 0.123 Uiso 1 1 calc R U . . .
K2 K 0.7301(3) 0.1075(3) 0.01330(19) 0.0360(10) Uani 1 1 d . . . . .
O12 O 0.8832(11) 0.0710(10) 0.0866(6) 0.045(3) Uani 1 1 d . . . . .
O13 O 0.9429(10) 0.1734(10) -0.0256(6) 0.048(3) Uani 1 1 d . . . . .
O14 O 0.5679(11) 0.1661(10) 0.1041(6) 0.044(3) Uani 1 1 d . . . . .
O15 O 0.6413(10) 0.3004(9) 0.0037(6) 0.043(3) Uani 1 1 d . . . . .
O16 O 0.6658(11) -0.0860(10) 0.0126(6) 0.047(3) Uani 1 1 d . . . . .
O17 O 0.6796(10) 0.0470(10) -0.0916(6) 0.040(3) Uani 1 1 d . . . . .
N7 N 0.6773(13) -0.0270(13) 0.1264(7) 0.047(3) Uani 1 1 d . . . . .
N8 N 0.7806(13) 0.2433(12) -0.1015(7) 0.043(3) Uani 1 1 d . . . . .
C46 C 0.7597(17) -0.0282(17) 0.1606(10) 0.053(5) Uani 1 1 d . . . . .
H46A H 0.756261 -0.090499 0.187467 0.063 Uiso 1 1 calc R U . . .
H46B H 0.743888 0.026265 0.184170 0.063 Uiso 1 1 calc R U . . .
C47 C 0.8729(16) -0.0185(16) 0.1254(9) 0.046(5) Uani 1 1 d . . . . .
H47A H 0.925521 -0.020555 0.151509 0.055 Uiso 1 1 calc R U . . .
H47B H 0.890611 -0.074539 0.103188 0.055 Uiso 1 1 calc R U . . .
C48 C 0.9986(17) 0.0896(17) 0.0602(10) 0.051(5) Uani 1 1 d . . . . .
H48A H 1.030759 0.035170 0.038771 0.062 Uiso 1 1 calc R U . . .
H48B H 1.040989 0.094958 0.090361 0.062 Uiso 1 1 calc R U . . .
C49 C 1.0004(18) 0.1841(17) 0.0197(10) 0.055(5) Uani 1 1 d . . . . .
H49A H 0.965445 0.237580 0.041199 0.067 Uiso 1 1 calc R U . . .
H49B H 1.076569 0.201553 0.002842 0.067 Uiso 1 1 calc R U . . .
C50 C 0.9618(17) 0.2572(17) -0.0708(10) 0.056(5) Uani 1 1 d . . . . .
H50A H 1.040474 0.261916 -0.087258 0.067 Uiso 1 1 calc R U . . .
H50B H 0.936103 0.318597 -0.054713 0.067 Uiso 1 1 calc R U . . .
C51 C 0.8984(17) 0.2421(17) -0.1180(10) 0.055(5) Uani 1 1 d . . . . .
H51A H 0.918649 0.294128 -0.151136 0.066 Uiso 1 1 calc R U . . .
H51B H 0.922764 0.178435 -0.131465 0.066 Uiso 1 1 calc R U . . .
C52 C 0.5699(17) 0.0013(16) 0.1566(10) 0.055(5) Uani 1 1 d . . . . .
H52A H 0.555349 -0.036223 0.195905 0.066 Uiso 1 1 calc R U . . .
H52B H 0.513896 -0.014901 0.135796 0.066 Uiso 1 1 calc R U . . .
C53 C 0.562(2) 0.1114(17) 0.1610(10) 0.057(5) Uani 1 1 d . . . . .
H53A H 0.492726 0.127660 0.186189 0.068 Uiso 1 1 calc R U . . .
H53B H 0.622690 0.129315 0.178170 0.068 Uiso 1 1 calc R U . . .
C54 C 0.5687(17) 0.2653(15) 0.1048(10) 0.048(4) Uani 1 1 d . . . . .
H54A H 0.639475 0.282819 0.112314 0.057 Uiso 1 1 calc R U . . .
H54B H 0.510728 0.284299 0.136268 0.057 Uiso 1 1 calc R U . . .
C55 C 0.5507(16) 0.3203(14) 0.0482(10) 0.045(4) Uani 1 1 d . . . . .
H55A H 0.482532 0.299594 0.039165 0.054 Uiso 1 1 calc R U . . .
H55B H 0.543885 0.391649 0.050541 0.054 Uiso 1 1 calc R U . . .
C56 C 0.6271(17) 0.3420(14) -0.0522(9) 0.045(4) Uani 1 1 d . . . . .
H56A H 0.596787 0.409911 -0.051477 0.054 Uiso 1 1 calc R U . . .
H56B H 0.575564 0.303116 -0.065573 0.054 Uiso 1 1 calc R U . . .
C57 C 0.7379(17) 0.3424(15) -0.0932(9) 0.049(5) Uani 1 1 d . . . . .
H57A H 0.730594 0.379702 -0.131087 0.059 Uiso 1 1 calc R U . . .
H57B H 0.790418 0.376331 -0.077463 0.059 Uiso 1 1 calc R U . . .
C58 C 0.6675(19) -0.1313(17) 0.1127(11) 0.061(5) Uani 1 1 d . . . . .
H58A H 0.741931 -0.160187 0.103133 0.073 Uiso 1 1 calc R U . . .
H58B H 0.629842 -0.170964 0.148336 0.073 Uiso 1 1 calc R U . . .
C59 C 0.6105(19) -0.1420(18) 0.0659(11) 0.064(6) Uani 1 1 d . . . . .
H59A H 0.610128 -0.212164 0.061066 0.076 Uiso 1 1 calc R U . . .
H59B H 0.534088 -0.117694 0.075432 0.076 Uiso 1 1 calc R U . . .
C60 C 0.6226(19) -0.1058(16) -0.0354(10) 0.056(5) Uani 1 1 d . . . . .
H60A H 0.546003 -0.081238 -0.031430 0.067 Uiso 1 1 calc R U . . .
H60B H 0.623744 -0.177548 -0.035886 0.067 Uiso 1 1 calc R U . . .
C61 C 0.6872(18) -0.0577(16) -0.0902(10) 0.051(5) Uani 1 1 d . . . . .
H61A H 0.764289 -0.080492 -0.093594 0.062 Uiso 1 1 calc R U . . .
H61B H 0.659634 -0.075819 -0.123237 0.062 Uiso 1 1 calc R U . . .
C62 C 0.744(2) 0.0943(18) -0.1434(10) 0.063(6) Uani 1 1 d . . . . .
H62A H 0.721169 0.075159 -0.177386 0.076 Uiso 1 1 calc R U . . .
H62B H 0.821881 0.073685 -0.144955 0.076 Uiso 1 1 calc R U . . .
C63 C 0.732(2) 0.2037(17) -0.1445(10) 0.059(5) Uani 1 1 d . . . . .
H63A H 0.765087 0.235596 -0.183479 0.070 Uiso 1 1 calc R U . . .
H63B H 0.653131 0.221891 -0.138082 0.070 Uiso 1 1 calc R U . . .


_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 O4 1.824(15) . ?
U1 O3 1.865(16) . ?
U1 O1 2.368(15) . ?
U1 O2 2.381(14) . ?
U1 N3 2.630(18) . ?
U1 N1 2.673(18) . ?
U1 N2 2.701(16) . ?
K1 O7 2.702(15) . ?
K1 O9 2.823(19) . ?
K1 O3 2.830(16) . ?
K1 O8 2.839(15) . ?
K1 N5 2.98(2) . ?
K1 O11 3.001(19) . ?
K1 O6 3.07(2) . ?
K1 O10 3.11(2) . ?
K1 N6 3.14(3) . ?
K1 C30 3.53(2) . ?
O1 C1 1.34(3) . ?
O2 C18 1.28(2) . ?
O5 C23 1.23(2) . ?
O6 C29 1.36(3) . ?
O6 C30 1.43(3) . ?
O7 C31 1.43(3) . ?
O7 C32 1.44(3) . ?
O8 C36 1.37(3) . ?
O8 C35 1.41(3) . ?
O9 C38 1.38(3) . ?
O9 C37 1.42(3) . ?
O10 C42 1.42(4) . ?
O10 C41 1.43(4) . ?
O11 C44 1.34(4) . ?
O11 C43 1.45(4) . ?
N1 C7 1.33(3) . ?
N1 C8 1.50(3) . ?
N2 C9 1.51(3) . ?
N2 C10 1.52(3) . ?
N2 C19 1.53(3) . ?
N3 C12 1.22(3) . ?
N3 C11 1.55(3) . ?
N4 C21 1.29(3) . ?
N4 C20 1.46(3) . ?
N5 C33 1.44(4) . ?
N5 C39 1.46(3) . ?
N5 C45 1.51(4) . ?
N6 C40 1.46(4) . ?
N6 C28 1.46(4) . ?
N6 C34 1.47(4) . ?
C1 C2 1.37(3) . ?
C1 C6 1.44(3) . ?
C2 C3 1.39(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.35(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.37(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.40(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.51(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.49(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.51(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.49(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.41(3) . ?
C13 C18 1.47(3) . ?
C14 C15 1.35(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.43(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.36(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.45(3) . ?
C17 H17 0.9500 . ?
C19 C20 1.55(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.50(3) . ?
C21 H21 0.9500 . ?
C22 C27 1.43(3) . ?
C22 C23 1.48(3) . ?
C23 C24 1.48(3) . ?
C24 C25 1.41(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.39(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.36(3) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.40(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.50(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.46(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.50(4) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.48(4) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.59(4) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.43(5) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.49(5) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.53(5) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
K2 O13 2.805(14) . ?
K2 O15 2.814(13) . ?
K2 O12 2.820(14) . ?
K2 O16 2.835(14) . ?
K2 O14 2.838(14) . ?
K2 O17 2.944(13) . ?
K2 N7 3.021(17) . ?
K2 N8 3.059(17) . ?
O12 C47 1.42(2) . ?
O12 C48 1.48(2) . ?
O13 C49 1.44(3) . ?
O13 C50 1.45(3) . ?
O14 C54 1.37(2) . ?
O14 C53 1.44(3) . ?
O15 C56 1.41(2) . ?
O15 C55 1.44(2) . ?
O16 C60 1.43(3) . ?
O16 C59 1.46(3) . ?
O17 C62 1.43(3) . ?
O17 C61 1.44(2) . ?
N7 C46 1.44(3) . ?
N7 C52 1.46(3) . ?
N7 C58 1.54(3) . ?
N8 C51 1.45(3) . ?
N8 C57 1.46(3) . ?
N8 C63 1.48(3) . ?
C46 C47 1.50(3) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.50(3) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.55(3) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53 1.53(3) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.50(3) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 C57 1.53(3) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 C59 1.47(3) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 C61 1.48(3) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 C63 1.50(3) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?

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 O3 173.7(6) . . ?
O4 U1 O1 90.4(6) . . ?
O3 U1 O1 94.4(6) . . ?
O4 U1 O2 90.0(6) . . ?
O3 U1 O2 94.3(6) . . ?
O1 U1 O2 86.7(5) . . ?
O4 U1 N3 91.6(6) . . ?
O3 U1 N3 85.7(6) . . ?
O1 U1 N3 155.1(5) . . ?
O2 U1 N3 68.5(5) . . ?
O4 U1 N1 90.0(6) . . ?
O3 U1 N1 87.7(6) . . ?
O1 U1 N1 71.2(5) . . ?
O2 U1 N1 157.9(5) . . ?
N3 U1 N1 133.5(6) . . ?
O4 U1 N2 89.1(5) . . ?
O3 U1 N2 84.6(5) . . ?
O1 U1 N2 137.2(5) . . ?
O2 U1 N2 136.1(5) . . ?
N3 U1 N2 67.6(5) . . ?
N1 U1 N2 66.0(5) . . ?
O7 K1 O9 119.6(6) . . ?
O7 K1 O3 76.0(5) . . ?
O9 K1 O3 85.0(5) . . ?
O7 K1 O8 154.9(5) . . ?
O9 K1 O8 60.6(6) . . ?
O3 K1 O8 79.1(4) . . ?
O7 K1 N5 61.5(6) . . ?
O9 K1 N5 62.7(6) . . ?
O3 K1 N5 92.3(6) . . ?
O8 K1 N5 123.1(6) . . ?
O7 K1 O11 90.7(6) . . ?
O9 K1 O11 81.4(6) . . ?
O3 K1 O11 153.1(7) . . ?
O8 K1 O11 113.3(5) . . ?
N5 K1 O11 60.8(7) . . ?
O7 K1 O6 60.1(5) . . ?
O9 K1 O6 176.7(5) . . ?
O3 K1 O6 91.7(5) . . ?
O8 K1 O6 118.2(6) . . ?
N5 K1 O6 118.3(5) . . ?
O11 K1 O6 101.9(6) . . ?
O7 K1 O10 123.7(5) . . ?
O9 K1 O10 101.5(6) . . ?
O3 K1 O10 148.7(6) . . ?
O8 K1 O10 77.8(6) . . ?
N5 K1 O10 118.0(7) . . ?
O11 K1 O10 57.5(7) . . ?
O6 K1 O10 80.9(6) . . ?
O7 K1 N6 115.8(6) . . ?
O9 K1 N6 122.5(6) . . ?
O3 K1 N6 94.2(6) . . ?
O8 K1 N6 62.9(6) . . ?
N5 K1 N6 172.1(7) . . ?
O11 K1 N6 112.7(7) . . ?
O6 K1 N6 57.0(6) . . ?
O10 K1 N6 56.4(7) . . ?
O7 K1 C30 42.4(6) . . ?
O9 K1 C30 154.0(6) . . ?
O3 K1 C30 72.8(5) . . ?
O8 K1 C30 125.7(6) . . ?
N5 K1 C30 103.9(6) . . ?
O11 K1 C30 112.7(6) . . ?
O6 K1 C30 23.7(5) . . ?
O10 K1 C30 104.5(6) . . ?
N6 K1 C30 73.7(7) . . ?
C1 O1 U1 143.4(14) . . ?
C18 O2 U1 142.9(15) . . ?
U1 O3 K1 160.0(7) . . ?
C29 O6 C30 115(2) . . ?
C29 O6 K1 116.8(18) . . ?
C30 O6 K1 96.5(14) . . ?
C31 O7 C32 112.3(18) . . ?
C31 O7 K1 122.4(14) . . ?
C32 O7 K1 124.9(14) . . ?
C36 O8 C35 113(2) . . ?
C36 O8 K1 112.9(15) . . ?
C35 O8 K1 112.5(16) . . ?
C38 O9 C37 112(2) . . ?
C38 O9 K1 103.0(13) . . ?
C37 O9 K1 108.7(16) . . ?
C42 O10 C41 113(3) . . ?
C42 O10 K1 113(2) . . ?
C41 O10 K1 108(2) . . ?
C44 O11 C43 112(3) . . ?
C44 O11 K1 114.2(18) . . ?
C43 O11 K1 111.8(19) . . ?
C7 N1 C8 115.4(18) . . ?
C7 N1 U1 129.5(15) . . ?
C8 N1 U1 114.6(13) . . ?
C9 N2 C10 108.3(16) . . ?
C9 N2 C19 112.8(16) . . ?
C10 N2 C19 112.1(16) . . ?
C9 N2 U1 104.7(12) . . ?
C10 N2 U1 107.7(12) . . ?
C19 N2 U1 110.9(11) . . ?
C12 N3 C11 110.7(19) . . ?
C12 N3 U1 133.3(16) . . ?
C11 N3 U1 115.0(12) . . ?
C21 N4 C20 112.6(19) . . ?
C33 N5 C39 114(2) . . ?
C33 N5 C45 110(2) . . ?
C39 N5 C45 112(2) . . ?
C33 N5 K1 102.4(16) . . ?
C39 N5 K1 111.0(16) . . ?
C45 N5 K1 107.1(19) . . ?
C40 N6 C28 121(3) . . ?
C40 N6 C34 107(3) . . ?
C28 N6 C34 118(3) . . ?
C40 N6 K1 112(2) . . ?
C28 N6 K1 96(2) . . ?
C34 N6 K1 99.6(19) . . ?
O1 C1 C2 121(2) . . ?
O1 C1 C6 124(2) . . ?
C2 C1 C6 115(2) . . ?
C1 C2 C3 122(2) . . ?
C1 C2 H2 119.0 . . ?
C3 C2 H2 119.0 . . ?
C4 C3 C2 122(2) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 119(2) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C4 C5 C6 120(2) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C5 C6 C1 121(2) . . ?
C5 C6 C7 115(2) . . ?
C1 C6 C7 123(2) . . ?
N1 C7 C6 128(2) . . ?
N1 C7 H7 116.0 . . ?
C6 C7 H7 116.0 . . ?
C9 C8 N1 112.3(18) . . ?
C9 C8 H8A 109.1 . . ?
N1 C8 H8A 109.1 . . ?
C9 C8 H8B 109.1 . . ?
N1 C8 H8B 109.1 . . ?
H8A C8 H8B 107.9 . . ?
C8 C9 N2 111.2(17) . . ?
C8 C9 H9A 109.4 . . ?
N2 C9 H9A 109.4 . . ?
C8 C9 H9B 109.4 . . ?
N2 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
C11 C10 N2 112.0(18) . . ?
C11 C10 H10A 109.2 . . ?
N2 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
N2 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C10 C11 N3 112.8(18) . . ?
C10 C11 H11A 109.0 . . ?
N3 C11 H11A 109.0 . . ?
C10 C11 H11B 109.0 . . ?
N3 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
N3 C12 C13 128(2) . . ?
N3 C12 H12 115.9 . . ?
C13 C12 H12 115.9 . . ?
C14 C13 C18 120(2) . . ?
C14 C13 C12 119(2) . . ?
C18 C13 C12 120.5(18) . . ?
C15 C14 C13 123(3) . . ?
C15 C14 H14 118.6 . . ?
C13 C14 H14 118.6 . . ?
C14 C15 C16 117(2) . . ?
C14 C15 H15 121.7 . . ?
C16 C15 H15 121.7 . . ?
C17 C16 C15 125(3) . . ?
C17 C16 H16 117.5 . . ?
C15 C16 H16 117.5 . . ?
C16 C17 C18 119(3) . . ?
C16 C17 H17 120.7 . . ?
C18 C17 H17 120.7 . . ?
O2 C18 C17 120(2) . . ?
O2 C18 C13 123(2) . . ?
C17 C18 C13 116(2) . . ?
N2 C19 C20 114.6(17) . . ?
N2 C19 H19A 108.6 . . ?
C20 C19 H19A 108.6 . . ?
N2 C19 H19B 108.6 . . ?
C20 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
N4 C20 C19 107.2(17) . . ?
N4 C20 H20A 110.3 . . ?
C19 C20 H20A 110.3 . . ?
N4 C20 H20B 110.3 . . ?
C19 C20 H20B 110.3 . . ?
H20A C20 H20B 108.5 . . ?
N4 C21 C22 122.2(19) . . ?
N4 C21 H21 118.9 . . ?
C22 C21 H21 118.9 . . ?
C27 C22 C23 121.9(19) . . ?
C27 C22 C21 121.2(19) . . ?
C23 C22 C21 116.3(18) . . ?
O5 C23 C22 125(2) . . ?
O5 C23 C24 121(2) . . ?
C22 C23 C24 113(2) . . ?
C25 C24 C23 121(2) . . ?
C25 C24 H24 119.5 . . ?
C23 C24 H24 119.5 . . ?
C26 C25 C24 122(2) . . ?
C26 C25 H25 119.0 . . ?
C24 C25 H25 119.0 . . ?
C27 C26 C25 120(2) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C26 C27 C22 121(2) . . ?
C26 C27 H27 119.4 . . ?
C22 C27 H27 119.4 . . ?
C29 C28 N6 117(3) . . ?
C29 C28 H28A 108.2 . . ?
N6 C28 H28A 108.2 . . ?
C29 C28 H28B 108.2 . . ?
N6 C28 H28B 108.2 . . ?
H28A C28 H28B 107.3 . . ?
O6 C29 C28 110(3) . . ?
O6 C29 H29A 109.7 . . ?
C28 C29 H29A 109.7 . . ?
O6 C29 H29B 109.7 . . ?
C28 C29 H29B 109.7 . . ?
H29A C29 H29B 108.2 . . ?
O6 C30 C31 112.5(19) . . ?
O6 C30 K1 59.8(12) . . ?
C31 C30 K1 83.4(14) . . ?
O6 C30 H30A 109.1 . . ?
C31 C30 H30A 109.1 . . ?
K1 C30 H30A 166.5 . . ?
O6 C30 H30B 109.1 . . ?
C31 C30 H30B 109.1 . . ?
K1 C30 H30B 71.5 . . ?
H30A C30 H30B 107.8 . . ?
O7 C31 C30 109(2) . . ?
O7 C31 H31A 109.9 . . ?
C30 C31 H31A 109.9 . . ?
O7 C31 H31B 109.9 . . ?
C30 C31 H31B 109.9 . . ?
H31A C31 H31B 108.3 . . ?
O7 C32 C33 108(2) . . ?
O7 C32 H32A 110.1 . . ?
C33 C32 H32A 110.1 . . ?
O7 C32 H32B 110.1 . . ?
C33 C32 H32B 110.1 . . ?
H32A C32 H32B 108.4 . . ?
N5 C33 C32 124(3) . . ?
N5 C33 H33A 106.4 . . ?
C32 C33 H33A 106.4 . . ?
N5 C33 H33B 106.4 . . ?
C32 C33 H33B 106.4 . . ?
H33A C33 H33B 106.5 . . ?
N6 C34 C35 119(3) . . ?
N6 C34 H34A 107.6 . . ?
C35 C34 H34A 107.6 . . ?
N6 C34 H34B 107.6 . . ?
C35 C34 H34B 107.6 . . ?
H34A C34 H34B 107.1 . . ?
O8 C35 C34 110(2) . . ?
O8 C35 H35A 109.7 . . ?
C34 C35 H35A 109.7 . . ?
O8 C35 H35B 109.7 . . ?
C34 C35 H35B 109.7 . . ?
H35A C35 H35B 108.2 . . ?
O8 C36 C37 106(2) . . ?
O8 C36 H36A 110.5 . . ?
C37 C36 H36A 110.5 . . ?
O8 C36 H36B 110.5 . . ?
C37 C36 H36B 110.5 . . ?
H36A C36 H36B 108.7 . . ?
O9 C37 C36 110(3) . . ?
O9 C37 H37A 109.6 . . ?
C36 C37 H37A 109.6 . . ?
O9 C37 H37B 109.6 . . ?
C36 C37 H37B 109.6 . . ?
H37A C37 H37B 108.1 . . ?
O9 C38 C39 115(2) . . ?
O9 C38 H38A 108.4 . . ?
C39 C38 H38A 108.4 . . ?
O9 C38 H38B 108.4 . . ?
C39 C38 H38B 108.4 . . ?
H38A C38 H38B 107.5 . . ?
N5 C39 C38 111(2) . . ?
N5 C39 H39A 109.4 . . ?
C38 C39 H39A 109.4 . . ?
N5 C39 H39B 109.4 . . ?
C38 C39 H39B 109.4 . . ?
H39A C39 H39B 108.0 . . ?
C41 C40 N6 120(4) . . ?
C41 C40 H40A 107.4 . . ?
N6 C40 H40A 107.4 . . ?
C41 C40 H40B 107.4 . . ?
N6 C40 H40B 107.4 . . ?
H40A C40 H40B 106.9 . . ?
C40 C41 O10 110(3) . . ?
C40 C41 H41A 109.7 . . ?
O10 C41 H41A 109.7 . . ?
C40 C41 H41B 109.7 . . ?
O10 C41 H41B 109.7 . . ?
H41A C41 H41B 108.2 . . ?
O10 C42 C43 114(3) . . ?
O10 C42 H42A 108.8 . . ?
C43 C42 H42A 108.8 . . ?
O10 C42 H42B 108.8 . . ?
C43 C42 H42B 108.8 . . ?
H42A C42 H42B 107.7 . . ?
O11 C43 C42 110(2) . . ?
O11 C43 H43A 109.8 . . ?
C42 C43 H43A 109.8 . . ?
O11 C43 H43B 109.8 . . ?
C42 C43 H43B 109.8 . . ?
H43A C43 H43B 108.2 . . ?
O11 C44 C45 110(3) . . ?
O11 C44 H44A 109.6 . . ?
C45 C44 H44A 109.6 . . ?
O11 C44 H44B 109.6 . . ?
C45 C44 H44B 109.6 . . ?
H44A C44 H44B 108.1 . . ?
N5 C45 C44 115(2) . . ?
N5 C45 H45A 108.6 . . ?
C44 C45 H45A 108.6 . . ?
N5 C45 H45B 108.6 . . ?
C44 C45 H45B 108.6 . . ?
H45A C45 H45B 107.5 . . ?
O13 K2 O15 92.1(4) . . ?
O13 K2 O12 60.2(4) . . ?
O15 K2 O12 114.7(4) . . ?
O13 K2 O16 124.7(4) . . ?
O15 K2 O16 138.9(4) . . ?
O12 K2 O16 100.7(4) . . ?
O13 K2 O14 128.9(4) . . ?
O15 K2 O14 60.2(4) . . ?
O12 K2 O14 91.5(4) . . ?
O16 K2 O14 100.4(4) . . ?
O13 K2 O17 102.0(4) . . ?
O15 K2 O17 99.4(4) . . ?
O12 K2 O17 141.0(4) . . ?
O16 K2 O17 58.9(4) . . ?
O14 K2 O17 123.1(4) . . ?
O13 K2 N7 119.2(5) . . ?
O15 K2 N7 119.9(5) . . ?
O12 K2 N7 59.6(4) . . ?
O16 K2 N7 61.1(5) . . ?
O14 K2 N7 60.3(4) . . ?
O17 K2 N7 119.2(5) . . ?
O13 K2 N8 61.6(4) . . ?
O15 K2 N8 60.0(4) . . ?
O12 K2 N8 121.1(4) . . ?
O16 K2 N8 118.5(5) . . ?
O14 K2 N8 119.4(4) . . ?
O17 K2 N8 60.2(4) . . ?
N7 K2 N8 179.2(5) . . ?
C47 O12 C48 111.2(14) . . ?
C47 O12 K2 116.3(11) . . ?
C48 O12 K2 117.2(11) . . ?
C49 O13 C50 109.9(16) . . ?
C49 O13 K2 114.5(12) . . ?
C50 O13 K2 118.8(11) . . ?
C54 O14 C53 112.0(16) . . ?
C54 O14 K2 110.9(12) . . ?
C53 O14 K2 117.8(11) . . ?
C56 O15 C55 113.2(14) . . ?
C56 O15 K2 115.7(10) . . ?
C55 O15 K2 116.1(11) . . ?
C60 O16 C59 110.7(16) . . ?
C60 O16 K2 118.3(12) . . ?
C59 O16 K2 119.7(13) . . ?
C62 O17 C61 110.6(15) . . ?
C62 O17 K2 112.8(12) . . ?
C61 O17 K2 112.0(11) . . ?
C46 N7 C52 112.7(18) . . ?
C46 N7 C58 108.9(16) . . ?
C52 N7 C58 106.1(17) . . ?
C46 N7 K2 112.4(13) . . ?
C52 N7 K2 108.5(12) . . ?
C58 N7 K2 108.0(12) . . ?
C51 N8 C57 110.6(17) . . ?
C51 N8 C63 110.8(18) . . ?
C57 N8 C63 111.4(17) . . ?
C51 N8 K2 105.6(12) . . ?
C57 N8 K2 109.4(12) . . ?
C63 N8 K2 108.8(12) . . ?
N7 C46 C47 113.4(18) . . ?
N7 C46 H46A 108.9 . . ?
C47 C46 H46A 108.9 . . ?
N7 C46 H46B 108.9 . . ?
C47 C46 H46B 108.9 . . ?
H46A C46 H46B 107.7 . . ?
O12 C47 C46 111.4(16) . . ?
O12 C47 H47A 109.4 . . ?
C46 C47 H47A 109.4 . . ?
O12 C47 H47B 109.4 . . ?
C46 C47 H47B 109.4 . . ?
H47A C47 H47B 108.0 . . ?
O12 C48 C49 107.0(16) . . ?
O12 C48 H48A 110.3 . . ?
C49 C48 H48A 110.3 . . ?
O12 C48 H48B 110.3 . . ?
C49 C48 H48B 110.3 . . ?
H48A C48 H48B 108.6 . . ?
O13 C49 C48 109.6(17) . . ?
O13 C49 H49A 109.8 . . ?
C48 C49 H49A 109.8 . . ?
O13 C49 H49B 109.8 . . ?
C48 C49 H49B 109.8 . . ?
H49A C49 H49B 108.2 . . ?
O13 C50 C51 107.8(18) . . ?
O13 C50 H50A 110.2 . . ?
C51 C50 H50A 110.2 . . ?
O13 C50 H50B 110.2 . . ?
C51 C50 H50B 110.2 . . ?
H50A C50 H50B 108.5 . . ?
N8 C51 C50 116.5(19) . . ?
N8 C51 H51A 108.2 . . ?
C50 C51 H51A 108.2 . . ?
N8 C51 H51B 108.2 . . ?
C50 C51 H51B 108.2 . . ?
H51A C51 H51B 107.3 . . ?
N7 C52 C53 110.9(18) . . ?
N7 C52 H52A 109.4 . . ?
C53 C52 H52A 109.4 . . ?
N7 C52 H52B 109.4 . . ?
C53 C52 H52B 109.4 . . ?
H52A C52 H52B 108.0 . . ?
O14 C53 C52 109.4(18) . . ?
O14 C53 H53A 109.8 . . ?
C52 C53 H53A 109.8 . . ?
O14 C53 H53B 109.8 . . ?
C52 C53 H53B 109.8 . . ?
H53A C53 H53B 108.2 . . ?
O14 C54 C55 110.5(17) . . ?
O14 C54 H54A 109.5 . . ?
C55 C54 H54A 109.5 . . ?
O14 C54 H54B 109.5 . . ?
C55 C54 H54B 109.5 . . ?
H54A C54 H54B 108.1 . . ?
O15 C55 C54 109.1(16) . . ?
O15 C55 H55A 109.9 . . ?
C54 C55 H55A 109.9 . . ?
O15 C55 H55B 109.9 . . ?
C54 C55 H55B 109.9 . . ?
H55A C55 H55B 108.3 . . ?
O15 C56 C57 108.6(16) . . ?
O15 C56 H56A 110.0 . . ?
C57 C56 H56A 110.0 . . ?
O15 C56 H56B 110.0 . . ?
C57 C56 H56B 110.0 . . ?
H56A C56 H56B 108.3 . . ?
N8 C57 C56 112.4(17) . . ?
N8 C57 H57A 109.1 . . ?
C56 C57 H57A 109.1 . . ?
N8 C57 H57B 109.1 . . ?
C56 C57 H57B 109.1 . . ?
H57A C57 H57B 107.9 . . ?
C59 C58 N7 117.5(19) . . ?
C59 C58 H58A 107.9 . . ?
N7 C58 H58A 107.9 . . ?
C59 C58 H58B 107.9 . . ?
N7 C58 H58B 107.9 . . ?
H58A C58 H58B 107.2 . . ?
O16 C59 C58 109.1(19) . . ?
O16 C59 H59A 109.9 . . ?
C58 C59 H59A 109.9 . . ?
O16 C59 H59B 109.9 . . ?
C58 C59 H59B 109.9 . . ?
H59A C59 H59B 108.3 . . ?
O16 C60 C61 110.5(17) . . ?
O16 C60 H60A 109.6 . . ?
C61 C60 H60A 109.6 . . ?
O16 C60 H60B 109.6 . . ?
C61 C60 H60B 109.6 . . ?
H60A C60 H60B 108.1 . . ?
O17 C61 C60 110.0(17) . . ?
O17 C61 H61A 109.7 . . ?
C60 C61 H61A 109.7 . . ?
O17 C61 H61B 109.7 . . ?
C60 C61 H61B 109.7 . . ?
H61A C61 H61B 108.2 . . ?
O17 C62 C63 109.4(18) . . ?
O17 C62 H62A 109.8 . . ?
C63 C62 H62A 109.8 . . ?
O17 C62 H62B 109.8 . . ?
C63 C62 H62B 109.8 . . ?
H62A C62 H62B 108.3 . . ?
N8 C63 C62 114.9(19) . . ?
N8 C63 H63A 108.5 . . ?
C62 C63 H63A 108.5 . . ?
N8 C63 H63B 108.5 . . ?
C62 C63 H63B 108.5 . . ?
H63A C63 H63B 107.5 . . ?

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
O1 U1 O3 K1 37(2) . . . . ?
O2 U1 O3 K1 -50(2) . . . . ?
N3 U1 O3 K1 -118(2) . . . . ?
N1 U1 O3 K1 108(2) . . . . ?
N2 U1 O3 K1 174(2) . . . . ?
U1 O1 C1 C2 172(2) . . . . ?
U1 O1 C1 C6 -6(5) . . . . ?
O1 C1 C2 C3 179(3) . . . . ?
C6 C1 C2 C3 -2(4) . . . . ?
C1 C2 C3 C4 -4(4) . . . . ?
C2 C3 C4 C5 9(4) . . . . ?
C3 C4 C5 C6 -8(4) . . . . ?
C4 C5 C6 C1 2(4) . . . . ?
C4 C5 C6 C7 -172(2) . . . . ?
O1 C1 C6 C5 -179(3) . . . . ?
C2 C1 C6 C5 3(4) . . . . ?
O1 C1 C6 C7 -5(4) . . . . ?
C2 C1 C6 C7 177(2) . . . . ?
C8 N1 C7 C6 180(2) . . . . ?
U1 N1 C7 C6 -8(4) . . . . ?
C5 C6 C7 N1 -174(2) . . . . ?
C1 C6 C7 N1 12(4) . . . . ?
C7 N1 C8 C9 153(2) . . . . ?
U1 N1 C8 C9 -20(2) . . . . ?
N1 C8 C9 N2 57(2) . . . . ?
C10 N2 C9 C8 -176.0(18) . . . . ?
C19 N2 C9 C8 59(2) . . . . ?
U1 N2 C9 C8 -61.3(18) . . . . ?
C9 N2 C10 C11 166.4(18) . . . . ?
C19 N2 C10 C11 -69(2) . . . . ?
U1 N2 C10 C11 54(2) . . . . ?
N2 C10 C11 N3 -54(2) . . . . ?
C12 N3 C11 C10 -165.8(19) . . . . ?
U1 N3 C11 C10 24(2) . . . . ?
C11 N3 C12 C13 -178.7(19) . . . . ?
U1 N3 C12 C13 -11(3) . . . . ?
N3 C12 C13 C14 178(2) . . . . ?
N3 C12 C13 C18 5(3) . . . . ?
C18 C13 C14 C15 -1(4) . . . . ?
C12 C13 C14 C15 -175(2) . . . . ?
C13 C14 C15 C16 3(4) . . . . ?
C14 C15 C16 C17 -7(4) . . . . ?
C15 C16 C17 C18 7(4) . . . . ?
U1 O2 C18 C17 -159.2(17) . . . . ?
U1 O2 C18 C13 25(4) . . . . ?
C16 C17 C18 O2 179(2) . . . . ?
C16 C17 C18 C13 -5(3) . . . . ?
C14 C13 C18 O2 178(2) . . . . ?
C12 C13 C18 O2 -9(3) . . . . ?
C14 C13 C18 C17 2(3) . . . . ?
C12 C13 C18 C17 175.1(18) . . . . ?
C9 N2 C19 C20 57(2) . . . . ?
C10 N2 C19 C20 -66(2) . . . . ?
U1 N2 C19 C20 173.6(15) . . . . ?
C21 N4 C20 C19 -133.6(19) . . . . ?
N2 C19 C20 N4 178.2(17) . . . . ?
C20 N4 C21 C22 177.2(17) . . . . ?
N4 C21 C22 C27 -1(3) . . . . ?
N4 C21 C22 C23 170.6(18) . . . . ?
C27 C22 C23 O5 176.1(18) . . . . ?
C21 C22 C23 O5 5(3) . . . . ?
C27 C22 C23 C24 -7(2) . . . . ?
C21 C22 C23 C24 -178.9(15) . . . . ?
O5 C23 C24 C25 -178.6(19) . . . . ?
C22 C23 C24 C25 5(3) . . . . ?
C23 C24 C25 C26 1(3) . . . . ?
C24 C25 C26 C27 -4(3) . . . . ?
C25 C26 C27 C22 2(3) . . . . ?
C23 C22 C27 C26 4(3) . . . . ?
C21 C22 C27 C26 175.6(17) . . . . ?
C40 N6 C28 C29 46(5) . . . . ?
C34 N6 C28 C29 -178(3) . . . . ?
K1 N6 C28 C29 -74(4) . . . . ?
C30 O6 C29 C28 89(3) . . . . ?
K1 O6 C29 C28 -23(3) . . . . ?
N6 C28 C29 O6 74(4) . . . . ?
C29 O6 C30 C31 169(3) . . . . ?
K1 O6 C30 C31 -67(2) . . . . ?
C29 O6 C30 K1 -124(2) . . . . ?
C32 O7 C31 C30 166(2) . . . . ?
K1 O7 C31 C30 -21(2) . . . . ?
O6 C30 C31 O7 67(3) . . . . ?
K1 C30 C31 O7 13.3(16) . . . . ?
C31 O7 C32 C33 -171(2) . . . . ?
K1 O7 C32 C33 16(3) . . . . ?
C39 N5 C33 C32 171(3) . . . . ?
C45 N5 C33 C32 -63(4) . . . . ?
K1 N5 C33 C32 51(3) . . . . ?
O7 C32 C33 N5 -49(4) . . . . ?
C40 N6 C34 C35 -70(4) . . . . ?
C28 N6 C34 C35 149(3) . . . . ?
K1 N6 C34 C35 47(3) . . . . ?
C36 O8 C35 C34 -177(2) . . . . ?
K1 O8 C35 C34 54(3) . . . . ?
N6 C34 C35 O8 -76(4) . . . . ?
C35 O8 C36 C37 179(2) . . . . ?
K1 O8 C36 C37 -52(3) . . . . ?
C38 O9 C37 C36 -168(2) . . . . ?
K1 O9 C37 C36 -55(2) . . . . ?
O8 C36 C37 O9 75(3) . . . . ?
C37 O9 C38 C39 -174(2) . . . . ?
K1 O9 C38 C39 69(2) . . . . ?
C33 N5 C39 C38 -99(3) . . . . ?
C45 N5 C39 C38 135(3) . . . . ?
K1 N5 C39 C38 16(3) . . . . ?
O9 C38 C39 N5 -62(3) . . . . ?
C28 N6 C40 C41 -91(5) . . . . ?
C34 N6 C40 C41 129(4) . . . . ?
K1 N6 C40 C41 21(5) . . . . ?
N6 C40 C41 O10 -61(5) . . . . ?
C42 O10 C41 C40 -169(3) . . . . ?
K1 O10 C41 C40 65(4) . . . . ?
C41 O10 C42 C43 -160(3) . . . . ?
K1 O10 C42 C43 -37(3) . . . . ?
C44 O11 C43 C42 170(3) . . . . ?
K1 O11 C43 C42 -60(3) . . . . ?
O10 C42 C43 O11 67(3) . . . . ?
C43 O11 C44 C45 176(2) . . . . ?
K1 O11 C44 C45 47(3) . . . . ?
C33 N5 C45 C44 160(3) . . . . ?
C39 N5 C45 C44 -72(4) . . . . ?
K1 N5 C45 C44 49(3) . . . . ?
O11 C44 C45 N5 -70(4) . . . . ?
C52 N7 C46 C47 -157.8(18) . . . . ?
C58 N7 C46 C47 85(2) . . . . ?
K2 N7 C46 C47 -35(2) . . . . ?
C48 O12 C47 C46 169.1(17) . . . . ?
K2 O12 C47 C46 -53(2) . . . . ?
N7 C46 C47 O12 60(2) . . . . ?
C47 O12 C48 C49 179.3(17) . . . . ?
K2 O12 C48 C49 42(2) . . . . ?
C50 O13 C49 C48 -169.1(17) . . . . ?
K2 O13 C49 C48 54(2) . . . . ?
O12 C48 C49 O13 -63(2) . . . . ?
C49 O13 C50 C51 -179.8(17) . . . . ?
K2 O13 C50 C51 -45.3(19) . . . . ?
C57 N8 C51 C50 70(2) . . . . ?
C63 N8 C51 C50 -165.6(18) . . . . ?
K2 N8 C51 C50 -48(2) . . . . ?
O13 C50 C51 N8 65(2) . . . . ?
C46 N7 C52 C53 73(2) . . . . ?
C58 N7 C52 C53 -167.6(18) . . . . ?
K2 N7 C52 C53 -52(2) . . . . ?
C54 O14 C53 C52 -175.9(17) . . . . ?
K2 O14 C53 C52 -46(2) . . . . ?
N7 C52 C53 O14 67(2) . . . . ?
C53 O14 C54 C55 -168.0(17) . . . . ?
K2 O14 C54 C55 58.2(17) . . . . ?
C56 O15 C55 C54 174.6(16) . . . . ?
K2 O15 C55 C54 37.3(19) . . . . ?
O14 C54 C55 O15 -65(2) . . . . ?
C55 O15 C56 C57 163.9(16) . . . . ?
K2 O15 C56 C57 -58.6(18) . . . . ?
C51 N8 C57 C56 -155.0(18) . . . . ?
C63 N8 C57 C56 81(2) . . . . ?
K2 N8 C57 C56 -39(2) . . . . ?
O15 C56 C57 N8 67(2) . . . . ?
C46 N7 C58 C59 -164(2) . . . . ?
C52 N7 C58 C59 75(2) . . . . ?
K2 N7 C58 C59 -41(2) . . . . ?
C60 O16 C59 C58 171.7(19) . . . . ?
K2 O16 C59 C58 -45(2) . . . . ?
N7 C58 C59 O16 59(3) . . . . ?
C59 O16 C60 C61 -173.5(18) . . . . ?
K2 O16 C60 C61 43(2) . . . . ?
C62 O17 C61 C60 178.1(18) . . . . ?
K2 O17 C61 C60 51.2(18) . . . . ?
O16 C60 C61 O17 -63(2) . . . . ?
C61 O17 C62 C63 178.0(18) . . . . ?
K2 O17 C62 C63 -56(2) . . . . ?
C51 N8 C63 C62 74(2) . . . . ?
C57 N8 C63 C62 -162.8(19) . . . . ?
K2 N8 C63 C62 -42(2) . . . . ?
O17 C62 C63 N8 69(3) . . . . ?

_refine_diff_density_max         2.396
_refine_diff_density_min         -2.432
_refine_diff_density_rms         0.276





_publcif_funding_html            
;
;
####################################################################### 
# 
# 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_sw76
_database_code_depnum_ccdc_archive 'CCDC 1842381'
_audit_update_record             
;
2018-05-09 deposited with the CCDC.
2018-08-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C99 H99 Fe3 N17 O10 U2, 2(I)'
_chemical_formula_sum            'C99 H99 Fe3 I2 N17 O10 U2'
_chemical_formula_weight         2584.36

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'
N N 0.0311 0.0180 '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'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.7743(3)
_cell_length_b                   21.1783(4)
_cell_length_c                   24.4520(5)
_cell_angle_alpha                99.7615(17)
_cell_angle_beta                 95.7326(16)
_cell_angle_gamma                98.8026(16)
_cell_volume                     6888.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    140.00(10)
_cell_measurement_reflns_used    27599
_cell_measurement_theta_min      3.8820
_cell_measurement_theta_max      75.8220

_exptl_crystal_description       plate
_exptl_crystal_colour            'clear intense red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_F_000             2520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.087
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
8 5 -5 0.1452
1 -13 7 0.1093
-9 5 0 0.1870
-2 13 -7 0.1053
9 -4 0 0.1377
0 0 -16 0.0361
-9 4 0 0.1918
0 0 16 0.0492
0 -13 0 0.0897
-6 -8 0 0.1603
-2 12 5 0.1172
_exptl_absorpt_coefficient_mu    12.901
_shelx_estimated_absorpt_T_min   0.093
_shelx_estimated_absorpt_T_max   0.400
_exptl_absorpt_correction_T_min  0.503
_exptl_absorpt_correction_T_max  0.816
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      140.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 5.1333
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     22.00  64.00   1.00    1.82    --   42.26  37.00 -90.00   42
  2  ω    126.00 163.00   1.00    7.28    --  110.51  61.00-150.00   37
  3  ω     84.00 175.00   1.00    7.28    --  110.51  30.00-180.00   91
  4  ω     92.00 134.00   1.00    7.28    --  110.51 -45.00-120.00   42
  5  ω     85.00 163.00   1.00    7.28    --  110.51  30.00 -90.00   78
  6  ω     81.00 122.00   1.00    7.28    --  110.51  61.00-150.00   41
  7  ω     37.00  65.00   1.00    7.28    --  110.51 -45.00-120.00   28
  8  ω     38.00 120.00   1.00    7.28    --  110.51-125.00   0.00   82
  9  ω     97.00 122.00   1.00    7.28    --  110.51-127.00 -88.00   25
 10  ω     63.00 134.00   1.00    7.28    --  110.51 -61.00  60.00   71
 11  ω     66.00 140.00   1.00    7.28    --  110.51 -77.00 150.00   74
 12  ω     85.00 178.00   1.00    7.28    --  110.51  45.00 120.00   93
 13  ω    105.00 175.00   1.00    7.28    --  110.51 143.00 157.00   70
 14  ω     39.00  81.00   1.00    1.82    --   42.26 -99.00   0.00   42
 15  ω     30.00 108.00   1.00    7.28    --  110.51 -94.00  90.00   78
 16  ω     49.00  91.00   1.00    7.28    --  110.51-125.00  60.00   42
 17  ω      1.00  51.00   1.00    1.82    --   42.26 -99.00 -60.00   50
 18  ω    -95.00  -8.00   1.00    1.82    --  -42.26 125.00 120.00   87
 19  ω   -112.00 -17.00   1.00    1.82    --  -42.26 -77.00   0.00   95
 20  ω   -117.00 -26.00   1.00    1.82    --  -42.26 -37.00  60.00   91
;
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            53233
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.274
_diffrn_reflns_theta_max         76.188
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             27994
_reflns_number_gt                24816
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 3.10 (CCDC, 2017)'
_computing_publication_material  'CIFTab (Sheldrick, 2015)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0864P)²+23.0602P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       ?
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         27994
_refine_ls_number_parameters     1199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0558
_refine_ls_wR_factor_ref         0.1480
_refine_ls_wR_factor_gt          0.1438
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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 -0.01808(2) 0.26830(2) 0.20266(2) 0.01789(6) Uani 1 1 d . . . . .
U2 U 0.16915(2) 0.60921(2) 0.21986(2) 0.01901(6) Uani 1 1 d . . . . .
Fe1 Fe -0.13752(7) 0.08300(4) 0.14311(4) 0.02129(18) Uani 1 1 d . . . . .
Fe2 Fe 0.06072(7) 0.45285(4) 0.26569(4) 0.02007(18) Uani 1 1 d . . . . .
Fe3 Fe 0.21921(7) 0.76484(4) 0.14952(4) 0.02096(18) Uani 1 1 d . . . . .
O1 O -0.2051(4) -0.0083(2) 0.1082(2) 0.0310(10) Uani 1 1 d . . . . .
O2 O -0.0681(3) 0.17746(19) 0.17565(17) 0.0209(8) Uani 1 1 d . . . . .
O3 O -0.1083(4) 0.2665(2) 0.27484(19) 0.0304(10) Uani 1 1 d . . . . .
O4 O 0.1099(3) 0.2434(2) 0.25523(19) 0.0253(9) Uani 1 1 d . . . . .
O5 O 0.0252(3) 0.3613(2) 0.2253(2) 0.0265(9) Uani 1 1 d . . . . .
O6 O 0.1331(3) 0.5398(2) 0.25973(19) 0.0263(9) Uani 1 1 d . . . . .
O7 O 0.0173(3) 0.6346(2) 0.2254(2) 0.0269(9) Uani 1 1 d . . . . .
O8 O 0.1200(3) 0.5403(2) 0.13743(18) 0.0256(9) Uani 1 1 d . . . . .
O9 O 0.1943(3) 0.6801(2) 0.18027(18) 0.0265(9) Uani 1 1 d . . . . .
O10 O 0.2487(3) 0.8492(2) 0.1220(2) 0.0283(9) Uani 1 1 d . . . . .
N1 N -0.1770(5) 0.0708(3) 0.2266(2) 0.0306(12) Uani 1 1 d . . . . .
N2 N 0.0039(4) 0.0464(3) 0.1661(2) 0.0270(11) Uani 1 1 d . . . . .
N3 N -0.2831(4) 0.1155(2) 0.1193(2) 0.0235(10) Uani 1 1 d . . . . .
N4 N -0.0930(4) 0.0893(3) 0.0618(2) 0.0261(11) Uani 1 1 d . . . . .
N5 N 0.1388(4) 0.2811(3) 0.1534(3) 0.0368(14) Uani 1 1 d . . . . .
N6 N -0.0478(4) 0.2691(3) 0.0908(2) 0.0289(11) Uani 1 1 d . . . . .
N7 N -0.1872(4) 0.2946(2) 0.1718(2) 0.0237(10) Uani 1 1 d . . . . .
N8 N 0.2056(4) 0.4373(3) 0.3034(3) 0.0312(12) Uani 1 1 d . . . . .
N9 N 0.0073(4) 0.4666(3) 0.3444(2) 0.0276(11) Uani 1 1 d . . . . .
N10 N -0.0827(4) 0.4704(3) 0.2235(2) 0.0269(11) Uani 1 1 d . . . . .
N11 N 0.1727(4) 0.6816(3) 0.3155(2) 0.0275(11) Uani 1 1 d . . . . .
N12 N 0.3566(4) 0.6619(3) 0.2712(2) 0.0284(11) Uani 1 1 d . . . . .
N13 N 0.3050(4) 0.5412(3) 0.1955(2) 0.0232(10) Uani 1 1 d . . . . .
N14 N 0.3771(4) 0.7768(3) 0.1736(2) 0.0242(10) Uani 1 1 d . . . . .
N15 N 0.2483(4) 0.7064(3) 0.0688(2) 0.0237(10) Uani 1 1 d . . . . .
N16 N 0.0605(4) 0.7586(3) 0.1171(2) 0.0243(10) Uani 1 1 d . . . . .
N17 N 0.1956(4) 0.8207(3) 0.2327(2) 0.0279(11) Uani 1 1 d . . . . .
C1 C -0.2130(5) -0.0424(3) 0.0579(3) 0.0285(13) Uani 1 1 d . . . . .
C2 C -0.2718(5) -0.1062(3) 0.0457(3) 0.0318(14) Uani 1 1 d . . . . .
H2 H -0.304377 -0.122597 0.074170 0.038 Uiso 1 1 calc R U . . .
C3 C -0.2815(5) -0.1442(3) -0.0074(4) 0.0388(18) Uani 1 1 d . . . . .
H3 H -0.323792 -0.185355 -0.015414 0.047 Uiso 1 1 calc R U . . .
C4 C -0.2314(6) -0.1233(4) -0.0480(4) 0.049(2) Uani 1 1 d . . . . .
H4 H -0.235167 -0.151136 -0.083265 0.058 Uiso 1 1 calc R U . . .
C5 C -0.1753(6) -0.0619(4) -0.0381(3) 0.0391(16) Uani 1 1 d . . . . .
H5 H -0.143593 -0.047034 -0.067424 0.047 Uiso 1 1 calc R U . . .
C6 C -0.1639(5) -0.0210(3) 0.0141(3) 0.0311(14) Uani 1 1 d . . . . .
C7 C -0.1053(5) 0.0432(3) 0.0195(3) 0.0280(13) Uani 1 1 d . . . . .
H7 H -0.072811 0.051807 -0.011664 0.034 Uiso 1 1 calc R U . . .
C8 C -0.0327(5) 0.1513(3) 0.0571(3) 0.0259(12) Uani 1 1 d . . . . .
H8A H -0.002374 0.145519 0.021892 0.031 Uiso 1 1 calc R U . . .
H8B H 0.021518 0.164259 0.088681 0.031 Uiso 1 1 calc R U . . .
C9 C -0.0953(5) 0.2052(3) 0.0574(3) 0.0293(13) Uani 1 1 d . . . . .
H9A H -0.112515 0.210381 0.018272 0.035 Uiso 1 1 calc R U . . .
H9B H -0.157985 0.191108 0.071956 0.035 Uiso 1 1 calc R U . . .
C10 C 0.0459(6) 0.2920(5) 0.0675(4) 0.046(2) Uani 1 1 d . . . . .
H10A H 0.066262 0.254245 0.044594 0.055 Uiso 1 1 calc R U . . .
H10B H 0.032419 0.322909 0.042699 0.055 Uiso 1 1 calc R U . . .
C11 C 0.1251(7) 0.3229(4) 0.1102(4) 0.0466(19) Uani 1 1 d . . . . .
H11A H 0.110844 0.365338 0.128367 0.056 Uiso 1 1 calc R U . . .
H11B H 0.187118 0.331151 0.093242 0.056 Uiso 1 1 calc R U . . .
C12 C 0.2253(5) 0.2675(4) 0.1660(3) 0.0347(16) Uani 1 1 d . . . . .
H12 H 0.273135 0.277000 0.141812 0.042 Uiso 1 1 calc R U . . .
C13 C 0.2566(5) 0.2396(3) 0.2124(3) 0.0336(15) Uani 1 1 d . . . . .
C14 C 0.3553(6) 0.2263(4) 0.2153(4) 0.046(2) Uani 1 1 d . . . . .
H14 H 0.393862 0.234092 0.186233 0.055 Uiso 1 1 calc R U . . .
C15 C 0.3947(7) 0.2026(5) 0.2592(5) 0.059(3) Uani 1 1 d . . . . .
H15 H 0.460591 0.193995 0.261126 0.070 Uiso 1 1 calc R U . . .
C16 C 0.3376(7) 0.1912(5) 0.3008(4) 0.055(2) Uani 1 1 d . . . . .
H16 H 0.364751 0.173436 0.330888 0.066 Uiso 1 1 calc R U . . .
C17 C 0.2424(6) 0.2045(5) 0.3007(4) 0.048(2) Uani 1 1 d . . . . .
H17 H 0.206000 0.196329 0.330494 0.058 Uiso 1 1 calc R U . . .
C18 C 0.1981(5) 0.2306(3) 0.2556(3) 0.0322(14) Uani 1 1 d . . . . .
C19 C -0.1140(5) 0.3172(3) 0.0872(3) 0.0268(12) Uani 1 1 d . . . . .
H19A H -0.131985 0.319060 0.047327 0.032 Uiso 1 1 calc R U . . .
H19B H -0.077945 0.360650 0.106220 0.032 Uiso 1 1 calc R U . . .
C20 C -0.2073(5) 0.3016(3) 0.1131(3) 0.0294(13) Uani 1 1 d . . . . .
H20A H -0.246808 0.336622 0.111123 0.035 Uiso 1 1 calc R U . . .
H20B H -0.247329 0.260573 0.091256 0.035 Uiso 1 1 calc R U . . .
C21 C -0.2590(4) 0.3043(3) 0.2000(3) 0.0260(12) Uani 1 1 d . . . . .
H21 H -0.313769 0.317565 0.181049 0.031 Uiso 1 1 calc R U . . .
C22 C -0.2660(5) 0.2975(3) 0.2572(3) 0.0301(14) Uani 1 1 d . . . . .
C23 C -0.3542(6) 0.3102(4) 0.2792(4) 0.0407(17) Uani 1 1 d . . . . .
H23 H -0.404258 0.322654 0.255802 0.049 Uiso 1 1 calc R U . . .
C24 C -0.3699(6) 0.3051(4) 0.3327(4) 0.0416(17) Uani 1 1 d . . . . .
H24 H -0.428818 0.315123 0.346617 0.050 Uiso 1 1 calc R U . . .
C25 C -0.2957(5) 0.2844(4) 0.3671(3) 0.0401(18) Uani 1 1 d . . . . .
H25 H -0.305711 0.279708 0.404223 0.048 Uiso 1 1 calc R U . . .
C26 C -0.2100(6) 0.2713(4) 0.3470(3) 0.0351(15) Uani 1 1 d . . . . .
H26 H -0.161085 0.257820 0.370573 0.042 Uiso 1 1 calc R U . . .
C27 C -0.1929(5) 0.2774(3) 0.2914(3) 0.0276(13) Uani 1 1 d . . . . .
C28 C 0.0054(6) -0.0162(4) 0.1641(4) 0.0410(18) Uani 1 1 d . . . . .
H28 H -0.055079 -0.046035 0.152713 0.049 Uiso 1 1 calc R U . . .
C29 C 0.0906(7) -0.0406(4) 0.1778(5) 0.053(2) Uani 1 1 d . . . . .
H29 H 0.087756 -0.085862 0.176709 0.064 Uiso 1 1 calc R U . . .
C30 C 0.1784(6) 0.0011(4) 0.1927(4) 0.0405(17) Uani 1 1 d . . . . .
H30 H 0.237605 -0.014614 0.202220 0.049 Uiso 1 1 calc R U . . .
C31 C 0.1800(6) 0.0657(4) 0.1938(4) 0.0437(18) Uani 1 1 d . . . . .
H31 H 0.240408 0.095879 0.203092 0.052 Uiso 1 1 calc R U . . .
C32 C 0.0914(5) 0.0864(3) 0.1809(3) 0.0335(15) Uani 1 1 d . . . . .
H32 H 0.092684 0.131684 0.182712 0.040 Uiso 1 1 calc R U . . .
C33 C -0.3267(5) 0.1017(3) 0.0668(3) 0.0263(12) Uani 1 1 d . . . . .
H33 H -0.296654 0.076380 0.039602 0.032 Uiso 1 1 calc R U . . .
C34 C -0.4138(5) 0.1220(4) 0.0493(3) 0.0357(15) Uani 1 1 d . . . . .
H34 H -0.442352 0.111276 0.011138 0.043 Uiso 1 1 calc R U . . .
C35 C -0.4577(5) 0.1583(4) 0.0891(4) 0.0391(17) Uani 1 1 d . . . . .
H35 H -0.516862 0.173687 0.078639 0.047 Uiso 1 1 calc R U . . .
C36 C -0.4145(5) 0.1721(4) 0.1444(4) 0.0381(16) Uani 1 1 d . . . . .
H36 H -0.444678 0.195450 0.172794 0.046 Uiso 1 1 calc R U . . .
C37 C -0.3256(5) 0.1508(3) 0.1574(3) 0.0306(14) Uani 1 1 d . . . . .
H37 H -0.294007 0.161836 0.194897 0.037 Uiso 1 1 calc R U . . .
C38 C -0.1325(7) 0.1102(4) 0.2739(3) 0.0388(17) Uani 1 1 d . . . . .
H38 H -0.084667 0.146501 0.271065 0.047 Uiso 1 1 calc R U . . .
C39 C -0.1520(8) 0.1012(4) 0.3269(3) 0.046(2) Uani 1 1 d . . . . .
H39 H -0.122723 0.132757 0.359047 0.055 Uiso 1 1 calc R U . . .
C40 C -0.2134(9) 0.0468(5) 0.3323(4) 0.059(2) Uani 1 1 d . . . . .
H40 H -0.225271 0.038461 0.368252 0.070 Uiso 1 1 calc R U . . .
C41 C -0.2576(8) 0.0045(5) 0.2852(4) 0.060(3) Uani 1 1 d . . . . .
H41 H -0.301414 -0.033835 0.287862 0.072 Uiso 1 1 calc R U . . .
C42 C -0.2386(7) 0.0172(5) 0.2333(4) 0.049(2) Uani 1 1 d . . . . .
H42 H -0.270142 -0.013086 0.200921 0.059 Uiso 1 1 calc R U . . .
C43 C 0.2481(6) 0.4748(4) 0.3516(3) 0.0401(17) Uani 1 1 d . . . . .
H43 H 0.212899 0.505689 0.369719 0.048 Uiso 1 1 calc R U . . .
C44 C 0.3423(6) 0.4710(5) 0.3769(4) 0.052(2) Uani 1 1 d . . . . .
H44 H 0.369966 0.498215 0.411712 0.062 Uiso 1 1 calc R U . . .
C45 C 0.3930(6) 0.4272(5) 0.3504(5) 0.063(3) Uani 1 1 d . . . . .
H45 H 0.456446 0.422651 0.366725 0.076 Uiso 1 1 calc R U . . .
C46 C 0.3512(7) 0.3899(5) 0.2998(7) 0.084(5) Uani 1 1 d . . . . .
H46 H 0.386538 0.360292 0.280087 0.101 Uiso 1 1 calc R U . . .
C47 C 0.2571(6) 0.3955(4) 0.2775(5) 0.054(3) Uani 1 1 d . . . . .
H47 H 0.228352 0.368705 0.242753 0.065 Uiso 1 1 calc R U . . .
C48 C -0.0870(5) 0.4826(3) 0.1719(3) 0.0335(15) Uani 1 1 d . . . . .
H48 H -0.026640 0.491225 0.156629 0.040 Uiso 1 1 calc R U . . .
C49 C -0.1737(6) 0.4834(4) 0.1393(3) 0.0373(16) Uani 1 1 d . . . . .
H49 H -0.172772 0.493075 0.102799 0.045 Uiso 1 1 calc R U . . .
C50 C -0.2627(6) 0.4698(4) 0.1605(4) 0.0400(18) Uani 1 1 d . . . . .
H50 H -0.323890 0.468162 0.138152 0.048 Uiso 1 1 calc R U . . .
C51 C -0.2608(5) 0.4589(3) 0.2131(3) 0.0341(15) Uani 1 1 d . . . . .
H51 H -0.320787 0.450920 0.228883 0.041 Uiso 1 1 calc R U . . .
C52 C -0.1697(5) 0.4595(4) 0.2448(3) 0.0346(15) Uani 1 1 d . . . . .
H52 H -0.168898 0.452000 0.282052 0.042 Uiso 1 1 calc R U . . .
C53 C 0.0171(6) 0.5264(4) 0.3748(3) 0.0401(17) Uani 1 1 d . . . . .
H53 H 0.054787 0.561280 0.362166 0.048 Uiso 1 1 calc R U . . .
C54 C -0.0246(7) 0.5402(4) 0.4236(4) 0.0464(19) Uani 1 1 d . . . . .
H54 H -0.016375 0.583564 0.443747 0.056 Uiso 1 1 calc R U . . .
C55 C -0.0785(6) 0.4895(4) 0.4425(3) 0.0411(17) Uani 1 1 d . . . . .
H55 H -0.108627 0.497198 0.475716 0.049 Uiso 1 1 calc R U . . .
C56 C -0.0877(6) 0.4272(4) 0.4118(3) 0.0409(17) Uani 1 1 d . . . . .
H56 H -0.124381 0.391394 0.423722 0.049 Uiso 1 1 calc R U . . .
C57 C -0.0432(6) 0.4178(4) 0.3641(3) 0.0365(15) Uani 1 1 d . . . . .
H57 H -0.048263 0.374616 0.344026 0.044 Uiso 1 1 calc R U . . .
C58 C -0.0424(5) 0.6436(3) 0.2637(3) 0.0232(12) Uani 1 1 d . . . . .
C59 C -0.1457(5) 0.6283(3) 0.2477(3) 0.0308(14) Uani 1 1 d . . . . .
H59 H -0.170813 0.612316 0.209447 0.037 Uiso 1 1 calc R U . . .
C60 C -0.2108(5) 0.6361(3) 0.2864(4) 0.0368(16) Uani 1 1 d . . . . .
H60 H -0.280110 0.624255 0.274818 0.044 Uiso 1 1 calc R U . . .
C61 C -0.1761(6) 0.6610(4) 0.3420(4) 0.0408(17) Uani 1 1 d . . . . .
H61 H -0.221519 0.667021 0.368374 0.049 Uiso 1 1 calc R U . . .
C62 C -0.0750(6) 0.6772(4) 0.3594(3) 0.0374(16) Uani 1 1 d . . . . .
H62 H -0.051464 0.694131 0.397760 0.045 Uiso 1 1 calc R U . . .
C63 C -0.0075(5) 0.6689(3) 0.3207(3) 0.0311(14) Uani 1 1 d . . . . .
C64 C 0.0968(5) 0.6881(3) 0.3425(3) 0.0301(13) Uani 1 1 d . . . . .
H64 H 0.111363 0.707702 0.381027 0.036 Uiso 1 1 calc R U . . .
C65 C 0.2685(5) 0.7097(3) 0.3483(3) 0.0304(13) Uani 1 1 d . . . . .
H65A H 0.262731 0.711200 0.388552 0.037 Uiso 1 1 calc R U . . .
H65B H 0.288002 0.754922 0.342736 0.037 Uiso 1 1 calc R U . . .
C66 C 0.3468(5) 0.6712(3) 0.3320(3) 0.0291(13) Uani 1 1 d . . . . .
H66A H 0.411205 0.693473 0.353445 0.035 Uiso 1 1 calc R U . . .
H66B H 0.331371 0.627929 0.342477 0.035 Uiso 1 1 calc R U . . .
C67 C 0.4305(5) 0.6188(3) 0.2592(3) 0.0283(13) Uani 1 1 d . . . . .
H67A H 0.480317 0.624474 0.292579 0.034 Uiso 1 1 calc R U . . .
H67B H 0.465340 0.630666 0.227935 0.034 Uiso 1 1 calc R U . . .
C68 C 0.3795(5) 0.5490(3) 0.2440(3) 0.0279(13) Uani 1 1 d . . . . .
H68A H 0.428647 0.520451 0.235303 0.033 Uiso 1 1 calc R U . . .
H68B H 0.347550 0.536362 0.275976 0.033 Uiso 1 1 calc R U . . .
C69 C 0.3120(5) 0.4996(3) 0.1518(3) 0.0264(12) Uani 1 1 d . . . . .
H69 H 0.368109 0.478568 0.152886 0.032 Uiso 1 1 calc R U . . .
C70 C 0.2425(5) 0.4821(3) 0.1013(3) 0.0260(12) Uani 1 1 d . . . . .
C71 C 0.2704(5) 0.4415(3) 0.0560(3) 0.0307(14) Uani 1 1 d . . . . .
H71 H 0.334030 0.429359 0.059602 0.037 Uiso 1 1 calc R U . . .
C72 C 0.2077(6) 0.4186(3) 0.0063(3) 0.0348(15) Uani 1 1 d . . . . .
H72 H 0.228992 0.393303 -0.024672 0.042 Uiso 1 1 calc R U . . .
C73 C 0.1122(5) 0.4337(3) 0.0029(3) 0.0306(14) Uani 1 1 d . . . . .
H73 H 0.066952 0.416631 -0.030114 0.037 Uiso 1 1 calc R U . . .
C74 C 0.0827(5) 0.4738(3) 0.0475(3) 0.0275(13) Uani 1 1 d . . . . .
H74 H 0.017133 0.482907 0.044317 0.033 Uiso 1 1 calc R U . . .
C75 C 0.1471(5) 0.5007(3) 0.0967(3) 0.0257(12) Uani 1 1 d . . . . .
C76 C 0.3902(5) 0.7267(3) 0.2566(3) 0.0286(13) Uani 1 1 d . . . . .
H76A H 0.451129 0.748452 0.281871 0.034 Uiso 1 1 calc R U . . .
H76B H 0.338616 0.753886 0.263132 0.034 Uiso 1 1 calc R U . . .
C77 C 0.4113(5) 0.7230(3) 0.1964(3) 0.0290(13) Uani 1 1 d . . . . .
H77A H 0.483299 0.725460 0.194924 0.035 Uiso 1 1 calc R U . . .
H77B H 0.376793 0.680911 0.173534 0.035 Uiso 1 1 calc R U . . .
C78 C 0.4427(5) 0.8207(3) 0.1621(3) 0.0270(13) Uani 1 1 d . . . . .
H78 H 0.509806 0.816041 0.170446 0.032 Uiso 1 1 calc R U . . .
C79 C 0.4262(5) 0.8765(3) 0.1377(3) 0.0272(13) Uani 1 1 d . . . . .
C80 C 0.5098(6) 0.9200(4) 0.1314(3) 0.0364(15) Uani 1 1 d . . . . .
H80 H 0.573738 0.911976 0.143456 0.044 Uiso 1 1 calc R U . . .
C81 C 0.5021(6) 0.9738(4) 0.1083(4) 0.0392(17) Uani 1 1 d . . . . .
H81 H 0.560005 1.003040 0.105079 0.047 Uiso 1 1 calc R U . . .
C82 C 0.4087(6) 0.9856(3) 0.0895(3) 0.0365(16) Uani 1 1 d . . . . .
H82 H 0.402869 1.022634 0.073185 0.044 Uiso 1 1 calc R U . . .
C83 C 0.3250(5) 0.9435(3) 0.0947(3) 0.0295(13) Uani 1 1 d . . . . .
H83 H 0.261814 0.951981 0.081813 0.035 Uiso 1 1 calc R U . . .
C84 C 0.3309(5) 0.8878(3) 0.1188(3) 0.0249(12) Uani 1 1 d . . . . .
C85 C 0.2636(6) 0.8726(3) 0.2580(3) 0.0356(15) Uani 1 1 d . . . . .
H85 H 0.316954 0.886418 0.238580 0.043 Uiso 1 1 calc R U . . .
C86 C 0.2596(7) 0.9068(4) 0.3106(4) 0.0466(19) Uani 1 1 d . . . . .
H86 H 0.309972 0.942818 0.327091 0.056 Uiso 1 1 calc R U . . .
C87 C 0.1835(7) 0.8888(4) 0.3387(3) 0.0470(19) Uani 1 1 d . . . . .
H87 H 0.179449 0.911820 0.375075 0.056 Uiso 1 1 calc R U . . .
C88 C 0.1111(7) 0.8358(4) 0.3133(3) 0.0405(17) Uani 1 1 d . . . . .
H88 H 0.055946 0.822728 0.331728 0.049 Uiso 1 1 calc R U . . .
C89 C 0.1206(6) 0.8030(4) 0.2617(3) 0.0326(14) Uani 1 1 d . . . . .
H89 H 0.072194 0.765854 0.245245 0.039 Uiso 1 1 calc R U . . .
C90 C 0.0314(5) 0.8040(3) 0.0912(3) 0.0301(13) Uani 1 1 d . . . . .
H90 H 0.080781 0.836925 0.083842 0.036 Uiso 1 1 calc R U . . .
C91 C -0.0687(5) 0.8062(3) 0.0739(3) 0.0310(14) Uani 1 1 d . . . . .
H91 H -0.086947 0.840810 0.057336 0.037 Uiso 1 1 calc R U . . .
C92 C -0.1393(5) 0.7558(4) 0.0821(3) 0.0371(16) Uani 1 1 d . . . . .
H92 H -0.207424 0.754052 0.069624 0.045 Uiso 1 1 calc R U . . .
C93 C -0.1094(6) 0.7082(4) 0.1085(3) 0.0383(16) Uani 1 1 d . . . . .
H93 H -0.157039 0.673771 0.115091 0.046 Uiso 1 1 calc R U . . .
C94 C -0.0095(5) 0.7105(3) 0.1254(3) 0.0317(14) Uani 1 1 d . . . . .
H94 H 0.010154 0.677225 0.143429 0.038 Uiso 1 1 calc R U . . .
C95 C 0.3160(5) 0.7342(3) 0.0400(3) 0.0269(12) Uani 1 1 d . . . . .
H95 H 0.334768 0.780247 0.047841 0.032 Uiso 1 1 calc R U . . .
C96 C 0.3592(5) 0.6982(4) -0.0009(3) 0.0322(14) Uani 1 1 d . . . . .
H96 H 0.407372 0.719253 -0.020193 0.039 Uiso 1 1 calc R U . . .
C97 C 0.3310(5) 0.6313(4) -0.0131(3) 0.0337(14) Uani 1 1 d . . . . .
H97 H 0.359698 0.605380 -0.040507 0.040 Uiso 1 1 calc R U . . .
C98 C 0.2592(6) 0.6028(4) 0.0160(3) 0.0360(15) Uani 1 1 d . . . . .
H98 H 0.237469 0.557015 0.008256 0.043 Uiso 1 1 calc R U . . .
C99 C 0.2204(5) 0.6417(3) 0.0561(3) 0.0294(13) Uani 1 1 d . . . . .
H99 H 0.171597 0.621827 0.075568 0.035 Uiso 1 1 calc R U . . .
I1 I 0.73818(6) 0.37573(3) 0.52578(2) 0.05914(17) Uani 1 1 d . . . . .
I2 I 0.48118(3) 0.35241(3) 0.12299(2) 0.03984(12) 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 O2 1.920(4) . ?
U1 O5 1.935(4) . ?
U1 O4 2.259(4) . ?
U1 O3 2.260(4) . ?
U1 N7 2.548(5) . ?
U1 N5 2.578(6) . ?
U1 N6 2.729(6) . ?
U2 O9 1.927(5) . ?
U2 O6 1.927(4) . ?
U2 O7 2.249(4) . ?
U2 O8 2.254(4) . ?
U2 N11 2.562(6) . ?
U2 N13 2.586(5) . ?
U2 N12 2.735(6) . ?
Fe1 O1 2.016(4) . ?
Fe1 O2 2.067(4) . ?
Fe1 N4 2.157(6) . ?
Fe1 N1 2.210(6) . ?
Fe1 N2 2.258(6) . ?
Fe1 N3 2.272(5) . ?
Fe2 O5 1.984(4) . ?
Fe2 O6 1.992(5) . ?
Fe2 N9 2.118(6) . ?
Fe2 N8 2.208(6) . ?
Fe2 N10 2.248(6) . ?
Fe3 O10 2.012(4) . ?
Fe3 O9 2.055(5) . ?
Fe3 N14 2.160(5) . ?
Fe3 N16 2.226(5) . ?
Fe3 N15 2.251(5) . ?
Fe3 N17 2.252(6) . ?
O1 C1 1.302(8) . ?
O3 C27 1.312(8) . ?
O4 C18 1.284(8) . ?
O7 C58 1.315(8) . ?
O8 C75 1.312(8) . ?
O10 C84 1.309(8) . ?
N1 C38 1.335(10) . ?
N1 C42 1.354(11) . ?
N2 C28 1.322(9) . ?
N2 C32 1.341(9) . ?
N3 C33 1.327(9) . ?
N3 C37 1.332(9) . ?
N4 C7 1.275(9) . ?
N4 C8 1.472(8) . ?
N5 C12 1.288(10) . ?
N5 C11 1.505(10) . ?
N6 C19 1.474(9) . ?
N6 C9 1.475(8) . ?
N6 C10 1.507(9) . ?
N7 C21 1.284(9) . ?
N7 C20 1.470(8) . ?
N8 C43 1.327(10) . ?
N8 C47 1.335(11) . ?
N9 C53 1.334(9) . ?
N9 C57 1.343(10) . ?
N10 C48 1.328(10) . ?
N10 C52 1.356(10) . ?
N11 C64 1.303(9) . ?
N11 C65 1.458(9) . ?
N12 C67 1.487(9) . ?
N12 C66 1.489(8) . ?
N12 C76 1.493(8) . ?
N13 C69 1.286(9) . ?
N13 C68 1.458(8) . ?
N14 C78 1.281(9) . ?
N14 C77 1.471(8) . ?
N15 C99 1.337(9) . ?
N15 C95 1.349(9) . ?
N16 C90 1.327(9) . ?
N16 C94 1.348(9) . ?
N17 C85 1.344(9) . ?
N17 C89 1.352(10) . ?
C1 C6 1.423(11) . ?
C1 C2 1.432(9) . ?
C2 C3 1.389(11) . ?
C2 H2 0.9500 . ?
C3 C4 1.361(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.377(12) . ?
C4 H4 0.9500 . ?
C5 C6 1.394(10) . ?
C5 H5 0.9500 . ?
C6 C7 1.449(10) . ?
C7 H7 0.9500 . ?
C8 C9 1.532(9) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.425(12) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.423(12) . ?
C12 H12 0.9500 . ?
C13 C18 1.412(11) . ?
C13 C14 1.427(10) . ?
C14 C15 1.361(14) . ?
C14 H14 0.9500 . ?
C15 C16 1.378(15) . ?
C15 H15 0.9500 . ?
C16 C17 1.383(12) . ?
C16 H16 0.9500 . ?
C17 C18 1.438(11) . ?
C17 H17 0.9500 . ?
C19 C20 1.506(10) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.441(10) . ?
C21 H21 0.9500 . ?
C22 C27 1.406(10) . ?
C22 C23 1.420(10) . ?
C23 C24 1.365(12) . ?
C23 H23 0.9500 . ?
C24 C25 1.427(13) . ?
C24 H24 0.9500 . ?
C25 C26 1.373(11) . ?
C25 H25 0.9500 . ?
C26 C27 1.427(10) . ?
C26 H26 0.9500 . ?
C28 C29 1.386(12) . ?
C28 H28 0.9500 . ?
C29 C30 1.360(13) . ?
C29 H29 0.9500 . ?
C30 C31 1.361(11) . ?
C30 H30 0.9500 . ?
C31 C32 1.382(10) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C34 1.387(10) . ?
C33 H33 0.9500 . ?
C34 C35 1.383(12) . ?
C34 H34 0.9500 . ?
C35 C36 1.387(12) . ?
C35 H35 0.9500 . ?
C36 C37 1.394(10) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C39 1.390(11) . ?
C38 H38 0.9500 . ?
C39 C40 1.354(14) . ?
C39 H39 0.9500 . ?
C40 C41 1.359(15) . ?
C40 H40 0.9500 . ?
C41 C42 1.382(13) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C44 1.401(11) . ?
C43 H43 0.9500 . ?
C44 C45 1.361(16) . ?
C44 H44 0.9500 . ?
C45 C46 1.368(17) . ?
C45 H45 0.9500 . ?
C46 C47 1.385(12) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C48 C49 1.371(10) . ?
C48 H48 0.9500 . ?
C49 C50 1.387(12) . ?
C49 H49 0.9500 . ?
C50 C51 1.345(12) . ?
C50 H50 0.9500 . ?
C51 C52 1.405(10) . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
C53 C54 1.383(12) . ?
C53 H53 0.9500 . ?
C54 C55 1.383(12) . ?
C54 H54 0.9500 . ?
C55 C56 1.382(11) . ?
C55 H55 0.9500 . ?
C56 C57 1.371(11) . ?
C56 H56 0.9500 . ?
C57 H57 0.9500 . ?
C58 C59 1.410(10) . ?
C58 C63 1.413(9) . ?
C59 C60 1.374(10) . ?
C59 H59 0.9500 . ?
C60 C61 1.380(12) . ?
C60 H60 0.9500 . ?
C61 C62 1.387(12) . ?
C61 H61 0.9500 . ?
C62 C63 1.400(10) . ?
C62 H62 0.9500 . ?
C63 C64 1.452(10) . ?
C64 H64 0.9500 . ?
C65 C66 1.496(10) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C67 C68 1.503(9) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C69 C70 1.442(9) . ?
C69 H69 0.9500 . ?
C70 C71 1.405(9) . ?
C70 C75 1.429(9) . ?
C71 C72 1.386(11) . ?
C71 H71 0.9500 . ?
C72 C73 1.398(11) . ?
C72 H72 0.9500 . ?
C73 C74 1.398(9) . ?
C73 H73 0.9500 . ?
C74 C75 1.400(10) . ?
C74 H74 0.9500 . ?
C76 C77 1.519(9) . ?
C76 H76A 0.9900 . ?
C76 H76B 0.9900 . ?
C77 H77A 0.9900 . ?
C77 H77B 0.9900 . ?
C78 C79 1.448(9) . ?
C78 H78 0.9500 . ?
C79 C80 1.400(9) . ?
C79 C84 1.417(9) . ?
C80 C81 1.368(11) . ?
C80 H80 0.9500 . ?
C81 C82 1.395(11) . ?
C81 H81 0.9500 . ?
C82 C83 1.376(10) . ?
C82 H82 0.9500 . ?
C83 C84 1.413(9) . ?
C83 H83 0.9500 . ?
C85 C86 1.376(11) . ?
C85 H85 0.9500 . ?
C86 C87 1.352(13) . ?
C86 H86 0.9500 . ?
C87 C88 1.391(12) . ?
C87 H87 0.9500 . ?
C88 C89 1.364(11) . ?
C88 H88 0.9500 . ?
C89 H89 0.9500 . ?
C90 C91 1.411(10) . ?
C90 H90 0.9500 . ?
C91 C92 1.385(10) . ?
C91 H91 0.9500 . ?
C92 C93 1.378(11) . ?
C92 H92 0.9500 . ?
C93 C94 1.387(10) . ?
C93 H93 0.9500 . ?
C94 H94 0.9500 . ?
C95 C96 1.392(10) . ?
C95 H95 0.9500 . ?
C96 C97 1.383(11) . ?
C96 H96 0.9500 . ?
C97 C98 1.398(11) . ?
C97 H97 0.9500 . ?
C98 C99 1.374(10) . ?
C98 H98 0.9500 . ?
C99 H99 0.9500 . ?

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
O2 U1 O5 175.53(17) . . ?
O2 U1 O4 90.30(17) . . ?
O5 U1 O4 94.07(17) . . ?
O2 U1 O3 89.93(18) . . ?
O5 U1 O3 91.1(2) . . ?
O4 U1 O3 89.75(17) . . ?
O2 U1 N7 89.81(16) . . ?
O5 U1 N7 86.35(16) . . ?
O4 U1 N7 161.77(17) . . ?
O3 U1 N7 72.02(17) . . ?
O2 U1 N5 99.9(2) . . ?
O5 U1 N5 80.7(2) . . ?
O4 U1 N5 70.03(19) . . ?
O3 U1 N5 157.35(19) . . ?
N7 U1 N5 127.83(19) . . ?
O2 U1 N6 80.88(17) . . ?
O5 U1 N6 95.51(19) . . ?
O4 U1 N6 130.45(17) . . ?
O3 U1 N6 138.39(17) . . ?
N7 U1 N6 67.49(17) . . ?
N5 U1 N6 63.87(19) . . ?
O9 U2 O6 175.31(19) . . ?
O9 U2 O7 86.67(18) . . ?
O6 U2 O7 88.64(18) . . ?
O9 U2 O8 89.53(18) . . ?
O6 U2 O8 90.55(17) . . ?
O7 U2 O8 92.80(17) . . ?
O9 U2 N11 95.32(18) . . ?
O6 U2 N11 83.37(18) . . ?
O7 U2 N11 72.16(17) . . ?
O8 U2 N11 163.84(18) . . ?
O9 U2 N13 103.61(18) . . ?
O6 U2 N13 80.81(18) . . ?
O7 U2 N13 159.47(16) . . ?
O8 U2 N13 69.90(17) . . ?
N11 U2 N13 123.42(17) . . ?
O9 U2 N12 81.57(17) . . ?
O6 U2 N12 101.96(18) . . ?
O7 U2 N12 135.65(17) . . ?
O8 U2 N12 129.44(18) . . ?
N11 U2 N12 66.64(18) . . ?
N13 U2 N12 64.32(17) . . ?
O1 Fe1 O2 177.62(19) . . ?
O1 Fe1 N4 86.0(2) . . ?
O2 Fe1 N4 91.79(18) . . ?
O1 Fe1 N1 92.1(2) . . ?
O2 Fe1 N1 90.21(19) . . ?
N4 Fe1 N1 175.9(2) . . ?
O1 Fe1 N2 90.5(2) . . ?
O2 Fe1 N2 90.24(18) . . ?
N4 Fe1 N2 89.0(2) . . ?
N1 Fe1 N2 87.4(2) . . ?
O1 Fe1 N3 87.2(2) . . ?
O2 Fe1 N3 92.05(17) . . ?
N4 Fe1 N3 91.4(2) . . ?
N1 Fe1 N3 92.1(2) . . ?
N2 Fe1 N3 177.66(19) . . ?
O5 Fe2 O6 142.4(2) . . ?
O5 Fe2 N9 112.3(2) . . ?
O6 Fe2 N9 105.3(2) . . ?
O5 Fe2 N8 92.5(2) . . ?
O6 Fe2 N8 85.1(2) . . ?
N9 Fe2 N8 92.1(2) . . ?
O5 Fe2 N10 87.64(18) . . ?
O6 Fe2 N10 92.96(19) . . ?
N9 Fe2 N10 90.7(2) . . ?
N8 Fe2 N10 176.9(2) . . ?
O10 Fe3 O9 177.5(2) . . ?
O10 Fe3 N14 85.98(19) . . ?
O9 Fe3 N14 91.87(19) . . ?
O10 Fe3 N16 88.42(19) . . ?
O9 Fe3 N16 93.79(19) . . ?
N14 Fe3 N16 173.6(2) . . ?
O10 Fe3 N15 92.4(2) . . ?
O9 Fe3 N15 88.67(18) . . ?
N14 Fe3 N15 85.2(2) . . ?
N16 Fe3 N15 91.88(19) . . ?
O10 Fe3 N17 89.4(2) . . ?
O9 Fe3 N17 89.36(19) . . ?
N14 Fe3 N17 92.6(2) . . ?
N16 Fe3 N17 90.5(2) . . ?
N15 Fe3 N17 177.0(2) . . ?
C1 O1 Fe1 132.8(5) . . ?
U1 O2 Fe1 173.2(2) . . ?
C27 O3 U1 143.4(4) . . ?
C18 O4 U1 144.8(5) . . ?
U1 O5 Fe2 166.6(3) . . ?
U2 O6 Fe2 153.1(3) . . ?
C58 O7 U2 137.8(4) . . ?
C75 O8 U2 146.0(4) . . ?
U2 O9 Fe3 171.1(3) . . ?
C84 O10 Fe3 133.5(4) . . ?
C38 N1 C42 115.3(7) . . ?
C38 N1 Fe1 122.9(5) . . ?
C42 N1 Fe1 121.1(5) . . ?
C28 N2 C32 116.1(6) . . ?
C28 N2 Fe1 121.6(5) . . ?
C32 N2 Fe1 122.2(4) . . ?
C33 N3 C37 118.0(6) . . ?
C33 N3 Fe1 121.0(4) . . ?
C37 N3 Fe1 120.9(4) . . ?
C7 N4 C8 116.9(6) . . ?
C7 N4 Fe1 126.7(5) . . ?
C8 N4 Fe1 116.0(4) . . ?
C12 N5 C11 119.0(7) . . ?
C12 N5 U1 130.9(5) . . ?
C11 N5 U1 108.9(5) . . ?
C19 N6 C9 110.3(5) . . ?
C19 N6 C10 108.4(6) . . ?
C9 N6 C10 108.8(6) . . ?
C19 N6 U1 103.2(4) . . ?
C9 N6 U1 112.8(4) . . ?
C10 N6 U1 113.2(4) . . ?
C21 N7 C20 113.3(5) . . ?
C21 N7 U1 130.0(4) . . ?
C20 N7 U1 116.8(4) . . ?
C43 N8 C47 117.7(7) . . ?
C43 N8 Fe2 119.3(5) . . ?
C47 N8 Fe2 122.7(5) . . ?
C53 N9 C57 117.1(6) . . ?
C53 N9 Fe2 120.1(5) . . ?
C57 N9 Fe2 122.7(5) . . ?
C48 N10 C52 117.1(6) . . ?
C48 N10 Fe2 119.4(5) . . ?
C52 N10 Fe2 122.7(5) . . ?
C64 N11 C65 114.6(6) . . ?
C64 N11 U2 126.0(4) . . ?
C65 N11 U2 118.5(4) . . ?
C67 N12 C66 108.9(5) . . ?
C67 N12 C76 110.1(5) . . ?
C66 N12 C76 108.8(5) . . ?
C67 N12 U2 113.6(4) . . ?
C66 N12 U2 104.1(4) . . ?
C76 N12 U2 111.1(4) . . ?
C69 N13 C68 117.8(5) . . ?
C69 N13 U2 131.7(4) . . ?
C68 N13 U2 110.2(4) . . ?
C78 N14 C77 117.8(5) . . ?
C78 N14 Fe3 125.8(4) . . ?
C77 N14 Fe3 115.5(4) . . ?
C99 N15 C95 118.0(6) . . ?
C99 N15 Fe3 121.7(4) . . ?
C95 N15 Fe3 118.2(4) . . ?
C90 N16 C94 118.0(6) . . ?
C90 N16 Fe3 120.7(4) . . ?
C94 N16 Fe3 121.2(4) . . ?
C85 N17 C89 116.4(6) . . ?
C85 N17 Fe3 119.0(5) . . ?
C89 N17 Fe3 124.4(5) . . ?
O1 C1 C6 124.0(6) . . ?
O1 C1 C2 118.7(7) . . ?
C6 C1 C2 117.3(6) . . ?
C3 C2 C1 120.4(7) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C4 C3 C2 121.0(7) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 120.0(8) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 121.6(8) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C1 119.6(7) . . ?
C5 C6 C7 116.9(7) . . ?
C1 C6 C7 123.5(6) . . ?
N4 C7 C6 126.5(7) . . ?
N4 C7 H7 116.8 . . ?
C6 C7 H7 116.8 . . ?
N4 C8 C9 111.3(5) . . ?
N4 C8 H8A 109.4 . . ?
C9 C8 H8A 109.4 . . ?
N4 C8 H8B 109.4 . . ?
C9 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
N6 C9 C8 115.2(6) . . ?
N6 C9 H9A 108.5 . . ?
C8 C9 H9A 108.5 . . ?
N6 C9 H9B 108.5 . . ?
C8 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C11 C10 N6 112.6(7) . . ?
C11 C10 H10A 109.1 . . ?
N6 C10 H10A 109.1 . . ?
C11 C10 H10B 109.1 . . ?
N6 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
C10 C11 N5 110.8(7) . . ?
C10 C11 H11A 109.5 . . ?
N5 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
N5 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
N5 C12 C13 126.8(7) . . ?
N5 C12 H12 116.6 . . ?
C13 C12 H12 116.6 . . ?
C18 C13 C12 122.9(6) . . ?
C18 C13 C14 121.2(8) . . ?
C12 C13 C14 115.7(7) . . ?
C15 C14 C13 120.8(9) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C16 118.9(8) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?
C15 C16 C17 122.7(9) . . ?
C15 C16 H16 118.7 . . ?
C17 C16 H16 118.7 . . ?
C16 C17 C18 120.4(8) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
O4 C18 C13 123.2(7) . . ?
O4 C18 C17 120.8(7) . . ?
C13 C18 C17 115.9(7) . . ?
N6 C19 C20 113.0(5) . . ?
N6 C19 H19A 109.0 . . ?
C20 C19 H19A 109.0 . . ?
N6 C19 H19B 109.0 . . ?
C20 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
N7 C20 C19 112.6(5) . . ?
N7 C20 H20A 109.1 . . ?
C19 C20 H20A 109.1 . . ?
N7 C20 H20B 109.1 . . ?
C19 C20 H20B 109.1 . . ?
H20A C20 H20B 107.8 . . ?
N7 C21 C22 127.5(6) . . ?
N7 C21 H21 116.2 . . ?
C22 C21 H21 116.2 . . ?
C27 C22 C23 118.7(7) . . ?
C27 C22 C21 124.1(6) . . ?
C23 C22 C21 117.1(7) . . ?
C24 C23 C22 122.7(8) . . ?
C24 C23 H23 118.6 . . ?
C22 C23 H23 118.6 . . ?
C23 C24 C25 118.4(7) . . ?
C23 C24 H24 120.8 . . ?
C25 C24 H24 120.8 . . ?
C26 C25 C24 120.4(7) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C27 121.2(7) . . ?
C25 C26 H26 119.4 . . ?
C27 C26 H26 119.4 . . ?
O3 C27 C22 122.5(6) . . ?
O3 C27 C26 118.8(6) . . ?
C22 C27 C26 118.6(6) . . ?
N2 C28 C29 123.3(7) . . ?
N2 C28 H28 118.3 . . ?
C29 C28 H28 118.3 . . ?
C30 C29 C28 119.3(8) . . ?
C30 C29 H29 120.4 . . ?
C28 C29 H29 120.4 . . ?
C29 C30 C31 118.9(8) . . ?
C29 C30 H30 120.5 . . ?
C31 C30 H30 120.5 . . ?
C30 C31 C32 118.3(7) . . ?
C30 C31 H31 120.8 . . ?
C32 C31 H31 120.8 . . ?
N2 C32 C31 124.0(7) . . ?
N2 C32 H32 118.0 . . ?
C31 C32 H32 118.0 . . ?
N3 C33 C34 123.8(6) . . ?
N3 C33 H33 118.1 . . ?
C34 C33 H33 118.1 . . ?
C35 C34 C33 117.8(7) . . ?
C35 C34 H34 121.1 . . ?
C33 C34 H34 121.1 . . ?
C34 C35 C36 119.3(7) . . ?
C34 C35 H35 120.3 . . ?
C36 C35 H35 120.4 . . ?
C35 C36 C37 118.3(7) . . ?
C35 C36 H36 120.9 . . ?
C37 C36 H36 120.9 . . ?
N3 C37 C36 122.7(7) . . ?
N3 C37 H37 118.6 . . ?
C36 C37 H37 118.6 . . ?
N1 C38 C39 123.9(8) . . ?
N1 C38 H38 118.1 . . ?
C39 C38 H38 118.1 . . ?
C40 C39 C38 119.1(8) . . ?
C40 C39 H39 120.4 . . ?
C38 C39 H39 120.4 . . ?
C39 C40 C41 118.5(9) . . ?
C39 C40 H40 120.7 . . ?
C41 C40 H40 120.7 . . ?
C40 C41 C42 119.8(9) . . ?
C40 C41 H41 120.1 . . ?
C42 C41 H41 120.1 . . ?
N1 C42 C41 123.1(8) . . ?
N1 C42 H42 118.5 . . ?
C41 C42 H42 118.5 . . ?
N8 C43 C44 123.3(9) . . ?
N8 C43 H43 118.4 . . ?
C44 C43 H43 118.4 . . ?
C45 C44 C43 118.1(9) . . ?
C45 C44 H44 120.9 . . ?
C43 C44 H44 120.9 . . ?
C44 C45 C46 119.0(8) . . ?
C44 C45 H45 120.5 . . ?
C46 C45 H45 120.5 . . ?
C45 C46 C47 119.8(10) . . ?
C45 C46 H46 120.1 . . ?
C47 C46 H46 120.1 . . ?
N8 C47 C46 122.0(9) . . ?
N8 C47 H47 119.0 . . ?
C46 C47 H47 119.0 . . ?
N10 C48 C49 123.7(7) . . ?
N10 C48 H48 118.1 . . ?
C49 C48 H48 118.1 . . ?
C48 C49 C50 119.0(8) . . ?
C48 C49 H49 120.5 . . ?
C50 C49 H49 120.5 . . ?
C51 C50 C49 118.8(7) . . ?
C51 C50 H50 120.6 . . ?
C49 C50 H50 120.6 . . ?
C50 C51 C52 119.7(7) . . ?
C50 C51 H51 120.2 . . ?
C52 C51 H51 120.2 . . ?
N10 C52 C51 121.6(7) . . ?
N10 C52 H52 119.2 . . ?
C51 C52 H52 119.2 . . ?
N9 C53 C54 123.5(8) . . ?
N9 C53 H53 118.2 . . ?
C54 C53 H53 118.2 . . ?
C55 C54 C53 118.5(8) . . ?
C55 C54 H54 120.8 . . ?
C53 C54 H54 120.8 . . ?
C56 C55 C54 118.5(7) . . ?
C56 C55 H55 120.8 . . ?
C54 C55 H55 120.8 . . ?
C57 C56 C55 119.2(7) . . ?
C57 C56 H56 120.4 . . ?
C55 C56 H56 120.4 . . ?
N9 C57 C56 123.1(7) . . ?
N9 C57 H57 118.4 . . ?
C56 C57 H57 118.4 . . ?
O7 C58 C59 119.4(6) . . ?
O7 C58 C63 122.8(6) . . ?
C59 C58 C63 117.8(6) . . ?
C60 C59 C58 121.4(7) . . ?
C60 C59 H59 119.3 . . ?
C58 C59 H59 119.3 . . ?
C59 C60 C61 120.3(7) . . ?
C59 C60 H60 119.8 . . ?
C61 C60 H60 119.8 . . ?
C60 C61 C62 120.2(7) . . ?
C60 C61 H61 119.9 . . ?
C62 C61 H61 119.9 . . ?
C61 C62 C63 120.2(7) . . ?
C61 C62 H62 119.9 . . ?
C63 C62 H62 119.9 . . ?
C62 C63 C58 120.0(7) . . ?
C62 C63 C64 116.4(7) . . ?
C58 C63 C64 123.6(6) . . ?
N11 C64 C63 127.6(6) . . ?
N11 C64 H64 116.2 . . ?
C63 C64 H64 116.2 . . ?
N11 C65 C66 111.6(6) . . ?
N11 C65 H65A 109.3 . . ?
C66 C65 H65A 109.3 . . ?
N11 C65 H65B 109.3 . . ?
C66 C65 H65B 109.3 . . ?
H65A C65 H65B 108.0 . . ?
N12 C66 C65 113.7(5) . . ?
N12 C66 H66A 108.8 . . ?
C65 C66 H66A 108.8 . . ?
N12 C66 H66B 108.8 . . ?
C65 C66 H66B 108.8 . . ?
H66A C66 H66B 107.7 . . ?
N12 C67 C68 109.9(5) . . ?
N12 C67 H67A 109.7 . . ?
C68 C67 H67A 109.7 . . ?
N12 C67 H67B 109.7 . . ?
C68 C67 H67B 109.7 . . ?
H67A C67 H67B 108.2 . . ?
N13 C68 C67 109.4(5) . . ?
N13 C68 H68A 109.8 . . ?
C67 C68 H68A 109.8 . . ?
N13 C68 H68B 109.8 . . ?
C67 C68 H68B 109.8 . . ?
H68A C68 H68B 108.2 . . ?
N13 C69 C70 126.0(6) . . ?
N13 C69 H69 117.0 . . ?
C70 C69 H69 117.0 . . ?
C71 C70 C75 119.9(6) . . ?
C71 C70 C69 116.6(6) . . ?
C75 C70 C69 123.5(6) . . ?
C72 C71 C70 121.8(6) . . ?
C72 C71 H71 119.1 . . ?
C70 C71 H71 119.1 . . ?
C71 C72 C73 118.4(6) . . ?
C71 C72 H72 120.8 . . ?
C73 C72 H72 120.8 . . ?
C72 C73 C74 120.7(7) . . ?
C72 C73 H73 119.6 . . ?
C74 C73 H73 119.6 . . ?
C73 C74 C75 121.7(6) . . ?
C73 C74 H74 119.1 . . ?
C75 C74 H74 119.1 . . ?
O8 C75 C74 121.3(6) . . ?
O8 C75 C70 121.4(6) . . ?
C74 C75 C70 117.3(6) . . ?
N12 C76 C77 113.7(6) . . ?
N12 C76 H76A 108.8 . . ?
C77 C76 H76A 108.8 . . ?
N12 C76 H76B 108.8 . . ?
C77 C76 H76B 108.8 . . ?
H76A C76 H76B 107.7 . . ?
N14 C77 C76 109.9(6) . . ?
N14 C77 H77A 109.7 . . ?
C76 C77 H77A 109.7 . . ?
N14 C77 H77B 109.7 . . ?
C76 C77 H77B 109.7 . . ?
H77A C77 H77B 108.2 . . ?
N14 C78 C79 127.4(6) . . ?
N14 C78 H78 116.3 . . ?
C79 C78 H78 116.3 . . ?
C80 C79 C84 119.1(6) . . ?
C80 C79 C78 117.4(6) . . ?
C84 C79 C78 123.5(6) . . ?
C81 C80 C79 121.9(7) . . ?
C81 C80 H80 119.1 . . ?
C79 C80 H80 119.1 . . ?
C80 C81 C82 119.6(7) . . ?
C80 C81 H81 120.2 . . ?
C82 C81 H81 120.2 . . ?
C83 C82 C81 120.1(7) . . ?
C83 C82 H82 120.0 . . ?
C81 C82 H82 120.0 . . ?
C82 C83 C84 121.5(6) . . ?
C82 C83 H83 119.3 . . ?
C84 C83 H83 119.3 . . ?
O10 C84 C83 118.7(6) . . ?
O10 C84 C79 123.4(6) . . ?
C83 C84 C79 117.9(6) . . ?
N17 C85 C86 123.3(7) . . ?
N17 C85 H85 118.4 . . ?
C86 C85 H85 118.4 . . ?
C87 C86 C85 119.4(8) . . ?
C87 C86 H86 120.3 . . ?
C85 C86 H86 120.3 . . ?
C86 C87 C88 118.7(8) . . ?
C86 C87 H87 120.6 . . ?
C88 C87 H87 120.6 . . ?
C89 C88 C87 119.0(8) . . ?
C89 C88 H88 120.5 . . ?
C87 C88 H88 120.5 . . ?
N17 C89 C88 123.1(7) . . ?
N17 C89 H89 118.4 . . ?
C88 C89 H89 118.4 . . ?
N16 C90 C91 123.7(7) . . ?
N16 C90 H90 118.1 . . ?
C91 C90 H90 118.1 . . ?
C92 C91 C90 117.4(7) . . ?
C92 C91 H91 121.3 . . ?
C90 C91 H91 121.3 . . ?
C93 C92 C91 119.0(7) . . ?
C93 C92 H92 120.5 . . ?
C91 C92 H92 120.5 . . ?
C92 C93 C94 119.9(7) . . ?
C92 C93 H93 120.0 . . ?
C94 C93 H93 120.0 . . ?
N16 C94 C93 121.9(7) . . ?
N16 C94 H94 119.0 . . ?
C93 C94 H94 119.0 . . ?
N15 C95 C96 122.5(6) . . ?
N15 C95 H95 118.7 . . ?
C96 C95 H95 118.7 . . ?
C97 C96 C95 118.9(6) . . ?
C97 C96 H96 120.6 . . ?
C95 C96 H96 120.6 . . ?
C96 C97 C98 118.4(7) . . ?
C96 C97 H97 120.8 . . ?
C98 C97 H97 120.8 . . ?
C99 C98 C97 119.2(7) . . ?
C99 C98 H98 120.4 . . ?
C97 C98 H98 120.4 . . ?
N15 C99 C98 123.0(7) . . ?
N15 C99 H99 118.5 . . ?
C98 C99 H99 118.5 . . ?

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
Fe1 O1 C1 C6 5.4(10) . . . . ?
Fe1 O1 C1 C2 -176.8(4) . . . . ?
O1 C1 C2 C3 -179.6(6) . . . . ?
C6 C1 C2 C3 -1.6(10) . . . . ?
C1 C2 C3 C4 3.6(11) . . . . ?
C2 C3 C4 C5 -4.5(12) . . . . ?
C3 C4 C5 C6 3.4(12) . . . . ?
C4 C5 C6 C1 -1.5(11) . . . . ?
C4 C5 C6 C7 -178.5(7) . . . . ?
O1 C1 C6 C5 178.4(7) . . . . ?
C2 C1 C6 C5 0.6(10) . . . . ?
O1 C1 C6 C7 -4.8(11) . . . . ?
C2 C1 C6 C7 177.4(6) . . . . ?
C8 N4 C7 C6 -178.0(6) . . . . ?
Fe1 N4 C7 C6 9.3(10) . . . . ?
C5 C6 C7 N4 173.8(7) . . . . ?
C1 C6 C7 N4 -3.1(11) . . . . ?
C7 N4 C8 C9 113.3(6) . . . . ?
Fe1 N4 C8 C9 -73.3(6) . . . . ?
C19 N6 C9 C8 179.0(5) . . . . ?
C10 N6 C9 C8 60.2(8) . . . . ?
U1 N6 C9 C8 -66.2(6) . . . . ?
N4 C8 C9 N6 138.6(6) . . . . ?
C19 N6 C10 C11 99.7(8) . . . . ?
C9 N6 C10 C11 -140.3(8) . . . . ?
U1 N6 C10 C11 -14.1(10) . . . . ?
N6 C10 C11 N5 50.9(11) . . . . ?
C12 N5 C11 C10 127.1(8) . . . . ?
U1 N5 C11 C10 -63.8(8) . . . . ?
C11 N5 C12 C13 167.3(7) . . . . ?
U1 N5 C12 C13 1.0(12) . . . . ?
N5 C12 C13 C18 -8.3(12) . . . . ?
N5 C12 C13 C14 176.9(8) . . . . ?
C18 C13 C14 C15 2.0(13) . . . . ?
C12 C13 C14 C15 176.9(8) . . . . ?
C13 C14 C15 C16 0.4(15) . . . . ?
C14 C15 C16 C17 -1.8(17) . . . . ?
C15 C16 C17 C18 0.8(16) . . . . ?
U1 O4 C18 C13 11.3(12) . . . . ?
U1 O4 C18 C17 -167.4(6) . . . . ?
C12 C13 C18 O4 3.9(11) . . . . ?
C14 C13 C18 O4 178.4(7) . . . . ?
C12 C13 C18 C17 -177.4(7) . . . . ?
C14 C13 C18 C17 -2.9(11) . . . . ?
C16 C17 C18 O4 -179.7(8) . . . . ?
C16 C17 C18 C13 1.6(13) . . . . ?
C9 N6 C19 C20 65.0(7) . . . . ?
C10 N6 C19 C20 -175.9(6) . . . . ?
U1 N6 C19 C20 -55.6(5) . . . . ?
C21 N7 C20 C19 156.7(5) . . . . ?
U1 N7 C20 C19 -22.0(7) . . . . ?
N6 C19 C20 N7 55.9(7) . . . . ?
C20 N7 C21 C22 175.9(6) . . . . ?
U1 N7 C21 C22 -5.7(10) . . . . ?
N7 C21 C22 C27 -1.1(11) . . . . ?
N7 C21 C22 C23 -179.1(7) . . . . ?
C27 C22 C23 C24 1.6(12) . . . . ?
C21 C22 C23 C24 179.7(7) . . . . ?
C22 C23 C24 C25 -1.9(13) . . . . ?
C23 C24 C25 C26 1.3(12) . . . . ?
C24 C25 C26 C27 -0.4(12) . . . . ?
U1 O3 C27 C22 1.0(11) . . . . ?
U1 O3 C27 C26 -176.3(5) . . . . ?
C23 C22 C27 O3 -178.0(6) . . . . ?
C21 C22 C27 O3 4.1(10) . . . . ?
C23 C22 C27 C26 -0.7(10) . . . . ?
C21 C22 C27 C26 -178.7(6) . . . . ?
C25 C26 C27 O3 177.6(7) . . . . ?
C25 C26 C27 C22 0.2(11) . . . . ?
C32 N2 C28 C29 1.8(13) . . . . ?
Fe1 N2 C28 C29 179.9(8) . . . . ?
N2 C28 C29 C30 -1.8(16) . . . . ?
C28 C29 C30 C31 0.0(15) . . . . ?
C29 C30 C31 C32 1.6(14) . . . . ?
C28 N2 C32 C31 0.0(12) . . . . ?
Fe1 N2 C32 C31 -178.1(7) . . . . ?
C30 C31 C32 N2 -1.7(14) . . . . ?
C37 N3 C33 C34 0.3(10) . . . . ?
Fe1 N3 C33 C34 -177.8(5) . . . . ?
N3 C33 C34 C35 -0.5(10) . . . . ?
C33 C34 C35 C36 -0.9(11) . . . . ?
C34 C35 C36 C37 2.6(11) . . . . ?
C33 N3 C37 C36 1.5(10) . . . . ?
Fe1 N3 C37 C36 179.6(5) . . . . ?
C35 C36 C37 N3 -2.9(11) . . . . ?
C42 N1 C38 C39 -5.0(12) . . . . ?
Fe1 N1 C38 C39 -176.0(7) . . . . ?
N1 C38 C39 C40 5.7(15) . . . . ?
C38 C39 C40 C41 -3.2(16) . . . . ?
C39 C40 C41 C42 0.6(18) . . . . ?
C38 N1 C42 C41 2.2(14) . . . . ?
Fe1 N1 C42 C41 173.4(9) . . . . ?
C40 C41 C42 N1 -0.1(18) . . . . ?
C47 N8 C43 C44 -2.0(12) . . . . ?
Fe2 N8 C43 C44 -176.2(6) . . . . ?
N8 C43 C44 C45 0.9(13) . . . . ?
C43 C44 C45 C46 1.3(16) . . . . ?
C44 C45 C46 C47 -2(2) . . . . ?
C43 N8 C47 C46 0.9(16) . . . . ?
Fe2 N8 C47 C46 174.9(10) . . . . ?
C45 C46 C47 N8 1(2) . . . . ?
C52 N10 C48 C49 -1.3(10) . . . . ?
Fe2 N10 C48 C49 168.9(6) . . . . ?
N10 C48 C49 C50 -1.1(11) . . . . ?
C48 C49 C50 C51 2.7(11) . . . . ?
C49 C50 C51 C52 -2.0(11) . . . . ?
C48 N10 C52 C51 2.0(10) . . . . ?
Fe2 N10 C52 C51 -167.9(5) . . . . ?
C50 C51 C52 N10 -0.4(11) . . . . ?
C57 N9 C53 C54 -2.4(12) . . . . ?
Fe2 N9 C53 C54 173.1(7) . . . . ?
N9 C53 C54 C55 0.7(14) . . . . ?
C53 C54 C55 C56 0.4(14) . . . . ?
C54 C55 C56 C57 0.1(13) . . . . ?
C53 N9 C57 C56 3.0(11) . . . . ?
Fe2 N9 C57 C56 -172.4(6) . . . . ?
C55 C56 C57 N9 -1.9(13) . . . . ?
U2 O7 C58 C59 -149.1(5) . . . . ?
U2 O7 C58 C63 31.7(9) . . . . ?
O7 C58 C59 C60 179.2(6) . . . . ?
C63 C58 C59 C60 -1.6(10) . . . . ?
C58 C59 C60 C61 1.9(11) . . . . ?
C59 C60 C61 C62 -1.2(12) . . . . ?
C60 C61 C62 C63 0.4(12) . . . . ?
C61 C62 C63 C58 -0.2(11) . . . . ?
C61 C62 C63 C64 179.1(7) . . . . ?
O7 C58 C63 C62 180.0(6) . . . . ?
C59 C58 C63 C62 0.8(10) . . . . ?
O7 C58 C63 C64 0.7(10) . . . . ?
C59 C58 C63 C64 -178.4(6) . . . . ?
C65 N11 C64 C63 176.1(6) . . . . ?
U2 N11 C64 C63 -15.2(10) . . . . ?
C62 C63 C64 N11 175.9(7) . . . . ?
C58 C63 C64 N11 -4.9(11) . . . . ?
C64 N11 C65 C66 146.3(6) . . . . ?
U2 N11 C65 C66 -23.3(7) . . . . ?
C67 N12 C66 C65 -175.6(5) . . . . ?
C76 N12 C66 C65 64.4(7) . . . . ?
U2 N12 C66 C65 -54.1(6) . . . . ?
N11 C65 C66 N12 54.9(8) . . . . ?
C66 N12 C67 C68 90.8(6) . . . . ?
C76 N12 C67 C68 -150.0(5) . . . . ?
U2 N12 C67 C68 -24.7(6) . . . . ?
C69 N13 C68 C67 122.4(7) . . . . ?
U2 N13 C68 C67 -63.5(6) . . . . ?
N12 C67 C68 N13 58.3(7) . . . . ?
C68 N13 C69 C70 175.8(6) . . . . ?
U2 N13 C69 C70 3.3(10) . . . . ?
N13 C69 C70 C71 172.5(7) . . . . ?
N13 C69 C70 C75 -11.1(11) . . . . ?
C75 C70 C71 C72 0.1(10) . . . . ?
C69 C70 C71 C72 176.6(7) . . . . ?
C70 C71 C72 C73 -3.7(11) . . . . ?
C71 C72 C73 C74 3.3(11) . . . . ?
C72 C73 C74 C75 0.8(10) . . . . ?
U2 O8 C75 C74 -171.1(5) . . . . ?
U2 O8 C75 C70 10.6(11) . . . . ?
C73 C74 C75 O8 177.3(6) . . . . ?
C73 C74 C75 C70 -4.3(9) . . . . ?
C71 C70 C75 O8 -177.8(6) . . . . ?
C69 C70 C75 O8 6.0(10) . . . . ?
C71 C70 C75 C74 3.9(9) . . . . ?
C69 C70 C75 C74 -172.4(6) . . . . ?
C67 N12 C76 C77 55.9(7) . . . . ?
C66 N12 C76 C77 175.1(6) . . . . ?
U2 N12 C76 C77 -70.8(6) . . . . ?
C78 N14 C77 C76 113.0(7) . . . . ?
Fe3 N14 C77 C76 -77.3(6) . . . . ?
N12 C76 C77 N14 141.1(6) . . . . ?
C77 N14 C78 C79 177.8(6) . . . . ?
Fe3 N14 C78 C79 9.3(10) . . . . ?
N14 C78 C79 C80 176.8(7) . . . . ?
N14 C78 C79 C84 -5.1(11) . . . . ?
C84 C79 C80 C81 1.2(12) . . . . ?
C78 C79 C80 C81 179.3(7) . . . . ?
C79 C80 C81 C82 -1.1(13) . . . . ?
C80 C81 C82 C83 0.5(13) . . . . ?
C81 C82 C83 C84 0.0(12) . . . . ?
Fe3 O10 C84 C83 177.6(5) . . . . ?
Fe3 O10 C84 C79 -1.8(10) . . . . ?
C82 C83 C84 O10 -179.3(7) . . . . ?
C82 C83 C84 C79 0.1(10) . . . . ?
C80 C79 C84 O10 178.7(7) . . . . ?
C78 C79 C84 O10 0.7(10) . . . . ?
C80 C79 C84 C83 -0.6(10) . . . . ?
C78 C79 C84 C83 -178.7(6) . . . . ?
C89 N17 C85 C86 0.4(11) . . . . ?
Fe3 N17 C85 C86 -174.9(7) . . . . ?
N17 C85 C86 C87 -1.1(14) . . . . ?
C85 C86 C87 C88 0.1(14) . . . . ?
C86 C87 C88 C89 1.6(13) . . . . ?
C85 N17 C89 C88 1.4(11) . . . . ?
Fe3 N17 C89 C88 176.4(6) . . . . ?
C87 C88 C89 N17 -2.4(12) . . . . ?
C94 N16 C90 C91 2.6(10) . . . . ?
Fe3 N16 C90 C91 -174.3(5) . . . . ?
N16 C90 C91 C92 -3.6(11) . . . . ?
C90 C91 C92 C93 2.8(11) . . . . ?
C91 C92 C93 C94 -1.3(12) . . . . ?
C90 N16 C94 C93 -0.9(10) . . . . ?
Fe3 N16 C94 C93 176.0(6) . . . . ?
C92 C93 C94 N16 0.3(12) . . . . ?
C99 N15 C95 C96 -2.0(9) . . . . ?
Fe3 N15 C95 C96 161.9(5) . . . . ?
N15 C95 C96 C97 0.9(10) . . . . ?
C95 C96 C97 C98 0.6(10) . . . . ?
C96 C97 C98 C99 -1.0(11) . . . . ?
C95 N15 C99 C98 1.6(10) . . . . ?
Fe3 N15 C99 C98 -161.7(5) . . . . ?
C97 C98 C99 N15 -0.1(11) . . . . ?

_refine_diff_density_max         5.508
_refine_diff_density_min         -2.564
_refine_diff_density_rms         0.194



####################################################################### 
# 
# 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_sw16
_database_code_depnum_ccdc_archive 'CCDC 1842379'
_audit_update_record             
;
2018-05-09 deposited with the CCDC.
2018-08-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H42 Fe N7 O5 U, C5 H5 N, 0.5(C6 H14)'
_chemical_formula_sum            'C50 H54 Fe N8 O5 U'
_chemical_formula_weight         1140.89

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'
N N 0.0311 0.0180 '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'
Fe Fe -1.1336 3.1974 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   19.5691(7)
_cell_length_b                   13.9341(3)
_cell_length_c                   19.6431(6)
_cell_angle_alpha                90
_cell_angle_beta                 118.260(4)
_cell_angle_gamma                90
_cell_volume                     4717.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    139.99(13)
_cell_measurement_reflns_used    17136
_cell_measurement_theta_min      4.0390
_cell_measurement_theta_max      75.4570

_exptl_crystal_description       plate
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_F_000             2272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.116
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 -5 11 0.1093
2 -8 5 0.1039
11 -3 -9 0.0992
-1 7 -6 0.1213
-11 3 8 0.0726
-3 -9 4 0.1182
10 -1 2 0.0469
3 9 -3 0.1242
-10 0 -1 0.0565
5 -5 -11 0.1099
2 4 9 0.0809
-7 6 10 0.0771
-4 0 13 0.0883
-12 2 5 0.0579
-12 -2 8 0.0887
-7 -2 -6 0.0758
-7 -5 -4 0.0934
_exptl_absorpt_coefficient_mu    12.500
_shelx_estimated_absorpt_T_min   0.130
_shelx_estimated_absorpt_T_max   0.325
_exptl_absorpt_correction_T_min  0.118
_exptl_absorpt_correction_T_max  0.390
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (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.
;
_diffrn_ambient_temperature      139.99(13)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      1.00  78.00   1.00    1.00    --   42.51 -99.00  60.00   77
  2  ω     37.00 131.00   1.00    2.00    --  109.26 -61.00 150.00   94
  3  ω     34.00  70.00   1.00    2.00    --  109.26 -94.00 120.00   36
  4  ω     35.00 109.00   1.00    2.00    --  109.26 -94.00  60.00   74
  5  ω     67.00 112.00   1.00    2.00    --  109.26-111.00 -60.00   45
  6  ω     37.00 116.00   1.00    2.00    --  109.26-111.00-180.00   79
  7  ω     33.00 134.00   1.00    2.00    --  109.26 -30.00-150.00  101
  8  ω     85.00 146.00   1.00    2.00    --  109.26  77.00-150.00   61
  9  ω    102.00 154.00   1.00    2.00    --  109.26 111.00-150.00   52
 10  ω    100.00 127.00   1.00    2.00    --  109.26 178.00  60.00   27
 11  ω     58.00 104.00   1.00    2.00    --  109.26 178.00 120.00   46
 12  ω     32.00 162.00   1.00    2.00    --  109.26 -15.00  30.00  130
 13  ω     33.00 110.00   1.00    2.00    --  109.26-111.00  30.00   77
 14  ω    -41.00  -3.00   1.00    1.00    --  -42.51 125.00-180.00   38
 15  ω    -68.00  -4.00   1.00    1.00    --  -42.51 125.00 -90.00   64
 16  ω    -85.00 -54.00   1.00    1.00    --  -42.51 125.00-180.00   31
 17  ω   -116.00 -18.00   1.00    1.00    --  -42.51 -37.00-180.00   98
 18  ω   -114.00 -24.00   1.00    1.00    --  -42.51 -37.00  90.00   90
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_reflns_number            34891
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         4.073
_diffrn_reflns_theta_max         75.947
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9657
_reflns_number_gt                8885
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 3.10 (CCDC, 2017)'
_computing_publication_material  'CIFTab (Sheldrick, 2015)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0605P)²+1.0751P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9657
_refine_ls_number_parameters     587
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_ref         0.0893
_refine_ls_wR_factor_gt          0.0858
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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 0.09307(2) 0.77395(2) 0.30997(2) 0.02526(6) Uani 1 1 d . . . . .
Fe1 Fe 0.23058(3) 0.60563(4) 0.48187(3) 0.02778(12) Uani 1 1 d . . . . .
O1 O 0.03284(16) 0.8336(2) 0.37711(16) 0.0349(6) Uani 1 1 d . . . . .
O2 O 0.18837(16) 0.88853(19) 0.36619(16) 0.0337(6) Uani 1 1 d . . . . .
O3 O 0.03355(17) 0.8464(2) 0.22376(17) 0.0404(6) Uani 1 1 d . . . . .
O4 O 0.15757(15) 0.69440(18) 0.39754(14) 0.0292(5) Uani 1 1 d . . . . .
O5 O 0.30558(16) 0.5156(2) 0.56406(16) 0.0372(6) Uani 1 1 d . . . . .
N1 N -0.0425(2) 0.6945(3) 0.2576(2) 0.0454(9) Uani 1 1 d . . . . .
N2 N 0.07631(18) 0.6099(2) 0.22897(17) 0.0303(6) Uani 1 1 d . . . . .
N3 N 0.1818(2) 0.7684(2) 0.2449(2) 0.0298(7) Uani 1 1 d . . . . .
N4 N 0.18413(18) 0.4793(2) 0.41259(18) 0.0306(6) Uani 1 1 d . . . . .
N5 N 0.14264(19) 0.5869(2) 0.52284(18) 0.0330(7) Uani 1 1 d . . . . .
N6 N 0.2812(2) 0.7277(2) 0.5654(2) 0.0359(8) Uani 1 1 d . . . . .
N7 N 0.32057(18) 0.6315(2) 0.44340(18) 0.0319(6) Uani 1 1 d . . . . .
C1 C -0.0294(2) 0.8283(3) 0.3846(2) 0.0315(7) Uani 1 1 d . . . . .
C2 C -0.0351(2) 0.8841(3) 0.4418(2) 0.0388(9) Uani 1 1 d . . . . .
H2 H 0.006704 0.924913 0.473930 0.047 Uiso 1 1 calc R U . . .
C3 C -0.1006(3) 0.8803(4) 0.4518(3) 0.0495(11) Uani 1 1 d . . . . .
H3 H -0.102837 0.918552 0.490683 0.059 Uiso 1 1 calc R U . . .
C4 C -0.1627(3) 0.8218(4) 0.4060(3) 0.0551(12) Uani 1 1 d . . . . .
H4 H -0.207042 0.819091 0.413718 0.066 Uiso 1 1 calc R U . . .
C5 C -0.1591(3) 0.7678(3) 0.3493(3) 0.0455(11) Uani 1 1 d . . . . .
H5 H -0.202160 0.728676 0.317115 0.055 Uiso 1 1 calc R U . . .
C6 C -0.0935(2) 0.7684(3) 0.3373(3) 0.0335(8) Uani 1 1 d . . . . .
C7 C -0.0970(3) 0.7096(3) 0.2742(3) 0.0425(9) Uani 1 1 d . . . . .
H7 H -0.145244 0.679393 0.242001 0.051 Uiso 1 1 calc R U . . .
C8 C -0.0629(3) 0.6474(4) 0.1822(3) 0.0481(10) Uani 1 1 d . . . . .
H8A H -0.115132 0.618269 0.160959 0.058 Uiso 1 1 calc R U . . .
H8B H -0.063902 0.695825 0.144891 0.058 Uiso 1 1 calc R U . . .
C9 C -0.0055(2) 0.5729(3) 0.1932(2) 0.0407(9) Uani 1 1 d . . . . .
H9A H -0.018757 0.543787 0.142490 0.049 Uiso 1 1 calc R U . . .
H9B H -0.008628 0.521731 0.226661 0.049 Uiso 1 1 calc R U . . .
C10 C 0.0945(2) 0.6383(3) 0.1667(2) 0.0364(8) Uani 1 1 d . . . . .
H10A H 0.054387 0.683714 0.131571 0.044 Uiso 1 1 calc R U . . .
H10B H 0.092307 0.580668 0.136205 0.044 Uiso 1 1 calc R U . . .
C11 C 0.1736(3) 0.6848(3) 0.1962(2) 0.0372(8) Uani 1 1 d . . . . .
H11A H 0.214366 0.637255 0.226541 0.045 Uiso 1 1 calc R U . . .
H11B H 0.180876 0.705032 0.151816 0.045 Uiso 1 1 calc R U . . .
C12 C 0.2175(2) 0.8410(3) 0.2363(2) 0.0321(8) Uani 1 1 d . . . . .
H12 H 0.230963 0.836200 0.195853 0.039 Uiso 1 1 calc R U . . .
C13 C 0.2400(2) 0.9296(3) 0.2808(2) 0.0319(7) Uani 1 1 d . . . . .
C14 C 0.2805(2) 0.9976(3) 0.2610(2) 0.0373(8) Uani 1 1 d . . . . .
H14 H 0.287903 0.985919 0.217240 0.045 Uiso 1 1 calc R U . . .
C15 C 0.3099(2) 1.0807(3) 0.3027(3) 0.0396(9) Uani 1 1 d . . . . .
H15 H 0.335780 1.126646 0.287305 0.048 Uiso 1 1 calc R U . . .
C16 C 0.3007(2) 1.0957(3) 0.3683(3) 0.0399(9) Uani 1 1 d . . . . .
H16 H 0.322590 1.151223 0.399167 0.048 Uiso 1 1 calc R U . . .
C17 C 0.2604(2) 1.0313(3) 0.3889(2) 0.0360(8) Uani 1 1 d . . . . .
H17 H 0.254800 1.043392 0.433604 0.043 Uiso 1 1 calc R U . . .
C18 C 0.2270(2) 0.9475(3) 0.3451(2) 0.0302(7) Uani 1 1 d . . . . .
C19 C 0.1314(2) 0.5350(3) 0.2780(2) 0.0320(7) Uani 1 1 d . . . . .
H19A H 0.184389 0.562514 0.303828 0.038 Uiso 1 1 calc R U . . .
H19B H 0.131246 0.481757 0.244564 0.038 Uiso 1 1 calc R U . . .
C20 C 0.1126(2) 0.4947(3) 0.3396(2) 0.0316(7) Uani 1 1 d . . . . .
H20A H 0.078502 0.540104 0.348174 0.038 Uiso 1 1 calc R U . . .
H20B H 0.084467 0.433139 0.321428 0.038 Uiso 1 1 calc R U . . .
C21 C 0.2047(2) 0.3925(3) 0.4322(2) 0.0358(8) Uani 1 1 d . . . . .
H21 H 0.174153 0.344116 0.396716 0.043 Uiso 1 1 calc R U . . .
C22 C 0.2708(2) 0.3603(3) 0.5039(2) 0.0355(8) Uani 1 1 d . . . . .
C23 C 0.2865(3) 0.2610(3) 0.5116(3) 0.0467(11) Uani 1 1 d . . . . .
H23 H 0.255889 0.219728 0.469523 0.056 Uiso 1 1 calc R U . . .
C24 C 0.3447(3) 0.2220(3) 0.5779(4) 0.0520(13) Uani 1 1 d . . . . .
H24 H 0.354513 0.154918 0.581626 0.062 Uiso 1 1 calc R U . . .
C25 C 0.3888(3) 0.2820(4) 0.6392(4) 0.0534(13) Uani 1 1 d . . . . .
H25 H 0.428564 0.255592 0.685737 0.064 Uiso 1 1 calc R U . . .
C26 C 0.3759(3) 0.3800(4) 0.6339(3) 0.0466(10) Uani 1 1 d . . . . .
H26 H 0.407599 0.419506 0.676789 0.056 Uiso 1 1 calc R U . . .
C27 C 0.3166(2) 0.4235(3) 0.5660(2) 0.0369(8) Uani 1 1 d . . . . .
C28 C 0.0888(2) 0.6550(3) 0.5101(2) 0.0355(8) Uani 1 1 d . . . . .
H28 H 0.086701 0.709512 0.480142 0.043 Uiso 1 1 calc R U . . .
C29 C 0.0366(2) 0.6489(3) 0.5389(2) 0.0387(9) Uani 1 1 d . . . . .
H29 H -0.000803 0.697979 0.528390 0.046 Uiso 1 1 calc R U . . .
C30 C 0.0396(3) 0.5705(3) 0.5831(2) 0.0410(9) Uani 1 1 d . . . . .
H30 H 0.004992 0.565321 0.604296 0.049 Uiso 1 1 calc R U . . .
C31 C 0.0934(3) 0.5002(3) 0.5960(2) 0.0398(9) Uani 1 1 d . . . . .
H31 H 0.096375 0.445489 0.626099 0.048 Uiso 1 1 calc R U . . .
C32 C 0.1435(2) 0.5095(3) 0.5647(2) 0.0357(8) Uani 1 1 d . . . . .
H32 H 0.179753 0.459683 0.573103 0.043 Uiso 1 1 calc R U . . .
C33 C 0.3380(3) 0.7099(4) 0.6369(3) 0.0440(10) Uani 1 1 d . . . . .
H33 H 0.355085 0.645554 0.650478 0.053 Uiso 1 1 calc R U . . .
C34 C 0.3731(3) 0.7809(5) 0.6921(3) 0.0617(16) Uani 1 1 d . . . . .
H34 H 0.412842 0.765294 0.742403 0.074 Uiso 1 1 calc R U . . .
C35 C 0.3491(3) 0.8748(5) 0.6725(3) 0.0652(16) Uani 1 1 d . . . . .
H35 H 0.372682 0.925164 0.708815 0.078 Uiso 1 1 calc R U . . .
C36 C 0.2901(4) 0.8941(4) 0.5991(3) 0.0614(14) Uani 1 1 d . . . . .
H36 H 0.271815 0.957758 0.584163 0.074 Uiso 1 1 calc R U . . .
C37 C 0.2585(3) 0.8194(3) 0.5480(3) 0.0502(11) Uani 1 1 d . . . . .
H37 H 0.218200 0.833335 0.497527 0.060 Uiso 1 1 calc R U . . .
C38 C 0.3681(2) 0.5610(3) 0.4449(2) 0.0367(8) Uani 1 1 d . . . . .
H38 H 0.362417 0.499178 0.461930 0.044 Uiso 1 1 calc R U . . .
C39 C 0.4249(2) 0.5740(3) 0.4229(2) 0.0398(9) Uani 1 1 d . . . . .
H39 H 0.457178 0.522036 0.424696 0.048 Uiso 1 1 calc R U . . .
C40 C 0.4340(2) 0.6641(3) 0.3982(2) 0.0419(9) Uani 1 1 d . . . . .
H40 H 0.473086 0.675361 0.383485 0.050 Uiso 1 1 calc R U . . .
C41 C 0.3850(3) 0.7372(3) 0.3956(3) 0.0402(9) Uani 1 1 d . . . . .
H41 H 0.389139 0.799323 0.378078 0.048 Uiso 1 1 calc R U . . .
C42 C 0.3296(2) 0.7184(3) 0.4190(2) 0.0354(9) Uani 1 1 d . . . . .
H42 H 0.296577 0.769222 0.417676 0.042 Uiso 1 1 calc R U . . .
N8 N 0.3990(3) 0.4121(3) 0.2698(2) 0.0545(10) Uani 1 1 d . . . . .
C43 C 0.3387(3) 0.3935(4) 0.2815(3) 0.0506(11) Uani 1 1 d . . . . .
H43 H 0.289071 0.416227 0.244573 0.061 Uiso 1 1 calc R U . . .
C44 C 0.3442(3) 0.3430(4) 0.3444(3) 0.0557(12) Uani 1 1 d . . . . .
H44 H 0.299617 0.332293 0.350733 0.067 Uiso 1 1 calc R U . . .
C45 C 0.4159(3) 0.3082(4) 0.3979(3) 0.0572(13) Uani 1 1 d . . . . .
H45 H 0.421510 0.273498 0.441856 0.069 Uiso 1 1 calc R U . . .
C46 C 0.4790(3) 0.3249(3) 0.3864(3) 0.0524(12) Uani 1 1 d . . . . .
H46 H 0.528864 0.300857 0.421411 0.063 Uiso 1 1 calc R U . . .
C47 C 0.4672(3) 0.3777(4) 0.3222(3) 0.0529(11) Uani 1 1 d . . . . .
H47 H 0.511036 0.390320 0.314893 0.063 Uiso 1 1 calc R U . . .
C48 C 0.5097(3) 0.0289(4) 0.5362(3) 0.0498(11) Uani 1 1 d . . . . .
H48A H 0.566774 0.036111 0.566177 0.060 Uiso 1 1 calc R U . . .
H48B H 0.487093 0.093873 0.520925 0.060 Uiso 1 1 calc R U . . .
C49 C 0.4803(3) -0.0161(5) 0.5875(3) 0.0642(14) Uani 1 1 d . . . . .
H49A H 0.500500 -0.082425 0.600512 0.077 Uiso 1 1 calc R U . . .
H49B H 0.422945 -0.019698 0.558731 0.077 Uiso 1 1 calc R U . . .
C50 C 0.5047(3) 0.0404(6) 0.6621(3) 0.077(2) Uani 1 1 d . . . . .
H50A H 0.559019 0.026323 0.698390 0.115 Uiso 1 1 calc R U . . .
H50B H 0.471861 0.021954 0.685183 0.115 Uiso 1 1 calc R U . . .
H50C H 0.498757 0.109274 0.650502 0.115 Uiso 1 1 calc R U . . .


_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 O3 1.837(3) . ?
U1 O4 1.930(2) . ?
U1 O1 2.300(3) . ?
U1 O2 2.301(3) . ?
U1 N1 2.595(4) . ?
U1 N3 2.598(3) . ?
U1 N2 2.715(3) . ?
Fe1 O4 2.018(3) . ?
Fe1 O5 2.023(3) . ?
Fe1 N4 2.147(3) . ?
Fe1 N5 2.234(3) . ?
Fe1 N6 2.242(3) . ?
Fe1 N7 2.250(3) . ?
O1 C1 1.297(5) . ?
O2 C18 1.309(4) . ?
O5 C27 1.299(5) . ?
N1 C7 1.272(6) . ?
N1 C8 1.492(6) . ?
N2 C10 1.482(5) . ?
N2 C19 1.482(5) . ?
N2 C9 1.503(5) . ?
N3 C12 1.286(5) . ?
N3 C11 1.467(5) . ?
N4 C21 1.275(5) . ?
N4 C20 1.470(5) . ?
N5 C28 1.350(5) . ?
N5 C32 1.351(5) . ?
N6 C33 1.339(6) . ?
N6 C37 1.342(6) . ?
N7 C38 1.343(5) . ?
N7 C42 1.345(5) . ?
C1 C2 1.412(6) . ?
C1 C6 1.424(6) . ?
C2 C3 1.386(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.374(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.411(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.460(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.468(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.515(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.455(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.404(5) . ?
C13 C18 1.424(5) . ?
C14 C15 1.377(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.400(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.376(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.413(6) . ?
C17 H17 0.9500 . ?
C19 C20 1.528(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.460(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.410(6) . ?
C22 C27 1.426(6) . ?
C23 C24 1.373(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.382(9) . ?
C24 H24 0.9500 . ?
C25 C26 1.384(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.423(6) . ?
C26 H26 0.9500 . ?
C28 C29 1.386(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.378(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.372(7) . ?
C30 H30 0.9500 . ?
C31 C32 1.387(6) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C34 1.385(7) . ?
C33 H33 0.9500 . ?
C34 C35 1.382(9) . ?
C34 H34 0.9500 . ?
C35 C36 1.381(9) . ?
C35 H35 0.9500 . ?
C36 C37 1.373(7) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C39 1.381(6) . ?
C38 H38 0.9500 . ?
C39 C40 1.388(7) . ?
C39 H39 0.9500 . ?
C40 C41 1.384(7) . ?
C40 H40 0.9500 . ?
C41 C42 1.387(6) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
N8 C47 1.330(7) . ?
N8 C43 1.331(7) . ?
C43 C44 1.380(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.382(8) . ?
C44 H44 0.9500 . ?
C45 C46 1.375(8) . ?
C45 H45 0.9500 . ?
C46 C47 1.384(7) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C48 C49 1.513(8) . ?
C48 C48 1.517(10) 3_656 ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.528(8) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 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
O3 U1 O4 177.12(12) . . ?
O3 U1 O1 93.24(12) . . ?
O4 U1 O1 89.59(11) . . ?
O3 U1 O2 94.43(12) . . ?
O4 U1 O2 86.06(10) . . ?
O1 U1 O2 89.60(9) . . ?
O3 U1 N1 77.65(14) . . ?
O4 U1 N1 102.86(13) . . ?
O1 U1 N1 71.10(11) . . ?
O2 U1 N1 158.43(11) . . ?
O3 U1 N3 80.96(12) . . ?
O4 U1 N3 96.54(10) . . ?
O1 U1 N3 159.32(10) . . ?
O2 U1 N3 71.23(10) . . ?
N1 U1 N3 126.02(11) . . ?
O3 U1 N2 94.27(12) . . ?
O4 U1 N2 83.41(10) . . ?
O1 U1 N2 133.45(10) . . ?
O2 U1 N2 135.31(10) . . ?
N1 U1 N2 65.89(11) . . ?
N3 U1 N2 67.06(10) . . ?
O4 Fe1 O5 177.97(12) . . ?
O4 Fe1 N4 93.42(11) . . ?
O5 Fe1 N4 85.79(12) . . ?
O4 Fe1 N5 90.03(11) . . ?
O5 Fe1 N5 91.80(12) . . ?
N4 Fe1 N5 88.01(12) . . ?
O4 Fe1 N6 91.79(12) . . ?
O5 Fe1 N6 89.11(13) . . ?
N4 Fe1 N6 173.73(13) . . ?
N5 Fe1 N6 88.52(13) . . ?
O4 Fe1 N7 89.36(11) . . ?
O5 Fe1 N7 88.85(12) . . ?
N4 Fe1 N7 94.72(12) . . ?
N5 Fe1 N7 177.24(12) . . ?
N6 Fe1 N7 88.81(12) . . ?
C1 O1 U1 144.0(3) . . ?
C18 O2 U1 137.9(2) . . ?
U1 O4 Fe1 173.47(15) . . ?
C27 O5 Fe1 133.2(3) . . ?
C7 N1 C8 117.6(4) . . ?
C7 N1 U1 130.7(3) . . ?
C8 N1 U1 108.9(3) . . ?
C10 N2 C19 109.8(3) . . ?
C10 N2 C9 109.0(3) . . ?
C19 N2 C9 110.4(3) . . ?
C10 N2 U1 104.5(2) . . ?
C19 N2 U1 111.3(2) . . ?
C9 N2 U1 111.7(2) . . ?
C12 N3 C11 115.9(3) . . ?
C12 N3 U1 125.0(3) . . ?
C11 N3 U1 116.8(2) . . ?
C21 N4 C20 116.9(3) . . ?
C21 N4 Fe1 127.5(3) . . ?
C20 N4 Fe1 114.8(2) . . ?
C28 N5 C32 117.2(3) . . ?
C28 N5 Fe1 121.2(3) . . ?
C32 N5 Fe1 121.5(3) . . ?
C33 N6 C37 116.9(4) . . ?
C33 N6 Fe1 119.1(3) . . ?
C37 N6 Fe1 123.9(3) . . ?
C38 N7 C42 117.4(4) . . ?
C38 N7 Fe1 121.3(3) . . ?
C42 N7 Fe1 121.3(3) . . ?
O1 C1 C2 119.4(4) . . ?
O1 C1 C6 122.9(4) . . ?
C2 C1 C6 117.7(4) . . ?
C3 C2 C1 121.2(4) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C4 C3 C2 121.1(4) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C5 C4 C3 118.9(4) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
C4 C5 C6 122.1(5) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C5 C6 C1 118.9(4) . . ?
C5 C6 C7 117.2(4) . . ?
C1 C6 C7 123.8(4) . . ?
N1 C7 C6 127.0(4) . . ?
N1 C7 H7 116.5 . . ?
C6 C7 H7 116.5 . . ?
C9 C8 N1 109.8(4) . . ?
C9 C8 H8A 109.7 . . ?
N1 C8 H8A 109.7 . . ?
C9 C8 H8B 109.7 . . ?
N1 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
C8 C9 N2 113.4(4) . . ?
C8 C9 H9A 108.9 . . ?
N2 C9 H9A 108.9 . . ?
C8 C9 H9B 108.9 . . ?
N2 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
N2 C10 C11 113.5(3) . . ?
N2 C10 H10A 108.9 . . ?
C11 C10 H10A 108.9 . . ?
N2 C10 H10B 108.9 . . ?
C11 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
N3 C11 C10 111.5(3) . . ?
N3 C11 H11A 109.3 . . ?
C10 C11 H11A 109.3 . . ?
N3 C11 H11B 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
N3 C12 C13 128.1(4) . . ?
N3 C12 H12 116.0 . . ?
C13 C12 H12 116.0 . . ?
C14 C13 C18 119.3(4) . . ?
C14 C13 C12 117.1(4) . . ?
C18 C13 C12 123.5(3) . . ?
C15 C14 C13 122.3(4) . . ?
C15 C14 H14 118.9 . . ?
C13 C14 H14 118.9 . . ?
C14 C15 C16 118.3(4) . . ?
C14 C15 H15 120.8 . . ?
C16 C15 H15 120.8 . . ?
C17 C16 C15 120.9(4) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C18 121.6(4) . . ?
C16 C17 H17 119.2 . . ?
C18 C17 H17 119.2 . . ?
O2 C18 C17 119.7(4) . . ?
O2 C18 C13 122.9(3) . . ?
C17 C18 C13 117.4(3) . . ?
N2 C19 C20 113.5(3) . . ?
N2 C19 H19A 108.9 . . ?
C20 C19 H19A 108.9 . . ?
N2 C19 H19B 108.9 . . ?
C20 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
N4 C20 C19 110.5(3) . . ?
N4 C20 H20A 109.5 . . ?
C19 C20 H20A 109.5 . . ?
N4 C20 H20B 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?
N4 C21 C22 126.3(4) . . ?
N4 C21 H21 116.9 . . ?
C22 C21 H21 116.9 . . ?
C23 C22 C27 119.9(4) . . ?
C23 C22 C21 117.0(4) . . ?
C27 C22 C21 123.1(4) . . ?
C24 C23 C22 122.0(5) . . ?
C24 C23 H23 119.0 . . ?
C22 C23 H23 119.0 . . ?
C23 C24 C25 118.9(4) . . ?
C23 C24 H24 120.6 . . ?
C25 C24 H24 120.6 . . ?
C24 C25 C26 121.0(5) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C25 C26 C27 122.0(5) . . ?
C25 C26 H26 119.0 . . ?
C27 C26 H26 119.0 . . ?
O5 C27 C26 119.9(4) . . ?
O5 C27 C22 123.9(4) . . ?
C26 C27 C22 116.2(4) . . ?
N5 C28 C29 122.9(4) . . ?
N5 C28 H28 118.6 . . ?
C29 C28 H28 118.6 . . ?
C30 C29 C28 119.1(4) . . ?
C30 C29 H29 120.5 . . ?
C28 C29 H29 120.5 . . ?
C31 C30 C29 118.8(4) . . ?
C31 C30 H30 120.6 . . ?
C29 C30 H30 120.6 . . ?
C30 C31 C32 119.6(4) . . ?
C30 C31 H31 120.2 . . ?
C32 C31 H31 120.2 . . ?
N5 C32 C31 122.4(4) . . ?
N5 C32 H32 118.8 . . ?
C31 C32 H32 118.8 . . ?
N6 C33 C34 123.1(5) . . ?
N6 C33 H33 118.4 . . ?
C34 C33 H33 118.4 . . ?
C35 C34 C33 118.8(5) . . ?
C35 C34 H34 120.6 . . ?
C33 C34 H34 120.6 . . ?
C36 C35 C34 118.7(5) . . ?
C36 C35 H35 120.7 . . ?
C34 C35 H35 120.7 . . ?
C37 C36 C35 118.7(6) . . ?
C37 C36 H36 120.6 . . ?
C35 C36 H36 120.6 . . ?
N6 C37 C36 123.8(5) . . ?
N6 C37 H37 118.1 . . ?
C36 C37 H37 118.1 . . ?
N7 C38 C39 123.3(4) . . ?
N7 C38 H38 118.3 . . ?
C39 C38 H38 118.3 . . ?
C38 C39 C40 118.9(4) . . ?
C38 C39 H39 120.6 . . ?
C40 C39 H39 120.6 . . ?
C41 C40 C39 118.5(4) . . ?
C41 C40 H40 120.8 . . ?
C39 C40 H40 120.8 . . ?
C40 C41 C42 119.1(4) . . ?
C40 C41 H41 120.4 . . ?
C42 C41 H41 120.4 . . ?
N7 C42 C41 122.8(4) . . ?
N7 C42 H42 118.6 . . ?
C41 C42 H42 118.6 . . ?
C47 N8 C43 116.3(4) . . ?
N8 C43 C44 123.6(5) . . ?
N8 C43 H43 118.2 . . ?
C44 C43 H43 118.2 . . ?
C43 C44 C45 118.7(5) . . ?
C43 C44 H44 120.7 . . ?
C45 C44 H44 120.7 . . ?
C46 C45 C44 118.9(5) . . ?
C46 C45 H45 120.6 . . ?
C44 C45 H45 120.6 . . ?
C45 C46 C47 117.7(5) . . ?
C45 C46 H46 121.1 . . ?
C47 C46 H46 121.1 . . ?
N8 C47 C46 124.8(5) . . ?
N8 C47 H47 117.6 . . ?
C46 C47 H47 117.6 . . ?
C49 C48 C48 113.4(6) . 3_656 ?
C49 C48 H48A 108.9 . . ?
C48 C48 H48A 108.9 3_656 . ?
C49 C48 H48B 108.9 . . ?
C48 C48 H48B 108.9 3_656 . ?
H48A C48 H48B 107.7 . . ?
C48 C49 C50 112.3(5) . . ?
C48 C49 H49A 109.1 . . ?
C50 C49 H49A 109.1 . . ?
C48 C49 H49B 109.1 . . ?
C50 C49 H49B 109.1 . . ?
H49A C49 H49B 107.9 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 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 O1 C1 C2 177.8(3) . . . . ?
U1 O1 C1 C6 -2.4(7) . . . . ?
O1 C1 C2 C3 -179.8(4) . . . . ?
C6 C1 C2 C3 0.3(6) . . . . ?
C1 C2 C3 C4 -0.1(7) . . . . ?
C2 C3 C4 C5 -0.8(8) . . . . ?
C3 C4 C5 C6 1.4(8) . . . . ?
C4 C5 C6 C1 -1.1(7) . . . . ?
C4 C5 C6 C7 -178.7(5) . . . . ?
O1 C1 C6 C5 -179.6(4) . . . . ?
C2 C1 C6 C5 0.3(6) . . . . ?
O1 C1 C6 C7 -2.2(6) . . . . ?
C2 C1 C6 C7 177.7(4) . . . . ?
C8 N1 C7 C6 -168.7(4) . . . . ?
U1 N1 C7 C6 -9.7(8) . . . . ?
C5 C6 C7 N1 -174.2(5) . . . . ?
C1 C6 C7 N1 8.4(8) . . . . ?
C7 N1 C8 C9 -135.8(5) . . . . ?
U1 N1 C8 C9 60.9(4) . . . . ?
N1 C8 C9 N2 -56.6(5) . . . . ?
C10 N2 C9 C8 -91.8(4) . . . . ?
C19 N2 C9 C8 147.5(4) . . . . ?
U1 N2 C9 C8 23.2(4) . . . . ?
C19 N2 C10 C11 -63.9(4) . . . . ?
C9 N2 C10 C11 175.1(3) . . . . ?
U1 N2 C10 C11 55.6(3) . . . . ?
C12 N3 C11 C10 -140.5(4) . . . . ?
U1 N3 C11 C10 23.4(4) . . . . ?
N2 C10 C11 N3 -56.0(4) . . . . ?
C11 N3 C12 C13 -174.2(4) . . . . ?
U1 N3 C12 C13 23.4(6) . . . . ?
N3 C12 C13 C14 178.5(4) . . . . ?
N3 C12 C13 C18 2.4(6) . . . . ?
C18 C13 C14 C15 1.5(6) . . . . ?
C12 C13 C14 C15 -174.9(4) . . . . ?
C13 C14 C15 C16 1.9(6) . . . . ?
C14 C15 C16 C17 -2.8(6) . . . . ?
C15 C16 C17 C18 0.3(6) . . . . ?
U1 O2 C18 C17 156.3(3) . . . . ?
U1 O2 C18 C13 -26.2(6) . . . . ?
C16 C17 C18 O2 -179.3(4) . . . . ?
C16 C17 C18 C13 3.1(6) . . . . ?
C14 C13 C18 O2 178.6(3) . . . . ?
C12 C13 C18 O2 -5.3(6) . . . . ?
C14 C13 C18 C17 -3.9(5) . . . . ?
C12 C13 C18 C17 172.2(3) . . . . ?
C10 N2 C19 C20 -174.8(3) . . . . ?
C9 N2 C19 C20 -54.6(4) . . . . ?
U1 N2 C19 C20 70.0(3) . . . . ?
C21 N4 C20 C19 -108.7(4) . . . . ?
Fe1 N4 C20 C19 80.8(3) . . . . ?
N2 C19 C20 N4 -140.3(3) . . . . ?
C20 N4 C21 C22 -176.3(4) . . . . ?
Fe1 N4 C21 C22 -7.3(6) . . . . ?
N4 C21 C22 C23 -175.6(4) . . . . ?
N4 C21 C22 C27 7.2(7) . . . . ?
C27 C22 C23 C24 0.6(7) . . . . ?
C21 C22 C23 C24 -176.7(4) . . . . ?
C22 C23 C24 C25 0.5(8) . . . . ?
C23 C24 C25 C26 -1.2(8) . . . . ?
C24 C25 C26 C27 0.7(8) . . . . ?
Fe1 O5 C27 C26 179.5(3) . . . . ?
Fe1 O5 C27 C22 -2.3(6) . . . . ?
C25 C26 C27 O5 178.6(4) . . . . ?
C25 C26 C27 C22 0.4(7) . . . . ?
C23 C22 C27 O5 -179.2(4) . . . . ?
C21 C22 C27 O5 -2.1(6) . . . . ?
C23 C22 C27 C26 -1.0(6) . . . . ?
C21 C22 C27 C26 176.1(4) . . . . ?
C32 N5 C28 C29 1.0(6) . . . . ?
Fe1 N5 C28 C29 -175.7(3) . . . . ?
N5 C28 C29 C30 0.6(6) . . . . ?
C28 C29 C30 C31 -1.2(6) . . . . ?
C29 C30 C31 C32 0.2(6) . . . . ?
C28 N5 C32 C31 -1.9(6) . . . . ?
Fe1 N5 C32 C31 174.7(3) . . . . ?
C30 C31 C32 N5 1.4(6) . . . . ?
C37 N6 C33 C34 0.1(7) . . . . ?
Fe1 N6 C33 C34 179.5(4) . . . . ?
N6 C33 C34 C35 -0.7(8) . . . . ?
C33 C34 C35 C36 1.1(9) . . . . ?
C34 C35 C36 C37 -1.0(8) . . . . ?
C33 N6 C37 C36 0.1(7) . . . . ?
Fe1 N6 C37 C36 -179.3(4) . . . . ?
C35 C36 C37 N6 0.4(8) . . . . ?
C42 N7 C38 C39 0.1(6) . . . . ?
Fe1 N7 C38 C39 -179.0(3) . . . . ?
N7 C38 C39 C40 0.3(6) . . . . ?
C38 C39 C40 C41 -0.9(6) . . . . ?
C39 C40 C41 C42 1.2(7) . . . . ?
C38 N7 C42 C41 0.2(6) . . . . ?
Fe1 N7 C42 C41 179.3(3) . . . . ?
C40 C41 C42 N7 -0.8(7) . . . . ?
C47 N8 C43 C44 1.1(8) . . . . ?
N8 C43 C44 C45 -1.0(8) . . . . ?
C43 C44 C45 C46 -0.3(8) . . . . ?
C44 C45 C46 C47 1.4(8) . . . . ?
C43 N8 C47 C46 0.1(8) . . . . ?
C45 C46 C47 N8 -1.3(8) . . . . ?
C48 C48 C49 C50 176.7(5) 3_656 . . . ?

_refine_diff_density_max         2.267
_refine_diff_density_min         -1.771
_refine_diff_density_rms         0.116

####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1842380'
_audit_update_record             
;
2018-05-09 deposited with the CCDC.
2018-08-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C69 H69 Fe N11 O8 U2, I'
_chemical_formula_sum            'C69 H69 Fe I N11 O8 U2'
_chemical_formula_weight         1839.16

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.964(2)
_cell_length_b                   23.884(3)
_cell_length_c                   20.0642(9)
_cell_angle_alpha                90
_cell_angle_beta                 105.849(6)
_cell_angle_gamma                90
_cell_volume                     7359.3(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    303
_cell_measurement_theta_min      3
_cell_measurement_theta_max      22

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_F_000             3548
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.329
_exptl_crystal_size_mid          0.312
_exptl_crystal_size_min          0.196
_exptl_absorpt_coefficient_mu    5.062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5310
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker, 2008) was used for absorption correction.
wR2(int) was 0.0650 before and 0.0572 after correction.
The Ration of minimum to maximum transmission is 0.8999.
The λ/2 correction factor is 0.0015.
;
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            94039
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.356
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             16710
_reflns_number_gt                12237
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2016)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0106P)²+103.6292P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16710
_refine_ls_number_parameters     805
_refine_ls_number_restraints     1397
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0584
_refine_ls_wR_factor_ref         0.1217
_refine_ls_wR_factor_gt          0.1091
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.34346(2) 0.54876(2) 0.71157(2) 0.02379(8) Uani 1 1 d . . . . .
U2 U 0.14757(2) 0.46815(2) 0.78520(2) 0.01980(8) Uani 1 1 d . . . . .
Fe1 Fe -0.03616(8) 0.36673(5) 0.82534(6) 0.0263(3) Uani 1 1 d . . . . .
O1 O 0.2497(4) 0.5112(2) 0.6179(3) 0.0287(13) Uani 1 1 d . . . . .
O2 O 0.4052(4) 0.5607(3) 0.6262(3) 0.0364(15) Uani 1 1 d . . . . .
O3 O 0.4257(4) 0.4740(3) 0.7353(4) 0.0385(16) Uani 1 1 d . . . . .
O4 O 0.2375(4) 0.5103(2) 0.7568(3) 0.0273(13) Uani 1 1 d . . . . .
O5 O 0.0615(4) 0.5449(2) 0.7758(3) 0.0289(13) Uani 1 1 d . . . . .
O6 O 0.2056(4) 0.4959(2) 0.8951(3) 0.0269(13) Uani 1 1 d . . . . .
O7 O 0.0620(4) 0.4235(2) 0.8120(3) 0.0240(12) Uani 1 1 d . . . . .
O8 O -0.1311(4) 0.3124(3) 0.8330(4) 0.0397(16) Uani 1 1 d . . . . .
N1 N 0.2470(5) 0.6272(3) 0.6417(4) 0.0386(18) Uani 1 1 d . U . . .
N2 N 0.3216(6) 0.6377(3) 0.7893(4) 0.0419(17) Uani 1 1 d . U . . .
N3 N 0.4764(5) 0.6178(3) 0.7447(5) 0.0404(17) Uani 1 1 d . U . . .
N4 N 0.4063(6) 0.5356(4) 0.8493(4) 0.0467(18) Uani 1 1 d . U . . .
N5 N 0.0682(5) 0.4848(3) 0.6526(4) 0.0278(14) Uani 1 1 d . U . . .
N6 N 0.1616(5) 0.3830(3) 0.7041(3) 0.0251(13) Uani 1 1 d . U . . .
N7 N 0.2645(5) 0.3955(3) 0.8488(4) 0.0251(14) Uani 1 1 d . U . . .
N8 N -0.0486(5) 0.3286(3) 0.7255(4) 0.0262(14) Uani 1 1 d . U . . .
N9 N -0.0238(5) 0.4015(3) 0.9313(4) 0.0324(15) Uani 1 1 d . U . . .
N10 N -0.1408(3) 0.4317(2) 0.7818(3) 0.0322(15) Uani 1 1 d G U . . .
C60 C -0.1170(3) 0.4876(2) 0.7811(3) 0.0346(18) Uani 1 1 d G U . . .
H60 H -0.057330 0.497932 0.796008 0.042 Uiso 1 1 calc R U . . .
C61 C -0.1805(4) 0.52840(18) 0.7585(3) 0.043(2) Uani 1 1 d G U . . .
H61 H -0.164250 0.566625 0.758018 0.052 Uiso 1 1 calc R U . . .
C62 C -0.2678(3) 0.5133(2) 0.7367(4) 0.044(2) Uani 1 1 d G U . . .
H62 H -0.311252 0.541165 0.721273 0.053 Uiso 1 1 calc R U . . .
C63 C -0.2917(3) 0.4573(3) 0.7374(4) 0.047(2) Uani 1 1 d G U . . .
H63 H -0.351335 0.447012 0.722519 0.057 Uiso 1 1 calc R U . . .
C64 C -0.2281(4) 0.4165(2) 0.7600(3) 0.042(2) Uani 1 1 d G U . . .
H64 H -0.244416 0.378318 0.760509 0.051 Uiso 1 1 calc R U . . .
N11 N 0.0634(4) 0.3039(2) 0.8847(3) 0.0359(16) Uani 1 1 d G U . . .
C69 C 0.0386(4) 0.2487(3) 0.8907(4) 0.079(3) Uani 1 1 d G U . . .
H69 H -0.015871 0.235516 0.862827 0.095 Uiso 1 1 calc R U . . .
C68 C 0.0935(5) 0.2129(2) 0.9375(5) 0.096(4) Uani 1 1 d G U . . .
H68 H 0.076546 0.175178 0.941552 0.115 Uiso 1 1 calc R U . . .
C67 C 0.1732(5) 0.2322(3) 0.9783(4) 0.072(3) Uani 1 1 d G U . . .
H67 H 0.210690 0.207690 1.010218 0.086 Uiso 1 1 calc R U . . .
C66 C 0.1980(3) 0.2873(3) 0.9723(3) 0.043(2) Uani 1 1 d G U . . .
H66 H 0.252417 0.300539 1.000161 0.052 Uiso 1 1 calc R U . . .
C65 C 0.1431(4) 0.3232(2) 0.9255(3) 0.042(2) Uani 1 1 d G U . . .
H65 H 0.160000 0.360878 0.921437 0.050 Uiso 1 1 calc R U . . .
C1 C 0.2260(6) 0.5244(4) 0.5513(4) 0.0282(16) Uani 1 1 d . U . . .
C2 C 0.2207(7) 0.4828(4) 0.5004(5) 0.0379(19) Uani 1 1 d . U . . .
H2 H 0.236351 0.445252 0.514167 0.045 Uiso 1 1 calc R U . . .
C3 C 0.1933(7) 0.4960(5) 0.4314(5) 0.041(2) Uani 1 1 d . U . . .
H3 H 0.190163 0.467121 0.398147 0.050 Uiso 1 1 calc R U . . .
C4 C 0.1703(7) 0.5494(5) 0.4086(5) 0.046(2) Uani 1 1 d . U . . .
H4 H 0.152288 0.557654 0.360494 0.055 Uiso 1 1 calc R U . . .
C5 C 0.1736(7) 0.5904(5) 0.4564(5) 0.043(2) Uani 1 1 d . U . . .
H5 H 0.156201 0.627268 0.440674 0.052 Uiso 1 1 calc R U . . .
C6 C 0.2022(6) 0.5803(4) 0.5290(5) 0.0337(17) Uani 1 1 d . U . . .
C7 C 0.2067(7) 0.6252(4) 0.5751(5) 0.041(2) Uani 1 1 d . U . . .
H7 H 0.176852 0.658289 0.555756 0.049 Uiso 1 1 calc R U . . .
C8 C 0.2432(8) 0.6806(4) 0.6781(6) 0.054(2) Uani 1 1 d . U . . .
H8A H 0.190210 0.701641 0.653791 0.065 Uiso 1 1 calc R U . . .
H8B H 0.294583 0.703862 0.678207 0.065 Uiso 1 1 calc R U . . .
C9 C 0.2417(7) 0.6689(5) 0.7508(6) 0.054(2) Uani 1 1 d . U . . .
H9A H 0.189444 0.646440 0.750458 0.065 Uiso 1 1 calc R U . . .
H9B H 0.238139 0.704613 0.774889 0.065 Uiso 1 1 calc R U . . .
C10 C 0.3974(7) 0.6769(4) 0.8070(6) 0.046(2) Uani 1 1 d . U . . .
H10A H 0.401314 0.694077 0.852687 0.055 Uiso 1 1 calc R U . . .
H10B H 0.386902 0.707353 0.772243 0.055 Uiso 1 1 calc R U . . .
C11 C 0.4832(7) 0.6492(4) 0.8096(6) 0.046(2) Uani 1 1 d . U . . .
H11A H 0.529266 0.678033 0.815729 0.055 Uiso 1 1 calc R U . . .
H11B H 0.499484 0.623320 0.849560 0.055 Uiso 1 1 calc R U . . .
C12 C 0.5352(7) 0.6288(4) 0.7143(6) 0.046(2) Uani 1 1 d . U . . .
H12 H 0.579776 0.654007 0.737393 0.055 Uiso 1 1 calc R U . . .
C13 C 0.5409(7) 0.6069(4) 0.6479(7) 0.049(2) Uani 1 1 d . U . . .
C14 C 0.6123(8) 0.6242(5) 0.6219(7) 0.061(2) Uani 1 1 d . U . . .
H14 H 0.657471 0.646645 0.650024 0.073 Uiso 1 1 calc R U . . .
C15 C 0.6159(9) 0.6084(5) 0.5555(8) 0.071(3) Uani 1 1 d . U . . .
H15 H 0.665166 0.617873 0.539929 0.086 Uiso 1 1 calc R U . . .
C16 C 0.5472(9) 0.5788(5) 0.5125(8) 0.068(3) Uani 1 1 d . U . . .
H16 H 0.548563 0.569529 0.466753 0.081 Uiso 1 1 calc R U . . .
C17 C 0.4760(8) 0.5627(5) 0.5359(7) 0.057(2) Uani 1 1 d . U . . .
H17 H 0.429271 0.542668 0.505872 0.068 Uiso 1 1 calc R U . . .
C18 C 0.4726(7) 0.5759(4) 0.6043(6) 0.045(2) Uani 1 1 d . U . . .
C19 C 0.3051(8) 0.6153(5) 0.8533(6) 0.053(2) Uani 1 1 d . U . . .
H19A H 0.250483 0.593328 0.840943 0.063 Uiso 1 1 calc R U . . .
H19B H 0.297089 0.646971 0.882854 0.063 Uiso 1 1 calc R U . . .
C20 C 0.3794(8) 0.5781(5) 0.8946(6) 0.055(2) Uani 1 1 d . U . . .
H20A H 0.430073 0.601875 0.917079 0.067 Uiso 1 1 calc R U . . .
H20B H 0.360518 0.558550 0.931529 0.067 Uiso 1 1 calc R U . . .
C21 C 0.4442(7) 0.4911(5) 0.8818(6) 0.056(2) Uani 1 1 d . U . . .
H21 H 0.450739 0.489804 0.930232 0.067 Uiso 1 1 calc R U . . .
C22 C 0.4777(7) 0.4432(5) 0.8520(7) 0.057(2) Uani 1 1 d . U . . .
C23 C 0.5197(8) 0.4023(5) 0.9013(8) 0.074(3) Uani 1 1 d . U . . .
H23 H 0.523627 0.406105 0.949221 0.089 Uiso 1 1 calc R U . . .
C24 C 0.5548(8) 0.3564(6) 0.8760(9) 0.081(3) Uani 1 1 d . U . . .
H24 H 0.584322 0.328689 0.907743 0.097 Uiso 1 1 calc R U . . .
C25 C 0.5485(8) 0.3495(5) 0.8073(9) 0.075(3) Uani 1 1 d . U . . .
H25 H 0.574060 0.317586 0.792434 0.090 Uiso 1 1 calc R U . . .
C26 C 0.5043(7) 0.3893(4) 0.7580(8) 0.060(2) Uani 1 1 d . U . . .
H26 H 0.499063 0.384235 0.710029 0.072 Uiso 1 1 calc R U . . .
C27 C 0.4684(6) 0.4364(4) 0.7816(7) 0.048(2) Uani 1 1 d . U . . .
C28 C 0.0394(6) 0.5886(4) 0.7336(5) 0.0320(17) Uani 1 1 d . U . . .
C29 C 0.0271(6) 0.6411(4) 0.7615(5) 0.0382(19) Uani 1 1 d . U . . .
H29 H 0.030418 0.643767 0.809358 0.046 Uiso 1 1 calc R U . . .
C30 C 0.0105(7) 0.6888(4) 0.7213(6) 0.048(2) Uani 1 1 d . U . . .
H30 H 0.006181 0.724122 0.741754 0.058 Uiso 1 1 calc R U . . .
C31 C -0.0001(8) 0.6844(5) 0.6495(6) 0.056(2) Uani 1 1 d . U . . .
H31 H -0.013137 0.716769 0.620982 0.067 Uiso 1 1 calc R U . . .
C32 C 0.0085(7) 0.6331(5) 0.6209(6) 0.050(2) Uani 1 1 d . U . . .
H32 H -0.000042 0.630541 0.572233 0.059 Uiso 1 1 calc R U . . .
C33 C 0.0297(6) 0.5839(4) 0.6614(5) 0.0359(17) Uani 1 1 d . U . . .
C34 C 0.0411(6) 0.5324(4) 0.6258(5) 0.0323(17) Uani 1 1 d . U . . .
H34 H 0.026678 0.534340 0.576639 0.039 Uiso 1 1 calc R U . . .
C35 C 0.0724(6) 0.4401(4) 0.6020(4) 0.0309(17) Uani 1 1 d . U . . .
H35A H 0.078189 0.457464 0.558692 0.037 Uiso 1 1 calc R U . . .
H35B H 0.017384 0.418404 0.590644 0.037 Uiso 1 1 calc R U . . .
C36 C 0.1485(6) 0.4006(4) 0.6301(4) 0.0303(17) Uani 1 1 d . U . . .
H36A H 0.139585 0.366580 0.600769 0.036 Uiso 1 1 calc R U . . .
H36B H 0.202354 0.418991 0.626006 0.036 Uiso 1 1 calc R U . . .
C37 C 0.2535(6) 0.3628(4) 0.7293(4) 0.0284(17) Uani 1 1 d . U . . .
H37A H 0.260518 0.329344 0.702176 0.034 Uiso 1 1 calc R U . . .
H37B H 0.292818 0.392243 0.720638 0.034 Uiso 1 1 calc R U . . .
C38 C 0.2803(6) 0.3482(4) 0.8044(4) 0.0293(17) Uani 1 1 d . U . . .
H38A H 0.343006 0.338494 0.818341 0.035 Uiso 1 1 calc R U . . .
H38B H 0.247368 0.314841 0.812227 0.035 Uiso 1 1 calc R U . . .
C39 C 0.3074(5) 0.3918(3) 0.9128(4) 0.0248(16) Uani 1 1 d . U . . .
H39 H 0.345854 0.360851 0.925363 0.030 Uiso 1 1 calc R U . . .
C40 C 0.3031(6) 0.4308(4) 0.9691(4) 0.0276(16) Uani 1 1 d . U . . .
C41 C 0.3502(7) 0.4157(4) 1.0369(5) 0.038(2) Uani 1 1 d . U . . .
H41 H 0.381691 0.381417 1.044696 0.045 Uiso 1 1 calc R U . . .
C42 C 0.3508(7) 0.4505(4) 1.0921(5) 0.040(2) Uani 1 1 d . U . . .
H42 H 0.382565 0.439946 1.137588 0.047 Uiso 1 1 calc R U . . .
C43 C 0.3061(6) 0.5003(4) 1.0817(5) 0.037(2) Uani 1 1 d . U . . .
H43 H 0.307907 0.523983 1.120080 0.044 Uiso 1 1 calc R U . . .
C44 C 0.2584(6) 0.5162(4) 1.0159(4) 0.0319(18) Uani 1 1 d . U . . .
H44 H 0.228425 0.551019 1.009416 0.038 Uiso 1 1 calc R U . . .
C45 C 0.2539(6) 0.4808(3) 0.9578(4) 0.0258(16) Uani 1 1 d . U . . .
C46 C 0.1005(6) 0.3372(4) 0.7095(5) 0.0286(17) Uani 1 1 d . U . . .
H46A H 0.112336 0.325883 0.758661 0.034 Uiso 1 1 calc R U . . .
H46B H 0.111861 0.304384 0.683099 0.034 Uiso 1 1 calc R U . . .
C47 C 0.0039(6) 0.3535(4) 0.6823(4) 0.0270(17) Uani 1 1 d . U . . .
H47A H -0.001601 0.394789 0.682439 0.032 Uiso 1 1 calc R U . . .
H47B H -0.018877 0.340398 0.633882 0.032 Uiso 1 1 calc R U . . .
C48 C -0.1042(6) 0.2908(4) 0.6958(5) 0.0345(19) Uani 1 1 d . U . . .
H48 H -0.103411 0.280165 0.650323 0.041 Uiso 1 1 calc R U . . .
C49 C -0.1673(6) 0.2630(4) 0.7238(5) 0.0394(18) Uani 1 1 d . U . . .
C50 C -0.2194(7) 0.2222(5) 0.6814(7) 0.056(2) Uani 1 1 d . U . . .
H50 H -0.211259 0.214228 0.637164 0.067 Uiso 1 1 calc R U . . .
C51 C -0.2820(8) 0.1939(5) 0.7033(7) 0.067(3) Uani 1 1 d . U . . .
H51 H -0.315474 0.165402 0.675088 0.080 Uiso 1 1 calc R U . . .
C52 C -0.2960(8) 0.2068(5) 0.7660(8) 0.067(3) Uani 1 1 d . U . . .
H52 H -0.340486 0.187889 0.780265 0.080 Uiso 1 1 calc R U . . .
C53 C -0.2459(7) 0.2474(5) 0.8095(7) 0.058(2) Uani 1 1 d . U . . .
H53 H -0.257659 0.256226 0.852198 0.069 Uiso 1 1 calc R U . . .
C54 C -0.1776(6) 0.2756(4) 0.7904(6) 0.0414(19) Uani 1 1 d . U . . .
C55 C -0.0786(6) 0.3829(4) 0.9667(5) 0.0373(19) Uani 1 1 d . U . . .
H55 H -0.127189 0.360939 0.942905 0.045 Uiso 1 1 calc R U . . .
C56 C -0.0676(7) 0.3941(5) 1.0360(5) 0.042(2) Uani 1 1 d . U . . .
H56 H -0.108646 0.380811 1.058758 0.051 Uiso 1 1 calc R U . . .
C57 C 0.0030(8) 0.4244(5) 1.0716(5) 0.049(2) Uani 1 1 d . U . . .
H57 H 0.012170 0.432371 1.119435 0.059 Uiso 1 1 calc R U . . .
C58 C 0.0602(8) 0.4432(5) 1.0365(6) 0.056(2) Uani 1 1 d . U . . .
H58 H 0.109990 0.464166 1.060217 0.067 Uiso 1 1 calc R U . . .
C59 C 0.0458(7) 0.4316(5) 0.9669(5) 0.045(2) Uani 1 1 d . U . . .
H59 H 0.085827 0.445150 0.943388 0.054 Uiso 1 1 calc R U . . .
I1 I 0.04511(4) 0.75713(3) 0.48217(3) 0.03644(15) 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 O3 2.191(6) . ?
U1 O2 2.216(6) . ?
U1 O1 2.244(6) . ?
U1 O4 2.317(6) . ?
U1 N1 2.583(7) . ?
U1 N3 2.625(8) . ?
U1 N4 2.688(8) . ?
U1 N2 2.713(8) . ?
U2 O7 1.922(6) . ?
U2 O4 1.960(6) . ?
U2 O6 2.246(5) . ?
U2 O5 2.267(6) . ?
U2 N7 2.612(7) . ?
U2 N5 2.646(7) . ?
U2 N6 2.653(7) . ?
Fe1 O8 2.033(6) . ?
Fe1 O7 2.144(6) . ?
Fe1 N8 2.159(7) . ?
Fe1 N9 2.241(8) . ?
Fe1 N10 2.272(4) . ?
Fe1 N11 2.273(5) . ?
O1 C1 1.324(10) . ?
O2 C18 1.319(11) . ?
O3 C27 1.336(11) . ?
O5 C28 1.330(10) . ?
O6 C45 1.333(10) . ?
O8 C54 1.307(12) . ?
N1 C7 1.315(12) . ?
N1 C8 1.480(12) . ?
N2 C19 1.480(14) . ?
N2 C10 1.494(12) . ?
N2 C9 1.496(13) . ?
N3 C12 1.278(13) . ?
N3 C11 1.482(14) . ?
N4 C21 1.306(14) . ?
N4 C20 1.502(15) . ?
N5 C34 1.281(11) . ?
N5 C35 1.488(11) . ?
N6 C46 1.488(10) . ?
N6 C37 1.495(11) . ?
N6 C36 1.500(10) . ?
N7 C39 1.283(10) . ?
N7 C38 1.502(11) . ?
N8 C48 1.292(11) . ?
N8 C47 1.485(11) . ?
N9 C55 1.344(11) . ?
N9 C59 1.352(12) . ?
N10 C60 1.3900 . ?
N10 C64 1.3900 . ?
C60 C61 1.3900 . ?
C60 H60 0.9500 . ?
C61 C62 1.3900 . ?
C61 H61 0.9500 . ?
C62 C63 1.3900 . ?
C62 H62 0.9500 . ?
C63 C64 1.3900 . ?
C63 H63 0.9500 . ?
C64 H64 0.9500 . ?
N11 C69 1.3900 . ?
N11 C65 1.3900 . ?
C69 C68 1.3900 . ?
C69 H69 0.9500 . ?
C68 C67 1.3900 . ?
C68 H68 0.9500 . ?
C67 C66 1.3900 . ?
C67 H67 0.9500 . ?
C66 C65 1.3900 . ?
C66 H66 0.9500 . ?
C65 H65 0.9500 . ?
C1 C2 1.411(12) . ?
C1 C6 1.426(13) . ?
C2 C3 1.372(13) . ?
C2 H2 0.9500 . ?
C3 C4 1.372(15) . ?
C3 H3 0.9500 . ?
C4 C5 1.361(15) . ?
C4 H4 0.9500 . ?
C5 C6 1.423(13) . ?
C5 H5 0.9500 . ?
C6 C7 1.406(13) . ?
C7 H7 0.9500 . ?
C8 C9 1.492(17) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.510(15) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.457(16) . ?
C12 H12 0.9500 . ?
C13 C18 1.408(16) . ?
C13 C14 1.438(15) . ?
C14 C15 1.401(19) . ?
C14 H14 0.9500 . ?
C15 C16 1.389(19) . ?
C15 H15 0.9500 . ?
C16 C17 1.398(15) . ?
C16 H16 0.9500 . ?
C17 C18 1.423(16) . ?
C17 H17 0.9500 . ?
C19 C20 1.531(17) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.458(18) . ?
C21 H21 0.9500 . ?
C22 C27 1.390(17) . ?
C22 C23 1.422(15) . ?
C23 C24 1.39(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.36(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.414(16) . ?
C25 H25 0.9500 . ?
C26 C27 1.403(16) . ?
C26 H26 0.9500 . ?
C28 C29 1.408(13) . ?
C28 C33 1.419(13) . ?
C29 C30 1.378(13) . ?
C29 H29 0.9500 . ?
C30 C31 1.406(16) . ?
C30 H30 0.9500 . ?
C31 C32 1.378(16) . ?
C31 H31 0.9500 . ?
C32 C33 1.414(13) . ?
C32 H32 0.9500 . ?
C33 C34 1.460(14) . ?
C34 H34 0.9500 . ?
C35 C36 1.520(13) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.492(12) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.480(12) . ?
C39 H39 0.9500 . ?
C40 C41 1.409(12) . ?
C40 C45 1.413(12) . ?
C41 C42 1.383(13) . ?
C41 H41 0.9500 . ?
C42 C43 1.372(14) . ?
C42 H42 0.9500 . ?
C43 C44 1.386(12) . ?
C43 H43 0.9500 . ?
C44 C45 1.426(12) . ?
C44 H44 0.9500 . ?
C46 C47 1.539(12) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.443(13) . ?
C48 H48 0.9500 . ?
C49 C50 1.406(14) . ?
C49 C54 1.422(15) . ?
C50 C51 1.376(16) . ?
C50 H50 0.9500 . ?
C51 C52 1.373(19) . ?
C51 H51 0.9500 . ?
C52 C53 1.399(17) . ?
C52 H52 0.9500 . ?
C53 C54 1.419(14) . ?
C53 H53 0.9500 . ?
C55 C56 1.379(13) . ?
C55 H55 0.9500 . ?
C56 C57 1.365(15) . ?
C56 H56 0.9500 . ?
C57 C58 1.372(15) . ?
C57 H57 0.9500 . ?
C58 C59 1.379(14) . ?
C58 H58 0.9500 . ?
C59 H59 0.9500 . ?

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
O3 U1 O2 84.6(2) . . ?
O3 U1 O1 94.5(2) . . ?
O2 U1 O1 74.9(2) . . ?
O3 U1 O4 92.9(2) . . ?
O2 U1 O4 151.7(2) . . ?
O1 U1 O4 77.2(2) . . ?
O3 U1 N1 160.5(3) . . ?
O2 U1 N1 79.2(3) . . ?
O1 U1 N1 70.9(2) . . ?
O4 U1 N1 96.3(3) . . ?
O3 U1 N3 93.5(2) . . ?
O2 U1 N3 67.4(3) . . ?
O1 U1 N3 140.4(2) . . ?
O4 U1 N3 140.9(2) . . ?
N1 U1 N3 90.1(2) . . ?
O3 U1 N4 69.4(3) . . ?
O2 U1 N4 133.6(3) . . ?
O1 U1 N4 142.2(2) . . ?
O4 U1 N4 70.0(2) . . ?
N1 U1 N4 130.0(3) . . ?
N3 U1 N4 76.4(2) . . ?
O3 U1 N2 132.6(3) . . ?
O2 U1 N2 119.9(3) . . ?
O1 U1 N2 129.3(2) . . ?
O4 U1 N2 82.1(2) . . ?
N1 U1 N2 66.0(3) . . ?
N3 U1 N2 65.5(3) . . ?
N4 U1 N2 64.6(3) . . ?
O7 U2 O4 177.2(2) . . ?
O7 U2 O6 91.3(2) . . ?
O4 U2 O6 89.7(2) . . ?
O7 U2 O5 90.6(2) . . ?
O4 U2 O5 92.0(2) . . ?
O6 U2 O5 85.5(2) . . ?
O7 U2 N7 87.9(2) . . ?
O4 U2 N7 90.0(2) . . ?
O6 U2 N7 70.6(2) . . ?
O5 U2 N7 156.0(2) . . ?
O7 U2 N5 100.5(2) . . ?
O4 U2 N5 79.5(2) . . ?
O6 U2 N5 154.0(2) . . ?
O5 U2 N5 71.4(2) . . ?
N7 U2 N5 132.3(2) . . ?
O7 U2 N6 86.1(2) . . ?
O4 U2 N6 91.4(2) . . ?
O6 U2 N6 138.4(2) . . ?
O5 U2 N6 136.0(2) . . ?
N7 U2 N6 67.8(2) . . ?
N5 U2 N6 66.2(2) . . ?
O8 Fe1 O7 177.3(3) . . ?
O8 Fe1 N8 85.4(3) . . ?
O7 Fe1 N8 92.1(2) . . ?
O8 Fe1 N9 92.2(3) . . ?
O7 Fe1 N9 90.4(2) . . ?
N8 Fe1 N9 176.8(3) . . ?
O8 Fe1 N10 88.8(2) . . ?
O7 Fe1 N10 90.4(2) . . ?
N8 Fe1 N10 93.4(2) . . ?
N9 Fe1 N10 88.7(2) . . ?
O8 Fe1 N11 88.1(3) . . ?
O7 Fe1 N11 93.0(2) . . ?
N8 Fe1 N11 94.7(3) . . ?
N9 Fe1 N11 83.1(3) . . ?
N10 Fe1 N11 171.1(2) . . ?
C1 O1 U1 133.8(5) . . ?
C18 O2 U1 150.2(7) . . ?
C27 O3 U1 149.3(8) . . ?
U2 O4 U1 171.2(3) . . ?
C28 O5 U2 137.6(5) . . ?
C45 O6 U2 145.4(5) . . ?
U2 O7 Fe1 170.3(3) . . ?
C54 O8 Fe1 133.0(6) . . ?
C7 N1 C8 117.3(8) . . ?
C7 N1 U1 125.3(6) . . ?
C8 N1 U1 117.1(6) . . ?
C19 N2 C10 110.1(8) . . ?
C19 N2 C9 107.4(9) . . ?
C10 N2 C9 109.3(8) . . ?
C19 N2 U1 107.3(6) . . ?
C10 N2 U1 113.9(6) . . ?
C9 N2 U1 108.6(6) . . ?
C12 N3 C11 115.3(9) . . ?
C12 N3 U1 131.1(8) . . ?
C11 N3 U1 113.6(6) . . ?
C21 N4 C20 114.7(10) . . ?
C21 N4 U1 126.9(8) . . ?
C20 N4 U1 117.1(7) . . ?
C34 N5 C35 115.0(7) . . ?
C34 N5 U2 124.7(6) . . ?
C35 N5 U2 118.7(5) . . ?
C46 N6 C37 109.9(7) . . ?
C46 N6 C36 111.1(6) . . ?
C37 N6 C36 106.5(6) . . ?
C46 N6 U2 110.6(5) . . ?
C37 N6 U2 106.2(5) . . ?
C36 N6 U2 112.3(5) . . ?
C39 N7 C38 114.3(7) . . ?
C39 N7 U2 130.5(6) . . ?
C38 N7 U2 115.1(5) . . ?
C48 N8 C47 115.8(7) . . ?
C48 N8 Fe1 126.9(7) . . ?
C47 N8 Fe1 116.7(5) . . ?
C55 N9 C59 117.1(8) . . ?
C55 N9 Fe1 118.5(6) . . ?
C59 N9 Fe1 123.1(6) . . ?
C60 N10 C64 120.0 . . ?
C60 N10 Fe1 119.0(3) . . ?
C64 N10 Fe1 120.8(3) . . ?
N10 C60 C61 120.0 . . ?
N10 C60 H60 120.0 . . ?
C61 C60 H60 120.0 . . ?
C62 C61 C60 120.0 . . ?
C62 C61 H61 120.0 . . ?
C60 C61 H61 120.0 . . ?
C63 C62 C61 120.0 . . ?
C63 C62 H62 120.0 . . ?
C61 C62 H62 120.0 . . ?
C62 C63 C64 120.0 . . ?
C62 C63 H63 120.0 . . ?
C64 C63 H63 120.0 . . ?
C63 C64 N10 120.0 . . ?
C63 C64 H64 120.0 . . ?
N10 C64 H64 120.0 . . ?
C69 N11 C65 120.0 . . ?
C69 N11 Fe1 119.8(3) . . ?
C65 N11 Fe1 119.1(3) . . ?
N11 C69 C68 120.0 . . ?
N11 C69 H69 120.0 . . ?
C68 C69 H69 120.0 . . ?
C67 C68 C69 120.0 . . ?
C67 C68 H68 120.0 . . ?
C69 C68 H68 120.0 . . ?
C68 C67 C66 120.0 . . ?
C68 C67 H67 120.0 . . ?
C66 C67 H67 120.0 . . ?
C65 C66 C67 120.0 . . ?
C65 C66 H66 120.0 . . ?
C67 C66 H66 120.0 . . ?
C66 C65 N11 120.0 . . ?
C66 C65 H65 120.0 . . ?
N11 C65 H65 120.0 . . ?
O1 C1 C2 120.5(8) . . ?
O1 C1 C6 121.2(8) . . ?
C2 C1 C6 118.3(8) . . ?
C3 C2 C1 120.6(10) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 122.2(10) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 H3 118.9 . . ?
C5 C4 C3 118.7(10) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
C4 C5 C6 122.5(10) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.8 . . ?
C7 C6 C5 119.2(9) . . ?
C7 C6 C1 123.1(8) . . ?
C5 C6 C1 117.7(9) . . ?
N1 C7 C6 128.3(9) . . ?
N1 C7 H7 115.8 . . ?
C6 C7 H7 115.8 . . ?
N1 C8 C9 109.6(9) . . ?
N1 C8 H8A 109.8 . . ?
C9 C8 H8A 109.8 . . ?
N1 C8 H8B 109.8 . . ?
C9 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
C8 C9 N2 111.0(9) . . ?
C8 C9 H9A 109.4 . . ?
N2 C9 H9A 109.4 . . ?
C8 C9 H9B 109.4 . . ?
N2 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
N2 C10 C11 113.7(8) . . ?
N2 C10 H10A 108.8 . . ?
C11 C10 H10A 108.8 . . ?
N2 C10 H10B 108.8 . . ?
C11 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
N3 C11 C10 110.1(8) . . ?
N3 C11 H11A 109.6 . . ?
C10 C11 H11A 109.6 . . ?
N3 C11 H11B 109.6 . . ?
C10 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
N3 C12 C13 126.8(10) . . ?
N3 C12 H12 116.6 . . ?
C13 C12 H12 116.6 . . ?
C18 C13 C14 118.8(12) . . ?
C18 C13 C12 121.7(10) . . ?
C14 C13 C12 118.8(11) . . ?
C15 C14 C13 120.6(13) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C16 C15 C14 119.9(12) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C15 C16 C17 120.5(13) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C16 C17 C18 120.8(13) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
O2 C18 C13 120.1(10) . . ?
O2 C18 C17 120.6(11) . . ?
C13 C18 C17 119.3(10) . . ?
N2 C19 C20 112.6(10) . . ?
N2 C19 H19A 109.1 . . ?
C20 C19 H19A 109.1 . . ?
N2 C19 H19B 109.1 . . ?
C20 C19 H19B 109.1 . . ?
H19A C19 H19B 107.8 . . ?
N4 C20 C19 111.8(9) . . ?
N4 C20 H20A 109.3 . . ?
C19 C20 H20A 109.3 . . ?
N4 C20 H20B 109.3 . . ?
C19 C20 H20B 109.3 . . ?
H20A C20 H20B 107.9 . . ?
N4 C21 C22 127.4(11) . . ?
N4 C21 H21 116.3 . . ?
C22 C21 H21 116.3 . . ?
C27 C22 C23 121.8(13) . . ?
C27 C22 C21 123.9(10) . . ?
C23 C22 C21 114.3(13) . . ?
C24 C23 C22 116.6(15) . . ?
C24 C23 H23 121.7 . . ?
C22 C23 H23 121.7 . . ?
C25 C24 C23 122.7(13) . . ?
C25 C24 H24 118.7 . . ?
C23 C24 H24 118.7 . . ?
C24 C25 C26 120.7(14) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C27 C26 C25 118.4(14) . . ?
C27 C26 H26 120.8 . . ?
C25 C26 H26 120.8 . . ?
O3 C27 C22 121.5(11) . . ?
O3 C27 C26 118.8(12) . . ?
C22 C27 C26 119.7(10) . . ?
O5 C28 C29 119.2(8) . . ?
O5 C28 C33 121.6(8) . . ?
C29 C28 C33 119.2(8) . . ?
C30 C29 C28 121.9(10) . . ?
C30 C29 H29 119.1 . . ?
C28 C29 H29 119.1 . . ?
C29 C30 C31 119.2(10) . . ?
C29 C30 H30 120.4 . . ?
C31 C30 H30 120.4 . . ?
C32 C31 C30 119.6(10) . . ?
C32 C31 H31 120.2 . . ?
C30 C31 H31 120.2 . . ?
C31 C32 C33 122.3(10) . . ?
C31 C32 H32 118.8 . . ?
C33 C32 H32 118.8 . . ?
C32 C33 C28 117.6(9) . . ?
C32 C33 C34 117.5(9) . . ?
C28 C33 C34 124.9(8) . . ?
N5 C34 C33 128.0(8) . . ?
N5 C34 H34 116.0 . . ?
C33 C34 H34 116.0 . . ?
N5 C35 C36 111.9(7) . . ?
N5 C35 H35A 109.2 . . ?
C36 C35 H35A 109.2 . . ?
N5 C35 H35B 109.2 . . ?
C36 C35 H35B 109.2 . . ?
H35A C35 H35B 107.9 . . ?
N6 C36 C35 115.0(7) . . ?
N6 C36 H36A 108.5 . . ?
C35 C36 H36A 108.5 . . ?
N6 C36 H36B 108.5 . . ?
C35 C36 H36B 108.5 . . ?
H36A C36 H36B 107.5 . . ?
C38 C37 N6 113.7(7) . . ?
C38 C37 H37A 108.8 . . ?
N6 C37 H37A 108.8 . . ?
C38 C37 H37B 108.8 . . ?
N6 C37 H37B 108.8 . . ?
H37A C37 H37B 107.7 . . ?
C37 C38 N7 112.0(7) . . ?
C37 C38 H38A 109.2 . . ?
N7 C38 H38A 109.2 . . ?
C37 C38 H38B 109.2 . . ?
N7 C38 H38B 109.2 . . ?
H38A C38 H38B 107.9 . . ?
N7 C39 C40 126.7(8) . . ?
N7 C39 H39 116.6 . . ?
C40 C39 H39 116.6 . . ?
C41 C40 C45 119.9(8) . . ?
C41 C40 C39 116.8(8) . . ?
C45 C40 C39 123.2(8) . . ?
C42 C41 C40 120.2(9) . . ?
C42 C41 H41 119.9 . . ?
C40 C41 H41 119.9 . . ?
C43 C42 C41 120.7(9) . . ?
C43 C42 H42 119.6 . . ?
C41 C42 H42 119.6 . . ?
C42 C43 C44 120.7(9) . . ?
C42 C43 H43 119.7 . . ?
C44 C43 H43 119.7 . . ?
C43 C44 C45 120.5(9) . . ?
C43 C44 H44 119.8 . . ?
C45 C44 H44 119.8 . . ?
O6 C45 C40 122.3(7) . . ?
O6 C45 C44 119.8(8) . . ?
C40 C45 C44 117.9(8) . . ?
N6 C46 C47 113.6(7) . . ?
N6 C46 H46A 108.8 . . ?
C47 C46 H46A 108.8 . . ?
N6 C46 H46B 108.8 . . ?
C47 C46 H46B 108.8 . . ?
H46A C46 H46B 107.7 . . ?
N8 C47 C46 111.2(7) . . ?
N8 C47 H47A 109.4 . . ?
C46 C47 H47A 109.4 . . ?
N8 C47 H47B 109.4 . . ?
C46 C47 H47B 109.4 . . ?
H47A C47 H47B 108.0 . . ?
N8 C48 C49 127.4(9) . . ?
N8 C48 H48 116.3 . . ?
C49 C48 H48 116.3 . . ?
C50 C49 C54 120.9(10) . . ?
C50 C49 C48 116.4(10) . . ?
C54 C49 C48 122.7(9) . . ?
C51 C50 C49 120.6(13) . . ?
C51 C50 H50 119.7 . . ?
C49 C50 H50 119.7 . . ?
C52 C51 C50 119.8(12) . . ?
C52 C51 H51 120.1 . . ?
C50 C51 H51 120.1 . . ?
C51 C52 C53 121.3(11) . . ?
C51 C52 H52 119.4 . . ?
C53 C52 H52 119.4 . . ?
C52 C53 C54 120.7(12) . . ?
C52 C53 H53 119.7 . . ?
C54 C53 H53 119.7 . . ?
O8 C54 C53 118.9(11) . . ?
O8 C54 C49 124.5(9) . . ?
C53 C54 C49 116.6(10) . . ?
N9 C55 C56 123.1(10) . . ?
N9 C55 H55 118.4 . . ?
C56 C55 H55 118.4 . . ?
C57 C56 C55 119.4(10) . . ?
C57 C56 H56 120.3 . . ?
C55 C56 H56 120.3 . . ?
C56 C57 C58 118.4(10) . . ?
C56 C57 H57 120.8 . . ?
C58 C57 H57 120.8 . . ?
C57 C58 C59 120.2(11) . . ?
C57 C58 H58 119.9 . . ?
C59 C58 H58 119.9 . . ?
N9 C59 C58 121.9(10) . . ?
N9 C59 H59 119.1 . . ?
C58 C59 H59 119.1 . . ?

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
C64 N10 C60 C61 0.0 . . . . ?
Fe1 N10 C60 C61 -176.2(4) . . . . ?
N10 C60 C61 C62 0.0 . . . . ?
C60 C61 C62 C63 0.0 . . . . ?
C61 C62 C63 C64 0.0 . . . . ?
C62 C63 C64 N10 0.0 . . . . ?
C60 N10 C64 C63 0.0 . . . . ?
Fe1 N10 C64 C63 176.1(4) . . . . ?
C65 N11 C69 C68 0.0 . . . . ?
Fe1 N11 C69 C68 -167.6(5) . . . . ?
N11 C69 C68 C67 0.0 . . . . ?
C69 C68 C67 C66 0.0 . . . . ?
C68 C67 C66 C65 0.0 . . . . ?
C67 C66 C65 N11 0.0 . . . . ?
C69 N11 C65 C66 0.0 . . . . ?
Fe1 N11 C65 C66 167.7(5) . . . . ?
U1 O1 C1 C2 133.8(8) . . . . ?
U1 O1 C1 C6 -48.5(12) . . . . ?
O1 C1 C2 C3 177.7(9) . . . . ?
C6 C1 C2 C3 -0.1(14) . . . . ?
C1 C2 C3 C4 0.2(16) . . . . ?
C2 C3 C4 C5 -1.0(17) . . . . ?
C3 C4 C5 C6 1.6(17) . . . . ?
C4 C5 C6 C7 177.8(10) . . . . ?
C4 C5 C6 C1 -1.5(15) . . . . ?
O1 C1 C6 C7 3.6(14) . . . . ?
C2 C1 C6 C7 -178.6(9) . . . . ?
O1 C1 C6 C5 -177.1(8) . . . . ?
C2 C1 C6 C5 0.7(13) . . . . ?
C8 N1 C7 C6 178.5(11) . . . . ?
U1 N1 C7 C6 4.3(16) . . . . ?
C5 C6 C7 N1 -164.9(11) . . . . ?
C1 C6 C7 N1 14.4(17) . . . . ?
C7 N1 C8 C9 146.5(10) . . . . ?
U1 N1 C8 C9 -38.8(11) . . . . ?
N1 C8 C9 N2 60.1(12) . . . . ?
C19 N2 C9 C8 -165.8(8) . . . . ?
C10 N2 C9 C8 74.7(10) . . . . ?
U1 N2 C9 C8 -50.1(10) . . . . ?
C19 N2 C10 C11 93.3(11) . . . . ?
C9 N2 C10 C11 -148.9(9) . . . . ?
U1 N2 C10 C11 -27.3(11) . . . . ?
C12 N3 C11 C10 128.1(9) . . . . ?
U1 N3 C11 C10 -51.5(9) . . . . ?
N2 C10 C11 N3 52.3(11) . . . . ?
C11 N3 C12 C13 -175.8(9) . . . . ?
U1 N3 C12 C13 3.7(15) . . . . ?
N3 C12 C13 C18 9.4(16) . . . . ?
N3 C12 C13 C14 -180.0(10) . . . . ?
C18 C13 C14 C15 -2.9(16) . . . . ?
C12 C13 C14 C15 -173.9(11) . . . . ?
C13 C14 C15 C16 4.3(19) . . . . ?
C14 C15 C16 C17 -3(2) . . . . ?
C15 C16 C17 C18 -0.3(19) . . . . ?
U1 O2 C18 C13 -14.4(18) . . . . ?
U1 O2 C18 C17 167.4(9) . . . . ?
C14 C13 C18 O2 -178.2(9) . . . . ?
C12 C13 C18 O2 -7.5(15) . . . . ?
C14 C13 C18 C17 0.0(15) . . . . ?
C12 C13 C18 C17 170.6(9) . . . . ?
C16 C17 C18 O2 179.8(10) . . . . ?
C16 C17 C18 C13 1.7(16) . . . . ?
C10 N2 C19 C20 -65.9(11) . . . . ?
C9 N2 C19 C20 175.1(8) . . . . ?
U1 N2 C19 C20 58.6(9) . . . . ?
C21 N4 C20 C19 -156.2(9) . . . . ?
U1 N4 C20 C19 11.6(11) . . . . ?
N2 C19 C20 N4 -48.1(12) . . . . ?
C20 N4 C21 C22 -179.6(10) . . . . ?
U1 N4 C21 C22 14.0(15) . . . . ?
N4 C21 C22 C27 -4.5(18) . . . . ?
N4 C21 C22 C23 176.9(10) . . . . ?
C27 C22 C23 C24 2.9(17) . . . . ?
C21 C22 C23 C24 -178.4(11) . . . . ?
C22 C23 C24 C25 -1.3(19) . . . . ?
C23 C24 C25 C26 -1(2) . . . . ?
C24 C25 C26 C27 1.0(18) . . . . ?
U1 O3 C27 C22 -8.4(18) . . . . ?
U1 O3 C27 C26 171.5(8) . . . . ?
C23 C22 C27 O3 177.2(10) . . . . ?
C21 C22 C27 O3 -1.3(16) . . . . ?
C23 C22 C27 C26 -2.7(16) . . . . ?
C21 C22 C27 C26 178.8(10) . . . . ?
C25 C26 C27 O3 -179.3(9) . . . . ?
C25 C26 C27 C22 0.6(15) . . . . ?
U2 O5 C28 C29 -143.4(7) . . . . ?
U2 O5 C28 C33 35.1(14) . . . . ?
O5 C28 C29 C30 175.1(9) . . . . ?
C33 C28 C29 C30 -3.4(15) . . . . ?
C28 C29 C30 C31 4.1(17) . . . . ?
C29 C30 C31 C32 -1.7(18) . . . . ?
C30 C31 C32 C33 -1.4(19) . . . . ?
C31 C32 C33 C28 2.0(16) . . . . ?
C31 C32 C33 C34 -177.2(11) . . . . ?
O5 C28 C33 C32 -178.2(9) . . . . ?
C29 C28 C33 C32 0.4(14) . . . . ?
O5 C28 C33 C34 1.0(15) . . . . ?
C29 C28 C33 C34 179.5(9) . . . . ?
C35 N5 C34 C33 179.9(9) . . . . ?
U2 N5 C34 C33 -14.6(13) . . . . ?
C32 C33 C34 N5 172.8(10) . . . . ?
C28 C33 C34 N5 -6.4(16) . . . . ?
C34 N5 C35 C36 145.5(8) . . . . ?
U2 N5 C35 C36 -21.0(9) . . . . ?
C46 N6 C36 C35 80.3(9) . . . . ?
C37 N6 C36 C35 -160.0(7) . . . . ?
U2 N6 C36 C35 -44.2(8) . . . . ?
N5 C35 C36 N6 43.4(10) . . . . ?
C46 N6 C37 C38 -64.6(9) . . . . ?
C36 N6 C37 C38 174.9(7) . . . . ?
U2 N6 C37 C38 55.0(8) . . . . ?
N6 C37 C38 N7 -53.9(10) . . . . ?
C39 N7 C38 C37 -161.5(8) . . . . ?
U2 N7 C38 C37 22.2(9) . . . . ?
C38 N7 C39 C40 -177.8(8) . . . . ?
U2 N7 C39 C40 -2.2(13) . . . . ?
N7 C39 C40 C41 174.4(9) . . . . ?
N7 C39 C40 C45 -4.7(14) . . . . ?
C45 C40 C41 C42 -2.2(14) . . . . ?
C39 C40 C41 C42 178.7(9) . . . . ?
C40 C41 C42 C43 -0.3(16) . . . . ?
C41 C42 C43 C44 0.9(16) . . . . ?
C42 C43 C44 C45 0.9(15) . . . . ?
U2 O6 C45 C40 12.4(15) . . . . ?
U2 O6 C45 C44 -169.0(7) . . . . ?
C41 C40 C45 O6 -177.4(8) . . . . ?
C39 C40 C45 O6 1.7(13) . . . . ?
C41 C40 C45 C44 3.9(13) . . . . ?
C39 C40 C45 C44 -177.0(8) . . . . ?
C43 C44 C45 O6 178.0(9) . . . . ?
C43 C44 C45 C40 -3.3(13) . . . . ?
C37 N6 C46 C47 -178.0(7) . . . . ?
C36 N6 C46 C47 -60.4(9) . . . . ?
U2 N6 C46 C47 65.1(7) . . . . ?
C48 N8 C47 C46 -112.8(9) . . . . ?
Fe1 N8 C47 C46 75.0(8) . . . . ?
N6 C46 C47 N8 -142.4(7) . . . . ?
C47 N8 C48 C49 -175.2(9) . . . . ?
Fe1 N8 C48 C49 -3.9(14) . . . . ?
N8 C48 C49 C50 -178.6(10) . . . . ?
N8 C48 C49 C54 1.6(16) . . . . ?
C54 C49 C50 C51 0.4(17) . . . . ?
C48 C49 C50 C51 -179.3(11) . . . . ?
C49 C50 C51 C52 2.4(19) . . . . ?
C50 C51 C52 C53 -2(2) . . . . ?
C51 C52 C53 C54 -1(2) . . . . ?
Fe1 O8 C54 C53 -173.9(7) . . . . ?
Fe1 O8 C54 C49 3.3(15) . . . . ?
C52 C53 C54 O8 -178.6(10) . . . . ?
C52 C53 C54 C49 4.0(16) . . . . ?
C50 C49 C54 O8 179.2(10) . . . . ?
C48 C49 C54 O8 -1.0(16) . . . . ?
C50 C49 C54 C53 -3.5(15) . . . . ?
C48 C49 C54 C53 176.2(9) . . . . ?
C59 N9 C55 C56 1.4(15) . . . . ?
Fe1 N9 C55 C56 168.7(8) . . . . ?
N9 C55 C56 C57 -1.5(17) . . . . ?
C55 C56 C57 C58 0.6(17) . . . . ?
C56 C57 C58 C59 0.4(19) . . . . ?
C55 N9 C59 C58 -0.4(16) . . . . ?
Fe1 N9 C59 C58 -167.1(9) . . . . ?
C57 C58 C59 N9 -0.5(19) . . . . ?

_refine_diff_density_max         1.896
_refine_diff_density_min         -3.104
_refine_diff_density_rms         0.191



