# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_5-bUP-296K
_database_code_depnum_ccdc_archive 'CCDC 1534046'
_audit_update_record             
;
2017-02-22 deposited with the CCDC.
2017-05-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C108 H112 Br2 N52 O34 U'
_chemical_formula_weight         3080.34

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'
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'
Br Br -0.2901 2.4595 '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                   12.7846(5)
_cell_length_b                   14.7915(6)
_cell_length_c                   17.0792(7)
_cell_angle_alpha                91.261(2)
_cell_angle_beta                 97.291(2)
_cell_angle_gamma                93.699(2)
_cell_volume                     3195.5(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9577
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      27.60

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_F_000             1558
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    1.995
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            72367
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.978
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             14613
_reflns_number_gt                13732
_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       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1100P)²+9.7677P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14613
_refine_ls_number_parameters     889
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0573
_refine_ls_wR_factor_ref         0.1683
_refine_ls_wR_factor_gt          0.1614
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.031
_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 1.0000 0.0000 0.5000 0.02624(9) Uani 1 2 d S . P . .
N1 N 0.6946(3) 0.3273(3) 0.3753(2) 0.0268(7) Uani 1 1 d . . . . .
C1 C 0.9447(4) 0.1557(4) 0.3607(3) 0.0340(10) Uani 1 1 d . . . . .
O1 O 1.0706(3) 0.0997(3) 0.5403(3) 0.0532(11) Uani 1 1 d . . . . .
N2 N 0.6252(3) 0.0599(3) 0.7752(2) 0.0276(8) Uani 1 1 d . . . . .
C2 C 0.8563(3) 0.2173(3) 0.3678(2) 0.0259(8) Uani 1 1 d . . . . .
O2 O 0.9343(4) 0.0789(3) 0.3945(2) 0.0548(12) Uani 1 1 d . . . . .
O3 O 1.0122(3) 0.1775(3) 0.3202(3) 0.0565(12) Uani 1 1 d . . . . .
N3 N 0.8582(3) 0.5431(3) 0.6088(2) 0.0304(8) Uani 1 1 d . . . . .
C3 C 0.8595(3) 0.3016(3) 0.3353(3) 0.0297(9) Uani 1 1 d . . . . .
H3 H 0.9167 0.3210 0.3100 0.036 Uiso 1 1 calc R U . . .
O4 O 0.8675(3) 0.0388(3) 0.5711(2) 0.0410(8) Uani 1 1 d . . . . .
N4 N 0.8010(3) 0.4242(3) 0.6723(2) 0.0319(8) Uani 1 1 d . . . . .
C4 C 0.7782(4) 0.3571(3) 0.3403(3) 0.0320(9) Uani 1 1 d . . . . .
H4 H 0.7811 0.4147 0.3196 0.038 Uiso 1 1 calc R U . . .
O5 O 0.7143(4) -0.0249(4) 0.5110(3) 0.0661(15) Uani 1 1 d . . . . .
N5 N 0.6748(3) 0.2979(3) 0.6844(2) 0.0326(8) Uani 1 1 d . . . . .
C5 C 0.6882(4) 0.2455(3) 0.4067(3) 0.0307(9) Uani 1 1 d . . . . .
H5 H 0.6287 0.2267 0.4298 0.037 Uiso 1 1 calc R U . . .
O6 O 0.6668(3) 0.2181(3) 0.5660(2) 0.0402(8) Uani 1 1 d . . . . .
N6 N 0.5237(3) 0.2242(3) 0.6356(2) 0.0324(8) Uani 1 1 d . . . . .
C6 C 0.7696(4) 0.1889(3) 0.4049(3) 0.0306(9) Uani 1 1 d . . . . .
H6 H 0.7666 0.1327 0.4282 0.037 Uiso 1 1 calc R U . . .
N7 N 0.3745(3) 0.2219(3) 0.5340(2) 0.0317(8) Uani 1 1 d . . . . .
C7 C 0.6047(4) 0.3857(4) 0.3776(3) 0.0346(10) Uani 1 1 d . . . . .
H7A H 0.5391 0.3505 0.3593 0.041 Uiso 1 1 calc R U . . .
H7B H 0.6119 0.4352 0.3420 0.041 Uiso 1 1 calc R U . . .
C55 C 0.3763(4) 0.2310(3) 0.4542(3) 0.0283(9) Uani 1 1 d . . . . .
O8 O 0.4475(3) 0.2132(2) 0.4176(2) 0.0376(8) Uani 1 1 d . . . . .
N8 N 0.2812(3) 0.2632(3) 0.4239(2) 0.0298(8) Uani 1 1 d . . . . .
C8 C 0.5996(4) 0.4238(3) 0.4599(3) 0.0315(9) Uani 1 1 d . . . . .
H8A H 0.6642 0.4605 0.4780 0.038 Uiso 1 1 calc R U . . .
H8B H 0.5932 0.3746 0.4960 0.038 Uiso 1 1 calc R U . . .
O9 O 0.6039(3) 0.6358(2) 0.7500(2) 0.0299(7) Uani 1 1 d . . . . .
N9 N 0.1810(3) 0.3587(3) 0.5011(2) 0.0278(7) Uani 1 1 d . . . . .
C9 C 0.5055(4) 0.4812(3) 0.4593(3) 0.0336(10) Uani 1 1 d . . . . .
H9A H 0.5133 0.5310 0.4241 0.040 Uiso 1 1 calc R U . . .
H9B H 0.4417 0.4447 0.4391 0.040 Uiso 1 1 calc R U . . .
O00D O 0.8499(3) 0.4013(3) 0.5480(2) 0.0416(8) Uani 1 1 d . . . . .
O10 O 0.4305(3) 0.4740(2) 0.7684(2) 0.0355(7) Uani 1 1 d . . . . .
N10 N 0.2728(3) 0.3159(3) 0.6109(2) 0.0283(8) Uani 1 1 d . . . . .
C10 C 0.7696(4) 0.0094(3) 0.5682(3) 0.0337(10) Uani 1 1 d . . . . .
O11 O 0.1917(3) 0.4499(2) 0.6137(2) 0.0370(8) Uani 1 1 d . . . . .
N11 N 0.4293(3) 0.3328(3) 0.7066(2) 0.0285(8) Uani 1 1 d . . . . .
C11 C 0.7225(4) 0.0267(3) 0.6442(3) 0.0252(8) Uani 1 1 d . . . . .
O12 O 0.6373(3) -0.1495(2) 0.79941(18) 0.0288(6) Uani 1 1 d . . . . .
N12 N 0.5821(3) 0.3987(3) 0.7632(2) 0.0286(8) Uani 1 1 d . . . . .
C12 C 0.6188(4) -0.0037(3) 0.6469(3) 0.0311(9) Uani 1 1 d . . . . .
H12 H 0.5804 -0.0358 0.6041 0.037 Uiso 1 1 calc R U . . .
O13 O 0.3634(3) -0.0729(3) 0.7377(2) 0.0372(8) Uani 1 1 d . . . . .
N13 N 0.7166(3) 0.5208(3) 0.7611(2) 0.0276(7) Uani 1 1 d . . . . .
C13 C 0.5729(4) 0.0140(3) 0.7134(3) 0.0336(10) Uani 1 1 d . . . . .
H13 H 0.5030 -0.0068 0.7152 0.040 Uiso 1 1 calc R U . . .
O14 O 0.3150(3) 0.1342(2) 0.7945(2) 0.0385(8) Uani 1 1 d . . . . .
N14 N 0.7502(3) 0.6347(3) 0.6840(2) 0.0273(7) Uani 1 1 d . . . . .
C14 C 0.7278(4) 0.0880(3) 0.7755(3) 0.0322(9) Uani 1 1 d . . . . .
H14 H 0.7650 0.1182 0.8198 0.039 Uiso 1 1 calc R U . . .
O15 O 0.5060(3) 0.2855(3) 0.8915(2) 0.0398(8) Uani 1 1 d . . . . .
N15 N 0.5356(3) 0.3150(3) 1.0257(2) 0.0312(8) Uani 1 1 d . . . . .
C15 C 0.7777(4) 0.0718(3) 0.7099(3) 0.0326(10) Uani 1 1 d . . . . .
H15 H 0.8483 0.0912 0.7099 0.039 Uiso 1 1 calc R U . . .
O16 O 0.2379(3) -0.2060(3) 1.0531(2) 0.0462(9) Uani 1 1 d . . . . .
N16 N 0.3704(3) 0.2852(3) 0.9693(2) 0.0306(8) Uani 1 1 d . . . . .
C16 C 0.5683(5) 0.0824(3) 0.8437(3) 0.0373(12) Uani 1 1 d . . . . .
H16A H 0.4964 0.0950 0.8238 0.045 Uiso 1 1 calc R U . . .
H16B H 0.6024 0.1371 0.8703 0.045 Uiso 1 1 calc R U . . .
O17 O 0.1569(3) 0.0131(3) 1.1015(2) 0.0381(8) Uani 1 1 d . . . . .
N17 N 0.2340(4) 0.1843(3) 0.8987(2) 0.0346(9) Uani 1 1 d . . . . .
C17 C 0.5650(4) 0.0084(3) 0.9029(3) 0.0277(9) Uani 1 1 d . . . . .
H17A H 0.6365 -0.0045 0.9237 0.033 Uiso 1 1 calc R U . . .
H17B H 0.5299 -0.0465 0.8772 0.033 Uiso 1 1 calc R U . . .
N18 N 0.1813(3) 0.0495(3) 0.8427(2) 0.0312(8) Uani 1 1 d . . . . .
C18 C 0.5056(4) 0.0376(3) 0.9707(3) 0.0309(10) Uani 1 1 d . . . . .
H18A H 0.5433 0.0905 0.9981 0.037 Uiso 1 1 calc R U . . .
H18B H 0.4359 0.0545 0.9492 0.037 Uiso 1 1 calc R U . . .
N19 N 0.2188(3) -0.1015(3) 0.8030(2) 0.0308(8) Uani 1 1 d . . . . .
C19 C 0.6816(3) 0.6008(3) 0.7330(2) 0.0231(8) Uani 1 1 d . . . . .
N22 N 0.6881(3) -0.2347(3) 0.9072(2) 0.0287(8) Uani 1 1 d . . . . .
C22 C 0.8378(3) 0.4508(3) 0.6039(3) 0.0287(9) Uani 1 1 d . . . . .
N21 N 0.5179(3) -0.2431(2) 0.8568(2) 0.0239(7) Uani 1 1 d . . . . .
C21 C 0.8129(3) 0.4972(3) 0.7315(3) 0.0281(9) Uani 1 1 d . . . . .
H21 H 0.8686 0.4868 0.7747 0.034 Uiso 1 1 calc R U . . .
N20 N 0.3422(3) -0.2003(3) 0.8099(2) 0.0300(8) Uani 1 1 d . . . . .
C20 C 0.8421(3) 0.5810(3) 0.6847(3) 0.0273(9) Uani 1 1 d . . . . .
H20 H 0.9063 0.6146 0.7106 0.033 Uiso 1 1 calc R U . . .
N23 N 0.2947(3) -0.2520(3) 0.9366(2) 0.0310(8) Uani 1 1 d . . . . .
C23 C 0.6554(4) 0.4640(3) 0.8087(3) 0.0294(9) Uani 1 1 d . . . . .
H23A H 0.7034 0.4320 0.8451 0.035 Uiso 1 1 calc R U . . .
H23B H 0.6163 0.5022 0.8397 0.035 Uiso 1 1 calc R U . . .
N24 N 0.1778(3) -0.1472(3) 0.9330(2) 0.0339(9) Uani 1 1 d . . . . .
C24 C 0.7848(4) 0.3294(3) 0.6902(3) 0.0342(10) Uani 1 1 d . . . . .
H24A H 0.8190 0.2933 0.6541 0.041 Uiso 1 1 calc R U . . .
H24B H 0.8184 0.3201 0.7433 0.041 Uiso 1 1 calc R U . . .
N25 N 0.1219(3) 0.0009(3) 0.9661(2) 0.0342(9) Uani 1 1 d . . . . .
C25 C 0.4758(4) 0.4090(3) 0.7484(3) 0.0272(9) Uani 1 1 d . . . . .
N26 N 0.1707(3) 0.1359(3) 1.0215(2) 0.0309(8) Uani 1 1 d . . . . .
C26 C 0.6084(4) 0.3079(3) 0.7464(3) 0.0261(8) Uani 1 1 d . . . . .
H26 H 0.6373 0.2787 0.7946 0.031 Uiso 1 1 calc R U . . .
C29 C 0.3161(4) 0.3163(3) 0.6932(3) 0.0306(9) Uani 1 1 d . . . . .
H29A H 0.2843 0.3626 0.7215 0.037 Uiso 1 1 calc R U . . .
H29B H 0.2971 0.2583 0.7147 0.037 Uiso 1 1 calc R U . . .
C28 C 0.6259(4) 0.2450(3) 0.6221(3) 0.0297(9) Uani 1 1 d . . . . .
C27 C 0.5013(4) 0.2603(3) 0.7106(3) 0.0276(9) Uani 1 1 d . . . . .
H27 H 0.4788 0.2119 0.7442 0.033 Uiso 1 1 calc R U . . .
C30 C 0.4494(4) 0.1694(3) 0.5807(3) 0.0355(10) Uani 1 1 d . . . . .
H30A H 0.4111 0.1257 0.6098 0.043 Uiso 1 1 calc R U . . .
H30B H 0.4881 0.1360 0.5456 0.043 Uiso 1 1 calc R U . . .
C31 C 0.2138(3) 0.3821(3) 0.5791(3) 0.0261(8) Uani 1 1 d . . . . .
C32 C 0.2731(4) 0.2376(3) 0.5576(3) 0.0277(9) Uani 1 1 d . . . . .
H32 H 0.2401 0.1829 0.5781 0.033 Uiso 1 1 calc R U . . .
C33 C 0.2076(3) 0.2683(3) 0.4809(3) 0.0262(8) Uani 1 1 d . . . . .
H33 H 0.1442 0.2278 0.4658 0.031 Uiso 1 1 calc R U . . .
C34 C 0.1022(3) 0.4067(4) 0.4539(3) 0.0310(9) Uani 1 1 d . . . . .
H34A H 0.0722 0.4484 0.4881 0.037 Uiso 1 1 calc R U . . .
H34B H 0.0458 0.3634 0.4311 0.037 Uiso 1 1 calc R U . . .
C35 C 0.2513(4) 0.2720(3) 0.3398(3) 0.0288(9) Uani 1 1 d . . . . .
H35A H 0.3007 0.2413 0.3115 0.035 Uiso 1 1 calc R U . . .
H35B H 0.1817 0.2419 0.3249 0.035 Uiso 1 1 calc R U . . .
C36 C 0.6489(4) 0.3284(3) 1.0326(3) 0.0339(10) Uani 1 1 d . . . . .
H36A H 0.6712 0.3811 1.0668 0.041 Uiso 1 1 calc R U . . .
H36B H 0.6689 0.3414 0.9809 0.041 Uiso 1 1 calc R U . . .
C37 C 0.4742(4) 0.2931(3) 0.9554(3) 0.0300(9) Uani 1 1 d . . . . .
C38 C 0.4743(4) 0.3187(3) 1.0912(2) 0.0258(8) Uani 1 1 d . . . . .
H38 H 0.4884 0.3767 1.1208 0.031 Uiso 1 1 calc R U . . .
C39 C 0.2841(4) 0.2742(3) 0.9064(3) 0.0344(10) Uani 1 1 d . . . . .
H39A H 0.2318 0.3166 0.9157 0.041 Uiso 1 1 calc R U . . .
H39B H 0.3102 0.2894 0.8571 0.041 Uiso 1 1 calc R U . . .
C40 C 0.2509(4) 0.1239(3) 0.8404(3) 0.0289(9) Uani 1 1 d . . . . .
C41 C 0.1449(4) 0.1555(3) 0.9391(3) 0.0298(9) Uani 1 1 d . . . . .
H41 H 0.0884 0.1974 0.9312 0.036 Uiso 1 1 calc R U . . .
C42 C 0.1093(3) 0.0609(3) 0.9001(3) 0.0312(9) Uani 1 1 d . . . . .
H42 H 0.0358 0.0586 0.8750 0.037 Uiso 1 1 calc R U . . .
C43 C 0.2015(4) 0.2050(3) 1.0837(3) 0.0309(9) Uani 1 1 d . . . . .
H43A H 0.1602 0.2570 1.0723 0.037 Uiso 1 1 calc R U . . .
H43B H 0.1843 0.1812 1.1333 0.037 Uiso 1 1 calc R U . . .
C44 C 0.1520(3) 0.0465(3) 1.0367(3) 0.0301(9) Uani 1 1 d . . . . .
C45 C 0.0960(4) -0.0961(4) 0.9600(3) 0.0369(11) Uani 1 1 d . . . . .
H45A H 0.0825 -0.1172 1.0114 0.044 Uiso 1 1 calc R U . . .
H45B H 0.0315 -0.1080 0.9238 0.044 Uiso 1 1 calc R U . . .
C46 C 0.1667(4) -0.0204(3) 0.7817(3) 0.0324(10) Uani 1 1 d . . . . .
H46A H 0.1930 0.0034 0.7349 0.039 Uiso 1 1 calc R U . . .
H46B H 0.0916 -0.0361 0.7683 0.039 Uiso 1 1 calc R U . . .
C47 C 0.2367(4) -0.2024(3) 0.9820(3) 0.0320(9) Uani 1 1 d . . . . .
C48 C 0.1782(3) -0.1720(3) 0.8500(3) 0.0285(9) Uani 1 1 d . . . . .
H48 H 0.1088 -0.1979 0.8259 0.034 Uiso 1 1 calc R U . . .
C49 C 0.2624(3) -0.2428(3) 0.8530(3) 0.0279(9) Uani 1 1 d . . . . .
H49 H 0.2329 -0.3007 0.8277 0.033 Uiso 1 1 calc R U . . .
C50 C 0.3143(3) -0.1197(3) 0.7799(3) 0.0272(9) Uani 1 1 d . . . . .
C51 C 0.4343(4) -0.2442(3) 0.7912(3) 0.0284(9) Uani 1 1 d . . . . .
H51A H 0.4612 -0.2140 0.7472 0.034 Uiso 1 1 calc R U . . .
H51B H 0.4134 -0.3065 0.7745 0.034 Uiso 1 1 calc R U . . .
C52 C 0.6168(3) -0.2033(3) 0.8485(2) 0.0232(8) Uani 1 1 d . . . . .
C53 C 0.6421(4) -0.3071(3) 0.9497(3) 0.0266(8) Uani 1 1 d . . . . .
H53 H 0.6786 -0.3629 0.9453 0.032 Uiso 1 1 calc R U . . .
Br1 Br 0.0330(2) 0.6164(2) 0.88019(19) 0.2542(18) Uani 1 1 d . 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 O1 1.758(4) . ?
U1 O1 1.758(4) 2_756 ?
U1 O2 2.269(4) . ?
U1 O2 2.269(4) 2_756 ?
U1 O4 2.301(3) 2_756 ?
U1 O4 2.301(3) . ?
N1 C5 1.336(6) . ?
N1 C4 1.346(6) . ?
N1 C7 1.485(6) . ?
C1 O3 1.204(7) . ?
C1 O2 1.292(7) . ?
C1 C2 1.511(6) . ?
N2 C13 1.323(7) . ?
N2 C14 1.350(6) . ?
N2 C16 1.496(5) . ?
C2 C3 1.376(7) . ?
C2 C6 1.392(6) . ?
N3 C22 1.372(6) . ?
N3 C34 1.442(6) 2_666 ?
N3 C20 1.445(6) . ?
C3 C4 1.375(7) . ?
C3 H3 0.9300 . ?
O4 C10 1.292(6) . ?
N4 C22 1.370(6) . ?
N4 C24 1.449(6) . ?
N4 C21 1.450(6) . ?
C4 H4 0.9300 . ?
O5 C10 1.212(7) . ?
N5 C28 1.366(6) . ?
N5 C24 1.443(6) . ?
N5 C26 1.449(6) . ?
C5 C6 1.380(7) . ?
C5 H5 0.9300 . ?
O6 C28 1.220(6) . ?
N6 C28 1.372(7) . ?
N6 C30 1.442(6) . ?
N6 C27 1.445(6) . ?
C6 H6 0.9300 . ?
N7 C55 1.375(6) . ?
N7 C32 1.438(6) . ?
N7 C30 1.444(6) . ?
C7 C8 1.513(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C55 O8 1.207(6) . ?
C55 N8 1.377(6) . ?
N8 C33 1.440(6) . ?
N8 C35 1.450(6) . ?
C8 C9 1.516(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
O9 C19 1.214(5) . ?
N9 C31 1.373(6) . ?
N9 C34 1.442(6) . ?
N9 C33 1.447(6) . ?
C9 C9 1.512(9) 2_666 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
O00D C22 1.222(6) . ?
O10 C25 1.218(6) . ?
N10 C31 1.356(6) . ?
N10 C29 1.443(6) . ?
N10 C32 1.457(6) . ?
C10 C11 1.522(6) . ?
O11 C31 1.220(6) . ?
N11 C25 1.380(6) . ?
N11 C29 1.440(6) . ?
N11 C27 1.455(6) . ?
C11 C12 1.379(6) . ?
C11 C15 1.381(7) . ?
O12 C52 1.209(5) . ?
N12 C25 1.370(6) . ?
N12 C26 1.436(6) . ?
N12 C23 1.443(6) . ?
C12 C13 1.371(6) . ?
C12 H12 0.9300 . ?
O13 C50 1.213(6) . ?
N13 C19 1.367(6) . ?
N13 C23 1.443(6) . ?
N13 C21 1.450(6) . ?
C13 H13 0.9300 . ?
O14 C40 1.210(6) . ?
N14 C19 1.368(5) . ?
N14 C35 1.448(6) 2_666 ?
N14 C20 1.459(6) . ?
C14 C15 1.382(6) . ?
C14 H14 0.9300 . ?
O15 C37 1.217(6) . ?
N15 C37 1.368(6) . ?
N15 C36 1.438(6) . ?
N15 C38 1.448(5) . ?
C15 H15 0.9300 . ?
O16 C47 1.216(6) . ?
N16 C37 1.376(6) . ?
N16 C39 1.438(6) . ?
N16 C53 1.445(5) 2_657 ?
C16 C17 1.509(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
O17 C44 1.217(6) . ?
N17 C40 1.370(6) . ?
N17 C39 1.435(6) . ?
N17 C41 1.451(6) . ?
C17 C18 1.531(5) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
N18 C40 1.374(6) . ?
N18 C46 1.439(6) . ?
N18 C42 1.441(6) . ?
C18 C18 1.525(8) 2_657 ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
N19 C50 1.370(6) . ?
N19 C48 1.439(6) . ?
N19 C46 1.441(6) . ?
N22 C52 1.377(6) . ?
N22 C43 1.439(6) 2_657 ?
N22 C53 1.443(6) . ?
N21 C52 1.384(6) . ?
N21 C38 1.445(6) 2_657 ?
N21 C51 1.447(6) . ?
C21 C20 1.541(6) . ?
C21 H21 0.9800 . ?
N20 C50 1.359(6) . ?
N20 C51 1.447(6) . ?
N20 C49 1.451(5) . ?
C20 H20 0.9800 . ?
N23 C47 1.371(6) . ?
N23 C49 1.448(6) . ?
N23 C36 1.452(6) 2_657 ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
N24 C47 1.372(7) . ?
N24 C45 1.445(6) . ?
N24 C48 1.458(6) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
N25 C44 1.368(7) . ?
N25 C45 1.449(7) . ?
N25 C42 1.450(6) . ?
N26 C44 1.365(6) . ?
N26 C41 1.443(6) . ?
N26 C43 1.457(6) . ?
C26 C27 1.545(6) . ?
C26 H26 0.9800 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C27 H27 0.9800 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C32 C33 1.556(6) . ?
C32 H32 0.9800 . ?
C33 H33 0.9800 . ?
C34 N3 1.442(6) 2_666 ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 N14 1.448(6) 2_666 ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 N23 1.452(6) 2_657 ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C38 N21 1.445(6) 2_657 ?
C38 C53 1.558(6) 2_657 ?
C38 H38 0.9800 . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C41 C42 1.551(7) . ?
C41 H41 0.9800 . ?
C42 H42 0.9800 . ?
C43 N22 1.439(6) 2_657 ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C48 C49 1.547(6) . ?
C48 H48 0.9800 . ?
C49 H49 0.9800 . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C53 N16 1.445(5) 2_657 ?
C53 C38 1.558(6) 2_657 ?
C53 H53 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
O1 U1 O1 180.0 . 2_756 ?
O1 U1 O2 89.2(2) . . ?
O1 U1 O2 90.8(2) 2_756 . ?
O1 U1 O2 90.8(2) . 2_756 ?
O1 U1 O2 89.2(2) 2_756 2_756 ?
O2 U1 O2 180.00(14) . 2_756 ?
O1 U1 O4 93.45(17) . 2_756 ?
O1 U1 O4 86.55(17) 2_756 2_756 ?
O2 U1 O4 87.76(15) . 2_756 ?
O2 U1 O4 92.24(15) 2_756 2_756 ?
O1 U1 O4 86.55(17) . . ?
O1 U1 O4 93.45(17) 2_756 . ?
O2 U1 O4 92.24(15) . . ?
O2 U1 O4 87.76(15) 2_756 . ?
O4 U1 O4 180.0 2_756 . ?
C5 N1 C4 122.1(4) . . ?
C5 N1 C7 118.5(4) . . ?
C4 N1 C7 119.4(4) . . ?
O3 C1 O2 125.8(5) . . ?
O3 C1 C2 119.3(5) . . ?
O2 C1 C2 114.6(4) . . ?
C13 N2 C14 120.4(4) . . ?
C13 N2 C16 119.1(4) . . ?
C14 N2 C16 120.5(4) . . ?
C3 C2 C6 119.2(4) . . ?
C3 C2 C1 120.0(4) . . ?
C6 C2 C1 120.8(4) . . ?
C1 O2 U1 142.8(4) . . ?
C22 N3 C34 122.3(4) . 2_666 ?
C22 N3 C20 112.2(4) . . ?
C34 N3 C20 125.3(4) 2_666 . ?
C4 C3 C2 120.2(4) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C10 O4 U1 132.3(3) . . ?
C22 N4 C24 121.8(4) . . ?
C22 N4 C21 111.9(4) . . ?
C24 N4 C21 123.6(4) . . ?
N1 C4 C3 119.4(4) . . ?
N1 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C28 N5 C24 122.1(4) . . ?
C28 N5 C26 112.5(4) . . ?
C24 N5 C26 124.9(4) . . ?
N1 C5 C6 120.2(4) . . ?
N1 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C28 N6 C30 122.2(4) . . ?
C28 N6 C27 112.9(4) . . ?
C30 N6 C27 124.8(4) . . ?
C5 C6 C2 118.9(4) . . ?
C5 C6 H6 120.5 . . ?
C2 C6 H6 120.5 . . ?
C55 N7 C32 112.5(4) . . ?
C55 N7 C30 121.6(4) . . ?
C32 N7 C30 121.8(4) . . ?
N1 C7 C8 111.9(4) . . ?
N1 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
N1 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
O8 C55 N7 126.3(5) . . ?
O8 C55 N8 126.6(4) . . ?
N7 C55 N8 107.1(4) . . ?
C55 N8 C33 113.4(4) . . ?
C55 N8 C35 122.1(4) . . ?
C33 N8 C35 123.2(4) . . ?
C7 C8 C9 109.8(4) . . ?
C7 C8 H8A 109.7 . . ?
C9 C8 H8A 109.7 . . ?
C7 C8 H8B 109.7 . . ?
C9 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
C31 N9 C34 122.0(4) . . ?
C31 N9 C33 112.1(4) . . ?
C34 N9 C33 123.3(4) . . ?
C9 C9 C8 112.2(5) 2_666 . ?
C9 C9 H9A 109.2 2_666 . ?
C8 C9 H9A 109.2 . . ?
C9 C9 H9B 109.2 2_666 . ?
C8 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C31 N10 C29 123.1(4) . . ?
C31 N10 C32 113.2(4) . . ?
C29 N10 C32 122.9(4) . . ?
O5 C10 O4 126.2(5) . . ?
O5 C10 C11 119.8(5) . . ?
O4 C10 C11 113.9(4) . . ?
C25 N11 C29 121.1(4) . . ?
C25 N11 C27 110.8(4) . . ?
C29 N11 C27 122.9(4) . . ?
C12 C11 C15 118.5(4) . . ?
C12 C11 C10 118.0(4) . . ?
C15 C11 C10 123.5(4) . . ?
C25 N12 C26 112.6(4) . . ?
C25 N12 C23 123.2(4) . . ?
C26 N12 C23 122.6(4) . . ?
C13 C12 C11 119.3(5) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C19 N13 C23 121.5(4) . . ?
C19 N13 C21 112.8(4) . . ?
C23 N13 C21 125.4(4) . . ?
N2 C13 C12 121.8(4) . . ?
N2 C13 H13 119.1 . . ?
C12 C13 H13 119.1 . . ?
C19 N14 C35 120.7(4) . 2_666 ?
C19 N14 C20 111.7(4) . . ?
C35 N14 C20 123.8(4) 2_666 . ?
N2 C14 C15 119.9(5) . . ?
N2 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C37 N15 C36 122.7(4) . . ?
C37 N15 C38 112.5(4) . . ?
C36 N15 C38 124.7(4) . . ?
C11 C15 C14 119.9(4) . . ?
C11 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C37 N16 C39 122.2(4) . . ?
C37 N16 C53 112.8(4) . 2_657 ?
C39 N16 C53 123.8(4) . 2_657 ?
N2 C16 C17 114.0(4) . . ?
N2 C16 H16A 108.7 . . ?
C17 C16 H16A 108.7 . . ?
N2 C16 H16B 108.7 . . ?
C17 C16 H16B 108.7 . . ?
H16A C16 H16B 107.6 . . ?
C40 N17 C39 122.4(4) . . ?
C40 N17 C41 112.8(4) . . ?
C39 N17 C41 123.4(4) . . ?
C16 C17 C18 110.3(3) . . ?
C16 C17 H17A 109.6 . . ?
C18 C17 H17A 109.6 . . ?
C16 C17 H17B 109.6 . . ?
C18 C17 H17B 109.6 . . ?
H17A C17 H17B 108.1 . . ?
C40 N18 C46 122.1(4) . . ?
C40 N18 C42 112.4(4) . . ?
C46 N18 C42 123.8(4) . . ?
C18 C18 C17 112.0(4) 2_657 . ?
C18 C18 H18A 109.2 2_657 . ?
C17 C18 H18A 109.2 . . ?
C18 C18 H18B 109.2 2_657 . ?
C17 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
C50 N19 C48 112.4(4) . . ?
C50 N19 C46 122.7(4) . . ?
C48 N19 C46 124.9(4) . . ?
O9 C19 N13 125.5(4) . . ?
O9 C19 N14 126.3(4) . . ?
N13 C19 N14 108.2(4) . . ?
C52 N22 C43 122.0(4) . 2_657 ?
C52 N22 C53 112.4(4) . . ?
C43 N22 C53 125.1(4) 2_657 . ?
O00D C22 N4 126.1(5) . . ?
O00D C22 N3 125.9(4) . . ?
N4 C22 N3 108.0(4) . . ?
C52 N21 C38 111.3(3) . 2_657 ?
C52 N21 C51 119.5(4) . . ?
C38 N21 C51 120.3(4) 2_657 . ?
N13 C21 N4 115.7(4) . . ?
N13 C21 C20 102.9(4) . . ?
N4 C21 C20 103.2(4) . . ?
N13 C21 H21 111.5 . . ?
N4 C21 H21 111.5 . . ?
C20 C21 H21 111.5 . . ?
C50 N20 C51 123.0(4) . . ?
C50 N20 C49 112.6(4) . . ?
C51 N20 C49 123.8(4) . . ?
N3 C20 N14 115.1(4) . . ?
N3 C20 C21 103.5(4) . . ?
N14 C20 C21 103.5(3) . . ?
N3 C20 H20 111.4 . . ?
N14 C20 H20 111.4 . . ?
C21 C20 H20 111.4 . . ?
C47 N23 C49 112.1(4) . . ?
C47 N23 C36 122.0(4) . 2_657 ?
C49 N23 C36 122.2(4) . 2_657 ?
N12 C23 N13 113.7(4) . . ?
N12 C23 H23A 108.8 . . ?
N13 C23 H23A 108.8 . . ?
N12 C23 H23B 108.8 . . ?
N13 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
C47 N24 C45 122.0(4) . . ?
C47 N24 C48 112.0(4) . . ?
C45 N24 C48 122.2(4) . . ?
N5 C24 N4 113.6(4) . . ?
N5 C24 H24A 108.9 . . ?
N4 C24 H24A 108.9 . . ?
N5 C24 H24B 108.9 . . ?
N4 C24 H24B 108.9 . . ?
H24A C24 H24B 107.7 . . ?
C44 N25 C45 122.8(4) . . ?
C44 N25 C42 112.7(4) . . ?
C45 N25 C42 124.2(4) . . ?
O10 C25 N12 126.0(4) . . ?
O10 C25 N11 126.2(4) . . ?
N12 C25 N11 107.8(4) . . ?
C44 N26 C41 113.0(4) . . ?
C44 N26 C43 122.7(4) . . ?
C41 N26 C43 123.9(4) . . ?
N12 C26 N5 115.9(4) . . ?
N12 C26 C27 103.3(4) . . ?
N5 C26 C27 103.5(4) . . ?
N12 C26 H26 111.2 . . ?
N5 C26 H26 111.2 . . ?
C27 C26 H26 111.2 . . ?
N11 C29 N10 113.6(4) . . ?
N11 C29 H29A 108.8 . . ?
N10 C29 H29A 108.8 . . ?
N11 C29 H29B 108.8 . . ?
N10 C29 H29B 108.8 . . ?
H29A C29 H29B 107.7 . . ?
O6 C28 N5 126.1(5) . . ?
O6 C28 N6 126.0(5) . . ?
N5 C28 N6 107.8(4) . . ?
N6 C27 N11 116.0(4) . . ?
N6 C27 C26 103.1(4) . . ?
N11 C27 C26 103.6(3) . . ?
N6 C27 H27 111.2 . . ?
N11 C27 H27 111.2 . . ?
C26 C27 H27 111.2 . . ?
N6 C30 N7 113.1(4) . . ?
N6 C30 H30A 109.0 . . ?
N7 C30 H30A 109.0 . . ?
N6 C30 H30B 109.0 . . ?
N7 C30 H30B 109.0 . . ?
H30A C30 H30B 107.8 . . ?
O11 C31 N10 126.1(4) . . ?
O11 C31 N9 125.7(4) . . ?
N10 C31 N9 108.1(4) . . ?
N7 C32 N10 114.6(4) . . ?
N7 C32 C33 104.0(4) . . ?
N10 C32 C33 102.3(3) . . ?
N7 C32 H32 111.8 . . ?
N10 C32 H32 111.8 . . ?
C33 C32 H32 111.8 . . ?
N8 C33 N9 115.4(4) . . ?
N8 C33 C32 102.5(4) . . ?
N9 C33 C32 103.8(3) . . ?
N8 C33 H33 111.5 . . ?
N9 C33 H33 111.5 . . ?
C32 C33 H33 111.5 . . ?
N9 C34 N3 114.1(4) . 2_666 ?
N9 C34 H34A 108.7 . . ?
N3 C34 H34A 108.7 2_666 . ?
N9 C34 H34B 108.7 . . ?
N3 C34 H34B 108.7 2_666 . ?
H34A C34 H34B 107.6 . . ?
N14 C35 N8 113.2(4) 2_666 . ?
N14 C35 H35A 108.9 2_666 . ?
N8 C35 H35A 108.9 . . ?
N14 C35 H35B 108.9 2_666 . ?
N8 C35 H35B 108.9 . . ?
H35A C35 H35B 107.8 . . ?
N15 C36 N23 114.7(4) . 2_657 ?
N15 C36 H36A 108.6 . . ?
N23 C36 H36A 108.6 2_657 . ?
N15 C36 H36B 108.6 . . ?
N23 C36 H36B 108.6 2_657 . ?
H36A C36 H36B 107.6 . . ?
O15 C37 N15 125.7(5) . . ?
O15 C37 N16 126.3(5) . . ?
N15 C37 N16 107.9(4) . . ?
N21 C38 N15 115.4(4) 2_657 . ?
N21 C38 C53 103.3(3) 2_657 2_657 ?
N15 C38 C53 103.3(3) . 2_657 ?
N21 C38 H38 111.4 2_657 . ?
N15 C38 H38 111.4 . . ?
C53 C38 H38 111.4 2_657 . ?
N17 C39 N16 113.6(4) . . ?
N17 C39 H39A 108.8 . . ?
N16 C39 H39A 108.8 . . ?
N17 C39 H39B 108.8 . . ?
N16 C39 H39B 108.8 . . ?
H39A C39 H39B 107.7 . . ?
O14 C40 N17 126.2(5) . . ?
O14 C40 N18 125.9(5) . . ?
N17 C40 N18 107.9(4) . . ?
N26 C41 N17 115.4(4) . . ?
N26 C41 C42 103.3(4) . . ?
N17 C41 C42 102.8(4) . . ?
N26 C41 H41 111.6 . . ?
N17 C41 H41 111.6 . . ?
C42 C41 H41 111.6 . . ?
N18 C42 N25 114.9(4) . . ?
N18 C42 C41 103.9(4) . . ?
N25 C42 C41 103.0(4) . . ?
N18 C42 H42 111.5 . . ?
N25 C42 H42 111.5 . . ?
C41 C42 H42 111.5 . . ?
N22 C43 N26 114.0(4) 2_657 . ?
N22 C43 H43A 108.7 2_657 . ?
N26 C43 H43A 108.7 . . ?
N22 C43 H43B 108.7 2_657 . ?
N26 C43 H43B 108.7 . . ?
H43A C43 H43B 107.6 . . ?
O17 C44 N26 126.6(5) . . ?
O17 C44 N25 125.5(5) . . ?
N26 C44 N25 107.8(4) . . ?
N24 C45 N25 113.9(4) . . ?
N24 C45 H45A 108.8 . . ?
N25 C45 H45A 108.8 . . ?
N24 C45 H45B 108.8 . . ?
N25 C45 H45B 108.8 . . ?
H45A C45 H45B 107.7 . . ?
N18 C46 N19 114.0(4) . . ?
N18 C46 H46A 108.7 . . ?
N19 C46 H46A 108.7 . . ?
N18 C46 H46B 108.7 . . ?
N19 C46 H46B 108.7 . . ?
H46A C46 H46B 107.6 . . ?
O16 C47 N23 126.1(5) . . ?
O16 C47 N24 126.0(5) . . ?
N23 C47 N24 108.0(4) . . ?
N19 C48 N24 115.1(4) . . ?
N19 C48 C49 103.6(3) . . ?
N24 C48 C49 102.9(4) . . ?
N19 C48 H48 111.5 . . ?
N24 C48 H48 111.5 . . ?
C49 C48 H48 111.5 . . ?
N23 C49 N20 115.1(4) . . ?
N23 C49 C48 103.8(4) . . ?
N20 C49 C48 103.0(4) . . ?
N23 C49 H49 111.5 . . ?
N20 C49 H49 111.5 . . ?
C48 C49 H49 111.5 . . ?
O13 C50 N20 126.2(4) . . ?
O13 C50 N19 125.5(5) . . ?
N20 C50 N19 108.3(4) . . ?
N20 C51 N21 113.3(4) . . ?
N20 C51 H51A 108.9 . . ?
N21 C51 H51A 108.9 . . ?
N20 C51 H51B 108.9 . . ?
N21 C51 H51B 108.9 . . ?
H51A C51 H51B 107.7 . . ?
O12 C52 N22 125.7(4) . . ?
O12 C52 N21 126.5(4) . . ?
N22 C52 N21 107.8(4) . . ?
N22 C53 N16 115.5(4) . 2_657 ?
N22 C53 C38 103.2(3) . 2_657 ?
N16 C53 C38 102.7(3) 2_657 2_657 ?
N22 C53 H53 111.6 . . ?
N16 C53 H53 111.6 2_657 . ?
C38 C53 H53 111.6 2_657 . ?

_refine_diff_density_max         1.963
_refine_diff_density_min         -3.379
_refine_diff_density_rms         0.155

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_2-bUP-320K
_database_code_depnum_ccdc_archive 'CCDC 1534043'
_audit_update_record             
;
2017-03-04 deposited with the CCDC.
2017-05-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C108 H112 Br2 N52 O34 U'
_chemical_formula_weight         3080.34

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'
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'
Br Br -0.2901 2.4595 '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                   12.8248(15)
_cell_length_b                   14.8362(16)
_cell_length_c                   17.044(2)
_cell_angle_alpha                91.439(5)
_cell_angle_beta                 96.887(6)
_cell_angle_gamma                93.574(5)
_cell_volume                     3211.6(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    320(2)
_cell_measurement_reflns_used    9464
_cell_measurement_theta_min      3.04
_cell_measurement_theta_max      27.52

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_F_000             1558
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    1.985
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      320(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            81895
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.041
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             14709
_reflns_number_gt                14028
_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       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0933P)²+3.5401P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14709
_refine_ls_number_parameters     889
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0468
_refine_ls_wR_factor_ref         0.1357
_refine_ls_wR_factor_gt          0.1323
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.048
_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 0.5000 0.5000 0.5000 0.02777(7) Uani 1 2 d S . P . .
Br1 Br 0.4737(4) 0.8732(4) 1.1188(4) 0.467(4) Uani 1 1 d . U . . .
N1 N 0.1201(3) 0.5589(2) 0.77307(17) 0.0322(6) Uani 1 1 d . . . . .
C1 C 0.2673(3) 0.5084(3) 0.5662(2) 0.0357(8) Uani 1 1 d . . . . .
O1 O 0.5687(3) 0.5995(2) 0.5411(2) 0.0524(8) Uani 1 1 d . . . . .
O2 O 0.3649(2) 0.5359(2) 0.57055(18) 0.0445(7) Uani 1 1 d . . . . .
N2 N 0.8040(2) 0.1723(2) 0.62473(17) 0.0313(6) Uani 1 1 d . . . . .
C2 C 0.2185(3) 0.5252(2) 0.6419(2) 0.0289(7) Uani 1 1 d . . . . .
O4 O 0.5665(3) 0.4224(3) 0.6058(2) 0.0567(9) Uani 1 1 d . . . . .
N4 N 0.3775(3) 0.4998(2) 1.0302(2) 0.0410(7) Uani 1 1 d . . . . .
C4 C 0.2226(3) 0.5866(3) 0.7735(2) 0.0384(8) Uani 1 1 d . . . . .
H4 H 0.2592 0.6169 0.8178 0.046 Uiso 1 1 calc R U . . .
O5 O 0.4868(3) 0.3242(3) 0.6791(3) 0.0649(10) Uani 1 1 d . . . . .
N5 N 0.3274(3) 0.3649(2) 0.9748(2) 0.0372(7) Uani 1 1 d . . . . .
C6 C 0.1145(3) 0.4961(3) 0.6442(2) 0.0354(8) Uani 1 1 d . . . . .
H6 H 0.0765 0.4647 0.6009 0.042 Uiso 1 1 calc R U . . .
N6 N 0.1869(2) 0.2661(2) 0.90456(18) 0.0342(6) Uani 1 1 d . . . . .
O6 O 0.0022(3) 0.7843(2) 0.89118(16) 0.0464(7) Uani 1 1 d . . . . .
C7 C 0.0627(4) 0.5815(3) 0.8416(2) 0.0432(10) Uani 1 1 d . . . . .
H7A H -0.0095 0.5921 0.8220 0.052 Uiso 1 1 calc R U . . .
H7B H 0.0950 0.6371 0.8674 0.052 Uiso 1 1 calc R U . . .
N7 N 0.0170(2) 0.2572(2) 0.85618(16) 0.0291(6) Uani 1 1 d . . . . .
O7 O 0.2581(3) 0.7043(2) 0.94376(18) 0.0522(8) Uani 1 1 d . . . . .
C8 C 0.0625(3) 0.5086(3) 0.9019(2) 0.0328(7) Uani 1 1 d . . . . .
H8A H 0.1344 0.4979 0.9224 0.039 Uiso 1 1 calc R U . . .
H8B H 0.0297 0.4528 0.8768 0.039 Uiso 1 1 calc R U . . .
N8 N 0.0340(3) 0.8132(2) 1.02544(18) 0.0365(7) Uani 1 1 d . . . . .
O8 O 0.3408(2) 0.4870(2) 0.89466(18) 0.0458(7) Uani 1 1 d . . . . .
O9 O 0.1344(2) 0.35078(18) 0.79737(15) 0.0348(5) Uani 1 1 d . . . . .
N9 N -0.1313(3) 0.7840(2) 0.97082(18) 0.0362(7) Uani 1 1 d . . . . .
C10 C 0.5554(3) 0.3461(3) 0.6390(2) 0.0391(8) Uani 1 1 d . . . . .
N10 N -0.2695(3) 0.6834(2) 0.9007(2) 0.0395(7) Uani 1 1 d . . . . .
O10 O -0.1885(3) 0.6339(2) 0.79549(17) 0.0442(7) Uani 1 1 d . . . . .
C11 C 0.6436(3) 0.2841(3) 0.6322(2) 0.0317(7) Uani 1 1 d . . . . .
O11 O 1.1658(3) -0.2818(2) 0.56499(17) 0.0458(7) Uani 1 1 d . . . . .
N11 N 0.2042(3) 0.7520(2) 1.06154(19) 0.0365(7) Uani 1 1 d . . . . .
C12 C 0.7310(3) 0.3113(3) 0.5958(2) 0.0348(8) Uani 1 1 d . . . . .
H12 H 0.7354 0.3675 0.5730 0.042 Uiso 1 1 calc R U . . .
O12 O 0.9308(2) -0.0250(2) 0.76900(18) 0.0419(6) Uani 1 1 d . . . . .
N12 N -0.1591(2) 0.2990(2) 0.81095(19) 0.0354(7) Uani 1 1 d . . . . .
C13 C 0.8113(3) 0.2542(3) 0.5938(2) 0.0363(8) Uani 1 1 d . . . . .
H13 H 0.8709 0.2726 0.5708 0.044 Uiso 1 1 calc R U . . .
O13 O -0.1387(2) 0.4262(2) 0.73932(19) 0.0436(7) Uani 1 1 d . . . . .
N13 N 1.3012(3) -0.0753(2) 0.6702(2) 0.0389(7) Uani 1 1 d . . . . .
C14 C 0.7197(3) 0.1438(3) 0.6592(2) 0.0378(8) Uani 1 1 d . . . . .
H14 H 0.7157 0.0862 0.6795 0.045 Uiso 1 1 calc R U . . .
O14 O 1.1041(2) 0.13611(18) 0.74879(16) 0.0364(6) Uani 1 1 d . . . . .
N14 N 1.2154(3) 0.0207(2) 0.75854(19) 0.0338(6) Uani 1 1 d . . . . .
C15 C 0.6394(3) 0.1999(3) 0.6645(2) 0.0356(8) Uani 1 1 d . . . . .
H15 H 0.5820 0.1809 0.6899 0.043 Uiso 1 1 calc R U . . .
O15 O 1.3492(3) -0.0983(2) 0.54493(19) 0.0491(7) Uani 1 1 d . . . . .
N15 N 1.0823(3) -0.1004(2) 0.76387(19) 0.0342(6) Uani 1 1 d . . . . .
C16 C 0.8931(3) 0.1135(3) 0.6223(2) 0.0390(9) Uani 1 1 d . . . . .
H16A H 0.8848 0.0639 0.6575 0.047 Uiso 1 1 calc R U . . .
H16B H 0.9583 0.1481 0.6413 0.047 Uiso 1 1 calc R U . . .
O16 O 0.6930(3) -0.0502(2) 0.61607(18) 0.0446(7) Uani 1 1 d . . . . .
N16 N 0.9302(3) -0.1661(2) 0.70705(18) 0.0337(6) Uani 1 1 d . . . . .
C17 C 0.9001(3) 0.0758(3) 0.5402(2) 0.0358(8) Uani 1 1 d . . . . .
H17A H 0.9072 0.1251 0.5044 0.043 Uiso 1 1 calc R U . . .
H17B H 0.8361 0.0394 0.5214 0.043 Uiso 1 1 calc R U . . .
O17 O 0.9473(2) -0.2851(2) 0.41811(18) 0.0440(7) Uani 1 1 d . . . . .
N17 N 1.1744(3) -0.1999(2) 0.68287(19) 0.0379(7) Uani 1 1 d . . . . .
C18 C 0.9938(3) 0.0185(3) 0.5408(2) 0.0392(9) Uani 1 1 d . . . . .
H18A H 1.0572 0.0547 0.5614 0.047 Uiso 1 1 calc R U . . .
H18B H 0.9854 -0.0313 0.5757 0.047 Uiso 1 1 calc R U . . .
N18 N 1.0241(3) -0.2749(2) 0.6358(2) 0.0382(7) Uani 1 1 d . . . . .
C19 C 0.2605(3) 0.7015(3) 1.0148(2) 0.0381(8) Uani 1 1 d . . . . .
N19 N 0.7729(3) -0.1842(2) 0.61306(19) 0.0349(7) Uani 1 1 d . . . . .
C20 C 0.4023(3) 0.5961(3) 1.0356(3) 0.0432(9) Uani 1 1 d . . . . .
H20A H 0.4151 0.6169 0.9839 0.052 Uiso 1 1 calc R U . . .
H20B H 0.4666 0.6086 1.0714 0.052 Uiso 1 1 calc R U . . .
N20 N 0.2817(2) 0.6020(2) 1.1938(2) 0.0359(7) Uani 1 1 d . . . . .
C21 C 0.3462(3) 0.4541(3) 0.9594(2) 0.0356(8) Uani 1 1 d . . . . .
N21 N -0.3203(3) 0.5491(2) 0.84561(19) 0.0360(7) Uani 1 1 d . . . . .
C22 C 0.2971(3) 0.2962(3) 0.9125(2) 0.0372(8) Uani 1 1 d . . . . .
H22A H 0.3135 0.3202 0.8626 0.045 Uiso 1 1 calc R U . . .
H22B H 0.3388 0.2446 0.9232 0.045 Uiso 1 1 calc R U . . .
N22 N 1.3194(3) 0.1416(2) 0.49665(19) 0.0341(6) Uani 1 1 d . . . . .
C23 C 0.1149(3) 0.2972(2) 0.8467(2) 0.0287(7) Uani 1 1 d . . . . .
N23 N 1.3567(3) 0.0432(2) 0.6063(2) 0.0376(7) Uani 1 1 d . . . . .
C24 C 0.1473(3) 0.8273(3) 1.0310(3) 0.0412(9) Uani 1 1 d . . . . .
H24A H 0.1694 0.8803 1.0648 0.049 Uiso 1 1 calc R U . . .
H24B H 0.1664 0.8399 0.9788 0.049 Uiso 1 1 calc R U . . .
N24 N 1.2505(2) 0.1353(2) 0.68283(19) 0.0320(6) Uani 1 1 d . . . . .
C25 C -0.0278(3) 0.7920(2) 0.9556(2) 0.0341(8) Uani 1 1 d . . . . .
N25 N 0.8748(3) -0.2771(2) 0.5350(2) 0.0361(7) Uani 1 1 d . . . . .
C26 C -0.2179(4) 0.7738(3) 0.9092(2) 0.0410(9) Uani 1 1 d . . . . .
H26A H -0.1928 0.7893 0.8595 0.049 Uiso 1 1 calc R U . . .
H26B H -0.2695 0.8162 0.9197 0.049 Uiso 1 1 calc R U . . .
N26 N 0.7814(3) -0.2360(2) 0.42519(19) 0.0355(7) Uani 1 1 d . . . . .
C27 C -0.2515(3) 0.6232(3) 0.8431(2) 0.0335(7) Uani 1 1 d . . . . .
C28 C -0.0672(3) 0.2558(3) 0.7913(2) 0.0340(8) Uani 1 1 d . . . . .
H28A H -0.0411 0.2858 0.7469 0.041 Uiso 1 1 calc R U . . .
H28B H -0.0876 0.1935 0.7747 0.041 Uiso 1 1 calc R U . . .
C29 C 0.2377(3) 0.7425(3) 1.1446(2) 0.0335(7) Uani 1 1 d . . . . .
H29 H 0.2676 0.8001 1.1697 0.040 Uiso 1 1 calc R U . . .
C30 C 0.3214(3) 0.6721(3) 1.1464(2) 0.0343(8) Uani 1 1 d . . . . .
H30 H 0.3909 0.6978 1.1696 0.041 Uiso 1 1 calc R U . . .
C31 C 0.3911(3) 0.4408(3) 1.0956(2) 0.0370(8) Uani 1 1 d . . . . .
H31 H 0.4646 0.4435 1.1197 0.044 Uiso 1 1 calc R U . . .
C32 C 0.3558(3) 0.3457(3) 1.0569(2) 0.0360(8) Uani 1 1 d . . . . .
H32 H 0.4127 0.3044 1.0636 0.043 Uiso 1 1 calc R U . . .
C33 C 0.1425(3) 0.1943(2) 0.9475(2) 0.0319(7) Uani 1 1 d . . . . .
H33 H 0.1791 0.1388 0.9425 0.038 Uiso 1 1 calc R U . . .
C35 C 0.0257(3) 0.1821(2) 0.9079(2) 0.0303(7) Uani 1 1 d . . . . .
H35 H 0.0113 0.1241 0.8786 0.036 Uiso 1 1 calc R U . . .
C36 C 0.3340(3) 0.5220(3) 1.2153(2) 0.0372(8) Uani 1 1 d . . . . .
H36A H 0.3080 0.4987 1.2624 0.045 Uiso 1 1 calc R U . . .
H36B H 0.4087 0.5381 1.2283 0.045 Uiso 1 1 calc R U . . .
C37 C 1.1251(3) -0.2542(3) 0.6211(2) 0.0348(8) Uani 1 1 d . . . . .
C38 C 0.9764(3) -0.0896(2) 0.7492(2) 0.0323(7) Uani 1 1 d . . . . .
C39 C 1.0018(3) -0.2381(2) 0.7106(2) 0.0330(7) Uani 1 1 d . . . . .
H39 H 0.9796 -0.2861 0.7446 0.040 Uiso 1 1 calc R U . . .
C40 C 1.1089(3) -0.1905(2) 0.7459(2) 0.0321(7) Uani 1 1 d . . . . .
H40 H 1.1382 -0.2200 0.7937 0.039 Uiso 1 1 calc R U . . .
C41 C 0.8172(3) -0.1829(3) 0.6946(2) 0.0360(8) Uani 1 1 d . . . . .
H41A H 0.7989 -0.2406 0.7167 0.043 Uiso 1 1 calc R U . . .
H41B H 0.7855 -0.1366 0.7232 0.043 Uiso 1 1 calc R U . . .
C42 C 1.1552(3) -0.0346(3) 0.8075(2) 0.0339(7) Uani 1 1 d . . . . .
H42A H 1.2034 -0.0657 0.8441 0.041 Uiso 1 1 calc R U . . .
H42B H 1.1164 0.0043 0.8385 0.041 Uiso 1 1 calc R U . . .
C43 C 1.2841(3) -0.1695(3) 0.6880(3) 0.0397(8) Uani 1 1 d . . . . .
H43A H 1.3178 -0.2060 0.6516 0.048 Uiso 1 1 calc R U . . .
H43B H 1.3176 -0.1791 0.7410 0.048 Uiso 1 1 calc R U . . .
C44 C 1.3368(3) -0.0491(3) 0.6006(2) 0.0361(8) Uani 1 1 d . . . . .
C45 C 1.3116(3) -0.0026(3) 0.7293(2) 0.0333(7) Uani 1 1 d . . . . .
H45 H 1.3665 -0.0127 0.7728 0.040 Uiso 1 1 calc R U . . .
C46 C 1.1814(3) 0.1012(2) 0.73148(19) 0.0276(6) Uani 1 1 d . . . . .
C48 C -0.1871(3) 0.3800(3) 0.7816(2) 0.0319(7) Uani 1 1 d . . . . .
C47 C 0.7730(3) -0.2616(2) 0.5595(2) 0.0339(7) Uani 1 1 d . . . . .
H47 H 0.7406 -0.3163 0.5801 0.041 Uiso 1 1 calc R U . . .
C49 C 1.3413(3) 0.0814(3) 0.6823(2) 0.0330(7) Uani 1 1 d . . . . .
H49 H 1.4056 0.1143 0.7079 0.040 Uiso 1 1 calc R U . . .
C50 C 1.2486(3) 0.2279(2) 0.6588(2) 0.0345(8) Uani 1 1 d . . . . .
H50A H 1.3178 0.2579 0.6732 0.041 Uiso 1 1 calc R U . . .
H50B H 1.1994 0.2586 0.6874 0.041 Uiso 1 1 calc R U . . .
C51 C 0.9494(4) -0.3290(2) 0.5807(3) 0.0405(9) Uani 1 1 d . . . . .
H51A H 0.9877 -0.3622 0.5450 0.049 Uiso 1 1 calc R U . . .
H51B H 0.9115 -0.3728 0.6099 0.049 Uiso 1 1 calc R U . . .
C52 C 0.7137(3) -0.1181(2) 0.5813(2) 0.0324(7) Uani 1 1 d . . . . .
C53 C 0.8759(3) -0.2676(2) 0.4555(2) 0.0336(7) Uani 1 1 d . . . . .
C54 C 1.3970(3) 0.0937(3) 0.5435(2) 0.0387(8) Uani 1 1 d . . . . .
H54A H 1.4530 0.1367 0.5666 0.046 Uiso 1 1 calc R U . . .
H54B H 1.4273 0.0522 0.5090 0.046 Uiso 1 1 calc R U . . .
C55 C 0.7080(3) -0.2317(2) 0.4830(2) 0.0315(7) Uani 1 1 d . . . . .
H55 H 0.6451 -0.2723 0.4681 0.038 Uiso 1 1 calc R U . . .
C9 C 0.0029(4) 0.5365(3) 0.9696(2) 0.0379(9) Uani 1 1 d . . . . .
H9A H -0.0680 0.5497 0.9485 0.046 Uiso 1 1 calc R U . . .
H9B H 0.0374 0.5913 0.9955 0.046 Uiso 1 1 calc R U . . .
C5 C 0.0677(3) 0.5137(3) 0.7106(2) 0.0381(8) Uani 1 1 d . . . . .
H5 H -0.0022 0.4936 0.7121 0.046 Uiso 1 1 calc R U . . .
O3 O 0.2124(3) 0.4750(3) 0.5088(2) 0.0733(13) Uani 1 1 d . . . . .
N3 N 0.3203(3) 0.6465(3) 1.0632(2) 0.0388(7) Uani 1 1 d . . . . .
C3 C 0.2725(3) 0.5699(3) 0.7079(2) 0.0370(8) Uani 1 1 d . . . . .
H3 H 0.3431 0.5888 0.7081 0.044 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 O1 1.756(3) . ?
U1 O1 1.756(3) 2_666 ?
U1 O4 2.273(3) . ?
U1 O4 2.273(3) 2_666 ?
U1 O2 2.306(3) 2_666 ?
U1 O2 2.306(3) . ?
N1 C5 1.331(5) . ?
N1 C4 1.351(5) . ?
N1 C7 1.495(4) . ?
C1 O3 1.209(5) . ?
C1 O2 1.285(5) . ?
C1 C2 1.523(5) . ?
N2 C13 1.339(5) . ?
N2 C14 1.342(5) . ?
N2 C16 1.483(5) . ?
C2 C3 1.379(6) . ?
C2 C6 1.382(5) . ?
O4 C10 1.285(6) . ?
N4 C21 1.373(5) . ?
N4 C31 1.436(6) . ?
N4 C20 1.442(6) . ?
C4 C3 1.378(5) . ?
C4 H4 0.9300 . ?
O5 C10 1.211(6) . ?
N5 C21 1.368(6) . ?
N5 C32 1.443(5) . ?
N5 C22 1.454(5) . ?
C6 C5 1.371(5) . ?
C6 H6 0.9300 . ?
N6 C23 1.376(5) . ?
N6 C33 1.435(5) . ?
N6 C22 1.446(5) . ?
O6 C25 1.211(5) . ?
C7 C8 1.511(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
N7 C23 1.384(5) . ?
N7 C35 1.440(5) . ?
N7 C28 1.449(5) . ?
O7 C19 1.210(5) . ?
C8 C9 1.522(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
N8 C25 1.367(5) . ?
N8 C35 1.446(4) 2_567 ?
N8 C24 1.446(5) . ?
O8 C21 1.213(5) . ?
O9 C23 1.208(5) . ?
N9 C25 1.381(5) . ?
N9 C26 1.433(5) . ?
N9 C33 1.447(4) 2_567 ?
C10 C11 1.515(5) . ?
N10 C27 1.361(5) . ?
N10 C32 1.444(5) 2_567 ?
N10 C26 1.453(5) . ?
O10 C27 1.218(5) . ?
C11 C15 1.379(6) . ?
C11 C12 1.389(5) . ?
O11 C37 1.218(5) . ?
N11 C19 1.375(5) . ?
N11 C29 1.443(5) . ?
N11 C24 1.447(6) . ?
C12 C13 1.377(5) . ?
C12 H12 0.9300 . ?
O12 C38 1.215(5) . ?
N12 C48 1.365(5) . ?
N12 C28 1.446(5) . ?
N12 C29 1.449(5) 2_567 ?
C13 H13 0.9300 . ?
O13 C48 1.206(5) . ?
N13 C44 1.378(5) . ?
N13 C43 1.446(5) . ?
N13 C45 1.447(5) . ?
C14 C15 1.374(6) . ?
C14 H14 0.9300 . ?
O14 C46 1.210(4) . ?
N14 C46 1.369(5) . ?
N14 C42 1.441(5) . ?
N14 C45 1.442(5) . ?
C15 H15 0.9300 . ?
O15 C44 1.214(5) . ?
N15 C38 1.372(5) . ?
N15 C40 1.435(5) . ?
N15 C42 1.436(5) . ?
C16 C17 1.509(5) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
O16 C52 1.216(5) . ?
N16 C38 1.388(5) . ?
N16 C41 1.444(5) . ?
N16 C39 1.449(5) . ?
C17 C18 1.514(5) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
O17 C53 1.214(5) . ?
N17 C37 1.375(5) . ?
N17 C43 1.443(5) . ?
N17 C40 1.450(5) . ?
C18 C18 1.511(7) 2_756 ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
N18 C37 1.366(6) . ?
N18 C39 1.441(5) . ?
N18 C51 1.447(5) . ?
C19 N3 1.377(6) . ?
N19 C52 1.361(5) . ?
N19 C41 1.436(5) . ?
N19 C47 1.450(5) . ?
C20 N3 1.443(5) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
N20 C48 1.369(5) 2_567 ?
N20 C36 1.434(5) . ?
N20 C30 1.438(5) . ?
N21 C27 1.371(5) . ?
N21 C31 1.442(5) 2_567 ?
N21 C36 1.448(5) 2_567 ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
N22 C52 1.375(5) 2_756 ?
N22 C54 1.434(5) . ?
N22 C55 1.447(5) 2_756 ?
N23 C44 1.377(5) . ?
N23 C49 1.442(5) . ?
N23 C54 1.448(5) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
N24 C46 1.368(4) . ?
N24 C50 1.444(5) . ?
N24 C49 1.454(5) . ?
N25 C53 1.367(5) . ?
N25 C51 1.436(5) . ?
N25 C47 1.447(5) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
N26 C53 1.374(5) . ?
N26 C55 1.445(5) . ?
N26 C50 1.447(5) 2_756 ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 N12 1.449(5) 2_567 ?
C29 C30 1.542(5) . ?
C29 H29 0.9800 . ?
C30 N3 1.457(5) . ?
C30 H30 0.9800 . ?
C31 N21 1.442(5) 2_567 ?
C31 C32 1.560(6) . ?
C31 H31 0.9800 . ?
C32 N10 1.444(5) 2_567 ?
C32 H32 0.9800 . ?
C33 N9 1.447(4) 2_567 ?
C33 C35 1.564(5) . ?
C33 H33 0.9800 . ?
C35 N8 1.446(4) 2_567 ?
C35 H35 0.9800 . ?
C36 N21 1.448(5) 2_567 ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C39 C40 1.552(5) . ?
C39 H39 0.9800 . ?
C40 H40 0.9800 . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C45 C49 1.550(5) . ?
C45 H45 0.9800 . ?
C48 N20 1.369(5) 2_567 ?
C47 C55 1.551(5) . ?
C47 H47 0.9800 . ?
C49 H49 0.9800 . ?
C50 N26 1.447(5) 2_756 ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 N22 1.375(5) 2_756 ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C55 N22 1.447(5) 2_756 ?
C55 H55 0.9800 . ?
C9 C9 1.522(7) 2_567 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C5 H5 0.9300 . ?
C3 H3 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O1 180.0 . 2_666 ?
O1 U1 O4 90.12(17) . . ?
O1 U1 O4 89.88(17) 2_666 . ?
O1 U1 O4 89.88(17) . 2_666 ?
O1 U1 O4 90.12(17) 2_666 2_666 ?
O4 U1 O4 180.0 . 2_666 ?
O1 U1 O2 92.77(13) . 2_666 ?
O1 U1 O2 87.23(13) 2_666 2_666 ?
O4 U1 O2 92.04(12) . 2_666 ?
O4 U1 O2 87.96(12) 2_666 2_666 ?
O1 U1 O2 87.23(13) . . ?
O1 U1 O2 92.77(13) 2_666 . ?
O4 U1 O2 87.96(12) . . ?
O4 U1 O2 92.04(12) 2_666 . ?
O2 U1 O2 180.0 2_666 . ?
C5 N1 C4 120.6(3) . . ?
C5 N1 C7 118.9(3) . . ?
C4 N1 C7 120.5(4) . . ?
O3 C1 O2 127.0(4) . . ?
O3 C1 C2 119.1(4) . . ?
O2 C1 C2 113.8(3) . . ?
C1 O2 U1 133.5(3) . . ?
C13 N2 C14 121.5(3) . . ?
C13 N2 C16 118.6(3) . . ?
C14 N2 C16 119.9(3) . . ?
C3 C2 C6 118.4(3) . . ?
C3 C2 C1 123.1(3) . . ?
C6 C2 C1 118.5(3) . . ?
C10 O4 U1 141.7(3) . . ?
C21 N4 C31 112.8(3) . . ?
C21 N4 C20 122.5(4) . . ?
C31 N4 C20 124.5(4) . . ?
N1 C4 C3 119.7(4) . . ?
N1 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C21 N5 C32 112.6(3) . . ?
C21 N5 C22 122.5(3) . . ?
C32 N5 C22 124.3(3) . . ?
C5 C6 C2 119.5(4) . . ?
C5 C6 H6 120.3 . . ?
C2 C6 H6 120.3 . . ?
C23 N6 C33 112.4(3) . . ?
C23 N6 C22 122.0(3) . . ?
C33 N6 C22 125.1(3) . . ?
N1 C7 C8 113.6(3) . . ?
N1 C7 H7A 108.8 . . ?
C8 C7 H7A 108.8 . . ?
N1 C7 H7B 108.8 . . ?
C8 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C23 N7 C35 111.5(3) . . ?
C23 N7 C28 119.5(3) . . ?
C35 N7 C28 120.2(3) . . ?
C7 C8 C9 110.5(3) . . ?
C7 C8 H8A 109.6 . . ?
C9 C8 H8A 109.6 . . ?
C7 C8 H8B 109.6 . . ?
C9 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
C25 N8 C35 112.9(3) . 2_567 ?
C25 N8 C24 122.7(3) . . ?
C35 N8 C24 124.4(3) 2_567 . ?
C25 N9 C26 122.6(3) . . ?
C25 N9 C33 112.6(3) . 2_567 ?
C26 N9 C33 123.7(3) . 2_567 ?
O5 C10 O4 125.8(4) . . ?
O5 C10 C11 119.1(4) . . ?
O4 C10 C11 114.8(4) . . ?
C27 N10 C32 113.4(3) . 2_567 ?
C27 N10 C26 122.4(3) . . ?
C32 N10 C26 123.5(3) 2_567 . ?
C15 C11 C12 118.7(4) . . ?
C15 C11 C10 120.0(4) . . ?
C12 C11 C10 121.2(4) . . ?
C19 N11 C29 112.0(3) . . ?
C19 N11 C24 121.7(3) . . ?
C29 N11 C24 123.0(3) . . ?
C13 C12 C11 119.3(4) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C48 N12 C28 122.8(3) . . ?
C48 N12 C29 112.4(3) . 2_567 ?
C28 N12 C29 124.4(3) . 2_567 ?
N2 C13 C12 120.5(4) . . ?
N2 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C44 N13 C43 121.8(3) . . ?
C44 N13 C45 112.5(3) . . ?
C43 N13 C45 123.6(3) . . ?
N2 C14 C15 119.8(4) . . ?
N2 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C46 N14 C42 121.4(3) . . ?
C46 N14 C45 112.9(3) . . ?
C42 N14 C45 125.6(3) . . ?
C14 C15 C11 120.2(4) . . ?
C14 C15 H15 119.9 . . ?
C11 C15 H15 119.9 . . ?
C38 N15 C40 112.8(3) . . ?
C38 N15 C42 123.0(3) . . ?
C40 N15 C42 122.9(3) . . ?
N2 C16 C17 112.4(3) . . ?
N2 C16 H16A 109.1 . . ?
C17 C16 H16A 109.1 . . ?
N2 C16 H16B 109.1 . . ?
C17 C16 H16B 109.1 . . ?
H16A C16 H16B 107.9 . . ?
C38 N16 C41 121.0(3) . . ?
C38 N16 C39 110.8(3) . . ?
C41 N16 C39 122.7(3) . . ?
C16 C17 C18 110.2(3) . . ?
C16 C17 H17A 109.6 . . ?
C18 C17 H17A 109.6 . . ?
C16 C17 H17B 109.6 . . ?
C18 C17 H17B 109.6 . . ?
H17A C17 H17B 108.1 . . ?
C37 N17 C43 122.3(3) . . ?
C37 N17 C40 112.0(3) . . ?
C43 N17 C40 124.9(3) . . ?
C18 C18 C17 112.2(4) 2_756 . ?
C18 C18 H18A 109.2 2_756 . ?
C17 C18 H18A 109.2 . . ?
C18 C18 H18B 109.2 2_756 . ?
C17 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
C37 N18 C39 113.1(3) . . ?
C37 N18 C51 122.1(3) . . ?
C39 N18 C51 124.8(4) . . ?
O7 C19 N11 126.4(4) . . ?
O7 C19 N3 125.7(4) . . ?
N11 C19 N3 107.9(3) . . ?
C52 N19 C41 123.2(3) . . ?
C52 N19 C47 112.8(3) . . ?
C41 N19 C47 123.5(3) . . ?
N4 C20 N3 113.5(3) . . ?
N4 C20 H20A 108.9 . . ?
N3 C20 H20A 108.9 . . ?
N4 C20 H20B 108.9 . . ?
N3 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
C48 N20 C36 122.3(3) 2_567 . ?
C48 N20 C30 112.7(3) 2_567 . ?
C36 N20 C30 125.0(3) . . ?
O8 C21 N5 126.4(4) . . ?
O8 C21 N4 125.6(4) . . ?
N5 C21 N4 107.9(3) . . ?
C27 N21 C31 112.7(3) . 2_567 ?
C27 N21 C36 122.4(3) . 2_567 ?
C31 N21 C36 123.6(3) 2_567 2_567 ?
N6 C22 N5 113.7(3) . . ?
N6 C22 H22A 108.8 . . ?
N5 C22 H22A 108.8 . . ?
N6 C22 H22B 108.8 . . ?
N5 C22 H22B 108.8 . . ?
H22A C22 H22B 107.7 . . ?
C52 N22 C54 122.2(3) 2_756 . ?
C52 N22 C55 111.9(3) 2_756 2_756 ?
C54 N22 C55 123.6(3) . 2_756 ?
O9 C23 N6 125.7(3) . . ?
O9 C23 N7 126.6(3) . . ?
N6 C23 N7 107.8(3) . . ?
C44 N23 C49 113.0(3) . . ?
C44 N23 C54 122.1(3) . . ?
C49 N23 C54 124.7(3) . . ?
N8 C24 N11 114.5(3) . . ?
N8 C24 H24A 108.6 . . ?
N11 C24 H24A 108.6 . . ?
N8 C24 H24B 108.6 . . ?
N11 C24 H24B 108.6 . . ?
H24A C24 H24B 107.6 . . ?
C46 N24 C50 120.8(3) . . ?
C46 N24 C49 111.9(3) . . ?
C50 N24 C49 124.1(3) . . ?
O6 C25 N8 126.2(4) . . ?
O6 C25 N9 125.8(4) . . ?
N8 C25 N9 107.9(3) . . ?
C53 N25 C51 121.8(3) . . ?
C53 N25 C47 112.2(3) . . ?
C51 N25 C47 121.9(3) . . ?
N9 C26 N10 114.2(3) . . ?
N9 C26 H26A 108.7 . . ?
N10 C26 H26A 108.7 . . ?
N9 C26 H26B 108.7 . . ?
N10 C26 H26B 108.7 . . ?
H26A C26 H26B 107.6 . . ?
C53 N26 C55 112.8(3) . . ?
C53 N26 C50 122.5(3) . 2_756 ?
C55 N26 C50 123.3(3) . 2_756 ?
O10 C27 N10 126.5(4) . . ?
O10 C27 N21 125.6(4) . . ?
N10 C27 N21 107.9(3) . . ?
N12 C28 N7 113.5(3) . . ?
N12 C28 H28A 108.9 . . ?
N7 C28 H28A 108.9 . . ?
N12 C28 H28B 108.9 . . ?
N7 C28 H28B 108.9 . . ?
H28A C28 H28B 107.7 . . ?
N11 C29 N12 115.2(3) . 2_567 ?
N11 C29 C30 104.1(3) . . ?
N12 C29 C30 103.3(3) 2_567 . ?
N11 C29 H29 111.2 . . ?
N12 C29 H29 111.2 2_567 . ?
C30 C29 H29 111.2 . . ?
N20 C30 N3 114.6(3) . . ?
N20 C30 C29 103.6(3) . . ?
N3 C30 C29 103.1(3) . . ?
N20 C30 H30 111.7 . . ?
N3 C30 H30 111.7 . . ?
C29 C30 H30 111.7 . . ?
N4 C31 N21 115.6(3) . 2_567 ?
N4 C31 C32 103.2(3) . . ?
N21 C31 C32 103.3(3) 2_567 . ?
N4 C31 H31 111.4 . . ?
N21 C31 H31 111.4 2_567 . ?
C32 C31 H31 111.4 . . ?
N5 C32 N10 115.5(3) . 2_567 ?
N5 C32 C31 103.2(3) . . ?
N10 C32 C31 102.7(3) 2_567 . ?
N5 C32 H32 111.6 . . ?
N10 C32 H32 111.6 2_567 . ?
C31 C32 H32 111.6 . . ?
N6 C33 N9 115.7(3) . 2_567 ?
N6 C33 C35 103.3(3) . . ?
N9 C33 C35 102.9(3) 2_567 . ?
N6 C33 H33 111.4 . . ?
N9 C33 H33 111.4 2_567 . ?
C35 C33 H33 111.4 . . ?
N7 C35 N8 115.0(3) . 2_567 ?
N7 C35 C33 103.1(3) . . ?
N8 C35 C33 103.1(3) 2_567 . ?
N7 C35 H35 111.7 . . ?
N8 C35 H35 111.7 2_567 . ?
C33 C35 H35 111.7 . . ?
N20 C36 N21 114.4(3) . 2_567 ?
N20 C36 H36A 108.7 . . ?
N21 C36 H36A 108.7 2_567 . ?
N20 C36 H36B 108.7 . . ?
N21 C36 H36B 108.7 2_567 . ?
H36A C36 H36B 107.6 . . ?
O11 C37 N18 126.2(4) . . ?
O11 C37 N17 125.8(4) . . ?
N18 C37 N17 108.0(3) . . ?
O12 C38 N15 126.5(4) . . ?
O12 C38 N16 125.9(4) . . ?
N15 C38 N16 107.6(3) . . ?
N18 C39 N16 116.3(3) . . ?
N18 C39 C40 103.1(3) . . ?
N16 C39 C40 103.7(3) . . ?
N18 C39 H39 111.0 . . ?
N16 C39 H39 111.0 . . ?
C40 C39 H39 111.0 . . ?
N15 C40 N17 116.1(3) . . ?
N15 C40 C39 103.2(3) . . ?
N17 C40 C39 103.4(3) . . ?
N15 C40 H40 111.2 . . ?
N17 C40 H40 111.2 . . ?
C39 C40 H40 111.2 . . ?
N19 C41 N16 114.1(3) . . ?
N19 C41 H41A 108.7 . . ?
N16 C41 H41A 108.7 . . ?
N19 C41 H41B 108.7 . . ?
N16 C41 H41B 108.7 . . ?
H41A C41 H41B 107.6 . . ?
N15 C42 N14 113.8(3) . . ?
N15 C42 H42A 108.8 . . ?
N14 C42 H42A 108.8 . . ?
N15 C42 H42B 108.8 . . ?
N14 C42 H42B 108.8 . . ?
H42A C42 H42B 107.7 . . ?
N17 C43 N13 113.5(3) . . ?
N17 C43 H43A 108.9 . . ?
N13 C43 H43A 108.9 . . ?
N17 C43 H43B 108.9 . . ?
N13 C43 H43B 108.9 . . ?
H43A C43 H43B 107.7 . . ?
O15 C44 N23 126.4(4) . . ?
O15 C44 N13 126.5(4) . . ?
N23 C44 N13 107.2(3) . . ?
N14 C45 N13 115.8(3) . . ?
N14 C45 C49 102.9(3) . . ?
N13 C45 C49 103.1(3) . . ?
N14 C45 H45 111.4 . . ?
N13 C45 H45 111.4 . . ?
C49 C45 H45 111.4 . . ?
O14 C46 N24 126.4(3) . . ?
O14 C46 N14 125.4(3) . . ?
N24 C46 N14 108.2(3) . . ?
O13 C48 N12 126.0(4) . . ?
O13 C48 N20 125.9(4) . 2_567 ?
N12 C48 N20 108.1(3) . 2_567 ?
N25 C47 N19 114.4(3) . . ?
N25 C47 C55 103.8(3) . . ?
N19 C47 C55 102.9(3) . . ?
N25 C47 H47 111.7 . . ?
N19 C47 H47 111.7 . . ?
C55 C47 H47 111.7 . . ?
N23 C49 N24 115.4(3) . . ?
N23 C49 C45 103.3(3) . . ?
N24 C49 C45 103.4(3) . . ?
N23 C49 H49 111.4 . . ?
N24 C49 H49 111.4 . . ?
C45 C49 H49 111.4 . . ?
N24 C50 N26 113.2(3) . 2_756 ?
N24 C50 H50A 108.9 . . ?
N26 C50 H50A 108.9 2_756 . ?
N24 C50 H50B 108.9 . . ?
N26 C50 H50B 108.9 2_756 . ?
H50A C50 H50B 107.8 . . ?
N25 C51 N18 113.7(3) . . ?
N25 C51 H51A 108.8 . . ?
N18 C51 H51A 108.8 . . ?
N25 C51 H51B 108.8 . . ?
N18 C51 H51B 108.8 . . ?
H51A C51 H51B 107.7 . . ?
O16 C52 N19 125.9(4) . . ?
O16 C52 N22 125.8(4) . 2_756 ?
N19 C52 N22 108.4(3) . 2_756 ?
O17 C53 N25 126.0(4) . . ?
O17 C53 N26 126.0(4) . . ?
N25 C53 N26 108.0(3) . . ?
N22 C54 N23 114.2(3) . . ?
N22 C54 H54A 108.7 . . ?
N23 C54 H54A 108.7 . . ?
N22 C54 H54B 108.7 . . ?
N23 C54 H54B 108.7 . . ?
H54A C54 H54B 107.6 . . ?
N26 C55 N22 115.1(3) . 2_756 ?
N26 C55 C47 102.8(3) . . ?
N22 C55 C47 103.7(3) 2_756 . ?
N26 C55 H55 111.5 . . ?
N22 C55 H55 111.5 2_756 . ?
C47 C55 H55 111.5 . . ?
C8 C9 C9 112.3(4) . 2_567 ?
C8 C9 H9A 109.1 . . ?
C9 C9 H9A 109.1 2_567 . ?
C8 C9 H9B 109.1 . . ?
C9 C9 H9B 109.1 2_567 . ?
H9A C9 H9B 107.9 . . ?
N1 C5 C6 121.4(4) . . ?
N1 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C19 N3 C20 122.3(3) . . ?
C19 N3 C30 111.7(3) . . ?
C20 N3 C30 121.8(4) . . ?
C4 C3 C2 120.4(4) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?

_refine_diff_density_max         3.265
_refine_diff_density_min         -1.877
_refine_diff_density_rms         0.111

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_4-aUP-296K
_database_code_depnum_ccdc_archive 'CCDC 1534039'
_audit_update_record             
;
2017-02-22 deposited with the CCDC.
2017-05-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C108 H112 Br2 N52 O34 U'
_chemical_formula_weight         3080.34

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'
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'
Br Br -0.2901 2.4595 '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                   12.7767(13)
_cell_length_b                   15.3536(16)
_cell_length_c                   17.0453(16)
_cell_angle_alpha                90.559(5)
_cell_angle_beta                 97.590(5)
_cell_angle_gamma                94.644(5)
_cell_volume                     3302.9(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9917
_cell_measurement_theta_min      2.90
_cell_measurement_theta_max      25.67

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_F_000             1558
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    1.930
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            74714
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.900
_diffrn_reflns_theta_max         27.538
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             15081
_reflns_number_gt                13077
_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       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0873P)²+3.4347P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15081
_refine_ls_number_parameters     926
_refine_ls_number_restraints     903
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0507
_refine_ls_wR_factor_ref         0.1438
_refine_ls_wR_factor_gt          0.1367
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.048
_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 1.0000 0.0000 0.5000 0.03547(8) Uani 1 2 d S U P . .
Br1 Br 0.0862(7) 0.0920(7) 1.2244(5) 0.399(5) Uani 0.5 1 d . . P . .
O1 O 0.9154(4) -0.0845(4) 0.4547(4) 0.1078(19) Uani 1 1 d . U . . .
O2 O 0.9279(4) 0.0938(4) 0.4118(3) 0.1050(19) Uani 1 1 d . U . . .
Br2 Br 0.0221(6) 0.7363(5) 0.4241(5) 0.335(4) Uani 0.5 1 d . . P . .
O3 O 1.0059(3) 0.1875(3) 0.3371(3) 0.0690(11) Uani 1 1 d . U . . .
C15A C 0.8439(13) 0.0399(10) 0.6143(8) 0.067(3) Uani 0.518(11) 1 d . U P A 1
O4 O 0.9102(13) -0.0061(12) 0.6280(9) 0.177(7) Uani 0.518(11) 1 d . U P A 1
O5 O 0.8444(10) 0.0765(8) 0.5544(6) 0.113(5) Uani 0.518(11) 1 d . U P A 1
C15B C 0.7967(13) 0.0072(11) 0.5814(10) 0.072(4) Uani 0.482(11) 1 d . U P A 2
O6 O 0.8882(6) 0.0337(5) 0.5835(4) 0.044(2) Uani 0.482(11) 1 d . U P A 2
O7 O 0.7403(10) -0.0345(12) 0.5254(8) 0.148(8) Uani 0.482(11) 1 d . U P A 2
O8 O 0.6537(3) 0.2255(2) 0.57211(19) 0.0523(8) Uani 1 1 d . U . . .
O9 O 0.4341(3) 0.2103(2) 0.4233(2) 0.0528(8) Uani 1 1 d . U . . .
O11 O 0.4227(3) 0.4755(2) 0.7662(2) 0.0485(7) Uani 1 1 d . U . . .
O10 O 0.6066(2) 0.63935(19) 0.74992(17) 0.0392(6) Uani 1 1 d . U . . .
O12 O 0.1947(3) 0.4529(2) 0.61420(17) 0.0433(7) Uani 1 1 d . U . . .
O13 O 0.1557(3) 0.5981(2) 0.44915(18) 0.0460(7) Uani 1 1 d . U . . .
O14 O 0.7614(3) 0.2020(2) 0.95807(18) 0.0464(7) Uani 1 1 d . U . . .
O15 O 0.5048(2) 0.2777(2) 0.89477(16) 0.0426(7) Uani 1 1 d . U . . .
O16 O 0.3178(2) 0.13371(19) 0.78851(17) 0.0403(6) Uani 1 1 d . U . . .
O17 O 0.1548(3) 0.0018(2) 1.09021(18) 0.0451(7) Uani 1 1 d . U . . .
O18 O 0.3465(3) 0.13753(19) 1.20096(16) 0.0416(7) Uani 1 1 d . U . . .
O19 O 0.6243(2) 0.0647(2) 1.26842(18) 0.0458(7) Uani 1 1 d . U . . .
C21 C 0.8456(3) 0.2213(3) 0.3780(2) 0.0356(8) Uani 1 1 d . U . . .
C20 C 0.9369(4) 0.1656(3) 0.3761(3) 0.0479(10) Uani 1 1 d . U . . .
C22 C 0.7572(4) 0.1923(3) 0.4113(2) 0.0423(9) Uani 1 1 d . U . . .
H22 H 0.7530 0.1376 0.4342 0.051 Uiso 1 1 calc R U . . .
C23 C 0.6756(4) 0.2448(3) 0.4104(2) 0.0430(9) Uani 1 1 d . U . . .
H23 H 0.6146 0.2251 0.4314 0.052 Uiso 1 1 calc R U . . .
C24 C 0.8505(3) 0.3033(3) 0.3442(3) 0.0398(9) Uani 1 1 d . U . . .
H24 H 0.9091 0.3229 0.3202 0.048 Uiso 1 1 calc R U . . .
C25 C 0.7683(4) 0.3550(3) 0.3464(3) 0.0418(9) Uani 1 1 d . U . . .
H25 H 0.7718 0.4106 0.3252 0.050 Uiso 1 1 calc R U . . .
C26 C 0.5936(4) 0.3806(3) 0.3802(3) 0.0472(11) Uani 1 1 d . U . . .
H26A H 0.5273 0.3452 0.3659 0.057 Uiso 1 1 calc R U . . .
H26B H 0.5984 0.4258 0.3412 0.057 Uiso 1 1 calc R U . . .
C27 C 0.5941(3) 0.4229(3) 0.4610(2) 0.0385(9) Uani 1 1 d . U . . .
H27A H 0.5891 0.3779 0.5002 0.046 Uiso 1 1 calc R U . . .
H27B H 0.6601 0.4586 0.4754 0.046 Uiso 1 1 calc R U . . .
C28 C 0.5020(4) 0.4792(3) 0.4605(3) 0.0442(10) Uani 1 1 d . U . . .
H28A H 0.5080 0.5245 0.4217 0.053 Uiso 1 1 calc R U . . .
H28B H 0.4364 0.4434 0.4447 0.053 Uiso 1 1 calc R U . . .
C29 C 0.7533(5) 0.0402(4) 0.6616(4) 0.0696(15) Uani 1 1 d . U . . .
C30 C 0.7957(5) 0.0890(5) 0.7273(4) 0.0737(15) Uani 1 1 d . U . . .
H30 H 0.8655 0.1129 0.7317 0.088 Uiso 1 1 calc R U . . .
C31 C 0.7341(4) 0.1033(4) 0.7886(3) 0.0536(11) Uani 1 1 d . U . . .
H31 H 0.7626 0.1360 0.8337 0.064 Uiso 1 1 calc R U . . .
C32 C 0.6505(6) 0.0062(4) 0.6551(3) 0.0718(16) Uani 1 1 d . U . . .
H32 H 0.6203 -0.0267 0.6105 0.086 Uiso 1 1 calc R U . . .
C33 C 0.5925(4) 0.0210(3) 0.7146(3) 0.0503(11) Uani 1 1 d . U . . .
H33 H 0.5225 -0.0024 0.7101 0.060 Uiso 1 1 calc R U . . .
C34 C 0.5652(4) 0.0832(3) 0.8419(2) 0.0391(9) Uani 1 1 d . U . . .
H34A H 0.4926 0.0846 0.8169 0.047 Uiso 1 1 calc R U . . .
H34B H 0.5870 0.1399 0.8671 0.047 Uiso 1 1 calc R U . . .
C35 C 0.5688(3) 0.0143(3) 0.9050(2) 0.0346(8) Uani 1 1 d . U . . .
H35A H 0.6414 0.0116 0.9294 0.041 Uiso 1 1 calc R U . . .
H35B H 0.5444 -0.0423 0.8806 0.041 Uiso 1 1 calc R U . . .
C36 C 0.5001(4) 0.0341(3) 0.9682(2) 0.0375(9) Uani 1 1 d . U . . .
H36A H 0.5254 0.0905 0.9928 0.045 Uiso 1 1 calc R U . . .
H36B H 0.4280 0.0382 0.9432 0.045 Uiso 1 1 calc R U . . .
C37 C 0.2255(3) 0.6650(3) 0.3061(3) 0.0410(9) Uani 1 1 d . U . . .
H37A H 0.1915 0.6726 0.2525 0.049 Uiso 1 1 calc R U . . .
H37B H 0.1919 0.7006 0.3412 0.049 Uiso 1 1 calc R U . . .
C38 C 0.1694(3) 0.5496(3) 0.3952(2) 0.0354(8) Uani 1 1 d . U . . .
C39 C 0.1963(3) 0.5026(3) 0.2690(2) 0.0356(8) Uani 1 1 d . U . . .
H39 H 0.1424 0.5125 0.2242 0.043 Uiso 1 1 calc R U . . .
C40 C 0.1620(3) 0.4214(3) 0.3172(2) 0.0345(8) Uani 1 1 d . U . . .
H40 H 0.0959 0.3906 0.2916 0.041 Uiso 1 1 calc R U . . .
C41 C 0.1043(3) 0.4130(3) 0.4546(2) 0.0385(9) Uani 1 1 d . U . . .
H41A H 0.0459 0.3728 0.4310 0.046 Uiso 1 1 calc R U . . .
H41B H 0.0760 0.4539 0.4884 0.046 Uiso 1 1 calc R U . . .
C42 C 0.2458(3) 0.2773(3) 0.3432(2) 0.0380(9) Uani 1 1 d . U . . .
H42A H 0.1744 0.2507 0.3278 0.046 Uiso 1 1 calc R U . . .
H42B H 0.2932 0.2460 0.3155 0.046 Uiso 1 1 calc R U . . .
C43 C 0.1998(3) 0.2757(3) 0.4840(2) 0.0352(8) Uani 1 1 d . U . . .
H43 H 0.1337 0.2391 0.4684 0.042 Uiso 1 1 calc R U . . .
C44 C 0.2606(3) 0.2447(3) 0.5618(2) 0.0372(8) Uani 1 1 d . U . . .
H44 H 0.2221 0.1943 0.5830 0.045 Uiso 1 1 calc R U . . .
C45 C 0.3640(3) 0.2316(3) 0.4591(3) 0.0391(8) Uani 1 1 d . U . . .
C46 C 0.2126(3) 0.3860(3) 0.5806(2) 0.0319(7) Uani 1 1 d . U . . .
C47 C 0.4351(4) 0.1762(3) 0.5896(3) 0.0463(10) Uani 1 1 d . U . . .
H47A H 0.4734 0.1418 0.5568 0.056 Uiso 1 1 calc R U . . .
H47B H 0.3969 0.1362 0.6215 0.056 Uiso 1 1 calc R U . . .
C48 C 0.3063(3) 0.3194(3) 0.6971(2) 0.0376(9) Uani 1 1 d . U . . .
H48A H 0.2733 0.3632 0.7245 0.045 Uiso 1 1 calc R U . . .
H48B H 0.2854 0.2628 0.7174 0.045 Uiso 1 1 calc R U . . .
C49 C 0.4914(3) 0.2671(3) 0.7169(2) 0.0353(8) Uani 1 1 d . U . . .
H49 H 0.4705 0.2200 0.7514 0.042 Uiso 1 1 calc R U . . .
C50 C 0.5999(3) 0.3152(3) 0.7511(2) 0.0341(8) Uani 1 1 d . U . . .
H50 H 0.6299 0.2887 0.8002 0.041 Uiso 1 1 calc R U . . .
C51 C 0.4674(3) 0.4118(3) 0.7498(2) 0.0354(8) Uani 1 1 d . U . . .
C52 C 0.6134(4) 0.2520(3) 0.6275(2) 0.0395(9) Uani 1 1 d . U . . .
C53 C 0.6466(3) 0.4690(3) 0.8079(2) 0.0384(9) Uani 1 1 d . U . . .
H53A H 0.6950 0.4408 0.8463 0.046 Uiso 1 1 calc R U . . .
H53B H 0.6072 0.5068 0.8368 0.046 Uiso 1 1 calc R U . . .
C54 C 0.6796(3) 0.6014(3) 0.7313(2) 0.0311(7) Uani 1 1 d . U . . .
C55 C 0.1086(3) 0.0527(3) 0.8884(2) 0.0346(8) Uani 1 1 d . U . . .
H55 H 0.0360 0.0494 0.8609 0.042 Uiso 1 1 calc R U . . .
C56 C 0.1416(3) 0.1435(3) 0.9294(2) 0.0339(8) Uani 1 1 d . U . . .
H56 H 0.0841 0.1823 0.9211 0.041 Uiso 1 1 calc R U . . .
C57 C 0.2517(3) 0.1198(3) 0.8335(2) 0.0324(8) Uani 1 1 d . U . . .
C58 C 0.1485(3) 0.0356(3) 1.0258(2) 0.0351(8) Uani 1 1 d . U . . .
C59 C 0.2824(3) 0.2627(3) 0.9037(2) 0.0359(8) Uani 1 1 d . U . . .
H59A H 0.3111 0.2808 0.8559 0.043 Uiso 1 1 calc R U . . .
H59B H 0.2300 0.3024 0.9133 0.043 Uiso 1 1 calc R U . . .
C60 C 0.1919(3) 0.1887(3) 1.0753(2) 0.0393(9) Uani 1 1 d . U . . .
H60A H 0.1511 0.2383 1.0618 0.047 Uiso 1 1 calc R U . . .
H60B H 0.1698 0.1644 1.1234 0.047 Uiso 1 1 calc R U . . .
C61 C 0.4707(3) 0.2808(2) 0.9577(2) 0.0323(7) Uani 1 1 d . U . . .
C62 C 0.3698(3) 0.1900(2) 1.1521(2) 0.0329(8) Uani 1 1 d . U . . .
C63 C 0.3509(3) 0.2900(2) 1.0494(2) 0.0319(8) Uani 1 1 d . U . . .
H63 H 0.3145 0.3434 1.0524 0.038 Uiso 1 1 calc R U . . .
C64 C 0.4656(3) 0.3018(2) 1.0931(2) 0.0322(8) Uani 1 1 d . U . . .
H64 H 0.4795 0.3580 1.1218 0.039 Uiso 1 1 calc R U . . .
C65 C 0.5524(3) 0.2294(3) 1.2134(2) 0.0388(9) Uani 1 1 d . U . . .
H65A H 0.5246 0.1989 1.2568 0.047 Uiso 1 1 calc R U . . .
H65B H 0.5729 0.2894 1.2309 0.047 Uiso 1 1 calc R U . . .
C66 C 0.6432(3) 0.3158(3) 1.0400(2) 0.0376(8) Uani 1 1 d . U . . .
H66A H 0.6617 0.3665 1.0748 0.045 Uiso 1 1 calc R U . . .
H66B H 0.6652 0.3304 0.9890 0.045 Uiso 1 1 calc R U . . .
C67 C 0.7279(3) 0.2333(3) 1.1564(2) 0.0336(8) Uani 1 1 d . U . . .
H67 H 0.7551 0.2890 1.1831 0.040 Uiso 1 1 calc R U . . .
C68 C 0.8143(3) 0.1676(3) 1.1617(2) 0.0358(8) Uani 1 1 d . U . . .
H68 H 0.8825 0.1941 1.1878 0.043 Uiso 1 1 calc R U . . .
C69 C 0.6748(3) 0.1116(3) 1.2273(2) 0.0350(8) Uani 1 1 d . U . . .
C70 C 0.7603(3) 0.1976(3) 1.0290(2) 0.0351(8) Uani 1 1 d . U . . .
C71 C 0.9043(3) 0.1000(3) 1.0538(3) 0.0395(9) Uani 1 1 d . U . . .
H71A H 0.9193 0.1225 1.0032 0.047 Uiso 1 1 calc R U . . .
H71B H 0.9676 0.1125 1.0916 0.047 Uiso 1 1 calc R U . . .
C72 C 0.8259(3) 0.0197(3) 1.2290(2) 0.0368(8) Uani 1 1 d . U . . .
H72A H 0.9006 0.0364 1.2445 0.044 Uiso 1 1 calc R U . . .
H72B H 0.7979 -0.0059 1.2745 0.044 Uiso 1 1 calc R U . . .
N73 N 0.6337(3) 0.0685(2) 0.77957(18) 0.0326(7) Uani 1 1 d . U . . .
N74 N 0.6829(3) 0.3252(2) 0.37916(19) 0.0364(7) Uani 1 1 d . U . . .
N75 N 0.2085(3) 0.5742(2) 0.3268(2) 0.0381(7) Uani 1 1 d . U . . .
N76 N 0.1484(3) 0.4606(2) 0.39263(19) 0.0372(7) Uani 1 1 d . U . . .
N77 N 0.2741(3) 0.2679(2) 0.4274(2) 0.0378(7) Uani 1 1 d . U . . .
N78 N 0.1797(3) 0.3644(2) 0.50279(19) 0.0345(7) Uani 1 1 d . U . . .
N79 N 0.2678(3) 0.3208(2) 0.61376(19) 0.0347(7) Uani 1 1 d . U . . .
N80 N 0.3603(3) 0.2223(2) 0.5394(2) 0.0419(8) Uani 1 1 d . U . . .
N81 N 0.4195(3) 0.3357(2) 0.7138(2) 0.0364(7) Uani 1 1 d . U . . .
N82 N 0.5110(3) 0.2333(2) 0.6419(2) 0.0421(8) Uani 1 1 d . U . . .
N83 N 0.5736(3) 0.4031(2) 0.7652(2) 0.0367(7) Uani 1 1 d . U . . .
N84 N 0.6640(3) 0.3044(2) 0.6889(2) 0.0391(7) Uani 1 1 d . U . . .
N85 N 0.7074(3) 0.5219(2) 0.7575(2) 0.0373(7) Uani 1 1 d . U . . .
N86 N 0.7494(3) 0.6325(2) 0.6813(2) 0.0349(7) Uani 1 1 d . U . . .
N87 N 0.1187(3) -0.0064(2) 0.9539(2) 0.0375(7) Uani 1 1 d . U . . .
N88 N 0.1852(3) 0.0455(2) 0.8337(2) 0.0353(7) Uani 1 1 d . U . . .
N89 N 0.1664(3) 0.1231(2) 1.0121(2) 0.0376(7) Uani 1 1 d . U . . .
N90 N 0.2311(3) 0.1755(2) 0.89105(19) 0.0347(7) Uani 1 1 d . U . . .
N91 N 0.3020(3) 0.2192(2) 1.09104(19) 0.0354(7) Uani 1 1 d . U . . .
N92 N 0.3666(3) 0.2697(2) 0.96908(18) 0.0342(7) Uani 1 1 d . U . . .
N93 N 0.4698(3) 0.2289(2) 1.14708(17) 0.0312(6) Uani 1 1 d . U . . .
N94 N 0.5302(3) 0.2967(2) 1.02996(19) 0.0351(7) Uani 1 1 d . U . . .
N95 N 0.6457(3) 0.1892(2) 1.1960(2) 0.0378(7) Uani 1 1 d . U . . .
N97 N 0.7010(3) 0.2440(2) 1.07238(19) 0.0353(7) Uani 1 1 d . U . . .
N98 N 0.7725(3) 0.0975(2) 1.2077(2) 0.0367(7) Uani 1 1 d . U . . .
N99 N 0.8193(3) 0.1454(2) 1.0793(2) 0.0376(7) Uani 1 1 d . 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 O1 1.727(4) 2_756 ?
U1 O1 1.727(4) . ?
U1 O6 2.231(7) . ?
U1 O6 2.231(7) 2_756 ?
U1 O2 2.253(4) 2_756 ?
U1 O2 2.253(4) . ?
U1 O4 2.595(10) . ?
U1 O4 2.595(10) 2_756 ?
U1 O5 2.653(9) 2_756 ?
U1 O5 2.653(9) . ?
U1 C15A 3.057(11) . ?
U1 C15A 3.057(11) 2_756 ?
O2 C20 1.268(7) . ?
O3 C20 1.201(6) . ?
C15A O4 1.149(15) . ?
C15A O5 1.170(14) . ?
C15A C29 1.496(12) . ?
C15B O6 1.203(17) . ?
C15B O7 1.25(2) . ?
C15B C29 1.633(14) . ?
O8 C52 1.214(5) . ?
O9 C45 1.212(5) . ?
O11 C51 1.219(5) . ?
O10 C54 1.213(5) . ?
O12 C46 1.223(5) . ?
O13 C38 1.217(5) . ?
O14 C70 1.214(5) . ?
O15 C61 1.213(5) . ?
O16 C57 1.221(5) . ?
O17 C58 1.215(5) . ?
O18 C62 1.213(5) . ?
O19 C69 1.217(5) . ?
C21 C22 1.374(6) . ?
C21 C24 1.390(6) . ?
C21 C20 1.505(6) . ?
C22 C23 1.368(6) . ?
C22 H22 0.9300 . ?
C23 N74 1.349(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.370(6) . ?
C24 H24 0.9300 . ?
C25 N74 1.341(6) . ?
C25 H25 0.9300 . ?
C26 N74 1.480(5) . ?
C26 C27 1.516(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.513(6) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C28 1.493(8) 2_666 ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C32 1.364(10) . ?
C29 C30 1.366(10) . ?
C30 C31 1.413(8) . ?
C30 H30 0.9300 . ?
C31 N73 1.338(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.359(7) . ?
C32 H32 0.9300 . ?
C33 N73 1.344(6) . ?
C33 H33 0.9300 . ?
C34 N73 1.490(4) . ?
C34 C35 1.514(5) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.520(5) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 C36 1.515(7) 2_657 ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 N84 1.444(5) 2_666 ?
C37 N75 1.448(5) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 N76 1.370(6) . ?
C38 N75 1.372(5) . ?
C39 N85 1.442(5) 2_666 ?
C39 N75 1.454(6) . ?
C39 C40 1.565(6) . ?
C39 H39 0.9800 . ?
C40 N76 1.452(5) . ?
C40 N86 1.453(5) 2_666 ?
C40 H40 0.9800 . ?
C41 N76 1.441(5) . ?
C41 N78 1.442(5) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 N77 1.445(5) . ?
C42 N86 1.449(5) 2_666 ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 N78 1.446(5) . ?
C43 N77 1.450(5) . ?
C43 C44 1.547(6) . ?
C43 H43 0.9800 . ?
C44 N80 1.443(6) . ?
C44 N79 1.449(5) . ?
C44 H44 0.9800 . ?
C45 N77 1.366(6) . ?
C45 N80 1.385(6) . ?
C46 N79 1.357(5) . ?
C46 N78 1.366(5) . ?
C47 N80 1.432(6) . ?
C47 N82 1.456(6) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 N81 1.437(5) . ?
C48 N79 1.441(5) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C49 N82 1.436(5) . ?
C49 N81 1.450(5) . ?
C49 C50 1.555(6) . ?
C49 H49 0.9800 . ?
C50 N84 1.438(5) . ?
C50 N83 1.443(5) . ?
C50 H50 0.9800 . ?
C51 N83 1.365(5) . ?
C51 N81 1.373(6) . ?
C52 N82 1.370(6) . ?
C52 N84 1.373(6) . ?
C53 N83 1.442(6) . ?
C53 N85 1.445(5) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 N85 1.362(5) . ?
C54 N86 1.374(5) . ?
C55 N87 1.445(5) . ?
C55 N88 1.448(5) . ?
C55 C56 1.554(6) . ?
C55 H55 0.9800 . ?
C56 N90 1.445(5) . ?
C56 N89 1.446(5) . ?
C56 H56 0.9800 . ?
C57 N90 1.362(5) . ?
C57 N88 1.365(5) . ?
C58 N89 1.373(5) . ?
C58 N87 1.373(6) . ?
C59 N92 1.440(5) . ?
C59 N90 1.443(5) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C60 N91 1.436(5) . ?
C60 N89 1.454(5) . ?
C60 H60A 0.9700 . ?
C60 H60B 0.9700 . ?
C61 N92 1.366(5) . ?
C61 N94 1.368(5) . ?
C62 N91 1.367(5) . ?
C62 N93 1.379(5) . ?
C63 N92 1.444(5) . ?
C63 N91 1.448(5) . ?
C63 C64 1.549(6) . ?
C63 H63 0.9800 . ?
C64 N94 1.446(5) . ?
C64 N93 1.456(5) . ?
C64 H64 0.9800 . ?
C65 N93 1.441(5) . ?
C65 N95 1.448(5) . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C66 N94 1.437(5) . ?
C66 N97 1.450(5) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C67 N97 1.442(5) . ?
C67 N95 1.448(5) . ?
C67 C68 1.550(6) . ?
C67 H67 0.9800 . ?
C68 N98 1.446(5) . ?
C68 N99 1.453(5) . ?
C68 H68 0.9800 . ?
C69 N98 1.367(5) . ?
C69 N95 1.369(5) . ?
C70 N97 1.361(5) . ?
C70 N99 1.373(5) . ?
C71 N87 1.443(5) 2_657 ?
C71 N99 1.447(5) . ?
C71 H71A 0.9700 . ?
C71 H71B 0.9700 . ?
C72 N88 1.442(5) 2_657 ?
C72 N98 1.449(5) . ?
C72 H72A 0.9700 . ?
C72 H72B 0.9700 . ?
N84 C37 1.444(6) 2_666 ?
N85 C39 1.442(5) 2_666 ?
N86 C42 1.449(5) 2_666 ?
N86 C40 1.453(5) 2_666 ?
N87 C71 1.443(5) 2_657 ?
N88 C72 1.442(5) 2_657 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O1 180.0(3) 2_756 . ?
O1 U1 O6 86.2(3) 2_756 . ?
O1 U1 O6 93.8(3) . . ?
O1 U1 O6 93.8(3) 2_756 2_756 ?
O1 U1 O6 86.2(3) . 2_756 ?
O6 U1 O6 180.0 . 2_756 ?
O1 U1 O2 90.0(3) 2_756 2_756 ?
O1 U1 O2 90.0(3) . 2_756 ?
O6 U1 O2 90.0(2) . 2_756 ?
O6 U1 O2 90.0(2) 2_756 2_756 ?
O1 U1 O2 90.0(3) 2_756 . ?
O1 U1 O2 90.0(3) . . ?
O6 U1 O2 90.0(2) . . ?
O6 U1 O2 90.0(2) 2_756 . ?
O2 U1 O2 180.0 2_756 . ?
O1 U1 O4 87.0(5) 2_756 . ?
O1 U1 O4 93.0(5) . . ?
O2 U1 O4 67.6(3) 2_756 . ?
O2 U1 O4 112.4(3) . . ?
O1 U1 O4 93.0(5) 2_756 2_756 ?
O1 U1 O4 87.0(5) . 2_756 ?
O2 U1 O4 112.4(3) 2_756 2_756 ?
O2 U1 O4 67.6(3) . 2_756 ?
O4 U1 O4 180.0 . 2_756 ?
O1 U1 O5 93.1(4) 2_756 2_756 ?
O1 U1 O5 86.9(4) . 2_756 ?
O2 U1 O5 68.7(2) 2_756 2_756 ?
O2 U1 O5 111.3(2) . 2_756 ?
O4 U1 O5 136.3(3) . 2_756 ?
O4 U1 O5 43.7(3) 2_756 2_756 ?
O1 U1 O5 86.9(4) 2_756 . ?
O1 U1 O5 93.1(4) . . ?
O2 U1 O5 111.3(2) 2_756 . ?
O2 U1 O5 68.7(2) . . ?
O4 U1 O5 43.7(3) . . ?
O4 U1 O5 136.3(3) 2_756 . ?
O5 U1 O5 180.0 2_756 . ?
O1 U1 C15A 87.9(4) 2_756 . ?
O1 U1 C15A 92.1(4) . . ?
O2 U1 C15A 89.1(2) 2_756 . ?
O2 U1 C15A 90.9(2) . . ?
O4 U1 C15A 21.5(3) . . ?
O4 U1 C15A 158.5(3) 2_756 . ?
O5 U1 C15A 157.8(3) 2_756 . ?
O5 U1 C15A 22.2(3) . . ?
O1 U1 C15A 92.1(4) 2_756 2_756 ?
O1 U1 C15A 87.9(4) . 2_756 ?
O2 U1 C15A 90.9(2) 2_756 2_756 ?
O2 U1 C15A 89.1(2) . 2_756 ?
O4 U1 C15A 158.5(3) . 2_756 ?
O4 U1 C15A 21.5(3) 2_756 2_756 ?
O5 U1 C15A 22.2(3) 2_756 2_756 ?
O5 U1 C15A 157.8(3) . 2_756 ?
C15A U1 C15A 180.0 . 2_756 ?
C20 O2 U1 148.6(5) . . ?
O4 C15A O5 114.8(13) . . ?
O4 C15A C29 122.0(10) . . ?
O5 C15A C29 122.3(11) . . ?
O4 C15A U1 55.9(7) . . ?
O5 C15A U1 59.0(7) . . ?
C29 C15A U1 166.4(11) . . ?
C15A O4 U1 102.6(9) . . ?
C15A O5 U1 98.7(9) . . ?
O6 C15B O7 126.6(13) . . ?
O6 C15B C29 108.9(14) . . ?
O7 C15B C29 124.4(11) . . ?
C15B O6 U1 127.4(9) . . ?
C22 C21 C24 119.6(4) . . ?
C22 C21 C20 121.4(4) . . ?
C24 C21 C20 119.0(4) . . ?
O3 C20 O2 125.5(5) . . ?
O3 C20 C21 119.6(5) . . ?
O2 C20 C21 114.6(5) . . ?
C23 C22 C21 119.2(4) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
N74 C23 C22 120.4(4) . . ?
N74 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C25 C24 C21 119.5(4) . . ?
C25 C24 H24 120.2 . . ?
C21 C24 H24 120.2 . . ?
N74 C25 C24 119.8(4) . . ?
N74 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
N74 C26 C27 111.7(3) . . ?
N74 C26 H26A 109.3 . . ?
C27 C26 H26A 109.3 . . ?
N74 C26 H26B 109.3 . . ?
C27 C26 H26B 109.3 . . ?
H26A C26 H26B 108.0 . . ?
C28 C27 C26 110.6(3) . . ?
C28 C27 H27A 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 108.1 . . ?
C28 C28 C27 112.5(5) 2_666 . ?
C28 C28 H28A 109.1 2_666 . ?
C27 C28 H28A 109.1 . . ?
C28 C28 H28B 109.1 2_666 . ?
C27 C28 H28B 109.1 . . ?
H28A C28 H28B 107.8 . . ?
C32 C29 C30 119.4(5) . . ?
C32 C29 C15A 137.7(10) . . ?
C30 C29 C15A 102.9(9) . . ?
C32 C29 C15B 105.1(8) . . ?
C30 C29 C15B 135.5(8) . . ?
C29 C30 C31 120.4(6) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
N73 C31 C30 118.0(6) . . ?
N73 C31 H31 121.0 . . ?
C30 C31 H31 121.0 . . ?
C33 C32 C29 119.2(6) . . ?
C33 C32 H32 120.4 . . ?
C29 C32 H32 120.4 . . ?
N73 C33 C32 121.7(5) . . ?
N73 C33 H33 119.1 . . ?
C32 C33 H33 119.1 . . ?
N73 C34 C35 113.9(3) . . ?
N73 C34 H34A 108.8 . . ?
C35 C34 H34A 108.8 . . ?
N73 C34 H34B 108.8 . . ?
C35 C34 H34B 108.8 . . ?
H34A C34 H34B 107.7 . . ?
C34 C35 C36 111.6(3) . . ?
C34 C35 H35A 109.3 . . ?
C36 C35 H35A 109.3 . . ?
C34 C35 H35B 109.3 . . ?
C36 C35 H35B 109.3 . . ?
H35A C35 H35B 108.0 . . ?
C36 C36 C35 113.3(4) 2_657 . ?
C36 C36 H36A 108.9 2_657 . ?
C35 C36 H36A 108.9 . . ?
C36 C36 H36B 108.9 2_657 . ?
C35 C36 H36B 108.9 . . ?
H36A C36 H36B 107.7 . . ?
N84 C37 N75 113.3(3) 2_666 . ?
N84 C37 H37A 108.9 2_666 . ?
N75 C37 H37A 108.9 . . ?
N84 C37 H37B 108.9 2_666 . ?
N75 C37 H37B 108.9 . . ?
H37A C37 H37B 107.7 . . ?
O13 C38 N76 125.5(4) . . ?
O13 C38 N75 126.3(4) . . ?
N76 C38 N75 108.2(3) . . ?
N85 C39 N75 115.8(3) 2_666 . ?
N85 C39 C40 102.6(3) 2_666 . ?
N75 C39 C40 103.5(3) . . ?
N85 C39 H39 111.4 2_666 . ?
N75 C39 H39 111.4 . . ?
C40 C39 H39 111.4 . . ?
N76 C40 N86 115.6(3) . 2_666 ?
N76 C40 C39 102.4(3) . . ?
N86 C40 C39 103.4(3) 2_666 . ?
N76 C40 H40 111.6 . . ?
N86 C40 H40 111.6 2_666 . ?
C39 C40 H40 111.6 . . ?
N76 C41 N78 113.6(3) . . ?
N76 C41 H41A 108.8 . . ?
N78 C41 H41A 108.8 . . ?
N76 C41 H41B 108.8 . . ?
N78 C41 H41B 108.8 . . ?
H41A C41 H41B 107.7 . . ?
N77 C42 N86 113.4(3) . 2_666 ?
N77 C42 H42A 108.9 . . ?
N86 C42 H42A 108.9 2_666 . ?
N77 C42 H42B 108.9 . . ?
N86 C42 H42B 108.9 2_666 . ?
H42A C42 H42B 107.7 . . ?
N78 C43 N77 114.9(3) . . ?
N78 C43 C44 103.5(3) . . ?
N77 C43 C44 103.2(3) . . ?
N78 C43 H43 111.5 . . ?
N77 C43 H43 111.5 . . ?
C44 C43 H43 111.5 . . ?
N80 C44 N79 114.8(3) . . ?
N80 C44 C43 103.9(3) . . ?
N79 C44 C43 102.9(3) . . ?
N80 C44 H44 111.5 . . ?
N79 C44 H44 111.5 . . ?
C43 C44 H44 111.5 . . ?
O9 C45 N77 126.3(4) . . ?
O9 C45 N80 125.9(4) . . ?
N77 C45 N80 107.8(4) . . ?
O12 C46 N79 126.2(4) . . ?
O12 C46 N78 125.5(4) . . ?
N79 C46 N78 108.4(3) . . ?
N80 C47 N82 113.6(3) . . ?
N80 C47 H47A 108.8 . . ?
N82 C47 H47A 108.8 . . ?
N80 C47 H47B 108.8 . . ?
N82 C47 H47B 108.8 . . ?
H47A C47 H47B 107.7 . . ?
N81 C48 N79 113.0(3) . . ?
N81 C48 H48A 109.0 . . ?
N79 C48 H48A 109.0 . . ?
N81 C48 H48B 109.0 . . ?
N79 C48 H48B 109.0 . . ?
H48A C48 H48B 107.8 . . ?
N82 C49 N81 115.9(3) . . ?
N82 C49 C50 103.2(3) . . ?
N81 C49 C50 103.2(3) . . ?
N82 C49 H49 111.3 . . ?
N81 C49 H49 111.3 . . ?
C50 C49 H49 111.3 . . ?
N84 C50 N83 115.9(3) . . ?
N84 C50 C49 103.0(3) . . ?
N83 C50 C49 103.2(3) . . ?
N84 C50 H50 111.4 . . ?
N83 C50 H50 111.4 . . ?
C49 C50 H50 111.4 . . ?
O11 C51 N83 125.9(4) . . ?
O11 C51 N81 126.0(4) . . ?
N83 C51 N81 108.0(3) . . ?
O8 C52 N82 127.0(4) . . ?
O8 C52 N84 125.7(4) . . ?
N82 C52 N84 107.3(3) . . ?
N83 C53 N85 113.4(3) . . ?
N83 C53 H53A 108.9 . . ?
N85 C53 H53A 108.9 . . ?
N83 C53 H53B 108.9 . . ?
N85 C53 H53B 108.9 . . ?
H53A C53 H53B 107.7 . . ?
O10 C54 N85 125.8(4) . . ?
O10 C54 N86 125.6(4) . . ?
N85 C54 N86 108.6(3) . . ?
N87 C55 N88 114.7(3) . . ?
N87 C55 C56 102.8(3) . . ?
N88 C55 C56 103.5(3) . . ?
N87 C55 H55 111.7 . . ?
N88 C55 H55 111.7 . . ?
C56 C55 H55 111.7 . . ?
N90 C56 N89 115.2(3) . . ?
N90 C56 C55 102.9(3) . . ?
N89 C56 C55 103.7(3) . . ?
N90 C56 H56 111.5 . . ?
N89 C56 H56 111.5 . . ?
C55 C56 H56 111.5 . . ?
O16 C57 N90 126.0(4) . . ?
O16 C57 N88 125.4(4) . . ?
N90 C57 N88 108.6(3) . . ?
O17 C58 N89 126.1(4) . . ?
O17 C58 N87 126.2(4) . . ?
N89 C58 N87 107.8(3) . . ?
N92 C59 N90 113.4(3) . . ?
N92 C59 H59A 108.9 . . ?
N90 C59 H59A 108.9 . . ?
N92 C59 H59B 108.9 . . ?
N90 C59 H59B 108.9 . . ?
H59A C59 H59B 107.7 . . ?
N91 C60 N89 114.7(3) . . ?
N91 C60 H60A 108.6 . . ?
N89 C60 H60A 108.6 . . ?
N91 C60 H60B 108.6 . . ?
N89 C60 H60B 108.6 . . ?
H60A C60 H60B 107.6 . . ?
O15 C61 N92 126.2(4) . . ?
O15 C61 N94 125.7(4) . . ?
N92 C61 N94 108.1(3) . . ?
O18 C62 N91 126.0(4) . . ?
O18 C62 N93 126.0(4) . . ?
N91 C62 N93 108.0(3) . . ?
N92 C63 N91 115.5(3) . . ?
N92 C63 C64 102.9(3) . . ?
N91 C63 C64 103.3(3) . . ?
N92 C63 H63 111.5 . . ?
N91 C63 H63 111.5 . . ?
C64 C63 H63 111.5 . . ?
N94 C64 N93 115.0(3) . . ?
N94 C64 C63 103.4(3) . . ?
N93 C64 C63 103.2(3) . . ?
N94 C64 H64 111.5 . . ?
N93 C64 H64 111.5 . . ?
C63 C64 H64 111.5 . . ?
N93 C65 N95 113.7(3) . . ?
N93 C65 H65A 108.8 . . ?
N95 C65 H65A 108.8 . . ?
N93 C65 H65B 108.8 . . ?
N95 C65 H65B 108.8 . . ?
H65A C65 H65B 107.7 . . ?
N94 C66 N97 113.4(3) . . ?
N94 C66 H66A 108.9 . . ?
N97 C66 H66A 108.9 . . ?
N94 C66 H66B 108.9 . . ?
N97 C66 H66B 108.9 . . ?
H66A C66 H66B 107.7 . . ?
N97 C67 N95 115.6(3) . . ?
N97 C67 C68 103.4(3) . . ?
N95 C67 C68 103.4(3) . . ?
N97 C67 H67 111.3 . . ?
N95 C67 H67 111.3 . . ?
C68 C67 H67 111.3 . . ?
N98 C68 N99 115.3(3) . . ?
N98 C68 C67 103.4(3) . . ?
N99 C68 C67 103.2(3) . . ?
N98 C68 H68 111.4 . . ?
N99 C68 H68 111.4 . . ?
C67 C68 H68 111.4 . . ?
O19 C69 N98 125.5(4) . . ?
O19 C69 N95 125.8(4) . . ?
N98 C69 N95 108.6(3) . . ?
O14 C70 N97 125.9(4) . . ?
O14 C70 N99 125.7(4) . . ?
N97 C70 N99 108.4(3) . . ?
N87 C71 N99 113.8(3) 2_657 . ?
N87 C71 H71A 108.8 2_657 . ?
N99 C71 H71A 108.8 . . ?
N87 C71 H71B 108.8 2_657 . ?
N99 C71 H71B 108.8 . . ?
H71A C71 H71B 107.7 . . ?
N88 C72 N98 113.9(3) 2_657 . ?
N88 C72 H72A 108.8 2_657 . ?
N98 C72 H72A 108.8 . . ?
N88 C72 H72B 108.8 2_657 . ?
N98 C72 H72B 108.8 . . ?
H72A C72 H72B 107.7 . . ?
C31 N73 C33 121.2(4) . . ?
C31 N73 C34 119.9(4) . . ?
C33 N73 C34 118.9(4) . . ?
C25 N74 C23 121.5(4) . . ?
C25 N74 C26 119.6(4) . . ?
C23 N74 C26 118.9(4) . . ?
C38 N75 C37 122.1(4) . . ?
C38 N75 C39 111.7(3) . . ?
C37 N75 C39 123.2(3) . . ?
C38 N76 C41 123.0(3) . . ?
C38 N76 C40 113.0(3) . . ?
C41 N76 C40 123.6(4) . . ?
C45 N77 C42 122.7(4) . . ?
C45 N77 C43 112.7(3) . . ?
C42 N77 C43 123.0(3) . . ?
C46 N78 C41 121.7(3) . . ?
C46 N78 C43 112.0(3) . . ?
C41 N78 C43 123.3(3) . . ?
C46 N79 C48 122.7(3) . . ?
C46 N79 C44 112.5(3) . . ?
C48 N79 C44 123.1(3) . . ?
C45 N80 C47 122.9(4) . . ?
C45 N80 C44 112.0(3) . . ?
C47 N80 C44 123.4(4) . . ?
C51 N81 C48 122.4(4) . . ?
C51 N81 C49 111.9(3) . . ?
C48 N81 C49 123.3(4) . . ?
C52 N82 C49 113.1(4) . . ?
C52 N82 C47 122.2(4) . . ?
C49 N82 C47 124.3(4) . . ?
C51 N83 C53 122.5(4) . . ?
C51 N83 C50 112.7(3) . . ?
C53 N83 C50 123.3(3) . . ?
C52 N84 C50 113.0(3) . . ?
C52 N84 C37 122.2(4) . 2_666 ?
C50 N84 C37 124.3(4) . 2_666 ?
C54 N85 C39 113.1(3) . 2_666 ?
C54 N85 C53 122.8(3) . . ?
C39 N85 C53 124.1(3) 2_666 . ?
C54 N86 C42 121.5(3) . 2_666 ?
C54 N86 C40 111.4(3) . 2_666 ?
C42 N86 C40 123.1(3) 2_666 2_666 ?
C58 N87 C71 122.6(3) . 2_657 ?
C58 N87 C55 113.1(3) . . ?
C71 N87 C55 124.2(4) 2_657 . ?
C57 N88 C72 122.0(3) . 2_657 ?
C57 N88 C55 112.0(3) . . ?
C72 N88 C55 123.6(3) 2_657 . ?
C58 N89 C56 112.4(3) . . ?
C58 N89 C60 123.0(3) . . ?
C56 N89 C60 124.0(3) . . ?
C57 N90 C59 123.2(3) . . ?
C57 N90 C56 112.7(3) . . ?
C59 N90 C56 123.4(3) . . ?
C62 N91 C60 123.3(3) . . ?
C62 N91 C63 112.5(3) . . ?
C60 N91 C63 123.9(3) . . ?
C61 N92 C59 121.8(3) . . ?
C61 N92 C63 112.5(3) . . ?
C59 N92 C63 123.5(3) . . ?
C62 N93 C65 120.9(3) . . ?
C62 N93 C64 111.2(3) . . ?
C65 N93 C64 120.3(3) . . ?
C61 N94 C66 123.2(3) . . ?
C61 N94 C64 112.3(3) . . ?
C66 N94 C64 124.1(3) . . ?
C69 N95 C67 112.1(3) . . ?
C69 N95 C65 123.2(3) . . ?
C67 N95 C65 123.8(3) . . ?
C70 N97 C67 112.6(3) . . ?
C70 N97 C66 122.4(3) . . ?
C67 N97 C66 122.3(3) . . ?
C69 N98 C68 112.3(3) . . ?
C69 N98 C72 123.3(3) . . ?
C68 N98 C72 124.3(3) . . ?
C70 N99 C71 121.6(3) . . ?
C70 N99 C68 111.5(3) . . ?
C71 N99 C68 123.0(3) . . ?

_refine_diff_density_max         2.236
_refine_diff_density_min         -1.409
_refine_diff_density_rms         0.106

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_7-aUP-170K
_database_code_depnum_ccdc_archive 'CCDC 1534040'
_audit_update_record             
;
2017-02-22 deposited with the CCDC.
2017-05-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C108 H106 Br2 N52 O34 U'
_chemical_formula_weight         3074.29

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'
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'
Br Br -0.2901 2.4595 '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                   12.6201(4)
_cell_length_b                   15.5773(6)
_cell_length_c                   17.0824(6)
_cell_angle_alpha                89.556(2)
_cell_angle_beta                 81.972(2)
_cell_angle_gamma                84.793(2)
_cell_volume                     3311.5(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    9813
_cell_measurement_theta_min      2.88
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_F_000             1552
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    1.925
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            59429
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.884
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             15107
_reflns_number_gt                13172
_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       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1384P)²+19.4333P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15107
_refine_ls_number_parameters     926
_refine_ls_number_restraints     918
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0747
_refine_ls_wR_factor_ref         0.2203
_refine_ls_wR_factor_gt          0.2059
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.028
_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 0.5000 0.5000 0.5000 0.02273(12) Uani 1 2 d S U P . .
N1 N 0.1736(4) 0.1775(3) 0.6181(3) 0.0236(10) Uani 1 1 d . U . . .
C1 C 0.4258(5) 0.3390(4) 0.6206(4) 0.0270(12) Uani 1 1 d . U . . .
Br1 Br 0.5802(3) 0.8874(3) 1.1519(2) 0.1214(14) Uani 0.5 1 d . . P . .
O1 O 0.5971(4) 0.4140(3) 0.4691(3) 0.0356(11) Uani 1 1 d . U . . .
O4 O 0.6508(8) 0.5813(6) 0.5553(5) 0.030(2) Uani 0.507(9) 1 d . U P A 1
O5 O 0.5628(8) 0.5012(6) 0.6417(6) 0.033(2) Uani 0.507(9) 1 d . U P A 1
O6 O 0.6096(7) 0.5289(6) 0.5878(5) 0.024(2) Uani 0.493(9) 1 d . U P A 2
O7 O 0.5207(9) 0.6362(7) 0.6645(7) 0.040(3) Uani 0.493(9) 1 d . U P A 2
O3 O 0.5005(4) 0.3139(3) 0.6556(4) 0.0394(12) Uani 1 1 d . U . . .
N3 N 0.9510(4) 0.2807(3) 0.8509(3) 0.0192(9) Uani 1 1 d . U . . .
C3 C 0.2465(5) 0.3087(4) 0.5847(4) 0.0275(12) Uani 1 1 d . U . . .
H3 H 0.2412 0.3641 0.5610 0.033 Uiso 1 1 calc R U . . .
O9 O 0.8206(3) 0.3634(3) 1.2162(2) 0.0209(8) Uani 1 1 d . U . . .
C9 C -0.0003(5) 0.0217(4) 0.5394(4) 0.0294(13) Uani 1 1 d . U . . .
H02U H 0.0049 -0.0230 0.5806 0.035 Uiso 1 1 calc R U . . .
H02V H -0.0693 0.0573 0.5533 0.035 Uiso 1 1 calc R U . . .
N9 N 0.8708(4) 0.6806(3) 1.2017(3) 0.0221(9) Uani 1 1 d . U . . .
O8 O 1.0029(3) 0.2249(3) 1.0991(2) 0.0237(8) Uani 1 1 d . U . . .
C8 C 0.0912(5) 0.0780(4) 0.5389(4) 0.0269(12) Uani 1 1 d . U . . .
H02I H 0.1606 0.0424 0.5272 0.032 Uiso 1 1 calc R U . . .
H02J H 0.0875 0.1221 0.4970 0.032 Uiso 1 1 calc R U . . .
N8 N 0.8079(4) 0.7434(3) 1.0828(3) 0.0200(9) Uani 1 1 d . U . . .
C7 C 0.0845(6) 0.1216(5) 0.6179(4) 0.0332(14) Uani 1 1 d . U . . .
H02O H 0.0148 0.1568 0.6297 0.040 Uiso 1 1 calc R U . . .
H02P H 0.0884 0.0774 0.6597 0.040 Uiso 1 1 calc R U . . .
N7 N 0.6879(4) 0.6481(3) 1.0910(3) 0.0221(9) Uani 1 1 d . U . . .
C6 C 0.3434(5) 0.2001(4) 0.6528(3) 0.0218(11) Uani 1 1 d . U . . .
H01F H 0.4046 0.1803 0.6767 0.026 Uiso 1 1 calc R U . . .
N6 N 0.6168(4) 0.5157(3) 1.0588(3) 0.0227(10) Uani 1 1 d . U . . .
C5 C 0.2612(5) 0.1490(4) 0.6516(4) 0.0249(11) Uani 1 1 d . U . . .
H02Q H 0.2656 0.0932 0.6745 0.030 Uiso 1 1 calc R U . . .
N5 N 0.6554(4) 0.3886(3) 0.9988(3) 0.0233(10) Uani 1 1 d . U . . .
C4 C 0.1646(5) 0.2563(4) 0.5851(4) 0.0284(12) Uani 1 1 d . U . . .
H4 H 0.1021 0.2754 0.5623 0.034 Uiso 1 1 calc R U . . .
N4 N 0.7835(4) 0.2920(3) 0.9127(3) 0.0222(10) Uani 1 1 d . U . . .
O10 O 0.8924(3) 0.5547(3) 1.2722(3) 0.0247(9) Uani 1 1 d . U . . .
C10 C 0.6385(11) 0.5463(9) 0.6216(8) 0.0227(19) Uani 0.507(9) 1 d . U P A .
N10 N 0.7387(4) 0.5950(3) 1.2174(3) 0.0203(9) Uani 1 1 d . U . . .
O11 O 0.7415(4) 0.7080(3) 0.9697(3) 0.0271(9) Uani 1 1 d . U . . .
C11 C 0.5987(11) 0.5818(9) 0.6455(8) 0.024(2) Uani 0.493(9) 1 d . U P A .
N11 N 0.6868(4) 0.4575(3) 1.1754(3) 0.0190(9) Uani 1 1 d . U . . .
O12 O 0.6430(4) 0.5110(3) 0.9222(3) 0.0305(10) Uani 1 1 d . U . . .
C12 C 0.7037(6) 0.5696(5) 0.6863(4) 0.0374(14) Uani 1 1 d . U . . .
N12 N 0.7248(4) 0.3300(3) 1.1165(3) 0.0197(9) Uani 1 1 d . U . . .
O13 O 0.8240(4) 0.3754(3) 0.8020(2) 0.0243(8) Uani 1 1 d . U . . .
C13 C 0.6773(6) 0.6132(5) 0.7577(5) 0.0387(15) Uani 1 1 d . U . . .
H02Y H 0.6071 0.6407 0.7724 0.046 Uiso 1 1 calc R U . . .
N13 N 0.8564(4) 0.2391(3) 1.0309(3) 0.0195(9) Uani 1 1 d . U . . .
O14 O 0.3434(4) 0.0998(3) 0.4469(3) 0.0280(9) Uani 1 1 d . U . . .
C14 C 0.7537(5) 0.6159(4) 0.8064(4) 0.0270(12) Uani 1 1 d . U . . .
H14 H 0.7358 0.6452 0.8557 0.032 Uiso 1 1 calc R U . . .
N14 N 1.0182(4) 0.2079(3) 0.9640(3) 0.0205(9) Uani 1 1 d . U . . .
O15 O 0.3056(4) -0.0404(3) 0.6143(3) 0.0260(9) Uani 1 1 d . U . . .
C15 C 0.8810(6) 0.5351(4) 0.7174(4) 0.0303(13) Uani 1 1 d . U . . .
H02X H 0.9516 0.5080 0.7037 0.036 Uiso 1 1 calc R U . . .
N15 N 0.2922(4) 0.0730(3) 0.3244(3) 0.0231(10) Uani 1 1 d . U . . .
O16 O 0.0760(4) -0.0199(3) 0.7678(4) 0.0398(12) Uani 1 1 d . U . . .
C16 C 0.8043(7) 0.5306(5) 0.6663(4) 0.0419(16) Uani 1 1 d . U . . .
H02W H 0.8226 0.5002 0.6176 0.050 Uiso 1 1 calc R U . . .
N16 N 0.3558(4) -0.0368(3) 0.3932(3) 0.0230(10) Uani 1 1 d . U . . .
O17 O -0.1135(3) 0.1425(3) 0.7482(3) 0.0251(9) Uani 1 1 d . U . . .
C17 C 0.9339(5) 0.5852(4) 0.8416(3) 0.0224(11) Uani 1 1 d . U . . .
H01K H 0.9240 0.6438 0.8650 0.027 Uiso 1 1 calc R U . . .
H01N H 1.0070 0.5773 0.8114 0.027 Uiso 1 1 calc R U . . .
N17 N 0.3250(4) -0.1298(3) 0.5056(3) 0.0223(10) Uani 1 1 d . U . . .
O19 O -0.1483(4) -0.2694(3) 0.5792(3) 0.0297(9) Uani 1 1 d . U . . .
C19 C 1.0030(5) 0.5326(4) 0.9664(3) 0.0217(11) Uani 1 1 d . U . . .
H01H H 1.0771 0.5283 0.9378 0.026 Uiso 1 1 calc R U . . .
H01I H 0.9871 0.5914 0.9891 0.026 Uiso 1 1 calc R U . . .
N19 N 0.2333(4) -0.2285(3) 0.4341(3) 0.0225(10) Uani 1 1 d . U . . .
O18 O 0.0749(4) -0.2907(3) 0.4320(3) 0.0338(10) Uani 1 1 d . U . . .
C18 C 0.9248(5) 0.5194(4) 0.9078(3) 0.0209(11) Uani 1 1 d . U . . .
H01C H 0.9402 0.4606 0.8850 0.025 Uiso 1 1 calc R U . . .
H01D H 0.8505 0.5244 0.9360 0.025 Uiso 1 1 calc R U . . .
N18 N 0.2347(4) -0.1719(3) 0.6180(3) 0.0196(9) Uani 1 1 d . U . . .
Br2 Br 0.5248(7) 0.7647(5) 0.5606(5) 0.219(3) Uani 0.5 1 d . . P . .
C2 C 0.3365(4) 0.2811(4) 0.6186(3) 0.0201(10) Uani 1 1 d . U . . .
N2 N 0.8537(4) 0.5783(3) 0.7863(3) 0.0172(9) Uani 1 1 d . U . . .
O2 O 0.4117(4) 0.4122(3) 0.5879(3) 0.0395(12) Uani 1 1 d . U . . .
C39 C 0.9479(5) 0.2074(4) 0.9041(3) 0.0190(10) Uani 1 1 d . U . . .
H01J H 0.9587 0.1516 0.8743 0.023 Uiso 1 1 calc R U . . .
C38 C 1.1319(5) 0.1867(4) 0.9503(4) 0.0221(11) Uani 1 1 d . U . . .
H38 H 1.1650 0.1318 0.9619 0.027 Uiso 1 1 calc R U . . .
C37 C -0.2757(5) -0.1621(4) 0.6989(4) 0.0237(12) Uani 1 1 d . U . . .
H02A H -0.3122 -0.1688 0.7535 0.028 Uiso 1 1 calc R U . . .
H02B H -0.3091 -0.1985 0.6637 0.028 Uiso 1 1 calc R U . . .
C36 C -0.1851(4) 0.1029(4) 0.7296(3) 0.0194(10) Uani 1 1 d . U . . .
C35 C -0.1511(5) -0.0262(4) 0.8096(4) 0.0263(12) Uani 1 1 d . U . . .
H02K H -0.2014 -0.0544 0.8493 0.032 Uiso 1 1 calc R U . . .
H02L H -0.1116 0.0125 0.8382 0.032 Uiso 1 1 calc R U . . .
C34 C -0.1096(5) -0.2424(4) 0.6347(3) 0.0219(10) Uani 1 1 d . U . . .
C33 C -0.0994(5) -0.1794(4) 0.7573(3) 0.0205(10) Uani 1 1 d . U . . .
H33 H -0.1301 -0.2051 0.8084 0.025 Uiso 1 1 calc R U . . .
C32 C 0.0111(4) -0.2268(4) 0.7243(3) 0.0200(10) Uani 1 1 d . U . . .
H32 H 0.0326 -0.2742 0.7602 0.024 Uiso 1 1 calc R U . . .
C31 C 0.0322(5) -0.0830(4) 0.7536(4) 0.0241(11) Uani 1 1 d . U . . .
C30 C 0.0718(5) -0.3183(4) 0.5999(4) 0.0258(12) Uani 1 1 d . U . . .
H02C H 0.1109 -0.3571 0.6345 0.031 Uiso 1 1 calc R U . . .
H02D H 0.0326 -0.3544 0.5684 0.031 Uiso 1 1 calc R U . . .
C40 C 0.8343(5) 0.2207(4) 0.9520(3) 0.0192(10) Uani 1 1 d . U . . .
H40 H 0.7948 0.1680 0.9511 0.023 Uiso 1 1 calc R U . . .
C41 C 0.9634(5) 0.2244(3) 1.0378(3) 0.0186(10) Uani 1 1 d . U . . .
C43 C 0.7752(5) 0.2437(4) 1.0997(3) 0.0201(10) Uani 1 1 d . U . . .
H02M H 0.8084 0.2222 1.1461 0.024 Uiso 1 1 calc R U . . .
H02N H 0.7192 0.2054 1.0915 0.024 Uiso 1 1 calc R U . . .
C42 C 0.8499(5) 0.3215(4) 0.8499(3) 0.0188(10) Uani 1 1 d . U . . .
C44 C 0.6726(5) 0.3259(4) 0.9349(3) 0.0254(12) Uani 1 1 d . U . . .
H02E H 0.6291 0.2772 0.9507 0.030 Uiso 1 1 calc R U . . .
H02F H 0.6459 0.3530 0.8879 0.030 Uiso 1 1 calc R U . . .
C46 C 0.6326(4) 0.3664(4) 1.0818(3) 0.0191(10) Uani 1 1 d . U . . .
H01G H 0.5710 0.3298 1.0919 0.023 Uiso 1 1 calc R U . . .
C45 C 0.7515(4) 0.3811(4) 1.1731(3) 0.0172(10) Uani 1 1 d . U . . .
C47 C 0.6060(4) 0.4560(4) 1.1234(3) 0.0196(10) Uani 1 1 d . U . . .
H47 H 0.5318 0.4619 1.1535 0.024 Uiso 1 1 calc R U . . .
C48 C 0.6396(4) 0.4755(4) 0.9862(4) 0.0224(11) Uani 1 1 d . U . . .
C51 C 0.8400(5) 0.6040(4) 1.2332(3) 0.0197(10) Uani 1 1 d . U . . .
C50 C 0.5973(5) 0.6077(4) 1.0681(4) 0.0250(12) Uani 1 1 d . U . . .
H02R H 0.5340 0.6209 1.1088 0.030 Uiso 1 1 calc R U . . .
H02S H 0.5797 0.6330 1.0177 0.030 Uiso 1 1 calc R U . . .
C49 C 0.6820(4) 0.5188(4) 1.2390(3) 0.0190(10) Uani 1 1 d . U . . .
H01R H 0.7130 0.4896 1.2834 0.023 Uiso 1 1 calc R U . . .
H01S H 0.6057 0.5375 1.2580 0.023 Uiso 1 1 calc R U . . .
C52 C 0.6962(4) 0.6662(4) 1.1731(3) 0.0207(10) Uani 1 1 d . U . . .
H01E H 0.6267 0.6934 1.2014 0.025 Uiso 1 1 calc R U . . .
C54 C 0.7455(4) 0.7001(4) 1.0403(3) 0.0205(10) Uani 1 1 d . U . . .
C53 C 0.7852(5) 0.7293(4) 1.1666(3) 0.0214(11) Uani 1 1 d . U . . .
H53 H 0.7598 0.7843 1.1960 0.026 Uiso 1 1 calc R U . . .
C55 C 0.9673(5) 0.7176(4) 1.2173(3) 0.0223(11) Uani 1 1 d . U . . .
H02H H 0.9760 0.7387 1.2679 0.027 Uiso 1 1 calc R U . . .
C29 C 0.1985(5) -0.1729(4) 0.7020(3) 0.0200(10) Uani 1 1 d . U . . .
H01A H 0.2227 -0.2293 0.7236 0.024 Uiso 1 1 calc R U . . .
H01B H 0.2321 -0.1278 0.7279 0.024 Uiso 1 1 calc R U . . .
C24 C 0.2895(4) -0.1069(3) 0.5827(3) 0.0180(10) Uani 1 1 d . U . . .
N24 N -0.1639(4) -0.1924(3) 0.6957(3) 0.0222(9) Uani 1 1 d . U . . .
C26 C 0.2473(5) -0.2492(4) 0.5690(3) 0.0196(10) Uani 1 1 d . U . . .
H26 H 0.2894 -0.2978 0.5925 0.024 Uiso 1 1 calc R U . . .
N26 N -0.2540(4) 0.1306(3) 0.6767(3) 0.0218(10) Uani 1 1 d . U . . .
C25 C 0.3082(4) -0.2181(4) 0.4895(3) 0.0196(10) Uani 1 1 d . U . . .
H25 H 0.3778 -0.2538 0.4741 0.024 Uiso 1 1 calc R U . . .
N25 N -0.2118(4) 0.0242(3) 0.7577(3) 0.0248(10) Uani 1 1 d . U . . .
C28 C 0.1450(5) -0.2664(4) 0.4672(4) 0.0234(11) Uani 1 1 d . U . . .
C27 C 0.2616(5) -0.2193(4) 0.3495(3) 0.0225(11) Uani 1 1 d . U . . .
H01P H 0.2136 -0.2519 0.3222 0.027 Uiso 1 1 calc R U . . .
H01Q H 0.3361 -0.2452 0.3339 0.027 Uiso 1 1 calc R U . . .
C23 C 0.4010(5) -0.0813(4) 0.4569(4) 0.0239(12) Uani 1 1 d . U . . .
H02T H 0.4733 -0.0789 0.4658 0.029 Uiso 1 1 calc R U . . .
N23 N -0.0056(4) -0.2601(3) 0.6490(3) 0.0246(10) Uani 1 1 d . U . . .
C22 C 0.3432(4) -0.0764(4) 0.3197(3) 0.0213(11) Uani 1 1 d . U . . .
H22 H 0.4121 -0.1076 0.2945 0.026 Uiso 1 1 calc R U . . .
N22 N -0.0748(4) -0.0921(3) 0.7682(3) 0.0249(10) Uani 1 1 d . U . . .
C20 C 0.3324(4) 0.0502(4) 0.3940(3) 0.0217(11) Uani 1 1 d . U . . .
N20 N 0.1490(4) -0.2752(3) 0.5467(3) 0.0243(10) Uani 1 1 d . U . . .
C21 C 0.3079(5) 0.0014(4) 0.2691(3) 0.0220(11) Uani 1 1 d . U . . .
H02G H 0.3645 0.0111 0.2235 0.026 Uiso 1 1 calc R U . . .
N21 N 0.0832(4) -0.1582(3) 0.7208(3) 0.0225(10) Uani 1 1 d . 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 O1 1.762(4) 2_666 ?
U1 O1 1.762(4) . ?
U1 O6 2.251(9) 2_666 ?
U1 O6 2.251(9) . ?
U1 O2 2.268(5) . ?
U1 O2 2.268(5) 2_666 ?
U1 O5 2.651(9) 2_666 ?
U1 O5 2.651(9) . ?
U1 O4 2.659(9) 2_666 ?
U1 O4 2.659(9) . ?
U1 C10 3.025(13) 2_666 ?
U1 C10 3.025(13) . ?
N1 C4 1.349(8) . ?
N1 C5 1.353(8) . ?
N1 C7 1.485(8) . ?
C1 O3 1.220(9) . ?
C1 O2 1.275(8) . ?
C1 C2 1.510(8) . ?
O4 C10 1.249(15) . ?
O4 C11 1.588(16) . ?
O5 C10 1.246(16) . ?
O5 C11 1.378(16) . ?
O6 C10 0.786(13) . ?
O6 C11 1.274(17) . ?
O7 C11 1.248(19) . ?
N3 C42 1.376(8) . ?
N3 C55 1.446(7) 2_767 ?
N3 C39 1.454(7) . ?
C3 C4 1.374(9) . ?
C3 C2 1.379(8) . ?
C3 H3 0.9500 . ?
O9 C45 1.229(7) . ?
C9 C9 1.509(13) 2_556 ?
C9 C8 1.512(9) . ?
C9 H02U 0.9900 . ?
C9 H02V 0.9900 . ?
N9 C51 1.371(8) . ?
N9 C55 1.451(8) . ?
N9 C53 1.458(8) . ?
O8 C41 1.220(7) . ?
C8 C7 1.504(9) . ?
C8 H02I 0.9900 . ?
C8 H02J 0.9900 . ?
N8 C54 1.367(8) . ?
N8 C53 1.440(7) . ?
N8 C38 1.449(7) 2_767 ?
C7 H02O 0.9900 . ?
C7 H02P 0.9900 . ?
N7 C54 1.362(8) . ?
N7 C52 1.453(8) . ?
N7 C50 1.454(8) . ?
C6 C5 1.365(9) . ?
C6 C2 1.387(8) . ?
C6 H01F 0.9500 . ?
N6 C48 1.375(8) . ?
N6 C50 1.438(8) . ?
N6 C47 1.438(7) . ?
C5 H02Q 0.9500 . ?
N5 C48 1.371(8) . ?
N5 C44 1.450(8) . ?
N5 C46 1.452(7) . ?
C4 H4 0.9500 . ?
N4 C42 1.369(7) . ?
N4 C40 1.440(7) . ?
N4 C44 1.450(8) . ?
O10 C51 1.222(7) . ?
C10 C11 0.787(16) . ?
C10 C12 1.533(14) . ?
N10 C51 1.363(8) . ?
N10 C52 1.443(7) . ?
N10 C49 1.460(7) . ?
O11 C54 1.220(7) . ?
C11 C12 1.579(14) . ?
N11 C45 1.380(7) . ?
N11 C49 1.443(7) . ?
N11 C47 1.444(7) . ?
O12 C48 1.218(7) . ?
C12 C16 1.356(12) . ?
C12 C13 1.384(12) . ?
N12 C45 1.353(7) . ?
N12 C43 1.447(7) . ?
N12 C46 1.448(7) . ?
O13 C42 1.223(7) . ?
C13 C14 1.362(9) . ?
C13 H02Y 0.9500 . ?
N13 C41 1.371(7) . ?
N13 C43 1.446(7) . ?
N13 C40 1.449(7) . ?
O14 C20 1.224(8) . ?
C14 N2 1.342(8) . ?
C14 H14 0.9500 . ?
N14 C41 1.366(7) . ?
N14 C38 1.429(8) . ?
N14 C39 1.445(7) . ?
O15 C24 1.219(7) . ?
C15 N2 1.348(8) . ?
C15 C16 1.397(10) . ?
C15 H02X 0.9500 . ?
N15 C20 1.388(7) . ?
N15 C37 1.446(8) 2_556 ?
N15 C21 1.450(8) . ?
O16 C31 1.213(8) . ?
C16 H02W 0.9500 . ?
N16 C20 1.360(8) . ?
N16 C22 1.438(8) . ?
N16 C23 1.442(7) . ?
O17 C36 1.219(7) . ?
C17 N2 1.488(6) . ?
C17 C18 1.521(8) . ?
C17 H01K 0.9900 . ?
C17 H01N 0.9900 . ?
N17 C24 1.369(8) . ?
N17 C23 1.443(7) . ?
N17 C25 1.445(7) . ?
O19 C34 1.220(8) . ?
C19 C19 1.525(11) 2_767 ?
C19 C18 1.528(7) . ?
C19 H01H 0.9900 . ?
C19 H01I 0.9900 . ?
N19 C28 1.360(8) . ?
N19 C27 1.448(8) . ?
N19 C25 1.449(7) . ?
O18 C28 1.225(8) . ?
C18 H01C 0.9900 . ?
C18 H01D 0.9900 . ?
N18 C24 1.367(7) . ?
N18 C29 1.444(7) . ?
N18 C26 1.455(7) . ?
C39 C40 1.546(8) . ?
C39 H01J 1.0000 . ?
C38 N8 1.449(7) 2_767 ?
C38 H38 0.9500 . ?
C37 N24 1.440(7) . ?
C37 N15 1.446(8) 2_556 ?
C37 H02A 0.9900 . ?
C37 H02B 0.9900 . ?
C36 N25 1.366(8) . ?
C36 N26 1.379(7) . ?
C35 N25 1.436(7) . ?
C35 N22 1.457(8) . ?
C35 H02K 0.9900 . ?
C35 H02L 0.9900 . ?
C34 N24 1.371(8) . ?
C34 N23 1.371(8) . ?
C33 N22 1.442(8) . ?
C33 N24 1.443(7) . ?
C33 C32 1.551(8) . ?
C33 H33 1.0000 . ?
C32 N23 1.440(8) . ?
C32 N21 1.460(7) . ?
C32 H32 1.0000 . ?
C31 N22 1.358(8) . ?
C31 N21 1.368(8) . ?
C30 N20 1.445(8) . ?
C30 N23 1.450(8) . ?
C30 H02C 0.9900 . ?
C30 H02D 0.9900 . ?
C40 H40 1.0000 . ?
C43 H02M 0.9900 . ?
C43 H02N 0.9900 . ?
C44 H02E 0.9900 . ?
C44 H02F 0.9900 . ?
C46 C47 1.560(8) . ?
C46 H01G 1.0000 . ?
C47 H47 1.0000 . ?
C50 H02R 0.9900 . ?
C50 H02S 0.9900 . ?
C49 H01R 0.9900 . ?
C49 H01S 0.9900 . ?
C52 C53 1.551(8) . ?
C52 H01E 1.0000 . ?
C53 H53 1.0000 . ?
C55 N3 1.446(7) 2_767 ?
C55 H02H 0.9500 . ?
C29 N21 1.444(7) . ?
C29 H01A 0.9900 . ?
C29 H01B 0.9900 . ?
C26 N20 1.440(8) . ?
C26 C25 1.561(8) . ?
C26 H26 1.0000 . ?
N26 C27 1.449(8) 2_556 ?
N26 C22 1.461(7) 2_556 ?
C25 H25 1.0000 . ?
N25 C21 1.444(8) 2_556 ?
C28 N20 1.370(8) . ?
C27 N26 1.449(8) 2_556 ?
C27 H01P 0.9900 . ?
C27 H01Q 0.9900 . ?
C23 H02T 0.9500 . ?
C22 N26 1.461(7) 2_556 ?
C22 C21 1.552(8) . ?
C22 H22 1.0000 . ?
C21 N25 1.444(8) 2_556 ?
C21 H02G 1.0000 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O1 180.0 2_666 . ?
O1 U1 O6 85.4(3) 2_666 2_666 ?
O1 U1 O6 94.6(3) . 2_666 ?
O1 U1 O6 94.6(3) 2_666 . ?
O1 U1 O6 85.4(3) . . ?
O6 U1 O6 180.0 2_666 . ?
O1 U1 O2 89.8(2) 2_666 . ?
O1 U1 O2 90.2(2) . . ?
O6 U1 O2 89.1(3) 2_666 . ?
O6 U1 O2 90.9(3) . . ?
O1 U1 O2 90.2(2) 2_666 2_666 ?
O1 U1 O2 89.8(2) . 2_666 ?
O6 U1 O2 90.9(3) 2_666 2_666 ?
O6 U1 O2 89.1(3) . 2_666 ?
O2 U1 O2 180.0(2) . 2_666 ?
O1 U1 O5 91.1(3) 2_666 2_666 ?
O1 U1 O5 88.9(3) . 2_666 ?
O2 U1 O5 113.4(2) . 2_666 ?
O2 U1 O5 66.6(2) 2_666 2_666 ?
O1 U1 O5 88.9(3) 2_666 . ?
O1 U1 O5 91.1(3) . . ?
O2 U1 O5 66.6(2) . . ?
O2 U1 O5 113.4(2) 2_666 . ?
O5 U1 O5 180.0 2_666 . ?
O1 U1 O4 89.3(3) 2_666 2_666 ?
O1 U1 O4 90.7(3) . 2_666 ?
O2 U1 O4 65.1(2) . 2_666 ?
O2 U1 O4 114.9(2) 2_666 2_666 ?
O5 U1 O4 48.4(3) 2_666 2_666 ?
O5 U1 O4 131.6(3) . 2_666 ?
O1 U1 O4 90.7(3) 2_666 . ?
O1 U1 O4 89.3(3) . . ?
O2 U1 O4 114.9(2) . . ?
O2 U1 O4 65.1(2) 2_666 . ?
O5 U1 O4 131.6(3) 2_666 . ?
O5 U1 O4 48.4(3) . . ?
O4 U1 O4 180.0 2_666 . ?
O1 U1 C10 88.4(3) 2_666 2_666 ?
O1 U1 C10 91.6(3) . 2_666 ?
O6 U1 C10 3.0(4) 2_666 2_666 ?
O6 U1 C10 177.0(4) . 2_666 ?
O2 U1 C10 89.4(3) . 2_666 ?
O2 U1 C10 90.6(3) 2_666 2_666 ?
O5 U1 C10 24.2(3) 2_666 2_666 ?
O5 U1 C10 155.8(3) . 2_666 ?
O4 U1 C10 24.3(3) 2_666 2_666 ?
O4 U1 C10 155.7(3) . 2_666 ?
O1 U1 C10 91.6(3) 2_666 . ?
O1 U1 C10 88.4(3) . . ?
O6 U1 C10 177.0(4) 2_666 . ?
O6 U1 C10 3.0(4) . . ?
O2 U1 C10 90.6(3) . . ?
O2 U1 C10 89.4(3) 2_666 . ?
O5 U1 C10 155.8(3) 2_666 . ?
O5 U1 C10 24.2(3) . . ?
O4 U1 C10 155.7(3) 2_666 . ?
O4 U1 C10 24.3(3) . . ?
C10 U1 C10 180.0 2_666 . ?
C4 N1 C5 121.5(5) . . ?
C4 N1 C7 118.7(6) . . ?
C5 N1 C7 119.7(6) . . ?
O3 C1 O2 126.5(6) . . ?
O3 C1 C2 118.2(6) . . ?
O2 C1 C2 115.2(6) . . ?
C10 O4 C11 29.2(7) . . ?
C10 O4 U1 94.5(8) . . ?
C11 O4 U1 96.5(6) . . ?
C10 O5 C11 34.5(8) . . ?
C10 O5 U1 95.0(8) . . ?
C11 O5 U1 102.8(7) . . ?
C10 O6 C11 36.0(12) . . ?
C10 O6 U1 168.2(14) . . ?
C11 O6 U1 132.3(9) . . ?
C42 N3 C55 120.9(5) . 2_767 ?
C42 N3 C39 111.1(5) . . ?
C55 N3 C39 121.2(5) 2_767 . ?
C4 C3 C2 120.0(6) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C9 C9 C8 112.4(7) 2_556 . ?
C9 C9 H02U 109.1 2_556 . ?
C8 C9 H02U 109.1 . . ?
C9 C9 H02V 109.1 2_556 . ?
C8 C9 H02V 109.1 . . ?
H02U C9 H02V 107.9 . . ?
C51 N9 C55 123.3(5) . . ?
C51 N9 C53 112.3(5) . . ?
C55 N9 C53 123.1(5) . . ?
C7 C8 C9 110.0(5) . . ?
C7 C8 H02I 109.7 . . ?
C9 C8 H02I 109.7 . . ?
C7 C8 H02J 109.7 . . ?
C9 C8 H02J 109.7 . . ?
H02I C8 H02J 108.2 . . ?
C54 N8 C53 112.9(5) . . ?
C54 N8 C38 122.6(5) . 2_767 ?
C53 N8 C38 122.5(5) . 2_767 ?
N1 C7 C8 110.5(5) . . ?
N1 C7 H02O 109.5 . . ?
C8 C7 H02O 109.5 . . ?
N1 C7 H02P 109.5 . . ?
C8 C7 H02P 109.5 . . ?
H02O C7 H02P 108.1 . . ?
C54 N7 C52 112.1(5) . . ?
C54 N7 C50 121.3(5) . . ?
C52 N7 C50 122.0(5) . . ?
C5 C6 C2 119.3(6) . . ?
C5 C6 H01F 120.4 . . ?
C2 C6 H01F 120.4 . . ?
C48 N6 C50 123.1(5) . . ?
C48 N6 C47 112.9(5) . . ?
C50 N6 C47 123.8(5) . . ?
N1 C5 C6 120.3(6) . . ?
N1 C5 H02Q 119.8 . . ?
C6 C5 H02Q 119.8 . . ?
C48 N5 C44 122.7(5) . . ?
C48 N5 C46 112.4(5) . . ?
C44 N5 C46 123.9(5) . . ?
N1 C4 C3 119.4(6) . . ?
N1 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C42 N4 C40 112.6(5) . . ?
C42 N4 C44 123.8(5) . . ?
C40 N4 C44 123.5(5) . . ?
O6 C10 C11 108(2) . . ?
C11 C10 O5 82.0(16) . . ?
C11 C10 O4 100.1(16) . . ?
O5 C10 O4 121.4(12) . . ?
O6 C10 C12 172.8(18) . . ?
C11 C10 C12 78.6(15) . . ?
O5 C10 C12 116.7(10) . . ?
O4 C10 C12 121.1(10) . . ?
O6 C10 U1 8.7(11) . . ?
C11 C10 U1 99.4(14) . . ?
O5 C10 U1 60.8(7) . . ?
O4 C10 U1 61.2(7) . . ?
C12 C10 U1 177.1(8) . . ?
C51 N10 C52 113.0(5) . . ?
C51 N10 C49 123.3(5) . . ?
C52 N10 C49 123.7(5) . . ?
C10 C11 O7 161.7(18) . . ?
C10 C11 O6 35.9(12) . . ?
O7 C11 O6 126.2(12) . . ?
C10 C11 O5 63.5(14) . . ?
C10 C11 C12 72.1(14) . . ?
O7 C11 C12 125.8(12) . . ?
O6 C11 C12 108.0(12) . . ?
O5 C11 C12 106.3(10) . . ?
C10 C11 O4 50.7(12) . . ?
O5 C11 O4 94.1(10) . . ?
C12 C11 O4 100.0(9) . . ?
C45 N11 C49 121.4(5) . . ?
C45 N11 C47 112.0(5) . . ?
C49 N11 C47 124.1(5) . . ?
C16 C12 C13 119.7(6) . . ?
C16 C12 C10 106.6(8) . . ?
C13 C12 C10 133.4(9) . . ?
C16 C12 C11 135.3(9) . . ?
C13 C12 C11 104.9(8) . . ?
C10 C12 C11 29.3(6) . . ?
C45 N12 C43 123.0(5) . . ?
C45 N12 C46 113.0(5) . . ?
C43 N12 C46 123.5(5) . . ?
C14 C13 C12 118.9(7) . . ?
C14 C13 H02Y 120.6 . . ?
C12 C13 H02Y 120.6 . . ?
C41 N13 C43 121.2(5) . . ?
C41 N13 C40 112.4(5) . . ?
C43 N13 C40 123.3(5) . . ?
N2 C14 C13 121.5(7) . . ?
N2 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C41 N14 C38 122.4(5) . . ?
C41 N14 C39 112.6(5) . . ?
C38 N14 C39 124.8(5) . . ?
N2 C15 C16 119.2(7) . . ?
N2 C15 H02X 120.4 . . ?
C16 C15 H02X 120.4 . . ?
C20 N15 C37 121.6(5) . 2_556 ?
C20 N15 C21 111.1(5) . . ?
C37 N15 C21 123.6(5) 2_556 . ?
C12 C16 C15 120.0(7) . . ?
C12 C16 H02W 120.0 . . ?
C15 C16 H02W 120.0 . . ?
C20 N16 C22 113.2(5) . . ?
C20 N16 C23 121.9(5) . . ?
C22 N16 C23 124.5(5) . . ?
N2 C17 C18 113.0(4) . . ?
N2 C17 H01K 109.0 . . ?
C18 C17 H01K 109.0 . . ?
N2 C17 H01N 109.0 . . ?
C18 C17 H01N 109.0 . . ?
H01K C17 H01N 107.8 . . ?
C24 N17 C23 121.2(5) . . ?
C24 N17 C25 112.1(5) . . ?
C23 N17 C25 123.6(5) . . ?
C19 C19 C18 113.1(6) 2_767 . ?
C19 C19 H01H 109.0 2_767 . ?
C18 C19 H01H 109.0 . . ?
C19 C19 H01I 109.0 2_767 . ?
C18 C19 H01I 109.0 . . ?
H01H C19 H01I 107.8 . . ?
C28 N19 C27 123.1(5) . . ?
C28 N19 C25 112.6(5) . . ?
C27 N19 C25 122.7(5) . . ?
C17 C18 C19 111.4(4) . . ?
C17 C18 H01C 109.3 . . ?
C19 C18 H01C 109.3 . . ?
C17 C18 H01D 109.3 . . ?
C19 C18 H01D 109.3 . . ?
H01C C18 H01D 108.0 . . ?
C24 N18 C29 122.2(5) . . ?
C24 N18 C26 112.5(5) . . ?
C29 N18 C26 122.6(5) . . ?
C3 C2 C6 119.4(6) . . ?
C3 C2 C1 120.6(5) . . ?
C6 C2 C1 119.9(5) . . ?
C14 N2 C15 120.6(5) . . ?
C14 N2 C17 118.8(5) . . ?
C15 N2 C17 120.6(5) . . ?
C1 O2 U1 140.3(4) . . ?
N14 C39 N3 115.1(5) . . ?
N14 C39 C40 103.5(4) . . ?
N3 C39 C40 103.3(5) . . ?
N14 C39 H01J 111.5 . . ?
N3 C39 H01J 111.5 . . ?
C40 C39 H01J 111.5 . . ?
N14 C38 N8 114.0(5) . 2_767 ?
N14 C38 H38 123.0 . . ?
N8 C38 H38 123.0 2_767 . ?
N24 C37 N15 113.1(5) . 2_556 ?
N24 C37 H02A 109.0 . . ?
N15 C37 H02A 109.0 2_556 . ?
N24 C37 H02B 109.0 . . ?
N15 C37 H02B 109.0 2_556 . ?
H02A C37 H02B 107.8 . . ?
O17 C36 N25 126.2(5) . . ?
O17 C36 N26 125.5(6) . . ?
N25 C36 N26 108.3(5) . . ?
N25 C35 N22 113.0(5) . . ?
N25 C35 H02K 109.0 . . ?
N22 C35 H02K 109.0 . . ?
N25 C35 H02L 109.0 . . ?
N22 C35 H02L 109.0 . . ?
H02K C35 H02L 107.8 . . ?
O19 C34 N24 125.8(6) . . ?
O19 C34 N23 126.1(6) . . ?
N24 C34 N23 108.0(5) . . ?
N22 C33 N24 115.9(5) . . ?
N22 C33 C32 103.4(5) . . ?
N24 C33 C32 102.9(5) . . ?
N22 C33 H33 111.3 . . ?
N24 C33 H33 111.3 . . ?
C32 C33 H33 111.3 . . ?
N23 C32 N21 115.5(5) . . ?
N23 C32 C33 104.0(4) . . ?
N21 C32 C33 102.8(5) . . ?
N23 C32 H32 111.3 . . ?
N21 C32 H32 111.3 . . ?
C33 C32 H32 111.3 . . ?
O16 C31 N22 126.4(6) . . ?
O16 C31 N21 125.4(6) . . ?
N22 C31 N21 108.3(5) . . ?
N20 C30 N23 113.9(5) . . ?
N20 C30 H02C 108.8 . . ?
N23 C30 H02C 108.8 . . ?
N20 C30 H02D 108.8 . . ?
N23 C30 H02D 108.8 . . ?
H02C C30 H02D 107.7 . . ?
N4 C40 N13 115.3(5) . . ?
N4 C40 C39 103.3(4) . . ?
N13 C40 C39 102.8(4) . . ?
N4 C40 H40 111.6 . . ?
N13 C40 H40 111.6 . . ?
C39 C40 H40 111.6 . . ?
O8 C41 N14 125.9(5) . . ?
O8 C41 N13 126.3(5) . . ?
N14 C41 N13 107.8(5) . . ?
N13 C43 N12 113.1(5) . . ?
N13 C43 H02M 109.0 . . ?
N12 C43 H02M 109.0 . . ?
N13 C43 H02N 109.0 . . ?
N12 C43 H02N 109.0 . . ?
H02M C43 H02N 107.8 . . ?
O13 C42 N4 126.0(6) . . ?
O13 C42 N3 126.1(5) . . ?
N4 C42 N3 107.9(5) . . ?
N4 C44 N5 114.8(5) . . ?
N4 C44 H02E 108.6 . . ?
N5 C44 H02E 108.6 . . ?
N4 C44 H02F 108.6 . . ?
N5 C44 H02F 108.6 . . ?
H02E C44 H02F 107.6 . . ?
N12 C46 N5 114.7(5) . . ?
N12 C46 C47 102.9(4) . . ?
N5 C46 C47 103.1(4) . . ?
N12 C46 H01G 111.8 . . ?
N5 C46 H01G 111.8 . . ?
C47 C46 H01G 111.8 . . ?
O9 C45 N12 126.7(5) . . ?
O9 C45 N11 124.9(5) . . ?
N12 C45 N11 108.4(5) . . ?
N6 C47 N11 114.7(5) . . ?
N6 C47 C46 103.3(5) . . ?
N11 C47 C46 103.4(4) . . ?
N6 C47 H47 111.6 . . ?
N11 C47 H47 111.6 . . ?
C46 C47 H47 111.6 . . ?
O12 C48 N5 126.2(6) . . ?
O12 C48 N6 125.9(6) . . ?
N5 C48 N6 107.9(5) . . ?
O10 C51 N10 126.0(5) . . ?
O10 C51 N9 125.7(6) . . ?
N10 C51 N9 108.2(5) . . ?
N6 C50 N7 113.5(5) . . ?
N6 C50 H02R 108.9 . . ?
N7 C50 H02R 108.9 . . ?
N6 C50 H02S 108.9 . . ?
N7 C50 H02S 108.9 . . ?
H02R C50 H02S 107.7 . . ?
N11 C49 N10 114.2(5) . . ?
N11 C49 H01R 108.7 . . ?
N10 C49 H01R 108.7 . . ?
N11 C49 H01S 108.7 . . ?
N10 C49 H01S 108.7 . . ?
H01R C49 H01S 107.6 . . ?
N10 C52 N7 115.9(5) . . ?
N10 C52 C53 103.4(5) . . ?
N7 C52 C53 103.0(4) . . ?
N10 C52 H01E 111.3 . . ?
N7 C52 H01E 111.3 . . ?
C53 C52 H01E 111.3 . . ?
O11 C54 N7 126.5(6) . . ?
O11 C54 N8 125.6(6) . . ?
N7 C54 N8 108.0(5) . . ?
N8 C53 N9 115.3(5) . . ?
N8 C53 C52 103.1(5) . . ?
N9 C53 C52 102.8(5) . . ?
N8 C53 H53 111.7 . . ?
N9 C53 H53 111.7 . . ?
C52 C53 H53 111.7 . . ?
N3 C55 N9 113.9(5) 2_767 . ?
N3 C55 H02H 123.0 2_767 . ?
N9 C55 H02H 123.0 . . ?
N21 C29 N18 112.8(5) . . ?
N21 C29 H01A 109.0 . . ?
N18 C29 H01A 109.0 . . ?
N21 C29 H01B 109.0 . . ?
N18 C29 H01B 109.0 . . ?
H01A C29 H01B 107.8 . . ?
O15 C24 N18 126.1(5) . . ?
O15 C24 N17 125.5(5) . . ?
N18 C24 N17 108.3(5) . . ?
C34 N24 C37 122.3(5) . . ?
C34 N24 C33 112.8(5) . . ?
C37 N24 C33 124.7(5) . . ?
N20 C26 N18 114.9(5) . . ?
N20 C26 C25 103.3(5) . . ?
N18 C26 C25 102.4(4) . . ?
N20 C26 H26 111.8 . . ?
N18 C26 H26 111.8 . . ?
C25 C26 H26 111.8 . . ?
C36 N26 C27 121.0(5) . 2_556 ?
C36 N26 C22 111.0(5) . 2_556 ?
C27 N26 C22 122.8(5) 2_556 2_556 ?
N17 C25 N19 114.8(5) . . ?
N17 C25 C26 103.8(4) . . ?
N19 C25 C26 102.9(4) . . ?
N17 C25 H25 111.6 . . ?
N19 C25 H25 111.6 . . ?
C26 C25 H25 111.6 . . ?
C36 N25 C35 123.0(5) . . ?
C36 N25 C21 112.9(5) . 2_556 ?
C35 N25 C21 124.1(5) . 2_556 ?
O18 C28 N19 126.0(6) . . ?
O18 C28 N20 125.5(6) . . ?
N19 C28 N20 108.5(5) . . ?
N19 C27 N26 113.5(5) . 2_556 ?
N19 C27 H01P 108.9 . . ?
N26 C27 H01P 108.9 2_556 . ?
N19 C27 H01Q 108.9 . . ?
N26 C27 H01Q 108.9 2_556 . ?
H01P C27 H01Q 107.7 . . ?
N16 C23 N17 113.0(5) . . ?
N16 C23 H02T 123.5 . . ?
N17 C23 H02T 123.5 . . ?
C34 N23 C32 112.2(5) . . ?
C34 N23 C30 122.6(5) . . ?
C32 N23 C30 124.3(5) . . ?
N16 C22 N26 115.4(5) . 2_556 ?
N16 C22 C21 103.1(5) . . ?
N26 C22 C21 103.4(4) 2_556 . ?
N16 C22 H22 111.4 . . ?
N26 C22 H22 111.4 2_556 . ?
C21 C22 H22 111.4 . . ?
C31 N22 C33 112.7(5) . . ?
C31 N22 C35 122.2(5) . . ?
C33 N22 C35 123.3(5) . . ?
O14 C20 N16 126.4(5) . . ?
O14 C20 N15 125.7(6) . . ?
N16 C20 N15 107.9(5) . . ?
C28 N20 C26 112.4(5) . . ?
C28 N20 C30 123.7(5) . . ?
C26 N20 C30 123.2(5) . . ?
N25 C21 N15 115.6(5) 2_556 . ?
N25 C21 C22 103.1(5) 2_556 . ?
N15 C21 C22 103.5(5) . . ?
N25 C21 H02G 111.3 2_556 . ?
N15 C21 H02G 111.3 . . ?
C22 C21 H02G 111.3 . . ?
C31 N21 C29 123.1(5) . . ?
C31 N21 C32 111.9(5) . . ?
C29 N21 C32 123.6(5) . . ?

_refine_diff_density_max         7.798
_refine_diff_density_min         -3.108
_refine_diff_density_rms         0.193

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_6-IMS-170K
_database_code_depnum_ccdc_archive 'CCDC 1534042'
_audit_update_record             
;
2017-02-22 deposited with the CCDC.
2017-05-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C108 H112 Br2 N52 O34 U'
_chemical_formula_weight         3080.34

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'
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'
Br Br -0.2901 2.4595 '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                   12.6946(10)
_cell_length_b                   14.7727(11)
_cell_length_c                   17.0721(12)
_cell_angle_alpha                90.387(3)
_cell_angle_beta                 98.122(4)
_cell_angle_gamma                94.716(4)
_cell_volume                     3158.2(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    9978
_cell_measurement_theta_min      3.00
_cell_measurement_theta_max      27.69

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_F_000             1558
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    2.018
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            56722
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.998
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             14362
_reflns_number_gt                12235
_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       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0791P)²+42.3265P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0075(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         14362
_refine_ls_number_parameters     918
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.1163
_refine_ls_R_factor_gt           0.0973
_refine_ls_wR_factor_ref         0.2472
_refine_ls_wR_factor_gt          0.2330
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.116
_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 0.5000 1.0000 0.5000 0.03407(17) Uani 1 2 d S . P . .
Br1 Br 0.5443(3) 0.6139(3) 0.8790(2) 0.214(2) Uani 1 1 d . . . . .
N9 N 0.1347(5) 0.7133(4) 1.0305(4) 0.0268(13) Uani 1 1 d . . . . .
O7 O 0.2284(19) 0.9652(16) 0.5212(14) 0.113(8) Uani 0.588(18) 1 d . U P A 1
N5 N -0.2768(5) 0.8994(4) 0.7974(4) 0.0274(13) Uani 1 1 d . . . . .
N14 N -0.3394(5) 1.1296(4) 1.0149(4) 0.0276(13) Uani 1 1 d . . . . .
N16 N 0.6981(5) 0.5684(4) 0.3234(4) 0.0279(13) Uani 1 1 d . . . . .
N8 N 0.1977(5) 0.7691(4) 0.9097(4) 0.0271(13) Uani 1 1 d . . . . .
N15 N 0.6335(5) 0.4527(4) 0.3884(4) 0.0254(12) Uani 1 1 d . . . . .
N7 N 0.0266(5) 0.7622(4) 0.8562(4) 0.0245(12) Uani 1 1 d . . . . .
N24 N 0.9161(5) 0.5896(5) 0.2310(4) 0.0305(14) Uani 1 1 d . . . . .
N10 N -0.0307(5) 0.6820(4) 0.9702(4) 0.0267(13) Uani 1 1 d . . . . .
N6 N -0.1507(5) 0.8042(5) 0.8063(4) 0.0284(13) Uani 1 1 d . . . . .
N13 N -0.3794(5) 0.9932(4) 0.9586(4) 0.0297(14) Uani 1 1 d . . . . .
N12 N -0.3182(5) 0.8488(4) 0.9259(4) 0.0285(13) Uani 1 1 d . . . . .
N4 N -0.3207(5) 1.0478(4) 0.8358(4) 0.0269(13) Uani 1 1 d . . . . .
N26 N 0.7450(5) 0.3581(4) 0.3196(4) 0.0287(13) Uani 1 1 d . . . . .
N23 N 1.0717(6) 0.6552(5) 0.2858(4) 0.0335(15) Uani 1 1 d . . . . .
N25 N 0.7786(5) 0.4685(5) 0.2365(4) 0.0292(13) Uani 1 1 d . . . . .
N17 N 0.8280(5) 0.6926(5) 0.3076(4) 0.0311(14) Uani 1 1 d . . . . .
O4 O 0.3717(14) 1.0919(13) 0.5680(9) 0.038(4) Uani 0.412(18) 1 d . U P A 2
N3 N -0.2688(5) 1.1804(4) 0.8954(4) 0.0272(13) Uani 1 1 d . . . . .
N20 N 1.2228(6) 0.7384(4) 0.5684(4) 0.0335(15) Uani 1 1 d . . . . .
N11 N -0.2006(5) 0.7453(4) 0.9301(4) 0.0270(13) Uani 1 1 d . . . . .
C33 C -0.3538(5) 1.0391(5) 1.0298(5) 0.0278(16) Uani 1 1 d . . . . .
N18 N 0.9821(6) 0.7695(5) 0.3520(5) 0.0400(17) Uani 1 1 d . . . . .
N19 N 1.1351(7) 0.7825(5) 0.4548(5) 0.045(2) Uani 1 1 d . . . . .
C45 C 0.6831(6) 0.4939(5) 0.2649(4) 0.0256(14) Uani 1 1 d . . . . .
H45 H 0.6254 0.5041 0.2203 0.031 Uiso 1 1 calc R U . . .
C17 C 0.0691(6) 1.0857(5) 0.8434(4) 0.0249(15) Uani 1 1 d . . . . .
H17A H -0.0056 1.0899 0.8183 0.030 Uiso 1 1 calc R U . . .
H17B H 0.0949 1.1451 0.8692 0.030 Uiso 1 1 calc R U . . .
C44 C 0.6580(6) 0.5445(5) 0.3904(5) 0.0284(16) Uani 1 1 d . . . . .
C41 C 1.0243(6) 0.5784(5) 0.2474(4) 0.0289(16) Uani 1 1 d . . . . .
C18 C 0.0703(6) 1.0142(5) 0.9057(4) 0.0258(15) Uani 1 1 d . . . . .
H18A H 0.1447 1.0092 0.9309 0.031 Uiso 1 1 calc R U . . .
H18B H 0.0429 0.9547 0.8805 0.031 Uiso 1 1 calc R U . . .
C22 C -0.3314(6) 0.9791(5) 0.7740(5) 0.0285(15) Uani 1 1 d . . . . .
H22A H -0.3028 1.0056 0.7274 0.034 Uiso 1 1 calc R U . . .
H22B H -0.4082 0.9606 0.7578 0.034 Uiso 1 1 calc R U . . .
C25 C 0.1273(6) 0.8025(5) 0.8511(4) 0.0255(15) Uani 1 1 d . . . . .
C31 C -0.3941(6) 1.0535(5) 0.8924(5) 0.0285(16) Uani 1 1 d . . . . .
H31 H -0.4699 1.0486 0.8660 0.034 Uiso 1 1 calc R U . . .
C28 C 0.0326(6) 0.6829(5) 0.9063(4) 0.0253(14) Uani 1 1 d . . . . .
H28 H 0.0187 0.6251 0.8743 0.030 Uiso 1 1 calc R U . . .
C23 C -0.1802(6) 0.8846(5) 0.7759(4) 0.0266(15) Uani 1 1 d . . . . .
N2 N 0.8178(8) 0.6757(5) 0.6210(5) 0.054(3) Uani 1 1 d . . . . .
C46 C 0.6523(6) 0.4115(5) 0.3148(5) 0.0276(15) Uani 1 1 d . . . . .
H46 H 0.5864 0.3759 0.2882 0.033 Uiso 1 1 calc R U . . .
C19 C 0.0028(6) 1.0363(5) 0.9683(4) 0.0265(15) Uani 1 1 d . . . . .
H19A H -0.0705 1.0443 0.9423 0.032 Uiso 1 1 calc R U . . .
H19B H 0.0323 1.0948 0.9945 0.032 Uiso 1 1 calc R U . . .
C14 C 0.0916(8) 1.0154(5) 0.7186(5) 0.0343(18) Uani 1 1 d . . . . .
H14 H 0.0202 0.9893 0.7165 0.041 Uiso 1 1 calc R U . . .
C32 C -0.3612(6) 1.1487(5) 0.9316(4) 0.0259(15) Uani 1 1 d . . . . .
H32 H -0.4198 1.1902 0.9205 0.031 Uiso 1 1 calc R U . . .
C40 C 0.8929(6) 0.6803(5) 0.2453(4) 0.0287(16) Uani 1 1 d . . . . .
H40 H 0.8622 0.7089 0.1951 0.034 Uiso 1 1 calc R U . . .
C20 C -0.2213(6) 1.2736(5) 0.9041(5) 0.0288(16) Uani 1 1 d . . . . .
H20A H -0.1939 1.2915 0.8545 0.035 Uiso 1 1 calc R U . . .
H20B H -0.2773 1.3141 0.9123 0.035 Uiso 1 1 calc R U . . .
C30 C -0.3180(6) 0.8263(5) 0.8433(4) 0.0252(14) Uani 1 1 d . . . . .
H30 H -0.3893 0.7989 0.8178 0.030 Uiso 1 1 calc R U . . .
C39 C 1.0022(7) 0.7289(5) 0.2789(5) 0.0321(17) Uani 1 1 d . . . . .
H39 H 1.0258 0.7762 0.2419 0.039 Uiso 1 1 calc R U . . .
C27 C 0.1502(6) 0.6947(5) 0.9501(4) 0.0240(14) Uani 1 1 d . . . . .
H27 H 0.1878 0.6383 0.9460 0.029 Uiso 1 1 calc R U . . .
C36 C -0.1458(6) 0.6672(5) 0.9603(5) 0.0290(16) Uani 1 1 d . . . . .
H36A H -0.1682 0.6509 1.0120 0.035 Uiso 1 1 calc R U . . .
H36B H -0.1686 0.6149 0.9235 0.035 Uiso 1 1 calc R U . . .
C47 C 0.8135(6) 0.3901(5) 0.2689(4) 0.0266(15) Uani 1 1 d . . . . .
C2 C 0.6485(8) 0.7748(6) 0.6263(5) 0.043(2) Uani 1 1 d . . . . .
C43 C 0.8399(6) 0.5224(6) 0.1869(4) 0.0309(16) Uani 1 1 d . . . . .
H43A H 0.7907 0.5539 0.1481 0.037 Uiso 1 1 calc R U . . .
H43B H 0.8789 0.4819 0.1570 0.037 Uiso 1 1 calc R U . . .
C3 C 0.7317(8) 0.8076(6) 0.5876(5) 0.043(2) Uani 1 1 d . . . . .
H3 H 0.7300 0.8645 0.5622 0.051 Uiso 1 1 calc R U . . .
C37 C 0.0299(6) 0.7030(5) 1.0417(4) 0.0260(15) Uani 1 1 d . . . . .
C26 C 0.3100(6) 0.8015(5) 0.9227(5) 0.0306(16) Uani 1 1 d . . . . .
H26A H 0.3295 0.8268 0.8726 0.037 Uiso 1 1 calc R U . . .
H26B H 0.3525 0.7490 0.9358 0.037 Uiso 1 1 calc R U . . .
C34 C -0.4024(6) 0.8963(5) 0.9527(5) 0.0312(16) Uani 1 1 d . . . . .
H34A H -0.4691 0.8823 0.9154 0.037 Uiso 1 1 calc R U . . .
H34B H -0.4150 0.8733 1.0051 0.037 Uiso 1 1 calc R U . . .
C35 C -0.2597(6) 0.7918(5) 0.9749(5) 0.0279(15) Uani 1 1 d . . . . .
C24 C -0.0576(6) 0.7627(6) 0.7892(4) 0.0298(16) Uani 1 1 d . . . . .
H24A H -0.0290 0.7955 0.7454 0.036 Uiso 1 1 calc R U . . .
H24B H -0.0791 0.6992 0.7709 0.036 Uiso 1 1 calc R U . . .
C29 C -0.2316(6) 0.7576(5) 0.8473(5) 0.0272(15) Uani 1 1 d . . . . .
H29 H -0.2608 0.6989 0.8199 0.033 Uiso 1 1 calc R U . . .
C54 C 1.2346(7) 0.7581(5) 0.4327(5) 0.0364(19) Uani 1 1 d . . . . .
H54 H 1.2728 0.8103 0.4086 0.044 Uiso 1 1 calc R U . . .
C55 C 1.2985(7) 0.7317(5) 0.5134(5) 0.0310(17) Uani 1 1 d . . . . .
H55 H 1.3640 0.7739 0.5286 0.037 Uiso 1 1 calc R U . . .
C21 C -0.2506(6) 1.1236(5) 0.8364(4) 0.0230(14) Uani 1 1 d . . . . .
C15 C 0.2377(7) 1.1047(6) 0.7858(5) 0.0362(19) Uani 1 1 d . . . . .
H15 H 0.2689 1.1407 0.8307 0.043 Uiso 1 1 calc R U . . .
C42 C 0.7161(7) 0.6621(5) 0.3024(5) 0.0338(17) Uani 1 1 d . . . . .
H42A H 0.6825 0.7005 0.3379 0.041 Uiso 1 1 calc R U . . .
H42B H 0.6809 0.6701 0.2476 0.041 Uiso 1 1 calc R U . . .
C38 C 0.8783(7) 0.7492(5) 0.3671(5) 0.0339(18) Uani 1 1 d . . . . .
C4 C 0.8161(9) 0.7570(6) 0.5867(6) 0.048(2) Uani 1 1 d . . . . .
H4 H 0.8747 0.7795 0.5614 0.058 Uiso 1 1 calc R U . . .
C52 C 1.1316(8) 0.7754(6) 0.5354(6) 0.042(2) Uani 1 1 d . . . . .
C1 C 0.5546(8) 0.8261(7) 0.6304(6) 0.050(3) Uani 1 1 d . . . . .
C10 C 0.3433(19) 1.0287(13) 0.6119(12) 0.025(4) Uani 0.412(18) 1 d . U P A 2
C50 C 1.0585(9) 0.8291(5) 0.4028(7) 0.050(3) Uani 1 1 d . . . . .
H50A H 1.0194 0.8666 0.4354 0.060 Uiso 1 1 calc R U . . .
H50B H 1.0974 0.8707 0.3695 0.060 Uiso 1 1 calc R U . . .
C16 C 0.2959(9) 1.0893(9) 0.7256(7) 0.062(4) Uani 1 1 d . . . . .
H16 H 0.3673 1.1154 0.7284 0.075 Uiso 1 1 calc R U . . .
C12 C 0.2503(12) 1.0359(7) 0.6611(7) 0.064(4) Uani 1 1 d . . . . .
C6 C 0.6535(9) 0.6932(6) 0.6636(5) 0.048(3) Uani 1 1 d . . . . .
H6 H 0.5982 0.6716 0.6926 0.058 Uiso 1 1 calc R U . . .
C7 C 0.9065(10) 0.6207(8) 0.6147(8) 0.067(3) Uani 1 1 d . . . . .
H7A H 0.9072 0.5728 0.6550 0.081 Uiso 1 1 calc R U . . .
H7B H 0.9744 0.6596 0.6262 0.081 Uiso 1 1 calc R U . . .
C13 C 0.1477(12) 0.9984(6) 0.6589(6) 0.059(3) Uani 1 1 d . . . . .
H13 H 0.1156 0.9605 0.6154 0.071 Uiso 1 1 calc R U . . .
C8 C 0.8998(9) 0.5771(7) 0.5345(7) 0.056(3) Uani 1 1 d . . . . .
H8A H 0.9031 0.6239 0.4935 0.067 Uiso 1 1 calc R U . . .
H8B H 0.8323 0.5381 0.5217 0.067 Uiso 1 1 calc R U . . .
C5 C 0.7375(11) 0.6434(7) 0.6593(6) 0.057(3) Uani 1 1 d . . . . .
H5 H 0.7396 0.5856 0.6834 0.069 Uiso 1 1 calc R U . . .
C9 C 0.9960(10) 0.5202(9) 0.5388(7) 0.064(3) Uani 1 1 d . . . . .
H9A H 1.0622 0.5591 0.5574 0.076 Uiso 1 1 calc R U . . .
H9B H 0.9890 0.4713 0.5775 0.076 Uiso 1 1 calc R U . . .
O5 O 0.3657(15) 0.9502(11) 0.6029(11) 0.052(5) Uani 0.412(18) 1 d . U P A 2
N22 N 1.2291(5) 0.6765(4) 0.3850(4) 0.0293(14) Uani 1 1 d . . . . .
C53 C 1.1875(7) 0.6714(6) 0.3019(5) 0.0343(18) Uani 1 1 d . . . . .
H53A H 1.2198 0.6219 0.2768 0.041 Uiso 1 1 calc R U . . .
H53B H 1.2095 0.7290 0.2771 0.041 Uiso 1 1 calc R U . . .
N21 N 1.3249(5) 0.6409(4) 0.4972(4) 0.0289(14) Uani 1 1 d . . . . .
C56 C 1.2911(6) 0.6125(5) 0.4204(4) 0.0260(15) Uani 1 1 d . . . . .
C48 C 0.5944(6) 0.4043(5) 0.4525(4) 0.0276(15) Uani 1 1 d . . . . .
H48A H 0.5365 0.3584 0.4303 0.033 Uiso 1 1 calc R U . . .
H48B H 0.5632 0.4476 0.4854 0.033 Uiso 1 1 calc R U . . .
C49 C 0.7460(7) 0.2665(5) 0.3468(5) 0.0371(19) Uani 1 1 d . . . . .
H49A H 0.7962 0.2344 0.3195 0.044 Uiso 1 1 calc R U . . .
H49B H 0.6739 0.2350 0.3325 0.044 Uiso 1 1 calc R U . . .
N1 N 0.1355(5) 1.0682(4) 0.7806(3) 0.0234(12) Uani 1 1 d . . . . .
C11 C 0.2884(18) 1.0052(12) 0.5814(13) 0.051(5) Uani 0.588(18) 1 d . U P A 1
O3 O 0.4985(6) 0.8138(6) 0.6831(4) 0.061(2) Uani 1 1 d . . . . .
O6 O 0.3827(11) 1.0428(11) 0.5807(9) 0.054(4) Uani 0.588(18) 1 d . U P A 1
O1 O 0.5994(8) 1.0575(7) 0.5669(6) 0.079(3) Uani 1 1 d . U . . .
O2 O 0.5320(9) 0.8752(7) 0.5704(7) 0.094(3) Uani 1 1 d . U . . .
O19 O -0.1850(4) 1.1382(4) 0.7921(3) 0.0300(11) Uani 1 1 d . . . . .
O17 O 0.1490(5) 0.8583(4) 0.8026(3) 0.0305(12) Uani 1 1 d . . . . .
O10 O 1.3136(5) 0.5439(4) 0.3889(3) 0.0323(12) Uani 1 1 d . . . . .
O11 O 0.6441(5) 0.5961(4) 0.4442(3) 0.0346(12) Uani 1 1 d . . . . .
O14 O -0.3491(4) 1.0041(4) 1.0945(3) 0.0308(12) Uani 1 1 d . . . . .
O15 O -0.2596(5) 0.7851(4) 1.0461(3) 0.0365(13) Uani 1 1 d . . . . .
O8 O 0.8918(5) 0.3546(4) 0.2531(4) 0.0357(13) Uani 1 1 d . . . . .
O18 O -0.1314(5) 0.9339(4) 0.7341(3) 0.0339(12) Uani 1 1 d . . . . .
O16 O -0.0038(5) 0.7088(4) 1.1048(3) 0.0327(12) Uani 1 1 d . . . . .
O9 O 1.0681(5) 0.5122(4) 0.2308(4) 0.0387(14) Uani 1 1 d . . . . .
O12 O 0.8407(6) 0.7795(4) 0.4221(4) 0.0439(16) Uani 1 1 d . . . . .
O13 O 1.0615(6) 0.7991(5) 0.5692(5) 0.061(2) 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 O1 1.739(10) . ?
U1 O1 1.739(10) 2_676 ?
U1 O2 2.241(8) . ?
U1 O2 2.241(9) 2_676 ?
U1 O6 2.289(13) . ?
U1 O6 2.289(14) 2_676 ?
U1 O4 2.593(17) . ?
U1 O4 2.593(17) 2_676 ?
U1 O5 2.681(15) . ?
U1 O5 2.682(15) 2_676 ?
U1 C10 3.00(2) 2_676 ?
U1 C10 3.00(2) . ?
N9 C37 1.367(10) . ?
N9 C27 1.441(9) . ?
N9 C20 1.452(10) 2_577 ?
O7 C11 1.30(3) . ?
N5 C23 1.362(10) . ?
N5 C22 1.445(10) . ?
N5 C30 1.446(9) . ?
N14 C33 1.366(10) . ?
N14 C32 1.443(9) . ?
N14 C26 1.457(11) 2_577 ?
N16 C44 1.354(10) . ?
N16 C42 1.439(10) . ?
N16 C45 1.464(10) . ?
N8 C25 1.367(9) . ?
N8 C27 1.438(9) . ?
N8 C26 1.451(10) . ?
N15 C44 1.365(10) . ?
N15 C48 1.436(9) . ?
N15 C46 1.451(10) . ?
N7 C25 1.379(10) . ?
N7 C24 1.452(9) . ?
N7 C28 1.457(9) . ?
N24 C41 1.386(10) . ?
N24 C40 1.423(10) . ?
N24 C43 1.454(10) . ?
N10 C37 1.366(10) . ?
N10 C28 1.443(9) . ?
N10 C36 1.446(10) . ?
N6 C23 1.360(10) . ?
N6 C24 1.439(10) . ?
N6 C29 1.453(10) . ?
N13 C33 1.372(11) . ?
N13 C34 1.437(10) . ?
N13 C31 1.445(10) . ?
N12 C35 1.377(10) . ?
N12 C30 1.447(10) . ?
N12 C34 1.449(10) . ?
N4 C21 1.371(9) . ?
N4 C31 1.441(10) . ?
N4 C22 1.444(10) . ?
N26 C47 1.371(10) . ?
N26 C49 1.434(10) . ?
N26 C46 1.462(9) . ?
N23 C41 1.359(10) . ?
N23 C39 1.452(10) . ?
N23 C53 1.456(10) . ?
N25 C47 1.366(10) . ?
N25 C43 1.431(10) . ?
N25 C45 1.444(10) . ?
N17 C38 1.363(11) . ?
N17 C42 1.445(10) . ?
N17 C40 1.454(11) . ?
O4 C10 1.26(3) . ?
N3 C21 1.363(10) . ?
N3 C32 1.448(9) . ?
N3 C20 1.456(10) . ?
N20 C52 1.371(11) . ?
N20 C55 1.443(11) . ?
N20 C49 1.450(11) 2_766 ?
N11 C35 1.364(10) . ?
N11 C29 1.429(10) . ?
N11 C36 1.456(9) . ?
C33 O14 1.218(9) . ?
N18 C38 1.387(12) . ?
N18 C50 1.442(11) . ?
N18 C39 1.446(12) . ?
N19 C52 1.389(13) . ?
N19 C54 1.441(13) . ?
N19 C50 1.443(10) . ?
C45 C46 1.546(11) . ?
C45 H45 1.0000 . ?
C17 N1 1.488(8) . ?
C17 C18 1.504(9) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C44 O11 1.231(10) . ?
C41 O9 1.214(10) . ?
C18 C19 1.511(9) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C25 O17 1.216(9) . ?
C31 C32 1.553(11) . ?
C31 H31 1.0000 . ?
C28 C27 1.568(10) . ?
C28 H28 1.0000 . ?
C23 O18 1.216(9) . ?
N2 C4 1.340(12) . ?
N2 C5 1.346(16) . ?
N2 C7 1.456(14) . ?
C46 H46 1.0000 . ?
C19 C19 1.533(13) 2_577 ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C14 N1 1.338(11) . ?
C14 C13 1.358(12) . ?
C14 H14 0.9500 . ?
C32 H32 1.0000 . ?
C40 C39 1.541(11) . ?
C40 H40 1.0000 . ?
C20 N9 1.452(10) 2_577 ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C30 C29 1.550(10) . ?
C30 H30 1.0000 . ?
C39 H39 1.0000 . ?
C27 H27 1.0000 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C47 O8 1.223(9) . ?
C2 C6 1.369(11) . ?
C2 C3 1.380(14) . ?
C2 C1 1.474(16) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C3 C4 1.357(14) . ?
C3 H3 0.9500 . ?
C37 O16 1.219(9) . ?
C26 N14 1.457(11) 2_577 ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 O15 1.221(10) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C29 H29 1.0000 . ?
C54 N22 1.441(11) . ?
C54 C55 1.565(11) . ?
C54 H54 1.0000 . ?
C55 N21 1.443(10) . ?
C55 H55 1.0000 . ?
C21 O19 1.210(9) . ?
C15 N1 1.353(11) . ?
C15 C16 1.376(13) . ?
C15 H15 0.9500 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C38 O12 1.210(11) . ?
C4 H4 0.9500 . ?
C52 O13 1.200(13) . ?
C1 O3 1.230(14) . ?
C1 O2 1.272(12) . ?
C10 O5 1.23(2) . ?
C10 C12 1.55(3) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C16 C12 1.380(19) . ?
C16 H16 0.9500 . ?
C12 C13 1.368(19) . ?
C12 C11 1.58(2) . ?
C6 C5 1.355(17) . ?
C6 H6 0.9500 . ?
C7 C8 1.497(18) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C13 H13 0.9500 . ?
C8 C9 1.533(16) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C5 H5 0.9500 . ?
C9 C9 1.47(2) 2_766 ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
N22 C56 1.370(10) . ?
N22 C53 1.441(10) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
N21 C56 1.372(10) . ?
N21 C48 1.451(9) 2_766 ?
C56 O10 1.217(9) . ?
C48 N21 1.451(9) 2_766 ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 N20 1.450(11) 2_766 ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C11 O6 1.28(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O1 180.0 . 2_676 ?
O1 U1 O2 86.9(5) . . ?
O1 U1 O2 93.1(5) 2_676 . ?
O1 U1 O2 93.1(5) . 2_676 ?
O1 U1 O2 86.9(5) 2_676 2_676 ?
O2 U1 O2 180.0(6) . 2_676 ?
O1 U1 O6 86.3(5) . . ?
O1 U1 O6 93.7(5) 2_676 . ?
O2 U1 O6 92.0(5) . . ?
O2 U1 O6 88.0(5) 2_676 . ?
O1 U1 O6 93.7(5) . 2_676 ?
O1 U1 O6 86.3(5) 2_676 2_676 ?
O2 U1 O6 88.0(5) . 2_676 ?
O2 U1 O6 92.0(5) 2_676 2_676 ?
O6 U1 O6 180.0(8) . 2_676 ?
O1 U1 O4 84.4(5) . . ?
O1 U1 O4 95.6(5) 2_676 . ?
O2 U1 O4 108.5(5) . . ?
O2 U1 O4 71.5(5) 2_676 . ?
O1 U1 O4 95.6(5) . 2_676 ?
O1 U1 O4 84.4(5) 2_676 2_676 ?
O2 U1 O4 71.5(5) . 2_676 ?
O2 U1 O4 108.5(5) 2_676 2_676 ?
O4 U1 O4 180.0 . 2_676 ?
O1 U1 O5 97.6(6) . . ?
O1 U1 O5 82.4(6) 2_676 . ?
O2 U1 O5 62.7(5) . . ?
O2 U1 O5 117.3(5) 2_676 . ?
O4 U1 O5 48.8(5) . . ?
O4 U1 O5 131.2(5) 2_676 . ?
O1 U1 O5 82.4(6) . 2_676 ?
O1 U1 O5 97.6(6) 2_676 2_676 ?
O2 U1 O5 117.3(5) . 2_676 ?
O2 U1 O5 62.7(5) 2_676 2_676 ?
O4 U1 O5 131.2(5) . 2_676 ?
O4 U1 O5 48.8(5) 2_676 2_676 ?
O5 U1 O5 180.0 . 2_676 ?
O1 U1 C10 91.0(6) . 2_676 ?
O1 U1 C10 89.0(6) 2_676 2_676 ?
O2 U1 C10 95.4(4) . 2_676 ?
O2 U1 C10 84.6(4) 2_676 2_676 ?
O4 U1 C10 155.2(5) . 2_676 ?
O4 U1 C10 24.8(5) 2_676 2_676 ?
O5 U1 C10 155.8(5) . 2_676 ?
O5 U1 C10 24.2(5) 2_676 2_676 ?
O1 U1 C10 89.0(6) . . ?
O1 U1 C10 91.0(6) 2_676 . ?
O2 U1 C10 84.6(4) . . ?
O2 U1 C10 95.4(4) 2_676 . ?
O4 U1 C10 24.8(5) . . ?
O4 U1 C10 155.2(5) 2_676 . ?
O5 U1 C10 24.2(5) . . ?
O5 U1 C10 155.8(5) 2_676 . ?
C10 U1 C10 180.0 2_676 . ?
C37 N9 C27 113.2(6) . . ?
C37 N9 C20 122.3(6) . 2_577 ?
C27 N9 C20 123.7(6) . 2_577 ?
C23 N5 C22 122.5(6) . . ?
C23 N5 C30 112.7(6) . . ?
C22 N5 C30 124.8(6) . . ?
C33 N14 C32 112.6(7) . . ?
C33 N14 C26 122.8(6) . 2_577 ?
C32 N14 C26 124.6(6) . 2_577 ?
C44 N16 C42 121.7(7) . . ?
C44 N16 C45 112.0(6) . . ?
C42 N16 C45 122.6(6) . . ?
C25 N8 C27 112.7(6) . . ?
C25 N8 C26 121.9(6) . . ?
C27 N8 C26 125.1(6) . . ?
C44 N15 C48 123.0(7) . . ?
C44 N15 C46 111.9(6) . . ?
C48 N15 C46 125.1(6) . . ?
C25 N7 C24 120.5(6) . . ?
C25 N7 C28 110.8(6) . . ?
C24 N7 C28 119.4(6) . . ?
C41 N24 C40 112.4(6) . . ?
C41 N24 C43 122.8(7) . . ?
C40 N24 C43 123.2(6) . . ?
C37 N10 C28 112.3(6) . . ?
C37 N10 C36 123.0(6) . . ?
C28 N10 C36 124.6(6) . . ?
C23 N6 C24 123.6(7) . . ?
C23 N6 C29 112.7(6) . . ?
C24 N6 C29 123.0(6) . . ?
C33 N13 C34 122.7(7) . . ?
C33 N13 C31 112.6(6) . . ?
C34 N13 C31 124.2(7) . . ?
C35 N12 C30 111.6(6) . . ?
C35 N12 C34 121.6(7) . . ?
C30 N12 C34 122.1(6) . . ?
C21 N4 C31 113.0(6) . . ?
C21 N4 C22 121.8(6) . . ?
C31 N4 C22 124.2(6) . . ?
C47 N26 C49 120.5(7) . . ?
C47 N26 C46 111.0(6) . . ?
C49 N26 C46 124.2(7) . . ?
C41 N23 C39 112.1(6) . . ?
C41 N23 C53 121.2(7) . . ?
C39 N23 C53 122.2(7) . . ?
C47 N25 C43 121.4(7) . . ?
C47 N25 C45 112.9(6) . . ?
C43 N25 C45 125.4(6) . . ?
C38 N17 C42 121.8(7) . . ?
C38 N17 C40 112.8(7) . . ?
C42 N17 C40 124.5(7) . . ?
C10 O4 U1 95.9(14) . . ?
C21 N3 C32 112.7(6) . . ?
C21 N3 C20 122.2(6) . . ?
C32 N3 C20 122.6(6) . . ?
C52 N20 C55 112.8(7) . . ?
C52 N20 C49 122.7(8) . 2_766 ?
C55 N20 C49 121.9(7) . 2_766 ?
C35 N11 C29 112.0(6) . . ?
C35 N11 C36 121.8(7) . . ?
C29 N11 C36 122.1(6) . . ?
O14 C33 N14 126.9(8) . . ?
O14 C33 N13 125.1(7) . . ?
N14 C33 N13 108.0(7) . . ?
C38 N18 C50 122.4(9) . . ?
C38 N18 C39 112.9(7) . . ?
C50 N18 C39 124.6(9) . . ?
C52 N19 C54 112.7(7) . . ?
C52 N19 C50 122.6(9) . . ?
C54 N19 C50 123.2(9) . . ?
N25 C45 N16 115.9(6) . . ?
N25 C45 C46 102.8(6) . . ?
N16 C45 C46 102.1(6) . . ?
N25 C45 H45 111.8 . . ?
N16 C45 H45 111.8 . . ?
C46 C45 H45 111.8 . . ?
N1 C17 C18 114.1(6) . . ?
N1 C17 H17A 108.7 . . ?
C18 C17 H17A 108.7 . . ?
N1 C17 H17B 108.7 . . ?
C18 C17 H17B 108.7 . . ?
H17A C17 H17B 107.6 . . ?
O11 C44 N16 126.4(7) . . ?
O11 C44 N15 124.9(7) . . ?
N16 C44 N15 108.7(7) . . ?
O9 C41 N23 126.6(8) . . ?
O9 C41 N24 126.4(7) . . ?
N23 C41 N24 107.0(7) . . ?
C17 C18 C19 111.6(6) . . ?
C17 C18 H18A 109.3 . . ?
C19 C18 H18A 109.3 . . ?
C17 C18 H18B 109.3 . . ?
C19 C18 H18B 109.3 . . ?
H18A C18 H18B 108.0 . . ?
N4 C22 N5 113.4(6) . . ?
N4 C22 H22A 108.9 . . ?
N5 C22 H22A 108.9 . . ?
N4 C22 H22B 108.9 . . ?
N5 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
O17 C25 N8 126.2(7) . . ?
O17 C25 N7 125.3(7) . . ?
N8 C25 N7 108.4(6) . . ?
N4 C31 N13 115.7(6) . . ?
N4 C31 C32 103.0(6) . . ?
N13 C31 C32 102.9(6) . . ?
N4 C31 H31 111.5 . . ?
N13 C31 H31 111.5 . . ?
C32 C31 H31 111.5 . . ?
N10 C28 N7 115.5(6) . . ?
N10 C28 C27 103.3(6) . . ?
N7 C28 C27 102.9(6) . . ?
N10 C28 H28 111.5 . . ?
N7 C28 H28 111.5 . . ?
C27 C28 H28 111.5 . . ?
O18 C23 N6 126.4(7) . . ?
O18 C23 N5 125.3(7) . . ?
N6 C23 N5 108.3(6) . . ?
C4 N2 C5 120.9(10) . . ?
C4 N2 C7 119.4(11) . . ?
C5 N2 C7 119.7(10) . . ?
N15 C46 N26 116.0(6) . . ?
N15 C46 C45 103.5(6) . . ?
N26 C46 C45 103.6(6) . . ?
N15 C46 H46 111.1 . . ?
N26 C46 H46 111.1 . . ?
C45 C46 H46 111.1 . . ?
C18 C19 C19 113.9(7) . 2_577 ?
C18 C19 H19A 108.8 . . ?
C19 C19 H19A 108.8 2_577 . ?
C18 C19 H19B 108.8 . . ?
C19 C19 H19B 108.8 2_577 . ?
H19A C19 H19B 107.7 . . ?
N1 C14 C13 120.8(10) . . ?
N1 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
N14 C32 N3 115.1(6) . . ?
N14 C32 C31 103.6(6) . . ?
N3 C32 C31 103.1(6) . . ?
N14 C32 H32 111.5 . . ?
N3 C32 H32 111.5 . . ?
C31 C32 H32 111.5 . . ?
N24 C40 N17 115.9(6) . . ?
N24 C40 C39 103.9(6) . . ?
N17 C40 C39 103.5(6) . . ?
N24 C40 H40 111.0 . . ?
N17 C40 H40 111.0 . . ?
C39 C40 H40 111.0 . . ?
N9 C20 N3 113.2(6) 2_577 . ?
N9 C20 H20A 108.9 2_577 . ?
N3 C20 H20A 108.9 . . ?
N9 C20 H20B 108.9 2_577 . ?
N3 C20 H20B 108.9 . . ?
H20A C20 H20B 107.8 . . ?
N5 C30 N12 114.8(6) . . ?
N5 C30 C29 103.4(6) . . ?
N12 C30 C29 102.5(6) . . ?
N5 C30 H30 111.8 . . ?
N12 C30 H30 111.8 . . ?
C29 C30 H30 111.8 . . ?
N18 C39 N23 116.6(6) . . ?
N18 C39 C40 103.1(7) . . ?
N23 C39 C40 102.7(6) . . ?
N18 C39 H39 111.2 . . ?
N23 C39 H39 111.2 . . ?
C40 C39 H39 111.2 . . ?
N8 C27 N9 115.9(6) . . ?
N8 C27 C28 103.0(6) . . ?
N9 C27 C28 102.2(6) . . ?
N8 C27 H27 111.6 . . ?
N9 C27 H27 111.6 . . ?
C28 C27 H27 111.6 . . ?
N10 C36 N11 114.0(6) . . ?
N10 C36 H36A 108.8 . . ?
N11 C36 H36A 108.8 . . ?
N10 C36 H36B 108.8 . . ?
N11 C36 H36B 108.8 . . ?
H36A C36 H36B 107.7 . . ?
O8 C47 N25 124.7(7) . . ?
O8 C47 N26 126.7(7) . . ?
N25 C47 N26 108.6(6) . . ?
C6 C2 C3 119.6(10) . . ?
C6 C2 C1 118.5(10) . . ?
C3 C2 C1 121.9(8) . . ?
N25 C43 N24 113.0(6) . . ?
N25 C43 H43A 109.0 . . ?
N24 C43 H43A 109.0 . . ?
N25 C43 H43B 109.0 . . ?
N24 C43 H43B 109.0 . . ?
H43A C43 H43B 107.8 . . ?
C4 C3 C2 118.8(9) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
O16 C37 N10 125.7(7) . . ?
O16 C37 N9 126.1(7) . . ?
N10 C37 N9 108.2(6) . . ?
N8 C26 N14 114.9(6) . 2_577 ?
N8 C26 H26A 108.5 . . ?
N14 C26 H26A 108.5 2_577 . ?
N8 C26 H26B 108.5 . . ?
N14 C26 H26B 108.5 2_577 . ?
H26A C26 H26B 107.5 . . ?
N13 C34 N12 113.7(6) . . ?
N13 C34 H34A 108.8 . . ?
N12 C34 H34A 108.8 . . ?
N13 C34 H34B 108.8 . . ?
N12 C34 H34B 108.8 . . ?
H34A C34 H34B 107.7 . . ?
O15 C35 N11 126.0(7) . . ?
O15 C35 N12 125.9(8) . . ?
N11 C35 N12 108.1(7) . . ?
N6 C24 N7 113.9(6) . . ?
N6 C24 H24A 108.8 . . ?
N7 C24 H24A 108.8 . . ?
N6 C24 H24B 108.8 . . ?
N7 C24 H24B 108.8 . . ?
H24A C24 H24B 107.7 . . ?
N11 C29 N6 115.4(6) . . ?
N11 C29 C30 104.3(6) . . ?
N6 C29 C30 102.8(6) . . ?
N11 C29 H29 111.3 . . ?
N6 C29 H29 111.3 . . ?
C30 C29 H29 111.3 . . ?
N19 C54 N22 116.1(7) . . ?
N19 C54 C55 103.1(7) . . ?
N22 C54 C55 103.2(6) . . ?
N19 C54 H54 111.3 . . ?
N22 C54 H54 111.3 . . ?
C55 C54 H54 111.3 . . ?
N20 C55 N21 115.5(6) . . ?
N20 C55 C54 103.3(7) . . ?
N21 C55 C54 102.6(6) . . ?
N20 C55 H55 111.6 . . ?
N21 C55 H55 111.6 . . ?
C54 C55 H55 111.6 . . ?
O19 C21 N3 126.0(7) . . ?
O19 C21 N4 126.3(7) . . ?
N3 C21 N4 107.7(6) . . ?
N1 C15 C16 119.6(10) . . ?
N1 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
N16 C42 N17 113.1(6) . . ?
N16 C42 H42A 109.0 . . ?
N17 C42 H42A 109.0 . . ?
N16 C42 H42B 109.0 . . ?
N17 C42 H42B 109.0 . . ?
H42A C42 H42B 107.8 . . ?
O12 C38 N17 127.6(8) . . ?
O12 C38 N18 125.2(8) . . ?
N17 C38 N18 107.2(8) . . ?
N2 C4 C3 120.8(11) . . ?
N2 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
O13 C52 N20 127.2(9) . . ?
O13 C52 N19 125.3(8) . . ?
N20 C52 N19 107.5(8) . . ?
O3 C1 O2 124.4(11) . . ?
O3 C1 C2 121.8(9) . . ?
O2 C1 C2 113.4(11) . . ?
O5 C10 O4 122(2) . . ?
O5 C10 C12 113.3(18) . . ?
O4 C10 C12 122.1(15) . . ?
O5 C10 U1 63.3(12) . . ?
O4 C10 U1 59.3(12) . . ?
C12 C10 U1 171.9(14) . . ?
N18 C50 N19 114.1(7) . . ?
N18 C50 H50A 108.7 . . ?
N19 C50 H50A 108.7 . . ?
N18 C50 H50B 108.7 . . ?
N19 C50 H50B 108.7 . . ?
H50A C50 H50B 107.6 . . ?
C15 C16 C12 119.8(11) . . ?
C15 C16 H16 120.1 . . ?
C12 C16 H16 120.1 . . ?
C13 C12 C16 118.8(8) . . ?
C13 C12 C10 137.1(14) . . ?
C16 C12 C10 103.7(14) . . ?
C13 C12 C11 106.3(13) . . ?
C16 C12 C11 134.9(14) . . ?
C5 C6 C2 119.9(11) . . ?
C5 C6 H6 120.0 . . ?
C2 C6 H6 120.0 . . ?
N2 C7 C8 112.6(9) . . ?
N2 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
N2 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.8 . . ?
C14 C13 C12 120.2(11) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C7 C8 C9 105.9(10) . . ?
C7 C8 H8A 110.6 . . ?
C9 C8 H8A 110.6 . . ?
C7 C8 H8B 110.6 . . ?
C9 C8 H8B 110.6 . . ?
H8A C8 H8B 108.7 . . ?
N2 C5 C6 119.9(9) . . ?
N2 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C9 C9 C8 111.2(13) 2_766 . ?
C9 C9 H9A 109.4 2_766 . ?
C8 C9 H9A 109.4 . . ?
C9 C9 H9B 109.4 2_766 . ?
C8 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
C10 O5 U1 92.5(14) . . ?
C56 N22 C54 112.7(6) . . ?
C56 N22 C53 121.9(7) . . ?
C54 N22 C53 123.5(7) . . ?
N22 C53 N23 113.8(7) . . ?
N22 C53 H53A 108.8 . . ?
N23 C53 H53A 108.8 . . ?
N22 C53 H53B 108.8 . . ?
N23 C53 H53B 108.8 . . ?
H53A C53 H53B 107.7 . . ?
C56 N21 C55 113.2(6) . . ?
C56 N21 C48 121.3(6) . 2_766 ?
C55 N21 C48 122.9(6) . 2_766 ?
O10 C56 N22 126.1(7) . . ?
O10 C56 N21 126.5(7) . . ?
N22 C56 N21 107.4(7) . . ?
N15 C48 N21 114.2(6) . 2_766 ?
N15 C48 H48A 108.7 . . ?
N21 C48 H48A 108.7 2_766 . ?
N15 C48 H48B 108.7 . . ?
N21 C48 H48B 108.7 2_766 . ?
H48A C48 H48B 107.6 . . ?
N26 C49 N20 112.8(6) . 2_766 ?
N26 C49 H49A 109.0 . . ?
N20 C49 H49A 109.0 2_766 . ?
N26 C49 H49B 109.0 . . ?
N20 C49 H49B 109.0 2_766 . ?
H49A C49 H49B 107.8 . . ?
C14 N1 C15 120.7(7) . . ?
C14 N1 C17 118.2(7) . . ?
C15 N1 C17 121.1(7) . . ?
O6 C11 O7 125.3(19) . . ?
O6 C11 C12 107.3(18) . . ?
O7 C11 C12 126.1(19) . . ?
C11 O6 U1 125.1(13) . . ?
C1 O2 U1 159.1(10) . . ?

_refine_diff_density_max         3.034
_refine_diff_density_min         -2.991
_refine_diff_density_rms         0.176

_shelxl_version_number           2014-3



