#------------------------------------------------------------------------------
#$Date: 2017-05-02 04:55:00 +0300 (Tue, 02 May 2017) $
#$Revision: 195887 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/28/7042834.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7042834
loop_
_publ_author_name
'Xie, Zhen-ni'
'Mei, Lei'
'Wu, Qunyan'
'Hu, Kong-qiu'
'Xia, Liang-Shu'
'Chai, Zhifang'
'Shi, Weiqun'
_publ_section_title
;
 Temperature-induced Reversible Single-Crystal-to-Single-Crystal
 Isomerisation of Uranyl Polyrotaxane: An Exquisite Case of Coordination
 Variability of Uranyl Center
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01034F
_journal_year                    2017
_chemical_formula_sum            'C108 H112 Br2 N52 O34 U'
_chemical_formula_weight         3080.34
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2017-02-22 deposited with the CCDC.
2017-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                91.261(2)
_cell_angle_beta                 97.291(2)
_cell_angle_gamma                93.699(2)
_cell_formula_units_Z            1
_cell_length_a                   12.7846(5)
_cell_length_b                   14.7915(6)
_cell_length_c                   17.0792(7)
_cell_measurement_reflns_used    9577
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      3.03
_cell_volume                     3195.5(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            72367
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.978
_exptl_absorpt_coefficient_mu    1.995
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_description       block
_exptl_crystal_F_000             1558
_refine_diff_density_max         1.963
_refine_diff_density_min         -3.379
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         14613
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1100P)²+9.7677P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.1683
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13732
_reflns_number_total             14613
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt01034f2.cif
_cod_data_source_block           5-bUP-296K
_cod_database_code               7042834
_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.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
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 .
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'
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
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 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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 .
