#------------------------------------------------------------------------------
#$Date: 2017-05-02 03:55:00 +0200 (mar 02 de may de 2017) $
#$Revision: 195887 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/28/7042835.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_7042835
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
;
2017-03-04 deposited with the CCDC.
2017-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                91.439(5)
_cell_angle_beta                 96.887(6)
_cell_angle_gamma                93.574(5)
_cell_formula_units_Z            1
_cell_length_a                   12.8248(15)
_cell_length_b                   14.8362(16)
_cell_length_c                   17.044(2)
_cell_measurement_reflns_used    9464
_cell_measurement_temperature    320(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      3.04
_cell_volume                     3211.6(6)
_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      320(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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  0.0437
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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            81895
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.041
_exptl_absorpt_coefficient_mu    1.985
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       block
_exptl_crystal_F_000             1558
_refine_diff_density_max         3.265
_refine_diff_density_min         -1.877
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         14709
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0468
_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)+(0.0933P)²+3.5401P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1357
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14028
_reflns_number_total             14709
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt01034f2.cif
_cod_data_source_block           2-bUP-320K
_cod_database_code               7042835
_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 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 .
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_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 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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 .
