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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_U(N2CPh2)(TIG)3
_database_code_depnum_ccdc_archive 'CCDC 1860826'
_audit_update_record             
;
2018-08-07 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT094_U(N2CPh2)(TIG)3     
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       4.50 Report
RESPONSE: Due to unresolved minor twin component
;
# Added during the CSD deposition process: Tuesday 07 August 2018 10:16 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            U(N2CPh2)(TIG)3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C57 H106 N11 U'
_chemical_formula_weight         1183.55

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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.3599(6)
_cell_length_b                   12.6609(6)
_cell_length_c                   21.0290(11)
_cell_angle_alpha                88.8639(11)
_cell_angle_beta                 77.3174(11)
_cell_angle_gamma                79.3741(11)
_cell_volume                     3154.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9842
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      25.36

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_F_000             1234
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.614
_shelx_estimated_absorpt_T_min   0.744
_shelx_estimated_absorpt_T_max   0.780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            50668
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.637
_diffrn_reflns_theta_max         25.396
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measured_fraction_theta_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_point_group_measured_fraction_full 0.961
_reflns_number_total             11131
_reflns_number_gt                10020
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury 3.10'
_computing_publication_material  WinGX
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0362P)²+4.0961P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11131
_refine_ls_number_parameters     648
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0750
_refine_ls_wR_factor_gt          0.0726
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_restrained_S_all      1.115
_refine_ls_shift/su_max          0.006
_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
C1 C 0.0978(3) 0.4155(3) 0.70748(17) 0.0212(8) Uani 1 1 d . . . . .
H1A H 0.1041 0.4147 0.7531 0.032 Uiso 1 1 calc R U . . .
H1B H 0.0184 0.4372 0.7053 0.032 Uiso 1 1 calc R U . . .
H1C H 0.1415 0.4666 0.6836 0.032 Uiso 1 1 calc R U . . .
C2 C 0.1432(3) 0.3038(3) 0.67707(16) 0.0181(8) Uani 1 1 d . . . . .
H2 H 0.1399 0.3067 0.6300 0.022 Uiso 1 1 calc R U . . .
C3 C 0.0657(3) 0.2293(3) 0.71124(19) 0.0241(9) Uani 1 1 d . . . . .
H3A H 0.0950 0.1558 0.6940 0.036 Uiso 1 1 calc R U . . .
H3B H -0.0103 0.2533 0.7034 0.036 Uiso 1 1 calc R U . . .
H3C H 0.0624 0.2310 0.7582 0.036 Uiso 1 1 calc R U . . .
C4 C 0.3425(3) 0.2468(3) 0.62774(16) 0.0152(7) Uani 1 1 d . . . . .
C5 C 0.1786(3) 0.1863(4) 0.50755(19) 0.0297(9) Uani 1 1 d . . . . .
H5A H 0.1232 0.2500 0.5258 0.044 Uiso 1 1 calc R U . . .
H5B H 0.1396 0.1270 0.5034 0.044 Uiso 1 1 calc R U . . .
H5C H 0.2209 0.2027 0.4645 0.044 Uiso 1 1 calc R U . . .
C6 C 0.2606(3) 0.1540(3) 0.55293(17) 0.0207(8) Uani 1 1 d . . . . .
H6 H 0.2135 0.1396 0.5962 0.025 Uiso 1 1 calc R U . . .
C7 C 0.3397(3) 0.0475(4) 0.52909(19) 0.0287(9) Uani 1 1 d . . . . .
H7A H 0.3818 0.0552 0.4845 0.043 Uiso 1 1 calc R U . . .
H7B H 0.2952 -0.0092 0.5298 0.043 Uiso 1 1 calc R U . . .
H7C H 0.3927 0.0285 0.5578 0.043 Uiso 1 1 calc R U . . .
C8 C 0.2804(4) 0.4038(4) 0.5006(2) 0.0329(10) Uani 1 1 d . . . . .
H8A H 0.2341 0.3777 0.4743 0.049 Uiso 1 1 calc R U . . .
H8B H 0.3180 0.4591 0.4768 0.049 Uiso 1 1 calc R U . . .
H8C H 0.2323 0.4345 0.5419 0.049 Uiso 1 1 calc R U . . .
C9 C 0.3694(3) 0.3101(3) 0.51451(17) 0.0233(8) Uani 1 1 d . . . . .
H9 H 0.4225 0.3434 0.5338 0.028 Uiso 1 1 calc R U . . .
C10 C 0.4400(3) 0.2549(4) 0.45072(18) 0.0320(10) Uani 1 1 d . . . . .
H10A H 0.4996 0.1983 0.4603 0.048 Uiso 1 1 calc R U . . .
H10B H 0.4743 0.3080 0.4225 0.048 Uiso 1 1 calc R U . . .
H10C H 0.3915 0.2231 0.4285 0.048 Uiso 1 1 calc R U . . .
C11 C 0.6271(3) 0.2618(3) 0.56083(18) 0.0261(9) Uani 1 1 d . . . . .
H11A H 0.5877 0.3154 0.5355 0.039 Uiso 1 1 calc R U . . .
H11B H 0.6943 0.2206 0.5321 0.039 Uiso 1 1 calc R U . . .
H11C H 0.6496 0.2981 0.5952 0.039 Uiso 1 1 calc R U . . .
C12 C 0.5485(3) 0.1856(3) 0.59170(16) 0.0202(8) Uani 1 1 d . . . . .
H12 H 0.5247 0.1502 0.5563 0.024 Uiso 1 1 calc R U . . .
C13 C 0.6121(3) 0.0990(3) 0.62835(18) 0.0260(9) Uani 1 1 d . . . . .
H13A H 0.6339 0.1324 0.6641 0.039 Uiso 1 1 calc R U . . .
H13B H 0.6799 0.0612 0.5984 0.039 Uiso 1 1 calc R U . . .
H13C H 0.5634 0.0476 0.6461 0.039 Uiso 1 1 calc R U . . .
C14 C 0.2003(3) 0.0322(3) 0.81340(18) 0.0242(8) Uani 1 1 d . . . . .
H14A H 0.2003 0.0356 0.8599 0.036 Uiso 1 1 calc R U . . .
H14B H 0.1605 -0.0247 0.8054 0.036 Uiso 1 1 calc R U . . .
H14C H 0.1620 0.1013 0.8003 0.036 Uiso 1 1 calc R U . . .
C15 C 0.3220(3) 0.0077(3) 0.77374(18) 0.0204(8) Uani 1 1 d . . . . .
H15 H 0.3613 -0.0603 0.7900 0.024 Uiso 1 1 calc R U . . .
C16 C 0.3241(3) -0.0088(3) 0.70205(18) 0.0252(9) Uani 1 1 d . . . . .
H16A H 0.2836 0.0563 0.6857 0.038 Uiso 1 1 calc R U . . .
H16B H 0.2876 -0.0697 0.6970 0.038 Uiso 1 1 calc R U . . .
H16C H 0.4025 -0.0238 0.6773 0.038 Uiso 1 1 calc R U . . .
C17 C 0.4723(3) 0.0765(3) 0.80926(16) 0.0186(8) Uani 1 1 d . . . . .
C18 C 0.6032(3) -0.1633(3) 0.7292(2) 0.0307(9) Uani 1 1 d . . . . .
H18A H 0.5901 -0.2265 0.7554 0.046 Uiso 1 1 calc R U . . .
H18B H 0.6686 -0.1838 0.6929 0.046 Uiso 1 1 calc R U . . .
H18C H 0.5364 -0.1348 0.7119 0.046 Uiso 1 1 calc R U . . .
C19 C 0.6261(3) -0.0773(3) 0.77175(18) 0.0235(8) Uani 1 1 d . . . . .
H19 H 0.6446 -0.0172 0.7422 0.028 Uiso 1 1 calc R U . . .
C20 C 0.7313(3) -0.1198(4) 0.7981(2) 0.0297(9) Uani 1 1 d . . . . .
H20A H 0.7482 -0.0624 0.8228 0.045 Uiso 1 1 calc R U . . .
H20B H 0.7953 -0.1440 0.7617 0.045 Uiso 1 1 calc R U . . .
H20C H 0.7179 -0.1802 0.8267 0.045 Uiso 1 1 calc R U . . .
C21 C 0.4941(4) -0.1878(3) 0.8917(2) 0.0319(10) Uani 1 1 d . . . . .
H21A H 0.4247 -0.1931 0.8777 0.048 Uiso 1 1 calc R U . . .
H21B H 0.4886 -0.2129 0.9365 0.048 Uiso 1 1 calc R U . . .
H21C H 0.5587 -0.2324 0.8628 0.048 Uiso 1 1 calc R U . . .
C22 C 0.5101(3) -0.0712(3) 0.88894(18) 0.0236(8) Uani 1 1 d . . . . .
H22 H 0.5805 -0.0676 0.9042 0.028 Uiso 1 1 calc R U . . .
C23 C 0.4117(3) -0.0012(4) 0.93479(18) 0.0286(9) Uani 1 1 d . . . . .
H23A H 0.4259 0.0724 0.9354 0.043 Uiso 1 1 calc R U . . .
H23B H 0.4038 -0.0299 0.9789 0.043 Uiso 1 1 calc R U . . .
H23C H 0.3422 -0.0010 0.9196 0.043 Uiso 1 1 calc R U . . .
C24 C 0.7169(3) 0.1731(3) 0.79787(17) 0.0225(8) Uani 1 1 d . . . . .
H24A H 0.7368 0.1165 0.7640 0.034 Uiso 1 1 calc R U . . .
H24B H 0.7794 0.1701 0.8199 0.034 Uiso 1 1 calc R U . . .
H24C H 0.7023 0.2434 0.7779 0.034 Uiso 1 1 calc R U . . .
C25 C 0.6115(3) 0.1563(3) 0.84724(18) 0.0210(8) Uani 1 1 d . . . . .
H25 H 0.6272 0.0823 0.8648 0.025 Uiso 1 1 calc R U . . .
C26 C 0.5859(3) 0.2359(3) 0.90419(18) 0.0272(9) Uani 1 1 d . . . . .
H26A H 0.5658 0.3090 0.8888 0.041 Uiso 1 1 calc R U . . .
H26B H 0.6527 0.2309 0.9228 0.041 Uiso 1 1 calc R U . . .
H26C H 0.5228 0.2193 0.9376 0.041 Uiso 1 1 calc R U . . .
C27 C 0.2613(4) 0.2890(4) 0.93520(18) 0.0324(10) Uani 1 1 d . . . . .
H27A H 0.2943 0.2214 0.9106 0.049 Uiso 1 1 calc R U . . .
H27B H 0.2219 0.2733 0.9791 0.049 Uiso 1 1 calc R U . . .
H27C H 0.3214 0.3282 0.9383 0.049 Uiso 1 1 calc R U . . .
C28 C 0.1776(3) 0.3576(3) 0.90012(16) 0.0206(8) Uani 1 1 d . . . . .
H28 H 0.1485 0.4283 0.9238 0.025 Uiso 1 1 calc R U . . .
C29 C 0.0786(3) 0.3020(3) 0.89955(18) 0.0289(9) Uani 1 1 d . . . . .
H29A H 0.0269 0.3458 0.8759 0.043 Uiso 1 1 calc R U . . .
H29B H 0.0386 0.2931 0.9445 0.043 Uiso 1 1 calc R U . . .
H29C H 0.1065 0.2314 0.8779 0.043 Uiso 1 1 calc R U . . .
C30 C 0.2483(3) 0.4755(3) 0.81324(16) 0.0153(7) Uani 1 1 d . . . . .
C31 C -0.0144(3) 0.6193(3) 0.92057(17) 0.0245(9) Uani 1 1 d . . . . .
H31A H 0.0118 0.5714 0.9535 0.037 Uiso 1 1 calc R U . . .
H31B H -0.0944 0.6189 0.9229 0.037 Uiso 1 1 calc R U . . .
H31C H -0.0046 0.6925 0.9288 0.037 Uiso 1 1 calc R U . . .
C32 C 0.0545(3) 0.5803(3) 0.85260(16) 0.0196(8) Uani 1 1 d . . . . .
H32 H 0.0397 0.5067 0.8460 0.023 Uiso 1 1 calc R U . . .
C33 C 0.0079(3) 0.6512(3) 0.80079(18) 0.0258(9) Uani 1 1 d . . . . .
H33A H 0.0127 0.7261 0.8083 0.039 Uiso 1 1 calc R U . . .
H33B H -0.0711 0.6455 0.8038 0.039 Uiso 1 1 calc R U . . .
H33C H 0.0524 0.6270 0.7573 0.039 Uiso 1 1 calc R U . . .
C34 C 0.2254(3) 0.6449(3) 0.94186(17) 0.0254(9) Uani 1 1 d . . . . .
H34A H 0.1484 0.6757 0.9649 0.038 Uiso 1 1 calc R U . . .
H34B H 0.2783 0.6861 0.9533 0.038 Uiso 1 1 calc R U . . .
H34C H 0.2445 0.5699 0.9545 0.038 Uiso 1 1 calc R U . . .
C35 C 0.2330(3) 0.6492(3) 0.86817(16) 0.0188(8) Uani 1 1 d . . . . .
H35 H 0.3151 0.6290 0.8474 0.023 Uiso 1 1 calc R U . . .
C36 C 0.1963(3) 0.7641(3) 0.84760(19) 0.0261(9) Uani 1 1 d . . . . .
H36A H 0.2046 0.7655 0.8002 0.039 Uiso 1 1 calc R U . . .
H36B H 0.2435 0.8104 0.8605 0.039 Uiso 1 1 calc R U . . .
H36C H 0.1172 0.7901 0.8689 0.039 Uiso 1 1 calc R U . . .
C37 C 0.3661(3) 0.5211(3) 0.64590(16) 0.0222(8) Uani 1 1 d . . . . .
H37A H 0.4402 0.4737 0.6378 0.033 Uiso 1 1 calc R U . . .
H37B H 0.3679 0.5802 0.6151 0.033 Uiso 1 1 calc R U . . .
H37C H 0.3089 0.4801 0.6400 0.033 Uiso 1 1 calc R U . . .
C38 C 0.3367(3) 0.5668(3) 0.71586(16) 0.0189(8) Uani 1 1 d . . . . .
H38 H 0.2603 0.6138 0.7236 0.023 Uiso 1 1 calc R U . . .
C39 C 0.4237(3) 0.6366(3) 0.72051(17) 0.0223(8) Uani 1 1 d . . . . .
H39A H 0.4091 0.6656 0.7651 0.033 Uiso 1 1 calc R U . . .
H39B H 0.4179 0.6960 0.6901 0.033 Uiso 1 1 calc R U . . .
H39C H 0.4997 0.5929 0.7094 0.033 Uiso 1 1 calc R U . . .
C40 C 0.6912(3) 0.4420(3) 0.72664(17) 0.0217(8) Uani 1 1 d . . . . .
C41 C 0.6676(3) 0.4688(3) 0.79733(18) 0.0201(8) Uani 1 1 d . . . . .
C42 C 0.7571(3) 0.4619(3) 0.82915(18) 0.0268(9) Uani 1 1 d . . . . .
H42 H 0.8324 0.4392 0.8053 0.032 Uiso 1 1 calc R U . . .
C43 C 0.7375(3) 0.4875(4) 0.89461(19) 0.0303(10) Uani 1 1 d . . . . .
H43 H 0.7991 0.4806 0.9156 0.036 Uiso 1 1 calc R U . . .
C44 C 0.6292(4) 0.5230(3) 0.92982(19) 0.0309(10) Uani 1 1 d . . . . .
H44 H 0.6158 0.5432 0.9745 0.037 Uiso 1 1 calc R U . . .
C45 C 0.5402(3) 0.5289(3) 0.89887(18) 0.0261(9) Uani 1 1 d . . . . .
H45 H 0.4652 0.5524 0.9230 0.031 Uiso 1 1 calc R U . . .
C46 C 0.5583(3) 0.5014(3) 0.83389(18) 0.0234(8) Uani 1 1 d . . . . .
H46 H 0.4960 0.5046 0.8139 0.028 Uiso 1 1 calc R U . . .
C47 C 0.7843(3) 0.4837(3) 0.68200(17) 0.0201(8) Uani 1 1 d . . . . .
C48 C 0.8088(3) 0.5827(3) 0.69376(18) 0.0227(8) Uani 1 1 d . . . . .
H48 H 0.7670 0.6235 0.7315 0.027 Uiso 1 1 calc R U . . .
C49 C 0.8934(3) 0.6236(4) 0.65128(19) 0.0279(9) Uani 1 1 d . . . . .
H49 H 0.9078 0.6925 0.6597 0.033 Uiso 1 1 calc R U . . .
C50 C 0.9567(3) 0.5644(4) 0.59691(19) 0.0303(10) Uani 1 1 d . . . . .
H50 H 1.0157 0.5914 0.5683 0.036 Uiso 1 1 calc R U . . .
C51 C 0.9332(3) 0.4657(4) 0.58483(18) 0.0272(9) Uani 1 1 d . . . . .
H51 H 0.9765 0.4250 0.5474 0.033 Uiso 1 1 calc R U . . .
C52 C 0.8481(3) 0.4243(3) 0.62590(17) 0.0225(8) Uani 1 1 d . . . . .
H52 H 0.8327 0.3563 0.6164 0.027 Uiso 1 1 calc R U . . .
C56 C 0.1680(4) 0.7511(5) 0.6056(3) 0.0668(18) Uani 1 1 d . . . . .
H56A H 0.2293 0.7846 0.6137 0.100 Uiso 1 1 calc R U . . .
H56B H 0.1964 0.7022 0.5676 0.100 Uiso 1 1 calc R U . . .
H56C H 0.1395 0.7106 0.6439 0.100 Uiso 1 1 calc R U . . .
C57 C 0.0746(5) 0.8365(5) 0.5927(3) 0.0643(17) Uani 1 1 d . . . . .
H57A H 0.1035 0.8817 0.5563 0.077 Uiso 1 1 calc R U . . .
H57B H 0.0146 0.8036 0.5810 0.077 Uiso 1 1 calc R U . . .
C58 C 0.0302(5) 0.9010(6) 0.6527(3) 0.076(2) Uani 1 1 d . . . . .
H58A H 0.0910 0.9354 0.6620 0.092 Uiso 1 1 calc R U . . .
H58B H 0.0097 0.8525 0.6890 0.092 Uiso 1 1 calc R U . . .
C59 C -0.0790(5) 0.9940(6) 0.6514(3) 0.0703(19) Uani 1 1 d . . . . .
H59A H -0.1414 0.9576 0.6471 0.084 Uiso 1 1 calc R U . . .
H59B H -0.1015 1.0310 0.6946 0.084 Uiso 1 1 calc R U . . .
C60 C -0.0718(5) 1.0779(7) 0.6015(3) 0.088(3) Uani 1 1 d . . . . .
H60A H -0.0079 1.1129 0.6028 0.131 Uiso 1 1 calc R U . . .
H60B H -0.1417 1.1315 0.6103 0.131 Uiso 1 1 calc R U . . .
H60C H -0.0609 1.0449 0.5582 0.131 Uiso 1 1 calc R U . . .
N1 N 0.2612(2) 0.2660(2) 0.68170(13) 0.0168(6) Uani 1 1 d . . . . .
N2 N 0.3219(2) 0.2374(3) 0.56465(13) 0.0177(6) Uani 1 1 d . . . . .
N3 N 0.4467(2) 0.2399(3) 0.63804(13) 0.0170(6) Uani 1 1 d . . . . .
N4 N 0.3807(2) 0.0950(2) 0.78386(14) 0.0180(6) Uani 1 1 d . . . . .
N5 N 0.5237(2) -0.0314(2) 0.82189(14) 0.0191(7) Uani 1 1 d . . . . .
N6 N 0.5126(2) 0.1634(2) 0.81790(14) 0.0189(7) Uani 1 1 d . . . . .
N7 N 0.2382(2) 0.3765(2) 0.83360(13) 0.0165(6) Uani 1 1 d . . . . .
N8 N 0.1781(2) 0.5690(2) 0.84392(13) 0.0158(6) Uani 1 1 d . . . . .
N9 N 0.3320(2) 0.4769(2) 0.76144(13) 0.0161(6) Uani 1 1 d . . . . .
N10 N 0.5504(2) 0.3422(3) 0.72681(14) 0.0192(7) Uani 1 1 d . . . . .
N11 N 0.6349(2) 0.3863(3) 0.69840(14) 0.0211(7) Uani 1 1 d . . . . .
U1 U 0.40233(2) 0.28339(2) 0.75132(2) 0.01565(5) 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
C1 C2 1.519(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N1 1.472(4) . ?
C2 C3 1.526(5) . ?
C2 H2 1.0000 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 N1 1.333(4) . ?
C4 N3 1.339(4) . ?
C4 N2 1.416(4) . ?
C4 U1 2.921(3) . ?
C5 C6 1.537(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 N2 1.462(5) . ?
C6 C7 1.533(5) . ?
C6 H6 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.532(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.481(5) . ?
C9 C10 1.532(5) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.530(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N3 1.475(4) . ?
C12 C13 1.526(5) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.531(5) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 N4 1.472(5) . ?
C15 C16 1.520(5) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N6 1.321(5) . ?
C17 N4 1.335(4) . ?
C17 N5 1.442(5) . ?
C17 U1 2.932(4) . ?
C18 C19 1.526(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 N5 1.489(5) . ?
C19 C20 1.528(5) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.523(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 N5 1.473(4) . ?
C22 C23 1.521(5) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.523(5) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 N6 1.473(4) . ?
C25 C26 1.522(5) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.532(5) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 N7 1.472(4) . ?
C28 C29 1.523(5) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 N9 1.330(4) . ?
C30 N7 1.336(5) . ?
C30 N8 1.405(4) . ?
C30 U1 2.927(3) . ?
C31 C32 1.533(5) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 N8 1.478(4) . ?
C32 C33 1.540(5) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.532(5) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 N8 1.477(5) . ?
C35 C36 1.525(5) . ?
C35 H35 1.0000 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.534(5) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 N9 1.474(4) . ?
C38 C39 1.532(5) . ?
C38 H38 1.0000 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 N11 1.309(5) . ?
C40 C41 1.484(5) . ?
C40 C47 1.488(5) . ?
C41 C46 1.392(5) . ?
C41 C42 1.402(5) . ?
C42 C43 1.379(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.377(6) . ?
C43 H43 0.9500 . ?
C44 C45 1.387(6) . ?
C44 H44 0.9500 . ?
C45 C46 1.376(5) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 C48 1.381(6) . ?
C47 C52 1.410(5) . ?
C48 C49 1.390(5) . ?
C48 H48 0.9500 . ?
C49 C50 1.381(6) . ?
C49 H49 0.9500 . ?
C50 C51 1.373(6) . ?
C50 H50 0.9500 . ?
C51 C52 1.384(5) . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
C56 C57 1.497(8) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 C58 1.460(8) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 C59 1.623(9) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 C60 1.480(9) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
N1 U1 2.552(3) . ?
N3 U1 2.376(3) . ?
N4 U1 2.513(3) . ?
N6 U1 2.473(3) . ?
N7 U1 2.481(3) . ?
N9 U1 2.441(3) . ?
N10 N11 1.299(4) . ?
N10 U1 2.060(3) . ?

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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C1 111.4(3) . . ?
N1 C2 C3 112.1(3) . . ?
C1 C2 C3 107.6(3) . . ?
N1 C2 H2 108.6 . . ?
C1 C2 H2 108.6 . . ?
C3 C2 H2 108.6 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 N3 113.9(3) . . ?
N1 C4 N2 123.7(3) . . ?
N3 C4 N2 122.4(3) . . ?
N1 C4 U1 60.80(17) . . ?
N3 C4 U1 53.26(16) . . ?
N2 C4 U1 173.4(2) . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C6 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 C7 112.4(3) . . ?
N2 C6 C5 114.8(3) . . ?
C7 C6 C5 110.1(3) . . ?
N2 C6 H6 106.3 . . ?
C7 C6 H6 106.3 . . ?
C5 C6 H6 106.3 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C8 112.9(3) . . ?
N2 C9 C10 115.3(3) . . ?
C8 C9 C10 110.6(3) . . ?
N2 C9 H9 105.7 . . ?
C8 C9 H9 105.7 . . ?
C10 C9 H9 105.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 C13 108.0(3) . . ?
N3 C12 C11 113.4(3) . . ?
C13 C12 C11 109.3(3) . . ?
N3 C12 H12 108.7 . . ?
C13 C12 H12 108.7 . . ?
C11 C12 H12 108.7 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N4 C15 C16 111.8(3) . . ?
N4 C15 C14 109.6(3) . . ?
C16 C15 C14 110.4(3) . . ?
N4 C15 H15 108.3 . . ?
C16 C15 H15 108.3 . . ?
C14 C15 H15 108.3 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N6 C17 N4 114.3(3) . . ?
N6 C17 N5 124.5(3) . . ?
N4 C17 N5 121.1(3) . . ?
N6 C17 U1 56.93(18) . . ?
N4 C17 U1 58.74(18) . . ?
N5 C17 U1 165.9(2) . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C19 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N5 C19 C18 111.8(3) . . ?
N5 C19 C20 115.1(3) . . ?
C18 C19 C20 110.2(3) . . ?
N5 C19 H19 106.4 . . ?
C18 C19 H19 106.4 . . ?
C20 C19 H19 106.4 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N5 C22 C23 111.1(3) . . ?
N5 C22 C21 111.4(3) . . ?
C23 C22 C21 110.2(3) . . ?
N5 C22 H22 108.0 . . ?
C23 C22 H22 108.0 . . ?
C21 C22 H22 108.0 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C25 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N6 C25 C26 110.4(3) . . ?
N6 C25 C24 112.6(3) . . ?
C26 C25 C24 110.5(3) . . ?
N6 C25 H25 107.7 . . ?
C26 C25 H25 107.7 . . ?
C24 C25 H25 107.7 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C28 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N7 C28 C29 111.6(3) . . ?
N7 C28 C27 108.3(3) . . ?
C29 C28 C27 110.4(3) . . ?
N7 C28 H28 108.8 . . ?
C29 C28 H28 108.8 . . ?
C27 C28 H28 108.8 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N9 C30 N7 113.3(3) . . ?
N9 C30 N8 123.4(3) . . ?
N7 C30 N8 123.3(3) . . ?
N9 C30 U1 55.78(18) . . ?
N7 C30 U1 57.55(17) . . ?
N8 C30 U1 177.6(2) . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N8 C32 C31 115.2(3) . . ?
N8 C32 C33 112.9(3) . . ?
C31 C32 C33 109.3(3) . . ?
N8 C32 H32 106.3 . . ?
C31 C32 H32 106.3 . . ?
C33 C32 H32 106.3 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C35 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N8 C35 C36 114.6(3) . . ?
N8 C35 C34 113.3(3) . . ?
C36 C35 C34 110.8(3) . . ?
N8 C35 H35 105.8 . . ?
C36 C35 H35 105.8 . . ?
C34 C35 H35 105.8 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N9 C38 C39 115.4(3) . . ?
N9 C38 C37 108.7(3) . . ?
C39 C38 C37 107.0(3) . . ?
N9 C38 H38 108.5 . . ?
C39 C38 H38 108.5 . . ?
C37 C38 H38 108.5 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N11 C40 C41 125.9(3) . . ?
N11 C40 C47 115.3(3) . . ?
C41 C40 C47 118.8(3) . . ?
C46 C41 C42 118.1(3) . . ?
C46 C41 C40 122.0(3) . . ?
C42 C41 C40 119.9(3) . . ?
C43 C42 C41 121.0(4) . . ?
C43 C42 H42 119.5 . . ?
C41 C42 H42 119.5 . . ?
C44 C43 C42 120.5(4) . . ?
C44 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
C43 C44 C45 118.9(4) . . ?
C43 C44 H44 120.6 . . ?
C45 C44 H44 120.6 . . ?
C46 C45 C44 121.3(4) . . ?
C46 C45 H45 119.4 . . ?
C44 C45 H45 119.4 . . ?
C45 C46 C41 120.3(4) . . ?
C45 C46 H46 119.9 . . ?
C41 C46 H46 119.9 . . ?
C48 C47 C52 118.3(3) . . ?
C48 C47 C40 120.8(3) . . ?
C52 C47 C40 120.9(4) . . ?
C47 C48 C49 121.1(4) . . ?
C47 C48 H48 119.4 . . ?
C49 C48 H48 119.4 . . ?
C50 C49 C48 120.3(4) . . ?
C50 C49 H49 119.9 . . ?
C48 C49 H49 119.9 . . ?
C51 C50 C49 119.0(4) . . ?
C51 C50 H50 120.5 . . ?
C49 C50 H50 120.5 . . ?
C50 C51 C52 121.6(4) . . ?
C50 C51 H51 119.2 . . ?
C52 C51 H51 119.2 . . ?
C51 C52 C47 119.6(4) . . ?
C51 C52 H52 120.2 . . ?
C47 C52 H52 120.2 . . ?
C57 C56 H56A 109.5 . . ?
C57 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C57 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C58 C57 C56 106.7(5) . . ?
C58 C57 H57A 110.4 . . ?
C56 C57 H57A 110.4 . . ?
C58 C57 H57B 110.4 . . ?
C56 C57 H57B 110.4 . . ?
H57A C57 H57B 108.6 . . ?
C57 C58 C59 115.0(5) . . ?
C57 C58 H58A 108.5 . . ?
C59 C58 H58A 108.5 . . ?
C57 C58 H58B 108.5 . . ?
C59 C58 H58B 108.5 . . ?
H58A C58 H58B 107.5 . . ?
C60 C59 C58 119.9(5) . . ?
C60 C59 H59A 107.3 . . ?
C58 C59 H59A 107.3 . . ?
C60 C59 H59B 107.3 . . ?
C58 C59 H59B 107.3 . . ?
H59A C59 H59B 106.9 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C4 N1 C2 120.2(3) . . ?
C4 N1 U1 92.1(2) . . ?
C2 N1 U1 142.5(2) . . ?
C4 N2 C6 118.1(3) . . ?
C4 N2 C9 116.9(3) . . ?
C6 N2 C9 124.9(3) . . ?
C4 N3 C12 122.8(3) . . ?
C4 N3 U1 99.9(2) . . ?
C12 N3 U1 134.6(2) . . ?
C17 N4 C15 121.3(3) . . ?
C17 N4 U1 94.2(2) . . ?
C15 N4 U1 143.1(2) . . ?
C17 N5 C22 120.7(3) . . ?
C17 N5 C19 114.3(3) . . ?
C22 N5 C19 119.6(3) . . ?
C17 N6 C25 120.6(3) . . ?
C17 N6 U1 96.5(2) . . ?
C25 N6 U1 141.3(2) . . ?
C30 N7 C28 121.4(3) . . ?
C30 N7 U1 95.4(2) . . ?
C28 N7 U1 137.7(2) . . ?
C30 N8 C35 117.3(3) . . ?
C30 N8 C32 119.1(3) . . ?
C35 N8 C32 123.5(3) . . ?
C30 N9 C38 123.6(3) . . ?
C30 N9 U1 97.4(2) . . ?
C38 N9 U1 134.5(2) . . ?
N11 N10 U1 165.8(2) . . ?
N10 N11 C40 126.7(3) . . ?
N10 U1 N3 82.24(11) . . ?
N10 U1 N9 78.59(11) . . ?
N3 U1 N9 106.38(10) . . ?
N10 U1 N6 81.39(11) . . ?
N3 U1 N6 115.51(10) . . ?
N9 U1 N6 130.12(10) . . ?
N10 U1 N7 121.47(11) . . ?
N3 U1 N7 137.74(9) . . ?
N9 U1 N7 53.78(9) . . ?
N6 U1 N7 103.13(9) . . ?
N10 U1 N4 127.05(11) . . ?
N3 U1 N4 93.35(10) . . ?
N9 U1 N4 150.21(9) . . ?
N6 U1 N4 53.16(9) . . ?
N7 U1 N4 96.67(10) . . ?
N10 U1 N1 129.26(10) . . ?
N3 U1 N1 53.92(9) . . ?
N9 U1 N1 89.65(10) . . ?
N6 U1 N1 136.78(10) . . ?
N7 U1 N1 86.40(9) . . ?
N4 U1 N1 84.13(9) . . ?
N10 U1 C4 105.53(10) . . ?
N3 U1 C4 26.84(9) . . ?
N9 U1 C4 97.83(10) . . ?
N6 U1 C4 131.57(10) . . ?
N7 U1 C4 112.12(9) . . ?
N4 U1 C4 89.77(10) . . ?
N1 U1 C4 27.13(9) . . ?
N10 U1 C30 100.04(11) . . ?
N3 U1 C30 125.34(10) . . ?
N9 U1 C30 26.78(9) . . ?
N6 U1 C30 118.82(9) . . ?
N7 U1 C30 27.01(9) . . ?
N4 U1 C30 123.65(10) . . ?
N1 U1 C30 88.37(9) . . ?
C4 U1 C30 107.23(9) . . ?
N10 U1 C17 102.68(11) . . ?
N3 U1 C17 102.71(10) . . ?
N9 U1 C17 150.76(9) . . ?
N6 U1 C17 26.59(10) . . ?
N7 U1 C17 104.67(9) . . ?
N4 U1 C17 27.01(10) . . ?
N1 U1 C17 110.20(10) . . ?
C4 U1 C17 109.63(10) . . ?
C30 U1 C17 128.96(9) . . ?

_refine_diff_density_max         3.501
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.100



_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_U(N3)(TIG)3
_database_code_depnum_ccdc_archive 'CCDC 1860828'
_audit_update_record             
;
2018-08-07 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_U(N3)(TIG)3         
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         16 Note
RESPONSE: Beamstop mask was incorrectly setup on instrument
;
# Added during the CSD deposition process: Tuesday 07 August 2018 10:16 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            U(N3)(TIG)3
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H84 N12 U'
_chemical_formula_sum            'C39 H84 N12 U'
_chemical_formula_weight         959.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.0981(2)
_cell_length_b                   13.2024(2)
_cell_length_c                   17.7597(2)
_cell_angle_alpha                96.1010(10)
_cell_angle_beta                 103.8660(10)
_cell_angle_gamma                119.6380(10)
_cell_volume                     2497.88(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    34744
_cell_measurement_theta_min      3.4830
_cell_measurement_theta_max      29.8460

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_F_000             988
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    3.286
_shelx_estimated_absorpt_T_min   0.589
_shelx_estimated_absorpt_T_max   0.639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.35101
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
Olex2 1.2-ac3
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            58226
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.140
_diffrn_reflns_theta_max         29.678
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             12188
_reflns_number_gt                11244
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.45f (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.45f (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45f (Rigaku OD, 2018)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0224P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         12188
_refine_ls_number_parameters     493
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0232
_refine_ls_wR_factor_ref         0.0522
_refine_ls_wR_factor_gt          0.0515
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.008
_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
C1 C 0.1436(2) -0.0519(2) 0.64893(14) 0.0226(5) Uani 1 1 d . . . . .
H1A H 0.1527 -0.0154 0.7030 0.034 Uiso 1 1 calc R U . . .
H1B H 0.0635 -0.1295 0.6260 0.034 Uiso 1 1 calc R U . . .
H1C H 0.1465 0.0023 0.6147 0.034 Uiso 1 1 calc R U . . .
C2 C 0.2491(2) -0.07203(18) 0.65366(13) 0.0154(4) Uani 1 1 d . . . . .
H2 H 0.2420 -0.1314 0.6859 0.019 Uiso 1 1 calc R U . . .
C3 C 0.2376(2) -0.1248(2) 0.56832(14) 0.0227(5) Uani 1 1 d . . . . .
H3A H 0.2358 -0.0712 0.5346 0.034 Uiso 1 1 calc R U . . .
H3B H 0.1604 -0.2049 0.5452 0.034 Uiso 1 1 calc R U . . .
H3C H 0.3093 -0.1320 0.5709 0.034 Uiso 1 1 calc R U . . .
C4 C 0.45605(19) 0.05758(18) 0.75986(12) 0.0119(4) Uani 1 1 d . . . . .
C5 C 0.3814(2) -0.2516(2) 0.70110(15) 0.0250(5) Uani 1 1 d . . . . .
H5A H 0.3967 -0.2782 0.7497 0.037 Uiso 1 1 calc R U . . .
H5B H 0.3920 -0.2946 0.6581 0.037 Uiso 1 1 calc R U . . .
H5C H 0.2961 -0.2691 0.6840 0.037 Uiso 1 1 calc R U . . .
C6 C 0.4738(2) -0.11616(19) 0.71891(14) 0.0174(4) Uani 1 1 d . . . . .
H6 H 0.4536 -0.0944 0.6676 0.021 Uiso 1 1 calc R U . . .
C7 C 0.6075(2) -0.0867(2) 0.73743(16) 0.0271(5) Uani 1 1 d . . . . .
H7A H 0.6658 0.0011 0.7527 0.041 Uiso 1 1 calc R U . . .
H7B H 0.6148 -0.1232 0.6896 0.041 Uiso 1 1 calc R U . . .
H7C H 0.6273 -0.1194 0.7819 0.041 Uiso 1 1 calc R U . . .
C8 C 0.3197(2) -0.1484(2) 0.85420(14) 0.0214(5) Uani 1 1 d . . . . .
H8A H 0.2651 -0.1245 0.8251 0.032 Uiso 1 1 calc R U . . .
H8B H 0.3156 -0.1479 0.9086 0.032 Uiso 1 1 calc R U . . .
H8C H 0.2924 -0.2299 0.8255 0.032 Uiso 1 1 calc R U . . .
C9 C 0.4541(2) -0.05939(19) 0.85939(13) 0.0159(4) Uani 1 1 d . . . . .
H9 H 0.4799 0.0201 0.8937 0.019 Uiso 1 1 calc R U . . .
C10 C 0.5424(2) -0.0941(2) 0.90392(15) 0.0256(5) Uani 1 1 d . . . . .
H10A H 0.5175 -0.1744 0.8746 0.038 Uiso 1 1 calc R U . . .
H10B H 0.5383 -0.0955 0.9582 0.038 Uiso 1 1 calc R U . . .
H10C H 0.6279 -0.0347 0.9075 0.038 Uiso 1 1 calc R U . . .
C11 C 0.7646(2) 0.2928(2) 0.83504(14) 0.0201(5) Uani 1 1 d . . . . .
H11A H 0.7557 0.2522 0.7822 0.030 Uiso 1 1 calc R U . . .
H11B H 0.8443 0.3159 0.8743 0.030 Uiso 1 1 calc R U . . .
H11C H 0.7625 0.3654 0.8315 0.030 Uiso 1 1 calc R U . . .
C12 C 0.65798(19) 0.20754(19) 0.86158(12) 0.0134(4) Uani 1 1 d . . . . .
H12 H 0.6598 0.1329 0.8631 0.016 Uiso 1 1 calc R U . . .
C13 C 0.6772(2) 0.2681(2) 0.94626(13) 0.0195(5) Uani 1 1 d . . . . .
H13A H 0.6813 0.3443 0.9465 0.029 Uiso 1 1 calc R U . . .
H13B H 0.7554 0.2845 0.9837 0.029 Uiso 1 1 calc R U . . .
H13C H 0.6074 0.2144 0.9629 0.029 Uiso 1 1 calc R U . . .
C14 C 0.6048(2) 0.1594(2) 0.59418(14) 0.0203(5) Uani 1 1 d . . . . .
H14A H 0.6243 0.1401 0.6454 0.030 Uiso 1 1 calc R U . . .
H14B H 0.6379 0.1325 0.5581 0.030 Uiso 1 1 calc R U . . .
H14C H 0.5141 0.1181 0.5693 0.030 Uiso 1 1 calc R U . . .
C15 C 0.6645(2) 0.2963(2) 0.60934(13) 0.0180(4) Uani 1 1 d . . . . .
H15 H 0.7572 0.3363 0.6314 0.022 Uiso 1 1 calc R U . . .
C16 C 0.6321(3) 0.3288(2) 0.53088(15) 0.0266(5) Uani 1 1 d . . . . .
H16A H 0.5415 0.2905 0.5083 0.040 Uiso 1 1 calc R U . . .
H16B H 0.6608 0.3001 0.4925 0.040 Uiso 1 1 calc R U . . .
H16C H 0.6731 0.4168 0.5415 0.040 Uiso 1 1 calc R U . . .
C17 C 0.6691(2) 0.45086(19) 0.70623(13) 0.0139(4) Uani 1 1 d . . . . .
C18 C 0.9635(2) 0.5792(2) 0.66606(17) 0.0293(6) Uani 1 1 d . . . . .
H18A H 0.9056 0.5262 0.6124 0.044 Uiso 1 1 calc R U . . .
H18B H 1.0314 0.5651 0.6821 0.044 Uiso 1 1 calc R U . . .
H18C H 0.9982 0.6638 0.6650 0.044 Uiso 1 1 calc R U . . .
C19 C 0.8939(2) 0.5520(2) 0.72627(15) 0.0208(5) Uani 1 1 d . . . . .
H19 H 0.8689 0.4683 0.7298 0.025 Uiso 1 1 calc R U . . .
C20 C 0.9807(2) 0.6362(2) 0.81098(16) 0.0294(6) Uani 1 1 d . . . . .
H20A H 1.0125 0.7204 0.8098 0.044 Uiso 1 1 calc R U . . .
H20B H 1.0509 0.6256 0.8286 0.044 Uiso 1 1 calc R U . . .
H20C H 0.9342 0.6163 0.8486 0.044 Uiso 1 1 calc R U . . .
C21 C 0.8515(3) 0.7689(2) 0.70353(17) 0.0290(6) Uani 1 1 d . . . . .
H21A H 0.8212 0.7811 0.7469 0.043 Uiso 1 1 calc R U . . .
H21B H 0.8485 0.8201 0.6681 0.043 Uiso 1 1 calc R U . . .
H21C H 0.9378 0.7905 0.7267 0.043 Uiso 1 1 calc R U . . .
C22 C 0.7693(2) 0.6364(2) 0.65510(15) 0.0204(5) Uani 1 1 d . . . . .
H22 H 0.8007 0.6293 0.6100 0.024 Uiso 1 1 calc R U . . .
C23 C 0.6357(2) 0.6021(2) 0.61672(15) 0.0253(5) Uani 1 1 d . . . . .
H23A H 0.5839 0.5169 0.5860 0.038 Uiso 1 1 calc R U . . .
H23B H 0.6337 0.6527 0.5806 0.038 Uiso 1 1 calc R U . . .
H23C H 0.6033 0.6145 0.6588 0.038 Uiso 1 1 calc R U . . .
C24 C 0.5492(3) 0.5984(2) 0.80789(15) 0.0249(5) Uani 1 1 d . . . . .
H24A H 0.5194 0.6094 0.7552 0.037 Uiso 1 1 calc R U . . .
H24B H 0.5827 0.6718 0.8500 0.037 Uiso 1 1 calc R U . . .
H24C H 0.4799 0.5299 0.8171 0.037 Uiso 1 1 calc R U . . .
C25 C 0.6516(2) 0.57337(18) 0.81000(13) 0.0162(4) Uani 1 1 d . . . . .
H25 H 0.7206 0.6421 0.7984 0.019 Uiso 1 1 calc R U . . .
C26 C 0.7026(2) 0.5627(2) 0.89331(14) 0.0228(5) Uani 1 1 d . . . . .
H26A H 0.6350 0.4964 0.9054 0.034 Uiso 1 1 calc R U . . .
H26B H 0.7375 0.6386 0.9335 0.034 Uiso 1 1 calc R U . . .
H26C H 0.7681 0.5462 0.8947 0.034 Uiso 1 1 calc R U . . .
C27 C 0.1042(2) 0.2115(2) 0.54532(14) 0.0256(5) Uani 1 1 d . . . . .
H27A H 0.1445 0.1824 0.5173 0.038 Uiso 1 1 calc R U . . .
H27B H 0.0611 0.2399 0.5091 0.038 Uiso 1 1 calc R U . . .
H27C H 0.0437 0.1455 0.5621 0.038 Uiso 1 1 calc R U . . .
C28 C 0.2029(2) 0.3155(2) 0.61936(13) 0.0178(4) Uani 1 1 d . . . . .
H28 H 0.1607 0.3477 0.6448 0.021 Uiso 1 1 calc R U . . .
C29 C 0.2994(2) 0.4171(2) 0.59381(15) 0.0241(5) Uani 1 1 d . . . . .
H29A H 0.3610 0.4848 0.6412 0.036 Uiso 1 1 calc R U . . .
H29B H 0.2577 0.4443 0.5554 0.036 Uiso 1 1 calc R U . . .
H29C H 0.3416 0.3873 0.5684 0.036 Uiso 1 1 calc R U . . .
C30 C 0.25220(19) 0.27941(17) 0.75216(12) 0.0117(4) Uani 1 1 d . . . . .
C31 C -0.0525(2) 0.2474(2) 0.68964(15) 0.0280(6) Uani 1 1 d . . . . .
H31A H -0.0594 0.2913 0.7343 0.042 Uiso 1 1 calc R U . . .
H31B H -0.1359 0.1800 0.6554 0.042 Uiso 1 1 calc R U . . .
H31C H -0.0140 0.3023 0.6579 0.042 Uiso 1 1 calc R U . . .
C32 C 0.0279(2) 0.1986(2) 0.72294(13) 0.0182(5) Uani 1 1 d . . . . .
H32 H 0.0300 0.1536 0.6750 0.022 Uiso 1 1 calc R U . . .
C33 C -0.0361(2) 0.1042(2) 0.76702(16) 0.0262(5) Uani 1 1 d . . . . .
H33A H 0.0184 0.0766 0.7902 0.039 Uiso 1 1 calc R U . . .
H33B H -0.1152 0.0353 0.7289 0.039 Uiso 1 1 calc R U . . .
H33C H -0.0523 0.1406 0.8101 0.039 Uiso 1 1 calc R U . . .
C34 C 0.1269(2) 0.3701(2) 0.89332(14) 0.0235(5) Uani 1 1 d . . . . .
H34A H 0.0417 0.3465 0.8635 0.035 Uiso 1 1 calc R U . . .
H34B H 0.1658 0.4429 0.9374 0.035 Uiso 1 1 calc R U . . .
H34C H 0.1245 0.3043 0.9154 0.035 Uiso 1 1 calc R U . . .
C35 C 0.2031(2) 0.39616(19) 0.83675(13) 0.0164(4) Uani 1 1 d . . . . .
H35 H 0.2892 0.4219 0.8703 0.020 Uiso 1 1 calc R U . . .
C36 C 0.2155(3) 0.5040(2) 0.80533(16) 0.0285(6) Uani 1 1 d . . . . .
H36A H 0.2632 0.5183 0.7684 0.043 Uiso 1 1 calc R U . . .
H36B H 0.2590 0.5761 0.8507 0.043 Uiso 1 1 calc R U . . .
H36C H 0.1323 0.4866 0.7768 0.043 Uiso 1 1 calc R U . . .
C37 C 0.2889(2) 0.1108(2) 0.87850(13) 0.0188(5) Uani 1 1 d . . . . .
H37A H 0.2117 0.0510 0.8342 0.028 Uiso 1 1 calc R U . . .
H37B H 0.2797 0.0938 0.9297 0.028 Uiso 1 1 calc R U . . .
H37C H 0.3585 0.1066 0.8710 0.028 Uiso 1 1 calc R U . . .
C38 C 0.3147(2) 0.23688(19) 0.87946(12) 0.0138(4) Uani 1 1 d . . . . .
H38 H 0.2398 0.2375 0.8825 0.017 Uiso 1 1 calc R U . . .
C39 C 0.4257(2) 0.3292(2) 0.95344(13) 0.0216(5) Uani 1 1 d . . . . .
H39A H 0.4999 0.3290 0.9519 0.032 Uiso 1 1 calc R U . . .
H39B H 0.4078 0.3082 1.0021 0.032 Uiso 1 1 calc R U . . .
H39C H 0.4407 0.4098 0.9540 0.032 Uiso 1 1 calc R U . . .
N1 N 0.36900(17) 0.04342(15) 0.69485(10) 0.0131(3) Uani 1 1 d . . . . .
N2 N 0.46278(18) -0.03963(16) 0.78000(11) 0.0149(4) Uani 1 1 d . . . . .
N3 N 0.53685(16) 0.17249(15) 0.80403(10) 0.0124(3) Uani 1 1 d . . . . .
N4 N 0.62445(17) 0.33553(16) 0.67108(11) 0.0144(4) Uani 1 1 d . . . . .
N5 N 0.77735(17) 0.55143(16) 0.70137(12) 0.0169(4) Uani 1 1 d . . . . .
N6 N 0.60202(17) 0.46131(15) 0.74908(11) 0.0139(4) Uani 1 1 d . . . . .
N7 N 0.26502(17) 0.27758(16) 0.67960(10) 0.0138(4) Uani 1 1 d . . . . .
N8 N 0.15949(17) 0.29086(15) 0.77102(10) 0.0129(3) Uani 1 1 d . . . . .
N9 N 0.33712(17) 0.26945(15) 0.80556(10) 0.0121(3) Uani 1 1 d . . . . .
N10 N 0.35211(19) 0.18330(17) 0.56657(11) 0.0191(4) Uani 1 1 d . . . . .
N11 N 0.3048(2) 0.12972(18) 0.49732(12) 0.0239(4) Uani 1 1 d . . . . .
N12 N 0.2599(3) 0.0785(2) 0.42998(14) 0.0495(8) Uani 1 1 d . . . . .
U1 U 0.43634(2) 0.24866(2) 0.70629(2) 0.00931(3) 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
C1 C2 1.516(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N1 1.473(3) . ?
C2 C3 1.539(3) . ?
C2 H2 1.0000 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 N1 1.334(3) . ?
C4 N3 1.341(3) . ?
C4 N2 1.406(3) . ?
C4 U1 2.893(2) . ?
C5 C6 1.522(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 N2 1.485(3) . ?
C6 C7 1.533(3) . ?
C6 H6 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.531(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.481(3) . ?
C9 C10 1.527(3) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.521(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N3 1.474(3) . ?
C12 C13 1.526(3) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.532(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 N4 1.473(3) . ?
C15 C16 1.527(3) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N6 1.338(3) . ?
C17 N4 1.339(3) . ?
C17 N5 1.415(3) . ?
C17 U1 2.894(2) . ?
C18 C19 1.526(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 N5 1.480(3) . ?
C19 C20 1.538(3) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.527(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 N5 1.489(3) . ?
C22 C23 1.520(3) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.524(3) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 N6 1.468(3) . ?
C25 C26 1.523(3) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.527(3) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 N7 1.469(3) . ?
C28 C29 1.526(3) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 N7 1.338(3) . ?
C30 N9 1.349(3) . ?
C30 N8 1.406(3) . ?
C30 U1 2.913(2) . ?
C31 C32 1.526(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 N8 1.477(3) . ?
C32 C33 1.535(3) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.529(3) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 N8 1.474(3) . ?
C35 C36 1.533(3) . ?
C35 H35 1.0000 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.522(3) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 N9 1.474(3) . ?
C38 C39 1.522(3) . ?
C38 H38 1.0000 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
N1 U1 2.3653(17) . ?
N3 U1 2.5184(17) . ?
N4 U1 2.4235(18) . ?
N6 U1 2.4288(17) . ?
N7 U1 2.4046(17) . ?
N9 U1 2.4941(17) . ?
N10 N11 1.189(3) . ?
N10 U1 2.3260(18) . ?
N11 N12 1.153(3) . ?

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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C1 108.92(17) . . ?
N1 C2 C3 112.19(19) . . ?
C1 C2 C3 109.40(19) . . ?
N1 C2 H2 108.8 . . ?
C1 C2 H2 108.8 . . ?
C3 C2 H2 108.8 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 N3 114.22(18) . . ?
N1 C4 N2 122.83(18) . . ?
N3 C4 N2 122.95(19) . . ?
N1 C4 U1 53.83(10) . . ?
N3 C4 U1 60.44(11) . . ?
N2 C4 U1 175.85(14) . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C6 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 C5 114.96(19) . . ?
N2 C6 C7 112.60(19) . . ?
C5 C6 C7 110.92(19) . . ?
N2 C6 H6 105.9 . . ?
C5 C6 H6 105.9 . . ?
C7 C6 H6 105.9 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 114.79(19) . . ?
N2 C9 C8 111.99(18) . . ?
C10 C9 C8 111.12(19) . . ?
N2 C9 H9 106.1 . . ?
C10 C9 H9 106.1 . . ?
C8 C9 H9 106.1 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 C11 110.64(17) . . ?
N3 C12 C13 111.59(17) . . ?
C11 C12 C13 109.22(18) . . ?
N3 C12 H12 108.4 . . ?
C11 C12 H12 108.4 . . ?
C13 C12 H12 108.4 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N4 C15 C16 113.55(18) . . ?
N4 C15 C14 107.90(18) . . ?
C16 C15 C14 110.70(19) . . ?
N4 C15 H15 108.2 . . ?
C16 C15 H15 108.2 . . ?
C14 C15 H15 108.2 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N6 C17 N4 112.49(19) . . ?
N6 C17 N5 123.00(18) . . ?
N4 C17 N5 124.48(19) . . ?
N6 C17 U1 56.57(11) . . ?
N4 C17 U1 56.34(11) . . ?
N5 C17 U1 175.50(15) . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C19 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N5 C19 C18 114.2(2) . . ?
N5 C19 C20 111.71(19) . . ?
C18 C19 C20 111.1(2) . . ?
N5 C19 H19 106.4 . . ?
C18 C19 H19 106.4 . . ?
C20 C19 H19 106.4 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N5 C22 C23 112.44(19) . . ?
N5 C22 C21 113.9(2) . . ?
C23 C22 C21 110.3(2) . . ?
N5 C22 H22 106.6 . . ?
C23 C22 H22 106.6 . . ?
C21 C22 H22 106.6 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C25 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N6 C25 C26 109.95(17) . . ?
N6 C25 C24 110.23(19) . . ?
C26 C25 C24 109.39(19) . . ?
N6 C25 H25 109.1 . . ?
C26 C25 H25 109.1 . . ?
C24 C25 H25 109.1 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C28 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N7 C28 C29 109.99(19) . . ?
N7 C28 C27 112.67(18) . . ?
C29 C28 C27 109.65(19) . . ?
N7 C28 H28 108.1 . . ?
C29 C28 H28 108.1 . . ?
C27 C28 H28 108.1 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N7 C30 N9 113.46(18) . . ?
N7 C30 N8 123.32(18) . . ?
N9 C30 N8 123.22(18) . . ?
N7 C30 U1 54.80(10) . . ?
N9 C30 U1 58.69(10) . . ?
N8 C30 U1 177.51(14) . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N8 C32 C31 115.57(19) . . ?
N8 C32 C33 112.49(19) . . ?
C31 C32 C33 110.4(2) . . ?
N8 C32 H32 105.8 . . ?
C31 C32 H32 105.8 . . ?
C33 C32 H32 105.8 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C35 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N8 C35 C34 114.79(19) . . ?
N8 C35 C36 111.93(19) . . ?
C34 C35 C36 110.69(19) . . ?
N8 C35 H35 106.3 . . ?
C34 C35 H35 106.3 . . ?
C36 C35 H35 106.3 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N9 C38 C39 110.49(18) . . ?
N9 C38 C37 111.31(17) . . ?
C39 C38 C37 110.08(18) . . ?
N9 C38 H38 108.3 . . ?
C39 C38 H38 108.3 . . ?
C37 C38 H38 108.3 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C4 N1 C2 123.32(17) . . ?
C4 N1 U1 99.09(12) . . ?
C2 N1 U1 134.00(13) . . ?
C4 N2 C9 117.17(17) . . ?
C4 N2 C6 117.31(17) . . ?
C9 N2 C6 125.50(17) . . ?
C4 N3 C12 120.05(17) . . ?
C4 N3 U1 91.96(12) . . ?
C12 N3 U1 142.04(13) . . ?
C17 N4 C15 124.78(18) . . ?
C17 N4 U1 96.29(13) . . ?
C15 N4 U1 135.41(14) . . ?
C17 N5 C19 116.90(17) . . ?
C17 N5 C22 121.39(18) . . ?
C19 N5 C22 120.03(18) . . ?
C17 N6 C25 121.63(18) . . ?
C17 N6 U1 96.07(12) . . ?
C25 N6 U1 141.06(14) . . ?
C30 N7 C28 121.82(17) . . ?
C30 N7 U1 98.16(12) . . ?
C28 N7 U1 138.24(14) . . ?
C30 N8 C35 116.55(17) . . ?
C30 N8 C32 117.77(16) . . ?
C35 N8 C32 125.66(17) . . ?
C30 N9 C38 119.23(17) . . ?
C30 N9 U1 93.79(12) . . ?
C38 N9 U1 142.46(13) . . ?
N11 N10 U1 167.79(17) . . ?
N12 N11 N10 179.3(4) . . ?
N10 U1 N1 83.22(6) . . ?
N10 U1 N7 77.92(6) . . ?
N1 U1 N7 112.07(6) . . ?
N10 U1 N4 79.10(7) . . ?
N1 U1 N4 105.37(6) . . ?
N7 U1 N4 132.81(6) . . ?
N10 U1 N6 110.12(7) . . ?
N1 U1 N6 150.45(6) . . ?
N7 U1 N6 96.75(6) . . ?
N4 U1 N6 54.59(6) . . ?
N10 U1 N9 129.05(6) . . ?
N1 U1 N9 97.35(6) . . ?
N7 U1 N9 54.55(6) . . ?
N4 U1 N9 146.14(6) . . ?
N6 U1 N9 94.06(6) . . ?
N10 U1 N3 129.71(6) . . ?
N1 U1 N3 54.66(6) . . ?
N7 U1 N3 138.90(6) . . ?
N4 U1 N3 86.46(6) . . ?
N6 U1 N3 99.17(6) . . ?
N9 U1 N3 86.62(6) . . ?
N10 U1 C4 106.46(6) . . ?
N1 U1 C4 27.09(6) . . ?
N7 U1 C4 129.94(6) . . ?
N4 U1 C4 95.99(6) . . ?
N6 U1 C4 125.41(6) . . ?
N9 U1 C4 92.98(6) . . ?
N3 U1 C4 27.59(6) . . ?
N10 U1 C17 93.33(7) . . ?
N1 U1 C17 130.73(6) . . ?
N7 U1 C17 115.13(6) . . ?
N4 U1 C17 27.37(6) . . ?
N6 U1 C17 27.36(6) . . ?
N9 U1 C17 121.01(6) . . ?
N3 U1 C17 95.15(6) . . ?
C4 U1 C17 114.33(6) . . ?
N10 U1 C30 103.27(6) . . ?
N1 U1 C30 105.96(6) . . ?
N7 U1 C30 27.04(6) . . ?
N4 U1 C30 148.63(6) . . ?
N6 U1 C30 96.68(6) . . ?
N9 U1 C30 27.52(6) . . ?
N3 U1 C30 113.07(6) . . ?
C4 U1 C30 112.73(6) . . ?
C17 U1 C30 122.48(6) . . ?

_refine_diff_density_max         0.798
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.097



_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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. 
# 
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data_U(TIG)3
_database_code_depnum_ccdc_archive 'CCDC 1860831'
_audit_update_record             
;
2018-08-07 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_U(TIG)3             
;
PROBLEM: Check Calcd Resid. Dens.  1.60A   From N1              2.97 eA-3
RESPONSE: Due to unresolved minor twin component
;
_vrf_PLAT971_U(TIG)3_2           
;
PROBLEM: Check Calcd Resid. Dens.  2.31A   From C8              2.81 eA-3
RESPONSE: Due to unresolved minor twin component
;
# Added during the CSD deposition process: Tuesday 07 August 2018 10:16 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            U(TIG)3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H84 N9 U'
_chemical_formula_weight         917.18

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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.2890(11)
_cell_length_b                   19.9565(16)
_cell_length_c                   18.7099(14)
_cell_angle_alpha                90
_cell_angle_beta                 110.091(3)
_cell_angle_gamma                90
_cell_volume                     4659.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9987
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      25.34

_exptl_crystal_description       Block
_exptl_crystal_colour            Blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_F_000             1892
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    3.517
_shelx_estimated_absorpt_T_min   0.844
_shelx_estimated_absorpt_T_max   0.844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            246388
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.544
_diffrn_reflns_theta_max         25.407
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8549
_reflns_number_gt                7173
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury 3.10'
_computing_publication_material  WinGX
_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)+(0.0155P)²+12.2771P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8549
_refine_ls_number_parameters     466
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0295
_refine_ls_wR_factor_ref         0.0622
_refine_ls_wR_factor_gt          0.0589
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_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
C1 C 0.5037(3) 0.2292(2) 0.7067(3) 0.0420(10) Uani 1 1 d . . . . .
H1A H 0.4362 0.2283 0.7169 0.063 Uiso 1 1 calc R U . . .
H1B H 0.5358 0.1844 0.7146 0.063 Uiso 1 1 calc R U . . .
H1C H 0.4898 0.2432 0.6539 0.063 Uiso 1 1 calc R U . . .
C2 C 0.5807(3) 0.2788(2) 0.7606(2) 0.0392(10) Uani 1 1 d . . . . .
H2 H 0.6491 0.2798 0.7495 0.047 Uiso 1 1 calc R U . . .
C3 C 0.6045(4) 0.2569(3) 0.8431(3) 0.0614(14) Uani 1 1 d . . . . .
H3A H 0.6536 0.2891 0.8773 0.092 Uiso 1 1 calc R U . . .
H3B H 0.6376 0.2124 0.8507 0.092 Uiso 1 1 calc R U . . .
H3C H 0.5375 0.2553 0.8540 0.092 Uiso 1 1 calc R U . . .
C4 C 0.5646(3) 0.39324(18) 0.7111(2) 0.0251(8) Uani 1 1 d . . . . .
C5 C 0.6633(4) 0.3233(2) 0.5882(3) 0.0448(11) Uani 1 1 d . . . . .
H5A H 0.7323 0.3018 0.6152 0.067 Uiso 1 1 calc R U . . .
H5B H 0.6530 0.3263 0.5339 0.067 Uiso 1 1 calc R U . . .
H5C H 0.6053 0.2966 0.5951 0.067 Uiso 1 1 calc R U . . .
C6 C 0.6622(3) 0.3934(2) 0.6202(2) 0.0315(9) Uani 1 1 d . . . . .
H6 H 0.5919 0.4139 0.5896 0.038 Uiso 1 1 calc R U . . .
C7 C 0.7488(3) 0.4366(2) 0.6071(3) 0.0437(11) Uani 1 1 d . . . . .
H7A H 0.7446 0.4822 0.6253 0.066 Uiso 1 1 calc R U . . .
H7B H 0.7380 0.4379 0.5526 0.066 Uiso 1 1 calc R U . . .
H7C H 0.8194 0.4176 0.6349 0.066 Uiso 1 1 calc R U . . .
C8 C 0.8462(3) 0.3474(3) 0.7738(3) 0.0542(13) Uani 1 1 d . . . . .
H8A H 0.8192 0.3073 0.7916 0.081 Uiso 1 1 calc R U . . .
H8B H 0.9148 0.3607 0.8117 0.081 Uiso 1 1 calc R U . . .
H8C H 0.8564 0.3375 0.7254 0.081 Uiso 1 1 calc R U . . .
C9 C 0.7657(3) 0.4041(2) 0.7624(2) 0.0407(10) Uani 1 1 d . . . . .
H9 H 0.7986 0.4443 0.7471 0.049 Uiso 1 1 calc R U . . .
C10 C 0.7486(4) 0.4223(3) 0.8348(3) 0.0656(15) Uani 1 1 d . . . . .
H10A H 0.6987 0.4601 0.8257 0.098 Uiso 1 1 calc R U . . .
H10B H 0.8173 0.4349 0.8732 0.098 Uiso 1 1 calc R U . . .
H10C H 0.7187 0.3838 0.8531 0.098 Uiso 1 1 calc R U . . .
C11 C 0.4548(3) 0.5295(2) 0.5850(2) 0.0374(10) Uani 1 1 d . . . . .
H11A H 0.4582 0.4957 0.5479 0.056 Uiso 1 1 calc R U . . .
H11B H 0.4796 0.5727 0.5724 0.056 Uiso 1 1 calc R U . . .
H11C H 0.3807 0.5339 0.5836 0.056 Uiso 1 1 calc R U . . .
C12 C 0.5261(3) 0.50811(18) 0.6644(2) 0.0310(9) Uani 1 1 d . . . . .
H12 H 0.6020 0.5057 0.6661 0.037 Uiso 1 1 calc R U . . .
C13 C 0.5180(4) 0.5592(2) 0.7228(3) 0.0482(11) Uani 1 1 d . . . . .
H13A H 0.4444 0.5603 0.7230 0.072 Uiso 1 1 calc R U . . .
H13B H 0.5376 0.6036 0.7095 0.072 Uiso 1 1 calc R U . . .
H13C H 0.5669 0.5465 0.7734 0.072 Uiso 1 1 calc R U . . .
C14 C 0.1912(4) 0.3979(2) 0.4607(2) 0.0398(10) Uani 1 1 d . . . . .
H14A H 0.1167 0.4003 0.4590 0.060 Uiso 1 1 calc R U . . .
H14B H 0.1929 0.3982 0.4088 0.060 Uiso 1 1 calc R U . . .
H14C H 0.2311 0.4365 0.4887 0.060 Uiso 1 1 calc R U . . .
C15 C 0.2423(3) 0.33352(19) 0.50064(19) 0.0281(8) Uani 1 1 d . . . . .
H15 H 0.1996 0.2944 0.4729 0.034 Uiso 1 1 calc R U . . .
C16 C 0.3570(3) 0.3273(2) 0.5010(2) 0.0390(10) Uani 1 1 d . . . . .
H16A H 0.4002 0.3643 0.5304 0.059 Uiso 1 1 calc R U . . .
H16B H 0.3568 0.3290 0.4487 0.059 Uiso 1 1 calc R U . . .
H16C H 0.3875 0.2846 0.5244 0.059 Uiso 1 1 calc R U . . .
C17 C 0.1922(3) 0.28645(17) 0.6050(2) 0.0242(8) Uani 1 1 d . . . . .
C18 C 0.2442(4) 0.1563(2) 0.5785(3) 0.0481(11) Uani 1 1 d . . . . .
H18A H 0.2960 0.1906 0.5767 0.072 Uiso 1 1 calc R U . . .
H18B H 0.2600 0.1143 0.5573 0.072 Uiso 1 1 calc R U . . .
H18C H 0.2492 0.1490 0.6314 0.072 Uiso 1 1 calc R U . . .
C19 C 0.1321(4) 0.1793(2) 0.5322(3) 0.0460(11) Uani 1 1 d . . . . .
H19 H 0.1288 0.1833 0.4782 0.055 Uiso 1 1 calc R U . . .
C20 C 0.0515(4) 0.1271(2) 0.5340(4) 0.0713(17) Uani 1 1 d . . . . .
H20A H 0.0534 0.1211 0.5864 0.107 Uiso 1 1 calc R U . . .
H20B H 0.0688 0.0846 0.5147 0.107 Uiso 1 1 calc R U . . .
H20C H -0.0203 0.1416 0.5019 0.107 Uiso 1 1 calc R U . . .
C21 C -0.0253(4) 0.2686(3) 0.4237(2) 0.0506(12) Uani 1 1 d . . . . .
H21A H 0.0339 0.2770 0.4049 0.076 Uiso 1 1 calc R U . . .
H21B H -0.0856 0.2980 0.3972 0.076 Uiso 1 1 calc R U . . .
H21C H -0.0479 0.2217 0.4142 0.076 Uiso 1 1 calc R U . . .
C22 C 0.0119(3) 0.2826(2) 0.5092(2) 0.0326(9) Uani 1 1 d . . . . .
H22 H 0.0312 0.3312 0.5156 0.039 Uiso 1 1 calc R U . . .
C23 C -0.0812(3) 0.2734(2) 0.5381(3) 0.0473(11) Uani 1 1 d . . . . .
H23A H -0.1074 0.2271 0.5288 0.071 Uiso 1 1 calc R U . . .
H23B H -0.1391 0.3043 0.5113 0.071 Uiso 1 1 calc R U . . .
H23C H -0.0569 0.2827 0.5928 0.071 Uiso 1 1 calc R U . . .
C24 C 0.1032(3) 0.2942(2) 0.7542(2) 0.0438(11) Uani 1 1 d . . . . .
H24A H 0.1561 0.3231 0.7906 0.066 Uiso 1 1 calc R U . . .
H24B H 0.0633 0.2691 0.7808 0.066 Uiso 1 1 calc R U . . .
H24C H 0.0534 0.3218 0.7143 0.066 Uiso 1 1 calc R U . . .
C25 C 0.1604(3) 0.2454(2) 0.7185(2) 0.0317(9) Uani 1 1 d . . . . .
H25 H 0.1061 0.2169 0.6803 0.038 Uiso 1 1 calc R U . . .
C26 C 0.2355(4) 0.2008(3) 0.7797(3) 0.0513(12) Uani 1 1 d . . . . .
H26A H 0.2709 0.1690 0.7562 0.077 Uiso 1 1 calc R U . . .
H26B H 0.1943 0.1762 0.8057 0.077 Uiso 1 1 calc R U . . .
H26C H 0.2896 0.2286 0.8167 0.077 Uiso 1 1 calc R U . . .
C27 C 0.1629(3) 0.5584(2) 0.6000(2) 0.0414(10) Uani 1 1 d . . . . .
H27A H 0.2138 0.5934 0.6264 0.062 Uiso 1 1 calc R U . . .
H27B H 0.0977 0.5792 0.5651 0.062 Uiso 1 1 calc R U . . .
H27C H 0.1952 0.5299 0.5710 0.062 Uiso 1 1 calc R U . . .
C28 C 0.1349(3) 0.51604(19) 0.6579(2) 0.0298(9) Uani 1 1 d . . . . .
H28 H 0.1040 0.5456 0.6883 0.036 Uiso 1 1 calc R U . . .
C29 C 0.0534(3) 0.4623(2) 0.6184(2) 0.0369(10) Uani 1 1 d . . . . .
H29A H 0.0832 0.4333 0.5884 0.055 Uiso 1 1 calc R U . . .
H29B H -0.0122 0.4837 0.5848 0.055 Uiso 1 1 calc R U . . .
H29C H 0.0366 0.4354 0.6567 0.055 Uiso 1 1 calc R U . . .
C30 C 0.2533(3) 0.48116(18) 0.7847(2) 0.0241(8) Uani 1 1 d . . . . .
C31 C 0.3228(4) 0.6295(2) 0.8756(3) 0.0456(11) Uani 1 1 d . . . . .
H31A H 0.3055 0.6324 0.9223 0.068 Uiso 1 1 calc R U . . .
H31B H 0.3383 0.6743 0.8608 0.068 Uiso 1 1 calc R U . . .
H31C H 0.3857 0.6007 0.8844 0.068 Uiso 1 1 calc R U . . .
C32 C 0.2275(3) 0.59964(19) 0.8118(2) 0.0364(10) Uani 1 1 d . . . . .
H32 H 0.2469 0.6021 0.7648 0.044 Uiso 1 1 calc R U . . .
C33 C 0.1284(4) 0.6442(2) 0.7964(3) 0.0491(12) Uani 1 1 d . . . . .
H33A H 0.0684 0.6247 0.7551 0.074 Uiso 1 1 calc R U . . .
H33B H 0.1440 0.6891 0.7817 0.074 Uiso 1 1 calc R U . . .
H33C H 0.1096 0.6472 0.8425 0.074 Uiso 1 1 calc R U . . .
C34 C 0.0345(3) 0.4995(2) 0.8322(3) 0.0478(11) Uani 1 1 d . . . . .
H34A H 0.0063 0.5452 0.8226 0.072 Uiso 1 1 calc R U . . .
H34B H 0.0009 0.4758 0.8640 0.072 Uiso 1 1 calc R U . . .
H34C H 0.0187 0.4758 0.7837 0.072 Uiso 1 1 calc R U . . .
C35 C 0.1555(3) 0.5019(2) 0.8730(2) 0.0334(9) Uani 1 1 d . . . . .
H35 H 0.1791 0.4542 0.8840 0.040 Uiso 1 1 calc R U . . .
C36 C 0.1833(3) 0.5360(2) 0.9504(2) 0.0377(10) Uani 1 1 d . . . . .
H36A H 0.2606 0.5324 0.9779 0.057 Uiso 1 1 calc R U . . .
H36B H 0.1443 0.5142 0.9799 0.057 Uiso 1 1 calc R U . . .
H36C H 0.1629 0.5834 0.9431 0.057 Uiso 1 1 calc R U . . .
C37 C 0.4966(3) 0.4522(2) 0.9081(2) 0.0418(10) Uani 1 1 d . . . . .
H37A H 0.5254 0.4202 0.8804 0.063 Uiso 1 1 calc R U . . .
H37B H 0.5417 0.4523 0.9620 0.063 Uiso 1 1 calc R U . . .
H37C H 0.4959 0.4971 0.8869 0.063 Uiso 1 1 calc R U . . .
C38 C 0.3831(3) 0.4321(2) 0.9006(2) 0.0321(9) Uani 1 1 d . . . . .
H38 H 0.3532 0.4660 0.9271 0.039 Uiso 1 1 calc R U . . .
C39 C 0.3815(4) 0.3635(2) 0.9359(2) 0.0482(12) Uani 1 1 d . . . . .
H39A H 0.3077 0.3517 0.9305 0.072 Uiso 1 1 calc R U . . .
H39B H 0.4256 0.3647 0.9899 0.072 Uiso 1 1 calc R U . . .
H39C H 0.4103 0.3299 0.9098 0.072 Uiso 1 1 calc R U . . .
N1 N 0.5330(2) 0.34591(16) 0.74878(17) 0.0292(7) Uani 1 1 d . . . . .
N2 N 0.6651(2) 0.39114(16) 0.70003(17) 0.0307(7) Uani 1 1 d . . . . .
N3 N 0.4935(2) 0.44227(14) 0.68296(17) 0.0257(7) Uani 1 1 d . . . . .
N4 N 0.2439(2) 0.33305(15) 0.57943(16) 0.0264(7) Uani 1 1 d . . . . .
N5 N 0.1082(2) 0.24549(15) 0.55575(17) 0.0267(7) Uani 1 1 d . . . . .
N6 N 0.2222(2) 0.28305(15) 0.68056(16) 0.0264(7) Uani 1 1 d . . . . .
N7 N 0.2327(2) 0.48391(15) 0.70932(16) 0.0257(7) Uani 1 1 d . . . . .
N8 N 0.2126(2) 0.52819(15) 0.82391(17) 0.0270(7) Uani 1 1 d . . . . .
N9 N 0.3155(2) 0.42976(15) 0.81976(16) 0.0272(7) Uani 1 1 d . . . . .
U1 U 0.34201(2) 0.38440(2) 0.70430(2) 0.02250(5) 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
C1 C2 1.527(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N1 1.466(5) . ?
C2 C3 1.529(6) . ?
C2 H2 1.0000 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 N1 1.330(5) . ?
C4 N3 1.336(4) . ?
C4 N2 1.422(4) . ?
C4 U1 2.922(3) . ?
C5 C6 1.523(6) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 N2 1.482(5) . ?
C6 C7 1.525(5) . ?
C6 H6 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.521(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.464(5) . ?
C9 C10 1.494(6) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.523(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N3 1.462(5) . ?
C12 C13 1.525(6) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.523(5) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 N4 1.467(4) . ?
C15 C16 1.526(5) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N6 1.332(4) . ?
C17 N4 1.338(4) . ?
C17 N5 1.435(4) . ?
C17 U1 2.948(3) . ?
C18 C19 1.515(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 N5 1.462(5) . ?
C19 C20 1.501(6) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.529(5) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 N5 1.476(5) . ?
C22 C23 1.521(6) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.524(6) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 N6 1.465(4) . ?
C25 C26 1.521(6) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.518(5) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 N7 1.471(4) . ?
C28 C29 1.523(5) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 N9 1.339(5) . ?
C30 N7 1.343(4) . ?
C30 N8 1.408(4) . ?
C30 U1 2.933(3) . ?
C31 C32 1.531(6) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 N8 1.468(5) . ?
C32 C33 1.531(6) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.526(6) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 N8 1.475(5) . ?
C35 C36 1.526(5) . ?
C35 H35 1.0000 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.520(5) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 N9 1.470(4) . ?
C38 C39 1.523(6) . ?
C38 H38 1.0000 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
N1 U1 2.504(3) . ?
N3 U1 2.469(3) . ?
N4 U1 2.473(3) . ?
N6 U1 2.517(3) . ?
N7 U1 2.481(3) . ?
N9 U1 2.477(3) . ?

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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C1 109.6(3) . . ?
N1 C2 C3 110.0(4) . . ?
C1 C2 C3 110.0(4) . . ?
N1 C2 H2 109.1 . . ?
C1 C2 H2 109.1 . . ?
C3 C2 H2 109.1 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 N3 114.8(3) . . ?
N1 C4 N2 122.7(3) . . ?
N3 C4 N2 122.5(3) . . ?
N1 C4 U1 58.72(18) . . ?
N3 C4 U1 57.23(17) . . ?
N2 C4 U1 168.5(2) . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C6 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 C5 111.6(3) . . ?
N2 C6 C7 114.8(3) . . ?
C5 C6 C7 110.3(3) . . ?
N2 C6 H6 106.6 . . ?
C5 C6 H6 106.6 . . ?
C7 C6 H6 106.6 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 112.6(3) . . ?
N2 C9 C8 112.7(4) . . ?
C10 C9 C8 111.8(4) . . ?
N2 C9 H9 106.4 . . ?
C10 C9 H9 106.4 . . ?
C8 C9 H9 106.4 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 C11 110.4(3) . . ?
N3 C12 C13 109.4(3) . . ?
C11 C12 C13 109.8(3) . . ?
N3 C12 H12 109.1 . . ?
C11 C12 H12 109.1 . . ?
C13 C12 H12 109.1 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N4 C15 C14 110.4(3) . . ?
N4 C15 C16 108.9(3) . . ?
C14 C15 C16 110.3(3) . . ?
N4 C15 H15 109.1 . . ?
C14 C15 H15 109.1 . . ?
C16 C15 H15 109.1 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N6 C17 N4 114.3(3) . . ?
N6 C17 N5 122.4(3) . . ?
N4 C17 N5 123.2(3) . . ?
N6 C17 U1 58.27(18) . . ?
N4 C17 U1 56.39(17) . . ?
N5 C17 U1 172.2(2) . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C19 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N5 C19 C20 112.9(4) . . ?
N5 C19 C18 112.0(3) . . ?
C20 C19 C18 110.3(4) . . ?
N5 C19 H19 107.1 . . ?
C20 C19 H19 107.1 . . ?
C18 C19 H19 107.1 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N5 C22 C23 112.1(3) . . ?
N5 C22 C21 115.4(3) . . ?
C23 C22 C21 109.9(3) . . ?
N5 C22 H22 106.3 . . ?
C23 C22 H22 106.3 . . ?
C21 C22 H22 106.3 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C25 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N6 C25 C26 109.4(3) . . ?
N6 C25 C24 109.4(3) . . ?
C26 C25 C24 109.9(3) . . ?
N6 C25 H25 109.4 . . ?
C26 C25 H25 109.4 . . ?
C24 C25 H25 109.4 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C28 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N7 C28 C27 109.4(3) . . ?
N7 C28 C29 109.4(3) . . ?
C27 C28 C29 110.7(3) . . ?
N7 C28 H28 109.1 . . ?
C27 C28 H28 109.1 . . ?
C29 C28 H28 109.1 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N9 C30 N7 114.5(3) . . ?
N9 C30 N8 122.6(3) . . ?
N7 C30 N8 122.9(3) . . ?
N9 C30 U1 57.15(17) . . ?
N7 C30 U1 57.38(17) . . ?
N8 C30 U1 179.0(2) . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N8 C32 C31 112.1(3) . . ?
N8 C32 C33 116.1(4) . . ?
C31 C32 C33 110.4(3) . . ?
N8 C32 H32 105.8 . . ?
C31 C32 H32 105.8 . . ?
C33 C32 H32 105.8 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C35 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N8 C35 C36 115.1(3) . . ?
N8 C35 C34 112.2(3) . . ?
C36 C35 C34 111.1(3) . . ?
N8 C35 H35 105.9 . . ?
C36 C35 H35 105.9 . . ?
C34 C35 H35 105.9 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N9 C38 C37 109.9(3) . . ?
N9 C38 C39 108.9(3) . . ?
C37 C38 C39 111.0(3) . . ?
N9 C38 H38 109.0 . . ?
C37 C38 H38 109.0 . . ?
C39 C38 H38 109.0 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C4 N1 C2 122.0(3) . . ?
C4 N1 U1 94.3(2) . . ?
C2 N1 U1 131.8(2) . . ?
C4 N2 C9 121.7(3) . . ?
C4 N2 C6 116.5(3) . . ?
C9 N2 C6 119.9(3) . . ?
C4 N3 C12 121.6(3) . . ?
C4 N3 U1 95.7(2) . . ?
C12 N3 U1 141.5(2) . . ?
C17 N4 C15 122.1(3) . . ?
C17 N4 U1 96.8(2) . . ?
C15 N4 U1 140.1(2) . . ?
C17 N5 C19 120.5(3) . . ?
C17 N5 C22 114.8(3) . . ?
C19 N5 C22 120.6(3) . . ?
C17 N6 C25 121.8(3) . . ?
C17 N6 U1 95.0(2) . . ?
C25 N6 U1 138.8(2) . . ?
C30 N7 C28 121.4(3) . . ?
C30 N7 U1 95.5(2) . . ?
C28 N7 U1 136.1(2) . . ?
C30 N8 C32 118.1(3) . . ?
C30 N8 C35 117.3(3) . . ?
C32 N8 C35 124.5(3) . . ?
C30 N9 C38 122.4(3) . . ?
C30 N9 U1 95.8(2) . . ?
C38 N9 U1 133.5(2) . . ?
N3 U1 N4 103.63(10) . . ?
N3 U1 N9 109.77(10) . . ?
N4 U1 N9 142.06(10) . . ?
N3 U1 N7 98.77(9) . . ?
N4 U1 N7 104.00(10) . . ?
N9 U1 N7 54.11(10) . . ?
N3 U1 N1 53.69(10) . . ?
N4 U1 N1 109.39(10) . . ?
N9 U1 N1 104.71(10) . . ?
N7 U1 N1 140.59(10) . . ?
N3 U1 N6 148.05(10) . . ?
N4 U1 N6 53.42(9) . . ?
N9 U1 N6 100.18(10) . . ?
N7 U1 N6 107.86(10) . . ?
N1 U1 N6 108.62(10) . . ?
N3 U1 C4 27.07(10) . . ?
N4 U1 C4 105.29(10) . . ?
N9 U1 C4 112.64(10) . . ?
N7 U1 C4 123.18(10) . . ?
N1 U1 C4 26.99(10) . . ?
N6 U1 C4 128.72(10) . . ?
N3 U1 C30 105.58(10) . . ?
N4 U1 C30 125.68(10) . . ?
N9 U1 C30 27.00(10) . . ?
N7 U1 C30 27.11(10) . . ?
N1 U1 C30 124.84(10) . . ?
N6 U1 C30 106.17(10) . . ?
C4 U1 C30 121.12(10) . . ?
N3 U1 C17 128.29(10) . . ?
N4 U1 C17 26.79(9) . . ?
N9 U1 C17 121.62(10) . . ?
N7 U1 C17 106.09(10) . . ?
N1 U1 C17 113.18(10) . . ?
N6 U1 C17 26.75(9) . . ?
C4 U1 C17 121.45(10) . . ?
C30 U1 C17 117.17(9) . . ?

_refine_diff_density_max         3.202
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.092


_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_UCl(TIG)3
_database_code_depnum_ccdc_archive 'CCDC 1860829'
_audit_update_record             
;
2018-08-07 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT412_UCl(TIG)3           
;
PROBLEM: Short Intra XH3 .. XHn     H37C     ..H35A             1.76 Ang.
RESPONSE: Due to modeled disorder of isopropyl moiety
;
_vrf_PLAT910_UCl(TIG)3           
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         16 Note
RESPONSE: Beamstop mask was incorrectly setup on instrument
;
# Added during the CSD deposition process: Tuesday 07 August 2018 10:16 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            UCl(TIG)3
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H84 Cl N9 U, C6 H14, C3 H7'
_chemical_formula_sum            'C48 H105 Cl N9 U'
_chemical_formula_weight         1081.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   11.6454(4)
_cell_length_b                   37.8373(10)
_cell_length_c                   13.3431(4)
_cell_angle_alpha                90
_cell_angle_beta                 109.795(3)
_cell_angle_gamma                90
_cell_volume                     5532.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    28552
_cell_measurement_theta_min      3.1580
_cell_measurement_theta_max      29.0340

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_F_000             2260
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    3.020
_shelx_estimated_absorpt_T_min   0.378
_shelx_estimated_absorpt_T_max   0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.49619
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
Olex2 1.2-ac3
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            61124
_diffrn_reflns_av_unetI/netI     0.0666
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.048
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        26.372
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11297
_reflns_number_gt                8807
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.45f (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.45f (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45f (Rigaku OD, 2018)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_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)+(0.0365P)²+4.7613P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11297
_refine_ls_number_parameters     554
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_ref         0.0880
_refine_ls_wR_factor_gt          0.0830
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.006
_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
C1 C 0.6534(5) 0.54041(11) 0.5504(4) 0.0307(12) Uani 1 1 d . . . . .
H1A H 0.7392 0.5456 0.5612 0.046 Uiso 1 1 calc R U . . .
H1B H 0.6286 0.5191 0.5067 0.046 Uiso 1 1 calc R U . . .
H1C H 0.6432 0.5366 0.6195 0.046 Uiso 1 1 calc R U . . .
C2 C 0.5748(4) 0.57125(11) 0.4942(3) 0.0200(10) Uani 1 1 d . . . . .
H2 H 0.5918 0.5763 0.4271 0.024 Uiso 1 1 calc R U . . .
C3 C 0.4409(5) 0.56181(12) 0.4658(4) 0.0301(11) Uani 1 1 d . . . . .
H3A H 0.4223 0.5578 0.5312 0.045 Uiso 1 1 calc R U . . .
H3B H 0.4235 0.5403 0.4224 0.045 Uiso 1 1 calc R U . . .
H3C H 0.3906 0.5813 0.4255 0.045 Uiso 1 1 calc R U . . .
C4 C 0.6099(4) 0.63499(11) 0.5198(3) 0.0162(9) Uani 1 1 d . . . . .
C5 C 0.7178(5) 0.60625(14) 0.3063(4) 0.0347(12) Uani 1 1 d . . . . .
H5A H 0.6922 0.5831 0.3241 0.052 Uiso 1 1 calc R U . . .
H5B H 0.7953 0.6038 0.2933 0.052 Uiso 1 1 calc R U . . .
H5C H 0.6554 0.6154 0.2421 0.052 Uiso 1 1 calc R U . . .
C6 C 0.7340(4) 0.63186(12) 0.3990(4) 0.0249(10) Uani 1 1 d . . . . .
H6 H 0.7636 0.6547 0.3791 0.030 Uiso 1 1 calc R U . . .
C7 C 0.8338(4) 0.61843(13) 0.4986(4) 0.0308(11) Uani 1 1 d . . . . .
H7A H 0.8429 0.6348 0.5577 0.046 Uiso 1 1 calc R U . . .
H7B H 0.9111 0.6168 0.4848 0.046 Uiso 1 1 calc R U . . .
H7C H 0.8114 0.5950 0.5173 0.046 Uiso 1 1 calc R U . . .
C8 C 0.4307(5) 0.63917(13) 0.2555(4) 0.0326(12) Uani 1 1 d . . . . .
H8A H 0.4708 0.6281 0.2097 0.049 Uiso 1 1 calc R U . . .
H8B H 0.3646 0.6545 0.2124 0.049 Uiso 1 1 calc R U . . .
H8C H 0.3970 0.6208 0.2893 0.049 Uiso 1 1 calc R U . . .
C9 C 0.5241(4) 0.66124(11) 0.3417(3) 0.0223(10) Uani 1 1 d . . . . .
H9 H 0.4779 0.6731 0.3833 0.027 Uiso 1 1 calc R U . . .
C10 C 0.5745(5) 0.69102(12) 0.2897(4) 0.0293(11) Uani 1 1 d . . . . .
H10A H 0.6320 0.7055 0.3452 0.044 Uiso 1 1 calc R U . . .
H10B H 0.5070 0.7059 0.2463 0.044 Uiso 1 1 calc R U . . .
H10C H 0.6166 0.6807 0.2443 0.044 Uiso 1 1 calc R U . . .
C11 C 0.7626(4) 0.70579(12) 0.5782(4) 0.0239(10) Uani 1 1 d . . . . .
H11A H 0.7806 0.6931 0.5212 0.029 Uiso 1 1 calc R U . . .
H11B H 0.8181 0.6977 0.6475 0.029 Uiso 1 1 calc R U . . .
H11C H 0.7736 0.7312 0.5709 0.029 Uiso 1 1 calc R U . . .
C12 C 0.6309(4) 0.69847(10) 0.5706(3) 0.0174(9) Uani 1 1 d . . . . .
H12 H 0.5765 0.7057 0.4979 0.021 Uiso 1 1 calc R U . . .
C13 C 0.5969(4) 0.72072(11) 0.6516(3) 0.0191(9) Uani 1 1 d . . . . .
H13A H 0.5122 0.7158 0.6456 0.029 Uiso 1 1 calc R U . . .
H13B H 0.6056 0.7458 0.6377 0.029 Uiso 1 1 calc R U . . .
H13C H 0.6511 0.7148 0.7236 0.029 Uiso 1 1 calc R U . . .
C14 C 0.6428(5) 0.64113(13) 1.0203(3) 0.0329(12) Uani 1 1 d . . . . .
H14A H 0.5883 0.6207 1.0100 0.049 Uiso 1 1 calc R U . . .
H14B H 0.6710 0.6481 1.0955 0.049 Uiso 1 1 calc R U . . .
H14C H 0.7132 0.6348 0.9995 0.049 Uiso 1 1 calc R U . . .
C15 C 0.5745(4) 0.67170(12) 0.9522(3) 0.0226(10) Uani 1 1 d . . . . .
H15 H 0.5014 0.6774 0.9725 0.027 Uiso 1 1 calc R U . . .
C16 C 0.6573(5) 0.70390(12) 0.9731(4) 0.0297(11) Uani 1 1 d . . . . .
H16A H 0.7279 0.6989 0.9512 0.044 Uiso 1 1 calc R U . . .
H16B H 0.6852 0.7096 1.0492 0.044 Uiso 1 1 calc R U . . .
H16C H 0.6120 0.7240 0.9322 0.044 Uiso 1 1 calc R U . . .
C17 C 0.4163(4) 0.66152(10) 0.7765(3) 0.0152(9) Uani 1 1 d . . . . .
C18 C 0.2797(5) 0.74147(12) 0.7116(5) 0.0400(14) Uani 1 1 d . . . . .
H18A H 0.2931 0.7308 0.6496 0.060 Uiso 1 1 calc R U . . .
H18B H 0.3084 0.7660 0.7193 0.060 Uiso 1 1 calc R U . . .
H18C H 0.1924 0.7410 0.7017 0.060 Uiso 1 1 calc R U . . .
C19 C 0.3507(5) 0.72047(12) 0.8126(4) 0.0307(12) Uani 1 1 d . . . . .
H19 H 0.4390 0.7237 0.8220 0.037 Uiso 1 1 calc R U . . .
C20 C 0.3335(5) 0.73664(15) 0.9116(5) 0.0508(16) Uani 1 1 d . . . . .
H20A H 0.2480 0.7342 0.9068 0.076 Uiso 1 1 calc R U . . .
H20B H 0.3553 0.7617 0.9161 0.076 Uiso 1 1 calc R U . . .
H20C H 0.3860 0.7244 0.9753 0.076 Uiso 1 1 calc R U . . .
C21 C 0.0979(5) 0.68256(14) 0.7531(4) 0.0347(12) Uani 1 1 d . . . . .
H21A H 0.0974 0.7054 0.7875 0.052 Uiso 1 1 calc R U . . .
H21B H 0.0308 0.6679 0.7585 0.052 Uiso 1 1 calc R U . . .
H21C H 0.0877 0.6863 0.6779 0.052 Uiso 1 1 calc R U . . .
C22 C 0.2188(4) 0.66395(12) 0.8081(4) 0.0258(10) Uani 1 1 d . . . . .
H22 H 0.2139 0.6408 0.7710 0.031 Uiso 1 1 calc R U . . .
C23 C 0.2328(5) 0.65517(15) 0.9244(4) 0.0401(13) Uani 1 1 d . . . . .
H23A H 0.3093 0.6423 0.9576 0.060 Uiso 1 1 calc R U . . .
H23B H 0.1640 0.6405 0.9258 0.060 Uiso 1 1 calc R U . . .
H23C H 0.2342 0.6771 0.9637 0.060 Uiso 1 1 calc R U . . .
C24 C 0.3095(4) 0.65917(13) 0.5016(3) 0.0258(10) Uani 1 1 d . . . . .
H24A H 0.2340 0.6625 0.4410 0.031 Uiso 1 1 calc R U . . .
H24B H 0.3605 0.6414 0.4834 0.031 Uiso 1 1 calc R U . . .
H24C H 0.3538 0.6816 0.5182 0.031 Uiso 1 1 calc R U . . .
C25 C 0.2785(4) 0.64670(11) 0.5984(3) 0.0189(9) Uani 1 1 d . . . . .
H25 H 0.2292 0.6655 0.6174 0.023 Uiso 1 1 calc R U . . .
C26 C 0.2015(4) 0.61340(12) 0.5701(4) 0.0262(10) Uani 1 1 d . . . . .
H26A H 0.2472 0.5949 0.5485 0.039 Uiso 1 1 calc R U . . .
H26B H 0.1259 0.6184 0.5112 0.039 Uiso 1 1 calc R U . . .
H26C H 0.1819 0.6054 0.6322 0.039 Uiso 1 1 calc R U . . .
C27 C 0.3673(5) 0.52837(13) 0.7093(4) 0.0303(11) Uani 1 1 d . . . . .
H27A H 0.3252 0.5462 0.6561 0.045 Uiso 1 1 calc R U . . .
H27B H 0.3069 0.5141 0.7275 0.045 Uiso 1 1 calc R U . . .
H27C H 0.4159 0.5130 0.6800 0.045 Uiso 1 1 calc R U . . .
C28 C 0.4515(4) 0.54686(12) 0.8097(4) 0.0250(10) Uani 1 1 d . . . . .
H28 H 0.4874 0.5284 0.8652 0.030 Uiso 1 1 calc R U . . .
C29 C 0.3773(4) 0.57203(12) 0.8518(4) 0.0276(11) Uani 1 1 d . . . . .
H29A H 0.4295 0.5821 0.9196 0.041 Uiso 1 1 calc R U . . .
H29B H 0.3095 0.5592 0.8628 0.041 Uiso 1 1 calc R U . . .
H29C H 0.3450 0.5911 0.8001 0.041 Uiso 1 1 calc R U . . .
C30 C 0.6685(4) 0.55508(11) 0.8406(3) 0.0186(9) Uani 1 1 d . . . . .
C31 C 0.7769(5) 0.47574(12) 0.8006(4) 0.0279(11) Uani 1 1 d . . . . .
H31A H 0.8095 0.4939 0.7650 0.042 Uiso 1 1 calc R U . . .
H31B H 0.7520 0.4550 0.7541 0.042 Uiso 1 1 calc R U . . .
H31C H 0.8400 0.4688 0.8675 0.042 Uiso 1 1 calc R U . . .
C32 C 0.6674(4) 0.49045(10) 0.8239(3) 0.0188(9) Uani 1 1 d . . . . .
H32 H 0.6090 0.4987 0.7540 0.023 Uiso 1 1 calc R U . . .
C33 C 0.6018(6) 0.46078(13) 0.8614(5) 0.0408(14) Uani 1 1 d . . . . .
H33A H 0.6583 0.4499 0.9260 0.061 Uiso 1 1 calc R U . . .
H33B H 0.5735 0.4429 0.8054 0.061 Uiso 1 1 calc R U . . .
H33C H 0.5317 0.4706 0.8769 0.061 Uiso 1 1 calc R U . . .
C34 C 0.8504(7) 0.50075(18) 1.0632(5) 0.0471(18) Uani 1 1 d . . . . .
C35 C 0.7152(9) 0.5159(2) 1.0076(6) 0.019(2) Uani 0.681(17) 1 d . . P A 1
H35 H 0.6547 0.4980 1.0133 0.023 Uiso 0.681(17) 1 calc R U P A 1
C36 C 0.6978(7) 0.5497(3) 1.0614(5) 0.025(2) Uani 0.681(17) 1 d . . P A 1
H36A H 0.7528 0.5680 1.0516 0.038 Uiso 0.681(17) 1 calc R U P A 1
H36B H 0.7162 0.5454 1.1377 0.038 Uiso 0.681(17) 1 calc R U P A 1
H36C H 0.6131 0.5577 1.0298 0.038 Uiso 0.681(17) 1 calc R U P A 1
C35A C 0.771(2) 0.5271(5) 1.0057(11) 0.017(4) Uani 0.319(17) 1 d . . P A 2
H35A H 0.8139 0.5505 1.0161 0.020 Uiso 0.319(17) 1 calc R U P A 2
C36A C 0.6807(15) 0.5260(6) 1.0651(12) 0.023(5) Uani 0.319(17) 1 d . . P A 2
H36D H 0.6438 0.5025 1.0580 0.035 Uiso 0.319(17) 1 calc R U P A 2
H36E H 0.6168 0.5437 1.0351 0.035 Uiso 0.319(17) 1 calc R U P A 2
H36F H 0.7232 0.5312 1.1407 0.035 Uiso 0.319(17) 1 calc R U P A 2
C37 C 0.9576(4) 0.58838(12) 0.9708(4) 0.0282(11) Uani 1 1 d . . . . .
H37A H 0.9515 0.6139 0.9567 0.042 Uiso 1 1 calc R U . . .
H37B H 1.0433 0.5811 0.9922 0.042 Uiso 1 1 calc R U . . .
H37C H 0.9255 0.5830 1.0282 0.042 Uiso 1 1 calc R U . . .
C38 C 0.8835(4) 0.56847(11) 0.8701(3) 0.0228(10) Uani 1 1 d . . . . .
H38 H 0.8909 0.5426 0.8865 0.027 Uiso 1 1 calc R U . . .
C39 C 0.9343(5) 0.57520(13) 0.7812(4) 0.0295(11) Uani 1 1 d . . . . .
H39A H 0.8900 0.5607 0.7193 0.044 Uiso 1 1 calc R U . . .
H39B H 1.0211 0.5690 0.8055 0.044 Uiso 1 1 calc R U . . .
H39C H 0.9245 0.6002 0.7614 0.044 Uiso 1 1 calc R U . . .
C40 C 1.0879(8) 0.6612(2) 0.1818(7) 0.083(3) Uani 1 1 d . . . . .
H40A H 1.0662 0.6711 0.1100 0.125 Uiso 1 1 calc R U . . .
H40B H 1.1276 0.6382 0.1842 0.125 Uiso 1 1 calc R U . . .
H40C H 1.1438 0.6773 0.2330 0.125 Uiso 1 1 calc R U . . .
C41 C 0.9806(7) 0.6567(2) 0.2084(7) 0.0815(12) Uani 1 1 d . . . . .
H41A H 0.9978 0.6382 0.2640 0.098 Uiso 1 1 calc R U . . .
H41B H 0.9165 0.6473 0.1446 0.098 Uiso 1 1 calc R U . . .
C42 C 0.9284(7) 0.6871(2) 0.2461(7) 0.0815(12) Uani 1 1 d . . . . .
H42A H 0.9074 0.7045 0.1874 0.098 Uiso 1 1 calc R U . . .
H42B H 0.8500 0.6787 0.2511 0.098 Uiso 1 1 calc R U . . .
C43 C 0.9872(7) 0.7072(2) 0.3435(7) 0.0815(12) Uani 1 1 d . . . . .
H43A H 1.0685 0.7145 0.3427 0.098 Uiso 1 1 calc R U . . .
H43B H 1.0012 0.6907 0.4041 0.098 Uiso 1 1 calc R U . . .
C44 C 0.9281(7) 0.7387(2) 0.3669(7) 0.0815(12) Uani 1 1 d . . . . .
H44A H 0.8445 0.7320 0.3631 0.098 Uiso 1 1 calc R U . . .
H44B H 0.9198 0.7561 0.3095 0.098 Uiso 1 1 calc R U . . .
C45 C 0.9881(8) 0.7568(2) 0.4711(6) 0.0808(12) Uani 1 1 d . . . . .
H45A H 1.0719 0.7632 0.4777 0.121 Uiso 1 1 calc R U . . .
H45B H 0.9894 0.7409 0.5295 0.121 Uiso 1 1 calc R U . . .
H45C H 0.9424 0.7783 0.4745 0.121 Uiso 1 1 calc R U . . .
C46 C 0.0173(8) 0.5565(2) 0.3293(6) 0.0808(12) Uani 1 1 d . . . . .
H46A H -0.0020 0.5755 0.3708 0.121 Uiso 1 1 calc R U . . .
H46B H -0.0404 0.5572 0.2561 0.121 Uiso 1 1 calc R U . . .
H46C H 0.1005 0.5596 0.3285 0.121 Uiso 1 1 calc R U . . .
C47 C 0.0082(9) 0.5239(2) 0.3753(6) 0.0808(12) Uani 1 1 d . . . . .
H47A H -0.0659 0.5128 0.3249 0.097 Uiso 1 1 calc R U . . .
H47B H 0.0777 0.5100 0.3698 0.097 Uiso 1 1 calc R U . . .
C48 C 0.0037(9) 0.51587(18) 0.4755(6) 0.0808(12) Uani 1 1 d . . . . .
H48A H 0.0771 0.5274 0.5254 0.097 Uiso 1 1 calc R U . . .
H48B H -0.0665 0.5297 0.4801 0.097 Uiso 1 1 calc R U . . .
Cl1 Cl 0.81580(10) 0.66064(3) 0.82287(8) 0.0202(2) Uani 1 1 d . . . . .
N1 N 0.6032(3) 0.60302(9) 0.5615(3) 0.0164(8) Uani 1 1 d . . . . .
N2 N 0.6181(3) 0.63958(9) 0.4180(3) 0.0185(8) Uani 1 1 d . . . . .
N3 N 0.6056(3) 0.66127(9) 0.5859(3) 0.0155(7) Uani 1 1 d . . . . .
N4 N 0.5333(3) 0.66045(9) 0.8398(3) 0.0165(8) Uani 1 1 d . . . . .
N5 N 0.3277(3) 0.68216(9) 0.8000(3) 0.0209(8) Uani 1 1 d . . . . .
N6 N 0.3915(3) 0.64132(8) 0.6903(3) 0.0150(7) Uani 1 1 d . . . . .
N7 N 0.5525(3) 0.56558(9) 0.7895(3) 0.0225(8) Uani 1 1 d . . . . .
N8 N 0.6980(4) 0.52187(9) 0.8932(3) 0.0197(8) Uani 1 1 d . . . . .
N9 N 0.7526(3) 0.57784(9) 0.8346(3) 0.0177(8) Uani 1 1 d . . . . .
U1 U 0.61170(2) 0.62371(2) 0.73521(2) 0.01270(6) Uani 1 1 d . . . . .
H34A H 0.858(4) 0.4773(14) 1.039(4) 0.025(13) Uiso 1 1 d . . . . .
H34B H 0.907(5) 0.5103(15) 1.047(4) 0.035(19) Uiso 1 1 d . . . . .
H34C H 0.872(8) 0.4942(19) 1.134(6) 0.10(3) Uiso 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
C1 C2 1.516(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N1 1.469(5) . ?
C2 C3 1.516(7) . ?
C2 H2 1.0000 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 N3 1.341(5) . ?
C4 N1 1.345(5) . ?
C4 N2 1.405(5) . ?
C4 U1 2.898(4) . ?
C5 C6 1.532(7) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 N2 1.485(6) . ?
C6 C7 1.526(7) . ?
C6 H6 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.535(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.466(5) . ?
C9 C10 1.541(6) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.528(6) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N3 1.467(5) . ?
C12 C13 1.524(6) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.519(7) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 N4 1.474(5) . ?
C15 C16 1.520(6) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N6 1.329(5) . ?
C17 N4 1.339(5) . ?
C17 N5 1.411(5) . ?
C17 U1 2.895(4) . ?
C18 C19 1.542(7) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 N5 1.473(6) . ?
C19 C20 1.530(7) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.522(7) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 N5 1.479(6) . ?
C22 C23 1.539(6) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.529(6) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 N6 1.478(5) . ?
C25 C26 1.518(6) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.536(6) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 N7 1.473(6) . ?
C28 C29 1.515(6) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 N9 1.327(6) . ?
C30 N7 1.350(6) . ?
C30 N8 1.423(5) . ?
C30 U1 2.920(4) . ?
C31 C32 1.517(6) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 N8 1.474(5) . ?
C32 C33 1.534(6) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35A 1.398(16) . ?
C34 C35 1.602(11) . ?
C34 H34A 0.96(5) . ?
C34 H34B 0.84(6) . ?
C34 H34C 0.92(8) . ?
C35 N8 1.489(8) . ?
C35 C36 1.514(13) . ?
C35 H35 1.0000 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C35A N8 1.468(15) . ?
C35A C36A 1.52(3) . ?
C35A H35A 1.0000 . ?
C36A H36D 0.9800 . ?
C36A H36E 0.9800 . ?
C36A H36F 0.9800 . ?
C37 C38 1.528(6) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 N9 1.478(6) . ?
C38 C39 1.515(6) . ?
C38 H38 1.0000 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.420(10) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.465(9) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.461(10) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.462(10) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.495(10) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C47 1.396(10) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.390(9) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C48 1.384(14) 3_566 ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
Cl1 U1 2.6621(11) . ?
N1 U1 2.416(3) . ?
N3 U1 2.428(3) . ?
N4 U1 2.362(3) . ?
N6 U1 2.517(3) . ?
N7 U1 2.486(3) . ?
N9 U1 2.448(3) . ?

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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C1 110.8(4) . . ?
N1 C2 C3 110.2(4) . . ?
C1 C2 C3 109.9(4) . . ?
N1 C2 H2 108.7 . . ?
C1 C2 H2 108.7 . . ?
C3 C2 H2 108.7 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N3 C4 N1 112.0(3) . . ?
N3 C4 N2 125.0(4) . . ?
N1 C4 N2 122.9(4) . . ?
N3 C4 U1 56.4(2) . . ?
N1 C4 U1 55.91(19) . . ?
N2 C4 U1 175.7(3) . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C6 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 C7 112.6(3) . . ?
N2 C6 C5 113.1(4) . . ?
C7 C6 C5 110.0(4) . . ?
N2 C6 H6 106.9 . . ?
C7 C6 H6 106.9 . . ?
C5 C6 H6 106.9 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C8 112.9(4) . . ?
N2 C9 C10 114.4(4) . . ?
C8 C9 C10 110.0(4) . . ?
N2 C9 H9 106.3 . . ?
C8 C9 H9 106.3 . . ?
C10 C9 H9 106.3 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 C13 108.6(3) . . ?
N3 C12 C11 114.1(4) . . ?
C13 C12 C11 110.4(4) . . ?
N3 C12 H12 107.8 . . ?
C13 C12 H12 107.8 . . ?
C11 C12 H12 107.8 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N4 C15 C14 108.3(4) . . ?
N4 C15 C16 112.7(4) . . ?
C14 C15 C16 109.3(4) . . ?
N4 C15 H15 108.8 . . ?
C14 C15 H15 108.8 . . ?
C16 C15 H15 108.8 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N6 C17 N4 113.9(4) . . ?
N6 C17 N5 123.4(4) . . ?
N4 C17 N5 122.7(4) . . ?
N6 C17 U1 60.3(2) . . ?
N4 C17 U1 53.7(2) . . ?
N5 C17 U1 175.4(3) . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C19 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N5 C19 C20 114.8(4) . . ?
N5 C19 C18 112.6(4) . . ?
C20 C19 C18 111.1(4) . . ?
N5 C19 H19 105.8 . . ?
C20 C19 H19 105.8 . . ?
C18 C19 H19 105.8 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N5 C22 C21 115.2(4) . . ?
N5 C22 C23 111.9(4) . . ?
C21 C22 C23 110.6(4) . . ?
N5 C22 H22 106.2 . . ?
C21 C22 H22 106.2 . . ?
C23 C22 H22 106.2 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C25 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N6 C25 C26 112.1(3) . . ?
N6 C25 C24 110.1(3) . . ?
C26 C25 C24 109.5(4) . . ?
N6 C25 H25 108.3 . . ?
C26 C25 H25 108.3 . . ?
C24 C25 H25 108.3 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C28 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N7 C28 C29 110.8(4) . . ?
N7 C28 C27 111.9(4) . . ?
C29 C28 C27 109.5(4) . . ?
N7 C28 H28 108.2 . . ?
C29 C28 H28 108.2 . . ?
C27 C28 H28 108.2 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N9 C30 N7 114.3(4) . . ?
N9 C30 N8 122.8(4) . . ?
N7 C30 N8 122.8(4) . . ?
N9 C30 U1 56.3(2) . . ?
N7 C30 U1 58.1(2) . . ?
N8 C30 U1 179.0(3) . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N8 C32 C31 112.5(4) . . ?
N8 C32 C33 115.3(4) . . ?
C31 C32 C33 110.2(4) . . ?
N8 C32 H32 106.0 . . ?
C31 C32 H32 106.0 . . ?
C33 C32 H32 106.0 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35A C34 H34A 127(3) . . ?
C35 C34 H34A 111(3) . . ?
C35A C34 H34B 89(4) . . ?
C35 C34 H34B 117(4) . . ?
H34A C34 H34B 98(5) . . ?
C35A C34 H34C 131(5) . . ?
C35 C34 H34C 117(5) . . ?
H34A C34 H34C 94(5) . . ?
H34B C34 H34C 114(7) . . ?
N8 C35 C36 111.4(7) . . ?
N8 C35 C34 107.4(6) . . ?
C36 C35 C34 110.6(7) . . ?
N8 C35 H35 109.1 . . ?
C36 C35 H35 109.1 . . ?
C34 C35 H35 109.1 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C35A N8 120.8(11) . . ?
C34 C35A C36A 97.9(15) . . ?
N8 C35A C36A 105.3(16) . . ?
C34 C35A H35A 110.5 . . ?
N8 C35A H35A 110.5 . . ?
C36A C35A H35A 110.5 . . ?
C35A C36A H36D 109.5 . . ?
C35A C36A H36E 109.5 . . ?
H36D C36A H36E 109.5 . . ?
C35A C36A H36F 109.5 . . ?
H36D C36A H36F 109.5 . . ?
H36E C36A H36F 109.5 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N9 C38 C39 110.0(4) . . ?
N9 C38 C37 112.2(4) . . ?
C39 C38 C37 110.6(4) . . ?
N9 C38 H38 108.0 . . ?
C39 C38 H38 108.0 . . ?
C37 C38 H38 108.0 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C41 C40 H40A 109.5 . . ?
C41 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C41 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C40 C41 C42 119.7(7) . . ?
C40 C41 H41A 107.4 . . ?
C42 C41 H41A 107.4 . . ?
C40 C41 H41B 107.4 . . ?
C42 C41 H41B 107.4 . . ?
H41A C41 H41B 106.9 . . ?
C43 C42 C41 126.2(8) . . ?
C43 C42 H42A 105.8 . . ?
C41 C42 H42A 105.8 . . ?
C43 C42 H42B 105.8 . . ?
C41 C42 H42B 105.8 . . ?
H42A C42 H42B 106.2 . . ?
C42 C43 C44 120.1(8) . . ?
C42 C43 H43A 107.3 . . ?
C44 C43 H43A 107.3 . . ?
C42 C43 H43B 107.3 . . ?
C44 C43 H43B 107.3 . . ?
H43A C43 H43B 106.9 . . ?
C43 C44 C45 117.9(7) . . ?
C43 C44 H44A 107.8 . . ?
C45 C44 H44A 107.8 . . ?
C43 C44 H44B 107.8 . . ?
C45 C44 H44B 107.8 . . ?
H44A C44 H44B 107.2 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C47 C46 H46A 109.5 . . ?
C47 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C47 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C47 C46 130.5(7) . . ?
C48 C47 H47A 104.6 . . ?
C46 C47 H47A 104.6 . . ?
C48 C47 H47B 104.6 . . ?
C46 C47 H47B 104.6 . . ?
H47A C47 H47B 105.7 . . ?
C48 C48 C47 132.3(9) 3_566 . ?
C48 C48 H48A 104.2 3_566 . ?
C47 C48 H48A 104.2 . . ?
C48 C48 H48B 104.2 3_566 . ?
C47 C48 H48B 104.2 . . ?
H48A C48 H48B 105.5 . . ?
C4 N1 C2 121.1(3) . . ?
C4 N1 U1 96.7(2) . . ?
C2 N1 U1 141.1(3) . . ?
C4 N2 C9 117.5(3) . . ?
C4 N2 C6 120.3(3) . . ?
C9 N2 C6 120.0(3) . . ?
C4 N3 C12 124.5(3) . . ?
C4 N3 U1 96.2(2) . . ?
C12 N3 U1 136.4(3) . . ?
C17 N4 C15 123.0(4) . . ?
C17 N4 U1 99.2(2) . . ?
C15 N4 U1 135.5(3) . . ?
C17 N5 C19 116.8(4) . . ?
C17 N5 C22 117.9(3) . . ?
C19 N5 C22 125.3(4) . . ?
C17 N6 C25 120.6(3) . . ?
C17 N6 U1 92.4(2) . . ?
C25 N6 U1 141.6(3) . . ?
C30 N7 C28 119.4(4) . . ?
C30 N7 U1 94.5(3) . . ?
C28 N7 U1 142.8(3) . . ?
C30 N8 C35A 110.2(8) . . ?
C30 N8 C32 115.9(3) . . ?
C35A N8 C32 133.2(7) . . ?
C30 N8 C35 124.4(4) . . ?
C32 N8 C35 116.2(5) . . ?
C30 N9 C38 121.8(3) . . ?
C30 N9 U1 96.9(3) . . ?
C38 N9 U1 140.6(3) . . ?
N4 U1 N1 149.22(12) . . ?
N4 U1 N3 103.35(11) . . ?
N1 U1 N3 54.73(11) . . ?
N4 U1 N9 114.82(11) . . ?
N1 U1 N9 95.27(11) . . ?
N3 U1 N9 133.42(12) . . ?
N4 U1 N7 98.46(12) . . ?
N1 U1 N7 93.88(12) . . ?
N3 U1 N7 145.41(12) . . ?
N9 U1 N7 54.26(12) . . ?
N4 U1 N6 54.45(11) . . ?
N1 U1 N6 98.60(11) . . ?
N3 U1 N6 84.57(11) . . ?
N9 U1 N6 139.36(11) . . ?
N7 U1 N6 86.72(12) . . ?
N4 U1 Cl1 84.14(9) . . ?
N1 U1 Cl1 109.40(9) . . ?
N3 U1 Cl1 80.03(9) . . ?
N9 U1 Cl1 78.41(9) . . ?
N7 U1 Cl1 129.12(9) . . ?
N6 U1 Cl1 130.67(8) . . ?
N4 U1 C17 27.17(12) . . ?
N1 U1 C17 124.27(12) . . ?
N3 U1 C17 93.47(11) . . ?
N9 U1 C17 132.34(11) . . ?
N7 U1 C17 93.90(12) . . ?
N6 U1 C17 27.31(11) . . ?
Cl1 U1 C17 107.43(8) . . ?
N4 U1 C4 128.69(11) . . ?
N1 U1 C4 27.44(11) . . ?
N3 U1 C4 27.39(11) . . ?
N9 U1 C4 114.83(11) . . ?
N7 U1 C4 120.66(12) . . ?
N6 U1 C4 93.43(11) . . ?
Cl1 U1 C4 93.67(9) . . ?
C17 U1 C4 111.95(11) . . ?
N4 U1 C30 107.97(11) . . ?
N1 U1 C30 95.89(11) . . ?
N3 U1 C30 148.68(11) . . ?
N9 U1 C30 26.82(12) . . ?
N7 U1 C30 27.45(12) . . ?
N6 U1 C30 113.35(12) . . ?
Cl1 U1 C30 103.44(9) . . ?
C17 U1 C30 114.35(12) . . ?
C4 U1 C30 122.19(11) . . ?

_refine_diff_density_max         1.855
_refine_diff_density_min         -1.469
_refine_diff_density_rms         0.133


_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_U(Nptolyl)(TIG)3
_database_code_depnum_ccdc_archive 'CCDC 1860827'
_audit_update_record             
;
2018-08-07 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT230_U(Nptolyl)(TIG)3    
;
PROBLEM: Hirshfeld Test Diff for   N7       --C28       .        7.4 s.u.
RESPONSE: Due to large thermal motion of atoms
;
_vrf_PLAT360_U(Nptolyl)(TIG)3    
;
PROBLEM: Short  C(sp3)-C(sp3) Bond  C48      - C49      .       1.32 Ang.
RESPONSE: Due to disorder of solvent molecule
;
# Added during the CSD deposition process: Tuesday 07 August 2018 10:16 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            U(Nptolyl)(TIG)3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49 H98 N10 U'
_chemical_formula_weight         1065.40

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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   39.246(4)
_cell_length_b                   14.3692(16)
_cell_length_c                   19.965(2)
_cell_angle_alpha                90
_cell_angle_beta                 109.062(9)
_cell_angle_gamma                90
_cell_volume                     10641(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9348
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      25.40

_exptl_crystal_description       Block
_exptl_crystal_colour            Brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_F_000             4432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    3.091
_shelx_estimated_absorpt_T_min   0.861
_shelx_estimated_absorpt_T_max   0.861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.643
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            88992
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.520
_diffrn_reflns_theta_max         25.451
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9820
_reflns_number_gt                8353
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    Mercury
_computing_publication_material  WinGX
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0361P)²+147.6751P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9820
_refine_ls_number_parameters     567
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.1043
_refine_ls_wR_factor_gt          0.0987
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_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
C1 C 0.39356(17) 0.5400(5) 0.5391(4) 0.0403(15) Uani 1 1 d . . . . .
H1A H 0.3815 0.5911 0.5549 0.060 Uiso 1 1 calc R U . . .
H1B H 0.3988 0.4897 0.5742 0.060 Uiso 1 1 calc R U . . .
H1C H 0.3778 0.5165 0.4934 0.060 Uiso 1 1 calc R U . . .
C2 C 0.42885(15) 0.5753(4) 0.5311(3) 0.0270(12) Uani 1 1 d . . . . .
H2 H 0.4442 0.6017 0.5774 0.032 Uiso 1 1 calc R U . . .
C3 C 0.44925(15) 0.4962(4) 0.5107(3) 0.0323(13) Uani 1 1 d . . . . .
H3A H 0.4368 0.4781 0.4614 0.048 Uiso 1 1 calc R U . . .
H3B H 0.4503 0.4427 0.5418 0.048 Uiso 1 1 calc R U . . .
H3C H 0.4738 0.5167 0.5157 0.048 Uiso 1 1 calc R U . . .
C4 C 0.43391(14) 0.7357(4) 0.4916(3) 0.0279(12) Uani 1 1 d . . . . .
C5 C 0.51751(15) 0.6620(5) 0.6305(3) 0.0362(14) Uani 1 1 d . . . . .
H5A H 0.5262 0.7114 0.6658 0.054 Uiso 1 1 calc R U . . .
H5B H 0.5380 0.6249 0.6278 0.054 Uiso 1 1 calc R U . . .
H5C H 0.5007 0.6219 0.6441 0.054 Uiso 1 1 calc R U . . .
C6 C 0.49828(14) 0.7054(4) 0.5583(3) 0.0318(13) Uani 1 1 d . . . . .
H6 H 0.4915 0.6525 0.5240 0.038 Uiso 1 1 calc R U . . .
C7 C 0.52463(16) 0.7660(5) 0.5347(4) 0.0412(16) Uani 1 1 d . . . . .
H7A H 0.5116 0.7970 0.4899 0.062 Uiso 1 1 calc R U . . .
H7B H 0.5437 0.7267 0.5280 0.062 Uiso 1 1 calc R U . . .
H7C H 0.5354 0.8130 0.5711 0.062 Uiso 1 1 calc R U . . .
C8 C 0.49032(18) 0.8911(5) 0.6324(4) 0.056(2) Uani 1 1 d . . . . .
H8A H 0.5122 0.8583 0.6607 0.085 Uiso 1 1 calc R U . . .
H8B H 0.4836 0.9373 0.6620 0.085 Uiso 1 1 calc R U . . .
H8C H 0.4949 0.9226 0.5926 0.085 Uiso 1 1 calc R U . . .
C9 C 0.45955(16) 0.8212(4) 0.6040(4) 0.0395(15) Uani 1 1 d . . . . .
H9 H 0.4377 0.8587 0.5782 0.047 Uiso 1 1 calc R U . . .
C10 C 0.45091(19) 0.7735(6) 0.6654(4) 0.0499(19) Uani 1 1 d . . . . .
H10A H 0.4299 0.7330 0.6464 0.075 Uiso 1 1 calc R U . . .
H10B H 0.4457 0.8209 0.6960 0.075 Uiso 1 1 calc R U . . .
H10C H 0.4716 0.7362 0.6930 0.075 Uiso 1 1 calc R U . . .
C11 C 0.4435(2) 0.9021(5) 0.3749(4) 0.056(2) Uani 1 1 d . . . . .
H11A H 0.4605 0.8537 0.3716 0.083 Uiso 1 1 calc R U . . .
H11B H 0.4544 0.9635 0.3746 0.083 Uiso 1 1 calc R U . . .
H11C H 0.4213 0.8972 0.3344 0.083 Uiso 1 1 calc R U . . .
C12 C 0.43485(17) 0.8898(4) 0.4439(4) 0.0442(17) Uani 1 1 d . . . . .
H12 H 0.4581 0.8907 0.4843 0.053 Uiso 1 1 calc R U . . .
C13 C 0.41157(19) 0.9704(5) 0.4540(5) 0.057(2) Uani 1 1 d . . . . .
H13A H 0.3898 0.9749 0.4125 0.086 Uiso 1 1 calc R U . . .
H13B H 0.4252 1.0286 0.4594 0.086 Uiso 1 1 calc R U . . .
H13C H 0.4048 0.9594 0.4964 0.086 Uiso 1 1 calc R U . . .
C14 C 0.47253(18) 0.6387(6) 0.3568(4) 0.054(2) Uani 1 1 d . . . . .
H14A H 0.4764 0.6934 0.3876 0.080 Uiso 1 1 calc R U . . .
H14B H 0.4957 0.6166 0.3544 0.080 Uiso 1 1 calc R U . . .
H14C H 0.4611 0.5893 0.3759 0.080 Uiso 1 1 calc R U . . .
C15 C 0.44842(14) 0.6643(4) 0.2837(3) 0.0280(12) Uani 1 1 d . . . . .
H15 H 0.4601 0.7162 0.2657 0.034 Uiso 1 1 calc R U . . .
C16 C 0.44416(19) 0.5817(6) 0.2340(5) 0.074(3) Uani 1 1 d . . . . .
H16A H 0.4346 0.5284 0.2530 0.111 Uiso 1 1 calc R U . . .
H16B H 0.4677 0.5654 0.2300 0.111 Uiso 1 1 calc R U . . .
H16C H 0.4274 0.5980 0.1872 0.111 Uiso 1 1 calc R U . . .
C17 C 0.39126(16) 0.7512(5) 0.2415(4) 0.0378(15) Uani 1 1 d . . . . .
C18 C 0.4521(3) 0.8283(8) 0.1474(6) 0.091(3) Uani 1 1 d . . . . .
H18A H 0.4589 0.7628 0.1570 0.137 Uiso 1 1 calc R U . . .
H18B H 0.4732 0.8679 0.1688 0.137 Uiso 1 1 calc R U . . .
H18C H 0.4431 0.8388 0.0961 0.137 Uiso 1 1 calc R U . . .
C19 C 0.4209(3) 0.8540(8) 0.1809(6) 0.090(3) Uani 1 1 d . . . . .
H19 H 0.4327 0.8695 0.2321 0.108 Uiso 1 1 calc R U . . .
C20 C 0.3990(3) 0.9437(6) 0.1422(6) 0.087(3) Uani 1 1 d . . . . .
H20A H 0.3881 0.9310 0.0914 0.130 Uiso 1 1 calc R U . . .
H20B H 0.4155 0.9967 0.1489 0.130 Uiso 1 1 calc R U . . .
H20C H 0.3801 0.9584 0.1625 0.130 Uiso 1 1 calc R U . . .
C21 C 0.3828(5) 0.7400(12) 0.0462(7) 0.149(7) Uani 1 1 d . . . . .
H21A H 0.4081 0.7206 0.0648 0.224 Uiso 1 1 calc R U . . .
H21B H 0.3813 0.8013 0.0238 0.224 Uiso 1 1 calc R U . . .
H21C H 0.3691 0.6947 0.0110 0.224 Uiso 1 1 calc R U . . .
C22 C 0.3688(3) 0.7449(6) 0.1004(5) 0.068(2) Uani 1 1 d . . . . .
H22 H 0.3500 0.7947 0.0866 0.082 Uiso 1 1 calc R U . . .
C23 C 0.3498(3) 0.6594(7) 0.1103(5) 0.071(3) Uani 1 1 d . . . . .
H23A H 0.3330 0.6393 0.0645 0.106 Uiso 1 1 calc R U . . .
H23B H 0.3364 0.6723 0.1430 0.106 Uiso 1 1 calc R U . . .
H23C H 0.3675 0.6100 0.1301 0.106 Uiso 1 1 calc R U . . .
C24 C 0.2975(2) 0.8055(6) 0.2041(5) 0.059(2) Uani 1 1 d . . . . .
H24A H 0.2937 0.7522 0.1718 0.089 Uiso 1 1 calc R U . . .
H24B H 0.2805 0.8552 0.1816 0.089 Uiso 1 1 calc R U . . .
H24C H 0.2935 0.7862 0.2481 0.089 Uiso 1 1 calc R U . . .
C25 C 0.33500(19) 0.8402(5) 0.2205(4) 0.0490(19) Uani 1 1 d . . . . .
H25 H 0.3390 0.8561 0.1749 0.059 Uiso 1 1 calc R U . . .
C26 C 0.3404(2) 0.9254(7) 0.2644(5) 0.072(3) Uani 1 1 d . . . . .
H26A H 0.3353 0.9118 0.3083 0.109 Uiso 1 1 calc R U . . .
H26B H 0.3241 0.9743 0.2381 0.109 Uiso 1 1 calc R U . . .
H26C H 0.3654 0.9464 0.2760 0.109 Uiso 1 1 calc R U . . .
C27 C 0.2964(2) 0.4497(6) 0.3240(6) 0.086(3) Uani 1 1 d . . . . .
H27A H 0.2774 0.4066 0.2976 0.129 Uiso 1 1 calc R U . . .
H27B H 0.2968 0.4533 0.3733 0.129 Uiso 1 1 calc R U . . .
H27C H 0.3197 0.4274 0.3228 0.129 Uiso 1 1 calc R U . . .
C28 C 0.2890(2) 0.5442(7) 0.2910(5) 0.070(3) Uani 1 1 d . . . . .
H28 H 0.2638 0.5620 0.2867 0.084 Uiso 1 1 calc R U . . .
C29 C 0.2926(3) 0.5473(7) 0.2190(5) 0.087(3) Uani 1 1 d . . . . .
H29A H 0.3182 0.5435 0.2232 0.131 Uiso 1 1 calc R U . . .
H29B H 0.2825 0.6058 0.1957 0.131 Uiso 1 1 calc R U . . .
H29C H 0.2796 0.4947 0.1909 0.131 Uiso 1 1 calc R U . . .
C30 C 0.30340(14) 0.6763(4) 0.3731(3) 0.0261(12) Uani 1 1 d . . . . .
C31 C 0.29211(19) 0.5744(7) 0.4828(4) 0.068(3) Uani 1 1 d . . . . .
H31A H 0.3011 0.5293 0.4557 0.103 Uiso 1 1 calc R U . . .
H31B H 0.2852 0.5417 0.5196 0.103 Uiso 1 1 calc R U . . .
H31C H 0.3111 0.6197 0.5051 0.103 Uiso 1 1 calc R U . . .
C32 C 0.25959(16) 0.6244(5) 0.4336(3) 0.0386(15) Uani 1 1 d . . . . .
H32 H 0.2524 0.6730 0.4623 0.046 Uiso 1 1 calc R U . . .
C33 C 0.22810(17) 0.5569(5) 0.4072(4) 0.0443(16) Uani 1 1 d . . . . .
H33A H 0.2063 0.5912 0.3807 0.066 Uiso 1 1 calc R U . . .
H33B H 0.2243 0.5255 0.4477 0.066 Uiso 1 1 calc R U . . .
H33C H 0.2335 0.5105 0.3761 0.066 Uiso 1 1 calc R U . . .
C34 C 0.22125(18) 0.7951(5) 0.3702(4) 0.0468(17) Uani 1 1 d . . . . .
H34A H 0.2068 0.7516 0.3876 0.070 Uiso 1 1 calc R U . . .
H34B H 0.2053 0.8400 0.3379 0.070 Uiso 1 1 calc R U . . .
H34C H 0.2381 0.8282 0.4104 0.070 Uiso 1 1 calc R U . . .
C35 C 0.24211(17) 0.7419(6) 0.3314(4) 0.053(2) Uani 1 1 d . . . . .
H35 H 0.2571 0.7888 0.3168 0.064 Uiso 1 1 calc R U . . .
C36 C 0.2165(2) 0.7012(8) 0.2635(4) 0.088(4) Uani 1 1 d . . . . .
H36A H 0.2304 0.6775 0.2342 0.132 Uiso 1 1 calc R U . . .
H36B H 0.1999 0.7496 0.2374 0.132 Uiso 1 1 calc R U . . .
H36C H 0.2028 0.6502 0.2750 0.132 Uiso 1 1 calc R U . . .
C37 C 0.35234(19) 0.7972(8) 0.5307(4) 0.075(3) Uani 1 1 d . . . . .
H37A H 0.3528 0.7353 0.5516 0.113 Uiso 1 1 calc R U . . .
H37B H 0.3485 0.8444 0.5630 0.113 Uiso 1 1 calc R U . . .
H37C H 0.3754 0.8088 0.5230 0.113 Uiso 1 1 calc R U . . .
C38 C 0.32158(18) 0.8020(7) 0.4595(4) 0.061(3) Uani 1 1 d . . . . .
H38 H 0.2991 0.7808 0.4681 0.073 Uiso 1 1 calc R U . . .
C39 C 0.3153(2) 0.9004(7) 0.4319(5) 0.069(3) Uani 1 1 d . . . . .
H39A H 0.3370 0.9235 0.4233 0.103 Uiso 1 1 calc R U . . .
H39B H 0.3098 0.9402 0.4669 0.103 Uiso 1 1 calc R U . . .
H39C H 0.2950 0.9015 0.3875 0.103 Uiso 1 1 calc R U . . .
C40 C 0.38250(15) 0.4477(4) 0.3266(4) 0.0429(17) Uani 1 1 d . . . . .
C41 C 0.38004(16) 0.4211(5) 0.2574(4) 0.0481(19) Uani 1 1 d . . . . .
H41 H 0.3783 0.4676 0.2226 0.058 Uiso 1 1 calc R U . . .
C42 C 0.38015(17) 0.3271(6) 0.2389(6) 0.063(3) Uani 1 1 d . . . . .
H42 H 0.3787 0.3114 0.1918 0.076 Uiso 1 1 calc R U . . .
C43 C 0.3823(2) 0.2581(6) 0.2859(6) 0.073(3) Uani 1 1 d . . . . .
C44 C 0.3835(3) 0.1557(6) 0.2672(7) 0.109(5) Uani 1 1 d . . . . .
H44A H 0.3722 0.1475 0.2160 0.164 Uiso 1 1 calc R U . . .
H44B H 0.3705 0.1189 0.2923 0.164 Uiso 1 1 calc R U . . .
H44C H 0.4087 0.1350 0.2814 0.164 Uiso 1 1 calc R U . . .
C45 C 0.3840(2) 0.2820(5) 0.3529(5) 0.068(3) Uani 1 1 d . . . . .
H45 H 0.3849 0.2340 0.3861 0.082 Uiso 1 1 calc R U . . .
C46 C 0.3845(2) 0.3752(5) 0.3746(5) 0.064(3) Uani 1 1 d . . . . .
H46 H 0.3861 0.3890 0.4221 0.076 Uiso 1 1 calc R U . . .
C47 C 0.2424(4) 0.7072(10) 0.0065(7) 0.122(5) Uani 1 1 d . . . . .
H47A H 0.2622 0.6629 0.0286 0.146 Uiso 1 1 calc R U . . .
H47B H 0.2275 0.6805 -0.0395 0.146 Uiso 1 1 calc R U . . .
C48 C 0.2190(4) 0.7173(12) 0.0547(8) 0.131(6) Uani 1 1 d . . . . .
H48A H 0.2341 0.7426 0.1009 0.157 Uiso 1 1 calc R U . . .
H48B H 0.1997 0.7630 0.0331 0.157 Uiso 1 1 calc R U . . .
C49 C 0.2041(9) 0.6389(16) 0.0658(13) 0.31(2) Uani 1 1 d . . . . .
H49A H 0.1951 0.6039 0.0214 0.459 Uiso 1 1 calc R U . . .
H49B H 0.1841 0.6531 0.0832 0.459 Uiso 1 1 calc R U . . .
H49C H 0.2222 0.6016 0.1012 0.459 Uiso 1 1 calc R U . . .
N1 N 0.42043(12) 0.6497(3) 0.4775(3) 0.0268(10) Uani 1 1 d . . . . .
N2 N 0.46443(12) 0.7547(3) 0.5523(3) 0.0300(11) Uani 1 1 d . . . . .
N3 N 0.41714(12) 0.7996(3) 0.4448(3) 0.0283(11) Uani 1 1 d . . . . .
N4 N 0.41390(12) 0.6988(3) 0.2892(2) 0.0284(11) Uani 1 1 d . . . . .
N5 N 0.39758(16) 0.7779(5) 0.1765(4) 0.067(2) Uani 1 1 d . . . . .
N6 N 0.36152(16) 0.7689(5) 0.2572(4) 0.0556(18) Uani 1 1 d . . . . .
N7 N 0.31439(14) 0.6215(5) 0.3322(3) 0.0526(17) Uani 1 1 d . . . . .
N8 N 0.26762(13) 0.6726(4) 0.3758(3) 0.0400(13) Uani 1 1 d . . . . .
N9 N 0.32864(13) 0.7367(5) 0.4084(3) 0.0529(18) Uani 1 1 d . . . . .
N10 N 0.38244(12) 0.5398(3) 0.3466(3) 0.0310(11) Uani 1 1 d . . . . .
U1 U 0.37678(2) 0.67382(2) 0.36435(2) 0.02133(7) 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
C1 C2 1.532(8) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N1 1.472(7) . ?
C2 C3 1.520(8) . ?
C2 H2 1.0000 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 N3 1.323(7) . ?
C4 N1 1.337(7) . ?
C4 N2 1.425(7) . ?
C4 U1 2.924(5) . ?
C5 C6 1.524(8) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 N2 1.475(7) . ?
C6 C7 1.539(8) . ?
C6 H6 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.530(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.464(8) . ?
C9 C10 1.537(10) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.534(11) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N3 1.473(8) . ?
C12 C13 1.528(10) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.503(8) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 N4 1.480(7) . ?
C15 C16 1.520(9) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N4 1.309(7) . ?
C17 N6 1.328(8) . ?
C17 N5 1.448(9) . ?
C17 U1 2.914(6) . ?
C18 C19 1.618(14) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 N5 1.410(12) . ?
C19 C20 1.601(14) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.367(15) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.484(12) . ?
C22 N5 1.640(12) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.486(11) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 N6 1.474(8) . ?
C25 C26 1.480(12) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.496(13) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.489(14) . ?
C28 N7 1.538(11) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 N7 1.305(8) . ?
C30 N9 1.332(8) . ?
C30 N8 1.423(7) . ?
C30 U1 2.942(5) . ?
C31 C32 1.515(9) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 N8 1.466(8) . ?
C32 C33 1.523(9) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.506(10) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 N8 1.482(8) . ?
C35 C36 1.516(12) . ?
C35 H35 1.0000 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.537(10) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 N9 1.478(8) . ?
C38 C39 1.508(13) . ?
C38 H38 1.0000 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 N10 1.382(8) . ?
C40 C46 1.402(11) . ?
C40 C41 1.405(11) . ?
C41 C42 1.401(10) . ?
C41 H41 0.9500 . ?
C42 C43 1.348(13) . ?
C42 H42 0.9500 . ?
C43 C45 1.362(14) . ?
C43 C44 1.521(11) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.406(11) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 C47 1.43(3) 7_565 ?
C47 C48 1.54(2) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.32(3) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
N1 U1 2.372(4) . ?
N3 U1 2.587(5) . ?
N4 U1 2.434(5) . ?
N6 U1 2.443(5) . ?
N7 U1 2.438(5) . ?
N9 U1 2.499(5) . ?
N10 U1 1.983(5) . ?

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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 111.2(5) . . ?
N1 C2 C1 108.7(5) . . ?
C3 C2 C1 110.7(5) . . ?
N1 C2 H2 108.7 . . ?
C3 C2 H2 108.7 . . ?
C1 C2 H2 108.7 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N3 C4 N1 114.9(5) . . ?
N3 C4 N2 123.6(5) . . ?
N1 C4 N2 121.4(5) . . ?
N3 C4 U1 62.2(3) . . ?
N1 C4 U1 52.9(3) . . ?
N2 C4 U1 172.0(4) . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C6 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 C5 115.3(5) . . ?
N2 C6 C7 112.4(5) . . ?
C5 C6 C7 110.3(5) . . ?
N2 C6 H6 106.0 . . ?
C5 C6 H6 106.0 . . ?
C7 C6 H6 106.0 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C8 114.9(6) . . ?
N2 C9 C10 112.6(5) . . ?
C8 C9 C10 110.5(6) . . ?
N2 C9 H9 106.0 . . ?
C8 C9 H9 106.0 . . ?
C10 C9 H9 106.0 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 C13 111.1(6) . . ?
N3 C12 C11 110.9(6) . . ?
C13 C12 C11 110.4(6) . . ?
N3 C12 H12 108.1 . . ?
C13 C12 H12 108.1 . . ?
C11 C12 H12 108.1 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N4 C15 C14 108.1(5) . . ?
N4 C15 C16 113.7(5) . . ?
C14 C15 C16 110.0(6) . . ?
N4 C15 H15 108.3 . . ?
C14 C15 H15 108.3 . . ?
C16 C15 H15 108.3 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 N6 112.2(5) . . ?
N4 C17 N5 122.1(5) . . ?
N6 C17 N5 125.5(6) . . ?
N4 C17 U1 55.9(3) . . ?
N6 C17 U1 56.4(3) . . ?
N5 C17 U1 172.7(5) . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C19 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N5 C19 C20 111.1(8) . . ?
N5 C19 C18 111.3(10) . . ?
C20 C19 C18 110.1(7) . . ?
N5 C19 H19 108.1 . . ?
C20 C19 H19 108.1 . . ?
C18 C19 H19 108.1 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C21 C22 C23 114.4(10) . . ?
C21 C22 N5 114.6(10) . . ?
C23 C22 N5 109.9(7) . . ?
C21 C22 H22 105.7 . . ?
C23 C22 H22 105.7 . . ?
N5 C22 H22 105.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C25 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N6 C25 C26 109.8(7) . . ?
N6 C25 C24 111.3(6) . . ?
C26 C25 C24 110.4(7) . . ?
N6 C25 H25 108.4 . . ?
C26 C25 H25 108.4 . . ?
C24 C25 H25 108.4 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C28 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C27 112.8(8) . . ?
C29 C28 N7 104.2(8) . . ?
C27 C28 N7 115.0(7) . . ?
C29 C28 H28 108.2 . . ?
C27 C28 H28 108.2 . . ?
N7 C28 H28 108.2 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N7 C30 N9 112.5(5) . . ?
N7 C30 N8 122.2(5) . . ?
N9 C30 N8 125.2(5) . . ?
N7 C30 U1 54.9(3) . . ?
N9 C30 U1 57.7(3) . . ?
N8 C30 U1 176.9(4) . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N8 C32 C31 112.5(5) . . ?
N8 C32 C33 112.8(5) . . ?
C31 C32 C33 109.8(6) . . ?
N8 C32 H32 107.1 . . ?
C31 C32 H32 107.1 . . ?
C33 C32 H32 107.1 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C35 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N8 C35 C34 114.1(6) . . ?
N8 C35 C36 113.3(7) . . ?
C34 C35 C36 110.1(6) . . ?
N8 C35 H35 106.2 . . ?
C34 C35 H35 106.2 . . ?
C36 C35 H35 106.2 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N9 C38 C39 112.8(7) . . ?
N9 C38 C37 110.0(6) . . ?
C39 C38 C37 111.5(7) . . ?
N9 C38 H38 107.4 . . ?
C39 C38 H38 107.4 . . ?
C37 C38 H38 107.4 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N10 C40 C46 121.3(7) . . ?
N10 C40 C41 122.6(7) . . ?
C46 C40 C41 116.1(7) . . ?
C42 C41 C40 121.1(8) . . ?
C42 C41 H41 119.4 . . ?
C40 C41 H41 119.4 . . ?
C43 C42 C41 122.1(9) . . ?
C43 C42 H42 119.0 . . ?
C41 C42 H42 119.0 . . ?
C42 C43 C45 118.0(7) . . ?
C42 C43 C44 122.7(11) . . ?
C45 C43 C44 119.3(10) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 C46 122.3(9) . . ?
C43 C45 H45 118.8 . . ?
C46 C45 H45 118.8 . . ?
C40 C46 C45 120.3(9) . . ?
C40 C46 H46 119.8 . . ?
C45 C46 H46 119.8 . . ?
C47 C47 C48 114(2) 7_565 . ?
C47 C47 H47A 108.8 7_565 . ?
C48 C47 H47A 108.8 . . ?
C47 C47 H47B 108.8 7_565 . ?
C48 C47 H47B 108.8 . . ?
H47A C47 H47B 107.7 . . ?
C49 C48 C47 114(2) . . ?
C49 C48 H48A 108.7 . . ?
C47 C48 H48A 108.7 . . ?
C49 C48 H48B 108.7 . . ?
C47 C48 H48B 108.7 . . ?
H48A C48 H48B 107.6 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C4 N1 C2 122.5(5) . . ?
C4 N1 U1 100.3(3) . . ?
C2 N1 U1 136.0(3) . . ?
C4 N2 C9 117.2(5) . . ?
C4 N2 C6 117.5(5) . . ?
C9 N2 C6 125.3(5) . . ?
C4 N3 C12 119.4(5) . . ?
C4 N3 U1 90.9(3) . . ?
C12 N3 U1 143.4(4) . . ?
C17 N4 C15 123.9(5) . . ?
C17 N4 U1 97.7(4) . . ?
C15 N4 U1 138.0(4) . . ?
C19 N5 C17 116.6(8) . . ?
C19 N5 C22 121.2(6) . . ?
C17 N5 C22 119.0(6) . . ?
C17 N6 C25 123.2(5) . . ?
C17 N6 U1 96.7(4) . . ?
C25 N6 U1 139.1(4) . . ?
C30 N7 C28 118.8(5) . . ?
C30 N7 U1 99.1(4) . . ?
C28 N7 U1 141.5(4) . . ?
C30 N8 C32 121.0(5) . . ?
C30 N8 C35 115.8(5) . . ?
C32 N8 C35 120.7(5) . . ?
C30 N9 C38 120.3(5) . . ?
C30 N9 U1 95.5(4) . . ?
C38 N9 U1 143.7(4) . . ?
C40 N10 U1 172.6(4) . . ?
N10 U1 N1 86.58(17) . . ?
N10 U1 N4 84.73(19) . . ?
N1 U1 N4 102.51(16) . . ?
N10 U1 N7 79.35(19) . . ?
N1 U1 N7 123.8(2) . . ?
N4 U1 N7 129.40(19) . . ?
N10 U1 N6 113.3(2) . . ?
N1 U1 N6 144.1(2) . . ?
N4 U1 N6 53.34(17) . . ?
N7 U1 N6 90.2(2) . . ?
N10 U1 N9 123.8(2) . . ?
N1 U1 N9 96.41(18) . . ?
N4 U1 N9 146.8(2) . . ?
N7 U1 N9 52.73(18) . . ?
N6 U1 N9 96.3(2) . . ?
N10 U1 N3 135.05(16) . . ?
N1 U1 N3 53.56(15) . . ?
N4 U1 N3 84.90(16) . . ?
N7 U1 N3 137.51(17) . . ?
N6 U1 N3 94.5(2) . . ?
N9 U1 N3 84.78(16) . . ?
N10 U1 C17 99.0(2) . . ?
N1 U1 C17 125.35(17) . . ?
N4 U1 C17 26.44(16) . . ?
N7 U1 C17 110.6(2) . . ?
N6 U1 C17 26.92(17) . . ?
N9 U1 C17 122.4(2) . . ?
N3 U1 C17 90.43(18) . . ?
N10 U1 C4 110.58(17) . . ?
N1 U1 C4 26.74(16) . . ?
N4 U1 C4 92.71(16) . . ?
N7 U1 C4 137.86(19) . . ?
N6 U1 C4 119.4(2) . . ?
N9 U1 C4 92.16(16) . . ?
N3 U1 C4 26.90(15) . . ?
C17 U1 C4 108.09(18) . . ?
N10 U1 C30 101.03(18) . . ?
N1 U1 C30 111.21(16) . . ?
N4 U1 C30 146.01(15) . . ?
N7 U1 C30 25.97(17) . . ?
N6 U1 C30 94.62(16) . . ?
N9 U1 C30 26.80(17) . . ?
N3 U1 C30 111.57(16) . . ?
C17 U1 C30 120.62(16) . . ?
C4 U1 C30 115.62(16) . . ?

_refine_diff_density_max         1.850
_refine_diff_density_min         -1.266
_refine_diff_density_rms         0.125


_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_UO(TIG)3
_database_code_depnum_ccdc_archive 'CCDC 1860830'
_audit_update_record             
;
2018-08-07 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            UO(TIG)3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H84 N9 O U'
_chemical_formula_weight         933.18

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'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   19.9133(19)
_cell_length_b                   12.7998(16)
_cell_length_c                   19.1902(16)
_cell_angle_alpha                90
_cell_angle_beta                 109.856(4)
_cell_angle_gamma                90
_cell_volume                     4600.5(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9661
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      26.40

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_F_000             1924
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    3.566
_shelx_estimated_absorpt_T_min   0.469
_shelx_estimated_absorpt_T_max   0.763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.366
_exptl_absorpt_correction_T_max  0.491
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            109654
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.927
_diffrn_reflns_theta_max         26.409
_diffrn_reflns_theta_full        26.409
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             9404
_reflns_number_gt                8329
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury 3.10'
_computing_publication_material  WinGX
_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)+(0.0130P)²+4.6893P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9404
_refine_ls_number_parameters     475
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0184
_refine_ls_wR_factor_ref         0.0427
_refine_ls_wR_factor_gt          0.0404
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.004
_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
C1 C 0.73235(12) 0.61517(19) 0.07840(13) 0.0226(5) Uani 1 1 d . . . . .
H1A H 0.7594 0.6770 0.1024 0.034 Uiso 1 1 calc R U . . .
H1B H 0.7325 0.6102 0.0275 0.034 Uiso 1 1 calc R U . . .
H1C H 0.7545 0.5525 0.1060 0.034 Uiso 1 1 calc R U . . .
C2 C 0.65591(12) 0.62416(18) 0.07735(12) 0.0169(5) Uani 1 1 d . . . . .
H2 H 0.6338 0.6893 0.0505 0.020 Uiso 1 1 calc R U . . .
C3 C 0.61569(14) 0.5284(2) 0.03488(13) 0.0263(6) Uani 1 1 d . . . . .
H3A H 0.6365 0.4646 0.0618 0.040 Uiso 1 1 calc R U . . .
H3B H 0.6196 0.5267 -0.0146 0.040 Uiso 1 1 calc R U . . .
H3C H 0.5653 0.5329 0.0304 0.040 Uiso 1 1 calc R U . . .
C4 C 0.62084(11) 0.70110(16) 0.17836(12) 0.0140(4) Uani 1 1 d . . . . .
C5 C 0.47787(15) 0.7419(2) -0.00034(15) 0.0346(6) Uani 1 1 d . . . . .
H5A H 0.4590 0.8131 -0.0040 0.052 Uiso 1 1 calc R U . . .
H5B H 0.4404 0.6948 -0.0303 0.052 Uiso 1 1 calc R U . . .
H5C H 0.5183 0.7404 -0.0185 0.052 Uiso 1 1 calc R U . . .
C6 C 0.50280(13) 0.7065(2) 0.08051(13) 0.0251(5) Uani 1 1 d . . . . .
H6 H 0.5179 0.6321 0.0802 0.030 Uiso 1 1 calc R U . . .
C7 C 0.44067(14) 0.7047(2) 0.11001(17) 0.0382(7) Uani 1 1 d . . . . .
H7A H 0.4578 0.6815 0.1617 0.057 Uiso 1 1 calc R U . . .
H7B H 0.4039 0.6565 0.0802 0.057 Uiso 1 1 calc R U . . .
H7C H 0.4205 0.7751 0.1070 0.057 Uiso 1 1 calc R U . . .
C8 C 0.59934(15) 0.9192(2) 0.07179(16) 0.0329(6) Uani 1 1 d . . . . .
H8A H 0.6429 0.8827 0.0728 0.049 Uiso 1 1 calc R U . . .
H8B H 0.6093 0.9941 0.0798 0.049 Uiso 1 1 calc R U . . .
H8C H 0.5621 0.9085 0.0235 0.049 Uiso 1 1 calc R U . . .
C9 C 0.57404(13) 0.87617(18) 0.13299(14) 0.0245(5) Uani 1 1 d . . . . .
H9 H 0.6132 0.8915 0.1807 0.029 Uiso 1 1 calc R U . . .
C10 C 0.50892(16) 0.9379(2) 0.13547(16) 0.0373(7) Uani 1 1 d . . . . .
H10A H 0.4695 0.9288 0.0886 0.056 Uiso 1 1 calc R U . . .
H10B H 0.5212 1.0122 0.1431 0.056 Uiso 1 1 calc R U . . .
H10C H 0.4945 0.9122 0.1764 0.056 Uiso 1 1 calc R U . . .
C11 C 0.57071(14) 0.6766(2) 0.33063(15) 0.0312(6) Uani 1 1 d . . . . .
H11A H 0.5425 0.6252 0.2946 0.047 Uiso 1 1 calc R U . . .
H11B H 0.5404 0.7103 0.3550 0.047 Uiso 1 1 calc R U . . .
H11C H 0.6106 0.6413 0.3679 0.047 Uiso 1 1 calc R U . . .
C12 C 0.59957(12) 0.75868(18) 0.29088(13) 0.0195(5) Uani 1 1 d . . . . .
H12 H 0.5583 0.7946 0.2536 0.023 Uiso 1 1 calc R U . . .
C13 C 0.64385(14) 0.8400(2) 0.34476(14) 0.0317(6) Uani 1 1 d . . . . .
H13A H 0.6862 0.8066 0.3798 0.047 Uiso 1 1 calc R U . . .
H13B H 0.6152 0.8712 0.3720 0.047 Uiso 1 1 calc R U . . .
H13C H 0.6587 0.8945 0.3173 0.047 Uiso 1 1 calc R U . . .
C14 C 0.77053(12) 0.86120(17) 0.21535(12) 0.0183(5) Uani 1 1 d . . . . .
H14A H 0.7441 0.8144 0.1749 0.027 Uiso 1 1 calc R U . . .
H14B H 0.7808 0.9268 0.1947 0.027 Uiso 1 1 calc R U . . .
H14C H 0.7418 0.8757 0.2468 0.027 Uiso 1 1 calc R U . . .
C15 C 0.84045(11) 0.80926(16) 0.26155(12) 0.0143(4) Uani 1 1 d . . . . .
H15 H 0.8655 0.8577 0.3032 0.017 Uiso 1 1 calc R U . . .
C16 C 0.88863(12) 0.79441(18) 0.21486(12) 0.0190(5) Uani 1 1 d . . . . .
H16A H 0.9328 0.7593 0.2446 0.028 Uiso 1 1 calc R U . . .
H16B H 0.9001 0.8627 0.1988 0.028 Uiso 1 1 calc R U . . .
H16C H 0.8638 0.7517 0.1713 0.028 Uiso 1 1 calc R U . . .
C17 C 0.84076(11) 0.70853(16) 0.36807(11) 0.0122(4) Uani 1 1 d . . . . .
C18 C 0.91624(14) 0.84393(19) 0.54794(13) 0.0257(6) Uani 1 1 d . . . . .
H18A H 0.9284 0.7727 0.5666 0.038 Uiso 1 1 calc R U . . .
H18B H 0.8931 0.8805 0.5785 0.038 Uiso 1 1 calc R U . . .
H18C H 0.9599 0.8812 0.5500 0.038 Uiso 1 1 calc R U . . .
C19 C 0.86548(12) 0.83983(17) 0.46793(12) 0.0175(5) Uani 1 1 d . . . . .
H19 H 0.8210 0.8055 0.4697 0.021 Uiso 1 1 calc R U . . .
C20 C 0.84330(13) 0.95053(17) 0.43770(14) 0.0232(5) Uani 1 1 d . . . . .
H20A H 0.8856 0.9896 0.4376 0.035 Uiso 1 1 calc R U . . .
H20B H 0.8209 0.9865 0.4692 0.035 Uiso 1 1 calc R U . . .
H20C H 0.8093 0.9460 0.3870 0.035 Uiso 1 1 calc R U . . .
C21 C 1.01402(12) 0.70819(18) 0.47466(13) 0.0223(5) Uani 1 1 d . . . . .
H21A H 1.0238 0.7412 0.5232 0.034 Uiso 1 1 calc R U . . .
H21B H 1.0589 0.6996 0.4647 0.034 Uiso 1 1 calc R U . . .
H21C H 0.9921 0.6396 0.4745 0.034 Uiso 1 1 calc R U . . .
C22 C 0.96299(11) 0.77731(17) 0.41454(12) 0.0157(5) Uani 1 1 d . . . . .
H22 H 0.9598 0.7448 0.3661 0.019 Uiso 1 1 calc R U . . .
C23 C 0.99568(12) 0.88549(18) 0.41512(14) 0.0221(5) Uani 1 1 d . . . . .
H23A H 0.9637 0.9278 0.3750 0.033 Uiso 1 1 calc R U . . .
H23B H 1.0420 0.8784 0.4080 0.033 Uiso 1 1 calc R U . . .
H23C H 1.0024 0.9196 0.4627 0.033 Uiso 1 1 calc R U . . .
C24 C 0.76106(13) 0.61673(18) 0.49650(12) 0.0208(5) Uani 1 1 d . . . . .
H24A H 0.7458 0.6899 0.4904 0.031 Uiso 1 1 calc R U . . .
H24B H 0.7756 0.5975 0.5490 0.031 Uiso 1 1 calc R U . . .
H24C H 0.7214 0.5720 0.4677 0.031 Uiso 1 1 calc R U . . .
C25 C 0.82408(12) 0.60227(17) 0.46907(12) 0.0166(5) Uani 1 1 d . . . . .
H25 H 0.8647 0.6463 0.5001 0.020 Uiso 1 1 calc R U . . .
C26 C 0.84736(14) 0.48813(18) 0.47757(13) 0.0252(5) Uani 1 1 d . . . . .
H26A H 0.8081 0.4443 0.4469 0.038 Uiso 1 1 calc R U . . .
H26B H 0.8601 0.4673 0.5296 0.038 Uiso 1 1 calc R U . . .
H26C H 0.8889 0.4795 0.4616 0.038 Uiso 1 1 calc R U . . .
C27 C 0.90684(12) 0.50827(18) 0.20663(13) 0.0201(5) Uani 1 1 d . . . . .
H27A H 0.8759 0.4825 0.1583 0.030 Uiso 1 1 calc R U . . .
H27B H 0.9567 0.5064 0.2088 0.030 Uiso 1 1 calc R U . . .
H27C H 0.8935 0.5802 0.2136 0.030 Uiso 1 1 calc R U . . .
C28 C 0.89805(11) 0.43942(16) 0.26759(12) 0.0155(4) Uani 1 1 d . . . . .
H28 H 0.9106 0.3660 0.2591 0.019 Uiso 1 1 calc R U . . .
C29 C 0.94819(12) 0.47546(19) 0.34278(13) 0.0210(5) Uani 1 1 d . . . . .
H29A H 0.9352 0.5464 0.3527 0.031 Uiso 1 1 calc R U . . .
H29B H 0.9974 0.4752 0.3428 0.031 Uiso 1 1 calc R U . . .
H29C H 0.9443 0.4280 0.3813 0.031 Uiso 1 1 calc R U . . .
C30 C 0.77571(11) 0.37345(16) 0.22524(11) 0.0130(4) Uani 1 1 d . . . . .
C31 C 0.72266(14) 0.15040(19) 0.10050(15) 0.0289(6) Uani 1 1 d . . . . .
H31A H 0.7601 0.0969 0.1120 0.043 Uiso 1 1 calc R U . . .
H31B H 0.6936 0.1464 0.0479 0.043 Uiso 1 1 calc R U . . .
H31C H 0.6923 0.1385 0.1306 0.043 Uiso 1 1 calc R U . . .
C32 C 0.75701(13) 0.25850(18) 0.11772(13) 0.0203(5) Uani 1 1 d . . . . .
H32 H 0.7171 0.3102 0.1009 0.024 Uiso 1 1 calc R U . . .
C33 C 0.80476(15) 0.2790(2) 0.07099(15) 0.0339(6) Uani 1 1 d . . . . .
H33A H 0.8235 0.3504 0.0798 0.051 Uiso 1 1 calc R U . . .
H33B H 0.7767 0.2704 0.0184 0.051 Uiso 1 1 calc R U . . .
H33C H 0.8446 0.2293 0.0849 0.051 Uiso 1 1 calc R U . . .
C34 C 0.89340(15) 0.1471(2) 0.22989(19) 0.0440(8) Uani 1 1 d . . . . .
H34A H 0.8778 0.1223 0.1785 0.066 Uiso 1 1 calc R U . . .
H34B H 0.9136 0.0886 0.2635 0.066 Uiso 1 1 calc R U . . .
H34C H 0.9298 0.2014 0.2368 0.066 Uiso 1 1 calc R U . . .
C35 C 0.82948(13) 0.19226(18) 0.24681(14) 0.0274(6) Uani 1 1 d . . . . .
H35 H 0.7933 0.1350 0.2373 0.033 Uiso 1 1 calc R U . . .
C36 C 0.85057(15) 0.21926(19) 0.32868(15) 0.0348(7) Uani 1 1 d . . . . .
H36A H 0.8895 0.2704 0.3418 0.052 Uiso 1 1 calc R U . . .
H36B H 0.8664 0.1559 0.3584 0.052 Uiso 1 1 calc R U . . .
H36C H 0.8094 0.2489 0.3386 0.052 Uiso 1 1 calc R U . . .
C37 C 0.57985(12) 0.39663(18) 0.18636(14) 0.0221(5) Uani 1 1 d . . . . .
H37A H 0.5836 0.4289 0.2338 0.033 Uiso 1 1 calc R U . . .
H37B H 0.5382 0.3504 0.1704 0.033 Uiso 1 1 calc R U . . .
H37C H 0.5746 0.4512 0.1491 0.033 Uiso 1 1 calc R U . . .
C38 C 0.64717(12) 0.33329(17) 0.19534(13) 0.0176(5) Uani 1 1 d . . . . .
H38 H 0.6408 0.2954 0.1479 0.021 Uiso 1 1 calc R U . . .
C39 C 0.65762(14) 0.25300(19) 0.25698(15) 0.0280(6) Uani 1 1 d . . . . .
H39A H 0.6972 0.2063 0.2587 0.042 Uiso 1 1 calc R U . . .
H39B H 0.6138 0.2121 0.2472 0.042 Uiso 1 1 calc R U . . .
H39C H 0.6686 0.2891 0.3046 0.042 Uiso 1 1 calc R U . . .
N1 N 0.65698(10) 0.62962(14) 0.15409(10) 0.0160(4) Uani 1 1 d . . . . .
N2 N 0.56523(10) 0.76164(14) 0.13018(10) 0.0161(4) Uani 1 1 d . . . . .
N3 N 0.64303(10) 0.70860(14) 0.25182(10) 0.0173(4) Uani 1 1 d . . . . .
N4 N 0.82597(9) 0.71095(13) 0.29448(9) 0.0127(4) Uani 1 1 d . . . . .
N5 N 0.88989(9) 0.77601(13) 0.41723(9) 0.0127(4) Uani 1 1 d . . . . .
N6 N 0.80491(9) 0.63527(13) 0.39126(10) 0.0136(4) Uani 1 1 d . . . . .
N7 N 0.82358(9) 0.44168(13) 0.26590(10) 0.0138(4) Uani 1 1 d . . . . .
N8 N 0.79451(10) 0.27937(14) 0.19752(10) 0.0172(4) Uani 1 1 d . . . . .
N9 N 0.70822(9) 0.40508(13) 0.21009(10) 0.0135(4) Uani 1 1 d . . . . .
O1 O 0.68764(8) 0.50106(12) 0.33479(8) 0.0187(3) Uani 1 1 d . . . . .
U1 U 0.73056(2) 0.56832(2) 0.27689(2) 0.01099(3) 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
C1 C2 1.520(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N1 1.467(3) . ?
C2 C3 1.537(3) . ?
C2 H2 1.0000 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 N3 1.330(3) . ?
C4 N1 1.342(3) . ?
C4 N2 1.409(3) . ?
C4 U1 2.904(2) . ?
C5 C6 1.528(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 N2 1.465(3) . ?
C6 C7 1.526(3) . ?
C6 H6 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.529(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.475(3) . ?
C9 C10 1.533(4) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.522(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N3 1.471(3) . ?
C12 C13 1.520(3) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.526(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 N4 1.480(3) . ?
C15 C16 1.531(3) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N4 1.342(3) . ?
C17 N6 1.343(3) . ?
C17 N5 1.402(3) . ?
C17 U1 2.914(2) . ?
C18 C19 1.526(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 N5 1.474(3) . ?
C19 C20 1.538(3) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.533(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 N5 1.474(3) . ?
C22 C23 1.529(3) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.528(3) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 N6 1.472(3) . ?
C25 C26 1.525(3) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.521(3) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 N7 1.473(3) . ?
C28 C29 1.521(3) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 N7 1.332(3) . ?
C30 N9 1.338(3) . ?
C30 N8 1.417(3) . ?
C30 U1 2.936(2) . ?
C31 C32 1.529(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 N8 1.482(3) . ?
C32 C33 1.535(3) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.530(4) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 N8 1.475(3) . ?
C35 C36 1.522(4) . ?
C35 H35 1.0000 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.526(3) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 N9 1.472(3) . ?
C38 C39 1.527(3) . ?
C38 H38 1.0000 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
N1 U1 2.4434(18) . ?
N3 U1 2.4339(18) . ?
N4 U1 2.5731(17) . ?
N6 U1 2.3529(18) . ?
N7 U1 2.5235(17) . ?
N9 U1 2.4124(17) . ?
O1 U1 1.8307(15) . ?

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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C1 108.49(18) . . ?
N1 C2 C3 113.42(18) . . ?
C1 C2 C3 106.60(19) . . ?
N1 C2 H2 109.4 . . ?
C1 C2 H2 109.4 . . ?
C3 C2 H2 109.4 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N3 C4 N1 113.14(19) . . ?
N3 C4 N2 124.05(19) . . ?
N1 C4 N2 122.81(19) . . ?
N3 C4 U1 56.38(11) . . ?
N1 C4 U1 56.85(11) . . ?
N2 C4 U1 177.27(14) . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C6 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 C7 112.4(2) . . ?
N2 C6 C5 115.4(2) . . ?
C7 C6 C5 110.9(2) . . ?
N2 C6 H6 105.7 . . ?
C7 C6 H6 105.7 . . ?
C5 C6 H6 105.7 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C8 113.3(2) . . ?
N2 C9 C10 115.0(2) . . ?
C8 C9 C10 109.9(2) . . ?
N2 C9 H9 105.9 . . ?
C8 C9 H9 105.9 . . ?
C10 C9 H9 105.9 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 C13 109.83(19) . . ?
N3 C12 C11 110.02(18) . . ?
C13 C12 C11 111.3(2) . . ?
N3 C12 H12 108.6 . . ?
C13 C12 H12 108.6 . . ?
C11 C12 H12 108.6 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N4 C15 C14 110.30(17) . . ?
N4 C15 C16 113.34(17) . . ?
C14 C15 C16 110.10(18) . . ?
N4 C15 H15 107.6 . . ?
C14 C15 H15 107.6 . . ?
C16 C15 H15 107.6 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 N6 114.45(18) . . ?
N4 C17 N5 123.19(18) . . ?
N6 C17 N5 122.36(18) . . ?
N4 C17 U1 62.02(11) . . ?
N6 C17 U1 52.57(10) . . ?
N5 C17 U1 173.99(14) . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C19 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N5 C19 C18 115.41(19) . . ?
N5 C19 C20 112.24(18) . . ?
C18 C19 C20 110.80(19) . . ?
N5 C19 H19 105.9 . . ?
C18 C19 H19 105.9 . . ?
C20 C19 H19 105.9 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N5 C22 C23 115.67(18) . . ?
N5 C22 C21 112.16(17) . . ?
C23 C22 C21 110.21(18) . . ?
N5 C22 H22 106.0 . . ?
C23 C22 H22 106.0 . . ?
C21 C22 H22 106.0 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C25 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N6 C25 C26 110.37(18) . . ?
N6 C25 C24 110.76(18) . . ?
C26 C25 C24 109.56(18) . . ?
N6 C25 H25 108.7 . . ?
C26 C25 H25 108.7 . . ?
C24 C25 H25 108.7 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C28 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N7 C28 C29 110.29(18) . . ?
N7 C28 C27 110.47(18) . . ?
C29 C28 C27 110.11(18) . . ?
N7 C28 H28 108.6 . . ?
C29 C28 H28 108.6 . . ?
C27 C28 H28 108.6 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N7 C30 N9 113.27(18) . . ?
N7 C30 N8 123.31(19) . . ?
N9 C30 N8 123.34(19) . . ?
N7 C30 U1 59.04(11) . . ?
N9 C30 U1 54.26(10) . . ?
N8 C30 U1 177.36(15) . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N8 C32 C31 114.7(2) . . ?
N8 C32 C33 112.22(19) . . ?
C31 C32 C33 110.42(19) . . ?
N8 C32 H32 106.3 . . ?
C31 C32 H32 106.3 . . ?
C33 C32 H32 106.3 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C35 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N8 C35 C36 113.27(19) . . ?
N8 C35 C34 113.3(2) . . ?
C36 C35 C34 110.3(2) . . ?
N8 C35 H35 106.5 . . ?
C36 C35 H35 106.5 . . ?
C34 C35 H35 106.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N9 C38 C37 109.06(17) . . ?
N9 C38 C39 112.62(19) . . ?
C37 C38 C39 109.17(19) . . ?
N9 C38 H38 108.6 . . ?
C37 C38 H38 108.6 . . ?
C39 C38 H38 108.6 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C4 N1 C2 123.66(18) . . ?
C4 N1 U1 95.79(13) . . ?
C2 N1 U1 138.79(14) . . ?
C4 N2 C6 117.79(18) . . ?
C4 N2 C9 117.73(18) . . ?
C6 N2 C9 124.49(18) . . ?
C4 N3 C12 122.04(18) . . ?
C4 N3 U1 96.55(13) . . ?
C12 N3 U1 136.62(14) . . ?
C17 N4 C15 117.67(17) . . ?
C17 N4 U1 90.57(12) . . ?
C15 N4 U1 142.15(13) . . ?
C17 N5 C19 118.31(17) . . ?
C17 N5 C22 117.07(16) . . ?
C19 N5 C22 124.62(17) . . ?
C17 N6 C25 123.57(18) . . ?
C17 N6 U1 100.49(13) . . ?
C25 N6 U1 134.90(13) . . ?
C30 N7 C28 120.99(17) . . ?
C30 N7 U1 94.05(13) . . ?
C28 N7 U1 140.63(13) . . ?
C30 N8 C35 121.93(18) . . ?
C30 N8 C32 115.87(17) . . ?
C35 N8 C32 119.26(18) . . ?
C30 N9 C38 123.77(18) . . ?
C30 N9 U1 98.99(13) . . ?
C38 N9 U1 129.34(13) . . ?
O1 U1 N6 83.15(6) . . ?
O1 U1 N9 82.83(6) . . ?
N6 U1 N9 139.04(6) . . ?
O1 U1 N3 90.93(6) . . ?
N6 U1 N3 95.58(6) . . ?
N9 U1 N3 122.92(6) . . ?
O1 U1 N1 119.06(7) . . ?
N6 U1 N1 139.81(6) . . ?
N9 U1 N1 79.85(6) . . ?
N3 U1 N1 54.40(6) . . ?
O1 U1 N7 104.83(6) . . ?
N6 U1 N7 93.71(6) . . ?
N9 U1 N7 53.66(6) . . ?
N3 U1 N7 162.56(6) . . ?
N1 U1 N7 110.02(6) . . ?
O1 U1 N4 136.91(6) . . ?
N6 U1 N4 54.31(6) . . ?
N9 U1 N4 132.76(6) . . ?
N3 U1 N4 87.12(6) . . ?
N1 U1 N4 94.18(6) . . ?
N7 U1 N4 86.36(6) . . ?
O1 U1 C4 105.50(6) . . ?
N6 U1 C4 119.35(6) . . ?
N9 U1 C4 101.46(6) . . ?
N3 U1 C4 27.06(6) . . ?
N1 U1 C4 27.36(6) . . ?
N7 U1 C4 137.13(6) . . ?
N4 U1 C4 91.66(6) . . ?
O1 U1 C17 109.68(6) . . ?
N6 U1 C17 26.94(6) . . ?
N9 U1 C17 144.88(6) . . ?
N3 U1 C17 90.40(6) . . ?
N1 U1 C17 117.65(6) . . ?
N7 U1 C17 91.23(6) . . ?
N4 U1 C17 27.41(5) . . ?
C4 U1 C17 106.09(6) . . ?
O1 U1 C30 93.73(6) . . ?
N6 U1 C30 117.17(6) . . ?
N9 U1 C30 26.75(6) . . ?
N3 U1 C30 147.24(6) . . ?
N1 U1 C30 95.70(6) . . ?
N7 U1 C30 26.91(6) . . ?
N4 U1 C30 110.49(6) . . ?
C4 U1 C30 121.77(6) . . ?
C17 U1 C30 118.14(6) . . ?

_refine_diff_density_max         0.682
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.070


_chemical_properties_physical    Air-sensitive,Moisture-sensitive
