# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_to355_refinalised
_database_code_depnum_ccdc_archive 'CCDC 2313497'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2023-12-11 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_audit_creation_date             2023-11-24
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            '[UO2(HL)]2'
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72 H96 N12 O4 U2, 2(C7 H8)'
_chemical_formula_sum            'C86 H112 N12 O4 U2'
_chemical_formula_weight         1853.93
_chemical_melting_point          ?
_chemical_oxdiff_formula         C36H47UO2N6
_chemical_oxdiff_usercomment     'Slow precip toluene'
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   14.6782(2)
_cell_length_b                   16.9971(2)
_cell_length_c                   18.3318(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.9870(10)
_cell_angle_gamma                90
_cell_volume                     4570.79(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    23869
_cell_measurement_temperature    120.0(7)
_cell_measurement_theta_max      29.3740
_cell_measurement_theta_min      3.7580
_shelx_estimated_absorpt_T_max   0.673
_shelx_estimated_absorpt_T_min   0.402
_exptl_absorpt_coefficient_mu    3.589
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 18 -17 0.1334
0 18 17 0.1136
0 -19 16 0.1344
0 -18 -17 0.1406
21 -1 2 0.0493
1 -8 24 0.1726
-20 1 -3 0.0693
-14 12 -12 0.1144
-13 -13 -14 0.1094
-20 -4 -3 0.0706
-19 -7 6 0.0954
-21 0 1 0.0607
-20 6 4 0.0738

_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.4137 17.9419 -17.1434 -0.1101 -0.4618 0.8801
-0.4474 18.1151 16.9273 -0.2181 -0.9091 -0.3548
-0.3941 -18.5337 16.3946 0.1178 0.4940 -0.8614
0.4550 -17.8620 -17.2373 0.2167 0.9035 0.3697
20.5697 -0.5830 1.7451 0.9697 -0.2324 -0.0752
0.7996 -8.2074 24.2211 0.0652 -0.0164 -0.9977
-20.4306 1.0082 -2.9997 -0.9646 0.2312 0.1269
-14.4912 12.2603 -12.2338 -0.7693 -0.1424 0.6228
-12.7403 -13.2095 -13.9985 -0.4526 0.8319 0.3211
-20.1334 -4.4032 -2.6718 -0.9022 0.4298 0.0373
-19.1993 -7.2130 6.4678 -0.8504 0.4055 -0.3352
-20.6784 -0.4084 1.1806 -0.9715 0.2328 -0.0453
-19.7416 6.4672 4.1229 -0.9955 -0.0787 -0.0536

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            51279
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.383
_diffrn_reflns_theta_min         3.498
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -53.00  23.00   1.00   12.50    --  -15.82  97.00 130.00   76
  2  ω    -23.00  54.00   1.00   12.50    --   17.54 -97.00  22.00   77
  3  ω    -30.00   5.00   1.00   12.50    --  -15.82  77.00   0.00   35
  4  ω    -88.00 -43.00   1.00   12.50    --  -15.82-178.00-180.00   45
  5  ω     35.00  90.00   1.00   12.50    --   17.54-178.00 -60.00   55
  6  ω     -9.00  36.00   1.00   12.50    --   17.54  77.00 -60.00   45
  7  ω     39.00  88.00   1.00   12.50    --   17.54 178.00  90.00   49
  8  ω      1.00  83.00   1.00   12.50    --   17.54  57.00-180.00   82
  9  ω     -9.00  39.00   1.00   12.50    --   17.54  77.00  30.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0470492000
_diffrn_orient_matrix_UB_12      -0.0090694000
_diffrn_orient_matrix_UB_13      -0.0019336000
_diffrn_orient_matrix_UB_21      -0.0112580000
_diffrn_orient_matrix_UB_22      -0.0381108000
_diffrn_orient_matrix_UB_23      -0.0132210000
_diffrn_orient_matrix_UB_31      -0.0001690000
_diffrn_orient_matrix_UB_32      0.0143505000
_diffrn_orient_matrix_UB_33      -0.0363245000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9250
_reflns_number_total             11102
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         11102
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0239
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0222P)²+4.6936P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0538
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9), C20(H20), C31(H31)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C2(H2A,H2B), C36(H36A,H36B), C34(H34A,H34B), C35(H35A,H35B),
 C10(H10A,H10B), C13(H13A,H13B), C25(H25A,H25B), C11(H11A,H11B), C32(H32A,H32B),
  C12(H12A,H12B), C21(H21A,H21B), C24(H24A,H24B), C33(H33A,H33B), C23(H23A,
 H23B), C22(H22A,H22B)
2.c Me refined with riding coordinates:
 C37(H37A,H37B,H37C)
2.d Aromatic/amide H refined with riding coordinates:
 N1(H1), C30(H30), C8(H8), C19(H19), C28(H28), C16(H16), C17(H17), C27(H27),
 C6(H6), C5(H5), C43(H43), C40(H40), C39(H39), C42(H42), C41(H41)
2.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.61091(2) 0.61964(2) 0.44228(2) 0.01187(3) Uani 1 1 d . . . . .
N2 N 0.33042(13) 0.27247(12) 0.46270(11) 0.0141(4) Uani 1 1 d . . . . .
N3 N 0.65517(14) 0.50095(12) 0.37615(11) 0.0149(4) Uani 1 1 d . . . . .
N5 N 0.49127(14) 0.58354(12) 0.35285(11) 0.0148(4) Uani 1 1 d . . . . .
N6 N 0.47501(14) 0.71323(12) 0.45018(11) 0.0162(4) Uani 1 1 d . . . . .
N4 N 0.76736(14) 0.57061(13) 0.48719(11) 0.0179(5) Uani 1 1 d . . . . .
N1 N 0.44135(14) 0.36668(12) 0.34936(11) 0.0146(4) Uani 1 1 d . . . . .
H1 H 0.445822 0.394693 0.389694 0.018 Uiso 1 1 calc R U . . .
C15 C 0.62213(16) 0.45192(14) 0.32376(13) 0.0145(5) Uani 1 1 d . . . . .
C18 C 0.73881(17) 0.46957(15) 0.39926(14) 0.0181(5) Uani 1 1 d . . . . .
C9 C 0.26929(17) 0.21746(15) 0.50191(14) 0.0176(5) Uani 1 1 d . . . . .
H9 H 0.234768 0.250424 0.536709 0.021 Uiso 1 1 calc R U . . .
C26 C 0.47202(17) 0.52818(14) 0.30178(13) 0.0152(5) Uani 1 1 d . . . . .
C3 C 0.53407(17) 0.46157(14) 0.27936(13) 0.0145(5) Uani 1 1 d . . . . .
C30 C 0.41022(17) 0.69536(15) 0.40290(14) 0.0184(5) Uani 1 1 d . . . . .
H30 H 0.356368 0.726400 0.402024 0.022 Uiso 1 1 calc R U . . .
C29 C 0.41517(17) 0.63280(15) 0.35298(14) 0.0182(5) Uani 1 1 d . . . . .
C20 C 0.82625(18) 0.59769(16) 0.54914(14) 0.0208(6) Uani 1 1 d . . . . .
H20 H 0.801993 0.650004 0.564141 0.025 Uiso 1 1 calc R U . . .
C14 C 0.32576(18) 0.15944(15) 0.54852(14) 0.0201(5) Uani 1 1 d . . . . .
H14A H 0.356553 0.121754 0.516383 0.024 Uiso 1 1 calc R U . . .
H14B H 0.373253 0.188397 0.577243 0.024 Uiso 1 1 calc R U . . .
C8 C 0.34171(16) 0.25687(14) 0.39453(13) 0.0155(5) Uani 1 1 d . . . . .
H8 H 0.310324 0.211496 0.376771 0.019 Uiso 1 1 calc R U . . .
C19 C 0.79158(17) 0.50612(15) 0.45540(14) 0.0196(5) Uani 1 1 d . . . . .
H19 H 0.847613 0.482317 0.470672 0.023 Uiso 1 1 calc R U . . .
C4 C 0.48026(16) 0.38580(14) 0.28556(13) 0.0149(5) Uani 1 1 d . . . . .
C31 C 0.45263(17) 0.77492(15) 0.50381(13) 0.0163(5) Uani 1 1 d . . . . .
H31 H 0.509049 0.784730 0.534617 0.020 Uiso 1 1 calc R U . . .
C7 C 0.39386(17) 0.29703(15) 0.34175(13) 0.0158(5) Uani 1 1 d . . . . .
C2 C 0.55762(18) 0.47388(15) 0.19785(13) 0.0185(5) Uani 1 1 d . . . . .
H2A H 0.594448 0.428757 0.181615 0.022 Uiso 1 1 calc R U . . .
H2B H 0.500380 0.474769 0.167661 0.022 Uiso 1 1 calc R U . . .
C28 C 0.34967(18) 0.60694(16) 0.30144(15) 0.0224(6) Uani 1 1 d . . . . .
H28 H 0.292054 0.630322 0.290360 0.027 Uiso 1 1 calc R U . . .
C16 C 0.68266(18) 0.38955(15) 0.31294(14) 0.0194(5) Uani 1 1 d . . . . .
H16 H 0.674379 0.347427 0.279303 0.023 Uiso 1 1 calc R U . . .
C36 C 0.42441(18) 0.85368(15) 0.46931(14) 0.0196(5) Uani 1 1 d . . . . .
H36A H 0.473510 0.872822 0.438146 0.023 Uiso 1 1 calc R U . . .
H36B H 0.368749 0.846248 0.438015 0.023 Uiso 1 1 calc R U . . .
C17 C 0.75666(18) 0.40092(16) 0.36044(15) 0.0220(6) Uani 1 1 d . . . . .
H17 H 0.809201 0.368486 0.365634 0.026 Uiso 1 1 calc R U . . .
C34 C 0.3333(2) 0.88556(17) 0.57929(15) 0.0274(6) Uani 1 1 d . . . . .
H34A H 0.324699 0.924909 0.618270 0.033 Uiso 1 1 calc R U . . .
H34B H 0.274601 0.879453 0.551620 0.033 Uiso 1 1 calc R U . . .
C27 C 0.38540(18) 0.54053(16) 0.26977(14) 0.0205(6) Uani 1 1 d . . . . .
H27 H 0.356419 0.509033 0.232984 0.025 Uiso 1 1 calc R U . . .
C35 C 0.4061(2) 0.91467(16) 0.52810(15) 0.0235(6) Uani 1 1 d . . . . .
H35A H 0.385541 0.964397 0.504726 0.028 Uiso 1 1 calc R U . . .
H35B H 0.463216 0.925504 0.556636 0.028 Uiso 1 1 calc R U . . .
C6 C 0.40407(19) 0.27243(16) 0.27028(14) 0.0210(6) Uani 1 1 d . . . . .
H6 H 0.378367 0.226308 0.248739 0.025 Uiso 1 1 calc R U . . .
C10 C 0.19811(18) 0.17197(16) 0.45619(15) 0.0224(6) Uani 1 1 d . . . . .
H10A H 0.228588 0.133428 0.424721 0.027 Uiso 1 1 calc R U . . .
H10B H 0.162541 0.208694 0.424428 0.027 Uiso 1 1 calc R U . . .
C38 C 0.8571(2) 0.23245(18) 0.59049(17) 0.0315(7) Uani 1 1 d . . . . .
C13 C 0.2651(2) 0.11466(17) 0.60005(16) 0.0278(6) Uani 1 1 d . . . . .
H13A H 0.239490 0.151791 0.635548 0.033 Uiso 1 1 calc R U . . .
H13B H 0.302127 0.075282 0.627653 0.033 Uiso 1 1 calc R U . . .
C25 C 0.9253(2) 0.6113(2) 0.52798(18) 0.0347(7) Uani 1 1 d . . . . .
H25A H 0.926856 0.649779 0.487469 0.042 Uiso 1 1 calc R U . . .
H25B H 0.951876 0.561324 0.511070 0.042 Uiso 1 1 calc R U . . .
C1 C 0.6101(2) 0.54974(17) 0.18520(15) 0.0262(6) Uani 1 1 d . . . . .
H1A H 0.625660 0.553209 0.133746 0.039 Uiso 1 1 calc R U . . .
H1B H 0.666108 0.549891 0.215887 0.039 Uiso 1 1 calc R U . . .
H1C H 0.572254 0.594906 0.197837 0.039 Uiso 1 1 calc R U . . .
C5 C 0.45857(19) 0.32712(15) 0.23559(14) 0.0207(6) Uani 1 1 d . . . . .
H5 H 0.477394 0.324568 0.186588 0.025 Uiso 1 1 calc R U . . .
C43 C 0.8959(2) 0.1858(2) 0.53772(17) 0.0335(7) Uani 1 1 d . . . . .
H43 H 0.925185 0.210304 0.498241 0.040 Uiso 1 1 calc R U . . .
C40 C 0.8121(2) 0.1135(2) 0.65231(17) 0.0358(7) Uani 1 1 d . . . . .
H40 H 0.783250 0.088900 0.691881 0.043 Uiso 1 1 calc R U . . .
C39 C 0.8155(2) 0.19485(19) 0.64807(18) 0.0341(7) Uani 1 1 d . . . . .
H39 H 0.788984 0.225526 0.685090 0.041 Uiso 1 1 calc R U . . .
C11 C 0.13470(19) 0.12927(17) 0.50735(17) 0.0291(7) Uani 1 1 d . . . . .
H11A H 0.102256 0.168404 0.536873 0.035 Uiso 1 1 calc R U . . .
H11B H 0.088577 0.099330 0.478078 0.035 Uiso 1 1 calc R U . . .
C32 C 0.37941(18) 0.74603(16) 0.55479(14) 0.0215(6) Uani 1 1 d . . . . .
H32A H 0.322428 0.735244 0.526054 0.026 Uiso 1 1 calc R U . . .
H32B H 0.399713 0.696307 0.578315 0.026 Uiso 1 1 calc R U . . .
C12 C 0.1874(2) 0.07310(18) 0.55801(17) 0.0337(7) Uani 1 1 d . . . . .
H12A H 0.212619 0.029700 0.528892 0.040 Uiso 1 1 calc R U . . .
H12B H 0.145177 0.049906 0.593085 0.040 Uiso 1 1 calc R U . . .
C21 C 0.8196(3) 0.5440(2) 0.61466(17) 0.0438(9) Uani 1 1 d . . . . .
H21A H 0.839915 0.490472 0.601538 0.053 Uiso 1 1 calc R U . . .
H21B H 0.755338 0.540716 0.629008 0.053 Uiso 1 1 calc R U . . .
C42 C 0.8930(2) 0.1049(2) 0.54126(18) 0.0351(8) Uani 1 1 d . . . . .
H42 H 0.919805 0.074278 0.504366 0.042 Uiso 1 1 calc R U . . .
C24 C 0.9817(2) 0.6427(2) 0.59423(19) 0.0411(8) Uani 1 1 d . . . . .
H24A H 1.046138 0.648849 0.580873 0.049 Uiso 1 1 calc R U . . .
H24B H 0.958495 0.695104 0.608158 0.049 Uiso 1 1 calc R U . . .
C41 C 0.8509(2) 0.06821(19) 0.59876(17) 0.0341(7) Uani 1 1 d . . . . .
H41 H 0.848667 0.012423 0.601365 0.041 Uiso 1 1 calc R U . . .
C33 C 0.3609(2) 0.80721(17) 0.61340(15) 0.0276(6) Uani 1 1 d . . . . .
H33A H 0.311603 0.788160 0.644400 0.033 Uiso 1 1 calc R U . . .
H33B H 0.416434 0.814485 0.644896 0.033 Uiso 1 1 calc R U . . .
C23 C 0.9765(3) 0.5880(2) 0.6575(2) 0.0524(11) Uani 1 1 d . . . . .
H23A H 1.012525 0.609791 0.699409 0.063 Uiso 1 1 calc R U . . .
H23B H 1.003736 0.536774 0.644453 0.063 Uiso 1 1 calc R U . . .
C22 C 0.8792(3) 0.5750(2) 0.67970(19) 0.0579(12) Uani 1 1 d . . . . .
H22A H 0.853631 0.625112 0.697294 0.069 Uiso 1 1 calc R U . . .
H22B H 0.878428 0.536485 0.720228 0.069 Uiso 1 1 calc R U . . .
C37 C 0.8609(2) 0.3209(2) 0.5861(2) 0.0458(9) Uani 1 1 d . . . . .
H37A H 0.830189 0.343627 0.627733 0.069 Uiso 1 1 calc R U . . .
H37B H 0.924666 0.338042 0.587015 0.069 Uiso 1 1 calc R U . . .
H37C H 0.830316 0.338432 0.540572 0.069 Uiso 1 1 calc R U . . .
O2 O 0.66113(12) 0.67771(10) 0.37434(9) 0.0177(4) Uani 1 1 d . . . . .
O1 O 0.56367(12) 0.56320(10) 0.51303(9) 0.0168(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 N2 2.652(2) 3_666 ?
U1 N3 2.453(2) . ?
U1 N5 2.439(2) . ?
U1 N6 2.559(2) . ?
U1 N4 2.552(2) . ?
U1 O2 1.7698(17) . ?
U1 O1 1.7736(17) . ?
N2 C9 1.497(3) . ?
N2 C8 1.294(3) . ?
N3 C15 1.349(3) . ?
N3 C18 1.391(3) . ?
N5 C26 1.350(3) . ?
N5 C29 1.396(3) . ?
N6 C30 1.300(3) . ?
N6 C31 1.482(3) . ?
N4 C20 1.477(3) . ?
N4 C19 1.297(3) . ?
N1 H1 0.8800 . ?
N1 C4 1.359(3) . ?
N1 C7 1.378(3) . ?
C15 C3 1.512(3) . ?
C15 C16 1.402(3) . ?
C18 C19 1.410(4) . ?
C18 C17 1.396(4) . ?
C9 H9 1.0000 . ?
C9 C14 1.530(3) . ?
C9 C10 1.527(4) . ?
C26 C3 1.519(3) . ?
C26 C27 1.398(3) . ?
C3 C4 1.517(3) . ?
C3 C2 1.560(3) . ?
C30 H30 0.9500 . ?
C30 C29 1.406(4) . ?
C29 C28 1.396(4) . ?
C20 H20 1.0000 . ?
C20 C25 1.535(4) . ?
C20 C21 1.514(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C13 1.524(4) . ?
C8 H8 0.9500 . ?
C8 C7 1.428(3) . ?
C19 H19 0.9500 . ?
C4 C5 1.384(3) . ?
C31 H31 1.0000 . ?
C31 C36 1.531(4) . ?
C31 C32 1.529(3) . ?
C7 C6 1.388(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.524(4) . ?
C28 H28 0.9500 . ?
C28 C27 1.381(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.382(4) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C35 1.526(4) . ?
C17 H17 0.9500 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.529(4) . ?
C34 C33 1.520(4) . ?
C27 H27 0.9500 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C6 H6 0.9500 . ?
C6 C5 1.394(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.527(4) . ?
C38 C43 1.388(4) . ?
C38 C39 1.393(4) . ?
C38 C37 1.506(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C12 1.528(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C24 1.542(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C5 H5 0.9500 . ?
C43 H43 0.9500 . ?
C43 C42 1.377(5) . ?
C40 H40 0.9500 . ?
C40 C39 1.385(4) . ?
C40 C41 1.386(4) . ?
C39 H39 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.524(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.526(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.546(5) . ?
C42 H42 0.9500 . ?
C42 C41 1.389(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C23 1.491(5) . ?
C41 H41 0.9500 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C22 1.515(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 U1 N2 143.88(6) . 3_666 ?
N3 U1 N6 139.42(7) . . ?
N3 U1 N4 68.91(7) . . ?
N5 U1 N2 145.61(6) . 3_666 ?
N5 U1 N3 69.99(7) . . ?
N5 U1 N6 69.51(7) . . ?
N5 U1 N4 138.90(7) . . ?
N6 U1 N2 76.64(6) . 3_666 ?
N4 U1 N2 75.28(6) . 3_666 ?
N4 U1 N6 151.51(7) . . ?
O2 U1 N2 86.73(7) . 3_666 ?
O2 U1 N3 89.26(7) . . ?
O2 U1 N5 88.57(7) . . ?
O2 U1 N6 92.16(7) . . ?
O2 U1 N4 90.98(7) . . ?
O2 U1 O1 177.67(8) . . ?
O1 U1 N2 91.14(7) . 3_666 ?
O1 U1 N3 91.92(7) . . ?
O1 U1 N5 93.72(7) . . ?
O1 U1 N6 88.25(7) . . ?
O1 U1 N4 87.58(7) . . ?
C9 N2 U1 107.63(14) . 3_666 ?
C8 N2 U1 136.60(16) . 3_666 ?
C8 N2 C9 115.8(2) . . ?
C15 N3 U1 139.91(16) . . ?
C15 N3 C18 105.8(2) . . ?
C18 N3 U1 114.26(15) . . ?
C26 N5 U1 140.34(16) . . ?
C26 N5 C29 105.7(2) . . ?
C29 N5 U1 113.92(15) . . ?
C30 N6 U1 111.75(16) . . ?
C30 N6 C31 115.7(2) . . ?
C31 N6 U1 131.95(15) . . ?
C20 N4 U1 129.98(16) . . ?
C19 N4 U1 112.86(16) . . ?
C19 N4 C20 116.5(2) . . ?
C4 N1 H1 124.9 . . ?
C4 N1 C7 110.1(2) . . ?
C7 N1 H1 124.9 . . ?
N3 C15 C3 126.6(2) . . ?
N3 C15 C16 110.7(2) . . ?
C16 C15 C3 122.7(2) . . ?
N3 C18 C19 120.7(2) . . ?
N3 C18 C17 110.1(2) . . ?
C17 C18 C19 129.2(2) . . ?
N2 C9 H9 106.4 . . ?
N2 C9 C14 110.4(2) . . ?
N2 C9 C10 117.6(2) . . ?
C14 C9 H9 106.4 . . ?
C10 C9 H9 106.4 . . ?
C10 C9 C14 109.1(2) . . ?
N5 C26 C3 126.5(2) . . ?
N5 C26 C27 110.6(2) . . ?
C27 C26 C3 122.9(2) . . ?
C15 C3 C26 116.4(2) . . ?
C15 C3 C4 107.8(2) . . ?
C15 C3 C2 108.5(2) . . ?
C26 C3 C2 108.3(2) . . ?
C4 C3 C26 107.1(2) . . ?
C4 C3 C2 108.60(19) . . ?
N6 C30 H30 118.1 . . ?
N6 C30 C29 123.9(2) . . ?
C29 C30 H30 118.1 . . ?
N5 C29 C30 120.9(2) . . ?
C28 C29 N5 110.0(2) . . ?
C28 C29 C30 129.0(2) . . ?
N4 C20 H20 106.5 . . ?
N4 C20 C25 112.8(2) . . ?
N4 C20 C21 111.7(2) . . ?
C25 C20 H20 106.5 . . ?
C21 C20 H20 106.5 . . ?
C21 C20 C25 112.3(3) . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C13 C14 C9 110.6(2) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
N2 C8 H8 114.9 . . ?
N2 C8 C7 130.2(2) . . ?
C7 C8 H8 114.9 . . ?
N4 C19 C18 123.2(2) . . ?
N4 C19 H19 118.4 . . ?
C18 C19 H19 118.4 . . ?
N1 C4 C3 120.2(2) . . ?
N1 C4 C5 107.7(2) . . ?
C5 C4 C3 132.1(2) . . ?
N6 C31 H31 107.1 . . ?
N6 C31 C36 114.0(2) . . ?
N6 C31 C32 110.8(2) . . ?
C36 C31 H31 107.1 . . ?
C32 C31 H31 107.1 . . ?
C32 C31 C36 110.3(2) . . ?
N1 C7 C8 128.5(2) . . ?
N1 C7 C6 106.5(2) . . ?
C6 C7 C8 125.0(2) . . ?
C3 C2 H2A 109.0 . . ?
C3 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C1 C2 C3 112.9(2) . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
C29 C28 H28 126.9 . . ?
C27 C28 C29 106.2(2) . . ?
C27 C28 H28 126.9 . . ?
C15 C16 H16 126.5 . . ?
C17 C16 C15 107.1(2) . . ?
C17 C16 H16 126.5 . . ?
C31 C36 H36A 109.5 . . ?
C31 C36 H36B 109.5 . . ?
H36A C36 H36B 108.1 . . ?
C35 C36 C31 110.7(2) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C18 C17 H17 126.8 . . ?
C16 C17 C18 106.3(2) . . ?
C16 C17 H17 126.8 . . ?
H34A C34 H34B 108.1 . . ?
C35 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 C35 110.7(2) . . ?
C26 C27 H27 126.3 . . ?
C28 C27 C26 107.4(2) . . ?
C28 C27 H27 126.3 . . ?
C36 C35 C34 111.0(2) . . ?
C36 C35 H35A 109.4 . . ?
C36 C35 H35B 109.4 . . ?
C34 C35 H35A 109.4 . . ?
C34 C35 H35B 109.4 . . ?
H35A C35 H35B 108.0 . . ?
C7 C6 H6 125.9 . . ?
C7 C6 C5 108.2(2) . . ?
C5 C6 H6 125.9 . . ?
C9 C10 H10A 109.9 . . ?
C9 C10 H10B 109.9 . . ?
C9 C10 C11 108.9(2) . . ?
H10A C10 H10B 108.3 . . ?
C11 C10 H10A 109.9 . . ?
C11 C10 H10B 109.9 . . ?
C43 C38 C39 117.9(3) . . ?
C43 C38 C37 121.0(3) . . ?
C39 C38 C37 121.1(3) . . ?
C14 C13 H13A 109.4 . . ?
C14 C13 H13B 109.4 . . ?
C14 C13 C12 111.1(2) . . ?
H13A C13 H13B 108.0 . . ?
C12 C13 H13A 109.4 . . ?
C12 C13 H13B 109.4 . . ?
C20 C25 H25A 109.7 . . ?
C20 C25 H25B 109.7 . . ?
C20 C25 C24 110.0(3) . . ?
H25A C25 H25B 108.2 . . ?
C24 C25 H25A 109.7 . . ?
C24 C25 H25B 109.7 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 C5 C6 107.5(2) . . ?
C4 C5 H5 126.2 . . ?
C6 C5 H5 126.2 . . ?
C38 C43 H43 119.2 . . ?
C42 C43 C38 121.5(3) . . ?
C42 C43 H43 119.2 . . ?
C39 C40 H40 120.0 . . ?
C39 C40 C41 119.9(3) . . ?
C41 C40 H40 120.0 . . ?
C38 C39 H39 119.4 . . ?
C40 C39 C38 121.2(3) . . ?
C40 C39 H39 119.4 . . ?
C10 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 C10 111.4(2) . . ?
C12 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 108.0 . . ?
C33 C32 C31 110.9(2) . . ?
C33 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
C13 C12 H12A 109.2 . . ?
C13 C12 H12B 109.2 . . ?
C11 C12 C13 111.8(2) . . ?
C11 C12 H12A 109.2 . . ?
C11 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 C22 110.9(3) . . ?
H21A C21 H21B 108.0 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
C43 C42 H42 120.0 . . ?
C43 C42 C41 120.0(3) . . ?
C41 C42 H42 120.0 . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
H24A C24 H24B 108.1 . . ?
C23 C24 C25 110.8(3) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C40 C41 C42 119.5(3) . . ?
C40 C41 H41 120.3 . . ?
C42 C41 H41 120.3 . . ?
C34 C33 C32 111.0(2) . . ?
C34 C33 H33A 109.4 . . ?
C34 C33 H33B 109.4 . . ?
C32 C33 H33A 109.4 . . ?
C32 C33 H33B 109.4 . . ?
H33A C33 H33B 108.0 . . ?
C24 C23 H23A 109.2 . . ?
C24 C23 H23B 109.2 . . ?
C24 C23 C22 112.0(3) . . ?
H23A C23 H23B 107.9 . . ?
C22 C23 H23A 109.2 . . ?
C22 C23 H23B 109.2 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C23 C22 C21 110.8(3) . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 N2 C9 C14 -78.1(2) 3_666 . . . ?
U1 N2 C9 C10 155.85(18) 3_666 . . . ?
U1 N2 C8 C7 -1.0(4) 3_666 . . . ?
U1 N3 C15 C3 5.3(4) . . . . ?
U1 N3 C15 C16 -176.74(18) . . . . ?
U1 N3 C18 C19 -1.0(3) . . . . ?
U1 N3 C18 C17 177.92(17) . . . . ?
U1 N5 C26 C3 -3.4(4) . . . . ?
U1 N5 C26 C27 177.60(19) . . . . ?
U1 N5 C29 C30 -1.8(3) . . . . ?
U1 N5 C29 C28 -178.76(17) . . . . ?
U1 N6 C30 C29 -0.8(3) . . . . ?
U1 N6 C31 C36 131.23(19) . . . . ?
U1 N6 C31 C32 -103.6(2) . . . . ?
U1 N4 C20 C25 -131.7(2) . . . . ?
U1 N4 C20 C21 100.8(3) . . . . ?
U1 N4 C19 C18 3.1(3) . . . . ?
N2 C9 C14 C13 168.5(2) . . . . ?
N2 C9 C10 C11 -171.7(2) . . . . ?
N2 C8 C7 N1 -4.7(4) . . . . ?
N2 C8 C7 C6 177.0(3) . . . . ?
N3 C15 C3 C26 -7.2(4) . . . . ?
N3 C15 C3 C4 -127.4(2) . . . . ?
N3 C15 C3 C2 115.2(3) . . . . ?
N3 C15 C16 C17 -0.4(3) . . . . ?
N3 C18 C19 N4 -1.6(4) . . . . ?
N3 C18 C17 C16 -0.3(3) . . . . ?
N5 C26 C3 C15 6.3(4) . . . . ?
N5 C26 C3 C4 126.9(2) . . . . ?
N5 C26 C3 C2 -116.1(3) . . . . ?
N5 C26 C27 C28 0.9(3) . . . . ?
N5 C29 C28 C27 0.6(3) . . . . ?
N6 C30 C29 N5 1.9(4) . . . . ?
N6 C30 C29 C28 178.2(3) . . . . ?
N6 C31 C36 C35 -177.8(2) . . . . ?
N6 C31 C32 C33 176.1(2) . . . . ?
N4 C20 C25 C24 177.7(2) . . . . ?
N4 C20 C21 C22 -178.1(3) . . . . ?
N1 C4 C5 C6 1.0(3) . . . . ?
N1 C7 C6 C5 0.6(3) . . . . ?
C15 N3 C18 C19 -178.8(2) . . . . ?
C15 N3 C18 C17 0.1(3) . . . . ?
C15 C3 C4 N1 71.2(3) . . . . ?
C15 C3 C4 C5 -110.4(3) . . . . ?
C15 C3 C2 C1 -64.5(3) . . . . ?
C15 C16 C17 C18 0.4(3) . . . . ?
C18 N3 C15 C3 -177.8(2) . . . . ?
C18 N3 C15 C16 0.2(3) . . . . ?
C9 N2 C8 C7 179.3(2) . . . . ?
C9 C14 C13 C12 55.8(3) . . . . ?
C9 C10 C11 C12 -58.6(3) . . . . ?
C26 N5 C29 C30 176.8(2) . . . . ?
C26 N5 C29 C28 -0.1(3) . . . . ?
C26 C3 C4 N1 -54.8(3) . . . . ?
C26 C3 C4 C5 123.7(3) . . . . ?
C26 C3 C2 C1 62.7(3) . . . . ?
C3 C15 C16 C17 177.7(2) . . . . ?
C3 C26 C27 C28 -178.2(2) . . . . ?
C3 C4 C5 C6 -177.6(3) . . . . ?
C30 N6 C31 C36 -58.6(3) . . . . ?
C30 N6 C31 C32 66.6(3) . . . . ?
C30 C29 C28 C27 -176.0(3) . . . . ?
C29 N5 C26 C3 178.5(2) . . . . ?
C29 N5 C26 C27 -0.4(3) . . . . ?
C29 C28 C27 C26 -0.9(3) . . . . ?
C20 N4 C19 C18 175.0(2) . . . . ?
C20 C25 C24 C23 56.3(4) . . . . ?
C20 C21 C22 C23 -53.8(4) . . . . ?
C14 C9 C10 C11 61.6(3) . . . . ?
C14 C13 C12 C11 -52.3(3) . . . . ?
C8 N2 C9 C14 101.7(2) . . . . ?
C8 N2 C9 C10 -24.4(3) . . . . ?
C8 C7 C6 C5 179.3(2) . . . . ?
C19 N4 C20 C25 58.2(3) . . . . ?
C19 N4 C20 C21 -69.4(3) . . . . ?
C19 C18 C17 C16 178.5(3) . . . . ?
C4 N1 C7 C8 -178.6(2) . . . . ?
C4 N1 C7 C6 0.0(3) . . . . ?
C4 C3 C2 C1 178.7(2) . . . . ?
C31 N6 C30 C29 -173.0(2) . . . . ?
C31 C36 C35 C34 -56.8(3) . . . . ?
C31 C32 C33 C34 56.8(3) . . . . ?
C7 N1 C4 C3 178.2(2) . . . . ?
C7 N1 C4 C5 -0.6(3) . . . . ?
C7 C6 C5 C4 -1.0(3) . . . . ?
C2 C3 C4 N1 -171.6(2) . . . . ?
C2 C3 C4 C5 6.9(4) . . . . ?
C16 C15 C3 C26 175.0(2) . . . . ?
C16 C15 C3 C4 54.8(3) . . . . ?
C16 C15 C3 C2 -62.6(3) . . . . ?
C36 C31 C32 C33 -56.7(3) . . . . ?
C17 C18 C19 N4 179.7(3) . . . . ?
C27 C26 C3 C15 -174.8(2) . . . . ?
C27 C26 C3 C4 -54.2(3) . . . . ?
C27 C26 C3 C2 62.8(3) . . . . ?
C35 C34 C33 C32 -56.3(3) . . . . ?
C10 C9 C14 C13 -60.9(3) . . . . ?
C10 C11 C12 C13 54.2(3) . . . . ?
C38 C43 C42 C41 -0.3(5) . . . . ?
C25 C20 C21 C22 54.1(4) . . . . ?
C25 C24 C23 C22 -58.1(4) . . . . ?
C43 C38 C39 C40 -0.6(5) . . . . ?
C43 C42 C41 C40 -0.1(5) . . . . ?
C39 C38 C43 C42 0.6(5) . . . . ?
C39 C40 C41 C42 0.1(5) . . . . ?
C32 C31 C36 C35 56.7(3) . . . . ?
C21 C20 C25 C24 -55.0(3) . . . . ?
C24 C23 C22 C21 56.6(4) . . . . ?
C41 C40 C39 C38 0.2(5) . . . . ?
C33 C34 C35 C36 56.5(3) . . . . ?
C37 C38 C43 C42 179.9(3) . . . . ?
C37 C38 C39 C40 -179.9(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.547 0.250 457.8 96.3 '2 Toluene'
2 0.000 -0.191 0.750 457.8 96.5 '2 Toluene'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.284
_oxdiff_exptl_absorpt_empirical_full_min 0.805
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Toluene'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-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_to257_2comp_221123_refinalized_twin1_hklf4
_database_code_depnum_ccdc_archive 'CCDC 2313498'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2023-12-11 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_audit_creation_date             2023-11-23
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H56 N6 O3 U'
_chemical_formula_sum            'C40 H56 N6 O3 U'
_chemical_formula_weight         906.93
_chemical_melting_point          ?
_chemical_oxdiff_formula         C36H48N6O2U
_chemical_oxdiff_usercomment     '@ 120 K'
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.5408(7)
_cell_length_b                   11.7266(6)
_cell_length_c                   15.0732(7)
_cell_angle_alpha                81.684(4)
_cell_angle_beta                 84.377(4)
_cell_angle_gamma                75.615(5)
_cell_volume                     1951.09(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11735
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      25.4270
_cell_measurement_theta_min      3.6040
_shelx_estimated_absorpt_T_max   0.787
_shelx_estimated_absorpt_T_min   0.460
_exptl_absorpt_coefficient_mu    4.204
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             908
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 0 1 0.0327
2 0 -1 0.0275
0 -2 1 0.0969
0 2 -1 0.1197
-1 -2 0 0.0856
0 0 -1 0.0763
0 0 1 0.0498
9 13 14 0.0623
-4 -13 -15 0.0806
4 12 17 0.0534
-12 0 -14 0.0736
14 4 12 0.0460

_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.06
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.9982 -0.0048 1.0002 -0.1284 0.0342 0.0390
1.9982 0.0048 -1.0002 0.1284 -0.0342 -0.0390
0.0050 -1.9949 0.9996 0.0443 0.0039 0.1325
-0.0050 1.9949 -0.9996 -0.0443 -0.0039 -0.1325
-0.9949 -1.9982 0.0014 -0.0158 -0.0418 0.1185
-0.0005 -0.0006 -0.9988 0.0028 -0.0419 -0.0224
0.0005 0.0006 0.9988 -0.0028 0.0419 0.0224
8.6151 12.5141 14.3529 0.2091 0.8738 -0.4391
-4.4922 -13.3367 -14.8774 0.0711 -0.8956 0.4392
3.9188 11.7314 16.9905 -0.0755 0.9514 -0.2985
-12.4464 -0.0513 -13.9773 -0.7434 -0.6353 -0.2094
14.1054 4.0518 12.3249 0.7586 0.6486 -0.0621

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0850
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15591
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.768
_diffrn_reflns_theta_min         3.262
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -42.00  14.00   1.00   30.00    --  -15.66 -84.00-146.00   56
  2  ω    -46.00  43.00   1.00   30.00    --  -15.66  84.00 -26.00   89
  3  ω    -43.00  48.00   1.00   30.00    --   17.38 -84.00-146.00   91
  4  ω    -88.00 -39.00   1.00   30.00    --  -15.66-178.00-150.00   49
  5  ω    -39.00  11.00   1.00   30.00    --  -15.66 -77.00 120.00   50
  6  ω    -85.00   3.00   1.00   30.00    --  -15.66 -38.00  30.00   88
  7  ω    -87.00  14.00   1.00   30.00    --  -15.66 -19.00 120.00  101
  8  ω     -9.00  39.00   1.00   30.00    --   17.38  77.00  30.00   48
  9  ω    -39.00  44.00   1.00   30.00    --   17.38 -77.00 120.00   83
 10  ω     -9.00  39.00   1.00   30.00    --   17.38  77.00 -30.00   48
 11  ω    -32.00  52.00   1.00   30.00    --  -15.66  57.00  90.00   84
 12  ω    -83.00   1.00   1.00   30.00    --  -15.66 -57.00 -30.00   84
 13  ω    -39.00  44.00   1.00   30.00    --   17.38 -77.00 -60.00   83
 14  ω     -9.00  39.00   1.00   30.00    --   17.38  77.00-180.00   48
 15  ω    -20.00  56.00   1.00   30.00    --   17.38 -99.00 150.00   76
 16  ω    -20.00   5.00   1.00   30.00    --   17.38 -99.00 -60.00   25
 17  ω    -20.00  56.00   1.00   30.00    --   17.38 -99.00  60.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0629418000
_diffrn_orient_matrix_UB_12      -0.0234360000
_diffrn_orient_matrix_UB_13      -0.0027774000
_diffrn_orient_matrix_UB_21      0.0038472000
_diffrn_orient_matrix_UB_22      0.0190550000
_diffrn_orient_matrix_UB_23      0.0419538000
_diffrn_orient_matrix_UB_31      -0.0081459000
_diffrn_orient_matrix_UB_32      -0.0552141000
_diffrn_orient_matrix_UB_33      0.0224358000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12658
_reflns_number_total             15591
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         2.244
_refine_diff_density_min         -1.212
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         15591
_refine_ls_number_restraints     460
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0393
_refine_ls_restrained_S_all      0.979
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0558P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1002
_refine_special_details          'Refined as a 2-component twin.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.4401(7)
 0.5599(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C31(H31), C20(H20), C9(H9)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C40(H40A,H40B), C32(H32A,H32B), C10(H10A,H10B), C21(H21A,H21B),
 C37(H37A,H37B), C25(H25A,H25B), C11(H11A,H11B), C36(H36A,H36B), C39(H39A,H39B),
  C33(H33A,H33B), C34(H34A,H34B), C14(H14A,H14B), C22(H22A,H22B), C23(H23A,
 H23B), C12(H12A,H12B), C35(H35A,H35B), C24(H24A,H24B), C38(H38A,H38B),
 C13(H13A,H13B)
4.c Aromatic/amide H refined with riding coordinates:
 C30(H30), N1(H1), C19(H19), C8(H8), C27(H27), C17(H17), C16(H16), C28(H28),
 C5(H5), C6(H6)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.70535(2) 0.58758(2) 0.45600(2) 0.01164(9) Uani 1 1 d . . . . .
O3 O 0.7764(4) 0.4154(4) 0.5683(3) 0.0120(10) Uani 1 1 d . . . . .
N4 N 0.8453(5) 0.4354(5) 0.3634(4) 0.0155(12) Uani 1 1 d . . . . .
N3 N 0.7198(5) 0.6633(5) 0.2963(3) 0.0176(13) Uani 1 1 d . . . . .
N6 N 0.5873(5) 0.6478(5) 0.6016(3) 0.0143(12) Uani 1 1 d . . . . .
N5 N 0.5679(5) 0.7821(5) 0.4331(3) 0.0130(12) Uani 1 1 d . . . . .
C30 C 0.5016(6) 0.7427(6) 0.5890(4) 0.0152(14) Uani 1 1 d . . . . .
H30 H 0.447604 0.766670 0.638314 0.018 Uiso 1 1 calc R U . . .
C26 C 0.5339(6) 0.8677(6) 0.3624(4) 0.0142(14) Uani 1 1 d . . . . .
N1 N 0.4461(5) 0.9151(5) 0.1714(4) 0.0173(13) Uani 1 1 d . . . . .
H1 H 0.431999 0.844412 0.187809 0.021 Uiso 1 1 calc R U . . .
C3 C 0.6081(7) 0.8792(6) 0.2759(4) 0.0171(15) Uani 1 1 d . . . . .
C31 C 0.6002(6) 0.5882(6) 0.6955(4) 0.0174(16) Uani 1 1 d . . . . .
H31 H 0.650226 0.505869 0.691925 0.021 Uiso 1 1 calc R U . . .
N2 N 0.2685(6) 0.8730(5) 0.0767(4) 0.0217(14) Uani 1 1 d . . . . .
C15 C 0.6679(6) 0.7609(6) 0.2411(4) 0.0173(15) Uani 1 1 d . . . . .
C19 C 0.8417(6) 0.4678(6) 0.2776(4) 0.0137(14) Uani 1 1 d . . . . .
H19 H 0.884046 0.413185 0.237999 0.016 Uiso 1 1 calc R U . . .
C29 C 0.4863(6) 0.8117(6) 0.5038(4) 0.0177(15) Uani 1 1 d . . . . .
C2 C 0.7085(6) 0.9384(6) 0.2950(4) 0.0179(15) Uani 1 1 d . . . . .
H2A H 0.670455 1.020404 0.307654 0.022 Uiso 1 1 calc R U . . .
H2B H 0.746206 0.894654 0.350171 0.022 Uiso 1 1 calc R U . . .
C40 C 0.7135(6) 0.3207(6) 0.5975(4) 0.0182(15) Uani 1 1 d . . . . .
H40A H 0.721285 0.268502 0.550083 0.022 Uiso 1 1 calc R U . . .
H40B H 0.627286 0.354333 0.612061 0.022 Uiso 1 1 calc R U . . .
C32 C 0.6694(7) 0.6504(7) 0.7455(5) 0.0211(16) Uani 1 1 d . . . . .
H32A H 0.621680 0.731951 0.751652 0.025 Uiso 1 1 calc R U . . .
H32B H 0.745310 0.656246 0.710430 0.025 Uiso 1 1 calc R U . . .
C10 C 0.2498(7) 0.7451(7) -0.0309(5) 0.0291(19) Uani 1 1 d . . . . .
H10A H 0.284010 0.676600 0.013110 0.035 Uiso 1 1 calc R U . . .
H10B H 0.316907 0.767479 -0.069752 0.035 Uiso 1 1 calc R U . . .
C20 C 0.9125(6) 0.3120(6) 0.3915(4) 0.0148(14) Uani 1 1 d . . . . .
H20 H 0.912165 0.301484 0.458551 0.018 Uiso 1 1 calc R U . . .
C7 C 0.3853(7) 0.9994(6) 0.1085(5) 0.0201(16) Uani 1 1 d . . . . .
C8 C 0.2961(7) 0.9709(7) 0.0588(5) 0.0213(16) Uani 1 1 d . . . . .
H8 H 0.258478 1.027393 0.012272 0.026 Uiso 1 1 calc R U . . .
C21 C 1.0426(6) 0.2891(6) 0.3555(5) 0.0206(16) Uani 1 1 d . . . . .
H21A H 1.081312 0.346475 0.375689 0.025 Uiso 1 1 calc R U . . .
H21B H 1.046527 0.300785 0.288975 0.025 Uiso 1 1 calc R U . . .
C4 C 0.5316(6) 0.9561(6) 0.2051(4) 0.0176(15) Uani 1 1 d . . . . .
C27 C 0.4275(6) 0.9478(6) 0.3882(5) 0.0201(16) Uani 1 1 d . . . . .
H27 H 0.383323 1.013462 0.351011 0.024 Uiso 1 1 calc R U . . .
C37 C 0.8846(6) 0.3945(6) 0.6166(5) 0.0219(16) Uani 1 1 d . . . . .
H37A H 0.873910 0.449737 0.662204 0.026 Uiso 1 1 calc R U . . .
H37B H 0.954094 0.404302 0.574764 0.026 Uiso 1 1 calc R U . . .
C25 C 0.8512(7) 0.2202(6) 0.3657(5) 0.0208(16) Uani 1 1 d . . . . .
H25A H 0.768200 0.233366 0.393241 0.025 Uiso 1 1 calc R U . . .
H25B H 0.847335 0.229489 0.299641 0.025 Uiso 1 1 calc R U . . .
C17 C 0.7602(6) 0.6258(6) 0.1515(4) 0.0170(16) Uani 1 1 d . . . . .
H17 H 0.790194 0.585947 0.100393 0.020 Uiso 1 1 calc R U . . .
C11 C 0.1668(8) 0.7085(8) -0.0886(5) 0.034(2) Uani 1 1 d . . . . .
H11A H 0.139201 0.773890 -0.136761 0.041 Uiso 1 1 calc R U . . .
H11B H 0.211637 0.638263 -0.117331 0.041 Uiso 1 1 calc R U . . .
C9 C 0.1844(7) 0.8487(7) 0.0191(5) 0.0224(17) Uani 1 1 d . . . . .
H9 H 0.156953 0.920221 -0.025389 0.027 Uiso 1 1 calc R U . . .
C36 C 0.4838(7) 0.5767(7) 0.7500(5) 0.0283(19) Uani 1 1 d . . . . .
H36A H 0.438970 0.535556 0.717718 0.034 Uiso 1 1 calc R U . . .
H36B H 0.432905 0.656599 0.757728 0.034 Uiso 1 1 calc R U . . .
C16 C 0.6903(7) 0.7403(6) 0.1515(4) 0.0208(17) Uani 1 1 d . . . . .
H16 H 0.662986 0.794467 0.100411 0.025 Uiso 1 1 calc R U . . .
C39 C 0.7745(7) 0.2522(6) 0.6809(5) 0.0275(18) Uani 1 1 d . . . . .
H39A H 0.737110 0.287010 0.735921 0.033 Uiso 1 1 calc R U . . .
H39B H 0.771889 0.167572 0.687817 0.033 Uiso 1 1 calc R U . . .
C33 C 0.6971(7) 0.5833(8) 0.8388(5) 0.032(2) Uani 1 1 d . . . . .
H33A H 0.751875 0.504761 0.832436 0.038 Uiso 1 1 calc R U . . .
H33B H 0.738169 0.628063 0.871074 0.038 Uiso 1 1 calc R U . . .
C18 C 0.7777(6) 0.5808(6) 0.2404(4) 0.0144(15) Uani 1 1 d . . . . .
C28 C 0.3994(6) 0.9135(6) 0.4772(5) 0.0196(16) Uani 1 1 d . . . . .
H28 H 0.333391 0.951851 0.513555 0.024 Uiso 1 1 calc R U . . .
C34 C 0.5831(7) 0.5664(7) 0.8930(5) 0.0246(18) Uani 1 1 d . . . . .
H34A H 0.603984 0.517665 0.951136 0.030 Uiso 1 1 calc R U . . .
H34B H 0.532735 0.644599 0.905752 0.030 Uiso 1 1 calc R U . . .
C5 C 0.5230(7) 1.0698(6) 0.1643(5) 0.0225(17) Uani 1 1 d . . . . .
H5 H 0.570038 1.121527 0.175370 0.027 Uiso 1 1 calc R U . . .
C14 C 0.0784(8) 0.8199(8) 0.0741(5) 0.034(2) Uani 1 1 d . . . . .
H14A H 0.034598 0.889831 0.103547 0.041 Uiso 1 1 calc R U . . .
H14B H 0.106146 0.753851 0.121751 0.041 Uiso 1 1 calc R U . . .
C22 C 1.1098(7) 0.1625(6) 0.3886(5) 0.0297(18) Uani 1 1 d . . . . .
H22A H 1.193515 0.148303 0.362469 0.036 Uiso 1 1 calc R U . . .
H22B H 1.111898 0.153292 0.454762 0.036 Uiso 1 1 calc R U . . .
C1 C 0.8074(7) 0.9438(7) 0.2204(5) 0.0287(19) Uani 1 1 d . . . . .
H1A H 0.771450 0.982912 0.164259 0.043 Uiso 1 1 calc R U . . .
H1B H 0.852895 0.863161 0.212182 0.043 Uiso 1 1 calc R U . . .
H1C H 0.861327 0.988937 0.236899 0.043 Uiso 1 1 calc R U . . .
C6 C 0.4319(8) 1.0971(7) 0.1028(5) 0.0265(18) Uani 1 1 d . . . . .
H6 H 0.407667 1.169540 0.064722 0.032 Uiso 1 1 calc R U . . .
C23 C 1.0514(8) 0.0730(6) 0.3629(5) 0.034(2) Uani 1 1 d . . . . .
H23A H 1.094666 -0.007543 0.387571 0.040 Uiso 1 1 calc R U . . .
H23B H 1.056112 0.076994 0.296614 0.040 Uiso 1 1 calc R U . . .
C12 C 0.0597(9) 0.6793(8) -0.0327(6) 0.039(2) Uani 1 1 d . . . . .
H12A H 0.086469 0.608603 0.011496 0.047 Uiso 1 1 calc R U . . .
H12B H 0.004897 0.660477 -0.072098 0.047 Uiso 1 1 calc R U . . .
C35 C 0.5131(8) 0.5061(7) 0.8425(5) 0.0294(19) Uani 1 1 d . . . . .
H35A H 0.437716 0.499294 0.877960 0.035 Uiso 1 1 calc R U . . .
H35B H 0.560682 0.425059 0.834615 0.035 Uiso 1 1 calc R U . . .
C24 C 0.9213(7) 0.0952(6) 0.3983(5) 0.0277(18) Uani 1 1 d . . . . .
H24A H 0.917318 0.083735 0.464767 0.033 Uiso 1 1 calc R U . . .
H24B H 0.883939 0.036743 0.378280 0.033 Uiso 1 1 calc R U . . .
C38 C 0.9020(7) 0.2668(6) 0.6610(5) 0.0257(18) Uani 1 1 d . . . . .
H38A H 0.947909 0.210540 0.619867 0.031 Uiso 1 1 calc R U . . .
H38B H 0.944343 0.254405 0.716899 0.031 Uiso 1 1 calc R U . . .
C13 C -0.0072(8) 0.7846(9) 0.0167(6) 0.046(2) Uani 1 1 d . . . . .
H13A H -0.074402 0.762870 0.055782 0.055 Uiso 1 1 calc R U . . .
H13B H -0.040851 0.852980 -0.027588 0.055 Uiso 1 1 calc R U . . .
O2 O 0.8268(4) 0.6427(4) 0.4809(3) 0.0188(11) Uani 1 1 d . . . . .
O1 O 0.5915(4) 0.5213(4) 0.4338(3) 0.0169(10) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O3 2.464(4) . ?
U1 N4 2.567(5) . ?
U1 N3 2.446(5) . ?
U1 N6 2.560(5) . ?
U1 N5 2.433(5) . ?
U1 O2 1.774(5) . ?
U1 O1 1.764(5) . ?
O3 C40 1.467(7) . ?
O3 C37 1.458(8) . ?
N4 C19 1.296(8) . ?
N4 C20 1.484(8) . ?
N3 C15 1.358(8) . ?
N3 C18 1.378(8) . ?
N6 C30 1.297(8) . ?
N6 C31 1.490(8) . ?
N5 C26 1.369(8) . ?
N5 C29 1.375(8) . ?
C30 H30 0.9500 . ?
C30 C29 1.417(9) . ?
C26 C3 1.496(9) . ?
C26 C27 1.407(9) . ?
N1 H1 0.8800 . ?
N1 C7 1.372(9) . ?
N1 C4 1.366(9) . ?
C3 C15 1.530(10) . ?
C3 C2 1.559(10) . ?
C3 C4 1.498(9) . ?
C31 H31 1.0000 . ?
C31 C32 1.518(10) . ?
C31 C36 1.530(10) . ?
N2 C8 1.252(9) . ?
N2 C9 1.467(9) . ?
C15 C16 1.394(9) . ?
C19 H19 0.9500 . ?
C19 C18 1.413(9) . ?
C29 C28 1.392(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.529(10) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C39 1.524(10) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.531(10) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.527(11) . ?
C10 C9 1.520(11) . ?
C20 H20 1.0000 . ?
C20 C21 1.517(9) . ?
C20 C25 1.538(9) . ?
C7 C8 1.458(10) . ?
C7 C6 1.370(10) . ?
C8 H8 0.9500 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.531(9) . ?
C4 C5 1.369(9) . ?
C27 H27 0.9500 . ?
C27 C28 1.375(10) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.522(9) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C24 1.524(10) . ?
C17 H17 0.9500 . ?
C17 C16 1.384(10) . ?
C17 C18 1.382(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.510(11) . ?
C9 H9 1.0000 . ?
C9 C14 1.491(10) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C35 1.537(10) . ?
C16 H16 0.9500 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C38 1.520(11) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.520(10) . ?
C28 H28 0.9500 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.513(11) . ?
C5 H5 0.9500 . ?
C5 C6 1.415(11) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C13 1.539(12) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.492(11) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C6 H6 0.9500 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.515(11) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.535(12) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 U1 N4 76.10(15) . . ?
O3 U1 N6 76.43(15) . . ?
N3 U1 O3 143.98(16) . . ?
N3 U1 N4 67.88(18) . . ?
N3 U1 N6 139.47(18) . . ?
N6 U1 N4 152.16(17) . . ?
N5 U1 O3 144.17(15) . . ?
N5 U1 N4 139.41(17) . . ?
N5 U1 N3 71.74(18) . . ?
N5 U1 N6 67.76(17) . . ?
O2 U1 O3 87.12(17) . . ?
O2 U1 N4 91.68(19) . . ?
O2 U1 N3 93.5(2) . . ?
O2 U1 N6 91.36(19) . . ?
O2 U1 N5 94.71(19) . . ?
O1 U1 O3 88.81(17) . . ?
O1 U1 N4 85.30(19) . . ?
O1 U1 N3 88.6(2) . . ?
O1 U1 N6 89.72(19) . . ?
O1 U1 N5 89.82(19) . . ?
O1 U1 O2 175.4(2) . . ?
C40 O3 U1 124.5(4) . . ?
C37 O3 U1 125.2(4) . . ?
C37 O3 C40 110.4(5) . . ?
C19 N4 U1 112.8(4) . . ?
C19 N4 C20 116.1(5) . . ?
C20 N4 U1 130.3(4) . . ?
C15 N3 U1 137.7(4) . . ?
C15 N3 C18 105.5(5) . . ?
C18 N3 U1 115.4(4) . . ?
C30 N6 U1 113.3(4) . . ?
C30 N6 C31 116.9(5) . . ?
C31 N6 U1 129.8(4) . . ?
C26 N5 U1 137.1(4) . . ?
C26 N5 C29 106.3(5) . . ?
C29 N5 U1 115.6(4) . . ?
N6 C30 H30 119.1 . . ?
N6 C30 C29 121.8(6) . . ?
C29 C30 H30 119.1 . . ?
N5 C26 C3 123.8(6) . . ?
N5 C26 C27 109.4(6) . . ?
C27 C26 C3 126.5(6) . . ?
C7 N1 H1 124.7 . . ?
C4 N1 H1 124.7 . . ?
C4 N1 C7 110.6(6) . . ?
C26 C3 C15 114.1(5) . . ?
C26 C3 C2 106.2(5) . . ?
C26 C3 C4 109.6(6) . . ?
C15 C3 C2 108.2(6) . . ?
C4 C3 C15 108.3(5) . . ?
C4 C3 C2 110.4(5) . . ?
N6 C31 H31 107.0 . . ?
N6 C31 C32 109.6(5) . . ?
N6 C31 C36 116.1(6) . . ?
C32 C31 H31 107.0 . . ?
C32 C31 C36 109.7(6) . . ?
C36 C31 H31 107.0 . . ?
C8 N2 C9 117.1(6) . . ?
N3 C15 C3 122.2(6) . . ?
N3 C15 C16 110.6(6) . . ?
C16 C15 C3 126.7(6) . . ?
N4 C19 H19 118.6 . . ?
N4 C19 C18 122.8(6) . . ?
C18 C19 H19 118.6 . . ?
N5 C29 C30 119.7(6) . . ?
N5 C29 C28 110.3(6) . . ?
C28 C29 C30 130.0(6) . . ?
C3 C2 H2A 108.2 . . ?
C3 C2 H2B 108.2 . . ?
H2A C2 H2B 107.4 . . ?
C1 C2 C3 116.2(6) . . ?
C1 C2 H2A 108.2 . . ?
C1 C2 H2B 108.2 . . ?
O3 C40 H40A 110.8 . . ?
O3 C40 H40B 110.8 . . ?
O3 C40 C39 104.9(6) . . ?
H40A C40 H40B 108.8 . . ?
C39 C40 H40A 110.8 . . ?
C39 C40 H40B 110.8 . . ?
C31 C32 H32A 109.4 . . ?
C31 C32 H32B 109.4 . . ?
C31 C32 C33 111.2(6) . . ?
H32A C32 H32B 108.0 . . ?
C33 C32 H32A 109.4 . . ?
C33 C32 H32B 109.4 . . ?
H10A C10 H10B 107.9 . . ?
C11 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
C9 C10 H10A 109.2 . . ?
C9 C10 H10B 109.2 . . ?
C9 C10 C11 112.0(7) . . ?
N4 C20 H20 107.2 . . ?
N4 C20 C21 112.2(5) . . ?
N4 C20 C25 111.8(5) . . ?
C21 C20 H20 107.2 . . ?
C21 C20 C25 111.0(6) . . ?
C25 C20 H20 107.2 . . ?
N1 C7 C8 119.8(6) . . ?
C6 C7 N1 107.2(7) . . ?
C6 C7 C8 132.9(7) . . ?
N2 C8 C7 120.9(7) . . ?
N2 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 C22 110.6(6) . . ?
H21A C21 H21B 108.1 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
N1 C4 C3 119.9(6) . . ?
N1 C4 C5 106.7(6) . . ?
C5 C4 C3 133.4(7) . . ?
C26 C27 H27 126.4 . . ?
C28 C27 C26 107.3(6) . . ?
C28 C27 H27 126.4 . . ?
O3 C37 H37A 110.9 . . ?
O3 C37 H37B 110.9 . . ?
O3 C37 C38 104.2(6) . . ?
H37A C37 H37B 108.9 . . ?
C38 C37 H37A 110.9 . . ?
C38 C37 H37B 110.9 . . ?
C20 C25 H25A 109.7 . . ?
C20 C25 H25B 109.7 . . ?
H25A C25 H25B 108.2 . . ?
C24 C25 C20 109.8(6) . . ?
C24 C25 H25A 109.7 . . ?
C24 C25 H25B 109.7 . . ?
C16 C17 H17 126.7 . . ?
C18 C17 H17 126.7 . . ?
C18 C17 C16 106.5(6) . . ?
C10 C11 H11A 109.4 . . ?
C10 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 C10 111.1(7) . . ?
C12 C11 H11A 109.4 . . ?
C12 C11 H11B 109.4 . . ?
N2 C9 C10 108.3(6) . . ?
N2 C9 H9 109.2 . . ?
N2 C9 C14 110.5(6) . . ?
C10 C9 H9 109.2 . . ?
C14 C9 C10 110.4(7) . . ?
C14 C9 H9 109.2 . . ?
C31 C36 H36A 109.8 . . ?
C31 C36 H36B 109.8 . . ?
C31 C36 C35 109.5(7) . . ?
H36A C36 H36B 108.2 . . ?
C35 C36 H36A 109.8 . . ?
C35 C36 H36B 109.8 . . ?
C15 C16 H16 126.7 . . ?
C17 C16 C15 106.7(6) . . ?
C17 C16 H16 126.7 . . ?
C40 C39 H39A 111.4 . . ?
C40 C39 H39B 111.4 . . ?
H39A C39 H39B 109.2 . . ?
C38 C39 C40 102.0(5) . . ?
C38 C39 H39A 111.4 . . ?
C38 C39 H39B 111.4 . . ?
C32 C33 H33A 109.4 . . ?
C32 C33 H33B 109.4 . . ?
H33A C33 H33B 108.0 . . ?
C34 C33 C32 111.1(6) . . ?
C34 C33 H33A 109.4 . . ?
C34 C33 H33B 109.4 . . ?
N3 C18 C19 119.6(6) . . ?
N3 C18 C17 110.7(6) . . ?
C17 C18 C19 129.6(6) . . ?
C29 C28 H28 126.6 . . ?
C27 C28 C29 106.8(6) . . ?
C27 C28 H28 126.6 . . ?
C33 C34 H34A 109.4 . . ?
C33 C34 H34B 109.4 . . ?
H34A C34 H34B 108.0 . . ?
C35 C34 C33 111.0(6) . . ?
C35 C34 H34A 109.4 . . ?
C35 C34 H34B 109.4 . . ?
C4 C5 H5 125.8 . . ?
C4 C5 C6 108.4(7) . . ?
C6 C5 H5 125.8 . . ?
C9 C14 H14A 109.2 . . ?
C9 C14 H14B 109.2 . . ?
C9 C14 C13 111.9(7) . . ?
H14A C14 H14B 107.9 . . ?
C13 C14 H14A 109.2 . . ?
C13 C14 H14B 109.2 . . ?
C21 C22 H22A 109.3 . . ?
C21 C22 H22B 109.3 . . ?
H22A C22 H22B 108.0 . . ?
C23 C22 C21 111.4(7) . . ?
C23 C22 H22A 109.3 . . ?
C23 C22 H22B 109.3 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C7 C6 C5 107.2(6) . . ?
C7 C6 H6 126.4 . . ?
C5 C6 H6 126.4 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 C24 110.9(6) . . ?
H23A C23 H23B 108.1 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C11 C12 H12A 109.6 . . ?
C11 C12 H12B 109.6 . . ?
C11 C12 C13 110.3(7) . . ?
H12A C12 H12B 108.1 . . ?
C13 C12 H12A 109.6 . . ?
C13 C12 H12B 109.6 . . ?
C36 C35 H35A 109.5 . . ?
C36 C35 H35B 109.5 . . ?
C34 C35 C36 110.9(6) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 108.1 . . ?
C25 C24 H24A 109.2 . . ?
C25 C24 H24B 109.2 . . ?
C23 C24 C25 111.9(6) . . ?
C23 C24 H24A 109.2 . . ?
C23 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
C37 C38 H38A 111.1 . . ?
C37 C38 H38B 111.1 . . ?
C39 C38 C37 103.2(6) . . ?
C39 C38 H38A 111.1 . . ?
C39 C38 H38B 111.1 . . ?
H38A C38 H38B 109.1 . . ?
C14 C13 H13A 109.6 . . ?
C14 C13 H13B 109.6 . . ?
C12 C13 C14 110.4(8) . . ?
C12 C13 H13A 109.6 . . ?
C12 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 O3 C40 C39 -167.2(4) . . . . ?
U1 O3 C37 C38 -168.1(4) . . . . ?
U1 N4 C19 C18 6.7(8) . . . . ?
U1 N4 C20 C21 -132.0(5) . . . . ?
U1 N4 C20 C25 102.6(6) . . . . ?
U1 N3 C15 C3 23.1(11) . . . . ?
U1 N3 C15 C16 -164.1(5) . . . . ?
U1 N3 C18 C19 -11.2(8) . . . . ?
U1 N3 C18 C17 168.0(4) . . . . ?
U1 N6 C30 C29 -6.9(8) . . . . ?
U1 N6 C31 C32 100.6(6) . . . . ?
U1 N6 C31 C36 -134.4(5) . . . . ?
U1 N5 C26 C3 -21.7(10) . . . . ?
U1 N5 C26 C27 164.8(5) . . . . ?
U1 N5 C29 C30 13.0(8) . . . . ?
U1 N5 C29 C28 -168.9(5) . . . . ?
O3 C40 C39 C38 -31.1(7) . . . . ?
O3 C37 C38 C39 -32.6(7) . . . . ?
N4 C19 C18 N3 2.7(10) . . . . ?
N4 C19 C18 C17 -176.2(7) . . . . ?
N4 C20 C21 C22 178.0(6) . . . . ?
N4 C20 C25 C24 -178.4(6) . . . . ?
N3 C15 C16 C17 -0.7(9) . . . . ?
N6 C30 C29 N5 -3.8(11) . . . . ?
N6 C30 C29 C28 178.5(7) . . . . ?
N6 C31 C32 C33 -173.4(6) . . . . ?
N6 C31 C36 C35 176.1(6) . . . . ?
N5 C26 C3 C15 41.7(9) . . . . ?
N5 C26 C3 C2 -77.4(8) . . . . ?
N5 C26 C3 C4 163.4(6) . . . . ?
N5 C26 C27 C28 2.7(8) . . . . ?
N5 C29 C28 C27 0.0(8) . . . . ?
C30 N6 C31 C32 -81.9(7) . . . . ?
C30 N6 C31 C36 43.1(9) . . . . ?
C30 C29 C28 C27 177.9(7) . . . . ?
C26 N5 C29 C30 -176.5(6) . . . . ?
C26 N5 C29 C28 1.6(8) . . . . ?
C26 C3 C15 N3 -42.0(10) . . . . ?
C26 C3 C15 C16 146.3(7) . . . . ?
C26 C3 C2 C1 171.5(6) . . . . ?
C26 C3 C4 N1 -70.3(8) . . . . ?
C26 C3 C4 C5 106.7(9) . . . . ?
C26 C27 C28 C29 -1.6(8) . . . . ?
N1 C7 C8 N2 4.6(11) . . . . ?
N1 C7 C6 C5 -0.1(9) . . . . ?
N1 C4 C5 C6 -1.5(8) . . . . ?
C3 C26 C27 C28 -170.6(7) . . . . ?
C3 C15 C16 C17 171.7(7) . . . . ?
C3 C4 C5 C6 -178.7(8) . . . . ?
C31 N6 C30 C29 175.2(6) . . . . ?
C31 C32 C33 C34 -55.9(9) . . . . ?
C31 C36 C35 C34 58.7(9) . . . . ?
N2 C9 C14 C13 -175.7(7) . . . . ?
C15 N3 C18 C19 179.8(6) . . . . ?
C15 N3 C18 C17 -1.0(8) . . . . ?
C15 C3 C2 C1 48.6(8) . . . . ?
C15 C3 C4 N1 54.7(8) . . . . ?
C15 C3 C4 C5 -128.3(8) . . . . ?
C19 N4 C20 C21 59.0(8) . . . . ?
C19 N4 C20 C25 -66.4(7) . . . . ?
C29 N5 C26 C3 170.9(6) . . . . ?
C29 N5 C26 C27 -2.6(8) . . . . ?
C2 C3 C15 N3 75.9(8) . . . . ?
C2 C3 C15 C16 -95.7(8) . . . . ?
C2 C3 C4 N1 173.1(6) . . . . ?
C2 C3 C4 C5 -9.9(11) . . . . ?
C40 O3 C37 C38 13.3(7) . . . . ?
C40 C39 C38 C37 39.1(7) . . . . ?
C32 C31 C36 C35 -59.0(8) . . . . ?
C32 C33 C34 C35 54.9(9) . . . . ?
C10 C11 C12 C13 55.9(10) . . . . ?
C10 C9 C14 C13 -56.0(10) . . . . ?
C20 N4 C19 C18 177.6(6) . . . . ?
C20 C21 C22 C23 56.8(8) . . . . ?
C20 C25 C24 C23 -55.6(8) . . . . ?
C7 N1 C4 C3 179.2(6) . . . . ?
C7 N1 C4 C5 1.4(8) . . . . ?
C8 N2 C9 C10 115.1(8) . . . . ?
C8 N2 C9 C14 -123.9(8) . . . . ?
C8 C7 C6 C5 -175.5(8) . . . . ?
C21 C20 C25 C24 55.6(7) . . . . ?
C21 C22 C23 C24 -56.5(8) . . . . ?
C4 N1 C7 C8 175.2(6) . . . . ?
C4 N1 C7 C6 -0.8(8) . . . . ?
C4 C3 C15 N3 -164.4(6) . . . . ?
C4 C3 C15 C16 24.0(10) . . . . ?
C4 C3 C2 C1 -69.8(8) . . . . ?
C4 C5 C6 C7 1.0(9) . . . . ?
C27 C26 C3 C15 -145.9(7) . . . . ?
C27 C26 C3 C2 95.0(8) . . . . ?
C27 C26 C3 C4 -24.2(9) . . . . ?
C37 O3 C40 C39 11.3(7) . . . . ?
C25 C20 C21 C22 -56.1(8) . . . . ?
C11 C10 C9 N2 176.6(6) . . . . ?
C11 C10 C9 C14 55.6(9) . . . . ?
C11 C12 C13 C14 -56.0(10) . . . . ?
C9 N2 C8 C7 -175.8(6) . . . . ?
C9 C10 C11 C12 -56.1(9) . . . . ?
C9 C14 C13 C12 56.8(10) . . . . ?
C36 C31 C32 C33 58.0(8) . . . . ?
C16 C17 C18 N3 0.6(8) . . . . ?
C16 C17 C18 C19 179.6(7) . . . . ?
C33 C34 C35 C36 -56.7(9) . . . . ?
C18 N3 C15 C3 -171.8(6) . . . . ?
C18 N3 C15 C16 1.1(8) . . . . ?
C18 C17 C16 C15 0.0(8) . . . . ?
C22 C23 C24 C25 56.7(8) . . . . ?
C6 C7 C8 N2 179.5(8) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.425
_oxdiff_exptl_absorpt_empirical_full_min 0.743
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.4401(7) 35454 10261 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.5599(7) 35082 10261 nmt 0.9863 -0.0006 0.0722 -0.0014 1.0061 -0.0397
-0.1477 0.1010 0.9913

_twin_special_details            
;
Component 2 rotated by 6.9604° 
around [0.56 0.82 0.11] (reciprocal) or [0.47 0.88 -0.05] (direct)
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Tetrahydrofuran'
_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_to500_twin1_hklf4_refinalised
_database_code_depnum_ccdc_archive 'CCDC 2313499'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2023-12-11 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_audit_creation_date             2023-11-23
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C41 H53 N7 O2 U'
_chemical_formula_sum            'C41 H53 N7 O2 U'
_chemical_formula_weight         913.93
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C41 H91 N7 U O2 '
_chemical_oxdiff_usercomment     pyr/hexane
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3701(3)
_cell_length_b                   11.9785(5)
_cell_length_c                   14.9463(4)
_cell_angle_alpha                83.518(3)
_cell_angle_beta                 85.015(2)
_cell_angle_gamma                75.569(3)
_cell_volume                     1955.15(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    14471
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      27.2660
_cell_measurement_theta_min      3.5150
_shelx_estimated_absorpt_T_max   0.758
_shelx_estimated_absorpt_T_min   0.356
_exptl_absorpt_coefficient_mu    4.195
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.631
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             912
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 15 -7 0.0426
-1 16 1 0.0460
-7 7 15 0.0588
2 -16 -3 0.0531
1 1 21 0.0259
-16 -4 -3 0.1349
0 -1 -21 0.0492
-11 -2 14 0.0855
12 3 15 0.0997
0 -16 2 0.0246
2 15 11 0.0280

_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2.3096 15.3109 -6.5899 -0.9263 0.0234 0.3762
-1.4388 15.9051 1.2498 -0.9964 0.0257 -0.0803
-7.4233 6.9179 14.8811 -0.4940 0.0135 -0.8693
2.1025 -15.6444 -2.6788 0.9862 -0.0255 0.1634
1.0895 0.9680 21.0388 0.0437 -0.5601 -0.8273
-15.9898 -3.5637 -2.9881 -0.0708 0.8883 -0.4537
0.2272 -0.6796 -20.9385 -0.0381 0.4904 0.8707
-10.9729 -2.0449 13.9891 -0.0090 0.2252 -0.9723
12.0050 2.9012 14.9675 0.0902 -0.9718 -0.1838
-0.0148 -15.9877 1.8841 0.9888 -0.0267 -0.1010
2.0257 14.9224 11.0825 -0.8366 -0.3847 -0.3633

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            36204
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.404
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -33.00  54.00   1.00   30.00    --  -14.44  40.00  -3.00   87
  2  ω    -83.00   4.00   1.00   30.00    --  -14.44 -40.00-156.00   87
  3  ω    -53.00  34.00   1.00   30.00    --   16.16 -40.00-156.00   87
  4  ω    -11.00  39.00   1.00   30.00    --   16.16  77.00-120.00   50
  5  ω     -1.00  83.00   1.00   30.00    --   16.16  57.00  30.00   84
  6  ω    -53.00  35.00   1.00   30.00    --   16.16 -38.00  90.00   88
  7  ω    -20.00  54.00   1.00   30.00    --   16.16 -99.00-180.00   74
  8  ω    -11.00  39.00   1.00   30.00    --   16.16  77.00 120.00   50
  9  ω    -39.00  12.00   1.00   30.00    --  -14.44 -77.00 -90.00   51
 10  ω    -41.00   2.00   1.00   30.00    --  -14.44  77.00  30.00   43
 11  ω    -39.00  43.00   1.00   30.00    --   16.16 -77.00 -90.00   82
 12  ω    -20.00  54.00   1.00   30.00    --   16.16 -99.00  30.00   74
 13  ω    -11.00  39.00   1.00   30.00    --   16.16  77.00-180.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0173602000
_diffrn_orient_matrix_UB_12      -0.0613927000
_diffrn_orient_matrix_UB_13      0.0040008000
_diffrn_orient_matrix_UB_21      -0.0508367000
_diffrn_orient_matrix_UB_22      -0.0011044000
_diffrn_orient_matrix_UB_23      -0.0239377000
_diffrn_orient_matrix_UB_31      0.0357648000
_diffrn_orient_matrix_UB_32      0.0014246000
_diffrn_orient_matrix_UB_33      -0.0412397000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6812
_reflns_number_total             7952
_reflns_odcompleteness_completeness 99.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         2.970
_refine_diff_density_min         -1.419
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         7952
_refine_ls_number_restraints     516
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0375
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0469P)²+1.8730P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0900
_refine_special_details          Twin
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H23C)=Sof(H23D)=Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C20A)=Sof(H20A)=
 Sof(C22A)=Sof(H22C)=Sof(H22D)=Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(C24A)=
 Sof(H24C)=Sof(H24D)=1-FVAR(1)
 Sof(C20)=Sof(H20)=Sof(H23A)=Sof(H23B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C21)=
 Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C24)=Sof(H24A)=Sof(H24B)=
 FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C31(H31), C9(H9), C20(H20), C20A(H20A)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C14(H14A,H14B), C32(H32A,H32B), C13(H13A,H13B), C33(H33A,H33B),
 C10(H10A,H10B), C12(H12A,H12B), C11(H11A,H11B), C23(H23A,H23B), C23(H23C,H23D),
  C34(H34A,H34B), C35(H35A,H35B), C25(H25A,H25B), C36(H36A,H36B), C21(H21A,
 H21B), C22(H22A,H22B), C24(H24A,H24B), C21A(H21C,H21D), C22A(H22C,H22D),
 C25A(H25C,H25D), C24A(H24C,H24D)
4.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C41(H41), C19(H19), C28(H28), C30(H30), C27(H27), C40(H40), C8(H8),
 C38(H38), C37(H37), C17(H17), C16(H16), C39(H39), C5(H5), C6(H6)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.29123(2) 0.40745(2) 0.54589(2) 0.02043(7) Uani 1 1 d . . . . .
O1 O 0.4051(3) 0.4742(3) 0.5709(2) 0.0229(7) Uani 1 1 d . . . . .
O2 O 0.1705(3) 0.3515(3) 0.5161(3) 0.0342(9) Uani 1 1 d . . . . .
N5 N 0.2720(3) 0.3318(4) 0.7041(3) 0.0232(9) Uani 1 1 d . . . . .
N3 N 0.4317(4) 0.2173(4) 0.5664(3) 0.0251(9) Uani 1 1 d . . . . .
N6 N 0.1427(3) 0.5554(4) 0.6414(3) 0.0245(9) Uani 1 1 d . . . . .
N7 N 0.2149(3) 0.5806(4) 0.4332(3) 0.0246(9) Uani 1 1 d . . . . .
N4 N 0.4208(5) 0.3504(4) 0.4005(3) 0.0390(12) Uani 1 1 d . . . . .
N1 N 0.5503(4) 0.0847(4) 0.8272(3) 0.0289(10) Uani 1 1 d . . . . .
H1 H 0.564170 0.153827 0.813409 0.035 Uiso 1 1 calc R U . . .
C26 C 0.3260(4) 0.2362(4) 0.7575(3) 0.0226(10) Uani 1 1 d . . . . .
C15 C 0.4649(4) 0.1329(5) 0.6338(3) 0.0244(10) Uani 1 1 d . . . . .
N2 N 0.7335(4) 0.1226(4) 0.9266(3) 0.0323(10) Uani 1 1 d . . . . .
C29 C 0.2136(4) 0.4126(5) 0.7614(3) 0.0253(11) Uani 1 1 d . . . . .
C41 C 0.2801(4) 0.6619(4) 0.4110(3) 0.0236(10) Uani 1 1 d . . . . .
H41 H 0.353884 0.653451 0.439237 0.028 Uiso 1 1 calc R U . . .
C19 C 0.5068(6) 0.2580(5) 0.4132(4) 0.0369(13) Uani 1 1 d . . . . .
H19 H 0.564568 0.235521 0.364720 0.044 Uiso 1 1 calc R U . . .
C3 C 0.3857(4) 0.1225(4) 0.7202(3) 0.0243(10) Uani 1 1 d . . . . .
C2 C 0.2839(5) 0.0643(5) 0.6972(3) 0.0263(11) Uani 1 1 d . . . . .
H2A H 0.243985 0.108920 0.643539 0.032 Uiso 1 1 calc R U . . .
H2B H 0.323239 -0.014679 0.680607 0.032 Uiso 1 1 calc R U . . .
C4 C 0.4644(5) 0.0456(5) 0.7896(3) 0.0290(11) Uani 1 1 d . . . . .
C31 C 0.0699(5) 0.6751(5) 0.6159(4) 0.0311(12) Uani 1 1 d . . . . .
H31 H 0.050673 0.678080 0.551507 0.037 Uiso 1 1 calc R U . . .
C18 C 0.5181(5) 0.1896(5) 0.4960(3) 0.0301(11) Uani 1 1 d . . . . .
C28 C 0.2305(5) 0.3684(5) 0.8502(3) 0.0326(12) Uani 1 1 d . . . . .
H28 H 0.199264 0.406991 0.902502 0.039 Uiso 1 1 calc R U . . .
C30 C 0.1473(4) 0.5226(5) 0.7262(4) 0.0279(11) Uani 1 1 d . . . . .
H30 H 0.103767 0.575209 0.767540 0.034 Uiso 1 1 calc R U . . .
C27 C 0.3024(5) 0.2562(5) 0.8476(3) 0.0295(12) Uani 1 1 d . . . . .
H27 H 0.330113 0.203354 0.898054 0.035 Uiso 1 1 calc R U . . .
C14 C 0.7498(5) 0.2493(6) 1.0375(4) 0.0436(15) Uani 1 1 d . . . . .
H14A H 0.679172 0.230520 1.074147 0.052 Uiso 1 1 calc R U . . .
H14B H 0.718665 0.315920 0.993267 0.052 Uiso 1 1 calc R U . . .
C40 C 0.2428(5) 0.7564(4) 0.3488(3) 0.0298(12) Uani 1 1 d . . . . .
H40 H 0.290948 0.811131 0.334004 0.036 Uiso 1 1 calc R U . . .
C9 C 0.8162(5) 0.1455(5) 0.9875(3) 0.0297(12) Uani 1 1 d . . . . .
H9 H 0.840366 0.076454 1.032144 0.036 Uiso 1 1 calc R U . . .
C8 C 0.7016(5) 0.0275(5) 0.9413(4) 0.0354(13) Uani 1 1 d . . . . .
H8 H 0.737451 -0.028587 0.987504 0.042 Uiso 1 1 calc R U . . .
C32 C 0.1434(4) 0.7642(4) 0.6200(3) 0.0251(11) Uani 1 1 d . . . . .
H32A H 0.219945 0.743759 0.582035 0.030 Uiso 1 1 calc R U . . .
H32B H 0.164570 0.764091 0.682915 0.030 Uiso 1 1 calc R U . . .
C38 C 0.0672(6) 0.6885(5) 0.3308(4) 0.0373(13) Uani 1 1 d . . . . .
H38 H -0.007132 0.695942 0.303557 0.045 Uiso 1 1 calc R U . . .
C37 C 0.1101(5) 0.5974(5) 0.3928(4) 0.0326(13) Uani 1 1 d . . . . .
H37 H 0.062463 0.542377 0.408302 0.039 Uiso 1 1 calc R U . . .
C7 C 0.6118(6) 0.0032(5) 0.8888(4) 0.0376(13) Uani 1 1 d . . . . .
C17 C 0.6028(5) 0.0895(6) 0.5203(4) 0.0386(13) Uani 1 1 d . . . . .
H17 H 0.671019 0.052577 0.483930 0.046 Uiso 1 1 calc R U . . .
C1 C 0.1864(5) 0.0556(5) 0.7718(4) 0.0348(13) Uani 1 1 d . . . . .
H1A H 0.127338 0.018654 0.750892 0.052 Uiso 1 1 calc R U . . .
H1B H 0.144848 0.133379 0.787894 0.052 Uiso 1 1 calc R U . . .
H1C H 0.224017 0.009177 0.824773 0.052 Uiso 1 1 calc R U . . .
C16 C 0.5704(5) 0.0528(5) 0.6071(4) 0.0354(13) Uani 1 1 d . . . . .
H16 H 0.611831 -0.014227 0.642345 0.042 Uiso 1 1 calc R U . . .
C20 C 0.4281(10) 0.4111(8) 0.3109(6) 0.025(2) Uani 0.653(11) 1 d . . P A 1
H20 H 0.400902 0.495634 0.318830 0.030 Uiso 0.653(11) 1 calc R U P A 1
C13 C 0.8331(6) 0.2828(7) 1.0990(5) 0.0541(18) Uani 1 1 d . . . . .
H13A H 0.788409 0.352532 1.128249 0.065 Uiso 1 1 calc R U . . .
H13B H 0.858062 0.219060 1.146890 0.065 Uiso 1 1 calc R U . . .
C33 C 0.0704(5) 0.8840(5) 0.5870(4) 0.0359(13) Uani 1 1 d . . . . .
H33A H 0.057875 0.885912 0.522021 0.043 Uiso 1 1 calc R U . . .
H33B H 0.117462 0.941561 0.593613 0.043 Uiso 1 1 calc R U . . .
C10 C 0.9297(5) 0.1699(5) 0.9359(4) 0.0361(13) Uani 1 1 d . . . . .
H10A H 0.905566 0.233928 0.888003 0.043 Uiso 1 1 calc R U . . .
H10B H 0.974427 0.100338 0.906399 0.043 Uiso 1 1 calc R U . . .
C12 C 0.9458(6) 0.3073(6) 1.0456(5) 0.0512(17) Uani 1 1 d . . . . .
H12A H 0.921489 0.375133 1.000945 0.061 Uiso 1 1 calc R U . . .
H12B H 1.000170 0.325757 1.087028 0.061 Uiso 1 1 calc R U . . .
C11 C 1.0134(5) 0.2026(6) 0.9971(4) 0.0435(15) Uani 1 1 d . . . . .
H11A H 1.084555 0.220541 0.960818 0.052 Uiso 1 1 calc R U . . .
H11B H 1.043361 0.136363 1.042033 0.052 Uiso 1 1 calc R U . . .
C23 C 0.4206(6) 0.4513(6) 0.1108(4) 0.0464(16) Uani 1 1 d . . . . .
H23A H 0.404347 0.509042 0.057644 0.056 Uiso 0.653(11) 1 calc R U P A 1
H23B H 0.446927 0.373253 0.089198 0.056 Uiso 0.653(11) 1 calc R U P A 1
H23C H 0.496042 0.388782 0.107279 0.056 Uiso 0.347(11) 1 calc R U P A 2
H23D H 0.406100 0.489027 0.048935 0.056 Uiso 0.347(11) 1 calc R U P A 2
C34 C -0.0530(5) 0.9180(5) 0.6383(4) 0.0355(13) Uani 1 1 d . . . . .
H34A H -0.041056 0.925070 0.702086 0.043 Uiso 1 1 calc R U . . .
H34B H -0.099052 0.994180 0.611862 0.043 Uiso 1 1 calc R U . . .
C39 C 0.1359(6) 0.7698(5) 0.3089(4) 0.0433(15) Uani 1 1 d . . . . .
H39 H 0.108586 0.834449 0.266461 0.052 Uiso 1 1 calc R U . . .
C5 C 0.4753(7) -0.0669(5) 0.8267(4) 0.0509(17) Uani 1 1 d . . . . .
H5 H 0.429165 -0.117840 0.812384 0.061 Uiso 1 1 calc R U . . .
C6 C 0.5661(7) -0.0938(6) 0.8893(5) 0.059(2) Uani 1 1 d . . . . .
H6 H 0.591357 -0.165234 0.925146 0.070 Uiso 1 1 calc R U . . .
C35 C -0.1241(5) 0.8291(5) 0.6341(6) 0.061(2) Uani 1 1 d . . . . .
H35A H -0.143123 0.827442 0.570916 0.073 Uiso 1 1 calc R U . . .
H35B H -0.201889 0.849917 0.670680 0.073 Uiso 1 1 calc R U . . .
C25 C 0.3306(10) 0.3823(11) 0.2622(8) 0.034(3) Uani 0.653(11) 1 d . . P A 1
H25A H 0.254061 0.394073 0.300815 0.041 Uiso 0.653(11) 1 calc R U P A 1
H25B H 0.355317 0.299892 0.250097 0.041 Uiso 0.653(11) 1 calc R U P A 1
C36 C -0.0506(5) 0.7085(5) 0.6700(6) 0.065(2) Uani 1 1 d . . . . .
H36A H -0.035547 0.709071 0.734191 0.077 Uiso 1 1 calc R U . . .
H36B H -0.098060 0.650420 0.666161 0.077 Uiso 1 1 calc R U . . .
C21 C 0.5466(7) 0.3945(8) 0.2519(5) 0.025(2) Uani 0.653(11) 1 d . . P A 1
H21A H 0.574765 0.312864 0.237956 0.031 Uiso 0.653(11) 1 calc R U P A 1
H21B H 0.610544 0.413635 0.284048 0.031 Uiso 0.653(11) 1 calc R U P A 1
C22 C 0.5231(9) 0.4746(9) 0.1645(6) 0.038(2) Uani 0.653(11) 1 d . . P A 1
H22A H 0.599339 0.464134 0.125572 0.045 Uiso 0.653(11) 1 calc R U P A 1
H22B H 0.499737 0.555993 0.179304 0.045 Uiso 0.653(11) 1 calc R U P A 1
C24 C 0.3081(9) 0.4597(13) 0.1715(7) 0.049(3) Uani 0.653(11) 1 d . . P A 1
H24A H 0.246090 0.436577 0.139990 0.059 Uiso 0.653(11) 1 calc R U P A 1
H24B H 0.275292 0.541348 0.184373 0.059 Uiso 0.653(11) 1 calc R U P A 1
C21A C 0.4712(14) 0.4724(16) 0.2599(10) 0.032(4) Uani 0.347(11) 1 d . . P A 2
H21C H 0.485291 0.527799 0.299798 0.039 Uiso 0.347(11) 1 calc R U P A 2
H21D H 0.547517 0.411511 0.253369 0.039 Uiso 0.347(11) 1 calc R U P A 2
C20A C 0.370(2) 0.4169(18) 0.3035(12) 0.027(4) Uani 0.347(11) 1 d . . P A 2
H20A H 0.294240 0.478730 0.315152 0.033 Uiso 0.347(11) 1 calc R U P A 2
C22A C 0.4391(18) 0.5361(18) 0.1669(11) 0.043(4) Uani 0.347(11) 1 d . . P A 2
H22C H 0.364136 0.598789 0.172547 0.051 Uiso 0.347(11) 1 calc R U P A 2
H22D H 0.506028 0.570730 0.139951 0.051 Uiso 0.347(11) 1 calc R U P A 2
C25A C 0.3433(17) 0.3348(18) 0.2397(13) 0.027(4) Uani 0.347(11) 1 d . . P A 2
H25C H 0.415686 0.269629 0.233224 0.032 Uiso 0.347(11) 1 calc R U P A 2
H25D H 0.274859 0.302407 0.266720 0.032 Uiso 0.347(11) 1 calc R U P A 2
C24A C 0.3112(16) 0.3959(19) 0.1458(13) 0.039(4) Uani 0.347(11) 1 d . . P A 2
H24C H 0.234210 0.456488 0.149736 0.046 Uiso 0.347(11) 1 calc R U P A 2
H24D H 0.302039 0.339631 0.104744 0.046 Uiso 0.347(11) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.768(3) . ?
U1 O2 1.778(3) . ?
U1 N5 2.447(4) . ?
U1 N3 2.439(4) . ?
U1 N6 2.587(4) . ?
U1 N7 2.542(4) . ?
U1 N4 2.576(4) . ?
N5 C26 1.361(6) . ?
N5 C29 1.371(6) . ?
N3 C15 1.352(6) . ?
N3 C18 1.385(6) . ?
N6 C31 1.492(6) . ?
N6 C30 1.285(7) . ?
N7 C41 1.361(6) . ?
N7 C37 1.343(6) . ?
N4 C19 1.289(8) . ?
N4 C20 1.455(10) . ?
N4 C20A 1.65(2) . ?
N1 H1 0.8800 . ?
N1 C4 1.368(7) . ?
N1 C7 1.362(7) . ?
C26 C3 1.507(7) . ?
C26 C27 1.386(7) . ?
C15 C3 1.520(7) . ?
C15 C16 1.396(7) . ?
N2 C9 1.455(7) . ?
N2 C8 1.271(8) . ?
C29 C28 1.383(7) . ?
C29 C30 1.414(7) . ?
C41 H41 0.9500 . ?
C41 C40 1.385(7) . ?
C19 H19 0.9500 . ?
C19 C18 1.402(8) . ?
C3 C2 1.572(7) . ?
C3 C4 1.503(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.516(7) . ?
C4 C5 1.378(8) . ?
C31 H31 1.0000 . ?
C31 C32 1.520(7) . ?
C31 C36 1.516(8) . ?
C18 C17 1.373(8) . ?
C28 H28 0.9500 . ?
C28 C27 1.391(8) . ?
C30 H30 0.9500 . ?
C27 H27 0.9500 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C9 1.523(8) . ?
C14 C13 1.525(9) . ?
C40 H40 0.9500 . ?
C40 C39 1.366(8) . ?
C9 H9 1.0000 . ?
C9 C10 1.521(7) . ?
C8 H8 0.9500 . ?
C8 C7 1.442(8) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.521(7) . ?
C38 H38 0.9500 . ?
C38 C37 1.369(7) . ?
C38 C39 1.388(8) . ?
C37 H37 0.9500 . ?
C7 C6 1.386(9) . ?
C17 H17 0.9500 . ?
C17 C16 1.372(8) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C16 H16 0.9500 . ?
C20 H20 1.0000 . ?
C20 C25 1.505(14) . ?
C20 C21 1.528(11) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C12 1.523(8) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.523(8) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.521(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C11 1.522(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 H23C 0.9900 . ?
C23 H23D 0.9900 . ?
C23 C22 1.566(12) . ?
C23 C24 1.492(11) . ?
C23 C22A 1.45(2) . ?
C23 C24A 1.58(2) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.499(9) . ?
C39 H39 0.9500 . ?
C5 H5 0.9500 . ?
C5 C6 1.406(9) . ?
C6 H6 0.9500 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.541(8) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C24 1.556(15) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.533(12) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C21A H21C 0.9900 . ?
C21A H21D 0.9900 . ?
C21A C20A 1.54(2) . ?
C21A C22A 1.54(2) . ?
C20A H20A 1.0000 . ?
C20A C25A 1.54(2) . ?
C22A H22C 0.9900 . ?
C22A H22D 0.9900 . ?
C25A H25C 0.9900 . ?
C25A H25D 0.9900 . ?
C25A C24A 1.54(3) . ?
C24A H24C 0.9900 . ?
C24A H24D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 175.25(15) . . ?
O1 U1 N5 90.31(14) . . ?
O1 U1 N3 90.51(15) . . ?
O1 U1 N6 86.11(14) . . ?
O1 U1 N7 88.50(14) . . ?
O1 U1 N4 87.49(15) . . ?
O2 U1 N5 92.71(15) . . ?
O2 U1 N3 93.92(16) . . ?
O2 U1 N6 91.63(16) . . ?
O2 U1 N7 86.90(14) . . ?
O2 U1 N4 92.62(17) . . ?
N5 U1 N6 67.94(13) . . ?
N5 U1 N7 143.70(14) . . ?
N5 U1 N4 138.94(15) . . ?
N3 U1 N5 71.57(13) . . ?
N3 U1 N6 139.33(13) . . ?
N3 U1 N7 144.71(13) . . ?
N3 U1 N4 67.46(15) . . ?
N7 U1 N6 75.78(13) . . ?
N7 U1 N4 77.25(15) . . ?
N4 U1 N6 152.41(15) . . ?
C26 N5 U1 137.0(3) . . ?
C26 N5 C29 106.2(4) . . ?
C29 N5 U1 114.8(3) . . ?
C15 N3 U1 138.1(3) . . ?
C15 N3 C18 105.5(4) . . ?
C18 N3 U1 115.5(3) . . ?
C31 N6 U1 131.0(3) . . ?
C30 N6 U1 111.6(3) . . ?
C30 N6 C31 116.7(5) . . ?
C41 N7 U1 120.6(3) . . ?
C37 N7 U1 122.8(3) . . ?
C37 N7 C41 116.6(4) . . ?
C19 N4 U1 113.2(3) . . ?
C19 N4 C20 113.7(6) . . ?
C19 N4 C20A 127.8(8) . . ?
C20 N4 U1 132.3(5) . . ?
C20A N4 U1 117.7(7) . . ?
C4 N1 H1 124.2 . . ?
C7 N1 H1 124.2 . . ?
C7 N1 C4 111.6(5) . . ?
N5 C26 C3 122.3(4) . . ?
N5 C26 C27 110.1(4) . . ?
C27 C26 C3 127.0(5) . . ?
N3 C15 C3 122.5(4) . . ?
N3 C15 C16 110.4(5) . . ?
C16 C15 C3 126.6(5) . . ?
C8 N2 C9 118.0(5) . . ?
N5 C29 C28 110.4(5) . . ?
N5 C29 C30 120.1(5) . . ?
C28 C29 C30 129.5(5) . . ?
N7 C41 H41 118.8 . . ?
N7 C41 C40 122.5(5) . . ?
C40 C41 H41 118.8 . . ?
N4 C19 H19 118.8 . . ?
N4 C19 C18 122.4(5) . . ?
C18 C19 H19 118.8 . . ?
C26 C3 C15 114.5(4) . . ?
C26 C3 C2 108.8(4) . . ?
C15 C3 C2 106.4(4) . . ?
C4 C3 C26 109.1(4) . . ?
C4 C3 C15 107.8(4) . . ?
C4 C3 C2 110.2(4) . . ?
C3 C2 H2A 108.4 . . ?
C3 C2 H2B 108.4 . . ?
H2A C2 H2B 107.4 . . ?
C1 C2 C3 115.7(4) . . ?
C1 C2 H2A 108.4 . . ?
C1 C2 H2B 108.4 . . ?
N1 C4 C3 120.2(5) . . ?
N1 C4 C5 105.8(5) . . ?
C5 C4 C3 134.0(5) . . ?
N6 C31 H31 106.9 . . ?
N6 C31 C32 111.3(4) . . ?
N6 C31 C36 114.2(4) . . ?
C32 C31 H31 106.9 . . ?
C36 C31 H31 106.9 . . ?
C36 C31 C32 110.2(5) . . ?
N3 C18 C19 119.9(5) . . ?
C17 C18 N3 110.3(5) . . ?
C17 C18 C19 129.7(5) . . ?
C29 C28 H28 126.9 . . ?
C29 C28 C27 106.3(5) . . ?
C27 C28 H28 126.9 . . ?
N6 C30 C29 123.6(5) . . ?
N6 C30 H30 118.2 . . ?
C29 C30 H30 118.2 . . ?
C26 C27 C28 107.0(5) . . ?
C26 C27 H27 126.5 . . ?
C28 C27 H27 126.5 . . ?
H14A C14 H14B 108.0 . . ?
C9 C14 H14A 109.3 . . ?
C9 C14 H14B 109.3 . . ?
C9 C14 C13 111.5(5) . . ?
C13 C14 H14A 109.3 . . ?
C13 C14 H14B 109.3 . . ?
C41 C40 H40 120.5 . . ?
C39 C40 C41 119.0(5) . . ?
C39 C40 H40 120.5 . . ?
N2 C9 C14 108.5(4) . . ?
N2 C9 H9 109.1 . . ?
N2 C9 C10 111.0(4) . . ?
C14 C9 H9 109.1 . . ?
C10 C9 C14 110.0(5) . . ?
C10 C9 H9 109.1 . . ?
N2 C8 H8 119.5 . . ?
N2 C8 C7 121.1(5) . . ?
C7 C8 H8 119.5 . . ?
C31 C32 H32A 109.6 . . ?
C31 C32 H32B 109.6 . . ?
C31 C32 C33 110.2(4) . . ?
H32A C32 H32B 108.1 . . ?
C33 C32 H32A 109.6 . . ?
C33 C32 H32B 109.6 . . ?
C37 C38 H38 121.1 . . ?
C37 C38 C39 117.9(5) . . ?
C39 C38 H38 121.1 . . ?
N7 C37 C38 124.4(5) . . ?
N7 C37 H37 117.8 . . ?
C38 C37 H37 117.8 . . ?
N1 C7 C8 121.5(5) . . ?
N1 C7 C6 106.6(5) . . ?
C6 C7 C8 131.9(5) . . ?
C18 C17 H17 126.5 . . ?
C16 C17 C18 107.0(5) . . ?
C16 C17 H17 126.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C15 C16 H16 126.6 . . ?
C17 C16 C15 106.8(5) . . ?
C17 C16 H16 126.6 . . ?
N4 C20 H20 106.4 . . ?
N4 C20 C25 104.3(7) . . ?
N4 C20 C21 122.1(8) . . ?
C25 C20 H20 106.4 . . ?
C25 C20 C21 110.2(8) . . ?
C21 C20 H20 106.4 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
C12 C13 C14 110.9(5) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C32 C33 H33A 109.1 . . ?
C32 C33 H33B 109.1 . . ?
C32 C33 C34 112.6(4) . . ?
H33A C33 H33B 107.8 . . ?
C34 C33 H33A 109.1 . . ?
C34 C33 H33B 109.1 . . ?
C9 C10 H10A 109.2 . . ?
C9 C10 H10B 109.2 . . ?
C9 C10 C11 112.0(4) . . ?
H10A C10 H10B 107.9 . . ?
C11 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
C13 C12 H12A 109.6 . . ?
C13 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
C11 C12 C13 110.3(5) . . ?
C11 C12 H12A 109.6 . . ?
C11 C12 H12B 109.6 . . ?
C10 C11 C12 110.4(5) . . ?
C10 C11 H11A 109.6 . . ?
C10 C11 H11B 109.6 . . ?
C12 C11 H11A 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
H23A C23 H23B 108.3 . . ?
H23C C23 H23D 107.7 . . ?
C22 C23 H23A 109.9 . . ?
C22 C23 H23B 109.9 . . ?
C24 C23 H23A 109.9 . . ?
C24 C23 H23B 109.9 . . ?
C24 C23 C22 108.8(7) . . ?
C22A C23 H23C 108.8 . . ?
C22A C23 H23D 108.8 . . ?
C22A C23 C24A 114.0(10) . . ?
C24A C23 H23C 108.8 . . ?
C24A C23 H23D 108.8 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 108.1 . . ?
C35 C34 C33 110.5(5) . . ?
C35 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
C40 C39 C38 119.7(5) . . ?
C40 C39 H39 120.1 . . ?
C38 C39 H39 120.1 . . ?
C4 C5 H5 125.6 . . ?
C4 C5 C6 108.7(6) . . ?
C6 C5 H5 125.6 . . ?
C7 C6 C5 107.2(6) . . ?
C7 C6 H6 126.4 . . ?
C5 C6 H6 126.4 . . ?
C34 C35 H35A 109.6 . . ?
C34 C35 H35B 109.6 . . ?
C34 C35 C36 110.3(5) . . ?
H35A C35 H35B 108.1 . . ?
C36 C35 H35A 109.6 . . ?
C36 C35 H35B 109.6 . . ?
C20 C25 H25A 109.4 . . ?
C20 C25 H25B 109.4 . . ?
C20 C25 C24 111.1(9) . . ?
H25A C25 H25B 108.0 . . ?
C24 C25 H25A 109.4 . . ?
C24 C25 H25B 109.4 . . ?
C31 C36 C35 110.7(6) . . ?
C31 C36 H36A 109.5 . . ?
C31 C36 H36B 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 108.1 . . ?
C20 C21 H21A 110.0 . . ?
C20 C21 H21B 110.0 . . ?
C20 C21 C22 108.4(7) . . ?
H21A C21 H21B 108.4 . . ?
C22 C21 H21A 110.0 . . ?
C22 C21 H21B 110.0 . . ?
C23 C22 H22A 109.0 . . ?
C23 C22 H22B 109.0 . . ?
C21 C22 C23 113.0(7) . . ?
C21 C22 H22A 109.0 . . ?
C21 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
C23 C24 C25 112.9(8) . . ?
C23 C24 H24A 109.0 . . ?
C23 C24 H24B 109.0 . . ?
C25 C24 H24A 109.0 . . ?
C25 C24 H24B 109.0 . . ?
H24A C24 H24B 107.8 . . ?
H21C C21A H21D 107.9 . . ?
C20A C21A H21C 109.3 . . ?
C20A C21A H21D 109.3 . . ?
C22A C21A H21C 109.3 . . ?
C22A C21A H21D 109.3 . . ?
C22A C21A C20A 111.7(14) . . ?
N4 C20A H20A 109.6 . . ?
C21A C20A N4 104.9(15) . . ?
C21A C20A H20A 109.6 . . ?
C21A C20A C25A 109.4(16) . . ?
C25A C20A N4 113.6(15) . . ?
C25A C20A H20A 109.6 . . ?
C23 C22A C21A 107.2(14) . . ?
C23 C22A H22C 110.3 . . ?
C23 C22A H22D 110.3 . . ?
C21A C22A H22C 110.3 . . ?
C21A C22A H22D 110.3 . . ?
H22C C22A H22D 108.5 . . ?
C20A C25A H25C 109.1 . . ?
C20A C25A H25D 109.1 . . ?
H25C C25A H25D 107.8 . . ?
C24A C25A C20A 112.6(17) . . ?
C24A C25A H25C 109.1 . . ?
C24A C25A H25D 109.1 . . ?
C23 C24A H24C 110.6 . . ?
C23 C24A H24D 110.6 . . ?
C25A C24A C23 105.5(13) . . ?
C25A C24A H24C 110.6 . . ?
C25A C24A H24D 110.6 . . ?
H24C C24A H24D 108.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 N5 C26 C3 -26.0(7) . . . . ?
U1 N5 C26 C27 162.1(4) . . . . ?
U1 N5 C29 C28 -166.8(3) . . . . ?
U1 N5 C29 C30 13.6(6) . . . . ?
U1 N3 C15 C3 19.9(8) . . . . ?
U1 N3 C15 C16 -167.5(4) . . . . ?
U1 N3 C18 C19 -12.1(6) . . . . ?
U1 N3 C18 C17 170.8(4) . . . . ?
U1 N6 C31 C32 -86.5(5) . . . . ?
U1 N6 C31 C36 147.9(5) . . . . ?
U1 N6 C30 C29 -7.6(6) . . . . ?
U1 N7 C41 C40 178.9(4) . . . . ?
U1 N7 C37 C38 -178.9(5) . . . . ?
U1 N4 C19 C18 7.0(7) . . . . ?
U1 N4 C20 C25 -87.1(9) . . . . ?
U1 N4 C20 C21 147.4(6) . . . . ?
U1 N4 C20A C21A 122.6(11) . . . . ?
U1 N4 C20A C25A -117.9(13) . . . . ?
N5 C26 C3 C15 44.1(6) . . . . ?
N5 C26 C3 C2 -74.8(6) . . . . ?
N5 C26 C3 C4 164.9(4) . . . . ?
N5 C26 C27 C28 0.3(6) . . . . ?
N5 C29 C28 C27 0.2(6) . . . . ?
N5 C29 C30 N6 -3.7(8) . . . . ?
N3 C15 C3 C26 -41.2(7) . . . . ?
N3 C15 C3 C2 79.0(6) . . . . ?
N3 C15 C3 C4 -162.8(5) . . . . ?
N3 C15 C16 C17 0.0(6) . . . . ?
N3 C18 C17 C16 0.0(6) . . . . ?
N6 C31 C32 C33 175.7(4) . . . . ?
N6 C31 C36 C35 -175.3(6) . . . . ?
N7 C41 C40 C39 1.0(8) . . . . ?
N4 C19 C18 N3 3.1(8) . . . . ?
N4 C19 C18 C17 179.6(6) . . . . ?
N4 C20 C25 C24 168.7(8) . . . . ?
N4 C20 C21 C22 -177.7(8) . . . . ?
N4 C20A C25A C24A -172.8(13) . . . . ?
N1 C4 C5 C6 1.9(8) . . . . ?
N1 C7 C6 C5 -0.4(8) . . . . ?
C26 N5 C29 C28 0.0(6) . . . . ?
C26 N5 C29 C30 -179.6(4) . . . . ?
C26 C3 C2 C1 -50.6(6) . . . . ?
C26 C3 C4 N1 -53.2(6) . . . . ?
C26 C3 C4 C5 129.3(7) . . . . ?
C15 N3 C18 C19 177.1(5) . . . . ?
C15 N3 C18 C17 0.0(6) . . . . ?
C15 C3 C2 C1 -174.4(4) . . . . ?
C15 C3 C4 N1 71.7(6) . . . . ?
C15 C3 C4 C5 -105.8(7) . . . . ?
N2 C9 C10 C11 175.9(5) . . . . ?
N2 C8 C7 N1 -5.8(9) . . . . ?
N2 C8 C7 C6 177.1(7) . . . . ?
C29 N5 C26 C3 171.8(4) . . . . ?
C29 N5 C26 C27 -0.1(6) . . . . ?
C29 C28 C27 C26 -0.3(6) . . . . ?
C41 N7 C37 C38 1.2(8) . . . . ?
C41 C40 C39 C38 -0.5(9) . . . . ?
C19 N4 C20 C25 104.2(9) . . . . ?
C19 N4 C20 C21 -21.3(11) . . . . ?
C19 N4 C20A C21A -71.3(16) . . . . ?
C19 N4 C20A C25A 48.3(18) . . . . ?
C19 C18 C17 C16 -176.8(5) . . . . ?
C3 C26 C27 C28 -171.2(5) . . . . ?
C3 C15 C16 C17 172.2(5) . . . . ?
C3 C4 C5 C6 179.6(6) . . . . ?
C2 C3 C4 N1 -172.6(4) . . . . ?
C2 C3 C4 C5 9.9(9) . . . . ?
C4 N1 C7 C8 -176.1(5) . . . . ?
C4 N1 C7 C6 1.7(7) . . . . ?
C4 C3 C2 C1 69.0(6) . . . . ?
C4 C5 C6 C7 -0.9(9) . . . . ?
C31 N6 C30 C29 -179.2(5) . . . . ?
C31 C32 C33 C34 55.3(6) . . . . ?
C18 N3 C15 C3 -172.6(5) . . . . ?
C18 N3 C15 C16 0.0(6) . . . . ?
C18 C17 C16 C15 0.0(6) . . . . ?
C28 C29 C30 N6 176.9(5) . . . . ?
C30 N6 C31 C32 83.1(5) . . . . ?
C30 N6 C31 C36 -42.6(7) . . . . ?
C30 C29 C28 C27 179.7(5) . . . . ?
C27 C26 C3 C15 -145.4(5) . . . . ?
C27 C26 C3 C2 95.7(6) . . . . ?
C27 C26 C3 C4 -24.6(7) . . . . ?
C14 C9 C10 C11 55.8(7) . . . . ?
C14 C13 C12 C11 -57.0(8) . . . . ?
C9 N2 C8 C7 174.5(5) . . . . ?
C9 C14 C13 C12 56.5(8) . . . . ?
C9 C10 C11 C12 -57.2(7) . . . . ?
C8 N2 C9 C14 -115.3(6) . . . . ?
C8 N2 C9 C10 123.7(6) . . . . ?
C8 C7 C6 C5 177.0(7) . . . . ?
C32 C31 C36 C35 58.4(8) . . . . ?
C32 C33 C34 C35 -55.6(7) . . . . ?
C37 N7 C41 C40 -1.3(7) . . . . ?
C37 C38 C39 C40 0.4(9) . . . . ?
C7 N1 C4 C3 179.7(5) . . . . ?
C7 N1 C4 C5 -2.2(7) . . . . ?
C16 C15 C3 C26 147.4(5) . . . . ?
C16 C15 C3 C2 -92.4(6) . . . . ?
C16 C15 C3 C4 25.8(7) . . . . ?
C20 N4 C19 C18 177.9(6) . . . . ?
C20 C25 C24 C23 56.4(13) . . . . ?
C20 C21 C22 C23 -58.4(9) . . . . ?
C13 C14 C9 N2 -176.8(5) . . . . ?
C13 C14 C9 C10 -55.2(7) . . . . ?
C13 C12 C11 C10 57.0(7) . . . . ?
C33 C34 C35 C36 56.0(8) . . . . ?
C34 C35 C36 C31 -58.5(9) . . . . ?
C39 C38 C37 N7 -0.8(9) . . . . ?
C25 C20 C21 C22 59.5(10) . . . . ?
C36 C31 C32 C33 -56.4(6) . . . . ?
C21 C20 C25 C24 -58.6(12) . . . . ?
C22 C23 C24 C25 -52.5(12) . . . . ?
C24 C23 C22 C21 55.1(10) . . . . ?
C21A C20A C25A C24A -56(2) . . . . ?
C20A N4 C19 C18 -159.7(10) . . . . ?
C20A C21A C22A C23 -59.6(19) . . . . ?
C20A C25A C24A C23 55.2(18) . . . . ?
C22A C23 C24A C25A -61.0(16) . . . . ?
C22A C21A C20A N4 178.6(14) . . . . ?
C22A C21A C20A C25A 56(2) . . . . ?
C24A C23 C22A C21A 62.9(16) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.482
_oxdiff_exptl_absorpt_empirical_full_min 0.832
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Pyridene, hexane'
_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_jl23019_231123_sadabs
_database_code_depnum_ccdc_archive 'CCDC 2313509'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2023-12-11 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_audit_creation_date             2023-11-24
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C80 H110 N12 O6 U2 Y2'
_chemical_formula_sum            'C80 H110 N12 O6 U2 Y2'
_chemical_formula_weight         1989.67
_chemical_melting_point          ?
_chemical_oxdiff_formula         C72H100N12O4Y2U2
_chemical_oxdiff_usercomment     '@ 120 K JHPC TO517-3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -0.2670 2.0244 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   15.3299(4)
_cell_length_b                   16.2642(4)
_cell_length_c                   21.1749(4)
_cell_angle_alpha                74.514(2)
_cell_angle_beta                 87.911(2)
_cell_angle_gamma                82.799(2)
_cell_volume                     5047.7(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    47441
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.7540
_cell_measurement_theta_min      4.2410
_shelx_estimated_absorpt_T_max   0.579
_shelx_estimated_absorpt_T_min   0.113
_exptl_absorpt_coefficient_mu    10.768
_exptl_absorpt_correction_T_max  0.5882
_exptl_absorpt_correction_T_min  0.1098
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1210 before and 0.0749 after correction.
The Ratio of minimum to maximum transmission is 0.1867.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       blade
_exptl_crystal_F_000             1968
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.0328
1 0 0 0.0246
0 0 -1 0.1634
0 0 1 0.1385
1 2 2 0.0313
0 2 -1 0.1662
0 -2 1 0.1603
0 -1 -1 0.0496
0 1 1 0.0364

_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.057
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.9987 0.0004 0.0005 0.0964 -0.0305 -0.0033
0.9987 -0.0004 -0.0005 -0.0964 0.0305 0.0033
0.0023 -0.0003 -0.9995 -0.0063 -0.0258 0.0706
-0.0023 0.0003 0.9995 0.0063 0.0258 -0.0706
1.0023 1.9996 2.0017 -0.0104 0.2257 -0.0233
0.0104 1.9992 -0.9964 0.0673 0.1177 0.1852
-0.0104 -1.9992 0.9964 -0.0673 -0.1177 -0.1852
-0.0018 -1.0000 -1.0011 -0.0430 -0.0976 0.0133
0.0018 1.0000 1.0011 0.0430 0.0976 -0.0133

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            107929
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.932
_diffrn_reflns_theta_min         3.630
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2792
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -118.00 -16.00   1.00    5.00    --  -42.00 -27.00  -4.00  102
  2  ω     16.00 118.00   1.00    5.00    --   42.00  27.00 157.00  102
  3  ω    -34.00  68.00   1.00    5.00    --   42.00 -27.00  -4.00  102
  4  ω     35.00 137.00   1.00   20.00    --  111.00 -27.00  -4.00  102
  5  ω     85.00 178.00   1.00   20.00    --  111.00  27.00 157.00   93
  6  ω    -65.00  31.00   1.00    5.00    --  -42.00  38.00 -60.00   96
  7  ω    -68.00  34.00   1.00    5.00    --  -42.00  27.00 157.00  102
  8  ω   -126.00 -37.00   1.00    5.00    --  -42.00 178.00 120.00   89
  9  ω     10.00  42.00   1.00    5.00    --   42.00  80.00  64.74   32
 10  ω     10.00  42.00   1.00    5.00    --   42.00  80.00 -33.33   32
 11  ω      9.00  42.00   1.00    5.00    --   42.00  82.00  14.12   33
 12  ω     10.00  42.00   1.00    5.00    --   42.00  79.00 157.13   32
 13  ω     61.00 129.00   1.00    5.00    --   42.00 178.00 -90.00   68
 14  ω     10.00  42.00   1.00    5.00    --   42.00  78.00  35.18   32
 15  ω     37.00 108.00   1.00   20.00    --  111.00-107.00 101.80   71
 16  ω     41.00 131.00   1.00   20.00    --  111.00-152.00 -83.39   90
 17  ω     30.00 107.00   1.00   20.00    --  111.00 -94.00-150.00   77
 18  ω     99.00 177.00   1.00   20.00    --  111.00  45.00   0.00   78
 19  ω     61.00 107.00   1.00   20.00    --  111.00 -94.00   0.00   46
 20  ω    121.00 148.00   1.00   20.00    --  111.00 125.00  60.00   27
 21  ω     74.00 107.00   1.00   20.00    --  111.00 -94.00  30.00   33
 22  ω    124.00 174.00   1.00   20.00    --  111.00  15.00-120.00   50
 23  ω     44.00 127.00   1.00   20.00    --  111.00 -61.00-180.00   83
 24  ω     80.00 107.00   1.00   20.00    --  111.00 -94.00 120.00   27
 25  ω     76.00 107.00   1.00   20.00    --  111.00 -94.00-180.00   31
 26  ω    106.00 139.00   1.00   20.00    --  111.00  45.00 -60.00   33
 27  ω     43.00  68.00   1.00   20.00    --  111.00-125.00  60.00   25
 28  ω     99.00 126.00   1.00   20.00    --  111.00 -45.00  30.00   27
 29  ω     98.00 161.00   1.00   20.00    --  111.00 125.00 -90.00   63
 30  ω     42.00 112.00   1.00   20.00    --  111.00-125.00   0.00   70
 31  ω    122.00 165.00   1.00   20.00    --  111.00 125.00-180.00   43
 32  ω     92.00 119.00   1.00   20.00    --  111.00-134.00 -88.39   27
 33  ω     88.00 125.00   1.00   20.00    --  111.00  30.00 -90.00   37
 34  ω     89.00 114.00   1.00   20.00    --  111.00  15.00-120.00   25
 35  ω    104.00 177.00   1.00   20.00    --  111.00  77.00  60.00   73
 36  ω     38.00  65.00   1.00   20.00    --  111.00 -94.00 120.00   27
 37  ω    114.00 165.00   1.00   20.00    --  111.00  30.00-180.00   51
 38  ω     57.00  84.00   1.00   20.00    --  111.00 -77.00 -30.00   27
 39  ω     76.00 103.00   1.00   20.00    --  111.00 -71.00 -41.58   27
 40  ω     44.00 109.00   1.00   20.00    --  111.00-112.00   2.71   65
 41  ω     45.00  70.00   1.00   20.00    --  111.00-107.00-102.22   25
 42  ω     78.00 108.00   1.00   20.00    --  111.00-107.00-102.22   30
 43  ω     44.00  81.00   1.00   20.00    --  111.00 -45.00 -30.00   37
 44  ω    142.00 168.00   1.00   20.00    --  111.00 101.00   0.90   26
 45  ω     42.00  69.00   1.00   20.00    --  111.00 -94.00-180.00   27
 46  ω     82.00 108.00   1.00   20.00    --  111.00-105.00 -87.12   26
 47  ω     83.00 125.00   1.00   20.00    --  111.00  68.00  82.95   42
 48  ω     85.00 113.00   1.00   20.00    --  111.00  66.00 -96.45   28
 49  ω    133.00 177.00   1.00   20.00    --  111.00  66.00 -96.45   44
 50  ω    127.00 154.00   1.00   20.00    --  111.00  30.00 120.00   27
 51  ω     80.00 112.00   1.00   20.00    --  111.00-125.00  60.00   32
 52  ω     52.00  88.00   1.00   20.00    --  111.00 -94.00 -90.00   36
 53  ω     71.00 107.00   1.00   20.00    --  111.00 -94.00  90.00   36
 54  ω     69.00  96.00   1.00   20.00    --  111.00-125.00  90.00   27
 55  ω     94.00 146.00   1.00   20.00    --  111.00  56.00 -63.77   52
 56  ω     84.00 124.00   1.00   20.00    --  111.00  61.00-180.00   40
 57  ω    129.00 155.00   1.00   20.00    --  111.00  61.00-180.00   26
 58  ω    100.00 129.00   1.00   20.00    --  111.00  70.00-112.42   29
 59  ω    138.00 166.00   1.00   20.00    --  111.00  70.00-112.42   28
 60  ω     77.00 108.00   1.00   20.00    --  111.00-125.00 120.00   31
 61  ω     65.00  92.00   1.00   20.00    --  111.00 -94.00 -60.00   27
 62  ω     41.00  87.00   1.00   20.00    --  111.00 -45.00   0.00   46
 63  ω    148.00 178.00   1.00   20.00    --  111.00 125.00-120.00   30
 64  ω    131.00 158.00   1.00   20.00    --  111.00 125.00 120.00   27
 65  ω    114.00 141.00   1.00   20.00    --  111.00  45.00-180.00   27
 66  ω     88.00 147.00   1.00   20.00    --  111.00  45.00  36.65   59
 67  ω    104.00 131.00   1.00   20.00    --  111.00 -77.00   0.00   27
 68  ω    101.00 128.00   1.00   20.00    --  111.00  30.00  90.00   27
 69  ω    107.00 134.00   1.00   20.00    --  111.00  30.00  30.00   27
 70  ω     95.00 132.00   1.00   20.00    --  111.00 -45.00   0.00   37
 71  ω     85.00 124.00   1.00   20.00    --  111.00  62.00-168.61   39
 72  ω    131.00 160.00   1.00   20.00    --  111.00  30.00 -90.00   29
 73  ω    105.00 176.00   1.00   20.00    --  111.00  77.00 120.00   71
 74  ω     71.00 116.00   1.00   20.00    --  111.00 -61.00  90.00   45
 75  ω    102.00 141.00   1.00   20.00    --  111.00 -77.00  60.00   39
 76  ω     81.00 108.00   1.00   20.00    --  111.00 -84.00 171.87   27
 77  ω     96.00 123.00   1.00   20.00    --  111.00 -86.00 123.27   27
 78  ω     37.00  69.00   1.00   20.00    --  111.00 -94.00  30.00   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0965039000
_diffrn_orient_matrix_UB_12      0.0371506000
_diffrn_orient_matrix_UB_13      0.0060286000
_diffrn_orient_matrix_UB_21      0.0305996000
_diffrn_orient_matrix_UB_22      0.0716021000
_diffrn_orient_matrix_UB_23      0.0258887000
_diffrn_orient_matrix_UB_31      0.0033144000
_diffrn_orient_matrix_UB_32      0.0574030000
_diffrn_orient_matrix_UB_33      -0.0706610000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                16990
_reflns_number_total             20831
_reflns_odcompleteness_completeness 97.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     76.86
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         4.558
_refine_diff_density_min         -5.129
_refine_diff_density_rms         0.181
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     949
_refine_ls_number_reflns         20831
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0576
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0372P)²+69.4686P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1457
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H3BC)=Sof(H3BD)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C80)=Sof(H80A)=Sof(H80B)=
 Sof(C79A)=Sof(H79C)=Sof(H79D)=1-FVAR(1)
 Sof(H3AA)=Sof(H3AB)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(C79)=Sof(H79A)=Sof(H79B)=
 Sof(C78)=Sof(H78A)=Sof(H78B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C20(H20), C27(H27), C28(H28), C31(H31), C45(H45), C56(H56), C63(H63),
 C64(H64), C67(H67), C81(H81)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
  C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,
 H36B), C38(H38A,H38B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B),
 C49(H49A,H49B), C50(H50A,H50B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B),
  C60(H60A,H60B), C61(H61A,H61B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,
 H70B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B),
 C75(H75A,H75B), C76(H76A,H76B), C82(H82A,H82B), C3(H3AA,H3AB), C3(H3BC,H3BD),
 C10(H10A,H10B), C77(H77A,H77B), C79(H79A,H79B), C78(H78A,H78B), C80(H80A,H80B),
  C79A(H79C,H79D)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C16(H16), C17(H17), C19(H19), C30(H30), C41(H41),
 C42(H42), C44(H44), C52(H52), C53(H53), C55(H55), C66(H66)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C37(H37A,H37B,H37C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.69831(2) 0.80890(2) 0.19805(2) 0.03146(8) Uani 1 1 d . . . . .
U2 U 0.55792(2) 0.65728(2) 0.28784(2) 0.02821(8) Uani 1 1 d . . . . .
Y1 Y 0.67601(5) 0.81726(5) 0.35990(4) 0.03580(18) Uani 1 1 d . . . . .
Y2 Y 0.69354(5) 0.56849(5) 0.18299(3) 0.03005(15) Uani 1 1 d . . . . .
O1 O 0.7513(4) 0.8543(4) 0.2673(3) 0.0372(14) Uani 1 1 d . . . . .
O2 O 0.6079(4) 0.7776(3) 0.2850(2) 0.0271(12) Uani 1 1 d . . . . .
O3 O 0.6392(4) 0.6946(3) 0.1966(2) 0.0236(11) Uani 1 1 d . . . . .
O4 O 0.6032(4) 0.5431(3) 0.2680(3) 0.0290(12) Uani 1 1 d . . . . .
O5 O 0.7225(5) 0.8113(5) 0.4743(3) 0.056(2) Uani 1 1 d . . . . .
O6 O 0.8006(5) 0.4589(4) 0.1458(3) 0.0452(16) Uani 1 1 d . . . . .
N1 N 0.4137(5) 0.7108(5) 0.3277(3) 0.0359(16) Uani 1 1 d . . . . .
N2 N 0.4315(5) 0.6946(4) 0.2036(3) 0.0308(15) Uani 1 1 d . . . . .
N3 N 0.5368(5) 0.8531(5) 0.4057(4) 0.0408(19) Uani 1 1 d . . . . .
N4 N 0.6580(6) 0.9709(6) 0.3569(4) 0.049(2) Uani 1 1 d . . . . .
N5 N 0.6147(5) 0.6859(5) 0.4163(3) 0.0365(17) Uani 1 1 d . . . . .
N6 N 0.7939(5) 0.6908(6) 0.3926(4) 0.047(2) Uani 1 1 d . . . . .
N7 N 0.6782(5) 0.8659(5) 0.0773(4) 0.0365(17) Uani 1 1 d . . . . .
N8 N 0.5804(5) 0.9410(4) 0.1619(4) 0.0340(16) Uani 1 1 d . . . . .
N9 N 0.8072(5) 0.6643(5) 0.1492(3) 0.0334(16) Uani 1 1 d . . . . .
N10 N 0.8196(5) 0.5311(5) 0.2628(4) 0.0378(17) Uani 1 1 d . . . . .
N11 N 0.6883(5) 0.6299(5) 0.0674(4) 0.0360(17) Uani 1 1 d . . . . .
N12 N 0.5987(5) 0.4891(5) 0.1342(3) 0.0338(16) Uani 1 1 d . . . . .
C1 C 0.4665(8) 0.6655(8) 0.5643(5) 0.055(3) Uani 1 1 d . . . . .
H1A H 0.520321 0.628208 0.559690 0.083 Uiso 1 1 calc R U . . .
H1B H 0.434771 0.638252 0.603890 0.083 Uiso 1 1 calc R U . . .
H1C H 0.481710 0.720893 0.567872 0.083 Uiso 1 1 calc R U . . .
C2 C 0.4086(7) 0.6799(7) 0.5049(4) 0.043(2) Uani 1 1 d . . . . .
H2A H 0.354146 0.716945 0.510587 0.052 Uiso 1 1 calc R U . . .
H2B H 0.391626 0.623861 0.503060 0.052 Uiso 1 1 calc R U . . .
C9 C 0.4516(6) 0.7217(6) 0.4389(4) 0.036(2) Uani 1 1 d . . . . .
C4 C 0.3846(6) 0.7296(6) 0.3846(4) 0.0349(19) Uani 1 1 d . . . . .
C5 C 0.2957(7) 0.7552(7) 0.3829(5) 0.043(2) Uani 1 1 d . . . . .
H5 H 0.260932 0.770803 0.416879 0.052 Uiso 1 1 calc R U . . .
C6 C 0.2663(7) 0.7540(7) 0.3214(5) 0.043(2) Uani 1 1 d . . . . .
H6 H 0.207875 0.768502 0.305111 0.052 Uiso 1 1 calc R U . . .
C7 C 0.3411(6) 0.7269(6) 0.2888(4) 0.037(2) Uani 1 1 d . . . . .
C8 C 0.3543(6) 0.7183(5) 0.2237(4) 0.0331(18) Uani 1 1 d . . . . .
H8 H 0.305649 0.730206 0.194789 0.040 Uiso 1 1 calc R U . . .
C11 C 0.4933(8) 0.7832(7) 0.0240(5) 0.049(2) Uani 1 1 d . . . . .
H11A H 0.545419 0.740510 0.024368 0.058 Uiso 1 1 calc R U . . .
H11B H 0.508591 0.840457 -0.000605 0.058 Uiso 1 1 calc R U . . .
C12 C 0.4156(8) 0.7599(9) -0.0097(5) 0.057(3) Uani 1 1 d . . . . .
H12A H 0.365494 0.805851 -0.013877 0.069 Uiso 1 1 calc R U . . .
H12B H 0.433414 0.755993 -0.054285 0.069 Uiso 1 1 calc R U . . .
C13 C 0.3870(8) 0.6751(8) 0.0294(5) 0.052(3) Uani 1 1 d . . . . .
H13A H 0.435327 0.628384 0.030202 0.063 Uiso 1 1 calc R U . . .
H13B H 0.335599 0.662798 0.008054 0.063 Uiso 1 1 calc R U . . .
C14 C 0.3626(7) 0.6779(7) 0.1002(4) 0.044(2) Uani 1 1 d . . . . .
H14A H 0.313273 0.723524 0.099725 0.052 Uiso 1 1 calc R U . . .
H14B H 0.343775 0.622200 0.125019 0.052 Uiso 1 1 calc R U . . .
C15 C 0.4682(7) 0.8127(7) 0.4385(4) 0.041(2) Uani 1 1 d . . . . .
C16 C 0.4140(7) 0.8688(7) 0.4668(5) 0.050(3) Uani 1 1 d . . . . .
H16 H 0.363037 0.855873 0.492682 0.060 Uiso 1 1 calc R U . . .
C17 C 0.4483(7) 0.9474(7) 0.4501(5) 0.051(3) Uani 1 1 d . . . . .
H17 H 0.424825 0.998631 0.461220 0.061 Uiso 1 1 calc R U . . .
C18 C 0.5239(7) 0.9350(7) 0.4139(5) 0.045(2) Uani 1 1 d . . . . .
C19 C 0.5854(8) 0.9940(7) 0.3870(5) 0.050(3) Uani 1 1 d . . . . .
H19 H 0.574068 1.051289 0.390721 0.060 Uiso 1 1 calc R U . . .
C20 C 0.7166(8) 1.0367(7) 0.3298(6) 0.057(3) Uani 1 1 d . . . . .
H20 H 0.708691 1.080504 0.355496 0.069 Uiso 1 1 calc R U . . .
C21 C 0.6928(9) 1.0800(7) 0.2599(7) 0.066(4) Uani 1 1 d . . . . .
H21A H 0.631191 1.107419 0.257727 0.079 Uiso 1 1 calc R U . . .
H21B H 0.697105 1.036487 0.234632 0.079 Uiso 1 1 calc R U . . .
C22 C 0.7534(11) 1.1485(9) 0.2287(10) 0.093(6) Uani 1 1 d . . . . .
H22A H 0.739880 1.172207 0.181509 0.112 Uiso 1 1 calc R U . . .
H22B H 0.743991 1.196205 0.250026 0.112 Uiso 1 1 calc R U . . .
C23 C 0.8488(11) 1.1071(10) 0.2374(11) 0.103(7) Uani 1 1 d . . . . .
H23A H 0.859072 1.065827 0.210279 0.124 Uiso 1 1 calc R U . . .
H23B H 0.887708 1.152398 0.220673 0.124 Uiso 1 1 calc R U . . .
C24 C 0.8744(11) 1.0609(11) 0.3067(9) 0.086(5) Uani 1 1 d . . . . .
H24A H 0.935319 1.032010 0.307605 0.103 Uiso 1 1 calc R U . . .
H24B H 0.872370 1.102801 0.333321 0.103 Uiso 1 1 calc R U . . .
C25 C 0.8130(9) 0.9958(9) 0.3352(7) 0.072(4) Uani 1 1 d . . . . .
H25A H 0.827744 0.968826 0.381838 0.086 Uiso 1 1 calc R U . . .
H25B H 0.820682 0.950132 0.311796 0.086 Uiso 1 1 calc R U . . .
C26 C 0.5329(6) 0.6634(5) 0.4301(5) 0.0359(19) Uani 1 1 d . . . . .
C27 C 0.5334(7) 0.5754(6) 0.4284(4) 0.036(2) Uani 1 1 d . . . . .
H27 H 0.486369 0.538414 0.447064 0.044 Uiso 1 1 calc R U . . .
C28 C 0.6201(6) 0.5451(6) 0.4172(4) 0.037(2) Uani 1 1 d . . . . .
H28 H 0.644962 0.483281 0.426285 0.044 Uiso 1 1 calc R U . . .
C29 C 0.6694(7) 0.6154(6) 0.4092(4) 0.038(2) Uani 1 1 d . . . . .
C30 C 0.7619(7) 0.6178(6) 0.4027(4) 0.039(2) Uani 1 1 d . . . . .
H30 H 0.800214 0.566239 0.405779 0.047 Uiso 1 1 calc R U . . .
C31 C 0.8917(8) 0.6839(9) 0.3977(6) 0.065(4) Uani 1 1 d . . . . .
H31 H 0.918266 0.648428 0.368303 0.078 Uiso 1 1 calc R U . . .
C32 C 0.9243(8) 0.6390(9) 0.4689(7) 0.065(3) Uani 1 1 d . . . . .
H32A H 0.899539 0.673180 0.499030 0.078 Uiso 1 1 calc R U . . .
H32B H 0.904404 0.581246 0.483722 0.078 Uiso 1 1 calc R U . . .
C33 C 1.0243(10) 0.6309(10) 0.4699(9) 0.084(4) Uani 1 1 d . . . . .
H33A H 1.048855 0.592758 0.442530 0.101 Uiso 1 1 calc R U . . .
H33B H 1.045488 0.604805 0.515325 0.101 Uiso 1 1 calc R U . . .
C34 C 1.0562(8) 0.7200(10) 0.4436(7) 0.078(4) Uani 1 1 d . . . . .
H34A H 1.037444 0.755539 0.474226 0.093 Uiso 1 1 calc R U . . .
H34B H 1.121247 0.713146 0.441827 0.093 Uiso 1 1 calc R U . . .
C35 C 1.0215(10) 0.7644(13) 0.3784(7) 0.094(6) Uani 1 1 d . . . . .
H35A H 1.047740 0.733318 0.346627 0.113 Uiso 1 1 calc R U . . .
H35B H 1.039381 0.822977 0.365358 0.113 Uiso 1 1 calc R U . . .
C36 C 0.9221(9) 0.7708(10) 0.3749(7) 0.076(4) Uani 1 1 d . . . . .
H36A H 0.895281 0.807513 0.402722 0.091 Uiso 1 1 calc R U . . .
H36B H 0.902728 0.798050 0.329250 0.091 Uiso 1 1 calc R U . . .
C37 C 0.9183(8) 0.6967(7) -0.0126(6) 0.058(3) Uani 1 1 d . . . . .
H37A H 0.965273 0.712036 -0.044650 0.087 Uiso 1 1 calc R U . . .
H37B H 0.889996 0.650398 -0.021802 0.087 Uiso 1 1 calc R U . . .
H37C H 0.943289 0.677358 0.031614 0.087 Uiso 1 1 calc R U . . .
C38 C 0.8510(7) 0.7743(6) -0.0171(5) 0.045(2) Uani 1 1 d . . . . .
H38A H 0.825599 0.792515 -0.061704 0.054 Uiso 1 1 calc R U . . .
H38B H 0.881348 0.821982 -0.011109 0.054 Uiso 1 1 calc R U . . .
C39 C 0.7748(7) 0.7598(6) 0.0336(4) 0.040(2) Uani 1 1 d . . . . .
C40 C 0.7161(7) 0.8435(6) 0.0248(4) 0.039(2) Uani 1 1 d . . . . .
C41 C 0.6887(7) 0.9065(6) -0.0332(5) 0.044(2) Uani 1 1 d . . . . .
H41 H 0.705365 0.905766 -0.076779 0.053 Uiso 1 1 calc R U . . .
C42 C 0.6329(7) 0.9694(7) -0.0143(5) 0.045(2) Uani 1 1 d . . . . .
H42 H 0.604105 1.020713 -0.042124 0.053 Uiso 1 1 calc R U . . .
C43 C 0.6275(6) 0.9421(6) 0.0541(5) 0.039(2) Uani 1 1 d . . . . .
C44 C 0.5761(7) 0.9793(6) 0.0995(4) 0.038(2) Uani 1 1 d . . . . .
H44 H 0.538985 1.031809 0.084208 0.046 Uiso 1 1 calc R U . . .
C45 C 0.5186(6) 0.9775(6) 0.2065(4) 0.0359(19) Uani 1 1 d . . . . .
H45 H 0.549619 0.968585 0.248933 0.043 Uiso 1 1 calc R U . . .
C46 C 0.4854(7) 1.0730(6) 0.1820(6) 0.048(2) Uani 1 1 d . . . . .
H46A H 0.451364 1.083248 0.141190 0.058 Uiso 1 1 calc R U . . .
H46B H 0.536038 1.106593 0.171898 0.058 Uiso 1 1 calc R U . . .
C47 C 0.4269(8) 1.1030(7) 0.2339(6) 0.054(3) Uani 1 1 d . . . . .
H47A H 0.461797 1.095647 0.273875 0.065 Uiso 1 1 calc R U . . .
H47B H 0.405458 1.164814 0.217062 0.065 Uiso 1 1 calc R U . . .
C48 C 0.3483(8) 1.0514(7) 0.2511(6) 0.055(3) Uani 1 1 d . . . . .
H48A H 0.314486 1.068195 0.287379 0.066 Uiso 1 1 calc R U . . .
H48B H 0.309019 1.065184 0.212651 0.066 Uiso 1 1 calc R U . . .
C49 C 0.3776(7) 0.9559(7) 0.2713(5) 0.046(2) Uani 1 1 d . . . . .
H49A H 0.325322 0.924545 0.277314 0.056 Uiso 1 1 calc R U . . .
H49B H 0.408580 0.940890 0.313788 0.056 Uiso 1 1 calc R U . . .
C50 C 0.4387(7) 0.9273(6) 0.2204(4) 0.039(2) Uani 1 1 d . . . . .
H50A H 0.405858 0.936398 0.179223 0.047 Uiso 1 1 calc R U . . .
H50B H 0.458970 0.865178 0.236618 0.047 Uiso 1 1 calc R U . . .
C51 C 0.7228(7) 0.6917(6) 0.0197(4) 0.038(2) Uani 1 1 d . . . . .
C52 C 0.7012(7) 0.6861(7) -0.0419(4) 0.046(2) Uani 1 1 d . . . . .
H52 H 0.718222 0.721632 -0.082695 0.055 Uiso 1 1 calc R U . . .
C53 C 0.6500(8) 0.6191(7) -0.0333(5) 0.051(3) Uani 1 1 d . . . . .
H53 H 0.624793 0.600477 -0.066574 0.062 Uiso 1 1 calc R U . . .
C54 C 0.6433(7) 0.5848(6) 0.0342(4) 0.040(2) Uani 1 1 d . . . . .
C55 C 0.5987(7) 0.5146(6) 0.0711(5) 0.040(2) Uani 1 1 d . . . . .
H55 H 0.567481 0.485294 0.047652 0.048 Uiso 1 1 calc R U . . .
C56 C 0.5479(6) 0.4182(6) 0.1647(4) 0.039(2) Uani 1 1 d . . . . .
H56 H 0.546573 0.381569 0.133603 0.047 Uiso 1 1 calc R U . . .
C57 C 0.5904(7) 0.3628(6) 0.2277(5) 0.045(2) Uani 1 1 d . . . . .
H57A H 0.593698 0.398554 0.258555 0.054 Uiso 1 1 calc R U . . .
H57B H 0.651187 0.340510 0.218300 0.054 Uiso 1 1 calc R U . . .
C58 C 0.5396(7) 0.2869(6) 0.2604(5) 0.046(2) Uani 1 1 d . . . . .
H58A H 0.540441 0.248071 0.231338 0.055 Uiso 1 1 calc R U . . .
H58B H 0.568536 0.253835 0.302064 0.055 Uiso 1 1 calc R U . . .
C59 C 0.4449(7) 0.3188(7) 0.2738(5) 0.044(2) Uani 1 1 d . . . . .
H59A H 0.411829 0.269015 0.291748 0.052 Uiso 1 1 calc R U . . .
H59B H 0.443814 0.351906 0.306886 0.052 Uiso 1 1 calc R U . . .
C60 C 0.4010(7) 0.3753(7) 0.2114(5) 0.045(2) Uani 1 1 d . . . . .
H60A H 0.340889 0.398169 0.221733 0.054 Uiso 1 1 calc R U . . .
H60B H 0.396041 0.340131 0.180311 0.054 Uiso 1 1 calc R U . . .
C61 C 0.4531(6) 0.4509(6) 0.1785(5) 0.038(2) Uani 1 1 d . . . . .
H61A H 0.424214 0.484324 0.136943 0.046 Uiso 1 1 calc R U . . .
H61B H 0.453072 0.489451 0.207641 0.046 Uiso 1 1 calc R U . . .
C62 C 0.8182(6) 0.7346(6) 0.1010(4) 0.0358(19) Uani 1 1 d . . . . .
C63 C 0.8680(6) 0.7900(6) 0.1249(5) 0.040(2) Uani 1 1 d . . . . .
H63 H 0.897274 0.838624 0.096692 0.048 Uiso 1 1 calc R U . . .
C64 C 0.8910(6) 0.7470(6) 0.1892(5) 0.037(2) Uani 1 1 d . . . . .
H64 H 0.939096 0.759609 0.214513 0.045 Uiso 1 1 calc R U . . .
C65 C 0.8536(6) 0.6685(6) 0.2033(4) 0.0354(19) Uani 1 1 d . . . . .
C66 C 0.8624(6) 0.5954(6) 0.2584(5) 0.040(2) Uani 1 1 d . . . . .
H66 H 0.900880 0.594183 0.292869 0.048 Uiso 1 1 calc R U . . .
C67 C 0.8459(8) 0.4541(7) 0.3160(5) 0.053(3) Uani 1 1 d . . . . .
H67 H 0.852528 0.471242 0.357351 0.064 Uiso 1 1 calc R U . . .
C68 C 0.9360(9) 0.4072(8) 0.2986(6) 0.064(3) Uani 1 1 d . . . . .
H68A H 0.930396 0.391813 0.256828 0.077 Uiso 1 1 calc R U . . .
H68B H 0.982015 0.446223 0.292857 0.077 Uiso 1 1 calc R U . . .
C69 C 0.9630(11) 0.3244(10) 0.3543(8) 0.084(4) Uani 1 1 d . . . . .
H69A H 1.017209 0.293008 0.341211 0.101 Uiso 1 1 calc R U . . .
H69B H 0.976215 0.340795 0.394439 0.101 Uiso 1 1 calc R U . . .
C70 C 0.8920(10) 0.2663(9) 0.3691(8) 0.082(4) Uani 1 1 d . . . . .
H70A H 0.908952 0.218809 0.408487 0.099 Uiso 1 1 calc R U . . .
H70B H 0.887646 0.240722 0.332037 0.099 Uiso 1 1 calc R U . . .
C71 C 0.8027(10) 0.3111(8) 0.3809(7) 0.070(4) Uani 1 1 d . . . . .
H71A H 0.803266 0.326143 0.423182 0.083 Uiso 1 1 calc R U . . .
H71B H 0.757865 0.271486 0.383783 0.083 Uiso 1 1 calc R U . . .
C72 C 0.7779(8) 0.3928(7) 0.3261(6) 0.058(3) Uani 1 1 d . . . . .
H72A H 0.770476 0.376945 0.284738 0.070 Uiso 1 1 calc R U . . .
H72B H 0.720843 0.421884 0.336859 0.070 Uiso 1 1 calc R U . . .
C73 C 0.7043(9) 0.7357(9) 0.5273(5) 0.063(3) Uani 1 1 d . . . . .
H73A H 0.734989 0.682381 0.518777 0.075 Uiso 1 1 calc R U . . .
H73B H 0.640437 0.731191 0.530692 0.075 Uiso 1 1 calc R U . . .
C74 C 0.7376(12) 0.7486(11) 0.5894(6) 0.083(5) Uani 1 1 d . . . . .
H74A H 0.704362 0.719622 0.628225 0.100 Uiso 1 1 calc R U . . .
H74B H 0.801059 0.728004 0.595877 0.100 Uiso 1 1 calc R U . . .
C75 C 0.7211(18) 0.8407(12) 0.5763(7) 0.128(9) Uani 1 1 d . . . . .
H75A H 0.757405 0.861718 0.604954 0.153 Uiso 1 1 calc R U . . .
H75B H 0.658324 0.858814 0.583734 0.153 Uiso 1 1 calc R U . . .
C76 C 0.7460(11) 0.8759(9) 0.5038(6) 0.074(4) Uani 1 1 d . . . . .
H76A H 0.712171 0.932496 0.484322 0.089 Uiso 1 1 calc R U . . .
H76B H 0.809630 0.881386 0.498801 0.089 Uiso 1 1 calc R U . . .
C81 C 0.4426(6) 0.6958(5) 0.1330(4) 0.0326(18) Uani 1 1 d . . . . .
H81 H 0.492546 0.651313 0.129577 0.039 Uiso 1 1 calc R U . . .
C82 C 0.4677(6) 0.7842(6) 0.0938(4) 0.0369(19) Uani 1 1 d . . . . .
H82A H 0.417297 0.828808 0.093106 0.044 Uiso 1 1 calc R U . . .
H82B H 0.517612 0.798758 0.115409 0.044 Uiso 1 1 calc R U . . .
C3 C 0.8818(8) 0.4856(8) 0.1171(7) 0.064(3) Uani 1 1 d . . . . .
H3AA H 0.869106 0.539408 0.081823 0.076 Uiso 0.59(4) 1 calc R U P A 1
H3AB H 0.917107 0.498156 0.150832 0.076 Uiso 0.59(4) 1 calc R U P A 1
H3BC H 0.932636 0.456728 0.145406 0.076 Uiso 0.41(4) 1 calc R U P A 2
H3BD H 0.881410 0.548673 0.107038 0.076 Uiso 0.41(4) 1 calc R U P A 2
C10 C 0.801(3) 0.372(3) 0.142(2) 0.049(9) Uani 0.41(4) 1 d . . P A 2
H10A H 0.836248 0.331134 0.177937 0.058 Uiso 0.41(4) 1 calc R U P A 2
H10B H 0.740736 0.356164 0.143468 0.058 Uiso 0.41(4) 1 calc R U P A 2
C77 C 0.782(2) 0.394(3) 0.112(2) 0.072(11) Uani 0.59(4) 1 d . . P A 1
H77A H 0.748517 0.421843 0.070986 0.087 Uiso 0.59(4) 1 calc R U P A 1
H77B H 0.747167 0.351039 0.140531 0.087 Uiso 0.59(4) 1 calc R U P A 1
C79 C 0.872(2) 0.352(2) 0.097(2) 0.069(9) Uani 0.59(4) 1 d . . P A 1
H79A H 0.871953 0.334770 0.055263 0.082 Uiso 0.59(4) 1 calc R U P A 1
H79B H 0.892457 0.300402 0.132758 0.082 Uiso 0.59(4) 1 calc R U P A 1
C78 C 0.930(2) 0.4251(17) 0.0914(17) 0.071(10) Uani 0.59(4) 1 d . . P A 1
H78A H 0.985581 0.402787 0.116386 0.085 Uiso 0.59(4) 1 calc R U P A 1
H78B H 0.945473 0.450653 0.045046 0.085 Uiso 0.59(4) 1 calc R U P A 1
C80 C 0.881(2) 0.455(2) 0.0546(17) 0.054(10) Uani 0.41(4) 1 d . . P A 2
H80A H 0.845441 0.496588 0.019570 0.064 Uiso 0.41(4) 1 calc R U P A 2
H80B H 0.941576 0.443214 0.037977 0.064 Uiso 0.41(4) 1 calc R U P A 2
C79A C 0.841(3) 0.377(3) 0.080(4) 0.09(2) Uani 0.41(4) 1 d . . P A 2
H79C H 0.796384 0.373645 0.048926 0.106 Uiso 0.41(4) 1 calc R U P A 2
H79D H 0.886690 0.327106 0.084212 0.106 Uiso 0.41(4) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.043(5) . ?
U1 O2 2.249(5) . ?
U1 O3 2.176(4) . ?
U1 N7 2.493(8) . ?
U1 N8 2.593(8) . ?
U1 C63 3.004(9) . ?
U1 C64 3.014(9) . ?
U1 C65 3.069(10) . ?
U2 O2 2.174(5) . ?
U2 O3 2.246(5) . ?
U2 O4 2.044(5) . ?
U2 N1 2.477(8) . ?
U2 N2 2.585(7) . ?
U2 C26 3.050(10) . ?
U2 C27 2.950(8) . ?
U2 C28 2.971(9) . ?
U2 C29 3.013(8) . ?
Y1 O1 2.218(6) . ?
Y1 O2 2.205(5) . ?
Y1 O5 2.524(7) . ?
Y1 N3 2.381(8) . ?
Y1 N4 2.463(8) . ?
Y1 N5 2.437(7) . ?
Y1 N6 2.524(10) . ?
Y2 O3 2.202(5) . ?
Y2 O4 2.213(5) . ?
Y2 O6 2.533(7) . ?
Y2 N9 2.443(7) . ?
Y2 N10 2.521(8) . ?
Y2 N11 2.385(7) . ?
Y2 N12 2.478(7) . ?
O5 C73 1.475(14) . ?
O5 C76 1.444(12) . ?
O6 C3 1.431(13) . ?
O6 C10 1.43(5) . ?
O6 C77 1.49(3) . ?
N1 C4 1.365(10) . ?
N1 C7 1.365(12) . ?
N2 C8 1.291(12) . ?
N2 C81 1.493(10) . ?
N3 C15 1.377(11) . ?
N3 C18 1.378(12) . ?
N4 C19 1.326(14) . ?
N4 C20 1.468(12) . ?
N5 C26 1.350(11) . ?
N5 C29 1.373(13) . ?
N6 C30 1.304(12) . ?
N6 C31 1.494(14) . ?
N7 C40 1.349(11) . ?
N7 C43 1.357(12) . ?
N8 C44 1.301(12) . ?
N8 C45 1.494(11) . ?
N9 C62 1.338(11) . ?
N9 C65 1.392(11) . ?
N10 C66 1.284(11) . ?
N10 C67 1.468(14) . ?
N11 C51 1.364(11) . ?
N11 C54 1.395(10) . ?
N12 C55 1.289(12) . ?
N12 C56 1.465(11) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.515(14) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C9 1.545(11) . ?
C9 C4 1.539(13) . ?
C9 C15 1.531(12) . ?
C9 C26 1.506(13) . ?
C4 C5 1.373(14) . ?
C5 H5 0.9500 . ?
C5 C6 1.400(13) . ?
C6 H6 0.9500 . ?
C6 C7 1.401(13) . ?
C7 C8 1.427(12) . ?
C8 H8 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.547(15) . ?
C11 C82 1.517(13) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.515(16) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.542(12) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C81 1.528(12) . ?
C15 C16 1.397(14) . ?
C16 H16 0.9500 . ?
C16 C17 1.396(14) . ?
C17 H17 0.9500 . ?
C17 C18 1.390(14) . ?
C18 C19 1.425(13) . ?
C19 H19 0.9500 . ?
C20 H20 1.0000 . ?
C20 C21 1.496(19) . ?
C20 C25 1.538(19) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.536(15) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.53(2) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.50(2) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.497(18) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.439(12) . ?
C27 H27 1.0000 . ?
C27 C28 1.392(14) . ?
C28 H28 1.0000 . ?
C28 C29 1.418(12) . ?
C29 C30 1.423(14) . ?
C30 H30 0.9500 . ?
C31 H31 1.0000 . ?
C31 C32 1.560(18) . ?
C31 C36 1.495(18) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.522(18) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.54(2) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.46(2) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.516(19) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C37 C38 1.511(15) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.554(12) . ?
C39 C40 1.505(14) . ?
C39 C51 1.536(11) . ?
C39 C62 1.529(13) . ?
C40 C41 1.413(14) . ?
C41 H41 0.9500 . ?
C41 C42 1.384(14) . ?
C42 H42 0.9500 . ?
C42 C43 1.399(13) . ?
C43 C44 1.432(13) . ?
C44 H44 0.9500 . ?
C45 H45 1.0000 . ?
C45 C46 1.526(13) . ?
C45 C50 1.533(12) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C47 1.535(13) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.532(15) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.511(15) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.529(12) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.388(12) . ?
C52 H52 0.9500 . ?
C52 C53 1.390(13) . ?
C53 H53 0.9500 . ?
C53 C54 1.393(13) . ?
C54 C55 1.436(12) . ?
C55 H55 0.9500 . ?
C56 H56 1.0000 . ?
C56 C57 1.514(14) . ?
C56 C61 1.530(13) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57 C58 1.534(13) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C58 C59 1.524(15) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 C60 1.518(15) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C60 C61 1.543(12) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 C63 1.449(11) . ?
C63 H63 1.0000 . ?
C63 C64 1.389(14) . ?
C64 H64 1.0000 . ?
C64 C65 1.419(12) . ?
C65 C66 1.422(14) . ?
C66 H66 0.9500 . ?
C67 H67 1.0000 . ?
C67 C68 1.573(18) . ?
C67 C72 1.502(14) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C68 C69 1.558(19) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C69 C70 1.50(2) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C70 C71 1.51(2) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C71 C72 1.529(17) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C73 C74 1.502(16) . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C74 C75 1.44(2) . ?
C75 H75A 0.9900 . ?
C75 H75B 0.9900 . ?
C75 C76 1.54(2) . ?
C76 H76A 0.9900 . ?
C76 H76B 0.9900 . ?
C81 H81 1.0000 . ?
C81 C82 1.543(11) . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C3 H3AA 0.9900 . ?
C3 H3AB 0.9900 . ?
C3 H3BC 0.9900 . ?
C3 H3BD 0.9900 . ?
C3 C78 1.37(2) . ?
C3 C80 1.53(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C79A 1.42(8) . ?
C77 H77A 0.9900 . ?
C77 H77B 0.9900 . ?
C77 C79 1.53(5) . ?
C79 H79A 0.9900 . ?
C79 H79B 0.9900 . ?
C79 C78 1.56(4) . ?
C78 H78A 0.9900 . ?
C78 H78B 0.9900 . ?
C80 H80A 0.9900 . ?
C80 H80B 0.9900 . ?
C80 C79A 1.44(6) . ?
C79A H79C 0.9900 . ?
C79A H79D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 75.4(2) . . ?
O1 U1 O3 136.3(2) . . ?
O1 U1 N7 133.2(2) . . ?
O1 U1 N8 94.1(3) . . ?
O1 U1 C63 94.7(2) . . ?
O1 U1 C64 78.1(2) . . ?
O1 U1 C65 93.1(3) . . ?
O2 U1 N7 135.2(2) . . ?
O2 U1 N8 81.9(2) . . ?
O2 U1 C63 154.5(3) . . ?
O2 U1 C64 128.3(2) . . ?
O2 U1 C65 112.8(2) . . ?
O3 U1 O2 71.45(17) . . ?
O3 U1 N7 90.5(2) . . ?
O3 U1 N8 108.3(2) . . ?
O3 U1 C63 103.2(2) . . ?
O3 U1 C64 101.1(2) . . ?
O3 U1 C65 74.8(2) . . ?
N7 U1 N8 65.0(2) . . ?
N7 U1 C63 68.1(3) . . ?
N7 U1 C64 94.7(3) . . ?
N7 U1 C65 100.6(2) . . ?
N8 U1 C63 122.7(2) . . ?
N8 U1 C64 143.8(2) . . ?
N8 U1 C65 164.9(2) . . ?
C63 U1 C64 26.7(3) . . ?
C63 U1 C65 43.4(2) . . ?
C64 U1 C65 27.0(2) . . ?
O2 U2 O3 71.54(17) . . ?
O2 U2 N1 90.5(2) . . ?
O2 U2 N2 106.5(2) . . ?
O2 U2 C26 78.80(19) . . ?
O2 U2 C27 104.7(2) . . ?
O2 U2 C28 102.6(2) . . ?
O2 U2 C29 75.9(2) . . ?
O3 U2 N1 136.1(2) . . ?
O3 U2 N2 82.1(2) . . ?
O3 U2 C26 145.66(19) . . ?
O3 U2 C27 153.6(2) . . ?
O3 U2 C28 126.7(2) . . ?
O3 U2 C29 111.3(2) . . ?
O4 U2 O2 137.7(2) . . ?
O4 U2 O3 75.68(19) . . ?
O4 U2 N1 131.8(2) . . ?
O4 U2 N2 94.5(2) . . ?
O4 U2 C26 119.2(2) . . ?
O4 U2 C27 93.0(2) . . ?
O4 U2 C28 76.5(2) . . ?
O4 U2 C29 92.3(2) . . ?
N1 U2 N2 64.7(2) . . ?
N1 U2 C26 59.1(2) . . ?
N1 U2 C27 68.7(3) . . ?
N1 U2 C28 95.8(3) . . ?
N1 U2 C29 101.9(3) . . ?
N2 U2 C26 123.6(2) . . ?
N2 U2 C27 123.1(2) . . ?
N2 U2 C28 144.7(2) . . ?
N2 U2 C29 166.2(2) . . ?
C27 U2 C26 27.7(2) . . ?
C27 U2 C28 27.2(3) . . ?
C27 U2 C29 44.4(3) . . ?
C28 U2 C26 44.4(3) . . ?
C28 U2 C29 27.4(2) . . ?
C29 U2 C26 42.8(3) . . ?
O1 Y1 O5 128.1(2) . . ?
O1 Y1 N3 140.0(3) . . ?
O1 Y1 N4 86.3(2) . . ?
O1 Y1 N5 132.7(2) . . ?
O1 Y1 N6 85.7(3) . . ?
O2 Y1 O1 72.92(19) . . ?
O2 Y1 O5 155.9(2) . . ?
O2 Y1 N3 89.1(2) . . ?
O2 Y1 N4 118.1(3) . . ?
O2 Y1 N5 73.4(2) . . ?
O2 Y1 N6 99.5(2) . . ?
N3 Y1 O5 80.1(3) . . ?
N3 Y1 N4 70.8(3) . . ?
N3 Y1 N5 70.6(3) . . ?
N3 Y1 N6 133.2(3) . . ?
N4 Y1 O5 78.6(3) . . ?
N4 Y1 N6 137.1(3) . . ?
N5 Y1 O5 82.7(2) . . ?
N5 Y1 N4 139.3(3) . . ?
N5 Y1 N6 68.2(3) . . ?
N6 Y1 O5 73.7(3) . . ?
O3 Y2 O4 73.33(18) . . ?
O3 Y2 O6 157.90(19) . . ?
O3 Y2 N9 72.8(2) . . ?
O3 Y2 N10 100.0(2) . . ?
O3 Y2 N11 88.9(2) . . ?
O3 Y2 N12 118.7(2) . . ?
O4 Y2 O6 126.8(2) . . ?
O4 Y2 N9 133.6(2) . . ?
O4 Y2 N10 88.1(2) . . ?
O4 Y2 N11 139.4(3) . . ?
O4 Y2 N12 85.5(2) . . ?
N9 Y2 O6 85.4(2) . . ?
N9 Y2 N10 67.7(2) . . ?
N9 Y2 N12 139.2(2) . . ?
N10 Y2 O6 74.2(2) . . ?
N11 Y2 O6 80.0(2) . . ?
N11 Y2 N9 69.9(2) . . ?
N11 Y2 N10 131.5(3) . . ?
N11 Y2 N12 71.4(2) . . ?
N12 Y2 O6 75.8(2) . . ?
N12 Y2 N10 136.7(2) . . ?
U1 O1 Y1 108.9(2) . . ?
U2 O2 U1 108.3(2) . . ?
U2 O2 Y1 131.0(3) . . ?
Y1 O2 U1 102.3(2) . . ?
U1 O3 U2 108.33(19) . . ?
U1 O3 Y2 133.1(3) . . ?
Y2 O3 U2 102.06(18) . . ?
U2 O4 Y2 108.6(2) . . ?
C73 O5 Y1 117.4(5) . . ?
C76 O5 Y1 132.6(8) . . ?
C76 O5 C73 108.2(8) . . ?
C3 O6 Y2 117.7(6) . . ?
C3 O6 C77 103.6(15) . . ?
C10 O6 Y2 136.3(19) . . ?
C10 O6 C3 105.9(19) . . ?
C77 O6 Y2 128.6(14) . . ?
C4 N1 U2 134.6(6) . . ?
C4 N1 C7 105.3(8) . . ?
C7 N1 U2 120.1(5) . . ?
C8 N2 U2 117.0(5) . . ?
C8 N2 C81 118.2(8) . . ?
C81 N2 U2 124.7(5) . . ?
C15 N3 Y1 139.1(7) . . ?
C15 N3 C18 105.3(8) . . ?
C18 N3 Y1 114.3(6) . . ?
C19 N4 Y1 112.7(6) . . ?
C19 N4 C20 117.6(8) . . ?
C20 N4 Y1 129.6(7) . . ?
C26 N5 Y1 135.4(7) . . ?
C26 N5 C29 108.7(7) . . ?
C29 N5 Y1 110.2(5) . . ?
C30 N6 Y1 111.9(7) . . ?
C30 N6 C31 115.1(10) . . ?
C31 N6 Y1 132.9(7) . . ?
C40 N7 U1 134.0(7) . . ?
C40 N7 C43 106.9(8) . . ?
C43 N7 U1 118.5(6) . . ?
C44 N8 U1 116.6(6) . . ?
C44 N8 C45 117.7(8) . . ?
C45 N8 U1 125.7(6) . . ?
C62 N9 Y2 136.6(6) . . ?
C62 N9 C65 107.4(7) . . ?
C65 N9 Y2 110.7(5) . . ?
C66 N10 Y2 111.7(6) . . ?
C66 N10 C67 116.1(8) . . ?
C67 N10 Y2 131.8(6) . . ?
C51 N11 Y2 140.7(6) . . ?
C51 N11 C54 105.5(7) . . ?
C54 N11 Y2 113.4(6) . . ?
C55 N12 Y2 111.8(5) . . ?
C55 N12 C56 117.1(7) . . ?
C56 N12 Y2 131.0(5) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C1 C2 H2A 108.6 . . ?
C1 C2 H2B 108.6 . . ?
C1 C2 C9 114.7(8) . . ?
H2A C2 H2B 107.6 . . ?
C9 C2 H2A 108.6 . . ?
C9 C2 H2B 108.6 . . ?
C4 C9 C2 107.4(7) . . ?
C15 C9 C2 108.8(7) . . ?
C15 C9 C4 107.7(8) . . ?
C26 C9 C2 107.9(8) . . ?
C26 C9 C4 110.4(7) . . ?
C26 C9 C15 114.5(7) . . ?
N1 C4 C9 118.8(8) . . ?
N1 C4 C5 111.6(8) . . ?
C5 C4 C9 129.6(8) . . ?
C4 C5 H5 126.6 . . ?
C4 C5 C6 106.7(8) . . ?
C6 C5 H5 126.6 . . ?
C5 C6 H6 127.2 . . ?
C5 C6 C7 105.6(9) . . ?
C7 C6 H6 127.2 . . ?
N1 C7 C6 110.9(8) . . ?
N1 C7 C8 117.0(8) . . ?
C6 C7 C8 132.0(9) . . ?
N2 C8 C7 120.9(8) . . ?
N2 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
H11A C11 H11B 108.2 . . ?
C12 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
C82 C11 H11A 109.8 . . ?
C82 C11 H11B 109.8 . . ?
C82 C11 C12 109.5(8) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C13 C12 C11 110.9(9) . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 C14 110.8(9) . . ?
H13A C13 H13B 108.1 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
C13 C14 H14A 109.9 . . ?
C13 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
C81 C14 C13 109.1(8) . . ?
C81 C14 H14A 109.9 . . ?
C81 C14 H14B 109.9 . . ?
N3 C15 C9 124.1(8) . . ?
N3 C15 C16 110.0(8) . . ?
C16 C15 C9 125.8(8) . . ?
C15 C16 H16 126.3 . . ?
C17 C16 C15 107.5(9) . . ?
C17 C16 H16 126.3 . . ?
C16 C17 H17 127.2 . . ?
C18 C17 C16 105.6(9) . . ?
C18 C17 H17 127.2 . . ?
N3 C18 C17 111.5(8) . . ?
N3 C18 C19 119.9(9) . . ?
C17 C18 C19 128.6(9) . . ?
N4 C19 C18 121.6(9) . . ?
N4 C19 H19 119.2 . . ?
C18 C19 H19 119.2 . . ?
N4 C20 H20 108.8 . . ?
N4 C20 C21 109.6(9) . . ?
N4 C20 C25 110.3(10) . . ?
C21 C20 H20 108.8 . . ?
C21 C20 C25 110.6(10) . . ?
C25 C20 H20 108.8 . . ?
C20 C21 H21A 109.3 . . ?
C20 C21 H21B 109.3 . . ?
C20 C21 C22 111.7(12) . . ?
H21A C21 H21B 107.9 . . ?
C22 C21 H21A 109.3 . . ?
C22 C21 H21B 109.3 . . ?
C21 C22 H22A 109.9 . . ?
C21 C22 H22B 109.9 . . ?
H22A C22 H22B 108.3 . . ?
C23 C22 C21 108.8(12) . . ?
C23 C22 H22A 109.9 . . ?
C23 C22 H22B 109.9 . . ?
C22 C23 H23A 108.6 . . ?
C22 C23 H23B 108.6 . . ?
H23A C23 H23B 107.5 . . ?
C24 C23 C22 114.8(15) . . ?
C24 C23 H23A 108.6 . . ?
C24 C23 H23B 108.6 . . ?
C23 C24 H24A 109.7 . . ?
C23 C24 H24B 109.7 . . ?
H24A C24 H24B 108.2 . . ?
C25 C24 C23 110.0(13) . . ?
C25 C24 H24A 109.7 . . ?
C25 C24 H24B 109.7 . . ?
C20 C25 H25A 109.3 . . ?
C20 C25 H25B 109.3 . . ?
C24 C25 C20 111.6(13) . . ?
C24 C25 H25A 109.3 . . ?
C24 C25 H25B 109.3 . . ?
H25A C25 H25B 108.0 . . ?
N5 C26 U2 77.4(5) . . ?
N5 C26 C9 126.6(8) . . ?
N5 C26 C27 108.6(8) . . ?
C9 C26 U2 111.7(6) . . ?
C27 C26 U2 72.3(5) . . ?
C27 C26 C9 124.5(8) . . ?
U2 C27 H27 125.0 . . ?
C26 C27 U2 80.0(5) . . ?
C26 C27 H27 125.0 . . ?
C28 C27 U2 77.3(5) . . ?
C28 C27 C26 106.8(8) . . ?
C28 C27 H27 125.0 . . ?
U2 C28 H28 125.6 . . ?
C27 C28 U2 75.6(5) . . ?
C27 C28 H28 125.6 . . ?
C27 C28 C29 106.5(9) . . ?
C29 C28 U2 77.9(5) . . ?
C29 C28 H28 125.6 . . ?
N5 C29 U2 78.5(5) . . ?
N5 C29 C28 109.2(9) . . ?
N5 C29 C30 120.6(8) . . ?
C28 C29 U2 74.7(5) . . ?
C28 C29 C30 129.8(10) . . ?
C30 C29 U2 119.5(6) . . ?
N6 C30 C29 119.9(9) . . ?
N6 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
N6 C31 H31 108.1 . . ?
N6 C31 C32 111.9(9) . . ?
N6 C31 C36 110.4(12) . . ?
C32 C31 H31 108.1 . . ?
C36 C31 H31 108.1 . . ?
C36 C31 C32 110.1(9) . . ?
C31 C32 H32A 109.9 . . ?
C31 C32 H32B 109.9 . . ?
H32A C32 H32B 108.3 . . ?
C33 C32 C31 109.0(12) . . ?
C33 C32 H32A 109.9 . . ?
C33 C32 H32B 109.9 . . ?
C32 C33 H33A 109.6 . . ?
C32 C33 H33B 109.6 . . ?
C32 C33 C34 110.3(13) . . ?
H33A C33 H33B 108.1 . . ?
C34 C33 H33A 109.6 . . ?
C34 C33 H33B 109.6 . . ?
C33 C34 H34A 109.2 . . ?
C33 C34 H34B 109.2 . . ?
H34A C34 H34B 107.9 . . ?
C35 C34 C33 112.0(12) . . ?
C35 C34 H34A 109.2 . . ?
C35 C34 H34B 109.2 . . ?
C34 C35 H35A 109.0 . . ?
C34 C35 H35B 109.0 . . ?
C34 C35 C36 113.0(11) . . ?
H35A C35 H35B 107.8 . . ?
C36 C35 H35A 109.0 . . ?
C36 C35 H35B 109.0 . . ?
C31 C36 C35 110.9(14) . . ?
C31 C36 H36A 109.5 . . ?
C31 C36 H36B 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 108.1 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
C37 C38 H38A 108.6 . . ?
C37 C38 H38B 108.6 . . ?
C37 C38 C39 114.7(9) . . ?
H38A C38 H38B 107.6 . . ?
C39 C38 H38A 108.6 . . ?
C39 C38 H38B 108.6 . . ?
C40 C39 C38 108.3(8) . . ?
C40 C39 C51 109.8(8) . . ?
C40 C39 C62 109.6(7) . . ?
C51 C39 C38 108.2(7) . . ?
C62 C39 C38 105.9(8) . . ?
C62 C39 C51 114.7(8) . . ?
N7 C40 C39 120.4(8) . . ?
N7 C40 C41 109.9(9) . . ?
C41 C40 C39 129.7(8) . . ?
C40 C41 H41 126.7 . . ?
C42 C41 C40 106.6(8) . . ?
C42 C41 H41 126.7 . . ?
C41 C42 H42 127.0 . . ?
C41 C42 C43 106.1(9) . . ?
C43 C42 H42 127.0 . . ?
N7 C43 C42 110.6(9) . . ?
N7 C43 C44 118.7(8) . . ?
C42 C43 C44 130.6(10) . . ?
N8 C44 C43 119.9(9) . . ?
N8 C44 H44 120.0 . . ?
C43 C44 H44 120.0 . . ?
N8 C45 H45 107.8 . . ?
N8 C45 C46 116.1(7) . . ?
N8 C45 C50 109.1(7) . . ?
C46 C45 H45 107.8 . . ?
C46 C45 C50 108.2(8) . . ?
C50 C45 H45 107.8 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 C47 110.6(9) . . ?
H46A C46 H46B 108.1 . . ?
C47 C46 H46A 109.5 . . ?
C47 C46 H46B 109.5 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 108.1 . . ?
C48 C47 C46 110.7(8) . . ?
C48 C47 H47A 109.5 . . ?
C48 C47 H47B 109.5 . . ?
C47 C48 H48A 109.3 . . ?
C47 C48 H48B 109.3 . . ?
H48A C48 H48B 108.0 . . ?
C49 C48 C47 111.4(9) . . ?
C49 C48 H48A 109.3 . . ?
C49 C48 H48B 109.3 . . ?
C48 C49 H49A 109.2 . . ?
C48 C49 H49B 109.2 . . ?
C48 C49 C50 112.0(8) . . ?
H49A C49 H49B 107.9 . . ?
C50 C49 H49A 109.2 . . ?
C50 C49 H49B 109.2 . . ?
C45 C50 H50A 109.4 . . ?
C45 C50 H50B 109.4 . . ?
C49 C50 C45 111.3(7) . . ?
C49 C50 H50A 109.4 . . ?
C49 C50 H50B 109.4 . . ?
H50A C50 H50B 108.0 . . ?
N11 C51 C39 123.9(7) . . ?
N11 C51 C52 110.5(8) . . ?
C52 C51 C39 125.5(8) . . ?
C51 C52 H52 126.2 . . ?
C51 C52 C53 107.6(8) . . ?
C53 C52 H52 126.2 . . ?
C52 C53 H53 127.0 . . ?
C52 C53 C54 106.1(8) . . ?
C54 C53 H53 127.0 . . ?
N11 C54 C55 119.4(8) . . ?
C53 C54 N11 110.3(8) . . ?
C53 C54 C55 130.4(8) . . ?
N12 C55 C54 123.6(8) . . ?
N12 C55 H55 118.2 . . ?
C54 C55 H55 118.2 . . ?
N12 C56 H56 108.2 . . ?
N12 C56 C57 111.1(7) . . ?
N12 C56 C61 111.6(8) . . ?
C57 C56 H56 108.2 . . ?
C57 C56 C61 109.4(8) . . ?
C61 C56 H56 108.2 . . ?
C56 C57 H57A 109.1 . . ?
C56 C57 H57B 109.1 . . ?
C56 C57 C58 112.5(8) . . ?
H57A C57 H57B 107.8 . . ?
C58 C57 H57A 109.1 . . ?
C58 C57 H57B 109.1 . . ?
C57 C58 H58A 109.6 . . ?
C57 C58 H58B 109.6 . . ?
H58A C58 H58B 108.1 . . ?
C59 C58 C57 110.5(8) . . ?
C59 C58 H58A 109.6 . . ?
C59 C58 H58B 109.6 . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 108.1 . . ?
C60 C59 C58 110.6(8) . . ?
C60 C59 H59A 109.5 . . ?
C60 C59 H59B 109.5 . . ?
C59 C60 H60A 109.2 . . ?
C59 C60 H60B 109.2 . . ?
C59 C60 C61 111.9(8) . . ?
H60A C60 H60B 107.9 . . ?
C61 C60 H60A 109.2 . . ?
C61 C60 H60B 109.2 . . ?
C56 C61 C60 110.8(8) . . ?
C56 C61 H61A 109.5 . . ?
C56 C61 H61B 109.5 . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
H61A C61 H61B 108.1 . . ?
N9 C62 C39 125.8(7) . . ?
N9 C62 C63 109.8(8) . . ?
C63 C62 C39 123.9(8) . . ?
U1 C63 H63 125.2 . . ?
C62 C63 U1 79.6(5) . . ?
C62 C63 H63 125.2 . . ?
C64 C63 U1 77.1(5) . . ?
C64 C63 C62 106.6(8) . . ?
C64 C63 H63 125.2 . . ?
U1 C64 H64 125.6 . . ?
C63 C64 U1 76.2(5) . . ?
C63 C64 H64 125.6 . . ?
C63 C64 C65 106.2(8) . . ?
C65 C64 U1 78.7(5) . . ?
C65 C64 H64 125.6 . . ?
N9 C65 U1 78.0(5) . . ?
N9 C65 C64 109.9(8) . . ?
N9 C65 C66 118.3(7) . . ?
C64 C65 U1 74.4(5) . . ?
C64 C65 C66 131.5(9) . . ?
C66 C65 U1 119.1(6) . . ?
N10 C66 C65 121.8(9) . . ?
N10 C66 H66 119.1 . . ?
C65 C66 H66 119.1 . . ?
N10 C67 H67 109.3 . . ?
N10 C67 C68 109.9(9) . . ?
N10 C67 C72 110.5(10) . . ?
C68 C67 H67 109.3 . . ?
C72 C67 H67 109.3 . . ?
C72 C67 C68 108.6(10) . . ?
C67 C68 H68A 109.7 . . ?
C67 C68 H68B 109.7 . . ?
H68A C68 H68B 108.2 . . ?
C69 C68 C67 110.0(11) . . ?
C69 C68 H68A 109.7 . . ?
C69 C68 H68B 109.7 . . ?
C68 C69 H69A 109.2 . . ?
C68 C69 H69B 109.2 . . ?
H69A C69 H69B 107.9 . . ?
C70 C69 C68 111.9(12) . . ?
C70 C69 H69A 109.2 . . ?
C70 C69 H69B 109.2 . . ?
C69 C70 H70A 108.8 . . ?
C69 C70 H70B 108.8 . . ?
C69 C70 C71 113.7(13) . . ?
H70A C70 H70B 107.7 . . ?
C71 C70 H70A 108.8 . . ?
C71 C70 H70B 108.8 . . ?
C70 C71 H71A 109.3 . . ?
C70 C71 H71B 109.3 . . ?
C70 C71 C72 111.7(11) . . ?
H71A C71 H71B 107.9 . . ?
C72 C71 H71A 109.3 . . ?
C72 C71 H71B 109.3 . . ?
C67 C72 C71 112.4(11) . . ?
C67 C72 H72A 109.1 . . ?
C67 C72 H72B 109.1 . . ?
C71 C72 H72A 109.1 . . ?
C71 C72 H72B 109.1 . . ?
H72A C72 H72B 107.9 . . ?
O5 C73 H73A 110.4 . . ?
O5 C73 H73B 110.4 . . ?
O5 C73 C74 106.4(10) . . ?
H73A C73 H73B 108.6 . . ?
C74 C73 H73A 110.4 . . ?
C74 C73 H73B 110.4 . . ?
C73 C74 H74A 111.6 . . ?
C73 C74 H74B 111.6 . . ?
H74A C74 H74B 109.4 . . ?
C75 C74 C73 100.7(13) . . ?
C75 C74 H74A 111.6 . . ?
C75 C74 H74B 111.6 . . ?
C74 C75 H75A 110.6 . . ?
C74 C75 H75B 110.6 . . ?
C74 C75 C76 105.6(13) . . ?
H75A C75 H75B 108.8 . . ?
C76 C75 H75A 110.6 . . ?
C76 C75 H75B 110.6 . . ?
O5 C76 C75 102.7(11) . . ?
O5 C76 H76A 111.2 . . ?
O5 C76 H76B 111.2 . . ?
C75 C76 H76A 111.2 . . ?
C75 C76 H76B 111.2 . . ?
H76A C76 H76B 109.1 . . ?
N2 C81 C14 115.7(7) . . ?
N2 C81 H81 107.9 . . ?
N2 C81 C82 109.4(6) . . ?
C14 C81 H81 107.9 . . ?
C14 C81 C82 107.9(8) . . ?
C82 C81 H81 107.9 . . ?
C11 C82 C81 110.8(8) . . ?
C11 C82 H82A 109.5 . . ?
C11 C82 H82B 109.5 . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 108.1 . . ?
O6 C3 H3AA 108.9 . . ?
O6 C3 H3AB 108.9 . . ?
O6 C3 H3BC 111.8 . . ?
O6 C3 H3BD 111.8 . . ?
O6 C3 C80 99.7(13) . . ?
H3AA C3 H3AB 107.8 . . ?
H3BC C3 H3BD 109.6 . . ?
C78 C3 O6 113.2(12) . . ?
C78 C3 H3AA 108.9 . . ?
C78 C3 H3AB 108.9 . . ?
C80 C3 H3BC 111.8 . . ?
C80 C3 H3BD 111.8 . . ?
O6 C10 H10A 111.6 . . ?
O6 C10 H10B 111.6 . . ?
H10A C10 H10B 109.4 . . ?
C79A C10 O6 101(3) . . ?
C79A C10 H10A 111.6 . . ?
C79A C10 H10B 111.6 . . ?
O6 C77 H77A 110.8 . . ?
O6 C77 H77B 110.8 . . ?
O6 C77 C79 105(2) . . ?
H77A C77 H77B 108.8 . . ?
C79 C77 H77A 110.8 . . ?
C79 C77 H77B 110.8 . . ?
C77 C79 H79A 111.4 . . ?
C77 C79 H79B 111.4 . . ?
C77 C79 C78 102(2) . . ?
H79A C79 H79B 109.3 . . ?
C78 C79 H79A 111.4 . . ?
C78 C79 H79B 111.4 . . ?
C3 C78 C79 106.6(18) . . ?
C3 C78 H78A 110.4 . . ?
C3 C78 H78B 110.4 . . ?
C79 C78 H78A 110.4 . . ?
C79 C78 H78B 110.4 . . ?
H78A C78 H78B 108.6 . . ?
C3 C80 H80A 111.9 . . ?
C3 C80 H80B 111.9 . . ?
H80A C80 H80B 109.6 . . ?
C79A C80 C3 99(3) . . ?
C79A C80 H80A 111.9 . . ?
C79A C80 H80B 111.9 . . ?
C10 C79A C80 113(4) . . ?
C10 C79A H79C 109.0 . . ?
C10 C79A H79D 109.0 . . ?
C80 C79A H79C 109.0 . . ?
C80 C79A H79D 109.0 . . ?
H79C C79A H79D 107.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 N7 C40 C39 11.3(13) . . . . ?
U1 N7 C40 C41 -171.0(6) . . . . ?
U1 N7 C43 C42 172.2(6) . . . . ?
U1 N7 C43 C44 -10.3(11) . . . . ?
U1 N8 C44 C43 7.4(11) . . . . ?
U1 N8 C45 C46 153.5(7) . . . . ?
U1 N8 C45 C50 -84.0(8) . . . . ?
U1 C63 C64 C65 73.6(6) . . . . ?
U1 C64 C65 N9 70.6(6) . . . . ?
U1 C64 C65 C66 -115.3(10) . . . . ?
U1 C65 C66 N10 82.6(10) . . . . ?
U2 N1 C4 C9 3.2(12) . . . . ?
U2 N1 C4 C5 -178.0(6) . . . . ?
U2 N1 C7 C6 178.2(6) . . . . ?
U2 N1 C7 C8 -5.1(10) . . . . ?
U2 N2 C8 C7 2.7(10) . . . . ?
U2 N2 C81 C14 152.6(6) . . . . ?
U2 N2 C81 C82 -85.4(8) . . . . ?
U2 C26 C27 C28 73.3(6) . . . . ?
U2 C27 C28 C29 72.5(6) . . . . ?
U2 C28 C29 N5 71.7(6) . . . . ?
U2 C28 C29 C30 -115.8(9) . . . . ?
U2 C29 C30 N6 82.5(9) . . . . ?
Y1 O5 C73 C74 -179.6(9) . . . . ?
Y1 O5 C76 C75 152.4(11) . . . . ?
Y1 N3 C15 C9 -19.2(16) . . . . ?
Y1 N3 C15 C16 165.0(8) . . . . ?
Y1 N3 C18 C17 -170.4(8) . . . . ?
Y1 N3 C18 C19 9.0(13) . . . . ?
Y1 N4 C19 C18 -3.5(13) . . . . ?
Y1 N4 C20 C21 91.0(12) . . . . ?
Y1 N4 C20 C25 -31.0(14) . . . . ?
Y1 N5 C26 U2 80.1(6) . . . . ?
Y1 N5 C26 C9 -27.7(14) . . . . ?
Y1 N5 C26 C27 146.3(6) . . . . ?
Y1 N5 C29 U2 -87.1(3) . . . . ?
Y1 N5 C29 C28 -156.2(5) . . . . ?
Y1 N5 C29 C30 30.5(9) . . . . ?
Y1 N6 C30 C29 -13.9(10) . . . . ?
Y1 N6 C31 C32 119.3(10) . . . . ?
Y1 N6 C31 C36 -3.6(13) . . . . ?
Y2 O6 C3 C78 -173(2) . . . . ?
Y2 O6 C3 C80 -129.8(17) . . . . ?
Y2 O6 C10 C79A 138(3) . . . . ?
Y2 O6 C77 C79 175(2) . . . . ?
Y2 N9 C62 C39 -26.0(15) . . . . ?
Y2 N9 C62 C63 146.3(7) . . . . ?
Y2 N9 C65 U1 -87.1(4) . . . . ?
Y2 N9 C65 C64 -155.3(6) . . . . ?
Y2 N9 C65 C66 29.7(10) . . . . ?
Y2 N10 C66 C65 -16.3(11) . . . . ?
Y2 N10 C67 C68 113.2(9) . . . . ?
Y2 N10 C67 C72 -6.6(13) . . . . ?
Y2 N11 C51 C39 -11.5(17) . . . . ?
Y2 N11 C51 C52 170.9(8) . . . . ?
Y2 N11 C54 C53 -174.3(8) . . . . ?
Y2 N11 C54 C55 6.2(12) . . . . ?
Y2 N12 C55 C54 -4.2(13) . . . . ?
Y2 N12 C56 C57 -29.5(11) . . . . ?
Y2 N12 C56 C61 92.9(9) . . . . ?
O5 C73 C74 C75 33.1(18) . . . . ?
O6 C3 C78 C79 6(3) . . . . ?
O6 C3 C80 C79A -36(3) . . . . ?
O6 C10 C79A C80 13(6) . . . . ?
O6 C77 C79 C78 -28(4) . . . . ?
N1 C4 C5 C6 -0.8(11) . . . . ?
N1 C7 C8 N2 1.5(12) . . . . ?
N2 C81 C82 C11 171.3(8) . . . . ?
N3 C15 C16 C17 1.3(13) . . . . ?
N3 C18 C19 N4 -3.7(17) . . . . ?
N4 C20 C21 C22 -179.0(10) . . . . ?
N4 C20 C25 C24 178.9(11) . . . . ?
N5 C26 C27 U2 -69.5(7) . . . . ?
N5 C26 C27 C28 3.8(10) . . . . ?
N5 C29 C30 N6 -11.4(13) . . . . ?
N6 C31 C32 C33 177.8(10) . . . . ?
N6 C31 C36 C35 -178.7(10) . . . . ?
N7 C40 C41 C42 0.7(11) . . . . ?
N7 C43 C44 N8 1.7(13) . . . . ?
N8 C45 C46 C47 -176.9(8) . . . . ?
N8 C45 C50 C49 174.3(8) . . . . ?
N9 C62 C63 U1 -69.6(7) . . . . ?
N9 C62 C63 C64 3.4(11) . . . . ?
N9 C65 C66 N10 -9.1(14) . . . . ?
N10 C67 C68 C69 -178.8(10) . . . . ?
N10 C67 C72 C71 179.6(10) . . . . ?
N11 C51 C52 C53 0.8(13) . . . . ?
N11 C54 C55 N12 -1.2(16) . . . . ?
N12 C56 C57 C58 -179.0(8) . . . . ?
N12 C56 C61 C60 -179.4(7) . . . . ?
C1 C2 C9 C4 178.9(9) . . . . ?
C1 C2 C9 C15 -64.8(12) . . . . ?
C1 C2 C9 C26 59.9(11) . . . . ?
C2 C9 C4 N1 -138.6(8) . . . . ?
C2 C9 C4 C5 42.9(13) . . . . ?
C2 C9 C15 N3 148.9(10) . . . . ?
C2 C9 C15 C16 -35.9(14) . . . . ?
C2 C9 C26 U2 142.1(5) . . . . ?
C2 C9 C26 N5 -127.8(9) . . . . ?
C2 C9 C26 C27 59.1(11) . . . . ?
C9 C4 C5 C6 177.9(9) . . . . ?
C9 C15 C16 C17 -174.4(10) . . . . ?
C9 C26 C27 U2 104.6(9) . . . . ?
C9 C26 C27 C28 177.9(8) . . . . ?
C4 N1 C7 C6 -1.1(10) . . . . ?
C4 N1 C7 C8 175.6(8) . . . . ?
C4 C9 C15 N3 -95.1(11) . . . . ?
C4 C9 C15 C16 80.2(12) . . . . ?
C4 C9 C26 U2 25.0(8) . . . . ?
C4 C9 C26 N5 115.1(10) . . . . ?
C4 C9 C26 C27 -58.0(11) . . . . ?
C4 C5 C6 C7 0.1(11) . . . . ?
C5 C6 C7 N1 0.7(11) . . . . ?
C5 C6 C7 C8 -175.4(9) . . . . ?
C6 C7 C8 N2 177.3(9) . . . . ?
C7 N1 C4 C9 -177.6(7) . . . . ?
C7 N1 C4 C5 1.2(10) . . . . ?
C8 N2 C81 C14 -31.4(11) . . . . ?
C8 N2 C81 C82 90.6(9) . . . . ?
C11 C12 C13 C14 56.6(13) . . . . ?
C12 C11 C82 C81 58.8(12) . . . . ?
C12 C13 C14 C81 -59.9(12) . . . . ?
C13 C14 C81 N2 -176.0(8) . . . . ?
C13 C14 C81 C82 61.1(10) . . . . ?
C14 C81 C82 C11 -62.1(10) . . . . ?
C15 N3 C18 C17 -1.0(12) . . . . ?
C15 N3 C18 C19 178.5(10) . . . . ?
C15 C9 C4 N1 104.4(9) . . . . ?
C15 C9 C4 C5 -74.1(11) . . . . ?
C15 C9 C26 U2 -96.7(7) . . . . ?
C15 C9 C26 N5 -6.5(13) . . . . ?
C15 C9 C26 C27 -179.6(8) . . . . ?
C15 C16 C17 C18 -1.8(13) . . . . ?
C16 C17 C18 N3 1.8(13) . . . . ?
C16 C17 C18 C19 -177.6(11) . . . . ?
C17 C18 C19 N4 175.6(12) . . . . ?
C18 N3 C15 C9 175.6(9) . . . . ?
C18 N3 C15 C16 -0.2(12) . . . . ?
C19 N4 C20 C21 -92.0(12) . . . . ?
C19 N4 C20 C25 146.0(11) . . . . ?
C20 N4 C19 C18 179.0(10) . . . . ?
C20 C21 C22 C23 54.3(18) . . . . ?
C21 C20 C25 C24 57.5(14) . . . . ?
C21 C22 C23 C24 -53.6(19) . . . . ?
C22 C23 C24 C25 54.6(18) . . . . ?
C23 C24 C25 C20 -54.7(17) . . . . ?
C25 C20 C21 C22 -57.2(13) . . . . ?
C26 N5 C29 U2 70.6(6) . . . . ?
C26 N5 C29 C28 1.4(10) . . . . ?
C26 N5 C29 C30 -171.9(8) . . . . ?
C26 C9 C4 N1 -21.2(11) . . . . ?
C26 C9 C4 C5 160.3(9) . . . . ?
C26 C9 C15 N3 28.0(13) . . . . ?
C26 C9 C15 C16 -156.7(10) . . . . ?
C26 C27 C28 U2 -75.2(6) . . . . ?
C26 C27 C28 C29 -2.8(9) . . . . ?
C27 C28 C29 U2 -70.8(6) . . . . ?
C27 C28 C29 N5 0.9(9) . . . . ?
C27 C28 C29 C30 173.4(8) . . . . ?
C28 C29 C30 N6 176.8(8) . . . . ?
C29 N5 C26 U2 -69.4(5) . . . . ?
C29 N5 C26 C9 -177.2(9) . . . . ?
C29 N5 C26 C27 -3.2(10) . . . . ?
C30 N6 C31 C32 -66.1(11) . . . . ?
C30 N6 C31 C36 171.0(9) . . . . ?
C31 N6 C30 C29 170.4(8) . . . . ?
C31 C32 C33 C34 56.7(15) . . . . ?
C32 C31 C36 C35 57.3(15) . . . . ?
C32 C33 C34 C35 -55.1(18) . . . . ?
C33 C34 C35 C36 54(2) . . . . ?
C34 C35 C36 C31 -55.7(19) . . . . ?
C36 C31 C32 C33 -59.1(14) . . . . ?
C37 C38 C39 C40 177.5(9) . . . . ?
C37 C38 C39 C51 -63.6(12) . . . . ?
C37 C38 C39 C62 59.9(10) . . . . ?
C38 C39 C40 N7 -143.5(8) . . . . ?
C38 C39 C40 C41 39.3(13) . . . . ?
C38 C39 C51 N11 142.0(10) . . . . ?
C38 C39 C51 C52 -40.8(14) . . . . ?
C38 C39 C62 N9 -126.3(10) . . . . ?
C38 C39 C62 C63 62.6(11) . . . . ?
C39 C40 C41 C42 178.1(9) . . . . ?
C39 C51 C52 C53 -176.7(10) . . . . ?
C39 C62 C63 U1 102.8(9) . . . . ?
C39 C62 C63 C64 175.8(9) . . . . ?
C40 N7 C43 C42 -0.1(10) . . . . ?
C40 N7 C43 C44 177.3(8) . . . . ?
C40 C39 C51 N11 -100.0(11) . . . . ?
C40 C39 C51 C52 77.1(12) . . . . ?
C40 C39 C62 N9 117.1(10) . . . . ?
C40 C39 C62 C63 -54.0(12) . . . . ?
C40 C41 C42 C43 -0.7(11) . . . . ?
C41 C42 C43 N7 0.6(11) . . . . ?
C41 C42 C43 C44 -176.5(10) . . . . ?
C42 C43 C44 N8 178.5(10) . . . . ?
C43 N7 C40 C39 -178.0(8) . . . . ?
C43 N7 C40 C41 -0.3(10) . . . . ?
C44 N8 C45 C46 -25.2(12) . . . . ?
C44 N8 C45 C50 97.2(9) . . . . ?
C45 N8 C44 C43 -173.7(8) . . . . ?
C45 C46 C47 C48 -58.6(13) . . . . ?
C46 C45 C50 C49 -58.7(11) . . . . ?
C46 C47 C48 C49 54.0(14) . . . . ?
C47 C48 C49 C50 -52.8(13) . . . . ?
C48 C49 C50 C45 55.9(12) . . . . ?
C50 C45 C46 C47 60.2(11) . . . . ?
C51 N11 C54 C53 -0.3(12) . . . . ?
C51 N11 C54 C55 -179.8(9) . . . . ?
C51 C39 C40 N7 98.5(10) . . . . ?
C51 C39 C40 C41 -78.6(12) . . . . ?
C51 C39 C62 N9 -7.0(14) . . . . ?
C51 C39 C62 C63 -178.1(9) . . . . ?
C51 C52 C53 C54 -0.9(14) . . . . ?
C52 C53 C54 N11 0.8(13) . . . . ?
C52 C53 C54 C55 -179.7(11) . . . . ?
C53 C54 C55 N12 179.3(11) . . . . ?
C54 N11 C51 C39 177.2(9) . . . . ?
C54 N11 C51 C52 -0.3(12) . . . . ?
C55 N12 C56 C57 147.5(9) . . . . ?
C55 N12 C56 C61 -90.1(10) . . . . ?
C56 N12 C55 C54 178.2(9) . . . . ?
C56 C57 C58 C59 -57.2(11) . . . . ?
C57 C56 C61 C60 -55.9(9) . . . . ?
C57 C58 C59 C60 55.0(10) . . . . ?
C58 C59 C60 C61 -55.4(11) . . . . ?
C59 C60 C61 C56 56.2(10) . . . . ?
C61 C56 C57 C58 57.3(10) . . . . ?
C62 N9 C65 U1 71.7(6) . . . . ?
C62 N9 C65 C64 3.4(10) . . . . ?
C62 N9 C65 C66 -171.6(8) . . . . ?
C62 C39 C40 N7 -28.4(11) . . . . ?
C62 C39 C40 C41 154.4(9) . . . . ?
C62 C39 C51 N11 24.0(14) . . . . ?
C62 C39 C51 C52 -158.8(10) . . . . ?
C62 C63 C64 U1 -74.8(7) . . . . ?
C62 C63 C64 C65 -1.2(10) . . . . ?
C63 C64 C65 U1 -71.9(6) . . . . ?
C63 C64 C65 N9 -1.3(10) . . . . ?
C63 C64 C65 C66 172.8(10) . . . . ?
C64 C65 C66 N10 177.3(9) . . . . ?
C65 N9 C62 C39 -176.3(9) . . . . ?
C65 N9 C62 C63 -4.1(10) . . . . ?
C66 N10 C67 C68 -74.1(11) . . . . ?
C66 N10 C67 C72 166.1(9) . . . . ?
C67 N10 C66 C65 169.6(9) . . . . ?
C67 C68 C69 C70 54.3(17) . . . . ?
C68 C67 C72 C71 59.1(13) . . . . ?
C68 C69 C70 C71 -51.1(19) . . . . ?
C69 C70 C71 C72 50.7(18) . . . . ?
C70 C71 C72 C67 -55.6(16) . . . . ?
C72 C67 C68 C69 -57.9(13) . . . . ?
C73 O5 C76 C75 -11.7(17) . . . . ?
C73 C74 C75 C76 -40.5(19) . . . . ?
C74 C75 C76 O5 34(2) . . . . ?
C76 O5 C73 C74 -12.8(15) . . . . ?
C81 N2 C8 C7 -173.6(7) . . . . ?
C82 C11 C12 C13 -55.8(12) . . . . ?
C3 O6 C10 C79A -38(4) . . . . ?
C3 O6 C77 C79 32(4) . . . . ?
C3 C80 C79A C10 14(5) . . . . ?
C10 O6 C3 C80 47(3) . . . . ?
C77 O6 C3 C78 -24(4) . . . . ?
C77 C79 C78 C3 14(4) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.151 -0.970 1646.0 411.2 '10 THF'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.824
_oxdiff_exptl_absorpt_empirical_full_min 0.595
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Tetrahydrofuran'
_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_to334_refinalize
_database_code_depnum_ccdc_archive 'CCDC 2313500'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2023-12-11 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_audit_creation_date             2023-10-11
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C51 H62 Li N9 O2 U'
_chemical_formula_sum            'C51 H62 Li N9 O2 U'
_chemical_formula_weight         1078.06
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C51 H62 Li N9 O2 U'
_chemical_oxdiff_usercomment     'Precipitation from pyridine'
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'
Li Li -0.0003 0.0001 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   18.3220(7)
_cell_length_b                   13.2763(4)
_cell_length_c                   20.5072(9)
_cell_angle_alpha                90
_cell_angle_beta                 108.143(4)
_cell_angle_gamma                90
_cell_volume                     4740.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9284
_cell_measurement_temperature    119.99(11)
_cell_measurement_theta_max      26.0820
_cell_measurement_theta_min      3.6190
_shelx_estimated_absorpt_T_max   0.903
_shelx_estimated_absorpt_T_min   0.642
_exptl_absorpt_coefficient_mu    3.474
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2168
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 17 -12 0.0691
-10 0 29 0.0568
-5 -16 14 0.0476
5 -16 -15 0.0443
10 1 -29 0.0573
-3 16 16 0.0576
-25 -1 0 0.0016
6 -16 -16 0.0459
25 1 0 0.0328

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Pyridene, hexane'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
4.2588 17.0437 -11.8956 0.1107 0.8413 0.5291
-9.7688 -0.2883 28.8375 -0.1091 -0.8343 0.5405
-4.9890 -16.3250 14.0808 -0.1161 -0.8828 -0.4553
4.9736 -15.8798 -15.3226 -0.0042 -0.0277 -0.9996
9.7646 1.0290 -28.7954 0.1119 0.8548 -0.5067
-3.3342 15.6100 15.9389 0.0762 -0.0028 0.9971
-24.5807 -1.0399 0.3073 -0.9996 0.0258 -0.0092
6.3272 -15.5311 -16.0245 0.0449 -0.0003 -0.9990
24.5807 1.0399 -0.3073 0.9996 -0.0258 0.0092

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_av_unetI/netI     0.0714
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            50829
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         3.284
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.99(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -33.00  53.00   1.00   40.00    --  -15.66  44.00 -21.00   86
  2  ω    -51.00  35.00   1.00   40.00    --   17.38 -44.00-171.00   86
  3  ω      0.00  86.00   1.00   40.00    --   17.38  44.00 -21.00   86
  4  ω    -88.00 -39.00   1.00   40.00    --  -15.66-178.00 -30.00   49
  5  ω    -39.00  11.00   1.00   40.00    --  -15.66 -77.00 -60.00   50
  6  ω    -20.00  56.00   1.00   40.00    --   17.38 -99.00-180.00   76
  7  ω     -9.00  39.00   1.00   40.00    --   17.38  77.00-150.00   48
  8  ω     -9.00  18.00   1.00   40.00    --   17.38  77.00 120.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0406514000
_diffrn_orient_matrix_UB_12      0.0033310000
_diffrn_orient_matrix_UB_13      0.0100194000
_diffrn_orient_matrix_UB_21      -0.0026612000
_diffrn_orient_matrix_UB_22      0.0294108000
_diffrn_orient_matrix_UB_23      -0.0295370000
_diffrn_orient_matrix_UB_31      -0.0012706000
_diffrn_orient_matrix_UB_32      0.0444528000
_diffrn_orient_matrix_UB_33      0.0187558000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7881
_reflns_number_total             10030
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.197
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         10030
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0399
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0179P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0641
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C20(H20), C31(H31), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C21(H21A,H21B), C32(H32A,H32B), C13(H13A,H13B), C2(H2A,H2B),
 C14(H14A,H14B), C12(H12A,H12B), C35(H35A,H35B), C33(H33A,H33B), C11(H11A,H11B),
  C34(H34A,H34B), C22(H22A,H22B), C25(H25A,H25B), C10(H10A,H10B), C23(H23A,
 H23B), C24(H24A,H24B)
2.c Aromatic/amide H refined with riding coordinates:
 C41(H41), C19(H19), C30(H30), C37(H37), C17(H17), C28(H28), C16(H16),
 C47(H47), C48(H48), C49(H49), C27(H27), C40(H40), C8(H8), C6(H6), C50(H50),
 C42(H42), C38(H38), C45(H45), C43(H43), C51(H51), C46(H46), C44(H44), C39(H39)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.54090(2) 0.48420(2) 0.37142(2) 0.01013(5) Uani 1 1 d . . . . .
N7 N 0.4167(2) 0.4010(2) 0.37591(17) 0.0133(8) Uani 1 1 d . . . . .
N4 N 0.46032(19) 0.6365(2) 0.38517(16) 0.0108(8) Uani 1 1 d . . . . .
N3 N 0.60903(18) 0.6444(2) 0.37811(16) 0.0095(7) Uani 1 1 d . . . . .
N6 N 0.5628(2) 0.2983(2) 0.35394(17) 0.0124(8) Uani 1 1 d . . . . .
N5 N 0.66285(19) 0.4539(2) 0.35082(16) 0.0118(8) Uani 1 1 d . . . . .
N1 N 0.86881(19) 0.7062(2) 0.42296(17) 0.0116(8) Uani 1 1 d . . . . .
C41 C 0.4100(2) 0.3655(3) 0.4359(2) 0.0138(10) Uani 1 1 d . . . . .
H41 H 0.452046 0.373244 0.476669 0.017 Uiso 1 1 calc R U . . .
C29 C 0.6656(2) 0.3615(3) 0.3189(2) 0.0130(9) Uani 1 1 d . . . . .
C19 C 0.4886(2) 0.7218(3) 0.3736(2) 0.0126(9) Uani 1 1 d . . . . .
H19 H 0.458029 0.780815 0.368385 0.015 Uiso 1 1 calc R U . . .
N9 N 0.9564(2) 0.6537(2) 0.60055(18) 0.0195(9) Uani 1 1 d . . . . .
C30 C 0.6145(2) 0.2843(3) 0.3238(2) 0.0123(9) Uani 1 1 d . . . . .
H30 H 0.618204 0.220193 0.304461 0.015 Uiso 1 1 calc R U . . .
C20 C 0.3819(2) 0.6365(3) 0.3913(2) 0.0118(9) Uani 1 1 d . . . . .
H20 H 0.375741 0.571421 0.413619 0.014 Uiso 1 1 calc R U . . .
C31 C 0.5187(2) 0.2113(3) 0.3667(2) 0.0120(9) Uani 1 1 d . . . . .
H31 H 0.493499 0.234598 0.400766 0.014 Uiso 1 1 calc R U . . .
C26 C 0.7251(2) 0.5065(3) 0.34892(19) 0.0104(8) Uani 1 1 d . . . . .
N2 N 1.0035(2) 0.8189(2) 0.49122(18) 0.0148(8) Uani 1 1 d . . . . .
C18 C 0.5632(2) 0.7295(3) 0.3684(2) 0.0130(10) Uani 1 1 d . . . . .
N8 N 0.8526(2) 0.8607(2) 0.56188(18) 0.0183(8) Uani 1 1 d . . . . .
C15 C 0.6784(2) 0.6750(3) 0.37487(19) 0.0103(9) Uani 1 1 d . . . . .
C37 C 0.3558(2) 0.3877(3) 0.3189(2) 0.0161(10) Uani 1 1 d . . . . .
H37 H 0.359662 0.410929 0.276256 0.019 Uiso 1 1 calc R U . . .
C3 C 0.7469(2) 0.6042(3) 0.3897(2) 0.0097(9) Uani 1 1 d . . . . .
C36 C 0.4541(2) 0.1790(3) 0.3033(2) 0.0143(10) Uani 1 1 d . . . . .
H36A H 0.423129 0.238476 0.282241 0.017 Uiso 1 1 calc R U . . .
H36B H 0.476045 0.149457 0.269188 0.017 Uiso 1 1 calc R U . . .
C17 C 0.6048(2) 0.8132(3) 0.3590(2) 0.0146(10) Uani 1 1 d . . . . .
H17 H 0.587027 0.880725 0.352090 0.017 Uiso 1 1 calc R U . . .
C4 C 0.8125(2) 0.6585(3) 0.3731(2) 0.0098(9) Uani 1 1 d . . . . .
C28 C 0.7306(2) 0.3593(3) 0.2977(2) 0.0160(10) Uani 1 1 d . . . . .
H28 H 0.746476 0.305047 0.275117 0.019 Uiso 1 1 calc R U . . .
C5 C 0.8196(2) 0.6747(3) 0.3079(2) 0.0122(9) Uani 1 1 d . . . . .
C16 C 0.6771(2) 0.7789(3) 0.3618(2) 0.0140(10) Uani 1 1 d . . . . .
H16 H 0.717972 0.818239 0.356050 0.017 Uiso 1 1 calc R U . . .
C21 C 0.3662(2) 0.7210(3) 0.4362(2) 0.0167(10) Uani 1 1 d . . . . .
H21A H 0.405433 0.719150 0.482066 0.020 Uiso 1 1 calc R U . . .
H21B H 0.369753 0.787119 0.415066 0.020 Uiso 1 1 calc R U . . .
C47 C 1.0028(2) 0.5834(3) 0.5877(2) 0.0214(11) Uani 1 1 d . . . . .
H47 H 1.024631 0.596147 0.552172 0.026 Uiso 1 1 calc R U . . .
C32 C 0.5678(2) 0.1200(3) 0.3991(2) 0.0136(9) Uani 1 1 d . . . . .
H32A H 0.589987 0.088891 0.365651 0.016 Uiso 1 1 calc R U . . .
H32B H 0.610502 0.141419 0.439686 0.016 Uiso 1 1 calc R U . . .
C48 C 1.0206(2) 0.4937(3) 0.6232(2) 0.0216(10) Uani 1 1 d . . . . .
H48 H 1.053588 0.445952 0.612264 0.026 Uiso 1 1 calc R U . . .
C13 C 1.1488(2) 0.9853(3) 0.6192(2) 0.0216(10) Uani 1 1 d . . . . .
H13A H 1.153642 1.040121 0.588017 0.026 Uiso 1 1 calc R U . . .
H13B H 1.147454 1.016239 0.662674 0.026 Uiso 1 1 calc R U . . .
C49 C 0.9893(3) 0.4754(3) 0.6747(2) 0.0279(11) Uani 1 1 d . . . . .
H49 H 0.999825 0.413851 0.699544 0.033 Uiso 1 1 calc R U . . .
C27 C 0.7681(2) 0.4508(3) 0.3155(2) 0.0147(9) Uani 1 1 d . . . . .
H27 H 0.813779 0.471684 0.306809 0.018 Uiso 1 1 calc R U . . .
C40 C 0.3442(3) 0.3184(3) 0.4395(2) 0.0180(10) Uani 1 1 d . . . . .
H40 H 0.341125 0.294186 0.482121 0.022 Uiso 1 1 calc R U . . .
C2 C 0.7692(2) 0.5746(3) 0.46685(19) 0.0121(9) Uani 1 1 d . . . . .
H2A H 0.788951 0.635151 0.494958 0.014 Uiso 1 1 calc R U . . .
H2B H 0.722353 0.552394 0.477039 0.014 Uiso 1 1 calc R U . . .
C14 C 1.0735(2) 0.9274(3) 0.5862(2) 0.0194(10) Uani 1 1 d . . . . .
H14A H 1.065605 0.878019 0.619527 0.023 Uiso 1 1 calc R U . . .
H14B H 1.029896 0.975236 0.574631 0.023 Uiso 1 1 calc R U . . .
C8 C 0.9810(2) 0.8069(3) 0.4256(2) 0.0156(10) Uani 1 1 d . . . . .
H8 H 1.011242 0.835984 0.400367 0.019 Uiso 1 1 calc R U . . .
C12 C 1.2178(2) 0.9166(3) 0.6333(2) 0.0231(11) Uani 1 1 d . . . . .
H12A H 1.217391 0.868983 0.670397 0.028 Uiso 1 1 calc R U . . .
H12B H 1.265221 0.957412 0.649567 0.028 Uiso 1 1 calc R U . . .
C9 C 1.0754(2) 0.8728(3) 0.5217(2) 0.0152(10) Uani 1 1 d . . . . .
H9 H 1.081487 0.923929 0.487993 0.018 Uiso 1 1 calc R U . . .
C35 C 0.4030(2) 0.1019(3) 0.3225(2) 0.0190(10) Uani 1 1 d . . . . .
H35A H 0.363594 0.078165 0.280311 0.023 Uiso 1 1 calc R U . . .
H35B H 0.376198 0.134345 0.352052 0.023 Uiso 1 1 calc R U . . .
C33 C 0.5169(2) 0.0440(3) 0.4205(2) 0.0168(10) Uani 1 1 d . . . . .
H33A H 0.547801 -0.016168 0.440351 0.020 Uiso 1 1 calc R U . . .
H33B H 0.498127 0.074239 0.456369 0.020 Uiso 1 1 calc R U . . .
C11 C 1.2186(2) 0.8575(3) 0.5704(2) 0.0210(10) Uani 1 1 d . . . . .
H11A H 1.261444 0.808457 0.583273 0.025 Uiso 1 1 calc R U . . .
H11B H 1.227722 0.904249 0.536053 0.025 Uiso 1 1 calc R U . . .
C7 C 0.9137(2) 0.7525(3) 0.3884(2) 0.0139(9) Uani 1 1 d . . . . .
C6 C 0.8847(2) 0.7347(3) 0.3180(2) 0.0152(10) Uani 1 1 d . . . . .
H6 H 0.905200 0.758717 0.283712 0.018 Uiso 1 1 calc R U . . .
C50 C 0.9428(3) 0.5463(3) 0.6903(2) 0.0298(12) Uani 1 1 d . . . . .
H50 H 0.921348 0.535861 0.726357 0.036 Uiso 1 1 calc R U . . .
C1 C 0.8291(2) 0.4919(3) 0.4884(2) 0.0190(10) Uani 1 1 d . . . . .
H1A H 0.807900 0.429075 0.464962 0.028 Uiso 1 1 calc R U . . .
H1B H 0.843220 0.482013 0.538161 0.028 Uiso 1 1 calc R U . . .
H1C H 0.874682 0.511085 0.476048 0.028 Uiso 1 1 calc R U . . .
C42 C 0.7796(3) 0.8826(3) 0.5283(2) 0.0238(11) Uani 1 1 d . . . . .
H42 H 0.757546 0.854991 0.483732 0.029 Uiso 1 1 calc R U . . .
C38 C 0.2883(3) 0.3422(3) 0.3195(2) 0.0215(11) Uani 1 1 d . . . . .
H38 H 0.246347 0.335433 0.278513 0.026 Uiso 1 1 calc R U . . .
C45 C 0.8412(3) 0.9634(3) 0.6538(3) 0.0329(13) Uani 1 1 d . . . . .
H45 H 0.864944 0.991240 0.698033 0.039 Uiso 1 1 calc R U . . .
C43 C 0.7340(3) 0.9436(3) 0.5547(3) 0.0312(12) Uani 1 1 d . . . . .
H43 H 0.682114 0.957406 0.528945 0.037 Uiso 1 1 calc R U . . .
C34 C 0.4485(2) 0.0118(3) 0.3602(2) 0.0202(10) Uani 1 1 d . . . . .
H34A H 0.414358 -0.031624 0.377083 0.024 Uiso 1 1 calc R U . . .
H34B H 0.466998 -0.028280 0.327757 0.024 Uiso 1 1 calc R U . . .
C51 C 0.9285(3) 0.6332(3) 0.6517(2) 0.0242(11) Uani 1 1 d . . . . .
H51 H 0.896206 0.682234 0.662463 0.029 Uiso 1 1 calc R U . . .
C22 C 0.2869(3) 0.7087(3) 0.4438(2) 0.0227(11) Uani 1 1 d . . . . .
H22A H 0.276908 0.765448 0.471170 0.027 Uiso 1 1 calc R U . . .
H22B H 0.285343 0.645595 0.468979 0.027 Uiso 1 1 calc R U . . .
C46 C 0.8820(3) 0.9019(3) 0.6235(2) 0.0261(11) Uani 1 1 d . . . . .
H46 H 0.934192 0.888272 0.648204 0.031 Uiso 1 1 calc R U . . .
C25 C 0.3205(2) 0.6382(3) 0.3211(2) 0.0164(10) Uani 1 1 d . . . . .
H25A H 0.330384 0.583063 0.292452 0.020 Uiso 1 1 calc R U . . .
H25B H 0.323267 0.702819 0.297972 0.020 Uiso 1 1 calc R U . . .
C44 C 0.7661(3) 0.9835(3) 0.6192(3) 0.0366(13) Uani 1 1 d . . . . .
H44 H 0.736416 1.024515 0.639351 0.044 Uiso 1 1 calc R U . . .
C39 C 0.2833(3) 0.3071(3) 0.3808(2) 0.0234(11) Uani 1 1 d . . . . .
H39 H 0.237723 0.274877 0.382578 0.028 Uiso 1 1 calc R U . . .
C10 C 1.1436(2) 0.8019(3) 0.5386(2) 0.0168(10) Uani 1 1 d . . . . .
H10A H 1.137511 0.749561 0.570916 0.020 Uiso 1 1 calc R U . . .
H10B H 1.145159 0.767739 0.496115 0.020 Uiso 1 1 calc R U . . .
C23 C 0.2241(3) 0.7058(3) 0.3746(2) 0.0258(11) Uani 1 1 d . . . . .
H23A H 0.174116 0.691597 0.381769 0.031 Uiso 1 1 calc R U . . .
H23B H 0.220504 0.772469 0.352153 0.031 Uiso 1 1 calc R U . . .
C24 C 0.2404(3) 0.6256(3) 0.3280(2) 0.0230(11) Uani 1 1 d . . . . .
H24A H 0.201570 0.630282 0.281992 0.028 Uiso 1 1 calc R U . . .
H24B H 0.236020 0.558098 0.346910 0.028 Uiso 1 1 calc R U . . .
Li1 Li 0.9167(4) 0.7572(5) 0.5222(4) 0.0192(17) Uani 1 1 d . . . . .
O1 O 0.57822(15) 0.46755(17) 0.46130(13) 0.0125(6) Uani 1 1 d . . . . .
O2 O 0.49313(15) 0.49461(17) 0.28211(13) 0.0139(6) Uani 1 1 d . . . . .
H5 H 0.785(2) 0.650(2) 0.2642(19) 0.014(11) 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
U1 N7 2.557(3) . ?
U1 N4 2.570(3) . ?
U1 N3 2.449(3) . ?
U1 N6 2.544(3) . ?
U1 N5 2.433(3) . ?
U1 O1 1.769(3) . ?
U1 O2 1.772(3) . ?
N7 C41 1.357(5) . ?
N7 C37 1.354(5) . ?
N4 C19 1.298(5) . ?
N4 C20 1.481(5) . ?
N3 C18 1.384(5) . ?
N3 C15 1.356(5) . ?
N6 C30 1.296(5) . ?
N6 C31 1.479(5) . ?
N5 C29 1.398(5) . ?
N5 C26 1.349(5) . ?
N1 C4 1.361(5) . ?
N1 C7 1.385(5) . ?
N1 Li1 2.063(8) . ?
C41 H41 0.9500 . ?
C41 C40 1.381(6) . ?
C29 C30 1.413(5) . ?
C29 C28 1.389(6) . ?
C19 H19 0.9500 . ?
C19 C18 1.406(6) . ?
N9 C47 1.342(5) . ?
N9 C51 1.331(5) . ?
N9 Li1 2.068(8) . ?
C30 H30 0.9500 . ?
C20 H20 1.0000 . ?
C20 C21 1.534(5) . ?
C20 C25 1.526(5) . ?
C31 H31 1.0000 . ?
C31 C36 1.522(5) . ?
C31 C32 1.532(5) . ?
C26 C3 1.528(5) . ?
C26 C27 1.404(5) . ?
N2 C8 1.288(5) . ?
N2 C9 1.458(5) . ?
N2 Li1 2.057(8) . ?
C18 C17 1.395(5) . ?
N8 C42 1.331(6) . ?
N8 C46 1.328(5) . ?
N8 Li1 2.128(8) . ?
C15 C3 1.520(5) . ?
C15 C16 1.405(5) . ?
C37 H37 0.9500 . ?
C37 C38 1.380(6) . ?
C3 C4 1.528(5) . ?
C3 C2 1.557(5) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C35 1.519(5) . ?
C17 H17 0.9500 . ?
C17 C16 1.384(6) . ?
C4 C5 1.401(5) . ?
C28 H28 0.9500 . ?
C28 C27 1.387(5) . ?
C5 C6 1.394(5) . ?
C5 H5 0.98(4) . ?
C16 H16 0.9500 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.517(6) . ?
C47 H47 0.9500 . ?
C47 C48 1.382(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.528(5) . ?
C48 H48 0.9500 . ?
C48 C49 1.370(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.539(5) . ?
C13 C12 1.511(5) . ?
C49 H49 0.9500 . ?
C49 C50 1.373(6) . ?
C27 H27 0.9500 . ?
C40 H40 0.9500 . ?
C40 C39 1.371(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.516(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C9 1.517(5) . ?
C8 H8 0.9500 . ?
C8 C7 1.428(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C11 1.516(5) . ?
C9 H9 1.0000 . ?
C9 C10 1.518(5) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C34 1.523(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.522(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C10 1.517(5) . ?
C7 C6 1.395(5) . ?
C6 H6 0.9500 . ?
C50 H50 0.9500 . ?
C50 C51 1.377(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C42 H42 0.9500 . ?
C42 C43 1.390(6) . ?
C38 H38 0.9500 . ?
C38 C39 1.369(6) . ?
C45 H45 0.9500 . ?
C45 C46 1.378(6) . ?
C45 C44 1.364(7) . ?
C43 H43 0.9500 . ?
C43 C44 1.376(6) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C51 H51 0.9500 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.524(6) . ?
C46 H46 0.9500 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C24 1.527(6) . ?
C44 H44 0.9500 . ?
C39 H39 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.521(6) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N7 U1 N4 77.74(10) . . ?
N3 U1 N7 144.80(10) . . ?
N3 U1 N4 67.10(10) . . ?
N3 U1 N6 138.66(11) . . ?
N6 U1 N7 76.53(10) . . ?
N6 U1 N4 154.14(11) . . ?
N5 U1 N7 144.14(10) . . ?
N5 U1 N4 137.66(10) . . ?
N5 U1 N3 70.97(10) . . ?
N5 U1 N6 67.75(10) . . ?
O1 U1 N7 88.17(11) . . ?
O1 U1 N4 91.89(10) . . ?
O1 U1 N3 91.45(11) . . ?
O1 U1 N6 89.93(10) . . ?
O1 U1 N5 94.72(11) . . ?
O1 U1 O2 173.13(12) . . ?
O2 U1 N7 84.97(11) . . ?
O2 U1 N4 86.35(11) . . ?
O2 U1 N3 93.97(11) . . ?
O2 U1 N6 88.78(10) . . ?
O2 U1 N5 91.04(11) . . ?
C41 N7 U1 121.0(3) . . ?
C37 N7 U1 121.9(3) . . ?
C37 N7 C41 117.1(4) . . ?
C19 N4 U1 113.0(3) . . ?
C19 N4 C20 117.9(3) . . ?
C20 N4 U1 128.0(2) . . ?
C18 N3 U1 115.1(2) . . ?
C15 N3 U1 136.6(2) . . ?
C15 N3 C18 106.6(3) . . ?
C30 N6 U1 112.2(2) . . ?
C30 N6 C31 119.5(3) . . ?
C31 N6 U1 127.9(2) . . ?
C29 N5 U1 113.3(3) . . ?
C26 N5 U1 138.6(2) . . ?
C26 N5 C29 106.6(3) . . ?
C4 N1 C7 104.7(3) . . ?
C4 N1 Li1 152.0(4) . . ?
C7 N1 Li1 102.8(3) . . ?
N7 C41 H41 118.9 . . ?
N7 C41 C40 122.2(4) . . ?
C40 C41 H41 118.9 . . ?
N5 C29 C30 118.8(4) . . ?
C28 C29 N5 108.9(3) . . ?
C28 C29 C30 131.2(4) . . ?
N4 C19 H19 119.0 . . ?
N4 C19 C18 122.0(4) . . ?
C18 C19 H19 119.0 . . ?
C47 N9 Li1 113.6(4) . . ?
C51 N9 C47 115.8(4) . . ?
C51 N9 Li1 128.3(4) . . ?
N6 C30 C29 121.9(3) . . ?
N6 C30 H30 119.0 . . ?
C29 C30 H30 119.0 . . ?
N4 C20 H20 106.8 . . ?
N4 C20 C21 114.8(3) . . ?
N4 C20 C25 111.7(3) . . ?
C21 C20 H20 106.8 . . ?
C25 C20 H20 106.8 . . ?
C25 C20 C21 109.6(3) . . ?
N6 C31 H31 106.1 . . ?
N6 C31 C36 113.1(3) . . ?
N6 C31 C32 114.6(3) . . ?
C36 C31 H31 106.1 . . ?
C36 C31 C32 110.1(3) . . ?
C32 C31 H31 106.1 . . ?
N5 C26 C3 120.2(3) . . ?
N5 C26 C27 110.5(3) . . ?
C27 C26 C3 128.6(4) . . ?
C8 N2 C9 117.5(3) . . ?
C8 N2 Li1 104.3(3) . . ?
C9 N2 Li1 138.2(3) . . ?
N3 C18 C19 119.4(3) . . ?
N3 C18 C17 109.6(4) . . ?
C17 C18 C19 130.9(4) . . ?
C42 N8 Li1 121.8(4) . . ?
C46 N8 C42 116.6(4) . . ?
C46 N8 Li1 121.5(4) . . ?
N3 C15 C3 122.2(3) . . ?
N3 C15 C16 110.0(3) . . ?
C16 C15 C3 127.5(4) . . ?
N7 C37 H37 118.3 . . ?
N7 C37 C38 123.3(4) . . ?
C38 C37 H37 118.3 . . ?
C26 C3 C2 106.4(3) . . ?
C15 C3 C26 110.9(3) . . ?
C15 C3 C4 108.8(3) . . ?
C15 C3 C2 107.4(3) . . ?
C4 C3 C26 111.6(3) . . ?
C4 C3 C2 111.7(3) . . ?
C31 C36 H36A 109.6 . . ?
C31 C36 H36B 109.6 . . ?
H36A C36 H36B 108.1 . . ?
C35 C36 C31 110.3(3) . . ?
C35 C36 H36A 109.6 . . ?
C35 C36 H36B 109.6 . . ?
C18 C17 H17 126.6 . . ?
C16 C17 C18 106.9(3) . . ?
C16 C17 H17 126.6 . . ?
N1 C4 C3 121.2(4) . . ?
N1 C4 C5 111.8(4) . . ?
C5 C4 C3 126.8(4) . . ?
C29 C28 H28 126.2 . . ?
C27 C28 C29 107.5(3) . . ?
C27 C28 H28 126.2 . . ?
C4 C5 H5 126(2) . . ?
C6 C5 C4 106.0(4) . . ?
C6 C5 H5 128(2) . . ?
C15 C16 H16 126.6 . . ?
C17 C16 C15 106.9(4) . . ?
C17 C16 H16 126.6 . . ?
C20 C21 H21A 109.6 . . ?
C20 C21 H21B 109.6 . . ?
H21A C21 H21B 108.1 . . ?
C22 C21 C20 110.3(3) . . ?
C22 C21 H21A 109.6 . . ?
C22 C21 H21B 109.6 . . ?
N9 C47 H47 118.1 . . ?
N9 C47 C48 123.8(4) . . ?
C48 C47 H47 118.1 . . ?
C31 C32 H32A 110.0 . . ?
C31 C32 H32B 110.0 . . ?
H32A C32 H32B 108.3 . . ?
C33 C32 C31 108.6(3) . . ?
C33 C32 H32A 110.0 . . ?
C33 C32 H32B 110.0 . . ?
C47 C48 H48 120.9 . . ?
C49 C48 C47 118.2(4) . . ?
C49 C48 H48 120.9 . . ?
H13A C13 H13B 108.0 . . ?
C14 C13 H13A 109.4 . . ?
C14 C13 H13B 109.4 . . ?
C12 C13 H13A 109.4 . . ?
C12 C13 H13B 109.4 . . ?
C12 C13 C14 111.4(3) . . ?
C48 C49 H49 120.1 . . ?
C48 C49 C50 119.7(4) . . ?
C50 C49 H49 120.1 . . ?
C26 C27 H27 126.8 . . ?
C28 C27 C26 106.4(4) . . ?
C28 C27 H27 126.8 . . ?
C41 C40 H40 120.4 . . ?
C39 C40 C41 119.2(4) . . ?
C39 C40 H40 120.4 . . ?
C3 C2 H2A 108.6 . . ?
C3 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
C1 C2 C3 114.6(3) . . ?
C1 C2 H2A 108.6 . . ?
C1 C2 H2B 108.6 . . ?
C13 C14 H14A 109.4 . . ?
C13 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C9 C14 C13 111.1(4) . . ?
C9 C14 H14A 109.4 . . ?
C9 C14 H14B 109.4 . . ?
N2 C8 H8 117.9 . . ?
N2 C8 C7 124.2(4) . . ?
C7 C8 H8 117.9 . . ?
C13 C12 H12A 109.2 . . ?
C13 C12 H12B 109.2 . . ?
C13 C12 C11 112.2(4) . . ?
H12A C12 H12B 107.9 . . ?
C11 C12 H12A 109.2 . . ?
C11 C12 H12B 109.2 . . ?
N2 C9 C14 110.3(3) . . ?
N2 C9 H9 108.5 . . ?
N2 C9 C10 111.3(3) . . ?
C14 C9 H9 108.5 . . ?
C14 C9 C10 109.8(3) . . ?
C10 C9 H9 108.5 . . ?
C36 C35 H35A 109.2 . . ?
C36 C35 H35B 109.2 . . ?
C36 C35 C34 112.1(3) . . ?
H35A C35 H35B 107.9 . . ?
C34 C35 H35A 109.2 . . ?
C34 C35 H35B 109.2 . . ?
C32 C33 H33A 109.2 . . ?
C32 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
C34 C33 C32 111.9(3) . . ?
C34 C33 H33A 109.2 . . ?
C34 C33 H33B 109.2 . . ?
C12 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C12 C11 C10 111.7(4) . . ?
H11A C11 H11B 107.9 . . ?
C10 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
N1 C7 C8 120.2(4) . . ?
N1 C7 C6 111.0(4) . . ?
C6 C7 C8 128.7(4) . . ?
C5 C6 C7 106.5(4) . . ?
C5 C6 H6 126.8 . . ?
C7 C6 H6 126.8 . . ?
C49 C50 H50 121.2 . . ?
C49 C50 C51 117.6(4) . . ?
C51 C50 H50 121.2 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N8 C42 H42 118.2 . . ?
N8 C42 C43 123.7(4) . . ?
C43 C42 H42 118.2 . . ?
C37 C38 H38 120.9 . . ?
C39 C38 C37 118.2(4) . . ?
C39 C38 H38 120.9 . . ?
C46 C45 H45 120.6 . . ?
C44 C45 H45 120.6 . . ?
C44 C45 C46 118.8(5) . . ?
C42 C43 H43 121.0 . . ?
C44 C43 C42 118.0(4) . . ?
C44 C43 H43 121.0 . . ?
C35 C34 H34A 109.2 . . ?
C35 C34 H34B 109.2 . . ?
C33 C34 C35 112.0(3) . . ?
C33 C34 H34A 109.2 . . ?
C33 C34 H34B 109.2 . . ?
H34A C34 H34B 107.9 . . ?
N9 C51 C50 124.9(4) . . ?
N9 C51 H51 117.5 . . ?
C50 C51 H51 117.5 . . ?
C21 C22 H22A 109.2 . . ?
C21 C22 H22B 109.2 . . ?
C21 C22 C23 112.2(4) . . ?
H22A C22 H22B 107.9 . . ?
C23 C22 H22A 109.2 . . ?
C23 C22 H22B 109.2 . . ?
N8 C46 C45 123.8(5) . . ?
N8 C46 H46 118.1 . . ?
C45 C46 H46 118.1 . . ?
C20 C25 H25A 109.4 . . ?
C20 C25 H25B 109.4 . . ?
C20 C25 C24 111.1(3) . . ?
H25A C25 H25B 108.0 . . ?
C24 C25 H25A 109.4 . . ?
C24 C25 H25B 109.4 . . ?
C45 C44 C43 119.0(5) . . ?
C45 C44 H44 120.5 . . ?
C43 C44 H44 120.5 . . ?
C40 C39 H39 120.0 . . ?
C38 C39 C40 120.0(4) . . ?
C38 C39 H39 120.0 . . ?
C9 C10 H10A 109.3 . . ?
C9 C10 H10B 109.3 . . ?
C11 C10 C9 111.6(3) . . ?
C11 C10 H10A 109.3 . . ?
C11 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
C22 C23 H23A 109.4 . . ?
C22 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
C24 C23 C22 111.4(4) . . ?
C24 C23 H23A 109.4 . . ?
C24 C23 H23B 109.4 . . ?
C25 C24 H24A 109.4 . . ?
C25 C24 H24B 109.4 . . ?
C23 C24 C25 111.3(4) . . ?
C23 C24 H24A 109.4 . . ?
C23 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
N1 Li1 N9 119.2(3) . . ?
N1 Li1 N8 118.3(4) . . ?
N9 Li1 N8 103.5(3) . . ?
N2 Li1 N1 87.6(3) . . ?
N2 Li1 N9 112.7(4) . . ?
N2 Li1 N8 115.6(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 N7 C41 C40 -178.7(3) . . . . ?
U1 N7 C37 C38 179.3(3) . . . . ?
U1 N4 C19 C18 -12.4(5) . . . . ?
U1 N4 C20 C21 147.6(3) . . . . ?
U1 N4 C20 C25 -86.9(3) . . . . ?
U1 N3 C18 C19 16.4(5) . . . . ?
U1 N3 C18 C17 -167.7(3) . . . . ?
U1 N3 C15 C3 -22.0(6) . . . . ?
U1 N3 C15 C16 162.6(3) . . . . ?
U1 N6 C30 C29 15.7(5) . . . . ?
U1 N6 C31 C36 93.0(4) . . . . ?
U1 N6 C31 C32 -139.8(3) . . . . ?
U1 N5 C29 C30 -21.8(4) . . . . ?
U1 N5 C29 C28 168.8(3) . . . . ?
U1 N5 C26 C3 25.5(6) . . . . ?
U1 N5 C26 C27 -163.6(3) . . . . ?
N7 C41 C40 C39 -0.1(6) . . . . ?
N7 C37 C38 C39 -1.3(6) . . . . ?
N4 C19 C18 N3 -2.1(6) . . . . ?
N4 C19 C18 C17 -177.1(4) . . . . ?
N4 C20 C21 C22 -175.3(3) . . . . ?
N4 C20 C25 C24 173.3(3) . . . . ?
N3 C18 C17 C16 1.1(5) . . . . ?
N3 C15 C3 C26 50.1(5) . . . . ?
N3 C15 C3 C4 173.2(3) . . . . ?
N3 C15 C3 C2 -65.8(4) . . . . ?
N3 C15 C16 C17 1.7(5) . . . . ?
N6 C31 C36 C35 -170.3(3) . . . . ?
N6 C31 C32 C33 170.3(3) . . . . ?
N5 C29 C30 N6 3.6(6) . . . . ?
N5 C29 C28 C27 -0.8(5) . . . . ?
N5 C26 C3 C15 -51.1(5) . . . . ?
N5 C26 C3 C4 -172.6(3) . . . . ?
N5 C26 C3 C2 65.4(4) . . . . ?
N5 C26 C27 C28 -1.3(4) . . . . ?
N1 C4 C5 C6 0.9(4) . . . . ?
N1 C7 C6 C5 -0.4(4) . . . . ?
C41 N7 C37 C38 1.2(6) . . . . ?
C41 C40 C39 C38 0.0(6) . . . . ?
C29 N5 C26 C3 -170.1(3) . . . . ?
C29 N5 C26 C27 0.8(4) . . . . ?
C29 C28 C27 C26 1.2(5) . . . . ?
C19 N4 C20 C21 -45.3(5) . . . . ?
C19 N4 C20 C25 80.2(4) . . . . ?
C19 C18 C17 C16 176.4(4) . . . . ?
N9 C47 C48 C49 -0.2(7) . . . . ?
C30 N6 C31 C36 -79.2(5) . . . . ?
C30 N6 C31 C32 48.1(5) . . . . ?
C30 C29 C28 C27 -168.4(4) . . . . ?
C20 N4 C19 C18 178.6(4) . . . . ?
C20 C21 C22 C23 -56.5(4) . . . . ?
C20 C25 C24 C23 56.3(4) . . . . ?
C31 N6 C30 C29 -171.0(4) . . . . ?
C31 C36 C35 C34 -54.9(4) . . . . ?
C31 C32 C33 C34 57.4(4) . . . . ?
C26 N5 C29 C30 169.3(3) . . . . ?
C26 N5 C29 C28 0.0(4) . . . . ?
C26 C3 C4 N1 -141.6(3) . . . . ?
C26 C3 C4 C5 45.1(5) . . . . ?
C26 C3 C2 C1 52.5(4) . . . . ?
N2 C8 C7 N1 -1.8(6) . . . . ?
N2 C8 C7 C6 -179.7(4) . . . . ?
N2 C9 C10 C11 180.0(3) . . . . ?
C18 N3 C15 C3 174.3(3) . . . . ?
C18 N3 C15 C16 -1.1(4) . . . . ?
C18 C17 C16 C15 -1.7(5) . . . . ?
N8 C42 C43 C44 0.0(7) . . . . ?
C15 N3 C18 C19 -175.9(4) . . . . ?
C15 N3 C18 C17 0.0(4) . . . . ?
C15 C3 C4 N1 95.7(4) . . . . ?
C15 C3 C4 C5 -77.7(4) . . . . ?
C15 C3 C2 C1 171.3(3) . . . . ?
C37 N7 C41 C40 -0.5(5) . . . . ?
C37 C38 C39 C40 0.6(6) . . . . ?
C3 C26 C27 C28 168.6(4) . . . . ?
C3 C15 C16 C17 -173.4(4) . . . . ?
C3 C4 C5 C6 174.8(3) . . . . ?
C36 C31 C32 C33 -60.9(4) . . . . ?
C36 C35 C34 C33 51.3(5) . . . . ?
C4 N1 C7 C8 -177.4(3) . . . . ?
C4 N1 C7 C6 0.9(4) . . . . ?
C4 C3 C2 C1 -69.6(4) . . . . ?
C4 C5 C6 C7 -0.3(4) . . . . ?
C28 C29 C30 N6 170.2(4) . . . . ?
C16 C15 C3 C26 -135.4(4) . . . . ?
C16 C15 C3 C4 -12.2(5) . . . . ?
C16 C15 C3 C2 108.8(4) . . . . ?
C21 C20 C25 C24 -58.4(4) . . . . ?
C21 C22 C23 C24 54.0(5) . . . . ?
C47 N9 C51 C50 -1.1(7) . . . . ?
C47 C48 C49 C50 -1.1(7) . . . . ?
C32 C31 C36 C35 60.1(4) . . . . ?
C32 C33 C34 C35 -53.0(5) . . . . ?
C48 C49 C50 C51 1.2(7) . . . . ?
C13 C14 C9 N2 -179.8(3) . . . . ?
C13 C14 C9 C10 57.2(4) . . . . ?
C13 C12 C11 C10 -52.9(5) . . . . ?
C49 C50 C51 N9 -0.1(7) . . . . ?
C27 C26 C3 C15 139.9(4) . . . . ?
C27 C26 C3 C4 18.4(5) . . . . ?
C27 C26 C3 C2 -103.7(4) . . . . ?
C2 C3 C4 N1 -22.6(5) . . . . ?
C2 C3 C4 C5 164.0(3) . . . . ?
C14 C13 C12 C11 52.6(5) . . . . ?
C14 C9 C10 C11 -57.6(4) . . . . ?
C8 N2 C9 C14 150.3(3) . . . . ?
C8 N2 C9 C10 -87.6(4) . . . . ?
C8 C7 C6 C5 177.7(4) . . . . ?
C12 C13 C14 C9 -55.2(5) . . . . ?
C12 C11 C10 C9 55.5(5) . . . . ?
C9 N2 C8 C7 177.4(3) . . . . ?
C7 N1 C4 C3 -175.4(3) . . . . ?
C7 N1 C4 C5 -1.1(4) . . . . ?
C42 N8 C46 C45 1.0(7) . . . . ?
C42 C43 C44 C45 1.2(7) . . . . ?
C51 N9 C47 C48 1.3(6) . . . . ?
C22 C23 C24 C25 -53.3(5) . . . . ?
C46 N8 C42 C43 -1.1(6) . . . . ?
C46 C45 C44 C43 -1.3(7) . . . . ?
C25 C20 C21 C22 58.2(4) . . . . ?
C44 C45 C46 N8 0.2(7) . . . . ?
Li1 N1 C4 C3 -6.2(8) . . . . ?
Li1 N1 C4 C5 168.1(6) . . . . ?
Li1 N1 C7 C8 7.8(4) . . . . ?
Li1 N1 C7 C6 -173.9(3) . . . . ?
Li1 N9 C47 C48 -163.1(4) . . . . ?
Li1 N9 C51 C50 160.6(4) . . . . ?
Li1 N2 C8 C7 -5.6(5) . . . . ?
Li1 N2 C9 C14 -25.3(6) . . . . ?
Li1 N2 C9 C10 96.8(5) . . . . ?
Li1 N8 C42 C43 174.9(4) . . . . ?
Li1 N8 C46 C45 -175.0(4) . . . . ?

_olex2_exptl_crystal_mounting_method ?
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.129
_oxdiff_exptl_absorpt_empirical_full_min 0.839
_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_to499_mp_221123
_database_code_depnum_ccdc_archive 'CCDC 2313506'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2023-12-11 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_audit_creation_date             2023-11-24
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C92 H114 Cl2 Dy2 N16 O4 U2, 3(C5 H5 N)'
_chemical_formula_sum            'C107 H129 Cl2 Dy2 N19 O4 U2'
_chemical_formula_weight         2617.24
_chemical_melting_point          ?
_chemical_oxdiff_formula         C80H110N12U2O4Dy2Cl2
_chemical_oxdiff_usercomment     Pyr/hex
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'
Dy Dy -0.1892 4.4098 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   17.5882(7)
_cell_length_b                   17.0832(4)
_cell_length_c                   17.6031(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.739(4)
_cell_angle_gamma                90
_cell_volume                     5115.0(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12385
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      29.0180
_cell_measurement_theta_min      3.6800
_shelx_estimated_absorpt_T_max   0.396
_shelx_estimated_absorpt_T_min   0.221
_exptl_absorpt_coefficient_mu    4.714
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2572
_exptl_crystal_size_max          0.458
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.241
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28997
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.376
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -53.00  21.00   1.00   60.00    --  -15.82  98.00-155.00   74
  2  ω    -21.00  55.00   1.00   60.00    --   17.54 -98.00  97.00   76
  3  ω    -39.00  11.00   1.00   60.00    --  -15.82 -77.00 -60.00   50
  4  ω     -9.00  29.00   1.00   60.00    --   17.54  77.00  30.00   38
  5  ω     -8.00  38.00   1.00   60.00    --   17.54  77.00  60.00   46
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0097873000
_diffrn_orient_matrix_UB_12      -0.0188712000
_diffrn_orient_matrix_UB_13      -0.0321055000
_diffrn_orient_matrix_UB_21      -0.0403281000
_diffrn_orient_matrix_UB_22      -0.0083800000
_diffrn_orient_matrix_UB_23      -0.0166525000
_diffrn_orient_matrix_UB_31      -0.0042172000
_diffrn_orient_matrix_UB_32      0.0360141000
_diffrn_orient_matrix_UB_33      -0.0207068000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7702
_reflns_number_total             9868
_reflns_odcompleteness_completeness 94.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         3.018
_refine_diff_density_min         -2.343
_refine_diff_density_rms         0.215
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         9868
_refine_ls_number_restraints     200
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0514
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0419P)²+66.7969P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1359
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N9-C47 = N9-C51
 1.33 with sigma of 0.02
 C47-C48 = C50-C51
 1.38 with sigma of 0.02
 C48-C49 = C49-C50
 1.37 with sigma of 0.02
 N10-C56 = N10-C52
 1.33 with sigma of 0.02
 C56-C55 = C53-C52
 1.38 with sigma of 0.02
 C55-C54 = C54-C53
 1.37 with sigma of 0.02
 N9-C50
 2.39 with sigma of 0.04
 C48-C50
 2.35 with sigma of 0.04
 C47-C49
 2.36 with sigma of 0.04
 C49-C51
 2.37 with sigma of 0.04
 N9-C48
 2.4 with sigma of 0.04
 C54-C52
 2.37 with sigma of 0.04
 N10-C53
 2.39 with sigma of 0.04
 C55-C53
 2.35 with sigma of 0.04
 N10-C55
 2.4 with sigma of 0.04
 C56-C54
 2.36 with sigma of 0.04
 N9-C47 \\sim N9-C51
 with sigma of 0.02
 C47-C48 \\sim C48-C49 \\sim C49-C50 \\sim C50-C51
 with sigma of 0.02
 N9-C50 \\sim N9-C48
 with sigma of 0.04
 C49-C51 \\sim C49-C47 \\sim C50-C48 \\sim C51-C47
 with sigma of 0.04
 C56-C55 \\sim C55-C54 \\sim C54-C53 \\sim C53-C52
 with sigma of 0.02
 N10-C53 \\sim N10-C55
 with sigma of 0.04
 N10-C56 \\sim N10-C52
 with sigma of 0.02
 C54-C52 \\sim C54-C56 \\sim C53-C55 \\sim C52-C56
 with sigma of 0.04
3. Restrained planarity
 N9, C47, C48, C49, C50, C51
 with sigma of 0.1
 N10, C56, C55, C54, C53, C52
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N9 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
N10 \\sim C56 \\sim C55 \\sim C54 \\sim C53 \\sim C52: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 N9, C47, C48, C49, C50, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N10, C56, C55, C54, C53, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: N10(0.5) C56(0.5) H56(0.5) C55(0.5) H55(0.5) C54(0.5) H54(0.5)
 C53(0.5) H53(0.5) C52(0.5) H52(0.5)
7.a Ternary CH refined with riding coordinates:
 C31(H31), C20(H20), C9(H9)
7.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C36(H36A,H36B), C21(H21A,H21B), C22(H22A,H22B), C35(H35A,H35B),
 C34(H34A,H34B), C25(H25A,H25B), C10(H10A,H10B), C32(H32A,H32B), C33(H33A,H33B),
  C23(H23A,H23B), C14(H14A,H14B), C11(H11A,H11B), C24(H24A,H24B), C12(H12A,
 H12B), C13(H13A,H13B)
7.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C30(H30), C17(H17), C27(H27), C16(H16), C6(H6), C28(H28), C5(H5),
 C41(H41), C42(H42), C8(H8), C37(H37), C39(H39), C43(H43), C46(H46), C40(H40),
 C44(H44), C38(H38), C45(H45), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51),
  C56(H56), C55(H55), C54(H54), C53(H53), C52(H52)
7.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.55333(2) 0.56235(2) 0.45642(2) 0.01615(10) Uani 1 1 d . . . . .
Dy1 Dy 0.67674(3) 0.71577(2) 0.41013(2) 0.02317(13) Uani 1 1 d . . . . .
Cl1 Cl 0.80488(15) 0.69651(14) 0.52475(14) 0.0305(5) Uani 1 1 d . . . . .
O2 O 0.4450(4) 0.5357(3) 0.4518(3) 0.0171(13) Uani 1 1 d . . . . .
N5 N 0.5198(5) 0.5848(4) 0.3145(4) 0.0176(15) Uani 1 1 d . . . . .
N4 N 0.5794(5) 0.6442(4) 0.5845(4) 0.0184(16) Uani 1 1 d . . . . .
N6 N 0.5860(5) 0.4428(4) 0.3832(4) 0.0204(16) Uani 1 1 d . . . . .
N3 N 0.5248(5) 0.7047(4) 0.4281(4) 0.0210(16) Uani 1 1 d . . . . .
C26 C 0.4794(6) 0.6375(5) 0.2621(5) 0.022(2) Uani 1 1 d . . . . .
N1 N 0.5982(5) 0.7762(4) 0.2940(4) 0.0207(16) Uani 1 1 d . . . . .
N8 N 0.7137(5) 0.6311(5) 0.3107(5) 0.031(2) Uani 1 1 d . . . . .
N7 N 0.6651(5) 0.8420(5) 0.4790(5) 0.0279(18) Uani 1 1 d . . . . .
C29 C 0.5279(6) 0.5188(5) 0.2712(5) 0.0196(19) Uani 1 1 d . . . . .
C19 C 0.5535(6) 0.7143(5) 0.5724(5) 0.0195(19) Uani 1 1 d . . . . .
H19 H 0.556451 0.747289 0.616484 0.023 Uiso 1 1 calc R U . . .
C31 C 0.6307(6) 0.3722(5) 0.4208(5) 0.0198(19) Uani 1 1 d . . . . .
H31 H 0.604342 0.352408 0.461077 0.024 Uiso 1 1 calc R U . . .
C3 C 0.4639(6) 0.7226(5) 0.2809(5) 0.0189(19) Uani 1 1 d . . . . .
C30 C 0.5655(6) 0.4497(5) 0.3087(5) 0.021(2) Uani 1 1 d . . . . .
H30 H 0.575372 0.407721 0.277215 0.025 Uiso 1 1 calc R U . . .
C18 C 0.5202(6) 0.7453(5) 0.4953(5) 0.0191(19) Uani 1 1 d . . . . .
N2 N 0.7614(6) 0.8077(5) 0.3478(5) 0.031(2) Uani 1 1 d . . . . .
C4 C 0.5229(6) 0.7698(5) 0.2497(5) 0.023(2) Uani 1 1 d . . . . .
C7 C 0.6390(6) 0.8181(6) 0.2494(6) 0.028(2) Uani 1 1 d . . . . .
C17 C 0.4727(6) 0.8100(5) 0.4758(5) 0.024(2) Uani 1 1 d . . . . .
H17 H 0.461203 0.847721 0.510928 0.029 Uiso 1 1 calc R U . . .
C27 C 0.4620(6) 0.6059(5) 0.1866(5) 0.028(2) Uani 1 1 d . . . . .
H27 H 0.433673 0.631063 0.139798 0.033 Uiso 1 1 calc R U . . .
C2 C 0.3787(6) 0.7429(5) 0.2362(5) 0.025(2) Uani 1 1 d . . . . .
H2A H 0.368905 0.798951 0.244257 0.030 Uiso 1 1 calc R U . . .
H2B H 0.372543 0.734582 0.179271 0.030 Uiso 1 1 calc R U . . .
C20 C 0.6132(6) 0.6150(5) 0.6643(5) 0.022(2) Uani 1 1 d . . . . .
H20 H 0.582701 0.567362 0.671372 0.026 Uiso 1 1 calc R U . . .
C16 C 0.4449(6) 0.8093(5) 0.3947(5) 0.025(2) Uani 1 1 d . . . . .
H16 H 0.410672 0.846828 0.363720 0.030 Uiso 1 1 calc R U . . .
C15 C 0.4763(5) 0.7435(5) 0.3667(5) 0.0173(18) Uani 1 1 d . . . . .
C36 C 0.6347(6) 0.3045(5) 0.3656(6) 0.026(2) Uani 1 1 d . . . . .
H36A H 0.580736 0.288416 0.337805 0.032 Uiso 1 1 calc R U . . .
H36B H 0.661932 0.321951 0.325770 0.032 Uiso 1 1 calc R U . . .
C6 C 0.5887(7) 0.8376(6) 0.1782(6) 0.033(2) Uani 1 1 d . . . . .
H6 H 0.601695 0.866637 0.137186 0.040 Uiso 1 1 calc R U . . .
C28 C 0.4933(7) 0.5318(6) 0.1920(5) 0.029(2) Uani 1 1 d . . . . .
H28 H 0.491659 0.496531 0.149873 0.035 Uiso 1 1 calc R U . . .
C21 C 0.6107(6) 0.6712(5) 0.7305(5) 0.024(2) Uani 1 1 d . . . . .
H21A H 0.555335 0.685725 0.726646 0.029 Uiso 1 1 calc R U . . .
H21B H 0.639437 0.719624 0.724134 0.029 Uiso 1 1 calc R U . . .
C5 C 0.5139(7) 0.8059(6) 0.1776(6) 0.029(2) Uani 1 1 d . . . . .
H5 H 0.467285 0.808884 0.136154 0.035 Uiso 1 1 calc R U . . .
C22 C 0.6467(6) 0.6368(6) 0.8121(5) 0.033(2) Uani 1 1 d . . . . .
H22A H 0.647363 0.677196 0.852591 0.039 Uiso 1 1 calc R U . . .
H22B H 0.614122 0.592508 0.821680 0.039 Uiso 1 1 calc R U . . .
C41 C 0.6859(7) 0.8476(6) 0.5581(6) 0.034(2) Uani 1 1 d . . . . .
H41 H 0.714695 0.805528 0.587137 0.041 Uiso 1 1 calc R U . . .
C42 C 0.6778(7) 0.6255(6) 0.2338(6) 0.038(3) Uani 1 1 d . . . . .
H42 H 0.630627 0.654508 0.215274 0.045 Uiso 1 1 calc R U . . .
C8 C 0.7182(6) 0.8340(5) 0.2796(5) 0.025(2) Uani 1 1 d . . . . .
H8 H 0.743382 0.866138 0.249228 0.030 Uiso 1 1 calc R U . . .
C37 C 0.6269(7) 0.9027(6) 0.4407(6) 0.036(3) Uani 1 1 d . . . . .
H37 H 0.613060 0.901047 0.384891 0.043 Uiso 1 1 calc R U . . .
C35 C 0.6780(6) 0.2353(6) 0.4102(6) 0.033(2) Uani 1 1 d . . . . .
H35A H 0.648667 0.215458 0.447327 0.039 Uiso 1 1 calc R U . . .
H35B H 0.680726 0.192736 0.372812 0.039 Uiso 1 1 calc R U . . .
C9 C 0.8433(7) 0.8341(6) 0.3711(6) 0.035(3) Uani 1 1 d . . . . .
H9 H 0.851838 0.871749 0.330563 0.042 Uiso 1 1 calc R U . . .
C34 C 0.7598(7) 0.2573(6) 0.4549(7) 0.039(3) Uani 1 1 d . . . . .
H34A H 0.791170 0.271182 0.417437 0.046 Uiso 1 1 calc R U . . .
H34B H 0.785258 0.211955 0.486267 0.046 Uiso 1 1 calc R U . . .
C1 C 0.3172(7) 0.6934(6) 0.2628(6) 0.034(2) Uani 1 1 d . . . . .
H1A H 0.264369 0.712674 0.237162 0.052 Uiso 1 1 calc R U . . .
H1B H 0.325993 0.697556 0.319939 0.052 Uiso 1 1 calc R U . . .
H1C H 0.321851 0.638595 0.248353 0.052 Uiso 1 1 calc R U . . .
C25 C 0.6981(6) 0.5891(6) 0.6716(5) 0.030(2) Uani 1 1 d . . . . .
H25A H 0.730136 0.634669 0.663954 0.036 Uiso 1 1 calc R U . . .
H25B H 0.699458 0.549910 0.630544 0.036 Uiso 1 1 calc R U . . .
C10 C 0.8593(7) 0.8765(7) 0.4495(6) 0.040(3) Uani 1 1 d . . . . .
H10A H 0.822654 0.921222 0.445399 0.047 Uiso 1 1 calc R U . . .
H10B H 0.850349 0.840470 0.490339 0.047 Uiso 1 1 calc R U . . .
C39 C 0.6261(8) 0.9724(7) 0.5586(8) 0.054(4) Uani 1 1 d . . . . .
H39 H 0.611794 1.015983 0.585376 0.065 Uiso 1 1 calc R U . . .
C43 C 0.7025(8) 0.5823(6) 0.1802(6) 0.042(3) Uani 1 1 d . . . . .
H43 H 0.673360 0.580160 0.126778 0.051 Uiso 1 1 calc R U . . .
C32 C 0.7143(7) 0.3961(6) 0.4639(6) 0.036(3) Uani 1 1 d . . . . .
H32A H 0.712304 0.439308 0.500878 0.043 Uiso 1 1 calc R U . . .
H32B H 0.742514 0.415244 0.425525 0.043 Uiso 1 1 calc R U . . .
C33 C 0.7587(8) 0.3264(7) 0.5093(7) 0.051(3) Uani 1 1 d . . . . .
H33A H 0.813380 0.342250 0.534983 0.061 Uiso 1 1 calc R U . . .
H33B H 0.733145 0.310446 0.550909 0.061 Uiso 1 1 calc R U . . .
C46 C 0.7790(8) 0.5880(6) 0.3340(7) 0.043(3) Uani 1 1 d . . . . .
H46 H 0.805024 0.588325 0.388423 0.052 Uiso 1 1 calc R U . . .
C23 C 0.7287(7) 0.6091(6) 0.8182(6) 0.037(3) Uani 1 1 d . . . . .
H23A H 0.749041 0.582553 0.869352 0.044 Uiso 1 1 calc R U . . .
H23B H 0.762863 0.654762 0.816458 0.044 Uiso 1 1 calc R U . . .
C40 C 0.6679(8) 0.9103(7) 0.5992(8) 0.049(3) Uani 1 1 d . . . . .
H40 H 0.684085 0.910933 0.654968 0.059 Uiso 1 1 calc R U . . .
C14 C 0.8985(7) 0.7662(7) 0.3745(7) 0.043(3) Uani 1 1 d . . . . .
H14A H 0.888069 0.740811 0.322336 0.051 Uiso 1 1 calc R U . . .
H14B H 0.889366 0.726987 0.412710 0.051 Uiso 1 1 calc R U . . .
C11 C 0.9433(9) 0.9061(9) 0.4727(7) 0.058(4) Uani 1 1 d . . . . .
H11A H 0.951115 0.945176 0.433909 0.070 Uiso 1 1 calc R U . . .
H11B H 0.953566 0.932027 0.524651 0.070 Uiso 1 1 calc R U . . .
C24 C 0.7325(7) 0.5534(7) 0.7530(6) 0.037(3) Uani 1 1 d . . . . .
H24A H 0.703187 0.505172 0.758307 0.045 Uiso 1 1 calc R U . . .
H24B H 0.788028 0.538758 0.757863 0.045 Uiso 1 1 calc R U . . .
C44 C 0.7731(10) 0.5408(7) 0.2070(7) 0.055(4) Uani 1 1 d . . . . .
H44 H 0.794207 0.511314 0.171434 0.066 Uiso 1 1 calc R U . . .
C38 C 0.6058(8) 0.9686(7) 0.4765(7) 0.047(3) Uani 1 1 d . . . . .
H38 H 0.578010 1.010390 0.445891 0.056 Uiso 1 1 calc R U . . .
C45 C 0.8113(9) 0.5435(7) 0.2856(8) 0.057(4) Uani 1 1 d . . . . .
H45 H 0.858655 0.515235 0.305590 0.068 Uiso 1 1 calc R U . . .
C12 C 1.0002(9) 0.8394(11) 0.4766(8) 0.071(5) Uani 1 1 d . . . . .
H12A H 0.996379 0.803504 0.519590 0.085 Uiso 1 1 calc R U . . .
H12B H 1.054478 0.860385 0.488822 0.085 Uiso 1 1 calc R U . . .
C13 C 0.9838(8) 0.7937(9) 0.3991(7) 0.060(4) Uani 1 1 d . . . . .
H13A H 0.994825 0.827471 0.357428 0.072 Uiso 1 1 calc R U . . .
H13B H 1.019258 0.747753 0.405392 0.072 Uiso 1 1 calc R U . . .
O1 O 0.6558(4) 0.5975(3) 0.4565(3) 0.0185(13) Uani 1 1 d . . . . .
N9 N 1.0190(8) 0.4495(7) 0.7956(8) 0.087(4) Uani 1 1 d D U . . .
C47 C 0.9847(8) 0.5144(8) 0.7609(7) 0.074(4) Uani 1 1 d D U . . .
H47 H 1.008518 0.563417 0.777949 0.088 Uiso 1 1 calc R U . . .
C48 C 0.9171(7) 0.5136(6) 0.7022(7) 0.060(3) Uani 1 1 d D U . . .
H48 H 0.895614 0.561077 0.677743 0.072 Uiso 1 1 calc R U . . .
C49 C 0.8805(8) 0.4440(6) 0.6790(7) 0.064(4) Uani 1 1 d D U . . .
H49 H 0.832150 0.442492 0.639803 0.076 Uiso 1 1 calc R U . . .
C50 C 0.9145(9) 0.3764(7) 0.7130(8) 0.079(4) Uani 1 1 d D U . . .
H50 H 0.890585 0.327158 0.697400 0.094 Uiso 1 1 calc R U . . .
C51 C 0.9838(9) 0.3811(8) 0.7702(9) 0.085(5) Uani 1 1 d D U . . .
H51 H 1.008032 0.333939 0.792803 0.101 Uiso 1 1 calc R U . . .
N10 N 1.029(4) 0.436(2) 0.503(3) 0.066(9) Uani 0.5 1 d D U P A -1
C56 C 1.076(4) 0.495(2) 0.493(3) 0.051(8) Uani 0.5 1 d D U P A -1
H56 H 1.127587 0.484063 0.487233 0.061 Uiso 0.5 1 calc R U P A -1
C55 C 1.051(4) 0.570(3) 0.492(3) 0.055(9) Uani 0.5 1 d D U P A -1
H55 H 1.084886 0.611785 0.484410 0.066 Uiso 0.5 1 calc R U P A -1
C54 C 0.978(4) 0.587(3) 0.500(4) 0.060(10) Uani 0.5 1 d D U P A -1
H54 H 0.960618 0.639448 0.500021 0.072 Uiso 0.5 1 calc R U P A -1
C53 C 0.930(4) 0.526(3) 0.510(4) 0.066(11) Uani 0.5 1 d D U P A -1
H53 H 0.879112 0.536495 0.515163 0.079 Uiso 0.5 1 calc R U P A -1
C52 C 0.957(4) 0.451(3) 0.511(3) 0.060(10) Uani 0.5 1 d D U P A -1
H52 H 0.923686 0.408984 0.516801 0.073 Uiso 0.5 1 calc R U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 U1 3.4461(6) 3_666 ?
U1 O2 1.941(6) . ?
U1 O2 2.322(5) 3_666 ?
U1 N5 2.446(7) . ?
U1 N4 2.593(7) . ?
U1 N6 2.557(7) . ?
U1 N3 2.508(7) . ?
U1 O1 1.899(6) . ?
Dy1 Cl1 2.635(3) . ?
Dy1 N3 2.776(8) . ?
Dy1 N1 2.391(8) . ?
Dy1 N8 2.482(8) . ?
Dy1 N7 2.508(8) . ?
Dy1 N2 2.593(8) . ?
Dy1 O1 2.245(6) . ?
N5 C26 1.355(11) . ?
N5 C29 1.389(10) . ?
N4 C19 1.278(11) . ?
N4 C20 1.466(10) . ?
N6 C31 1.499(11) . ?
N6 C30 1.273(11) . ?
N3 C18 1.391(10) . ?
N3 C15 1.366(11) . ?
C26 C3 1.531(12) . ?
C26 C27 1.395(12) . ?
N1 C4 1.359(12) . ?
N1 C7 1.389(12) . ?
N8 C42 1.344(13) . ?
N8 C46 1.338(15) . ?
N7 C41 1.350(12) . ?
N7 C37 1.324(13) . ?
C29 C30 1.429(12) . ?
C29 C28 1.391(12) . ?
C19 H19 0.9500 . ?
C19 C18 1.436(12) . ?
C31 H31 1.0000 . ?
C31 C36 1.524(12) . ?
C31 C32 1.528(14) . ?
C3 C4 1.523(13) . ?
C3 C2 1.545(13) . ?
C3 C15 1.514(11) . ?
C30 H30 0.9500 . ?
C18 C17 1.375(13) . ?
N2 C8 1.324(13) . ?
N2 C9 1.464(14) . ?
C4 C5 1.383(13) . ?
C7 C6 1.378(14) . ?
C7 C8 1.387(14) . ?
C17 H17 0.9500 . ?
C17 C16 1.387(13) . ?
C27 H27 0.9500 . ?
C27 C28 1.373(13) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.537(14) . ?
C20 H20 1.0000 . ?
C20 C21 1.520(11) . ?
C20 C25 1.531(14) . ?
C16 H16 0.9500 . ?
C16 C15 1.396(12) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C35 1.514(13) . ?
C6 H6 0.9500 . ?
C6 C5 1.420(15) . ?
C28 H28 0.9500 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.531(13) . ?
C5 H5 0.9500 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.496(15) . ?
C41 H41 0.9500 . ?
C41 C40 1.373(15) . ?
C42 H42 0.9500 . ?
C42 C43 1.353(14) . ?
C8 H8 0.9500 . ?
C37 H37 0.9500 . ?
C37 C38 1.386(15) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C34 1.501(16) . ?
C9 H9 1.0000 . ?
C9 C10 1.521(14) . ?
C9 C14 1.504(17) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C33 1.523(15) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C24 1.532(13) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.516(17) . ?
C39 H39 0.9500 . ?
C39 C40 1.382(18) . ?
C39 C38 1.399(17) . ?
C43 H43 0.9500 . ?
C43 C44 1.403(19) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.533(14) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C46 H46 0.9500 . ?
C46 C45 1.369(15) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.505(15) . ?
C40 H40 0.9500 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C13 1.526(17) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.51(2) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C44 H44 0.9500 . ?
C44 C45 1.376(18) . ?
C38 H38 0.9500 . ?
C45 H45 0.9500 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.536(19) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
N9 C47 1.333(12) . ?
N9 C51 1.344(12) . ?
C47 H47 0.9500 . ?
C47 C48 1.363(11) . ?
C48 H48 0.9500 . ?
C48 C49 1.365(10) . ?
C49 H49 0.9500 . ?
C49 C50 1.366(10) . ?
C50 H50 0.9500 . ?
C50 C51 1.371(11) . ?
C51 H51 0.9500 . ?
N10 C56 1.342(14) . ?
N10 C52 1.341(14) . ?
C56 H56 0.9500 . ?
C56 C55 1.359(12) . ?
C55 H55 0.9500 . ?
C55 C54 1.363(12) . ?
C54 H54 0.9500 . ?
C54 C53 1.367(12) . ?
C53 H53 0.9500 . ?
C53 C52 1.365(12) . ?
C52 H52 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U1 U1 32.49(16) 3_666 3_666 ?
O2 U1 U1 39.99(16) . 3_666 ?
O2 U1 O2 72.5(3) . 3_666 ?
O2 U1 N5 90.8(2) . . ?
O2 U1 N5 141.3(2) 3_666 . ?
O2 U1 N4 79.4(2) 3_666 . ?
O2 U1 N4 96.7(2) . . ?
O2 U1 N6 79.1(2) 3_666 . ?
O2 U1 N6 97.8(2) . . ?
O2 U1 N3 94.3(2) . . ?
O2 U1 N3 143.6(2) 3_666 . ?
N5 U1 U1 122.29(17) . 3_666 ?
N5 U1 N4 138.3(2) . . ?
N5 U1 N6 68.7(2) . . ?
N5 U1 N3 70.2(2) . . ?
N4 U1 U1 86.68(16) . 3_666 ?
N6 U1 U1 87.07(16) . 3_666 ?
N6 U1 N4 148.9(2) . . ?
N3 U1 U1 125.73(17) . 3_666 ?
N3 U1 N4 68.4(2) . . ?
N3 U1 N6 137.2(2) . . ?
O1 U1 U1 144.99(18) . 3_666 ?
O1 U1 O2 174.6(2) . . ?
O1 U1 O2 112.5(2) . 3_666 ?
O1 U1 N5 86.2(2) . . ?
O1 U1 N4 82.6(2) . . ?
O1 U1 N6 85.3(2) . . ?
O1 U1 N3 80.5(2) . . ?
Cl1 Dy1 N3 124.37(17) . . ?
N1 Dy1 Cl1 154.70(19) . . ?
N1 Dy1 N3 76.3(2) . . ?
N1 Dy1 N8 81.1(3) . . ?
N1 Dy1 N7 86.7(3) . . ?
N1 Dy1 N2 69.2(3) . . ?
N8 Dy1 Cl1 98.1(2) . . ?
N8 Dy1 N3 118.2(3) . . ?
N8 Dy1 N7 155.6(3) . . ?
N8 Dy1 N2 76.9(2) . . ?
N7 Dy1 Cl1 84.0(2) . . ?
N7 Dy1 N3 78.7(2) . . ?
N7 Dy1 N2 79.0(2) . . ?
N2 Dy1 Cl1 85.9(2) . . ?
N2 Dy1 N3 139.7(3) . . ?
O1 Dy1 Cl1 78.28(16) . . ?
O1 Dy1 N3 69.2(2) . . ?
O1 Dy1 N1 125.9(2) . . ?
O1 Dy1 N8 80.1(2) . . ?
O1 Dy1 N7 123.9(2) . . ?
O1 Dy1 N2 149.8(2) . . ?
U1 O2 U1 107.5(3) . 3_666 ?
C26 N5 U1 138.4(6) . . ?
C26 N5 C29 106.0(7) . . ?
C29 N5 U1 113.7(5) . . ?
C19 N4 U1 112.6(5) . . ?
C19 N4 C20 121.2(7) . . ?
C20 N4 U1 126.0(5) . . ?
C31 N6 U1 125.4(5) . . ?
C30 N6 U1 113.8(6) . . ?
C30 N6 C31 120.6(7) . . ?
U1 N3 Dy1 86.5(2) . . ?
C18 N3 U1 111.5(5) . . ?
C18 N3 Dy1 109.2(6) . . ?
C15 N3 U1 132.9(6) . . ?
C15 N3 Dy1 107.6(5) . . ?
C15 N3 C18 105.7(7) . . ?
N5 C26 C3 125.2(8) . . ?
N5 C26 C27 110.0(8) . . ?
C27 C26 C3 124.5(8) . . ?
C4 N1 Dy1 136.3(6) . . ?
C4 N1 C7 106.5(8) . . ?
C7 N1 Dy1 115.9(6) . . ?
C42 N8 Dy1 127.7(7) . . ?
C46 N8 Dy1 117.5(7) . . ?
C46 N8 C42 114.7(9) . . ?
C41 N7 Dy1 121.7(7) . . ?
C37 N7 Dy1 121.4(7) . . ?
C37 N7 C41 116.1(9) . . ?
N5 C29 C30 121.1(7) . . ?
N5 C29 C28 109.9(8) . . ?
C28 C29 C30 129.0(8) . . ?
N4 C19 H19 118.5 . . ?
N4 C19 C18 123.1(7) . . ?
C18 C19 H19 118.5 . . ?
N6 C31 H31 107.5 . . ?
N6 C31 C36 115.6(7) . . ?
N6 C31 C32 109.5(7) . . ?
C36 C31 H31 107.5 . . ?
C36 C31 C32 109.0(8) . . ?
C32 C31 H31 107.5 . . ?
C26 C3 C2 107.8(7) . . ?
C4 C3 C26 104.5(7) . . ?
C4 C3 C2 111.1(7) . . ?
C15 C3 C26 116.9(7) . . ?
C15 C3 C4 107.3(7) . . ?
C15 C3 C2 109.2(7) . . ?
N6 C30 C29 122.0(7) . . ?
N6 C30 H30 119.0 . . ?
C29 C30 H30 119.0 . . ?
N3 C18 C19 121.4(8) . . ?
C17 C18 N3 110.6(8) . . ?
C17 C18 C19 127.5(8) . . ?
C8 N2 Dy1 109.3(7) . . ?
C8 N2 C9 116.5(8) . . ?
C9 N2 Dy1 134.2(6) . . ?
N1 C4 C3 119.3(8) . . ?
N1 C4 C5 111.0(9) . . ?
C5 C4 C3 129.6(9) . . ?
C6 C7 N1 109.6(9) . . ?
C6 C7 C8 130.6(9) . . ?
C8 C7 N1 119.8(9) . . ?
C18 C17 H17 126.8 . . ?
C18 C17 C16 106.5(8) . . ?
C16 C17 H17 126.8 . . ?
C26 C27 H27 126.1 . . ?
C28 C27 C26 107.7(8) . . ?
C28 C27 H27 126.1 . . ?
C3 C2 H2A 109.0 . . ?
C3 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C1 C2 C3 112.9(8) . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
N4 C20 H20 107.3 . . ?
N4 C20 C21 115.8(7) . . ?
N4 C20 C25 109.2(7) . . ?
C21 C20 H20 107.3 . . ?
C21 C20 C25 109.6(8) . . ?
C25 C20 H20 107.3 . . ?
C17 C16 H16 126.2 . . ?
C17 C16 C15 107.6(8) . . ?
C15 C16 H16 126.2 . . ?
N3 C15 C3 125.2(7) . . ?
N3 C15 C16 109.6(7) . . ?
C16 C15 C3 124.9(8) . . ?
C31 C36 H36A 109.4 . . ?
C31 C36 H36B 109.4 . . ?
H36A C36 H36B 108.0 . . ?
C35 C36 C31 111.1(8) . . ?
C35 C36 H36A 109.4 . . ?
C35 C36 H36B 109.4 . . ?
C7 C6 H6 126.5 . . ?
C7 C6 C5 107.1(8) . . ?
C5 C6 H6 126.5 . . ?
C29 C28 H28 126.8 . . ?
C27 C28 C29 106.4(8) . . ?
C27 C28 H28 126.8 . . ?
C20 C21 H21A 109.0 . . ?
C20 C21 H21B 109.0 . . ?
C20 C21 C22 113.0(8) . . ?
H21A C21 H21B 107.8 . . ?
C22 C21 H21A 109.0 . . ?
C22 C21 H21B 109.0 . . ?
C4 C5 C6 105.8(9) . . ?
C4 C5 H5 127.1 . . ?
C6 C5 H5 127.1 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
C23 C22 C21 110.5(8) . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
N7 C41 H41 118.0 . . ?
N7 C41 C40 124.1(11) . . ?
C40 C41 H41 118.0 . . ?
N8 C42 H42 117.0 . . ?
N8 C42 C43 126.1(12) . . ?
C43 C42 H42 117.0 . . ?
N2 C8 C7 124.7(9) . . ?
N2 C8 H8 117.6 . . ?
C7 C8 H8 117.6 . . ?
N7 C37 H37 117.8 . . ?
N7 C37 C38 124.4(10) . . ?
C38 C37 H37 117.8 . . ?
C36 C35 H35A 109.4 . . ?
C36 C35 H35B 109.4 . . ?
H35A C35 H35B 108.0 . . ?
C34 C35 C36 111.4(8) . . ?
C34 C35 H35A 109.4 . . ?
C34 C35 H35B 109.4 . . ?
N2 C9 H9 108.2 . . ?
N2 C9 C10 110.1(9) . . ?
N2 C9 C14 110.7(9) . . ?
C10 C9 H9 108.2 . . ?
C14 C9 H9 108.2 . . ?
C14 C9 C10 111.3(10) . . ?
C35 C34 H34A 109.4 . . ?
C35 C34 H34B 109.4 . . ?
C35 C34 C33 111.1(9) . . ?
H34A C34 H34B 108.0 . . ?
C33 C34 H34A 109.4 . . ?
C33 C34 H34B 109.4 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C20 C25 H25A 109.7 . . ?
C20 C25 H25B 109.7 . . ?
C20 C25 C24 109.8(8) . . ?
H25A C25 H25B 108.2 . . ?
C24 C25 H25A 109.7 . . ?
C24 C25 H25B 109.7 . . ?
C9 C10 H10A 109.6 . . ?
C9 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
C11 C10 C9 110.3(10) . . ?
C11 C10 H10A 109.6 . . ?
C11 C10 H10B 109.6 . . ?
C40 C39 H39 121.2 . . ?
C40 C39 C38 117.6(10) . . ?
C38 C39 H39 121.2 . . ?
C42 C43 H43 121.5 . . ?
C42 C43 C44 117.0(11) . . ?
C44 C43 H43 121.5 . . ?
C31 C32 H32A 109.6 . . ?
C31 C32 H32B 109.6 . . ?
C31 C32 C33 110.5(9) . . ?
H32A C32 H32B 108.1 . . ?
C33 C32 H32A 109.6 . . ?
C33 C32 H32B 109.6 . . ?
C34 C33 C32 111.1(9) . . ?
C34 C33 H33A 109.4 . . ?
C34 C33 H33B 109.4 . . ?
C32 C33 H33A 109.4 . . ?
C32 C33 H33B 109.4 . . ?
H33A C33 H33B 108.0 . . ?
N8 C46 H46 117.5 . . ?
N8 C46 C45 124.9(12) . . ?
C45 C46 H46 117.5 . . ?
C22 C23 H23A 109.2 . . ?
C22 C23 H23B 109.2 . . ?
C22 C23 C24 112.0(9) . . ?
H23A C23 H23B 107.9 . . ?
C24 C23 H23A 109.2 . . ?
C24 C23 H23B 109.2 . . ?
C41 C40 C39 119.3(11) . . ?
C41 C40 H40 120.4 . . ?
C39 C40 H40 120.4 . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
C9 C14 C13 110.6(11) . . ?
H14A C14 H14B 108.1 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
C12 C11 C10 110.6(11) . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C25 C24 H24A 109.2 . . ?
C25 C24 H24B 109.2 . . ?
C23 C24 C25 112.2(9) . . ?
C23 C24 H24A 109.2 . . ?
C23 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
C43 C44 H44 120.5 . . ?
C45 C44 C43 119.0(11) . . ?
C45 C44 H44 120.5 . . ?
C37 C38 C39 118.6(11) . . ?
C37 C38 H38 120.7 . . ?
C39 C38 H38 120.7 . . ?
C46 C45 C44 118.1(13) . . ?
C46 C45 H45 120.9 . . ?
C44 C45 H45 120.9 . . ?
C11 C12 H12A 109.2 . . ?
C11 C12 H12B 109.2 . . ?
C11 C12 C13 111.9(12) . . ?
H12A C12 H12B 107.9 . . ?
C13 C12 H12A 109.2 . . ?
C13 C12 H12B 109.2 . . ?
C14 C13 C12 110.9(11) . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 108.0 . . ?
U1 O1 Dy1 121.9(3) . . ?
C47 N9 C51 117.0(13) . . ?
N9 C47 H47 118.5 . . ?
N9 C47 C48 123.0(12) . . ?
C48 C47 H47 118.5 . . ?
C47 C48 H48 120.4 . . ?
C47 C48 C49 119.3(11) . . ?
C49 C48 H48 120.4 . . ?
C48 C49 H49 120.5 . . ?
C48 C49 C50 119.0(11) . . ?
C50 C49 H49 120.5 . . ?
C49 C50 H50 120.6 . . ?
C49 C50 C51 118.7(11) . . ?
C51 C50 H50 120.6 . . ?
N9 C51 C50 122.8(12) . . ?
N9 C51 H51 118.6 . . ?
C50 C51 H51 118.6 . . ?
C52 N10 C56 120.1(19) . . ?
N10 C56 H56 119.8 . . ?
N10 C56 C55 120.4(16) . . ?
C55 C56 H56 119.8 . . ?
C56 C55 H55 119.9 . . ?
C56 C55 C54 120.3(14) . . ?
C54 C55 H55 119.9 . . ?
C55 C54 H54 120.6 . . ?
C55 C54 C53 118.8(13) . . ?
C53 C54 H54 120.6 . . ?
C54 C53 H53 120.1 . . ?
C52 C53 C54 119.8(14) . . ?
C52 C53 H53 120.1 . . ?
N10 C52 C53 120.5(17) . . ?
N10 C52 H52 119.7 . . ?
C53 C52 H52 119.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 U1 O1 Dy1 -155.78(12) 3_666 . . . ?
U1 N5 C26 C3 24.7(15) . . . . ?
U1 N5 C26 C27 -162.5(7) . . . . ?
U1 N5 C29 C30 -10.2(11) . . . . ?
U1 N5 C29 C28 168.2(6) . . . . ?
U1 N4 C19 C18 -5.2(11) . . . . ?
U1 N4 C20 C21 -170.7(6) . . . . ?
U1 N4 C20 C25 65.0(9) . . . . ?
U1 N6 C31 C36 173.2(6) . . . . ?
U1 N6 C31 C32 -63.2(9) . . . . ?
U1 N6 C30 C29 0.2(11) . . . . ?
U1 N3 C18 C19 19.2(10) . . . . ?
U1 N3 C18 C17 -153.3(6) . . . . ?
U1 N3 C15 C3 -40.8(13) . . . . ?
U1 N3 C15 C16 144.2(7) . . . . ?
Dy1 N3 C18 C19 -74.8(9) . . . . ?
Dy1 N3 C18 C17 112.8(7) . . . . ?
Dy1 N3 C15 C3 61.2(9) . . . . ?
Dy1 N3 C15 C16 -113.8(7) . . . . ?
Dy1 N1 C4 C3 10.8(12) . . . . ?
Dy1 N1 C4 C5 -165.4(6) . . . . ?
Dy1 N1 C7 C6 169.3(6) . . . . ?
Dy1 N1 C7 C8 -10.8(11) . . . . ?
Dy1 N8 C42 C43 175.5(8) . . . . ?
Dy1 N8 C46 C45 -174.2(10) . . . . ?
Dy1 N7 C41 C40 -167.8(9) . . . . ?
Dy1 N7 C37 C38 167.7(9) . . . . ?
Dy1 N2 C8 C7 3.5(12) . . . . ?
Dy1 N2 C9 C10 -59.6(12) . . . . ?
Dy1 N2 C9 C14 63.8(11) . . . . ?
O2 U1 O1 Dy1 -157.7(3) 3_666 . . . ?
N5 U1 O1 Dy1 57.3(3) . . . . ?
N5 C26 C3 C4 102.1(10) . . . . ?
N5 C26 C3 C2 -139.6(9) . . . . ?
N5 C26 C3 C15 -16.2(14) . . . . ?
N5 C26 C27 C28 -0.8(12) . . . . ?
N5 C29 C30 N6 7.0(14) . . . . ?
N5 C29 C28 C27 -1.3(12) . . . . ?
N4 U1 O1 Dy1 -82.5(3) . . . . ?
N4 C19 C18 N3 -9.9(14) . . . . ?
N4 C19 C18 C17 161.2(10) . . . . ?
N4 C20 C21 C22 179.8(8) . . . . ?
N4 C20 C25 C24 -176.3(8) . . . . ?
N6 U1 O1 Dy1 126.2(3) . . . . ?
N6 C31 C36 C35 -177.5(8) . . . . ?
N6 C31 C32 C33 174.7(8) . . . . ?
N3 U1 O1 Dy1 -13.3(3) . . . . ?
N3 C18 C17 C16 1.6(11) . . . . ?
C26 N5 C29 C30 -177.6(9) . . . . ?
C26 N5 C29 C28 0.9(11) . . . . ?
C26 C3 C4 N1 -81.6(9) . . . . ?
C26 C3 C4 C5 93.9(11) . . . . ?
C26 C3 C2 C1 63.1(9) . . . . ?
C26 C3 C15 N3 25.1(13) . . . . ?
C26 C3 C15 C16 -160.7(9) . . . . ?
C26 C27 C28 C29 1.3(12) . . . . ?
N1 C4 C5 C6 -0.9(11) . . . . ?
N1 C7 C6 C5 -0.7(11) . . . . ?
N1 C7 C8 N2 4.6(15) . . . . ?
N8 C42 C43 C44 -1.5(18) . . . . ?
N8 C46 C45 C44 -2(2) . . . . ?
N7 C41 C40 C39 -0.1(19) . . . . ?
N7 C37 C38 C39 0.4(19) . . . . ?
C29 N5 C26 C3 -172.9(9) . . . . ?
C29 N5 C26 C27 -0.1(11) . . . . ?
C19 N4 C20 C21 3.6(13) . . . . ?
C19 N4 C20 C25 -120.7(9) . . . . ?
C19 C18 C17 C16 -170.3(9) . . . . ?
C31 N6 C30 C29 -175.4(8) . . . . ?
C31 C36 C35 C34 -57.8(11) . . . . ?
C31 C32 C33 C34 56.6(14) . . . . ?
C3 C26 C27 C28 172.2(9) . . . . ?
C3 C4 C5 C6 -176.6(9) . . . . ?
C30 N6 C31 C36 -11.7(12) . . . . ?
C30 N6 C31 C32 111.9(10) . . . . ?
C30 C29 C28 C27 176.9(10) . . . . ?
C18 N3 C15 C3 177.8(8) . . . . ?
C18 N3 C15 C16 2.8(10) . . . . ?
C18 C17 C16 C15 0.2(11) . . . . ?
N2 C9 C10 C11 -178.3(10) . . . . ?
N2 C9 C14 C13 -179.9(8) . . . . ?
C4 N1 C7 C6 0.1(10) . . . . ?
C4 N1 C7 C8 180.0(9) . . . . ?
C4 C3 C2 C1 177.0(7) . . . . ?
C4 C3 C15 N3 -91.8(10) . . . . ?
C4 C3 C15 C16 82.4(11) . . . . ?
C7 N1 C4 C3 176.7(7) . . . . ?
C7 N1 C4 C5 0.5(10) . . . . ?
C7 C6 C5 C4 0.9(11) . . . . ?
C17 C16 C15 N3 -1.9(11) . . . . ?
C17 C16 C15 C3 -176.9(9) . . . . ?
C27 C26 C3 C4 -69.7(12) . . . . ?
C27 C26 C3 C2 48.5(12) . . . . ?
C27 C26 C3 C15 171.9(9) . . . . ?
C2 C3 C4 N1 162.5(8) . . . . ?
C2 C3 C4 C5 -22.1(13) . . . . ?
C2 C3 C15 N3 147.7(8) . . . . ?
C2 C3 C15 C16 -38.1(12) . . . . ?
C20 N4 C19 C18 179.8(8) . . . . ?
C20 C21 C22 C23 54.7(12) . . . . ?
C20 C25 C24 C23 -56.7(12) . . . . ?
C15 N3 C18 C19 169.7(8) . . . . ?
C15 N3 C18 C17 -2.8(10) . . . . ?
C15 C3 C4 N1 43.1(10) . . . . ?
C15 C3 C4 C5 -141.4(10) . . . . ?
C15 C3 C2 C1 -64.8(9) . . . . ?
C36 C31 C32 C33 -57.9(11) . . . . ?
C36 C35 C34 C33 55.2(12) . . . . ?
C6 C7 C8 N2 -175.7(10) . . . . ?
C28 C29 C30 N6 -171.1(10) . . . . ?
C21 C20 C25 C24 55.8(10) . . . . ?
C21 C22 C23 C24 -53.5(12) . . . . ?
C22 C23 C24 C25 56.0(13) . . . . ?
C41 N7 C37 C38 -1.9(17) . . . . ?
C42 N8 C46 C45 2.8(17) . . . . ?
C42 C43 C44 C45 2.6(19) . . . . ?
C8 N2 C9 C10 121.4(9) . . . . ?
C8 N2 C9 C14 -115.2(10) . . . . ?
C8 C7 C6 C5 179.5(10) . . . . ?
C37 N7 C41 C40 1.8(16) . . . . ?
C35 C34 C33 C32 -54.8(14) . . . . ?
C9 N2 C8 C7 -177.3(9) . . . . ?
C9 C10 C11 C12 -57.3(13) . . . . ?
C9 C14 C13 C12 54.4(14) . . . . ?
C25 C20 C21 C22 -56.1(11) . . . . ?
C10 C9 C14 C13 -57.2(12) . . . . ?
C10 C11 C12 C13 55.6(13) . . . . ?
C43 C44 C45 C46 -1(2) . . . . ?
C32 C31 C36 C35 58.6(10) . . . . ?
C46 N8 C42 C43 -1.1(16) . . . . ?
C40 C39 C38 C37 1.3(19) . . . . ?
C14 C9 C10 C11 58.6(12) . . . . ?
C11 C12 C13 C14 -54.2(15) . . . . ?
C38 C39 C40 C41 -1(2) . . . . ?
N9 C47 C48 C49 2.4(15) . . . . ?
C47 N9 C51 C50 -2(2) . . . . ?
C47 C48 C49 C50 -2.7(19) . . . . ?
C48 C49 C50 C51 1(2) . . . . ?
C49 C50 C51 N9 2(3) . . . . ?
C51 N9 C47 C48 0.0(16) . . . . ?
N10 C56 C55 C54 0(2) . . . . ?
C56 N10 C52 C53 -1(5) . . . . ?
C56 C55 C54 C53 -1(5) . . . . ?
C55 C54 C53 C52 1(5) . . . . ?
C54 C53 C52 N10 0(5) . . . . ?
C52 N10 C56 C55 1(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.338
_oxdiff_exptl_absorpt_empirical_full_min 0.837
_vrf_PLAT029_to499_mp_221123     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.954 Why?  
RESPONSE: The initial unit cell parameters indexed as C-centred orthorhombic and 
a data collection strategy was planned using this unit cell. The crystal had 
been removed from the diffractometer, and decomposed, before the correct 
monoclinic unit cell was identified. There is thus a missing unique portion
 of the monoclinic data set. However, the model refines well against the 
measured data set with a data/parameter ratio of 15.4.
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Pyridene, hexane'
_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_to516_refinalised
_database_code_depnum_ccdc_archive 'CCDC 2313505'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2023-12-11 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_audit_creation_date             2023-11-24
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C92 H114 Cl2 N16 O4 Sm2 U2'
_chemical_formula_sum            'C92 H114 Cl2 N16 O4 Sm2 U2'
_chemical_formula_weight         2355.65
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C72 H94 N12 U2 O4 Sm2 Cl2'
_chemical_oxdiff_usercomment     pyridine/hexane
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   17.5417(2)
_cell_length_b                   17.1342(2)
_cell_length_c                   17.6710(2)
_cell_angle_alpha                90
_cell_angle_beta                 104.5910(10)
_cell_angle_gamma                90
_cell_volume                     5139.95(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    45983
_cell_measurement_temperature    120.1(3)
_cell_measurement_theta_max      29.3130
_cell_measurement_theta_min      3.6640
_shelx_estimated_absorpt_T_max   0.831
_shelx_estimated_absorpt_T_min   0.393
_exptl_absorpt_coefficient_mu    4.371
_exptl_absorpt_correction_T_max  0.756
_exptl_absorpt_correction_T_min  0.363
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             2304
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-23 -8 9 0.0998
0 -21 12 0.0531
23 9 -10 0.0946
0 21 -12 0.0669
0 16 18 0.0049
0 -16 -18 0.0393

_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.044
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-23.1857 -7.6622 9.3388 0.0403 -0.4988 0.8658
-0.1658 -20.8127 12.2470 0.0778 -0.9835 -0.1633
22.5010 9.0521 -10.0113 -0.0451 0.5604 -0.8270
0.3424 20.8147 -12.2850 -0.0779 0.9846 0.1562
0.1212 16.2270 17.8480 0.9586 0.2845 -0.0089
-0.1212 -16.2270 -17.8480 -0.9586 -0.2845 0.0089

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            133748
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.478
_diffrn_reflns_theta_min         3.366
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.1(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -33.00  51.00   1.00   20.00    --  -15.66  60.00-143.00   84
  2  ω    -83.00   2.00   1.00   20.00    --  -15.66 -60.00  76.00   85
  3  ω      0.00  84.00   1.00   20.00    --   17.38  60.00-143.00   84
  4  ω    -50.00  35.00   1.00   20.00    --   17.38 -60.00  76.00   85
  5  ω    -88.00 -39.00   1.00   20.00    --  -15.66-178.00 -90.00   49
  6  ω    -52.00  36.00   1.00   20.00    --   17.38 -38.00 -60.00   88
  7  ω     -9.00  39.00   1.00   20.00    --   17.38  77.00 -60.00   48
  8  ω     -9.00  39.00   1.00   20.00    --   17.38  77.00-180.00   48
  9  ω     -9.00  39.00   1.00   20.00    --   17.38  77.00  60.00   48
 10  ω    -42.00  39.00   1.00   20.00    --  -15.66  77.00-120.00   81
 11  ω      1.00  85.00   1.00   20.00    --   17.38  57.00 -60.00   84
 12  ω    -20.00  55.00   1.00   20.00    --   17.38 -99.00  30.00   75
 13  ω    -20.00  55.00   1.00   20.00    --   17.38 -99.00-180.00   75
 14  ω     -9.00  39.00   1.00   20.00    --   17.38  77.00   0.00   48
 15  ω    -20.00  55.00   1.00   20.00    --   17.38 -99.00 -90.00   75
 16  ω    -52.00  36.00   1.00   20.00    --   17.38 -38.00 120.00   88
 17  ω      1.00  30.00   1.00   20.00    --   17.38  57.00  30.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0072686000
_diffrn_orient_matrix_UB_12      0.0180993000
_diffrn_orient_matrix_UB_13      0.0372064000
_diffrn_orient_matrix_UB_21      0.0022353000
_diffrn_orient_matrix_UB_22      0.0368782000
_diffrn_orient_matrix_UB_23      -0.0176048000
_diffrn_orient_matrix_UB_31      -0.0410802000
_diffrn_orient_matrix_UB_32      0.0052392000
_diffrn_orient_matrix_UB_33      -0.0049846000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11074
_reflns_number_total             13125
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.035
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         13125
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0274
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0231P)²+7.0749P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0561
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C31(H31), C20(H20), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C2(H2A,H2B), C25(H25A,H25B), C14(H14A,H14B), C22(H22A,H22B),
 C32(H32A,H32B), C36(H36A,H36B), C10(H10A,H10B), C23(H23A,H23B), C34(H34A,H34B),
  C33(H33A,H33B), C35(H35A,H35B), C24(H24A,H24B), C11(H11A,H11B), C13(H13A,
 H13B), C12(H12A,H12B)
2.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C30(H30), C17(H17), C16(H16), C42(H42), C27(H27), C28(H28), C6(H6),
 C37(H37), C5(H5), C8(H8), C41(H41), C46(H46), C43(H43), C40(H40), C39(H39),
 C44(H44), C45(H45), C38(H38)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.55356(2) 0.56210(2) 0.45674(2) 0.01066(3) Uani 1 1 d . . . . .
Sm1 Sm 0.67863(2) 0.71732(2) 0.41234(2) 0.01272(4) Uani 1 1 d . . . . .
Cl1 Cl 0.80937(4) 0.69820(5) 0.52824(4) 0.02086(15) Uani 1 1 d . . . . .
N5 N 0.52101(14) 0.58570(14) 0.31568(14) 0.0141(5) Uani 1 1 d . . . . .
N4 N 0.57852(14) 0.64363(14) 0.58388(13) 0.0142(5) Uani 1 1 d . . . . .
N6 N 0.58816(14) 0.44330(14) 0.38470(14) 0.0159(5) Uani 1 1 d . . . . .
N3 N 0.52571(13) 0.70424(14) 0.42887(13) 0.0128(5) Uani 1 1 d . . . . .
N1 N 0.59841(14) 0.77839(14) 0.29508(14) 0.0152(5) Uani 1 1 d . . . . .
N8 N 0.71639(15) 0.63239(15) 0.30906(15) 0.0196(5) Uani 1 1 d . . . . .
C19 C 0.55397(16) 0.71461(17) 0.57246(17) 0.0148(6) Uani 1 1 d . . . . .
H19 H 0.557695 0.747559 0.616474 0.018 Uiso 1 1 calc R U . . .
N7 N 0.66796(15) 0.84585(15) 0.48325(15) 0.0199(5) Uani 1 1 d . . . . .
C31 C 0.63151(17) 0.37319(17) 0.42127(17) 0.0163(6) Uani 1 1 d . . . . .
H31 H 0.604491 0.353715 0.461118 0.020 Uiso 1 1 calc R U . . .
C26 C 0.48119(16) 0.63820(17) 0.26350(16) 0.0141(6) Uani 1 1 d . . . . .
C18 C 0.52134(16) 0.74562(17) 0.49601(16) 0.0140(6) Uani 1 1 d . . . . .
C15 C 0.47731(15) 0.74373(17) 0.36749(16) 0.0129(5) Uani 1 1 d . . . . .
C20 C 0.61341(16) 0.61444(17) 0.66387(16) 0.0152(6) Uani 1 1 d . . . . .
H20 H 0.582861 0.567044 0.671378 0.018 Uiso 1 1 calc R U . . .
N2 N 0.76030(14) 0.81231(15) 0.34653(15) 0.0185(5) Uani 1 1 d . . . . .
C29 C 0.52992(17) 0.51966(17) 0.27234(16) 0.0162(6) Uani 1 1 d . . . . .
C30 C 0.56731(17) 0.45111(17) 0.30952(18) 0.0174(6) Uani 1 1 d . . . . .
H30 H 0.577355 0.409465 0.277878 0.021 Uiso 1 1 calc R U . . .
C3 C 0.46494(16) 0.72260(17) 0.28184(16) 0.0144(6) Uani 1 1 d . . . . .
C17 C 0.47411(17) 0.81019(17) 0.47612(17) 0.0162(6) Uani 1 1 d . . . . .
H17 H 0.462896 0.848276 0.510868 0.019 Uiso 1 1 calc R U . . .
C16 C 0.44588(17) 0.80894(17) 0.39503(18) 0.0178(6) Uani 1 1 d . . . . .
H16 H 0.411330 0.846051 0.364168 0.021 Uiso 1 1 calc R U . . .
C4 C 0.52317(16) 0.77104(17) 0.25021(16) 0.0144(6) Uani 1 1 d . . . . .
C42 C 0.67860(19) 0.6283(2) 0.23340(19) 0.0240(7) Uani 1 1 d . . . . .
H42 H 0.631491 0.657503 0.215387 0.029 Uiso 1 1 calc R U . . .
C7 C 0.63792(17) 0.82060(18) 0.24975(17) 0.0175(6) Uani 1 1 d . . . . .
C27 C 0.46402(18) 0.60728(19) 0.18781(17) 0.0213(7) Uani 1 1 d . . . . .
H27 H 0.436322 0.632708 0.141208 0.026 Uiso 1 1 calc R U . . .
C21 C 0.61041(18) 0.67135(19) 0.72963(17) 0.0199(6) Uani 1 1 d . . . . .
H21A H 0.639523 0.719464 0.723516 0.024 Uiso 1 1 calc R U . . .
H21B H 0.554951 0.685875 0.725866 0.024 Uiso 1 1 calc R U . . .
C2 C 0.37905(16) 0.74222(18) 0.23810(17) 0.0173(6) Uani 1 1 d . . . . .
H2A H 0.368934 0.798083 0.246066 0.021 Uiso 1 1 calc R U . . .
H2B H 0.372377 0.733771 0.181379 0.021 Uiso 1 1 calc R U . . .
C28 C 0.49510(19) 0.53254(19) 0.19374(18) 0.0219(7) Uani 1 1 d . . . . .
H28 H 0.492961 0.496967 0.152019 0.026 Uiso 1 1 calc R U . . .
C6 C 0.58752(18) 0.83867(19) 0.17781(18) 0.0231(7) Uani 1 1 d . . . . .
H6 H 0.600272 0.867125 0.136520 0.028 Uiso 1 1 calc R U . . .
C37 C 0.62875(19) 0.9062(2) 0.4443(2) 0.0261(7) Uani 1 1 d . . . . .
H37 H 0.615479 0.904689 0.388791 0.031 Uiso 1 1 calc R U . . .
C25 C 0.69776(18) 0.5884(2) 0.67059(18) 0.0234(7) Uani 1 1 d . . . . .
H25A H 0.730040 0.633807 0.663105 0.028 Uiso 1 1 calc R U . . .
H25B H 0.698815 0.549591 0.629397 0.028 Uiso 1 1 calc R U . . .
C9 C 0.84313(18) 0.8381(2) 0.37088(18) 0.0226(7) Uani 1 1 d . . . . .
H9 H 0.852121 0.875759 0.330734 0.027 Uiso 1 1 calc R U . . .
C5 C 0.51435(19) 0.80674(19) 0.17816(18) 0.0223(7) Uani 1 1 d . . . . .
H5 H 0.467615 0.809044 0.136988 0.027 Uiso 1 1 calc R U . . .
C8 C 0.71924(18) 0.83799(18) 0.27974(17) 0.0181(6) Uani 1 1 d . . . . .
H8 H 0.744553 0.869867 0.249423 0.022 Uiso 1 1 calc R U . . .
C14 C 0.8591(2) 0.8810(2) 0.44902(19) 0.0306(8) Uani 1 1 d . . . . .
H14A H 0.823943 0.926938 0.444056 0.037 Uiso 1 1 calc R U . . .
H14B H 0.847502 0.845938 0.489267 0.037 Uiso 1 1 calc R U . . .
C22 C 0.64630(19) 0.6358(2) 0.80998(18) 0.0253(7) Uani 1 1 d . . . . .
H22A H 0.646037 0.675075 0.850957 0.030 Uiso 1 1 calc R U . . .
H22B H 0.613774 0.590937 0.818408 0.030 Uiso 1 1 calc R U . . .
C41 C 0.68740(19) 0.8500(2) 0.5622(2) 0.0269(7) Uani 1 1 d . . . . .
H41 H 0.717078 0.808541 0.591122 0.032 Uiso 1 1 calc R U . . .
C46 C 0.7818(2) 0.5899(2) 0.3332(2) 0.0328(8) Uani 1 1 d . . . . .
H46 H 0.808141 0.590269 0.387193 0.039 Uiso 1 1 calc R U . . .
C32 C 0.63444(19) 0.30561(18) 0.36606(19) 0.0229(7) Uani 1 1 d . . . . .
H32A H 0.661420 0.322660 0.325971 0.027 Uiso 1 1 calc R U . . .
H32B H 0.580121 0.289853 0.338972 0.027 Uiso 1 1 calc R U . . .
C36 C 0.71487(19) 0.3963(2) 0.4648(2) 0.0299(8) Uani 1 1 d . . . . .
H36A H 0.712674 0.438901 0.502072 0.036 Uiso 1 1 calc R U . . .
H36B H 0.743619 0.415807 0.427096 0.036 Uiso 1 1 calc R U . . .
C43 C 0.7050(2) 0.5835(2) 0.1803(2) 0.0307(8) Uani 1 1 d . . . . .
H43 H 0.675567 0.580744 0.127249 0.037 Uiso 1 1 calc R U . . .
C10 C 0.89883(19) 0.7699(2) 0.3739(2) 0.0315(8) Uani 1 1 d . . . . .
H10A H 0.889207 0.745790 0.321433 0.038 Uiso 1 1 calc R U . . .
H10B H 0.888590 0.730069 0.410661 0.038 Uiso 1 1 calc R U . . .
C40 C 0.6659(2) 0.9120(2) 0.6027(2) 0.0354(9) Uani 1 1 d . . . . .
H40 H 0.679852 0.912543 0.658221 0.043 Uiso 1 1 calc R U . . .
C1 C 0.31866(18) 0.6930(2) 0.2655(2) 0.0240(7) Uani 1 1 d . . . . .
H1A H 0.265457 0.708432 0.236676 0.036 Uiso 1 1 calc R U . . .
H1B H 0.324779 0.701255 0.321550 0.036 Uiso 1 1 calc R U . . .
H1C H 0.326944 0.637736 0.255729 0.036 Uiso 1 1 calc R U . . .
C23 C 0.72954(19) 0.6086(2) 0.81713(19) 0.0270(7) Uani 1 1 d . . . . .
H23A H 0.749915 0.582515 0.868198 0.032 Uiso 1 1 calc R U . . .
H23B H 0.763593 0.654208 0.814823 0.032 Uiso 1 1 calc R U . . .
C39 C 0.6241(2) 0.9727(2) 0.5611(2) 0.0396(10) Uani 1 1 d . . . . .
H39 H 0.607619 1.015363 0.587549 0.047 Uiso 1 1 calc R U . . .
C34 C 0.7610(2) 0.2578(2) 0.4551(2) 0.0323(8) Uani 1 1 d . . . . .
H34A H 0.792059 0.272245 0.417514 0.039 Uiso 1 1 calc R U . . .
H34B H 0.786940 0.212496 0.485883 0.039 Uiso 1 1 calc R U . . .
C44 C 0.7742(2) 0.5429(2) 0.2050(2) 0.0384(9) Uani 1 1 d . . . . .
H44 H 0.794904 0.513736 0.169036 0.046 Uiso 1 1 calc R U . . .
C33 C 0.67825(19) 0.23571(19) 0.4110(2) 0.0272(7) Uani 1 1 d . . . . .
H33A H 0.649020 0.216271 0.448313 0.033 Uiso 1 1 calc R U . . .
H33B H 0.680561 0.193098 0.373774 0.033 Uiso 1 1 calc R U . . .
C35 C 0.7590(2) 0.3261(2) 0.5095(2) 0.0421(10) Uani 1 1 d . . . . .
H35A H 0.813568 0.341761 0.535784 0.050 Uiso 1 1 calc R U . . .
H35B H 0.732715 0.309624 0.550351 0.050 Uiso 1 1 calc R U . . .
C45 C 0.8130(2) 0.5455(2) 0.2829(2) 0.0421(10) Uani 1 1 d . . . . .
H45 H 0.860447 0.517086 0.301890 0.050 Uiso 1 1 calc R U . . .
C24 C 0.7321(2) 0.5523(2) 0.7515(2) 0.0333(8) Uani 1 1 d . . . . .
H24A H 0.701937 0.504715 0.756944 0.040 Uiso 1 1 calc R U . . .
H24B H 0.787407 0.536681 0.755846 0.040 Uiso 1 1 calc R U . . .
C11 C 0.9846(2) 0.7966(3) 0.4003(2) 0.0488(12) Uani 1 1 d . . . . .
H11A H 1.019711 0.750509 0.406025 0.059 Uiso 1 1 calc R U . . .
H11B H 0.996762 0.831097 0.359950 0.059 Uiso 1 1 calc R U . . .
C13 C 0.9445(2) 0.9074(3) 0.4743(2) 0.0493(12) Uani 1 1 d . . . . .
H13A H 0.954328 0.946867 0.436943 0.059 Uiso 1 1 calc R U . . .
H13B H 0.954481 0.932222 0.526495 0.059 Uiso 1 1 calc R U . . .
C38 C 0.6063(2) 0.9710(2) 0.4804(2) 0.0363(9) Uani 1 1 d . . . . .
H38 H 0.579319 1.013159 0.450297 0.044 Uiso 1 1 calc R U . . .
C12 C 1.0002(2) 0.8401(3) 0.4778(2) 0.0604(15) Uani 1 1 d . . . . .
H12A H 0.994592 0.803583 0.519465 0.072 Uiso 1 1 calc R U . . .
H12B H 1.055060 0.859842 0.491457 0.072 Uiso 1 1 calc R U . . .
O1 O 0.65724(11) 0.59580(12) 0.45772(11) 0.0141(4) Uani 1 1 d . . . . .
O2 O 0.44456(11) 0.53628(11) 0.45224(11) 0.0132(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 N5 2.447(2) . ?
U1 N4 2.588(2) . ?
U1 N6 2.554(2) . ?
U1 N3 2.508(2) . ?
U1 O1 1.9041(18) . ?
U1 O2 1.9445(18) . ?
U1 O2 2.3243(19) 3_666 ?
Sm1 Cl1 2.6824(7) . ?
Sm1 N3 2.779(2) . ?
Sm1 N1 2.429(2) . ?
Sm1 N8 2.549(2) . ?
Sm1 N7 2.564(3) . ?
Sm1 N2 2.626(2) . ?
Sm1 O1 2.296(2) . ?
N5 C26 1.350(4) . ?
N5 C29 1.397(4) . ?
N4 C19 1.289(4) . ?
N4 C20 1.479(4) . ?
N6 C31 1.480(4) . ?
N6 C30 1.293(4) . ?
N3 C18 1.401(3) . ?
N3 C15 1.375(4) . ?
N1 C4 1.364(4) . ?
N1 C7 1.387(4) . ?
N8 C42 1.336(4) . ?
N8 C46 1.335(4) . ?
C19 H19 0.9500 . ?
C19 C18 1.430(4) . ?
N7 C37 1.333(4) . ?
N7 C41 1.351(4) . ?
C31 H31 1.0000 . ?
C31 C32 1.523(4) . ?
C31 C36 1.523(4) . ?
C26 C3 1.524(4) . ?
C26 C27 1.399(4) . ?
C18 C17 1.374(4) . ?
C15 C3 1.518(4) . ?
C15 C16 1.387(4) . ?
C20 H20 1.0000 . ?
C20 C21 1.528(4) . ?
C20 C25 1.521(4) . ?
N2 C9 1.475(4) . ?
N2 C8 1.295(4) . ?
C29 C30 1.423(4) . ?
C29 C28 1.387(4) . ?
C30 H30 0.9500 . ?
C3 C4 1.527(4) . ?
C3 C2 1.547(4) . ?
C17 H17 0.9500 . ?
C17 C16 1.393(4) . ?
C16 H16 0.9500 . ?
C4 C5 1.386(4) . ?
C42 H42 0.9500 . ?
C42 C43 1.380(4) . ?
C7 C6 1.388(4) . ?
C7 C8 1.423(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.385(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.528(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.525(4) . ?
C28 H28 0.9500 . ?
C6 H6 0.9500 . ?
C6 C5 1.397(4) . ?
C37 H37 0.9500 . ?
C37 C38 1.385(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C24 1.535(5) . ?
C9 H9 1.0000 . ?
C9 C14 1.526(5) . ?
C9 C10 1.516(5) . ?
C5 H5 0.9500 . ?
C8 H8 0.9500 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C13 1.522(5) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.507(4) . ?
C41 H41 0.9500 . ?
C41 C40 1.386(5) . ?
C46 H46 0.9500 . ?
C46 C45 1.383(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.532(4) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C35 1.537(5) . ?
C43 H43 0.9500 . ?
C43 C44 1.371(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.529(5) . ?
C40 H40 0.9500 . ?
C40 C39 1.374(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.519(5) . ?
C39 H39 0.9500 . ?
C39 C38 1.382(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C33 1.513(5) . ?
C34 C35 1.522(5) . ?
C44 H44 0.9500 . ?
C44 C45 1.373(6) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C45 H45 0.9500 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.523(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C12 1.503(7) . ?
C38 H38 0.9500 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 U1 N4 137.76(8) . . ?
N5 U1 N6 69.37(8) . . ?
N5 U1 N3 69.85(8) . . ?
N6 U1 N4 148.62(8) . . ?
N3 U1 N4 68.18(7) . . ?
N3 U1 N6 137.31(7) . . ?
O1 U1 N5 86.35(8) . . ?
O1 U1 N4 82.88(8) . . ?
O1 U1 N6 84.25(8) . . ?
O1 U1 N3 81.12(8) . . ?
O1 U1 O2 111.51(8) . 3_666 ?
O1 U1 O2 175.17(8) . . ?
O2 U1 N5 141.62(7) 3_666 . ?
O2 U1 N5 91.22(8) . . ?
O2 U1 N4 96.20(8) . . ?
O2 U1 N4 79.68(7) 3_666 . ?
O2 U1 N6 78.65(7) 3_666 . ?
O2 U1 N6 98.80(8) . . ?
O2 U1 N3 143.91(7) 3_666 . ?
O2 U1 N3 94.13(8) . . ?
O2 U1 O2 72.88(8) . 3_666 ?
Cl1 Sm1 N3 124.89(5) . . ?
N1 Sm1 Cl1 154.70(6) . . ?
N1 Sm1 N3 75.96(7) . . ?
N1 Sm1 N8 80.46(8) . . ?
N1 Sm1 N7 87.07(8) . . ?
N1 Sm1 N2 67.58(8) . . ?
N8 Sm1 Cl1 98.66(6) . . ?
N8 Sm1 N3 117.45(7) . . ?
N8 Sm1 N7 154.76(8) . . ?
N8 Sm1 N2 76.56(8) . . ?
N7 Sm1 Cl1 83.42(6) . . ?
N7 Sm1 N3 80.02(7) . . ?
N7 Sm1 N2 78.42(8) . . ?
N2 Sm1 Cl1 87.53(6) . . ?
N2 Sm1 N3 138.18(7) . . ?
O1 Sm1 Cl1 78.82(5) . . ?
O1 Sm1 N3 69.10(7) . . ?
O1 Sm1 N1 125.32(8) . . ?
O1 Sm1 N8 80.04(7) . . ?
O1 Sm1 N7 124.74(7) . . ?
O1 Sm1 N2 150.73(7) . . ?
C26 N5 U1 138.92(18) . . ?
C26 N5 C29 106.0(2) . . ?
C29 N5 U1 113.27(18) . . ?
C19 N4 U1 113.37(19) . . ?
C19 N4 C20 120.7(2) . . ?
C20 N4 U1 125.88(17) . . ?
C31 N6 U1 126.13(17) . . ?
C30 N6 U1 112.86(19) . . ?
C30 N6 C31 120.9(2) . . ?
U1 N3 Sm1 87.34(7) . . ?
C18 N3 U1 112.00(17) . . ?
C18 N3 Sm1 107.97(16) . . ?
C15 N3 U1 133.12(18) . . ?
C15 N3 Sm1 107.33(16) . . ?
C15 N3 C18 105.3(2) . . ?
C4 N1 Sm1 136.39(19) . . ?
C4 N1 C7 105.3(2) . . ?
C7 N1 Sm1 116.80(18) . . ?
C42 N8 Sm1 126.4(2) . . ?
C46 N8 Sm1 116.1(2) . . ?
C46 N8 C42 117.4(3) . . ?
N4 C19 H19 118.8 . . ?
N4 C19 C18 122.5(3) . . ?
C18 C19 H19 118.8 . . ?
C37 N7 Sm1 120.4(2) . . ?
C37 N7 C41 117.1(3) . . ?
C41 N7 Sm1 121.2(2) . . ?
N6 C31 H31 107.2 . . ?
N6 C31 C32 115.7(2) . . ?
N6 C31 C36 109.4(2) . . ?
C32 C31 H31 107.2 . . ?
C36 C31 H31 107.2 . . ?
C36 C31 C32 109.8(2) . . ?
N5 C26 C3 125.4(2) . . ?
N5 C26 C27 110.5(3) . . ?
C27 C26 C3 123.8(3) . . ?
N3 C18 C19 121.2(3) . . ?
C17 C18 N3 110.4(2) . . ?
C17 C18 C19 127.8(3) . . ?
N3 C15 C3 125.0(2) . . ?
N3 C15 C16 109.9(2) . . ?
C16 C15 C3 124.9(3) . . ?
N4 C20 H20 107.2 . . ?
N4 C20 C21 115.2(2) . . ?
N4 C20 C25 109.5(2) . . ?
C21 C20 H20 107.2 . . ?
C25 C20 H20 107.2 . . ?
C25 C20 C21 110.3(2) . . ?
C9 N2 Sm1 131.60(19) . . ?
C8 N2 Sm1 111.96(19) . . ?
C8 N2 C9 116.4(2) . . ?
N5 C29 C30 121.2(3) . . ?
C28 C29 N5 109.8(3) . . ?
C28 C29 C30 129.0(3) . . ?
N6 C30 C29 122.6(3) . . ?
N6 C30 H30 118.7 . . ?
C29 C30 H30 118.7 . . ?
C26 C3 C4 105.0(2) . . ?
C26 C3 C2 108.1(2) . . ?
C15 C3 C26 116.8(2) . . ?
C15 C3 C4 107.1(2) . . ?
C15 C3 C2 108.8(2) . . ?
C4 C3 C2 110.8(2) . . ?
C18 C17 H17 126.7 . . ?
C18 C17 C16 106.6(3) . . ?
C16 C17 H17 126.7 . . ?
C15 C16 C17 107.7(3) . . ?
C15 C16 H16 126.2 . . ?
C17 C16 H16 126.2 . . ?
N1 C4 C3 118.4(2) . . ?
N1 C4 C5 111.2(3) . . ?
C5 C4 C3 130.3(3) . . ?
N8 C42 H42 118.5 . . ?
N8 C42 C43 122.9(3) . . ?
C43 C42 H42 118.5 . . ?
N1 C7 C6 110.5(3) . . ?
N1 C7 C8 119.6(3) . . ?
C6 C7 C8 129.9(3) . . ?
C26 C27 H27 126.5 . . ?
C28 C27 C26 107.0(3) . . ?
C28 C27 H27 126.5 . . ?
C20 C21 H21A 109.3 . . ?
C20 C21 H21B 109.3 . . ?
H21A C21 H21B 108.0 . . ?
C22 C21 C20 111.5(3) . . ?
C22 C21 H21A 109.3 . . ?
C22 C21 H21B 109.3 . . ?
C3 C2 H2A 109.0 . . ?
C3 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C1 C2 C3 112.9(2) . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
C29 C28 H28 126.6 . . ?
C27 C28 C29 106.8(3) . . ?
C27 C28 H28 126.6 . . ?
C7 C6 H6 126.8 . . ?
C7 C6 C5 106.4(3) . . ?
C5 C6 H6 126.8 . . ?
N7 C37 H37 118.2 . . ?
N7 C37 C38 123.6(3) . . ?
C38 C37 H37 118.2 . . ?
C20 C25 H25A 109.7 . . ?
C20 C25 H25B 109.7 . . ?
C20 C25 C24 109.7(3) . . ?
H25A C25 H25B 108.2 . . ?
C24 C25 H25A 109.7 . . ?
C24 C25 H25B 109.7 . . ?
N2 C9 H9 107.8 . . ?
N2 C9 C14 110.5(3) . . ?
N2 C9 C10 111.0(3) . . ?
C14 C9 H9 107.8 . . ?
C10 C9 H9 107.8 . . ?
C10 C9 C14 111.7(3) . . ?
C4 C5 C6 106.7(3) . . ?
C4 C5 H5 126.7 . . ?
C6 C5 H5 126.7 . . ?
N2 C8 C7 122.9(3) . . ?
N2 C8 H8 118.5 . . ?
C7 C8 H8 118.5 . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C13 C14 C9 110.6(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C21 C22 H22A 109.3 . . ?
C21 C22 H22B 109.3 . . ?
H22A C22 H22B 108.0 . . ?
C23 C22 C21 111.4(3) . . ?
C23 C22 H22A 109.3 . . ?
C23 C22 H22B 109.3 . . ?
N7 C41 H41 118.6 . . ?
N7 C41 C40 122.8(3) . . ?
C40 C41 H41 118.6 . . ?
N8 C46 H46 118.6 . . ?
N8 C46 C45 122.8(3) . . ?
C45 C46 H46 118.6 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 C33 110.9(3) . . ?
H32A C32 H32B 108.1 . . ?
C33 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
C31 C36 H36A 109.5 . . ?
C31 C36 H36B 109.5 . . ?
C31 C36 C35 110.6(3) . . ?
H36A C36 H36B 108.1 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C42 C43 H43 120.4 . . ?
C44 C43 C42 119.1(3) . . ?
C44 C43 H43 120.4 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 C11 110.9(3) . . ?
H10A C10 H10B 108.0 . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
C41 C40 H40 120.6 . . ?
C39 C40 C41 118.9(4) . . ?
C39 C40 H40 120.6 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C22 C23 H23A 109.6 . . ?
C22 C23 H23B 109.6 . . ?
C22 C23 C24 110.3(3) . . ?
H23A C23 H23B 108.1 . . ?
C24 C23 H23A 109.6 . . ?
C24 C23 H23B 109.6 . . ?
C40 C39 H39 120.5 . . ?
C40 C39 C38 119.1(3) . . ?
C38 C39 H39 120.5 . . ?
H34A C34 H34B 108.1 . . ?
C33 C34 H34A 109.6 . . ?
C33 C34 H34B 109.6 . . ?
C33 C34 C35 110.2(3) . . ?
C35 C34 H34A 109.6 . . ?
C35 C34 H34B 109.6 . . ?
C43 C44 H44 120.7 . . ?
C43 C44 C45 118.6(3) . . ?
C45 C44 H44 120.7 . . ?
C32 C33 H33A 109.4 . . ?
C32 C33 H33B 109.4 . . ?
C34 C33 C32 111.3(3) . . ?
C34 C33 H33A 109.4 . . ?
C34 C33 H33B 109.4 . . ?
H33A C33 H33B 108.0 . . ?
C36 C35 H35A 109.3 . . ?
C36 C35 H35B 109.3 . . ?
C34 C35 C36 111.5(3) . . ?
C34 C35 H35A 109.3 . . ?
C34 C35 H35B 109.3 . . ?
H35A C35 H35B 108.0 . . ?
C46 C45 H45 120.5 . . ?
C44 C45 C46 119.0(4) . . ?
C44 C45 H45 120.5 . . ?
C25 C24 H24A 109.2 . . ?
C25 C24 H24B 109.2 . . ?
C23 C24 C25 112.0(3) . . ?
C23 C24 H24A 109.2 . . ?
C23 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
C10 C11 H11A 109.4 . . ?
C10 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 C10 111.2(3) . . ?
C12 C11 H11A 109.4 . . ?
C12 C11 H11B 109.4 . . ?
C14 C13 H13A 109.3 . . ?
C14 C13 H13B 109.3 . . ?
H13A C13 H13B 108.0 . . ?
C12 C13 C14 111.5(4) . . ?
C12 C13 H13A 109.3 . . ?
C12 C13 H13B 109.3 . . ?
C37 C38 H38 120.8 . . ?
C39 C38 C37 118.4(4) . . ?
C39 C38 H38 120.8 . . ?
C11 C12 H12A 109.3 . . ?
C11 C12 H12B 109.3 . . ?
C13 C12 C11 111.8(4) . . ?
C13 C12 H12A 109.3 . . ?
C13 C12 H12B 109.3 . . ?
H12A C12 H12B 107.9 . . ?
U1 O1 Sm1 120.77(9) . . ?
U1 O2 U1 107.12(8) . 3_666 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 N5 C26 C3 24.3(4) . . . . ?
U1 N5 C26 C27 -162.2(2) . . . . ?
U1 N5 C29 C30 -10.2(3) . . . . ?
U1 N5 C29 C28 167.45(19) . . . . ?
U1 N4 C19 C18 -4.1(3) . . . . ?
U1 N4 C20 C21 -171.25(18) . . . . ?
U1 N4 C20 C25 63.8(3) . . . . ?
U1 N6 C31 C32 171.63(19) . . . . ?
U1 N6 C31 C36 -63.8(3) . . . . ?
U1 N6 C30 C29 0.7(3) . . . . ?
U1 N3 C18 C19 18.6(3) . . . . ?
U1 N3 C18 C17 -153.35(19) . . . . ?
U1 N3 C15 C3 -40.2(4) . . . . ?
U1 N3 C15 C16 144.0(2) . . . . ?
Sm1 N3 C18 C19 -75.9(3) . . . . ?
Sm1 N3 C18 C17 112.2(2) . . . . ?
Sm1 N3 C15 C3 62.8(3) . . . . ?
Sm1 N3 C15 C16 -112.9(2) . . . . ?
Sm1 N1 C4 C3 11.7(4) . . . . ?
Sm1 N1 C4 C5 -164.3(2) . . . . ?
Sm1 N1 C7 C6 168.0(2) . . . . ?
Sm1 N1 C7 C8 -11.2(3) . . . . ?
Sm1 N8 C42 C43 176.8(2) . . . . ?
Sm1 N8 C46 C45 -175.2(3) . . . . ?
Sm1 N7 C37 C38 166.0(3) . . . . ?
Sm1 N7 C41 C40 -164.7(3) . . . . ?
Sm1 N2 C9 C14 -61.0(4) . . . . ?
Sm1 N2 C9 C10 63.5(3) . . . . ?
Sm1 N2 C8 C7 4.4(4) . . . . ?
N5 C26 C3 C15 -15.1(4) . . . . ?
N5 C26 C3 C4 103.5(3) . . . . ?
N5 C26 C3 C2 -138.1(3) . . . . ?
N5 C26 C27 C28 -0.3(3) . . . . ?
N5 C29 C30 N6 6.7(4) . . . . ?
N5 C29 C28 C27 -0.1(3) . . . . ?
N4 C19 C18 N3 -10.2(4) . . . . ?
N4 C19 C18 C17 160.2(3) . . . . ?
N4 C20 C21 C22 178.9(2) . . . . ?
N4 C20 C25 C24 -175.7(3) . . . . ?
N6 C31 C32 C33 -178.1(2) . . . . ?
N6 C31 C36 C35 174.9(3) . . . . ?
N3 C18 C17 C16 1.7(3) . . . . ?
N3 C15 C3 C26 23.7(4) . . . . ?
N3 C15 C3 C4 -93.7(3) . . . . ?
N3 C15 C3 C2 146.4(3) . . . . ?
N3 C15 C16 C17 -0.9(3) . . . . ?
N1 C4 C5 C6 -0.4(4) . . . . ?
N1 C7 C6 C5 -0.1(4) . . . . ?
N1 C7 C8 N2 4.1(5) . . . . ?
N8 C42 C43 C44 -2.0(5) . . . . ?
N8 C46 C45 C44 -1.7(6) . . . . ?
C19 N4 C20 C21 5.5(4) . . . . ?
C19 N4 C20 C25 -119.4(3) . . . . ?
C19 C18 C17 C16 -169.5(3) . . . . ?
N7 C37 C38 C39 -1.3(6) . . . . ?
N7 C41 C40 C39 -1.1(5) . . . . ?
C31 N6 C30 C29 -176.0(3) . . . . ?
C31 C32 C33 C34 -57.6(4) . . . . ?
C31 C36 C35 C34 56.9(4) . . . . ?
C26 N5 C29 C30 -177.8(3) . . . . ?
C26 N5 C29 C28 -0.1(3) . . . . ?
C26 C3 C4 N1 -82.0(3) . . . . ?
C26 C3 C4 C5 93.0(4) . . . . ?
C26 C3 C2 C1 63.1(3) . . . . ?
C26 C27 C28 C29 0.2(4) . . . . ?
C18 N3 C15 C3 177.7(3) . . . . ?
C18 N3 C15 C16 1.9(3) . . . . ?
C18 C17 C16 C15 -0.5(3) . . . . ?
C15 N3 C18 C19 169.6(2) . . . . ?
C15 N3 C18 C17 -2.3(3) . . . . ?
C15 C3 C4 N1 42.8(3) . . . . ?
C15 C3 C4 C5 -142.1(3) . . . . ?
C15 C3 C2 C1 -64.6(3) . . . . ?
C20 N4 C19 C18 178.7(2) . . . . ?
C20 C21 C22 C23 55.9(4) . . . . ?
C20 C25 C24 C23 -57.6(4) . . . . ?
N2 C9 C14 C13 179.8(3) . . . . ?
N2 C9 C10 C11 -179.2(3) . . . . ?
C29 N5 C26 C3 -173.2(3) . . . . ?
C29 N5 C26 C27 0.3(3) . . . . ?
C30 N6 C31 C32 -12.1(4) . . . . ?
C30 N6 C31 C36 112.4(3) . . . . ?
C30 C29 C28 C27 177.3(3) . . . . ?
C3 C26 C27 C28 173.2(3) . . . . ?
C3 C15 C16 C17 -176.7(3) . . . . ?
C3 C4 C5 C6 -175.8(3) . . . . ?
C16 C15 C3 C26 -161.2(3) . . . . ?
C16 C15 C3 C4 81.5(3) . . . . ?
C16 C15 C3 C2 -38.5(4) . . . . ?
C4 N1 C7 C6 -0.2(3) . . . . ?
C4 N1 C7 C8 -179.4(3) . . . . ?
C4 C3 C2 C1 177.8(2) . . . . ?
C42 N8 C46 C45 2.8(5) . . . . ?
C42 C43 C44 C45 3.1(6) . . . . ?
C7 N1 C4 C3 176.4(2) . . . . ?
C7 N1 C4 C5 0.4(3) . . . . ?
C7 C6 C5 C4 0.3(4) . . . . ?
C27 C26 C3 C15 172.3(3) . . . . ?
C27 C26 C3 C4 -69.2(3) . . . . ?
C27 C26 C3 C2 49.2(4) . . . . ?
C21 C20 C25 C24 56.5(4) . . . . ?
C21 C22 C23 C24 -55.2(4) . . . . ?
C2 C3 C4 N1 161.4(2) . . . . ?
C2 C3 C4 C5 -23.5(4) . . . . ?
C28 C29 C30 N6 -170.5(3) . . . . ?
C6 C7 C8 N2 -174.9(3) . . . . ?
C37 N7 C41 C40 2.3(5) . . . . ?
C25 C20 C21 C22 -56.5(3) . . . . ?
C9 N2 C8 C7 -177.6(3) . . . . ?
C9 C14 C13 C12 -55.7(4) . . . . ?
C9 C10 C11 C12 54.4(5) . . . . ?
C8 N2 C9 C14 121.5(3) . . . . ?
C8 N2 C9 C10 -114.0(3) . . . . ?
C8 C7 C6 C5 179.1(3) . . . . ?
C14 C9 C10 C11 -55.3(4) . . . . ?
C14 C13 C12 C11 55.7(4) . . . . ?
C22 C23 C24 C25 56.7(4) . . . . ?
C41 N7 C37 C38 -1.2(5) . . . . ?
C41 C40 C39 C38 -1.5(6) . . . . ?
C46 N8 C42 C43 -0.9(5) . . . . ?
C32 C31 C36 C35 -57.1(4) . . . . ?
C36 C31 C32 C33 57.6(3) . . . . ?
C43 C44 C45 C46 -1.3(6) . . . . ?
C10 C9 C14 C13 55.8(4) . . . . ?
C10 C11 C12 C13 -54.9(5) . . . . ?
C40 C39 C38 C37 2.6(6) . . . . ?
C33 C34 C35 C36 -55.9(4) . . . . ?
C35 C34 C33 C32 56.1(4) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 0.500 448.3 126.6 '2.25 pyridines'
2 0.196 0.964 0.471 37.3 0.0 ?
3 0.304 0.464 0.029 37.3 0.0 ?
4 0.500 0.000 0.000 448.3 126.6 '2.25 pyridines'
5 0.696 0.536 0.971 37.3 0.0 ?
6 0.804 0.036 0.529 37.3 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.091
_oxdiff_exptl_absorpt_empirical_full_min 0.917
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Pyridene, hexane'
_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_to506_2_refinalised
_database_code_depnum_ccdc_archive 'CCDC 2313502'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2023-12-11 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_audit_creation_date             2023-11-17
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C112.003 H136.003 K4 N20.001 O4 U2'
_chemical_formula_sum            'C112 H136 K4 N20 O4 U2'
_chemical_formula_weight         2458.86
_chemical_melting_point          ?
_chemical_oxdiff_formula         C70H90N6U2O4K4
_chemical_oxdiff_usercomment     Pyr/hex
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.5339(3)
_cell_length_b                   12.5763(2)
_cell_length_c                   19.5151(5)
_cell_angle_alpha                76.777(2)
_cell_angle_beta                 79.539(2)
_cell_angle_gamma                68.993(2)
_cell_volume                     2778.75(12)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    24560
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      29.2040
_cell_measurement_theta_min      3.6730
_shelx_estimated_absorpt_T_max   0.521
_shelx_estimated_absorpt_T_min   0.248
_exptl_absorpt_coefficient_mu    3.120
_exptl_absorpt_correction_T_max  0.274
_exptl_absorpt_correction_T_min  0.069
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1240
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
16 13 4 0.2764
-1 16 9 0.2633
-16 -1 3 0.2318
-15 -14 -5 0.2508
1 -16 -9 0.2263
15 -1 -4 0.2511
2 17 3 0.2171
0 -1 26 0.1287
-2 -17 0 0.2177
0 0 -26 0.1073

_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.24
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
15.5241 13.3250 4.0503 -0.0656 0.8345 0.5471
-0.6077 16.0771 9.1528 0.0129 -0.1515 0.9884
-16.2328 -0.6041 3.2420 0.0769 -0.9680 0.2388
-14.9722 -14.0727 -4.5915 0.0625 -0.7961 -0.6020
1.1447 -15.8419 -9.1393 -0.0153 0.1820 -0.9832
15.4109 -1.4624 -4.2200 -0.0743 0.9336 -0.3506
2.0488 17.1266 3.2758 -0.2158 0.0292 0.9760
-0.0124 -0.5943 26.4297 0.9860 -0.1292 0.1058
-2.0089 -16.8510 -0.1029 0.3274 -0.0438 -0.9439
-0.0032 0.4641 -26.4768 -0.9851 0.1291 -0.1133

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.869
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            51201
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.734
_diffrn_reflns_theta_min         3.360
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -88.00 -25.00   1.00    5.70    --  -16.54 161.00   7.00   63
  2  ω    -62.00   6.00   1.00    5.70    --  -16.54 117.00-143.00   68
  3  ω     24.00  91.00   1.00    5.70    --   18.41-161.00 -22.00   67
  4  ω     -6.00  64.00   1.00    5.70    --   18.41-117.00 129.00   70
  5  ω    -35.00  53.00   1.00    5.70    --  -16.54  38.00 -30.00   88
  6  ω    -89.00 -39.00   1.00    5.70    --  -16.54-178.00 120.00   50
  7  ω    -43.00  39.00   1.00    5.70    --  -16.54  77.00-120.00   82
  8  ω     -8.00  39.00   1.00    5.70    --   18.41  77.00-150.00   47
  9  ω     -8.00  39.00   1.00    5.70    --   18.41  77.00   0.00   47
 10  ω      2.00  86.00   1.00    5.70    --   18.41  57.00 120.00   84
 11  ω    -51.00  37.00   1.00    5.70    --   18.41 -38.00 -30.00   88
 12  ω    -86.00 -20.00   1.00    5.70    --  -16.54 -38.00-150.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0033709000
_diffrn_orient_matrix_UB_12      -0.0200555000
_diffrn_orient_matrix_UB_13      0.0368558000
_diffrn_orient_matrix_UB_21      0.0588065000
_diffrn_orient_matrix_UB_22      -0.0043797000
_diffrn_orient_matrix_UB_23      -0.0049591000
_diffrn_orient_matrix_UB_31      -0.0158058000
_diffrn_orient_matrix_UB_32      0.0578649000
_diffrn_orient_matrix_UB_33      0.0052951000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12167
_reflns_number_total             13766
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.67
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.415
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         13766
_refine_ls_number_restraints     301
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0328
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0333P)²+1.7319P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0740
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N8-C42 = N8-C46
 1.33 with sigma of 0.02
 C42-C43 = C45-C46
 1.38 with sigma of 0.02
 C43-C44 = C44-C45
 1.37 with sigma of 0.02
 N8A-C46A = N8A-C42A
 1.33 with sigma of 0.02
 C46A-C45A = C43A-C42A
 1.38 with sigma of 0.02
 C45A-C44A = C44A-C43A
 1.37 with sigma of 0.02
 N8B-C42B = N8B-C46B
 1.33 with sigma of 0.02
 C42B-C43B = C45B-C46B
 1.38 with sigma of 0.02
 C43B-C44B = C44B-C45B
 1.37 with sigma of 0.02
 N8-C43
 2.4 with sigma of 0.04
 N8-C45
 2.39 with sigma of 0.04
 C42-C44
 2.36 with sigma of 0.04
 C43-C45
 2.35 with sigma of 0.04
 C44-C46
 2.37 with sigma of 0.04
 N8A-C45A
 2.4 with sigma of 0.04
 N8A-C43A
 2.39 with sigma of 0.04
 C46A-C44A
 2.36 with sigma of 0.04
 C45A-C43A
 2.35 with sigma of 0.04
 C44A-C42A
 2.37 with sigma of 0.04
 N8B-C43B
 2.4 with sigma of 0.04
 N8B-C45B
 2.39 with sigma of 0.04
 C42B-C44B
 2.36 with sigma of 0.04
 C43B-C45B
 2.35 with sigma of 0.04
 C44B-C46B
 2.37 with sigma of 0.04
 N8-C42 \\sim N8-C46
 with sigma of 0.02
 C42-C43 \\sim C43-C44 \\sim C44-C45 \\sim C45-C46
 with sigma of 0.02
 N8-C45 \\sim N8-C43
 with sigma of 0.04
 C44-C46 \\sim C44-C42 \\sim C45-C43 \\sim C46-C42
 with sigma of 0.04
 N8A-C46A \\sim N8A-C42A
 with sigma of 0.02
 C46A-C45A \\sim C45A-C44A \\sim C44A-C43A \\sim C43A-C42A
 with sigma of 0.02
 N8A-C43A \\sim N8A-C45A
 with sigma of 0.04
 C44A-C42A \\sim C44A-C46A \\sim C43A-C45A \\sim C42A-C46A
 with sigma of 0.04
 N8B-C42B \\sim N8B-C46B
 with sigma of 0.02
 C42B-C43B \\sim C43B-C44B \\sim C44B-C45B \\sim C45B-C46B
 with sigma of 0.02
 N8B-C45B \\sim N8B-C43B
 with sigma of 0.04
 C44B-C46B \\sim C44B-C42B \\sim C45B-C43B \\sim C46B-C42B
 with sigma of 0.04
3. Restrained planarity
 N8, C42, C43, C44, C45, C46
 with sigma of 0.1
 N8A, C46A, C45A, C44A, C43A, C42A
 with sigma of 0.1
 N8B, C42B, C43B, C44B, C45B, C46B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N8 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
N8A \\sim C46A \\sim C45A \\sim C44A \\sim C43A \\sim C42A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N8B \\sim C42B \\sim C43B \\sim C44B \\sim C45B \\sim C46B: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 N8, C42, C43, C44, C45, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N8A, C46A, C45A, C44A, C43A, C42A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N8B, C42B, C43B, C44B, C45B, C46B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(N8)+Sof(C42)+Sof(H42)+Sof(C43)+Sof(H43)+Sof(C44)+Sof(H44)+Sof(C45)+
 Sof(H45)+Sof(C46)+Sof(H46)]+1*[Sof(N8A)+Sof(C46A)+Sof(H46A)+Sof(C45A)+
 Sof(H45A)+Sof(C44A)+Sof(H44A)+Sof(C43A)+Sof(H43A)+Sof(C42A)+Sof(H42A)]+1*
 [Sof(N8B)+Sof(C42B)+Sof(H42B)+Sof(C43B)+Sof(H43B)+Sof(C44B)+Sof(H44B)+
 Sof(C45B)+Sof(H45B)+Sof(C46B)+Sof(H46B)]=1 with esd of 0.001
 Sof(N8)=Sof(C42)=Sof(H42)=Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44)=Sof(C45)=
 Sof(H45)=Sof(C46)=Sof(H46)=FVAR(1)
 Sof(N8A)=Sof(C46A)=Sof(H46A)=Sof(C45A)=Sof(H45A)=Sof(C44A)=Sof(H44A)=
 Sof(C43A)=Sof(H43A)=Sof(C42A)=Sof(H42A)=FVAR(2)
 Sof(N8B)=Sof(C42B)=Sof(H42B)=Sof(C43B)=Sof(H43B)=Sof(C44B)=Sof(H44B)=
 Sof(C45B)=Sof(H45B)=Sof(C46B)=Sof(H46B)=FVAR(3)
7.a Ternary CH refined with riding coordinates:
 C4(H4), C7(H7), C18(H18), C29(H29)
7.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B),
  C23(H23A,H23B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C35(H35A,H35B)
7.c Aromatic/amide H refined with riding coordinates:
 C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C46A(H46A), C45A(H45A),
 C44A(H44A), C43A(H43A), C42A(H42A), C42B(H42B), C43B(H43B), C44B(H44B),
 C45B(H45B), C46B(H46B), C6(H6), C14(H14), C15(H15), C17(H17), C25(H25),
 C26(H26), C28(H28), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C47(H47),
  C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54),
 C55(H55), C56(H56)
7.d Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.52079(2) 0.57787(2) 0.41500(2) 0.01391(4) Uani 1 1 d . . . . .
K1 K 0.67652(6) 0.60517(6) 0.21005(4) 0.02543(16) Uani 1 1 d . . . . .
K2 K 0.52565(6) 0.86672(6) 0.27569(4) 0.02138(14) Uani 1 1 d . . . . .
O1 O 0.62239(17) 0.64685(17) 0.35592(11) 0.0176(4) Uani 1 1 d . . . . .
O2 O 0.41093(16) 0.50945(16) 0.47269(11) 0.0148(4) Uani 1 1 d . . . . .
N1 N 0.4915(2) 0.5255(2) 0.30703(14) 0.0169(5) Uani 1 1 d . . . . .
N2 N 0.6753(2) 0.3890(2) 0.38649(14) 0.0165(5) Uani 1 1 d . . . . .
N3 N 0.3639(2) 0.7393(2) 0.35741(14) 0.0168(5) Uani 1 1 d . . . . .
N4 N 0.4528(2) 0.7549(2) 0.47614(14) 0.0166(5) Uani 1 1 d . . . . .
N5 N 0.4705(2) 0.7701(2) 0.17635(14) 0.0175(5) Uani 1 1 d . . . . .
N6 N 0.6684(2) 0.8427(2) 0.12983(15) 0.0268(6) Uani 1 1 d . . . . .
N7 N 0.9117(3) 0.4477(4) 0.20766(19) 0.0523(10) Uani 1 1 d . . . . .
N8 N 0.730(3) 0.529(3) 0.0768(19) 0.063(11) Uani 0.224(16) 1 d D U P A 2
N9 N 0.7280(2) 0.8994(3) 0.31666(16) 0.0297(7) Uani 1 1 d . . . . .
N10 N 0.4048(3) 1.0859(3) 0.20162(17) 0.0332(7) Uani 1 1 d . . . . .
N8A N 0.7175(13) 0.530(2) 0.0757(13) 0.043(6) Uani 0.317(13) 1 d D U P A -1
N8B N 0.7475(12) 0.5154(14) 0.0736(9) 0.050(4) Uani 0.459(13) 1 d D U P A 3
C1 C 0.3265(2) 0.6877(3) 0.24649(17) 0.0182(6) Uani 1 1 d . . . . .
C42 C 0.641(3) 0.513(3) 0.0570(14) 0.063(9) Uani 0.224(16) 1 d D U P A 2
H42 H 0.566509 0.544623 0.080860 0.076 Uiso 0.224(16) 1 calc R U P A 2
C43 C 0.652(4) 0.453(3) 0.0037(16) 0.081(10) Uani 0.224(16) 1 d D U P A 2
H43 H 0.587713 0.442291 -0.009116 0.097 Uiso 0.224(16) 1 calc R U P A 2
C44 C 0.761(4) 0.410(3) -0.030(2) 0.085(11) Uani 0.224(16) 1 d D U P A 2
H44 H 0.771507 0.369972 -0.067935 0.102 Uiso 0.224(16) 1 calc R U P A 2
C45 C 0.853(3) 0.425(2) -0.0104(15) 0.082(10) Uani 0.224(16) 1 d D U P A 2
H45 H 0.928221 0.393471 -0.033261 0.098 Uiso 0.224(16) 1 calc R U P A 2
C46 C 0.835(3) 0.486(2) 0.0436(14) 0.055(8) Uani 0.224(16) 1 d D U P A 2
H46 H 0.898638 0.498219 0.057145 0.066 Uiso 0.224(16) 1 calc R U P A 2
C46A C 0.7996(16) 0.4455(18) 0.0462(9) 0.076(6) Uani 0.317(13) 1 d D U P A -1
H46A H 0.877014 0.428572 0.054157 0.091 Uiso 0.317(13) 1 calc R U P A -1
C45A C 0.777(2) 0.3821(16) 0.0053(10) 0.088(8) Uani 0.317(13) 1 d D U P A -1
H45A H 0.838376 0.322458 -0.013947 0.106 Uiso 0.317(13) 1 calc R U P A -1
C44A C 0.667(2) 0.4052(15) -0.0077(10) 0.080(7) Uani 0.317(13) 1 d D U P A -1
H44A H 0.650015 0.362937 -0.036574 0.096 Uiso 0.317(13) 1 calc R U P A -1
C43A C 0.5807(16) 0.4900(14) 0.0216(8) 0.054(4) Uani 0.317(13) 1 d D U P A -1
H43A H 0.502953 0.507058 0.014351 0.065 Uiso 0.317(13) 1 calc R U P A -1
C42A C 0.6093(13) 0.5502(14) 0.0619(9) 0.033(3) Uani 0.317(13) 1 d D U P A -1
H42A H 0.548849 0.610041 0.081400 0.040 Uiso 0.317(13) 1 calc R U P A -1
C42B C 0.6974(13) 0.4572(12) 0.0488(6) 0.065(4) Uani 0.459(13) 1 d D U P A 3
H42B H 0.631872 0.442596 0.076603 0.078 Uiso 0.459(13) 1 calc R U P A 3
C43B C 0.7331(16) 0.4167(17) -0.0139(8) 0.073(5) Uani 0.459(13) 1 d D U P A 3
H43B H 0.694524 0.374143 -0.028350 0.088 Uiso 0.459(13) 1 calc R U P A 3
C44B C 0.8257(13) 0.4391(14) -0.0550(7) 0.082(4) Uani 0.459(13) 1 d D U P A 3
H44B H 0.852783 0.413047 -0.099001 0.098 Uiso 0.459(13) 1 calc R U P A 3
C45B C 0.8785(12) 0.4996(18) -0.0318(7) 0.097(6) Uani 0.459(13) 1 d D U P A 3
H45B H 0.943414 0.516330 -0.058972 0.116 Uiso 0.459(13) 1 calc R U P A 3
C46B C 0.8359(13) 0.5359(16) 0.0317(7) 0.072(5) Uani 0.459(13) 1 d D U P A 3
H46B H 0.872816 0.579200 0.046886 0.086 Uiso 0.459(13) 1 calc R U P A 3
C2 C 0.4178(3) 0.5679(3) 0.25742(17) 0.0187(6) Uani 1 1 d . . . . .
C3 C 0.4451(3) 0.4912(3) 0.20934(19) 0.0270(7) Uani 1 1 d . . . . .
H3A H 0.380060 0.463486 0.210451 0.032 Uiso 1 1 calc R U . . .
H3B H 0.461659 0.530498 0.160568 0.032 Uiso 1 1 calc R U . . .
C4 C 0.5422(3) 0.3983(3) 0.23046(18) 0.0243(7) Uani 1 1 d . . . . .
H4 H 0.574905 0.323503 0.212380 0.029 Uiso 1 1 calc R U . . .
C5 C 0.5687(3) 0.4204(2) 0.29024(17) 0.0183(6) Uani 1 1 d . . . . .
C6 C 0.6620(2) 0.3560(2) 0.33200(17) 0.0193(6) Uani 1 1 d . . . . .
H6 H 0.715830 0.286460 0.318903 0.023 Uiso 1 1 calc R U . . .
C7 C 0.7754(2) 0.3268(2) 0.42657(17) 0.0188(6) Uani 1 1 d . . . . .
H7 H 0.745128 0.312628 0.477664 0.023 Uiso 1 1 calc R U . . .
C8 C 0.8500(3) 0.2094(3) 0.40754(18) 0.0229(7) Uani 1 1 d . . . . .
H8A H 0.883302 0.219750 0.357427 0.027 Uiso 1 1 calc R U . . .
H8B H 0.802303 0.159308 0.413407 0.027 Uiso 1 1 calc R U . . .
C9 C 0.9468(3) 0.1520(3) 0.4557(2) 0.0286(8) Uani 1 1 d . . . . .
H9A H 0.913050 0.137475 0.505459 0.034 Uiso 1 1 calc R U . . .
H9B H 0.995686 0.076487 0.442587 0.034 Uiso 1 1 calc R U . . .
C10 C 1.0205(3) 0.2280(3) 0.4494(2) 0.0305(8) Uani 1 1 d . . . . .
H10A H 1.060291 0.236322 0.400787 0.037 Uiso 1 1 calc R U . . .
H10B H 1.079606 0.190701 0.482765 0.037 Uiso 1 1 calc R U . . .
C11 C 0.9464(3) 0.3477(3) 0.4658(2) 0.0314(8) Uani 1 1 d . . . . .
H11A H 0.914511 0.340032 0.516308 0.038 Uiso 1 1 calc R U . . .
H11B H 0.994900 0.397456 0.457858 0.038 Uiso 1 1 calc R U . . .
C12 C 0.8477(3) 0.4048(3) 0.41939(19) 0.0239(7) Uani 1 1 d . . . . .
H12A H 0.798450 0.479521 0.433496 0.029 Uiso 1 1 calc R U . . .
H12B H 0.879427 0.420894 0.369301 0.029 Uiso 1 1 calc R U . . .
C13 C 0.3036(2) 0.7628(2) 0.30197(17) 0.0176(6) Uani 1 1 d . . . . .
C14 C 0.2216(3) 0.8748(3) 0.29797(18) 0.0217(7) Uani 1 1 d . . . . .
H14 H 0.168757 0.911913 0.263589 0.026 Uiso 1 1 calc R U . . .
C15 C 0.2323(3) 0.9208(3) 0.35347(17) 0.0204(7) Uani 1 1 d . . . . .
H15 H 0.188308 0.995170 0.364422 0.024 Uiso 1 1 calc R U . . .
C16 C 0.3203(2) 0.8366(2) 0.39025(16) 0.0172(6) Uani 1 1 d . . . . .
C17 C 0.3690(2) 0.8404(2) 0.44936(17) 0.0174(6) Uani 1 1 d . . . . .
H17 H 0.338949 0.908152 0.469994 0.021 Uiso 1 1 calc R U . . .
C18 C 0.5073(2) 0.7601(2) 0.53529(16) 0.0165(6) Uani 1 1 d . . . . .
H18 H 0.500996 0.693851 0.573602 0.020 Uiso 1 1 calc R U . . .
C19 C 0.6349(3) 0.7381(3) 0.51299(18) 0.0222(7) Uani 1 1 d . . . . .
H19A H 0.668424 0.666880 0.492071 0.027 Uiso 1 1 calc R U . . .
H19B H 0.645873 0.803551 0.476551 0.027 Uiso 1 1 calc R U . . .
C20 C 0.6960(3) 0.7246(3) 0.5766(2) 0.0287(8) Uani 1 1 d . . . . .
H20A H 0.688399 0.656612 0.611823 0.034 Uiso 1 1 calc R U . . .
H20B H 0.778891 0.710987 0.561326 0.034 Uiso 1 1 calc R U . . .
C21 C 0.6458(3) 0.8321(3) 0.6105(2) 0.0289(8) Uani 1 1 d . . . . .
H21A H 0.660226 0.898715 0.576855 0.035 Uiso 1 1 calc R U . . .
H21B H 0.683717 0.819658 0.653261 0.035 Uiso 1 1 calc R U . . .
C22 C 0.5165(3) 0.8586(3) 0.6307(2) 0.0300(8) Uani 1 1 d . . . . .
H22A H 0.503138 0.796333 0.668979 0.036 Uiso 1 1 calc R U . . .
H22B H 0.484414 0.932043 0.649281 0.036 Uiso 1 1 calc R U . . .
C23 C 0.4538(3) 0.8688(3) 0.56825(18) 0.0222(7) Uani 1 1 d . . . . .
H23A H 0.371611 0.879721 0.584577 0.027 Uiso 1 1 calc R U . . .
H23B H 0.458429 0.937175 0.532298 0.027 Uiso 1 1 calc R U . . .
C24 C 0.3692(3) 0.7527(3) 0.17818(17) 0.0186(6) Uani 1 1 d . . . . .
C25 C 0.3253(3) 0.7974(3) 0.11284(18) 0.0247(7) Uani 1 1 d . . . . .
H25 H 0.255377 0.796697 0.100901 0.030 Uiso 1 1 calc R U . . .
C26 C 0.4052(3) 0.8436(3) 0.06849(19) 0.0286(8) Uani 1 1 d . . . . .
H26 H 0.400452 0.880227 0.020296 0.034 Uiso 1 1 calc R U . . .
C27 C 0.4931(3) 0.8253(3) 0.10900(17) 0.0211(7) Uani 1 1 d . . . . .
C28 C 0.5917(3) 0.8603(3) 0.08882(18) 0.0243(7) Uani 1 1 d . . . . .
H28 H 0.601902 0.899555 0.041639 0.029 Uiso 1 1 calc R U . . .
C29 C 0.7626(3) 0.8884(3) 0.0997(2) 0.0316(8) Uani 1 1 d . . . . .
H29 H 0.769750 0.897928 0.046902 0.038 Uiso 1 1 calc R U . . .
C30 C 0.8755(3) 0.8037(4) 0.1257(2) 0.0398(9) Uani 1 1 d . . . . .
H30A H 0.867393 0.789137 0.178102 0.048 Uiso 1 1 calc R U . . .
H30B H 0.892709 0.729081 0.110135 0.048 Uiso 1 1 calc R U . . .
C31 C 0.9752(4) 0.8500(4) 0.0975(2) 0.0512(12) Uani 1 1 d . . . . .
H31A H 1.045712 0.795178 0.117854 0.061 Uiso 1 1 calc R U . . .
H31B H 0.989323 0.855860 0.045376 0.061 Uiso 1 1 calc R U . . .
C32 C 0.9503(4) 0.9672(5) 0.1158(3) 0.0573(13) Uani 1 1 d . . . . .
H32A H 1.013503 0.997569 0.093155 0.069 Uiso 1 1 calc R U . . .
H32B H 0.947379 0.959271 0.167712 0.069 Uiso 1 1 calc R U . . .
C33 C 0.8370(4) 1.0529(4) 0.0915(3) 0.0548(12) Uani 1 1 d . . . . .
H33A H 0.843992 1.069900 0.039076 0.066 Uiso 1 1 calc R U . . .
H33B H 0.820292 1.126218 0.108440 0.066 Uiso 1 1 calc R U . . .
C34 C 0.7373(3) 1.0057(3) 0.1193(2) 0.0349(9) Uani 1 1 d . . . . .
H34A H 0.723523 0.998571 0.171490 0.042 Uiso 1 1 calc R U . . .
H34B H 0.666593 1.060882 0.099339 0.042 Uiso 1 1 calc R U . . .
C35 C 0.2115(3) 0.6713(3) 0.2405(2) 0.0264(7) Uani 1 1 d . . . . .
H35A H 0.151444 0.748052 0.231186 0.032 Uiso 1 1 calc R U . . .
H35B H 0.221747 0.632123 0.199933 0.032 Uiso 1 1 calc R U . . .
C36 C 0.1721(3) 0.5997(3) 0.3079(2) 0.0382(9) Uani 1 1 d . . . . .
H36A H 0.096612 0.596267 0.303846 0.057 Uiso 1 1 calc R U . . .
H36B H 0.166493 0.635676 0.348564 0.057 Uiso 1 1 calc R U . . .
H36C H 0.227757 0.521102 0.314689 0.057 Uiso 1 1 calc R U . . .
C37 C 1.0000(4) 0.4622(5) 0.2287(3) 0.0615(15) Uani 1 1 d . . . . .
H37 H 0.994216 0.538088 0.232554 0.074 Uiso 1 1 calc R U . . .
C38 C 1.0996(4) 0.3725(6) 0.2452(3) 0.0743(19) Uani 1 1 d . . . . .
H38 H 1.160451 0.386690 0.260213 0.089 Uiso 1 1 calc R U . . .
C39 C 1.1092(4) 0.2642(5) 0.2396(3) 0.0704(18) Uani 1 1 d . . . . .
H39 H 1.176831 0.201227 0.251089 0.085 Uiso 1 1 calc R U . . .
C40 C 1.0204(4) 0.2457(5) 0.2173(3) 0.0654(15) Uani 1 1 d . . . . .
H40 H 1.025692 0.170505 0.212361 0.078 Uiso 1 1 calc R U . . .
C41 C 0.9227(4) 0.3406(5) 0.2021(2) 0.0577(14) Uani 1 1 d . . . . .
H41 H 0.860697 0.328346 0.187056 0.069 Uiso 1 1 calc R U . . .
C47 C 0.7756(3) 0.9811(3) 0.3082(2) 0.0350(9) Uani 1 1 d . . . . .
H47 H 0.733935 1.057381 0.287009 0.042 Uiso 1 1 calc R U . . .
C48 C 0.8820(3) 0.9617(4) 0.3283(2) 0.0363(9) Uani 1 1 d . . . . .
H48 H 0.912716 1.023067 0.320162 0.044 Uiso 1 1 calc R U . . .
C49 C 0.9425(3) 0.8532(4) 0.3600(2) 0.0399(10) Uani 1 1 d . . . . .
H49 H 1.015661 0.837471 0.374716 0.048 Uiso 1 1 calc R U . . .
C50 C 0.8947(3) 0.7672(4) 0.3700(2) 0.0375(9) Uani 1 1 d . . . . .
H50 H 0.934204 0.690785 0.392138 0.045 Uiso 1 1 calc R U . . .
C51 C 0.7886(3) 0.7936(3) 0.34745(19) 0.0288(8) Uani 1 1 d . . . . .
H51 H 0.756845 0.733249 0.354191 0.035 Uiso 1 1 calc R U . . .
C52 C 0.3426(3) 1.0662(3) 0.1605(2) 0.0331(8) Uani 1 1 d . . . . .
H52 H 0.325287 0.996106 0.173012 0.040 Uiso 1 1 calc R U . . .
C53 C 0.3022(5) 1.1421(4) 0.1008(2) 0.0557(13) Uani 1 1 d . . . . .
H53 H 0.256616 1.125657 0.073367 0.067 Uiso 1 1 calc R U . . .
C54 C 0.3289(7) 1.2417(4) 0.0818(3) 0.099(3) Uani 1 1 d . . . . .
H54 H 0.303534 1.295157 0.040238 0.119 Uiso 1 1 calc R U . . .
C55 C 0.3924(7) 1.2635(4) 0.1233(3) 0.089(2) Uani 1 1 d . . . . .
H55 H 0.411581 1.332525 0.111145 0.107 Uiso 1 1 calc R U . . .
C56 C 0.4283(4) 1.1845(4) 0.1827(2) 0.0509(12) Uani 1 1 d . . . . .
H56 H 0.471718 1.200770 0.211669 0.061 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.872(2) . ?
U1 O2 2.377(2) 2_666 ?
U1 O2 1.936(2) . ?
U1 N1 2.470(3) . ?
U1 N2 2.573(2) . ?
U1 N3 2.479(2) . ?
U1 N4 2.568(2) . ?
K1 O1 2.927(2) . ?
K1 N1 3.029(3) . ?
K1 N5 2.748(2) . ?
K1 N6 3.014(3) . ?
K1 N7 2.902(3) . ?
K1 N8 2.86(3) . ?
K1 N8A 2.88(2) . ?
K1 N8B 2.993(16) . ?
K1 C2 3.376(3) . ?
K1 C4 3.490(3) . ?
K1 C5 3.081(3) . ?
K2 O1 2.806(2) . ?
K2 N3 3.035(3) . ?
K2 N5 2.807(3) . ?
K2 N6 3.091(3) . ?
K2 N9 2.979(3) . ?
K2 N10 2.821(3) . ?
K2 C13 3.391(3) . ?
K2 C16 3.160(3) . ?
N1 C2 1.345(4) . ?
N1 C5 1.399(4) . ?
N2 C6 1.283(4) . ?
N2 C7 1.473(4) . ?
N3 C13 1.349(4) . ?
N3 C16 1.400(4) . ?
N4 C17 1.290(4) . ?
N4 C18 1.468(4) . ?
N5 C24 1.357(4) . ?
N5 C27 1.370(4) . ?
N6 C28 1.288(4) . ?
N6 C29 1.466(4) . ?
N7 C37 1.331(6) . ?
N7 C41 1.332(7) . ?
N8 C42 1.341(14) . ?
N8 C46 1.336(14) . ?
N9 C47 1.329(5) . ?
N9 C51 1.335(5) . ?
N10 C52 1.331(5) . ?
N10 C56 1.332(5) . ?
N8A C46A 1.343(13) . ?
N8A C42A 1.354(13) . ?
N8B C42B 1.329(12) . ?
N8B C46B 1.319(12) . ?
C1 C2 1.526(4) . ?
C1 C13 1.519(4) . ?
C1 C24 1.513(4) . ?
C1 C35 1.556(4) . ?
C42 H42 0.9500 . ?
C42 C43 1.380(12) . ?
C43 H43 0.9500 . ?
C43 C44 1.374(12) . ?
C44 H44 0.9500 . ?
C44 C45 1.370(12) . ?
C45 H45 0.9500 . ?
C45 C46 1.385(12) . ?
C46 H46 0.9500 . ?
C46A H46A 0.9500 . ?
C46A C45A 1.372(12) . ?
C45A H45A 0.9500 . ?
C45A C44A 1.372(12) . ?
C44A H44A 0.9500 . ?
C44A C43A 1.361(11) . ?
C43A H43A 0.9500 . ?
C43A C42A 1.375(11) . ?
C42A H42A 0.9500 . ?
C42B H42B 0.9500 . ?
C42B C43B 1.372(11) . ?
C43B H43B 0.9500 . ?
C43B C44B 1.366(11) . ?
C44B H44B 0.9500 . ?
C44B C45B 1.360(11) . ?
C45B H45B 0.9500 . ?
C45B C46B 1.369(10) . ?
C46B H46B 0.9500 . ?
C2 C3 1.410(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.400(4) . ?
C4 H4 1.0000 . ?
C4 C5 1.379(4) . ?
C5 C6 1.432(4) . ?
C6 H6 0.9500 . ?
C7 H7 1.0000 . ?
C7 C8 1.525(4) . ?
C7 C12 1.527(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.534(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.523(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.530(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.530(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.411(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.386(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.399(4) . ?
C16 C17 1.417(4) . ?
C17 H17 0.9500 . ?
C18 H18 1.0000 . ?
C18 C19 1.520(4) . ?
C18 C23 1.524(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.520(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.519(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.527(5) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.525(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.397(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.401(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.393(5) . ?
C27 C28 1.418(5) . ?
C28 H28 0.9500 . ?
C29 H29 1.0000 . ?
C29 C30 1.527(5) . ?
C29 C34 1.517(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.526(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.506(7) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.522(7) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.532(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.526(5) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37 0.9500 . ?
C37 C38 1.380(6) . ?
C38 H38 0.9500 . ?
C38 C39 1.352(8) . ?
C39 H39 0.9500 . ?
C39 C40 1.375(8) . ?
C40 H40 0.9500 . ?
C40 C41 1.391(6) . ?
C41 H41 0.9500 . ?
C47 H47 0.9500 . ?
C47 C48 1.380(5) . ?
C48 H48 0.9500 . ?
C48 C49 1.365(6) . ?
C49 H49 0.9500 . ?
C49 C50 1.375(5) . ?
C50 H50 0.9500 . ?
C50 C51 1.379(5) . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
C52 C53 1.371(5) . ?
C53 H53 0.9500 . ?
C53 C54 1.365(8) . ?
C54 H54 0.9500 . ?
C54 C55 1.362(9) . ?
C55 H55 0.9500 . ?
C55 C56 1.369(7) . ?
C56 H56 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 177.33(8) . . ?
O1 U1 O2 110.70(8) . 2_666 ?
O1 U1 N1 86.04(9) . . ?
O1 U1 N2 83.47(8) . . ?
O1 U1 N3 86.77(8) . . ?
O1 U1 N4 86.11(8) . . ?
O2 U1 O2 71.95(8) . 2_666 ?
O2 U1 N1 91.96(8) . . ?
O2 U1 N1 140.69(7) 2_666 . ?
O2 U1 N2 78.79(7) 2_666 . ?
O2 U1 N2 97.41(8) . . ?
O2 U1 N3 141.88(8) 2_666 . ?
O2 U1 N3 90.91(8) . . ?
O2 U1 N4 94.26(8) . . ?
O2 U1 N4 79.40(7) 2_666 . ?
N1 U1 N2 67.75(8) . . ?
N1 U1 N3 71.24(8) . . ?
N1 U1 N4 138.74(8) . . ?
N3 U1 N2 138.35(8) . . ?
N3 U1 N4 67.92(8) . . ?
N4 U1 N2 150.63(8) . . ?
O1 K1 N1 60.34(6) . . ?
O1 K1 N6 100.91(7) . . ?
O1 K1 N8B 169.2(3) . . ?
O1 K1 C2 77.69(7) . . ?
O1 K1 C4 97.52(7) . . ?
O1 K1 C5 75.57(7) . . ?
N1 K1 C2 23.46(7) . . ?
N1 K1 C4 40.23(7) . . ?
N1 K1 C5 26.45(7) . . ?
N5 K1 O1 90.03(7) . . ?
N5 K1 N1 73.91(7) . . ?
N5 K1 N6 59.52(8) . . ?
N5 K1 N7 165.39(10) . . ?
N5 K1 N8 94.2(7) . . ?
N5 K1 N8A 91.7(4) . . ?
N5 K1 N8B 97.9(3) . . ?
N5 K1 C2 55.33(7) . . ?
N5 K1 C4 87.38(8) . . ?
N5 K1 C5 94.71(8) . . ?
N6 K1 N1 130.20(7) . . ?
N6 K1 C2 114.81(7) . . ?
N6 K1 C4 141.71(8) . . ?
N6 K1 C5 154.17(8) . . ?
N7 K1 O1 102.94(8) . . ?
N7 K1 N1 118.31(10) . . ?
N7 K1 N6 110.58(11) . . ?
N7 K1 N8B 70.2(3) . . ?
N7 K1 C2 133.63(11) . . ?
N7 K1 C4 97.41(11) . . ?
N7 K1 C5 95.04(11) . . ?
N8 K1 O1 171.3(8) . . ?
N8 K1 N1 113.6(7) . . ?
N8 K1 N6 87.8(8) . . ?
N8 K1 N7 73.9(7) . . ?
N8 K1 C2 98.5(7) . . ?
N8 K1 C4 75.1(7) . . ?
N8 K1 C5 96.5(8) . . ?
N8A K1 O1 170.3(5) . . ?
N8A K1 N1 111.0(4) . . ?
N8A K1 N6 88.2(5) . . ?
N8A K1 N7 76.7(4) . . ?
N8A K1 C2 95.5(4) . . ?
N8A K1 C4 73.0(5) . . ?
N8A K1 C5 94.7(5) . . ?
N8B K1 N1 114.8(3) . . ?
N8B K1 N6 89.5(3) . . ?
N8B K1 C2 100.8(3) . . ?
N8B K1 C4 75.6(3) . . ?
N8B K1 C5 96.4(3) . . ?
C2 K1 C4 38.32(7) . . ?
C5 K1 C2 39.38(7) . . ?
C5 K1 C4 23.18(8) . . ?
O1 K2 N3 62.16(6) . . ?
O1 K2 N5 91.37(7) . . ?
O1 K2 N6 101.87(7) . . ?
O1 K2 N9 80.39(8) . . ?
O1 K2 N10 173.76(8) . . ?
O1 K2 C13 79.32(7) . . ?
O1 K2 C16 76.81(7) . . ?
N3 K2 N6 129.71(8) . . ?
N3 K2 C13 23.40(7) . . ?
N3 K2 C16 26.02(7) . . ?
N5 K2 N3 74.21(7) . . ?
N5 K2 N6 57.99(8) . . ?
N5 K2 N9 139.99(8) . . ?
N5 K2 N10 87.31(8) . . ?
N5 K2 C13 55.40(8) . . ?
N5 K2 C16 94.59(8) . . ?
N6 K2 C13 113.39(8) . . ?
N6 K2 C16 152.58(8) . . ?
N9 K2 N3 131.45(8) . . ?
N9 K2 N6 85.31(8) . . ?
N9 K2 C13 154.82(8) . . ?
N9 K2 C16 120.82(8) . . ?
N10 K2 N3 111.63(8) . . ?
N10 K2 N6 82.60(8) . . ?
N10 K2 N9 104.48(9) . . ?
N10 K2 C13 94.94(8) . . ?
N10 K2 C16 97.21(8) . . ?
C16 K2 C13 39.20(8) . . ?
U1 O1 K1 116.40(9) . . ?
U1 O1 K2 117.15(9) . . ?
K2 O1 K1 76.58(6) . . ?
U1 O2 U1 108.04(8) . 2_666 ?
U1 N1 K1 96.41(8) . . ?
C2 N1 U1 138.3(2) . . ?
C2 N1 K1 92.92(18) . . ?
C2 N1 C5 106.1(3) . . ?
C5 N1 U1 115.52(19) . . ?
C5 N1 K1 78.88(17) . . ?
C6 N2 U1 114.71(19) . . ?
C6 N2 C7 122.2(2) . . ?
C7 N2 U1 122.99(19) . . ?
U1 N3 K2 93.11(8) . . ?
C13 N3 U1 138.53(19) . . ?
C13 N3 K2 93.30(18) . . ?
C13 N3 C16 106.9(2) . . ?
C16 N3 U1 114.59(19) . . ?
C16 N3 K2 82.00(16) . . ?
C17 N4 U1 114.6(2) . . ?
C17 N4 C18 122.6(3) . . ?
C18 N4 U1 122.79(17) . . ?
K1 N5 K2 79.52(7) . . ?
C24 N5 K1 127.02(19) . . ?
C24 N5 K2 125.48(19) . . ?
C24 N5 C27 106.2(3) . . ?
C27 N5 K1 105.36(18) . . ?
C27 N5 K2 110.35(19) . . ?
K1 N6 K2 71.17(6) . . ?
C28 N6 K1 99.4(2) . . ?
C28 N6 K2 102.8(2) . . ?
C28 N6 C29 116.6(3) . . ?
C29 N6 K1 129.8(2) . . ?
C29 N6 K2 126.9(2) . . ?
C37 N7 K1 126.8(3) . . ?
C37 N7 C41 117.1(4) . . ?
C41 N7 K1 113.8(3) . . ?
C42 N8 K1 112.4(17) . . ?
C46 N8 K1 126.5(18) . . ?
C46 N8 C42 119(2) . . ?
C47 N9 K2 139.5(3) . . ?
C47 N9 C51 116.3(3) . . ?
C51 N9 K2 104.0(2) . . ?
C52 N10 K2 105.8(2) . . ?
C52 N10 C56 117.2(4) . . ?
C56 N10 K2 131.8(3) . . ?
C46A N8A K1 134.5(13) . . ?
C46A N8A C42A 115.2(17) . . ?
C42A N8A K1 101.9(10) . . ?
C42B N8B K1 126.6(10) . . ?
C46B N8B K1 118.6(9) . . ?
C46B N8B C42B 114.8(14) . . ?
C2 C1 C35 107.6(2) . . ?
C13 C1 C2 118.1(2) . . ?
C13 C1 C35 108.0(3) . . ?
C24 C1 C2 105.4(2) . . ?
C24 C1 C13 106.1(2) . . ?
C24 C1 C35 111.6(3) . . ?
N8 C42 H42 118.6 . . ?
N8 C42 C43 122.8(18) . . ?
C43 C42 H42 118.6 . . ?
C42 C43 H43 121.5 . . ?
C44 C43 C42 117.1(14) . . ?
C44 C43 H43 121.5 . . ?
C43 C44 H44 119.5 . . ?
C45 C44 C43 120.9(14) . . ?
C45 C44 H44 119.5 . . ?
C44 C45 H45 120.6 . . ?
C44 C45 C46 118.8(14) . . ?
C46 C45 H45 120.6 . . ?
N8 C46 C45 121.0(18) . . ?
N8 C46 H46 119.5 . . ?
C45 C46 H46 119.5 . . ?
N8A C46A H46A 118.3 . . ?
N8A C46A C45A 123.4(14) . . ?
C45A C46A H46A 118.3 . . ?
C46A C45A H45A 120.1 . . ?
C44A C45A C46A 119.7(12) . . ?
C44A C45A H45A 120.1 . . ?
C45A C44A H44A 120.6 . . ?
C43A C44A C45A 118.7(12) . . ?
C43A C44A H44A 120.6 . . ?
C44A C43A H43A 120.8 . . ?
C44A C43A C42A 118.4(11) . . ?
C42A C43A H43A 120.8 . . ?
N8A C42A C43A 124.5(13) . . ?
N8A C42A H42A 117.7 . . ?
C43A C42A H42A 117.7 . . ?
N8B C42B H42B 117.6 . . ?
N8B C42B C43B 124.9(12) . . ?
C43B C42B H42B 117.6 . . ?
C42B C43B H43B 121.0 . . ?
C44B C43B C42B 118.1(11) . . ?
C44B C43B H43B 121.0 . . ?
C43B C44B H44B 120.7 . . ?
C45B C44B C43B 118.7(10) . . ?
C45B C44B H44B 120.7 . . ?
C44B C45B H45B 120.8 . . ?
C44B C45B C46B 118.4(10) . . ?
C46B C45B H45B 120.8 . . ?
N8B C46B C45B 125.1(12) . . ?
N8B C46B H46B 117.5 . . ?
C45B C46B H46B 117.5 . . ?
N1 C2 K1 63.63(16) . . ?
N1 C2 C1 126.7(3) . . ?
N1 C2 C3 110.3(3) . . ?
C1 C2 K1 107.17(18) . . ?
C3 C2 K1 90.5(2) . . ?
C3 C2 C1 122.6(3) . . ?
C2 C3 H3A 110.4 . . ?
C2 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
C4 C3 C2 106.8(3) . . ?
C4 C3 H3A 110.4 . . ?
C4 C3 H3B 110.4 . . ?
K1 C4 H4 126.3 . . ?
C3 C4 K1 86.1(2) . . ?
C3 C4 H4 126.3 . . ?
C5 C4 K1 61.53(17) . . ?
C5 C4 C3 106.2(3) . . ?
C5 C4 H4 126.3 . . ?
N1 C5 K1 74.66(16) . . ?
N1 C5 C6 119.5(3) . . ?
C4 C5 K1 95.3(2) . . ?
C4 C5 N1 110.5(3) . . ?
C4 C5 C6 129.9(3) . . ?
C6 C5 K1 95.26(18) . . ?
N2 C6 C5 122.3(3) . . ?
N2 C6 H6 118.8 . . ?
C5 C6 H6 118.8 . . ?
N2 C7 H7 107.1 . . ?
N2 C7 C8 115.3(3) . . ?
N2 C7 C12 109.3(2) . . ?
C8 C7 H7 107.1 . . ?
C8 C7 C12 110.7(3) . . ?
C12 C7 H7 107.1 . . ?
C7 C8 H8A 109.7 . . ?
C7 C8 H8B 109.7 . . ?
C7 C8 C9 109.7(3) . . ?
H8A C8 H8B 108.2 . . ?
C9 C8 H8A 109.7 . . ?
C9 C8 H8B 109.7 . . ?
C8 C9 H9A 109.4 . . ?
C8 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
C10 C9 C8 111.3(3) . . ?
C10 C9 H9A 109.4 . . ?
C10 C9 H9B 109.4 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 C11 110.7(3) . . ?
H10A C10 H10B 108.1 . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
C10 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 C10 111.4(3) . . ?
C12 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C7 C12 C11 110.9(3) . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 108.0 . . ?
N3 C13 K2 63.30(16) . . ?
N3 C13 C1 126.4(2) . . ?
N3 C13 C14 109.9(3) . . ?
C1 C13 K2 106.65(18) . . ?
C14 C13 K2 92.25(19) . . ?
C14 C13 C1 123.5(3) . . ?
C13 C14 H14 126.3 . . ?
C15 C14 C13 107.3(3) . . ?
C15 C14 H14 126.3 . . ?
C14 C15 H15 126.6 . . ?
C14 C15 C16 106.7(3) . . ?
C16 C15 H15 126.6 . . ?
N3 C16 K2 71.97(16) . . ?
N3 C16 C17 120.6(2) . . ?
C15 C16 K2 96.48(19) . . ?
C15 C16 N3 109.2(3) . . ?
C15 C16 C17 130.1(3) . . ?
C17 C16 K2 96.36(18) . . ?
N4 C17 C16 122.3(3) . . ?
N4 C17 H17 118.9 . . ?
C16 C17 H17 118.9 . . ?
N4 C18 H18 106.5 . . ?
N4 C18 C19 109.4(2) . . ?
N4 C18 C23 116.6(2) . . ?
C19 C18 H18 106.5 . . ?
C19 C18 C23 110.7(3) . . ?
C23 C18 H18 106.5 . . ?
C18 C19 H19A 109.6 . . ?
C18 C19 H19B 109.6 . . ?
H19A C19 H19B 108.1 . . ?
C20 C19 C18 110.2(3) . . ?
C20 C19 H19A 109.6 . . ?
C20 C19 H19B 109.6 . . ?
C19 C20 H20A 109.4 . . ?
C19 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
C21 C20 C19 111.0(3) . . ?
C21 C20 H20A 109.4 . . ?
C21 C20 H20B 109.4 . . ?
C20 C21 H21A 109.6 . . ?
C20 C21 H21B 109.6 . . ?
C20 C21 C22 110.3(3) . . ?
H21A C21 H21B 108.1 . . ?
C22 C21 H21A 109.6 . . ?
C22 C21 H21B 109.6 . . ?
C21 C22 H22A 109.1 . . ?
C21 C22 H22B 109.1 . . ?
H22A C22 H22B 107.9 . . ?
C23 C22 C21 112.4(3) . . ?
C23 C22 H22A 109.1 . . ?
C23 C22 H22B 109.1 . . ?
C18 C23 C22 110.2(3) . . ?
C18 C23 H23A 109.6 . . ?
C18 C23 H23B 109.6 . . ?
C22 C23 H23A 109.6 . . ?
C22 C23 H23B 109.6 . . ?
H23A C23 H23B 108.1 . . ?
N5 C24 C1 117.1(3) . . ?
N5 C24 C25 110.9(3) . . ?
C25 C24 C1 131.9(3) . . ?
C24 C25 H25 127.0 . . ?
C24 C25 C26 106.0(3) . . ?
C26 C25 H25 127.0 . . ?
C25 C26 H26 126.8 . . ?
C27 C26 C25 106.5(3) . . ?
C27 C26 H26 126.8 . . ?
N5 C27 C26 110.4(3) . . ?
N5 C27 C28 121.5(3) . . ?
C26 C27 C28 128.1(3) . . ?
N6 C28 C27 124.7(3) . . ?
N6 C28 H28 117.6 . . ?
C27 C28 H28 117.6 . . ?
N6 C29 H29 108.6 . . ?
N6 C29 C30 110.1(3) . . ?
N6 C29 C34 110.4(3) . . ?
C30 C29 H29 108.6 . . ?
C34 C29 H29 108.6 . . ?
C34 C29 C30 110.4(3) . . ?
C29 C30 H30A 109.3 . . ?
C29 C30 H30B 109.3 . . ?
H30A C30 H30B 107.9 . . ?
C31 C30 C29 111.7(3) . . ?
C31 C30 H30A 109.3 . . ?
C31 C30 H30B 109.3 . . ?
C30 C31 H31A 109.3 . . ?
C30 C31 H31B 109.3 . . ?
H31A C31 H31B 108.0 . . ?
C32 C31 C30 111.5(4) . . ?
C32 C31 H31A 109.3 . . ?
C32 C31 H31B 109.3 . . ?
C31 C32 H32A 109.3 . . ?
C31 C32 H32B 109.3 . . ?
C31 C32 C33 111.8(4) . . ?
H32A C32 H32B 107.9 . . ?
C33 C32 H32A 109.3 . . ?
C33 C32 H32B 109.3 . . ?
C32 C33 H33A 109.3 . . ?
C32 C33 H33B 109.3 . . ?
C32 C33 C34 111.7(4) . . ?
H33A C33 H33B 107.9 . . ?
C34 C33 H33A 109.3 . . ?
C34 C33 H33B 109.3 . . ?
C29 C34 C33 111.5(3) . . ?
C29 C34 H34A 109.3 . . ?
C29 C34 H34B 109.3 . . ?
C33 C34 H34A 109.3 . . ?
C33 C34 H34B 109.3 . . ?
H34A C34 H34B 108.0 . . ?
C1 C35 H35A 109.3 . . ?
C1 C35 H35B 109.3 . . ?
H35A C35 H35B 108.0 . . ?
C36 C35 C1 111.6(3) . . ?
C36 C35 H35A 109.3 . . ?
C36 C35 H35B 109.3 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N7 C37 H37 118.4 . . ?
N7 C37 C38 123.2(6) . . ?
C38 C37 H37 118.4 . . ?
C37 C38 H38 120.5 . . ?
C39 C38 C37 119.0(5) . . ?
C39 C38 H38 120.5 . . ?
C38 C39 H39 120.2 . . ?
C38 C39 C40 119.6(5) . . ?
C40 C39 H39 120.2 . . ?
C39 C40 H40 121.0 . . ?
C39 C40 C41 117.9(6) . . ?
C41 C40 H40 121.0 . . ?
N7 C41 C40 123.2(5) . . ?
N7 C41 H41 118.4 . . ?
C40 C41 H41 118.4 . . ?
N9 C47 H47 118.0 . . ?
N9 C47 C48 123.9(4) . . ?
C48 C47 H47 118.0 . . ?
C47 C48 H48 120.5 . . ?
C49 C48 C47 119.0(4) . . ?
C49 C48 H48 120.5 . . ?
C48 C49 H49 120.9 . . ?
C48 C49 C50 118.2(4) . . ?
C50 C49 H49 120.9 . . ?
C49 C50 H50 120.5 . . ?
C49 C50 C51 119.1(4) . . ?
C51 C50 H50 120.5 . . ?
N9 C51 C50 123.5(3) . . ?
N9 C51 H51 118.3 . . ?
C50 C51 H51 118.3 . . ?
N10 C52 H52 118.4 . . ?
N10 C52 C53 123.2(4) . . ?
C53 C52 H52 118.4 . . ?
C52 C53 H53 120.7 . . ?
C54 C53 C52 118.5(5) . . ?
C54 C53 H53 120.7 . . ?
C53 C54 H54 120.4 . . ?
C55 C54 C53 119.1(5) . . ?
C55 C54 H54 120.4 . . ?
C54 C55 H55 120.5 . . ?
C54 C55 C56 119.1(5) . . ?
C56 C55 H55 120.5 . . ?
N10 C56 C55 122.8(5) . . ?
N10 C56 H56 118.6 . . ?
C55 C56 H56 118.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 N1 C2 K1 103.0(3) . . . . ?
U1 N1 C2 C1 10.6(5) . . . . ?
U1 N1 C2 C3 -176.9(2) . . . . ?
U1 N1 C5 K1 -91.85(14) . . . . ?
U1 N1 C5 C4 178.2(2) . . . . ?
U1 N1 C5 C6 -4.5(4) . . . . ?
U1 N2 C6 C5 0.6(4) . . . . ?
U1 N2 C7 C8 173.1(2) . . . . ?
U1 N2 C7 C12 -61.5(3) . . . . ?
U1 N3 C13 K2 -98.5(3) . . . . ?
U1 N3 C13 C1 -6.9(5) . . . . ?
U1 N3 C13 C14 179.3(2) . . . . ?
U1 N3 C16 K2 89.77(13) . . . . ?
U1 N3 C16 C15 -179.54(19) . . . . ?
U1 N3 C16 C17 3.0(3) . . . . ?
U1 N4 C17 C16 -1.0(4) . . . . ?
U1 N4 C18 C19 56.1(3) . . . . ?
U1 N4 C18 C23 -177.3(2) . . . . ?
K1 N1 C2 C1 -92.4(3) . . . . ?
K1 N1 C2 C3 80.1(3) . . . . ?
K1 N1 C5 C4 -90.0(2) . . . . ?
K1 N1 C5 C6 87.4(3) . . . . ?
K1 N5 C24 C1 53.0(3) . . . . ?
K1 N5 C24 C25 -125.1(2) . . . . ?
K1 N5 C27 C26 137.4(2) . . . . ?
K1 N5 C27 C28 -45.1(3) . . . . ?
K1 N6 C28 C27 37.7(3) . . . . ?
K1 N6 C29 C30 -10.7(4) . . . . ?
K1 N6 C29 C34 -132.9(3) . . . . ?
K1 N7 C37 C38 160.8(4) . . . . ?
K1 N7 C41 C40 -163.6(4) . . . . ?
K1 N8 C42 C43 -165(2) . . . . ?
K1 N8 C46 C45 163(2) . . . . ?
K1 N8A C46A C45A 141.0(18) . . . . ?
K1 N8A C42A C43A -152.3(15) . . . . ?
K1 N8B C42B C43B -179.5(13) . . . . ?
K1 N8B C46B C45B 179.5(13) . . . . ?
K1 C2 C3 C4 60.8(3) . . . . ?
K1 C4 C5 N1 75.6(2) . . . . ?
K1 C4 C5 C6 -101.4(3) . . . . ?
K1 C5 C6 N2 78.0(3) . . . . ?
K2 N3 C13 C1 91.6(3) . . . . ?
K2 N3 C13 C14 -82.2(2) . . . . ?
K2 N3 C16 C15 90.7(2) . . . . ?
K2 N3 C16 C17 -86.7(3) . . . . ?
K2 N5 C24 C1 -52.0(3) . . . . ?
K2 N5 C24 C25 130.0(2) . . . . ?
K2 N5 C27 C26 -138.3(2) . . . . ?
K2 N5 C27 C28 39.2(3) . . . . ?
K2 N6 C28 C27 -35.0(4) . . . . ?
K2 N6 C29 C30 85.0(3) . . . . ?
K2 N6 C29 C34 -37.1(4) . . . . ?
K2 N9 C47 C48 -171.6(3) . . . . ?
K2 N9 C51 C50 175.0(3) . . . . ?
K2 N10 C52 C53 -158.0(3) . . . . ?
K2 N10 C56 C55 149.9(5) . . . . ?
K2 C13 C14 C15 -62.7(2) . . . . ?
K2 C16 C17 N4 -74.2(3) . . . . ?
O2 U1 O1 K1 135.23(8) 2_666 . . . ?
O2 U1 O1 K2 -136.87(8) 2_666 . . . ?
N1 U1 O1 K1 -8.18(9) . . . . ?
N1 U1 O1 K2 79.72(10) . . . . ?
N1 C2 C3 C4 -1.2(4) . . . . ?
N1 C5 C6 N2 2.7(5) . . . . ?
N2 U1 O1 K1 59.86(9) . . . . ?
N2 U1 O1 K2 147.76(11) . . . . ?
N2 C7 C8 C9 -177.1(3) . . . . ?
N2 C7 C12 C11 174.7(3) . . . . ?
N3 U1 O1 K1 -79.58(9) . . . . ?
N3 U1 O1 K2 8.32(10) . . . . ?
N3 C13 C14 C15 -0.3(4) . . . . ?
N3 C16 C17 N4 -1.4(4) . . . . ?
N4 U1 O1 K1 -147.64(9) . . . . ?
N4 U1 O1 K2 -59.74(10) . . . . ?
N4 C18 C19 C20 -171.3(2) . . . . ?
N4 C18 C23 C22 177.5(3) . . . . ?
N5 C24 C25 C26 0.6(4) . . . . ?
N5 C27 C28 N6 1.2(5) . . . . ?
N6 C29 C30 C31 -178.0(3) . . . . ?
N6 C29 C34 C33 177.2(3) . . . . ?
N7 C37 C38 C39 0.3(8) . . . . ?
N8 C42 C43 C44 -1(2) . . . . ?
N9 C47 C48 C49 -1.2(6) . . . . ?
N10 C52 C53 C54 1.4(7) . . . . ?
N8A C46A C45A C44A 0.6(18) . . . . ?
N8B C42B C43B C44B -1.3(18) . . . . ?
C1 C2 C3 C4 171.6(3) . . . . ?
C1 C13 C14 C15 -174.4(3) . . . . ?
C1 C24 C25 C26 -177.0(3) . . . . ?
C42 N8 C46 C45 -1(4) . . . . ?
C42 C43 C44 C45 1(4) . . . . ?
C43 C44 C45 C46 -1(5) . . . . ?
C44 C45 C46 N8 1(4) . . . . ?
C46 N8 C42 C43 0(2) . . . . ?
C46A N8A C42A C43A 1(2) . . . . ?
C46A C45A C44A C43A -1(3) . . . . ?
C45A C44A C43A C42A 1(3) . . . . ?
C44A C43A C42A N8A -1(3) . . . . ?
C42A N8A C46A C45A -0.4(18) . . . . ?
C42B N8B C46B C45B -2(3) . . . . ?
C42B C43B C44B C45B 0(2) . . . . ?
C43B C44B C45B C46B 0(3) . . . . ?
C44B C45B C46B N8B 1(3) . . . . ?
C46B N8B C42B C43B 1.9(17) . . . . ?
C2 N1 C5 K1 89.8(2) . . . . ?
C2 N1 C5 C4 -0.1(4) . . . . ?
C2 N1 C5 C6 177.2(3) . . . . ?
C2 C1 C13 K2 75.8(3) . . . . ?
C2 C1 C13 N3 7.0(5) . . . . ?
C2 C1 C13 C14 -179.9(3) . . . . ?
C2 C1 C24 N5 -61.9(3) . . . . ?
C2 C1 C24 C25 115.6(4) . . . . ?
C2 C1 C35 C36 61.5(4) . . . . ?
C2 C3 C4 K1 -57.8(3) . . . . ?
C2 C3 C4 C5 1.0(4) . . . . ?
C3 C4 C5 K1 -76.2(3) . . . . ?
C3 C4 C5 N1 -0.6(4) . . . . ?
C3 C4 C5 C6 -177.6(3) . . . . ?
C4 C5 C6 N2 179.4(3) . . . . ?
C5 N1 C2 K1 -79.3(2) . . . . ?
C5 N1 C2 C1 -171.7(3) . . . . ?
C5 N1 C2 C3 0.8(4) . . . . ?
C6 N2 C7 C8 -10.7(4) . . . . ?
C6 N2 C7 C12 114.7(3) . . . . ?
C7 N2 C6 C5 -175.9(3) . . . . ?
C7 C8 C9 C10 -58.1(4) . . . . ?
C8 C7 C12 C11 -57.2(4) . . . . ?
C8 C9 C10 C11 56.3(4) . . . . ?
C9 C10 C11 C12 -54.7(4) . . . . ?
C10 C11 C12 C7 55.3(4) . . . . ?
C12 C7 C8 C9 58.2(4) . . . . ?
C13 N3 C16 K2 -91.0(2) . . . . ?
C13 N3 C16 C15 -0.3(3) . . . . ?
C13 N3 C16 C17 -177.8(3) . . . . ?
C13 C1 C2 K1 -78.3(3) . . . . ?
C13 C1 C2 N1 -8.8(5) . . . . ?
C13 C1 C2 C3 179.6(3) . . . . ?
C13 C1 C24 N5 64.1(3) . . . . ?
C13 C1 C24 C25 -118.4(4) . . . . ?
C13 C1 C35 C36 -67.0(3) . . . . ?
C13 C14 C15 C16 0.1(4) . . . . ?
C14 C15 C16 K2 73.3(2) . . . . ?
C14 C15 C16 N3 0.2(4) . . . . ?
C14 C15 C16 C17 177.3(3) . . . . ?
C15 C16 C17 N4 -178.2(3) . . . . ?
C16 N3 C13 K2 82.6(2) . . . . ?
C16 N3 C13 C1 174.2(3) . . . . ?
C16 N3 C13 C14 0.4(3) . . . . ?
C17 N4 C18 C19 -121.8(3) . . . . ?
C17 N4 C18 C23 4.8(4) . . . . ?
C18 N4 C17 C16 177.1(3) . . . . ?
C18 C19 C20 C21 -58.7(4) . . . . ?
C19 C18 C23 C22 -56.5(4) . . . . ?
C19 C20 C21 C22 56.0(4) . . . . ?
C20 C21 C22 C23 -54.5(4) . . . . ?
C21 C22 C23 C18 54.8(4) . . . . ?
C23 C18 C19 C20 58.8(3) . . . . ?
C24 N5 C27 C26 0.5(3) . . . . ?
C24 N5 C27 C28 178.0(3) . . . . ?
C24 C1 C2 K1 40.0(2) . . . . ?
C24 C1 C2 N1 109.5(3) . . . . ?
C24 C1 C2 C3 -62.1(4) . . . . ?
C24 C1 C13 K2 -42.2(2) . . . . ?
C24 C1 C13 N3 -110.9(3) . . . . ?
C24 C1 C13 C14 62.1(4) . . . . ?
C24 C1 C35 C36 176.7(3) . . . . ?
C24 C25 C26 C27 -0.3(4) . . . . ?
C25 C26 C27 N5 -0.1(4) . . . . ?
C25 C26 C27 C28 -177.4(3) . . . . ?
C26 C27 C28 N6 178.2(3) . . . . ?
C27 N5 C24 C1 177.3(3) . . . . ?
C27 N5 C24 C25 -0.7(3) . . . . ?
C28 N6 C29 C30 -141.6(3) . . . . ?
C28 N6 C29 C34 96.2(4) . . . . ?
C29 N6 C28 C27 -178.3(3) . . . . ?
C29 C30 C31 C32 55.4(5) . . . . ?
C30 C29 C34 C33 55.3(4) . . . . ?
C30 C31 C32 C33 -54.0(5) . . . . ?
C31 C32 C33 C34 53.6(5) . . . . ?
C32 C33 C34 C29 -54.5(5) . . . . ?
C34 C29 C30 C31 -55.9(4) . . . . ?
C35 C1 C2 K1 159.2(2) . . . . ?
C35 C1 C2 N1 -131.2(3) . . . . ?
C35 C1 C2 C3 57.2(4) . . . . ?
C35 C1 C13 K2 -161.99(18) . . . . ?
C35 C1 C13 N3 129.2(3) . . . . ?
C35 C1 C13 C14 -57.7(4) . . . . ?
C35 C1 C24 N5 -178.5(3) . . . . ?
C35 C1 C24 C25 -0.9(5) . . . . ?
C37 N7 C41 C40 0.2(7) . . . . ?
C37 C38 C39 C40 0.5(8) . . . . ?
C38 C39 C40 C41 -0.9(8) . . . . ?
C39 C40 C41 N7 0.6(7) . . . . ?
C41 N7 C37 C38 -0.6(7) . . . . ?
C47 N9 C51 C50 0.1(5) . . . . ?
C47 C48 C49 C50 0.5(6) . . . . ?
C48 C49 C50 C51 0.4(6) . . . . ?
C49 C50 C51 N9 -0.7(6) . . . . ?
C51 N9 C47 C48 0.9(5) . . . . ?
C52 N10 C56 C55 -0.8(7) . . . . ?
C52 C53 C54 C55 -1.3(9) . . . . ?
C53 C54 C55 C56 0.4(10) . . . . ?
C54 C55 C56 N10 0.8(9) . . . . ?
C56 N10 C52 C53 -0.3(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.282
_oxdiff_exptl_absorpt_empirical_full_min 0.713
_vrf_PLAT220_to506_2_refinalised 
;
PROBLEM: NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        6.1 Ratio 
RESPONSE: Pyridine ligand disordered over three positions
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Pyridene, hexane'
####################################################################### 
# 
# 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_mo_jl23016_0m
_database_code_depnum_ccdc_archive 'CCDC 2313503'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2023-12-11 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_audit_creation_date             2023-09-04
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C87 H109 N15 O4 U2 Zn2'
_chemical_formula_sum            'C87 H109 N15 O4 U2 Zn2'
_chemical_formula_weight         2035.69
_chemical_melting_point          ?
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.3634(6)
_cell_length_b                   18.9972(7)
_cell_length_c                   15.4266(6)
_cell_angle_alpha                90
_cell_angle_beta                 100.975(2)
_cell_angle_gamma                90
_cell_volume                     4132.4(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9385
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      32.499
_cell_measurement_theta_min      2.586
_shelx_estimated_absorpt_T_max   0.815
_shelx_estimated_absorpt_T_min   0.427
_exptl_absorpt_coefficient_mu    4.540
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.5516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0886 before and 0.0493 after correction.
The Ratio of minimum to maximum transmission is 0.7390.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       slab
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.047
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            196713
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.620
_diffrn_reflns_theta_min         2.144
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12811
_reflns_number_total             15026
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.927
_refine_diff_density_min         -2.158
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         15026
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0230
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0173P)²+6.4586P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0513
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: N2(0.5) C7(0.5) C5(0.5) H5(0.5) C6(0.5) H6(0.5) C8(0.5) H8(0.5)
 C9(0.5) H9(0.5) N52(0.5) C53(0.5) H53(0.5) C54(0.5) H54(0.5) C55(0.5) H55(0.5)
 CXF(0.5) HXF(0.5) C24(0.5) H24(0.5) C14(0.5) H14A(0.5) H14B(0.5) C13(0.5)
 H13A(0.5) H13B(0.5) C11(0.5) H11A(0.5) H11B(0.5) C12(0.5) H12A(0.5) H12B(0.5)
 C10(0.5) H10A(0.5) H10B(0.5) C19(0.5) H19(0.5) N3(0.5) C23(0.5) H23A(0.5)
 H23B(0.5) C52(0.5) H52A(0.5) H52B(0.5) C20(0.5) H20A(0.5) H20B(0.5) C21(0.5)
 H21A(0.5) H21B(0.5) C18(0.5) H18(0.5) C22(0.5) H22A(0.5) H22B(0.5) C17(0.5)
 C16(0.5) H16(0.5) C15(0.5) H15(0.5)
3.a Ternary CH refined with riding coordinates:
 C41(H41), C30(H30), C24(H24), C19(H19)
3.b Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C35(H35A,H35B), C31(H31A,H31B), C2(H2A,H2B), C34(H34A,H34B),
 C42(H42A,H42B), C45(H45A,H45B), C32(H32A,H32B), C43(H43A,H43B), C44(H44A,H44B),
  C33(H33A,H33B), C14(H14A,H14B), C13(H13A,H13B), C11(H11A,H11B), C12(H12A,
 H12B), C10(H10A,H10B), C23(H23A,H23B), C52(H52A,H52B), C20(H20A,H20B),
 C21(H21A,H21B), C22(H22A,H22B)
3.c Aromatic/amide H refined with riding coordinates:
 C29(H29), C26(H26), C40(H40), C27(H27), C37(H37), C38(H38), C51(H51),
 C47(H47), C5(H5), C50(H50), C6(H6), C49(H49), C48(H48), C8(H8), C9(H9),
 C53(H53), C54(H54), C55(H55), CXF(HXF), C18(H18), C16(H16), C15(H15)
3.d Fitted hexagon refined as free rotating group:
 C9(N52,C53,C54,C55,CXF)
3.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.41571(2) 0.54788(2) 0.54298(2) 0.01218(2) Uani 1 1 d . . . . .
Zn1 Zn 0.25595(2) 0.62756(2) 0.64781(2) 0.02972(6) Uani 1 1 d . . . . .
N5 N 0.55053(12) 0.57117(9) 0.67380(11) 0.0165(3) Uani 1 1 d . . . . .
N4 N 0.43659(12) 0.67415(8) 0.57307(11) 0.0163(3) Uani 1 1 d . . . . .
N6 N 0.28770(11) 0.61203(8) 0.44759(10) 0.0155(3) Uani 1 1 d . . . . .
N7 N 0.29243(12) 0.46394(8) 0.45706(11) 0.0158(3) Uani 1 1 d . . . . .
C25 C 0.40327(14) 0.73548(10) 0.53388(13) 0.0184(4) Uani 1 1 d . . . . .
C41 C 0.29323(14) 0.38679(10) 0.46835(13) 0.0175(3) Uani 1 1 d . . . . .
H41 H 0.353983 0.369378 0.453464 0.021 Uiso 1 1 calc R U . . .
N8 N 0.35458(14) 0.67074(11) 0.75554(14) 0.0277(4) Uani 1 1 d . . . . .
N1 N 0.21127(13) 0.71653(10) 0.58653(12) 0.0230(4) Uani 1 1 d . . . . .
C29 C 0.57105(14) 0.63693(11) 0.68589(13) 0.0179(3) Uani 1 1 d . . . . .
H29 H 0.622888 0.650041 0.730949 0.021 Uiso 1 1 calc R U . . .
C30 C 0.60571(14) 0.51610(10) 0.72867(13) 0.0175(3) Uani 1 1 d . . . . .
H30 H 0.634737 0.485851 0.687876 0.021 Uiso 1 1 calc R U . . .
C28 C 0.51818(14) 0.69055(10) 0.63360(13) 0.0169(3) Uani 1 1 d . . . . .
C36 C 0.26510(14) 0.67939(10) 0.42339(12) 0.0175(3) Uani 1 1 d . . . . .
C26 C 0.46399(16) 0.79128(11) 0.56943(14) 0.0216(4) Uani 1 1 d . . . . .
H26 H 0.456657 0.839484 0.553181 0.026 Uiso 1 1 calc R U . . .
C40 C 0.22537(13) 0.49509(10) 0.40294(12) 0.0168(3) Uani 1 1 d . . . . .
H40 H 0.176800 0.467497 0.368504 0.020 Uiso 1 1 calc R U . . .
C3 C 0.30822(14) 0.74426(10) 0.47346(13) 0.0181(4) Uani 1 1 d . . . . .
C46 C 0.29588(16) 0.36853(12) 0.56502(14) 0.0241(4) Uani 1 1 d . . . . .
H46A H 0.349718 0.393107 0.602499 0.029 Uiso 1 1 calc R U . . .
H46B H 0.236605 0.384640 0.582615 0.029 Uiso 1 1 calc R U . . .
C27 C 0.53618(15) 0.76282(11) 0.63234(14) 0.0212(4) Uani 1 1 d . . . . .
H27 H 0.587447 0.787463 0.667428 0.025 Uiso 1 1 calc R U . . .
C39 C 0.22228(14) 0.56975(11) 0.39351(12) 0.0172(3) Uani 1 1 d . . . . .
C37 C 0.18670(16) 0.68076(11) 0.35366(13) 0.0229(4) Uani 1 1 d . . . . .
H37 H 0.157681 0.721492 0.324588 0.027 Uiso 1 1 calc R U . . .
C35 C 0.53961(15) 0.46888(12) 0.76954(15) 0.0243(4) Uani 1 1 d . . . . .
H35A H 0.488499 0.450715 0.722588 0.029 Uiso 1 1 calc R U . . .
H35B H 0.509951 0.496584 0.811390 0.029 Uiso 1 1 calc R U . . .
C31 C 0.68699(15) 0.54275(11) 0.79971(13) 0.0218(4) Uani 1 1 d . . . . .
H31A H 0.661318 0.573203 0.841653 0.026 Uiso 1 1 calc R U . . .
H31B H 0.730908 0.571325 0.771890 0.026 Uiso 1 1 calc R U . . .
C2 C 0.31488(17) 0.80313(11) 0.40566(15) 0.0258(4) Uani 1 1 d . . . . .
H2A H 0.250677 0.812955 0.371292 0.031 Uiso 1 1 calc R U . . .
H2B H 0.338620 0.846684 0.437618 0.031 Uiso 1 1 calc R U . . .
C4 C 0.23889(15) 0.76511(11) 0.53248(13) 0.0206(4) Uani 1 1 d . . . . .
C38 C 0.15934(15) 0.61128(11) 0.33501(13) 0.0215(4) Uani 1 1 d . . . . .
H38 H 0.108025 0.595335 0.291169 0.026 Uiso 1 1 calc R U . . .
N2 N 0.1413(3) 0.6592(2) 0.7210(3) 0.0160(7) Uani 0.5 1 d . . P A 1
C34 C 0.59506(17) 0.40708(13) 0.81825(18) 0.0314(5) Uani 1 1 d . . . . .
H34A H 0.551654 0.377451 0.845392 0.038 Uiso 1 1 calc R U . . .
H34B H 0.621120 0.377692 0.775523 0.038 Uiso 1 1 calc R U . . .
C51 C 0.37486(19) 0.73968(14) 0.75903(17) 0.0329(5) Uani 1 1 d . . . . .
H51 H 0.341704 0.769936 0.714618 0.040 Uiso 1 1 calc R U . . .
C42 C 0.21340(16) 0.34733(11) 0.40889(14) 0.0228(4) Uani 1 1 d . . . . .
H42A H 0.214804 0.358120 0.346371 0.027 Uiso 1 1 calc R U . . .
H42B H 0.151645 0.363342 0.421260 0.027 Uiso 1 1 calc R U . . .
C45 C 0.3067(2) 0.28933(14) 0.57920(19) 0.0405(7) Uani 1 1 d . . . . .
H45A H 0.368458 0.274015 0.566242 0.049 Uiso 1 1 calc R U . . .
H45B H 0.306024 0.278175 0.641770 0.049 Uiso 1 1 calc R U . . .
C32 C 0.74117(16) 0.48108(12) 0.84983(14) 0.0264(4) Uani 1 1 d . . . . .
H32A H 0.772354 0.453553 0.808913 0.032 Uiso 1 1 calc R U . . .
H32B H 0.791237 0.499604 0.897473 0.032 Uiso 1 1 calc R U . . .
C43 C 0.22290(18) 0.26795(12) 0.42371(17) 0.0293(5) Uani 1 1 d . . . . .
H43A H 0.168083 0.243871 0.387002 0.035 Uiso 1 1 calc R U . . .
H43B H 0.281245 0.251110 0.404983 0.035 Uiso 1 1 calc R U . . .
C47 C 0.40215(17) 0.62922(15) 0.8188(2) 0.0373(6) Uani 1 1 d . . . . .
H47 H 0.388677 0.580227 0.816339 0.045 Uiso 1 1 calc R U . . .
C44 C 0.2272(2) 0.24932(13) 0.52014(18) 0.0362(6) Uani 1 1 d . . . . .
H44A H 0.237819 0.198077 0.528520 0.043 Uiso 1 1 calc R U . . .
H44B H 0.165877 0.261046 0.537043 0.043 Uiso 1 1 calc R U . . .
C7 C 0.1499(8) 0.7594(3) 0.6307(7) 0.0168(14) Uani 0.5 1 d . . P A 1
C5 C 0.1999(10) 0.8362(6) 0.5390(9) 0.0193(15) Uani 0.5 1 d . . P A 1
H5 H 0.209127 0.877037 0.506061 0.023 Uiso 0.5 1 calc R U P A 1
C1 C 0.3802(2) 0.78357(15) 0.34240(17) 0.0374(6) Uani 1 1 d . . . . .
H1A H 0.382676 0.822551 0.301297 0.056 Uiso 1 1 calc R U . . .
H1B H 0.355832 0.741345 0.309153 0.056 Uiso 1 1 calc R U . . .
H1C H 0.444009 0.774229 0.376025 0.056 Uiso 1 1 calc R U . . .
C33 C 0.67578(19) 0.43307(14) 0.88968(16) 0.0322(5) Uani 1 1 d . . . . .
H33A H 0.649576 0.459058 0.935243 0.039 Uiso 1 1 calc R U . . .
H33B H 0.712192 0.392359 0.918442 0.039 Uiso 1 1 calc R U . . .
C50 C 0.4430(2) 0.76799(17) 0.82580(19) 0.0426(7) Uani 1 1 d . . . . .
H50 H 0.456403 0.816977 0.826553 0.051 Uiso 1 1 calc R U . . .
C6 C 0.1460(5) 0.8295(3) 0.6051(5) 0.0208(12) Uani 0.5 1 d . . P A 1
H6 H 0.112909 0.866171 0.628252 0.025 Uiso 0.5 1 calc R U P A 1
C49 C 0.4911(2) 0.72491(19) 0.89091(19) 0.0462(8) Uani 1 1 d . . . . .
H49 H 0.537796 0.743498 0.937203 0.055 Uiso 1 1 calc R U . . .
C48 C 0.46988(19) 0.65429(19) 0.8873(2) 0.0454(7) Uani 1 1 d . . . . .
H48 H 0.501482 0.623172 0.931516 0.054 Uiso 1 1 calc R U . . .
C8 C 0.1148(3) 0.7226(3) 0.6987(3) 0.0164(8) Uani 0.5 1 d . . P A 1
H8 H 0.070946 0.745478 0.728234 0.020 Uiso 0.5 1 calc R U P A 1
C9 C 0.05511(19) 0.59791(12) 0.51459(18) 0.0245(8) Uani 0.5 1 d G . P A -1
H9 H 0.058352 0.646950 0.503460 0.029 Uiso 0.5 1 calc R U P A -1
N52 N 0.13022(14) 0.56435(12) 0.56910(16) 0.0163(6) Uani 0.5 1 d G . P A -1
C53 C 0.12548(18) 0.49260(12) 0.58538(17) 0.0219(8) Uani 0.5 1 d G . P A -1
H53 H 0.176815 0.469668 0.622639 0.026 Uiso 0.5 1 calc R U P A -1
C54 C 0.0456(2) 0.45442(11) 0.5472(2) 0.0287(12) Uani 0.5 1 d G . P A -1
H54 H 0.042381 0.405380 0.558293 0.034 Uiso 0.5 1 calc R U P A -1
C55 C -0.0295(2) 0.48798(18) 0.4927(2) 0.0301(10) Uani 0.5 1 d G . P A -1
H55 H -0.084069 0.461876 0.466531 0.036 Uiso 0.5 1 calc R U P A -1
CXF C -0.02475(17) 0.55972(18) 0.4764(2) 0.0295(12) Uani 0.5 1 d G . P A -1
HXF H -0.076085 0.582661 0.439114 0.035 Uiso 0.5 1 calc R U P A -1
C24 C 0.1020(3) 0.6227(2) 0.7893(2) 0.0157(7) Uani 0.5 1 d . . P A 1
H24 H 0.086376 0.658435 0.832009 0.019 Uiso 0.5 1 calc R U P A 1
C14 C 0.0106(3) 0.5833(2) 0.7485(2) 0.0169(7) Uani 0.5 1 d . . P A 1
H14A H -0.036800 0.617314 0.718048 0.020 Uiso 0.5 1 calc R U P A 1
H14B H 0.024533 0.549250 0.704052 0.020 Uiso 0.5 1 calc R U P A 1
C13 C -0.0302(3) 0.5443(2) 0.8191(3) 0.0219(8) Uani 0.5 1 d . . P A 1
H13A H -0.048035 0.578615 0.861345 0.026 Uiso 0.5 1 calc R U P A 1
H13B H -0.088232 0.518694 0.791032 0.026 Uiso 0.5 1 calc R U P A 1
C11 C 0.1343(4) 0.5301(3) 0.9087(3) 0.0302(10) Uani 0.5 1 d . . P A 1
H11A H 0.122457 0.562798 0.955404 0.036 Uiso 0.5 1 calc R U P A 1
H11B H 0.181483 0.494858 0.936468 0.036 Uiso 0.5 1 calc R U P A 1
C12 C 0.0413(4) 0.4924(2) 0.8683(3) 0.0297(10) Uani 0.5 1 d . . P A 1
H12A H 0.054416 0.455321 0.827185 0.036 Uiso 0.5 1 calc R U P A 1
H12B H 0.014525 0.469531 0.915808 0.036 Uiso 0.5 1 calc R U P A 1
C10 C 0.1743(3) 0.5710(3) 0.8395(3) 0.0243(8) Uani 0.5 1 d . . P A 1
H10A H 0.194013 0.537622 0.797162 0.029 Uiso 0.5 1 calc R U P A 1
H10B H 0.231304 0.597283 0.868667 0.029 Uiso 0.5 1 calc R U P A 1
O2 O 0.49402(9) 0.55554(7) 0.45397(9) 0.0151(2) Uani 1 1 d . . . . .
O1 O 0.33497(10) 0.54658(7) 0.62956(9) 0.0157(2) Uani 1 1 d . . . . .
C19 C 0.1009(3) 0.5830(3) 0.7634(3) 0.0290(10) Uani 0.5 1 d . . P A 2
H19 H 0.030359 0.582332 0.744042 0.035 Uiso 0.5 1 calc R U P A 2
N3 N 0.1423(3) 0.6300(3) 0.7041(3) 0.0240(8) Uani 0.5 1 d . . P A 2
C23 C 0.0863(4) 0.5607(3) 0.9210(4) 0.0366(11) Uani 0.5 1 d . . P A 2
H23A H 0.105974 0.578561 0.982045 0.044 Uiso 0.5 1 calc R U P A 2
H23B H 0.016153 0.560386 0.906437 0.044 Uiso 0.5 1 calc R U P A 2
C52 C 0.1251(4) 0.6093(2) 0.8566(3) 0.0280(9) Uani 0.5 1 d . . P A 2
H52A H 0.098462 0.657119 0.859654 0.034 Uiso 0.5 1 calc R U P A 2
H52B H 0.194923 0.612696 0.874702 0.034 Uiso 0.5 1 calc R U P A 2
C20 C 0.1395(5) 0.5077(3) 0.7584(3) 0.0396(13) Uani 0.5 1 d . . P A 2
H20A H 0.120649 0.489724 0.697314 0.048 Uiso 0.5 1 calc R U P A 2
H20B H 0.209691 0.508676 0.773215 0.048 Uiso 0.5 1 calc R U P A 2
C21 C 0.1018(6) 0.4583(3) 0.8220(4) 0.0484(16) Uani 0.5 1 d . . P A 2
H21A H 0.032436 0.452527 0.802756 0.058 Uiso 0.5 1 calc R U P A 2
H21B H 0.131712 0.411429 0.821074 0.058 Uiso 0.5 1 calc R U P A 2
C18 C 0.1043(4) 0.6907(3) 0.6850(4) 0.0275(10) Uani 0.5 1 d . . P A 2
H18 H 0.050466 0.704692 0.708206 0.033 Uiso 0.5 1 calc R U P A 2
C22 C 0.1231(5) 0.4876(3) 0.9151(3) 0.0377(12) Uani 0.5 1 d . . P A 2
H22A H 0.094376 0.456467 0.954211 0.045 Uiso 0.5 1 calc R U P A 2
H22B H 0.192555 0.487603 0.936557 0.045 Uiso 0.5 1 calc R U P A 2
C17 C 0.1441(9) 0.7373(4) 0.6280(9) 0.029(2) Uani 0.5 1 d . . P A 2
C16 C 0.1246(6) 0.8066(4) 0.6004(6) 0.0343(16) Uani 0.5 1 d . . P A 2
H16 H 0.078475 0.837144 0.616639 0.041 Uiso 0.5 1 calc R U P A 2
C15 C 0.1875(13) 0.8215(7) 0.5434(12) 0.035(3) Uani 0.5 1 d . . P A 2
H15 H 0.192585 0.865880 0.516290 0.043 Uiso 0.5 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 U1 3.48623(15) 3_666 ?
U1 N5 2.5555(16) . ?
U1 N4 2.4510(16) . ?
U1 N6 2.4497(16) . ?
U1 N7 2.5575(16) . ?
U1 O2 1.9390(13) . ?
U1 O2 2.3495(13) 3_666 ?
U1 O1 1.9284(13) . ?
Zn1 N8 2.132(2) . ?
Zn1 N1 1.983(2) . ?
Zn1 N2 2.249(4) . ?
Zn1 N52 2.3114(18) . ?
Zn1 O1 1.9636(13) . ?
Zn1 N3 1.990(4) . ?
N5 C29 1.289(3) . ?
N5 C30 1.478(3) . ?
N4 C25 1.357(2) . ?
N4 C28 1.388(3) . ?
N6 C36 1.355(2) . ?
N6 C39 1.388(2) . ?
N7 C41 1.476(2) . ?
N7 C40 1.292(2) . ?
C25 C26 1.415(3) . ?
C25 C3 1.509(3) . ?
C41 H41 1.0000 . ?
C41 C46 1.525(3) . ?
C41 C42 1.522(3) . ?
N8 C51 1.341(3) . ?
N8 C47 1.336(3) . ?
N1 C4 1.353(3) . ?
N1 C7 1.460(10) . ?
N1 C17 1.316(13) . ?
C29 H29 0.9500 . ?
C29 C28 1.425(3) . ?
C30 H30 1.0000 . ?
C30 C35 1.527(3) . ?
C30 C31 1.527(3) . ?
C28 C27 1.398(3) . ?
C36 C3 1.522(3) . ?
C36 C37 1.402(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.388(3) . ?
C40 H40 0.9500 . ?
C40 C39 1.426(3) . ?
C3 C2 1.546(3) . ?
C3 C4 1.524(3) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C45 1.524(3) . ?
C27 H27 0.9500 . ?
C39 C38 1.394(3) . ?
C37 H37 0.9500 . ?
C37 C38 1.392(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C34 1.533(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.532(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.523(3) . ?
C4 C5 1.474(13) . ?
C4 C15 1.330(18) . ?
C38 H38 0.9500 . ?
N2 C8 1.290(6) . ?
N2 C24 1.462(6) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C33 1.522(4) . ?
C51 H51 0.9500 . ?
C51 C50 1.387(4) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C43 1.527(3) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C44 1.522(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.520(3) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.519(4) . ?
C47 H47 0.9500 . ?
C47 C48 1.378(4) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C7 C6 1.388(9) . ?
C7 C8 1.430(11) . ?
C5 H5 0.9500 . ?
C5 C6 1.398(15) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C50 H50 0.9500 . ?
C50 C49 1.375(5) . ?
C6 H6 0.9500 . ?
C49 H49 0.9500 . ?
C49 C48 1.374(5) . ?
C48 H48 0.9500 . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C9 N52 1.3900 . ?
C9 H55 1.225(4) 3_566 ?
C9 CXF 1.3900 . ?
N52 C53 1.3900 . ?
N52 H55 0.923(4) 3_566 ?
C53 H53 0.9500 . ?
C53 C54 1.3900 . ?
C53 H55 1.250(4) 3_566 ?
C54 H54 0.9500 . ?
C54 C55 1.3900 . ?
C54 HXF 0.835(6) 3_566 ?
C55 H55 0.9500 . ?
C55 CXF 1.3900 . ?
CXF HXF 0.9500 . ?
C24 H24 1.0000 . ?
C24 C14 1.539(5) . ?
C24 C10 1.529(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C13 1.524(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C12 1.519(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.539(8) . ?
C11 C10 1.519(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C19 H19 1.0000 . ?
C19 N3 1.481(6) . ?
C19 C52 1.500(7) . ?
C19 C20 1.542(8) . ?
N3 C18 1.286(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C52 1.536(7) . ?
C23 C22 1.494(8) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.530(8) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.516(7) . ?
C18 H18 0.9500 . ?
C18 C17 1.440(12) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C17 C16 1.395(10) . ?
C16 H16 0.9500 . ?
C16 C15 1.404(17) . ?
C15 H15 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 U1 U1 85.06(4) . 3_666 ?
N5 U1 N7 149.66(5) . . ?
N4 U1 U1 120.93(4) . 3_666 ?
N4 U1 N5 68.53(5) . . ?
N4 U1 N7 139.12(5) . . ?
N6 U1 U1 121.83(4) . 3_666 ?
N6 U1 N5 139.24(5) . . ?
N6 U1 N4 71.19(5) . . ?
N6 U1 N7 68.44(5) . . ?
N7 U1 U1 86.56(4) . 3_666 ?
O2 U1 U1 31.86(3) 3_666 3_666 ?
O2 U1 U1 39.76(4) . 3_666 ?
O2 U1 N5 95.26(5) . . ?
O2 U1 N5 78.27(5) 3_666 . ?
O2 U1 N4 140.13(5) 3_666 . ?
O2 U1 N4 89.66(6) . . ?
O2 U1 N6 140.92(5) 3_666 . ?
O2 U1 N6 90.43(5) . . ?
O2 U1 N7 79.28(5) 3_666 . ?
O2 U1 N7 96.75(5) . . ?
O2 U1 O2 71.61(6) . 3_666 ?
O1 U1 U1 144.06(4) . 3_666 ?
O1 U1 N5 85.44(5) . . ?
O1 U1 N4 87.10(6) . . ?
O1 U1 N6 86.61(5) . . ?
O1 U1 N7 84.42(5) . . ?
O1 U1 O2 112.20(5) . 3_666 ?
O1 U1 O2 176.18(5) . . ?
N8 Zn1 N2 86.97(11) . . ?
N8 Zn1 N52 161.11(8) . . ?
N1 Zn1 N8 98.65(8) . . ?
N1 Zn1 N2 79.04(12) . . ?
N1 Zn1 N52 92.45(8) . . ?
N1 Zn1 N3 88.31(15) . . ?
N2 Zn1 N52 80.17(12) . . ?
O1 Zn1 N8 95.55(7) . . ?
O1 Zn1 N1 137.98(7) . . ?
O1 Zn1 N2 141.28(12) . . ?
O1 Zn1 N52 86.15(7) . . ?
O1 Zn1 N3 128.70(15) . . ?
N3 Zn1 N8 97.43(15) . . ?
C29 N5 U1 113.58(13) . . ?
C29 N5 C30 121.35(17) . . ?
C30 N5 U1 124.96(12) . . ?
C25 N4 U1 137.37(13) . . ?
C25 N4 C28 106.74(16) . . ?
C28 N4 U1 113.85(12) . . ?
C36 N6 U1 138.45(13) . . ?
C36 N6 C39 106.36(16) . . ?
C39 N6 U1 114.71(12) . . ?
C41 N7 U1 124.68(12) . . ?
C40 N7 U1 114.01(13) . . ?
C40 N7 C41 121.28(17) . . ?
N4 C25 C26 109.35(18) . . ?
N4 C25 C3 124.83(18) . . ?
C26 C25 C3 125.10(18) . . ?
N7 C41 H41 106.8 . . ?
N7 C41 C46 109.86(16) . . ?
N7 C41 C42 115.46(16) . . ?
C46 C41 H41 106.8 . . ?
C42 C41 H41 106.8 . . ?
C42 C41 C46 110.67(17) . . ?
C51 N8 Zn1 120.95(18) . . ?
C47 N8 Zn1 120.88(18) . . ?
C47 N8 C51 118.0(2) . . ?
C4 N1 Zn1 140.27(15) . . ?
C4 N1 C7 100.4(4) . . ?
C7 N1 Zn1 115.0(4) . . ?
C17 N1 Zn1 103.0(5) . . ?
C17 N1 C4 115.1(4) . . ?
N5 C29 H29 119.1 . . ?
N5 C29 C28 121.89(18) . . ?
C28 C29 H29 119.1 . . ?
N5 C30 H30 106.8 . . ?
N5 C30 C35 110.15(16) . . ?
N5 C30 C31 115.45(16) . . ?
C35 C30 H30 106.8 . . ?
C35 C30 C31 110.42(17) . . ?
C31 C30 H30 106.8 . . ?
N4 C28 C29 120.74(17) . . ?
N4 C28 C27 110.23(17) . . ?
C27 C28 C29 129.03(19) . . ?
N6 C36 C3 124.88(17) . . ?
N6 C36 C37 110.14(18) . . ?
C37 C36 C3 124.35(17) . . ?
C25 C26 H26 126.2 . . ?
C27 C26 C25 107.61(18) . . ?
C27 C26 H26 126.2 . . ?
N7 C40 H40 119.1 . . ?
N7 C40 C39 121.77(18) . . ?
C39 C40 H40 119.1 . . ?
C25 C3 C36 117.19(16) . . ?
C25 C3 C2 109.43(17) . . ?
C25 C3 C4 106.08(16) . . ?
C36 C3 C2 108.29(16) . . ?
C36 C3 C4 105.34(16) . . ?
C4 C3 C2 110.35(16) . . ?
C41 C46 H46A 109.6 . . ?
C41 C46 H46B 109.6 . . ?
H46A C46 H46B 108.1 . . ?
C45 C46 C41 110.4(2) . . ?
C45 C46 H46A 109.6 . . ?
C45 C46 H46B 109.6 . . ?
C28 C27 H27 127.0 . . ?
C26 C27 C28 106.07(18) . . ?
C26 C27 H27 127.0 . . ?
N6 C39 C40 120.68(17) . . ?
N6 C39 C38 110.06(18) . . ?
C38 C39 C40 129.26(19) . . ?
C36 C37 H37 126.4 . . ?
C38 C37 C36 107.17(18) . . ?
C38 C37 H37 126.4 . . ?
C30 C35 H35A 109.6 . . ?
C30 C35 H35B 109.6 . . ?
C30 C35 C34 110.28(18) . . ?
H35A C35 H35B 108.1 . . ?
C34 C35 H35A 109.6 . . ?
C34 C35 H35B 109.6 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 C32 110.74(17) . . ?
H31A C31 H31B 108.1 . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
C3 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
C1 C2 C3 112.46(18) . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
N1 C4 C3 119.51(18) . . ?
N1 C4 C5 115.0(5) . . ?
C5 C4 C3 125.4(5) . . ?
C15 C4 N1 103.7(6) . . ?
C15 C4 C3 136.6(6) . . ?
C39 C38 H38 126.9 . . ?
C37 C38 C39 106.26(18) . . ?
C37 C38 H38 126.9 . . ?
C8 N2 Zn1 108.8(3) . . ?
C8 N2 C24 120.1(4) . . ?
C24 N2 Zn1 130.9(3) . . ?
C35 C34 H34A 109.4 . . ?
C35 C34 H34B 109.4 . . ?
H34A C34 H34B 108.0 . . ?
C33 C34 C35 111.1(2) . . ?
C33 C34 H34A 109.4 . . ?
C33 C34 H34B 109.4 . . ?
N8 C51 H51 119.1 . . ?
N8 C51 C50 121.7(3) . . ?
C50 C51 H51 119.1 . . ?
C41 C42 H42A 109.4 . . ?
C41 C42 H42B 109.4 . . ?
C41 C42 C43 111.13(18) . . ?
H42A C42 H42B 108.0 . . ?
C43 C42 H42A 109.4 . . ?
C43 C42 H42B 109.4 . . ?
C46 C45 H45A 109.4 . . ?
C46 C45 H45B 109.4 . . ?
H45A C45 H45B 108.0 . . ?
C44 C45 C46 111.3(2) . . ?
C44 C45 H45A 109.4 . . ?
C44 C45 H45B 109.4 . . ?
C31 C32 H32A 109.3 . . ?
C31 C32 H32B 109.3 . . ?
H32A C32 H32B 107.9 . . ?
C33 C32 C31 111.67(19) . . ?
C33 C32 H32A 109.3 . . ?
C33 C32 H32B 109.3 . . ?
C42 C43 H43A 109.4 . . ?
C42 C43 H43B 109.4 . . ?
H43A C43 H43B 108.0 . . ?
C44 C43 C42 111.2(2) . . ?
C44 C43 H43A 109.4 . . ?
C44 C43 H43B 109.4 . . ?
N8 C47 H47 118.5 . . ?
N8 C47 C48 123.0(3) . . ?
C48 C47 H47 118.5 . . ?
C45 C44 H44A 109.5 . . ?
C45 C44 H44B 109.5 . . ?
C43 C44 C45 110.8(2) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 108.1 . . ?
C6 C7 N1 113.5(7) . . ?
C6 C7 C8 132.6(8) . . ?
C8 C7 N1 113.5(5) . . ?
C4 C5 H5 128.2 . . ?
C6 C5 C4 103.7(7) . . ?
C6 C5 H5 128.2 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C34 C33 H33A 109.6 . . ?
C34 C33 H33B 109.6 . . ?
C32 C33 C34 110.24(19) . . ?
C32 C33 H33A 109.6 . . ?
C32 C33 H33B 109.6 . . ?
H33A C33 H33B 108.1 . . ?
C51 C50 H50 120.1 . . ?
C49 C50 C51 119.8(3) . . ?
C49 C50 H50 120.1 . . ?
C7 C6 C5 107.3(8) . . ?
C7 C6 H6 126.4 . . ?
C5 C6 H6 126.4 . . ?
C50 C49 H49 120.8 . . ?
C48 C49 C50 118.3(3) . . ?
C48 C49 H49 120.8 . . ?
C47 C48 H48 120.4 . . ?
C49 C48 C47 119.1(3) . . ?
C49 C48 H48 120.4 . . ?
N2 C8 C7 121.6(5) . . ?
N2 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
H9 C9 H55 157.8 . 3_566 ?
N52 C9 H9 120.0 . . ?
N52 C9 H55 40.70(17) . 3_566 ?
N52 C9 CXF 120.0 . . ?
CXF C9 H9 120.0 . . ?
CXF C9 H55 80.35(17) . 3_566 ?
Zn1 N52 H55 174.0(3) . 3_566 ?
C9 N52 Zn1 121.22(13) . . ?
C9 N52 H55 60.0(3) . 3_566 ?
C53 N52 Zn1 118.34(13) . . ?
C53 N52 C9 120.0 . . ?
C53 N52 H55 61.6(3) . 3_566 ?
N52 C53 H53 120.0 . . ?
N52 C53 C54 120.0 . . ?
N52 C53 H55 40.48(17) . 3_566 ?
H53 C53 H55 157.7 . 3_566 ?
C54 C53 H53 120.0 . . ?
C54 C53 H55 80.54(17) . 3_566 ?
C53 C54 H54 120.0 . . ?
C53 C54 HXF 89.0(5) . 3_566 ?
H54 C54 HXF 33.7 . 3_566 ?
C55 C54 C53 120.0 . . ?
C55 C54 H54 120.0 . . ?
C55 C54 HXF 148.1(5) . 3_566 ?
C54 C55 H55 120.0 . . ?
C54 C55 CXF 120.0 . . ?
CXF C55 H55 120.0 . . ?
C9 CXF HXF 120.0 . . ?
C55 CXF C9 120.0 . . ?
C55 CXF HXF 120.0 . . ?
N2 C24 H24 108.6 . . ?
N2 C24 C14 110.6(3) . . ?
N2 C24 C10 110.6(3) . . ?
C14 C24 H24 108.6 . . ?
C10 C24 H24 108.6 . . ?
C10 C24 C14 109.8(3) . . ?
C24 C14 H14A 109.4 . . ?
C24 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C13 C14 C24 111.0(3) . . ?
C13 C14 H14A 109.4 . . ?
C13 C14 H14B 109.4 . . ?
C14 C13 H13A 109.4 . . ?
C14 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
C12 C13 C14 110.9(4) . . ?
C12 C13 H13A 109.4 . . ?
C12 C13 H13B 109.4 . . ?
H11A C11 H11B 107.9 . . ?
C12 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C10 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
C10 C11 C12 111.7(4) . . ?
C13 C12 C11 110.7(4) . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C24 C10 H10A 109.2 . . ?
C24 C10 H10B 109.2 . . ?
C11 C10 C24 111.9(4) . . ?
C11 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
U1 O2 U1 108.39(6) . 3_666 ?
U1 O1 Zn1 121.98(7) . . ?
N3 C19 H19 109.1 . . ?
N3 C19 C52 110.1(4) . . ?
N3 C19 C20 109.7(4) . . ?
C52 C19 H19 109.1 . . ?
C52 C19 C20 109.7(4) . . ?
C20 C19 H19 109.1 . . ?
C19 N3 Zn1 135.6(4) . . ?
C18 N3 Zn1 105.5(4) . . ?
C18 N3 C19 118.6(5) . . ?
H23A C23 H23B 108.2 . . ?
C52 C23 H23A 109.6 . . ?
C52 C23 H23B 109.6 . . ?
C22 C23 H23A 109.6 . . ?
C22 C23 H23B 109.6 . . ?
C22 C23 C52 110.1(5) . . ?
C19 C52 C23 111.9(4) . . ?
C19 C52 H52A 109.2 . . ?
C19 C52 H52B 109.2 . . ?
C23 C52 H52A 109.2 . . ?
C23 C52 H52B 109.2 . . ?
H52A C52 H52B 107.9 . . ?
C19 C20 H20A 109.4 . . ?
C19 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
C21 C20 C19 111.2(5) . . ?
C21 C20 H20A 109.4 . . ?
C21 C20 H20B 109.4 . . ?
C20 C21 H21A 109.6 . . ?
C20 C21 H21B 109.6 . . ?
H21A C21 H21B 108.1 . . ?
C22 C21 C20 110.5(4) . . ?
C22 C21 H21A 109.6 . . ?
C22 C21 H21B 109.6 . . ?
N3 C18 H18 120.3 . . ?
N3 C18 C17 119.4(6) . . ?
C17 C18 H18 120.3 . . ?
C23 C22 C21 112.9(5) . . ?
C23 C22 H22A 109.0 . . ?
C23 C22 H22B 109.0 . . ?
C21 C22 H22A 109.0 . . ?
C21 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
N1 C17 C18 121.7(7) . . ?
N1 C17 C16 104.9(8) . . ?
C16 C17 C18 133.3(10) . . ?
C17 C16 H16 127.3 . . ?
C17 C16 C15 105.4(10) . . ?
C15 C16 H16 127.3 . . ?
C4 C15 C16 110.8(9) . . ?
C4 C15 H15 124.6 . . ?
C16 C15 H15 124.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 N5 C29 C28 3.7(2) . . . . ?
U1 N5 C30 C35 -57.8(2) . . . . ?
U1 N5 C30 C31 176.34(13) . . . . ?
U1 N4 C25 C26 -161.77(15) . . . . ?
U1 N4 C25 C3 27.6(3) . . . . ?
U1 N4 C28 C29 -13.0(2) . . . . ?
U1 N4 C28 C27 166.68(13) . . . . ?
U1 N6 C36 C3 -18.4(3) . . . . ?
U1 N6 C36 C37 170.41(15) . . . . ?
U1 N6 C39 C40 7.4(2) . . . . ?
U1 N6 C39 C38 -173.06(13) . . . . ?
U1 N7 C41 C46 54.9(2) . . . . ?
U1 N7 C41 C42 -179.07(13) . . . . ?
U1 N7 C40 C39 -0.1(2) . . . . ?
Zn1 N8 C51 C50 -176.06(18) . . . . ?
Zn1 N8 C47 C48 176.8(2) . . . . ?
Zn1 N1 C4 C3 24.9(3) . . . . ?
Zn1 N1 C4 C5 -153.1(6) . . . . ?
Zn1 N1 C4 C15 -159.5(8) . . . . ?
Zn1 N1 C7 C6 159.3(6) . . . . ?
Zn1 N1 C7 C8 -13.8(8) . . . . ?
Zn1 N1 C17 C18 -14.5(11) . . . . ?
Zn1 N1 C17 C16 167.7(7) . . . . ?
Zn1 N2 C8 C7 6.0(7) . . . . ?
Zn1 N2 C24 C14 -96.7(4) . . . . ?
Zn1 N2 C24 C10 25.2(5) . . . . ?
Zn1 N52 C53 C54 172.51(18) . . . . ?
Zn1 N3 C18 C17 3.7(8) . . . . ?
N5 C29 C28 N4 6.3(3) . . . . ?
N5 C29 C28 C27 -173.3(2) . . . . ?
N5 C30 C35 C34 173.91(18) . . . . ?
N5 C30 C31 C32 -177.86(17) . . . . ?
N4 C25 C26 C27 -0.2(2) . . . . ?
N4 C25 C3 C36 -26.2(3) . . . . ?
N4 C25 C3 C2 -149.95(19) . . . . ?
N4 C25 C3 C4 91.0(2) . . . . ?
N4 C28 C27 C26 -0.1(2) . . . . ?
N6 C36 C3 C25 21.9(3) . . . . ?
N6 C36 C3 C2 146.20(19) . . . . ?
N6 C36 C3 C4 -95.7(2) . . . . ?
N6 C36 C37 C38 0.7(2) . . . . ?
N6 C39 C38 C37 -0.1(2) . . . . ?
N7 C41 C46 C45 -174.37(18) . . . . ?
N7 C41 C42 C43 178.04(17) . . . . ?
N7 C40 C39 N6 -5.1(3) . . . . ?
N7 C40 C39 C38 175.5(2) . . . . ?
C25 N4 C28 C29 -179.65(18) . . . . ?
C25 N4 C28 C27 0.0(2) . . . . ?
C25 C26 C27 C28 0.2(2) . . . . ?
C25 C3 C2 C1 66.1(2) . . . . ?
C25 C3 C4 N1 -72.2(2) . . . . ?
C25 C3 C4 C5 105.6(7) . . . . ?
C25 C3 C4 C15 114.0(12) . . . . ?
C41 N7 C40 C39 178.01(17) . . . . ?
C41 C46 C45 C44 -57.1(3) . . . . ?
C41 C42 C43 C44 55.6(3) . . . . ?
N8 C51 C50 C49 -0.5(4) . . . . ?
N8 C47 C48 C49 -1.0(4) . . . . ?
N1 C4 C5 C6 1.7(10) . . . . ?
N1 C4 C15 C16 -3.2(14) . . . . ?
N1 C7 C6 C5 3.5(11) . . . . ?
N1 C7 C8 N2 4.2(10) . . . . ?
N1 C17 C16 C15 -1.5(13) . . . . ?
C29 N5 C30 C35 126.2(2) . . . . ?
C29 N5 C30 C31 0.3(3) . . . . ?
C29 C28 C27 C26 179.5(2) . . . . ?
C30 N5 C29 C28 -179.80(17) . . . . ?
C30 C35 C34 C33 58.0(3) . . . . ?
C30 C31 C32 C33 -56.0(2) . . . . ?
C28 N4 C25 C26 0.1(2) . . . . ?
C28 N4 C25 C3 -170.53(18) . . . . ?
C36 N6 C39 C40 -179.01(18) . . . . ?
C36 N6 C39 C38 0.5(2) . . . . ?
C36 C3 C2 C1 -62.7(2) . . . . ?
C36 C3 C4 N1 52.7(2) . . . . ?
C36 C3 C4 C5 -129.5(7) . . . . ?
C36 C3 C4 C15 -121.1(12) . . . . ?
C36 C37 C38 C39 -0.4(2) . . . . ?
C26 C25 C3 C36 164.58(19) . . . . ?
C26 C25 C3 C2 40.8(3) . . . . ?
C26 C25 C3 C4 -78.2(2) . . . . ?
C40 N7 C41 C46 -122.9(2) . . . . ?
C40 N7 C41 C42 3.1(3) . . . . ?
C40 C39 C38 C37 179.4(2) . . . . ?
C3 C25 C26 C27 170.43(18) . . . . ?
C3 C36 C37 C38 -170.51(19) . . . . ?
C3 C4 C5 C6 -176.1(5) . . . . ?
C3 C4 C15 C16 171.2(5) . . . . ?
C46 C41 C42 C43 -56.4(2) . . . . ?
C46 C45 C44 C43 56.3(3) . . . . ?
C39 N6 C36 C3 170.43(18) . . . . ?
C39 N6 C36 C37 -0.8(2) . . . . ?
C37 C36 C3 C25 -168.14(19) . . . . ?
C37 C36 C3 C2 -43.8(3) . . . . ?
C37 C36 C3 C4 74.2(2) . . . . ?
C35 C30 C31 C32 56.4(2) . . . . ?
C35 C34 C33 C32 -56.8(3) . . . . ?
C31 C30 C35 C34 -57.4(2) . . . . ?
C31 C32 C33 C34 55.9(3) . . . . ?
C2 C3 C4 N1 169.37(19) . . . . ?
C2 C3 C4 C5 -12.9(7) . . . . ?
C2 C3 C4 C15 -4.4(12) . . . . ?
C4 N1 C7 C6 -2.3(8) . . . . ?
C4 N1 C7 C8 -175.3(6) . . . . ?
C4 N1 C17 C18 177.3(8) . . . . ?
C4 N1 C17 C16 -0.5(11) . . . . ?
C4 C3 C2 C1 -177.6(2) . . . . ?
C4 C5 C6 C7 -3.0(11) . . . . ?
N2 C24 C14 C13 179.3(4) . . . . ?
N2 C24 C10 C11 -177.8(4) . . . . ?
C51 N8 C47 C48 0.7(4) . . . . ?
C51 C50 C49 C48 0.2(4) . . . . ?
C42 C41 C46 C45 57.0(2) . . . . ?
C42 C43 C44 C45 -55.2(3) . . . . ?
C47 N8 C51 C50 0.0(3) . . . . ?
C7 N1 C4 C3 178.2(5) . . . . ?
C7 N1 C4 C5 0.2(8) . . . . ?
C50 C49 C48 C47 0.5(4) . . . . ?
C6 C7 C8 N2 -167.2(9) . . . . ?
C8 N2 C24 C14 88.9(5) . . . . ?
C8 N2 C24 C10 -149.2(4) . . . . ?
C8 C7 C6 C5 174.8(11) . . . . ?
C9 N52 C53 C54 0.0 . . . . ?
N52 C9 CXF C55 0.0 . . . . ?
N52 C53 C54 C55 0.0 . . . . ?
C53 C54 C55 CXF 0.0 . . . . ?
C54 C55 CXF C9 0.0 . . . . ?
CXF C9 N52 Zn1 -172.29(18) . . . . ?
CXF C9 N52 C53 0.0 . . . . ?
C24 N2 C8 C7 -178.4(6) . . . . ?
C24 C14 C13 C12 -58.1(5) . . . . ?
C14 C24 C10 C11 -55.4(5) . . . . ?
C14 C13 C12 C11 56.2(5) . . . . ?
C12 C11 C10 C24 54.8(6) . . . . ?
C10 C24 C14 C13 56.9(4) . . . . ?
C10 C11 C12 C13 -54.6(6) . . . . ?
C19 N3 C18 C17 179.5(7) . . . . ?
C19 C20 C21 C22 -54.6(7) . . . . ?
N3 C19 C52 C23 -178.1(4) . . . . ?
N3 C19 C20 C21 177.4(5) . . . . ?
N3 C18 C17 N1 8.2(14) . . . . ?
N3 C18 C17 C16 -174.7(11) . . . . ?
C52 C19 N3 Zn1 100.6(6) . . . . ?
C52 C19 N3 C18 -73.6(6) . . . . ?
C52 C19 C20 C21 56.3(6) . . . . ?
C52 C23 C22 C21 -55.3(7) . . . . ?
C20 C19 N3 Zn1 -20.2(7) . . . . ?
C20 C19 N3 C18 165.6(5) . . . . ?
C20 C19 C52 C23 -57.3(6) . . . . ?
C20 C21 C22 C23 55.0(8) . . . . ?
C18 C17 C16 C15 -178.9(14) . . . . ?
C22 C23 C52 C19 56.9(6) . . . . ?
C17 N1 C4 C3 -173.3(6) . . . . ?
C17 N1 C4 C15 2.3(10) . . . . ?
C17 C16 C15 C4 3.0(16) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Pyridene, hexane'
_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_mo_jl23017_0m
_database_code_depnum_ccdc_archive 'CCDC 2313504'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2023-12-11 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_audit_creation_date             2023-11-24
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C92 H114 Cl2 N16 O4 U2 Y2'
_chemical_formula_sum            'C92 H114 Cl2 N16 O4 U2 Y2'
_chemical_formula_weight         2232.77
_chemical_melting_point          ?
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'
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'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   17.5026(9)
_cell_length_b                   17.0392(9)
_cell_length_c                   17.5819(9)
_cell_angle_alpha                90
_cell_angle_beta                 104.439(2)
_cell_angle_gamma                90
_cell_volume                     5077.8(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.287
_cell_measurement_theta_min      2.240
_shelx_estimated_absorpt_T_max   0.909
_shelx_estimated_absorpt_T_min   0.793
_exptl_absorpt_coefficient_mu    4.416
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6896
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0803 before and 0.0702 after correction.
The Ratio of minimum to maximum transmission is 0.9251.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2212
_exptl_crystal_size_max          0.055
_exptl_crystal_size_mid          0.049
_exptl_crystal_size_min          0.022
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0889
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            176971
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.418
_diffrn_reflns_theta_min         2.241
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8731
_reflns_number_total             10409
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         10409
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0302
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0190P)²+17.6030P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0666
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C31(H31), C20(H20), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C32(H32A,H32B), C2(H2A,H2B), C25(H25A,H25B), C36(H36A,H36B),
 C22(H22A,H22B), C34(H34A,H34B), C33(H33A,H33B), C35(H35A,H35B), C14(H14A,H14B),
  C23(H23A,H23B), C10(H10A,H10B), C24(H24A,H24B), C11(H11A,H11B), C13(H13A,
 H13B), C12(H12A,H12B)
2.c Aromatic/amide H refined with riding coordinates:
 C30(H30), C17(H17), C19(H19), C37(H37), C27(H27), C16(H16), C28(H28), C8(H8),
 C5(H5), C42(H42), C6(H6), C38(H38), C41(H41), C40(H40), C46(H46), C39(H39),
 C44(H44), C43(H43), C45(H45)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.54394(2) 0.56309(2) 0.44725(2) 0.01158(4) Uani 1 1 d . . . . .
Y1 Y 0.59049(2) 0.71737(2) 0.32424(2) 0.01337(8) Uani 1 1 d . . . . .
Cl1 Cl 0.47640(6) 0.69787(6) 0.19656(6) 0.0195(2) Uani 1 1 d . . . . .
O1 O 0.54521(15) 0.59894(15) 0.34506(15) 0.0137(5) Uani 1 1 d . . . . .
O2 O 0.54729(15) 0.53670(15) 0.55514(15) 0.0136(5) Uani 1 1 d . . . . .
N3 N 0.68555(18) 0.58520(18) 0.48173(18) 0.0135(7) Uani 1 1 d . . . . .
N4 N 0.61701(19) 0.44386(18) 0.41271(18) 0.0148(7) Uani 1 1 d . . . . .
N5 N 0.57161(18) 0.70552(18) 0.47539(18) 0.0139(7) Uani 1 1 d . . . . .
N6 N 0.41532(19) 0.64389(19) 0.42170(19) 0.0157(7) Uani 1 1 d . . . . .
N7 N 0.6902(2) 0.63313(19) 0.28654(19) 0.0181(7) Uani 1 1 d . . . . .
N1 N 0.70577(19) 0.77675(18) 0.40395(18) 0.0142(7) Uani 1 1 d . . . . .
N2 N 0.65339(19) 0.80981(19) 0.24257(19) 0.0166(7) Uani 1 1 d . . . . .
N8 N 0.5196(2) 0.8417(2) 0.33623(19) 0.0185(7) Uani 1 1 d . . . . .
C31 C 0.5804(2) 0.3739(2) 0.3686(2) 0.0182(9) Uani 1 1 d . . . . .
H31 H 0.539713 0.354128 0.395002 0.022 Uiso 1 1 calc R U . . .
C30 C 0.6928(2) 0.4513(2) 0.4348(2) 0.0145(8) Uani 1 1 d . . . . .
H30 H 0.724849 0.409404 0.425008 0.017 Uiso 1 1 calc R U . . .
C18 C 0.5034(2) 0.7457(2) 0.4804(2) 0.0132(8) Uani 1 1 d . . . . .
C20 C 0.3348(2) 0.6146(2) 0.3874(2) 0.0183(8) Uani 1 1 d . . . . .
H20 H 0.327187 0.567213 0.418240 0.022 Uiso 1 1 calc R U . . .
C15 C 0.6327(2) 0.7443(2) 0.5253(2) 0.0145(8) Uani 1 1 d . . . . .
C26 C 0.7381(2) 0.6383(2) 0.5223(2) 0.0153(8) Uani 1 1 d . . . . .
C29 C 0.7299(2) 0.5197(2) 0.4730(2) 0.0157(8) Uani 1 1 d . . . . .
C17 C 0.5230(2) 0.8101(2) 0.5289(2) 0.0168(8) Uani 1 1 d . . . . .
H17 H 0.487580 0.847987 0.540286 0.020 Uiso 1 1 calc R U . . .
C19 C 0.4270(2) 0.7150(2) 0.4473(2) 0.0159(8) Uani 1 1 d . . . . .
H19 H 0.382597 0.748080 0.443849 0.019 Uiso 1 1 calc R U . . .
C3 C 0.7192(2) 0.7231(2) 0.5377(2) 0.0141(8) Uani 1 1 d . . . . .
C37 C 0.7662(2) 0.6272(2) 0.3243(2) 0.0216(9) Uani 1 1 d . . . . .
H37 H 0.784540 0.655625 0.371858 0.026 Uiso 1 1 calc R U . . .
C27 C 0.8148(2) 0.6074(2) 0.5401(2) 0.0186(9) Uani 1 1 d . . . . .
H27 H 0.861587 0.632951 0.568224 0.022 Uiso 1 1 calc R U . . .
C7 C 0.7508(2) 0.8193(2) 0.3635(2) 0.0174(8) Uani 1 1 d . . . . .
C4 C 0.7503(2) 0.7707(2) 0.4789(2) 0.0148(8) Uani 1 1 d . . . . .
C16 C 0.6048(2) 0.8090(2) 0.5580(2) 0.0168(8) Uani 1 1 d . . . . .
H16 H 0.635593 0.845612 0.593536 0.020 Uiso 1 1 calc R U . . .
C21 C 0.2685(2) 0.6718(2) 0.3901(2) 0.0192(9) Uani 1 1 d . . . . .
H21A H 0.274926 0.720168 0.361088 0.023 Uiso 1 1 calc R U . . .
H21B H 0.271940 0.686468 0.445332 0.023 Uiso 1 1 calc R U . . .
C32 C 0.6359(3) 0.3060(2) 0.3655(2) 0.0218(9) Uani 1 1 d . . . . .
H32A H 0.662282 0.289320 0.419634 0.026 Uiso 1 1 calc R U . . .
H32B H 0.677108 0.323452 0.339619 0.026 Uiso 1 1 calc R U . . .
C28 C 0.8092(2) 0.5321(2) 0.5088(2) 0.0199(9) Uani 1 1 d . . . . .
H28 H 0.851275 0.496182 0.511319 0.024 Uiso 1 1 calc R U . . .
C2 C 0.7633(2) 0.7439(2) 0.6227(2) 0.0170(8) Uani 1 1 d . . . . .
H2A H 0.820554 0.735646 0.629139 0.020 Uiso 1 1 calc R U . . .
H2B H 0.754971 0.800166 0.632156 0.020 Uiso 1 1 calc R U . . .
C25 C 0.3283(2) 0.5877(3) 0.3035(2) 0.0232(9) Uani 1 1 d . . . . .
H25A H 0.369818 0.548462 0.302927 0.028 Uiso 1 1 calc R U . . .
H25B H 0.336237 0.633033 0.271096 0.028 Uiso 1 1 calc R U . . .
C8 C 0.7201(2) 0.8361(2) 0.2830(2) 0.0175(8) Uani 1 1 d . . . . .
H8 H 0.750161 0.868444 0.257410 0.021 Uiso 1 1 calc R U . . .
C5 C 0.8228(2) 0.8078(2) 0.4876(2) 0.0209(9) Uani 1 1 d . . . . .
H5 H 0.864064 0.811233 0.534275 0.025 Uiso 1 1 calc R U . . .
C36 C 0.5372(3) 0.3977(3) 0.2855(3) 0.0278(10) Uani 1 1 d . . . . .
H36A H 0.575696 0.418196 0.257646 0.033 Uiso 1 1 calc R U . . .
H36B H 0.499258 0.440215 0.287839 0.033 Uiso 1 1 calc R U . . .
C42 C 0.4403(3) 0.8464(3) 0.3153(2) 0.0238(9) Uani 1 1 d . . . . .
H42 H 0.411282 0.804603 0.285821 0.029 Uiso 1 1 calc R U . . .
C22 C 0.1872(2) 0.6359(3) 0.3539(2) 0.0232(9) Uani 1 1 d . . . . .
H22A H 0.178313 0.591068 0.386421 0.028 Uiso 1 1 calc R U . . .
H22B H 0.145836 0.675590 0.353647 0.028 Uiso 1 1 calc R U . . .
C1 C 0.7362(3) 0.6951(3) 0.6836(2) 0.0231(9) Uani 1 1 d . . . . .
H1A H 0.746935 0.639526 0.676363 0.035 Uiso 1 1 calc R U . . .
H1B H 0.679446 0.702638 0.677243 0.035 Uiso 1 1 calc R U . . .
H1C H 0.764772 0.711750 0.736378 0.035 Uiso 1 1 calc R U . . .
C6 C 0.8231(2) 0.8389(2) 0.4142(2) 0.0212(9) Uani 1 1 d . . . . .
H6 H 0.864494 0.867859 0.401351 0.025 Uiso 1 1 calc R U . . .
C9 C 0.6294(2) 0.8373(2) 0.1607(2) 0.0216(9) Uani 1 1 d . . . . .
H9 H 0.670546 0.874845 0.152484 0.026 Uiso 1 1 calc R U . . .
C38 C 0.8197(3) 0.5818(3) 0.2977(3) 0.0263(10) Uani 1 1 d . . . . .
H38 H 0.873051 0.578390 0.327162 0.032 Uiso 1 1 calc R U . . .
C41 C 0.6662(3) 0.5916(3) 0.2203(3) 0.0289(10) Uani 1 1 d . . . . .
H41 H 0.611960 0.593503 0.193409 0.035 Uiso 1 1 calc R U . . .
C40 C 0.7156(3) 0.5463(3) 0.1892(3) 0.0357(12) Uani 1 1 d . . . . .
H40 H 0.696109 0.518514 0.141507 0.043 Uiso 1 1 calc R U . . .
C46 C 0.5586(3) 0.9027(3) 0.3753(3) 0.0240(9) Uani 1 1 d . . . . .
H46 H 0.614619 0.900782 0.389772 0.029 Uiso 1 1 calc R U . . .
C34 C 0.5478(3) 0.2595(3) 0.2378(3) 0.0287(10) Uani 1 1 d . . . . .
H34A H 0.516847 0.214302 0.211086 0.034 Uiso 1 1 calc R U . . .
H34B H 0.586402 0.274377 0.207602 0.034 Uiso 1 1 calc R U . . .
C33 C 0.5911(3) 0.2363(3) 0.3203(3) 0.0275(10) Uani 1 1 d . . . . .
H33A H 0.628795 0.193592 0.318004 0.033 Uiso 1 1 calc R U . . .
H33B H 0.552758 0.216237 0.348570 0.033 Uiso 1 1 calc R U . . .
C39 C 0.7948(3) 0.5419(3) 0.2287(3) 0.0347(12) Uani 1 1 d . . . . .
H39 H 0.830719 0.511889 0.208126 0.042 Uiso 1 1 calc R U . . .
C35 C 0.4930(3) 0.3281(3) 0.2400(3) 0.0383(13) Uani 1 1 d . . . . .
H35A H 0.451019 0.311062 0.265060 0.046 Uiso 1 1 calc R U . . .
H35B H 0.467599 0.344718 0.185663 0.046 Uiso 1 1 calc R U . . .
C14 C 0.6254(3) 0.7700(3) 0.1036(2) 0.0265(10) Uani 1 1 d . . . . .
H14A H 0.587213 0.730314 0.112456 0.032 Uiso 1 1 calc R U . . .
H14B H 0.677765 0.744670 0.112657 0.032 Uiso 1 1 calc R U . . .
C23 C 0.1809(3) 0.6083(3) 0.2712(3) 0.0265(10) Uani 1 1 d . . . . .
H23A H 0.183669 0.653943 0.237188 0.032 Uiso 1 1 calc R U . . .
H23B H 0.129380 0.582114 0.250644 0.032 Uiso 1 1 calc R U . . .
C10 C 0.5513(3) 0.8816(3) 0.1460(3) 0.0268(10) Uani 1 1 d . . . . .
H10A H 0.509814 0.846419 0.155973 0.032 Uiso 1 1 calc R U . . .
H10B H 0.556772 0.926617 0.182634 0.032 Uiso 1 1 calc R U . . .
C24 C 0.2469(3) 0.5515(3) 0.2690(3) 0.0308(11) Uani 1 1 d . . . . .
H24A H 0.242841 0.535705 0.213971 0.037 Uiso 1 1 calc R U . . .
H24B H 0.241003 0.503769 0.299139 0.037 Uiso 1 1 calc R U . . .
C44 C 0.4407(3) 0.9712(3) 0.3761(3) 0.0334(11) Uani 1 1 d . . . . .
H44 H 0.413902 1.014957 0.390738 0.040 Uiso 1 1 calc R U . . .
C43 C 0.3992(3) 0.9095(3) 0.3347(3) 0.0311(11) Uani 1 1 d . . . . .
H43 H 0.343131 0.910229 0.319735 0.037 Uiso 1 1 calc R U . . .
C45 C 0.5221(3) 0.9683(3) 0.3957(3) 0.0309(11) Uani 1 1 d . . . . .
H45 H 0.552335 1.010589 0.422875 0.037 Uiso 1 1 calc R U . . .
C11 C 0.5273(3) 0.9111(3) 0.0616(3) 0.0379(13) Uani 1 1 d . . . . .
H11A H 0.475226 0.937219 0.052213 0.045 Uiso 1 1 calc R U . . .
H11B H 0.566135 0.950539 0.053655 0.045 Uiso 1 1 calc R U . . .
C13 C 0.5998(3) 0.7996(4) 0.0187(3) 0.0411(13) Uani 1 1 d . . . . .
H13A H 0.641725 0.833657 0.007871 0.049 Uiso 1 1 calc R U . . .
H13B H 0.593049 0.754301 -0.017601 0.049 Uiso 1 1 calc R U . . .
C12 C 0.5228(3) 0.8456(4) 0.0037(3) 0.0481(16) Uani 1 1 d . . . . .
H12A H 0.510634 0.867614 -0.050105 0.058 Uiso 1 1 calc R U . . .
H12B H 0.479376 0.809661 0.007187 0.058 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.903(3) . ?
U1 O2 2.326(2) 3_666 ?
U1 O2 1.936(3) . ?
U1 N3 2.430(3) . ?
U1 N4 2.553(3) . ?
U1 N5 2.500(3) . ?
U1 N6 2.581(3) . ?
Y1 Cl1 2.6271(10) . ?
Y1 O1 2.231(3) . ?
Y1 N5 2.766(3) . ?
Y1 N7 2.475(3) . ?
Y1 N1 2.377(3) . ?
Y1 N2 2.558(3) . ?
Y1 N8 2.490(3) . ?
N3 C26 1.359(5) . ?
N3 C29 1.389(5) . ?
N4 C31 1.478(5) . ?
N4 C30 1.291(5) . ?
N5 C18 1.398(5) . ?
N5 C15 1.372(5) . ?
N6 C20 1.475(5) . ?
N6 C19 1.290(5) . ?
N7 C37 1.334(5) . ?
N7 C41 1.338(5) . ?
N1 C7 1.390(5) . ?
N1 C4 1.357(5) . ?
N2 C8 1.286(5) . ?
N2 C9 1.472(5) . ?
N8 C42 1.348(5) . ?
N8 C46 1.336(5) . ?
C31 H31 1.0000 . ?
C31 C32 1.522(5) . ?
C31 C36 1.523(6) . ?
C30 H30 0.9500 . ?
C30 C29 1.420(5) . ?
C18 C17 1.380(5) . ?
C18 C19 1.418(5) . ?
C20 H20 1.0000 . ?
C20 C21 1.525(5) . ?
C20 C25 1.521(6) . ?
C15 C3 1.518(5) . ?
C15 C16 1.387(5) . ?
C26 C3 1.522(5) . ?
C26 C27 1.402(5) . ?
C29 C28 1.390(5) . ?
C17 H17 0.9500 . ?
C17 C16 1.396(5) . ?
C19 H19 0.9500 . ?
C3 C4 1.518(5) . ?
C3 C2 1.542(5) . ?
C37 H37 0.9500 . ?
C37 C38 1.382(6) . ?
C27 H27 0.9500 . ?
C27 C28 1.390(6) . ?
C7 C8 1.413(6) . ?
C7 C6 1.394(6) . ?
C4 C5 1.391(6) . ?
C16 H16 0.9500 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.533(6) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.531(6) . ?
C28 H28 0.9500 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.522(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C24 1.532(6) . ?
C8 H8 0.9500 . ?
C5 H5 0.9500 . ?
C5 C6 1.395(6) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C35 1.529(6) . ?
C42 H42 0.9500 . ?
C42 C43 1.382(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.506(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C6 H6 0.9500 . ?
C9 H9 1.0000 . ?
C9 C14 1.514(6) . ?
C9 C10 1.527(6) . ?
C38 H38 0.9500 . ?
C38 C39 1.364(7) . ?
C41 H41 0.9500 . ?
C41 C40 1.370(6) . ?
C40 H40 0.9500 . ?
C40 C39 1.388(7) . ?
C46 H46 0.9500 . ?
C46 C45 1.379(6) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C33 1.513(6) . ?
C34 C35 1.519(6) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C39 H39 0.9500 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C13 1.532(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.514(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.523(6) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C44 H44 0.9500 . ?
C44 C43 1.380(7) . ?
C44 C45 1.379(7) . ?
C43 H43 0.9500 . ?
C45 H45 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.500(8) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C12 1.525(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 174.23(11) . . ?
O1 U1 O2 112.78(10) . 3_666 ?
O1 U1 N3 86.24(11) . . ?
O1 U1 N4 84.62(10) . . ?
O1 U1 N5 80.10(10) . . ?
O1 U1 N6 83.08(10) . . ?
O2 U1 O2 72.60(11) . 3_666 ?
O2 U1 N3 90.67(10) . . ?
O2 U1 N3 140.43(10) 3_666 . ?
O2 U1 N4 98.84(10) . . ?
O2 U1 N4 78.24(10) 3_666 . ?
O2 U1 N5 144.26(10) 3_666 . ?
O2 U1 N5 94.28(10) . . ?
O2 U1 N6 96.11(10) . . ?
O2 U1 N6 79.73(10) 3_666 . ?
N3 U1 N4 69.05(10) . . ?
N3 U1 N5 70.42(10) . . ?
N3 U1 N6 138.77(10) . . ?
N4 U1 N6 148.21(10) . . ?
N5 U1 N4 137.36(10) . . ?
N5 U1 N6 68.54(10) . . ?
Cl1 Y1 N5 124.36(7) . . ?
O1 Y1 Cl1 78.49(7) . . ?
O1 Y1 N5 69.14(9) . . ?
O1 Y1 N7 79.78(10) . . ?
O1 Y1 N1 124.91(10) . . ?
O1 Y1 N2 150.36(10) . . ?
O1 Y1 N8 123.41(10) . . ?
N7 Y1 Cl1 97.73(8) . . ?
N7 Y1 N5 118.44(10) . . ?
N7 Y1 N2 77.04(10) . . ?
N7 Y1 N8 156.30(11) . . ?
N1 Y1 Cl1 155.55(8) . . ?
N1 Y1 N5 75.63(10) . . ?
N1 Y1 N7 81.55(11) . . ?
N1 Y1 N2 69.38(11) . . ?
N1 Y1 N8 87.45(11) . . ?
N2 Y1 Cl1 86.56(8) . . ?
N2 Y1 N5 139.07(10) . . ?
N8 Y1 Cl1 83.76(8) . . ?
N8 Y1 N5 78.43(10) . . ?
N8 Y1 N2 79.45(11) . . ?
U1 O1 Y1 122.23(12) . . ?
U1 O2 U1 107.41(11) . 3_666 ?
C26 N3 U1 138.5(2) . . ?
C26 N3 C29 105.6(3) . . ?
C29 N3 U1 114.3(2) . . ?
C31 N4 U1 126.1(2) . . ?
C30 N4 U1 112.8(2) . . ?
C30 N4 C31 121.0(3) . . ?
U1 N5 Y1 86.81(9) . . ?
C18 N5 U1 111.2(2) . . ?
C18 N5 Y1 109.4(2) . . ?
C15 N5 U1 132.5(2) . . ?
C15 N5 Y1 108.6(2) . . ?
C15 N5 C18 105.4(3) . . ?
C20 N6 U1 126.4(2) . . ?
C19 N6 U1 112.6(3) . . ?
C19 N6 C20 120.8(3) . . ?
C37 N7 Y1 126.4(3) . . ?
C37 N7 C41 116.8(4) . . ?
C41 N7 Y1 116.8(3) . . ?
C7 N1 Y1 115.3(2) . . ?
C4 N1 Y1 137.6(2) . . ?
C4 N1 C7 105.9(3) . . ?
C8 N2 Y1 111.2(2) . . ?
C8 N2 C9 115.3(3) . . ?
C9 N2 Y1 133.4(2) . . ?
C42 N8 Y1 122.0(3) . . ?
C46 N8 Y1 120.3(3) . . ?
C46 N8 C42 117.0(4) . . ?
N4 C31 H31 107.1 . . ?
N4 C31 C32 115.8(3) . . ?
N4 C31 C36 109.6(3) . . ?
C32 C31 H31 107.1 . . ?
C32 C31 C36 109.7(3) . . ?
C36 C31 H31 107.1 . . ?
N4 C30 H30 118.8 . . ?
N4 C30 C29 122.5(3) . . ?
C29 C30 H30 118.8 . . ?
N5 C18 C19 121.8(3) . . ?
C17 C18 N5 110.1(3) . . ?
C17 C18 C19 127.6(4) . . ?
N6 C20 H20 107.1 . . ?
N6 C20 C21 115.3(3) . . ?
N6 C20 C25 109.3(3) . . ?
C21 C20 H20 107.1 . . ?
C25 C20 H20 107.1 . . ?
C25 C20 C21 110.4(3) . . ?
N5 C15 C3 124.6(3) . . ?
N5 C15 C16 110.4(3) . . ?
C16 C15 C3 124.8(3) . . ?
N3 C26 C3 125.2(3) . . ?
N3 C26 C27 110.6(3) . . ?
C27 C26 C3 123.8(3) . . ?
N3 C29 C30 120.7(3) . . ?
N3 C29 C28 110.5(3) . . ?
C28 C29 C30 128.8(4) . . ?
C18 C17 H17 126.6 . . ?
C18 C17 C16 106.9(3) . . ?
C16 C17 H17 126.6 . . ?
N6 C19 C18 122.7(4) . . ?
N6 C19 H19 118.6 . . ?
C18 C19 H19 118.6 . . ?
C15 C3 C26 117.0(3) . . ?
C15 C3 C4 106.9(3) . . ?
C15 C3 C2 108.9(3) . . ?
C26 C3 C2 108.2(3) . . ?
C4 C3 C26 104.8(3) . . ?
C4 C3 C2 111.1(3) . . ?
N7 C37 H37 118.3 . . ?
N7 C37 C38 123.3(4) . . ?
C38 C37 H37 118.3 . . ?
C26 C27 H27 126.6 . . ?
C28 C27 C26 106.8(4) . . ?
C28 C27 H27 126.6 . . ?
N1 C7 C8 119.7(4) . . ?
N1 C7 C6 109.7(3) . . ?
C6 C7 C8 130.6(4) . . ?
N1 C4 C3 119.0(3) . . ?
N1 C4 C5 111.1(3) . . ?
C5 C4 C3 129.8(4) . . ?
C15 C16 C17 107.1(3) . . ?
C15 C16 H16 126.4 . . ?
C17 C16 H16 126.4 . . ?
C20 C21 H21A 109.3 . . ?
C20 C21 H21B 109.3 . . ?
C20 C21 C22 111.5(3) . . ?
H21A C21 H21B 108.0 . . ?
C22 C21 H21A 109.3 . . ?
C22 C21 H21B 109.3 . . ?
C31 C32 H32A 109.4 . . ?
C31 C32 H32B 109.4 . . ?
C31 C32 C33 111.1(4) . . ?
H32A C32 H32B 108.0 . . ?
C33 C32 H32A 109.4 . . ?
C33 C32 H32B 109.4 . . ?
C29 C28 H28 126.8 . . ?
C27 C28 C29 106.5(4) . . ?
C27 C28 H28 126.8 . . ?
C3 C2 H2A 109.0 . . ?
C3 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C1 C2 C3 112.8(3) . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
C20 C25 H25A 109.7 . . ?
C20 C25 H25B 109.7 . . ?
C20 C25 C24 110.0(3) . . ?
H25A C25 H25B 108.2 . . ?
C24 C25 H25A 109.7 . . ?
C24 C25 H25B 109.7 . . ?
N2 C8 C7 123.4(4) . . ?
N2 C8 H8 118.3 . . ?
C7 C8 H8 118.3 . . ?
C4 C5 H5 126.8 . . ?
C4 C5 C6 106.5(4) . . ?
C6 C5 H5 126.8 . . ?
C31 C36 H36A 109.4 . . ?
C31 C36 H36B 109.4 . . ?
C31 C36 C35 111.1(4) . . ?
H36A C36 H36B 108.0 . . ?
C35 C36 H36A 109.4 . . ?
C35 C36 H36B 109.4 . . ?
N8 C42 H42 118.5 . . ?
N8 C42 C43 122.9(4) . . ?
C43 C42 H42 118.5 . . ?
C21 C22 H22A 109.4 . . ?
C21 C22 H22B 109.4 . . ?
H22A C22 H22B 108.0 . . ?
C23 C22 C21 111.3(3) . . ?
C23 C22 H22A 109.4 . . ?
C23 C22 H22B 109.4 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C7 C6 C5 106.8(3) . . ?
C7 C6 H6 126.6 . . ?
C5 C6 H6 126.6 . . ?
N2 C9 H9 107.8 . . ?
N2 C9 C14 111.3(3) . . ?
N2 C9 C10 110.3(3) . . ?
C14 C9 H9 107.8 . . ?
C14 C9 C10 111.7(4) . . ?
C10 C9 H9 107.8 . . ?
C37 C38 H38 120.4 . . ?
C39 C38 C37 119.1(4) . . ?
C39 C38 H38 120.4 . . ?
N7 C41 H41 118.2 . . ?
N7 C41 C40 123.5(4) . . ?
C40 C41 H41 118.2 . . ?
C41 C40 H40 120.6 . . ?
C41 C40 C39 118.8(4) . . ?
C39 C40 H40 120.6 . . ?
N8 C46 H46 118.2 . . ?
N8 C46 C45 123.6(4) . . ?
C45 C46 H46 118.2 . . ?
H34A C34 H34B 108.1 . . ?
C33 C34 H34A 109.6 . . ?
C33 C34 H34B 109.6 . . ?
C33 C34 C35 110.1(4) . . ?
C35 C34 H34A 109.6 . . ?
C35 C34 H34B 109.6 . . ?
C32 C33 H33A 109.4 . . ?
C32 C33 H33B 109.4 . . ?
C34 C33 C32 111.4(4) . . ?
C34 C33 H33A 109.4 . . ?
C34 C33 H33B 109.4 . . ?
H33A C33 H33B 108.0 . . ?
C38 C39 C40 118.4(4) . . ?
C38 C39 H39 120.8 . . ?
C40 C39 H39 120.8 . . ?
C36 C35 H35A 109.3 . . ?
C36 C35 H35B 109.3 . . ?
C34 C35 C36 111.8(4) . . ?
C34 C35 H35A 109.3 . . ?
C34 C35 H35B 109.3 . . ?
H35A C35 H35B 107.9 . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
C9 C14 C13 110.6(4) . . ?
H14A C14 H14B 108.1 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 C24 110.6(4) . . ?
H23A C23 H23B 108.1 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C9 C10 H10A 109.6 . . ?
C9 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
C11 C10 C9 110.2(4) . . ?
C11 C10 H10A 109.6 . . ?
C11 C10 H10B 109.6 . . ?
C25 C24 H24A 109.2 . . ?
C25 C24 H24B 109.2 . . ?
C23 C24 C25 111.9(4) . . ?
C23 C24 H24A 109.2 . . ?
C23 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
C43 C44 H44 120.7 . . ?
C45 C44 H44 120.7 . . ?
C45 C44 C43 118.7(4) . . ?
C42 C43 H43 120.5 . . ?
C44 C43 C42 119.0(5) . . ?
C44 C43 H43 120.5 . . ?
C46 C45 C44 118.8(4) . . ?
C46 C45 H45 120.6 . . ?
C44 C45 H45 120.6 . . ?
C10 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
C12 C11 C10 111.8(4) . . ?
C12 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C14 C13 H13A 109.3 . . ?
C14 C13 H13B 109.3 . . ?
H13A C13 H13B 108.0 . . ?
C12 C13 C14 111.6(4) . . ?
C12 C13 H13A 109.3 . . ?
C12 C13 H13B 109.3 . . ?
C11 C12 C13 111.8(4) . . ?
C11 C12 H12A 109.3 . . ?
C11 C12 H12B 109.3 . . ?
C13 C12 H12A 109.3 . . ?
C13 C12 H12B 109.3 . . ?
H12A C12 H12B 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 N3 C26 C3 -24.0(6) . . . . ?
U1 N3 C26 C27 163.2(3) . . . . ?
U1 N3 C29 C30 9.9(4) . . . . ?
U1 N3 C29 C28 -167.7(3) . . . . ?
U1 N4 C31 C32 -171.8(3) . . . . ?
U1 N4 C31 C36 63.6(4) . . . . ?
U1 N4 C30 C29 -0.9(5) . . . . ?
U1 N5 C18 C17 152.5(3) . . . . ?
U1 N5 C18 C19 -19.8(4) . . . . ?
U1 N5 C15 C3 42.3(5) . . . . ?
U1 N5 C15 C16 -142.3(3) . . . . ?
U1 N6 C20 C21 171.3(2) . . . . ?
U1 N6 C20 C25 -63.6(4) . . . . ?
U1 N6 C19 C18 4.4(4) . . . . ?
Y1 N5 C18 C17 -113.3(3) . . . . ?
Y1 N5 C18 C19 74.4(4) . . . . ?
Y1 N5 C15 C3 -60.9(4) . . . . ?
Y1 N5 C15 C16 114.5(3) . . . . ?
Y1 N7 C37 C38 -176.7(3) . . . . ?
Y1 N7 C41 C40 175.6(4) . . . . ?
Y1 N1 C7 C8 10.9(5) . . . . ?
Y1 N1 C7 C6 -169.3(3) . . . . ?
Y1 N1 C4 C3 -10.9(6) . . . . ?
Y1 N1 C4 C5 165.4(3) . . . . ?
Y1 N2 C8 C7 -3.9(5) . . . . ?
Y1 N2 C9 C14 -63.8(4) . . . . ?
Y1 N2 C9 C10 60.8(5) . . . . ?
Y1 N8 C42 C43 167.5(3) . . . . ?
Y1 N8 C46 C45 -168.8(3) . . . . ?
N3 C26 C3 C15 16.2(5) . . . . ?
N3 C26 C3 C4 -101.9(4) . . . . ?
N3 C26 C3 C2 139.6(4) . . . . ?
N3 C26 C27 C28 0.3(5) . . . . ?
N3 C29 C28 C27 -0.4(5) . . . . ?
N4 C31 C32 C33 178.5(3) . . . . ?
N4 C31 C36 C35 -175.5(4) . . . . ?
N4 C30 C29 N3 -6.2(6) . . . . ?
N4 C30 C29 C28 170.9(4) . . . . ?
N5 C18 C17 C16 -2.6(4) . . . . ?
N5 C18 C19 N6 11.0(6) . . . . ?
N5 C15 C3 C26 -26.1(5) . . . . ?
N5 C15 C3 C4 90.9(4) . . . . ?
N5 C15 C3 C2 -149.1(4) . . . . ?
N5 C15 C16 C17 1.2(4) . . . . ?
N6 C20 C21 C22 -179.5(3) . . . . ?
N6 C20 C25 C24 175.8(3) . . . . ?
N7 C37 C38 C39 1.4(7) . . . . ?
N7 C41 C40 C39 1.1(8) . . . . ?
N1 C7 C8 N2 -4.5(6) . . . . ?
N1 C7 C6 C5 0.1(5) . . . . ?
N1 C4 C5 C6 0.4(5) . . . . ?
N2 C9 C14 C13 179.6(3) . . . . ?
N2 C9 C10 C11 179.1(4) . . . . ?
N8 C42 C43 C44 1.3(7) . . . . ?
N8 C46 C45 C44 0.9(7) . . . . ?
C31 N4 C30 C29 176.2(3) . . . . ?
C31 C32 C33 C34 57.5(5) . . . . ?
C31 C36 C35 C34 -56.4(6) . . . . ?
C30 N4 C31 C32 11.6(5) . . . . ?
C30 N4 C31 C36 -113.0(4) . . . . ?
C30 C29 C28 C27 -177.8(4) . . . . ?
C18 N5 C15 C3 -178.1(3) . . . . ?
C18 N5 C15 C16 -2.8(4) . . . . ?
C18 C17 C16 C15 0.8(4) . . . . ?
C20 N6 C19 C18 -179.7(3) . . . . ?
C20 C21 C22 C23 -55.6(5) . . . . ?
C20 C25 C24 C23 57.3(5) . . . . ?
C15 N5 C18 C17 3.3(4) . . . . ?
C15 N5 C18 C19 -169.0(3) . . . . ?
C15 C3 C4 N1 -43.4(4) . . . . ?
C15 C3 C4 C5 141.1(4) . . . . ?
C15 C3 C2 C1 64.9(4) . . . . ?
C26 N3 C29 C30 178.2(3) . . . . ?
C26 N3 C29 C28 0.6(4) . . . . ?
C26 C3 C4 N1 81.4(4) . . . . ?
C26 C3 C4 C5 -94.2(5) . . . . ?
C26 C3 C2 C1 -63.2(4) . . . . ?
C26 C27 C28 C29 0.1(4) . . . . ?
C29 N3 C26 C3 172.2(3) . . . . ?
C29 N3 C26 C27 -0.6(4) . . . . ?
C17 C18 C19 N6 -159.8(4) . . . . ?
C19 N6 C20 C21 -4.1(5) . . . . ?
C19 N6 C20 C25 121.1(4) . . . . ?
C19 C18 C17 C16 169.1(4) . . . . ?
C3 C15 C16 C17 176.6(3) . . . . ?
C3 C26 C27 C28 -172.6(3) . . . . ?
C3 C4 C5 C6 176.2(4) . . . . ?
C37 N7 C41 C40 -2.1(7) . . . . ?
C37 C38 C39 C40 -2.4(7) . . . . ?
C27 C26 C3 C15 -171.9(4) . . . . ?
C27 C26 C3 C4 70.0(5) . . . . ?
C27 C26 C3 C2 -48.5(5) . . . . ?
C7 N1 C4 C3 -176.7(3) . . . . ?
C7 N1 C4 C5 -0.4(4) . . . . ?
C4 N1 C7 C8 -179.6(3) . . . . ?
C4 N1 C7 C6 0.2(4) . . . . ?
C4 C3 C2 C1 -177.7(3) . . . . ?
C4 C5 C6 C7 -0.3(5) . . . . ?
C16 C15 C3 C26 159.2(4) . . . . ?
C16 C15 C3 C4 -83.8(4) . . . . ?
C16 C15 C3 C2 36.2(5) . . . . ?
C21 C20 C25 C24 -56.2(5) . . . . ?
C21 C22 C23 C24 55.3(5) . . . . ?
C32 C31 C36 C35 56.3(5) . . . . ?
C2 C3 C4 N1 -162.1(3) . . . . ?
C2 C3 C4 C5 22.4(6) . . . . ?
C25 C20 C21 C22 56.0(4) . . . . ?
C8 N2 C9 C14 115.4(4) . . . . ?
C8 N2 C9 C10 -120.0(4) . . . . ?
C8 C7 C6 C5 179.8(4) . . . . ?
C36 C31 C32 C33 -56.9(5) . . . . ?
C42 N8 C46 C45 1.1(6) . . . . ?
C22 C23 C24 C25 -56.7(5) . . . . ?
C6 C7 C8 N2 175.8(4) . . . . ?
C9 N2 C8 C7 176.8(4) . . . . ?
C9 C14 C13 C12 -54.1(6) . . . . ?
C9 C10 C11 C12 55.9(5) . . . . ?
C41 N7 C37 C38 0.8(6) . . . . ?
C41 C40 C39 C38 1.2(7) . . . . ?
C46 N8 C42 C43 -2.2(6) . . . . ?
C33 C34 C35 C36 55.5(6) . . . . ?
C35 C34 C33 C32 -55.9(5) . . . . ?
C14 C9 C10 C11 -56.6(5) . . . . ?
C14 C13 C12 C11 54.1(6) . . . . ?
C10 C9 C14 C13 55.8(5) . . . . ?
C10 C11 C12 C13 -55.1(5) . . . . ?
C43 C44 C45 C46 -1.9(7) . . . . ?
C45 C44 C43 C42 0.8(7) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 475.8 77.8 '3 pyridines'
2 -0.020 0.454 0.696 41.5 0.0 ?
3 0.020 0.546 0.304 41.5 0.0 ?
4 0.500 0.500 0.000 475.8 77.8 '3 pyridines'
5 0.480 0.046 0.196 41.5 0.0 ?
6 0.520 0.954 0.804 41.5 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Pyridene, hexane'
_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_tom_jl22023_i2oa
_database_code_depnum_ccdc_archive 'CCDC 2313501'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2023-12-11 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_audit_creation_date             2023-12-11
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C47 H70 K N8 Na O2 Si2 U, 1.5(C6 H14)'
_chemical_formula_sum            'C56 H91 K N8 Na O2 Si2 U'
_chemical_formula_weight         1264.66
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
Si Si 0.0817 0.0704 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   26.8382(18)
_cell_length_b                   15.5671(10)
_cell_length_c                   28.998(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.423(2)
_cell_angle_gamma                90
_cell_volume                     12104.4(17)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      2.48
_cell_measurement_theta_min      26.08
_shelx_estimated_absorpt_T_max   0.907
_shelx_estimated_absorpt_T_min   0.431
_exptl_absorpt_coefficient_mu    2.843
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 595361 reflections, Rint = 0.0925
 (208722 with I > 3sig(I), Rint = 0.0572)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5192
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Pyridene, hexane'
_exptl_crystal_size_max          0.356
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.035
_exptl_transmission_factor_max   0.431466
_exptl_transmission_factor_min   0.334954
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0729
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21269
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.702
_diffrn_reflns_theta_min         2.043
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                16103
_reflns_number_total             21269
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.226
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.175
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         21269
_refine_ls_number_restraints     246
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0518
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+129.8202P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.1055
_refine_special_details          'Refined as a 2-component twin.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5741(6)
 0.4259(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C53-C52 = C52-C51 = C51-C50 = C50-C49 = C49-C48
 1.52 with sigma of 0.02
 C54-C55 = C55-C56 = C56-C57 = C57-C58 = C58-C59
 1.52 with sigma of 0.02
 C60-C61 = C61-C62 = C62-C63 = C63-C64 = C64-C65
 1.52 with sigma of 0.02
 C53-C51 = C50-C48
 2.53 with sigma of 0.04
 C52-C50 = C51-C49
 2.54 with sigma of 0.04
 C54-C56 = C57-C59
 2.53 with sigma of 0.04
 C55-C57 = C56-C58
 2.54 with sigma of 0.04
 C60-C62 = C63-C65
 2.53 with sigma of 0.04
 C61-C63 = C62-C64
 2.54 with sigma of 0.04
 C53-C52 \\sim C52-C51 \\sim C51-C50 \\sim C50-C49 \\sim C49-C48
 with sigma of 0.02
 C53-C51 \\sim C51-C49 \\sim C52-C50 \\sim C50-C48
 with sigma of 0.04
 C54-C56 \\sim C56-C58 \\sim C55-C57 \\sim C57-C59
 with sigma of 0.04
 C54-C55 \\sim C55-C56 \\sim C56-C57 \\sim C57-C58 \\sim C58-C59
 with sigma of 0.02
 C60-C61 \\sim C61-C62 \\sim C62-C63 \\sim C63-C64 \\sim C64-C65
 with sigma of 0.02
 C60-C62 \\sim C62-C64 \\sim C61-C63 \\sim C63-C65
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
C53 \\sim C52 \\sim C51 \\sim C50 \\sim C49 \\sim C48: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C53, C52, C51, C50, C49, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C54, C55, C56, C57, C58, C59
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C60, C61, C62, C63, C64, C65
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C53(0.5) H53A(0.5) H53B(0.5) H53C(0.5) C52(0.5) H52A(0.5)
 H52B(0.5) C51(0.5) H51A(0.5) H51B(0.5) C50(0.5) H50A(0.5) H50B(0.5) C49(0.5)
 H49A(0.5) H49B(0.5) C48(0.5) H48A(0.5) H48B(0.5) H48C(0.5) C54(0.5) H54A(0.5)
 H54B(0.5) H54C(0.5) C55(0.5) H55A(0.5) H55B(0.5) C56(0.5) H56A(0.5) H56B(0.5)
 C57(0.5) H57A(0.5) H57B(0.5) C58(0.5) H58A(0.5) H58B(0.5) C59(0.5) H59A(0.5)
 H59B(0.5) H59C(0.5) C60(0.5) H60A(0.5) H60B(0.5) H60C(0.5) C61(0.5) H61A(0.5)
 H61B(0.5) C62(0.5) H62A(0.5) H62B(0.5) C63(0.5) H63A(0.5) H63B(0.5) C64(0.5)
 H64A(0.5) H64B(0.5) C65(0.5) H65A(0.5) H65B(0.5) H65C(0.5)
7.a Ternary CH refined with riding coordinates:
 C17(H17), C20(H20), C16(H16), C31(H31), C9(H9)
7.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C2(H2A,H2B), C21(H21A,H21B), C25(H25A,H25B), C11(H11A,H11B),
 C32(H32A,H32B), C13(H13A,H13B), C23(H23A,H23B), C35(H35A,H35B), C36(H36A,H36B),
  C33(H33A,H33B), C12(H12A,H12B), C14(H14A,H14B), C34(H34A,H34B), C22(H22A,
 H22B), C24(H24A,H24B), C52(H52A,H52B), C51(H51A,H51B), C50(H50A,H50B),
 C49(H49A,H49B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B),
  C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B)
7.c Me refined with riding coordinates:
 C53(H53A,H53B,H53C), C48(H48A,H48B,H48C)
7.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C19(H19), C8(H8), C6(H6), C27(H27), C28(H28), C30(H30), C44(H44),
 C47(H47), C43(H43)
7.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C42(H42A,H42B,
 H42C), C38(H38A,H38B,H38C), C41(H41A,H41B,H41C), C40(H40A,H40B,H40C), C54(H54A,
 H54B,H54C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C65(H65A,H65B,H65C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.44217(2) 0.49543(2) 0.23076(2) 0.01734(5) Uani 1 1 d . . . . .
K1 K 0.48824(5) 0.22852(9) 0.23142(5) 0.0241(3) Uani 1 1 d . . . . .
Si1 Si 0.32981(7) 0.58978(12) 0.18438(7) 0.0214(4) Uani 1 1 d . . . . .
Si2 Si 0.33144(8) 0.39982(13) 0.17982(7) 0.0263(4) Uani 1 1 d . . . . .
Na1 Na 0.45190(9) 0.58392(16) 0.34239(8) 0.0219(5) Uani 1 1 d . . . . .
O2 O 0.45295(16) 0.3907(3) 0.20790(15) 0.0217(9) Uani 1 1 d . . . . .
O1 O 0.43464(15) 0.5989(3) 0.25709(14) 0.0190(9) Uani 1 1 d . . . . .
N5 N 0.49309(18) 0.4465(3) 0.30006(17) 0.0181(10) Uani 1 1 d . . . . .
N1 N 0.53731(19) 0.6177(3) 0.34190(18) 0.0186(11) Uani 1 1 d . . . . .
N4 N 0.4649(2) 0.5542(4) 0.15167(17) 0.0225(11) Uani 1 1 d . . . . .
N3 N 0.53231(19) 0.5404(3) 0.22769(17) 0.0190(10) Uani 1 1 d . . . . .
N6 N 0.39134(19) 0.4393(4) 0.29890(18) 0.0239(11) Uani 1 1 d . . . . .
C15 C 0.5737(2) 0.5491(4) 0.2565(2) 0.0181(12) Uani 1 1 d . . . . .
C26 C 0.5427(2) 0.4336(4) 0.31023(19) 0.0172(12) Uani 1 1 d . . . . .
C17 C 0.5877(2) 0.6344(4) 0.1962(2) 0.0237(14) Uani 1 1 d . . . . .
H17 H 0.606421 0.663541 0.171594 0.028 Uiso 1 1 calc R U . . .
C1 C 0.6446(2) 0.4010(5) 0.2645(2) 0.0267(15) Uani 1 1 d . . . . .
H1A H 0.643828 0.433439 0.235469 0.040 Uiso 1 1 calc R U . . .
H1B H 0.619065 0.356010 0.262671 0.040 Uiso 1 1 calc R U . . .
H1C H 0.677528 0.374731 0.269672 0.040 Uiso 1 1 calc R U . . .
N2 N 0.4639(2) 0.7343(4) 0.37131(17) 0.0231(11) Uani 1 1 d . . . . .
C3 C 0.58156(18) 0.5011(5) 0.30217(16) 0.0174(10) Uani 1 1 d . . . . .
C4 C 0.5785(2) 0.5692(4) 0.3402(2) 0.0194(13) Uani 1 1 d . . . . .
C18 C 0.5412(2) 0.5930(4) 0.1904(2) 0.0226(13) Uani 1 1 d . . . . .
N7 N 0.36187(16) 0.4946(4) 0.19691(14) 0.0197(9) Uani 1 1 d . . . . .
C5 C 0.6132(2) 0.5909(4) 0.3756(2) 0.0235(14) Uani 1 1 d . . . . .
H5 H 0.644862 0.565194 0.381712 0.028 Uiso 1 1 calc R U . . .
C19 C 0.5079(2) 0.5921(4) 0.1517(2) 0.0226(13) Uani 1 1 d . . . . .
H19 H 0.517352 0.620501 0.124380 0.027 Uiso 1 1 calc R U . . .
C7 C 0.5453(2) 0.6725(4) 0.3791(2) 0.0204(12) Uani 1 1 d . . . . .
N8 N 0.4482(2) 0.5129(4) 0.41759(17) 0.0290(13) Uani 1 1 d . . . . .
C8 C 0.5075(2) 0.7309(4) 0.3919(2) 0.0210(13) Uani 1 1 d . . . . .
H8 H 0.514665 0.769239 0.416794 0.025 Uiso 1 1 calc R U . . .
C6 C 0.5921(2) 0.6578(4) 0.4002(2) 0.0233(13) Uani 1 1 d . . . . .
H6 H 0.606791 0.687234 0.426068 0.028 Uiso 1 1 calc R U . . .
C29 C 0.4693(2) 0.3770(4) 0.3188(2) 0.0186(12) Uani 1 1 d . . . . .
C20 C 0.4376(3) 0.5447(5) 0.1065(2) 0.0268(15) Uani 1 1 d . . . . .
H20 H 0.402385 0.529415 0.112821 0.032 Uiso 1 1 calc R U . . .
C27 C 0.5499(2) 0.3568(4) 0.3339(2) 0.0205(13) Uani 1 1 d . . . . .
H27 H 0.581075 0.333385 0.344179 0.025 Uiso 1 1 calc R U . . .
C16 C 0.6074(2) 0.6067(4) 0.2384(2) 0.0235(14) Uani 1 1 d . . . . .
H16 H 0.642829 0.614401 0.249786 0.028 Uiso 1 1 calc R U . . .
C10 C 0.4233(2) 0.8704(5) 0.3508(2) 0.0255(14) Uani 1 1 d . . . . .
H10A H 0.456044 0.898584 0.347294 0.031 Uiso 1 1 calc R U . . .
H10B H 0.412553 0.845496 0.320606 0.031 Uiso 1 1 calc R U . . .
C28 C 0.5034(2) 0.3202(4) 0.3398(2) 0.0219(13) Uani 1 1 d . . . . .
H28 H 0.496291 0.267792 0.355000 0.026 Uiso 1 1 calc R U . . .
C30 C 0.4163(2) 0.3791(4) 0.3206(2) 0.0223(13) Uani 1 1 d . . . . .
H30 H 0.399309 0.336837 0.337650 0.027 Uiso 1 1 calc R U . . .
C31 C 0.3384(2) 0.4533(5) 0.3091(2) 0.0281(15) Uani 1 1 d . . . . .
H31 H 0.319619 0.462011 0.278900 0.034 Uiso 1 1 calc R U . . .
C2 C 0.6344(2) 0.4610(4) 0.3039(2) 0.0224(14) Uani 1 1 d . . . . .
H2A H 0.659228 0.508003 0.304113 0.027 Uiso 1 1 calc R U . . .
H2B H 0.639246 0.429012 0.333230 0.027 Uiso 1 1 calc R U . . .
C21 C 0.4362(3) 0.6257(5) 0.0768(2) 0.0344(17) Uani 1 1 d . . . . .
H21A H 0.470702 0.643955 0.070878 0.041 Uiso 1 1 calc R U . . .
H21B H 0.419855 0.672608 0.093501 0.041 Uiso 1 1 calc R U . . .
C37 C 0.3698(3) 0.6877(5) 0.1859(3) 0.0320(16) Uani 1 1 d . . . . .
H37A H 0.377836 0.703634 0.218087 0.048 Uiso 1 1 calc R U . . .
H37B H 0.351905 0.735039 0.170312 0.048 Uiso 1 1 calc R U . . .
H37C H 0.400688 0.675934 0.170216 0.048 Uiso 1 1 calc R U . . .
C25 C 0.4599(3) 0.4692(5) 0.0811(2) 0.0362(19) Uani 1 1 d . . . . .
H25A H 0.457747 0.416754 0.100171 0.043 Uiso 1 1 calc R U . . .
H25B H 0.495498 0.480702 0.076050 0.043 Uiso 1 1 calc R U . . .
C9 C 0.4288(2) 0.7987(5) 0.3868(2) 0.0243(14) Uani 1 1 d . . . . .
H9 H 0.442501 0.824191 0.416367 0.029 Uiso 1 1 calc R U . . .
C39 C 0.2995(2) 0.5915(5) 0.1246(2) 0.0298(15) Uani 1 1 d . . . . .
H39A H 0.325223 0.595506 0.101705 0.045 Uiso 1 1 calc R U . . .
H39B H 0.277188 0.641269 0.121488 0.045 Uiso 1 1 calc R U . . .
H39C H 0.280166 0.538676 0.119411 0.045 Uiso 1 1 calc R U . . .
C42 C 0.2620(3) 0.4028(5) 0.1887(3) 0.0382(18) Uani 1 1 d . . . . .
H42A H 0.256158 0.409228 0.221676 0.057 Uiso 1 1 calc R U . . .
H42B H 0.246706 0.349186 0.177371 0.057 Uiso 1 1 calc R U . . .
H42C H 0.247064 0.451441 0.171708 0.057 Uiso 1 1 calc R U . . .
C11 C 0.3852(3) 0.9372(5) 0.3652(3) 0.0316(16) Uani 1 1 d . . . . .
H11A H 0.398021 0.966906 0.393442 0.038 Uiso 1 1 calc R U . . .
H11B H 0.380671 0.980649 0.340435 0.038 Uiso 1 1 calc R U . . .
C32 C 0.3351(2) 0.5370(5) 0.3362(2) 0.0318(17) Uani 1 1 d . . . . .
H32A H 0.356900 0.532645 0.364554 0.038 Uiso 1 1 calc R U . . .
H32B H 0.347904 0.584573 0.317350 0.038 Uiso 1 1 calc R U . . .
C13 C 0.3400(3) 0.8238(5) 0.4095(3) 0.0315(16) Uani 1 1 d . . . . .
H13A H 0.307299 0.795152 0.412043 0.038 Uiso 1 1 calc R U . . .
H13B H 0.349883 0.848027 0.440075 0.038 Uiso 1 1 calc R U . . .
C23 C 0.4298(3) 0.5343(6) 0.0050(3) 0.049(3) Uani 1 1 d . . . . .
H23A H 0.409232 0.522866 -0.023503 0.059 Uiso 1 1 calc R U . . .
H23B H 0.463819 0.549408 -0.004094 0.059 Uiso 1 1 calc R U . . .
C38 C 0.2797(3) 0.6154(5) 0.2249(2) 0.0331(17) Uani 1 1 d . . . . .
H38A H 0.257359 0.565945 0.227099 0.050 Uiso 1 1 calc R U . . .
H38B H 0.260713 0.665271 0.213342 0.050 Uiso 1 1 calc R U . . .
H38C H 0.294780 0.628440 0.255447 0.050 Uiso 1 1 calc R U . . .
C46 C 0.4990(3) 0.4077(6) 0.4580(3) 0.0406(19) Uani 1 1 d . . . . .
C41 C 0.3401(3) 0.3740(5) 0.1172(3) 0.0413(19) Uani 1 1 d . . . . .
H41A H 0.326054 0.420464 0.097895 0.062 Uiso 1 1 calc R U . . .
H41B H 0.323018 0.320052 0.109272 0.062 Uiso 1 1 calc R U . . .
H41C H 0.375760 0.368157 0.111864 0.062 Uiso 1 1 calc R U . . .
C35 C 0.2584(3) 0.4043(7) 0.3442(3) 0.053(3) Uani 1 1 d . . . . .
H35A H 0.239126 0.414620 0.314815 0.063 Uiso 1 1 calc R U . . .
H35B H 0.242531 0.356303 0.360486 0.063 Uiso 1 1 calc R U . . .
C36 C 0.3126(3) 0.3811(6) 0.3342(3) 0.041(2) Uani 1 1 d . . . . .
H36A H 0.331296 0.369034 0.363721 0.049 Uiso 1 1 calc R U . . .
H36B H 0.312993 0.328280 0.315205 0.049 Uiso 1 1 calc R U . . .
C40 C 0.3526(3) 0.3004(5) 0.2105(3) 0.041(2) Uani 1 1 d . . . . .
H40A H 0.385289 0.283222 0.199794 0.062 Uiso 1 1 calc R U . . .
H40B H 0.328478 0.254205 0.204158 0.062 Uiso 1 1 calc R U . . .
H40C H 0.355221 0.311385 0.243829 0.062 Uiso 1 1 calc R U . . .
C44 C 0.4211(3) 0.4493(6) 0.4878(3) 0.045(2) Uani 1 1 d . . . . .
H44 H 0.396580 0.445625 0.510337 0.053 Uiso 1 1 calc R U . . .
C47 C 0.4897(3) 0.4657(5) 0.4225(2) 0.0321(16) Uani 1 1 d . . . . .
H47 H 0.514322 0.472405 0.400164 0.039 Uiso 1 1 calc R U . . .
C33 C 0.2823(3) 0.5587(6) 0.3498(3) 0.0380(19) Uani 1 1 d . . . . .
H33A H 0.283263 0.609689 0.370186 0.046 Uiso 1 1 calc R U . . .
H33B H 0.261796 0.573399 0.321656 0.046 Uiso 1 1 calc R U . . .
C12 C 0.3351(3) 0.8960(5) 0.3743(2) 0.0323(16) Uani 1 1 d . . . . .
H12A H 0.312256 0.940347 0.385715 0.039 Uiso 1 1 calc R U . . .
H12B H 0.320304 0.872976 0.344995 0.039 Uiso 1 1 calc R U . . .
C14 C 0.3787(3) 0.7578(5) 0.3957(2) 0.0285(15) Uani 1 1 d . . . . .
H14A H 0.383139 0.714654 0.420662 0.034 Uiso 1 1 calc R U . . .
H14B H 0.366282 0.727471 0.367501 0.034 Uiso 1 1 calc R U . . .
C34 C 0.2583(2) 0.4854(7) 0.3741(2) 0.043(2) Uani 1 1 d . . . . .
H34A H 0.223582 0.500798 0.380863 0.052 Uiso 1 1 calc R U . . .
H34B H 0.276754 0.474210 0.403789 0.052 Uiso 1 1 calc R U . . .
C43 C 0.4150(2) 0.5040(7) 0.4504(2) 0.0358(15) Uani 1 1 d . . . . .
H43 H 0.385321 0.537357 0.447871 0.043 Uiso 1 1 calc R U . . .
C45 C 0.4638(4) 0.4001(6) 0.4914(3) 0.045(2) Uani 1 1 d . . . . .
C22 C 0.4076(3) 0.6096(6) 0.0306(2) 0.041(2) Uani 1 1 d . . . . .
H22A H 0.372234 0.597416 0.036329 0.049 Uiso 1 1 calc R U . . .
H22B H 0.408946 0.661805 0.011215 0.049 Uiso 1 1 calc R U . . .
C24 C 0.4321(3) 0.4543(6) 0.0342(3) 0.045(2) Uani 1 1 d . . . . .
H24A H 0.449191 0.408351 0.017363 0.054 Uiso 1 1 calc R U . . .
H24B H 0.397755 0.434545 0.039568 0.054 Uiso 1 1 calc R U . . .
C53 C 0.3481(9) 0.652(2) 0.5652(11) 0.055(8) Uani 0.5 1 d D U P A -1
H53A H 0.374849 0.693437 0.572616 0.083 Uiso 0.5 1 calc R U P A -1
H53B H 0.330354 0.638977 0.593194 0.083 Uiso 0.5 1 calc R U P A -1
H53C H 0.362452 0.599352 0.553071 0.083 Uiso 0.5 1 calc R U P A -1
C52 C 0.3130(9) 0.6895(15) 0.5302(10) 0.101(10) Uani 0.5 1 d D U P A -1
H52A H 0.300647 0.744103 0.543070 0.121 Uiso 0.5 1 calc R U P A -1
H52B H 0.332530 0.704745 0.503216 0.121 Uiso 0.5 1 calc R U P A -1
C51 C 0.2695(9) 0.6414(15) 0.5130(13) 0.078(8) Uani 0.5 1 d D U P A -1
H51A H 0.253777 0.617442 0.540442 0.094 Uiso 0.5 1 calc R U P A -1
H51B H 0.282477 0.591882 0.495760 0.094 Uiso 0.5 1 calc R U P A -1
C50 C 0.2291(9) 0.6785(14) 0.4838(12) 0.073(7) Uani 0.5 1 d D U P A -1
H50A H 0.215836 0.728183 0.500677 0.088 Uiso 0.5 1 calc R U P A -1
H50B H 0.244310 0.701579 0.455866 0.088 Uiso 0.5 1 calc R U P A -1
C49 C 0.1864(7) 0.6258(14) 0.4683(10) 0.080(7) Uani 0.5 1 d D U P A -1
H49A H 0.175995 0.592078 0.495166 0.097 Uiso 0.5 1 calc R U P A -1
H49B H 0.198452 0.584229 0.445449 0.097 Uiso 0.5 1 calc R U P A -1
C48 C 0.1413(11) 0.667(2) 0.4476(13) 0.078(11) Uani 0.5 1 d D U P A -1
H48A H 0.116525 0.622916 0.439157 0.117 Uiso 0.5 1 calc R U P A -1
H48B H 0.127453 0.706731 0.469900 0.117 Uiso 0.5 1 calc R U P A -1
H48C H 0.150046 0.698834 0.419880 0.117 Uiso 0.5 1 calc R U P A -1
C54 C 0.2033(8) 0.382(2) 0.4933(10) 0.111(10) Uani 0.5 1 d D U P B -1
H54A H 0.189296 0.357044 0.464486 0.166 Uiso 0.5 1 calc R U P B -1
H54B H 0.199211 0.444198 0.492669 0.166 Uiso 0.5 1 calc R U P B -1
H54C H 0.185765 0.357903 0.519437 0.166 Uiso 0.5 1 calc R U P B -1
C55 C 0.2590(8) 0.3593(17) 0.4987(13) 0.089(8) Uani 0.5 1 d D U P B -1
H55A H 0.279358 0.411179 0.493418 0.107 Uiso 0.5 1 calc R U P B -1
H55B H 0.267025 0.338079 0.530287 0.107 Uiso 0.5 1 calc R U P B -1
C56 C 0.2707(7) 0.2899(14) 0.4633(7) 0.083(6) Uani 0.5 1 d D U P B -1
H56A H 0.250471 0.238198 0.469141 0.100 Uiso 0.5 1 calc R U P B -1
H56B H 0.261274 0.311061 0.431916 0.100 Uiso 0.5 1 calc R U P B -1
C57 C 0.3255(8) 0.2655(15) 0.4653(8) 0.092(7) Uani 0.5 1 d D U P B -1
H57A H 0.335449 0.245343 0.496705 0.110 Uiso 0.5 1 calc R U P B -1
H57B H 0.345985 0.316448 0.458295 0.110 Uiso 0.5 1 calc R U P B -1
C58 C 0.3346(9) 0.1947(15) 0.4304(7) 0.076(8) Uani 0.5 1 d D U P B -1
H58A H 0.320794 0.211568 0.399486 0.091 Uiso 0.5 1 calc R U P B -1
H58B H 0.318176 0.140907 0.439696 0.091 Uiso 0.5 1 calc R U P B -1
C59 C 0.3910(10) 0.181(2) 0.4289(14) 0.089(10) Uani 0.5 1 d D U P B -1
H59A H 0.403893 0.212952 0.402740 0.134 Uiso 0.5 1 calc R U P B -1
H59B H 0.398179 0.119977 0.425463 0.134 Uiso 0.5 1 calc R U P B -1
H59C H 0.407187 0.202461 0.457684 0.134 Uiso 0.5 1 calc R U P B -1
H45 H 0.470(3) 0.361(5) 0.516(3) 0.05(2) Uiso 1 1 d . . . . .
H46 H 0.529(3) 0.375(6) 0.458(3) 0.06(3) Uiso 1 1 d . . . . .
C60 C 0.3904(9) 0.224(2) 0.4365(11) 0.080(9) Uani 0.5 1 d D U P C -2
H60A H 0.408364 0.237987 0.408704 0.120 Uiso 0.5 1 calc R U P C -2
H60B H 0.413503 0.198261 0.459583 0.120 Uiso 0.5 1 calc R U P C -2
H60C H 0.376209 0.276713 0.449032 0.120 Uiso 0.5 1 calc R U P C -2
C61 C 0.3490(12) 0.161(2) 0.4243(9) 0.107(11) Uani 0.5 1 d D U P C -2
H61A H 0.325856 0.188003 0.400914 0.129 Uiso 0.5 1 calc R U P C -2
H61B H 0.363469 0.109634 0.410265 0.129 Uiso 0.5 1 calc R U P C -2
C62 C 0.3202(7) 0.1350(15) 0.4649(6) 0.072(6) Uani 0.5 1 d D U P C -2
H62A H 0.344541 0.111688 0.488233 0.086 Uiso 0.5 1 calc R U P C -2
H62B H 0.306321 0.188022 0.478128 0.086 Uiso 0.5 1 calc R U P C -2
C63 C 0.2794(12) 0.073(2) 0.4602(7) 0.132(10) Uani 0.5 1 d D U P C -2
H63A H 0.291563 0.024006 0.442260 0.159 Uiso 0.5 1 calc R U P C -2
H63B H 0.252374 0.100686 0.441228 0.159 Uiso 0.5 1 calc R U P C -2
C64 C 0.2566(19) 0.0376(16) 0.5022(12) 0.097(10) Uani 0.5 1 d D U P C -2
H64A H 0.281250 0.042283 0.528395 0.117 Uiso 0.5 1 calc R U P C -2
H64B H 0.227671 0.073962 0.509430 0.117 Uiso 0.5 1 calc R U P C -2
C65 C 0.2395(15) -0.0530(16) 0.4988(13) 0.115(14) Uani 0.5 1 d D U P C -2
H65A H 0.245480 -0.075280 0.467967 0.173 Uiso 0.5 1 calc R U P C -2
H65B H 0.203757 -0.055789 0.504383 0.173 Uiso 0.5 1 calc R U P C -2
H65C H 0.257960 -0.087680 0.522010 0.173 Uiso 0.5 1 calc R U P C -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 K1 4.2052(14) 4 ?
U1 K1 4.3349(14) . ?
U1 O2 1.788(4) . ?
U1 O1 1.798(4) . ?
U1 N5 2.501(5) . ?
U1 N4 2.566(5) . ?
U1 N3 2.523(5) . ?
U1 N6 2.599(5) . ?
U1 N7 2.330(4) . ?
K1 Na1 3.538(3) 4_545 ?
K1 O2 2.771(4) . ?
K1 O1 2.900(4) 4_545 ?
K1 N1 2.801(5) 4_545 ?
K1 N3 3.217(5) 4_545 ?
K1 C15 3.277(6) 4_545 ?
K1 C17 3.326(7) 4_545 ?
K1 N2 3.294(5) 4_545 ?
K1 C18 3.220(7) 4_545 ?
K1 C7 3.406(6) 4_545 ?
K1 C16 3.338(7) 4_545 ?
Si1 N7 1.744(6) . ?
Si1 C37 1.864(7) . ?
Si1 C39 1.885(7) . ?
Si1 C38 1.865(7) . ?
Si2 N7 1.748(6) . ?
Si2 C42 1.894(8) . ?
Si2 C41 1.884(8) . ?
Si2 C40 1.863(8) . ?
Na1 O1 2.508(5) . ?
Na1 N5 2.725(6) . ?
Na1 N1 2.352(6) . ?
Na1 N6 3.021(6) . ?
Na1 N2 2.503(6) . ?
Na1 N8 2.451(6) . ?
N5 C26 1.366(7) . ?
N5 C29 1.379(8) . ?
N1 C4 1.341(8) . ?
N1 C7 1.386(8) . ?
N4 C19 1.298(8) . ?
N4 C20 1.480(8) . ?
N3 C15 1.370(8) . ?
N3 C18 1.386(8) . ?
N6 C30 1.299(8) . ?
N6 C31 1.480(8) . ?
C15 C3 1.526(8) . ?
C15 C16 1.391(9) . ?
C26 C3 1.506(9) . ?
C26 C27 1.388(8) . ?
C17 H17 1.0000 . ?
C17 C18 1.409(9) . ?
C17 C16 1.381(9) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.510(9) . ?
N2 C8 1.292(8) . ?
N2 C9 1.461(8) . ?
C3 C4 1.535(9) . ?
C3 C2 1.548(8) . ?
C4 C5 1.398(8) . ?
C18 C19 1.403(9) . ?
C5 H5 0.9500 . ?
C5 C6 1.394(9) . ?
C19 H19 0.9500 . ?
C7 C8 1.422(9) . ?
C7 C6 1.394(8) . ?
N8 C47 1.336(9) . ?
N8 C43 1.339(8) . ?
C8 H8 0.9500 . ?
C6 H6 0.9500 . ?
C29 C28 1.393(8) . ?
C29 C30 1.427(8) . ?
C20 H20 1.0000 . ?
C20 C21 1.528(10) . ?
C20 C25 1.522(10) . ?
C27 H27 0.9500 . ?
C27 C28 1.390(9) . ?
C16 H16 1.0000 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C9 1.531(9) . ?
C10 C11 1.528(10) . ?
C28 H28 0.9500 . ?
C30 H30 0.9500 . ?
C31 H31 1.0000 . ?
C31 C32 1.527(10) . ?
C31 C36 1.522(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.535(9) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C24 1.539(9) . ?
C9 H9 1.0000 . ?
C9 C14 1.520(9) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.523(10) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.526(9) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C12 1.520(10) . ?
C13 C14 1.526(9) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C22 1.521(11) . ?
C23 C24 1.506(12) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C46 C47 1.385(10) . ?
C46 C45 1.386(12) . ?
C46 H46 0.96(9) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.540(10) . ?
C35 C34 1.532(13) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C44 H44 0.9500 . ?
C44 C43 1.383(11) . ?
C44 C45 1.377(12) . ?
C47 H47 0.9500 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.501(12) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C43 H43 0.9500 . ?
C45 H45 0.95(9) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C53 C52 1.474(13) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C52 C51 1.456(13) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C51 C50 1.466(12) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C50 C49 1.465(13) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C48 1.474(14) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C54 C55 1.537(15) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C55 C56 1.532(15) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 C57 1.517(14) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57 C58 1.523(14) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C58 C59 1.531(15) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C60 C61 1.509(15) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 C62 1.493(14) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C62 C63 1.458(14) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C63 C64 1.492(15) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C64 C65 1.485(14) . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
K1 U1 K1 134.627(8) 4 . ?
O2 U1 K1 143.75(14) . 4 ?
O2 U1 K1 22.64(13) . . ?
O2 U1 O1 175.79(19) . . ?
O2 U1 N5 85.89(17) . . ?
O2 U1 N4 86.87(18) . . ?
O2 U1 N3 93.97(18) . . ?
O2 U1 N6 94.22(19) . . ?
O2 U1 N7 90.00(19) . . ?
O1 U1 K1 153.40(13) . . ?
O1 U1 K1 34.18(13) . 4 ?
O1 U1 N5 89.96(17) . . ?
O1 U1 N4 95.49(18) . . ?
O1 U1 N3 83.79(17) . . ?
O1 U1 N6 84.62(19) . . ?
O1 U1 N7 93.76(19) . . ?
N5 U1 K1 63.78(11) . . ?
N5 U1 K1 80.32(11) . 4 ?
N5 U1 N4 133.17(16) . . ?
N5 U1 N3 67.71(16) . . ?
N5 U1 N6 64.74(16) . . ?
N4 U1 K1 78.81(12) . 4 ?
N4 U1 K1 105.48(12) . . ?
N4 U1 N6 162.04(16) . . ?
N3 U1 K1 89.55(12) . . ?
N3 U1 K1 49.78(12) . 4 ?
N3 U1 N4 66.75(16) . . ?
N3 U1 N6 130.90(16) . . ?
N6 U1 K1 109.47(12) . 4 ?
N6 U1 K1 80.40(13) . . ?
N7 U1 K1 104.77(15) . . ?
N7 U1 K1 120.49(15) . 4 ?
N7 U1 N5 143.23(16) . . ?
N7 U1 N4 82.88(16) . . ?
N7 U1 N3 149.06(16) . . ?
N7 U1 N6 79.20(16) . . ?
Na1 K1 U1 53.19(4) 4_545 4_545 ?
O2 K1 U1 173.49(10) . 4_545 ?
O2 K1 Na1 126.15(11) . 4_545 ?
O2 K1 O1 153.77(13) . 4_545 ?
O2 K1 N1 107.72(14) . 4_545 ?
O2 K1 N3 149.10(14) . 4_545 ?
O2 K1 C15 129.26(15) . 4_545 ?
O2 K1 C17 110.14(16) . 4_545 ?
O2 K1 N2 83.97(14) . 4_545 ?
O2 K1 C18 132.74(16) . 4_545 ?
O2 K1 C7 85.85(14) . 4_545 ?
O2 K1 C16 108.87(15) . 4_545 ?
O1 K1 U1 20.38(8) 4_545 4_545 ?
O1 K1 Na1 44.49(9) 4_545 4_545 ?
O1 K1 N3 57.09(13) 4_545 4_545 ?
O1 K1 C15 75.98(14) 4_545 4_545 ?
O1 K1 C17 94.26(15) 4_545 4_545 ?
O1 K1 N2 79.59(13) 4_545 4_545 ?
O1 K1 C18 70.02(15) 4_545 4_545 ?
O1 K1 C7 95.10(13) 4_545 4_545 ?
O1 K1 C16 97.33(15) 4_545 4_545 ?
N1 K1 U1 76.00(10) 4_545 4_545 ?
N1 K1 Na1 41.56(11) 4_545 4_545 ?
N1 K1 O1 78.99(13) 4_545 4_545 ?
N1 K1 N3 71.25(14) 4_545 4_545 ?
N1 K1 C15 56.41(15) 4_545 4_545 ?
N1 K1 C17 94.03(16) 4_545 4_545 ?
N1 K1 N2 54.73(15) 4_545 4_545 ?
N1 K1 C18 94.11(16) 4_545 4_545 ?
N1 K1 C7 23.29(14) 4_545 4_545 ?
N1 K1 C16 71.48(16) 4_545 4_545 ?
N3 K1 U1 36.80(9) 4_545 4_545 ?
N3 K1 Na1 74.52(10) 4_545 4_545 ?
N3 K1 C15 24.33(14) 4_545 4_545 ?
N3 K1 C17 41.15(15) 4_545 4_545 ?
N3 K1 N2 115.95(14) 4_545 4_545 ?
N3 K1 C18 24.87(14) 4_545 4_545 ?
N3 K1 C7 94.10(14) 4_545 4_545 ?
N3 K1 C16 40.55(15) 4_545 4_545 ?
C15 K1 U1 57.23(11) 4_545 4_545 ?
C15 K1 Na1 76.58(12) 4_545 4_545 ?
C15 K1 C17 39.63(16) 4_545 4_545 ?
C15 K1 N2 109.79(15) 4_545 4_545 ?
C15 K1 C7 76.54(15) 4_545 4_545 ?
C15 K1 C16 24.26(15) 4_545 4_545 ?
C17 K1 U1 74.49(12) 4_545 4_545 ?
C17 K1 Na1 114.02(13) 4_545 4_545 ?
C17 K1 C7 109.65(16) 4_545 4_545 ?
C17 K1 C16 23.92(15) 4_545 4_545 ?
N2 K1 U1 94.22(10) 4_545 4_545 ?
N2 K1 Na1 42.79(11) 4_545 4_545 ?
N2 K1 C17 148.74(15) 4_545 4_545 ?
N2 K1 C7 41.71(14) 4_545 4_545 ?
N2 K1 C16 125.85(15) 4_545 4_545 ?
C18 K1 U1 50.98(12) 4_545 4_545 ?
C18 K1 Na1 98.07(13) 4_545 4_545 ?
C18 K1 C15 39.28(15) 4_545 4_545 ?
C18 K1 C17 24.79(16) 4_545 4_545 ?
C18 K1 N2 140.47(16) 4_545 4_545 ?
C18 K1 C7 115.63(16) 4_545 4_545 ?
C18 K1 C16 39.57(16) 4_545 4_545 ?
C7 K1 U1 96.98(11) 4_545 4_545 ?
C7 K1 Na1 51.43(11) 4_545 4_545 ?
C16 K1 U1 77.26(12) 4_545 4_545 ?
C16 K1 Na1 99.84(13) 4_545 4_545 ?
C16 K1 C7 85.74(16) 4_545 4_545 ?
N7 Si1 C37 114.3(3) . . ?
N7 Si1 C39 113.2(3) . . ?
N7 Si1 C38 114.4(3) . . ?
C37 Si1 C39 103.7(3) . . ?
C37 Si1 C38 103.9(4) . . ?
C38 Si1 C39 106.3(3) . . ?
N7 Si2 C42 113.1(3) . . ?
N7 Si2 C41 112.2(3) . . ?
N7 Si2 C40 115.9(3) . . ?
C41 Si2 C42 107.4(4) . . ?
C40 Si2 C42 103.7(4) . . ?
C40 Si2 C41 103.7(4) . . ?
O1 Na1 K1 54.12(11) . 4 ?
O1 Na1 N5 71.96(15) . . ?
O1 Na1 N6 65.41(15) . . ?
N5 Na1 K1 91.37(12) . 4 ?
N5 Na1 N6 56.50(15) . . ?
N1 Na1 K1 52.18(14) . 4 ?
N1 Na1 O1 96.47(18) . . ?
N1 Na1 N5 76.03(18) . . ?
N1 Na1 N6 132.15(19) . . ?
N1 Na1 N2 71.41(19) . . ?
N1 Na1 N8 100.5(2) . . ?
N6 Na1 K1 118.13(13) . 4 ?
N2 Na1 K1 63.40(14) . 4 ?
N2 Na1 O1 105.03(18) . . ?
N2 Na1 N5 146.78(19) . . ?
N2 Na1 N6 153.67(19) . . ?
N8 Na1 K1 149.52(16) . 4 ?
N8 Na1 O1 155.1(2) . . ?
N8 Na1 N5 94.5(2) . . ?
N8 Na1 N6 89.65(19) . . ?
N8 Na1 N2 97.7(2) . . ?
U1 O2 K1 143.0(2) . . ?
U1 O1 K1 125.44(19) . 4 ?
U1 O1 Na1 108.43(19) . . ?
Na1 O1 K1 81.39(12) . 4 ?
U1 N5 Na1 84.50(15) . . ?
C26 N5 U1 135.4(4) . . ?
C26 N5 Na1 115.3(4) . . ?
C26 N5 C29 105.3(5) . . ?
C29 N5 U1 108.0(4) . . ?
C29 N5 Na1 103.6(4) . . ?
Na1 N1 K1 86.27(17) . 4 ?
C4 N1 K1 119.6(4) . 4 ?
C4 N1 Na1 132.8(4) . . ?
C4 N1 C7 105.9(5) . . ?
C7 N1 K1 103.7(4) . 4 ?
C7 N1 Na1 104.5(4) . . ?
C19 N4 U1 114.0(4) . . ?
C19 N4 C20 116.9(6) . . ?
C20 N4 U1 128.9(4) . . ?
U1 N3 K1 93.42(15) . 4 ?
C15 N3 U1 139.5(4) . . ?
C15 N3 K1 80.3(3) . 4 ?
C15 N3 C18 104.9(5) . . ?
C18 N3 U1 112.8(4) . . ?
C18 N3 K1 77.7(3) . 4 ?
U1 N6 Na1 77.09(15) . . ?
C30 N6 U1 109.6(4) . . ?
C30 N6 Na1 94.5(4) . . ?
C30 N6 C31 119.2(6) . . ?
C31 N6 U1 129.9(4) . . ?
C31 N6 Na1 108.2(4) . . ?
N3 C15 K1 75.4(3) . 4 ?
N3 C15 C3 124.0(5) . . ?
N3 C15 C16 110.9(5) . . ?
C3 C15 K1 112.1(4) . 4 ?
C16 C15 K1 80.3(4) . 4 ?
C16 C15 C3 125.1(5) . . ?
N5 C26 C3 122.7(5) . . ?
N5 C26 C27 110.3(6) . . ?
C27 C26 C3 126.5(5) . . ?
K1 C17 H17 126.2 4 . ?
C18 C17 K1 73.4(4) . 4 ?
C18 C17 H17 126.2 . . ?
C16 C17 K1 78.5(4) . 4 ?
C16 C17 H17 126.2 . . ?
C16 C17 C18 105.6(6) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
Na1 N2 K1 73.81(14) . 4 ?
C8 N2 K1 92.1(4) . 4 ?
C8 N2 Na1 102.6(4) . . ?
C8 N2 C9 118.0(5) . . ?
C9 N2 K1 125.3(4) . 4 ?
C9 N2 Na1 132.0(4) . . ?
C15 C3 C4 106.0(5) . . ?
C15 C3 C2 108.5(4) . . ?
C26 C3 C15 113.9(4) . . ?
C26 C3 C4 108.2(4) . . ?
C26 C3 C2 110.7(6) . . ?
C4 C3 C2 109.4(4) . . ?
N1 C4 C3 119.0(5) . . ?
N1 C4 C5 111.2(6) . . ?
C5 C4 C3 129.8(6) . . ?
N3 C18 K1 77.4(3) . 4 ?
N3 C18 C17 110.9(5) . . ?
N3 C18 C19 119.6(6) . . ?
C17 C18 K1 81.8(4) . 4 ?
C19 C18 K1 113.8(4) . 4 ?
C19 C18 C17 129.1(6) . . ?
Si1 N7 U1 121.5(3) . . ?
Si1 N7 Si2 116.0(2) . . ?
Si2 N7 U1 122.5(3) . . ?
C4 C5 H5 126.7 . . ?
C6 C5 C4 106.6(6) . . ?
C6 C5 H5 126.7 . . ?
N4 C19 C18 122.7(6) . . ?
N4 C19 H19 118.6 . . ?
C18 C19 H19 118.6 . . ?
N1 C7 K1 53.0(3) . 4 ?
N1 C7 C8 120.5(5) . . ?
N1 C7 C6 110.3(6) . . ?
C8 C7 K1 85.3(3) . 4 ?
C6 C7 K1 130.7(4) . 4 ?
C6 C7 C8 129.2(6) . . ?
C47 N8 Na1 106.1(4) . . ?
C47 N8 C43 116.5(6) . . ?
C43 N8 Na1 137.1(5) . . ?
N2 C8 C7 123.2(6) . . ?
N2 C8 H8 118.4 . . ?
C7 C8 H8 118.4 . . ?
C5 C6 C7 106.0(5) . . ?
C5 C6 H6 127.0 . . ?
C7 C6 H6 127.0 . . ?
N5 C29 C28 111.3(5) . . ?
N5 C29 C30 118.4(5) . . ?
C28 C29 C30 129.4(6) . . ?
N4 C20 H20 107.3 . . ?
N4 C20 C21 114.7(6) . . ?
N4 C20 C25 108.5(5) . . ?
C21 C20 H20 107.3 . . ?
C25 C20 H20 107.3 . . ?
C25 C20 C21 111.4(6) . . ?
C26 C27 H27 126.0 . . ?
C26 C27 C28 107.9(6) . . ?
C28 C27 H27 126.0 . . ?
K1 C16 H16 125.2 4 . ?
C15 C16 K1 75.4(4) . 4 ?
C15 C16 H16 125.2 . . ?
C17 C16 K1 77.6(4) . 4 ?
C17 C16 C15 107.8(6) . . ?
C17 C16 H16 125.2 . . ?
H10A C10 H10B 108.1 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
C11 C10 C9 110.8(6) . . ?
C29 C28 H28 127.4 . . ?
C27 C28 C29 105.2(6) . . ?
C27 C28 H28 127.4 . . ?
N6 C30 C29 119.5(6) . . ?
N6 C30 H30 120.2 . . ?
C29 C30 H30 120.2 . . ?
N6 C31 H31 107.3 . . ?
N6 C31 C32 107.7(5) . . ?
N6 C31 C36 116.5(6) . . ?
C32 C31 H31 107.3 . . ?
C36 C31 H31 107.3 . . ?
C36 C31 C32 110.3(6) . . ?
C1 C2 C3 114.9(5) . . ?
C1 C2 H2A 108.5 . . ?
C1 C2 H2B 108.5 . . ?
C3 C2 H2A 108.5 . . ?
C3 C2 H2B 108.5 . . ?
H2A C2 H2B 107.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 C22 110.9(7) . . ?
H21A C21 H21B 108.0 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
Si1 C37 H37A 109.5 . . ?
Si1 C37 H37B 109.5 . . ?
Si1 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C20 C25 H25A 109.4 . . ?
C20 C25 H25B 109.4 . . ?
C20 C25 C24 111.1(6) . . ?
H25A C25 H25B 108.0 . . ?
C24 C25 H25A 109.4 . . ?
C24 C25 H25B 109.4 . . ?
N2 C9 C10 109.6(5) . . ?
N2 C9 H9 108.5 . . ?
N2 C9 C14 110.6(6) . . ?
C10 C9 H9 108.5 . . ?
C14 C9 C10 111.2(5) . . ?
C14 C9 H9 108.5 . . ?
Si1 C39 H39A 109.5 . . ?
Si1 C39 H39B 109.5 . . ?
Si1 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
Si2 C42 H42A 109.5 . . ?
Si2 C42 H42B 109.5 . . ?
Si2 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C10 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 C10 111.5(6) . . ?
C12 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C31 C32 H32A 108.9 . . ?
C31 C32 H32B 108.9 . . ?
H32A C32 H32B 107.7 . . ?
C33 C32 C31 113.3(6) . . ?
C33 C32 H32A 108.9 . . ?
C33 C32 H32B 108.9 . . ?
H13A C13 H13B 108.0 . . ?
C12 C13 H13A 109.4 . . ?
C12 C13 H13B 109.4 . . ?
C12 C13 C14 111.3(6) . . ?
C14 C13 H13A 109.4 . . ?
C14 C13 H13B 109.4 . . ?
H23A C23 H23B 107.9 . . ?
C22 C23 H23A 109.3 . . ?
C22 C23 H23B 109.3 . . ?
C24 C23 H23A 109.3 . . ?
C24 C23 H23B 109.3 . . ?
C24 C23 C22 111.7(7) . . ?
Si1 C38 H38A 109.5 . . ?
Si1 C38 H38B 109.5 . . ?
Si1 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C47 C46 C45 118.0(8) . . ?
C47 C46 H46 119(6) . . ?
C45 C46 H46 123(6) . . ?
Si2 C41 H41A 109.5 . . ?
Si2 C41 H41B 109.5 . . ?
Si2 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
H35A C35 H35B 108.3 . . ?
C36 C35 H35A 109.9 . . ?
C36 C35 H35B 109.9 . . ?
C34 C35 H35A 109.9 . . ?
C34 C35 H35B 109.9 . . ?
C34 C35 C36 108.9(7) . . ?
C31 C36 C35 111.6(7) . . ?
C31 C36 H36A 109.3 . . ?
C31 C36 H36B 109.3 . . ?
C35 C36 H36A 109.3 . . ?
C35 C36 H36B 109.3 . . ?
H36A C36 H36B 108.0 . . ?
Si2 C40 H40A 109.5 . . ?
Si2 C40 H40B 109.5 . . ?
Si2 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C43 C44 H44 120.8 . . ?
C45 C44 H44 120.8 . . ?
C45 C44 C43 118.3(7) . . ?
N8 C47 C46 124.0(7) . . ?
N8 C47 H47 118.0 . . ?
C46 C47 H47 118.0 . . ?
C32 C33 H33A 109.2 . . ?
C32 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
C34 C33 C32 112.0(7) . . ?
C34 C33 H33A 109.2 . . ?
C34 C33 H33B 109.2 . . ?
C11 C12 H12A 109.2 . . ?
C11 C12 H12B 109.2 . . ?
C13 C12 C11 112.1(6) . . ?
C13 C12 H12A 109.2 . . ?
C13 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
C9 C14 C13 112.2(6) . . ?
C9 C14 H14A 109.2 . . ?
C9 C14 H14B 109.2 . . ?
C13 C14 H14A 109.2 . . ?
C13 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C35 C34 H34A 109.6 . . ?
C35 C34 H34B 109.6 . . ?
C33 C34 C35 110.4(6) . . ?
C33 C34 H34A 109.6 . . ?
C33 C34 H34B 109.6 . . ?
H34A C34 H34B 108.1 . . ?
N8 C43 C44 124.0(8) . . ?
N8 C43 H43 118.0 . . ?
C44 C43 H43 118.0 . . ?
C46 C45 H45 118(6) . . ?
C44 C45 C46 119.2(7) . . ?
C44 C45 H45 122(6) . . ?
C21 C22 H22A 109.4 . . ?
C21 C22 H22B 109.4 . . ?
C23 C22 C21 111.1(6) . . ?
C23 C22 H22A 109.4 . . ?
C23 C22 H22B 109.4 . . ?
H22A C22 H22B 108.0 . . ?
C25 C24 H24A 109.2 . . ?
C25 C24 H24B 109.2 . . ?
C23 C24 C25 112.3(7) . . ?
C23 C24 H24A 109.2 . . ?
C23 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
C53 C52 H52A 107.1 . . ?
C53 C52 H52B 107.1 . . ?
H52A C52 H52B 106.8 . . ?
C51 C52 C53 120.8(17) . . ?
C51 C52 H52A 107.1 . . ?
C51 C52 H52B 107.1 . . ?
C52 C51 H51A 106.3 . . ?
C52 C51 H51B 106.3 . . ?
C52 C51 C50 123.9(17) . . ?
H51A C51 H51B 106.4 . . ?
C50 C51 H51A 106.3 . . ?
C50 C51 H51B 106.3 . . ?
C51 C50 H50A 107.2 . . ?
C51 C50 H50B 107.2 . . ?
H50A C50 H50B 106.8 . . ?
C49 C50 C51 120.5(15) . . ?
C49 C50 H50A 107.2 . . ?
C49 C50 H50B 107.2 . . ?
C50 C49 H49A 107.3 . . ?
C50 C49 H49B 107.3 . . ?
C50 C49 C48 120(2) . . ?
H49A C49 H49B 106.9 . . ?
C48 C49 H49A 107.3 . . ?
C48 C49 H49B 107.3 . . ?
C49 C48 H48A 109.5 . . ?
C49 C48 H48B 109.5 . . ?
C49 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C55 C54 H54A 109.5 . . ?
C55 C54 H54B 109.5 . . ?
C55 C54 H54C 109.5 . . ?
C54 C55 H55A 110.0 . . ?
C54 C55 H55B 110.0 . . ?
H55A C55 H55B 108.4 . . ?
C56 C55 C54 108.6(18) . . ?
C56 C55 H55A 110.0 . . ?
C56 C55 H55B 110.0 . . ?
C55 C56 H56A 109.2 . . ?
C55 C56 H56B 109.2 . . ?
H56A C56 H56B 107.9 . . ?
C57 C56 C55 112.1(15) . . ?
C57 C56 H56A 109.2 . . ?
C57 C56 H56B 109.2 . . ?
C56 C57 H57A 109.7 . . ?
C56 C57 H57B 109.7 . . ?
C56 C57 C58 109.7(16) . . ?
H57A C57 H57B 108.2 . . ?
C58 C57 H57A 109.7 . . ?
C58 C57 H57B 109.7 . . ?
C57 C58 H58A 110.2 . . ?
C57 C58 H58B 110.2 . . ?
C57 C58 C59 107.7(16) . . ?
H58A C58 H58B 108.5 . . ?
C59 C58 H58A 110.2 . . ?
C59 C58 H58B 110.2 . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C61 C60 H60A 109.5 . . ?
C61 C60 H60B 109.5 . . ?
C61 C60 H60C 109.5 . . ?
C60 C61 H61A 108.9 . . ?
C60 C61 H61B 108.9 . . ?
H61A C61 H61B 107.7 . . ?
C62 C61 C60 113.2(19) . . ?
C62 C61 H61A 108.9 . . ?
C62 C61 H61B 108.9 . . ?
C61 C62 H62A 107.0 . . ?
C61 C62 H62B 107.0 . . ?
H62A C62 H62B 106.7 . . ?
C63 C62 C61 121.4(17) . . ?
C63 C62 H62A 107.0 . . ?
C63 C62 H62B 107.0 . . ?
C62 C63 H63A 107.3 . . ?
C62 C63 H63B 107.3 . . ?
C62 C63 C64 120(2) . . ?
H63A C63 H63B 106.9 . . ?
C64 C63 H63A 107.3 . . ?
C64 C63 H63B 107.3 . . ?
C63 C64 H64A 108.3 . . ?
C63 C64 H64B 108.3 . . ?
H64A C64 H64B 107.4 . . ?
C65 C64 C63 116(2) . . ?
C65 C64 H64A 108.3 . . ?
C65 C64 H64B 108.3 . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 N5 C26 C3 52.0(8) . . . . ?
U1 N5 C26 C27 -135.9(5) . . . . ?
U1 N5 C29 C28 149.0(4) . . . . ?
U1 N5 C29 C30 -40.6(6) . . . . ?
U1 N4 C19 C18 6.3(8) . . . . ?
U1 N4 C20 C21 139.2(5) . . . . ?
U1 N4 C20 C25 -95.6(6) . . . . ?
U1 N3 C15 K1 -83.9(5) . . . 4 ?
U1 N3 C15 C3 23.2(10) . . . . ?
U1 N3 C15 C16 -157.2(5) . . . . ?
U1 N3 C18 K1 88.6(3) . . . 4 ?
U1 N3 C18 C17 164.6(4) . . . . ?
U1 N3 C18 C19 -21.8(7) . . . . ?
U1 N6 C30 C29 25.1(7) . . . . ?
U1 N6 C31 C32 -86.3(6) . . . . ?
U1 N6 C31 C36 149.2(5) . . . . ?
K1 U1 O2 K1 79.4(4) 4 . . . ?
K1 U1 O1 K1 81.5(4) . . . 4 ?
K1 U1 O1 Na1 -92.5(2) 4 . . . ?
K1 U1 O1 Na1 -11.0(4) . . . . ?
K1 N1 C4 C3 -63.4(7) 4 . . . ?
K1 N1 C4 C5 116.7(5) 4 . . . ?
K1 N1 C7 C8 55.8(6) 4 . . . ?
K1 N1 C7 C6 -126.3(4) 4 . . . ?
K1 N3 C15 C3 107.1(6) 4 . . . ?
K1 N3 C15 C16 -73.4(5) 4 . . . ?
K1 N3 C18 C17 76.1(5) 4 . . . ?
K1 N3 C18 C19 -110.4(6) 4 . . . ?
K1 C15 C3 C26 94.5(5) 4 . . . ?
K1 C15 C3 C4 -24.3(5) 4 . . . ?
K1 C15 C3 C2 -141.7(4) 4 . . . ?
K1 C15 C16 C17 -71.6(5) 4 . . . ?
K1 C17 C18 N3 -73.1(5) 4 . . . ?
K1 C17 C18 C19 114.1(7) 4 . . . ?
K1 C17 C16 C15 70.1(5) 4 . . . ?
K1 N2 C8 C7 -45.8(6) 4 . . . ?
K1 N2 C9 C10 -8.2(7) 4 . . . ?
K1 N2 C9 C14 114.8(5) 4 . . . ?
K1 C18 C19 N4 -77.7(7) 4 . . . ?
K1 C7 C8 N2 44.1(6) 4 . . . ?
K1 C7 C6 C5 -59.1(7) 4 . . . ?
Na1 N5 C26 C3 -57.2(6) . . . . ?
Na1 N5 C26 C27 114.9(5) . . . . ?
Na1 N5 C29 C28 -122.5(4) . . . . ?
Na1 N5 C29 C30 48.0(6) . . . . ?
Na1 N1 C4 C3 51.8(8) . . . . ?
Na1 N1 C4 C5 -128.2(5) . . . . ?
Na1 N1 C7 K1 -89.7(3) . . . 4 ?
Na1 N1 C7 C8 -33.9(6) . . . . ?
Na1 N1 C7 C6 144.0(4) . . . . ?
Na1 N6 C30 C29 -52.8(6) . . . . ?
Na1 N6 C31 C32 1.8(6) . . . . ?
Na1 N6 C31 C36 -122.6(6) . . . . ?
Na1 N2 C8 C7 28.0(7) . . . . ?
Na1 N2 C9 C10 -108.5(6) . . . . ?
Na1 N2 C9 C14 14.5(8) . . . . ?
Na1 N8 C47 C46 -172.0(7) . . . . ?
Na1 N8 C43 C44 171.1(6) . . . . ?
N5 U1 O2 K1 11.9(4) . . . . ?
N5 U1 O1 K1 72.7(2) . . . 4 ?
N5 U1 O1 Na1 -19.84(19) . . . . ?
N5 C26 C3 C15 -41.7(8) . . . . ?
N5 C26 C3 C4 75.9(6) . . . . ?
N5 C26 C3 C2 -164.3(5) . . . . ?
N5 C26 C27 C28 -1.2(7) . . . . ?
N5 C29 C28 C27 0.2(7) . . . . ?
N5 C29 C30 N6 10.1(9) . . . . ?
N1 C4 C5 C6 -0.8(8) . . . . ?
N1 C7 C8 N2 2.6(9) . . . . ?
N1 C7 C6 C5 -1.0(7) . . . . ?
N4 U1 O2 K1 145.6(4) . . . . ?
N4 U1 O1 K1 -60.8(2) . . . 4 ?
N4 U1 O1 Na1 -153.25(18) . . . . ?
N4 C20 C21 C22 179.5(6) . . . . ?
N4 C20 C25 C24 178.4(7) . . . . ?
N3 U1 O2 K1 79.2(4) . . . . ?
N3 U1 O1 K1 5.1(2) . . . 4 ?
N3 U1 O1 Na1 -87.42(19) . . . . ?
N3 C15 C3 C26 7.7(9) . . . . ?
N3 C15 C3 C4 -111.1(6) . . . . ?
N3 C15 C3 C2 131.5(6) . . . . ?
N3 C15 C16 K1 70.1(4) . . . 4 ?
N3 C15 C16 C17 -1.4(7) . . . . ?
N3 C18 C19 N4 10.9(10) . . . . ?
N6 U1 O2 K1 -52.3(4) . . . . ?
N6 U1 O1 K1 137.3(2) . . . 4 ?
N6 U1 O1 Na1 44.79(18) . . . . ?
N6 C31 C32 C33 -179.1(6) . . . . ?
N6 C31 C36 C35 178.2(7) . . . . ?
C15 N3 C18 K1 -76.4(4) . . . 4 ?
C15 N3 C18 C17 -0.3(7) . . . . ?
C15 N3 C18 C19 173.3(6) . . . . ?
C15 C3 C4 N1 56.8(7) . . . . ?
C15 C3 C4 C5 -123.2(7) . . . . ?
C15 C3 C2 C1 -57.3(7) . . . . ?
C26 N5 C29 C28 -1.0(7) . . . . ?
C26 N5 C29 C30 169.5(5) . . . . ?
C26 C3 C4 N1 -65.7(7) . . . . ?
C26 C3 C4 C5 114.2(7) . . . . ?
C26 C3 C2 C1 68.4(6) . . . . ?
C26 C27 C28 C29 0.6(7) . . . . ?
C17 C18 C19 N4 -176.8(7) . . . . ?
N2 C9 C14 C13 -176.9(5) . . . . ?
C3 C15 C16 K1 -110.3(6) . . . 4 ?
C3 C15 C16 C17 178.1(6) . . . . ?
C3 C26 C27 C28 170.5(5) . . . . ?
C3 C4 C5 C6 179.3(6) . . . . ?
C4 N1 C7 K1 126.8(5) . . . 4 ?
C4 N1 C7 C8 -177.4(6) . . . . ?
C4 N1 C7 C6 0.5(7) . . . . ?
C4 C3 C2 C1 -172.5(5) . . . . ?
C4 C5 C6 C7 1.1(7) . . . . ?
C18 N3 C15 K1 74.4(4) . . . 4 ?
C18 N3 C15 C3 -178.5(6) . . . . ?
C18 N3 C15 C16 1.0(7) . . . . ?
C18 C17 C16 K1 -68.9(5) . . . 4 ?
C18 C17 C16 C15 1.2(7) . . . . ?
N7 U1 O2 K1 -131.5(4) . . . . ?
N7 U1 O1 K1 -144.0(2) . . . 4 ?
N7 U1 O1 Na1 123.55(19) . . . . ?
C19 N4 C20 C21 -46.0(8) . . . . ?
C19 N4 C20 C25 79.2(7) . . . . ?
C7 N1 C4 C3 -179.9(5) . . . . ?
C7 N1 C4 C5 0.2(7) . . . . ?
C8 N2 C9 C10 107.2(7) . . . . ?
C8 N2 C9 C14 -129.8(6) . . . . ?
C8 C7 C6 C5 176.7(6) . . . . ?
C6 C7 C8 N2 -174.9(6) . . . . ?
C29 N5 C26 C3 -170.8(5) . . . . ?
C29 N5 C26 C27 1.3(6) . . . . ?
C20 N4 C19 C18 -169.3(6) . . . . ?
C20 C21 C22 C23 -55.8(9) . . . . ?
C20 C25 C24 C23 53.9(9) . . . . ?
C27 C26 C3 C15 147.6(6) . . . . ?
C27 C26 C3 C4 -94.9(7) . . . . ?
C27 C26 C3 C2 25.0(8) . . . . ?
C16 C15 C3 C26 -171.8(6) . . . . ?
C16 C15 C3 C4 69.4(7) . . . . ?
C16 C15 C3 C2 -48.0(8) . . . . ?
C16 C17 C18 K1 72.6(5) . . . 4 ?
C16 C17 C18 N3 -0.5(8) . . . . ?
C16 C17 C18 C19 -173.4(7) . . . . ?
C10 C9 C14 C13 -54.9(8) . . . . ?
C10 C11 C12 C13 54.7(8) . . . . ?
C28 C29 C30 N6 178.6(6) . . . . ?
C30 N6 C31 C32 108.0(7) . . . . ?
C30 N6 C31 C36 -16.5(9) . . . . ?
C30 C29 C28 C27 -168.9(6) . . . . ?
C31 N6 C30 C29 -166.5(6) . . . . ?
C31 C32 C33 C34 52.4(8) . . . . ?
C2 C3 C4 N1 173.6(5) . . . . ?
C2 C3 C4 C5 -6.4(9) . . . . ?
C21 C20 C25 C24 -54.5(9) . . . . ?
C37 Si1 N7 U1 14.9(4) . . . . ?
C37 Si1 N7 Si2 -161.9(3) . . . . ?
C25 C20 C21 C22 55.9(8) . . . . ?
C9 N2 C8 C7 -178.3(6) . . . . ?
C9 C10 C11 C12 -55.2(8) . . . . ?
C39 Si1 N7 U1 133.3(3) . . . . ?
C39 Si1 N7 Si2 -43.4(4) . . . . ?
C42 Si2 N7 U1 144.3(3) . . . . ?
C42 Si2 N7 Si1 -38.9(4) . . . . ?
C11 C10 C9 N2 177.8(5) . . . . ?
C11 C10 C9 C14 55.2(7) . . . . ?
C32 C31 C36 C35 55.1(9) . . . . ?
C32 C33 C34 C35 -56.3(8) . . . . ?
C38 Si1 N7 U1 -104.6(3) . . . . ?
C38 Si1 N7 Si2 78.6(4) . . . . ?
C41 Si2 N7 U1 -94.0(4) . . . . ?
C41 Si2 N7 Si1 82.7(4) . . . . ?
C36 C31 C32 C33 -51.0(8) . . . . ?
C36 C35 C34 C33 59.5(9) . . . . ?
C40 Si2 N7 U1 24.8(5) . . . . ?
C40 Si2 N7 Si1 -158.5(4) . . . . ?
C47 N8 C43 C44 -0.7(12) . . . . ?
C47 C46 C45 C44 0.8(13) . . . . ?
C12 C13 C14 C9 53.8(8) . . . . ?
C14 C13 C12 C11 -53.5(8) . . . . ?
C34 C35 C36 C31 -59.6(9) . . . . ?
C43 N8 C47 C46 2.1(11) . . . . ?
C43 C44 C45 C46 0.5(14) . . . . ?
C45 C46 C47 N8 -2.2(12) . . . . ?
C45 C44 C43 N8 -0.6(14) . . . . ?
C22 C23 C24 C25 -54.2(10) . . . . ?
C24 C23 C22 C21 55.1(10) . . . . ?
C53 C52 C51 C50 170(3) . . . . ?
C52 C51 C50 C49 -179(4) . . . . ?
C51 C50 C49 C48 167(3) . . . . ?
C54 C55 C56 C57 179(3) . . . . ?
C55 C56 C57 C58 178(2) . . . . ?
C56 C57 C58 C59 172(2) . . . . ?
C60 C61 C62 C63 -179(3) . . . . ?
C61 C62 C63 C64 170(4) . . . . ?
C62 C63 C64 C65 -145(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.5741(6)
2 0.4259(6)

_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_to517-pyr_twin1_hklf4_refinalised
_database_code_depnum_ccdc_archive 'CCDC 2313510'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2023-12-11 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_audit_creation_date             2023-11-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C87 H109 N15 O4 U2 Y2, C6 H14, [+ solvents]'
_chemical_formula_sum            'C93 H123 N15 O4 U2 Y2'
_chemical_formula_weight         2168.94
_chemical_melting_point          ?
_chemical_oxdiff_formula         C93H123N15U2O4Y2
_chemical_oxdiff_usercomment     pyr/hex
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'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.1503(3)
_cell_length_b                   16.1749(4)
_cell_length_c                   24.3853(7)
_cell_angle_alpha                79.382(2)
_cell_angle_beta                 82.241(2)
_cell_angle_gamma                85.201(2)
_cell_volume                     4658.7(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    30892
_cell_measurement_temperature    120.1(4)
_cell_measurement_theta_max      29.2200
_cell_measurement_theta_min      3.5450
_shelx_estimated_absorpt_T_max   0.590
_shelx_estimated_absorpt_T_min   0.198
_exptl_absorpt_coefficient_mu    4.755
_exptl_absorpt_correction_T_max  0.650
_exptl_absorpt_correction_T_min  0.311
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2160
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -22 -1 0.0508
-17 0 -3 0.2313
-1 22 0 0.0840
-1 -1 -34 0.0377
-2 1 33 0.0682
1 -1 -34 0.0575
1 -22 -4 0.0478
-17 2 -3 0.2336
0 23 4 0.0689
17 5 4 0.2604
2 1 34 0.1037
-1 16 28 0.0691
12 -11 17 0.1717

_exptl_crystal_size_max          0.504
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.124
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.1215 -22.4312 -0.6241 -0.3332 -0.9426 0.0232
-17.0773 -0.2434 -3.2340 0.0164 0.0489 -0.9987
-1.2412 22.2572 0.4075 0.3319 0.9391 -0.0886
-0.7859 -1.2705 -33.9807 0.9724 -0.2329 -0.0089
-2.1047 1.0140 32.9903 -0.9601 0.2298 -0.1595
0.5004 -1.1635 -33.6598 0.9703 -0.2325 0.0662
1.2650 -22.4933 -3.9462 -0.2318 -0.9682 0.0939
-16.8504 2.1624 -2.5670 0.0356 0.1522 -0.9877
0.0909 22.7025 4.2238 0.2329 0.9724 -0.0148
16.8967 5.4725 3.9902 0.0427 0.1748 0.9837
2.4044 1.3991 34.1125 -0.9672 0.2318 0.1037
-1.0807 15.9096 27.5935 -0.5637 0.8194 -0.1038
11.6112 -10.9611 16.6883 -0.6104 -0.4207 0.6712

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            93776
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.388
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.1(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -71.00  -3.00   1.00   30.00    --  -15.82 129.00-153.00   68
  2  ω    -78.00 -11.00   1.00   30.00    --  -15.82 141.00  18.00   67
  3  ω     11.00  80.00   1.00   30.00    --   17.54-141.00 -39.00   69
  4  ω      3.00  72.00   1.00   30.00    --   17.54-129.00 133.00   69
  5  ω    -43.00  39.00   1.00   30.00    --  -15.82  77.00-120.00   82
  6  ω    -83.00   1.00   1.00   30.00    --  -15.82 -57.00 -60.00   84
  7  ω    -88.00 -39.00   1.00   30.00    --  -15.82-178.00 120.00   49
  8  ω     -9.00  39.00   1.00   30.00    --   17.54  77.00-150.00   48
  9  ω     39.00  90.00   1.00   30.00    --   17.54 178.00-120.00   51
 10  ω     -9.00  39.00   1.00   30.00    --   17.54  77.00 -60.00   48
 11  ω      1.00  85.00   1.00   30.00    --   17.54  57.00 120.00   84
 12  ω     -9.00  39.00   1.00   30.00    --   17.54  77.00  30.00   48
 13  ω    -52.00  36.00   1.00   30.00    --   17.54 -38.00 -30.00   88
 14  ω    -85.00   3.00   1.00   30.00    --  -15.82 -38.00-150.00   88
 15  ω     -9.00  39.00   1.00   30.00    --   17.54  77.00  90.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0043671000
_diffrn_orient_matrix_UB_12      0.0156942000
_diffrn_orient_matrix_UB_13      -0.0293055000
_diffrn_orient_matrix_UB_21      -0.0044812000
_diffrn_orient_matrix_UB_22      0.0418459000
_diffrn_orient_matrix_UB_23      0.0053944000
_diffrn_orient_matrix_UB_31      0.0586915000
_diffrn_orient_matrix_UB_32      -0.0006863000
_diffrn_orient_matrix_UB_33      -0.0010690000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                15700
_reflns_number_total             19017
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         4.139
_refine_diff_density_min         -2.022
_refine_diff_density_rms         0.197
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1049
_refine_ls_number_reflns         19017
_refine_ls_number_restraints     1233
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0625
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0349P)²+76.4691P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1459
_refine_special_details          Twin
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C88-C89 = C89-C90 = C90-C91 = C91-C92 = C92-C93
 1.52 with sigma of 0.02
 C89-C91 = C90-C92
 2.54 with sigma of 0.04
 C88-C90 = C91-C93
 2.53 with sigma of 0.04
 C88-C89 \\sim C89-C90 \\sim C90-C91 \\sim C91-C92 \\sim C92-C93
 with sigma of 0.02
 C88-C90 \\sim C90-C92 \\sim C89-C91 \\sim C91-C93
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C88 \\sim C89 \\sim C90 \\sim C91 \\sim C92 \\sim C93: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C17(H17), C9(H9), C45(H45), C31(H31), C67(H67), C56(H56), C20(H20)
5.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C13(H13A,H13B), C50(H50A,H50B), C38(H38A,H38B), C46(H46A,
 H46B), C47(H47A,H47B), C61(H61A,H61B), C10(H10A,H10B), C2(H2A,H2B), C94(H94A,
 H94B), C36(H36A,H36B), C34(H34A,H34B), C22(H22A,H22B), C24(H24A,H24B),
 C23(H23A,H23B), C21(H21A,H21B), C72(H72A,H72B), C25(H25A,H25B), C32(H32A,H32B),
  C35(H35A,H35B), C12(H12A,H12B), C70(H70A,H70B), C48(H48A,H48B), C58(H58A,
 H58B), C49(H49A,H49B), C57(H57A,H57B), C59(H59A,H59B), C68(H68A,H68B),
 C69(H69A,H69B), C33(H33A,H33B), C71(H71A,H71B), C60(H60A,H60B), C89(H89A,H89B),
  C90(H90A,H90B), C91(H91A,H91B), C92(H92A,H92B)
5.c Aromatic/amide H refined with riding coordinates:
 C53(H53), C73(H73), C55(H55), C8(H8), C44(H44), C52(H52), C66(H66), C16(H16),
 C76(H76), C81(H81), C77(H77), C42(H42), C84(H84), C75(H75), C64(H64), C41(H41),
  C85(H85), C74(H74), C83(H83), C5(H5), C19(H19), C87(H87), C6(H6), C30(H30),
 C80(H80), C82(H82), C78(H78), C86(H86), C63(H63), C79(H79), C28(H28), C27(H27)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C37(H37A,H37B,H37C), C88(H88A,H88B,H88C), C93(H93A,H93B,H93C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
U2 U 0.87663(2) 0.64420(2) 0.75323(2) 0.01659(9) Uani 1 1 d . . . . .
U1 U 0.69167(2) 0.59079(2) 0.66204(2) 0.01619(9) Uani 1 1 d . . . . .
Y2 Y 0.82117(6) 0.82329(5) 0.65650(3) 0.01717(17) Uani 1 1 d . . . . .
Y1 Y 0.62846(6) 0.49878(5) 0.80175(3) 0.01758(17) Uani 1 1 d . . . . .
O3 O 0.7727(4) 0.5464(4) 0.7425(2) 0.0174(12) Uani 1 1 d . . . . .
O2 O 0.8058(5) 0.6863(3) 0.6717(2) 0.0175(12) Uani 1 1 d . . . . .
O4 O 0.5653(4) 0.5472(4) 0.7214(2) 0.0195(12) Uani 1 1 d . . . . .
N8 N 0.8175(5) 0.4638(4) 0.6364(3) 0.0196(14) Uani 1 1 d . . . . .
N2 N 1.0643(5) 0.6268(4) 0.6913(3) 0.0177(14) Uani 1 1 d . . . . .
N13 N 0.5605(6) 0.4997(5) 0.6095(3) 0.0219(15) Uani 1 1 d . . . . .
N3 N 0.7342(6) 0.5607(5) 0.8606(3) 0.0204(14) Uani 1 1 d . . . . .
N1 N 1.0117(6) 0.5296(5) 0.7953(3) 0.0208(15) Uani 1 1 d . . . . .
N7 N 0.7791(5) 0.6122(4) 0.5604(3) 0.0175(13) Uani 1 1 d . . . . .
N9 N 0.6616(5) 0.8040(4) 0.6108(3) 0.0176(13) Uani 1 1 d . . . . .
N5 N 0.7585(6) 0.3934(5) 0.8443(3) 0.0231(15) Uani 1 1 d . . . . .
N4 N 0.5266(6) 0.6360(5) 0.8314(3) 0.0232(15) Uani 1 1 d . . . . .
C17 C 0.7967(7) 0.6872(6) 0.8698(4) 0.0249(18) Uani 1 1 d . . . . .
H17 H 0.792040 0.744514 0.880195 0.030 Uiso 1 1 calc R U . . .
N15 N 0.7677(5) 0.9812(4) 0.6150(3) 0.0216(15) Uani 1 1 d . . . . .
N12 N 1.0066(6) 0.8845(4) 0.6287(3) 0.0213(14) Uani 1 1 d . . . . .
N10 N 0.6393(6) 0.8586(5) 0.7150(3) 0.0226(15) Uani 1 1 d . . . . .
N6 N 0.5838(6) 0.3567(5) 0.7893(3) 0.0246(15) Uani 1 1 d . . . . .
C9 C 1.0917(6) 0.6727(5) 0.6335(3) 0.0175(16) Uani 1 1 d . . . . .
H9 H 1.044672 0.726701 0.629874 0.021 Uiso 1 1 calc R U . . .
C43 C 0.8364(6) 0.5422(5) 0.5438(4) 0.0173(15) Uani 1 1 d . . . . .
N16 N 0.8770(5) 0.8290(4) 0.5587(3) 0.0169(13) Uani 1 1 d . . . . .
C18 C 0.7081(7) 0.6462(6) 0.8573(4) 0.0236(17) Uani 1 1 d . . . . .
C15 C 0.8393(7) 0.5476(6) 0.8759(4) 0.0226(17) Uani 1 1 d . . . . .
C53 C 0.5034(7) 0.7322(6) 0.6342(4) 0.0220(18) Uani 1 1 d . . . . .
H53 H 0.435705 0.711240 0.653983 0.026 Uiso 1 1 calc R U . . .
C40 C 0.7803(6) 0.6725(5) 0.5133(3) 0.0160(15) Uani 1 1 d . . . . .
C45 C 0.8530(7) 0.3890(5) 0.6759(4) 0.0208(17) Uani 1 1 d . . . . .
H45 H 0.797866 0.384144 0.710574 0.025 Uiso 1 1 calc R U . . .
C14 C 1.0577(7) 0.6214(6) 0.5924(4) 0.0195(17) Uani 1 1 d . . . . .
H14A H 1.099041 0.565690 0.597104 0.023 Uiso 1 1 calc R U . . .
H14B H 0.977313 0.611916 0.601540 0.023 Uiso 1 1 calc R U . . .
C73 C 0.4507(7) 0.5115(6) 0.6232(4) 0.0250(19) Uani 1 1 d . . . . .
H73 H 0.424880 0.544234 0.651504 0.030 Uiso 1 1 calc R U . . .
N14 N 0.5033(6) 0.4454(5) 0.8911(3) 0.0266(16) Uani 1 1 d . . . . .
C55 C 0.5596(7) 0.8214(6) 0.7009(4) 0.0229(17) Uani 1 1 d . . . . .
H55 H 0.491349 0.817033 0.725070 0.028 Uiso 1 1 calc R U . . .
C4 C 1.0096(7) 0.4703(6) 0.8422(4) 0.0231(17) Uani 1 1 d . . . . .
C8 C 1.1365(7) 0.5697(5) 0.7117(4) 0.0197(16) Uani 1 1 d . . . . .
H8 H 1.206319 0.561854 0.689942 0.024 Uiso 1 1 calc R U . . .
C44 C 0.8566(6) 0.4699(5) 0.5841(4) 0.0187(16) Uani 1 1 d . . . . .
H44 H 0.900852 0.423751 0.572169 0.022 Uiso 1 1 calc R U . . .
C52 C 0.5559(6) 0.7144(6) 0.5824(4) 0.0209(17) Uani 1 1 d . . . . .
H52 H 0.531647 0.677967 0.560645 0.025 Uiso 1 1 calc R U . . .
C13 C 1.0800(7) 0.6645(6) 0.5318(4) 0.0227(18) Uani 1 1 d . . . . .
H13A H 1.034359 0.718296 0.525940 0.027 Uiso 1 1 calc R U . . .
H13B H 1.058827 0.628184 0.506809 0.027 Uiso 1 1 calc R U . . .
C7 C 1.1147(7) 0.5194(6) 0.7647(4) 0.0226(17) Uani 1 1 d . . . . .
C54 C 0.5703(7) 0.7867(6) 0.6508(4) 0.0216(17) Uani 1 1 d . . . . .
C66 C 1.0332(7) 0.9020(5) 0.5748(4) 0.0206(16) Uani 1 1 d . . . . .
H66 H 1.097168 0.932677 0.560043 0.025 Uiso 1 1 calc R U . . .
C16 C 0.8787(7) 0.6236(6) 0.8820(4) 0.0276(19) Uani 1 1 d . . . . .
H16 H 0.949269 0.630685 0.892564 0.033 Uiso 1 1 calc R U . . .
C76 C 0.5216(8) 0.4121(7) 0.5455(4) 0.030(2) Uani 1 1 d . . . . .
H76 H 0.549010 0.376224 0.519353 0.036 Uiso 1 1 calc R U . . .
C50 C 0.9662(7) 0.4002(6) 0.6932(4) 0.027(2) Uani 1 1 d . . . . .
H50A H 0.963211 0.452838 0.708737 0.033 Uiso 1 1 calc R U . . .
H50B H 1.023149 0.404710 0.659832 0.033 Uiso 1 1 calc R U . . .
C31 C 0.4983(8) 0.3315(6) 0.7586(4) 0.030(2) Uani 1 1 d . . . . .
H31 H 0.454253 0.384066 0.744044 0.037 Uiso 1 1 calc R U . . .
C81 C 0.3245(9) 0.4097(8) 0.9402(5) 0.040(3) Uani 1 1 d . . . . .
H81 H 0.248020 0.403533 0.938529 0.049 Uiso 1 1 calc R U . . .
C77 C 0.5935(7) 0.4496(6) 0.5714(4) 0.0255(19) Uani 1 1 d . . . . .
H77 H 0.671180 0.439256 0.561590 0.031 Uiso 1 1 calc R U . . .
C42 C 0.8719(7) 0.5584(6) 0.4858(4) 0.0201(16) Uani 1 1 d . . . . .
H42 H 0.912096 0.520058 0.464158 0.024 Uiso 1 1 calc R U . . .
C67 C 1.0817(7) 0.9047(6) 0.6665(4) 0.0231(18) Uani 1 1 d . . . . .
H67 H 1.099752 0.851120 0.692287 0.028 Uiso 1 1 calc R U . . .
C84 C 0.6784(8) 1.0711(6) 0.5415(4) 0.031(2) Uani 1 1 d . . . . .
H84 H 0.651461 1.077634 0.506085 0.037 Uiso 1 1 calc R U . . .
C65 C 0.9685(6) 0.8760(5) 0.5371(4) 0.0192(16) Uani 1 1 d . . . . .
C75 C 0.4088(7) 0.4283(6) 0.5587(4) 0.028(2) Uani 1 1 d . . . . .
H75 H 0.356973 0.405224 0.540682 0.034 Uiso 1 1 calc R U . . .
C64 C 0.9831(7) 0.8894(6) 0.4788(4) 0.0228(17) Uani 1 1 d . . . . .
H64 H 1.040464 0.918742 0.454490 0.027 Uiso 1 1 calc R U . . .
C41 C 0.8369(6) 0.6414(5) 0.4662(4) 0.0190(16) Uani 1 1 d . . . . .
H41 H 0.848657 0.671099 0.428692 0.023 Uiso 1 1 calc R U . . .
C38 C 0.6689(7) 0.7943(6) 0.4655(4) 0.0237(18) Uani 1 1 d . . . . .
H38A H 0.720099 0.791531 0.430611 0.028 Uiso 1 1 calc R U . . .
H38B H 0.608974 0.755934 0.466651 0.028 Uiso 1 1 calc R U . . .
C85 C 0.6684(8) 1.1370(6) 0.5702(4) 0.0298(19) Uani 1 1 d . . . . .
H85 H 0.633438 1.189540 0.555412 0.036 Uiso 1 1 calc R U . . .
C74 C 0.3724(7) 0.4781(6) 0.5982(4) 0.029(2) Uani 1 1 d . . . . .
H74 H 0.295031 0.489613 0.608210 0.034 Uiso 1 1 calc R U . . .
C83 C 0.7282(7) 0.9950(6) 0.5646(4) 0.0289(19) Uani 1 1 d . . . . .
H83 H 0.734967 0.949989 0.544014 0.035 Uiso 1 1 calc R U . . .
C3 C 0.9036(7) 0.4619(6) 0.8842(4) 0.0265(17) Uani 1 1 d . . . . .
C46 C 0.8577(8) 0.3059(6) 0.6537(4) 0.029(2) Uani 1 1 d . . . . .
H46A H 0.784357 0.298241 0.642552 0.034 Uiso 1 1 calc R U . . .
H46B H 0.913577 0.307985 0.620040 0.034 Uiso 1 1 calc R U . . .
C51 C 0.6520(6) 0.7613(5) 0.5691(3) 0.0152(15) Uani 1 1 d . . . . .
C29 C 0.7353(8) 0.3118(6) 0.8433(4) 0.031(2) Uani 1 1 d . . . . .
C39 C 0.7336(7) 0.7618(5) 0.5162(4) 0.0183(15) Uani 1 1 d . . . . .
C5 C 1.1109(7) 0.4204(7) 0.8429(4) 0.034(2) Uani 1 1 d . . . . .
H5 H 1.129770 0.374286 0.870982 0.041 Uiso 1 1 calc R U . . .
C56 C 0.6120(8) 0.8964(6) 0.7660(4) 0.0274(19) Uani 1 1 d . . . . .
H56 H 0.571811 0.854130 0.795419 0.033 Uiso 1 1 calc R U . . .
C47 C 0.8885(9) 0.2313(6) 0.6987(5) 0.038(2) Uani 1 1 d . . . . .
H47A H 0.831324 0.227799 0.731909 0.045 Uiso 1 1 calc R U . . .
H47B H 0.890872 0.178174 0.683677 0.045 Uiso 1 1 calc R U . . .
C26 C 0.8453(7) 0.3877(6) 0.8751(4) 0.029(2) Uani 1 1 d . . . . .
C19 C 0.5989(7) 0.6792(6) 0.8458(4) 0.0236(18) Uani 1 1 d . . . . .
H19 H 0.578548 0.736249 0.849062 0.028 Uiso 1 1 calc R U . . .
C61 C 0.7164(9) 0.9140(7) 0.7884(5) 0.038(2) Uani 1 1 d . . . . .
H61A H 0.762510 0.860706 0.796238 0.045 Uiso 1 1 calc R U . . .
H61B H 0.760037 0.953305 0.759220 0.045 Uiso 1 1 calc R U . . .
C10 C 1.2130(7) 0.6953(6) 0.6172(4) 0.0209(17) Uani 1 1 d . . . . .
H10A H 1.230636 0.734073 0.641394 0.025 Uiso 1 1 calc R U . . .
H10B H 1.262101 0.643411 0.624289 0.025 Uiso 1 1 calc R U . . .
C2 C 0.9384(8) 0.4438(7) 0.9447(4) 0.031(2) Uani 1 1 d . . . . .
H2A H 0.989314 0.392594 0.948580 0.037 Uiso 1 1 calc R U . . .
H2B H 0.979874 0.491433 0.949841 0.037 Uiso 1 1 calc R U . . .
C87 C 0.7601(7) 1.0480(6) 0.6404(4) 0.0270(19) Uani 1 1 d . . . . .
H87 H 0.791713 1.041346 0.674601 0.032 Uiso 1 1 calc R U . . .
C6 C 1.1772(8) 0.4533(6) 0.7938(4) 0.0278(19) Uani 1 1 d . . . . .
H6 H 1.251352 0.434231 0.782268 0.033 Uiso 1 1 calc R U . . .
C94 C 1.2372(7) 0.7363(6) 0.5564(4) 0.0225(18) Uani 1 1 d . . . . .
H94A H 1.317682 0.745436 0.547522 0.027 Uiso 1 1 calc R U . . .
H94B H 1.195899 0.791936 0.550338 0.027 Uiso 1 1 calc R U . . .
C30 C 0.6469(8) 0.2969(6) 0.8145(4) 0.030(2) Uani 1 1 d . . . . .
H30 H 0.633165 0.240221 0.813524 0.036 Uiso 1 1 calc R U . . .
C36 C 0.5491(9) 0.2934(7) 0.7083(4) 0.035(2) Uani 1 1 d . . . . .
H36A H 0.596235 0.242438 0.721144 0.042 Uiso 1 1 calc R U . . .
H36B H 0.597630 0.334248 0.683088 0.042 Uiso 1 1 calc R U . . .
C34 C 0.3826(10) 0.2109(7) 0.7129(6) 0.052(3) Uani 1 1 d . . . . .
H34A H 0.423162 0.156729 0.725909 0.063 Uiso 1 1 calc R U . . .
H34B H 0.323803 0.199410 0.691340 0.063 Uiso 1 1 calc R U . . .
C22 C 0.2342(8) 0.7247(8) 0.8776(5) 0.042(3) Uani 1 1 d . . . . .
H22A H 0.186113 0.714834 0.914113 0.050 Uiso 1 1 calc R U . . .
H22B H 0.248293 0.785366 0.868470 0.050 Uiso 1 1 calc R U . . .
C20 C 0.4172(7) 0.6825(6) 0.8264(4) 0.0240(18) Uani 1 1 d . . . . .
H20 H 0.430591 0.743606 0.813511 0.029 Uiso 1 1 calc R U . . .
C80 C 0.3678(10) 0.3911(9) 0.9907(5) 0.050(3) Uani 1 1 d . . . . .
H80 H 0.321819 0.372553 1.024694 0.060 Uiso 1 1 calc R U . . .
C82 C 0.3940(8) 0.4374(6) 0.8924(4) 0.029(2) Uani 1 1 d . . . . .
H82 H 0.362796 0.451915 0.857931 0.035 Uiso 1 1 calc R U . . .
C24 C 0.2474(8) 0.7085(7) 0.7775(4) 0.032(2) Uani 1 1 d . . . . .
H24A H 0.264945 0.767943 0.763280 0.038 Uiso 1 1 calc R U . . .
H24B H 0.206995 0.689820 0.749729 0.038 Uiso 1 1 calc R U . . .
C62 C 0.8331(7) 0.8148(5) 0.5127(4) 0.0193(16) Uani 1 1 d . . . . .
C23 C 0.1742(8) 0.7025(7) 0.8332(5) 0.040(2) Uani 1 1 d . . . . .
H23A H 0.107174 0.741149 0.828613 0.047 Uiso 1 1 calc R U . . .
H23B H 0.149595 0.644419 0.845110 0.047 Uiso 1 1 calc R U . . .
C21 C 0.3444(8) 0.6735(7) 0.8834(4) 0.034(2) Uani 1 1 d . . . . .
H21A H 0.330301 0.613453 0.897367 0.041 Uiso 1 1 calc R U . . .
H21B H 0.383748 0.693590 0.911005 0.041 Uiso 1 1 calc R U . . .
C78 C 0.5428(9) 0.4267(9) 0.9400(5) 0.049(3) Uani 1 1 d . . . . .
H78 H 0.619929 0.431890 0.940594 0.059 Uiso 1 1 calc R U . . .
C86 C 0.7106(8) 1.1254(6) 0.6215(4) 0.032(2) Uani 1 1 d . . . . .
H86 H 0.705287 1.169543 0.642766 0.038 Uiso 1 1 calc R U . . .
C72 C 1.0185(8) 0.9651(7) 0.7031(5) 0.035(2) Uani 1 1 d . . . . .
H72A H 0.948603 0.940312 0.722225 0.041 Uiso 1 1 calc R U . . .
H72B H 0.998551 1.018904 0.678816 0.041 Uiso 1 1 calc R U . . .
C25 C 0.3551(8) 0.6542(6) 0.7835(4) 0.029(2) Uani 1 1 d . . . . .
H25A H 0.402183 0.659488 0.746753 0.035 Uiso 1 1 calc R U . . .
H25B H 0.338146 0.594374 0.795943 0.035 Uiso 1 1 calc R U . . .
C32 C 0.4165(8) 0.2730(7) 0.7969(5) 0.039(2) Uani 1 1 d . . . . .
H32A H 0.378754 0.301579 0.827518 0.047 Uiso 1 1 calc R U . . .
H32B H 0.457624 0.221434 0.814173 0.047 Uiso 1 1 calc R U . . .
C1 C 0.8396(9) 0.4313(8) 0.9911(4) 0.044(3) Uani 1 1 d . . . . .
H1A H 0.801758 0.381397 0.988267 0.067 Uiso 1 1 calc R U . . .
H1B H 0.787459 0.481004 0.986820 0.067 Uiso 1 1 calc R U . . .
H1C H 0.866623 0.423568 1.027934 0.067 Uiso 1 1 calc R U . . .
C63 C 0.8968(7) 0.8513(5) 0.4630(4) 0.0217(17) Uani 1 1 d . . . . .
H63 H 0.883471 0.850048 0.425660 0.026 Uiso 1 1 calc R U . . .
C35 C 0.4620(10) 0.2694(7) 0.6751(5) 0.047(3) Uani 1 1 d . . . . .
H35A H 0.420151 0.320954 0.658396 0.057 Uiso 1 1 calc R U . . .
H35B H 0.499593 0.241521 0.644180 0.057 Uiso 1 1 calc R U . . .
C12 C 1.2037(7) 0.6816(6) 0.5169(4) 0.0251(19) Uani 1 1 d . . . . .
H12A H 1.217484 0.711013 0.477455 0.030 Uiso 1 1 calc R U . . .
H12B H 1.249126 0.627609 0.520564 0.030 Uiso 1 1 calc R U . . .
C79 C 0.4780(10) 0.4000(10) 0.9906(5) 0.059(4) Uani 1 1 d . . . . .
H79 H 0.510368 0.388087 1.024739 0.071 Uiso 1 1 calc R U . . .
C37 C 0.6172(8) 0.8839(6) 0.4627(4) 0.030(2) Uani 1 1 d . . . . .
H37A H 0.572788 0.897613 0.431168 0.045 Uiso 1 1 calc R U . . .
H37B H 0.676257 0.923406 0.457262 0.045 Uiso 1 1 calc R U . . .
H37C H 0.569216 0.888393 0.497853 0.045 Uiso 1 1 calc R U . . .
C70 C 1.1990(10) 1.0170(7) 0.7190(6) 0.048(3) Uani 1 1 d . . . . .
H70A H 1.184819 1.072495 0.695300 0.058 Uiso 1 1 calc R U . . .
H70B H 1.244710 1.025246 0.748060 0.058 Uiso 1 1 calc R U . . .
C48 C 1.0015(9) 0.2423(7) 0.7158(5) 0.040(3) Uani 1 1 d . . . . .
H48A H 1.020545 0.194602 0.745467 0.049 Uiso 1 1 calc R U . . .
H48B H 1.059382 0.242547 0.683054 0.049 Uiso 1 1 calc R U . . .
C58 C 0.5062(10) 1.0111(7) 0.8114(5) 0.047(3) Uani 1 1 d . . . . .
H58A H 0.464112 0.969832 0.839930 0.056 Uiso 1 1 calc R U . . .
H58B H 0.458712 1.063848 0.804776 0.056 Uiso 1 1 calc R U . . .
C28 C 0.8075(10) 0.2545(7) 0.8730(5) 0.047(3) Uani 1 1 d . . . . .
H28 H 0.809326 0.194809 0.878060 0.057 Uiso 1 1 calc R U . . .
C27 C 0.8760(10) 0.3029(7) 0.8935(5) 0.044(3) Uani 1 1 d . . . . .
H27 H 0.933630 0.282047 0.916114 0.053 Uiso 1 1 calc R U . . .
C49 C 0.9984(9) 0.3247(7) 0.7376(5) 0.039(2) Uani 1 1 d . . . . .
H49A H 1.072505 0.332071 0.748070 0.047 Uiso 1 1 calc R U . . .
H49B H 0.943856 0.322546 0.771836 0.047 Uiso 1 1 calc R U . . .
C57 C 0.5343(9) 0.9765(7) 0.7571(4) 0.035(2) Uani 1 1 d . . . . .
H57A H 0.571058 1.019598 0.727667 0.043 Uiso 1 1 calc R U . . .
H57B H 0.465048 0.963347 0.744141 0.043 Uiso 1 1 calc R U . . .
C59 C 0.6124(11) 1.0285(9) 0.8333(6) 0.059(3) Uani 1 1 d . . . . .
H59A H 0.650110 1.074122 0.806473 0.070 Uiso 1 1 calc R U . . .
H59B H 0.592698 1.048112 0.869732 0.070 Uiso 1 1 calc R U . . .
C68 C 1.1914(7) 0.9402(6) 0.6392(4) 0.031(2) Uani 1 1 d . . . . .
H68A H 1.176671 0.993265 0.612957 0.037 Uiso 1 1 calc R U . . .
H68B H 1.233423 0.899694 0.617099 0.037 Uiso 1 1 calc R U . . .
C69 C 1.2622(8) 0.9576(7) 0.6831(5) 0.038(2) Uani 1 1 d . . . . .
H69A H 1.282568 0.903904 0.707323 0.045 Uiso 1 1 calc R U . . .
H69B H 1.331678 0.982745 0.663755 0.045 Uiso 1 1 calc R U . . .
C33 C 0.3291(10) 0.2487(9) 0.7635(6) 0.059(3) Uani 1 1 d . . . . .
H33A H 0.280907 0.207358 0.788506 0.070 Uiso 1 1 calc R U . . .
H33B H 0.281586 0.299410 0.750639 0.070 Uiso 1 1 calc R U . . .
C71 C 1.0886(10) 0.9825(8) 0.7475(5) 0.047(3) Uani 1 1 d . . . . .
H71A H 1.047095 1.023861 0.769104 0.056 Uiso 1 1 calc R U . . .
H71B H 1.102714 0.929750 0.774082 0.056 Uiso 1 1 calc R U . . .
C60 C 0.6915(12) 0.9513(9) 0.8411(6) 0.057(4) Uani 1 1 d . . . . .
H60A H 0.761790 0.966730 0.851855 0.069 Uiso 1 1 calc R U . . .
H60B H 0.658339 0.908666 0.872055 0.069 Uiso 1 1 calc R U . . .
O1 O 0.8902(5) 0.7698(4) 0.7371(2) 0.0211(12) Uani 1 1 d . . . . .
C88 C 1.106(3) 1.1079(17) 0.8745(10) 0.198(13) Uani 1 1 d D U . . .
H88A H 1.098531 1.127802 0.834596 0.298 Uiso 1 1 calc R U . . .
H88B H 1.175834 1.074007 0.878184 0.298 Uiso 1 1 calc R U . . .
H88C H 1.105028 1.156451 0.893431 0.298 Uiso 1 1 calc R U . . .
C89 C 1.009(2) 1.0547(14) 0.9012(13) 0.195(12) Uani 1 1 d D U . . .
H89A H 0.974230 1.076200 0.935338 0.234 Uiso 1 1 calc R U . . .
H89B H 0.952864 1.061831 0.874662 0.234 Uiso 1 1 calc R U . . .
C90 C 1.040(2) 0.9617(13) 0.9174(12) 0.188(10) Uani 1 1 d D U . . .
H90A H 1.101454 0.954403 0.941027 0.226 Uiso 1 1 calc R U . . .
H90B H 1.067560 0.938456 0.882863 0.226 Uiso 1 1 calc R U . . .
C91 C 0.943(2) 0.9119(14) 0.9491(13) 0.200(11) Uani 1 1 d D U . . .
H91A H 0.927557 0.926887 0.987119 0.240 Uiso 1 1 calc R U . . .
H91B H 0.876916 0.930379 0.929643 0.240 Uiso 1 1 calc R U . . .
C92 C 0.959(3) 0.8176(14) 0.9557(13) 0.195(12) Uani 1 1 d D U . . .
H92A H 1.033091 0.799734 0.967938 0.235 Uiso 1 1 calc R U . . .
H92B H 0.958710 0.801445 0.918469 0.235 Uiso 1 1 calc R U . . .
C93 C 0.872(2) 0.7697(16) 0.9971(11) 0.171(12) Uani 1 1 d D U . . .
H93A H 0.801693 0.775020 0.980749 0.256 Uiso 1 1 calc R U . . .
H93B H 0.860491 0.793088 1.031894 0.256 Uiso 1 1 calc R U . . .
H93C H 0.897180 0.710098 1.005367 0.256 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U2 O3 2.177(6) . ?
U2 O2 2.242(6) . ?
U2 N2 2.584(6) . ?
U2 N1 2.535(7) . ?
U2 C17 3.063(9) . ?
U2 C18 3.042(9) . ?
U2 O1 2.013(6) . ?
U1 O3 2.285(6) . ?
U1 O2 2.223(5) . ?
U1 O4 2.038(6) . ?
U1 N8 2.576(7) . ?
U1 N13 2.826(7) . ?
U1 N7 2.536(7) . ?
U1 C52 3.061(9) . ?
Y2 O2 2.198(6) . ?
Y2 N9 2.432(7) . ?
Y2 N15 2.630(7) . ?
Y2 N12 2.496(7) . ?
Y2 N10 2.546(7) . ?
Y2 N16 2.376(7) . ?
Y2 O1 2.240(6) . ?
Y1 O3 2.210(5) . ?
Y1 O4 2.187(6) . ?
Y1 N3 2.440(7) . ?
Y1 N5 2.412(7) . ?
Y1 N4 2.621(8) . ?
Y1 N6 2.485(8) . ?
Y1 N14 2.538(7) . ?
N8 C45 1.476(11) . ?
N8 C44 1.289(11) . ?
N2 C9 1.476(11) . ?
N2 C8 1.297(11) . ?
N13 C73 1.338(11) . ?
N13 C77 1.345(11) . ?
N3 C18 1.383(12) . ?
N3 C15 1.367(11) . ?
N1 C4 1.349(11) . ?
N1 C7 1.382(11) . ?
N7 C43 1.376(10) . ?
N7 C40 1.360(11) . ?
N9 C54 1.385(11) . ?
N9 C51 1.350(11) . ?
N5 C29 1.378(12) . ?
N5 C26 1.363(11) . ?
N4 C19 1.289(11) . ?
N4 C20 1.480(11) . ?
C17 H17 1.0000 . ?
C17 C18 1.406(12) . ?
C17 C16 1.390(14) . ?
N15 C83 1.353(12) . ?
N15 C87 1.331(12) . ?
N12 C66 1.296(12) . ?
N12 C67 1.475(11) . ?
N10 C55 1.296(11) . ?
N10 C56 1.473(12) . ?
N6 C31 1.483(12) . ?
N6 C30 1.298(12) . ?
C9 H9 1.0000 . ?
C9 C14 1.530(11) . ?
C9 C10 1.530(11) . ?
C43 C44 1.409(12) . ?
C43 C42 1.403(12) . ?
N16 C65 1.388(10) . ?
N16 C62 1.369(11) . ?
C18 C19 1.432(12) . ?
C15 C16 1.396(13) . ?
C15 C3 1.526(13) . ?
C53 H53 0.9500 . ?
C53 C52 1.403(12) . ?
C53 C54 1.395(12) . ?
C40 C41 1.410(11) . ?
C40 C39 1.518(12) . ?
C45 H45 1.0000 . ?
C45 C50 1.525(11) . ?
C45 C46 1.533(12) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C13 1.512(12) . ?
C73 H73 0.9500 . ?
C73 C74 1.391(12) . ?
N14 C82 1.340(11) . ?
N14 C78 1.319(13) . ?
C55 H55 0.9500 . ?
C55 C54 1.422(13) . ?
C4 C3 1.532(12) . ?
C4 C5 1.415(13) . ?
C8 H8 0.9500 . ?
C8 C7 1.400(13) . ?
C44 H44 0.9500 . ?
C52 H52 0.9500 . ?
C52 C51 1.415(11) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C12 1.534(11) . ?
C7 C6 1.398(13) . ?
C66 H66 0.9500 . ?
C66 C65 1.426(12) . ?
C16 H16 0.9500 . ?
C76 H76 0.9500 . ?
C76 C77 1.381(12) . ?
C76 C75 1.379(12) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C50 C49 1.539(14) . ?
C31 H31 1.0000 . ?
C31 C36 1.509(14) . ?
C31 C32 1.528(14) . ?
C81 H81 0.9500 . ?
C81 C80 1.376(16) . ?
C81 C82 1.371(13) . ?
C77 H77 0.9500 . ?
C42 H42 0.9500 . ?
C42 C41 1.391(12) . ?
C67 H67 1.0000 . ?
C67 C72 1.533(13) . ?
C67 C68 1.516(12) . ?
C84 H84 0.9500 . ?
C84 C85 1.367(14) . ?
C84 C83 1.382(13) . ?
C65 C64 1.387(13) . ?
C75 H75 0.9500 . ?
C75 C74 1.372(14) . ?
C64 H64 0.9500 . ?
C64 C63 1.389(12) . ?
C41 H41 0.9500 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.541(12) . ?
C38 C37 1.525(13) . ?
C85 H85 0.9500 . ?
C85 C86 1.391(14) . ?
C74 H74 0.9500 . ?
C83 H83 0.9500 . ?
C3 C26 1.509(13) . ?
C3 C2 1.557(13) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C47 1.532(13) . ?
C51 C39 1.518(11) . ?
C29 C30 1.421(13) . ?
C29 C28 1.392(14) . ?
C39 C62 1.524(11) . ?
C5 H5 0.9500 . ?
C5 C6 1.394(13) . ?
C56 H56 1.0000 . ?
C56 C61 1.513(14) . ?
C56 C57 1.538(13) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.522(15) . ?
C26 C27 1.399(14) . ?
C19 H19 0.9500 . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 C60 1.504(15) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C94 1.508(12) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.534(13) . ?
C87 H87 0.9500 . ?
C87 C86 1.370(13) . ?
C6 H6 0.9500 . ?
C94 H94A 0.9900 . ?
C94 H94B 0.9900 . ?
C94 C12 1.536(12) . ?
C30 H30 0.9500 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C35 1.529(14) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.505(18) . ?
C34 C33 1.522(19) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.495(16) . ?
C22 C21 1.523(14) . ?
C20 H20 1.0000 . ?
C20 C21 1.533(13) . ?
C20 C25 1.524(13) . ?
C80 H80 0.9500 . ?
C80 C79 1.358(16) . ?
C82 H82 0.9500 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C23 1.512(14) . ?
C24 C25 1.522(13) . ?
C62 C63 1.406(12) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C78 H78 0.9500 . ?
C78 C79 1.388(15) . ?
C86 H86 0.9500 . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C72 C71 1.544(14) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.538(15) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C63 H63 0.9500 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C79 H79 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C70 C69 1.512(16) . ?
C70 C71 1.524(16) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.520(15) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C58 C57 1.518(15) . ?
C58 C59 1.527(18) . ?
C28 H28 0.9500 . ?
C28 C27 1.387(15) . ?
C27 H27 0.9500 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 C60 1.510(17) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C68 C69 1.538(13) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
C88 C89 1.515(13) . ?
C89 H89A 0.9900 . ?
C89 H89B 0.9900 . ?
C89 C90 1.512(13) . ?
C90 H90A 0.9900 . ?
C90 H90B 0.9900 . ?
C90 C91 1.519(13) . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C91 C92 1.503(13) . ?
C92 H92A 0.9900 . ?
C92 H92B 0.9900 . ?
C92 C93 1.516(13) . ?
C93 H93A 0.9800 . ?
C93 H93B 0.9800 . ?
C93 H93C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 U2 O2 72.2(2) . . ?
O3 U2 N2 107.4(2) . . ?
O3 U2 N1 88.7(2) . . ?
O3 U2 C17 106.3(2) . . ?
O3 U2 C18 81.0(2) . . ?
O2 U2 N2 85.3(2) . . ?
O2 U2 N1 138.2(2) . . ?
O2 U2 C17 130.1(2) . . ?
O2 U2 C18 114.4(2) . . ?
N2 U2 C17 137.3(2) . . ?
N2 U2 C18 160.2(2) . . ?
N1 U2 N2 65.0(2) . . ?
N1 U2 C17 90.5(2) . . ?
N1 U2 C18 98.0(2) . . ?
C18 U2 C17 26.6(2) . . ?
O1 U2 O3 142.5(2) . . ?
O1 U2 O2 76.0(2) . . ?
O1 U2 N2 89.1(2) . . ?
O1 U2 N1 128.7(2) . . ?
O1 U2 C17 79.6(2) . . ?
O1 U2 C18 94.7(2) . . ?
O3 U1 N8 78.7(2) . . ?
O3 U1 N13 128.3(2) . . ?
O3 U1 N7 129.7(2) . . ?
O3 U1 C52 154.6(2) . . ?
O2 U1 O3 70.6(2) . . ?
O2 U1 N8 106.0(2) . . ?
O2 U1 N13 159.4(2) . . ?
O2 U1 N7 85.1(2) . . ?
O2 U1 C52 94.4(2) . . ?
O4 U1 O3 75.0(2) . . ?
O4 U1 O2 124.3(2) . . ?
O4 U1 N8 108.5(2) . . ?
O4 U1 N13 73.4(2) . . ?
O4 U1 N7 149.1(2) . . ?
O4 U1 C52 99.0(2) . . ?
N8 U1 N13 74.1(2) . . ?
N8 U1 C52 126.0(2) . . ?
N13 U1 C52 70.7(2) . . ?
N7 U1 N8 66.3(2) . . ?
N7 U1 N13 76.0(2) . . ?
N7 U1 C52 66.3(2) . . ?
O2 Y2 N9 75.1(2) . . ?
O2 Y2 N15 155.3(2) . . ?
O2 Y2 N12 121.0(2) . . ?
O2 Y2 N10 96.3(2) . . ?
O2 Y2 N16 92.9(2) . . ?
O2 Y2 O1 72.5(2) . . ?
N9 Y2 N15 80.2(2) . . ?
N9 Y2 N12 137.4(2) . . ?
N9 Y2 N10 68.8(2) . . ?
N12 Y2 N15 77.4(2) . . ?
N12 Y2 N10 136.8(2) . . ?
N10 Y2 N15 75.4(2) . . ?
N16 Y2 N9 70.6(2) . . ?
N16 Y2 N15 77.8(2) . . ?
N16 Y2 N12 69.5(2) . . ?
N16 Y2 N10 134.2(2) . . ?
O1 Y2 N9 137.3(2) . . ?
O1 Y2 N15 129.2(2) . . ?
O1 Y2 N12 83.9(2) . . ?
O1 Y2 N10 87.9(2) . . ?
O1 Y2 N16 137.4(2) . . ?
O3 Y1 N3 77.0(2) . . ?
O3 Y1 N5 86.3(2) . . ?
O3 Y1 N4 103.3(2) . . ?
O3 Y1 N6 112.0(2) . . ?
O3 Y1 N14 162.6(2) . . ?
O4 Y1 O3 73.7(2) . . ?
O4 Y1 N3 132.9(2) . . ?
O4 Y1 N5 141.5(2) . . ?
O4 Y1 N4 84.0(2) . . ?
O4 Y1 N6 87.0(2) . . ?
O4 Y1 N14 123.0(2) . . ?
N3 Y1 N4 67.9(2) . . ?
N3 Y1 N6 138.6(2) . . ?
N3 Y1 N14 86.8(2) . . ?
N5 Y1 N3 70.3(3) . . ?
N5 Y1 N4 133.4(3) . . ?
N5 Y1 N6 70.2(3) . . ?
N5 Y1 N14 82.2(2) . . ?
N6 Y1 N4 139.4(2) . . ?
N6 Y1 N14 76.2(3) . . ?
N14 Y1 N4 76.0(2) . . ?
U2 O3 U1 108.6(2) . . ?
U2 O3 Y1 125.6(3) . . ?
Y1 O3 U1 101.0(2) . . ?
U1 O2 U2 108.5(2) . . ?
Y2 O2 U2 102.5(2) . . ?
Y2 O2 U1 141.1(3) . . ?
U1 O4 Y1 110.3(2) . . ?
C45 N8 U1 126.3(5) . . ?
C44 N8 U1 115.3(6) . . ?
C44 N8 C45 118.2(7) . . ?
C9 N2 U2 124.8(5) . . ?
C8 N2 U2 117.0(6) . . ?
C8 N2 C9 118.0(7) . . ?
C73 N13 U1 114.7(6) . . ?
C73 N13 C77 116.4(8) . . ?
C77 N13 U1 128.8(5) . . ?
C18 N3 Y1 111.9(5) . . ?
C15 N3 Y1 135.3(6) . . ?
C15 N3 C18 105.6(7) . . ?
C4 N1 U2 136.0(6) . . ?
C4 N1 C7 106.7(7) . . ?
C7 N1 U2 117.4(5) . . ?
C43 N7 U1 114.9(5) . . ?
C40 N7 U1 138.8(5) . . ?
C40 N7 C43 106.0(7) . . ?
C54 N9 Y2 109.7(5) . . ?
C51 N9 Y2 131.4(5) . . ?
C51 N9 C54 106.7(7) . . ?
C29 N5 Y1 114.1(6) . . ?
C26 N5 Y1 139.4(6) . . ?
C26 N5 C29 106.1(8) . . ?
C19 N4 Y1 108.5(6) . . ?
C19 N4 C20 113.2(8) . . ?
C20 N4 Y1 137.2(6) . . ?
U2 C17 H17 126.1 . . ?
C18 C17 U2 75.8(5) . . ?
C18 C17 H17 126.1 . . ?
C16 C17 U2 78.4(5) . . ?
C16 C17 H17 126.1 . . ?
C16 C17 C18 105.0(8) . . ?
C83 N15 Y2 116.1(6) . . ?
C87 N15 Y2 128.1(6) . . ?
C87 N15 C83 115.1(8) . . ?
C66 N12 Y2 113.2(5) . . ?
C66 N12 C67 119.7(7) . . ?
C67 N12 Y2 127.0(6) . . ?
C55 N10 Y2 109.3(6) . . ?
C55 N10 C56 115.8(8) . . ?
C56 N10 Y2 133.6(6) . . ?
C31 N6 Y1 130.3(6) . . ?
C30 N6 Y1 112.6(6) . . ?
C30 N6 C31 117.1(8) . . ?
N2 C9 H9 107.3 . . ?
N2 C9 C14 108.7(7) . . ?
N2 C9 C10 115.7(7) . . ?
C14 C9 H9 107.3 . . ?
C14 C9 C10 110.3(7) . . ?
C10 C9 H9 107.3 . . ?
N7 C43 C44 119.9(8) . . ?
N7 C43 C42 110.3(8) . . ?
C42 C43 C44 129.7(8) . . ?
C65 N16 Y2 114.9(5) . . ?
C62 N16 Y2 138.2(5) . . ?
C62 N16 C65 105.1(7) . . ?
N3 C18 U2 78.8(5) . . ?
N3 C18 C17 111.1(8) . . ?
N3 C18 C19 119.0(8) . . ?
C17 C18 U2 77.5(5) . . ?
C17 C18 C19 129.7(9) . . ?
C19 C18 U2 114.4(6) . . ?
N3 C15 C16 110.1(8) . . ?
N3 C15 C3 124.4(8) . . ?
C16 C15 C3 125.5(8) . . ?
C52 C53 H53 126.9 . . ?
C54 C53 H53 126.9 . . ?
C54 C53 C52 106.3(7) . . ?
N7 C40 C41 111.0(7) . . ?
N7 C40 C39 121.2(7) . . ?
C41 C40 C39 127.6(8) . . ?
N8 C45 H45 107.5 . . ?
N8 C45 C50 110.5(7) . . ?
N8 C45 C46 114.4(7) . . ?
C50 C45 H45 107.5 . . ?
C50 C45 C46 109.2(7) . . ?
C46 C45 H45 107.5 . . ?
C9 C14 H14A 109.0 . . ?
C9 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C13 C14 C9 112.7(7) . . ?
C13 C14 H14A 109.0 . . ?
C13 C14 H14B 109.0 . . ?
N13 C73 H73 118.4 . . ?
N13 C73 C74 123.3(9) . . ?
C74 C73 H73 118.4 . . ?
C82 N14 Y1 123.1(6) . . ?
C78 N14 Y1 120.8(6) . . ?
C78 N14 C82 116.0(8) . . ?
N10 C55 H55 118.7 . . ?
N10 C55 C54 122.6(8) . . ?
C54 C55 H55 118.7 . . ?
N1 C4 C3 119.8(8) . . ?
N1 C4 C5 111.0(8) . . ?
C5 C4 C3 129.2(8) . . ?
N2 C8 H8 119.0 . . ?
N2 C8 C7 122.0(8) . . ?
C7 C8 H8 119.0 . . ?
N8 C44 C43 122.8(8) . . ?
N8 C44 H44 118.6 . . ?
C43 C44 H44 118.6 . . ?
U1 C52 H52 101.6 . . ?
C53 C52 U1 80.4(5) . . ?
C53 C52 H52 126.8 . . ?
C53 C52 C51 106.5(8) . . ?
C51 C52 U1 85.8(5) . . ?
C51 C52 H52 126.8 . . ?
C14 C13 H13A 109.6 . . ?
C14 C13 H13B 109.6 . . ?
C14 C13 C12 110.1(7) . . ?
H13A C13 H13B 108.2 . . ?
C12 C13 H13A 109.6 . . ?
C12 C13 H13B 109.6 . . ?
N1 C7 C8 118.6(8) . . ?
N1 C7 C6 109.4(8) . . ?
C6 C7 C8 131.9(8) . . ?
N9 C54 C53 110.3(8) . . ?
N9 C54 C55 119.5(8) . . ?
C53 C54 C55 130.2(8) . . ?
N12 C66 H66 119.3 . . ?
N12 C66 C65 121.3(8) . . ?
C65 C66 H66 119.3 . . ?
C17 C16 C15 108.2(8) . . ?
C17 C16 H16 125.9 . . ?
C15 C16 H16 125.9 . . ?
C77 C76 H76 120.9 . . ?
C75 C76 H76 120.9 . . ?
C75 C76 C77 118.2(9) . . ?
C45 C50 H50A 109.7 . . ?
C45 C50 H50B 109.7 . . ?
C45 C50 C49 110.0(8) . . ?
H50A C50 H50B 108.2 . . ?
C49 C50 H50A 109.7 . . ?
C49 C50 H50B 109.7 . . ?
N6 C31 H31 106.9 . . ?
N6 C31 C36 112.3(8) . . ?
N6 C31 C32 112.5(8) . . ?
C36 C31 H31 106.9 . . ?
C36 C31 C32 110.9(8) . . ?
C32 C31 H31 106.9 . . ?
C80 C81 H81 120.7 . . ?
C82 C81 H81 120.7 . . ?
C82 C81 C80 118.6(10) . . ?
N13 C77 C76 124.1(8) . . ?
N13 C77 H77 118.0 . . ?
C76 C77 H77 118.0 . . ?
C43 C42 H42 126.6 . . ?
C41 C42 C43 106.8(8) . . ?
C41 C42 H42 126.6 . . ?
N12 C67 H67 107.0 . . ?
N12 C67 C72 108.8(7) . . ?
N12 C67 C68 116.9(8) . . ?
C72 C67 H67 107.0 . . ?
C68 C67 H67 107.0 . . ?
C68 C67 C72 109.7(8) . . ?
C85 C84 H84 120.3 . . ?
C85 C84 C83 119.3(10) . . ?
C83 C84 H84 120.3 . . ?
N16 C65 C66 119.2(8) . . ?
C64 C65 N16 111.2(7) . . ?
C64 C65 C66 129.5(8) . . ?
C76 C75 H75 120.4 . . ?
C74 C75 C76 119.1(8) . . ?
C74 C75 H75 120.4 . . ?
C65 C64 H64 126.9 . . ?
C65 C64 C63 106.2(7) . . ?
C63 C64 H64 126.9 . . ?
C40 C41 H41 127.0 . . ?
C42 C41 C40 106.0(8) . . ?
C42 C41 H41 127.0 . . ?
H38A C38 H38B 107.5 . . ?
C39 C38 H38A 108.5 . . ?
C39 C38 H38B 108.5 . . ?
C37 C38 H38A 108.5 . . ?
C37 C38 H38B 108.5 . . ?
C37 C38 C39 115.1(8) . . ?
C84 C85 H85 120.7 . . ?
C84 C85 C86 118.6(9) . . ?
C86 C85 H85 120.7 . . ?
C73 C74 H74 120.6 . . ?
C75 C74 C73 118.8(8) . . ?
C75 C74 H74 120.6 . . ?
N15 C83 C84 123.5(9) . . ?
N15 C83 H83 118.3 . . ?
C84 C83 H83 118.3 . . ?
C15 C3 C4 106.5(7) . . ?
C15 C3 C2 108.3(8) . . ?
C4 C3 C2 108.2(7) . . ?
C26 C3 C15 116.8(7) . . ?
C26 C3 C4 107.7(8) . . ?
C26 C3 C2 109.1(8) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 108.1 . . ?
C47 C46 C45 110.8(8) . . ?
C47 C46 H46A 109.5 . . ?
C47 C46 H46B 109.5 . . ?
N9 C51 C52 110.2(7) . . ?
N9 C51 C39 125.2(7) . . ?
C52 C51 C39 124.6(7) . . ?
N5 C29 C30 119.5(8) . . ?
N5 C29 C28 110.8(9) . . ?
C28 C29 C30 129.7(10) . . ?
C40 C39 C38 109.1(7) . . ?
C40 C39 C51 109.2(7) . . ?
C40 C39 C62 106.6(6) . . ?
C51 C39 C38 107.6(7) . . ?
C51 C39 C62 114.5(7) . . ?
C62 C39 C38 109.8(7) . . ?
C4 C5 H5 127.3 . . ?
C6 C5 C4 105.4(8) . . ?
C6 C5 H5 127.3 . . ?
N10 C56 H56 107.4 . . ?
N10 C56 C61 111.1(8) . . ?
N10 C56 C57 112.7(8) . . ?
C61 C56 H56 107.4 . . ?
C61 C56 C57 110.7(8) . . ?
C57 C56 H56 107.4 . . ?
C46 C47 H47A 109.7 . . ?
C46 C47 H47B 109.7 . . ?
H47A C47 H47B 108.2 . . ?
C48 C47 C46 109.8(9) . . ?
C48 C47 H47A 109.7 . . ?
C48 C47 H47B 109.7 . . ?
N5 C26 C3 124.7(8) . . ?
N5 C26 C27 109.6(9) . . ?
C27 C26 C3 125.7(8) . . ?
N4 C19 C18 123.8(9) . . ?
N4 C19 H19 118.1 . . ?
C18 C19 H19 118.1 . . ?
C56 C61 H61A 109.1 . . ?
C56 C61 H61B 109.1 . . ?
H61A C61 H61B 107.8 . . ?
C60 C61 C56 112.5(10) . . ?
C60 C61 H61A 109.1 . . ?
C60 C61 H61B 109.1 . . ?
C9 C10 H10A 109.0 . . ?
C9 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
C94 C10 C9 112.9(7) . . ?
C94 C10 H10A 109.0 . . ?
C94 C10 H10B 109.0 . . ?
C3 C2 H2A 108.9 . . ?
C3 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C1 C2 C3 113.5(8) . . ?
C1 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 . . ?
N15 C87 H87 117.1 . . ?
N15 C87 C86 125.8(9) . . ?
C86 C87 H87 117.1 . . ?
C7 C6 H6 126.2 . . ?
C5 C6 C7 107.5(8) . . ?
C5 C6 H6 126.2 . . ?
C10 C94 H94A 109.3 . . ?
C10 C94 H94B 109.3 . . ?
C10 C94 C12 111.4(7) . . ?
H94A C94 H94B 108.0 . . ?
C12 C94 H94A 109.3 . . ?
C12 C94 H94B 109.3 . . ?
N6 C30 C29 123.4(9) . . ?
N6 C30 H30 118.3 . . ?
C29 C30 H30 118.3 . . ?
C31 C36 H36A 109.0 . . ?
C31 C36 H36B 109.0 . . ?
C31 C36 C35 113.0(9) . . ?
H36A C36 H36B 107.8 . . ?
C35 C36 H36A 109.0 . . ?
C35 C36 H36B 109.0 . . ?
H34A C34 H34B 108.0 . . ?
C35 C34 H34A 109.4 . . ?
C35 C34 H34B 109.4 . . ?
C35 C34 C33 111.4(10) . . ?
C33 C34 H34A 109.4 . . ?
C33 C34 H34B 109.4 . . ?
H22A C22 H22B 107.8 . . ?
C23 C22 H22A 109.1 . . ?
C23 C22 H22B 109.1 . . ?
C23 C22 C21 112.6(9) . . ?
C21 C22 H22A 109.1 . . ?
C21 C22 H22B 109.1 . . ?
N4 C20 H20 107.9 . . ?
N4 C20 C21 111.2(7) . . ?
N4 C20 C25 112.3(8) . . ?
C21 C20 H20 107.9 . . ?
C25 C20 H20 107.9 . . ?
C25 C20 C21 109.6(8) . . ?
C81 C80 H80 120.8 . . ?
C79 C80 C81 118.3(10) . . ?
C79 C80 H80 120.8 . . ?
N14 C82 C81 124.1(9) . . ?
N14 C82 H82 117.9 . . ?
C81 C82 H82 117.9 . . ?
H24A C24 H24B 108.0 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 C25 110.9(8) . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
N16 C62 C39 123.7(7) . . ?
N16 C62 C63 110.4(7) . . ?
C63 C62 C39 125.8(8) . . ?
C22 C23 C24 111.6(8) . . ?
C22 C23 H23A 109.3 . . ?
C22 C23 H23B 109.3 . . ?
C24 C23 H23A 109.3 . . ?
C24 C23 H23B 109.3 . . ?
H23A C23 H23B 108.0 . . ?
C22 C21 C20 110.2(8) . . ?
C22 C21 H21A 109.6 . . ?
C22 C21 H21B 109.6 . . ?
C20 C21 H21A 109.6 . . ?
C20 C21 H21B 109.6 . . ?
H21A C21 H21B 108.1 . . ?
N14 C78 H78 118.2 . . ?
N14 C78 C79 123.7(10) . . ?
C79 C78 H78 118.2 . . ?
C85 C86 H86 121.2 . . ?
C87 C86 C85 117.6(9) . . ?
C87 C86 H86 121.2 . . ?
C67 C72 H72A 109.3 . . ?
C67 C72 H72B 109.3 . . ?
C67 C72 C71 111.6(8) . . ?
H72A C72 H72B 108.0 . . ?
C71 C72 H72A 109.3 . . ?
C71 C72 H72B 109.3 . . ?
C20 C25 H25A 109.8 . . ?
C20 C25 H25B 109.8 . . ?
C24 C25 C20 109.6(8) . . ?
C24 C25 H25A 109.8 . . ?
C24 C25 H25B 109.8 . . ?
H25A C25 H25B 108.2 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 C33 110.8(10) . . ?
H32A C32 H32B 108.1 . . ?
C33 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C64 C63 C62 107.1(8) . . ?
C64 C63 H63 126.5 . . ?
C62 C63 H63 126.5 . . ?
C36 C35 H35A 109.5 . . ?
C36 C35 H35B 109.5 . . ?
C34 C35 C36 110.6(10) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 108.1 . . ?
C13 C12 C94 109.7(7) . . ?
C13 C12 H12A 109.7 . . ?
C13 C12 H12B 109.7 . . ?
C94 C12 H12A 109.7 . . ?
C94 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
C80 C79 C78 119.2(11) . . ?
C80 C79 H79 120.4 . . ?
C78 C79 H79 120.4 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
H70A C70 H70B 108.0 . . ?
C69 C70 H70A 109.4 . . ?
C69 C70 H70B 109.4 . . ?
C69 C70 C71 111.2(9) . . ?
C71 C70 H70A 109.4 . . ?
C71 C70 H70B 109.4 . . ?
C47 C48 H48A 109.7 . . ?
C47 C48 H48B 109.7 . . ?
H48A C48 H48B 108.2 . . ?
C49 C48 C47 109.6(9) . . ?
C49 C48 H48A 109.7 . . ?
C49 C48 H48B 109.7 . . ?
H58A C58 H58B 108.1 . . ?
C57 C58 H58A 109.6 . . ?
C57 C58 H58B 109.6 . . ?
C57 C58 C59 110.4(10) . . ?
C59 C58 H58A 109.6 . . ?
C59 C58 H58B 109.6 . . ?
C29 C28 H28 127.2 . . ?
C27 C28 C29 105.7(9) . . ?
C27 C28 H28 127.2 . . ?
C26 C27 H27 126.1 . . ?
C28 C27 C26 107.8(9) . . ?
C28 C27 H27 126.1 . . ?
C50 C49 H49A 109.4 . . ?
C50 C49 H49B 109.4 . . ?
C48 C49 C50 111.3(9) . . ?
C48 C49 H49A 109.4 . . ?
C48 C49 H49B 109.4 . . ?
H49A C49 H49B 108.0 . . ?
C56 C57 H57A 109.6 . . ?
C56 C57 H57B 109.6 . . ?
C58 C57 C56 110.3(9) . . ?
C58 C57 H57A 109.6 . . ?
C58 C57 H57B 109.6 . . ?
H57A C57 H57B 108.1 . . ?
C58 C59 H59A 109.2 . . ?
C58 C59 H59B 109.2 . . ?
H59A C59 H59B 107.9 . . ?
C60 C59 C58 112.1(11) . . ?
C60 C59 H59A 109.2 . . ?
C60 C59 H59B 109.2 . . ?
C67 C68 H68A 109.3 . . ?
C67 C68 H68B 109.3 . . ?
C67 C68 C69 111.7(8) . . ?
H68A C68 H68B 107.9 . . ?
C69 C68 H68A 109.3 . . ?
C69 C68 H68B 109.3 . . ?
C70 C69 C68 110.8(9) . . ?
C70 C69 H69A 109.5 . . ?
C70 C69 H69B 109.5 . . ?
C68 C69 H69A 109.5 . . ?
C68 C69 H69B 109.5 . . ?
H69A C69 H69B 108.1 . . ?
C34 C33 C32 112.0(10) . . ?
C34 C33 H33A 109.2 . . ?
C34 C33 H33B 109.2 . . ?
C32 C33 H33A 109.2 . . ?
C32 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
C72 C71 H71A 109.6 . . ?
C72 C71 H71B 109.6 . . ?
C70 C71 C72 110.2(10) . . ?
C70 C71 H71A 109.6 . . ?
C70 C71 H71B 109.6 . . ?
H71A C71 H71B 108.1 . . ?
C61 C60 C59 111.6(10) . . ?
C61 C60 H60A 109.3 . . ?
C61 C60 H60B 109.3 . . ?
C59 C60 H60A 109.3 . . ?
C59 C60 H60B 109.3 . . ?
H60A C60 H60B 108.0 . . ?
U2 O1 Y2 108.9(3) . . ?
H88A C88 H88B 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
C89 C88 H88A 109.5 . . ?
C89 C88 H88B 109.5 . . ?
C89 C88 H88C 109.5 . . ?
C88 C89 H89A 108.6 . . ?
C88 C89 H89B 108.6 . . ?
H89A C89 H89B 107.5 . . ?
C90 C89 C88 114.8(18) . . ?
C90 C89 H89A 108.6 . . ?
C90 C89 H89B 108.6 . . ?
C89 C90 H90A 109.0 . . ?
C89 C90 H90B 109.0 . . ?
C89 C90 C91 113.1(18) . . ?
H90A C90 H90B 107.8 . . ?
C91 C90 H90A 109.0 . . ?
C91 C90 H90B 109.0 . . ?
C90 C91 H91A 108.2 . . ?
C90 C91 H91B 108.2 . . ?
H91A C91 H91B 107.3 . . ?
C92 C91 C90 116.5(19) . . ?
C92 C91 H91A 108.2 . . ?
C92 C91 H91B 108.2 . . ?
C91 C92 H92A 108.5 . . ?
C91 C92 H92B 108.5 . . ?
C91 C92 C93 115.0(18) . . ?
H92A C92 H92B 107.5 . . ?
C93 C92 H92A 108.5 . . ?
C93 C92 H92B 108.5 . . ?
C92 C93 H93A 109.5 . . ?
C92 C93 H93B 109.5 . . ?
C92 C93 H93C 109.5 . . ?
H93A C93 H93B 109.5 . . ?
H93A C93 H93C 109.5 . . ?
H93B C93 H93C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U2 N2 C9 C14 -89.8(7) . . . . ?
U2 N2 C9 C10 145.5(6) . . . . ?
U2 N2 C8 C7 0.0(11) . . . . ?
U2 N1 C4 C3 1.0(13) . . . . ?
U2 N1 C4 C5 178.1(7) . . . . ?
U2 N1 C7 C8 -2.8(11) . . . . ?
U2 N1 C7 C6 -179.4(6) . . . . ?
U2 C17 C18 N3 72.6(6) . . . . ?
U2 C17 C18 C19 -111.5(10) . . . . ?
U2 C17 C16 C15 -70.9(7) . . . . ?
U2 C18 C19 N4 81.6(10) . . . . ?
U1 N8 C45 C50 -94.4(8) . . . . ?
U1 N8 C45 C46 141.9(6) . . . . ?
U1 N8 C44 C43 2.7(10) . . . . ?
U1 N13 C73 C74 174.2(7) . . . . ?
U1 N13 C77 C76 -175.6(7) . . . . ?
U1 N7 C43 C44 -9.1(9) . . . . ?
U1 N7 C43 C42 174.2(5) . . . . ?
U1 N7 C40 C41 -172.7(6) . . . . ?
U1 N7 C40 C39 12.0(12) . . . . ?
U1 C52 C51 N9 -76.8(6) . . . . ?
U1 C52 C51 C39 102.0(7) . . . . ?
Y2 N9 C54 C53 -146.8(6) . . . . ?
Y2 N9 C54 C55 30.8(9) . . . . ?
Y2 N9 C51 C52 135.8(6) . . . . ?
Y2 N9 C51 C39 -43.0(11) . . . . ?
Y2 N15 C83 C84 168.3(7) . . . . ?
Y2 N15 C87 C86 -165.8(7) . . . . ?
Y2 N12 C66 C65 -8.8(10) . . . . ?
Y2 N12 C67 C72 -56.3(9) . . . . ?
Y2 N12 C67 C68 178.9(6) . . . . ?
Y2 N10 C55 C54 -15.4(10) . . . . ?
Y2 N10 C56 C61 -2.7(12) . . . . ?
Y2 N10 C56 C57 122.1(8) . . . . ?
Y2 N16 C65 C66 12.1(9) . . . . ?
Y2 N16 C65 C64 -168.8(6) . . . . ?
Y2 N16 C62 C39 -20.0(13) . . . . ?
Y2 N16 C62 C63 163.7(6) . . . . ?
Y1 N3 C18 U2 -82.7(3) . . . . ?
Y1 N3 C18 C17 -154.5(6) . . . . ?
Y1 N3 C18 C19 29.1(10) . . . . ?
Y1 N3 C15 C16 146.3(7) . . . . ?
Y1 N3 C15 C3 -33.0(13) . . . . ?
Y1 N5 C29 C30 5.3(12) . . . . ?
Y1 N5 C29 C28 -174.6(8) . . . . ?
Y1 N5 C26 C3 -12.4(16) . . . . ?
Y1 N5 C26 C27 171.5(8) . . . . ?
Y1 N4 C19 C18 -14.7(11) . . . . ?
Y1 N4 C20 C21 108.1(9) . . . . ?
Y1 N4 C20 C25 -15.0(12) . . . . ?
Y1 N6 C31 C36 113.7(8) . . . . ?
Y1 N6 C31 C32 -120.4(8) . . . . ?
Y1 N6 C30 C29 -3.1(12) . . . . ?
Y1 N14 C82 C81 -179.2(8) . . . . ?
Y1 N14 C78 C79 177.7(11) . . . . ?
N8 C45 C50 C49 175.9(8) . . . . ?
N8 C45 C46 C47 -176.6(8) . . . . ?
N2 C9 C14 C13 178.6(7) . . . . ?
N2 C9 C10 C94 175.8(7) . . . . ?
N2 C8 C7 N1 1.9(13) . . . . ?
N2 C8 C7 C6 177.5(9) . . . . ?
N13 C73 C74 C75 2.2(15) . . . . ?
N3 C18 C19 N4 -8.9(13) . . . . ?
N3 C15 C16 C17 -0.4(11) . . . . ?
N3 C15 C3 C4 119.9(9) . . . . ?
N3 C15 C3 C26 -0.4(13) . . . . ?
N3 C15 C3 C2 -124.0(9) . . . . ?
N1 C4 C3 C15 -24.1(11) . . . . ?
N1 C4 C3 C26 101.9(10) . . . . ?
N1 C4 C3 C2 -140.4(9) . . . . ?
N1 C4 C5 C6 0.9(12) . . . . ?
N1 C7 C6 C5 1.4(11) . . . . ?
N7 C43 C44 N8 4.5(12) . . . . ?
N7 C43 C42 C41 0.9(9) . . . . ?
N7 C40 C41 C42 -0.3(9) . . . . ?
N7 C40 C39 C38 -139.3(7) . . . . ?
N7 C40 C39 C51 -21.9(10) . . . . ?
N7 C40 C39 C62 102.3(8) . . . . ?
N9 C51 C39 C40 120.2(8) . . . . ?
N9 C51 C39 C38 -121.5(8) . . . . ?
N9 C51 C39 C62 0.8(11) . . . . ?
N5 C29 C30 N6 -1.4(16) . . . . ?
N5 C29 C28 C27 1.0(14) . . . . ?
N5 C26 C27 C28 0.8(14) . . . . ?
N4 C20 C21 C22 177.8(9) . . . . ?
N4 C20 C25 C24 -176.0(8) . . . . ?
C17 C18 C19 N4 175.5(9) . . . . ?
N15 C87 C86 C85 -2.8(15) . . . . ?
N12 C66 C65 N16 -1.9(12) . . . . ?
N12 C66 C65 C64 179.3(9) . . . . ?
N12 C67 C72 C71 174.7(8) . . . . ?
N12 C67 C68 C69 -179.4(8) . . . . ?
N10 C55 C54 N9 -10.3(13) . . . . ?
N10 C55 C54 C53 166.8(9) . . . . ?
N10 C56 C61 C60 -179.1(9) . . . . ?
N10 C56 C57 C58 178.2(9) . . . . ?
N6 C31 C36 C35 -178.3(9) . . . . ?
N6 C31 C32 C33 179.8(9) . . . . ?
C9 N2 C8 C7 -175.8(8) . . . . ?
C9 C14 C13 C12 57.5(9) . . . . ?
C9 C10 C94 C12 -54.7(10) . . . . ?
C43 N7 C40 C41 0.8(8) . . . . ?
C43 N7 C40 C39 -174.5(7) . . . . ?
C43 C42 C41 C40 -0.4(9) . . . . ?
N16 C65 C64 C63 1.3(10) . . . . ?
N16 C62 C63 C64 -0.1(10) . . . . ?
C18 N3 C15 C16 -0.2(10) . . . . ?
C18 N3 C15 C3 -179.5(8) . . . . ?
C18 C17 C16 C15 0.8(10) . . . . ?
C15 N3 C18 U2 72.5(6) . . . . ?
C15 N3 C18 C17 0.7(10) . . . . ?
C15 N3 C18 C19 -175.6(8) . . . . ?
C15 C3 C26 N5 21.4(14) . . . . ?
C15 C3 C26 C27 -163.1(10) . . . . ?
C15 C3 C2 C1 66.7(11) . . . . ?
C53 C52 C51 N9 1.9(10) . . . . ?
C53 C52 C51 C39 -179.4(8) . . . . ?
C40 N7 C43 C44 175.6(7) . . . . ?
C40 N7 C43 C42 -1.1(9) . . . . ?
C40 C39 C62 N16 -91.8(9) . . . . ?
C40 C39 C62 C63 83.9(10) . . . . ?
C45 N8 C44 C43 -173.9(7) . . . . ?
C45 C50 C49 C48 58.1(12) . . . . ?
C45 C46 C47 C48 -59.5(11) . . . . ?
C14 C9 C10 C94 51.9(10) . . . . ?
C14 C13 C12 C94 -58.0(10) . . . . ?
C73 N13 C77 C76 1.4(14) . . . . ?
N14 C78 C79 C80 1(2) . . . . ?
C55 N10 C56 C61 162.7(8) . . . . ?
C55 N10 C56 C57 -72.5(11) . . . . ?
C4 N1 C7 C8 175.8(8) . . . . ?
C4 N1 C7 C6 -0.8(10) . . . . ?
C4 C3 C26 N5 -98.3(11) . . . . ?
C4 C3 C26 C27 77.2(13) . . . . ?
C4 C3 C2 C1 -178.2(9) . . . . ?
C4 C5 C6 C7 -1.3(11) . . . . ?
C8 N2 C9 C14 85.7(9) . . . . ?
C8 N2 C9 C10 -39.0(11) . . . . ?
C8 C7 C6 C5 -174.6(10) . . . . ?
C44 N8 C45 C50 81.7(9) . . . . ?
C44 N8 C45 C46 -41.9(10) . . . . ?
C44 C43 C42 C41 -175.4(8) . . . . ?
C52 C53 C54 N9 0.7(10) . . . . ?
C52 C53 C54 C55 -176.6(9) . . . . ?
C52 C51 C39 C40 -58.3(10) . . . . ?
C52 C51 C39 C38 60.0(10) . . . . ?
C52 C51 C39 C62 -177.7(8) . . . . ?
C7 N1 C4 C3 -177.2(8) . . . . ?
C7 N1 C4 C5 -0.1(11) . . . . ?
C54 N9 C51 C52 -1.4(9) . . . . ?
C54 N9 C51 C39 179.8(7) . . . . ?
C54 C53 C52 U1 81.2(6) . . . . ?
C54 C53 C52 C51 -1.5(10) . . . . ?
C66 N12 C67 C72 120.8(9) . . . . ?
C66 N12 C67 C68 -4.0(12) . . . . ?
C66 C65 C64 C63 -179.8(9) . . . . ?
C16 C17 C18 U2 -73.6(6) . . . . ?
C16 C17 C18 N3 -1.0(10) . . . . ?
C16 C17 C18 C19 174.9(9) . . . . ?
C16 C15 C3 C4 -59.3(11) . . . . ?
C16 C15 C3 C26 -179.6(9) . . . . ?
C16 C15 C3 C2 56.8(11) . . . . ?
C76 C75 C74 C73 0.7(15) . . . . ?
C50 C45 C46 C47 59.0(10) . . . . ?
C31 N6 C30 C29 177.2(9) . . . . ?
C31 C36 C35 C34 -55.6(13) . . . . ?
C31 C32 C33 C34 54.4(14) . . . . ?
C81 C80 C79 C78 0(2) . . . . ?
C77 N13 C73 C74 -3.2(14) . . . . ?
C77 C76 C75 C74 -2.3(15) . . . . ?
C42 C43 C44 N8 -179.6(8) . . . . ?
C67 N12 C66 C65 173.8(7) . . . . ?
C67 C72 C71 C70 56.4(12) . . . . ?
C67 C68 C69 C70 -57.0(11) . . . . ?
C84 C85 C86 C87 0.0(14) . . . . ?
C65 N16 C62 C39 177.1(8) . . . . ?
C65 N16 C62 C63 0.8(9) . . . . ?
C65 C64 C63 C62 -0.7(10) . . . . ?
C75 C76 C77 N13 1.3(15) . . . . ?
C41 C40 C39 C38 46.3(10) . . . . ?
C41 C40 C39 C51 163.6(7) . . . . ?
C41 C40 C39 C62 -72.2(10) . . . . ?
C38 C39 C62 N16 150.2(8) . . . . ?
C38 C39 C62 C63 -34.1(11) . . . . ?
C85 C84 C83 N15 0.4(15) . . . . ?
C83 N15 C87 C86 4.2(13) . . . . ?
C83 C84 C85 C86 1.0(14) . . . . ?
C3 C15 C16 C17 178.9(8) . . . . ?
C3 C4 C5 C6 177.6(9) . . . . ?
C3 C26 C27 C28 -175.3(11) . . . . ?
C46 C45 C50 C49 -57.5(10) . . . . ?
C46 C47 C48 C49 58.1(12) . . . . ?
C51 N9 C54 C53 0.5(10) . . . . ?
C51 N9 C54 C55 178.1(8) . . . . ?
C51 C39 C62 N16 29.1(11) . . . . ?
C51 C39 C62 C63 -155.3(8) . . . . ?
C29 N5 C26 C3 175.9(9) . . . . ?
C29 N5 C26 C27 -0.2(12) . . . . ?
C29 C28 C27 C26 -1.1(15) . . . . ?
C39 C40 C41 C42 174.6(7) . . . . ?
C39 C62 C63 C64 -176.2(8) . . . . ?
C5 C4 C3 C15 159.4(10) . . . . ?
C5 C4 C3 C26 -74.6(12) . . . . ?
C5 C4 C3 C2 43.1(14) . . . . ?
C56 N10 C55 C54 175.7(8) . . . . ?
C56 C61 C60 C59 -53.5(15) . . . . ?
C47 C48 C49 C50 -58.0(13) . . . . ?
C26 N5 C29 C30 179.4(9) . . . . ?
C26 N5 C29 C28 -0.5(12) . . . . ?
C26 C3 C2 C1 -61.3(12) . . . . ?
C19 N4 C20 C21 -85.9(10) . . . . ?
C19 N4 C20 C25 151.0(8) . . . . ?
C61 C56 C57 C58 -56.7(12) . . . . ?
C10 C9 C14 C13 -53.6(9) . . . . ?
C10 C94 C12 C13 57.0(10) . . . . ?
C2 C3 C26 N5 144.5(9) . . . . ?
C2 C3 C26 C27 -40.0(14) . . . . ?
C87 N15 C83 C84 -2.9(13) . . . . ?
C30 N6 C31 C36 -66.7(11) . . . . ?
C30 N6 C31 C32 59.3(12) . . . . ?
C30 C29 C28 C27 -178.8(11) . . . . ?
C36 C31 C32 C33 -53.6(12) . . . . ?
C20 N4 C19 C18 175.4(8) . . . . ?
C80 C81 C82 N14 2.1(18) . . . . ?
C82 N14 C78 C79 0.2(19) . . . . ?
C82 C81 C80 C79 -1(2) . . . . ?
C62 N16 C65 C66 179.7(7) . . . . ?
C62 N16 C65 C64 -1.3(9) . . . . ?
C23 C22 C21 C20 54.7(13) . . . . ?
C23 C24 C25 C20 -58.8(11) . . . . ?
C21 C22 C23 C24 -53.5(13) . . . . ?
C21 C20 C25 C24 59.9(10) . . . . ?
C78 N14 C82 C81 -1.7(16) . . . . ?
C72 C67 C68 C69 56.2(11) . . . . ?
C25 C20 C21 C22 -57.5(11) . . . . ?
C25 C24 C23 C22 55.3(12) . . . . ?
C32 C31 C36 C35 54.9(12) . . . . ?
C35 C34 C33 C32 -55.6(14) . . . . ?
C37 C38 C39 C40 -179.8(7) . . . . ?
C37 C38 C39 C51 61.8(9) . . . . ?
C37 C38 C39 C62 -63.4(10) . . . . ?
C58 C59 C60 C61 53.7(17) . . . . ?
C28 C29 C30 N6 178.4(12) . . . . ?
C57 C56 C61 C60 55.0(13) . . . . ?
C57 C58 C59 C60 -55.9(15) . . . . ?
C59 C58 C57 C56 57.0(13) . . . . ?
C68 C67 C72 C71 -56.3(11) . . . . ?
C69 C70 C71 C72 -56.3(13) . . . . ?
C33 C34 C35 C36 55.0(13) . . . . ?
C71 C70 C69 C68 56.5(12) . . . . ?
C88 C89 C90 C91 174(3) . . . . ?
C89 C90 C91 C92 167(3) . . . . ?
C90 C91 C92 C93 168(3) . . . . ?


# start Validation Reply Form
_vrf_PLAT602_to517-pyr_twin1_hklf4_refinalised 
;
PROBLEM: Solvent Accessible VOID(S) in Structure ........          ! Check 
RESPONSE: SQUEEZE finds a void with 10 electrons. This is too small for any 
solvent used in the preparation of the crystal. Assigning the electron density 
as a water molecule results in very large ellipsoids and the presence of water
is unlikely as the sample is prepared under an inert atmosphere with dry 
reagents and solvents. A solvent mask has not been usedin this structure.
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.232
_oxdiff_exptl_absorpt_empirical_full_min 0.760
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Pyridene, hexane'
_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_to505_refinalised
_database_code_depnum_ccdc_archive 'CCDC 2313507'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2023-12-11 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_audit_creation_date             2023-10-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C66 H77 Cl3 Li2 N12 O2 U Y, C5 H5 N'
_chemical_formula_sum            'C71 H82 Cl3 Li2 N13 O2 U Y'
_chemical_formula_weight         1596.66
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C50 H70 N6 U O2 Y Cl2 Li'
_chemical_oxdiff_usercomment     Pyr/hex
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'
Li Li -0.0003 0.0001 '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'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   19.0604(3)
_cell_length_b                   17.0605(2)
_cell_length_c                   24.4496(4)
_cell_angle_alpha                90
_cell_angle_beta                 106.506(2)
_cell_angle_gamma                90
_cell_volume                     7622.9(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    41820
_cell_measurement_temperature    120.2(8)
_cell_measurement_theta_max      28.4090
_cell_measurement_theta_min      3.5350
_shelx_estimated_absorpt_T_max   0.778
_shelx_estimated_absorpt_T_min   0.383
_exptl_absorpt_coefficient_mu    3.034
_exptl_absorpt_correction_T_max  0.653
_exptl_absorpt_correction_T_min  0.203
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3212
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
11 3 26 0.1885
-3 -24 2 0.1539
-10 1 -27 0.1704
-1 23 -11 0.1704
7 4 29 0.1822
-24 3 22 0.0541
-10 -3 -26 0.1950
24 -3 -23 0.0279

_exptl_crystal_preparation       
'Vapour diffusion of hexane into pyridine solution'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Pyridene, hexane'
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.382
_exptl_crystal_size_min          0.087
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
10.7174 2.9358 26.1372 -0.0015 -0.0177 0.9998
-2.8585 -23.8971 2.2820 -0.1287 -0.9807 -0.1474
-10.2626 1.4751 -26.7439 0.0253 0.1997 -0.9795
-0.7040 22.6430 -10.8589 0.1277 0.9747 -0.1835
6.8309 3.7093 29.0733 -0.1518 0.0189 0.9882
-24.3666 2.7719 22.2771 -0.9913 0.1300 0.0212
-10.4949 -3.3598 -26.2532 0.0092 -0.0002 -1.0000
24.0369 -2.8641 -22.9963 0.9903 -0.1298 -0.0496

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            153359
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.868
_diffrn_reflns_theta_min         3.327
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.2(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -35.00  55.00   1.00   60.00    --  -14.44  33.00  95.00   90
  2  ω    -53.00  37.00   1.00   60.00    --   16.16 -33.00 -62.00   90
  3  ω     -4.00  86.00   1.00   60.00    --   16.16  33.00  95.00   90
  4  ω    -39.00  12.00   1.00   60.00    --  -14.44 -77.00-180.00   51
  5  ω    -41.00  39.00   1.00   60.00    --  -14.44  77.00 -90.00   80
  6  ω    -39.00  12.00   1.00   60.00    --  -14.44 -77.00  60.00   51
  7  ω    -87.00 -39.00   1.00   60.00    --  -14.44-178.00 120.00   48
  8  ω    -11.00  39.00   1.00   60.00    --   16.16  77.00 -30.00   50
  9  ω     35.00  89.00   1.00   60.00    --   16.16-178.00-120.00   54
 10  ω    -11.00  39.00   1.00   60.00    --   16.16  77.00-180.00   50
 11  ω    -20.00  54.00   1.00   60.00    --   16.16 -99.00-180.00   74
 12  ω    -11.00  39.00   1.00   60.00    --   16.16  77.00-120.00   50
 13  ω    -20.00  54.00   1.00   60.00    --   16.16 -99.00  60.00   74
 14  ω     -1.00  83.00   1.00   60.00    --   16.16  57.00   0.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0295581000
_diffrn_orient_matrix_UB_12      0.0006810000
_diffrn_orient_matrix_UB_13      -0.0122524000
_diffrn_orient_matrix_UB_21      -0.0039983000
_diffrn_orient_matrix_UB_22      0.0411658000
_diffrn_orient_matrix_UB_23      -0.0036612000
_diffrn_orient_matrix_UB_31      0.0248521000
_diffrn_orient_matrix_UB_32      0.0058121000
_diffrn_orient_matrix_UB_33      0.0274104000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13924
_reflns_number_total             18097
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.187
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         18097
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0359
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0254P)²+10.9349P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0723
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C31(H31), C20(H20), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C14(H14A,H14B), C2(H2A,H2B), C25(H25A,H25B), C24(H24A,H24B),
 C36(H36A,H36B), C21(H21A,H21B), C23(H23A,H23B), C33(H33A,H33B), C10(H10A,H10B),
  C22(H22A,H22B), C13(H13A,H13B), C11(H11A,H11B), C35(H35A,H35B), C12(H12A,
 H12B), C34(H34A,H34B)
2.c Aromatic/amide H refined with riding coordinates:
 C30(H30), C19(H19), C52(H52), C27(H27), C17(H17), C28(H28), C16(H16),
 C41(H41), C37(H37), C6(H6), C8(H8), C42(H42), C71(H71), C57(H57), C38(H38),
 C5(H5), C59(H59), C56(H56), C61(H61), C39(H39), C64(H64), C51(H51), C53(H53),
 C62(H62), C46(H46), C66(H66), C47(H47), C50(H50), C40(H40), C60(H60), C63(H63),
  C58(H58), C67(H67), C54(H54), C49(H49), C70(H70), C55(H55), C65(H65),
 C48(H48), C68(H68), C69(H69), C43(H43), C45(H45), C44(H44)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.56799(2) 0.72176(2) 0.36591(2) 0.01121(4) Uani 1 1 d . . . . .
Y1 Y 0.49999(2) 0.58016(2) 0.24230(2) 0.01352(7) Uani 1 1 d . . . . .
Cl3 Cl 0.47234(5) 0.84731(4) 0.35532(3) 0.01855(17) Uani 1 1 d . . . . .
Cl2 Cl 0.38590(5) 0.65882(5) 0.17960(3) 0.02052(18) Uani 1 1 d . . . . .
Cl1 Cl 0.40989(5) 0.49133(5) 0.27382(4) 0.02562(19) Uani 1 1 d . . . . .
N5 N 0.66917(14) 0.66798(15) 0.33098(10) 0.0136(6) Uani 1 1 d . . . . .
N4 N 0.47261(15) 0.66963(15) 0.41445(11) 0.0151(6) Uani 1 1 d . . . . .
N3 N 0.57957(15) 0.57745(15) 0.38087(11) 0.0154(6) Uani 1 1 d . . . . .
N6 N 0.63253(15) 0.82885(15) 0.32338(11) 0.0163(6) Uani 1 1 d . . . . .
N1 N 0.59677(15) 0.48958(15) 0.25503(10) 0.0145(6) Uani 1 1 d . . . . .
N8 N 0.32057(17) 0.74555(19) 0.27992(12) 0.0264(7) Uani 1 1 d . . . . .
N2 N 0.48092(15) 0.49750(15) 0.15468(11) 0.0162(6) Uani 1 1 d . . . . .
N10 N 0.69130(16) 0.68788(17) 0.56295(12) 0.0221(6) Uani 1 1 d . . . . .
N7 N 0.56999(15) 0.66201(16) 0.18875(11) 0.0186(6) Uani 1 1 d . . . . .
C26 C 0.70346(17) 0.59861(18) 0.32820(12) 0.0136(7) Uani 1 1 d . . . . .
C29 C 0.70221(17) 0.72213(19) 0.30324(12) 0.0146(6) Uani 1 1 d . . . . .
N12 N 0.79457(16) 0.78741(16) 0.49469(11) 0.0212(6) Uani 1 1 d . . . . .
C31 C 0.61982(19) 0.91359(18) 0.32508(13) 0.0165(7) Uani 1 1 d . . . . .
H31 H 0.565548 0.921065 0.313047 0.020 Uiso 1 1 calc R U . . .
N11 N 0.66415(16) 0.87801(16) 0.54987(12) 0.0204(6) Uani 1 1 d . . . . .
C30 C 0.68265(18) 0.80250(19) 0.30089(13) 0.0148(7) Uani 1 1 d . . . . .
H30 H 0.706613 0.838315 0.282442 0.018 Uiso 1 1 calc R U . . .
N9 N 0.40656(16) 0.86349(17) 0.20233(12) 0.0243(7) Uani 1 1 d . . . . .
C18 C 0.53161(18) 0.54753(18) 0.40959(13) 0.0159(7) Uani 1 1 d . . . . .
C15 C 0.62591(17) 0.51730(18) 0.37876(12) 0.0134(7) Uani 1 1 d . . . . .
C19 C 0.47910(18) 0.59559(19) 0.42469(13) 0.0160(7) Uani 1 1 d . . . . .
H19 H 0.447097 0.571791 0.443333 0.019 Uiso 1 1 calc R U . . .
C20 C 0.42058(18) 0.71518(18) 0.43605(13) 0.0163(7) Uani 1 1 d . . . . .
H20 H 0.395930 0.753204 0.405501 0.020 Uiso 1 1 calc R U . . .
C52 C 0.6760(2) 0.6210(2) 0.53335(14) 0.0234(8) Uani 1 1 d . . . . .
H52 H 0.671800 0.622430 0.493705 0.028 Uiso 1 1 calc R U . . .
C27 C 0.75634(19) 0.6083(2) 0.29904(14) 0.0200(7) Uani 1 1 d . . . . .
H27 H 0.786966 0.568398 0.291276 0.024 Uiso 1 1 calc R U . . .
C17 C 0.54752(19) 0.47007(19) 0.42370(13) 0.0177(7) Uani 1 1 d . . . . .
H17 H 0.522512 0.436397 0.442825 0.021 Uiso 1 1 calc R U . . .
N13 N 0.48283(19) 0.17754(19) 0.26069(15) 0.0369(8) Uani 1 1 d . . . . .
C4 C 0.65879(18) 0.46841(18) 0.29587(13) 0.0146(7) Uani 1 1 d . . . . .
C28 C 0.75599(19) 0.6863(2) 0.28353(14) 0.0189(7) Uani 1 1 d . . . . .
H28 H 0.786268 0.710527 0.263533 0.023 Uiso 1 1 calc R U . . .
C3 C 0.68553(17) 0.51913(18) 0.34894(13) 0.0147(7) Uani 1 1 d . . . . .
C16 C 0.60755(19) 0.45072(19) 0.40442(13) 0.0183(7) Uani 1 1 d . . . . .
H16 H 0.631407 0.401295 0.408132 0.022 Uiso 1 1 calc R U . . .
C32 C 0.6471(2) 0.9420(2) 0.38703(15) 0.0250(8) Uani 1 1 d . . . . .
H32A H 0.627979 0.907241 0.411874 0.030 Uiso 1 1 calc R U . . .
H32B H 0.701228 0.939782 0.400057 0.030 Uiso 1 1 calc R U . . .
C14 C 0.4407(2) 0.4847(2) 0.04729(14) 0.0290(9) Uani 1 1 d . . . . .
H14A H 0.467222 0.434378 0.049416 0.035 Uiso 1 1 calc R U . . .
H14B H 0.474221 0.527407 0.043623 0.035 Uiso 1 1 calc R U . . .
C9 C 0.41810(18) 0.49629(19) 0.10182(13) 0.0181(7) Uani 1 1 d . . . . .
H9 H 0.394059 0.548838 0.098825 0.022 Uiso 1 1 calc R U . . .
C2 C 0.75690(18) 0.4836(2) 0.38901(14) 0.0195(7) Uani 1 1 d . . . . .
H2A H 0.746908 0.429236 0.398726 0.023 Uiso 1 1 calc R U . . .
H2B H 0.794500 0.481423 0.368232 0.023 Uiso 1 1 calc R U . . .
C25 C 0.46273(19) 0.76292(19) 0.48759(14) 0.0203(7) Uani 1 1 d . . . . .
H25A H 0.487294 0.726877 0.518914 0.024 Uiso 1 1 calc R U . . .
H25B H 0.501006 0.793995 0.477334 0.024 Uiso 1 1 calc R U . . .
C41 C 0.5558(2) 0.7389(2) 0.18110(14) 0.0235(8) Uani 1 1 d . . . . .
H41 H 0.522637 0.762024 0.198930 0.028 Uiso 1 1 calc R U . . .
C7 C 0.58851(19) 0.43492(19) 0.21179(13) 0.0186(7) Uani 1 1 d . . . . .
C37 C 0.6179(2) 0.6312(2) 0.16439(15) 0.0265(8) Uani 1 1 d . . . . .
H37 H 0.629749 0.577210 0.170341 0.032 Uiso 1 1 calc R U . . .
C24 C 0.4127(2) 0.8179(2) 0.50818(15) 0.0255(8) Uani 1 1 d . . . . .
H24A H 0.392259 0.857592 0.478380 0.031 Uiso 1 1 calc R U . . .
H24B H 0.441532 0.845712 0.542821 0.031 Uiso 1 1 calc R U . . .
C36 C 0.6498(2) 0.9660(2) 0.28671(16) 0.0266(8) Uani 1 1 d . . . . .
H36A H 0.632514 0.947309 0.246784 0.032 Uiso 1 1 calc R U . . .
H36B H 0.703974 0.964385 0.298891 0.032 Uiso 1 1 calc R U . . .
C1 C 0.7874(2) 0.5296(2) 0.44400(14) 0.0262(8) Uani 1 1 d . . . . .
H1A H 0.797358 0.583681 0.434837 0.039 Uiso 1 1 calc R U . . .
H1B H 0.832842 0.505098 0.466657 0.039 Uiso 1 1 calc R U . . .
H1C H 0.751564 0.529769 0.465895 0.039 Uiso 1 1 calc R U . . .
C21 C 0.36037(18) 0.66844(19) 0.45151(14) 0.0194(7) Uani 1 1 d . . . . .
H21A H 0.332238 0.638043 0.417932 0.023 Uiso 1 1 calc R U . . .
H21B H 0.382703 0.631033 0.482522 0.023 Uiso 1 1 calc R U . . .
C6 C 0.64470(19) 0.3808(2) 0.22559(14) 0.0213(8) Uani 1 1 d . . . . .
H6 H 0.651158 0.337619 0.203011 0.026 Uiso 1 1 calc R U . . .
C8 C 0.52794(19) 0.44127(19) 0.16188(13) 0.0187(7) Uani 1 1 d . . . . .
H8 H 0.521989 0.402714 0.132889 0.022 Uiso 1 1 calc R U . . .
C23 C 0.3502(2) 0.7735(2) 0.52169(15) 0.0254(8) Uani 1 1 d . . . . .
H23A H 0.316084 0.811347 0.531265 0.030 Uiso 1 1 calc R U . . .
H23B H 0.370038 0.739319 0.555227 0.030 Uiso 1 1 calc R U . . .
C33 C 0.6217(2) 1.0261(2) 0.39183(16) 0.0278(9) Uani 1 1 d . . . . .
H33A H 0.567660 1.027231 0.382622 0.033 Uiso 1 1 calc R U . . .
H33B H 0.642038 1.044762 0.431540 0.033 Uiso 1 1 calc R U . . .
C42 C 0.2972(2) 0.6739(3) 0.28737(16) 0.0356(10) Uani 1 1 d . . . . .
H42 H 0.326063 0.630341 0.282891 0.043 Uiso 1 1 calc R U . . .
C10 C 0.36173(19) 0.4364(2) 0.10707(14) 0.0241(8) Uani 1 1 d . . . . .
H10A H 0.345360 0.448594 0.141094 0.029 Uiso 1 1 calc R U . . .
H10B H 0.384407 0.383729 0.112466 0.029 Uiso 1 1 calc R U . . .
C71 C 0.4540(2) 0.1610(2) 0.30304(18) 0.0357(10) Uani 1 1 d . . . . .
H71 H 0.434402 0.110020 0.304068 0.043 Uiso 1 1 calc R U . . .
C57 C 0.6053(2) 0.9240(2) 0.53385(15) 0.0258(8) Uani 1 1 d . . . . .
H57 H 0.572341 0.916384 0.496969 0.031 Uiso 1 1 calc R U . . .
C38 C 0.6510(2) 0.6743(3) 0.13088(16) 0.0332(9) Uani 1 1 d . . . . .
H38 H 0.684270 0.649939 0.113686 0.040 Uiso 1 1 calc R U . . .
C5 C 0.69022(19) 0.40194(19) 0.27917(14) 0.0204(8) Uani 1 1 d . . . . .
H5 H 0.733807 0.376217 0.300048 0.024 Uiso 1 1 calc R U . . .
C59 C 0.6375(2) 0.9942(2) 0.62143(17) 0.0334(9) Uani 1 1 d . . . . .
H59 H 0.628022 1.033664 0.645843 0.040 Uiso 1 1 calc R U . . .
C56 C 0.6964(2) 0.6837(2) 0.61881(15) 0.0298(9) Uani 1 1 d . . . . .
H56 H 0.708238 0.730112 0.640996 0.036 Uiso 1 1 calc R U . . .
C61 C 0.7098(2) 0.8912(2) 0.60202(14) 0.0228(8) Uani 1 1 d . . . . .
H61 H 0.752184 0.859333 0.614456 0.027 Uiso 1 1 calc R U . . .
C22 C 0.30892(19) 0.7238(2) 0.47080(15) 0.0239(8) Uani 1 1 d . . . . .
H22A H 0.284091 0.758599 0.438763 0.029 Uiso 1 1 calc R U . . .
H22B H 0.270929 0.692650 0.481409 0.029 Uiso 1 1 calc R U . . .
C13 C 0.3738(2) 0.4844(2) -0.00507(14) 0.0307(9) Uani 1 1 d . . . . .
H13A H 0.350436 0.536737 -0.009561 0.037 Uiso 1 1 calc R U . . .
H13B H 0.389522 0.473580 -0.039584 0.037 Uiso 1 1 calc R U . . .
C39 C 0.6354(2) 0.7529(3) 0.12263(16) 0.0358(10) Uani 1 1 d . . . . .
H39 H 0.657348 0.783582 0.099561 0.043 Uiso 1 1 calc R U . . .
C11 C 0.2955(2) 0.4358(2) 0.05415(15) 0.0316(9) Uani 1 1 d . . . . .
H11A H 0.261545 0.393465 0.057807 0.038 Uiso 1 1 calc R U . . .
H11B H 0.269115 0.486296 0.051397 0.038 Uiso 1 1 calc R U . . .
C64 C 0.9288(2) 0.7865(2) 0.46992(17) 0.0335(9) Uani 1 1 d . . . . .
H64 H 0.974407 0.786437 0.461349 0.040 Uiso 1 1 calc R U . . .
C51 C 0.4223(2) 0.9373(2) 0.21964(16) 0.0276(9) Uani 1 1 d . . . . .
H51 H 0.440621 0.946777 0.259451 0.033 Uiso 1 1 calc R U . . .
C53 C 0.6661(2) 0.5503(2) 0.55725(15) 0.0285(9) Uani 1 1 d . . . . .
H53 H 0.656566 0.504098 0.534691 0.034 Uiso 1 1 calc R U . . .
C62 C 0.7998(2) 0.7721(2) 0.44239(14) 0.0286(9) Uani 1 1 d . . . . .
H62 H 0.756066 0.760799 0.413205 0.034 Uiso 1 1 calc R U . . .
C46 C 0.2790(2) 0.8059(3) 0.28619(17) 0.0423(11) Uani 1 1 d . . . . .
H46 H 0.295123 0.857489 0.281669 0.051 Uiso 1 1 calc R U . . .
C66 C 0.8574(2) 0.8017(2) 0.53470(15) 0.0275(9) Uani 1 1 d . . . . .
H66 H 0.855359 0.812622 0.572323 0.033 Uiso 1 1 calc R U . . .
C47 C 0.3806(2) 0.8528(2) 0.14579(16) 0.0332(10) Uani 1 1 d . . . . .
H47 H 0.369214 0.800960 0.132020 0.040 Uiso 1 1 calc R U . . .
C35 C 0.6232(2) 1.0501(2) 0.29083(17) 0.0321(9) Uani 1 1 d . . . . .
H35A H 0.643374 1.084825 0.266574 0.039 Uiso 1 1 calc R U . . .
H35B H 0.569181 1.051558 0.276072 0.039 Uiso 1 1 calc R U . . .
C50 C 0.4137(2) 1.0006(2) 0.18324(17) 0.0368(10) Uani 1 1 d . . . . .
H50 H 0.426664 1.051934 0.197686 0.044 Uiso 1 1 calc R U . . .
C40 C 0.5872(2) 0.7861(2) 0.14848(15) 0.0300(9) Uani 1 1 d . . . . .
H40 H 0.575730 0.840315 0.144018 0.036 Uiso 1 1 calc R U . . .
C12 C 0.3186(2) 0.4231(2) 0.00031(15) 0.0294(9) Uani 1 1 d . . . . .
H12A H 0.340439 0.370250 0.001274 0.035 Uiso 1 1 calc R U . . .
H12B H 0.275100 0.425814 -0.033366 0.035 Uiso 1 1 calc R U . . .
C60 C 0.6987(2) 0.9485(2) 0.63868(15) 0.0273(9) Uani 1 1 d . . . . .
H60 H 0.732885 0.955961 0.675054 0.033 Uiso 1 1 calc R U . . .
C34 C 0.6461(2) 1.0806(2) 0.35161(17) 0.0320(9) Uani 1 1 d . . . . .
H34A H 0.624588 1.133125 0.352695 0.038 Uiso 1 1 calc R U . . .
H34B H 0.700068 1.085946 0.364612 0.038 Uiso 1 1 calc R U . . .
C63 C 0.8644(2) 0.7716(2) 0.42838(15) 0.0335(9) Uani 1 1 d . . . . .
H63 H 0.864739 0.761059 0.390312 0.040 Uiso 1 1 calc R U . . .
C58 C 0.5895(2) 0.9822(2) 0.56792(17) 0.0303(9) Uani 1 1 d . . . . .
H58 H 0.546655 1.013185 0.554818 0.036 Uiso 1 1 calc R U . . .
C67 C 0.5115(2) 0.2491(2) 0.26175(18) 0.0381(10) Uani 1 1 d . . . . .
H67 H 0.533621 0.262107 0.232712 0.046 Uiso 1 1 calc R U . . .
C54 C 0.6702(2) 0.5477(2) 0.61448(15) 0.0322(9) Uani 1 1 d . . . . .
H54 H 0.662663 0.499897 0.631976 0.039 Uiso 1 1 calc R U . . .
C49 C 0.3860(2) 0.9879(2) 0.12575(18) 0.0395(11) Uani 1 1 d . . . . .
H49 H 0.378486 1.030470 0.099698 0.047 Uiso 1 1 calc R U . . .
C70 C 0.4507(2) 0.2128(3) 0.34529(17) 0.0385(10) Uani 1 1 d . . . . .
H70 H 0.429513 0.198139 0.374565 0.046 Uiso 1 1 calc R U . . .
C55 C 0.6854(2) 0.6160(2) 0.64558(16) 0.0356(10) Uani 1 1 d . . . . .
H55 H 0.688179 0.616277 0.685002 0.043 Uiso 1 1 calc R U . . .
C65 C 0.9248(2) 0.8016(2) 0.52466(16) 0.0325(10) Uani 1 1 d . . . . .
H65 H 0.967960 0.811640 0.554734 0.039 Uiso 1 1 calc R U . . .
C48 C 0.3694(2) 0.9130(2) 0.10646(17) 0.0377(10) Uani 1 1 d . . . . .
H48 H 0.350634 0.902618 0.066809 0.045 Uiso 1 1 calc R U . . .
C68 C 0.5111(2) 0.3051(2) 0.30183(18) 0.0367(10) Uani 1 1 d . . . . .
H68 H 0.532277 0.355226 0.300523 0.044 Uiso 1 1 calc R U . . .
C69 C 0.4793(2) 0.2867(3) 0.34371(18) 0.0416(11) Uani 1 1 d . . . . .
H69 H 0.476984 0.324621 0.371586 0.050 Uiso 1 1 calc R U . . .
C43 C 0.2334(3) 0.6598(4) 0.30120(19) 0.0582(15) Uani 1 1 d . . . . .
H43 H 0.218896 0.607747 0.306514 0.070 Uiso 1 1 calc R U . . .
C45 C 0.2135(3) 0.7964(4) 0.2990(2) 0.0648(18) Uani 1 1 d . . . . .
H45 H 0.184418 0.840521 0.302053 0.078 Uiso 1 1 calc R U . . .
C44 C 0.1912(3) 0.7218(5) 0.3071(2) 0.075(2) Uani 1 1 d . . . . .
H44 H 0.146919 0.713617 0.316830 0.090 Uiso 1 1 calc R U . . .
O2 O 0.62743(13) 0.75033(13) 0.43708(9) 0.0192(5) Uani 1 1 d . . . . .
O1 O 0.50410(12) 0.69192(12) 0.29132(8) 0.0140(5) Uani 1 1 d . . . . .
Li1 Li 0.4156(3) 0.7639(4) 0.2589(2) 0.0250(14) Uani 1 1 d . . . . .
Li2 Li 0.6921(3) 0.7817(3) 0.5088(2) 0.0213(12) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 Cl3 2.7767(8) . ?
U1 N5 2.495(3) . ?
U1 N4 2.594(3) . ?
U1 N3 2.490(3) . ?
U1 N6 2.581(3) . ?
U1 O2 1.852(2) . ?
U1 O1 1.951(2) . ?
U1 Li2 3.762(5) . ?
Y1 Cl2 2.6430(8) . ?
Y1 Cl1 2.5675(9) . ?
Y1 N1 2.358(3) . ?
Y1 N2 2.504(3) . ?
Y1 N7 2.537(3) . ?
Y1 O1 2.242(2) . ?
Cl3 Li1 2.702(6) . ?
Cl2 Li1 2.583(6) . ?
N5 C26 1.363(4) . ?
N5 C29 1.397(4) . ?
N4 C19 1.287(4) . ?
N4 C20 1.471(4) . ?
N3 C18 1.398(4) . ?
N3 C15 1.365(4) . ?
N6 C31 1.468(4) . ?
N6 C30 1.310(4) . ?
N1 C4 1.362(4) . ?
N1 C7 1.385(4) . ?
N8 C42 1.331(5) . ?
N8 C46 1.334(5) . ?
N8 Li1 2.043(7) . ?
N2 C9 1.492(4) . ?
N2 C8 1.290(4) . ?
N10 C52 1.338(4) . ?
N10 C56 1.343(4) . ?
N10 Li2 2.079(6) . ?
N7 C41 1.341(4) . ?
N7 C37 1.331(4) . ?
C26 C27 1.400(5) . ?
C26 C3 1.520(4) . ?
C29 C30 1.418(4) . ?
C29 C28 1.392(5) . ?
N12 C62 1.336(4) . ?
N12 C66 1.336(4) . ?
N12 Li2 2.081(7) . ?
C31 H31 1.0000 . ?
C31 C32 1.534(4) . ?
C31 C36 1.520(5) . ?
N11 C57 1.334(4) . ?
N11 C61 1.343(4) . ?
N11 Li2 2.072(6) . ?
C30 H30 0.9500 . ?
N9 C51 1.335(5) . ?
N9 C47 1.342(5) . ?
N9 Li1 2.166(6) . ?
C18 C19 1.421(5) . ?
C18 C17 1.378(4) . ?
C15 C3 1.515(5) . ?
C15 C16 1.389(4) . ?
C19 H19 0.9500 . ?
C20 H20 1.0000 . ?
C20 C25 1.524(4) . ?
C20 C21 1.530(5) . ?
C52 H52 0.9500 . ?
C52 C53 1.377(5) . ?
C27 H27 0.9500 . ?
C27 C28 1.384(5) . ?
C17 H17 0.9500 . ?
C17 C16 1.395(5) . ?
N13 C71 1.333(5) . ?
N13 C67 1.334(5) . ?
C4 C3 1.522(4) . ?
C4 C5 1.397(4) . ?
C28 H28 0.9500 . ?
C3 C2 1.555(4) . ?
C16 H16 0.9500 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.530(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C9 1.526(5) . ?
C14 C13 1.529(5) . ?
C9 H9 1.0000 . ?
C9 C10 1.514(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.522(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C24 1.522(5) . ?
C41 H41 0.9500 . ?
C41 C40 1.383(5) . ?
C7 C6 1.381(5) . ?
C7 C8 1.426(4) . ?
C37 H37 0.9500 . ?
C37 C38 1.380(5) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C23 1.525(5) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C35 1.535(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.529(5) . ?
C6 H6 0.9500 . ?
C6 C5 1.397(4) . ?
C8 H8 0.9500 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C22 1.527(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.519(5) . ?
C42 H42 0.9500 . ?
C42 C43 1.373(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.530(5) . ?
C71 H71 0.9500 . ?
C71 C70 1.374(6) . ?
C57 H57 0.9500 . ?
C57 C58 1.382(5) . ?
C38 H38 0.9500 . ?
C38 C39 1.376(6) . ?
C5 H5 0.9500 . ?
C59 H59 0.9500 . ?
C59 C60 1.367(5) . ?
C59 C58 1.382(5) . ?
C56 H56 0.9500 . ?
C56 C55 1.373(5) . ?
C61 H61 0.9500 . ?
C61 C60 1.382(5) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C12 1.515(5) . ?
C39 H39 0.9500 . ?
C39 C40 1.376(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.518(5) . ?
C64 H64 0.9500 . ?
C64 C63 1.377(5) . ?
C64 C65 1.386(5) . ?
C51 H51 0.9500 . ?
C51 C50 1.380(5) . ?
C53 H53 0.9500 . ?
C53 C54 1.380(5) . ?
C62 H62 0.9500 . ?
C62 C63 1.368(5) . ?
C46 H46 0.9500 . ?
C46 C45 1.379(7) . ?
C66 H66 0.9500 . ?
C66 C65 1.376(5) . ?
C47 H47 0.9500 . ?
C47 C48 1.381(5) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C34 1.517(5) . ?
C50 H50 0.9500 . ?
C50 C49 1.371(6) . ?
C40 H40 0.9500 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C60 H60 0.9500 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C63 H63 0.9500 . ?
C58 H58 0.9500 . ?
C67 H67 0.9500 . ?
C67 C68 1.370(6) . ?
C54 H54 0.9500 . ?
C54 C55 1.377(5) . ?
C49 H49 0.9500 . ?
C49 C48 1.367(6) . ?
C70 H70 0.9500 . ?
C70 C69 1.379(6) . ?
C55 H55 0.9500 . ?
C65 H65 0.9500 . ?
C48 H48 0.9500 . ?
C68 H68 0.9500 . ?
C68 C69 1.366(6) . ?
C69 H69 0.9500 . ?
C43 H43 0.9500 . ?
C43 C44 1.361(8) . ?
C45 H45 0.9500 . ?
C45 C44 1.374(8) . ?
C44 H44 0.9500 . ?
O2 Li2 1.911(6) . ?
O1 Li1 2.055(6) . ?

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
Cl3 U1 Li2 95.73(9) . . ?
N5 U1 Cl3 143.37(6) . . ?
N5 U1 N4 137.79(8) . . ?
N5 U1 N6 67.61(9) . . ?
N5 U1 Li2 94.29(11) . . ?
N4 U1 Cl3 77.30(6) . . ?
N4 U1 Li2 90.32(11) . . ?
N3 U1 Cl3 143.60(6) . . ?
N3 U1 N5 69.01(9) . . ?
N3 U1 N4 68.78(8) . . ?
N3 U1 N6 136.62(9) . . ?
N3 U1 Li2 97.25(10) . . ?
N6 U1 Cl3 77.99(6) . . ?
N6 U1 N4 154.59(9) . . ?
N6 U1 Li2 86.33(11) . . ?
O2 U1 Cl3 95.44(7) . . ?
O2 U1 N5 95.30(9) . . ?
O2 U1 N4 88.94(9) . . ?
O2 U1 N3 96.73(9) . . ?
O2 U1 N6 87.59(9) . . ?
O2 U1 O1 179.16(10) . . ?
O2 U1 Li2 1.38(12) . . ?
O1 U1 Cl3 83.99(6) . . ?
O1 U1 N5 85.52(8) . . ?
O1 U1 N4 90.33(9) . . ?
O1 U1 N3 83.40(9) . . ?
O1 U1 N6 92.89(8) . . ?
O1 U1 Li2 179.21(11) . . ?
Cl1 Y1 Cl2 87.91(3) . . ?
N1 Y1 Cl2 153.26(6) . . ?
N1 Y1 Cl1 97.96(7) . . ?
N1 Y1 N2 70.23(9) . . ?
N1 Y1 N7 85.55(9) . . ?
N2 Y1 Cl2 83.92(6) . . ?
N2 Y1 Cl1 88.71(7) . . ?
N2 Y1 N7 80.69(9) . . ?
N7 Y1 Cl2 83.56(7) . . ?
N7 Y1 Cl1 167.02(6) . . ?
O1 Y1 Cl2 77.07(5) . . ?
O1 Y1 Cl1 105.45(6) . . ?
O1 Y1 N1 125.42(8) . . ?
O1 Y1 N2 155.66(8) . . ?
O1 Y1 N7 82.19(8) . . ?
Li1 Cl3 U1 76.39(13) . . ?
Li1 Cl2 Y1 87.04(13) . . ?
C26 N5 U1 139.9(2) . . ?
C26 N5 C29 105.1(3) . . ?
C29 N5 U1 114.95(19) . . ?
C19 N4 U1 112.6(2) . . ?
C19 N4 C20 119.1(3) . . ?
C20 N4 U1 127.92(19) . . ?
C18 N3 U1 113.06(19) . . ?
C15 N3 U1 140.3(2) . . ?
C15 N3 C18 105.5(3) . . ?
C31 N6 U1 125.7(2) . . ?
C30 N6 U1 114.5(2) . . ?
C30 N6 C31 119.7(3) . . ?
C4 N1 Y1 139.0(2) . . ?
C4 N1 C7 105.5(3) . . ?
C7 N1 Y1 115.2(2) . . ?
C42 N8 C46 117.3(4) . . ?
C42 N8 Li1 122.1(3) . . ?
C46 N8 Li1 120.6(3) . . ?
C9 N2 Y1 129.4(2) . . ?
C8 N2 Y1 112.1(2) . . ?
C8 N2 C9 117.6(3) . . ?
C52 N10 C56 116.5(3) . . ?
C52 N10 Li2 110.6(3) . . ?
C56 N10 Li2 132.6(3) . . ?
C41 N7 Y1 119.7(2) . . ?
C37 N7 Y1 122.8(2) . . ?
C37 N7 C41 117.4(3) . . ?
N5 C26 C27 110.4(3) . . ?
N5 C26 C3 127.0(3) . . ?
C27 C26 C3 122.5(3) . . ?
N5 C29 C30 120.6(3) . . ?
C28 C29 N5 110.9(3) . . ?
C28 C29 C30 128.4(3) . . ?
C62 N12 Li2 118.6(3) . . ?
C66 N12 C62 116.2(3) . . ?
C66 N12 Li2 125.1(3) . . ?
N6 C31 H31 106.4 . . ?
N6 C31 C32 109.1(3) . . ?
N6 C31 C36 117.9(3) . . ?
C32 C31 H31 106.4 . . ?
C36 C31 H31 106.4 . . ?
C36 C31 C32 110.0(3) . . ?
C57 N11 C61 116.3(3) . . ?
C57 N11 Li2 129.4(3) . . ?
C61 N11 Li2 114.0(3) . . ?
N6 C30 C29 122.0(3) . . ?
N6 C30 H30 119.0 . . ?
C29 C30 H30 119.0 . . ?
C51 N9 C47 116.0(3) . . ?
C51 N9 Li1 124.6(3) . . ?
C47 N9 Li1 119.4(3) . . ?
N3 C18 C19 121.9(3) . . ?
C17 C18 N3 110.3(3) . . ?
C17 C18 C19 127.5(3) . . ?
N3 C15 C3 125.8(3) . . ?
N3 C15 C16 110.4(3) . . ?
C16 C15 C3 123.6(3) . . ?
N4 C19 C18 123.5(3) . . ?
N4 C19 H19 118.3 . . ?
C18 C19 H19 118.3 . . ?
N4 C20 H20 107.2 . . ?
N4 C20 C25 109.2(3) . . ?
N4 C20 C21 116.3(3) . . ?
C25 C20 H20 107.2 . . ?
C25 C20 C21 109.3(3) . . ?
C21 C20 H20 107.2 . . ?
N10 C52 H52 118.2 . . ?
N10 C52 C53 123.5(3) . . ?
C53 C52 H52 118.2 . . ?
C26 C27 H27 126.1 . . ?
C28 C27 C26 107.7(3) . . ?
C28 C27 H27 126.1 . . ?
C18 C17 H17 126.7 . . ?
C18 C17 C16 106.6(3) . . ?
C16 C17 H17 126.7 . . ?
C71 N13 C67 115.8(4) . . ?
N1 C4 C3 119.0(3) . . ?
N1 C4 C5 110.9(3) . . ?
C5 C4 C3 130.0(3) . . ?
C29 C28 H28 127.1 . . ?
C27 C28 C29 105.9(3) . . ?
C27 C28 H28 127.1 . . ?
C26 C3 C4 106.0(2) . . ?
C26 C3 C2 108.5(3) . . ?
C15 C3 C26 116.7(3) . . ?
C15 C3 C4 106.5(3) . . ?
C15 C3 C2 109.3(3) . . ?
C4 C3 C2 109.7(3) . . ?
C15 C16 C17 107.2(3) . . ?
C15 C16 H16 126.4 . . ?
C17 C16 H16 126.4 . . ?
C31 C32 H32A 109.6 . . ?
C31 C32 H32B 109.6 . . ?
H32A C32 H32B 108.1 . . ?
C33 C32 C31 110.3(3) . . ?
C33 C32 H32A 109.6 . . ?
C33 C32 H32B 109.6 . . ?
H14A C14 H14B 108.0 . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
C9 C14 C13 110.9(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
N2 C9 C14 113.7(3) . . ?
N2 C9 H9 106.8 . . ?
N2 C9 C10 110.5(3) . . ?
C14 C9 H9 106.8 . . ?
C10 C9 C14 111.7(3) . . ?
C10 C9 H9 106.8 . . ?
C3 C2 H2A 108.8 . . ?
C3 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
C1 C2 C3 113.7(3) . . ?
C1 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
C20 C25 H25A 109.3 . . ?
C20 C25 H25B 109.3 . . ?
H25A C25 H25B 107.9 . . ?
C24 C25 C20 111.7(3) . . ?
C24 C25 H25A 109.3 . . ?
C24 C25 H25B 109.3 . . ?
N7 C41 H41 118.4 . . ?
N7 C41 C40 123.1(4) . . ?
C40 C41 H41 118.4 . . ?
N1 C7 C8 119.4(3) . . ?
C6 C7 N1 110.6(3) . . ?
C6 C7 C8 130.0(3) . . ?
N7 C37 H37 118.6 . . ?
N7 C37 C38 122.9(4) . . ?
C38 C37 H37 118.6 . . ?
C25 C24 H24A 109.3 . . ?
C25 C24 H24B 109.3 . . ?
C25 C24 C23 111.6(3) . . ?
H24A C24 H24B 108.0 . . ?
C23 C24 H24A 109.3 . . ?
C23 C24 H24B 109.3 . . ?
C31 C36 H36A 110.0 . . ?
C31 C36 H36B 110.0 . . ?
C31 C36 C35 108.7(3) . . ?
H36A C36 H36B 108.3 . . ?
C35 C36 H36A 110.0 . . ?
C35 C36 H36B 110.0 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C20 C21 H21A 109.6 . . ?
C20 C21 H21B 109.6 . . ?
H21A C21 H21B 108.1 . . ?
C22 C21 C20 110.3(3) . . ?
C22 C21 H21A 109.6 . . ?
C22 C21 H21B 109.6 . . ?
C7 C6 H6 126.6 . . ?
C7 C6 C5 106.8(3) . . ?
C5 C6 H6 126.6 . . ?
N2 C8 C7 122.4(3) . . ?
N2 C8 H8 118.8 . . ?
C7 C8 H8 118.8 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C24 C23 C22 110.7(3) . . ?
H23A C23 H23B 108.1 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C32 C33 H33A 109.4 . . ?
C32 C33 H33B 109.4 . . ?
H33A C33 H33B 108.0 . . ?
C34 C33 C32 111.2(3) . . ?
C34 C33 H33A 109.4 . . ?
C34 C33 H33B 109.4 . . ?
N8 C42 H42 118.3 . . ?
N8 C42 C43 123.3(5) . . ?
C43 C42 H42 118.3 . . ?
C9 C10 H10A 109.3 . . ?
C9 C10 H10B 109.3 . . ?
C9 C10 C11 111.6(3) . . ?
H10A C10 H10B 108.0 . . ?
C11 C10 H10A 109.3 . . ?
C11 C10 H10B 109.3 . . ?
N13 C71 H71 117.8 . . ?
N13 C71 C70 124.4(4) . . ?
C70 C71 H71 117.8 . . ?
N11 C57 H57 118.2 . . ?
N11 C57 C58 123.6(3) . . ?
C58 C57 H57 118.2 . . ?
C37 C38 H38 120.4 . . ?
C39 C38 C37 119.3(4) . . ?
C39 C38 H38 120.4 . . ?
C4 C5 C6 106.2(3) . . ?
C4 C5 H5 126.9 . . ?
C6 C5 H5 126.9 . . ?
C60 C59 H59 120.5 . . ?
C60 C59 C58 118.9(4) . . ?
C58 C59 H59 120.5 . . ?
N10 C56 H56 118.2 . . ?
N10 C56 C55 123.6(3) . . ?
C55 C56 H56 118.2 . . ?
N11 C61 H61 118.1 . . ?
N11 C61 C60 123.9(3) . . ?
C60 C61 H61 118.1 . . ?
C21 C22 H22A 109.3 . . ?
C21 C22 H22B 109.3 . . ?
C23 C22 C21 111.6(3) . . ?
C23 C22 H22A 109.3 . . ?
C23 C22 H22B 109.3 . . ?
H22A C22 H22B 108.0 . . ?
C14 C13 H13A 109.4 . . ?
C14 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
C12 C13 C14 111.4(3) . . ?
C12 C13 H13A 109.4 . . ?
C12 C13 H13B 109.4 . . ?
C38 C39 H39 120.7 . . ?
C40 C39 C38 118.6(4) . . ?
C40 C39 H39 120.7 . . ?
C10 C11 H11A 109.4 . . ?
C10 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 C10 111.1(3) . . ?
C12 C11 H11A 109.4 . . ?
C12 C11 H11B 109.4 . . ?
C63 C64 H64 121.2 . . ?
C63 C64 C65 117.7(4) . . ?
C65 C64 H64 121.2 . . ?
N9 C51 H51 118.0 . . ?
N9 C51 C50 124.0(3) . . ?
C50 C51 H51 118.0 . . ?
C52 C53 H53 120.5 . . ?
C52 C53 C54 119.0(3) . . ?
C54 C53 H53 120.5 . . ?
N12 C62 H62 118.1 . . ?
N12 C62 C63 123.9(3) . . ?
C63 C62 H62 118.1 . . ?
N8 C46 H46 118.6 . . ?
N8 C46 C45 122.8(5) . . ?
C45 C46 H46 118.6 . . ?
N12 C66 H66 118.1 . . ?
N12 C66 C65 123.9(3) . . ?
C65 C66 H66 118.1 . . ?
N9 C47 H47 118.1 . . ?
N9 C47 C48 123.7(4) . . ?
C48 C47 H47 118.1 . . ?
C36 C35 H35A 109.2 . . ?
C36 C35 H35B 109.2 . . ?
H35A C35 H35B 107.9 . . ?
C34 C35 C36 112.1(3) . . ?
C34 C35 H35A 109.2 . . ?
C34 C35 H35B 109.2 . . ?
C51 C50 H50 120.7 . . ?
C49 C50 C51 118.5(4) . . ?
C49 C50 H50 120.7 . . ?
C41 C40 H40 120.7 . . ?
C39 C40 C41 118.7(4) . . ?
C39 C40 H40 120.7 . . ?
C13 C12 C11 110.9(3) . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C59 C60 C61 118.5(3) . . ?
C59 C60 H60 120.7 . . ?
C61 C60 H60 120.7 . . ?
C33 C34 H34A 109.3 . . ?
C33 C34 H34B 109.3 . . ?
C35 C34 C33 111.6(3) . . ?
C35 C34 H34A 109.3 . . ?
C35 C34 H34B 109.3 . . ?
H34A C34 H34B 108.0 . . ?
C64 C63 H63 120.3 . . ?
C62 C63 C64 119.5(3) . . ?
C62 C63 H63 120.3 . . ?
C57 C58 C59 118.6(3) . . ?
C57 C58 H58 120.7 . . ?
C59 C58 H58 120.7 . . ?
N13 C67 H67 117.7 . . ?
N13 C67 C68 124.5(4) . . ?
C68 C67 H67 117.7 . . ?
C53 C54 H54 120.8 . . ?
C55 C54 C53 118.3(3) . . ?
C55 C54 H54 120.8 . . ?
C50 C49 H49 120.5 . . ?
C48 C49 C50 119.1(4) . . ?
C48 C49 H49 120.5 . . ?
C71 C70 H70 121.2 . . ?
C71 C70 C69 117.6(4) . . ?
C69 C70 H70 121.2 . . ?
C56 C55 C54 119.1(3) . . ?
C56 C55 H55 120.5 . . ?
C54 C55 H55 120.5 . . ?
C64 C65 H65 120.6 . . ?
C66 C65 C64 118.9(3) . . ?
C66 C65 H65 120.6 . . ?
C47 C48 H48 120.7 . . ?
C49 C48 C47 118.6(4) . . ?
C49 C48 H48 120.7 . . ?
C67 C68 H68 121.0 . . ?
C69 C68 C67 118.0(4) . . ?
C69 C68 H68 121.0 . . ?
C70 C69 H69 120.2 . . ?
C68 C69 C70 119.6(4) . . ?
C68 C69 H69 120.2 . . ?
C42 C43 H43 120.6 . . ?
C44 C43 C42 118.8(5) . . ?
C44 C43 H43 120.6 . . ?
C46 C45 H45 120.7 . . ?
C44 C45 C46 118.5(5) . . ?
C44 C45 H45 120.7 . . ?
C43 C44 C45 119.2(5) . . ?
C43 C44 H44 120.4 . . ?
C45 C44 H44 120.4 . . ?
U1 O2 Li2 177.3(2) . . ?
U1 O1 Y1 129.75(10) . . ?
U1 O1 Li1 115.5(2) . . ?
Li1 O1 Y1 113.7(2) . . ?
Cl2 Li1 Cl3 165.6(3) . . ?
N8 Li1 Cl3 91.4(2) . . ?
N8 Li1 Cl2 93.5(2) . . ?
N8 Li1 N9 111.4(3) . . ?
N8 Li1 O1 120.0(3) . . ?
N9 Li1 Cl3 94.8(2) . . ?
N9 Li1 Cl2 96.0(2) . . ?
O1 Li1 Cl3 84.1(2) . . ?
O1 Li1 Cl2 81.7(2) . . ?
O1 Li1 N9 128.5(3) . . ?
N10 Li2 U1 105.4(2) . . ?
N10 Li2 N12 108.6(3) . . ?
N12 Li2 U1 103.3(2) . . ?
N11 Li2 U1 119.0(2) . . ?
N11 Li2 N10 104.6(3) . . ?
N11 Li2 N12 115.2(3) . . ?
O2 Li2 U1 1.34(11) . . ?
O2 Li2 N10 104.4(3) . . ?
O2 Li2 N12 104.6(3) . . ?
O2 Li2 N11 118.6(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 N5 C26 C27 176.7(2) . . . . ?
U1 N5 C26 C3 1.0(5) . . . . ?
U1 N5 C29 C30 5.6(3) . . . . ?
U1 N5 C29 C28 -177.9(2) . . . . ?
U1 N4 C19 C18 -1.6(4) . . . . ?
U1 N4 C20 C25 -67.9(3) . . . . ?
U1 N4 C20 C21 167.9(2) . . . . ?
U1 N3 C18 C19 3.8(4) . . . . ?
U1 N3 C18 C17 -171.5(2) . . . . ?
U1 N3 C15 C3 -17.5(5) . . . . ?
U1 N3 C15 C16 166.9(2) . . . . ?
U1 N6 C31 C32 67.1(3) . . . . ?
U1 N6 C31 C36 -166.6(2) . . . . ?
U1 N6 C30 C29 -3.7(4) . . . . ?
Y1 N1 C4 C3 -9.8(5) . . . . ?
Y1 N1 C4 C5 173.2(2) . . . . ?
Y1 N1 C7 C6 -174.9(2) . . . . ?
Y1 N1 C7 C8 5.7(4) . . . . ?
Y1 N2 C9 C14 141.9(3) . . . . ?
Y1 N2 C9 C10 -91.5(3) . . . . ?
Y1 N2 C8 C7 -7.5(4) . . . . ?
Y1 N7 C41 C40 -174.5(3) . . . . ?
Y1 N7 C37 C38 173.9(3) . . . . ?
N5 C26 C27 C28 0.7(4) . . . . ?
N5 C26 C3 C15 -3.6(4) . . . . ?
N5 C26 C3 C4 114.7(3) . . . . ?
N5 C26 C3 C2 -127.5(3) . . . . ?
N5 C29 C30 N6 -1.3(5) . . . . ?
N5 C29 C28 C27 0.3(4) . . . . ?
N4 C20 C25 C24 174.0(3) . . . . ?
N4 C20 C21 C22 -177.6(3) . . . . ?
N3 C18 C19 N4 -1.6(5) . . . . ?
N3 C18 C17 C16 1.0(4) . . . . ?
N3 C15 C3 C26 10.8(4) . . . . ?
N3 C15 C3 C4 -107.3(3) . . . . ?
N3 C15 C3 C2 134.4(3) . . . . ?
N3 C15 C16 C17 -0.4(4) . . . . ?
N6 C31 C32 C33 -169.2(3) . . . . ?
N6 C31 C36 C35 174.1(3) . . . . ?
N1 C4 C3 C26 -62.8(4) . . . . ?
N1 C4 C3 C15 62.1(4) . . . . ?
N1 C4 C3 C2 -179.8(3) . . . . ?
N1 C4 C5 C6 -0.6(4) . . . . ?
N1 C7 C6 C5 -0.2(4) . . . . ?
N1 C7 C8 N2 1.7(5) . . . . ?
N8 C42 C43 C44 0.6(7) . . . . ?
N8 C46 C45 C44 1.9(7) . . . . ?
N2 C9 C10 C11 178.2(3) . . . . ?
N10 C52 C53 C54 1.7(6) . . . . ?
N10 C56 C55 C54 1.8(7) . . . . ?
N7 C41 C40 C39 -0.1(6) . . . . ?
N7 C37 C38 C39 1.1(6) . . . . ?
C26 N5 C29 C30 -176.3(3) . . . . ?
C26 N5 C29 C28 0.2(3) . . . . ?
C26 C27 C28 C29 -0.6(4) . . . . ?
C26 C3 C2 C1 65.6(4) . . . . ?
C29 N5 C26 C27 -0.5(3) . . . . ?
C29 N5 C26 C3 -176.2(3) . . . . ?
N12 C62 C63 C64 1.0(6) . . . . ?
N12 C66 C65 C64 0.6(6) . . . . ?
C31 N6 C30 C29 173.6(3) . . . . ?
C31 C32 C33 C34 -55.8(4) . . . . ?
C31 C36 C35 C34 57.7(4) . . . . ?
N11 C57 C58 C59 0.6(6) . . . . ?
N11 C61 C60 C59 0.7(6) . . . . ?
C30 N6 C31 C32 -109.8(3) . . . . ?
C30 N6 C31 C36 16.5(4) . . . . ?
C30 C29 C28 C27 176.4(3) . . . . ?
N9 C51 C50 C49 1.2(6) . . . . ?
N9 C47 C48 C49 0.4(7) . . . . ?
C18 N3 C15 C3 176.5(3) . . . . ?
C18 N3 C15 C16 0.9(3) . . . . ?
C18 C17 C16 C15 -0.4(4) . . . . ?
C15 N3 C18 C19 174.2(3) . . . . ?
C15 N3 C18 C17 -1.2(3) . . . . ?
C15 C3 C2 C1 -62.7(4) . . . . ?
C19 N4 C20 C25 104.4(3) . . . . ?
C19 N4 C20 C21 -19.8(4) . . . . ?
C19 C18 C17 C16 -174.0(3) . . . . ?
C20 N4 C19 C18 -175.0(3) . . . . ?
C20 C25 C24 C23 56.0(4) . . . . ?
C20 C21 C22 C23 -57.8(4) . . . . ?
C52 N10 C56 C55 -1.4(6) . . . . ?
C52 C53 C54 C55 -1.1(6) . . . . ?
C27 C26 C3 C15 -178.7(3) . . . . ?
C27 C26 C3 C4 -60.4(4) . . . . ?
C27 C26 C3 C2 57.3(4) . . . . ?
C17 C18 C19 N4 172.9(3) . . . . ?
N13 C71 C70 C69 -0.1(6) . . . . ?
N13 C67 C68 C69 0.1(7) . . . . ?
C4 N1 C7 C6 -0.2(4) . . . . ?
C4 N1 C7 C8 -179.6(3) . . . . ?
C4 C3 C2 C1 -179.0(3) . . . . ?
C28 C29 C30 N6 -177.1(3) . . . . ?
C3 C26 C27 C28 176.6(3) . . . . ?
C3 C15 C16 C17 -176.0(3) . . . . ?
C3 C4 C5 C6 -177.2(3) . . . . ?
C16 C15 C3 C26 -174.3(3) . . . . ?
C16 C15 C3 C4 67.7(4) . . . . ?
C16 C15 C3 C2 -50.7(4) . . . . ?
C32 C31 C36 C35 -60.1(4) . . . . ?
C32 C33 C34 C35 53.1(4) . . . . ?
C14 C9 C10 C11 -54.1(4) . . . . ?
C14 C13 C12 C11 56.7(4) . . . . ?
C9 N2 C8 C7 -177.6(3) . . . . ?
C9 C14 C13 C12 -55.6(4) . . . . ?
C9 C10 C11 C12 54.9(4) . . . . ?
C25 C20 C21 C22 58.3(3) . . . . ?
C25 C24 C23 C22 -53.6(4) . . . . ?
C41 N7 C37 C38 -2.0(5) . . . . ?
C7 N1 C4 C3 177.5(3) . . . . ?
C7 N1 C4 C5 0.5(4) . . . . ?
C7 C6 C5 C4 0.5(4) . . . . ?
C37 N7 C41 C40 1.4(5) . . . . ?
C37 C38 C39 C40 0.3(6) . . . . ?
C24 C23 C22 C21 55.0(4) . . . . ?
C36 C31 C32 C33 60.1(4) . . . . ?
C36 C35 C34 C33 -54.5(4) . . . . ?
C21 C20 C25 C24 -57.8(4) . . . . ?
C6 C7 C8 N2 -177.6(4) . . . . ?
C8 N2 C9 C14 -50.0(4) . . . . ?
C8 N2 C9 C10 76.5(4) . . . . ?
C8 C7 C6 C5 179.1(4) . . . . ?
C42 N8 C46 C45 -1.0(6) . . . . ?
C42 C43 C44 C45 0.2(7) . . . . ?
C10 C11 C12 C13 -56.0(4) . . . . ?
C71 N13 C67 C68 -1.7(6) . . . . ?
C71 C70 C69 C68 -1.6(6) . . . . ?
C57 N11 C61 C60 0.1(5) . . . . ?
C38 C39 C40 C41 -0.8(6) . . . . ?
C5 C4 C3 C26 113.5(4) . . . . ?
C5 C4 C3 C15 -121.6(4) . . . . ?
C5 C4 C3 C2 -3.5(5) . . . . ?
C56 N10 C52 C53 -0.4(5) . . . . ?
C61 N11 C57 C58 -0.7(5) . . . . ?
C13 C14 C9 N2 -179.8(3) . . . . ?
C13 C14 C9 C10 54.3(4) . . . . ?
C51 N9 C47 C48 -0.5(6) . . . . ?
C51 C50 C49 C48 -1.4(7) . . . . ?
C53 C54 C55 C56 -0.5(6) . . . . ?
C62 N12 C66 C65 0.2(5) . . . . ?
C46 N8 C42 C43 -0.3(6) . . . . ?
C46 C45 C44 C43 -1.4(7) . . . . ?
C66 N12 C62 C63 -1.0(6) . . . . ?
C47 N9 C51 C50 -0.3(6) . . . . ?
C50 C49 C48 C47 0.6(7) . . . . ?
C60 C59 C58 C57 0.2(6) . . . . ?
C63 C64 C65 C66 -0.6(6) . . . . ?
C58 C59 C60 C61 -0.8(6) . . . . ?
C67 N13 C71 C70 1.7(6) . . . . ?
C67 C68 C69 C70 1.7(6) . . . . ?
C65 C64 C63 C62 -0.1(6) . . . . ?
Li1 N8 C42 C43 -179.6(4) . . . . ?
Li1 N8 C46 C45 178.4(4) . . . . ?
Li1 N9 C51 C50 -177.4(4) . . . . ?
Li1 N9 C47 C48 176.8(4) . . . . ?
Li2 N10 C52 C53 -174.7(4) . . . . ?
Li2 N10 C56 C55 171.3(4) . . . . ?
Li2 N12 C62 C63 -177.9(4) . . . . ?
Li2 N12 C66 C65 176.9(3) . . . . ?
Li2 N11 C57 C58 173.4(3) . . . . ?
Li2 N11 C61 C60 -175.0(3) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 156 electrons were 
found in a volume of 910Å³ in 4 voids per unit cell. 
This is consistent with the presence of 
1[C5H5N] per Formula Unit 
which account for 168 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 0.500 365.1 78.4 '2 pyridine'
2 0.180 0.048 0.624 13.2 0.0 ?
3 0.192 0.237 0.859 23.2 0.0 ?
4 0.222 0.487 0.261 9.2 0.0 ?
5 0.278 -0.013 0.239 9.2 0.0 ?
6 0.308 0.737 0.641 23.2 0.0 ?
7 0.500 0.000 0.000 365.1 78.4 '2 pyridine'
8 0.320 0.548 0.876 13.2 0.0 ?
9 0.692 0.263 0.359 23.2 0.0 ?
10 0.680 0.452 0.124 13.2 0.0 ?
11 0.722 0.013 0.761 9.2 0.0 ?
12 0.778 0.513 0.739 9.2 0.0 ?
13 0.808 0.763 0.141 23.2 0.0 ?
14 0.820 0.952 0.376 13.2 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.263
_oxdiff_exptl_absorpt_empirical_full_min 0.705
_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_to509_refinalised
_database_code_depnum_ccdc_archive 'CCDC 2313508'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2023-12-11 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_audit_creation_date             2023-11-24
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C66 H77 Cl3 Dy Li2 N12 O2 U, 2(C5 H5 N)'
_chemical_formula_sum            'C76 H87 Cl3 Dy Li2 N14 O2 U'
_chemical_formula_weight         1749.35
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C36 H47 N6 U O2 Dy Li2 Cl3'
_chemical_oxdiff_usercomment     Pyr/hex
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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   19.0653(4)
_cell_length_b                   17.0891(3)
_cell_length_c                   24.4481(5)
_cell_angle_alpha                90
_cell_angle_beta                 106.566(2)
_cell_angle_gamma                90
_cell_volume                     7634.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    21649
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.5940
_cell_measurement_theta_min      3.5370
_shelx_estimated_absorpt_T_max   0.829
_shelx_estimated_absorpt_T_min   0.318
_exptl_absorpt_coefficient_mu    3.249
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_correction_T_min  0.224
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3488
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 23 9 0.1059
-11 16 -17 0.2107
-12 5 -24 0.1959
2 -24 -5 0.1093
-24 -3 23 0.0115
25 3 -22 0.0394
13 -3 24 0.2437

_exptl_crystal_preparation       
'Vapour diffusion of hexane into pyridine solution'
_exptl_crystal_size_max          0.457
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.06
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.2846 23.1391 9.0700 -0.0236 -0.9315 0.3630
-10.5377 16.4041 -16.5877 -0.0202 -0.7641 -0.6448
-12.1526 4.9591 -24.2335 -0.0090 -0.3176 -0.9482
1.5794 -23.7972 -5.3155 0.0249 0.9761 -0.2161
-24.0729 -2.8242 22.9849 0.9996 -0.0257 -0.0089
24.5199 2.9337 -21.8960 -0.9984 0.0257 0.0505
12.6853 -2.9539 24.2102 -0.0181 0.2394 0.9707

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0738
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            79648
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.901
_diffrn_reflns_theta_min         3.335
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -35.00  55.00   1.00   15.00    --  -14.44  34.00 -95.00   90
  2  ω    -53.00  36.00   1.00   15.00    --   16.16 -34.00 106.00   89
  3  ω    -87.00 -39.00   1.00   15.00    --  -14.44-178.00 -90.00   48
  4  ω    -11.00  39.00   1.00   15.00    --   16.16  77.00   0.00   50
  5  ω    -11.00  39.00   1.00   15.00    --   16.16  77.00 120.00   50
  6  ω    -51.00  33.00   1.00   15.00    --   16.16 -57.00  60.00   84
  7  ω     -1.00  83.00   1.00   15.00    --   16.16  57.00-150.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0281516000
_diffrn_orient_matrix_UB_12      -0.0058810000
_diffrn_orient_matrix_UB_13      0.0132839000
_diffrn_orient_matrix_UB_21      0.0070274000
_diffrn_orient_matrix_UB_22      -0.0408235000
_diffrn_orient_matrix_UB_23      0.0012268000
_diffrn_orient_matrix_UB_31      0.0257625000
_diffrn_orient_matrix_UB_32      0.0047192000
_diffrn_orient_matrix_UB_33      0.0271736000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13292
_reflns_number_total             17518
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.362
_refine_diff_density_min         -1.258
_refine_diff_density_rms         0.159
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     893
_refine_ls_number_reflns         17518
_refine_ls_number_restraints     100
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0420
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0231P)²+10.4983P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0790
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N14-C72 = N14-C76
 1.33 with sigma of 0.02
 C72-C73 = C75-C76
 1.38 with sigma of 0.02
 C73-C74 = C74-C75
 1.37 with sigma of 0.02
 N14-C75
 2.39 with sigma of 0.04
 C73-C75
 2.35 with sigma of 0.04
 C72-C74
 2.36 with sigma of 0.04
 C74-C76
 2.37 with sigma of 0.04
 N14-C73
 2.4 with sigma of 0.04
 N14-C72 \\sim N14-C76
 with sigma of 0.02
 C72-C73 \\sim C73-C74 \\sim C74-C75 \\sim C75-C76
 with sigma of 0.02
 N14-C75 \\sim N14-C73
 with sigma of 0.04
 C74-C76 \\sim C74-C72 \\sim C75-C73 \\sim C76-C72
 with sigma of 0.04
3. Restrained planarity
 N14, C72, C73, C74, C75, C76
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N14 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 N14, C72, C73, C74, C75, C76
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Ternary CH refined with riding coordinates:
 C31(H31), C20(H20), C9(H9)
6.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C2(H2A,H2B), C36(H36A,H36B), C24(H24A,H24B), C21(H21A,H21B),
 C14(H14A,H14B), C23(H23A,H23B), C32(H32A,H32B), C22(H22A,H22B), C10(H10A,H10B),
  C35(H35A,H35B), C33(H33A,H33B), C11(H11A,H11B), C13(H13A,H13B), C12(H12A,
 H12B), C34(H34A,H34B)
6.c Aromatic/amide H refined with riding coordinates:
 C30(H30), C19(H19), C41(H41), C17(H17), C28(H28), C27(H27), C16(H16),
 C37(H37), C8(H8), C57(H57), C61(H61), C5(H5), C66(H66), C51(H51), C62(H62),
 C67(H67), C40(H40), C6(H6), C68(H68), C39(H39), C71(H71), C52(H52), C38(H38),
 C54(H54), C56(H56), C46(H46), C58(H58), C60(H60), C65(H65), C47(H47), C70(H70),
  C42(H42), C59(H59), C63(H63), C55(H55), C64(H64), C44(H44), C45(H45),
 C53(H53), C43(H43), C69(H69), C50(H50), C48(H48), C49(H49), C72(H72), C73(H73),
  C74(H74), C75(H75), C76(H76)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.43198(2) 0.22235(2) 0.63379(2) 0.01158(5) Uani 1 1 d . . . . .
Dy1 Dy 0.49923(2) 0.08005(2) 0.75634(2) 0.01523(6) Uani 1 1 d . . . . .
Cl3 Cl 0.52686(6) 0.34787(6) 0.64329(5) 0.0203(2) Uani 1 1 d . . . . .
Cl2 Cl 0.61355(6) 0.15907(7) 0.82011(4) 0.0218(3) Uani 1 1 d . . . . .
Cl1 Cl 0.59154(7) -0.00889(7) 0.72672(5) 0.0279(3) Uani 1 1 d . . . . .
N5 N 0.3311(2) 0.1679(2) 0.66930(14) 0.0141(8) Uani 1 1 d . . . . .
N4 N 0.5276(2) 0.1697(2) 0.58570(14) 0.0159(8) Uani 1 1 d . . . . .
N3 N 0.4211(2) 0.0776(2) 0.62001(14) 0.0150(8) Uani 1 1 d . . . . .
N6 N 0.3667(2) 0.3284(2) 0.67651(14) 0.0173(8) Uani 1 1 d . . . . .
N7 N 0.4298(2) 0.1620(2) 0.81127(14) 0.0204(9) Uani 1 1 d . . . . .
N1 N 0.4033(2) -0.0111(2) 0.74513(14) 0.0150(8) Uani 1 1 d . . . . .
C29 C 0.2984(2) 0.2225(2) 0.69699(16) 0.0134(9) Uani 1 1 d . . . . .
N9 N 0.6791(2) 0.2459(2) 0.71986(16) 0.0261(10) Uani 1 1 d . . . . .
C26 C 0.2970(2) 0.0988(2) 0.67242(17) 0.0152(10) Uani 1 1 d . . . . .
C15 C 0.3747(2) 0.0175(2) 0.62172(16) 0.0148(10) Uani 1 1 d . . . . .
N2 N 0.5186(2) -0.0029(2) 0.84485(14) 0.0195(9) Uani 1 1 d . . . . .
N10 N 0.3084(2) 0.1876(2) 0.43678(15) 0.0222(9) Uani 1 1 d . . . . .
N12 N 0.2052(2) 0.2872(2) 0.50526(15) 0.0194(9) Uani 1 1 d . . . . .
N11 N 0.3353(2) 0.3776(2) 0.44978(15) 0.0214(9) Uani 1 1 d . . . . .
C30 C 0.3178(2) 0.3029(3) 0.69922(17) 0.0161(10) Uani 1 1 d . . . . .
H30 H 0.294144 0.338755 0.717855 0.019 Uiso 1 1 calc R U . . .
C18 C 0.4691(2) 0.0476(2) 0.59124(17) 0.0151(10) Uani 1 1 d . . . . .
C19 C 0.5211(2) 0.0958(2) 0.57596(17) 0.0156(10) Uani 1 1 d . . . . .
H19 H 0.553151 0.071908 0.557403 0.019 Uiso 1 1 calc R U . . .
N8 N 0.5928(2) 0.3638(2) 0.79718(16) 0.0254(10) Uani 1 1 d . . . . .
C4 C 0.3407(2) -0.0321(2) 0.70431(17) 0.0140(9) Uani 1 1 d . . . . .
C3 C 0.3146(2) 0.0196(2) 0.65138(17) 0.0155(10) Uani 1 1 d . . . . .
C41 C 0.4436(3) 0.2387(3) 0.81913(19) 0.0234(11) Uani 1 1 d . . . . .
H41 H 0.476558 0.262069 0.801197 0.028 Uiso 1 1 calc R U . . .
C31 C 0.3799(3) 0.4136(2) 0.67444(17) 0.0168(10) Uani 1 1 d . . . . .
H31 H 0.434208 0.420646 0.686120 0.020 Uiso 1 1 calc R U . . .
N13 N 0.5169(3) -0.3225(3) 0.7381(2) 0.0402(12) Uani 1 1 d . . . . .
C7 C 0.4111(3) -0.0661(3) 0.78802(17) 0.0185(10) Uani 1 1 d . . . . .
C20 C 0.5797(2) 0.2150(2) 0.56366(17) 0.0156(10) Uani 1 1 d . . . . .
H20 H 0.604184 0.253355 0.593989 0.019 Uiso 1 1 calc R U . . .
C17 C 0.4529(2) -0.0295(2) 0.57658(17) 0.0168(10) Uani 1 1 d . . . . .
H17 H 0.477706 -0.063144 0.557336 0.020 Uiso 1 1 calc R U . . .
C9 C 0.5813(3) -0.0041(3) 0.89743(17) 0.0198(11) Uani 1 1 d . . . . .
H9 H 0.605371 0.048342 0.900263 0.024 Uiso 1 1 calc R U . . .
C25 C 0.5372(3) 0.2622(3) 0.51199(19) 0.0209(11) Uani 1 1 d . . . . .
H25A H 0.498767 0.292980 0.522147 0.025 Uiso 1 1 calc R U . . .
H25B H 0.512886 0.225947 0.480759 0.025 Uiso 1 1 calc R U . . .
C28 C 0.2454(3) 0.1864(3) 0.71711(18) 0.0191(10) Uani 1 1 d . . . . .
H28 H 0.215678 0.210436 0.737596 0.023 Uiso 1 1 calc R U . . .
C27 C 0.2444(3) 0.1087(3) 0.70153(18) 0.0204(10) Uani 1 1 d . . . . .
H27 H 0.213485 0.069091 0.709203 0.025 Uiso 1 1 calc R U . . .
C16 C 0.3927(3) -0.0484(3) 0.59564(17) 0.0194(10) Uani 1 1 d . . . . .
H16 H 0.368426 -0.097512 0.591493 0.023 Uiso 1 1 calc R U . . .
C37 C 0.3828(3) 0.1308(3) 0.83615(19) 0.0262(12) Uani 1 1 d . . . . .
H37 H 0.371608 0.076663 0.830698 0.031 Uiso 1 1 calc R U . . .
C8 C 0.4720(3) -0.0592(3) 0.83805(18) 0.0207(11) Uani 1 1 d . . . . .
H8 H 0.478243 -0.097423 0.867258 0.025 Uiso 1 1 calc R U . . .
C2 C 0.2436(2) -0.0152(3) 0.61087(17) 0.0188(10) Uani 1 1 d . . . . .
H2A H 0.253659 -0.069308 0.600728 0.023 Uiso 1 1 calc R U . . .
H2B H 0.205878 -0.018072 0.631527 0.023 Uiso 1 1 calc R U . . .
C57 C 0.3245(3) 0.1210(3) 0.46610(19) 0.0242(11) Uani 1 1 d . . . . .
H57 H 0.329581 0.122387 0.505883 0.029 Uiso 1 1 calc R U . . .
C36 C 0.3524(3) 0.4420(3) 0.61300(19) 0.0259(12) Uani 1 1 d . . . . .
H36A H 0.298236 0.439637 0.600143 0.031 Uiso 1 1 calc R U . . .
H36B H 0.371318 0.407367 0.587982 0.031 Uiso 1 1 calc R U . . .
C24 C 0.5871(3) 0.3176(3) 0.4912(2) 0.0252(11) Uani 1 1 d . . . . .
H24A H 0.558167 0.345041 0.456390 0.030 Uiso 1 1 calc R U . . .
H24B H 0.607445 0.357410 0.520858 0.030 Uiso 1 1 calc R U . . .
C1 C 0.2128(3) 0.0316(3) 0.55597(18) 0.0273(12) Uani 1 1 d . . . . .
H1A H 0.166996 0.007645 0.533397 0.041 Uiso 1 1 calc R U . . .
H1B H 0.248309 0.031510 0.533797 0.041 Uiso 1 1 calc R U . . .
H1C H 0.203506 0.085530 0.565519 0.041 Uiso 1 1 calc R U . . .
C61 C 0.3022(3) 0.1833(3) 0.38076(19) 0.0304(13) Uani 1 1 d . . . . .
H61 H 0.289650 0.229451 0.358441 0.037 Uiso 1 1 calc R U . . .
C5 C 0.3097(3) -0.0986(3) 0.72069(18) 0.0205(11) Uani 1 1 d . . . . .
H5 H 0.266376 -0.124571 0.699537 0.025 Uiso 1 1 calc R U . . .
C21 C 0.6400(2) 0.1689(3) 0.54856(18) 0.0184(10) Uani 1 1 d . . . . .
H21A H 0.617823 0.131084 0.517792 0.022 Uiso 1 1 calc R U . . .
H21B H 0.668237 0.138963 0.582349 0.022 Uiso 1 1 calc R U . . .
C66 C 0.3944(3) 0.4231(3) 0.4662(2) 0.0248(11) Uani 1 1 d . . . . .
H66 H 0.427360 0.414875 0.503074 0.030 Uiso 1 1 calc R U . . .
C51 C 0.7023(3) 0.1744(3) 0.7127(2) 0.0355(13) Uani 1 1 d . . . . .
H51 H 0.673282 0.131069 0.717226 0.043 Uiso 1 1 calc R U . . .
C14 C 0.6378(3) -0.0640(3) 0.89254(19) 0.0283(12) Uani 1 1 d . . . . .
H14A H 0.654280 -0.052179 0.858528 0.034 Uiso 1 1 calc R U . . .
H14B H 0.615194 -0.116665 0.887338 0.034 Uiso 1 1 calc R U . . .
C23 C 0.6494(3) 0.2730(3) 0.47799(19) 0.0247(11) Uani 1 1 d . . . . .
H23A H 0.683377 0.310607 0.468075 0.030 Uiso 1 1 calc R U . . .
H23B H 0.629436 0.238562 0.444623 0.030 Uiso 1 1 calc R U . . .
C32 C 0.3508(3) 0.4663(3) 0.7136(2) 0.0266(12) Uani 1 1 d . . . . .
H32A H 0.368671 0.447579 0.753485 0.032 Uiso 1 1 calc R U . . .
H32B H 0.296633 0.465077 0.701921 0.032 Uiso 1 1 calc R U . . .
C62 C 0.2897(3) 0.3913(3) 0.39781(19) 0.0229(11) Uani 1 1 d . . . . .
H62 H 0.247121 0.359735 0.385288 0.028 Uiso 1 1 calc R U . . .
C22 C 0.6913(3) 0.2236(3) 0.5289(2) 0.0244(11) Uani 1 1 d . . . . .
H22A H 0.729018 0.192275 0.518111 0.029 Uiso 1 1 calc R U . . .
H22B H 0.716549 0.258473 0.560787 0.029 Uiso 1 1 calc R U . . .
C10 C 0.5593(3) -0.0153(3) 0.95201(18) 0.0288(12) Uani 1 1 d . . . . .
H10A H 0.533108 -0.065704 0.950154 0.035 Uiso 1 1 calc R U . . .
H10B H 0.525552 0.027138 0.955496 0.035 Uiso 1 1 calc R U . . .
C67 C 0.5460(3) -0.3385(3) 0.6961(2) 0.0404(15) Uani 1 1 d . . . . .
H67 H 0.565251 -0.389478 0.694733 0.049 Uiso 1 1 calc R U . . .
C35 C 0.3778(3) 0.5265(3) 0.6082(2) 0.0299(12) Uani 1 1 d . . . . .
H35A H 0.431786 0.527757 0.617307 0.036 Uiso 1 1 calc R U . . .
H35B H 0.357197 0.545248 0.568533 0.036 Uiso 1 1 calc R U . . .
C40 C 0.4126(3) 0.2856(3) 0.8519(2) 0.0308(12) Uani 1 1 d . . . . .
H40 H 0.424091 0.339754 0.856448 0.037 Uiso 1 1 calc R U . . .
C6 C 0.3548(3) -0.1197(3) 0.77418(19) 0.0231(11) Uani 1 1 d . . . . .
H6 H 0.347962 -0.162687 0.796788 0.028 Uiso 1 1 calc R U . . .
C68 C 0.5503(3) -0.2866(3) 0.6548(2) 0.0369(14) Uani 1 1 d . . . . .
H68 H 0.572089 -0.300916 0.625879 0.044 Uiso 1 1 calc R U . . .
C39 C 0.3647(3) 0.2525(3) 0.8778(2) 0.0373(14) Uani 1 1 d . . . . .
H39 H 0.342568 0.283101 0.900868 0.045 Uiso 1 1 calc R U . . .
C71 C 0.4884(3) -0.2512(3) 0.7375(2) 0.0391(14) Uani 1 1 d . . . . .
H71 H 0.465607 -0.238749 0.766196 0.047 Uiso 1 1 calc R U . . .
C52 C 0.1998(3) 0.2719(3) 0.5575(2) 0.0311(13) Uani 1 1 d . . . . .
H52 H 0.243490 0.260726 0.586770 0.037 Uiso 1 1 calc R U . . .
C38 C 0.3494(3) 0.1739(3) 0.8697(2) 0.0357(14) Uani 1 1 d . . . . .
H38 H 0.316265 0.149455 0.886862 0.043 Uiso 1 1 calc R U . . .
C54 C 0.0713(3) 0.2861(3) 0.5299(2) 0.0342(13) Uani 1 1 d . . . . .
H54 H 0.025664 0.285608 0.538265 0.041 Uiso 1 1 calc R U . . .
C56 C 0.1420(3) 0.3021(3) 0.4655(2) 0.0279(12) Uani 1 1 d . . . . .
H56 H 0.143799 0.313833 0.427984 0.033 Uiso 1 1 calc R U . . .
C46 C 0.5781(3) 0.4371(3) 0.7797(2) 0.0295(12) Uani 1 1 d . . . . .
H46 H 0.560146 0.446417 0.739850 0.035 Uiso 1 1 calc R U . . .
C58 C 0.3342(3) 0.0506(3) 0.44234(19) 0.0282(12) Uani 1 1 d . . . . .
H58 H 0.344452 0.004648 0.465119 0.034 Uiso 1 1 calc R U . . .
C60 C 0.3131(3) 0.1152(3) 0.3540(2) 0.0368(14) Uani 1 1 d . . . . .
H60 H 0.309714 0.115416 0.314476 0.044 Uiso 1 1 calc R U . . .
C65 C 0.4104(3) 0.4814(3) 0.4328(2) 0.0300(12) Uani 1 1 d . . . . .
H65 H 0.453192 0.512423 0.446104 0.036 Uiso 1 1 calc R U . . .
C47 C 0.7212(3) 0.3059(4) 0.7126(2) 0.0413(15) Uani 1 1 d . . . . .
H47 H 0.705333 0.357743 0.716443 0.050 Uiso 1 1 calc R U . . .
Li1 Li 0.5853(5) 0.2647(5) 0.7416(3) 0.0264(19) Uani 1 1 d . . . . .
C33 C 0.3777(3) 0.5500(3) 0.7092(2) 0.0328(13) Uani 1 1 d . . . . .
H33A H 0.358382 0.584959 0.733833 0.039 Uiso 1 1 calc R U . . .
H33B H 0.431819 0.551176 0.723355 0.039 Uiso 1 1 calc R U . . .
C11 C 0.6265(3) -0.0149(3) 1.00475(18) 0.0317(13) Uani 1 1 d . . . . .
H11A H 0.650028 0.037254 1.008791 0.038 Uiso 1 1 calc R U . . .
H11B H 0.610823 -0.025000 1.039355 0.038 Uiso 1 1 calc R U . . .
C70 C 0.4898(3) -0.1948(3) 0.6981(2) 0.0397(15) Uani 1 1 d . . . . .
H70 H 0.469087 -0.144651 0.699875 0.048 Uiso 1 1 calc R U . . .
C42 C 0.6190(3) 0.3533(3) 0.8538(2) 0.0330(13) Uani 1 1 d . . . . .
H42 H 0.630549 0.301534 0.867548 0.040 Uiso 1 1 calc R U . . .
C59 C 0.3289(3) 0.0474(3) 0.3849(2) 0.0346(14) Uani 1 1 d . . . . .
H59 H 0.335964 -0.000405 0.367285 0.042 Uiso 1 1 calc R U . . .
C13 C 0.7043(3) -0.0641(3) 0.9460(2) 0.0351(13) Uani 1 1 d . . . . .
H13A H 0.738476 -0.106255 0.942603 0.042 Uiso 1 1 calc R U . . .
H13B H 0.730479 -0.013579 0.948623 0.042 Uiso 1 1 calc R U . . .
C63 C 0.3010(3) 0.4481(3) 0.3615(2) 0.0312(13) Uani 1 1 d . . . . .
H63 H 0.266969 0.455721 0.325037 0.037 Uiso 1 1 calc R U . . .
C55 C 0.0749(3) 0.3016(3) 0.4757(2) 0.0351(14) Uani 1 1 d . . . . .
H55 H 0.031673 0.311702 0.445726 0.042 Uiso 1 1 calc R U . . .
C64 C 0.3622(3) 0.4935(3) 0.3792(2) 0.0335(13) Uani 1 1 d . . . . .
H64 H 0.371667 0.533007 0.354880 0.040 Uiso 1 1 calc R U . . .
C44 C 0.6140(3) 0.4881(3) 0.8732(2) 0.0413(15) Uani 1 1 d . . . . .
H44 H 0.621489 0.530701 0.899212 0.050 Uiso 1 1 calc R U . . .
C45 C 0.5873(3) 0.5011(3) 0.8161(2) 0.0375(14) Uani 1 1 d . . . . .
H45 H 0.575205 0.552475 0.801614 0.045 Uiso 1 1 calc R U . . .
C53 C 0.1350(3) 0.2715(3) 0.5715(2) 0.0343(13) Uani 1 1 d . . . . .
H53 H 0.134477 0.261180 0.609531 0.041 Uiso 1 1 calc R U . . .
C12 C 0.6812(3) -0.0765(3) 0.9997(2) 0.0325(13) Uani 1 1 d . . . . .
H12A H 0.659024 -0.129078 0.998700 0.039 Uiso 1 1 calc R U . . .
H12B H 0.724693 -0.073969 1.033415 0.039 Uiso 1 1 calc R U . . .
C43 C 0.6301(3) 0.4132(3) 0.8931(2) 0.0398(15) Uani 1 1 d . . . . .
H43 H 0.648389 0.402952 0.932809 0.048 Uiso 1 1 calc R U . . .
C34 C 0.3536(3) 0.5802(3) 0.6484(2) 0.0347(13) Uani 1 1 d . . . . .
H34A H 0.299613 0.584944 0.635770 0.042 Uiso 1 1 calc R U . . .
H34B H 0.374519 0.632952 0.646983 0.042 Uiso 1 1 calc R U . . .
C69 C 0.5218(3) -0.2124(3) 0.6564(2) 0.0437(16) Uani 1 1 d . . . . .
H69 H 0.524532 -0.174223 0.628832 0.052 Uiso 1 1 calc R U . . .
C50 C 0.7663(4) 0.1597(5) 0.6989(2) 0.058(2) Uani 1 1 d . . . . .
H50 H 0.780033 0.107461 0.693640 0.070 Uiso 1 1 calc R U . . .
Li2 Li 0.3074(5) 0.2815(5) 0.4907(3) 0.0224(18) Uani 1 1 d . . . . .
C48 C 0.7869(4) 0.2953(5) 0.6998(2) 0.065(2) Uani 1 1 d . . . . .
H48 H 0.815885 0.338936 0.695807 0.078 Uiso 1 1 calc R U . . .
C49 C 0.8094(4) 0.2199(7) 0.6929(3) 0.078(3) Uani 1 1 d . . . . .
H49 H 0.854214 0.210625 0.684225 0.094 Uiso 1 1 calc R U . . .
O2 O 0.37205(17) 0.24972(17) 0.56262(12) 0.0186(7) Uani 1 1 d . . . . .
O1 O 0.49608(16) 0.19390(16) 0.70808(11) 0.0153(7) Uani 1 1 d . . . . .
N14 N 0.0126(4) 0.1422(5) 0.6212(3) 0.102(2) Uani 1 1 d D U . . .
C72 C 0.0297(5) 0.1002(4) 0.5814(5) 0.092(3) Uani 1 1 d D U . . .
H72 H 0.072911 0.069342 0.590727 0.111 Uiso 1 1 calc R U . . .
C73 C -0.0148(6) 0.1015(5) 0.5273(4) 0.111(3) Uani 1 1 d D U . . .
H73 H -0.002153 0.071269 0.498870 0.134 Uiso 1 1 calc R U . . .
C74 C -0.0763(5) 0.1445(5) 0.5128(3) 0.099(4) Uani 1 1 d D U . . .
H74 H -0.107779 0.145535 0.474879 0.118 Uiso 1 1 calc R U . . .
C75 C -0.0904(4) 0.1850(5) 0.5541(4) 0.090(3) Uani 1 1 d D U . . .
H75 H -0.133943 0.215329 0.545659 0.108 Uiso 1 1 calc R U . . .
C76 C -0.0463(5) 0.1855(5) 0.6074(4) 0.077(2) Uani 1 1 d D U . . .
H76 H -0.057822 0.217524 0.635437 0.092 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 Cl3 2.7726(11) . ?
U1 N5 2.504(4) . ?
U1 N4 2.595(4) . ?
U1 N3 2.498(3) . ?
U1 N6 2.581(4) . ?
U1 O2 1.849(3) . ?
U1 O1 1.940(3) . ?
Dy1 Cl2 2.6583(11) . ?
Dy1 Cl1 2.5804(12) . ?
Dy1 N7 2.555(4) . ?
Dy1 N1 2.359(4) . ?
Dy1 N2 2.525(3) . ?
Dy1 O1 2.267(3) . ?
Cl3 Li1 2.741(8) . ?
Cl2 Li1 2.577(8) . ?
N5 C29 1.401(5) . ?
N5 C26 1.360(5) . ?
N4 C19 1.285(5) . ?
N4 C20 1.477(5) . ?
N3 C15 1.363(5) . ?
N3 C18 1.401(5) . ?
N6 C30 1.291(5) . ?
N6 C31 1.480(5) . ?
N7 C41 1.341(6) . ?
N7 C37 1.330(6) . ?
N1 C4 1.367(5) . ?
N1 C7 1.384(5) . ?
C29 C30 1.419(6) . ?
C29 C28 1.388(6) . ?
N9 C51 1.329(6) . ?
N9 C47 1.345(7) . ?
N9 Li1 2.031(10) . ?
C26 C3 1.518(6) . ?
C26 C27 1.396(6) . ?
C15 C3 1.521(6) . ?
C15 C16 1.385(6) . ?
N2 C9 1.485(5) . ?
N2 C8 1.288(6) . ?
N10 C57 1.333(6) . ?
N10 C61 1.343(6) . ?
N10 Li2 2.080(8) . ?
N12 C52 1.336(6) . ?
N12 C56 1.338(6) . ?
N12 Li2 2.082(9) . ?
N11 C66 1.335(6) . ?
N11 C62 1.339(6) . ?
N11 Li2 2.069(8) . ?
C30 H30 0.9500 . ?
C18 C19 1.417(6) . ?
C18 C17 1.379(6) . ?
C19 H19 0.9500 . ?
N8 C46 1.327(6) . ?
N8 Li1 2.151(9) . ?
N8 C42 1.342(6) . ?
C4 C3 1.528(6) . ?
C4 C5 1.392(6) . ?
C3 C2 1.551(6) . ?
C41 H41 0.9500 . ?
C41 C40 1.381(7) . ?
C31 H31 1.0000 . ?
C31 C36 1.522(6) . ?
C31 C32 1.529(6) . ?
N13 C67 1.328(7) . ?
N13 C71 1.332(7) . ?
C7 C8 1.431(6) . ?
C7 C6 1.378(6) . ?
C20 H20 1.0000 . ?
C20 C25 1.522(6) . ?
C20 C21 1.524(6) . ?
C17 H17 0.9500 . ?
C17 C16 1.394(6) . ?
C9 H9 1.0000 . ?
C9 C14 1.516(6) . ?
C9 C10 1.520(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C24 1.528(6) . ?
C28 H28 0.9500 . ?
C28 C27 1.381(6) . ?
C27 H27 0.9500 . ?
C16 H16 0.9500 . ?
C37 H37 0.9500 . ?
C37 C38 1.384(7) . ?
C8 H8 0.9500 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.528(6) . ?
C57 H57 0.9500 . ?
C57 C58 1.371(6) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C35 1.540(6) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C23 1.521(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C61 H61 0.9500 . ?
C61 C60 1.379(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.392(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.527(6) . ?
C66 H66 0.9500 . ?
C66 C65 1.376(7) . ?
C51 H51 0.9500 . ?
C51 C50 1.377(8) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C13 1.540(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C22 1.528(6) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.534(6) . ?
C62 H62 0.9500 . ?
C62 C63 1.373(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.537(6) . ?
C67 H67 0.9500 . ?
C67 C68 1.362(7) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C34 1.508(7) . ?
C40 H40 0.9500 . ?
C40 C39 1.373(7) . ?
C6 H6 0.9500 . ?
C68 H68 0.9500 . ?
C68 C69 1.385(7) . ?
C39 H39 0.9500 . ?
C39 C38 1.377(8) . ?
C71 H71 0.9500 . ?
C71 C70 1.367(7) . ?
C52 H52 0.9500 . ?
C52 C53 1.372(7) . ?
C38 H38 0.9500 . ?
C54 H54 0.9500 . ?
C54 C55 1.371(7) . ?
C54 C53 1.367(7) . ?
C56 H56 0.9500 . ?
C56 C55 1.371(7) . ?
C46 H46 0.9500 . ?
C46 C45 1.389(7) . ?
C58 H58 0.9500 . ?
C58 C59 1.381(6) . ?
C60 H60 0.9500 . ?
C60 C59 1.369(7) . ?
C65 H65 0.9500 . ?
C65 C64 1.385(7) . ?
C47 H47 0.9500 . ?
C47 C48 1.386(9) . ?
Li1 O1 2.058(8) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.517(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.511(7) . ?
C70 H70 0.9500 . ?
C70 C69 1.362(8) . ?
C42 H42 0.9500 . ?
C42 C43 1.379(7) . ?
C59 H59 0.9500 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C12 1.514(7) . ?
C63 H63 0.9500 . ?
C63 C64 1.364(7) . ?
C55 H55 0.9500 . ?
C64 H64 0.9500 . ?
C44 H44 0.9500 . ?
C44 C45 1.360(7) . ?
C44 C43 1.372(7) . ?
C45 H45 0.9500 . ?
C53 H53 0.9500 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C43 H43 0.9500 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C69 H69 0.9500 . ?
C50 H50 0.9500 . ?
C50 C49 1.350(10) . ?
Li2 O2 1.916(8) . ?
C48 H48 0.9500 . ?
C48 C49 1.384(11) . ?
C49 H49 0.9500 . ?
N14 C72 1.323(8) . ?
N14 C76 1.307(8) . ?
C72 H72 0.9500 . ?
C72 C73 1.352(9) . ?
C73 H73 0.9500 . ?
C73 C74 1.344(9) . ?
C74 H74 0.9500 . ?
C74 C75 1.315(8) . ?
C75 H75 0.9500 . ?
C75 C76 1.334(8) . ?
C76 H76 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 U1 Cl3 143.68(8) . . ?
N5 U1 N4 137.40(11) . . ?
N5 U1 N6 67.32(12) . . ?
N4 U1 Cl3 77.32(8) . . ?
N3 U1 Cl3 143.59(9) . . ?
N3 U1 N5 68.66(11) . . ?
N3 U1 N4 68.75(11) . . ?
N3 U1 N6 135.97(12) . . ?
N6 U1 Cl3 78.53(9) . . ?
N6 U1 N4 155.27(12) . . ?
O2 U1 Cl3 95.53(10) . . ?
O2 U1 N5 95.20(12) . . ?
O2 U1 N4 89.24(12) . . ?
O2 U1 N3 96.80(12) . . ?
O2 U1 N6 87.90(12) . . ?
O2 U1 O1 179.17(13) . . ?
O1 U1 Cl3 83.90(9) . . ?
O1 U1 N5 85.60(12) . . ?
O1 U1 N4 90.06(11) . . ?
O1 U1 N3 83.33(11) . . ?
O1 U1 N6 92.57(11) . . ?
Cl1 Dy1 Cl2 87.31(4) . . ?
N7 Dy1 Cl2 82.79(9) . . ?
N7 Dy1 Cl1 165.28(8) . . ?
N1 Dy1 Cl2 151.98(8) . . ?
N1 Dy1 Cl1 98.44(9) . . ?
N1 Dy1 N7 85.54(12) . . ?
N1 Dy1 N2 69.38(12) . . ?
N2 Dy1 Cl2 83.54(9) . . ?
N2 Dy1 Cl1 87.97(9) . . ?
N2 Dy1 N7 80.14(11) . . ?
O1 Dy1 Cl2 76.40(7) . . ?
O1 Dy1 Cl1 106.16(8) . . ?
O1 Dy1 N7 82.10(11) . . ?
O1 Dy1 N1 127.00(11) . . ?
O1 Dy1 N2 154.65(11) . . ?
Li1 Cl3 U1 76.40(17) . . ?
Li1 Cl2 Dy1 87.53(18) . . ?
C29 N5 U1 114.3(3) . . ?
C26 N5 U1 140.2(3) . . ?
C26 N5 C29 105.4(4) . . ?
C19 N4 U1 112.5(3) . . ?
C19 N4 C20 119.1(4) . . ?
C20 N4 U1 128.0(3) . . ?
C15 N3 U1 140.4(3) . . ?
C15 N3 C18 105.3(3) . . ?
C18 N3 U1 112.8(3) . . ?
C30 N6 U1 115.4(3) . . ?
C30 N6 C31 119.8(4) . . ?
C31 N6 U1 124.8(3) . . ?
C41 N7 Dy1 120.1(3) . . ?
C37 N7 Dy1 122.6(3) . . ?
C37 N7 C41 117.2(4) . . ?
C4 N1 Dy1 138.1(3) . . ?
C4 N1 C7 105.0(4) . . ?
C7 N1 Dy1 116.6(3) . . ?
N5 C29 C30 121.1(4) . . ?
C28 C29 N5 110.1(4) . . ?
C28 C29 C30 128.7(4) . . ?
C51 N9 C47 116.7(5) . . ?
C51 N9 Li1 122.1(4) . . ?
C47 N9 Li1 121.2(5) . . ?
N5 C26 C3 126.8(4) . . ?
N5 C26 C27 110.4(4) . . ?
C27 C26 C3 122.7(4) . . ?
N3 C15 C3 125.5(4) . . ?
N3 C15 C16 110.4(4) . . ?
C16 C15 C3 123.9(4) . . ?
C9 N2 Dy1 129.4(3) . . ?
C8 N2 Dy1 112.4(3) . . ?
C8 N2 C9 117.2(4) . . ?
C57 N10 C61 116.2(4) . . ?
C57 N10 Li2 111.1(3) . . ?
C61 N10 Li2 132.4(4) . . ?
C52 N12 C56 115.6(4) . . ?
C52 N12 Li2 119.0(4) . . ?
C56 N12 Li2 125.3(4) . . ?
C66 N11 C62 116.6(4) . . ?
C66 N11 Li2 128.9(4) . . ?
C62 N11 Li2 114.3(4) . . ?
N6 C30 C29 121.5(4) . . ?
N6 C30 H30 119.2 . . ?
C29 C30 H30 119.2 . . ?
N3 C18 C19 121.8(4) . . ?
C17 C18 N3 110.4(4) . . ?
C17 C18 C19 127.5(4) . . ?
N4 C19 C18 124.0(4) . . ?
N4 C19 H19 118.0 . . ?
C18 C19 H19 118.0 . . ?
C46 N8 Li1 124.8(4) . . ?
C46 N8 C42 116.1(4) . . ?
C42 N8 Li1 118.9(4) . . ?
N1 C4 C3 118.2(4) . . ?
N1 C4 C5 110.9(4) . . ?
C5 C4 C3 130.8(4) . . ?
C26 C3 C15 116.8(4) . . ?
C26 C3 C4 106.2(3) . . ?
C26 C3 C2 108.8(4) . . ?
C15 C3 C4 106.4(4) . . ?
C15 C3 C2 109.0(3) . . ?
C4 C3 C2 109.4(3) . . ?
N7 C41 H41 118.3 . . ?
N7 C41 C40 123.5(5) . . ?
C40 C41 H41 118.3 . . ?
N6 C31 H31 106.3 . . ?
N6 C31 C36 109.4(3) . . ?
N6 C31 C32 117.6(4) . . ?
C36 C31 H31 106.3 . . ?
C36 C31 C32 110.2(4) . . ?
C32 C31 H31 106.3 . . ?
C67 N13 C71 116.0(5) . . ?
N1 C7 C8 118.5(4) . . ?
C6 C7 N1 110.9(4) . . ?
C6 C7 C8 130.6(4) . . ?
N4 C20 H20 107.1 . . ?
N4 C20 C25 109.1(4) . . ?
N4 C20 C21 116.7(4) . . ?
C25 C20 H20 107.1 . . ?
C25 C20 C21 109.4(3) . . ?
C21 C20 H20 107.1 . . ?
C18 C17 H17 126.9 . . ?
C18 C17 C16 106.3(4) . . ?
C16 C17 H17 126.9 . . ?
N2 C9 H9 106.8 . . ?
N2 C9 C14 110.8(4) . . ?
N2 C9 C10 114.0(4) . . ?
C14 C9 H9 106.8 . . ?
C14 C9 C10 111.3(4) . . ?
C10 C9 H9 106.8 . . ?
C20 C25 H25A 109.3 . . ?
C20 C25 H25B 109.3 . . ?
C20 C25 C24 111.7(4) . . ?
H25A C25 H25B 107.9 . . ?
C24 C25 H25A 109.3 . . ?
C24 C25 H25B 109.3 . . ?
C29 C28 H28 126.7 . . ?
C27 C28 C29 106.6(4) . . ?
C27 C28 H28 126.7 . . ?
C26 C27 H27 126.2 . . ?
C28 C27 C26 107.5(4) . . ?
C28 C27 H27 126.2 . . ?
C15 C16 C17 107.6(4) . . ?
C15 C16 H16 126.2 . . ?
C17 C16 H16 126.2 . . ?
N7 C37 H37 118.6 . . ?
N7 C37 C38 122.7(5) . . ?
C38 C37 H37 118.6 . . ?
N2 C8 C7 122.3(4) . . ?
N2 C8 H8 118.8 . . ?
C7 C8 H8 118.8 . . ?
C3 C2 H2A 108.8 . . ?
C3 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
C1 C2 C3 114.0(4) . . ?
C1 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
N10 C57 H57 118.0 . . ?
N10 C57 C58 124.0(4) . . ?
C58 C57 H57 118.0 . . ?
C31 C36 H36A 109.6 . . ?
C31 C36 H36B 109.6 . . ?
C31 C36 C35 110.3(4) . . ?
H36A C36 H36B 108.1 . . ?
C35 C36 H36A 109.6 . . ?
C35 C36 H36B 109.6 . . ?
C25 C24 H24A 109.4 . . ?
C25 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
C23 C24 C25 111.0(4) . . ?
C23 C24 H24A 109.4 . . ?
C23 C24 H24B 109.4 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N10 C61 H61 118.4 . . ?
N10 C61 C60 123.3(5) . . ?
C60 C61 H61 118.4 . . ?
C4 C5 H5 126.8 . . ?
C6 C5 C4 106.4(4) . . ?
C6 C5 H5 126.8 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 C22 110.8(4) . . ?
H21A C21 H21B 108.1 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
N11 C66 H66 118.2 . . ?
N11 C66 C65 123.6(4) . . ?
C65 C66 H66 118.2 . . ?
N9 C51 H51 118.3 . . ?
N9 C51 C50 123.4(6) . . ?
C50 C51 H51 118.3 . . ?
C9 C14 H14A 109.3 . . ?
C9 C14 H14B 109.3 . . ?
C9 C14 C13 111.5(4) . . ?
H14A C14 H14B 108.0 . . ?
C13 C14 H14A 109.3 . . ?
C13 C14 H14B 109.3 . . ?
C24 C23 H23A 109.4 . . ?
C24 C23 H23B 109.4 . . ?
C24 C23 C22 111.3(4) . . ?
H23A C23 H23B 108.0 . . ?
C22 C23 H23A 109.4 . . ?
C22 C23 H23B 109.4 . . ?
C31 C32 H32A 110.0 . . ?
C31 C32 H32B 110.0 . . ?
C31 C32 C33 108.5(4) . . ?
H32A C32 H32B 108.4 . . ?
C33 C32 H32A 110.0 . . ?
C33 C32 H32B 110.0 . . ?
N11 C62 H62 118.0 . . ?
N11 C62 C63 124.0(5) . . ?
C63 C62 H62 118.0 . . ?
C21 C22 C23 111.2(4) . . ?
C21 C22 H22A 109.4 . . ?
C21 C22 H22B 109.4 . . ?
C23 C22 H22A 109.4 . . ?
C23 C22 H22B 109.4 . . ?
H22A C22 H22B 108.0 . . ?
C9 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
C9 C10 C11 111.3(4) . . ?
H10A C10 H10B 108.0 . . ?
C11 C10 H10A 109.4 . . ?
C11 C10 H10B 109.4 . . ?
N13 C67 H67 117.8 . . ?
N13 C67 C68 124.4(5) . . ?
C68 C67 H67 117.8 . . ?
C36 C35 H35A 109.4 . . ?
C36 C35 H35B 109.4 . . ?
H35A C35 H35B 108.0 . . ?
C34 C35 C36 111.1(4) . . ?
C34 C35 H35A 109.4 . . ?
C34 C35 H35B 109.4 . . ?
C41 C40 H40 120.6 . . ?
C39 C40 C41 118.7(5) . . ?
C39 C40 H40 120.6 . . ?
C7 C6 C5 106.7(4) . . ?
C7 C6 H6 126.6 . . ?
C5 C6 H6 126.6 . . ?
C67 C68 H68 121.0 . . ?
C67 C68 C69 118.0(5) . . ?
C69 C68 H68 121.0 . . ?
C40 C39 H39 120.8 . . ?
C40 C39 C38 118.4(5) . . ?
C38 C39 H39 120.8 . . ?
N13 C71 H71 117.8 . . ?
N13 C71 C70 124.3(5) . . ?
C70 C71 H71 117.8 . . ?
N12 C52 H52 118.0 . . ?
N12 C52 C53 124.0(5) . . ?
C53 C52 H52 118.0 . . ?
C37 C38 H38 120.3 . . ?
C39 C38 C37 119.5(5) . . ?
C39 C38 H38 120.3 . . ?
C55 C54 H54 120.8 . . ?
C53 C54 H54 120.8 . . ?
C53 C54 C55 118.4(5) . . ?
N12 C56 H56 118.0 . . ?
N12 C56 C55 124.1(4) . . ?
C55 C56 H56 118.0 . . ?
N8 C46 H46 118.0 . . ?
N8 C46 C45 124.1(5) . . ?
C45 C46 H46 118.0 . . ?
C57 C58 H58 120.4 . . ?
C57 C58 C59 119.1(5) . . ?
C59 C58 H58 120.4 . . ?
C61 C60 H60 120.3 . . ?
C59 C60 C61 119.5(5) . . ?
C59 C60 H60 120.3 . . ?
C66 C65 H65 120.9 . . ?
C66 C65 C64 118.1(5) . . ?
C64 C65 H65 120.9 . . ?
N9 C47 H47 118.6 . . ?
N9 C47 C48 122.8(6) . . ?
C48 C47 H47 118.6 . . ?
Cl2 Li1 Cl3 164.3(3) . . ?
N9 Li1 Cl3 91.2(3) . . ?
N9 Li1 Cl2 94.1(3) . . ?
N9 Li1 N8 112.7(4) . . ?
N9 Li1 O1 119.5(4) . . ?
N8 Li1 Cl3 94.7(3) . . ?
N8 Li1 Cl2 96.8(3) . . ?
O1 Li1 Cl3 82.7(3) . . ?
O1 Li1 Cl2 81.8(3) . . ?
O1 Li1 N8 127.8(4) . . ?
C32 C33 H33A 109.3 . . ?
C32 C33 H33B 109.3 . . ?
H33A C33 H33B 107.9 . . ?
C34 C33 C32 111.8(4) . . ?
C34 C33 H33A 109.3 . . ?
C34 C33 H33B 109.3 . . ?
C10 C11 H11A 109.4 . . ?
C10 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 C10 110.9(4) . . ?
C12 C11 H11A 109.4 . . ?
C12 C11 H11B 109.4 . . ?
C71 C70 H70 120.9 . . ?
C69 C70 C71 118.3(5) . . ?
C69 C70 H70 120.9 . . ?
N8 C42 H42 118.1 . . ?
N8 C42 C43 123.9(5) . . ?
C43 C42 H42 118.1 . . ?
C58 C59 H59 121.1 . . ?
C60 C59 C58 117.9(5) . . ?
C60 C59 H59 121.1 . . ?
C14 C13 H13A 109.4 . . ?
C14 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
C12 C13 C14 111.3(4) . . ?
C12 C13 H13A 109.4 . . ?
C12 C13 H13B 109.4 . . ?
C62 C63 H63 120.8 . . ?
C64 C63 C62 118.3(5) . . ?
C64 C63 H63 120.8 . . ?
C54 C55 H55 120.6 . . ?
C56 C55 C54 118.8(5) . . ?
C56 C55 H55 120.6 . . ?
C65 C64 H64 120.3 . . ?
C63 C64 C65 119.4(5) . . ?
C63 C64 H64 120.3 . . ?
C45 C44 H44 120.1 . . ?
C45 C44 C43 119.8(5) . . ?
C43 C44 H44 120.1 . . ?
C46 C45 H45 121.0 . . ?
C44 C45 C46 118.1(5) . . ?
C44 C45 H45 121.0 . . ?
C52 C53 H53 120.5 . . ?
C54 C53 C52 119.1(5) . . ?
C54 C53 H53 120.5 . . ?
C11 C12 C13 110.6(4) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C42 C43 H43 120.9 . . ?
C44 C43 C42 118.1(5) . . ?
C44 C43 H43 120.9 . . ?
C35 C34 C33 111.6(4) . . ?
C35 C34 H34A 109.3 . . ?
C35 C34 H34B 109.3 . . ?
C33 C34 H34A 109.3 . . ?
C33 C34 H34B 109.3 . . ?
H34A C34 H34B 108.0 . . ?
C68 C69 H69 120.5 . . ?
C70 C69 C68 119.0(5) . . ?
C70 C69 H69 120.5 . . ?
C51 C50 H50 120.1 . . ?
C49 C50 C51 119.8(7) . . ?
C49 C50 H50 120.1 . . ?
N10 Li2 N12 108.8(4) . . ?
N11 Li2 N10 104.9(3) . . ?
N11 Li2 N12 115.3(4) . . ?
O2 Li2 N10 104.1(4) . . ?
O2 Li2 N12 104.2(4) . . ?
O2 Li2 N11 118.8(4) . . ?
C47 C48 H48 120.6 . . ?
C49 C48 C47 118.7(7) . . ?
C49 C48 H48 120.6 . . ?
C50 C49 C48 118.4(7) . . ?
C50 C49 H49 120.8 . . ?
C48 C49 H49 120.8 . . ?
U1 O2 Li2 177.2(3) . . ?
U1 O1 Dy1 128.20(14) . . ?
U1 O1 Li1 117.0(3) . . ?
Li1 O1 Dy1 113.6(3) . . ?
C76 N14 C72 119.4(8) . . ?
N14 C72 H72 120.2 . . ?
N14 C72 C73 119.6(8) . . ?
C73 C72 H72 120.2 . . ?
C72 C73 H73 119.2 . . ?
C74 C73 C72 121.6(7) . . ?
C74 C73 H73 119.2 . . ?
C73 C74 H74 122.0 . . ?
C75 C74 C73 116.1(7) . . ?
C75 C74 H74 122.0 . . ?
C74 C75 H75 118.5 . . ?
C74 C75 C76 123.0(7) . . ?
C76 C75 H75 118.5 . . ?
N14 C76 C75 120.3(8) . . ?
N14 C76 H76 119.9 . . ?
C75 C76 H76 119.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 N5 C29 C30 5.4(5) . . . . ?
U1 N5 C29 C28 -177.6(3) . . . . ?
U1 N5 C26 C3 0.6(7) . . . . ?
U1 N5 C26 C27 177.0(3) . . . . ?
U1 N4 C19 C18 -1.8(5) . . . . ?
U1 N4 C20 C25 -67.5(4) . . . . ?
U1 N4 C20 C21 167.9(3) . . . . ?
U1 N3 C15 C3 -18.9(7) . . . . ?
U1 N3 C15 C16 165.0(3) . . . . ?
U1 N3 C18 C19 4.2(5) . . . . ?
U1 N3 C18 C17 -170.2(3) . . . . ?
U1 N6 C30 C29 -4.1(5) . . . . ?
U1 N6 C31 C36 67.6(4) . . . . ?
U1 N6 C31 C32 -165.7(3) . . . . ?
Dy1 N7 C41 C40 -174.9(4) . . . . ?
Dy1 N7 C37 C38 174.8(4) . . . . ?
Dy1 N1 C4 C3 -9.3(6) . . . . ?
Dy1 N1 C4 C5 172.9(3) . . . . ?
Dy1 N1 C7 C8 6.2(5) . . . . ?
Dy1 N1 C7 C6 -174.9(3) . . . . ?
Dy1 N2 C9 C14 -91.6(4) . . . . ?
Dy1 N2 C9 C10 141.9(3) . . . . ?
Dy1 N2 C8 C7 -7.4(6) . . . . ?
N5 C29 C30 N6 -0.8(6) . . . . ?
N5 C29 C28 C27 -0.5(5) . . . . ?
N5 C26 C3 C15 -2.4(6) . . . . ?
N5 C26 C3 C4 116.0(4) . . . . ?
N5 C26 C3 C2 -126.3(4) . . . . ?
N5 C26 C27 C28 0.1(5) . . . . ?
N4 C20 C25 C24 173.5(4) . . . . ?
N4 C20 C21 C22 -177.5(4) . . . . ?
N3 C15 C3 C26 10.5(6) . . . . ?
N3 C15 C3 C4 -107.8(4) . . . . ?
N3 C15 C3 C2 134.2(4) . . . . ?
N3 C15 C16 C17 0.0(5) . . . . ?
N3 C18 C19 N4 -1.7(7) . . . . ?
N3 C18 C17 C16 0.9(5) . . . . ?
N6 C31 C36 C35 -169.8(4) . . . . ?
N6 C31 C32 C33 173.9(4) . . . . ?
N7 C41 C40 C39 -0.3(8) . . . . ?
N7 C37 C38 C39 0.3(8) . . . . ?
N1 C4 C3 C26 -63.2(5) . . . . ?
N1 C4 C3 C15 61.9(5) . . . . ?
N1 C4 C3 C2 179.5(4) . . . . ?
N1 C4 C5 C6 0.4(5) . . . . ?
N1 C7 C8 N2 1.3(7) . . . . ?
N1 C7 C6 C5 0.4(5) . . . . ?
C29 N5 C26 C3 -176.8(4) . . . . ?
C29 N5 C26 C27 -0.4(5) . . . . ?
C29 C28 C27 C26 0.3(5) . . . . ?
N9 C51 C50 C49 1.0(9) . . . . ?
N9 C47 C48 C49 1.4(9) . . . . ?
C26 N5 C29 C30 -176.5(4) . . . . ?
C26 N5 C29 C28 0.6(5) . . . . ?
C26 C3 C2 C1 65.0(5) . . . . ?
C15 N3 C18 C19 173.4(4) . . . . ?
C15 N3 C18 C17 -1.0(5) . . . . ?
C15 C3 C2 C1 -63.4(5) . . . . ?
N2 C9 C14 C13 178.2(4) . . . . ?
N2 C9 C10 C11 -179.3(4) . . . . ?
N10 C57 C58 C59 1.6(8) . . . . ?
N10 C61 C60 C59 2.1(9) . . . . ?
N12 C52 C53 C54 1.1(9) . . . . ?
N12 C56 C55 C54 1.1(8) . . . . ?
N11 C66 C65 C64 0.2(8) . . . . ?
N11 C62 C63 C64 0.2(8) . . . . ?
C30 N6 C31 C36 -109.9(4) . . . . ?
C30 N6 C31 C32 16.8(6) . . . . ?
C30 C29 C28 C27 176.2(4) . . . . ?
C18 N3 C15 C3 176.7(4) . . . . ?
C18 N3 C15 C16 0.6(5) . . . . ?
C18 C17 C16 C15 -0.5(5) . . . . ?
C19 N4 C20 C25 104.6(4) . . . . ?
C19 N4 C20 C21 -20.0(6) . . . . ?
C19 C18 C17 C16 -173.1(4) . . . . ?
N8 C46 C45 C44 1.0(9) . . . . ?
N8 C42 C43 C44 -0.5(9) . . . . ?
C4 N1 C7 C8 -179.0(4) . . . . ?
C4 N1 C7 C6 -0.1(5) . . . . ?
C4 C3 C2 C1 -179.4(4) . . . . ?
C4 C5 C6 C7 -0.4(5) . . . . ?
C3 C26 C27 C28 176.6(4) . . . . ?
C3 C15 C16 C17 -176.2(4) . . . . ?
C3 C4 C5 C6 -177.0(4) . . . . ?
C41 N7 C37 C38 -0.9(7) . . . . ?
C41 C40 C39 C38 -0.4(8) . . . . ?
C31 N6 C30 C29 173.6(4) . . . . ?
C31 C36 C35 C34 -55.9(6) . . . . ?
C31 C32 C33 C34 57.8(6) . . . . ?
N13 C67 C68 C69 -0.5(9) . . . . ?
N13 C71 C70 C69 0.6(9) . . . . ?
C7 N1 C4 C3 177.6(4) . . . . ?
C7 N1 C4 C5 -0.2(5) . . . . ?
C20 N4 C19 C18 -175.1(4) . . . . ?
C20 C25 C24 C23 56.0(5) . . . . ?
C20 C21 C22 C23 -57.2(5) . . . . ?
C17 C18 C19 N4 171.7(4) . . . . ?
C9 N2 C8 C7 -177.4(4) . . . . ?
C9 C14 C13 C12 55.1(6) . . . . ?
C9 C10 C11 C12 -56.3(6) . . . . ?
C25 C20 C21 C22 58.1(5) . . . . ?
C25 C24 C23 C22 -53.8(5) . . . . ?
C28 C29 C30 N6 -177.3(4) . . . . ?
C27 C26 C3 C15 -178.4(4) . . . . ?
C27 C26 C3 C4 -60.0(5) . . . . ?
C27 C26 C3 C2 57.7(5) . . . . ?
C16 C15 C3 C26 -174.0(4) . . . . ?
C16 C15 C3 C4 67.7(5) . . . . ?
C16 C15 C3 C2 -50.2(5) . . . . ?
C37 N7 C41 C40 0.9(7) . . . . ?
C8 N2 C9 C14 76.3(5) . . . . ?
C8 N2 C9 C10 -50.2(6) . . . . ?
C8 C7 C6 C5 179.0(5) . . . . ?
C57 N10 C61 C60 -1.4(8) . . . . ?
C57 C58 C59 C60 -0.8(8) . . . . ?
C36 C31 C32 C33 -59.8(5) . . . . ?
C36 C35 C34 C33 53.8(6) . . . . ?
C24 C23 C22 C21 54.8(5) . . . . ?
C61 N10 C57 C58 -0.4(8) . . . . ?
C61 C60 C59 C58 -0.9(9) . . . . ?
C5 C4 C3 C26 114.0(5) . . . . ?
C5 C4 C3 C15 -120.9(5) . . . . ?
C5 C4 C3 C2 -3.2(6) . . . . ?
C21 C20 C25 C24 -57.8(5) . . . . ?
C66 N11 C62 C63 0.3(7) . . . . ?
C66 C65 C64 C63 0.4(8) . . . . ?
C51 N9 C47 C48 -1.7(7) . . . . ?
C51 C50 C49 C48 -1.3(10) . . . . ?
C14 C9 C10 C11 54.5(6) . . . . ?
C14 C13 C12 C11 -56.7(6) . . . . ?
C32 C31 C36 C35 59.5(5) . . . . ?
C32 C33 C34 C35 -55.5(6) . . . . ?
C62 N11 C66 C65 -0.5(7) . . . . ?
C62 C63 C64 C65 -0.5(8) . . . . ?
C10 C9 C14 C13 -53.8(6) . . . . ?
C10 C11 C12 C13 57.2(6) . . . . ?
C67 N13 C71 C70 -2.2(9) . . . . ?
C67 C68 C69 C70 -1.2(9) . . . . ?
C40 C39 C38 C37 0.4(8) . . . . ?
C6 C7 C8 N2 -177.2(5) . . . . ?
C71 N13 C67 C68 2.1(9) . . . . ?
C71 C70 C69 C68 1.1(9) . . . . ?
C52 N12 C56 C55 -0.8(7) . . . . ?
C56 N12 C52 C53 -0.4(8) . . . . ?
C46 N8 C42 C43 0.7(8) . . . . ?
C47 N9 C51 C50 0.5(7) . . . . ?
C47 C48 C49 C50 0.1(10) . . . . ?
Li1 N9 C51 C50 -178.8(5) . . . . ?
Li1 N9 C47 C48 177.6(5) . . . . ?
Li1 N8 C46 C45 -176.0(5) . . . . ?
Li1 N8 C42 C43 176.1(5) . . . . ?
C42 N8 C46 C45 -0.9(8) . . . . ?
C55 C54 C53 C52 -0.7(8) . . . . ?
C45 C44 C43 C42 0.6(9) . . . . ?
C53 C54 C55 C56 -0.3(8) . . . . ?
C43 C44 C45 C46 -0.8(9) . . . . ?
Li2 N10 C57 C58 -175.1(5) . . . . ?
Li2 N10 C61 C60 171.9(5) . . . . ?
Li2 N12 C52 C53 -177.8(5) . . . . ?
Li2 N12 C56 C55 176.5(5) . . . . ?
Li2 N11 C66 C65 173.8(5) . . . . ?
Li2 N11 C62 C63 -174.8(5) . . . . ?
N14 C72 C73 C74 -0.1(12) . . . . ?
C72 N14 C76 C75 2.7(12) . . . . ?
C72 C73 C74 C75 0.1(13) . . . . ?
C73 C74 C75 C76 1.2(13) . . . . ?
C74 C75 C76 N14 -2.7(13) . . . . ?
C76 N14 C72 C73 -1.3(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.274
_oxdiff_exptl_absorpt_empirical_full_min 0.716
_vrf_PLAT220_to509_refinalised   
;
PROBLEM: NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        5.9 Ratio 
RESPONSE: Disorder on pyridine ligand
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Pyridene, hexane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
