# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_p14107_reint_ref-sr
_database_code_depnum_ccdc_archive 'CCDC 1883750'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;university of edinburgh
United Kingdom
;
_audit_update_record             
;
2018-12-07 deposited with the CCDC.	2019-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C65 H73 Ca I N11 O4 U'
_chemical_formula_weight         1477.35

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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'

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

_cell_length_a                   17.4073(7)
_cell_length_b                   15.5310(4)
_cell_length_c                   33.3439(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.157(5)
_cell_angle_gamma                90.00
_cell_volume                     8225.2(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    25595
_cell_measurement_theta_min      3.2350
_cell_measurement_theta_max      25.9330

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.6567
_exptl_crystal_size_mid          0.5351
_exptl_crystal_size_min          0.2440
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2948
_exptl_absorpt_coefficient_mu    2.454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.52719
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            130415
_diffrn_reflns_av_R_equivalents  0.1213
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         23.25
_reflns_number_total             11791
_reflns_number_gt                10091
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    MERCURY
_computing_publication_material  ORTEP

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0305P)²+1017.9722P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11791
_refine_ls_number_parameters     724
_refine_ls_number_restraints     102
_refine_ls_R_factor_all          0.1315
_refine_ls_R_factor_gt           0.1207
_refine_ls_wR_factor_ref         0.2816
_refine_ls_wR_factor_gt          0.2758
_refine_ls_goodness_of_fit_ref   0.870
_refine_ls_restrained_S_all      0.868
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3496(14) 0.7042(13) 0.3158(7) 0.038(5) Uani 1 1 d . . .
C2 C 0.4360(15) 0.7050(13) 0.3437(8) 0.050(7) Uani 1 1 d . . .
H2 H 0.4619 0.7214 0.3738 0.060 Uiso 1 1 calc R . .
C3 C 0.4737(16) 0.6767(15) 0.3176(8) 0.053(6) Uani 1 1 d . . .
H3 H 0.5328 0.6709 0.3266 0.063 Uiso 1 1 calc R . .
C4 C 0.4120(12) 0.6572(12) 0.2752(7) 0.032(3) Uani 1 1 d . . .
C5 C 0.4157(12) 0.6285(13) 0.2370(7) 0.039(5) Uani 1 1 d . . .
H5 H 0.4692 0.6144 0.2375 0.047 Uiso 1 1 calc R . .
C6 C 0.3572(12) 0.5937(16) 0.1609(7) 0.043(6) Uani 1 1 d . . .
C7 C 0.3960(14) 0.5128(13) 0.1590(8) 0.043(5) Uani 1 1 d . . .
H7 H 0.4182 0.4781 0.1847 0.052 Uiso 1 1 calc R . .
C8 C 0.4023(14) 0.4839(14) 0.1214(8) 0.044(5) Uani 1 1 d . . .
C9 C 0.4391(18) 0.4008(18) 0.1194(10) 0.072(8) Uani 1 1 d . . .
H9A H 0.4375 0.3922 0.0900 0.108 Uiso 1 1 calc R . .
H9B H 0.4071 0.3550 0.1258 0.108 Uiso 1 1 calc R . .
H9C H 0.4977 0.3992 0.1412 0.108 Uiso 1 1 calc R . .
C10 C 0.3646(13) 0.5382(16) 0.0834(7) 0.047(6) Uani 1 1 d . . .
C11 C 0.371(2) 0.511(2) 0.0397(9) 0.088(11) Uani 1 1 d . . .
H11A H 0.3979 0.4543 0.0436 0.131 Uiso 1 1 calc R . .
H11B H 0.4036 0.5533 0.0319 0.131 Uiso 1 1 calc R . .
H11C H 0.3138 0.5072 0.0161 0.131 Uiso 1 1 calc R . .
C12 C 0.3310(11) 0.6089(16) 0.0866(6) 0.038(5) Uani 1 1 d . . .
H12 H 0.3060 0.6416 0.0603 0.045 Uiso 1 1 calc R . .
C13 C 0.3261(12) 0.6458(13) 0.1253(7) 0.035(5) Uani 1 1 d . . .
C14 C 0.2965(13) 0.7876(13) 0.1095(7) 0.040(5) Uani 1 1 d . . .
H14 H 0.3309 0.7882 0.0935 0.048 Uiso 1 1 calc R . .
C15 C 0.2533(12) 0.8631(12) 0.1155(8) 0.039(4) Uani 1 1 d . . .
C16 C 0.2507(12) 0.9472(12) 0.0980(8) 0.039(5) Uani 1 1 d U . .
H16 H 0.2806 0.9646 0.0811 0.047 Uiso 1 1 calc R . .
C17 C 0.1977(15) 1.0006(13) 0.1092(8) 0.051(4) Uani 1 1 d U . .
H17 H 0.1855 1.0596 0.1020 0.061 Uiso 1 1 calc R . .
C18 C 0.1666(12) 0.9480(11) 0.1334(7) 0.035(5) Uani 1 1 d U . .
C19 C 0.1055(12) 0.9717(12) 0.1501(6) 0.033(3) Uani 1 1 d . . .
C20 C 0.1405(15) 0.9476(15) 0.2017(9) 0.057(7) Uani 1 1 d . . .
H20A H 0.0987 0.9640 0.2130 0.086 Uiso 1 1 calc R . .
H20B H 0.1932 0.9787 0.2180 0.086 Uiso 1 1 calc R . .
H20C H 0.1508 0.8855 0.2055 0.086 Uiso 1 1 calc R . .
C21 C 0.0839(15) 1.0634(12) 0.1479(9) 0.054(7) Uani 1 1 d . . .
H21A H 0.0425 1.0723 0.1604 0.081 Uiso 1 1 calc R . .
H21B H 0.0602 1.0824 0.1172 0.081 Uiso 1 1 calc R . .
H21C H 0.1348 1.0969 0.1647 0.081 Uiso 1 1 calc R . .
C22 C 0.0246(14) 0.9125(12) 0.1301(8) 0.041(5) Uani 1 1 d U . .
C23 C -0.0579(15) 0.9391(13) 0.1010(8) 0.051(4) Uani 1 1 d U . .
H23 H -0.0765 0.9966 0.0929 0.061 Uiso 1 1 calc R . .
C24 C -0.1038(14) 0.8675(12) 0.0874(8) 0.048(6) Uani 1 1 d U . .
H24 H -0.1615 0.8656 0.0676 0.058 Uiso 1 1 calc R . .
C25 C -0.0536(13) 0.7958(12) 0.1069(8) 0.039(4) Uani 1 1 d U . .
C26 C -0.0739(14) 0.7083(15) 0.1045(7) 0.045(6) Uani 1 1 d . . .
H26 H -0.1293 0.6895 0.0864 0.054 Uiso 1 1 calc R . .
C27 C -0.0369(12) 0.5624(12) 0.1224(7) 0.031(5) Uani 1 1 d . . .
C28 C -0.0897(15) 0.5246(14) 0.0835(7) 0.047(6) Uani 1 1 d . . .
H28 H -0.1189 0.5597 0.0585 0.056 Uiso 1 1 calc R . .
C29 C -0.1011(13) 0.4327(15) 0.0803(8) 0.047(6) Uani 1 1 d . . .
C30 C -0.1589(17) 0.3970(14) 0.0382(8) 0.063(7) Uani 1 1 d . . .
H30A H -0.1806 0.4435 0.0166 0.095 Uiso 1 1 calc R . .
H30B H -0.2058 0.3685 0.0418 0.095 Uiso 1 1 calc R . .
H30C H -0.1289 0.3550 0.0279 0.095 Uiso 1 1 calc R . .
C31 C -0.0596(14) 0.3892(14) 0.1182(8) 0.050(6) Uani 1 1 d . . .
C32 C -0.071(2) 0.2868(19) 0.1166(10) 0.094(12) Uani 1 1 d . . .
H32A H -0.0376 0.2625 0.1457 0.141 Uiso 1 1 calc R . .
H32B H -0.0519 0.2625 0.0952 0.141 Uiso 1 1 calc R . .
H32C H -0.1305 0.2727 0.1080 0.141 Uiso 1 1 calc R . .
C33 C -0.0046(12) 0.4243(12) 0.1573(8) 0.038(5) Uani 1 1 d . . .
H33 H 0.0256 0.3887 0.1820 0.045 Uiso 1 1 calc R . .
C34 C 0.0059(10) 0.5139(12) 0.1600(6) 0.030(4) Uani 1 1 d . . .
C35 C 0.0574(13) 0.5372(14) 0.2356(7) 0.041(5) Uani 1 1 d . . .
H35 H 0.0149 0.4982 0.2351 0.049 Uiso 1 1 calc R . .
C36 C 0.1108(12) 0.5744(12) 0.2759(7) 0.032(3) Uani 1 1 d U . .
C37 C 0.1126(13) 0.5674(13) 0.3170(7) 0.036(5) Uani 1 1 d U . .
H37 H 0.0770 0.5327 0.3256 0.043 Uiso 1 1 calc R . .
C38 C 0.1792(14) 0.6233(13) 0.3449(7) 0.040(5) Uani 1 1 d U . .
H38 H 0.1981 0.6304 0.3757 0.048 Uiso 1 1 calc R . .
C39 C 0.2102(13) 0.6646(12) 0.3180(7) 0.032(5) Uani 1 1 d U . .
C40 C 0.2792(12) 0.7335(12) 0.3292(6) 0.033(3) Uani 1 1 d . . .
C41 C 0.2358(17) 0.8139(13) 0.3004(8) 0.053(6) Uani 1 1 d . . .
H41A H 0.2771 0.8604 0.3063 0.079 Uiso 1 1 calc R . .
H41B H 0.1894 0.8333 0.3075 0.079 Uiso 1 1 calc R . .
H41C H 0.2139 0.7982 0.2692 0.079 Uiso 1 1 calc R . .
C42 C 0.3105(18) 0.7574(18) 0.3771(8) 0.065(7) Uani 1 1 d . . .
H42A H 0.3545 0.8013 0.3841 0.098 Uiso 1 1 calc R . .
H42B H 0.3335 0.7063 0.3953 0.098 Uiso 1 1 calc R . .
H42C H 0.2637 0.7803 0.3830 0.098 Uiso 1 1 calc R . .
C43 C 0.1266(14) 0.6198(15) 0.0954(7) 0.047(5) Uani 1 1 d . . .
H43 H 0.1283 0.6801 0.1004 0.056 Uiso 1 1 calc R . .
C44 C 0.0924(14) 0.5892(17) 0.0520(7) 0.046(6) Uani 1 1 d . . .
H44 H 0.0628 0.6267 0.0282 0.055 Uiso 1 1 calc R . .
C45 C 0.1023(17) 0.507(2) 0.0450(9) 0.072(8) Uani 1 1 d . . .
H45 H 0.0832 0.4861 0.0158 0.086 Uiso 1 1 calc R . .
C46 C 0.1400(19) 0.453(2) 0.0798(10) 0.078(9) Uani 1 1 d . . .
H46 H 0.1470 0.3935 0.0746 0.094 Uiso 1 1 calc R . .
C47 C 0.1682(11) 0.4834(11) 0.1227(6) 0.026(4) Uani 1 1 d . . .
H47 H 0.1956 0.4451 0.1465 0.031 Uiso 1 1 calc R . .
C48 C 0.1417(13) 0.3536(12) 0.2863(7) 0.035(5) Uani 1 1 d U . .
H48 H 0.1736 0.4012 0.3026 0.042 Uiso 1 1 calc R . .
C49 C 0.0710(12) 0.3284(13) 0.2927(9) 0.046(6) Uani 1 1 d . . .
H49 H 0.0535 0.3578 0.3126 0.055 Uiso 1 1 calc R . .
C50 C 0.0278(14) 0.2588(18) 0.2688(9) 0.060(7) Uani 1 1 d . . .
H50 H -0.0188 0.2379 0.2738 0.072 Uiso 1 1 calc R . .
C51 C 0.0470(15) 0.2200(16) 0.2397(9) 0.054(6) Uani 1 1 d . . .
H51 H 0.0135 0.1753 0.2214 0.064 Uiso 1 1 calc R . .
C52 C 0.1233(14) 0.2504(15) 0.2376(8) 0.046(5) Uani 1 1 d U . .
H52 H 0.1422 0.2194 0.2188 0.055 Uiso 1 1 calc R . .
C53 C 0.4905(13) 0.3466(13) 0.2458(8) 0.042(5) Uani 1 1 d . . .
H53 H 0.4592 0.3019 0.2266 0.051 Uiso 1 1 calc R . .
C54 C 0.5721(18) 0.3598(18) 0.2512(12) 0.080(10) Uani 1 1 d . . .
H54 H 0.5971 0.3242 0.2366 0.096 Uiso 1 1 calc R . .
C55 C 0.6184(17) 0.4282(18) 0.2790(11) 0.071(9) Uani 1 1 d . . .
H55 H 0.6736 0.4415 0.2817 0.085 Uiso 1 1 calc R . .
C56 C 0.5854(18) 0.471(2) 0.3003(11) 0.079(9) Uani 1 1 d . . .
H56 H 0.6180 0.5142 0.3201 0.094 Uiso 1 1 calc R . .
C57 C 0.4990(17) 0.4567(16) 0.2953(10) 0.065(7) Uani 1 1 d . . .
H57 H 0.4756 0.4898 0.3115 0.077 Uiso 1 1 calc R . .
C58 C 0.3407(17) 0.3542(15) 0.3651(9) 0.059(7) Uani 1 1 d . . .
H58A H 0.3955 0.3244 0.3796 0.071 Uiso 1 1 calc R . .
H58B H 0.2959 0.3100 0.3535 0.071 Uiso 1 1 calc R . .
C59 C 0.325(4) 0.411(3) 0.3980(13) 0.16(2) Uani 1 1 d . . .
H59A H 0.3519 0.3881 0.4284 0.188 Uiso 1 1 calc R . .
H59B H 0.2643 0.4208 0.3899 0.188 Uiso 1 1 calc R . .
C60 C 0.372(3) 0.496(2) 0.3911(11) 0.111(14) Uani 1 1 d . . .
H60A H 0.3514 0.5484 0.4000 0.133 Uiso 1 1 calc R . .
H60B H 0.4338 0.4913 0.4078 0.133 Uiso 1 1 calc R . .
C61 C 0.349(2) 0.4942(16) 0.3431(10) 0.078(9) Uani 1 1 d . . .
H61A H 0.2945 0.5247 0.3274 0.094 Uiso 1 1 calc R . .
H61B H 0.3924 0.5233 0.3362 0.094 Uiso 1 1 calc R . .
C62 C 0.4493(14) 0.2270(16) 0.3240(9) 0.061(7) Uani 1 1 d U . .
H62A H 0.4650 0.2787 0.3430 0.073 Uiso 1 1 calc R . .
H62B H 0.4913 0.2178 0.3114 0.073 Uiso 1 1 calc R . .
C63 C 0.4413(17) 0.1468(19) 0.3494(9) 0.071(8) Uani 1 1 d . . .
H63A H 0.4113 0.1605 0.3682 0.085 Uiso 1 1 calc R . .
H63B H 0.4971 0.1220 0.3677 0.085 Uiso 1 1 calc R . .
C64 C 0.3883(16) 0.0847(16) 0.3109(10) 0.068(8) Uani 1 1 d . . .
H64A H 0.4251 0.0520 0.3002 0.082 Uiso 1 1 calc R . .
H64B H 0.3555 0.0436 0.3203 0.082 Uiso 1 1 calc R . .
C65 C 0.3295(18) 0.1456(12) 0.2750(9) 0.060(7) Uani 1 1 d U . .
H65A H 0.3301 0.1316 0.2461 0.073 Uiso 1 1 calc R . .
H65B H 0.2711 0.1409 0.2725 0.073 Uiso 1 1 calc R . .
N1 N 0.3343(9) 0.6722(9) 0.2762(5) 0.028(4) Uani 1 1 d U . .
N2 N 0.3521(10) 0.6199(10) 0.2016(6) 0.033(4) Uani 1 1 d . . .
N3 N 0.2840(10) 0.7216(10) 0.1275(5) 0.035(4) Uani 1 1 d . . .
N4 N 0.2011(10) 0.8645(9) 0.1352(5) 0.032(4) Uani 1 1 d U . .
H4 H 0.1893 0.8196 0.1477 0.038 Uiso 1 1 calc R . .
N5 N 0.0237(11) 0.8261(10) 0.1335(6) 0.036(4) Uani 1 1 d . . .
H5A H 0.0666 0.7943 0.1504 0.043 Uiso 1 1 calc R . .
N6 N -0.0176(10) 0.6539(10) 0.1267(6) 0.035(4) Uani 1 1 d . . .
N7 N 0.0640(9) 0.5541(9) 0.2002(5) 0.029(4) Uani 1 1 d . . .
N8 N 0.1713(10) 0.6325(11) 0.2754(5) 0.035(4) Uani 1 1 d . . .
N9 N 0.1578(11) 0.5645(10) 0.1309(6) 0.040(4) Uani 1 1 d . . .
N10 N 0.1675(10) 0.3129(13) 0.2576(6) 0.043(5) Uani 1 1 d U . .
N11 N 0.4523(11) 0.3937(12) 0.2664(7) 0.051(5) Uani 1 1 d . . .
O1 O 0.1723(8) 0.7283(8) 0.1891(4) 0.032(3) Uani 1 1 d . . .
O2 O 0.2474(7) 0.5040(9) 0.2300(4) 0.033(3) Uani 1 1 d . . .
O3 O 0.3633(9) 0.2346(11) 0.2892(6) 0.059(5) Uani 1 1 d . . .
O4 O 0.3410(9) 0.4074(9) 0.3297(5) 0.048(4) Uani 1 1 d . . .
Ca1 Ca 0.3006(2) 0.3669(2) 0.25331(13) 0.0275(9) Uani 1 1 d U . .
I1 I 0.26492(10) 0.26410(10) 0.16756(5) 0.0498(4) Uani 1 1 d . . .
U1 U 0.21032(4) 0.61792(5) 0.21146(2) 0.0256(2) Uani 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.33(3) . ?
C1 C2 1.41(3) . ?
C1 C40 1.54(3) . ?
C2 C3 1.36(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.42(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.38(3) . ?
C4 N1 1.39(2) . ?
C5 N2 1.25(3) . ?
C5 H5 0.9500 . ?
C6 C13 1.35(3) . ?
C6 C7 1.44(3) . ?
C6 N2 1.45(3) . ?
C7 C8 1.38(3) . ?
C7 H7 0.9500 . ?
C8 C10 1.44(3) . ?
C8 C9 1.45(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C12 1.27(3) . ?
C10 C11 1.56(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.45(3) . ?
C12 H12 0.9500 . ?
C13 N3 1.41(3) . ?
C14 N3 1.25(2) . ?
C14 C15 1.45(3) . ?
C14 H14 0.9500 . ?
C15 N4 1.32(2) . ?
C15 C16 1.42(3) . ?
C16 C17 1.40(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.40(3) . ?
C17 H17 0.9500 . ?
C18 N4 1.42(2) . ?
C18 C19 1.44(3) . ?
C19 C21 1.47(3) . ?
C19 C22 1.58(3) . ?
C19 C20 1.62(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 N5 1.35(2) . ?
C22 C23 1.43(3) . ?
C23 C24 1.34(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.40(3) . ?
C24 H24 0.9500 . ?
C25 N5 1.36(3) . ?
C25 C26 1.40(3) . ?
C26 N6 1.28(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.38(3) . ?
C27 C34 1.39(3) . ?
C27 N6 1.46(2) . ?
C28 C29 1.44(3) . ?
C28 H28 0.9500 . ?
C29 C31 1.35(3) . ?
C29 C30 1.46(3) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C33 1.38(3) . ?
C31 C32 1.60(3) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.40(3) . ?
C33 H33 0.9500 . ?
C34 N7 1.45(2) . ?
C35 N7 1.26(3) . ?
C35 C36 1.41(3) . ?
C35 H35 0.9500 . ?
C36 C37 1.37(3) . ?
C36 N8 1.39(2) . ?
C37 C38 1.44(3) . ?
C37 H37 0.9500 . ?
C38 C39 1.38(3) . ?
C38 H38 0.9500 . ?
C39 N8 1.39(3) . ?
C39 C40 1.54(3) . ?
C40 C42 1.51(3) . ?
C40 C41 1.57(3) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 N9 1.38(3) . ?
C43 C44 1.40(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.32(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.37(4) . ?
C45 H45 0.9500 . ?
C46 C47 1.39(3) . ?
C46 H46 0.9500 . ?
C47 N9 1.32(2) . ?
C47 H47 0.9500 . ?
C48 N10 1.37(3) . ?
C48 C49 1.39(3) . ?
C48 H48 0.9500 . ?
C49 C50 1.37(3) . ?
C49 H49 0.9500 . ?
C50 C51 1.30(4) . ?
C50 H50 0.9500 . ?
C51 C52 1.44(3) . ?
C51 H51 0.9500 . ?
C52 N10 1.25(3) . ?
C52 H52 0.9500 . ?
C53 N11 1.35(3) . ?
C53 C54 1.37(3) . ?
C53 H53 0.9500 . ?
C54 C55 1.42(4) . ?
C54 H54 0.9500 . ?
C55 C56 1.27(4) . ?
C55 H55 0.9500 . ?
C56 C57 1.46(4) . ?
C56 H56 0.9500 . ?
C57 N11 1.38(3) . ?
C57 H57 0.9500 . ?
C58 O4 1.44(3) . ?
C58 C59 1.52(5) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 C60 1.61(5) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 C61 1.48(4) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 O4 1.41(3) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 O3 1.48(3) . ?
C62 C63 1.54(4) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 C64 1.57(4) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 C65 1.54(3) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 O3 1.50(3) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
N1 U1 2.494(14) . ?
N2 U1 2.620(14) . ?
N4 H4 0.8800 . ?
N5 H5A 0.8800 . ?
N7 U1 2.613(14) . ?
N8 U1 2.499(15) . ?
N9 U1 2.594(18) . ?
N10 Ca1 2.522(17) . ?
N11 Ca1 2.529(18) . ?
O1 U1 1.879(12) . ?
O2 U1 1.897(13) . ?
O2 Ca1 2.325(13) . ?
O3 Ca1 2.404(16) . ?
O4 Ca1 2.433(16) . ?
Ca1 I1 3.108(4) . ?
Ca1 U1 4.221(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 112.6(19) . . ?
N1 C1 C40 122.7(19) . . ?
C2 C1 C40 125(2) . . ?
C3 C2 C1 104(2) . . ?
C3 C2 H2 128.1 . . ?
C1 C2 H2 128.1 . . ?
C2 C3 C4 110(2) . . ?
C2 C3 H3 125.0 . . ?
C4 C3 H3 125.0 . . ?
C5 C4 N1 119.6(18) . . ?
C5 C4 C3 133.7(19) . . ?
N1 C4 C3 106.6(18) . . ?
N2 C5 C4 123.3(19) . . ?
N2 C5 H5 118.4 . . ?
C4 C5 H5 118.4 . . ?
C13 C6 C7 121(2) . . ?
C13 C6 N2 119.7(19) . . ?
C7 C6 N2 119.6(19) . . ?
C8 C7 C6 122(2) . . ?
C8 C7 H7 118.8 . . ?
C6 C7 H7 118.8 . . ?
C7 C8 C10 116(2) . . ?
C7 C8 C9 122(2) . . ?
C10 C8 C9 122(2) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C12 C10 C8 120(2) . . ?
C12 C10 C11 122(2) . . ?
C8 C10 C11 119(2) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 C13 128(2) . . ?
C10 C12 H12 116.0 . . ?
C13 C12 H12 116.0 . . ?
C6 C13 N3 119.0(19) . . ?
C6 C13 C12 113(2) . . ?
N3 C13 C12 127(2) . . ?
N3 C14 C15 113.1(19) . . ?
N3 C14 H14 123.4 . . ?
C15 C14 H14 123.4 . . ?
N4 C15 C16 106.0(16) . . ?
N4 C15 C14 125.7(18) . . ?
C16 C15 C14 128.1(19) . . ?
C17 C16 C15 110.3(18) . . ?
C17 C16 H16 124.8 . . ?
C15 C16 H16 124.8 . . ?
C16 C17 C18 105.1(17) . . ?
C16 C17 H17 127.4 . . ?
C18 C17 H17 127.4 . . ?
C17 C18 N4 107.4(17) . . ?
C17 C18 C19 126.6(18) . . ?
N4 C18 C19 125.9(17) . . ?
C18 C19 C21 116.4(19) . . ?
C18 C19 C22 111.1(15) . . ?
C21 C19 C22 112.2(17) . . ?
C18 C19 C20 109.7(16) . . ?
C21 C19 C20 104.8(17) . . ?
C22 C19 C20 101.3(17) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N5 C22 C23 107.7(19) . . ?
N5 C22 C19 125.6(19) . . ?
C23 C22 C19 126.3(17) . . ?
C24 C23 C22 106.6(18) . . ?
C24 C23 H23 126.7 . . ?
C22 C23 H23 126.7 . . ?
C23 C24 C25 109(2) . . ?
C23 C24 H24 125.3 . . ?
C25 C24 H24 125.3 . . ?
N5 C25 C26 122(2) . . ?
N5 C25 C24 106.9(17) . . ?
C26 C25 C24 131(2) . . ?
N6 C26 C25 120(2) . . ?
N6 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C28 C27 C34 121.7(18) . . ?
C28 C27 N6 123.1(18) . . ?
C34 C27 N6 115.1(18) . . ?
C27 C28 C29 121(2) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
C31 C29 C28 115(2) . . ?
C31 C29 C30 127(2) . . ?
C28 C29 C30 118(2) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 C33 126(2) . . ?
C29 C31 C32 117(2) . . ?
C33 C31 C32 117(2) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 C34 118(2) . . ?
C31 C33 H33 120.8 . . ?
C34 C33 H33 120.8 . . ?
C27 C34 C33 118.2(19) . . ?
C27 C34 N7 121.0(17) . . ?
C33 C34 N7 120.7(17) . . ?
N7 C35 C36 122(2) . . ?
N7 C35 H35 119.0 . . ?
C36 C35 H35 119.0 . . ?
C37 C36 N8 110.8(19) . . ?
C37 C36 C35 131.4(19) . . ?
N8 C36 C35 117.7(18) . . ?
C36 C37 C38 106.3(18) . . ?
C36 C37 H37 126.9 . . ?
C38 C37 H37 126.9 . . ?
C39 C38 C37 106.7(18) . . ?
C39 C38 H38 126.6 . . ?
C37 C38 H38 126.6 . . ?
C38 C39 N8 109.9(18) . . ?
C38 C39 C40 129.8(19) . . ?
N8 C39 C40 120.2(16) . . ?
C42 C40 C1 113.4(18) . . ?
C42 C40 C39 109.7(19) . . ?
C1 C40 C39 111.1(15) . . ?
C42 C40 C41 109.2(17) . . ?
C1 C40 C41 107.4(18) . . ?
C39 C40 C41 105.8(16) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N9 C43 C44 122(2) . . ?
N9 C43 H43 119.2 . . ?
C44 C43 H43 119.2 . . ?
C45 C44 C43 119(2) . . ?
C45 C44 H44 120.7 . . ?
C43 C44 H44 120.7 . . ?
C44 C45 C46 120(3) . . ?
C44 C45 H45 120.0 . . ?
C46 C45 H45 120.0 . . ?
C45 C46 C47 120(3) . . ?
C45 C46 H46 119.9 . . ?
C47 C46 H46 119.9 . . ?
N9 C47 C46 121(2) . . ?
N9 C47 H47 119.3 . . ?
C46 C47 H47 119.3 . . ?
N10 C48 C49 122.9(19) . . ?
N10 C48 H48 118.6 . . ?
C49 C48 H48 118.6 . . ?
C50 C49 C48 116(2) . . ?
C50 C49 H49 121.9 . . ?
C48 C49 H49 121.9 . . ?
C51 C50 C49 124(2) . . ?
C51 C50 H50 118.2 . . ?
C49 C50 H50 118.2 . . ?
C50 C51 C52 114(2) . . ?
C50 C51 H51 123.0 . . ?
C52 C51 H51 123.0 . . ?
N10 C52 C51 128(2) . . ?
N10 C52 H52 116.2 . . ?
C51 C52 H52 116.2 . . ?
N11 C53 C54 123(2) . . ?
N11 C53 H53 118.3 . . ?
C54 C53 H53 118.3 . . ?
C53 C54 C55 118(3) . . ?
C53 C54 H54 120.8 . . ?
C55 C54 H54 120.8 . . ?
C56 C55 C54 119(3) . . ?
C56 C55 H55 120.3 . . ?
C54 C55 H55 120.3 . . ?
C55 C56 C57 123(3) . . ?
C55 C56 H56 118.7 . . ?
C57 C56 H56 118.7 . . ?
N11 C57 C56 118(3) . . ?
N11 C57 H57 120.9 . . ?
C56 C57 H57 120.9 . . ?
O4 C58 C59 109(2) . . ?
O4 C58 H58A 109.9 . . ?
C59 C58 H58A 109.9 . . ?
O4 C58 H58B 109.9 . . ?
C59 C58 H58B 109.9 . . ?
H58A C58 H58B 108.3 . . ?
C58 C59 C60 97(2) . . ?
C58 C59 H59A 112.4 . . ?
C60 C59 H59A 112.4 . . ?
C58 C59 H59B 112.4 . . ?
C60 C59 H59B 112.4 . . ?
H59A C59 H59B 110.0 . . ?
C61 C60 C59 102(3) . . ?
C61 C60 H60A 111.3 . . ?
C59 C60 H60A 111.3 . . ?
C61 C60 H60B 111.3 . . ?
C59 C60 H60B 111.3 . . ?
H60A C60 H60B 109.2 . . ?
O4 C61 C60 108(2) . . ?
O4 C61 H61A 110.2 . . ?
C60 C61 H61A 110.2 . . ?
O4 C61 H61B 110.2 . . ?
C60 C61 H61B 110.2 . . ?
H61A C61 H61B 108.5 . . ?
O3 C62 C63 102(2) . . ?
O3 C62 H62A 111.4 . . ?
C63 C62 H62A 111.4 . . ?
O3 C62 H62B 111.4 . . ?
C63 C62 H62B 111.4 . . ?
H62A C62 H62B 109.3 . . ?
C62 C63 C64 102(2) . . ?
C62 C63 H63A 111.4 . . ?
C64 C63 H63A 111.4 . . ?
C62 C63 H63B 111.4 . . ?
C64 C63 H63B 111.4 . . ?
H63A C63 H63B 109.3 . . ?
C65 C64 C63 104(2) . . ?
C65 C64 H64A 111.0 . . ?
C63 C64 H64A 111.0 . . ?
C65 C64 H64B 111.0 . . ?
C63 C64 H64B 111.0 . . ?
H64A C64 H64B 109.0 . . ?
O3 C65 C64 106(2) . . ?
O3 C65 H65A 110.6 . . ?
C64 C65 H65A 110.6 . . ?
O3 C65 H65B 110.6 . . ?
C64 C65 H65B 110.6 . . ?
H65A C65 H65B 108.7 . . ?
C1 N1 C4 106.7(16) . . ?
C1 N1 U1 137.4(13) . . ?
C4 N1 U1 115.3(12) . . ?
C5 N2 C6 122.8(17) . . ?
C5 N2 U1 113.4(13) . . ?
C6 N2 U1 122.3(12) . . ?
C14 N3 C13 117.5(17) . . ?
C15 N4 C18 111.1(16) . . ?
C15 N4 H4 124.4 . . ?
C18 N4 H4 124.4 . . ?
C22 N5 C25 109.4(18) . . ?
C22 N5 H5A 125.3 . . ?
C25 N5 H5A 125.3 . . ?
C26 N6 C27 119.9(18) . . ?
C35 N7 C34 118.7(17) . . ?
C35 N7 U1 113.7(13) . . ?
C34 N7 U1 124.5(12) . . ?
C39 N8 C36 106.0(15) . . ?
C39 N8 U1 135.7(12) . . ?
C36 N8 U1 114.9(13) . . ?
C47 N9 C43 117.1(18) . . ?
C47 N9 U1 120.0(14) . . ?
C43 N9 U1 122.5(13) . . ?
C52 N10 C48 115.1(18) . . ?
C52 N10 Ca1 127.6(14) . . ?
C48 N10 Ca1 117.2(14) . . ?
C53 N11 C57 118(2) . . ?
C53 N11 Ca1 121.3(16) . . ?
C57 N11 Ca1 120.8(16) . . ?
U1 O2 Ca1 176.7(6) . . ?
C62 O3 C65 108.4(17) . . ?
C62 O3 Ca1 124.6(14) . . ?
C65 O3 Ca1 126.2(13) . . ?
C61 O4 C58 108.8(19) . . ?
C61 O4 Ca1 121.8(15) . . ?
C58 O4 Ca1 127.8(14) . . ?
O2 Ca1 O3 170.8(6) . . ?
O2 Ca1 O4 91.1(5) . . ?
O3 Ca1 O4 79.7(5) . . ?
O2 Ca1 N10 94.3(5) . . ?
O3 Ca1 N10 85.9(6) . . ?
O4 Ca1 N10 84.6(5) . . ?
O2 Ca1 N11 98.7(5) . . ?
O3 Ca1 N11 79.9(6) . . ?
O4 Ca1 N11 86.7(6) . . ?
N10 Ca1 N11 164.4(6) . . ?
O2 Ca1 I1 105.1(4) . . ?
O3 Ca1 I1 84.1(4) . . ?
O4 Ca1 I1 163.7(4) . . ?
N10 Ca1 I1 92.2(4) . . ?
N11 Ca1 I1 92.6(5) . . ?
O2 Ca1 U1 1.5(3) . . ?
O3 Ca1 U1 170.4(4) . . ?
O4 Ca1 U1 91.0(3) . . ?
N10 Ca1 U1 95.7(5) . . ?
N11 Ca1 U1 97.3(4) . . ?
I1 Ca1 U1 105.27(10) . . ?
O1 U1 O2 176.0(6) . . ?
O1 U1 N1 94.2(5) . . ?
O2 U1 N1 88.6(5) . . ?
O1 U1 N8 94.6(6) . . ?
O2 U1 N8 89.0(6) . . ?
N1 U1 N8 70.8(5) . . ?
O1 U1 N9 87.9(5) . . ?
O2 U1 N9 88.1(5) . . ?
N1 U1 N9 144.9(5) . . ?
N8 U1 N9 144.0(5) . . ?
O1 U1 N7 97.2(5) . . ?
O2 U1 N7 82.8(5) . . ?
N1 U1 N7 134.4(5) . . ?
N8 U1 N7 64.4(5) . . ?
N9 U1 N7 79.6(5) . . ?
O1 U1 N2 97.8(5) . . ?
O2 U1 N2 80.8(5) . . ?
N1 U1 N2 65.1(5) . . ?
N8 U1 N2 134.8(5) . . ?
N9 U1 N2 79.9(5) . . ?
N7 U1 N2 154.1(5) . . ?
O1 U1 Ca1 175.6(4) . . ?
O2 U1 Ca1 1.8(3) . . ?
N1 U1 Ca1 87.3(3) . . ?
N8 U1 Ca1 89.8(4) . . ?
N9 U1 Ca1 88.5(4) . . ?
N7 U1 Ca1 84.6(3) . . ?
N2 U1 Ca1 79.1(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
N1 C1 C2 C3 4(2) . . . . ?
C40 C1 C2 C3 -178(2) . . . . ?
C1 C2 C3 C4 -1(3) . . . . ?
C2 C3 C4 C5 179(2) . . . . ?
C2 C3 C4 N1 -2(2) . . . . ?
N1 C4 C5 N2 5(3) . . . . ?
C3 C4 C5 N2 -176(2) . . . . ?
C13 C6 C7 C8 -1(3) . . . . ?
N2 C6 C7 C8 179(2) . . . . ?
C6 C7 C8 C10 -2(3) . . . . ?
C6 C7 C8 C9 -178(2) . . . . ?
C7 C8 C10 C12 2(3) . . . . ?
C9 C8 C10 C12 178(2) . . . . ?
C7 C8 C10 C11 179(2) . . . . ?
C9 C8 C10 C11 -6(3) . . . . ?
C8 C10 C12 C13 1(3) . . . . ?
C11 C10 C12 C13 -175(2) . . . . ?
C7 C6 C13 N3 176.0(18) . . . . ?
N2 C6 C13 N3 -5(3) . . . . ?
C7 C6 C13 C12 4(3) . . . . ?
N2 C6 C13 C12 -176.4(17) . . . . ?
C10 C12 C13 C6 -5(3) . . . . ?
C10 C12 C13 N3 -176(2) . . . . ?
N3 C14 C15 N4 -4(3) . . . . ?
N3 C14 C15 C16 -177(2) . . . . ?
N4 C15 C16 C17 2(3) . . . . ?
C14 C15 C16 C17 176(2) . . . . ?
C15 C16 C17 C18 -1(3) . . . . ?
C16 C17 C18 N4 -1(3) . . . . ?
C16 C17 C18 C19 -176(2) . . . . ?
C17 C18 C19 C21 -11(3) . . . . ?
N4 C18 C19 C21 175(2) . . . . ?
C17 C18 C19 C22 119(2) . . . . ?
N4 C18 C19 C22 -55(3) . . . . ?
C17 C18 C19 C20 -129(2) . . . . ?
N4 C18 C19 C20 56(3) . . . . ?
C18 C19 C22 N5 59(3) . . . . ?
C21 C19 C22 N5 -169(2) . . . . ?
C20 C19 C22 N5 -58(2) . . . . ?
C18 C19 C22 C23 -113(2) . . . . ?
C21 C19 C22 C23 19(3) . . . . ?
C20 C19 C22 C23 130(2) . . . . ?
N5 C22 C23 C24 -2(3) . . . . ?
C19 C22 C23 C24 171(2) . . . . ?
C22 C23 C24 C25 0(3) . . . . ?
C23 C24 C25 N5 1(3) . . . . ?
C23 C24 C25 C26 177(3) . . . . ?
N5 C25 C26 N6 -3(4) . . . . ?
C24 C25 C26 N6 -178(2) . . . . ?
C34 C27 C28 C29 -1(3) . . . . ?
N6 C27 C28 C29 174.8(19) . . . . ?
C27 C28 C29 C31 3(3) . . . . ?
C27 C28 C29 C30 179(2) . . . . ?
C28 C29 C31 C33 -5(3) . . . . ?
C30 C29 C31 C33 179(2) . . . . ?
C28 C29 C31 C32 179(2) . . . . ?
C30 C29 C31 C32 3(4) . . . . ?
C29 C31 C33 C34 5(3) . . . . ?
C32 C31 C33 C34 -179(2) . . . . ?
C28 C27 C34 C33 1(3) . . . . ?
N6 C27 C34 C33 -175.1(17) . . . . ?
C28 C27 C34 N7 177.3(19) . . . . ?
N6 C27 C34 N7 1(3) . . . . ?
C31 C33 C34 C27 -3(3) . . . . ?
C31 C33 C34 N7 -179.1(18) . . . . ?
N7 C35 C36 C37 177.4(19) . . . . ?
N7 C35 C36 N8 1(3) . . . . ?
N8 C36 C37 C38 -1(2) . . . . ?
C35 C36 C37 C38 -177(2) . . . . ?
C36 C37 C38 C39 4(2) . . . . ?
C37 C38 C39 N8 -5(2) . . . . ?
C37 C38 C39 C40 177.6(18) . . . . ?
N1 C1 C40 C42 173(2) . . . . ?
C2 C1 C40 C42 -5(3) . . . . ?
N1 C1 C40 C39 49(3) . . . . ?
C2 C1 C40 C39 -129(2) . . . . ?
N1 C1 C40 C41 -66(2) . . . . ?
C2 C1 C40 C41 116(2) . . . . ?
C38 C39 C40 C42 -3(3) . . . . ?
N8 C39 C40 C42 179.7(18) . . . . ?
C38 C39 C40 C1 123(2) . . . . ?
N8 C39 C40 C1 -54(2) . . . . ?
C38 C39 C40 C41 -121(2) . . . . ?
N8 C39 C40 C41 62(2) . . . . ?
N9 C43 C44 C45 -11(4) . . . . ?
C43 C44 C45 C46 5(4) . . . . ?
C44 C45 C46 C47 0(4) . . . . ?
C45 C46 C47 N9 2(4) . . . . ?
N10 C48 C49 C50 1(3) . . . . ?
C48 C49 C50 C51 -4(4) . . . . ?
C49 C50 C51 C52 6(4) . . . . ?
C50 C51 C52 N10 -6(4) . . . . ?
N11 C53 C54 C55 -2(4) . . . . ?
C53 C54 C55 C56 5(4) . . . . ?
C54 C55 C56 C57 -4(5) . . . . ?
C55 C56 C57 N11 0(5) . . . . ?
O4 C58 C59 C60 -32(4) . . . . ?
C58 C59 C60 C61 38(4) . . . . ?
C59 C60 C61 O4 -33(4) . . . . ?
O3 C62 C63 C64 43(2) . . . . ?
C62 C63 C64 C65 -34(3) . . . . ?
C63 C64 C65 O3 12(3) . . . . ?
C2 C1 N1 C4 -5(2) . . . . ?
C40 C1 N1 C4 176.9(17) . . . . ?
C2 C1 N1 U1 165.1(14) . . . . ?
C40 C1 N1 U1 -13(3) . . . . ?
C5 C4 N1 C1 -176.2(18) . . . . ?
C3 C4 N1 C1 4(2) . . . . ?
C5 C4 N1 U1 11(2) . . . . ?
C3 C4 N1 U1 -168.7(13) . . . . ?
C4 C5 N2 C6 176.8(19) . . . . ?
C4 C5 N2 U1 -17(2) . . . . ?
C13 C6 N2 C5 -121(2) . . . . ?
C7 C6 N2 C5 58(3) . . . . ?
C13 C6 N2 U1 74(2) . . . . ?
C7 C6 N2 U1 -106.9(18) . . . . ?
C15 C14 N3 C13 -177.3(18) . . . . ?
C6 C13 N3 C14 141(2) . . . . ?
C12 C13 N3 C14 -49(3) . . . . ?
C16 C15 N4 C18 -3(2) . . . . ?
C14 C15 N4 C18 -177(2) . . . . ?
C17 C18 N4 C15 3(3) . . . . ?
C19 C18 N4 C15 178(2) . . . . ?
C23 C22 N5 C25 2(3) . . . . ?
C19 C22 N5 C25 -170.6(19) . . . . ?
C26 C25 N5 C22 -178(2) . . . . ?
C24 C25 N5 C22 -2(3) . . . . ?
C25 C26 N6 C27 -177(2) . . . . ?
C28 C27 N6 C26 35(3) . . . . ?
C34 C27 N6 C26 -149(2) . . . . ?
C36 C35 N7 C34 -179.3(17) . . . . ?
C36 C35 N7 U1 20(2) . . . . ?
C27 C34 N7 C35 130.7(19) . . . . ?
C33 C34 N7 C35 -53(2) . . . . ?
C27 C34 N7 U1 -70(2) . . . . ?
C33 C34 N7 U1 105.6(18) . . . . ?
C38 C39 N8 C36 4(2) . . . . ?
C40 C39 N8 C36 -178.0(16) . . . . ?
C38 C39 N8 U1 -152.7(14) . . . . ?
C40 C39 N8 U1 25(3) . . . . ?
C37 C36 N8 C39 -2(2) . . . . ?
C35 C36 N8 C39 175.1(17) . . . . ?
C37 C36 N8 U1 160.6(12) . . . . ?
C35 C36 N8 U1 -22(2) . . . . ?
C46 C47 N9 C43 -7(3) . . . . ?
C46 C47 N9 U1 179.4(17) . . . . ?
C44 C43 N9 C47 12(3) . . . . ?
C44 C43 N9 U1 -175.0(15) . . . . ?
C51 C52 N10 C48 4(4) . . . . ?
C51 C52 N10 Ca1 -179.4(18) . . . . ?
C49 C48 N10 C52 -1(3) . . . . ?
C49 C48 N10 Ca1 -178.0(16) . . . . ?
C54 C53 N11 C57 -2(4) . . . . ?
C54 C53 N11 Ca1 178.6(19) . . . . ?
C56 C57 N11 C53 3(4) . . . . ?
C56 C57 N11 Ca1 -177.9(19) . . . . ?
C63 C62 O3 C65 -37(3) . . . . ?
C63 C62 O3 Ca1 153.5(16) . . . . ?
C64 C65 O3 C62 15(3) . . . . ?
C64 C65 O3 Ca1 -175.3(16) . . . . ?
C60 C61 O4 C58 12(3) . . . . ?
C60 C61 O4 Ca1 179(2) . . . . ?
C59 C58 O4 C61 15(4) . . . . ?
C59 C58 O4 Ca1 -150(3) . . . . ?
U1 O2 Ca1 O3 79(14) . . . . ?
U1 O2 Ca1 O4 85(14) . . . . ?
U1 O2 Ca1 N10 170(14) . . . . ?
U1 O2 Ca1 N11 -2(14) . . . . ?
U1 O2 Ca1 I1 -97(14) . . . . ?
C62 O3 Ca1 O2 -49(4) . . . . ?
C65 O3 Ca1 O2 143(3) . . . . ?
C62 O3 Ca1 O4 -54.8(17) . . . . ?
C65 O3 Ca1 O4 137.1(19) . . . . ?
C62 O3 Ca1 N10 -140.0(18) . . . . ?
C65 O3 Ca1 N10 51.9(19) . . . . ?
C62 O3 Ca1 N11 33.7(17) . . . . ?
C65 O3 Ca1 N11 -134(2) . . . . ?
C62 O3 Ca1 I1 127.3(17) . . . . ?
C65 O3 Ca1 I1 -40.7(19) . . . . ?
C62 O3 Ca1 U1 -40(4) . . . . ?
C65 O3 Ca1 U1 152(2) . . . . ?
C61 O4 Ca1 O2 -18(2) . . . . ?
C58 O4 Ca1 O2 145.7(17) . . . . ?
C61 O4 Ca1 O3 161(2) . . . . ?
C58 O4 Ca1 O3 -35.3(17) . . . . ?
C61 O4 Ca1 N10 -112(2) . . . . ?
C58 O4 Ca1 N10 51.5(18) . . . . ?
C61 O4 Ca1 N11 81(2) . . . . ?
C58 O4 Ca1 N11 -115.6(18) . . . . ?
C61 O4 Ca1 I1 168.6(18) . . . . ?
C58 O4 Ca1 I1 -28(3) . . . . ?
C61 O4 Ca1 U1 -17(2) . . . . ?
C58 O4 Ca1 U1 147.1(17) . . . . ?
C52 N10 Ca1 O2 121(2) . . . . ?
C48 N10 Ca1 O2 -61.5(15) . . . . ?
C52 N10 Ca1 O3 -68(2) . . . . ?
C48 N10 Ca1 O3 109.3(15) . . . . ?
C52 N10 Ca1 O4 -148(2) . . . . ?
C48 N10 Ca1 O4 29.2(15) . . . . ?
C52 N10 Ca1 N11 -92(3) . . . . ?
C48 N10 Ca1 N11 85(3) . . . . ?
C52 N10 Ca1 I1 16(2) . . . . ?
C48 N10 Ca1 I1 -166.8(14) . . . . ?
C52 N10 Ca1 U1 121.7(19) . . . . ?
C48 N10 Ca1 U1 -61.2(15) . . . . ?
C53 N11 Ca1 O2 -122.9(16) . . . . ?
C57 N11 Ca1 O2 57.8(18) . . . . ?
C53 N11 Ca1 O3 66.3(16) . . . . ?
C57 N11 Ca1 O3 -113.0(18) . . . . ?
C53 N11 Ca1 O4 146.5(16) . . . . ?
C57 N11 Ca1 O4 -32.8(18) . . . . ?
C53 N11 Ca1 N10 91(3) . . . . ?
C57 N11 Ca1 N10 -89(3) . . . . ?
C53 N11 Ca1 I1 -17.2(16) . . . . ?
C57 N11 Ca1 I1 163.4(18) . . . . ?
C53 N11 Ca1 U1 -123.0(16) . . . . ?
C57 N11 Ca1 U1 57.7(18) . . . . ?
Ca1 O2 U1 O1 89(16) . . . . ?
Ca1 O2 U1 N1 -45(14) . . . . ?
Ca1 O2 U1 N8 -116(14) . . . . ?
Ca1 O2 U1 N9 100(14) . . . . ?
Ca1 O2 U1 N7 180(100) . . . . ?
Ca1 O2 U1 N2 20(14) . . . . ?
C1 N1 U1 O1 80.9(19) . . . . ?
C4 N1 U1 O1 -109.5(13) . . . . ?
C1 N1 U1 O2 -102.0(19) . . . . ?
C4 N1 U1 O2 67.7(13) . . . . ?
C1 N1 U1 N8 -12.6(18) . . . . ?
C4 N1 U1 N8 157.1(14) . . . . ?
C1 N1 U1 N9 173.3(16) . . . . ?
C4 N1 U1 N9 -17.0(17) . . . . ?
C1 N1 U1 N7 -23(2) . . . . ?
C4 N1 U1 N7 146.2(12) . . . . ?
C1 N1 U1 N2 178(2) . . . . ?
C4 N1 U1 N2 -12.8(12) . . . . ?
C1 N1 U1 Ca1 -103.3(18) . . . . ?
C4 N1 U1 Ca1 66.4(12) . . . . ?
C39 N8 U1 O1 -87.1(18) . . . . ?
C36 N8 U1 O1 117.5(13) . . . . ?
C39 N8 U1 O2 94.6(18) . . . . ?
C36 N8 U1 O2 -60.8(13) . . . . ?
C39 N8 U1 N1 5.8(17) . . . . ?
C36 N8 U1 N1 -149.6(14) . . . . ?
C39 N8 U1 N9 -180.0(15) . . . . ?
C36 N8 U1 N9 24.6(18) . . . . ?
C39 N8 U1 N7 177(2) . . . . ?
C36 N8 U1 N7 21.7(12) . . . . ?
C39 N8 U1 N2 19(2) . . . . ?
C36 N8 U1 N2 -136.7(12) . . . . ?
C39 N8 U1 Ca1 93.0(18) . . . . ?
C36 N8 U1 Ca1 -62.4(13) . . . . ?
C47 N9 U1 O1 178.6(15) . . . . ?
C43 N9 U1 O1 5.7(16) . . . . ?
C47 N9 U1 O2 -0.7(15) . . . . ?
C43 N9 U1 O2 -173.6(16) . . . . ?
C47 N9 U1 N1 84.2(17) . . . . ?
C43 N9 U1 N1 -88.8(17) . . . . ?
C47 N9 U1 N8 -86.4(16) . . . . ?
C43 N9 U1 N8 100.7(17) . . . . ?
C47 N9 U1 N7 -83.7(15) . . . . ?
C43 N9 U1 N7 103.3(16) . . . . ?
C47 N9 U1 N2 80.3(15) . . . . ?
C43 N9 U1 N2 -92.7(16) . . . . ?
C47 N9 U1 Ca1 1.1(14) . . . . ?
C43 N9 U1 Ca1 -171.8(16) . . . . ?
C35 N7 U1 O1 -113.3(14) . . . . ?
C34 N7 U1 O1 87.0(13) . . . . ?
C35 N7 U1 O2 70.8(14) . . . . ?
C34 N7 U1 O2 -89.0(14) . . . . ?
C35 N7 U1 N1 -10.1(16) . . . . ?
C34 N7 U1 N1 -169.8(12) . . . . ?
C35 N7 U1 N8 -21.5(13) . . . . ?
C34 N7 U1 N8 178.7(15) . . . . ?
C35 N7 U1 N9 160.2(14) . . . . ?
C34 N7 U1 N9 0.4(13) . . . . ?
C35 N7 U1 N2 121.8(16) . . . . ?
C34 N7 U1 N2 -37.9(19) . . . . ?
C35 N7 U1 Ca1 70.8(13) . . . . ?
C34 N7 U1 Ca1 -89.0(13) . . . . ?
C5 N2 U1 O1 106.3(15) . . . . ?
C6 N2 U1 O1 -87.2(15) . . . . ?
C5 N2 U1 O2 -77.5(15) . . . . ?
C6 N2 U1 O2 89.0(15) . . . . ?
C5 N2 U1 N1 15.2(14) . . . . ?
C6 N2 U1 N1 -178.3(16) . . . . ?
C5 N2 U1 N8 1.7(18) . . . . ?
C6 N2 U1 N8 168.2(14) . . . . ?
C5 N2 U1 N9 -167.3(15) . . . . ?
C6 N2 U1 N9 -0.7(15) . . . . ?
C5 N2 U1 N7 -128.9(15) . . . . ?
C6 N2 U1 N7 38(2) . . . . ?
C5 N2 U1 Ca1 -76.9(14) . . . . ?
C6 N2 U1 Ca1 89.6(15) . . . . ?
O2 Ca1 U1 O1 -115(15) . . . . ?
O3 Ca1 U1 O1 136(6) . . . . ?
O4 Ca1 U1 O1 150(5) . . . . ?
N10 Ca1 U1 O1 -125(5) . . . . ?
N11 Ca1 U1 O1 63(5) . . . . ?
I1 Ca1 U1 O1 -31(5) . . . . ?
O3 Ca1 U1 O2 -110(14) . . . . ?
O4 Ca1 U1 O2 -95(14) . . . . ?
N10 Ca1 U1 O2 -11(14) . . . . ?
N11 Ca1 U1 O2 178(100) . . . . ?
I1 Ca1 U1 O2 83(14) . . . . ?
O2 Ca1 U1 N1 135(14) . . . . ?
O3 Ca1 U1 N1 25(3) . . . . ?
O4 Ca1 U1 N1 39.5(5) . . . . ?
N10 Ca1 U1 N1 124.1(6) . . . . ?
N11 Ca1 U1 N1 -47.3(6) . . . . ?
I1 Ca1 U1 N1 -142.0(4) . . . . ?
O2 Ca1 U1 N8 64(14) . . . . ?
O3 Ca1 U1 N8 -46(3) . . . . ?
O4 Ca1 U1 N8 -31.3(5) . . . . ?
N10 Ca1 U1 N8 53.4(6) . . . . ?
N11 Ca1 U1 N8 -118.1(6) . . . . ?
I1 Ca1 U1 N8 147.2(4) . . . . ?
O2 Ca1 U1 N9 -80(14) . . . . ?
O3 Ca1 U1 N9 170(3) . . . . ?
O4 Ca1 U1 N9 -175.3(5) . . . . ?
N10 Ca1 U1 N9 -90.7(6) . . . . ?
N11 Ca1 U1 N9 97.9(6) . . . . ?
I1 Ca1 U1 N9 3.2(4) . . . . ?
O2 Ca1 U1 N7 0(14) . . . . ?
O3 Ca1 U1 N7 -110(3) . . . . ?
O4 Ca1 U1 N7 -95.6(5) . . . . ?
N10 Ca1 U1 N7 -11.0(5) . . . . ?
N11 Ca1 U1 N7 177.6(6) . . . . ?
I1 Ca1 U1 N7 82.9(4) . . . . ?
O2 Ca1 U1 N2 -160(14) . . . . ?
O3 Ca1 U1 N2 90(3) . . . . ?
O4 Ca1 U1 N2 104.7(5) . . . . ?
N10 Ca1 U1 N2 -170.7(6) . . . . ?
N11 Ca1 U1 N2 17.8(6) . . . . ?
I1 Ca1 U1 N2 -76.8(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        23.25
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         3.217
_refine_diff_density_min         -9.138
_refine_diff_density_rms         0.256

_vrf_PLAT602_p14107_reint_ref-sr 
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure!
RESPONSE: Due to strongly disordered tetrahydrofuran 
solvent molecules the model was refined using SQUEEZE, 
leaving very large solvent accessible voids, hence the alert.
;
####################################################################### 
# 
# 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_p15015ref
_database_code_depnum_ccdc_archive 'CCDC 1883752'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;university of edinburgh
United Kingdom
;
_audit_update_record             
;
2018-12-07 deposited with the CCDC.	2019-08-27 downloaded from the CCDC.
;
_audit_creation_date             2015-02-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C62 H62 N12 O2 Rb U, 3(C5 H5 N)'
_chemical_formula_sum            'C77 H77 N15 O2 Rb U'
_chemical_formula_weight         1568.03
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C64 H64 N12 O2 Rb1 U1'
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'
Rb Rb -0.9393 2.9676 '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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   13.6821(2)
_cell_length_b                   21.8875(3)
_cell_length_c                   24.2440(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7260.27(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    80366
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      32.5830
_cell_measurement_theta_min      3.4820
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.958
_exptl_absorpt_correction_T_max  0.681
_exptl_absorpt_correction_T_min  0.425
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3156
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 'from conc. pyridine-d5 solution'
_exptl_crystal_size_max          1.2579
_exptl_crystal_size_mid          0.8559
_exptl_crystal_size_min          0.5198
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0764
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            216174
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.072
_diffrn_ambient_temperature      170.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -99.00  -13.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.6393  151.0000 -114.8201 172

#__ type_ start__ end____ width___ exp.time_
  2 omega  -40.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518  -57.0000 -150.0000 178

#__ type_ start__ end____ width___ exp.time_
  3 omega  -25.00   70.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518  -99.0000  150.0000 190

#__ type_ start__ end____ width___ exp.time_
  4 omega    7.00   97.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518   57.0000   90.0000 180

#__ type_ start__ end____ width___ exp.time_
  5 omega  -45.00   73.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518  -19.0000  -90.0000 236

#__ type_ start__ end____ width___ exp.time_
  6 omega  -96.00    4.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.6393  -77.0000  -30.0000 200

#__ type_ start__ end____ width___ exp.time_
  7 omega  -46.00   43.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.6393   57.0000   60.0000 178

#__ type_ start__ end____ width___ exp.time_
  8 omega -102.00  -34.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.6393 -179.0000  -60.0000 136

#__ type_ start__ end____ width___ exp.time_
  9 omega   -2.00   99.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518   77.0000 -180.0000 202

#__ type_ start__ end____ width___ exp.time_
 10 omega   -2.00   99.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518   77.0000   90.0000 202

#__ type_ start__ end____ width___ exp.time_
 11 omega   34.00  105.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518  179.0000  -90.0000 142

#__ type_ start__ end____ width___ exp.time_
 12 omega    7.00   97.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518   57.0000    0.0000 180

#__ type_ start__ end____ width___ exp.time_
 13 omega   -2.00   99.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518   77.0000  -90.0000 202

#__ type_ start__ end____ width___ exp.time_
 14 omega  -25.00   70.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518  -99.0000   30.0000 190

#__ type_ start__ end____ width___ exp.time_
 15 omega  -42.00   59.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518  -77.0000 -150.0000 202

#__ type_ start__ end____ width___ exp.time_
 16 omega    3.00  101.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4518   37.0000 -150.0000 196
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0107609000
_diffrn_orient_matrix_UB_12      0.0104059000
_diffrn_orient_matrix_UB_13      -0.0270435000
_diffrn_orient_matrix_UB_21      -0.0439954000
_diffrn_orient_matrix_UB_22      0.0171085000
_diffrn_orient_matrix_UB_23      -0.0002119000
_diffrn_orient_matrix_UB_31      0.0251670000
_diffrn_orient_matrix_UB_32      0.0254952000
_diffrn_orient_matrix_UB_33      0.0111724000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.836
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                15775
_reflns_number_total             16642
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_refine_diff_density_max         1.243
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 
;
 Flack x determined using 6849 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0820(16)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     873
_refine_ls_number_reflns         16642
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0247
_refine_ls_restrained_S_all      1.051
_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)+(0.0206P)²+6.1773P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0538
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C36(H36), C38(H38), C39(H39), C48(H48), C49(H49), C50(H50),
 C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58),
  C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C67(H), C78(HA), N4(H4),
 C69(HB), C2(H2), C3(H3), C5(H5), C7(H7), C12(H12), C15(H15), C17(H17),
 C18(H18), C25(H25), C27(H27), C29(H29), C34(H34), C44(H44), C45(H45), C46(H46),
  C47(H47), C64(HC), C65(HD), C66(HE), C68(HF), C70(HG), C71(HH), C72(HI),
 C73(HJ), N5(H5A), C74(HK), C75(HL), C76(HM), C77(HN)
2.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C21(H21A,H21B,H21C), C9(H9A,H9B,H9C), C22(H22A,H22B,
 H22C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
C11 C -0.1521(5) -1.1300(2) -0.2057(2) 0.0466(15) Uani 1 1 d . . . . .
H11A H -0.0807 -1.1323 -0.2073 0.070 Uiso 1 1 calc GR . . . .
H11B H -0.1771 -1.1135 -0.2406 0.070 Uiso 1 1 calc GR . . . .
H11C H -0.1790 -1.1710 -0.1997 0.070 Uiso 1 1 calc GR . . . .
C21 C -0.5171(4) -1.1958(2) 0.20637(17) 0.0365(11) Uani 1 1 d . . . . .
H21A H -0.4599 -1.1876 0.2296 0.055 Uiso 1 1 calc GR . . . .
H21B H -0.5185 -1.2391 0.1964 0.055 Uiso 1 1 calc GR . . . .
H21C H -0.5767 -1.1853 0.2267 0.055 Uiso 1 1 calc GR . . . .
C23 C -0.6019(3) -1.1673(2) 0.11903(17) 0.0226(9) Uani 1 1 d . . . . .
C24 C -0.6766(4) -1.2090(2) 0.12457(19) 0.0298(11) Uani 1 1 d . . . . .
H24 H -0.6835 -1.2379 0.1536 0.036 Uiso 1 1 calc R . . . .
C26 C -0.7041(3) -1.1552(2) 0.04777(18) 0.0239(9) Uani 1 1 d . . . . .
C36 C -0.7024(3) -0.9086(2) -0.02775(18) 0.0227(9) Uani 1 1 d . . . . .
H36 H -0.7585 -0.8947 -0.0471 0.027 Uiso 1 1 calc R . . . .
C38 C -0.6955(3) -0.8164(2) 0.0359(2) 0.0285(10) Uani 1 1 d . . . . .
H38 H -0.7504 -0.7936 0.0237 0.034 Uiso 1 1 calc R . . . .
C39 C -0.6325(4) -0.8018(2) 0.0792(2) 0.0279(10) Uani 1 1 d . . . . .
H39 H -0.6360 -0.7667 0.1021 0.033 Uiso 1 1 calc R . . . .
C48 C -0.4993(3) -1.1108(2) -0.0794(2) 0.0303(11) Uani 1 1 d . . . . .
H48 H -0.4980 -1.1249 -0.0424 0.036 Uiso 1 1 calc R . . . .
C49 C -0.4889(5) -0.6481(3) 0.0603(3) 0.0565(16) Uani 1 1 d . . . . .
H49 H -0.5073 -0.6822 0.0822 0.068 Uiso 1 1 calc R . . . .
C50 C -0.4728(5) -0.5947(4) 0.0865(3) 0.0643(18) Uani 1 1 d . . . . .
H50 H -0.4784 -0.5919 0.1254 0.077 Uiso 1 1 calc R . . . .
C51 C -0.4488(4) -0.5454(3) 0.0562(4) 0.069(2) Uani 1 1 d . . . . .
H51 H -0.4371 -0.5070 0.0734 0.083 Uiso 1 1 calc R . . . .
C52 C -0.4415(4) -0.5513(3) 0.0012(4) 0.070(2) Uani 1 1 d . . . . .
H52 H -0.4254 -0.5172 -0.0213 0.083 Uiso 1 1 calc R . . . .
C53 C -0.4578(5) -0.6076(3) -0.0219(3) 0.0613(18) Uani 1 1 d . . . . .
H53 H -0.4522 -0.6115 -0.0608 0.074 Uiso 1 1 calc R . . . .
C54 C -0.3379(5) -0.7301(3) -0.1597(3) 0.0591(18) Uani 1 1 d . . . . .
H54 H -0.3596 -0.6912 -0.1472 0.071 Uiso 1 1 calc R . . . .
C55 C -0.3032(7) -0.7351(4) -0.2125(4) 0.085(3) Uani 1 1 d . . . . .
H55 H -0.3024 -0.7009 -0.2366 0.102 Uiso 1 1 calc R . . . .
C56 C -0.2698(7) -0.7911(5) -0.2296(3) 0.096(3) Uani 1 1 d . . . . .
H56 H -0.2435 -0.7961 -0.2656 0.115 Uiso 1 1 calc R . . . .
C57 C -0.2747(7) -0.8396(4) -0.1942(3) 0.089(3) Uani 1 1 d . . . . .
H57 H -0.2534 -0.8791 -0.2053 0.106 Uiso 1 1 calc R . . . .
C58 C -0.3111(5) -0.8299(3) -0.1427(3) 0.0555(16) Uani 1 1 d . . . . .
H58 H -0.3138 -0.8634 -0.1179 0.067 Uiso 1 1 calc R . . . .
C59 C -0.6159(7) -0.7336(6) -0.1774(5) 0.120(4) Uani 1 1 d . . . . .
H59 H -0.6266 -0.6943 -0.1620 0.144 Uiso 1 1 calc R . . . .
C60 C -0.6318(10) -0.7415(8) -0.2325(6) 0.149(7) Uani 1 1 d . . . . .
H60 H -0.6533 -0.7084 -0.2549 0.179 Uiso 1 1 calc R . . . .
C61 C -0.6167(12) -0.7964(9) -0.2540(6) 0.165(7) Uani 1 1 d . . . . .
H61 H -0.6274 -0.8030 -0.2923 0.198 Uiso 1 1 calc R . . . .
C62 C -0.5857(9) -0.8437(6) -0.2215(4) 0.124(4) Uani 1 1 d . . . . .
H62 H -0.5747 -0.8833 -0.2363 0.149 Uiso 1 1 calc R . . . .
C63 C -0.5714(6) -0.8316(4) -0.1672(4) 0.079(2) Uani 1 1 d . . . . .
H63 H -0.5492 -0.8641 -0.1443 0.095 Uiso 1 1 calc R . . . .
C67 C -0.1602(6) -1.0691(3) 0.1941(3) 0.0636(19) Uani 1 1 d . . . . .
H H -0.1395 -1.1063 0.2105 0.076 Uiso 1 1 calc R . . . .
C78 C -0.4105(5) -0.5299(4) -0.1676(3) 0.079(2) Uani 1 1 d . . . . .
HA H -0.4711 -0.5390 -0.1848 0.095 Uiso 1 1 calc R . . . .
N1 N -0.3697(3) -0.90007(16) 0.04870(15) 0.0212(7) Uani 1 1 d . . . . .
N3 N -0.3022(3) -1.09964(16) -0.02022(14) 0.0225(8) Uani 1 1 d . . . . .
N4 N -0.3944(3) -1.14519(16) 0.07425(14) 0.0204(7) Uani 1 1 d . . . . .
H4 H -0.4227 -1.1119 0.0616 0.024 Uiso 1 1 calc R . . . .
N7 N -0.6650(2) -0.96098(17) -0.04021(13) 0.0207(7) Uani 1 1 d . . . . .
N8 N -0.5799(3) -0.89113(15) 0.04248(14) 0.0196(7) Uani 1 1 d . . . . .
N9 N -0.4886(3) -1.05049(16) -0.08862(14) 0.0252(8) Uani 1 1 d . . . . .
N10 N -0.4810(4) -0.65647(19) 0.0069(2) 0.0548(12) Uani 1 1 d . . . . .
N11 N -0.3426(4) -0.7766(2) -0.1254(2) 0.0476(12) Uani 1 1 d . . . . .
N12 N -0.5859(5) -0.7786(4) -0.1442(3) 0.081(2) Uani 1 1 d . . . . .
C69 C -0.5066(4) -1.2807(3) 0.0091(3) 0.0528(15) Uani 1 1 d . . . . .
HB H -0.4970 -1.2406 0.0232 0.063 Uiso 1 1 calc R . . . .
N15 N -0.3489(5) -0.5754(3) -0.1577(3) 0.0746(19) Uani 1 1 d . . . . .
O1 O -0.49160(19) -1.03224(13) 0.04320(10) 0.0207(6) Uani 1 1 d . . . . .
O2 O -0.4676(2) -0.91265(12) -0.06413(11) 0.0219(6) Uani 1 1 d . . . . .
C1 C -0.3853(3) -0.8554(2) 0.08617(17) 0.0227(9) Uani 1 1 d . . . . .
C2 C -0.3080(4) -0.8130(2) 0.0859(2) 0.0330(11) Uani 1 1 d . . . . .
H2 H -0.3027 -0.7773 0.1079 0.040 Uiso 1 1 calc R . . . .
C3 C -0.2408(4) -0.8335(2) 0.0471(2) 0.0363(12) Uani 1 1 d . . . . .
H3 H -0.1804 -0.8148 0.0375 0.044 Uiso 1 1 calc R . . . .
C4 C -0.2803(3) -0.8875(2) 0.02504(19) 0.0255(10) Uani 1 1 d . . . . .
C5 C -0.2400(3) -0.9282(2) -0.01442(19) 0.0257(9) Uani 1 1 d . . . . .
H5 H -0.1773 -0.9200 -0.0295 0.031 Uiso 1 1 calc R . . . .
C6 C -0.2479(3) -1.01344(19) -0.07235(17) 0.0215(9) Uani 1 1 d . . . . .
C7 C -0.2004(3) -0.9890(2) -0.11864(18) 0.0257(10) Uani 1 1 d . . . . .
H7 H -0.1914 -0.9460 -0.1211 0.031 Uiso 1 1 calc R . . . .
C8 C -0.1660(3) -1.0260(2) -0.16111(17) 0.0291(10) Uani 1 1 d . . . . .
C9 C -0.1144(5) -0.9970(2) -0.2095(2) 0.0432(14) Uani 1 1 d . . . . .
H9A H -0.1514 -1.0050 -0.2433 0.065 Uiso 1 1 calc GR . . . .
H9B H -0.0486 -1.0143 -0.2129 0.065 Uiso 1 1 calc GR . . . .
H9C H -0.1097 -0.9528 -0.2036 0.065 Uiso 1 1 calc GR . . . .
C10 C -0.1824(4) -1.0886(2) -0.15866(19) 0.0299(11) Uani 1 1 d . . . . .
C12 C -0.2273(3) -1.1130(2) -0.11232(18) 0.0265(10) Uani 1 1 d . . . . .
H12 H -0.2371 -1.1560 -0.1104 0.032 Uiso 1 1 calc R . . . .
C13 C -0.2585(3) -1.0770(2) -0.06863(17) 0.0218(9) Uani 1 1 d . . . . .
C15 C -0.2714(3) -1.14957(19) 0.00107(17) 0.0231(9) Uani 1 1 d . . . . .
H15 H -0.2189 -1.1711 -0.0157 0.028 Uiso 1 1 calc R . . . .
C16 C -0.3161(3) -1.17323(19) 0.05045(18) 0.0213(9) Uani 1 1 d . . . . .
C17 C -0.2930(4) -1.2233(2) 0.08226(19) 0.0264(10) Uani 1 1 d . . . . .
H17 H -0.2413 -1.2513 0.0757 0.032 Uiso 1 1 calc R . . . .
C18 C -0.3602(3) -1.2252(2) 0.12638(18) 0.0267(10) Uani 1 1 d . . . . .
H18 H -0.3620 -1.2548 0.1550 0.032 Uiso 1 1 calc R . . . .
C19 C -0.4227(3) -1.17614(19) 0.12047(16) 0.0204(9) Uani 1 1 d . . . . .
C20 C -0.5109(4) -1.1569(2) 0.15365(15) 0.0235(9) Uani 1 1 d . . . . .
C22 C -0.5027(4) -1.0889(2) 0.17027(17) 0.0325(12) Uani 1 1 d . . . . .
H22A H -0.4979 -1.0636 0.1370 0.049 Uiso 1 1 calc GR . . . .
H22B H -0.4441 -1.0830 0.1929 0.049 Uiso 1 1 calc GR . . . .
H22C H -0.5607 -1.0769 0.1914 0.049 Uiso 1 1 calc GR . . . .
C25 C -0.7408(4) -1.2015(2) 0.0799(2) 0.0289(10) Uani 1 1 d . . . . .
H25 H -0.7989 -1.2241 0.0731 0.035 Uiso 1 1 calc R . . . .
C27 C -0.7413(3) -1.12752(19) -0.00190(18) 0.0250(9) Uani 1 1 d . . . . .
H27 H -0.7997 -1.1425 -0.0181 0.030 Uiso 1 1 calc R . . . .
C28 C -0.7283(3) -1.0576(2) -0.07389(17) 0.0225(9) Uani 1 1 d . . . . .
C29 C -0.7729(4) -1.0912(2) -0.11592(19) 0.0291(10) Uani 1 1 d . . . . .
H29 H -0.7853 -1.1335 -0.1102 0.035 Uiso 1 1 calc R . . . .
C30 C -0.7997(4) -1.0648(2) -0.1658(2) 0.0324(11) Uani 1 1 d . . . . .
C31 C -0.8443(5) -1.1036(3) -0.2110(2) 0.0532(17) Uani 1 1 d . . . . .
H31A H -0.8461 -1.1463 -0.1991 0.080 Uiso 1 1 calc GR . . . .
H31B H -0.8048 -1.1000 -0.2445 0.080 Uiso 1 1 calc GR . . . .
H31C H -0.9110 -1.0894 -0.2185 0.080 Uiso 1 1 calc GR . . . .
C32 C -0.7820(4) -1.0025(2) -0.17416(19) 0.0315(11) Uani 1 1 d . . . . .
C33 C -0.8091(5) -0.9719(3) -0.2278(2) 0.0523(15) Uani 1 1 d . . . . .
H33A H -0.7984 -0.9278 -0.2246 0.078 Uiso 1 1 calc GR . . . .
H33B H -0.8780 -0.9799 -0.2360 0.078 Uiso 1 1 calc GR . . . .
H33C H -0.7683 -0.9883 -0.2576 0.078 Uiso 1 1 calc GR . . . .
C34 C -0.7379(3) -0.9691(3) -0.13287(17) 0.0275(9) Uani 1 1 d . . . . .
H34 H -0.7258 -0.9268 -0.1388 0.033 Uiso 1 1 calc R . . . .
C35 C -0.7105(3) -0.9952(2) -0.08287(18) 0.0212(9) Uani 1 1 d . . . . .
C37 C -0.6616(3) -0.87141(18) 0.01424(19) 0.0223(8) Uani 1 1 d . . . . .
C40 C -0.5636(3) -0.84830(19) 0.08231(17) 0.0217(9) Uani 1 1 d . . . . .
C41 C -0.4774(4) -0.85508(18) 0.12096(15) 0.0236(8) Uani 1 1 d . . . . .
C42 C -0.4755(4) -0.8030(2) 0.16305(17) 0.0343(10) Uani 1 1 d . . . . .
H42A H -0.5364 -0.8031 0.1843 0.051 Uiso 1 1 calc GR . . . .
H42B H -0.4688 -0.7639 0.1437 0.051 Uiso 1 1 calc GR . . . .
H42C H -0.4200 -0.8086 0.1881 0.051 Uiso 1 1 calc GR . . . .
C43 C -0.4848(4) -0.9166(2) 0.15216(17) 0.0323(10) Uani 1 1 d . . . . .
H43A H -0.4836 -0.9503 0.1256 0.048 Uiso 1 1 calc GR . . . .
H43B H -0.5460 -0.9178 0.1731 0.048 Uiso 1 1 calc GR . . . .
H43C H -0.4294 -0.9205 0.1775 0.048 Uiso 1 1 calc GR . . . .
C44 C -0.4921(4) -1.0324(3) -0.14112(17) 0.0472(14) Uani 1 1 d . . . . .
H44 H -0.4849 -0.9901 -0.1489 0.057 Uiso 1 1 calc R . . . .
C45 C -0.5056(7) -1.0717(3) -0.1843(2) 0.081(3) Uani 1 1 d . . . . .
H45 H -0.5071 -1.0567 -0.2211 0.097 Uiso 1 1 calc R . . . .
C46 C -0.5169(7) -1.1324(3) -0.1742(3) 0.075(2) Uani 1 1 d . . . . .
H46 H -0.5279 -1.1601 -0.2038 0.091 Uiso 1 1 calc R . . . .
C47 C -0.5121(5) -1.1531(3) -0.1207(2) 0.0499(15) Uani 1 1 d . . . . .
H47 H -0.5175 -1.1955 -0.1125 0.060 Uiso 1 1 calc R . . . .
C64 C -0.2176(5) -0.9624(3) 0.1491(3) 0.0621(18) Uani 1 1 d . . . . .
HC H -0.2362 -0.9243 0.1336 0.075 Uiso 1 1 calc R . . . .
C65 C -0.1692(5) -0.9643(4) 0.1981(3) 0.0641(19) Uani 1 1 d . . . . .
HD H -0.1571 -0.9276 0.2177 0.077 Uiso 1 1 calc R . . . .
C66 C -0.1391(6) -1.0167(3) 0.2183(3) 0.070(2) Uani 1 1 d . . . . .
HE H -0.1013 -1.0169 0.2512 0.084 Uiso 1 1 calc R . . . .
C68 C -0.2103(5) -1.0705(3) 0.1467(3) 0.0578(17) Uani 1 1 d . . . . .
HF H -0.2261 -1.1084 0.1299 0.069 Uiso 1 1 calc R . . . .
C70 C -0.5140(5) -1.3272(3) 0.0463(3) 0.0533(15) Uani 1 1 d . . . . .
HG H -0.5098 -1.3195 0.0848 0.064 Uiso 1 1 calc R . . . .
C71 C -0.5276(5) -1.3851(3) 0.0266(3) 0.0585(16) Uani 1 1 d . . . . .
HH H -0.5333 -1.4187 0.0512 0.070 Uiso 1 1 calc R . . . .
C72 C -0.5329(6) -1.3940(3) -0.0286(3) 0.0642(19) Uani 1 1 d . . . . .
HI H -0.5420 -1.4339 -0.0431 0.077 Uiso 1 1 calc R . . . .
C73 C -0.5250(6) -1.3449(3) -0.0630(3) 0.0642(17) Uani 1 1 d . . . . .
HJ H -0.5291 -1.3522 -0.1016 0.077 Uiso 1 1 calc R . . . .
N14 N -0.5119(5) -1.2874(3) -0.0462(2) 0.0643(15) Uani 1 1 d . . . . .
N2 N -0.2875(2) -0.97619(17) -0.03017(14) 0.0211(7) Uani 1 1 d . . . . .
N5 N -0.6201(3) -1.13506(16) 0.07205(14) 0.0206(8) Uani 1 1 d . . . . .
H5A H -0.5830 -1.1055 0.0592 0.025 Uiso 1 1 calc R . . . .
N6 N -0.6961(3) -1.08295(17) -0.02417(15) 0.0250(8) Uani 1 1 d . . . . .
N13 N -0.2392(5) -1.0155(3) 0.1224(3) 0.080(2) Uani 1 1 d . . . . .
Rb1 Rb -0.47566(5) -0.78867(2) -0.03021(2) 0.03857(11) Uani 1 1 d . . . . .
U1 U -0.47826(2) -0.96972(2) -0.00888(2) 0.01624(4) Uani 1 1 d . . . . .
C74 C -0.2689(5) -0.5618(3) -0.1304(3) 0.0473(15) Uani 1 1 d . . . . .
HK H -0.2249 -0.5940 -0.1220 0.057 Uiso 1 1 calc R . . . .
C75 C -0.2451(5) -0.5048(3) -0.1136(3) 0.0519(17) Uani 1 1 d . . . . .
HL H -0.1870 -0.4979 -0.0931 0.062 Uiso 1 1 calc R . . . .
C76 C -0.3061(6) -0.4572(3) -0.1265(3) 0.0606(19) Uani 1 1 d . . . . .
HM H -0.2897 -0.4165 -0.1164 0.073 Uiso 1 1 calc R . . . .
C77 C -0.3906(5) -0.4694(4) -0.1542(3) 0.0659(19) Uani 1 1 d . . . . .
HN H -0.4346 -0.4376 -0.1639 0.079 Uiso 1 1 calc R . . . .


_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
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C11 C10 1.515(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C21 C20 1.538(5) . ?
C23 C24 1.378(7) . ?
C23 C20 1.518(6) . ?
C23 N5 1.362(5) . ?
C24 H24 0.9500 . ?
C24 C25 1.405(7) . ?
C26 C25 1.372(6) . ?
C26 C27 1.441(6) . ?
C26 N5 1.365(6) . ?
C36 H36 0.9500 . ?
C36 N7 1.290(6) . ?
C36 C37 1.418(6) . ?
C38 H38 0.9500 . ?
C38 C39 1.396(7) . ?
C38 C37 1.392(6) . ?
C38 Rb1 3.462(5) . ?
C39 H39 0.9500 . ?
C39 C40 1.390(6) . ?
C39 Rb1 3.423(5) . ?
C48 H48 0.9500 . ?
C48 N9 1.347(6) . ?
C48 C47 1.375(6) . ?
C49 H49 0.9500 . ?
C49 C50 1.348(9) . ?
C49 N10 1.313(8) . ?
C50 H50 0.9500 . ?
C50 C51 1.347(10) . ?
C51 H51 0.9500 . ?
C51 C52 1.344(11) . ?
C52 H52 0.9500 . ?
C52 C53 1.371(10) . ?
C53 H53 0.9500 . ?
C53 N10 1.317(8) . ?
C54 H54 0.9500 . ?
C54 C55 1.370(11) . ?
C54 N11 1.315(8) . ?
C55 H55 0.9500 . ?
C55 C56 1.372(13) . ?
C56 H56 0.9500 . ?
C56 C57 1.367(11) . ?
C57 H57 0.9500 . ?
C57 C58 1.362(9) . ?
C58 H58 0.9500 . ?
C58 N11 1.312(8) . ?
C58 Rb1 3.649(6) . ?
C59 H59 0.9500 . ?
C59 C60 1.364(18) . ?
C59 N12 1.337(11) . ?
C60 H60 0.9500 . ?
C60 C61 1.33(2) . ?
C61 H61 0.9500 . ?
C61 C62 1.369(17) . ?
C62 H62 0.9500 . ?
C62 C63 1.358(12) . ?
C63 H63 0.9500 . ?
C63 N12 1.303(11) . ?
C63 Rb1 3.691(9) . ?
C67 H 0.9500 . ?
C67 C66 1.321(9) . ?
C67 C68 1.337(9) . ?
C78 HA 0.9500 . ?
C78 N15 1.327(9) . ?
C78 C77 1.390(11) . ?
N1 C1 1.352(5) . ?
N1 C4 1.379(6) . ?
N1 Rb1 3.422(4) . ?
N1 U1 2.546(4) . ?
N3 C13 1.408(5) . ?
N3 C15 1.280(5) . ?
N4 H4 0.8800 . ?
N4 C16 1.363(5) . ?
N4 C19 1.365(5) . ?
N7 C35 1.420(5) . ?
N7 U1 2.672(3) . ?
N8 C37 1.381(5) . ?
N8 C40 1.364(5) . ?
N8 Rb1 3.189(3) . ?
N8 U1 2.538(3) . ?
N9 C44 1.334(5) . ?
N9 U1 2.624(3) . ?
N10 Rb1 3.031(4) . ?
N11 Rb1 2.952(5) . ?
N12 Rb1 3.156(7) . ?
C69 HB 0.9500 . ?
C69 C70 1.362(9) . ?
C69 N14 1.352(9) . ?
N15 C74 1.313(8) . ?
O1 U1 1.871(3) . ?
O2 Rb1 2.838(3) . ?
O2 U1 1.838(3) . ?
C1 C2 1.407(7) . ?
C1 C41 1.516(6) . ?
C1 Rb1 3.409(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.388(7) . ?
C2 Rb1 3.670(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.406(6) . ?
C4 C5 1.419(6) . ?
C4 Rb1 3.690(4) . ?
C5 H5 0.9500 . ?
C5 N2 1.293(6) . ?
C6 C7 1.403(6) . ?
C6 C13 1.401(6) . ?
C6 N2 1.416(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.392(6) . ?
C8 C9 1.509(6) . ?
C8 C10 1.388(7) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C12 1.388(6) . ?
C12 H12 0.9500 . ?
C12 C13 1.388(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.441(6) . ?
C16 C17 1.377(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.411(7) . ?
C18 H18 0.9500 . ?
C18 C19 1.380(6) . ?
C19 C20 1.511(6) . ?
C20 C22 1.546(6) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C25 H25 0.9500 . ?
C27 H27 0.9500 . ?
C27 N6 1.275(6) . ?
C28 C29 1.398(6) . ?
C28 C35 1.405(6) . ?
C28 N6 1.399(5) . ?
C29 H29 0.9500 . ?
C29 C30 1.390(6) . ?
C30 C31 1.513(7) . ?
C30 C32 1.400(7) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.508(6) . ?
C32 C34 1.379(7) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34 0.9500 . ?
C34 C35 1.392(6) . ?
C37 Rb1 3.304(4) . ?
C40 C41 1.513(6) . ?
C40 Rb1 3.254(4) . ?
C41 C42 1.530(5) . ?
C41 C43 1.547(6) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44 0.9500 . ?
C44 C45 1.367(7) . ?
C45 H45 0.9500 . ?
C45 C46 1.358(9) . ?
C46 H46 0.9500 . ?
C46 C47 1.377(9) . ?
C47 H47 0.9500 . ?
C64 HC 0.9500 . ?
C64 C65 1.360(9) . ?
C64 N13 1.363(9) . ?
C65 HD 0.9500 . ?
C65 C66 1.314(10) . ?
C66 HE 0.9500 . ?
C68 HF 0.9500 . ?
C68 N13 1.397(9) . ?
C70 HG 0.9500 . ?
C70 C71 1.369(8) . ?
C71 HH 0.9500 . ?
C71 C72 1.353(9) . ?
C72 HI 0.9500 . ?
C72 C73 1.365(9) . ?
C73 HJ 0.9500 . ?
C73 N14 1.336(8) . ?
N2 U1 2.664(3) . ?
N5 H5A 0.8800 . ?
C74 HK 0.9500 . ?
C74 C75 1.351(8) . ?
C75 HL 0.9500 . ?
C75 C76 1.372(9) . ?
C76 HM 0.9500 . ?
C76 C77 1.363(9) . ?
C77 HN 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
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
C24 C23 C20 130.8(4) . . ?
N5 C23 C24 106.8(4) . . ?
N5 C23 C20 122.3(4) . . ?
C23 C24 H24 125.9 . . ?
C23 C24 C25 108.1(4) . . ?
C25 C24 H24 125.9 . . ?
C25 C26 C27 130.9(4) . . ?
N5 C26 C25 107.6(4) . . ?
N5 C26 C27 121.4(4) . . ?
N7 C36 H36 119.3 . . ?
N7 C36 C37 121.5(4) . . ?
C37 C36 H36 119.3 . . ?
C39 C38 H38 127.0 . . ?
C39 C38 Rb1 76.7(3) . . ?
C37 C38 H38 127.0 . . ?
C37 C38 C39 106.0(4) . . ?
C37 C38 Rb1 71.8(2) . . ?
Rb1 C38 H38 116.8 . . ?
C38 C39 H39 126.5 . . ?
C38 C39 Rb1 79.9(3) . . ?
C40 C39 C38 107.0(4) . . ?
C40 C39 H39 126.5 . . ?
C40 C39 Rb1 71.2(3) . . ?
Rb1 C39 H39 114.7 . . ?
N9 C48 H48 118.2 . . ?
N9 C48 C47 123.6(5) . . ?
C47 C48 H48 118.2 . . ?
C50 C49 H49 117.6 . . ?
N10 C49 H49 117.6 . . ?
N10 C49 C50 124.8(6) . . ?
C49 C50 H50 120.7 . . ?
C51 C50 C49 118.7(7) . . ?
C51 C50 H50 120.7 . . ?
C50 C51 H51 120.6 . . ?
C52 C51 C50 118.7(6) . . ?
C52 C51 H51 120.6 . . ?
C51 C52 H52 120.6 . . ?
C51 C52 C53 118.7(6) . . ?
C53 C52 H52 120.6 . . ?
C52 C53 H53 118.2 . . ?
N10 C53 C52 123.5(7) . . ?
N10 C53 H53 118.2 . . ?
C55 C54 H54 118.5 . . ?
N11 C54 H54 118.5 . . ?
N11 C54 C55 123.0(7) . . ?
C54 C55 H55 121.0 . . ?
C54 C55 C56 118.0(7) . . ?
C56 C55 H55 121.0 . . ?
C55 C56 H56 120.4 . . ?
C57 C56 C55 119.2(7) . . ?
C57 C56 H56 120.4 . . ?
C56 C57 H57 120.9 . . ?
C58 C57 C56 118.2(8) . . ?
C58 C57 H57 120.9 . . ?
C57 C58 H58 118.3 . . ?
C57 C58 Rb1 161.8(6) . . ?
N11 C58 C57 123.5(7) . . ?
N11 C58 H58 118.3 . . ?
N11 C58 Rb1 48.7(3) . . ?
Rb1 C58 H58 72.2 . . ?
C60 C59 H59 118.4 . . ?
N12 C59 H59 118.4 . . ?
N12 C59 C60 123.2(12) . . ?
C59 C60 H60 120.9 . . ?
C61 C60 C59 118.2(12) . . ?
C61 C60 H60 120.9 . . ?
C60 C61 H61 119.7 . . ?
C60 C61 C62 120.6(14) . . ?
C62 C61 H61 119.7 . . ?
C61 C62 H62 121.5 . . ?
C63 C62 C61 117.1(13) . . ?
C63 C62 H62 121.5 . . ?
C62 C63 H63 117.7 . . ?
C62 C63 Rb1 166.8(7) . . ?
N12 C63 C62 124.6(9) . . ?
N12 C63 H63 117.7 . . ?
N12 C63 Rb1 56.1(4) . . ?
Rb1 C63 H63 63.4 . . ?
C66 C67 H 119.5 . . ?
C66 C67 C68 120.9(7) . . ?
C68 C67 H 119.5 . . ?
N15 C78 HA 118.3 . . ?
N15 C78 C77 123.3(6) . . ?
C77 C78 HA 118.3 . . ?
C1 N1 C4 106.0(4) . . ?
C1 N1 Rb1 78.0(2) . . ?
C1 N1 U1 135.2(3) . . ?
C4 N1 Rb1 90.0(2) . . ?
C4 N1 U1 114.2(3) . . ?
U1 N1 Rb1 82.69(9) . . ?
C15 N3 C13 119.8(4) . . ?
C16 N4 H4 124.8 . . ?
C16 N4 C19 110.3(4) . . ?
C19 N4 H4 124.8 . . ?
C36 N7 C35 117.7(4) . . ?
C36 N7 U1 112.1(3) . . ?
C35 N7 U1 126.0(3) . . ?
C37 N8 Rb1 82.4(2) . . ?
C37 N8 U1 114.4(3) . . ?
C40 N8 C37 105.6(3) . . ?
C40 N8 Rb1 80.5(2) . . ?
C40 N8 U1 136.3(3) . . ?
U1 N8 Rb1 87.74(10) . . ?
C48 N9 U1 123.0(3) . . ?
C44 N9 C48 116.4(4) . . ?
C44 N9 U1 120.4(3) . . ?
C49 N10 C53 115.5(5) . . ?
C49 N10 Rb1 115.3(4) . . ?
C53 N10 Rb1 127.8(4) . . ?
C54 N11 Rb1 126.4(5) . . ?
C58 N11 C54 118.1(6) . . ?
C58 N11 Rb1 111.8(4) . . ?
C59 N12 Rb1 136.6(8) . . ?
C63 N12 C59 116.4(9) . . ?
C63 N12 Rb1 103.9(5) . . ?
C70 C69 HB 117.5 . . ?
N14 C69 HB 117.5 . . ?
N14 C69 C70 124.9(6) . . ?
C74 N15 C78 116.7(6) . . ?
U1 O2 Rb1 115.83(12) . . ?
N1 C1 C2 110.7(4) . . ?
N1 C1 C41 120.6(4) . . ?
N1 C1 Rb1 79.1(2) . . ?
C2 C1 C41 128.7(4) . . ?
C2 C1 Rb1 89.2(3) . . ?
C41 C1 Rb1 99.1(2) . . ?
C1 C2 H2 126.6 . . ?
C1 C2 Rb1 68.2(3) . . ?
C3 C2 C1 106.9(4) . . ?
C3 C2 H2 126.6 . . ?
C3 C2 Rb1 86.7(3) . . ?
Rb1 C2 H2 111.1 . . ?
C2 C3 H3 127.1 . . ?
C2 C3 C4 105.9(4) . . ?
C4 C3 H3 127.1 . . ?
N1 C4 C3 110.5(4) . . ?
N1 C4 C5 120.0(4) . . ?
N1 C4 Rb1 68.0(2) . . ?
C3 C4 C5 129.5(4) . . ?
C3 C4 Rb1 85.7(3) . . ?
C5 C4 Rb1 113.9(3) . . ?
C4 C5 H5 119.5 . . ?
N2 C5 C4 121.0(4) . . ?
N2 C5 H5 119.5 . . ?
C7 C6 N2 122.4(4) . . ?
C13 C6 C7 118.6(4) . . ?
C13 C6 N2 119.1(4) . . ?
C6 C7 H7 119.1 . . ?
C8 C7 C6 121.7(4) . . ?
C8 C7 H7 119.1 . . ?
C7 C8 C9 119.2(5) . . ?
C10 C8 C7 119.2(4) . . ?
C10 C8 C9 121.6(4) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 C11 120.9(4) . . ?
C8 C10 C12 119.1(4) . . ?
C12 C10 C11 119.9(4) . . ?
C10 C12 H12 118.9 . . ?
C13 C12 C10 122.3(4) . . ?
C13 C12 H12 118.9 . . ?
C6 C13 N3 116.6(4) . . ?
C12 C13 N3 124.5(4) . . ?
C12 C13 C6 118.9(4) . . ?
N3 C15 H15 120.0 . . ?
N3 C15 C16 120.1(4) . . ?
C16 C15 H15 120.0 . . ?
N4 C16 C15 121.6(4) . . ?
N4 C16 C17 107.6(4) . . ?
C17 C16 C15 130.8(4) . . ?
C16 C17 H17 126.3 . . ?
C16 C17 C18 107.3(4) . . ?
C18 C17 H17 126.3 . . ?
C17 C18 H18 126.2 . . ?
C19 C18 C17 107.6(4) . . ?
C19 C18 H18 126.2 . . ?
N4 C19 C18 107.2(4) . . ?
N4 C19 C20 121.7(4) . . ?
C18 C19 C20 131.1(4) . . ?
C21 C20 C22 108.7(3) . . ?
C23 C20 C21 109.4(4) . . ?
C23 C20 C22 110.4(4) . . ?
C19 C20 C21 109.4(4) . . ?
C19 C20 C23 108.6(3) . . ?
C19 C20 C22 110.4(4) . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C25 H25 126.4 . . ?
C26 C25 C24 107.2(4) . . ?
C26 C25 H25 126.4 . . ?
C26 C27 H27 119.8 . . ?
N6 C27 C26 120.3(4) . . ?
N6 C27 H27 119.8 . . ?
C29 C28 C35 118.4(4) . . ?
C29 C28 N6 123.8(4) . . ?
N6 C28 C35 117.7(4) . . ?
C28 C29 H29 119.0 . . ?
C30 C29 C28 122.0(5) . . ?
C30 C29 H29 119.0 . . ?
C29 C30 C31 120.2(5) . . ?
C29 C30 C32 119.0(5) . . ?
C32 C30 C31 120.8(5) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 C33 120.9(5) . . ?
C34 C32 C30 119.2(5) . . ?
C34 C32 C33 119.8(5) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34 118.9 . . ?
C32 C34 C35 122.2(5) . . ?
C35 C34 H34 118.9 . . ?
C28 C35 N7 118.4(4) . . ?
C34 C35 N7 122.4(4) . . ?
C34 C35 C28 119.2(4) . . ?
C36 C37 Rb1 112.6(3) . . ?
C38 C37 C36 129.5(4) . . ?
C38 C37 Rb1 84.6(3) . . ?
N8 C37 C36 119.6(4) . . ?
N8 C37 C38 110.7(4) . . ?
N8 C37 Rb1 73.1(2) . . ?
C39 C40 C41 129.4(4) . . ?
C39 C40 Rb1 84.9(3) . . ?
N8 C40 C39 110.7(4) . . ?
N8 C40 C41 119.9(4) . . ?
N8 C40 Rb1 75.1(2) . . ?
C41 C40 Rb1 105.7(3) . . ?
C1 C41 C42 111.1(4) . . ?
C1 C41 C43 108.8(4) . . ?
C40 C41 C1 107.7(3) . . ?
C40 C41 C42 110.7(4) . . ?
C40 C41 C43 109.7(4) . . ?
C42 C41 C43 108.9(3) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N9 C44 H44 118.4 . . ?
N9 C44 C45 123.3(5) . . ?
C45 C44 H44 118.4 . . ?
C44 C45 H45 120.2 . . ?
C46 C45 C44 119.5(6) . . ?
C46 C45 H45 120.2 . . ?
C45 C46 H46 120.4 . . ?
C45 C46 C47 119.1(5) . . ?
C47 C46 H46 120.4 . . ?
C48 C47 C46 118.0(5) . . ?
C48 C47 H47 121.0 . . ?
C46 C47 H47 121.0 . . ?
C65 C64 HC 120.2 . . ?
C65 C64 N13 119.6(7) . . ?
N13 C64 HC 120.2 . . ?
C64 C65 HD 119.8 . . ?
C66 C65 C64 120.4(7) . . ?
C66 C65 HD 119.8 . . ?
C67 C66 HE 119.2 . . ?
C65 C66 C67 121.5(6) . . ?
C65 C66 HE 119.2 . . ?
C67 C68 HF 120.4 . . ?
C67 C68 N13 119.2(7) . . ?
N13 C68 HF 120.4 . . ?
C69 C70 HG 121.0 . . ?
C69 C70 C71 118.0(6) . . ?
C71 C70 HG 121.0 . . ?
C70 C71 HH 120.4 . . ?
C72 C71 C70 119.1(7) . . ?
C72 C71 HH 120.4 . . ?
C71 C72 HI 120.4 . . ?
C71 C72 C73 119.1(6) . . ?
C73 C72 HI 120.4 . . ?
C72 C73 HJ 117.7 . . ?
N14 C73 C72 124.5(6) . . ?
N14 C73 HJ 117.7 . . ?
C73 N14 C69 114.3(6) . . ?
C5 N2 C6 119.3(4) . . ?
C5 N2 U1 113.1(3) . . ?
C6 N2 U1 123.1(3) . . ?
C23 N5 C26 110.3(4) . . ?
C23 N5 H5A 124.8 . . ?
C26 N5 H5A 124.8 . . ?
C27 N6 C28 121.0(4) . . ?
C64 N13 C68 118.2(6) . . ?
C38 Rb1 C58 146.99(14) . . ?
C39 Rb1 C38 23.38(11) . . ?
C39 Rb1 C58 160.87(13) . . ?
N1 Rb1 C38 89.10(10) . . ?
N1 Rb1 C39 76.87(10) . . ?
N1 Rb1 C58 88.86(12) . . ?
N8 Rb1 C38 39.84(10) . . ?
N8 Rb1 C39 39.88(10) . . ?
N8 Rb1 C58 121.00(12) . . ?
N8 Rb1 N1 51.64(8) . . ?
N8 Rb1 C1 53.38(10) . . ?
N8 Rb1 C37 24.47(9) . . ?
N8 Rb1 C40 24.42(9) . . ?
N10 Rb1 C38 90.55(13) . . ?
N10 Rb1 C39 80.52(13) . . ?
N10 Rb1 C58 118.19(15) . . ?
N10 Rb1 N1 121.64(12) . . ?
N10 Rb1 N8 119.79(13) . . ?
N10 Rb1 N12 100.47(18) . . ?
N10 Rb1 C1 99.90(13) . . ?
N10 Rb1 C37 114.09(13) . . ?
N10 Rb1 C40 97.20(13) . . ?
N11 Rb1 C38 156.00(13) . . ?
N11 Rb1 C39 179.20(14) . . ?
N11 Rb1 C58 19.49(14) . . ?
N11 Rb1 N1 103.88(12) . . ?
N11 Rb1 N8 140.45(12) . . ?
N11 Rb1 N10 99.28(15) . . ?
N11 Rb1 N12 66.64(16) . . ?
N11 Rb1 C1 117.54(13) . . ?
N11 Rb1 C37 141.18(12) . . ?
N11 Rb1 C40 156.84(13) . . ?
N12 Rb1 C38 90.13(14) . . ?
N12 Rb1 C39 112.62(15) . . ?
N12 Rb1 C58 70.00(16) . . ?
N12 Rb1 N1 137.89(16) . . ?
N12 Rb1 N8 108.62(15) . . ?
N12 Rb1 C1 158.12(17) . . ?
N12 Rb1 C37 87.46(15) . . ?
N12 Rb1 C40 125.82(15) . . ?
O2 Rb1 C38 90.02(10) . . ?
O2 Rb1 C39 99.72(10) . . ?
O2 Rb1 C58 61.51(12) . . ?
O2 Rb1 N1 57.59(8) . . ?
O2 Rb1 N8 60.34(8) . . ?
O2 Rb1 N10 179.04(12) . . ?
O2 Rb1 N11 80.49(11) . . ?
O2 Rb1 N12 80.31(16) . . ?
O2 Rb1 C1 79.41(9) . . ?
O2 Rb1 C37 66.45(9) . . ?
O2 Rb1 C40 82.76(9) . . ?
C1 Rb1 C38 81.76(11) . . ?
C1 Rb1 C39 63.26(11) . . ?
C1 Rb1 C58 106.79(13) . . ?
C1 Rb1 N1 22.84(9) . . ?
C37 Rb1 C38 23.60(10) . . ?
C37 Rb1 C39 38.62(11) . . ?
C37 Rb1 C58 125.69(13) . . ?
C37 Rb1 N1 75.73(9) . . ?
C37 Rb1 C1 76.97(11) . . ?
C40 Rb1 C38 38.78(11) . . ?
C40 Rb1 C39 23.85(11) . . ?
C40 Rb1 C58 139.04(13) . . ?
C40 Rb1 N1 53.29(10) . . ?
C40 Rb1 C1 42.98(10) . . ?
C40 Rb1 C37 38.94(11) . . ?
N1 U1 N7 132.15(11) . . ?
N1 U1 N9 147.05(12) . . ?
N1 U1 N2 64.30(11) . . ?
N1 U1 Rb1 58.13(8) . . ?
N7 U1 Rb1 84.30(8) . . ?
N8 U1 N1 69.20(10) . . ?
N8 U1 N7 64.35(11) . . ?
N8 U1 N9 142.05(12) . . ?
N8 U1 N2 131.89(11) . . ?
N8 U1 Rb1 52.87(8) . . ?
N9 U1 N7 77.71(12) . . ?
N9 U1 N2 82.78(12) . . ?
N9 U1 Rb1 124.98(7) . . ?
O1 U1 N1 97.18(12) . . ?
O1 U1 N7 98.69(11) . . ?
O1 U1 N8 96.39(11) . . ?
O1 U1 N9 89.95(11) . . ?
O1 U1 N2 100.80(11) . . ?
O1 U1 Rb1 144.44(8) . . ?
O2 U1 N1 86.91(12) . . ?
O2 U1 N7 79.65(12) . . ?
O2 U1 N8 86.59(12) . . ?
O2 U1 N9 85.71(11) . . ?
O2 U1 O1 175.60(12) . . ?
O2 U1 N2 79.44(13) . . ?
O2 U1 Rb1 39.72(8) . . ?
N2 U1 N7 152.29(10) . . ?
N2 U1 Rb1 91.08(8) . . ?
N15 C74 HK 117.9 . . ?
N15 C74 C75 124.3(6) . . ?
C75 C74 HK 117.9 . . ?
C74 C75 HL 120.5 . . ?
C74 C75 C76 119.0(6) . . ?
C76 C75 HL 120.5 . . ?
C75 C76 HM 120.7 . . ?
C77 C76 C75 118.6(6) . . ?
C77 C76 HM 120.7 . . ?
C78 C77 HN 121.1 . . ?
C76 C77 C78 117.9(6) . . ?
C76 C77 HN 121.1 . . ?

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
C11 C10 C12 C13 -178.5(5) . . . . ?
C23 C24 C25 C26 0.1(6) . . . . ?
C24 C23 C20 C21 -8.8(7) . . . . ?
C24 C23 C20 C19 110.5(5) . . . . ?
C24 C23 C20 C22 -128.3(5) . . . . ?
C24 C23 N5 C26 0.0(5) . . . . ?
C26 C27 N6 C28 176.7(4) . . . . ?
C36 N7 C35 C28 -133.6(4) . . . . ?
C36 N7 C35 C34 46.3(6) . . . . ?
C38 C39 C40 N8 0.7(5) . . . . ?
C38 C39 C40 C41 178.8(4) . . . . ?
C38 C39 C40 Rb1 72.7(3) . . . . ?
C39 C38 C37 C36 175.3(4) . . . . ?
C39 C38 C37 N8 -0.1(5) . . . . ?
C39 C38 C37 Rb1 -69.8(3) . . . . ?
C39 C40 C41 C1 -117.8(5) . . . . ?
C39 C40 C41 C42 3.8(6) . . . . ?
C39 C40 C41 C43 123.9(5) . . . . ?
C48 N9 C44 C45 -0.1(9) . . . . ?
C49 C50 C51 C52 -0.1(10) . . . . ?
C50 C49 N10 C53 -1.8(11) . . . . ?
C50 C49 N10 Rb1 165.8(6) . . . . ?
C50 C51 C52 C53 -0.8(10) . . . . ?
C51 C52 C53 N10 0.4(10) . . . . ?
C52 C53 N10 C49 0.8(10) . . . . ?
C52 C53 N10 Rb1 -165.0(5) . . . . ?
C54 C55 C56 C57 1.8(15) . . . . ?
C55 C54 N11 C58 1.1(10) . . . . ?
C55 C54 N11 Rb1 -155.5(6) . . . . ?
C55 C56 C57 C58 -1.4(15) . . . . ?
C56 C57 C58 N11 0.8(14) . . . . ?
C56 C57 C58 Rb1 59(2) . . . . ?
C57 C58 N11 C54 -0.7(11) . . . . ?
C57 C58 N11 Rb1 159.2(7) . . . . ?
C59 C60 C61 C62 0(3) . . . . ?
C60 C59 N12 C63 0.5(16) . . . . ?
C60 C59 N12 Rb1 156.5(10) . . . . ?
C60 C61 C62 C63 0(2) . . . . ?
C61 C62 C63 N12 0.7(18) . . . . ?
C61 C62 C63 Rb1 -88(4) . . . . ?
C62 C63 N12 C59 -0.8(14) . . . . ?
C62 C63 N12 Rb1 -164.1(9) . . . . ?
C67 C68 N13 C64 -2.1(11) . . . . ?
C78 N15 C74 C75 -1.8(12) . . . . ?
N1 C1 C2 C3 -1.2(6) . . . . ?
N1 C1 C2 Rb1 78.1(3) . . . . ?
N1 C1 C41 C40 -62.8(5) . . . . ?
N1 C1 C41 C42 175.9(4) . . . . ?
N1 C1 C41 C43 56.1(5) . . . . ?
N1 C4 C5 N2 2.4(7) . . . . ?
N3 C15 C16 N4 3.1(6) . . . . ?
N3 C15 C16 C17 -176.0(5) . . . . ?
N4 C16 C17 C18 0.3(5) . . . . ?
N4 C19 C20 C21 -173.6(4) . . . . ?
N4 C19 C20 C23 67.0(5) . . . . ?
N4 C19 C20 C22 -54.1(5) . . . . ?
N7 C36 C37 C38 -174.8(4) . . . . ?
N7 C36 C37 N8 0.3(6) . . . . ?
N7 C36 C37 Rb1 83.0(4) . . . . ?
N8 C40 C41 C1 60.1(5) . . . . ?
N8 C40 C41 C42 -178.3(4) . . . . ?
N8 C40 C41 C43 -58.2(5) . . . . ?
N9 C48 C47 C46 -1.8(9) . . . . ?
N9 C44 C45 C46 0.5(13) . . . . ?
N10 C49 C50 C51 1.5(12) . . . . ?
N11 C54 C55 C56 -1.7(13) . . . . ?
N12 C59 C60 C61 0(2) . . . . ?
C69 C70 C71 C72 0.2(11) . . . . ?
N15 C78 C77 C76 -3.9(13) . . . . ?
N15 C74 C75 C76 -1.7(12) . . . . ?
C1 N1 C4 C3 -1.4(5) . . . . ?
C1 N1 C4 C5 176.7(4) . . . . ?
C1 N1 C4 Rb1 -77.6(3) . . . . ?
C1 C2 C3 C4 0.4(6) . . . . ?
C2 C1 C41 C40 116.2(5) . . . . ?
C2 C1 C41 C42 -5.1(6) . . . . ?
C2 C1 C41 C43 -124.9(5) . . . . ?
C2 C3 C4 N1 0.6(6) . . . . ?
C2 C3 C4 C5 -177.2(5) . . . . ?
C2 C3 C4 Rb1 65.2(4) . . . . ?
C3 C4 C5 N2 -179.9(5) . . . . ?
C4 N1 C1 C2 1.6(5) . . . . ?
C4 N1 C1 C41 -179.2(4) . . . . ?
C4 N1 C1 Rb1 86.6(3) . . . . ?
C4 C5 N2 C6 175.7(4) . . . . ?
C4 C5 N2 U1 19.0(5) . . . . ?
C6 C7 C8 C9 -179.2(5) . . . . ?
C6 C7 C8 C10 2.4(7) . . . . ?
C7 C6 C13 N3 176.9(4) . . . . ?
C7 C6 C13 C12 -4.1(7) . . . . ?
C7 C6 N2 C5 -39.5(6) . . . . ?
C7 C6 N2 U1 114.8(4) . . . . ?
C7 C8 C10 C11 176.0(5) . . . . ?
C7 C8 C10 C12 -3.9(7) . . . . ?
C8 C10 C12 C13 1.4(8) . . . . ?
C9 C8 C10 C11 -2.3(8) . . . . ?
C9 C8 C10 C12 177.8(5) . . . . ?
C10 C12 C13 N3 -178.4(4) . . . . ?
C10 C12 C13 C6 2.7(7) . . . . ?
C13 N3 C15 C16 -179.7(4) . . . . ?
C13 C6 C7 C8 1.6(7) . . . . ?
C13 C6 N2 C5 142.2(4) . . . . ?
C13 C6 N2 U1 -63.6(5) . . . . ?
C15 N3 C13 C6 -142.6(4) . . . . ?
C15 N3 C13 C12 38.4(7) . . . . ?
C15 C16 C17 C18 179.5(4) . . . . ?
C16 N4 C19 C18 0.3(5) . . . . ?
C16 N4 C19 C20 -177.0(4) . . . . ?
C16 C17 C18 C19 -0.1(5) . . . . ?
C17 C18 C19 N4 -0.1(5) . . . . ?
C17 C18 C19 C20 176.9(4) . . . . ?
C18 C19 C20 C21 9.7(7) . . . . ?
C18 C19 C20 C23 -109.6(5) . . . . ?
C18 C19 C20 C22 129.3(5) . . . . ?
C19 N4 C16 C15 -179.6(4) . . . . ?
C19 N4 C16 C17 -0.4(5) . . . . ?
C20 C23 C24 C25 -177.0(4) . . . . ?
C20 C23 N5 C26 177.3(4) . . . . ?
C25 C26 C27 N6 177.5(5) . . . . ?
C25 C26 N5 C23 0.1(5) . . . . ?
C27 C26 C25 C24 -178.1(5) . . . . ?
C27 C26 N5 C23 178.3(4) . . . . ?
C28 C29 C30 C31 177.7(5) . . . . ?
C28 C29 C30 C32 -0.4(8) . . . . ?
C29 C28 C35 N7 -179.9(4) . . . . ?
C29 C28 C35 C34 0.2(7) . . . . ?
C29 C28 N6 C27 -33.5(7) . . . . ?
C29 C30 C32 C33 179.5(5) . . . . ?
C29 C30 C32 C34 0.5(8) . . . . ?
C30 C32 C34 C35 -0.3(8) . . . . ?
C31 C30 C32 C33 1.4(9) . . . . ?
C31 C30 C32 C34 -177.6(5) . . . . ?
C32 C34 C35 N7 180.0(4) . . . . ?
C32 C34 C35 C28 -0.1(7) . . . . ?
C33 C32 C34 C35 -179.3(5) . . . . ?
C35 C28 C29 C30 0.1(7) . . . . ?
C35 C28 N6 C27 149.6(4) . . . . ?
C37 C36 N7 C35 -179.9(4) . . . . ?
C37 C36 N7 U1 -21.5(5) . . . . ?
C37 C38 C39 C40 -0.4(5) . . . . ?
C37 C38 C39 Rb1 66.3(3) . . . . ?
C37 N8 C40 C39 -0.8(5) . . . . ?
C37 N8 C40 C41 -179.1(4) . . . . ?
C37 N8 C40 Rb1 -79.3(3) . . . . ?
C40 N8 C37 C36 -175.4(4) . . . . ?
C40 N8 C37 C38 0.6(5) . . . . ?
C40 N8 C37 Rb1 77.9(3) . . . . ?
C41 C1 C2 C3 179.7(4) . . . . ?
C41 C1 C2 Rb1 -101.0(5) . . . . ?
C44 C45 C46 C47 -1.6(14) . . . . ?
C45 C46 C47 C48 2.2(12) . . . . ?
C47 C48 N9 C44 0.8(7) . . . . ?
C47 C48 N9 U1 175.0(4) . . . . ?
C64 C65 C66 C67 -4.6(13) . . . . ?
C65 C64 N13 C68 0.0(11) . . . . ?
C66 C67 C68 N13 1.1(13) . . . . ?
C68 C67 C66 C65 2.3(14) . . . . ?
C70 C69 N14 C73 -0.3(11) . . . . ?
C70 C71 C72 C73 -0.3(13) . . . . ?
C71 C72 C73 N14 0.2(13) . . . . ?
C72 C73 N14 C69 0.1(12) . . . . ?
N14 C69 C70 C71 0.1(10) . . . . ?
N2 C6 C7 C8 -176.8(4) . . . . ?
N2 C6 C13 N3 -4.7(6) . . . . ?
N2 C6 C13 C12 174.3(4) . . . . ?
N5 C23 C24 C25 0.0(5) . . . . ?
N5 C23 C20 C21 174.6(4) . . . . ?
N5 C23 C20 C19 -66.1(5) . . . . ?
N5 C23 C20 C22 55.1(5) . . . . ?
N5 C26 C25 C24 -0.1(5) . . . . ?
N5 C26 C27 N6 -0.3(6) . . . . ?
N6 C28 C29 C30 -176.8(5) . . . . ?
N6 C28 C35 N7 -2.8(6) . . . . ?
N6 C28 C35 C34 177.3(4) . . . . ?
N13 C64 C65 C66 3.4(12) . . . . ?
Rb1 C38 C39 C40 -66.7(3) . . . . ?
Rb1 C38 C37 C36 -114.9(5) . . . . ?
Rb1 C38 C37 N8 69.6(3) . . . . ?
Rb1 C39 C40 N8 -71.9(3) . . . . ?
Rb1 C39 C40 C41 106.1(5) . . . . ?
Rb1 C58 N11 C54 -159.9(7) . . . . ?
Rb1 C63 N12 C59 163.2(9) . . . . ?
Rb1 N1 C1 C2 -85.0(4) . . . . ?
Rb1 N1 C1 C41 94.2(4) . . . . ?
Rb1 N1 C4 C3 76.2(4) . . . . ?
Rb1 N1 C4 C5 -105.7(4) . . . . ?
Rb1 N8 C37 C36 106.8(4) . . . . ?
Rb1 N8 C37 C38 -77.3(3) . . . . ?
Rb1 N8 C40 C39 78.5(3) . . . . ?
Rb1 N8 C40 C41 -99.8(4) . . . . ?
Rb1 O2 U1 N1 -40.32(14) . . . . ?
Rb1 O2 U1 N7 93.55(14) . . . . ?
Rb1 O2 U1 N8 29.01(14) . . . . ?
Rb1 O2 U1 N9 171.82(15) . . . . ?
Rb1 O2 U1 N2 -104.74(15) . . . . ?
Rb1 C1 C2 C3 -79.3(4) . . . . ?
Rb1 C1 C41 C40 19.9(3) . . . . ?
Rb1 C1 C41 C42 -101.4(3) . . . . ?
Rb1 C1 C41 C43 138.7(3) . . . . ?
Rb1 C2 C3 C4 -65.7(4) . . . . ?
Rb1 C4 C5 N2 -75.0(5) . . . . ?
Rb1 C40 C41 C1 -21.5(3) . . . . ?
Rb1 C40 C41 C42 100.1(3) . . . . ?
Rb1 C40 C41 C43 -139.7(3) . . . . ?
U1 N1 C1 C2 -151.6(3) . . . . ?
U1 N1 C1 C41 27.6(6) . . . . ?
U1 N1 C1 Rb1 -66.6(3) . . . . ?
U1 N1 C4 C3 158.2(3) . . . . ?
U1 N1 C4 C5 -23.7(5) . . . . ?
U1 N1 C4 Rb1 82.00(18) . . . . ?
U1 N7 C35 C28 71.3(5) . . . . ?
U1 N7 C35 C34 -108.7(4) . . . . ?
U1 N8 C37 C36 22.7(5) . . . . ?
U1 N8 C37 C38 -161.3(3) . . . . ?
U1 N8 C37 Rb1 -84.04(17) . . . . ?
U1 N8 C40 C39 155.0(3) . . . . ?
U1 N8 C40 C41 -23.3(6) . . . . ?
U1 N8 C40 Rb1 76.5(3) . . . . ?
U1 N9 C44 C45 -174.5(6) . . . . ?
C74 C75 C76 C77 2.5(11) . . . . ?
C75 C76 C77 C78 0.2(11) . . . . ?
C77 C78 N15 C74 4.7(13) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_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
-19 -5 -7 0.4127 -19.0000 -4.9998 -7.0000 -0.0672 0.7519 -0.6839
19 5 7 0.4127 19.0000 4.9998 7.0000 0.0672 -0.7519 0.6839
6 -28 -10 0.6029 5.9999 -27.9997 -10.0000 0.0436 -0.7409 -0.6746
-6 28 10 0.6029 -5.9999 27.9997 10.0000 -0.0436 0.7409 0.6746
3 -24 21 0.2909 2.9999 -23.9996 20.9999 -0.7854 -0.5470 -0.3018
-3 24 -21 0.2909 -2.9999 23.9996 -20.9999 0.7854 0.5470 0.3018
-9 -9 29 0.2088 -9.0000 -8.9997 28.9999 -0.9748 0.2358 -0.1320
13 20 -12 0.4126 13.0000 19.9996 -11.9999 0.6725 -0.2272 0.7030
12 13 -22 0.4821 12.0000 12.9996 -21.9999 0.8594 -0.3009 0.3876
1 12 -32 0.3082 1.0000 11.9997 -31.9999 1.0010 0.1681 -0.0264
2 -22 24 0.2147 2.0000 -21.9996 23.9999 -0.8564 -0.4695 -0.2424
10 7 28 0.4662 10.0000 7.0000 28.0000 -0.5768 -0.3261 0.7430
-6 -29 1 0.4097 -6.0001 -28.9996 0.9999 -0.3934 -0.2324 -0.8792
-12 -18 18 0.2910 -12.0000 -17.9996 17.9999 -0.8032 0.2162 -0.5598
7 10 30 0.4649 7.0000 10.0000 30.0000 -0.6319 -0.1432 0.7663
-14 21 1 0.4675 -13.9999 20.9998 1.0000 0.0408 0.9750 0.1942
2 -21 -25 0.5574 1.9999 -20.9999 -25.0000 0.4791 -0.4420 -0.7644

_olex2_date_sample_data_collection 2015-02-05
_olex2_date_sample_submission    2015-02-05
_olex2_exptl_crystal_mounting_method 'glass fibre'
_olex2_submission_original_sample_id RML119
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_po4056_refinalized
_database_code_depnum_ccdc_archive 'CCDC 1883756'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;university of edinburgh
United Kingdom
;
_audit_update_record             
;
2018-12-07 deposited with the CCDC.	2019-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C62 H62 I N12 O2 U Zn'
_chemical_formula_weight         1437.54

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'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'

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

_cell_length_a                   13.27300(10)
_cell_length_b                   16.43680(10)
_cell_length_c                   27.8646(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6079.10(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    47386
_cell_measurement_theta_min      3.6740
_cell_measurement_theta_max      76.1280

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.1234
_exptl_crystal_size_mid          0.0547
_exptl_crystal_size_min          0.0264
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2836
_exptl_absorpt_coefficient_mu    12.323
_exptl_absorpt_correction_T_min  0.69232
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            99868
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         76.49
_reflns_number_total             12683
_reflns_number_gt                12267
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_structure_solution    'Direct Methods, SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    MERCURY
_computing_publication_material  ORTEP

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0272P)²+5.8603P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.020(2)
_refine_ls_number_reflns         12683
_refine_ls_number_parameters     720
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0202
_refine_ls_wR_factor_ref         0.0473
_refine_ls_wR_factor_gt          0.0468
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_restrained_S_all      0.900
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7315(3) 0.45855(19) 0.29671(11) 0.0200(6) Uani 1 1 d . . .
C2 C 0.6705(3) 0.4936(2) 0.33241(13) 0.0256(7) Uani 1 1 d . . .
H2 H 0.6828 0.4931 0.3660 0.031 Uiso 1 1 calc R . .
C3 C 0.5886(3) 0.5293(2) 0.30912(13) 0.0276(8) Uani 1 1 d . . .
H3 H 0.5341 0.5577 0.3235 0.033 Uiso 1 1 calc R . .
C4 C 0.6034(2) 0.5146(2) 0.25983(12) 0.0231(6) Uani 1 1 d . . .
C5 C 0.5401(3) 0.5342(2) 0.22039(13) 0.0242(7) Uani 1 1 d . . .
H5 H 0.4779 0.5611 0.2260 0.029 Uiso 1 1 calc R . .
C6 C 0.5003(3) 0.5384(2) 0.13848(13) 0.0206(7) Uani 1 1 d . . .
C7 C 0.4538(3) 0.6147(2) 0.13586(14) 0.0251(7) Uani 1 1 d . . .
H7 H 0.4654 0.6533 0.1606 0.030 Uiso 1 1 calc R . .
C8 C 0.3908(3) 0.6353(2) 0.09773(14) 0.0273(8) Uani 1 1 d . . .
C9 C 0.3375(3) 0.7163(3) 0.09721(17) 0.0373(9) Uani 1 1 d . . .
H9A H 0.3603 0.7491 0.1245 0.056 Uiso 1 1 calc R . .
H9B H 0.2646 0.7075 0.0996 0.056 Uiso 1 1 calc R . .
H9C H 0.3528 0.7448 0.0672 0.056 Uiso 1 1 calc R . .
C10 C 0.3769(3) 0.5796(2) 0.06004(14) 0.0264(8) Uani 1 1 d . . .
C11 C 0.3119(3) 0.5996(3) 0.01734(16) 0.0362(9) Uani 1 1 d . . .
H11A H 0.3112 0.5532 -0.0048 0.054 Uiso 1 1 calc R . .
H11B H 0.3392 0.6474 0.0009 0.054 Uiso 1 1 calc R . .
H11C H 0.2431 0.6110 0.0281 0.054 Uiso 1 1 calc R . .
C12 C 0.4239(2) 0.5037(2) 0.06284(13) 0.0236(7) Uani 1 1 d . . .
H12 H 0.4152 0.4660 0.0373 0.028 Uiso 1 1 calc R . .
C13 C 0.4835(2) 0.4814(2) 0.10225(12) 0.0206(6) Uani 1 1 d . . .
C14 C 0.4823(2) 0.3416(2) 0.09210(12) 0.0188(6) Uani 1 1 d . . .
H14 H 0.4180 0.3475 0.0775 0.023 Uiso 1 1 calc R . .
C15 C 0.5263(2) 0.2617(2) 0.09606(12) 0.0185(6) Uani 1 1 d . . .
C16 C 0.4898(3) 0.1865(2) 0.08345(12) 0.0220(7) Uani 1 1 d . . .
H16 H 0.4264 0.1755 0.0690 0.026 Uiso 1 1 calc R . .
C17 C 0.5638(3) 0.1284(2) 0.09590(13) 0.0228(7) Uani 1 1 d . . .
H17 H 0.5596 0.0713 0.0911 0.027 Uiso 1 1 calc R . .
C18 C 0.6434(3) 0.1700(2) 0.11626(13) 0.0193(6) Uani 1 1 d . . .
C19 C 0.7442(3) 0.13841(18) 0.13394(11) 0.0200(6) Uani 1 1 d . . .
C20 C 0.7659(3) 0.1698(2) 0.18527(12) 0.0256(7) Uani 1 1 d . . .
H20A H 0.8306 0.1481 0.1964 0.038 Uiso 1 1 calc R . .
H20B H 0.7122 0.1518 0.2069 0.038 Uiso 1 1 calc R . .
H20C H 0.7687 0.2294 0.1850 0.038 Uiso 1 1 calc R . .
C21 C 0.7422(3) 0.0449(2) 0.13524(13) 0.0276(7) Uani 1 1 d . . .
H21A H 0.7328 0.0238 0.1026 0.041 Uiso 1 1 calc R . .
H21B H 0.6864 0.0266 0.1556 0.041 Uiso 1 1 calc R . .
H21C H 0.8060 0.0246 0.1483 0.041 Uiso 1 1 calc R . .
C22 C 0.8256(3) 0.1667(2) 0.09964(13) 0.0208(7) Uani 1 1 d . . .
C23 C 0.8899(3) 0.1231(2) 0.06954(14) 0.0240(7) Uani 1 1 d . . .
H23 H 0.8941 0.0655 0.0672 0.029 Uiso 1 1 calc R . .
C24 C 0.9474(3) 0.1796(2) 0.04324(13) 0.0246(7) Uani 1 1 d . . .
H24 H 0.9974 0.1669 0.0200 0.029 Uiso 1 1 calc R . .
C25 C 0.9183(2) 0.2563(2) 0.05717(12) 0.0196(6) Uani 1 1 d . . .
C26 C 0.9527(2) 0.3356(2) 0.04300(12) 0.0205(7) Uani 1 1 d . . .
H26 H 1.0016 0.3406 0.0183 0.025 Uiso 1 1 calc R . .
C27 C 0.9505(2) 0.4770(2) 0.04930(12) 0.0198(6) Uani 1 1 d . . .
C28 C 0.9689(3) 0.4997(2) 0.00163(12) 0.0221(7) Uani 1 1 d . . .
H28 H 0.9596 0.4607 -0.0231 0.027 Uiso 1 1 calc R . .
C29 C 1.0007(3) 0.5781(2) -0.01042(14) 0.0255(7) Uani 1 1 d . . .
C30 C 1.0200(4) 0.6002(3) -0.06226(15) 0.0359(9) Uani 1 1 d . . .
H30A H 1.0927 0.6053 -0.0676 0.054 Uiso 1 1 calc R . .
H30B H 0.9871 0.6521 -0.0696 0.054 Uiso 1 1 calc R . .
H30C H 0.9927 0.5576 -0.0831 0.054 Uiso 1 1 calc R . .
C31 C 1.0155(3) 0.6353(2) 0.02649(14) 0.0260(7) Uani 1 1 d . . .
C32 C 1.0512(3) 0.7211(2) 0.01537(16) 0.0346(9) Uani 1 1 d . . .
H32A H 0.9974 0.7511 -0.0009 0.052 Uiso 1 1 calc R . .
H32B H 1.1106 0.7187 -0.0055 0.052 Uiso 1 1 calc R . .
H32C H 1.0688 0.7489 0.0453 0.052 Uiso 1 1 calc R . .
C33 C 0.9957(3) 0.6133(2) 0.07396(13) 0.0240(7) Uani 1 1 d . . .
H33 H 1.0051 0.6521 0.0988 0.029 Uiso 1 1 calc R . .
C34 C 0.9626(2) 0.5357(2) 0.08534(12) 0.0195(7) Uani 1 1 d . . .
C35 C 1.0092(2) 0.5235(2) 0.16528(13) 0.0222(6) Uani 1 1 d . . .
H35 H 1.0716 0.5471 0.1560 0.027 Uiso 1 1 calc R . .
C36 C 0.9931(3) 0.5017(2) 0.21404(13) 0.0219(7) Uani 1 1 d . . .
C37 C 1.0607(3) 0.5022(2) 0.25266(13) 0.0241(8) Uani 1 1 d . . .
H37 H 1.1281 0.5216 0.2524 0.029 Uiso 1 1 calc R . .
C38 C 1.0091(3) 0.4686(2) 0.29143(12) 0.0231(7) Uani 1 1 d . . .
H38 H 1.0347 0.4606 0.3229 0.028 Uiso 1 1 calc R . .
C39 C 0.9119(3) 0.4488(2) 0.27500(12) 0.0189(6) Uani 1 1 d . . .
C40 C 0.8274(3) 0.4091(2) 0.30236(12) 0.0214(7) Uani 1 1 d . . .
C41 C 0.8550(3) 0.4010(3) 0.35542(13) 0.0280(8) Uani 1 1 d . . .
H41A H 0.9130 0.3646 0.3588 0.042 Uiso 1 1 calc R . .
H41B H 0.7976 0.3787 0.3731 0.042 Uiso 1 1 calc R . .
H41C H 0.8722 0.4547 0.3684 0.042 Uiso 1 1 calc R . .
C42 C 0.8094(3) 0.3229(2) 0.28220(13) 0.0250(7) Uani 1 1 d . . .
H42A H 0.7949 0.3264 0.2478 0.038 Uiso 1 1 calc R . .
H42B H 0.7522 0.2979 0.2988 0.038 Uiso 1 1 calc R . .
H42C H 0.8698 0.2897 0.2872 0.038 Uiso 1 1 calc R . .
C43 C 0.7240(3) 0.5846(2) 0.06091(14) 0.0305(8) Uani 1 1 d . . .
H43 H 0.7333 0.6286 0.0825 0.037 Uiso 1 1 calc R . .
C44 C 0.7148(4) 0.6012(3) 0.01258(17) 0.0478(13) Uani 1 1 d . . .
H44 H 0.7184 0.6555 0.0010 0.057 Uiso 1 1 calc R . .
C45 C 0.6998(4) 0.5359(3) -0.01894(15) 0.0525(14) Uani 1 1 d . . .
H45 H 0.6923 0.5454 -0.0524 0.063 Uiso 1 1 calc R . .
C46 C 0.6960(3) 0.4579(3) -0.00119(14) 0.0356(9) Uani 1 1 d . . .
H46 H 0.6862 0.4128 -0.0220 0.043 Uiso 1 1 calc R . .
C47 C 0.7067(3) 0.4467(2) 0.04752(13) 0.0248(7) Uani 1 1 d . . .
H47 H 0.7043 0.3928 0.0597 0.030 Uiso 1 1 calc R . .
C48 C 0.6141(3) 0.7233(3) 0.25891(15) 0.0301(8) Uani 1 1 d . . .
H48 H 0.6571 0.6853 0.2745 0.036 Uiso 1 1 calc R . .
C49 C 0.5263(3) 0.7473(3) 0.28186(16) 0.0356(9) Uani 1 1 d . . .
H49 H 0.5093 0.7262 0.3126 0.043 Uiso 1 1 calc R . .
C50 C 0.4641(3) 0.8024(3) 0.25919(16) 0.0345(9) Uani 1 1 d . . .
H50 H 0.4043 0.8208 0.2744 0.041 Uiso 1 1 calc R . .
C51 C 0.4899(3) 0.8304(3) 0.21423(17) 0.0357(9) Uani 1 1 d . . .
H51 H 0.4473 0.8673 0.1976 0.043 Uiso 1 1 calc R . .
C52 C 0.5785(3) 0.8038(2) 0.19383(14) 0.0300(8) Uani 1 1 d . . .
H52 H 0.5962 0.8233 0.1629 0.036 Uiso 1 1 calc R . .
C53 C 0.8629(3) 0.6516(2) 0.27544(13) 0.0258(7) Uani 1 1 d . . .
H53 H 0.8264 0.6043 0.2665 0.031 Uiso 1 1 calc R . .
C54 C 0.9123(3) 0.6530(2) 0.31909(14) 0.0295(8) Uani 1 1 d . . .
H54 H 0.9087 0.6076 0.3401 0.035 Uiso 1 1 calc R . .
C55 C 0.9664(3) 0.7206(3) 0.33162(17) 0.0361(9) Uani 1 1 d . . .
H55 H 1.0003 0.7226 0.3616 0.043 Uiso 1 1 calc R . .
C56 C 0.9715(3) 0.7852(3) 0.30077(18) 0.0396(10) Uani 1 1 d . . .
H56 H 1.0102 0.8320 0.3086 0.048 Uiso 1 1 calc R . .
C57 C 0.9192(3) 0.7810(3) 0.25782(16) 0.0332(9) Uani 1 1 d . . .
H57 H 0.9217 0.8261 0.2365 0.040 Uiso 1 1 calc R . .
C58 C 0.7198(3) 0.2031(3) -0.01856(18) 0.0449(11) Uani 1 1 d . . .
H58 H 0.7231 0.2224 0.0135 0.054 Uiso 1 1 calc R . .
C59 C 0.7023(3) 0.1210(3) -0.0254(2) 0.0448(11) Uani 1 1 d . . .
H59 H 0.6947 0.0855 0.0013 0.054 Uiso 1 1 calc R . .
C60 C 0.6961(4) 0.0920(4) -0.0715(2) 0.0529(13) Uani 1 1 d . . .
H60 H 0.6836 0.0361 -0.0775 0.064 Uiso 1 1 calc R . .
C61 C 0.7085(4) 0.1458(5) -0.1087(2) 0.0645(18) Uani 1 1 d . . .
H61 H 0.7047 0.1279 -0.1410 0.077 Uiso 1 1 calc R . .
C62 C 0.7267(4) 0.2262(4) -0.0981(2) 0.0641(16) Uani 1 1 d . . .
H62 H 0.7359 0.2626 -0.1242 0.077 Uiso 1 1 calc R . .
N1 N 0.6913(2) 0.47198(18) 0.25223(10) 0.0190(5) Uani 1 1 d . . .
N2 N 0.5658(2) 0.51613(19) 0.17696(10) 0.0209(5) Uani 1 1 d . . .
N3 N 0.5276(2) 0.40395(19) 0.10770(11) 0.0209(6) Uani 1 1 d . . .
N4 N 0.6199(2) 0.25073(17) 0.11643(11) 0.0183(5) Uani 1 1 d . . .
H4 H 0.6585 0.2898 0.1278 0.022 Uiso 1 1 calc R . .
N5 N 0.8441(2) 0.24731(17) 0.09158(10) 0.0172(5) Uani 1 1 d . . .
H5A H 0.8132 0.2877 0.1062 0.021 Uiso 1 1 calc R . .
N6 N 0.9180(2) 0.39961(18) 0.06344(10) 0.0182(5) Uani 1 1 d . . .
N7 N 0.9399(2) 0.51183(19) 0.13328(10) 0.0216(6) Uani 1 1 d . . .
N8 N 0.9016(2) 0.46885(17) 0.22763(10) 0.0183(5) Uani 1 1 d . . .
N9 N 0.7204(2) 0.50822(18) 0.07873(10) 0.0218(6) Uani 1 1 d . . .
N10 N 0.6408(2) 0.75168(18) 0.21570(11) 0.0220(6) Uani 1 1 d . . .
N11 N 0.8652(2) 0.71555(19) 0.24532(11) 0.0213(6) Uani 1 1 d . . .
N12 N 0.7324(3) 0.2570(3) -0.05377(16) 0.0494(10) Uani 1 1 d . . .
O1 O 0.75458(19) 0.37037(14) 0.15762(7) 0.0218(5) Uani 1 1 d . . .
O2 O 0.76307(19) 0.59783(14) 0.17553(8) 0.0222(5) Uani 1 1 d . . .
Zn1 Zn 0.77548(3) 0.71344(3) 0.186158(15) 0.01998(9) Uani 1 1 d . . .
I1 I 0.82428(2) 0.805151(15) 0.117129(9) 0.03029(6) Uani 1 1 d . . .
U1 U 0.759947(7) 0.482246(6) 0.168919(3) 0.01494(3) Uani 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.367(4) . ?
C1 C2 1.406(5) . ?
C1 C40 1.518(5) . ?
C2 C3 1.396(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.408(5) . ?
C3 H3 0.9500 . ?
C4 N1 1.377(5) . ?
C4 C5 1.420(5) . ?
C5 N2 1.292(5) . ?
C5 H5 0.9500 . ?
C6 C13 1.395(5) . ?
C6 C7 1.400(5) . ?
C6 N2 1.428(4) . ?
C7 C8 1.394(5) . ?
C7 H7 0.9500 . ?
C8 C10 1.405(5) . ?
C8 C9 1.508(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C12 1.398(5) . ?
C10 C11 1.506(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.402(5) . ?
C12 H12 0.9500 . ?
C13 N3 1.410(5) . ?
C14 N3 1.266(5) . ?
C14 C15 1.442(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.373(5) . ?
C15 N4 1.378(4) . ?
C16 C17 1.413(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.380(5) . ?
C17 H17 0.9500 . ?
C18 N4 1.363(4) . ?
C18 C19 1.518(5) . ?
C19 C22 1.515(5) . ?
C19 C21 1.538(4) . ?
C19 C20 1.548(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 N5 1.366(4) . ?
C22 C23 1.395(5) . ?
C23 C24 1.408(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.375(5) . ?
C24 H24 0.9500 . ?
C25 N5 1.383(4) . ?
C25 C26 1.436(5) . ?
C26 N6 1.282(5) . ?
C26 H26 0.9500 . ?
C27 N6 1.400(5) . ?
C27 C28 1.401(5) . ?
C27 C34 1.402(5) . ?
C28 C29 1.397(5) . ?
C28 H28 0.9500 . ?
C29 C31 1.407(6) . ?
C29 C30 1.511(5) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C33 1.396(5) . ?
C31 C32 1.521(5) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.385(5) . ?
C33 H33 0.9500 . ?
C34 N7 1.425(4) . ?
C35 N7 1.295(4) . ?
C35 C36 1.421(5) . ?
C35 H35 0.9500 . ?
C36 N8 1.381(4) . ?
C36 C37 1.401(5) . ?
C37 C38 1.394(5) . ?
C37 H37 0.9500 . ?
C38 C39 1.407(5) . ?
C38 H38 0.9500 . ?
C39 N8 1.368(4) . ?
C39 C40 1.505(5) . ?
C40 C41 1.529(4) . ?
C40 C42 1.543(5) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 N9 1.350(5) . ?
C43 C44 1.380(6) . ?
C43 H43 0.9500 . ?
C44 C45 1.401(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.375(7) . ?
C45 H45 0.9500 . ?
C46 C47 1.377(5) . ?
C46 H46 0.9500 . ?
C47 N9 1.346(5) . ?
C47 H47 0.9500 . ?
C48 N10 1.339(5) . ?
C48 C49 1.387(6) . ?
C48 H48 0.9500 . ?
C49 C50 1.378(6) . ?
C49 H49 0.9500 . ?
C50 C51 1.378(6) . ?
C50 H50 0.9500 . ?
C51 C52 1.378(6) . ?
C51 H51 0.9500 . ?
C52 N10 1.336(5) . ?
C52 H52 0.9500 . ?
C53 N11 1.345(5) . ?
C53 C54 1.382(5) . ?
C53 H53 0.9500 . ?
C54 C55 1.368(6) . ?
C54 H54 0.9500 . ?
C55 C56 1.369(7) . ?
C55 H55 0.9500 . ?
C56 C57 1.386(6) . ?
C56 H56 0.9500 . ?
C57 N11 1.339(5) . ?
C57 H57 0.9500 . ?
C58 N12 1.333(7) . ?
C58 C59 1.381(7) . ?
C58 H58 0.9500 . ?
C59 C60 1.374(8) . ?
C59 H59 0.9500 . ?
C60 C61 1.371(9) . ?
C60 H60 0.9500 . ?
C61 C62 1.376(9) . ?
C61 H61 0.9500 . ?
C62 N12 1.337(8) . ?
C62 H62 0.9500 . ?
N1 U1 2.499(3) . ?
N2 U1 2.645(3) . ?
N4 H4 0.8800 . ?
N5 H5A 0.8800 . ?
N7 U1 2.632(3) . ?
N8 U1 2.502(3) . ?
N9 U1 2.602(3) . ?
N10 Zn1 2.067(3) . ?
N11 Zn1 2.034(3) . ?
O1 U1 1.867(2) . ?
O2 U1 1.909(2) . ?
O2 Zn1 1.930(2) . ?
Zn1 I1 2.5282(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 110.5(3) . . ?
N1 C1 C40 120.5(3) . . ?
C2 C1 C40 128.9(3) . . ?
C3 C2 C1 107.0(3) . . ?
C3 C2 H2 126.5 . . ?
C1 C2 H2 126.5 . . ?
C2 C3 C4 105.8(3) . . ?
C2 C3 H3 127.1 . . ?
C4 C3 H3 127.1 . . ?
N1 C4 C3 110.8(3) . . ?
N1 C4 C5 119.8(3) . . ?
C3 C4 C5 129.3(3) . . ?
N2 C5 C4 121.1(3) . . ?
N2 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C13 C6 C7 119.6(3) . . ?
C13 C6 N2 118.0(3) . . ?
C7 C6 N2 122.5(3) . . ?
C8 C7 C6 121.4(3) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
C7 C8 C10 119.4(3) . . ?
C7 C8 C9 120.2(4) . . ?
C10 C8 C9 120.4(4) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C12 C10 C8 118.8(3) . . ?
C12 C10 C11 119.6(4) . . ?
C8 C10 C11 121.6(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 C13 121.9(3) . . ?
C10 C12 H12 119.0 . . ?
C13 C12 H12 119.0 . . ?
C6 C13 C12 118.8(3) . . ?
C6 C13 N3 117.5(3) . . ?
C12 C13 N3 123.7(3) . . ?
N3 C14 C15 121.3(3) . . ?
N3 C14 H14 119.4 . . ?
C15 C14 H14 119.4 . . ?
C16 C15 N4 107.8(3) . . ?
C16 C15 C14 131.1(3) . . ?
N4 C15 C14 121.1(3) . . ?
C15 C16 C17 107.4(3) . . ?
C15 C16 H16 126.3 . . ?
C17 C16 H16 126.3 . . ?
C18 C17 C16 107.4(3) . . ?
C18 C17 H17 126.3 . . ?
C16 C17 H17 126.3 . . ?
N4 C18 C17 108.0(3) . . ?
N4 C18 C19 122.2(3) . . ?
C17 C18 C19 129.7(3) . . ?
C22 C19 C18 108.6(3) . . ?
C22 C19 C21 109.5(3) . . ?
C18 C19 C21 109.5(3) . . ?
C22 C19 C20 110.4(3) . . ?
C18 C19 C20 110.5(3) . . ?
C21 C19 C20 108.4(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N5 C22 C23 106.9(3) . . ?
N5 C22 C19 122.0(3) . . ?
C23 C22 C19 131.1(3) . . ?
C22 C23 C24 107.8(3) . . ?
C22 C23 H23 126.1 . . ?
C24 C23 H23 126.1 . . ?
C25 C24 C23 107.8(3) . . ?
C25 C24 H24 126.1 . . ?
C23 C24 H24 126.1 . . ?
C24 C25 N5 107.3(3) . . ?
C24 C25 C26 131.7(3) . . ?
N5 C25 C26 121.0(3) . . ?
N6 C26 C25 120.6(3) . . ?
N6 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
N6 C27 C28 124.2(3) . . ?
N6 C27 C34 117.3(3) . . ?
C28 C27 C34 118.4(3) . . ?
C29 C28 C27 121.8(3) . . ?
C29 C28 H28 119.1 . . ?
C27 C28 H28 119.1 . . ?
C28 C29 C31 118.8(3) . . ?
C28 C29 C30 120.2(4) . . ?
C31 C29 C30 121.0(4) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C33 C31 C29 119.6(4) . . ?
C33 C31 C32 119.5(4) . . ?
C29 C31 C32 120.9(4) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C31 121.0(3) . . ?
C34 C33 H33 119.5 . . ?
C31 C33 H33 119.5 . . ?
C33 C34 C27 120.4(3) . . ?
C33 C34 N7 122.4(3) . . ?
C27 C34 N7 117.2(3) . . ?
N7 C35 C36 120.9(3) . . ?
N7 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
N8 C36 C37 110.8(3) . . ?
N8 C36 C35 119.5(3) . . ?
C37 C36 C35 129.5(3) . . ?
C38 C37 C36 106.2(3) . . ?
C38 C37 H37 126.9 . . ?
C36 C37 H37 126.9 . . ?
C37 C38 C39 106.9(3) . . ?
C37 C38 H38 126.6 . . ?
C39 C38 H38 126.6 . . ?
N8 C39 C38 110.5(3) . . ?
N8 C39 C40 121.3(3) . . ?
C38 C39 C40 128.2(3) . . ?
C39 C40 C1 109.9(3) . . ?
C39 C40 C41 110.4(3) . . ?
C1 C40 C41 110.4(3) . . ?
C39 C40 C42 109.2(3) . . ?
C1 C40 C42 108.9(3) . . ?
C41 C40 C42 108.0(3) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N9 C43 C44 122.7(4) . . ?
N9 C43 H43 118.6 . . ?
C44 C43 H43 118.6 . . ?
C43 C44 C45 118.2(4) . . ?
C43 C44 H44 120.9 . . ?
C45 C44 H44 120.9 . . ?
C46 C45 C44 119.6(4) . . ?
C46 C45 H45 120.2 . . ?
C44 C45 H45 120.2 . . ?
C45 C46 C47 118.4(4) . . ?
C45 C46 H46 120.8 . . ?
C47 C46 H46 120.8 . . ?
N9 C47 C46 123.4(4) . . ?
N9 C47 H47 118.3 . . ?
C46 C47 H47 118.3 . . ?
N10 C48 C49 122.6(4) . . ?
N10 C48 H48 118.7 . . ?
C49 C48 H48 118.7 . . ?
C50 C49 C48 118.6(4) . . ?
C50 C49 H49 120.7 . . ?
C48 C49 H49 120.7 . . ?
C51 C50 C49 119.2(4) . . ?
C51 C50 H50 120.4 . . ?
C49 C50 H50 120.4 . . ?
C50 C51 C52 118.7(4) . . ?
C50 C51 H51 120.6 . . ?
C52 C51 H51 120.6 . . ?
N10 C52 C51 122.9(4) . . ?
N10 C52 H52 118.6 . . ?
C51 C52 H52 118.6 . . ?
N11 C53 C54 121.7(4) . . ?
N11 C53 H53 119.2 . . ?
C54 C53 H53 119.2 . . ?
C55 C54 C53 119.2(4) . . ?
C55 C54 H54 120.4 . . ?
C53 C54 H54 120.4 . . ?
C56 C55 C54 119.8(4) . . ?
C56 C55 H55 120.1 . . ?
C54 C55 H55 120.1 . . ?
C55 C56 C57 118.6(4) . . ?
C55 C56 H56 120.7 . . ?
C57 C56 H56 120.7 . . ?
N11 C57 C56 122.3(4) . . ?
N11 C57 H57 118.9 . . ?
C56 C57 H57 118.9 . . ?
N12 C58 C59 124.7(5) . . ?
N12 C58 H58 117.6 . . ?
C59 C58 H58 117.6 . . ?
C60 C59 C58 118.5(5) . . ?
C60 C59 H59 120.8 . . ?
C58 C59 H59 120.8 . . ?
C61 C60 C59 118.5(6) . . ?
C61 C60 H60 120.8 . . ?
C59 C60 H60 120.8 . . ?
C60 C61 C62 118.6(5) . . ?
C60 C61 H61 120.7 . . ?
C62 C61 H61 120.7 . . ?
N12 C62 C61 124.9(6) . . ?
N12 C62 H62 117.6 . . ?
C61 C62 H62 117.6 . . ?
C1 N1 C4 105.8(3) . . ?
C1 N1 U1 135.3(2) . . ?
C4 N1 U1 114.7(2) . . ?
C5 N2 C6 118.9(3) . . ?
C5 N2 U1 112.7(2) . . ?
C6 N2 U1 125.7(2) . . ?
C14 N3 C13 119.8(3) . . ?
C18 N4 C15 109.4(3) . . ?
C18 N4 H4 125.3 . . ?
C15 N4 H4 125.3 . . ?
C22 N5 C25 110.2(3) . . ?
C22 N5 H5A 124.9 . . ?
C25 N5 H5A 124.9 . . ?
C26 N6 C27 120.7(3) . . ?
C35 N7 C34 117.0(3) . . ?
C35 N7 U1 114.3(2) . . ?
C34 N7 U1 126.6(2) . . ?
C39 N8 C36 105.7(3) . . ?
C39 N8 U1 136.7(2) . . ?
C36 N8 U1 116.5(2) . . ?
C47 N9 C43 117.7(3) . . ?
C47 N9 U1 121.9(2) . . ?
C43 N9 U1 120.0(2) . . ?
C52 N10 C48 118.0(3) . . ?
C52 N10 Zn1 123.2(3) . . ?
C48 N10 Zn1 118.7(3) . . ?
C57 N11 C53 118.5(3) . . ?
C57 N11 Zn1 122.5(3) . . ?
C53 N11 Zn1 118.6(2) . . ?
C58 N12 C62 114.9(5) . . ?
U1 O2 Zn1 175.07(15) . . ?
O2 Zn1 N11 101.02(11) . . ?
O2 Zn1 N10 106.66(11) . . ?
N11 Zn1 N10 100.28(12) . . ?
O2 Zn1 I1 119.48(7) . . ?
N11 Zn1 I1 117.17(9) . . ?
N10 Zn1 I1 110.08(9) . . ?
O1 U1 O2 175.72(10) . . ?
O1 U1 N1 94.37(9) . . ?
O2 U1 N1 89.17(9) . . ?
O1 U1 N8 93.00(10) . . ?
O2 U1 N8 90.46(10) . . ?
N1 U1 N8 70.17(9) . . ?
O1 U1 N9 89.49(9) . . ?
O2 U1 N9 86.24(9) . . ?
N1 U1 N9 146.57(8) . . ?
N8 U1 N9 142.86(9) . . ?
O1 U1 N7 98.80(10) . . ?
O2 U1 N7 80.38(10) . . ?
N1 U1 N7 133.91(9) . . ?
N8 U1 N7 65.22(9) . . ?
N9 U1 N7 77.78(9) . . ?
O1 U1 N2 100.64(10) . . ?
O2 U1 N2 78.67(10) . . ?
N1 U1 N2 65.20(9) . . ?
N8 U1 N2 134.03(9) . . ?
N9 U1 N2 81.44(8) . . ?
N7 U1 N2 151.27(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
N1 C1 C2 C3 0.8(4) . . . . ?
C40 C1 C2 C3 -177.2(3) . . . . ?
C1 C2 C3 C4 -0.2(4) . . . . ?
C2 C3 C4 N1 -0.5(4) . . . . ?
C2 C3 C4 C5 176.6(4) . . . . ?
N1 C4 C5 N2 -3.3(6) . . . . ?
C3 C4 C5 N2 179.9(4) . . . . ?
C13 C6 C7 C8 0.0(6) . . . . ?
N2 C6 C7 C8 179.4(3) . . . . ?
C6 C7 C8 C10 -2.7(6) . . . . ?
C6 C7 C8 C9 176.8(4) . . . . ?
C7 C8 C10 C12 2.4(6) . . . . ?
C9 C8 C10 C12 -177.1(4) . . . . ?
C7 C8 C10 C11 -178.4(4) . . . . ?
C9 C8 C10 C11 2.1(6) . . . . ?
C8 C10 C12 C13 0.5(6) . . . . ?
C11 C10 C12 C13 -178.7(4) . . . . ?
C7 C6 C13 C12 2.9(5) . . . . ?
N2 C6 C13 C12 -176.5(3) . . . . ?
C7 C6 C13 N3 -176.7(3) . . . . ?
N2 C6 C13 N3 3.8(5) . . . . ?
C10 C12 C13 C6 -3.2(5) . . . . ?
C10 C12 C13 N3 176.4(3) . . . . ?
N3 C14 C15 C16 177.3(4) . . . . ?
N3 C14 C15 N4 -0.9(5) . . . . ?
N4 C15 C16 C17 -0.8(4) . . . . ?
C14 C15 C16 C17 -179.2(4) . . . . ?
C15 C16 C17 C18 0.5(4) . . . . ?
C16 C17 C18 N4 -0.1(4) . . . . ?
C16 C17 C18 C19 -177.0(3) . . . . ?
N4 C18 C19 C22 -67.7(4) . . . . ?
C17 C18 C19 C22 108.8(4) . . . . ?
N4 C18 C19 C21 172.7(3) . . . . ?
C17 C18 C19 C21 -10.8(5) . . . . ?
N4 C18 C19 C20 53.4(4) . . . . ?
C17 C18 C19 C20 -130.1(4) . . . . ?
C18 C19 C22 N5 60.5(4) . . . . ?
C21 C19 C22 N5 -179.9(3) . . . . ?
C20 C19 C22 N5 -60.7(4) . . . . ?
C18 C19 C22 C23 -115.8(4) . . . . ?
C21 C19 C22 C23 3.7(5) . . . . ?
C20 C19 C22 C23 123.0(4) . . . . ?
N5 C22 C23 C24 0.0(4) . . . . ?
C19 C22 C23 C24 176.8(3) . . . . ?
C22 C23 C24 C25 0.0(4) . . . . ?
C23 C24 C25 N5 0.1(4) . . . . ?
C23 C24 C25 C26 178.6(4) . . . . ?
C24 C25 C26 N6 -175.5(4) . . . . ?
N5 C25 C26 N6 2.8(5) . . . . ?
N6 C27 C28 C29 179.7(3) . . . . ?
C34 C27 C28 C29 1.3(5) . . . . ?
C27 C28 C29 C31 0.7(5) . . . . ?
C27 C28 C29 C30 179.9(3) . . . . ?
C28 C29 C31 C33 -1.6(5) . . . . ?
C30 C29 C31 C33 179.2(4) . . . . ?
C28 C29 C31 C32 179.2(3) . . . . ?
C30 C29 C31 C32 0.0(6) . . . . ?
C29 C31 C33 C34 0.5(6) . . . . ?
C32 C31 C33 C34 179.7(3) . . . . ?
C31 C33 C34 C27 1.4(5) . . . . ?
C31 C33 C34 N7 -178.7(3) . . . . ?
N6 C27 C34 C33 179.2(3) . . . . ?
C28 C27 C34 C33 -2.3(5) . . . . ?
N6 C27 C34 N7 -0.6(4) . . . . ?
C28 C27 C34 N7 177.9(3) . . . . ?
N7 C35 C36 N8 -1.2(5) . . . . ?
N7 C35 C36 C37 173.3(4) . . . . ?
N8 C36 C37 C38 0.0(4) . . . . ?
C35 C36 C37 C38 -174.9(4) . . . . ?
C36 C37 C38 C39 0.0(4) . . . . ?
C37 C38 C39 N8 0.0(4) . . . . ?
C37 C38 C39 C40 178.5(3) . . . . ?
N8 C39 C40 C1 -52.4(4) . . . . ?
C38 C39 C40 C1 129.3(4) . . . . ?
N8 C39 C40 C41 -174.4(3) . . . . ?
C38 C39 C40 C41 7.3(5) . . . . ?
N8 C39 C40 C42 67.0(4) . . . . ?
C38 C39 C40 C42 -111.3(4) . . . . ?
N1 C1 C40 C39 59.5(4) . . . . ?
C2 C1 C40 C39 -122.8(4) . . . . ?
N1 C1 C40 C41 -178.5(3) . . . . ?
C2 C1 C40 C41 -0.7(5) . . . . ?
N1 C1 C40 C42 -60.1(4) . . . . ?
C2 C1 C40 C42 117.7(4) . . . . ?
N9 C43 C44 C45 0.8(7) . . . . ?
C43 C44 C45 C46 -0.8(8) . . . . ?
C44 C45 C46 C47 0.3(8) . . . . ?
C45 C46 C47 N9 0.2(6) . . . . ?
N10 C48 C49 C50 0.0(7) . . . . ?
C48 C49 C50 C51 1.5(7) . . . . ?
C49 C50 C51 C52 -1.6(7) . . . . ?
C50 C51 C52 N10 0.2(7) . . . . ?
N11 C53 C54 C55 -1.2(6) . . . . ?
C53 C54 C55 C56 -0.5(6) . . . . ?
C54 C55 C56 C57 1.5(7) . . . . ?
C55 C56 C57 N11 -0.9(7) . . . . ?
N12 C58 C59 C60 -0.7(7) . . . . ?
C58 C59 C60 C61 0.5(7) . . . . ?
C59 C60 C61 C62 0.1(7) . . . . ?
C60 C61 C62 N12 -0.7(8) . . . . ?
C2 C1 N1 C4 -1.1(4) . . . . ?
C40 C1 N1 C4 177.1(3) . . . . ?
C2 C1 N1 U1 153.6(3) . . . . ?
C40 C1 N1 U1 -28.3(5) . . . . ?
C3 C4 N1 C1 0.9(4) . . . . ?
C5 C4 N1 C1 -176.4(3) . . . . ?
C3 C4 N1 U1 -159.7(3) . . . . ?
C5 C4 N1 U1 22.9(4) . . . . ?
C4 C5 N2 C6 -179.0(3) . . . . ?
C4 C5 N2 U1 -16.7(4) . . . . ?
C13 C6 N2 C5 -136.8(4) . . . . ?
C7 C6 N2 C5 43.8(5) . . . . ?
C13 C6 N2 U1 63.4(4) . . . . ?
C7 C6 N2 U1 -116.0(3) . . . . ?
C15 C14 N3 C13 178.5(3) . . . . ?
C6 C13 N3 C14 146.1(3) . . . . ?
C12 C13 N3 C14 -33.6(5) . . . . ?
C17 C18 N4 C15 -0.4(4) . . . . ?
C19 C18 N4 C15 176.7(3) . . . . ?
C16 C15 N4 C18 0.8(4) . . . . ?
C14 C15 N4 C18 179.3(3) . . . . ?
C23 C22 N5 C25 0.0(4) . . . . ?
C19 C22 N5 C25 -177.1(3) . . . . ?
C24 C25 N5 C22 -0.1(4) . . . . ?
C26 C25 N5 C22 -178.8(3) . . . . ?
C25 C26 N6 C27 -179.2(3) . . . . ?
C28 C27 N6 C26 38.9(5) . . . . ?
C34 C27 N6 C26 -142.7(3) . . . . ?
C36 C35 N7 C34 179.9(3) . . . . ?
C36 C35 N7 U1 14.9(4) . . . . ?
C33 C34 N7 C35 -53.5(5) . . . . ?
C27 C34 N7 C35 126.4(3) . . . . ?
C33 C34 N7 U1 109.4(3) . . . . ?
C27 C34 N7 U1 -70.8(4) . . . . ?
C38 C39 N8 C36 -0.1(4) . . . . ?
C40 C39 N8 C36 -178.6(3) . . . . ?
C38 C39 N8 U1 -167.2(2) . . . . ?
C40 C39 N8 U1 14.2(5) . . . . ?
C37 C36 N8 C39 0.1(4) . . . . ?
C35 C36 N8 C39 175.5(3) . . . . ?
C37 C36 N8 U1 170.3(2) . . . . ?
C35 C36 N8 U1 -14.3(4) . . . . ?
C46 C47 N9 C43 -0.2(5) . . . . ?
C46 C47 N9 U1 -173.1(3) . . . . ?
C44 C43 N9 C47 -0.4(6) . . . . ?
C44 C43 N9 U1 172.7(4) . . . . ?
C51 C52 N10 C48 1.3(6) . . . . ?
C51 C52 N10 Zn1 -178.5(3) . . . . ?
C49 C48 N10 C52 -1.4(6) . . . . ?
C49 C48 N10 Zn1 178.4(3) . . . . ?
C56 C57 N11 C53 -0.7(6) . . . . ?
C56 C57 N11 Zn1 172.9(3) . . . . ?
C54 C53 N11 C57 1.8(6) . . . . ?
C54 C53 N11 Zn1 -172.1(3) . . . . ?
C59 C58 N12 C62 0.1(7) . . . . ?
C61 C62 N12 C58 0.6(8) . . . . ?
U1 O2 Zn1 N11 -12.1(17) . . . . ?
U1 O2 Zn1 N10 -116.4(16) . . . . ?
U1 O2 Zn1 I1 118.0(16) . . . . ?
C57 N11 Zn1 O2 159.3(3) . . . . ?
C53 N11 Zn1 O2 -27.1(3) . . . . ?
C57 N11 Zn1 N10 -91.3(3) . . . . ?
C53 N11 Zn1 N10 82.3(3) . . . . ?
C57 N11 Zn1 I1 27.7(3) . . . . ?
C53 N11 Zn1 I1 -158.7(2) . . . . ?
C52 N10 Zn1 O2 -116.0(3) . . . . ?
C48 N10 Zn1 O2 64.2(3) . . . . ?
C52 N10 Zn1 N11 139.1(3) . . . . ?
C48 N10 Zn1 N11 -40.7(3) . . . . ?
C52 N10 Zn1 I1 15.1(3) . . . . ?
C48 N10 Zn1 I1 -164.7(3) . . . . ?
Zn1 O2 U1 O1 -144.9(15) . . . . ?
Zn1 O2 U1 N1 69.2(16) . . . . ?
Zn1 O2 U1 N8 -0.9(16) . . . . ?
Zn1 O2 U1 N9 -143.9(16) . . . . ?
Zn1 O2 U1 N7 -65.7(16) . . . . ?
Zn1 O2 U1 N2 134.1(16) . . . . ?
C1 N1 U1 O1 86.3(3) . . . . ?
C4 N1 U1 O1 -120.7(2) . . . . ?
C1 N1 U1 O2 -96.1(3) . . . . ?
C4 N1 U1 O2 56.9(2) . . . . ?
C1 N1 U1 N8 -5.3(3) . . . . ?
C4 N1 U1 N8 147.7(3) . . . . ?
C1 N1 U1 N9 -178.0(3) . . . . ?
C4 N1 U1 N9 -25.0(3) . . . . ?
C1 N1 U1 N7 -20.4(4) . . . . ?
C4 N1 U1 N7 132.6(2) . . . . ?
C1 N1 U1 N2 -174.0(3) . . . . ?
C4 N1 U1 N2 -21.0(2) . . . . ?
C39 N8 U1 O1 -80.8(3) . . . . ?
C36 N8 U1 O1 113.0(2) . . . . ?
C39 N8 U1 O2 101.7(3) . . . . ?
C36 N8 U1 O2 -64.5(2) . . . . ?
C39 N8 U1 N1 12.7(3) . . . . ?
C36 N8 U1 N1 -153.4(3) . . . . ?
C39 N8 U1 N9 -173.9(3) . . . . ?
C36 N8 U1 N9 19.9(3) . . . . ?
C39 N8 U1 N7 -179.1(3) . . . . ?
C36 N8 U1 N7 14.7(2) . . . . ?
C39 N8 U1 N2 27.1(4) . . . . ?
C36 N8 U1 N2 -139.1(2) . . . . ?
C47 N9 U1 O1 -0.1(3) . . . . ?
C43 N9 U1 O1 -172.9(3) . . . . ?
C47 N9 U1 O2 179.9(3) . . . . ?
C43 N9 U1 O2 7.2(3) . . . . ?
C47 N9 U1 N1 -97.3(3) . . . . ?
C43 N9 U1 N1 89.9(3) . . . . ?
C47 N9 U1 N8 94.2(3) . . . . ?
C43 N9 U1 N8 -78.6(3) . . . . ?
C47 N9 U1 N7 99.0(3) . . . . ?
C43 N9 U1 N7 -73.8(3) . . . . ?
C47 N9 U1 N2 -101.0(3) . . . . ?
C43 N9 U1 N2 86.3(3) . . . . ?
C35 N7 U1 O1 -104.6(3) . . . . ?
C34 N7 U1 O1 92.2(3) . . . . ?
C35 N7 U1 O2 79.7(3) . . . . ?
C34 N7 U1 O2 -83.6(3) . . . . ?
C35 N7 U1 N1 0.3(3) . . . . ?
C34 N7 U1 N1 -163.0(2) . . . . ?
C35 N7 U1 N8 -15.3(2) . . . . ?
C34 N7 U1 N8 -178.6(3) . . . . ?
C35 N7 U1 N9 167.9(3) . . . . ?
C34 N7 U1 N9 4.6(3) . . . . ?
C35 N7 U1 N2 123.3(3) . . . . ?
C34 N7 U1 N2 -39.9(4) . . . . ?
C5 N2 U1 O1 109.5(3) . . . . ?
C6 N2 U1 O1 -89.6(3) . . . . ?
C5 N2 U1 O2 -74.8(3) . . . . ?
C6 N2 U1 O2 86.1(3) . . . . ?
C5 N2 U1 N1 19.6(2) . . . . ?
C6 N2 U1 N1 -179.5(3) . . . . ?
C5 N2 U1 N8 4.7(3) . . . . ?
C6 N2 U1 N8 165.6(2) . . . . ?
C5 N2 U1 N9 -162.6(3) . . . . ?
C6 N2 U1 N9 -1.8(3) . . . . ?
C5 N2 U1 N7 -118.7(3) . . . . ?
C6 N2 U1 N7 42.2(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        76.49
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.459
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.071
####################################################################### 
# 
# 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_po4036_refinalized
_database_code_depnum_ccdc_archive 'CCDC 1883758'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;university of edinburgh
United Kingdom
;
_audit_update_record             
;
2018-12-07 deposited with the CCDC.	2019-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C87 H87 Cl N9 O2 Ti U'
_chemical_formula_weight         1612.04

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'

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

_cell_length_a                   20.517(5)
_cell_length_b                   21.431(5)
_cell_length_c                   19.018(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 117.115(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     7443(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    43218
_cell_measurement_theta_min      3.1010
_cell_measurement_theta_max      28.5880

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.2064
_exptl_crystal_size_mid          0.1031
_exptl_crystal_size_min          0.0712
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3276
_exptl_absorpt_coefficient_mu    2.372
_exptl_absorpt_correction_T_min  0.916
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            156288
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         28.91
_reflns_number_total             18357
_reflns_number_gt                15202
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    MERCURY
_computing_publication_material  ORTEP

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0372P)²+17.9554P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         18357
_refine_ls_number_parameters     910
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.0800
_refine_ls_wR_factor_gt          0.0740
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_restrained_S_all      0.918
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.55424(15) 0.18370(14) 0.09902(17) 0.0194(6) Uani 1 1 d . . .
C2 C 0.49339(16) 0.17779(15) 0.02428(18) 0.0221(6) Uani 1 1 d . . .
H2 H 0.4547 0.2070 -0.0002 0.027 Uiso 1 1 calc R . .
C3 C 0.50048(17) 0.12113(15) -0.00708(18) 0.0221(6) Uani 1 1 d . . .
H3 H 0.4677 0.1041 -0.0569 0.026 Uiso 1 1 calc R . .
C4 C 0.56556(16) 0.09421(14) 0.04932(17) 0.0185(6) Uani 1 1 d . . .
C5 C 0.59526(16) 0.03484(14) 0.04851(17) 0.0183(6) Uani 1 1 d . . .
H5A H 0.5703 0.0087 0.0038 0.022 Uiso 1 1 calc R . .
C6 C 0.67569(15) -0.04811(14) 0.09932(17) 0.0180(6) Uani 1 1 d . . .
C7 C 0.67750(16) -0.06905(14) 0.03077(18) 0.0206(6) Uani 1 1 d . . .
H7 H 0.6684 -0.0401 -0.0105 0.025 Uiso 1 1 calc R . .
C8 C 0.69213(17) -0.13061(16) 0.02066(18) 0.0238(7) Uani 1 1 d . . .
C9 C 0.6909(2) -0.15119(18) -0.0561(2) 0.0352(8) Uani 1 1 d . . .
H9A H 0.7023 -0.1958 -0.0533 0.053 Uiso 1 1 calc R . .
H9B H 0.7273 -0.1274 -0.0649 0.053 Uiso 1 1 calc R . .
H9C H 0.6421 -0.1437 -0.0999 0.053 Uiso 1 1 calc R . .
C10 C 0.7189(2) -0.24188(16) 0.0714(2) 0.0336(8) Uani 1 1 d . . .
H10A H 0.7179 -0.2482 0.0199 0.050 Uiso 1 1 calc R . .
H10B H 0.6805 -0.2672 0.0746 0.050 Uiso 1 1 calc R . .
H10C H 0.7668 -0.2544 0.1135 0.050 Uiso 1 1 calc R . .
C11 C 0.70560(17) -0.17385(15) 0.08118(19) 0.0240(7) Uani 1 1 d . . .
C12 C 0.70461(16) -0.15316(15) 0.14969(18) 0.0227(6) Uani 1 1 d . . .
H12 H 0.7154 -0.1820 0.1914 0.027 Uiso 1 1 calc R . .
C13 C 0.68834(16) -0.09132(14) 0.15990(17) 0.0194(6) Uani 1 1 d . . .
C14 C 0.66725(17) -0.10755(15) 0.26925(19) 0.0245(7) Uani 1 1 d . . .
H14 H 0.6622 -0.1507 0.2564 0.029 Uiso 1 1 calc R . .
C15 C 0.65919(18) -0.08718(16) 0.33628(19) 0.0252(7) Uani 1 1 d . . .
C16 C 0.6469(2) -0.12097(17) 0.3912(2) 0.0336(8) Uani 1 1 d . . .
H16 H 0.6434 -0.1651 0.3931 0.040 Uiso 1 1 calc R . .
C17 C 0.6406(2) -0.07824(18) 0.4435(2) 0.0348(8) Uani 1 1 d . . .
H17 H 0.6321 -0.0883 0.4873 0.042 Uiso 1 1 calc R . .
C18 C 0.64886(18) -0.01878(17) 0.42011(18) 0.0269(7) Uani 1 1 d . . .
C19 C 0.65086(19) 0.04459(17) 0.45697(19) 0.0286(7) Uani 1 1 d . . .
C20 C 0.6156(2) 0.0394(2) 0.5131(2) 0.0422(10) Uani 1 1 d . . .
H20A H 0.6168 0.0802 0.5369 0.063 Uiso 1 1 calc R . .
H20B H 0.6429 0.0090 0.5548 0.063 Uiso 1 1 calc R . .
H20C H 0.5647 0.0255 0.4832 0.063 Uiso 1 1 calc R . .
C21 C 0.6087(2) 0.09358(18) 0.3930(2) 0.0329(8) Uani 1 1 d . . .
H21A H 0.6107 0.1339 0.4181 0.049 Uiso 1 1 calc R . .
H21B H 0.5576 0.0805 0.3628 0.049 Uiso 1 1 calc R . .
H21C H 0.6311 0.0975 0.3574 0.049 Uiso 1 1 calc R . .
C22 C 0.73012(18) 0.06377(15) 0.50306(18) 0.0258(7) Uani 1 1 d . . .
C23 C 0.7727(2) 0.07531(17) 0.58274(19) 0.0318(8) Uani 1 1 d . . .
H23 H 0.7570 0.0729 0.6226 0.038 Uiso 1 1 calc R . .
C24 C 0.8431(2) 0.09122(17) 0.59410(19) 0.0335(8) Uani 1 1 d . . .
H24 H 0.8837 0.1016 0.6430 0.040 Uiso 1 1 calc R . .
C25 C 0.84294(18) 0.08911(15) 0.52133(18) 0.0244(7) Uani 1 1 d . . .
C26 C 0.89804(18) 0.10145(15) 0.49715(19) 0.0258(7) Uani 1 1 d . . .
H26 H 0.9450 0.1155 0.5348 0.031 Uiso 1 1 calc R . .
C27 C 0.94022(17) 0.10758(15) 0.40348(19) 0.0240(7) Uani 1 1 d . . .
C28 C 1.01182(18) 0.08476(16) 0.4444(2) 0.0282(7) Uani 1 1 d . . .
H28 H 1.0233 0.0571 0.4875 0.034 Uiso 1 1 calc R . .
C29 C 1.06631(18) 0.10107(16) 0.4243(2) 0.0309(8) Uani 1 1 d . . .
C30 C 1.14320(19) 0.07639(19) 0.4723(2) 0.0417(9) Uani 1 1 d . . .
H30A H 1.1749 0.0921 0.4503 0.062 Uiso 1 1 calc R . .
H30B H 1.1425 0.0307 0.4706 0.062 Uiso 1 1 calc R . .
H30C H 1.1621 0.0904 0.5272 0.062 Uiso 1 1 calc R . .
C31 C 1.1072(2) 0.1641(2) 0.3387(3) 0.0450(10) Uani 1 1 d . . .
H31A H 1.0849 0.1913 0.2922 0.067 Uiso 1 1 calc R . .
H31B H 1.1305 0.1285 0.3269 0.067 Uiso 1 1 calc R . .
H31C H 1.1441 0.1876 0.3832 0.067 Uiso 1 1 calc R . .
C32 C 1.04879(18) 0.14090(16) 0.3597(2) 0.0299(8) Uani 1 1 d . . .
C33 C 0.97675(18) 0.16193(16) 0.3169(2) 0.0273(7) Uani 1 1 d . . .
H33 H 0.9647 0.1882 0.2724 0.033 Uiso 1 1 calc R . .
C34 C 0.92225(16) 0.14545(14) 0.33751(18) 0.0228(6) Uani 1 1 d . . .
C35 C 0.83934(17) 0.22740(15) 0.28957(17) 0.0216(6) Uani 1 1 d . . .
H35 H 0.8813 0.2536 0.3123 0.026 Uiso 1 1 calc R . .
C36 C 0.76877(16) 0.25558(14) 0.25120(17) 0.0195(6) Uani 1 1 d . . .
C37 C 0.75000(17) 0.31848(15) 0.24169(18) 0.0233(6) Uani 1 1 d . . .
H37 H 0.7826 0.3530 0.2582 0.028 Uiso 1 1 calc R . .
C38 C 0.67359(18) 0.32066(15) 0.20296(18) 0.0236(6) Uani 1 1 d . . .
H38 H 0.6440 0.3571 0.1874 0.028 Uiso 1 1 calc R . .
C39 C 0.64882(16) 0.25863(14) 0.19136(17) 0.0195(6) Uani 1 1 d . . .
C40 C 0.57033(17) 0.23529(15) 0.15882(19) 0.0241(7) Uani 1 1 d . . .
C41 C 0.51667(19) 0.28942(18) 0.1213(2) 0.0394(9) Uani 1 1 d . . .
H41A H 0.5273 0.3227 0.1604 0.059 Uiso 1 1 calc R . .
H41B H 0.4664 0.2745 0.1036 0.059 Uiso 1 1 calc R . .
H41C H 0.5220 0.3056 0.0760 0.059 Uiso 1 1 calc R . .
C42 C 0.55991(19) 0.20913(18) 0.2292(2) 0.0328(8) Uani 1 1 d . . .
H42A H 0.5701 0.2421 0.2686 0.049 Uiso 1 1 calc R . .
H42B H 0.5937 0.1742 0.2533 0.049 Uiso 1 1 calc R . .
H42C H 0.5094 0.1946 0.2102 0.049 Uiso 1 1 calc R . .
C43 C 0.88559(18) 0.03147(18) 0.2302(2) 0.0320(8) Uani 1 1 d . . .
H43 H 0.8829 0.0637 0.1947 0.038 Uiso 1 1 calc R . .
C44 C 0.9456(2) -0.0080(2) 0.2591(2) 0.0485(11) Uani 1 1 d . . .
H44 H 0.9834 -0.0031 0.2438 0.058 Uiso 1 1 calc R . .
C45 C 0.9491(2) -0.0547(2) 0.3108(2) 0.0531(13) Uani 1 1 d . . .
H45 H 0.9891 -0.0831 0.3307 0.064 Uiso 1 1 calc R . .
C46 C 0.8947(2) -0.05989(18) 0.3332(2) 0.0425(10) Uani 1 1 d . . .
H46 H 0.8966 -0.0914 0.3693 0.051 Uiso 1 1 calc R . .
C47 C 0.83688(19) -0.01830(16) 0.3023(2) 0.0319(8) Uani 1 1 d . . .
H47 H 0.7997 -0.0213 0.3187 0.038 Uiso 1 1 calc R . .
C48 C 0.8487(2) 0.08086(18) 0.0315(2) 0.0359(8) Uani 1 1 d . . .
H48 H 0.8966 0.0773 0.0741 0.043 Uiso 1 1 calc R . .
C49 C 0.78608(19) 0.05157(15) 0.02622(19) 0.0273(7) Uani 1 1 d . . .
H49 H 0.7836 0.0241 0.0641 0.033 Uiso 1 1 calc R . .
C50 C 0.7268(2) 0.07033(15) -0.04593(19) 0.0297(7) Uani 1 1 d . . .
H50 H 0.6770 0.0588 -0.0641 0.036 Uiso 1 1 calc R . .
C51 C 0.7542(2) 0.10895(17) -0.0859(2) 0.0365(9) Uani 1 1 d . . .
H51 H 0.7266 0.1265 -0.1369 0.044 Uiso 1 1 calc R . .
C52 C 0.8287(2) 0.11696(18) -0.0377(3) 0.0412(10) Uani 1 1 d . . .
H52 H 0.8607 0.1422 -0.0491 0.049 Uiso 1 1 calc R . .
C53 C 0.65559(19) 0.20091(16) -0.07310(19) 0.0297(7) Uani 1 1 d . . .
H53 H 0.6245 0.1731 -0.1132 0.036 Uiso 1 1 calc R . .
C54 C 0.65347(19) 0.21367(16) -0.0014(2) 0.0296(8) Uani 1 1 d . . .
H54 H 0.6200 0.1962 0.0150 0.036 Uiso 1 1 calc R . .
C55 C 0.7091(2) 0.25636(16) 0.0415(2) 0.0314(8) Uani 1 1 d . . .
H55 H 0.7208 0.2722 0.0925 0.038 Uiso 1 1 calc R . .
C56 C 0.7446(2) 0.27159(16) -0.0044(2) 0.0327(8) Uani 1 1 d . . .
H56 H 0.7837 0.3004 0.0098 0.039 Uiso 1 1 calc R . .
C57 C 0.7128(2) 0.23737(16) -0.0742(2) 0.0287(7) Uani 1 1 d . . .
H57 H 0.7269 0.2383 -0.1153 0.034 Uiso 1 1 calc R . .
C58 C 0.5224(2) -0.04618(18) 0.8205(2) 0.0379(9) Uani 1 1 d . . .
H58 H 0.5101 -0.0820 0.8414 0.045 Uiso 1 1 calc R . .
C59 C 0.49786(19) 0.01137(18) 0.8292(2) 0.0328(8) Uani 1 1 d . . .
H59 H 0.4676 0.0150 0.8548 0.039 Uiso 1 1 calc R . .
C60 C 0.5168(2) 0.06363(19) 0.8013(3) 0.0435(10) Uani 1 1 d . . .
H60 H 0.5002 0.1035 0.8079 0.052 Uiso 1 1 calc R . .
C61 C 0.5594(2) 0.0580(2) 0.7639(3) 0.0562(13) Uani 1 1 d . . .
H61 H 0.5732 0.0944 0.7454 0.067 Uiso 1 1 calc R . .
C62 C 0.5827(2) 0.0004(3) 0.7525(3) 0.0545(12) Uani 1 1 d . . .
H62 H 0.6111 -0.0029 0.7248 0.065 Uiso 1 1 calc R . .
C63 C 0.5647(2) -0.0526(2) 0.7816(2) 0.0438(10) Uani 1 1 d . . .
H63 H 0.5812 -0.0926 0.7749 0.053 Uiso 1 1 calc R . .
C64 C 0.0488(3) 0.2367(2) 0.6189(3) 0.0552(12) Uani 1 1 d . . .
H64 H 0.0215 0.2351 0.6480 0.066 Uiso 1 1 calc R . .
C65 C 0.0144(2) 0.25115(19) 0.5406(3) 0.0448(10) Uani 1 1 d . . .
H65 H -0.0369 0.2585 0.5151 0.054 Uiso 1 1 calc R . .
C66 C 0.0530(3) 0.2552(2) 0.4987(2) 0.0498(11) Uani 1 1 d . . .
H66 H 0.0294 0.2662 0.4443 0.060 Uiso 1 1 calc R . .
C67 C 0.1274(3) 0.2429(2) 0.5364(3) 0.0612(14) Uani 1 1 d . . .
H67 H 0.1549 0.2447 0.5076 0.073 Uiso 1 1 calc R . .
C68 C 0.1615(3) 0.2283(3) 0.6151(3) 0.0655(14) Uani 1 1 d . . .
H68 H 0.2127 0.2207 0.6414 0.079 Uiso 1 1 calc R . .
C69 C 0.1211(3) 0.2247(3) 0.6555(3) 0.0620(13) Uani 1 1 d . . .
H69 H 0.1443 0.2137 0.7098 0.074 Uiso 1 1 calc R . .
C70 C 0.5803(3) 0.6462(2) 0.1037(3) 0.0498(11) Uani 1 1 d . . .
H70 H 0.5591 0.6232 0.0557 0.060 Uiso 1 1 calc R . .
C71 C 0.6497(3) 0.6322(2) 0.1603(3) 0.0549(12) Uani 1 1 d . . .
H71 H 0.6767 0.5998 0.1514 0.066 Uiso 1 1 calc R . .
C72 C 0.6804(3) 0.6653(2) 0.2305(3) 0.0607(14) Uani 1 1 d . . .
H72 H 0.7285 0.6561 0.2700 0.073 Uiso 1 1 calc R . .
C73 C 0.6401(4) 0.7118(2) 0.2420(3) 0.0639(15) Uani 1 1 d . . .
H73 H 0.6604 0.7342 0.2904 0.077 Uiso 1 1 calc R . .
C74 C 0.5714(3) 0.7261(2) 0.1851(3) 0.0602(14) Uani 1 1 d . . .
H74 H 0.5444 0.7588 0.1932 0.072 Uiso 1 1 calc R . .
C75 C 0.5418(3) 0.6926(2) 0.1159(3) 0.0526(11) Uani 1 1 d . . .
H75 H 0.4939 0.7021 0.0762 0.063 Uiso 1 1 calc R . .
C76 C 0.9880(5) 0.8325(2) 0.2028(3) 0.078(2) Uani 1 1 d . . .
H76 H 1.0024 0.8008 0.2420 0.094 Uiso 1 1 calc R . .
C77 C 0.9141(4) 0.8470(3) 0.1569(4) 0.0717(17) Uani 1 1 d . . .
H77 H 0.8772 0.8255 0.1644 0.086 Uiso 1 1 calc R . .
C78 C 0.8960(3) 0.8928(3) 0.1010(3) 0.0661(16) Uani 1 1 d . . .
H78 H 0.8461 0.9038 0.0696 0.079 Uiso 1 1 calc R . .
C79 C 0.9482(4) 0.9217(3) 0.0906(3) 0.0717(16) Uani 1 1 d . . .
H79 H 0.9349 0.9532 0.0513 0.086 Uiso 1 1 calc R . .
C80 C 1.0185(4) 0.9079(3) 0.1339(4) 0.080(2) Uani 1 1 d . . .
H80 H 1.0546 0.9289 0.1244 0.096 Uiso 1 1 calc R . .
C81 C 1.0390(3) 0.8647(4) 0.1903(4) 0.083(2) Uani 1 1 d . . .
H81 H 1.0896 0.8562 0.2220 0.100 Uiso 1 1 calc R . .
C82 C 0.9062(3) 0.9323(3) 0.8132(3) 0.0730(16) Uani 1 1 d . . .
H82 H 0.9468 0.9193 0.8055 0.088 Uiso 1 1 calc R . .
C83 C 0.8956(4) 0.9097(3) 0.8769(3) 0.082(2) Uani 1 1 d . . .
H83 H 0.9296 0.8811 0.9134 0.099 Uiso 1 1 calc R . .
C84 C 0.8367(4) 0.9289(4) 0.8858(3) 0.093(2) Uani 1 1 d . . .
H84 H 0.8295 0.9130 0.9284 0.111 Uiso 1 1 calc R . .
C85 C 0.7883(4) 0.9699(3) 0.8356(3) 0.0749(16) Uani 1 1 d . . .
H85 H 0.7477 0.9828 0.8431 0.090 Uiso 1 1 calc R . .
C86 C 0.7973(3) 0.9926(2) 0.7748(3) 0.0649(14) Uani 1 1 d . . .
H86 H 0.7629 1.0218 0.7400 0.078 Uiso 1 1 calc R . .
C87 C 0.8548(3) 0.9746(3) 0.7622(3) 0.0658(14) Uani 1 1 d . . .
H87 H 0.8598 0.9909 0.7184 0.079 Uiso 1 1 calc R . .
N1 N 0.59849(13) 0.13297(12) 0.11476(14) 0.0177(5) Uani 1 1 d . . .
N2 N 0.65596(13) 0.01441(11) 0.10706(14) 0.0173(5) Uani 1 1 d . . .
N3 N 0.68110(13) -0.06944(12) 0.22595(14) 0.0199(5) Uani 1 1 d . . .
N4 N 0.66039(14) -0.02524(13) 0.35497(15) 0.0229(6) Uani 1 1 d . . .
H4 H 0.6675 0.0058 0.3289 0.027 Uiso 1 1 calc R . .
N5 N 0.77341(14) 0.07280(12) 0.46686(15) 0.0227(6) Uani 1 1 d . . .
H5 H 0.7588 0.0688 0.4158 0.027 Uiso 1 1 calc R . .
N6 N 0.88474(14) 0.09375(12) 0.42536(16) 0.0245(6) Uani 1 1 d . . .
N7 N 0.84858(13) 0.16766(12) 0.29464(14) 0.0207(5) Uani 1 1 d . . .
N8 N 0.70639(13) 0.21880(12) 0.22039(14) 0.0195(5) Uani 1 1 d . . .
N9 N 0.83103(14) 0.02602(12) 0.25025(15) 0.0238(6) Uani 1 1 d . . .
O1 O 0.70753(11) 0.08136(10) 0.28461(11) 0.0205(4) Uani 1 1 d . . .
O2 O 0.74904(11) 0.13134(10) 0.11643(12) 0.0189(4) Uani 1 1 d . . .
Cl1 Cl 0.88043(5) 0.20804(5) 0.11314(5) 0.0378(2) Uani 1 1 d . . .
Ti1 Ti 0.76616(3) 0.16293(3) 0.02997(3) 0.02011(11) Uani 1 1 d . . .
U1 U 0.726865(5) 0.107310(5) 0.203717(6) 0.01481(4) Uani 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.360(4) . ?
C1 C2 1.406(4) . ?
C1 C40 1.511(4) . ?
C2 C3 1.389(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.400(4) . ?
C3 H3 0.9500 . ?
C4 N1 1.389(4) . ?
C4 C5 1.414(4) . ?
C5 N2 1.311(4) . ?
C5 H5A 0.9500 . ?
C6 C7 1.395(4) . ?
C6 C13 1.407(4) . ?
C6 N2 1.426(4) . ?
C7 C8 1.386(5) . ?
C7 H7 0.9500 . ?
C8 C11 1.403(5) . ?
C8 C9 1.514(4) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.510(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.385(4) . ?
C12 C13 1.402(4) . ?
C12 H12 0.9500 . ?
C13 N3 1.411(4) . ?
C14 N3 1.280(4) . ?
C14 C15 1.427(5) . ?
C14 H14 0.9500 . ?
C15 N4 1.372(4) . ?
C15 C16 1.386(5) . ?
C16 C17 1.400(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.385(5) . ?
C17 H17 0.9500 . ?
C18 N4 1.370(4) . ?
C18 C19 1.520(5) . ?
C19 C22 1.511(5) . ?
C19 C21 1.540(5) . ?
C19 C20 1.542(5) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 N5 1.363(4) . ?
C22 C23 1.383(4) . ?
C23 C24 1.402(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.383(5) . ?
C24 H24 0.9500 . ?
C25 N5 1.372(4) . ?
C25 C26 1.426(5) . ?
C26 N6 1.275(4) . ?
C26 H26 0.9500 . ?
C27 C34 1.395(5) . ?
C27 C28 1.400(4) . ?
C27 N6 1.410(4) . ?
C28 C29 1.381(5) . ?
C28 H28 0.9500 . ?
C29 C32 1.401(5) . ?
C29 C30 1.513(5) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.510(5) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.398(5) . ?
C33 C34 1.389(5) . ?
C33 H33 0.9500 . ?
C34 N7 1.433(4) . ?
C35 N7 1.292(4) . ?
C35 C36 1.425(4) . ?
C35 H35 0.9500 . ?
C36 N8 1.385(4) . ?
C36 C37 1.391(4) . ?
C37 C38 1.397(4) . ?
C37 H37 0.9500 . ?
C38 C39 1.404(4) . ?
C38 H38 0.9500 . ?
C39 N8 1.354(4) . ?
C39 C40 1.523(4) . ?
C40 C41 1.533(5) . ?
C40 C42 1.554(5) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 N9 1.342(4) . ?
C43 C44 1.384(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.383(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.370(6) . ?
C45 H45 0.9500 . ?
C46 C47 1.382(5) . ?
C46 H46 0.9500 . ?
C47 N9 1.337(5) . ?
C47 H47 0.9500 . ?
C48 C49 1.392(5) . ?
C48 C52 1.416(6) . ?
C48 Ti1 2.433(4) . ?
C48 H48 0.9500 . ?
C49 C50 1.415(5) . ?
C49 Ti1 2.428(3) . ?
C49 H49 0.9500 . ?
C50 C51 1.403(5) . ?
C50 Ti1 2.369(3) . ?
C50 H50 0.9500 . ?
C51 C52 1.390(6) . ?
C51 Ti1 2.400(4) . ?
C51 H51 0.9500 . ?
C52 Ti1 2.404(4) . ?
C52 H52 0.9500 . ?
C53 C54 1.411(5) . ?
C53 C57 1.417(5) . ?
C53 Ti1 2.366(3) . ?
C53 H53 0.9500 . ?
C54 C55 1.398(5) . ?
C54 Ti1 2.372(3) . ?
C54 H54 0.9500 . ?
C55 C56 1.407(5) . ?
C55 Ti1 2.380(3) . ?
C55 H55 0.9500 . ?
C56 C57 1.391(5) . ?
C56 Ti1 2.405(3) . ?
C56 H56 0.9500 . ?
C57 Ti1 2.385(3) . ?
C57 H57 0.9500 . ?
C58 C59 1.371(5) . ?
C58 C63 1.380(6) . ?
C58 H58 0.9500 . ?
C59 C60 1.369(5) . ?
C59 H59 0.9500 . ?
C60 C61 1.360(6) . ?
C60 H60 0.9500 . ?
C61 C62 1.377(7) . ?
C61 H61 0.9500 . ?
C62 C63 1.386(6) . ?
C62 H62 0.9500 . ?
C63 H63 0.9500 . ?
C64 C69 1.347(7) . ?
C64 C65 1.362(6) . ?
C64 H64 0.9500 . ?
C65 C66 1.359(6) . ?
C65 H65 0.9500 . ?
C66 C67 1.382(7) . ?
C66 H66 0.9500 . ?
C67 C68 1.370(7) . ?
C67 H67 0.9500 . ?
C68 C69 1.363(7) . ?
C68 H68 0.9500 . ?
C69 H69 0.9500 . ?
C70 C75 1.354(7) . ?
C70 C71 1.370(7) . ?
C70 H70 0.9500 . ?
C71 C72 1.384(7) . ?
C71 H71 0.9500 . ?
C72 C73 1.374(8) . ?
C72 H72 0.9500 . ?
C73 C74 1.364(8) . ?
C73 H73 0.9500 . ?
C74 C75 1.373(7) . ?
C74 H74 0.9500 . ?
C75 H75 0.9500 . ?
C76 C81 1.362(9) . ?
C76 C77 1.398(9) . ?
C76 H76 0.9500 . ?
C77 C78 1.368(8) . ?
C77 H77 0.9500 . ?
C78 C79 1.329(8) . ?
C78 H78 0.9500 . ?
C79 C80 1.328(9) . ?
C79 H79 0.9500 . ?
C80 C81 1.332(10) . ?
C80 H80 0.9500 . ?
C81 H81 0.9500 . ?
C82 C87 1.394(8) . ?
C82 C83 1.410(9) . ?
C82 H82 0.9500 . ?
C83 C84 1.359(10) . ?
C83 H83 0.9500 . ?
C84 C85 1.343(9) . ?
C84 H84 0.9500 . ?
C85 C86 1.341(8) . ?
C85 H85 0.9500 . ?
C86 C87 1.363(8) . ?
C86 H86 0.9500 . ?
C87 H87 0.9500 . ?
N1 U1 2.458(2) . ?
N2 U1 2.650(2) . ?
N4 H4 0.8800 . ?
N5 H5 0.8800 . ?
N7 U1 2.639(2) . ?
N8 U1 2.471(3) . ?
N9 U1 2.581(3) . ?
O1 U1 1.841(2) . ?
O2 Ti1 1.952(2) . ?
O2 U1 1.979(2) . ?
Cl1 Ti1 2.3565(11) . ?

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
N1 C1 C2 110.3(3) . . ?
N1 C1 C40 121.6(3) . . ?
C2 C1 C40 128.0(3) . . ?
C3 C2 C1 107.1(3) . . ?
C3 C2 H2 126.4 . . ?
C1 C2 H2 126.4 . . ?
C2 C3 C4 106.3(3) . . ?
C2 C3 H3 126.8 . . ?
C4 C3 H3 126.8 . . ?
N1 C4 C3 110.2(3) . . ?
N1 C4 C5 120.8(3) . . ?
C3 C4 C5 128.9(3) . . ?
N2 C5 C4 122.6(3) . . ?
N2 C5 H5A 118.7 . . ?
C4 C5 H5A 118.7 . . ?
C7 C6 C13 118.7(3) . . ?
C7 C6 N2 121.9(3) . . ?
C13 C6 N2 119.3(3) . . ?
C8 C7 C6 122.4(3) . . ?
C8 C7 H7 118.8 . . ?
C6 C7 H7 118.8 . . ?
C7 C8 C11 119.3(3) . . ?
C7 C8 C9 120.1(3) . . ?
C11 C8 C9 120.6(3) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C8 118.6(3) . . ?
C12 C11 C10 120.3(3) . . ?
C8 C11 C10 121.1(3) . . ?
C11 C12 C13 122.6(3) . . ?
C11 C12 H12 118.7 . . ?
C13 C12 H12 118.7 . . ?
C12 C13 C6 118.4(3) . . ?
C12 C13 N3 124.5(3) . . ?
C6 C13 N3 117.1(3) . . ?
N3 C14 C15 122.0(3) . . ?
N3 C14 H14 119.0 . . ?
C15 C14 H14 119.0 . . ?
N4 C15 C16 107.4(3) . . ?
N4 C15 C14 122.1(3) . . ?
C16 C15 C14 130.5(3) . . ?
C15 C16 C17 107.5(3) . . ?
C15 C16 H16 126.2 . . ?
C17 C16 H16 126.2 . . ?
C18 C17 C16 108.0(3) . . ?
C18 C17 H17 126.0 . . ?
C16 C17 H17 126.0 . . ?
N4 C18 C17 107.1(3) . . ?
N4 C18 C19 121.9(3) . . ?
C17 C18 C19 130.9(3) . . ?
C22 C19 C18 107.8(3) . . ?
C22 C19 C21 110.0(3) . . ?
C18 C19 C21 110.9(3) . . ?
C22 C19 C20 109.8(3) . . ?
C18 C19 C20 109.4(3) . . ?
C21 C19 C20 108.9(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N5 C22 C23 107.3(3) . . ?
N5 C22 C19 121.5(3) . . ?
C23 C22 C19 131.2(3) . . ?
C22 C23 C24 107.7(3) . . ?
C22 C23 H23 126.2 . . ?
C24 C23 H23 126.2 . . ?
C25 C24 C23 107.8(3) . . ?
C25 C24 H24 126.1 . . ?
C23 C24 H24 126.1 . . ?
N5 C25 C24 106.9(3) . . ?
N5 C25 C26 120.5(3) . . ?
C24 C25 C26 132.5(3) . . ?
N6 C26 C25 120.5(3) . . ?
N6 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C34 C27 C28 118.9(3) . . ?
C34 C27 N6 118.0(3) . . ?
C28 C27 N6 123.1(3) . . ?
C29 C28 C27 122.3(3) . . ?
C29 C28 H28 118.9 . . ?
C27 C28 H28 118.9 . . ?
C28 C29 C32 118.7(3) . . ?
C28 C29 C30 119.8(3) . . ?
C32 C29 C30 121.5(3) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 C29 119.2(3) . . ?
C33 C32 C31 119.7(3) . . ?
C29 C32 C31 121.0(3) . . ?
C34 C33 C32 121.8(3) . . ?
C34 C33 H33 119.1 . . ?
C32 C33 H33 119.1 . . ?
C33 C34 C27 119.0(3) . . ?
C33 C34 N7 122.1(3) . . ?
C27 C34 N7 118.9(3) . . ?
N7 C35 C36 122.6(3) . . ?
N7 C35 H35 118.7 . . ?
C36 C35 H35 118.7 . . ?
N8 C36 C37 110.4(3) . . ?
N8 C36 C35 120.2(3) . . ?
C37 C36 C35 129.3(3) . . ?
C36 C37 C38 106.2(3) . . ?
C36 C37 H37 126.9 . . ?
C38 C37 H37 126.9 . . ?
C37 C38 C39 106.9(3) . . ?
C37 C38 H38 126.6 . . ?
C39 C38 H38 126.6 . . ?
N8 C39 C38 110.3(3) . . ?
N8 C39 C40 121.5(3) . . ?
C38 C39 C40 127.9(3) . . ?
C1 C40 C39 112.0(3) . . ?
C1 C40 C41 109.8(3) . . ?
C39 C40 C41 110.1(3) . . ?
C1 C40 C42 108.4(3) . . ?
C39 C40 C42 107.7(3) . . ?
C41 C40 C42 108.8(3) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N9 C43 C44 122.7(4) . . ?
N9 C43 H43 118.7 . . ?
C44 C43 H43 118.7 . . ?
C45 C44 C43 118.3(4) . . ?
C45 C44 H44 120.9 . . ?
C43 C44 H44 120.9 . . ?
C46 C45 C44 119.7(4) . . ?
C46 C45 H45 120.2 . . ?
C44 C45 H45 120.2 . . ?
C45 C46 C47 118.6(4) . . ?
C45 C46 H46 120.7 . . ?
C47 C46 H46 120.7 . . ?
N9 C47 C46 122.9(4) . . ?
N9 C47 H47 118.5 . . ?
C46 C47 H47 118.5 . . ?
C49 C48 C52 108.2(3) . . ?
C49 C48 Ti1 73.2(2) . . ?
C52 C48 Ti1 71.9(2) . . ?
C49 C48 H48 125.9 . . ?
C52 C48 H48 125.9 . . ?
Ti1 C48 H48 120.8 . . ?
C48 C49 C50 107.4(3) . . ?
C48 C49 Ti1 73.6(2) . . ?
C50 C49 Ti1 70.57(19) . . ?
C48 C49 H49 126.3 . . ?
C50 C49 H49 126.3 . . ?
Ti1 C49 H49 121.3 . . ?
C51 C50 C49 108.3(3) . . ?
C51 C50 Ti1 74.1(2) . . ?
C49 C50 Ti1 75.14(19) . . ?
C51 C50 H50 125.9 . . ?
C49 C50 H50 125.9 . . ?
Ti1 C50 H50 116.9 . . ?
C52 C51 C50 107.9(3) . . ?
C52 C51 Ti1 73.3(2) . . ?
C50 C51 Ti1 71.67(19) . . ?
C52 C51 H51 126.0 . . ?
C50 C51 H51 126.0 . . ?
Ti1 C51 H51 120.7 . . ?
C51 C52 C48 108.1(3) . . ?
C51 C52 Ti1 73.0(2) . . ?
C48 C52 Ti1 74.1(2) . . ?
C51 C52 H52 125.9 . . ?
C48 C52 H52 125.9 . . ?
Ti1 C52 H52 118.8 . . ?
C54 C53 C57 107.3(3) . . ?
C54 C53 Ti1 72.91(19) . . ?
C57 C53 Ti1 73.39(19) . . ?
C54 C53 H53 126.3 . . ?
C57 C53 H53 126.3 . . ?
Ti1 C53 H53 119.3 . . ?
C55 C54 C53 108.3(3) . . ?
C55 C54 Ti1 73.2(2) . . ?
C53 C54 Ti1 72.44(19) . . ?
C55 C54 H54 125.8 . . ?
C53 C54 H54 125.8 . . ?
Ti1 C54 H54 120.3 . . ?
C54 C55 C56 107.8(3) . . ?
C54 C55 Ti1 72.59(19) . . ?
C56 C55 Ti1 73.9(2) . . ?
C54 C55 H55 126.1 . . ?
C56 C55 H55 126.1 . . ?
Ti1 C55 H55 119.3 . . ?
C57 C56 C55 108.6(3) . . ?
C57 C56 Ti1 72.4(2) . . ?
C55 C56 Ti1 71.92(19) . . ?
C57 C56 H56 125.7 . . ?
C55 C56 H56 125.7 . . ?
Ti1 C56 H56 121.7 . . ?
C56 C57 C53 108.0(3) . . ?
C56 C57 Ti1 73.90(19) . . ?
C53 C57 Ti1 71.90(18) . . ?
C56 C57 H57 126.0 . . ?
C53 C57 H57 126.0 . . ?
Ti1 C57 H57 120.0 . . ?
C59 C58 C63 120.7(4) . . ?
C59 C58 H58 119.7 . . ?
C63 C58 H58 119.7 . . ?
C60 C59 C58 120.3(4) . . ?
C60 C59 H59 119.9 . . ?
C58 C59 H59 119.9 . . ?
C61 C60 C59 119.6(4) . . ?
C61 C60 H60 120.2 . . ?
C59 C60 H60 120.2 . . ?
C60 C61 C62 120.9(4) . . ?
C60 C61 H61 119.5 . . ?
C62 C61 H61 119.5 . . ?
C61 C62 C63 119.8(4) . . ?
C61 C62 H62 120.1 . . ?
C63 C62 H62 120.1 . . ?
C58 C63 C62 118.6(4) . . ?
C58 C63 H63 120.7 . . ?
C62 C63 H63 120.7 . . ?
C69 C64 C65 120.5(4) . . ?
C69 C64 H64 119.8 . . ?
C65 C64 H64 119.8 . . ?
C66 C65 C64 120.4(4) . . ?
C66 C65 H65 119.8 . . ?
C64 C65 H65 119.8 . . ?
C65 C66 C67 118.9(4) . . ?
C65 C66 H66 120.5 . . ?
C67 C66 H66 120.5 . . ?
C68 C67 C66 120.3(4) . . ?
C68 C67 H67 119.9 . . ?
C66 C67 H67 119.9 . . ?
C69 C68 C67 119.3(4) . . ?
C69 C68 H68 120.4 . . ?
C67 C68 H68 120.4 . . ?
C64 C69 C68 120.6(5) . . ?
C64 C69 H69 119.7 . . ?
C68 C69 H69 119.7 . . ?
C75 C70 C71 120.3(5) . . ?
C75 C70 H70 119.8 . . ?
C71 C70 H70 119.8 . . ?
C70 C71 C72 119.8(5) . . ?
C70 C71 H71 120.1 . . ?
C72 C71 H71 120.1 . . ?
C73 C72 C71 118.9(5) . . ?
C73 C72 H72 120.5 . . ?
C71 C72 H72 120.5 . . ?
C74 C73 C72 121.0(5) . . ?
C74 C73 H73 119.5 . . ?
C72 C73 H73 119.5 . . ?
C73 C74 C75 119.3(5) . . ?
C73 C74 H74 120.4 . . ?
C75 C74 H74 120.4 . . ?
C70 C75 C74 120.7(5) . . ?
C70 C75 H75 119.7 . . ?
C74 C75 H75 119.7 . . ?
C81 C76 C77 118.7(5) . . ?
C81 C76 H76 120.6 . . ?
C77 C76 H76 120.6 . . ?
C78 C77 C76 118.5(5) . . ?
C78 C77 H77 120.8 . . ?
C76 C77 H77 120.8 . . ?
C79 C78 C77 120.0(5) . . ?
C79 C78 H78 120.0 . . ?
C77 C78 H78 120.0 . . ?
C80 C79 C78 121.7(6) . . ?
C80 C79 H79 119.2 . . ?
C78 C79 H79 119.2 . . ?
C79 C80 C81 120.6(6) . . ?
C79 C80 H80 119.7 . . ?
C81 C80 H80 119.7 . . ?
C80 C81 C76 120.5(5) . . ?
C80 C81 H81 119.7 . . ?
C76 C81 H81 119.7 . . ?
C87 C82 C83 117.2(6) . . ?
C87 C82 H82 121.4 . . ?
C83 C82 H82 121.4 . . ?
C84 C83 C82 119.8(6) . . ?
C84 C83 H83 120.1 . . ?
C82 C83 H83 120.1 . . ?
C85 C84 C83 121.3(6) . . ?
C85 C84 H84 119.3 . . ?
C83 C84 H84 119.3 . . ?
C86 C85 C84 120.2(6) . . ?
C86 C85 H85 119.9 . . ?
C84 C85 H85 119.9 . . ?
C85 C86 C87 121.2(6) . . ?
C85 C86 H86 119.4 . . ?
C87 C86 H86 119.4 . . ?
C86 C87 C82 120.2(5) . . ?
C86 C87 H87 119.9 . . ?
C82 C87 H87 119.9 . . ?
C1 N1 C4 106.1(2) . . ?
C1 N1 U1 136.81(19) . . ?
C4 N1 U1 114.47(19) . . ?
C5 N2 C6 115.5(2) . . ?
C5 N2 U1 110.30(19) . . ?
C6 N2 U1 133.26(18) . . ?
C14 N3 C13 120.3(3) . . ?
C18 N4 C15 110.0(3) . . ?
C18 N4 H4 125.0 . . ?
C15 N4 H4 125.0 . . ?
C22 N5 C25 110.3(3) . . ?
C22 N5 H5 124.8 . . ?
C25 N5 H5 124.8 . . ?
C26 N6 C27 118.8(3) . . ?
C35 N7 C34 116.9(3) . . ?
C35 N7 U1 111.98(19) . . ?
C34 N7 U1 130.39(19) . . ?
C39 N8 C36 106.2(3) . . ?
C39 N8 U1 136.45(19) . . ?
C36 N8 U1 115.22(19) . . ?
C47 N9 C43 117.8(3) . . ?
C47 N9 U1 120.9(2) . . ?
C43 N9 U1 120.7(2) . . ?
Ti1 O2 U1 174.31(12) . . ?
O2 Ti1 Cl1 94.76(7) . . ?
O2 Ti1 C53 110.15(11) . . ?
Cl1 Ti1 C53 134.42(9) . . ?
O2 Ti1 C50 94.61(11) . . ?
Cl1 Ti1 C50 135.34(10) . . ?
C53 Ti1 C50 81.46(12) . . ?
O2 Ti1 C54 80.90(10) . . ?
Cl1 Ti1 C54 122.57(10) . . ?
C53 Ti1 C54 34.65(12) . . ?
C50 Ti1 C54 102.02(13) . . ?
O2 Ti1 C55 85.94(11) . . ?
Cl1 Ti1 C55 88.51(10) . . ?
C53 Ti1 C55 57.35(12) . . ?
C50 Ti1 C55 135.68(13) . . ?
C54 Ti1 C55 34.22(13) . . ?
O2 Ti1 C57 137.77(10) . . ?
Cl1 Ti1 C57 102.88(9) . . ?
C53 Ti1 C57 34.71(12) . . ?
C50 Ti1 C57 98.88(12) . . ?
C54 Ti1 C57 57.22(11) . . ?
C55 Ti1 C57 56.95(12) . . ?
O2 Ti1 C51 128.58(11) . . ?
Cl1 Ti1 C51 117.92(11) . . ?
C53 Ti1 C51 75.33(13) . . ?
C50 Ti1 C51 34.20(12) . . ?
C54 Ti1 C51 108.05(14) . . ?
C55 Ti1 C51 129.89(13) . . ?
C57 Ti1 C51 75.16(12) . . ?
O2 Ti1 C52 130.81(11) . . ?
Cl1 Ti1 C52 85.22(12) . . ?
C53 Ti1 C52 103.99(14) . . ?
C50 Ti1 C52 56.46(14) . . ?
C54 Ti1 C52 138.62(14) . . ?
C55 Ti1 C52 143.07(13) . . ?
C57 Ti1 C52 89.13(13) . . ?
C51 Ti1 C52 33.63(15) . . ?
O2 Ti1 C56 118.92(11) . . ?
Cl1 Ti1 C56 77.81(9) . . ?
C53 Ti1 C56 56.86(12) . . ?
C50 Ti1 C56 132.54(12) . . ?
C54 Ti1 C56 56.65(12) . . ?
C55 Ti1 C56 34.21(12) . . ?
C57 Ti1 C56 33.75(12) . . ?
C51 Ti1 C56 106.72(12) . . ?
C52 Ti1 C56 109.16(13) . . ?
O2 Ti1 C49 77.36(10) . . ?
Cl1 Ti1 C49 107.08(9) . . ?
C53 Ti1 C49 115.12(12) . . ?
C50 Ti1 C49 34.29(11) . . ?
C54 Ti1 C49 126.95(12) . . ?
C55 Ti1 C49 157.86(12) . . ?
C57 Ti1 C49 130.75(12) . . ?
C51 Ti1 C49 56.45(12) . . ?
C52 Ti1 C49 56.17(12) . . ?
C56 Ti1 C49 163.03(12) . . ?
O2 Ti1 C48 97.52(11) . . ?
Cl1 Ti1 C48 79.30(10) . . ?
C53 Ti1 C48 131.14(13) . . ?
C50 Ti1 C48 56.20(13) . . ?
C54 Ti1 C48 158.11(13) . . ?
C55 Ti1 C48 167.55(14) . . ?
C57 Ti1 C48 123.17(12) . . ?
C51 Ti1 C48 56.07(14) . . ?
C52 Ti1 C48 34.04(13) . . ?
C56 Ti1 C48 138.09(13) . . ?
C49 Ti1 C48 33.28(12) . . ?
O1 U1 O2 177.43(9) . . ?
O1 U1 N1 94.09(9) . . ?
O2 U1 N1 87.04(8) . . ?
O1 U1 N8 94.06(9) . . ?
O2 U1 N8 88.48(8) . . ?
N1 U1 N8 71.37(8) . . ?
O1 U1 N9 88.26(9) . . ?
O2 U1 N9 89.56(9) . . ?
N1 U1 N9 147.90(8) . . ?
N8 U1 N9 140.46(8) . . ?
O1 U1 N7 95.77(9) . . ?
O2 U1 N7 84.92(8) . . ?
N1 U1 N7 137.62(8) . . ?
N8 U1 N7 66.89(8) . . ?
N9 U1 N7 73.60(8) . . ?
O1 U1 N2 95.36(9) . . ?
O2 U1 N2 82.94(8) . . ?
N1 U1 N2 67.25(8) . . ?
N8 U1 N2 138.05(8) . . ?
N9 U1 N2 80.66(8) . . ?
N7 U1 N2 151.55(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
N1 C1 C2 C3 0.1(4) . . . . ?
C40 C1 C2 C3 -176.6(3) . . . . ?
C1 C2 C3 C4 -0.2(4) . . . . ?
C2 C3 C4 N1 0.2(3) . . . . ?
C2 C3 C4 C5 175.4(3) . . . . ?
N1 C4 C5 N2 -2.7(4) . . . . ?
C3 C4 C5 N2 -177.4(3) . . . . ?
C13 C6 C7 C8 -0.8(4) . . . . ?
N2 C6 C7 C8 -175.9(3) . . . . ?
C6 C7 C8 C11 0.1(5) . . . . ?
C6 C7 C8 C9 177.9(3) . . . . ?
C7 C8 C11 C12 -0.7(5) . . . . ?
C9 C8 C11 C12 -178.6(3) . . . . ?
C7 C8 C11 C10 177.6(3) . . . . ?
C9 C8 C11 C10 -0.2(5) . . . . ?
C8 C11 C12 C13 2.2(5) . . . . ?
C10 C11 C12 C13 -176.2(3) . . . . ?
C11 C12 C13 C6 -2.8(5) . . . . ?
C11 C12 C13 N3 174.8(3) . . . . ?
C7 C6 C13 C12 2.1(4) . . . . ?
N2 C6 C13 C12 177.3(3) . . . . ?
C7 C6 C13 N3 -175.7(3) . . . . ?
N2 C6 C13 N3 -0.5(4) . . . . ?
N3 C14 C15 N4 4.9(5) . . . . ?
N3 C14 C15 C16 -177.5(3) . . . . ?
N4 C15 C16 C17 0.1(4) . . . . ?
C14 C15 C16 C17 -177.8(3) . . . . ?
C15 C16 C17 C18 0.1(4) . . . . ?
C16 C17 C18 N4 -0.3(4) . . . . ?
C16 C17 C18 C19 -176.6(3) . . . . ?
N4 C18 C19 C22 -76.2(4) . . . . ?
C17 C18 C19 C22 99.7(4) . . . . ?
N4 C18 C19 C21 44.3(4) . . . . ?
C17 C18 C19 C21 -139.9(4) . . . . ?
N4 C18 C19 C20 164.5(3) . . . . ?
C17 C18 C19 C20 -19.7(5) . . . . ?
C18 C19 C22 N5 62.1(4) . . . . ?
C21 C19 C22 N5 -58.9(4) . . . . ?
C20 C19 C22 N5 -178.8(3) . . . . ?
C18 C19 C22 C23 -117.8(4) . . . . ?
C21 C19 C22 C23 121.1(4) . . . . ?
C20 C19 C22 C23 1.3(5) . . . . ?
N5 C22 C23 C24 -0.4(4) . . . . ?
C19 C22 C23 C24 179.6(3) . . . . ?
C22 C23 C24 C25 -0.1(4) . . . . ?
C23 C24 C25 N5 0.6(4) . . . . ?
C23 C24 C25 C26 179.0(3) . . . . ?
N5 C25 C26 N6 -4.4(5) . . . . ?
C24 C25 C26 N6 177.3(4) . . . . ?
C34 C27 C28 C29 3.5(5) . . . . ?
N6 C27 C28 C29 -177.0(3) . . . . ?
C27 C28 C29 C32 -1.2(5) . . . . ?
C27 C28 C29 C30 178.1(3) . . . . ?
C28 C29 C32 C33 -1.2(5) . . . . ?
C30 C29 C32 C33 179.4(3) . . . . ?
C28 C29 C32 C31 175.5(3) . . . . ?
C30 C29 C32 C31 -3.9(5) . . . . ?
C29 C32 C33 C34 1.4(5) . . . . ?
C31 C32 C33 C34 -175.3(3) . . . . ?
C32 C33 C34 C27 0.9(5) . . . . ?
C32 C33 C34 N7 179.0(3) . . . . ?
C28 C27 C34 C33 -3.3(5) . . . . ?
N6 C27 C34 C33 177.2(3) . . . . ?
C28 C27 C34 N7 178.6(3) . . . . ?
N6 C27 C34 N7 -0.9(4) . . . . ?
N7 C35 C36 N8 2.8(4) . . . . ?
N7 C35 C36 C37 179.3(3) . . . . ?
N8 C36 C37 C38 -0.7(3) . . . . ?
C35 C36 C37 C38 -177.4(3) . . . . ?
C36 C37 C38 C39 0.8(3) . . . . ?
C37 C38 C39 N8 -0.6(3) . . . . ?
C37 C38 C39 C40 173.8(3) . . . . ?
N1 C1 C40 C39 50.7(4) . . . . ?
C2 C1 C40 C39 -132.9(3) . . . . ?
N1 C1 C40 C41 173.3(3) . . . . ?
C2 C1 C40 C41 -10.3(5) . . . . ?
N1 C1 C40 C42 -67.9(4) . . . . ?
C2 C1 C40 C42 108.4(4) . . . . ?
N8 C39 C40 C1 -50.8(4) . . . . ?
C38 C39 C40 C1 135.4(3) . . . . ?
N8 C39 C40 C41 -173.3(3) . . . . ?
C38 C39 C40 C41 12.9(4) . . . . ?
N8 C39 C40 C42 68.3(4) . . . . ?
C38 C39 C40 C42 -105.5(4) . . . . ?
N9 C43 C44 C45 -0.1(6) . . . . ?
C43 C44 C45 C46 -1.4(6) . . . . ?
C44 C45 C46 C47 0.8(6) . . . . ?
C45 C46 C47 N9 1.4(5) . . . . ?
C52 C48 C49 C50 -0.9(4) . . . . ?
Ti1 C48 C49 C50 62.9(2) . . . . ?
C52 C48 C49 Ti1 -63.8(3) . . . . ?
C48 C49 C50 C51 2.5(4) . . . . ?
Ti1 C49 C50 C51 67.3(2) . . . . ?
C48 C49 C50 Ti1 -64.8(2) . . . . ?
C49 C50 C51 C52 -3.1(4) . . . . ?
Ti1 C50 C51 C52 64.9(3) . . . . ?
C49 C50 C51 Ti1 -68.0(2) . . . . ?
C50 C51 C52 C48 2.5(4) . . . . ?
Ti1 C51 C52 C48 66.3(3) . . . . ?
C50 C51 C52 Ti1 -63.8(2) . . . . ?
C49 C48 C52 C51 -1.0(4) . . . . ?
Ti1 C48 C52 C51 -65.6(3) . . . . ?
C49 C48 C52 Ti1 64.6(3) . . . . ?
C57 C53 C54 C55 -1.0(4) . . . . ?
Ti1 C53 C54 C55 64.9(2) . . . . ?
C57 C53 C54 Ti1 -65.9(2) . . . . ?
C53 C54 C55 C56 1.6(4) . . . . ?
Ti1 C54 C55 C56 66.0(2) . . . . ?
C53 C54 C55 Ti1 -64.4(2) . . . . ?
C54 C55 C56 C57 -1.7(4) . . . . ?
Ti1 C55 C56 C57 63.5(3) . . . . ?
C54 C55 C56 Ti1 -65.2(2) . . . . ?
C55 C56 C57 C53 1.1(4) . . . . ?
Ti1 C56 C57 C53 64.3(2) . . . . ?
C55 C56 C57 Ti1 -63.2(2) . . . . ?
C54 C53 C57 C56 -0.1(4) . . . . ?
Ti1 C53 C57 C56 -65.6(2) . . . . ?
C54 C53 C57 Ti1 65.5(2) . . . . ?
C63 C58 C59 C60 -1.8(6) . . . . ?
C58 C59 C60 C61 0.7(6) . . . . ?
C59 C60 C61 C62 1.2(7) . . . . ?
C60 C61 C62 C63 -2.1(7) . . . . ?
C59 C58 C63 C62 0.9(6) . . . . ?
C61 C62 C63 C58 1.0(6) . . . . ?
C69 C64 C65 C66 -1.6(8) . . . . ?
C64 C65 C66 C67 1.5(7) . . . . ?
C65 C66 C67 C68 -1.3(7) . . . . ?
C66 C67 C68 C69 1.2(8) . . . . ?
C65 C64 C69 C68 1.5(8) . . . . ?
C67 C68 C69 C64 -1.3(9) . . . . ?
C75 C70 C71 C72 0.5(7) . . . . ?
C70 C71 C72 C73 0.3(7) . . . . ?
C71 C72 C73 C74 -1.1(7) . . . . ?
C72 C73 C74 C75 1.3(7) . . . . ?
C71 C70 C75 C74 -0.3(7) . . . . ?
C73 C74 C75 C70 -0.5(7) . . . . ?
C81 C76 C77 C78 0.3(7) . . . . ?
C76 C77 C78 C79 0.9(7) . . . . ?
C77 C78 C79 C80 -0.6(8) . . . . ?
C78 C79 C80 C81 -1.0(9) . . . . ?
C79 C80 C81 C76 2.2(8) . . . . ?
C77 C76 C81 C80 -1.9(8) . . . . ?
C87 C82 C83 C84 0.6(8) . . . . ?
C82 C83 C84 C85 -0.8(10) . . . . ?
C83 C84 C85 C86 0.3(10) . . . . ?
C84 C85 C86 C87 0.5(9) . . . . ?
C85 C86 C87 C82 -0.8(8) . . . . ?
C83 C82 C87 C86 0.2(8) . . . . ?
C2 C1 N1 C4 0.0(3) . . . . ?
C40 C1 N1 C4 177.0(3) . . . . ?
C2 C1 N1 U1 159.7(2) . . . . ?
C40 C1 N1 U1 -23.3(5) . . . . ?
C3 C4 N1 C1 -0.1(3) . . . . ?
C5 C4 N1 C1 -175.8(3) . . . . ?
C3 C4 N1 U1 -165.0(2) . . . . ?
C5 C4 N1 U1 19.3(3) . . . . ?
C4 C5 N2 C6 175.8(3) . . . . ?
C4 C5 N2 U1 -13.8(3) . . . . ?
C7 C6 N2 C5 49.8(4) . . . . ?
C13 C6 N2 C5 -125.2(3) . . . . ?
C7 C6 N2 U1 -117.8(3) . . . . ?
C13 C6 N2 U1 67.2(4) . . . . ?
C15 C14 N3 C13 -179.7(3) . . . . ?
C12 C13 N3 C14 -21.2(4) . . . . ?
C6 C13 N3 C14 156.4(3) . . . . ?
C17 C18 N4 C15 0.3(4) . . . . ?
C19 C18 N4 C15 177.0(3) . . . . ?
C16 C15 N4 C18 -0.3(4) . . . . ?
C14 C15 N4 C18 177.8(3) . . . . ?
C23 C22 N5 C25 0.7(4) . . . . ?
C19 C22 N5 C25 -179.2(3) . . . . ?
C24 C25 N5 C22 -0.8(4) . . . . ?
C26 C25 N5 C22 -179.5(3) . . . . ?
C25 C26 N6 C27 178.8(3) . . . . ?
C34 C27 N6 C26 -130.4(3) . . . . ?
C28 C27 N6 C26 50.1(4) . . . . ?
C36 C35 N7 C34 -177.6(3) . . . . ?
C36 C35 N7 U1 11.1(4) . . . . ?
C33 C34 N7 C35 -57.7(4) . . . . ?
C27 C34 N7 C35 120.4(3) . . . . ?
C33 C34 N7 U1 111.7(3) . . . . ?
C27 C34 N7 U1 -70.2(4) . . . . ?
C38 C39 N8 C36 0.2(3) . . . . ?
C40 C39 N8 C36 -174.6(3) . . . . ?
C38 C39 N8 U1 -161.7(2) . . . . ?
C40 C39 N8 U1 23.5(4) . . . . ?
C37 C36 N8 C39 0.3(3) . . . . ?
C35 C36 N8 C39 177.4(3) . . . . ?
C37 C36 N8 U1 166.6(2) . . . . ?
C35 C36 N8 U1 -16.3(3) . . . . ?
C46 C47 N9 C43 -2.8(5) . . . . ?
C46 C47 N9 U1 -175.1(3) . . . . ?
C44 C43 N9 C47 2.2(5) . . . . ?
C44 C43 N9 U1 174.5(3) . . . . ?
U1 O2 Ti1 Cl1 90.0(12) . . . . ?
U1 O2 Ti1 C53 -51.1(12) . . . . ?
U1 O2 Ti1 C50 -133.7(12) . . . . ?
U1 O2 Ti1 C54 -32.2(12) . . . . ?
U1 O2 Ti1 C55 1.9(12) . . . . ?
U1 O2 Ti1 C57 -25.1(13) . . . . ?
U1 O2 Ti1 C51 -138.1(12) . . . . ?
U1 O2 Ti1 C52 177.8(12) . . . . ?
U1 O2 Ti1 C56 11.3(13) . . . . ?
U1 O2 Ti1 C49 -163.5(12) . . . . ?
U1 O2 Ti1 C48 169.8(12) . . . . ?
C54 C53 Ti1 O2 34.2(2) . . . . ?
C57 C53 Ti1 O2 148.80(19) . . . . ?
C54 C53 Ti1 Cl1 -84.7(2) . . . . ?
C57 C53 Ti1 Cl1 29.9(3) . . . . ?
C54 C53 Ti1 C50 126.0(2) . . . . ?
C57 C53 Ti1 C50 -119.4(2) . . . . ?
C57 C53 Ti1 C54 114.6(3) . . . . ?
C54 C53 Ti1 C55 -36.9(2) . . . . ?
C57 C53 Ti1 C55 77.7(2) . . . . ?
C54 C53 Ti1 C57 -114.6(3) . . . . ?
C54 C53 Ti1 C51 160.4(2) . . . . ?
C57 C53 Ti1 C51 -85.0(2) . . . . ?
C54 C53 Ti1 C52 178.2(2) . . . . ?
C57 C53 Ti1 C52 -67.2(2) . . . . ?
C54 C53 Ti1 C56 -77.9(2) . . . . ?
C57 C53 Ti1 C56 36.7(2) . . . . ?
C54 C53 Ti1 C49 119.3(2) . . . . ?
C57 C53 Ti1 C49 -126.1(2) . . . . ?
C54 C53 Ti1 C48 154.6(2) . . . . ?
C57 C53 Ti1 C48 -90.8(2) . . . . ?
C51 C50 Ti1 O2 -173.8(2) . . . . ?
C49 C50 Ti1 O2 -59.5(2) . . . . ?
C51 C50 Ti1 Cl1 -72.3(2) . . . . ?
C49 C50 Ti1 Cl1 42.1(2) . . . . ?
C51 C50 Ti1 C53 76.4(2) . . . . ?
C49 C50 Ti1 C53 -169.2(2) . . . . ?
C51 C50 Ti1 C54 104.5(2) . . . . ?
C49 C50 Ti1 C54 -141.1(2) . . . . ?
C51 C50 Ti1 C55 97.2(3) . . . . ?
C49 C50 Ti1 C55 -148.4(2) . . . . ?
C51 C50 Ti1 C57 46.3(2) . . . . ?
C49 C50 Ti1 C57 160.7(2) . . . . ?
C49 C50 Ti1 C51 114.4(3) . . . . ?
C51 C50 Ti1 C52 -36.7(2) . . . . ?
C49 C50 Ti1 C52 77.7(2) . . . . ?
C51 C50 Ti1 C56 49.1(3) . . . . ?
C49 C50 Ti1 C56 163.4(2) . . . . ?
C51 C50 Ti1 C49 -114.4(3) . . . . ?
C51 C50 Ti1 C48 -77.9(2) . . . . ?
C49 C50 Ti1 C48 36.5(2) . . . . ?
C55 C54 Ti1 O2 96.2(2) . . . . ?
C53 C54 Ti1 O2 -147.7(2) . . . . ?
C55 C54 Ti1 Cl1 6.4(2) . . . . ?
C53 C54 Ti1 Cl1 122.45(19) . . . . ?
C55 C54 Ti1 C53 -116.1(3) . . . . ?
C55 C54 Ti1 C50 -171.0(2) . . . . ?
C53 C54 Ti1 C50 -54.9(2) . . . . ?
C53 C54 Ti1 C55 116.1(3) . . . . ?
C55 C54 Ti1 C57 -78.1(2) . . . . ?
C53 C54 Ti1 C57 38.0(2) . . . . ?
C55 C54 Ti1 C51 -136.1(2) . . . . ?
C53 C54 Ti1 C51 -20.0(2) . . . . ?
C55 C54 Ti1 C52 -118.8(2) . . . . ?
C53 C54 Ti1 C52 -2.7(3) . . . . ?
C55 C54 Ti1 C56 -37.6(2) . . . . ?
C53 C54 Ti1 C56 78.5(2) . . . . ?
C55 C54 Ti1 C49 162.77(19) . . . . ?
C53 C54 Ti1 C49 -81.1(2) . . . . ?
C55 C54 Ti1 C48 -176.3(3) . . . . ?
C53 C54 Ti1 C48 -60.2(4) . . . . ?
C54 C55 Ti1 O2 -79.8(2) . . . . ?
C56 C55 Ti1 O2 165.2(2) . . . . ?
C54 C55 Ti1 Cl1 -174.64(19) . . . . ?
C56 C55 Ti1 Cl1 70.3(2) . . . . ?
C54 C55 Ti1 C53 37.34(19) . . . . ?
C56 C55 Ti1 C53 -77.7(2) . . . . ?
C54 C55 Ti1 C50 12.7(3) . . . . ?
C56 C55 Ti1 C50 -102.4(2) . . . . ?
C56 C55 Ti1 C54 -115.1(3) . . . . ?
C54 C55 Ti1 C57 78.9(2) . . . . ?
C56 C55 Ti1 C57 -36.2(2) . . . . ?
C54 C55 Ti1 C51 59.3(3) . . . . ?
C56 C55 Ti1 C51 -55.8(3) . . . . ?
C54 C55 Ti1 C52 105.3(3) . . . . ?
C56 C55 Ti1 C52 -9.8(3) . . . . ?
C54 C55 Ti1 C56 115.1(3) . . . . ?
C54 C55 Ti1 C49 -38.9(4) . . . . ?
C56 C55 Ti1 C49 -154.0(3) . . . . ?
C54 C55 Ti1 C48 173.6(5) . . . . ?
C56 C55 Ti1 C48 58.5(6) . . . . ?
C56 C57 Ti1 O2 69.3(3) . . . . ?
C53 C57 Ti1 O2 -46.3(3) . . . . ?
C56 C57 Ti1 Cl1 -42.9(2) . . . . ?
C53 C57 Ti1 Cl1 -158.58(19) . . . . ?
C56 C57 Ti1 C53 115.6(3) . . . . ?
C56 C57 Ti1 C50 176.3(2) . . . . ?
C53 C57 Ti1 C50 60.7(2) . . . . ?
C56 C57 Ti1 C54 77.7(2) . . . . ?
C53 C57 Ti1 C54 -37.9(2) . . . . ?
C56 C57 Ti1 C55 36.7(2) . . . . ?
C53 C57 Ti1 C55 -79.0(2) . . . . ?
C56 C57 Ti1 C51 -158.8(2) . . . . ?
C53 C57 Ti1 C51 85.6(2) . . . . ?
C56 C57 Ti1 C52 -127.8(2) . . . . ?
C53 C57 Ti1 C52 116.5(2) . . . . ?
C53 C57 Ti1 C56 -115.6(3) . . . . ?
C56 C57 Ti1 C49 -169.4(2) . . . . ?
C53 C57 Ti1 C49 74.9(2) . . . . ?
C56 C57 Ti1 C48 -128.5(2) . . . . ?
C53 C57 Ti1 C48 115.9(2) . . . . ?
C52 C51 Ti1 O2 -108.1(2) . . . . ?
C50 C51 Ti1 O2 7.9(3) . . . . ?
C52 C51 Ti1 Cl1 14.8(2) . . . . ?
C50 C51 Ti1 Cl1 130.7(2) . . . . ?
C52 C51 Ti1 C53 147.6(2) . . . . ?
C50 C51 Ti1 C53 -96.4(2) . . . . ?
C52 C51 Ti1 C50 -115.9(3) . . . . ?
C52 C51 Ti1 C54 159.2(2) . . . . ?
C50 C51 Ti1 C54 -84.8(2) . . . . ?
C52 C51 Ti1 C55 128.7(2) . . . . ?
C50 C51 Ti1 C55 -115.4(2) . . . . ?
C52 C51 Ti1 C57 111.7(2) . . . . ?
C50 C51 Ti1 C57 -132.4(2) . . . . ?
C50 C51 Ti1 C52 115.9(3) . . . . ?
C52 C51 Ti1 C56 99.6(2) . . . . ?
C50 C51 Ti1 C56 -144.5(2) . . . . ?
C52 C51 Ti1 C49 -77.9(2) . . . . ?
C50 C51 Ti1 C49 38.0(2) . . . . ?
C52 C51 Ti1 C48 -37.6(2) . . . . ?
C50 C51 Ti1 C48 78.3(2) . . . . ?
C51 C52 Ti1 O2 100.9(2) . . . . ?
C48 C52 Ti1 O2 -14.2(3) . . . . ?
C51 C52 Ti1 Cl1 -166.9(2) . . . . ?
C48 C52 Ti1 Cl1 77.9(2) . . . . ?
C51 C52 Ti1 C53 -32.2(2) . . . . ?
C48 C52 Ti1 C53 -147.4(2) . . . . ?
C51 C52 Ti1 C50 37.3(2) . . . . ?
C48 C52 Ti1 C50 -77.8(2) . . . . ?
C51 C52 Ti1 C54 -30.7(3) . . . . ?
C48 C52 Ti1 C54 -145.8(2) . . . . ?
C51 C52 Ti1 C55 -85.8(3) . . . . ?
C48 C52 Ti1 C55 159.0(2) . . . . ?
C51 C52 Ti1 C57 -63.9(2) . . . . ?
C48 C52 Ti1 C57 -179.1(3) . . . . ?
C48 C52 Ti1 C51 -115.2(3) . . . . ?
C51 C52 Ti1 C56 -91.6(2) . . . . ?
C48 C52 Ti1 C56 153.3(2) . . . . ?
C51 C52 Ti1 C49 78.8(2) . . . . ?
C48 C52 Ti1 C49 -36.3(2) . . . . ?
C51 C52 Ti1 C48 115.2(3) . . . . ?
C57 C56 Ti1 O2 -134.1(2) . . . . ?
C55 C56 Ti1 O2 -17.0(2) . . . . ?
C57 C56 Ti1 Cl1 137.2(2) . . . . ?
C55 C56 Ti1 Cl1 -105.7(2) . . . . ?
C57 C56 Ti1 C53 -37.8(2) . . . . ?
C55 C56 Ti1 C53 79.3(2) . . . . ?
C57 C56 Ti1 C50 -4.9(3) . . . . ?
C55 C56 Ti1 C50 112.2(2) . . . . ?
C57 C56 Ti1 C54 -79.5(2) . . . . ?
C55 C56 Ti1 C54 37.6(2) . . . . ?
C57 C56 Ti1 C55 -117.1(3) . . . . ?
C55 C56 Ti1 C57 117.1(3) . . . . ?
C57 C56 Ti1 C51 21.4(2) . . . . ?
C55 C56 Ti1 C51 138.5(2) . . . . ?
C57 C56 Ti1 C52 56.7(2) . . . . ?
C55 C56 Ti1 C52 173.8(2) . . . . ?
C57 C56 Ti1 C49 28.4(5) . . . . ?
C55 C56 Ti1 C49 145.6(4) . . . . ?
C57 C56 Ti1 C48 78.9(3) . . . . ?
C55 C56 Ti1 C48 -164.0(2) . . . . ?
C48 C49 Ti1 O2 -125.9(2) . . . . ?
C50 C49 Ti1 O2 118.4(2) . . . . ?
C48 C49 Ti1 Cl1 -34.7(2) . . . . ?
C50 C49 Ti1 Cl1 -150.49(19) . . . . ?
C48 C49 Ti1 C53 127.6(2) . . . . ?
C50 C49 Ti1 C53 11.8(2) . . . . ?
C48 C49 Ti1 C50 115.8(3) . . . . ?
C48 C49 Ti1 C54 165.9(2) . . . . ?
C50 C49 Ti1 C54 50.2(2) . . . . ?
C48 C49 Ti1 C55 -167.8(3) . . . . ?
C50 C49 Ti1 C55 76.4(4) . . . . ?
C48 C49 Ti1 C57 90.2(2) . . . . ?
C50 C49 Ti1 C57 -25.6(3) . . . . ?
C48 C49 Ti1 C51 77.9(2) . . . . ?
C50 C49 Ti1 C51 -37.9(2) . . . . ?
C48 C49 Ti1 C52 37.2(2) . . . . ?
C50 C49 Ti1 C52 -78.6(2) . . . . ?
C48 C49 Ti1 C56 69.8(5) . . . . ?
C50 C49 Ti1 C56 -46.0(5) . . . . ?
C50 C49 Ti1 C48 -115.8(3) . . . . ?
C49 C48 Ti1 O2 52.9(2) . . . . ?
C52 C48 Ti1 O2 169.2(2) . . . . ?
C49 C48 Ti1 Cl1 146.4(2) . . . . ?
C52 C48 Ti1 Cl1 -97.4(2) . . . . ?
C49 C48 Ti1 C53 -72.3(3) . . . . ?
C52 C48 Ti1 C53 44.0(3) . . . . ?
C49 C48 Ti1 C50 -37.6(2) . . . . ?
C52 C48 Ti1 C50 78.7(3) . . . . ?
C49 C48 Ti1 C54 -31.4(4) . . . . ?
C52 C48 Ti1 C54 84.9(4) . . . . ?
C49 C48 Ti1 C55 158.4(5) . . . . ?
C52 C48 Ti1 C55 -85.4(6) . . . . ?
C49 C48 Ti1 C57 -115.2(2) . . . . ?
C52 C48 Ti1 C57 1.1(3) . . . . ?
C49 C48 Ti1 C51 -79.1(2) . . . . ?
C52 C48 Ti1 C51 37.2(2) . . . . ?
C49 C48 Ti1 C52 -116.3(3) . . . . ?
C49 C48 Ti1 C56 -155.8(2) . . . . ?
C52 C48 Ti1 C56 -39.5(3) . . . . ?
C52 C48 Ti1 C49 116.3(3) . . . . ?
Ti1 O2 U1 O1 170.1(15) . . . . ?
Ti1 O2 U1 N1 54.0(12) . . . . ?
Ti1 O2 U1 N8 -17.4(12) . . . . ?
Ti1 O2 U1 N9 -157.9(12) . . . . ?
Ti1 O2 U1 N7 -84.3(12) . . . . ?
Ti1 O2 U1 N2 121.4(12) . . . . ?
C1 N1 U1 O1 89.7(3) . . . . ?
C4 N1 U1 O1 -111.8(2) . . . . ?
C1 N1 U1 O2 -92.6(3) . . . . ?
C4 N1 U1 O2 65.9(2) . . . . ?
C1 N1 U1 N8 -3.2(3) . . . . ?
C4 N1 U1 N8 155.3(2) . . . . ?
C1 N1 U1 N9 -177.0(3) . . . . ?
C4 N1 U1 N9 -18.5(3) . . . . ?
C1 N1 U1 N7 -13.4(3) . . . . ?
C4 N1 U1 N7 145.07(18) . . . . ?
C1 N1 U1 N2 -176.2(3) . . . . ?
C4 N1 U1 N2 -17.65(19) . . . . ?
C39 N8 U1 O1 -90.0(3) . . . . ?
C36 N8 U1 O1 109.3(2) . . . . ?
C39 N8 U1 O2 90.4(3) . . . . ?
C36 N8 U1 O2 -70.4(2) . . . . ?
C39 N8 U1 N1 3.0(3) . . . . ?
C36 N8 U1 N1 -157.8(2) . . . . ?
C39 N8 U1 N9 177.8(3) . . . . ?
C36 N8 U1 N9 17.1(3) . . . . ?
C39 N8 U1 N7 175.5(3) . . . . ?
C36 N8 U1 N7 14.71(19) . . . . ?
C39 N8 U1 N2 12.7(3) . . . . ?
C36 N8 U1 N2 -148.09(18) . . . . ?
C47 N9 U1 O1 12.6(2) . . . . ?
C43 N9 U1 O1 -159.5(2) . . . . ?
C47 N9 U1 O2 -166.1(2) . . . . ?
C43 N9 U1 O2 21.9(2) . . . . ?
C47 N9 U1 N1 -82.3(3) . . . . ?
C43 N9 U1 N1 105.6(3) . . . . ?
C47 N9 U1 N8 106.9(2) . . . . ?
C43 N9 U1 N8 -65.2(3) . . . . ?
C47 N9 U1 N7 109.1(2) . . . . ?
C43 N9 U1 N7 -63.0(2) . . . . ?
C47 N9 U1 N2 -83.1(2) . . . . ?
C43 N9 U1 N2 104.8(2) . . . . ?
C35 N7 U1 O1 -105.3(2) . . . . ?
C34 N7 U1 O1 84.9(3) . . . . ?
C35 N7 U1 O2 77.2(2) . . . . ?
C34 N7 U1 O2 -92.6(3) . . . . ?
C35 N7 U1 N1 -2.8(3) . . . . ?
C34 N7 U1 N1 -172.6(2) . . . . ?
C35 N7 U1 N8 -13.4(2) . . . . ?
C34 N7 U1 N8 176.8(3) . . . . ?
C35 N7 U1 N9 168.2(2) . . . . ?
C34 N7 U1 N9 -1.6(2) . . . . ?
C35 N7 U1 N2 142.1(2) . . . . ?
C34 N7 U1 N2 -27.7(3) . . . . ?
C5 N2 U1 O1 108.4(2) . . . . ?
C6 N2 U1 O1 -83.5(3) . . . . ?
C5 N2 U1 O2 -73.5(2) . . . . ?
C6 N2 U1 O2 94.6(3) . . . . ?
C5 N2 U1 N1 16.24(19) . . . . ?
C6 N2 U1 N1 -175.7(3) . . . . ?
C5 N2 U1 N8 6.3(2) . . . . ?
C6 N2 U1 N8 174.3(2) . . . . ?
C5 N2 U1 N9 -164.2(2) . . . . ?
C6 N2 U1 N9 3.8(2) . . . . ?
C5 N2 U1 N7 -138.9(2) . . . . ?
C6 N2 U1 N7 29.1(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.936
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.119
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.097
####################################################################### 
# 
# 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_exp_1443mcref
_database_code_depnum_ccdc_archive 'CCDC 1883753'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;university of edinburgh
United Kingdom
;
_audit_update_record             
;
2018-12-07 deposited with the CCDC.	2019-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C86.48 H86.48 Cl3 Mg N15 O2 U Zr'
_chemical_formula_weight         1827.82

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'
Zr Zr -2.9673 0.5597 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'

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

_cell_length_a                   47.424(5)
_cell_length_b                   14.484(5)
_cell_length_c                   30.602(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 127.576(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     16659(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    2688
_cell_measurement_theta_min      2.9406
_cell_measurement_theta_max      24.6598

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.3022
_exptl_crystal_size_mid          0.0610
_exptl_crystal_size_min          0.0197
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7371
_exptl_absorpt_coefficient_mu    2.227
_exptl_absorpt_correction_T_min  0.97105
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            49400
_diffrn_reflns_av_R_equivalents  0.1985
_diffrn_reflns_av_sigmaI/netI    0.2458
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         24.71
_reflns_number_total             14167
_reflns_number_gt                7401
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    MERCURY
_computing_publication_material  ORTEP

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0593P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14167
_refine_ls_number_parameters     979
_refine_ls_number_restraints     108
_refine_ls_R_factor_all          0.1889
_refine_ls_R_factor_gt           0.0965
_refine_ls_wR_factor_ref         0.2032
_refine_ls_wR_factor_gt          0.1660
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2185(4) 0.3316(8) 0.6754(5) 0.027(3) Uani 1 1 d . . .
C2 C 0.2292(4) 0.3517(9) 0.7281(5) 0.035(4) Uani 1 1 d . . .
H2 H 0.2398 0.3097 0.7582 0.042 Uiso 1 1 calc R . .
C3 C 0.2215(4) 0.4444(10) 0.7288(6) 0.039(4) Uani 1 1 d . . .
H3 H 0.2261 0.4783 0.7592 0.047 Uiso 1 1 calc R . .
C4 C 0.2055(3) 0.4769(9) 0.6756(5) 0.029(4) Uani 1 1 d . . .
C5 C 0.1902(3) 0.5665(9) 0.6542(5) 0.026(3) Uani 1 1 d . . .
H5 H 0.1914 0.6120 0.6776 0.031 Uiso 1 1 calc R . .
C6 C 0.1585(4) 0.6758(9) 0.5845(6) 0.028(3) Uani 1 1 d . . .
C7 C 0.1776(4) 0.7551(8) 0.6105(6) 0.027(3) Uani 1 1 d . . .
H7 H 0.2023 0.7503 0.6401 0.032 Uiso 1 1 calc R . .
C8 C 0.1623(4) 0.8398(8) 0.5952(6) 0.031(4) Uani 1 1 d . . .
C9 C 0.1827(4) 0.9247(9) 0.6243(6) 0.051(5) Uani 1 1 d . . .
H9A H 0.1670 0.9785 0.6071 0.076 Uiso 1 1 calc R . .
H9B H 0.2023 0.9309 0.6221 0.076 Uiso 1 1 calc R . .
H9C H 0.1922 0.9210 0.6631 0.076 Uiso 1 1 calc R . .
C10 C 0.1257(4) 0.8466(9) 0.5483(6) 0.038(4) Uani 1 1 d . . .
C11 C 0.1082(4) 0.9394(9) 0.5290(7) 0.057(5) Uani 1 1 d . . .
H11A H 0.1257 0.9877 0.5520 0.085 Uiso 1 1 calc R . .
H11B H 0.0887 0.9425 0.5317 0.085 Uiso 1 1 calc R . .
H11C H 0.0988 0.9486 0.4905 0.085 Uiso 1 1 calc R . .
C12 C 0.1071(4) 0.7674(10) 0.5229(6) 0.039(4) Uani 1 1 d . . .
H12 H 0.0827 0.7720 0.4919 0.047 Uiso 1 1 calc R . .
C13 C 0.1226(4) 0.6797(9) 0.5409(6) 0.031(4) Uani 1 1 d . . .
C14 C 0.0731(4) 0.5884(10) 0.5021(6) 0.037(4) Uani 1 1 d . . .
H14 H 0.0619 0.6398 0.5050 0.045 Uiso 1 1 calc R . .
C15 C 0.0544(4) 0.5015(11) 0.4806(6) 0.040(4) Uani 1 1 d . . .
C16 C 0.0203(4) 0.4774(11) 0.4630(7) 0.059(5) Uani 1 1 d . . .
H16 H 0.0042 0.5160 0.4631 0.071 Uiso 1 1 calc R . .
C17 C 0.0146(4) 0.3844(11) 0.4451(6) 0.048(5) Uani 1 1 d . . .
H17 H -0.0060 0.3482 0.4310 0.057 Uiso 1 1 calc R . .
C18 C 0.0450(4) 0.3569(11) 0.4524(6) 0.041(4) Uani 1 1 d . . .
C19 C 0.0536(4) 0.2632(11) 0.4396(6) 0.042(4) Uani 1 1 d . . .
C20 C 0.0873(4) 0.2226(10) 0.4908(6) 0.060(5) Uani 1 1 d . . .
H20A H 0.0920 0.1624 0.4818 0.090 Uiso 1 1 calc R . .
H20B H 0.0844 0.2150 0.5196 0.090 Uiso 1 1 calc R . .
H20C H 0.1073 0.2643 0.5039 0.090 Uiso 1 1 calc R . .
C21 C 0.0226(4) 0.1946(10) 0.4198(6) 0.060(5) Uani 1 1 d . . .
H21A H 0.0004 0.2193 0.3868 0.090 Uiso 1 1 calc R . .
H21B H 0.0200 0.1866 0.4491 0.090 Uiso 1 1 calc R . .
H21C H 0.0278 0.1349 0.4112 0.090 Uiso 1 1 calc R . .
C22 C 0.0582(4) 0.2774(10) 0.3954(7) 0.047(4) Uani 1 1 d . . .
C23 C 0.0355(5) 0.2581(11) 0.3396(7) 0.061(5) Uani 1 1 d . . .
H23 H 0.0129 0.2294 0.3203 0.074 Uiso 1 1 calc R . .
C24 C 0.0516(4) 0.2880(11) 0.3170(7) 0.054(5) Uani 1 1 d . . .
H24 H 0.0427 0.2788 0.2799 0.065 Uiso 1 1 calc R . .
C25 C 0.0828(4) 0.3334(10) 0.3568(7) 0.046(4) Uani 1 1 d . . .
C26 C 0.1091(4) 0.3760(9) 0.3555(6) 0.037(4) Uani 1 1 d . . .
H26 H 0.1061 0.3770 0.3218 0.044 Uiso 1 1 calc R . .
C27 C 0.1622(4) 0.4551(10) 0.3950(5) 0.033(4) Uani 1 1 d . . .
C28 C 0.1545(4) 0.4958(9) 0.3472(6) 0.038(4) Uani 1 1 d . . .
H28 H 0.1304 0.4993 0.3154 0.045 Uiso 1 1 calc R . .
C29 C 0.1804(4) 0.5312(10) 0.3441(6) 0.043(4) Uani 1 1 d . . .
C30 C 0.1694(4) 0.5681(11) 0.2903(6) 0.062(5) Uani 1 1 d . . .
H30A H 0.1903 0.5906 0.2944 0.093 Uiso 1 1 calc R . .
H30B H 0.1525 0.6190 0.2786 0.093 Uiso 1 1 calc R . .
H30C H 0.1580 0.5189 0.2626 0.093 Uiso 1 1 calc R . .
C31 C 0.2156(4) 0.5261(9) 0.3903(6) 0.039(4) Uani 1 1 d . . .
C33 C 0.2443(4) 0.5579(11) 0.3877(6) 0.058(5) Uani 1 1 d . . .
H33A H 0.2338 0.5806 0.3505 0.087 Uiso 1 1 calc R . .
H33B H 0.2604 0.5063 0.3965 0.087 Uiso 1 1 calc R . .
H33C H 0.2577 0.6078 0.4144 0.087 Uiso 1 1 calc R . .
C34 C 0.2230(4) 0.4909(9) 0.4379(6) 0.034(4) Uani 1 1 d . . .
H34 H 0.2470 0.4912 0.4703 0.041 Uiso 1 1 calc R . .
C35 C 0.1975(4) 0.4551(8) 0.4411(5) 0.027(3) Uani 1 1 d . . .
C36 C 0.2336(4) 0.3599(9) 0.5169(6) 0.040(4) Uani 1 1 d . . .
H36 H 0.2476 0.3545 0.5044 0.047 Uiso 1 1 calc R . .
C37 C 0.2433(4) 0.3064(9) 0.5644(6) 0.031(4) Uani 1 1 d . . .
C38 C 0.2689(4) 0.2389(10) 0.5937(6) 0.045(4) Uani 1 1 d . . .
H38 H 0.2860 0.2193 0.5891 0.054 Uiso 1 1 calc R . .
C39 C 0.2644(4) 0.2063(9) 0.6310(6) 0.037(4) Uani 1 1 d . . .
H39 H 0.2788 0.1607 0.6582 0.044 Uiso 1 1 calc R . .
C40 C 0.2354(4) 0.2502(9) 0.6228(6) 0.035(4) Uani 1 1 d . . .
C41 C 0.2196(4) 0.2397(9) 0.6529(6) 0.031(4) Uani 1 1 d . . .
C42 C 0.2403(4) 0.1690(9) 0.6991(5) 0.034(4) Uani 1 1 d . . .
H42A H 0.2295 0.1627 0.7178 0.051 Uiso 1 1 calc R . .
H42B H 0.2650 0.1895 0.7256 0.051 Uiso 1 1 calc R . .
H42C H 0.2398 0.1093 0.6835 0.051 Uiso 1 1 calc R . .
C43 C 0.1807(4) 0.2065(9) 0.6113(6) 0.043(4) Uani 1 1 d . . .
H43A H 0.1701 0.1989 0.6302 0.065 Uiso 1 1 calc R . .
H43B H 0.1803 0.1473 0.5954 0.065 Uiso 1 1 calc R . .
H43C H 0.1671 0.2523 0.5818 0.065 Uiso 1 1 calc R . .
C44 C 0.1779(4) 0.6789(10) 0.4973(7) 0.049(5) Uani 1 1 d . . .
H44 H 0.2014 0.6830 0.5308 0.059 Uiso 1 1 calc R . .
C45 C 0.1642(5) 0.7562(11) 0.4636(9) 0.083(7) Uani 1 1 d U . .
H45 H 0.1775 0.8117 0.4741 0.100 Uiso 1 1 calc R . .
C46 C 0.1315(6) 0.7499(16) 0.4158(11) 0.111(10) Uani 1 1 d . . .
H46 H 0.1216 0.8008 0.3911 0.133 Uiso 1 1 calc R . .
C47 C 0.1122(5) 0.6697(14) 0.4022(7) 0.069(6) Uani 1 1 d . . .
H47 H 0.0889 0.6645 0.3685 0.083 Uiso 1 1 calc R . .
C48 C 0.1279(4) 0.5963(11) 0.4394(6) 0.047(4) Uani 1 1 d . . .
H48 H 0.1144 0.5415 0.4306 0.057 Uiso 1 1 calc R . .
C49 C 0.2985(4) 0.4216(10) 0.6909(7) 0.046(5) Uani 1 1 d . . .
H49 H 0.2829 0.3719 0.6695 0.056 Uiso 1 1 calc R . .
C50 C 0.2953(4) 0.4782(11) 0.7229(6) 0.048(4) Uani 1 1 d . . .
H50 H 0.2772 0.4750 0.7273 0.058 Uiso 1 1 calc R . .
C51 C 0.3237(4) 0.5428(12) 0.7488(6) 0.055(5) Uani 1 1 d . . .
H51 H 0.3283 0.5903 0.7738 0.067 Uiso 1 1 calc R . .
C52 C 0.3429(4) 0.5223(11) 0.7301(7) 0.054(5) Uani 1 1 d . . .
H52 H 0.3635 0.5547 0.7402 0.065 Uiso 1 1 calc R . .
C53 C 0.3278(5) 0.4467(12) 0.6938(7) 0.061(5) Uani 1 1 d . . .
H53 H 0.3360 0.4188 0.6752 0.073 Uiso 1 1 calc R . .
C54 C 0.3269(4) 0.6130(11) 0.6251(6) 0.042(4) Uani 1 1 d . . .
H54 H 0.3506 0.5906 0.6495 0.050 Uiso 1 1 calc R . .
C55 C 0.3151(5) 0.6986(11) 0.6281(7) 0.056(5) Uani 1 1 d . . .
H55 H 0.3290 0.7447 0.6553 0.067 Uiso 1 1 calc R . .
C56 C 0.2793(4) 0.7044(9) 0.5842(6) 0.038(4) Uani 1 1 d . . .
H56 H 0.2644 0.7559 0.5760 0.046 Uiso 1 1 calc R . .
C57 C 0.2686(4) 0.6236(10) 0.5542(6) 0.039(4) Uani 1 1 d . . .
H57 H 0.2455 0.6097 0.5217 0.047 Uiso 1 1 calc R . .
C58 C 0.2985(4) 0.5662(10) 0.5809(6) 0.037(4) Uani 1 1 d . . .
H58 H 0.2991 0.5050 0.5702 0.045 Uiso 1 1 calc R . .
C59 C 0.0511(7) 0.379(2) 0.7205(11) 0.160(15) Uani 1 1 d . . .
H59 H 0.0746 0.3552 0.7414 0.192 Uiso 1 1 calc R . .
C60 C 0.0456(8) 0.452(3) 0.7397(17) 0.20(2) Uani 1 1 d . . .
H60 H 0.0625 0.4716 0.7768 0.238 Uiso 1 1 calc R . .
C61 C 0.0152(10) 0.4984(17) 0.7046(14) 0.137(12) Uani 1 1 d . . .
H61 H 0.0130 0.5604 0.7124 0.165 Uiso 1 1 calc R . .
C62 C -0.0130(6) 0.4559(16) 0.6572(9) 0.092(8) Uani 1 1 d . . .
H62 H -0.0364 0.4812 0.6351 0.111 Uiso 1 1 calc R . .
C63 C -0.0050(5) 0.3744(15) 0.6442(7) 0.077(6) Uani 1 1 d . . .
H63 H -0.0233 0.3439 0.6110 0.093 Uiso 1 1 calc R . .
C64 C 0.1133(4) 0.2495(10) 0.6822(6) 0.043(4) Uani 1 1 d . . .
H64 H 0.1217 0.2070 0.7114 0.051 Uiso 1 1 calc R . .
C65 C 0.1371(5) 0.2891(11) 0.6771(7) 0.050(5) Uani 1 1 d . . .
H65 H 0.1612 0.2699 0.7004 0.061 Uiso 1 1 calc R . .
C66 C 0.1269(5) 0.3536(13) 0.6401(8) 0.069(6) Uani 1 1 d . . .
H66 H 0.1440 0.3852 0.6389 0.083 Uiso 1 1 calc R . .
C67 C 0.0921(6) 0.3747(12) 0.6039(8) 0.070(6) Uani 1 1 d . . .
H67 H 0.0841 0.4192 0.5757 0.084 Uiso 1 1 calc R . .
C68 C 0.0678(4) 0.3293(12) 0.6086(6) 0.062(5) Uani 1 1 d . . .
H68 H 0.0431 0.3428 0.5831 0.075 Uiso 1 1 calc R . .
C69 C 0.0631(6) -0.0092(16) 0.6673(13) 0.170(10) Uani 1 1 d U . .
H69 H 0.0658 0.0011 0.7003 0.204 Uiso 1 1 calc R . .
C70 C 0.0705(7) -0.1044(17) 0.6512(14) 0.197(14) Uani 1 1 d U . .
H70 H 0.0805 -0.1575 0.6742 0.237 Uiso 1 1 calc R . .
C71 C 0.0600(7) -0.098(2) 0.5976(16) 0.185(12) Uani 1 1 d U . .
H71 H 0.0654 -0.1490 0.5844 0.222 Uiso 1 1 calc R . .
C72 C 0.0442(8) -0.033(2) 0.5659(15) 0.177(11) Uani 1 1 d U . .
H72 H 0.0350 -0.0443 0.5287 0.212 Uiso 1 1 calc R . .
C73 C 0.0382(15) 0.051(4) 0.575(3) 0.135(13) Uani 0.48 1 d PU . .
H73 H 0.0260 0.0996 0.5490 0.162 Uiso 0.48 1 calc PR . .
N13 N 0.0005(4) 0.1372(15) 0.6636(7) 0.172(9) Uani 1 1 d GU . .
C74 C -0.0021(5) 0.1837(13) 0.7008(7) 0.202(10) Uani 1 1 d GU . .
H74 H 0.0147 0.2304 0.7238 0.242 Uiso 1 1 calc R . .
C75 C -0.0291(5) 0.1618(16) 0.7044(7) 0.218(11) Uani 1 1 d GU . .
H75 H -0.0309 0.1935 0.7299 0.261 Uiso 1 1 calc R . .
C76 C -0.0537(4) 0.0934(16) 0.6708(9) 0.216(11) Uani 1 1 d GU . .
H76 H -0.0722 0.0785 0.6732 0.260 Uiso 1 1 calc R . .
C77 C -0.0511(5) 0.0470(14) 0.6335(8) 0.224(11) Uani 1 1 d GU . .
H77 H -0.0679 0.0003 0.6105 0.269 Uiso 1 1 calc R . .
C78 C -0.0241(5) 0.0689(15) 0.6299(7) 0.213(11) Uani 1 1 d GU . .
H78 H -0.0224 0.0372 0.6045 0.256 Uiso 1 1 calc R . .
C79 C 0.0856(8) 0.620(2) 0.6866(15) 0.130(14) Uani 1 1 d . . .
H79 H 0.0656 0.5845 0.6767 0.156 Uiso 1 1 calc R . .
C80 C 0.1048(6) 0.6541(17) 0.7330(9) 0.089(9) Uani 1 1 d U . .
H80 H 0.0991 0.6472 0.7577 0.106 Uiso 1 1 calc R . .
C81 C 0.1324(7) 0.6991(17) 0.7476(9) 0.091(7) Uani 1 1 d . . .
H81 H 0.1468 0.7253 0.7836 0.109 Uiso 1 1 calc R . .
C82 C 0.1422(6) 0.7117(18) 0.7154(13) 0.111(9) Uani 1 1 d . . .
H82 H 0.1639 0.7429 0.7297 0.134 Uiso 1 1 calc R . .
C83 C 0.1225(9) 0.682(2) 0.6644(12) 0.130(12) Uani 1 1 d . . .
H83 H 0.1286 0.6941 0.6407 0.156 Uiso 1 1 calc R . .
C84 C 0.3626(6) 0.4878(12) 0.5713(13) 0.080(8) Uani 1 1 d . . .
H84 H 0.3714 0.5489 0.5764 0.096 Uiso 1 1 calc R . .
C85 C 0.3387(6) 0.4559(17) 0.5211(10) 0.082(6) Uani 1 1 d . . .
H85 H 0.3323 0.4925 0.4905 0.098 Uiso 1 1 calc R . .
C86 C 0.3236(6) 0.3751(18) 0.5122(8) 0.079(7) Uani 1 1 d . . .
H86 H 0.3045 0.3551 0.4762 0.095 Uiso 1 1 calc R . .
C87 C 0.3362(6) 0.3234(14) 0.5557(11) 0.087(7) Uani 1 1 d . . .
H87 H 0.3269 0.2626 0.5494 0.105 Uiso 1 1 calc R . .
C88 C 0.3606(5) 0.3483(14) 0.6073(9) 0.074(6) Uani 1 1 d . . .
H88 H 0.3683 0.3091 0.6376 0.088 Uiso 1 1 calc R . .
N1 N 0.2044(3) 0.4088(7) 0.6434(4) 0.027(3) Uani 1 1 d . . .
N2 N 0.1745(3) 0.5855(7) 0.6021(4) 0.028(3) Uani 1 1 d . . .
N3 N 0.1041(3) 0.5962(8) 0.5169(4) 0.038(3) Uani 1 1 d . . .
N4 N 0.0679(3) 0.4273(8) 0.4737(5) 0.033(3) Uani 1 1 d . . .
H4 H 0.0892 0.4250 0.4822 0.040 Uiso 1 1 calc R . .
N5 N 0.0859(3) 0.3247(7) 0.4043(5) 0.043(4) Uani 1 1 d . . .
H5A H 0.1037 0.3471 0.4365 0.051 Uiso 1 1 calc R . .
N6 N 0.1372(3) 0.4135(7) 0.3986(4) 0.030(3) Uani 1 1 d . . .
N7 N 0.2064(3) 0.4148(7) 0.4912(4) 0.031(3) Uani 1 1 d . . .
N8 N 0.2227(3) 0.3154(7) 0.5817(4) 0.027(3) Uani 1 1 d . . .
N9 N 0.1607(3) 0.5990(7) 0.4866(5) 0.033(3) Uani 1 1 d . . .
N10 N 0.0270(4) 0.3361(10) 0.6754(6) 0.063(4) Uani 1 1 d . . .
N11 N 0.0790(3) 0.2679(9) 0.6482(5) 0.049(4) Uani 1 1 d . . .
N12 N 0.0525(4) 0.0563(11) 0.6286(11) 0.123(8) Uani 1 1 d U . .
N14 N 0.0921(8) 0.6304(19) 0.6462(13) 0.176(14) Uani 1 1 d . . .
N15 N 0.3743(5) 0.4361(16) 0.6139(9) 0.131(9) Uani 1 1 d . . .
O1 O 0.1448(2) 0.4054(5) 0.5143(3) 0.028(2) Uani 1 1 d . . .
O2 O 0.2347(2) 0.5257(5) 0.5950(3) 0.025(2) Uani 1 1 d . . .
Zr1 Zr 0.28517(4) 0.57764(9) 0.64690(6) 0.0332(4) Uani 1 1 d . . .
U1 U 0.188205(14) 0.46093(3) 0.55417(2) 0.02450(17) Uani 1 1 d . . .
Cl1 Cl 0.27133(11) 0.7073(3) 0.68130(16) 0.0489(11) Uani 1 1 d . . .
Cl2 Cl -0.00860(11) 0.2187(3) 0.55678(18) 0.0686(14) Uani 1 1 d . . .
Cl3 Cl 0.08672(13) 0.1679(5) 0.7547(2) 0.108(2) Uani 1 1 d . . .
Mg1 Mg 0.03992(15) 0.1960(4) 0.6551(2) 0.0632(18) Uani 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.362(15) . ?
C1 C2 1.397(17) . ?
C1 C41 1.513(17) . ?
C2 C3 1.396(17) . ?
C2 H2 0.9500 . ?
C3 C4 1.392(17) . ?
C3 H3 0.9500 . ?
C4 N1 1.372(15) . ?
C4 C5 1.436(17) . ?
C5 N2 1.314(15) . ?
C5 H5 0.9500 . ?
C6 C7 1.377(17) . ?
C6 C13 1.383(18) . ?
C6 N2 1.443(15) . ?
C7 C8 1.357(16) . ?
C7 H7 0.9500 . ?
C8 C10 1.427(18) . ?
C8 C9 1.480(17) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C12 1.364(18) . ?
C10 C11 1.500(17) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.401(17) . ?
C12 H12 0.9500 . ?
C13 N3 1.410(16) . ?
C14 N3 1.248(17) . ?
C14 C15 1.448(19) . ?
C14 H14 0.9500 . ?
C15 N4 1.333(17) . ?
C15 C16 1.40(2) . ?
C16 C17 1.42(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.38(2) . ?
C17 H17 0.9500 . ?
C18 N4 1.332(16) . ?
C18 C19 1.53(2) . ?
C19 C22 1.51(2) . ?
C19 C20 1.517(19) . ?
C19 C21 1.558(18) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 N5 1.355(17) . ?
C22 C23 1.38(2) . ?
C23 C24 1.37(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.38(2) . ?
C24 H24 0.9500 . ?
C25 N5 1.375(18) . ?
C25 C26 1.41(2) . ?
C26 N6 1.289(15) . ?
C26 H26 0.9500 . ?
C27 C35 1.382(17) . ?
C27 N6 1.396(16) . ?
C27 C28 1.403(18) . ?
C28 C29 1.387(19) . ?
C28 H28 0.9500 . ?
C29 C31 1.382(19) . ?
C29 C30 1.490(19) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C34 1.372(18) . ?
C31 C33 1.482(19) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.374(18) . ?
C34 H34 0.9500 . ?
C35 N7 1.442(16) . ?
C36 N7 1.296(16) . ?
C36 C37 1.451(18) . ?
C36 H36 0.9500 . ?
C37 N8 1.373(16) . ?
C37 C38 1.382(18) . ?
C38 C39 1.366(19) . ?
C38 H38 0.9500 . ?
C39 C40 1.393(18) . ?
C39 H39 0.9500 . ?
C40 N8 1.384(16) . ?
C40 C41 1.505(19) . ?
C41 C42 1.521(16) . ?
C41 C43 1.547(18) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 N9 1.336(17) . ?
C44 C45 1.388(19) . ?
C44 H44 0.9500 . ?
C45 C46 1.34(2) . ?
C45 H45 0.9500 . ?
C46 C47 1.38(2) . ?
C46 H46 0.9500 . ?
C47 C48 1.40(2) . ?
C47 H47 0.9500 . ?
C48 N9 1.330(16) . ?
C48 H48 0.9500 . ?
C49 C50 1.35(2) . ?
C49 C53 1.39(2) . ?
C49 Zr1 2.506(14) . ?
C49 H49 0.9500 . ?
C50 C51 1.42(2) . ?
C50 Zr1 2.521(15) . ?
C50 H50 0.9500 . ?
C51 C52 1.37(2) . ?
C51 Zr1 2.523(14) . ?
C51 H51 0.9500 . ?
C52 C53 1.40(2) . ?
C52 Zr1 2.473(14) . ?
C52 H52 0.9500 . ?
C53 Zr1 2.491(15) . ?
C53 H53 0.9500 . ?
C54 C58 1.372(17) . ?
C54 C55 1.386(19) . ?
C54 Zr1 2.497(14) . ?
C54 H54 0.9500 . ?
C55 C56 1.38(2) . ?
C55 Zr1 2.531(16) . ?
C55 H55 0.9500 . ?
C56 C57 1.380(18) . ?
C56 Zr1 2.545(13) . ?
C56 H56 0.9500 . ?
C57 C58 1.399(18) . ?
C57 Zr1 2.529(15) . ?
C57 H57 0.9500 . ?
C58 Zr1 2.465(14) . ?
C58 H58 0.9500 . ?
C59 N10 1.29(2) . ?
C59 C60 1.32(3) . ?
C59 H59 0.9500 . ?
C60 C61 1.34(4) . ?
C60 H60 0.9500 . ?
C61 C62 1.38(3) . ?
C61 H61 0.9500 . ?
C62 C63 1.37(2) . ?
C62 H62 0.9500 . ?
C63 N10 1.32(2) . ?
C63 H63 0.9500 . ?
C64 N11 1.316(16) . ?
C64 C65 1.36(2) . ?
C64 H64 0.9500 . ?
C65 C66 1.31(2) . ?
C65 H65 0.9500 . ?
C66 C67 1.35(2) . ?
C66 H66 0.9500 . ?
C67 C68 1.41(2) . ?
C67 H67 0.9500 . ?
C68 N11 1.325(18) . ?
C68 H68 0.9500 . ?
C69 N12 1.35(3) . ?
C69 C70 1.57(4) . ?
C69 H69 0.9500 . ?
C70 C71 1.40(5) . ?
C70 H70 0.9500 . ?
C71 C72 1.23(3) . ?
C71 H71 0.9500 . ?
C72 C73 1.32(6) . ?
C72 H72 0.9500 . ?
C73 N12 1.33(7) . ?
C73 H73 0.9500 . ?
N13 C74 1.3900 . ?
N13 C78 1.3900 . ?
N13 Mg1 2.210(13) . ?
C74 C75 1.3900 . ?
C74 H74 0.9500 . ?
C75 C76 1.3900 . ?
C75 H75 0.9500 . ?
C76 C77 1.3900 . ?
C76 H76 0.9500 . ?
C77 C78 1.3900 . ?
C77 H77 0.9500 . ?
C78 H78 0.9500 . ?
C79 C80 1.23(4) . ?
C79 N14 1.45(4) . ?
C79 H79 0.9500 . ?
C80 C81 1.27(3) . ?
C80 H80 0.9500 . ?
C81 C82 1.34(3) . ?
C81 H81 0.9500 . ?
C82 C83 1.31(3) . ?
C82 H82 0.9500 . ?
C83 N14 1.40(3) . ?
C83 H83 0.9500 . ?
C84 N15 1.30(3) . ?
C84 C85 1.32(3) . ?
C84 H84 0.9500 . ?
C85 C86 1.31(2) . ?
C85 H85 0.9500 . ?
C86 C87 1.31(2) . ?
C86 H86 0.9500 . ?
C87 C88 1.32(2) . ?
C87 H87 0.9500 . ?
C88 N15 1.38(2) . ?
C88 H88 0.9500 . ?
N1 U1 2.463(10) . ?
N2 U1 2.643(10) . ?
N4 H4 0.8800 . ?
N5 H5A 0.8800 . ?
N7 U1 2.635(11) . ?
N8 U1 2.480(9) . ?
N9 U1 2.587(10) . ?
N10 Mg1 2.313(16) . ?
N11 Mg1 2.248(14) . ?
N12 Mg1 2.39(2) . ?
O1 U1 1.820(8) . ?
O2 U1 1.987(8) . ?
O2 Zr1 2.044(8) . ?
Zr1 Cl1 2.431(4) . ?
Cl2 Mg1 2.453(7) . ?
Cl3 Mg1 2.476(7) . ?

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
N1 C1 C2 109.4(11) . . ?
N1 C1 C41 122.3(11) . . ?
C2 C1 C41 128.3(12) . . ?
C3 C2 C1 107.7(12) . . ?
C3 C2 H2 126.2 . . ?
C1 C2 H2 126.2 . . ?
C4 C3 C2 105.6(12) . . ?
C4 C3 H3 127.2 . . ?
C2 C3 H3 127.2 . . ?
N1 C4 C3 110.6(12) . . ?
N1 C4 C5 122.3(12) . . ?
C3 C4 C5 127.0(13) . . ?
N2 C5 C4 119.9(12) . . ?
N2 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C7 C6 C13 121.0(12) . . ?
C7 C6 N2 121.9(12) . . ?
C13 C6 N2 117.1(12) . . ?
C8 C7 C6 121.8(13) . . ?
C8 C7 H7 119.1 . . ?
C6 C7 H7 119.1 . . ?
C7 C8 C10 118.5(12) . . ?
C7 C8 C9 121.8(13) . . ?
C10 C8 C9 119.7(12) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C12 C10 C8 118.9(12) . . ?
C12 C10 C11 121.2(14) . . ?
C8 C10 C11 120.0(12) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 C13 122.4(14) . . ?
C10 C12 H12 118.8 . . ?
C13 C12 H12 118.8 . . ?
C6 C13 C12 117.2(13) . . ?
C6 C13 N3 118.5(12) . . ?
C12 C13 N3 124.3(13) . . ?
N3 C14 C15 120.2(14) . . ?
N3 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
N4 C15 C16 106.9(14) . . ?
N4 C15 C14 123.5(13) . . ?
C16 C15 C14 129.6(16) . . ?
C15 C16 C17 106.9(14) . . ?
C15 C16 H16 126.6 . . ?
C17 C16 H16 126.6 . . ?
C18 C17 C16 106.1(13) . . ?
C18 C17 H17 126.9 . . ?
C16 C17 H17 126.9 . . ?
N4 C18 C17 108.5(14) . . ?
N4 C18 C19 122.7(14) . . ?
C17 C18 C19 128.8(14) . . ?
C22 C19 C20 109.8(14) . . ?
C22 C19 C18 108.1(13) . . ?
C20 C19 C18 110.9(13) . . ?
C22 C19 C21 110.9(13) . . ?
C20 C19 C21 107.8(12) . . ?
C18 C19 C21 109.3(13) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N5 C22 C23 106.1(16) . . ?
N5 C22 C19 122.9(15) . . ?
C23 C22 C19 130.6(15) . . ?
C24 C23 C22 107.8(15) . . ?
C24 C23 H23 126.1 . . ?
C22 C23 H23 126.1 . . ?
C23 C24 C25 109.5(16) . . ?
C23 C24 H24 125.3 . . ?
C25 C24 H24 125.3 . . ?
N5 C25 C24 104.7(15) . . ?
N5 C25 C26 122.8(15) . . ?
C24 C25 C26 132.4(17) . . ?
N6 C26 C25 122.3(15) . . ?
N6 C26 H26 118.9 . . ?
C25 C26 H26 118.9 . . ?
C35 C27 N6 118.7(12) . . ?
C35 C27 C28 116.5(14) . . ?
N6 C27 C28 124.7(13) . . ?
C29 C28 C27 123.3(14) . . ?
C29 C28 H28 118.4 . . ?
C27 C28 H28 118.4 . . ?
C31 C29 C28 118.5(14) . . ?
C31 C29 C30 122.7(16) . . ?
C28 C29 C30 118.6(14) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C34 C31 C29 118.2(15) . . ?
C34 C31 C33 121.5(14) . . ?
C29 C31 C33 120.3(15) . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 C35 123.3(14) . . ?
C31 C34 H34 118.3 . . ?
C35 C34 H34 118.3 . . ?
C34 C35 C27 119.9(13) . . ?
C34 C35 N7 121.9(12) . . ?
C27 C35 N7 118.2(12) . . ?
N7 C36 C37 121.7(14) . . ?
N7 C36 H36 119.1 . . ?
C37 C36 H36 119.1 . . ?
N8 C37 C38 111.4(13) . . ?
N8 C37 C36 118.1(12) . . ?
C38 C37 C36 130.2(14) . . ?
C39 C38 C37 105.3(14) . . ?
C39 C38 H38 127.3 . . ?
C37 C38 H38 127.3 . . ?
C38 C39 C40 109.5(13) . . ?
C38 C39 H39 125.2 . . ?
C40 C39 H39 125.2 . . ?
N8 C40 C39 107.8(13) . . ?
N8 C40 C41 121.6(12) . . ?
C39 C40 C41 130.4(13) . . ?
C40 C41 C1 110.9(11) . . ?
C40 C41 C42 110.8(12) . . ?
C1 C41 C42 110.6(11) . . ?
C40 C41 C43 108.4(12) . . ?
C1 C41 C43 107.0(11) . . ?
C42 C41 C43 109.0(11) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N9 C44 C45 125.2(16) . . ?
N9 C44 H44 117.4 . . ?
C45 C44 H44 117.4 . . ?
C46 C45 C44 117.7(18) . . ?
C46 C45 H45 121.1 . . ?
C44 C45 H45 121.1 . . ?
C45 C46 C47 120.1(19) . . ?
C45 C46 H46 120.0 . . ?
C47 C46 H46 120.0 . . ?
C46 C47 C48 118.2(17) . . ?
C46 C47 H47 120.9 . . ?
C48 C47 H47 120.9 . . ?
N9 C48 C47 123.4(16) . . ?
N9 C48 H48 118.3 . . ?
C47 C48 H48 118.3 . . ?
C50 C49 C53 110.2(16) . . ?
C50 C49 Zr1 75.0(9) . . ?
C53 C49 Zr1 73.3(9) . . ?
C50 C49 H49 124.9 . . ?
C53 C49 H49 124.9 . . ?
Zr1 C49 H49 118.5 . . ?
C49 C50 C51 108.5(16) . . ?
C49 C50 Zr1 73.8(9) . . ?
C51 C50 Zr1 73.8(9) . . ?
C49 C50 H50 125.8 . . ?
C51 C50 H50 125.8 . . ?
Zr1 C50 H50 118.6 . . ?
C52 C51 C50 105.6(15) . . ?
C52 C51 Zr1 72.1(9) . . ?
C50 C51 Zr1 73.6(8) . . ?
C52 C51 H51 127.2 . . ?
C50 C51 H51 127.2 . . ?
Zr1 C51 H51 119.2 . . ?
C51 C52 C53 110.5(16) . . ?
C51 C52 Zr1 76.1(9) . . ?
C53 C52 Zr1 74.3(9) . . ?
C51 C52 H52 124.7 . . ?
C53 C52 H52 124.7 . . ?
Zr1 C52 H52 116.7 . . ?
C49 C53 C52 105.2(16) . . ?
C49 C53 Zr1 74.5(9) . . ?
C52 C53 Zr1 72.9(9) . . ?
C49 C53 H53 127.4 . . ?
C52 C53 H53 127.4 . . ?
Zr1 C53 H53 117.6 . . ?
C58 C54 C55 108.4(14) . . ?
C58 C54 Zr1 72.7(9) . . ?
C55 C54 Zr1 75.4(10) . . ?
C58 C54 H54 125.8 . . ?
C55 C54 H54 125.8 . . ?
Zr1 C54 H54 118.1 . . ?
C56 C55 C54 107.2(14) . . ?
C56 C55 Zr1 74.7(9) . . ?
C54 C55 Zr1 72.6(9) . . ?
C56 C55 H55 126.4 . . ?
C54 C55 H55 126.4 . . ?
Zr1 C55 H55 118.3 . . ?
C57 C56 C55 109.2(14) . . ?
C57 C56 Zr1 73.6(8) . . ?
C55 C56 Zr1 73.6(9) . . ?
C57 C56 H56 125.4 . . ?
C55 C56 H56 125.4 . . ?
Zr1 C56 H56 119.2 . . ?
C56 C57 C58 106.7(13) . . ?
C56 C57 Zr1 74.9(9) . . ?
C58 C57 Zr1 71.2(9) . . ?
C56 C57 H57 126.7 . . ?
C58 C57 H57 126.7 . . ?
Zr1 C57 H57 119.2 . . ?
C54 C58 C57 108.5(13) . . ?
C54 C58 Zr1 75.2(9) . . ?
C57 C58 Zr1 76.3(9) . . ?
C54 C58 H58 125.8 . . ?
C57 C58 H58 125.8 . . ?
Zr1 C58 H58 114.9 . . ?
N10 C59 C60 125(3) . . ?
N10 C59 H59 117.4 . . ?
C60 C59 H59 117.4 . . ?
C59 C60 C61 117(3) . . ?
C59 C60 H60 121.4 . . ?
C61 C60 H60 121.4 . . ?
C60 C61 C62 120(3) . . ?
C60 C61 H61 120.1 . . ?
C62 C61 H61 120.1 . . ?
C63 C62 C61 115(2) . . ?
C63 C62 H62 122.4 . . ?
C61 C62 H62 122.4 . . ?
N10 C63 C62 123(2) . . ?
N10 C63 H63 118.3 . . ?
C62 C63 H63 118.3 . . ?
N11 C64 C65 122.4(15) . . ?
N11 C64 H64 118.8 . . ?
C65 C64 H64 118.8 . . ?
C66 C65 C64 120.4(17) . . ?
C66 C65 H65 119.8 . . ?
C64 C65 H65 119.8 . . ?
C65 C66 C67 119.5(18) . . ?
C65 C66 H66 120.3 . . ?
C67 C66 H66 120.3 . . ?
C66 C67 C68 118.6(17) . . ?
C66 C67 H67 120.7 . . ?
C68 C67 H67 120.7 . . ?
N11 C68 C67 120.5(15) . . ?
N11 C68 H68 119.7 . . ?
C67 C68 H68 119.7 . . ?
N12 C69 C70 112(3) . . ?
N12 C69 H69 124.0 . . ?
C70 C69 H69 124.0 . . ?
C71 C70 C69 109(2) . . ?
C71 C70 H70 125.6 . . ?
C69 C70 H70 125.6 . . ?
C72 C71 C70 126(4) . . ?
C72 C71 H71 117.0 . . ?
C70 C71 H71 117.0 . . ?
C71 C72 C73 130(5) . . ?
C71 C72 H72 115.0 . . ?
C73 C72 H72 115.0 . . ?
C72 C73 N12 107(5) . . ?
C72 C73 H73 126.3 . . ?
N12 C73 H73 126.3 . . ?
C74 N13 C78 120.0 . . ?
C74 N13 Mg1 114.3(11) . . ?
C78 N13 Mg1 125.0(11) . . ?
C75 C74 N13 120.0 . . ?
C75 C74 H74 120.0 . . ?
N13 C74 H74 120.0 . . ?
C74 C75 C76 120.0 . . ?
C74 C75 H75 120.0 . . ?
C76 C75 H75 120.0 . . ?
C77 C76 C75 120.0 . . ?
C77 C76 H76 120.0 . . ?
C75 C76 H76 120.0 . . ?
C78 C77 C76 120.0 . . ?
C78 C77 H77 120.0 . . ?
C76 C77 H77 120.0 . . ?
C77 C78 N13 120.0 . . ?
C77 C78 H78 120.0 . . ?
N13 C78 H78 120.0 . . ?
C80 C79 N14 123(3) . . ?
C80 C79 H79 118.5 . . ?
N14 C79 H79 118.5 . . ?
C79 C80 C81 119(3) . . ?
C79 C80 H80 120.3 . . ?
C81 C80 H80 120.3 . . ?
C80 C81 C82 124(2) . . ?
C80 C81 H81 118.1 . . ?
C82 C81 H81 118.1 . . ?
C83 C82 C81 121(3) . . ?
C83 C82 H82 119.5 . . ?
C81 C82 H82 119.5 . . ?
C82 C83 N14 118(3) . . ?
C82 C83 H83 121.2 . . ?
N14 C83 H83 121.2 . . ?
N15 C84 C85 120.4(19) . . ?
N15 C84 H84 119.8 . . ?
C85 C84 H84 119.8 . . ?
C86 C85 C84 122(2) . . ?
C86 C85 H85 119.1 . . ?
C84 C85 H85 119.1 . . ?
C87 C86 C85 116(2) . . ?
C87 C86 H86 121.8 . . ?
C85 C86 H86 121.8 . . ?
C86 C87 C88 126(2) . . ?
C86 C87 H87 117.1 . . ?
C88 C87 H87 117.1 . . ?
C87 C88 N15 115(2) . . ?
C87 C88 H88 122.7 . . ?
N15 C88 H88 122.7 . . ?
C1 N1 C4 106.7(11) . . ?
C1 N1 U1 137.0(9) . . ?
C4 N1 U1 115.2(8) . . ?
C5 N2 C6 115.0(11) . . ?
C5 N2 U1 112.4(8) . . ?
C6 N2 U1 131.6(8) . . ?
C14 N3 C13 119.0(13) . . ?
C18 N4 C15 111.6(13) . . ?
C18 N4 H4 124.2 . . ?
C15 N4 H4 124.2 . . ?
C22 N5 C25 111.7(14) . . ?
C22 N5 H5A 124.1 . . ?
C25 N5 H5A 124.1 . . ?
C26 N6 C27 119.9(12) . . ?
C36 N7 C35 115.6(12) . . ?
C36 N7 U1 111.1(9) . . ?
C35 N7 U1 131.4(8) . . ?
C37 N8 C40 105.7(11) . . ?
C37 N8 U1 115.3(8) . . ?
C40 N8 U1 136.0(9) . . ?
C48 N9 C44 115.4(13) . . ?
C48 N9 U1 122.0(10) . . ?
C44 N9 U1 122.5(10) . . ?
C59 N10 C63 116.7(19) . . ?
C59 N10 Mg1 120.0(16) . . ?
C63 N10 Mg1 123.2(14) . . ?
C64 N11 C68 118.3(14) . . ?
C64 N11 Mg1 121.5(11) . . ?
C68 N11 Mg1 120.1(11) . . ?
C73 N12 C69 132(4) . . ?
C73 N12 Mg1 114(3) . . ?
C69 N12 Mg1 109(2) . . ?
C83 N14 C79 115(3) . . ?
C84 N15 C88 121(2) . . ?
U1 O2 Zr1 170.9(4) . . ?
O2 Zr1 Cl1 97.1(2) . . ?
O2 Zr1 C58 95.9(4) . . ?
Cl1 Zr1 C58 132.8(3) . . ?
O2 Zr1 C52 135.8(4) . . ?
Cl1 Zr1 C52 103.1(5) . . ?
C58 Zr1 C52 98.3(6) . . ?
O2 Zr1 C53 108.8(5) . . ?
Cl1 Zr1 C53 132.6(4) . . ?
C58 Zr1 C53 84.1(6) . . ?
C52 Zr1 C53 32.9(5) . . ?
O2 Zr1 C54 127.7(4) . . ?
Cl1 Zr1 C54 115.1(4) . . ?
C58 Zr1 C54 32.1(4) . . ?
C52 Zr1 C54 77.4(5) . . ?
C53 Zr1 C54 79.2(6) . . ?
O2 Zr1 C49 83.0(4) . . ?
Cl1 Zr1 C49 120.7(5) . . ?
C58 Zr1 C49 105.8(6) . . ?
C52 Zr1 C49 52.9(5) . . ?
C53 Zr1 C49 32.2(5) . . ?
C54 Zr1 C49 110.3(6) . . ?
O2 Zr1 C50 88.9(4) . . ?
Cl1 Zr1 C50 89.5(4) . . ?
C58 Zr1 C50 135.9(5) . . ?
C52 Zr1 C50 52.9(5) . . ?
C53 Zr1 C50 53.3(6) . . ?
C54 Zr1 C50 128.9(5) . . ?
C49 Zr1 C50 31.3(5) . . ?
O2 Zr1 C51 120.6(5) . . ?
Cl1 Zr1 C51 78.6(4) . . ?
C58 Zr1 C51 130.2(5) . . ?
C52 Zr1 C51 31.9(5) . . ?
C53 Zr1 C51 54.2(6) . . ?
C54 Zr1 C51 106.1(5) . . ?
C49 Zr1 C51 53.2(5) . . ?
C50 Zr1 C51 32.7(5) . . ?
O2 Zr1 C57 79.1(4) . . ?
Cl1 Zr1 C57 107.6(4) . . ?
C58 Zr1 C57 32.5(4) . . ?
C52 Zr1 C57 129.1(5) . . ?
C53 Zr1 C57 115.7(6) . . ?
C54 Zr1 C57 53.1(4) . . ?
C49 Zr1 C57 130.1(5) . . ?
C50 Zr1 C57 160.0(5) . . ?
C51 Zr1 C57 159.2(5) . . ?
O2 Zr1 C55 129.1(5) . . ?
Cl1 Zr1 C55 84.3(4) . . ?
C58 Zr1 C55 53.2(5) . . ?
C52 Zr1 C55 92.1(6) . . ?
C53 Zr1 C55 106.7(6) . . ?
C54 Zr1 C55 32.0(5) . . ?
C49 Zr1 C55 138.9(6) . . ?
C50 Zr1 C55 141.9(5) . . ?
C51 Zr1 C55 109.6(6) . . ?
C57 Zr1 C55 52.9(5) . . ?
O2 Zr1 C56 98.1(4) . . ?
Cl1 Zr1 C56 80.5(4) . . ?
C58 Zr1 C56 52.8(5) . . ?
C52 Zr1 C56 123.6(5) . . ?
C53 Zr1 C56 131.4(6) . . ?
C54 Zr1 C56 52.5(5) . . ?
C49 Zr1 C56 158.6(6) . . ?
C50 Zr1 C56 168.4(5) . . ?
C51 Zr1 C56 137.7(5) . . ?
C57 Zr1 C56 31.6(4) . . ?
C55 Zr1 C56 31.6(4) . . ?
O1 U1 O2 177.4(3) . . ?
O1 U1 N1 93.9(4) . . ?
O2 U1 N1 88.4(3) . . ?
O1 U1 N8 95.4(3) . . ?
O2 U1 N8 86.4(3) . . ?
N1 U1 N8 70.6(4) . . ?
O1 U1 N9 89.6(4) . . ?
O2 U1 N9 87.9(4) . . ?
N1 U1 N9 142.0(3) . . ?
N8 U1 N9 146.7(4) . . ?
O1 U1 N7 98.0(4) . . ?
O2 U1 N7 81.1(3) . . ?
N1 U1 N7 135.6(4) . . ?
N8 U1 N7 65.8(4) . . ?
N9 U1 N7 80.9(3) . . ?
O1 U1 N2 96.5(3) . . ?
O2 U1 N2 83.3(3) . . ?
N1 U1 N2 67.0(3) . . ?
N8 U1 N2 136.6(3) . . ?
N9 U1 N2 75.0(3) . . ?
N7 U1 N2 151.6(3) . . ?
N13 Mg1 N11 175.0(7) . . ?
N13 Mg1 N10 85.7(7) . . ?
N11 Mg1 N10 89.3(5) . . ?
N13 Mg1 N12 96.9(8) . . ?
N11 Mg1 N12 88.2(6) . . ?
N10 Mg1 N12 176.0(8) . . ?
N13 Mg1 Cl2 88.1(5) . . ?
N11 Mg1 Cl2 91.9(4) . . ?
N10 Mg1 Cl2 90.5(5) . . ?
N12 Mg1 Cl2 86.5(6) . . ?
N13 Mg1 Cl3 88.9(5) . . ?
N11 Mg1 Cl3 91.2(4) . . ?
N10 Mg1 Cl3 89.9(5) . . ?
N12 Mg1 Cl3 93.3(6) . . ?
Cl2 Mg1 Cl3 176.9(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
N1 C1 C2 C3 -0.2(17) . . . . ?
C41 C1 C2 C3 -177.0(13) . . . . ?
C1 C2 C3 C4 1.4(17) . . . . ?
C2 C3 C4 N1 -2.1(16) . . . . ?
C2 C3 C4 C5 174.7(13) . . . . ?
N1 C4 C5 N2 0(2) . . . . ?
C3 C4 C5 N2 -176.7(13) . . . . ?
C13 C6 C7 C8 1(2) . . . . ?
N2 C6 C7 C8 -177.7(12) . . . . ?
C6 C7 C8 C10 -4(2) . . . . ?
C6 C7 C8 C9 178.0(13) . . . . ?
C7 C8 C10 C12 4(2) . . . . ?
C9 C8 C10 C12 -178.1(14) . . . . ?
C7 C8 C10 C11 -178.0(14) . . . . ?
C9 C8 C10 C11 0(2) . . . . ?
C8 C10 C12 C13 0(2) . . . . ?
C11 C10 C12 C13 -178.3(14) . . . . ?
C7 C6 C13 C12 3(2) . . . . ?
N2 C6 C13 C12 -178.5(12) . . . . ?
C7 C6 C13 N3 -178.2(12) . . . . ?
N2 C6 C13 N3 0(2) . . . . ?
C10 C12 C13 C6 -3(2) . . . . ?
C10 C12 C13 N3 178.2(14) . . . . ?
N3 C14 C15 N4 -2(2) . . . . ?
N3 C14 C15 C16 178.5(16) . . . . ?
N4 C15 C16 C17 -0.3(18) . . . . ?
C14 C15 C16 C17 179.3(15) . . . . ?
C15 C16 C17 C18 -0.3(18) . . . . ?
C16 C17 C18 N4 0.7(17) . . . . ?
C16 C17 C18 C19 -179.7(15) . . . . ?
N4 C18 C19 C22 -63.9(18) . . . . ?
C17 C18 C19 C22 116.6(17) . . . . ?
N4 C18 C19 C20 56.6(19) . . . . ?
C17 C18 C19 C20 -123.0(17) . . . . ?
N4 C18 C19 C21 175.3(13) . . . . ?
C17 C18 C19 C21 -4(2) . . . . ?
C20 C19 C22 N5 -52.6(19) . . . . ?
C18 C19 C22 N5 68.5(18) . . . . ?
C21 C19 C22 N5 -171.7(13) . . . . ?
C20 C19 C22 C23 135.8(17) . . . . ?
C18 C19 C22 C23 -103.1(19) . . . . ?
C21 C19 C22 C23 17(2) . . . . ?
N5 C22 C23 C24 4.7(19) . . . . ?
C19 C22 C23 C24 177.4(16) . . . . ?
C22 C23 C24 C25 -5(2) . . . . ?
C23 C24 C25 N5 3.6(19) . . . . ?
C23 C24 C25 C26 179.4(16) . . . . ?
N5 C25 C26 N6 -3(2) . . . . ?
C24 C25 C26 N6 -178.5(15) . . . . ?
C35 C27 C28 C29 3(2) . . . . ?
N6 C27 C28 C29 -175.6(13) . . . . ?
C27 C28 C29 C31 0(2) . . . . ?
C27 C28 C29 C30 176.5(13) . . . . ?
C28 C29 C31 C34 -4(2) . . . . ?
C30 C29 C31 C34 -179.9(13) . . . . ?
C28 C29 C31 C33 176.3(13) . . . . ?
C30 C29 C31 C33 0(2) . . . . ?
C29 C31 C34 C35 4(2) . . . . ?
C33 C31 C34 C35 -175.6(13) . . . . ?
C31 C34 C35 C27 -1(2) . . . . ?
C31 C34 C35 N7 177.1(12) . . . . ?
N6 C27 C35 C34 176.3(12) . . . . ?
C28 C27 C35 C34 -2(2) . . . . ?
N6 C27 C35 N7 -2.1(19) . . . . ?
C28 C27 C35 N7 179.3(11) . . . . ?
N7 C36 C37 N8 0(2) . . . . ?
N7 C36 C37 C38 173.3(15) . . . . ?
N8 C37 C38 C39 -1.0(17) . . . . ?
C36 C37 C38 C39 -174.7(14) . . . . ?
C37 C38 C39 C40 2.7(17) . . . . ?
C38 C39 C40 N8 -3.4(16) . . . . ?
C38 C39 C40 C41 -179.5(14) . . . . ?
N8 C40 C41 C1 -52.0(17) . . . . ?
C39 C40 C41 C1 123.6(15) . . . . ?
N8 C40 C41 C42 -175.3(11) . . . . ?
C39 C40 C41 C42 0(2) . . . . ?
N8 C40 C41 C43 65.1(15) . . . . ?
C39 C40 C41 C43 -119.2(15) . . . . ?
N1 C1 C41 C40 50.5(18) . . . . ?
C2 C1 C41 C40 -133.0(15) . . . . ?
N1 C1 C41 C42 173.9(12) . . . . ?
C2 C1 C41 C42 -10(2) . . . . ?
N1 C1 C41 C43 -67.4(16) . . . . ?
C2 C1 C41 C43 109.1(17) . . . . ?
N9 C44 C45 C46 -2(3) . . . . ?
C44 C45 C46 C47 2(4) . . . . ?
C45 C46 C47 C48 -1(3) . . . . ?
C46 C47 C48 N9 -2(3) . . . . ?
C53 C49 C50 C51 -0.7(18) . . . . ?
Zr1 C49 C50 C51 -66.2(11) . . . . ?
C53 C49 C50 Zr1 65.4(11) . . . . ?
C49 C50 C51 C52 0.7(18) . . . . ?
Zr1 C50 C51 C52 -65.4(11) . . . . ?
C49 C50 C51 Zr1 66.2(11) . . . . ?
C50 C51 C52 C53 -0.5(18) . . . . ?
Zr1 C51 C52 C53 -67.0(11) . . . . ?
C50 C51 C52 Zr1 66.5(10) . . . . ?
C50 C49 C53 C52 0.4(17) . . . . ?
Zr1 C49 C53 C52 66.9(10) . . . . ?
C50 C49 C53 Zr1 -66.5(11) . . . . ?
C51 C52 C53 C49 0.1(18) . . . . ?
Zr1 C52 C53 C49 -68.1(10) . . . . ?
C51 C52 C53 Zr1 68.1(11) . . . . ?
C58 C54 C55 C56 -1.6(19) . . . . ?
Zr1 C54 C55 C56 -67.3(12) . . . . ?
C58 C54 C55 Zr1 65.7(11) . . . . ?
C54 C55 C56 C57 0.4(19) . . . . ?
Zr1 C55 C56 C57 -65.5(11) . . . . ?
C54 C55 C56 Zr1 65.9(11) . . . . ?
C55 C56 C57 C58 1.0(18) . . . . ?
Zr1 C56 C57 C58 -64.6(10) . . . . ?
C55 C56 C57 Zr1 65.6(11) . . . . ?
C55 C54 C58 C57 2.2(18) . . . . ?
Zr1 C54 C58 C57 69.7(11) . . . . ?
C55 C54 C58 Zr1 -67.5(11) . . . . ?
C56 C57 C58 C54 -2.0(17) . . . . ?
Zr1 C57 C58 C54 -69.0(11) . . . . ?
C56 C57 C58 Zr1 67.1(11) . . . . ?
N10 C59 C60 C61 -16(6) . . . . ?
C59 C60 C61 C62 19(6) . . . . ?
C60 C61 C62 C63 -13(5) . . . . ?
C61 C62 C63 N10 3(3) . . . . ?
N11 C64 C65 C66 6(3) . . . . ?
C64 C65 C66 C67 -6(3) . . . . ?
C65 C66 C67 C68 3(3) . . . . ?
C66 C67 C68 N11 1(3) . . . . ?
N12 C69 C70 C71 -7(3) . . . . ?
C69 C70 C71 C72 -7(5) . . . . ?
C70 C71 C72 C73 12(7) . . . . ?
C71 C72 C73 N12 0(7) . . . . ?
C78 N13 C74 C75 0.0 . . . . ?
Mg1 N13 C74 C75 171.2(12) . . . . ?
N13 C74 C75 C76 0.0 . . . . ?
C74 C75 C76 C77 0.0 . . . . ?
C75 C76 C77 C78 0.0 . . . . ?
C76 C77 C78 N13 0.0 . . . . ?
C74 N13 C78 C77 0.0 . . . . ?
Mg1 N13 C78 C77 -170.2(14) . . . . ?
N14 C79 C80 C81 -2(5) . . . . ?
C79 C80 C81 C82 0(4) . . . . ?
C80 C81 C82 C83 4(4) . . . . ?
C81 C82 C83 N14 -4(4) . . . . ?
N15 C84 C85 C86 6(4) . . . . ?
C84 C85 C86 C87 -7(3) . . . . ?
C85 C86 C87 C88 6(4) . . . . ?
C86 C87 C88 N15 -3(4) . . . . ?
C2 C1 N1 C4 -1.1(15) . . . . ?
C41 C1 N1 C4 176.0(12) . . . . ?
C2 C1 N1 U1 166.0(10) . . . . ?
C41 C1 N1 U1 -17(2) . . . . ?
C3 C4 N1 C1 2.0(15) . . . . ?
C5 C4 N1 C1 -175.0(12) . . . . ?
C3 C4 N1 U1 -168.3(9) . . . . ?
C5 C4 N1 U1 14.7(16) . . . . ?
C4 C5 N2 C6 176.8(11) . . . . ?
C4 C5 N2 U1 -13.0(15) . . . . ?
C7 C6 N2 C5 55.5(18) . . . . ?
C13 C6 N2 C5 -123.0(14) . . . . ?
C7 C6 N2 U1 -112.3(13) . . . . ?
C13 C6 N2 U1 69.2(16) . . . . ?
C15 C14 N3 C13 -176.0(12) . . . . ?
C6 C13 N3 C14 141.0(14) . . . . ?
C12 C13 N3 C14 -40(2) . . . . ?
C17 C18 N4 C15 -0.9(18) . . . . ?
C19 C18 N4 C15 179.4(14) . . . . ?
C16 C15 N4 C18 0.7(18) . . . . ?
C14 C15 N4 C18 -178.8(13) . . . . ?
C23 C22 N5 C25 -2.6(18) . . . . ?
C19 C22 N5 C25 -175.9(14) . . . . ?
C24 C25 N5 C22 -0.6(18) . . . . ?
C26 C25 N5 C22 -176.9(13) . . . . ?
C25 C26 N6 C27 -179.7(13) . . . . ?
C35 C27 N6 C26 -149.6(13) . . . . ?
C28 C27 N6 C26 29(2) . . . . ?
C37 C36 N7 C35 -173.0(12) . . . . ?
C37 C36 N7 U1 20.8(16) . . . . ?
C34 C35 N7 C36 -44.2(17) . . . . ?
C27 C35 N7 C36 134.1(14) . . . . ?
C34 C35 N7 U1 118.5(13) . . . . ?
C27 C35 N7 U1 -63.2(16) . . . . ?
C38 C37 N8 C40 -1.0(16) . . . . ?
C36 C37 N8 C40 173.6(11) . . . . ?
C38 C37 N8 U1 162.6(9) . . . . ?
C36 C37 N8 U1 -22.9(15) . . . . ?
C39 C40 N8 C37 2.6(14) . . . . ?
C41 C40 N8 C37 179.1(12) . . . . ?
C39 C40 N8 U1 -155.8(10) . . . . ?
C41 C40 N8 U1 20.7(19) . . . . ?
C47 C48 N9 C44 2(2) . . . . ?
C47 C48 N9 U1 179.7(12) . . . . ?
C45 C44 N9 C48 0(2) . . . . ?
C45 C44 N9 U1 -177.9(14) . . . . ?
C60 C59 N10 C63 6(5) . . . . ?
C60 C59 N10 Mg1 -171(3) . . . . ?
C62 C63 N10 C59 1(3) . . . . ?
C62 C63 N10 Mg1 177.5(15) . . . . ?
C65 C64 N11 C68 -2(2) . . . . ?
C65 C64 N11 Mg1 176.9(12) . . . . ?
C67 C68 N11 C64 -1(2) . . . . ?
C67 C68 N11 Mg1 -179.9(13) . . . . ?
C72 C73 N12 C69 -18(6) . . . . ?
C72 C73 N12 Mg1 -173(2) . . . . ?
C70 C69 N12 C73 21(5) . . . . ?
C70 C69 N12 Mg1 177.9(15) . . . . ?
C82 C83 N14 C79 2(4) . . . . ?
C80 C79 N14 C83 1(5) . . . . ?
C85 C84 N15 C88 -3(4) . . . . ?
C87 C88 N15 C84 1(3) . . . . ?
U1 O2 Zr1 Cl1 -99(3) . . . . ?
U1 O2 Zr1 C58 126(3) . . . . ?
U1 O2 Zr1 C52 18(3) . . . . ?
U1 O2 Zr1 C53 41(3) . . . . ?
U1 O2 Zr1 C54 131(3) . . . . ?
U1 O2 Zr1 C49 21(3) . . . . ?
U1 O2 Zr1 C50 -10(3) . . . . ?
U1 O2 Zr1 C51 -18(3) . . . . ?
U1 O2 Zr1 C57 154(3) . . . . ?
U1 O2 Zr1 C55 173(3) . . . . ?
U1 O2 Zr1 C56 180(100) . . . . ?
C54 C58 Zr1 O2 172.5(9) . . . . ?
C57 C58 Zr1 O2 58.9(8) . . . . ?
C54 C58 Zr1 Cl1 67.2(11) . . . . ?
C57 C58 Zr1 Cl1 -46.5(10) . . . . ?
C54 C58 Zr1 C52 -49.5(10) . . . . ?
C57 C58 Zr1 C52 -163.1(8) . . . . ?
C54 C58 Zr1 C53 -79.1(10) . . . . ?
C57 C58 Zr1 C53 167.2(9) . . . . ?
C57 C58 Zr1 C54 -113.7(12) . . . . ?
C54 C58 Zr1 C49 -103.1(10) . . . . ?
C57 C58 Zr1 C49 143.2(8) . . . . ?
C54 C58 Zr1 C50 -92.9(11) . . . . ?
C57 C58 Zr1 C50 153.4(8) . . . . ?
C54 C58 Zr1 C51 -48.3(12) . . . . ?
C57 C58 Zr1 C51 -162.0(8) . . . . ?
C54 C58 Zr1 C57 113.7(12) . . . . ?
C54 C58 Zr1 C55 36.9(9) . . . . ?
C57 C58 Zr1 C55 -76.8(9) . . . . ?
C54 C58 Zr1 C56 76.8(9) . . . . ?
C57 C58 Zr1 C56 -36.9(7) . . . . ?
C51 C52 Zr1 O2 -74.2(13) . . . . ?
C53 C52 Zr1 O2 42.2(15) . . . . ?
C51 C52 Zr1 Cl1 40.7(11) . . . . ?
C53 C52 Zr1 Cl1 157.1(11) . . . . ?
C51 C52 Zr1 C58 178.4(11) . . . . ?
C53 C52 Zr1 C58 -65.2(12) . . . . ?
C51 C52 Zr1 C53 -116.5(16) . . . . ?
C51 C52 Zr1 C54 153.9(12) . . . . ?
C53 C52 Zr1 C54 -89.6(12) . . . . ?
C51 C52 Zr1 C49 -78.1(11) . . . . ?
C53 C52 Zr1 C49 38.4(10) . . . . ?
C51 C52 Zr1 C50 -38.6(10) . . . . ?
C53 C52 Zr1 C50 77.9(11) . . . . ?
C53 C52 Zr1 C51 116.5(16) . . . . ?
C51 C52 Zr1 C57 166.8(10) . . . . ?
C53 C52 Zr1 C57 -76.8(12) . . . . ?
C51 C52 Zr1 C55 125.3(11) . . . . ?
C53 C52 Zr1 C55 -118.2(12) . . . . ?
C51 C52 Zr1 C56 127.9(10) . . . . ?
C53 C52 Zr1 C56 -115.7(11) . . . . ?
C49 C53 Zr1 O2 -38.6(11) . . . . ?
C52 C53 Zr1 O2 -150.3(10) . . . . ?
C49 C53 Zr1 Cl1 80.8(12) . . . . ?
C52 C53 Zr1 Cl1 -30.9(14) . . . . ?
C49 C53 Zr1 C58 -132.8(11) . . . . ?
C52 C53 Zr1 C58 115.5(12) . . . . ?
C49 C53 Zr1 C52 111.7(16) . . . . ?
C49 C53 Zr1 C54 -164.9(11) . . . . ?
C52 C53 Zr1 C54 83.4(12) . . . . ?
C52 C53 Zr1 C49 -111.7(16) . . . . ?
C49 C53 Zr1 C50 35.2(9) . . . . ?
C52 C53 Zr1 C50 -76.5(11) . . . . ?
C49 C53 Zr1 C51 76.1(11) . . . . ?
C52 C53 Zr1 C51 -35.7(10) . . . . ?
C49 C53 Zr1 C57 -125.2(10) . . . . ?
C52 C53 Zr1 C57 123.1(11) . . . . ?
C49 C53 Zr1 C55 178.5(10) . . . . ?
C52 C53 Zr1 C55 66.8(12) . . . . ?
C49 C53 Zr1 C56 -158.5(10) . . . . ?
C52 C53 Zr1 C56 89.8(12) . . . . ?
C58 C54 Zr1 O2 -9.4(12) . . . . ?
C55 C54 Zr1 O2 105.6(10) . . . . ?
C58 C54 Zr1 Cl1 -131.7(8) . . . . ?
C55 C54 Zr1 Cl1 -16.7(10) . . . . ?
C55 C54 Zr1 C58 115.0(14) . . . . ?
C58 C54 Zr1 C52 129.6(10) . . . . ?
C55 C54 Zr1 C52 -115.4(10) . . . . ?
C58 C54 Zr1 C53 96.1(10) . . . . ?
C55 C54 Zr1 C53 -148.9(10) . . . . ?
C58 C54 Zr1 C49 87.5(10) . . . . ?
C55 C54 Zr1 C49 -157.4(9) . . . . ?
C58 C54 Zr1 C50 116.8(10) . . . . ?
C55 C54 Zr1 C50 -128.2(10) . . . . ?
C58 C54 Zr1 C51 143.6(9) . . . . ?
C55 C54 Zr1 C51 -101.4(10) . . . . ?
C58 C54 Zr1 C57 -38.0(8) . . . . ?
C55 C54 Zr1 C57 77.1(10) . . . . ?
C58 C54 Zr1 C55 -115.0(14) . . . . ?
C58 C54 Zr1 C56 -77.9(9) . . . . ?
C55 C54 Zr1 C56 37.1(9) . . . . ?
C50 C49 Zr1 O2 -99.5(10) . . . . ?
C53 C49 Zr1 O2 143.5(11) . . . . ?
C50 C49 Zr1 Cl1 -5.4(11) . . . . ?
C53 C49 Zr1 Cl1 -122.4(10) . . . . ?
C50 C49 Zr1 C58 166.3(10) . . . . ?
C53 C49 Zr1 C58 49.3(11) . . . . ?
C50 C49 Zr1 C52 77.7(11) . . . . ?
C53 C49 Zr1 C52 -39.2(10) . . . . ?
C50 C49 Zr1 C53 117.0(15) . . . . ?
C50 C49 Zr1 C54 132.8(10) . . . . ?
C53 C49 Zr1 C54 15.9(12) . . . . ?
C53 C49 Zr1 C50 -117.0(15) . . . . ?
C50 C49 Zr1 C51 37.5(9) . . . . ?
C53 C49 Zr1 C51 -79.4(11) . . . . ?
C50 C49 Zr1 C57 -168.8(9) . . . . ?
C53 C49 Zr1 C57 74.2(12) . . . . ?
C50 C49 Zr1 C55 114.8(12) . . . . ?
C53 C49 Zr1 C55 -2.2(15) . . . . ?
C50 C49 Zr1 C56 166.1(12) . . . . ?
C53 C49 Zr1 C56 49.1(19) . . . . ?
C49 C50 Zr1 O2 78.2(10) . . . . ?
C51 C50 Zr1 O2 -166.4(10) . . . . ?
C49 C50 Zr1 Cl1 175.3(10) . . . . ?
C51 C50 Zr1 Cl1 -69.3(10) . . . . ?
C49 C50 Zr1 C58 -19.1(13) . . . . ?
C51 C50 Zr1 C58 96.3(12) . . . . ?
C49 C50 Zr1 C52 -77.8(11) . . . . ?
C51 C50 Zr1 C52 37.6(10) . . . . ?
C49 C50 Zr1 C53 -36.3(9) . . . . ?
C51 C50 Zr1 C53 79.0(11) . . . . ?
C49 C50 Zr1 C54 -62.1(12) . . . . ?
C51 C50 Zr1 C54 53.3(13) . . . . ?
C51 C50 Zr1 C49 115.4(15) . . . . ?
C49 C50 Zr1 C51 -115.4(15) . . . . ?
C49 C50 Zr1 C57 26(2) . . . . ?
C51 C50 Zr1 C57 141.1(14) . . . . ?
C49 C50 Zr1 C55 -104.6(12) . . . . ?
C51 C50 Zr1 C55 10.8(16) . . . . ?
C49 C50 Zr1 C56 -154(2) . . . . ?
C51 C50 Zr1 C56 -39(3) . . . . ?
C52 C51 Zr1 O2 128.8(10) . . . . ?
C50 C51 Zr1 O2 15.8(12) . . . . ?
C52 C51 Zr1 Cl1 -139.6(11) . . . . ?
C50 C51 Zr1 Cl1 107.4(10) . . . . ?
C52 C51 Zr1 C58 -2.1(14) . . . . ?
C50 C51 Zr1 C58 -115.1(11) . . . . ?
C50 C51 Zr1 C52 -113.0(15) . . . . ?
C52 C51 Zr1 C53 36.8(10) . . . . ?
C50 C51 Zr1 C53 -76.1(11) . . . . ?
C52 C51 Zr1 C54 -26.5(12) . . . . ?
C50 C51 Zr1 C54 -139.5(10) . . . . ?
C52 C51 Zr1 C49 77.1(11) . . . . ?
C50 C51 Zr1 C49 -35.9(9) . . . . ?
C52 C51 Zr1 C50 113.0(15) . . . . ?
C52 C51 Zr1 C57 -30(2) . . . . ?
C50 C51 Zr1 C57 -143.0(14) . . . . ?
C52 C51 Zr1 C55 -60.0(12) . . . . ?
C50 C51 Zr1 C55 -172.9(10) . . . . ?
C52 C51 Zr1 C56 -77.8(13) . . . . ?
C50 C51 Zr1 C56 169.2(9) . . . . ?
C56 C57 Zr1 O2 126.2(9) . . . . ?
C58 C57 Zr1 O2 -119.9(8) . . . . ?
C56 C57 Zr1 Cl1 32.1(9) . . . . ?
C58 C57 Zr1 Cl1 146.1(8) . . . . ?
C56 C57 Zr1 C58 -113.9(12) . . . . ?
C56 C57 Zr1 C52 -92.2(11) . . . . ?
C58 C57 Zr1 C52 21.7(11) . . . . ?
C56 C57 Zr1 C53 -128.1(10) . . . . ?
C58 C57 Zr1 C53 -14.2(10) . . . . ?
C56 C57 Zr1 C54 -76.5(9) . . . . ?
C58 C57 Zr1 C54 37.5(8) . . . . ?
C56 C57 Zr1 C49 -162.8(9) . . . . ?
C58 C57 Zr1 C49 -48.9(10) . . . . ?
C56 C57 Zr1 C50 -180(54) . . . . ?
C58 C57 Zr1 C50 -66.0(17) . . . . ?
C56 C57 Zr1 C51 -72.3(18) . . . . ?
C58 C57 Zr1 C51 41.6(18) . . . . ?
C56 C57 Zr1 C55 -36.1(9) . . . . ?
C58 C57 Zr1 C55 77.8(9) . . . . ?
C58 C57 Zr1 C56 113.9(12) . . . . ?
C56 C55 Zr1 O2 13.4(12) . . . . ?
C54 C55 Zr1 O2 -100.6(10) . . . . ?
C56 C55 Zr1 Cl1 -81.1(9) . . . . ?
C54 C55 Zr1 Cl1 164.9(9) . . . . ?
C56 C55 Zr1 C58 77.1(10) . . . . ?
C54 C55 Zr1 C58 -37.0(8) . . . . ?
C56 C55 Zr1 C52 175.9(10) . . . . ?
C54 C55 Zr1 C52 61.9(10) . . . . ?
C56 C55 Zr1 C53 146.0(10) . . . . ?
C54 C55 Zr1 C53 32.0(11) . . . . ?
C56 C55 Zr1 C54 114.0(14) . . . . ?
C56 C55 Zr1 C49 147.2(10) . . . . ?
C54 C55 Zr1 C49 33.2(13) . . . . ?
C56 C55 Zr1 C50 -163.0(10) . . . . ?
C54 C55 Zr1 C50 83.0(12) . . . . ?
C56 C55 Zr1 C51 -156.8(9) . . . . ?
C54 C55 Zr1 C51 89.1(10) . . . . ?
C56 C55 Zr1 C57 36.0(9) . . . . ?
C54 C55 Zr1 C57 -78.0(9) . . . . ?
C54 C55 Zr1 C56 -114.0(14) . . . . ?
C57 C56 Zr1 O2 -53.2(9) . . . . ?
C55 C56 Zr1 O2 -169.5(10) . . . . ?
C57 C56 Zr1 Cl1 -149.1(9) . . . . ?
C55 C56 Zr1 Cl1 94.6(10) . . . . ?
C57 C56 Zr1 C58 38.1(8) . . . . ?
C55 C56 Zr1 C58 -78.3(10) . . . . ?
C57 C56 Zr1 C52 111.5(10) . . . . ?
C55 C56 Zr1 C52 -4.9(12) . . . . ?
C57 C56 Zr1 C53 70.8(11) . . . . ?
C55 C56 Zr1 C53 -45.5(13) . . . . ?
C57 C56 Zr1 C54 78.8(9) . . . . ?
C55 C56 Zr1 C54 -37.6(9) . . . . ?
C57 C56 Zr1 C49 38.4(18) . . . . ?
C55 C56 Zr1 C49 -78.0(17) . . . . ?
C57 C56 Zr1 C50 180(100) . . . . ?
C55 C56 Zr1 C50 64(3) . . . . ?
C57 C56 Zr1 C51 149.8(9) . . . . ?
C55 C56 Zr1 C51 33.4(13) . . . . ?
C55 C56 Zr1 C57 -116.4(14) . . . . ?
C57 C56 Zr1 C55 116.4(14) . . . . ?
Zr1 O2 U1 O1 176(100) . . . . ?
Zr1 O2 U1 N1 23(3) . . . . ?
Zr1 O2 U1 N8 -48(3) . . . . ?
Zr1 O2 U1 N9 165(3) . . . . ?
Zr1 O2 U1 N7 -114(3) . . . . ?
Zr1 O2 U1 N2 90(3) . . . . ?
C1 N1 U1 O1 84.0(13) . . . . ?
C4 N1 U1 O1 -109.7(9) . . . . ?
C1 N1 U1 O2 -97.2(12) . . . . ?
C4 N1 U1 O2 69.2(9) . . . . ?
C1 N1 U1 N8 -10.4(12) . . . . ?
C4 N1 U1 N8 156.0(10) . . . . ?
C1 N1 U1 N9 178.3(11) . . . . ?
C4 N1 U1 N9 -15.3(12) . . . . ?
C1 N1 U1 N7 -21.6(14) . . . . ?
C4 N1 U1 N7 144.8(8) . . . . ?
C1 N1 U1 N2 179.4(13) . . . . ?
C4 N1 U1 N2 -14.2(8) . . . . ?
C37 N8 U1 O1 119.2(9) . . . . ?
C40 N8 U1 O1 -83.8(12) . . . . ?
C37 N8 U1 O2 -59.0(9) . . . . ?
C40 N8 U1 O2 97.9(12) . . . . ?
C37 N8 U1 N1 -148.6(10) . . . . ?
C40 N8 U1 N1 8.4(12) . . . . ?
C37 N8 U1 N9 21.6(13) . . . . ?
C40 N8 U1 N9 178.6(11) . . . . ?
C37 N8 U1 N7 22.9(9) . . . . ?
C40 N8 U1 N7 179.8(13) . . . . ?
C37 N8 U1 N2 -135.3(9) . . . . ?
C40 N8 U1 N2 21.6(14) . . . . ?
C48 N9 U1 O1 -10.0(11) . . . . ?
C44 N9 U1 O1 167.6(11) . . . . ?
C48 N9 U1 O2 169.5(11) . . . . ?
C44 N9 U1 O2 -12.9(11) . . . . ?
C48 N9 U1 N1 -105.9(11) . . . . ?
C44 N9 U1 N1 71.8(13) . . . . ?
C48 N9 U1 N8 89.2(12) . . . . ?
C44 N9 U1 N8 -93.1(12) . . . . ?
C48 N9 U1 N7 88.1(11) . . . . ?
C44 N9 U1 N7 -94.3(11) . . . . ?
C48 N9 U1 N2 -106.9(11) . . . . ?
C44 N9 U1 N2 70.7(11) . . . . ?
C36 N7 U1 O1 -114.7(9) . . . . ?
C35 N7 U1 O1 82.0(11) . . . . ?
C36 N7 U1 O2 67.7(9) . . . . ?
C35 N7 U1 O2 -95.6(11) . . . . ?
C36 N7 U1 N1 -10.8(11) . . . . ?
C35 N7 U1 N1 -174.1(10) . . . . ?
C36 N7 U1 N8 -22.4(9) . . . . ?
C35 N7 U1 N8 174.3(12) . . . . ?
C36 N7 U1 N9 157.0(10) . . . . ?
C35 N7 U1 N9 -6.4(11) . . . . ?
C36 N7 U1 N2 125.1(10) . . . . ?
C35 N7 U1 N2 -38.2(15) . . . . ?
C5 N2 U1 O1 105.7(9) . . . . ?
C6 N2 U1 O1 -86.2(11) . . . . ?
C5 N2 U1 O2 -76.8(9) . . . . ?
C6 N2 U1 O2 91.2(11) . . . . ?
C5 N2 U1 N1 14.3(9) . . . . ?
C6 N2 U1 N1 -177.7(12) . . . . ?
C5 N2 U1 N8 0.7(11) . . . . ?
C6 N2 U1 N8 168.7(10) . . . . ?
C5 N2 U1 N9 -166.4(10) . . . . ?
C6 N2 U1 N9 1.6(11) . . . . ?
C5 N2 U1 N7 -133.8(9) . . . . ?
C6 N2 U1 N7 34.2(15) . . . . ?
C74 N13 Mg1 N11 -31(8) . . . . ?
C78 N13 Mg1 N11 140(7) . . . . ?
C74 N13 Mg1 N10 -30.4(10) . . . . ?
C78 N13 Mg1 N10 140.3(11) . . . . ?
C74 N13 Mg1 N12 152.8(11) . . . . ?
C78 N13 Mg1 N12 -36.6(12) . . . . ?
C74 N13 Mg1 Cl2 -121.0(10) . . . . ?
C78 N13 Mg1 Cl2 49.7(11) . . . . ?
C74 N13 Mg1 Cl3 59.6(10) . . . . ?
C78 N13 Mg1 Cl3 -129.7(11) . . . . ?
C64 N11 Mg1 N13 117(7) . . . . ?
C68 N11 Mg1 N13 -65(8) . . . . ?
C64 N11 Mg1 N10 116.0(13) . . . . ?
C68 N11 Mg1 N10 -65.3(13) . . . . ?
C64 N11 Mg1 N12 -67.2(14) . . . . ?
C68 N11 Mg1 N12 111.6(14) . . . . ?
C64 N11 Mg1 Cl2 -153.6(12) . . . . ?
C68 N11 Mg1 Cl2 25.2(13) . . . . ?
C64 N11 Mg1 Cl3 26.1(13) . . . . ?
C68 N11 Mg1 Cl3 -155.2(12) . . . . ?
C59 N10 Mg1 N13 115(2) . . . . ?
C63 N10 Mg1 N13 -62.1(16) . . . . ?
C59 N10 Mg1 N11 -66(2) . . . . ?
C63 N10 Mg1 N11 117.9(15) . . . . ?
C59 N10 Mg1 N12 -117(9) . . . . ?
C63 N10 Mg1 N12 66(10) . . . . ?
C59 N10 Mg1 Cl2 -157.4(19) . . . . ?
C63 N10 Mg1 Cl2 26.0(15) . . . . ?
C59 N10 Mg1 Cl3 26(2) . . . . ?
C63 N10 Mg1 Cl3 -150.9(15) . . . . ?
C73 N12 Mg1 N13 105(3) . . . . ?
C69 N12 Mg1 N13 -56.0(15) . . . . ?
C73 N12 Mg1 N11 -74(3) . . . . ?
C69 N12 Mg1 N11 124.3(14) . . . . ?
C73 N12 Mg1 N10 -23(11) . . . . ?
C69 N12 Mg1 N10 176(100) . . . . ?
C73 N12 Mg1 Cl2 18(3) . . . . ?
C69 N12 Mg1 Cl2 -143.7(14) . . . . ?
C73 N12 Mg1 Cl3 -166(3) . . . . ?
C69 N12 Mg1 Cl3 33.3(14) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.71
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.337
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.167


_vrf_PLAT411_exp_1443mcref       
;
PROBLEM: Short Inter H...H Contact H74 
.. H75 .. 1.25 Ang.
RESPONSE: The pyridine ligand N13-C74...C78 on the 
MgCl2 had to be refined using idealised coordinates 
causing H74 of one ligand to come into close proximity with H75
of another ligand in the packing on which no further modelling 
was undertaken hence the Alert.
;

_vrf_PLAT412_exp_1443mcref       
;
PROBLEM:  Short Intra XH3 .. XHn 
H9A .. H11A .. 1.63 Ang.
RESPONSE: The methyl groups on the phenyl ring of
the ligand were placed geometrically. This 
resulted in an eclipsed confirmation and a short 
intramolecular H..H contact for two adjacent 
methyl-H atoms on which no further modelling 
was undertaken, hence the Alert.
;

_vrf_PLATA01_exp_1443mcref       
;
PROBLEM: The value of Rint is greater than 0.18
Rint given   0.199
RESPONSE: The crystal used for this experiment was very weakly diffracting, 
resulting in a large proportion of essentially "unobserved" 
reflections being used in the refinement, hence the Alert.
;

_vrf_PLAT020_exp_1443mcref       
;
PROBLEM: The value of Rint is greater than 0.12 
......... 0.199 Report
RESPONSE:
The crystal used for this experiment was very weakly diffracting, 
resulting in a large proportion of essentially "unobserved" 
reflections being used in the refinement, hence the Alert.
;
####################################################################### 
# 
# 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_po4055_refinalized_sq
_database_code_depnum_ccdc_archive 'CCDC 1883755'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;university of edinburgh
United Kingdom
;
_audit_update_record             
;
2018-12-07 deposited with the CCDC.	2019-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C57 H57 Cl N11 O2 U Zn'
_chemical_formula_weight         1266.98

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'
Cl Cl 0.3639 0.7018 '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'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+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                   28.7327(5)
_cell_length_b                   22.9300(3)
_cell_length_c                   24.8036(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.0775(13)
_cell_angle_gamma                90
_cell_volume                     15980.0(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    36633
_cell_measurement_theta_min      3.7100
_cell_measurement_theta_max      75.9250

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.053
_exptl_crystal_F_000             5048
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1250
_exptl_crystal_size_mid          0.0842
_exptl_crystal_size_min          0.0477
_exptl_absorpt_coefficient_mu    6.618
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_reflns_number            129575
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_av_R_equivalents  0.0807
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.146
_diffrn_reflns_theta_max         76.294
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             16675
_reflns_number_gt                14839
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    Sir-2014
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    MERCURY
_computing_publication_material  ORTEP
_refine_special_details          
'refined using SQUEEZE because of solvent disorder'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0001P)²+1381.1740P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16675
_refine_ls_number_parameters     660
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0983
_refine_ls_wR_factor_ref         0.2365
_refine_ls_wR_factor_gt          0.2329
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_restrained_S_all      1.142
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0316(5) 0.2746(5) 0.1673(5) 0.027(3) Uani 1 1 d . . . . .
C2 C 0.0029(5) 0.2884(6) 0.1151(5) 0.037(3) Uani 1 1 d . . . . .
H2 H 0.0139 0.2986 0.0828 0.044 Uiso 1 1 calc R U . . .
C3 C -0.0439(5) 0.2842(6) 0.1198(5) 0.037(3) Uani 1 1 d . . . . .
H3 H -0.0712 0.2912 0.0915 0.045 Uiso 1 1 calc R U . . .
C4 C -0.0437(5) 0.2677(5) 0.1745(5) 0.030(3) Uani 1 1 d . . . . .
C5 C -0.0815(5) 0.2635(6) 0.2019(5) 0.031(3) Uani 1 1 d . . . . .
H5 H -0.1134 0.2660 0.1816 0.038 Uiso 1 1 calc R U . . .
C6 C -0.1149(4) 0.2509(5) 0.2798(5) 0.026(3) Uani 1 1 d . . . . .
C7 C -0.1498(5) 0.2116(6) 0.2592(6) 0.037(3) Uani 1 1 d . . . . .
H7 H -0.1476 0.1884 0.2282 0.044 Uiso 1 1 calc R U . . .
C8 C -0.1895(5) 0.2058(6) 0.2847(6) 0.035(3) Uani 1 1 d . . . . .
C9 C -0.2273(5) 0.1621(7) 0.2640(8) 0.051(4) Uani 1 1 d . . . . .
H9A H -0.2310 0.1361 0.2942 0.076 Uiso 1 1 calc R U . . .
H9B H -0.2183 0.1391 0.2344 0.076 Uiso 1 1 calc R U . . .
H9C H -0.2575 0.1822 0.2497 0.076 Uiso 1 1 calc R U . . .
C10 C -0.1923(5) 0.2417(7) 0.3291(6) 0.039(3) Uani 1 1 d . . . . .
C11 C -0.2346(6) 0.2370(8) 0.3577(7) 0.052(4) Uani 1 1 d . . . . .
H11A H -0.2634 0.2513 0.3328 0.078 Uiso 1 1 calc R U . . .
H11B H -0.2282 0.2606 0.3914 0.078 Uiso 1 1 calc R U . . .
H11C H -0.2390 0.1962 0.3671 0.078 Uiso 1 1 calc R U . . .
C12 C -0.1566(5) 0.2816(6) 0.3495(6) 0.036(3) Uani 1 1 d . . . . .
H12 H -0.1593 0.3052 0.3801 0.043 Uiso 1 1 calc R U . . .
C13 C -0.1165(5) 0.2878(6) 0.3257(5) 0.028(3) Uani 1 1 d . . . . .
C14 C -0.0830(5) 0.3714(6) 0.3701(5) 0.031(3) Uani 1 1 d . . . . .
H14 H -0.1137 0.3828 0.3745 0.037 Uiso 1 1 calc R U . . .
C15 C -0.0424(5) 0.4063(5) 0.3924(5) 0.028(3) Uani 1 1 d . . . . .
C16 C -0.0379(5) 0.4592(5) 0.4203(4) 0.028(3) Uani 1 1 d . . . . .
H16 H -0.0631 0.4812 0.4295 0.033 Uiso 1 1 calc R U . . .
C17 C 0.0104(5) 0.4745(6) 0.4323(5) 0.029(3) Uani 1 1 d . . . . .
H17 H 0.0239 0.5081 0.4520 0.035 Uiso 1 1 calc R U . . .
C18 C 0.0348(5) 0.4318(5) 0.4104(5) 0.025(2) Uani 1 1 d . . . . .
C19 C 0.0868(5) 0.4248(5) 0.4133(5) 0.027(3) Uani 1 1 d . . . . .
C20 C 0.1139(5) 0.4822(6) 0.4348(5) 0.034(3) Uani 1 1 d . . . . .
H20A H 0.1011 0.5147 0.4106 0.052 Uiso 1 1 calc R U . . .
H20B H 0.1479 0.4775 0.4350 0.052 Uiso 1 1 calc R U . . .
H20C H 0.1099 0.4903 0.4724 0.052 Uiso 1 1 calc R U . . .
C21 C 0.0987(5) 0.4113(5) 0.3563(5) 0.027(3) Uani 1 1 d . . . . .
H21A H 0.0723 0.3898 0.3336 0.041 Uiso 1 1 calc R U . . .
H21B H 0.1277 0.3877 0.3615 0.041 Uiso 1 1 calc R U . . .
H21C H 0.1037 0.4479 0.3379 0.041 Uiso 1 1 calc R U . . .
C22 C 0.1065(4) 0.3757(5) 0.4541(5) 0.024(2) Uani 1 1 d . . . . .
C23 C 0.1341(5) 0.3765(5) 0.5057(5) 0.027(3) Uani 1 1 d . . . . .
H23 H 0.1484 0.4102 0.5245 0.032 Uiso 1 1 calc R U . . .
C24 C 0.1380(5) 0.3194(6) 0.5266(5) 0.028(3) Uani 1 1 d . . . . .
H24 H 0.1553 0.3075 0.5618 0.034 Uiso 1 1 calc R U . . .
C25 C 0.1117(4) 0.2832(5) 0.4859(5) 0.023(2) Uani 1 1 d . . . . .
C26 C 0.1052(5) 0.2222(5) 0.4864(5) 0.026(2) Uani 1 1 d . . . . .
H26 H 0.1206 0.2000 0.5174 0.031 Uiso 1 1 calc R U . . .
C27 C 0.0724(5) 0.1361(5) 0.4470(5) 0.027(3) Uani 1 1 d . . . . .
C28 C 0.0698(5) 0.1049(5) 0.4947(5) 0.030(3) Uani 1 1 d . . . . .
H28 H 0.0701 0.1258 0.5278 0.036 Uiso 1 1 calc R U . . .
C29 C 0.0667(5) 0.0442(6) 0.4954(5) 0.032(3) Uani 1 1 d . . . . .
C30 C 0.0649(7) 0.0134(6) 0.5497(6) 0.047(4) Uani 1 1 d . . . . .
H30A H 0.0684 0.0422 0.5794 0.070 Uiso 1 1 calc R U . . .
H30B H 0.0909 -0.0150 0.5583 0.070 Uiso 1 1 calc R U . . .
H30C H 0.0344 -0.0068 0.5462 0.070 Uiso 1 1 calc R U . . .
C31 C 0.0652(5) 0.0129(5) 0.4471(6) 0.033(3) Uani 1 1 d . . . . .
C32 C 0.0630(7) -0.0525(6) 0.4459(6) 0.044(4) Uani 1 1 d . . . . .
H32A H 0.0301 -0.0652 0.4433 0.066 Uiso 1 1 calc R U . . .
H32B H 0.0830 -0.0681 0.4797 0.066 Uiso 1 1 calc R U . . .
H32C H 0.0746 -0.0669 0.4139 0.066 Uiso 1 1 calc R U . . .
C33 C 0.0653(6) 0.0445(5) 0.3981(5) 0.034(3) Uani 1 1 d . . . . .
H33 H 0.0632 0.0234 0.3647 0.041 Uiso 1 1 calc R U . . .
C34 C 0.0683(5) 0.1046(5) 0.3968(5) 0.026(3) Uani 1 1 d . U . . .
C35 C 0.0993(5) 0.1137(6) 0.3189(5) 0.030(3) Uani 1 1 d . . . . .
H35 H 0.1147 0.0775 0.3291 0.036 Uiso 1 1 calc R U . . .
C36 C 0.1067(5) 0.1424(5) 0.2715(5) 0.027(3) Uani 1 1 d . . . . .
C37 C 0.1373(5) 0.1286(5) 0.2354(5) 0.027(3) Uani 1 1 d . . . . .
H37 H 0.1565 0.0947 0.2365 0.032 Uiso 1 1 calc R U . . .
C38 C 0.1338(5) 0.1745(6) 0.1980(5) 0.027(3) Uani 1 1 d . . . . .
H38 H 0.1503 0.1779 0.1687 0.033 Uiso 1 1 calc R U . . .
C39 C 0.1009(5) 0.2154(6) 0.2119(5) 0.028(3) Uani 1 1 d . . . . .
C40 C 0.0851(5) 0.2735(5) 0.1849(5) 0.026(3) Uani 1 1 d . . . . .
C41 C 0.1013(5) 0.3228(5) 0.2273(5) 0.029(3) Uani 1 1 d . . . . .
H41A H 0.0930 0.3607 0.2097 0.043 Uiso 1 1 calc R U . . .
H41B H 0.1359 0.3206 0.2408 0.043 Uiso 1 1 calc R U . . .
H41C H 0.0854 0.3183 0.2584 0.043 Uiso 1 1 calc R U . . .
C42 C 0.1077(5) 0.2847(6) 0.1346(5) 0.034(3) Uani 1 1 d . . . . .
H42A H 0.0954 0.2563 0.1056 0.050 Uiso 1 1 calc R U . . .
H42B H 0.1423 0.2809 0.1456 0.050 Uiso 1 1 calc R U . . .
H42C H 0.0996 0.3242 0.1206 0.050 Uiso 1 1 calc R U . . .
C43 C -0.0665(5) 0.1524(6) 0.3673(6) 0.036(3) Uani 1 1 d . . . . .
H43 H -0.0708 0.1292 0.3348 0.043 Uiso 1 1 calc R U . . .
C44 C -0.0953(6) 0.1412(6) 0.4041(6) 0.039(3) Uani 1 1 d . . . . .
H44 H -0.1195 0.1123 0.3967 0.047 Uiso 1 1 calc R U . . .
C45 C -0.0877(6) 0.1734(7) 0.4520(6) 0.042(4) Uani 1 1 d . . . . .
H45 H -0.1059 0.1655 0.4790 0.051 Uiso 1 1 calc R U . . .
C46 C -0.0530(5) 0.2180(7) 0.4613(5) 0.038(3) Uani 1 1 d . . . . .
H46 H -0.0480 0.2414 0.4936 0.046 Uiso 1 1 calc R U . . .
C47 C -0.0266(5) 0.2263(6) 0.4211(5) 0.031(3) Uani 1 1 d . . . . .
H47 H -0.0030 0.2559 0.4267 0.037 Uiso 1 1 calc R U . . .
C48 C -0.0533(5) 0.1265(6) 0.0868(5) 0.031(3) Uani 1 1 d . . . . .
H48 H -0.0862 0.1254 0.0876 0.038 Uiso 1 1 calc R U . . .
C49 C -0.0398(6) 0.1380(6) 0.0374(5) 0.036(3) Uani 1 1 d . . . . .
H49 H -0.0629 0.1449 0.0046 0.043 Uiso 1 1 calc R U . . .
C50 C 0.0085(6) 0.1390(6) 0.0371(6) 0.039(3) Uani 1 1 d . . . . .
H50 H 0.0191 0.1454 0.0038 0.047 Uiso 1 1 calc R U . . .
C51 C 0.0409(6) 0.1306(6) 0.0864(5) 0.037(3) Uani 1 1 d . . . . .
H51 H 0.0741 0.1321 0.0872 0.044 Uiso 1 1 calc R U . . .
C52 C 0.0253(5) 0.1199(6) 0.1342(5) 0.035(3) Uani 1 1 d . . . . .
H52 H 0.0477 0.1147 0.1679 0.042 Uiso 1 1 calc R U . . .
C53 C -0.0316(6) 0.0000(6) 0.2816(6) 0.043(4) Uani 1 1 d . . . . .
H53 H -0.0538 0.0250 0.2937 0.051 Uiso 1 1 calc R U . . .
C54 C -0.0199(7) -0.0502(7) 0.3103(6) 0.049(4) Uani 1 1 d . U . . .
H54 H -0.0315 -0.0592 0.3425 0.059 Uiso 1 1 calc R U . . .
C55 C 0.0114(8) -0.0895(6) 0.2884(6) 0.054(5) Uani 1 1 d . . . . .
H55 H 0.0193 -0.1270 0.3039 0.065 Uiso 1 1 calc R U . . .
C56 C 0.0290(7) -0.0699(8) 0.2446(6) 0.053(4) Uani 1 1 d . . . . .
H56 H 0.0520 -0.0927 0.2316 0.063 Uiso 1 1 calc R U . . .
C57 C 0.0145(5) -0.0189(7) 0.2192(5) 0.038(3) Uani 1 1 d . . . . .
H57 H 0.0253 -0.0086 0.1868 0.045 Uiso 1 1 calc R U . . .
N1 N 0.0032(4) 0.2633(5) 0.2030(4) 0.025(2) Uani 1 1 d . . . . .
N2 N -0.0730(4) 0.2561(5) 0.2557(4) 0.028(2) Uani 1 1 d . . . . .
N3 N -0.0775(4) 0.3244(4) 0.3441(4) 0.0217(14) Uani 1 1 d . . . . .
N4 N 0.0026(4) 0.3915(5) 0.3869(4) 0.029(2) Uani 1 1 d . . . . .
H4 H 0.0096 0.3598 0.3701 0.035 Uiso 1 1 calc R U . . .
N5 N 0.0917(4) 0.3198(4) 0.4429(4) 0.024(2) Uani 1 1 d . . . . .
H5A H 0.0722 0.3085 0.4125 0.029 Uiso 1 1 calc R U . . .
N6 N 0.0787(4) 0.1969(4) 0.4452(4) 0.0217(14) Uani 1 1 d . . . . .
N7 N 0.0722(4) 0.1354(4) 0.3489(4) 0.025(2) Uani 1 1 d . . . . .
N8 N 0.0834(4) 0.1953(4) 0.2559(4) 0.027(2) Uani 1 1 d . . . . .
N9 N -0.0328(4) 0.1939(5) 0.3742(4) 0.031(2) Uani 1 1 d . . . . .
N10 N -0.0210(4) 0.1170(4) 0.1335(4) 0.031(2) Uani 1 1 d . . . . .
N11 N -0.0148(4) 0.0174(4) 0.2384(4) 0.030(2) Uani 1 1 d . . . . .
O1 O 0.0378(3) 0.2842(4) 0.3354(3) 0.0286(18) Uani 1 1 d . . . . .
O2 O -0.0163(3) 0.1483(4) 0.2611(4) 0.0289(19) Uani 1 1 d . . . . .
Cl1 Cl -0.12102(13) 0.08162(17) 0.18938(15) 0.0420(8) Uani 1 1 d . . . . .
Zn1 Zn -0.04267(6) 0.09518(7) 0.20417(7) 0.0279(4) Uani 1 1 d . . . . .
U1 U 0.01311(2) 0.21725(2) 0.29647(2) 0.02324(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
C1 N1 1.351(15) . ?
C1 C2 1.417(17) . ?
C1 C40 1.507(19) . ?
C2 C3 1.38(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.406(18) . ?
C3 H3 0.9500 . ?
C4 N1 1.388(17) . ?
C4 C5 1.400(18) . ?
C5 N2 1.317(16) . ?
C5 H5 0.9500 . ?
C6 C7 1.364(19) . ?
C6 C13 1.428(16) . ?
C6 N2 1.457(15) . ?
C7 C8 1.42(2) . ?
C7 H7 0.9500 . ?
C8 C10 1.39(2) . ?
C8 C9 1.489(19) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C12 1.39(2) . ?
C10 C11 1.532(19) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.406(19) . ?
C12 H12 0.9500 . ?
C13 N3 1.399(16) . ?
C14 N3 1.281(16) . ?
C14 C15 1.427(19) . ?
C14 H14 0.9500 . ?
C15 N4 1.371(17) . ?
C15 C16 1.388(17) . ?
C16 C17 1.402(19) . ?
C16 H16 0.9500 . ?
C17 C18 1.381(18) . ?
C17 H17 0.9500 . ?
C18 N4 1.351(16) . ?
C18 C19 1.490(18) . ?
C19 C22 1.540(16) . ?
C19 C21 1.554(15) . ?
C19 C20 1.564(17) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.358(17) . ?
C22 N5 1.359(15) . ?
C23 C24 1.405(17) . ?
C23 H23 0.9500 . ?
C24 C25 1.399(17) . ?
C24 H24 0.9500 . ?
C25 N5 1.385(14) . ?
C25 C26 1.411(17) . ?
C26 N6 1.280(15) . ?
C26 H26 0.9500 . ?
C27 C28 1.398(16) . ?
C27 N6 1.406(15) . ?
C27 C34 1.423(15) . ?
C28 C29 1.395(18) . ?
C28 H28 0.9500 . ?
C29 C31 1.388(19) . ?
C29 C30 1.531(17) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C33 1.416(18) . ?
C31 C32 1.501(17) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.382(17) . ?
C33 H33 0.9500 . ?
C34 N7 1.408(15) . ?
C35 N7 1.284(17) . ?
C35 C36 1.402(17) . ?
C35 H35 0.9500 . ?
C36 N8 1.402(16) . ?
C36 C37 1.414(15) . ?
C37 C38 1.393(17) . ?
C37 H37 0.9500 . ?
C38 C39 1.425(17) . ?
C38 H38 0.9500 . ?
C39 N8 1.371(16) . ?
C39 C40 1.516(17) . ?
C40 C42 1.544(16) . ?
C40 C41 1.548(15) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 N9 1.343(18) . ?
C43 C44 1.379(19) . ?
C43 H43 0.9500 . ?
C44 C45 1.38(2) . ?
C44 H44 0.9500 . ?
C45 C46 1.41(2) . ?
C45 H45 0.9500 . ?
C46 C47 1.385(18) . ?
C46 H46 0.9500 . ?
C47 N9 1.360(16) . ?
C47 H47 0.9500 . ?
C48 N10 1.342(17) . ?
C48 C49 1.385(18) . ?
C48 H48 0.9500 . ?
C49 C50 1.39(2) . ?
C49 H49 0.9500 . ?
C50 C51 1.39(2) . ?
C50 H50 0.9500 . ?
C51 C52 1.374(18) . ?
C51 H51 0.9500 . ?
C52 N10 1.329(18) . ?
C52 H52 0.9500 . ?
C53 N11 1.326(16) . ?
C53 C54 1.36(2) . ?
C53 H53 0.9500 . ?
C54 C55 1.46(3) . ?
C54 H54 0.9500 . ?
C55 C56 1.37(2) . ?
C55 H55 0.9500 . ?
C56 C57 1.35(2) . ?
C56 H56 0.9500 . ?
C57 N11 1.341(17) . ?
C57 H57 0.9500 . ?
N1 U1 2.509(10) . ?
N2 U1 2.625(11) . ?
N4 H4 0.8800 . ?
N5 H5A 0.8800 . ?
N7 U1 2.678(11) . ?
N8 U1 2.491(11) . ?
N9 U1 2.610(11) . ?
N10 Zn1 2.042(11) . ?
N11 Zn1 2.063(10) . ?
O1 U1 1.873(9) . ?
O2 Zn1 1.899(9) . ?
O2 U1 1.916(8) . ?
Cl1 Zn1 2.226(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 108.9(12) . . ?
N1 C1 C40 121.7(11) . . ?
C2 C1 C40 129.3(11) . . ?
C3 C2 C1 107.4(12) . . ?
C3 C2 H2 126.3 . . ?
C1 C2 H2 126.3 . . ?
C2 C3 C4 107.1(12) . . ?
C2 C3 H3 126.5 . . ?
C4 C3 H3 126.5 . . ?
N1 C4 C5 121.0(11) . . ?
N1 C4 C3 108.6(12) . . ?
C5 C4 C3 129.8(13) . . ?
N2 C5 C4 120.2(13) . . ?
N2 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C7 C6 C13 123.1(12) . . ?
C7 C6 N2 120.5(11) . . ?
C13 C6 N2 116.4(11) . . ?
C6 C7 C8 119.4(13) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 H7 120.3 . . ?
C10 C8 C7 118.8(13) . . ?
C10 C8 C9 120.8(14) . . ?
C7 C8 C9 120.3(14) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C12 C10 C8 121.1(12) . . ?
C12 C10 C11 118.3(14) . . ?
C8 C10 C11 120.6(14) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 C13 121.5(12) . . ?
C10 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
N3 C13 C12 126.5(11) . . ?
N3 C13 C6 117.4(11) . . ?
C12 C13 C6 116.1(12) . . ?
N3 C14 C15 119.3(13) . . ?
N3 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
N4 C15 C16 106.0(12) . . ?
N4 C15 C14 122.2(12) . . ?
C16 C15 C14 131.8(13) . . ?
C15 C16 C17 108.1(11) . . ?
C15 C16 H16 126.0 . . ?
C17 C16 H16 126.0 . . ?
C18 C17 C16 107.4(11) . . ?
C18 C17 H17 126.3 . . ?
C16 C17 H17 126.3 . . ?
N4 C18 C17 107.3(12) . . ?
N4 C18 C19 122.5(11) . . ?
C17 C18 C19 130.0(12) . . ?
C18 C19 C22 109.7(10) . . ?
C18 C19 C21 112.7(10) . . ?
C22 C19 C21 109.3(10) . . ?
C18 C19 C20 110.5(11) . . ?
C22 C19 C20 107.7(10) . . ?
C21 C19 C20 106.8(10) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 N5 107.6(10) . . ?
C23 C22 C19 132.1(11) . . ?
N5 C22 C19 120.0(10) . . ?
C22 C23 C24 108.7(11) . . ?
C22 C23 H23 125.7 . . ?
C24 C23 H23 125.7 . . ?
C25 C24 C23 107.3(11) . . ?
C25 C24 H24 126.4 . . ?
C23 C24 H24 126.4 . . ?
N5 C25 C24 105.7(11) . . ?
N5 C25 C26 125.0(11) . . ?
C24 C25 C26 129.3(11) . . ?
N6 C26 C25 120.1(10) . . ?
N6 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C28 C27 N6 124.3(11) . . ?
C28 C27 C34 118.0(11) . . ?
N6 C27 C34 117.7(10) . . ?
C29 C28 C27 122.5(12) . . ?
C29 C28 H28 118.8 . . ?
C27 C28 H28 118.8 . . ?
C31 C29 C28 119.7(12) . . ?
C31 C29 C30 121.2(12) . . ?
C28 C29 C30 119.1(12) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 C33 118.1(11) . . ?
C29 C31 C32 121.9(12) . . ?
C33 C31 C32 120.1(12) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C31 122.8(12) . . ?
C34 C33 H33 118.6 . . ?
C31 C33 H33 118.6 . . ?
C33 C34 N7 122.4(10) . . ?
C33 C34 C27 118.7(11) . . ?
N7 C34 C27 118.5(10) . . ?
N7 C35 C36 121.5(12) . . ?
N7 C35 H35 119.3 . . ?
C36 C35 H35 119.3 . . ?
C35 C36 N8 119.3(11) . . ?
C35 C36 C37 130.6(12) . . ?
N8 C36 C37 110.0(10) . . ?
C38 C37 C36 106.5(11) . . ?
C38 C37 H37 126.7 . . ?
C36 C37 H37 126.7 . . ?
C37 C38 C39 107.2(10) . . ?
C37 C38 H38 126.4 . . ?
C39 C38 H38 126.4 . . ?
N8 C39 C38 110.1(11) . . ?
N8 C39 C40 121.3(11) . . ?
C38 C39 C40 128.6(11) . . ?
C1 C40 C39 109.6(10) . . ?
C1 C40 C42 109.7(10) . . ?
C39 C40 C42 111.5(10) . . ?
C1 C40 C41 109.2(10) . . ?
C39 C40 C41 108.8(10) . . ?
C42 C40 C41 108.0(10) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N9 C43 C44 124.3(13) . . ?
N9 C43 H43 117.9 . . ?
C44 C43 H43 117.9 . . ?
C45 C44 C43 117.6(14) . . ?
C45 C44 H44 121.2 . . ?
C43 C44 H44 121.2 . . ?
C44 C45 C46 120.5(13) . . ?
C44 C45 H45 119.7 . . ?
C46 C45 H45 119.7 . . ?
C47 C46 C45 117.1(13) . . ?
C47 C46 H46 121.5 . . ?
C45 C46 H46 121.5 . . ?
N9 C47 C46 123.2(13) . . ?
N9 C47 H47 118.4 . . ?
C46 C47 H47 118.4 . . ?
N10 C48 C49 121.5(13) . . ?
N10 C48 H48 119.2 . . ?
C49 C48 H48 119.2 . . ?
C48 C49 C50 118.3(13) . . ?
C48 C49 H49 120.9 . . ?
C50 C49 H49 120.9 . . ?
C51 C50 C49 118.6(12) . . ?
C51 C50 H50 120.7 . . ?
C49 C50 H50 120.7 . . ?
C52 C51 C50 120.4(15) . . ?
C52 C51 H51 119.8 . . ?
C50 C51 H51 119.8 . . ?
N10 C52 C51 120.2(14) . . ?
N10 C52 H52 119.9 . . ?
C51 C52 H52 119.9 . . ?
N11 C53 C54 125.9(15) . . ?
N11 C53 H53 117.0 . . ?
C54 C53 H53 117.0 . . ?
C53 C54 C55 115.7(13) . . ?
C53 C54 H54 122.1 . . ?
C55 C54 H54 122.1 . . ?
C56 C55 C54 117.0(14) . . ?
C56 C55 H55 121.5 . . ?
C54 C55 H55 121.5 . . ?
C57 C56 C55 121.6(17) . . ?
C57 C56 H56 119.2 . . ?
C55 C56 H56 119.2 . . ?
N11 C57 C56 121.9(13) . . ?
N11 C57 H57 119.0 . . ?
C56 C57 H57 119.0 . . ?
C1 N1 C4 107.9(10) . . ?
C1 N1 U1 136.0(9) . . ?
C4 N1 U1 114.4(8) . . ?
C5 N2 C6 115.5(11) . . ?
C5 N2 U1 113.2(8) . . ?
C6 N2 U1 127.5(8) . . ?
C14 N3 C13 119.7(11) . . ?
C18 N4 C15 111.2(11) . . ?
C18 N4 H4 124.4 . . ?
C15 N4 H4 124.4 . . ?
C22 N5 C25 110.6(10) . . ?
C22 N5 H5A 124.7 . . ?
C25 N5 H5A 124.7 . . ?
C26 N6 C27 118.9(10) . . ?
C35 N7 C34 117.4(11) . . ?
C35 N7 U1 113.0(8) . . ?
C34 N7 U1 127.4(8) . . ?
C39 N8 C36 106.1(10) . . ?
C39 N8 U1 135.8(9) . . ?
C36 N8 U1 116.4(8) . . ?
C43 N9 C47 117.3(12) . . ?
C43 N9 U1 120.9(9) . . ?
C47 N9 U1 121.6(9) . . ?
C52 N10 C48 120.9(11) . . ?
C52 N10 Zn1 119.0(9) . . ?
C48 N10 Zn1 120.1(9) . . ?
C53 N11 C57 117.4(12) . . ?
C53 N11 Zn1 114.7(10) . . ?
C57 N11 Zn1 127.6(9) . . ?
Zn1 O2 U1 159.9(5) . . ?
O2 Zn1 N10 109.6(4) . . ?
O2 Zn1 N11 100.9(4) . . ?
N10 Zn1 N11 113.8(4) . . ?
O2 Zn1 Cl1 116.4(3) . . ?
N10 Zn1 Cl1 111.9(4) . . ?
N11 Zn1 Cl1 103.8(4) . . ?
O1 U1 O2 174.6(4) . . ?
O1 U1 N8 97.1(3) . . ?
O2 U1 N8 88.0(3) . . ?
O1 U1 N1 95.2(3) . . ?
O2 U1 N1 88.3(4) . . ?
N8 U1 N1 69.9(3) . . ?
O1 U1 N9 89.0(3) . . ?
O2 U1 N9 85.8(4) . . ?
N8 U1 N9 146.7(3) . . ?
N1 U1 N9 142.4(3) . . ?
O1 U1 N2 98.3(4) . . ?
O2 U1 N2 79.3(4) . . ?
N8 U1 N2 133.8(3) . . ?
N1 U1 N2 65.5(3) . . ?
N9 U1 N2 76.9(3) . . ?
O1 U1 N7 101.1(3) . . ?
O2 U1 N7 79.5(3) . . ?
N8 U1 N7 64.5(3) . . ?
N1 U1 N7 132.9(3) . . ?
N9 U1 N7 82.2(3) . . ?
N2 U1 N7 151.1(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
N1 C1 C2 C3 -1.0(15) . . . . ?
C40 C1 C2 C3 -178.9(12) . . . . ?
C1 C2 C3 C4 -0.3(16) . . . . ?
C2 C3 C4 N1 1.4(15) . . . . ?
C2 C3 C4 C5 172.6(14) . . . . ?
N1 C4 C5 N2 1(2) . . . . ?
C3 C4 C5 N2 -169.1(14) . . . . ?
C13 C6 C7 C8 -1(2) . . . . ?
N2 C6 C7 C8 177.7(12) . . . . ?
C6 C7 C8 C10 2(2) . . . . ?
C6 C7 C8 C9 -178.2(13) . . . . ?
C7 C8 C10 C12 -2(2) . . . . ?
C9 C8 C10 C12 178.3(14) . . . . ?
C7 C8 C10 C11 179.9(14) . . . . ?
C9 C8 C10 C11 0(2) . . . . ?
C8 C10 C12 C13 1(2) . . . . ?
C11 C10 C12 C13 179.3(14) . . . . ?
C10 C12 C13 N3 -177.0(13) . . . . ?
C10 C12 C13 C6 0(2) . . . . ?
C7 C6 C13 N3 177.4(12) . . . . ?
N2 C6 C13 N3 -1.4(17) . . . . ?
C7 C6 C13 C12 0.1(19) . . . . ?
N2 C6 C13 C12 -178.6(12) . . . . ?
N3 C14 C15 N4 0.2(18) . . . . ?
N3 C14 C15 C16 177.6(12) . . . . ?
N4 C15 C16 C17 -1.6(13) . . . . ?
C14 C15 C16 C17 -179.2(12) . . . . ?
C15 C16 C17 C18 1.7(13) . . . . ?
C16 C17 C18 N4 -1.2(13) . . . . ?
C16 C17 C18 C19 -176.8(11) . . . . ?
N4 C18 C19 C22 -69.8(14) . . . . ?
C17 C18 C19 C22 105.3(14) . . . . ?
N4 C18 C19 C21 52.3(15) . . . . ?
C17 C18 C19 C21 -132.6(13) . . . . ?
N4 C18 C19 C20 171.7(10) . . . . ?
C17 C18 C19 C20 -13.2(17) . . . . ?
C18 C19 C22 C23 -106.8(15) . . . . ?
C21 C19 C22 C23 129.2(14) . . . . ?
C20 C19 C22 C23 13.4(19) . . . . ?
C18 C19 C22 N5 65.0(14) . . . . ?
C21 C19 C22 N5 -59.0(15) . . . . ?
C20 C19 C22 N5 -174.7(11) . . . . ?
N5 C22 C23 C24 2.0(15) . . . . ?
C19 C22 C23 C24 174.6(13) . . . . ?
C22 C23 C24 C25 -0.1(15) . . . . ?
C23 C24 C25 N5 -1.8(14) . . . . ?
C23 C24 C25 C26 178.7(13) . . . . ?
N5 C25 C26 N6 -1.0(19) . . . . ?
C24 C25 C26 N6 178.4(12) . . . . ?
N6 C27 C28 C29 -175.7(13) . . . . ?
C34 C27 C28 C29 5(2) . . . . ?
C27 C28 C29 C31 -1(2) . . . . ?
C27 C28 C29 C30 178.8(14) . . . . ?
C28 C29 C31 C33 -2(2) . . . . ?
C30 C29 C31 C33 177.8(15) . . . . ?
C28 C29 C31 C32 178.5(14) . . . . ?
C30 C29 C31 C32 -2(2) . . . . ?
C29 C31 C33 C34 2(2) . . . . ?
C32 C31 C33 C34 -178.5(15) . . . . ?
C31 C33 C34 N7 174.8(13) . . . . ?
C31 C33 C34 C27 1(2) . . . . ?
C28 C27 C34 C33 -5(2) . . . . ?
N6 C27 C34 C33 175.8(13) . . . . ?
C28 C27 C34 N7 -178.3(12) . . . . ?
N6 C27 C34 N7 2.1(19) . . . . ?
N7 C35 C36 N8 -1(2) . . . . ?
N7 C35 C36 C37 175.0(13) . . . . ?
C35 C36 C37 C38 -174.6(14) . . . . ?
N8 C36 C37 C38 1.7(15) . . . . ?
C36 C37 C38 C39 -0.3(15) . . . . ?
C37 C38 C39 N8 -1.2(15) . . . . ?
C37 C38 C39 C40 178.7(12) . . . . ?
N1 C1 C40 C39 54.2(13) . . . . ?
C2 C1 C40 C39 -128.0(13) . . . . ?
N1 C1 C40 C42 176.9(11) . . . . ?
C2 C1 C40 C42 -5.3(17) . . . . ?
N1 C1 C40 C41 -64.9(13) . . . . ?
C2 C1 C40 C41 112.8(14) . . . . ?
N8 C39 C40 C1 -55.4(14) . . . . ?
C38 C39 C40 C1 124.8(13) . . . . ?
N8 C39 C40 C42 -177.0(11) . . . . ?
C38 C39 C40 C42 3.1(18) . . . . ?
N8 C39 C40 C41 64.0(15) . . . . ?
C38 C39 C40 C41 -115.9(13) . . . . ?
N9 C43 C44 C45 -2(2) . . . . ?
C43 C44 C45 C46 3(2) . . . . ?
C44 C45 C46 C47 -2(2) . . . . ?
C45 C46 C47 N9 0(2) . . . . ?
N10 C48 C49 C50 0(2) . . . . ?
C48 C49 C50 C51 -2(2) . . . . ?
C49 C50 C51 C52 2(2) . . . . ?
C50 C51 C52 N10 1(2) . . . . ?
N11 C53 C54 C55 -4(3) . . . . ?
C53 C54 C55 C56 5(2) . . . . ?
C54 C55 C56 C57 -6(3) . . . . ?
C55 C56 C57 N11 6(3) . . . . ?
C2 C1 N1 C4 1.8(14) . . . . ?
C40 C1 N1 C4 180.0(10) . . . . ?
C2 C1 N1 U1 165.5(9) . . . . ?
C40 C1 N1 U1 -16.4(17) . . . . ?
C5 C4 N1 C1 -174.1(12) . . . . ?
C3 C4 N1 C1 -2.0(14) . . . . ?
C5 C4 N1 U1 18.3(15) . . . . ?
C3 C4 N1 U1 -169.6(8) . . . . ?
C4 C5 N2 C6 -178.5(12) . . . . ?
C4 C5 N2 U1 -18.8(16) . . . . ?
C7 C6 N2 C5 51.9(17) . . . . ?
C13 C6 N2 C5 -129.3(13) . . . . ?
C7 C6 N2 U1 -104.4(12) . . . . ?
C13 C6 N2 U1 74.4(13) . . . . ?
C15 C14 N3 C13 175.3(10) . . . . ?
C12 C13 N3 C14 -28.0(19) . . . . ?
C6 C13 N3 C14 155.0(11) . . . . ?
C17 C18 N4 C15 0.2(13) . . . . ?
C19 C18 N4 C15 176.3(10) . . . . ?
C16 C15 N4 C18 0.9(13) . . . . ?
C14 C15 N4 C18 178.8(11) . . . . ?
C23 C22 N5 C25 -3.2(14) . . . . ?
C19 C22 N5 C25 -176.9(10) . . . . ?
C24 C25 N5 C22 3.1(13) . . . . ?
C26 C25 N5 C22 -177.3(12) . . . . ?
C25 C26 N6 C27 -179.4(11) . . . . ?
C28 C27 N6 C26 35.9(19) . . . . ?
C34 C27 N6 C26 -144.6(13) . . . . ?
C36 C35 N7 C34 -177.7(12) . . . . ?
C36 C35 N7 U1 18.0(16) . . . . ?
C33 C34 N7 C35 -40.4(19) . . . . ?
C27 C34 N7 C35 133.1(13) . . . . ?
C33 C34 N7 U1 121.3(13) . . . . ?
C27 C34 N7 U1 -65.2(15) . . . . ?
C38 C39 N8 C36 2.2(14) . . . . ?
C40 C39 N8 C36 -177.7(11) . . . . ?
C38 C39 N8 U1 -161.3(9) . . . . ?
C40 C39 N8 U1 18.8(18) . . . . ?
C35 C36 N8 C39 174.4(12) . . . . ?
C37 C36 N8 C39 -2.4(14) . . . . ?
C35 C36 N8 U1 -18.4(15) . . . . ?
C37 C36 N8 U1 164.9(8) . . . . ?
C44 C43 N9 C47 1(2) . . . . ?
C44 C43 N9 U1 -173.7(11) . . . . ?
C46 C47 N9 C43 0.3(19) . . . . ?
C46 C47 N9 U1 174.8(10) . . . . ?
C51 C52 N10 C48 -3(2) . . . . ?
C51 C52 N10 Zn1 175.5(10) . . . . ?
C49 C48 N10 C52 2.0(19) . . . . ?
C49 C48 N10 Zn1 -176.1(10) . . . . ?
C54 C53 N11 C57 4(2) . . . . ?
C54 C53 N11 Zn1 178.0(14) . . . . ?
C56 C57 N11 C53 -4(2) . . . . ?
C56 C57 N11 Zn1 -177.7(13) . . . . ?
U1 O2 Zn1 N10 18.0(17) . . . . ?
U1 O2 Zn1 N11 138.3(15) . . . . ?
U1 O2 Zn1 Cl1 -110.2(15) . . . . ?

_refine_diff_density_max         5.273
_refine_diff_density_min         -3.704
_refine_diff_density_rms         0.251



####################################################################### 
# 
# 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_p14093mono
_database_code_depnum_ccdc_archive 'CCDC 1883751'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;university of edinburgh
United Kingdom
;
_audit_update_record             
;
2018-12-07 deposited with the CCDC.	2019-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C82 H86 Cl N12 O3 U Zr'
_chemical_formula_weight         1652.33

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'
Zr Zr -2.9673 0.5597 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'

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

_cell_length_a                   20.2769(12)
_cell_length_b                   21.7767(10)
_cell_length_c                   18.5794(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.829(7)
_cell_angle_gamma                90.00
_cell_volume                     7384.4(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    18401
_cell_measurement_theta_min      3.4440
_cell_measurement_theta_max      29.3660

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.5278
_exptl_crystal_size_mid          0.2306
_exptl_crystal_size_min          0.1686
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3340
_exptl_absorpt_coefficient_mu    2.426
_exptl_absorpt_correction_T_min  0.62636
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            75846
_diffrn_reflns_av_R_equivalents  0.1048
_diffrn_reflns_av_sigmaI/netI    0.0794
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.88
_diffrn_reflns_theta_max         25.68
_reflns_number_total             14015
_reflns_number_gt                10516
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_structure_solution    WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    MERCURY
_computing_publication_material  ORTEP

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0536P)²+79.3412P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14015
_refine_ls_number_parameters     901
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0717
_refine_ls_wR_factor_ref         0.1783
_refine_ls_wR_factor_gt          0.1606
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3511(5) 0.2505(4) 0.3045(5) 0.0302(19) Uani 1 1 d . . .
C2 C 0.3267(5) 0.1895(4) 0.2973(5) 0.038(2) Uani 1 1 d . . .
H2 H 0.3566 0.1538 0.3122 0.046 Uiso 1 1 calc R . .
C3 C 0.2504(5) 0.1908(5) 0.2643(5) 0.037(2) Uani 1 1 d . . .
H3 H 0.2184 0.1566 0.2530 0.044 Uiso 1 1 calc R . .
C4 C 0.2308(5) 0.2521(4) 0.2511(5) 0.0275(18) Uani 1 1 d . . .
C5 C 0.1610(4) 0.2797(4) 0.2138(5) 0.0301(19) Uani 1 1 d . . .
H5 H 0.1190 0.2540 0.1944 0.036 Uiso 1 1 calc R . .
C6 C 0.0779(5) 0.3605(4) 0.1628(5) 0.035(2) Uani 1 1 d . . .
C7 C 0.0237(5) 0.3484(5) 0.1870(6) 0.040(2) Uani 1 1 d . . .
H7 H 0.0353 0.3240 0.2333 0.048 Uiso 1 1 calc R . .
C8 C -0.0467(5) 0.3709(5) 0.1460(6) 0.044(2) Uani 1 1 d . . .
C9 C -0.1037(6) 0.3562(6) 0.1744(8) 0.068(4) Uani 1 1 d . . .
H9A H -0.1503 0.3754 0.1387 0.102 Uiso 1 1 calc R . .
H9B H -0.0880 0.3719 0.2288 0.102 Uiso 1 1 calc R . .
H9C H -0.1103 0.3116 0.1742 0.102 Uiso 1 1 calc R . .
C10 C -0.0632(5) 0.4075(5) 0.0789(6) 0.045(3) Uani 1 1 d . . .
C11 C -0.1390(6) 0.4343(6) 0.0321(8) 0.063(3) Uani 1 1 d . . .
H11A H -0.1707 0.4221 0.0572 0.094 Uiso 1 1 calc R . .
H11B H -0.1597 0.4189 -0.0230 0.094 Uiso 1 1 calc R . .
H11C H -0.1357 0.4792 0.0318 0.094 Uiso 1 1 calc R . .
C12 C -0.0092(5) 0.4189(5) 0.0541(6) 0.042(2) Uani 1 1 d . . .
H12 H -0.0205 0.4438 0.0082 0.051 Uiso 1 1 calc R . .
C13 C 0.0605(5) 0.3955(4) 0.0939(5) 0.037(2) Uani 1 1 d . . .
C14 C 0.1056(5) 0.3957(4) -0.0009(6) 0.040(2) Uani 1 1 d . . .
H14 H 0.0593 0.3801 -0.0375 0.049 Uiso 1 1 calc R . .
C15 C 0.1614(5) 0.4075(4) -0.0276(5) 0.038(2) Uani 1 1 d . . .
C16 C 0.1612(7) 0.4050(6) -0.1012(7) 0.056(3) Uani 1 1 d . . .
H16 H 0.1216 0.3921 -0.1496 0.067 Uiso 1 1 calc R . .
C17 C 0.2297(6) 0.4251(5) -0.0922(6) 0.049(3) Uani 1 1 d . . .
H17 H 0.2448 0.4288 -0.1337 0.059 Uiso 1 1 calc R . .
C18 C 0.2716(6) 0.4385(5) -0.0129(6) 0.042(2) Uani 1 1 d . . .
C19 C 0.3491(5) 0.4626(5) 0.0312(6) 0.042(2) Uani 1 1 d . . .
C20 C 0.3841(7) 0.4697(7) -0.0265(7) 0.068(4) Uani 1 1 d . . .
H20A H 0.4342 0.4852 0.0027 0.101 Uiso 1 1 calc R . .
H20B H 0.3553 0.4987 -0.0689 0.101 Uiso 1 1 calc R . .
H20C H 0.3852 0.4298 -0.0502 0.101 Uiso 1 1 calc R . .
C21 C 0.3950(6) 0.4161(6) 0.0971(6) 0.053(3) Uani 1 1 d . . .
H21A H 0.4452 0.4314 0.1259 0.079 Uiso 1 1 calc R . .
H21B H 0.3956 0.3764 0.0725 0.079 Uiso 1 1 calc R . .
H21C H 0.3732 0.4110 0.1345 0.079 Uiso 1 1 calc R . .
C22 C 0.3479(5) 0.5246(5) 0.0680(5) 0.042(2) Uani 1 1 d . . .
C23 C 0.3539(6) 0.5827(6) 0.0445(7) 0.054(3) Uani 1 1 d . . .
H23 H 0.3622 0.5933 -0.0005 0.065 Uiso 1 1 calc R . .
C24 C 0.3461(6) 0.6237(5) 0.0972(6) 0.052(3) Uani 1 1 d . . .
H24 H 0.3480 0.6672 0.0946 0.063 Uiso 1 1 calc R . .
C25 C 0.3350(5) 0.5907(4) 0.1538(6) 0.038(2) Uani 1 1 d . . .
C26 C 0.3269(5) 0.6101(4) 0.2233(6) 0.039(2) Uani 1 1 d . . .
H26 H 0.3291 0.6526 0.2353 0.047 Uiso 1 1 calc R . .
C27 C 0.3082(4) 0.5923(4) 0.3372(5) 0.0303(19) Uani 1 1 d . . .
C28 C 0.2914(5) 0.6528(5) 0.3485(6) 0.042(2) Uani 1 1 d . . .
H28 H 0.2818 0.6819 0.3069 0.050 Uiso 1 1 calc R . .
C29 C 0.2884(6) 0.6716(5) 0.4169(6) 0.046(3) Uani 1 1 d . . .
C30 C 0.2725(8) 0.7376(6) 0.4274(8) 0.070(4) Uani 1 1 d . . .
H30A H 0.2724 0.7428 0.4798 0.105 Uiso 1 1 calc R . .
H30B H 0.2245 0.7490 0.3852 0.105 Uiso 1 1 calc R . .
H30C H 0.3103 0.7639 0.4242 0.105 Uiso 1 1 calc R . .
C31 C 0.3012(6) 0.6287(5) 0.4780(6) 0.043(2) Uani 1 1 d . . .
C32 C 0.2989(7) 0.6481(6) 0.5551(7) 0.062(3) Uani 1 1 d . . .
H32A H 0.2871 0.6920 0.5525 0.093 Uiso 1 1 calc R . .
H32B H 0.3468 0.6407 0.6001 0.093 Uiso 1 1 calc R . .
H32C H 0.2614 0.6243 0.5626 0.093 Uiso 1 1 calc R . .
C33 C 0.3167(5) 0.5689(5) 0.4665(5) 0.038(2) Uani 1 1 d . . .
H33 H 0.3246 0.5396 0.5074 0.045 Uiso 1 1 calc R . .
C34 C 0.3212(4) 0.5499(4) 0.3977(5) 0.032(2) Uani 1 1 d . . .
C35 C 0.4020(5) 0.4680(4) 0.4478(5) 0.0302(19) Uani 1 1 d . . .
H35 H 0.4264 0.4936 0.4932 0.036 Uiso 1 1 calc R . .
C36 C 0.4328(5) 0.4099(4) 0.4469(5) 0.031(2) Uani 1 1 d . . .
C37 C 0.4981(5) 0.3852(4) 0.5005(5) 0.035(2) Uani 1 1 d . . .
H37 H 0.5312 0.4024 0.5501 0.042 Uiso 1 1 calc R . .
C38 C 0.5063(5) 0.3300(4) 0.4679(5) 0.034(2) Uani 1 1 d . . .
H38 H 0.5458 0.3019 0.4914 0.041 Uiso 1 1 calc R . .
C39 C 0.4455(5) 0.3236(4) 0.3943(5) 0.033(2) Uani 1 1 d . . .
C40 C 0.4285(5) 0.2738(4) 0.3321(6) 0.036(2) Uani 1 1 d . . .
C41 C 0.4833(6) 0.2207(5) 0.3665(7) 0.060(3) Uani 1 1 d . . .
H41A H 0.4722 0.1887 0.3258 0.090 Uiso 1 1 calc R . .
H41B H 0.4796 0.2036 0.4134 0.090 Uiso 1 1 calc R . .
H41C H 0.5331 0.2360 0.3822 0.090 Uiso 1 1 calc R . .
C42 C 0.4369(6) 0.3010(5) 0.2605(6) 0.047(3) Uani 1 1 d . . .
H42A H 0.4263 0.2693 0.2195 0.071 Uiso 1 1 calc R . .
H42B H 0.4871 0.3158 0.2779 0.071 Uiso 1 1 calc R . .
H42C H 0.4025 0.3352 0.2382 0.071 Uiso 1 1 calc R . .
C43 C 0.1166(6) 0.4755(6) 0.2710(6) 0.057(3) Uani 1 1 d . . .
H43 H 0.1192 0.4434 0.3068 0.069 Uiso 1 1 calc R . .
C44 C 0.0580(8) 0.5158(9) 0.2455(9) 0.095(6) Uani 1 1 d . . .
H44 H 0.0215 0.5121 0.2644 0.114 Uiso 1 1 calc R . .
C45 C 0.0537(10) 0.5607(10) 0.1935(9) 0.109(7) Uani 1 1 d . . .
H45 H 0.0137 0.5886 0.1750 0.131 Uiso 1 1 calc R . .
C46 C 0.1064(8) 0.5659(6) 0.1676(8) 0.071(4) Uani 1 1 d . . .
H46 H 0.1052 0.5980 0.1325 0.085 Uiso 1 1 calc R . .
C47 C 0.1617(6) 0.5231(5) 0.1938(6) 0.050(3) Uani 1 1 d . . .
H47 H 0.1964 0.5247 0.1723 0.060 Uiso 1 1 calc R . .
C48 C 0.3530(6) 0.2971(6) 0.5163(8) 0.065(4) Uani 1 1 d . . .
H48 H 0.3865 0.3188 0.5025 0.079 Uiso 1 1 calc R . .
C49 C 0.3063(8) 0.2516(6) 0.4728(7) 0.061(3) Uani 1 1 d . . .
H49 H 0.3011 0.2367 0.4225 0.073 Uiso 1 1 calc R . .
C50 C 0.2682(6) 0.2306(5) 0.5137(8) 0.062(4) Uani 1 1 d . . .
H50 H 0.2334 0.1982 0.4973 0.075 Uiso 1 1 calc R . .
C51 C 0.2892(7) 0.2648(6) 0.5820(7) 0.058(3) Uani 1 1 d . . .
H51 H 0.2710 0.2613 0.6211 0.070 Uiso 1 1 calc R . .
C52 C 0.3423(7) 0.3055(6) 0.5831(7) 0.060(3) Uani 1 1 d . . .
H52 H 0.3672 0.3347 0.6240 0.073 Uiso 1 1 calc R . .
C53 C 0.1514(11) 0.3844(7) 0.5348(12) 0.092(6) Uani 1 1 d . . .
H53 H 0.1179 0.3587 0.5439 0.111 Uiso 1 1 calc R . .
C54 C 0.2246(13) 0.3937(7) 0.5875(9) 0.093(6) Uani 1 1 d . . .
H54 H 0.2495 0.3753 0.6387 0.111 Uiso 1 1 calc R . .
C55 C 0.2559(9) 0.4350(6) 0.5524(7) 0.071(4) Uani 1 1 d . . .
H55 H 0.3054 0.4485 0.5748 0.086 Uiso 1 1 calc R . .
C56 C 0.2000(8) 0.4523(6) 0.4782(6) 0.067(4) Uani 1 1 d . . .
H56 H 0.2048 0.4811 0.4424 0.080 Uiso 1 1 calc R . .
C57 C 0.1355(8) 0.4200(7) 0.4654(10) 0.076(4) Uani 1 1 d . . .
H57 H 0.0901 0.4217 0.4189 0.091 Uiso 1 1 calc R . .
C58 C -0.1386(10) 0.2273(8) 0.4564(10) 0.105(6) Uani 1 1 d D . .
H58 H -0.1630 0.2185 0.4887 0.126 Uiso 1 1 calc R . .
C59 C -0.0669(11) 0.2325(9) 0.4869(10) 0.102(6) Uani 1 1 d . . .
H59 H -0.0394 0.2264 0.5428 0.123 Uiso 1 1 calc R . .
C60 C -0.0321(8) 0.2452(8) 0.4452(11) 0.090(5) Uani 1 1 d . . .
H60 H 0.0196 0.2497 0.4713 0.108 Uiso 1 1 calc R . .
C61 C -0.0660(10) 0.2521(12) 0.3688(11) 0.127(8) Uani 1 1 d . . .
H61 H -0.0390 0.2608 0.3391 0.152 Uiso 1 1 calc R . .
C62 C -0.1387(10) 0.2472(12) 0.3313(10) 0.130(9) Uani 1 1 d . . .
H62 H -0.1619 0.2519 0.2748 0.156 Uiso 1 1 calc R . .
C63 C -0.1797(8) 0.2363(8) 0.3676(10) 0.095(5) Uani 1 1 d D . .
H63 H -0.2317 0.2341 0.3401 0.114 Uiso 1 1 calc R . .
C64 C 0.1353(17) 0.5011(14) 0.7125(15) 0.174(12) Uani 1 1 d . . .
H64A H 0.1419 0.4991 0.7685 0.209 Uiso 1 1 calc R . .
H64B H 0.1315 0.4585 0.6924 0.209 Uiso 1 1 calc R . .
C65 C 0.1955(15) 0.5289(19) 0.711(2) 0.203(17) Uani 1 1 d . . .
H65A H 0.2305 0.4980 0.7091 0.244 Uiso 1 1 calc R . .
H65B H 0.2208 0.5554 0.7584 0.244 Uiso 1 1 calc R . .
C66 C 0.163(2) 0.5672(18) 0.634(3) 0.23(2) Uani 1 1 d . . .
H66A H 0.1802 0.6103 0.6442 0.279 Uiso 1 1 calc R . .
H66B H 0.1758 0.5496 0.5924 0.279 Uiso 1 1 calc R . .
C67 C 0.085(2) 0.5625(19) 0.6115(17) 0.24(2) Uani 1 1 d . . .
H67A H 0.0644 0.6044 0.6033 0.289 Uiso 1 1 calc R . .
H67B H 0.0618 0.5406 0.5598 0.289 Uiso 1 1 calc R . .
C68 C 0.045(4) 0.5985(19) 0.407(2) 0.24(3) Uani 1 1 d . . .
H68 H 0.0522 0.5585 0.4295 0.287 Uiso 1 1 calc R . .
C69 C 0.0989(15) 0.6251(18) 0.401(3) 0.20(2) Uani 1 1 d . . .
H69 H 0.1488 0.6165 0.4349 0.243 Uiso 1 1 calc R . .
C70 C 0.077(2) 0.6673(16) 0.339(2) 0.171(11) Uani 1 1 d . . .
H70 H 0.1107 0.6894 0.3263 0.206 Uiso 1 1 calc R . .
C71 C 0.002(2) 0.6752(12) 0.2973(13) 0.138(10) Uani 1 1 d . . .
H71 H -0.0217 0.7007 0.2516 0.166 Uiso 1 1 calc R . .
C72 C -0.0322(14) 0.6436(15) 0.329(2) 0.176(17) Uani 1 1 d . . .
H72 H -0.0840 0.6411 0.3002 0.211 Uiso 1 1 calc R . .
C73 C 0.5272(9) 0.4602(7) 0.3204(8) 0.076(4) Uani 1 1 d . . .
H73 H 0.5137 0.4269 0.3443 0.091 Uiso 1 1 calc R . .
C74 C 0.4984(8) 0.5151(8) 0.3166(8) 0.075(4) Uani 1 1 d . . .
H74 H 0.4648 0.5219 0.3389 0.090 Uiso 1 1 calc R . .
C75 C 0.5170(9) 0.5618(8) 0.2808(13) 0.112(7) Uani 1 1 d . . .
H75 H 0.4954 0.6011 0.2768 0.135 Uiso 1 1 calc R . .
C76 C 0.5633(14) 0.5533(12) 0.2525(15) 0.137(9) Uani 1 1 d . . .
H76 H 0.5785 0.5870 0.2309 0.164 Uiso 1 1 calc R . .
C77 C 0.5898(11) 0.4996(14) 0.2527(13) 0.120(7) Uani 1 1 d . . .
H77 H 0.6199 0.4935 0.2260 0.144 Uiso 1 1 calc R . .
C78 C 0.5673(10) 0.2577(10) 0.1760(12) 0.102(5) Uani 1 1 d . . .
H78 H 0.5451 0.2198 0.1783 0.122 Uiso 1 1 calc R . .
C79 C 0.5323(9) 0.2944(8) 0.1130(11) 0.090(5) Uani 1 1 d . . .
H79 H 0.4826 0.2878 0.0764 0.108 Uiso 1 1 calc R . .
C80 C 0.5712(11) 0.3409(11) 0.1043(12) 0.110(6) Uani 1 1 d . . .
H80 H 0.5513 0.3619 0.0546 0.132 Uiso 1 1 calc R . .
C81 C 0.6339(14) 0.3596(11) 0.1585(14) 0.128(7) Uani 1 1 d . . .
H81 H 0.6584 0.3951 0.1531 0.153 Uiso 1 1 calc R . .
C82 C 0.6608(10) 0.3223(10) 0.2246(12) 0.101(5) Uani 1 1 d . . .
H82 H 0.7058 0.3344 0.2674 0.121 Uiso 1 1 calc R . .
N1 N 0.2930(4) 0.2883(3) 0.2760(4) 0.0259(15) Uani 1 1 d . . .
N2 N 0.1517(4) 0.3384(4) 0.2048(4) 0.0323(17) Uani 1 1 d . . .
N3 N 0.1176(4) 0.4060(4) 0.0709(4) 0.0332(17) Uani 1 1 d . . .
N4 N 0.2288(4) 0.4272(4) 0.0256(4) 0.0353(17) Uani 1 1 d . . .
H4 H 0.2427 0.4320 0.0772 0.042 Uiso 1 1 calc R . .
N5 N 0.3361(4) 0.5300(4) 0.1349(4) 0.0368(18) Uani 1 1 d . . .
H5A H 0.3300 0.4990 0.1618 0.044 Uiso 1 1 calc R . .
N6 N 0.3170(4) 0.5717(3) 0.2693(4) 0.0304(16) Uani 1 1 d . . .
N7 N 0.3422(4) 0.4881(3) 0.3899(4) 0.0275(15) Uani 1 1 d . . .
N8 N 0.4002(4) 0.3728(3) 0.3804(4) 0.0282(16) Uani 1 1 d . . .
N9 N 0.1697(4) 0.4802(3) 0.2467(5) 0.0355(18) Uani 1 1 d . . .
N10 N -0.005(3) 0.618(3) 0.389(6) 0.43(6) Uani 1 1 d . . .
N11 N 0.5757(11) 0.4516(10) 0.2900(11) 0.142(7) Uani 1 1 d . . .
N12 N 0.6310(9) 0.2718(7) 0.2349(8) 0.096(4) Uani 1 1 d . . .
O1 O 0.2926(3) 0.4245(3) 0.2098(4) 0.0340(14) Uani 1 1 d . . .
O2 O 0.2468(3) 0.3744(3) 0.3800(3) 0.0320(14) Uani 1 1 d . . .
O3 O 0.0686(10) 0.5334(11) 0.6649(12) 0.184(7) Uani 1 1 d . . .
Zr1 Zr 0.22795(5) 0.33940(4) 0.47067(5) 0.0359(2) Uani 1 1 d . . .
U1 U 0.272236(16) 0.398376(15) 0.291525(17) 0.02474(11) Uani 1 1 d . . .
Cl1 Cl 0.11634(16) 0.28289(18) 0.38882(19) 0.0752(10) Uani 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.343(11) . ?
C1 C2 1.403(13) . ?
C1 C40 1.511(13) . ?
C2 C3 1.394(13) . ?
C2 H2 0.9500 . ?
C3 C4 1.385(13) . ?
C3 H3 0.9500 . ?
C4 N1 1.385(10) . ?
C4 C5 1.410(12) . ?
C5 N2 1.291(11) . ?
C5 H5 0.9500 . ?
C6 C7 1.381(13) . ?
C6 C13 1.396(13) . ?
C6 N2 1.436(11) . ?
C7 C8 1.382(14) . ?
C7 H7 0.9500 . ?
C8 C10 1.392(15) . ?
C8 C9 1.501(15) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C12 1.384(14) . ?
C10 C11 1.515(14) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.376(13) . ?
C12 H12 0.9500 . ?
C13 N3 1.418(12) . ?
C14 N3 1.267(12) . ?
C14 C15 1.444(14) . ?
C14 H14 0.9500 . ?
C15 N4 1.360(12) . ?
C15 C16 1.366(14) . ?
C16 C17 1.396(16) . ?
C16 H16 0.9500 . ?
C17 C18 1.373(13) . ?
C17 H17 0.9500 . ?
C18 N4 1.367(12) . ?
C18 C19 1.515(14) . ?
C19 C22 1.519(15) . ?
C19 C20 1.530(13) . ?
C19 C21 1.548(15) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.361(15) . ?
C22 N5 1.368(12) . ?
C23 C24 1.387(16) . ?
C23 H23 0.9500 . ?
C24 C25 1.370(14) . ?
C24 H24 0.9500 . ?
C25 N5 1.372(12) . ?
C25 C26 1.433(14) . ?
C26 N6 1.273(11) . ?
C26 H26 0.9500 . ?
C27 C34 1.388(12) . ?
C27 C28 1.400(13) . ?
C27 N6 1.422(11) . ?
C28 C29 1.362(14) . ?
C28 H28 0.9500 . ?
C29 C31 1.404(15) . ?
C29 C30 1.503(15) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C33 1.379(14) . ?
C31 C32 1.514(14) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.385(13) . ?
C33 H33 0.9500 . ?
C34 N7 1.437(11) . ?
C35 N7 1.297(10) . ?
C35 C36 1.413(13) . ?
C35 H35 0.9500 . ?
C36 C37 1.374(12) . ?
C36 N8 1.380(11) . ?
C37 C38 1.387(13) . ?
C37 H37 0.9500 . ?
C38 C39 1.392(12) . ?
C38 H38 0.9500 . ?
C39 N8 1.361(11) . ?
C39 C40 1.511(13) . ?
C40 C42 1.532(14) . ?
C40 C41 1.537(13) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 N9 1.341(14) . ?
C43 C44 1.384(17) . ?
C43 H43 0.9500 . ?
C44 C45 1.35(2) . ?
C44 H44 0.9500 . ?
C45 C46 1.35(2) . ?
C45 H45 0.9500 . ?
C46 C47 1.372(16) . ?
C46 H46 0.9500 . ?
C47 N9 1.314(13) . ?
C47 H47 0.9500 . ?
C48 C52 1.364(17) . ?
C48 C49 1.365(18) . ?
C48 Zr1 2.475(11) . ?
C48 H48 0.9500 . ?
C49 C50 1.376(17) . ?
C49 Zr1 2.476(11) . ?
C49 H49 0.9500 . ?
C50 C51 1.370(17) . ?
C50 Zr1 2.520(11) . ?
C50 H50 0.9500 . ?
C51 C52 1.388(17) . ?
C51 Zr1 2.495(10) . ?
C51 H51 0.9500 . ?
C52 Zr1 2.462(11) . ?
C52 H52 0.9500 . ?
C53 C54 1.39(2) . ?
C53 C57 1.42(2) . ?
C53 Zr1 2.531(13) . ?
C53 H53 0.9500 . ?
C54 C55 1.41(2) . ?
C54 Zr1 2.499(13) . ?
C54 H54 0.9500 . ?
C55 C56 1.402(16) . ?
C55 Zr1 2.493(13) . ?
C55 H55 0.9500 . ?
C56 C57 1.410(19) . ?
C56 Zr1 2.541(11) . ?
C56 H56 0.9500 . ?
C57 Zr1 2.538(12) . ?
C57 H57 0.9500 . ?
C58 C59 1.31(2) . ?
C58 C63 1.503(9) . ?
C58 H58 0.9500 . ?
C59 C60 1.28(2) . ?
C59 H59 0.9500 . ?
C60 C61 1.29(2) . ?
C60 H60 0.9500 . ?
C61 C62 1.33(2) . ?
C61 H61 0.9500 . ?
C62 C63 1.30(2) . ?
C62 H62 0.9500 . ?
C63 H63 0.9500 . ?
C64 C65 1.37(3) . ?
C64 O3 1.44(3) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 C66 1.53(4) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 C67 1.45(4) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C67 O3 1.34(3) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C68 N10 1.00(9) . ?
C68 C69 1.29(5) . ?
C68 C72 1.88(7) . ?
C68 H68 0.9500 . ?
C69 C70 1.38(4) . ?
C69 H69 0.9500 . ?
C70 C71 1.39(4) . ?
C70 H70 0.9500 . ?
C71 C72 1.28(4) . ?
C71 H71 0.9500 . ?
C72 N10 1.17(10) . ?
C72 H72 0.9500 . ?
C73 C74 1.32(2) . ?
C73 N11 1.34(2) . ?
C73 H73 0.9500 . ?
C74 C75 1.36(2) . ?
C74 H74 0.9500 . ?
C75 C76 1.27(3) . ?
C75 H75 0.9500 . ?
C76 C77 1.28(3) . ?
C76 H76 0.9500 . ?
C77 N11 1.35(3) . ?
C77 H77 0.9500 . ?
C78 N12 1.32(2) . ?
C78 C79 1.34(2) . ?
C78 H78 0.9500 . ?
C79 C80 1.33(2) . ?
C79 H79 0.9500 . ?
C80 C81 1.30(3) . ?
C80 H80 0.9500 . ?
C81 C82 1.37(3) . ?
C81 H81 0.9500 . ?
C82 N12 1.31(2) . ?
C82 H82 0.9500 . ?
N1 U1 2.472(7) . ?
N2 U1 2.617(7) . ?
N4 H4 0.8800 . ?
N5 H5A 0.8800 . ?
N7 U1 2.629(7) . ?
N8 U1 2.456(7) . ?
N9 U1 2.585(7) . ?
O1 U1 1.830(6) . ?
O2 U1 1.996(6) . ?
O2 Zr1 2.030(6) . ?
Zr1 Cl1 2.439(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 109.3(8) . . ?
N1 C1 C40 122.0(8) . . ?
C2 C1 C40 128.5(8) . . ?
C3 C2 C1 107.5(8) . . ?
C3 C2 H2 126.3 . . ?
C1 C2 H2 126.3 . . ?
C4 C3 C2 106.0(8) . . ?
C4 C3 H3 127.0 . . ?
C2 C3 H3 127.0 . . ?
C3 C4 N1 109.9(8) . . ?
C3 C4 C5 130.4(8) . . ?
N1 C4 C5 119.6(8) . . ?
N2 C5 C4 123.0(8) . . ?
N2 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
C7 C6 C13 118.9(9) . . ?
C7 C6 N2 123.2(8) . . ?
C13 C6 N2 117.9(8) . . ?
C6 C7 C8 122.0(9) . . ?
C6 C7 H7 119.0 . . ?
C8 C7 H7 119.0 . . ?
C7 C8 C10 119.0(9) . . ?
C7 C8 C9 120.0(10) . . ?
C10 C8 C9 121.0(10) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C12 C10 C8 118.9(9) . . ?
C12 C10 C11 119.5(10) . . ?
C8 C10 C11 121.6(10) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C10 122.0(9) . . ?
C13 C12 H12 119.0 . . ?
C10 C12 H12 119.0 . . ?
C12 C13 C6 119.0(9) . . ?
C12 C13 N3 124.1(9) . . ?
C6 C13 N3 116.8(8) . . ?
N3 C14 C15 120.7(8) . . ?
N3 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
N4 C15 C16 107.7(9) . . ?
N4 C15 C14 119.7(8) . . ?
C16 C15 C14 132.5(9) . . ?
C15 C16 C17 107.4(9) . . ?
C15 C16 H16 126.3 . . ?
C17 C16 H16 126.3 . . ?
C18 C17 C16 108.3(9) . . ?
C18 C17 H17 125.9 . . ?
C16 C17 H17 125.9 . . ?
N4 C18 C17 106.6(9) . . ?
N4 C18 C19 121.7(8) . . ?
C17 C18 C19 131.7(9) . . ?
C18 C19 C22 109.6(8) . . ?
C18 C19 C20 110.1(8) . . ?
C22 C19 C20 109.2(10) . . ?
C18 C19 C21 109.0(9) . . ?
C22 C19 C21 110.4(8) . . ?
C20 C19 C21 108.5(9) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 N5 106.7(10) . . ?
C23 C22 C19 131.3(9) . . ?
N5 C22 C19 121.9(9) . . ?
C22 C23 C24 108.5(10) . . ?
C22 C23 H23 125.7 . . ?
C24 C23 H23 125.7 . . ?
C25 C24 C23 108.2(10) . . ?
C25 C24 H24 125.9 . . ?
C23 C24 H24 125.9 . . ?
C24 C25 N5 106.4(9) . . ?
C24 C25 C26 131.2(9) . . ?
N5 C25 C26 122.3(8) . . ?
N6 C26 C25 121.7(9) . . ?
N6 C26 H26 119.1 . . ?
C25 C26 H26 119.1 . . ?
C34 C27 C28 118.6(8) . . ?
C34 C27 N6 117.1(8) . . ?
C28 C27 N6 124.2(8) . . ?
C29 C28 C27 122.3(10) . . ?
C29 C28 H28 118.8 . . ?
C27 C28 H28 118.8 . . ?
C28 C29 C31 119.2(10) . . ?
C28 C29 C30 120.5(10) . . ?
C31 C29 C30 120.3(10) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C33 C31 C29 118.5(9) . . ?
C33 C31 C32 120.9(10) . . ?
C29 C31 C32 120.6(10) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 C34 122.5(9) . . ?
C31 C33 H33 118.8 . . ?
C34 C33 H33 118.8 . . ?
C33 C34 C27 118.9(9) . . ?
C33 C34 N7 121.0(8) . . ?
C27 C34 N7 120.1(8) . . ?
N7 C35 C36 123.4(8) . . ?
N7 C35 H35 118.3 . . ?
C36 C35 H35 118.3 . . ?
C37 C36 N8 110.7(8) . . ?
C37 C36 C35 129.3(8) . . ?
N8 C36 C35 119.5(8) . . ?
C36 C37 C38 106.5(8) . . ?
C36 C37 H37 126.7 . . ?
C38 C37 H37 126.7 . . ?
C37 C38 C39 107.0(8) . . ?
C37 C38 H38 126.5 . . ?
C39 C38 H38 126.5 . . ?
N8 C39 C38 110.1(8) . . ?
N8 C39 C40 120.6(7) . . ?
C38 C39 C40 129.2(8) . . ?
C39 C40 C1 111.1(7) . . ?
C39 C40 C42 108.2(8) . . ?
C1 C40 C42 109.1(7) . . ?
C39 C40 C41 109.8(8) . . ?
C1 C40 C41 110.1(8) . . ?
C42 C40 C41 108.5(8) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N9 C43 C44 122.1(13) . . ?
N9 C43 H43 119.0 . . ?
C44 C43 H43 119.0 . . ?
C45 C44 C43 118.8(15) . . ?
C45 C44 H44 120.6 . . ?
C43 C44 H44 120.6 . . ?
C44 C45 C46 120.0(14) . . ?
C44 C45 H45 120.0 . . ?
C46 C45 H45 120.0 . . ?
C45 C46 C47 117.8(14) . . ?
C45 C46 H46 121.1 . . ?
C47 C46 H46 121.1 . . ?
N9 C47 C46 124.3(12) . . ?
N9 C47 H47 117.8 . . ?
C46 C47 H47 117.8 . . ?
C52 C48 C49 107.0(11) . . ?
C52 C48 Zr1 73.5(7) . . ?
C49 C48 Zr1 74.1(7) . . ?
C52 C48 H48 126.5 . . ?
C49 C48 H48 126.5 . . ?
Zr1 C48 H48 118.0 . . ?
C48 C49 C50 109.0(11) . . ?
C48 C49 Zr1 73.9(7) . . ?
C50 C49 Zr1 75.7(7) . . ?
C48 C49 H49 125.5 . . ?
C50 C49 H49 125.5 . . ?
Zr1 C49 H49 116.8 . . ?
C51 C50 C49 108.0(11) . . ?
C51 C50 Zr1 73.1(7) . . ?
C49 C50 Zr1 72.3(6) . . ?
C51 C50 H50 126.0 . . ?
C49 C50 H50 126.0 . . ?
Zr1 C50 H50 120.4 . . ?
C50 C51 C52 106.7(11) . . ?
C50 C51 Zr1 75.2(6) . . ?
C52 C51 Zr1 72.5(6) . . ?
C50 C51 H51 126.7 . . ?
C52 C51 H51 126.7 . . ?
Zr1 C51 H51 117.8 . . ?
C48 C52 C51 109.3(11) . . ?
C48 C52 Zr1 74.5(6) . . ?
C51 C52 Zr1 75.0(6) . . ?
C48 C52 H52 125.4 . . ?
C51 C52 H52 125.4 . . ?
Zr1 C52 H52 117.0 . . ?
C54 C53 C57 108.0(14) . . ?
C54 C53 Zr1 72.7(8) . . ?
C57 C53 Zr1 74.0(7) . . ?
C54 C53 H53 126.0 . . ?
C57 C53 H53 126.0 . . ?
Zr1 C53 H53 119.2 . . ?
C53 C54 C55 108.9(13) . . ?
C53 C54 Zr1 75.2(9) . . ?
C55 C54 Zr1 73.3(7) . . ?
C53 C54 H54 125.5 . . ?
C55 C54 H54 125.5 . . ?
Zr1 C54 H54 117.8 . . ?
C56 C55 C54 107.0(15) . . ?
C56 C55 Zr1 75.7(7) . . ?
C54 C55 Zr1 73.8(8) . . ?
C56 C55 H55 126.5 . . ?
C54 C55 H55 126.5 . . ?
Zr1 C55 H55 116.2 . . ?
C55 C56 C57 109.0(12) . . ?
C55 C56 Zr1 71.9(7) . . ?
C57 C56 Zr1 73.8(7) . . ?
C55 C56 H56 125.5 . . ?
C57 C56 H56 125.5 . . ?
Zr1 C56 H56 120.5 . . ?
C56 C57 C53 107.1(15) . . ?
C56 C57 Zr1 74.0(7) . . ?
C53 C57 Zr1 73.5(7) . . ?
C56 C57 H57 126.5 . . ?
C53 C57 H57 126.5 . . ?
Zr1 C57 H57 118.1 . . ?
C59 C58 C63 116.3(14) . . ?
C59 C58 H58 121.8 . . ?
C63 C58 H58 121.8 . . ?
C60 C59 C58 123.6(17) . . ?
C60 C59 H59 118.2 . . ?
C58 C59 H59 118.2 . . ?
C59 C60 C61 121.3(17) . . ?
C59 C60 H60 119.3 . . ?
C61 C60 H60 119.3 . . ?
C60 C61 C62 120.3(17) . . ?
C60 C61 H61 119.9 . . ?
C62 C61 H61 119.9 . . ?
C63 C62 C61 123.8(17) . . ?
C63 C62 H62 118.1 . . ?
C61 C62 H62 118.1 . . ?
C62 C63 C58 114.7(14) . . ?
C62 C63 H63 122.6 . . ?
C58 C63 H63 122.6 . . ?
C65 C64 O3 112(3) . . ?
C65 C64 H64A 109.2 . . ?
O3 C64 H64A 109.2 . . ?
C65 C64 H64B 109.2 . . ?
O3 C64 H64B 109.2 . . ?
H64A C64 H64B 107.9 . . ?
C64 C65 C66 104(3) . . ?
C64 C65 H65A 111.0 . . ?
C66 C65 H65A 111.0 . . ?
C64 C65 H65B 111.0 . . ?
C66 C65 H65B 111.0 . . ?
H65A C65 H65B 109.0 . . ?
C67 C66 C65 101(2) . . ?
C67 C66 H66A 111.5 . . ?
C65 C66 H66A 111.5 . . ?
C67 C66 H66B 111.5 . . ?
C65 C66 H66B 111.5 . . ?
H66A C66 H66B 109.3 . . ?
O3 C67 C66 115(3) . . ?
O3 C67 H67A 108.6 . . ?
C66 C67 H67A 108.6 . . ?
O3 C67 H67B 108.6 . . ?
C66 C67 H67B 108.6 . . ?
H67A C67 H67B 107.6 . . ?
N10 C68 C69 124(7) . . ?
N10 C68 C72 32(6) . . ?
C69 C68 C72 99(3) . . ?
N10 C68 H68 118.1 . . ?
C69 C68 H68 118.1 . . ?
C72 C68 H68 137.7 . . ?
C68 C69 C70 113(3) . . ?
C68 C69 H69 123.5 . . ?
C70 C69 H69 123.5 . . ?
C69 C70 C71 115(3) . . ?
C69 C70 H70 122.4 . . ?
C71 C70 H70 122.4 . . ?
C72 C71 C70 111(2) . . ?
C72 C71 H71 124.6 . . ?
C70 C71 H71 124.6 . . ?
N10 C72 C71 125(4) . . ?
N10 C72 C68 27(3) . . ?
C71 C72 C68 102(3) . . ?
N10 C72 H72 117.4 . . ?
C71 C72 H72 117.4 . . ?
C68 C72 H72 138.1 . . ?
C74 C73 N11 119.4(16) . . ?
C74 C73 H73 120.3 . . ?
N11 C73 H73 120.3 . . ?
C73 C74 C75 119.6(16) . . ?
C73 C74 H74 120.2 . . ?
C75 C74 H74 120.2 . . ?
C76 C75 C74 120.4(19) . . ?
C76 C75 H75 119.8 . . ?
C74 C75 H75 119.8 . . ?
C75 C76 C77 121(2) . . ?
C75 C76 H76 119.6 . . ?
C77 C76 H76 119.6 . . ?
C76 C77 N11 122(2) . . ?
C76 C77 H77 119.2 . . ?
N11 C77 H77 119.2 . . ?
N12 C78 C79 122.9(19) . . ?
N12 C78 H78 118.6 . . ?
C79 C78 H78 118.6 . . ?
C80 C79 C78 116.3(18) . . ?
C80 C79 H79 121.9 . . ?
C78 C79 H79 121.9 . . ?
C81 C80 C79 125(2) . . ?
C81 C80 H80 117.4 . . ?
C79 C80 H80 117.4 . . ?
C80 C81 C82 112(2) . . ?
C80 C81 H81 123.8 . . ?
C82 C81 H81 123.8 . . ?
N12 C82 C81 127(2) . . ?
N12 C82 H82 116.5 . . ?
C81 C82 H82 116.5 . . ?
C1 N1 C4 107.3(7) . . ?
C1 N1 U1 135.6(5) . . ?
C4 N1 U1 114.5(5) . . ?
C5 N2 C6 117.5(7) . . ?
C5 N2 U1 111.6(5) . . ?
C6 N2 U1 129.8(6) . . ?
C14 N3 C13 118.7(8) . . ?
C15 N4 C18 110.0(8) . . ?
C15 N4 H4 125.0 . . ?
C18 N4 H4 125.0 . . ?
C22 N5 C25 110.1(8) . . ?
C22 N5 H5A 124.9 . . ?
C25 N5 H5A 124.9 . . ?
C26 N6 C27 120.4(8) . . ?
C35 N7 C34 116.3(7) . . ?
C35 N7 U1 110.6(6) . . ?
C34 N7 U1 132.2(5) . . ?
C39 N8 C36 105.7(7) . . ?
C39 N8 U1 137.3(6) . . ?
C36 N8 U1 115.0(6) . . ?
C47 N9 C43 116.8(9) . . ?
C47 N9 U1 123.5(7) . . ?
C43 N9 U1 119.3(7) . . ?
C68 N10 C72 121(9) . . ?
C73 N11 C77 117.7(19) . . ?
C82 N12 C78 115.0(17) . . ?
U1 O2 Zr1 172.4(3) . . ?
C67 O3 C64 102(2) . . ?
O2 Zr1 Cl1 97.53(19) . . ?
O2 Zr1 C52 111.6(4) . . ?
Cl1 Zr1 C52 130.7(3) . . ?
O2 Zr1 C48 83.6(3) . . ?
Cl1 Zr1 C48 124.0(4) . . ?
C52 Zr1 C48 32.1(4) . . ?
O2 Zr1 C49 87.2(3) . . ?
Cl1 Zr1 C49 92.0(4) . . ?
C52 Zr1 C49 52.8(4) . . ?
C48 Zr1 C49 32.0(4) . . ?
O2 Zr1 C55 96.7(3) . . ?
Cl1 Zr1 C55 134.7(4) . . ?
C52 Zr1 C55 81.6(4) . . ?
C48 Zr1 C55 100.1(5) . . ?
C49 Zr1 C55 131.4(5) . . ?
O2 Zr1 C51 136.6(3) . . ?
Cl1 Zr1 C51 100.4(3) . . ?
C52 Zr1 C51 32.5(4) . . ?
C48 Zr1 C51 53.7(4) . . ?
C49 Zr1 C51 53.1(4) . . ?
C55 Zr1 C51 98.0(4) . . ?
O2 Zr1 C54 129.0(4) . . ?
Cl1 Zr1 C54 114.3(5) . . ?
C52 Zr1 C54 77.1(5) . . ?
C48 Zr1 C54 106.9(6) . . ?
C49 Zr1 C54 127.7(5) . . ?
C55 Zr1 C54 32.9(5) . . ?
C51 Zr1 C54 77.3(4) . . ?
O2 Zr1 C50 117.6(4) . . ?
Cl1 Zr1 C50 78.9(3) . . ?
C52 Zr1 C50 52.7(4) . . ?
C48 Zr1 C50 53.1(4) . . ?
C49 Zr1 C50 32.0(4) . . ?
C55 Zr1 C50 129.5(4) . . ?
C51 Zr1 C50 31.7(4) . . ?
C54 Zr1 C50 107.3(5) . . ?
O2 Zr1 C53 128.4(4) . . ?
Cl1 Zr1 C53 84.0(5) . . ?
C52 Zr1 C53 105.1(6) . . ?
C48 Zr1 C53 136.9(6) . . ?
C49 Zr1 C53 144.4(4) . . ?
C55 Zr1 C53 54.0(6) . . ?
C51 Zr1 C53 92.7(5) . . ?
C54 Zr1 C53 32.1(6) . . ?
C50 Zr1 C53 113.3(5) . . ?
O2 Zr1 C57 96.4(3) . . ?
Cl1 Zr1 C57 81.7(4) . . ?
C52 Zr1 C57 130.3(5) . . ?
C48 Zr1 C57 154.2(6) . . ?
C49 Zr1 C57 173.1(5) . . ?
C55 Zr1 C57 54.1(5) . . ?
C51 Zr1 C57 125.1(4) . . ?
C54 Zr1 C57 53.6(6) . . ?
C50 Zr1 C57 142.6(4) . . ?
C53 Zr1 C57 32.5(5) . . ?
O2 Zr1 C56 79.0(3) . . ?
Cl1 Zr1 C56 110.7(3) . . ?
C52 Zr1 C56 113.2(4) . . ?
C48 Zr1 C56 124.2(5) . . ?
C49 Zr1 C56 154.7(5) . . ?
C55 Zr1 C56 32.3(4) . . ?
C51 Zr1 C56 128.8(4) . . ?
C54 Zr1 C56 53.3(4) . . ?
C50 Zr1 C56 160.3(4) . . ?
C53 Zr1 C56 53.3(5) . . ?
C57 Zr1 C56 32.2(4) . . ?
O1 U1 O2 176.7(3) . . ?
O1 U1 N8 94.3(2) . . ?
O2 U1 N8 87.9(2) . . ?
O1 U1 N1 95.4(3) . . ?
O2 U1 N1 87.7(2) . . ?
N8 U1 N1 71.0(2) . . ?
O1 U1 N9 87.7(3) . . ?
O2 U1 N9 89.2(2) . . ?
N8 U1 N9 147.0(2) . . ?
N1 U1 N9 141.7(2) . . ?
O1 U1 N2 97.6(2) . . ?
O2 U1 N2 82.5(2) . . ?
N8 U1 N2 136.9(2) . . ?
N1 U1 N2 66.7(2) . . ?
N9 U1 N2 75.0(2) . . ?
O1 U1 N7 95.6(2) . . ?
O2 U1 N7 82.9(2) . . ?
N8 U1 N7 67.0(2) . . ?
N1 U1 N7 137.2(2) . . ?
N9 U1 N7 80.0(2) . . ?
N2 U1 N7 151.1(2) . . ?

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
N1 C1 C2 C3 -1.1(10) . . . . ?
C40 C1 C2 C3 -175.9(8) . . . . ?
C1 C2 C3 C4 1.0(10) . . . . ?
C2 C3 C4 N1 -0.6(10) . . . . ?
C2 C3 C4 C5 174.9(9) . . . . ?
C3 C4 C5 N2 -178.7(9) . . . . ?
N1 C4 C5 N2 -3.5(13) . . . . ?
C13 C6 C7 C8 -1.3(15) . . . . ?
N2 C6 C7 C8 179.3(9) . . . . ?
C6 C7 C8 C10 -0.9(16) . . . . ?
C6 C7 C8 C9 179.7(11) . . . . ?
C7 C8 C10 C12 1.7(16) . . . . ?
C9 C8 C10 C12 -178.9(11) . . . . ?
C7 C8 C10 C11 -179.0(10) . . . . ?
C9 C8 C10 C11 0.4(17) . . . . ?
C8 C10 C12 C13 -0.2(16) . . . . ?
C11 C10 C12 C13 -179.5(10) . . . . ?
C10 C12 C13 C6 -2.0(15) . . . . ?
C10 C12 C13 N3 -179.9(9) . . . . ?
C7 C6 C13 C12 2.7(14) . . . . ?
N2 C6 C13 C12 -177.9(9) . . . . ?
C7 C6 C13 N3 -179.3(8) . . . . ?
N2 C6 C13 N3 0.2(13) . . . . ?
N3 C14 C15 N4 3.0(14) . . . . ?
N3 C14 C15 C16 -174.3(11) . . . . ?
N4 C15 C16 C17 -1.3(13) . . . . ?
C14 C15 C16 C17 176.2(11) . . . . ?
C15 C16 C17 C18 1.1(14) . . . . ?
C16 C17 C18 N4 -0.5(13) . . . . ?
C16 C17 C18 C19 -179.0(11) . . . . ?
N4 C18 C19 C22 -60.8(12) . . . . ?
C17 C18 C19 C22 117.5(12) . . . . ?
N4 C18 C19 C20 179.0(10) . . . . ?
C17 C18 C19 C20 -2.6(17) . . . . ?
N4 C18 C19 C21 60.0(12) . . . . ?
C17 C18 C19 C21 -121.6(12) . . . . ?
C18 C19 C22 C23 -101.8(13) . . . . ?
C20 C19 C22 C23 18.9(16) . . . . ?
C21 C19 C22 C23 138.2(12) . . . . ?
C18 C19 C22 N5 75.0(11) . . . . ?
C20 C19 C22 N5 -164.2(9) . . . . ?
C21 C19 C22 N5 -45.0(13) . . . . ?
N5 C22 C23 C24 0.2(13) . . . . ?
C19 C22 C23 C24 177.4(11) . . . . ?
C22 C23 C24 C25 0.0(13) . . . . ?
C23 C24 C25 N5 -0.2(12) . . . . ?
C23 C24 C25 C26 176.9(11) . . . . ?
C24 C25 C26 N6 -179.9(11) . . . . ?
N5 C25 C26 N6 -3.2(15) . . . . ?
C34 C27 C28 C29 0.9(14) . . . . ?
N6 C27 C28 C29 -175.5(9) . . . . ?
C27 C28 C29 C31 -1.2(15) . . . . ?
C27 C28 C29 C30 178.0(10) . . . . ?
C28 C29 C31 C33 0.2(15) . . . . ?
C30 C29 C31 C33 -179.0(10) . . . . ?
C28 C29 C31 C32 179.4(10) . . . . ?
C30 C29 C31 C32 0.2(16) . . . . ?
C29 C31 C33 C34 1.0(15) . . . . ?
C32 C31 C33 C34 -178.2(10) . . . . ?
C31 C33 C34 C27 -1.3(14) . . . . ?
C31 C33 C34 N7 175.9(8) . . . . ?
C28 C27 C34 C33 0.4(12) . . . . ?
N6 C27 C34 C33 177.0(8) . . . . ?
C28 C27 C34 N7 -176.9(8) . . . . ?
N6 C27 C34 N7 -0.3(11) . . . . ?
N7 C35 C36 C37 174.2(9) . . . . ?
N7 C35 C36 N8 2.4(13) . . . . ?
N8 C36 C37 C38 -1.4(11) . . . . ?
C35 C36 C37 C38 -173.7(9) . . . . ?
C36 C37 C38 C39 1.0(11) . . . . ?
C37 C38 C39 N8 -0.2(11) . . . . ?
C37 C38 C39 C40 176.5(9) . . . . ?
N8 C39 C40 C1 -51.6(11) . . . . ?
C38 C39 C40 C1 131.9(10) . . . . ?
N8 C39 C40 C42 68.1(11) . . . . ?
C38 C39 C40 C42 -108.4(11) . . . . ?
N8 C39 C40 C41 -173.7(9) . . . . ?
C38 C39 C40 C41 9.9(14) . . . . ?
N1 C1 C40 C39 54.4(11) . . . . ?
C2 C1 C40 C39 -131.3(9) . . . . ?
N1 C1 C40 C42 -64.7(10) . . . . ?
C2 C1 C40 C42 109.5(10) . . . . ?
N1 C1 C40 C41 176.3(8) . . . . ?
C2 C1 C40 C41 -9.4(13) . . . . ?
N9 C43 C44 C45 1(2) . . . . ?
C43 C44 C45 C46 -1(3) . . . . ?
C44 C45 C46 C47 2(2) . . . . ?
C45 C46 C47 N9 -5.1(19) . . . . ?
C52 C48 C49 C50 -1.7(13) . . . . ?
Zr1 C48 C49 C50 -68.3(8) . . . . ?
C52 C48 C49 Zr1 66.6(8) . . . . ?
C48 C49 C50 C51 2.1(14) . . . . ?
Zr1 C49 C50 C51 -64.9(9) . . . . ?
C48 C49 C50 Zr1 67.1(8) . . . . ?
C49 C50 C51 C52 -1.7(13) . . . . ?
Zr1 C50 C51 C52 -66.1(8) . . . . ?
C49 C50 C51 Zr1 64.4(8) . . . . ?
C49 C48 C52 C51 0.6(13) . . . . ?
Zr1 C48 C52 C51 67.6(8) . . . . ?
C49 C48 C52 Zr1 -67.0(8) . . . . ?
C50 C51 C52 C48 0.7(13) . . . . ?
Zr1 C51 C52 C48 -67.2(8) . . . . ?
C50 C51 C52 Zr1 68.0(8) . . . . ?
C57 C53 C54 C55 0.0(17) . . . . ?
Zr1 C53 C54 C55 66.1(9) . . . . ?
C57 C53 C54 Zr1 -66.1(10) . . . . ?
C53 C54 C55 C56 1.7(15) . . . . ?
Zr1 C54 C55 C56 69.1(8) . . . . ?
C53 C54 C55 Zr1 -67.4(11) . . . . ?
C54 C55 C56 C57 -2.8(14) . . . . ?
Zr1 C55 C56 C57 65.0(9) . . . . ?
C54 C55 C56 Zr1 -67.8(9) . . . . ?
C55 C56 C57 C53 2.8(15) . . . . ?
Zr1 C56 C57 C53 66.6(9) . . . . ?
C55 C56 C57 Zr1 -63.8(9) . . . . ?
C54 C53 C57 C56 -1.7(16) . . . . ?
Zr1 C53 C57 C56 -67.0(9) . . . . ?
C54 C53 C57 Zr1 65.2(10) . . . . ?
C63 C58 C59 C60 1(3) . . . . ?
C58 C59 C60 C61 -2(4) . . . . ?
C59 C60 C61 C62 1(4) . . . . ?
C60 C61 C62 C63 1(4) . . . . ?
C61 C62 C63 C58 -2(4) . . . . ?
C59 C58 C63 C62 1(3) . . . . ?
O3 C64 C65 C66 -22(4) . . . . ?
C64 C65 C66 C67 10(4) . . . . ?
C65 C66 C67 O3 6(5) . . . . ?
N10 C68 C69 C70 -27(9) . . . . ?
C72 C68 C69 C70 -5(4) . . . . ?
C68 C69 C70 C71 2(5) . . . . ?
C69 C70 C71 C72 4(4) . . . . ?
C70 C71 C72 N10 9(8) . . . . ?
C70 C71 C72 C68 -6(4) . . . . ?
C69 C68 C72 N10 -145(11) . . . . ?
N10 C68 C72 C71 152(11) . . . . ?
C69 C68 C72 C71 7(4) . . . . ?
N11 C73 C74 C75 1(2) . . . . ?
C73 C74 C75 C76 -2(3) . . . . ?
C74 C75 C76 C77 4(4) . . . . ?
C75 C76 C77 N11 -7(4) . . . . ?
N12 C78 C79 C80 13(3) . . . . ?
C78 C79 C80 C81 -13(3) . . . . ?
C79 C80 C81 C82 6(3) . . . . ?
C80 C81 C82 N12 2(3) . . . . ?
C2 C1 N1 C4 0.7(9) . . . . ?
C40 C1 N1 C4 175.9(7) . . . . ?
C2 C1 N1 U1 160.1(6) . . . . ?
C40 C1 N1 U1 -24.6(12) . . . . ?
C3 C4 N1 C1 -0.1(9) . . . . ?
C5 C4 N1 C1 -176.2(7) . . . . ?
C3 C4 N1 U1 -164.4(6) . . . . ?
C5 C4 N1 U1 19.5(9) . . . . ?
C4 C5 N2 C6 177.5(8) . . . . ?
C4 C5 N2 U1 -13.3(11) . . . . ?
C7 C6 N2 C5 58.2(13) . . . . ?
C13 C6 N2 C5 -121.2(10) . . . . ?
C7 C6 N2 U1 -108.7(9) . . . . ?
C13 C6 N2 U1 71.8(11) . . . . ?
C15 C14 N3 C13 178.2(9) . . . . ?
C12 C13 N3 C14 -51.6(14) . . . . ?
C6 C13 N3 C14 130.5(10) . . . . ?
C16 C15 N4 C18 1.0(12) . . . . ?
C14 C15 N4 C18 -176.9(9) . . . . ?
C17 C18 N4 C15 -0.3(11) . . . . ?
C19 C18 N4 C15 178.4(9) . . . . ?
C23 C22 N5 C25 -0.3(12) . . . . ?
C19 C22 N5 C25 -177.8(9) . . . . ?
C24 C25 N5 C22 0.3(11) . . . . ?
C26 C25 N5 C22 -177.1(9) . . . . ?
C25 C26 N6 C27 -179.2(8) . . . . ?
C34 C27 N6 C26 -159.7(8) . . . . ?
C28 C27 N6 C26 16.7(13) . . . . ?
C36 C35 N7 C34 -175.7(8) . . . . ?
C36 C35 N7 U1 13.7(10) . . . . ?
C33 C34 N7 C35 -51.4(11) . . . . ?
C27 C34 N7 C35 125.8(8) . . . . ?
C33 C34 N7 U1 116.7(8) . . . . ?
C27 C34 N7 U1 -66.2(10) . . . . ?
C38 C39 N8 C36 -0.6(10) . . . . ?
C40 C39 N8 C36 -177.7(8) . . . . ?
C38 C39 N8 U1 -162.8(6) . . . . ?
C40 C39 N8 U1 20.2(13) . . . . ?
C37 C36 N8 C39 1.3(10) . . . . ?
C35 C36 N8 C39 174.4(8) . . . . ?
C37 C36 N8 U1 168.0(6) . . . . ?
C35 C36 N8 U1 -18.9(10) . . . . ?
C46 C47 N9 C43 5.6(16) . . . . ?
C46 C47 N9 U1 178.1(8) . . . . ?
C44 C43 N9 C47 -3.6(17) . . . . ?
C44 C43 N9 U1 -176.4(10) . . . . ?
C69 C68 N10 C72 43(12) . . . . ?
C71 C72 N10 C68 -34(13) . . . . ?
C74 C73 N11 C77 -4(3) . . . . ?
C76 C77 N11 C73 6(4) . . . . ?
C81 C82 N12 C78 -3(3) . . . . ?
C79 C78 N12 C82 -5(3) . . . . ?
C66 C67 O3 C64 -18(4) . . . . ?
C65 C64 O3 C67 25(4) . . . . ?
U1 O2 Zr1 Cl1 -86(3) . . . . ?
U1 O2 Zr1 C52 53(3) . . . . ?
U1 O2 Zr1 C48 37(3) . . . . ?
U1 O2 Zr1 C49 6(3) . . . . ?
U1 O2 Zr1 C55 137(3) . . . . ?
U1 O2 Zr1 C51 28(3) . . . . ?
U1 O2 Zr1 C54 144(3) . . . . ?
U1 O2 Zr1 C50 -5(3) . . . . ?
U1 O2 Zr1 C53 -174(3) . . . . ?
U1 O2 Zr1 C57 -169(3) . . . . ?
U1 O2 Zr1 C56 164(3) . . . . ?
C48 C52 Zr1 O2 -30.9(9) . . . . ?
C51 C52 Zr1 O2 -146.3(7) . . . . ?
C48 C52 Zr1 Cl1 90.9(9) . . . . ?
C51 C52 Zr1 Cl1 -24.5(9) . . . . ?
C51 C52 Zr1 C48 -115.4(11) . . . . ?
C48 C52 Zr1 C49 37.6(7) . . . . ?
C51 C52 Zr1 C49 -77.8(8) . . . . ?
C48 C52 Zr1 C55 -124.9(9) . . . . ?
C51 C52 Zr1 C55 119.7(8) . . . . ?
C48 C52 Zr1 C51 115.4(11) . . . . ?
C48 C52 Zr1 C54 -158.0(10) . . . . ?
C51 C52 Zr1 C54 86.6(9) . . . . ?
C48 C52 Zr1 C50 78.1(9) . . . . ?
C51 C52 Zr1 C50 -37.3(7) . . . . ?
C48 C52 Zr1 C53 -173.9(9) . . . . ?
C51 C52 Zr1 C53 70.7(8) . . . . ?
C48 C52 Zr1 C57 -150.4(8) . . . . ?
C51 C52 Zr1 C57 94.2(8) . . . . ?
C48 C52 Zr1 C56 -117.9(8) . . . . ?
C51 C52 Zr1 C56 126.7(8) . . . . ?
C52 C48 Zr1 O2 151.3(8) . . . . ?
C49 C48 Zr1 O2 -95.0(7) . . . . ?
C52 C48 Zr1 Cl1 -114.0(8) . . . . ?
C49 C48 Zr1 Cl1 -0.2(8) . . . . ?
C49 C48 Zr1 C52 113.7(10) . . . . ?
C52 C48 Zr1 C49 -113.7(10) . . . . ?
C52 C48 Zr1 C55 55.5(9) . . . . ?
C49 C48 Zr1 C55 169.3(7) . . . . ?
C52 C48 Zr1 C51 -37.1(7) . . . . ?
C49 C48 Zr1 C51 76.7(8) . . . . ?
C52 C48 Zr1 C54 22.4(9) . . . . ?
C49 C48 Zr1 C54 136.1(8) . . . . ?
C52 C48 Zr1 C50 -76.8(8) . . . . ?
C49 C48 Zr1 C50 36.9(7) . . . . ?
C52 C48 Zr1 C53 8.6(12) . . . . ?
C49 C48 Zr1 C53 122.3(9) . . . . ?
C52 C48 Zr1 C57 59.8(12) . . . . ?
C49 C48 Zr1 C57 173.6(9) . . . . ?
C52 C48 Zr1 C56 79.2(8) . . . . ?
C49 C48 Zr1 C56 -167.1(7) . . . . ?
C48 C49 Zr1 O2 82.4(7) . . . . ?
C50 C49 Zr1 O2 -162.7(8) . . . . ?
C48 C49 Zr1 Cl1 179.8(7) . . . . ?
C50 C49 Zr1 Cl1 -65.2(8) . . . . ?
C48 C49 Zr1 C52 -37.6(7) . . . . ?
C50 C49 Zr1 C52 77.3(8) . . . . ?
C50 C49 Zr1 C48 115.0(10) . . . . ?
C48 C49 Zr1 C55 -14.1(10) . . . . ?
C50 C49 Zr1 C55 100.8(9) . . . . ?
C48 C49 Zr1 C51 -78.7(8) . . . . ?
C50 C49 Zr1 C51 36.3(7) . . . . ?
C48 C49 Zr1 C54 -57.0(10) . . . . ?
C50 C49 Zr1 C54 58.0(11) . . . . ?
C48 C49 Zr1 C50 -115.0(10) . . . . ?
C48 C49 Zr1 C53 -97.6(13) . . . . ?
C50 C49 Zr1 C53 17.3(14) . . . . ?
C48 C49 Zr1 C57 -156(3) . . . . ?
C50 C49 Zr1 C57 -41(4) . . . . ?
C48 C49 Zr1 C56 25.5(12) . . . . ?
C50 C49 Zr1 C56 140.5(9) . . . . ?
C56 C55 Zr1 O2 57.0(9) . . . . ?
C54 C55 Zr1 O2 169.8(10) . . . . ?
C56 C55 Zr1 Cl1 -50.6(10) . . . . ?
C54 C55 Zr1 Cl1 62.2(11) . . . . ?
C56 C55 Zr1 C52 168.0(10) . . . . ?
C54 C55 Zr1 C52 -79.3(10) . . . . ?
C56 C55 Zr1 C48 141.7(9) . . . . ?
C54 C55 Zr1 C48 -105.5(10) . . . . ?
C56 C55 Zr1 C49 149.2(8) . . . . ?
C54 C55 Zr1 C49 -98.0(11) . . . . ?
C56 C55 Zr1 C51 -163.9(9) . . . . ?
C54 C55 Zr1 C51 -51.2(11) . . . . ?
C56 C55 Zr1 C54 -112.8(14) . . . . ?
C56 C55 Zr1 C50 -168.4(8) . . . . ?
C54 C55 Zr1 C50 -55.6(12) . . . . ?
C56 C55 Zr1 C53 -76.4(10) . . . . ?
C54 C55 Zr1 C53 36.4(9) . . . . ?
C56 C55 Zr1 C57 -36.0(8) . . . . ?
C54 C55 Zr1 C57 76.8(11) . . . . ?
C54 C55 Zr1 C56 112.8(14) . . . . ?
C50 C51 Zr1 O2 -64.7(10) . . . . ?
C52 C51 Zr1 O2 48.6(10) . . . . ?
C50 C51 Zr1 Cl1 48.1(8) . . . . ?
C52 C51 Zr1 Cl1 161.4(7) . . . . ?
C50 C51 Zr1 C52 -113.3(11) . . . . ?
C50 C51 Zr1 C48 -76.8(9) . . . . ?
C52 C51 Zr1 C48 36.5(8) . . . . ?
C50 C51 Zr1 C49 -36.6(8) . . . . ?
C52 C51 Zr1 C49 76.7(8) . . . . ?
C50 C51 Zr1 C55 -173.4(8) . . . . ?
C52 C51 Zr1 C55 -60.2(8) . . . . ?
C50 C51 Zr1 C54 160.9(10) . . . . ?
C52 C51 Zr1 C54 -85.8(9) . . . . ?
C52 C51 Zr1 C50 113.3(11) . . . . ?
C50 C51 Zr1 C53 132.5(9) . . . . ?
C52 C51 Zr1 C53 -114.2(9) . . . . ?
C50 C51 Zr1 C57 135.2(8) . . . . ?
C52 C51 Zr1 C57 -111.5(8) . . . . ?
C50 C51 Zr1 C56 175.6(8) . . . . ?
C52 C51 Zr1 C56 -71.1(9) . . . . ?
C53 C54 Zr1 O2 102.4(10) . . . . ?
C55 C54 Zr1 O2 -13.1(13) . . . . ?
C53 C54 Zr1 Cl1 -21.0(10) . . . . ?
C55 C54 Zr1 Cl1 -136.4(9) . . . . ?
C53 C54 Zr1 C52 -150.1(10) . . . . ?
C55 C54 Zr1 C52 94.4(10) . . . . ?
C53 C54 Zr1 C48 -162.1(9) . . . . ?
C55 C54 Zr1 C48 82.4(10) . . . . ?
C53 C54 Zr1 C49 -134.4(9) . . . . ?
C55 C54 Zr1 C49 110.1(9) . . . . ?
C53 C54 Zr1 C55 115.5(13) . . . . ?
C53 C54 Zr1 C51 -116.8(10) . . . . ?
C55 C54 Zr1 C51 127.8(11) . . . . ?
C53 C54 Zr1 C50 -106.4(9) . . . . ?
C55 C54 Zr1 C50 138.2(9) . . . . ?
C55 C54 Zr1 C53 -115.5(13) . . . . ?
C53 C54 Zr1 C57 37.1(9) . . . . ?
C55 C54 Zr1 C57 -78.4(9) . . . . ?
C53 C54 Zr1 C56 77.5(10) . . . . ?
C55 C54 Zr1 C56 -37.9(9) . . . . ?
C51 C50 Zr1 O2 135.5(8) . . . . ?
C49 C50 Zr1 O2 19.6(9) . . . . ?
C51 C50 Zr1 Cl1 -131.8(8) . . . . ?
C49 C50 Zr1 Cl1 112.4(8) . . . . ?
C51 C50 Zr1 C52 38.4(7) . . . . ?
C49 C50 Zr1 C52 -77.5(8) . . . . ?
C51 C50 Zr1 C48 78.9(8) . . . . ?
C49 C50 Zr1 C48 -37.0(7) . . . . ?
C51 C50 Zr1 C49 115.8(11) . . . . ?
C51 C50 Zr1 C55 8.4(11) . . . . ?
C49 C50 Zr1 C55 -107.4(9) . . . . ?
C49 C50 Zr1 C51 -115.8(11) . . . . ?
C51 C50 Zr1 C54 -19.6(10) . . . . ?
C49 C50 Zr1 C54 -135.4(9) . . . . ?
C51 C50 Zr1 C53 -53.3(10) . . . . ?
C49 C50 Zr1 C53 -169.1(9) . . . . ?
C51 C50 Zr1 C57 -71.6(11) . . . . ?
C49 C50 Zr1 C57 172.5(9) . . . . ?
C51 C50 Zr1 C56 -10.2(18) . . . . ?
C49 C50 Zr1 C56 -126.1(15) . . . . ?
C54 C53 Zr1 O2 -104.3(10) . . . . ?
C57 C53 Zr1 O2 11.0(14) . . . . ?
C54 C53 Zr1 Cl1 160.8(9) . . . . ?
C57 C53 Zr1 Cl1 -83.9(11) . . . . ?
C54 C53 Zr1 C52 30.2(10) . . . . ?
C57 C53 Zr1 C52 145.4(11) . . . . ?
C54 C53 Zr1 C48 25.5(13) . . . . ?
C57 C53 Zr1 C48 140.7(10) . . . . ?
C54 C53 Zr1 C49 75.7(13) . . . . ?
C57 C53 Zr1 C49 -169.0(10) . . . . ?
C54 C53 Zr1 C55 -37.3(8) . . . . ?
C57 C53 Zr1 C55 78.0(11) . . . . ?
C54 C53 Zr1 C51 60.7(10) . . . . ?
C57 C53 Zr1 C51 175.9(11) . . . . ?
C57 C53 Zr1 C54 115.2(15) . . . . ?
C54 C53 Zr1 C50 85.6(10) . . . . ?
C57 C53 Zr1 C50 -159.1(10) . . . . ?
C54 C53 Zr1 C57 -115.2(15) . . . . ?
C54 C53 Zr1 C56 -77.7(10) . . . . ?
C57 C53 Zr1 C56 37.5(9) . . . . ?
C56 C57 Zr1 O2 -57.6(8) . . . . ?
C53 C57 Zr1 O2 -171.4(11) . . . . ?
C56 C57 Zr1 Cl1 -154.3(8) . . . . ?
C53 C57 Zr1 Cl1 91.9(11) . . . . ?
C56 C57 Zr1 C52 67.9(9) . . . . ?
C53 C57 Zr1 C52 -45.9(13) . . . . ?
C56 C57 Zr1 C48 30.9(14) . . . . ?
C53 C57 Zr1 C48 -82.9(14) . . . . ?
C56 C57 Zr1 C49 -179(78) . . . . ?
C53 C57 Zr1 C49 67(4) . . . . ?
C56 C57 Zr1 C55 36.1(7) . . . . ?
C53 C57 Zr1 C55 -77.7(12) . . . . ?
C56 C57 Zr1 C51 108.8(8) . . . . ?
C53 C57 Zr1 C51 -5.0(14) . . . . ?
C56 C57 Zr1 C54 77.1(10) . . . . ?
C53 C57 Zr1 C54 -36.7(11) . . . . ?
C56 C57 Zr1 C50 146.4(7) . . . . ?
C53 C57 Zr1 C50 32.6(15) . . . . ?
C56 C57 Zr1 C53 113.8(15) . . . . ?
C53 C57 Zr1 C56 -113.8(15) . . . . ?
C55 C56 Zr1 O2 -121.9(9) . . . . ?
C57 C56 Zr1 O2 121.3(8) . . . . ?
C55 C56 Zr1 Cl1 144.1(8) . . . . ?
C57 C56 Zr1 Cl1 27.3(8) . . . . ?
C55 C56 Zr1 C52 -13.0(10) . . . . ?
C57 C56 Zr1 C52 -129.8(8) . . . . ?
C55 C56 Zr1 C48 -47.5(10) . . . . ?
C57 C56 Zr1 C48 -164.3(8) . . . . ?
C55 C56 Zr1 C49 -63.6(13) . . . . ?
C57 C56 Zr1 C49 179.6(9) . . . . ?
C57 C56 Zr1 C55 -116.8(13) . . . . ?
C55 C56 Zr1 C51 20.6(11) . . . . ?
C57 C56 Zr1 C51 -96.2(9) . . . . ?
C55 C56 Zr1 C54 38.6(10) . . . . ?
C57 C56 Zr1 C54 -78.2(10) . . . . ?
C55 C56 Zr1 C50 27.5(19) . . . . ?
C57 C56 Zr1 C50 -89.3(15) . . . . ?
C55 C56 Zr1 C53 79.0(10) . . . . ?
C57 C56 Zr1 C53 -37.8(10) . . . . ?
C55 C56 Zr1 C57 116.8(13) . . . . ?
Zr1 O2 U1 O1 178(23) . . . . ?
Zr1 O2 U1 N8 -52(3) . . . . ?
Zr1 O2 U1 N1 19(3) . . . . ?
Zr1 O2 U1 N9 161(3) . . . . ?
Zr1 O2 U1 N2 86(3) . . . . ?
Zr1 O2 U1 N7 -119(3) . . . . ?
C39 N8 U1 O1 -87.3(8) . . . . ?
C36 N8 U1 O1 111.7(6) . . . . ?
C39 N8 U1 O2 95.2(8) . . . . ?
C36 N8 U1 O2 -65.7(6) . . . . ?
C39 N8 U1 N1 6.9(8) . . . . ?
C36 N8 U1 N1 -154.1(6) . . . . ?
C39 N8 U1 N9 -179.6(7) . . . . ?
C36 N8 U1 N9 19.4(8) . . . . ?
C39 N8 U1 N2 18.6(10) . . . . ?
C36 N8 U1 N2 -142.4(6) . . . . ?
C39 N8 U1 N7 178.4(9) . . . . ?
C36 N8 U1 N7 17.5(6) . . . . ?
C1 N1 U1 O1 88.0(8) . . . . ?
C4 N1 U1 O1 -113.7(5) . . . . ?
C1 N1 U1 O2 -93.2(8) . . . . ?
C4 N1 U1 O2 65.1(5) . . . . ?
C1 N1 U1 N8 -4.7(7) . . . . ?
C4 N1 U1 N8 153.6(6) . . . . ?
C1 N1 U1 N9 -179.0(7) . . . . ?
C4 N1 U1 N9 -20.7(7) . . . . ?
C1 N1 U1 N2 -176.0(8) . . . . ?
C4 N1 U1 N2 -17.7(5) . . . . ?
C1 N1 U1 N7 -16.2(9) . . . . ?
C4 N1 U1 N7 142.2(5) . . . . ?
C47 N9 U1 O1 -10.3(8) . . . . ?
C43 N9 U1 O1 162.0(8) . . . . ?
C47 N9 U1 O2 168.7(8) . . . . ?
C43 N9 U1 O2 -18.9(8) . . . . ?
C47 N9 U1 N8 83.9(9) . . . . ?
C43 N9 U1 N8 -103.7(8) . . . . ?
C47 N9 U1 N1 -106.0(8) . . . . ?
C43 N9 U1 N1 66.4(9) . . . . ?
C47 N9 U1 N2 -108.8(8) . . . . ?
C43 N9 U1 N2 63.5(7) . . . . ?
C47 N9 U1 N7 85.7(7) . . . . ?
C43 N9 U1 N7 -101.9(8) . . . . ?
C5 N2 U1 O1 108.6(6) . . . . ?
C6 N2 U1 O1 -83.9(7) . . . . ?
C5 N2 U1 O2 -74.8(6) . . . . ?
C6 N2 U1 O2 92.8(7) . . . . ?
C5 N2 U1 N8 3.9(8) . . . . ?
C6 N2 U1 N8 171.5(6) . . . . ?
C5 N2 U1 N1 16.0(6) . . . . ?
C6 N2 U1 N1 -176.5(8) . . . . ?
C5 N2 U1 N9 -166.0(7) . . . . ?
C6 N2 U1 N9 1.6(7) . . . . ?
C5 N2 U1 N7 -135.1(6) . . . . ?
C6 N2 U1 N7 32.5(10) . . . . ?
C35 N7 U1 O1 -108.3(6) . . . . ?
C34 N7 U1 O1 83.1(7) . . . . ?
C35 N7 U1 O2 74.7(6) . . . . ?
C34 N7 U1 O2 -93.9(7) . . . . ?
C35 N7 U1 N8 -16.0(5) . . . . ?
C34 N7 U1 N8 175.4(8) . . . . ?
C35 N7 U1 N1 -4.2(7) . . . . ?
C34 N7 U1 N1 -172.8(7) . . . . ?
C35 N7 U1 N9 165.1(6) . . . . ?
C34 N7 U1 N9 -3.5(7) . . . . ?
C35 N7 U1 N2 134.9(6) . . . . ?
C34 N7 U1 N2 -33.7(10) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         5.636
_refine_diff_density_min         -1.568
_refine_diff_density_rms         0.187

_vrf_PLAT412_p14093mono          
;
PROBLEM: Short Intra XH3 .. XHn H30A .. H32A ..
1.67 Ang and Short Intra XH3 .. XHn H9A .. H11A ..
1.72 Ang.
RESPONSE: The methyl groups on the phenyl ring of
the ligand were placed geometrically. This 
resulted in an eclipsed confirmation and a short 
intramolecular H..H contact for two adjacent 
methyl-H atoms on which no further modelling 
was undertaken, hence the Alert.
;
####################################################################### 
# 
# 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_po4006_refinalized
_database_code_depnum_ccdc_archive 'CCDC 1883754'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;university of edinburgh
United Kingdom
;
_audit_update_record             
;
2018-12-07 deposited with the CCDC.	2019-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C175 H175 Cl2 Mg2 N33 O4 U2'
_chemical_formula_weight         3400.06

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'
Cl Cl 0.3639 0.7018 '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'
Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'I 1 2/a 1'

loop_
_symmetry_equiv_pos_as_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                   24.852(5)
_cell_length_b                   23.010(5)
_cell_length_c                   28.754(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 102.183(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     16072(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    59332
_cell_measurement_theta_min      3.7700
_cell_measurement_theta_max      75.6780

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.1720
_exptl_crystal_size_mid          0.0393
_exptl_crystal_size_min          0.0362

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6920
_exptl_absorpt_coefficient_mu    6.532
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54180
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            165331
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.64
_diffrn_reflns_theta_max         76.31
_reflns_number_total             16761
_reflns_number_gt                14608
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    MERCURY
_computing_publication_material  ORTEP

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0412P)²+59.0107P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         16761
_refine_ls_number_parameters     984
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0295
_refine_ls_wR_factor_ref         0.0735
_refine_ls_wR_factor_gt          0.0698
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_restrained_S_all      0.925
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.91838(12) 0.02371(13) 0.28077(12) 0.0256(6) Uani 1 1 d . . .
C2 C 0.86620(13) 0.03650(15) 0.25252(13) 0.0319(7) Uani 1 1 d . . .
H2 H 0.8339 0.0460 0.2637 0.038 Uiso 1 1 calc R . .
C3 C 0.87074(13) 0.03253(16) 0.20525(13) 0.0342(7) Uani 1 1 d . . .
H3 H 0.8424 0.0387 0.1778 0.041 Uiso 1 1 calc R . .
C4 C 0.92595(13) 0.01741(14) 0.20637(12) 0.0282(6) Uani 1 1 d . . .
C5 C 0.95390(13) 0.01337(14) 0.16853(12) 0.0291(7) Uani 1 1 d . . .
H5 H 0.9337 0.0163 0.1367 0.035 Uiso 1 1 calc R . .
C6 C 1.03113(13) 0.00146(14) 0.13615(12) 0.0267(6) Uani 1 1 d . . .
C7 C 1.01186(14) -0.03805(15) 0.09993(12) 0.0311(7) Uani 1 1 d . . .
H7 H 0.9815 -0.0623 0.1021 0.037 Uiso 1 1 calc R . .
C8 C 1.03604(15) -0.04296(16) 0.06051(13) 0.0341(7) Uani 1 1 d . . .
C9 C 1.01541(18) -0.08774(18) 0.02289(14) 0.0438(9) Uani 1 1 d . . .
H9A H 1.0367 -0.0852 -0.0021 0.066 Uiso 1 1 calc R . .
H9B H 0.9764 -0.0806 0.0091 0.066 Uiso 1 1 calc R . .
H9C H 1.0197 -0.1266 0.0372 0.066 Uiso 1 1 calc R . .
C10 C 1.08086(15) -0.00727(17) 0.05779(13) 0.0348(7) Uani 1 1 d . . .
C11 C 1.10739(19) -0.0110(2) 0.01512(16) 0.0498(10) Uani 1 1 d . . .
H11A H 1.0887 -0.0408 -0.0068 0.075 Uiso 1 1 calc R . .
H11B H 1.1463 -0.0214 0.0257 0.075 Uiso 1 1 calc R . .
H11C H 1.1044 0.0267 -0.0011 0.075 Uiso 1 1 calc R . .
C12 C 1.10021(14) 0.03209(15) 0.09407(12) 0.0312(7) Uani 1 1 d . . .
H12 H 1.1307 0.0561 0.0920 0.037 Uiso 1 1 calc R . .
C13 C 1.07612(13) 0.03737(14) 0.13359(11) 0.0262(6) Uani 1 1 d . . .
C14 C 1.12071(12) 0.12164(14) 0.16732(12) 0.0267(6) Uani 1 1 d . . .
H14 H 1.1254 0.1330 0.1367 0.032 Uiso 1 1 calc R . .
C15 C 1.14199(12) 0.15724(14) 0.20800(12) 0.0251(6) Uani 1 1 d . . .
C16 C 1.16994(13) 0.20985(14) 0.21224(12) 0.0285(6) Uani 1 1 d . . .
H16 H 1.1794 0.2315 0.1870 0.034 Uiso 1 1 calc R . .
C17 C 1.18167(13) 0.22529(14) 0.26061(12) 0.0280(6) Uani 1 1 d . . .
H17 H 1.2007 0.2592 0.2740 0.034 Uiso 1 1 calc R . .
C18 C 1.16056(12) 0.18215(13) 0.28545(12) 0.0245(6) Uani 1 1 d . . .
C19 C 1.16411(12) 0.17461(13) 0.33824(12) 0.0255(6) Uani 1 1 d . . .
C20 C 1.18587(14) 0.23062(14) 0.36458(13) 0.0320(7) Uani 1 1 d . . .
H20A H 1.1603 0.2626 0.3536 0.048 Uiso 1 1 calc R . .
H20B H 1.2221 0.2400 0.3581 0.048 Uiso 1 1 calc R . .
H20C H 1.1892 0.2251 0.3989 0.048 Uiso 1 1 calc R . .
C21 C 1.10680(13) 0.16098(15) 0.34872(12) 0.0290(6) Uani 1 1 d . . .
H21A H 1.0816 0.1931 0.3374 0.044 Uiso 1 1 calc R . .
H21B H 1.1101 0.1560 0.3831 0.044 Uiso 1 1 calc R . .
H21C H 1.0924 0.1251 0.3323 0.044 Uiso 1 1 calc R . .
C22 C 1.20375(12) 0.12546(13) 0.35556(11) 0.0225(6) Uani 1 1 d . . .
C23 C 1.25623(13) 0.12690(14) 0.38439(12) 0.0266(6) Uani 1 1 d . . .
H23 H 1.2748 0.1604 0.3989 0.032 Uiso 1 1 calc R . .
C24 C 1.27684(13) 0.06970(15) 0.38814(12) 0.0270(6) Uani 1 1 d . . .
H24 H 1.3118 0.0575 0.4057 0.032 Uiso 1 1 calc R . .
C25 C 1.23681(12) 0.03458(13) 0.36162(11) 0.0233(6) Uani 1 1 d . . .
C26 C 1.23623(12) -0.02731(13) 0.35493(11) 0.0244(6) Uani 1 1 d . . .
H26 H 1.2670 -0.0496 0.3705 0.029 Uiso 1 1 calc R . .
C27 C 1.19771(13) -0.11375(13) 0.32239(12) 0.0258(6) Uani 1 1 d . . .
C28 C 1.24599(13) -0.14405(14) 0.31988(12) 0.0290(7) Uani 1 1 d . . .
H28 H 1.2789 -0.1227 0.3205 0.035 Uiso 1 1 calc R . .
C29 C 1.24729(14) -0.20411(15) 0.31647(13) 0.0319(7) Uani 1 1 d . . .
C30 C 1.30059(16) -0.23484(17) 0.31491(17) 0.0434(9) Uani 1 1 d . . .
H30A H 1.2941 -0.2768 0.3124 0.065 Uiso 1 1 calc R . .
H30B H 1.3279 -0.2263 0.3441 0.065 Uiso 1 1 calc R . .
H30C H 1.3143 -0.2213 0.2873 0.065 Uiso 1 1 calc R . .
C31 C 1.19867(15) -0.23587(15) 0.31483(14) 0.0341(7) Uani 1 1 d . . .
C32 C 1.19881(18) -0.30131(16) 0.31292(18) 0.0466(10) Uani 1 1 d . . .
H32A H 1.2361 -0.3151 0.3128 0.070 Uiso 1 1 calc R . .
H32B H 1.1736 -0.3145 0.2839 0.070 Uiso 1 1 calc R . .
H32C H 1.1868 -0.3169 0.3408 0.070 Uiso 1 1 calc R . .
C33 C 1.15009(14) -0.20547(14) 0.31539(13) 0.0316(7) Uani 1 1 d . . .
H33 H 1.1169 -0.2267 0.3131 0.038 Uiso 1 1 calc R . .
C34 C 1.14870(13) -0.14516(14) 0.31917(12) 0.0267(6) Uani 1 1 d . . .
C35 C 1.06987(13) -0.13547(14) 0.34899(13) 0.0293(7) Uani 1 1 d . . .
H35 H 1.0803 -0.1712 0.3650 0.035 Uiso 1 1 calc R . .
C36 C 1.02115(13) -0.10698(14) 0.35551(12) 0.0281(6) Uani 1 1 d . . .
C37 C 0.98603(13) -0.12088(15) 0.38652(13) 0.0308(7) Uani 1 1 d . . .
H37 H 0.9875 -0.1545 0.4059 0.037 Uiso 1 1 calc R . .
C38 C 0.94883(13) -0.07509(15) 0.38293(12) 0.0294(7) Uani 1 1 d . . .
H38 H 0.9197 -0.0714 0.3995 0.035 Uiso 1 1 calc R . .
C39 C 0.96234(12) -0.03539(14) 0.35024(12) 0.0254(6) Uani 1 1 d . . .
C40 C 0.93614(12) 0.02270(13) 0.33434(12) 0.0255(6) Uani 1 1 d . . .
C41 C 0.97902(13) 0.07107(14) 0.35089(13) 0.0295(7) Uani 1 1 d . . .
H41A H 0.9905 0.0703 0.3857 0.044 Uiso 1 1 calc R . .
H41B H 0.9627 0.1090 0.3407 0.044 Uiso 1 1 calc R . .
H41C H 1.0111 0.0647 0.3368 0.044 Uiso 1 1 calc R . .
C42 C 0.88640(14) 0.03300(15) 0.35711(13) 0.0327(7) Uani 1 1 d . . .
H42A H 0.8984 0.0323 0.3918 0.049 Uiso 1 1 calc R . .
H42B H 0.8590 0.0024 0.3470 0.049 Uiso 1 1 calc R . .
H42C H 0.8700 0.0709 0.3470 0.049 Uiso 1 1 calc R . .
C43 C 1.11923(14) -0.09662(15) 0.18395(13) 0.0319(7) Uani 1 1 d . . .
H43 H 1.0868 -0.1196 0.1794 0.038 Uiso 1 1 calc R . .
C44 C 1.15637(16) -0.10770(16) 0.15550(14) 0.0379(8) Uani 1 1 d . . .
H44 H 1.1495 -0.1370 0.1317 0.045 Uiso 1 1 calc R . .
C45 C 1.20444(15) -0.07445(16) 0.16274(14) 0.0374(8) Uani 1 1 d . . .
H45 H 1.2313 -0.0812 0.1442 0.045 Uiso 1 1 calc R . .
C46 C 1.21240(14) -0.03186(15) 0.19698(13) 0.0331(7) Uani 1 1 d . . .
H46 H 1.2448 -0.0087 0.2025 0.040 Uiso 1 1 calc R . .
C47 C 1.17238(13) -0.02311(14) 0.22348(12) 0.0282(6) Uani 1 1 d . . .
H47 H 1.1777 0.0069 0.2467 0.034 Uiso 1 1 calc R . .
C48 C 0.83570(14) -0.12368(14) 0.19649(13) 0.0310(7) Uani 1 1 d . . .
H48 H 0.8362 -0.1246 0.1636 0.037 Uiso 1 1 calc R . .
C49 C 0.78629(14) -0.11341(14) 0.20977(14) 0.0344(7) Uani 1 1 d . . .
H49 H 0.7535 -0.1074 0.1865 0.041 Uiso 1 1 calc R . .
C50 C 0.78562(15) -0.11214(15) 0.25785(15) 0.0375(8) Uani 1 1 d . . .
H50 H 0.7521 -0.1062 0.2680 0.045 Uiso 1 1 calc R . .
C51 C 0.83422(15) -0.11960(16) 0.29074(15) 0.0378(8) Uani 1 1 d . . .
H51 H 0.8349 -0.1180 0.3239 0.045 Uiso 1 1 calc R . .
C52 C 0.88218(14) -0.12944(15) 0.27451(13) 0.0320(7) Uani 1 1 d . . .
H52 H 0.9157 -0.1342 0.2972 0.038 Uiso 1 1 calc R . .
C53 C 1.03355(17) -0.24968(18) 0.21978(17) 0.0460(10) Uani 1 1 d . . .
H53 H 1.0475 -0.2241 0.1993 0.055 Uiso 1 1 calc R . .
C54 C 1.05973(18) -0.30185(19) 0.23138(18) 0.0504(10) Uani 1 1 d . . .
H54 H 1.0912 -0.3119 0.2193 0.061 Uiso 1 1 calc R . .
C55 C 1.03954(16) -0.33922(17) 0.26088(17) 0.0478(10) Uani 1 1 d . . .
H55 H 1.0569 -0.3756 0.2694 0.057 Uiso 1 1 calc R . .
C56 C 0.99458(17) -0.3234(2) 0.27765(18) 0.0520(11) Uani 1 1 d . . .
H56 H 0.9799 -0.3488 0.2979 0.062 Uiso 1 1 calc R . .
C57 C 0.97019(15) -0.26946(18) 0.26473(15) 0.0408(8) Uani 1 1 d . . .
H57 H 0.9390 -0.2584 0.2769 0.049 Uiso 1 1 calc R . .
C58 C 0.0286(4) 0.7235(4) 0.4442(3) 0.102(2) Uani 1 1 d . . .
H58 H 0.0074 0.7436 0.4630 0.123 Uiso 1 1 calc R . .
C59 C 0.0105(3) 0.6732(3) 0.4227(3) 0.087(2) Uani 1 1 d . . .
H59 H -0.0247 0.6588 0.4248 0.105 Uiso 1 1 calc R . .
C60 C 0.0412(4) 0.6437(4) 0.3983(3) 0.105(3) Uani 1 1 d . . .
H60 H 0.0277 0.6081 0.3835 0.126 Uiso 1 1 calc R . .
C61 C 0.0903(5) 0.6630(6) 0.3944(4) 0.168(6) Uani 1 1 d . . .
H61 H 0.1131 0.6396 0.3793 0.202 Uiso 1 1 calc R . .
C62 C 0.1081(4) 0.7160(5) 0.4118(3) 0.136(4) Uani 1 1 d . . .
H62 H 0.1409 0.7322 0.4051 0.163 Uiso 1 1 calc R . .
N13 N 0.1142(2) 0.7850(2) 0.07196(18) 0.0743(13) Uani 1 1 d . . .
C64 C 0.0668(2) 0.7727(3) 0.0842(2) 0.0688(14) Uani 1 1 d . . .
H64 H 0.0470 0.8038 0.0945 0.083 Uiso 1 1 calc R . .
C65 C 0.0452(3) 0.7191(3) 0.0830(2) 0.0845(19) Uani 1 1 d . . .
H65 H 0.0113 0.7124 0.0924 0.101 Uiso 1 1 calc R . .
C66 C 0.0742(4) 0.6735(3) 0.0676(3) 0.114(3) Uani 1 1 d . . .
H66 H 0.0594 0.6352 0.0648 0.137 Uiso 1 1 calc R . .
C67 C 0.1238(4) 0.6845(3) 0.0567(3) 0.092(2) Uani 1 1 d . . .
H67 H 0.1451 0.6539 0.0476 0.111 Uiso 1 1 calc R . .
C68 C 0.7492(2) 0.8636(3) 0.0735(2) 0.0640(13) Uani 1 1 d . . .
H68 H 0.7307 0.8277 0.0749 0.077 Uiso 1 1 calc R . .
C69 C 0.7993(2) 0.8627(3) 0.0621(2) 0.0701(15) Uani 1 1 d . . .
H69 H 0.8155 0.8268 0.0561 0.084 Uiso 1 1 calc R . .
C70 C 0.7507(3) 0.9615(3) 0.0798(2) 0.0734(16) Uani 1 1 d . . .
H70 H 0.7332 0.9966 0.0860 0.088 Uiso 1 1 calc R . .
C71 C 0.8029(3) 0.9645(3) 0.0681(2) 0.0730(15) Uani 1 1 d . . .
H71 H 0.8209 1.0007 0.0666 0.088 Uiso 1 1 calc R . .
C72 C 0.8266(2) 0.9139(3) 0.0592(2) 0.0768(18) Uani 1 1 d . . .
H72 H 0.8616 0.9138 0.0510 0.092 Uiso 1 1 calc R . .
N15 N 0.8751(2) 0.7805(2) 0.92549(18) 0.0733(13) Uani 1 1 d . . .
C74 C 0.88066(18) 0.7241(2) 0.92003(16) 0.0500(10) Uani 1 1 d . . .
H74 H 0.8763 0.7096 0.8885 0.060 Uiso 1 1 calc R . .
C75 C 0.8920(2) 0.6858(2) 0.95590(18) 0.0561(11) Uani 1 1 d . . .
H75 H 0.8937 0.6453 0.9498 0.067 Uiso 1 1 calc R . .
C76 C 0.9012(3) 0.7065(3) 1.0018(2) 0.0740(16) Uani 1 1 d . . .
H76 H 0.9101 0.6807 1.0281 0.089 Uiso 1 1 calc R . .
C77 C 0.8971(2) 0.7654(3) 1.0088(2) 0.0793(19) Uani 1 1 d . . .
H77 H 0.9035 0.7812 1.0400 0.095 Uiso 1 1 calc R . .
C78 C 0.15997(17) 0.0564(2) 0.49430(15) 0.0476(10) Uani 1 1 d . . .
H78 H 0.1896 0.0798 0.5103 0.057 Uiso 1 1 calc R . .
C79 C 0.08255(17) 0.0049(2) 0.49569(15) 0.0518(11) Uani 1 1 d . . .
H79 H 0.0558 -0.0089 0.5123 0.062 Uiso 1 1 calc R . .
C80 C 0.07724(17) -0.0105(2) 0.44896(15) 0.0484(10) Uani 1 1 d . . .
H80 H 0.0476 -0.0344 0.4338 0.058 Uiso 1 1 calc R . .
C81 C 0.11525(18) 0.0091(2) 0.42417(15) 0.0487(10) Uani 1 1 d . . .
H81 H 0.1123 -0.0010 0.3917 0.058 Uiso 1 1 calc R . .
C82 C 0.15749(16) 0.04355(19) 0.44739(14) 0.0417(9) Uani 1 1 d . . .
H82 H 0.1844 0.0582 0.4313 0.050 Uiso 1 1 calc R . .
C83 C 0.2177(5) 0.6309(5) 0.5322(7) 0.165(6) Uani 1 1 d D . .
H83 H 0.1941 0.6322 0.5543 0.197 Uiso 1 1 calc R . .
C84 C 0.1945(10) 0.6310(10) 0.4838(8) 0.342(16) Uani 1 1 d U . .
H84 H 0.1556 0.6325 0.4736 0.410 Uiso 1 1 calc R . .
C85 C 0.2735(6) 0.6289(9) 0.5492(7) 0.286(13) Uani 1 1 d D . .
H85 H 0.2891 0.6263 0.5823 0.343 Uiso 1 1 calc R . .
C88 C 0.2500 0.7038(4) 0.0000 0.132(7) Uani 1 2 d SD . .
H88 H 0.2500 0.7451 0.0000 0.158 Uiso 1 2 calc SR . .
C87 C 0.2770(3) 0.6755(4) 0.0360(3) 0.134(5) Uani 1 1 d D . .
H87 H 0.2969 0.6968 0.0624 0.160 Uiso 1 1 calc R . .
C86 C 0.2786(4) 0.6171(4) 0.0382(3) 0.121(4) Uani 1 1 d D . .
H86 H 0.2988 0.5973 0.0653 0.145 Uiso 1 1 calc R . .
N17 N 0.2500 0.5875(5) 0.0000 0.162(6) Uani 1 2 d SD . .
N1 N 0.95483(10) 0.01223(11) 0.25259(10) 0.0241(5) Uani 1 1 d . . .
N2 N 1.00695(11) 0.00563(12) 0.17660(10) 0.0271(5) Uani 1 1 d . . .
N3 N 1.09526(10) 0.07428(12) 0.17260(10) 0.0255(5) Uani 1 1 d . . .
N4 N 1.13684(10) 0.14137(11) 0.25298(9) 0.0232(5) Uani 1 1 d . . .
H4 H 1.1206 0.1095 0.2599 0.028 Uiso 1 1 calc R . .
N5 N 1.19274(10) 0.06923(11) 0.34193(9) 0.0227(5) Uani 1 1 d . . .
H5A H 1.1621 0.0569 0.3233 0.027 Uiso 1 1 calc R . .
N6 N 1.19554(10) -0.05314(11) 0.32860(10) 0.0247(5) Uani 1 1 d . . .
N7 N 1.10019(11) -0.11399(12) 0.32192(10) 0.0279(6) Uani 1 1 d . . .
N8 N 1.00642(10) -0.05460(11) 0.33327(10) 0.0251(5) Uani 1 1 d . . .
N9 N 1.12628(11) -0.05547(12) 0.21749(10) 0.0279(5) Uani 1 1 d . . .
N10 N 0.88320(11) -0.13243(12) 0.22834(10) 0.0278(6) Uani 1 1 d . . .
N11 N 0.98881(12) -0.23312(12) 0.23615(12) 0.0331(6) Uani 1 1 d . . .
N12 N 0.0787(4) 0.7455(3) 0.4388(3) 0.127(3) Uani 1 1 d . . .
C63 C 0.1423(3) 0.7408(3) 0.0590(2) 0.0803(17) Uani 1 1 d . . .
H63 H 0.1768 0.7485 0.0509 0.096 Uiso 1 1 calc R . .
N14 N 0.72500(19) 0.9114(2) 0.0825(2) 0.0744(13) Uani 1 1 d . . .
C73 C 0.8838(3) 0.8003(3) 0.9698(2) 0.0778(17) Uani 1 1 d . . .
H73 H 0.8806 0.8409 0.9745 0.093 Uiso 1 1 calc R . .
N16 N 0.12328(16) 0.0380(2) 0.51896(13) 0.0568(11) Uani 1 1 d . . .
O1 O 1.08619(8) 0.03393(9) 0.28791(8) 0.0245(4) Uani 1 1 d . . .
O2 O 1.01398(9) -0.10152(10) 0.23350(8) 0.0279(4) Uani 1 1 d . . .
Cl1 Cl 0.93985(4) -0.16958(4) 0.12718(3) 0.03967(19) Uani 1 1 d . . .
U1 U 1.048030(4) -0.032715(4) 0.263132(3) 0.02048(4) Uani 1 1 d . . .
Mg1 Mg 0.95617(4) -0.15358(5) 0.20720(4) 0.0275(2) Uani 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.362(4) . ?
C1 C2 1.409(4) . ?
C1 C40 1.510(5) . ?
C2 C3 1.390(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.409(5) . ?
C3 H3 0.9500 . ?
C4 N1 1.376(4) . ?
C4 C5 1.412(5) . ?
C5 N2 1.302(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.389(5) . ?
C6 C13 1.404(4) . ?
C6 N2 1.421(4) . ?
C7 C8 1.395(5) . ?
C7 H7 0.9500 . ?
C8 C10 1.399(5) . ?
C8 C9 1.503(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C12 1.388(5) . ?
C10 C11 1.513(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.397(5) . ?
C12 H12 0.9500 . ?
C13 N3 1.407(4) . ?
C14 N3 1.285(4) . ?
C14 C15 1.435(5) . ?
C14 H14 0.9500 . ?
C15 N4 1.376(4) . ?
C15 C16 1.388(4) . ?
C16 C17 1.405(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.389(4) . ?
C17 H17 0.9500 . ?
C18 N4 1.367(4) . ?
C18 C19 1.512(5) . ?
C19 C22 1.513(4) . ?
C19 C20 1.534(4) . ?
C19 C21 1.549(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 N5 1.363(4) . ?
C22 C23 1.390(4) . ?
C23 C24 1.408(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.380(4) . ?
C24 H24 0.9500 . ?
C25 N5 1.376(4) . ?
C25 C26 1.437(4) . ?
C26 N6 1.275(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.403(4) . ?
C27 C34 1.402(4) . ?
C27 N6 1.409(4) . ?
C28 C29 1.386(5) . ?
C28 H28 0.9500 . ?
C29 C31 1.404(5) . ?
C29 C30 1.511(5) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C33 1.398(5) . ?
C31 C32 1.507(5) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.393(4) . ?
C33 H33 0.9500 . ?
C34 N7 1.419(4) . ?
C35 N7 1.291(4) . ?
C35 C36 1.424(4) . ?
C35 H35 0.9500 . ?
C36 N8 1.377(4) . ?
C36 C37 1.410(4) . ?
C37 C38 1.391(5) . ?
C37 H37 0.9500 . ?
C38 C39 1.401(5) . ?
C38 H38 0.9500 . ?
C39 N8 1.364(4) . ?
C39 C40 1.515(4) . ?
C40 C42 1.534(4) . ?
C40 C41 1.545(4) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 N9 1.336(5) . ?
C43 C44 1.380(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.397(5) . ?
C44 H44 0.9500 . ?
C45 C46 1.373(6) . ?
C45 H45 0.9500 . ?
C46 C47 1.389(5) . ?
C46 H46 0.9500 . ?
C47 N9 1.347(4) . ?
C47 H47 0.9500 . ?
C48 N10 1.348(4) . ?
C48 C49 1.381(5) . ?
C48 H48 0.9500 . ?
C49 C50 1.386(6) . ?
C49 H49 0.9500 . ?
C50 C51 1.379(6) . ?
C50 H50 0.9500 . ?
C51 C52 1.387(5) . ?
C51 H51 0.9500 . ?
C52 N10 1.335(5) . ?
C52 H52 0.9500 . ?
C53 N11 1.351(5) . ?
C53 C54 1.372(6) . ?
C53 H53 0.9500 . ?
C54 C55 1.375(6) . ?
C54 H54 0.9500 . ?
C55 C56 1.357(6) . ?
C55 H55 0.9500 . ?
C56 C57 1.397(6) . ?
C56 H56 0.9500 . ?
C57 N11 1.323(5) . ?
C57 H57 0.9500 . ?
C58 C59 1.344(11) . ?
C58 N12 1.384(11) . ?
C58 H58 0.9500 . ?
C59 C60 1.326(11) . ?
C59 H59 0.9500 . ?
C60 C61 1.327(12) . ?
C60 H60 0.9500 . ?
C61 C62 1.356(13) . ?
C61 H61 0.9500 . ?
C62 N12 1.355(13) . ?
C62 H62 0.9500 . ?
N13 C64 1.327(7) . ?
N13 C63 1.333(8) . ?
C64 C65 1.343(9) . ?
C64 H64 0.9500 . ?
C65 C66 1.397(11) . ?
C65 H65 0.9500 . ?
C66 C67 1.359(11) . ?
C66 H66 0.9500 . ?
C67 C63 1.371(10) . ?
C67 H67 0.9500 . ?
C68 N14 1.306(7) . ?
C68 C69 1.354(7) . ?
C68 H68 0.9500 . ?
C69 C72 1.370(9) . ?
C69 H69 0.9500 . ?
C70 N14 1.327(8) . ?
C70 C71 1.411(8) . ?
C70 H70 0.9500 . ?
C71 C72 1.354(8) . ?
C71 H71 0.9500 . ?
C72 H72 0.9500 . ?
N15 C74 1.317(7) . ?
N15 C73 1.326(8) . ?
C74 C75 1.342(7) . ?
C74 H74 0.9500 . ?
C75 C76 1.377(7) . ?
C75 H75 0.9500 . ?
C76 C77 1.377(9) . ?
C76 H76 0.9500 . ?
C77 C73 1.363(9) . ?
C77 H77 0.9500 . ?
C78 N16 1.336(5) . ?
C78 C82 1.369(6) . ?
C78 H78 0.9500 . ?
C79 N16 1.330(5) . ?
C79 C80 1.369(6) . ?
C79 H79 0.9500 . ?
C80 C81 1.374(6) . ?
C80 H80 0.9500 . ?
C81 C82 1.371(6) . ?
C81 H81 0.9500 . ?
C82 H82 0.9500 . ?
C83 C85 1.371(9) . ?
C83 C84 1.39(2) . ?
C83 H83 0.9500 . ?
C84 C85 1.36(3) 2_556 ?
C84 H84 0.9500 . ?
C85 C84 1.36(3) 2_556 ?
C85 H85 0.9500 . ?
C88 C87 1.286(10) . ?
C88 C87 1.286(10) 2 ?
C88 H88 0.9500 . ?
C87 C86 1.345(8) . ?
C87 H87 0.9500 . ?
C86 N17 1.357(8) . ?
C86 H86 0.9500 . ?
N17 C86 1.357(8) 2 ?
N1 U1 2.496(3) . ?
N2 U1 2.634(3) . ?
N4 H4 0.8800 . ?
N5 H5A 0.8800 . ?
N7 U1 2.667(3) . ?
N8 U1 2.504(3) . ?
N9 U1 2.618(3) . ?
N10 Mg1 2.088(3) . ?
N11 Mg1 2.101(3) . ?
C63 H63 0.9500 . ?
C73 H73 0.9500 . ?
O1 U1 1.864(2) . ?
O2 Mg1 1.901(2) . ?
O2 U1 1.909(2) . ?
Cl1 Mg1 2.2804(15) . ?
U1 Mg1 3.7395(12) . ?

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
N1 C1 C2 110.1(3) . . ?
N1 C1 C40 121.1(3) . . ?
C2 C1 C40 128.8(3) . . ?
C3 C2 C1 107.2(3) . . ?
C3 C2 H2 126.4 . . ?
C1 C2 H2 126.4 . . ?
C2 C3 C4 105.9(3) . . ?
C2 C3 H3 127.1 . . ?
C4 C3 H3 127.1 . . ?
N1 C4 C3 110.5(3) . . ?
N1 C4 C5 119.8(3) . . ?
C3 C4 C5 129.3(3) . . ?
N2 C5 C4 121.1(3) . . ?
N2 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C7 C6 C13 119.9(3) . . ?
C7 C6 N2 121.3(3) . . ?
C13 C6 N2 118.8(3) . . ?
C6 C7 C8 121.5(3) . . ?
C6 C7 H7 119.2 . . ?
C8 C7 H7 119.2 . . ?
C7 C8 C10 118.8(3) . . ?
C7 C8 C9 120.0(3) . . ?
C10 C8 C9 121.1(3) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C12 C10 C8 119.6(3) . . ?
C12 C10 C11 120.4(3) . . ?
C8 C10 C11 120.0(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 C13 121.9(3) . . ?
C10 C12 H12 119.1 . . ?
C13 C12 H12 119.1 . . ?
C12 C13 C6 118.3(3) . . ?
C12 C13 N3 124.8(3) . . ?
C6 C13 N3 116.9(3) . . ?
N3 C14 C15 119.6(3) . . ?
N3 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
N4 C15 C16 107.0(3) . . ?
N4 C15 C14 121.6(3) . . ?
C16 C15 C14 131.4(3) . . ?
C15 C16 C17 107.6(3) . . ?
C15 C16 H16 126.2 . . ?
C17 C16 H16 126.2 . . ?
C18 C17 C16 107.8(3) . . ?
C18 C17 H17 126.1 . . ?
C16 C17 H17 126.1 . . ?
N4 C18 C17 107.1(3) . . ?
N4 C18 C19 122.2(3) . . ?
C17 C18 C19 130.6(3) . . ?
C18 C19 C22 108.2(2) . . ?
C18 C19 C20 109.8(3) . . ?
C22 C19 C20 109.2(3) . . ?
C18 C19 C21 110.9(3) . . ?
C22 C19 C21 110.3(3) . . ?
C20 C19 C21 108.5(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N5 C22 C23 107.5(3) . . ?
N5 C22 C19 122.5(3) . . ?
C23 C22 C19 129.9(3) . . ?
C22 C23 C24 107.7(3) . . ?
C22 C23 H23 126.2 . . ?
C24 C23 H23 126.2 . . ?
C25 C24 C23 107.3(3) . . ?
C25 C24 H24 126.4 . . ?
C23 C24 H24 126.4 . . ?
N5 C25 C24 107.8(3) . . ?
N5 C25 C26 122.3(3) . . ?
C24 C25 C26 129.8(3) . . ?
N6 C26 C25 121.7(3) . . ?
N6 C26 H26 119.1 . . ?
C25 C26 H26 119.1 . . ?
C28 C27 C34 118.7(3) . . ?
C28 C27 N6 123.7(3) . . ?
C34 C27 N6 117.6(3) . . ?
C29 C28 C27 122.1(3) . . ?
C29 C28 H28 118.9 . . ?
C27 C28 H28 118.9 . . ?
C28 C29 C31 119.2(3) . . ?
C28 C29 C30 120.2(3) . . ?
C31 C29 C30 120.6(3) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C33 C31 C29 118.6(3) . . ?
C33 C31 C32 120.6(3) . . ?
C29 C31 C32 120.8(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C31 122.3(3) . . ?
C34 C33 H33 118.8 . . ?
C31 C33 H33 118.8 . . ?
C33 C34 C27 118.9(3) . . ?
C33 C34 N7 122.9(3) . . ?
C27 C34 N7 118.2(3) . . ?
N7 C35 C36 121.6(3) . . ?
N7 C35 H35 119.2 . . ?
C36 C35 H35 119.2 . . ?
N8 C36 C37 110.7(3) . . ?
N8 C36 C35 119.5(3) . . ?
C37 C36 C35 129.5(3) . . ?
C38 C37 C36 105.8(3) . . ?
C38 C37 H37 127.1 . . ?
C36 C37 H37 127.1 . . ?
C37 C38 C39 107.1(3) . . ?
C37 C38 H38 126.5 . . ?
C39 C38 H38 126.5 . . ?
N8 C39 C38 110.7(3) . . ?
N8 C39 C40 120.3(3) . . ?
C38 C39 C40 129.0(3) . . ?
C1 C40 C39 109.6(3) . . ?
C1 C40 C42 110.2(3) . . ?
C39 C40 C42 110.0(3) . . ?
C1 C40 C41 109.7(3) . . ?
C39 C40 C41 108.6(3) . . ?
C42 C40 C41 108.8(3) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N9 C43 C44 123.8(3) . . ?
N9 C43 H43 118.1 . . ?
C44 C43 H43 118.1 . . ?
C43 C44 C45 117.9(4) . . ?
C43 C44 H44 121.0 . . ?
C45 C44 H44 121.0 . . ?
C46 C45 C44 119.1(3) . . ?
C46 C45 H45 120.4 . . ?
C44 C45 H45 120.4 . . ?
C45 C46 C47 119.0(3) . . ?
C45 C46 H46 120.5 . . ?
C47 C46 H46 120.5 . . ?
N9 C47 C46 122.5(3) . . ?
N9 C47 H47 118.7 . . ?
C46 C47 H47 118.7 . . ?
N10 C48 C49 122.7(3) . . ?
N10 C48 H48 118.7 . . ?
C49 C48 H48 118.7 . . ?
C48 C49 C50 118.5(3) . . ?
C48 C49 H49 120.7 . . ?
C50 C49 H49 120.7 . . ?
C51 C50 C49 119.2(3) . . ?
C51 C50 H50 120.4 . . ?
C49 C50 H50 120.4 . . ?
C50 C51 C52 118.7(4) . . ?
C50 C51 H51 120.7 . . ?
C52 C51 H51 120.7 . . ?
N10 C52 C51 122.7(3) . . ?
N10 C52 H52 118.6 . . ?
C51 C52 H52 118.6 . . ?
N11 C53 C54 123.0(4) . . ?
N11 C53 H53 118.5 . . ?
C54 C53 H53 118.5 . . ?
C53 C54 C55 118.7(4) . . ?
C53 C54 H54 120.6 . . ?
C55 C54 H54 120.6 . . ?
C56 C55 C54 119.2(4) . . ?
C56 C55 H55 120.4 . . ?
C54 C55 H55 120.4 . . ?
C55 C56 C57 119.1(4) . . ?
C55 C56 H56 120.4 . . ?
C57 C56 H56 120.4 . . ?
N11 C57 C56 122.6(4) . . ?
N11 C57 H57 118.7 . . ?
C56 C57 H57 118.7 . . ?
C59 C58 N12 119.0(9) . . ?
C59 C58 H58 120.5 . . ?
N12 C58 H58 120.5 . . ?
C60 C59 C58 120.6(8) . . ?
C60 C59 H59 119.7 . . ?
C58 C59 H59 119.7 . . ?
C61 C60 C59 121.1(8) . . ?
C61 C60 H60 119.4 . . ?
C59 C60 H60 119.4 . . ?
C60 C61 C62 120.2(10) . . ?
C60 C61 H61 119.9 . . ?
C62 C61 H61 119.9 . . ?
N12 C62 C61 119.2(8) . . ?
N12 C62 H62 120.4 . . ?
C61 C62 H62 120.4 . . ?
C64 N13 C63 117.3(6) . . ?
N13 C64 C65 124.2(6) . . ?
N13 C64 H64 117.9 . . ?
C65 C64 H64 117.9 . . ?
C64 C65 C66 117.8(7) . . ?
C64 C65 H65 121.1 . . ?
C66 C65 H65 121.1 . . ?
C67 C66 C65 119.1(7) . . ?
C67 C66 H66 120.4 . . ?
C65 C66 H66 120.4 . . ?
C66 C67 C63 118.5(7) . . ?
C66 C67 H67 120.7 . . ?
C63 C67 H67 120.7 . . ?
N14 C68 C69 123.2(6) . . ?
N14 C68 H68 118.4 . . ?
C69 C68 H68 118.4 . . ?
C68 C69 C72 119.5(6) . . ?
C68 C69 H69 120.2 . . ?
C72 C69 H69 120.2 . . ?
N14 C70 C71 122.3(5) . . ?
N14 C70 H70 118.9 . . ?
C71 C70 H70 118.9 . . ?
C72 C71 C70 117.4(6) . . ?
C72 C71 H71 121.3 . . ?
C70 C71 H71 121.3 . . ?
C71 C72 C69 119.3(5) . . ?
C71 C72 H72 120.3 . . ?
C69 C72 H72 120.3 . . ?
C74 N15 C73 116.9(5) . . ?
N15 C74 C75 124.5(5) . . ?
N15 C74 H74 117.7 . . ?
C75 C74 H74 117.7 . . ?
C74 C75 C76 118.4(5) . . ?
C74 C75 H75 120.8 . . ?
C76 C75 H75 120.8 . . ?
C77 C76 C75 118.6(6) . . ?
C77 C76 H76 120.7 . . ?
C75 C76 H76 120.7 . . ?
C73 C77 C76 118.2(5) . . ?
C73 C77 H77 120.9 . . ?
C76 C77 H77 120.9 . . ?
N16 C78 C82 124.1(4) . . ?
N16 C78 H78 117.9 . . ?
C82 C78 H78 117.9 . . ?
N16 C79 C80 123.2(4) . . ?
N16 C79 H79 118.4 . . ?
C80 C79 H79 118.4 . . ?
C79 C80 C81 119.4(4) . . ?
C79 C80 H80 120.3 . . ?
C81 C80 H80 120.3 . . ?
C82 C81 C80 118.5(4) . . ?
C82 C81 H81 120.8 . . ?
C80 C81 H81 120.8 . . ?
C78 C82 C81 118.4(4) . . ?
C78 C82 H82 120.8 . . ?
C81 C82 H82 120.8 . . ?
C85 C83 C84 122.0(19) . . ?
C85 C83 H83 119.0 . . ?
C84 C83 H83 119.0 . . ?
C85 C84 C83 121(2) 2_556 . ?
C85 C84 H84 119.3 2_556 . ?
C83 C84 H84 119.3 . . ?
C83 C85 C84 116.5(18) . 2_556 ?
C83 C85 H85 121.8 . . ?
C84 C85 H85 121.7 2_556 . ?
C87 C88 C87 119.1(11) . 2 ?
C87 C88 H88 120.5 . . ?
C87 C88 H88 120.5 2 . ?
C88 C87 C86 123.3(9) . . ?
C88 C87 H87 118.4 . . ?
C86 C87 H87 118.4 . . ?
C87 C86 N17 117.3(9) . . ?
C87 C86 H86 121.4 . . ?
N17 C86 H86 121.4 . . ?
C86 N17 C86 119.9(12) . 2 ?
C1 N1 C4 106.3(3) . . ?
C1 N1 U1 136.4(2) . . ?
C4 N1 U1 115.8(2) . . ?
C5 N2 C6 116.8(3) . . ?
C5 N2 U1 113.0(2) . . ?
C6 N2 U1 127.2(2) . . ?
C14 N3 C13 120.6(3) . . ?
C18 N4 C15 110.3(3) . . ?
C18 N4 H4 124.8 . . ?
C15 N4 H4 124.8 . . ?
C22 N5 C25 109.7(2) . . ?
C22 N5 H5A 125.1 . . ?
C25 N5 H5A 125.1 . . ?
C26 N6 C27 119.3(3) . . ?
C35 N7 C34 116.8(3) . . ?
C35 N7 U1 112.5(2) . . ?
C34 N7 U1 128.6(2) . . ?
C39 N8 C36 105.8(3) . . ?
C39 N8 U1 136.3(2) . . ?
C36 N8 U1 115.8(2) . . ?
C43 N9 C47 117.5(3) . . ?
C43 N9 U1 120.3(2) . . ?
C47 N9 U1 121.8(2) . . ?
C52 N10 C48 118.0(3) . . ?
C52 N10 Mg1 120.1(2) . . ?
C48 N10 Mg1 121.8(2) . . ?
C57 N11 C53 117.4(3) . . ?
C57 N11 Mg1 129.8(3) . . ?
C53 N11 Mg1 112.6(3) . . ?
C62 N12 C58 119.3(8) . . ?
N13 C63 C67 122.9(7) . . ?
N13 C63 H63 118.6 . . ?
C67 C63 H63 118.6 . . ?
C68 N14 C70 118.3(5) . . ?
N15 C73 C77 123.4(6) . . ?
N15 C73 H73 118.3 . . ?
C77 C73 H73 118.3 . . ?
C79 N16 C78 116.5(4) . . ?
Mg1 O2 U1 157.97(13) . . ?
O1 U1 O2 174.20(9) . . ?
O1 U1 N1 95.15(9) . . ?
O2 U1 N1 88.67(9) . . ?
O1 U1 N8 96.95(9) . . ?
O2 U1 N8 88.46(9) . . ?
N1 U1 N8 69.56(9) . . ?
O1 U1 N9 89.10(9) . . ?
O2 U1 N9 85.21(9) . . ?
N1 U1 N9 142.22(9) . . ?
N8 U1 N9 147.15(9) . . ?
O1 U1 N2 98.63(9) . . ?
O2 U1 N2 79.00(9) . . ?
N1 U1 N2 65.27(9) . . ?
N8 U1 N2 133.19(8) . . ?
N9 U1 N2 76.96(9) . . ?
O1 U1 N7 101.22(9) . . ?
O2 U1 N7 79.15(9) . . ?
N1 U1 N7 133.01(8) . . ?
N8 U1 N7 64.95(8) . . ?
N9 U1 N7 82.20(8) . . ?
N2 U1 N7 150.85(8) . . ?
O1 U1 Mg1 172.57(7) . . ?
O2 U1 Mg1 10.99(7) . . ?
N1 U1 Mg1 77.84(6) . . ?
N8 U1 Mg1 83.01(6) . . ?
N9 U1 Mg1 94.95(6) . . ?
N2 U1 Mg1 76.30(6) . . ?
N7 U1 Mg1 85.53(6) . . ?
O2 Mg1 N10 111.55(11) . . ?
O2 Mg1 N11 101.25(11) . . ?
N10 Mg1 N11 111.96(12) . . ?
O2 Mg1 Cl1 117.50(9) . . ?
N10 Mg1 Cl1 110.54(10) . . ?
N11 Mg1 Cl1 103.34(10) . . ?
O2 Mg1 U1 11.04(7) . . ?
N10 Mg1 U1 100.97(8) . . ?
N11 Mg1 U1 109.13(9) . . ?
Cl1 Mg1 U1 121.10(4) . . ?

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
N1 C1 C2 C3 0.2(4) . . . . ?
C40 C1 C2 C3 179.1(3) . . . . ?
C1 C2 C3 C4 0.0(4) . . . . ?
C2 C3 C4 N1 -0.1(4) . . . . ?
C2 C3 C4 C5 -173.2(3) . . . . ?
N1 C4 C5 N2 -1.0(5) . . . . ?
C3 C4 C5 N2 171.5(3) . . . . ?
C13 C6 C7 C8 -0.3(5) . . . . ?
N2 C6 C7 C8 -179.0(3) . . . . ?
C6 C7 C8 C10 0.3(5) . . . . ?
C6 C7 C8 C9 177.7(3) . . . . ?
C7 C8 C10 C12 -0.1(5) . . . . ?
C9 C8 C10 C12 -177.5(3) . . . . ?
C7 C8 C10 C11 -179.1(4) . . . . ?
C9 C8 C10 C11 3.5(6) . . . . ?
C8 C10 C12 C13 -0.1(5) . . . . ?
C11 C10 C12 C13 178.9(4) . . . . ?
C10 C12 C13 C6 0.1(5) . . . . ?
C10 C12 C13 N3 176.8(3) . . . . ?
C7 C6 C13 C12 0.1(5) . . . . ?
N2 C6 C13 C12 178.8(3) . . . . ?
C7 C6 C13 N3 -176.9(3) . . . . ?
N2 C6 C13 N3 1.8(4) . . . . ?
N3 C14 C15 N4 1.4(4) . . . . ?
N3 C14 C15 C16 -179.1(3) . . . . ?
N4 C15 C16 C17 0.2(3) . . . . ?
C14 C15 C16 C17 -179.5(3) . . . . ?
C15 C16 C17 C18 -0.3(4) . . . . ?
C16 C17 C18 N4 0.3(3) . . . . ?
C16 C17 C18 C19 176.0(3) . . . . ?
N4 C18 C19 C22 68.3(3) . . . . ?
C17 C18 C19 C22 -106.9(4) . . . . ?
N4 C18 C19 C20 -172.7(3) . . . . ?
C17 C18 C19 C20 12.1(4) . . . . ?
N4 C18 C19 C21 -52.8(4) . . . . ?
C17 C18 C19 C21 132.0(3) . . . . ?
C18 C19 C22 N5 -67.0(4) . . . . ?
C20 C19 C22 N5 173.5(3) . . . . ?
C21 C19 C22 N5 54.5(4) . . . . ?
C18 C19 C22 C23 109.6(4) . . . . ?
C20 C19 C22 C23 -9.9(5) . . . . ?
C21 C19 C22 C23 -128.9(3) . . . . ?
N5 C22 C23 C24 -0.3(4) . . . . ?
C19 C22 C23 C24 -177.3(3) . . . . ?
C22 C23 C24 C25 0.1(4) . . . . ?
C23 C24 C25 N5 0.2(4) . . . . ?
C23 C24 C25 C26 -177.6(3) . . . . ?
N5 C25 C26 N6 3.0(5) . . . . ?
C24 C25 C26 N6 -179.5(3) . . . . ?
C34 C27 C28 C29 -3.0(5) . . . . ?
N6 C27 C28 C29 176.2(3) . . . . ?
C27 C28 C29 C31 0.9(6) . . . . ?
C27 C28 C29 C30 -178.7(3) . . . . ?
C28 C29 C31 C33 1.7(6) . . . . ?
C30 C29 C31 C33 -178.7(4) . . . . ?
C28 C29 C31 C32 -177.8(4) . . . . ?
C30 C29 C31 C32 1.8(6) . . . . ?
C29 C31 C33 C34 -2.3(6) . . . . ?
C32 C31 C33 C34 177.2(4) . . . . ?
C31 C33 C34 C27 0.2(6) . . . . ?
C31 C33 C34 N7 -177.1(3) . . . . ?
C28 C27 C34 C33 2.4(5) . . . . ?
N6 C27 C34 C33 -176.9(3) . . . . ?
C28 C27 C34 N7 179.8(3) . . . . ?
N6 C27 C34 N7 0.5(5) . . . . ?
N7 C35 C36 N8 -1.4(5) . . . . ?
N7 C35 C36 C37 -173.7(3) . . . . ?
N8 C36 C37 C38 -0.2(4) . . . . ?
C35 C36 C37 C38 172.7(3) . . . . ?
C36 C37 C38 C39 0.1(4) . . . . ?
C37 C38 C39 N8 0.1(4) . . . . ?
C37 C38 C39 C40 -178.0(3) . . . . ?
N1 C1 C40 C39 -55.1(4) . . . . ?
C2 C1 C40 C39 126.1(3) . . . . ?
N1 C1 C40 C42 -176.2(3) . . . . ?
C2 C1 C40 C42 5.0(5) . . . . ?
N1 C1 C40 C41 64.1(4) . . . . ?
C2 C1 C40 C41 -114.8(3) . . . . ?
N8 C39 C40 C1 56.8(4) . . . . ?
C38 C39 C40 C1 -125.3(3) . . . . ?
N8 C39 C40 C42 178.0(3) . . . . ?
C38 C39 C40 C42 -4.1(5) . . . . ?
N8 C39 C40 C41 -63.0(4) . . . . ?
C38 C39 C40 C41 114.9(4) . . . . ?
N9 C43 C44 C45 0.9(6) . . . . ?
C43 C44 C45 C46 -1.0(5) . . . . ?
C44 C45 C46 C47 0.0(5) . . . . ?
C45 C46 C47 N9 1.1(5) . . . . ?
N10 C48 C49 C50 -0.1(5) . . . . ?
C48 C49 C50 C51 1.7(5) . . . . ?
C49 C50 C51 C52 -1.4(5) . . . . ?
C50 C51 C52 N10 -0.5(5) . . . . ?
N11 C53 C54 C55 0.2(7) . . . . ?
C53 C54 C55 C56 -0.1(7) . . . . ?
C54 C55 C56 C57 -0.4(7) . . . . ?
C55 C56 C57 N11 0.9(7) . . . . ?
N12 C58 C59 C60 3.2(11) . . . . ?
C58 C59 C60 C61 -0.4(15) . . . . ?
C59 C60 C61 C62 -5.7(19) . . . . ?
C60 C61 C62 N12 9(2) . . . . ?
C63 N13 C64 C65 -1.9(10) . . . . ?
N13 C64 C65 C66 -0.5(11) . . . . ?
C64 C65 C66 C67 3.0(12) . . . . ?
C65 C66 C67 C63 -3.1(13) . . . . ?
N14 C68 C69 C72 -0.7(9) . . . . ?
N14 C70 C71 C72 0.4(10) . . . . ?
C70 C71 C72 C69 -0.3(10) . . . . ?
C68 C69 C72 C71 0.5(9) . . . . ?
C73 N15 C74 C75 3.0(8) . . . . ?
N15 C74 C75 C76 -3.2(8) . . . . ?
C74 C75 C76 C77 1.3(9) . . . . ?
C75 C76 C77 C73 0.5(9) . . . . ?
N16 C79 C80 C81 -0.3(8) . . . . ?
C79 C80 C81 C82 0.1(7) . . . . ?
N16 C78 C82 C81 -0.9(8) . . . . ?
C80 C81 C82 C78 0.5(7) . . . . ?
C85 C83 C84 C85 0(3) . . . 2_556 ?
C84 C83 C85 C84 4(2) . . . 2_556 ?
C87 C88 C87 C86 -0.1(7) 2 . . . ?
C88 C87 C86 N17 0.2(13) . . . . ?
C87 C86 N17 C86 -0.1(6) . . . 2 ?
C2 C1 N1 C4 -0.3(3) . . . . ?
C40 C1 N1 C4 -179.3(3) . . . . ?
C2 C1 N1 U1 -165.0(2) . . . . ?
C40 C1 N1 U1 16.0(4) . . . . ?
C3 C4 N1 C1 0.2(4) . . . . ?
C5 C4 N1 C1 174.0(3) . . . . ?
C3 C4 N1 U1 168.6(2) . . . . ?
C5 C4 N1 U1 -17.6(4) . . . . ?
C4 C5 N2 C6 179.3(3) . . . . ?
C4 C5 N2 U1 17.7(4) . . . . ?
C7 C6 N2 C5 -53.4(4) . . . . ?
C13 C6 N2 C5 127.9(3) . . . . ?
C7 C6 N2 U1 105.2(3) . . . . ?
C13 C6 N2 U1 -73.5(4) . . . . ?
C15 C14 N3 C13 -177.2(3) . . . . ?
C12 C13 N3 C14 28.9(5) . . . . ?
C6 C13 N3 C14 -154.3(3) . . . . ?
C17 C18 N4 C15 -0.2(3) . . . . ?
C19 C18 N4 C15 -176.4(3) . . . . ?
C16 C15 N4 C18 0.0(3) . . . . ?
C14 C15 N4 C18 179.7(3) . . . . ?
C23 C22 N5 C25 0.4(3) . . . . ?
C19 C22 N5 C25 177.7(3) . . . . ?
C24 C25 N5 C22 -0.3(3) . . . . ?
C26 C25 N5 C22 177.6(3) . . . . ?
C25 C26 N6 C27 178.5(3) . . . . ?
C28 C27 N6 C26 -35.6(5) . . . . ?
C34 C27 N6 C26 143.6(3) . . . . ?
C36 C35 N7 C34 178.1(3) . . . . ?
C36 C35 N7 U1 -16.7(4) . . . . ?
C33 C34 N7 C35 42.5(5) . . . . ?
C27 C34 N7 C35 -134.8(3) . . . . ?
C33 C34 N7 U1 -119.9(3) . . . . ?
C27 C34 N7 U1 62.8(4) . . . . ?
C38 C39 N8 C36 -0.1(4) . . . . ?
C40 C39 N8 C36 178.1(3) . . . . ?
C38 C39 N8 U1 161.8(2) . . . . ?
C40 C39 N8 U1 -19.9(5) . . . . ?
C37 C36 N8 C39 0.2(4) . . . . ?
C35 C36 N8 C39 -173.5(3) . . . . ?
C37 C36 N8 U1 -166.0(2) . . . . ?
C35 C36 N8 U1 20.3(4) . . . . ?
C44 C43 N9 C47 0.2(5) . . . . ?
C44 C43 N9 U1 174.1(3) . . . . ?
C46 C47 N9 C43 -1.2(5) . . . . ?
C46 C47 N9 U1 -175.1(2) . . . . ?
C51 C52 N10 C48 2.1(5) . . . . ?
C51 C52 N10 Mg1 -175.4(3) . . . . ?
C49 C48 N10 C52 -1.8(5) . . . . ?
C49 C48 N10 Mg1 175.6(2) . . . . ?
C56 C57 N11 C53 -0.7(6) . . . . ?
C56 C57 N11 Mg1 174.4(3) . . . . ?
C54 C53 N11 C57 0.2(6) . . . . ?
C54 C53 N11 Mg1 -175.8(4) . . . . ?
C61 C62 N12 C58 -6.0(17) . . . . ?
C59 C58 N12 C62 0.1(13) . . . . ?
C64 N13 C63 C67 1.8(10) . . . . ?
C66 C67 C63 N13 0.7(12) . . . . ?
C69 C68 N14 C70 0.8(9) . . . . ?
C71 C70 N14 C68 -0.6(10) . . . . ?
C74 N15 C73 C77 -1.0(10) . . . . ?
C76 C77 C73 N15 -0.7(10) . . . . ?
C80 C79 N16 C78 0.0(8) . . . . ?
C82 C78 N16 C79 0.6(8) . . . . ?
Mg1 O2 U1 O1 -141.0(8) . . . . ?
Mg1 O2 U1 N1 -9.6(4) . . . . ?
Mg1 O2 U1 N8 60.0(4) . . . . ?
Mg1 O2 U1 N9 -152.3(4) . . . . ?
Mg1 O2 U1 N2 -74.6(4) . . . . ?
Mg1 O2 U1 N7 124.8(4) . . . . ?
C1 N1 U1 O1 -81.3(3) . . . . ?
C4 N1 U1 O1 115.0(2) . . . . ?
C1 N1 U1 O2 103.0(3) . . . . ?
C4 N1 U1 O2 -60.7(2) . . . . ?
C1 N1 U1 N8 14.2(3) . . . . ?
C4 N1 U1 N8 -149.5(2) . . . . ?
C1 N1 U1 N9 -176.5(3) . . . . ?
C4 N1 U1 N9 19.8(3) . . . . ?
C1 N1 U1 N2 -178.5(3) . . . . ?
C4 N1 U1 N2 17.8(2) . . . . ?
C1 N1 U1 N7 29.2(3) . . . . ?
C4 N1 U1 N7 -134.5(2) . . . . ?
C1 N1 U1 Mg1 101.2(3) . . . . ?
C4 N1 U1 Mg1 -62.5(2) . . . . ?
C39 N8 U1 O1 80.9(3) . . . . ?
C36 N8 U1 O1 -118.5(2) . . . . ?
C39 N8 U1 O2 -101.2(3) . . . . ?
C36 N8 U1 O2 59.5(2) . . . . ?
C39 N8 U1 N1 -12.0(3) . . . . ?
C36 N8 U1 N1 148.6(2) . . . . ?
C39 N8 U1 N9 -179.9(3) . . . . ?
C36 N8 U1 N9 -19.3(3) . . . . ?
C39 N8 U1 N2 -27.9(3) . . . . ?
C36 N8 U1 N2 132.8(2) . . . . ?
C39 N8 U1 N7 -179.9(3) . . . . ?
C36 N8 U1 N7 -19.3(2) . . . . ?
C39 N8 U1 Mg1 -91.6(3) . . . . ?
C36 N8 U1 Mg1 69.0(2) . . . . ?
C43 N9 U1 O1 -168.5(3) . . . . ?
C47 N9 U1 O1 5.2(2) . . . . ?
C43 N9 U1 O2 10.4(3) . . . . ?
C47 N9 U1 O2 -175.9(3) . . . . ?
C43 N9 U1 N1 -71.2(3) . . . . ?
C47 N9 U1 N1 102.5(3) . . . . ?
C43 N9 U1 N8 90.1(3) . . . . ?
C47 N9 U1 N8 -96.3(3) . . . . ?
C43 N9 U1 N2 -69.4(3) . . . . ?
C47 N9 U1 N2 104.3(2) . . . . ?
C43 N9 U1 N7 90.1(3) . . . . ?
C47 N9 U1 N7 -96.3(2) . . . . ?
C43 N9 U1 Mg1 5.3(3) . . . . ?
C47 N9 U1 Mg1 179.0(2) . . . . ?
C5 N2 U1 O1 -110.0(2) . . . . ?
C6 N2 U1 O1 90.6(3) . . . . ?
C5 N2 U1 O2 75.3(2) . . . . ?
C6 N2 U1 O2 -84.0(3) . . . . ?
C5 N2 U1 N1 -18.3(2) . . . . ?
C6 N2 U1 N1 -177.6(3) . . . . ?
C5 N2 U1 N8 -2.0(3) . . . . ?
C6 N2 U1 N8 -161.3(2) . . . . ?
C5 N2 U1 N9 162.9(2) . . . . ?
C6 N2 U1 N9 3.6(2) . . . . ?
C5 N2 U1 N7 117.4(2) . . . . ?
C6 N2 U1 N7 -41.9(3) . . . . ?
C5 N2 U1 Mg1 64.4(2) . . . . ?
C6 N2 U1 Mg1 -94.9(2) . . . . ?
C35 N7 U1 O1 111.0(2) . . . . ?
C34 N7 U1 O1 -86.0(3) . . . . ?
C35 N7 U1 O2 -74.9(2) . . . . ?
C34 N7 U1 O2 88.1(3) . . . . ?
C35 N7 U1 N1 2.9(3) . . . . ?
C34 N7 U1 N1 166.0(2) . . . . ?
C35 N7 U1 N8 18.5(2) . . . . ?
C34 N7 U1 N8 -178.4(3) . . . . ?
C35 N7 U1 N9 -161.5(2) . . . . ?
C34 N7 U1 N9 1.6(3) . . . . ?
C35 N7 U1 N2 -117.0(2) . . . . ?
C34 N7 U1 N2 46.1(3) . . . . ?
C35 N7 U1 Mg1 -65.8(2) . . . . ?
C34 N7 U1 Mg1 97.2(3) . . . . ?
U1 O2 Mg1 N10 -17.2(4) . . . . ?
U1 O2 Mg1 N11 -136.5(4) . . . . ?
U1 O2 Mg1 Cl1 111.9(4) . . . . ?
C52 N10 Mg1 O2 -56.8(3) . . . . ?
C48 N10 Mg1 O2 125.8(2) . . . . ?
C52 N10 Mg1 N11 55.9(3) . . . . ?
C48 N10 Mg1 N11 -121.5(3) . . . . ?
C52 N10 Mg1 Cl1 170.5(2) . . . . ?
C48 N10 Mg1 Cl1 -6.9(3) . . . . ?
C52 N10 Mg1 U1 -60.1(2) . . . . ?
C48 N10 Mg1 U1 122.5(2) . . . . ?
C57 N11 Mg1 O2 118.6(3) . . . . ?
C53 N11 Mg1 O2 -66.1(3) . . . . ?
C57 N11 Mg1 N10 -0.3(4) . . . . ?
C53 N11 Mg1 N10 175.0(3) . . . . ?
C57 N11 Mg1 Cl1 -119.3(3) . . . . ?
C53 N11 Mg1 Cl1 56.0(3) . . . . ?
C57 N11 Mg1 U1 110.6(3) . . . . ?
C53 N11 Mg1 U1 -74.1(3) . . . . ?
O1 U1 Mg1 O2 150.6(6) . . . . ?
N1 U1 Mg1 O2 170.2(4) . . . . ?
N8 U1 Mg1 O2 -119.3(4) . . . . ?
N9 U1 Mg1 O2 27.7(4) . . . . ?
N2 U1 Mg1 O2 103.0(4) . . . . ?
N7 U1 Mg1 O2 -54.0(4) . . . . ?
O1 U1 Mg1 N10 -45.7(5) . . . . ?
O2 U1 Mg1 N10 163.7(4) . . . . ?
N1 U1 Mg1 N10 -26.11(11) . . . . ?
N8 U1 Mg1 N10 44.41(11) . . . . ?
N9 U1 Mg1 N10 -168.56(11) . . . . ?
N2 U1 Mg1 N10 -93.29(11) . . . . ?
N7 U1 Mg1 N10 109.68(11) . . . . ?
O1 U1 Mg1 N11 -163.8(5) . . . . ?
O2 U1 Mg1 N11 45.6(4) . . . . ?
N1 U1 Mg1 N11 -144.17(12) . . . . ?
N8 U1 Mg1 N11 -73.66(11) . . . . ?
N9 U1 Mg1 N11 73.37(11) . . . . ?
N2 U1 Mg1 N11 148.65(12) . . . . ?
N7 U1 Mg1 N11 -8.38(11) . . . . ?
O1 U1 Mg1 Cl1 76.6(5) . . . . ?
O2 U1 Mg1 Cl1 -74.0(4) . . . . ?
N1 U1 Mg1 Cl1 96.19(8) . . . . ?
N8 U1 Mg1 Cl1 166.71(8) . . . . ?
N9 U1 Mg1 Cl1 -46.26(8) . . . . ?
N2 U1 Mg1 Cl1 29.01(8) . . . . ?
N7 U1 Mg1 Cl1 -128.02(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        76.31
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.358
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.083

_vrf_PLAT412_po4006_refinalized  
;
PROBLEM: Short Intra XH3 .. XHn H9A .. H11A ..
1.69 Ang and Short Intra XH3 .. XHn H30A .. H32A ..
1.69 Ang.
RESPONSE: The methyl groups on the phenyl ring of
the ligand were placed geometrically. This 
resulted in an eclipsed confirmation and a short 
intramolecular H..H contact for two adjacent 
methyl-H atoms on which no further modelling 
was undertaken, hence the Alert.
;
####################################################################### 
# 
# 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_po15003_refinalized
_database_code_depnum_ccdc_archive 'CCDC 1883757'
loop_
_audit_author_name
_audit_author_address
'Gary Nichol'
;university of edinburgh
United Kingdom
;
_audit_update_record             
;
2018-12-07 deposited with the CCDC.	2019-08-27 downloaded from the CCDC.
;
_audit_creation_date             2015-03-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C282 H282 Cs6 N54 O12 U6, 6(C5 H5 N)'
_chemical_formula_sum            'C312 H312 Cs6 N60 O12 U6'
_chemical_formula_weight         7319.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C54 H54 Cs N12 O2 U'
_chemical_oxdiff_usercomment     '@ 120 K RML126'
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'
Cs Cs -0.7457 7.9052 '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'

_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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   27.7671(4)
_cell_length_b                   27.7671(4)
_cell_length_c                   35.7644(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     23880.5(8)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    21727
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      75.7770
_cell_measurement_theta_min      3.0797
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    14.249
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.992
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             10746
_exptl_crystal_size_max          0.0466
_exptl_crystal_size_mid          0.0416
_exptl_crystal_size_min          0.0293
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0962
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            123779
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.240
_diffrn_reflns_theta_min         3.080
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -122.00   -7.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.4186  -19.0000  -30.0000 115

#__ type_ start__ end____ width___ exp.time_
  2 omega  -75.00   30.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.4186   77.0000 -120.0000 105

#__ type_ start__ end____ width___ exp.time_
  3 omega  -50.00   29.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.4186   38.0000  150.0000 79

#__ type_ start__ end____ width___ exp.time_
  4 omega  -95.00   -2.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.4186  125.0000 -120.0000 93

#__ type_ start__ end____ width___ exp.time_
  5 omega   23.00   98.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4186 -125.0000   30.0000 75

#__ type_ start__ end____ width___ exp.time_
  6 omega   23.00   98.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4186 -125.0000  -90.0000 75

#__ type_ start__ end____ width___ exp.time_
  7 omega   37.00  142.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000  120.0000 105

#__ type_ start__ end____ width___ exp.time_
  8 omega   66.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000 -150.0000 112

#__ type_ start__ end____ width___ exp.time_
  9 omega   39.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -120.0000 82

#__ type_ start__ end____ width___ exp.time_
 10 omega   30.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -60.0000 79

#__ type_ start__ end____ width___ exp.time_
 11 omega   40.00   98.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   90.0000 58

#__ type_ start__ end____ width___ exp.time_
 12 omega   36.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000    0.0000 55

#__ type_ start__ end____ width___ exp.time_
 13 omega   36.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -120.0000 55

#__ type_ start__ end____ width___ exp.time_
 14 omega   40.00   98.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -60.0000 58

#__ type_ start__ end____ width___ exp.time_
 15 omega   30.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 79

#__ type_ start__ end____ width___ exp.time_
 16 omega   39.00  121.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   60.0000 82

#__ type_ start__ end____ width___ exp.time_
 17 omega   87.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000  -90.0000 91

#__ type_ start__ end____ width___ exp.time_
 18 omega   40.00   98.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   30.0000 58

#__ type_ start__ end____ width___ exp.time_
 19 omega   30.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   60.0000 79

#__ type_ start__ end____ width___ exp.time_
 20 omega   36.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -60.0000 55

#__ type_ start__ end____ width___ exp.time_
 21 omega   40.00   98.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -150.0000 58

#__ type_ start__ end____ width___ exp.time_
 22 omega -114.00  -17.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.4186  -57.0000 -120.0000 97

#__ type_ start__ end____ width___ exp.time_
 23 omega -117.00  -12.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.4186  -77.0000  -30.0000 105

#__ type_ start__ end____ width___ exp.time_
 24 omega -117.00  -12.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.4186  -77.0000  150.0000 105

#__ type_ start__ end____ width___ exp.time_
 25 omega -117.00  -12.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.4186  -77.0000 -150.0000 105

#__ type_ start__ end____ width___ exp.time_
 26 omega  -50.00   29.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.4186   38.0000   60.0000 79

#__ type_ start__ end____ width___ exp.time_
 27 omega -117.00  -12.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.4186  -77.0000   60.0000 105

#__ type_ start__ end____ width___ exp.time_
 28 omega   66.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000   60.0000 112

#__ type_ start__ end____ width___ exp.time_
 29 omega   87.00  137.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000  120.0000 50

#__ type_ start__ end____ width___ exp.time_
 30 omega   87.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000  -30.0000 91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0023395000
_diffrn_orient_matrix_UB_12      -0.0541677000
_diffrn_orient_matrix_UB_13      -0.0126432000
_diffrn_orient_matrix_UB_21      -0.0412007000
_diffrn_orient_matrix_UB_22      -0.0068761000
_diffrn_orient_matrix_UB_23      -0.0312236000
_diffrn_orient_matrix_UB_31      0.0490105000
_diffrn_orient_matrix_UB_32      0.0335224000
_diffrn_orient_matrix_UB_33      -0.0268371000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9096
_reflns_number_total             11060
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         12.923
_refine_diff_density_min         -1.915
_refine_diff_density_rms         0.228
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         11060
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0658
_refine_ls_restrained_S_all      1.026
_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)+(0.0917P)²+1001.9244P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1764
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C45) = Uanis(C47)
Uanis(C44) = Uanis(C43)
3. Rigid body (RIGU) restrains
 C43, C44, C45, C46, C47
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 N5(H5), N6(H6), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C2(H2),
 C3(H3), C5(H5A), C7(H7), C12(H12), C14(H14), C16(H16), C17(H17), C23(H23),
 C24(H24), C26(H26), C28(H28), C33(H33), C35(H35), C37(H37), C38(H38), C48(H48),
  C49(H49), C50(H50), C51(H51), C52(H52)
4.b Fitted hexagon refined as free rotating group:
 N9(C43,C44,C45,C46,C47)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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 0.52534(2) 0.51819(2) 0.69183(2) 0.02449(11) Uani 1 1 d . . . . .
Cs1 Cs 0.58512(2) 0.68607(2) 0.67146(2) 0.02756(14) Uani 1 1 d . . . . .
O1 O 0.4662(3) 0.4563(3) 0.71387(19) 0.0323(15) Uani 1 1 d . . . . .
O2 O 0.5808(3) 0.5770(3) 0.66627(18) 0.0290(14) Uani 1 1 d . . . . .
N1 N 0.4628(3) 0.5563(3) 0.6739(2) 0.0270(17) Uani 1 1 d . . . . .
N2 N 0.4821(4) 0.4923(4) 0.6227(2) 0.0302(18) Uani 1 1 d . . . . .
N3 N 0.4311(4) 0.3790(4) 0.6325(3) 0.038(2) Uani 1 1 d . . . . .
N4 N 0.3778(4) 0.3372(4) 0.7004(2) 0.0307(18) Uani 1 1 d . . . . .
N5 N 0.4492(4) 0.3781(3) 0.7741(2) 0.0290(17) Uani 1 1 d . . . . .
H5 H 0.4558 0.4002 0.7548 0.035 Uiso 1 1 calc R . . . .
N6 N 0.5648(4) 0.4449(4) 0.7595(2) 0.0335(19) Uani 1 1 d . . . . .
H6 H 0.5413 0.4477 0.7444 0.040 Uiso 1 1 calc R . . . .
N7 N 0.6081(4) 0.5527(3) 0.7410(2) 0.0299(18) Uani 1 1 d . . . . .
N8 N 0.5325(3) 0.5897(3) 0.7397(2) 0.0246(16) Uani 1 1 d . . . . .
N9 N 0.5698(5) 0.4640(4) 0.6666(3) 0.052(3) Uani 1 1 d . . . . .
C43 C 0.6180(7) 0.4941(5) 0.6457(6) 0.256(18) Uani 1 1 d G U . . .
H43 H 0.6324 0.5327 0.6414 0.307 Uiso 1 1 calc R . . . .
C44 C 0.6451(8) 0.4677(8) 0.6309(7) 0.256(18) Uani 1 1 d G U . . .
H44 H 0.6781 0.4883 0.6166 0.307 Uiso 1 1 calc R . . . .
C45 C 0.6241(9) 0.4113(8) 0.6371(6) 0.163(9) Uani 1 1 d G U . . .
H45 H 0.6426 0.3933 0.6270 0.196 Uiso 1 1 calc R . . . .
C46 C 0.5759(9) 0.3812(5) 0.6581(5) 0.151(10) Uani 1 1 d G U . . .
H46 H 0.5615 0.3426 0.6623 0.181 Uiso 1 1 calc R . . . .
C47 C 0.5488(6) 0.4075(4) 0.6728(5) 0.163(9) Uani 1 1 d G U . . .
H47 H 0.5159 0.3870 0.6872 0.196 Uiso 1 1 calc R . . . .
C1 C 0.4470(4) 0.5909(4) 0.6898(3) 0.028(2) Uani 1 1 d . . . . .
C2 C 0.4367(4) 0.6202(4) 0.6625(3) 0.033(2) Uani 1 1 d . . . . .
H2 H 0.4265 0.6477 0.6667 0.039 Uiso 1 1 calc R . . . .
C3 C 0.4441(4) 0.6020(4) 0.6278(3) 0.034(2) Uani 1 1 d . . . . .
H3 H 0.4386 0.6135 0.6039 0.040 Uiso 1 1 calc R . . . .
C4 C 0.4613(4) 0.5632(4) 0.6352(3) 0.031(2) Uani 1 1 d . . . . .
C5 C 0.4711(4) 0.5295(4) 0.6106(3) 0.031(2) Uani 1 1 d . . . . .
H5A H 0.4695 0.5343 0.5845 0.037 Uiso 1 1 calc R . . . .
C6 C 0.4896(5) 0.4592(5) 0.5954(3) 0.035(2) Uani 1 1 d . . . . .
C7 C 0.5229(5) 0.4840(5) 0.5635(3) 0.038(2) Uani 1 1 d . . . . .
H7 H 0.5408 0.5232 0.5606 0.045 Uiso 1 1 calc R . . . .
C8 C 0.5299(5) 0.4526(6) 0.5366(3) 0.048(3) Uani 1 1 d . . . . .
C9 C 0.5677(6) 0.4813(6) 0.5036(3) 0.057(4) Uani 1 1 d . . . . .
H9A H 0.5760 0.5200 0.5023 0.085 Uiso 1 1 calc GR . . . .
H9B H 0.5493 0.4620 0.4804 0.085 Uiso 1 1 calc GR . . . .
H9C H 0.6025 0.4806 0.5066 0.085 Uiso 1 1 calc GR . . . .
C10 C 0.5026(7) 0.3953(6) 0.5402(4) 0.061(4) Uani 1 1 d . . . . .
C11 C 0.5084(9) 0.3596(7) 0.5107(5) 0.094(7) Uani 1 1 d . . . . .
H11A H 0.5142 0.3776 0.4862 0.141 Uiso 1 1 calc GR . . . .
H11B H 0.4745 0.3231 0.5100 0.141 Uiso 1 1 calc GR . . . .
H11C H 0.5403 0.3550 0.5167 0.141 Uiso 1 1 calc GR . . . .
C12 C 0.4712(7) 0.3713(6) 0.5713(4) 0.058(4) Uani 1 1 d . . . . .
H12 H 0.4535 0.3320 0.5739 0.069 Uiso 1 1 calc R . . . .
C13 C 0.4640(5) 0.4021(5) 0.5994(3) 0.039(3) Uani 1 1 d . . . . .
C14 C 0.3961(5) 0.3275(5) 0.6346(3) 0.036(2) Uani 1 1 d . . . . .
H14 H 0.3893 0.3040 0.6136 0.044 Uiso 1 1 calc R . . . .
C15 C 0.3664(4) 0.3045(4) 0.6695(3) 0.032(2) Uani 1 1 d . . . . .
C16 C 0.3249(5) 0.2513(5) 0.6781(3) 0.043(3) Uani 1 1 d . . . . .
H16 H 0.3098 0.2200 0.6618 0.051 Uiso 1 1 calc R . . . .
C17 C 0.3093(5) 0.2518(5) 0.7154(3) 0.040(3) Uani 1 1 d . . . . .
H17 H 0.2811 0.2212 0.7289 0.048 Uiso 1 1 calc R . . . .
C18 C 0.3427(4) 0.3056(4) 0.7289(3) 0.031(2) Uani 1 1 d . . . . .
C19 C 0.3450(5) 0.3295(5) 0.7669(3) 0.034(2) Uani 1 1 d . . . . .
C20 C 0.2942(5) 0.2878(6) 0.7896(4) 0.048(3) Uani 1 1 d . . . . .
H20A H 0.2601 0.2817 0.7771 0.072 Uiso 1 1 calc GR . . . .
H20B H 0.2960 0.3027 0.8147 0.072 Uiso 1 1 calc GR . . . .
H20C H 0.2939 0.2524 0.7914 0.072 Uiso 1 1 calc GR . . . .
C21 C 0.3436(5) 0.3843(5) 0.7638(3) 0.039(3) Uani 1 1 d . . . . .
H21A H 0.3770 0.4122 0.7507 0.059 Uiso 1 1 calc GR . . . .
H21B H 0.3424 0.3978 0.7889 0.059 Uiso 1 1 calc GR . . . .
H21C H 0.3105 0.3776 0.7498 0.059 Uiso 1 1 calc GR . . . .
C22 C 0.3972(5) 0.3395(4) 0.7865(3) 0.033(2) Uani 1 1 d . . . . .
C23 C 0.4056(5) 0.3141(5) 0.8170(3) 0.041(3) Uani 1 1 d . . . . .
H23 H 0.3771 0.2851 0.8314 0.049 Uiso 1 1 calc R . . . .
C24 C 0.4624(5) 0.3378(5) 0.8233(3) 0.041(3) Uani 1 1 d . . . . .
H24 H 0.4795 0.3284 0.8428 0.049 Uiso 1 1 calc R . . . .
C25 C 0.4894(5) 0.3773(4) 0.7959(3) 0.034(2) Uani 1 1 d . . . . .
C26 C 0.5472(4) 0.4124(4) 0.7882(3) 0.033(2) Uani 1 1 d . . . . .
H26 H 0.5736 0.4119 0.8048 0.039 Uiso 1 1 calc R . . . .
C27 C 0.6225(5) 0.4758(4) 0.7531(3) 0.033(2) Uani 1 1 d . . . . .
C28 C 0.6568(5) 0.4537(5) 0.7549(4) 0.046(3) Uani 1 1 d . . . . .
H28 H 0.6411 0.4152 0.7603 0.055 Uiso 1 1 calc R . . . .
C29 C 0.7141(5) 0.4858(6) 0.7492(5) 0.060(4) Uani 1 1 d . . . . .
C30 C 0.7496(7) 0.4595(8) 0.7514(7) 0.100(8) Uani 1 1 d . . . . .
H30A H 0.7745 0.4744 0.7730 0.150 Uiso 1 1 calc GR . . . .
H30B H 0.7718 0.4677 0.7285 0.150 Uiso 1 1 calc GR . . . .
H30C H 0.7259 0.4192 0.7541 0.150 Uiso 1 1 calc GR . . . .
C31 C 0.7373(5) 0.5422(6) 0.7414(4) 0.051(3) Uani 1 1 d . . . . .
C32 C 0.7995(6) 0.5787(8) 0.7347(6) 0.079(5) Uani 1 1 d . . . . .
H32A H 0.8198 0.5796 0.7573 0.118 Uiso 1 1 calc GR . . . .
H32B H 0.8079 0.6166 0.7285 0.118 Uiso 1 1 calc GR . . . .
H32C H 0.8107 0.5635 0.7139 0.118 Uiso 1 1 calc GR . . . .
C33 C 0.7019(5) 0.5638(5) 0.7386(4) 0.042(3) Uani 1 1 d . . . . .
H33 H 0.7173 0.6021 0.7326 0.050 Uiso 1 1 calc R . . . .
C34 C 0.6458(5) 0.5324(5) 0.7440(3) 0.035(2) Uani 1 1 d . . . . .
C35 C 0.6225(4) 0.6006(4) 0.7559(3) 0.030(2) Uani 1 1 d . . . . .
H35 H 0.6579 0.6215 0.7675 0.035 Uiso 1 1 calc R . . . .
C36 C 0.5850(4) 0.6222(4) 0.7550(3) 0.0273(19) Uani 1 1 d . . . . .
C37 C 0.5906(4) 0.6714(4) 0.7699(3) 0.030(2) Uani 1 1 d . . . . .
H37 H 0.6227 0.7006 0.7816 0.036 Uiso 1 1 calc R . . . .
C38 C 0.5399(4) 0.6690(4) 0.7642(3) 0.030(2) Uani 1 1 d . . . . .
H38 H 0.5306 0.6963 0.7715 0.036 Uiso 1 1 calc R . . . .
C39 C 0.5050(4) 0.6187(4) 0.7455(3) 0.0263(19) Uani 1 1 d . . . . .
C40 C 0.4464(4) 0.5948(4) 0.7315(3) 0.0263(19) Uani 1 1 d . . . . .
C41 C 0.4235(5) 0.6330(5) 0.7429(3) 0.036(2) Uani 1 1 d . . . . .
H41A H 0.4462 0.6698 0.7316 0.054 Uiso 1 1 calc GR . . . .
H41B H 0.4246 0.6367 0.7702 0.054 Uiso 1 1 calc GR . . . .
H41C H 0.3850 0.6169 0.7343 0.054 Uiso 1 1 calc GR . . . .
C42 C 0.4090(4) 0.5370(4) 0.7492(3) 0.031(2) Uani 1 1 d . . . . .
H42A H 0.3723 0.5193 0.7373 0.046 Uiso 1 1 calc GR . . . .
H42B H 0.4050 0.5412 0.7760 0.046 Uiso 1 1 calc GR . . . .
H42C H 0.4260 0.5138 0.7454 0.046 Uiso 1 1 calc GR . . . .
N10 N 0.8066(7) 0.7003(7) 0.7779(4) 0.076(4) Uani 1 1 d . . . . .
C48 C 0.8571(7) 0.7436(7) 0.7722(4) 0.060(4) Uani 1 1 d . . . . .
H48 H 0.8651 0.7630 0.7491 0.072 Uiso 1 1 calc R . . . .
C49 C 0.8992(6) 0.7613(6) 0.7994(5) 0.060(4) Uani 1 1 d . . . . .
H49 H 0.9349 0.7926 0.7951 0.072 Uiso 1 1 calc R . . . .
C50 C 0.8873(6) 0.7321(6) 0.8326(3) 0.047(3) Uani 1 1 d . . . . .
H50 H 0.9149 0.7425 0.8514 0.057 Uiso 1 1 calc R . . . .
C51 C 0.8359(7) 0.6887(7) 0.8378(5) 0.067(4) Uani 1 1 d . . . . .
H51 H 0.8273 0.6676 0.8602 0.080 Uiso 1 1 calc R . . . .
C52 C 0.7962(7) 0.6748(6) 0.8114(5) 0.066(4) Uani 1 1 d . . . . .
H52 H 0.7594 0.6458 0.8167 0.079 Uiso 1 1 calc R . . . .


_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 Cs1 4.1566(6) . ?
U1 Cs1 4.2872(6) 14_456 ?
U1 O1 1.858(7) . ?
U1 O2 1.832(7) . ?
U1 N1 2.527(9) . ?
U1 N2 2.685(8) . ?
U1 N7 2.661(9) . ?
U1 N8 2.554(8) . ?
U1 N9 2.542(8) . ?
Cs1 O1 3.439(7) 15_556 ?
Cs1 O2 2.977(7) . ?
Cs1 N1 3.264(8) 15_556 ?
Cs1 N2 3.417(9) 15_556 ?
Cs1 N3 3.395(10) 15_556 ?
Cs1 N4 3.396(8) 15_556 ?
Cs1 N8 3.369(8) . ?
Cs1 C1 3.462(10) . ?
Cs1 C4 3.467(10) 15_556 ?
Cs1 C36 3.475(9) . ?
Cs1 C38 3.493(10) . ?
Cs1 C39 3.362(10) . ?
O1 Cs1 3.439(7) 14_456 ?
N1 Cs1 3.264(8) 14_456 ?
N1 C1 1.363(13) . ?
N1 C4 1.400(12) . ?
N2 Cs1 3.417(8) 14_456 ?
N2 C5 1.288(14) . ?
N2 C6 1.425(13) . ?
N3 Cs1 3.395(10) 14_456 ?
N3 C13 1.437(14) . ?
N3 C14 1.268(14) . ?
N4 Cs1 3.397(8) 14_456 ?
N4 C15 1.365(14) . ?
N4 C18 1.380(12) . ?
N5 H5 0.8800 . ?
N5 C22 1.373(13) . ?
N5 C25 1.370(13) . ?
N6 H6 0.8800 . ?
N6 C26 1.289(14) . ?
N6 C27 1.409(14) . ?
N7 C34 1.421(13) . ?
N7 C35 1.297(14) . ?
N8 C36 1.388(12) . ?
N8 C39 1.373(12) . ?
N9 C43 1.3900 . ?
N9 C47 1.3900 . ?
C43 H43 0.9500 . ?
C43 C44 1.3900 . ?
C44 H44 0.9500 . ?
C44 C45 1.3900 . ?
C45 H45 0.9500 . ?
C45 C46 1.3900 . ?
C46 H46 0.9500 . ?
C46 C47 1.3900 . ?
C47 H47 0.9500 . ?
C1 C2 1.390(14) . ?
C1 C40 1.496(14) . ?
C2 H2 0.9500 . ?
C2 C3 1.392(16) . ?
C3 H3 0.9500 . ?
C3 C4 1.407(15) . ?
C4 Cs1 3.466(10) 14_456 ?
C4 C5 1.404(15) . ?
C5 Cs1 3.530(9) 14_456 ?
C5 H5A 0.9500 . ?
C6 C7 1.412(14) . ?
C6 C13 1.384(15) . ?
C7 H7 0.9500 . ?
C7 C8 1.377(17) . ?
C8 C9 1.516(15) . ?
C8 C10 1.384(19) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.512(19) . ?
C10 C12 1.362(16) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12 0.9500 . ?
C12 C13 1.398(15) . ?
C14 Cs1 3.842(11) 14_456 ?
C14 H14 0.9500 . ?
C14 C15 1.453(14) . ?
C15 Cs1 3.818(10) 14_456 ?
C15 C16 1.380(15) . ?
C16 H16 0.9500 . ?
C16 C17 1.408(17) . ?
C17 H17 0.9500 . ?
C17 C18 1.392(16) . ?
C18 C19 1.497(15) . ?
C19 C20 1.536(14) . ?
C19 C21 1.547(15) . ?
C19 C22 1.506(16) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 Cs1 3.863(10) 14_456 ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.381(14) . ?
C23 H23 0.9500 . ?
C23 C24 1.390(18) . ?
C24 H24 0.9500 . ?
C24 C25 1.381(15) . ?
C25 C26 1.426(16) . ?
C26 H26 0.9500 . ?
C27 C28 1.367(15) . ?
C27 C34 1.406(16) . ?
C28 H28 0.9500 . ?
C28 C29 1.397(18) . ?
C29 C30 1.493(18) . ?
C29 C31 1.39(2) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.521(18) . ?
C31 C33 1.387(17) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33 0.9500 . ?
C33 C34 1.367(16) . ?
C35 H35 0.9500 . ?
C35 C36 1.436(14) . ?
C36 C37 1.402(14) . ?
C37 H37 0.9500 . ?
C37 C38 1.391(15) . ?
C38 H38 0.9500 . ?
C38 C39 1.409(13) . ?
C39 C40 1.503(14) . ?
C40 C41 1.540(13) . ?
C40 C42 1.546(13) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
N10 C48 1.33(2) . ?
N10 C52 1.35(2) . ?
C48 H48 0.9500 . ?
C48 C49 1.41(2) . ?
C49 H49 0.9500 . ?
C49 C50 1.38(2) . ?
C50 H50 0.9500 . ?
C50 C51 1.34(2) . ?
C51 H51 0.9500 . ?
C51 C52 1.35(2) . ?
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
Cs1 U1 Cs1 106.064(17) . 14_456 ?
O1 U1 Cs1 141.7(2) . . ?
O1 U1 Cs1 51.1(2) . 14_456 ?
O1 U1 N1 91.2(3) . . ?
O1 U1 N2 94.2(3) . . ?
O1 U1 N7 104.9(3) . . ?
O1 U1 N8 97.1(3) . . ?
O1 U1 N9 94.0(3) . . ?
O2 U1 Cs1 124.9(2) . 14_456 ?
O2 U1 Cs1 39.4(2) . . ?
O2 U1 O1 175.1(3) . . ?
O2 U1 N1 87.0(3) . . ?
O2 U1 N2 81.0(3) . . ?
O2 U1 N7 79.6(3) . . ?
O2 U1 N8 86.5(3) . . ?
O2 U1 N9 84.8(3) . . ?
N1 U1 Cs1 49.36(18) . 14_456 ?
N1 U1 Cs1 57.20(18) . . ?
N1 U1 N2 64.5(3) . . ?
N1 U1 N7 131.8(3) . . ?
N1 U1 N8 69.3(2) . . ?
N1 U1 N9 142.9(3) . . ?
N2 U1 Cs1 52.81(18) . 14_456 ?
N2 U1 Cs1 90.74(18) . . ?
N7 U1 Cs1 85.59(18) . . ?
N7 U1 Cs1 152.86(18) . 14_456 ?
N7 U1 N2 153.4(3) . . ?
N8 U1 Cs1 54.09(17) . . ?
N8 U1 Cs1 102.77(17) . 14_456 ?
N8 U1 N2 132.5(3) . . ?
N8 U1 N7 63.9(3) . . ?
N9 U1 Cs1 109.4(3) . 14_456 ?
N9 U1 Cs1 124.2(2) . . ?
N9 U1 N2 78.5(3) . . ?
N9 U1 N7 81.9(3) . . ?
N9 U1 N8 145.7(3) . . ?
O1 Cs1 C1 146.1(2) 15_556 . ?
O1 Cs1 C4 73.7(2) 15_556 15_556 ?
O1 Cs1 C36 138.1(2) 15_556 . ?
O1 Cs1 C38 133.5(2) 15_556 . ?
O2 Cs1 O1 122.27(18) . 15_556 ?
O2 Cs1 N1 166.78(19) . 15_556 ?
O2 Cs1 N2 143.38(19) . 15_556 ?
O2 Cs1 N3 98.4(2) . 15_556 ?
O2 Cs1 N4 73.2(2) . 15_556 ?
O2 Cs1 N8 57.06(18) . . ?
O2 Cs1 C1 76.7(2) . . ?
O2 Cs1 C4 163.9(2) . 15_556 ?
O2 Cs1 C36 62.9(2) . . ?
O2 Cs1 C38 95.3(2) . . ?
O2 Cs1 C39 78.7(2) . . ?
N1 Cs1 O1 56.31(19) 15_556 15_556 ?
N1 Cs1 N2 49.2(2) 15_556 15_556 ?
N1 Cs1 N3 91.8(2) 15_556 15_556 ?
N1 Cs1 N4 108.3(2) 15_556 15_556 ?
N1 Cs1 N8 129.2(2) 15_556 . ?
N1 Cs1 C1 98.5(2) 15_556 . ?
N1 Cs1 C4 23.8(2) 15_556 15_556 ?
N1 Cs1 C36 128.1(2) 15_556 . ?
N1 Cs1 C38 93.1(2) 15_556 . ?
N1 Cs1 C39 106.0(2) 15_556 . ?
N2 Cs1 O1 58.97(18) 15_556 15_556 ?
N2 Cs1 C1 124.3(2) 15_556 . ?
N2 Cs1 C4 40.0(2) 15_556 15_556 ?
N2 Cs1 C36 92.1(2) 15_556 . ?
N2 Cs1 C38 74.5(2) 15_556 . ?
N3 Cs1 O1 60.7(2) 15_556 15_556 ?
N3 Cs1 N2 47.6(2) 15_556 15_556 ?
N3 Cs1 N4 48.3(2) 15_556 15_556 ?
N3 Cs1 C1 150.3(2) 15_556 . ?
N3 Cs1 C4 87.6(2) 15_556 15_556 ?
N3 Cs1 C36 77.5(2) 15_556 . ?
N3 Cs1 C38 89.8(2) 15_556 . ?
N4 Cs1 O1 52.3(2) 15_556 15_556 ?
N4 Cs1 N2 87.5(2) 15_556 15_556 ?
N4 Cs1 C1 147.7(2) 15_556 . ?
N4 Cs1 C4 120.9(2) 15_556 15_556 ?
N4 Cs1 C36 101.5(2) 15_556 . ?
N4 Cs1 C38 131.9(2) 15_556 . ?
N8 Cs1 O1 161.42(18) . 15_556 ?
N8 Cs1 N2 109.34(19) . 15_556 ?
N8 Cs1 N3 100.7(2) . 15_556 ?
N8 Cs1 N4 116.7(2) . 15_556 ?
N8 Cs1 C1 51.8(2) . . ?
N8 Cs1 C4 107.3(2) . 15_556 ?
N8 Cs1 C36 23.3(2) . . ?
N8 Cs1 C38 38.8(2) . . ?
C1 Cs1 C4 90.7(2) . 15_556 ?
C1 Cs1 C36 74.3(2) . . ?
C1 Cs1 C38 62.0(2) . . ?
C4 Cs1 C36 104.4(2) 15_556 . ?
C4 Cs1 C38 69.7(2) 15_556 . ?
C36 Cs1 C38 37.4(2) . . ?
C39 Cs1 O1 156.3(2) . 15_556 ?
C39 Cs1 N2 97.8(2) . 15_556 ?
C39 Cs1 N3 108.7(2) . 15_556 ?
C39 Cs1 N4 138.5(2) . 15_556 ?
C39 Cs1 N8 23.5(2) . . ?
C39 Cs1 C1 41.7(2) . . ?
C39 Cs1 C4 85.3(2) . 15_556 ?
C39 Cs1 C36 37.5(2) . . ?
C39 Cs1 C38 23.6(2) . . ?
U1 O1 Cs1 104.0(3) . 14_456 ?
U1 O2 Cs1 117.6(3) . . ?
U1 N1 Cs1 94.7(2) . 14_456 ?
U1 N1 Cs1 85.5(2) . . ?
Cs1 N1 Cs1 170.7(3) 14_456 . ?
C1 N1 U1 136.1(6) . . ?
C1 N1 Cs1 108.8(6) . 14_456 ?
C1 N1 Cs1 76.9(5) . . ?
C1 N1 C4 106.0(9) . . ?
C4 N1 U1 112.3(6) . . ?
C4 N1 Cs1 86.2(5) . 14_456 ?
C4 N1 Cs1 85.1(5) . . ?
U1 N2 Cs1 88.4(2) . 14_456 ?
C5 N2 U1 110.3(6) . . ?
C5 N2 Cs1 84.3(6) . 14_456 ?
C5 N2 C6 117.3(9) . . ?
C6 N2 U1 127.7(7) . . ?
C6 N2 Cs1 115.8(6) . 14_456 ?
C13 N3 Cs1 117.6(7) . 14_456 ?
C14 N3 Cs1 100.9(7) . 14_456 ?
C14 N3 C13 120.7(10) . . ?
C15 N4 Cs1 97.3(6) . 14_456 ?
C15 N4 C18 108.8(9) . . ?
C18 N4 Cs1 116.4(6) . 14_456 ?
C22 N5 H5 124.7 . . ?
C25 N5 H5 124.7 . . ?
C25 N5 C22 110.5(8) . . ?
C26 N6 H6 120.9 . . ?
C26 N6 C27 118.3(9) . . ?
C27 N6 H6 120.9 . . ?
C34 N7 U1 125.7(7) . . ?
C35 N7 U1 114.2(6) . . ?
C35 N7 C34 117.7(9) . . ?
U1 N8 Cs1 88.0(2) . . ?
C36 N8 U1 114.6(6) . . ?
C36 N8 Cs1 82.6(5) . . ?
C39 N8 U1 135.0(6) . . ?
C39 N8 Cs1 78.0(5) . . ?
C39 N8 C36 105.8(8) . . ?
C43 N9 U1 116.2(6) . . ?
C43 N9 C47 120.0 . . ?
C47 N9 U1 123.8(6) . . ?
N9 C43 H43 120.0 . . ?
N9 C43 C44 120.0 . . ?
C44 C43 H43 120.0 . . ?
C43 C44 H44 120.0 . . ?
C43 C44 C45 120.0 . . ?
C45 C44 H44 120.0 . . ?
C44 C45 H45 120.0 . . ?
C46 C45 C44 120.0 . . ?
C46 C45 H45 120.0 . . ?
C45 C46 H46 120.0 . . ?
C45 C46 C47 120.0 . . ?
C47 C46 H46 120.0 . . ?
N9 C47 H47 120.0 . . ?
C46 C47 N9 120.0 . . ?
C46 C47 H47 120.0 . . ?
N1 C1 Cs1 80.5(5) . . ?
N1 C1 C2 110.6(9) . . ?
N1 C1 C40 119.1(9) . . ?
C2 C1 Cs1 83.9(6) . . ?
C2 C1 C40 130.2(9) . . ?
C40 C1 Cs1 100.5(6) . . ?
Cs1 C2 H2 107.7 . . ?
C1 C2 Cs1 73.5(6) . . ?
C1 C2 H2 126.2 . . ?
C1 C2 C3 107.7(9) . . ?
C3 C2 Cs1 85.7(6) . . ?
C3 C2 H2 126.2 . . ?
Cs1 C3 H3 117.3 . . ?
C2 C3 Cs1 72.6(6) . . ?
C2 C3 H3 126.9 . . ?
C2 C3 C4 106.2(9) . . ?
C4 C3 Cs1 75.5(6) . . ?
C4 C3 H3 126.9 . . ?
Cs1 C4 Cs1 142.3(3) 14_456 . ?
N1 C4 Cs1 72.5(5) . . ?
N1 C4 Cs1 70.0(5) . 14_456 ?
N1 C4 C3 109.5(9) . . ?
N1 C4 C5 120.0(9) . . ?
C3 C4 Cs1 112.9(6) . 14_456 ?
C3 C4 Cs1 82.7(6) . . ?
C5 C4 Cs1 116.0(6) . . ?
C5 C4 Cs1 81.0(6) . 14_456 ?
C5 C4 C3 130.1(10) . . ?
Cs1 C5 H5A 121.7 14_456 . ?
N2 C5 Cs1 74.4(6) . 14_456 ?
N2 C5 C4 121.7(9) . . ?
N2 C5 H5A 119.2 . . ?
C4 C5 Cs1 75.9(6) . 14_456 ?
C4 C5 H5A 119.2 . . ?
C7 C6 N2 120.7(10) . . ?
C13 C6 N2 120.9(9) . . ?
C13 C6 C7 118.4(10) . . ?
C6 C7 H7 119.2 . . ?
C8 C7 C6 121.5(11) . . ?
C8 C7 H7 119.2 . . ?
C7 C8 C9 119.5(12) . . ?
C7 C8 C10 119.5(11) . . ?
C10 C8 C9 121.0(12) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 C11 120.7(12) . . ?
C12 C10 C8 119.2(12) . . ?
C12 C10 C11 120.0(13) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12 118.7 . . ?
C10 C12 C13 122.6(12) . . ?
C13 C12 H12 118.7 . . ?
C6 C13 N3 116.2(9) . . ?
C6 C13 C12 118.7(10) . . ?
C12 C13 N3 125.1(10) . . ?
Cs1 C14 H14 134.3 14_456 . ?
N3 C14 Cs1 60.2(6) . 14_456 ?
N3 C14 H14 120.2 . . ?
N3 C14 C15 119.6(10) . . ?
C15 C14 Cs1 78.1(6) . 14_456 ?
C15 C14 H14 120.2 . . ?
N4 C15 Cs1 61.9(5) . 14_456 ?
N4 C15 C14 120.7(9) . . ?
N4 C15 C16 108.8(9) . . ?
C14 C15 Cs1 80.0(6) . 14_456 ?
C16 C15 Cs1 127.1(8) . 14_456 ?
C16 C15 C14 130.5(11) . . ?
C15 C16 H16 126.3 . . ?
C15 C16 C17 107.3(11) . . ?
C17 C16 H16 126.3 . . ?
C16 C17 H17 126.4 . . ?
C18 C17 C16 107.2(10) . . ?
C18 C17 H17 126.4 . . ?
N4 C18 C17 107.8(10) . . ?
N4 C18 C19 121.9(9) . . ?
C17 C18 C19 130.3(9) . . ?
C18 C19 C20 109.0(10) . . ?
C18 C19 C21 110.8(8) . . ?
C18 C19 C22 109.2(9) . . ?
C20 C19 C21 108.2(9) . . ?
C22 C19 C20 109.2(9) . . ?
C22 C19 C21 110.3(10) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Cs1 C21 H21A 53.1 14_456 . ?
Cs1 C21 H21B 137.4 14_456 . ?
Cs1 C21 H21C 58.2 14_456 . ?
C19 C21 Cs1 113.1(6) . 14_456 ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N5 C22 C19 122.2(8) . . ?
N5 C22 C23 105.9(10) . . ?
C23 C22 C19 131.9(10) . . ?
C22 C23 H23 125.5 . . ?
C22 C23 C24 109.1(10) . . ?
C24 C23 H23 125.5 . . ?
C23 C24 H24 126.3 . . ?
C25 C24 C23 107.4(10) . . ?
C25 C24 H24 126.3 . . ?
N5 C25 C24 107.0(10) . . ?
N5 C25 C26 121.8(9) . . ?
C24 C25 C26 131.2(10) . . ?
N6 C26 C25 122.3(10) . . ?
N6 C26 H26 118.8 . . ?
C25 C26 H26 118.8 . . ?
C28 C27 N6 123.7(10) . . ?
C28 C27 C34 118.6(11) . . ?
C34 C27 N6 117.7(9) . . ?
C27 C28 H28 118.9 . . ?
C27 C28 C29 122.3(12) . . ?
C29 C28 H28 118.9 . . ?
C28 C29 C30 120.1(14) . . ?
C31 C29 C28 119.0(11) . . ?
C31 C29 C30 120.9(14) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 C32 120.9(13) . . ?
C33 C31 C29 118.2(12) . . ?
C33 C31 C32 120.9(13) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33 118.6 . . ?
C34 C33 C31 122.8(12) . . ?
C34 C33 H33 118.6 . . ?
C27 C34 N7 116.4(10) . . ?
C33 C34 N7 124.5(11) . . ?
C33 C34 C27 119.1(10) . . ?
N7 C35 H35 120.0 . . ?
N7 C35 C36 120.1(9) . . ?
C36 C35 H35 120.0 . . ?
N8 C36 Cs1 74.0(5) . . ?
N8 C36 C35 118.9(9) . . ?
N8 C36 C37 110.5(9) . . ?
C35 C36 Cs1 114.6(6) . . ?
C37 C36 Cs1 81.8(6) . . ?
C37 C36 C35 130.4(9) . . ?
Cs1 C37 H37 114.4 . . ?
C36 C37 Cs1 75.3(5) . . ?
C36 C37 H37 126.8 . . ?
C38 C37 Cs1 76.1(6) . . ?
C38 C37 C36 106.4(9) . . ?
C38 C37 H37 126.8 . . ?
Cs1 C38 H38 112.1 . . ?
C37 C38 Cs1 81.2(6) . . ?
C37 C38 H38 126.4 . . ?
C37 C38 C39 107.2(9) . . ?
C39 C38 Cs1 73.0(6) . . ?
C39 C38 H38 126.4 . . ?
N8 C39 Cs1 78.5(5) . . ?
N8 C39 C38 110.2(9) . . ?
N8 C39 C40 119.2(8) . . ?
C38 C39 Cs1 83.4(6) . . ?
C38 C39 C40 130.7(9) . . ?
C40 C39 Cs1 104.6(6) . . ?
C1 C40 C39 108.4(8) . . ?
C1 C40 C41 109.8(8) . . ?
C1 C40 C42 111.0(8) . . ?
C39 C40 C41 109.7(8) . . ?
C39 C40 C42 109.7(8) . . ?
C41 C40 C42 108.2(8) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C48 N10 C52 117.5(14) . . ?
N10 C48 H48 119.1 . . ?
N10 C48 C49 121.8(14) . . ?
C49 C48 H48 119.1 . . ?
C48 C49 H49 120.8 . . ?
C50 C49 C48 118.4(14) . . ?
C50 C49 H49 120.8 . . ?
C49 C50 H50 120.6 . . ?
C51 C50 C49 118.8(14) . . ?
C51 C50 H50 120.6 . . ?
C50 C51 H51 119.7 . . ?
C50 C51 C52 120.5(17) . . ?
C52 C51 H51 119.7 . . ?
N10 C52 C51 122.7(17) . . ?
N10 C52 H52 118.7 . . ?
C51 C52 H52 118.7 . . ?

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 N1 C1 Cs1 69.1(8) . . . . ?
U1 N1 C1 C2 148.8(7) . . . . ?
U1 N1 C1 C40 -27.7(14) . . . . ?
U1 N1 C4 Cs1 -83.1(4) . . . . ?
U1 N1 C4 Cs1 93.5(4) . . . 14_456 ?
U1 N1 C4 C3 -158.4(6) . . . . ?
U1 N1 C4 C5 27.3(11) . . . . ?
U1 N2 C5 Cs1 -86.2(4) . . . 14_456 ?
U1 N2 C5 C4 -24.2(12) . . . . ?
U1 N2 C6 C7 -107.7(11) . . . . ?
U1 N2 C6 C13 73.2(13) . . . . ?
U1 N7 C34 C27 -62.0(11) . . . . ?
U1 N7 C34 C33 117.5(11) . . . . ?
U1 N7 C35 C36 19.4(11) . . . . ?
U1 N8 C36 Cs1 84.4(4) . . . . ?
U1 N8 C36 C35 -25.2(11) . . . . ?
U1 N8 C36 C37 158.9(6) . . . . ?
U1 N8 C39 Cs1 -74.8(7) . . . . ?
U1 N8 C39 C38 -153.2(7) . . . . ?
U1 N8 C39 C40 25.6(13) . . . . ?
U1 N9 C43 C44 179.8(8) . . . . ?
U1 N9 C47 C46 -179.8(9) . . . . ?
Cs1 U1 O1 Cs1 63.4(4) . . . 14_456 ?
Cs1 U1 O2 Cs1 71.4(3) 14_456 . . . ?
Cs1 N1 C1 Cs1 -172.4(3) 14_456 . . . ?
Cs1 N1 C1 C2 79.7(7) . . . . ?
Cs1 N1 C1 C2 -92.7(8) 14_456 . . . ?
Cs1 N1 C1 C40 -96.8(8) . . . . ?
Cs1 N1 C1 C40 90.8(8) 14_456 . . . ?
Cs1 N1 C4 Cs1 176.6(2) . . . 14_456 ?
Cs1 N1 C4 Cs1 -176.6(2) 14_456 . . . ?
Cs1 N1 C4 C3 -75.3(7) . . . . ?
Cs1 N1 C4 C3 108.1(7) 14_456 . . . ?
Cs1 N1 C4 C5 110.4(9) . . . . ?
Cs1 N1 C4 C5 -66.2(9) 14_456 . . . ?
Cs1 N2 C5 C4 62.0(9) 14_456 . . . ?
Cs1 N2 C6 C7 142.7(9) 14_456 . . . ?
Cs1 N2 C6 C13 -36.4(13) 14_456 . . . ?
Cs1 N3 C13 C6 39.4(13) 14_456 . . . ?
Cs1 N3 C13 C12 -139.6(13) 14_456 . . . ?
Cs1 N3 C14 C15 -53.3(11) 14_456 . . . ?
Cs1 N4 C15 C14 56.9(10) 14_456 . . . ?
Cs1 N4 C15 C16 -122.7(8) 14_456 . . . ?
Cs1 N4 C18 C17 109.3(8) 14_456 . . . ?
Cs1 N4 C18 C19 -71.8(11) 14_456 . . . ?
Cs1 N8 C36 C35 -109.6(8) . . . . ?
Cs1 N8 C36 C37 74.5(7) . . . . ?
Cs1 N8 C39 C38 -78.5(7) . . . . ?
Cs1 N8 C39 C40 100.4(8) . . . . ?
Cs1 C1 C2 C3 79.9(7) . . . . ?
Cs1 C1 C40 C39 -20.8(8) . . . . ?
Cs1 C1 C40 C41 99.0(7) . . . . ?
Cs1 C1 C40 C42 -141.4(6) . . . . ?
Cs1 C2 C3 C4 68.6(7) . . . . ?
Cs1 C3 C4 Cs1 144.3(5) . . . 14_456 ?
Cs1 C3 C4 N1 68.4(7) . . . . ?
Cs1 C3 C4 C5 -118.0(11) . . . . ?
Cs1 C4 C5 Cs1 144.5(5) . . . 14_456 ?
Cs1 C4 C5 N2 83.2(10) . . . . ?
Cs1 C4 C5 N2 -61.3(9) 14_456 . . . ?
Cs1 C14 C15 N4 -48.7(9) 14_456 . . . ?
Cs1 C14 C15 C16 130.9(13) 14_456 . . . ?
Cs1 C15 C16 C17 -66.8(12) 14_456 . . . ?
Cs1 C36 C37 C38 70.4(7) . . . . ?
Cs1 C37 C38 C39 69.0(7) . . . . ?
Cs1 C38 C39 N8 75.1(7) . . . . ?
Cs1 C38 C39 C40 -103.6(10) . . . . ?
Cs1 C39 C40 C1 21.8(8) . . . . ?
Cs1 C39 C40 C41 -98.0(7) . . . . ?
Cs1 C39 C40 C42 143.2(6) . . . . ?
N1 U1 O1 Cs1 31.4(3) . . . 14_456 ?
N1 U1 O2 Cs1 37.7(3) . . . . ?
N1 C1 C2 Cs1 -77.4(7) . . . . ?
N1 C1 C2 C3 2.4(12) . . . . ?
N1 C1 C40 C39 64.1(11) . . . . ?
N1 C1 C40 C41 -176.1(9) . . . . ?
N1 C1 C40 C42 -56.5(12) . . . . ?
N1 C4 C5 Cs1 60.5(8) . . . 14_456 ?
N1 C4 C5 N2 -0.8(15) . . . . ?
N2 U1 O1 Cs1 -33.1(3) . . . 14_456 ?
N2 U1 O2 Cs1 102.4(3) . . . . ?
N2 C6 C7 C8 -178.8(11) . . . . ?
N2 C6 C13 N3 -1.3(17) . . . . ?
N2 C6 C13 C12 177.8(12) . . . . ?
N3 C14 C15 Cs1 45.3(10) . . . 14_456 ?
N3 C14 C15 N4 -3.4(17) . . . . ?
N3 C14 C15 C16 176.2(12) . . . . ?
N4 C15 C16 C17 1.8(13) . . . . ?
N4 C18 C19 C20 169.2(10) . . . . ?
N4 C18 C19 C21 50.2(13) . . . . ?
N4 C18 C19 C22 -71.5(12) . . . . ?
N5 C22 C23 C24 0.8(13) . . . . ?
N5 C25 C26 N6 -3.2(16) . . . . ?
N6 C27 C28 C29 -178.5(12) . . . . ?
N6 C27 C34 N7 -2.2(14) . . . . ?
N6 C27 C34 C33 178.3(10) . . . . ?
N7 U1 O1 Cs1 165.5(2) . . . 14_456 ?
N7 U1 O2 Cs1 -95.8(3) . . . . ?
N7 C35 C36 Cs1 -81.3(10) . . . . ?
N7 C35 C36 N8 3.3(14) . . . . ?
N7 C35 C36 C37 178.2(10) . . . . ?
N8 U1 O1 Cs1 100.7(2) . . . 14_456 ?
N8 U1 O2 Cs1 -31.7(3) . . . . ?
N8 C36 C37 Cs1 -69.4(7) . . . . ?
N8 C36 C37 C38 0.9(11) . . . . ?
N8 C39 C40 C1 -62.9(11) . . . . ?
N8 C39 C40 C41 177.2(9) . . . . ?
N8 C39 C40 C42 58.4(11) . . . . ?
N9 U1 O1 Cs1 -111.8(3) . . . 14_456 ?
N9 U1 O2 Cs1 -178.5(4) . . . . ?
N9 C43 C44 C45 0.0 . . . . ?
C43 N9 C47 C46 0.0 . . . . ?
C43 C44 C45 C46 0.0 . . . . ?
C44 C45 C46 C47 0.0 . . . . ?
C45 C46 C47 N9 0.0 . . . . ?
C47 N9 C43 C44 0.0 . . . . ?
C1 N1 C4 Cs1 -108.5(6) . . . 14_456 ?
C1 N1 C4 Cs1 74.9(6) . . . . ?
C1 N1 C4 C3 -0.4(11) . . . . ?
C1 N1 C4 C5 -174.7(9) . . . . ?
C1 C2 C3 Cs1 -71.2(7) . . . . ?
C1 C2 C3 C4 -2.6(11) . . . . ?
C2 C1 C40 C39 -111.6(12) . . . . ?
C2 C1 C40 C41 8.2(14) . . . . ?
C2 C1 C40 C42 127.8(11) . . . . ?
C2 C3 C4 Cs1 -66.6(7) . . . . ?
C2 C3 C4 Cs1 77.7(9) . . . 14_456 ?
C2 C3 C4 N1 1.9(11) . . . . ?
C2 C3 C4 C5 175.4(10) . . . . ?
C3 C4 C5 Cs1 -112.4(11) . . . 14_456 ?
C3 C4 C5 N2 -173.7(10) . . . . ?
C4 N1 C1 Cs1 -81.0(6) . . . . ?
C4 N1 C1 C2 -1.3(11) . . . . ?
C4 N1 C1 C40 -177.7(8) . . . . ?
C5 N2 C6 C7 45.6(15) . . . . ?
C5 N2 C6 C13 -133.6(12) . . . . ?
C6 N2 C5 Cs1 116.1(8) . . . 14_456 ?
C6 N2 C5 C4 178.1(9) . . . . ?
C6 C7 C8 C9 -177.7(12) . . . . ?
C6 C7 C8 C10 2(2) . . . . ?
C7 C6 C13 N3 179.5(11) . . . . ?
C7 C6 C13 C12 -1.4(19) . . . . ?
C7 C8 C10 C11 178.6(17) . . . . ?
C7 C8 C10 C12 -3(2) . . . . ?
C8 C10 C12 C13 2(3) . . . . ?
C9 C8 C10 C11 -2(3) . . . . ?
C9 C8 C10 C12 176.6(15) . . . . ?
C10 C12 C13 N3 179.4(15) . . . . ?
C10 C12 C13 C6 0(2) . . . . ?
C11 C10 C12 C13 -179.6(18) . . . . ?
C13 N3 C14 Cs1 -131.5(12) . . . 14_456 ?
C13 N3 C14 C15 175.2(11) . . . . ?
C13 C6 C7 C8 0.4(18) . . . . ?
C14 N3 C13 C6 163.4(11) . . . . ?
C14 N3 C13 C12 -16(2) . . . . ?
C14 C15 C16 C17 -177.8(11) . . . . ?
C15 N4 C18 C17 0.8(12) . . . . ?
C15 N4 C18 C19 179.7(9) . . . . ?
C15 C16 C17 C18 -1.3(13) . . . . ?
C16 C17 C18 N4 0.3(13) . . . . ?
C16 C17 C18 C19 -178.5(11) . . . . ?
C17 C18 C19 C20 -12.2(16) . . . . ?
C17 C18 C19 C21 -131.2(12) . . . . ?
C17 C18 C19 C22 107.2(13) . . . . ?
C18 N4 C15 Cs1 121.1(8) . . . 14_456 ?
C18 N4 C15 C14 178.0(10) . . . . ?
C18 N4 C15 C16 -1.6(12) . . . . ?
C18 C19 C21 Cs1 -6.8(11) . . . 14_456 ?
C18 C19 C22 N5 65.7(13) . . . . ?
C18 C19 C22 C23 -110.9(13) . . . . ?
C19 C22 C23 C24 177.8(11) . . . . ?
C20 C19 C21 Cs1 -126.3(8) . . . 14_456 ?
C20 C19 C22 N5 -175.1(10) . . . . ?
C20 C19 C22 C23 8.3(17) . . . . ?
C21 C19 C22 N5 -56.3(13) . . . . ?
C21 C19 C22 C23 127.1(13) . . . . ?
C22 N5 C25 C24 -0.8(12) . . . . ?
C22 N5 C25 C26 178.2(10) . . . . ?
C22 C19 C21 Cs1 114.2(8) . . . 14_456 ?
C22 C23 C24 C25 -1.3(14) . . . . ?
C23 C24 C25 N5 1.3(13) . . . . ?
C23 C24 C25 C26 -177.6(11) . . . . ?
C24 C25 C26 N6 175.5(12) . . . . ?
C25 N5 C22 C19 -177.4(10) . . . . ?
C25 N5 C22 C23 0.0(12) . . . . ?
C26 N6 C27 C28 45.9(15) . . . . ?
C26 N6 C27 C34 -134.4(10) . . . . ?
C27 N6 C26 C25 -176.5(9) . . . . ?
C27 C28 C29 C30 -179.7(16) . . . . ?
C27 C28 C29 C31 0(2) . . . . ?
C28 C27 C34 N7 177.5(10) . . . . ?
C28 C27 C34 C33 -2.1(16) . . . . ?
C28 C29 C31 C32 -179.4(15) . . . . ?
C28 C29 C31 C33 -2(2) . . . . ?
C29 C31 C33 C34 2(2) . . . . ?
C30 C29 C31 C32 0(3) . . . . ?
C30 C29 C31 C33 177.9(17) . . . . ?
C31 C33 C34 N7 -179.2(12) . . . . ?
C31 C33 C34 C27 0.3(19) . . . . ?
C32 C31 C33 C34 179.3(14) . . . . ?
C34 N7 C35 C36 -177.4(9) . . . . ?
C34 C27 C28 C29 1.9(19) . . . . ?
C35 N7 C34 C27 136.9(10) . . . . ?
C35 N7 C34 C33 -43.6(15) . . . . ?
C35 C36 C37 Cs1 115.4(11) . . . . ?
C35 C36 C37 C38 -174.3(10) . . . . ?
C36 N8 C39 Cs1 78.7(6) . . . . ?
C36 N8 C39 C38 0.2(11) . . . . ?
C36 N8 C39 C40 179.1(8) . . . . ?
C36 C37 C38 Cs1 -69.8(7) . . . . ?
C36 C37 C38 C39 -0.8(11) . . . . ?
C37 C38 C39 Cs1 -74.8(7) . . . . ?
C37 C38 C39 N8 0.4(11) . . . . ?
C37 C38 C39 C40 -178.3(10) . . . . ?
C38 C39 C40 C1 115.7(11) . . . . ?
C38 C39 C40 C41 -4.2(15) . . . . ?
C38 C39 C40 C42 -123.0(11) . . . . ?
C39 N8 C36 Cs1 -75.2(6) . . . . ?
C39 N8 C36 C35 175.1(8) . . . . ?
C39 N8 C36 C37 -0.7(11) . . . . ?
C40 C1 C2 Cs1 98.6(10) . . . . ?
C40 C1 C2 C3 178.4(10) . . . . ?
N10 C48 C49 C50 1(2) . . . . ?
C48 N10 C52 C51 -5(3) . . . . ?
C48 C49 C50 C51 -1(2) . . . . ?
C49 C50 C51 C52 -2(2) . . . . ?
C50 C51 C52 N10 5(3) . . . . ?
C52 N10 C48 C49 2(2) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_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 1 -5 0.0251 2.0011 0.9998 -5.0005 0.0044 0.0668 0.2658
5 -1 5 0.0187 5.0008 -1.0020 4.9996 -0.0206 -0.3553 0.0773
-2 -1 5 0.0187 -2.0011 -0.9998 5.0005 -0.0044 -0.0668 -0.2658
4 -5 -5 0.0147 4.0014 -4.9985 -4.9998 0.3246 0.0256 0.1627
-4 5 5 0.0147 -4.0014 4.9985 4.9998 -0.3246 -0.0256 -0.1627
2 5 -3 0.0269 2.0009 4.9979 -3.0011 -0.2375 -0.0231 0.3462
-2 -5 3 0.0118 -2.0009 -4.9979 3.0011 0.2375 0.0231 -0.3462
-5 2 -4 0.0203 -5.0009 2.0014 -3.9997 -0.0461 0.3172 -0.0707
-5 5 2 0.0125 -5.0014 4.9993 1.9999 -0.2844 0.1092 -0.1312

_olex2_submission_special_instructions 'No special instructions were received'
_vrf_DIFMX01_po15003_refinalized 
;
PROBLEM: The maximum difference density is 
0.1*ZMAX*1.00
 _refine_diff_density_max given = 12.923
Test value = 9.200
RESPONSE: This maximum electron density peak is 
located at U1 
with a distance of 1.091 Ang and is an 
artefact of the heavy atom.
;
_vrf_PLAT601_po15003_refinalized 
;
PROBLEM: Structure Contains Solvent Accessible VOID(S) of 653 Ang3
RESPONSE: This is an immanent feature of the structure.
;
