# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1437894'
_audit_update_record             
;
2015-11-19 deposited with the CCDC.
2016-01-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C53 H42 N8 Ni O21 S3 U2'
_chemical_formula_weight         1757.89

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   13.8935(5)
_cell_length_b                   14.0662(8)
_cell_length_c                   18.2195(11)
_cell_angle_alpha                108.577(2)
_cell_angle_beta                 110.263(3)
_cell_angle_gamma                97.592(3)
_cell_volume                     3046.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    171362
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_F_000             1688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    5.793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.388
_exptl_absorpt_correction_T_max  0.629
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 30 mm'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'2 φ and 13 ω scans with 2° steps (750 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            171362
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.212
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11564
_reflns_number_gt                9122
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters, with restraints on bond lengths, angles and
 displacement parameters for the badly resolved NMP solvent molecule.
 The water solvent molecule is disordered over three positions close to
 one another, which have been given occupancy parameters of 0.33.
 The H atom bound to O15 was found on a difference Fourier map, but
 not those of the water molecules, and all the others were introduced
 at calculated positions; all were treated as riding atoms with an isotropic
 displacement parameter equal to 1.2 times that of the parent atom
 (1.5 for CH₃, with optimized geometry). 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0403P)²+2.8650P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11564
_refine_ls_number_parameters     812
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0934
_refine_ls_wR_factor_gt          0.0881
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.002
_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
U1 U 0.22104(2) 0.55626(2) 0.87835(2) 0.03614(8) Uani 1 1 d . . . . .
U2 U 0.78269(2) 0.75827(2) 0.63696(2) 0.03285(7) Uani 1 1 d . . . . .
Ni1 Ni 0.38940(5) 0.96618(5) 0.70344(5) 0.02920(16) Uani 1 1 d . . . . .
S1 S 0.49351(11) 0.66012(10) 0.74858(9) 0.0347(3) Uani 1 1 d . . . . .
S2 S 0.00119(12) 0.16101(11) 0.75893(10) 0.0395(4) Uani 1 1 d . . . . .
S3 S 1.02042(12) 0.71014(12) 0.46463(11) 0.0401(4) Uani 1 1 d . . . . .
O1 O 0.1229(3) 0.6022(3) 0.8199(3) 0.0442(10) Uani 1 1 d . . . . .
O2 O 0.3227(4) 0.5174(3) 0.9425(3) 0.0457(11) Uani 1 1 d . . . . .
O3 O 0.6934(3) 0.7738(3) 0.5479(3) 0.0404(10) Uani 1 1 d . . . . .
O4 O 0.8730(3) 0.7425(3) 0.7253(3) 0.0390(9) Uani 1 1 d . . . . .
O5 O 0.3529(3) 0.6386(3) 0.8400(3) 0.0408(10) Uani 1 1 d . . . . .
O6 O 0.2638(3) 0.4751(3) 0.7578(3) 0.0406(10) Uani 1 1 d . . . . .
O7 O 0.6447(3) 0.5985(3) 0.6005(3) 0.0378(9) Uani 1 1 d . . . . .
O8 O 0.6470(3) 0.7452(3) 0.6936(3) 0.0425(10) Uani 1 1 d . . . . .
O9 O 0.1226(3) 0.3743(3) 0.7977(3) 0.0469(11) Uani 1 1 d . . . . .
O10 O 0.0858(4) 0.4575(3) 0.9047(3) 0.0546(13) Uani 1 1 d . . . . .
O11 O -0.2151(3) -0.0702(3) 0.7359(3) 0.0444(10) Uani 1 1 d . . . . .
O12 O -0.0990(3) -0.0686(3) 0.6791(3) 0.0395(10) Uani 1 1 d . . . . .
O13 O 0.9153(3) 0.7584(3) 0.5774(3) 0.0404(10) Uani 1 1 d . . . . .
O14 O 0.8097(3) 0.6033(3) 0.5373(3) 0.0360(9) Uani 1 1 d . . . . .
O15 O 1.1297(4) 0.5614(3) 0.3052(3) 0.0555(13) Uani 1 1 d . . . . .
H15 H 1.1798 0.5802 0.2828 0.067 Uiso 1 1 d R U . . .
O16 O 1.1648(3) 0.7325(3) 0.3790(3) 0.0459(11) Uani 1 1 d . . . . .
O17 O 0.2058(4) 0.6588(4) 1.0138(3) 0.0570(13) Uani 1 1 d . . . . .
O18 O 0.3173(3) 0.7398(3) 0.9811(3) 0.0399(10) Uani 1 1 d . . . . .
O19 O 0.3079(4) 0.8143(4) 1.1023(3) 0.0698(16) Uani 1 1 d . . . . .
O20 O 1.2777(5) 0.5955(4) 0.2529(4) 0.0801(19) Uani 1 1 d . . . . .
O21 O 0.9906(12) 0.1365(12) 0.0395(13) 0.084(6) Uani 0.3333 1 d . . P . .
O22 O 0.9734(9) 0.0297(12) 0.0229(8) 0.052(4) Uani 0.3333 1 d . . P . .
O23 O 0.9232(8) -0.0346(12) 0.0535(7) 0.044(3) Uani 0.3333 1 d . U P . .
N1 N 0.2778(4) 0.7411(4) 1.0354(4) 0.0486(14) Uani 1 1 d . . . . .
N2 N 0.2908(4) 0.9031(4) 0.7489(3) 0.0344(11) Uani 1 1 d . . . . .
N3 N 0.4979(3) 0.9347(3) 0.7986(3) 0.0313(10) Uani 1 1 d . . . . .
N4 N 0.3796(4) 0.8284(3) 0.6119(3) 0.0332(11) Uani 1 1 d . . . . .
N5 N 0.4992(4) 1.0179(4) 0.6624(3) 0.0331(11) Uani 1 1 d . . . . .
N6 N 0.2724(4) 1.0074(4) 0.6213(3) 0.0356(11) Uani 1 1 d . . . . .
N7 N 0.3940(4) 1.1136(4) 0.7849(3) 0.0352(11) Uani 1 1 d . . . . .
N8 N 1.3305(6) 0.4971(6) 0.1524(5) 0.1034(15) Uani 1 1 d D U . . .
C1 C 0.3332(4) 0.5567(5) 0.7764(4) 0.0353(13) Uani 1 1 d . . . . .
C2 C 0.3939(4) 0.5528(4) 0.7225(4) 0.0325(12) Uani 1 1 d . . . . .
C3 C 0.3833(4) 0.4709(4) 0.6528(4) 0.0348(13) Uani 1 1 d . . . . .
H3 H 0.3318 0.4056 0.6291 0.042 Uiso 1 1 calc R U . . .
C4 C 0.4570(4) 0.4940(4) 0.6199(4) 0.0328(13) Uani 1 1 d . . . . .
H4 H 0.4606 0.4460 0.5712 0.039 Uiso 1 1 calc R U . . .
C5 C 0.5228(4) 0.5926(4) 0.6655(4) 0.0305(12) Uani 1 1 d . . . . .
C6 C 0.6083(5) 0.6481(5) 0.6519(4) 0.0372(14) Uani 1 1 d . . . . .
C7 C 0.0724(5) 0.3748(5) 0.8447(4) 0.0433(16) Uani 1 1 d . . . . .
C8 C -0.0004(5) 0.2762(5) 0.8281(4) 0.0435(15) Uani 1 1 d . . . . .
C9 C -0.0728(5) 0.2632(5) 0.8604(5) 0.0502(18) Uani 1 1 d . . . . .
H9 H -0.0838 0.3188 0.9000 0.060 Uiso 1 1 calc R U . . .
C10 C -0.1303(5) 0.1576(5) 0.8288(5) 0.0501(17) Uani 1 1 d . . . . .
H10 H -0.1848 0.1341 0.8442 0.060 Uiso 1 1 calc R U . . .
C11 C -0.0981(5) 0.0927(4) 0.7729(4) 0.0383(14) Uani 1 1 d . . . . .
C12 C -0.1397(4) -0.0211(4) 0.7274(4) 0.0361(13) Uani 1 1 d . . . . .
C13 C 0.8819(4) 0.6616(5) 0.5322(4) 0.0365(13) Uani 1 1 d . . . . .
C14 C 0.9312(4) 0.6208(4) 0.4723(4) 0.0346(13) Uani 1 1 d . . . . .
C15 C 0.9193(5) 0.5212(5) 0.4219(4) 0.0409(14) Uani 1 1 d . . . . .
H15A H 0.8726 0.4618 0.4174 0.049 Uiso 1 1 calc R U . . .
C16 C 0.9861(5) 0.5162(5) 0.3759(4) 0.0400(14) Uani 1 1 d . . . . .
H16 H 0.9896 0.4532 0.3384 0.048 Uiso 1 1 calc R U . . .
C17 C 1.0431(5) 0.6125(5) 0.3928(4) 0.0366(13) Uani 1 1 d . . . . .
C18 C 1.1189(5) 0.6429(5) 0.3585(4) 0.0407(14) Uani 1 1 d . . . . .
C19 C 0.1841(5) 0.8880(5) 0.7191(4) 0.0440(15) Uani 1 1 d . . . . .
H19 H 0.1482 0.8976 0.6682 0.053 Uiso 1 1 calc R U . . .
C20 C 0.1257(5) 0.8594(6) 0.7596(5) 0.060(2) Uani 1 1 d . . . . .
H20 H 0.0506 0.8489 0.7373 0.072 Uiso 1 1 calc R U . . .
C21 C 0.1789(6) 0.8464(7) 0.8333(6) 0.076(3) Uani 1 1 d . . . . .
H21 H 0.1399 0.8250 0.8617 0.092 Uiso 1 1 calc R U . . .
C22 C 0.2879(6) 0.8642(6) 0.8666(5) 0.0565(19) Uani 1 1 d . . . . .
H22 H 0.3254 0.8585 0.9189 0.068 Uiso 1 1 calc R U . . .
C23 C 0.3417(5) 0.8907(4) 0.8210(4) 0.0345(13) Uani 1 1 d . . . . .
C24 C 0.4577(5) 0.9049(4) 0.8479(4) 0.0337(13) Uani 1 1 d . . . . .
C25 C 0.5224(5) 0.8880(5) 0.9182(4) 0.0441(15) Uani 1 1 d . . . . .
H25 H 0.4930 0.8688 0.9530 0.053 Uiso 1 1 calc R U . . .
C26 C 0.6297(5) 0.8996(5) 0.9363(4) 0.0477(16) Uani 1 1 d . . . . .
H26 H 0.6754 0.8896 0.9843 0.057 Uiso 1 1 calc R U . . .
C27 C 0.6682(5) 0.9254(5) 0.8841(4) 0.0467(16) Uani 1 1 d . . . . .
H27 H 0.7410 0.9315 0.8942 0.056 Uiso 1 1 calc R U . . .
C28 C 0.6015(4) 0.9430(4) 0.8164(4) 0.0376(14) Uani 1 1 d . . . . .
H28 H 0.6302 0.9616 0.7809 0.045 Uiso 1 1 calc R U . . .
C29 C 0.3171(5) 0.7341(4) 0.5889(4) 0.0390(14) Uani 1 1 d . . . . .
H29 H 0.2724 0.7275 0.6174 0.047 Uiso 1 1 calc R U . . .
C30 C 0.3138(5) 0.6452(5) 0.5257(4) 0.0405(14) Uani 1 1 d . . . . .
H30 H 0.2687 0.5793 0.5118 0.049 Uiso 1 1 calc R U . . .
C31 C 0.3766(5) 0.6546(5) 0.4843(4) 0.0466(16) Uani 1 1 d . . . . .
H31 H 0.3747 0.5952 0.4399 0.056 Uiso 1 1 calc R U . . .
C32 C 0.4438(5) 0.7511(5) 0.5067(4) 0.0404(14) Uani 1 1 d . . . . .
H32 H 0.4884 0.7582 0.4782 0.048 Uiso 1 1 calc R U . . .
C33 C 0.4447(4) 0.8375(4) 0.5718(4) 0.0326(12) Uani 1 1 d . . . . .
C34 C 0.5144(4) 0.9434(4) 0.6020(4) 0.0313(12) Uani 1 1 d . . . . .
C35 C 0.5909(5) 0.9681(5) 0.5737(4) 0.0410(15) Uani 1 1 d . . . . .
H35 H 0.6016 0.9151 0.5320 0.049 Uiso 1 1 calc R U . . .
C36 C 0.6519(5) 1.0701(5) 0.6062(4) 0.0433(15) Uani 1 1 d . . . . .
H36 H 0.7051 1.0875 0.5874 0.052 Uiso 1 1 calc R U . . .
C37 C 0.6346(5) 1.1453(5) 0.6655(4) 0.0448(16) Uani 1 1 d . . . . .
H37 H 0.6742 1.2161 0.6875 0.054 Uiso 1 1 calc R U . . .
C38 C 0.5584(5) 1.1168(5) 0.6929(4) 0.0413(14) Uani 1 1 d . . . . .
H38 H 0.5474 1.1692 0.7349 0.050 Uiso 1 1 calc R U . . .
C39 C 0.2151(5) 0.9511(5) 0.5394(4) 0.0393(14) Uani 1 1 d . . . . .
H39 H 0.2223 0.8830 0.5160 0.047 Uiso 1 1 calc R U . . .
C40 C 0.1448(5) 0.9867(5) 0.4856(4) 0.0450(15) Uani 1 1 d . . . . .
H40 H 0.1057 0.9443 0.4268 0.054 Uiso 1 1 calc R U . . .
C41 C 0.1334(5) 1.0846(6) 0.5199(5) 0.0513(17) Uani 1 1 d . . . . .
H41 H 0.0878 1.1120 0.4847 0.062 Uiso 1 1 calc R U . . .
C42 C 0.1894(5) 1.1428(5) 0.6065(5) 0.0496(17) Uani 1 1 d . . . . .
H42 H 0.1794 1.2090 0.6318 0.060 Uiso 1 1 calc R U . . .
C43 C 0.2596(5) 1.1039(5) 0.6558(4) 0.0389(14) Uani 1 1 d . . . . .
C44 C 0.3233(5) 1.1596(5) 0.7480(4) 0.0379(14) Uani 1 1 d . . . . .
C45 C 0.3103(5) 1.2524(5) 0.7958(5) 0.0493(17) Uani 1 1 d . . . . .
H45 H 0.2603 1.2841 0.7693 0.059 Uiso 1 1 calc R U . . .
C46 C 0.3718(6) 1.2977(5) 0.8830(5) 0.0551(18) Uani 1 1 d . . . . .
H46 H 0.3635 1.3604 0.9169 0.066 Uiso 1 1 calc R U . . .
C47 C 0.4446(5) 1.2513(5) 0.9200(4) 0.0465(16) Uani 1 1 d . . . . .
H47 H 0.4882 1.2824 0.9793 0.056 Uiso 1 1 calc R U . . .
C48 C 0.4536(5) 1.1594(4) 0.8701(4) 0.0379(14) Uani 1 1 d . . . . .
H48 H 0.5032 1.1269 0.8961 0.045 Uiso 1 1 calc R U . . .
C49 C 1.2635(8) 0.5131(7) 0.1914(6) 0.1029(17) Uani 1 1 d D U . . .
C50 C 1.1731(8) 0.4121(7) 0.1490(7) 0.1104(18) Uani 1 1 d D U . . .
H50A H 1.1058 0.4220 0.1140 0.132 Uiso 1 1 calc R U . . .
H50B H 1.1618 0.3897 0.1924 0.132 Uiso 1 1 calc R U . . .
C51 C 1.2095(8) 0.3302(6) 0.0926(7) 0.1120(18) Uani 1 1 d D U . . .
H51A H 1.1499 0.2869 0.0368 0.134 Uiso 1 1 calc R U . . .
H51B H 1.2385 0.2844 0.1208 0.134 Uiso 1 1 calc R U . . .
C52 C 1.2978(8) 0.3986(7) 0.0825(6) 0.1028(17) Uani 1 1 d D U . . .
H52A H 1.3582 0.3675 0.0856 0.123 Uiso 1 1 calc R U . . .
H52B H 1.2691 0.4065 0.0275 0.123 Uiso 1 1 calc R U . . .
C53 C 1.4112(8) 0.5828(7) 0.1704(6) 0.0980(18) Uani 1 1 d D U . . .
H53A H 1.3794 0.6306 0.1469 0.147 Uiso 1 1 calc R U . . .
H53B H 1.4595 0.5589 0.1448 0.147 Uiso 1 1 calc R U . . .
H53C H 1.4511 0.6190 0.2321 0.147 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.754(4) . ?
U1 O2 1.769(4) . ?
U1 O9 2.422(4) . ?
U1 O6 2.443(4) . ?
U1 O5 2.456(4) . ?
U1 O10 2.459(4) . ?
U1 O18 2.496(4) . ?
U1 O17 2.528(4) . ?
U2 O4 1.765(4) . ?
U2 O3 1.767(4) . ?
U2 O13 2.441(3) . ?
U2 O8 2.456(3) . ?
U2 O12 2.470(4) 1_665 ?
U2 O7 2.490(4) . ?
U2 O11 2.499(4) 1_665 ?
U2 O14 2.521(4) . ?
Ni1 N4 2.067(5) . ?
Ni1 N5 2.064(4) . ?
Ni1 N2 2.070(5) . ?
Ni1 N3 2.080(5) . ?
Ni1 N6 2.082(5) . ?
Ni1 N7 2.108(5) . ?
S1 C2 1.719(5) . ?
S1 C5 1.724(5) . ?
S2 C11 1.715(6) . ?
S2 C8 1.716(6) . ?
S3 C14 1.720(6) . ?
S3 C17 1.719(6) . ?
O5 C1 1.261(7) . ?
O6 C1 1.263(7) . ?
O7 C6 1.274(6) . ?
O8 C6 1.263(7) . ?
O9 C7 1.277(7) . ?
O10 C7 1.255(7) . ?
O11 C12 1.261(7) . ?
O11 U2 2.499(4) 1_445 ?
O12 C12 1.269(7) . ?
O12 U2 2.470(4) 1_445 ?
O13 C13 1.265(7) . ?
O14 C13 1.258(7) . ?
O15 C18 1.311(7) . ?
O15 H15 0.9682 . ?
O16 C18 1.207(7) . ?
O17 N1 1.276(7) . ?
O18 N1 1.284(6) . ?
O19 N1 1.207(7) . ?
O20 C49 1.264(9) . ?
N2 C23 1.337(7) . ?
N2 C19 1.350(7) . ?
N3 C28 1.341(7) . ?
N3 C24 1.350(7) . ?
N4 C29 1.334(7) . ?
N4 C33 1.360(7) . ?
N5 C38 1.346(7) . ?
N5 C34 1.356(7) . ?
N6 C39 1.321(8) . ?
N6 C43 1.366(7) . ?
N7 C44 1.350(7) . ?
N7 C48 1.357(8) . ?
N8 C53 1.398(8) . ?
N8 C49 1.355(8) . ?
N8 C52 1.434(8) . ?
C1 C2 1.493(7) . ?
C2 C3 1.362(8) . ?
C3 C4 1.405(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.362(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.470(7) . ?
C7 C8 1.479(8) . ?
C8 C9 1.349(8) . ?
C9 C10 1.414(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.379(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.470(8) . ?
C13 C14 1.488(8) . ?
C14 C15 1.360(8) . ?
C15 C16 1.444(8) . ?
C15 H15A 0.9500 . ?
C16 C17 1.357(8) . ?
C16 H16 0.9500 . ?
C17 C18 1.478(8) . ?
C19 C20 1.372(8) . ?
C19 H19 0.9500 . ?
C20 C21 1.374(11) . ?
C20 H20 0.9500 . ?
C21 C22 1.375(10) . ?
C21 H21 0.9500 . ?
C22 C23 1.393(8) . ?
C22 H22 0.9500 . ?
C23 C24 1.478(8) . ?
C24 C25 1.399(8) . ?
C25 C26 1.386(9) . ?
C25 H25 0.9500 . ?
C26 C27 1.359(9) . ?
C26 H26 0.9500 . ?
C27 C28 1.380(9) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C30 1.387(8) . ?
C29 H29 0.9500 . ?
C30 C31 1.356(9) . ?
C30 H30 0.9500 . ?
C31 C32 1.388(9) . ?
C31 H31 0.9500 . ?
C32 C33 1.397(8) . ?
C32 H32 0.9500 . ?
C33 C34 1.479(8) . ?
C34 C35 1.382(7) . ?
C35 C36 1.385(9) . ?
C35 H35 0.9500 . ?
C36 C37 1.365(9) . ?
C36 H36 0.9500 . ?
C37 C38 1.383(8) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.396(8) . ?
C39 H39 0.9500 . ?
C40 C41 1.374(9) . ?
C40 H40 0.9500 . ?
C41 C42 1.388(10) . ?
C41 H41 0.9500 . ?
C42 C43 1.381(8) . ?
C42 H42 0.9500 . ?
C43 C44 1.473(9) . ?
C44 C45 1.393(8) . ?
C45 C46 1.389(10) . ?
C45 H45 0.9500 . ?
C46 C47 1.373(9) . ?
C46 H46 0.9500 . ?
C47 C48 1.373(8) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C49 C50 1.533(8) . ?
C50 C51 1.548(8) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.556(8) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 176.51(19) . . ?
O1 U1 O9 94.51(18) . . ?
O2 U1 O9 88.68(18) . . ?
O1 U1 O6 92.89(17) . . ?
O2 U1 O6 89.65(16) . . ?
O9 U1 O6 67.48(13) . . ?
O1 U1 O5 90.92(17) . . ?
O2 U1 O5 88.67(17) . . ?
O9 U1 O5 120.76(13) . . ?
O6 U1 O5 53.33(13) . . ?
O1 U1 O10 89.67(18) . . ?
O2 U1 O10 91.08(18) . . ?
O9 U1 O10 53.47(13) . . ?
O6 U1 O10 120.91(14) . . ?
O5 U1 O10 174.22(14) . . ?
O1 U1 O18 89.10(17) . . ?
O2 U1 O18 87.54(17) . . ?
O9 U1 O18 170.64(13) . . ?
O6 U1 O18 121.02(13) . . ?
O5 U1 O18 67.72(13) . . ?
O10 U1 O18 118.04(13) . . ?
O1 U1 O17 90.82(18) . . ?
O2 U1 O17 86.33(18) . . ?
O9 U1 O17 120.29(14) . . ?
O6 U1 O17 171.09(14) . . ?
O5 U1 O17 118.55(14) . . ?
O10 U1 O17 67.18(14) . . ?
O18 U1 O17 50.91(14) . . ?
O4 U2 O3 179.27(17) . . ?
O4 U2 O13 90.17(16) . . ?
O3 U2 O13 89.10(16) . . ?
O4 U2 O8 88.95(16) . . ?
O3 U2 O8 91.76(16) . . ?
O13 U2 O8 176.09(12) . . ?
O4 U2 O12 90.56(16) . 1_665 ?
O3 U2 O12 89.22(17) . 1_665 ?
O13 U2 O12 64.69(13) . 1_665 ?
O8 U2 O12 119.12(12) . 1_665 ?
O4 U2 O7 92.55(16) . . ?
O3 U2 O7 87.77(17) . . ?
O13 U2 O7 123.37(12) . . ?
O8 U2 O7 52.88(12) . . ?
O12 U2 O7 171.32(12) 1_665 . ?
O4 U2 O11 88.79(17) . 1_665 ?
O3 U2 O11 91.64(17) . 1_665 ?
O13 U2 O11 117.20(13) . 1_665 ?
O8 U2 O11 66.59(13) . 1_665 ?
O12 U2 O11 52.54(12) 1_665 1_665 ?
O7 U2 O11 119.40(12) . 1_665 ?
O4 U2 O14 90.34(16) . . ?
O3 U2 O14 89.14(16) . . ?
O13 U2 O14 52.63(12) . . ?
O8 U2 O14 123.57(12) . . ?
O12 U2 O14 117.32(12) 1_665 . ?
O7 U2 O14 70.79(11) . . ?
O11 U2 O14 169.80(12) 1_665 . ?
N4 Ni1 N5 79.09(18) . . ?
N4 Ni1 N2 97.49(18) . . ?
N5 Ni1 N2 173.07(17) . . ?
N4 Ni1 N3 90.98(17) . . ?
N5 Ni1 N3 95.42(17) . . ?
N2 Ni1 N3 78.53(18) . . ?
N4 Ni1 N6 95.84(18) . . ?
N5 Ni1 N6 90.64(18) . . ?
N2 Ni1 N6 95.73(18) . . ?
N3 Ni1 N6 171.63(17) . . ?
N4 Ni1 N7 172.99(18) . . ?
N5 Ni1 N7 97.23(18) . . ?
N2 Ni1 N7 86.78(18) . . ?
N3 Ni1 N7 95.32(18) . . ?
N6 Ni1 N7 78.15(19) . . ?
C2 S1 C5 90.7(3) . . ?
C11 S2 C8 91.1(3) . . ?
C14 S3 C17 91.2(3) . . ?
C1 O5 U1 92.5(3) . . ?
C1 O6 U1 93.0(3) . . ?
C6 O7 U2 92.4(3) . . ?
C6 O8 U2 94.2(3) . . ?
C7 O9 U1 93.6(4) . . ?
C7 O10 U1 92.5(3) . . ?
C12 O11 U2 92.7(3) . 1_445 ?
C12 O12 U2 93.9(3) . 1_445 ?
C13 O13 U2 94.6(3) . . ?
C13 O14 U2 91.0(3) . . ?
C18 O15 H15 112.5 . . ?
N1 O17 U1 96.2(3) . . ?
N1 O18 U1 97.5(3) . . ?
O19 N1 O17 122.6(5) . . ?
O19 N1 O18 122.3(5) . . ?
O17 N1 O18 115.1(5) . . ?
C23 N2 C19 119.0(5) . . ?
C23 N2 Ni1 114.8(4) . . ?
C19 N2 Ni1 125.6(4) . . ?
C28 N3 C24 117.9(5) . . ?
C28 N3 Ni1 127.3(4) . . ?
C24 N3 Ni1 114.8(3) . . ?
C29 N4 C33 118.1(5) . . ?
C29 N4 Ni1 126.9(4) . . ?
C33 N4 Ni1 115.0(4) . . ?
C38 N5 C34 118.7(5) . . ?
C38 N5 Ni1 125.5(4) . . ?
C34 N5 Ni1 115.8(4) . . ?
C39 N6 C43 118.5(5) . . ?
C39 N6 Ni1 125.6(4) . . ?
C43 N6 Ni1 115.7(4) . . ?
C44 N7 C48 119.0(5) . . ?
C44 N7 Ni1 115.0(4) . . ?
C48 N7 Ni1 125.7(4) . . ?
C53 N8 C49 118.1(8) . . ?
C53 N8 C52 124.6(8) . . ?
C49 N8 C52 115.8(7) . . ?
O5 C1 O6 121.2(5) . . ?
O5 C1 C2 120.7(5) . . ?
O6 C1 C2 118.1(5) . . ?
C3 C2 C1 128.0(5) . . ?
C3 C2 S1 112.3(4) . . ?
C1 C2 S1 119.7(4) . . ?
C2 C3 C4 112.4(5) . . ?
C2 C3 H3 123.8 . . ?
C4 C3 H3 123.8 . . ?
C5 C4 C3 112.6(5) . . ?
C5 C4 H4 123.7 . . ?
C3 C4 H4 123.7 . . ?
C4 C5 C6 130.1(5) . . ?
C4 C5 S1 112.0(4) . . ?
C6 C5 S1 117.9(4) . . ?
O8 C6 O7 120.5(5) . . ?
O8 C6 C5 118.9(5) . . ?
O7 C6 C5 120.5(5) . . ?
O10 C7 O9 120.4(5) . . ?
O10 C7 C8 120.6(5) . . ?
O9 C7 C8 119.0(5) . . ?
C9 C8 C7 128.0(5) . . ?
C9 C8 S2 112.7(5) . . ?
C7 C8 S2 119.3(4) . . ?
C8 C9 C10 112.4(5) . . ?
C8 C9 H9 123.8 . . ?
C10 C9 H9 123.8 . . ?
C11 C10 C9 112.1(5) . . ?
C11 C10 H10 123.9 . . ?
C9 C10 H10 123.9 . . ?
C10 C11 C12 127.6(5) . . ?
C10 C11 S2 111.6(4) . . ?
C12 C11 S2 120.8(4) . . ?
O11 C12 O12 120.8(5) . . ?
O11 C12 C11 120.3(5) . . ?
O12 C12 C11 118.9(5) . . ?
O14 C13 O13 121.4(5) . . ?
O14 C13 C14 121.8(5) . . ?
O13 C13 C14 116.7(5) . . ?
C15 C14 C13 130.4(5) . . ?
C15 C14 S3 112.3(4) . . ?
C13 C14 S3 117.3(4) . . ?
C14 C15 C16 112.1(5) . . ?
C14 C15 H15A 123.9 . . ?
C16 C15 H15A 123.9 . . ?
C17 C16 C15 111.7(5) . . ?
C17 C16 H16 124.2 . . ?
C15 C16 H16 124.2 . . ?
C16 C17 C18 129.5(5) . . ?
C16 C17 S3 112.7(4) . . ?
C18 C17 S3 117.8(5) . . ?
O16 C18 O15 125.5(5) . . ?
O16 C18 C17 122.8(5) . . ?
O15 C18 C17 111.7(5) . . ?
N2 C19 C20 122.3(6) . . ?
N2 C19 H19 118.8 . . ?
C20 C19 H19 118.8 . . ?
C19 C20 C21 118.1(6) . . ?
C19 C20 H20 120.9 . . ?
C21 C20 H20 120.9 . . ?
C20 C21 C22 120.8(6) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C21 C22 C23 117.8(7) . . ?
C21 C22 H22 121.1 . . ?
C23 C22 H22 121.1 . . ?
N2 C23 C22 121.9(6) . . ?
N2 C23 C24 115.7(5) . . ?
C22 C23 C24 122.4(5) . . ?
N3 C24 C25 121.6(5) . . ?
N3 C24 C23 114.8(5) . . ?
C25 C24 C23 123.6(5) . . ?
C26 C25 C24 119.2(6) . . ?
C26 C25 H25 120.4 . . ?
C24 C25 H25 120.4 . . ?
C27 C26 C25 118.6(6) . . ?
C27 C26 H26 120.7 . . ?
C25 C26 H26 120.7 . . ?
C26 C27 C28 120.0(6) . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
N3 C28 C27 122.6(6) . . ?
N3 C28 H28 118.7 . . ?
C27 C28 H28 118.7 . . ?
N4 C29 C30 123.6(6) . . ?
N4 C29 H29 118.2 . . ?
C30 C29 H29 118.2 . . ?
C31 C30 C29 118.3(6) . . ?
C31 C30 H30 120.9 . . ?
C29 C30 H30 120.9 . . ?
C30 C31 C32 120.1(6) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C31 C32 C33 118.9(6) . . ?
C31 C32 H32 120.5 . . ?
C33 C32 H32 120.5 . . ?
N4 C33 C32 121.0(5) . . ?
N4 C33 C34 115.5(5) . . ?
C32 C33 C34 123.5(5) . . ?
N5 C34 C35 120.7(5) . . ?
N5 C34 C33 114.6(5) . . ?
C35 C34 C33 124.7(5) . . ?
C34 C35 C36 120.1(6) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C37 C36 C35 119.1(6) . . ?
C37 C36 H36 120.5 . . ?
C35 C36 H36 120.5 . . ?
C36 C37 C38 119.0(6) . . ?
C36 C37 H37 120.5 . . ?
C38 C37 H37 120.5 . . ?
N5 C38 C37 122.6(6) . . ?
N5 C38 H38 118.7 . . ?
C37 C38 H38 118.7 . . ?
N6 C39 C40 123.2(6) . . ?
N6 C39 H39 118.4 . . ?
C40 C39 H39 118.4 . . ?
C41 C40 C39 118.3(6) . . ?
C41 C40 H40 120.9 . . ?
C39 C40 H40 120.9 . . ?
C40 C41 C42 119.2(6) . . ?
C40 C41 H41 120.4 . . ?
C42 C41 H41 120.4 . . ?
C43 C42 C41 119.5(6) . . ?
C43 C42 H42 120.3 . . ?
C41 C42 H42 120.3 . . ?
N6 C43 C42 121.2(6) . . ?
N6 C43 C44 115.0(5) . . ?
C42 C43 C44 123.8(6) . . ?
N7 C44 C45 121.2(6) . . ?
N7 C44 C43 115.8(5) . . ?
C45 C44 C43 122.9(5) . . ?
C46 C45 C44 118.8(6) . . ?
C46 C45 H45 120.6 . . ?
C44 C45 H45 120.6 . . ?
C47 C46 C45 119.7(6) . . ?
C47 C46 H46 120.2 . . ?
C45 C46 H46 120.2 . . ?
C48 C47 C46 119.2(6) . . ?
C48 C47 H47 120.4 . . ?
C46 C47 H47 120.4 . . ?
N7 C48 C47 122.1(6) . . ?
N7 C48 H48 119.0 . . ?
C47 C48 H48 119.0 . . ?
O20 C49 N8 124.9(8) . . ?
O20 C49 C50 128.3(8) . . ?
N8 C49 C50 106.8(6) . . ?
C49 C50 C51 105.6(6) . . ?
C49 C50 H50A 110.6 . . ?
C51 C50 H50A 110.6 . . ?
C49 C50 H50B 110.6 . . ?
C51 C50 H50B 110.6 . . ?
H50A C50 H50B 108.7 . . ?
C50 C51 C52 103.0(5) . . ?
C50 C51 H51A 111.2 . . ?
C52 C51 H51A 111.2 . . ?
C50 C51 H51B 111.2 . . ?
C52 C51 H51B 111.2 . . ?
H51A C51 H51B 109.1 . . ?
N8 C52 C51 104.3(5) . . ?
N8 C52 H52A 110.9 . . ?
C51 C52 H52A 110.9 . . ?
N8 C52 H52B 110.9 . . ?
C51 C52 H52B 110.9 . . ?
H52A C52 H52B 108.9 . . ?
N8 C53 H53A 109.5 . . ?
N8 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
N8 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O15 H15 O20 0.97 1.64 2.599(6) 167.6 .

_refine_diff_density_max         1.736
_refine_diff_density_min         -1.674
_refine_diff_density_rms         0.172

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1437895'
_audit_update_record             
;
2015-11-19 deposited with the CCDC.
2016-01-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H56 Cl Co N8 O26 S4 U2'
_chemical_formula_weight         1739.58

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   10.8016(4)
_cell_length_b                   20.4090(8)
_cell_length_c                   12.8547(5)
_cell_angle_alpha                90
_cell_angle_beta                 105.973(2)
_cell_angle_gamma                90
_cell_volume                     2724.41(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    101930
_cell_measurement_theta_min      2.96
_cell_measurement_theta_max      25.68

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'translucent light yellow-orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.121
_exptl_crystal_F_000             1680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    6.525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.384
_exptl_absorpt_correction_T_max  0.488
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 30 mm'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and six ω scans with 2° steps (492 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            101930
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.961
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             10337
_reflns_number_gt                9510
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. Two lattice water molecules were given occupancy factors of
 0.5 in order to retain acceptable displacement parameters. All non-hydrogen
 atoms were refined with anisotropic displacement parameters, with restraints
 for three badly behaving oxygen atoms. The H atoms bound to N7, N8 and 
 three water molecules were found on difference Fourier maps; those bound 
 to N1-N6 and to C atoms were introduced at calculated positions; all were
 treated as riding atoms with an isotropic displacement parameter equal
 to 1.2 times that of the parent atom.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0876P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_Flack   -0.005(9)
_refine_ls_abs_structure_details 
;
absolute configuration determined from Flack parameter
;
_chemical_absolute_configuration syn
_refine_ls_number_reflns         10337
_refine_ls_number_parameters     731
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0338
_refine_ls_wR_factor_ref         0.1194
_refine_ls_wR_factor_gt          0.1163
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.52394(5) 0.36918(2) 0.22439(4) 0.03140(17) Uani 1 1 d . . . . .
U2 U 0.03812(4) 0.62845(2) 0.73694(3) 0.02661(15) Uani 1 1 d . . . . .
Co1 Co 0.25428(18) 0.24889(12) 0.74711(13) 0.0231(3) Uani 1 1 d . . . . .
S1 S 0.2670(3) 0.48830(18) 0.4761(3) 0.0278(7) Uani 1 1 d . . . . .
S2 S 0.7622(3) 0.50825(19) -0.0254(3) 0.0289(8) Uani 1 1 d . . . . .
S3 S 0.4093(3) 0.1313(2) 0.3656(3) 0.0345(8) Uani 1 1 d . . . . .
S4 S -0.0850(3) 0.8674(2) 0.8670(3) 0.0312(7) Uani 1 1 d . . . . .
Cl1 Cl -0.1404(3) 0.25810(17) 0.7498(3) 0.0373(7) Uani 1 1 d . . . . .
O1 O 0.6662(9) 0.3743(8) 0.3342(8) 0.041(3) Uani 1 1 d . . . . .
O2 O 0.3828(9) 0.3659(7) 0.1152(7) 0.039(2) Uani 1 1 d . . . . .
O3 O 0.1820(8) 0.6237(8) 0.8431(7) 0.037(2) Uani 1 1 d . . . . .
O4 O -0.1049(8) 0.6333(6) 0.6302(6) 0.0277(19) Uani 1 1 d . U . . .
O5 O 0.3942(11) 0.4037(5) 0.3475(8) 0.038(3) Uani 1 1 d . . . . .
O6 O 0.4638(10) 0.4829(7) 0.2603(8) 0.039(3) Uani 1 1 d . . . . .
O7 O 0.1571(9) 0.6467(5) 0.6007(8) 0.032(2) Uani 1 1 d . . . . .
O8 O 0.1263(11) 0.5437(6) 0.6342(9) 0.037(3) Uani 1 1 d . . . . .
O9 O 0.6125(11) 0.4529(6) 0.1258(8) 0.038(3) Uani 1 1 d . . . . .
O10 O 0.6483(9) 0.3499(5) 0.0955(8) 0.032(2) Uani 1 1 d . . . . .
O11 O 0.9771(9) 0.5166(7) -0.2266(7) 0.033(3) Uani 1 1 d . . . . .
O12 O 0.9094(10) 0.5953(5) -0.1394(8) 0.035(2) Uani 1 1 d . . . . .
O13 O 0.5570(11) 0.2519(6) 0.1935(8) 0.039(3) Uani 1 1 d . . . . .
O14 O 0.4507(12) 0.2729(6) 0.3103(9) 0.045(3) Uani 1 1 d . . . . .
O15 O 0.3406(10) 0.0028(5) 0.4594(8) 0.042(3) Uani 1 1 d . . . . .
O16 O 0.4262(10) -0.0608(5) 0.3551(8) 0.038(2) Uani 1 1 d . . . . .
H16 H 0.4009 -0.0934 0.3915 0.045 Uiso 1 1 d R U . . .
O17 O -0.0218(11) 0.7240(5) 0.8344(8) 0.037(2) Uani 1 1 d . . . . .
O18 O 0.0738(10) 0.7445(5) 0.7054(8) 0.036(2) Uani 1 1 d . . . . .
O19 O -0.1660(11) 0.9946(6) 0.9463(10) 0.051(3) Uani 1 1 d . . . . .
O20 O -0.0598(10) 1.0591(5) 0.8577(8) 0.040(2) Uani 1 1 d . . . . .
H20 H -0.1118 1.0844 0.8830 0.048 Uiso 1 1 d R U . . .
O21 O 0.3915(14) 0.5803(8) 0.0779(14) 0.093(6) Uani 1 1 d . . . . .
H21A H 0.4266 0.5762 0.1509 0.111 Uiso 1 1 d R U . . .
H21B H 0.3791 0.6253 0.0876 0.111 Uiso 1 1 d R U . . .
O22 O 0.9030(17) 0.4375(9) -0.4250(16) 0.105(6) Uani 1 1 d . . . . .
H22A H 0.9335 0.4605 -0.3594 0.126 Uiso 1 1 d R U . . .
H22B H 0.8119 0.4440 -0.4632 0.126 Uiso 1 1 d R U . . .
O23 O 0.3497(10) -0.1685(6) 0.4347(8) 0.045(3) Uani 1 1 d . . . . .
H23A H 0.2792 -0.1857 0.3926 0.054 Uiso 1 1 d R U . . .
H23B H 0.4302 -0.1932 0.4373 0.054 Uiso 1 1 d R U . . .
O24 O 0.5392(11) 0.1994(5) -0.0095(8) 0.049(3) Uani 1 1 d . . . . .
O25 O -0.1384(15) 1.1644(6) 0.9397(10) 0.069(4) Uani 1 1 d . . . . .
O26 O 0.3479(18) 0.2974(9) 0.4816(15) 0.034(4) Uani 0.5 1 d . U P . .
O27 O 0.259(2) -0.2387(13) 0.5744(19) 0.060(6) Uani 0.5 1 d . U P . .
N1 N 0.0941(11) 0.2088(6) 0.6558(9) 0.027(2) Uani 1 1 d . . . . .
H1 H 0.0252 0.2182 0.6921 0.033 Uiso 1 1 calc R U . . .
N2 N 0.2146(11) 0.3242(6) 0.6481(8) 0.031(3) Uani 1 1 d . . . . .
H2 H 0.2698 0.3176 0.5980 0.037 Uiso 1 1 calc R U . . .
N3 N 0.3537(10) 0.2059(6) 0.6580(9) 0.029(2) Uani 1 1 d . . . . .
H3 H 0.3354 0.2318 0.5894 0.035 Uiso 1 1 calc R U . . .
N4 N 0.4180(10) 0.2913(6) 0.8267(9) 0.030(3) Uani 1 1 d . . . . .
H4 H 0.4552 0.2639 0.8924 0.035 Uiso 1 1 calc R U . . .
N5 N 0.2820(12) 0.1738(6) 0.8473(9) 0.032(3) Uani 1 1 d . . . . .
H5 H 0.3716 0.1784 0.8955 0.038 Uiso 1 1 calc R U . . .
N6 N 0.1616(11) 0.2901(6) 0.8447(9) 0.033(3) Uani 1 1 d . . . . .
H6 H 0.0680 0.2817 0.8107 0.039 Uiso 1 1 calc R U . . .
N7 N 0.2042(12) 0.0345(6) 0.6467(10) 0.035(3) Uani 1 1 d . . . . .
H7A H 0.2865 0.0099 0.6757 0.042 Uiso 1 1 d R U . . .
H7B H 0.1899 0.0323 0.5748 0.042 Uiso 1 1 d R U . . .
N8 N 0.2964(12) 0.4635(6) 0.8507(9) 0.032(3) Uani 1 1 d . . . . .
H8A H 0.2064 0.4835 0.8269 0.038 Uiso 1 1 d R U . . .
H8B H 0.3662 0.4675 0.9186 0.038 Uiso 1 1 d R U . . .
C1 C 0.4011(13) 0.4640(8) 0.3257(11) 0.031(3) Uani 1 1 d . . . . .
C2 C 0.3352(11) 0.5123(7) 0.3778(11) 0.028(3) Uani 1 1 d . . . . .
C3 C 0.3245(13) 0.5759(8) 0.3567(11) 0.033(3) Uani 1 1 d . . . . .
H3A H 0.3529 0.5963 0.3010 0.040 Uiso 1 1 calc R U . . .
C4 C 0.2650(13) 0.6106(8) 0.4279(11) 0.035(3) Uani 1 1 d . . . . .
H4A H 0.2529 0.6567 0.4271 0.042 Uiso 1 1 calc R U . . .
C5 C 0.2283(12) 0.5690(7) 0.4964(10) 0.027(3) Uani 1 1 d . . . . .
C6 C 0.1680(14) 0.5870(8) 0.5822(11) 0.031(4) Uani 1 1 d . . . . .
C7 C 0.6635(14) 0.4093(7) 0.0772(11) 0.028(3) Uani 1 1 d . . . . .
C8 C 0.7304(11) 0.4290(7) -0.0027(11) 0.028(3) Uani 1 1 d . . . . .
C9 C 0.7817(11) 0.3848(7) -0.0637(10) 0.030(3) Uani 1 1 d . . . . .
H9 H 0.7744 0.3384 -0.0614 0.036 Uiso 1 1 calc R U . . .
C10 C 0.8447(12) 0.4187(7) -0.1282(11) 0.029(3) Uani 1 1 d . . . . .
H10 H 0.8831 0.3971 -0.1769 0.035 Uiso 1 1 calc R U . . .
C11 C 0.8473(12) 0.4857(7) -0.1162(10) 0.028(3) Uani 1 1 d . . . . .
C12 C 0.9139(14) 0.5363(9) -0.1641(12) 0.034(4) Uani 1 1 d . . . . .
C13 C 0.5009(18) 0.2306(10) 0.2622(14) 0.043(4) Uani 1 1 d . . . . .
C14 C 0.4871(14) 0.1621(8) 0.2763(10) 0.034(3) Uani 1 1 d . . . . .
C15 C 0.5366(13) 0.1124(8) 0.2274(10) 0.033(4) Uani 1 1 d . . . . .
H15 H 0.5855 0.1196 0.1773 0.040 Uiso 1 1 calc R U . . .
C16 C 0.5067(16) 0.0496(9) 0.2595(12) 0.036(4) Uani 1 1 d . . . . .
H16A H 0.5304 0.0098 0.2316 0.044 Uiso 1 1 calc R U . . .
C17 C 0.4396(13) 0.0526(7) 0.3355(10) 0.029(3) Uani 1 1 d . . . . .
C18 C 0.3963(14) -0.0024(7) 0.3899(12) 0.034(3) Uani 1 1 d . . . . .
C19 C 0.0159(15) 0.7648(8) 0.7744(10) 0.028(3) Uani 1 1 d . . . . .
C20 C 0.0004(13) 0.8362(8) 0.7841(11) 0.030(3) Uani 1 1 d . . . . .
C21 C 0.0465(12) 0.8845(9) 0.7315(10) 0.033(4) Uani 1 1 d . . . . .
H21 H 0.0939 0.8762 0.6807 0.040 Uiso 1 1 calc R U . . .
C22 C 0.0168(15) 0.9475(7) 0.7600(12) 0.032(3) Uani 1 1 d . . . . .
H22 H 0.0428 0.9865 0.7316 0.039 Uiso 1 1 calc R U . . .
C23 C -0.0537(12) 0.9467(7) 0.8331(11) 0.030(3) Uani 1 1 d . . . . .
C24 C -0.1001(13) 1.0017(8) 0.8849(12) 0.035(3) Uani 1 1 d . . . . .
C25 C 0.2251(13) 0.1038(7) 0.6795(10) 0.029(3) Uani 1 1 d . . . . .
C26 C 0.0946(12) 0.1372(7) 0.6400(10) 0.029(3) Uani 1 1 d . . . . .
H26A H 0.0593 0.1279 0.5619 0.034 Uiso 1 1 calc R U . . .
H26B H 0.0355 0.1172 0.6778 0.034 Uiso 1 1 calc R U . . .
C27 C 0.0590(14) 0.2461(7) 0.5511(10) 0.036(3) Uani 1 1 d . . . . .
H27A H 0.1130 0.2315 0.5044 0.044 Uiso 1 1 calc R U . . .
H27B H -0.0325 0.2385 0.5121 0.044 Uiso 1 1 calc R U . . .
C28 C 0.0816(13) 0.3171(7) 0.5784(11) 0.036(3) Uani 1 1 d . . . . .
H28A H 0.0700 0.3431 0.5114 0.044 Uiso 1 1 calc R U . . .
H28B H 0.0196 0.3329 0.6168 0.044 Uiso 1 1 calc R U . . .
C29 C 0.2485(14) 0.3920(7) 0.6933(10) 0.033(3) Uani 1 1 d . . . . .
H29A H 0.1754 0.4219 0.6625 0.039 Uiso 1 1 calc R U . . .
H29B H 0.3239 0.4083 0.6712 0.039 Uiso 1 1 calc R U . . .
C30 C 0.2796(13) 0.3932(6) 0.8163(10) 0.027(3) Uani 1 1 d . . . . .
C31 C 0.3236(12) 0.1365(8) 0.6239(11) 0.033(3) Uani 1 1 d . . . . .
H31A H 0.4044 0.1108 0.6424 0.040 Uiso 1 1 calc R U . . .
H31B H 0.2870 0.1349 0.5444 0.040 Uiso 1 1 calc R U . . .
C32 C 0.4932(12) 0.2154(7) 0.7115(12) 0.034(3) Uani 1 1 d . . . . .
H32A H 0.5439 0.2089 0.6588 0.041 Uiso 1 1 calc R U . . .
H32B H 0.5232 0.1836 0.7712 0.041 Uiso 1 1 calc R U . . .
C33 C 0.5097(15) 0.2853(8) 0.7552(14) 0.044(4) Uani 1 1 d . . . . .
H33A H 0.4870 0.3174 0.6951 0.053 Uiso 1 1 calc R U . . .
H33B H 0.5998 0.2931 0.7980 0.053 Uiso 1 1 calc R U . . .
C34 C 0.4117(13) 0.3592(7) 0.8651(11) 0.030(3) Uani 1 1 d . . . . .
H34A H 0.4798 0.3854 0.8468 0.036 Uiso 1 1 calc R U . . .
H34B H 0.4299 0.3587 0.9450 0.036 Uiso 1 1 calc R U . . .
C35 C 0.2736(14) 0.1065(6) 0.7997(11) 0.031(3) Uani 1 1 d . . . . .
H35A H 0.3603 0.0863 0.8219 0.037 Uiso 1 1 calc R U . . .
H35B H 0.2163 0.0796 0.8309 0.037 Uiso 1 1 calc R U . . .
C36 C 0.1950(16) 0.1822(7) 0.9174(11) 0.043(4) Uani 1 1 d . . . . .
H36A H 0.2251 0.1551 0.9834 0.052 Uiso 1 1 calc R U . . .
H36B H 0.1066 0.1682 0.8784 0.052 Uiso 1 1 calc R U . . .
C37 C 0.1955(15) 0.2532(7) 0.9472(11) 0.039(3) Uani 1 1 d . . . . .
H37A H 0.1317 0.2616 0.9882 0.046 Uiso 1 1 calc R U . . .
H37B H 0.2817 0.2663 0.9925 0.046 Uiso 1 1 calc R U . . .
C38 C 0.1751(13) 0.3633(8) 0.8588(11) 0.033(3) Uani 1 1 d . . . . .
H38A H 0.1932 0.3736 0.9368 0.039 Uiso 1 1 calc R U . . .
H38B H 0.0919 0.3840 0.8213 0.039 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 1.767(10) . ?
U1 O1 1.781(10) . ?
U1 O10 2.435(9) . ?
U1 O13 2.468(12) . ?
U1 O9 2.471(10) . ?
U1 O5 2.487(10) . ?
U1 O14 2.488(11) . ?
U1 O6 2.488(13) . ?
U2 O4 1.765(8) . ?
U2 O3 1.766(9) . ?
U2 O18 2.451(11) . ?
U2 O11 2.456(13) 1_456 ?
U2 O7 2.468(9) . ?
U2 O12 2.476(9) 1_456 ?
U2 O17 2.498(10) . ?
U2 O8 2.518(10) . ?
Co1 N2 1.966(11) . ?
Co1 N5 1.971(12) . ?
Co1 N3 1.978(11) . ?
Co1 N1 1.980(12) . ?
Co1 N4 1.982(11) . ?
Co1 N6 1.993(12) . ?
S1 C2 1.701(12) . ?
S1 C5 1.735(14) . ?
S2 C8 1.696(15) . ?
S2 C11 1.734(12) . ?
S3 C17 1.704(15) . ?
S3 C14 1.718(13) . ?
S4 C20 1.713(14) . ?
S4 C23 1.733(15) . ?
O5 C1 1.270(19) . ?
O6 C1 1.275(17) . ?
O7 C6 1.254(19) . ?
O8 C6 1.263(19) . ?
O9 C7 1.293(18) . ?
O10 C7 1.254(17) . ?
O11 C12 1.255(17) . ?
O11 U2 2.456(13) 1_654 ?
O12 C12 1.25(2) . ?
O12 U2 2.476(9) 1_654 ?
O13 C13 1.28(2) . ?
O14 C13 1.27(2) . ?
O15 C18 1.211(17) . ?
O16 C18 1.343(18) . ?
O16 H16 0.8981 . ?
O17 C19 1.275(18) . ?
O18 C19 1.286(18) . ?
O19 C24 1.209(18) . ?
O20 C24 1.329(19) . ?
O20 H20 0.8873 . ?
O21 H21A 0.9132 . ?
O21 H21B 0.9421 . ?
O22 H22A 0.9420 . ?
O22 H22B 0.9799 . ?
O23 H23A 0.8769 . ?
O23 H23B 0.9969 . ?
N1 C26 1.476(19) . ?
N1 C27 1.500(17) . ?
N1 H1 1.0000 . ?
N2 C28 1.476(17) . ?
N2 C29 1.506(18) . ?
N2 H2 1.0000 . ?
N3 C32 1.486(17) . ?
N3 C31 1.49(2) . ?
N3 H3 1.0000 . ?
N4 C34 1.479(19) . ?
N4 C33 1.53(2) . ?
N4 H4 1.0000 . ?
N5 C36 1.481(17) . ?
N5 C35 1.496(17) . ?
N5 H5 1.0000 . ?
N6 C37 1.474(18) . ?
N6 C38 1.51(2) . ?
N6 H6 1.0000 . ?
N7 C25 1.475(18) . ?
N7 H7A 0.9983 . ?
N7 H7B 0.8962 . ?
N8 C30 1.498(17) . ?
N8 H8A 1.0206 . ?
N8 H8B 0.9873 . ?
C1 C2 1.48(2) . ?
C2 C3 1.32(2) . ?
C3 C4 1.44(2) . ?
C3 H3A 0.9500 . ?
C4 C5 1.36(2) . ?
C4 H4A 0.9500 . ?
C5 C6 1.474(19) . ?
C7 C8 1.465(18) . ?
C8 C9 1.406(19) . ?
C9 C10 1.393(18) . ?
C9 H9 0.9500 . ?
C10 C11 1.37(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.49(2) . ?
C13 C14 1.42(3) . ?
C14 C15 1.38(2) . ?
C15 C16 1.41(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.37(2) . ?
C16 H16A 0.9500 . ?
C17 C18 1.47(2) . ?
C19 C20 1.48(2) . ?
C20 C21 1.36(2) . ?
C21 C22 1.40(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.36(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.46(2) . ?
C25 C35 1.491(19) . ?
C25 C26 1.522(19) . ?
C25 C31 1.583(18) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.495(19) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.524(18) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C38 1.512(18) . ?
C30 C34 1.555(18) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.525(19) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.50(2) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U1 O1 178.8(8) . . ?
O2 U1 O10 88.3(4) . . ?
O1 U1 O10 91.8(4) . . ?
O2 U1 O13 88.1(5) . . ?
O1 U1 O13 93.0(6) . . ?
O10 U1 O13 66.6(3) . . ?
O2 U1 O9 89.4(5) . . ?
O1 U1 O9 89.7(5) . . ?
O10 U1 O9 53.0(4) . . ?
O13 U1 O9 119.6(3) . . ?
O2 U1 O5 90.1(4) . . ?
O1 U1 O5 89.6(4) . . ?
O10 U1 O5 172.6(4) . . ?
O13 U1 O5 120.6(3) . . ?
O9 U1 O5 119.7(4) . . ?
O2 U1 O14 90.7(5) . . ?
O1 U1 O14 90.3(5) . . ?
O10 U1 O14 118.5(4) . . ?
O13 U1 O14 51.9(3) . . ?
O9 U1 O14 171.5(4) . . ?
O5 U1 O14 68.8(4) . . ?
O2 U1 O6 88.3(5) . . ?
O1 U1 O6 90.6(5) . . ?
O10 U1 O6 119.9(3) . . ?
O13 U1 O6 172.5(3) . . ?
O9 U1 O6 66.9(3) . . ?
O5 U1 O6 52.8(3) . . ?
O14 U1 O6 121.6(4) . . ?
O4 U2 O3 179.6(4) . . ?
O4 U2 O18 87.8(5) . . ?
O3 U2 O18 92.1(5) . . ?
O4 U2 O11 88.7(5) . 1_456 ?
O3 U2 O11 91.5(5) . 1_456 ?
O18 U2 O11 172.8(3) . 1_456 ?
O4 U2 O7 87.4(3) . . ?
O3 U2 O7 92.1(4) . . ?
O18 U2 O7 66.5(3) . . ?
O11 U2 O7 119.7(3) 1_456 . ?
O4 U2 O12 89.3(4) . 1_456 ?
O3 U2 O12 91.1(4) . 1_456 ?
O18 U2 O12 120.8(3) . 1_456 ?
O11 U2 O12 52.9(3) 1_456 1_456 ?
O7 U2 O12 172.0(3) . 1_456 ?
O4 U2 O17 93.1(4) . . ?
O3 U2 O17 87.1(5) . . ?
O18 U2 O17 53.3(3) . . ?
O11 U2 O17 120.6(3) 1_456 . ?
O7 U2 O17 119.7(3) . . ?
O12 U2 O17 67.8(4) 1_456 . ?
O4 U2 O8 90.4(4) . . ?
O3 U2 O8 89.3(5) . . ?
O18 U2 O8 118.6(3) . . ?
O11 U2 O8 67.8(3) 1_456 . ?
O7 U2 O8 52.1(3) . . ?
O12 U2 O8 120.6(4) 1_456 . ?
O17 U2 O8 170.9(4) . . ?
N2 Co1 N5 176.1(6) . . ?
N2 Co1 N3 91.6(5) . . ?
N5 Co1 N3 91.4(5) . . ?
N2 Co1 N1 86.6(5) . . ?
N5 Co1 N1 91.0(5) . . ?
N3 Co1 N1 89.9(5) . . ?
N2 Co1 N4 89.8(5) . . ?
N5 Co1 N4 92.8(5) . . ?
N3 Co1 N4 86.7(5) . . ?
N1 Co1 N4 175.0(5) . . ?
N2 Co1 N6 91.1(5) . . ?
N5 Co1 N6 86.0(5) . . ?
N3 Co1 N6 176.6(5) . . ?
N1 Co1 N6 92.3(5) . . ?
N4 Co1 N6 91.3(5) . . ?
C2 S1 C5 90.6(7) . . ?
C8 S2 C11 91.9(7) . . ?
C17 S3 C14 91.9(7) . . ?
C20 S4 C23 90.9(7) . . ?
C1 O5 U1 93.3(8) . . ?
C1 O6 U1 93.0(10) . . ?
C6 O7 U2 94.7(9) . . ?
C6 O8 U2 92.2(9) . . ?
C7 O9 U1 92.8(8) . . ?
C7 O10 U1 95.5(8) . . ?
C12 O11 U2 92.7(11) . 1_654 ?
C12 O12 U2 91.8(9) . 1_654 ?
C13 O13 U1 95.9(10) . . ?
C13 O14 U1 95.2(11) . . ?
C18 O16 H16 110.4 . . ?
C19 O17 U2 92.1(8) . . ?
C19 O18 U2 93.9(9) . . ?
C24 O20 H20 97.5 . . ?
H21A O21 H21B 89.2 . . ?
H22A O22 H22B 115.9 . . ?
H23A O23 H23B 114.8 . . ?
C26 N1 C27 112.9(11) . . ?
C26 N1 Co1 117.1(8) . . ?
C27 N1 Co1 106.7(8) . . ?
C26 N1 H1 106.5 . . ?
C27 N1 H1 106.5 . . ?
Co1 N1 H1 106.5 . . ?
C28 N2 C29 114.7(11) . . ?
C28 N2 Co1 108.5(8) . . ?
C29 N2 Co1 118.9(7) . . ?
C28 N2 H2 104.4 . . ?
C29 N2 H2 104.4 . . ?
Co1 N2 H2 104.4 . . ?
C32 N3 C31 111.8(11) . . ?
C32 N3 Co1 108.5(8) . . ?
C31 N3 Co1 118.8(8) . . ?
C32 N3 H3 105.6 . . ?
C31 N3 H3 105.6 . . ?
Co1 N3 H3 105.6 . . ?
C34 N4 C33 111.9(11) . . ?
C34 N4 Co1 117.7(8) . . ?
C33 N4 Co1 106.7(8) . . ?
C34 N4 H4 106.6 . . ?
C33 N4 H4 106.6 . . ?
Co1 N4 H4 106.6 . . ?
C36 N5 C35 112.2(11) . . ?
C36 N5 Co1 107.4(9) . . ?
C35 N5 Co1 117.8(8) . . ?
C36 N5 H5 106.2 . . ?
C35 N5 H5 106.2 . . ?
Co1 N5 H5 106.2 . . ?
C37 N6 C38 114.0(11) . . ?
C37 N6 Co1 107.6(8) . . ?
C38 N6 Co1 116.5(8) . . ?
C37 N6 H6 106.0 . . ?
C38 N6 H6 106.0 . . ?
Co1 N6 H6 106.0 . . ?
C25 N7 H7A 108.9 . . ?
C25 N7 H7B 108.1 . . ?
H7A N7 H7B 104.1 . . ?
C30 N8 H8A 105.5 . . ?
C30 N8 H8B 110.0 . . ?
H8A N8 H8B 131.7 . . ?
O5 C1 O6 120.8(14) . . ?
O5 C1 C2 118.8(12) . . ?
O6 C1 C2 120.4(14) . . ?
C3 C2 C1 125.8(12) . . ?
C3 C2 S1 113.7(10) . . ?
C1 C2 S1 120.4(11) . . ?
C2 C3 C4 112.4(12) . . ?
C2 C3 H3A 123.8 . . ?
C4 C3 H3A 123.8 . . ?
C5 C4 C3 111.4(14) . . ?
C5 C4 H4A 124.3 . . ?
C3 C4 H4A 124.3 . . ?
C4 C5 C6 126.7(14) . . ?
C4 C5 S1 111.8(10) . . ?
C6 C5 S1 121.5(11) . . ?
O7 C6 O8 120.9(14) . . ?
O7 C6 C5 117.9(14) . . ?
O8 C6 C5 121.1(14) . . ?
O10 C7 O9 118.6(12) . . ?
O10 C7 C8 120.7(13) . . ?
O9 C7 C8 120.5(13) . . ?
C9 C8 C7 124.2(13) . . ?
C9 C8 S2 112.8(10) . . ?
C7 C8 S2 123.0(10) . . ?
C10 C9 C8 110.2(13) . . ?
C10 C9 H9 124.9 . . ?
C8 C9 H9 124.9 . . ?
C11 C10 C9 115.2(12) . . ?
C11 C10 H10 122.4 . . ?
C9 C10 H10 122.4 . . ?
C10 C11 C12 129.9(12) . . ?
C10 C11 S2 110.0(10) . . ?
C12 C11 S2 120.1(11) . . ?
O12 C12 O11 122.5(15) . . ?
O12 C12 C11 120.5(13) . . ?
O11 C12 C11 117.0(15) . . ?
O14 C13 O13 116.9(17) . . ?
O14 C13 C14 122.2(16) . . ?
O13 C13 C14 120.6(16) . . ?
C15 C14 C13 126.8(14) . . ?
C15 C14 S3 111.0(12) . . ?
C13 C14 S3 122.1(12) . . ?
C14 C15 C16 112.8(13) . . ?
C14 C15 H15 123.6 . . ?
C16 C15 H15 123.6 . . ?
C17 C16 C15 112.1(15) . . ?
C17 C16 H16A 124.0 . . ?
C15 C16 H16A 124.0 . . ?
C16 C17 C18 127.4(14) . . ?
C16 C17 S3 112.2(12) . . ?
C18 C17 S3 120.4(10) . . ?
O15 C18 O16 122.5(14) . . ?
O15 C18 C17 125.0(14) . . ?
O16 C18 C17 112.5(12) . . ?
O17 C19 O18 120.3(14) . . ?
O17 C19 C20 122.0(12) . . ?
O18 C19 C20 117.6(13) . . ?
C21 C20 C19 127.3(13) . . ?
C21 C20 S4 111.8(12) . . ?
C19 C20 S4 120.9(10) . . ?
C20 C21 C22 113.2(13) . . ?
C20 C21 H21 123.4 . . ?
C22 C21 H21 123.4 . . ?
C23 C22 C21 112.4(14) . . ?
C23 C22 H22 123.8 . . ?
C21 C22 H22 123.8 . . ?
C22 C23 C24 129.1(14) . . ?
C22 C23 S4 111.7(11) . . ?
C24 C23 S4 119.2(11) . . ?
O19 C24 O20 124.9(14) . . ?
O19 C24 C23 122.9(14) . . ?
O20 C24 C23 112.3(12) . . ?
N7 C25 C35 108.3(11) . . ?
N7 C25 C26 106.3(11) . . ?
C35 C25 C26 111.0(11) . . ?
N7 C25 C31 110.2(11) . . ?
C35 C25 C31 111.3(11) . . ?
C26 C25 C31 109.6(11) . . ?
N1 C26 C25 115.8(11) . . ?
N1 C26 H26A 108.3 . . ?
C25 C26 H26A 108.3 . . ?
N1 C26 H26B 108.3 . . ?
C25 C26 H26B 108.3 . . ?
H26A C26 H26B 107.4 . . ?
C28 C27 N1 107.2(10) . . ?
C28 C27 H27A 110.3 . . ?
N1 C27 H27A 110.3 . . ?
C28 C27 H27B 110.3 . . ?
N1 C27 H27B 110.3 . . ?
H27A C27 H27B 108.5 . . ?
N2 C28 C27 107.9(11) . . ?
N2 C28 H28A 110.1 . . ?
C27 C28 H28A 110.1 . . ?
N2 C28 H28B 110.1 . . ?
C27 C28 H28B 110.1 . . ?
H28A C28 H28B 108.4 . . ?
N2 C29 C30 112.0(10) . . ?
N2 C29 H29A 109.2 . . ?
C30 C29 H29A 109.2 . . ?
N2 C29 H29B 109.2 . . ?
C30 C29 H29B 109.2 . . ?
H29A C29 H29B 107.9 . . ?
N8 C30 C38 108.8(10) . . ?
N8 C30 C29 107.2(11) . . ?
C38 C30 C29 113.3(12) . . ?
N8 C30 C34 106.6(11) . . ?
C38 C30 C34 111.6(11) . . ?
C29 C30 C34 109.1(11) . . ?
N3 C31 C25 112.8(11) . . ?
N3 C31 H31A 109.0 . . ?
C25 C31 H31A 109.0 . . ?
N3 C31 H31B 109.0 . . ?
C25 C31 H31B 109.0 . . ?
H31A C31 H31B 107.8 . . ?
N3 C32 C33 107.0(11) . . ?
N3 C32 H32A 110.3 . . ?
C33 C32 H32A 110.3 . . ?
N3 C32 H32B 110.3 . . ?
C33 C32 H32B 110.3 . . ?
H32A C32 H32B 108.6 . . ?
C32 C33 N4 105.5(12) . . ?
C32 C33 H33A 110.6 . . ?
N4 C33 H33A 110.6 . . ?
C32 C33 H33B 110.6 . . ?
N4 C33 H33B 110.6 . . ?
H33A C33 H33B 108.8 . . ?
N4 C34 C30 113.9(11) . . ?
N4 C34 H34A 108.8 . . ?
C30 C34 H34A 108.8 . . ?
N4 C34 H34B 108.8 . . ?
C30 C34 H34B 108.8 . . ?
H34A C34 H34B 107.7 . . ?
C25 C35 N5 115.0(11) . . ?
C25 C35 H35A 108.5 . . ?
N5 C35 H35A 108.5 . . ?
C25 C35 H35B 108.5 . . ?
N5 C35 H35B 108.5 . . ?
H35A C35 H35B 107.5 . . ?
N5 C36 C37 108.1(10) . . ?
N5 C36 H36A 110.1 . . ?
C37 C36 H36A 110.1 . . ?
N5 C36 H36B 110.1 . . ?
C37 C36 H36B 110.1 . . ?
H36A C36 H36B 108.4 . . ?
N6 C37 C36 106.4(11) . . ?
N6 C37 H37A 110.4 . . ?
C36 C37 H37A 110.4 . . ?
N6 C37 H37B 110.4 . . ?
C36 C37 H37B 110.4 . . ?
H37A C37 H37B 108.6 . . ?
N6 C38 C30 114.4(11) . . ?
N6 C38 H38A 108.7 . . ?
C30 C38 H38A 108.7 . . ?
N6 C38 H38B 108.7 . . ?
C30 C38 H38B 108.7 . . ?
H38A C38 H38B 107.6 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 Cl1 1.00 2.27 3.252(12) 167.7 .
O16 H16 O23 0.90 1.77 2.651(15) 166.2 .
O20 H20 O25 0.89 1.84 2.635(16) 147.5 .
O21 H21A O6 0.91 2.34 3.007(19) 130.2 .
O21 H21B O24 0.94 2.13 2.758(18) 122.5 2_655
O21 H21B O25 0.94 2.65 3.18(2) 116.5 2_546
O22 H22A O11 0.94 2.00 2.94(2) 172.3 .
O22 H22B O15 0.98 2.05 2.87(2) 140.3 2_655
O23 H23A Cl1 0.88 2.33 3.167(12) 161.0 2_546
O23 H23B O26 1.00 2.34 3.22(2) 146.3 2_646
N1 H1 Cl1 1.00 2.27 3.252(12) 167.7 .
N2 H2 O26 1.00 1.95 2.941(19) 169.0 .
N3 H3 O26 1.00 1.96 2.92(2) 161.8 .
N4 H4 O24 1.00 1.88 2.854(16) 165.4 1_556
N5 H5 O24 1.00 1.93 2.926(17) 172.4 1_556
N6 H6 Cl1 1.00 2.22 3.219(12) 174.5 .
N7 H7A O6 1.00 2.65 3.610(16) 160.9 2_646
N7 H7B O15 0.90 2.56 3.215(14) 130.8 .
N8 H8A O11 1.02 2.48 3.489(16) 171.9 1_456

_refine_diff_density_max         1.709
_refine_diff_density_min         -1.318
_refine_diff_density_rms         0.128

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1437896'
_audit_update_record             
;
2015-11-19 deposited with the CCDC.
2016-01-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C128 H96 Fe2 N18 O44 S6 U5'
_chemical_formula_weight         4084.43

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   13.7311(8)
_cell_length_b                   15.5105(9)
_cell_length_c                   17.8862(9)
_cell_angle_alpha                68.574(3)
_cell_angle_beta                 70.094(3)
_cell_angle_gamma                76.948(3)
_cell_volume                     3311.7(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    156076
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      25.68

_exptl_crystal_description       irregular
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.048
_exptl_crystal_F_000             1950
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    6.492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.426
_exptl_absorpt_correction_T_max  0.595
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 30 mm'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'2 φ and 11 ω scans with 2° steps (630 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            156076
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.031
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             12556
_reflns_number_gt                10361
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 The structure of the isomorphous Ni-containing compound was used
 as a starting point for refinement. All non-hydrogen atoms were refined
 with anisotropic displacement parameters, with restraints for the methyl
 group of the solvent NMP molecule (C64). The H atoms were introduced
 at calculated positions and were treated as riding atoms with an isotropic
 displacement parameter equal to 1.2 times that of the parent atom
 (1.5 for CH₃, with optimized geometry). 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0655P)²+42.4307P] 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         12556
_refine_ls_number_parameters     918
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0519
_refine_ls_wR_factor_ref         0.1436
_refine_ls_wR_factor_gt          0.1371
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.002
_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
U1 U 0.36431(3) 0.24770(2) 1.06941(2) 0.02144(10) Uani 1 1 d . . . . .
U2 U 0.69678(3) 0.59197(2) 0.41716(2) 0.02227(10) Uani 1 1 d . . . . .
U3 U 0.0000 0.0000 0.5000 0.0548(2) Uani 1 2 d S . P . .
Fe1 Fe 0.13629(10) 0.74407(9) 0.10696(8) 0.0222(3) Uani 1 1 d . . . . .
S1 S 0.52006(18) 0.41902(15) 0.73944(13) 0.0250(5) Uani 1 1 d . . . . .
S2 S 0.03710(18) 0.42251(15) 1.25028(13) 0.0239(5) Uani 1 1 d . . . . .
S3 S 0.54201(19) 0.92395(15) 0.23686(14) 0.0259(5) Uani 1 1 d . . . . .
O1 O 0.4527(5) 0.3000(4) 1.0872(4) 0.0294(15) Uani 1 1 d . . . . .
O2 O 0.2784(5) 0.1940(5) 1.0501(4) 0.0292(15) Uani 1 1 d . . . . .
O3 O 0.7672(5) 0.6576(4) 0.4390(4) 0.0303(15) Uani 1 1 d . . . . .
O4 O 0.6271(5) 0.5266(5) 0.3953(4) 0.0314(15) Uani 1 1 d . . . . .
O5 O 0.1043(8) 0.0453(6) 0.4128(6) 0.072(3) Uani 1 1 d . . . . .
O6 O 0.4540(5) 0.2977(4) 0.9184(4) 0.0283(15) Uani 1 1 d . . . . .
O7 O 0.3308(5) 0.3999(4) 0.9648(4) 0.0284(15) Uani 1 1 d . . . . .
O8 O 0.6406(5) 0.4937(4) 0.5623(4) 0.0281(15) Uani 1 1 d . . . . .
O9 O 0.5488(5) 0.6308(4) 0.5325(4) 0.0307(15) Uani 1 1 d . . . . .
O10 O 0.2111(5) 0.3479(4) 1.1272(4) 0.0278(15) Uani 1 1 d . . . . .
O11 O 0.2572(6) 0.2179(5) 1.2166(4) 0.0353(17) Uani 1 1 d . . . . .
O12 O -0.1420(6) 0.5386(5) 1.3233(4) 0.0347(17) Uani 1 1 d . . . . .
O13 O -0.1732(5) 0.4510(4) 1.4551(4) 0.0301(15) Uani 1 1 d . . . . .
O14 O 0.5939(5) 0.7384(4) 0.3567(4) 0.0300(15) Uani 1 1 d . . . . .
O15 O 0.7326(5) 0.6929(5) 0.2671(4) 0.0322(16) Uani 1 1 d . . . . .
O16 O 0.4219(5) 1.0998(4) 0.1648(4) 0.0289(15) Uani 1 1 d . . . . .
O17 O 0.5101(5) 1.1253(4) 0.0329(4) 0.0262(14) Uani 1 1 d . . . . .
O18 O 0.0990(10) -0.0326(7) 0.6052(7) 0.081(3) Uani 1 1 d . . . . .
O19 O 0.0279(9) 0.1067(7) 0.5672(7) 0.074(3) Uani 1 1 d . . . . .
O20 O 0.1134(10) 0.0692(8) 0.6591(8) 0.082(3) Uani 1 1 d . . . . .
O21 O -0.1080(7) 0.1417(6) 0.4790(6) 0.058(2) Uani 1 1 d . . . . .
N1 N 0.0824(11) 0.0495(9) 0.6119(8) 0.066(3) Uani 1 1 d . . . . .
N2 N -0.2522(8) 0.2476(7) 0.4822(6) 0.047(2) Uani 1 1 d . . . . .
N3 N 0.0820(6) 0.6973(5) 0.2312(5) 0.0249(16) Uani 1 1 d . . . . .
N4 N 0.2321(6) 0.6260(5) 0.1253(5) 0.0241(16) Uani 1 1 d . . . . .
N5 N 0.0382(6) 0.6861(5) 0.0870(4) 0.0221(16) Uani 1 1 d . . . . .
N6 N 0.1993(6) 0.7722(5) -0.0145(5) 0.0245(16) Uani 1 1 d . . . . .
N7 N 0.0399(6) 0.8610(5) 0.1017(5) 0.0266(17) Uani 1 1 d . . . . .
N8 N 0.2261(6) 0.8147(5) 0.1242(5) 0.0245(16) Uani 1 1 d . . . . .
C1 C 0.4037(7) 0.3794(6) 0.9054(6) 0.025(2) Uani 1 1 d . . . . .
C2 C 0.4291(7) 0.4490(6) 0.8220(5) 0.0248(19) Uani 1 1 d . . . . .
C3 C 0.3935(8) 0.5420(7) 0.8000(6) 0.033(2) Uani 1 1 d . . . . .
H3 H 0.3448 0.5717 0.8381 0.040 Uiso 1 1 calc R U . . .
C4 C 0.4371(8) 0.5883(6) 0.7153(6) 0.031(2) Uani 1 1 d . . . . .
H4 H 0.4197 0.6528 0.6891 0.037 Uiso 1 1 calc R U . . .
C5 C 0.5074(7) 0.5312(6) 0.6740(6) 0.025(2) Uani 1 1 d . . . . .
C6 C 0.5675(7) 0.5536(6) 0.5848(6) 0.025(2) Uani 1 1 d . . . . .
C7 C 0.1992(8) 0.2936(7) 1.2019(6) 0.028(2) Uani 1 1 d . . . . .
C8 C 0.1167(7) 0.3190(6) 1.2707(6) 0.0244(19) Uani 1 1 d . . . . .
C9 C 0.0921(8) 0.2712(7) 1.3547(6) 0.031(2) Uani 1 1 d . . . . .
H9 H 0.1282 0.2127 1.3778 0.038 Uiso 1 1 calc R U . . .
C10 C 0.0094(8) 0.3163(6) 1.4031(6) 0.029(2) Uani 1 1 d . . . . .
H10 H -0.0166 0.2926 1.4624 0.035 Uiso 1 1 calc R U . . .
C11 C -0.0299(8) 0.3992(6) 1.3545(6) 0.026(2) Uani 1 1 d . . . . .
C12 C -0.1195(8) 0.4660(6) 1.3799(5) 0.027(2) Uani 1 1 d . . . . .
C13 C 0.6538(8) 0.7496(7) 0.2820(6) 0.028(2) Uani 1 1 d . . . . .
C14 C 0.6289(7) 0.8318(6) 0.2143(6) 0.0245(19) Uani 1 1 d . . . . .
C15 C 0.6666(7) 0.8461(6) 0.1286(6) 0.0246(19) Uani 1 1 d . . . . .
H15 H 0.7153 0.8029 0.1040 0.029 Uiso 1 1 calc R U . . .
C16 C 0.6239(7) 0.9330(6) 0.0823(6) 0.0249(19) Uani 1 1 d . . . . .
H16 H 0.6398 0.9540 0.0230 0.030 Uiso 1 1 calc R U . . .
C17 C 0.5575(7) 0.9834(6) 0.1316(5) 0.0221(18) Uani 1 1 d . . . . .
C18 C 0.4934(7) 1.0740(6) 0.1078(6) 0.0233(19) Uani 1 1 d . . . . .
C19 C -0.1865(10) 0.1831(8) 0.5183(8) 0.047(3) Uani 1 1 d . . . . .
C20 C -0.2168(12) 0.1717(11) 0.6086(8) 0.067(4) Uani 1 1 d . . . . .
H20A H -0.1568 0.1753 0.6256 0.080 Uiso 1 1 calc R U . . .
H20B H -0.2445 0.1113 0.6426 0.080 Uiso 1 1 calc R U . . .
C21 C -0.3018(13) 0.2538(10) 0.6181(9) 0.069(4) Uani 1 1 d . . . . .
H21A H -0.3599 0.2333 0.6693 0.083 Uiso 1 1 calc R U . . .
H21B H -0.2729 0.3045 0.6219 0.083 Uiso 1 1 calc R U . . .
C22 C -0.3394(10) 0.2868(9) 0.5408(8) 0.048(3) Uani 1 1 d . . . . .
H22A H -0.4051 0.2618 0.5523 0.058 Uiso 1 1 calc R U . . .
H22B H -0.3499 0.3557 0.5189 0.058 Uiso 1 1 calc R U . . .
C23 C -0.2455(13) 0.2716(11) 0.3940(8) 0.070(4) Uani 1 1 d . . . . .
H23A H -0.1759 0.2490 0.3640 0.105 Uiso 1 1 calc R U . . .
H23B H -0.2579 0.3395 0.3699 0.105 Uiso 1 1 calc R U . . .
H23C H -0.2981 0.2425 0.3888 0.105 Uiso 1 1 calc R U . . .
C24 C 0.0080(7) 0.7366(7) 0.2843(6) 0.027(2) Uani 1 1 d . . . . .
H24 H -0.0319 0.7930 0.2619 0.032 Uiso 1 1 calc R U . . .
C25 C -0.0130(8) 0.6980(7) 0.3720(6) 0.032(2) Uani 1 1 d . . . . .
H25 H -0.0646 0.7293 0.4075 0.038 Uiso 1 1 calc R U . . .
C26 C 0.0409(8) 0.6156(7) 0.4057(6) 0.033(2) Uani 1 1 d . . . . .
H26 H 0.0274 0.5891 0.4647 0.040 Uiso 1 1 calc R U . . .
C27 C 0.1169(8) 0.5698(7) 0.3522(6) 0.028(2) Uani 1 1 d . . . . .
C28 C 0.1364(7) 0.6153(6) 0.2653(6) 0.0245(19) Uani 1 1 d . . . . .
C29 C 0.2170(7) 0.5750(6) 0.2082(6) 0.0253(19) Uani 1 1 d . . . . .
C30 C 0.2739(8) 0.4915(7) 0.2376(6) 0.031(2) Uani 1 1 d . . . . .
C31 C 0.2498(9) 0.4437(7) 0.3261(6) 0.034(2) Uani 1 1 d . . . . .
H31 H 0.2851 0.3837 0.3463 0.041 Uiso 1 1 calc R U . . .
C32 C 0.1779(9) 0.4830(7) 0.3807(6) 0.034(2) Uani 1 1 d . . . . .
H32 H 0.1672 0.4528 0.4391 0.041 Uiso 1 1 calc R U . . .
C33 C 0.3519(8) 0.4559(7) 0.1771(7) 0.033(2) Uani 1 1 d . . . . .
H33 H 0.3930 0.3982 0.1940 0.039 Uiso 1 1 calc R U . . .
C34 C 0.3672(8) 0.5050(6) 0.0945(6) 0.030(2) Uani 1 1 d . . . . .
H34 H 0.4190 0.4813 0.0535 0.037 Uiso 1 1 calc R U . . .
C35 C 0.3074(8) 0.5900(7) 0.0695(6) 0.030(2) Uani 1 1 d . . . . .
H35 H 0.3200 0.6236 0.0115 0.036 Uiso 1 1 calc R U . . .
C36 C -0.0472(8) 0.6466(6) 0.1393(6) 0.027(2) Uani 1 1 d . . . . .
H36 H -0.0653 0.6420 0.1967 0.032 Uiso 1 1 calc R U . . .
C37 C -0.1113(8) 0.6119(7) 0.1131(6) 0.030(2) Uani 1 1 d . . . . .
H37 H -0.1725 0.5863 0.1524 0.036 Uiso 1 1 calc R U . . .
C38 C -0.0864(8) 0.6145(7) 0.0312(6) 0.031(2) Uani 1 1 d . . . . .
H38 H -0.1290 0.5904 0.0131 0.037 Uiso 1 1 calc R U . . .
C39 C 0.0055(8) 0.6545(7) -0.0259(6) 0.030(2) Uani 1 1 d . . . . .
C40 C 0.0632(8) 0.6908(6) 0.0038(6) 0.025(2) Uani 1 1 d . . . . .
C41 C 0.1519(7) 0.7348(6) -0.0496(6) 0.0249(19) Uani 1 1 d . . . . .
C42 C 0.1881(8) 0.7407(6) -0.1352(6) 0.028(2) Uani 1 1 d . . . . .
C43 C 0.1285(9) 0.7000(7) -0.1643(6) 0.036(2) Uani 1 1 d . . . . .
H43 H 0.1517 0.7005 -0.2209 0.043 Uiso 1 1 calc R U . . .
C44 C 0.0407(9) 0.6613(7) -0.1128(6) 0.035(2) Uani 1 1 d . . . . .
H44 H 0.0016 0.6382 -0.1347 0.043 Uiso 1 1 calc R U . . .
C45 C 0.2781(9) 0.7838(7) -0.1842(6) 0.036(2) Uani 1 1 d . . . . .
H45 H 0.3053 0.7886 -0.2419 0.043 Uiso 1 1 calc R U . . .
C46 C 0.3267(8) 0.8189(7) -0.1483(6) 0.036(2) Uani 1 1 d . . . . .
H46 H 0.3889 0.8470 -0.1807 0.044 Uiso 1 1 calc R U . . .
C47 C 0.2853(8) 0.8137(7) -0.0642(6) 0.029(2) Uani 1 1 d . . . . .
H47 H 0.3191 0.8405 -0.0411 0.035 Uiso 1 1 calc R U . . .
C48 C -0.0548(8) 0.8834(7) 0.0880(6) 0.030(2) Uani 1 1 d . . . . .
H48 H -0.0773 0.8445 0.0681 0.036 Uiso 1 1 calc R U . . .
C49 C -0.1203(8) 0.9618(7) 0.1023(7) 0.035(2) Uani 1 1 d . . . . .
H49 H -0.1863 0.9760 0.0917 0.042 Uiso 1 1 calc R U . . .
C50 C -0.0901(8) 1.0193(7) 0.1318(7) 0.036(2) Uani 1 1 d . . . . .
H50 H -0.1361 1.0715 0.1436 0.044 Uiso 1 1 calc R U . . .
C51 C 0.0089(8) 0.9999(7) 0.1439(6) 0.033(2) Uani 1 1 d . . . . .
C52 C 0.0711(8) 0.9212(6) 0.1269(6) 0.026(2) Uani 1 1 d . . . . .
C53 C 0.1712(7) 0.8954(6) 0.1401(5) 0.0232(19) Uani 1 1 d . . . . .
C54 C 0.2098(8) 0.9510(6) 0.1683(5) 0.026(2) Uani 1 1 d . . . . .
C55 C 0.1463(8) 1.0313(7) 0.1851(6) 0.033(2) Uani 1 1 d . . . . .
H55 H 0.1718 1.0690 0.2044 0.040 Uiso 1 1 calc R U . . .
C56 C 0.0483(9) 1.0553(7) 0.1740(7) 0.036(2) Uani 1 1 d . . . . .
H56 H 0.0063 1.1090 0.1863 0.043 Uiso 1 1 calc R U . . .
C57 C 0.3109(8) 0.9221(7) 0.1779(6) 0.029(2) Uani 1 1 d . . . . .
H57 H 0.3403 0.9571 0.1971 0.035 Uiso 1 1 calc R U . . .
C58 C 0.3670(7) 0.8435(7) 0.1596(6) 0.028(2) Uani 1 1 d . . . . .
H58 H 0.4361 0.8248 0.1641 0.034 Uiso 1 1 calc R U . . .
C59 C 0.3209(7) 0.7909(6) 0.1339(6) 0.026(2) Uani 1 1 d . . . . .
H59 H 0.3597 0.7356 0.1231 0.032 Uiso 1 1 calc R U . . .
O22 O 0.4275(9) 0.8356(8) 0.6283(7) 0.082(3) Uani 1 1 d . . . . .
N9 N 0.5952(13) 0.8685(14) 0.5782(9) 0.103(6) Uani 1 1 d . . . . .
C60 C 0.5054(12) 0.8555(11) 0.5704(11) 0.068(4) Uani 1 1 d . . . . .
C61 C 0.5198(14) 0.8737(11) 0.4780(9) 0.073(4) Uani 1 1 d . . . . .
H61A H 0.4675 0.9245 0.4579 0.087 Uiso 1 1 calc R U . . .
H61B H 0.5127 0.8169 0.4682 0.087 Uiso 1 1 calc R U . . .
C62 C 0.6334(13) 0.9024(14) 0.4321(12) 0.084(5) Uani 1 1 d . . . . .
H62A H 0.6736 0.8638 0.3956 0.100 Uiso 1 1 calc R U . . .
H62B H 0.6310 0.9688 0.3972 0.100 Uiso 1 1 calc R U . . .
C63 C 0.6831(16) 0.886(2) 0.5004(12) 0.118(8) Uani 1 1 d . . . . .
H63A H 0.7374 0.8318 0.5027 0.141 Uiso 1 1 calc R U . . .
H63B H 0.7150 0.9418 0.4914 0.141 Uiso 1 1 calc R U . . .
C64 C 0.611(2) 0.852(2) 0.6573(13) 0.138(9) Uani 1 1 d . U . . .
H64A H 0.6429 0.7878 0.6770 0.207 Uiso 1 1 calc R U . . .
H64B H 0.5435 0.8612 0.6979 0.207 Uiso 1 1 calc R U . . .
H64C H 0.6567 0.8955 0.6515 0.207 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.769(7) . ?
U1 O2 1.770(7) . ?
U1 O16 2.458(6) 1_546 ?
U1 O6 2.459(6) . ?
U1 O11 2.467(6) . ?
U1 O10 2.475(6) . ?
U1 O7 2.481(6) . ?
U1 O17 2.518(6) 1_546 ?
U2 O4 1.754(7) . ?
U2 O3 1.766(7) . ?
U2 O8 2.436(6) . ?
U2 O12 2.462(6) 1_654 ?
U2 O14 2.474(6) . ?
U2 O9 2.500(6) . ?
U2 O15 2.505(6) . ?
U2 O13 2.531(6) 1_654 ?
U3 O5 1.763(9) . ?
U3 O5 1.763(9) 2_556 ?
U3 O21 2.340(9) 2_556 ?
U3 O21 2.340(9) . ?
U3 O18 2.526(13) . ?
U3 O18 2.526(13) 2_556 ?
U3 O19 2.527(11) 2_556 ?
U3 O19 2.528(11) . ?
Fe1 N6 1.963(7) . ?
Fe1 N5 1.965(8) . ?
Fe1 N7 1.981(8) . ?
Fe1 N8 1.982(8) . ?
Fe1 N4 1.990(8) . ?
Fe1 N3 1.990(8) . ?
S1 C2 1.715(9) . ?
S1 C5 1.715(9) . ?
S2 C11 1.716(9) . ?
S2 C8 1.720(9) . ?
S3 C14 1.719(9) . ?
S3 C17 1.728(9) . ?
O6 C1 1.278(11) . ?
O7 C1 1.269(11) . ?
O8 C6 1.267(11) . ?
O9 C6 1.258(11) . ?
O10 C7 1.270(11) . ?
O11 C7 1.256(11) . ?
O12 C12 1.269(11) . ?
O12 U2 2.462(6) 1_456 ?
O13 C12 1.257(11) . ?
O13 U2 2.531(6) 1_456 ?
O14 C13 1.280(11) . ?
O15 C13 1.248(11) . ?
O16 C18 1.266(11) . ?
O16 U1 2.458(6) 1_564 ?
O17 C18 1.255(11) . ?
O17 U1 2.518(6) 1_564 ?
O18 N1 1.284(15) . ?
O19 N1 1.255(16) . ?
O20 N1 1.216(15) . ?
O21 C19 1.253(14) . ?
N2 C19 1.322(15) . ?
N2 C23 1.458(16) . ?
N2 C22 1.477(16) . ?
N3 C24 1.339(12) . ?
N3 C28 1.364(12) . ?
N4 C35 1.349(12) . ?
N4 C29 1.370(12) . ?
N5 C36 1.335(12) . ?
N5 C40 1.387(11) . ?
N6 C47 1.346(12) . ?
N6 C41 1.368(12) . ?
N7 C48 1.350(13) . ?
N7 C52 1.371(12) . ?
N8 C59 1.323(12) . ?
N8 C53 1.380(11) . ?
C1 C2 1.466(12) . ?
C2 C3 1.369(13) . ?
C3 C4 1.397(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.367(13) . ?
C4 H4 0.9500 . ?
C5 C6 1.475(12) . ?
C7 C8 1.468(13) . ?
C8 C9 1.368(13) . ?
C9 C10 1.394(13) . ?
C9 H9 0.9500 . ?
C10 C11 1.375(13) . ?
C10 H10 0.9500 . ?
C11 C12 1.476(13) . ?
C13 C14 1.473(13) . ?
C14 C15 1.388(13) . ?
C15 C16 1.416(12) . ?
C15 H15 0.9500 . ?
C16 C17 1.361(13) . ?
C16 H16 0.9500 . ?
C17 C18 1.480(12) . ?
C19 C20 1.475(18) . ?
C20 C21 1.537(18) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.513(19) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.409(13) . ?
C24 H24 0.9500 . ?
C25 C26 1.364(15) . ?
C25 H25 0.9500 . ?
C26 C27 1.410(14) . ?
C26 H26 0.9500 . ?
C27 C28 1.409(13) . ?
C27 C32 1.433(14) . ?
C28 C29 1.429(13) . ?
C29 C30 1.374(13) . ?
C30 C33 1.415(14) . ?
C30 C31 1.437(14) . ?
C31 C32 1.344(15) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C34 1.358(14) . ?
C33 H33 0.9500 . ?
C34 C35 1.394(14) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.401(13) . ?
C36 H36 0.9500 . ?
C37 C38 1.375(14) . ?
C37 H37 0.9500 . ?
C38 C39 1.426(14) . ?
C38 H38 0.9500 . ?
C39 C40 1.389(13) . ?
C39 C44 1.433(14) . ?
C40 C41 1.402(13) . ?
C41 C42 1.413(12) . ?
C42 C45 1.397(15) . ?
C42 C43 1.450(15) . ?
C43 C44 1.352(15) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 C46 1.367(15) . ?
C45 H45 0.9500 . ?
C46 C47 1.392(14) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C48 C49 1.389(14) . ?
C48 H48 0.9500 . ?
C49 C50 1.380(15) . ?
C49 H49 0.9500 . ?
C50 C51 1.399(15) . ?
C50 H50 0.9500 . ?
C51 C52 1.392(13) . ?
C51 C56 1.438(14) . ?
C52 C53 1.418(13) . ?
C53 C54 1.408(13) . ?
C54 C57 1.409(14) . ?
C54 C55 1.417(13) . ?
C55 C56 1.375(15) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 C58 1.373(14) . ?
C57 H57 0.9500 . ?
C58 C59 1.408(13) . ?
C58 H58 0.9500 . ?
C59 H59 0.9500 . ?
O22 C60 1.214(18) . ?
N9 C60 1.35(2) . ?
N9 C64 1.42(2) . ?
N9 C63 1.48(2) . ?
C60 C61 1.52(2) . ?
C61 C62 1.58(2) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 C63 1.51(3) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 178.6(3) . . ?
O1 U1 O16 87.5(3) . 1_546 ?
O2 U1 O16 92.0(3) . 1_546 ?
O1 U1 O6 89.9(3) . . ?
O2 U1 O6 89.2(3) . . ?
O16 U1 O6 121.7(2) 1_546 . ?
O1 U1 O11 90.8(3) . . ?
O2 U1 O11 90.2(3) . . ?
O16 U1 O11 66.4(2) 1_546 . ?
O6 U1 O11 171.9(2) . . ?
O1 U1 O10 93.1(3) . . ?
O2 U1 O10 88.3(3) . . ?
O16 U1 O10 118.9(2) 1_546 . ?
O6 U1 O10 119.4(2) . . ?
O11 U1 O10 52.5(2) . . ?
O1 U1 O7 87.1(3) . . ?
O2 U1 O7 93.2(3) . . ?
O16 U1 O7 172.5(2) 1_546 . ?
O6 U1 O7 53.0(2) . . ?
O11 U1 O7 119.0(2) . . ?
O10 U1 O7 66.7(2) . . ?
O1 U1 O17 89.2(3) . 1_546 ?
O2 U1 O17 89.5(3) . 1_546 ?
O16 U1 O17 52.1(2) 1_546 1_546 ?
O6 U1 O17 69.7(2) . 1_546 ?
O11 U1 O17 118.4(2) . 1_546 ?
O10 U1 O17 170.6(2) . 1_546 ?
O7 U1 O17 122.5(2) . 1_546 ?
O4 U2 O3 179.9(3) . . ?
O4 U2 O8 86.1(3) . . ?
O3 U2 O8 93.9(3) . . ?
O4 U2 O12 89.5(3) . 1_654 ?
O3 U2 O12 90.4(3) . 1_654 ?
O8 U2 O12 118.7(2) . 1_654 ?
O4 U2 O14 91.0(3) . . ?
O3 U2 O14 89.0(3) . . ?
O8 U2 O14 123.2(2) . . ?
O12 U2 O14 118.1(2) 1_654 . ?
O4 U2 O9 95.1(3) . . ?
O3 U2 O9 85.0(3) . . ?
O8 U2 O9 52.8(2) . . ?
O12 U2 O9 169.8(2) 1_654 . ?
O14 U2 O9 71.1(2) . . ?
O4 U2 O15 88.4(3) . . ?
O3 U2 O15 91.5(3) . . ?
O8 U2 O15 173.0(2) . . ?
O12 U2 O15 65.7(2) 1_654 . ?
O14 U2 O15 52.4(2) . . ?
O9 U2 O15 123.5(2) . . ?
O4 U2 O13 91.2(3) . 1_654 ?
O3 U2 O13 88.7(3) . 1_654 ?
O8 U2 O13 66.8(2) . 1_654 ?
O12 U2 O13 52.1(2) 1_654 1_654 ?
O14 U2 O13 169.9(2) . 1_654 ?
O9 U2 O13 118.5(2) . 1_654 ?
O15 U2 O13 117.9(2) . 1_654 ?
O5 U3 O5 180.0 . 2_556 ?
O5 U3 O21 86.4(4) . 2_556 ?
O5 U3 O21 93.6(4) 2_556 2_556 ?
O5 U3 O21 93.6(4) . . ?
O5 U3 O21 86.4(4) 2_556 . ?
O21 U3 O21 180.0 2_556 . ?
O5 U3 O18 94.2(5) . . ?
O5 U3 O18 85.8(5) 2_556 . ?
O21 U3 O18 64.6(3) 2_556 . ?
O21 U3 O18 115.4(3) . . ?
O5 U3 O18 85.8(5) . 2_556 ?
O5 U3 O18 94.2(5) 2_556 2_556 ?
O21 U3 O18 115.4(3) 2_556 2_556 ?
O21 U3 O18 64.6(3) . 2_556 ?
O18 U3 O18 180.0 . 2_556 ?
O5 U3 O19 92.3(5) . 2_556 ?
O5 U3 O19 87.7(5) 2_556 2_556 ?
O21 U3 O19 66.7(3) 2_556 2_556 ?
O21 U3 O19 113.3(3) . 2_556 ?
O18 U3 O19 130.3(3) . 2_556 ?
O18 U3 O19 49.7(3) 2_556 2_556 ?
O5 U3 O19 87.7(5) . . ?
O5 U3 O19 92.3(5) 2_556 . ?
O21 U3 O19 113.3(3) 2_556 . ?
O21 U3 O19 66.7(3) . . ?
O18 U3 O19 49.7(3) . . ?
O18 U3 O19 130.3(3) 2_556 . ?
O19 U3 O19 180.0 2_556 . ?
N6 Fe1 N5 83.2(3) . . ?
N6 Fe1 N7 96.3(3) . . ?
N5 Fe1 N7 91.4(3) . . ?
N6 Fe1 N8 96.3(3) . . ?
N5 Fe1 N8 174.2(3) . . ?
N7 Fe1 N8 82.8(3) . . ?
N6 Fe1 N4 89.6(3) . . ?
N5 Fe1 N4 91.9(3) . . ?
N7 Fe1 N4 173.5(3) . . ?
N8 Fe1 N4 93.9(3) . . ?
N6 Fe1 N3 171.9(3) . . ?
N5 Fe1 N3 94.8(3) . . ?
N7 Fe1 N3 91.6(3) . . ?
N8 Fe1 N3 86.4(3) . . ?
N4 Fe1 N3 82.6(3) . . ?
C2 S1 C5 91.2(4) . . ?
C11 S2 C8 91.2(4) . . ?
C14 S3 C17 91.4(4) . . ?
C1 O6 U1 93.9(5) . . ?
C1 O7 U1 93.2(5) . . ?
C6 O8 U2 94.7(5) . . ?
C6 O9 U2 91.9(5) . . ?
C7 O10 U1 93.4(5) . . ?
C7 O11 U1 94.1(6) . . ?
C12 O12 U2 94.9(5) . 1_456 ?
C12 O13 U2 92.0(5) . 1_456 ?
C13 O14 U2 93.7(5) . . ?
C13 O15 U2 93.1(5) . . ?
C18 O16 U1 95.1(5) . 1_564 ?
C18 O17 U1 92.5(5) . 1_564 ?
N1 O18 U3 98.0(9) . . ?
N1 O19 U3 98.8(8) . . ?
C19 O21 U3 140.3(8) . . ?
O20 N1 O19 123.2(13) . . ?
O20 N1 O18 123.3(15) . . ?
O19 N1 O18 113.5(13) . . ?
O20 N1 U3 178.2(11) . . ?
C19 N2 C23 123.1(11) . . ?
C19 N2 C22 114.1(10) . . ?
C23 N2 C22 122.5(11) . . ?
C24 N3 C28 117.2(8) . . ?
C24 N3 Fe1 130.3(6) . . ?
C28 N3 Fe1 112.3(6) . . ?
C35 N4 C29 116.8(8) . . ?
C35 N4 Fe1 130.2(7) . . ?
C29 N4 Fe1 113.0(6) . . ?
C36 N5 C40 117.2(8) . . ?
C36 N5 Fe1 130.5(6) . . ?
C40 N5 Fe1 112.2(6) . . ?
C47 N6 C41 117.4(8) . . ?
C47 N6 Fe1 129.8(7) . . ?
C41 N6 Fe1 112.5(6) . . ?
C48 N7 C52 117.2(8) . . ?
C48 N7 Fe1 129.9(6) . . ?
C52 N7 Fe1 112.3(6) . . ?
C59 N8 C53 117.3(8) . . ?
C59 N8 Fe1 130.7(6) . . ?
C53 N8 Fe1 111.2(6) . . ?
O7 C1 O6 119.7(8) . . ?
O7 C1 C2 120.0(8) . . ?
O6 C1 C2 120.3(8) . . ?
C3 C2 C1 127.7(8) . . ?
C3 C2 S1 111.9(7) . . ?
C1 C2 S1 120.2(7) . . ?
C2 C3 C4 112.3(9) . . ?
C2 C3 H3 123.9 . . ?
C4 C3 H3 123.9 . . ?
C5 C4 C3 113.0(8) . . ?
C5 C4 H4 123.5 . . ?
C3 C4 H4 123.5 . . ?
C4 C5 C6 129.0(8) . . ?
C4 C5 S1 111.6(7) . . ?
C6 C5 S1 119.4(7) . . ?
O9 C6 O8 120.6(8) . . ?
O9 C6 C5 121.1(8) . . ?
O8 C6 C5 118.2(8) . . ?
O11 C7 O10 119.9(8) . . ?
O11 C7 C8 120.2(8) . . ?
O10 C7 C8 119.9(8) . . ?
C9 C8 C7 128.9(8) . . ?
C9 C8 S2 111.1(7) . . ?
C7 C8 S2 120.0(7) . . ?
C8 C9 C10 113.9(8) . . ?
C8 C9 H9 123.1 . . ?
C10 C9 H9 123.1 . . ?
C11 C10 C9 111.6(8) . . ?
C11 C10 H10 124.2 . . ?
C9 C10 H10 124.2 . . ?
C10 C11 C12 129.2(8) . . ?
C10 C11 S2 112.2(7) . . ?
C12 C11 S2 118.5(7) . . ?
O13 C12 O12 120.7(9) . . ?
O13 C12 C11 121.2(8) . . ?
O12 C12 C11 118.1(8) . . ?
O15 C13 O14 120.8(9) . . ?
O15 C13 C14 120.7(8) . . ?
O14 C13 C14 118.5(8) . . ?
C15 C14 C13 127.6(8) . . ?
C15 C14 S3 111.8(7) . . ?
C13 C14 S3 120.6(7) . . ?
C14 C15 C16 111.8(8) . . ?
C14 C15 H15 124.1 . . ?
C16 C15 H15 124.1 . . ?
C17 C16 C15 113.1(8) . . ?
C17 C16 H16 123.5 . . ?
C15 C16 H16 123.5 . . ?
C16 C17 C18 129.4(8) . . ?
C16 C17 S3 111.9(7) . . ?
C18 C17 S3 118.4(7) . . ?
O17 C18 O16 120.3(8) . . ?
O17 C18 C17 121.0(8) . . ?
O16 C18 C17 118.7(8) . . ?
O21 C19 N2 123.4(12) . . ?
O21 C19 C20 126.3(12) . . ?
N2 C19 C20 110.2(11) . . ?
C19 C20 C21 103.7(11) . . ?
C19 C20 H20A 111.0 . . ?
C21 C20 H20A 111.0 . . ?
C19 C20 H20B 111.0 . . ?
C21 C20 H20B 111.0 . . ?
H20A C20 H20B 109.0 . . ?
C22 C21 C20 106.0(11) . . ?
C22 C21 H21A 110.5 . . ?
C20 C21 H21A 110.5 . . ?
C22 C21 H21B 110.5 . . ?
C20 C21 H21B 110.5 . . ?
H21A C21 H21B 108.7 . . ?
N2 C22 C21 101.9(10) . . ?
N2 C22 H22A 111.4 . . ?
C21 C22 H22A 111.4 . . ?
N2 C22 H22B 111.4 . . ?
C21 C22 H22B 111.4 . . ?
H22A C22 H22B 109.3 . . ?
N2 C23 H23A 109.5 . . ?
N2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N3 C24 C25 122.8(9) . . ?
N3 C24 H24 118.6 . . ?
C25 C24 H24 118.6 . . ?
C26 C25 C24 119.7(9) . . ?
C26 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
C25 C26 C27 119.5(9) . . ?
C25 C26 H26 120.2 . . ?
C27 C26 H26 120.2 . . ?
C28 C27 C26 117.1(9) . . ?
C28 C27 C32 118.6(9) . . ?
C26 C27 C32 124.2(9) . . ?
N3 C28 C27 123.6(9) . . ?
N3 C28 C29 116.9(8) . . ?
C27 C28 C29 119.6(8) . . ?
N4 C29 C30 124.5(9) . . ?
N4 C29 C28 115.1(8) . . ?
C30 C29 C28 120.4(9) . . ?
C29 C30 C33 117.0(9) . . ?
C29 C30 C31 119.4(9) . . ?
C33 C30 C31 123.5(9) . . ?
C32 C31 C30 120.7(9) . . ?
C32 C31 H31 119.6 . . ?
C30 C31 H31 119.6 . . ?
C31 C32 C27 121.1(9) . . ?
C31 C32 H32 119.5 . . ?
C27 C32 H32 119.5 . . ?
C34 C33 C30 119.3(9) . . ?
C34 C33 H33 120.3 . . ?
C30 C33 H33 120.3 . . ?
C33 C34 C35 120.4(9) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
N4 C35 C34 122.0(9) . . ?
N4 C35 H35 119.0 . . ?
C34 C35 H35 119.0 . . ?
N5 C36 C37 122.9(9) . . ?
N5 C36 H36 118.6 . . ?
C37 C36 H36 118.6 . . ?
C38 C37 C36 120.6(9) . . ?
C38 C37 H37 119.7 . . ?
C36 C37 H37 119.7 . . ?
C37 C38 C39 117.9(9) . . ?
C37 C38 H38 121.1 . . ?
C39 C38 H38 121.1 . . ?
C40 C39 C38 118.4(9) . . ?
C40 C39 C44 117.9(9) . . ?
C38 C39 C44 123.6(9) . . ?
N5 C40 C39 123.0(9) . . ?
N5 C40 C41 115.5(8) . . ?
C39 C40 C41 121.5(8) . . ?
N6 C41 C40 116.3(8) . . ?
N6 C41 C42 122.6(9) . . ?
C40 C41 C42 121.0(9) . . ?
C45 C42 C41 117.9(9) . . ?
C45 C42 C43 125.5(9) . . ?
C41 C42 C43 116.6(9) . . ?
C44 C43 C42 121.6(9) . . ?
C44 C43 H43 119.2 . . ?
C42 C43 H43 119.2 . . ?
C43 C44 C39 121.3(10) . . ?
C43 C44 H44 119.4 . . ?
C39 C44 H44 119.4 . . ?
C46 C45 C42 119.2(9) . . ?
C46 C45 H45 120.4 . . ?
C42 C45 H45 120.4 . . ?
C45 C46 C47 120.2(10) . . ?
C45 C46 H46 119.9 . . ?
C47 C46 H46 119.9 . . ?
N6 C47 C46 122.6(10) . . ?
N6 C47 H47 118.7 . . ?
C46 C47 H47 118.7 . . ?
N7 C48 C49 121.7(9) . . ?
N7 C48 H48 119.1 . . ?
C49 C48 H48 119.1 . . ?
C50 C49 C48 120.5(10) . . ?
C50 C49 H49 119.8 . . ?
C48 C49 H49 119.8 . . ?
C49 C50 C51 119.3(10) . . ?
C49 C50 H50 120.4 . . ?
C51 C50 H50 120.4 . . ?
C52 C51 C50 117.1(9) . . ?
C52 C51 C56 119.0(10) . . ?
C50 C51 C56 123.9(10) . . ?
N7 C52 C51 124.1(9) . . ?
N7 C52 C53 115.4(8) . . ?
C51 C52 C53 120.4(9) . . ?
N8 C53 C54 123.4(9) . . ?
N8 C53 C52 116.5(8) . . ?
C54 C53 C52 120.1(8) . . ?
C53 C54 C57 116.8(9) . . ?
C53 C54 C55 119.2(9) . . ?
C57 C54 C55 124.0(9) . . ?
C56 C55 C54 120.7(9) . . ?
C56 C55 H55 119.6 . . ?
C54 C55 H55 119.6 . . ?
C55 C56 C51 120.5(9) . . ?
C55 C56 H56 119.7 . . ?
C51 C56 H56 119.7 . . ?
C58 C57 C54 119.9(9) . . ?
C58 C57 H57 120.0 . . ?
C54 C57 H57 120.0 . . ?
C57 C58 C59 119.2(9) . . ?
C57 C58 H58 120.4 . . ?
C59 C58 H58 120.4 . . ?
N8 C59 C58 123.3(9) . . ?
N8 C59 H59 118.4 . . ?
C58 C59 H59 118.4 . . ?
C60 N9 C64 122.8(18) . . ?
C60 N9 C63 115.6(15) . . ?
C64 N9 C63 120.9(19) . . ?
O22 C60 N9 124.3(17) . . ?
O22 C60 C61 127.7(16) . . ?
N9 C60 C61 108.0(14) . . ?
C60 C61 C62 105.1(14) . . ?
C60 C61 H61A 110.7 . . ?
C62 C61 H61A 110.7 . . ?
C60 C61 H61B 110.7 . . ?
C62 C61 H61B 110.7 . . ?
H61A C61 H61B 108.8 . . ?
C63 C62 C61 106.1(15) . . ?
C63 C62 H62A 110.5 . . ?
C61 C62 H62A 110.5 . . ?
C63 C62 H62B 110.5 . . ?
C61 C62 H62B 110.5 . . ?
H62A C62 H62B 108.7 . . ?
N9 C63 C62 104.0(16) . . ?
N9 C63 H63A 111.0 . . ?
C62 C63 H63A 111.0 . . ?
N9 C63 H63B 111.0 . . ?
C62 C63 H63B 111.0 . . ?
H63A C63 H63B 109.0 . . ?
N9 C64 H64A 109.5 . . ?
N9 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
N9 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?

_refine_diff_density_max         1.489
_refine_diff_density_min         -6.563
_refine_diff_density_rms         0.235

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1437897'
_audit_update_record             
;
2015-11-19 deposited with the CCDC.
2016-01-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C123 H87 N17 Ni2 O43 S6 U5'
_chemical_formula_weight         3991.02

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   13.7804(3)
_cell_length_b                   15.5944(3)
_cell_length_c                   18.0932(4)
_cell_angle_alpha                67.6388(9)
_cell_angle_beta                 69.3880(9)
_cell_angle_gamma                76.7394(11)
_cell_volume                     3345.09(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    211033
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light pink'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.981
_exptl_crystal_F_000             1900
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    6.488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.402
_exptl_absorpt_correction_T_max  0.678
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 30 mm'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'2 φ and 16 ω scans with 1° steps (1646 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            211033
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.992
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             12668
_reflns_number_gt                11466
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. The NMP solvent molecule has been given an occupancy factor
 of 0.5 in order to retain acceptable displacement parameters. All
 non-hydrogen atoms were refined with anisotropic displacement parameters,
 with restraints on bond lengths and displacement parameters for the atoms
 of the solvent NMP molecule. The H atoms were introduced at calculated
 positions and were treated as riding atoms with an isotropic displacement
 parameter equal to 1.2 times that of the parent atom (1.5 for CH₃, with
 optimized geometry). The largest negative residual electron density is
 located near atom U3, as a result of imperfect absorption corrections
 and/or of unresolved disorder on this group, as suggested by the large
 displacement parameters of U3 and its ligands. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0777P)²+77.8864P] 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         12668
_refine_ls_number_parameters     918
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0685
_refine_ls_wR_factor_ref         0.1898
_refine_ls_wR_factor_gt          0.1862
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.36668(3) 0.24738(3) 1.06867(3) 0.02697(13) Uani 1 1 d . . . . .
U2 U 0.69748(3) 0.58964(3) 0.41398(3) 0.02899(13) Uani 1 1 d . . . . .
U3 U 0.0000 0.0000 0.5000 0.0895(4) Uani 1 2 d S . P . .
Ni1 Ni 0.13534(12) 0.74525(11) 0.10647(10) 0.0313(3) Uani 1 1 d . . . . .
S1 S 0.5239(2) 0.41678(19) 0.73803(17) 0.0305(6) Uani 1 1 d . . . . .
S2 S 0.0389(2) 0.4222(2) 1.24700(17) 0.0298(6) Uani 1 1 d . . . . .
S3 S 0.5419(2) 0.9226(2) 0.23594(18) 0.0323(6) Uani 1 1 d . . . . .
O1 O 0.4574(7) 0.3002(6) 1.0830(6) 0.0350(19) Uani 1 1 d . . . . .
O2 O 0.2800(6) 0.1926(6) 1.0533(5) 0.0331(18) Uani 1 1 d . . . . .
O3 O 0.7706(7) 0.6546(6) 0.4331(6) 0.040(2) Uani 1 1 d . . . . .
O4 O 0.6240(7) 0.5243(6) 0.3957(6) 0.040(2) Uani 1 1 d . . . . .
O5 O 0.1008(12) 0.0455(10) 0.4099(11) 0.108(6) Uani 1 1 d . U . . .
O6 O 0.4557(6) 0.2961(6) 0.9177(5) 0.0330(19) Uani 1 1 d . . . . .
O7 O 0.3323(6) 0.3980(6) 0.9630(5) 0.0353(19) Uani 1 1 d . . . . .
O8 O 0.6432(6) 0.4918(6) 0.5600(5) 0.0332(18) Uani 1 1 d . . . . .
O9 O 0.5524(7) 0.6287(6) 0.5297(5) 0.037(2) Uani 1 1 d . . . . .
O10 O 0.2142(6) 0.3479(6) 1.1258(5) 0.0328(18) Uani 1 1 d . . . . .
O11 O 0.2617(7) 0.2200(6) 1.2168(5) 0.041(2) Uani 1 1 d . . . . .
O12 O -0.1440(7) 0.5359(7) 1.3184(5) 0.045(2) Uani 1 1 d . . . . .
O13 O -0.1741(7) 0.4494(6) 1.4504(5) 0.039(2) Uani 1 1 d . . . . .
O14 O 0.5941(6) 0.7359(6) 0.3554(5) 0.037(2) Uani 1 1 d . . . . .
O15 O 0.7289(7) 0.6905(6) 0.2645(5) 0.040(2) Uani 1 1 d . . . . .
O16 O 0.4247(6) 1.1007(5) 0.1653(5) 0.0333(18) Uani 1 1 d . . . . .
O17 O 0.5101(6) 1.1248(5) 0.0328(5) 0.0327(18) Uani 1 1 d . . . . .
O18 O 0.0996(19) -0.0289(14) 0.6050(13) 0.133(7) Uani 1 1 d . . . . .
O19 O 0.0243(16) 0.1076(12) 0.5694(15) 0.123(7) Uani 1 1 d . . . . .
O20 O 0.118(2) 0.0743(17) 0.652(2) 0.187(12) Uani 1 1 d . . . . .
O21 O -0.1100(11) 0.1407(10) 0.4781(9) 0.085(4) Uani 1 1 d . . . . .
N1 N 0.086(2) 0.0538(19) 0.602(2) 0.136(11) Uani 1 1 d . . . . .
N2 N -0.2530(13) 0.2466(11) 0.4841(10) 0.070(4) Uani 1 1 d . . . . .
N3 N 0.0817(8) 0.6899(8) 0.2377(7) 0.038(2) Uani 1 1 d . . . . .
N4 N 0.2370(8) 0.6210(7) 0.1277(6) 0.031(2) Uani 1 1 d . . . . .
N5 N 0.0323(8) 0.6869(7) 0.0834(6) 0.031(2) Uani 1 1 d . . . . .
N6 N 0.2021(8) 0.7716(7) -0.0222(6) 0.034(2) Uani 1 1 d . . . . .
N7 N 0.0339(8) 0.8685(7) 0.1035(7) 0.037(2) Uani 1 1 d . . . . .
N8 N 0.2249(8) 0.8249(7) 0.1222(6) 0.033(2) Uani 1 1 d . . . . .
C1 C 0.4060(8) 0.3771(8) 0.9030(7) 0.029(2) Uani 1 1 d . . . . .
C2 C 0.4317(9) 0.4460(8) 0.8210(7) 0.030(2) Uani 1 1 d . . . . .
C3 C 0.3947(10) 0.5398(9) 0.7966(8) 0.042(3) Uani 1 1 d . . . . .
H3 H 0.3444 0.5699 0.8332 0.050 Uiso 1 1 calc R U . . .
C4 C 0.4407(10) 0.5851(9) 0.7112(7) 0.038(3) Uani 1 1 d . . . . .
H4 H 0.4243 0.6494 0.6836 0.045 Uiso 1 1 calc R U . . .
C5 C 0.5104(9) 0.5282(8) 0.6723(7) 0.030(2) Uani 1 1 d . . . . .
C6 C 0.5707(9) 0.5498(9) 0.5834(8) 0.033(3) Uani 1 1 d . . . . .
C7 C 0.2012(9) 0.2947(8) 1.2013(7) 0.031(2) Uani 1 1 d . . . . .
C8 C 0.1186(9) 0.3197(8) 1.2688(8) 0.031(2) Uani 1 1 d . . . . .
C9 C 0.0943(11) 0.2722(9) 1.3522(8) 0.041(3) Uani 1 1 d . . . . .
H9 H 0.1313 0.2145 1.3758 0.049 Uiso 1 1 calc R U . . .
C10 C 0.0092(10) 0.3163(8) 1.4006(8) 0.036(3) Uani 1 1 d . . . . .
H10 H -0.0181 0.2920 1.4597 0.043 Uiso 1 1 calc R U . . .
C11 C -0.0298(9) 0.3999(9) 1.3508(7) 0.033(3) Uani 1 1 d . . . . .
C12 C -0.1200(10) 0.4647(9) 1.3747(8) 0.036(3) Uani 1 1 d . . . . .
C13 C 0.6518(9) 0.7475(8) 0.2808(8) 0.034(3) Uani 1 1 d . . . . .
C14 C 0.6277(9) 0.8304(8) 0.2120(7) 0.032(3) Uani 1 1 d . . . . .
C15 C 0.6653(9) 0.8448(8) 0.1281(8) 0.032(3) Uani 1 1 d . . . . .
H15 H 0.7128 0.8014 0.1037 0.039 Uiso 1 1 calc R U . . .
C16 C 0.6236(9) 0.9340(8) 0.0818(7) 0.030(2) Uani 1 1 d . . . . .
H16 H 0.6405 0.9566 0.0225 0.036 Uiso 1 1 calc R U . . .
C17 C 0.5570(9) 0.9829(8) 0.1317(7) 0.030(2) Uani 1 1 d . . . . .
C18 C 0.4936(9) 1.0752(8) 0.1081(8) 0.030(2) Uani 1 1 d . . . . .
C19 C -0.1866(15) 0.1817(13) 0.5182(13) 0.071(5) Uani 1 1 d . . . . .
C20 C -0.2162(18) 0.1719(18) 0.6053(12) 0.094(8) Uani 1 1 d . . . . .
H20A H -0.1553 0.1755 0.6206 0.112 Uiso 1 1 calc R U . . .
H20B H -0.2430 0.1109 0.6403 0.112 Uiso 1 1 calc R U . . .
C21 C -0.300(2) 0.2503(16) 0.6191(14) 0.100(8) Uani 1 1 d . . . . .
H21A H -0.2709 0.3015 0.6213 0.120 Uiso 1 1 calc R U . . .
H21B H -0.3565 0.2280 0.6715 0.120 Uiso 1 1 calc R U . . .
C22 C -0.3402(14) 0.2827(13) 0.5414(12) 0.069(5) Uani 1 1 d . . . . .
H22A H -0.4045 0.2551 0.5542 0.082 Uiso 1 1 calc R U . . .
H22B H -0.3532 0.3516 0.5191 0.082 Uiso 1 1 calc R U . . .
C23 C -0.247(2) 0.2700(17) 0.3941(13) 0.096(7) Uani 1 1 d . . . . .
H23A H -0.1782 0.2458 0.3644 0.144 Uiso 1 1 calc R U . . .
H23B H -0.2572 0.3379 0.3683 0.144 Uiso 1 1 calc R U . . .
H23C H -0.3012 0.2417 0.3909 0.144 Uiso 1 1 calc R U . . .
C24 C 0.0084(10) 0.7297(11) 0.2915(9) 0.045(3) Uani 1 1 d . . . . .
H24 H -0.0325 0.7856 0.2697 0.054 Uiso 1 1 calc R U . . .
C25 C -0.0091(11) 0.6918(12) 0.3773(9) 0.049(3) Uani 1 1 d . . . . .
H25 H -0.0596 0.7221 0.4135 0.058 Uiso 1 1 calc R U . . .
C26 C 0.0466(12) 0.6113(12) 0.4083(9) 0.052(4) Uani 1 1 d . . . . .
H26 H 0.0355 0.5850 0.4670 0.062 Uiso 1 1 calc R U . . .
C27 C 0.1216(11) 0.5649(10) 0.3550(9) 0.046(3) Uani 1 1 d . . . . .
C28 C 0.1377(9) 0.6097(9) 0.2698(8) 0.035(3) Uani 1 1 d . . . . .
C29 C 0.2187(10) 0.5701(9) 0.2098(8) 0.038(3) Uani 1 1 d . . . . .
C30 C 0.2759(11) 0.4853(10) 0.2414(9) 0.044(3) Uani 1 1 d . . . . .
C31 C 0.2519(12) 0.4389(10) 0.3304(10) 0.051(4) Uani 1 1 d . . . . .
H31 H 0.2889 0.3800 0.3512 0.062 Uiso 1 1 calc R U . . .
C32 C 0.1810(12) 0.4753(11) 0.3831(9) 0.050(4) Uani 1 1 d . . . . .
H32 H 0.1677 0.4426 0.4413 0.060 Uiso 1 1 calc R U . . .
C33 C 0.3556(11) 0.4504(10) 0.1821(10) 0.046(3) Uani 1 1 d . . . . .
H33 H 0.3973 0.3933 0.1996 0.055 Uiso 1 1 calc R U . . .
C34 C 0.3719(10) 0.5009(9) 0.0977(9) 0.042(3) Uani 1 1 d . . . . .
H34 H 0.4237 0.4779 0.0566 0.051 Uiso 1 1 calc R U . . .
C35 C 0.3123(11) 0.5849(9) 0.0741(9) 0.042(3) Uani 1 1 d . . . . .
H35 H 0.3257 0.6191 0.0161 0.050 Uiso 1 1 calc R U . . .
C36 C -0.0532(10) 0.6494(9) 0.1341(8) 0.037(3) Uani 1 1 d . . . . .
H36 H -0.0739 0.6463 0.1909 0.044 Uiso 1 1 calc R U . . .
C37 C -0.1160(9) 0.6134(9) 0.1081(9) 0.039(3) Uani 1 1 d . . . . .
H37 H -0.1778 0.5876 0.1470 0.047 Uiso 1 1 calc R U . . .
C38 C -0.0882(11) 0.6157(9) 0.0277(9) 0.043(3) Uani 1 1 d . . . . .
H38 H -0.1295 0.5911 0.0097 0.051 Uiso 1 1 calc R U . . .
C39 C 0.0042(10) 0.6557(9) -0.0290(8) 0.035(3) Uani 1 1 d . . . . .
C40 C 0.0615(10) 0.6915(8) -0.0001(8) 0.032(3) Uani 1 1 d . . . . .
C41 C 0.1532(9) 0.7336(8) -0.0534(8) 0.031(2) Uani 1 1 d . . . . .
C42 C 0.1913(10) 0.7359(9) -0.1379(8) 0.038(3) Uani 1 1 d . . . . .
C43 C 0.1306(13) 0.6963(11) -0.1656(10) 0.052(4) Uani 1 1 d . . . . .
H43 H 0.1545 0.6963 -0.2217 0.062 Uiso 1 1 calc R U . . .
C44 C 0.0421(12) 0.6599(10) -0.1150(9) 0.046(3) Uani 1 1 d . . . . .
H44 H 0.0036 0.6364 -0.1362 0.056 Uiso 1 1 calc R U . . .
C45 C 0.2811(11) 0.7767(10) -0.1876(8) 0.045(3) Uani 1 1 d . . . . .
H45 H 0.3079 0.7801 -0.2446 0.054 Uiso 1 1 calc R U . . .
C46 C 0.3332(10) 0.8134(9) -0.1542(8) 0.042(3) Uani 1 1 d . . . . .
H46 H 0.3967 0.8398 -0.1874 0.050 Uiso 1 1 calc R U . . .
C47 C 0.2897(10) 0.8103(9) -0.0707(8) 0.039(3) Uani 1 1 d . . . . .
H47 H 0.3236 0.8365 -0.0481 0.047 Uiso 1 1 calc R U . . .
C48 C -0.0632(11) 0.8893(9) 0.0962(9) 0.044(3) Uani 1 1 d . . . . .
H48 H -0.0871 0.8501 0.0784 0.052 Uiso 1 1 calc R U . . .
C49 C -0.1310(11) 0.9656(10) 0.1137(11) 0.051(4) Uani 1 1 d . . . . .
H49 H -0.1985 0.9785 0.1065 0.062 Uiso 1 1 calc R U . . .
C50 C -0.0982(12) 1.0218(10) 0.1415(10) 0.051(4) Uani 1 1 d . . . . .
H50 H -0.1439 1.0733 0.1544 0.061 Uiso 1 1 calc R U . . .
C51 C 0.0021(11) 1.0036(10) 0.1510(9) 0.045(3) Uani 1 1 d . . . . .
C52 C 0.0652(9) 0.9245(8) 0.1308(8) 0.033(3) Uani 1 1 d . . . . .
C53 C 0.1676(9) 0.9013(9) 0.1415(8) 0.032(3) Uani 1 1 d . . . . .
C54 C 0.2057(9) 0.9556(9) 0.1689(8) 0.035(3) Uani 1 1 d . . . . .
C55 C 0.1384(11) 1.0348(9) 0.1893(9) 0.044(3) Uani 1 1 d . . . . .
H55 H 0.1626 1.0724 0.2084 0.052 Uiso 1 1 calc R U . . .
C56 C 0.0413(11) 1.0550(10) 0.1810(10) 0.049(4) Uani 1 1 d . . . . .
H56 H -0.0023 1.1062 0.1962 0.059 Uiso 1 1 calc R U . . .
C57 C 0.3071(9) 0.9281(10) 0.1787(8) 0.038(3) Uani 1 1 d . . . . .
H57 H 0.3354 0.9623 0.1985 0.046 Uiso 1 1 calc R U . . .
C58 C 0.3630(10) 0.8516(9) 0.1590(8) 0.038(3) Uani 1 1 d . . . . .
H58 H 0.4314 0.8321 0.1646 0.045 Uiso 1 1 calc R U . . .
C59 C 0.3202(9) 0.8020(9) 0.1308(8) 0.036(3) Uani 1 1 d . . . . .
H59 H 0.3609 0.7491 0.1171 0.043 Uiso 1 1 calc R U . . .
O22 O 0.4337(16) 0.8355(17) 0.6323(13) 0.063(5) Uani 0.5 1 d D U P . .
N9 N 0.5957(18) 0.876(2) 0.5750(15) 0.071(5) Uani 0.5 1 d D U P . .
C60 C 0.5101(18) 0.854(3) 0.5689(13) 0.065(5) Uani 0.5 1 d D U P . .
C61 C 0.527(2) 0.865(3) 0.4782(14) 0.063(5) Uani 0.5 1 d D U P . .
H61A H 0.4712 0.9096 0.4572 0.075 Uiso 0.5 1 calc R U P . .
H61B H 0.5277 0.8045 0.4723 0.075 Uiso 0.5 1 calc R U P . .
C62 C 0.632(2) 0.902(3) 0.4301(18) 0.065(5) Uani 0.5 1 d D U P . .
H62A H 0.6239 0.9699 0.3985 0.078 Uiso 0.5 1 calc R U P . .
H62B H 0.6751 0.8686 0.3907 0.078 Uiso 0.5 1 calc R U P . .
C63 C 0.682(2) 0.884(3) 0.4986(15) 0.072(6) Uani 0.5 1 d D U P . .
H63A H 0.7302 0.8264 0.5042 0.087 Uiso 0.5 1 calc R U P . .
H63B H 0.7205 0.9369 0.4858 0.087 Uiso 0.5 1 calc R U P . .
C64 C 0.617(3) 0.865(3) 0.6538(18) 0.076(7) Uani 0.5 1 d D U P . .
H64A H 0.6020 0.8034 0.6945 0.114 Uiso 0.5 1 calc R U P . .
H64B H 0.5735 0.9134 0.6771 0.114 Uiso 0.5 1 calc R U P . .
H64C H 0.6911 0.8719 0.6413 0.114 Uiso 0.5 1 calc R U P . .


_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 O2 1.765(8) . ?
U1 O1 1.781(8) . ?
U1 O16 2.456(7) 1_546 ?
U1 O6 2.456(8) . ?
U1 O7 2.471(8) . ?
U1 O10 2.477(8) . ?
U1 O11 2.479(8) . ?
U1 O17 2.508(8) 1_546 ?
U2 O4 1.772(9) . ?
U2 O3 1.772(9) . ?
U2 O8 2.436(8) . ?
U2 O12 2.463(8) 1_654 ?
U2 O14 2.467(8) . ?
U2 O9 2.493(8) . ?
U2 O15 2.496(8) . ?
U2 O13 2.510(8) 1_654 ?
U3 O5 1.751(14) . ?
U3 O5 1.751(14) 2_556 ?
U3 O21 2.346(13) . ?
U3 O21 2.346(13) 2_556 ?
U3 O18 2.57(2) 2_556 ?
U3 O18 2.57(2) . ?
U3 O19 2.582(18) . ?
U3 O19 2.582(18) 2_556 ?
Ni1 N5 2.078(10) . ?
Ni1 N8 2.090(11) . ?
Ni1 N6 2.091(10) . ?
Ni1 N7 2.096(10) . ?
Ni1 N3 2.104(11) . ?
Ni1 N4 2.105(10) . ?
S1 C5 1.703(11) . ?
S1 C2 1.728(12) . ?
S2 C8 1.714(11) . ?
S2 C11 1.717(12) . ?
S3 C17 1.717(11) . ?
S3 C14 1.727(12) . ?
O6 C1 1.269(14) . ?
O7 C1 1.288(14) . ?
O8 C6 1.255(14) . ?
O9 C6 1.282(14) . ?
O10 C7 1.273(14) . ?
O11 C7 1.265(14) . ?
O12 C12 1.260(15) . ?
O12 U2 2.463(8) 1_456 ?
O13 C12 1.266(15) . ?
O13 U2 2.510(8) 1_456 ?
O14 C13 1.269(15) . ?
O15 C13 1.247(14) . ?
O16 C18 1.256(14) . ?
O16 U1 2.456(7) 1_564 ?
O17 C18 1.252(14) . ?
O17 U1 2.508(8) 1_564 ?
O18 N1 1.24(3) . ?
O19 N1 1.19(3) . ?
O20 N1 1.30(3) . ?
O21 C19 1.25(2) . ?
N2 C19 1.32(2) . ?
N2 C22 1.45(2) . ?
N2 C23 1.50(2) . ?
N3 C28 1.348(16) . ?
N3 C24 1.355(17) . ?
N4 C35 1.332(17) . ?
N4 C29 1.353(16) . ?
N5 C36 1.311(16) . ?
N5 C40 1.397(15) . ?
N6 C47 1.334(17) . ?
N6 C41 1.353(16) . ?
N7 C48 1.344(16) . ?
N7 C52 1.359(16) . ?
N8 C59 1.327(15) . ?
N8 C53 1.362(16) . ?
C1 C2 1.440(16) . ?
C2 C3 1.386(16) . ?
C3 C4 1.405(17) . ?
C3 H3 0.9500 . ?
C4 C5 1.346(17) . ?
C4 H4 0.9500 . ?
C5 C6 1.472(16) . ?
C7 C8 1.456(16) . ?
C8 C9 1.359(18) . ?
C9 C10 1.406(17) . ?
C9 H9 0.9500 . ?
C10 C11 1.388(16) . ?
C10 H10 0.9500 . ?
C11 C12 1.460(16) . ?
C13 C14 1.483(16) . ?
C14 C15 1.365(17) . ?
C15 C16 1.433(15) . ?
C15 H15 0.9500 . ?
C16 C17 1.364(16) . ?
C16 H16 0.9500 . ?
C17 C18 1.495(15) . ?
C19 C20 1.44(3) . ?
C20 C21 1.51(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.56(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.39(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.34(2) . ?
C25 H25 0.9500 . ?
C26 C27 1.42(2) . ?
C26 H26 0.9500 . ?
C27 C28 1.387(18) . ?
C27 C32 1.45(2) . ?
C28 C29 1.465(18) . ?
C29 C30 1.400(18) . ?
C30 C33 1.41(2) . ?
C30 C31 1.44(2) . ?
C31 C32 1.30(2) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C34 1.39(2) . ?
C33 H33 0.9500 . ?
C34 C35 1.379(18) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.412(18) . ?
C36 H36 0.9500 . ?
C37 C38 1.36(2) . ?
C37 H37 0.9500 . ?
C38 C39 1.421(19) . ?
C38 H38 0.9500 . ?
C39 C40 1.387(17) . ?
C39 C44 1.437(19) . ?
C40 C41 1.413(18) . ?
C41 C42 1.420(17) . ?
C42 C45 1.37(2) . ?
C42 C43 1.45(2) . ?
C43 C44 1.34(2) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 C46 1.40(2) . ?
C45 H45 0.9500 . ?
C46 C47 1.400(19) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C48 C49 1.398(19) . ?
C48 H48 0.9500 . ?
C49 C50 1.38(2) . ?
C49 H49 0.9500 . ?
C50 C51 1.402(19) . ?
C50 H50 0.9500 . ?
C51 C56 1.40(2) . ?
C51 C52 1.428(18) . ?
C52 C53 1.437(16) . ?
C53 C54 1.396(18) . ?
C54 C57 1.417(17) . ?
C54 C55 1.449(18) . ?
C55 C56 1.35(2) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 C58 1.362(18) . ?
C57 H57 0.9500 . ?
C58 C59 1.389(18) . ?
C58 H58 0.9500 . ?
C59 H59 0.9500 . ?
O22 C60 1.242(10) . ?
N9 C60 1.352(10) . ?
N9 C63 1.453(10) . ?
N9 C64 1.499(10) . ?
C60 C61 1.518(10) . ?
C61 C62 1.520(10) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 C63 1.521(10) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U1 O1 178.2(4) . . ?
O2 U1 O16 92.1(3) . 1_546 ?
O1 U1 O16 87.0(3) . 1_546 ?
O2 U1 O6 89.6(3) . . ?
O1 U1 O6 89.6(4) . . ?
O16 U1 O6 121.7(3) 1_546 . ?
O2 U1 O7 93.1(3) . . ?
O1 U1 O7 87.7(3) . . ?
O16 U1 O7 172.6(3) 1_546 . ?
O6 U1 O7 53.1(3) . . ?
O2 U1 O10 88.2(3) . . ?
O1 U1 O10 93.5(3) . . ?
O16 U1 O10 118.8(3) 1_546 . ?
O6 U1 O10 119.5(3) . . ?
O7 U1 O10 66.6(3) . . ?
O2 U1 O11 90.8(4) . . ?
O1 U1 O11 90.2(4) . . ?
O16 U1 O11 66.4(3) 1_546 . ?
O6 U1 O11 171.8(3) . . ?
O7 U1 O11 118.7(3) . . ?
O10 U1 O11 52.4(3) . . ?
O2 U1 O17 88.9(3) . 1_546 ?
O1 U1 O17 89.3(3) . 1_546 ?
O16 U1 O17 52.4(3) 1_546 1_546 ?
O6 U1 O17 69.4(3) . 1_546 ?
O7 U1 O17 122.4(3) . 1_546 ?
O10 U1 O17 170.6(3) . 1_546 ?
O11 U1 O17 118.8(3) . 1_546 ?
O4 U2 O3 179.6(4) . . ?
O4 U2 O8 86.3(4) . . ?
O3 U2 O8 93.3(4) . . ?
O4 U2 O12 89.5(4) . 1_654 ?
O3 U2 O12 90.7(4) . 1_654 ?
O8 U2 O12 118.9(3) . 1_654 ?
O4 U2 O14 90.8(4) . . ?
O3 U2 O14 89.4(4) . . ?
O8 U2 O14 122.7(3) . . ?
O12 U2 O14 118.3(3) 1_654 . ?
O4 U2 O9 94.7(4) . . ?
O3 U2 O9 84.9(4) . . ?
O8 U2 O9 52.7(3) . . ?
O12 U2 O9 170.1(3) 1_654 . ?
O14 U2 O9 70.6(3) . . ?
O4 U2 O15 88.0(4) . . ?
O3 U2 O15 92.4(4) . . ?
O8 U2 O15 172.4(3) . . ?
O12 U2 O15 66.1(3) 1_654 . ?
O14 U2 O15 52.3(3) . . ?
O9 U2 O15 122.9(3) . . ?
O4 U2 O13 91.4(4) . 1_654 ?
O3 U2 O13 88.5(4) . 1_654 ?
O8 U2 O13 66.9(3) . 1_654 ?
O12 U2 O13 52.3(3) 1_654 1_654 ?
O14 U2 O13 170.3(3) . 1_654 ?
O9 U2 O13 118.6(3) . 1_654 ?
O15 U2 O13 118.3(3) . 1_654 ?
O5 U3 O5 180.0 . 2_556 ?
O5 U3 O21 93.4(6) . . ?
O5 U3 O21 86.6(6) 2_556 . ?
O5 U3 O21 86.6(6) . 2_556 ?
O5 U3 O21 93.4(6) 2_556 2_556 ?
O21 U3 O21 180.0 . 2_556 ?
O5 U3 O18 83.7(9) . 2_556 ?
O5 U3 O18 96.3(9) 2_556 2_556 ?
O21 U3 O18 65.2(6) . 2_556 ?
O21 U3 O18 114.8(6) 2_556 2_556 ?
O5 U3 O18 96.3(9) . . ?
O5 U3 O18 83.7(9) 2_556 . ?
O21 U3 O18 114.8(6) . . ?
O21 U3 O18 65.2(6) 2_556 . ?
O18 U3 O18 180.0 2_556 . ?
O5 U3 O19 91.0(8) . . ?
O5 U3 O19 89.0(8) 2_556 . ?
O21 U3 O19 67.3(6) . . ?
O21 U3 O19 112.7(6) 2_556 . ?
O18 U3 O19 131.7(6) 2_556 . ?
O18 U3 O19 48.3(6) . . ?
O5 U3 O19 89.0(8) . 2_556 ?
O5 U3 O19 91.0(8) 2_556 2_556 ?
O21 U3 O19 112.7(6) . 2_556 ?
O21 U3 O19 67.3(6) 2_556 2_556 ?
O18 U3 O19 48.3(6) 2_556 2_556 ?
O18 U3 O19 131.7(6) . 2_556 ?
O19 U3 O19 180.0 . 2_556 ?
N5 Ni1 N8 170.5(4) . . ?
N5 Ni1 N6 80.3(4) . . ?
N8 Ni1 N6 98.1(4) . . ?
N5 Ni1 N7 91.7(4) . . ?
N8 Ni1 N7 79.3(4) . . ?
N6 Ni1 N7 98.9(4) . . ?
N5 Ni1 N3 96.3(4) . . ?
N8 Ni1 N3 87.1(4) . . ?
N6 Ni1 N3 168.0(4) . . ?
N7 Ni1 N3 92.7(4) . . ?
N5 Ni1 N4 93.6(4) . . ?
N8 Ni1 N4 95.7(4) . . ?
N6 Ni1 N4 89.1(4) . . ?
N7 Ni1 N4 171.1(4) . . ?
N3 Ni1 N4 79.7(4) . . ?
C5 S1 C2 91.2(6) . . ?
C8 S2 C11 91.6(6) . . ?
C17 S3 C14 90.9(6) . . ?
C1 O6 U1 94.4(7) . . ?
C1 O7 U1 93.2(7) . . ?
C6 O8 U2 95.7(7) . . ?
C6 O9 U2 92.3(7) . . ?
C7 O10 U1 94.3(7) . . ?
C7 O11 U1 94.4(7) . . ?
C12 O12 U2 94.8(7) . 1_456 ?
C12 O13 U2 92.5(7) . 1_456 ?
C13 O14 U2 93.8(7) . . ?
C13 O15 U2 93.0(7) . . ?
C18 O16 U1 94.0(7) . 1_564 ?
C18 O17 U1 91.7(7) . 1_564 ?
N1 O18 U3 94.9(18) . . ?
N1 O19 U3 95.6(17) . . ?
C19 O21 U3 139.8(13) . . ?
O19 N1 O18 120(3) . . ?
O19 N1 O20 120(3) . . ?
O18 N1 O20 118(3) . . ?
C19 N2 C22 115.7(16) . . ?
C19 N2 C23 121.5(17) . . ?
C22 N2 C23 122.2(16) . . ?
C28 N3 C24 118.1(12) . . ?
C28 N3 Ni1 113.3(9) . . ?
C24 N3 Ni1 128.2(9) . . ?
C35 N4 C29 116.7(11) . . ?
C35 N4 Ni1 130.6(9) . . ?
C29 N4 Ni1 112.7(8) . . ?
C36 N5 C40 117.9(11) . . ?
C36 N5 Ni1 129.9(9) . . ?
C40 N5 Ni1 112.1(8) . . ?
C47 N6 C41 119.8(11) . . ?
C47 N6 Ni1 127.5(9) . . ?
C41 N6 Ni1 112.2(8) . . ?
C48 N7 C52 117.0(11) . . ?
C48 N7 Ni1 129.6(9) . . ?
C52 N7 Ni1 111.7(7) . . ?
C59 N8 C53 117.9(11) . . ?
C59 N8 Ni1 128.5(9) . . ?
C53 N8 Ni1 112.4(8) . . ?
O6 C1 O7 119.1(10) . . ?
O6 C1 C2 121.2(10) . . ?
O7 C1 C2 119.7(10) . . ?
C3 C2 C1 128.5(11) . . ?
C3 C2 S1 111.1(9) . . ?
C1 C2 S1 120.3(8) . . ?
C2 C3 C4 111.7(11) . . ?
C2 C3 H3 124.1 . . ?
C4 C3 H3 124.1 . . ?
C5 C4 C3 113.4(11) . . ?
C5 C4 H4 123.3 . . ?
C3 C4 H4 123.3 . . ?
C4 C5 C6 128.7(11) . . ?
C4 C5 S1 112.6(9) . . ?
C6 C5 S1 118.7(9) . . ?
O8 C6 O9 119.3(11) . . ?
O8 C6 C5 119.9(10) . . ?
O9 C6 C5 120.7(10) . . ?
O11 C7 O10 119.0(10) . . ?
O11 C7 C8 120.5(11) . . ?
O10 C7 C8 120.5(10) . . ?
C9 C8 C7 128.5(11) . . ?
C9 C8 S2 111.5(9) . . ?
C7 C8 S2 120.0(9) . . ?
C8 C9 C10 113.9(11) . . ?
C8 C9 H9 123.1 . . ?
C10 C9 H9 123.1 . . ?
C11 C10 C9 111.2(11) . . ?
C11 C10 H10 124.4 . . ?
C9 C10 H10 124.4 . . ?
C10 C11 C12 129.2(11) . . ?
C10 C11 S2 111.7(9) . . ?
C12 C11 S2 119.0(9) . . ?
O12 C12 O13 120.3(11) . . ?
O12 C12 C11 118.8(11) . . ?
O13 C12 C11 120.9(11) . . ?
O15 C13 O14 120.9(11) . . ?
O15 C13 C14 119.4(11) . . ?
O14 C13 C14 119.7(10) . . ?
C15 C14 C13 127.8(11) . . ?
C15 C14 S3 113.0(8) . . ?
C13 C14 S3 119.2(9) . . ?
C14 C15 C16 111.0(10) . . ?
C14 C15 H15 124.5 . . ?
C16 C15 H15 124.5 . . ?
C17 C16 C15 112.9(10) . . ?
C17 C16 H16 123.5 . . ?
C15 C16 H16 123.5 . . ?
C16 C17 C18 129.2(11) . . ?
C16 C17 S3 112.2(8) . . ?
C18 C17 S3 118.5(9) . . ?
O17 C18 O16 121.9(10) . . ?
O17 C18 C17 119.8(11) . . ?
O16 C18 C17 118.4(10) . . ?
O21 C19 N2 123.6(19) . . ?
O21 C19 C20 128.1(19) . . ?
N2 C19 C20 108.3(17) . . ?
C19 C20 C21 107.3(17) . . ?
C19 C20 H20A 110.2 . . ?
C21 C20 H20A 110.2 . . ?
C19 C20 H20B 110.2 . . ?
C21 C20 H20B 110.2 . . ?
H20A C20 H20B 108.5 . . ?
C20 C21 C22 103.2(18) . . ?
C20 C21 H21A 111.1 . . ?
C22 C21 H21A 111.1 . . ?
C20 C21 H21B 111.1 . . ?
C22 C21 H21B 111.1 . . ?
H21A C21 H21B 109.1 . . ?
N2 C22 C21 100.9(15) . . ?
N2 C22 H22A 111.6 . . ?
C21 C22 H22A 111.6 . . ?
N2 C22 H22B 111.6 . . ?
C21 C22 H22B 111.6 . . ?
H22A C22 H22B 109.4 . . ?
N2 C23 H23A 109.5 . . ?
N2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N3 C24 C25 122.3(14) . . ?
N3 C24 H24 118.8 . . ?
C25 C24 H24 118.8 . . ?
C26 C25 C24 118.8(14) . . ?
C26 C25 H25 120.6 . . ?
C24 C25 H25 120.6 . . ?
C25 C26 C27 121.2(13) . . ?
C25 C26 H26 119.4 . . ?
C27 C26 H26 119.4 . . ?
C28 C27 C26 116.3(13) . . ?
C28 C27 C32 118.7(14) . . ?
C26 C27 C32 125.0(14) . . ?
N3 C28 C27 123.2(13) . . ?
N3 C28 C29 116.7(11) . . ?
C27 C28 C29 120.2(12) . . ?
N4 C29 C30 124.6(12) . . ?
N4 C29 C28 117.4(11) . . ?
C30 C29 C28 117.9(12) . . ?
C29 C30 C33 116.6(13) . . ?
C29 C30 C31 119.7(14) . . ?
C33 C30 C31 123.7(13) . . ?
C32 C31 C30 121.8(14) . . ?
C32 C31 H31 119.1 . . ?
C30 C31 H31 119.1 . . ?
C31 C32 C27 121.5(14) . . ?
C31 C32 H32 119.2 . . ?
C27 C32 H32 119.2 . . ?
C34 C33 C30 118.9(12) . . ?
C34 C33 H33 120.6 . . ?
C30 C33 H33 120.6 . . ?
C35 C34 C33 119.3(13) . . ?
C35 C34 H34 120.3 . . ?
C33 C34 H34 120.3 . . ?
N4 C35 C34 123.9(13) . . ?
N4 C35 H35 118.0 . . ?
C34 C35 H35 118.0 . . ?
N5 C36 C37 123.0(12) . . ?
N5 C36 H36 118.5 . . ?
C37 C36 H36 118.5 . . ?
C38 C37 C36 120.1(12) . . ?
C38 C37 H37 120.0 . . ?
C36 C37 H37 120.0 . . ?
C37 C38 C39 118.4(12) . . ?
C37 C38 H38 120.8 . . ?
C39 C38 H38 120.8 . . ?
C40 C39 C38 118.8(12) . . ?
C40 C39 C44 118.1(12) . . ?
C38 C39 C44 123.1(12) . . ?
C39 C40 N5 121.7(12) . . ?
C39 C40 C41 121.7(11) . . ?
N5 C40 C41 116.5(11) . . ?
N6 C41 C40 118.6(11) . . ?
N6 C41 C42 121.5(11) . . ?
C40 C41 C42 119.8(12) . . ?
C45 C42 C41 118.1(13) . . ?
C45 C42 C43 124.9(13) . . ?
C41 C42 C43 116.9(12) . . ?
C44 C43 C42 122.2(14) . . ?
C44 C43 H43 118.9 . . ?
C42 C43 H43 118.9 . . ?
C43 C44 C39 121.1(13) . . ?
C43 C44 H44 119.5 . . ?
C39 C44 H44 119.5 . . ?
C42 C45 C46 120.0(12) . . ?
C42 C45 H45 120.0 . . ?
C46 C45 H45 120.0 . . ?
C47 C46 C45 118.6(12) . . ?
C47 C46 H46 120.7 . . ?
C45 C46 H46 120.7 . . ?
N6 C47 C46 121.8(13) . . ?
N6 C47 H47 119.1 . . ?
C46 C47 H47 119.1 . . ?
N7 C48 C49 123.4(13) . . ?
N7 C48 H48 118.3 . . ?
C49 C48 H48 118.3 . . ?
C50 C49 C48 119.0(12) . . ?
C50 C49 H49 120.5 . . ?
C48 C49 H49 120.5 . . ?
C49 C50 C51 120.6(13) . . ?
C49 C50 H50 119.7 . . ?
C51 C50 H50 119.7 . . ?
C50 C51 C56 124.7(13) . . ?
C50 C51 C52 116.0(13) . . ?
C56 C51 C52 119.3(12) . . ?
N7 C52 C51 124.1(11) . . ?
N7 C52 C53 117.7(11) . . ?
C51 C52 C53 118.2(12) . . ?
N8 C53 C54 122.5(11) . . ?
N8 C53 C52 116.3(11) . . ?
C54 C53 C52 121.2(11) . . ?
C53 C54 C57 118.1(12) . . ?
C53 C54 C55 118.5(11) . . ?
C57 C54 C55 123.3(12) . . ?
C56 C55 C54 120.0(13) . . ?
C56 C55 H55 120.0 . . ?
C54 C55 H55 120.0 . . ?
C55 C56 C51 122.7(13) . . ?
C55 C56 H56 118.6 . . ?
C51 C56 H56 118.6 . . ?
C58 C57 C54 118.4(12) . . ?
C58 C57 H57 120.8 . . ?
C54 C57 H57 120.8 . . ?
C57 C58 C59 120.1(12) . . ?
C57 C58 H58 120.0 . . ?
C59 C58 H58 120.0 . . ?
N8 C59 C58 123.1(12) . . ?
N8 C59 H59 118.4 . . ?
C58 C59 H59 118.4 . . ?
C60 N9 C63 111(2) . . ?
C60 N9 C64 127(3) . . ?
C63 N9 C64 119(2) . . ?
O22 C60 N9 118(2) . . ?
O22 C60 C61 133(2) . . ?
N9 C60 C61 108.6(19) . . ?
C60 C61 C62 106(2) . . ?
C60 C61 H61A 110.6 . . ?
C62 C61 H61A 110.6 . . ?
C60 C61 H61B 110.6 . . ?
C62 C61 H61B 110.6 . . ?
H61A C61 H61B 108.7 . . ?
C61 C62 C63 103(2) . . ?
C61 C62 H62A 111.1 . . ?
C63 C62 H62A 111.1 . . ?
C61 C62 H62B 111.1 . . ?
C63 C62 H62B 111.1 . . ?
H62A C62 H62B 109.1 . . ?
N9 C63 C62 106(2) . . ?
N9 C63 H63A 110.5 . . ?
C62 C63 H63A 110.5 . . ?
N9 C63 H63B 110.5 . . ?
C62 C63 H63B 110.5 . . ?
H63A C63 H63B 108.7 . . ?
N9 C64 H64A 109.5 . . ?
N9 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
N9 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?

_refine_diff_density_max         1.812
_refine_diff_density_min         -9.089
_refine_diff_density_rms         0.288

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1437898'
_audit_update_record             
;
2015-11-19 deposited with the CCDC.
2016-01-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H26 Ag2 N6 O17 S3 U2'
_chemical_formula_weight         1530.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           137
_space_group_name_H-M_alt        'P 42/n m c'
_space_group_name_Hall           '-P 4ac 2a'

_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+1/2, z'
'-y+1/2, x, z+1/2'
'y, -x+1/2, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y, -z'
'y+1/2, x+1/2, -z+1/2'
'-y, -x, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z-1/2'
'-y, x-1/2, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y, z'
'-y-1/2, -x-1/2, z-1/2'
'y, x, z-1/2'

_cell_length_a                   26.1007(3)
_cell_length_b                   26.1007(3)
_cell_length_c                   6.6950(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4560.95(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    101372
_cell_measurement_theta_min      3.14
_cell_measurement_theta_max      25.68

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.229
_exptl_crystal_F_000             2840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    8.134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.325
_exptl_absorpt_correction_T_max  0.409
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and four ω scans with 1° steps (661 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            101372
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_av_R_equivalents  0.0122
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.141
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2263
_reflns_number_gt                1989
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. One dicarboxylate ligand is disordered over two positions related 
 by a mirror; only the two positions of the central ring are well resolved and 
 a mean position only was found for the carboxylate group (notwithstanding
 its large and very anisotropic displacement parameters). One of the 
 acetonitrile molecules bound to Ag1 is too close to its image by symmetry
 and was given an occupancy factor of 0.5 accordingly. The water solvent 
 molecule was also given half-occupancy in order to retain an acceptable 
 displacement parameter. All non-hydrogen atoms were refined with anisotropic
 displacement parameters, with restraints on bond lengths for the disordered
 acetonitrile molecule and on displacement parameters for both acetonitrile
 molecules. The water H atoms were not found; all the others were introduced
 at calculated positions and were treated as riding atoms with an isotropic
 displacement parameter equal to 1.2 times that of the parent atom (1.5 for
 CH₃, with optimized geometry). Some voids in the lattice probably indicate
 the presence of other, unresolved solvent molecules.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0447P)²+38.7996P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2263
_refine_ls_number_parameters     174
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.1023
_refine_ls_wR_factor_gt          0.0993
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.7500 0.54057(2) 0.66891(6) 0.03339(15) Uani 1 2 d S T P . .
Ag1 Ag 0.59035(7) 0.40965(7) 0.2500 0.1517(8) Uani 1 2 d DS T P . .
S1 S 0.60639(7) 0.39361(7) 0.7500 0.0437(6) Uani 1 2 d S T P . .
S2 S 0.72379(18) 0.7500 0.6190(7) 0.0319(10) Uani 0.5 2 d S T P . .
O1 O 0.7500 0.5318(3) 0.4047(12) 0.0428(17) Uani 1 2 d S T P . .
O2 O 0.7500 0.5492(3) 0.9281(12) 0.0463(18) Uani 1 2 d S T P . .
O3 O 0.65516(19) 0.53478(18) 0.6814(8) 0.0437(12) Uani 1 1 d . . . . .
O4 O 0.6975(2) 0.46209(18) 0.7058(9) 0.0471(14) Uani 1 1 d . . . . .
O5 O 0.7909(3) 0.6246(2) 0.6249(11) 0.0669(18) Uani 1 1 d . . . . .
O6 O 0.7500 0.3582(8) 0.674(5) 0.147(13) Uani 0.5 2 d S T P . .
C1 C 0.6555(3) 0.4865(3) 0.7035(11) 0.0409(17) Uani 1 1 d . . . . .
C2 C 0.6067(3) 0.4593(3) 0.7257(11) 0.0400(17) Uani 1 1 d . . . . .
C3 C 0.5587(3) 0.4786(3) 0.7365(13) 0.0463(18) Uani 1 1 d . . . . .
H3A H 0.5512 0.5141 0.7266 0.056 Uiso 1 1 calc R U . . .
C4 C 0.7500 0.6478(4) 0.617(2) 0.070(4) Uani 1 2 d S T P . .
C5 C 0.7695(5) 0.7033(4) 0.604(2) 0.034(3) Uani 0.5 1 d . . P . .
C6 C 0.8180(5) 0.7234(5) 0.583(2) 0.038(3) Uani 0.5 1 d . . P . .
H6A H 0.8482 0.7028 0.5663 0.046 Uiso 0.5 1 d R U P . .
N1 N 0.5110(6) 0.3849(5) 0.2812(16) 0.115(4) Uani 1 1 d . U . . .
C7 C 0.4703(7) 0.3726(6) 0.2964(19) 0.097(3) Uani 1 1 d . U . . .
C8 C 0.4190(5) 0.3564(5) 0.3136(16) 0.092(3) Uani 1 1 d . U . . .
H8A H 0.4105 0.3336 0.2021 0.138 Uiso 1 1 calc R U . . .
H8B H 0.3963 0.3864 0.3105 0.138 Uiso 1 1 calc R U . . .
H8C H 0.4143 0.3381 0.4400 0.138 Uiso 1 1 calc R U . . .
N2 N 0.6676(6) 0.3820(14) 0.253(5) 0.200(12) Uani 0.5 1 d D U P A -1
C9 C 0.7049(19) 0.404(2) 0.217(7) 0.205(13) Uani 0.5 1 d D U P A -1
C10 C 0.7582(14) 0.4247(19) 0.174(5) 0.205(13) Uani 0.5 1 d D U P A -1
H10A H 0.7824 0.4223 0.2811 0.307 Uiso 0.5 1 d R U P A -1
H10B H 0.7721 0.4087 0.0566 0.307 Uiso 0.5 1 d R U P A -1
H10C H 0.7512 0.4601 0.1461 0.307 Uiso 0.5 1 d R U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 1.750(8) . ?
U1 O1 1.783(8) . ?
U1 O5 2.458(5) 14_755 ?
U1 O5 2.458(5) . ?
U1 O4 2.476(5) 14_755 ?
U1 O4 2.476(5) . ?
U1 O3 2.481(5) . ?
U1 O3 2.482(5) 14_755 ?
Ag1 N2 2.142(10) . ?
Ag1 N1 2.181(17) 8_665 ?
Ag1 N1 2.181(17) . ?
S1 C2 1.724(7) . ?
S1 C2 1.724(7) 8_666 ?
S2 C5 1.707(12) . ?
S2 C5 1.707(12) 13_575 ?
O3 C1 1.268(8) . ?
O4 C1 1.270(9) . ?
O5 C4 1.229(8) . ?
C1 C2 1.464(10) . ?
C2 C3 1.353(10) . ?
C3 C3 1.387(14) 8_666 ?
C3 H3A 0.9500 . ?
C4 O5 1.229(8) 14_755 ?
C4 C5 1.538(15) 14_755 ?
C4 C5 1.538(15) . ?
C5 C6 1.379(18) . ?
C6 C6 1.39(2) 13_575 ?
C6 H6A 0.9601 . ?
N1 C7 1.113(19) . ?
C7 C8 1.41(2) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
N2 C9 1.153(10) . ?
C9 C10 1.523(10) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9599 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U1 O1 180.0(3) . . ?
O2 U1 O5 90.2(3) . 14_755 ?
O1 U1 O5 89.8(3) . 14_755 ?
O2 U1 O5 90.2(3) . . ?
O1 U1 O5 89.8(3) . . ?
O5 U1 O5 51.5(3) 14_755 . ?
O2 U1 O4 90.4(2) . 14_755 ?
O1 U1 O4 89.6(2) . 14_755 ?
O5 U1 O4 172.2(2) 14_755 14_755 ?
O5 U1 O4 120.7(2) . 14_755 ?
O2 U1 O4 90.4(2) . . ?
O1 U1 O4 89.6(2) . . ?
O5 U1 O4 120.7(2) 14_755 . ?
O5 U1 O4 172.2(2) . . ?
O4 U1 O4 67.1(2) 14_755 . ?
O2 U1 O3 88.53(13) . . ?
O1 U1 O3 91.47(13) . . ?
O5 U1 O3 68.0(2) 14_755 . ?
O5 U1 O3 119.5(2) . . ?
O4 U1 O3 119.86(17) 14_755 . ?
O4 U1 O3 52.75(16) . . ?
O2 U1 O3 88.53(13) . 14_755 ?
O1 U1 O3 91.47(13) . 14_755 ?
O5 U1 O3 119.5(2) 14_755 14_755 ?
O5 U1 O3 68.0(2) . 14_755 ?
O4 U1 O3 52.75(16) 14_755 14_755 ?
O4 U1 O3 119.86(17) . 14_755 ?
O3 U1 O3 172.0(2) . 14_755 ?
N2 Ag1 N1 92.4(11) . 8_665 ?
N2 Ag1 N1 142.6(11) . . ?
N1 Ag1 N1 124.9(7) 8_665 . ?
C2 S1 C2 91.1(5) . 8_666 ?
C5 S2 C5 91.0(8) . 13_575 ?
C1 O3 U1 93.3(4) . . ?
C1 O4 U1 93.5(4) . . ?
C4 O5 U1 93.9(6) . . ?
O3 C1 O4 120.4(7) . . ?
O3 C1 C2 119.2(7) . . ?
O4 C1 C2 120.5(6) . . ?
C3 C2 C1 129.1(6) . . ?
C3 C2 S1 111.1(5) . . ?
C1 C2 S1 119.8(5) . . ?
C2 C3 C3 113.4(4) . 8_666 ?
C2 C3 H3A 123.3 . . ?
C3 C3 H3A 123.3 8_666 . ?
O5 C4 O5 120.7(10) . 14_755 ?
O5 C4 C5 100.3(6) . . ?
C6 C5 C4 131.8(10) . . ?
C6 C5 S2 112.2(9) . . ?
C4 C5 S2 116.0(8) . . ?
C5 C6 H6A 123.6 . . ?
C6 C6 H6A 124.1 13_575 . ?
C7 N1 Ag1 179.5(15) . . ?
N1 C7 C8 179.2(17) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 N2 Ag1 129(4) . . ?
N2 C9 C10 171(7) . . ?
C9 C10 H10A 115.9 . . ?
C9 C10 H10B 110.2 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 102.0 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

_refine_diff_density_max         1.376
_refine_diff_density_min         -1.286
_refine_diff_density_rms         0.137

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1437899'
_audit_update_record             
;
2015-11-19 deposited with the CCDC.
2016-01-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C136 H104 Ag5 N21 O41 S6 U4'
_chemical_formula_weight         4372.23

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   18.4849(2)
_cell_length_b                   26.8834(6)
_cell_length_c                   31.5917(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     15699.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    327711
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      25.68

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_F_000             8376
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    4.881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.433
_exptl_absorpt_correction_T_max  0.530
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'one φ and five ω scans with 2° steps (343 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            327711
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.991
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             29722
_reflns_number_gt                24835
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.864
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. Three aromatic rings were refined as idealized 
 hexagons and restraints on bond lengths and displacement parameters
 had to be applied for several atoms, particularly in the bipy molecules and
 nitrate counter-ion. Several solvent water molecules were given occupancy
 factors of 0.5 in order to retain acceptable displacement parameters. The
 H atoms bound to three water O atoms were found on a difference Fourier
 map, but not those of the other water molecules; the C-bound H atoms were
 introduced at calculated positions; all H atoms were treated as riding atoms
 with an isotropic displacement parameter equal to 1.2 times that of the
 parent atom. Some voids in the lattice likely indicate the presence of other,
 unresolved water solvent molecules.
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0516P)²+55.5132P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.018(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         29722
_refine_ls_number_parameters     1910
_refine_ls_number_restraints     320
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0446
_refine_ls_wR_factor_ref         0.1107
_refine_ls_wR_factor_gt          0.1066
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.08577(2) 0.67056(2) 0.45736(2) 0.03659(12) Uani 1 1 d . . . . .
U2 U 0.06864(2) 0.32654(2) 0.30027(2) 0.03494(11) Uani 1 1 d . . . . .
U3 U 0.56933(2) 0.17995(2) 0.19655(2) 0.03868(12) Uani 1 1 d . . . . .
U4 U 0.56028(2) -0.16987(2) 0.04717(2) 0.03434(11) Uani 1 1 d . . . . .
Ag1 Ag 1.03560(8) 0.50439(5) 0.13003(4) 0.0699(4) Uani 1 1 d . . . . .
Ag2 Ag 0.79375(7) 0.49672(4) 0.10836(4) 0.0602(3) Uani 1 1 d . . . . .
Ag3 Ag 0.62033(8) 0.51748(5) 0.12017(4) 0.0686(4) Uani 1 1 d . . . . .
Ag4 Ag 0.42279(9) 0.49966(5) 0.12752(4) 0.0784(4) Uani 1 1 d . . . . .
Ag5 Ag 0.22005(11) 0.48764(7) 0.14082(6) 0.1110(7) Uani 1 1 d . . . . .
S1 S 0.06954(17) 0.49303(12) 0.38473(10) 0.0394(7) Uani 1 1 d . . . . .
S2 S 0.34129(17) 0.75105(12) 0.48920(12) 0.0417(8) Uani 1 1 d . . . . .
S3 S 0.32414(18) 0.25566(12) 0.25316(11) 0.0388(7) Uani 1 1 d . . . . .
S4 S -0.17594(17) 0.25507(12) 0.23915(11) 0.0399(8) Uani 1 1 d . . . . .
S5 S 0.55706(16) 0.00755(11) 0.11601(10) 0.0362(7) Uani 1 1 d . . . . .
S6 S 0.31638(17) -0.25680(12) -0.00166(12) 0.0378(7) Uani 1 1 d . . . . .
O1 O 0.0703(5) 0.7082(3) 0.4133(3) 0.051(2) Uani 1 1 d . . . . .
O2 O 0.1010(5) 0.6329(4) 0.5019(3) 0.054(3) Uani 1 1 d . . . . .
O3 O 0.0782(5) 0.3723(3) 0.2597(3) 0.047(2) Uani 1 1 d . . . . .
O4 O 0.0587(5) 0.2810(3) 0.3403(3) 0.046(2) Uani 1 1 d . . . . .
O5 O 0.5596(5) 0.2231(3) 0.1543(3) 0.049(2) Uani 1 1 d . . . . .
O6 O 0.5794(5) 0.1370(3) 0.2386(3) 0.049(2) Uani 1 1 d . . . . .
O7 O 0.5665(5) -0.1310(3) 0.0021(3) 0.048(2) Uani 1 1 d . . . . .
O8 O 0.5547(5) -0.2088(3) 0.0920(3) 0.044(2) Uani 1 1 d . . . . .
O9 O 0.0995(5) 0.5966(3) 0.4129(3) 0.053(3) Uani 1 1 d . . . . .
O10 O -0.0107(4) 0.6139(3) 0.4341(4) 0.057(3) Uani 1 1 d . . . . .
O11 O -0.0268(4) 0.3793(3) 0.3326(3) 0.045(2) Uani 1 1 d . . . . .
O12 O 0.0878(4) 0.3921(3) 0.3537(3) 0.041(2) Uani 1 1 d . . . . .
O13 O 0.1915(4) 0.7201(3) 0.4760(3) 0.042(2) Uani 1 1 d . . . . .
O14 O 0.2116(4) 0.6574(3) 0.4336(3) 0.050(2) Uani 1 1 d . . . . .
O15 O 0.4654(5) 0.8070(4) 0.5171(4) 0.057(3) Uani 1 1 d . . . . .
O16 O 0.5527(4) 0.7576(3) 0.4956(3) 0.046(2) Uani 1 1 d . . . . .
O17 O 0.1957(4) 0.3379(3) 0.3216(3) 0.044(2) Uani 1 1 d . . . . .
O18 O 0.1754(5) 0.2835(4) 0.2717(3) 0.057(3) Uani 1 1 d . . . . .
O19 O 0.4481(5) 0.2019(4) 0.2196(3) 0.054(3) Uani 1 1 d . . . . .
O20 O 0.5355(5) 0.2443(4) 0.2505(3) 0.051(3) Uani 1 1 d . . . . .
O21 O 0.0334(5) 0.2650(3) 0.2446(3) 0.046(2) Uani 1 1 d . . . . .
O22 O -0.0530(5) 0.3060(3) 0.2752(3) 0.044(2) Uani 1 1 d . . . . .
O23 O -0.3245(5) 0.2261(3) 0.2202(3) 0.049(2) Uani 1 1 d . . . . .
O24 O -0.3033(4) 0.1670(3) 0.1746(3) 0.043(2) Uani 1 1 d . . . . .
O25 O 0.5843(4) 0.1085(3) 0.1481(3) 0.042(2) Uani 1 1 d . . . . .
O26 O 0.4731(5) 0.1280(3) 0.1647(3) 0.045(2) Uani 1 1 d . . . . .
O27 O 0.5784(5) -0.0955(3) 0.0900(3) 0.048(2) Uani 1 1 d . . . . .
O28 O 0.4649(5) -0.1137(3) 0.0756(3) 0.050(2) Uani 1 1 d . . . . .
O29 O 0.4380(5) -0.1977(3) 0.0276(3) 0.048(2) Uani 1 1 d . . . . .
O30 O 0.5265(4) -0.2396(3) -0.0010(3) 0.044(2) Uani 1 1 d . . . . .
O31 O 0.1660(4) -0.2838(3) -0.0211(3) 0.045(2) Uani 1 1 d . . . . .
O32 O 0.1886(4) -0.3439(4) -0.0672(3) 0.050(2) Uani 1 1 d . . . . .
O33 O 0.2502(13) -0.0168(8) 0.1567(8) 0.220(8) Uani 1 1 d D U . . .
O34 O 0.2025(12) 0.0569(8) 0.1711(6) 0.194(8) Uani 1 1 d D U . . .
O35 O 0.2465(10) 0.0399(9) 0.1070(6) 0.186(8) Uani 1 1 d D U . . .
O36 O -0.1409(11) 0.6833(8) 0.4137(7) 0.074(7) Uani 0.5 1 d . . P . .
H36A H -0.1912 0.6843 0.4046 0.089 Uiso 0.5 1 d R U P . .
H36B H -0.1056 0.6964 0.3954 0.089 Uiso 0.5 1 d R U P . .
O37 O -0.1340(9) 0.5831(6) 0.4928(7) 0.137(7) Uani 1 1 d . . . . .
O38 O 0.2724(8) 0.5711(4) 0.3862(4) 0.082(4) Uani 1 1 d . . . . .
O39 O 0.6200(6) 0.6764(5) 0.4499(4) 0.090(4) Uani 1 1 d . . . . .
H39A H 0.6143 0.6881 0.4230 0.108 Uiso 1 1 d R U . . .
H39B H 0.6521 0.6512 0.4507 0.108 Uiso 1 1 d R U . . .
O40 O 0.1434(15) 0.1808(8) 0.2312(7) 0.081(7) Uani 0.5 1 d . . P . .
H40A H 0.1770 0.1633 0.2515 0.097 Uiso 0.5 1 d R U P . .
H40B H 0.1725 0.1995 0.2108 0.097 Uiso 0.5 1 d R U P . .
O41 O 0.3583(11) 0.1990(6) 0.1345(6) 0.054(5) Uani 0.5 1 d . . P . .
O42 O 0.2306(14) 0.1021(8) 0.2537(6) 0.073(7) Uani 0.5 1 d . . P . .
O43 O 0.2564(11) 0.1147(10) 0.0452(7) 0.081(7) Uani 0.5 1 d . U P . .
O44 O 0.0802(17) 0.1388(10) 0.1644(7) 0.102(10) Uani 0.5 1 d . . P . .
N2 N 1.0590(8) 0.5939(5) 0.1296(4) 0.060(3) Uani 1 1 d . . . . .
N3 N 0.9848(6) 0.4795(5) 0.0671(4) 0.053(3) Uani 1 1 d . . . . .
N4 N 1.0449(7) 0.4151(5) 0.1248(4) 0.055(3) Uani 1 1 d . . . . .
N5 N 0.8475(6) 0.5754(4) 0.1150(4) 0.049(3) Uani 1 1 d . . . . .
N6 N 0.7703(6) 0.5397(4) 0.0469(4) 0.045(3) Uani 1 1 d . . . . .
N7 N 0.8183(6) 0.4126(4) 0.0990(4) 0.048(3) Uani 1 1 d . . . . .
N8 N 0.8046(7) 0.4612(4) 0.1757(4) 0.059(3) Uani 1 1 d . . . . .
N9 N 0.6580(7) 0.6002(5) 0.1195(4) 0.056(3) Uani 1 1 d . . . . .
N10 N 0.5817(6) 0.5527(5) 0.0577(4) 0.055(3) Uani 1 1 d . . . . .
N13 N 0.4428(8) 0.5858(5) 0.1238(5) 0.069(4) Uani 1 1 d . . . . .
N14 N 0.3831(7) 0.5273(5) 0.0633(4) 0.058(3) Uani 1 1 d . . . . .
N15 N 0.4449(8) 0.4160(5) 0.1328(5) 0.064(4) Uani 1 1 d . . . . .
N16 N 0.4157(7) 0.4769(5) 0.1982(4) 0.065(4) Uani 1 1 d . . . . .
N17 N 0.2151(10) 0.4952(7) 0.2150(5) 0.101(6) Uani 1 1 d . . . . .
N18 N 0.2468(7) 0.5669(6) 0.1591(5) 0.078(4) Uani 1 1 d . . . . .
N19 N 0.1790(7) 0.4787(6) 0.0704(5) 0.068(4) Uani 1 1 d . . . . .
N20 N 0.2426(7) 0.4087(7) 0.1208(5) 0.078(4) Uani 1 1 d . U . . .
N21 N 0.2371(16) 0.0284(8) 0.1458(7) 0.185(7) Uani 1 1 d D U . . .
C1 C 0.0338(6) 0.5845(5) 0.4156(5) 0.044(3) Uani 1 1 d . . . . .
C2 C 0.0081(7) 0.5374(5) 0.3987(5) 0.045(3) Uani 1 1 d . . . . .
C3 C -0.0631(7) 0.5227(5) 0.3915(4) 0.044(3) Uani 1 1 d . . . . .
H3 H -0.1041 0.5430 0.3970 0.053 Uiso 1 1 calc R U . . .
C4 C -0.0668(7) 0.4745(5) 0.3752(4) 0.046(3) Uani 1 1 d . . . . .
H4 H -0.1108 0.4580 0.3685 0.055 Uiso 1 1 calc R U . . .
C5 C 0.0012(6) 0.4535(5) 0.3701(4) 0.039(3) Uani 1 1 d . . . . .
C6 C 0.0216(7) 0.4050(5) 0.3519(4) 0.041(3) Uani 1 1 d . . . . .
C7 C 0.2335(6) 0.6936(4) 0.4559(5) 0.040(3) Uani 1 1 d . . . . .
C8 C 0.3123(6) 0.7042(4) 0.4575(4) 0.036(3) Uani 1 1 d . . . . .
C9 C 0.3686(6) 0.6797(5) 0.4384(4) 0.038(3) Uani 1 1 d . . . . .
H9 H 0.3624 0.6532 0.4189 0.045 Uiso 1 1 calc R U . . .
C10 C 0.4367(6) 0.6983(4) 0.4508(4) 0.042(3) Uani 1 1 d . . . . .
H10 H 0.4816 0.6853 0.4412 0.050 Uiso 1 1 calc R U . . .
C11 C 0.4302(6) 0.7377(4) 0.4785(4) 0.035(3) Uani 1 1 d . . . . .
C12 C 0.4856(7) 0.7681(5) 0.4975(4) 0.041(3) Uani 1 1 d . . . . .
C13 C 0.2179(7) 0.3064(5) 0.2954(4) 0.040(3) Uani 1 1 d . . . . .
C14 C 0.2958(7) 0.2953(4) 0.2920(4) 0.039(3) Uani 1 1 d . . . . .
C15 C 0.3522(6) 0.3154(4) 0.3158(4) 0.040(3) Uani 1 1 d . . . . .
H15 H 0.3466 0.3396 0.3375 0.048 Uiso 1 1 calc R U . . .
C16 C 0.4186(6) 0.2947(5) 0.3029(4) 0.041(3) Uani 1 1 d . . . . .
H16 H 0.4634 0.3018 0.3163 0.049 Uiso 1 1 calc R U . . .
C17 C 0.4120(6) 0.2637(4) 0.2695(4) 0.039(3) Uani 1 1 d D . . . .
C18 C 0.4700(7) 0.2353(5) 0.2450(5) 0.052(4) Uani 1 1 d D . . . .
C19 C -0.0321(6) 0.2738(4) 0.2505(4) 0.035(3) Uani 1 1 d . . . . .
C20 C -0.0875(6) 0.2465(4) 0.2253(4) 0.036(3) Uani 1 1 d . . . . .
C21 C -0.0802(6) 0.2144(5) 0.1920(5) 0.045(3) Uani 1 1 d . . . . .
H21 H -0.0351 0.2067 0.1792 0.053 Uiso 1 1 calc R U . . .
C22 C -0.1468(7) 0.1940(5) 0.1787(5) 0.045(3) Uani 1 1 d . . . . .
H22 H -0.1519 0.1702 0.1567 0.054 Uiso 1 1 calc R U . . .
C23 C -0.2020(7) 0.2130(4) 0.2013(4) 0.041(3) Uani 1 1 d . . . . .
C24 C -0.2815(7) 0.2011(5) 0.1988(5) 0.041(3) Uani 1 1 d . . . . .
C25 C 0.5181(6) 0.0989(5) 0.1482(4) 0.036(3) Uani 1 1 d . . . . .
C26 C 0.4943(6) 0.0512(4) 0.1314(4) 0.033(3) Uani 1 1 d . . . . .
C27 C 0.4246(7) 0.0330(4) 0.1281(4) 0.039(3) Uani 1 1 d . . . . .
H27 H 0.3828 0.0518 0.1353 0.047 Uiso 1 1 calc R U . . .
C28 C 0.4216(6) -0.0167(5) 0.1128(4) 0.040(3) Uani 1 1 d . . . . .
H28 H 0.3783 -0.0348 0.1077 0.049 Uiso 1 1 calc R U . . .
C29 C 0.4907(6) -0.0350(5) 0.1064(4) 0.041(3) Uani 1 1 d . . . . .
C30 C 0.5119(6) -0.0824(5) 0.0903(4) 0.040(3) Uani 1 1 d . . . . .
C31 C 0.4602(7) -0.2321(5) 0.0037(4) 0.039(3) Uani 1 1 d . . . . .
C32 C 0.4040(7) -0.2610(5) -0.0180(4) 0.039(3) Uani 1 1 d . . . . .
C33 C 0.4113(6) -0.2925(5) -0.0530(4) 0.037(3) Uani 1 1 d . . . . .
H33 H 0.4563 -0.2994 -0.0663 0.044 Uiso 1 1 calc R U . . .
C34 C 0.3439(6) -0.3132(5) -0.0664(4) 0.038(3) Uani 1 1 d . . . . .
H34 H 0.3384 -0.3353 -0.0897 0.046 Uiso 1 1 calc R U . . .
C35 C 0.2886(6) -0.2971(4) -0.0414(4) 0.038(3) Uani 1 1 d . . . . .
C36 C 0.2097(6) -0.3091(5) -0.0428(4) 0.038(3) Uani 1 1 d . . . . .
N1 N 1.0352(8) 0.5320(5) 0.1971(3) 0.092(4) Uani 1 1 d G U . . .
C37 C 1.0235(9) 0.4993(4) 0.2305(5) 0.114(5) Uani 1 1 d G U . . .
H37 H 1.0116 0.4655 0.2249 0.137 Uiso 1 1 calc R U . . .
C38 C 1.0292(10) 0.5160(6) 0.2720(4) 0.143(6) Uani 1 1 d G U . . .
H38 H 1.0213 0.4936 0.2948 0.171 Uiso 1 1 calc R U . . .
C39 C 1.0467(10) 0.5654(7) 0.2801(3) 0.146(6) Uani 1 1 d G U . . .
H39 H 1.0506 0.5768 0.3085 0.175 Uiso 1 1 calc R U . . .
C40 C 1.0583(10) 0.5981(5) 0.2467(5) 0.123(6) Uani 1 1 d G U . . .
H40 H 1.0702 0.6318 0.2522 0.148 Uiso 1 1 calc R U . . .
C41 C 1.0526(9) 0.5813(5) 0.2052(4) 0.096(5) Uani 1 1 d G U . . .
C42 C 1.0641(9) 0.6139(6) 0.1692(5) 0.061(4) Uani 1 1 d . . . . .
C43 C 1.0728(9) 0.6652(7) 0.1739(6) 0.076(5) Uani 1 1 d . . . . .
H43 H 1.0753 0.6797 0.2013 0.091 Uiso 1 1 calc R U . . .
C44 C 1.0775(10) 0.6937(7) 0.1388(7) 0.078(5) Uani 1 1 d . . . . .
H44 H 1.0830 0.7287 0.1415 0.093 Uiso 1 1 calc R U . . .
C45 C 1.0745(9) 0.6727(6) 0.0999(6) 0.068(4) Uani 1 1 d . . . . .
H45 H 1.0794 0.6923 0.0750 0.081 Uiso 1 1 calc R U . . .
C46 C 1.0645(10) 0.6238(6) 0.0977(5) 0.066(4) Uani 1 1 d . . . . .
H46 H 1.0610 0.6095 0.0703 0.079 Uiso 1 1 calc R U . . .
C47 C 0.9596(9) 0.5120(8) 0.0386(5) 0.082(6) Uani 1 1 d . . . . .
H47 H 0.9556 0.5458 0.0470 0.098 Uiso 1 1 calc R U . . .
C48 C 0.9394(9) 0.5002(8) -0.0014(5) 0.072(5) Uani 1 1 d . . . . .
H48 H 0.9192 0.5239 -0.0204 0.086 Uiso 1 1 calc R U . . .
C49 C 0.9507(9) 0.4510(8) -0.0124(5) 0.076(5) Uani 1 1 d . . . . .
H49 H 0.9402 0.4412 -0.0406 0.091 Uiso 1 1 calc R U . . .
C50 C 0.9756(10) 0.4161(7) 0.0146(5) 0.071(5) Uani 1 1 d . . . . .
H50 H 0.9821 0.3826 0.0059 0.085 Uiso 1 1 calc R U . . .
C51 C 0.9913(7) 0.4312(6) 0.0555(5) 0.054(4) Uani 1 1 d . . . . .
C52 C 1.0171(8) 0.3954(6) 0.0896(5) 0.054(4) Uani 1 1 d . . . . .
C53 C 1.0089(10) 0.3441(6) 0.0844(6) 0.072(5) Uani 1 1 d . . . . .
H53 H 0.9871 0.3303 0.0597 0.086 Uiso 1 1 calc R U . . .
C54 C 1.0344(10) 0.3141(7) 0.1171(6) 0.074(5) Uani 1 1 d . . . . .
H54 H 1.0327 0.2789 0.1144 0.089 Uiso 1 1 calc R U . . .
C55 C 1.0614(10) 0.3349(8) 0.1526(6) 0.083(5) Uani 1 1 d . . . . .
H55 H 1.0785 0.3147 0.1751 0.099 Uiso 1 1 calc R U . . .
C56 C 1.0638(10) 0.3843(7) 0.1555(6) 0.073(5) Uani 1 1 d . . . . .
H56 H 1.0801 0.3984 0.1814 0.087 Uiso 1 1 calc R U . . .
C57 C 0.8732(9) 0.5949(6) 0.1508(5) 0.064(4) Uani 1 1 d . . . . .
H57 H 0.8817 0.5732 0.1740 0.077 Uiso 1 1 calc R U . . .
C58 C 0.8886(9) 0.6462(7) 0.1562(6) 0.073(5) Uani 1 1 d . . . . .
H58 H 0.9079 0.6586 0.1820 0.087 Uiso 1 1 calc R U . . .
C59 C 0.8742(9) 0.6777(6) 0.1222(6) 0.077(5) Uani 1 1 d . . . . .
H59 H 0.8819 0.7126 0.1243 0.093 Uiso 1 1 calc R U . . .
C60 C 0.8483(7) 0.6563(5) 0.0850(5) 0.049(4) Uani 1 1 d . . . . .
H60 H 0.8400 0.6769 0.0611 0.059 Uiso 1 1 calc R U . . .
C61 C 0.8347(7) 0.6069(5) 0.0820(5) 0.042(3) Uani 1 1 d . . . . .
C62 C 0.8054(6) 0.5834(4) 0.0431(4) 0.042(3) Uani 1 1 d . . . . .
C63 C 0.8109(8) 0.6071(5) 0.0034(5) 0.050(4) Uani 1 1 d . . . . .
H63 H 0.8341 0.6386 0.0014 0.060 Uiso 1 1 calc R U . . .
C64 C 0.7834(9) 0.5855(6) -0.0324(5) 0.066(4) Uani 1 1 d . . . . .
H64 H 0.7895 0.6004 -0.0594 0.079 Uiso 1 1 calc R U . . .
C65 C 0.7463(8) 0.5413(6) -0.0277(5) 0.060(4) Uani 1 1 d . . . . .
H65 H 0.7244 0.5259 -0.0516 0.072 Uiso 1 1 calc R U . . .
C66 C 0.7410(7) 0.5193(5) 0.0122(5) 0.054(4) Uani 1 1 d . . . . .
H66 H 0.7158 0.4886 0.0148 0.064 Uiso 1 1 calc R U . . .
C67 C 0.8137(8) 0.3880(5) 0.0639(5) 0.053(4) Uani 1 1 d . . . . .
H67 H 0.8070 0.4062 0.0384 0.063 Uiso 1 1 calc R U . . .
C68 C 0.8181(8) 0.3374(5) 0.0615(6) 0.061(4) Uani 1 1 d . . . . .
H68 H 0.8145 0.3210 0.0349 0.074 Uiso 1 1 calc R U . . .
C69 C 0.8276(9) 0.3107(6) 0.0977(6) 0.068(5) Uani 1 1 d . . . . .
H69 H 0.8319 0.2755 0.0965 0.082 Uiso 1 1 calc R U . . .
C70 C 0.8307(8) 0.3340(5) 0.1345(6) 0.062(4) Uani 1 1 d . . . . .
H70 H 0.8335 0.3152 0.1599 0.075 Uiso 1 1 calc R U . . .
C71 C 0.8300(8) 0.3864(5) 0.1365(5) 0.049(3) Uani 1 1 d . . . . .
C72 C 0.8330(9) 0.4139(6) 0.1749(5) 0.063(4) Uani 1 1 d . . . . .
C73 C 0.8695(10) 0.3964(6) 0.2125(6) 0.075(5) Uani 1 1 d . . . . .
H73 H 0.8952 0.3658 0.2117 0.090 Uiso 1 1 calc R U . . .
C74 C 0.8677(12) 0.4232(6) 0.2492(6) 0.078(5) Uani 1 1 d . . . . .
H74 H 0.8876 0.4094 0.2743 0.094 Uiso 1 1 calc R U . . .
C75 C 0.8373(14) 0.4700(7) 0.2500(7) 0.104(8) Uani 1 1 d . . . . .
H75 H 0.8362 0.4892 0.2752 0.125 Uiso 1 1 calc R U . . .
C76 C 0.8085(13) 0.4878(7) 0.2126(7) 0.096(7) Uani 1 1 d . . . . .
H76 H 0.7901 0.5208 0.2125 0.115 Uiso 1 1 calc R U . . .
C77 C 0.6885(10) 0.6239(7) 0.1519(6) 0.075(5) Uani 1 1 d . . . . .
H77 H 0.7054 0.6051 0.1753 0.090 Uiso 1 1 calc R U . . .
C78 C 0.6963(9) 0.6757(7) 0.1523(6) 0.071(5) Uani 1 1 d . . . . .
H78 H 0.7184 0.6918 0.1757 0.086 Uiso 1 1 calc R U . . .
C79 C 0.6722(11) 0.7023(6) 0.1193(7) 0.083(6) Uani 1 1 d . . . . .
H79 H 0.6738 0.7376 0.1205 0.100 Uiso 1 1 calc R U . . .
C80 C 0.6450(8) 0.6793(6) 0.0838(6) 0.065(4) Uani 1 1 d . . . . .
H80 H 0.6327 0.6978 0.0592 0.078 Uiso 1 1 calc R U . . .
C81 C 0.6361(8) 0.6272(6) 0.0851(5) 0.051(4) Uani 1 1 d . . . . .
C82 C 0.6042(7) 0.6010(6) 0.0511(5) 0.060(4) Uani 1 1 d . . . . .
C83 C 0.5952(10) 0.6245(9) 0.0083(6) 0.086(6) Uani 1 1 d . . . . .
H83 H 0.6099 0.6578 0.0033 0.104 Uiso 1 1 calc R U . . .
C84 C 0.5649(11) 0.5962(10) -0.0232(7) 0.093(6) Uani 1 1 d . . . . .
H84 H 0.5600 0.6093 -0.0510 0.111 Uiso 1 1 calc R U . . .
C85 C 0.5425(10) 0.5508(10) -0.0148(6) 0.089(7) Uani 1 1 d . . . . .
H85 H 0.5189 0.5329 -0.0367 0.107 Uiso 1 1 calc R U . . .
C86 C 0.5514(8) 0.5273(7) 0.0242(6) 0.067(5) Uani 1 1 d . . . . .
H86 H 0.5366 0.4937 0.0277 0.080 Uiso 1 1 calc R U . . .
N11 N 0.6363(7) 0.4376(5) 0.1300(6) 0.112(5) Uani 1 1 d G U . . .
C87 C 0.6366(8) 0.4023(7) 0.0979(5) 0.110(5) Uani 1 1 d G U . . .
H87 H 0.6380 0.4127 0.0691 0.133 Uiso 1 1 calc R U . . .
C88 C 0.6348(8) 0.3520(6) 0.1078(6) 0.120(6) Uani 1 1 d G U . . .
H88 H 0.6351 0.3279 0.0858 0.144 Uiso 1 1 calc R U . . .
C89 C 0.6328(8) 0.3369(5) 0.1498(7) 0.127(6) Uani 1 1 d G U . . .
H89 H 0.6316 0.3025 0.1566 0.153 Uiso 1 1 calc R U . . .
C90 C 0.6325(9) 0.3721(7) 0.1820(5) 0.139(6) Uani 1 1 d G U . . .
H90 H 0.6311 0.3618 0.2108 0.167 Uiso 1 1 calc R U . . .
C91 C 0.6342(9) 0.4225(6) 0.1721(5) 0.129(5) Uani 1 1 d G U . . .
N12 N 0.6082(10) 0.5007(10) 0.1921(5) 0.155(6) Uani 1 1 d G U . . .
C92 C 0.6259(12) 0.4531(8) 0.2057(7) 0.154(6) Uani 1 1 d G U . . .
C93 C 0.6425(12) 0.4446(7) 0.2481(8) 0.176(7) Uani 1 1 d G U . . .
H93 H 0.6546 0.4121 0.2574 0.211 Uiso 1 1 calc R U . . .
C94 C 0.6414(12) 0.4839(11) 0.2767(5) 0.180(8) Uani 1 1 d G U . . .
H94 H 0.6528 0.4781 0.3056 0.216 Uiso 1 1 calc R U . . .
C95 C 0.6237(12) 0.5315(9) 0.2631(7) 0.182(8) Uani 1 1 d G U . . .
H95 H 0.6230 0.5583 0.2827 0.218 Uiso 1 1 calc R U . . .
C96 C 0.6072(11) 0.5399(7) 0.2208(8) 0.170(7) Uani 1 1 d G U . . .
H96 H 0.5951 0.5725 0.2114 0.205 Uiso 1 1 calc R U . . .
C97 C 0.4710(13) 0.6122(8) 0.1545(8) 0.092(7) Uani 1 1 d . . . . .
H97 H 0.4881 0.5960 0.1792 0.110 Uiso 1 1 calc R U . . .
C98 C 0.4764(12) 0.6648(9) 0.1510(8) 0.104(7) Uani 1 1 d . . . . .
H98 H 0.4939 0.6842 0.1740 0.125 Uiso 1 1 calc R U . . .
C99 C 0.4556(11) 0.6873(8) 0.1135(7) 0.088(6) Uani 1 1 d . . . . .
H99 H 0.4600 0.7223 0.1100 0.105 Uiso 1 1 calc R U . . .
C100 C 0.4297(9) 0.6594(6) 0.0830(6) 0.070(5) Uani 1 1 d . . . . .
H100 H 0.4156 0.6751 0.0574 0.084 Uiso 1 1 calc R U . . .
C101 C 0.4218(8) 0.6077(6) 0.0864(5) 0.059(4) Uani 1 1 d . . . . .
C102 C 0.3914(8) 0.5736(6) 0.0536(5) 0.061(4) Uani 1 1 d . . . . .
C103 C 0.3688(11) 0.5929(8) 0.0128(6) 0.084(6) Uani 1 1 d . . . . .
H103 H 0.3715 0.6276 0.0072 0.100 Uiso 1 1 calc R U . . .
C104 C 0.3446(11) 0.5623(10) -0.0163(6) 0.088(6) Uani 1 1 d . . . . .
H104 H 0.3294 0.5748 -0.0429 0.105 Uiso 1 1 calc R U . . .
C105 C 0.3413(9) 0.5114(8) -0.0081(6) 0.075(5) Uani 1 1 d . . . . .
H105 H 0.3281 0.4878 -0.0291 0.090 Uiso 1 1 calc R U . . .
C106 C 0.3586(8) 0.4981(8) 0.0326(6) 0.078(6) Uani 1 1 d . . . . .
H106 H 0.3523 0.4640 0.0397 0.093 Uiso 1 1 calc R U . . .
C107 C 0.4484(10) 0.3852(7) 0.1005(7) 0.078(6) Uani 1 1 d . . . . .
H107 H 0.4543 0.3998 0.0734 0.093 Uiso 1 1 calc R U . . .
C108 C 0.4442(8) 0.3316(6) 0.1017(6) 0.070(4) Uani 1 1 d . . . . .
H108 H 0.4435 0.3117 0.0769 0.085 Uiso 1 1 calc R U . . .
C109 C 0.4412(9) 0.3117(6) 0.1426(7) 0.076(5) Uani 1 1 d . . . . .
H109 H 0.4395 0.2768 0.1468 0.091 Uiso 1 1 calc R U . . .
C110 C 0.4408(10) 0.3435(6) 0.1761(6) 0.073(5) Uani 1 1 d . . . . .
H110 H 0.4400 0.3299 0.2039 0.087 Uiso 1 1 calc R U . . .
C111 C 0.4415(9) 0.3954(6) 0.1715(6) 0.065(5) Uani 1 1 d . . . . .
C112 C 0.4366(12) 0.4292(6) 0.2053(5) 0.081(6) Uani 1 1 d . . . . .
C113 C 0.4593(16) 0.4151(11) 0.2459(9) 0.133(10) Uani 1 1 d . U . . .
H113 H 0.4816 0.3837 0.2503 0.160 Uiso 1 1 calc R U . . .
C114 C 0.4480(18) 0.4502(11) 0.2827(10) 0.148(11) Uani 1 1 d . U . . .
H114 H 0.4595 0.4422 0.3112 0.177 Uiso 1 1 calc R U . . .
C115 C 0.4182(15) 0.4969(10) 0.2697(8) 0.127(9) Uani 1 1 d . U . . .
H115 H 0.4050 0.5199 0.2912 0.152 Uiso 1 1 calc R U . . .
C116 C 0.4074(10) 0.5105(7) 0.2295(6) 0.076(5) Uani 1 1 d . . . . .
H116 H 0.3939 0.5437 0.2230 0.091 Uiso 1 1 calc R U . . .
C117 C 0.2051(13) 0.4551(9) 0.2452(8) 0.107(7) Uani 1 1 d . U . . .
H117 H 0.1918 0.4234 0.2345 0.128 Uiso 1 1 calc R U . . .
C118 C 0.2137(14) 0.4600(9) 0.2882(8) 0.113(8) Uani 1 1 d D U . . .
H118 H 0.2030 0.4325 0.3059 0.136 Uiso 1 1 calc R U . . .
C119 C 0.2378(16) 0.5048(9) 0.3068(10) 0.146(11) Uani 1 1 d D U . . .
H119 H 0.2475 0.5090 0.3361 0.175 Uiso 1 1 calc R U . . .
C120 C 0.2458(13) 0.5437(9) 0.2750(7) 0.103(7) Uani 1 1 d . U . . .
H120 H 0.2608 0.5753 0.2851 0.124 Uiso 1 1 calc R U . . .
C121 C 0.2337(11) 0.5396(8) 0.2301(6) 0.083(6) Uani 1 1 d . . . . .
C122 C 0.2469(9) 0.5795(7) 0.2004(6) 0.071(5) Uani 1 1 d . . . . .
C123 C 0.2614(11) 0.6275(8) 0.2123(7) 0.083(6) Uani 1 1 d . . . . .
H123 H 0.2651 0.6353 0.2415 0.100 Uiso 1 1 calc R U . . .
C124 C 0.2703(10) 0.6636(8) 0.1835(7) 0.081(5) Uani 1 1 d . . . . .
H124 H 0.2798 0.6965 0.1932 0.097 Uiso 1 1 calc R U . . .
C125 C 0.2661(9) 0.6548(8) 0.1383(7) 0.086(6) Uani 1 1 d . . . . .
H125 H 0.2709 0.6796 0.1170 0.103 Uiso 1 1 calc R U . . .
C126 C 0.2538(9) 0.6040(8) 0.1307(7) 0.082(6) Uani 1 1 d . . . . .
H126 H 0.2498 0.5946 0.1018 0.098 Uiso 1 1 calc R U . . .
C127 C 0.1599(9) 0.5146(8) 0.0450(8) 0.090(7) Uani 1 1 d . . . . .
H127 H 0.1512 0.5464 0.0571 0.109 Uiso 1 1 calc R U . . .
C128 C 0.1514(11) 0.5097(9) 0.0016(7) 0.091(6) Uani 1 1 d . . . . .
H128 H 0.1354 0.5371 -0.0149 0.109 Uiso 1 1 calc R U . . .
C129 C 0.1662(10) 0.4654(8) -0.0170(8) 0.094(7) Uani 1 1 d . . . . .
H129 H 0.1633 0.4604 -0.0467 0.113 Uiso 1 1 calc R U . . .
C130 C 0.1862(10) 0.4275(8) 0.0112(7) 0.084(6) Uani 1 1 d . . . . .
H130 H 0.1955 0.3955 -0.0003 0.101 Uiso 1 1 calc R U . . .
C131 C 0.1933(7) 0.4332(7) 0.0534(5) 0.067(5) Uani 1 1 d . . . . .
C132 C 0.2166(9) 0.3940(7) 0.0833(6) 0.069(4) Uani 1 1 d . U . . .
C133 C 0.2133(11) 0.3454(7) 0.0728(7) 0.085(4) Uani 1 1 d . U . . .
H133 H 0.1948 0.3370 0.0456 0.102 Uiso 1 1 calc R U . . .
C134 C 0.2344(12) 0.3082(9) 0.0981(7) 0.097(5) Uani 1 1 d . U . . .
H134 H 0.2350 0.2745 0.0890 0.117 Uiso 1 1 calc R U . . .
C135 C 0.2550(10) 0.3220(10) 0.1382(7) 0.098(5) Uani 1 1 d . U . . .
H135 H 0.2650 0.2983 0.1598 0.117 Uiso 1 1 calc R U . . .
C136 C 0.2606(10) 0.3741(9) 0.1456(7) 0.090(5) Uani 1 1 d . U . . .
H136 H 0.2801 0.3839 0.1721 0.108 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.745(9) . ?
U1 O2 1.755(10) . ?
U1 O13 2.438(8) . ?
U1 O15 2.442(8) 4_466 ?
U1 O9 2.448(8) . ?
U1 O10 2.458(8) . ?
U1 O14 2.469(8) . ?
U1 O16 2.513(8) 4_466 ?
U2 O4 1.770(9) . ?
U2 O3 1.785(9) . ?
U2 O22 2.448(8) . ?
U2 O18 2.459(9) . ?
U2 O17 2.462(8) . ?
U2 O12 2.466(8) . ?
U2 O11 2.483(8) . ?
U2 O21 2.501(9) . ?
U3 O6 1.770(9) . ?
U3 O5 1.777(9) . ?
U3 O19 2.429(8) . ?
U3 O23 2.439(8) 1_655 ?
U3 O25 2.471(8) . ?
U3 O26 2.475(9) . ?
U3 O24 2.479(7) 1_655 ?
U3 O20 2.508(9) . ?
U4 O8 1.762(8) . ?
U4 O7 1.771(9) . ?
U4 O27 2.437(8) . ?
U4 O31 2.458(8) 4_545 ?
U4 O29 2.460(8) . ?
U4 O32 2.483(8) 4_545 ?
U4 O28 2.489(9) . ?
U4 O30 2.495(9) . ?
Ag1 N1 2.244(10) . ?
Ag1 N3 2.298(12) . ?
Ag1 N4 2.413(13) . ?
Ag1 N2 2.444(13) . ?
Ag2 N6 2.301(12) . ?
Ag2 N7 2.326(11) . ?
Ag2 N8 2.342(13) . ?
Ag2 N5 2.345(11) . ?
Ag2 Ag3 3.2752(19) . ?
Ag3 N11 2.190(12) . ?
Ag3 N10 2.304(13) . ?
Ag3 N12 2.327(16) . ?
Ag3 N9 2.331(13) . ?
Ag4 N14 2.282(13) . ?
Ag4 N15 2.293(14) . ?
Ag4 N16 2.319(13) . ?
Ag4 N13 2.349(14) . ?
Ag5 N20 2.254(17) . ?
Ag5 N18 2.262(16) . ?
Ag5 N17 2.354(16) . ?
Ag5 N19 2.361(15) . ?
S1 C2 1.705(13) . ?
S1 C5 1.715(12) . ?
S2 C8 1.697(12) . ?
S2 C11 1.717(12) . ?
S3 C14 1.707(13) . ?
S3 C17 1.717(12) . ?
S4 C20 1.708(12) . ?
S4 C23 1.715(13) . ?
S5 C29 1.705(12) . ?
S5 C26 1.721(12) . ?
S6 C32 1.705(13) . ?
S6 C35 1.737(13) . ?
O9 C1 1.260(14) . ?
O10 C1 1.282(15) . ?
O11 C6 1.285(15) . ?
O12 C6 1.273(15) . ?
O13 C7 1.229(14) . ?
O14 C7 1.269(15) . ?
O15 C12 1.273(15) . ?
O15 U1 2.442(8) 4_566 ?
O16 C12 1.273(15) . ?
O16 U1 2.514(8) 4_566 ?
O17 C13 1.252(14) . ?
O18 C13 1.246(16) . ?
O19 C18 1.270(17) . ?
O20 C18 1.247(16) . ?
O21 C19 1.248(14) . ?
O22 C19 1.227(15) . ?
O23 C24 1.242(16) . ?
O23 U3 2.439(8) 1_455 ?
O24 C24 1.260(15) . ?
O24 U3 2.480(7) 1_455 ?
O25 C25 1.251(14) . ?
O26 C25 1.256(14) . ?
O27 C30 1.280(15) . ?
O28 C30 1.294(15) . ?
O29 C31 1.264(15) . ?
O30 C31 1.249(15) . ?
O31 C36 1.258(15) . ?
O31 U4 2.458(8) 4_445 ?
O32 C36 1.277(14) . ?
O32 U4 2.483(8) 4_445 ?
O33 N21 1.287(12) . ?
O34 N21 1.277(12) . ?
O35 N21 1.277(12) . ?
O36 H36A 0.9736 . ?
O36 H36B 0.9402 . ?
O39 H39A 0.9109 . ?
O39 H39B 0.9025 . ?
O40 H40A 1.0096 . ?
O40 H40B 0.9782 . ?
N2 C46 1.293(19) . ?
N2 C42 1.366(19) . ?
N3 C47 1.34(2) . ?
N3 C51 1.357(19) . ?
N4 C56 1.32(2) . ?
N4 C52 1.335(19) . ?
N5 C57 1.334(19) . ?
N5 C61 1.365(17) . ?
N6 C66 1.341(17) . ?
N6 C62 1.346(15) . ?
N7 C67 1.294(18) . ?
N7 C71 1.393(18) . ?
N8 C76 1.37(2) . ?
N8 C72 1.376(19) . ?
N9 C77 1.33(2) . ?
N9 C81 1.368(18) . ?
N10 C86 1.378(19) . ?
N10 C82 1.38(2) . ?
N13 C97 1.31(2) . ?
N13 C101 1.375(19) . ?
N14 C102 1.290(19) . ?
N14 C106 1.33(2) . ?
N15 C107 1.31(2) . ?
N15 C111 1.35(2) . ?
N16 C116 1.35(2) . ?
N16 C112 1.36(2) . ?
N17 C121 1.33(2) . ?
N17 C117 1.45(3) . ?
N18 C122 1.35(2) . ?
N18 C126 1.35(3) . ?
N19 C127 1.31(3) . ?
N19 C131 1.362(19) . ?
N20 C136 1.26(3) . ?
N20 C132 1.34(2) . ?
C1 C2 1.454(18) . ?
C2 C3 1.394(18) . ?
C3 C4 1.395(19) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(17) . ?
C4 H4 0.9500 . ?
C5 C6 1.473(17) . ?
C7 C8 1.485(15) . ?
C8 C9 1.370(16) . ?
C9 C10 1.410(16) . ?
C9 H9 0.9500 . ?
C10 C11 1.378(16) . ?
C10 H10 0.9500 . ?
C11 C12 1.441(16) . ?
C13 C14 1.475(18) . ?
C14 C15 1.394(18) . ?
C15 C16 1.408(17) . ?
C15 H15 0.9500 . ?
C16 C17 1.351(17) . ?
C16 H16 0.9500 . ?
C17 C18 1.527(11) . ?
C19 C20 1.493(16) . ?
C20 C21 1.366(17) . ?
C21 C22 1.411(17) . ?
C21 H21 0.9500 . ?
C22 C23 1.347(18) . ?
C22 H22 0.9500 . ?
C23 C24 1.506(18) . ?
C25 C26 1.455(17) . ?
C26 C27 1.383(17) . ?
C27 C28 1.422(18) . ?
C27 H27 0.9500 . ?
C28 C29 1.384(17) . ?
C28 H28 0.9500 . ?
C29 C30 1.426(17) . ?
C31 C32 1.467(17) . ?
C32 C33 1.397(18) . ?
C33 C34 1.431(16) . ?
C33 H33 0.9500 . ?
C34 C35 1.363(17) . ?
C34 H34 0.9500 . ?
C35 C36 1.493(17) . ?
N1 C37 1.3900 . ?
N1 C41 1.3900 . ?
C37 C38 1.3900 . ?
C37 H37 0.9500 . ?
C38 C39 1.3900 . ?
C38 H38 0.9500 . ?
C39 C40 1.3900 . ?
C39 H39 0.9500 . ?
C40 C41 1.3900 . ?
C40 H40 0.9500 . ?
C41 C42 1.449(19) . ?
C42 C43 1.40(2) . ?
C43 C44 1.35(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.35(2) . ?
C44 H44 0.9500 . ?
C45 C46 1.33(2) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 C48 1.35(2) . ?
C47 H47 0.9500 . ?
C48 C49 1.38(3) . ?
C48 H48 0.9500 . ?
C49 C50 1.35(2) . ?
C49 H49 0.9500 . ?
C50 C51 1.38(2) . ?
C50 H50 0.9500 . ?
C51 C52 1.52(2) . ?
C52 C53 1.40(2) . ?
C53 C54 1.39(2) . ?
C53 H53 0.9500 . ?
C54 C55 1.35(3) . ?
C54 H54 0.9500 . ?
C55 C56 1.33(3) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 C58 1.42(2) . ?
C57 H57 0.9500 . ?
C58 C59 1.39(2) . ?
C58 H58 0.9500 . ?
C59 C60 1.39(2) . ?
C59 H59 0.9500 . ?
C60 C61 1.355(18) . ?
C60 H60 0.9500 . ?
C61 C62 1.484(18) . ?
C62 C63 1.412(19) . ?
C63 C64 1.37(2) . ?
C63 H63 0.9500 . ?
C64 C65 1.38(2) . ?
C64 H64 0.9500 . ?
C65 C66 1.40(2) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C67 C68 1.37(2) . ?
C67 H67 0.9500 . ?
C68 C69 1.36(2) . ?
C68 H68 0.9500 . ?
C69 C70 1.32(2) . ?
C69 H69 0.9500 . ?
C70 C71 1.41(2) . ?
C70 H70 0.9500 . ?
C71 C72 1.42(2) . ?
C72 C73 1.44(2) . ?
C73 C74 1.36(2) . ?
C73 H73 0.9500 . ?
C74 C75 1.38(2) . ?
C74 H74 0.9500 . ?
C75 C76 1.38(3) . ?
C75 H75 0.9500 . ?
C76 H76 0.9500 . ?
C77 C78 1.40(2) . ?
C77 H77 0.9500 . ?
C78 C79 1.34(2) . ?
C78 H78 0.9500 . ?
C79 C80 1.38(2) . ?
C79 H79 0.9500 . ?
C80 C81 1.41(2) . ?
C80 H80 0.9500 . ?
C81 C82 1.41(2) . ?
C82 C83 1.50(3) . ?
C83 C84 1.37(3) . ?
C83 H83 0.9500 . ?
C84 C85 1.32(3) . ?
C84 H84 0.9500 . ?
C85 C86 1.39(3) . ?
C85 H85 0.9500 . ?
C86 H86 0.9500 . ?
N11 C87 1.3900 . ?
N11 C91 1.3900 . ?
C87 C88 1.3900 . ?
C87 H87 0.9500 . ?
C88 C89 1.3900 . ?
C88 H88 0.9500 . ?
C89 C90 1.3900 . ?
C89 H89 0.9500 . ?
C90 C91 1.3900 . ?
C90 H90 0.9500 . ?
C91 C92 1.35(2) . ?
N12 C92 1.3900 . ?
N12 C96 1.3900 . ?
C92 C93 1.3900 . ?
C93 C94 1.3900 . ?
C93 H93 0.9500 . ?
C94 C95 1.3900 . ?
C94 H94 0.9500 . ?
C95 C96 1.3900 . ?
C95 H95 0.9500 . ?
C96 H96 0.9500 . ?
C97 C98 1.42(3) . ?
C97 H97 0.9500 . ?
C98 C99 1.38(3) . ?
C98 H98 0.9500 . ?
C99 C100 1.31(3) . ?
C99 H99 0.9500 . ?
C100 C101 1.40(2) . ?
C100 H100 0.9500 . ?
C101 C102 1.49(2) . ?
C102 C103 1.45(2) . ?
C103 C104 1.31(3) . ?
C103 H103 0.9500 . ?
C104 C105 1.39(3) . ?
C104 H104 0.9500 . ?
C105 C106 1.37(2) . ?
C105 H105 0.9500 . ?
C106 H106 0.9500 . ?
C107 C108 1.44(2) . ?
C107 H107 0.9500 . ?
C108 C109 1.40(3) . ?
C108 H108 0.9500 . ?
C109 C110 1.36(2) . ?
C109 H109 0.9500 . ?
C110 C111 1.40(2) . ?
C110 H110 0.9500 . ?
C111 C112 1.40(3) . ?
C112 C113 1.40(3) . ?
C113 C114 1.51(4) . ?
C113 H113 0.9500 . ?
C114 C115 1.43(3) . ?
C114 H114 0.9500 . ?
C115 C116 1.34(3) . ?
C115 H115 0.9500 . ?
C116 H116 0.9500 . ?
C117 C118 1.37(3) . ?
C117 H117 0.9500 . ?
C118 C119 1.411(13) . ?
C118 H118 0.9500 . ?
C119 C120 1.46(3) . ?
C119 H119 0.9500 . ?
C120 C121 1.44(3) . ?
C120 H120 0.9500 . ?
C121 C122 1.44(3) . ?
C122 C123 1.37(2) . ?
C123 C124 1.34(3) . ?
C123 H123 0.9500 . ?
C124 C125 1.45(3) . ?
C124 H124 0.9500 . ?
C125 C126 1.40(3) . ?
C125 H125 0.9500 . ?
C126 H126 0.9500 . ?
C127 C128 1.39(3) . ?
C127 H127 0.9500 . ?
C128 C129 1.36(3) . ?
C128 H128 0.9500 . ?
C129 C130 1.40(3) . ?
C129 H129 0.9500 . ?
C130 C131 1.35(2) . ?
C130 H130 0.9500 . ?
C131 C132 1.48(3) . ?
C132 C133 1.35(2) . ?
C133 C134 1.34(3) . ?
C133 H133 0.9500 . ?
C134 C135 1.38(3) . ?
C134 H134 0.9500 . ?
C135 C136 1.42(3) . ?
C135 H135 0.9500 . ?
C136 H136 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 179.7(5) . . ?
O1 U1 O13 90.4(4) . . ?
O2 U1 O13 89.6(4) . . ?
O1 U1 O15 88.4(4) . 4_466 ?
O2 U1 O15 91.4(4) . 4_466 ?
O13 U1 O15 121.1(3) . 4_466 ?
O1 U1 O9 91.7(4) . . ?
O2 U1 O9 88.6(4) . . ?
O13 U1 O9 120.0(3) . . ?
O15 U1 O9 119.0(3) 4_466 . ?
O1 U1 O10 90.1(4) . . ?
O2 U1 O10 89.9(4) . . ?
O13 U1 O10 173.1(3) . . ?
O15 U1 O10 65.8(3) 4_466 . ?
O9 U1 O10 53.2(3) . . ?
O1 U1 O14 89.7(4) . . ?
O2 U1 O14 90.6(4) . . ?
O13 U1 O14 52.9(3) . . ?
O15 U1 O14 173.6(3) 4_466 . ?
O9 U1 O14 67.1(3) . . ?
O10 U1 O14 120.3(3) . . ?
O1 U1 O16 89.2(4) . 4_466 ?
O2 U1 O16 90.4(4) . 4_466 ?
O13 U1 O16 68.4(3) . 4_466 ?
O15 U1 O16 52.7(3) 4_466 4_466 ?
O9 U1 O16 171.6(3) . 4_466 ?
O10 U1 O16 118.5(3) . 4_466 ?
O14 U1 O16 121.3(3) . 4_466 ?
O4 U2 O3 179.6(4) . . ?
O4 U2 O22 88.9(4) . . ?
O3 U2 O22 90.8(4) . . ?
O4 U2 O18 91.2(4) . . ?
O3 U2 O18 88.9(4) . . ?
O22 U2 O18 120.9(3) . . ?
O4 U2 O17 89.4(4) . . ?
O3 U2 O17 91.0(4) . . ?
O22 U2 O17 173.2(3) . . ?
O18 U2 O17 52.6(3) . . ?
O4 U2 O12 91.1(4) . . ?
O3 U2 O12 89.1(4) . . ?
O22 U2 O12 121.0(3) . . ?
O18 U2 O12 118.1(3) . . ?
O17 U2 O12 65.6(3) . . ?
O4 U2 O11 91.6(4) . . ?
O3 U2 O11 88.4(4) . . ?
O22 U2 O11 67.0(3) . . ?
O18 U2 O11 171.7(3) . . ?
O17 U2 O11 119.6(3) . . ?
O12 U2 O11 54.0(3) . . ?
O4 U2 O21 91.1(4) . . ?
O3 U2 O21 88.6(4) . . ?
O22 U2 O21 52.0(3) . . ?
O18 U2 O21 68.9(3) . . ?
O17 U2 O21 121.5(3) . . ?
O12 U2 O21 172.6(3) . . ?
O11 U2 O21 118.8(3) . . ?
O6 U3 O5 179.7(5) . . ?
O6 U3 O19 91.8(4) . . ?
O5 U3 O19 88.4(4) . . ?
O6 U3 O23 91.0(4) . 1_655 ?
O5 U3 O23 88.8(4) . 1_655 ?
O19 U3 O23 121.8(3) . 1_655 ?
O6 U3 O25 86.8(4) . . ?
O5 U3 O25 93.1(4) . . ?
O19 U3 O25 118.5(3) . . ?
O23 U3 O25 119.7(3) 1_655 . ?
O6 U3 O26 90.7(4) . . ?
O5 U3 O26 89.5(4) . . ?
O19 U3 O26 66.1(3) . . ?
O23 U3 O26 171.8(3) 1_655 . ?
O25 U3 O26 52.4(3) . . ?
O6 U3 O24 91.1(3) . 1_655 ?
O5 U3 O24 88.7(4) . 1_655 ?
O19 U3 O24 173.8(3) . 1_655 ?
O23 U3 O24 52.6(3) 1_655 1_655 ?
O25 U3 O24 67.1(3) . 1_655 ?
O26 U3 O24 119.3(3) . 1_655 ?
O6 U3 O20 88.1(4) . . ?
O5 U3 O20 91.9(4) . . ?
O19 U3 O20 53.1(3) . . ?
O23 U3 O20 69.0(3) 1_655 . ?
O25 U3 O20 170.0(3) . . ?
O26 U3 O20 119.1(3) . . ?
O24 U3 O20 121.6(3) 1_655 . ?
O8 U4 O7 179.6(5) . . ?
O8 U4 O27 92.8(4) . . ?
O7 U4 O27 87.3(4) . . ?
O8 U4 O31 90.9(4) . 4_545 ?
O7 U4 O31 88.7(4) . 4_545 ?
O27 U4 O31 119.5(3) . 4_545 ?
O8 U4 O29 88.2(4) . . ?
O7 U4 O29 92.1(4) . . ?
O27 U4 O29 121.0(3) . . ?
O31 U4 O29 119.5(3) 4_545 . ?
O8 U4 O32 86.5(4) . 4_545 ?
O7 U4 O32 93.2(4) . 4_545 ?
O27 U4 O32 66.7(3) . 4_545 ?
O31 U4 O32 53.3(3) 4_545 4_545 ?
O29 U4 O32 170.9(3) . 4_545 ?
O8 U4 O28 91.7(4) . . ?
O7 U4 O28 88.7(4) . . ?
O27 U4 O28 53.1(3) . . ?
O31 U4 O28 172.2(3) 4_545 . ?
O29 U4 O28 68.0(3) . . ?
O32 U4 O28 119.6(3) 4_545 . ?
O8 U4 O30 91.7(4) . . ?
O7 U4 O30 88.2(4) . . ?
O27 U4 O30 171.8(3) . . ?
O31 U4 O30 67.3(3) 4_545 . ?
O29 U4 O30 52.3(3) . . ?
O32 U4 O30 120.5(3) 4_545 . ?
O28 U4 O30 119.9(3) . . ?
N1 Ag1 N3 155.7(5) . . ?
N1 Ag1 N4 113.2(4) . . ?
N3 Ag1 N4 71.4(4) . . ?
N1 Ag1 N2 71.4(4) . . ?
N3 Ag1 N2 110.7(4) . . ?
N4 Ag1 N2 165.1(4) . . ?
N6 Ag2 N7 114.7(4) . . ?
N6 Ag2 N8 171.2(4) . . ?
N7 Ag2 N8 72.7(4) . . ?
N6 Ag2 N5 72.7(4) . . ?
N7 Ag2 N5 143.7(4) . . ?
N8 Ag2 N5 104.5(4) . . ?
N11 Ag3 N10 124.5(6) . . ?
N11 Ag3 N12 71.6(8) . . ?
N10 Ag3 N12 152.5(6) . . ?
N11 Ag3 N9 153.8(5) . . ?
N10 Ag3 N9 72.1(4) . . ?
N12 Ag3 N9 102.9(7) . . ?
N14 Ag4 N15 116.2(5) . . ?
N14 Ag4 N16 157.5(5) . . ?
N15 Ag4 N16 71.4(5) . . ?
N14 Ag4 N13 71.6(5) . . ?
N15 Ag4 N13 160.6(5) . . ?
N16 Ag4 N13 108.5(5) . . ?
N20 Ag5 N18 156.7(5) . . ?
N20 Ag5 N17 111.6(7) . . ?
N18 Ag5 N17 70.9(6) . . ?
N20 Ag5 N19 72.5(5) . . ?
N18 Ag5 N19 114.0(6) . . ?
N17 Ag5 N19 159.0(6) . . ?
C2 S1 C5 90.8(6) . . ?
C8 S2 C11 91.7(5) . . ?
C14 S3 C17 89.8(6) . . ?
C20 S4 C23 90.0(6) . . ?
C29 S5 C26 91.3(6) . . ?
C32 S6 C35 91.2(6) . . ?
C1 O9 U1 94.0(7) . . ?
C1 O10 U1 93.0(7) . . ?
C6 O11 U2 90.4(7) . . ?
C6 O12 U2 91.5(7) . . ?
C7 O13 U1 93.7(7) . . ?
C7 O14 U1 91.2(7) . . ?
C12 O15 U1 95.5(7) . 4_566 ?
C12 O16 U1 92.2(7) . 4_566 ?
C13 O17 U2 92.8(7) . . ?
C13 O18 U2 93.1(8) . . ?
C18 O19 U3 93.8(7) . . ?
C18 O20 U3 90.7(7) . . ?
C19 O21 U2 91.2(7) . . ?
C19 O22 U2 94.3(7) . . ?
C24 O23 U3 94.2(7) . 1_455 ?
C24 O24 U3 91.8(7) . 1_455 ?
C25 O25 U3 92.9(7) . . ?
C25 O26 U3 92.6(7) . . ?
C30 O27 U4 95.6(7) . . ?
C30 O28 U4 92.8(7) . . ?
C31 O29 U4 94.3(7) . . ?
C31 O30 U4 93.0(7) . . ?
C36 O31 U4 93.2(7) . 4_445 ?
C36 O32 U4 91.6(7) . 4_445 ?
H36A O36 H36B 118.2 . . ?
H39A O39 H39B 111.4 . . ?
H40A O40 H40B 108.6 . . ?
C46 N2 C42 117.6(14) . . ?
C46 N2 Ag1 129.0(11) . . ?
C42 N2 Ag1 113.3(10) . . ?
C47 N3 C51 118.3(15) . . ?
C47 N3 Ag1 122.4(12) . . ?
C51 N3 Ag1 118.4(10) . . ?
C56 N4 C52 117.6(15) . . ?
C56 N4 Ag1 126.3(11) . . ?
C52 N4 Ag1 115.1(10) . . ?
C57 N5 C61 117.7(12) . . ?
C57 N5 Ag2 125.5(10) . . ?
C61 N5 Ag2 114.7(9) . . ?
C66 N6 C62 118.6(13) . . ?
C66 N6 Ag2 124.1(9) . . ?
C62 N6 Ag2 115.0(9) . . ?
C67 N7 C71 118.8(12) . . ?
C67 N7 Ag2 126.3(10) . . ?
C71 N7 Ag2 114.4(9) . . ?
C76 N8 C72 118.6(15) . . ?
C76 N8 Ag2 124.4(11) . . ?
C72 N8 Ag2 113.1(10) . . ?
C77 N9 C81 118.9(15) . . ?
C77 N9 Ag3 125.2(12) . . ?
C81 N9 Ag3 115.1(10) . . ?
C86 N10 C82 118.3(15) . . ?
C86 N10 Ag3 125.4(11) . . ?
C82 N10 Ag3 115.0(10) . . ?
C97 N13 C101 121.1(17) . . ?
C97 N13 Ag4 124.1(13) . . ?
C101 N13 Ag4 114.8(12) . . ?
C102 N14 C106 116.0(15) . . ?
C102 N14 Ag4 119.2(12) . . ?
C106 N14 Ag4 124.4(11) . . ?
C107 N15 C111 116.7(14) . . ?
C107 N15 Ag4 124.8(11) . . ?
C111 N15 Ag4 117.4(12) . . ?
C116 N16 C112 122.9(14) . . ?
C116 N16 Ag4 122.4(11) . . ?
C112 N16 Ag4 113.1(12) . . ?
C121 N17 C117 117.7(17) . . ?
C121 N17 Ag5 115.1(14) . . ?
C117 N17 Ag5 126.4(14) . . ?
C122 N18 C126 117.2(17) . . ?
C122 N18 Ag5 119.0(13) . . ?
C126 N18 Ag5 123.2(13) . . ?
C127 N19 C131 118.2(17) . . ?
C127 N19 Ag5 126.2(13) . . ?
C131 N19 Ag5 113.7(13) . . ?
C136 N20 C132 115.3(19) . . ?
C136 N20 Ag5 124.7(15) . . ?
C132 N20 Ag5 117.4(13) . . ?
O35 N21 O34 121.6(14) . . ?
O35 N21 O33 117.4(14) . . ?
O34 N21 O33 119.5(14) . . ?
O9 C1 O10 119.4(11) . . ?
O9 C1 C2 120.9(11) . . ?
O10 C1 C2 119.7(11) . . ?
C3 C2 C1 128.0(12) . . ?
C3 C2 S1 112.8(10) . . ?
C1 C2 S1 119.2(9) . . ?
C2 C3 C4 111.7(12) . . ?
C2 C3 H3 124.1 . . ?
C4 C3 H3 124.1 . . ?
C5 C4 C3 112.2(11) . . ?
C5 C4 H4 123.9 . . ?
C3 C4 H4 123.9 . . ?
C4 C5 C6 129.7(11) . . ?
C4 C5 S1 112.5(9) . . ?
C6 C5 S1 117.8(9) . . ?
O12 C6 O11 123.0(11) . . ?
O12 C6 C5 118.0(11) . . ?
O11 C6 C5 118.8(11) . . ?
O13 C7 O14 122.0(10) . . ?
O13 C7 C8 119.5(11) . . ?
O14 C7 C8 118.5(11) . . ?
C9 C8 C7 129.7(11) . . ?
C9 C8 S2 112.1(8) . . ?
C7 C8 S2 118.1(9) . . ?
C8 C9 C10 112.7(11) . . ?
C8 C9 H9 123.7 . . ?
C10 C9 H9 123.7 . . ?
C11 C10 C9 111.8(10) . . ?
C11 C10 H10 124.1 . . ?
C9 C10 H10 124.1 . . ?
C10 C11 C12 129.6(11) . . ?
C10 C11 S2 111.7(8) . . ?
C12 C11 S2 118.7(9) . . ?
O15 C12 O16 119.4(11) . . ?
O15 C12 C11 117.4(11) . . ?
O16 C12 C11 123.1(11) . . ?
O18 C13 O17 121.5(12) . . ?
O18 C13 C14 118.1(11) . . ?
O17 C13 C14 120.4(12) . . ?
C15 C14 C13 127.7(12) . . ?
C15 C14 S3 113.7(9) . . ?
C13 C14 S3 118.6(10) . . ?
C14 C15 C16 109.9(11) . . ?
C14 C15 H15 125.0 . . ?
C16 C15 H15 125.0 . . ?
C17 C16 C15 113.1(11) . . ?
C17 C16 H16 123.4 . . ?
C15 C16 H16 123.4 . . ?
C16 C17 C18 129.9(12) . . ?
C16 C17 S3 113.4(8) . . ?
C18 C17 S3 116.7(10) . . ?
O20 C18 O19 122.4(11) . . ?
O20 C18 C17 121.0(12) . . ?
O19 C18 C17 116.7(12) . . ?
O22 C19 O21 122.3(11) . . ?
O22 C19 C20 118.0(11) . . ?
O21 C19 C20 119.5(11) . . ?
C21 C20 C19 130.9(11) . . ?
C21 C20 S4 112.2(9) . . ?
C19 C20 S4 116.9(9) . . ?
C20 C21 C22 112.9(11) . . ?
C20 C21 H21 123.6 . . ?
C22 C21 H21 123.6 . . ?
C23 C22 C21 110.8(12) . . ?
C23 C22 H22 124.6 . . ?
C21 C22 H22 124.6 . . ?
C22 C23 C24 129.1(12) . . ?
C22 C23 S4 114.0(10) . . ?
C24 C23 S4 116.8(10) . . ?
O23 C24 O24 121.3(11) . . ?
O23 C24 C23 118.8(11) . . ?
O24 C24 C23 119.9(12) . . ?
O25 C25 O26 121.3(12) . . ?
O25 C25 C26 118.5(11) . . ?
O26 C25 C26 120.1(11) . . ?
C27 C26 C25 128.4(11) . . ?
C27 C26 S5 111.4(9) . . ?
C25 C26 S5 120.0(8) . . ?
C26 C27 C28 113.3(11) . . ?
C26 C27 H27 123.4 . . ?
C28 C27 H27 123.4 . . ?
C29 C28 C27 110.4(11) . . ?
C29 C28 H28 124.8 . . ?
C27 C28 H28 124.8 . . ?
C28 C29 C30 128.5(11) . . ?
C28 C29 S5 113.5(10) . . ?
C30 C29 S5 117.7(9) . . ?
O27 C30 O28 117.6(11) . . ?
O27 C30 C29 120.8(11) . . ?
O28 C30 C29 121.6(11) . . ?
O30 C31 O29 120.5(11) . . ?
O30 C31 C32 123.6(12) . . ?
O29 C31 C32 115.9(12) . . ?
C33 C32 C31 128.4(12) . . ?
C33 C32 S6 111.8(9) . . ?
C31 C32 S6 119.7(10) . . ?
C32 C33 C34 112.7(11) . . ?
C32 C33 H33 123.6 . . ?
C34 C33 H33 123.6 . . ?
C35 C34 C33 111.0(11) . . ?
C35 C34 H34 124.5 . . ?
C33 C34 H34 124.5 . . ?
C34 C35 C36 130.3(12) . . ?
C34 C35 S6 113.3(9) . . ?
C36 C35 S6 116.4(9) . . ?
O31 C36 O32 121.9(11) . . ?
O31 C36 C35 119.7(11) . . ?
O32 C36 C35 118.3(11) . . ?
C37 N1 C41 120.0 . . ?
C37 N1 Ag1 120.6(7) . . ?
C41 N1 Ag1 119.2(7) . . ?
C38 C37 N1 120.0 . . ?
C38 C37 H37 120.0 . . ?
N1 C37 H37 120.0 . . ?
C39 C38 C37 120.0 . . ?
C39 C38 H38 120.0 . . ?
C37 C38 H38 120.0 . . ?
C38 C39 C40 120.0 . . ?
C38 C39 H39 120.0 . . ?
C40 C39 H39 120.0 . . ?
C41 C40 C39 120.0 . . ?
C41 C40 H40 120.0 . . ?
C39 C40 H40 120.0 . . ?
C40 C41 N1 120.0 . . ?
C40 C41 C42 122.2(11) . . ?
N1 C41 C42 117.8(11) . . ?
N2 C42 C43 119.7(16) . . ?
N2 C42 C41 118.0(14) . . ?
C43 C42 C41 122.0(15) . . ?
C44 C43 C42 118.7(17) . . ?
C44 C43 H43 120.6 . . ?
C42 C43 H43 120.6 . . ?
C43 C44 C45 120.4(17) . . ?
C43 C44 H44 119.8 . . ?
C45 C44 H44 119.8 . . ?
C46 C45 C44 117.7(17) . . ?
C46 C45 H45 121.2 . . ?
C44 C45 H45 121.2 . . ?
N2 C46 C45 125.9(17) . . ?
N2 C46 H46 117.1 . . ?
C45 C46 H46 117.1 . . ?
N3 C47 C48 125(2) . . ?
N3 C47 H47 117.6 . . ?
C48 C47 H47 117.6 . . ?
C47 C48 C49 114.5(17) . . ?
C47 C48 H48 122.7 . . ?
C49 C48 H48 122.7 . . ?
C50 C49 C48 123.9(17) . . ?
C50 C49 H49 118.0 . . ?
C48 C49 H49 118.0 . . ?
C49 C50 C51 117.3(18) . . ?
C49 C50 H50 121.4 . . ?
C51 C50 H50 121.4 . . ?
N3 C51 C50 120.9(15) . . ?
N3 C51 C52 116.3(14) . . ?
C50 C51 C52 122.8(15) . . ?
N4 C52 C53 122.2(15) . . ?
N4 C52 C51 117.3(14) . . ?
C53 C52 C51 120.5(15) . . ?
C54 C53 C52 116.5(17) . . ?
C54 C53 H53 121.7 . . ?
C52 C53 H53 121.7 . . ?
C55 C54 C53 120.1(17) . . ?
C55 C54 H54 119.9 . . ?
C53 C54 H54 119.9 . . ?
C56 C55 C54 118.9(18) . . ?
C56 C55 H55 120.6 . . ?
C54 C55 H55 120.6 . . ?
N4 C56 C55 124.4(18) . . ?
N4 C56 H56 117.8 . . ?
C55 C56 H56 117.8 . . ?
N5 C57 C58 123.7(15) . . ?
N5 C57 H57 118.1 . . ?
C58 C57 H57 118.1 . . ?
C59 C58 C57 117.5(16) . . ?
C59 C58 H58 121.3 . . ?
C57 C58 H58 121.3 . . ?
C60 C59 C58 117.6(15) . . ?
C60 C59 H59 121.2 . . ?
C58 C59 H59 121.2 . . ?
C61 C60 C59 121.9(14) . . ?
C61 C60 H60 119.0 . . ?
C59 C60 H60 119.0 . . ?
C60 C61 N5 121.5(13) . . ?
C60 C61 C62 123.0(13) . . ?
N5 C61 C62 115.6(11) . . ?
N6 C62 C63 120.6(12) . . ?
N6 C62 C61 118.3(12) . . ?
C63 C62 C61 121.1(11) . . ?
C64 C63 C62 120.9(13) . . ?
C64 C63 H63 119.6 . . ?
C62 C63 H63 119.6 . . ?
C63 C64 C65 117.6(16) . . ?
C63 C64 H64 121.2 . . ?
C65 C64 H64 121.2 . . ?
C64 C65 C66 119.7(14) . . ?
C64 C65 H65 120.1 . . ?
C66 C65 H65 120.1 . . ?
N6 C66 C65 122.5(13) . . ?
N6 C66 H66 118.8 . . ?
C65 C66 H66 118.8 . . ?
N7 C67 C68 123.5(15) . . ?
N7 C67 H67 118.3 . . ?
C68 C67 H67 118.3 . . ?
C69 C68 C67 119.1(16) . . ?
C69 C68 H68 120.5 . . ?
C67 C68 H68 120.5 . . ?
C70 C69 C68 119.7(15) . . ?
C70 C69 H69 120.1 . . ?
C68 C69 H69 120.1 . . ?
C69 C70 C71 120.7(16) . . ?
C69 C70 H70 119.6 . . ?
C71 C70 H70 119.6 . . ?
N7 C71 C70 117.9(14) . . ?
N7 C71 C72 118.0(12) . . ?
C70 C71 C72 123.8(14) . . ?
N8 C72 C71 118.7(14) . . ?
N8 C72 C73 117.6(16) . . ?
C71 C72 C73 123.5(15) . . ?
C74 C73 C72 121.1(16) . . ?
C74 C73 H73 119.5 . . ?
C72 C73 H73 119.5 . . ?
C73 C74 C75 120.5(18) . . ?
C73 C74 H74 119.8 . . ?
C75 C74 H74 119.8 . . ?
C74 C75 C76 117(2) . . ?
C74 C75 H75 121.4 . . ?
C76 C75 H75 121.4 . . ?
N8 C76 C75 124.6(17) . . ?
N8 C76 H76 117.7 . . ?
C75 C76 H76 117.7 . . ?
N9 C77 C78 121.8(18) . . ?
N9 C77 H77 119.1 . . ?
C78 C77 H77 119.1 . . ?
C79 C78 C77 119.3(17) . . ?
C79 C78 H78 120.4 . . ?
C77 C78 H78 120.4 . . ?
C78 C79 C80 121.1(16) . . ?
C78 C79 H79 119.4 . . ?
C80 C79 H79 119.4 . . ?
C79 C80 C81 117.6(16) . . ?
C79 C80 H80 121.2 . . ?
C81 C80 H80 121.2 . . ?
N9 C81 C80 121.0(15) . . ?
N9 C81 C82 117.6(14) . . ?
C80 C81 C82 121.3(15) . . ?
N10 C82 C81 118.7(15) . . ?
N10 C82 C83 120.0(15) . . ?
C81 C82 C83 121.4(16) . . ?
C84 C83 C82 118(2) . . ?
C84 C83 H83 121.2 . . ?
C82 C83 H83 121.2 . . ?
C85 C84 C83 120(2) . . ?
C85 C84 H84 120.2 . . ?
C83 C84 H84 120.2 . . ?
C84 C85 C86 124.2(19) . . ?
C84 C85 H85 117.9 . . ?
C86 C85 H85 117.9 . . ?
N10 C86 C85 120.0(18) . . ?
N10 C86 H86 120.0 . . ?
C85 C86 H86 120.0 . . ?
C87 N11 C91 120.0 . . ?
C87 N11 Ag3 124.4(10) . . ?
C91 N11 Ag3 114.8(10) . . ?
N11 C87 C88 120.0 . . ?
N11 C87 H87 120.0 . . ?
C88 C87 H87 120.0 . . ?
C87 C88 C89 120.0 . . ?
C87 C88 H88 120.0 . . ?
C89 C88 H88 120.0 . . ?
C90 C89 C88 120.0 . . ?
C90 C89 H89 120.0 . . ?
C88 C89 H89 120.0 . . ?
C89 C90 C91 120.0 . . ?
C89 C90 H90 120.0 . . ?
C91 C90 H90 120.0 . . ?
C92 C91 C90 114.4(17) . . ?
C92 C91 N11 125.2(18) . . ?
C90 C91 N11 120.0 . . ?
C92 N12 C96 120.0 . . ?
C92 N12 Ag3 117.3(14) . . ?
C96 N12 Ag3 119.4(14) . . ?
C91 C92 C93 129(2) . . ?
C91 C92 N12 110(2) . . ?
C93 C92 N12 120.0 . . ?
C92 C93 C94 120.0 . . ?
C92 C93 H93 120.0 . . ?
C94 C93 H93 120.0 . . ?
C95 C94 C93 120.0 . . ?
C95 C94 H94 120.0 . . ?
C93 C94 H94 120.0 . . ?
C96 C95 C94 120.0 . . ?
C96 C95 H95 120.0 . . ?
C94 C95 H95 120.0 . . ?
C95 C96 N12 120.0 . . ?
C95 C96 H96 120.0 . . ?
N12 C96 H96 120.0 . . ?
N13 C97 C98 121(2) . . ?
N13 C97 H97 119.7 . . ?
C98 C97 H97 119.7 . . ?
C99 C98 C97 119(2) . . ?
C99 C98 H98 120.7 . . ?
C97 C98 H98 120.7 . . ?
C100 C99 C98 119(2) . . ?
C100 C99 H99 120.7 . . ?
C98 C99 H99 120.6 . . ?
C99 C100 C101 123.3(17) . . ?
C99 C100 H100 118.3 . . ?
C101 C100 H100 118.3 . . ?
N13 C101 C100 117.3(16) . . ?
N13 C101 C102 116.2(15) . . ?
C100 C101 C102 126.5(15) . . ?
N14 C102 C103 121.5(19) . . ?
N14 C102 C101 118.0(14) . . ?
C103 C102 C101 120.4(16) . . ?
C104 C103 C102 120(2) . . ?
C104 C103 H103 120.2 . . ?
C102 C103 H103 120.2 . . ?
C103 C104 C105 120(2) . . ?
C103 C104 H104 119.9 . . ?
C105 C104 H104 119.9 . . ?
C106 C105 C104 115(2) . . ?
C106 C105 H105 122.6 . . ?
C104 C105 H105 122.6 . . ?
N14 C106 C105 127.5(19) . . ?
N14 C106 H106 116.2 . . ?
C105 C106 H106 116.2 . . ?
N15 C107 C108 127.4(17) . . ?
N15 C107 H107 116.3 . . ?
C108 C107 H107 116.3 . . ?
C109 C108 C107 114.0(18) . . ?
C109 C108 H108 123.0 . . ?
C107 C108 H108 123.0 . . ?
C110 C109 C108 118.6(16) . . ?
C110 C109 H109 120.7 . . ?
C108 C109 H109 120.7 . . ?
C109 C110 C111 122.9(17) . . ?
C109 C110 H110 118.5 . . ?
C111 C110 H110 118.5 . . ?
N15 C111 C110 120.2(17) . . ?
N15 C111 C112 115.4(14) . . ?
C110 C111 C112 124.4(16) . . ?
N16 C112 C113 119.4(19) . . ?
N16 C112 C111 120.2(14) . . ?
C113 C112 C111 120.1(19) . . ?
C112 C113 C114 120(3) . . ?
C112 C113 H113 120.2 . . ?
C114 C113 H113 120.2 . . ?
C115 C114 C113 112(3) . . ?
C115 C114 H114 123.8 . . ?
C113 C114 H114 123.8 . . ?
C116 C115 C114 125(3) . . ?
C116 C115 H115 117.6 . . ?
C114 C115 H115 117.6 . . ?
C115 C116 N16 120(2) . . ?
C115 C116 H116 120.1 . . ?
N16 C116 H116 120.1 . . ?
C118 C117 N17 124(2) . . ?
C118 C117 H117 117.9 . . ?
N17 C117 H117 117.9 . . ?
C117 C118 C119 122(3) . . ?
C117 C118 H118 119.0 . . ?
C119 C118 H118 119.0 . . ?
C118 C119 C120 111(3) . . ?
C118 C119 H119 124.5 . . ?
C120 C119 H119 124.5 . . ?
C121 C120 C119 128(2) . . ?
C121 C120 H120 116.2 . . ?
C119 C120 H120 116.2 . . ?
N17 C121 C120 117.4(19) . . ?
N17 C121 C122 118.4(17) . . ?
C120 C121 C122 123.9(17) . . ?
N18 C122 C123 120.1(19) . . ?
N18 C122 C121 116.2(16) . . ?
C123 C122 C121 123.6(18) . . ?
C124 C123 C122 121.5(19) . . ?
C124 C123 H123 119.3 . . ?
C122 C123 H123 119.3 . . ?
C123 C124 C125 122.8(19) . . ?
C123 C124 H124 118.6 . . ?
C125 C124 H124 118.6 . . ?
C126 C125 C124 110(2) . . ?
C126 C125 H125 125.2 . . ?
C124 C125 H125 125.2 . . ?
N18 C126 C125 129(2) . . ?
N18 C126 H126 115.7 . . ?
C125 C126 H126 115.7 . . ?
N19 C127 C128 125(2) . . ?
N19 C127 H127 117.6 . . ?
C128 C127 H127 117.6 . . ?
C129 C128 C127 119(2) . . ?
C129 C128 H128 120.4 . . ?
C127 C128 H128 120.4 . . ?
C128 C129 C130 115(2) . . ?
C128 C129 H129 122.7 . . ?
C130 C129 H129 122.7 . . ?
C131 C130 C129 125(2) . . ?
C131 C130 H130 117.6 . . ?
C129 C130 H130 117.6 . . ?
C130 C131 N19 118.3(19) . . ?
C130 C131 C132 125.4(17) . . ?
N19 C131 C132 116.3(15) . . ?
N20 C132 C133 121.3(19) . . ?
N20 C132 C131 117.4(16) . . ?
C133 C132 C131 121.3(16) . . ?
C134 C133 C132 124(2) . . ?
C134 C133 H133 117.8 . . ?
C132 C133 H133 117.8 . . ?
C133 C134 C135 115(2) . . ?
C133 C134 H134 122.3 . . ?
C135 C134 H134 122.3 . . ?
C134 C135 C136 116(2) . . ?
C134 C135 H135 122.1 . . ?
C136 C135 H135 122.1 . . ?
N20 C136 C135 127(2) . . ?
N20 C136 H136 116.4 . . ?
C135 C136 H136 116.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O36 H36B O44 0.94 2.49 2.96(4) 111.2 3
O39 H39A O41 0.91 1.91 2.76(2) 155.3 3_655
O39 H39B O43 0.90 1.96 2.83(2) 161.2 3_655
O40 H40A O42 1.01 1.92 2.75(3) 137.6 .

_refine_diff_density_max         1.022
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.125

_shelxl_version_number           2014-3

