# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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 2202986'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2022-08-23 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H43 N3 O18 U'
_chemical_formula_iupac          ?
_chemical_formula_weight         1067.78
_chemical_absolute_configuration ?

_chemical_melting_point          ?

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z'

_cell_length_a                   14.7890(4)
_cell_length_b                   9.6838(3)
_cell_length_c                   28.1690(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4034.19(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9920
_cell_measurement_theta_min      2.5525
_cell_measurement_theta_max      30.4136
_cell_measurement_temperature    100(2)

_exptl_crystal_description       block
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.079
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.072
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2112

_exptl_absorpt_coefficient_mu    4.106
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_T_max  0.75

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100(2)

_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms 70 W'
_diffrn_source_current           1.4
_diffrn_source_voltage           50

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'multilayer mirror optics'

_diffrn_measurement_device       'Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_detector_area_resol_mean 7.41

_diffrn_reflns_number            111788
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_full        28.70
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38

_refine_special_details          
;
The H atoms bound to O atoms were found and refined with
restraints on bond lengths and with isotropic displacement
parameters equal to 1.2 (COOH) or 1.5 (H2O) that
of the attached O atom.
Refined as a 2-component inversion twin.
;

_reflns_number_total             10343
_reflns_number_gt                9644
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0187
_refine_ls_wR_factor_gt          0.0424
_refine_ls_wR_factor_ref         0.0437
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.044
_refine_ls_number_reflns         10343
_refine_ls_number_parameters     573
_refine_ls_number_restraints     12
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0159P)²+2.4508P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.376
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.005(4)

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

_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1328)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U U1 0.28463(2) 0.68626(2) 0.36805(2) 0.01162(4) Uani d . . . 1 . .
O O1 0.39968(18) 0.6475(3) 0.35707(9) 0.0191(6) Uani d . . . 1 . .
O O2 0.16897(19) 0.7246(3) 0.37985(9) 0.0202(6) Uani d . . . 1 . .
O O3 0.2345(2) 0.5096(4) 0.31907(12) 0.0226(8) Uani d . . . 1 . .
O O4 0.3141(2) 0.4726(3) 0.25221(12) 0.0212(6) Uani d . . . 1 . .
O O5 0.18535(19) -0.0765(2) -0.13022(17) 0.0228(5) Uani d . . . 1 . .
O O6 0.2716(2) 0.0672(4) -0.08863(13) 0.0312(8) Uani d . . . 1 . .
O O7 0.3186(2) 0.7401(3) 0.44790(10) 0.0155(5) Uani d . . . 1 . .
O O8 0.4656(2) 0.7187(3) 0.46677(10) 0.0219(6) Uani d . . . 1 . .
O O9 0.3422(2) 0.4733(3) 0.50675(10) 0.0184(6) Uani d . . . 1 . .
O O10 0.3482(2) 0.4244(3) 0.58403(10) 0.0206(6) Uani d . . D 1 . .
H H10 0.343(4) 0.337(2) 0.5742(18) 0.025000 Uiso d U . D 1 . .
O O11 0.3099(2) 0.7438(3) 0.70221(10) 0.0187(6) Uani d . . . 1 . .
O O12 0.2815(2) 0.9647(3) 0.69417(10) 0.0222(6) Uani d . . D 1 . .
H H12 0.284(3) 1.029(4) 0.6714(14) 0.027000 Uiso d U . D 1 . .
O O13 0.2903(2) 1.1401(3) 0.63409(11) 0.0217(6) Uani d . . . 1 . .
O O14 0.3528(2) 1.1693(3) 0.56388(10) 0.0220(6) Uani d . . . 1 . .
O O15 0.2631(3) 0.4810(4) 0.41676(12) 0.0234(8) Uani d . . D 1 . .
H H15A 0.283(3) 0.480(6) 0.4440(9) 0.035000 Uiso d U . D 1 . .
H H15B 0.218(2) 0.433(5) 0.4143(17) 0.035000 Uiso d U . D 1 . .
O O16 0.2750(2) 0.7803(3) 0.28837(10) 0.0186(6) Uani d . . D 1 . .
H H16A 0.244(3) 0.768(5) 0.2639(11) 0.028000 Uiso d U . D 1 . .
H H16B 0.316(3) 0.837(4) 0.2822(16) 0.028000 Uiso d U . D 1 . .
O O17 0.4163(2) -0.0688(3) 0.27193(11) 0.0255(6) Uani d . . . 1 . .
O O18 0.3774(2) 0.3113(3) -0.09155(14) 0.0338(8) Uani d . . D 1 . .
H H18A 0.421(3) 0.300(5) -0.0724(19) 0.051000 Uiso d U . D 1 . .
H H18B 0.348(3) 0.238(4) -0.091(2) 0.051000 Uiso d U . D 1 . .
N N1 0.0002(2) 0.3313(3) 0.21168(11) 0.0145(6) Uani d . . . 1 . .
N N2 -0.0399(2) 0.1812(4) -0.03740(12) 0.0171(7) Uani d . . . 1 . .
N N3 0.4947(4) 0.1171(5) 0.29144(17) 0.0426(11) Uani d . . . 1 . .
C C1 0.2447(3) 0.4692(4) 0.27634(14) 0.0162(7) Uani d . . . 1 . .
C C2 0.1585(3) 0.4135(4) 0.25399(13) 0.0141(7) Uani d . . . 1 . .
C C3 0.0799(3) 0.3987(4) 0.28072(14) 0.0169(7) Uani d . . . 1 . .
H H3 0.080509 0.416497 0.313877 0.020000 Uiso calc U . R 1 . .
C C4 0.0015(3) 0.3581(4) 0.25873(14) 0.0172(8) Uani d . . . 1 . .
H H4 -0.052458 0.348718 0.276782 0.021000 Uiso calc U . R 1 . .
C C5 0.0760(3) 0.3411(4) 0.18550(14) 0.0167(8) Uani d . . . 1 . .
H H5 0.074202 0.319548 0.152617 0.020000 Uiso calc U . R 1 . .
C C6 0.1560(3) 0.3821(4) 0.20591(14) 0.0173(8) Uani d . . . 1 . .
H H6 0.209286 0.388831 0.187243 0.021000 Uiso calc U . R 1 . .
C C7 -0.0885(3) 0.2884(4) 0.19044(14) 0.0179(8) Uani d . . . 1 . .
H H7A -0.135218 0.356241 0.199853 0.021000 Uiso calc U . R 1 . .
H H7B -0.105915 0.197897 0.203981 0.021000 Uiso calc U . R 1 . .
C C8 -0.0880(3) 0.2768(4) 0.13705(14) 0.0178(8) Uani d . . . 1 . .
C C9 -0.0973(3) 0.3968(4) 0.10935(14) 0.0189(8) Uani d . . . 1 . .
C C10 -0.1036(3) 0.3842(5) 0.05990(15) 0.0217(8) Uani d . . . 1 . .
C C11 -0.1084(3) 0.2524(5) 0.03938(15) 0.0207(8) Uani d . . . 1 . .
C C12 -0.0992(3) 0.1325(5) 0.06729(15) 0.0206(8) Uani d . . . 1 . .
C C13 -0.0835(3) 0.1454(5) 0.11616(15) 0.0191(8) Uani d . . . 1 . .
C C14 -0.0975(3) 0.5390(5) 0.13166(16) 0.0247(9) Uani d . . . 1 . .
H H14A -0.042185 0.588179 0.122714 0.037000 Uiso calc U . R 1 . .
H H14B -0.100303 0.530116 0.166282 0.037000 Uiso calc U . R 1 . .
H H14C -0.150294 0.590805 0.120419 0.037000 Uiso calc U . R 1 . .
C C15 -0.1045(3) 0.5151(5) 0.02996(16) 0.0284(10) Uani d . . . 1 . .
H H15C -0.164428 0.557922 0.031655 0.043000 Uiso calc U . R 1 . .
H H15D -0.090601 0.491776 -0.003104 0.043000 Uiso calc U . R 1 . .
H H15E -0.059003 0.579700 0.042049 0.043000 Uiso calc U . R 1 . .
C C16 -0.1064(3) -0.0099(5) 0.04507(17) 0.0267(9) Uani d . . . 1 . .
H H16C -0.046443 -0.040401 0.034629 0.040000 Uiso calc U . R 1 . .
H H16D -0.147266 -0.006074 0.017705 0.040000 Uiso calc U . R 1 . .
H H16E -0.130238 -0.075201 0.068528 0.040000 Uiso calc U . R 1 . .
C C17 -0.0610(3) 0.0187(5) 0.14547(16) 0.0240(9) Uani d . . . 1 . .
H H17A -0.117119 -0.024955 0.156320 0.036000 Uiso calc U . R 1 . .
H H17B -0.024689 0.045946 0.173013 0.036000 Uiso calc U . R 1 . .
H H17C -0.026715 -0.046872 0.126020 0.036000 Uiso calc U . R 1 . .
C C18 -0.1225(3) 0.2366(5) -0.01344(15) 0.0234(9) Uani d . . . 1 . .
H H18C -0.173846 0.173262 -0.019230 0.028000 Uiso calc U . R 1 . .
H H18D -0.137978 0.327520 -0.027298 0.028000 Uiso calc U . R 1 . .
C C19 0.0411(3) 0.2389(4) -0.02737(14) 0.0191(8) Uani d . . . 1 . .
H H19 0.044799 0.313504 -0.005539 0.023000 Uiso calc U . R 1 . .
C C20 0.1178(3) 0.1898(4) -0.04870(15) 0.0175(8) Uani d . . . 1 . .
H H20 0.174573 0.231045 -0.041840 0.021000 Uiso calc U . R 1 . .
C C21 0.1130(3) 0.0817(4) -0.07987(13) 0.0160(7) Uani d . . . 1 . .
C C22 0.0291(3) 0.0253(4) -0.09032(15) 0.0202(8) Uani d . . . 1 . .
H H22 0.024288 -0.048949 -0.112204 0.024000 Uiso calc U . R 1 . .
C C23 -0.0469(3) 0.0774(5) -0.06887(16) 0.0203(9) Uani d . . . 1 . .
H H23 -0.104623 0.040126 -0.076282 0.024000 Uiso calc U . R 1 . .
C C24 0.1987(3) 0.0201(4) -0.10116(15) 0.0196(8) Uani d . . . 1 . .
C C25 0.3612(2) 0.7618(4) 0.52796(12) 0.0104(7) Uani d . . . 1 . .
C C26 0.3476(2) 0.6585(4) 0.56210(13) 0.0105(6) Uani d . . . 1 . .
C C27 0.3309(2) 0.6954(3) 0.60881(13) 0.0109(6) Uani d . . . 1 . .
H H27 0.323969 0.624076 0.631694 0.013000 Uiso calc U . R 1 . .
C C28 0.3237(2) 0.8329(4) 0.62387(13) 0.0109(7) Uani d . . . 1 . .
C C29 0.3344(2) 0.9377(4) 0.58928(13) 0.0109(6) Uani d . . . 1 . .
C C30 0.3542(3) 0.8991(4) 0.54280(13) 0.0118(7) Uani d . . . 1 . .
H H30 0.363344 0.969933 0.519956 0.014000 Uiso calc U . R 1 . .
C C31 0.3857(2) 0.7348(4) 0.47669(13) 0.0108(7) Uani d . . . 1 . .
C C32 0.3462(2) 0.5098(4) 0.54792(13) 0.0124(7) Uani d . . . 1 . .
C C33 0.3050(3) 0.8459(4) 0.67656(14) 0.0141(7) Uani d . . . 1 . .
C C34 0.3259(3) 1.0934(4) 0.59656(13) 0.0138(7) Uani d . . . 1 . .
C C35 0.4178(4) 0.0569(5) 0.28095(17) 0.0339(11) Uani d . . . 1 . .
C C36 0.3315(4) 0.1439(5) 0.2807(2) 0.0366(12) Uani d . . . 1 . .
H H36A 0.331266 0.204025 0.252760 0.055000 Uiso calc U . R 1 . .
H H36B 0.329288 0.200585 0.309550 0.055000 Uiso calc U . R 1 . .
H H36C 0.278670 0.082907 0.279804 0.055000 Uiso calc U . R 1 . .
C C37 0.5755(4) 0.0336(6) 0.2949(2) 0.0343(12) Uani d . . . 1 . .
H H37A 0.558918 -0.061044 0.303672 0.051000 Uiso calc U . R 1 . .
H H37B 0.615644 0.072253 0.319188 0.051000 Uiso calc U . R 1 . .
H H37C 0.606717 0.032817 0.264217 0.051000 Uiso calc U . R 1 . .
C C38 0.5044(5) 0.2678(6) 0.2966(3) 0.060(2) Uani d . . . 1 . .
H H38A 0.444609 0.309555 0.301002 0.090000 Uiso calc U . R 1 . .
H H38B 0.532547 0.305941 0.267918 0.090000 Uiso calc U . R 1 . .
H H38C 0.542431 0.288289 0.324166 0.090000 Uiso calc U . R 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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
U1 O1 . 1.770(3) ?
U1 O2 . 1.781(3) ?
U1 O3 . 2.320(3) ?
U1 O5 3_565 2.340(2) ?
U1 O7 . 2.363(3) ?
U1 O16 . 2.427(3) ?
U1 O15 . 2.436(3) ?
O3 C1 . 1.275(5) ?
O4 C1 . 1.232(5) ?
O5 C24 . 1.259(5) ?
O6 C24 . 1.223(5) ?
O7 C31 . 1.284(5) ?
O8 C31 . 1.223(5) ?
O9 C32 . 1.214(5) ?
O10 C32 . 1.312(4) ?
O10 H10 . 0.892(14) ?
O11 C33 . 1.226(5) ?
O12 C33 . 1.300(5) ?
O12 H12 . 0.896(14) ?
O13 C34 . 1.264(5) ?
O14 C34 . 1.244(5) ?
O15 H15A . 0.824(14) ?
O15 H15B . 0.821(14) ?
O16 H16A . 0.834(14) ?
O16 H16B . 0.834(14) ?
O17 C35 . 1.243(6) ?
O18 H18A . 0.844(14) ?
O18 H18B . 0.839(14) ?
N1 C5 . 1.346(5) ?
N1 C4 . 1.350(5) ?
N1 C7 . 1.499(5) ?
N2 C23 . 1.344(5) ?
N2 C19 . 1.351(5) ?
N2 C18 . 1.495(5) ?
N3 C35 . 1.312(7) ?
N3 C37 . 1.446(7) ?
N3 C38 . 1.473(7) ?
C1 C2 . 1.521(5) ?
C2 C6 . 1.388(5) ?
C2 C3 . 1.392(5) ?
C3 C4 . 1.372(6) ?
C3 H3 . 0.950000 ?
C4 H4 . 0.950000 ?
C5 C6 . 1.374(5) ?
C5 H5 . 0.950000 ?
C6 H6 . 0.950000 ?
C7 C8 . 1.508(5) ?
C7 H7A . 0.990000 ?
C7 H7B . 0.990000 ?
C8 C13 . 1.404(6) ?
C8 C9 . 1.406(6) ?
C9 C10 . 1.401(6) ?
C9 C14 . 1.514(6) ?
C10 C11 . 1.403(7) ?
C10 C15 . 1.522(6) ?
C11 C12 . 1.408(6) ?
C11 C18 . 1.510(6) ?
C12 C13 . 1.401(6) ?
C12 C16 . 1.518(6) ?
C13 C17 . 1.516(6) ?
C14 H14A . 0.980000 ?
C14 H14B . 0.980000 ?
C14 H14C . 0.980000 ?
C15 H15C . 0.980000 ?
C15 H15D . 0.980000 ?
C15 H15E . 0.980000 ?
C16 H16C . 0.980000 ?
C16 H16D . 0.980000 ?
C16 H16E . 0.980000 ?
C17 H17A . 0.980000 ?
C17 H17B . 0.980000 ?
C17 H17C . 0.980000 ?
C18 H18C . 0.990000 ?
C18 H18D . 0.990000 ?
C19 C20 . 1.368(6) ?
C19 H19 . 0.950000 ?
C20 C21 . 1.369(6) ?
C20 H20 . 0.950000 ?
C21 C22 . 1.387(6) ?
C21 C24 . 1.524(6) ?
C22 C23 . 1.373(6) ?
C22 H22 . 0.950000 ?
C23 H23 . 0.950000 ?
C25 C30 . 1.398(5) ?
C25 C26 . 1.402(5) ?
C25 C31 . 1.512(5) ?
C26 C27 . 1.385(5) ?
C26 C32 . 1.495(5) ?
C27 C28 . 1.402(5) ?
C27 H27 . 0.950000 ?
C28 C29 . 1.416(5) ?
C28 C33 . 1.515(5) ?
C29 C30 . 1.393(5) ?
C29 C34 . 1.527(5) ?
C30 H30 . 0.950000 ?
C35 C36 . 1.530(8) ?
C36 H36A . 0.980000 ?
C36 H36B . 0.980000 ?
C36 H36C . 0.980000 ?
C37 H37A . 0.980000 ?
C37 H37B . 0.980000 ?
C37 H37C . 0.980000 ?
C38 H38A . 0.980000 ?
C38 H38B . 0.980000 ?
C38 H38C . 0.980000 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 U1 O2 . . 179.28(12) ?
O1 U1 O3 . . 92.68(12) ?
O2 U1 O3 . . 87.57(13) ?
O1 U1 O5 . 3_565 91.70(12) ?
O2 U1 O5 . 3_565 88.51(12) ?
O3 U1 O5 . 3_565 142.85(14) ?
O1 U1 O7 . . 90.52(11) ?
O2 U1 O7 . . 88.88(12) ?
O3 U1 O7 . . 142.82(11) ?
O5 U1 O7 3_565 . 73.95(13) ?
O1 U1 O16 . . 88.54(12) ?
O2 U1 O16 . . 92.18(12) ?
O3 U1 O16 . . 73.02(11) ?
O5 U1 O16 3_565 . 70.23(14) ?
O7 U1 O16 . . 144.12(10) ?
O1 U1 O15 . . 92.90(13) ?
O2 U1 O15 . . 86.53(13) ?
O3 U1 O15 . . 72.03(10) ?
O5 U1 O15 3_565 . 144.49(14) ?
O7 U1 O15 . . 70.82(11) ?
O16 U1 O15 . . 145.05(11) ?
C1 O3 U1 . . 138.6(3) ?
C24 O5 U1 . 3_544 135.5(3) ?
C31 O7 U1 . . 139.2(2) ?
C32 O10 H10 . . 111.(3) ?
C33 O12 H12 . . 109.(3) ?
U1 O15 H15A . . 119.(4) ?
U1 O15 H15B . . 122.(4) ?
H15A O15 H15B . . 112.(3) ?
U1 O16 H16A . . 138.(3) ?
U1 O16 H16B . . 114.(3) ?
H16A O16 H16B . . 108.(2) ?
H18A O18 H18B . . 106.(2) ?
C5 N1 C4 . . 120.8(3) ?
C5 N1 C7 . . 122.0(3) ?
C4 N1 C7 . . 117.2(3) ?
C23 N2 C19 . . 121.1(4) ?
C23 N2 C18 . . 120.2(3) ?
C19 N2 C18 . . 118.8(3) ?
C35 N3 C37 . . 118.8(5) ?
C35 N3 C38 . . 123.1(5) ?
C37 N3 C38 . . 117.9(5) ?
O4 C1 O3 . . 127.7(4) ?
O4 C1 C2 . . 118.7(3) ?
O3 C1 C2 . . 113.6(4) ?
C6 C2 C3 . . 118.9(4) ?
C6 C2 C1 . . 120.2(3) ?
C3 C2 C1 . . 120.8(3) ?
C4 C3 C2 . . 119.4(4) ?
C4 C3 H3 . . 120.300000 ?
C2 C3 H3 . . 120.300000 ?
N1 C4 C3 . . 120.7(4) ?
N1 C4 H4 . . 119.700000 ?
C3 C4 H4 . . 119.700000 ?
N1 C5 C6 . . 120.6(4) ?
N1 C5 H5 . . 119.700000 ?
C6 C5 H5 . . 119.700000 ?
C5 C6 C2 . . 119.6(4) ?
C5 C6 H6 . . 120.200000 ?
C2 C6 H6 . . 120.200000 ?
N1 C7 C8 . . 114.5(3) ?
N1 C7 H7A . . 108.600000 ?
C8 C7 H7A . . 108.600000 ?
N1 C7 H7B . . 108.600000 ?
C8 C7 H7B . . 108.600000 ?
H7A C7 H7B . . 107.600000 ?
C13 C8 C9 . . 121.4(4) ?
C13 C8 C7 . . 119.0(4) ?
C9 C8 C7 . . 119.4(4) ?
C10 C9 C8 . . 119.1(4) ?
C10 C9 C14 . . 119.5(4) ?
C8 C9 C14 . . 121.4(4) ?
C9 C10 C11 . . 119.5(4) ?
C9 C10 C15 . . 118.6(4) ?
C11 C10 C15 . . 121.9(4) ?
C10 C11 C12 . . 121.0(4) ?
C10 C11 C18 . . 120.3(4) ?
C12 C11 C18 . . 118.7(4) ?
C13 C12 C11 . . 119.4(4) ?
C13 C12 C16 . . 119.8(4) ?
C11 C12 C16 . . 120.8(4) ?
C12 C13 C8 . . 119.0(4) ?
C12 C13 C17 . . 120.0(4) ?
C8 C13 C17 . . 121.1(4) ?
C9 C14 H14A . . 109.500000 ?
C9 C14 H14B . . 109.500000 ?
H14A C14 H14B . . 109.500000 ?
C9 C14 H14C . . 109.500000 ?
H14A C14 H14C . . 109.500000 ?
H14B C14 H14C . . 109.500000 ?
C10 C15 H15C . . 109.500000 ?
C10 C15 H15D . . 109.500000 ?
H15C C15 H15D . . 109.500000 ?
C10 C15 H15E . . 109.500000 ?
H15C C15 H15E . . 109.500000 ?
H15D C15 H15E . . 109.500000 ?
C12 C16 H16C . . 109.500000 ?
C12 C16 H16D . . 109.500000 ?
H16C C16 H16D . . 109.500000 ?
C12 C16 H16E . . 109.500000 ?
H16C C16 H16E . . 109.500000 ?
H16D C16 H16E . . 109.500000 ?
C13 C17 H17A . . 109.500000 ?
C13 C17 H17B . . 109.500000 ?
H17A C17 H17B . . 109.500000 ?
C13 C17 H17C . . 109.500000 ?
H17A C17 H17C . . 109.500000 ?
H17B C17 H17C . . 109.500000 ?
N2 C18 C11 . . 111.6(3) ?
N2 C18 H18C . . 109.300000 ?
C11 C18 H18C . . 109.300000 ?
N2 C18 H18D . . 109.300000 ?
C11 C18 H18D . . 109.300000 ?
H18C C18 H18D . . 108.000000 ?
N2 C19 C20 . . 119.9(4) ?
N2 C19 H19 . . 120.100000 ?
C20 C19 H19 . . 120.100000 ?
C19 C20 C21 . . 120.3(4) ?
C19 C20 H20 . . 119.800000 ?
C21 C20 H20 . . 119.800000 ?
C20 C21 C22 . . 118.9(4) ?
C20 C21 C24 . . 120.6(4) ?
C22 C21 C24 . . 120.4(4) ?
C23 C22 C21 . . 119.7(4) ?
C23 C22 H22 . . 120.200000 ?
C21 C22 H22 . . 120.200000 ?
N2 C23 C22 . . 120.1(4) ?
N2 C23 H23 . . 119.900000 ?
C22 C23 H23 . . 119.900000 ?
O6 C24 O5 . . 127.1(4) ?
O6 C24 C21 . . 118.3(4) ?
O5 C24 C21 . . 114.6(4) ?
C30 C25 C26 . . 117.6(3) ?
C30 C25 C31 . . 117.9(3) ?
C26 C25 C31 . . 124.5(3) ?
C27 C26 C25 . . 119.6(3) ?
C27 C26 C32 . . 120.0(3) ?
C25 C26 C32 . . 120.4(3) ?
C26 C27 C28 . . 123.1(3) ?
C26 C27 H27 . . 118.500000 ?
C28 C27 H27 . . 118.500000 ?
C27 C28 C29 . . 117.7(3) ?
C27 C28 C33 . . 112.9(3) ?
C29 C28 C33 . . 129.4(3) ?
C30 C29 C28 . . 118.6(3) ?
C30 C29 C34 . . 114.1(3) ?
C28 C29 C34 . . 127.3(3) ?
C29 C30 C25 . . 123.5(3) ?
C29 C30 H30 . . 118.300000 ?
C25 C30 H30 . . 118.300000 ?
O8 C31 O7 . . 127.4(3) ?
O8 C31 C25 . . 118.2(3) ?
O7 C31 C25 . . 114.2(3) ?
O9 C32 O10 . . 123.9(3) ?
O9 C32 C26 . . 122.5(3) ?
O10 C32 C26 . . 113.6(3) ?
O11 C33 O12 . . 120.3(4) ?
O11 C33 C28 . . 120.0(3) ?
O12 C33 C28 . . 119.7(3) ?
O14 C34 O13 . . 122.7(3) ?
O14 C34 C29 . . 117.2(3) ?
O13 C34 C29 . . 120.0(3) ?
O17 C35 N3 . . 119.8(5) ?
O17 C35 C36 . . 121.6(5) ?
N3 C35 C36 . . 118.6(5) ?
C35 C36 H36A . . 109.500000 ?
C35 C36 H36B . . 109.500000 ?
H36A C36 H36B . . 109.500000 ?
C35 C36 H36C . . 109.500000 ?
H36A C36 H36C . . 109.500000 ?
H36B C36 H36C . . 109.500000 ?
N3 C37 H37A . . 109.500000 ?
N3 C37 H37B . . 109.500000 ?
H37A C37 H37B . . 109.500000 ?
N3 C37 H37C . . 109.500000 ?
H37A C37 H37C . . 109.500000 ?
H37B C37 H37C . . 109.500000 ?
N3 C38 H38A . . 109.500000 ?
N3 C38 H38B . . 109.500000 ?
H38A C38 H38B . . 109.500000 ?
N3 C38 H38C . . 109.500000 ?
H38A C38 H38C . . 109.500000 ?
H38B C38 H38C . . 109.500000 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O10 H10 O14 1_545 0.892(14) 1.658(19) 2.535(4) 167.(5) ?
O12 H12 O13 . 0.896(14) 1.506(15) 2.402(4) 178.(6) ?
O15 H15A O9 . 0.824(14) 1.971(15) 2.792(4) 175.(5) ?
O15 H15B O18 3 0.821(14) 1.841(16) 2.660(5) 175.(6) ?
O16 H16A O11 3_554 0.834(14) 1.928(17) 2.755(4) 171.(5) ?
O16 H16B O17 1_565 0.834(14) 1.769(17) 2.592(4) 169.(5) ?
O18 H18A O8 2_664 0.844(14) 2.021(16) 2.859(4) 173.(6) ?
O18 H18B O6 . 0.839(14) 1.997(15) 2.835(5) 177.(7) ?
C4 H4 O1 4_465 0.950000 2.370000 3.153(5) 139.500000 ?
C5 H5 O10 3_554 0.950000 2.470000 3.174(5) 131.300000 ?
C7 H7A O4 4_465 0.990000 2.340000 3.234(5) 149.500000 ?
C7 H7B O17 4_455 0.990000 2.310000 3.130(5) 139.600000 ?
C18 H18C O7 2_564 0.990000 2.480000 3.106(5) 121.000000 ?
C19 H19 O9 3_554 0.950000 2.300000 3.009(5) 130.500000 ?
C23 H23 O6 4_455 0.950000 2.130000 3.078(5) 172.700000 ?
C37 H37C O12 2_664 0.980000 2.570000 3.539(6) 168.100000 ?
C38 H38C O2 4_565 0.980000 2.440000 3.381(7) 159.700000 ?


####################################################################### 
# 
# 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 2202987'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2022-08-23 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT420_2                   
;
PROBLEM: D-H Bond Without Acceptor  O16      --H16B     .     Please Check 
RESPONSE: This H atom is probably involved in hydrogen bonding 
to one of the disordered water molecules whose contribution to the
structure factors was subtracted with SQUEEZE.
;
_vrf_PLAT971_2                   
;
PROBLEM: Check Calcd Resid. Dens.  2.35Ang From O16             2.56 eA-3  
RESPONSE: This residual electron density corresponds to a badly resolved
and disordered water molecule.
;
# end Validation Reply Form

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C86 H96 N6 O34 S2 U2'
_chemical_formula_iupac          ?
_chemical_formula_weight         2297.86

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.2147(4)
_cell_length_b                   14.8422(5)
_cell_length_c                   17.7684(5)
_cell_angle_alpha                96.2142(11)
_cell_angle_beta                 90.5305(15)
_cell_angle_gamma                91.3134(17)
_cell_volume                     2415.04(15)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9833
_cell_measurement_theta_min      2.4786
_cell_measurement_theta_max      33.1211
_cell_measurement_temperature    100(2)

_exptl_crystal_description       irregular
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.086
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1142

_exptl_absorpt_coefficient_mu    3.476
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_T_max  0.74

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100(2)

_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms 70 W'
_diffrn_source_current           1.4
_diffrn_source_voltage           50

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'multilayer mirror optics'

_diffrn_measurement_device       'Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_detector_area_resol_mean 7.41

_diffrn_reflns_number            93059
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_full        28.70
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24

_refine_special_details          
;
The H atoms of water molecules have been found and refined
with restraints on bond lengths and with an isotropic displacement
parameter equal to 1.5 times that of the attached O atom. Some
voids indicate the presence of other, badly resolved and probably
disordered water molecules, whose contribution to the structure
factors has been subtracted with SQUEEZE.
;

_reflns_number_total             12483
_reflns_number_gt                11921
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0209
_refine_ls_wR_factor_gt          0.0521
_refine_ls_wR_factor_ref         0.0528
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.095
_refine_ls_number_reflns         12483
_refine_ls_number_parameters     616
_refine_ls_number_restraints     24
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0225P)²+3.5119P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         2.846
_refine_diff_density_min         -1.201
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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

_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1328)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U U1 0.59384(2) 0.37894(2) 0.66319(2) 0.01163(3) Uani d . . . 1 . .
S S1 0.78190(6) 0.83657(4) 0.90855(3) 0.01670(10) Uani d . . . 1 . .
O O1 0.66622(17) 0.44840(10) 0.59632(9) 0.0168(3) Uani d . . . 1 . .
O O2 0.51844(17) 0.31091(11) 0.73022(9) 0.0171(3) Uani d . . . 1 . .
O O3 0.37142(17) 0.36881(12) 0.59641(9) 0.0220(3) Uani d . . . 1 . .
O O4 0.2527(3) 0.24163(17) 0.61754(18) 0.0740(10) Uani d U . . 1 . .
O O5 -0.64599(18) -0.25603(10) 0.42286(9) 0.0193(3) Uani d . . . 1 . .
O O6 -0.6537(5) -0.13830(18) 0.50914(14) 0.0808(11) Uani d U . . 1 . .
O O7 0.81856(16) 0.33541(11) 0.71089(9) 0.0177(3) Uani d . . . 1 . .
O O8 0.98119(18) 0.43148(13) 0.66740(10) 0.0255(4) Uani d . . . 1 . .
O O9 0.67918(17) 0.50199(11) 0.76058(9) 0.0190(3) Uani d . . . 1 . .
O O10 0.45076(16) 0.50425(10) 0.72362(9) 0.0165(3) Uani d . . . 1 . .
O O11 0.90297(18) 0.77925(12) 0.92259(10) 0.0244(4) Uani d . . . 1 . .
O O12 0.7385(2) 0.89354(12) 0.97630(9) 0.0259(4) Uani d . . . 1 . .
O O13 0.80319(18) 0.88798(11) 0.84418(9) 0.0203(3) Uani d . . . 1 . .
O O14 1.1166(2) 0.82222(13) 1.03709(11) 0.0282(4) Uani d . . D 1 . .
H H14A 1.063(3) 0.820(2) 0.9982(12) 0.042000 Uiso d U . D 1 . .
H H14B 1.184(3) 0.8594(19) 1.0316(17) 0.042000 Uiso d U . D 1 . .
O O15 1.3550(2) 0.93117(14) 1.03552(16) 0.0456(6) Uani d . . D 1 . .
H H15A 1.390(5) 0.928(3) 1.0786(12) 0.068000 Uiso d U . D 1 . .
H H15B 1.332(5) 0.9858(11) 1.034(2) 0.068000 Uiso d U . D 1 . .
O O16 1.5985(2) 0.88654(18) 1.11507(12) 0.0421(5) Uani d . . D 1 . .
H H16A 1.658(3) 0.888(3) 1.0797(14) 0.063000 Uiso d U . D 1 . .
H H16B 1.642(4) 0.868(3) 1.1514(14) 0.063000 Uiso d U . D 1 . .
O O17 0.9260(3) 1.06868(17) 0.82706(15) 0.0510(6) Uani d . . D 1 . .
H H17A 0.923(5) 1.0134(10) 0.831(2) 0.077000 Uiso d U . D 1 . .
H H17B 0.956(5) 1.076(3) 0.7841(13) 0.077000 Uiso d U . D 1 . .
N N1 -0.06136(19) 0.37417(12) 0.43201(10) 0.0147(3) Uani d . . . 1 . .
N N2 -0.5078(2) 0.00896(12) 0.28562(10) 0.0154(3) Uani d . . . 1 . .
N N3 1.2310(2) 0.34279(13) 0.89260(10) 0.0157(3) Uani d . . . 1 . .
C C1 0.2663(3) 0.31114(17) 0.58787(15) 0.0275(5) Uani d . . . 1 . .
C C2 0.1484(2) 0.33441(16) 0.53352(13) 0.0189(4) Uani d . . . 1 . .
C C3 0.0148(3) 0.28863(18) 0.52913(14) 0.0257(5) Uani d . . . 1 . .
H H3 -0.004832 0.242787 0.561273 0.031000 Uiso calc U . R 1 . .
C C4 -0.0890(3) 0.30988(17) 0.47804(13) 0.0224(5) Uani d . . . 1 . .
H H4 -0.180620 0.278930 0.475352 0.027000 Uiso calc U . R 1 . .
C C5 0.0666(2) 0.42034(14) 0.43532(12) 0.0148(4) Uani d . . . 1 . .
H H5 0.083803 0.465944 0.402624 0.018000 Uiso calc U . R 1 . .
C C6 0.1733(2) 0.40124(15) 0.48647(12) 0.0154(4) Uani d . . . 1 . .
H H6 0.263282 0.434054 0.489139 0.018000 Uiso calc U . R 1 . .
C C7 -0.1754(2) 0.39680(15) 0.37650(13) 0.0189(4) Uani d . . . 1 . .
H H7A -0.129294 0.429971 0.337236 0.023000 Uiso calc U . R 1 . .
H H7B -0.246939 0.437128 0.403223 0.023000 Uiso calc U . R 1 . .
C C8 -0.2532(2) 0.31300(14) 0.33894(12) 0.0144(4) Uani d . . . 1 . .
C C9 -0.1783(2) 0.25435(15) 0.28635(12) 0.0163(4) Uani d . . . 1 . .
C C10 -0.2485(2) 0.17503(15) 0.25247(12) 0.0162(4) Uani d . . . 1 . .
C C11 -0.3957(2) 0.15956(14) 0.26738(11) 0.0134(4) Uani d . . . 1 . .
C C12 -0.4718(2) 0.22001(14) 0.31808(11) 0.0129(4) Uani d . . . 1 . .
C C13 -0.3982(2) 0.29543(14) 0.35678(11) 0.0132(4) Uani d . . . 1 . .
C C14 -0.0228(3) 0.27533(18) 0.26587(15) 0.0264(5) Uani d . . . 1 . .
H H14C 0.000371 0.339486 0.281290 0.040000 Uiso calc U . R 1 . .
H H14D -0.010940 0.262393 0.211042 0.040000 Uiso calc U . R 1 . .
H H14E 0.042804 0.237676 0.292050 0.040000 Uiso calc U . R 1 . .
C C15 -0.1678(3) 0.10761(18) 0.19996(17) 0.0300(6) Uani d . . . 1 . .
H H15C -0.185523 0.046459 0.214359 0.045000 Uiso calc U . R 1 . .
H H15D -0.063520 0.122312 0.203544 0.045000 Uiso calc U . R 1 . .
H H15E -0.201684 0.110226 0.147823 0.045000 Uiso calc U . R 1 . .
C C16 -0.6298(2) 0.20309(16) 0.33411(13) 0.0198(4) Uani d . . . 1 . .
H H16C -0.638430 0.175640 0.381655 0.030000 Uiso calc U . R 1 . .
H H16D -0.673083 0.161931 0.292675 0.030000 Uiso calc U . R 1 . .
H H16E -0.680552 0.260680 0.338411 0.030000 Uiso calc U . R 1 . .
C C17 -0.4782(3) 0.35376(16) 0.41657(13) 0.0202(4) Uani d . . . 1 . .
H H17C -0.540446 0.395156 0.392352 0.030000 Uiso calc U . R 1 . .
H H17D -0.408113 0.388951 0.450383 0.030000 Uiso calc U . R 1 . .
H H17E -0.538133 0.315141 0.445887 0.030000 Uiso calc U . R 1 . .
C C18 -0.4731(2) 0.07578(14) 0.23019(12) 0.0157(4) Uani d . . . 1 . .
H H18A -0.564301 0.093310 0.206404 0.019000 Uiso calc U . R 1 . .
H H18B -0.411419 0.046552 0.189695 0.019000 Uiso calc U . R 1 . .
C C19 -0.4333(3) 0.01060(16) 0.35079(13) 0.0233(5) Uani d . . . 1 . .
H H19 -0.354956 0.052911 0.361503 0.028000 Uiso calc U . R 1 . .
C C20 -0.4697(3) -0.04888(17) 0.40242(14) 0.0271(5) Uani d . . . 1 . .
H H20 -0.417890 -0.046713 0.449081 0.032000 Uiso calc U . R 1 . .
C C21 -0.5820(3) -0.11178(16) 0.38612(13) 0.0249(5) Uani d . . . 1 . .
C C22 -0.6531(3) -0.11497(16) 0.31694(13) 0.0236(5) Uani d . . . 1 . .
H H22 -0.727054 -0.159613 0.303426 0.028000 Uiso calc U . R 1 . .
C C23 -0.6157(3) -0.05270(15) 0.26780(13) 0.0196(4) Uani d . . . 1 . .
H H23 -0.666349 -0.053298 0.220942 0.023000 Uiso calc U . R 1 . .
C C24 -0.6287(4) -0.17310(18) 0.44476(14) 0.0340(7) Uani d . . . 1 . .
C C25 0.9407(2) 0.37783(15) 0.71133(12) 0.0163(4) Uani d . . . 1 . .
C C26 1.0443(2) 0.36011(14) 0.77427(12) 0.0149(4) Uani d . . . 1 . .
C C27 1.1817(2) 0.40059(15) 0.77681(12) 0.0169(4) Uani d . . . 1 . .
H H27 1.212056 0.434849 0.737347 0.020000 Uiso calc U . R 1 . .
C C28 1.2738(2) 0.39103(15) 0.83651(12) 0.0171(4) Uani d . . . 1 . .
H H28 1.368034 0.418575 0.838205 0.021000 Uiso calc U . R 1 . .
C C29 1.1009(2) 0.29983(16) 0.89022(13) 0.0188(4) Uani d . . . 1 . .
H H29 1.074761 0.263982 0.929368 0.023000 Uiso calc U . R 1 . .
C C30 1.0051(2) 0.30741(15) 0.83135(13) 0.0182(4) Uani d . . . 1 . .
H H30 0.913121 0.276951 0.829748 0.022000 Uiso calc U . R 1 . .
C C31 1.3307(3) 0.33478(16) 0.95862(12) 0.0198(4) Uani d . . . 1 . .
H H31A 1.396711 0.283836 0.945837 0.024000 Uiso calc U . R 1 . .
H H31B 1.272487 0.320902 1.002671 0.024000 Uiso calc U . R 1 . .
C C32 1.4194(2) 0.42042(16) 0.97973(12) 0.0174(4) Uani d . . . 1 . .
C C33 1.3540(2) 0.49406(16) 1.02149(12) 0.0180(4) Uani d . . . 1 . .
C C34 1.5652(2) 0.42581(16) 0.95750(12) 0.0178(4) Uani d . . . 1 . .
C C35 1.1963(2) 0.48963(19) 1.04458(14) 0.0249(5) Uani d . . . 1 . .
H H35A 1.190828 0.488370 1.099509 0.037000 Uiso calc U . R 1 . .
H H35B 1.149409 0.434631 1.018918 0.037000 Uiso calc U . R 1 . .
H H35C 1.146649 0.543021 1.030229 0.037000 Uiso calc U . R 1 . .
C C36 1.6373(3) 0.34847(17) 0.91113(14) 0.0237(5) Uani d . . . 1 . .
H H36A 1.706851 0.320514 0.943035 0.036000 Uiso calc U . R 1 . .
H H36B 1.688455 0.371517 0.868770 0.036000 Uiso calc U . R 1 . .
H H36C 1.563500 0.303181 0.891484 0.036000 Uiso calc U . R 1 . .
C C37 0.5573(2) 0.53936(15) 0.76388(12) 0.0158(4) Uani d . . . 1 . .
C C38 0.5357(2) 0.62411(14) 0.81509(11) 0.0146(4) Uani d . . . 1 . .
C C39 0.6541(2) 0.68122(14) 0.83676(11) 0.0149(4) Uani d . . . 1 . .
H H39 0.748742 0.665940 0.819769 0.018000 Uiso calc U . R 1 . .
C C40 0.6321(2) 0.76117(14) 0.88373(11) 0.0146(4) Uani d . . . 1 . .
C C41 0.4948(2) 0.78220(15) 0.91102(12) 0.0171(4) Uani d . . . 1 . .
H H41 0.480935 0.836213 0.943763 0.021000 Uiso calc U . R 1 . .
C C42 0.3777(2) 0.72361(16) 0.89009(12) 0.0185(4) Uani d . . . 1 . .
H H42 0.283945 0.737151 0.909354 0.022000 Uiso calc U . R 1 . .
C C43 0.3973(2) 0.64562(15) 0.84127(12) 0.0169(4) Uani d . . . 1 . .
H H43 0.316616 0.606899 0.825676 0.020000 Uiso calc U . R 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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
U1 O2 . 1.7788(15) ?
U1 O1 . 1.7798(15) ?
U1 O5 2_556 2.3123(16) ?
U1 O3 . 2.3523(16) ?
U1 O7 . 2.3603(15) ?
U1 O10 . 2.4610(15) ?
U1 O9 . 2.4845(15) ?
S1 O11 . 1.4543(18) ?
S1 O13 . 1.4544(17) ?
S1 O12 . 1.4587(17) ?
S1 C40 . 1.779(2) ?
O3 C1 . 1.275(3) ?
O4 C1 . 1.213(3) ?
O5 C24 . 1.256(3) ?
O6 C24 . 1.229(4) ?
O7 C25 . 1.276(3) ?
O8 C25 . 1.229(3) ?
O9 C37 . 1.263(3) ?
O10 C37 . 1.276(3) ?
O14 H14A . 0.842(10) ?
O14 H14B . 0.837(10) ?
O15 H15A . 0.835(10) ?
O15 H15B . 0.847(10) ?
O16 H16A . 0.839(10) ?
O16 H16B . 0.835(10) ?
O17 H17A . 0.832(10) ?
O17 H17B . 0.833(10) ?
N1 C4 . 1.344(3) ?
N1 C5 . 1.348(3) ?
N1 C7 . 1.503(3) ?
N2 C19 . 1.339(3) ?
N2 C23 . 1.347(3) ?
N2 C18 . 1.503(3) ?
N3 C29 . 1.343(3) ?
N3 C28 . 1.346(3) ?
N3 C31 . 1.500(3) ?
C1 C2 . 1.517(3) ?
C2 C6 . 1.381(3) ?
C2 C3 . 1.389(3) ?
C3 C4 . 1.378(3) ?
C3 H3 . 0.950000 ?
C4 H4 . 0.950000 ?
C5 C6 . 1.387(3) ?
C5 H5 . 0.950000 ?
C6 H6 . 0.950000 ?
C7 C8 . 1.509(3) ?
C7 H7A . 0.990000 ?
C7 H7B . 0.990000 ?
C8 C13 . 1.401(3) ?
C8 C9 . 1.404(3) ?
C9 C10 . 1.404(3) ?
C9 C14 . 1.515(3) ?
C10 C11 . 1.402(3) ?
C10 C15 . 1.507(3) ?
C11 C12 . 1.405(3) ?
C11 C18 . 1.505(3) ?
C12 C13 . 1.406(3) ?
C12 C16 . 1.507(3) ?
C13 C17 . 1.505(3) ?
C14 H14C . 0.980000 ?
C14 H14D . 0.980000 ?
C14 H14E . 0.980000 ?
C15 H15C . 0.980000 ?
C15 H15D . 0.980000 ?
C15 H15E . 0.980000 ?
C16 H16C . 0.980000 ?
C16 H16D . 0.980000 ?
C16 H16E . 0.980000 ?
C17 H17C . 0.980000 ?
C17 H17D . 0.980000 ?
C17 H17E . 0.980000 ?
C18 H18A . 0.990000 ?
C18 H18B . 0.990000 ?
C19 C20 . 1.379(3) ?
C19 H19 . 0.950000 ?
C20 C21 . 1.385(4) ?
C20 H20 . 0.950000 ?
C21 C22 . 1.383(3) ?
C21 C24 . 1.515(3) ?
C22 C23 . 1.379(3) ?
C22 H22 . 0.950000 ?
C23 H23 . 0.950000 ?
C25 C26 . 1.513(3) ?
C26 C27 . 1.387(3) ?
C26 C30 . 1.392(3) ?
C27 C28 . 1.374(3) ?
C27 H27 . 0.950000 ?
C28 H28 . 0.950000 ?
C29 C30 . 1.378(3) ?
C29 H29 . 0.950000 ?
C30 H30 . 0.950000 ?
C31 C32 . 1.506(3) ?
C31 H31A . 0.990000 ?
C31 H31B . 0.990000 ?
C32 C33 . 1.404(3) ?
C32 C34 . 1.407(3) ?
C33 C34 2_867 1.402(3) ?
C33 C35 . 1.516(3) ?
C34 C36 . 1.509(3) ?
C35 H35A . 0.980000 ?
C35 H35B . 0.980000 ?
C35 H35C . 0.980000 ?
C36 H36A . 0.980000 ?
C36 H36B . 0.980000 ?
C36 H36C . 0.980000 ?
C37 C38 . 1.489(3) ?
C38 C39 . 1.391(3) ?
C38 C43 . 1.394(3) ?
C39 C40 . 1.395(3) ?
C39 H39 . 0.950000 ?
C40 C41 . 1.389(3) ?
C41 C42 . 1.393(3) ?
C41 H41 . 0.950000 ?
C42 C43 . 1.386(3) ?
C42 H42 . 0.950000 ?
C43 H43 . 0.950000 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 U1 O1 . . 178.86(7) ?
O2 U1 O5 . 2_556 93.87(6) ?
O1 U1 O5 . 2_556 86.88(6) ?
O2 U1 O3 . . 89.76(7) ?
O1 U1 O3 . . 89.50(7) ?
O5 U1 O3 2_556 . 82.22(6) ?
O2 U1 O7 . . 84.27(6) ?
O1 U1 O7 . . 96.71(6) ?
O5 U1 O7 2_556 . 78.83(6) ?
O3 U1 O7 . . 159.66(6) ?
O2 U1 O10 . . 87.18(6) ?
O1 U1 O10 . . 91.79(6) ?
O5 U1 O10 2_556 . 157.24(6) ?
O3 U1 O10 . . 75.05(5) ?
O7 U1 O10 . . 123.85(5) ?
O2 U1 O9 . . 94.23(6) ?
O1 U1 O9 . . 85.54(6) ?
O5 U1 O9 2_556 . 149.29(6) ?
O3 U1 O9 . . 127.37(6) ?
O7 U1 O9 . . 72.59(5) ?
O10 U1 O9 . . 52.86(5) ?
O11 S1 O13 . . 113.57(11) ?
O11 S1 O12 . . 112.67(11) ?
O13 S1 O12 . . 112.39(11) ?
O11 S1 C40 . . 105.68(10) ?
O13 S1 C40 . . 105.86(10) ?
O12 S1 C40 . . 105.87(10) ?
C1 O3 U1 . . 135.12(16) ?
C24 O5 U1 . 2_556 149.00(17) ?
C25 O7 U1 . . 127.90(14) ?
C37 O9 U1 . . 93.10(13) ?
C37 O10 U1 . . 93.86(13) ?
H14A O14 H14B . . 106.8(16) ?
H15A O15 H15B . . 106.2(16) ?
H16A O16 H16B . . 107.5(17) ?
H17A O17 H17B . . 108.9(17) ?
C4 N1 C5 . . 121.25(19) ?
C4 N1 C7 . . 119.88(18) ?
C5 N1 C7 . . 118.86(18) ?
C19 N2 C23 . . 120.98(19) ?
C19 N2 C18 . . 120.83(18) ?
C23 N2 C18 . . 118.20(18) ?
C29 N3 C28 . . 121.28(19) ?
C29 N3 C31 . . 118.82(18) ?
C28 N3 C31 . . 119.88(18) ?
O4 C1 O3 . . 127.2(2) ?
O4 C1 C2 . . 118.5(2) ?
O3 C1 C2 . . 114.3(2) ?
C6 C2 C3 . . 118.7(2) ?
C6 C2 C1 . . 120.1(2) ?
C3 C2 C1 . . 121.2(2) ?
C4 C3 C2 . . 119.9(2) ?
C4 C3 H3 . . 120.100000 ?
C2 C3 H3 . . 120.100000 ?
N1 C4 C3 . . 120.3(2) ?
N1 C4 H4 . . 119.800000 ?
C3 C4 H4 . . 119.800000 ?
N1 C5 C6 . . 120.0(2) ?
N1 C5 H5 . . 120.000000 ?
C6 C5 H5 . . 120.000000 ?
C2 C6 C5 . . 119.8(2) ?
C2 C6 H6 . . 120.100000 ?
C5 C6 H6 . . 120.100000 ?
N1 C7 C8 . . 111.95(17) ?
N1 C7 H7A . . 109.200000 ?
C8 C7 H7A . . 109.200000 ?
N1 C7 H7B . . 109.200000 ?
C8 C7 H7B . . 109.200000 ?
H7A C7 H7B . . 107.900000 ?
C13 C8 C9 . . 121.39(19) ?
C13 C8 C7 . . 119.65(19) ?
C9 C8 C7 . . 118.96(19) ?
C8 C9 C10 . . 119.42(19) ?
C8 C9 C14 . . 121.0(2) ?
C10 C9 C14 . . 119.6(2) ?
C11 C10 C9 . . 119.21(19) ?
C11 C10 C15 . . 120.2(2) ?
C9 C10 C15 . . 120.6(2) ?
C10 C11 C12 . . 121.10(19) ?
C10 C11 C18 . . 119.77(19) ?
C12 C11 C18 . . 119.11(18) ?
C11 C12 C13 . . 119.59(19) ?
C11 C12 C16 . . 120.96(19) ?
C13 C12 C16 . . 119.40(19) ?
C8 C13 C12 . . 118.97(19) ?
C8 C13 C17 . . 122.51(19) ?
C12 C13 C17 . . 118.51(19) ?
C9 C14 H14C . . 109.500000 ?
C9 C14 H14D . . 109.500000 ?
H14C C14 H14D . . 109.500000 ?
C9 C14 H14E . . 109.500000 ?
H14C C14 H14E . . 109.500000 ?
H14D C14 H14E . . 109.500000 ?
C10 C15 H15C . . 109.500000 ?
C10 C15 H15D . . 109.500000 ?
H15C C15 H15D . . 109.500000 ?
C10 C15 H15E . . 109.500000 ?
H15C C15 H15E . . 109.500000 ?
H15D C15 H15E . . 109.500000 ?
C12 C16 H16C . . 109.500000 ?
C12 C16 H16D . . 109.500000 ?
H16C C16 H16D . . 109.500000 ?
C12 C16 H16E . . 109.500000 ?
H16C C16 H16E . . 109.500000 ?
H16D C16 H16E . . 109.500000 ?
C13 C17 H17C . . 109.500000 ?
C13 C17 H17D . . 109.500000 ?
H17C C17 H17D . . 109.500000 ?
C13 C17 H17E . . 109.500000 ?
H17C C17 H17E . . 109.500000 ?
H17D C17 H17E . . 109.500000 ?
N2 C18 C11 . . 112.13(17) ?
N2 C18 H18A . . 109.200000 ?
C11 C18 H18A . . 109.200000 ?
N2 C18 H18B . . 109.200000 ?
C11 C18 H18B . . 109.200000 ?
H18A C18 H18B . . 107.900000 ?
N2 C19 C20 . . 120.3(2) ?
N2 C19 H19 . . 119.900000 ?
C20 C19 H19 . . 119.900000 ?
C19 C20 C21 . . 119.8(2) ?
C19 C20 H20 . . 120.100000 ?
C21 C20 H20 . . 120.100000 ?
C22 C21 C20 . . 118.8(2) ?
C22 C21 C24 . . 121.2(2) ?
C20 C21 C24 . . 120.0(2) ?
C23 C22 C21 . . 119.3(2) ?
C23 C22 H22 . . 120.300000 ?
C21 C22 H22 . . 120.300000 ?
N2 C23 C22 . . 120.6(2) ?
N2 C23 H23 . . 119.700000 ?
C22 C23 H23 . . 119.700000 ?
O6 C24 O5 . . 124.5(2) ?
O6 C24 C21 . . 118.3(2) ?
O5 C24 C21 . . 117.1(2) ?
O8 C25 O7 . . 127.3(2) ?
O8 C25 C26 . . 117.44(19) ?
O7 C25 C26 . . 115.25(19) ?
C27 C26 C30 . . 118.7(2) ?
C27 C26 C25 . . 118.82(19) ?
C30 C26 C25 . . 122.39(19) ?
C28 C27 C26 . . 119.8(2) ?
C28 C27 H27 . . 120.100000 ?
C26 C27 H27 . . 120.100000 ?
N3 C28 C27 . . 120.2(2) ?
N3 C28 H28 . . 119.900000 ?
C27 C28 H28 . . 119.900000 ?
N3 C29 C30 . . 120.4(2) ?
N3 C29 H29 . . 119.800000 ?
C30 C29 H29 . . 119.800000 ?
C29 C30 C26 . . 119.4(2) ?
C29 C30 H30 . . 120.300000 ?
C26 C30 H30 . . 120.300000 ?
N3 C31 C32 . . 112.02(18) ?
N3 C31 H31A . . 109.200000 ?
C32 C31 H31A . . 109.200000 ?
N3 C31 H31B . . 109.200000 ?
C32 C31 H31B . . 109.200000 ?
H31A C31 H31B . . 107.900000 ?
C33 C32 C34 . . 121.1(2) ?
C33 C32 C31 . . 118.9(2) ?
C34 C32 C31 . . 120.0(2) ?
C34 C33 C32 2_867 . 120.0(2) ?
C34 C33 C35 2_867 . 118.5(2) ?
C32 C33 C35 . . 121.5(2) ?
C33 C34 C32 2_867 . 119.0(2) ?
C33 C34 C36 2_867 . 118.8(2) ?
C32 C34 C36 . . 122.2(2) ?
C33 C35 H35A . . 109.500000 ?
C33 C35 H35B . . 109.500000 ?
H35A C35 H35B . . 109.500000 ?
C33 C35 H35C . . 109.500000 ?
H35A C35 H35C . . 109.500000 ?
H35B C35 H35C . . 109.500000 ?
C34 C36 H36A . . 109.500000 ?
C34 C36 H36B . . 109.500000 ?
H36A C36 H36B . . 109.500000 ?
C34 C36 H36C . . 109.500000 ?
H36A C36 H36C . . 109.500000 ?
H36B C36 H36C . . 109.500000 ?
O9 C37 O10 . . 120.2(2) ?
O9 C37 C38 . . 120.54(19) ?
O10 C37 C38 . . 119.30(19) ?
C39 C38 C43 . . 120.4(2) ?
C39 C38 C37 . . 119.76(19) ?
C43 C38 C37 . . 119.86(19) ?
C38 C39 C40 . . 119.2(2) ?
C38 C39 H39 . . 120.400000 ?
C40 C39 H39 . . 120.400000 ?
C41 C40 C39 . . 120.6(2) ?
C41 C40 S1 . . 119.99(16) ?
C39 C40 S1 . . 119.37(16) ?
C40 C41 C42 . . 119.6(2) ?
C40 C41 H41 . . 120.200000 ?
C42 C41 H41 . . 120.200000 ?
C43 C42 C41 . . 120.3(2) ?
C43 C42 H42 . . 119.900000 ?
C41 C42 H42 . . 119.900000 ?
C42 C43 C38 . . 119.9(2) ?
C42 C43 H43 . . 120.100000 ?
C38 C43 H43 . . 120.100000 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O14 H14A O11 . 0.842(10) 2.024(12) 2.830(2) 160.(3) ?
O14 H14B O15 . 0.837(10) 1.876(11) 2.700(3) 168.(3) ?
O15 H15A O16 . 0.835(10) 2.15(3) 2.772(4) 132.(4) ?
O15 H15B O12 2_777 0.847(10) 1.944(11) 2.788(3) 174.(4) ?
O16 H16A O12 1_655 0.839(10) 1.997(14) 2.804(3) 161.(3) ?
O17 H17A O13 . 0.832(10) 2.18(2) 2.934(3) 152.(5) ?
C4 H4 O5 2_456 0.950000 2.470000 3.162(3) 129.600000 ?
C4 H4 O6 2_456 0.950000 2.600000 3.466(4) 152.100000 ?
C5 H5 O1 2_666 0.950000 2.600000 3.196(3) 120.700000 ?
C5 H5 O8 2_666 0.950000 2.160000 3.043(3) 154.300000 ?
C6 H6 O1 2_666 0.950000 2.510000 3.151(3) 124.700000 ?
C7 H7A O8 2_666 0.990000 2.450000 3.249(3) 137.300000 ?
C18 H18A O13 2_566 0.990000 2.400000 3.383(3) 170.000000 ?
C18 H18B O16 1_344 0.990000 2.600000 3.373(3) 135.400000 ?
C19 H19 O6 2_456 0.950000 2.500000 3.050(3) 116.800000 ?
C23 H23 O17 2_566 0.950000 2.530000 3.297(3) 137.900000 ?
C27 H27 O10 1_655 0.950000 2.430000 3.097(3) 126.800000 ?
C29 H29 O14 2_767 0.950000 2.280000 3.058(3) 139.100000 ?
C41 H41 O15 1_455 0.950000 2.370000 3.251(3) 154.500000 ?



####################################################################### 
# 
# 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 2202990'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2022-08-23 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT971_5                   
;
PROBLEM: Check Calcd Resid. Dens.  1.10Ang From O7              5.94 eA-3  
RESPONSE: The main residual electron density peaks are large and 
the two largest ones in particular are located 
in the vicinity of uranium-bound oxygen atoms. These peaks are 
reproducible
in experiments made on different crystals with varying size and shape, and
they do not vary significantly depending on the absorption correction made 
(multi-scan or based on crystal shape). There is no indication of twinning,
and these peaks cannot be interpreted as arising from obvious disorder in the 
model. In the absence of a better explanation, they could be hypothesized 
to come from the presence of small components (less than about 7%) of
differently oriented molecules, of which only uranium is apparent, or to 
an effect of truncation of Fourier series, known to produce such residues
in structures containing heavy atoms. Another, smaller peak close to atom 
C16 is also of unknown origin.

;
_vrf_PLAT975_5                   
;
PROBLEM: Check Calcd Resid. Dens.  1.10Ang From O7      .       5.94 eA-3  
RESPONSE: See answer above.
;
_vrf_PLAT306_5                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O28 Check 
RESPONSE: This oxygen atom pertains to a water molecule for which the H
atoms were not found.
;
_vrf_PLAT430_5                   
;
PROBLEM: Short Inter D...A Contact  O8       ..O30      .       2.76 Ang.  
RESPONSE: This contact corresponds to a hydrogen bond involving a
water molecule for which the H atoms were not found.
;
_vrf_PLAT976_5                   
;
PROBLEM: Check Calcd Resid. Dens.  1.04Ang From O6      .      -1.76 eA-3  
RESPONSE: This residual electron density peak is moderate with respect 
to those indicated above.
;
# end Validation Reply Form

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C108 H108 N6 O60 S6 U6'
_chemical_formula_iupac          ?
_chemical_formula_weight         4070.54

_chemical_melting_point          ?

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

_cell_length_a                   13.2023(7)
_cell_length_b                   31.6383(17)
_cell_length_c                   15.1219(8)
_cell_angle_alpha                90
_cell_angle_beta                 97.7928(16)
_cell_angle_gamma                90
_cell_volume                     6258.1(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9863
_cell_measurement_theta_min      2.3204
_cell_measurement_theta_max      26.3826
_cell_measurement_temperature    100(2)

_exptl_crystal_description       irregular
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.086
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.059
_exptl_crystal_density_diffrn    2.160
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3852

_exptl_absorpt_coefficient_mu    7.938
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_T_max  0.75

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100(2)

_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms 70 W'
_diffrn_source_current           1.4
_diffrn_source_voltage           50

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'multilayer mirror optics'

_diffrn_measurement_device       'Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_detector_area_resol_mean 7.41

_diffrn_reflns_number            113226
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18

_refine_special_details          
;
One thiophenedicarboxylate molecule is disordered
over two positions sharing the S atom and partly 
the carboxylate groups, which were refined with
occupancy parameters constrained to sum to unity.
The protons have been found for only three out of
six water molecules (one coordinated and two free),
and they were either refined with restraints on bond 
lengths (O25, O27) or treated as riding atoms (O26),
with in all cases an isotropic displacement parameter
equal to 1.5 times that of the parent atom.
;

_reflns_number_total             11873
_reflns_number_gt                10542
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0643
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1634
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_restrained_S_all      1.174
_refine_ls_number_reflns         11873
_refine_ls_number_parameters     901
_refine_ls_number_restraints     12
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0490P)²+130.3576P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         6.129
_refine_diff_density_min         -1.890
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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

_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1328)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U U1 0.31629(4) 0.48890(2) 1.06206(3) 0.04276(14) Uani d . . . 1.000000 . .
U U2 0.28036(3) 0.33224(2) 0.34926(3) 0.03525(13) Uani d . . . 1.000000 . .
U U3 0.19269(3) 0.66557(2) 0.44300(3) 0.03537(13) Uani d . . . 1.000000 . .
S S1 0.5341(2) 0.24818(9) 0.59463(19) 0.0340(6) Uani d . . . 1.000000 . .
S S2 0.2563(3) 0.50040(10) 0.3967(2) 0.0417(7) Uani d . . . 1.000000 . .
S S3 0.4446(2) 0.74982(9) 0.6916(2) 0.0348(6) Uani d . . . 1.000000 . .
O O1 0.2026(8) 0.5204(3) 1.0503(7) 0.058(3) Uani d . . . 1.000000 . .
O O2 0.4286(8) 0.4570(3) 1.0707(7) 0.055(2) Uani d . . . 1.000000 . .
O O3 0.1776(7) 0.3345(3) 0.4114(6) 0.050(2) Uani d . . . 1.000000 . .
O O4 0.3839(6) 0.3308(2) 0.2837(6) 0.042(2) Uani d . . . 1.000000 . .
O O5 0.0928(7) 0.6598(3) 0.5109(6) 0.045(2) Uani d . . . 1.000000 . .
O O6 0.2926(7) 0.6708(2) 0.3750(6) 0.0410(19) Uani d . . . 1.000000 . .
O O7 0.3311(8) 0.5117(3) 0.9208(6) 0.051(2) Uani d U . . 1.000000 . .
O O8 0.3767(8) 0.4904(3) 0.7902(6) 0.051(2) Uani d . . . 1.000000 . .
O O9 -0.0843(7) 0.9465(3) 0.5917(6) 0.048(2) Uani d . . . 1.000000 . .
O O10 -0.1272(8) 0.9788(3) 0.7080(7) 0.059(3) Uani d . . . 1.000000 . .
O O11 0.2173(7) 0.4370(3) 0.9839(6) 0.050(2) Uani d . . . 1.000000 . .
O O12 0.0745(9) 0.4285(4) 1.0477(7) 0.064(3) Uani d . . . 1.000000 . .
O O13 0.3943(7) 0.3052(3) 0.4791(5) 0.0407(19) Uani d . . . 1.000000 . .
O O14 0.3126(6) 0.2565(3) 0.3917(5) 0.0367(18) Uani d . . . 1.000000 . .
O O15 0.6863(6) 0.2155(3) 0.7415(5) 0.0381(18) Uani d . . . 1.000000 . .
O O16 0.6626(6) 0.1474(3) 0.7146(5) 0.0377(18) Uani d . . . 1.000000 . .
O O17 0.2695(7) 0.4112(3) 0.3337(6) 0.045(2) Uani d . . . 1.000000 . .
O O18A 0.385(3) 0.3898(11) 0.437(3) 0.051(9) Uani d . P . 0.41(2) A 1
O O18B 0.3456(18) 0.3856(8) 0.4634(17) 0.044(5) Uani d . P . 0.59(2) A 2
O O19 0.1909(7) 0.5888(3) 0.4082(6) 0.045(2) Uani d . . . 1.000000 . .
O O20 0.2859(11) 0.6069(3) 0.5309(8) 0.080(4) Uani d . . . 1.000000 . .
O O21 0.3114(7) 0.6915(3) 0.5733(6) 0.045(2) Uani d . . . 1.000000 . .
O O22 0.2206(6) 0.7400(3) 0.4923(6) 0.0378(18) Uani d . . . 1.000000 . .
O O23 0.5925(6) 0.7840(3) 0.8414(6) 0.0387(18) Uani d . . . 1.000000 . .
O O24 0.5690(7) 0.8510(3) 0.8090(6) 0.0407(19) Uani d . . . 1.000000 . .
O O25 0.2403(10) 0.4478(4) 1.1716(7) 0.078(4) Uani d . . D 1.000000 . .
H H25A 0.211(13) 0.425(3) 1.154(12) 0.118000 Uiso d U . D 1.000000 . .
H H25B 0.285(12) 0.442(5) 1.215(9) 0.118000 Uiso d U . D 1.000000 . .
O O26 0.4899(8) 0.3676(3) 1.0117(7) 0.061(3) Uani d . . . 1.000000 . .
H H26A 0.467741 0.395466 1.023193 0.091000 Uiso d U . R 1.000000 . .
H H26B 0.444031 0.354896 1.045673 0.091000 Uiso d U . R 1.000000 . .
O O27 0.3662(11) 0.3144(4) 0.0907(7) 0.070(3) Uani d . . D 1.000000 . .
H H27A 0.357(16) 0.315(5) 0.144(4) 0.105000 Uiso d U . D 1.000000 . .
H H27B 0.353(16) 0.290(2) 0.073(10) 0.105000 Uiso d U . D 1.000000 . .
O O28 0.1043(9) 0.5561(4) 0.8708(8) 0.069(3) Uani d . . . 1.000000 . .
O O29 0.2538(9) 0.6200(4) 0.0819(8) 0.071(3) Uani d . . . 1.000000 . .
O O30 0.7121(12) 0.5867(5) 0.1838(11) 0.104(5) Uani d . . . 1.000000 . .
N N1 0.3212(8) 0.6352(3) 0.8347(7) 0.042(2) Uani d . . . 1.000000 . .
N N2 0.0611(9) 0.8508(4) 0.7463(7) 0.049(3) Uani d . . . 1.000000 . .
N N3 0.0543(9) 0.4684(4) 0.7451(7) 0.047(3) Uani d . . . 1.000000 . .
C C1 0.3596(9) 0.5177(4) 0.8436(8) 0.040(3) Uani d . . . 1.000000 . .
C C2 0.3686(9) 0.5636(4) 0.8185(8) 0.039(3) Uani d . . . 1.000000 . .
C C3 0.3229(10) 0.5947(4) 0.8618(8) 0.043(3) Uani d . . . 1.000000 . .
H H3 0.291352 0.587420 0.912531 0.052000 Uiso calc U . R 1.000000 . .
C C4 0.3643(10) 0.6462(4) 0.7647(7) 0.039(3) Uani d . . . 1.000000 . .
H H4 0.358790 0.674591 0.744219 0.046000 Uiso calc U . R 1.000000 . .
C C5 0.4179(9) 0.6171(4) 0.7202(8) 0.041(3) Uani d . . . 1.000000 . .
H H5 0.452604 0.625633 0.672055 0.049000 Uiso calc U . R 1.000000 . .
C C6 0.4192(11) 0.5756(4) 0.7476(9) 0.047(3) Uani d . . . 1.000000 . .
H H6 0.454828 0.554998 0.718017 0.057000 Uiso calc U . R 1.000000 . .
C C7 0.2739(12) 0.6680(5) 0.8899(10) 0.056(4) Uani d . . . 1.000000 . .
H H7A 0.325155 0.676393 0.940853 0.067000 Uiso calc U . R 1.000000 . .
H H7B 0.215423 0.655053 0.914490 0.067000 Uiso calc U . R 1.000000 . .
C C8 0.2369(10) 0.7075(4) 0.8370(8) 0.042(3) Uani d . . . 1.000000 . .
C C9 0.1569(9) 0.7066(4) 0.7676(9) 0.042(3) Uani d . . . 1.000000 . .
C C10 0.1215(9) 0.7437(4) 0.7247(7) 0.039(3) Uani d . . . 1.000000 . .
C C11 0.1672(10) 0.7817(4) 0.7557(8) 0.041(3) Uani d . . . 1.000000 . .
C C12 0.2460(10) 0.7839(4) 0.8273(8) 0.038(3) Uani d . . . 1.000000 . .
C C13 0.2827(10) 0.7460(4) 0.8691(8) 0.041(3) Uani d . . . 1.000000 . .
C C14 0.1112(12) 0.6636(5) 0.7363(11) 0.058(4) Uani d . . . 1.000000 . .
H H14A 0.144614 0.641728 0.773190 0.087000 Uiso d U . R 1.000000 . .
H H14B 0.039374 0.663389 0.740590 0.087000 Uiso d U . R 1.000000 . .
H H14C 0.121414 0.658909 0.675310 0.087000 Uiso d U . R 1.000000 . .
C C15 0.0308(10) 0.7421(5) 0.6493(9) 0.052(3) Uani d . . . 1.000000 . .
H H15A -0.021056 0.762652 0.661359 0.078000 Uiso calc U . R 1.000000 . .
H H15B 0.001103 0.713637 0.646216 0.078000 Uiso calc U . R 1.000000 . .
H H15C 0.054680 0.748859 0.592381 0.078000 Uiso calc U . R 1.000000 . .
C C16 0.2929(11) 0.8260(4) 0.8591(10) 0.049(3) Uani d . . . 1.000000 . .
H H16A 0.272707 0.847747 0.813963 0.073000 Uiso calc U . R 1.000000 . .
H H16B 0.367540 0.823485 0.868713 0.073000 Uiso calc U . R 1.000000 . .
H H16C 0.268607 0.833989 0.915255 0.073000 Uiso calc U . R 1.000000 . .
C C17 0.3720(11) 0.7478(5) 0.9424(9) 0.051(3) Uani d . . . 1.000000 . .
H H17A 0.407550 0.774827 0.939749 0.076000 Uiso calc U . R 1.000000 . .
H H17B 0.419227 0.724568 0.934784 0.076000 Uiso calc U . R 1.000000 . .
H H17C 0.347297 0.745026 1.000407 0.076000 Uiso calc U . R 1.000000 . .
C C18 0.1296(14) 0.8205(5) 0.7004(11) 0.062(4) Uani d . . . 1.000000 . .
H H18A 0.090904 0.810886 0.643329 0.075000 Uiso calc U . R 1.000000 . .
H H18B 0.189789 0.836516 0.686122 0.075000 Uiso calc U . R 1.000000 . .
C C19 0.0164(11) 0.8818(4) 0.6946(9) 0.050(3) Uani d . . . 1.000000 . .
H H19 0.022772 0.882457 0.632785 0.060000 Uiso calc U . R 1.000000 . .
C C20 -0.0399(10) 0.9133(5) 0.7320(9) 0.048(3) Uani d . . . 1.000000 . .
C C21 -0.0534(10) 0.9097(4) 0.8222(8) 0.044(3) Uani d . . . 1.000000 . .
H H21 -0.092060 0.930103 0.849286 0.052000 Uiso calc U . R 1.000000 . .
C C22 -0.0098(9) 0.8762(4) 0.8703(8) 0.038(3) Uani d . . . 1.000000 . .
H H22 -0.021034 0.872550 0.930582 0.046000 Uiso calc U . R 1.000000 . .
C C23 0.0502(9) 0.8477(4) 0.8324(8) 0.037(3) Uani d . . . 1.000000 . .
H H23 0.083968 0.825792 0.867729 0.045000 Uiso calc U . R 1.000000 . .
C C24 -0.0850(10) 0.9482(4) 0.6751(9) 0.044(3) Uani d . . . 1.000000 . .
C C25 0.1176(12) 0.4345(5) 0.9827(10) 0.055(4) Uani d . . . 1.000000 . .
C C26 0.0566(11) 0.4424(4) 0.8923(9) 0.049(3) Uani d . . . 1.000000 . .
C C27 0.1049(11) 0.4623(4) 0.8274(9) 0.050(3) Uani d . . . 1.000000 . .
H H27 0.173660 0.471562 0.841214 0.060000 Uiso calc U . R 1.000000 . .
C C28 -0.0433(11) 0.4554(4) 0.7236(9) 0.048(3) Uani d . . . 1.000000 . .
H H28 -0.076912 0.459230 0.664555 0.058000 Uiso calc U . R 1.000000 . .
C C29 -0.0946(11) 0.4365(4) 0.7868(9) 0.048(3) Uani d . . . 1.000000 . .
H H29 -0.163787 0.428038 0.771544 0.058000 Uiso calc U . R 1.000000 . .
C C30 -0.0440(11) 0.4297(4) 0.8741(9) 0.047(3) Uani d . . . 1.000000 . .
H H30 -0.077997 0.416854 0.918659 0.057000 Uiso calc U . R 1.000000 . .
C C31 0.1114(11) 0.4900(5) 0.6793(9) 0.051(3) Uani d . . . 1.000000 . .
H H31A 0.174140 0.473575 0.673860 0.061000 Uiso calc U . R 1.000000 . .
H H31B 0.132811 0.518277 0.702714 0.061000 Uiso calc U . R 1.000000 . .
C C32 0.0508(9) 0.4952(4) 0.5864(8) 0.040(3) Uani d . . . 1.000000 . .
C C33 0.0476(10) 0.4610(4) 0.5253(9) 0.046(3) Uani d . . . 1.000000 . .
C C34 -0.0036(10) 0.4658(4) 0.4381(8) 0.041(3) Uani d . . . 1.000000 . .
C C35 0.0936(11) 0.4189(4) 0.5521(10) 0.054(3) Uani d . . . 1.000000 . .
H H35A 0.132255 0.420922 0.611996 0.080000 Uiso calc U . R 1.000000 . .
H H35B 0.139618 0.410349 0.509572 0.080000 Uiso calc U . R 1.000000 . .
H H35C 0.039122 0.397887 0.552112 0.080000 Uiso calc U . R 1.000000 . .
C C36 -0.0021(13) 0.4298(5) 0.3723(10) 0.058(4) Uani d . . . 1.000000 . .
H H36A 0.062648 0.414449 0.384946 0.087000 Uiso calc U . R 1.000000 . .
H H36B -0.008950 0.441230 0.311473 0.087000 Uiso calc U . R 1.000000 . .
H H36C -0.059058 0.410578 0.377711 0.087000 Uiso calc U . R 1.000000 . .
C C37 0.3799(10) 0.2663(4) 0.4574(8) 0.039(3) Uani d . . . 1.000000 . .
C C38 0.4400(9) 0.2332(4) 0.5080(8) 0.035(2) Uani d . . . 1.000000 . .
C C39 0.4337(9) 0.1908(4) 0.4992(8) 0.038(3) Uani d . . . 1.000000 . .
H H39 0.387034 0.176935 0.455216 0.045000 Uiso calc U . R 1.000000 . .
C C40 0.5046(9) 0.1690(4) 0.5629(8) 0.035(2) Uani d . . . 1.000000 . .
H H40 0.510647 0.139055 0.566152 0.042000 Uiso calc U . R 1.000000 . .
C C41 0.5626(9) 0.1961(4) 0.6184(8) 0.035(2) Uani d . . . 1.000000 . .
C C42 0.6416(9) 0.1856(4) 0.6944(8) 0.037(3) Uani d . . . 1.000000 . .
C C43 0.3203(13) 0.4179(5) 0.4110(11) 0.063(4) Uani d . . . 1.000000 . .
C C44A 0.348(3) 0.4611(14) 0.437(4) 0.050(11) Uani d . P . 0.41(2) A 1
C C45A 0.415(3) 0.4801(10) 0.495(2) 0.048(9) Uani d . P . 0.41(2) A 1
H H45A 0.471795 0.464721 0.523571 0.058000 Uiso calc U P R 0.41(2) A 1
C C46A 0.405(3) 0.5204(12) 0.514(2) 0.057(10) Uani d . P . 0.41(2) A 1
H H46A 0.454511 0.536553 0.550754 0.068000 Uiso calc U P R 0.41(2) A 1
C C47A 0.309(3) 0.5363(14) 0.472(3) 0.029(9) Uani d . P . 0.41(2) A 1
C C44B 0.305(2) 0.4597(9) 0.456(2) 0.042(7) Uani d . P . 0.59(2) A 2
C C45B 0.3366(18) 0.4694(7) 0.5469(17) 0.051(7) Uani d . P . 0.59(2) A 2
H H45B 0.363824 0.449823 0.591410 0.061000 Uiso calc U P R 0.59(2) A 2
C C46B 0.3218(16) 0.5117(6) 0.5605(14) 0.040(5) Uani d . P . 0.59(2) A 2
H H46B 0.342512 0.524931 0.616444 0.048000 Uiso calc U P R 0.59(2) A 2
C C47B 0.274(3) 0.5342(14) 0.486(3) 0.044(9) Uani d . P . 0.59(2) A 2
C C48 0.2568(12) 0.5794(4) 0.4729(10) 0.053(3) Uani d . . . 1.000000 . .
C C49 0.2921(10) 0.7303(4) 0.5538(8) 0.038(3) Uani d . . . 1.000000 . .
C C50 0.3499(9) 0.7643(4) 0.6065(8) 0.036(3) Uani d . . . 1.000000 . .
C C51 0.3412(9) 0.8065(4) 0.5949(8) 0.037(3) Uani d . . . 1.000000 . .
H H51 0.295648 0.819755 0.549133 0.044000 Uiso calc U . R 1.000000 . .
C C52 0.4098(9) 0.8288(4) 0.6606(8) 0.037(3) Uani d . . . 1.000000 . .
H H52 0.413235 0.858712 0.665120 0.044000 Uiso calc U . R 1.000000 . .
C C53 0.4707(9) 0.8015(4) 0.7170(8) 0.037(3) Uani d . . . 1.000000 . .
C C54 0.5480(8) 0.8132(4) 0.7934(8) 0.035(3) Uani d . . . 1.000000 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
U1 O2 . 1.784(10) ?
U1 O1 . 1.790(10) ?
U1 O7 . 2.288(9) ?
U1 O11 . 2.320(9) ?
U1 O25 . 2.428(11) ?
U1 O9 4_676 2.437(9) ?
U1 O10 4_676 2.454(10) ?
U2 O3 . 1.753(9) ?
U2 O4 . 1.794(8) ?
U2 O15 4_565 2.435(8) ?
U2 O13 . 2.460(8) ?
U2 O16 4_565 2.474(8) ?
U2 O18B . 2.48(3) ?
U2 O14 . 2.501(8) ?
U2 O17 . 2.513(9) ?
U2 O18A . 2.55(3) ?
U3 O6 . 1.787(9) ?
U3 O5 . 1.787(8) ?
U3 O23 4_575 2.471(8) ?
U3 O24 4_575 2.479(8) ?
U3 O22 . 2.483(8) ?
U3 O21 . 2.485(9) ?
U3 O19 . 2.486(8) ?
U3 O20 . 2.506(10) ?
S1 C41 . 1.719(12) ?
S1 C38 . 1.744(12) ?
S2 C44B . 1.65(3) ?
S2 C47A . 1.69(4) ?
S2 C47B . 1.72(4) ?
S2 C44A . 1.78(4) ?
S3 C53 . 1.704(12) ?
S3 C50 . 1.731(13) ?
O7 C1 . 1.289(15) ?
O8 C1 . 1.224(15) ?
O9 C24 . 1.262(15) ?
O10 C24 . 1.252(16) ?
O11 C25 . 1.316(18) ?
O12 C25 . 1.217(18) ?
O13 C37 . 1.282(14) ?
O14 C37 . 1.277(14) ?
O15 C42 . 1.280(14) ?
O16 C42 . 1.267(14) ?
O17 C43 . 1.283(17) ?
O18A C43 . 1.26(4) ?
O18B C43 . 1.31(3) ?
O19 C48 . 1.253(16) ?
O20 C48 . 1.259(17) ?
O21 C49 . 1.280(15) ?
O22 C49 . 1.270(14) ?
O23 C54 . 1.269(14) ?
O24 C54 . 1.243(15) ?
O25 H25A . 0.839(10) ?
O25 H25B . 0.840(11) ?
O26 H26A . 0.951100 ?
O26 H26B . 0.936900 ?
O27 H27A . 0.840(10) ?
O27 H27B . 0.840(10) ?
N1 C4 . 1.316(15) ?
N1 C3 . 1.344(16) ?
N1 C7 . 1.517(15) ?
N2 C23 . 1.333(16) ?
N2 C19 . 1.340(17) ?
N2 C18 . 1.543(18) ?
N3 C27 . 1.344(17) ?
N3 C28 . 1.350(18) ?
N3 C31 . 1.492(18) ?
C1 C2 . 1.510(18) ?
C2 C3 . 1.364(18) ?
C2 C6 . 1.390(18) ?
C3 H3 . 0.950000 ?
C4 C5 . 1.389(17) ?
C4 H4 . 0.950000 ?
C5 C6 . 1.378(18) ?
C5 H5 . 0.950000 ?
C6 H6 . 0.950000 ?
C7 C8 . 1.527(19) ?
C7 H7A . 0.990000 ?
C7 H7B . 0.990000 ?
C8 C9 . 1.385(19) ?
C8 C13 . 1.418(18) ?
C9 C10 . 1.391(18) ?
C9 C14 . 1.537(18) ?
C10 C11 . 1.396(18) ?
C10 C15 . 1.538(17) ?
C11 C12 . 1.398(18) ?
C11 C18 . 1.531(18) ?
C12 C13 . 1.411(17) ?
C12 C16 . 1.519(17) ?
C13 C17 . 1.505(18) ?
C14 H14A . 0.958900 ?
C14 H14B . 0.958800 ?
C14 H14C . 0.961800 ?
C15 H15A . 0.980000 ?
C15 H15B . 0.980000 ?
C15 H15C . 0.980000 ?
C16 H16A . 0.980000 ?
C16 H16B . 0.980000 ?
C16 H16C . 0.980000 ?
C17 H17A . 0.980000 ?
C17 H17B . 0.980000 ?
C17 H17C . 0.980000 ?
C18 H18A . 0.990000 ?
C18 H18B . 0.990000 ?
C19 C20 . 1.408(19) ?
C19 H19 . 0.950000 ?
C20 C21 . 1.404(19) ?
C20 C24 . 1.476(18) ?
C21 C22 . 1.368(18) ?
C21 H21 . 0.950000 ?
C22 C23 . 1.374(17) ?
C22 H22 . 0.950000 ?
C23 H23 . 0.950000 ?
C25 C26 . 1.51(2) ?
C26 C30 . 1.38(2) ?
C26 C27 . 1.39(2) ?
C27 H27 . 0.950000 ?
C28 C29 . 1.379(19) ?
C28 H28 . 0.950000 ?
C29 C30 . 1.414(19) ?
C29 H29 . 0.950000 ?
C30 H30 . 0.950000 ?
C31 C32 . 1.528(18) ?
C31 H31A . 0.990000 ?
C31 H31B . 0.990000 ?
C32 C34 3_566 1.411(18) ?
C32 C33 . 1.419(18) ?
C33 C34 . 1.405(19) ?
C33 C35 . 1.498(18) ?
C34 C36 . 1.514(18) ?
C35 H35A . 0.980000 ?
C35 H35B . 0.980000 ?
C35 H35C . 0.980000 ?
C36 H36A . 0.980000 ?
C36 H36B . 0.980000 ?
C36 H36C . 0.980000 ?
C37 C38 . 1.465(17) ?
C38 C39 . 1.350(17) ?
C39 C40 . 1.427(17) ?
C39 H39 . 0.950000 ?
C40 C41 . 1.361(16) ?
C40 H40 . 0.950000 ?
C41 C42 . 1.481(16) ?
C43 C44A . 1.46(5) ?
C43 C44B . 1.52(3) ?
C44A C45A . 1.30(6) ?
C45A C46A . 1.32(5) ?
C45A H45A . 0.950000 ?
C46A C47A . 1.43(6) ?
C46A H46A . 0.950000 ?
C47A C48 . 1.53(5) ?
C44B C45B . 1.41(4) ?
C45B C46B . 1.37(3) ?
C45B H45B . 0.950000 ?
C46B C47B . 1.40(5) ?
C46B H46B . 0.950000 ?
C47B C48 . 1.46(5) ?
C49 C50 . 1.486(16) ?
C50 C51 . 1.350(17) ?
C51 C52 . 1.436(16) ?
C51 H51 . 0.950000 ?
C52 C53 . 1.390(17) ?
C52 H52 . 0.950000 ?
C53 C54 . 1.481(17) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 U1 O1 . . 178.5(5) ?
O2 U1 O7 . . 94.1(4) ?
O1 U1 O7 . . 84.8(4) ?
O2 U1 O11 . . 92.5(4) ?
O1 U1 O11 . . 86.4(4) ?
O7 U1 O11 . . 82.0(3) ?
O2 U1 O25 . . 93.6(5) ?
O1 U1 O25 . . 87.0(5) ?
O7 U1 O25 . . 154.4(4) ?
O11 U1 O25 . . 73.3(4) ?
O2 U1 O9 . 4_676 92.2(4) ?
O1 U1 O9 . 4_676 88.6(4) ?
O7 U1 O9 . 4_676 78.2(3) ?
O11 U1 O9 . 4_676 159.9(3) ?
O25 U1 O9 . 4_676 125.8(4) ?
O2 U1 O10 . 4_676 91.2(4) ?
O1 U1 O10 . 4_676 90.3(4) ?
O7 U1 O10 . 4_676 130.8(3) ?
O11 U1 O10 . 4_676 146.6(3) ?
O25 U1 O10 . 4_676 73.3(4) ?
O9 U1 O10 4_676 4_676 52.7(3) ?
O3 U2 O4 . . 178.6(4) ?
O3 U2 O15 . 4_565 91.3(4) ?
O4 U2 O15 . 4_565 88.4(3) ?
O3 U2 O13 . . 91.2(4) ?
O4 U2 O13 . . 90.2(4) ?
O15 U2 O13 4_565 . 121.3(3) ?
O3 U2 O16 . 4_565 89.1(4) ?
O4 U2 O16 . 4_565 89.6(4) ?
O15 U2 O16 4_565 4_565 53.4(3) ?
O13 U2 O16 . 4_565 174.7(3) ?
O3 U2 O18B . . 79.6(6) ?
O4 U2 O18B . . 100.5(6) ?
O15 U2 O18B 4_565 . 169.7(6) ?
O13 U2 O18B . . 64.2(6) ?
O16 U2 O18B 4_565 . 121.0(6) ?
O3 U2 O14 . . 91.1(4) ?
O4 U2 O14 . . 90.1(3) ?
O15 U2 O14 4_565 . 68.4(3) ?
O13 U2 O14 . . 52.9(3) ?
O16 U2 O14 4_565 . 121.8(3) ?
O18B U2 O14 . . 116.2(6) ?
O3 U2 O17 . . 88.3(4) ?
O4 U2 O17 . . 90.7(3) ?
O15 U2 O17 4_565 . 122.5(3) ?
O13 U2 O17 . . 116.2(3) ?
O16 U2 O17 4_565 . 69.1(3) ?
O18B U2 O17 . . 53.0(6) ?
O14 U2 O17 . . 169.2(3) ?
O3 U2 O18A . . 95.6(10) ?
O4 U2 O18A . . 84.5(10) ?
O15 U2 O18A 4_565 . 169.4(9) ?
O13 U2 O18A . . 66.7(8) ?
O16 U2 O18A 4_565 . 118.5(8) ?
O14 U2 O18A . . 119.4(8) ?
O17 U2 O18A . . 50.0(8) ?
O6 U3 O5 . . 179.4(4) ?
O6 U3 O23 . 4_575 87.5(3) ?
O5 U3 O23 . 4_575 92.8(4) ?
O6 U3 O24 . 4_575 90.3(4) ?
O5 U3 O24 . 4_575 89.6(4) ?
O23 U3 O24 4_575 4_575 52.5(3) ?
O6 U3 O22 . . 89.7(3) ?
O5 U3 O22 . . 90.9(3) ?
O23 U3 O22 4_575 . 67.6(3) ?
O24 U3 O22 4_575 . 120.0(3) ?
O6 U3 O21 . . 89.5(4) ?
O5 U3 O21 . . 90.8(4) ?
O23 U3 O21 4_575 . 120.4(3) ?
O24 U3 O21 4_575 . 172.9(3) ?
O22 U3 O21 . . 52.9(3) ?
O6 U3 O19 . . 87.4(3) ?
O5 U3 O19 . . 92.0(4) ?
O23 U3 O19 4_575 . 120.7(3) ?
O24 U3 O19 4_575 . 68.5(3) ?
O22 U3 O19 . . 171.0(3) ?
O21 U3 O19 . . 118.6(3) ?
O6 U3 O20 . . 91.5(5) ?
O5 U3 O20 . . 88.1(5) ?
O23 U3 O20 4_575 . 172.3(3) ?
O24 U3 O20 4_575 . 119.9(3) ?
O22 U3 O20 . . 120.1(3) ?
O21 U3 O20 . . 67.2(3) ?
O19 U3 O20 . . 51.6(3) ?
C41 S1 C38 . . 90.5(6) ?
C44B S2 C47B . . 92.9(19) ?
C47A S2 C44A . . 92.(2) ?
C53 S3 C50 . . 91.0(6) ?
C1 O7 U1 . . 164.8(9) ?
C24 O9 U1 . 4_575 94.1(8) ?
C24 O10 U1 . 4_575 93.6(8) ?
C25 O11 U1 . . 122.9(9) ?
C37 O13 U2 . . 94.4(7) ?
C37 O14 U2 . . 92.6(7) ?
C42 O15 U2 . 4_666 93.9(7) ?
C42 O16 U2 . 4_666 92.4(7) ?
C43 O17 U2 . . 93.5(8) ?
C43 O18A U2 . . 92.7(18) ?
C43 O18B U2 . . 94.2(14) ?
C48 O19 U3 . . 94.6(8) ?
C48 O20 U3 . . 93.5(8) ?
C49 O21 U3 . . 92.9(7) ?
C49 O22 U3 . . 93.2(7) ?
C54 O23 U3 . 4_676 93.1(7) ?
C54 O24 U3 . 4_676 93.3(7) ?
U1 O25 H25A . . 117.(10) ?
U1 O25 H25B . . 110.(10) ?
H25A O25 H25B . . 107.1(18) ?
H26A O26 H26B . . 93.500000 ?
H27A O27 H27B . . 106.8(18) ?
C4 N1 C3 . . 120.4(11) ?
C4 N1 C7 . . 121.1(11) ?
C3 N1 C7 . . 118.5(11) ?
C23 N2 C19 . . 121.7(12) ?
C23 N2 C18 . . 122.9(11) ?
C19 N2 C18 . . 115.4(11) ?
C27 N3 C28 . . 121.1(12) ?
C27 N3 C31 . . 116.8(11) ?
C28 N3 C31 . . 122.1(11) ?
O8 C1 O7 . . 126.5(12) ?
O8 C1 C2 . . 119.1(11) ?
O7 C1 C2 . . 114.3(11) ?
C3 C2 C6 . . 117.6(12) ?
C3 C2 C1 . . 121.2(11) ?
C6 C2 C1 . . 121.1(12) ?
N1 C3 C2 . . 122.1(12) ?
N1 C3 H3 . . 119.000000 ?
C2 C3 H3 . . 119.000000 ?
N1 C4 C5 . . 121.3(11) ?
N1 C4 H4 . . 119.400000 ?
C5 C4 H4 . . 119.400000 ?
C6 C5 C4 . . 118.2(11) ?
C6 C5 H5 . . 120.900000 ?
C4 C5 H5 . . 120.900000 ?
C5 C6 C2 . . 120.2(12) ?
C5 C6 H6 . . 119.900000 ?
C2 C6 H6 . . 119.900000 ?
N1 C7 C8 . . 113.4(11) ?
N1 C7 H7A . . 108.900000 ?
C8 C7 H7A . . 108.900000 ?
N1 C7 H7B . . 108.900000 ?
C8 C7 H7B . . 108.900000 ?
H7A C7 H7B . . 107.700000 ?
C9 C8 C13 . . 121.5(12) ?
C9 C8 C7 . . 122.6(13) ?
C13 C8 C7 . . 115.7(12) ?
C8 C9 C10 . . 120.7(12) ?
C8 C9 C14 . . 118.6(13) ?
C10 C9 C14 . . 120.7(13) ?
C9 C10 C11 . . 117.9(11) ?
C9 C10 C15 . . 119.7(12) ?
C11 C10 C15 . . 122.3(12) ?
C10 C11 C12 . . 123.0(11) ?
C10 C11 C18 . . 114.5(12) ?
C12 C11 C18 . . 122.3(13) ?
C11 C12 C13 . . 118.6(11) ?
C11 C12 C16 . . 121.2(12) ?
C13 C12 C16 . . 120.2(12) ?
C12 C13 C8 . . 118.2(11) ?
C12 C13 C17 . . 119.1(12) ?
C8 C13 C17 . . 122.6(12) ?
C9 C14 H14A . . 109.200000 ?
C9 C14 H14B . . 109.700000 ?
H14A C14 H14B . . 109.700000 ?
C9 C14 H14C . . 109.400000 ?
H14A C14 H14C . . 109.400000 ?
H14B C14 H14C . . 109.400000 ?
C10 C15 H15A . . 109.500000 ?
C10 C15 H15B . . 109.500000 ?
H15A C15 H15B . . 109.500000 ?
C10 C15 H15C . . 109.500000 ?
H15A C15 H15C . . 109.500000 ?
H15B C15 H15C . . 109.500000 ?
C12 C16 H16A . . 109.500000 ?
C12 C16 H16B . . 109.500000 ?
H16A C16 H16B . . 109.500000 ?
C12 C16 H16C . . 109.500000 ?
H16A C16 H16C . . 109.500000 ?
H16B C16 H16C . . 109.500000 ?
C13 C17 H17A . . 109.500000 ?
C13 C17 H17B . . 109.500000 ?
H17A C17 H17B . . 109.500000 ?
C13 C17 H17C . . 109.500000 ?
H17A C17 H17C . . 109.500000 ?
H17B C17 H17C . . 109.500000 ?
C11 C18 N2 . . 114.7(12) ?
C11 C18 H18A . . 108.600000 ?
N2 C18 H18A . . 108.600000 ?
C11 C18 H18B . . 108.600000 ?
N2 C18 H18B . . 108.600000 ?
H18A C18 H18B . . 107.600000 ?
N2 C19 C20 . . 119.9(12) ?
N2 C19 H19 . . 120.000000 ?
C20 C19 H19 . . 120.000000 ?
C21 C20 C19 . . 118.4(12) ?
C21 C20 C24 . . 122.3(12) ?
C19 C20 C24 . . 119.3(12) ?
C22 C21 C20 . . 118.7(12) ?
C22 C21 H21 . . 120.600000 ?
C20 C21 H21 . . 120.600000 ?
C21 C22 C23 . . 120.7(11) ?
C21 C22 H22 . . 119.700000 ?
C23 C22 H22 . . 119.700000 ?
N2 C23 C22 . . 120.4(11) ?
N2 C23 H23 . . 119.800000 ?
C22 C23 H23 . . 119.800000 ?
O10 C24 O9 . . 119.5(12) ?
O10 C24 C20 . . 120.8(12) ?
O9 C24 C20 . . 119.6(12) ?
O12 C25 O11 . . 125.1(14) ?
O12 C25 C26 . . 120.4(14) ?
O11 C25 C26 . . 114.3(13) ?
C30 C26 C27 . . 120.8(13) ?
C30 C26 C25 . . 120.9(13) ?
C27 C26 C25 . . 118.3(13) ?
N3 C27 C26 . . 120.1(13) ?
N3 C27 H27 . . 120.000000 ?
C26 C27 H27 . . 120.000000 ?
N3 C28 C29 . . 120.5(13) ?
N3 C28 H28 . . 119.700000 ?
C29 C28 H28 . . 119.700000 ?
C28 C29 C30 . . 119.9(14) ?
C28 C29 H29 . . 120.000000 ?
C30 C29 H29 . . 120.000000 ?
C26 C30 C29 . . 117.5(13) ?
C26 C30 H30 . . 121.200000 ?
C29 C30 H30 . . 121.200000 ?
N3 C31 C32 . . 114.4(11) ?
N3 C31 H31A . . 108.700000 ?
C32 C31 H31A . . 108.700000 ?
N3 C31 H31B . . 108.700000 ?
C32 C31 H31B . . 108.700000 ?
H31A C31 H31B . . 107.600000 ?
C34 C32 C33 3_566 . 121.5(11) ?
C34 C32 C31 3_566 . 119.6(12) ?
C33 C32 C31 . . 118.9(12) ?
C34 C33 C32 . . 119.9(12) ?
C34 C33 C35 . . 118.3(12) ?
C32 C33 C35 . . 121.7(13) ?
C33 C34 C32 . 3_566 118.7(11) ?
C33 C34 C36 . . 119.3(12) ?
C32 C34 C36 3_566 . 122.0(12) ?
C33 C35 H35A . . 109.500000 ?
C33 C35 H35B . . 109.500000 ?
H35A C35 H35B . . 109.500000 ?
C33 C35 H35C . . 109.500000 ?
H35A C35 H35C . . 109.500000 ?
H35B C35 H35C . . 109.500000 ?
C34 C36 H36A . . 109.500000 ?
C34 C36 H36B . . 109.500000 ?
H36A C36 H36B . . 109.500000 ?
C34 C36 H36C . . 109.500000 ?
H36A C36 H36C . . 109.500000 ?
H36B C36 H36C . . 109.500000 ?
O14 C37 O13 . . 119.6(11) ?
O14 C37 C38 . . 120.4(11) ?
O13 C37 C38 . . 120.0(11) ?
C39 C38 C37 . . 129.5(11) ?
C39 C38 S1 . . 111.9(9) ?
C37 C38 S1 . . 118.6(9) ?
C38 C39 C40 . . 112.8(11) ?
C38 C39 H39 . . 123.600000 ?
C40 C39 H39 . . 123.600000 ?
C41 C40 C39 . . 112.0(11) ?
C41 C40 H40 . . 124.000000 ?
C39 C40 H40 . . 124.000000 ?
C40 C41 C42 . . 128.0(11) ?
C40 C41 S1 . . 112.8(9) ?
C42 C41 S1 . . 119.2(9) ?
O16 C42 O15 . . 120.1(10) ?
O16 C42 C41 . . 120.6(11) ?
O15 C42 C41 . . 119.3(11) ?
O18A C43 O17 . . 115.(2) ?
O17 C43 O18B . . 119.0(16) ?
O18A C43 C44A . . 116.(2) ?
O17 C43 C44A . . 119.(2) ?
O17 C43 C44B . . 118.1(16) ?
O18B C43 C44B . . 116.(2) ?
C45A C44A C43 . . 138.(4) ?
C45A C44A S2 . . 106.(3) ?
C43 C44A S2 . . 115.(3) ?
C44A C45A C46A . . 121.(4) ?
C44A C45A H45A . . 119.500000 ?
C46A C45A H45A . . 119.500000 ?
C45A C46A C47A . . 111.(4) ?
C45A C46A H46A . . 124.700000 ?
C47A C46A H46A . . 124.700000 ?
C46A C47A C48 . . 133.(4) ?
C46A C47A S2 . . 109.(3) ?
C48 C47A S2 . . 117.(3) ?
C45B C44B C43 . . 126.(2) ?
C45B C44B S2 . . 114.(2) ?
C43 C44B S2 . . 120.(2) ?
C46B C45B C44B . . 109.(2) ?
C46B C45B H45B . . 125.400000 ?
C44B C45B H45B . . 125.400000 ?
C45B C46B C47B . . 116.(3) ?
C45B C46B H46B . . 122.200000 ?
C47B C46B H46B . . 122.200000 ?
C46B C47B C48 . . 131.(3) ?
C46B C47B S2 . . 108.(3) ?
C48 C47B S2 . . 120.(3) ?
O19 C48 O20 . . 119.7(12) ?
O19 C48 C47B . . 115.(2) ?
O20 C48 C47B . . 124.(2) ?
O19 C48 C47A . . 118.(2) ?
O20 C48 C47A . . 122.(2) ?
O19 C48 U3 . . 59.6(7) ?
O22 C49 O21 . . 120.3(11) ?
O22 C49 C50 . . 119.6(11) ?
O21 C49 C50 . . 120.0(11) ?
C51 C50 C49 . . 128.2(11) ?
C51 C50 S3 . . 113.5(9) ?
C49 C50 S3 . . 118.3(9) ?
C50 C51 C52 . . 111.1(11) ?
C50 C51 H51 . . 124.400000 ?
C52 C51 H51 . . 124.400000 ?
C53 C52 C51 . . 112.2(11) ?
C53 C52 H52 . . 123.900000 ?
C51 C52 H52 . . 123.900000 ?
C52 C53 C54 . . 127.1(11) ?
C52 C53 S3 . . 112.1(9) ?
C54 C53 S3 . . 120.8(9) ?
O24 C54 O23 . . 121.1(11) ?
O24 C54 C53 . . 120.0(11) ?
O23 C54 C53 . . 118.8(11) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O25 H25A O12 . 0.839(10) 2.26(15) 2.750(15) 118.(13) ?
O25 H25A O16 4_566 0.839(10) 2.58(12) 3.275(14) 141.(16) ?
O25 H25B O17 1_556 0.840(11) 2.07(16) 2.690(14) 130.(17) ?
O26 H26A O2 . 0.950000 2.160000 3.106(14) 171.000000 ?
O26 H26B O27 1_556 0.940000 1.830000 2.732(16) 160.400000 ?
O27 H27A O4 . 0.840(10) 2.15(7) 2.943(14) 158.(17) ?
O27 H27B O22 2_545 0.840(10) 2.03(7) 2.834(13) 160.(20) ?
C4 H4 S3 . 0.950000 2.800000 3.662(12) 151.800000 ?
C5 H5 O4 3_666 0.950000 2.570000 3.100(15) 115.400000 ?
C18 H18B O30 4_576 0.990000 2.450000 3.15(2) 127.700000 ?
C19 H19 O26 2_556 0.950000 2.220000 3.141(17) 163.600000 ?
C22 H22 O18A^a 2_556 0.950000 2.560000 3.18(4) 122.800000 ?
C23 H23 O13 2_556 0.950000 2.390000 3.148(15) 137.000000 ?
C27 H27 O7 . 0.950000 2.590000 3.495(17) 159.500000 ?
C28 H28 S2 3_566 0.950000 2.740000 3.434(14) 130.600000 ?
C28 H28 O19 3_566 0.950000 2.310000 2.944(17) 123.700000 ?
C39 H39 O29 2_545 0.950000 2.600000 3.439(17) 148.100000 ?
C40 H40 O12 4_665 0.950000 2.330000 3.236(16) 159.600000 ?




####################################################################### 
# 
# 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 2202988'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2022-08-23 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H35 N2 O19.50 S2 U2'
_chemical_formula_iupac          ?
_chemical_formula_weight         1371.86

_chemical_melting_point          ?

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

_cell_length_a                   9.6207(7)
_cell_length_b                   11.1875(6)
_cell_length_c                   19.8035(17)
_cell_angle_alpha                90
_cell_angle_beta                 92.098(3)
_cell_angle_gamma                90
_cell_volume                     2130.1(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9737
_cell_measurement_theta_min      2.3221
_cell_measurement_theta_max      33.0812
_cell_measurement_temperature    100(2)

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent pale yellow'
_exptl_crystal_size_max          0.082
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.039
_exptl_crystal_density_diffrn    2.139
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1298

_exptl_absorpt_coefficient_mu    7.774
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_T_max  0.75

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100(2)

_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms 70 W'
_diffrn_source_current           1.4
_diffrn_source_voltage           50

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'multilayer mirror optics'

_diffrn_measurement_device       'Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_detector_area_resol_mean 7.41

_diffrn_reflns_number            88765
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_full        30.50
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28

_refine_special_details          
;
The water molecule (O10) has been given an occupancy
parameter of 0.75 in order to retain an acceptable
displacement parameter. Its H atoms were found and
were treated as riding atoms with an isotropic 
displacement parameter equal to 1.5 times that of O10.
;

_reflns_number_total             6484
_reflns_number_gt                5910
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0173
_refine_ls_wR_factor_gt          0.0362
_refine_ls_wR_factor_ref         0.0376
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_refine_ls_number_reflns         6484
_refine_ls_number_parameters     291
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0126P)²+2.8659P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.161
_refine_diff_density_min         -0.719
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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

_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1328)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U U1 0.21519(2) 0.61371(2) 0.21218(2) 0.00990(2) Uani d . . . 1 . .
S S1 0.57293(5) 0.21594(4) 0.40143(3) 0.01268(10) Uani d . . . 1 . .
O O1 0.09981(17) 0.59599(15) 0.27880(9) 0.0197(3) Uani d . . . 1 . .
O O2 0.33055(17) 0.63082(14) 0.14502(8) 0.0183(3) Uani d . . . 1 . .
O O3 0.35346(18) 0.73179(14) 0.28705(9) 0.0208(4) Uani d . . . 1 . .
O O4 0.33975(17) 0.91871(13) 0.32544(9) 0.0179(3) Uani d . . . 1 . .
O O5 0.39293(16) 0.49373(13) 0.26407(8) 0.0165(3) Uani d . . . 1 . .
O O6 0.35145(16) 0.31312(13) 0.30400(8) 0.0166(3) Uani d . . . 1 . .
O O7 0.48382(18) 0.12729(13) 0.36442(9) 0.0214(4) Uani d . . . 1 . .
O O8 0.68021(17) 0.15323(15) 0.44046(8) 0.0184(3) Uani d . . . 1 . .
O O9 0.49410(17) 0.30055(15) 0.43922(8) 0.0190(3) Uani d . . . 1 . .
O O10 0.9220(4) 0.0051(3) 0.43793(19) 0.0584(10) Uani d . P . 0.75 . .
H H10A 0.868755 0.064411 0.440202 0.088000 Uiso d U P R 0.75 . .
H H10B 0.973885 0.031421 0.408112 0.088000 Uiso d U P R 0.75 . .
N N1 0.72272(18) 0.73575(16) 0.46479(9) 0.0120(3) Uani d . . . 1 . .
C C1 0.3905(2) 0.81606(18) 0.32481(11) 0.0133(4) Uani d . . . 1 . .
C C2 0.5100(2) 0.78901(18) 0.37457(11) 0.0122(4) Uani d . . . 1 . .
C C3 0.5723(2) 0.67760(19) 0.37384(12) 0.0181(4) Uani d . . . 1 . .
H H3 0.541736 0.618891 0.341970 0.022000 Uiso calc U . R 1 . .
C C4 0.6793(2) 0.6528(2) 0.41995(12) 0.0185(4) Uani d . . . 1 . .
H H4 0.722543 0.576493 0.419931 0.022000 Uiso calc U . R 1 . .
C C5 0.6642(2) 0.84444(19) 0.46574(11) 0.0150(4) Uani d . . . 1 . .
H H5 0.697215 0.902044 0.497713 0.018000 Uiso calc U . R 1 . .
C C6 0.5567(2) 0.87355(18) 0.42088(11) 0.0157(4) Uani d . . . 1 . .
H H6 0.515351 0.950613 0.421782 0.019000 Uiso calc U . R 1 . .
C C7 0.8276(2) 0.7067(2) 0.52020(11) 0.0162(4) Uani d . . . 1 . .
H H7A 0.778126 0.694533 0.562632 0.019000 Uiso calc U . R 1 . .
H H7B 0.890293 0.776187 0.526988 0.019000 Uiso calc U . R 1 . .
C C8 0.9142(2) 0.59785(19) 0.50719(11) 0.0143(4) Uani d . . . 1 . .
C C9 0.8725(2) 0.4868(2) 0.53261(11) 0.0143(4) Uani d . . . 1 . .
C C10 1.0388(2) 0.61197(19) 0.47336(11) 0.0143(4) Uani d . . . 1 . .
C C11 0.7328(2) 0.4687(2) 0.56395(12) 0.0203(5) Uani d . . . 1 . .
H H11A 0.746281 0.458745 0.612924 0.030000 Uiso calc U . R 1 . .
H H11B 0.688066 0.397065 0.544676 0.030000 Uiso calc U . R 1 . .
H H11C 0.673623 0.538441 0.554543 0.030000 Uiso calc U . R 1 . .
C C12 1.0788(2) 0.7298(2) 0.44188(12) 0.0195(5) Uani d . . . 1 . .
H H12A 1.151929 0.767966 0.470047 0.029000 Uiso calc U . R 1 . .
H H12B 0.997201 0.782167 0.438602 0.029000 Uiso calc U . R 1 . .
H H12C 1.113100 0.715387 0.396605 0.029000 Uiso calc U . R 1 . .
C C13 0.4332(2) 0.39381(18) 0.28643(11) 0.0128(4) Uani d . . . 1 . .
C C14 0.5891(2) 0.37667(19) 0.29240(11) 0.0143(4) Uani d . . . 1 . .
C C15 0.6589(2) 0.30068(19) 0.33904(11) 0.0142(4) Uani d . . . 1 . .
C C16 0.8042(2) 0.2992(2) 0.34275(13) 0.0229(5) Uani d . . . 1 . .
H H16 0.851283 0.248705 0.374675 0.028000 Uiso calc U . R 1 . .
C C17 0.8806(3) 0.3703(3) 0.30047(15) 0.0293(6) Uani d . . . 1 . .
H H17 0.979335 0.368870 0.303678 0.035000 Uiso calc U . R 1 . .
C C18 0.8129(3) 0.4433(3) 0.25364(14) 0.0284(6) Uani d . . . 1 . .
H H18 0.865093 0.491459 0.224248 0.034000 Uiso calc U . R 1 . .
C C19 0.6684(3) 0.4464(2) 0.24949(12) 0.0211(5) Uani d . . . 1 . .
H H19 0.622757 0.496711 0.217008 0.025000 Uiso calc U . R 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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
U1 O1 . 1.7660(17) ?
U1 O2 . 1.7736(17) ?
U1 O6 2 2.3400(15) ?
U1 O4 2_545 2.3590(15) ?
U1 O3 . 2.3597(15) ?
U1 O5 . 2.3775(15) ?
U1 O7 2 2.4036(16) ?
S1 O9 . 1.4397(17) ?
S1 O8 . 1.4479(16) ?
S1 O7 . 1.4865(16) ?
S1 C15 . 1.785(2) ?
O3 C1 . 1.247(3) ?
O4 C1 . 1.248(3) ?
O5 C13 . 1.258(2) ?
O6 C13 . 1.255(3) ?
O10 H10A . 0.840400 ?
O10 H10B . 0.840700 ?
N1 C4 . 1.340(3) ?
N1 C5 . 1.340(3) ?
N1 C7 . 1.499(3) ?
C1 C2 . 1.517(3) ?
C2 C6 . 1.381(3) ?
C2 C3 . 1.383(3) ?
C3 C4 . 1.379(3) ?
C3 H3 . 0.950000 ?
C4 H4 . 0.950000 ?
C5 C6 . 1.377(3) ?
C5 H5 . 0.950000 ?
C6 H6 . 0.950000 ?
C7 C8 . 1.503(3) ?
C7 H7A . 0.990000 ?
C7 H7B . 0.990000 ?
C8 C10 . 1.404(3) ?
C8 C9 . 1.404(3) ?
C9 C10 3_766 1.404(3) ?
C9 C11 . 1.515(3) ?
C10 C12 . 1.513(3) ?
C11 H11A . 0.980000 ?
C11 H11B . 0.980000 ?
C11 H11C . 0.980000 ?
C12 H12A . 0.980000 ?
C12 H12B . 0.980000 ?
C12 H12C . 0.980000 ?
C13 C14 . 1.512(3) ?
C14 C19 . 1.401(3) ?
C14 C15 . 1.408(3) ?
C15 C16 . 1.398(3) ?
C16 C17 . 1.385(4) ?
C16 H16 . 0.950000 ?
C17 C18 . 1.381(4) ?
C17 H17 . 0.950000 ?
C18 C19 . 1.389(3) ?
C18 H18 . 0.950000 ?
C19 H19 . 0.950000 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 U1 O2 . . 179.66(8) ?
O1 U1 O6 . 2 91.88(7) ?
O2 U1 O6 . 2 88.29(7) ?
O1 U1 O4 . 2_545 89.57(7) ?
O2 U1 O4 . 2_545 90.12(7) ?
O6 U1 O4 2 2_545 141.38(5) ?
O1 U1 O3 . . 87.07(7) ?
O2 U1 O3 . . 93.26(7) ?
O6 U1 O3 2 . 72.40(5) ?
O4 U1 O3 2_545 . 146.18(5) ?
O1 U1 O5 . . 94.34(7) ?
O2 U1 O5 . . 85.71(7) ?
O6 U1 O5 2 . 141.86(5) ?
O4 U1 O5 2_545 . 76.33(5) ?
O3 U1 O5 . . 70.40(5) ?
O1 U1 O7 . 2 88.31(7) ?
O2 U1 O7 . 2 91.47(7) ?
O6 U1 O7 2 2 69.23(5) ?
O4 U1 O7 2_545 2 72.24(5) ?
O3 U1 O7 . 2 141.15(5) ?
O5 U1 O7 . 2 148.44(5) ?
O9 S1 O8 . . 114.82(10) ?
O9 S1 O7 . . 112.94(10) ?
O8 S1 O7 . . 109.08(9) ?
O9 S1 C15 . . 106.08(10) ?
O8 S1 C15 . . 106.72(10) ?
O7 S1 C15 . . 106.65(10) ?
C1 O3 U1 . . 160.38(15) ?
C1 O4 U1 . 2 158.58(16) ?
C13 O5 U1 . . 149.43(14) ?
C13 O6 U1 . 2_545 145.01(15) ?
S1 O7 U1 . 2_545 141.73(9) ?
H10A O10 H10B . . 98.000000 ?
C4 N1 C5 . . 121.08(18) ?
C4 N1 C7 . . 121.36(18) ?
C5 N1 C7 . . 117.26(17) ?
O3 C1 O4 . . 126.8(2) ?
O3 C1 C2 . . 115.57(18) ?
O4 C1 C2 . . 117.67(18) ?
C6 C2 C3 . . 119.56(19) ?
C6 C2 C1 . . 121.01(18) ?
C3 C2 C1 . . 119.42(18) ?
C4 C3 C2 . . 119.2(2) ?
C4 C3 H3 . . 120.400000 ?
C2 C3 H3 . . 120.400000 ?
N1 C4 C3 . . 120.4(2) ?
N1 C4 H4 . . 119.800000 ?
C3 C4 H4 . . 119.800000 ?
N1 C5 C6 . . 120.75(19) ?
N1 C5 H5 . . 119.600000 ?
C6 C5 H5 . . 119.600000 ?
C5 C6 C2 . . 119.00(19) ?
C5 C6 H6 . . 120.500000 ?
C2 C6 H6 . . 120.500000 ?
N1 C7 C8 . . 114.35(17) ?
N1 C7 H7A . . 108.700000 ?
C8 C7 H7A . . 108.700000 ?
N1 C7 H7B . . 108.700000 ?
C8 C7 H7B . . 108.700000 ?
H7A C7 H7B . . 107.600000 ?
C10 C8 C9 . . 122.04(19) ?
C10 C8 C7 . . 118.6(2) ?
C9 C8 C7 . . 119.2(2) ?
C10 C9 C8 3_766 . 118.9(2) ?
C10 C9 C11 3_766 . 118.7(2) ?
C8 C9 C11 . . 122.31(19) ?
C9 C10 C8 3_766 . 119.0(2) ?
C9 C10 C12 3_766 . 119.1(2) ?
C8 C10 C12 . . 121.93(19) ?
C9 C11 H11A . . 109.500000 ?
C9 C11 H11B . . 109.500000 ?
H11A C11 H11B . . 109.500000 ?
C9 C11 H11C . . 109.500000 ?
H11A C11 H11C . . 109.500000 ?
H11B C11 H11C . . 109.500000 ?
C10 C12 H12A . . 109.500000 ?
C10 C12 H12B . . 109.500000 ?
H12A C12 H12B . . 109.500000 ?
C10 C12 H12C . . 109.500000 ?
H12A C12 H12C . . 109.500000 ?
H12B C12 H12C . . 109.500000 ?
O6 C13 O5 . . 123.3(2) ?
O6 C13 C14 . . 121.13(19) ?
O5 C13 C14 . . 115.59(19) ?
C19 C14 C15 . . 118.5(2) ?
C19 C14 C13 . . 116.29(19) ?
C15 C14 C13 . . 125.2(2) ?
C16 C15 C14 . . 119.6(2) ?
C16 C15 S1 . . 116.45(17) ?
C14 C15 S1 . . 123.57(17) ?
C17 C16 C15 . . 120.9(2) ?
C17 C16 H16 . . 119.600000 ?
C15 C16 H16 . . 119.600000 ?
C18 C17 C16 . . 119.9(2) ?
C18 C17 H17 . . 120.100000 ?
C16 C17 H17 . . 120.100000 ?
C17 C18 C19 . . 120.0(2) ?
C17 C18 H18 . . 120.000000 ?
C19 C18 H18 . . 120.000000 ?
C18 C19 C14 . . 121.1(2) ?
C18 C19 H19 . . 119.500000 ?
C14 C19 H19 . . 119.500000 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O10 H10A O8 . 0.84 2.07 2.858(3) 156.3 ?
O10 H10B O2 2_645 0.84 2.46 3.261(4) 160.8 ?
C3 H3 O5 . 0.95 2.50 3.415(3) 162.8 ?
C6 H6 O7 1_565 0.95 2.29 3.121(3) 145.1 ?
C7 H7A O2 4_676 0.99 2.58 3.067(3) 110.1 ?


