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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1958810'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2019-10-11 deposited with the CCDC.	2019-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H8 O6 U'
_chemical_formula_weight         510.23

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

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

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

_cell_length_a                   9.3038(10)
_cell_length_b                   9.3958(8)
_cell_length_c                   9.9840(15)
_cell_angle_alpha                92.354(7)
_cell_angle_beta                 116.196(5)
_cell_angle_gamma                111.110(6)
_cell_volume                     709.40(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    32551
_cell_measurement_theta_min      3.73
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.389
_exptl_crystal_F_000             464
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    11.464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.303
_exptl_absorpt_correction_T_max  0.632
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and ten ω scans with 2° steps (734 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            32551
_diffrn_reflns_av_unetI/netI     0.1059
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.728
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2687
_reflns_number_gt                2207
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms were introduced at calculated
 positions and were treated as riding atoms with an isotropic displacement
 parameter equal to 1.2 times that of the parent atom.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2687
_refine_ls_number_parameters     190
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0529
_refine_ls_wR_factor_gt          0.0494
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_restrained_S_all      0.916
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.52224(3) 1.22322(3) 0.95942(2) 0.02171(9) Uani 1 1 d . . . . .
O1 O 0.2961(5) 1.1632(5) 0.8955(4) 0.0220(11) Uani 1 1 d . . . . .
O2 O 0.7496(5) 1.2802(5) 1.0286(4) 0.0218(11) Uani 1 1 d . . . . .
O3 O 0.4169(5) 1.0895(5) 0.6961(4) 0.0265(11) Uani 1 1 d . . . . .
O4 O 0.4694(5) 0.9443(5) 0.8614(4) 0.0235(11) Uani 1 1 d . . . . .
O5 O 0.4194(5) 0.5780(5) 0.8546(4) 0.0234(11) Uani 1 1 d . . . . .
O6 O 0.5449(5) 0.4235(5) 0.8288(4) 0.0258(11) Uani 1 1 d . . . . .
C1 C 0.3010(7) 0.8128(7) 0.5924(6) 0.0186(14) Uani 1 1 d . . . . .
C2 C 0.3809(8) 0.7169(8) 0.5828(6) 0.0216(15) Uani 1 1 d . . . . .
C3 C 0.2793(8) 0.5792(8) 0.4654(6) 0.0277(17) Uani 1 1 d . . . . .
H3 H 0.3323 0.5125 0.4560 0.033 Uiso 1 1 calc R U . . .
C4 C 0.1013(9) 0.5378(8) 0.3618(7) 0.0297(17) Uani 1 1 d . . . . .
H4 H 0.0321 0.4419 0.2851 0.036 Uiso 1 1 calc R U . . .
C5 C 0.0272(8) 0.6402(8) 0.3733(7) 0.0286(18) Uani 1 1 d . . . . .
H5 H -0.0921 0.6161 0.3010 0.034 Uiso 1 1 calc R U . . .
C6 C 0.1254(8) 0.7752(8) 0.4881(6) 0.0236(15) Uani 1 1 d . . . . .
H6 H 0.0734 0.8432 0.4964 0.028 Uiso 1 1 calc R U . . .
C7 C 0.5750(8) 0.7654(8) 0.6819(6) 0.0218(15) Uani 1 1 d . . . . .
C8 C 0.6425(8) 0.6777(7) 0.7813(6) 0.0205(15) Uani 1 1 d . . . . .
C9 C 0.8228(8) 0.7158(8) 0.8606(6) 0.0254(16) Uani 1 1 d . . . . .
H9 H 0.8652 0.6508 0.9227 0.030 Uiso 1 1 calc R U . . .
C10 C 0.9393(8) 0.8483(8) 0.8482(7) 0.0282(17) Uani 1 1 d . . . . .
H10 H 1.0629 0.8776 0.9047 0.034 Uiso 1 1 calc R U . . .
C11 C 0.8735(8) 0.9393(8) 0.7514(6) 0.0258(17) Uani 1 1 d . . . . .
H11 H 0.9529 1.0311 0.7427 0.031 Uiso 1 1 calc R U . . .
C12 C 0.6935(8) 0.8963(7) 0.6685(6) 0.0229(16) Uani 1 1 d . . . . .
H12 H 0.6507 0.9576 0.6013 0.027 Uiso 1 1 calc R U . . .
C13 C 0.4021(7) 0.9583(8) 0.7207(7) 0.0233(16) Uani 1 1 d . . . . .
C14 C 0.5273(8) 0.5494(8) 0.8239(6) 0.0220(15) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.756(4) . ?
U1 O2 1.761(4) . ?
U1 O5 2.307(4) 2_677 ?
U1 O6 2.334(4) 1_565 ?
U1 O4 2.425(4) 2_677 ?
U1 O3 2.453(4) . ?
U1 O4 2.550(5) . ?
O3 C13 1.237(8) . ?
O4 C13 1.296(6) . ?
O4 U1 2.425(4) 2_677 ?
O5 C14 1.279(7) . ?
O5 U1 2.307(4) 2_677 ?
O6 C14 1.251(8) . ?
O6 U1 2.334(4) 1_545 ?
C1 C2 1.383(9) . ?
C1 C6 1.389(8) . ?
C1 C13 1.503(8) . ?
C2 C3 1.399(9) . ?
C2 C7 1.497(8) . ?
C3 C4 1.398(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.397(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.371(9) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.383(8) . ?
C7 C8 1.396(8) . ?
C8 C9 1.393(8) . ?
C8 C14 1.515(8) . ?
C9 C10 1.378(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.401(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.383(8) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 178.06(17) . . ?
O1 U1 O5 88.39(17) . 2_677 ?
O2 U1 O5 91.27(16) . 2_677 ?
O1 U1 O6 94.72(17) . 1_565 ?
O2 U1 O6 87.11(17) . 1_565 ?
O5 U1 O6 81.53(15) 2_677 1_565 ?
O1 U1 O4 88.79(16) . 2_677 ?
O2 U1 O4 89.29(16) . 2_677 ?
O5 U1 O4 88.25(14) 2_677 2_677 ?
O6 U1 O4 169.08(14) 1_565 2_677 ?
O1 U1 O3 83.54(16) . . ?
O2 U1 O3 97.54(15) . . ?
O5 U1 O3 154.87(16) 2_677 . ?
O6 U1 O3 75.50(15) 1_565 . ?
O4 U1 O3 115.22(15) 2_677 . ?
O1 U1 O4 91.11(17) . . ?
O2 U1 O4 88.31(17) . . ?
O5 U1 O4 152.56(13) 2_677 . ?
O6 U1 O4 125.82(13) 1_565 . ?
O4 U1 O4 64.31(14) 2_677 . ?
O3 U1 O4 51.74(13) . . ?
C13 O3 U1 97.0(4) . . ?
C13 O4 U1 148.7(4) . 2_677 ?
C13 O4 U1 90.9(4) . . ?
U1 O4 U1 115.69(14) 2_677 . ?
C14 O5 U1 129.0(4) . 2_677 ?
C14 O6 U1 140.5(4) . 1_545 ?
C2 C1 C6 121.3(6) . . ?
C2 C1 C13 120.2(5) . . ?
C6 C1 C13 118.5(6) . . ?
C1 C2 C3 118.1(6) . . ?
C1 C2 C7 121.8(6) . . ?
C3 C2 C7 119.7(6) . . ?
C4 C3 C2 121.2(7) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C5 C4 C3 118.7(6) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
C6 C5 C4 120.5(6) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C1 120.1(7) . . ?
C5 C6 H6 120.0 . . ?
C1 C6 H6 120.0 . . ?
C12 C7 C8 118.0(6) . . ?
C12 C7 C2 119.4(6) . . ?
C8 C7 C2 122.5(5) . . ?
C9 C8 C7 121.5(6) . . ?
C9 C8 C14 116.3(6) . . ?
C7 C8 C14 121.7(5) . . ?
C10 C9 C8 119.7(6) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C9 C10 C11 119.2(6) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
C12 C11 C10 120.5(6) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C7 121.0(6) . . ?
C11 C12 H12 119.5 . . ?
C7 C12 H12 119.5 . . ?
O3 C13 O4 119.2(6) . . ?
O3 C13 C1 122.1(5) . . ?
O4 C13 C1 118.6(6) . . ?
O6 C14 O5 124.1(6) . . ?
O6 C14 C8 118.4(6) . . ?
O5 C14 C8 117.5(6) . . ?

_refine_diff_density_max         2.095
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.279

_shelxl_version_number           2014-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6
_database_code_depnum_ccdc_archive 'CCDC 1958815'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2019-10-11 deposited with the CCDC.	2019-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H56 N4 Ni O12 U'
_chemical_formula_weight         1129.66

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

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

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

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

_cell_length_a                   9.6239(8)
_cell_length_b                   11.7355(7)
_cell_length_c                   12.0230(10)
_cell_angle_alpha                61.358(4)
_cell_angle_beta                 67.648(4)
_cell_angle_gamma                80.938(5)
_cell_volume                     1101.68(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    59752
_cell_measurement_theta_min      3.07
_cell_measurement_theta_max      25.68

_exptl_crystal_description       irregular
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_F_000             564
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    4.165
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.470
_exptl_absorpt_correction_T_max  0.558
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'2 φ and 12 ω scans with 2° steps (701 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            59752
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.072
_diffrn_reflns_theta_max         25.677
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4172
_reflns_number_gt                3981
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms bound to O and N atoms were found
 on a difference Fourier map and were refined with restraints on bond
 lengths and with an isotropic displacement parameter equal to 1.2 (NH)
 or 1.5 (H2O) times that of the parent atom. The C-bound H atoms 
 were introduced at calculated positions and were treated as riding
 atoms with an isotropic displacement parameter equal to 1.2 times that
 of the parent atom (1.5 for CH₃, with optimized geometry).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0146P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4172
_refine_ls_number_parameters     298
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0306
_refine_ls_wR_factor_ref         0.0589
_refine_ls_wR_factor_gt          0.0581
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.500000 0.500000 0.500000 0.02247(7) Uani 1 2 d S . P . .
Ni1 Ni 0.500000 0.000000 0.500000 0.01948(16) Uani 1 2 d S . P . .
O1 O 0.6972(2) 0.5159(3) 0.4509(2) 0.0226(6) Uani 1 1 d . . . . .
O2 O 0.4924(2) 0.7129(3) 0.3455(2) 0.0218(6) Uani 1 1 d . . . . .
O3 O 0.3141(3) 0.8602(3) 0.3307(3) 0.0295(7) Uani 1 1 d . . . . .
O4 O 0.5375(2) 0.4441(3) 0.3316(2) 0.0216(6) Uani 1 1 d . . . . .
O5 O 0.7199(3) 0.3651(3) 0.2096(3) 0.0293(7) Uani 1 1 d . . . . .
O6 O 0.6694(3) 0.1368(3) 0.4425(3) 0.0240(6) Uani 1 1 d D . . . .
H6A H 0.674(4) 0.145(4) 0.506(3) 0.036 Uiso 1 1 d D U . . .
H6B H 0.683(4) 0.205(5) 0.373(4) 0.036 Uiso 1 1 d . U . . .
N1 N 0.5997(3) -0.0073(4) 0.3182(3) 0.0223(7) Uani 1 1 d D . . . .
H1 H 0.547(3) -0.075(3) 0.325(4) 0.027 Uiso 1 1 d D U . . .
N2 N 0.3854(3) 0.1593(4) 0.3969(3) 0.0220(7) Uani 1 1 d D . . . .
H2 H 0.444(3) 0.231(2) 0.377(3) 0.026 Uiso 1 1 d D U . . .
C1 C 0.3360(3) 0.7249(4) 0.2275(4) 0.0239(9) Uani 1 1 d . . . . .
C2 C 0.4377(3) 0.6795(4) 0.1386(3) 0.0205(8) Uani 1 1 d . . . . .
C3 C 0.3796(4) 0.6263(4) 0.0834(4) 0.0241(9) Uani 1 1 d . . . . .
H3 H 0.447090 0.592826 0.025212 0.029 Uiso 1 1 calc R U . . .
C4 C 0.2271(4) 0.6203(4) 0.1100(4) 0.0255(9) Uani 1 1 d . . . . .
H4 H 0.190837 0.584715 0.069514 0.031 Uiso 1 1 calc R U . . .
C5 C 0.1278(4) 0.6670(5) 0.1969(4) 0.0290(10) Uani 1 1 d . . . . .
H5 H 0.022643 0.662388 0.217453 0.035 Uiso 1 1 calc R U . . .
C6 C 0.1824(4) 0.7203(5) 0.2534(4) 0.0293(10) Uani 1 1 d . . . . .
H6 H 0.114207 0.754331 0.310721 0.035 Uiso 1 1 calc R U . . .
C7 C 0.6045(4) 0.6982(4) 0.0878(3) 0.0209(8) Uani 1 1 d . . . . .
C8 C 0.7024(3) 0.5944(4) 0.1181(4) 0.0223(9) Uani 1 1 d . . . . .
C9 C 0.8580(4) 0.6190(5) 0.0476(4) 0.0287(10) Uani 1 1 d . . . . .
H9 H 0.924576 0.549003 0.066311 0.034 Uiso 1 1 calc R U . . .
C10 C 0.9162(4) 0.7423(4) -0.0479(4) 0.0272(9) Uani 1 1 d . . . . .
H10 H 1.021662 0.756956 -0.093957 0.033 Uiso 1 1 calc R U . . .
C11 C 0.8194(4) 0.8453(5) -0.0763(4) 0.0285(10) Uani 1 1 d . . . . .
H11 H 0.858195 0.930637 -0.142320 0.034 Uiso 1 1 calc R U . . .
C12 C 0.6653(4) 0.8223(5) -0.0073(4) 0.0247(9) Uani 1 1 d . . . . .
H12 H 0.599857 0.893295 -0.025601 0.030 Uiso 1 1 calc R U . . .
C13 C 0.3822(4) 0.7721(4) 0.3050(4) 0.0242(9) Uani 1 1 d . . . . .
C14 C 0.6523(4) 0.4593(4) 0.2234(4) 0.0219(9) Uani 1 1 d . . . . .
C15 C 0.5693(3) 0.1163(4) 0.2160(4) 0.0265(9) Uani 1 1 d . . . . .
H15A H 0.584495 0.108435 0.133793 0.032 Uiso 1 1 calc R U . . .
H15B H 0.640168 0.184469 0.190837 0.032 Uiso 1 1 calc R U . . .
C16 C 0.4077(3) 0.1549(4) 0.2707(4) 0.0250(9) Uani 1 1 d . . . . .
H16A H 0.389305 0.241099 0.203097 0.030 Uiso 1 1 calc R U . . .
H16B H 0.336125 0.090752 0.288808 0.030 Uiso 1 1 calc R U . . .
C17 C 0.2277(3) 0.1908(4) 0.4678(4) 0.0233(9) Uani 1 1 d . . . . .
C18 C 0.2256(3) 0.1771(4) 0.6021(4) 0.0229(9) Uani 1 1 d . . . . .
H18A H 0.308660 0.232996 0.580412 0.028 Uiso 1 1 calc R U . . .
H18B H 0.130665 0.213575 0.640932 0.028 Uiso 1 1 calc R U . . .
C19 C 0.2390(3) 0.0435(4) 0.7128(4) 0.0253(9) Uani 1 1 d . . . . .
H19 H 0.181006 -0.021213 0.714328 0.030 Uiso 1 1 calc R U . . .
C20 C 0.1096(4) 0.1015(4) 0.4908(4) 0.0275(10) Uani 1 1 d . . . . .
H20A H 0.104461 0.121107 0.403526 0.041 Uiso 1 1 calc R U . . .
H20B H 0.011461 0.115105 0.548540 0.041 Uiso 1 1 calc R U . . .
H20C H 0.137140 0.010860 0.535010 0.041 Uiso 1 1 calc R U . . .
C21 C 0.1941(4) 0.3301(4) 0.3830(4) 0.0284(9) Uani 1 1 d . . . . .
H21A H 0.269926 0.388781 0.366171 0.043 Uiso 1 1 calc R U . . .
H21B H 0.094327 0.351092 0.431656 0.043 Uiso 1 1 calc R U . . .
H21C H 0.196196 0.340383 0.296555 0.043 Uiso 1 1 calc R U . . .
C22 C 0.1722(4) 0.0430(5) 0.8506(4) 0.0347(11) Uani 1 1 d . . . . .
H22A H 0.180931 -0.043476 0.921283 0.052 Uiso 1 1 calc R U . . .
H22B H 0.065976 0.065020 0.868726 0.052 Uiso 1 1 calc R U . . .
H22C H 0.226860 0.107185 0.849916 0.052 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.772(2) 2_666 ?
U1 O1 1.772(2) . ?
U1 O2 2.301(3) 2_666 ?
U1 O2 2.301(3) . ?
U1 O4 2.303(2) 2_666 ?
U1 O4 2.303(2) . ?
Ni1 N1 2.065(3) 2_656 ?
Ni1 N1 2.065(3) . ?
Ni1 N2 2.102(3) . ?
Ni1 N2 2.102(3) 2_656 ?
Ni1 O6 2.149(3) 2_656 ?
Ni1 O6 2.149(3) . ?
O2 C13 1.297(4) . ?
O3 C13 1.238(4) . ?
O4 C14 1.300(4) . ?
O5 C14 1.241(4) . ?
O6 H6A 0.835(10) . ?
O6 H6B 0.82(5) . ?
N1 C15 1.459(5) . ?
N1 C19 1.495(4) 2_656 ?
N1 H1 0.964(10) . ?
N2 C16 1.475(4) . ?
N2 C17 1.520(4) . ?
N2 H2 0.962(10) . ?
C1 C6 1.394(4) . ?
C1 C2 1.403(4) . ?
C1 C13 1.503(5) . ?
C2 C3 1.391(5) . ?
C2 C7 1.494(4) . ?
C3 C4 1.384(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.391(6) . ?
C7 C8 1.407(5) . ?
C8 C9 1.408(5) . ?
C8 C14 1.483(6) . ?
C9 C10 1.378(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.392(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.392(5) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C15 C16 1.531(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C21 1.517(6) . ?
C17 C20 1.525(5) . ?
C17 C18 1.537(5) . ?
C18 C19 1.521(6) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C22 1.529(4) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O1 180.0 2_666 . ?
O1 U1 O2 90.41(10) 2_666 2_666 ?
O1 U1 O2 89.59(10) . 2_666 ?
O1 U1 O2 89.59(10) 2_666 . ?
O1 U1 O2 90.41(10) . . ?
O2 U1 O2 180.0 2_666 . ?
O1 U1 O4 89.52(9) 2_666 2_666 ?
O1 U1 O4 90.48(9) . 2_666 ?
O2 U1 O4 87.77(9) 2_666 2_666 ?
O2 U1 O4 92.23(9) . 2_666 ?
O1 U1 O4 90.48(9) 2_666 . ?
O1 U1 O4 89.52(9) . . ?
O2 U1 O4 92.23(9) 2_666 . ?
O2 U1 O4 87.77(9) . . ?
O4 U1 O4 180.0 2_666 . ?
N1 Ni1 N1 180.0 2_656 . ?
N1 Ni1 N2 94.58(12) 2_656 . ?
N1 Ni1 N2 85.42(12) . . ?
N1 Ni1 N2 85.42(12) 2_656 2_656 ?
N1 Ni1 N2 94.58(12) . 2_656 ?
N2 Ni1 N2 180.0 . 2_656 ?
N1 Ni1 O6 91.33(11) 2_656 2_656 ?
N1 Ni1 O6 88.67(11) . 2_656 ?
N2 Ni1 O6 92.66(11) . 2_656 ?
N2 Ni1 O6 87.34(11) 2_656 2_656 ?
N1 Ni1 O6 88.67(11) 2_656 . ?
N1 Ni1 O6 91.33(11) . . ?
N2 Ni1 O6 87.34(11) . . ?
N2 Ni1 O6 92.66(11) 2_656 . ?
O6 Ni1 O6 180.00(13) 2_656 . ?
C13 O2 U1 128.4(3) . . ?
C14 O4 U1 132.3(2) . . ?
Ni1 O6 H6A 115(3) . . ?
Ni1 O6 H6B 119(3) . . ?
H6A O6 H6B 113(4) . . ?
C15 N1 C19 115.3(3) . 2_656 ?
C15 N1 Ni1 106.0(2) . . ?
C19 N1 Ni1 114.7(2) 2_656 . ?
C15 N1 H1 108(2) . . ?
C19 N1 H1 106(2) 2_656 . ?
Ni1 N1 H1 107(2) . . ?
C16 N2 C17 115.3(2) . . ?
C16 N2 Ni1 105.5(2) . . ?
C17 N2 Ni1 122.2(2) . . ?
C16 N2 H2 110(2) . . ?
C17 N2 H2 101(2) . . ?
Ni1 N2 H2 101(2) . . ?
C6 C1 C2 119.7(3) . . ?
C6 C1 C13 116.7(3) . . ?
C2 C1 C13 123.4(3) . . ?
C3 C2 C1 118.0(3) . . ?
C3 C2 C7 117.7(3) . . ?
C1 C2 C7 124.0(3) . . ?
C4 C3 C2 122.4(3) . . ?
C4 C3 H3 118.8 . . ?
C2 C3 H3 118.8 . . ?
C3 C4 C5 119.0(3) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C6 C5 C4 119.8(3) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C1 121.0(3) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
C12 C7 C8 118.8(3) . . ?
C12 C7 C2 117.6(3) . . ?
C8 C7 C2 123.0(4) . . ?
C9 C8 C7 118.8(4) . . ?
C9 C8 C14 117.2(4) . . ?
C7 C8 C14 124.0(3) . . ?
C10 C9 C8 121.6(4) . . ?
C10 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
C9 C10 C11 119.5(3) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C10 C11 C12 119.5(4) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C7 C12 C11 121.7(4) . . ?
C7 C12 H12 119.1 . . ?
C11 C12 H12 119.1 . . ?
O3 C13 O2 123.1(3) . . ?
O3 C13 C1 120.6(3) . . ?
O2 C13 C1 116.2(3) . . ?
O5 C14 O4 121.6(4) . . ?
O5 C14 C8 121.0(3) . . ?
O4 C14 C8 117.3(3) . . ?
N1 C15 C16 110.2(3) . . ?
N1 C15 H15A 109.6 . . ?
C16 C15 H15A 109.6 . . ?
N1 C15 H15B 109.6 . . ?
C16 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
N2 C16 C15 108.6(3) . . ?
N2 C16 H16A 110.0 . . ?
C15 C16 H16A 110.0 . . ?
N2 C16 H16B 110.0 . . ?
C15 C16 H16B 110.0 . . ?
H16A C16 H16B 108.3 . . ?
C21 C17 N2 110.0(3) . . ?
C21 C17 C20 108.4(3) . . ?
N2 C17 C20 111.5(3) . . ?
C21 C17 C18 108.7(3) . . ?
N2 C17 C18 106.6(2) . . ?
C20 C17 C18 111.6(3) . . ?
C19 C18 C17 119.6(3) . . ?
C19 C18 H18A 107.4 . . ?
C17 C18 H18A 107.4 . . ?
C19 C18 H18B 107.4 . . ?
C17 C18 H18B 107.4 . . ?
H18A C18 H18B 107.0 . . ?
N1 C19 C18 109.4(3) 2_656 . ?
N1 C19 C22 111.5(3) 2_656 . ?
C18 C19 C22 110.0(3) . . ?
N1 C19 H19 108.6 2_656 . ?
C18 C19 H19 108.6 . . ?
C22 C19 H19 108.6 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O6 H6A O3 0.835(10) 1.978(12) 2.808(3) 172(5) 2_666 yes
O6 H6B O5 0.82(5) 1.91(5) 2.728(4) 178(4) . yes
N1 H1 O2 0.964(10) 2.500(15) 3.426(4) 161(3) 1_545 yes
N1 H1 O3 0.964(10) 2.45(2) 3.287(4) 145(3) 1_545 yes
N2 H2 O4 0.962(10) 2.533(13) 3.476(4) 166(3) . yes
C15 H15B O5 0.99 2.50 3.415(5) 154.2 . yes
C16 H16B O3 0.99 2.53 3.375(5) 142.8 1_545 yes
C20 H20C O6 0.98 2.34 3.203(5) 147.0 2_656 yes
C21 H21A O4 0.98 2.58 3.484(4) 152.7 . yes

_refine_diff_density_max         0.793
_refine_diff_density_min         -1.114
_refine_diff_density_rms         0.140

####################################################################### 
# 
# 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 1958814'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2019-10-11 deposited with the CCDC.	2019-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H29 Ag2 N O17 U2'
_chemical_formula_weight         1535.48

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

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

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

_cell_length_a                   9.4256(5)
_cell_length_b                   15.0290(5)
_cell_length_c                   15.8358(8)
_cell_angle_alpha                76.635(3)
_cell_angle_beta                 78.852(2)
_cell_angle_gamma                87.993(3)
_cell_volume                     2141.21(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    128849
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.382
_exptl_crystal_F_000             1428
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    8.520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.287
_exptl_absorpt_correction_T_max  0.464
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'2 φ and 13 ω scans with 2° steps (837 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            128849
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.594
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8145
_reflns_number_gt                7000
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The AG2 atom is disordered over two sites
 which were refined with occupancy parameters constrained to sum to unity.
 The H atoms bound to O17 were found on a difference Fourier map and were
 refined with restraints on bond lengths and angles, and with an isotropic
 displacement parameter equal to 1.5 times that of the parent atom. The 
 C-bound H atoms were introduced at calculated positions and were treated
 as riding atoms with an isotropic displacement parameter equal to 1.2 times
 that of the parent atom (1.5 for CH₃, with optimized geometry). 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0162P)²+0.0092P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8145
_refine_ls_number_parameters     612
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0586
_refine_ls_wR_factor_gt          0.0562
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.25337(2) 0.43681(2) 0.26395(2) 0.01870(5) Uani 1 1 d . . . . .
U2 U 0.13702(2) 0.03597(2) 0.70957(2) 0.02101(6) Uani 1 1 d . . . . .
Ag1 Ag 0.51837(4) 0.19052(3) 0.33935(2) 0.02868(10) Uani 1 1 d . . . . .
Ag2A Ag 0.03766(15) 0.66848(6) 0.34692(7) 0.0322(2) Uani 0.945(5) 1 d . U P A 1
Ag2B Ag -0.018(3) 0.6815(10) 0.3229(14) 0.040(4) Uani 0.055(5) 1 d . U P A 2
O1 O 0.0792(3) 0.3856(2) 0.2971(2) 0.0225(8) Uani 1 1 d . . . . .
O2 O 0.4255(3) 0.4879(2) 0.2297(2) 0.0243(8) Uani 1 1 d . . . . .
O3 O 0.1015(3) 0.0199(2) 0.6084(2) 0.0275(8) Uani 1 1 d . . . . .
O4 O 0.1742(3) 0.0490(2) 0.8109(2) 0.0251(8) Uani 1 1 d . . . . .
O5 O 0.2043(3) 0.4893(2) 0.4029(2) 0.0257(8) Uani 1 1 d . . . . .
O6 O 0.3076(3) 0.3555(2) 0.4056(2) 0.0238(8) Uani 1 1 d . . . . .
O7 O 0.2495(3) 0.1850(2) 0.6301(2) 0.0276(8) Uani 1 1 d . . . . .
O8 O 0.3946(3) 0.0674(2) 0.6367(2) 0.0256(8) Uani 1 1 d . . . . .
O9 O 0.3783(3) 0.2897(2) 0.25950(19) 0.0231(8) Uani 1 1 d . . . . .
O10 O 0.2895(3) 0.3526(2) 0.14203(19) 0.0215(7) Uani 1 1 d . . . . .
O11 O 0.7186(3) 0.1045(2) 0.2696(2) 0.0204(7) Uani 1 1 d . . . . .
O12 O 0.9502(3) 0.1203(2) 0.2134(2) 0.0243(8) Uani 1 1 d . . . . .
O13 O 0.1752(3) 0.5298(2) 0.1317(2) 0.0212(7) Uani 1 1 d . . . . .
O14 O 0.1542(3) 0.5929(2) 0.24442(19) 0.0206(7) Uani 1 1 d . . . . .
O15 O 0.1280(3) 0.9690(2) 0.2348(2) 0.0286(8) Uani 1 1 d . . . . .
O16 O 0.0248(3) 0.8327(2) 0.2797(2) 0.0239(7) Uani 1 1 d . . . . .
O17 O 0.3793(4) 0.0550(3) 0.3504(3) 0.0418(10) Uani 1 1 d D . . . .
H17A H 0.444(4) 0.015(3) 0.357(4) 0.063 Uiso 1 1 d D U . . .
H17B H 0.325(4) 0.038(3) 0.320(3) 0.063 Uiso 1 1 d D U . . .
N1 N 0.0219(4) 0.7173(3) 0.4695(3) 0.0371(12) Uani 1 1 d . . . . .
C1 C 0.2746(4) 0.4115(3) 0.5381(3) 0.0175(10) Uani 1 1 d . . . . .
C2 C 0.3829(4) 0.3585(3) 0.5750(3) 0.0187(10) Uani 1 1 d . . . . .
C3 C 0.3978(4) 0.3619(4) 0.6595(3) 0.0244(11) Uani 1 1 d . . . . .
H3 H 0.4752 0.3301 0.6833 0.029 Uiso 1 1 calc R U . . .
C4 C 0.3032(5) 0.4102(4) 0.7103(3) 0.0248(11) Uani 1 1 d . . . . .
H4 H 0.3153 0.4107 0.7683 0.030 Uiso 1 1 calc R U . . .
C5 C 0.1898(4) 0.4582(3) 0.6756(3) 0.0222(11) Uani 1 1 d . . . . .
H5 H 0.1223 0.4898 0.7107 0.027 Uiso 1 1 calc R U . . .
C6 C 0.1764(4) 0.4594(4) 0.5897(3) 0.0238(11) Uani 1 1 d . . . . .
H6 H 0.1004 0.4928 0.5656 0.029 Uiso 1 1 calc R U . . .
C7 C 0.4888(4) 0.3050(3) 0.5233(3) 0.0188(10) Uani 1 1 d . . . . .
C8 C 0.4872(4) 0.2097(4) 0.5412(3) 0.0222(11) Uani 1 1 d . . . . .
C9 C 0.5949(4) 0.1645(4) 0.4921(3) 0.0223(11) Uani 1 1 d . . . . .
H9 H 0.5954 0.0996 0.5042 0.027 Uiso 1 1 calc R U . . .
C10 C 0.7006(4) 0.2145(4) 0.4260(3) 0.0258(12) Uani 1 1 d . . . . .
H10 H 0.7719 0.1835 0.3926 0.031 Uiso 1 1 calc R U . . .
C11 C 0.7025(4) 0.3092(4) 0.4087(3) 0.0260(12) Uani 1 1 d . . . . .
H11 H 0.7747 0.3433 0.3637 0.031 Uiso 1 1 calc R U . . .
C12 C 0.5984(4) 0.3534(4) 0.4574(3) 0.0226(11) Uani 1 1 d . . . . .
H12 H 0.6009 0.4182 0.4462 0.027 Uiso 1 1 calc R U . . .
C13 C 0.2604(5) 0.4186(4) 0.4436(3) 0.0226(11) Uani 1 1 d . . . . .
C14 C 0.3709(5) 0.1526(4) 0.6064(3) 0.0247(11) Uani 1 1 d . . . . .
C15 C 0.4255(4) 0.2146(3) 0.1400(3) 0.0202(10) Uani 1 1 d . . . . .
C16 C 0.5771(4) 0.2018(3) 0.1228(3) 0.0195(10) Uani 1 1 d . . . . .
C17 C 0.6302(4) 0.1261(3) 0.0926(3) 0.0207(11) Uani 1 1 d . . . . .
H17 H 0.7317 0.1170 0.0807 0.025 Uiso 1 1 calc R U . . .
C18 C 0.5373(4) 0.0624(4) 0.0790(3) 0.0222(11) Uani 1 1 d . . . . .
H18 H 0.5754 0.0103 0.0584 0.027 Uiso 1 1 calc R U . . .
C19 C 0.3890(4) 0.0761(3) 0.0958(3) 0.0212(11) Uani 1 1 d . . . . .
H19 H 0.3254 0.0331 0.0865 0.025 Uiso 1 1 calc R U . . .
C20 C 0.3338(4) 0.1510(3) 0.1257(3) 0.0208(10) Uani 1 1 d . . . . .
H20 H 0.2322 0.1597 0.1368 0.025 Uiso 1 1 calc R U . . .
C21 C 0.6790(4) 0.2728(4) 0.1304(3) 0.0193(10) Uani 1 1 d . . . . .
C22 C 0.8017(4) 0.2472(3) 0.1705(3) 0.0196(10) Uani 1 1 d . . . . .
C23 C 0.9032(5) 0.3159(4) 0.1659(3) 0.0239(11) Uani 1 1 d . . . . .
H23 H 0.9868 0.2998 0.1911 0.029 Uiso 1 1 calc R U . . .
C24 C 0.8838(5) 0.4052(4) 0.1261(3) 0.0264(11) Uani 1 1 d . . . . .
H24 H 0.9529 0.4505 0.1241 0.032 Uiso 1 1 calc R U . . .
C25 C 0.7634(4) 0.4289(4) 0.0891(3) 0.0253(11) Uani 1 1 d . . . . .
H25 H 0.7491 0.4912 0.0625 0.030 Uiso 1 1 calc R U . . .
C26 C 0.6637(5) 0.3642(4) 0.0899(3) 0.0232(11) Uani 1 1 d . . . . .
H26 H 0.5830 0.3821 0.0623 0.028 Uiso 1 1 calc R U . . .
C27 C 0.3618(4) 0.2898(3) 0.1804(3) 0.0201(10) Uani 1 1 d . . . . .
C28 C 0.8253(4) 0.1536(4) 0.2184(3) 0.0225(11) Uani 1 1 d . . . . .
C29 C 0.0809(4) 0.6809(3) 0.1131(3) 0.0190(10) Uani 1 1 d . . . . .
C30 C 0.1280(4) 0.7684(4) 0.1122(3) 0.0210(11) Uani 1 1 d . . . . .
C31 C 0.0578(4) 0.8444(4) 0.0696(3) 0.0232(11) Uani 1 1 d . . . . .
H31 H 0.0867 0.9042 0.0698 0.028 Uiso 1 1 calc R U . . .
C32 C -0.0550(4) 0.8329(4) 0.0266(3) 0.0251(11) Uani 1 1 d . . . . .
H32 H -0.1034 0.8846 -0.0013 0.030 Uiso 1 1 calc R U . . .
C33 C -0.0951(4) 0.7460(4) 0.0252(3) 0.0257(12) Uani 1 1 d . . . . .
H33 H -0.1693 0.7381 -0.0055 0.031 Uiso 1 1 calc R U . . .
C34 C -0.0294(4) 0.6711(4) 0.0675(3) 0.0249(11) Uani 1 1 d . . . . .
H34 H -0.0585 0.6117 0.0661 0.030 Uiso 1 1 calc R U . . .
C35 C 0.2627(4) 0.7826(3) 0.1450(3) 0.0215(10) Uani 1 1 d . . . . .
C36 C 0.2685(4) 0.8411(3) 0.2007(3) 0.0215(10) Uani 1 1 d . . . . .
C37 C 0.4023(4) 0.8614(4) 0.2193(3) 0.0264(11) Uani 1 1 d . . . . .
H37 H 0.4067 0.9025 0.2562 0.032 Uiso 1 1 calc R U . . .
C38 C 0.5275(5) 0.8213(4) 0.1839(3) 0.0290(12) Uani 1 1 d . . . . .
H38 H 0.6178 0.8353 0.1962 0.035 Uiso 1 1 calc R U . . .
C39 C 0.5209(4) 0.7608(3) 0.1305(3) 0.0234(11) Uani 1 1 d . . . . .
H39 H 0.6065 0.7324 0.1071 0.028 Uiso 1 1 calc R U . . .
C40 C 0.3896(4) 0.7418(3) 0.1115(3) 0.0201(10) Uani 1 1 d . . . . .
H40 H 0.3858 0.7003 0.0750 0.024 Uiso 1 1 calc R U . . .
C41 C 0.1404(4) 0.5980(3) 0.1637(3) 0.0197(10) Uani 1 1 d . . . . .
C42 C 0.1358(4) 0.8840(4) 0.2406(3) 0.0246(11) Uani 1 1 d . . . . .
C43 C -0.0280(5) 0.7649(4) 0.5151(3) 0.0309(13) Uani 1 1 d . . . . .
C44 C -0.0902(5) 0.8242(4) 0.5718(3) 0.0344(13) Uani 1 1 d . . . . .
H44A H -0.0880 0.7941 0.6334 0.052 Uiso 1 1 calc R U . . .
H44B H -0.1905 0.8375 0.5652 0.052 Uiso 1 1 calc R U . . .
H44C H -0.0344 0.8815 0.5555 0.052 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 1.753(3) . ?
U1 O1 1.769(3) . ?
U1 O6 2.433(3) . ?
U1 O13 2.461(3) . ?
U1 O5 2.463(3) . ?
U1 O14 2.469(3) . ?
U1 O9 2.477(3) . ?
U1 O10 2.508(3) . ?
U2 O4 1.761(3) . ?
U2 O3 1.769(3) . ?
U2 O7 2.464(3) . ?
U2 O11 2.463(3) 2_656 ?
U2 O16 2.469(3) 2_566 ?
U2 O12 2.470(3) 2_656 ?
U2 O15 2.480(3) 2_566 ?
U2 O8 2.489(3) . ?
Ag1 O9 2.280(3) . ?
Ag1 O17 2.414(4) . ?
Ag1 O11 2.477(3) . ?
Ag1 C10 2.479(4) . ?
Ag1 C9 2.597(4) . ?
Ag2A N1 2.206(4) . ?
Ag2A O14 2.282(3) . ?
Ag2A O16 2.460(4) . ?
Ag2A C6 2.714(4) 2_566 ?
Ag2A C5 3.040(5) 2_566 ?
Ag2B O16 2.244(13) . ?
Ag2B O14 2.404(15) . ?
Ag2B N1 2.60(3) . ?
Ag2B C6 2.588(12) 2_566 ?
Ag2B C5 2.69(2) 2_566 ?
O5 C13 1.264(6) . ?
O6 C13 1.262(5) . ?
O7 C14 1.252(5) . ?
O8 C14 1.288(6) . ?
O9 C27 1.292(5) . ?
O10 C27 1.254(5) . ?
O11 C28 1.294(5) . ?
O11 U2 2.463(3) 2_656 ?
O12 C28 1.259(5) . ?
O12 U2 2.470(3) 2_656 ?
O13 C41 1.251(5) . ?
O14 C41 1.294(5) . ?
O15 C42 1.259(6) . ?
O15 U2 2.480(3) 2_566 ?
O16 C42 1.287(5) . ?
O16 U2 2.469(3) 2_566 ?
O17 H17A 0.840(10) . ?
O17 H17B 0.844(10) . ?
N1 C43 1.157(6) . ?
C1 C6 1.406(6) . ?
C1 C2 1.406(6) . ?
C1 C13 1.507(6) . ?
C2 C3 1.384(6) . ?
C2 C7 1.499(6) . ?
C3 C4 1.384(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.398(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(6) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.395(7) . ?
C7 C12 1.403(6) . ?
C8 C9 1.409(6) . ?
C8 C14 1.490(6) . ?
C9 C10 1.393(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.385(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.378(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C15 C20 1.395(6) . ?
C15 C16 1.417(5) . ?
C15 C27 1.478(6) . ?
C16 C17 1.376(6) . ?
C16 C21 1.500(6) . ?
C17 C18 1.398(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.389(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.368(6) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C26 1.390(7) . ?
C21 C22 1.425(6) . ?
C22 C23 1.413(6) . ?
C22 C28 1.468(7) . ?
C23 C24 1.366(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.375(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.372(6) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C29 C30 1.399(7) . ?
C29 C34 1.404(6) . ?
C29 C41 1.474(6) . ?
C30 C31 1.400(7) . ?
C30 C35 1.500(5) . ?
C31 C32 1.404(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.379(7) . ?
C32 H32 0.9500 . ?
C33 C34 1.364(7) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C40 1.393(6) . ?
C35 C36 1.391(6) . ?
C36 C37 1.407(6) . ?
C36 C42 1.486(6) . ?
C37 C38 1.386(6) . ?
C37 H37 0.9500 . ?
C38 C39 1.388(6) . ?
C38 H38 0.9500 . ?
C39 C40 1.383(6) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C43 C44 1.441(7) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U1 O1 179.28(14) . . ?
O2 U1 O6 92.40(13) . . ?
O1 U1 O6 88.30(12) . . ?
O2 U1 O13 90.72(13) . . ?
O1 U1 O13 88.61(12) . . ?
O6 U1 O13 172.62(10) . . ?
O2 U1 O5 93.64(12) . . ?
O1 U1 O5 86.94(12) . . ?
O6 U1 O5 53.38(11) . . ?
O13 U1 O5 119.74(10) . . ?
O2 U1 O14 87.19(13) . . ?
O1 U1 O14 92.63(12) . . ?
O6 U1 O14 120.96(10) . . ?
O13 U1 O14 52.52(10) . . ?
O5 U1 O14 67.72(10) . . ?
O2 U1 O9 86.34(13) . . ?
O1 U1 O9 93.75(13) . . ?
O6 U1 O9 66.17(10) . . ?
O13 U1 O9 120.74(10) . . ?
O5 U1 O9 119.51(10) . . ?
O14 U1 O9 170.60(10) . . ?
O2 U1 O10 93.40(12) . . ?
O1 U1 O10 86.10(11) . . ?
O6 U1 O10 117.32(11) . . ?
O13 U1 O10 69.13(10) . . ?
O5 U1 O10 168.58(12) . . ?
O14 U1 O10 121.64(10) . . ?
O9 U1 O10 52.07(10) . . ?
O4 U2 O3 178.49(16) . . ?
O4 U2 O7 92.09(13) . . ?
O3 U2 O7 88.94(14) . . ?
O4 U2 O11 86.67(13) . 2_656 ?
O3 U2 O11 91.86(13) . 2_656 ?
O7 U2 O11 121.26(10) . 2_656 ?
O4 U2 O16 84.51(13) . 2_566 ?
O3 U2 O16 96.91(13) . 2_566 ?
O7 U2 O16 66.12(10) . 2_566 ?
O11 U2 O16 168.76(10) 2_656 2_566 ?
O4 U2 O12 87.56(14) . 2_656 ?
O3 U2 O12 91.30(14) . 2_656 ?
O7 U2 O12 174.01(9) . 2_656 ?
O11 U2 O12 52.75(9) 2_656 2_656 ?
O16 U2 O12 119.76(10) 2_566 2_656 ?
O4 U2 O15 92.56(12) . 2_566 ?
O3 U2 O15 87.92(12) . 2_566 ?
O7 U2 O15 117.86(11) . 2_566 ?
O11 U2 O15 120.86(11) 2_656 2_566 ?
O16 U2 O15 52.81(11) 2_566 2_566 ?
O12 U2 O15 68.13(10) 2_656 2_566 ?
O4 U2 O8 91.17(12) . . ?
O3 U2 O8 88.59(12) . . ?
O7 U2 O8 52.54(11) . . ?
O11 U2 O8 68.76(11) 2_656 . ?
O16 U2 O8 118.30(11) 2_566 . ?
O12 U2 O8 121.49(10) 2_656 . ?
O15 U2 O8 169.86(12) 2_566 . ?
O9 Ag1 O17 95.96(12) . . ?
O9 Ag1 O11 122.63(10) . . ?
O17 Ag1 O11 83.24(11) . . ?
N1 Ag2A O14 151.86(16) . . ?
N1 Ag2A O16 83.02(15) . . ?
O14 Ag2A O16 110.25(12) . . ?
O16 Ag2B O14 113.7(5) . . ?
O16 Ag2B N1 79.2(6) . . ?
O14 Ag2B N1 121.0(14) . . ?
C13 O5 U1 92.0(3) . . ?
C13 O6 U1 93.5(3) . . ?
C14 O7 U2 94.8(3) . . ?
C14 O8 U2 92.7(3) . . ?
C27 O9 Ag1 125.5(3) . . ?
C27 O9 U1 94.8(3) . . ?
Ag1 O9 U1 138.72(13) . . ?
C27 O10 U1 94.4(2) . . ?
C28 O11 U2 93.5(3) . 2_656 ?
C28 O11 Ag1 115.6(3) . . ?
U2 O11 Ag1 145.09(14) 2_656 . ?
C28 O12 U2 94.0(3) . 2_656 ?
C41 O13 U1 95.6(3) . . ?
C41 O14 Ag2A 130.8(3) . . ?
C41 O14 Ag2B 114.5(8) . . ?
C41 O14 U1 94.0(3) . . ?
Ag2A O14 U1 130.16(14) . . ?
Ag2B O14 U1 139.7(4) . . ?
C42 O15 U2 93.5(3) . 2_566 ?
C42 O16 Ag2B 135.4(7) . . ?
C42 O16 Ag2A 124.2(3) . . ?
C42 O16 U2 93.3(3) . 2_566 ?
Ag2B O16 U2 131.3(6) . 2_566 ?
Ag2A O16 U2 140.04(13) . 2_566 ?
Ag1 O17 H17A 100(4) . . ?
Ag1 O17 H17B 136(4) . . ?
H17A O17 H17B 106.8(17) . . ?
C43 N1 Ag2A 150.7(4) . . ?
C43 N1 Ag2B 137.1(7) . . ?
C6 C1 C2 119.9(4) . . ?
C6 C1 C13 118.5(4) . . ?
C2 C1 C13 121.6(4) . . ?
C3 C2 C1 118.3(4) . . ?
C3 C2 C7 119.5(4) . . ?
C1 C2 C7 122.0(4) . . ?
C4 C3 C2 122.0(4) . . ?
C4 C3 H3 119.0 . . ?
C2 C3 H3 119.0 . . ?
C3 C4 C5 119.6(4) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C6 C5 C4 119.5(4) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C1 120.4(4) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
C8 C7 C12 119.1(4) . . ?
C8 C7 C2 122.7(4) . . ?
C12 C7 C2 118.0(4) . . ?
C7 C8 C9 119.1(4) . . ?
C7 C8 C14 123.0(4) . . ?
C9 C8 C14 117.8(5) . . ?
C10 C9 C8 120.4(5) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C11 C10 C9 120.4(4) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C12 C11 C10 119.3(4) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C11 C12 C7 121.7(5) . . ?
C11 C12 H12 119.2 . . ?
C7 C12 H12 119.2 . . ?
O6 C13 O5 121.1(4) . . ?
O6 C13 C1 119.8(4) . . ?
O5 C13 C1 119.1(4) . . ?
O7 C14 O8 119.4(4) . . ?
O7 C14 C8 121.5(5) . . ?
O8 C14 C8 119.1(4) . . ?
C20 C15 C16 119.7(4) . . ?
C20 C15 C27 119.1(4) . . ?
C16 C15 C27 121.0(4) . . ?
C17 C16 C15 118.7(4) . . ?
C17 C16 C21 120.2(4) . . ?
C15 C16 C21 120.9(4) . . ?
C16 C17 C18 121.1(4) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C19 C18 C17 119.4(4) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C20 C19 C18 120.4(4) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C19 C20 C15 120.6(4) . . ?
C19 C20 H20 119.7 . . ?
C15 C20 H20 119.7 . . ?
C26 C21 C22 118.6(4) . . ?
C26 C21 C16 120.2(4) . . ?
C22 C21 C16 120.9(4) . . ?
C23 C22 C21 118.2(5) . . ?
C23 C22 C28 118.6(4) . . ?
C21 C22 C28 123.2(4) . . ?
C24 C23 C22 121.5(4) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
C23 C24 C25 119.5(5) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
C26 C25 C24 121.1(5) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C25 C26 C21 121.1(4) . . ?
C25 C26 H26 119.5 . . ?
C21 C26 H26 119.5 . . ?
O10 C27 O9 118.5(4) . . ?
O10 C27 C15 122.9(4) . . ?
O9 C27 C15 118.6(4) . . ?
O12 C28 O11 118.3(5) . . ?
O12 C28 C22 121.0(4) . . ?
O11 C28 C22 120.7(4) . . ?
C30 C29 C34 119.7(5) . . ?
C30 C29 C41 121.6(4) . . ?
C34 C29 C41 118.7(4) . . ?
C31 C30 C29 118.6(4) . . ?
C31 C30 C35 119.4(4) . . ?
C29 C30 C35 121.5(4) . . ?
C32 C31 C30 120.6(5) . . ?
C32 C31 H31 119.7 . . ?
C30 C31 H31 119.7 . . ?
C33 C32 C31 119.5(5) . . ?
C33 C32 H32 120.2 . . ?
C31 C32 H32 120.2 . . ?
C34 C33 C32 120.6(4) . . ?
C34 C33 H33 119.7 . . ?
C32 C33 H33 119.7 . . ?
C33 C34 C29 120.8(5) . . ?
C33 C34 H34 119.6 . . ?
C29 C34 H34 119.6 . . ?
C40 C35 C36 119.0(4) . . ?
C40 C35 C30 118.1(4) . . ?
C36 C35 C30 122.7(4) . . ?
C35 C36 C37 119.9(4) . . ?
C35 C36 C42 121.2(4) . . ?
C37 C36 C42 118.8(4) . . ?
C38 C37 C36 120.0(4) . . ?
C38 C37 H37 120.0 . . ?
C36 C37 H37 120.0 . . ?
C39 C38 C37 120.0(4) . . ?
C39 C38 H38 120.0 . . ?
C37 C38 H38 120.0 . . ?
C40 C39 C38 119.8(4) . . ?
C40 C39 H39 120.1 . . ?
C38 C39 H39 120.1 . . ?
C39 C40 C35 121.2(4) . . ?
C39 C40 H40 119.4 . . ?
C35 C40 H40 119.4 . . ?
O13 C41 O14 117.9(4) . . ?
O13 C41 C29 121.8(4) . . ?
O14 C41 C29 120.2(4) . . ?
O15 C42 O16 119.6(4) . . ?
O15 C42 C36 121.8(4) . . ?
O16 C42 C36 118.6(5) . . ?
N1 C43 C44 180.0(7) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O17 H17A O8 0.840(10) 1.935(12) 2.772(5) 174(6) 2_656

_refine_diff_density_max         1.060
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.245

_shelxl_version_number           2014-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_7
_database_code_depnum_ccdc_archive 'CCDC 1958816'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2019-10-11 deposited with the CCDC.	2019-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C70 H68 N6 Ni O22 U2'
_chemical_formula_weight         1880.07

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

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

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

_cell_length_a                   11.7413(6)
_cell_length_b                   12.9324(7)
_cell_length_c                   13.9484(5)
_cell_angle_alpha                116.738(3)
_cell_angle_beta                 99.863(3)
_cell_angle_gamma                104.484(3)
_cell_volume                     1729.92(17)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    92782
_cell_measurement_theta_min      2.96
_cell_measurement_theta_max      25.68

_exptl_crystal_description       lath
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_F_000             918
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    5.020
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.517
_exptl_absorpt_correction_T_max  0.740
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and eleven ω scans with 2° steps (752 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            92782
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.958
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6561
_reflns_number_gt                5805
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms bound to O and N atoms were found
 on a difference Fourier map and were refined (with restraints on bond lengths
 and angles when necessary) with an isotropic displacement parameter
 equal to 1.2 or 1.5 (water) times that of the parent atom. The C-bound H
 atoms were introduced at calculated positions and were treated as riding
 atoms with an isotropic displacement parameter equal to 1.2 times that of
 the parent atom (1.5 for CH₃, with optimized geometry). 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0168P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6561
_refine_ls_number_parameters     473
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0272
_refine_ls_wR_factor_ref         0.0557
_refine_ls_wR_factor_gt          0.0538
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.81978(2) 0.29743(2) 0.44408(2) 0.01989(5) Uani 1 1 d . . . . .
Ni1 Ni 0.5000 0.0000 0.0000 0.02152(16) Uani 1 2 d S . P . .
O1 O 0.7558(2) 0.3960(2) 0.4184(2) 0.0231(6) Uani 1 1 d . . . . .
O2 O 0.8833(2) 0.1977(2) 0.4684(2) 0.0211(6) Uani 1 1 d . . . . .
O3 O 0.9851(2) 0.3581(2) 0.3850(2) 0.0199(6) Uani 1 1 d . . . . .
O4 O 1.0435(2) 0.5334(2) 0.3797(2) 0.0221(6) Uani 1 1 d . . . . .
O5 O 0.7400(2) 0.1588(2) 0.2454(2) 0.0245(6) Uani 1 1 d . . . . .
O6 O 0.6697(2) -0.0137(2) 0.0755(2) 0.0246(6) Uani 1 1 d . . . . .
O7 O 0.7124(2) 0.3051(2) 0.5809(2) 0.0237(6) Uani 1 1 d . . . . .
O8 O 0.6059(2) 0.1620(2) 0.4015(2) 0.0244(6) Uani 1 1 d . . . . .
O9 O 0.4705(2) 0.4104(3) 0.5530(2) 0.0287(7) Uani 1 1 d . . . . .
O10 O 0.6460(2) 0.5762(3) 0.6203(2) 0.0283(7) Uani 1 1 d . . . . .
H10 H 0.604(3) 0.570(4) 0.561(3) 0.034 Uiso 1 1 d . U . . .
O11 O 0.8575(3) 0.2766(4) 0.7633(3) 0.0667(11) Uani 1 1 d D . . . .
H11A H 0.825(4) 0.298(5) 0.718(4) 0.100 Uiso 1 1 d D U . . .
H11B H 0.9366(13) 0.307(5) 0.773(5) 0.100 Uiso 1 1 d D U . . .
N1 N 0.3913(3) -0.1423(3) 0.0146(3) 0.0229(7) Uani 1 1 d . . . . .
H1 H 0.316(3) -0.166(4) -0.024(3) 0.027 Uiso 1 1 d . U . . .
N2 N 0.4849(3) 0.1176(3) 0.1529(3) 0.0219(7) Uani 1 1 d D . . . .
H2 H 0.5604(17) 0.136(3) 0.203(2) 0.026 Uiso 1 1 d D U . . .
N3 N 1.1277(4) 0.3224(4) 0.7483(4) 0.0502(11) Uani 1 1 d . . . . .
C1 C 0.9744(3) 0.3425(3) 0.2065(3) 0.0185(8) Uani 1 1 d . . . . .
C2 C 0.9651(3) 0.2180(4) 0.1472(3) 0.0191(8) Uani 1 1 d . . . . .
C3 C 0.9399(3) 0.1595(4) 0.0302(3) 0.0236(9) Uani 1 1 d . . . . .
H3 H 0.9353 0.0759 -0.0106 0.028 Uiso 1 1 calc R U . . .
C4 C 0.9212(3) 0.2201(4) -0.0290(3) 0.0250(9) Uani 1 1 d . . . . .
H4 H 0.9039 0.1782 -0.1090 0.030 Uiso 1 1 calc R U . . .
C5 C 0.9281(3) 0.3429(4) 0.0307(3) 0.0253(9) Uani 1 1 d . . . . .
H5 H 0.9141 0.3848 -0.0086 0.030 Uiso 1 1 calc R U . . .
C6 C 0.9551(3) 0.4030(4) 0.1463(3) 0.0217(9) Uani 1 1 d . . . . .
H6 H 0.9609 0.4871 0.1866 0.026 Uiso 1 1 calc R U . . .
C7 C 0.9825(3) 0.1415(3) 0.1997(3) 0.0198(8) Uani 1 1 d . . . . .
C8 C 0.8778(3) 0.0556(3) 0.1955(3) 0.0193(8) Uani 1 1 d . . . . .
C9 C 0.8919(3) -0.0285(4) 0.2288(3) 0.0228(9) Uani 1 1 d . . . . .
H9 H 0.8203 -0.0898 0.2208 0.027 Uiso 1 1 calc R U . . .
C10 C 1.0095(3) -0.0233(4) 0.2734(3) 0.0256(9) Uani 1 1 d . . . . .
H10A H 1.0192 -0.0789 0.2983 0.031 Uiso 1 1 calc R U . . .
C11 C 1.1131(3) 0.0646(4) 0.2812(3) 0.0253(9) Uani 1 1 d . . . . .
H11 H 1.1941 0.0700 0.3133 0.030 Uiso 1 1 calc R U . . .
C12 C 1.0995(3) 0.1440(4) 0.2430(3) 0.0230(9) Uani 1 1 d . . . . .
H12 H 1.1712 0.2012 0.2463 0.028 Uiso 1 1 calc R U . . .
C13 C 1.0033(3) 0.4160(4) 0.3321(3) 0.0213(9) Uani 1 1 d . . . . .
C14 C 0.7520(3) 0.0638(4) 0.1669(3) 0.0201(8) Uani 1 1 d . . . . .
C15 C 0.5007(3) 0.1771(4) 0.5373(3) 0.0212(9) Uani 1 1 d . . . . .
C16 C 0.4874(3) 0.2503(4) 0.6424(3) 0.0241(9) Uani 1 1 d . . . . .
C17 C 0.3794(3) 0.1991(4) 0.6621(3) 0.0271(9) Uani 1 1 d . . . . .
H17 H 0.3675 0.2462 0.7323 0.032 Uiso 1 1 calc R U . . .
C18 C 0.2902(4) 0.0824(4) 0.5824(4) 0.0304(10) Uani 1 1 d . . . . .
H18 H 0.2188 0.0507 0.5989 0.036 Uiso 1 1 calc R U . . .
C19 C 0.3037(3) 0.0116(4) 0.4794(3) 0.0276(9) Uani 1 1 d . . . . .
H19 H 0.2424 -0.0685 0.4244 0.033 Uiso 1 1 calc R U . . .
C20 C 0.4094(3) 0.0605(4) 0.4581(3) 0.0250(9) Uani 1 1 d . . . . .
H20 H 0.4196 0.0127 0.3872 0.030 Uiso 1 1 calc R U . . .
C21 C 0.5791(3) 0.3742(4) 0.7364(3) 0.0212(8) Uani 1 1 d . . . . .
C22 C 0.6219(3) 0.4833(4) 0.7304(3) 0.0238(9) Uani 1 1 d . . . . .
C23 C 0.7078(3) 0.5931(4) 0.8255(3) 0.0264(9) Uani 1 1 d . . . . .
H23 H 0.7383 0.6646 0.8196 0.032 Uiso 1 1 calc R U . . .
C24 C 0.7503(3) 0.6018(4) 0.9285(4) 0.0297(9) Uani 1 1 d . . . . .
H24 H 0.8079 0.6786 0.9929 0.036 Uiso 1 1 calc R U . . .
C25 C 0.7080(4) 0.4975(4) 0.9363(4) 0.0328(10) Uani 1 1 d . . . . .
H25 H 0.7359 0.5020 1.0067 0.039 Uiso 1 1 calc R U . . .
C26 C 0.6249(4) 0.3862(4) 0.8419(3) 0.0292(10) Uani 1 1 d . . . . .
H26 H 0.5977 0.3150 0.8489 0.035 Uiso 1 1 calc R U . . .
C27 C 0.6125(3) 0.2173(4) 0.5054(3) 0.0211(8) Uani 1 1 d . . . . .
C28 C 0.5713(4) 0.4845(4) 0.6256(3) 0.0233(9) Uani 1 1 d . . . . .
C29 C 0.3972(3) -0.0826(4) 0.1357(3) 0.0250(9) Uani 1 1 d . . . . .
H29A H 0.4776 -0.0701 0.1841 0.030 Uiso 1 1 calc R U . . .
H29B H 0.3290 -0.1365 0.1449 0.030 Uiso 1 1 calc R U . . .
C30 C 0.3842(3) 0.0423(4) 0.1705(3) 0.0247(9) Uani 1 1 d . . . . .
H30A H 0.3024 0.0296 0.1240 0.030 Uiso 1 1 calc R U . . .
H30B H 0.3896 0.0855 0.2514 0.030 Uiso 1 1 calc R U . . .
C31 C 0.4739(3) 0.2350(4) 0.1700(3) 0.0281(9) Uani 1 1 d . . . . .
H31A H 0.4751 0.2858 0.2488 0.034 Uiso 1 1 calc R U . . .
H31B H 0.3929 0.2160 0.1179 0.034 Uiso 1 1 calc R U . . .
C32 C 0.5785(4) 0.3106(4) 0.1490(3) 0.0280(9) Uani 1 1 d . . . . .
H32A H 0.6590 0.3218 0.1962 0.034 Uiso 1 1 calc R U . . .
H32B H 0.5749 0.3944 0.1758 0.034 Uiso 1 1 calc R U . . .
C33 C 0.5771(4) 0.2550(4) 0.0256(3) 0.0268(9) Uani 1 1 d . . . . .
H33A H 0.4934 0.2335 -0.0240 0.032 Uiso 1 1 calc R U . . .
H33B H 0.6376 0.3184 0.0193 0.032 Uiso 1 1 calc R U . . .
C34 C 1.1526(4) 0.3257(4) 0.6749(4) 0.0352(11) Uani 1 1 d . . . . .
C35 C 1.1839(4) 0.3302(4) 0.5781(4) 0.0359(11) Uani 1 1 d . . . . .
H35A H 1.2712 0.3399 0.5874 0.054 Uiso 1 1 calc R U . . .
H35B H 1.1707 0.4011 0.5757 0.054 Uiso 1 1 calc R U . . .
H35C H 1.1303 0.2526 0.5070 0.054 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.765(2) . ?
U1 O2 1.767(2) . ?
U1 O3 2.331(2) . ?
U1 O4 2.336(3) 2_766 ?
U1 O5 2.360(3) . ?
U1 O7 2.441(2) . ?
U1 O8 2.466(2) . ?
Ni1 N2 2.059(3) . ?
Ni1 N2 2.059(3) 2_655 ?
Ni1 N1 2.076(3) 2_655 ?
Ni1 N1 2.076(3) . ?
Ni1 O6 2.176(2) 2_655 ?
Ni1 O6 2.176(2) . ?
O3 C13 1.274(4) . ?
O4 C13 1.263(4) . ?
O4 U1 2.336(3) 2_766 ?
O5 C14 1.288(4) . ?
O6 C14 1.228(4) . ?
O7 C27 1.268(4) . ?
O8 C27 1.273(4) . ?
O9 C28 1.222(4) . ?
O10 C28 1.327(4) . ?
O10 H10 0.85(4) . ?
O11 H11A 0.868(10) . ?
O11 H11B 0.873(10) . ?
N1 C33 1.476(5) 2_655 ?
N1 C29 1.488(5) . ?
N1 H1 0.84(4) . ?
N2 C30 1.465(4) . ?
N2 C31 1.470(5) . ?
N2 H2 0.927(10) . ?
N3 C34 1.127(5) . ?
C1 C2 1.404(5) . ?
C1 C6 1.408(5) . ?
C1 C13 1.492(5) . ?
C2 C3 1.391(5) . ?
C2 C7 1.503(4) . ?
C3 C4 1.397(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.394(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.371(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.388(5) . ?
C7 C8 1.408(5) . ?
C8 C9 1.394(5) . ?
C8 C14 1.506(5) . ?
C9 C10 1.385(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.391(5) . ?
C10 H10A 0.9500 . ?
C11 C12 1.383(5) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C15 C20 1.389(5) . ?
C15 C16 1.405(5) . ?
C15 C27 1.502(5) . ?
C16 C17 1.409(5) . ?
C16 C21 1.486(5) . ?
C17 C18 1.383(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.376(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.390(5) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C26 1.401(5) . ?
C21 C22 1.420(5) . ?
C22 C23 1.387(5) . ?
C22 C28 1.489(5) . ?
C23 C24 1.381(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.377(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.382(5) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C29 C30 1.520(5) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.527(5) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.534(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 N1 1.476(5) 2_655 ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.481(6) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 179.48(11) . . ?
O1 U1 O3 90.32(9) . . ?
O2 U1 O3 89.57(9) . . ?
O1 U1 O4 90.57(10) . 2_766 ?
O2 U1 O4 89.92(10) . 2_766 ?
O3 U1 O4 81.73(8) . 2_766 ?
O1 U1 O5 86.43(10) . . ?
O2 U1 O5 93.05(10) . . ?
O3 U1 O5 77.22(8) . . ?
O4 U1 O5 158.72(8) 2_766 . ?
O1 U1 O7 91.32(9) . . ?
O2 U1 O7 88.99(9) . . ?
O3 U1 O7 155.90(9) . . ?
O4 U1 O7 74.21(8) 2_766 . ?
O5 U1 O7 126.87(8) . . ?
O1 U1 O8 87.82(9) . . ?
O2 U1 O8 92.02(9) . . ?
O3 U1 O8 150.75(9) . . ?
O4 U1 O8 127.46(8) 2_766 . ?
O5 U1 O8 73.52(8) . . ?
O7 U1 O8 53.35(8) . . ?
N2 Ni1 N2 180.0 . 2_655 ?
N2 Ni1 N1 94.86(12) . 2_655 ?
N2 Ni1 N1 85.14(12) 2_655 2_655 ?
N2 Ni1 N1 85.14(12) . . ?
N2 Ni1 N1 94.86(12) 2_655 . ?
N1 Ni1 N1 180.00(13) 2_655 . ?
N2 Ni1 O6 85.02(10) . 2_655 ?
N2 Ni1 O6 94.98(10) 2_655 2_655 ?
N1 Ni1 O6 91.16(10) 2_655 2_655 ?
N1 Ni1 O6 88.84(10) . 2_655 ?
N2 Ni1 O6 94.98(10) . . ?
N2 Ni1 O6 85.02(10) 2_655 . ?
N1 Ni1 O6 88.84(10) 2_655 . ?
N1 Ni1 O6 91.16(10) . . ?
O6 Ni1 O6 180.00(14) 2_655 . ?
C13 O3 U1 132.8(2) . . ?
C13 O4 U1 136.2(2) . 2_766 ?
C14 O5 U1 140.9(2) . . ?
C14 O6 Ni1 128.1(2) . . ?
C27 O7 U1 93.9(2) . . ?
C27 O8 U1 92.6(2) . . ?
C28 O10 H10 103(3) . . ?
H11A O11 H11B 101.7(15) . . ?
C33 N1 C29 113.9(3) 2_655 . ?
C33 N1 Ni1 115.8(2) 2_655 . ?
C29 N1 Ni1 105.1(2) . . ?
C33 N1 H1 107(3) 2_655 . ?
C29 N1 H1 106(3) . . ?
Ni1 N1 H1 109(2) . . ?
C30 N2 C31 113.5(3) . . ?
C30 N2 Ni1 106.7(2) . . ?
C31 N2 Ni1 117.4(2) . . ?
C30 N2 H2 109(2) . . ?
C31 N2 H2 109(2) . . ?
Ni1 N2 H2 101(2) . . ?
C2 C1 C6 119.6(3) . . ?
C2 C1 C13 123.4(3) . . ?
C6 C1 C13 117.1(3) . . ?
C3 C2 C1 118.3(3) . . ?
C3 C2 C7 116.2(3) . . ?
C1 C2 C7 125.5(3) . . ?
C2 C3 C4 121.9(4) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
C5 C4 C3 119.2(4) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C6 C5 C4 119.8(3) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C1 121.2(4) . . ?
C5 C6 H6 119.4 . . ?
C1 C6 H6 119.4 . . ?
C12 C7 C8 118.2(3) . . ?
C12 C7 C2 121.6(3) . . ?
C8 C7 C2 119.9(3) . . ?
C9 C8 C7 120.4(3) . . ?
C9 C8 C14 119.7(3) . . ?
C7 C8 C14 119.6(3) . . ?
C10 C9 C8 120.5(3) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C11 119.0(3) . . ?
C9 C10 H10A 120.5 . . ?
C11 C10 H10A 120.5 . . ?
C12 C11 C10 120.8(3) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C7 121.0(3) . . ?
C11 C12 H12 119.5 . . ?
C7 C12 H12 119.5 . . ?
O4 C13 O3 123.8(3) . . ?
O4 C13 C1 117.3(3) . . ?
O3 C13 C1 118.9(3) . . ?
O6 C14 O5 123.9(3) . . ?
O6 C14 C8 121.9(3) . . ?
O5 C14 C8 114.2(3) . . ?
C20 C15 C16 120.1(3) . . ?
C20 C15 C27 116.8(3) . . ?
C16 C15 C27 123.0(4) . . ?
C15 C16 C17 116.8(4) . . ?
C15 C16 C21 126.0(3) . . ?
C17 C16 C21 117.1(3) . . ?
C18 C17 C16 122.1(4) . . ?
C18 C17 H17 119.0 . . ?
C16 C17 H17 119.0 . . ?
C19 C18 C17 120.7(4) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C18 C19 C20 118.2(4) . . ?
C18 C19 H19 120.9 . . ?
C20 C19 H19 120.9 . . ?
C15 C20 C19 122.1(4) . . ?
C15 C20 H20 119.0 . . ?
C19 C20 H20 119.0 . . ?
C26 C21 C22 116.6(4) . . ?
C26 C21 C16 117.3(3) . . ?
C22 C21 C16 126.0(3) . . ?
C23 C22 C21 119.7(3) . . ?
C23 C22 C28 118.9(3) . . ?
C21 C22 C28 121.3(4) . . ?
C24 C23 C22 122.1(4) . . ?
C24 C23 H23 118.9 . . ?
C22 C23 H23 118.9 . . ?
C25 C24 C23 118.9(4) . . ?
C25 C24 H24 120.6 . . ?
C23 C24 H24 120.6 . . ?
C24 C25 C26 120.1(4) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C25 C26 C21 122.6(4) . . ?
C25 C26 H26 118.7 . . ?
C21 C26 H26 118.7 . . ?
O7 C27 O8 120.2(3) . . ?
O7 C27 C15 120.6(3) . . ?
O8 C27 C15 119.2(3) . . ?
O9 C28 O10 123.4(3) . . ?
O9 C28 C22 123.6(3) . . ?
O10 C28 C22 112.9(3) . . ?
N1 C29 C30 108.1(3) . . ?
N1 C29 H29A 110.1 . . ?
C30 C29 H29A 110.1 . . ?
N1 C29 H29B 110.1 . . ?
C30 C29 H29B 110.1 . . ?
H29A C29 H29B 108.4 . . ?
N2 C30 C29 108.1(3) . . ?
N2 C30 H30A 110.1 . . ?
C29 C30 H30A 110.1 . . ?
N2 C30 H30B 110.1 . . ?
C29 C30 H30B 110.1 . . ?
H30A C30 H30B 108.4 . . ?
N2 C31 C32 112.5(3) . . ?
N2 C31 H31A 109.1 . . ?
C32 C31 H31A 109.1 . . ?
N2 C31 H31B 109.1 . . ?
C32 C31 H31B 109.1 . . ?
H31A C31 H31B 107.8 . . ?
C31 C32 C33 116.1(3) . . ?
C31 C32 H32A 108.3 . . ?
C33 C32 H32A 108.3 . . ?
C31 C32 H32B 108.3 . . ?
C33 C32 H32B 108.3 . . ?
H32A C32 H32B 107.4 . . ?
N1 C33 C32 112.5(3) 2_655 . ?
N1 C33 H33A 109.1 2_655 . ?
C32 C33 H33A 109.1 . . ?
N1 C33 H33B 109.1 2_655 . ?
C32 C33 H33B 109.1 . . ?
H33A C33 H33B 107.8 . . ?
N3 C34 C35 179.3(5) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O10 H10 O9 0.85(4) 1.83(4) 2.665(4) 169(4) 2_666
O11 H11A O7 0.868(10) 2.183(16) 3.032(4) 166(5) .
O11 H11B N3 0.873(10) 2.30(2) 3.139(5) 161(6) .
N2 H2 O5 0.927(10) 1.998(18) 2.860(4) 154(3) .
N2 H2 O8 0.927(10) 2.58(3) 3.239(4) 129(3) .
C31 H31B O6 0.99 2.58 3.090(5) 111.8 2_655
C35 H35A O9 0.98 2.50 3.392(4) 151.4 1_655
C35 H35B O1 0.98 2.51 3.409(5) 152.7 2_766

_refine_diff_density_max         1.188
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.126

_shelxl_version_number           2014-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_8
_database_code_depnum_ccdc_archive 'CCDC 1958817'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2019-10-11 deposited with the CCDC.	2019-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H52 Cu N6 O18 U2'
_chemical_formula_weight         1492.51

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.4464(8)
_cell_length_b                   9.6422(10)
_cell_length_c                   15.0190(12)
_cell_angle_alpha                82.508(5)
_cell_angle_beta                 73.613(5)
_cell_angle_gamma                67.945(4)
_cell_volume                     1215.9(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    56007
_cell_measurement_theta_min      2.66
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.038
_exptl_crystal_F_000             715
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    7.157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.356
_exptl_absorpt_correction_T_max  0.606
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'2 φ and 12 ω scans with 2° steps (737 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            56007
_diffrn_reflns_av_unetI/netI     0.1166
_diffrn_reflns_av_R_equivalents  0.1037
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.660
_diffrn_reflns_theta_max         25.679
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4604
_reflns_number_gt                3761
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms bound to N atoms were found on a 
 difference Fourier map and were refined with restraints on bond lengths
 and with an isotropic displacement parameter equal to 1.2 times 
 that of the parent atom. The C-bound H atoms were introduced
 at calculated positions and were treated as riding atoms with an
 isotropic displacement parameter equal to 1.2 times that of the parent
 atom (1.5 for CH₃, with optimized geometry).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0049P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4604
_refine_ls_number_parameters     331
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.0710
_refine_ls_wR_factor_gt          0.0677
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_restrained_S_all      0.965
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.04625(3) 0.51040(3) 0.81900(2) 0.03275(9) Uani 1 1 d . . . . .
Cu1 Cu 0.500000 0.500000 0.500000 0.0321(3) Uani 1 2 d S . P . .
O1 O 0.1629(4) 0.5957(4) 0.8445(4) 0.0319(11) Uani 1 1 d . . . . .
O2 O -0.0710(4) 0.4269(4) 0.7914(3) 0.0351(11) Uani 1 1 d . . . . .
O3 O 0.0997(4) 0.3471(4) 0.9414(3) 0.0314(11) Uani 1 1 d . . . . .
O4 O 0.1809(5) 0.3653(4) 1.0638(4) 0.0367(12) Uani 1 1 d . . . . .
O5 O 0.2638(4) 0.3435(4) 0.7256(4) 0.0342(12) Uani 1 1 d . . . . .
O6 O 0.3188(5) 0.1781(5) 0.6180(4) 0.0383(12) Uani 1 1 d . . . . .
O7 O 0.0837(5) 0.6381(4) 0.6603(4) 0.0393(12) Uani 1 1 d . . . . .
O8 O -0.1082(5) 0.7715(4) 0.7649(4) 0.0371(12) Uani 1 1 d . . . . .
O9 O -0.0335(5) 0.8762(5) 0.6315(4) 0.0418(13) Uani 1 1 d . . . . .
N1 N -0.0223(6) 0.7683(6) 0.6841(5) 0.0372(15) Uani 1 1 d . . . . .
N2 N 0.7030(6) 0.3491(5) 0.5270(4) 0.0298(13) Uani 1 1 d D . . . .
H2 H 0.756(6) 0.365(6) 0.4635(15) 0.036 Uiso 1 1 d D U . . .
N3 N 0.4711(6) 0.3212(5) 0.4619(5) 0.0334(14) Uani 1 1 d D . . . .
H3 H 0.398(5) 0.308(6) 0.519(2) 0.040 Uiso 1 1 d D U . . .
C1 C 0.3761(6) 0.2649(6) 0.9274(5) 0.0303(16) Uani 1 1 d . . . . .
C2 C 0.4257(7) 0.1520(6) 0.8629(5) 0.0336(16) Uani 1 1 d . . . . .
C3 C 0.5819(7) 0.1049(7) 0.8130(5) 0.0361(17) Uani 1 1 d . . . . .
H3A H 0.619327 0.025855 0.770934 0.043 Uiso 1 1 calc R U . . .
C4 C 0.6850(7) 0.1684(7) 0.8222(5) 0.0387(17) Uani 1 1 d . . . . .
H4 H 0.790737 0.134700 0.785176 0.046 Uiso 1 1 calc R U . . .
C5 C 0.6374(7) 0.2793(7) 0.8837(5) 0.0352(17) Uani 1 1 d . . . . .
H5 H 0.708649 0.323900 0.889008 0.042 Uiso 1 1 calc R U . . .
C6 C 0.4822(7) 0.3262(6) 0.9387(5) 0.0354(17) Uani 1 1 d . . . . .
H6 H 0.448791 0.399923 0.983855 0.043 Uiso 1 1 calc R U . . .
C7 C 0.3164(7) 0.0785(6) 0.8551(5) 0.0315(16) Uani 1 1 d . . . . .
C8 C 0.2550(7) 0.1008(6) 0.7769(5) 0.0318(17) Uani 1 1 d . . . . .
C9 C 0.1566(7) 0.0286(6) 0.7721(5) 0.0361(17) Uani 1 1 d . . . . .
H9 H 0.116914 0.042314 0.718879 0.043 Uiso 1 1 calc R U . . .
C10 C 0.1151(7) -0.0653(6) 0.8460(6) 0.0355(17) Uani 1 1 d . . . . .
H10 H 0.043018 -0.111278 0.844010 0.043 Uiso 1 1 calc R U . . .
C11 C 0.1774(7) -0.0909(7) 0.9205(6) 0.043(2) Uani 1 1 d . . . . .
H11 H 0.151317 -0.157669 0.969086 0.051 Uiso 1 1 calc R U . . .
C12 C 0.2785(7) -0.0208(6) 0.9267(5) 0.0372(17) Uani 1 1 d . . . . .
H12 H 0.321702 -0.039879 0.978960 0.045 Uiso 1 1 calc R U . . .
C13 C 0.2083(7) 0.3287(7) 0.9819(5) 0.0323(16) Uani 1 1 d . . . . .
C14 C 0.2845(7) 0.2088(7) 0.6983(6) 0.0343(17) Uani 1 1 d . . . . .
C15 C 0.6865(7) 0.2014(6) 0.5347(5) 0.0336(17) Uani 1 1 d . . . . .
H15A H 0.615341 0.189879 0.595416 0.040 Uiso 1 1 calc R U . . .
H15B H 0.790844 0.120783 0.530096 0.040 Uiso 1 1 calc R U . . .
C16 C 0.6201(7) 0.1907(6) 0.4579(6) 0.0388(19) Uani 1 1 d . . . . .
H16A H 0.696595 0.191034 0.397322 0.047 Uiso 1 1 calc R U . . .
H16B H 0.598782 0.096373 0.464818 0.047 Uiso 1 1 calc R U . . .
C17 C 0.3998(7) 0.3402(6) 0.3817(6) 0.0327(17) Uani 1 1 d . . . . .
C18 C 0.2378(6) 0.4653(6) 0.4046(5) 0.0299(15) Uani 1 1 d . . . . .
H18A H 0.177712 0.458024 0.362091 0.036 Uiso 1 1 calc R U . . .
H18B H 0.181029 0.445718 0.468370 0.036 Uiso 1 1 calc R U . . .
C19 C 0.2329(7) 0.6262(6) 0.3988(5) 0.0322(16) Uani 1 1 d . . . . .
H19 H 0.298525 0.645219 0.336820 0.039 Uiso 1 1 calc R U . . .
C20 C 0.3757(7) 0.1972(6) 0.3677(6) 0.0430(19) Uani 1 1 d . . . . .
H20A H 0.475384 0.112248 0.362652 0.065 Uiso 1 1 calc R U . . .
H20B H 0.341004 0.207850 0.310747 0.065 Uiso 1 1 calc R U . . .
H20C H 0.295228 0.179896 0.420829 0.065 Uiso 1 1 calc R U . . .
C21 C 0.5098(7) 0.3788(7) 0.2933(6) 0.0432(19) Uani 1 1 d . . . . .
H21A H 0.549307 0.451569 0.307661 0.065 Uiso 1 1 calc R U . . .
H21B H 0.451219 0.421649 0.245809 0.065 Uiso 1 1 calc R U . . .
H21C H 0.598910 0.287657 0.270196 0.065 Uiso 1 1 calc R U . . .
C22 C 0.0602(6) 0.7347(6) 0.4098(6) 0.0382(18) Uani 1 1 d . . . . .
H22A H -0.005026 0.715224 0.469968 0.057 Uiso 1 1 calc R U . . .
H22B H 0.019985 0.719356 0.359871 0.057 Uiso 1 1 calc R U . . .
H22C H 0.056335 0.838205 0.406466 0.057 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.742(4) . ?
U1 O2 1.750(4) . ?
U1 O5 2.293(4) . ?
U1 O3 2.299(5) . ?
U1 O4 2.372(4) 2_567 ?
U1 O7 2.532(5) . ?
U1 O8 2.551(4) . ?
Cu1 N3 2.019(5) 2_666 ?
Cu1 N3 2.019(5) . ?
Cu1 N2 2.037(5) . ?
Cu1 N2 2.037(5) 2_666 ?
O3 C13 1.281(7) . ?
O4 C13 1.252(8) . ?
O5 C14 1.340(7) . ?
O6 C14 1.203(9) . ?
O7 N1 1.295(6) . ?
O8 N1 1.252(7) . ?
O9 N1 1.211(7) . ?
N2 C15 1.476(7) . ?
N2 C19 1.490(8) 2_666 ?
N2 H2 0.968(10) . ?
N3 C16 1.486(7) . ?
N3 C17 1.499(9) . ?
N3 H3 0.964(10) . ?
C1 C6 1.396(8) . ?
C1 C2 1.406(8) . ?
C1 C13 1.492(8) . ?
C2 C3 1.380(8) . ?
C2 C7 1.491(8) . ?
C3 C4 1.374(8) . ?
C3 H3A 0.9500 . ?
C4 C5 1.364(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.397(8) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.405(9) . ?
C7 C8 1.410(9) . ?
C8 C9 1.375(8) . ?
C8 C14 1.506(9) . ?
C9 C10 1.401(9) . ?
C9 H9 0.9500 . ?
C10 C11 1.361(10) . ?
C10 H10 0.9500 . ?
C11 C12 1.389(8) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C15 C16 1.490(9) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C20 1.527(7) . ?
C17 C18 1.530(7) . ?
C17 C21 1.537(9) . ?
C18 C19 1.527(7) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C22 1.548(7) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 178.9(2) . . ?
O1 U1 O5 91.02(16) . . ?
O2 U1 O5 88.84(16) . . ?
O1 U1 O3 86.93(18) . . ?
O2 U1 O3 94.17(18) . . ?
O5 U1 O3 87.36(15) . . ?
O1 U1 O4 94.26(17) . 2_567 ?
O2 U1 O4 86.10(17) . 2_567 ?
O5 U1 O4 167.21(14) . 2_567 ?
O3 U1 O4 81.30(15) . 2_567 ?
O1 U1 O7 87.23(19) . . ?
O2 U1 O7 91.66(19) . . ?
O5 U1 O7 74.23(15) . . ?
O3 U1 O7 160.57(13) . . ?
O4 U1 O7 117.62(14) 2_567 . ?
O1 U1 O8 85.21(16) . . ?
O2 U1 O8 93.94(16) . . ?
O5 U1 O8 123.99(16) . . ?
O3 U1 O8 147.73(15) . . ?
O4 U1 O8 68.17(16) 2_567 . ?
O7 U1 O8 49.79(14) . . ?
N3 Cu1 N3 180.0 2_666 . ?
N3 Cu1 N2 94.7(2) 2_666 . ?
N3 Cu1 N2 85.3(2) . . ?
N3 Cu1 N2 85.3(2) 2_666 2_666 ?
N3 Cu1 N2 94.7(2) . 2_666 ?
N2 Cu1 N2 180.0(2) . 2_666 ?
C13 O3 U1 125.9(4) . . ?
C13 O4 U1 136.2(4) . 2_567 ?
C14 O5 U1 129.5(4) . . ?
N1 O7 U1 97.3(4) . . ?
N1 O8 U1 97.7(4) . . ?
O9 N1 O8 124.2(6) . . ?
O9 N1 O7 121.5(6) . . ?
O8 N1 O7 114.3(6) . . ?
C15 N2 C19 113.4(5) . 2_666 ?
C15 N2 Cu1 106.0(3) . . ?
C19 N2 Cu1 121.4(4) 2_666 . ?
C15 N2 H2 108(3) . . ?
C19 N2 H2 117(3) 2_666 . ?
Cu1 N2 H2 88(3) . . ?
C16 N3 C17 115.6(6) . . ?
C16 N3 Cu1 107.9(4) . . ?
C17 N3 Cu1 118.3(4) . . ?
C16 N3 H3 106(3) . . ?
C17 N3 H3 110(4) . . ?
Cu1 N3 H3 97(4) . . ?
C6 C1 C2 120.4(6) . . ?
C6 C1 C13 117.8(6) . . ?
C2 C1 C13 121.7(5) . . ?
C3 C2 C1 117.3(5) . . ?
C3 C2 C7 121.8(6) . . ?
C1 C2 C7 120.7(6) . . ?
C4 C3 C2 122.2(6) . . ?
C4 C3 H3A 118.9 . . ?
C2 C3 H3A 118.9 . . ?
C5 C4 C3 120.8(6) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 119.0(6) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C1 C6 C5 120.1(6) . . ?
C1 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C12 C7 C8 119.1(5) . . ?
C12 C7 C2 118.6(6) . . ?
C8 C7 C2 122.3(6) . . ?
C9 C8 C7 120.2(6) . . ?
C9 C8 C14 116.9(7) . . ?
C7 C8 C14 122.9(5) . . ?
C8 C9 C10 119.9(7) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C11 C10 C9 120.3(6) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C10 C11 C12 121.0(7) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C11 C12 C7 119.5(7) . . ?
C11 C12 H12 120.3 . . ?
C7 C12 H12 120.3 . . ?
O4 C13 O3 123.4(6) . . ?
O4 C13 C1 118.5(6) . . ?
O3 C13 C1 118.0(6) . . ?
O6 C14 O5 123.0(7) . . ?
O6 C14 C8 122.7(6) . . ?
O5 C14 C8 114.2(6) . . ?
N2 C15 C16 108.4(5) . . ?
N2 C15 H15A 110.0 . . ?
C16 C15 H15A 110.0 . . ?
N2 C15 H15B 110.0 . . ?
C16 C15 H15B 110.0 . . ?
H15A C15 H15B 108.4 . . ?
N3 C16 C15 108.4(5) . . ?
N3 C16 H16A 110.0 . . ?
C15 C16 H16A 110.0 . . ?
N3 C16 H16B 110.0 . . ?
C15 C16 H16B 110.0 . . ?
H16A C16 H16B 108.4 . . ?
N3 C17 C20 110.9(5) . . ?
N3 C17 C18 107.8(6) . . ?
C20 C17 C18 108.1(5) . . ?
N3 C17 C21 109.1(5) . . ?
C20 C17 C21 109.6(6) . . ?
C18 C17 C21 111.4(6) . . ?
C19 C18 C17 117.8(4) . . ?
C19 C18 H18A 107.9 . . ?
C17 C18 H18A 107.9 . . ?
C19 C18 H18B 107.9 . . ?
C17 C18 H18B 107.9 . . ?
H18A C18 H18B 107.2 . . ?
N2 C19 C18 110.2(5) 2_666 . ?
N2 C19 C22 110.1(5) 2_666 . ?
C18 C19 C22 109.1(4) . . ?
N2 C19 H19 109.1 2_666 . ?
C18 C19 H19 109.1 . . ?
C22 C19 H19 109.1 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N2 H2 O7 0.968(10) 2.033(18) 2.981(7) 166(5) 2_666 yes
N3 H3 O6 0.964(10) 1.98(3) 2.866(7) 151(5) . yes

_refine_diff_density_max         1.546
_refine_diff_density_min         -1.398
_refine_diff_density_rms         0.175

####################################################################### 
# 
# 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 1958811'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2019-10-11 deposited with the CCDC.	2019-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H16 N2 O6 U'
_chemical_formula_weight         666.42

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   9.6615(5)
_cell_length_b                   12.0553(4)
_cell_length_c                   17.6732(8)
_cell_angle_alpha                90
_cell_angle_beta                 92.542(3)
_cell_angle_gamma                90
_cell_volume                     2056.41(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    63892
_cell_measurement_theta_min      2.86
_cell_measurement_theta_max      25.68

_exptl_crystal_description       irregular
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.153
_exptl_crystal_F_000             1256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    7.940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.294
_exptl_absorpt_correction_T_max  0.418
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'two φ and four ω scans with 2° steps (432 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            63892
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.860
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3899
_reflns_number_gt                3311
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms were introduced at calculated
 positions and were treated as riding atoms with an isotropic
 displacement parameter equal to 1.2 times that of the parent atom.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0293P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3899
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0286
_refine_ls_wR_factor_ref         0.0647
_refine_ls_wR_factor_gt          0.0619
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.77901(2) 0.53292(2) 0.32853(2) 0.01910(7) Uani 1 1 d . . . . .
O1 O 0.8939(3) 0.6470(3) 0.33854(15) 0.0227(7) Uani 1 1 d . . . . .
O2 O 0.6667(3) 0.4176(3) 0.31963(15) 0.0230(7) Uani 1 1 d . . . . .
O3 O 0.5860(3) 0.6252(3) 0.24797(15) 0.0231(7) Uani 1 1 d . . . . .
O4 O 0.7686(3) 0.5630(3) 0.19311(16) 0.0281(8) Uani 1 1 d . . . . .
O5 O 0.5402(3) 0.9399(3) 0.24251(15) 0.0230(7) Uani 1 1 d . . . . .
O6 O 0.5375(3) 0.9081(3) 0.12076(15) 0.0232(7) Uani 1 1 d . . . . .
N1 N 0.7454(4) 0.4940(3) 0.47523(19) 0.0209(8) Uani 1 1 d . . . . .
N2 N 0.6373(3) 0.6737(3) 0.40639(18) 0.0195(8) Uani 1 1 d . . . . .
C1 C 0.5859(4) 0.6280(4) 0.1109(2) 0.0184(9) Uani 1 1 d . . . . .
C2 C 0.4558(4) 0.6766(4) 0.0950(2) 0.0201(10) Uani 1 1 d . . . . .
C3 C 0.4092(4) 0.6882(4) 0.0191(2) 0.0229(10) Uani 1 1 d . . . . .
H3 H 0.320452 0.719648 0.007888 0.027 Uiso 1 1 calc R U . . .
C4 C 0.4900(5) 0.6547(4) -0.0401(2) 0.0242(10) Uani 1 1 d . . . . .
H4 H 0.457151 0.664724 -0.091109 0.029 Uiso 1 1 calc R U . . .
C5 C 0.6179(5) 0.6068(4) -0.0244(2) 0.0246(10) Uani 1 1 d . . . . .
H5 H 0.673287 0.583688 -0.064649 0.029 Uiso 1 1 calc R U . . .
C6 C 0.6648(4) 0.5926(4) 0.0491(2) 0.0228(10) Uani 1 1 d . . . . .
H6 H 0.752110 0.558220 0.059271 0.027 Uiso 1 1 calc R U . . .
C7 C 0.3560(4) 0.7132(4) 0.1530(2) 0.0189(10) Uani 1 1 d . . . . .
C8 C 0.3713(4) 0.8119(4) 0.1943(2) 0.0199(9) Uani 1 1 d . . . . .
C9 C 0.2688(4) 0.8422(4) 0.2440(2) 0.0225(10) Uani 1 1 d . . . . .
H9 H 0.280762 0.907511 0.273676 0.027 Uiso 1 1 calc R U . . .
C10 C 0.1515(4) 0.7792(4) 0.2506(2) 0.0233(10) Uani 1 1 d . . . . .
H10 H 0.081097 0.802810 0.282847 0.028 Uiso 1 1 calc R U . . .
C11 C 0.1361(4) 0.6817(4) 0.2103(2) 0.0235(10) Uani 1 1 d . . . . .
H11 H 0.056053 0.637070 0.215503 0.028 Uiso 1 1 calc R U . . .
C12 C 0.2386(4) 0.6488(4) 0.1617(2) 0.0218(10) Uani 1 1 d . . . . .
H12 H 0.227909 0.581432 0.134201 0.026 Uiso 1 1 calc R U . . .
C13 C 0.6485(4) 0.6048(4) 0.1879(2) 0.0218(10) Uani 1 1 d . . . . .
C14 C 0.4889(4) 0.8896(4) 0.1854(2) 0.0223(10) Uani 1 1 d . . . . .
C15 C 0.8009(5) 0.4035(4) 0.5091(2) 0.0262(11) Uani 1 1 d . . . . .
H15 H 0.862754 0.359418 0.481562 0.031 Uiso 1 1 calc R U . . .
C16 C 0.7725(5) 0.3708(4) 0.5829(2) 0.0281(11) Uani 1 1 d . . . . .
H16 H 0.815848 0.307097 0.604889 0.034 Uiso 1 1 calc R U . . .
C17 C 0.6807(4) 0.4325(4) 0.6231(2) 0.0251(11) Uani 1 1 d . . . . .
H17 H 0.656846 0.410802 0.672494 0.030 Uiso 1 1 calc R U . . .
C18 C 0.6240(5) 0.5272(4) 0.5893(2) 0.0231(11) Uani 1 1 d . . . . .
H18 H 0.562728 0.572731 0.616241 0.028 Uiso 1 1 calc R U . . .
C19 C 0.6573(4) 0.5552(4) 0.5158(2) 0.0181(9) Uani 1 1 d . . . . .
C20 C 0.6033(4) 0.6571(4) 0.4795(2) 0.0218(10) Uani 1 1 d . . . . .
C21 C 0.5295(4) 0.7382(4) 0.5180(2) 0.0240(10) Uani 1 1 d . . . . .
H21 H 0.500545 0.724052 0.567772 0.029 Uiso 1 1 calc R U . . .
C22 C 0.4990(5) 0.8385(4) 0.4835(2) 0.0276(11) Uani 1 1 d . . . . .
H22 H 0.451121 0.894641 0.509602 0.033 Uiso 1 1 calc R U . . .
C23 C 0.5391(4) 0.8559(4) 0.4106(2) 0.0252(10) Uani 1 1 d . . . . .
H23 H 0.520723 0.924689 0.385893 0.030 Uiso 1 1 calc R U . . .
C24 C 0.6065(5) 0.7719(4) 0.3740(2) 0.0242(10) Uani 1 1 d . . . . .
H24 H 0.632294 0.784149 0.323437 0.029 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 1.766(3) . ?
U1 O1 1.771(3) . ?
U1 O4 2.418(3) . ?
U1 O6 2.463(3) 2_645 ?
U1 O5 2.466(3) 2_645 ?
U1 O3 2.551(3) . ?
U1 N2 2.611(3) . ?
U1 N1 2.668(3) . ?
O3 C13 1.268(5) . ?
O4 C13 1.265(5) . ?
O5 C14 1.260(5) . ?
O6 C14 1.275(5) . ?
N1 C15 1.345(6) . ?
N1 C19 1.355(6) . ?
N2 C24 1.342(6) . ?
N2 C20 1.361(5) . ?
C1 C2 1.404(6) . ?
C1 C6 1.424(6) . ?
C1 C13 1.492(6) . ?
C2 C3 1.403(5) . ?
C2 C7 1.504(6) . ?
C3 C4 1.394(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.381(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.368(6) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.388(6) . ?
C7 C8 1.400(6) . ?
C8 C9 1.401(6) . ?
C8 C14 1.486(6) . ?
C9 C10 1.374(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.380(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.397(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C15 C16 1.401(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.378(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.390(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.394(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.471(6) . ?
C20 C21 1.404(6) . ?
C21 C22 1.380(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.378(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.380(6) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U1 O1 178.89(13) . . ?
O2 U1 O4 91.79(12) . . ?
O1 U1 O4 88.90(12) . . ?
O2 U1 O6 88.89(12) . 2_645 ?
O1 U1 O6 90.03(12) . 2_645 ?
O4 U1 O6 116.69(10) . 2_645 ?
O2 U1 O5 92.43(12) . 2_645 ?
O1 U1 O5 87.10(12) . 2_645 ?
O4 U1 O5 64.12(10) . 2_645 ?
O6 U1 O5 52.61(9) 2_645 2_645 ?
O2 U1 O3 82.12(12) . . ?
O1 U1 O3 98.98(12) . . ?
O4 U1 O3 52.05(9) . . ?
O6 U1 O3 165.00(10) 2_645 . ?
O5 U1 O3 115.53(9) 2_645 . ?
O2 U1 N2 102.98(12) . . ?
O1 U1 N2 77.49(12) . . ?
O4 U1 N2 115.12(11) . . ?
O6 U1 N2 126.23(10) 2_645 . ?
O5 U1 N2 164.59(11) 2_645 . ?
O3 U1 N2 67.86(9) . . ?
O2 U1 N1 81.24(12) . . ?
O1 U1 N1 98.17(12) . . ?
O4 U1 N1 170.51(11) . . ?
O6 U1 N1 69.86(10) 2_645 . ?
O5 U1 N1 122.28(10) 2_645 . ?
O3 U1 N1 120.10(10) . . ?
N2 U1 N1 60.85(11) . . ?
C13 O3 U1 91.1(2) . . ?
C13 O4 U1 97.4(2) . . ?
C14 O5 U1 94.2(2) . 2_655 ?
C14 O6 U1 94.0(3) . 2_655 ?
C15 N1 C19 117.0(4) . . ?
C15 N1 U1 120.8(3) . . ?
C19 N1 U1 121.6(3) . . ?
C24 N2 C20 118.4(4) . . ?
C24 N2 U1 117.4(3) . . ?
C20 N2 U1 124.0(3) . . ?
C2 C1 C6 118.5(4) . . ?
C2 C1 C13 125.7(4) . . ?
C6 C1 C13 115.7(4) . . ?
C3 C2 C1 118.6(4) . . ?
C3 C2 C7 115.7(4) . . ?
C1 C2 C7 125.6(4) . . ?
C4 C3 C2 121.5(4) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C5 C4 C3 119.8(4) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C6 C5 C4 119.9(4) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C1 121.7(4) . . ?
C5 C6 H6 119.2 . . ?
C1 C6 H6 119.2 . . ?
C12 C7 C8 119.0(4) . . ?
C12 C7 C2 117.6(4) . . ?
C8 C7 C2 123.2(4) . . ?
C7 C8 C9 119.2(4) . . ?
C7 C8 C14 123.0(4) . . ?
C9 C8 C14 117.8(4) . . ?
C10 C9 C8 121.2(4) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C9 C10 C11 119.8(4) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C10 C11 C12 119.7(4) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C7 C12 C11 121.0(4) . . ?
C7 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
O4 C13 O3 119.1(4) . . ?
O4 C13 C1 118.3(4) . . ?
O3 C13 C1 122.6(4) . . ?
O5 C14 O6 119.1(4) . . ?
O5 C14 C8 119.7(4) . . ?
O6 C14 C8 121.2(4) . . ?
N1 C15 C16 123.5(4) . . ?
N1 C15 H15 118.2 . . ?
C16 C15 H15 118.2 . . ?
C17 C16 C15 119.0(5) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
C16 C17 C18 118.2(4) . . ?
C16 C17 H17 120.9 . . ?
C18 C17 H17 120.9 . . ?
C17 C18 C19 119.7(4) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
N1 C19 C18 122.5(4) . . ?
N1 C19 C20 116.3(4) . . ?
C18 C19 C20 121.1(4) . . ?
N2 C20 C21 120.5(4) . . ?
N2 C20 C19 116.1(4) . . ?
C21 C20 C19 123.2(4) . . ?
C22 C21 C20 119.9(4) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C23 C22 C21 118.9(4) . . ?
C23 C22 H22 120.6 . . ?
C21 C22 H22 120.6 . . ?
C22 C23 C24 119.0(5) . . ?
C22 C23 H23 120.5 . . ?
C24 C23 H23 120.5 . . ?
N2 C24 C23 123.2(4) . . ?
N2 C24 H24 118.4 . . ?
C23 C24 H24 118.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C15 H15 O6 0.95 2.17 2.833(5) 126.1 2_645 yes
C18 H18 O2 0.95 2.54 3.365(5) 145.7 3_666 yes
C23 H23 O5 0.95 2.56 3.139(5) 119.8 . yes
C24 H24 O3 0.95 2.37 2.844(5) 110.7 . yes
C24 H24 O5 0.95 2.50 3.127(5) 123.6 . yes

_refine_diff_density_max         1.910
_refine_diff_density_min         -1.608
_refine_diff_density_rms         0.186

####################################################################### 
# 
# 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 1958812'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2019-10-11 deposited with the CCDC.	2019-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H16 N2 O6 U'
_chemical_formula_weight         690.44

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   9.9607(4)
_cell_length_b                   11.8944(9)
_cell_length_c                   18.5400(16)
_cell_angle_alpha                90
_cell_angle_beta                 96.404(4)
_cell_angle_gamma                90
_cell_volume                     2182.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    116607
_cell_measurement_theta_min      2.80
_cell_measurement_theta_max      25.68

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.101
_exptl_crystal_F_000             1304
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    7.484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.245
_exptl_absorpt_correction_T_max  0.378
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'2 φ and 12 ω scans with 2° steps (782 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            116607
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.797
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4137
_reflns_number_gt                3322
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms were introduced at calculated
 positions and were treated as riding atoms with an isotropic
 displacement parameter equal to 1.2 times that of the parent atom.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0376P)²+0.0773P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4137
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0314
_refine_ls_wR_factor_ref         0.0696
_refine_ls_wR_factor_gt          0.0660
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.30206(2) 0.95154(2) 0.32250(2) 0.02623(8) Uani 1 1 d . . . . .
O1 O 0.4164(3) 0.8395(3) 0.33818(17) 0.0285(8) Uani 1 1 d . . . . .
O2 O 0.1912(3) 1.0669(3) 0.30725(18) 0.0282(8) Uani 1 1 d . . . . .
O3 O 0.4734(3) 1.0869(3) 0.37593(19) 0.0310(9) Uani 1 1 d . . . . .
O4 O 0.4721(3) 1.0497(3) 0.26049(18) 0.0279(8) Uani 1 1 d . . . . .
O5 O 0.2093(3) 1.4186(3) 0.30780(19) 0.0326(9) Uani 1 1 d . . . . .
O6 O 0.3820(3) 1.3524(3) 0.25713(17) 0.0314(8) Uani 1 1 d . . . . .
N1 N 0.1607(4) 0.8112(4) 0.3936(2) 0.0257(10) Uani 1 1 d . . . . .
N2 N 0.2712(4) 0.9973(4) 0.4615(2) 0.0285(10) Uani 1 1 d . . . . .
C1 C 0.6206(5) 1.1954(4) 0.3076(3) 0.0257(11) Uani 1 1 d . . . . .
C2 C 0.6285(5) 1.2948(5) 0.3470(3) 0.0286(12) Uani 1 1 d . . . . .
C3 C 0.7322(5) 1.3708(5) 0.3364(3) 0.0328(13) Uani 1 1 d . . . . .
H3 H 0.738089 1.439611 0.362626 0.039 Uiso 1 1 calc R U . . .
C4 C 0.8259(5) 1.3479(5) 0.2888(3) 0.0333(13) Uani 1 1 d . . . . .
H4 H 0.896245 1.399939 0.282901 0.040 Uiso 1 1 calc R U . . .
C5 C 0.8165(5) 1.2489(5) 0.2498(3) 0.0308(12) Uani 1 1 d . . . . .
H5 H 0.880300 1.232659 0.216774 0.037 Uiso 1 1 calc R U . . .
C6 C 0.7143(5) 1.1731(5) 0.2587(3) 0.0299(12) Uani 1 1 d . . . . .
H6 H 0.707736 1.105452 0.231305 0.036 Uiso 1 1 calc R U . . .
C7 C 0.5361(5) 1.3251(4) 0.4033(3) 0.0273(12) Uani 1 1 d . . . . .
C8 C 0.4013(5) 1.3610(5) 0.3881(3) 0.0278(11) Uani 1 1 d . . . . .
C9 C 0.3300(5) 1.3904(4) 0.4464(3) 0.0276(12) Uani 1 1 d . . . . .
H9 H 0.239195 1.415358 0.436590 0.033 Uiso 1 1 calc R U . . .
C10 C 0.3869(5) 1.3844(5) 0.5174(3) 0.0332(13) Uani 1 1 d . . . . .
H10 H 0.335496 1.403603 0.555812 0.040 Uiso 1 1 calc R U . . .
C11 C 0.5196(5) 1.3502(5) 0.5321(3) 0.0326(12) Uani 1 1 d . . . . .
H11 H 0.560406 1.346145 0.580883 0.039 Uiso 1 1 calc R U . . .
C12 C 0.5936(5) 1.3216(5) 0.4753(3) 0.0320(13) Uani 1 1 d . . . . .
H12 H 0.685296 1.299348 0.485893 0.038 Uiso 1 1 calc R U . . .
C13 C 0.5177(5) 1.1077(5) 0.3157(3) 0.0269(12) Uani 1 1 d . . . . .
C14 C 0.3267(5) 1.3768(5) 0.3138(3) 0.0284(12) Uani 1 1 d . . . . .
C15 C 0.1258(5) 0.7113(5) 0.3650(3) 0.0308(13) Uani 1 1 d . . . . .
H15 H 0.155034 0.692112 0.319562 0.037 Uiso 1 1 calc R U . . .
C16 C 0.0476(5) 0.6328(5) 0.3989(3) 0.0334(13) Uani 1 1 d . . . . .
H16 H 0.026456 0.561484 0.377510 0.040 Uiso 1 1 calc R U . . .
C17 C 0.0027(5) 0.6622(5) 0.4638(3) 0.0325(13) Uani 1 1 d . . . . .
H17 H -0.054276 0.612541 0.486605 0.039 Uiso 1 1 calc R U . . .
C18 C 0.0406(5) 0.7647(5) 0.4962(3) 0.0283(12) Uani 1 1 d . . . . .
C19 C 0.1241(5) 0.8366(5) 0.4604(2) 0.0263(12) Uani 1 1 d . . . . .
C20 C 0.1788(5) 0.9359(4) 0.4951(3) 0.0257(12) Uani 1 1 d . . . . .
C21 C 0.1432(5) 0.9640(4) 0.5642(3) 0.0275(12) Uani 1 1 d . . . . .
C22 C 0.0500(5) 0.8948(5) 0.5977(3) 0.0311(13) Uani 1 1 d . . . . .
H22 H 0.021991 0.916494 0.643057 0.037 Uiso 1 1 calc R U . . .
C23 C 0.0017(5) 0.7991(5) 0.5655(3) 0.0321(13) Uani 1 1 d . . . . .
H23 H -0.058947 0.753633 0.588784 0.039 Uiso 1 1 calc R U . . .
C24 C 0.2038(5) 1.0603(5) 0.5986(3) 0.0309(12) Uani 1 1 d . . . . .
H24 H 0.181067 1.082725 0.644908 0.037 Uiso 1 1 calc R U . . .
C25 C 0.2941(5) 1.1203(4) 0.5653(3) 0.0281(12) Uani 1 1 d . . . . .
H25 H 0.335690 1.185091 0.587910 0.034 Uiso 1 1 calc R U . . .
C26 C 0.3258(5) 1.0858(5) 0.4967(3) 0.0303(12) Uani 1 1 d . . . . .
H26 H 0.390300 1.128494 0.474336 0.036 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.756(3) . ?
U1 O2 1.764(3) . ?
U1 O5 2.438(3) 2_545 ?
U1 O4 2.447(3) . ?
U1 O3 2.472(4) . ?
U1 O6 2.516(3) 2_545 ?
U1 N1 2.631(4) . ?
U1 N2 2.684(4) . ?
O3 C13 1.270(6) . ?
O4 C13 1.275(6) . ?
O5 C14 1.265(6) . ?
O6 C14 1.272(6) . ?
N1 C15 1.331(7) . ?
N1 C19 1.363(6) . ?
N2 C26 1.324(7) . ?
N2 C20 1.377(6) . ?
C1 C2 1.387(7) . ?
C1 C6 1.397(7) . ?
C1 C13 1.481(7) . ?
C2 C3 1.403(7) . ?
C2 C7 1.511(7) . ?
C3 C4 1.382(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.383(7) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.393(7) . ?
C7 C8 1.408(7) . ?
C8 C9 1.403(7) . ?
C8 C14 1.502(7) . ?
C9 C10 1.375(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.382(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.393(7) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C15 C16 1.408(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.375(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.392(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.409(7) . ?
C18 C23 1.442(7) . ?
C19 C20 1.424(7) . ?
C20 C21 1.406(7) . ?
C21 C24 1.413(7) . ?
C21 C22 1.434(7) . ?
C22 C23 1.349(8) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C25 1.351(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.405(7) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 178.34(16) . . ?
O1 U1 O5 89.98(14) . 2_545 ?
O2 U1 O5 90.40(14) . 2_545 ?
O1 U1 O4 88.29(13) . . ?
O2 U1 O4 90.42(14) . . ?
O5 U1 O4 64.48(12) 2_545 . ?
O1 U1 O3 91.28(15) . . ?
O2 U1 O3 87.11(15) . . ?
O5 U1 O3 117.10(11) 2_545 . ?
O4 U1 O3 52.72(11) . . ?
O1 U1 O6 99.08(14) . 2_545 ?
O2 U1 O6 82.42(15) . 2_545 ?
O5 U1 O6 52.61(11) 2_545 2_545 ?
O4 U1 O6 116.44(11) . 2_545 ?
O3 U1 O6 165.02(12) . 2_545 ?
O1 U1 N1 78.97(14) . . ?
O2 U1 N1 102.31(14) . . ?
O5 U1 N1 115.25(12) 2_545 . ?
O4 U1 N1 167.26(12) . . ?
O3 U1 N1 126.63(12) . . ?
O6 U1 N1 66.49(11) 2_545 . ?
O1 U1 N2 97.85(14) . . ?
O2 U1 N2 81.93(14) . . ?
O5 U1 N2 170.48(12) 2_545 . ?
O4 U1 N2 120.90(13) . . ?
O3 U1 N2 68.36(12) . . ?
O6 U1 N2 120.29(12) 2_545 . ?
N1 U1 N2 61.48(13) . . ?
C13 O3 U1 93.8(3) . . ?
C13 O4 U1 94.9(3) . . ?
C14 O5 U1 95.2(3) . 2 ?
C14 O6 U1 91.3(3) . 2 ?
C15 N1 C19 118.4(4) . . ?
C15 N1 U1 119.8(3) . . ?
C19 N1 U1 121.8(3) . . ?
C26 N2 C20 117.2(4) . . ?
C26 N2 U1 123.4(3) . . ?
C20 N2 U1 118.8(3) . . ?
C2 C1 C6 120.0(5) . . ?
C2 C1 C13 123.1(4) . . ?
C6 C1 C13 116.9(5) . . ?
C1 C2 C3 118.4(5) . . ?
C1 C2 C7 124.3(5) . . ?
C3 C2 C7 117.2(5) . . ?
C4 C3 C2 121.5(5) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C5 C4 C3 119.5(5) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 120.1(5) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C1 120.5(5) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
C12 C7 C8 118.8(5) . . ?
C12 C7 C2 116.0(4) . . ?
C8 C7 C2 125.0(4) . . ?
C9 C8 C7 118.3(5) . . ?
C9 C8 C14 115.8(4) . . ?
C7 C8 C14 125.8(4) . . ?
C10 C9 C8 122.4(5) . . ?
C10 C9 H9 118.8 . . ?
C8 C9 H9 118.8 . . ?
C9 C10 C11 119.2(5) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
C10 C11 C12 119.8(5) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C7 C12 C11 121.4(5) . . ?
C7 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
O3 C13 O4 118.2(5) . . ?
O3 C13 C1 122.6(5) . . ?
O4 C13 C1 119.2(4) . . ?
O5 C14 O6 119.9(4) . . ?
O5 C14 C8 119.1(4) . . ?
O6 C14 C8 120.9(4) . . ?
N1 C15 C16 123.2(5) . . ?
N1 C15 H15 118.4 . . ?
C16 C15 H15 118.4 . . ?
C17 C16 C15 118.2(5) . . ?
C17 C16 H16 120.9 . . ?
C15 C16 H16 120.9 . . ?
C16 C17 C18 120.0(5) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C17 C18 C19 118.4(5) . . ?
C17 C18 C23 123.0(5) . . ?
C19 C18 C23 118.6(5) . . ?
N1 C19 C18 121.6(5) . . ?
N1 C19 C20 117.8(4) . . ?
C18 C19 C20 120.5(4) . . ?
N2 C20 C21 122.4(5) . . ?
N2 C20 C19 118.5(4) . . ?
C21 C20 C19 119.0(5) . . ?
C20 C21 C24 117.7(5) . . ?
C20 C21 C22 120.0(5) . . ?
C24 C21 C22 122.2(5) . . ?
C23 C22 C21 120.5(5) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C22 C23 C18 121.1(5) . . ?
C22 C23 H23 119.4 . . ?
C18 C23 H23 119.4 . . ?
C25 C24 C21 119.6(5) . . ?
C25 C24 H24 120.2 . . ?
C21 C24 H24 120.2 . . ?
C24 C25 C26 119.2(5) . . ?
C24 C25 H25 120.4 . . ?
C26 C25 H25 120.4 . . ?
N2 C26 C25 123.9(5) . . ?
N2 C26 H26 118.0 . . ?
C25 C26 H26 118.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C15 H15 O4 0.95 2.50 3.091(6) 120.3 2_545 yes
C16 H16 O4 0.95 2.56 3.101(6) 116.1 2_545 yes
C26 H26 O3 0.95 2.14 2.813(6) 126.3 . yes

_refine_diff_density_max         0.893
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.130

####################################################################### 
# 
# 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_9
_database_code_depnum_ccdc_archive 'CCDC 1958818'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2019-10-11 deposited with the CCDC.	2019-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H84 Cu N4 O30 U3'
_chemical_formula_weight         2263.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.6248(9)
_cell_length_b                   13.5485(10)
_cell_length_c                   15.1649(16)
_cell_angle_alpha                88.758(6)
_cell_angle_beta                 78.287(5)
_cell_angle_gamma                82.984(6)
_cell_volume                     1921.8(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    95479
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light purple'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_F_000             1089
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    6.661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.423
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'2 φ and 11 ω scans with 2° steps (744 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            95479
_diffrn_reflns_av_unetI/netI     0.0963
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.327
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7291
_reflns_number_gt                5402
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms bound to O and N atoms were
 found on a difference Fourier map, except for those of two free
 water molecules (O14 and O15), and they were refined with restraints
 on bond lengths and angles, and with an isotropic displacement
 parameter equal to 1.2 (NH) or 1.5 (H2O) times that of the parent atom.
 The C-bound H atoms were introduced at calculated positions and were
 treated as riding atoms with an isotropic displacement parameter equal
 to 1.2 times that of the parent atom (1.5 for CH₃, with optimized
 geometry).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0303P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7291
_refine_ls_number_parameters     520
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.0880
_refine_ls_wR_factor_gt          0.0816
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U -0.03458(2) 0.40447(2) 0.35612(2) 0.02360(9) Uani 1 1 d . . . . .
U2 U 0.500000 0.000000 0.000000 0.03088(11) Uani 1 2 d S . P . .
Cu1 Cu 0.000000 0.000000 0.500000 0.0247(3) Uani 1 2 d S . P . .
O1 O 0.1355(5) 0.3564(3) 0.3751(3) 0.0337(12) Uani 1 1 d . . . . .
O2 O -0.2002(4) 0.4580(3) 0.3351(3) 0.0292(12) Uani 1 1 d . . . . .
O3 O 0.5315(5) -0.0343(4) 0.1091(3) 0.0374(13) Uani 1 1 d . . . . .
O4 O 0.0042(5) 0.3149(4) 0.2104(3) 0.0330(12) Uani 1 1 d . . . . .
O5 O 0.0734(5) 0.4633(4) 0.2085(3) 0.0313(12) Uani 1 1 d . . . . .
O6 O 0.3715(5) 0.1618(4) 0.0575(3) 0.0373(13) Uani 1 1 d . . . . .
O7 O 0.6050(5) 0.1515(4) 0.0185(4) 0.0390(13) Uani 1 1 d . . . . .
O8 O -0.1374(4) 0.4076(3) 0.5112(3) 0.0259(11) Uani 1 1 d . . . . .
O9 O -0.0171(4) 0.4377(3) 0.6166(3) 0.0259(11) Uani 1 1 d . . . . .
O10 O -0.0988(4) 0.2407(3) 0.3900(3) 0.0242(11) Uani 1 1 d . . . . .
O11 O -0.1739(4) 0.1465(3) 0.5084(3) 0.0266(11) Uani 1 1 d . . . . .
O12 O 0.7586(5) -0.0006(4) -0.0606(4) 0.0448(15) Uani 1 1 d D . . . .
H12A H 0.816(6) -0.051(3) -0.078(6) 0.067 Uiso 1 1 d D U . . .
H12B H 0.808(6) 0.047(3) -0.059(6) 0.067 Uiso 1 1 d D U . . .
O13 O 0.0084(6) 0.1363(5) 0.1235(4) 0.0492(15) Uani 1 1 d D . . . .
H13A H 0.004(8) 0.188(4) 0.153(5) 0.074 Uiso 1 1 d D U . . .
H13B H -0.062(6) 0.107(5) 0.146(5) 0.074 Uiso 1 1 d D U . . .
O14 O 0.8001(6) 0.0097(6) 0.1583(4) 0.077(2) Uani 1 1 d . . . . .
O15 O 0.9790(7) 0.1275(4) -0.0525(4) 0.072(2) Uani 1 1 d . . . . .
N1 N -0.1270(5) -0.0586(4) 0.6057(4) 0.0263(14) Uani 1 1 d D . . . .
H1 H -0.056(5) -0.113(3) 0.612(4) 0.032 Uiso 1 1 d D U . . .
N2 N 0.0647(5) 0.0788(4) 0.5946(4) 0.0247(13) Uani 1 1 d D . . . .
H2 H -0.005(5) 0.135(3) 0.586(4) 0.030 Uiso 1 1 d D U . . .
C1 C 0.1157(7) 0.3752(5) 0.0678(5) 0.0304(17) Uani 1 1 d . . . . .
C2 C 0.2619(8) 0.3703(5) 0.0301(5) 0.0327(18) Uani 1 1 d . . . . .
C3 C 0.3041(8) 0.3569(5) -0.0626(5) 0.041(2) Uani 1 1 d . . . . .
H3 H 0.403112 0.348196 -0.088929 0.049 Uiso 1 1 calc R U . . .
C4 C 0.2049(9) 0.3558(6) -0.1178(6) 0.046(2) Uani 1 1 d . . . . .
H4 H 0.236212 0.349079 -0.181146 0.056 Uiso 1 1 calc R U . . .
C5 C 0.0606(9) 0.3645(6) -0.0797(5) 0.043(2) Uani 1 1 d . . . . .
H5 H -0.008405 0.366264 -0.116633 0.051 Uiso 1 1 calc R U . . .
C6 C 0.0181(8) 0.3706(5) 0.0136(5) 0.0372(19) Uani 1 1 d . . . . .
H6 H -0.080243 0.371489 0.040316 0.045 Uiso 1 1 calc R U . . .
C7 C 0.3733(8) 0.3793(6) 0.0851(5) 0.0348(18) Uani 1 1 d . . . . .
C8 C 0.4824(7) 0.3019(5) 0.0904(5) 0.0329(18) Uani 1 1 d . . . . .
C9 C 0.5905(8) 0.3157(6) 0.1357(5) 0.040(2) Uani 1 1 d . . . . .
H9 H 0.665951 0.263755 0.136708 0.047 Uiso 1 1 calc R U . . .
C10 C 0.5889(8) 0.4047(7) 0.1793(5) 0.046(2) Uani 1 1 d . . . . .
H10 H 0.660965 0.413482 0.211905 0.056 Uiso 1 1 calc R U . . .
C11 C 0.4788(8) 0.4817(6) 0.1745(5) 0.040(2) Uani 1 1 d . . . . .
H11 H 0.475924 0.543012 0.204392 0.048 Uiso 1 1 calc R U . . .
C12 C 0.3752(7) 0.4686(6) 0.1266(5) 0.039(2) Uani 1 1 d . . . . .
H12 H 0.303469 0.522120 0.122152 0.047 Uiso 1 1 calc R U . . .
C13 C 0.0648(7) 0.3864(6) 0.1670(5) 0.0303(17) Uani 1 1 d . . . . .
C14 C 0.4847(8) 0.2022(6) 0.0533(5) 0.0368(19) Uani 1 1 d . . . . .
C15 C -0.2066(6) 0.3352(5) 0.6555(4) 0.0233(15) Uani 1 1 d . . . . .
C16 C -0.3333(7) 0.3019(5) 0.6403(5) 0.0257(16) Uani 1 1 d . . . . .
C17 C -0.4070(7) 0.2480(5) 0.7103(5) 0.0282(17) Uani 1 1 d . . . . .
H17 H -0.492540 0.224367 0.702174 0.034 Uiso 1 1 calc R U . . .
C18 C -0.3635(7) 0.2272(5) 0.7899(5) 0.0316(17) Uani 1 1 d . . . . .
H18 H -0.416494 0.188648 0.834603 0.038 Uiso 1 1 calc R U . . .
C19 C -0.2410(7) 0.2631(5) 0.8046(5) 0.0326(18) Uani 1 1 d . . . . .
H19 H -0.210018 0.250766 0.859863 0.039 Uiso 1 1 calc R U . . .
C20 C -0.1653(7) 0.3171(5) 0.7374(5) 0.0295(17) Uani 1 1 d . . . . .
H20 H -0.082232 0.342655 0.747460 0.035 Uiso 1 1 calc R U . . .
C21 C -0.3978(6) 0.3201(5) 0.5588(5) 0.0224(15) Uani 1 1 d . . . . .
C22 C -0.3380(6) 0.2810(5) 0.4754(5) 0.0212(15) Uani 1 1 d . . . . .
C23 C -0.4064(6) 0.2993(5) 0.4027(5) 0.0260(16) Uani 1 1 d . . . . .
H23 H -0.361981 0.272594 0.345039 0.031 Uiso 1 1 calc R U . . .
C24 C -0.5396(6) 0.3565(5) 0.4145(5) 0.0266(16) Uani 1 1 d . . . . .
H24 H -0.587441 0.368515 0.365663 0.032 Uiso 1 1 calc R U . . .
C25 C -0.5995(6) 0.3948(5) 0.4979(5) 0.0277(17) Uani 1 1 d . . . . .
H25 H -0.690906 0.432855 0.507287 0.033 Uiso 1 1 calc R U . . .
C26 C -0.5301(7) 0.3794(5) 0.5686(5) 0.0245(16) Uani 1 1 d . . . . .
H26 H -0.572622 0.409410 0.625234 0.029 Uiso 1 1 calc R U . . .
C27 C -0.1168(7) 0.3971(5) 0.5906(5) 0.0257(16) Uani 1 1 d . . . . .
C28 C -0.1928(7) 0.2177(5) 0.4578(5) 0.0265(17) Uani 1 1 d . . . . .
C29 C -0.1342(7) 0.0078(5) 0.6838(5) 0.0289(17) Uani 1 1 d . . . . .
H29A H -0.170153 -0.026313 0.740788 0.035 Uiso 1 1 calc R U . . .
H29B H -0.199741 0.069165 0.679579 0.035 Uiso 1 1 calc R U . . .
C30 C 0.0134(7) 0.0328(6) 0.6819(5) 0.0319(17) Uani 1 1 d . . . . .
H30A H 0.012261 0.079426 0.731431 0.038 Uiso 1 1 calc R U . . .
H30B H 0.077563 -0.028268 0.689690 0.038 Uiso 1 1 calc R U . . .
C31 C 0.2132(7) 0.1104(5) 0.5817(5) 0.0289(17) Uani 1 1 d . . . . .
C32 C 0.2541(7) 0.1505(5) 0.4860(5) 0.0315(18) Uani 1 1 d . . . . .
H32A H 0.181263 0.206712 0.478867 0.038 Uiso 1 1 calc R U . . .
H32B H 0.345947 0.178177 0.481084 0.038 Uiso 1 1 calc R U . . .
C33 C 0.2700(6) 0.0797(5) 0.4062(5) 0.0264(16) Uani 1 1 d . . . . .
H33 H 0.324100 0.015615 0.420429 0.032 Uiso 1 1 calc R U . . .
C34 C 0.3204(7) 0.0223(5) 0.5990(5) 0.0373(19) Uani 1 1 d . . . . .
H34A H 0.300304 0.004961 0.663015 0.056 Uiso 1 1 calc R U . . .
H34B H 0.417628 0.040682 0.582072 0.056 Uiso 1 1 calc R U . . .
H34C H 0.311666 -0.034892 0.562925 0.056 Uiso 1 1 calc R U . . .
C35 C 0.2123(7) 0.1952(5) 0.6480(5) 0.0339(18) Uani 1 1 d . . . . .
H35A H 0.138328 0.249432 0.640428 0.051 Uiso 1 1 calc R U . . .
H35B H 0.305828 0.219943 0.635743 0.051 Uiso 1 1 calc R U . . .
H35C H 0.192066 0.170301 0.709825 0.051 Uiso 1 1 calc R U . . .
C36 C 0.3570(7) 0.1228(6) 0.3233(5) 0.0356(19) Uani 1 1 d . . . . .
H36A H 0.382409 0.072557 0.275335 0.053 Uiso 1 1 calc R U . . .
H36B H 0.444388 0.142725 0.337712 0.053 Uiso 1 1 calc R U . . .
H36C H 0.300793 0.180927 0.303119 0.053 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 1.756(4) . ?
U1 O1 1.763(4) . ?
U1 O9 2.318(4) 2_566 ?
U1 O8 2.359(4) . ?
U1 O10 2.393(5) . ?
U1 O5 2.430(5) . ?
U1 O4 2.483(5) . ?
U2 O3 1.784(5) . ?
U2 O3 1.784(5) 2_655 ?
U2 O7 2.441(5) 2_655 ?
U2 O7 2.441(5) . ?
U2 O6 2.466(5) . ?
U2 O6 2.466(4) 2_655 ?
U2 O12 2.471(5) . ?
U2 O12 2.471(5) 2_655 ?
Cu1 N1 2.020(6) . ?
Cu1 N1 2.020(6) 2_556 ?
Cu1 N2 2.043(5) . ?
Cu1 N2 2.043(5) 2_556 ?
Cu1 O11 2.423(4) 2_556 ?
Cu1 O11 2.423(4) . ?
O4 C13 1.291(8) . ?
O5 C13 1.249(8) . ?
O6 C14 1.268(8) . ?
O7 C14 1.290(8) . ?
O8 C27 1.261(8) . ?
O9 C27 1.293(8) . ?
O10 C28 1.285(8) . ?
O11 C28 1.238(8) . ?
O12 H12A 0.839(10) . ?
O12 H12B 0.842(10) . ?
O13 H13A 0.838(10) . ?
O13 H13B 0.837(10) . ?
N1 C33 1.486(8) 2_556 ?
N1 C29 1.488(8) . ?
N1 H1 0.962(10) . ?
N2 C30 1.470(9) . ?
N2 C31 1.516(8) . ?
N2 H2 0.971(10) . ?
C1 C6 1.376(9) . ?
C1 C2 1.401(9) . ?
C1 C13 1.489(10) . ?
C2 C3 1.391(10) . ?
C2 C7 1.503(10) . ?
C3 C4 1.392(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.391(10) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.379(10) . ?
C7 C8 1.404(10) . ?
C8 C9 1.390(10) . ?
C8 C14 1.470(10) . ?
C9 C10 1.384(10) . ?
C9 H9 0.9500 . ?
C10 C11 1.405(10) . ?
C10 H10 0.9500 . ?
C11 C12 1.377(10) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C15 C20 1.387(9) . ?
C15 C16 1.413(8) . ?
C15 C27 1.488(10) . ?
C16 C17 1.396(10) . ?
C16 C21 1.494(9) . ?
C17 C18 1.369(10) . ?
C17 H17 0.9500 . ?
C18 C19 1.388(9) . ?
C18 H18 0.9500 . ?
C19 C20 1.379(10) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.367(9) . ?
C21 C26 1.403(8) . ?
C22 C23 1.398(9) . ?
C22 C28 1.525(8) . ?
C23 C24 1.396(8) . ?
C23 H23 0.9500 . ?
C24 C25 1.364(9) . ?
C24 H24 0.9500 . ?
C25 C26 1.373(9) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C29 C30 1.494(9) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.531(10) . ?
C31 C34 1.533(9) . ?
C31 C35 1.541(9) . ?
C32 C33 1.533(9) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C36 1.510(9) . ?
C33 H33 1.0000 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U1 O1 177.0(2) . . ?
O2 U1 O9 88.92(17) . 2_566 ?
O1 U1 O9 88.54(18) . 2_566 ?
O2 U1 O8 88.59(18) . . ?
O1 U1 O8 92.65(19) . . ?
O9 U1 O8 83.89(15) 2_566 . ?
O2 U1 O10 97.00(18) . . ?
O1 U1 O10 85.93(18) . . ?
O9 U1 O10 157.68(16) 2_566 . ?
O8 U1 O10 74.80(15) . . ?
O2 U1 O5 87.47(19) . . ?
O1 U1 O5 90.43(19) . . ?
O9 U1 O5 75.84(16) 2_566 . ?
O8 U1 O5 159.42(16) . . ?
O10 U1 O5 125.74(15) . . ?
O2 U1 O4 87.84(18) . . ?
O1 U1 O4 92.56(18) . . ?
O9 U1 O4 128.81(16) 2_566 . ?
O8 U1 O4 146.99(16) . . ?
O10 U1 O4 73.10(16) . . ?
O5 U1 O4 52.98(16) . . ?
O3 U2 O3 180 . 2_655 ?
O3 U2 O7 93.4(2) . 2_655 ?
O3 U2 O7 86.6(2) 2_655 2_655 ?
O3 U2 O7 86.6(2) . . ?
O3 U2 O7 93.4(2) 2_655 . ?
O7 U2 O7 180.0 2_655 . ?
O3 U2 O6 91.20(19) . . ?
O3 U2 O6 88.80(19) 2_655 . ?
O7 U2 O6 126.92(15) 2_655 . ?
O7 U2 O6 53.08(15) . . ?
O3 U2 O6 88.80(19) . 2_655 ?
O3 U2 O6 91.20(19) 2_655 2_655 ?
O7 U2 O6 53.08(15) 2_655 2_655 ?
O7 U2 O6 126.92(15) . 2_655 ?
O6 U2 O6 180.0 . 2_655 ?
O3 U2 O12 91.5(2) . . ?
O3 U2 O12 88.5(2) 2_655 . ?
O7 U2 O12 117.41(17) 2_655 . ?
O7 U2 O12 62.59(17) . . ?
O6 U2 O12 115.27(17) . . ?
O6 U2 O12 64.73(17) 2_655 . ?
O3 U2 O12 88.5(2) . 2_655 ?
O3 U2 O12 91.5(2) 2_655 2_655 ?
O7 U2 O12 62.59(17) 2_655 2_655 ?
O7 U2 O12 117.41(17) . 2_655 ?
O6 U2 O12 64.73(17) . 2_655 ?
O6 U2 O12 115.27(17) 2_655 2_655 ?
O12 U2 O12 180.0 . 2_655 ?
N1 Cu1 N1 180.0(3) . 2_556 ?
N1 Cu1 N2 85.4(2) . . ?
N1 Cu1 N2 94.6(2) 2_556 . ?
N1 Cu1 N2 94.6(2) . 2_556 ?
N1 Cu1 N2 85.4(2) 2_556 2_556 ?
N2 Cu1 N2 180.0 . 2_556 ?
N1 Cu1 O11 90.37(18) . 2_556 ?
N1 Cu1 O11 89.63(18) 2_556 2_556 ?
N2 Cu1 O11 99.13(18) . 2_556 ?
N2 Cu1 O11 80.87(18) 2_556 2_556 ?
N1 Cu1 O11 89.63(18) . . ?
N1 Cu1 O11 90.37(18) 2_556 . ?
N2 Cu1 O11 80.87(18) . . ?
N2 Cu1 O11 99.13(18) 2_556 . ?
O11 Cu1 O11 180.0(2) 2_556 . ?
C13 O4 U1 92.1(4) . . ?
C13 O5 U1 95.6(4) . . ?
C14 O6 U2 94.1(4) . . ?
C14 O7 U2 94.6(4) . . ?
C27 O8 U1 147.0(4) . . ?
C27 O9 U1 138.6(4) . 2_566 ?
C28 O10 U1 125.2(4) . . ?
C28 O11 Cu1 134.6(4) . . ?
U2 O12 H12A 125(5) . . ?
U2 O12 H12B 127(5) . . ?
H12A O12 H12B 106.7(17) . . ?
H13A O13 H13B 107.9(18) . . ?
C33 N1 C29 113.0(5) 2_556 . ?
C33 N1 Cu1 117.6(4) 2_556 . ?
C29 N1 Cu1 106.2(4) . . ?
C33 N1 H1 119(4) 2_556 . ?
C29 N1 H1 105(4) . . ?
Cu1 N1 H1 94(4) . . ?
C30 N2 C31 115.1(5) . . ?
C30 N2 Cu1 106.4(4) . . ?
C31 N2 Cu1 123.0(4) . . ?
C30 N2 H2 108(4) . . ?
C31 N2 H2 111(4) . . ?
Cu1 N2 H2 90(4) . . ?
C6 C1 C2 120.4(7) . . ?
C6 C1 C13 119.5(6) . . ?
C2 C1 C13 120.1(6) . . ?
C3 C2 C1 117.7(7) . . ?
C3 C2 C7 119.3(7) . . ?
C1 C2 C7 123.0(7) . . ?
C2 C3 C4 121.8(7) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 H3 119.1 . . ?
C5 C4 C3 119.6(8) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C6 C5 C4 119.0(7) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C1 C6 C5 121.3(7) . . ?
C1 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
C12 C7 C8 118.5(7) . . ?
C12 C7 C2 119.3(7) . . ?
C8 C7 C2 122.0(6) . . ?
C9 C8 C7 120.5(7) . . ?
C9 C8 C14 116.9(7) . . ?
C7 C8 C14 122.6(6) . . ?
C10 C9 C8 120.4(7) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C11 118.9(7) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
C12 C11 C10 120.2(7) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C7 121.4(7) . . ?
C11 C12 H12 119.3 . . ?
C7 C12 H12 119.3 . . ?
O5 C13 O4 119.2(7) . . ?
O5 C13 C1 122.6(7) . . ?
O4 C13 C1 118.1(6) . . ?
O6 C14 O7 118.0(7) . . ?
O6 C14 C8 122.0(7) . . ?
O7 C14 C8 120.0(7) . . ?
C20 C15 C16 120.1(7) . . ?
C20 C15 C27 116.0(6) . . ?
C16 C15 C27 123.7(6) . . ?
C17 C16 C15 115.8(6) . . ?
C17 C16 C21 117.0(6) . . ?
C15 C16 C21 127.1(6) . . ?
C18 C17 C16 124.0(7) . . ?
C18 C17 H17 118.0 . . ?
C16 C17 H17 118.0 . . ?
C17 C18 C19 119.3(7) . . ?
C17 C18 H18 120.4 . . ?
C19 C18 H18 120.4 . . ?
C20 C19 C18 118.6(7) . . ?
C20 C19 H19 120.7 . . ?
C18 C19 H19 120.7 . . ?
C19 C20 C15 122.1(6) . . ?
C19 C20 H20 119.0 . . ?
C15 C20 H20 119.0 . . ?
C22 C21 C26 117.5(6) . . ?
C22 C21 C16 124.4(5) . . ?
C26 C21 C16 118.1(6) . . ?
C21 C22 C23 121.3(6) . . ?
C21 C22 C28 121.2(6) . . ?
C23 C22 C28 117.5(6) . . ?
C22 C23 C24 120.2(6) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C25 C24 C23 118.4(6) . . ?
C25 C24 H24 120.8 . . ?
C23 C24 H24 120.8 . . ?
C24 C25 C26 121.3(6) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 H25 119.4 . . ?
C25 C26 C21 121.3(6) . . ?
C25 C26 H26 119.4 . . ?
C21 C26 H26 119.4 . . ?
O8 C27 O9 121.2(7) . . ?
O8 C27 C15 119.8(6) . . ?
O9 C27 C15 119.0(6) . . ?
O11 C28 O10 124.2(6) . . ?
O11 C28 C22 118.2(6) . . ?
O10 C28 C22 117.6(6) . . ?
N1 C29 C30 107.7(5) . . ?
N1 C29 H29A 110.2 . . ?
C30 C29 H29A 110.2 . . ?
N1 C29 H29B 110.2 . . ?
C30 C29 H29B 110.2 . . ?
H29A C29 H29B 108.5 . . ?
N2 C30 C29 108.2(5) . . ?
N2 C30 H30A 110.1 . . ?
C29 C30 H30A 110.1 . . ?
N2 C30 H30B 110.1 . . ?
C29 C30 H30B 110.1 . . ?
H30A C30 H30B 108.4 . . ?
N2 C31 C32 108.6(5) . . ?
N2 C31 C34 110.1(6) . . ?
C32 C31 C34 111.3(6) . . ?
N2 C31 C35 109.5(5) . . ?
C32 C31 C35 107.9(6) . . ?
C34 C31 C35 109.3(6) . . ?
C33 C32 C31 118.9(6) . . ?
C33 C32 H32A 107.6 . . ?
C31 C32 H32A 107.6 . . ?
C33 C32 H32B 107.6 . . ?
C31 C32 H32B 107.6 . . ?
H32A C32 H32B 107.0 . . ?
N1 C33 C36 113.5(6) 2_556 . ?
N1 C33 C32 110.1(5) 2_556 . ?
C36 C33 C32 109.4(6) . . ?
N1 C33 H33 107.9 2_556 . ?
C36 C33 H33 107.9 . . ?
C32 C33 H33 107.9 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C31 C35 H35A 109.5 . . ?
C31 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C31 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O12 H12A O13 0.839(10) 1.93(3) 2.743(7) 162(6) 2_655 yes
O12 H12B O15 0.842(10) 2.11(3) 2.922(8) 162(7) . yes
O13 H13A O4 0.838(10) 1.938(13) 2.773(7) 174(8) . yes
O13 H13B O14 0.837(10) 1.96(3) 2.758(9) 159(7) 1_455 yes
N1 H1 O10 0.962(10) 2.134(14) 3.092(7) 173(5) 2_556 yes
N2 H2 O11 0.971(10) 2.18(5) 2.911(7) 131(5) . yes
C32 H32A O1 0.99 2.59 3.423(9) 142 . yes
C34 H34C O11 0.98 2.52 3.429(8) 154 2_556 yes

_refine_diff_density_max         1.171
_refine_diff_density_min         -1.842
_refine_diff_density_rms         0.202

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1958813'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2019-10-11 deposited with the CCDC.	2019-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H40 N2 O16 U2'
_chemical_formula_weight         1352.86

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

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

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

_cell_length_a                   9.3807(5)
_cell_length_b                   15.4285(7)
_cell_length_c                   16.3847(9)
_cell_angle_alpha                76.348(3)
_cell_angle_beta                 74.879(3)
_cell_angle_gamma                86.421(3)
_cell_volume                     2224.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    123754
_cell_measurement_theta_min      1.67
_cell_measurement_theta_max      25.68

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.020
_exptl_crystal_F_000             1284
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    7.346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.259
_exptl_absorpt_correction_T_max  0.309
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 33 mm'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       
'2 φ and 12 ω scans with 2° steps (775 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            123754
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.666
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8441
_reflns_number_gt                6754
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_refine_special_details          
;
 Structure solved by intrinsic phasing and subsequent difference Fourier
 synthesis. All non-hydrogen atoms were refined with anisotropic
 displacement parameters. The H atoms were introduced at calculated
 positions and were treated as riding atoms with an isotropic displacement
 parameter equal to 1.2 times that of the parent atom (1.5 for CH₃, with
 optimized geometry). 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0256P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8441
_refine_ls_number_parameters     599
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0277
_refine_ls_wR_factor_ref         0.0610
_refine_ls_wR_factor_gt          0.0578
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.65210(2) 0.52717(2) 0.71610(2) 0.02216(6) Uani 1 1 d . . . . .
U2 U 0.74557(2) 0.93724(2) 0.26206(2) 0.02059(6) Uani 1 1 d . . . . .
O1 O 0.6064(3) 0.5073(2) 0.62401(19) 0.0310(8) Uani 1 1 d . . . . .
O2 O 0.6979(3) 0.5466(2) 0.80802(18) 0.0250(7) Uani 1 1 d . . . . .
O3 O 0.5693(3) 0.8868(2) 0.30690(19) 0.0260(7) Uani 1 1 d . . . . .
O4 O 0.9209(3) 0.9874(2) 0.21816(19) 0.0273(7) Uani 1 1 d . . . . .
O5 O 0.7578(3) 0.6711(2) 0.62623(19) 0.0286(7) Uani 1 1 d . . . . .
O6 O 0.9099(3) 0.5571(2) 0.6271(2) 0.0354(8) Uani 1 1 d . . . . .
O7 O 0.7108(3) 0.98813(19) 0.39941(18) 0.0247(7) Uani 1 1 d . . . . .
O8 O 0.8162(3) 0.8579(2) 0.39488(18) 0.0260(7) Uani 1 1 d . . . . .
O9 O 0.8057(3) 0.39073(19) 0.73555(18) 0.0221(7) Uani 1 1 d . . . . .
O10 O 0.5668(3) 0.37743(19) 0.79419(19) 0.0262(7) Uani 1 1 d . . . . .
O11 O 1.1399(3) 0.2081(2) 0.75074(19) 0.0273(7) Uani 1 1 d . . . . .
O12 O 1.2182(3) 0.1367(2) 0.86302(19) 0.0262(7) Uani 1 1 d . . . . .
O13 O 0.3849(3) 0.5228(2) 0.7969(2) 0.0277(7) Uani 1 1 d . . . . .
O14 O 0.4772(3) 0.65369(19) 0.72375(19) 0.0260(7) Uani 1 1 d . . . . .
O15 O 0.3457(3) 0.9738(2) 0.85815(19) 0.0262(7) Uani 1 1 d . . . . .
O16 O 0.3551(3) 0.90849(18) 0.75186(18) 0.0232(7) Uani 1 1 d . . . . .
N1 N 0.4064(4) 0.8099(2) 0.6214(2) 0.0252(9) Uani 1 1 d . . . . .
H1A H 0.4283 0.7690 0.6664 0.030 Uiso 1 1 calc R U . . .
H1B H 0.4358 0.8643 0.6234 0.030 Uiso 1 1 calc R U . . .
N2 N 1.1170(4) 0.3772(3) 0.6545(2) 0.0330(10) Uani 1 1 d . . . . .
H2A H 1.1051 0.3238 0.6936 0.040 Uiso 1 1 calc R U . . .
H2B H 1.0285 0.3927 0.6421 0.040 Uiso 1 1 calc R U . . .
C1 C 1.0030(5) 0.6974(3) 0.5347(3) 0.0280(11) Uani 1 1 d . . . . .
C2 C 0.9924(5) 0.7914(3) 0.5119(3) 0.0232(10) Uani 1 1 d . . . . .
C3 C 1.1029(5) 0.8379(3) 0.4436(3) 0.0228(10) Uani 1 1 d . . . . .
H3 H 1.0969 0.9011 0.4270 0.027 Uiso 1 1 calc R U . . .
C4 C 1.2211(5) 0.7945(3) 0.3992(3) 0.0275(11) Uani 1 1 d . . . . .
H4 H 1.2939 0.8278 0.3525 0.033 Uiso 1 1 calc R U . . .
C5 C 1.2329(5) 0.7030(3) 0.4228(3) 0.0313(12) Uani 1 1 d . . . . .
H5 H 1.3152 0.6732 0.3938 0.038 Uiso 1 1 calc R U . . .
C6 C 1.1238(5) 0.6552(3) 0.4892(3) 0.0306(11) Uani 1 1 d . . . . .
H6 H 1.1310 0.5920 0.5044 0.037 Uiso 1 1 calc R U . . .
C7 C 0.8805(4) 0.8451(3) 0.5621(3) 0.0224(10) Uani 1 1 d . . . . .
C8 C 0.7871(5) 0.9094(3) 0.5256(3) 0.0228(10) Uani 1 1 d . . . . .
C9 C 0.6978(5) 0.9633(3) 0.5760(3) 0.0247(10) Uani 1 1 d . . . . .
H9 H 0.6340 1.0057 0.5513 0.030 Uiso 1 1 calc R U . . .
C10 C 0.7011(5) 0.9559(3) 0.6614(3) 0.0255(10) Uani 1 1 d . . . . .
H10 H 0.6414 0.9934 0.6951 0.031 Uiso 1 1 calc R U . . .
C11 C 0.7925(5) 0.8931(3) 0.6966(3) 0.0280(11) Uani 1 1 d . . . . .
H11 H 0.7952 0.8875 0.7551 0.034 Uiso 1 1 calc R U . . .
C12 C 0.8798(5) 0.8385(3) 0.6489(3) 0.0270(11) Uani 1 1 d . . . . .
H12 H 0.9408 0.7954 0.6753 0.032 Uiso 1 1 calc R U . . .
C13 C 0.8843(5) 0.6397(3) 0.6004(3) 0.0298(11) Uani 1 1 d . . . . .
C14 C 0.7733(5) 0.9184(3) 0.4343(3) 0.0240(10) Uani 1 1 d . . . . .
C15 C 0.7135(4) 0.2510(3) 0.8334(3) 0.0198(10) Uani 1 1 d . . . . .
C16 C 0.8258(5) 0.2243(3) 0.8762(3) 0.0225(10) Uani 1 1 d . . . . .
C17 C 0.8339(5) 0.1342(3) 0.9169(3) 0.0255(10) Uani 1 1 d . . . . .
H17 H 0.9107 0.1151 0.9451 0.031 Uiso 1 1 calc R U . . .
C18 C 0.7337(5) 0.0726(3) 0.9174(3) 0.0299(11) Uani 1 1 d . . . . .
H18 H 0.7414 0.0119 0.9458 0.036 Uiso 1 1 calc R U . . .
C19 C 0.6205(5) 0.1000(3) 0.8759(3) 0.0311(11) Uani 1 1 d . . . . .
H19 H 0.5509 0.0578 0.8759 0.037 Uiso 1 1 calc R U . . .
C20 C 0.6099(5) 0.1880(3) 0.8350(3) 0.0263(11) Uani 1 1 d . . . . .
H20 H 0.5320 0.2065 0.8076 0.032 Uiso 1 1 calc R U . . .
C21 C 0.9284(5) 0.2894(3) 0.8863(3) 0.0203(10) Uani 1 1 d . . . . .
C22 C 1.0807(5) 0.2731(3) 0.8730(3) 0.0226(10) Uani 1 1 d . . . . .
C23 C 1.1715(5) 0.3295(3) 0.8919(3) 0.0254(10) Uani 1 1 d . . . . .
H23 H 1.2741 0.3171 0.8837 0.030 Uiso 1 1 calc R U . . .
C24 C 1.1125(5) 0.4039(3) 0.9227(3) 0.0249(10) Uani 1 1 d . . . . .
H24 H 1.1744 0.4423 0.9358 0.030 Uiso 1 1 calc R U . . .
C25 C 0.9626(5) 0.4218(3) 0.9342(3) 0.0226(10) Uani 1 1 d . . . . .
H25 H 0.9223 0.4734 0.9540 0.027 Uiso 1 1 calc R U . . .
C26 C 0.8713(5) 0.3647(3) 0.9167(3) 0.0252(10) Uani 1 1 d . . . . .
H26 H 0.7687 0.3772 0.9256 0.030 Uiso 1 1 calc R U . . .
C27 C 0.6969(5) 0.3435(3) 0.7853(3) 0.0224(10) Uani 1 1 d . . . . .
C28 C 1.1489(5) 0.2011(3) 0.8290(3) 0.0228(10) Uani 1 1 d . . . . .
C29 C 0.2349(5) 0.6525(3) 0.8166(3) 0.0231(10) Uani 1 1 d . . . . .
C30 C 0.2454(4) 0.7210(3) 0.8577(3) 0.0196(9) Uani 1 1 d . . . . .
C31 C 0.1176(4) 0.7711(3) 0.8825(3) 0.0221(10) Uani 1 1 d . . . . .
H31 H 0.1226 0.8192 0.9088 0.027 Uiso 1 1 calc R U . . .
C32 C -0.0148(5) 0.7514(3) 0.8692(3) 0.0275(11) Uani 1 1 d . . . . .
H32 H -0.0995 0.7867 0.8854 0.033 Uiso 1 1 calc R U . . .
C33 C -0.0256(5) 0.6803(3) 0.8325(3) 0.0299(11) Uani 1 1 d . . . . .
H33 H -0.1177 0.6655 0.8253 0.036 Uiso 1 1 calc R U . . .
C34 C 0.0994(5) 0.6317(3) 0.8065(3) 0.0262(11) Uani 1 1 d . . . . .
H34 H 0.0928 0.5832 0.7812 0.031 Uiso 1 1 calc R U . . .
C35 C 0.3798(5) 0.7373(3) 0.8832(3) 0.0224(10) Uani 1 1 d . . . . .
C36 C 0.4284(4) 0.8235(3) 0.8780(3) 0.0205(10) Uani 1 1 d . . . . .
C37 C 0.5344(5) 0.8355(3) 0.9207(3) 0.0263(11) Uani 1 1 d . . . . .
H37 H 0.5628 0.8940 0.9191 0.032 Uiso 1 1 calc R U . . .
C38 C 0.5977(4) 0.7623(3) 0.9652(3) 0.0248(10) Uani 1 1 d . . . . .
H38 H 0.6685 0.7707 0.9948 0.030 Uiso 1 1 calc R U . . .
C39 C 0.5587(5) 0.6779(3) 0.9669(3) 0.0262(11) Uani 1 1 d . . . . .
H39 H 0.6055 0.6277 0.9954 0.031 Uiso 1 1 calc R U . . .
C40 C 0.4510(4) 0.6657(3) 0.9269(3) 0.0226(10) Uani 1 1 d . . . . .
H40 H 0.4243 0.6067 0.9291 0.027 Uiso 1 1 calc R U . . .
C41 C 0.3719(5) 0.6063(3) 0.7779(3) 0.0255(10) Uani 1 1 d . . . . .
C42 C 0.3749(5) 0.9048(3) 0.8269(3) 0.0249(10) Uani 1 1 d . . . . .
C43 C 0.2440(5) 0.8112(3) 0.6322(3) 0.0293(11) Uani 1 1 d . . . . .
H43A H 0.2194 0.8566 0.5849 0.044 Uiso 1 1 calc R U . . .
H43B H 0.1942 0.8254 0.6880 0.044 Uiso 1 1 calc R U . . .
H43C H 0.2115 0.7526 0.6308 0.044 Uiso 1 1 calc R U . . .
C44 C 0.4897(5) 0.7879(3) 0.5383(3) 0.0318(11) Uani 1 1 d . . . . .
H44A H 0.4503 0.7330 0.5326 0.048 Uiso 1 1 calc R U . . .
H44B H 0.5943 0.7795 0.5380 0.048 Uiso 1 1 calc R U . . .
H44C H 0.4796 0.8369 0.4897 0.048 Uiso 1 1 calc R U . . .
C45 C 1.1581(6) 0.4440(3) 0.6943(3) 0.0438(14) Uani 1 1 d . . . . .
H45A H 1.2585 0.4321 0.7014 0.066 Uiso 1 1 calc R U . . .
H45B H 1.0891 0.4413 0.7512 0.066 Uiso 1 1 calc R U . . .
H45C H 1.1543 0.5035 0.6570 0.066 Uiso 1 1 calc R U . . .
C46 C 1.2241(6) 0.3663(4) 0.5752(3) 0.0479(15) Uani 1 1 d . . . . .
H46A H 1.2282 0.4211 0.5299 0.072 Uiso 1 1 calc R U . . .
H46B H 1.1944 0.3164 0.5558 0.072 Uiso 1 1 calc R U . . .
H46C H 1.3217 0.3541 0.5866 0.072 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 1.763(3) . ?
U1 O1 1.768(3) . ?
U1 O10 2.432(3) . ?
U1 O5 2.460(3) . ?
U1 O14 2.475(3) . ?
U1 O9 2.480(3) . ?
U1 O6 2.483(3) . ?
U1 O13 2.507(3) . ?
U2 O4 1.760(3) . ?
U2 O3 1.771(3) . ?
U2 O15 2.441(3) 2_676 ?
U2 O11 2.456(3) 2_766 ?
U2 O8 2.463(3) . ?
U2 O16 2.487(3) 2_676 ?
U2 O7 2.491(3) . ?
U2 O12 2.511(3) 2_766 ?
O5 C13 1.259(5) . ?
O6 C13 1.275(5) . ?
O7 C14 1.278(5) . ?
O8 C14 1.245(5) . ?
O9 C27 1.271(5) . ?
O10 C27 1.283(5) . ?
O11 C28 1.285(5) . ?
O11 U2 2.456(3) 2_766 ?
O12 C28 1.252(5) . ?
O12 U2 2.511(3) 2_766 ?
O13 C41 1.259(5) . ?
O14 C41 1.275(5) . ?
O15 C42 1.271(5) . ?
O15 U2 2.440(3) 2_676 ?
O16 C42 1.278(5) . ?
O16 U2 2.487(3) 2_676 ?
N1 C43 1.486(5) . ?
N1 C44 1.486(5) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N2 C46 1.458(6) . ?
N2 C45 1.462(6) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
C1 C6 1.401(6) . ?
C1 C2 1.413(6) . ?
C1 C13 1.495(6) . ?
C2 C3 1.397(6) . ?
C2 C7 1.493(6) . ?
C3 C4 1.387(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.378(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(6) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.401(6) . ?
C7 C8 1.412(6) . ?
C8 C9 1.397(6) . ?
C8 C14 1.509(6) . ?
C9 C10 1.385(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.377(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.371(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C15 C16 1.402(6) . ?
C15 C20 1.407(6) . ?
C15 C27 1.480(6) . ?
C16 C17 1.399(6) . ?
C16 C21 1.498(6) . ?
C17 C18 1.375(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.398(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.375(6) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C26 1.394(6) . ?
C21 C22 1.404(6) . ?
C22 C23 1.392(6) . ?
C22 C28 1.488(6) . ?
C23 C24 1.387(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.388(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.390(6) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C29 C34 1.390(6) . ?
C29 C30 1.402(6) . ?
C29 C41 1.494(6) . ?
C30 C31 1.406(5) . ?
C30 C35 1.481(6) . ?
C31 C32 1.379(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.390(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.378(6) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C40 1.400(6) . ?
C35 C36 1.408(6) . ?
C36 C37 1.400(6) . ?
C36 C42 1.474(6) . ?
C37 C38 1.383(6) . ?
C37 H37 0.9500 . ?
C38 C39 1.367(6) . ?
C38 H38 0.9500 . ?
C39 C40 1.383(6) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U1 O1 179.83(14) . . ?
O2 U1 O10 91.19(12) . . ?
O1 U1 O10 88.68(13) . . ?
O2 U1 O5 91.82(12) . . ?
O1 U1 O5 88.31(13) . . ?
O10 U1 O5 173.89(10) . . ?
O2 U1 O14 87.84(11) . . ?
O1 U1 O14 92.32(12) . . ?
O10 U1 O14 119.34(10) . . ?
O5 U1 O14 66.11(10) . . ?
O2 U1 O9 85.90(11) . . ?
O1 U1 O9 93.93(12) . . ?
O10 U1 O9 53.12(9) . . ?
O5 U1 O9 121.83(9) . . ?
O14 U1 O9 170.02(9) . . ?
O2 U1 O6 91.49(12) . . ?
O1 U1 O6 88.49(13) . . ?
O10 U1 O6 121.90(10) . . ?
O5 U1 O6 52.70(10) . . ?
O14 U1 O6 118.76(10) . . ?
O9 U1 O6 69.24(10) . . ?
O2 U1 O13 88.92(12) . . ?
O1 U1 O13 91.12(12) . . ?
O10 U1 O13 67.17(10) . . ?
O5 U1 O13 118.20(10) . . ?
O14 U1 O13 52.17(10) . . ?
O9 U1 O13 119.85(10) . . ?
O6 U1 O13 170.90(10) . . ?
O4 U2 O3 179.64(13) . . ?
O4 U2 O15 91.42(12) . 2_676 ?
O3 U2 O15 88.85(12) . 2_676 ?
O4 U2 O11 89.27(12) . 2_766 ?
O3 U2 O11 90.80(12) . 2_766 ?
O15 U2 O11 118.99(10) 2_676 2_766 ?
O4 U2 O8 91.34(12) . . ?
O3 U2 O8 88.35(12) . . ?
O15 U2 O8 172.90(10) 2_676 . ?
O11 U2 O8 67.59(10) 2_766 . ?
O4 U2 O16 86.27(12) . 2_676 ?
O3 U2 O16 93.71(11) . 2_676 ?
O15 U2 O16 52.74(10) 2_676 2_676 ?
O11 U2 O16 170.41(9) 2_766 2_676 ?
O8 U2 O16 120.96(9) . 2_676 ?
O4 U2 O7 92.34(12) . . ?
O3 U2 O7 87.32(12) . . ?
O15 U2 O7 120.83(9) 2_676 . ?
O11 U2 O7 120.08(9) 2_766 . ?
O8 U2 O7 52.50(9) . . ?
O16 U2 O7 68.65(9) 2_676 . ?
O4 U2 O12 90.94(12) . 2_766 ?
O3 U2 O12 89.38(12) . 2_766 ?
O15 U2 O12 66.75(10) 2_676 2_766 ?
O11 U2 O12 52.24(9) 2_766 2_766 ?
O8 U2 O12 119.73(10) . 2_766 ?
O16 U2 O12 119.29(9) 2_676 2_766 ?
O7 U2 O12 171.62(9) . 2_766 ?
C13 O5 U1 94.4(3) . . ?
C13 O6 U1 92.9(3) . . ?
C14 O7 U2 92.3(3) . . ?
C14 O8 U2 94.5(3) . . ?
C27 O9 U1 92.8(2) . . ?
C27 O10 U1 94.7(3) . . ?
C28 O11 U2 95.0(2) . 2_766 ?
C28 O12 U2 93.2(3) . 2_766 ?
C41 O13 U1 93.2(3) . . ?
C41 O14 U1 94.3(2) . . ?
C42 O15 U2 95.6(3) . 2_676 ?
C42 O16 U2 93.2(3) . 2_676 ?
C43 N1 C44 112.6(3) . . ?
C43 N1 H1A 109.1 . . ?
C44 N1 H1A 109.1 . . ?
C43 N1 H1B 109.1 . . ?
C44 N1 H1B 109.1 . . ?
H1A N1 H1B 107.8 . . ?
C46 N2 C45 114.2(4) . . ?
C46 N2 H2A 108.7 . . ?
C45 N2 H2A 108.7 . . ?
C46 N2 H2B 108.7 . . ?
C45 N2 H2B 108.7 . . ?
H2A N2 H2B 107.6 . . ?
C6 C1 C2 119.0(4) . . ?
C6 C1 C13 117.7(4) . . ?
C2 C1 C13 123.0(4) . . ?
C3 C2 C1 118.0(4) . . ?
C3 C2 C7 117.3(4) . . ?
C1 C2 C7 124.3(4) . . ?
C4 C3 C2 121.8(4) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C5 C4 C3 120.1(4) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 119.3(4) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C5 C6 C1 121.7(5) . . ?
C5 C6 H6 119.1 . . ?
C1 C6 H6 119.1 . . ?
C12 C7 C8 117.6(4) . . ?
C12 C7 C2 117.5(4) . . ?
C8 C7 C2 124.4(4) . . ?
C9 C8 C7 120.0(4) . . ?
C9 C8 C14 118.1(4) . . ?
C7 C8 C14 121.8(4) . . ?
C10 C9 C8 120.9(4) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C11 C10 C9 118.8(4) . . ?
C11 C10 H10 120.6 . . ?
C9 C10 H10 120.6 . . ?
C12 C11 C10 121.5(4) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C11 C12 C7 121.1(4) . . ?
C11 C12 H12 119.4 . . ?
C7 C12 H12 119.4 . . ?
O5 C13 O6 119.9(4) . . ?
O5 C13 C1 120.5(4) . . ?
O6 C13 C1 119.5(4) . . ?
O8 C14 O7 120.6(4) . . ?
O8 C14 C8 121.0(4) . . ?
O7 C14 C8 118.3(4) . . ?
C16 C15 C20 119.7(4) . . ?
C16 C15 C27 123.3(4) . . ?
C20 C15 C27 117.0(4) . . ?
C17 C16 C15 118.3(4) . . ?
C17 C16 C21 119.0(4) . . ?
C15 C16 C21 122.5(4) . . ?
C18 C17 C16 121.9(4) . . ?
C18 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
C17 C18 C19 119.5(4) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C20 C19 C18 120.0(4) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C20 C15 120.6(4) . . ?
C19 C20 H20 119.7 . . ?
C15 C20 H20 119.7 . . ?
C26 C21 C22 118.3(4) . . ?
C26 C21 C16 119.8(4) . . ?
C22 C21 C16 121.7(4) . . ?
C23 C22 C21 120.7(4) . . ?
C23 C22 C28 119.2(4) . . ?
C21 C22 C28 119.7(4) . . ?
C24 C23 C22 120.2(4) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 119.6(4) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
C24 C25 C26 120.3(4) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C21 C26 C25 120.9(4) . . ?
C21 C26 H26 119.6 . . ?
C25 C26 H26 119.6 . . ?
O9 C27 O10 118.7(4) . . ?
O9 C27 C15 122.9(4) . . ?
O10 C27 C15 118.4(4) . . ?
O12 C28 O11 119.1(4) . . ?
O12 C28 C22 123.4(4) . . ?
O11 C28 C22 117.4(4) . . ?
C34 C29 C30 120.2(4) . . ?
C34 C29 C41 120.0(4) . . ?
C30 C29 C41 119.6(4) . . ?
C29 C30 C31 117.9(4) . . ?
C29 C30 C35 123.1(4) . . ?
C31 C30 C35 118.8(4) . . ?
C32 C31 C30 120.8(4) . . ?
C32 C31 H31 119.6 . . ?
C30 C31 H31 119.6 . . ?
C31 C32 C33 120.7(4) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 H32 119.6 . . ?
C34 C33 C32 119.0(4) . . ?
C34 C33 H33 120.5 . . ?
C32 C33 H33 120.5 . . ?
C33 C34 C29 121.2(4) . . ?
C33 C34 H34 119.4 . . ?
C29 C34 H34 119.4 . . ?
C40 C35 C36 116.6(4) . . ?
C40 C35 C30 119.7(4) . . ?
C36 C35 C30 122.9(4) . . ?
C37 C36 C35 120.6(4) . . ?
C37 C36 C42 116.4(4) . . ?
C35 C36 C42 122.9(4) . . ?
C38 C37 C36 120.1(4) . . ?
C38 C37 H37 119.9 . . ?
C36 C37 H37 119.9 . . ?
C39 C38 C37 120.3(4) . . ?
C39 C38 H38 119.8 . . ?
C37 C38 H38 119.8 . . ?
C38 C39 C40 119.7(4) . . ?
C38 C39 H39 120.1 . . ?
C40 C39 H39 120.1 . . ?
C39 C40 C35 122.4(4) . . ?
C39 C40 H40 118.8 . . ?
C35 C40 H40 118.8 . . ?
O13 C41 O14 119.7(4) . . ?
O13 C41 C29 121.9(4) . . ?
O14 C41 C29 118.4(4) . . ?
O15 C42 O16 118.3(4) . . ?
O15 C42 C36 119.5(4) . . ?
O16 C42 C36 122.2(4) . . ?
N1 C43 H43A 109.5 . . ?
N1 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N1 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N1 C44 H44A 109.5 . . ?
N1 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
N1 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N2 C45 H45A 109.5 . . ?
N2 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
N2 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N2 C46 H46A 109.5 . . ?
N2 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
N2 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1B O7 0.91 2.59 3.209(5) 126.2 2_676
N1 H1B O16 0.91 2.29 2.832(5) 117.8 .
N1 H1A O14 0.91 1.89 2.745(4) 154.7 .
N2 H2B O9 0.91 2.24 2.893(5) 128.0 .
N2 H2A O11 0.91 1.86 2.739(5) 161.4 .
C45 H45C O6 0.98 2.52 3.098(6) 117.9 .

_refine_diff_density_max         2.069
_refine_diff_density_min         -1.171
_refine_diff_density_rms         0.215

_shelxl_version_number           2014-3

