# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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 2264768'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2023-05-23 deposited with the CCDC.	2023-06-21 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT306_1                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O12 Check 
RESPONSE: This oxygen atom pertains to a water molecule for
which the H atoms were not found.
;
# end Validation Reply Form

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H26 N2 O13 U'
_chemical_formula_iupac          ?
_chemical_formula_weight         644.38

_chemical_melting_point          ?

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

_cell_length_a                   11.6052(7)
_cell_length_b                   15.1797(10)
_cell_length_c                   12.7681(13)
_cell_angle_alpha                90
_cell_angle_beta                 116.773(3)
_cell_angle_gamma                90
_cell_volume                     2008.1(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    796
_cell_measurement_theta_min      4.5035
_cell_measurement_theta_max      26.1956
_cell_measurement_temperature    100(2)

_exptl_crystal_description       irregular
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.031
_exptl_crystal_density_diffrn    2.131
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1232

_exptl_absorpt_coefficient_mu    8.150
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_T_max  0.75

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100(2)

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

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

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

_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_detector_area_resol_mean 7.41

_diffrn_reflns_number            71359
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15

_refine_special_details          
;
The H atoms bound to N2 and O11 were found and either
refined freely (N2) or with restraints on bond lengths and
angle (O11). Those bound to O12 and O13 were not found.
;

_reflns_number_total             3814
_reflns_number_gt                3589
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0187
_refine_ls_wR_factor_gt          0.0454
_refine_ls_wR_factor_ref         0.0464
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_number_reflns         3814
_refine_ls_number_parameters     269
_refine_ls_number_restraints     3
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0185P)²+6.2592P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.177
_refine_diff_density_min         -0.645
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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

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

loop_
_atom_site_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 0.35244(2) 0.91984(2) 0.65860(2) 0.01530(5) Uani 1 1 d . . . . .
O1 O 0.3897(3) 0.85122(17) 0.7810(2) 0.0267(6) Uani 1 1 d . . . . .
O2 O 0.3160(3) 0.98680(16) 0.5342(2) 0.0264(6) Uani 1 1 d . . . . .
O3 O 0.3838(2) 0.79782(16) 0.5454(2) 0.0250(6) Uani 1 1 d . . . . .
O4 O 0.5563(2) 0.87107(18) 0.6605(3) 0.0324(7) Uani 1 1 d . . . . .
O5 O 0.9656(2) 0.52205(17) 0.7264(2) 0.0278(6) Uani 1 1 d . . . . .
O6 O 1.1463(2) 0.54462(17) 0.7182(2) 0.0273(6) Uani 1 1 d . . . . .
O7 O 1.1423(2) 0.96076(16) 0.6437(2) 0.0223(5) Uani 1 1 d . . . . .
O8 O 1.1463(2) 0.83775(16) 0.5565(2) 0.0215(5) Uani 1 1 d . . . . .
O9 O 0.6400(3) 0.7429(2) 0.3083(2) 0.0445(8) Uani 1 1 d . . . . .
O10 O 0.6977(3) 0.61952(19) 0.3955(3) 0.0409(7) Uani 1 1 d . . . . .
O11 O 0.7693(4) 0.5614(3) 0.7920(4) 0.0702(12) Uani 1 1 d D . . . .
H11A H 0.796(6) 0.550(5) 0.864(2) 0.105 Uiso 1 1 d D U . . .
H11B H 0.832(4) 0.553(5) 0.778(5) 0.105 Uiso 1 1 d D U . . .
O12 O 0.3073(4) 0.6898(3) 0.3284(4) 0.0776(13) Uani 1 1 d . . . . .
O13 O 1.5565(5) 0.4722(3) 0.6339(5) 0.0944(17) Uani 1 1 d . . . . .
N1 N 0.7008(3) 0.6999(2) 0.3953(3) 0.0219(6) Uani 1 1 d . . . . .
N2 N 1.3669(4) 0.5607(3) 0.6687(4) 0.0382(9) Uani 1 1 d . . . . .
H2A H 1.322(5) 0.533(3) 0.700(5) 0.049(15) Uiso 1 1 d . . . . .
H2B H 1.413(5) 0.517(4) 0.653(4) 0.050(15) Uiso 1 1 d . . . . .
C1 C 0.7832(3) 0.7504(2) 0.5089(3) 0.0159(6) Uani 1 1 d . . . . .
C2 C 0.6876(3) 0.8044(2) 0.5336(3) 0.0200(7) Uani 1 1 d . . . . .
H2C H 0.642060 0.845094 0.466908 0.024 Uiso 1 1 calc R U . . .
H2D H 0.736707 0.840803 0.604166 0.024 Uiso 1 1 calc R U . . .
C3 C 0.5870(3) 0.7515(2) 0.5528(4) 0.0258(8) Uani 1 1 d . . . . .
H3A H 0.531333 0.719280 0.479898 0.031 Uiso 1 1 calc R U . . .
H3B H 0.631054 0.707502 0.615537 0.031 Uiso 1 1 calc R U . . .
C4 C 0.5040(3) 0.8104(2) 0.5866(3) 0.0221(7) Uani 1 1 d . . . . .
C5 C 0.8555(3) 0.6831(2) 0.6041(3) 0.0185(7) Uani 1 1 d . . . . .
H5A H 0.793557 0.637161 0.601222 0.022 Uiso 1 1 calc R U . . .
H5B H 0.887522 0.712786 0.681202 0.022 Uiso 1 1 calc R U . . .
C6 C 0.9699(3) 0.6377(2) 0.5973(3) 0.0202(7) Uani 1 1 d . . . . .
H6A H 0.940411 0.612781 0.517674 0.024 Uiso 1 1 calc R U . . .
H6B H 1.036757 0.682442 0.609100 0.024 Uiso 1 1 calc R U . . .
C7 C 1.0298(3) 0.5653(2) 0.6859(3) 0.0221(7) Uani 1 1 d . . . . .
C8 C 0.8712(3) 0.8103(2) 0.4789(3) 0.0161(7) Uani 1 1 d . . . . .
H8A H 0.928643 0.773132 0.459016 0.019 Uiso 1 1 calc R U . . .
H8B H 0.817154 0.845932 0.408859 0.019 Uiso 1 1 calc R U . . .
C9 C 0.9533(3) 0.8718(2) 0.5788(3) 0.0185(7) Uani 1 1 d . . . . .
H9A H 0.906875 0.928455 0.567386 0.022 Uiso 1 1 calc R U . . .
H9B H 0.962152 0.845914 0.653184 0.022 Uiso 1 1 calc R U . . .
C10 C 1.0859(3) 0.8905(2) 0.5912(3) 0.0175(7) Uani 1 1 d . . . . .
C11 C 1.4510(6) 0.6280(3) 0.7475(4) 0.0479(13) Uani 1 1 d . . . . .
H11C H 1.513240 0.647264 0.719912 0.072 Uiso 1 1 calc R U . . .
H11D H 1.497395 0.603602 0.826781 0.072 Uiso 1 1 calc R U . . .
H11E H 1.398993 0.678457 0.748895 0.072 Uiso 1 1 calc R U . . .
C12 C 1.2801(6) 0.5938(4) 0.5525(5) 0.0576(14) Uani 1 1 d . . . . .
H12C H 1.231216 0.644008 0.559995 0.086 Uiso 1 1 calc R U . . .
H12D H 1.220235 0.547081 0.507008 0.086 Uiso 1 1 calc R U . . .
H12E H 1.330576 0.612744 0.512206 0.086 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 1.763(3) . ?
U1 O2 1.769(3) . ?
U1 O7 2.440(2) 1_455 ?
U1 O6 2.458(2) 2_656 ?
U1 O4 2.469(3) . ?
U1 O3 2.475(2) . ?
U1 O8 2.483(2) 1_455 ?
U1 O5 2.496(2) 2_656 ?
U1 C10 2.847(3) 1_455 ?
U1 C4 2.856(3) . ?
U1 C7 2.871(4) 2_656 ?
O3 C4 1.264(4) . ?
O4 C4 1.262(4) . ?
O5 C7 1.265(4) . ?
O6 C7 1.262(4) . ?
O7 C10 1.272(4) . ?
O8 C10 1.268(4) . ?
O9 N1 1.205(4) . ?
O10 N1 1.221(4) . ?
O11 H11A 0.842(10) . ?
O11 H11B 0.842(10) . ?
N1 C1 1.535(4) . ?
N2 C12 1.457(7) . ?
N2 C11 1.458(6) . ?
N2 H2A 0.89(6) . ?
N2 H2B 0.93(6) . ?
C1 C5 1.519(4) . ?
C1 C2 1.521(4) . ?
C1 C8 1.539(4) . ?
C2 C3 1.526(5) . ?
C2 H2C 0.9900 . ?
C2 H2D 0.9900 . ?
C3 C4 1.512(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C5 C6 1.533(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.504(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C8 C9 1.520(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.501(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C11 H11C 0.9800 . ?
C11 H11D 0.9800 . ?
C11 H11E 0.9800 . ?
C12 H12C 0.9800 . ?
C12 H12D 0.9800 . ?
C12 H12E 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 178.75(12) . . ?
O1 U1 O7 93.26(10) . 1_455 ?
O2 U1 O7 87.55(10) . 1_455 ?
O1 U1 O6 87.68(11) . 2_656 ?
O2 U1 O6 93.53(11) . 2_656 ?
O7 U1 O6 64.61(8) 1_455 2_656 ?
O1 U1 O4 87.86(11) . . ?
O2 U1 O4 91.26(11) . . ?
O7 U1 O4 175.63(8) 1_455 . ?
O6 U1 O4 119.69(8) 2_656 . ?
O1 U1 O3 91.93(11) . . ?
O2 U1 O3 86.82(10) . . ?
O7 U1 O3 123.37(8) 1_455 . ?
O6 U1 O3 172.01(8) 2_656 . ?
O4 U1 O3 52.33(8) . . ?
O1 U1 O8 87.85(11) . 1_455 ?
O2 U1 O8 91.88(10) . 1_455 ?
O7 U1 O8 52.70(8) 1_455 1_455 ?
O6 U1 O8 116.70(8) 2_656 1_455 ?
O4 U1 O8 123.18(8) . 1_455 ?
O3 U1 O8 71.25(8) . 1_455 ?
O1 U1 O5 92.34(11) . 2_656 ?
O2 U1 O5 88.16(11) . 2_656 ?
O7 U1 O5 116.02(8) 1_455 2_656 ?
O6 U1 O5 52.03(8) 2_656 2_656 ?
O4 U1 O5 68.13(8) . 2_656 ?
O3 U1 O5 120.04(8) . 2_656 ?
O8 U1 O5 168.68(8) 1_455 2_656 ?
O1 U1 C10 88.57(11) . 1_455 ?
O2 U1 C10 91.74(11) . 1_455 ?
O7 U1 C10 26.44(9) 1_455 1_455 ?
O6 U1 C10 90.36(9) 2_656 1_455 ?
O4 U1 C10 149.54(9) . 1_455 ?
O3 U1 C10 97.60(9) . 1_455 ?
O8 U1 C10 26.41(9) 1_455 1_455 ?
O5 U1 C10 142.27(9) 2_656 1_455 ?
O1 U1 C4 90.06(11) . . ?
O2 U1 C4 88.76(11) . . ?
O7 U1 C4 149.55(9) 1_455 . ?
O6 U1 C4 145.82(9) 2_656 . ?
O4 U1 C4 26.14(9) . . ?
O3 U1 C4 26.19(9) . . ?
O8 U1 C4 97.27(9) 1_455 . ?
O5 U1 C4 94.04(9) 2_656 . ?
C10 U1 C4 123.68(10) 1_455 . ?
O1 U1 C7 89.47(11) . 2_656 ?
O2 U1 C7 91.48(11) . 2_656 ?
O7 U1 C7 90.32(9) 1_455 2_656 ?
O6 U1 C7 25.95(9) 2_656 2_656 ?
O4 U1 C7 93.92(9) . 2_656 ?
O3 U1 C7 146.10(9) . 2_656 ?
O8 U1 C7 142.65(9) 1_455 2_656 ?
O5 U1 C7 26.09(9) 2_656 2_656 ?
C10 U1 C7 116.30(10) 1_455 2_656 ?
C4 U1 C7 119.99(10) . 2_656 ?
C4 O3 U1 94.0(2) . . ?
C4 O4 U1 94.3(2) . . ?
C7 O5 U1 93.7(2) . 2_646 ?
C7 O6 U1 95.6(2) . 2_646 ?
C10 O7 U1 94.93(19) . 1_655 ?
C10 O8 U1 93.03(19) . 1_655 ?
H11A O11 H11B 106.2(17) . . ?
O9 N1 O10 122.5(3) . . ?
O9 N1 C1 117.2(3) . . ?
O10 N1 C1 120.2(3) . . ?
C12 N2 C11 113.7(4) . . ?
C12 N2 H2A 110(3) . . ?
C11 N2 H2A 111(3) . . ?
C12 N2 H2B 103(3) . . ?
C11 N2 H2B 112(3) . . ?
H2A N2 H2B 106(5) . . ?
C5 C1 C2 112.8(3) . . ?
C5 C1 N1 107.7(3) . . ?
C2 C1 N1 105.2(3) . . ?
C5 C1 C8 114.0(3) . . ?
C2 C1 C8 111.1(3) . . ?
N1 C1 C8 105.1(3) . . ?
C1 C2 C3 115.6(3) . . ?
C1 C2 H2C 108.4 . . ?
C3 C2 H2C 108.4 . . ?
C1 C2 H2D 108.4 . . ?
C3 C2 H2D 108.4 . . ?
H2C C2 H2D 107.4 . . ?
C4 C3 C2 111.5(3) . . ?
C4 C3 H3A 109.3 . . ?
C2 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
C2 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
O4 C4 O3 119.4(3) . . ?
O4 C4 C3 119.4(3) . . ?
O3 C4 C3 121.1(3) . . ?
O4 C4 U1 59.54(18) . . ?
O3 C4 U1 59.83(17) . . ?
C3 C4 U1 178.1(3) . . ?
C1 C5 C6 115.9(3) . . ?
C1 C5 H5A 108.3 . . ?
C6 C5 H5A 108.3 . . ?
C1 C5 H5B 108.3 . . ?
C6 C5 H5B 108.3 . . ?
H5A C5 H5B 107.4 . . ?
C7 C6 C5 113.8(3) . . ?
C7 C6 H6A 108.8 . . ?
C5 C6 H6A 108.8 . . ?
C7 C6 H6B 108.8 . . ?
C5 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
O6 C7 O5 118.6(3) . . ?
O6 C7 C6 119.4(3) . . ?
O5 C7 C6 121.9(3) . . ?
O6 C7 U1 58.44(18) . 2_646 ?
O5 C7 U1 60.18(18) . 2_646 ?
C6 C7 U1 175.5(3) . 2_646 ?
C9 C8 C1 112.9(3) . . ?
C9 C8 H8A 109.0 . . ?
C1 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
C1 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C10 C9 C8 115.5(3) . . ?
C10 C9 H9A 108.4 . . ?
C8 C9 H9A 108.4 . . ?
C10 C9 H9B 108.4 . . ?
C8 C9 H9B 108.4 . . ?
H9A C9 H9B 107.5 . . ?
O8 C10 O7 118.7(3) . . ?
O8 C10 C9 123.0(3) . . ?
O7 C10 C9 118.2(3) . . ?
O8 C10 U1 60.56(16) . 1_655 ?
O7 C10 U1 58.63(16) . 1_655 ?
C9 C10 U1 169.6(2) . 1_655 ?
N2 C11 H11C 109.5 . . ?
N2 C11 H11D 109.5 . . ?
H11C C11 H11D 109.5 . . ?
N2 C11 H11E 109.5 . . ?
H11C C11 H11E 109.5 . . ?
H11D C11 H11E 109.5 . . ?
N2 C12 H12C 109.5 . . ?
N2 C12 H12D 109.5 . . ?
H12C C12 H12D 109.5 . . ?
N2 C12 H12E 109.5 . . ?
H12C C12 H12E 109.5 . . ?
H12D C12 H12E 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
O11 H11A O2 0.842(10) 2.155(17) 2.981(5) 167(6) 4_676 yes
O11 H11B O5 0.842(10) 1.986(14) 2.823(4) 172(7) . yes
N2 H2A O6 0.89(6) 2.16(6) 2.911(5) 142(5) . yes
N2 H2A O7 0.89(6) 2.15(5) 2.877(5) 138(4) 2_746 yes
N2 H2B O10 0.93(6) 2.37(5) 2.857(5) 113(4) 3_766 yes
N2 H2B O13 0.93(6) 1.91(6) 2.779(6) 154(5) . yes
C2 H2C O2 0.99 2.60 3.281(4) 126.1 3_676 yes
C3 H3A O12 0.99 2.48 3.353(6) 146.2 . yes
C6 H6A O10 0.99 2.53 3.060(5) 113.0 . yes
C6 H6B O9 0.99 2.54 3.106(5) 116.3 4_676 yes
C9 H9B O9 0.99 2.51 3.255(5) 131.5 4_676 yes
C12 H12E O12 0.98 2.53 3.349(7) 141.6 1_655 yes

####################################################################### 
# 
# 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 2264774'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2023-05-23 deposited with the CCDC.	2023-06-21 downloaded from the CCDC.
;

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H13 O9 P U'
_chemical_formula_iupac          ?
_chemical_formula_weight         534.19

_chemical_melting_point          ?

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

_cell_length_a                   7.3820(5)
_cell_length_b                   23.3063(18)
_cell_length_c                   8.5496(7)
_cell_angle_alpha                90
_cell_angle_beta                 113.584(2)
_cell_angle_gamma                90
_cell_volume                     1348.07(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9688
_cell_measurement_theta_min      2.7427
_cell_measurement_theta_max      30.5663
_cell_measurement_temperature    100(2)

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.037
_exptl_crystal_density_diffrn    2.632
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             984

_exptl_absorpt_coefficient_mu    12.199
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_T_max  0.75

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100(2)

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

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

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

_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_detector_area_resol_mean 7.41

_diffrn_reflns_number            44893
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_theta_min         2.74
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_full        28.70
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11

_refine_special_details          
;
The H atom bounf to O8 was found and refined with a restraint 
on the bond length and with an isotropic displacement
parameter equal to 1.2 times that of O8.
;

_reflns_number_total             3476
_reflns_number_gt                3338
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0224
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0516
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.095
_refine_ls_number_reflns         3476
_refine_ls_number_parameters     184
_refine_ls_number_restraints     1
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+9.6135P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.370
_refine_diff_density_min         -1.564
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U U1 0.27428(2) 0.66922(2) 0.17881(2) 0.00870(5) Uani d . . . 1 . .
P P1 0.65705(14) 0.62317(4) 0.58782(12) 0.00959(17) Uani d . . . 1 . .
O O1 0.0894(4) 0.61537(12) 0.1239(4) 0.0141(5) Uani d . . . 1 . .
O O2 0.4590(4) 0.72310(12) 0.2248(4) 0.0152(6) Uani d . . . 1 . .
O O3 0.4653(4) 0.62278(12) 0.4282(4) 0.0139(5) Uani d . . . 1 . .
O O4 0.4993(4) 0.60462(13) 1.0959(4) 0.0149(6) Uani d . . . 1 . .
O O5 0.2701(4) 0.65473(13) 0.8949(4) 0.0153(6) Uani d . . . 1 . .
O O6 1.0312(4) 0.76625(12) 0.5123(4) 0.0135(5) Uani d . . . 1 . .
O O7 1.1636(4) 0.71090(13) 0.3749(4) 0.0167(6) Uani d . . . 1 . .
O O8 1.2312(5) 0.48316(15) 0.8677(5) 0.0278(7) Uani d . . D 1 . .
H H8 1.286(8) 0.4521(16) 0.842(8) 0.033000 Uiso d U . D 1 . .
O O9 0.9871(6) 0.45635(14) 0.6217(4) 0.0256(7) Uani d . . . 1 . .
C C1 0.6107(6) 0.63891(17) 0.7734(5) 0.0128(7) Uani d . . . 1 . .
H H1A 0.738099 0.639845 0.874309 0.015000 Uiso calc U . R 1 . .
H H1B 0.550273 0.677480 0.760550 0.015000 Uiso calc U . R 1 . .
C C2 0.4735(6) 0.59496(18) 0.8047(5) 0.0151(7) Uani d . . . 1 . .
H H2A 0.355881 0.588049 0.697777 0.018000 Uiso calc U . R 1 . .
H H2B 0.543739 0.558070 0.843356 0.018000 Uiso calc U . R 1 . .
C C3 0.4115(6) 0.61869(16) 0.9392(5) 0.0132(7) Uani d . . . 1 . .
C C4 0.8268(6) 0.67774(16) 0.5835(5) 0.0130(7) Uani d . . . 1 . .
H H4A 0.759275 0.715353 0.566809 0.016000 Uiso calc U . R 1 . .
H H4B 0.939293 0.678634 0.696376 0.016000 Uiso calc U . R 1 . .
C C5 0.9090(6) 0.67070(17) 0.4458(6) 0.0147(8) Uani d . . . 1 . .
H H5A 0.982386 0.634017 0.464925 0.018000 Uiso calc U . R 1 . .
H H5B 0.797245 0.668547 0.332691 0.018000 Uiso calc U . R 1 . .
C C6 1.0442(6) 0.71884(16) 0.4439(5) 0.0105(7) Uani d . . . 1 . .
C C7 0.7596(6) 0.55265(17) 0.6065(5) 0.0145(7) Uani d . . . 1 . .
H H7A 0.659524 0.524735 0.608679 0.017000 Uiso calc U . R 1 . .
H H7B 0.783919 0.544733 0.502770 0.017000 Uiso calc U . R 1 . .
C C8 0.9497(7) 0.5419(2) 0.7610(6) 0.0218(9) Uani d . . . 1 . .
H H8A 1.037837 0.575575 0.779581 0.026000 Uiso calc U . R 1 . .
H H8B 0.919519 0.537425 0.863167 0.026000 Uiso calc U . R 1 . .
C C9 1.0551(7) 0.48901(19) 0.7395(6) 0.0209(9) Uani d . . . 1 . .


_geom_special_details            
;

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
U1 O1 . 1.774(3) ?
U1 O2 . 1.778(3) ?
U1 O3 . 2.302(3) ?
U1 O6 4_475 2.337(3) ?
U1 O7 1_455 2.349(3) ?
U1 O5 1_554 2.439(3) ?
U1 O4 1_554 2.544(3) ?
P1 O3 . 1.523(3) ?
P1 C7 . 1.790(4) ?
P1 C1 . 1.790(4) ?
P1 C4 . 1.796(4) ?
O4 C3 . 1.276(5) ?
O5 C3 . 1.274(5) ?
O6 C6 . 1.272(5) ?
O7 C6 . 1.255(5) ?
O8 C9 . 1.330(6) ?
O8 H8 . 0.900(10) ?
O9 C9 . 1.201(6) ?
C1 C2 . 1.537(5) ?
C1 H1A . 0.990000 ?
C1 H1B . 0.990000 ?
C2 C3 . 1.503(5) ?
C2 H2A . 0.990000 ?
C2 H2B . 0.990000 ?
C4 C5 . 1.534(5) ?
C4 H4A . 0.990000 ?
C4 H4B . 0.990000 ?
C5 C6 . 1.506(5) ?
C5 H5A . 0.990000 ?
C5 H5B . 0.990000 ?
C7 C8 . 1.515(6) ?
C7 H7A . 0.990000 ?
C7 H7B . 0.990000 ?
C8 C9 . 1.508(6) ?
C8 H8A . 0.990000 ?
C8 H8B . 0.990000 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 U1 O2 . . 177.58(13) ?
O1 U1 O3 . . 91.93(12) ?
O2 U1 O3 . . 89.75(12) ?
O1 U1 O6 . 4_475 88.40(12) ?
O2 U1 O6 . 4_475 90.82(12) ?
O3 U1 O6 . 4_475 154.56(10) ?
O1 U1 O7 . 1_455 91.76(12) ?
O2 U1 O7 . 1_455 90.28(12) ?
O3 U1 O7 . 1_455 78.04(11) ?
O6 U1 O7 4_475 1_455 76.53(10) ?
O1 U1 O5 . 1_554 86.38(12) ?
O2 U1 O5 . 1_554 91.21(12) ?
O3 U1 O5 . 1_554 128.00(10) ?
O6 U1 O5 4_475 1_554 77.41(10) ?
O7 U1 O5 1_455 1_554 153.92(10) ?
O1 U1 O4 . 1_554 91.53(11) ?
O2 U1 O4 . 1_554 87.20(12) ?
O3 U1 O4 . 1_554 75.73(10) ?
O6 U1 O4 4_475 1_554 129.70(9) ?
O7 U1 O4 1_455 1_554 153.65(10) ?
O5 U1 O4 1_554 1_554 52.42(9) ?
O3 P1 C7 . . 106.41(18) ?
O3 P1 C1 . . 110.91(18) ?
C7 P1 C1 . . 109.46(19) ?
O3 P1 C4 . . 113.05(18) ?
C7 P1 C4 . . 112.25(19) ?
C1 P1 C4 . . 104.80(18) ?
P1 O3 U1 . . 146.34(17) ?
C3 O4 U1 . 1_556 91.5(2) ?
C3 O5 U1 . 1_556 96.5(2) ?
C6 O6 U1 . 4_676 131.2(3) ?
C6 O7 U1 . 1_655 155.0(3) ?
C9 O8 H8 . . 106.(4) ?
C2 C1 P1 . . 113.0(3) ?
C2 C1 H1A . . 109.000000 ?
P1 C1 H1A . . 109.000000 ?
C2 C1 H1B . . 109.000000 ?
P1 C1 H1B . . 109.000000 ?
H1A C1 H1B . . 107.800000 ?
C3 C2 C1 . . 108.1(3) ?
C3 C2 H2A . . 110.100000 ?
C1 C2 H2A . . 110.100000 ?
C3 C2 H2B . . 110.100000 ?
C1 C2 H2B . . 110.100000 ?
H2A C2 H2B . . 108.400000 ?
O5 C3 O4 . . 119.5(4) ?
O5 C3 C2 . . 118.7(4) ?
O4 C3 C2 . . 121.8(4) ?
C5 C4 P1 . . 115.7(3) ?
C5 C4 H4A . . 108.400000 ?
P1 C4 H4A . . 108.400000 ?
C5 C4 H4B . . 108.400000 ?
P1 C4 H4B . . 108.400000 ?
H4A C4 H4B . . 107.400000 ?
C6 C5 C4 . . 113.3(3) ?
C6 C5 H5A . . 108.900000 ?
C4 C5 H5A . . 108.900000 ?
C6 C5 H5B . . 108.900000 ?
C4 C5 H5B . . 108.900000 ?
H5A C5 H5B . . 107.700000 ?
O7 C6 O6 . . 122.7(4) ?
O7 C6 C5 . . 119.2(3) ?
O6 C6 C5 . . 118.0(3) ?
C8 C7 P1 . . 116.1(3) ?
C8 C7 H7A . . 108.300000 ?
P1 C7 H7A . . 108.300000 ?
C8 C7 H7B . . 108.300000 ?
P1 C7 H7B . . 108.300000 ?
H7A C7 H7B . . 107.400000 ?
C9 C8 C7 . . 111.8(4) ?
C9 C8 H8A . . 109.200000 ?
C7 C8 H8A . . 109.300000 ?
C9 C8 H8B . . 109.200000 ?
C7 C8 H8B . . 109.200000 ?
H8A C8 H8B . . 107.900000 ?
O9 C9 O8 . . 124.7(4) ?
O9 C9 C8 . . 123.9(4) ?
O8 C9 C8 . . 111.4(4) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O8 H8 O4 3_767 0.900(10) 1.97(3) 2.783(4) 150(6) ?
C1 H1B O2 4_576 0.990000 2.400000 3.376(5) 169 ?
C2 H2B O8 3_767 0.990000 2.550000 3.321(6) 135 ?
C4 H4B O5 1_655 0.990000 2.420000 3.334(5) 154 ?
C5 H5A O9 3_766 0.990000 2.270000 3.169(5) 150 ?
C7 H7B O9 3_766 0.990000 2.330000 3.204(5) 147 ?
C8 H8A O5 1_655 0.990000 2.440000 3.413(6) 167 ?

####################################################################### 
# 
# 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 2264769'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2023-05-23 deposited with the CCDC.	2023-06-21 downloaded from the CCDC.
;

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H38 N8 O21 U2'
_chemical_formula_iupac          ?
_chemical_formula_weight         1226.66
_chemical_absolute_configuration unk

_chemical_melting_point          ?

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

_cell_length_a                   11.6822(6)
_cell_length_b                   15.3912(8)
_cell_length_c                   11.7959(5)
_cell_angle_alpha                90
_cell_angle_beta                 115.5602(16)
_cell_angle_gamma                90
_cell_volume                     1913.37(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9645
_cell_measurement_theta_min      2.4408
_cell_measurement_theta_max      30.5237
_cell_measurement_temperature    100(2)

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.091
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.045
_exptl_crystal_density_diffrn    2.129
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1156

_exptl_absorpt_coefficient_mu    8.542
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_T_max  0.75

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100(2)

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

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

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

_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_detector_area_resol_mean 7.41

_diffrn_reflns_number            46015
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_theta_min         2.05
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14

_refine_special_details          
;
The H atoms bound to O21 were found and refined with restraints
on bond lengths and angle. The H atoms of the guanidinium
cations were introduced at calculated positions and treated
as riding atoms. Some voids indicate the presence of unresolved
solvent molecules whose contribution to the structure factors
were subtracted with SQUEEZE.

ADDSYM suggests space group P21/c with 86% fit, but no
satisfying refinement can be made in this space group.

Refined as a 2-component inversion twin.
;

_reflns_number_total             7198
_reflns_number_gt                7097
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0750
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_number_reflns         7198
_refine_ls_number_parameters     485
_refine_ls_number_restraints     4
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0538P)²+1.0223P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.591
_refine_diff_density_min         -0.724
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.416(11)

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

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

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U U1 0.83068(2) 0.61088(2) 1.16479(2) 0.02678(10) Uani d . . . 1 . .
U U2 0.32647(2) 0.49201(2) 0.17591(2) 0.02622(10) Uani d . . . 1 . .
O O1 0.9135(6) 0.6164(10) 1.0677(6) 0.0307(16) Uani d . . . 1 . .
O O2 0.7456(6) 0.6120(12) 1.2601(7) 0.0384(15) Uani d . . . 1 . .
O O3 0.3995(7) 0.4928(12) 0.0726(6) 0.0376(16) Uani d . . . 1 . .
O O4 0.2550(7) 0.4987(11) 0.2802(7) 0.0371(19) Uani d . . . 1 . .
O O5 0.7193(11) 0.4774(7) 1.0578(9) 0.041(3) Uani d . . . 1 . .
O O6 0.6245(6) 0.5992(7) 0.9729(6) 0.035(2) Uani d . . . 1 . .
O O7 0.2688(11) 0.2504(8) 0.9081(9) 0.036(2) Uani d . . . 1 . .
O O8 0.0827(11) 0.2513(8) 0.7453(10) 0.039(2) Uani d . . . 1 . .
O O9 0.0387(6) 0.5936(5) 0.3503(6) 0.032(2) Uani d . . . 1 . .
O O10 -0.0675(11) 0.4746(8) 0.2734(9) 0.037(3) Uani d . . . 1 . .
O O11 0.4623(7) 0.4932(8) 0.5707(7) 0.0562(18) Uani d . . . 1 . .
O O12 0.4186(8) 0.3582(6) 0.5721(9) 0.054(2) Uani d . . . 1 . .
O O13 0.4393(10) 0.6240(8) 0.2810(9) 0.032(2) Uani d . . . 1 . .
O O14 0.5448(6) 0.5027(7) 0.3508(6) 0.0294(17) Uani d . . . 1 . .
O O15 0.5857(10) 0.8460(7) 0.7442(9) 0.036(2) Uani d . . . 1 . .
O O16 0.7781(10) 0.8492(7) 0.8910(8) 0.039(2) Uani d . . . 1 . .
O O17 1.1233(6) 0.5040(7) 0.9873(6) 0.037(2) Uani d . . . 1 . .
O O18 1.2160(11) 0.6252(8) 1.0760(10) 0.034(2) Uani d . . . 1 . .
O O19 0.9672(8) 0.5978(8) 0.5699(8) 0.066(3) Uani d . . . 1 . .
O O20 0.9376(10) 0.7339(8) 0.5739(10) 0.067(3) Uani d . . . 1 . .
O O21 -0.2706(8) 0.3982(5) 0.3181(8) 0.0450(18) Uani d . . D 1 . .
H H21A -0.226(10) 0.432(5) 0.298(12) 0.068000 Uiso d U . D 1 . .
H H21B -0.320(8) 0.431(6) 0.334(11) 0.068000 Uiso d U . D 1 . .
N N1 0.4086(7) 0.4355(6) 0.5974(7) 0.0377(19) Uani d . . . 1 . .
N N2 0.9200(7) 0.6611(7) 0.5976(7) 0.042(2) Uani d . . . 1 . .
N N3 0.7177(8) 0.2891(5) 1.0357(9) 0.050(2) Uani d . . . 1 . .
H H3A 0.751921 0.265732 0.989441 0.060000 Uiso calc U . R 1 . .
H H3B 0.758307 0.330169 1.090123 0.060000 Uiso calc U . R 1 . .
N N4 0.5507(8) 0.2962(5) 1.0911(8) 0.047(2) Uani d . . . 1 . .
H H4A 0.475775 0.278581 1.082594 0.056000 Uiso calc U . R 1 . .
H H4B 0.591174 0.337345 1.145600 0.056000 Uiso calc U . R 1 . .
N N5 0.5461(9) 0.2019(6) 0.9436(9) 0.052(2) Uani d . . . 1 . .
H H5A 0.471088 0.183213 0.933337 0.062000 Uiso calc U . R 1 . .
H H5B 0.582543 0.179484 0.898761 0.062000 Uiso calc U . R 1 . .
N N6 0.2421(10) 0.7073(7) 0.3460(10) 0.054(3) Uani d . . . 1 . .
H H6A 0.171437 0.676952 0.312561 0.065000 Uiso calc U . R 1 . .
H H6B 0.294352 0.707762 0.310121 0.065000 Uiso calc U . R 1 . .
N N7 0.3759(8) 0.7983(6) 0.4951(9) 0.054(2) Uani d . . . 1 . .
H H7A 0.425239 0.798316 0.456052 0.065000 Uiso calc U . R 1 . .
H H7B 0.397035 0.829005 0.564242 0.065000 Uiso calc U . R 1 . .
N N8 0.1930(10) 0.7529(7) 0.5061(10) 0.061(3) Uani d . . . 1 . .
H H8A 0.121906 0.722945 0.474162 0.073000 Uiso calc U . R 1 . .
H H8B 0.213180 0.783246 0.575259 0.073000 Uiso calc U . R 1 . .
C C1 0.3280(6) 0.4574(8) 0.6680(7) 0.027(2) Uani d . . . 1 . .
C C2 0.4116(8) 0.5134(5) 0.7781(8) 0.031(2) Uani d . . . 1 . .
H H2A 0.361393 0.534824 0.821913 0.037000 Uiso calc U . R 1 . .
H H2B 0.440765 0.564460 0.746745 0.037000 Uiso calc U . R 1 . .
C C3 0.5269(9) 0.4634(7) 0.8713(9) 0.035(2) Uani d . . . 1 . .
H H3C 0.496966 0.418310 0.912080 0.042000 Uiso calc U . R 1 . .
H H3D 0.567030 0.433089 0.823614 0.042000 Uiso calc U . R 1 . .
C C4 0.6273(9) 0.5176(6) 0.9731(8) 0.027(2) Uani d . . . 1 . .
C C5 0.2867(8) 0.3732(6) 0.7057(8) 0.0304(19) Uani d . . . 1 . .
H H5C 0.235966 0.339848 0.628326 0.036000 Uiso calc U . R 1 . .
H H5D 0.363603 0.338579 0.755557 0.036000 Uiso calc U . R 1 . .
C C6 0.2102(10) 0.3815(7) 0.7804(9) 0.036(2) Uani d . . . 1 . .
H H6C 0.258005 0.415863 0.857495 0.044000 Uiso calc U . R 1 . .
H H6D 0.129310 0.411754 0.729918 0.044000 Uiso calc U . R 1 . .
C C7 0.1841(9) 0.2920(6) 0.8149(8) 0.034(2) Uani d . . . 1 . .
C C8 0.2168(9) 0.5107(6) 0.5734(8) 0.033(2) Uani d . . . 1 . .
H H8C 0.172249 0.538918 0.618460 0.039000 Uiso calc U . R 1 . .
H H8D 0.251120 0.557359 0.539025 0.039000 Uiso calc U . R 1 . .
C C9 0.1204(9) 0.4581(7) 0.4639(9) 0.031(2) Uani d . . . 1 . .
H H9A 0.166679 0.419652 0.430623 0.037000 Uiso calc U . R 1 . .
H H9B 0.071782 0.420615 0.495786 0.037000 Uiso calc U . R 1 . .
C C10 0.0273(9) 0.5138(6) 0.3566(8) 0.024(2) Uani d . . . 1 . .
C C11 0.8380(8) 0.6414(8) 0.6680(8) 0.034(3) Uani d . . . 1 . .
C C12 0.7252(8) 0.5853(6) 0.5769(8) 0.031(2) Uani d . . . 1 . .
H H12A 0.758796 0.534971 0.548550 0.037000 Uiso calc U . R 1 . .
H H12B 0.677544 0.562722 0.622537 0.037000 Uiso calc U . R 1 . .
C C13 0.6349(10) 0.6361(6) 0.4623(9) 0.032(2) Uani d . . . 1 . .
H H13A 0.591813 0.680741 0.490550 0.038000 Uiso calc U . R 1 . .
H H13B 0.685578 0.666919 0.425883 0.038000 Uiso calc U . R 1 . .
C C14 0.5349(10) 0.5829(8) 0.3602(9) 0.038(3) Uani d . . . 1 . .
C C15 0.7978(9) 0.7291(6) 0.7000(8) 0.0291(18) Uani d . . . 1 . .
H H15A 0.749181 0.761554 0.621263 0.035000 Uiso calc U . R 1 . .
H H15B 0.874527 0.763326 0.751342 0.035000 Uiso calc U . R 1 . .
C C16 0.7156(9) 0.7195(7) 0.7728(9) 0.031(2) Uani d . . . 1 . .
H H16A 0.634695 0.689954 0.719930 0.037000 Uiso calc U . R 1 . .
H H16B 0.761017 0.684800 0.849976 0.037000 Uiso calc U . R 1 . .
C C17 0.6902(8) 0.8103(6) 0.8060(8) 0.0319(19) Uani d . . . 1 . .
C C18 0.9216(8) 0.5873(6) 0.7852(8) 0.032(2) Uani d . . . 1 . .
H H18A 0.951188 0.534583 0.757663 0.038000 Uiso calc U . R 1 . .
H H18B 0.869100 0.568195 0.827795 0.038000 Uiso calc U . R 1 . .
C C19 1.0385(10) 0.6374(6) 0.8807(9) 0.033(2) Uani d . . . 1 . .
H H19A 1.084667 0.662618 0.835210 0.039000 Uiso calc U . R 1 . .
H H19B 1.008098 0.686205 0.915167 0.039000 Uiso calc U . R 1 . .
C C20 1.1275(10) 0.5856(7) 0.9855(9) 0.036(3) Uani d . . . 1 . .
C C21 0.6018(10) 0.2615(6) 1.0231(9) 0.040(2) Uani d . . . 1 . .
C C22 0.2697(9) 0.7522(6) 0.4499(9) 0.041(2) Uani d . . . 1 . .


_geom_special_details            
;

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
U1 O1 . 1.791(7) ?
U1 O2 . 1.793(7) ?
U1 O7 2_657 2.416(12) ?
U1 O8 2_657 2.427(12) ?
U1 O5 . 2.468(11) ?
U1 O10 1_656 2.478(11) ?
U1 O9 1_656 2.485(6) ?
U1 O6 . 2.501(6) ?
U2 O4 . 1.763(7) ?
U2 O3 . 1.763(6) ?
U2 O18 1_454 2.438(12) ?
U2 O13 . 2.447(12) ?
U2 O17 1_454 2.462(6) ?
U2 O16 2_646 2.473(11) ?
U2 O15 2_646 2.481(11) ?
U2 O14 . 2.499(6) ?
O5 C4 . 1.268(14) ?
O6 C4 . 1.257(14) ?
O7 C7 . 1.288(14) ?
O8 C7 . 1.277(15) ?
O9 C10 . 1.240(12) ?
O10 C10 . 1.272(14) ?
O11 N1 . 1.205(13) ?
O12 N1 . 1.244(13) ?
O13 C14 . 1.273(15) ?
O14 C14 . 1.249(16) ?
O15 C17 . 1.248(13) ?
O16 C17 . 1.237(14) ?
O17 C20 . 1.258(16) ?
O18 C20 . 1.276(15) ?
O19 N2 . 1.232(13) ?
O20 N2 . 1.194(14) ?
O21 H21A . 0.845(15) ?
O21 H21B . 0.846(15) ?
N1 C1 . 1.540(11) ?
N2 C11 . 1.545(12) ?
N3 C21 . 1.365(13) ?
N3 H3A . 0.880000 ?
N3 H3B . 0.880000 ?
N4 C21 . 1.304(13) ?
N4 H4A . 0.880000 ?
N4 H4B . 0.880000 ?
N5 C21 . 1.271(13) ?
N5 H5A . 0.880000 ?
N5 H5B . 0.880000 ?
N6 C22 . 1.321(13) ?
N6 H6A . 0.880000 ?
N6 H6B . 0.880000 ?
N7 C22 . 1.325(12) ?
N7 H7A . 0.880000 ?
N7 H7B . 0.880000 ?
N8 C22 . 1.324(14) ?
N8 H8A . 0.880000 ?
N8 H8B . 0.880000 ?
C1 C2 . 1.513(12) ?
C1 C5 . 1.515(15) ?
C1 C8 . 1.535(12) ?
C2 C3 . 1.529(12) ?
C2 H2A . 0.990000 ?
C2 H2B . 0.990000 ?
C3 C4 . 1.516(12) ?
C3 H3C . 0.990000 ?
C3 H3D . 0.990000 ?
C5 C6 . 1.507(13) ?
C5 H5C . 0.990000 ?
C5 H5D . 0.990000 ?
C6 C7 . 1.504(15) ?
C6 H6C . 0.990000 ?
C6 H6D . 0.990000 ?
C8 C9 . 1.529(13) ?
C8 H8C . 0.990000 ?
C8 H8D . 0.990000 ?
C9 C10 . 1.527(12) ?
C9 H9A . 0.990000 ?
C9 H9B . 0.990000 ?
C11 C15 . 1.529(15) ?
C11 C18 . 1.546(12) ?
C11 C12 . 1.554(13) ?
C12 C13 . 1.523(13) ?
C12 H12A . 0.990000 ?
C12 H12B . 0.990000 ?
C13 C14 . 1.507(14) ?
C13 H13A . 0.990000 ?
C13 H13B . 0.990000 ?
C15 C16 . 1.546(12) ?
C15 H15A . 0.990000 ?
C15 H15B . 0.990000 ?
C16 C17 . 1.514(14) ?
C16 H16A . 0.990000 ?
C16 H16B . 0.990000 ?
C18 C19 . 1.550(12) ?
C18 H18A . 0.990000 ?
C18 H18B . 0.990000 ?
C19 C20 . 1.461(14) ?
C19 H19A . 0.990000 ?
C19 H19B . 0.990000 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 U1 O2 . . 176.6(10) ?
O1 U1 O7 . 2_657 92.3(5) ?
O2 U1 O7 . 2_657 84.4(6) ?
O1 U1 O8 . 2_657 89.9(5) ?
O2 U1 O8 . 2_657 87.6(6) ?
O7 U1 O8 2_657 2_657 53.9(5) ?
O1 U1 O5 . . 91.4(5) ?
O2 U1 O5 . . 90.9(6) ?
O7 U1 O5 2_657 . 119.4(3) ?
O8 U1 O5 2_657 . 173.2(4) ?
O1 U1 O10 . 1_656 95.7(5) ?
O2 U1 O10 . 1_656 87.5(6) ?
O7 U1 O10 2_657 1_656 170.4(3) ?
O8 U1 O10 2_657 1_656 120.7(2) ?
O5 U1 O10 . 1_656 65.7(5) ?
O1 U1 O9 . 1_656 88.6(3) ?
O2 U1 O9 . 1_656 92.6(3) ?
O7 U1 O9 2_657 1_656 123.1(3) ?
O8 U1 O9 2_657 1_656 69.2(3) ?
O5 U1 O9 . 1_656 117.4(3) ?
O10 U1 O9 1_656 1_656 52.1(3) ?
O1 U1 O6 . . 90.0(3) ?
O2 U1 O6 . . 89.4(3) ?
O7 U1 O6 2_657 . 67.3(4) ?
O8 U1 O6 2_657 . 121.1(4) ?
O5 U1 O6 . . 52.3(3) ?
O10 U1 O6 1_656 . 117.9(4) ?
O9 U1 O6 1_656 . 169.6(4) ?
O4 U2 O3 . . 176.2(11) ?
O4 U2 O18 . 1_454 88.7(6) ?
O3 U2 O18 . 1_454 88.5(6) ?
O4 U2 O13 . . 85.0(5) ?
O3 U2 O13 . . 91.7(6) ?
O18 U2 O13 1_454 . 66.7(4) ?
O4 U2 O17 . 1_454 93.7(3) ?
O3 U2 O17 . 1_454 86.6(3) ?
O18 U2 O17 1_454 1_454 53.0(4) ?
O13 U2 O17 . 1_454 119.6(3) ?
O4 U2 O16 . 2_646 87.5(5) ?
O3 U2 O16 . 2_646 96.0(6) ?
O18 U2 O16 1_454 2_646 120.5(2) ?
O13 U2 O16 . 2_646 169.5(3) ?
O17 U2 O16 1_454 2_646 68.1(3) ?
O4 U2 O15 . 2_646 91.8(6) ?
O3 U2 O15 . 2_646 91.4(6) ?
O18 U2 O15 1_454 2_646 172.3(4) ?
O13 U2 O15 . 2_646 121.0(3) ?
O17 U2 O15 1_454 2_646 119.4(4) ?
O16 U2 O15 2_646 2_646 51.9(4) ?
O4 U2 O14 . . 92.4(3) ?
O3 U2 O14 . . 86.8(3) ?
O18 U2 O14 1_454 . 118.8(3) ?
O13 U2 O14 . . 52.6(3) ?
O17 U2 O14 1_454 . 169.6(3) ?
O16 U2 O14 2_646 . 120.6(3) ?
O15 U2 O14 2_646 . 68.8(3) ?
C4 O5 U1 . . 94.4(7) ?
C4 O6 U1 . . 93.2(6) ?
C7 O7 U1 . 2_647 93.7(7) ?
C7 O8 U1 . 2_647 93.4(7) ?
C10 O9 U1 . 1_454 94.0(6) ?
C10 O10 U1 . 1_454 93.5(7) ?
C14 O13 U2 . . 94.0(9) ?
C14 O14 U2 . . 92.2(6) ?
C17 O15 U2 . 2_656 92.1(7) ?
C17 O16 U2 . 2_656 92.8(7) ?
C20 O17 U2 . 1_656 93.5(6) ?
C20 O18 U2 . 1_656 94.1(8) ?
H21A O21 H21B . . 106.(2) ?
O11 N1 O12 . . 121.9(9) ?
O11 N1 C1 . . 119.3(9) ?
O12 N1 C1 . . 118.9(9) ?
O20 N2 O19 . . 122.6(10) ?
O20 N2 C11 . . 121.3(10) ?
O19 N2 C11 . . 116.0(10) ?
C21 N3 H3A . . 120.000000 ?
C21 N3 H3B . . 120.000000 ?
H3A N3 H3B . . 120.000000 ?
C21 N4 H4A . . 120.000000 ?
C21 N4 H4B . . 120.000000 ?
H4A N4 H4B . . 120.000000 ?
C21 N5 H5A . . 120.000000 ?
C21 N5 H5B . . 120.000000 ?
H5A N5 H5B . . 120.000000 ?
C22 N6 H6A . . 120.000000 ?
C22 N6 H6B . . 120.000000 ?
H6A N6 H6B . . 120.000000 ?
C22 N7 H7A . . 120.000000 ?
C22 N7 H7B . . 120.000000 ?
H7A N7 H7B . . 120.000000 ?
C22 N8 H8A . . 120.000000 ?
C22 N8 H8B . . 120.000000 ?
H8A N8 H8B . . 120.000000 ?
C2 C1 C5 . . 113.9(7) ?
C2 C1 C8 . . 110.5(9) ?
C5 C1 C8 . . 113.2(7) ?
C2 C1 N1 . . 105.7(6) ?
C5 C1 N1 . . 108.5(8) ?
C8 C1 N1 . . 104.3(7) ?
C1 C2 C3 . . 111.9(7) ?
C1 C2 H2A . . 109.200000 ?
C3 C2 H2A . . 109.200000 ?
C1 C2 H2B . . 109.200000 ?
C3 C2 H2B . . 109.200000 ?
H2A C2 H2B . . 107.900000 ?
C4 C3 C2 . . 115.6(8) ?
C4 C3 H3C . . 108.400000 ?
C2 C3 H3C . . 108.400000 ?
C4 C3 H3D . . 108.400000 ?
C2 C3 H3D . . 108.400000 ?
H3C C3 H3D . . 107.400000 ?
O6 C4 O5 . . 120.1(10) ?
O6 C4 C3 . . 122.5(9) ?
O5 C4 C3 . . 117.3(9) ?
C6 C5 C1 . . 116.3(8) ?
C6 C5 H5C . . 108.200000 ?
C1 C5 H5C . . 108.200000 ?
C6 C5 H5D . . 108.200000 ?
C1 C5 H5D . . 108.200000 ?
H5C C5 H5D . . 107.400000 ?
C7 C6 C5 . . 108.8(8) ?
C7 C6 H6C . . 109.900000 ?
C5 C6 H6C . . 109.900000 ?
C7 C6 H6D . . 109.900000 ?
C5 C6 H6D . . 109.900000 ?
H6C C6 H6D . . 108.300000 ?
O8 C7 O7 . . 117.5(13) ?
O8 C7 C6 . . 121.1(9) ?
O7 C7 C6 . . 121.0(10) ?
C9 C8 C1 . . 114.5(8) ?
C9 C8 H8C . . 108.600000 ?
C1 C8 H8C . . 108.600000 ?
C9 C8 H8D . . 108.600000 ?
C1 C8 H8D . . 108.600000 ?
H8C C8 H8D . . 107.600000 ?
C10 C9 C8 . . 113.8(8) ?
C10 C9 H9A . . 108.800000 ?
C8 C9 H9A . . 108.800000 ?
C10 C9 H9B . . 108.800000 ?
C8 C9 H9B . . 108.800000 ?
H9A C9 H9B . . 107.700000 ?
O9 C10 O10 . . 120.2(10) ?
O9 C10 C9 . . 123.3(9) ?
O10 C10 C9 . . 116.4(9) ?
C15 C11 N2 . . 106.7(9) ?
C15 C11 C18 . . 113.4(7) ?
N2 C11 C18 . . 106.7(7) ?
C15 C11 C12 . . 113.7(7) ?
N2 C11 C12 . . 105.9(7) ?
C18 C11 C12 . . 109.9(9) ?
C13 C12 C11 . . 112.7(8) ?
C13 C12 H12A . . 109.100000 ?
C11 C12 H12A . . 109.100000 ?
C13 C12 H12B . . 109.100000 ?
C11 C12 H12B . . 109.100000 ?
H12A C12 H12B . . 107.800000 ?
C14 C13 C12 . . 115.6(8) ?
C14 C13 H13A . . 108.400000 ?
C12 C13 H13A . . 108.400000 ?
C14 C13 H13B . . 108.400000 ?
C12 C13 H13B . . 108.400000 ?
H13A C13 H13B . . 107.500000 ?
O14 C14 O13 . . 120.7(11) ?
O14 C14 C13 . . 122.6(9) ?
O13 C14 C13 . . 116.6(11) ?
C11 C15 C16 . . 112.6(8) ?
C11 C15 H15A . . 109.100000 ?
C16 C15 H15A . . 109.100000 ?
C11 C15 H15B . . 109.100000 ?
C16 C15 H15B . . 109.100000 ?
H15A C15 H15B . . 107.800000 ?
C17 C16 C15 . . 107.1(8) ?
C17 C16 H16A . . 110.300000 ?
C15 C16 H16A . . 110.300000 ?
C17 C16 H16B . . 110.300000 ?
C15 C16 H16B . . 110.300000 ?
H16A C16 H16B . . 108.500000 ?
O16 C17 O15 . . 121.4(12) ?
O16 C17 C16 . . 118.0(9) ?
O15 C17 C16 . . 120.5(9) ?
C11 C18 C19 . . 113.6(8) ?
C11 C18 H18A . . 108.800000 ?
C19 C18 H18A . . 108.800000 ?
C11 C18 H18B . . 108.800000 ?
C19 C18 H18B . . 108.800000 ?
H18A C18 H18B . . 107.700000 ?
C20 C19 C18 . . 115.2(8) ?
C20 C19 H19A . . 108.500000 ?
C18 C19 H19A . . 108.500000 ?
C20 C19 H19B . . 108.500000 ?
C18 C19 H19B . . 108.500000 ?
H19A C19 H19B . . 107.500000 ?
O17 C20 O18 . . 119.1(11) ?
O17 C20 C19 . . 122.7(9) ?
O18 C20 C19 . . 118.2(11) ?
N5 C21 N4 . . 121.7(10) ?
N5 C21 N3 . . 118.2(10) ?
N4 C21 N3 . . 120.1(9) ?
N6 C22 N8 . . 121.4(9) ?
N6 C22 N7 . . 117.7(10) ?
N8 C22 N7 . . 120.8(9) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O21 H21A O10 . 0.845(15) 2.09(4) 2.894(14) 158(10) ?
O21 H21B O14 1_455 0.846(15) 2.01(2) 2.846(12) 172(11) ?
N3 H3A O18 2_747 0.880000 2.380000 3.095(15) 139 ?
N3 H3B O5 . 0.880000 2.310000 2.910(14) 125 ?
N4 H4A O7 . 0.880000 2.440000 3.142(14) 137 ?
N4 H4B O21 1_656 0.880000 2.190000 3.027(12) 159 ?
N5 H5A O6 2_647 0.880000 2.280000 3.023(13) 142 ?
N5 H5A O7 . 0.880000 2.480000 3.171(15) 136 ?
N5 H5B O13 2_646 0.880000 2.200000 2.979(14) 148 ?
N5 H5B O18 2_747 0.880000 2.390000 3.118(15) 140 ?
N6 H6B O13 . 0.880000 2.270000 3.011(15) 142 ?
N6 H6A O9 . 0.880000 2.200000 2.970(13) 146 ?
N7 H7A O12 2_656 0.880000 2.190000 2.980(12) 149 ?
N7 H7B O15 . 0.880000 2.320000 2.994(13) 133 ?
N8 H8B O21 2_556 0.880000 2.110000 2.916(12) 153 ?
N8 H8A O9 . 0.880000 2.410000 3.127(12) 139 ?
C8 H8C O19 1_455 0.990000 2.390000 3.193(13) 138 ?
C12 H12B O11 . 0.990000 2.550000 3.355(12) 138 ?
C13 H13B O2 1_554 0.990000 2.490000 3.188(12) 127 ?


####################################################################### 
# 
# 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 2264771'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2023-05-23 deposited with the CCDC.	2023-06-21 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT306_4                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O23 Check 
RESPONSE: This O atom pertains to a water molecule for which the H
atoms were not found.
;
# end Validation Reply Form

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H46 N6 Ni O23 U2'
_chemical_formula_iupac          ?
_chemical_formula_weight         1513.60
_chemical_absolute_configuration ad

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   12.4106(7)
_cell_length_b                   17.2410(9)
_cell_length_c                   23.5189(14)
_cell_angle_alpha                90
_cell_angle_beta                 102.782(2)
_cell_angle_gamma                90
_cell_volume                     4907.7(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6481
_cell_measurement_theta_min      2.3604
_cell_measurement_theta_max      30.3574
_cell_measurement_temperature    100(2)

_exptl_crystal_description       irregular
_exptl_crystal_colour            'translucent pale pink'
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.036
_exptl_crystal_density_diffrn    2.049
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2896

_exptl_absorpt_coefficient_mu    7.052
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_T_max  0.75

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100(2)

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

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

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

_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_detector_area_resol_mean 7.41

_diffrn_reflns_number            60642
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28

_refine_special_details          
;
The H atoms bound to O21 and O22 were found and treated
as riding atoms. Those of O23 were not found.
;

_reflns_number_total             9277
_reflns_number_gt                9090
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0934
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_number_reflns         9277
_refine_ls_number_parameters     650
_refine_ls_number_restraints     20
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0567P)²+46.6260P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.186
_refine_diff_density_min         -1.145
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
Determined from the refined Flack parameter.
;
_refine_ls_abs_structure_Flack   -0.001(10)

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U U1 0.40793(3) 0.73527(2) 0.47517(2) 0.01182(12) Uani d . . . 1 . .
U U2 0.75299(3) 0.56226(2) 0.64495(2) 0.01324(12) Uani d . . . 1 . .
Ni Ni1 0.37527(12) 0.53744(9) 0.39967(7) 0.0114(3) Uani d . . . 1 . .
O O1 0.3835(8) 0.7723(5) 0.4034(4) 0.021(2) Uani d . . . 1 . .
O O2 0.4361(8) 0.6991(5) 0.5474(4) 0.0197(19) Uani d . . . 1 . .
O O3 0.6999(8) 0.5653(5) 0.5690(5) 0.021(2) Uani d . . . 1 . .
O O4 0.8046(8) 0.5591(6) 0.7221(4) 0.024(2) Uani d . . . 1 . .
O O5 0.2873(7) 0.6264(5) 0.4330(4) 0.0160(17) Uani d . . . 1 . .
O O6 0.2070(9) 0.7154(7) 0.4747(5) 0.023(2) Uani d . . . 1 . .
O O7 -0.1724(8) 0.3557(5) 0.5003(4) 0.021(2) Uani d . . . 1 . .
O O8 0.0064(7) 0.3553(5) 0.5074(4) 0.0207(19) Uani d . . . 1 . .
O O9 -0.3941(8) 0.7151(6) 0.4727(4) 0.0174(19) Uani d . . . 1 . .
O O10 -0.5026(7) 0.6159(5) 0.4478(4) 0.0146(18) Uani d . . . 1 . .
O O11 -0.1335(11) 0.6832(7) 0.3579(5) 0.043(3) Uani d . . . 1 . .
O O12 -0.1513(12) 0.5617(7) 0.3360(5) 0.045(3) Uani d . . . 1 . .
O O13 0.6759(8) 0.4306(5) 0.6474(5) 0.026(2) Uani d . . . 1 . .
O O14 0.8430(9) 0.4383(6) 0.6320(5) 0.028(2) Uani d . . . 1 . .
O O15 0.4480(9) 0.0766(7) 0.6365(6) 0.025(2) Uani d . . . 1 . .
O O16 0.3563(8) 0.1834(5) 0.6409(4) 0.022(2) Uani d . . . 1 . .
O O17 1.1495(8) 0.1765(6) 0.6610(4) 0.022(2) Uani d . . . 1 . .
O O18 1.0629(9) 0.0663(5) 0.6601(5) 0.020(2) Uani d . . . 1 . .
O O19 0.8253(14) 0.0932(11) 0.7615(8) 0.082(6) Uani d . . . 1 . .
O O20 0.7413(14) 0.1933(8) 0.7827(6) 0.056(4) Uani d . . . 1 . .
O O21 0.0655(12) 0.6892(10) 0.3055(7) 0.062(4) Uani d . . D 1 . .
H H21A 0.011849 0.694590 0.321689 0.093000 Uiso d U . DR 1 . .
H H21B 0.075487 0.641845 0.302150 0.093000 Uiso d U . DR 1 . .
O O22 0.6554(10) 0.8289(7) 0.6205(5) 0.040(3) Uani d . . D 1 . .
H H22A 0.612468 0.828509 0.587278 0.060000 Uiso d U . DR 1 . .
H H22B 0.622882 0.854273 0.642396 0.060000 Uiso d U . DR 1 . .
O O23 0.5582(12) 0.8973(9) 0.7039(6) 0.058(4) Uani d . . . 1 . .
N N1 -0.1321(9) 0.6153(8) 0.3716(6) 0.026(3) Uani d . . . 1 . .
N N2 0.7814(10) 0.1547(8) 0.7482(5) 0.029(3) Uani d . . . 1 . .
N N3 0.2346(8) 0.4758(6) 0.3661(4) 0.013(2) Uani d . . . 1 . .
N N4 0.3690(9) 0.4698(6) 0.4695(4) 0.016(2) Uani d . . . 1 . .
N N5 0.3833(8) 0.5955(6) 0.3250(4) 0.015(2) Uani d . . . 1 . .
N N6 0.4898(8) 0.4703(6) 0.3709(4) 0.016(2) Uani d . . . 1 . .
C C1 -0.1075(10) 0.5958(8) 0.4379(6) 0.019(3) Uani d U . . 1 . .
C C2 0.0041(11) 0.6341(8) 0.4622(6) 0.020(3) Uani d . . . 1 . .
H H2A -0.002189 0.690198 0.452974 0.024000 Uiso calc U . R 1 . .
H H2B 0.021559 0.628897 0.505184 0.024000 Uiso calc U . R 1 . .
C C3 0.1000(11) 0.6009(8) 0.4390(7) 0.023(3) Uani d . . . 1 . .
H H3A 0.119990 0.549670 0.457409 0.028000 Uiso calc U . R 1 . .
H H3B 0.074822 0.592397 0.396530 0.028000 Uiso calc U . R 1 . .
C C4 0.2019(10) 0.6510(7) 0.4497(5) 0.016(2) Uani d . . . 1 . .
C C5 -0.1055(11) 0.5069(7) 0.4437(6) 0.016(3) Uani d . . . 1 . .
H H5A -0.177506 0.485707 0.422784 0.019000 Uiso calc U . R 1 . .
H H5B -0.047686 0.485672 0.425020 0.019000 Uiso calc U . R 1 . .
C C6 -0.0826(12) 0.4803(7) 0.5072(6) 0.021(3) Uani d . . . 1 . .
H H6A -0.010232 0.500225 0.528782 0.025000 Uiso calc U . R 1 . .
H H6B -0.140717 0.499739 0.526413 0.025000 Uiso calc U . R 1 . .
C C7 -0.0823(11) 0.3920(8) 0.5063(6) 0.019(3) Uani d . . . 1 . .
C C8 -0.1993(10) 0.6355(7) 0.4613(6) 0.016(2) Uani d U . . 1 . .
H H8A -0.182201 0.630706 0.504264 0.019000 Uiso calc U . R 1 . .
H H8B -0.199968 0.691397 0.451642 0.019000 Uiso calc U . R 1 . .
C C9 -0.3143(11) 0.6022(8) 0.4371(6) 0.019(3) Uani d . . . 1 . .
H H9A -0.327367 0.600643 0.394009 0.023000 Uiso calc U . R 1 . .
H H9B -0.316239 0.548156 0.451005 0.023000 Uiso calc U . R 1 . .
C C10 -0.4063(10) 0.6469(7) 0.4538(5) 0.014(2) Uani d . . . 1 . .
C C11 0.7674(11) 0.1849(8) 0.6859(6) 0.019(3) Uani d . . . 1 . .
C C12 0.7699(11) 0.2737(8) 0.6891(6) 0.018(3) Uani d . . . 1 . .
H H12A 0.707278 0.291848 0.705313 0.021000 Uiso calc U . R 1 . .
H H12B 0.839133 0.290289 0.716021 0.021000 Uiso calc U . R 1 . .
C C13 0.7630(13) 0.3118(8) 0.6296(6) 0.026(3) Uani d . . . 1 . .
H H13A 0.827827 0.296640 0.614009 0.032000 Uiso calc U . R 1 . .
H H13B 0.695470 0.294030 0.601803 0.032000 Uiso calc U . R 1 . .
C C14 0.7601(12) 0.3984(8) 0.6361(6) 0.021(3) Uani d . . . 1 . .
C C15 0.6548(11) 0.1514(8) 0.6531(7) 0.024(3) Uani d . . . 1 . .
H H15A 0.651470 0.153901 0.610693 0.029000 Uiso calc U . R 1 . .
H H15B 0.651473 0.096044 0.663702 0.029000 Uiso calc U . R 1 . .
C C16 0.5542(11) 0.1919(9) 0.6651(7) 0.027(3) Uani d . . . 1 . .
H H16A 0.546814 0.243055 0.645451 0.032000 Uiso calc U . R 1 . .
H H16B 0.566219 0.201461 0.707575 0.032000 Uiso calc U . R 1 . .
C C17 0.4469(11) 0.1480(8) 0.6454(6) 0.020(3) Uani d . . . 1 . .
C C18 0.8588(10) 0.1484(8) 0.6611(6) 0.022(3) Uani d . . . 1 . .
H H18A 0.841643 0.156206 0.618372 0.027000 Uiso calc U . R 1 . .
H H18B 0.859856 0.091884 0.668528 0.027000 Uiso calc U . R 1 . .
C C19 0.9739(11) 0.1813(9) 0.6867(7) 0.024(3) Uani d . . . 1 . .
H H19A 0.975285 0.236620 0.675496 0.029000 Uiso calc U . R 1 . .
H H19B 0.987764 0.178907 0.729757 0.029000 Uiso calc U . R 1 . .
C C20 1.0653(10) 0.1395(8) 0.6671(5) 0.018(3) Uani d . . . 1 . .
C C21 0.1641(10) 0.4883(7) 0.3151(5) 0.017(3) Uani d . . . 1 . .
H H21 0.182346 0.526483 0.289644 0.021000 Uiso calc U . R 1 . .
C C22 0.0656(11) 0.4483(8) 0.2977(6) 0.020(3) Uani d . . . 1 . .
H H22 0.016570 0.459581 0.261514 0.025000 Uiso calc U . R 1 . .
C C23 0.0403(11) 0.3913(9) 0.3342(6) 0.025(3) Uani d . . . 1 . .
H H23 -0.026814 0.362965 0.323618 0.030000 Uiso calc U . R 1 . .
C C24 0.1150(10) 0.3762(8) 0.3869(6) 0.019(3) Uani d . . . 1 . .
H H24 0.100641 0.336318 0.412153 0.023000 Uiso calc U . R 1 . .
C C25 0.2105(10) 0.4204(7) 0.4017(5) 0.014(2) Uani d . . . 1 . .
C C26 0.2897(10) 0.4146(7) 0.4589(5) 0.015(2) Uani d . . . 1 . .
C C27 0.2814(11) 0.3582(8) 0.4994(6) 0.025(3) Uani d . . . 1 . .
H H27 0.224907 0.320043 0.490859 0.031000 Uiso calc U . R 1 . .
C C28 0.3565(13) 0.3582(10) 0.5525(7) 0.035(4) Uani d . . . 1 . .
H H28 0.353474 0.319016 0.580543 0.042000 Uiso calc U . R 1 . .
C C29 0.4361(13) 0.4157(10) 0.5644(7) 0.033(4) Uani d . . . 1 . .
H H29 0.486543 0.417919 0.601155 0.040000 Uiso calc U . R 1 . .
C C30 0.4407(11) 0.4697(9) 0.5219(6) 0.025(3) Uani d . . . 1 . .
H H30 0.496515 0.508368 0.529668 0.030000 Uiso calc U . R 1 . .
C C31 0.3202(12) 0.6559(8) 0.3023(6) 0.020(3) Uani d . . . 1 . .
H H31 0.269034 0.676019 0.323150 0.024000 Uiso calc U . R 1 . .
C C32 0.3260(13) 0.6903(8) 0.2497(6) 0.027(3) Uani d . . . 1 . .
H H32 0.281193 0.733515 0.234702 0.033000 Uiso calc U . R 1 . .
C C33 0.4003(14) 0.6586(10) 0.2203(7) 0.038(4) Uani d . . . 1 . .
H H33 0.405954 0.679942 0.183858 0.046000 Uiso calc U . R 1 . .
C C34 0.4669(14) 0.5962(10) 0.2428(6) 0.034(4) Uani d . . . 1 . .
H H34 0.518388 0.575011 0.222626 0.040000 Uiso calc U . R 1 . .
C C35 0.4557(11) 0.5660(7) 0.2957(6) 0.019(3) Uani d . . . 1 . .
C C36 0.5203(10) 0.4978(8) 0.3231(6) 0.019(3) Uani d . . . 1 . .
C C37 0.6065(12) 0.4646(10) 0.3027(7) 0.030(3) Uani d . . . 1 . .
H H37 0.629094 0.486495 0.270156 0.036000 Uiso calc U . R 1 . .
C C38 0.6589(12) 0.3998(10) 0.3298(7) 0.033(4) Uani d . . . 1 . .
H H38 0.717539 0.376338 0.316047 0.039000 Uiso calc U . R 1 . .
C C39 0.6254(13) 0.3696(9) 0.3772(7) 0.033(3) Uani d . . . 1 . .
H H39 0.658536 0.324031 0.396090 0.039000 Uiso calc U . R 1 . .
C C40 0.5411(11) 0.4077(8) 0.3967(6) 0.022(3) Uani d . . . 1 . .
H H40 0.519353 0.387978 0.430148 0.027000 Uiso calc U . R 1 . .


_geom_special_details            
;

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
U1 O1 . 1.768(10) ?
U1 O2 . 1.771(9) ?
U1 O7 3 2.432(9) ?
U1 O8 3 2.437(9) ?
U1 O5 . 2.468(8) ?
U1 O10 1_655 2.490(9) ?
U1 O9 1_655 2.494(10) ?
U1 O6 . 2.515(10) ?
U2 O3 . 1.762(10) ?
U2 O4 . 1.787(10) ?
U2 O17 3_455 2.426(10) ?
U2 O14 . 2.461(10) ?
U2 O16 3 2.464(9) ?
U2 O18 3_455 2.464(11) ?
U2 O13 . 2.470(10) ?
U2 O15 3 2.484(11) ?
Ni1 N4 . 2.030(10) ?
Ni1 N5 . 2.043(10) ?
Ni1 N3 . 2.047(10) ?
Ni1 N6 . 2.061(10) ?
Ni1 O5 . 2.130(8) ?
Ni1 O10 1_655 2.156(9) ?
O5 C4 . 1.281(15) ?
O6 C4 . 1.252(17) ?
O7 C7 . 1.262(17) ?
O8 C7 . 1.265(16) ?
O9 C10 . 1.255(17) ?
O10 C10 . 1.287(15) ?
O11 N1 . 1.213(17) ?
O12 N1 . 1.233(17) ?
O13 C14 . 1.263(18) ?
O14 C14 . 1.259(17) ?
O15 C17 . 1.250(18) ?
O16 C17 . 1.264(17) ?
O17 C20 . 1.260(17) ?
O18 C20 . 1.271(17) ?
O19 N2 . 1.202(19) ?
O20 N2 . 1.235(19) ?
O21 H21A . 0.842100 ?
O21 H21B . 0.831800 ?
O22 H22A . 0.843100 ?
O22 H22B . 0.842800 ?
N1 C1 . 1.558(18) ?
N2 C11 . 1.529(17) ?
N3 C21 . 1.337(16) ?
N3 C25 . 1.347(16) ?
N4 C30 . 1.350(17) ?
N4 C26 . 1.353(16) ?
N5 C31 . 1.340(17) ?
N5 C35 . 1.347(17) ?
N6 C40 . 1.328(17) ?
N6 C36 . 1.348(17) ?
C1 C2 . 1.527(18) ?
C1 C8 . 1.531(16) ?
C1 C5 . 1.540(18) ?
C2 C3 . 1.526(18) ?
C2 H2A . 0.990000 ?
C2 H2B . 0.990000 ?
C3 C4 . 1.506(18) ?
C3 H3A . 0.990000 ?
C3 H3B . 0.990000 ?
C5 C6 . 1.527(19) ?
C5 H5A . 0.990000 ?
C5 H5B . 0.990000 ?
C6 C7 . 1.524(18) ?
C6 H6A . 0.990000 ?
C6 H6B . 0.990000 ?
C8 C9 . 1.526(17) ?
C8 H8A . 0.990000 ?
C8 H8B . 0.990000 ?
C9 C10 . 1.501(17) ?
C9 H9A . 0.990000 ?
C9 H9B . 0.990000 ?
C11 C18 . 1.520(18) ?
C11 C12 . 1.533(19) ?
C11 C15 . 1.550(19) ?
C12 C13 . 1.531(19) ?
C12 H12A . 0.990000 ?
C12 H12B . 0.990000 ?
C13 C14 . 1.502(19) ?
C13 H13A . 0.990000 ?
C13 H13B . 0.990000 ?
C15 C16 . 1.511(18) ?
C15 H15A . 0.990000 ?
C15 H15B . 0.990000 ?
C16 C17 . 1.512(19) ?
C16 H16A . 0.990000 ?
C16 H16B . 0.990000 ?
C18 C19 . 1.530(18) ?
C18 H18A . 0.990000 ?
C18 H18B . 0.990000 ?
C19 C20 . 1.501(18) ?
C19 H19A . 0.990000 ?
C19 H19B . 0.990000 ?
C21 C22 . 1.384(18) ?
C21 H21 . 0.950000 ?
C22 C23 . 1.39(2) ?
C22 H22 . 0.950000 ?
C23 C24 . 1.399(19) ?
C23 H23 . 0.950000 ?
C24 C25 . 1.388(17) ?
C24 H24 . 0.950000 ?
C25 C26 . 1.483(17) ?
C26 C27 . 1.379(18) ?
C27 C28 . 1.38(2) ?
C27 H27 . 0.950000 ?
C28 C29 . 1.38(2) ?
C28 H28 . 0.950000 ?
C29 C30 . 1.38(2) ?
C29 H29 . 0.950000 ?
C30 H30 . 0.950000 ?
C31 C32 . 1.39(2) ?
C31 H31 . 0.950000 ?
C32 C33 . 1.38(2) ?
C32 H32 . 0.950000 ?
C33 C34 . 1.39(2) ?
C33 H33 . 0.950000 ?
C34 C35 . 1.384(19) ?
C34 H34 . 0.950000 ?
C35 C36 . 1.487(19) ?
C36 C37 . 1.389(19) ?
C37 C38 . 1.38(2) ?
C37 H37 . 0.950000 ?
C38 C39 . 1.38(2) ?
C38 H38 . 0.950000 ?
C39 C40 . 1.40(2) ?
C39 H39 . 0.950000 ?
C40 H40 . 0.950000 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 U1 O2 . . 178.5(5) ?
O1 U1 O7 . 3 86.1(4) ?
O2 U1 O7 . 3 94.1(4) ?
O1 U1 O8 . 3 87.6(4) ?
O2 U1 O8 . 3 91.2(4) ?
O7 U1 O8 3 3 53.4(3) ?
O1 U1 O5 . . 86.0(4) ?
O2 U1 O5 . . 95.2(4) ?
O7 U1 O5 3 . 120.1(3) ?
O8 U1 O5 3 . 171.3(3) ?
O1 U1 O10 . 1_655 92.5(4) ?
O2 U1 O10 . 1_655 87.3(4) ?
O7 U1 O10 3 1_655 177.1(3) ?
O8 U1 O10 3 1_655 124.1(3) ?
O5 U1 O10 . 1_655 62.2(3) ?
O1 U1 O9 . 1_655 89.4(4) ?
O2 U1 O9 . 1_655 89.3(4) ?
O7 U1 O9 3 1_655 125.7(3) ?
O8 U1 O9 3 1_655 72.3(3) ?
O5 U1 O9 . 1_655 113.4(3) ?
O10 U1 O9 1_655 1_655 51.7(3) ?
O1 U1 O6 . . 94.9(4) ?
O2 U1 O6 . . 86.6(4) ?
O7 U1 O6 3 . 70.0(3) ?
O8 U1 O6 3 . 123.0(3) ?
O5 U1 O6 . . 51.8(3) ?
O10 U1 O6 1_655 . 112.7(3) ?
O9 U1 O6 1_655 . 164.1(3) ?
O3 U2 O4 . . 179.1(5) ?
O3 U2 O17 . 3_455 92.4(4) ?
O4 U2 O17 . 3_455 87.1(4) ?
O3 U2 O14 . . 88.8(4) ?
O4 U2 O14 . . 91.7(4) ?
O17 U2 O14 3_455 . 174.0(3) ?
O3 U2 O16 . 3 91.0(4) ?
O4 U2 O16 . 3 89.6(4) ?
O17 U2 O16 3_455 3 67.4(3) ?
O14 U2 O16 . 3 118.5(3) ?
O3 U2 O18 . 3_455 89.5(4) ?
O4 U2 O18 . 3_455 89.6(4) ?
O17 U2 O18 3_455 3_455 53.0(3) ?
O14 U2 O18 . 3_455 121.2(3) ?
O16 U2 O18 3 3_455 120.3(3) ?
O3 U2 O13 . . 89.5(4) ?
O4 U2 O13 . . 90.1(4) ?
O17 U2 O13 3_455 . 121.5(3) ?
O14 U2 O13 . . 52.7(3) ?
O16 U2 O13 3 . 171.1(3) ?
O18 U2 O13 3_455 . 68.6(3) ?
O3 U2 O15 . 3 93.9(4) ?
O4 U2 O15 . 3 87.0(4) ?
O17 U2 O15 3_455 3 119.4(3) ?
O14 U2 O15 . 3 66.4(4) ?
O16 U2 O15 3 3 52.3(3) ?
O18 U2 O15 3_455 3 171.8(3) ?
O13 U2 O15 . 3 118.9(3) ?
N4 Ni1 N5 . . 174.3(4) ?
N4 Ni1 N3 . . 80.3(4) ?
N5 Ni1 N3 . . 97.0(4) ?
N4 Ni1 N6 . . 95.5(4) ?
N5 Ni1 N6 . . 79.9(4) ?
N3 Ni1 N6 . . 100.0(4) ?
N4 Ni1 O5 . . 90.0(4) ?
N5 Ni1 O5 . . 95.2(4) ?
N3 Ni1 O5 . . 93.0(4) ?
N6 Ni1 O5 . . 166.6(4) ?
N4 Ni1 O10 . 1_655 94.8(4) ?
N5 Ni1 O10 . 1_655 88.9(4) ?
N3 Ni1 O10 . 1_655 165.6(4) ?
N6 Ni1 O10 . 1_655 94.0(4) ?
O5 Ni1 O10 . 1_655 73.3(3) ?
C4 O5 Ni1 . . 151.4(8) ?
C4 O5 U1 . . 95.4(7) ?
Ni1 O5 U1 . . 112.4(3) ?
C4 O6 U1 . . 94.0(8) ?
C7 O7 U1 . 3_445 92.8(8) ?
C7 O8 U1 . 3_445 92.5(8) ?
C10 O9 U1 . 1_455 95.5(8) ?
C10 O10 Ni1 . 1_455 147.7(8) ?
C10 O10 U1 . 1_455 94.9(7) ?
Ni1 O10 U1 1_455 1_455 110.6(3) ?
C14 O13 U2 . . 93.2(8) ?
C14 O14 U2 . . 93.7(8) ?
C17 O15 U2 . 3_445 92.2(8) ?
C17 O16 U2 . 3_445 92.8(8) ?
C20 O17 U2 . 3_545 95.0(8) ?
C20 O18 U2 . 3_545 92.9(8) ?
H21A O21 H21B . . 107.500000 ?
H22A O22 H22B . . 106.300000 ?
O11 N1 O12 . . 123.6(14) ?
O11 N1 C1 . . 117.5(13) ?
O12 N1 C1 . . 118.8(12) ?
O19 N2 O20 . . 122.1(15) ?
O19 N2 C11 . . 119.8(14) ?
O20 N2 C11 . . 118.0(13) ?
C21 N3 C25 . . 118.7(10) ?
C21 N3 Ni1 . . 126.5(8) ?
C25 N3 Ni1 . . 114.6(8) ?
C30 N4 C26 . . 118.2(11) ?
C30 N4 Ni1 . . 127.1(9) ?
C26 N4 Ni1 . . 114.3(8) ?
C31 N5 C35 . . 119.1(11) ?
C31 N5 Ni1 . . 126.0(9) ?
C35 N5 Ni1 . . 114.8(8) ?
C40 N6 C36 . . 118.2(11) ?
C40 N6 Ni1 . . 127.0(9) ?
C36 N6 Ni1 . . 114.6(9) ?
C2 C1 C8 . . 111.0(11) ?
C2 C1 C5 . . 113.7(11) ?
C8 C1 C5 . . 114.3(10) ?
C2 C1 N1 . . 104.1(10) ?
C8 C1 N1 . . 105.5(10) ?
C5 C1 N1 . . 107.4(11) ?
C3 C2 C1 . . 114.7(11) ?
C3 C2 H2A . . 108.600000 ?
C1 C2 H2A . . 108.600000 ?
C3 C2 H2B . . 108.600000 ?
C1 C2 H2B . . 108.600000 ?
H2A C2 H2B . . 107.600000 ?
C4 C3 C2 . . 114.6(11) ?
C4 C3 H3A . . 108.600000 ?
C2 C3 H3A . . 108.600000 ?
C4 C3 H3B . . 108.600000 ?
C2 C3 H3B . . 108.600000 ?
H3A C3 H3B . . 107.600000 ?
O6 C4 O5 . . 118.6(11) ?
O6 C4 C3 . . 122.7(11) ?
O5 C4 C3 . . 118.6(11) ?
C6 C5 C1 . . 112.4(10) ?
C6 C5 H5A . . 109.100000 ?
C1 C5 H5A . . 109.100000 ?
C6 C5 H5B . . 109.100000 ?
C1 C5 H5B . . 109.100000 ?
H5A C5 H5B . . 107.900000 ?
C7 C6 C5 . . 106.7(10) ?
C7 C6 H6A . . 110.400000 ?
C5 C6 H6A . . 110.400000 ?
C7 C6 H6B . . 110.400000 ?
C5 C6 H6B . . 110.400000 ?
H6A C6 H6B . . 108.600000 ?
O7 C7 O8 . . 120.0(12) ?
O7 C7 C6 . . 119.5(12) ?
O8 C7 C6 . . 120.3(12) ?
C9 C8 C1 . . 114.0(10) ?
C9 C8 H8A . . 108.700000 ?
C1 C8 H8A . . 108.700000 ?
C9 C8 H8B . . 108.700000 ?
C1 C8 H8B . . 108.700000 ?
H8A C8 H8B . . 107.600000 ?
C10 C9 C8 . . 114.4(11) ?
C10 C9 H9A . . 108.700000 ?
C8 C9 H9A . . 108.700000 ?
C10 C9 H9B . . 108.700000 ?
C8 C9 H9B . . 108.700000 ?
H9A C9 H9B . . 107.600000 ?
O9 C10 O10 . . 117.7(11) ?
O9 C10 C9 . . 122.3(11) ?
O10 C10 C9 . . 120.0(11) ?
C18 C11 N2 . . 106.9(11) ?
C18 C11 C12 . . 115.0(11) ?
N2 C11 C12 . . 107.2(11) ?
C18 C11 C15 . . 108.9(11) ?
N2 C11 C15 . . 104.4(11) ?
C12 C11 C15 . . 113.7(11) ?
C13 C12 C11 . . 112.8(11) ?
C13 C12 H12A . . 109.000000 ?
C11 C12 H12A . . 109.000000 ?
C13 C12 H12B . . 109.000000 ?
C11 C12 H12B . . 109.000000 ?
H12A C12 H12B . . 107.800000 ?
C14 C13 C12 . . 109.4(12) ?
C14 C13 H13A . . 109.800000 ?
C12 C13 H13A . . 109.800000 ?
C14 C13 H13B . . 109.800000 ?
C12 C13 H13B . . 109.800000 ?
H13A C13 H13B . . 108.200000 ?
O14 C14 O13 . . 120.3(12) ?
O14 C14 C13 . . 119.9(13) ?
O13 C14 C13 . . 119.8(12) ?
C16 C15 C11 . . 115.2(12) ?
C16 C15 H15A . . 108.500000 ?
C11 C15 H15A . . 108.500000 ?
C16 C15 H15B . . 108.500000 ?
C11 C15 H15B . . 108.500000 ?
H15A C15 H15B . . 107.500000 ?
C15 C16 C17 . . 114.8(12) ?
C15 C16 H16A . . 108.600000 ?
C17 C16 H16A . . 108.600000 ?
C15 C16 H16B . . 108.600000 ?
C17 C16 H16B . . 108.600000 ?
H16A C16 H16B . . 107.600000 ?
O15 C17 O16 . . 120.3(13) ?
O15 C17 C16 . . 120.2(12) ?
O16 C17 C16 . . 119.4(12) ?
C11 C18 C19 . . 114.0(12) ?
C11 C18 H18A . . 108.700000 ?
C19 C18 H18A . . 108.800000 ?
C11 C18 H18B . . 108.700000 ?
C19 C18 H18B . . 108.800000 ?
H18A C18 H18B . . 107.600000 ?
C20 C19 C18 . . 113.8(12) ?
C20 C19 H19A . . 108.800000 ?
C18 C19 H19A . . 108.800000 ?
C20 C19 H19B . . 108.800000 ?
C18 C19 H19B . . 108.800000 ?
H19A C19 H19B . . 107.700000 ?
O17 C20 O18 . . 119.0(12) ?
O17 C20 C19 . . 119.6(12) ?
O18 C20 C19 . . 121.2(12) ?
N3 C21 C22 . . 123.0(12) ?
N3 C21 H21 . . 118.500000 ?
C22 C21 H21 . . 118.500000 ?
C21 C22 C23 . . 118.4(12) ?
C21 C22 H22 . . 120.800000 ?
C23 C22 H22 . . 120.800000 ?
C22 C23 C24 . . 119.0(12) ?
C22 C23 H23 . . 120.500000 ?
C24 C23 H23 . . 120.500000 ?
C25 C24 C23 . . 118.8(12) ?
C25 C24 H24 . . 120.600000 ?
C23 C24 H24 . . 120.600000 ?
N3 C25 C24 . . 121.9(11) ?
N3 C25 C26 . . 114.7(11) ?
C24 C25 C26 . . 123.2(11) ?
N4 C26 C27 . . 122.1(11) ?
N4 C26 C25 . . 115.4(11) ?
C27 C26 C25 . . 122.5(11) ?
C26 C27 C28 . . 119.0(13) ?
C26 C27 H27 . . 120.500000 ?
C28 C27 H27 . . 120.500000 ?
C29 C28 C27 . . 119.3(14) ?
C29 C28 H28 . . 120.400000 ?
C27 C28 H28 . . 120.400000 ?
C30 C29 C28 . . 118.7(14) ?
C30 C29 H29 . . 120.600000 ?
C28 C29 H29 . . 120.600000 ?
N4 C30 C29 . . 122.6(13) ?
N4 C30 H30 . . 118.700000 ?
C29 C30 H30 . . 118.700000 ?
N5 C31 C32 . . 123.1(13) ?
N5 C31 H31 . . 118.500000 ?
C32 C31 H31 . . 118.500000 ?
C33 C32 C31 . . 116.6(13) ?
C33 C32 H32 . . 121.700000 ?
C31 C32 H32 . . 121.700000 ?
C32 C33 C34 . . 121.5(13) ?
C32 C33 H33 . . 119.200000 ?
C34 C33 H33 . . 119.200000 ?
C35 C34 C33 . . 117.7(14) ?
C35 C34 H34 . . 121.100000 ?
C33 C34 H34 . . 121.100000 ?
N5 C35 C34 . . 121.9(13) ?
N5 C35 C36 . . 115.7(11) ?
C34 C35 C36 . . 122.4(13) ?
N6 C36 C37 . . 121.5(13) ?
N6 C36 C35 . . 114.6(11) ?
C37 C36 C35 . . 124.0(13) ?
C38 C37 C36 . . 119.7(15) ?
C38 C37 H37 . . 120.100000 ?
C36 C37 H37 . . 120.100000 ?
C37 C38 C39 . . 119.1(14) ?
C37 C38 H38 . . 120.500000 ?
C39 C38 H38 . . 120.500000 ?
C38 C39 C40 . . 118.1(14) ?
C38 C39 H39 . . 121.000000 ?
C40 C39 H39 . . 121.000000 ?
N6 C40 C39 . . 123.4(13) ?
N6 C40 H40 . . 118.300000 ?
C39 C40 H40 . . 118.300000 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O21 H21A O11 . 0.84 2.17 3.00(2) 167.8 ?
O21 H21B O23 4_464 0.83 2.37 2.80(2) 112.8 ?
O22 H22A O8 3 0.84 2.09 2.919(14) 166.7 ?
O22 H22B O23 . 0.84 1.95 2.781(19) 169.0 ?
C8 H8A O3 1_455 0.99 2.59 3.295(16) 128.0 ?
C16 H16B O20 . 0.99 2.48 3.19(2) 128.4 ?
C18 H18A O2 3_545 0.99 2.36 3.157(17) 137.0 ?
C24 H24 O9 3_545 0.95 2.52 3.448(17) 165.2 ?
C27 H27 O9 3_545 0.95 2.31 3.259(17) 172.5 ?
C29 H29 O13 . 0.95 2.37 3.188(18) 143.9 ?
C31 H31 O21 . 0.95 2.48 3.23(2) 136.0 ?

####################################################################### 
# 
# 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 2264773'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2023-05-23 deposited with the CCDC.	2023-06-21 downloaded from the CCDC.
;

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H64 Cu N6 O22 U2'
_chemical_formula_iupac          ?
_chemical_formula_weight         1472.53

_chemical_melting_point          ?

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

_cell_length_a                   11.3872(4)
_cell_length_b                   11.5224(4)
_cell_length_c                   12.7894(5)
_cell_angle_alpha                114.7971(13)
_cell_angle_beta                 98.3735(14)
_cell_angle_gamma                110.7704(13)
_cell_volume                     1335.95(9)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9429
_cell_measurement_theta_min      2.1993
_cell_measurement_theta_max      30.5374
_cell_measurement_temperature    100(2)

_exptl_crystal_description       irregular
_exptl_crystal_colour            'translucent intense purple'
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.055
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             711

_exptl_absorpt_coefficient_mu    6.517
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_T_max  0.75

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100(2)

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

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

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

_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_detector_area_resol_mean 7.41

_diffrn_reflns_number            53010
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_full        28.70
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17

_refine_special_details          
;
The H atoms bound to O11 were found and refined with
restraints on bond lengths and angle. Some voids in the 
structure indicate the presence of other, unresolved
solvent molecules whose contribution to the structure 
factors was removed with SQUEEZE.
;

_reflns_number_total             6907
_reflns_number_gt                6523
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0186
_refine_ls_wR_factor_gt          0.0409
_refine_ls_wR_factor_ref         0.0417
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.073
_refine_ls_number_reflns         6907
_refine_ls_number_parameters     313
_refine_ls_number_restraints     3
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0100P)²+1.6601P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.891
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U U1 0.85623(2) 0.82500(2) 0.74974(2) 0.00962(3) Uani d . . . 1 . .
Cu Cu1 0.500000 0.000000 0.500000 0.01717(9) Uani d . P S 1 . .
O O1 0.73533(16) 0.67351(18) 0.74829(15) 0.0139(3) Uani d . . . 1 . .
O O2 0.98100(17) 0.97166(19) 0.74981(17) 0.0190(4) Uani d . . . 1 . .
O O3 0.92902(17) 0.65807(19) 0.61850(15) 0.0160(4) Uani d . . . 1 . .
O O4 0.76507(17) 0.67485(18) 0.52197(15) 0.0142(3) Uani d . . . 1 . .
O O5 0.30539(16) 0.11713(18) 0.31435(15) 0.0134(3) Uani d . . . 1 . .
O O6 0.47977(19) 0.0741(2) 0.33828(19) 0.0230(4) Uani d . . . 1 . .
O O7 0.84632(18) -0.0259(2) -0.06548(16) 0.0195(4) Uani d . . . 1 . .
O O8 0.97987(17) 0.17081(19) 0.11471(15) 0.0161(4) Uani d . . . 1 . .
O O9 0.6444(2) 0.4019(2) 0.05396(19) 0.0318(5) Uani d . . . 1 . .
O O10 0.50142(19) 0.1845(2) -0.01063(17) 0.0246(4) Uani d . . . 1 . .
O O11 0.5157(2) 0.3926(2) 0.5586(2) 0.0282(5) Uani d . . D 1 . .
H H11A 0.568(2) 0.4773(18) 0.618(2) 0.042000 Uiso d U . D 1 . .
H H11B 0.4416(18) 0.391(3) 0.535(3) 0.042000 Uiso d U . D 1 . .
N N1 0.6010(2) 0.2968(2) 0.06547(18) 0.0118(4) Uani d . . . 1 . .
N N2 0.7028(2) 0.1221(3) 0.5967(2) 0.0235(5) Uani d . . . 1 . .
H H2 0.719639 0.086832 0.653882 0.028000 Uiso calc U . R 1 . .
N N3 0.4813(2) 0.1654(3) 0.6258(2) 0.0242(5) Uani d . . . 1 . .
H H3 0.473960 0.223973 0.587915 0.029000 Uiso calc U . R 1 . .
C C1 0.6819(2) 0.3039(2) 0.1787(2) 0.0094(4) Uani d . . . 1 . .
C C2 0.7376(2) 0.4592(2) 0.2863(2) 0.0113(4) Uani d . . . 1 . .
H H2A 0.799749 0.527194 0.267963 0.014000 Uiso calc U . R 1 . .
H H2B 0.662847 0.482928 0.295705 0.014000 Uiso calc U . R 1 . .
C C3 0.8114(3) 0.4776(3) 0.4067(2) 0.0164(5) Uani d . . . 1 . .
H H3A 0.758009 0.392946 0.412539 0.020000 Uiso calc U . R 1 . .
H H3B 0.898120 0.478320 0.404047 0.020000 Uiso calc U . R 1 . .
C C4 0.8377(2) 0.6122(2) 0.5205(2) 0.0120(4) Uani d . . . 1 . .
C C5 0.5895(2) 0.1896(2) 0.2009(2) 0.0106(4) Uani d . . . 1 . .
H H5A 0.544704 0.095894 0.122846 0.013000 Uiso calc U . R 1 . .
H H5B 0.645174 0.179810 0.260633 0.013000 Uiso calc U . R 1 . .
C C6 0.4820(2) 0.2195(3) 0.2487(2) 0.0134(5) Uani d . . . 1 . .
H H6A 0.522045 0.322912 0.311912 0.016000 Uiso calc U . R 1 . .
H H6B 0.410329 0.200006 0.180280 0.016000 Uiso calc U . R 1 . .
C C7 0.4202(2) 0.1296(2) 0.3039(2) 0.0121(4) Uani d . . . 1 . .
C C8 0.7968(2) 0.2745(2) 0.1459(2) 0.0122(4) Uani d . . . 1 . .
H H8A 0.850103 0.348208 0.127988 0.015000 Uiso calc U . R 1 . .
H H8B 0.856096 0.287104 0.218844 0.015000 Uiso calc U . R 1 . .
C C9 0.7548(2) 0.1257(3) 0.0371(2) 0.0147(5) Uani d . . . 1 . .
H H9A 0.684170 0.052134 0.044534 0.018000 Uiso calc U . R 1 . .
H H9B 0.716011 0.121502 -0.039612 0.018000 Uiso calc U . R 1 . .
C C10 0.8693(2) 0.0892(3) 0.0284(2) 0.0114(4) Uani d . . . 1 . .
C C11 0.7221(3) 0.2695(3) 0.6781(3) 0.0394(8) Uani d . . . 1 . .
H H11C 0.720634 0.318857 0.630811 0.047000 Uiso calc U . R 1 . .
H H11D 0.809671 0.326760 0.745550 0.047000 Uiso calc U . R 1 . .
C C12 0.6106(3) 0.2568(3) 0.7296(3) 0.0365(8) Uani d . . . 1 . .
H H12A 0.615313 0.212753 0.780951 0.044000 Uiso calc U . R 1 . .
H H12B 0.618752 0.353583 0.781589 0.044000 Uiso calc U . R 1 . .
C C13 0.8054(3) 0.1173(4) 0.5354(3) 0.0273(6) Uani d . . . 1 . .
C C14 0.8110(3) 0.1989(4) 0.4669(4) 0.0427(9) Uani d . . . 1 . .
H H14A 0.719880 0.176789 0.425532 0.064000 Uiso calc U . R 1 . .
H H14B 0.853254 0.169589 0.405763 0.064000 Uiso calc U . R 1 . .
H H14C 0.863337 0.302784 0.525275 0.064000 Uiso calc U . R 1 . .
C C15 0.9444(3) 0.1853(4) 0.6305(4) 0.0439(9) Uani d . . . 1 . .
H H15A 0.970669 0.286064 0.689683 0.066000 Uiso calc U . R 1 . .
H H15B 1.009733 0.181324 0.588791 0.066000 Uiso calc U . R 1 . .
H H15C 0.941347 0.131992 0.673759 0.066000 Uiso calc U . R 1 . .
C C16 0.3625(3) 0.1281(4) 0.6643(3) 0.0296(7) Uani d . . . 1 . .
H H16 0.366157 0.067529 0.701102 0.035000 Uiso calc U . R 1 . .
C C17 0.2345(3) 0.0397(4) 0.5524(3) 0.0307(7) Uani d . . . 1 . .
H H17A 0.159605 0.042735 0.582355 0.037000 Uiso calc U . R 1 . .
H H17B 0.242745 0.089113 0.504512 0.037000 Uiso calc U . R 1 . .
C C18 0.3606(4) 0.2623(5) 0.7607(3) 0.0487(10) Uani d . . . 1 . .
H H18A 0.360487 0.324985 0.727447 0.073000 Uiso calc U . R 1 . .
H H18B 0.440144 0.314682 0.834459 0.073000 Uiso calc U . R 1 . .
H H18C 0.279906 0.233204 0.781901 0.073000 Uiso calc U . R 1 . .


_geom_special_details            
;

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
U1 O2 . 1.7803(18) ?
U1 O1 . 1.7899(17) ?
U1 O7 1_566 2.3149(17) ?
U1 O5 2_666 2.3223(17) ?
U1 O8 2_766 2.3269(17) ?
U1 O3 . 2.4560(17) ?
U1 O4 . 2.4850(16) ?
Cu1 N3 2_656 2.020(2) ?
Cu1 N3 . 2.020(2) ?
Cu1 N2 . 2.061(2) ?
Cu1 N2 2_656 2.061(2) ?
Cu1 O6 . 2.5581(18) ?
O3 C4 . 1.268(3) ?
O4 C4 . 1.274(3) ?
O5 C7 . 1.297(3) ?
O6 C7 . 1.232(3) ?
O7 C10 . 1.263(3) ?
O8 C10 . 1.254(3) ?
O9 N1 . 1.216(3) ?
O10 N1 . 1.220(3) ?
O11 H11A . 0.844(10) ?
O11 H11B . 0.846(10) ?
N1 C1 . 1.553(3) ?
N2 C11 . 1.484(4) ?
N2 C13 . 1.504(4) ?
N2 H2 . 1.000000 ?
N3 C12 . 1.483(4) ?
N3 C16 . 1.489(4) ?
N3 H3 . 1.000000 ?
C1 C5 . 1.531(3) ?
C1 C8 . 1.535(3) ?
C1 C2 . 1.541(3) ?
C2 C3 . 1.531(3) ?
C2 H2A . 0.990000 ?
C2 H2B . 0.990000 ?
C3 C4 . 1.505(3) ?
C3 H3A . 0.990000 ?
C3 H3B . 0.990000 ?
C5 C6 . 1.526(3) ?
C5 H5A . 0.990000 ?
C5 H5B . 0.990000 ?
C6 C7 . 1.518(3) ?
C6 H6A . 0.990000 ?
C6 H6B . 0.990000 ?
C8 C9 . 1.526(3) ?
C8 H8A . 0.990000 ?
C8 H8B . 0.990000 ?
C9 C10 . 1.510(3) ?
C9 H9A . 0.990000 ?
C9 H9B . 0.990000 ?
C11 C12 . 1.504(5) ?
C11 H11C . 0.990000 ?
C11 H11D . 0.990000 ?
C12 H12A . 0.990000 ?
C12 H12B . 0.990000 ?
C13 C17 2_656 1.518(5) ?
C13 C14 . 1.524(4) ?
C13 C15 . 1.535(4) ?
C14 H14A . 0.980000 ?
C14 H14B . 0.980000 ?
C14 H14C . 0.980000 ?
C15 H15A . 0.980000 ?
C15 H15B . 0.980000 ?
C15 H15C . 0.980000 ?
C16 C17 . 1.526(4) ?
C16 C18 . 1.531(4) ?
C16 H16 . 1.000000 ?
C17 H17A . 0.990000 ?
C17 H17B . 0.990000 ?
C18 H18A . 0.980000 ?
C18 H18B . 0.980000 ?
C18 H18C . 0.980000 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 U1 O1 . . 177.43(8) ?
O2 U1 O7 . 1_566 93.02(8) ?
O1 U1 O7 . 1_566 88.64(7) ?
O2 U1 O5 . 2_666 89.60(7) ?
O1 U1 O5 . 2_666 92.66(7) ?
O7 U1 O5 1_566 2_666 78.05(6) ?
O2 U1 O8 . 2_766 89.94(8) ?
O1 U1 O8 . 2_766 88.42(7) ?
O7 U1 O8 1_566 2_766 80.13(6) ?
O5 U1 O8 2_666 2_766 158.11(6) ?
O2 U1 O3 . . 90.84(7) ?
O1 U1 O3 . . 86.82(7) ?
O7 U1 O3 1_566 . 154.79(6) ?
O5 U1 O3 2_666 . 126.92(6) ?
O8 U1 O3 2_766 . 74.96(6) ?
O2 U1 O4 . . 93.10(7) ?
O1 U1 O4 . . 86.35(7) ?
O7 U1 O4 1_566 . 151.46(6) ?
O5 U1 O4 2_666 . 74.15(6) ?
O8 U1 O4 2_766 . 127.72(6) ?
O3 U1 O4 . . 52.83(5) ?
N3 Cu1 N3 2_656 . 180.00(13) ?
N3 Cu1 N2 2_656 . 93.94(10) ?
N3 Cu1 N2 . . 86.07(10) ?
N3 Cu1 N2 2_656 2_656 86.07(10) ?
N3 Cu1 N2 . 2_656 93.93(10) ?
N2 Cu1 N2 . 2_656 180.000000 ?
C4 O3 U1 . . 94.03(14) ?
C4 O4 U1 . . 92.53(13) ?
C7 O5 U1 . 2_666 137.17(15) ?
C10 O7 U1 . 1_544 159.00(18) ?
C10 O8 U1 . 2_766 143.35(17) ?
H11A O11 H11B . . 106.1(16) ?
O9 N1 O10 . . 123.1(2) ?
O9 N1 C1 . . 117.90(19) ?
O10 N1 C1 . . 118.88(19) ?
C11 N2 C13 . . 114.4(2) ?
C11 N2 Cu1 . . 105.15(18) ?
C13 N2 Cu1 . . 122.34(19) ?
C11 N2 H2 . . 104.400000 ?
C13 N2 H2 . . 104.400000 ?
Cu1 N2 H2 . . 104.400000 ?
C12 N3 C16 . . 113.5(2) ?
C12 N3 Cu1 . . 106.31(18) ?
C16 N3 Cu1 . . 117.15(19) ?
C12 N3 H3 . . 106.400000 ?
C16 N3 H3 . . 106.400000 ?
Cu1 N3 H3 . . 106.400000 ?
C5 C1 C8 . . 111.88(19) ?
C5 C1 C2 . . 113.38(18) ?
C8 C1 C2 . . 110.31(18) ?
C5 C1 N1 . . 108.89(17) ?
C8 C1 N1 . . 105.70(18) ?
C2 C1 N1 . . 106.23(18) ?
C3 C2 C1 . . 111.43(19) ?
C3 C2 H2A . . 109.300000 ?
C1 C2 H2A . . 109.300000 ?
C3 C2 H2B . . 109.300000 ?
C1 C2 H2B . . 109.300000 ?
H2A C2 H2B . . 108.000000 ?
C4 C3 C2 . . 114.6(2) ?
C4 C3 H3A . . 108.600000 ?
C2 C3 H3A . . 108.600000 ?
C4 C3 H3B . . 108.600000 ?
C2 C3 H3B . . 108.600000 ?
H3A C3 H3B . . 107.600000 ?
O3 C4 O4 . . 119.8(2) ?
O3 C4 C3 . . 118.7(2) ?
O4 C4 C3 . . 121.4(2) ?
C6 C5 C1 . . 115.53(19) ?
C6 C5 H5A . . 108.400000 ?
C1 C5 H5A . . 108.400000 ?
C6 C5 H5B . . 108.400000 ?
C1 C5 H5B . . 108.400000 ?
H5A C5 H5B . . 107.500000 ?
C7 C6 C5 . . 113.5(2) ?
C7 C6 H6A . . 108.900000 ?
C5 C6 H6A . . 108.900000 ?
C7 C6 H6B . . 108.900000 ?
C5 C6 H6B . . 108.900000 ?
H6A C6 H6B . . 107.700000 ?
O6 C7 O5 . . 122.8(2) ?
O6 C7 C6 . . 120.2(2) ?
O5 C7 C6 . . 117.1(2) ?
C9 C8 C1 . . 115.61(19) ?
C9 C8 H8A . . 108.400000 ?
C1 C8 H8A . . 108.400000 ?
C9 C8 H8B . . 108.400000 ?
C1 C8 H8B . . 108.400000 ?
H8A C8 H8B . . 107.400000 ?
C10 C9 C8 . . 113.13(19) ?
C10 C9 H9A . . 109.000000 ?
C8 C9 H9A . . 109.000000 ?
C10 C9 H9B . . 109.000000 ?
C8 C9 H9B . . 109.000000 ?
H9A C9 H9B . . 107.800000 ?
O8 C10 O7 . . 123.4(2) ?
O8 C10 C9 . . 119.2(2) ?
O7 C10 C9 . . 117.3(2) ?
N2 C11 C12 . . 108.3(3) ?
N2 C11 H11C . . 110.000000 ?
C12 C11 H11C . . 110.000000 ?
N2 C11 H11D . . 110.000000 ?
C12 C11 H11D . . 110.000000 ?
H11C C11 H11D . . 108.400000 ?
N3 C12 C11 . . 108.3(3) ?
N3 C12 H12A . . 110.000000 ?
C11 C12 H12A . . 110.000000 ?
N3 C12 H12B . . 110.000000 ?
C11 C12 H12B . . 110.000000 ?
H12A C12 H12B . . 108.400000 ?
N2 C13 C17 . 2_656 108.1(2) ?
N2 C13 C14 . . 109.5(3) ?
C17 C13 C14 2_656 . 110.8(3) ?
N2 C13 C15 . . 110.7(3) ?
C17 C13 C15 2_656 . 108.3(3) ?
C14 C13 C15 . . 109.4(3) ?
C13 C14 H14A . . 109.500000 ?
C13 C14 H14B . . 109.500000 ?
H14A C14 H14B . . 109.500000 ?
C13 C14 H14C . . 109.500000 ?
H14A C14 H14C . . 109.500000 ?
H14B C14 H14C . . 109.500000 ?
C13 C15 H15A . . 109.500000 ?
C13 C15 H15B . . 109.500000 ?
H15A C15 H15B . . 109.500000 ?
C13 C15 H15C . . 109.500000 ?
H15A C15 H15C . . 109.500000 ?
H15B C15 H15C . . 109.500000 ?
N3 C16 C17 . . 109.8(2) ?
N3 C16 C18 . . 112.1(3) ?
C17 C16 C18 . . 110.1(3) ?
N3 C16 H16 . . 108.200000 ?
C17 C16 H16 . . 108.200000 ?
C18 C16 H16 . . 108.200000 ?
C13 C17 C16 2_656 . 118.8(2) ?
C13 C17 H17A 2_656 . 107.600000 ?
C16 C17 H17A . . 107.600000 ?
C13 C17 H17B 2_656 . 107.600000 ?
C16 C17 H17B . . 107.600000 ?
H17A C17 H17B . . 107.100000 ?
C16 C18 H18A . . 109.500000 ?
C16 C18 H18B . . 109.500000 ?
H18A C18 H18B . . 109.500000 ?
C16 C18 H18C . . 109.500000 ?
H18A C18 H18C . . 109.500000 ?
H18B C18 H18C . . 109.500000 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O11 H11A O1 . 0.844(10) 2.096(12) 2.919(3) 165(3) ?
O11 H11B O4 2_666 0.846(10) 2.101(14) 2.914(3) 161(3) ?
N2 H2 O5 2_656 1.000000 2.480000 3.373(3) 149 ?
N2 H2 O6 2_656 1.000000 2.420000 2.979(3) 115 ?
N3 H3 O11 . 1.000000 2.040000 3.001(3) 161. ?
C14 H14A O6 . 0.980000 2.410000 3.371(4) 165 ?
C15 H15C O2 1_545 0.980000 2.560000 3.501(4) 162 ?


####################################################################### 
# 
# 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 2264772'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2023-05-23 deposited with the CCDC.	2023-06-21 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT306_5                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O23 Check 
RESPONSE: This O atom pertains to a water molecule for which the H
atoms were not found.
;
# end Validation Reply Form

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H46 Cu N6 O23 U2'
_chemical_formula_iupac          ?
_chemical_formula_weight         1518.43
_chemical_absolute_configuration ad

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   12.4847(7)
_cell_length_b                   17.0888(11)
_cell_length_c                   23.5455(16)
_cell_angle_alpha                90
_cell_angle_beta                 103.131(2)
_cell_angle_gamma                90
_cell_volume                     4892.1(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9936
_cell_measurement_theta_min      2.5439
_cell_measurement_theta_max      30.5395
_cell_measurement_temperature    100(2)

_exptl_crystal_description       irregular
_exptl_crystal_colour            'translucent intense blue-purple'
_exptl_crystal_size_max          0.093
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.045
_exptl_crystal_density_diffrn    2.062
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2900

_exptl_absorpt_coefficient_mu    7.125
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_T_max  0.75

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100(2)

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

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

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

_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_detector_area_resol_mean 7.41

_diffrn_reflns_number            39817
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28

_refine_special_details          
;
The H atoms bound to O21 and O22 were found and treated
as riding atoms. Those of O23 were not found.
;

_reflns_number_total             8866
_reflns_number_gt                8727
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0706
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.043
_refine_ls_number_reflns         8866
_refine_ls_number_parameters     650
_refine_ls_number_restraints     20
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0412P)²+7.1661P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.504
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
Determined from the refined Flack parameter.
;
_refine_ls_abs_structure_Flack   -0.003(7)

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U U1 0.59182(2) 0.26627(2) 0.52349(2) 0.02508(9) Uani d . . . 1 . .
U U2 0.24769(2) 0.44100(2) 0.35616(2) 0.02450(9) Uani d . . . 1 . .
Cu Cu1 0.62113(9) 0.47628(6) 0.60670(5) 0.0299(2) Uani d . . . 1 . .
O O1 0.6178(6) 0.2327(4) 0.5967(3) 0.0336(15) Uani d . . . 1 . .
O O2 0.5618(6) 0.3000(4) 0.4503(3) 0.0333(14) Uani d . . . 1 . .
O O3 0.3001(6) 0.4362(4) 0.4329(3) 0.0328(16) Uani d . . . 1 . .
O O4 0.1953(6) 0.4469(4) 0.2796(3) 0.0370(17) Uani d . . . 1 . .
O O5 0.7121(5) 0.3768(4) 0.5593(3) 0.0365(15) Uani d . . . 1 . .
O O6 0.7904(7) 0.2813(5) 0.5232(4) 0.0382(18) Uani d . . . 1 . .
O O7 1.1712(6) 0.6434(4) 0.5008(3) 0.0347(15) Uani d . . . 1 . .
O O8 0.9941(5) 0.6429(4) 0.4921(3) 0.0331(14) Uani d . . . 1 . .
O O9 1.3938(6) 0.2815(5) 0.5257(4) 0.0311(16) Uani d . . . 1 . .
O O10 1.4989(5) 0.3843(4) 0.5517(3) 0.0287(13) Uani d . . . 1 . .
O O11 1.1270(8) 0.3096(5) 0.6389(4) 0.054(2) Uani d . . . 1 . .
O O12 1.1512(8) 0.4306(5) 0.6628(4) 0.054(2) Uani d . . . 1 . .
O O13 0.3240(6) 0.5741(4) 0.3540(4) 0.0374(16) Uani d . . . 1 . .
O O14 0.1583(6) 0.5657(4) 0.3699(3) 0.0351(15) Uani d . . . 1 . .
O O15 0.5521(7) 0.9282(5) 0.3644(4) 0.0345(18) Uani d . . . 1 . .
O O16 0.6416(5) 0.8189(4) 0.3574(3) 0.0357(15) Uani d . . . 1 . .
O O17 -0.1492(5) 0.8271(4) 0.3380(3) 0.0347(15) Uani d . . . 1 . .
O O18 -0.0641(7) 0.9381(4) 0.3419(4) 0.0301(18) Uani d . . . 1 . .
O O19 0.1726(9) 0.9134(7) 0.2382(5) 0.073(3) Uani d . . . 1 . .
O O20 0.2583(8) 0.8124(5) 0.2178(3) 0.054(2) Uani d . . . 1 . .
O O21 0.9341(8) 0.3115(7) 0.6958(5) 0.070(3) Uani d . . D 1 . .
H H21A 0.987706 0.306066 0.679614 0.105000 Uiso d U . DR 1 . .
H H21B 0.924068 0.358811 0.699152 0.105000 Uiso d U . DR 1 . .
O O22 0.3430(7) 0.1730(5) 0.3796(3) 0.0474(18) Uani d . . D 1 . .
H H22A 0.385906 0.173428 0.412803 0.071000 Uiso d U . DR 1 . .
H H22B 0.375491 0.147664 0.357686 0.071000 Uiso d U . DR 1 . .
O O23 0.4436(8) 0.1033(7) 0.2978(4) 0.066(3) Uani d . . . 1 . .
N N1 1.1300(7) 0.3782(5) 0.6268(4) 0.0364(18) Uani d . . . 1 . .
N N2 0.2185(6) 0.8510(5) 0.2510(4) 0.0372(18) Uani d . . . 1 . .
N N3 0.7745(6) 0.5242(4) 0.6363(3) 0.0290(15) Uani d . . . 1 . .
N N4 0.6267(7) 0.5378(5) 0.5375(3) 0.0302(16) Uani d . . . 1 . .
N N5 0.6136(6) 0.4135(5) 0.6753(3) 0.0310(16) Uani d . . . 1 . .
N N6 0.4924(6) 0.5344(5) 0.6310(3) 0.0322(16) Uani d . . . 1 . .
C C1 1.1066(7) 0.3997(6) 0.5608(4) 0.030(2) Uani d U . . 1 . .
C C2 0.9947(7) 0.3615(6) 0.5343(4) 0.0316(19) Uani d . . . 1 . .
H H2A 0.978606 0.367815 0.491364 0.038000 Uiso calc U . R 1 . .
H H2B 0.999645 0.304748 0.542873 0.038000 Uiso calc U . R 1 . .
C C3 0.9000(8) 0.3960(6) 0.5571(5) 0.035(2) Uani d . . . 1 . .
H H3A 0.925032 0.403377 0.599768 0.042000 Uiso calc U . R 1 . .
H H3B 0.882520 0.448360 0.539429 0.042000 Uiso calc U . R 1 . .
C C4 0.7962(7) 0.3481(5) 0.5454(4) 0.0300(18) Uani d . . . 1 . .
C C5 1.1055(8) 0.4889(6) 0.5559(4) 0.029(2) Uani d . . . 1 . .
H H5A 1.177545 0.509522 0.577198 0.035000 Uiso calc U . R 1 . .
H H5B 1.048508 0.510021 0.574906 0.035000 Uiso calc U . R 1 . .
C C6 1.0824(9) 0.5177(6) 0.4928(5) 0.036(2) Uani d . . . 1 . .
H H6A 1.140169 0.498748 0.473490 0.043000 Uiso calc U . R 1 . .
H H6B 1.010422 0.497838 0.470831 0.043000 Uiso calc U . R 1 . .
C C7 1.0818(8) 0.6060(5) 0.4942(4) 0.0273(18) Uani d . . . 1 . .
C C8 1.1992(7) 0.3596(5) 0.5372(4) 0.0283(18) Uani d U . . 1 . .
H H8A 1.199832 0.303048 0.546331 0.034000 Uiso calc U . R 1 . .
H H8B 1.182499 0.365137 0.494242 0.034000 Uiso calc U . R 1 . .
C C9 1.3126(7) 0.3931(6) 0.5623(4) 0.0302(18) Uani d . . . 1 . .
H H9A 1.313613 0.448332 0.549705 0.036000 Uiso calc U . R 1 . .
H H9B 1.325488 0.392870 0.605362 0.036000 Uiso calc U . R 1 . .
C C10 1.4063(7) 0.3506(5) 0.5452(4) 0.0286(18) Uani d . . . 1 . .
C C11 0.2328(7) 0.8213(5) 0.3147(4) 0.0278(18) Uani d . . . 1 . .
C C12 0.2289(8) 0.7323(5) 0.3121(4) 0.0288(19) Uani d . . . 1 . .
H H12A 0.290147 0.713207 0.295498 0.035000 Uiso calc U . R 1 . .
H H12B 0.159169 0.715853 0.285633 0.035000 Uiso calc U . R 1 . .
C C13 0.2373(8) 0.6941(5) 0.3717(4) 0.0299(19) Uani d . . . 1 . .
H H13A 0.305213 0.711861 0.399132 0.036000 Uiso calc U . R 1 . .
H H13B 0.173558 0.709689 0.387555 0.036000 Uiso calc U . R 1 . .
C C14 0.2394(8) 0.6066(6) 0.3653(4) 0.032(2) Uani d . . . 1 . .
C C15 0.3448(7) 0.8547(6) 0.3478(4) 0.032(2) Uani d . . . 1 . .
H H15A 0.348909 0.910423 0.337083 0.039000 Uiso calc U . R 1 . .
H H15B 0.348175 0.852319 0.390149 0.039000 Uiso calc U . R 1 . .
C C16 0.4454(7) 0.8118(6) 0.3356(5) 0.035(2) Uani d . . . 1 . .
H H16A 0.452606 0.760670 0.355838 0.042000 Uiso calc U . R 1 . .
H H16B 0.432371 0.801399 0.293223 0.042000 Uiso calc U . R 1 . .
C C17 0.5523(7) 0.8558(6) 0.3546(4) 0.0316(19) Uani d . . . 1 . .
C C18 0.1415(7) 0.8582(6) 0.3396(4) 0.0293(18) Uani d . . . 1 . .
H H18A 0.140197 0.915236 0.332307 0.035000 Uiso calc U . R 1 . .
H H18B 0.158929 0.850164 0.382376 0.035000 Uiso calc U . R 1 . .
C C19 0.0267(7) 0.8245(6) 0.3136(4) 0.0317(19) Uani d . . . 1 . .
H H19A 0.012347 0.827531 0.270566 0.038000 Uiso calc U . R 1 . .
H H19B 0.025803 0.768519 0.324433 0.038000 Uiso calc U . R 1 . .
C C20 -0.0637(7) 0.8662(6) 0.3338(4) 0.0281(18) Uani d . . . 1 . .
C C21 0.8462(8) 0.5114(6) 0.6861(4) 0.033(2) Uani d . . . 1 . .
H H21 0.829121 0.472916 0.711843 0.040000 Uiso calc U . R 1 . .
C C22 0.9446(9) 0.5511(7) 0.7026(5) 0.040(2) Uani d . . . 1 . .
H H22 0.995164 0.539583 0.738280 0.048000 Uiso calc U . R 1 . .
C C23 0.9673(8) 0.6086(7) 0.6653(4) 0.039(2) Uani d . . . 1 . .
H H23 1.034306 0.637127 0.675483 0.047000 Uiso calc U . R 1 . .
C C24 0.8928(8) 0.6246(6) 0.6133(4) 0.034(2) Uani d . . . 1 . .
H H24 0.906552 0.664724 0.587946 0.041000 Uiso calc U . R 1 . .
C C25 0.7965(8) 0.5797(5) 0.5995(4) 0.0296(18) Uani d . . . 1 . .
C C26 0.7150(7) 0.5867(5) 0.5436(4) 0.0291(18) Uani d . . . 1 . .
C C27 0.7265(8) 0.6352(6) 0.4990(4) 0.038(2) Uani d . . . 1 . .
H H27 0.788144 0.669215 0.503966 0.046000 Uiso calc U . R 1 . .
C C28 0.6483(9) 0.6349(7) 0.4463(4) 0.046(2) Uani d . . . 1 . .
H H28 0.655398 0.668428 0.415229 0.055000 Uiso calc U . R 1 . .
C C29 0.5602(10) 0.5845(8) 0.4407(5) 0.049(3) Uani d . . . 1 . .
H H29 0.506167 0.582002 0.405058 0.059000 Uiso calc U . R 1 . .
C C30 0.5510(8) 0.5376(7) 0.4874(4) 0.037(2) Uani d . . . 1 . .
H H30 0.488855 0.504262 0.483553 0.045000 Uiso calc U . R 1 . .
C C31 0.6807(8) 0.3538(6) 0.6952(4) 0.035(2) Uani d . . . 1 . .
H H31 0.733955 0.338775 0.674247 0.042000 Uiso calc U . R 1 . .
C C32 0.6754(9) 0.3129(6) 0.7454(5) 0.042(2) Uani d . . . 1 . .
H H32 0.722968 0.269964 0.758355 0.051000 Uiso calc U . R 1 . .
C C33 0.5981(9) 0.3367(7) 0.7763(4) 0.045(2) Uani d . . . 1 . .
H H33 0.594247 0.311222 0.811664 0.054000 Uiso calc U . R 1 . .
C C34 0.5269(9) 0.3977(7) 0.7553(4) 0.042(2) Uani d . . . 1 . .
H H34 0.472575 0.413675 0.775296 0.050000 Uiso calc U . R 1 . .
C C35 0.5368(8) 0.4347(6) 0.7044(4) 0.034(2) Uani d . . . 1 . .
C C36 0.4664(8) 0.5027(6) 0.6786(4) 0.0325(19) Uani d . . . 1 . .
C C37 0.3809(9) 0.5315(7) 0.7011(5) 0.041(2) Uani d . . . 1 . .
H H37 0.360592 0.506294 0.733013 0.049000 Uiso calc U . R 1 . .
C C38 0.3254(9) 0.5978(8) 0.6762(5) 0.049(3) Uani d . . . 1 . .
H H38 0.267875 0.619691 0.691521 0.058000 Uiso calc U . R 1 . .
C C39 0.3554(9) 0.6315(7) 0.6286(5) 0.045(2) Uani d . . . 1 . .
H H39 0.319263 0.677334 0.611132 0.054000 Uiso calc U . R 1 . .
C C40 0.4380(9) 0.5980(6) 0.6069(5) 0.041(2) Uani d . . . 1 . .
H H40 0.456982 0.620817 0.573717 0.049000 Uiso calc U . R 1 . .


_geom_special_details            
;

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
U1 O2 . 1.774(7) ?
U1 O1 . 1.776(7) ?
U1 O7 3_445 2.433(7) ?
U1 O5 . 2.441(7) ?
U1 O8 3_445 2.464(7) ?
U1 O10 1_455 2.491(6) ?
U1 O6 . 2.494(8) ?
U1 O9 1_455 2.498(8) ?
U2 O4 . 1.776(8) ?
U2 O3 . 1.778(7) ?
U2 O17 3_545 2.424(7) ?
U2 O18 3_545 2.449(8) ?
U2 O14 . 2.460(7) ?
U2 O13 . 2.470(7) ?
U2 O16 3_445 2.475(7) ?
U2 O15 3_445 2.502(8) ?
Cu1 N4 . 1.953(7) ?
Cu1 N5 . 1.960(7) ?
Cu1 N3 . 2.054(8) ?
Cu1 N6 . 2.076(8) ?
Cu1 O10 1_455 2.362(7) ?
Cu1 O5 . 2.450(6) ?
O5 C4 . 1.268(11) ?
O6 C4 . 1.250(12) ?
O7 C7 . 1.264(12) ?
O8 C7 . 1.255(11) ?
O9 C10 . 1.264(12) ?
O10 C10 . 1.269(11) ?
O11 N1 . 1.209(12) ?
O12 N1 . 1.220(12) ?
O13 C14 . 1.273(12) ?
O14 C14 . 1.254(12) ?
O15 C17 . 1.260(12) ?
O16 C17 . 1.268(12) ?
O17 C20 . 1.282(11) ?
O18 C20 . 1.244(12) ?
O19 N2 . 1.215(13) ?
O20 N2 . 1.214(12) ?
O21 H21A . 0.847600 ?
O21 H21B . 0.825000 ?
O22 H22A . 0.842200 ?
O22 H22B . 0.844100 ?
N1 C1 . 1.559(13) ?
N2 C11 . 1.554(12) ?
N3 C21 . 1.323(12) ?
N3 C25 . 1.353(12) ?
N4 C30 . 1.334(13) ?
N4 C26 . 1.365(12) ?
N5 C31 . 1.336(13) ?
N5 C35 . 1.348(13) ?
N6 C40 . 1.338(14) ?
N6 C36 . 1.349(12) ?
C1 C5 . 1.529(14) ?
C1 C2 . 1.539(13) ?
C1 C8 . 1.551(12) ?
C2 C3 . 1.525(13) ?
C2 H2A . 0.990000 ?
C2 H2B . 0.990000 ?
C3 C4 . 1.504(12) ?
C3 H3A . 0.990000 ?
C3 H3B . 0.990000 ?
C5 C6 . 1.530(13) ?
C5 H5A . 0.990000 ?
C5 H5B . 0.990000 ?
C6 C7 . 1.510(13) ?
C6 H6A . 0.990000 ?
C6 H6B . 0.990000 ?
C8 C9 . 1.517(13) ?
C8 H8A . 0.990000 ?
C8 H8B . 0.990000 ?
C9 C10 . 1.507(12) ?
C9 H9A . 0.990000 ?
C9 H9B . 0.990000 ?
C11 C12 . 1.523(13) ?
C11 C18 . 1.531(12) ?
C11 C15 . 1.546(13) ?
C12 C13 . 1.528(13) ?
C12 H12A . 0.990000 ?
C12 H12B . 0.990000 ?
C13 C14 . 1.504(13) ?
C13 H13A . 0.990000 ?
C13 H13B . 0.990000 ?
C15 C16 . 1.536(12) ?
C15 H15A . 0.990000 ?
C15 H15B . 0.990000 ?
C16 C17 . 1.508(13) ?
C16 H16A . 0.990000 ?
C16 H16B . 0.990000 ?
C18 C19 . 1.537(12) ?
C18 H18A . 0.990000 ?
C18 H18B . 0.990000 ?
C19 C20 . 1.501(12) ?
C19 H19A . 0.990000 ?
C19 H19B . 0.990000 ?
C21 C22 . 1.380(15) ?
C21 H21 . 0.950000 ?
C22 C23 . 1.389(16) ?
C22 H22 . 0.950000 ?
C23 C24 . 1.386(14) ?
C23 H23 . 0.950000 ?
C24 C25 . 1.401(13) ?
C24 H24 . 0.950000 ?
C25 C26 . 1.474(13) ?
C26 C27 . 1.372(13) ?
C27 C28 . 1.392(15) ?
C27 H27 . 0.950000 ?
C28 C29 . 1.379(16) ?
C28 H28 . 0.950000 ?
C29 C30 . 1.387(15) ?
C29 H29 . 0.950000 ?
C30 H30 . 0.950000 ?
C31 C32 . 1.387(14) ?
C31 H31 . 0.950000 ?
C32 C33 . 1.394(17) ?
C32 H32 . 0.950000 ?
C33 C34 . 1.386(16) ?
C33 H33 . 0.950000 ?
C34 C35 . 1.385(14) ?
C34 H34 . 0.950000 ?
C35 C36 . 1.500(14) ?
C36 C37 . 1.387(14) ?
C37 C38 . 1.386(17) ?
C37 H37 . 0.950000 ?
C38 C39 . 1.385(17) ?
C38 H38 . 0.950000 ?
C39 C40 . 1.375(15) ?
C39 H39 . 0.950000 ?
C40 H40 . 0.950000 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 U1 O1 . . 178.4(3) ?
O2 U1 O7 . 3_445 94.2(3) ?
O1 U1 O7 . 3_445 86.6(3) ?
O2 U1 O5 . . 93.5(3) ?
O1 U1 O5 . . 87.2(3) ?
O7 U1 O5 3_445 . 119.6(2) ?
O2 U1 O8 . 3_445 90.4(3) ?
O1 U1 O8 . 3_445 89.1(3) ?
O7 U1 O8 3_445 3_445 52.7(2) ?
O5 U1 O8 . 3_445 171.8(2) ?
O2 U1 O10 . 1_455 89.3(3) ?
O1 U1 O10 . 1_455 89.8(3) ?
O7 U1 O10 3_445 1_455 174.3(2) ?
O5 U1 O10 . 1_455 64.4(2) ?
O8 U1 O10 3_445 1_455 122.9(2) ?
O2 U1 O6 . . 87.4(3) ?
O1 U1 O6 . . 94.2(3) ?
O7 U1 O6 3_445 . 68.5(3) ?
O5 U1 O6 . . 52.2(2) ?
O8 U1 O6 3_445 . 120.8(2) ?
O10 U1 O6 1_455 . 116.1(2) ?
O2 U1 O9 . 1_455 89.7(3) ?
O1 U1 O9 . 1_455 88.6(3) ?
O7 U1 O9 3_445 1_455 123.3(2) ?
O5 U1 O9 . 1_455 116.5(2) ?
O8 U1 O9 3_445 1_455 70.7(2) ?
O10 U1 O9 1_455 1_455 52.2(2) ?
O6 U1 O9 . 1_455 168.1(2) ?
O4 U2 O3 . . 179.4(3) ?
O4 U2 O17 . 3_545 87.4(3) ?
O3 U2 O17 . 3_545 93.1(3) ?
O4 U2 O18 . 3_545 90.3(3) ?
O3 U2 O18 . 3_545 89.7(3) ?
O17 U2 O18 3_545 3_545 52.8(2) ?
O4 U2 O14 . . 90.6(3) ?
O3 U2 O14 . . 88.8(3) ?
O17 U2 O14 3_545 . 173.3(2) ?
O18 U2 O14 3_545 . 120.9(2) ?
O4 U2 O13 . . 89.0(3) ?
O3 U2 O13 . . 90.5(3) ?
O17 U2 O13 3_545 . 120.9(2) ?
O18 U2 O13 3_545 . 68.2(2) ?
O14 U2 O13 . . 52.7(2) ?
O4 U2 O16 . 3_445 89.2(3) ?
O3 U2 O16 . 3_445 91.4(3) ?
O17 U2 O16 3_545 3_445 68.4(2) ?
O18 U2 O16 3_545 3_445 121.2(2) ?
O14 U2 O16 . 3_445 117.9(2) ?
O13 U2 O16 . 3_445 170.4(2) ?
O4 U2 O15 . 3_445 86.7(3) ?
O3 U2 O15 . 3_445 93.3(3) ?
O17 U2 O15 3_545 3_445 120.7(2) ?
O18 U2 O15 3_545 3_445 173.0(2) ?
O14 U2 O15 . 3_445 65.5(2) ?
O13 U2 O15 . 3_445 118.0(2) ?
O16 U2 O15 3_445 3_445 52.5(2) ?
N4 Cu1 N5 . . 179.1(3) ?
N4 Cu1 N3 . . 82.0(3) ?
N5 Cu1 N3 . . 98.9(3) ?
N4 Cu1 N6 . . 98.6(3) ?
N5 Cu1 N6 . . 81.3(3) ?
N3 Cu1 N6 . . 115.9(3) ?
N4 Cu1 O10 . 1_455 92.4(3) ?
N5 Cu1 O10 . 1_455 86.7(3) ?
N3 Cu1 O10 . 1_455 152.6(2) ?
N6 Cu1 O10 . 1_455 91.4(3) ?
C4 O5 U1 . . 95.3(5) ?
C4 O6 U1 . . 93.3(6) ?
C7 O7 U1 . 3 94.0(5) ?
C7 O8 U1 . 3 92.8(5) ?
C10 O9 U1 . 1_655 93.6(6) ?
C10 O10 Cu1 . 1_655 145.7(6) ?
C10 O10 U1 . 1_655 93.8(5) ?
Cu1 O10 U1 1_655 1_655 113.7(2) ?
C14 O13 U2 . . 93.2(6) ?
C14 O14 U2 . . 94.1(6) ?
C17 O15 U2 . 3 91.7(6) ?
C17 O16 U2 . 3 92.7(5) ?
C20 O17 U2 . 3_455 94.6(6) ?
C20 O18 U2 . 3_455 94.5(6) ?
H21A O21 H21B . . 107.600000 ?
H22A O22 H22B . . 106.200000 ?
O11 N1 O12 . . 124.2(9) ?
O11 N1 C1 . . 117.0(9) ?
O12 N1 C1 . . 118.8(8) ?
O20 N2 O19 . . 123.7(9) ?
O20 N2 C11 . . 118.1(8) ?
O19 N2 C11 . . 118.1(9) ?
C21 N3 C25 . . 119.3(8) ?
C21 N3 Cu1 . . 128.7(7) ?
C25 N3 Cu1 . . 111.8(6) ?
C30 N4 C26 . . 119.2(8) ?
C30 N4 Cu1 . . 125.8(7) ?
C26 N4 Cu1 . . 115.0(6) ?
C31 N5 C35 . . 119.3(8) ?
C31 N5 Cu1 . . 124.3(7) ?
C35 N5 Cu1 . . 116.4(7) ?
C40 N6 C36 . . 118.9(9) ?
C40 N6 Cu1 . . 128.5(7) ?
C36 N6 Cu1 . . 112.6(6) ?
C5 C1 C2 . . 113.6(8) ?
C5 C1 C8 . . 114.1(7) ?
C2 C1 C8 . . 110.4(7) ?
C5 C1 N1 . . 107.8(7) ?
C2 C1 N1 . . 104.6(7) ?
C8 C1 N1 . . 105.5(7) ?
C3 C2 C1 . . 113.5(8) ?
C3 C2 H2A . . 108.900000 ?
C1 C2 H2A . . 108.900000 ?
C3 C2 H2B . . 108.900000 ?
C1 C2 H2B . . 108.900000 ?
H2A C2 H2B . . 107.700000 ?
C4 C3 C2 . . 115.5(8) ?
C4 C3 H3A . . 108.400000 ?
C2 C3 H3A . . 108.400000 ?
C4 C3 H3B . . 108.400000 ?
C2 C3 H3B . . 108.400000 ?
H3A C3 H3B . . 107.500000 ?
O6 C4 O5 . . 119.2(8) ?
O6 C4 C3 . . 122.6(8) ?
O5 C4 C3 . . 118.2(8) ?
C1 C5 C6 . . 113.0(7) ?
C1 C5 H5A . . 109.000000 ?
C6 C5 H5A . . 109.000000 ?
C1 C5 H5B . . 109.000000 ?
C6 C5 H5B . . 109.000000 ?
H5A C5 H5B . . 107.800000 ?
C7 C6 C5 . . 107.5(7) ?
C7 C6 H6A . . 110.200000 ?
C5 C6 H6A . . 110.200000 ?
C7 C6 H6B . . 110.200000 ?
C5 C6 H6B . . 110.200000 ?
H6A C6 H6B . . 108.500000 ?
O8 C7 O7 . . 119.3(8) ?
O8 C7 C6 . . 120.7(8) ?
O7 C7 C6 . . 119.9(8) ?
C9 C8 C1 . . 113.6(7) ?
C9 C8 H8A . . 108.800000 ?
C1 C8 H8A . . 108.800000 ?
C9 C8 H8B . . 108.800000 ?
C1 C8 H8B . . 108.800000 ?
H8A C8 H8B . . 107.700000 ?
C10 C9 C8 . . 115.2(8) ?
C10 C9 H9A . . 108.500000 ?
C8 C9 H9A . . 108.500000 ?
C10 C9 H9B . . 108.500000 ?
C8 C9 H9B . . 108.500000 ?
H9A C9 H9B . . 107.500000 ?
O9 C10 O10 . . 120.1(8) ?
O9 C10 C9 . . 120.5(8) ?
O10 C10 C9 . . 119.3(8) ?
O9 C10 U1 . 1_655 60.3(5) ?
O10 C10 U1 . 1_655 60.0(4) ?
C9 C10 U1 . 1_655 174.9(6) ?
C12 C11 C18 . . 113.9(7) ?
C12 C11 C15 . . 113.9(8) ?
C18 C11 C15 . . 108.8(7) ?
C12 C11 N2 . . 107.0(7) ?
C18 C11 N2 . . 107.6(7) ?
C15 C11 N2 . . 105.0(7) ?
C11 C12 C13 . . 113.3(8) ?
C11 C12 H12A . . 108.900000 ?
C13 C12 H12A . . 108.900000 ?
C11 C12 H12B . . 108.900000 ?
C13 C12 H12B . . 108.900000 ?
H12A C12 H12B . . 107.700000 ?
C14 C13 C12 . . 109.4(7) ?
C14 C13 H13A . . 109.800000 ?
C12 C13 H13A . . 109.800000 ?
C14 C13 H13B . . 109.800000 ?
C12 C13 H13B . . 109.800000 ?
H13A C13 H13B . . 108.200000 ?
O14 C14 O13 . . 119.9(9) ?
O14 C14 C13 . . 120.9(9) ?
O13 C14 C13 . . 119.2(8) ?
C16 C15 C11 . . 114.5(8) ?
C16 C15 H15A . . 108.600000 ?
C11 C15 H15A . . 108.600000 ?
C16 C15 H15B . . 108.600000 ?
C11 C15 H15B . . 108.600000 ?
H15A C15 H15B . . 107.600000 ?
C17 C16 C15 . . 114.4(8) ?
C17 C16 H16A . . 108.600000 ?
C15 C16 H16A . . 108.600000 ?
C17 C16 H16B . . 108.600000 ?
C15 C16 H16B . . 108.600000 ?
H16A C16 H16B . . 107.600000 ?
O15 C17 O16 . . 121.1(9) ?
O15 C17 C16 . . 120.4(9) ?
O16 C17 C16 . . 118.4(8) ?
C11 C18 C19 . . 113.7(8) ?
C11 C18 H18A . . 108.800000 ?
C19 C18 H18A . . 108.800000 ?
C11 C18 H18B . . 108.800000 ?
C19 C18 H18B . . 108.800000 ?
H18A C18 H18B . . 107.700000 ?
C20 C19 C18 . . 113.4(8) ?
C20 C19 H19A . . 108.900000 ?
C18 C19 H19A . . 108.900000 ?
C20 C19 H19B . . 108.900000 ?
C18 C19 H19B . . 108.900000 ?
H19A C19 H19B . . 107.700000 ?
O18 C20 O17 . . 118.1(8) ?
O18 C20 C19 . . 123.2(8) ?
O17 C20 C19 . . 118.5(8) ?
N3 C21 C22 . . 123.1(9) ?
N3 C21 H21 . . 118.400000 ?
C22 C21 H21 . . 118.400000 ?
C21 C22 C23 . . 117.9(10) ?
C21 C22 H22 . . 121.100000 ?
C23 C22 H22 . . 121.100000 ?
C24 C23 C22 . . 120.3(10) ?
C24 C23 H23 . . 119.800000 ?
C22 C23 H23 . . 119.800000 ?
C23 C24 C25 . . 117.7(9) ?
C23 C24 H24 . . 121.100000 ?
C25 C24 H24 . . 121.100000 ?
N3 C25 C24 . . 121.5(8) ?
N3 C25 C26 . . 115.4(8) ?
C24 C25 C26 . . 123.0(8) ?
N4 C26 C27 . . 120.8(9) ?
N4 C26 C25 . . 114.9(8) ?
C27 C26 C25 . . 124.2(8) ?
C26 C27 C28 . . 120.3(9) ?
C26 C27 H27 . . 119.800000 ?
C28 C27 H27 . . 119.800000 ?
C29 C28 C27 . . 118.1(10) ?
C29 C28 H28 . . 120.900000 ?
C27 C28 H28 . . 120.900000 ?
C28 C29 C30 . . 119.5(10) ?
C28 C29 H29 . . 120.300000 ?
C30 C29 H29 . . 120.300000 ?
N4 C30 C29 . . 122.1(9) ?
N4 C30 H30 . . 119.000000 ?
C29 C30 H30 . . 119.000000 ?
N5 C31 C32 . . 122.4(10) ?
N5 C31 H31 . . 118.800000 ?
C32 C31 H31 . . 118.800000 ?
C31 C32 C33 . . 118.0(10) ?
C31 C32 H32 . . 121.000000 ?
C33 C32 H32 . . 121.000000 ?
C34 C33 C32 . . 119.7(9) ?
C34 C33 H33 . . 120.100000 ?
C32 C33 H33 . . 120.100000 ?
C35 C34 C33 . . 118.5(10) ?
C35 C34 H34 . . 120.800000 ?
C33 C34 H34 . . 120.800000 ?
N5 C35 C34 . . 122.0(10) ?
N5 C35 C36 . . 114.9(8) ?
C34 C35 C36 . . 123.1(9) ?
N6 C36 C37 . . 121.8(9) ?
N6 C36 C35 . . 114.8(8) ?
C37 C36 C35 . . 123.5(9) ?
C38 C37 C36 . . 119.0(10) ?
C38 C37 H37 . . 120.500000 ?
C36 C37 H37 . . 120.500000 ?
C39 C38 C37 . . 118.7(10) ?
C39 C38 H38 . . 120.700000 ?
C37 C38 H38 . . 120.700000 ?
C40 C39 C38 . . 119.5(11) ?
C40 C39 H39 . . 120.300000 ?
C38 C39 H39 . . 120.300000 ?
N6 C40 C39 . . 122.2(10) ?
N6 C40 H40 . . 118.900000 ?
C39 C40 H40 . . 118.900000 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O21 H21A O11 . 0.85 2.17 3.011(13) 172.1 ?
O21 H21B O23 4 0.82 2.37 2.787(16) 112.2 ?
O22 H22A O8 3_445 0.84 2.11 2.928(10) 165.0 ?
O22 H22B O23 . 0.84 1.96 2.794(12) 170.4 ?
C8 H8B O3 1_655 0.99 2.59 3.278(11) 127.0 ?
C16 H16B O20 . 0.99 2.48 3.195(14) 128.6 ?
C18 H18B O2 3_455 0.99 2.38 3.154(11) 135.0 ?
C21 H21 O23 4 0.95 2.55 3.283(14) 133.8 ?
C22 H22 O4 2_665 0.95 2.48 3.241(13) 137.4 ?
C24 H24 O9 3_455 0.95 2.46 3.383(13) 164.5 ?
C27 H27 O9 3_455 0.95 2.32 3.226(13) 159.7 ?
C29 H29 O13 . 0.95 2.32 3.186(14) 151.0 ?
C31 H31 O21 . 0.95 2.48 3.243(14) 137.5 ?

####################################################################### 
# 
# 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 2264770'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2023-05-23 deposited with the CCDC.	2023-06-21 downloaded from the CCDC.
;

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H30 N O10 P U'
_chemical_formula_iupac          ?
_chemical_formula_weight         821.54

_chemical_melting_point          ?

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

_cell_length_a                   11.4827(4)
_cell_length_b                   14.2168(5)
_cell_length_c                   17.7990(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.2934(15)
_cell_angle_gamma                90
_cell_volume                     2903.31(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9765
_cell_measurement_theta_min      2.5205
_cell_measurement_theta_max      30.5304
_cell_measurement_temperature    100(2)

_exptl_crystal_description       irregular
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.042
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1592

_exptl_absorpt_coefficient_mu    5.705
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.51
_exptl_absorpt_correction_T_max  0.75

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100(2)

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

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

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

_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_detector_area_resol_mean 7.41

_diffrn_reflns_number            89833
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_full        28.70
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24

_refine_special_details          
;
;

_reflns_number_total             7497
_reflns_number_gt                6879
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0206
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0554
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_number_reflns         7497
_refine_ls_number_parameters     380
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0269P)²+3.7806P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.434
_refine_diff_density_min         -1.576
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U U1 0.67167(2) 0.52116(2) 0.72475(2) 0.01084(4) Uani d . . . 1 . .
P P1 0.73947(5) 0.36069(4) 0.46766(3) 0.01258(11) Uani d . . . 1 . .
O O1 0.70275(16) 0.42354(12) 0.66698(10) 0.0162(3) Uani d . . . 1 . .
O O2 0.64058(17) 0.62147(14) 0.78007(10) 0.0212(4) Uani d . . . 1 . .
O O3 0.46372(17) 0.49226(14) 0.68861(11) 0.0192(4) Uani d . . . 1 . .
O O4 0.52879(16) 0.43326(16) 0.79634(11) 0.0242(4) Uani d . . . 1 . .
O O5 -0.24103(15) 0.43692(13) 0.83195(10) 0.0182(4) Uani d . . . 1 . .
O O6 -0.12408(17) 0.52645(12) 0.76866(12) 0.0193(4) Uani d . . . 1 . .
O O7 0.21025(15) 0.12267(12) 0.85552(10) 0.0170(3) Uani d . . . 1 . .
O O8 0.39737(15) 0.11878(12) 0.88454(10) 0.0160(3) Uani d . . . 1 . .
O O9 0.15566(19) 0.54589(14) 0.96248(12) 0.0245(4) Uani d . . . 1 . .
O O10 0.20258(19) 0.41313(14) 1.01401(10) 0.0251(4) Uani d . . . 1 . .
N N1 0.18021(18) 0.46200(15) 0.95880(12) 0.0147(4) Uani d . . . 1 . .
C C1 0.1860(2) 0.41830(16) 0.87992(13) 0.0126(4) Uani d . . . 1 . .
C C2 0.2988(2) 0.45826(18) 0.84929(14) 0.0150(4) Uani d . . . 1 . .
H H2A 0.294044 0.527787 0.849055 0.018000 Uiso calc U . R 1 . .
H H2B 0.365096 0.440102 0.883554 0.018000 Uiso calc U . R 1 . .
C C3 0.3231(2) 0.4243(2) 0.76979(14) 0.0217(6) Uani d . . . 1 . .
H H3A 0.314161 0.355066 0.767040 0.026000 Uiso calc U . R 1 . .
H H3B 0.266220 0.452904 0.733292 0.026000 Uiso calc U . R 1 . .
C C4 0.4456(2) 0.4514(2) 0.75002(14) 0.0175(5) Uani d . . . 1 . .
C C5 0.0792(2) 0.45413(17) 0.83425(14) 0.0143(4) Uani d . . . 1 . .
H H5A 0.083957 0.523523 0.830852 0.017000 Uiso calc U . R 1 . .
H H5B 0.081840 0.428813 0.782529 0.017000 Uiso calc U . R 1 . .
C C6 -0.0374(2) 0.42785(18) 0.86627(14) 0.0147(4) Uani d . . . 1 . .
H H6A -0.043716 0.358469 0.868666 0.018000 Uiso calc U . R 1 . .
H H6B -0.040505 0.452454 0.918183 0.018000 Uiso calc U . R 1 . .
C C7 -0.1393(2) 0.46611(17) 0.81998(14) 0.0135(4) Uani d . . . 1 . .
C C8 0.1837(2) 0.31065(16) 0.88619(14) 0.0137(4) Uani d . . . 1 . .
H H8A 0.119969 0.293522 0.919468 0.016000 Uiso calc U . R 1 . .
H H8B 0.162720 0.285090 0.835707 0.016000 Uiso calc U . R 1 . .
C C9 0.2941(2) 0.26027(17) 0.91534(15) 0.0183(5) Uani d . . . 1 . .
H H9A 0.363331 0.296130 0.900384 0.022000 Uiso calc U . R 1 . .
H H9B 0.295088 0.257931 0.970956 0.022000 Uiso calc U . R 1 . .
C C10 0.3004(2) 0.16140(17) 0.88466(13) 0.0138(4) Uani d . . . 1 . .
C C11 0.6812(2) 0.47735(17) 0.47173(15) 0.0181(5) Uani d . . . 1 . .
H H11A 0.610781 0.481572 0.438924 0.027000 Uiso calc U . R 1 . .
H H11B 0.739252 0.522423 0.454937 0.027000 Uiso calc U . R 1 . .
H H11C 0.661649 0.491886 0.523550 0.027000 Uiso calc U . R 1 . .
C C12 0.8716(2) 0.35127(17) 0.52517(13) 0.0133(4) Uani d . . . 1 . .
C C13 0.9272(2) 0.26363(18) 0.52986(14) 0.0176(5) Uani d . . . 1 . .
H H13 0.896385 0.211760 0.501874 0.021000 Uiso calc U . R 1 . .
C C14 1.0274(2) 0.2526(2) 0.57552(15) 0.0213(5) Uani d . . . 1 . .
H H14 1.065514 0.193303 0.578513 0.026000 Uiso calc U . R 1 . .
C C15 1.0715(2) 0.3282(2) 0.61662(16) 0.0234(5) Uani d . . . 1 . .
H H15 1.140073 0.320552 0.647694 0.028000 Uiso calc U . R 1 . .
C C16 1.0166(2) 0.4150(2) 0.61283(15) 0.0221(5) Uani d . . . 1 . .
H H16 1.047191 0.466208 0.641674 0.027000 Uiso calc U . R 1 . .
C C17 0.9163(2) 0.42745(18) 0.56666(14) 0.0167(5) Uani d . . . 1 . .
H H17 0.878972 0.487043 0.563568 0.020000 Uiso calc U . R 1 . .
C C18 0.6355(2) 0.27695(17) 0.49958(13) 0.0143(4) Uani d . . . 1 . .
C C19 0.6401(2) 0.18426(18) 0.47363(14) 0.0175(5) Uani d . . . 1 . .
H H19 0.692169 0.167484 0.435693 0.021000 Uiso calc U . R 1 . .
C C20 0.5679(2) 0.11695(18) 0.50383(15) 0.0199(5) Uani d . . . 1 . .
H H20 0.570540 0.053873 0.486363 0.024000 Uiso calc U . R 1 . .
C C21 0.4917(2) 0.1411(2) 0.55938(15) 0.0207(5) Uani d . . . 1 . .
H H21 0.444089 0.094350 0.580685 0.025000 Uiso calc U . R 1 . .
C C22 0.4852(2) 0.2339(2) 0.58383(14) 0.0202(5) Uani d . . . 1 . .
H H22 0.431951 0.250509 0.621098 0.024000 Uiso calc U . R 1 . .
C C23 0.5562(2) 0.30208(19) 0.55402(14) 0.0174(5) Uani d . . . 1 . .
H H23 0.551093 0.365510 0.570367 0.021000 Uiso calc U . R 1 . .
C C24 0.7717(2) 0.33299(16) 0.37231(13) 0.0144(4) Uani d . . . 1 . .
C C25 0.6785(2) 0.31084(18) 0.32236(14) 0.0181(5) Uani d . . . 1 . .
H H25 0.600877 0.310424 0.338874 0.022000 Uiso calc U . R 1 . .
C C26 0.7014(3) 0.28945(19) 0.24824(15) 0.0218(5) Uani d . . . 1 . .
H H26 0.639040 0.273801 0.213830 0.026000 Uiso calc U . R 1 . .
C C27 0.8147(3) 0.29083(19) 0.22422(15) 0.0230(6) Uani d . . . 1 . .
H H27 0.829578 0.274669 0.173709 0.028000 Uiso calc U . R 1 . .
C C28 0.9066(3) 0.31554(18) 0.27316(15) 0.0206(5) Uani d . . . 1 . .
H H28 0.983651 0.318525 0.255702 0.025000 Uiso calc U . R 1 . .
C C29 0.8858(2) 0.33595(17) 0.34781(14) 0.0170(5) Uani d . . . 1 . .
H H29 0.948603 0.351759 0.381880 0.020000 Uiso calc U . R 1 . .


_geom_special_details            
;

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
U1 O1 . 1.7721(17) ?
U1 O2 . 1.7773(18) ?
U1 O5 1_655 2.4345(18) ?
U1 O6 1_655 2.4434(19) ?
U1 O4 . 2.4585(19) ?
U1 O7 2_656 2.4732(18) ?
U1 O3 . 2.4823(19) ?
U1 O8 2_656 2.4930(17) ?
P1 C11 . 1.791(2) ?
P1 C18 . 1.795(2) ?
P1 C24 . 1.795(2) ?
P1 C12 . 1.801(2) ?
O3 C4 . 1.262(3) ?
O4 C4 . 1.263(3) ?
O5 C7 . 1.266(3) ?
O6 C7 . 1.270(3) ?
O7 C10 . 1.265(3) ?
O8 C10 . 1.268(3) ?
O9 N1 . 1.228(3) ?
O10 N1 . 1.222(3) ?
N1 C1 . 1.539(3) ?
C1 C5 . 1.531(3) ?
C1 C2 . 1.535(3) ?
C1 C8 . 1.535(3) ?
C2 C3 . 1.531(3) ?
C2 H2A . 0.990000 ?
C2 H2B . 0.990000 ?
C3 C4 . 1.514(3) ?
C3 H3A . 0.990000 ?
C3 H3B . 0.990000 ?
C5 C6 . 1.523(3) ?
C5 H5A . 0.990000 ?
C5 H5B . 0.990000 ?
C6 C7 . 1.505(3) ?
C6 H6A . 0.990000 ?
C6 H6B . 0.990000 ?
C8 C9 . 1.529(3) ?
C8 H8A . 0.990000 ?
C8 H8B . 0.990000 ?
C9 C10 . 1.511(3) ?
C9 H9A . 0.990000 ?
C9 H9B . 0.990000 ?
C11 H11A . 0.980000 ?
C11 H11B . 0.980000 ?
C11 H11C . 0.980000 ?
C12 C17 . 1.397(3) ?
C12 C13 . 1.401(3) ?
C13 C14 . 1.391(4) ?
C13 H13 . 0.950000 ?
C14 C15 . 1.385(4) ?
C14 H14 . 0.950000 ?
C15 C16 . 1.386(4) ?
C15 H15 . 0.950000 ?
C16 C17 . 1.399(4) ?
C16 H16 . 0.950000 ?
C17 H17 . 0.950000 ?
C18 C19 . 1.398(3) ?
C18 C23 . 1.402(3) ?
C19 C20 . 1.389(4) ?
C19 H19 . 0.950000 ?
C20 C21 . 1.389(4) ?
C20 H20 . 0.950000 ?
C21 C22 . 1.391(4) ?
C21 H21 . 0.950000 ?
C22 C23 . 1.385(4) ?
C22 H22 . 0.950000 ?
C23 H23 . 0.950000 ?
C24 C29 . 1.399(4) ?
C24 C25 . 1.399(3) ?
C25 C26 . 1.389(4) ?
C25 H25 . 0.950000 ?
C26 C27 . 1.386(4) ?
C26 H26 . 0.950000 ?
C27 C28 . 1.386(4) ?
C27 H27 . 0.950000 ?
C28 C29 . 1.390(4) ?
C28 H28 . 0.950000 ?
C29 H29 . 0.950000 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 U1 O2 . . 178.13(8) ?
O1 U1 O5 . 1_655 89.04(7) ?
O2 U1 O5 . 1_655 92.64(8) ?
O1 U1 O6 . 1_655 89.81(8) ?
O2 U1 O6 . 1_655 90.55(8) ?
O5 U1 O6 1_655 1_655 53.46(6) ?
O1 U1 O4 . . 93.25(8) ?
O2 U1 O4 . . 88.15(8) ?
O5 U1 O4 1_655 . 66.80(6) ?
O6 U1 O4 1_655 . 120.12(6) ?
O1 U1 O7 . 2_656 89.65(7) ?
O2 U1 O7 . 2_656 88.78(8) ?
O5 U1 O7 1_655 2_656 121.45(6) ?
O6 U1 O7 1_655 2_656 68.00(6) ?
O4 U1 O7 . 2_656 171.34(6) ?
O1 U1 O3 . . 86.21(8) ?
O2 U1 O3 . . 93.67(8) ?
O5 U1 O3 1_655 . 118.90(6) ?
O6 U1 O3 1_655 . 171.52(6) ?
O4 U1 O3 . . 52.78(6) ?
O7 U1 O3 2_656 . 119.39(6) ?
O1 U1 O8 . 2_656 92.77(7) ?
O2 U1 O8 . 2_656 85.47(7) ?
O5 U1 O8 1_655 2_656 173.47(6) ?
O6 U1 O8 1_655 2_656 120.24(6) ?
O4 U1 O8 . 2_656 119.30(6) ?
O7 U1 O8 2_656 2_656 52.34(6) ?
O3 U1 O8 . 2_656 67.50(6) ?
C11 P1 C18 . . 110.30(13) ?
C11 P1 C24 . . 109.44(12) ?
C18 P1 C24 . . 108.59(11) ?
C11 P1 C12 . . 110.70(12) ?
C18 P1 C12 . . 109.08(11) ?
C24 P1 C12 . . 108.68(11) ?
C4 O3 U1 . . 92.39(15) ?
C4 O4 U1 . . 93.47(15) ?
C7 O5 U1 . 1_455 93.48(15) ?
C7 O6 U1 . 1_455 92.94(15) ?
C10 O7 U1 . 2_646 91.86(14) ?
C10 O8 U1 . 2_646 90.88(14) ?
O10 N1 O9 . . 123.4(2) ?
O10 N1 C1 . . 119.2(2) ?
O9 N1 C1 . . 117.3(2) ?
C5 C1 C2 . . 110.98(19) ?
C5 C1 C8 . . 110.75(19) ?
C2 C1 C8 . . 114.4(2) ?
C5 C1 N1 . . 106.67(19) ?
C2 C1 N1 . . 104.04(18) ?
C8 C1 N1 . . 109.55(19) ?
C3 C2 C1 . . 113.5(2) ?
C3 C2 H2A . . 108.900000 ?
C1 C2 H2A . . 108.900000 ?
C3 C2 H2B . . 108.900000 ?
C1 C2 H2B . . 108.900000 ?
H2A C2 H2B . . 107.700000 ?
C4 C3 C2 . . 109.8(2) ?
C4 C3 H3A . . 109.700000 ?
C2 C3 H3A . . 109.700000 ?
C4 C3 H3B . . 109.700000 ?
C2 C3 H3B . . 109.700000 ?
H3A C3 H3B . . 108.200000 ?
O3 C4 O4 . . 120.9(2) ?
O3 C4 C3 . . 120.3(2) ?
O4 C4 C3 . . 118.8(2) ?
O3 C4 U1 . . 61.16(13) ?
O4 C4 U1 . . 60.08(13) ?
C3 C4 U1 . . 173.1(2) ?
C6 C5 C1 . . 114.7(2) ?
C6 C5 H5A . . 108.600000 ?
C1 C5 H5A . . 108.600000 ?
C6 C5 H5B . . 108.600000 ?
C1 C5 H5B . . 108.600000 ?
H5A C5 H5B . . 107.600000 ?
C7 C6 C5 . . 112.5(2) ?
C7 C6 H6A . . 109.100000 ?
C5 C6 H6A . . 109.100000 ?
C7 C6 H6B . . 109.100000 ?
C5 C6 H6B . . 109.100000 ?
H6A C6 H6B . . 107.800000 ?
O5 C7 O6 . . 119.8(2) ?
O5 C7 C6 . . 119.4(2) ?
O6 C7 C6 . . 120.8(2) ?
O5 C7 U1 . 1_455 59.82(13) ?
O6 C7 U1 . 1_455 60.24(13) ?
C6 C7 U1 . 1_455 174.26(17) ?
C9 C8 C1 . . 118.4(2) ?
C9 C8 H8A . . 107.700000 ?
C1 C8 H8A . . 107.700000 ?
C9 C8 H8B . . 107.700000 ?
C1 C8 H8B . . 107.700000 ?
H8A C8 H8B . . 107.100000 ?
C10 C9 C8 . . 111.4(2) ?
C10 C9 H9A . . 109.400000 ?
C8 C9 H9A . . 109.400000 ?
C10 C9 H9B . . 109.400000 ?
C8 C9 H9B . . 109.400000 ?
H9A C9 H9B . . 108.000000 ?
O7 C10 O8 . . 119.7(2) ?
O7 C10 C9 . . 120.2(2) ?
O8 C10 C9 . . 120.0(2) ?
O7 C10 U1 . 2_646 61.44(12) ?
O8 C10 U1 . 2_646 62.34(12) ?
C9 C10 U1 . 2_646 156.59(17) ?
P1 C11 H11A . . 109.500000 ?
P1 C11 H11B . . 109.500000 ?
H11A C11 H11B . . 109.500000 ?
P1 C11 H11C . . 109.500000 ?
H11A C11 H11C . . 109.500000 ?
H11B C11 H11C . . 109.500000 ?
C17 C12 C13 . . 120.1(2) ?
C17 C12 P1 . . 121.74(19) ?
C13 C12 P1 . . 118.12(18) ?
C14 C13 C12 . . 120.0(2) ?
C14 C13 H13 . . 120.000000 ?
C12 C13 H13 . . 120.000000 ?
C15 C14 C13 . . 119.8(3) ?
C15 C14 H14 . . 120.100000 ?
C13 C14 H14 . . 120.100000 ?
C14 C15 C16 . . 120.6(3) ?
C14 C15 H15 . . 119.700000 ?
C16 C15 H15 . . 119.700000 ?
C15 C16 C17 . . 120.2(2) ?
C15 C16 H16 . . 119.900000 ?
C17 C16 H16 . . 119.900000 ?
C12 C17 C16 . . 119.3(2) ?
C12 C17 H17 . . 120.400000 ?
C16 C17 H17 . . 120.400000 ?
C19 C18 C23 . . 120.2(2) ?
C19 C18 P1 . . 119.08(19) ?
C23 C18 P1 . . 120.57(19) ?
C20 C19 C18 . . 119.4(2) ?
C20 C19 H19 . . 120.300000 ?
C18 C19 H19 . . 120.300000 ?
C19 C20 C21 . . 120.5(2) ?
C19 C20 H20 . . 119.700000 ?
C21 C20 H20 . . 119.700000 ?
C20 C21 C22 . . 120.0(2) ?
C20 C21 H21 . . 120.000000 ?
C22 C21 H21 . . 120.000000 ?
C23 C22 C21 . . 120.2(2) ?
C23 C22 H22 . . 119.900000 ?
C21 C22 H22 . . 119.900000 ?
C22 C23 C18 . . 119.6(2) ?
C22 C23 H23 . . 120.200000 ?
C18 C23 H23 . . 120.200000 ?
C29 C24 C25 . . 120.7(2) ?
C29 C24 P1 . . 121.28(19) ?
C25 C24 P1 . . 117.97(19) ?
C26 C25 C24 . . 118.9(3) ?
C26 C25 H25 . . 120.500000 ?
C24 C25 H25 . . 120.500000 ?
C27 C26 C25 . . 120.4(3) ?
C27 C26 H26 . . 119.800000 ?
C25 C26 H26 . . 119.800000 ?
C26 C27 C28 . . 120.7(2) ?
C26 C27 H27 . . 119.700000 ?
C28 C27 H27 . . 119.700000 ?
C27 C28 C29 . . 119.9(3) ?
C27 C28 H28 . . 120.100000 ?
C29 C28 H28 . . 120.100000 ?
C28 C29 C24 . . 119.4(2) ?
C28 C29 H29 . . 120.300000 ?
C24 C29 H29 . . 120.300000 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C6 H6B O9 3_567 0.99 2.55 3.407(3) 145.2 ?
C11 H11A O3 3_666 0.98 2.42 3.274(3) 145.1 ?
C11 H11C O8 2_656 0.98 2.55 3.404(3) 146.2 ?
C13 H13 O9 2_646 0.95 2.52 3.243(3) 132.9 ?
C19 H19 O5 4_665 0.95 2.51 3.386(3) 152.9 ?
C23 H23 O1 . 0.95 2.54 3.096(3) 117.9 ?

