# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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 2290585'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2023-08-24 deposited with the CCDC.	2024-02-01 downloaded from the CCDC.
;

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H16.50 N1.50 O6 U'
_chemical_formula_iupac          ?
_chemical_formula_weight         623.89

_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                   8.7652(4)
_cell_length_b                   10.7608(5)
_cell_length_c                   11.2060(5)
_cell_angle_alpha                103.3336(18)
_cell_angle_beta                 92.5999(18)
_cell_angle_gamma                107.6526(17)
_cell_volume                     972.43(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9914
_cell_measurement_theta_min      2.4043
_cell_measurement_theta_max      30.8893
_cell_measurement_temperature    100(2)

_exptl_crystal_description       lath
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.033
_exptl_crystal_density_diffrn    2.131
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             586

_exptl_absorpt_coefficient_mu    8.386
_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  0.55
_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            50533
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_theta_min         1.88
_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       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13

_refine_special_details          
;
One of the solvent acetonitrile molecules has been given
an occupancy factor of 0.5 to account for its closeness
to its image by symmetry.
;

_reflns_number_total             3696
_reflns_number_gt                3431
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0210
_refine_ls_wR_factor_gt          0.0447
_refine_ls_wR_factor_ref         0.0456
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_restrained_S_all      1.152
_refine_ls_number_reflns         3696
_refine_ls_number_parameters     282
_refine_ls_number_restraints     12
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0027P)²+3.1447P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.947
_refine_diff_density_min         -1.733
_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_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 0.70112(2) 0.44623(2) 0.53846(2) 0.02048(5) Uani d . . . 1 . .
O O1 0.6068(4) 0.2881(3) 0.4342(3) 0.0322(7) Uani d . . . 1 . .
O O2 0.7952(4) 0.6062(3) 0.6411(3) 0.0299(7) Uani d . . . 1 . .
O O3 0.5717(3) 0.5510(3) 0.4163(3) 0.0232(6) Uani d . . . 1 . .
O O4 0.4497(4) 0.6314(3) 0.2934(3) 0.0302(7) Uani d . . . 1 . .
O O5 0.8808(3) 0.5027(3) 0.4006(3) 0.0247(6) Uani d . . . 1 . .
O O6 1.1155(4) 0.6498(3) 0.3870(3) 0.0302(7) Uani d . . . 1 . .
N N1 0.4818(6) 0.3089(6) 0.1459(4) 0.0524(12) Uani d . . . 1 . .
C C1 0.7178(5) 0.6212(4) 0.2548(4) 0.0245(9) Uani d U . . 1 . .
H H1 0.725484 0.529491 0.218985 0.029000 Uiso calc U . R 1 . .
C C2 0.8765(5) 0.7042(4) 0.3433(4) 0.0223(8) Uani d U . . 1 . .
H H2 0.844209 0.749892 0.421639 0.027000 Uiso calc U . R 1 . .
C C3 0.5712(5) 0.6021(4) 0.3214(4) 0.0263(9) Uani d . . . 1 . .
C C4 0.9647(5) 0.6112(4) 0.3775(4) 0.0246(9) Uani d . . . 1 . .
C C5 0.7117(5) 0.6879(4) 0.1451(4) 0.0259(9) Uani d . . . 1 . .
H H5 0.609676 0.641310 0.086970 0.031000 Uiso calc U . R 1 . .
C C6 0.9808(5) 0.8164(4) 0.2901(4) 0.0231(9) Uani d . . . 1 . .
H H6 1.085593 0.868379 0.343684 0.028000 Uiso calc U . R 1 . .
C C7 0.8598(5) 0.6811(4) 0.0821(4) 0.0252(9) Uani d . . . 1 . .
C C8 1.0053(5) 0.7493(4) 0.1619(4) 0.0240(9) Uani d . . . 1 . .
C C9 1.1517(5) 0.7530(4) 0.1179(4) 0.0287(10) Uani d . . . 1 . .
H H9 1.249751 0.796375 0.171883 0.034000 Uiso calc U . R 1 . .
C C10 1.1541(6) 0.6930(5) -0.0054(4) 0.0317(10) Uani d . . . 1 . .
H H10 1.254341 0.697658 -0.036214 0.038000 Uiso calc U . R 1 . .
C C11 1.0109(6) 0.6263(5) -0.0838(4) 0.0325(11) Uani d . . . 1 . .
H H11 1.014194 0.586252 -0.168201 0.039000 Uiso calc U . R 1 . .
C C12 0.8619(6) 0.6173(5) -0.0404(4) 0.0293(10) Uani d . . . 1 . .
H H12 0.764088 0.568592 -0.093635 0.035000 Uiso calc U . R 1 . .
C C13 0.7350(5) 0.8358(5) 0.1983(4) 0.0265(10) Uani d . . . 1 . .
C C14 0.6327(6) 0.9058(5) 0.1715(4) 0.0296(10) Uani d . . . 1 . .
H H14 0.532306 0.859248 0.120963 0.036000 Uiso calc U . R 1 . .
C C15 0.6802(6) 1.0452(5) 0.2203(5) 0.0374(12) Uani d . . . 1 . .
H H15 0.612063 1.093675 0.201272 0.045000 Uiso calc U . R 1 . .
C C16 0.8251(6) 1.1146(5) 0.2960(5) 0.0368(11) Uani d . . . 1 . .
H H16 0.855964 1.209694 0.327876 0.044000 Uiso calc U . R 1 . .
C C17 0.9258(6) 1.0433(5) 0.3252(4) 0.0338(11) Uani d . . . 1 . .
H H17 1.023557 1.089337 0.379137 0.041000 Uiso calc U . R 1 . .
C C18 0.8813(5) 0.9058(4) 0.2747(4) 0.0260(9) Uani d . . . 1 . .
C C19 0.3682(8) 0.2225(6) 0.1416(5) 0.0433(13) Uani d . . . 1 . .
C C20 0.2207(10) 0.1119(7) 0.1323(9) 0.093(3) Uani d . . . 1 . .
H H20A 0.129424 0.146726 0.140306 0.140000 Uiso calc U . R 1 . .
H H20B 0.228775 0.067678 0.198516 0.140000 Uiso calc U . R 1 . .
H H20C 0.203952 0.046595 0.051980 0.140000 Uiso calc U . R 1 . .
N N2 1.2987(11) 1.0763(10) 0.4602(9) 0.048(2) Uani d . P . 0.5 A -1
C C21 1.4091(16) 1.0494(12) 0.4894(11) 0.043(3) Uani d . P . 0.5 A -1
C C22 1.5534(14) 1.0219(16) 0.5291(14) 0.052(3) Uani d . P . 0.5 A -1
H H22A 1.629102 1.104148 0.584436 0.079000 Uiso calc U P R 0.5 A -1
H H22B 1.604534 0.992448 0.456718 0.079000 Uiso calc U P R 0.5 A -1
H H22C 1.523787 0.950742 0.573001 0.079000 Uiso calc U P R 0.5 A -1


_geom_special_details            
;

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
U1 O1 . 1.757(3) ?
U1 O2 . 1.762(3) ?
U1 O5 . 2.304(3) ?
U1 O6 2_766 2.374(3) ?
U1 O3 . 2.404(3) ?
U1 O3 2_666 2.474(3) ?
U1 O4 2_666 2.506(3) ?
O3 C3 . 1.305(5) ?
O4 C3 . 1.245(5) ?
O5 C4 . 1.268(5) ?
O6 C4 . 1.251(5) ?
N1 C19 . 1.128(7) ?
C1 C3 . 1.499(6) ?
C1 C2 . 1.559(6) ?
C1 C5 . 1.567(6) ?
C1 H1 . 1.000000 ?
C2 C6 . 1.536(5) ?
C2 C4 . 1.537(5) ?
C2 H2 . 1.000000 ?
C5 C13 . 1.511(6) ?
C5 C7 . 1.518(6) ?
C5 H5 . 1.000000 ?
C6 C8 . 1.509(6) ?
C6 C18 . 1.513(6) ?
C6 H6 . 1.000000 ?
C7 C12 . 1.390(6) ?
C7 C8 . 1.411(6) ?
C8 C9 . 1.388(6) ?
C9 C10 . 1.387(6) ?
C9 H9 . 0.950000 ?
C10 C11 . 1.388(7) ?
C10 H10 . 0.950000 ?
C11 C12 . 1.398(6) ?
C11 H11 . 0.950000 ?
C12 H12 . 0.950000 ?
C13 C14 . 1.398(6) ?
C13 C18 . 1.400(6) ?
C14 C15 . 1.395(7) ?
C14 H14 . 0.950000 ?
C15 C16 . 1.387(7) ?
C15 H15 . 0.950000 ?
C16 C17 . 1.406(7) ?
C16 H16 . 0.950000 ?
C17 C18 . 1.381(6) ?
C17 H17 . 0.950000 ?
C19 C20 . 1.448(9) ?
C20 H20A . 0.980000 ?
C20 H20B . 0.980000 ?
C20 H20C . 0.980000 ?
N2 C21 . 1.145(16) ?
C21 C22 . 1.46(2) ?
C22 H22A . 0.980000 ?
C22 H22B . 0.980000 ?
C22 H22C . 0.980000 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 U1 O2 . . 179.02(15) ?
O1 U1 O5 . . 89.75(13) ?
O2 U1 O5 . . 89.69(13) ?
O1 U1 O6 . 2_766 87.39(13) ?
O2 U1 O6 . 2_766 93.38(13) ?
O5 U1 O6 . 2_766 86.03(10) ?
O1 U1 O3 . . 90.39(12) ?
O2 U1 O3 . . 88.70(12) ?
O5 U1 O3 . . 76.48(10) ?
O6 U1 O3 2_766 . 162.38(10) ?
O1 U1 O3 . 2_666 87.30(13) ?
O2 U1 O3 . 2_666 92.62(12) ?
O5 U1 O3 . 2_666 140.04(9) ?
O6 U1 O3 2_766 2_666 133.54(10) ?
O3 U1 O3 . 2_666 63.71(11) ?
O1 U1 O4 . 2_666 90.83(13) ?
O2 U1 O4 . 2_666 89.89(13) ?
O5 U1 O4 . 2_666 167.97(9) ?
O6 U1 O4 2_766 2_666 81.99(10) ?
O3 U1 O4 . 2_666 115.53(9) ?
O3 U1 O4 2_666 2_666 51.98(9) ?
C3 O3 U1 . . 148.2(3) ?
C3 O3 U1 . 2_666 95.1(2) ?
U1 O3 U1 . 2_666 116.29(11) ?
C3 O4 U1 . 2_666 95.2(3) ?
C4 O5 U1 . . 135.8(3) ?
C4 O6 U1 . 2_766 129.4(3) ?
C3 C1 C2 . . 112.4(3) ?
C3 C1 C5 . . 114.5(4) ?
C2 C1 C5 . . 108.4(3) ?
C3 C1 H1 . . 107.000000 ?
C2 C1 H1 . . 107.000000 ?
C5 C1 H1 . . 107.000000 ?
C6 C2 C4 . . 114.4(3) ?
C6 C2 C1 . . 110.7(3) ?
C4 C2 C1 . . 111.2(4) ?
C6 C2 H2 . . 106.700000 ?
C4 C2 H2 . . 106.700000 ?
C1 C2 H2 . . 106.700000 ?
O4 C3 O3 . . 117.7(4) ?
O4 C3 C1 . . 125.1(4) ?
O3 C3 C1 . . 117.2(4) ?
O6 C4 O5 . . 123.5(4) ?
O6 C4 C2 . . 118.3(4) ?
O5 C4 C2 . . 118.1(4) ?
C13 C5 C7 . . 106.6(3) ?
C13 C5 C1 . . 108.3(3) ?
C7 C5 C1 . . 105.4(3) ?
C13 C5 H5 . . 112.100000 ?
C7 C5 H5 . . 112.100000 ?
C1 C5 H5 . . 112.100000 ?
C8 C6 C18 . . 106.6(3) ?
C8 C6 C2 . . 106.8(3) ?
C18 C6 C2 . . 107.1(3) ?
C8 C6 H6 . . 112.000000 ?
C18 C6 H6 . . 112.000000 ?
C2 C6 H6 . . 112.000000 ?
C12 C7 C8 . . 120.4(4) ?
C12 C7 C5 . . 126.7(4) ?
C8 C7 C5 . . 112.9(4) ?
C9 C8 C7 . . 119.9(4) ?
C9 C8 C6 . . 126.8(4) ?
C7 C8 C6 . . 113.3(4) ?
C10 C9 C8 . . 119.7(4) ?
C10 C9 H9 . . 120.100000 ?
C8 C9 H9 . . 120.100000 ?
C9 C10 C11 . . 120.3(4) ?
C9 C10 H10 . . 119.800000 ?
C11 C10 H10 . . 119.800000 ?
C10 C11 C12 . . 120.9(4) ?
C10 C11 H11 . . 119.500000 ?
C12 C11 H11 . . 119.500000 ?
C7 C12 C11 . . 118.7(4) ?
C7 C12 H12 . . 120.700000 ?
C11 C12 H12 . . 120.700000 ?
C14 C13 C18 . . 119.8(4) ?
C14 C13 C5 . . 126.5(4) ?
C18 C13 C5 . . 113.6(4) ?
C15 C14 C13 . . 118.9(5) ?
C15 C14 H14 . . 120.500000 ?
C13 C14 H14 . . 120.500000 ?
C16 C15 C14 . . 121.3(4) ?
C16 C15 H15 . . 119.300000 ?
C14 C15 H15 . . 119.300000 ?
C15 C16 C17 . . 119.6(5) ?
C15 C16 H16 . . 120.200000 ?
C17 C16 H16 . . 120.200000 ?
C18 C17 C16 . . 119.3(5) ?
C18 C17 H17 . . 120.300000 ?
C16 C17 H17 . . 120.300000 ?
C17 C18 C13 . . 121.0(4) ?
C17 C18 C6 . . 125.8(4) ?
C13 C18 C6 . . 113.1(4) ?
N1 C19 C20 . . 178.3(7) ?
C19 C20 H20A . . 109.500000 ?
C19 C20 H20B . . 109.500000 ?
H20A C20 H20B . . 109.500000 ?
C19 C20 H20C . . 109.500000 ?
H20A C20 H20C . . 109.500000 ?
H20B C20 H20C . . 109.500000 ?
N2 C21 C22 . . 177.3(14) ?
C21 C22 H22A . . 109.500000 ?
C21 C22 H22B . . 109.500000 ?
H22A C22 H22B . . 109.500000 ?
C21 C22 H22C . . 109.500000 ?
H22A C22 H22C . . 109.500000 ?
H22B C22 H22C . . 109.500000 ?

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

data_2
_database_code_depnum_ccdc_archive 'CCDC 2290586'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2023-08-24 deposited with the CCDC.	2024-02-01 downloaded from the CCDC.
;

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H56 N2 O18 U2'
_chemical_formula_iupac          ?
_chemical_formula_weight         1545.10

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 2/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'
'-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                   15.7139(5)
_cell_length_b                   15.0080(5)
_cell_length_c                   22.3323(6)
_cell_angle_alpha                90
_cell_angle_beta                 96.4976(11)
_cell_angle_gamma                90
_cell_volume                     5232.9(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9895
_cell_measurement_theta_min      2.6091
_cell_measurement_theta_max      33.1064
_cell_measurement_temperature    100(2)

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.071
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.054
_exptl_crystal_density_diffrn    1.961
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2984

_exptl_absorpt_coefficient_mu    6.262
_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  0.67
_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            85794
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_full        28.70
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       30

_refine_special_details          
;
The H atoms bound to N1 and O9 were found and refined
with geometric restraints.
;

_reflns_number_total             6774
_reflns_number_gt                6126
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0194
_refine_ls_wR_factor_gt          0.0410
_refine_ls_wR_factor_ref         0.0431
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.058
_refine_ls_number_reflns         6774
_refine_ls_number_parameters     375
_refine_ls_number_restraints     6
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0103P)²+19.4026P] 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         0.693
_refine_diff_density_min         -0.835
_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_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 0.36407(2) 0.25591(2) 0.41521(2) 0.00744(3) Uani d . . . 1 . .
O O1 0.38828(11) 0.15200(11) 0.45175(8) 0.0131(3) Uani d . . . 1 . .
O O2 0.34024(11) 0.36026(11) 0.37992(8) 0.0136(3) Uani d . . . 1 . .
O O3 0.49220(11) 0.30772(12) 0.46663(8) 0.0135(4) Uani d . . . 1 . .
O O4 0.59889(12) 0.39565(13) 0.50291(9) 0.0202(4) Uani d . . . 1 . .
O O5 0.31562(11) 0.31753(11) 0.50196(7) 0.0101(3) Uani d . . . 1 . .
O O6 0.28221(11) 0.28503(12) 0.59415(8) 0.0128(3) Uani d . . . 1 . .
O O7 0.34626(11) 0.18738(12) 0.31565(8) 0.0132(3) Uani d . . . 1 . .
O O8 0.47950(11) 0.22005(11) 0.34864(7) 0.0107(3) Uani d . . . 1 . .
O O9 0.61850(15) 0.18085(18) 0.43808(11) 0.0367(6) Uani d . . D 1 . .
H H9A 0.587(2) 0.223(2) 0.4473(18) 0.055000 Uiso d U . D 1 . .
H H9B 0.592(2) 0.154(2) 0.4088(13) 0.055000 Uiso d U . D 1 . .
N N1 0.76029(14) 0.38993(15) 0.47694(10) 0.0157(4) Uani d . . D 1 . .
H H1A 0.7055(7) 0.378(2) 0.4813(12) 0.019000 Uiso d U . D 1 . .
H H1B 0.7927(13) 0.375(2) 0.5113(8) 0.019000 Uiso d U . D 1 . .
C C1 0.47281(15) 0.39612(16) 0.55343(10) 0.0100(4) Uani d . . . 1 . .
H H1 0.426733 0.436118 0.534122 0.012000 Uiso calc U . R 1 . .
C C2 0.42870(15) 0.31630(15) 0.58255(10) 0.0092(4) Uani d . . . 1 . .
H H2 0.458413 0.261014 0.571033 0.011000 Uiso calc U . R 1 . .
C C3 0.52643(15) 0.36540(16) 0.50472(11) 0.0114(5) Uani d . . . 1 . .
C C4 0.33544(15) 0.30634(15) 0.55817(11) 0.0092(4) Uani d . . . 1 . .
C C5 0.52652(16) 0.45026(16) 0.60424(11) 0.0122(5) Uani d . . . 1 . .
H H5 0.559227 0.499914 0.587644 0.015000 Uiso calc U . R 1 . .
C C6 0.44442(15) 0.32314(16) 0.65226(10) 0.0103(4) Uani d . . . 1 . .
H H6 0.413994 0.275257 0.672571 0.012000 Uiso calc U . R 1 . .
C C7 0.54071(16) 0.31642(17) 0.66616(11) 0.0127(5) Uani d . . . 1 . .
C C8 0.58490(16) 0.38410(17) 0.63971(11) 0.0134(5) Uani d . . . 1 . .
C C9 0.67419(17) 0.3837(2) 0.64523(12) 0.0202(6) Uani d . . . 1 . .
H H9 0.704298 0.429263 0.626931 0.024000 Uiso calc U . R 1 . .
C C10 0.71866(18) 0.3163(2) 0.67763(13) 0.0241(6) Uani d . . . 1 . .
H H10 0.779499 0.316169 0.681774 0.029000 Uiso calc U . R 1 . .
C C11 0.67527(18) 0.2490(2) 0.70408(13) 0.0232(6) Uani d . . . 1 . .
H H11 0.706523 0.203260 0.726230 0.028000 Uiso calc U . R 1 . .
C C12 0.58580(18) 0.24825(18) 0.69827(12) 0.0184(5) Uani d . . . 1 . .
H H12 0.555992 0.201850 0.715971 0.022000 Uiso calc U . R 1 . .
C C13 0.46282(16) 0.48397(17) 0.64502(11) 0.0120(5) Uani d . . . 1 . .
C C14 0.41685(16) 0.41599(15) 0.66966(10) 0.0101(4) Uani d . . . 1 . .
C C15 0.35321(16) 0.43609(17) 0.70572(11) 0.0131(5) Uani d . . . 1 . .
H H15 0.320019 0.390049 0.720795 0.016000 Uiso calc U . R 1 . .
C C16 0.33874(17) 0.52526(17) 0.71953(12) 0.0165(5) Uani d . . . 1 . .
H H16 0.296252 0.539826 0.744978 0.020000 Uiso calc U . R 1 . .
C C17 0.38577(17) 0.59258(17) 0.69646(12) 0.0171(5) Uani d . . . 1 . .
H H17 0.376044 0.652816 0.706851 0.020000 Uiso calc U . R 1 . .
C C18 0.44731(17) 0.57263(17) 0.65808(12) 0.0156(5) Uani d . . . 1 . .
H H18 0.478126 0.618948 0.641130 0.019000 Uiso calc U . R 1 . .
C C19 0.45147(14) 0.13863(15) 0.25341(10) 0.0081(4) Uani d . . . 1 . .
H H19 0.420337 0.167094 0.216799 0.010000 Uiso calc U . R 1 . .
C C20 0.42565(15) 0.18601(15) 0.30897(10) 0.0085(4) Uani d . . . 1 . .
C C21 0.41903(15) 0.03946(15) 0.25720(11) 0.0104(4) Uani d . . . 1 . .
H H21 0.356892 0.036330 0.262888 0.013000 Uiso calc U . R 1 . .
C C22 0.47519(16) -0.00219(15) 0.30912(11) 0.0114(5) Uani d . . . 1 . .
C C23 0.56209(16) -0.00469(16) 0.30075(11) 0.0123(5) Uani d . . . 1 . .
C C24 0.62188(17) -0.04153(17) 0.34444(12) 0.0161(5) Uani d . . . 1 . .
H H24 0.680550 -0.045029 0.338092 0.019000 Uiso calc U . R 1 . .
C C25 0.59435(19) -0.07338(18) 0.39791(12) 0.0203(6) Uani d . . . 1 . .
H H25 0.634463 -0.099468 0.427851 0.024000 Uiso calc U . R 1 . .
C C26 0.5089(2) -0.06711(18) 0.40745(12) 0.0214(6) Uani d . . . 1 . .
H H26 0.491258 -0.086838 0.444529 0.026000 Uiso calc U . R 1 . .
C C27 0.44874(18) -0.03207(17) 0.36303(12) 0.0168(5) Uani d . . . 1 . .
H H27 0.390117 -0.028604 0.369504 0.020000 Uiso calc U . R 1 . .
C C28 0.7694(2) 0.48642(18) 0.46471(14) 0.0244(6) Uani d . . . 1 . .
H H28A 0.830124 0.501078 0.464660 0.037000 Uiso calc U . R 1 . .
H H28B 0.745503 0.521027 0.496073 0.037000 Uiso calc U . R 1 . .
H H28C 0.738444 0.500883 0.425314 0.037000 Uiso calc U . R 1 . .
C C29 0.78094(19) 0.33207(19) 0.42666(13) 0.0214(6) Uani d . . . 1 . .
H H29A 0.747698 0.351360 0.389123 0.032000 Uiso calc U . R 1 . .
H H29B 0.766542 0.270156 0.435160 0.032000 Uiso calc U . R 1 . .
H H29C 0.842216 0.336492 0.422509 0.032000 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 . 1.7740(17) ?
U1 O1 . 1.7811(17) ?
U1 O3 . 2.3354(17) ?
U1 O5 . 2.3499(16) ?
U1 O6 7_556 2.3656(17) ?
U1 O7 . 2.4368(17) ?
U1 O8 . 2.5298(16) ?
O3 C3 . 1.288(3) ?
O4 C3 . 1.231(3) ?
O5 C4 . 1.270(3) ?
O6 C4 . 1.265(3) ?
O7 C20 . 1.273(3) ?
O8 C20 . 1.262(3) ?
O9 H9A . 0.838(10) ?
O9 H9B . 0.839(10) ?
N1 C28 . 1.483(3) ?
N1 C29 . 1.484(3) ?
N1 H1A . 0.897(9) ?
N1 H1B . 0.898(9) ?
C1 C3 . 1.521(3) ?
C1 C2 . 1.562(3) ?
C1 C5 . 1.563(3) ?
C1 H1 . 1.000000 ?
C2 C4 . 1.512(3) ?
C2 C6 . 1.552(3) ?
C2 H2 . 1.000000 ?
C5 C8 . 1.513(4) ?
C5 C13 . 1.514(3) ?
C5 H5 . 1.000000 ?
C6 C7 . 1.513(3) ?
C6 C14 . 1.523(3) ?
C6 H6 . 1.000000 ?
C7 C12 . 1.396(4) ?
C7 C8 . 1.398(4) ?
C8 C9 . 1.395(4) ?
C9 C10 . 1.386(4) ?
C9 H9 . 0.950000 ?
C10 C11 . 1.387(4) ?
C10 H10 . 0.950000 ?
C11 C12 . 1.397(4) ?
C11 H11 . 0.950000 ?
C12 H12 . 0.950000 ?
C13 C18 . 1.390(3) ?
C13 C14 . 1.398(3) ?
C14 C15 . 1.386(3) ?
C15 C16 . 1.398(4) ?
C15 H15 . 0.950000 ?
C16 C17 . 1.385(4) ?
C16 H16 . 0.950000 ?
C17 C18 . 1.395(4) ?
C17 H17 . 0.950000 ?
C18 H18 . 0.950000 ?
C19 C20 . 1.524(3) ?
C19 C19 2_655 1.550(4) ?
C19 C21 . 1.579(3) ?
C19 H19 . 1.000000 ?
C21 C22 . 1.511(3) ?
C21 C23 2_655 1.513(3) ?
C21 H21 . 1.000000 ?
C22 C27 . 1.392(3) ?
C22 C23 . 1.399(3) ?
C23 C24 . 1.390(4) ?
C24 C25 . 1.399(4) ?
C24 H24 . 0.950000 ?
C25 C26 . 1.386(4) ?
C25 H25 . 0.950000 ?
C26 C27 . 1.394(4) ?
C26 H26 . 0.950000 ?
C27 H27 . 0.950000 ?
C28 H28A . 0.980000 ?
C28 H28B . 0.980000 ?
C28 H28C . 0.980000 ?
C29 H29A . 0.980000 ?
C29 H29B . 0.980000 ?
C29 H29C . 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 . . 179.10(8) ?
O2 U1 O3 . . 92.94(7) ?
O1 U1 O3 . . 86.49(7) ?
O2 U1 O5 . . 86.96(7) ?
O1 U1 O5 . . 92.24(7) ?
O3 U1 O5 . . 78.77(6) ?
O2 U1 O6 . 7_556 92.06(7) ?
O1 U1 O6 . 7_556 88.17(7) ?
O3 U1 O6 . 7_556 154.82(6) ?
O5 U1 O6 . 7_556 76.87(6) ?
O2 U1 O7 . . 88.32(7) ?
O1 U1 O7 . . 92.58(7) ?
O3 U1 O7 . . 126.35(6) ?
O5 U1 O7 . . 154.67(6) ?
O6 U1 O7 7_556 . 78.44(6) ?
O2 U1 O8 . . 93.22(7) ?
O1 U1 O8 . . 87.29(7) ?
O3 U1 O8 . . 73.99(6) ?
O5 U1 O8 . . 152.74(6) ?
O6 U1 O8 7_556 . 130.31(6) ?
O7 U1 O8 . . 52.41(5) ?
C3 O3 U1 . . 145.18(16) ?
C4 O5 U1 . . 134.18(15) ?
C4 O6 U1 . 7_556 135.67(16) ?
C20 O7 U1 . . 95.79(14) ?
C20 O8 U1 . . 91.74(13) ?
H9A O9 H9B . . 107.2(16) ?
C28 N1 C29 . . 113.5(2) ?
C28 N1 H1A . . 109.3(19) ?
C29 N1 H1A . . 105.(2) ?
C28 N1 H1B . . 110.(2) ?
C29 N1 H1B . . 111.(2) ?
H1A N1 H1B . . 108.5(14) ?
C3 C1 C2 . . 111.91(19) ?
C3 C1 C5 . . 112.30(19) ?
C2 C1 C5 . . 108.97(19) ?
C3 C1 H1 . . 107.800000 ?
C2 C1 H1 . . 107.800000 ?
C5 C1 H1 . . 107.800000 ?
C4 C2 C6 . . 113.94(19) ?
C4 C2 C1 . . 112.56(19) ?
C6 C2 C1 . . 109.82(19) ?
C4 C2 H2 . . 106.700000 ?
C6 C2 H2 . . 106.700000 ?
C1 C2 H2 . . 106.700000 ?
O4 C3 O3 . . 123.0(2) ?
O4 C3 C1 . . 120.1(2) ?
O3 C3 C1 . . 116.9(2) ?
O6 C4 O5 . . 123.8(2) ?
O6 C4 C2 . . 118.7(2) ?
O5 C4 C2 . . 117.5(2) ?
C8 C5 C13 . . 107.9(2) ?
C8 C5 C1 . . 106.52(19) ?
C13 C5 C1 . . 105.71(19) ?
C8 C5 H5 . . 112.100000 ?
C13 C5 H5 . . 112.100000 ?
C1 C5 H5 . . 112.100000 ?
C7 C6 C14 . . 108.4(2) ?
C7 C6 C2 . . 104.08(18) ?
C14 C6 C2 . . 107.39(19) ?
C7 C6 H6 . . 112.200000 ?
C14 C6 H6 . . 112.200000 ?
C2 C6 H6 . . 112.200000 ?
C12 C7 C8 . . 120.1(2) ?
C12 C7 C6 . . 126.3(2) ?
C8 C7 C6 . . 113.4(2) ?
C9 C8 C7 . . 120.1(3) ?
C9 C8 C5 . . 126.4(2) ?
C7 C8 C5 . . 113.4(2) ?
C10 C9 C8 . . 119.5(3) ?
C10 C9 H9 . . 120.300000 ?
C8 C9 H9 . . 120.300000 ?
C9 C10 C11 . . 120.7(3) ?
C9 C10 H10 . . 119.700000 ?
C11 C10 H10 . . 119.700000 ?
C10 C11 C12 . . 120.3(3) ?
C10 C11 H11 . . 119.900000 ?
C12 C11 H11 . . 119.900000 ?
C7 C12 C11 . . 119.2(3) ?
C7 C12 H12 . . 120.400000 ?
C11 C12 H12 . . 120.400000 ?
C18 C13 C14 . . 120.4(2) ?
C18 C13 C5 . . 126.1(2) ?
C14 C13 C5 . . 113.5(2) ?
C15 C14 C13 . . 120.6(2) ?
C15 C14 C6 . . 126.3(2) ?
C13 C14 C6 . . 113.1(2) ?
C14 C15 C16 . . 118.8(2) ?
C14 C15 H15 . . 120.600000 ?
C16 C15 H15 . . 120.600000 ?
C17 C16 C15 . . 120.6(2) ?
C17 C16 H16 . . 119.700000 ?
C15 C16 H16 . . 119.700000 ?
C16 C17 C18 . . 120.5(2) ?
C16 C17 H17 . . 119.700000 ?
C18 C17 H17 . . 119.700000 ?
C13 C18 C17 . . 119.0(2) ?
C13 C18 H18 . . 120.500000 ?
C17 C18 H18 . . 120.500000 ?
C20 C19 C19 . 2_655 115.8(2) ?
C20 C19 C21 . . 106.20(17) ?
C19 C19 C21 2_655 . 109.43(12) ?
C20 C19 H19 . . 108.400000 ?
C19 C19 H19 2_655 . 108.400000 ?
C21 C19 H19 . . 108.400000 ?
O8 C20 O7 . . 119.9(2) ?
O8 C20 C19 . . 122.8(2) ?
O7 C20 C19 . . 117.2(2) ?
C22 C21 C23 . 2_655 108.74(19) ?
C22 C21 C19 . . 105.49(19) ?
C23 C21 C19 2_655 . 105.75(18) ?
C22 C21 H21 . . 112.100000 ?
C23 C21 H21 2_655 . 112.100000 ?
C19 C21 H21 . . 112.100000 ?
C27 C22 C23 . . 119.9(2) ?
C27 C22 C21 . . 126.3(2) ?
C23 C22 C21 . . 113.7(2) ?
C24 C23 C22 . . 120.6(2) ?
C24 C23 C21 . 2_655 126.3(2) ?
C22 C23 C21 . 2_655 113.0(2) ?
C23 C24 C25 . . 119.0(3) ?
C23 C24 H24 . . 120.500000 ?
C25 C24 H24 . . 120.500000 ?
C26 C25 C24 . . 120.4(3) ?
C26 C25 H25 . . 119.800000 ?
C24 C25 H25 . . 119.800000 ?
C25 C26 C27 . . 120.5(2) ?
C25 C26 H26 . . 119.800000 ?
C27 C26 H26 . . 119.800000 ?
C22 C27 C26 . . 119.5(3) ?
C22 C27 H27 . . 120.300000 ?
C26 C27 H27 . . 120.300000 ?
N1 C28 H28A . . 109.500000 ?
N1 C28 H28B . . 109.500000 ?
H28A C28 H28B . . 109.500000 ?
N1 C28 H28C . . 109.500000 ?
H28A C28 H28C . . 109.500000 ?
H28B C28 H28C . . 109.500000 ?
N1 C29 H29A . . 109.500000 ?
N1 C29 H29B . . 109.500000 ?
H29A C29 H29B . . 109.500000 ?
N1 C29 H29C . . 109.500000 ?
H29A C29 H29C . . 109.500000 ?
H29B C29 H29C . . 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
O9 H9A O3 . 0.838(10) 2.047(14) 2.874(3) 169.(4) ?
N1 H1A O4 . 0.897(9) 1.814(15) 2.666(3) 158.(3) ?
N1 H1B O9 7_656 0.898(9) 1.892(14) 2.746(3) 158.(3) ?

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

data_4
_database_code_depnum_ccdc_archive 'CCDC 2290588'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2023-08-24 deposited with the CCDC.	2024-02-01 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT972_4                   
;
PROBLEM: Check Calcd Resid. Dens.  1.86Ang From C62            -2.77 eA-3  
RESPONSE: This negative residual density is of unknown origin and, 
moreover, it does not appear on the checkcif version included in
ShelxLe.
;
# end Validation Reply Form

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C70 H52 N8 Ni O21 U2'
_chemical_formula_iupac          ?
_chemical_formula_weight         1875.96

_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                   8.6348(3)
_cell_length_b                   14.3691(5)
_cell_length_c                   27.8539(11)
_cell_angle_alpha                93.9567(17)
_cell_angle_beta                 98.1776(17)
_cell_angle_gamma                94.8470(16)
_cell_volume                     3397.1(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9421
_cell_measurement_theta_min      2.2236
_cell_measurement_theta_max      32.9401
_cell_measurement_temperature    100(2)

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent dark orange'
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.063
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1816

_exptl_absorpt_coefficient_mu    5.113
_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  0.64
_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            137913
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33

_refine_special_details          
;
The H atoms bound to O16, O20 and O21 were found and
refined with geometric restraints. 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             12911
_reflns_number_gt                12122
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0796
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_restrained_S_all      1.207
_refine_ls_number_reflns         12911
_refine_ls_number_parameters     935
_refine_ls_number_restraints     7
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0203P)²+22.2443P] 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         2.072
_refine_diff_density_min         -2.324
_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'
Ni Ni 0.3393 1.1124 '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 0.63937(2) 0.71910(2) 0.43350(2) 0.01072(5) Uani d . . . 1 . .
U U2 0.90121(2) 0.65598(2) 1.06176(2) 0.00921(5) Uani d . . . 1 . .
Ni Ni1 0.67832(7) 0.55149(4) 0.73515(2) 0.00741(12) Uani d . . . 1 . .
O O1 0.6102(4) 0.6160(3) 0.39320(13) 0.0147(8) Uani d . . . 1 . .
O O2 0.6696(5) 0.8214(3) 0.47387(14) 0.0201(8) Uani d . . . 1 . .
O O3 1.0243(5) 0.5637(3) 1.06554(14) 0.0190(8) Uani d . . . 1 . .
O O4 0.7754(5) 0.7477(3) 1.05625(14) 0.0201(8) Uani d . . . 1 . .
O O5 0.7699(4) 0.6309(3) 0.50026(13) 0.0153(8) Uani d . . . 1 . .
O O6 0.5142(4) 0.6355(3) 0.49396(14) 0.0222(9) Uani d . . . 1 . .
O O7 0.7404(4) 0.5705(3) 0.98852(13) 0.0166(8) Uani d . . . 1 . .
O O8 0.9361(5) 0.6712(3) 0.97826(13) 0.0173(8) Uani d . . . 1 . .
O O9 0.3488(4) 0.7329(3) 0.43005(14) 0.0234(9) Uani d . . . 1 . .
O O10 0.4662(4) 0.7871(3) 0.37194(14) 0.0180(8) Uani d . . . 1 . .
O O11 -0.2047(4) 0.8038(3) 0.37959(14) 0.0184(8) Uani d . . . 1 . .
O O12 -0.0700(4) 0.7275(3) 0.43346(13) 0.0162(8) Uani d . . . 1 . .
O O13 1.1266(5) 0.7644(3) 1.05510(13) 0.0185(8) Uani d . . . 1 . .
O O14 1.0650(4) 0.7556(3) 1.12852(13) 0.0172(8) Uani d . . . 1 . .
O O15 1.5959(4) 0.8727(3) 1.12214(14) 0.0204(8) Uani d . . . 1 . .
O O16 1.5705(5) 0.8838(3) 1.04160(15) 0.0258(9) Uani d . . D 1 . .
H H16 1.666(4) 0.862(5) 1.045(2) 0.031000 Uiso d U . D 1 . .
O O17 0.8492(5) 0.6196(3) 1.14480(13) 0.0212(9) Uani d . . . 1 . .
O O18 0.6848(4) 0.5492(3) 1.08479(13) 0.0189(8) Uani d . . . 1 . .
O O19 0.6743(5) 0.5103(3) 1.15884(14) 0.0215(9) Uani d . . . 1 . .
O O20 0.1708(5) 0.6813(4) 0.50537(17) 0.0336(11) Uani d . . D 1 . .
H H20A 0.257(4) 0.689(6) 0.495(2) 0.050000 Uiso d U . D 1 . .
H H20B 0.102(5) 0.700(5) 0.485(2) 0.050000 Uiso d U . D 1 . .
O O21 0.1096(5) 0.5233(3) 0.55323(14) 0.0225(9) Uani d . . D 1 . .
H H21A 0.128(8) 0.478(2) 0.5350(18) 0.034000 Uiso d U . D 1 . .
H H21B 0.123(8) 0.572(2) 0.5386(19) 0.034000 Uiso d U . D 1 . .
N N1 0.8800(5) 0.4893(3) 0.71880(14) 0.0090(8) Uani d . . . 1 . .
N N2 0.6488(5) 0.5479(3) 0.66264(14) 0.0089(8) Uani d . . . 1 . .
N N3 0.4540(5) 0.5990(3) 0.71995(15) 0.0101(8) Uani d . . . 1 . .
N N4 0.5868(5) 0.4235(3) 0.75558(14) 0.0089(8) Uani d . . . 1 . .
N N5 0.7244(5) 0.5696(3) 0.80731(15) 0.0099(8) Uani d . . . 1 . .
N N6 0.7893(5) 0.6912(3) 0.74604(15) 0.0110(8) Uani d . . . 1 . .
N N7 0.7333(5) 0.5580(3) 1.13080(16) 0.0159(9) Uani d . . . 1 . .
N N8 1.2084(8) 0.6821(5) 0.8771(3) 0.0484(17) Uani d . . . 1 . .
C C1 0.9845(6) 0.4502(3) 0.74933(18) 0.0120(10) Uani d . . . 1 . .
H H1 0.973725 0.452957 0.782854 0.014000 Uiso calc U . R 1 . .
C C2 1.1074(6) 0.4060(4) 0.73433(19) 0.0135(10) Uani d . . . 1 . .
H H2 1.178455 0.377818 0.756874 0.016000 Uiso calc U . R 1 . .
C C3 1.1246(6) 0.4039(4) 0.68519(18) 0.0123(10) Uani d . . . 1 . .
H H3 1.209380 0.375330 0.673872 0.015000 Uiso calc U . R 1 . .
C C4 1.0169(6) 0.4440(4) 0.65308(18) 0.0120(10) Uani d . . . 1 . .
H H4 1.027156 0.443474 0.619551 0.014000 Uiso calc U . R 1 . .
C C5 0.8943(6) 0.4847(3) 0.67054(18) 0.0102(10) Uani d . . . 1 . .
C C6 0.7691(6) 0.5264(3) 0.63931(18) 0.0110(10) Uani d . . . 1 . .
C C7 0.7723(6) 0.5454(4) 0.59129(19) 0.0134(10) Uani d . . . 1 . .
H H7 0.858333 0.531704 0.575062 0.016000 Uiso calc U . R 1 . .
C C8 0.6438(6) 0.5853(4) 0.56794(18) 0.0122(10) Uani d . . . 1 . .
C C9 0.5170(6) 0.6039(3) 0.59139(18) 0.0116(10) Uani d . . . 1 . .
H H9 0.426845 0.627664 0.574700 0.014000 Uiso calc U . R 1 . .
C C10 0.5263(6) 0.5864(3) 0.64016(17) 0.0096(10) Uani d . . . 1 . .
C C11 0.4106(6) 0.6118(3) 0.67227(18) 0.0108(10) Uani d . . . 1 . .
C C12 0.2693(6) 0.6451(4) 0.65540(19) 0.0156(11) Uani d . . . 1 . .
H H12 0.241355 0.654096 0.621915 0.019000 Uiso calc U . R 1 . .
C C13 0.1695(6) 0.6652(4) 0.6886(2) 0.0191(12) Uani d . . . 1 . .
H H13 0.071780 0.688492 0.677987 0.023000 Uiso calc U . R 1 . .
C C14 0.2110(6) 0.6515(4) 0.7368(2) 0.0164(11) Uani d . . . 1 . .
H H14 0.142561 0.664476 0.759712 0.020000 Uiso calc U . R 1 . .
C C15 0.3550(6) 0.6184(3) 0.75128(19) 0.0142(11) Uani d . . . 1 . .
H H15 0.384423 0.609075 0.784665 0.017000 Uiso calc U . R 1 . .
C C16 0.6425(6) 0.6171(4) 0.51734(18) 0.0149(11) Uani d . . . 1 . .
C C17 0.5206(6) 0.3497(3) 0.72511(18) 0.0113(10) Uani d . . . 1 . .
H H17 0.512147 0.354627 0.691017 0.014000 Uiso calc U . R 1 . .
C C18 0.4646(6) 0.2670(4) 0.74179(19) 0.0135(10) Uani d . . . 1 . .
H H18 0.417058 0.216092 0.719504 0.016000 Uiso calc U . R 1 . .
C C19 0.4788(6) 0.2592(4) 0.79141(19) 0.0134(10) Uani d . . . 1 . .
H H19 0.440600 0.203016 0.803696 0.016000 Uiso calc U . R 1 . .
C C20 0.5501(6) 0.3352(4) 0.82321(18) 0.0126(10) Uani d . . . 1 . .
H H20 0.562951 0.331067 0.857419 0.015000 Uiso calc U . R 1 . .
C C21 0.6012(6) 0.4159(3) 0.80413(17) 0.0096(10) Uani d . . . 1 . .
C C22 0.6759(6) 0.5025(3) 0.83405(18) 0.0094(10) Uani d . . . 1 . .
C C23 0.6983(6) 0.5150(4) 0.88459(17) 0.0115(10) Uani d . . . 1 . .
H H23 0.658831 0.468346 0.903459 0.014000 Uiso calc U . R 1 . .
C C24 0.7804(6) 0.5980(4) 0.90662(18) 0.0126(10) Uani d . . . 1 . .
C C25 0.8338(6) 0.6667(4) 0.87864(18) 0.0138(10) Uani d . . . 1 . .
H H25 0.891619 0.723036 0.893530 0.017000 Uiso calc U . R 1 . .
C C26 0.8006(6) 0.6510(3) 0.82834(18) 0.0105(10) Uani d . . . 1 . .
C C27 0.8444(6) 0.7179(3) 0.79352(18) 0.0106(10) Uani d . . . 1 . .
C C28 0.9349(6) 0.8023(3) 0.80767(19) 0.0127(10) Uani d . . . 1 . .
H H28 0.974816 0.819278 0.840981 0.015000 Uiso calc U . R 1 . .
C C29 0.9661(6) 0.8618(4) 0.77202(19) 0.0161(11) Uani d . . . 1 . .
H H29 1.028297 0.919898 0.780752 0.019000 Uiso calc U . R 1 . .
C C30 0.9058(6) 0.8357(4) 0.7239(2) 0.0159(11) Uani d . . . 1 . .
H H30 0.924127 0.875650 0.699086 0.019000 Uiso calc U . R 1 . .
C C31 0.8189(6) 0.7505(4) 0.71275(19) 0.0123(10) Uani d . . . 1 . .
H H31 0.777511 0.732627 0.679632 0.015000 Uiso calc U . R 1 . .
C C32 0.8198(6) 0.6132(4) 0.96078(18) 0.0136(10) Uani d . . . 1 . .
C C33 0.1857(6) 0.7964(4) 0.36381(18) 0.0124(10) Uani d . . . 1 . .
H H33 0.125761 0.736767 0.348231 0.015000 Uiso calc U . R 1 . .
C C34 0.0768(6) 0.8473(4) 0.39599(18) 0.0121(10) Uani d . . . 1 . .
H H34 0.139274 0.862856 0.429074 0.015000 Uiso calc U . R 1 . .
C C35 0.3417(6) 0.7720(4) 0.39069(19) 0.0143(11) Uani d . . . 1 . .
C C36 -0.0733(6) 0.7887(4) 0.40271(18) 0.0125(10) Uani d . . . 1 . .
C C37 0.2207(6) 0.8592(4) 0.32253(19) 0.0135(10) Uani d . . . 1 . .
H H37 0.291170 0.830165 0.301420 0.016000 Uiso calc U . R 1 . .
C C38 0.0399(6) 0.9427(4) 0.37470(18) 0.0134(10) Uani d . . . 1 . .
H H38 -0.030108 0.977206 0.393787 0.016000 Uiso calc U . R 1 . .
C C39 0.0651(6) 0.8757(3) 0.29370(18) 0.0115(10) Uani d . . . 1 . .
C C40 0.0145(6) 0.8496(4) 0.24500(18) 0.0135(10) Uani d . . . 1 . .
H H40 0.076513 0.813376 0.226802 0.016000 Uiso calc U . R 1 . .
C C41 -0.1279(6) 0.8765(4) 0.22253(19) 0.0155(11) Uani d . . . 1 . .
H H41 -0.163315 0.858459 0.189057 0.019000 Uiso calc U . R 1 . .
C C42 -0.2176(6) 0.9298(4) 0.2493(2) 0.0165(11) Uani d . . . 1 . .
H H42 -0.311723 0.950913 0.233612 0.020000 Uiso calc U . R 1 . .
C C43 -0.1704(6) 0.9528(4) 0.2993(2) 0.0167(11) Uani d . . . 1 . .
H H43 -0.233215 0.987877 0.317708 0.020000 Uiso calc U . R 1 . .
C C44 -0.0309(6) 0.9235(3) 0.32133(18) 0.0112(10) Uani d . . . 1 . .
C C45 0.2941(6) 0.9535(4) 0.34730(19) 0.0159(11) Uani d . . . 1 . .
C C46 0.1976(6) 0.9977(4) 0.37574(19) 0.0160(11) Uani d . . . 1 . .
C C47 0.2482(8) 1.0845(4) 0.4014(2) 0.0251(13) Uani d . . . 1 . .
H H47 0.182878 1.114441 0.421115 0.030000 Uiso calc U . R 1 . .
C C48 0.3962(9) 1.1259(5) 0.3973(2) 0.0349(16) Uani d . . . 1 . .
H H48 0.431930 1.185330 0.414040 0.042000 Uiso calc U . R 1 . .
C C49 0.4933(8) 1.0818(5) 0.3690(2) 0.0326(16) Uani d . . . 1 . .
H H49 0.594168 1.111309 0.366478 0.039000 Uiso calc U . R 1 . .
C C50 0.4434(7) 0.9951(4) 0.3445(2) 0.0245(13) Uani d . . . 1 . .
H H50 0.510752 0.964203 0.325819 0.029000 Uiso calc U . R 1 . .
C C51 1.2667(6) 0.8753(3) 1.11940(17) 0.0111(10) Uani d . . . 1 . .
H H51 1.347379 0.850882 1.143504 0.013000 Uiso calc U . R 1 . .
C C52 1.3530(6) 0.9174(3) 1.07991(18) 0.0124(10) Uani d . . . 1 . .
H H52 1.295288 0.893175 1.047153 0.015000 Uiso calc U . R 1 . .
C C53 1.1463(6) 0.7947(3) 1.09982(18) 0.0119(10) Uani d . . . 1 . .
C C54 1.5177(7) 0.8886(4) 1.08452(19) 0.0163(11) Uani d . . . 1 . .
C C55 1.1918(6) 0.9545(3) 1.14698(18) 0.0120(10) Uani d . . . 1 . .
H H55 1.128293 0.929368 1.171389 0.014000 Uiso calc U . R 1 . .
C C56 1.3543(6) 1.0274(3) 1.08522(19) 0.0129(10) Uani d . . . 1 . .
H H56 1.415673 1.058202 1.061816 0.015000 Uiso calc U . R 1 . .
C C57 1.0942(6) 1.0042(3) 1.10906(18) 0.0118(10) Uani d . . . 1 . .
C C58 1.1821(6) 1.0460(3) 1.07670(18) 0.0126(10) Uani d . . . 1 . .
C C59 1.1129(7) 1.1004(4) 1.04213(19) 0.0164(11) Uani d . . . 1 . .
H H59 1.173449 1.130245 1.020613 0.020000 Uiso calc U . R 1 . .
C C60 0.9528(7) 1.1107(4) 1.0394(2) 0.0188(12) Uani d . . . 1 . .
H H60 0.904405 1.149226 1.016445 0.023000 Uiso calc U . R 1 . .
C C61 0.8641(6) 1.0654(4) 1.0698(2) 0.0174(11) Uani d . . . 1 . .
H H61 0.754494 1.071374 1.066889 0.021000 Uiso calc U . R 1 . .
C C62 0.9337(6) 1.0112(4) 1.10454(19) 0.0136(10) Uani d . . . 1 . .
H H62 0.871999 0.979120 1.125034 0.016000 Uiso calc U . R 1 . .
C C63 1.3308(6) 1.0225(4) 1.17082(19) 0.0130(10) Uani d . . . 1 . .
C C64 1.4179(6) 1.0607(4) 1.1374(2) 0.0151(11) Uani d . . . 1 . .
C C65 1.5492(7) 1.1227(4) 1.1530(2) 0.0225(13) Uani d . . . 1 . .
H H65 1.608727 1.148570 1.130068 0.027000 Uiso calc U . R 1 . .
C C66 1.5931(7) 1.1470(4) 1.2023(2) 0.0249(13) Uani d . . . 1 . .
H H66 1.683168 1.189902 1.213156 0.030000 Uiso calc U . R 1 . .
C C67 1.5065(7) 1.1090(4) 1.2363(2) 0.0243(13) Uani d . . . 1 . .
H H67 1.537156 1.126291 1.270034 0.029000 Uiso calc U . R 1 . .
C C68 1.3745(6) 1.0455(4) 1.2202(2) 0.0181(11) Uani d . . . 1 . .
H H68 1.315596 1.018480 1.242915 0.022000 Uiso calc U . R 1 . .
C C69 1.2599(9) 0.6731(5) 0.9171(3) 0.0395(17) Uani d . . . 1 . .
C C70 1.3248(10) 0.6595(6) 0.9671(3) 0.050(2) Uani d . . . 1 . .
H H70A 1.244079 0.626614 0.982845 0.074000 Uiso calc U . R 1 . .
H H70B 1.359344 0.720560 0.985019 0.074000 Uiso calc U . R 1 . .
H H70C 1.414696 0.622136 0.967149 0.074000 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 . 1.765(4) ?
U1 O1 . 1.773(4) ?
U1 O10 . 2.425(4) ?
U1 O6 . 2.454(4) ?
U1 O11 1_655 2.470(4) ?
U1 O12 1_655 2.502(4) ?
U1 O5 . 2.510(4) ?
U1 O9 . 2.523(4) ?
U2 O3 . 1.767(4) ?
U2 O4 . 1.779(4) ?
U2 O8 . 2.410(3) ?
U2 O13 . 2.424(4) ?
U2 O14 . 2.459(3) ?
U2 O7 . 2.482(4) ?
U2 O17 . 2.500(4) ?
U2 O18 . 2.500(4) ?
Ni1 N5 . 1.987(4) ?
Ni1 N2 . 1.996(4) ?
Ni1 N4 . 2.088(4) ?
Ni1 N3 . 2.104(4) ?
Ni1 N1 . 2.115(4) ?
Ni1 N6 . 2.133(4) ?
O5 C16 . 1.265(6) ?
O6 C16 . 1.260(6) ?
O7 C32 . 1.261(6) ?
O8 C32 . 1.266(6) ?
O9 C35 . 1.262(6) ?
O10 C35 . 1.269(6) ?
O11 C36 . 1.266(6) ?
O12 C36 . 1.267(6) ?
O13 C53 . 1.274(6) ?
O14 C53 . 1.266(6) ?
O15 C54 . 1.210(7) ?
O16 C54 . 1.338(6) ?
O16 H16 . 0.899(10) ?
O17 N7 . 1.276(6) ?
O18 N7 . 1.284(6) ?
O19 N7 . 1.211(6) ?
O20 H20A . 0.838(10) ?
O20 H20B . 0.838(10) ?
O21 H21A . 0.838(10) ?
O21 H21B . 0.839(10) ?
N1 C1 . 1.336(6) ?
N1 C5 . 1.365(6) ?
N2 C10 . 1.332(6) ?
N2 C6 . 1.347(6) ?
N3 C15 . 1.338(6) ?
N3 C11 . 1.357(7) ?
N4 C17 . 1.344(6) ?
N4 C21 . 1.353(6) ?
N5 C22 . 1.335(6) ?
N5 C26 . 1.345(6) ?
N6 C31 . 1.338(6) ?
N6 C27 . 1.357(6) ?
N8 C69 . 1.159(10) ?
C1 C2 . 1.381(7) ?
C1 H1 . 0.950000 ?
C2 C3 . 1.396(7) ?
C2 H2 . 0.950000 ?
C3 C4 . 1.386(7) ?
C3 H3 . 0.950000 ?
C4 C5 . 1.383(7) ?
C4 H4 . 0.950000 ?
C5 C6 . 1.482(7) ?
C6 C7 . 1.387(7) ?
C7 C8 . 1.392(7) ?
C7 H7 . 0.950000 ?
C8 C9 . 1.388(7) ?
C8 C16 . 1.510(7) ?
C9 C10 . 1.391(7) ?
C9 H9 . 0.950000 ?
C10 C11 . 1.484(7) ?
C11 C12 . 1.381(7) ?
C12 C13 . 1.383(7) ?
C12 H12 . 0.950000 ?
C13 C14 . 1.371(8) ?
C13 H13 . 0.950000 ?
C14 C15 . 1.385(8) ?
C14 H14 . 0.950000 ?
C15 H15 . 0.950000 ?
C17 C18 . 1.381(7) ?
C17 H17 . 0.950000 ?
C18 C19 . 1.383(7) ?
C18 H18 . 0.950000 ?
C19 C20 . 1.398(7) ?
C19 H19 . 0.950000 ?
C20 C21 . 1.374(7) ?
C20 H20 . 0.950000 ?
C21 C22 . 1.492(7) ?
C22 C23 . 1.390(7) ?
C23 C24 . 1.390(7) ?
C23 H23 . 0.950000 ?
C24 C25 . 1.388(7) ?
C24 C32 . 1.495(7) ?
C25 C26 . 1.388(7) ?
C25 H25 . 0.950000 ?
C26 C27 . 1.476(7) ?
C27 C28 . 1.388(7) ?
C28 C29 . 1.394(7) ?
C28 H28 . 0.950000 ?
C29 C30 . 1.382(8) ?
C29 H29 . 0.950000 ?
C30 C31 . 1.373(7) ?
C30 H30 . 0.950000 ?
C31 H31 . 0.950000 ?
C33 C35 . 1.526(7) ?
C33 C37 . 1.557(7) ?
C33 C34 . 1.577(7) ?
C33 H33 . 1.000000 ?
C34 C36 . 1.527(7) ?
C34 C38 . 1.570(7) ?
C34 H34 . 1.000000 ?
C37 C39 . 1.510(7) ?
C37 C45 . 1.522(7) ?
C37 H37 . 1.000000 ?
C38 C46 . 1.512(7) ?
C38 C44 . 1.522(7) ?
C38 H38 . 1.000000 ?
C39 C40 . 1.380(7) ?
C39 C44 . 1.398(7) ?
C40 C41 . 1.396(7) ?
C40 H40 . 0.950000 ?
C41 C42 . 1.388(8) ?
C41 H41 . 0.950000 ?
C42 C43 . 1.401(8) ?
C42 H42 . 0.950000 ?
C43 C44 . 1.384(7) ?
C43 H43 . 0.950000 ?
C45 C50 . 1.389(8) ?
C45 C46 . 1.390(8) ?
C46 C47 . 1.398(8) ?
C47 C48 . 1.386(9) ?
C47 H47 . 0.950000 ?
C48 C49 . 1.390(10) ?
C48 H48 . 0.950000 ?
C49 C50 . 1.382(9) ?
C49 H49 . 0.950000 ?
C50 H50 . 0.950000 ?
C51 C53 . 1.506(7) ?
C51 C52 . 1.543(7) ?
C51 C55 . 1.565(7) ?
C51 H51 . 1.000000 ?
C52 C54 . 1.505(7) ?
C52 C56 . 1.576(7) ?
C52 H52 . 1.000000 ?
C55 C57 . 1.512(7) ?
C55 C63 . 1.524(7) ?
C55 H55 . 1.000000 ?
C56 C64 . 1.508(7) ?
C56 C58 . 1.521(7) ?
C56 H56 . 1.000000 ?
C57 C62 . 1.387(7) ?
C57 C58 . 1.394(7) ?
C58 C59 . 1.384(7) ?
C59 C60 . 1.395(8) ?
C59 H59 . 0.950000 ?
C60 C61 . 1.379(8) ?
C60 H60 . 0.950000 ?
C61 C62 . 1.387(8) ?
C61 H61 . 0.950000 ?
C62 H62 . 0.950000 ?
C63 C68 . 1.382(7) ?
C63 C64 . 1.391(8) ?
C64 C65 . 1.379(8) ?
C65 C66 . 1.384(9) ?
C65 H65 . 0.950000 ?
C66 C67 . 1.399(9) ?
C66 H66 . 0.950000 ?
C67 C68 . 1.398(8) ?
C67 H67 . 0.950000 ?
C68 H68 . 0.950000 ?
C69 C70 . 1.459(12) ?
C70 H70A . 0.980000 ?
C70 H70B . 0.980000 ?
C70 H70C . 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 . . 179.57(18) ?
O2 U1 O10 . . 94.24(16) ?
O1 U1 O10 . . 86.18(15) ?
O2 U1 O6 . . 89.49(17) ?
O1 U1 O6 . . 90.43(16) ?
O10 U1 O6 . . 116.65(13) ?
O2 U1 O11 . 1_655 87.94(16) ?
O1 U1 O11 . 1_655 92.10(15) ?
O10 U1 O11 . 1_655 70.00(12) ?
O6 U1 O11 . 1_655 173.05(13) ?
O2 U1 O12 . 1_655 88.61(15) ?
O1 U1 O12 . 1_655 91.08(15) ?
O10 U1 O12 . 1_655 121.80(12) ?
O6 U1 O12 . 1_655 121.50(12) ?
O11 U1 O12 1_655 1_655 51.99(12) ?
O2 U1 O5 . . 89.08(15) ?
O1 U1 O5 . . 90.53(14) ?
O10 U1 O5 . . 168.70(12) ?
O6 U1 O5 . . 52.50(12) ?
O11 U1 O5 1_655 . 120.98(12) ?
O12 U1 O5 1_655 . 69.02(11) ?
O2 U1 O9 . . 86.98(16) ?
O1 U1 O9 . . 93.36(16) ?
O10 U1 O9 . . 52.30(12) ?
O6 U1 O9 . . 64.86(12) ?
O11 U1 O9 1_655 . 121.41(12) ?
O12 U1 O9 1_655 . 172.25(13) ?
O5 U1 O9 . . 117.25(12) ?
O3 U2 O4 . . 178.42(17) ?
O3 U2 O8 . . 90.92(16) ?
O4 U2 O8 . . 87.78(16) ?
O3 U2 O13 . . 89.56(16) ?
O4 U2 O13 . . 90.78(17) ?
O8 U2 O13 . . 68.02(12) ?
O3 U2 O14 . . 94.11(16) ?
O4 U2 O14 . . 87.33(16) ?
O8 U2 O14 . . 121.08(12) ?
O13 U2 O14 . . 53.39(12) ?
O3 U2 O7 . . 89.42(16) ?
O4 U2 O7 . . 89.08(16) ?
O8 U2 O7 . . 53.26(12) ?
O13 U2 O7 . . 121.24(12) ?
O14 U2 O7 . . 173.47(12) ?
O3 U2 O17 . . 85.76(16) ?
O4 U2 O17 . . 95.44(16) ?
O8 U2 O17 . . 172.71(12) ?
O13 U2 O17 . . 118.37(12) ?
O14 U2 O17 . . 65.72(12) ?
O7 U2 O17 . . 120.12(12) ?
O3 U2 O18 . . 89.41(16) ?
O4 U2 O18 . . 90.53(17) ?
O8 U2 O18 . . 122.29(12) ?
O13 U2 O18 . . 169.66(12) ?
O14 U2 O18 . . 116.44(12) ?
O7 U2 O18 . . 69.04(12) ?
O17 U2 O18 . . 51.29(12) ?
N5 Ni1 N2 . . 172.95(17) ?
N5 Ni1 N4 . . 77.93(16) ?
N2 Ni1 N4 . . 109.01(16) ?
N5 Ni1 N3 . . 102.89(16) ?
N2 Ni1 N3 . . 78.45(16) ?
N4 Ni1 N3 . . 92.50(16) ?
N5 Ni1 N1 . . 101.03(16) ?
N2 Ni1 N1 . . 78.13(16) ?
N4 Ni1 N1 . . 89.95(16) ?
N3 Ni1 N1 . . 155.94(16) ?
N5 Ni1 N6 . . 78.41(16) ?
N2 Ni1 N6 . . 94.66(16) ?
N4 Ni1 N6 . . 156.33(16) ?
N3 Ni1 N6 . . 91.99(16) ?
N1 Ni1 N6 . . 95.31(16) ?
C16 O5 U1 . . 91.4(3) ?
C16 O6 U1 . . 94.2(3) ?
C32 O7 U2 . . 91.5(3) ?
C32 O8 U2 . . 94.7(3) ?
C35 O9 U1 . . 92.1(3) ?
C35 O10 U1 . . 96.5(3) ?
C36 O11 U1 . 1_455 94.5(3) ?
C36 O12 U1 . 1_455 93.0(3) ?
C53 O13 U2 . . 94.0(3) ?
C53 O14 U2 . . 92.6(3) ?
C54 O16 H16 . . 110.(4) ?
N7 O17 U2 . . 96.5(3) ?
N7 O18 U2 . . 96.3(3) ?
H20A O20 H20B . . 107.4(18) ?
H21A O21 H21B . . 107.1(17) ?
C1 N1 C5 . . 118.7(4) ?
C1 N1 Ni1 . . 127.5(3) ?
C5 N1 Ni1 . . 113.7(3) ?
C10 N2 C6 . . 121.3(4) ?
C10 N2 Ni1 . . 118.3(3) ?
C6 N2 Ni1 . . 118.7(3) ?
C15 N3 C11 . . 118.5(4) ?
C15 N3 Ni1 . . 127.9(4) ?
C11 N3 Ni1 . . 113.6(3) ?
C17 N4 C21 . . 118.9(4) ?
C17 N4 Ni1 . . 125.9(3) ?
C21 N4 Ni1 . . 115.2(3) ?
C22 N5 C26 . . 121.2(4) ?
C22 N5 Ni1 . . 119.8(3) ?
C26 N5 Ni1 . . 119.0(3) ?
C31 N6 C27 . . 118.3(4) ?
C31 N6 Ni1 . . 128.8(4) ?
C27 N6 Ni1 . . 112.8(3) ?
O19 N7 O17 . . 122.4(4) ?
O19 N7 O18 . . 122.3(4) ?
O17 N7 O18 . . 115.3(4) ?
N1 C1 C2 . . 122.9(5) ?
N1 C1 H1 . . 118.500000 ?
C2 C1 H1 . . 118.500000 ?
C1 C2 C3 . . 118.3(5) ?
C1 C2 H2 . . 120.900000 ?
C3 C2 H2 . . 120.900000 ?
C4 C3 C2 . . 119.4(5) ?
C4 C3 H3 . . 120.300000 ?
C2 C3 H3 . . 120.300000 ?
C5 C4 C3 . . 119.0(5) ?
C5 C4 H4 . . 120.500000 ?
C3 C4 H4 . . 120.500000 ?
N1 C5 C4 . . 121.6(5) ?
N1 C5 C6 . . 114.7(4) ?
C4 C5 C6 . . 123.7(4) ?
N2 C6 C7 . . 121.4(5) ?
N2 C6 C5 . . 113.2(4) ?
C7 C6 C5 . . 125.4(5) ?
C6 C7 C8 . . 117.0(5) ?
C6 C7 H7 . . 121.500000 ?
C8 C7 H7 . . 121.500000 ?
C9 C8 C7 . . 121.5(5) ?
C9 C8 C16 . . 117.2(5) ?
C7 C8 C16 . . 121.2(5) ?
C8 C9 C10 . . 117.7(5) ?
C8 C9 H9 . . 121.100000 ?
C10 C9 H9 . . 121.100000 ?
N2 C10 C9 . . 120.9(4) ?
N2 C10 C11 . . 114.0(4) ?
C9 C10 C11 . . 125.0(5) ?
N3 C11 C12 . . 122.2(5) ?
N3 C11 C10 . . 114.6(4) ?
C12 C11 C10 . . 123.2(5) ?
C11 C12 C13 . . 118.1(5) ?
C11 C12 H12 . . 120.900000 ?
C13 C12 H12 . . 120.900000 ?
C14 C13 C12 . . 120.3(5) ?
C14 C13 H13 . . 119.900000 ?
C12 C13 H13 . . 119.900000 ?
C13 C14 C15 . . 118.6(5) ?
C13 C14 H14 . . 120.700000 ?
C15 C14 H14 . . 120.700000 ?
N3 C15 C14 . . 122.3(5) ?
N3 C15 H15 . . 118.800000 ?
C14 C15 H15 . . 118.800000 ?
O6 C16 O5 . . 120.8(5) ?
O6 C16 C8 . . 118.8(5) ?
O5 C16 C8 . . 120.2(5) ?
N4 C17 C18 . . 122.1(5) ?
N4 C17 H17 . . 119.000000 ?
C18 C17 H17 . . 119.000000 ?
C17 C18 C19 . . 119.1(5) ?
C17 C18 H18 . . 120.500000 ?
C19 C18 H18 . . 120.500000 ?
C18 C19 C20 . . 119.0(5) ?
C18 C19 H19 . . 120.500000 ?
C20 C19 H19 . . 120.500000 ?
C21 C20 C19 . . 118.8(5) ?
C21 C20 H20 . . 120.600000 ?
C19 C20 H20 . . 120.600000 ?
N4 C21 C20 . . 122.0(4) ?
N4 C21 C22 . . 113.8(4) ?
C20 C21 C22 . . 124.1(4) ?
N5 C22 C23 . . 121.3(4) ?
N5 C22 C21 . . 113.1(4) ?
C23 C22 C21 . . 125.6(4) ?
C24 C23 C22 . . 117.8(5) ?
C24 C23 H23 . . 121.100000 ?
C22 C23 H23 . . 121.100000 ?
C25 C24 C23 . . 120.6(5) ?
C25 C24 C32 . . 118.5(5) ?
C23 C24 C32 . . 120.8(5) ?
C26 C25 C24 . . 118.3(5) ?
C26 C25 H25 . . 120.900000 ?
C24 C25 H25 . . 120.900000 ?
N5 C26 C25 . . 120.8(5) ?
N5 C26 C27 . . 114.1(4) ?
C25 C26 C27 . . 125.1(5) ?
N6 C27 C28 . . 121.7(5) ?
N6 C27 C26 . . 115.2(4) ?
C28 C27 C26 . . 123.1(5) ?
C27 C28 C29 . . 118.7(5) ?
C27 C28 H28 . . 120.700000 ?
C29 C28 H28 . . 120.700000 ?
C30 C29 C28 . . 119.4(5) ?
C30 C29 H29 . . 120.300000 ?
C28 C29 H29 . . 120.300000 ?
C31 C30 C29 . . 118.4(5) ?
C31 C30 H30 . . 120.800000 ?
C29 C30 H30 . . 120.800000 ?
N6 C31 C30 . . 123.5(5) ?
N6 C31 H31 . . 118.200000 ?
C30 C31 H31 . . 118.200000 ?
O7 C32 O8 . . 120.5(5) ?
O7 C32 C24 . . 121.7(5) ?
O8 C32 C24 . . 117.8(5) ?
C35 C33 C37 . . 108.4(4) ?
C35 C33 C34 . . 115.9(4) ?
C37 C33 C34 . . 108.9(4) ?
C35 C33 H33 . . 107.800000 ?
C37 C33 H33 . . 107.800000 ?
C34 C33 H33 . . 107.800000 ?
C36 C34 C38 . . 111.5(4) ?
C36 C34 C33 . . 115.0(4) ?
C38 C34 C33 . . 109.0(4) ?
C36 C34 H34 . . 107.000000 ?
C38 C34 H34 . . 107.000000 ?
C33 C34 H34 . . 107.000000 ?
O9 C35 O10 . . 119.1(5) ?
O9 C35 C33 . . 121.4(5) ?
O10 C35 C33 . . 119.4(5) ?
O11 C36 O12 . . 118.7(5) ?
O11 C36 C34 . . 120.5(4) ?
O12 C36 C34 . . 120.7(5) ?
C39 C37 C45 . . 107.0(4) ?
C39 C37 C33 . . 107.6(4) ?
C45 C37 C33 . . 106.6(4) ?
C39 C37 H37 . . 111.800000 ?
C45 C37 H37 . . 111.800000 ?
C33 C37 H37 . . 111.800000 ?
C46 C38 C44 . . 106.3(4) ?
C46 C38 C34 . . 105.7(4) ?
C44 C38 C34 . . 108.9(4) ?
C46 C38 H38 . . 111.900000 ?
C44 C38 H38 . . 111.900000 ?
C34 C38 H38 . . 111.900000 ?
C40 C39 C44 . . 120.1(5) ?
C40 C39 C37 . . 126.7(5) ?
C44 C39 C37 . . 113.2(4) ?
C39 C40 C41 . . 119.9(5) ?
C39 C40 H40 . . 120.100000 ?
C41 C40 H40 . . 120.100000 ?
C42 C41 C40 . . 119.7(5) ?
C42 C41 H41 . . 120.100000 ?
C40 C41 H41 . . 120.100000 ?
C41 C42 C43 . . 120.6(5) ?
C41 C42 H42 . . 119.700000 ?
C43 C42 H42 . . 119.700000 ?
C44 C43 C42 . . 119.0(5) ?
C44 C43 H43 . . 120.500000 ?
C42 C43 H43 . . 120.500000 ?
C43 C44 C39 . . 120.4(5) ?
C43 C44 C38 . . 126.4(5) ?
C39 C44 C38 . . 113.1(4) ?
C50 C45 C46 . . 120.1(5) ?
C50 C45 C37 . . 126.3(5) ?
C46 C45 C37 . . 113.6(5) ?
C45 C46 C47 . . 120.8(5) ?
C45 C46 C38 . . 113.0(5) ?
C47 C46 C38 . . 126.2(5) ?
C48 C47 C46 . . 118.3(6) ?
C48 C47 H47 . . 120.800000 ?
C46 C47 H47 . . 120.800000 ?
C47 C48 C49 . . 121.1(6) ?
C47 C48 H48 . . 119.500000 ?
C49 C48 H48 . . 119.500000 ?
C50 C49 C48 . . 120.2(6) ?
C50 C49 H49 . . 119.900000 ?
C48 C49 H49 . . 119.900000 ?
C49 C50 C45 . . 119.5(6) ?
C49 C50 H50 . . 120.200000 ?
C45 C50 H50 . . 120.200000 ?
C53 C51 C52 . . 113.3(4) ?
C53 C51 C55 . . 111.4(4) ?
C52 C51 C55 . . 109.5(4) ?
C53 C51 H51 . . 107.400000 ?
C52 C51 H51 . . 107.400000 ?
C55 C51 H51 . . 107.400000 ?
C54 C52 C51 . . 110.0(4) ?
C54 C52 C56 . . 111.0(4) ?
C51 C52 C56 . . 109.2(4) ?
C54 C52 H52 . . 108.900000 ?
C51 C52 H52 . . 108.900000 ?
C56 C52 H52 . . 108.900000 ?
O14 C53 O13 . . 119.5(4) ?
O14 C53 C51 . . 119.3(4) ?
O13 C53 C51 . . 121.2(4) ?
O15 C54 O16 . . 123.1(5) ?
O15 C54 C52 . . 125.1(5) ?
O16 C54 C52 . . 111.8(5) ?
C57 C55 C63 . . 108.2(4) ?
C57 C55 C51 . . 107.3(4) ?
C63 C55 C51 . . 104.8(4) ?
C57 C55 H55 . . 112.000000 ?
C63 C55 H55 . . 112.000000 ?
C51 C55 H55 . . 112.000000 ?
C64 C56 C58 . . 107.2(4) ?
C64 C56 C52 . . 107.8(4) ?
C58 C56 C52 . . 105.1(4) ?
C64 C56 H56 . . 112.100000 ?
C58 C56 H56 . . 112.100000 ?
C52 C56 H56 . . 112.100000 ?
C62 C57 C58 . . 120.0(5) ?
C62 C57 C55 . . 126.7(5) ?
C58 C57 C55 . . 113.3(4) ?
C59 C58 C57 . . 120.6(5) ?
C59 C58 C56 . . 126.2(5) ?
C57 C58 C56 . . 113.2(4) ?
C58 C59 C60 . . 118.8(5) ?
C58 C59 H59 . . 120.600000 ?
C60 C59 H59 . . 120.600000 ?
C61 C60 C59 . . 120.6(5) ?
C61 C60 H60 . . 119.700000 ?
C59 C60 H60 . . 119.700000 ?
C60 C61 C62 . . 120.5(5) ?
C60 C61 H61 . . 119.700000 ?
C62 C61 H61 . . 119.700000 ?
C61 C62 C57 . . 119.3(5) ?
C61 C62 H62 . . 120.300000 ?
C57 C62 H62 . . 120.300000 ?
C68 C63 C64 . . 120.7(5) ?
C68 C63 C55 . . 126.3(5) ?
C64 C63 C55 . . 113.0(5) ?
C65 C64 C63 . . 120.5(5) ?
C65 C64 C56 . . 125.9(5) ?
C63 C64 C56 . . 113.6(5) ?
C64 C65 C66 . . 119.3(6) ?
C64 C65 H65 . . 120.300000 ?
C66 C65 H65 . . 120.300000 ?
C65 C66 C67 . . 120.7(5) ?
C65 C66 H66 . . 119.600000 ?
C67 C66 H66 . . 119.600000 ?
C66 C67 C68 . . 119.6(5) ?
C66 C67 H67 . . 120.200000 ?
C68 C67 H67 . . 120.200000 ?
C63 C68 C67 . . 119.2(5) ?
C63 C68 H68 . . 120.400000 ?
C67 C68 H68 . . 120.400000 ?
N8 C69 C70 . . 178.7(8) ?
C69 C70 H70A . . 109.500000 ?
C69 C70 H70B . . 109.500000 ?
H70A C70 H70B . . 109.500000 ?
C69 C70 H70C . . 109.500000 ?
H70A C70 H70C . . 109.500000 ?
H70B C70 H70C . . 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
O16 H16 O4 1_655 0.899(10) 1.99(4) 2.758(6) 143.(6) ?
O20 H20A O6 . 0.838(10) 2.42(4) 3.146(6) 146.(6) ?
O20 H20A O9 . 0.838(10) 2.18(4) 2.872(6) 140.(6) ?
O20 H20B O12 . 0.838(10) 1.997(15) 2.830(6) 173.(8) ?
O21 H21A O5 2_666 0.838(10) 2.11(2) 2.931(5) 166.(7) ?
O21 H21B O20 . 0.839(10) 1.924(14) 2.761(6) 175.(7) ?
C4 H4 O21 1_655 0.950000 2.400000 3.254(6) 149.300000 ?
C7 H7 O21 1_655 0.950000 2.350000 3.270(6) 164.300000 ?
C15 H15 O19 2_667 0.950000 2.480000 3.239(6) 137.300000 ?
C17 H17 O1 2_666 0.950000 2.510000 3.412(6) 158.300000 ?
C51 H51 O15 . 1.000000 2.310000 2.836(6) 111.700000 ?


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

data_5
_database_code_depnum_ccdc_archive 'CCDC 2290589'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2023-08-24 deposited with the CCDC.	2024-02-01 downloaded from the CCDC.
;

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H21 N O7 U'
_chemical_formula_iupac          ?
_chemical_formula_weight         649.43

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 2/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'
'-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                   28.9120(13)
_cell_length_b                   11.9986(5)
_cell_length_c                   13.6561(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.2025(17)
_cell_angle_gamma                90
_cell_volume                     4717.8(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9773
_cell_measurement_theta_min      2.3307
_cell_measurement_theta_max      29.9596
_cell_measurement_temperature    100(2)

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.093
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.061
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2464

_exptl_absorpt_coefficient_mu    6.921
_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            63094
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_theta_min         2.33
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16

_refine_special_details          
;
;

_reflns_number_total             4484
_reflns_number_gt                4047
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0892
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_restrained_S_all      1.176
_refine_ls_number_reflns         4484
_refine_ls_number_parameters     283
_refine_ls_number_restraints     1
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0178P)²+116.5584P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         2.155
_refine_diff_density_min         -1.313
_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_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 0.72642(2) 0.32133(2) 0.81745(2) 0.01781(9) Uani d . . . 1 . .
O O1 0.75737(17) 0.4308(4) 0.8807(4) 0.0259(11) Uani d . . . 1 . .
O O2 0.69427(19) 0.2125(4) 0.7554(4) 0.0283(11) Uani d . . . 1 . .
O O3 0.70339(17) 0.4417(4) 0.6793(4) 0.0253(11) Uani d . . . 1 . .
O O4 0.65969(16) 0.4496(4) 0.8025(3) 0.0217(10) Uani d . . . 1 . .
O O5 0.68710(16) 0.7169(4) 0.4540(3) 0.0207(10) Uani d . . . 1 . .
O O6 0.72127(17) 0.6957(4) 0.6053(4) 0.0290(12) Uani d . . . 1 . .
O O7 0.78332(19) 0.3039(5) 0.7035(4) 0.0320(12) Uani d . . . 1 . .
N N1 0.8152(3) 0.3045(9) 0.5659(7) 0.061(2) Uani d U . . 1 . .
C C1 0.6471(2) 0.5884(5) 0.6754(5) 0.0193(14) Uani d . . . 1 . .
H H1 0.663178 0.654918 0.706689 0.023000 Uiso calc U . R 1 . .
C C2 0.6516(2) 0.5963(6) 0.5633(5) 0.0181(13) Uani d . . . 1 . .
H H2 0.661728 0.521152 0.542041 0.022000 Uiso calc U . R 1 . .
C C3 0.6706(2) 0.4866(6) 0.7212(5) 0.0204(14) Uani d . . . 1 . .
C C4 0.6888(2) 0.6775(5) 0.5391(5) 0.0184(13) Uani d . . . 1 . .
C C5 0.5949(2) 0.5973(6) 0.6946(5) 0.0213(14) Uani d . . . 1 . .
H H5 0.590282 0.590284 0.766027 0.026000 Uiso calc U . R 1 . .
C C6 0.6030(2) 0.6180(6) 0.5075(5) 0.0202(14) Uani d . . . 1 . .
H H6 0.604482 0.626083 0.434986 0.024000 Uiso calc U . R 1 . .
C C7 0.5740(2) 0.5173(6) 0.5337(5) 0.0197(14) Uani d . . . 1 . .
C C8 0.5702(2) 0.5054(6) 0.6337(5) 0.0209(14) Uani d . . . 1 . .
C C9 0.5482(2) 0.4133(6) 0.6701(6) 0.0268(16) Uani d . . . 1 . .
H H9 0.546230 0.404335 0.738680 0.032000 Uiso calc U . R 1 . .
C C10 0.5292(2) 0.3342(6) 0.6031(6) 0.0292(16) Uani d . . . 1 . .
H H10 0.514033 0.270728 0.626653 0.035000 Uiso calc U . R 1 . .
C C11 0.5321(3) 0.3464(6) 0.5039(6) 0.0290(16) Uani d . . . 1 . .
H H11 0.518787 0.291729 0.459527 0.035000 Uiso calc U . R 1 . .
C C12 0.5546(2) 0.4389(6) 0.4678(5) 0.0240(15) Uani d . . . 1 . .
H H12 0.556626 0.447864 0.399214 0.029000 Uiso calc U . R 1 . .
C C13 0.5786(2) 0.7089(6) 0.6532(6) 0.0234(15) Uani d . . . 1 . .
C C14 0.5836(2) 0.7207(6) 0.5535(5) 0.0220(14) Uani d . . . 1 . .
C C15 0.5733(2) 0.8210(6) 0.5068(6) 0.0282(16) Uani d . . . 1 . .
H H15 0.578174 0.830077 0.439351 0.034000 Uiso calc U . R 1 . .
C C16 0.5558(3) 0.9090(7) 0.5591(7) 0.041(2) Uani d . . . 1 . .
H H16 0.547784 0.977392 0.526922 0.049000 Uiso calc U . R 1 . .
C C17 0.5502(3) 0.8964(7) 0.6572(8) 0.044(2) Uani d . . . 1 . .
H H17 0.538170 0.956692 0.692281 0.053000 Uiso calc U . R 1 . .
C C18 0.5617(3) 0.7970(7) 0.7065(6) 0.0343(18) Uani d . . . 1 . .
H H18 0.558088 0.789451 0.774622 0.041000 Uiso calc U . R 1 . .
C C19 0.8026(3) 0.3501(9) 0.6383(7) 0.045(2) Uani d . . . 1 . .
C C20 0.8112(4) 0.4799(7) 0.6468(9) 0.059(3) Uani d . . . 1 . .
H H20A 0.844358 0.495439 0.644554 0.088000 Uiso calc U . R 1 . .
H H20B 0.801115 0.506950 0.709174 0.088000 Uiso calc U . R 1 . .
H H20C 0.793453 0.517779 0.592024 0.088000 Uiso calc U . R 1 . .
C C21 0.8388(4) 0.3594(9) 0.4848(7) 0.055(3) Uani d . . . 1 . .
H H21A 0.837261 0.440577 0.492109 0.083000 Uiso calc U . R 1 . .
H H21B 0.823130 0.337673 0.421054 0.083000 Uiso calc U . R 1 . .
H H21C 0.871349 0.335858 0.488571 0.083000 Uiso calc U . R 1 . .
C C22 0.8061(5) 0.1838(8) 0.5529(8) 0.069(4) Uani d U . . 1 . .
H H22A 0.783776 0.159610 0.598546 0.103000 Uiso calc U . R 1 . .
H H22B 0.835170 0.142365 0.566443 0.103000 Uiso calc U . R 1 . .
H H22C 0.793245 0.169359 0.485206 0.103000 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 . 1.769(5) ?
U1 O2 . 1.773(5) ?
U1 O5 6_566 2.316(5) ?
U1 O6 4_646 2.320(5) ?
U1 O7 . 2.374(5) ?
U1 O3 . 2.421(5) ?
U1 O4 . 2.462(5) ?
O3 C3 . 1.271(8) ?
O4 C3 . 1.262(8) ?
O5 C4 . 1.252(8) ?
O6 C4 . 1.261(8) ?
O7 C19 . 1.225(10) ?
N1 C19 . 1.215(13) ?
N1 C22 . 1.480(13) ?
N1 C21 . 1.504(12) ?
C1 C3 . 1.506(9) ?
C1 C2 . 1.552(9) ?
C1 C5 . 1.557(9) ?
C1 H1 . 1.000000 ?
C2 C4 . 1.510(9) ?
C2 C6 . 1.558(9) ?
C2 H2 . 1.000000 ?
C5 C13 . 1.512(9) ?
C5 C8 . 1.520(10) ?
C5 H5 . 1.000000 ?
C6 C14 . 1.513(10) ?
C6 C7 . 1.531(9) ?
C6 H6 . 1.000000 ?
C7 C12 . 1.384(10) ?
C7 C8 . 1.387(10) ?
C8 C9 . 1.389(10) ?
C9 C10 . 1.395(11) ?
C9 H9 . 0.950000 ?
C10 C11 . 1.373(11) ?
C10 H10 . 0.950000 ?
C11 C12 . 1.399(10) ?
C11 H11 . 0.950000 ?
C12 H12 . 0.950000 ?
C13 C14 . 1.390(10) ?
C13 C18 . 1.397(10) ?
C14 C15 . 1.382(10) ?
C15 C16 . 1.395(12) ?
C15 H15 . 0.950000 ?
C16 C17 . 1.372(14) ?
C16 H16 . 0.950000 ?
C17 C18 . 1.395(12) ?
C17 H17 . 0.950000 ?
C18 H18 . 0.950000 ?
C19 C20 . 1.579(13) ?
C20 H20A . 0.980000 ?
C20 H20B . 0.980000 ?
C20 H20C . 0.980000 ?
C21 H21A . 0.980000 ?
C21 H21B . 0.980000 ?
C21 H21C . 0.980000 ?
C22 H22A . 0.980000 ?
C22 H22B . 0.980000 ?
C22 H22C . 0.980000 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 U1 O2 . . 178.7(2) ?
O1 U1 O5 . 6_566 91.0(2) ?
O2 U1 O5 . 6_566 88.0(2) ?
O1 U1 O6 . 4_646 88.9(2) ?
O2 U1 O6 . 4_646 91.8(2) ?
O5 U1 O6 6_566 4_646 81.52(17) ?
O1 U1 O7 . . 92.1(2) ?
O2 U1 O7 . . 89.2(2) ?
O5 U1 O7 6_566 . 158.47(17) ?
O6 U1 O7 4_646 . 77.24(18) ?
O1 U1 O3 . . 91.6(2) ?
O2 U1 O3 . . 88.4(2) ?
O5 U1 O3 6_566 . 128.69(16) ?
O6 U1 O3 4_646 . 149.76(17) ?
O7 U1 O3 . . 72.52(17) ?
O1 U1 O4 . . 86.2(2) ?
O2 U1 O4 . . 92.8(2) ?
O5 U1 O4 6_566 . 75.65(15) ?
O6 U1 O4 4_646 . 156.53(17) ?
O7 U1 O4 . . 125.82(16) ?
O3 U1 O4 . . 53.45(15) ?
C3 O3 U1 . . 93.8(4) ?
C3 O4 U1 . . 92.1(4) ?
C4 O5 U1 . 6_565 133.8(4) ?
C4 O6 U1 . 4_656 148.3(5) ?
C19 O7 U1 . . 145.5(6) ?
C19 N1 C22 . . 118.4(10) ?
C19 N1 C21 . . 126.2(10) ?
C22 N1 C21 . . 115.4(9) ?
C3 C1 C2 . . 112.6(5) ?
C3 C1 C5 . . 113.2(5) ?
C2 C1 C5 . . 109.3(5) ?
C3 C1 H1 . . 107.100000 ?
C2 C1 H1 . . 107.100000 ?
C5 C1 H1 . . 107.100000 ?
C4 C2 C1 . . 112.3(5) ?
C4 C2 C6 . . 114.5(5) ?
C1 C2 C6 . . 109.9(5) ?
C4 C2 H2 . . 106.500000 ?
C1 C2 H2 . . 106.500000 ?
C6 C2 H2 . . 106.500000 ?
O4 C3 O3 . . 120.2(6) ?
O4 C3 C1 . . 120.7(6) ?
O3 C3 C1 . . 119.0(6) ?
O5 C4 O6 . . 124.3(6) ?
O5 C4 C2 . . 118.5(6) ?
O6 C4 C2 . . 117.0(6) ?
C13 C5 C8 . . 108.8(6) ?
C13 C5 C1 . . 105.8(5) ?
C8 C5 C1 . . 105.8(5) ?
C13 C5 H5 . . 112.000000 ?
C8 C5 H5 . . 112.000000 ?
C1 C5 H5 . . 112.000000 ?
C14 C6 C7 . . 108.3(5) ?
C14 C6 C2 . . 106.5(5) ?
C7 C6 C2 . . 104.1(5) ?
C14 C6 H6 . . 112.500000 ?
C7 C6 H6 . . 112.500000 ?
C2 C6 H6 . . 112.500000 ?
C12 C7 C8 . . 120.5(6) ?
C12 C7 C6 . . 125.5(6) ?
C8 C7 C6 . . 113.9(6) ?
C7 C8 C9 . . 120.9(7) ?
C7 C8 C5 . . 112.9(6) ?
C9 C8 C5 . . 126.1(6) ?
C8 C9 C10 . . 118.2(7) ?
C8 C9 H9 . . 120.900000 ?
C10 C9 H9 . . 120.900000 ?
C11 C10 C9 . . 121.3(7) ?
C11 C10 H10 . . 119.400000 ?
C9 C10 H10 . . 119.400000 ?
C10 C11 C12 . . 120.2(7) ?
C10 C11 H11 . . 119.900000 ?
C12 C11 H11 . . 119.900000 ?
C7 C12 C11 . . 118.9(7) ?
C7 C12 H12 . . 120.500000 ?
C11 C12 H12 . . 120.500000 ?
C14 C13 C18 . . 120.4(7) ?
C14 C13 C5 . . 113.5(6) ?
C18 C13 C5 . . 126.0(7) ?
C15 C14 C13 . . 120.2(7) ?
C15 C14 C6 . . 126.2(7) ?
C13 C14 C6 . . 113.5(6) ?
C14 C15 C16 . . 119.7(8) ?
C14 C15 H15 . . 120.200000 ?
C16 C15 H15 . . 120.200000 ?
C17 C16 C15 . . 119.9(8) ?
C17 C16 H16 . . 120.100000 ?
C15 C16 H16 . . 120.100000 ?
C16 C17 C18 . . 121.4(8) ?
C16 C17 H17 . . 119.300000 ?
C18 C17 H17 . . 119.300000 ?
C17 C18 C13 . . 118.4(8) ?
C17 C18 H18 . . 120.800000 ?
C13 C18 H18 . . 120.800000 ?
N1 C19 O7 . . 125.2(11) ?
N1 C19 C20 . . 116.6(9) ?
O7 C19 C20 . . 118.2(9) ?
C19 C20 H20A . . 109.500000 ?
C19 C20 H20B . . 109.500000 ?
H20A C20 H20B . . 109.500000 ?
C19 C20 H20C . . 109.500000 ?
H20A C20 H20C . . 109.500000 ?
H20B C20 H20C . . 109.500000 ?
N1 C21 H21A . . 109.500000 ?
N1 C21 H21B . . 109.500000 ?
H21A C21 H21B . . 109.500000 ?
N1 C21 H21C . . 109.500000 ?
H21A C21 H21C . . 109.500000 ?
H21B C21 H21C . . 109.500000 ?
N1 C22 H22A . . 109.500000 ?
N1 C22 H22B . . 109.500000 ?
H22A C22 H22B . . 109.500000 ?
N1 C22 H22C . . 109.500000 ?
H22A C22 H22C . . 109.500000 ?
H22B C22 H22C . . 109.500000 ?

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

data_6
_database_code_depnum_ccdc_archive 'CCDC 2290590'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2023-08-24 deposited with the CCDC.	2024-02-01 downloaded from the CCDC.
;

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H12 O6 U'
_chemical_formula_iupac          ?
_chemical_formula_weight         562.31

_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                   8.4166(3)
_cell_length_b                   21.8953(7)
_cell_length_c                   8.4203(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.6517(12)
_cell_angle_gamma                90
_cell_volume                     1548.58(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9010
_cell_measurement_theta_min      2.4237
_cell_measurement_theta_max      36.8979
_cell_measurement_temperature    100(2)

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.048
_exptl_crystal_density_diffrn    2.412
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1040

_exptl_absorpt_coefficient_mu    10.515
_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  0.58
_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            19826
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_theta_min         2.42
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_full        28.70
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11

_refine_special_details          
;
;

_reflns_number_total             3990
_reflns_number_gt                3814
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0164
_refine_ls_wR_factor_gt          0.0385
_refine_ls_wR_factor_ref         0.0390
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.119
_refine_ls_number_reflns         3990
_refine_ls_number_parameters     226
_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)+1.8844P] 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         1.284
_refine_diff_density_min         -1.070
_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'
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 0.22359(2) 0.74198(2) 0.15999(2) 0.00557(4) Uani d . . . 1 . .
O O1 0.2399(2) 0.82015(8) 0.2097(2) 0.0093(3) Uani d . . . 1 . .
O O2 0.2076(2) 0.66399(8) 0.1117(2) 0.0111(3) Uani d . . . 1 . .
O O3 0.3762(2) 0.73269(8) 0.4295(2) 0.0090(3) Uani d . . . 1 . .
O O4 0.5114(2) 0.71937(8) 0.2198(2) 0.0092(3) Uani d . . . 1 . .
O O5 1.0738(2) 0.72260(8) 0.3982(2) 0.0094(3) Uani d . . . 1 . .
O O6 0.9379(2) 0.74300(8) 0.6027(2) 0.0099(3) Uani d . . . 1 . .
C C1 0.6478(3) 0.69992(11) 0.4791(3) 0.0071(4) Uani d . . . 1 . .
H H1 0.673031 0.734106 0.555327 0.008000 Uiso calc U . R 1 . .
C C2 0.8013(3) 0.68318(10) 0.3962(3) 0.0058(4) Uani d . . . 1 . .
H H2 0.786112 0.691713 0.279594 0.007000 Uiso calc U . R 1 . .
C C3 0.5082(3) 0.71881(10) 0.3684(3) 0.0067(4) Uani d . . . 1 . .
C C4 0.9420(3) 0.71943(11) 0.4677(3) 0.0073(4) Uani d . . . 1 . .
C C5 0.5918(3) 0.64314(11) 0.5760(3) 0.0077(4) Uani d . . . 1 . .
H H5 0.496496 0.652796 0.636531 0.009000 Uiso calc U . R 1 . .
C C6 0.8387(3) 0.61234(11) 0.4245(3) 0.0090(4) Uani d . . . 1 . .
H H6 0.933285 0.598627 0.367829 0.011000 Uiso calc U . R 1 . .
C C7 0.5563(3) 0.59433(11) 0.4515(3) 0.0092(4) Uani d . . . 1 . .
C C8 0.6890(3) 0.57827(11) 0.3684(3) 0.0096(4) Uani d . . . 1 . .
C C9 0.6746(3) 0.53406(11) 0.2496(3) 0.0138(5) Uani d . . . 1 . .
H H9 0.764718 0.522058 0.194712 0.017000 Uiso calc U . R 1 . .
C C10 0.5256(4) 0.50752(12) 0.2120(3) 0.0183(6) Uani d . . . 1 . .
H H10 0.515109 0.476755 0.132432 0.022000 Uiso calc U . R 1 . .
C C11 0.3935(3) 0.52572(12) 0.2896(3) 0.0178(6) Uani d . . . 1 . .
H H11 0.292471 0.508258 0.260685 0.021000 Uiso calc U . R 1 . .
C C12 0.4076(3) 0.56949(11) 0.4100(3) 0.0131(5) Uani d . . . 1 . .
H H12 0.316784 0.582126 0.462926 0.016000 Uiso calc U . R 1 . .
C C13 0.7318(3) 0.62322(11) 0.6846(3) 0.0076(4) Uani d . . . 1 . .
C C14 0.8628(3) 0.60368(10) 0.6030(3) 0.0077(4) Uani d . . . 1 . .
C C15 0.9978(3) 0.58147(11) 0.6861(3) 0.0119(5) Uani d . . . 1 . .
H H15 1.084640 0.566408 0.630910 0.014000 Uiso calc U . R 1 . .
C C16 1.0046(3) 0.58153(12) 0.8519(3) 0.0145(5) Uani d . . . 1 . .
H H16 1.096797 0.566324 0.909846 0.017000 Uiso calc U . R 1 . .
C C17 0.8782(3) 0.60355(12) 0.9335(3) 0.0141(5) Uani d . . . 1 . .
H H17 0.886231 0.604895 1.046462 0.017000 Uiso calc U . R 1 . .
C C18 0.7388(3) 0.62382(11) 0.8495(3) 0.0115(5) Uani d . . . 1 . .
H H18 0.650744 0.637713 0.904748 0.014000 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 . 1.7586(17) ?
U1 O1 . 1.7652(17) ?
U1 O6 4_475 2.4440(19) ?
U1 O3 4_575 2.4582(17) ?
U1 O5 1_455 2.4727(17) ?
U1 O4 . 2.4921(17) ?
U1 O3 . 2.5432(18) ?
U1 O5 4_475 2.5874(17) ?
O3 C3 . 1.290(3) ?
O4 C3 . 1.253(3) ?
O5 C4 . 1.288(3) ?
O6 C4 . 1.252(3) ?
C1 C3 . 1.510(3) ?
C1 C2 . 1.551(3) ?
C1 C5 . 1.576(3) ?
C1 H1 . 1.000000 ?
C2 C4 . 1.518(3) ?
C2 C6 . 1.598(3) ?
C2 H2 . 1.000000 ?
C5 C13 . 1.509(3) ?
C5 C7 . 1.514(3) ?
C5 H5 . 1.000000 ?
C6 C8 . 1.514(3) ?
C6 C14 . 1.516(3) ?
C6 H6 . 1.000000 ?
C7 C12 . 1.389(3) ?
C7 C8 . 1.399(3) ?
C8 C9 . 1.392(3) ?
C9 C10 . 1.400(4) ?
C9 H9 . 0.950000 ?
C10 C11 . 1.384(4) ?
C10 H10 . 0.950000 ?
C11 C12 . 1.395(4) ?
C11 H11 . 0.950000 ?
C12 H12 . 0.950000 ?
C13 C18 . 1.386(3) ?
C13 C14 . 1.402(3) ?
C14 C15 . 1.385(3) ?
C15 C16 . 1.393(4) ?
C15 H15 . 0.950000 ?
C16 C17 . 1.389(4) ?
C16 H16 . 0.950000 ?
C17 C18 . 1.403(4) ?
C17 H17 . 0.950000 ?
C18 H18 . 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 . . 179.65(8) ?
O2 U1 O6 . 4_475 91.44(7) ?
O1 U1 O6 . 4_475 88.67(7) ?
O2 U1 O3 . 4_575 94.16(7) ?
O1 U1 O3 . 4_575 86.10(7) ?
O6 U1 O3 4_475 4_575 111.76(6) ?
O2 U1 O5 . 1_455 89.16(7) ?
O1 U1 O5 . 1_455 90.57(7) ?
O6 U1 O5 4_475 1_455 68.73(6) ?
O3 U1 O5 4_575 1_455 176.61(5) ?
O2 U1 O4 . . 85.00(7) ?
O1 U1 O4 . . 94.87(7) ?
O6 U1 O4 4_475 . 176.25(5) ?
O3 U1 O4 4_575 . 69.77(6) ?
O5 U1 O4 1_455 . 109.95(5) ?
O2 U1 O3 . . 98.94(7) ?
O1 U1 O3 . . 80.73(7) ?
O6 U1 O3 4_475 . 128.41(6) ?
O3 U1 O3 4_575 . 117.58(7) ?
O5 U1 O3 1_455 . 61.12(6) ?
O4 U1 O3 . . 51.30(5) ?
O2 U1 O5 . 4_475 93.90(7) ?
O1 U1 O5 . 4_475 86.43(7) ?
O6 U1 O5 4_475 4_475 51.09(6) ?
O3 U1 O5 4_575 4_475 60.68(6) ?
O5 U1 O5 1_455 4_475 119.78(7) ?
O4 U1 O5 . 4_475 130.25(5) ?
O3 U1 O5 . 4_475 167.15(5) ?
C3 O3 U1 . 4_576 150.99(15) ?
C3 O3 U1 . . 93.55(14) ?
U1 O3 U1 4_576 . 115.27(7) ?
C3 O4 U1 . . 96.96(14) ?
C4 O5 U1 . 1_655 151.10(15) ?
C4 O5 U1 . 4_676 90.94(13) ?
U1 O5 U1 1_655 4_676 113.19(6) ?
C4 O6 U1 . 4_676 98.70(14) ?
C3 C1 C2 . . 115.13(18) ?
C3 C1 C5 . . 106.82(18) ?
C2 C1 C5 . . 109.37(18) ?
C3 C1 H1 . . 108.400000 ?
C2 C1 H1 . . 108.400000 ?
C5 C1 H1 . . 108.400000 ?
C4 C2 C1 . . 110.47(18) ?
C4 C2 C6 . . 107.91(18) ?
C1 C2 C6 . . 108.92(18) ?
C4 C2 H2 . . 109.800000 ?
C1 C2 H2 . . 109.800000 ?
C6 C2 H2 . . 109.800000 ?
O4 C3 O3 . . 118.0(2) ?
O4 C3 C1 . . 123.6(2) ?
O3 C3 C1 . . 118.3(2) ?
O6 C4 O5 . . 117.7(2) ?
O6 C4 C2 . . 120.7(2) ?
O5 C4 C2 . . 121.4(2) ?
C13 C5 C7 . . 109.14(19) ?
C13 C5 C1 . . 107.11(18) ?
C7 C5 C1 . . 104.51(18) ?
C13 C5 H5 . . 111.900000 ?
C7 C5 H5 . . 111.900000 ?
C1 C5 H5 . . 111.900000 ?
C8 C6 C14 . . 107.67(19) ?
C8 C6 C2 . . 106.25(19) ?
C14 C6 C2 . . 106.36(18) ?
C8 C6 H6 . . 112.100000 ?
C14 C6 H6 . . 112.100000 ?
C2 C6 H6 . . 112.100000 ?
C12 C7 C8 . . 120.7(2) ?
C12 C7 C5 . . 125.8(2) ?
C8 C7 C5 . . 113.3(2) ?
C9 C8 C7 . . 119.9(2) ?
C9 C8 C6 . . 126.8(2) ?
C7 C8 C6 . . 113.3(2) ?
C8 C9 C10 . . 119.1(2) ?
C8 C9 H9 . . 120.400000 ?
C10 C9 H9 . . 120.400000 ?
C11 C10 C9 . . 120.6(2) ?
C11 C10 H10 . . 119.700000 ?
C9 C10 H10 . . 119.700000 ?
C10 C11 C12 . . 120.5(2) ?
C10 C11 H11 . . 119.700000 ?
C12 C11 H11 . . 119.700000 ?
C7 C12 C11 . . 119.0(2) ?
C7 C12 H12 . . 120.500000 ?
C11 C12 H12 . . 120.500000 ?
C18 C13 C14 . . 120.6(2) ?
C18 C13 C5 . . 125.9(2) ?
C14 C13 C5 . . 113.5(2) ?
C15 C14 C13 . . 120.3(2) ?
C15 C14 C6 . . 126.8(2) ?
C13 C14 C6 . . 112.8(2) ?
C14 C15 C16 . . 119.1(2) ?
C14 C15 H15 . . 120.500000 ?
C16 C15 H15 . . 120.500000 ?
C17 C16 C15 . . 120.8(2) ?
C17 C16 H16 . . 119.600000 ?
C15 C16 H16 . . 119.600000 ?
C16 C17 C18 . . 120.2(2) ?
C16 C17 H17 . . 119.900000 ?
C18 C17 H17 . . 119.900000 ?
C13 C18 C17 . . 118.9(2) ?
C13 C18 H18 . . 120.600000 ?
C17 C18 H18 . . 120.600000 ?

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
C1 H1 O4 4_576 1.00 2.25 2.974(3) 128.5 ?
C1 H1 O6 . 1.00 2.25 2.759(3) 110.3 ?
C2 H2 O6 4_575 1.00 2.48 3.226(3) 131.3 ?

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

data_7
_database_code_depnum_ccdc_archive 'CCDC 2290591'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2023-08-24 deposited with the CCDC.	2024-02-01 downloaded from the CCDC.
;

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C102 H76 O16 P2 U2'
_chemical_formula_iupac          ?
_chemical_formula_weight         2095.62
_chemical_absolute_configuration ad

_chemical_melting_point          ?

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

_cell_length_a                   23.3097(6)
_cell_length_b                   13.3655(3)
_cell_length_c                   13.5379(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4217.68(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9234
_cell_measurement_theta_min      2.3058
_cell_measurement_theta_max      32.6494
_cell_measurement_temperature    100(2)

_exptl_crystal_description       lath
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.054
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2060

_exptl_absorpt_coefficient_mu    3.943
_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            96094
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_full        28.70
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18

_refine_special_details          
;
;

_reflns_number_total             10917
_reflns_number_gt                10575
_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           0.0190
_refine_ls_wR_factor_gt          0.0400
_refine_ls_wR_factor_ref         0.0408
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.057
_refine_ls_number_reflns         10917
_refine_ls_number_parameters     551
_refine_ls_number_restraints     42
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0129P)²+3.1237P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_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         0.435
_refine_diff_density_min         -0.471
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
Known absolute configuration, confirmed by Flack parameter.
;
_refine_ls_abs_structure_Flack   -0.012(4)

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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    ?
_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 0.66221(2) 0.39857(2) 0.84939(2) 0.01182(3) Uani d . . . 1 . .
P P1 0.67566(4) 0.91893(6) 0.71171(7) 0.01659(19) Uani d . . . 1 . .
O O1 0.61867(11) 0.44434(18) 0.94714(19) 0.0178(5) Uani d . . . 1 . .
O O2 0.70487(11) 0.35302(19) 0.74996(19) 0.0198(5) Uani d . . . 1 . .
O O3 0.70500(11) 0.56378(18) 0.81872(19) 0.0185(5) Uani d . . . 1 . .
O O4 0.74751(10) 0.47250(18) 0.93169(19) 0.0168(5) Uani d . . . 1 . .
O O5 0.79182(11) 0.78379(18) 1.03120(19) 0.0190(5) Uani d . . . 1 . .
O O6 0.86478(11) 0.72288(19) 1.11359(19) 0.0192(5) Uani d . . . 1 . .
O O7 0.57411(11) 0.34442(18) 0.7640(2) 0.0200(6) Uani d . . . 1 . .
O O8 0.60150(11) 0.4988(2) 0.7368(2) 0.0212(6) Uani d . . . 1 . .
C C1 0.79144(15) 0.6316(2) 0.8871(3) 0.0144(7) Uani d . . . 1 . .
H H1 0.772064 0.698313 0.888750 0.017000 Uiso calc U . R 1 . .
C C2 0.83005(14) 0.6223(2) 0.9797(2) 0.0147(7) Uani d . . . 1 . .
H H2 0.817043 0.563237 1.019157 0.018000 Uiso calc U . R 1 . .
C C3 0.74551(15) 0.5510(2) 0.8802(3) 0.0146(7) Uani d . . . 1 . .
C C4 0.82806(14) 0.7147(2) 1.0453(3) 0.0144(7) Uani d . . . 1 . .
C C5 0.82974(15) 0.6264(2) 0.7920(3) 0.0181(7) Uani d . . . 1 . .
H H5 0.806638 0.634479 0.730241 0.022000 Uiso calc U . R 1 . .
C C6 0.89385(13) 0.6048(3) 0.9471(3) 0.0173(6) Uani d . . . 1 . .
H H6 0.920039 0.596051 1.004999 0.021000 Uiso calc U . R 1 . .
C C7 0.87608(16) 0.7060(3) 0.8010(3) 0.0208(8) Uani d . . . 1 . .
C C8 0.90968(15) 0.6955(3) 0.8854(3) 0.0190(7) Uani d . . . 1 . .
C C9 0.95210(17) 0.7653(3) 0.9075(4) 0.0252(9) Uani d . . . 1 . .
H H9 0.972980 0.761285 0.967662 0.030000 Uiso calc U . R 1 . .
C C10 0.96332(16) 0.8414(3) 0.8394(4) 0.0314(10) Uani d . . . 1 . .
H H10 0.992661 0.888815 0.852819 0.038000 Uiso calc U . R 1 . .
C C11 0.93224(18) 0.8485(3) 0.7527(4) 0.0326(10) Uani d . . . 1 . .
H H11 0.941193 0.899111 0.705873 0.039000 Uiso calc U . R 1 . .
C C12 0.88746(17) 0.7810(3) 0.7340(3) 0.0270(9) Uani d . . . 1 . .
H H12 0.865169 0.786905 0.675526 0.032000 Uiso calc U . R 1 . .
C C13 0.86027(17) 0.5263(3) 0.7955(3) 0.0220(8) Uani d . . . 1 . .
C C14 0.89535(16) 0.5155(3) 0.8784(3) 0.0206(8) Uani d . . . 1 . .
C C15 0.92843(19) 0.4301(3) 0.8895(4) 0.0313(10) Uani d . . . 1 . .
H H15 0.952852 0.422565 0.945159 0.038000 Uiso calc U . R 1 . .
C C16 0.9254(2) 0.3559(3) 0.8181(4) 0.0438(14) Uani d . . . 1 . .
H H16 0.948234 0.297403 0.824657 0.053000 Uiso calc U . R 1 . .
C C17 0.8896(2) 0.3659(4) 0.7379(4) 0.0432(13) Uani d . . . 1 . .
H H17 0.887816 0.314081 0.689995 0.052000 Uiso calc U . R 1 . .
C C18 0.85605(19) 0.4509(3) 0.7261(3) 0.0327(10) Uani d . . . 1 . .
H H18 0.830717 0.457119 0.671499 0.039000 Uiso calc U . R 1 . .
C C19 0.51015(14) 0.4453(2) 0.6681(2) 0.0148(7) Uani d . . . 1 . .
H H19 0.479327 0.402936 0.697952 0.018000 Uiso calc U . R 1 . .
C C20 0.56518(15) 0.4296(3) 0.7266(3) 0.0148(7) Uani d . . . 1 . .
C C21 0.52013(14) 0.4100(3) 0.5588(3) 0.0201(7) Uani d . . . 1 . .
H H21 0.535600 0.340334 0.555655 0.024000 Uiso calc U . R 1 . .
C C22 0.46199(16) 0.4185(3) 0.5090(3) 0.0264(8) Uani d U . . 1 . .
C C23 0.44039(16) 0.5162(3) 0.5101(3) 0.0235(8) Uani d U . . 1 . .
C C24 0.38745(17) 0.5371(4) 0.4686(3) 0.0304(9) Uani d U . . 1 . .
H H24 0.372338 0.603058 0.470697 0.037000 Uiso calc U . R 1 . .
C C25 0.35692(19) 0.4611(4) 0.4241(3) 0.0385(10) Uani d U . . 1 . .
H H25 0.321189 0.475608 0.393537 0.046000 Uiso calc U . R 1 . .
C C26 0.3776(2) 0.3638(4) 0.4234(4) 0.0428(10) Uani d U . . 1 . .
H H26 0.355748 0.311960 0.393596 0.051000 Uiso calc U . R 1 . .
C C27 0.43069(19) 0.3421(4) 0.4665(4) 0.0396(10) Uani d U . . 1 . .
H H27 0.445031 0.275539 0.466560 0.048000 Uiso calc U . R 1 . .
C C28 0.70677(15) 0.8271(3) 0.6305(3) 0.0182(7) Uani d . . . 1 . .
C C29 0.70097(17) 0.7248(3) 0.6505(3) 0.0243(7) Uani d . . . 1 . .
H H29 0.678393 0.702857 0.704754 0.029000 Uiso calc U . R 1 . .
C C30 0.7286(2) 0.6557(3) 0.5902(3) 0.0320(10) Uani d . . . 1 . .
H H30 0.725850 0.586317 0.604606 0.038000 Uiso calc U . R 1 . .
C C31 0.7598(2) 0.6872(3) 0.5099(3) 0.0342(10) Uani d . . . 1 . .
H H31 0.777973 0.639185 0.468680 0.041000 Uiso calc U . R 1 . .
C C32 0.76528(18) 0.7887(3) 0.4883(3) 0.0284(9) Uani d . . . 1 . .
H H32 0.786867 0.809814 0.432508 0.034000 Uiso calc U . R 1 . .
C C33 0.73885(16) 0.8587(3) 0.5489(3) 0.0220(8) Uani d . . . 1 . .
H H33 0.742569 0.928068 0.535027 0.026000 Uiso calc U . R 1 . .
C C34 0.64032(16) 0.8537(3) 0.8101(3) 0.0181(7) Uani d . . . 1 . .
C C35 0.66788(18) 0.8362(3) 0.8996(3) 0.0224(7) Uani d . . . 1 . .
H H35 0.702536 0.870006 0.915401 0.027000 Uiso calc U . R 1 . .
C C36 0.64382(18) 0.7683(4) 0.9655(3) 0.0336(10) Uani d . . . 1 . .
H H36 0.662915 0.753774 1.025774 0.040000 Uiso calc U . R 1 . .
C C37 0.59240(19) 0.7219(3) 0.9439(4) 0.0329(10) Uani d . . . 1 . .
H H37 0.576751 0.674809 0.989025 0.039000 Uiso calc U . R 1 . .
C C38 0.56350(18) 0.7435(3) 0.8574(4) 0.0317(9) Uani d . . . 1 . .
H H38 0.527397 0.713281 0.844245 0.038000 Uiso calc U . R 1 . .
C C39 0.58739(18) 0.8093(3) 0.7897(3) 0.0289(9) Uani d . . . 1 . .
H H39 0.567868 0.824091 0.729903 0.035000 Uiso calc U . R 1 . .
C C40 0.73333(15) 0.9945(3) 0.7581(3) 0.0169(7) Uani d . . . 1 . .
C C41 0.77988(16) 0.9433(3) 0.8001(3) 0.0224(8) Uani d . . . 1 . .
H H41 0.779839 0.872235 0.802536 0.027000 Uiso calc U . R 1 . .
C C42 0.82595(16) 0.9965(3) 0.8379(3) 0.0257(8) Uani d . . . 1 . .
H H42 0.857068 0.962216 0.868035 0.031000 Uiso calc U . R 1 . .
C C43 0.82642(15) 1.1000(3) 0.8316(3) 0.0277(8) Uani d . . . 1 . .
H H43 0.858441 1.136296 0.856190 0.033000 Uiso calc U . R 1 . .
C C44 0.78084(17) 1.1511(3) 0.7901(3) 0.0246(8) Uani d . . . 1 . .
H H44 0.781656 1.222044 0.786322 0.030000 Uiso calc U . R 1 . .
C C45 0.73370(14) 1.0986(3) 0.7536(3) 0.0189(7) Uani d . . . 1 . .
H H45 0.702075 1.133605 0.725943 0.023000 Uiso calc U . R 1 . .
C C46 0.62476(15) 0.9943(3) 0.6451(3) 0.0202(7) Uani d . . . 1 . .
C C47 0.61347(17) 0.9765(3) 0.5455(3) 0.0244(8) Uani d . . . 1 . .
H H47 0.631853 0.922871 0.511962 0.029000 Uiso calc U . R 1 . .
C C48 0.5750(2) 1.0381(3) 0.4956(4) 0.0335(10) Uani d . . . 1 . .
H H48 0.566456 1.026063 0.428029 0.040000 Uiso calc U . R 1 . .
C C49 0.54918(19) 1.1165(3) 0.5447(4) 0.0364(11) Uani d . . . 1 . .
H H49 0.523724 1.159382 0.509824 0.044000 Uiso calc U . R 1 . .
C C50 0.55974(17) 1.1339(3) 0.6435(4) 0.0309(9) Uani d . . . 1 . .
H H50 0.541187 1.187700 0.676423 0.037000 Uiso calc U . R 1 . .
C C51 0.59750(16) 1.0727(3) 0.6949(3) 0.0247(8) Uani d . . . 1 . .
H H51 0.604742 1.083899 0.763056 0.030000 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 . 1.776(3) ?
U1 O2 . 1.781(3) ?
U1 O3 . 2.458(2) ?
U1 O7 . 2.465(3) ?
U1 O5 4_647 2.473(2) ?
U1 O8 . 2.474(3) ?
U1 O6 4_647 2.482(3) ?
U1 O4 . 2.484(2) ?
P1 C34 . 1.793(4) ?
P1 C40 . 1.795(4) ?
P1 C46 . 1.798(4) ?
P1 C28 . 1.800(4) ?
O3 C3 . 1.271(4) ?
O4 C3 . 1.260(4) ?
O5 C4 . 1.266(4) ?
O6 C4 . 1.264(4) ?
O7 C20 . 1.263(4) ?
O8 C20 . 1.262(4) ?
C1 C3 . 1.522(5) ?
C1 C2 . 1.549(5) ?
C1 C5 . 1.568(5) ?
C1 H1 . 1.000000 ?
C2 C4 . 1.522(4) ?
C2 C6 . 1.569(5) ?
C2 H2 . 1.000000 ?
C5 C13 . 1.516(5) ?
C5 C7 . 1.521(5) ?
C5 H5 . 1.000000 ?
C6 C14 . 1.514(5) ?
C6 C8 . 1.518(5) ?
C6 H6 . 1.000000 ?
C7 C12 . 1.378(5) ?
C7 C8 . 1.392(5) ?
C8 C9 . 1.392(5) ?
C9 C10 . 1.398(6) ?
C9 H9 . 0.950000 ?
C10 C11 . 1.382(7) ?
C10 H10 . 0.950000 ?
C11 C12 . 1.403(6) ?
C11 H11 . 0.950000 ?
C12 H12 . 0.950000 ?
C13 C18 . 1.381(5) ?
C13 C14 . 1.396(6) ?
C14 C15 . 1.385(5) ?
C15 C16 . 1.387(7) ?
C15 H15 . 0.950000 ?
C16 C17 . 1.375(8) ?
C16 H16 . 0.950000 ?
C17 C18 . 1.389(6) ?
C17 H17 . 0.950000 ?
C18 H18 . 0.950000 ?
C19 C20 . 1.522(5) ?
C19 C19 2_665 1.537(6) ?
C19 C21 . 1.571(5) ?
C19 H19 . 1.000000 ?
C21 C23 2_665 1.501(6) ?
C21 C22 . 1.518(5) ?
C21 H21 . 1.000000 ?
C22 C27 . 1.380(6) ?
C22 C23 . 1.400(6) ?
C23 C24 . 1.384(5) ?
C24 C25 . 1.378(7) ?
C24 H24 . 0.950000 ?
C25 C26 . 1.387(7) ?
C25 H25 . 0.950000 ?
C26 C27 . 1.398(6) ?
C26 H26 . 0.950000 ?
C27 H27 . 0.950000 ?
C28 C33 . 1.399(5) ?
C28 C29 . 1.400(5) ?
C29 C30 . 1.391(6) ?
C29 H29 . 0.950000 ?
C30 C31 . 1.374(6) ?
C30 H30 . 0.950000 ?
C31 C32 . 1.393(6) ?
C31 H31 . 0.950000 ?
C32 C33 . 1.389(5) ?
C32 H32 . 0.950000 ?
C33 H33 . 0.950000 ?
C34 C35 . 1.391(5) ?
C34 C39 . 1.397(5) ?
C35 C36 . 1.390(5) ?
C35 H35 . 0.950000 ?
C36 C37 . 1.381(6) ?
C36 H36 . 0.950000 ?
C37 C38 . 1.382(7) ?
C37 H37 . 0.950000 ?
C38 C39 . 1.386(6) ?
C38 H38 . 0.950000 ?
C39 H39 . 0.950000 ?
C40 C45 . 1.393(5) ?
C40 C41 . 1.403(5) ?
C41 C42 . 1.387(5) ?
C41 H41 . 0.950000 ?
C42 C43 . 1.386(6) ?
C42 H42 . 0.950000 ?
C43 C44 . 1.383(5) ?
C43 H43 . 0.950000 ?
C44 C45 . 1.394(5) ?
C44 H44 . 0.950000 ?
C45 H45 . 0.950000 ?
C46 C47 . 1.395(6) ?
C46 C51 . 1.399(5) ?
C47 C48 . 1.393(6) ?
C47 H47 . 0.950000 ?
C48 C49 . 1.379(6) ?
C48 H48 . 0.950000 ?
C49 C50 . 1.381(7) ?
C49 H49 . 0.950000 ?
C50 C51 . 1.388(6) ?
C50 H50 . 0.950000 ?
C51 H51 . 0.950000 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 U1 O2 . . 179.02(13) ?
O1 U1 O3 . . 92.76(10) ?
O2 U1 O3 . . 87.30(10) ?
O1 U1 O7 . . 88.54(10) ?
O2 U1 O7 . . 90.59(11) ?
O3 U1 O7 . . 121.49(8) ?
O1 U1 O5 . 4_647 88.52(10) ?
O2 U1 O5 . 4_647 92.30(10) ?
O3 U1 O5 . 4_647 119.47(8) ?
O7 U1 O5 . 4_647 119.04(8) ?
O1 U1 O8 . . 86.89(11) ?
O2 U1 O8 . . 92.22(11) ?
O3 U1 O8 . . 69.01(8) ?
O7 U1 O8 . . 52.66(8) ?
O5 U1 O8 4_647 . 170.59(8) ?
O1 U1 O6 . 4_647 91.75(10) ?
O2 U1 O6 . 4_647 88.33(10) ?
O3 U1 O6 . 4_647 170.66(8) ?
O7 U1 O6 . 4_647 66.78(8) ?
O5 U1 O6 4_647 4_647 52.48(8) ?
O8 U1 O6 . 4_647 119.44(8) ?
O1 U1 O4 . . 89.20(10) ?
O2 U1 O4 . . 91.61(10) ?
O3 U1 O4 . . 52.68(8) ?
O7 U1 O4 . . 173.63(8) ?
O5 U1 O4 4_647 . 66.84(8) ?
O8 U1 O4 . . 121.26(8) ?
O6 U1 O4 4_647 . 119.25(8) ?
C34 P1 C40 . . 110.95(17) ?
C34 P1 C46 . . 109.98(18) ?
C40 P1 C46 . . 110.78(17) ?
C34 P1 C28 . . 107.91(17) ?
C40 P1 C28 . . 107.19(17) ?
C46 P1 C28 . . 109.94(18) ?
C3 O3 U1 . . 94.0(2) ?
C3 O4 U1 . . 93.1(2) ?
C4 O5 U1 . 4_657 93.7(2) ?
C4 O6 U1 . 4_657 93.32(19) ?
C20 O7 U1 . . 93.5(2) ?
C20 O8 U1 . . 93.1(2) ?
C3 C1 C2 . . 113.7(3) ?
C3 C1 C5 . . 108.6(3) ?
C2 C1 C5 . . 109.3(3) ?
C3 C1 H1 . . 108.400000 ?
C2 C1 H1 . . 108.400000 ?
C5 C1 H1 . . 108.400000 ?
C4 C2 C1 . . 113.0(3) ?
C4 C2 C6 . . 108.3(3) ?
C1 C2 C6 . . 109.6(3) ?
C4 C2 H2 . . 108.600000 ?
C1 C2 H2 . . 108.600000 ?
C6 C2 H2 . . 108.600000 ?
O4 C3 O3 . . 120.1(3) ?
O4 C3 C1 . . 122.0(3) ?
O3 C3 C1 . . 117.9(3) ?
O6 C4 O5 . . 119.9(3) ?
O6 C4 C2 . . 118.4(3) ?
O5 C4 C2 . . 121.6(3) ?
C13 C5 C7 . . 106.3(3) ?
C13 C5 C1 . . 106.3(3) ?
C7 C5 C1 . . 107.9(3) ?
C13 C5 H5 . . 112.000000 ?
C7 C5 H5 . . 112.000000 ?
C1 C5 H5 . . 112.000000 ?
C14 C6 C8 . . 106.6(3) ?
C14 C6 C2 . . 108.2(3) ?
C8 C6 C2 . . 105.4(3) ?
C14 C6 H6 . . 112.100000 ?
C8 C6 H6 . . 112.100000 ?
C2 C6 H6 . . 112.100000 ?
C12 C7 C8 . . 120.4(4) ?
C12 C7 C5 . . 126.3(4) ?
C8 C7 C5 . . 113.3(3) ?
C7 C8 C9 . . 120.6(4) ?
C7 C8 C6 . . 113.3(3) ?
C9 C8 C6 . . 126.1(3) ?
C8 C9 C10 . . 118.6(4) ?
C8 C9 H9 . . 120.700000 ?
C10 C9 H9 . . 120.700000 ?
C11 C10 C9 . . 120.8(4) ?
C11 C10 H10 . . 119.600000 ?
C9 C10 H10 . . 119.600000 ?
C10 C11 C12 . . 119.9(4) ?
C10 C11 H11 . . 120.000000 ?
C12 C11 H11 . . 120.000000 ?
C7 C12 C11 . . 119.5(4) ?
C7 C12 H12 . . 120.300000 ?
C11 C12 H12 . . 120.300000 ?
C18 C13 C14 . . 120.8(4) ?
C18 C13 C5 . . 126.1(4) ?
C14 C13 C5 . . 113.1(3) ?
C15 C14 C13 . . 119.9(4) ?
C15 C14 C6 . . 126.5(4) ?
C13 C14 C6 . . 113.5(3) ?
C14 C15 C16 . . 119.0(4) ?
C14 C15 H15 . . 120.500000 ?
C16 C15 H15 . . 120.500000 ?
C17 C16 C15 . . 120.7(4) ?
C17 C16 H16 . . 119.600000 ?
C15 C16 H16 . . 119.600000 ?
C16 C17 C18 . . 120.8(4) ?
C16 C17 H17 . . 119.600000 ?
C18 C17 H17 . . 119.600000 ?
C13 C18 C17 . . 118.6(5) ?
C13 C18 H18 . . 120.700000 ?
C17 C18 H18 . . 120.700000 ?
C20 C19 C19 . 2_665 113.0(3) ?
C20 C19 C21 . . 108.9(3) ?
C19 C19 C21 2_665 . 109.33(18) ?
C20 C19 H19 . . 108.500000 ?
C19 C19 H19 2_665 . 108.500000 ?
C21 C19 H19 . . 108.500000 ?
O8 C20 O7 . . 120.4(3) ?
O8 C20 C19 . . 121.4(3) ?
O7 C20 C19 . . 118.2(3) ?
C23 C21 C22 2_665 . 107.7(3) ?
C23 C21 C19 2_665 . 107.9(3) ?
C22 C21 C19 . . 105.3(3) ?
C23 C21 H21 2_665 . 111.900000 ?
C22 C21 H21 . . 111.900000 ?
C19 C21 H21 . . 111.900000 ?
C27 C22 C23 . . 120.3(4) ?
C27 C22 C21 . . 127.0(4) ?
C23 C22 C21 . . 112.7(4) ?
C24 C23 C22 . . 120.3(4) ?
C24 C23 C21 . 2_665 126.3(4) ?
C22 C23 C21 . 2_665 113.4(3) ?
C25 C24 C23 . . 119.3(4) ?
C25 C24 H24 . . 120.400000 ?
C23 C24 H24 . . 120.400000 ?
C24 C25 C26 . . 120.9(4) ?
C24 C25 H25 . . 119.500000 ?
C26 C25 H25 . . 119.500000 ?
C25 C26 C27 . . 120.0(4) ?
C25 C26 H26 . . 120.000000 ?
C27 C26 H26 . . 120.000000 ?
C22 C27 C26 . . 119.2(4) ?
C22 C27 H27 . . 120.400000 ?
C26 C27 H27 . . 120.400000 ?
C33 C28 C29 . . 119.9(3) ?
C33 C28 P1 . . 119.5(3) ?
C29 C28 P1 . . 120.5(3) ?
C30 C29 C28 . . 119.3(4) ?
C30 C29 H29 . . 120.300000 ?
C28 C29 H29 . . 120.300000 ?
C31 C30 C29 . . 120.4(4) ?
C31 C30 H30 . . 119.800000 ?
C29 C30 H30 . . 119.800000 ?
C30 C31 C32 . . 120.8(4) ?
C30 C31 H31 . . 119.600000 ?
C32 C31 H31 . . 119.600000 ?
C33 C32 C31 . . 119.4(4) ?
C33 C32 H32 . . 120.300000 ?
C31 C32 H32 . . 120.300000 ?
C32 C33 C28 . . 120.0(4) ?
C32 C33 H33 . . 120.000000 ?
C28 C33 H33 . . 120.000000 ?
C35 C34 C39 . . 120.6(4) ?
C35 C34 P1 . . 121.1(3) ?
C39 C34 P1 . . 117.8(3) ?
C36 C35 C34 . . 118.8(4) ?
C36 C35 H35 . . 120.600000 ?
C34 C35 H35 . . 120.600000 ?
C37 C36 C35 . . 120.5(4) ?
C37 C36 H36 . . 119.700000 ?
C35 C36 H36 . . 119.700000 ?
C36 C37 C38 . . 120.6(4) ?
C36 C37 H37 . . 119.700000 ?
C38 C37 H37 . . 119.700000 ?
C37 C38 C39 . . 119.8(4) ?
C37 C38 H38 . . 120.100000 ?
C39 C38 H38 . . 120.100000 ?
C38 C39 C34 . . 119.6(4) ?
C38 C39 H39 . . 120.200000 ?
C34 C39 H39 . . 120.200000 ?
C45 C40 C41 . . 120.0(3) ?
C45 C40 P1 . . 123.5(3) ?
C41 C40 P1 . . 116.5(3) ?
C42 C41 C40 . . 119.9(4) ?
C42 C41 H41 . . 120.100000 ?
C40 C41 H41 . . 120.100000 ?
C43 C42 C41 . . 119.7(3) ?
C43 C42 H42 . . 120.100000 ?
C41 C42 H42 . . 120.100000 ?
C44 C43 C42 . . 120.8(4) ?
C44 C43 H43 . . 119.600000 ?
C42 C43 H43 . . 119.600000 ?
C43 C44 C45 . . 120.1(4) ?
C43 C44 H44 . . 119.900000 ?
C45 C44 H44 . . 119.900000 ?
C40 C45 C44 . . 119.5(3) ?
C40 C45 H45 . . 120.300000 ?
C44 C45 H45 . . 120.300000 ?
C47 C46 C51 . . 120.5(4) ?
C47 C46 P1 . . 120.9(3) ?
C51 C46 P1 . . 118.5(3) ?
C48 C47 C46 . . 119.3(4) ?
C48 C47 H47 . . 120.300000 ?
C46 C47 H47 . . 120.300000 ?
C49 C48 C47 . . 119.8(4) ?
C49 C48 H48 . . 120.100000 ?
C47 C48 H48 . . 120.100000 ?
C48 C49 C50 . . 121.1(4) ?
C48 C49 H49 . . 119.400000 ?
C50 C49 H49 . . 119.400000 ?
C49 C50 C51 . . 120.0(4) ?
C49 C50 H50 . . 120.000000 ?
C51 C50 H50 . . 120.000000 ?
C50 C51 C46 . . 119.2(4) ?
C50 C51 H51 . . 120.400000 ?
C46 C51 H51 . . 120.400000 ?

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
C1 H1 O5 . 1.00 2.29 2.819(4) 111.9 ?
C2 H2 O4 . 1.00 2.35 2.852(4) 110.4 ?
C19 H19 O8 2_665 1.00 2.36 2.863(4) 110.4 ?
C29 H29 O3 . 0.95 2.49 3.135(5) 124.8 ?
C51 H51 O6 4_657 0.95 2.60 3.395(5) 141.8 ?

####################################################################### 
# 
# 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 2290587'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2023-08-24 deposited with the CCDC.	2024-02-01 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT342_3                   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02233 Ang.  
RESPONSE: This low precision results from the rather low quality of the
crystals and the disorder affecting part of the structure.
;
# end Validation Reply Form

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C80 H80 N4 O26 U4'
_chemical_formula_iupac          ?
_chemical_formula_weight         2465.60
_chemical_absolute_configuration syn

_chemical_melting_point          ?

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

_cell_length_a                   17.5195(6)
_cell_length_b                   26.5815(7)
_cell_length_c                   8.8808(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4135.7(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6739
_cell_measurement_theta_min      2.2936
_cell_measurement_theta_max      23.8597
_cell_measurement_temperature    100(2)

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'translucent intense yellow-green'
_exptl_crystal_size_max          0.086
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.064
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2328

_exptl_absorpt_coefficient_mu    7.887
_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            53405
_diffrn_reflns_av_R_equivalents  0.1176
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_theta_min         1.92
_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       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10

_refine_special_details          
;
One dimethylammonium cation is disordered over two positions
which have been refined with occupancy parameters constrained
to sum to unity and with restraints on bond lengths and
displacement parameters. Some voids in the structure indicate 
the presence of unresolved solvent molecules whose contribution
to the structure factors was removed with SQUEEZE.
;

_reflns_number_total             7839
_reflns_number_gt                6652
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0472
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1058
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.037
_refine_ls_number_reflns         7839
_refine_ls_number_parameters     533
_refine_ls_number_restraints     132
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0365P)²+23.6777P] 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         1.427
_refine_diff_density_min         -1.068
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
Known absolute configuration.
;
_refine_ls_abs_structure_Flack   0.016(17)

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 0.54111(3) 0.37215(2) 0.60890(8) 0.03601(18) Uani d . . . 1.000000 . .
U U2 0.60333(3) 0.51428(2) 0.57316(8) 0.03681(18) Uani d . . . 1.000000 . .
O O1 0.5352(8) 0.3531(4) 0.4168(15) 0.054(3) Uani d . . . 1.000000 . .
O O2 0.5481(6) 0.3892(4) 0.7990(14) 0.040(3) Uani d . . . 1.000000 . .
O O3 0.6178(7) 0.5199(4) 0.3792(13) 0.047(3) Uani d . . . 1.000000 . .
O O4 0.5951(6) 0.5102(4) 0.7719(12) 0.038(3) Uani d . . . 1.000000 . .
O O5 0.4052(5) 0.3913(4) 0.5998(16) 0.043(3) Uani d . . . 1.000000 . .
O O6 0.2888(6) 0.4189(4) 0.6317(18) 0.056(4) Uani d . . . 1.000000 . .
O O7 0.4800(6) 0.2991(4) 0.6844(13) 0.034(3) Uani d . . . 1.000000 . .
O O8 0.4402(6) 0.2416(4) 0.8489(14) 0.047(3) Uani d . . . 1.000000 . .
O O9 0.6453(7) 0.3194(4) 0.6386(17) 0.055(4) Uani d . . . 1.000000 . .
O O10 0.7199(6) 0.2582(4) 0.5499(14) 0.040(3) Uani d . . . 1.000000 . .
O O11 0.6518(7) 0.4243(4) 0.5510(17) 0.047(3) Uani d . . . 1.000000 . .
O O12 0.7427(6) 0.4771(4) 0.6004(18) 0.052(3) Uani d . . . 1.000000 . .
O O13 0.5159(6) 0.4524(4) 0.5487(15) 0.040(3) Uani d . . . 1.000000 . .
N N1 0.5866(8) 0.2124(5) 0.6717(16) 0.039(3) Uani d . . . 1.000000 . .
H H1A 0.625638 0.229288 0.626689 0.047000 Uiso calc U . R 1.000000 . .
H H1B 0.545187 0.233041 0.671924 0.047000 Uiso calc U . R 1.000000 . .
C C1 0.3177(8) 0.3350(6) 0.7290(19) 0.031(4) Uani d . . . 1.000000 . .
H H1 0.320180 0.307583 0.652082 0.037000 Uiso calc U . R 1.000000 . .
C C2 0.3787(8) 0.3225(6) 0.8499(18) 0.030(4) Uani d . . . 1.000000 . .
H H2 0.407305 0.354141 0.873083 0.036000 Uiso calc U . R 1.000000 . .
C C3 0.3362(10) 0.3842(6) 0.647(2) 0.049(5) Uani d . . . 1.000000 . .
C C4 0.4365(8) 0.2833(6) 0.7943(19) 0.030(4) Uani d . . . 1.000000 . .
C C5 0.2366(9) 0.3343(6) 0.794(2) 0.046(5) Uani d . . . 1.000000 . .
H H5 0.197600 0.344935 0.718001 0.055000 Uiso calc U . R 1.000000 . .
C C6 0.3342(9) 0.3065(6) 0.9950(19) 0.033(4) Uani d . . . 1.000000 . .
H H6 0.369672 0.295687 1.077116 0.040000 Uiso calc U . R 1.000000 . .
C C7 0.2359(7) 0.3675(5) 0.9322(14) 0.064(4) Uani d U . G 1.000000 . .
C C8 0.2874(6) 0.3512(5) 1.0410(16) 0.061(4) Uani d U . G 1.000000 . .
C C9 0.2925(7) 0.3764(6) 1.1779(15) 0.069(4) Uani d U . G 1.000000 . .
H H9 0.327622 0.365299 1.252220 0.083000 Uiso calc U . R 1.000000 . .
C C10 0.2461(9) 0.4178(6) 1.2059(16) 0.088(5) Uani d U . G 1.000000 . .
H H10 0.249612 0.434991 1.299442 0.106000 Uiso calc U . R 1.000000 . .
C C11 0.1947(9) 0.4340(5) 1.0971(19) 0.095(5) Uani d U . G 1.000000 . .
H H11 0.163018 0.462336 1.116289 0.114000 Uiso calc U . R 1.000000 . .
C C12 0.1896(8) 0.4089(6) 0.9603(17) 0.082(5) Uani d U . G 1.000000 . .
H H12 0.154432 0.419988 0.885912 0.099000 Uiso calc U . R 1.000000 . .
C C13 0.2237(9) 0.2807(7) 0.8479(19) 0.038(4) Uani d . . . 1.000000 . .
C C14 0.2755(8) 0.2657(6) 0.9579(18) 0.032(4) Uani d . . . 1.000000 . .
C C15 0.2701(9) 0.2207(6) 1.0260(18) 0.037(4) Uani d . . . 1.000000 . .
H H15 0.305890 0.210385 1.100297 0.044000 Uiso calc U . R 1.000000 . .
C C16 0.2090(11) 0.1894(8) 0.982(2) 0.053(5) Uani d . . . 1.000000 . .
H H16 0.201944 0.158108 1.031824 0.064000 Uiso calc U . R 1.000000 . .
C C17 0.1587(9) 0.2034(7) 0.8683(19) 0.042(4) Uani d . . . 1.000000 . .
H H17 0.119020 0.181336 0.837360 0.051000 Uiso calc U . R 1.000000 . .
C C18 0.1671(9) 0.2486(6) 0.8029(19) 0.034(4) Uani d . . . 1.000000 . .
H H18 0.133375 0.258471 0.724493 0.041000 Uiso calc U . R 1.000000 . .
C C19 0.7550(8) 0.3438(5) 0.4980(17) 0.026(3) Uani d . . . 1.000000 . .
H H19 0.725493 0.358575 0.412359 0.031000 Uiso calc U . R 1.000000 . .
C C20 0.7726(10) 0.3887(6) 0.6118(18) 0.041(4) Uani d . . . 1.000000 . .
H H20 0.760855 0.375974 0.715204 0.049000 Uiso calc U . R 1.000000 . .
C C21 0.7051(8) 0.3028(5) 0.567(2) 0.034(4) Uani d . . . 1.000000 . .
C C22 0.7220(9) 0.4322(5) 0.585(2) 0.034(4) Uani d . . . 1.000000 . .
C C23 0.8314(8) 0.3250(6) 0.432(2) 0.033(4) Uani d . . . 1.000000 . .
H H23 0.824025 0.295754 0.362904 0.039000 Uiso calc U . R 1.000000 . .
C C24 0.8592(9) 0.3999(6) 0.607(2) 0.041(4) Uani d . . . 1.000000 . .
H H24 0.872789 0.428656 0.674693 0.049000 Uiso calc U . R 1.000000 . .
C C25 0.8648(8) 0.3697(7) 0.3523(19) 0.038(4) Uani d . . . 1.000000 . .
C C26 0.8792(9) 0.4110(6) 0.4447(19) 0.035(4) Uani d . . . 1.000000 . .
C C27 0.9050(10) 0.4558(8) 0.385(3) 0.069(7) Uani d . . . 1.000000 . .
H H27 0.912369 0.484519 0.446960 0.082000 Uiso calc U . R 1.000000 . .
C C28 0.9199(11) 0.4575(9) 0.230(3) 0.069(7) Uani d . . . 1.000000 . .
H H28 0.941179 0.487130 0.187562 0.082000 Uiso calc U . R 1.000000 . .
C C29 0.9046(13) 0.4180(9) 0.141(3) 0.063(6) Uani d . . . 1.000000 . .
H H29 0.911829 0.421324 0.035896 0.076000 Uiso calc U . R 1.000000 . .
C C30 0.8791(9) 0.3733(8) 0.1974(19) 0.043(4) Uani d . . . 1.000000 . .
H H30 0.871271 0.345216 0.132884 0.051000 Uiso calc U . R 1.000000 . .
C C31 0.8839(8) 0.3118(6) 0.5642(18) 0.030(3) Uani d . . . 1.000000 . .
C C32 0.8995(10) 0.3527(6) 0.653(2) 0.042(4) Uani d . . . 1.000000 . .
C C33 0.9488(11) 0.3487(8) 0.776(2) 0.051(5) Uani d . . . 1.000000 . .
H H33 0.960844 0.377299 0.835974 0.062000 Uiso calc U . R 1.000000 . .
C C34 0.9798(10) 0.3018(9) 0.809(2) 0.054(6) Uani d . . . 1.000000 . .
H H34 1.012650 0.298088 0.893506 0.065000 Uiso calc U . R 1.000000 . .
C C35 0.9634(10) 0.2602(7) 0.720(2) 0.044(4) Uani d . . . 1.000000 . .
H H35 0.986303 0.228553 0.740519 0.053000 Uiso calc U . R 1.000000 . .
C C36 0.9140(8) 0.2656(6) 0.602(2) 0.034(4) Uani d . . . 1.000000 . .
H H36 0.899934 0.236824 0.545491 0.041000 Uiso calc U . R 1.000000 . .
C C37 0.6074(12) 0.2018(9) 0.824(2) 0.066(6) Uani d . . . 1.000000 . .
H H37A 0.562964 0.188750 0.878057 0.099000 Uiso calc U . R 1.000000 . .
H H37B 0.625390 0.232661 0.872324 0.099000 Uiso calc U . R 1.000000 . .
H H37C 0.648273 0.176566 0.824946 0.099000 Uiso calc U . R 1.000000 . .
C C38 0.5687(9) 0.1673(6) 0.581(2) 0.040(4) Uani d . . . 1.000000 . .
H H38A 0.612585 0.144418 0.581618 0.060000 Uiso calc U . R 1.000000 . .
H H38B 0.557343 0.177339 0.477278 0.060000 Uiso calc U . R 1.000000 . .
H H38C 0.524247 0.150133 0.624175 0.060000 Uiso calc U . R 1.000000 . .
N N2A 0.608(2) 0.4299(12) 0.162(4) 0.103(8) Uani d U P D 0.60(2) A 1
H H2A 0.606816 0.437218 0.261732 0.123000 Uiso calc U P R 0.60(2) A 1
H H2B 0.627009 0.398408 0.149334 0.123000 Uiso calc U P R 0.60(2) A 1
C C39A 0.527(2) 0.4332(16) 0.095(5) 0.106(8) Uani d U P D 0.60(2) A 1
H H39A 0.516095 0.468397 0.070675 0.158000 Uiso d U P R 0.60(2) A 1
H H39B 0.489649 0.420783 0.167838 0.158000 Uiso d U P R 0.60(2) A 1
H H39C 0.524954 0.412859 0.003342 0.158000 Uiso d U P R 0.60(2) A 1
C C40A 0.656(2) 0.4680(14) 0.077(5) 0.099(9) Uani d U P D 0.60(2) A 1
H H40A 0.648503 0.463805 -0.031354 0.148000 Uiso d U P R 0.60(2) A 1
H H40B 0.709433 0.462624 0.102855 0.148000 Uiso d U P R 0.60(2) A 1
H H40C 0.640487 0.502095 0.106802 0.148000 Uiso d U P R 0.60(2) A 1
N N2B 0.531(4) 0.4469(19) 0.195(5) 0.103(8) Uani d U P D 0.40(2) A -2
H H2C 0.511646 0.471034 0.256648 0.124000 Uiso calc U P R 0.40(2) A -2
H H2D 0.575177 0.435137 0.235164 0.124000 Uiso calc U P R 0.40(2) A -2
C C39B 0.474(4) 0.404(2) 0.176(7) 0.102(9) Uani d U P D 0.40(2) A -2
H H39D 0.427973 0.417264 0.125850 0.153000 Uiso d U P R 0.40(2) A -2
H H39E 0.459980 0.390154 0.273841 0.153000 Uiso d U P R 0.40(2) A -2
H H39F 0.496929 0.378009 0.113101 0.153000 Uiso d U P R 0.40(2) A -2
C C40B 0.545(4) 0.468(2) 0.038(6) 0.100(9) Uani d U P D 0.40(2) A -2
H H40D 0.498114 0.466717 -0.021632 0.150000 Uiso d U P R 0.40(2) A -2
H H40E 0.585080 0.448612 -0.011512 0.150000 Uiso d U P R 0.40(2) A -2
H H40F 0.561479 0.503209 0.048488 0.150000 Uiso d U P R 0.40(2) A -2


_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 . 1.753(12) ?
U1 O1 . 1.783(13) ?
U1 O13 . 2.243(10) ?
U1 O7 . 2.315(10) ?
U1 O9 . 2.316(11) ?
U1 O5 . 2.436(10) ?
U1 O11 . 2.439(11) ?
U1 U2 . 3.9450(8) ?
U1 U2 2_665 3.9521(8) ?
U2 O3 . 1.748(12) ?
U2 O4 . 1.774(11) ?
U2 O13 . 2.259(10) ?
U2 O13 2_665 2.278(11) ?
U2 O5 2_665 2.526(10) ?
U2 O11 . 2.545(10) ?
U2 O6 2_665 2.644(12) ?
U2 O12 . 2.646(11) ?
U2 U2 2_665 3.6993(12) ?
O5 C3 . 1.29(2) ?
O6 C3 . 1.249(19) ?
O7 C4 . 1.309(18) ?
O8 C4 . 1.210(18) ?
O9 C21 . 1.305(18) ?
O10 C21 . 1.221(17) ?
O11 C22 . 1.283(19) ?
O12 C22 . 1.253(16) ?
N1 C37 . 1.43(2) ?
N1 C38 . 1.48(2) ?
N1 H1A . 0.910000 ?
N1 H1B . 0.910000 ?
C1 C3 . 1.53(2) ?
C1 C5 . 1.53(2) ?
C1 C2 . 1.55(2) ?
C1 H1 . 1.000000 ?
C2 C4 . 1.535(19) ?
C2 C6 . 1.57(2) ?
C2 H2 . 1.000000 ?
C5 C7 . 1.51(2) ?
C5 C13 . 1.52(3) ?
C5 H5 . 1.000000 ?
C6 C8 . 1.501(17) ?
C6 C14 . 1.53(2) ?
C6 H6 . 1.000000 ?
C7 C8 . 1.390000 ?
C7 C12 . 1.390000 ?
C8 C9 . 1.390000 ?
C9 C10 . 1.390000 ?
C9 H9 . 0.950000 ?
C10 C11 . 1.390000 ?
C10 H10 . 0.950000 ?
C11 C12 . 1.390000 ?
C11 H11 . 0.950000 ?
C12 H12 . 0.950000 ?
C13 C18 . 1.37(2) ?
C13 C14 . 1.39(2) ?
C14 C15 . 1.34(2) ?
C15 C16 . 1.41(2) ?
C15 H15 . 0.950000 ?
C16 C17 . 1.39(3) ?
C16 H16 . 0.950000 ?
C17 C18 . 1.34(2) ?
C17 H17 . 0.950000 ?
C18 H18 . 0.950000 ?
C19 C21 . 1.53(2) ?
C19 C23 . 1.544(19) ?
C19 C20 . 1.59(2) ?
C19 H19 . 1.000000 ?
C20 C22 . 1.48(2) ?
C20 C24 . 1.55(2) ?
C20 H20 . 1.000000 ?
C23 C25 . 1.50(2) ?
C23 C31 . 1.53(2) ?
C23 H23 . 1.000000 ?
C24 C32 . 1.50(2) ?
C24 C26 . 1.52(3) ?
C24 H24 . 1.000000 ?
C25 C26 . 1.39(2) ?
C25 C30 . 1.40(2) ?
C26 C27 . 1.38(2) ?
C27 C28 . 1.40(4) ?
C27 H27 . 0.950000 ?
C28 C29 . 1.34(3) ?
C28 H28 . 0.950000 ?
C29 C30 . 1.36(3) ?
C29 H29 . 0.950000 ?
C30 H30 . 0.950000 ?
C31 C32 . 1.37(2) ?
C31 C36 . 1.38(2) ?
C32 C33 . 1.40(2) ?
C33 C34 . 1.39(3) ?
C33 H33 . 0.950000 ?
C34 C35 . 1.39(3) ?
C34 H34 . 0.950000 ?
C35 C36 . 1.36(2) ?
C35 H35 . 0.950000 ?
C36 H36 . 0.950000 ?
C37 H37A . 0.980000 ?
C37 H37B . 0.980000 ?
C37 H37C . 0.980000 ?
C38 H38A . 0.980000 ?
C38 H38B . 0.980000 ?
C38 H38C . 0.980000 ?
N2A C40A . 1.513(14) ?
N2A C39A . 1.529(14) ?
N2A H2A . 0.910000 ?
N2A H2B . 0.910000 ?
C39A H39A . 0.980000 ?
C39A H39B . 0.980000 ?
C39A H39C . 0.980000 ?
C40A H40A . 0.980000 ?
C40A H40B . 0.980000 ?
C40A H40C . 0.980000 ?
N2B C40B . 1.519(14) ?
N2B C39B . 1.520(14) ?
N2B H2C . 0.910000 ?
N2B H2D . 0.910000 ?
C39B H39D . 0.980000 ?
C39B H39E . 0.980000 ?
C39B H39F . 0.980000 ?
C40B H40D . 0.980000 ?
C40B H40E . 0.980000 ?
C40B H40F . 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 . . 178.3(5) ?
O2 U1 O13 . . 89.9(5) ?
O1 U1 O13 . . 91.7(5) ?
O2 U1 O7 . . 88.3(4) ?
O1 U1 O7 . . 90.7(4) ?
O13 U1 O7 . . 140.8(4) ?
O2 U1 O9 . . 89.5(5) ?
O1 U1 O9 . . 89.0(6) ?
O13 U1 O9 . . 139.3(4) ?
O7 U1 O9 . . 79.9(4) ?
O2 U1 O5 . . 92.7(5) ?
O1 U1 O5 . . 88.3(6) ?
O13 U1 O5 . . 66.5(4) ?
O7 U1 O5 . . 74.5(3) ?
O9 U1 O5 . . 154.2(4) ?
O2 U1 O11 . . 90.0(5) ?
O1 U1 O11 . . 90.4(5) ?
O13 U1 O11 . . 64.3(4) ?
O7 U1 O11 . . 154.8(4) ?
O9 U1 O11 . . 75.0(4) ?
O5 U1 O11 . . 130.6(4) ?
O3 U2 O4 . . 176.0(5) ?
O3 U2 O13 . . 93.8(5) ?
O4 U2 O13 . . 89.8(5) ?
O3 U2 O13 . 2_665 90.3(5) ?
O4 U2 O13 . 2_665 92.6(5) ?
O13 U2 O13 . 2_665 69.6(4) ?
O3 U2 O5 . 2_665 90.9(5) ?
O4 U2 O5 . 2_665 87.9(5) ?
O13 U2 O5 . 2_665 133.8(3) ?
O13 U2 O5 2_665 2_665 64.4(3) ?
O3 U2 O11 . . 87.4(5) ?
O4 U2 O11 . . 92.7(5) ?
O13 U2 O11 . . 62.3(4) ?
O13 U2 O11 2_665 . 131.6(4) ?
O5 U2 O11 2_665 . 163.9(3) ?
O3 U2 O6 . 2_665 91.9(5) ?
O4 U2 O6 . 2_665 84.4(5) ?
O13 U2 O6 . 2_665 173.1(5) ?
O13 U2 O6 2_665 2_665 114.4(3) ?
O5 U2 O6 2_665 2_665 49.9(3) ?
O11 U2 O6 . 2_665 114.1(3) ?
O3 U2 O12 . . 89.3(5) ?
O4 U2 O12 . . 87.8(5) ?
O13 U2 O12 . . 111.3(4) ?
O13 U2 O12 2_665 . 179.0(3) ?
O5 U2 O12 2_665 . 114.7(3) ?
O11 U2 O12 . . 49.3(4) ?
O6 U2 O12 2_665 . 64.8(3) ?
C3 O5 U1 . . 150.8(11) ?
C3 O5 U2 . 2_665 96.9(9) ?
U1 O5 U2 . 2_665 105.6(3) ?
C3 O6 U2 . 2_665 92.5(10) ?
C4 O7 U1 . . 139.1(10) ?
C21 O9 U1 . . 141.5(12) ?
C22 O11 U1 . . 143.7(12) ?
C22 O11 U2 . . 98.5(8) ?
U1 O11 U2 . . 104.6(4) ?
C22 O12 U2 . . 94.5(9) ?
U1 O13 U2 . . 122.4(5) ?
U1 O13 U2 . 2_665 121.8(5) ?
U2 O13 U2 . 2_665 109.2(4) ?
C37 N1 C38 . . 114.1(15) ?
C37 N1 H1A . . 108.700000 ?
C38 N1 H1A . . 108.700000 ?
C37 N1 H1B . . 108.700000 ?
C38 N1 H1B . . 108.700000 ?
H1A N1 H1B . . 107.600000 ?
C3 C1 C5 . . 112.7(14) ?
C3 C1 C2 . . 111.6(13) ?
C5 C1 C2 . . 112.1(14) ?
C3 C1 H1 . . 106.700000 ?
C5 C1 H1 . . 106.700000 ?
C2 C1 H1 . . 106.700000 ?
C4 C2 C1 . . 112.2(13) ?
C4 C2 C6 . . 114.1(13) ?
C1 C2 C6 . . 106.6(12) ?
C4 C2 H2 . . 107.900000 ?
C1 C2 H2 . . 107.900000 ?
C6 C2 H2 . . 107.900000 ?
O6 C3 O5 . . 118.6(16) ?
O6 C3 C1 . . 122.8(17) ?
O5 C3 C1 . . 118.4(14) ?
O8 C4 O7 . . 124.2(14) ?
O8 C4 C2 . . 121.9(14) ?
O7 C4 C2 . . 113.9(13) ?
C7 C5 C13 . . 106.8(16) ?
C7 C5 C1 . . 107.7(13) ?
C13 C5 C1 . . 105.5(13) ?
C7 C5 H5 . . 112.100000 ?
C13 C5 H5 . . 112.100000 ?
C1 C5 H5 . . 112.100000 ?
C8 C6 C14 . . 104.6(12) ?
C8 C6 C2 . . 106.4(13) ?
C14 C6 C2 . . 110.4(12) ?
C8 C6 H6 . . 111.700000 ?
C14 C6 H6 . . 111.700000 ?
C2 C6 H6 . . 111.700000 ?
C8 C7 C12 . . 120.000000 ?
C8 C7 C5 . . 112.2(11) ?
C12 C7 C5 . . 127.7(11) ?
C7 C8 C9 . . 120.000000 ?
C7 C8 C6 . . 114.3(11) ?
C9 C8 C6 . . 125.7(11) ?
C10 C9 C8 . . 120.000000 ?
C10 C9 H9 . . 120.000000 ?
C8 C9 H9 . . 120.000000 ?
C9 C10 C11 . . 120.000000 ?
C9 C10 H10 . . 120.000000 ?
C11 C10 H10 . . 120.000000 ?
C12 C11 C10 . . 120.000000 ?
C12 C11 H11 . . 120.000000 ?
C10 C11 H11 . . 120.000000 ?
C11 C12 C7 . . 120.000000 ?
C11 C12 H12 . . 120.000000 ?
C7 C12 H12 . . 120.000000 ?
C18 C13 C14 . . 120.0(17) ?
C18 C13 C5 . . 126.8(16) ?
C14 C13 C5 . . 113.2(14) ?
C15 C14 C13 . . 121.7(15) ?
C15 C14 C6 . . 125.5(15) ?
C13 C14 C6 . . 112.7(15) ?
C14 C15 C16 . . 117.0(17) ?
C14 C15 H15 . . 121.500000 ?
C16 C15 H15 . . 121.500000 ?
C17 C16 C15 . . 121.6(18) ?
C17 C16 H16 . . 119.200000 ?
C15 C16 H16 . . 119.200000 ?
C18 C17 C16 . . 118.9(15) ?
C18 C17 H17 . . 120.600000 ?
C16 C17 H17 . . 120.600000 ?
C17 C18 C13 . . 120.7(17) ?
C17 C18 H18 . . 119.600000 ?
C13 C18 H18 . . 119.600000 ?
C21 C19 C23 . . 114.6(12) ?
C21 C19 C20 . . 113.1(12) ?
C23 C19 C20 . . 108.3(12) ?
C21 C19 H19 . . 106.800000 ?
C23 C19 H19 . . 106.800000 ?
C20 C19 H19 . . 106.800000 ?
C22 C20 C24 . . 115.7(13) ?
C22 C20 C19 . . 111.6(14) ?
C24 C20 C19 . . 108.5(13) ?
C22 C20 H20 . . 106.900000 ?
C24 C20 H20 . . 106.900000 ?
C19 C20 H20 . . 106.900000 ?
O10 C21 O9 . . 124.1(15) ?
O10 C21 C19 . . 121.5(14) ?
O9 C21 C19 . . 114.4(12) ?
O12 C22 O11 . . 117.3(13) ?
O12 C22 C20 . . 123.6(15) ?
O11 C22 C20 . . 119.0(13) ?
O12 C22 U2 . . 61.1(8) ?
O11 C22 U2 . . 56.6(7) ?
C20 C22 U2 . . 170.4(12) ?
C25 C23 C31 . . 108.0(12) ?
C25 C23 C19 . . 105.1(12) ?
C31 C23 C19 . . 107.8(13) ?
C25 C23 H23 . . 111.900000 ?
C31 C23 H23 . . 111.900000 ?
C19 C23 H23 . . 111.900000 ?
C32 C24 C26 . . 108.2(14) ?
C32 C24 C20 . . 107.2(14) ?
C26 C24 C20 . . 106.8(14) ?
C32 C24 H24 . . 111.500000 ?
C26 C24 H24 . . 111.500000 ?
C20 C24 H24 . . 111.500000 ?
C26 C25 C30 . . 119.5(17) ?
C26 C25 C23 . . 114.5(14) ?
C30 C25 C23 . . 126.0(17) ?
C27 C26 C25 . . 120.9(19) ?
C27 C26 C24 . . 127.6(18) ?
C25 C26 C24 . . 111.5(13) ?
C26 C27 C28 . . 118.(2) ?
C26 C27 H27 . . 121.100000 ?
C28 C27 H27 . . 121.100000 ?
C29 C28 C27 . . 121.0(19) ?
C29 C28 H28 . . 119.500000 ?
C27 C28 H28 . . 119.500000 ?
C28 C29 C30 . . 122.(2) ?
C28 C29 H29 . . 118.900000 ?
C30 C29 H29 . . 118.900000 ?
C29 C30 C25 . . 118.(2) ?
C29 C30 H30 . . 120.800000 ?
C25 C30 H30 . . 120.800000 ?
C32 C31 C36 . . 119.1(16) ?
C32 C31 C23 . . 112.4(14) ?
C36 C31 C23 . . 128.5(14) ?
C31 C32 C33 . . 121.0(16) ?
C31 C32 C24 . . 114.4(15) ?
C33 C32 C24 . . 124.6(16) ?
C34 C33 C32 . . 118.2(17) ?
C34 C33 H33 . . 120.900000 ?
C32 C33 H33 . . 120.900000 ?
C35 C34 C33 . . 120.9(17) ?
C35 C34 H34 . . 119.600000 ?
C33 C34 H34 . . 119.600000 ?
C36 C35 C34 . . 118.9(16) ?
C36 C35 H35 . . 120.500000 ?
C34 C35 H35 . . 120.500000 ?
C35 C36 C31 . . 121.7(15) ?
C35 C36 H36 . . 119.200000 ?
C31 C36 H36 . . 119.200000 ?
N1 C37 H37A . . 109.500000 ?
N1 C37 H37B . . 109.500000 ?
H37A C37 H37B . . 109.500000 ?
N1 C37 H37C . . 109.500000 ?
H37A C37 H37C . . 109.500000 ?
H37B C37 H37C . . 109.500000 ?
N1 C38 H38A . . 109.500000 ?
N1 C38 H38B . . 109.500000 ?
H38A C38 H38B . . 109.500000 ?
N1 C38 H38C . . 109.500000 ?
H38A C38 H38C . . 109.500000 ?
H38B C38 H38C . . 109.500000 ?
C40A N2A C39A . . 106.4(13) ?
C40A N2A H2A . . 110.500000 ?
C39A N2A H2A . . 110.500000 ?
C40A N2A H2B . . 110.500000 ?
C39A N2A H2B . . 110.500000 ?
H2A N2A H2B . . 108.600000 ?
N2A C39A H39A . . 109.000000 ?
N2A C39A H39B . . 110.300000 ?
H39A C39A H39B . . 109.500000 ?
N2A C39A H39C . . 109.200000 ?
H39A C39A H39C . . 109.500000 ?
H39B C39A H39C . . 109.500000 ?
N2A C40A H40A . . 109.900000 ?
N2A C40A H40B . . 108.800000 ?
H40A C40A H40B . . 109.500000 ?
N2A C40A H40C . . 109.700000 ?
H40A C40A H40C . . 109.500000 ?
H40B C40A H40C . . 109.500000 ?
C40B N2B C39B . . 106.4(13) ?
C40B N2B H2C . . 110.500000 ?
C39B N2B H2C . . 110.500000 ?
C40B N2B H2D . . 110.500000 ?
C39B N2B H2D . . 110.500000 ?
H2C N2B H2D . . 108.600000 ?
N2B C39B H39D . . 109.100000 ?
N2B C39B H39E . . 110.400000 ?
H39D C39B H39E . . 109.500000 ?
N2B C39B H39F . . 108.800000 ?
H39D C39B H39F . . 109.500000 ?
H39E C39B H39F . . 109.500000 ?
N2B C40B H40D . . 110.300000 ?
N2B C40B H40E . . 109.500000 ?
H40D C40B H40E . . 109.500000 ?
N2B C40B H40F . . 108.600000 ?
H40D C40B H40F . . 109.500000 ?
H40E C40B H40F . . 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
N1 H1A O9 . 0.91 2.42 3.039(17) 125 ?
N1 H1A O10 . 0.91 1.95 2.847(18) 171 ?
N1 H1B O7 . 0.91 2.10 2.969(16) 160 ?
N1 H1B O8 . 0.91 2.43 3.109(18) 132 ?
C37 H37A O8 . 0.98 2.58 3.12(2) 115 ?
N2A H2A O3 . 0.91 2.44 3.08(4) 128 ?
C39A H39C O2 1_554 0.98 1.96 2.90(5) 160 ?
C40A H40C O3 . 0.98 2.50 3.09(5) 119 ?
C40A H40A O4 1_554 0.98 2.33 3.12(4) 137 ?
N2B H2C O3 . 0.91 2.52 2.96(5) 111 ?
N2B H2C O3 2_665 0.91 2.53 3.20(7) 131 ?
C39B H39E O1 . 0.98 2.08 2.76(7) 125 ?
C40B H40D O4 2_664 0.98 2.53 3.46(7) 158 ?
C40B H40E O2 1_554 0.98 2.40 2.99(6) 118 ?


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

data_8
_database_code_depnum_ccdc_archive 'CCDC 2290592'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2023-08-24 deposited with the CCDC.	2024-02-01 downloaded from the CCDC.
;

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H43 Ag2 N2 O16.50 U2'
_chemical_formula_iupac          ?
_chemical_formula_weight         1723.74

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 2/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'
'-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                   15.4596(4)
_cell_length_b                   15.1930(4)
_cell_length_c                   21.8735(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.5571(9)
_cell_angle_gamma                90
_cell_volume                     5113.5(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9349
_cell_measurement_theta_min      2.5634
_cell_measurement_theta_max      36.4043
_cell_measurement_temperature    100(2)

_exptl_crystal_description       irregular
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.070
_exptl_crystal_density_diffrn    2.239
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3260

_exptl_absorpt_coefficient_mu    7.149
_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  0.67
_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            90293
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_theta_min         1.88
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_full        28.70
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29

_refine_special_details          
;
The solvent water molecule has been given partial occupancy
so as to retain an acceptable displacement parameter, and its
H atoms were not found.
;

_reflns_number_total             6585
_reflns_number_gt                6542
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0182
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0466
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.119
_refine_ls_number_reflns         6585
_refine_ls_number_parameters     371
_refine_ls_number_restraints     12
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0200P)²+22.0710P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_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         1.561
_refine_diff_density_min         -0.875
_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'
Ag Ag -0.8971 1.1015 '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 0.13717(2) 0.23815(2) 0.58682(2) 0.01133(3) Uani d . . . 1 . .
Ag Ag1 0.34039(2) 0.60452(2) 0.59791(2) 0.02090(5) Uani d . . . 1 . .
O O1 0.16643(11) 0.13964(11) 0.62756(8) 0.0174(3) Uani d . . . 1 . .
O O2 0.10737(11) 0.33588(12) 0.54574(8) 0.0179(3) Uani d . . . 1 . .
O O3 0.28426(11) 0.28391(12) 0.59540(8) 0.0167(3) Uani d . . . 1 . .
O O4 0.31447(10) 0.32414(12) 0.50177(7) 0.0156(3) Uani d . . . 1 . .
O O5 0.48899(11) 0.32565(12) 0.45816(8) 0.0177(3) Uani d . . . 1 . .
O O6 0.60045(11) 0.40709(12) 0.49621(8) 0.0188(3) Uani d . . . 1 . .
O O7 0.02325(11) 0.27131(11) 0.65767(8) 0.0149(3) Uani d . . . 1 . .
O O8 0.15578(11) 0.32010(12) 0.68212(8) 0.0179(3) Uani d . . . 1 . .
O O9 0.2401(6) 0.4757(7) 0.5891(5) 0.041(2) Uani d . P . 0.25 . .
N N1 0.2177(2) 0.6359(3) 0.54603(16) 0.0633(10) Uani d U . . 1 . .
C C1 0.43212(14) 0.31583(15) 0.58128(10) 0.0127(4) Uani d . . . 1 . .
H H1 0.461587 0.262223 0.566746 0.015000 Uiso calc U . R 1 . .
C C2 0.47748(14) 0.39727(15) 0.55457(10) 0.0125(4) Uani d . . . 1 . .
H H2 0.430685 0.439852 0.539888 0.015000 Uiso calc U . R 1 . .
C C3 0.33649(14) 0.30822(15) 0.55823(10) 0.0132(4) Uani d . . . 1 . .
C C4 0.52730(14) 0.37515(15) 0.49980(10) 0.0137(4) Uani d . . . 1 . .
C C5 0.44841(14) 0.31669(15) 0.65275(10) 0.0122(4) Uani d . . . 1 . .
H H5 0.416011 0.268767 0.672044 0.015000 Uiso calc U . R 1 . .
C C6 0.53605(14) 0.44357(15) 0.60739(10) 0.0130(4) Uani d . . . 1 . .
H H6 0.570707 0.493034 0.592003 0.016000 Uiso calc U . R 1 . .
C C7 0.42329(14) 0.40730(15) 0.67400(10) 0.0130(4) Uani d . . . 1 . .
C C8 0.47279(14) 0.47468(15) 0.65156(10) 0.0135(4) Uani d . . . 1 . .
C C9 0.45928(15) 0.56267(16) 0.66826(10) 0.0156(4) Uani d . . . 1 . .
H H9 0.493911 0.608574 0.654015 0.019000 Uiso calc U . R 1 . .
C C10 0.39317(16) 0.58143(16) 0.70664(11) 0.0168(4) Uani d . . . 1 . .
H H10 0.383123 0.640435 0.718471 0.020000 Uiso calc U . R 1 . .
C C11 0.34240(15) 0.51319(16) 0.72730(11) 0.0170(4) Uani d . . . 1 . .
H H11 0.297367 0.526400 0.752475 0.020000 Uiso calc U . R 1 . .
C C12 0.35732(15) 0.42639(16) 0.71129(10) 0.0147(4) Uani d . . . 1 . .
H H12 0.322907 0.380361 0.725610 0.018000 Uiso calc U . R 1 . .
C C13 0.54594(14) 0.30626(15) 0.66528(10) 0.0138(4) Uani d . . . 1 . .
C C14 0.59305(14) 0.37288(15) 0.63910(10) 0.0139(4) Uani d . . . 1 . .
C C15 0.68319(15) 0.36804(17) 0.64148(11) 0.0180(4) Uani d . . . 1 . .
H H15 0.715192 0.412408 0.622933 0.022000 Uiso calc U . R 1 . .
C C16 0.72598(16) 0.29681(18) 0.67161(12) 0.0210(5) Uani d . . . 1 . .
H H16 0.787514 0.292964 0.673524 0.025000 Uiso calc U . R 1 . .
C C17 0.67941(18) 0.23148(17) 0.69883(13) 0.0216(5) Uani d . . . 1 . .
H H17 0.709288 0.184089 0.719875 0.026000 Uiso calc U . R 1 . .
C C18 0.58874(17) 0.23565(16) 0.69517(12) 0.0174(5) Uani d . . . 1 . .
H H18 0.556650 0.190632 0.712945 0.021000 Uiso calc U . R 1 . .
C C19 0.04915(14) 0.36876(15) 0.74640(10) 0.0120(4) Uani d . . . 1 . .
H H19 0.079821 0.343410 0.784756 0.014000 Uiso calc U . R 1 . .
C C20 0.07650(14) 0.31644(15) 0.69243(10) 0.0127(4) Uani d . . . 1 . .
C C21 0.08127(15) 0.46626(15) 0.74031(11) 0.0151(4) Uani d . . . 1 . .
H H21 0.143959 0.469083 0.732706 0.018000 Uiso calc U . R 1 . .
C C22 0.02292(16) 0.50672(15) 0.68818(11) 0.0162(4) Uani d . . . 1 . .
C C23 -0.06465(16) 0.51012(15) 0.69994(11) 0.0169(4) Uani d . . . 1 . .
C C24 -0.12681(18) 0.54623(17) 0.65706(12) 0.0211(5) Uani d . . . 1 . .
H H24 -0.185765 0.550047 0.665647 0.025000 Uiso calc U . R 1 . .
C C25 -0.1018(2) 0.57689(18) 0.60118(13) 0.0251(5) Uani d . . . 1 . .
H H25 -0.143707 0.602143 0.571693 0.030000 Uiso calc U . R 1 . .
C C26 -0.0157(2) 0.57044(17) 0.58876(12) 0.0253(5) Uani d . . . 1 . .
H H26 0.000468 0.589708 0.550134 0.030000 Uiso calc U . R 1 . .
C C27 0.04763(18) 0.53606(17) 0.63213(12) 0.0209(5) Uani d . . . 1 . .
H H27 0.106609 0.532762 0.623523 0.025000 Uiso calc U . R 1 . .
C C28 0.1722(2) 0.6444(3) 0.50268(16) 0.0423(8) Uani d U . . 1 . .
C C29 0.11439(18) 0.6536(2) 0.44690(13) 0.0267(5) Uani d . . . 1 . .
H H29A 0.138848 0.622420 0.413334 0.040000 Uiso calc U . R 1 . .
H H29B 0.107650 0.716113 0.436419 0.040000 Uiso calc U . R 1 . .
H H29C 0.057527 0.628517 0.453182 0.040000 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 . 1.7732(17) ?
U1 O1 . 1.7778(17) ?
U1 O5 7_556 2.3107(17) ?
U1 O4 7_556 2.3431(16) ?
U1 O3 . 2.3680(17) ?
U1 O8 . 2.4214(17) ?
U1 O7 . 2.5071(17) ?
Ag1 N1 . 2.167(3) ?
Ag1 O6 5_666 2.3389(17) ?
Ag1 C9 . 2.367(2) ?
Ag1 C10 . 2.464(2) ?
Ag1 O9 . 2.493(9) ?
O3 C3 . 1.256(3) ?
O4 C3 . 1.272(3) ?
O5 C4 . 1.281(3) ?
O6 C4 . 1.240(3) ?
O7 C20 . 1.267(3) ?
O8 C20 . 1.269(3) ?
N1 C28 . 1.132(5) ?
C1 C3 . 1.519(3) ?
C1 C5 . 1.559(3) ?
C1 C2 . 1.563(3) ?
C1 H1 . 1.000000 ?
C2 C4 . 1.523(3) ?
C2 C6 . 1.564(3) ?
C2 H2 . 1.000000 ?
C5 C13 . 1.514(3) ?
C5 C7 . 1.516(3) ?
C5 H5 . 1.000000 ?
C6 C14 . 1.514(3) ?
C6 C8 . 1.515(3) ?
C6 H6 . 1.000000 ?
C7 C8 . 1.396(3) ?
C7 C12 . 1.397(3) ?
C8 C9 . 1.407(3) ?
C9 C10 . 1.413(3) ?
C9 H9 . 0.950000 ?
C10 C11 . 1.401(3) ?
C10 H10 . 0.950000 ?
C11 C12 . 1.389(3) ?
C11 H11 . 0.950000 ?
C12 H12 . 0.950000 ?
C13 C18 . 1.390(3) ?
C13 C14 . 1.401(3) ?
C14 C15 . 1.391(3) ?
C15 C16 . 1.400(4) ?
C15 H15 . 0.950000 ?
C16 C17 . 1.393(4) ?
C16 H16 . 0.950000 ?
C17 C18 . 1.398(4) ?
C17 H17 . 0.950000 ?
C18 H18 . 0.950000 ?
C19 C20 . 1.517(3) ?
C19 C19 2_556 1.543(4) ?
C19 C21 . 1.572(3) ?
C19 H19 . 1.000000 ?
C21 C23 2_556 1.511(3) ?
C21 C22 . 1.514(3) ?
C21 H21 . 1.000000 ?
C22 C27 . 1.392(3) ?
C22 C23 . 1.403(3) ?
C23 C24 . 1.389(3) ?
C24 C25 . 1.397(4) ?
C24 H24 . 0.950000 ?
C25 C26 . 1.388(4) ?
C25 H25 . 0.950000 ?
C26 C27 . 1.397(4) ?
C26 H26 . 0.950000 ?
C27 H27 . 0.950000 ?
C28 C29 . 1.448(4) ?
C29 H29A . 0.980000 ?
C29 H29B . 0.980000 ?
C29 H29C . 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 . . 179.52(8) ?
O2 U1 O5 . 7_556 88.19(7) ?
O1 U1 O5 . 7_556 91.36(7) ?
O2 U1 O4 . 7_556 90.41(7) ?
O1 U1 O4 . 7_556 89.34(7) ?
O5 U1 O4 7_556 7_556 78.59(6) ?
O2 U1 O3 . . 89.69(7) ?
O1 U1 O3 . . 90.67(7) ?
O5 U1 O3 7_556 . 157.13(6) ?
O4 U1 O3 7_556 . 78.65(6) ?
O2 U1 O8 . . 90.52(7) ?
O1 U1 O8 . . 89.89(7) ?
O5 U1 O8 7_556 . 127.40(6) ?
O4 U1 O8 7_556 . 154.01(6) ?
O3 U1 O8 . . 75.38(6) ?
O2 U1 O7 . . 88.93(7) ?
O1 U1 O7 . . 91.10(7) ?
O5 U1 O7 7_556 . 74.52(6) ?
O4 U1 O7 7_556 . 153.11(6) ?
O3 U1 O7 . . 128.22(6) ?
O8 U1 O7 . . 52.88(5) ?
N1 Ag1 O6 . 5_666 87.29(10) ?
N1 Ag1 C9 . . 169.97(12) ?
O6 Ag1 C9 5_666 . 101.93(7) ?
N1 Ag1 C10 . . 136.73(11) ?
O6 Ag1 C10 5_666 . 135.87(7) ?
C9 Ag1 C10 . . 33.94(8) ?
N1 Ag1 O9 . . 68.0(3) ?
O6 Ag1 O9 5_666 . 99.5(3) ?
C9 Ag1 O9 . . 106.1(2) ?
C10 Ag1 O9 . . 96.2(3) ?
C3 O3 U1 . . 135.06(15) ?
C3 O4 U1 . 7_556 130.49(15) ?
C4 O5 U1 . 7_556 149.53(15) ?
C4 O6 Ag1 . 5_666 117.58(15) ?
C20 O7 U1 . . 91.45(13) ?
C20 O8 U1 . . 95.39(13) ?
C28 N1 Ag1 . . 154.8(3) ?
C3 C1 C5 . . 113.01(18) ?
C3 C1 C2 . . 113.17(18) ?
C5 C1 C2 . . 109.47(17) ?
C3 C1 H1 . . 106.900000 ?
C5 C1 H1 . . 106.900000 ?
C2 C1 H1 . . 106.900000 ?
C4 C2 C1 . . 113.49(18) ?
C4 C2 C6 . . 112.31(18) ?
C1 C2 C6 . . 109.18(17) ?
C4 C2 H2 . . 107.200000 ?
C1 C2 H2 . . 107.200000 ?
C6 C2 H2 . . 107.200000 ?
O3 C3 O4 . . 123.8(2) ?
O3 C3 C1 . . 118.3(2) ?
O4 C3 C1 . . 117.90(19) ?
O6 C4 O5 . . 123.1(2) ?
O6 C4 C2 . . 119.8(2) ?
O5 C4 C2 . . 117.03(19) ?
C13 C5 C7 . . 108.65(18) ?
C13 C5 C1 . . 104.00(17) ?
C7 C5 C1 . . 107.08(18) ?
C13 C5 H5 . . 112.200000 ?
C7 C5 H5 . . 112.200000 ?
C1 C5 H5 . . 112.200000 ?
C14 C6 C8 . . 108.18(18) ?
C14 C6 C2 . . 106.79(18) ?
C8 C6 C2 . . 104.37(17) ?
C14 C6 H6 . . 112.300000 ?
C8 C6 H6 . . 112.300000 ?
C2 C6 H6 . . 112.300000 ?
C8 C7 C12 . . 120.6(2) ?
C8 C7 C5 . . 113.14(19) ?
C12 C7 C5 . . 126.2(2) ?
C7 C8 C9 . . 120.4(2) ?
C7 C8 C6 . . 113.9(2) ?
C9 C8 C6 . . 125.7(2) ?
C8 C9 C10 . . 118.7(2) ?
C8 C9 Ag1 . . 102.24(15) ?
C10 C9 Ag1 . . 76.78(14) ?
C8 C9 H9 . . 120.700000 ?
C10 C9 H9 . . 120.700000 ?
Ag1 C9 H9 . . 90.900000 ?
C11 C10 C9 . . 120.1(2) ?
C11 C10 Ag1 . . 105.85(16) ?
C9 C10 Ag1 . . 69.28(13) ?
C11 C10 H10 . . 119.900000 ?
C9 C10 H10 . . 119.900000 ?
Ag1 C10 H10 . . 94.600000 ?
C12 C11 C10 . . 120.6(2) ?
C12 C11 H11 . . 119.700000 ?
C10 C11 H11 . . 119.700000 ?
C11 C12 C7 . . 119.5(2) ?
C11 C12 H12 . . 120.200000 ?
C7 C12 H12 . . 120.200000 ?
C18 C13 C14 . . 120.5(2) ?
C18 C13 C5 . . 125.9(2) ?
C14 C13 C5 . . 113.5(2) ?
C15 C14 C13 . . 120.3(2) ?
C15 C14 C6 . . 126.2(2) ?
C13 C14 C6 . . 113.40(19) ?
C14 C15 C16 . . 119.0(2) ?
C14 C15 H15 . . 120.500000 ?
C16 C15 H15 . . 120.500000 ?
C17 C16 C15 . . 120.8(2) ?
C17 C16 H16 . . 119.600000 ?
C15 C16 H16 . . 119.600000 ?
C16 C17 C18 . . 120.0(2) ?
C16 C17 H17 . . 120.000000 ?
C18 C17 H17 . . 120.000000 ?
C13 C18 C17 . . 119.4(2) ?
C13 C18 H18 . . 120.300000 ?
C17 C18 H18 . . 120.300000 ?
C20 C19 C19 . 2_556 115.5(2) ?
C20 C19 C21 . . 108.29(17) ?
C19 C19 C21 2_556 . 109.33(11) ?
C20 C19 H19 . . 107.800000 ?
C19 C19 H19 2_556 . 107.800000 ?
C21 C19 H19 . . 107.800000 ?
O7 C20 O8 . . 120.0(2) ?
O7 C20 C19 . . 122.5(2) ?
O8 C20 C19 . . 117.52(19) ?
C23 C21 C22 2_556 . 109.48(19) ?
C23 C21 C19 2_556 . 105.11(18) ?
C22 C21 C19 . . 106.04(18) ?
C23 C21 H21 2_556 . 111.900000 ?
C22 C21 H21 . . 111.900000 ?
C19 C21 H21 . . 111.900000 ?
C27 C22 C23 . . 120.1(2) ?
C27 C22 C21 . . 126.8(2) ?
C23 C22 C21 . . 113.1(2) ?
C24 C23 C22 . . 120.5(2) ?
C24 C23 C21 . 2_556 126.4(2) ?
C22 C23 C21 . 2_556 113.0(2) ?
C23 C24 C25 . . 119.4(2) ?
C23 C24 H24 . . 120.300000 ?
C25 C24 H24 . . 120.300000 ?
C26 C25 C24 . . 120.0(3) ?
C26 C25 H25 . . 120.000000 ?
C24 C25 H25 . . 120.000000 ?
C25 C26 C27 . . 121.0(2) ?
C25 C26 H26 . . 119.500000 ?
C27 C26 H26 . . 119.500000 ?
C22 C27 C26 . . 118.9(2) ?
C22 C27 H27 . . 120.500000 ?
C26 C27 H27 . . 120.500000 ?
N1 C28 C29 . . 178.9(5) ?
C28 C29 H29A . . 109.500000 ?
C28 C29 H29B . . 109.500000 ?
H29A C29 H29B . . 109.500000 ?
C28 C29 H29C . . 109.500000 ?
H29A C29 H29C . . 109.500000 ?
H29B C29 H29C . . 109.500000 ?

