# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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 2105578'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2021-08-26 deposited with the CCDC.	2021-10-04 downloaded from the CCDC.
;

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H13 N3 O10 U2'
_chemical_formula_iupac          ?
_chemical_formula_weight         895.36
_chemical_absolute_configuration ?

_chemical_melting_point          ?

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_cell_length_a                   8.1750(4)
_cell_length_b                   11.2250(5)
_cell_length_c                   12.1741(5)
_cell_angle_alpha                76.648(2)
_cell_angle_beta                 86.085(2)
_cell_angle_gamma                70.908(2)
_cell_volume                     1027.13(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    648
_cell_measurement_theta_min      1.9189
_cell_measurement_theta_max      19.7800
_cell_measurement_temperature    293(2)

_exptl_crystal_description       irregular
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.088
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.059
_exptl_crystal_density_diffrn    2.895
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             800

_exptl_absorpt_coefficient_mu    15.809
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_T_max  0.75

_exptl_special_details           
;
;

_diffrn_ambient_temperature      293(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            67332
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_theta_min         1.97
_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       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14

_refine_special_details          
;
The H atoms bound to O9 and O10 were found and fully
refined with a restraint on the bond length.
;

_reflns_number_total             3890
_reflns_number_gt                3201
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0252
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0630
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_restrained_S_all      1.157
_refine_ls_number_reflns         3890
_refine_ls_number_parameters     297
_refine_ls_number_restraints     2
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0147P)²+8.8556P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.827
_refine_diff_density_min         -1.095
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
;
_refine_ls_abs_structure_Flack   .

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 vV6.2.14'
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_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 0.93046(3) 0.44914(2) 0.87429(2) 0.02302(9) Uani d . . . 1 . .
U U2 1.24758(4) 0.20671(2) 0.66949(2) 0.02412(9) Uani d . . . 1 . .
O O1 0.9148(8) 0.6037(5) 0.7903(5) 0.0378(14) Uani d . . . 1 . .
O O2 0.9495(7) 0.2926(5) 0.9580(5) 0.0369(14) Uani d . . . 1 . .
O O3 1.3874(8) 0.2751(5) 0.5774(5) 0.0391(14) Uani d . . . 1 . .
O O4 1.1113(7) 0.1348(5) 0.7603(5) 0.0330(13) Uani d . . . 1 . .
O O5 0.6236(7) 0.4905(5) 0.8816(4) 0.0294(12) Uani d . . . 1 . .
O O6 0.3874(8) 0.5146(5) 0.7899(5) 0.0429(15) Uani d . . . 1 . .
O O7 0.8260(8) 0.4174(8) 0.7021(6) 0.060(2) Uani d . . . 1 . .
O O8 0.9994(8) 0.3487(6) 0.5661(5) 0.0454(16) Uani d . . . 1 . .
O O9 1.1858(7) 0.3615(5) 0.7684(5) 0.0313(12) Uani d . . D 1 . .
H H9 1.227(10) 0.422(5) 0.757(7) 0.03(2) Uiso d . . D 1 . .
O O10 1.1633(7) 0.4514(5) 0.9736(5) 0.0288(12) Uani d . . D 1 . .
H H10 1.211(11) 0.498(8) 0.929(6) 0.05(3) Uiso d . . D 1 . .
N N1 0.5018(8) 1.1055(5) 0.8083(5) 0.0237(13) Uani d . . . 1 . .
N N2 0.4143(8) 0.9615(6) 0.6911(5) 0.0237(13) Uani d . . . 1 . .
N N3 0.2142(9) 1.0992(6) 0.5099(5) 0.0298(15) Uani d . . . 1 . .
C C1 0.5032(9) 0.8976(6) 0.7869(6) 0.0214(15) Uani d . . . 1 . .
C C2 0.5357(10) 0.7669(7) 0.8293(6) 0.0252(16) Uani d . . . 1 . .
H H2 0.599684 0.72572 0.895561 0.03 Uiso calc U . R 1 . .
C C3 0.4719(9) 0.6974(7) 0.7719(6) 0.0239(16) Uani d . . . 1 . .
C C4 0.3834(10) 0.7622(7) 0.6724(7) 0.0279(17) Uani d . . . 1 . .
H H4 0.341654 0.717904 0.631203 0.033 Uiso calc U . R 1 . .
C C5 0.3560(9) 0.8941(7) 0.6332(6) 0.0245(16) Uani d . . . 1 . .
C C6 0.4955(10) 0.5561(7) 0.8173(7) 0.0287(17) Uani d . . . 1 . .
C C7 0.5695(9) 0.9769(7) 0.8439(6) 0.0233(15) Uani d . . . 1 . .
C C8 0.7008(10) 0.9203(7) 0.9239(6) 0.0281(17) Uani d . . . 1 . .
H H8 0.744035 0.830875 0.947798 0.034 Uiso calc U . R 1 . .
C C9 0.7668(11) 0.9983(8) 0.9678(7) 0.0345(19) Uani d . . . 1 . .
H H9A 0.855483 0.961819 1.021292 0.041 Uiso calc U . R 1 . .
C C10 0.6993(11) 1.1318(8) 0.9312(7) 0.0334(18) Uani d . . . 1 . .
H H10A 0.742714 1.186246 0.958775 0.04 Uiso calc U . R 1 . .
C C11 0.5658(11) 1.1813(7) 0.8528(7) 0.0325(18) Uani d . . . 1 . .
H H11 0.517797 1.270584 0.829593 0.039 Uiso calc U . R 1 . .
C C12 0.2614(9) 0.9693(7) 0.5264(6) 0.0237(15) Uani d . . . 1 . .
C C13 0.2257(10) 0.9112(7) 0.4460(7) 0.0291(17) Uani d . . . 1 . .
H H13 0.26098 0.821555 0.457743 0.035 Uiso calc U . R 1 . .
C C14 0.1386(10) 0.9865(8) 0.3497(7) 0.0328(18) Uani d . . . 1 . .
H H14 0.108399 0.948729 0.297149 0.039 Uiso calc U . R 1 . .
C C15 0.0952(10) 1.1199(8) 0.3307(6) 0.0317(18) Uani d . . . 1 . .
H H15 0.041134 1.173023 0.263891 0.038 Uiso calc U . R 1 . .
C C16 0.1346(10) 1.1708(7) 0.4135(6) 0.0295(17) Uani d . . . 1 . .
H H16 0.104136 1.260214 0.401732 0.035 Uiso calc U . R 1 . .
C C17 0.8581(13) 0.4081(10) 0.6045(8) 0.051(3) Uani d . . . 1 . .
H H17 0.767369 0.449886 0.552929 0.062 Uiso calc U . R 1 . .


_geom_special_details            
;

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
U1 O1 . 1.768(5) ?
U1 O2 . 1.780(5) ?
U1 O10 . 2.334(5) ?
U1 O10 2_767 2.337(5) ?
U1 O5 . 2.396(5) ?
U1 O9 . 2.421(5) ?
U1 O7 . 2.457(6) ?
U1 U1 2_767 3.8605(5) ?
U2 O4 . 1.767(5) ?
U2 O3 . 1.776(6) ?
U2 O9 . 2.244(5) ?
U2 O8 . 2.355(6) ?
U2 N1 1_645 2.552(6) ?
U2 N3 1_645 2.583(6) ?
U2 N2 1_645 2.601(6) ?
O5 C6 . 1.262(9) ?
O6 C6 . 1.221(9) ?
O7 C17 . 1.220(11) ?
O8 C17 . 1.251(11) ?
O9 H9 . 0.838(10) ?
O10 H10 . 0.838(10) ?
N1 C7 . 1.341(9) ?
N1 C11 . 1.354(9) ?
N2 C1 . 1.338(9) ?
N2 C5 . 1.350(9) ?
N3 C16 . 1.332(10) ?
N3 C12 . 1.351(9) ?
C1 C2 . 1.379(10) ?
C1 C7 . 1.489(9) ?
C2 C3 . 1.392(10) ?
C2 H2 . 0.93 ?
C3 C4 . 1.374(11) ?
C3 C6 . 1.506(10) ?
C4 C5 . 1.394(10) ?
C4 H4 . 0.93 ?
C5 C12 . 1.485(10) ?
C7 C8 . 1.384(10) ?
C8 C9 . 1.381(11) ?
C8 H8 . 0.93 ?
C9 C10 . 1.390(11) ?
C9 H9A . 0.93 ?
C10 C11 . 1.383(11) ?
C10 H10A . 0.93 ?
C11 H11 . 0.93 ?
C12 C13 . 1.388(10) ?
C13 C14 . 1.364(11) ?
C13 H13 . 0.93 ?
C14 C15 . 1.387(11) ?
C14 H14 . 0.93 ?
C15 C16 . 1.370(11) ?
C15 H15 . 0.93 ?
C16 H16 . 0.93 ?
C17 H17 . 0.93 ?

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 . . 179.1(3) ?
O1 U1 O10 . . 90.3(2) ?
O2 U1 O10 . . 89.3(2) ?
O1 U1 O10 . 2_767 87.6(2) ?
O2 U1 O10 . 2_767 93.0(2) ?
O10 U1 O10 . 2_767 68.5(2) ?
O1 U1 O5 . . 94.2(2) ?
O2 U1 O5 . . 86.7(2) ?
O10 U1 O5 . . 142.77(18) ?
O10 U1 O5 2_767 . 74.73(18) ?
O1 U1 O9 . . 88.0(2) ?
O2 U1 O9 . . 91.2(2) ?
O10 U1 O9 . . 74.41(18) ?
O10 U1 O9 2_767 . 142.64(18) ?
O5 U1 O9 . . 142.61(18) ?
O1 U1 O7 . . 83.6(3) ?
O2 U1 O7 . . 96.4(3) ?
O10 U1 O7 . . 147.8(2) ?
O10 U1 O7 2_767 . 142.2(2) ?
O5 U1 O7 . . 69.4(2) ?
O9 U1 O7 . . 73.8(2) ?
O4 U2 O3 . . 178.5(2) ?
O4 U2 O9 . . 88.8(2) ?
O3 U2 O9 . . 92.5(2) ?
O4 U2 O8 . . 88.3(2) ?
O3 U2 O8 . . 92.4(3) ?
O9 U2 O8 . . 82.6(2) ?
O4 U2 N1 . 1_645 93.1(2) ?
O3 U2 N1 . 1_645 86.6(2) ?
O9 U2 N1 . 1_645 81.42(19) ?
O8 U2 N1 . 1_645 163.97(19) ?
O4 U2 N3 . 1_645 92.2(2) ?
O3 U2 N3 . 1_645 86.8(2) ?
O9 U2 N3 . 1_645 156.7(2) ?
O8 U2 N3 . 1_645 74.1(2) ?
N1 U2 N3 1_645 1_645 121.71(19) ?
O4 U2 N2 . 1_645 77.9(2) ?
O3 U2 N2 . 1_645 100.7(2) ?
O9 U2 N2 . 1_645 140.2(2) ?
O8 U2 N2 . 1_645 133.3(2) ?
N1 U2 N2 1_645 1_645 62.37(18) ?
N3 U2 N2 1_645 1_645 62.30(19) ?
C6 O5 U1 . . 136.5(5) ?
C17 O7 U1 . . 145.9(7) ?
C17 O8 U2 . . 127.3(6) ?
U2 O9 U1 . . 130.7(2) ?
U2 O9 H9 . . 126.(6) ?
U1 O9 H9 . . 100.(6) ?
U1 O10 U1 . 2_767 111.5(2) ?
U1 O10 H10 . . 106.(7) ?
U1 O10 H10 2_767 . 106.(7) ?
C7 N1 C11 . . 118.2(6) ?
C7 N1 U2 . 1_465 121.4(4) ?
C11 N1 U2 . 1_465 120.3(5) ?
C1 N2 C5 . . 118.2(6) ?
C1 N2 U2 . 1_465 118.0(4) ?
C5 N2 U2 . 1_465 118.3(5) ?
C16 N3 C12 . . 118.3(6) ?
C16 N3 U2 . 1_465 120.5(5) ?
C12 N3 U2 . 1_465 120.8(5) ?
N2 C1 C2 . . 122.9(7) ?
N2 C1 C7 . . 115.3(6) ?
C2 C1 C7 . . 121.8(7) ?
C1 C2 C3 . . 119.3(7) ?
C1 C2 H2 . . 120.3 ?
C3 C2 H2 . . 120.3 ?
C4 C3 C2 . . 117.9(6) ?
C4 C3 C6 . . 120.4(6) ?
C2 C3 C6 . . 121.7(7) ?
C3 C4 C5 . . 120.1(7) ?
C3 C4 H4 . . 119.9 ?
C5 C4 H4 . . 119.9 ?
N2 C5 C4 . . 121.5(7) ?
N2 C5 C12 . . 115.9(6) ?
C4 C5 C12 . . 122.6(7) ?
O6 C6 O5 . . 125.2(7) ?
O6 C6 C3 . . 117.1(7) ?
O5 C6 C3 . . 117.6(7) ?
N1 C7 C8 . . 122.2(6) ?
N1 C7 C1 . . 116.1(6) ?
C8 C7 C1 . . 121.5(6) ?
C9 C8 C7 . . 119.2(7) ?
C9 C8 H8 . . 120.4 ?
C7 C8 H8 . . 120.4 ?
C8 C9 C10 . . 119.3(7) ?
C8 C9 H9A . . 120.3 ?
C10 C9 H9A . . 120.3 ?
C11 C10 C9 . . 118.1(7) ?
C11 C10 H10A . . 120.9 ?
C9 C10 H10A . . 120.9 ?
N1 C11 C10 . . 122.8(7) ?
N1 C11 H11 . . 118.6 ?
C10 C11 H11 . . 118.6 ?
N3 C12 C13 . . 121.1(7) ?
N3 C12 C5 . . 116.1(6) ?
C13 C12 C5 . . 122.8(7) ?
C14 C13 C12 . . 119.5(7) ?
C14 C13 H13 . . 120.3 ?
C12 C13 H13 . . 120.3 ?
C13 C14 C15 . . 119.5(7) ?
C13 C14 H14 . . 120.2 ?
C15 C14 H14 . . 120.2 ?
C16 C15 C14 . . 117.8(7) ?
C16 C15 H15 . . 121.1 ?
C14 C15 H15 . . 121.1 ?
N3 C16 C15 . . 123.6(7) ?
N3 C16 H16 . . 118.2 ?
C15 C16 H16 . . 118.2 ?
O7 C17 O8 . . 127.3(9) ?
O7 C17 H17 . . 116.4 ?
O8 C17 H17 . . 116.4 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O9 H9 O6 1_655 0.838(10) 2.02(4) 2.802(7) 155(8) ?
O10 H10 O6 1_655 0.838(10) 2.16(5) 2.901(8) 148(9) ?
C2 H2 O10 2_767 0.93 2.59 3.459(9) 156.6 ?
C10 H10A O2 1_565 0.93 2.37 3.214(10) 151.5 ?
C11 H11 O6 1_565 0.93 2.53 3.459(9) 173.5 ?
C15 H15 O1 2_676 0.93 2.58 3.089(10) 115.1 ?
C16 H16 O1 2_676 0.93 2.46 3.048(9) 121.0 ?
C16 H16 O8 1_465 0.93 2.42 2.941(9) 115.4 ?


####################################################################### 
# 
# 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 2105579'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2021-08-26 deposited with the CCDC.	2021-10-04 downloaded from the CCDC.
;

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H17 N3 O11 Pb U'
_chemical_formula_iupac          ?
_chemical_formula_weight         896.57
_chemical_absolute_configuration ?

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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                   10.4295(5)
_cell_length_b                   10.5028(6)
_cell_length_c                   11.5621(6)
_cell_angle_alpha                63.375(2)
_cell_angle_beta                 74.261(2)
_cell_angle_gamma                80.690(2)
_cell_volume                     1088.56(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    667
_cell_measurement_theta_min      2.0155
_cell_measurement_theta_max      24.1853
_cell_measurement_temperature    100(2)

_exptl_crystal_description       irregular
_exptl_crystal_colour            'translucent intense yellow'
_exptl_crystal_size_max          0.109
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.057
_exptl_crystal_density_diffrn    2.735
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816

_exptl_absorpt_coefficient_mu    15.219
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_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            74394
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14

_refine_special_details          
;
Two water molecules (O11 and O12) were given occupancy 
parameters of 0.5 in order to retain acceptable 
displacement parameters. The H atoms bound to O9, O10
and O12 were found and refined with restraints, but not
those of O11.
;

_reflns_number_total             4133
_reflns_number_gt                3998
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0203
_refine_ls_wR_factor_gt          0.0466
_refine_ls_wR_factor_ref         0.0468
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_restrained_S_all      1.194
_refine_ls_number_reflns         4133
_refine_ls_number_parameters     332
_refine_ls_number_restraints     13
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+6.8950P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.971
_refine_diff_density_min         -1.054
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

# start Validation Reply Form
_vrf_PLAT430_2                   
;
PROBLEM: Short Inter D...A Contact  O2       ..O11      .       2.78 Ang. and
	  Short Inter D...A Contact  O8       ..O11      .       2.55 Ang. 

RESPONSE: This short contact is indicative of hydrogen bonding
involving a water molecule (O11) for which the H atoms were not found.
;
# end Validation Reply Form

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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'Bruker Instrument Service vV6.2.14'
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_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 0.44756(2) 0.90489(2) 0.91116(2) 0.01251(6) Uani d . . . 1 . .
Pb Pb1 0.22507(2) 0.80215(2) 0.61246(2) 0.01967(6) Uani d . . . 1 . .
O O1 0.5382(3) 0.7413(4) 0.9906(3) 0.0181(7) Uani d . . . 1 . .
O O2 0.3551(3) 1.0622(4) 0.8200(3) 0.0214(7) Uani d . . . 1 . .
O O3 -0.2477(3) 0.2154(4) 0.9461(3) 0.0187(7) Uani d . . . 1 . .
O O4 -0.1586(3) 0.1816(3) 0.7624(3) 0.0164(7) Uani d . . . 1 . .
O O5 0.3698(3) 0.7899(3) 0.8029(3) 0.0166(7) Uani d . . . 1 . .
O O6 0.3224(3) 0.6038(3) 0.7839(3) 0.0181(7) Uani d . . . 1 . .
O O7 0.6070(3) 0.9415(4) 0.7053(3) 0.0194(7) Uani d . . . 1 . .
O O8 0.7769(5) 0.8467(5) 0.6009(5) 0.0470(12) Uani d . . . 1 . .
O O9 0.6029(3) 1.0405(4) 0.9069(3) 0.0205(7) Uani d . . D 1 . .
H H9 0.668(4) 1.075(7) 0.844(4) 0.038(18) Uiso d . . D 1 . .
O O10 0.0508(4) 0.8722(4) 0.4616(4) 0.0250(8) Uani d . . D 1 . .
H H10A -0.028(2) 0.853(7) 0.502(5) 0.037 Uiso d U . D 1 . .
H H10B 0.070(5) 0.845(7) 0.401(4) 0.037 Uiso d U . D 1 . .
O O11 0.2035(7) 1.1091(7) 0.6389(7) 0.0217(14) Uani d . P . 0.5 . .
O O12 0.5129(7) 0.8669(8) 0.5095(7) 0.0254(16) Uani d U P D 0.5 . .
H H12A 0.592(5) 0.858(11) 0.471(10) 0.038 Uiso d U P D 0.5 . .
H H12B 0.487(10) 0.952(4) 0.470(10) 0.038 Uiso d U P D 0.5 . .
N N1 0.3032(4) 0.6395(4) 0.4999(4) 0.0178(8) Uani d . . . 1 . .
N N2 0.0836(4) 0.5916(4) 0.6996(4) 0.0121(7) Uani d . . . 1 . .
N N3 0.0385(4) 0.7750(4) 0.8132(4) 0.0173(8) Uani d . . . 1 . .
C C1 -0.0793(4) 0.3662(5) 0.7864(4) 0.0118(8) Uani d . . . 1 . .
C C2 0.0302(4) 0.3896(5) 0.6801(4) 0.0138(9) Uani d . . . 1 . .
H H2 0.049993 0.329075 0.635746 0.017 Uiso calc U . R 1 . .
C C3 0.1106(4) 0.5029(5) 0.6393(4) 0.0129(8) Uani d . . . 1 . .
C C4 -0.0221(4) 0.5691(5) 0.8032(4) 0.0122(8) Uani d . . . 1 . .
C C5 -0.1047(4) 0.4575(5) 0.8479(4) 0.0135(9) Uani d . . . 1 . .
H H5 -0.178776 0.443629 0.920889 0.016 Uiso calc U . R 1 . .
C C6 -0.1687(4) 0.2447(5) 0.8337(4) 0.0135(9) Uani d . . . 1 . .
C C7 0.2298(4) 0.5319(5) 0.5269(4) 0.0141(9) Uani d . . . 1 . .
C C8 0.2627(5) 0.4532(5) 0.4527(5) 0.0197(10) Uani d . . . 1 . .
H H8 0.209533 0.377606 0.47245 0.024 Uiso calc U . R 1 . .
C C9 0.3747(5) 0.4870(6) 0.3494(5) 0.0245(11) Uani d . . . 1 . .
H H9A 0.398791 0.434341 0.297369 0.029 Uiso calc U . R 1 . .
C C10 0.4506(5) 0.5955(6) 0.3219(5) 0.0231(11) Uani d . . . 1 . .
H H10 0.528034 0.618808 0.251556 0.028 Uiso calc U . R 1 . .
C C11 0.4123(5) 0.6705(5) 0.3985(5) 0.0214(10) Uani d . . . 1 . .
H H11 0.464332 0.746741 0.379431 0.026 Uiso calc U . R 1 . .
C C12 -0.0461(4) 0.6695(5) 0.8671(4) 0.0136(9) Uani d . . . 1 . .
C C13 -0.1502(5) 0.6560(5) 0.9744(5) 0.0174(9) Uani d . . . 1 . .
H H13 -0.207983 0.579305 1.012174 0.021 Uiso calc U . R 1 . .
C C14 -0.1701(5) 0.7554(5) 1.0271(5) 0.0188(10) Uani d . . . 1 . .
H H14 -0.241974 0.748224 1.100388 0.023 Uiso calc U . R 1 . .
C C15 -0.0835(5) 0.8646(5) 0.9709(5) 0.0213(10) Uani d . . . 1 . .
H H15 -0.094835 0.934207 1.004642 0.026 Uiso calc U . R 1 . .
C C16 0.0203(5) 0.8710(5) 0.8643(5) 0.0215(10) Uani d . . . 1 . .
H H16 0.080671 0.945511 0.826049 0.026 Uiso calc U . R 1 . .
C C17 0.3735(4) 0.6588(5) 0.8349(4) 0.0158(9) Uani d . . . 1 . .
H H17 0.418654 0.597247 0.902731 0.019 Uiso calc U . R 1 . .
C C18 0.7224(5) 0.8857(6) 0.6881(5) 0.0282(12) Uani d . . . 1 . .
H H18 0.773066 0.872306 0.750032 0.034 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 . 1.794(3) ?
U1 O2 . 1.802(3) ?
U1 O9 . 2.301(3) ?
U1 O9 2_677 2.327(3) ?
U1 O3 2_567 2.405(3) ?
U1 O7 . 2.411(3) ?
U1 O5 . 2.430(3) ?
U1 U1 2_677 3.8746(3) ?
Pb1 O6 . 2.451(3) ?
Pb1 N1 . 2.498(4) ?
Pb1 N2 . 2.517(4) ?
Pb1 N3 . 2.528(4) ?
Pb1 O10 . 2.650(4) ?
Pb1 O5 . 2.938(3) ?
Pb1 O12 . 2.982(7) ?
Pb1 O11 . 3.339(7) ?
Pb1 O8 2_676 3.397(5) ?
O3 C6 . 1.267(6) ?
O4 C6 . 1.245(5) ?
O5 C17 . 1.252(6) ?
O6 C17 . 1.241(6) ?
O7 C18 . 1.257(6) ?
O8 C18 . 1.222(7) ?
O9 H9 . 0.835(10) ?
O10 H10A . 0.835(10) ?
O10 H10B . 0.835(10) ?
O12 H12A . 0.837(10) ?
O12 H12B . 0.836(10) ?
N1 C7 . 1.341(6) ?
N1 C11 . 1.352(6) ?
N2 C3 . 1.351(6) ?
N2 C4 . 1.349(6) ?
N3 C12 . 1.339(6) ?
N3 C16 . 1.347(6) ?
C1 C5 . 1.386(6) ?
C1 C2 . 1.390(6) ?
C1 C6 . 1.511(6) ?
C2 C3 . 1.395(6) ?
C2 H2 . 0.95 ?
C3 C7 . 1.489(6) ?
C4 C5 . 1.387(6) ?
C4 C12 . 1.494(6) ?
C5 H5 . 0.95 ?
C7 C8 . 1.385(7) ?
C8 C9 . 1.384(7) ?
C8 H8 . 0.95 ?
C9 C10 . 1.362(8) ?
C9 H9A . 0.95 ?
C10 C11 . 1.377(8) ?
C10 H10 . 0.95 ?
C11 H11 . 0.95 ?
C12 C13 . 1.378(7) ?
C13 C14 . 1.391(7) ?
C13 H13 . 0.95 ?
C14 C15 . 1.379(7) ?
C14 H14 . 0.95 ?
C15 C16 . 1.387(7) ?
C15 H15 . 0.95 ?
C16 H16 . 0.95 ?
C17 H17 . 0.95 ?
C18 H18 . 0.95 ?

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 . . 174.23(15) ?
O1 U1 O9 . . 92.49(14) ?
O2 U1 O9 . . 91.46(14) ?
O1 U1 O9 . 2_677 93.98(14) ?
O2 U1 O9 . 2_677 91.45(14) ?
O9 U1 O9 . 2_677 66.31(13) ?
O1 U1 O3 . 2_567 87.12(13) ?
O2 U1 O3 . 2_567 92.56(14) ?
O9 U1 O3 . 2_567 139.94(11) ?
O9 U1 O3 2_677 2_567 73.75(11) ?
O1 U1 O7 . . 88.48(13) ?
O2 U1 O7 . . 88.31(14) ?
O9 U1 O7 . . 77.02(11) ?
O9 U1 O7 2_677 . 143.31(11) ?
O3 U1 O7 2_567 . 142.92(11) ?
O1 U1 O5 . . 88.12(13) ?
O2 U1 O5 . . 86.33(13) ?
O9 U1 O5 . . 148.87(11) ?
O9 U1 O5 2_677 . 144.72(11) ?
O3 U1 O5 2_567 . 71.19(11) ?
O7 U1 O5 . . 71.88(11) ?
O1 U1 U1 . 2_677 93.87(10) ?
O2 U1 U1 . 2_677 91.74(11) ?
O9 U1 U1 . 2_677 33.37(8) ?
O9 U1 U1 2_677 2_677 32.94(8) ?
O3 U1 U1 2_567 2_677 106.64(8) ?
O7 U1 U1 . 2_677 110.38(8) ?
O5 U1 U1 . 2_677 177.00(8) ?
O6 Pb1 N1 . . 80.34(11) ?
O6 Pb1 N2 . . 72.84(11) ?
N1 Pb1 N2 . . 65.17(12) ?
O6 Pb1 N3 . . 80.69(12) ?
N1 Pb1 N3 . . 129.64(12) ?
N2 Pb1 N3 . . 64.73(12) ?
O6 Pb1 O10 . . 144.35(11) ?
N1 Pb1 O10 . . 78.74(12) ?
N2 Pb1 O10 . . 72.25(12) ?
N3 Pb1 O10 . . 90.89(12) ?
O6 Pb1 O5 . . 47.29(10) ?
N1 Pb1 O5 . . 118.54(11) ?
N2 Pb1 O5 . . 113.45(10) ?
N3 Pb1 O5 . . 77.93(11) ?
O10 Pb1 O5 . . 162.72(10) ?
O6 Pb1 O12 . . 79.18(15) ?
N1 Pb1 O12 . . 80.05(18) ?
N2 Pb1 O12 . . 138.11(18) ?
N3 Pb1 O12 . . 140.01(17) ?
O10 Pb1 O12 . . 124.53(15) ?
O5 Pb1 O12 . . 63.04(15) ?
O6 Pb1 O11 . . 112.96(14) ?
N1 Pb1 O11 . . 155.11(15) ?
N2 Pb1 O11 . . 137.63(14) ?
N3 Pb1 O11 . . 74.66(14) ?
O10 Pb1 O11 . . 97.72(14) ?
O5 Pb1 O11 . . 66.80(13) ?
O12 Pb1 O11 . . 82.0(2) ?
O6 Pb1 O8 . 2_676 148.44(11) ?
N1 Pb1 O8 . 2_676 113.73(12) ?
N2 Pb1 O8 . 2_676 138.39(12) ?
N3 Pb1 O8 . 2_676 106.62(11) ?
O10 Pb1 O8 . 2_676 67.14(12) ?
O5 Pb1 O8 . 2_676 103.19(11) ?
O12 Pb1 O8 . 2_676 75.99(16) ?
O11 Pb1 O8 . 2_676 44.52(14) ?
C6 O3 U1 . 2_567 143.7(3) ?
C17 O5 U1 . . 126.7(3) ?
C17 O5 Pb1 . . 82.3(2) ?
U1 O5 Pb1 . . 150.59(13) ?
C17 O6 Pb1 . . 105.9(3) ?
C18 O7 U1 . . 128.6(3) ?
U1 O9 U1 . 2_677 113.69(13) ?
U1 O9 H9 . . 125.(5) ?
U1 O9 H9 2_677 . 121.(5) ?
Pb1 O10 H10A . . 116.(4) ?
Pb1 O10 H10B . . 117.(4) ?
H10A O10 H10B . . 108.0(18) ?
Pb1 O12 H12A . . 155.(9) ?
Pb1 O12 H12B . . 86.(7) ?
H12A O12 H12B . . 107.4(18) ?
C7 N1 C11 . . 118.8(4) ?
C7 N1 Pb1 . . 121.0(3) ?
C11 N1 Pb1 . . 119.7(3) ?
C3 N2 C4 . . 119.5(4) ?
C3 N2 Pb1 . . 119.8(3) ?
C4 N2 Pb1 . . 120.7(3) ?
C12 N3 C16 . . 119.1(4) ?
C12 N3 Pb1 . . 121.2(3) ?
C16 N3 Pb1 . . 119.7(3) ?
C5 C1 C2 . . 118.4(4) ?
C5 C1 C6 . . 120.7(4) ?
C2 C1 C6 . . 120.9(4) ?
C1 C2 C3 . . 119.3(4) ?
C1 C2 H2 . . 120.3 ?
C3 C2 H2 . . 120.3 ?
N2 C3 C2 . . 121.5(4) ?
N2 C3 C7 . . 117.0(4) ?
C2 C3 C7 . . 121.5(4) ?
N2 C4 C5 . . 121.2(4) ?
N2 C4 C12 . . 117.1(4) ?
C5 C4 C12 . . 121.7(4) ?
C1 C5 C4 . . 120.1(4) ?
C1 C5 H5 . . 119.9 ?
C4 C5 H5 . . 119.9 ?
O4 C6 O3 . . 125.8(4) ?
O4 C6 C1 . . 118.9(4) ?
O3 C6 C1 . . 115.3(4) ?
N1 C7 C8 . . 121.5(4) ?
N1 C7 C3 . . 116.5(4) ?
C8 C7 C3 . . 122.1(4) ?
C7 C8 C9 . . 118.7(5) ?
C7 C8 H8 . . 120.7 ?
C9 C8 H8 . . 120.7 ?
C10 C9 C8 . . 120.3(5) ?
C10 C9 H9A . . 119.8 ?
C8 C9 H9A . . 119.8 ?
C9 C10 C11 . . 118.3(4) ?
C9 C10 H10 . . 120.8 ?
C11 C10 H10 . . 120.8 ?
N1 C11 C10 . . 122.4(5) ?
N1 C11 H11 . . 118.8 ?
C10 C11 H11 . . 118.8 ?
N3 C12 C13 . . 121.6(4) ?
N3 C12 C4 . . 116.2(4) ?
C13 C12 C4 . . 122.2(4) ?
C12 C13 C14 . . 119.6(4) ?
C12 C13 H13 . . 120.2 ?
C14 C13 H13 . . 120.2 ?
C15 C14 C13 . . 118.8(5) ?
C15 C14 H14 . . 120.6 ?
C13 C14 H14 . . 120.6 ?
C14 C15 C16 . . 118.8(4) ?
C14 C15 H15 . . 120.6 ?
C16 C15 H15 . . 120.6 ?
N3 C16 C15 . . 122.2(4) ?
N3 C16 H16 . . 118.9 ?
C15 C16 H16 . . 118.9 ?
O6 C17 O5 . . 124.5(4) ?
O6 C17 H17 . . 117.7 ?
O5 C17 H17 . . 117.7 ?
O8 C18 O7 . . 127.4(6) ?
O8 C18 H18 . . 116.3 ?
O7 C18 H18 . . 116.3 ?

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 H9 O4 1_665 0.835(10) 2.05(3) 2.809(4) 152.(6) ?
O10 H10A O8 1_455 0.835(10) 2.040(16) 2.862(6) 168.(6) ?
O10 H10B O4 2_566 0.835(10) 1.986(17) 2.796(5) 163.(5) ?
O12 H12A O11 2_676 0.837(10) 2.16(3) 2.976(10) 165.(10) ?
O12 H12B O7 2_676 0.836(10) 2.24(10) 2.859(7) 131.(11) ?
O12 H12B O12 2_676 0.836(10) 2.02(9) 2.678(16) 135.(12) ?
C2 H2 O11 1_545 0.95 2.58 3.353(8) 138.6 ?
C11 H11 O12 . 0.95 2.54 3.288(9) 136.1 ?
C13 H13 O6 2_567 0.95 2.41 3.242(6) 145.3 ?
C16 H16 O11 . 0.95 2.27 3.114(8) 147.7 ?


####################################################################### 
# 
# 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 2105580'
loop_
_audit_author_name
_audit_author_address
'Pierre Thuery'
;CEA Saclay
France
;
_audit_update_record             
;
2021-08-26 deposited with the CCDC.	2021-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H26 N7 Ni O12.50 U'
_chemical_formula_weight         1005.34

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'

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

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

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

_cell_length_a                   8.7682(2)
_cell_length_b                   16.9333(5)
_cell_length_c                   28.1757(7)
_cell_angle_alpha                90
_cell_angle_beta                 98.6612(13)
_cell_angle_gamma                90
_cell_volume                     4135.67(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1097
_cell_measurement_theta_min      2.3671
_cell_measurement_theta_max      20.2450

_exptl_crystal_description       lath
_exptl_crystal_colour            'translucent light yellow-orange'
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.046
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_F_000             1948
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_absorpt_coefficient_mu    4.430
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_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_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            210879
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_av_R_equivalents  0.0874
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.893
_diffrn_reflns_theta_max         28.700
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10673
_reflns_number_gt                9652
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'Bruker Instrument Service vV6.2.14'
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_computing_publication_material  ?

_refine_special_details          
;
The H atoms bound to O7, O8 and O12 were found and either
refined with restraints (O7 and O12) or treated as riding
atoms (O8) with isotropic displacement parameters equal to
1.5 times that of the attached O atom. The H atoms bound 
to O13 (affected with an occupancy parameter of 0.5 in 
order to retain an acceptable displacement parameter)
were not found. The SQUEEZE software was used to subtract
the contribution to the structure factors of other, very
badly resolved water molecules. Some restraints on 
displacement parameters have been applied for atoms O6,
O9 and O10, possibly affected by unresolved disorder which
could not be modelled satisfyingly. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0159P)²+25.1130P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10673
_refine_ls_number_parameters     496
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0763
_refine_ls_wR_factor_gt          0.0747
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         2.263
_refine_diff_density_min         -1.705
_refine_diff_density_rms         0.138

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.36800(2) 0.42660(2) 0.45973(2) 0.01298(4) Uani 1 1 d . . . . .
Ni1 Ni 0.02052(6) 0.34388(3) 0.70354(2) 0.01651(10) Uani 1 1 d . . . . .
O1 O 0.3972(3) 0.35191(18) 0.50500(11) 0.0237(6) Uani 1 1 d . . . . .
O2 O 0.3312(3) 0.49653(19) 0.41233(10) 0.0208(6) Uani 1 1 d . . . . .
O3 O 0.1097(3) 0.43689(19) 0.47192(10) 0.0219(6) Uani 1 1 d . . . . .
O4 O -0.1316(3) 0.3931(2) 0.45707(10) 0.0261(6) Uani 1 1 d . . . . .
O5 O 0.0264(4) 0.14247(19) 0.91353(11) 0.0266(7) Uani 1 1 d . U . . .
O6 O 0.1012(8) 0.2580(3) 0.94713(16) 0.0842(17) Uani 1 1 d . U . . .
O7 O 0.6157(3) 0.47647(18) 0.48123(10) 0.0194(6) Uani 1 1 d D . . . .
H7 H 0.690(4) 0.448(3) 0.4767(19) 0.029 Uiso 1 1 d D U . . .
O8 O 0.2121(4) 0.3271(3) 0.40934(16) 0.0534(12) Uani 1 1 d . . . . .
H8A H 0.239155 0.296251 0.388748 0.080 Uiso 1 1 d R U . . .
H8B H 0.151435 0.306491 0.426198 0.080 Uiso 1 1 d R U . . .
O9 O 0.1739(7) 0.2679(4) 0.31740(19) 0.0775(16) Uani 1 1 d . U . . .
O10 O -0.0606(6) 0.2290(3) 0.3307(2) 0.0781(16) Uani 1 1 d . U . . .
O11 O 0.1196(5) 0.1477(3) 0.32380(18) 0.0605(14) Uani 1 1 d . . . . .
O12 O -0.0814(5) 0.3967(3) 0.35920(14) 0.0531(13) Uani 1 1 d D . . . .
H12A H -0.103(9) 0.395(4) 0.3872(11) 0.080 Uiso 1 1 d D U . . .
H12B H -0.075(10) 0.3499(14) 0.350(2) 0.080 Uiso 1 1 d D U . . .
O13 O -0.0161(8) 0.2337(4) 0.4528(3) 0.0342(15) Uani 0.5 1 d . . P . .
N1 N 0.2397(4) 0.3952(2) 0.70027(12) 0.0183(6) Uani 1 1 d . . . . .
N2 N 0.0006(4) 0.3736(2) 0.63467(11) 0.0159(6) Uani 1 1 d . . . . .
N3 N -0.2088(4) 0.3088(2) 0.67736(12) 0.0164(6) Uani 1 1 d . . . . .
N4 N -0.0508(4) 0.4426(2) 0.74018(12) 0.0205(7) Uani 1 1 d . . . . .
N5 N 0.0437(4) 0.3048(2) 0.77085(12) 0.0206(7) Uani 1 1 d . . . . .
N6 N 0.1033(4) 0.2278(2) 0.69619(13) 0.0214(7) Uani 1 1 d . . . . .
N7 N 0.0662(7) 0.2143(3) 0.32200(17) 0.0499(13) Uani 1 1 d . . . . .
C1 C 0.3564(5) 0.4068(3) 0.73620(15) 0.0217(8) Uani 1 1 d . . . . .
H1 H 0.347046 0.387545 0.767295 0.026 Uiso 1 1 calc R U . . .
C2 C 0.4907(5) 0.4462(3) 0.72947(15) 0.0228(8) Uani 1 1 d . . . . .
H2 H 0.571474 0.453778 0.755579 0.027 Uiso 1 1 calc R U . . .
C3 C 0.5050(5) 0.4743(3) 0.68416(15) 0.0224(8) Uani 1 1 d . . . . .
H3 H 0.595573 0.501624 0.678879 0.027 Uiso 1 1 calc R U . . .
C4 C 0.3859(4) 0.4620(3) 0.64666(14) 0.0198(8) Uani 1 1 d . . . . .
H4 H 0.393665 0.480450 0.615274 0.024 Uiso 1 1 calc R U . . .
C5 C 0.2541(4) 0.4219(2) 0.65581(13) 0.0180(7) Uani 1 1 d . . . . .
C6 C 0.1233(4) 0.4041(2) 0.61794(13) 0.0164(7) Uani 1 1 d . . . . .
C7 C 0.1235(4) 0.4157(2) 0.56957(14) 0.0191(8) Uani 1 1 d . . . . .
H7A H 0.210530 0.438112 0.558168 0.023 Uiso 1 1 calc R U . . .
C8 C -0.0072(4) 0.3938(2) 0.53773(14) 0.0179(7) Uani 1 1 d . . . . .
C9 C -0.1322(4) 0.3600(2) 0.55520(14) 0.0174(7) Uani 1 1 d . . . . .
H9 H -0.220356 0.343059 0.533801 0.021 Uiso 1 1 calc R U . . .
C10 C -0.1260(4) 0.3515(2) 0.60452(14) 0.0173(7) Uani 1 1 d . . . . .
C11 C -0.2489(4) 0.3184(2) 0.62921(14) 0.0170(7) Uani 1 1 d . . . . .
C12 C -0.3921(5) 0.2973(3) 0.60579(16) 0.0230(8) Uani 1 1 d . . . . .
H12 H -0.417436 0.304075 0.572046 0.028 Uiso 1 1 calc R U . . .
C13 C -0.4995(5) 0.2659(3) 0.63234(17) 0.0263(9) Uani 1 1 d . . . . .
H13 H -0.599307 0.251089 0.616928 0.032 Uiso 1 1 calc R U . . .
C14 C -0.4593(5) 0.2567(3) 0.68128(16) 0.0241(8) Uani 1 1 d . . . . .
H14 H -0.530472 0.235211 0.700087 0.029 Uiso 1 1 calc R U . . .
C15 C -0.3131(5) 0.2794(2) 0.70243(15) 0.0196(8) Uani 1 1 d . . . . .
H15 H -0.285890 0.273677 0.736184 0.023 Uiso 1 1 calc R U . . .
C16 C -0.0110(4) 0.4076(3) 0.48470(14) 0.0198(8) Uani 1 1 d . . . . .
C17 C -0.0961(5) 0.5132(2) 0.72149(16) 0.0229(8) Uani 1 1 d . . . . .
H17 H -0.091706 0.522831 0.688497 0.027 Uiso 1 1 calc R U . . .
C18 C -0.1492(6) 0.5729(3) 0.74883(18) 0.0306(9) Uani 1 1 d . . . . .
H18 H -0.179926 0.622464 0.734767 0.037 Uiso 1 1 calc R U . . .
C19 C -0.1564(6) 0.5588(3) 0.79677(19) 0.0343(11) Uani 1 1 d . . . . .
H19 H -0.194931 0.598124 0.815877 0.041 Uiso 1 1 calc R U . . .
C20 C -0.1069(6) 0.4865(3) 0.81672(17) 0.0306(10) Uani 1 1 d . . . . .
H20 H -0.108551 0.476095 0.849769 0.037 Uiso 1 1 calc R U . . .
C21 C -0.0550(5) 0.4300(3) 0.78755(15) 0.0240(8) Uani 1 1 d . . . . .
C22 C 0.0021(5) 0.3513(3) 0.80516(15) 0.0242(8) Uani 1 1 d . . . . .
C23 C 0.0150(6) 0.3252(3) 0.85250(16) 0.0327(11) Uani 1 1 d . . . . .
H23 H -0.006557 0.359591 0.877286 0.039 Uiso 1 1 calc R U . . .
C24 C 0.0597(6) 0.2484(3) 0.86238(16) 0.0319(11) Uani 1 1 d . . . . .
C25 C 0.0974(5) 0.1992(3) 0.82632(16) 0.0284(10) Uani 1 1 d . . . . .
H25 H 0.125429 0.145690 0.832848 0.034 Uiso 1 1 calc R U . . .
C26 C 0.0930(5) 0.2306(3) 0.78022(15) 0.0228(8) Uani 1 1 d . . . . .
C27 C 0.1358(5) 0.1884(3) 0.73832(16) 0.0239(8) Uani 1 1 d . . . . .
C28 C 0.2035(5) 0.1140(3) 0.74141(18) 0.0311(10) Uani 1 1 d . . . . .
H28 H 0.226907 0.087941 0.771470 0.037 Uiso 1 1 calc R U . . .
C29 C 0.2361(6) 0.0789(3) 0.6999(2) 0.0362(11) Uani 1 1 d . . . . .
H29 H 0.283221 0.028271 0.701087 0.043 Uiso 1 1 calc R U . . .
C30 C 0.1997(6) 0.1180(3) 0.65651(19) 0.0338(11) Uani 1 1 d . . . . .
H30 H 0.219314 0.094420 0.627437 0.041 Uiso 1 1 calc R U . . .
C31 C 0.1339(5) 0.1924(3) 0.65655(16) 0.0264(9) Uani 1 1 d . . . . .
H31 H 0.109468 0.219481 0.626829 0.032 Uiso 1 1 calc R U . . .
C32 C 0.0648(7) 0.2143(4) 0.91256(18) 0.0468(14) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 1.778(3) . ?
U1 O1 1.787(3) . ?
U1 O7 2.324(3) . ?
U1 O7 2.326(3) 3_666 ?
U1 O3 2.348(3) . ?
U1 O5 2.353(3) 4_665 ?
U1 O8 2.478(4) . ?
U1 U1 3.8864(3) 3_666 ?
Ni1 N2 1.987(3) . ?
Ni1 N5 1.990(3) . ?
Ni1 N4 2.109(4) . ?
Ni1 N6 2.116(4) . ?
Ni1 N3 2.120(3) . ?
Ni1 N1 2.123(3) . ?
O3 C16 1.269(5) . ?
O4 C16 1.239(5) . ?
O5 C32 1.263(6) . ?
O6 C32 1.227(7) . ?
O7 H7 0.838(10) . ?
O8 H8A 0.8406 . ?
O8 H8B 0.8403 . ?
O9 N7 1.330(8) . ?
O10 N7 1.200(7) . ?
O11 N7 1.220(7) . ?
O12 H12A 0.838(10) . ?
O12 H12B 0.837(10) . ?
N1 C1 1.341(5) . ?
N1 C5 1.356(5) . ?
N2 C6 1.342(5) . ?
N2 C10 1.346(5) . ?
N3 C15 1.333(5) . ?
N3 C11 1.359(5) . ?
N4 C17 1.342(5) . ?
N4 C21 1.358(5) . ?
N5 C22 1.339(6) . ?
N5 C26 1.343(6) . ?
N6 C31 1.330(6) . ?
N6 C27 1.354(5) . ?
C1 C2 1.391(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.385(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.385(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.397(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.476(5) . ?
C6 C7 1.377(5) . ?
C7 C8 1.396(5) . ?
C7 H7A 0.9500 . ?
C8 C9 1.390(5) . ?
C8 C16 1.508(5) . ?
C9 C10 1.390(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.478(5) . ?
C11 C12 1.375(6) . ?
C12 C13 1.393(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.380(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.384(6) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C17 C18 1.392(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.383(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.389(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.382(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.483(6) . ?
C22 C23 1.393(6) . ?
C23 C24 1.375(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.391(7) . ?
C24 C32 1.521(6) . ?
C25 C26 1.398(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.476(6) . ?
C27 C28 1.389(6) . ?
C28 C29 1.380(7) . ?
C28 H28 0.9500 . ?
C29 C30 1.385(7) . ?
C29 H29 0.9500 . ?
C30 C31 1.386(6) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U1 O1 176.30(14) . . ?
O2 U1 O7 90.60(12) . . ?
O1 U1 O7 92.48(12) . . ?
O2 U1 O7 92.97(13) . 3_666 ?
O1 U1 O7 90.13(13) . 3_666 ?
O7 U1 O7 66.59(11) . 3_666 ?
O2 U1 O3 89.47(11) . . ?
O1 U1 O3 89.19(12) . . ?
O7 U1 O3 145.00(10) . . ?
O7 U1 O3 78.46(10) 3_666 . ?
O2 U1 O5 88.33(12) . 4_665 ?
O1 U1 O5 90.57(13) . 4_665 ?
O7 U1 O5 73.65(10) . 4_665 ?
O7 U1 O5 140.23(10) 3_666 4_665 ?
O3 U1 O5 141.32(11) . 4_665 ?
O2 U1 O8 90.04(16) . . ?
O1 U1 O8 86.27(16) . . ?
O7 U1 O8 144.07(11) . . ?
O7 U1 O8 149.21(11) 3_666 . ?
O3 U1 O8 70.93(12) . . ?
O5 U1 O8 70.46(12) 4_665 . ?
O2 U1 U1 92.14(10) . 3_666 ?
O1 U1 U1 91.56(10) . 3_666 ?
O7 U1 U1 33.31(6) . 3_666 ?
O7 U1 U1 33.28(6) 3_666 3_666 ?
O3 U1 U1 111.72(8) . 3_666 ?
O5 U1 U1 106.96(8) 4_665 3_666 ?
O8 U1 U1 176.58(10) . 3_666 ?
N2 Ni1 N5 175.15(15) . . ?
N2 Ni1 N4 106.77(14) . . ?
N5 Ni1 N4 78.01(14) . . ?
N2 Ni1 N6 96.91(14) . . ?
N5 Ni1 N6 78.31(14) . . ?
N4 Ni1 N6 156.32(13) . . ?
N2 Ni1 N3 77.99(13) . . ?
N5 Ni1 N3 101.17(13) . . ?
N4 Ni1 N3 93.24(13) . . ?
N6 Ni1 N3 91.58(13) . . ?
N2 Ni1 N1 78.52(13) . . ?
N5 Ni1 N1 102.37(13) . . ?
N4 Ni1 N1 91.94(13) . . ?
N6 Ni1 N1 92.84(13) . . ?
N3 Ni1 N1 156.46(12) . . ?
C16 O3 U1 151.3(3) . . ?
C32 O5 U1 132.2(4) . 4_566 ?
U1 O7 U1 113.41(11) . 3_666 ?
U1 O7 H7 118(4) . . ?
U1 O7 H7 123(4) 3_666 . ?
U1 O8 H8A 129.0 . . ?
U1 O8 H8B 107.4 . . ?
H8A O8 H8B 113.6 . . ?
H12A O12 H12B 107.2(17) . . ?
C1 N1 C5 118.8(3) . . ?
C1 N1 Ni1 128.3(3) . . ?
C5 N1 Ni1 112.8(3) . . ?
C6 N2 C10 120.9(3) . . ?
C6 N2 Ni1 118.9(3) . . ?
C10 N2 Ni1 119.3(2) . . ?
C15 N3 C11 118.6(3) . . ?
C15 N3 Ni1 127.6(3) . . ?
C11 N3 Ni1 113.7(2) . . ?
C17 N4 C21 118.4(4) . . ?
C17 N4 Ni1 127.3(3) . . ?
C21 N4 Ni1 114.2(3) . . ?
C22 N5 C26 121.5(4) . . ?
C22 N5 Ni1 119.6(3) . . ?
C26 N5 Ni1 118.8(3) . . ?
C31 N6 C27 118.2(4) . . ?
C31 N6 Ni1 128.0(3) . . ?
C27 N6 Ni1 113.7(3) . . ?
O10 N7 O11 123.1(6) . . ?
O10 N7 O9 124.8(6) . . ?
O11 N7 O9 111.2(6) . . ?
N1 C1 C2 122.2(4) . . ?
N1 C1 H1 118.9 . . ?
C2 C1 H1 118.9 . . ?
C3 C2 C1 119.1(4) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C4 C3 C2 119.3(4) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 118.8(4) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 121.9(4) . . ?
N1 C5 C6 115.4(3) . . ?
C4 C5 C6 122.7(3) . . ?
N2 C6 C7 121.6(4) . . ?
N2 C6 C5 113.7(3) . . ?
C7 C6 C5 124.7(3) . . ?
C6 C7 C8 118.3(3) . . ?
C6 C7 H7A 120.8 . . ?
C8 C7 H7A 120.8 . . ?
C9 C8 C7 119.8(3) . . ?
C9 C8 C16 120.9(3) . . ?
C7 C8 C16 119.3(3) . . ?
C10 C9 C8 118.8(4) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
N2 C10 C9 120.5(3) . . ?
N2 C10 C11 113.5(3) . . ?
C9 C10 C11 126.0(4) . . ?
N3 C11 C12 121.9(3) . . ?
N3 C11 C10 114.7(3) . . ?
C12 C11 C10 123.4(4) . . ?
C11 C12 C13 118.9(4) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 H12 120.5 . . ?
C14 C13 C12 119.2(4) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C13 C14 C15 118.7(4) . . ?
C13 C14 H14 120.7 . . ?
C15 C14 H14 120.7 . . ?
N3 C15 C14 122.7(4) . . ?
N3 C15 H15 118.7 . . ?
C14 C15 H15 118.7 . . ?
O4 C16 O3 124.6(4) . . ?
O4 C16 C8 118.8(3) . . ?
O3 C16 C8 116.5(3) . . ?
N4 C17 C18 122.2(4) . . ?
N4 C17 H17 118.9 . . ?
C18 C17 H17 118.9 . . ?
C19 C18 C17 118.9(5) . . ?
C19 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
C18 C19 C20 119.3(5) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
C21 C20 C19 118.7(4) . . ?
C21 C20 H20 120.6 . . ?
C19 C20 H20 120.6 . . ?
N4 C21 C20 122.4(4) . . ?
N4 C21 C22 114.4(4) . . ?
C20 C21 C22 123.2(4) . . ?
N5 C22 C23 120.9(4) . . ?
N5 C22 C21 113.7(4) . . ?
C23 C22 C21 125.4(4) . . ?
C24 C23 C22 118.2(5) . . ?
C24 C23 H23 120.9 . . ?
C22 C23 H23 120.9 . . ?
C23 C24 C25 120.6(4) . . ?
C23 C24 C32 121.0(5) . . ?
C25 C24 C32 118.4(5) . . ?
C24 C25 C26 118.4(4) . . ?
C24 C25 H25 120.8 . . ?
C26 C25 H25 120.8 . . ?
N5 C26 C25 120.1(4) . . ?
N5 C26 C27 114.1(3) . . ?
C25 C26 C27 125.8(4) . . ?
N6 C27 C28 122.2(4) . . ?
N6 C27 C26 114.7(4) . . ?
C28 C27 C26 123.1(4) . . ?
C29 C28 C27 118.6(4) . . ?
C29 C28 H28 120.7 . . ?
C27 C28 H28 120.7 . . ?
C28 C29 C30 119.5(4) . . ?
C28 C29 H29 120.3 . . ?
C30 C29 H29 120.3 . . ?
C29 C30 C31 118.3(5) . . ?
C29 C30 H30 120.8 . . ?
C31 C30 H30 120.8 . . ?
N6 C31 C30 123.1(4) . . ?
N6 C31 H31 118.4 . . ?
C30 C31 H31 118.4 . . ?
O6 C32 O5 127.0(5) . . ?
O6 C32 C24 118.5(5) . . ?
O5 C32 C24 114.5(5) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O7 H7 O4 0.838(10) 1.967(14) 2.796(4) 170(5) 1_655 yes
O8 H8A O9 0.84 2.06 2.751(7) 138.7 . yes
O8 H8B O13 0.84 2.14 2.957(9) 164.6 . yes
O12 H12A O4 0.838(10) 2.023(14) 2.858(5) 174(8) . yes
O12 H12B O10 0.837(10) 2.127(13) 2.963(7) 177(6) . yes
C2 H2 O11 0.95 2.56 3.157(6) 120.6 4_666 yes
C7 H7A O7 0.95 2.48 3.405(5) 164.2 3_666 yes
C12 H12 O1 0.95 2.44 3.279(5) 147.5 1_455 yes
C15 H15 O9 0.95 2.47 3.355(7) 155.1 4_566 yes
C17 H17 O12 0.95 2.57 3.314(6) 135.8 3_566 yes
C18 H18 O9 0.95 2.37 3.268(8) 156.7 3_566 yes


