# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_shx97
_database_code_depnum_ccdc_archive 'CCDC 1575472'
_audit_update_record             
;
2017-09-20 deposited with the CCDC.
2018-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H18 O16 U2'
_chemical_formula_sum            'C36 H18 O16 U2'
_chemical_formula_weight         1182.57

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           23
_space_group_name_H-M_alt        'I 2 2 2'
_space_group_name_Hall           'I 2 2'

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

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

_cell_length_a                   19.196(4)
_cell_length_b                   27.013(5)
_cell_length_c                   21.601(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     11201(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    71667
_cell_measurement_theta_min      3.08
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_F_000             4368
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    5.824
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.391
_exptl_absorpt_correction_T_max  0.527
_exptl_absorpt_process_details   ABSCOR(Higashi,1995)
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'rigaku r-axis rapid'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            71667
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.022
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9900
_reflns_number_gt                8044
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.845
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.036 0.000 0.000 629 85 ' '
2 -0.039 -0.004 0.436 3948 531 ' '
3 -0.022 0.500 0.500 629 85 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?


_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0884P)²+93.5104P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9877
_refine_ls_number_parameters     487
_refine_ls_number_restraints     143
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0555
_refine_ls_wR_factor_ref         0.1825
_refine_ls_wR_factor_gt          0.1454
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_restrained_S_all      8.167
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U -0.24853(5) -0.16929(2) 0.10266(3) 0.0509(2) Uani 1 1 d . . . . .
U2 U -0.25209(5) -0.52435(2) -0.18244(3) 0.0570(2) Uani 1 1 d . . . . .
O4 O -0.3068(8) -0.4575(6) -0.1240(8) 0.067(4) Uani 1 1 d . U . . .
O6 O -0.2638(8) -0.4968(6) -0.2526(6) 0.071(4) Uani 1 1 d . . . . .
O11 O -0.1800(7) -0.1050(6) 0.1525(8) 0.061(4) Uani 1 1 d . U . . .
O7 O -0.3237(7) -0.1179(6) 0.1686(7) 0.057(4) Uani 1 1 d . U . . .
O1 O -0.3030(9) -0.2332(7) 0.0411(10) 0.069(5) Uani 1 1 d . U . . .
O2 O -0.1899(8) -0.2318(8) 0.0351(12) 0.105(9) Uani 1 1 d . . . . .
O13 O 0.1167(8) -0.0287(7) 0.3194(8) 0.071(5) Uani 1 1 d . . . . .
O16 O -0.2529(13) -0.1290(6) 0.0384(5) 0.081(4) Uani 1 1 d . . . . .
O8 O -0.3767(8) -0.1723(8) 0.1132(12) 0.098(7) Uani 1 1 d . . . . .
O12 O -0.1232(7) -0.1621(8) 0.1062(10) 0.083(6) Uani 1 1 d . . . . .
O10 O -0.6246(6) -0.0243(6) 0.2968(7) 0.054(4) Uani 1 1 d . . . . .
C32 C 0.1444(9) -0.1232(9) 0.0951(10) 0.059(5) Uani 1 1 d . . . . .
H32A H 0.188980 -0.129272 0.080016 0.071 Uiso 1 1 calc R U . . .
C20 C -0.6464(19) -0.1613(13) 0.0994(15) 0.104(8) Uani 1 1 d . U . . .
H20A H -0.688594 -0.176647 0.090407 0.125 Uiso 1 1 calc R U . . .
C11 C -0.2161(10) -0.2955(9) -0.0791(12) 0.070(4) Uani 1 1 d . U . . .
C19 C -0.6379(14) -0.1257(11) 0.1509(14) 0.082(6) Uani 1 1 d . U . . .
H19A H -0.677591 -0.111436 0.167911 0.098 Uiso 1 1 calc R U . . .
C31 C 0.1368(10) -0.1011(8) 0.1504(12) 0.067(7) Uani 1 1 d . . . . .
H31A H 0.175823 -0.086979 0.168736 0.081 Uiso 1 1 calc R U . . .
C34 C 0.0205(10) -0.1327(7) 0.0818(9) 0.051(4) Uani 1 1 d . . . . .
H34A H -0.017406 -0.140595 0.056875 0.062 Uiso 1 1 calc R U . . .
C6 C -0.2498(14) -0.4291(8) -0.1247(14) 0.103(10) Uani 1 1 d . . . . .
C23 C -0.5128(16) -0.1324(11) 0.1513(16) 0.085(8) Uani 1 1 d . U . . .
C35 C 0.0102(8) -0.1151(8) 0.1456(10) 0.051(5) Uani 1 1 d . . . . .
O9 O -0.6803(8) -0.0920(6) 0.2700(8) 0.063(4) Uani 1 1 d D U . . .
C16 C -0.5040(12) -0.0716(8) 0.2515(9) 0.051(5) Uani 1 1 d . . . . .
H16A H -0.501839 -0.047356 0.282002 0.062 Uiso 1 1 calc R U . . .
C28 C -0.0069(12) -0.0688(9) 0.2649(14) 0.076(8) Uani 1 1 d . . . . .
H28A H -0.014000 -0.058019 0.305356 0.091 Uiso 1 1 calc R U . . .
C24 C -0.5746(10) -0.1128(8) 0.1746(10) 0.049(5) Uani 1 1 d D U . . .
C36 C 0.0703(10) -0.0983(8) 0.1831(11) 0.055(6) Uani 1 1 d . . . . .
C13 C -0.3807(13) -0.1376(12) 0.1454(14) 0.079(9) Uani 1 1 d . . . . .
C15 C -0.4422(11) -0.0926(8) 0.2300(10) 0.055(5) Uani 1 1 d D U . . .
H15A H -0.400415 -0.089768 0.251541 0.066 Uiso 1 1 calc R U . . .
C17 C -0.5679(11) -0.0858(8) 0.2291(12) 0.061(7) Uani 1 1 d D . . . .
C25 C -0.1232(10) -0.1268(9) 0.1482(14) 0.065(7) Uani 1 1 d . . . . .
C14 C -0.4472(12) -0.1186(11) 0.1729(12) 0.068(7) Uani 1 1 d D . . . .
C29 C 0.0619(12) -0.0760(8) 0.2395(11) 0.052(5) Uani 1 1 d . U . . .
C27 C -0.0638(10) -0.0794(8) 0.2234(10) 0.047(5) Uani 1 1 d . U . . .
H27A H -0.107234 -0.065745 0.232029 0.057 Uiso 1 1 calc R U . . .
C26 C -0.0575(10) -0.1074(10) 0.1739(15) 0.067(8) Uani 1 1 d . . . . .
C5 C -0.2491(18) -0.3842(7) -0.0870(10) 0.073(4) Uani 1 1 d . U . . .
C2 C -0.2432(13) -0.2984(8) -0.0158(10) 0.067(5) Uani 1 1 d . U . . .
C1 C -0.2465(17) -0.2527(7) 0.0215(10) 0.076(7) Uani 1 1 d . . . . .
C33 C 0.0869(11) -0.1371(9) 0.0598(10) 0.068(6) Uani 1 1 d . . . . .
H33A H 0.093934 -0.149809 0.020287 0.082 Uiso 1 1 calc R U . . .
C22 C -0.5190(15) -0.1601(10) 0.0932(13) 0.083(8) Uani 1 1 d . U . . .
H22A H -0.478965 -0.171593 0.073765 0.100 Uiso 1 1 calc R U . . .
C7 C -0.2011(12) -0.3367(11) -0.1783(12) 0.078(5) Uani 1 1 d . U . . .
H7A H -0.207675 -0.363490 -0.204791 0.094 Uiso 1 1 calc R U . . .
C10 C -0.1940(13) -0.2508(10) -0.1108(13) 0.085(6) Uani 1 1 d . U . . .
H10A H -0.196816 -0.220883 -0.089608 0.103 Uiso 1 1 calc R U . . .
C8 C -0.1740(14) -0.2924(11) -0.2015(13) 0.090(7) Uani 1 1 d . U . . .
H8A H -0.158153 -0.292416 -0.242189 0.108 Uiso 1 1 calc R U . . .
C9 C -0.1691(17) -0.2504(12) -0.1701(15) 0.100(9) Uani 1 1 d . U . . .
H9A H -0.149720 -0.222042 -0.187586 0.120 Uiso 1 1 calc R U . . .
C21 C -0.5862(19) -0.1698(14) 0.066(2) 0.122(12) Uani 1 1 d . U . . .
H21A H -0.589064 -0.181690 0.025254 0.146 Uiso 1 1 calc R U . . .
C3 C -0.2712(12) -0.3394(9) 0.0066(13) 0.084(8) Uani 1 1 d . . . . .
H3A H -0.290214 -0.339268 0.046161 0.101 Uiso 1 1 calc R U . . .
C4 C -0.2724(12) -0.3837(9) -0.0292(14) 0.089(9) Uani 1 1 d . . . . .
H4A H -0.289878 -0.412638 -0.011761 0.107 Uiso 1 1 calc R U . . .
C12 C -0.2188(10) -0.3412(9) -0.1139(10) 0.063(4) Uani 1 1 d . U . . .
C30 C 0.1198(13) -0.0615(11) 0.2826(14) 0.068(7) Uani 1 1 d . U . . .
O15 O -0.2379(8) -0.2095(6) 0.1643(6) 0.072(4) Uani 1 1 d . U . . .
O5 O -0.2431(11) -0.5522(7) -0.1112(6) 0.085(4) Uani 1 1 d . U . . .
O3 O -0.1955(7) -0.4460(5) -0.1502(7) 0.057(3) Uani 1 1 d . U . . .
O14 O 0.1714(8) -0.0900(6) 0.2822(8) 0.067(4) Uani 1 1 d D U . . .
C18 C -0.6248(10) -0.0672(8) 0.2684(11) 0.051(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O15 1.731(13) . ?
U1 O16 1.765(13) . ?
U1 O12 2.415(14) . ?
U1 O1 2.416(18) . ?
U1 O11 2.429(14) . ?
U1 O7 2.457(14) . ?
U1 O8 2.472(16) . ?
U1 O2 2.498(16) . ?
U1 C13 2.83(2) . ?
U1 C25 2.84(2) . ?
U1 C1 2.856(17) . ?
U2 O6 1.703(14) . ?
U2 O5 1.721(14) . ?
U2 O14 2.427(14) 5_444 ?
U2 O4 2.442(15) . ?
U2 O3 2.479(13) . ?
U2 O10 2.489(12) 5_544 ?
U2 O9 2.509(17) 5_544 ?
U2 O13 2.523(16) 5_444 ?
U2 C30 2.76(3) 5_444 ?
U2 C6 2.860(18) . ?
U2 C18 2.905(18) 5_544 ?
O4 C6 1.34(3) . ?
O11 C25 1.24(2) . ?
O7 C13 1.32(3) . ?
O1 C1 1.28(3) . ?
O2 C1 1.26(3) . ?
O13 C30 1.19(3) . ?
O8 C13 1.17(3) . ?
O12 C25 1.31(3) . ?
O10 C18 1.31(2) . ?
C32 C31 1.34(3) . ?
C32 C33 1.39(3) . ?
C32 H32A 0.9300 . ?
C20 C21 1.39(4) . ?
C20 C19 1.48(4) . ?
C20 H20A 0.9300 . ?
C11 C12 1.45(3) . ?
C11 C10 1.45(4) . ?
C11 C2 1.47(3) . ?
C19 C24 1.36(3) . ?
C19 H19A 0.9300 . ?
C31 C36 1.46(3) . ?
C31 H31A 0.9300 . ?
C34 C33 1.36(3) . ?
C34 C35 1.47(3) . ?
C34 H34A 0.9300 . ?
C6 O3 1.27(3) . ?
C6 C5 1.46(3) . ?
C23 C24 1.39(3) . ?
C23 C14 1.39(4) . ?
C23 C22 1.46(4) . ?
C35 C26 1.45(3) . ?
C35 C36 1.48(3) . ?
O9 C18 1.26(2) . ?
C16 C17 1.37(3) . ?
C16 C15 1.39(3) . ?
C16 H16A 0.9300 . ?
C28 C27 1.44(3) . ?
C28 C29 1.44(3) . ?
C28 H28A 0.9300 . ?
C24 C17 1.39(2) . ?
C36 C29 1.37(3) . ?
C13 C14 1.50(3) . ?
C15 C14 1.42(2) . ?
C15 H15A 0.9300 . ?
C17 C18 1.47(3) . ?
C25 C26 1.47(3) . ?
C29 C30 1.50(3) . ?
C27 C26 1.31(3) . ?
C27 H27A 0.9300 . ?
C5 C4 1.33(3) . ?
C5 C12 1.42(3) . ?
C2 C3 1.32(3) . ?
C2 C1 1.47(2) . ?
C33 H33A 0.9300 . ?
C22 C21 1.45(4) . ?
C22 H22A 0.9300 . ?
C7 C8 1.40(4) . ?
C7 C12 1.44(3) . ?
C7 H7A 0.9300 . ?
C10 C9 1.37(4) . ?
C10 H10A 0.9300 . ?
C8 C9 1.33(4) . ?
C8 H8A 0.9300 . ?
C9 H9A 0.9300 . ?
C21 H21A 0.9300 . ?
C3 C4 1.43(3) . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9300 . ?
C30 O14 1.26(3) . ?

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
O15 U1 O16 175.8(10) . . ?
O15 U1 O12 84.7(8) . . ?
O16 U1 O12 91.3(10) . . ?
O15 U1 O1 91.5(7) . . ?
O16 U1 O1 89.3(7) . . ?
O12 U1 O1 120.4(6) . . ?
O15 U1 O11 92.5(7) . . ?
O16 U1 O11 86.2(7) . . ?
O12 U1 O11 52.3(6) . . ?
O1 U1 O11 171.3(6) . . ?
O15 U1 O7 88.7(6) . . ?
O16 U1 O7 94.6(8) . . ?
O12 U1 O7 121.4(5) . . ?
O1 U1 O7 117.9(5) . . ?
O11 U1 O7 69.9(4) . . ?
O15 U1 O8 91.5(9) . . ?
O16 U1 O8 92.6(10) . . ?
O12 U1 O8 172.4(5) . . ?
O1 U1 O8 66.2(6) . . ?
O11 U1 O8 121.4(6) . . ?
O7 U1 O8 51.8(6) . . ?
O15 U1 O2 88.4(9) . . ?
O16 U1 O2 88.8(9) . . ?
O12 U1 O2 67.9(6) . . ?
O1 U1 O2 52.5(4) . . ?
O11 U1 O2 119.8(5) . . ?
O7 U1 O2 169.9(5) . . ?
O8 U1 O2 118.7(6) . . ?
O15 U1 C13 92.6(9) . . ?
O16 U1 C13 91.6(11) . . ?
O12 U1 C13 149.1(7) . . ?
O1 U1 C13 90.4(7) . . ?
O11 U1 C13 97.1(6) . . ?
O7 U1 C13 27.7(6) . . ?
O8 U1 C13 24.3(7) . . ?
O2 U1 C13 142.9(6) . . ?
O15 U1 C25 83.5(8) . . ?
O16 U1 C25 93.6(9) . . ?
O12 U1 C25 27.5(6) . . ?
O1 U1 C25 147.7(6) . . ?
O11 U1 C25 25.8(6) . . ?
O7 U1 C25 93.9(6) . . ?
O8 U1 C25 145.5(7) . . ?
O2 U1 C25 95.3(6) . . ?
C13 U1 C25 121.6(6) . . ?
O15 U1 C1 88.6(7) . . ?
O16 U1 C1 90.3(7) . . ?
O12 U1 C1 94.0(8) . . ?
O1 U1 C1 26.4(8) . . ?
O11 U1 C1 146.0(7) . . ?
O7 U1 C1 144.1(7) . . ?
O8 U1 C1 92.5(8) . . ?
O2 U1 C1 26.1(7) . . ?
C13 U1 C1 116.8(8) . . ?
C25 U1 C1 121.3(8) . . ?
O6 U2 O5 178.2(9) . . ?
O6 U2 O14 87.7(7) . 5_444 ?
O5 U2 O14 91.3(8) . 5_444 ?
O6 U2 O4 94.6(7) . . ?
O5 U2 O4 84.5(7) . . ?
O14 U2 O4 116.3(6) 5_444 . ?
O6 U2 O3 86.3(6) . . ?
O5 U2 O3 94.5(7) . . ?
O14 U2 O3 168.0(5) 5_444 . ?
O4 U2 O3 53.9(4) . . ?
O6 U2 O10 88.2(7) . 5_544 ?
O5 U2 O10 93.6(8) . 5_544 ?
O14 U2 O10 122.6(5) 5_444 5_544 ?
O4 U2 O10 121.0(5) . 5_544 ?
O3 U2 O10 67.6(5) . 5_544 ?
O6 U2 O9 91.6(7) . 5_544 ?
O5 U2 O9 89.5(7) . 5_544 ?
O14 U2 O9 70.8(5) 5_444 5_544 ?
O4 U2 O9 170.7(6) . 5_544 ?
O3 U2 O9 119.8(5) . 5_544 ?
O10 U2 O9 52.2(5) 5_544 5_544 ?
O6 U2 O13 84.4(7) . 5_444 ?
O5 U2 O13 93.8(8) . 5_444 ?
O14 U2 O13 50.6(6) 5_444 5_444 ?
O4 U2 O13 66.3(5) . 5_444 ?
O3 U2 O13 118.3(5) . 5_444 ?
O10 U2 O13 170.1(5) 5_544 5_444 ?
O9 U2 O13 121.4(5) 5_544 5_444 ?
O6 U2 C30 78.4(8) . 5_444 ?
O5 U2 C30 100.1(10) . 5_444 ?
O14 U2 C30 27.0(7) 5_444 5_444 ?
O4 U2 C30 91.6(7) . 5_444 ?
O3 U2 C30 141.0(7) . 5_444 ?
O10 U2 C30 145.8(7) 5_544 5_444 ?
O9 U2 C30 96.5(7) 5_544 5_444 ?
O13 U2 C30 25.5(6) 5_444 5_444 ?
O6 U2 C6 89.8(8) . . ?
O5 U2 C6 90.1(8) . . ?
O14 U2 C6 143.5(7) 5_444 . ?
O4 U2 C6 27.8(7) . . ?
O3 U2 C6 26.2(7) . . ?
O10 U2 C6 93.6(7) 5_544 . ?
O9 U2 C6 145.7(7) 5_544 . ?
O13 U2 C6 92.9(7) 5_444 . ?
C30 U2 C6 117.4(8) 5_444 . ?
O6 U2 C18 87.7(8) . 5_544 ?
O5 U2 C18 93.9(8) . 5_544 ?
O14 U2 C18 95.9(6) 5_444 5_544 ?
O4 U2 C18 147.8(5) . 5_544 ?
O3 U2 C18 94.3(5) . 5_544 ?
O10 U2 C18 26.8(5) 5_544 5_544 ?
O9 U2 C18 25.6(5) 5_544 5_544 ?
O13 U2 C18 145.8(5) 5_444 5_544 ?
C30 U2 C18 120.3(7) 5_444 5_544 ?
C6 U2 C18 120.4(7) . 5_544 ?
C6 O4 U2 93.8(12) . . ?
C25 O11 U1 95.9(13) . . ?
C13 O7 U1 92.2(13) . . ?
C1 O1 U1 96.3(14) . . ?
C1 O2 U1 93.0(13) . . ?
C30 O13 U2 88.5(16) . 5 ?
C13 O8 U1 95.4(16) . . ?
C25 O12 U1 94.6(12) . . ?
C18 O10 U2 94.6(11) . 5_455 ?
C31 C32 C33 121.3(18) . . ?
C31 C32 H32A 119.3 . . ?
C33 C32 H32A 119.3 . . ?
C21 C20 C19 114(3) . . ?
C21 C20 H20A 122.9 . . ?
C19 C20 H20A 122.9 . . ?
C12 C11 C10 118(2) . . ?
C12 C11 C2 115(2) . . ?
C10 C11 C2 126(2) . . ?
C24 C19 C20 123(3) . . ?
C24 C19 H19A 118.4 . . ?
C20 C19 H19A 118.4 . . ?
C32 C31 C36 123.3(18) . . ?
C32 C31 H31A 118.3 . . ?
C36 C31 H31A 118.3 . . ?
C33 C34 C35 118.7(18) . . ?
C33 C34 H34A 120.7 . . ?
C35 C34 H34A 120.7 . . ?
O3 C6 O4 118.2(16) . . ?
O3 C6 C5 122(3) . . ?
O4 C6 C5 119(3) . . ?
O3 C6 U2 59.8(9) . . ?
O4 C6 U2 58.4(9) . . ?
C5 C6 U2 172(2) . . ?
C24 C23 C14 123(3) . . ?
C24 C23 C22 116(3) . . ?
C14 C23 C22 120(3) . . ?
C26 C35 C34 124.2(19) . . ?
C26 C35 C36 115.1(19) . . ?
C34 C35 C36 120.4(15) . . ?
C18 O9 U2 95.1(13) . 5_455 ?
C17 C16 C15 122.0(19) . . ?
C17 C16 H16A 119.0 . . ?
C15 C16 H16A 119.0 . . ?
C27 C28 C29 115(2) . . ?
C27 C28 H28A 122.3 . . ?
C29 C28 H28A 122.3 . . ?
C19 C24 C23 122(2) . . ?
C19 C24 C17 122(2) . . ?
C23 C24 C17 115(2) . . ?
C29 C36 C31 123.9(19) . . ?
C29 C36 C35 122.0(18) . . ?
C31 C36 C35 113.6(18) . . ?
O8 C13 O7 120(2) . . ?
O8 C13 C14 124(2) . . ?
O7 C13 C14 115(2) . . ?
O8 C13 U1 60.3(13) . . ?
O7 C13 U1 60.1(11) . . ?
C14 C13 U1 174.7(18) . . ?
C16 C15 C14 116(2) . . ?
C16 C15 H15A 122.2 . . ?
C14 C15 H15A 122.2 . . ?
C16 C17 C24 121.8(19) . . ?
C16 C17 C18 111.4(18) . . ?
C24 C17 C18 127(2) . . ?
O11 C25 O12 113(2) . . ?
O11 C25 C26 124(2) . . ?
O12 C25 C26 121.2(19) . . ?
O11 C25 U1 58.3(11) . . ?
O12 C25 U1 57.9(10) . . ?
C26 C25 U1 177(2) . . ?
C23 C14 C15 119(2) . . ?
C23 C14 C13 123(2) . . ?
C15 C14 C13 117(2) . . ?
C36 C29 C28 120(2) . . ?
C36 C29 C30 125(2) . . ?
C28 C29 C30 114(2) . . ?
C26 C27 C28 123(2) . . ?
C26 C27 H27A 118.3 . . ?
C28 C27 H27A 118.3 . . ?
C27 C26 C35 120.5(19) . . ?
C27 C26 C25 116(2) . . ?
C35 C26 C25 124(2) . . ?
C4 C5 C12 120.9(19) . . ?
C4 C5 C6 122(3) . . ?
C12 C5 C6 117(2) . . ?
C3 C2 C11 122.0(18) . . ?
C3 C2 C1 119(2) . . ?
C11 C2 C1 119(2) . . ?
O2 C1 O1 117.9(15) . . ?
O2 C1 C2 118(3) . . ?
O1 C1 C2 124(3) . . ?
O2 C1 U1 60.9(10) . . ?
O1 C1 U1 57.2(10) . . ?
C2 C1 U1 175(2) . . ?
C34 C33 C32 122(2) . . ?
C34 C33 H33A 119.1 . . ?
C32 C33 H33A 119.1 . . ?
C21 C22 C23 121(3) . . ?
C21 C22 H22A 119.3 . . ?
C23 C22 H22A 119.3 . . ?
C8 C7 C12 120(2) . . ?
C8 C7 H7A 119.8 . . ?
C12 C7 H7A 119.8 . . ?
C9 C10 C11 123(2) . . ?
C9 C10 H10A 118.3 . . ?
C11 C10 H10A 118.3 . . ?
C9 C8 C7 125(3) . . ?
C9 C8 H8A 117.4 . . ?
C7 C8 H8A 117.4 . . ?
C8 C9 C10 117(3) . . ?
C8 C9 H9A 121.7 . . ?
C10 C9 H9A 121.7 . . ?
C20 C21 C22 120(4) . . ?
C20 C21 H21A 120.1 . . ?
C22 C21 H21A 120.1 . . ?
C2 C3 C4 121(3) . . ?
C2 C3 H3A 119.6 . . ?
C4 C3 H3A 119.6 . . ?
C5 C4 C3 121(3) . . ?
C5 C4 H4A 119.5 . . ?
C3 C4 H4A 119.6 . . ?
C5 C12 C7 124(2) . . ?
C5 C12 C11 120(2) . . ?
C7 C12 C11 115(2) . . ?
O13 C30 O14 120(3) . . ?
O13 C30 C29 125(2) . . ?
O14 C30 C29 115(2) . . ?
O13 C30 U2 66.0(14) . 5 ?
O14 C30 U2 61.5(12) . 5 ?
C29 C30 U2 157(2) . 5 ?
C6 O3 U2 94.0(12) . . ?
C30 O14 U2 91.5(15) . 5 ?
O9 C18 O10 117.4(18) . . ?
O9 C18 C17 117.6(19) . . ?
O10 C18 C17 124.6(17) . . ?
O9 C18 U2 59.3(11) . 5_455 ?
O10 C18 U2 58.6(9) . 5_455 ?
C17 C18 U2 166.2(18) . 5_455 ?

_refine_diff_density_max         1.587
_refine_diff_density_min         -2.754
_refine_diff_density_rms         0.179

####################################################################### 
# 
# 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_shx97_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1575476'
_audit_update_record             
;
2017-09-20 deposited with the CCDC.
2018-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H12 O10 U,C5 H5 N,0.5(C10 H10 N2)'
_chemical_formula_sum            'C34 H22 N2 O10 U'
_chemical_formula_weight         856.57

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   12.734(3)
_cell_length_b                   13.956(3)
_cell_length_c                   19.524(6)
_cell_angle_alpha                90
_cell_angle_beta                 118.66(2)
_cell_angle_gamma                90
_cell_volume                     3044.6(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    28690
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_F_000             1648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    5.396
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.194
_exptl_absorpt_correction_T_max  0.359
_exptl_absorpt_process_details   ABSCOR(Higashi,1995)
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'rigaku r-axis rapid'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28690
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.991
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6986
_reflns_number_gt                5351
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0400P)²+15.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6932
_refine_ls_number_parameters     496
_refine_ls_number_restraints     420
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.1125
_refine_ls_wR_factor_gt          0.0860
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.392
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.32099(2) 0.46109(2) 0.79669(2) 0.03612(9) Uani 1 1 d . . . . .
O1 O 0.2964(7) 0.3084(3) 0.7267(3) 0.080(2) Uani 1 1 d . . . . .
O2 O 0.2849(6) 0.4358(3) 0.6601(3) 0.0598(16) Uani 1 1 d . . . . .
O3 O 0.3272(5) 0.0441(3) 0.4256(3) 0.0527(13) Uani 1 1 d . . . . .
O4 O 0.2967(6) 0.1786(3) 0.3630(3) 0.0594(15) Uani 1 1 d . . . . .
O5 O 0.3314(6) 0.6174(3) 0.7381(3) 0.0583(15) Uani 1 1 d . . . . .
O6 O 0.3529(5) 0.6196(3) 0.8557(3) 0.0539(13) Uani 1 1 d . . . . .
O7 O 0.3601(15) 1.1227(6) 0.7867(6) 0.165(6) Uani 1 1 d . U . . .
O8 O 0.1606(14) 1.1079(8) 0.7376(8) 0.186(6) Uani 1 1 d . . . . .
O9 O 0.4741(6) 0.4437(4) 0.8372(3) 0.0651(15) Uani 1 1 d . . . . .
O10 O 0.1698(5) 0.4820(4) 0.7568(3) 0.0656(15) Uani 1 1 d . . . . .
C1 C 0.2817(8) 0.3465(5) 0.6646(4) 0.055(2) Uani 1 1 d . . . . .
C2 C 0.2685(7) 0.2841(5) 0.5978(4) 0.0452(17) Uani 1 1 d . . . . .
C3 C 0.3452(8) 0.2076(5) 0.6156(4) 0.0517(19) Uani 1 1 d . . . . .
H3A H 0.394834 0.190676 0.667403 0.062 Uiso 1 1 calc R U . . .
C4 C 0.3484(7) 0.1552(5) 0.5553(4) 0.0458(17) Uani 1 1 d . . . . .
H4A H 0.399565 0.102907 0.567406 0.055 Uiso 1 1 calc R U . . .
C5 C 0.2769(6) 0.1800(4) 0.4786(4) 0.0397(15) Uani 1 1 d . . . . .
C6 C 0.1877(6) 0.2522(4) 0.4586(4) 0.0390(14) Uani 1 1 d . . . . .
C7 C 0.1002(7) 0.2710(5) 0.3802(4) 0.0516(19) Uani 1 1 d . . . . .
H7A H 0.103187 0.238611 0.339562 0.062 Uiso 1 1 calc R U . . .
C8 C 0.0118(7) 0.3362(6) 0.3643(5) 0.062(2) Uani 1 1 d . . . . .
H8A H -0.046021 0.346559 0.312790 0.075 Uiso 1 1 calc R U . . .
C9 C 0.0061(8) 0.3876(6) 0.4233(5) 0.065(2) Uani 1 1 d . . . . .
H9A H -0.054867 0.431876 0.411167 0.079 Uiso 1 1 calc R U . . .
C10 C 0.0900(8) 0.3730(5) 0.4989(5) 0.058(2) Uani 1 1 d . . . . .
H10A H 0.086090 0.408173 0.538049 0.069 Uiso 1 1 calc R U . . .
C11 C 0.1833(6) 0.3052(4) 0.5193(4) 0.0410(15) Uani 1 1 d . . . . .
C12 C 0.3012(7) 0.1319(5) 0.4194(4) 0.0428(15) Uani 1 1 d . . . . .
C13 C 0.3342(7) 0.6631(5) 0.7945(4) 0.0446(16) Uani 1 1 d . . . . .
C14 C 0.3151(7) 0.7695(5) 0.7892(4) 0.0464(17) Uani 1 1 d . . . . .
C15 C 0.3764(9) 0.8248(5) 0.7632(5) 0.063(2) Uani 1 1 d . . . . .
H15A H 0.426944 0.796532 0.747049 0.076 Uiso 1 1 calc R U . . .
C16 C 0.3632(10) 0.9252(6) 0.7608(6) 0.075(3) Uani 1 1 d . . . . .
H16A H 0.407705 0.962811 0.744775 0.090 Uiso 1 1 calc R U . . .
C17 C 0.2869(11) 0.9679(6) 0.7814(6) 0.079(3) Uani 1 1 d . . . . .
C18 C 0.2200(9) 0.9121(6) 0.8076(5) 0.067(2) Uani 1 1 d . . . . .
C19 C 0.1403(12) 0.9514(8) 0.8324(7) 0.099(4) Uani 1 1 d . . . . .
H19A H 0.130735 1.017473 0.832030 0.118 Uiso 1 1 calc R U . . .
C20 C 0.0788(12) 0.8951(12) 0.8564(7) 0.112(5) Uani 1 1 d . . . . .
H20A H 0.030414 0.923414 0.874301 0.134 Uiso 1 1 calc R U . . .
C21 C 0.0852(9) 0.7964(10) 0.8551(6) 0.088(3) Uani 1 1 d . . . . .
H21A H 0.037292 0.758338 0.867963 0.105 Uiso 1 1 calc R U . . .
C22 C 0.1633(7) 0.7562(7) 0.8346(5) 0.061(2) Uani 1 1 d . . . . .
H22A H 0.170439 0.689806 0.835785 0.073 Uiso 1 1 calc R U . . .
C23 C 0.2343(7) 0.8114(5) 0.8114(4) 0.0491(17) Uani 1 1 d . . . . .
C24 C 0.268(2) 1.0744(10) 0.7687(10) 0.141(6) Uani 1 1 d . U . . .
N1 N 0.7185(14) 0.1887(11) 0.4521(8) 0.069(3) Uani 0.5 1 d D U P A -1
H1A H 0.761046 0.138546 0.449691 0.083 Uiso 0.5 1 d R U P A -1
N2 N 0.455(7) 0.5765(19) 0.519(7) 0.083(6) Uani 0.5 1 d D U P A -1
H2A H 0.426360 0.628579 0.532004 0.100 Uiso 0.5 1 d R U P A -1
C25 C 0.6539(18) 0.1763(16) 0.4872(12) 0.065(5) Uani 0.5 1 d D U P A -1
H25A H 0.649746 0.116359 0.506633 0.078 Uiso 0.5 1 calc R U P A -1
C26 C 0.5921(16) 0.2532(11) 0.4952(10) 0.066(4) Uani 0.5 1 d D U P A -1
H26A H 0.544979 0.244876 0.519263 0.079 Uiso 0.5 1 calc R U P A -1
C27 C 0.6003(17) 0.3425(12) 0.4673(11) 0.069(4) Uani 0.5 1 d D U P A -1
C28 C 0.6653(16) 0.3490(14) 0.4274(11) 0.073(4) Uani 0.5 1 d D U P A -1
H28A H 0.668743 0.406996 0.405111 0.088 Uiso 0.5 1 calc R U P A -1
C29 C 0.725(2) 0.2699(14) 0.4203(15) 0.073(5) Uani 0.5 1 d D U P A -1
H29A H 0.769335 0.274214 0.393687 0.087 Uiso 0.5 1 calc R U P A -1
C30 C 0.547(9) 0.418(3) 0.478(8) 0.080(6) Uani 0.5 1 d D U P A -1
C31 C 0.4569(11) 0.4128(8) 0.4993(7) 0.096(3) Uani 1 1 d D U . A -1
H31A H 0.425146 0.352950 0.499642 0.116 Uiso 1 1 calc R U . A -1
C32 C 0.4128(10) 0.4908(9) 0.5194(7) 0.098(3) Uani 1 1 d D U . A -1
H32A H 0.352655 0.483168 0.533051 0.117 Uiso 1 1 calc R U . A -1
N3 N 0.3475(15) 0.7335(12) 0.5522(9) 0.076(3) Uani 0.5 1 d D U P B -2
H3B H 0.402212 0.688969 0.557945 0.091 Uiso 0.5 1 d R U P B -2
N4 N -0.084(3) 1.061(3) 0.4867(14) 0.094(8) Uani 0.5 1 d D U P B -2
H4B H -0.143829 1.103126 0.476953 0.113 Uiso 0.5 1 d R U P B -2
C33 C 0.2710(19) 0.7125(16) 0.5774(13) 0.078(5) Uani 0.5 1 d D U P B -2
H33A H 0.273504 0.653213 0.599803 0.093 Uiso 0.5 1 calc R U P B -2
C34 C 0.1864(18) 0.7808(12) 0.5697(11) 0.079(4) Uani 0.5 1 d D U P B -2
H34A H 0.132660 0.769446 0.588392 0.094 Uiso 0.5 1 calc R U P B -2
C35 C 0.185(2) 0.8661(13) 0.5333(12) 0.079(4) Uani 0.5 1 d D U P B -2
C36 C 0.2679(18) 0.8856(14) 0.5113(12) 0.077(4) Uani 0.5 1 d D U P B -2
H36A H 0.270243 0.945315 0.490987 0.092 Uiso 0.5 1 calc R U P B -2
C37 C 0.350(2) 0.8151(16) 0.5194(16) 0.076(6) Uani 0.5 1 d D U P B -2
H37A H 0.405385 0.825285 0.501963 0.091 Uiso 0.5 1 calc R U P B -2
C38 C 0.112(4) 0.936(3) 0.529(2) 0.089(5) Uani 0.5 1 d D U P B -2
C39 C 0.0509(12) 0.9493(9) 0.5707(8) 0.106(3) Uani 1 1 d D U . B -2
H39A H 0.076100 0.913550 0.616093 0.127 Uiso 1 1 calc R U . B -2
C40 C -0.0443(12) 1.0110(9) 0.5509(8) 0.110(4) Uani 1 1 d D U . B -2
H40A H -0.079485 1.016586 0.582861 0.132 Uiso 1 1 calc R U . B -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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O10 1.721(6) . ?
U1 O9 1.734(6) . ?
U1 O6 2.436(5) . ?
U1 O4 2.441(5) 4_566 ?
U1 O1 2.468(5) . ?
U1 O3 2.480(5) 4_566 ?
U1 O5 2.496(5) . ?
U1 O2 2.505(5) . ?
U1 C13 2.826(7) . ?
U1 C12 2.840(6) 4_566 ?
U1 C1 2.867(7) . ?
O1 C1 1.253(8) . ?
O2 C1 1.251(8) . ?
O3 C12 1.260(8) . ?
O4 C12 1.258(8) . ?
O5 C13 1.258(8) . ?
O6 C13 1.257(8) . ?
O7 C24 1.25(3) . ?
O8 C24 1.29(2) . ?
C1 C2 1.509(9) . ?
C2 C3 1.374(10) . ?
C2 C11 1.421(9) . ?
C3 C4 1.404(9) . ?
C3 H3A 0.9300 . ?
C4 C5 1.371(9) . ?
C4 H4A 0.9300 . ?
C5 C6 1.426(9) . ?
C5 C12 1.492(9) . ?
C6 C7 1.419(9) . ?
C6 C11 1.421(9) . ?
C7 C8 1.363(11) . ?
C7 H7A 0.9300 . ?
C8 C9 1.387(12) . ?
C8 H8A 0.9300 . ?
C9 C10 1.360(11) . ?
C9 H9A 0.9300 . ?
C10 C11 1.418(10) . ?
C10 H10A 0.9300 . ?
C13 C14 1.500(9) . ?
C14 C15 1.357(11) . ?
C14 C23 1.419(10) . ?
C15 C16 1.409(11) . ?
C15 H15A 0.9300 . ?
C16 C17 1.355(14) . ?
C16 H16A 0.9300 . ?
C17 C18 1.418(14) . ?
C17 C24 1.507(15) . ?
C18 C23 1.414(11) . ?
C18 C19 1.428(14) . ?
C19 C20 1.340(18) . ?
C19 H19A 0.9300 . ?
C20 C21 1.382(18) . ?
C20 H20A 0.9300 . ?
C21 C22 1.358(13) . ?
C21 H21A 0.9300 . ?
C22 C23 1.418(11) . ?
C22 H22A 0.9300 . ?
N1 C25 1.311(15) . ?
N1 C29 1.315(15) . ?
N1 H1A 0.9000 . ?
N2 C32 1.312(19) . ?
N2 H2A 0.9001 . ?
C25 C26 1.383(17) . ?
C25 H25A 0.9300 . ?
C26 C27 1.385(15) . ?
C26 H26A 0.9300 . ?
C27 C30 1.33(4) . ?
C27 C28 1.385(16) . ?
C28 C29 1.387(17) . ?
C28 H28A 0.9300 . ?
C29 H29A 0.9300 . ?
C30 C31 1.39(6) . ?
C31 C32 1.367(13) . ?
C31 H31A 0.9300 . ?
C32 H32A 0.9300 . ?
N3 C37 1.313(16) . ?
N3 C33 1.317(16) . ?
N3 H3B 0.9001 . ?
N4 C40 1.309(17) . ?
N4 H4B 0.9000 . ?
C33 C34 1.391(18) . ?
C33 H33A 0.9300 . ?
C34 C35 1.384(16) . ?
C34 H34A 0.9300 . ?
C35 C38 1.33(4) . ?
C35 C36 1.34(3) . ?
C36 C37 1.388(18) . ?
C36 H36A 0.9300 . ?
C37 H37A 0.9300 . ?
C38 C39 1.38(2) . ?
C39 C40 1.382(13) . ?
C39 H39A 0.9300 . ?
C40 H40A 0.9300 . ?

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
O10 U1 O9 178.3(3) . . ?
O10 U1 O6 87.5(2) . . ?
O9 U1 O6 90.9(2) . . ?
O10 U1 O4 88.6(3) . 4_566 ?
O9 U1 O4 92.7(2) . 4_566 ?
O6 U1 O4 120.63(16) . 4_566 ?
O10 U1 O1 94.5(3) . . ?
O9 U1 O1 87.0(3) . . ?
O6 U1 O1 173.41(18) . . ?
O4 U1 O1 65.75(17) 4_566 . ?
O10 U1 O3 87.0(2) . 4_566 ?
O9 U1 O3 92.9(2) . 4_566 ?
O6 U1 O3 68.28(15) . 4_566 ?
O4 U1 O3 52.36(15) 4_566 4_566 ?
O1 U1 O3 118.05(16) . 4_566 ?
O10 U1 O5 86.5(2) . . ?
O9 U1 O5 92.1(2) . . ?
O6 U1 O5 52.39(16) . . ?
O4 U1 O5 171.64(17) 4_566 . ?
O1 U1 O5 121.40(16) . . ?
O3 U1 O5 120.50(15) 4_566 . ?
O10 U1 O2 87.0(3) . . ?
O9 U1 O2 93.3(2) . . ?
O6 U1 O2 122.36(16) . . ?
O4 U1 O2 116.54(16) 4_566 . ?
O1 U1 O2 51.62(16) . . ?
O3 U1 O2 167.54(17) 4_566 . ?
O5 U1 O2 70.01(16) . . ?
O10 U1 C13 83.5(2) . . ?
O9 U1 C13 94.8(2) . . ?
O6 U1 C13 26.33(17) . . ?
O4 U1 C13 145.97(18) 4_566 . ?
O1 U1 C13 147.70(18) . . ?
O3 U1 C13 94.09(17) 4_566 . ?
O5 U1 C13 26.43(17) . . ?
O2 U1 C13 96.11(18) . . ?
O10 U1 C12 85.8(3) . 4_566 ?
O9 U1 C12 94.9(2) . 4_566 ?
O6 U1 C12 94.48(18) . 4_566 ?
O4 U1 C12 26.18(17) 4_566 4_566 ?
O1 U1 C12 91.93(18) . 4_566 ?
O3 U1 C12 26.29(17) 4_566 4_566 ?
O5 U1 C12 146.27(18) . 4_566 ?
O2 U1 C12 142.06(18) . 4_566 ?
C13 U1 C12 119.91(19) . 4_566 ?
O10 U1 C1 90.8(3) . . ?
O9 U1 C1 90.3(3) . . ?
O6 U1 C1 148.12(18) . . ?
O4 U1 C1 91.12(18) 4_566 . ?
O1 U1 C1 25.80(18) . . ?
O3 U1 C1 143.43(18) 4_566 . ?
O5 U1 C1 95.73(18) . . ?
O2 U1 C1 25.82(17) . . ?
C13 U1 C1 121.9(2) . . ?
C12 U1 C1 117.1(2) 4_566 . ?
C1 O1 U1 95.2(4) . . ?
C1 O2 U1 93.5(4) . . ?
C12 O3 U1 93.0(4) . 4_565 ?
C12 O4 U1 94.9(4) . 4_565 ?
C13 O5 U1 91.6(4) . . ?
C13 O6 U1 94.4(4) . . ?
O2 C1 O1 119.7(6) . . ?
O2 C1 C2 120.5(6) . . ?
O1 C1 C2 119.6(6) . . ?
O2 C1 U1 60.7(4) . . ?
O1 C1 U1 59.0(4) . . ?
C2 C1 U1 176.6(6) . . ?
C3 C2 C11 121.1(6) . . ?
C3 C2 C1 117.3(6) . . ?
C11 C2 C1 121.6(6) . . ?
C2 C3 C4 119.7(6) . . ?
C2 C3 H3A 120.1 . . ?
C4 C3 H3A 120.1 . . ?
C5 C4 C3 120.9(7) . . ?
C5 C4 H4A 119.6 . . ?
C3 C4 H4A 119.6 . . ?
C4 C5 C6 120.2(6) . . ?
C4 C5 C12 117.2(6) . . ?
C6 C5 C12 122.6(6) . . ?
C7 C6 C11 118.6(6) . . ?
C7 C6 C5 122.5(6) . . ?
C11 C6 C5 118.9(6) . . ?
C8 C7 C6 120.3(7) . . ?
C8 C7 H7A 119.8 . . ?
C6 C7 H7A 119.8 . . ?
C7 C8 C9 121.5(7) . . ?
C7 C8 H8A 119.3 . . ?
C9 C8 H8A 119.3 . . ?
C10 C9 C8 119.8(7) . . ?
C10 C9 H9A 120.1 . . ?
C8 C9 H9A 120.1 . . ?
C9 C10 C11 121.4(7) . . ?
C9 C10 H10A 119.3 . . ?
C11 C10 H10A 119.3 . . ?
C10 C11 C2 123.0(6) . . ?
C10 C11 C6 118.4(6) . . ?
C2 C11 C6 118.5(6) . . ?
O4 C12 O3 119.2(6) . . ?
O4 C12 C5 120.4(6) . . ?
O3 C12 C5 120.4(6) . . ?
O4 C12 U1 58.9(3) . 4_565 ?
O3 C12 U1 60.7(3) . 4_565 ?
C5 C12 U1 174.0(5) . 4_565 ?
O6 C13 O5 120.0(6) . . ?
O6 C13 C14 119.6(6) . . ?
O5 C13 C14 120.4(6) . . ?
O6 C13 U1 59.3(3) . . ?
O5 C13 U1 62.0(4) . . ?
C14 C13 U1 168.4(5) . . ?
C15 C14 C23 120.7(7) . . ?
C15 C14 C13 119.0(7) . . ?
C23 C14 C13 120.3(7) . . ?
C14 C15 C16 119.8(9) . . ?
C14 C15 H15A 120.1 . . ?
C16 C15 H15A 120.1 . . ?
C17 C16 C15 121.2(9) . . ?
C17 C16 H16A 119.4 . . ?
C15 C16 H16A 119.4 . . ?
C16 C17 C18 120.4(8) . . ?
C16 C17 C24 117.8(11) . . ?
C18 C17 C24 121.6(12) . . ?
C23 C18 C17 118.7(8) . . ?
C23 C18 C19 117.3(10) . . ?
C17 C18 C19 124.1(9) . . ?
C20 C19 C18 121.5(11) . . ?
C20 C19 H19A 119.2 . . ?
C18 C19 H19A 119.2 . . ?
C19 C20 C21 121.9(11) . . ?
C19 C20 H20A 119.1 . . ?
C21 C20 H20A 119.1 . . ?
C22 C21 C20 118.4(11) . . ?
C22 C21 H21A 120.8 . . ?
C20 C21 H21A 120.8 . . ?
C21 C22 C23 122.6(10) . . ?
C21 C22 H22A 118.7 . . ?
C23 C22 H22A 118.7 . . ?
C18 C23 C22 118.1(8) . . ?
C18 C23 C14 119.2(8) . . ?
C22 C23 C14 122.7(7) . . ?
O7 C24 O8 125.4(13) . . ?
O7 C24 C17 115.5(18) . . ?
O8 C24 C17 119(2) . . ?
C25 N1 C29 124(2) . . ?
C25 N1 H1A 117.9 . . ?
C29 N1 H1A 117.9 . . ?
C32 N2 H2A 121.0 . . ?
N1 C25 C26 119.3(19) . . ?
N1 C25 H25A 120.3 . . ?
C26 C25 H25A 120.3 . . ?
C25 C26 C27 120.0(18) . . ?
C25 C26 H26A 120.0 . . ?
C27 C26 H26A 120.0 . . ?
C30 C27 C26 121(3) . . ?
C30 C27 C28 122(3) . . ?
C26 C27 C28 117.3(17) . . ?
C27 C28 C29 120.8(18) . . ?
C27 C28 H28A 119.6 . . ?
C29 C28 H28A 119.6 . . ?
N1 C29 C28 118(2) . . ?
N1 C29 H29A 120.9 . . ?
C28 C29 H29A 120.9 . . ?
C27 C30 C31 124(3) . . ?
C32 C31 C30 123.6(18) . . ?
C32 C31 H31A 118.2 . . ?
C30 C31 H31A 118.2 . . ?
N2 C32 C31 120(2) . . ?
N2 C32 H32A 120.0 . . ?
C31 C32 H32A 120.0 . . ?
C37 N3 C33 125(2) . . ?
C37 N3 H3B 117.4 . . ?
C33 N3 H3B 117.8 . . ?
C40 N4 H4B 116.9 . . ?
N3 C33 C34 119(2) . . ?
N3 C33 H33A 120.6 . . ?
C34 C33 H33A 120.6 . . ?
C35 C34 C33 117(2) . . ?
C35 C34 H34A 121.3 . . ?
C33 C34 H34A 121.3 . . ?
C38 C35 C36 118(2) . . ?
C38 C35 C34 120(2) . . ?
C36 C35 C34 121(2) . . ?
C35 C36 C37 119(2) . . ?
C35 C36 H36A 120.5 . . ?
C37 C36 H36A 120.5 . . ?
N3 C37 C36 118(2) . . ?
N3 C37 H37A 120.8 . . ?
C36 C37 H37A 120.8 . . ?
C35 C38 C39 130(3) . . ?
C38 C39 C40 126(2) . . ?
C38 C39 H39A 117.1 . . ?
C40 C39 H39A 117.1 . . ?
N4 C40 C39 119.3(17) . . ?
N4 C40 H40A 120.3 . . ?
C39 C40 H40A 120.3 . . ?

_refine_diff_density_max         1.929
_refine_diff_density_min         -3.575
_refine_diff_density_rms         0.174

####################################################################### 
# 
# 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_shx97_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1575475'
_audit_update_record             
;
2017-09-20 deposited with the CCDC.
2018-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2 (C24 H13 O10 U), C13 H16 N2, 2(H2 O)'
_chemical_formula_sum            'C61 H46 N2 O22 U2'
_chemical_formula_weight         1635.06

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

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

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

_cell_length_a                   19.736(4)
_cell_length_b                   13.954(3)
_cell_length_c                   21.808(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6006(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    46383
_cell_measurement_theta_min      3.64
_cell_measurement_theta_max      25.35

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_F_000             3144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    5.467
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.211
_exptl_absorpt_correction_T_max  0.269
_exptl_absorpt_process_details   ABSCOR(Higashi,1995)
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'rigaku r-axis rapid'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 0
_diffrn_reflns_number            46383
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.097
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             10989
_reflns_number_gt                9257
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_max     0.994
_reflns_Friedel_fraction_full    0.994

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0701P)²+53.1988P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10948
_refine_ls_number_parameters     784
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1437
_refine_ls_wR_factor_gt          0.1288
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U -0.40940(3) -0.03817(4) -0.24139(3) 0.03112(18) Uani 1 1 d . . . . .
O1 O -0.4734(5) -0.1901(8) -0.2409(12) 0.047(3) Uani 1 1 d . . . . .
O2 O -0.5344(6) -0.0615(9) -0.2486(11) 0.053(4) Uani 1 1 d . . . . .
O3 O -0.8381(6) -0.3167(8) -0.2505(10) 0.046(4) Uani 1 1 d . . . . .
O4 O -0.7852(6) -0.4525(9) -0.2342(12) 0.057(5) Uani 1 1 d . . . . .
O5 O -0.4724(7) 0.1123(9) -0.2374(14) 0.062(4) Uani 1 1 d . . . . .
O6 O -0.3632(8) 0.1283(10) -0.2431(14) 0.071(5) Uani 1 1 d . . . . .
O7 O -0.3907(16) 0.6246(13) -0.2567(12) 0.126(9) Uani 1 1 d . U . . .
H7 H -0.373399 0.688127 -0.255198 0.189 Uiso 1 1 d R U . . .
O8 O -0.478(2) 0.6137(15) -0.3206(13) 0.169(16) Uani 1 1 d . . . . .
O9 O -0.4107(8) -0.0400(11) -0.1536(11) 0.056(6) Uani 1 1 d . . . . .
O10 O -0.4083(7) -0.0352(10) -0.3159(8) 0.041(5) Uani 1 1 d . . . . .
C1 C -0.5945(8) -0.2088(11) -0.2393(14) 0.040(4) Uani 1 1 d . . . . .
C2 C -0.6468(9) -0.1859(15) -0.2787(10) 0.046(5) Uani 1 1 d . . . . .
H2A H -0.640368 -0.137584 -0.307430 0.055 Uiso 1 1 calc R U . . .
C3 C -0.7091(10) -0.2332(15) -0.2765(10) 0.048(5) Uani 1 1 d . . . . .
H3A H -0.744186 -0.214577 -0.302408 0.058 Uiso 1 1 calc R U . . .
C4 C -0.7184(8) -0.3088(12) -0.2351(12) 0.038(4) Uani 1 1 d . . . . .
C5 C -0.6782(11) -0.3965(14) -0.1395(10) 0.047(5) Uani 1 1 d . . . . .
H5A H -0.719495 -0.427963 -0.135873 0.056 Uiso 1 1 calc R U . . .
C6 C -0.6294(13) -0.4115(17) -0.0984(12) 0.056(6) Uani 1 1 d . . . . .
H6A H -0.638243 -0.452559 -0.065763 0.067 Uiso 1 1 calc R U . . .
C7 C -0.5657(12) -0.3683(19) -0.1020(12) 0.066(7) Uani 1 1 d . . . . .
H7A H -0.532582 -0.381177 -0.072801 0.079 Uiso 1 1 calc R U . . .
C8 C -0.5534(10) -0.3074(16) -0.1488(11) 0.052(5) Uani 1 1 d . . . . .
H8A H -0.510626 -0.279847 -0.151835 0.062 Uiso 1 1 calc R U . . .
C9 C -0.6666(9) -0.3308(13) -0.1901(9) 0.039(4) Uani 1 1 d . . . . .
C10 C -0.6033(10) -0.2833(15) -0.1942(9) 0.045(5) Uani 1 1 d . . . . .
C11 C -0.5301(8) -0.1508(12) -0.2415(13) 0.037(4) Uani 1 1 d . . . . .
C12 C -0.7830(9) -0.3627(12) -0.2372(14) 0.043(4) Uani 1 1 d . . . . .
C13 C -0.4346(15) 0.2740(17) -0.2530(14) 0.071(8) Uani 1 1 d . . . . .
C14 C -0.3775(17) 0.3240(18) -0.2649(12) 0.074(8) Uani 1 1 d . . . . .
H14A H -0.336239 0.292212 -0.267788 0.089 Uiso 1 1 calc R U . . .
C15 C -0.380(2) 0.428(2) -0.2732(14) 0.086(10) Uani 1 1 d . . . . .
H15A H -0.341105 0.462707 -0.280028 0.103 Uiso 1 1 calc R U . . .
C16 C -0.439(2) 0.470(2) -0.2708(12) 0.083(9) Uani 1 1 d . U . . .
C17 C -0.561(2) 0.473(2) -0.2540(12) 0.093(11) Uani 1 1 d . . . . .
H17A H -0.561568 0.539462 -0.257701 0.112 Uiso 1 1 calc R U . . .
C18 C -0.622(3) 0.421(3) -0.242(3) 0.140(18) Uani 1 1 d . . . . .
H18A H -0.663943 0.452111 -0.240094 0.168 Uiso 1 1 calc R U . . .
C19 C -0.617(2) 0.327(3) -0.235(2) 0.135(17) Uani 1 1 d . . . . .
H19A H -0.656351 0.293236 -0.226616 0.162 Uiso 1 1 calc R U . . .
C20 C -0.5587(16) 0.275(2) -0.2395(19) 0.108(12) Uani 1 1 d . . . . .
H20A H -0.560647 0.208582 -0.235061 0.130 Uiso 1 1 calc R U . . .
C21 C -0.500(2) 0.4227(19) -0.2597(11) 0.083(9) Uani 1 1 d . U . . .
C22 C -0.4971(13) 0.3179(14) -0.2503(12) 0.061(6) Uani 1 1 d . . . . .
C23 C -0.4239(11) 0.1661(12) -0.2444(17) 0.052(5) Uani 1 1 d . . . . .
C24 C -0.442(2) 0.578(2) -0.2858(16) 0.106(13) Uani 1 1 d . . . . .
U2 U -0.74574(3) -0.04286(4) -0.44177(3) 0.03090(18) Uani 1 1 d . . . . .
O11 O -0.8105(6) -0.1957(8) -0.4362(11) 0.050(4) Uani 1 1 d . . . . .
O12 O -0.8684(6) -0.0660(9) -0.4536(10) 0.052(5) Uani 1 1 d . . . . .
O13 O -1.1213(6) -0.4520(9) -0.4354(12) 0.056(5) Uani 1 1 d . . . . .
O14 O -1.1728(6) -0.3145(9) -0.4415(11) 0.050(3) Uani 1 1 d . . . . .
O15 O -0.8068(6) 0.1130(8) -0.4418(12) 0.049(3) Uani 1 1 d . . . . .
O16 O -0.6972(7) 0.1176(10) -0.4435(16) 0.075(6) Uani 1 1 d . . . . .
O17 O -0.7717(11) 0.6195(12) -0.4205(9) 0.077(5) Uani 1 1 d . . . . .
H17 H -0.785127 0.684341 -0.425941 0.115 Uiso 1 1 d R U . . .
O18 O -0.7740(18) 0.6116(15) -0.5220(14) 0.137(12) Uani 1 1 d . . . . .
O19 O -0.7416(8) -0.0455(11) -0.5179(9) 0.045(5) Uani 1 1 d . . . . .
O20 O -0.7489(7) -0.0373(11) -0.3546(11) 0.051(5) Uani 1 1 d . . . . .
C25 C -0.9291(8) -0.2153(13) -0.4548(10) 0.041(5) Uani 1 1 d . . . . .
C26 C -0.9396(10) -0.2866(15) -0.4106(11) 0.052(6) Uani 1 1 d . . . . .
H26A H -0.906130 -0.300643 -0.381938 0.063 Uiso 1 1 calc R U . . .
C27 C -1.0014(10) -0.3364(14) -0.4102(10) 0.045(5) Uani 1 1 d . . . . .
H27A H -1.008138 -0.385038 -0.381652 0.054 Uiso 1 1 calc R U . . .
C28 C -1.0518(9) -0.3152(12) -0.4506(11) 0.040(5) Uani 1 1 d . . . . .
C29 C -1.0899(11) -0.2259(16) -0.5463(11) 0.057(6) Uani 1 1 d . . . . .
H29A H -1.131407 -0.257435 -0.545801 0.068 Uiso 1 1 calc R U . . .
C30 C -1.0769(13) -0.163(2) -0.5908(10) 0.064(7) Uani 1 1 d . . . . .
H30A H -1.109859 -0.152537 -0.620427 0.077 Uiso 1 1 calc R U . . .
C31 C -1.0166(14) -0.114(2) -0.5948(12) 0.068(7) Uani 1 1 d . . . . .
H31A H -1.008054 -0.072783 -0.627185 0.082 Uiso 1 1 calc R U . . .
C32 C -0.9700(14) -0.1291(18) -0.5499(12) 0.064(7) Uani 1 1 d . . . . .
H32A H -0.929865 -0.094328 -0.551442 0.077 Uiso 1 1 calc R U . . .
C33 C -1.0418(9) -0.2458(15) -0.4992(9) 0.043(5) Uani 1 1 d . . . . .
C34 C -0.9792(9) -0.1944(14) -0.5009(9) 0.039(4) Uani 1 1 d . . . . .
C35 C -0.8660(8) -0.1575(13) -0.4467(13) 0.045(5) Uani 1 1 d . . . . .
C36 C -1.1182(8) -0.3634(12) -0.4412(13) 0.039(4) Uani 1 1 d . . . . .
C37 C -0.7557(10) 0.2665(13) -0.4548(14) 0.054(7) Uani 1 1 d . . . . .
C38 C -0.7862(11) 0.3235(15) -0.4124(13) 0.062(7) Uani 1 1 d . . . . .
H38A H -0.806959 0.293557 -0.379261 0.074 Uiso 1 1 calc R U . . .
C39 C -0.7887(12) 0.4225(16) -0.4148(11) 0.057(6) Uani 1 1 d . . . . .
H39A H -0.809486 0.458318 -0.384078 0.068 Uiso 1 1 calc R U . . .
C40 C -0.7580(13) 0.4667(16) -0.4665(16) 0.067(8) Uani 1 1 d . . . . .
C41 C -0.688(2) 0.4539(19) -0.5603(15) 0.095(11) Uani 1 1 d . . . . .
H41A H -0.687592 0.520315 -0.564232 0.114 Uiso 1 1 calc R U . . .
C42 C -0.652(2) 0.399(3) -0.6036(16) 0.104(12) Uani 1 1 d . . . . .
H42A H -0.628046 0.428482 -0.634817 0.124 Uiso 1 1 calc R U . . .
C43 C -0.6534(19) 0.299(3) -0.5996(15) 0.102(11) Uani 1 1 d . . . . .
H43A H -0.631407 0.261220 -0.628580 0.122 Uiso 1 1 calc R U . . .
C44 C -0.6875(13) 0.2585(18) -0.5524(12) 0.067(7) Uani 1 1 d . . . . .
H44A H -0.688779 0.191983 -0.550234 0.080 Uiso 1 1 calc R U . . .
C45 C -0.7219(12) 0.4128(17) -0.5125(11) 0.056(6) Uani 1 1 d . . . . .
C46 C -0.7209(11) 0.3106(15) -0.5066(10) 0.048(5) Uani 1 1 d . . . . .
C47 C -0.7533(10) 0.1601(12) -0.4460(18) 0.046(5) Uani 1 1 d . . . . .
C48 C -0.7686(14) 0.5709(17) -0.4733(13) 0.063(6) Uani 1 1 d . . . . .
N1 N -0.867(3) 0.538(5) -0.636(3) 0.18(3) Uani 1 1 d . . . . .
H1A H -0.839870 0.566845 -0.660382 0.216 Uiso 1 1 calc R U . . .
N2 N -1.0498(16) 0.0528(19) -0.4120(12) 0.085(7) Uani 1 1 d . . . . .
H2B H -1.059591 -0.007268 -0.411106 0.102 Uiso 1 1 calc R U . . .
C49 C -0.896(2) 0.402(3) -0.5837(19) 0.102(11) Uani 1 1 d . . . . .
H49A H -0.886034 0.339100 -0.572648 0.123 Uiso 1 1 calc R U . . .
C50 C -0.855(3) 0.450(6) -0.622(3) 0.16(3) Uani 1 1 d . . . . .
H50A H -0.817733 0.418889 -0.638452 0.194 Uiso 1 1 calc R U . . .
C51 C -0.921(4) 0.586(3) -0.612(3) 0.15(2) Uani 1 1 d . . . . .
H51A H -0.925140 0.651489 -0.618650 0.183 Uiso 1 1 calc R U . . .
C52 C -0.969(3) 0.539(3) -0.5782(19) 0.123(16) Uani 1 1 d . . . . .
H52A H -1.010341 0.567386 -0.567916 0.148 Uiso 1 1 calc R U . . .
C53 C -0.9528(19) 0.449(3) -0.5609(15) 0.090(10) Uani 1 1 d . . . . .
C54 C -1.0023(18) 0.389(3) -0.5152(14) 0.098(10) Uani 1 1 d . . . . .
H54A H -1.047381 0.416135 -0.515327 0.118 Uiso 1 1 calc R U . . .
H54B H -1.005528 0.322467 -0.528786 0.118 Uiso 1 1 calc R U . . .
C55 C -0.971(2) 0.393(3) -0.4491(17) 0.104(11) Uani 1 1 d . . . . .
H55A H -0.926920 0.363192 -0.449504 0.125 Uiso 1 1 calc R U . . .
H55B H -0.965548 0.459519 -0.437355 0.125 Uiso 1 1 calc R U . . .
C56 C -1.011(2) 0.348(3) -0.4062(19) 0.116(13) Uani 1 1 d . U . . .
H56A H -1.055711 0.377442 -0.407195 0.140 Uiso 1 1 calc R U . . .
H56B H -0.992114 0.360262 -0.366071 0.140 Uiso 1 1 calc R U . . .
C57 C -1.0210(16) 0.240(2) -0.4123(13) 0.077(8) Uani 1 1 d . . . . .
C58 C -1.0829(16) 0.208(2) -0.4006(14) 0.082(8) Uani 1 1 d . . . . .
H58A H -1.117458 0.251267 -0.391056 0.098 Uiso 1 1 calc R U . . .
C59 C -1.0957(16) 0.111(3) -0.4026(15) 0.090(9) Uani 1 1 d . . . . .
H59A H -1.139712 0.089302 -0.396851 0.108 Uiso 1 1 calc R U . . .
C60 C -0.9879(19) 0.077(3) -0.4231(14) 0.089(10) Uani 1 1 d . U . . .
H60A H -0.954234 0.031768 -0.429366 0.107 Uiso 1 1 calc R U . . .
C61 C -0.9733(16) 0.177(3) -0.4253(12) 0.082(8) Uani 1 1 d . U . . .
H61A H -0.930131 0.198432 -0.436018 0.098 Uiso 1 1 calc R U . . .
O21 O -1.1159(16) -0.1172(18) -0.3851(13) 0.129(10) Uani 1 1 d . . . . .
H211 H -1.158492 -0.127415 -0.384025 0.194 Uiso 1 1 d R U . . .
H212 H -1.099964 -0.145027 -0.353641 0.194 Uiso 1 1 d R U . . .
O22 O -0.643(3) 0.079(3) -0.283(3) 0.36(5) Uani 1 1 d . . . . .
H221 H -0.672688 0.047097 -0.302632 0.544 Uiso 1 1 d R U . . .
H222 H -0.612467 0.039917 -0.274081 0.544 Uiso 1 1 d R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O10 1.626(17) . ?
U1 O9 1.91(2) . ?
U1 O5 2.441(12) . ?
U1 O4 2.459(13) 4_545 ?
U1 O1 2.467(11) . ?
U1 O3 2.475(11) 4_545 ?
U1 O2 2.493(12) . ?
U1 O6 2.497(13) . ?
U1 C11 2.854(15) . ?
U1 C12 2.855(17) 4_545 ?
U1 C23 2.865(17) . ?
O1 C11 1.246(19) . ?
O2 C11 1.26(2) . ?
O3 C12 1.30(2) . ?
O4 C12 1.26(2) . ?
O5 C23 1.23(2) . ?
O6 C23 1.31(2) . ?
O7 C24 1.37(4) . ?
O7 H7 0.9499 . ?
O8 C24 1.15(4) . ?
C1 C2 1.38(3) . ?
C1 C10 1.44(3) . ?
C1 C11 1.51(2) . ?
C2 C3 1.40(3) . ?
C2 H2A 0.9300 . ?
C3 C4 1.40(3) . ?
C3 H3A 0.9300 . ?
C4 C9 1.45(3) . ?
C4 C12 1.48(2) . ?
C5 C6 1.33(3) . ?
C5 C9 1.45(3) . ?
C5 H5A 0.9300 . ?
C6 C7 1.40(3) . ?
C6 H6A 0.9300 . ?
C7 C8 1.35(3) . ?
C7 H7A 0.9300 . ?
C8 C10 1.44(3) . ?
C8 H8A 0.9300 . ?
C9 C10 1.42(3) . ?
C13 C14 1.35(4) . ?
C13 C22 1.38(4) . ?
C13 C23 1.53(3) . ?
C14 C15 1.46(4) . ?
C14 H14A 0.9300 . ?
C15 C16 1.30(5) . ?
C15 H15A 0.9300 . ?
C16 C21 1.40(5) . ?
C16 C24 1.54(4) . ?
C17 C21 1.40(5) . ?
C17 C18 1.43(6) . ?
C17 H17A 0.9300 . ?
C18 C19 1.33(5) . ?
C18 H18A 0.9300 . ?
C19 C20 1.36(4) . ?
C19 H19A 0.9300 . ?
C20 C22 1.38(4) . ?
C20 H20A 0.9300 . ?
C21 C22 1.48(3) . ?
U2 O19 1.662(19) . ?
U2 O20 1.90(2) . ?
U2 O16 2.436(14) . ?
U2 O12 2.455(12) . ?
U2 O14 2.456(11) 4_545 ?
U2 O13 2.462(13) 4_545 ?
U2 O15 2.486(12) . ?
U2 O11 2.489(11) . ?
U2 C47 2.837(17) . ?
U2 C36 2.836(16) 4_545 ?
U2 C35 2.865(17) . ?
O11 C35 1.24(2) . ?
O12 C35 1.29(2) . ?
O13 C36 1.24(2) . ?
O14 C36 1.27(2) . ?
O15 C47 1.25(2) . ?
O16 C47 1.26(2) . ?
O17 C48 1.34(3) . ?
O17 H17 0.9498 . ?
O18 C48 1.21(3) . ?
C25 C26 1.40(3) . ?
C25 C34 1.44(3) . ?
C25 C35 1.49(2) . ?
C26 C27 1.41(3) . ?
C26 H26A 0.9300 . ?
C27 C28 1.36(3) . ?
C27 H27A 0.9300 . ?
C28 C33 1.45(3) . ?
C28 C36 1.49(2) . ?
C29 C30 1.33(3) . ?
C29 C33 1.43(3) . ?
C29 H29A 0.9300 . ?
C30 C31 1.37(4) . ?
C30 H30A 0.9300 . ?
C31 C32 1.36(4) . ?
C31 H31A 0.9300 . ?
C32 C34 1.42(3) . ?
C32 H32A 0.9300 . ?
C33 C34 1.43(3) . ?
C37 C38 1.36(3) . ?
C37 C46 1.46(3) . ?
C37 C47 1.50(2) . ?
C38 C39 1.38(3) . ?
C38 H38A 0.9300 . ?
C39 C40 1.42(4) . ?
C39 H39A 0.9300 . ?
C40 C45 1.44(4) . ?
C40 C48 1.48(3) . ?
C41 C45 1.37(4) . ?
C41 C42 1.40(5) . ?
C41 H41A 0.9300 . ?
C42 C43 1.39(5) . ?
C42 H42A 0.9300 . ?
C43 C44 1.35(4) . ?
C43 H43A 0.9300 . ?
C44 C46 1.40(3) . ?
C44 H44A 0.9300 . ?
C45 C46 1.43(3) . ?
N1 C50 1.29(7) . ?
N1 C51 1.37(7) . ?
N1 H1A 0.8600 . ?
N2 C59 1.24(4) . ?
N2 C60 1.29(4) . ?
N2 H2B 0.8600 . ?
C49 C50 1.33(7) . ?
C49 C53 1.40(5) . ?
C49 H49A 0.9300 . ?
C50 H50A 0.9300 . ?
C51 C52 1.37(7) . ?
C51 H51A 0.9300 . ?
C52 C53 1.36(4) . ?
C52 H52A 0.9300 . ?
C53 C54 1.63(5) . ?
C54 C55 1.57(4) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C55 C56 1.38(5) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C56 C57 1.52(5) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C57 C61 1.32(4) . ?
C57 C58 1.32(4) . ?
C58 C59 1.38(5) . ?
C58 H58A 0.9300 . ?
C59 H59A 0.9300 . ?
C60 C61 1.43(5) . ?
C60 H60A 0.9300 . ?
C61 H61A 0.9300 . ?
O21 H211 0.8521 . ?
O21 H212 0.8483 . ?
O22 H221 0.8400 . ?
O22 H222 0.8401 . ?

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
O10 U1 O9 179.3(6) . . ?
O10 U1 O5 91.2(9) . . ?
O9 U1 O5 88.3(9) . . ?
O10 U1 O4 92.9(8) . 4_545 ?
O9 U1 O4 87.1(8) . 4_545 ?
O5 U1 O4 123.4(4) . 4_545 ?
O10 U1 O1 91.9(8) . . ?
O9 U1 O1 88.7(8) . . ?
O5 U1 O1 118.5(4) . . ?
O4 U1 O1 117.7(4) 4_545 . ?
O10 U1 O3 86.2(7) . 4_545 ?
O9 U1 O3 94.4(7) . 4_545 ?
O5 U1 O3 175.1(6) . 4_545 ?
O4 U1 O3 52.8(4) 4_545 4_545 ?
O1 U1 O3 65.7(4) . 4_545 ?
O10 U1 O2 87.4(7) . . ?
O9 U1 O2 92.8(7) . . ?
O5 U1 O2 67.1(4) . . ?
O4 U1 O2 169.5(4) 4_545 . ?
O1 U1 O2 51.8(4) . . ?
O3 U1 O2 116.8(4) 4_545 . ?
O10 U1 O6 87.5(9) . . ?
O9 U1 O6 91.9(9) . . ?
O5 U1 O6 52.2(5) . . ?
O4 U1 O6 71.7(5) 4_545 . ?
O1 U1 O6 170.6(5) . . ?
O3 U1 O6 123.5(5) 4_545 . ?
O2 U1 O6 118.8(5) . . ?
O10 U1 C11 91.4(7) . . ?
O9 U1 C11 89.0(7) . . ?
O5 U1 C11 92.8(4) . . ?
O4 U1 C11 143.4(4) 4_545 . ?
O1 U1 C11 25.8(4) . . ?
O3 U1 C11 91.4(4) 4_545 . ?
O2 U1 C11 26.1(4) . . ?
O6 U1 C11 144.8(5) . . ?
O10 U1 C12 91.8(8) . 4_545 ?
O9 U1 C12 88.5(8) . 4_545 ?
O5 U1 C12 149.4(5) . 4_545 ?
O4 U1 C12 26.0(4) 4_545 4_545 ?
O1 U1 C12 91.8(4) . 4_545 ?
O3 U1 C12 26.9(5) 4_545 4_545 ?
O2 U1 C12 143.5(4) . 4_545 ?
O6 U1 C12 97.6(5) . 4_545 ?
C11 U1 C12 117.6(5) . 4_545 ?
O10 U1 C23 87.3(9) . . ?
O9 U1 C23 92.0(9) . . ?
O5 U1 C23 25.1(5) . . ?
O4 U1 C23 98.8(5) 4_545 . ?
O1 U1 C23 143.5(5) . . ?
O3 U1 C23 150.4(5) 4_545 . ?
O2 U1 C23 91.7(5) . . ?
O6 U1 C23 27.2(5) . . ?
C11 U1 C23 117.7(5) . . ?
C12 U1 C23 124.8(6) 4_545 . ?
C11 O1 U1 94.7(9) . . ?
C11 O2 U1 93.1(10) . . ?
C12 O3 U1 93.1(10) . 4_445 ?
C12 O4 U1 94.9(11) . 4_445 ?
C23 O5 U1 97.1(12) . . ?
C23 O6 U1 92.3(10) . . ?
C24 O7 H7 136.9 . . ?
C2 C1 C10 120.0(16) . . ?
C2 C1 C11 119.1(19) . . ?
C10 C1 C11 121(2) . . ?
C1 C2 C3 121.9(19) . . ?
C1 C2 H2A 119.0 . . ?
C3 C2 H2A 119.0 . . ?
C2 C3 C4 119.5(17) . . ?
C2 C3 H3A 120.2 . . ?
C4 C3 H3A 120.2 . . ?
C3 C4 C9 120.2(16) . . ?
C3 C4 C12 118.4(19) . . ?
C9 C4 C12 121.4(19) . . ?
C6 C5 C9 119.8(19) . . ?
C6 C5 H5A 120.1 . . ?
C9 C5 H5A 120.1 . . ?
C5 C6 C7 123(2) . . ?
C5 C6 H6A 118.5 . . ?
C7 C6 H6A 118.5 . . ?
C8 C7 C6 118(2) . . ?
C8 C7 H7A 120.8 . . ?
C6 C7 H7A 120.8 . . ?
C7 C8 C10 123(2) . . ?
C7 C8 H8A 118.5 . . ?
C10 C8 H8A 118.5 . . ?
C10 C9 C4 118.7(17) . . ?
C10 C9 C5 118.8(18) . . ?
C4 C9 C5 122.4(17) . . ?
C9 C10 C8 116.8(19) . . ?
C9 C10 C1 119.2(18) . . ?
C8 C10 C1 123.8(18) . . ?
O1 C11 O2 119.8(15) . . ?
O1 C11 C1 121.3(14) . . ?
O2 C11 C1 118.6(14) . . ?
O1 C11 U1 59.5(8) . . ?
O2 C11 U1 60.7(8) . . ?
C1 C11 U1 177.9(19) . . ?
O4 C12 O3 118.4(17) . . ?
O4 C12 C4 122.4(17) . . ?
O3 C12 C4 118.6(15) . . ?
O4 C12 U1 59.1(9) . 4_445 ?
O3 C12 U1 59.9(8) . 4_445 ?
C4 C12 U1 178.5(13) . 4_445 ?
C14 C13 C22 122(2) . . ?
C14 C13 C23 115(3) . . ?
C22 C13 C23 124(2) . . ?
C13 C14 C15 120(3) . . ?
C13 C14 H14A 119.9 . . ?
C15 C14 H14A 119.9 . . ?
C16 C15 C14 119(3) . . ?
C16 C15 H15A 120.5 . . ?
C14 C15 H15A 120.5 . . ?
C15 C16 C21 124(3) . . ?
C15 C16 C24 118(4) . . ?
C21 C16 C24 118(4) . . ?
C21 C17 C18 119(3) . . ?
C21 C17 H17A 120.4 . . ?
C18 C17 H17A 120.4 . . ?
C19 C18 C17 117(4) . . ?
C19 C18 H18A 121.6 . . ?
C17 C18 H18A 121.6 . . ?
C18 C19 C20 126(5) . . ?
C18 C19 H19A 117.0 . . ?
C20 C19 H19A 117.0 . . ?
C19 C20 C22 122(3) . . ?
C19 C20 H20A 119.2 . . ?
C22 C20 H20A 119.2 . . ?
C17 C21 C16 121(3) . . ?
C17 C21 C22 121(3) . . ?
C16 C21 C22 117(3) . . ?
C20 C22 C13 127(2) . . ?
C20 C22 C21 115(2) . . ?
C13 C22 C21 118(3) . . ?
O5 C23 O6 117.8(16) . . ?
O5 C23 C13 121(2) . . ?
O6 C23 C13 121.6(19) . . ?
O5 C23 U1 57.7(9) . . ?
O6 C23 U1 60.6(9) . . ?
C13 C23 U1 174(2) . . ?
O8 C24 O7 124(3) . . ?
O8 C24 C16 126(4) . . ?
O7 C24 C16 110(3) . . ?
O19 U2 O20 178.6(7) . . ?
O19 U2 O16 89.1(10) . . ?
O20 U2 O16 89.5(9) . . ?
O19 U2 O12 86.6(7) . . ?
O20 U2 O12 94.4(7) . . ?
O16 U2 O12 120.4(4) . . ?
O19 U2 O14 87.4(8) . 4_545 ?
O20 U2 O14 92.9(7) . 4_545 ?
O16 U2 O14 121.0(4) . 4_545 ?
O12 U2 O14 118.1(4) . 4_545 ?
O19 U2 O13 90.4(8) . 4_545 ?
O20 U2 O13 88.7(7) . 4_545 ?
O16 U2 O13 68.6(4) . 4_545 ?
O12 U2 O13 170.4(4) . 4_545 ?
O14 U2 O13 52.5(4) 4_545 4_545 ?
O19 U2 O15 92.5(8) . . ?
O20 U2 O15 87.0(7) . . ?
O16 U2 O15 52.1(4) . . ?
O12 U2 O15 68.7(4) . . ?
O14 U2 O15 173.1(4) 4_545 . ?
O13 U2 O15 120.6(4) 4_545 . ?
O19 U2 O11 93.2(8) . . ?
O20 U2 O11 88.2(7) . . ?
O16 U2 O11 172.0(5) . . ?
O12 U2 O11 52.1(4) . . ?
O14 U2 O11 66.8(4) 4_545 . ?
O13 U2 O11 119.0(4) 4_545 . ?
O15 U2 O11 120.0(4) . . ?
O19 U2 C47 89.6(9) . . ?
O20 U2 C47 89.4(9) . . ?
O16 U2 C47 26.1(5) . . ?
O12 U2 C47 94.4(5) . . ?
O14 U2 C47 147.1(5) 4_545 . ?
O13 U2 C47 94.8(5) 4_545 . ?
O15 U2 C47 26.0(5) . . ?
O11 U2 C47 146.1(5) . . ?
O19 U2 C36 87.1(8) . 4_545 ?
O20 U2 C36 92.5(7) . 4_545 ?
O16 U2 C36 94.3(5) . 4_545 ?
O12 U2 C36 144.5(5) . 4_545 ?
O14 U2 C36 26.6(5) 4_545 4_545 ?
O13 U2 C36 26.0(5) 4_545 4_545 ?
O15 U2 C36 146.4(4) . 4_545 ?
O11 U2 C36 93.4(4) . 4_545 ?
C47 U2 C36 120.5(5) . 4_545 ?
O19 U2 C35 89.5(8) . . ?
O20 U2 C35 91.9(7) . . ?
O16 U2 C35 147.0(5) . . ?
O12 U2 C35 26.6(5) . . ?
O14 U2 C35 91.9(5) 4_545 . ?
O13 U2 C35 144.4(5) 4_545 . ?
O15 U2 C35 95.0(4) . . ?
O11 U2 C35 25.6(5) . . ?
C47 U2 C35 120.9(5) . . ?
C36 U2 C35 118.5(5) 4_545 . ?
C35 O11 U2 94.4(10) . . ?
C35 O12 U2 94.8(10) . . ?
C36 O13 U2 94.1(10) . 4_445 ?
C36 O14 U2 93.5(10) . 4_445 ?
C47 O15 U2 92.9(11) . . ?
C47 O16 U2 95.1(11) . . ?
C48 O17 H17 112.8 . . ?
C26 C25 C34 121.5(17) . . ?
C26 C25 C35 115.1(19) . . ?
C34 C25 C35 123.1(18) . . ?
C25 C26 C27 119.0(19) . . ?
C25 C26 H26A 120.5 . . ?
C27 C26 H26A 120.5 . . ?
C28 C27 C26 121.5(18) . . ?
C28 C27 H27A 119.2 . . ?
C26 C27 H27A 119.2 . . ?
C27 C28 C33 121.3(16) . . ?
C27 C28 C36 117.2(19) . . ?
C33 C28 C36 121.5(18) . . ?
C30 C29 C33 122(2) . . ?
C30 C29 H29A 119.2 . . ?
C33 C29 H29A 119.2 . . ?
C29 C30 C31 123(2) . . ?
C29 C30 H30A 118.7 . . ?
C31 C30 H30A 118.7 . . ?
C32 C31 C30 118(2) . . ?
C32 C31 H31A 121.2 . . ?
C30 C31 H31A 121.2 . . ?
C31 C32 C34 124(2) . . ?
C31 C32 H32A 118.2 . . ?
C34 C32 H32A 118.2 . . ?
C29 C33 C34 117.4(19) . . ?
C29 C33 C28 124.4(18) . . ?
C34 C33 C28 118.2(16) . . ?
C32 C34 C33 116.9(19) . . ?
C32 C34 C25 124.7(19) . . ?
C33 C34 C25 118.3(16) . . ?
O11 C35 O12 118.6(16) . . ?
O11 C35 C25 121.8(16) . . ?
O12 C35 C25 119.5(16) . . ?
O11 C35 U2 60.0(9) . . ?
O12 C35 U2 58.6(9) . . ?
C25 C35 U2 175.2(19) . . ?
O13 C36 O14 119.4(15) . . ?
O13 C36 C28 120.3(16) . . ?
O14 C36 C28 120.2(15) . . ?
O13 C36 U2 60.0(9) . 4_445 ?
O14 C36 U2 59.8(8) . 4_445 ?
C28 C36 U2 171.9(19) . 4_445 ?
C38 C37 C46 119.2(18) . . ?
C38 C37 C47 120(3) . . ?
C46 C37 C47 120(2) . . ?
C37 C38 C39 125(2) . . ?
C37 C38 H38A 117.4 . . ?
C39 C38 H38A 117.4 . . ?
C38 C39 C40 117(2) . . ?
C38 C39 H39A 121.7 . . ?
C40 C39 H39A 121.7 . . ?
C39 C40 C45 123(2) . . ?
C39 C40 C48 117(2) . . ?
C45 C40 C48 121(3) . . ?
C45 C41 C42 122(3) . . ?
C45 C41 H41A 119.1 . . ?
C42 C41 H41A 119.1 . . ?
C43 C42 C41 120(3) . . ?
C43 C42 H42A 120.1 . . ?
C41 C42 H42A 120.1 . . ?
C44 C43 C42 118(3) . . ?
C44 C43 H43A 120.9 . . ?
C42 C43 H43A 120.9 . . ?
C43 C44 C46 124(3) . . ?
C43 C44 H44A 118.0 . . ?
C46 C44 H44A 118.0 . . ?
C41 C45 C46 119(2) . . ?
C41 C45 C40 124(2) . . ?
C46 C45 C40 118(2) . . ?
C44 C46 C45 117(2) . . ?
C44 C46 C37 124(2) . . ?
C45 C46 C37 118.9(19) . . ?
O15 C47 O16 119.6(16) . . ?
O15 C47 C37 120.3(18) . . ?
O16 C47 C37 120.1(17) . . ?
O15 C47 U2 61.0(9) . . ?
O16 C47 U2 58.8(9) . . ?
C37 C47 U2 174(3) . . ?
O18 C48 O17 121(2) . . ?
O18 C48 C40 124(3) . . ?
O17 C48 C40 115(2) . . ?
C50 N1 C51 121(7) . . ?
C50 N1 H1A 119.3 . . ?
C51 N1 H1A 119.3 . . ?
C59 N2 C60 123(3) . . ?
C59 N2 H2B 118.4 . . ?
C60 N2 H2B 118.4 . . ?
C50 C49 C53 118(5) . . ?
C50 C49 H49A 120.8 . . ?
C53 C49 H49A 120.8 . . ?
N1 C50 C49 121(7) . . ?
N1 C50 H50A 119.4 . . ?
C49 C50 H50A 119.4 . . ?
N1 C51 C52 121(5) . . ?
N1 C51 H51A 119.6 . . ?
C52 C51 H51A 119.6 . . ?
C53 C52 C51 115(5) . . ?
C53 C52 H52A 122.3 . . ?
C51 C52 H52A 122.3 . . ?
C52 C53 C49 122(4) . . ?
C52 C53 C54 121(4) . . ?
C49 C53 C54 118(3) . . ?
C55 C54 C53 108(3) . . ?
C55 C54 H54A 110.1 . . ?
C53 C54 H54A 110.1 . . ?
C55 C54 H54B 110.1 . . ?
C53 C54 H54B 110.1 . . ?
H54A C54 H54B 108.4 . . ?
C56 C55 C54 113(3) . . ?
C56 C55 H55A 109.1 . . ?
C54 C55 H55A 109.1 . . ?
C56 C55 H55B 109.1 . . ?
C54 C55 H55B 109.1 . . ?
H55A C55 H55B 107.8 . . ?
C55 C56 C57 118(4) . . ?
C55 C56 H56A 107.8 . . ?
C57 C56 H56A 107.8 . . ?
C55 C56 H56B 107.8 . . ?
C57 C56 H56B 107.8 . . ?
H56A C56 H56B 107.2 . . ?
C61 C57 C58 119(3) . . ?
C61 C57 C56 126(3) . . ?
C58 C57 C56 116(3) . . ?
C57 C58 C59 119(3) . . ?
C57 C58 H58A 120.3 . . ?
C59 C58 H58A 120.3 . . ?
N2 C59 C58 121(3) . . ?
N2 C59 H59A 119.3 . . ?
C58 C59 H59A 119.3 . . ?
N2 C60 C61 117(3) . . ?
N2 C60 H60A 121.4 . . ?
C61 C60 H60A 121.4 . . ?
C57 C61 C60 120(3) . . ?
C57 C61 H61A 120.1 . . ?
C60 C61 H61A 120.1 . . ?
H211 O21 H212 105.6 . . ?
H221 O22 H222 106.4 . . ?

_refine_diff_density_max         1.231
_refine_diff_density_min         -2.191
_refine_diff_density_rms         0.151

####################################################################### 
# 
# 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_shx97_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1575474'
_audit_update_record             
;
2017-09-20 deposited with the CCDC.
2018-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H18 O16 U2, C6 H6 N'
_chemical_formula_sum            'C48 H30 N2 O16 U2'
_chemical_formula_weight         1366.80

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

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

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

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

_cell_length_a                   10.014(2)
_cell_length_b                   15.315(3)
_cell_length_c                   16.677(3)
_cell_angle_alpha                97.86(3)
_cell_angle_beta                 97.56(3)
_cell_angle_gamma                98.90(3)
_cell_volume                     2472.5(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    23965
_cell_measurement_theta_min      3.08
_cell_measurement_theta_max      27.482

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_F_000             1288
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    6.611
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.206
_exptl_absorpt_correction_T_max  0.304
_exptl_absorpt_process_details   ABSCOR(Higashi,1995)
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'rigaku r-axis rapid'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23965
_diffrn_reflns_av_unetI/netI     0.0824
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.992
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             11321
_reflns_number_gt                8796
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.029 0.000 0.500 362 104 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0547P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11127
_refine_ls_number_parameters     676
_refine_ls_number_restraints     394
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0430
_refine_ls_wR_factor_ref         0.1245
_refine_ls_wR_factor_gt          0.1059
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U2 U 0.49311(2) 0.85595(2) 0.10629(2) 0.02771(8) Uani 1 1 d . . . . .
U1 U 0.25118(2) 0.43033(2) -0.51040(2) 0.02500(8) Uani 1 1 d . . . . .
O1 O 0.3009(5) 0.7393(3) 0.1257(3) 0.0493(13) Uani 1 1 d . . . . .
O2 O 0.3829(5) 0.8470(4) 0.2286(3) 0.0514(14) Uani 1 1 d . . . . .
O3 O -0.1507(5) 0.5537(3) 0.3834(3) 0.0412(11) Uani 1 1 d . . . . .
O4 O -0.0474(5) 0.6627(3) 0.4805(3) 0.0430(12) Uani 1 1 d . . . . .
O5 O 0.5874(6) 0.8418(4) -0.0265(3) 0.0604(16) Uani 1 1 d . . . . .
O6 O 0.4396(5) 0.7293(4) -0.0074(3) 0.0625(16) Uani 1 1 d . . . . .
O7 O 0.5887(4) 0.5413(3) -0.4022(2) 0.0369(10) Uani 1 1 d . . . . .
O8 O 0.3757(4) 0.5654(3) -0.4260(2) 0.0352(10) Uani 1 1 d . . . . .
O9 O 0.5738(5) 0.9870(3) 0.2160(3) 0.0459(13) Uani 1 1 d . . . . .
O10 O 0.6757(5) 0.9812(4) 0.1076(3) 0.0579(15) Uani 1 1 d . . . . .
O11 O 1.2522(7) 1.1938(5) 0.4002(5) 0.109(3) Uani 1 1 d . . . . .
O12 O 1.1747(5) 1.3186(3) 0.3786(3) 0.0421(12) Uani 1 1 d . . . . .
O13 O 0.6166(6) 0.8011(4) 0.1503(3) 0.0573(15) Uani 1 1 d . . . . .
O14 O 0.3689(5) 0.9102(4) 0.0632(3) 0.0510(14) Uani 1 1 d . . . . .
O15 O 0.1507(4) 0.4976(3) -0.5582(3) 0.0355(11) Uani 1 1 d . . . . .
O16 O 0.3559(5) 0.3677(3) -0.4603(3) 0.0393(11) Uani 1 1 d . . . . .
C1 C 0.2986(7) 0.7757(5) 0.1982(4) 0.0408(16) Uani 1 1 d . . . . .
C2 C 0.2003(6) 0.7382(5) 0.2477(4) 0.0328(14) Uani 1 1 d . . . . .
C3 C 0.2466(7) 0.7359(5) 0.3289(4) 0.0476(19) Uani 1 1 d . U . . .
H3A H 0.337516 0.759498 0.350521 0.057 Uiso 1 1 calc R U . . .
C4 C 0.1586(7) 0.6984(6) 0.3802(4) 0.053(2) Uani 1 1 d . . . . .
H4A H 0.192003 0.697661 0.434765 0.064 Uiso 1 1 calc R U . . .
C5 C 0.0245(6) 0.6633(5) 0.3493(4) 0.0361(15) Uani 1 1 d . . . . .
C6 C -0.0625(7) 0.6237(5) 0.4070(4) 0.0386(16) Uani 1 1 d . . . . .
C7 C -0.1709(6) 0.6334(5) 0.2337(4) 0.0394(15) Uani 1 1 d . . . . .
H7A H -0.230491 0.608381 0.266005 0.047 Uiso 1 1 calc R U . . .
C8 C -0.2174(7) 0.6408(6) 0.1555(4) 0.0508(19) Uani 1 1 d . . . . .
H8A H -0.309004 0.619366 0.134026 0.061 Uiso 1 1 calc R U . . .
C9 C -0.1307(8) 0.6800(6) 0.1063(4) 0.053(2) Uani 1 1 d . . . . .
H9A H -0.165834 0.686035 0.053230 0.064 Uiso 1 1 calc R U . . .
C10 C 0.0048(7) 0.7095(5) 0.1350(4) 0.0437(17) Uani 1 1 d . . . . .
H10A H 0.061688 0.733689 0.100746 0.052 Uiso 1 1 calc R U . . .
C11 C 0.0595(7) 0.7039(4) 0.2154(4) 0.0358(14) Uani 1 1 d . . . . .
C12 C -0.0294(6) 0.6644(4) 0.2664(3) 0.0302(13) Uani 1 1 d . . . . .
C13 C 0.5166(7) 0.7653(5) -0.0508(4) 0.0454(17) Uani 1 1 d . . . . .
C14 C 0.5246(6) 0.7157(5) -0.1353(4) 0.0409(17) Uani 1 1 d . . . . .
C15 C 0.4989(7) 0.7587(5) -0.2019(4) 0.0430(16) Uani 1 1 d . . . . .
H15A H 0.489672 0.818654 -0.194097 0.052 Uiso 1 1 calc R U . . .
C16 C 0.4870(6) 0.7111(5) -0.2816(4) 0.0396(16) Uani 1 1 d . . . . .
H16A H 0.468292 0.739465 -0.326619 0.048 Uiso 1 1 calc R U . . .
C17 C 0.5028(5) 0.6235(4) -0.2933(3) 0.0261(12) Uani 1 1 d . . . . .
C18 C 0.4887(6) 0.5738(4) -0.3811(3) 0.0298(13) Uani 1 1 d . . . . .
C19 C 0.5448(6) 0.4855(5) -0.2370(4) 0.0414(16) Uani 1 1 d . . . . .
H19A H 0.535334 0.453800 -0.289699 0.050 Uiso 1 1 calc R U . . .
C20 C 0.5704(8) 0.4432(6) -0.1728(5) 0.057(2) Uani 1 1 d . . . . .
H20A H 0.577722 0.382908 -0.181291 0.069 Uiso 1 1 calc R U . . .
C21 C 0.5861(7) 0.4903(6) -0.0923(5) 0.058(2) Uani 1 1 d . . . . .
H21A H 0.606625 0.461732 -0.047644 0.070 Uiso 1 1 calc R U . . .
C22 C 0.5711(7) 0.5779(6) -0.0801(4) 0.052(2) Uani 1 1 d . . . . .
H22A H 0.581031 0.607852 -0.026667 0.063 Uiso 1 1 calc R U . . .
C23 C 0.5410(6) 0.6254(5) -0.1459(3) 0.0366(15) Uani 1 1 d . . . . .
C24 C 0.5317(5) 0.5771(4) -0.2269(3) 0.0291(13) Uani 1 1 d . . . . .
C25 C 0.6725(6) 1.0159(5) 0.1807(4) 0.0385(15) Uani 1 1 d . . . . .
C26 C 0.7928(6) 1.0821(4) 0.2278(4) 0.0338(14) Uani 1 1 d . . . . .
C27 C 0.8226(7) 1.0809(5) 0.3097(4) 0.0461(18) Uani 1 1 d . . . . .
H27A H 0.760533 1.047788 0.335640 0.055 Uiso 1 1 calc R U . . .
C28 C 0.9471(8) 1.1296(5) 0.3555(4) 0.0506(19) Uani 1 1 d . . . . .
H28A H 0.967906 1.126211 0.410928 0.061 Uiso 1 1 calc R U . . .
C29 C 1.0364(6) 1.1811(4) 0.3195(4) 0.0347(14) Uani 1 1 d . . . . .
C30 C 1.1642(7) 1.2343(5) 0.3692(4) 0.0460(18) Uani 1 1 d . . . . .
C31 C 1.0971(7) 1.2394(5) 0.1958(4) 0.0407(16) Uani 1 1 d . . . . .
H31A H 1.180433 1.269867 0.225258 0.049 Uiso 1 1 calc R U . . .
C32 C 1.0639(7) 1.2460(5) 0.1139(4) 0.0477(17) Uani 1 1 d . . . . .
H32A H 1.125356 1.279964 0.088126 0.057 Uiso 1 1 calc R U . . .
C33 C 0.9401(8) 1.2023(5) 0.0709(4) 0.053(2) Uani 1 1 d . . . . .
H33A H 0.917326 1.208716 0.016401 0.063 Uiso 1 1 calc R U . . .
C34 C 0.8510(8) 1.1504(5) 0.1053(4) 0.0471(18) Uani 1 1 d . . . . .
H34A H 0.768112 1.121495 0.074162 0.056 Uiso 1 1 calc R U . . .
C35 C 0.8805(6) 1.1385(4) 0.1885(4) 0.0340(14) Uani 1 1 d . . . . .
C36 C 1.0068(6) 1.1876(4) 0.2343(3) 0.0276(12) Uani 1 1 d . . . . .
C38 C 1.0656(7) 0.4841(5) 0.1593(4) 0.0459(17) Uani 1 1 d . . . . .
H38A H 1.145378 0.517405 0.148674 0.055 Uiso 1 1 calc R U . . .
C39 C 0.9552(7) 0.4548(5) 0.0978(4) 0.0406(16) Uani 1 1 d . . . . .
C40 C 0.8402(7) 0.4033(5) 0.1158(5) 0.0511(19) Uani 1 1 d . . . . .
H40A H 0.764905 0.382021 0.075022 0.061 Uiso 1 1 calc R U . . .
C41 C 0.8365(8) 0.3835(6) 0.1925(5) 0.056(2) Uani 1 1 d . . . . .
H41A H 0.758748 0.348822 0.204138 0.067 Uiso 1 1 calc R U . . .
C42 C 0.9537(7) 0.4718(5) 0.0135(5) 0.0512(19) Uani 1 1 d . . . . .
H42A H 0.880749 0.440112 -0.025145 0.061 Uiso 1 1 calc R U . . .
N1 N 0.9443(7) 0.4137(4) 0.2512(3) 0.0509(16) Uani 1 1 d . . . . .
H1A H 0.940462 0.400342 0.299361 0.061 Uiso 1 1 calc R U . . .
C37 C 1.0572(8) 0.4637(5) 0.2377(4) 0.0471(18) Uani 1 1 d . . . . .
H37A H 1.129987 0.484826 0.280068 0.056 Uiso 1 1 calc R U . . .
N2 N 0.866(2) 1.0194(16) -0.2094(13) 0.108(5) Uani 0.5 1 d D U P A -1
H2A H 0.830031 1.019662 -0.259140 0.130 Uiso 0.5 1 calc R U P A -1
C43 C 0.9946(17) 1.0633(13) -0.1718(13) 0.077(4) Uani 0.5 1 d D U P A -1
H43A H 1.044114 1.095705 -0.204792 0.093 Uiso 0.5 1 calc R U P A -1
C44 C 1.0604(19) 1.0669(15) -0.0946(13) 0.092(4) Uani 0.5 1 d D U P A -1
H44A H 1.144964 1.103973 -0.077468 0.111 Uiso 0.5 1 calc R U P A -1
C45 C 1.002(2) 1.0150(15) -0.0400(12) 0.091(4) Uani 0.5 1 d D U P A -1
C46 C 0.8697(19) 0.9783(16) -0.0770(14) 0.094(4) Uani 0.5 1 d D U P A -1
H46A H 0.816020 0.951120 -0.042782 0.112 Uiso 0.5 1 calc R U P A -1
C47 C 0.8049(19) 0.9747(14) -0.1528(13) 0.086(4) Uani 0.5 1 d D U P A -1
H47A H 0.716918 0.941680 -0.168169 0.103 Uiso 0.5 1 calc R U P A -1
C48 C 1.083(2) 1.0180(17) 0.0399(12) 0.086(4) Uani 0.5 1 d D U P A -1
H48A H 1.172361 1.049332 0.052497 0.103 Uiso 0.5 1 calc R U P A -1
C49 C 1.027(2) 0.9751(16) 0.0941(13) 0.093(4) Uani 0.5 1 d D U P A -1
H49A H 0.938392 0.942432 0.080012 0.111 Uiso 0.5 1 calc R U P A -1
C50 C 1.104(2) 0.9787(19) 0.1779(15) 0.093(4) Uani 0.5 1 d D U P A -1
C51 C 1.2357(18) 1.0270(14) 0.2075(14) 0.086(4) Uani 0.5 1 d D U P A -1
H51A H 1.285823 1.061280 0.176043 0.104 Uiso 0.5 1 calc R U P A -1
C52 C 1.286(2) 1.0198(14) 0.2878(13) 0.096(4) Uani 0.5 1 d D U P A -1
H52A H 1.378326 1.042498 0.304885 0.115 Uiso 0.5 1 calc R U P A -1
N3 N 1.2181(17) 0.9842(12) 0.3450(11) 0.095(4) Uani 0.5 1 d D U P A -1
H3B H 1.247854 0.991225 0.396619 0.113 Uiso 0.5 1 calc R U P A -1
C53 C 1.0949(19) 0.9355(14) 0.3061(14) 0.105(5) Uani 0.5 1 d D U P A -1
H53A H 1.045624 0.896765 0.334346 0.126 Uiso 0.5 1 calc R U P A -1
C54 C 1.041(2) 0.9410(15) 0.2283(14) 0.089(4) Uani 0.5 1 d D U P A -1
H54A H 0.950050 0.914678 0.210449 0.107 Uiso 0.5 1 calc R U P 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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U2 O14 1.733(5) . ?
U2 O13 1.739(5) . ?
U2 O10 2.432(5) . ?
U2 O2 2.453(5) . ?
U2 O6 2.459(5) . ?
U2 O9 2.476(4) . ?
U2 O1 2.502(5) . ?
U2 O5 2.515(5) . ?
U2 C25 2.827(6) . ?
U2 C13 2.849(6) . ?
U2 C1 2.866(7) . ?
U1 O16 1.737(5) . ?
U1 O15 1.745(5) . ?
U1 O12 2.301(4) 1_444 ?
U1 O7 2.337(4) 2_664 ?
U1 O8 2.399(4) . ?
U1 O4 2.451(5) 2_565 ?
U1 O3 2.461(5) 2_565 ?
U1 C6 2.827(7) 2_565 ?
O1 C1 1.265(8) . ?
O2 C1 1.270(8) . ?
O3 C6 1.258(8) . ?
O4 C6 1.267(8) . ?
O5 C13 1.255(8) . ?
O6 C13 1.245(8) . ?
O7 C18 1.254(7) . ?
O8 C18 1.251(6) . ?
O9 C25 1.269(7) . ?
O10 C25 1.267(7) . ?
O11 C30 1.250(9) . ?
O12 C30 1.267(9) . ?
C1 C2 1.466(9) . ?
C2 C3 1.379(9) . ?
C2 C11 1.431(9) . ?
C3 C4 1.419(10) . ?
C3 H3A 0.9300 . ?
C4 C5 1.370(9) . ?
C4 H4A 0.9300 . ?
C5 C12 1.420(8) . ?
C5 C6 1.506(9) . ?
C7 C8 1.352(9) . ?
C7 C12 1.431(8) . ?
C7 H7A 0.9300 . ?
C8 C9 1.396(10) . ?
C8 H8A 0.9300 . ?
C9 C10 1.362(10) . ?
C9 H9A 0.9300 . ?
C10 C11 1.400(9) . ?
C10 H10A 0.9300 . ?
C11 C12 1.433(8) . ?
C13 C14 1.524(8) . ?
C14 C15 1.382(9) . ?
C14 C23 1.409(10) . ?
C15 C16 1.407(9) . ?
C15 H15A 0.9300 . ?
C16 C17 1.366(9) . ?
C16 H16A 0.9300 . ?
C17 C24 1.418(8) . ?
C17 C18 1.533(7) . ?
C19 C20 1.342(10) . ?
C19 C24 1.418(9) . ?
C19 H19A 0.9300 . ?
C20 C21 1.412(11) . ?
C20 H20A 0.9300 . ?
C21 C22 1.364(11) . ?
C21 H21A 0.9300 . ?
C22 C23 1.422(9) . ?
C22 H22A 0.9300 . ?
C23 C24 1.432(8) . ?
C25 C26 1.500(8) . ?
C26 C27 1.362(8) . ?
C26 C35 1.421(9) . ?
C27 C28 1.415(9) . ?
C27 H27A 0.9300 . ?
C28 C29 1.355(9) . ?
C28 H28A 0.9300 . ?
C29 C36 1.433(8) . ?
C29 C30 1.484(8) . ?
C31 C32 1.384(9) . ?
C31 C36 1.389(9) . ?
C31 H31A 0.9300 . ?
C32 C33 1.370(10) . ?
C32 H32A 0.9300 . ?
C33 C34 1.341(10) . ?
C33 H33A 0.9300 . ?
C34 C35 1.421(8) . ?
C34 H34A 0.9300 . ?
C35 C36 1.429(8) . ?
C38 C39 1.379(9) . ?
C38 C37 1.395(9) . ?
C38 H38A 0.9300 . ?
C39 C40 1.383(10) . ?
C39 C42 1.463(10) . ?
C40 C41 1.359(10) . ?
C40 H40A 0.9300 . ?
C41 N1 1.335(9) . ?
C41 H41A 0.9300 . ?
C42 C42 1.333(15) 2_765 ?
C42 H42A 0.9300 . ?
N1 C37 1.327(9) . ?
N1 H1A 0.8600 . ?
C37 H37A 0.9300 . ?
N2 C43 1.381(17) . ?
N2 C47 1.390(17) . ?
N2 H2A 0.8600 . ?
C43 C44 1.357(16) . ?
C43 H43A 0.9300 . ?
C44 C45 1.415(17) . ?
C44 H44A 0.9300 . ?
C45 C46 1.383(17) . ?
C45 C48 1.457(16) . ?
C46 C47 1.332(17) . ?
C46 H46A 0.9300 . ?
C47 H47A 0.9300 . ?
C48 C49 1.321(17) . ?
C48 H48A 0.9300 . ?
C49 C50 1.497(17) . ?
C49 H49A 0.9300 . ?
C50 C54 1.27(3) . ?
C50 C51 1.396(17) . ?
C51 C52 1.392(17) . ?
C51 H51A 0.9300 . ?
C52 N3 1.365(16) . ?
C52 H52A 0.9300 . ?
N3 C53 1.368(16) . ?
N3 H3B 0.8600 . ?
C53 C54 1.356(17) . ?
C53 H53A 0.9300 . ?
C54 H54A 0.9300 . ?

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
O14 U2 O13 179.4(2) . . ?
O14 U2 O10 92.7(2) . . ?
O13 U2 O10 87.7(2) . . ?
O14 U2 O2 91.5(2) . . ?
O13 U2 O2 87.9(2) . . ?
O10 U2 O2 118.97(16) . . ?
O14 U2 O6 93.0(2) . . ?
O13 U2 O6 87.2(2) . . ?
O10 U2 O6 120.92(16) . . ?
O2 U2 O6 119.58(17) . . ?
O14 U2 O9 90.1(2) . . ?
O13 U2 O9 89.9(2) . . ?
O10 U2 O9 52.91(15) . . ?
O2 U2 O9 66.24(16) . . ?
O6 U2 O9 173.31(15) . . ?
O14 U2 O1 86.9(2) . . ?
O13 U2 O1 92.7(2) . . ?
O10 U2 O1 171.24(15) . . ?
O2 U2 O1 52.32(15) . . ?
O6 U2 O1 67.83(16) . . ?
O9 U2 O1 118.33(15) . . ?
O14 U2 O5 89.6(2) . . ?
O13 U2 O5 91.0(2) . . ?
O10 U2 O5 69.39(16) . . ?
O2 U2 O5 171.49(17) . . ?
O6 U2 O5 51.92(17) . . ?
O9 U2 O5 122.21(16) . . ?
O1 U2 O5 119.34(15) . . ?
O14 U2 C25 94.4(2) . . ?
O13 U2 C25 85.8(3) . . ?
O10 U2 C25 26.55(16) . . ?
O2 U2 C25 92.43(17) . . ?
O6 U2 C25 146.91(17) . . ?
O9 U2 C25 26.65(15) . . ?
O1 U2 C25 144.75(16) . . ?
O5 U2 C25 95.90(17) . . ?
O14 U2 C13 91.2(2) . . ?
O13 U2 C13 89.2(2) . . ?
O10 U2 C13 95.35(18) . . ?
O2 U2 C13 145.39(19) . . ?
O6 U2 C13 25.80(18) . . ?
O9 U2 C13 148.25(18) . . ?
O1 U2 C13 93.41(18) . . ?
O5 U2 C13 26.12(18) . . ?
C25 U2 C13 121.73(19) . . ?
O14 U2 C1 89.0(2) . . ?
O13 U2 C1 90.4(2) . . ?
O10 U2 C1 145.14(18) . . ?
O2 U2 C1 26.17(17) . . ?
O6 U2 C1 93.71(19) . . ?
O9 U2 C1 92.30(18) . . ?
O1 U2 C1 26.15(17) . . ?
O5 U2 C1 145.47(18) . . ?
C25 U2 C1 118.60(19) . . ?
C13 U2 C1 119.4(2) . . ?
O16 U1 O15 177.42(19) . . ?
O16 U1 O12 93.6(2) . 1_444 ?
O15 U1 O12 88.7(2) . 1_444 ?
O16 U1 O7 90.1(2) . 2_664 ?
O15 U1 O7 89.49(18) . 2_664 ?
O12 U1 O7 76.92(16) 1_444 2_664 ?
O16 U1 O8 90.47(18) . . ?
O15 U1 O8 86.96(19) . . ?
O12 U1 O8 161.13(16) 1_444 . ?
O7 U1 O8 84.68(15) 2_664 . ?
O16 U1 O4 90.6(2) . 2_565 ?
O15 U1 O4 91.08(19) . 2_565 ?
O12 U1 O4 72.71(16) 1_444 2_565 ?
O7 U1 O4 149.60(15) 2_664 2_565 ?
O8 U1 O4 125.70(15) . 2_565 ?
O16 U1 O3 85.2(2) . 2_565 ?
O15 U1 O3 94.29(18) . 2_565 ?
O12 U1 O3 125.42(16) 1_444 2_565 ?
O7 U1 O3 157.36(15) 2_664 2_565 ?
O8 U1 O3 73.26(15) . 2_565 ?
O4 U1 O3 52.77(15) 2_565 2_565 ?
O16 U1 C6 85.4(2) . 2_565 ?
O15 U1 C6 95.3(2) . 2_565 ?
O12 U1 C6 99.04(18) 1_444 2_565 ?
O7 U1 C6 173.70(18) 2_664 2_565 ?
O8 U1 C6 99.65(17) . 2_565 ?
O4 U1 C6 26.56(16) 2_565 2_565 ?
O3 U1 C6 26.39(17) 2_565 2_565 ?
C1 O1 U2 93.2(4) . . ?
C1 O2 U2 95.4(4) . . ?
C6 O3 U1 93.2(4) . 2_565 ?
C6 O4 U1 93.5(4) . 2_565 ?
C13 O5 U2 92.0(4) . . ?
C13 O6 U2 94.9(4) . . ?
C18 O7 U1 137.1(4) . 2_664 ?
C18 O8 U1 126.2(4) . . ?
C25 O9 U2 92.3(3) . . ?
C25 O10 U2 94.4(4) . . ?
C30 O12 U1 133.2(4) . 1_666 ?
O1 C1 O2 119.1(7) . . ?
O1 C1 C2 121.7(6) . . ?
O2 C1 C2 119.2(6) . . ?
O1 C1 U2 60.7(4) . . ?
O2 C1 U2 58.5(4) . . ?
C2 C1 U2 177.6(5) . . ?
C3 C2 C11 118.9(6) . . ?
C3 C2 C1 118.1(6) . . ?
C11 C2 C1 122.9(6) . . ?
C2 C3 C4 121.4(7) . . ?
C2 C3 H3A 119.3 . . ?
C4 C3 H3A 119.3 . . ?
C5 C4 C3 120.1(7) . . ?
C5 C4 H4A 120.0 . . ?
C3 C4 H4A 120.0 . . ?
C4 C5 C12 121.1(6) . . ?
C4 C5 C6 117.1(6) . . ?
C12 C5 C6 121.8(6) . . ?
O3 C6 O4 119.6(6) . . ?
O3 C6 C5 121.4(6) . . ?
O4 C6 C5 119.0(6) . . ?
O3 C6 U1 60.4(4) . 2_565 ?
O4 C6 U1 59.9(4) . 2_565 ?
C5 C6 U1 171.0(5) . 2_565 ?
C8 C7 C12 119.7(6) . . ?
C8 C7 H7A 120.2 . . ?
C12 C7 H7A 120.2 . . ?
C7 C8 C9 121.3(7) . . ?
C7 C8 H8A 119.4 . . ?
C9 C8 H8A 119.4 . . ?
C10 C9 C8 120.8(6) . . ?
C10 C9 H9A 119.6 . . ?
C8 C9 H9A 119.6 . . ?
C9 C10 C11 120.8(6) . . ?
C9 C10 H10A 119.6 . . ?
C11 C10 H10A 119.6 . . ?
C10 C11 C12 118.6(6) . . ?
C10 C11 C2 121.4(6) . . ?
C12 C11 C2 119.9(6) . . ?
C5 C12 C11 118.5(6) . . ?
C5 C12 C7 122.5(6) . . ?
C11 C12 C7 118.9(5) . . ?
O6 C13 O5 121.2(6) . . ?
O6 C13 C14 119.3(6) . . ?
O5 C13 C14 119.5(6) . . ?
O6 C13 U2 59.3(3) . . ?
O5 C13 U2 61.9(4) . . ?
C14 C13 U2 178.2(5) . . ?
C15 C14 C23 121.0(6) . . ?
C15 C14 C13 117.8(7) . . ?
C23 C14 C13 120.8(6) . . ?
C14 C15 C16 119.5(7) . . ?
C14 C15 H15A 120.3 . . ?
C16 C15 H15A 120.3 . . ?
C17 C16 C15 120.4(6) . . ?
C17 C16 H16A 119.8 . . ?
C15 C16 H16A 119.8 . . ?
C16 C17 C24 122.1(5) . . ?
C16 C17 C18 118.9(5) . . ?
C24 C17 C18 119.0(5) . . ?
O8 C18 O7 124.3(5) . . ?
O8 C18 C17 117.4(5) . . ?
O7 C18 C17 118.2(5) . . ?
C20 C19 C24 122.0(7) . . ?
C20 C19 H19A 119.0 . . ?
C24 C19 H19A 119.0 . . ?
C19 C20 C21 119.8(8) . . ?
C19 C20 H20A 120.1 . . ?
C21 C20 H20A 120.1 . . ?
C22 C21 C20 119.9(7) . . ?
C22 C21 H21A 120.1 . . ?
C20 C21 H21A 120.1 . . ?
C21 C22 C23 122.6(7) . . ?
C21 C22 H22A 118.7 . . ?
C23 C22 H22A 118.7 . . ?
C14 C23 C22 123.9(6) . . ?
C14 C23 C24 119.7(6) . . ?
C22 C23 C24 116.4(7) . . ?
C17 C24 C19 123.5(5) . . ?
C17 C24 C23 117.2(6) . . ?
C19 C24 C23 119.3(6) . . ?
O9 C25 O10 119.1(6) . . ?
O9 C25 C26 120.5(5) . . ?
O10 C25 C26 119.9(6) . . ?
O9 C25 U2 61.1(3) . . ?
O10 C25 U2 59.1(3) . . ?
C26 C25 U2 163.5(5) . . ?
C27 C26 C35 120.4(5) . . ?
C27 C26 C25 117.3(6) . . ?
C35 C26 C25 122.0(5) . . ?
C26 C27 C28 120.6(6) . . ?
C26 C27 H27A 119.7 . . ?
C28 C27 H27A 119.7 . . ?
C29 C28 C27 120.6(6) . . ?
C29 C28 H28A 119.7 . . ?
C27 C28 H28A 119.7 . . ?
C28 C29 C36 120.8(5) . . ?
C28 C29 C30 119.8(6) . . ?
C36 C29 C30 119.3(6) . . ?
O11 C30 O12 124.5(6) . . ?
O11 C30 C29 118.8(7) . . ?
O12 C30 C29 116.7(6) . . ?
C32 C31 C36 120.5(6) . . ?
C32 C31 H31A 119.8 . . ?
C36 C31 H31A 119.8 . . ?
C33 C32 C31 119.7(7) . . ?
C33 C32 H32A 120.2 . . ?
C31 C32 H32A 120.2 . . ?
C34 C33 C32 121.7(6) . . ?
C34 C33 H33A 119.1 . . ?
C32 C33 H33A 119.1 . . ?
C33 C34 C35 121.4(6) . . ?
C33 C34 H34A 119.3 . . ?
C35 C34 H34A 119.3 . . ?
C34 C35 C26 124.2(5) . . ?
C34 C35 C36 116.7(6) . . ?
C26 C35 C36 119.1(5) . . ?
C31 C36 C35 119.9(5) . . ?
C31 C36 C29 121.9(5) . . ?
C35 C36 C29 118.2(6) . . ?
C39 C38 C37 119.6(7) . . ?
C39 C38 H38A 120.2 . . ?
C37 C38 H38A 120.2 . . ?
C38 C39 C40 118.2(7) . . ?
C38 C39 C42 124.1(7) . . ?
C40 C39 C42 117.7(6) . . ?
C41 C40 C39 120.5(7) . . ?
C41 C40 H40A 119.8 . . ?
C39 C40 H40A 119.8 . . ?
N1 C41 C40 120.0(7) . . ?
N1 C41 H41A 120.0 . . ?
C40 C41 H41A 120.0 . . ?
C42 C42 C39 126.5(9) 2_765 . ?
C42 C42 H42A 116.7 2_765 . ?
C39 C42 H42A 116.7 . . ?
C37 N1 C41 122.2(6) . . ?
C37 N1 H1A 118.9 . . ?
C41 N1 H1A 118.9 . . ?
N1 C37 C38 119.4(6) . . ?
N1 C37 H37A 120.3 . . ?
C38 C37 H37A 120.3 . . ?
C43 N2 C47 108.0(17) . . ?
C43 N2 H2A 126.0 . . ?
C47 N2 H2A 126.0 . . ?
C44 C43 N2 130.5(17) . . ?
C44 C43 H43A 114.7 . . ?
N2 C43 H43A 114.7 . . ?
C43 C44 C45 120.8(16) . . ?
C43 C44 H44A 119.6 . . ?
C45 C44 H44A 119.6 . . ?
C46 C45 C44 106.6(16) . . ?
C46 C45 C48 136(2) . . ?
C44 C45 C48 117.5(19) . . ?
C47 C46 C45 131.9(19) . . ?
C47 C46 H46A 114.1 . . ?
C45 C46 H46A 114.1 . . ?
C46 C47 N2 121.4(17) . . ?
C46 C47 H47A 119.3 . . ?
N2 C47 H47A 119.3 . . ?
C49 C48 C45 118(2) . . ?
C49 C48 H48A 120.8 . . ?
C45 C48 H48A 120.8 . . ?
C48 C49 C50 120(2) . . ?
C48 C49 H49A 119.8 . . ?
C50 C49 H49A 119.8 . . ?
C54 C50 C51 117(2) . . ?
C54 C50 C49 117(2) . . ?
C51 C50 C49 126(2) . . ?
C52 C51 C50 114.7(19) . . ?
C52 C51 H51A 122.7 . . ?
C50 C51 H51A 122.7 . . ?
N3 C52 C51 129.1(17) . . ?
N3 C52 H52A 115.4 . . ?
C51 C52 H52A 115.4 . . ?
C52 N3 C53 108.3(16) . . ?
C52 N3 H3B 125.8 . . ?
C53 N3 H3B 125.8 . . ?
C54 C53 N3 123.2(18) . . ?
C54 C53 H53A 118.4 . . ?
N3 C53 H53A 118.4 . . ?
C50 C54 C53 125.6(19) . . ?
C50 C54 H54A 117.2 . . ?
C53 C54 H54A 117.2 . . ?

_refine_diff_density_max         2.883
_refine_diff_density_min         -3.110
_refine_diff_density_rms         0.201

####################################################################### 
# 
# 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_shx97_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1575477'
_audit_update_record             
;
2017-09-20 deposited with the CCDC.
2018-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H18 O16 U2, C13 H16 N2'
_chemical_formula_sum            'C49 H34 N2 O16 U2'
_chemical_formula_weight         1382.84

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   17.017(3)
_cell_length_b                   22.500(5)
_cell_length_c                   13.661(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.29(3)
_cell_angle_gamma                90
_cell_volume                     5222.1(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    67177
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      23.348

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_F_000             2616
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    6.262
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.269
_exptl_absorpt_correction_T_max  0.472
_exptl_absorpt_process_details   ABSCOR(Higashi,1995)
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'rigaku r-axis rapid'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            67177
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.005
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             9540
_reflns_number_gt                7808
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.003 0.381 -0.002 66 16 ' '
2 0.003 0.619 0.002 66 16 ' '
3 0.500 0.500 0.000 328 77 ' '
4 0.500 0.000 0.500 328 77 ' '
5 1.003 0.881 0.502 66 16 ' '
6 0.997 0.119 0.498 66 16 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0553P)²+4.8735P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9540
_refine_ls_number_parameters     622
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_ref         0.1013
_refine_ls_wR_factor_gt          0.0934
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U -0.49738(2) 0.10948(2) -0.04896(2) 0.03137(9) Uani 1 1 d . . . . .
O1 O -0.4027(3) 0.04153(19) 0.0136(4) 0.0460(13) Uani 1 1 d . . . . .
O2 O -0.4419(2) -0.02583(18) 0.1194(4) 0.0409(12) Uani 1 1 d . . . . .
C1 C -0.3054(4) 0.0004(2) 0.1217(6) 0.0356(17) Uani 1 1 d . . . . .
C2 C -0.2488(4) 0.0022(3) 0.0534(6) 0.0476(19) Uani 1 1 d . . . . .
H2A H -0.264187 0.006241 -0.012675 0.057 Uiso 1 1 calc R U . . .
C3 C -0.1669(4) -0.0021(3) 0.0823(6) 0.0474(19) Uani 1 1 d . . . . .
H3A H -0.129422 -0.001164 0.035316 0.057 Uiso 1 1 calc R U . . .
C4 C -0.1444(4) -0.0075(2) 0.1777(6) 0.0399(18) Uani 1 1 d . . . . .
C5 C -0.1787(6) -0.0150(4) 0.3535(8) 0.078(3) Uani 1 1 d . . . . .
H5A H -0.125570 -0.018055 0.373049 0.093 Uiso 1 1 calc R U . . .
C6 C -0.2323(7) -0.0156(6) 0.4220(9) 0.106(4) Uani 1 1 d . . . . .
H6A H -0.216328 -0.018604 0.488065 0.127 Uiso 1 1 calc R U . . .
C7 C -0.3127(7) -0.0118(6) 0.3929(8) 0.111(5) Uani 1 1 d . . . . .
H7A H -0.349797 -0.012532 0.440249 0.133 Uiso 1 1 calc R U . . .
C8 C -0.3369(5) -0.0070(4) 0.2982(7) 0.070(3) Uani 1 1 d . . . . .
H8A H -0.390490 -0.003732 0.281570 0.084 Uiso 1 1 calc R U . . .
C9 C -0.2835(4) -0.0067(3) 0.2230(6) 0.0423(18) Uani 1 1 d . . . . .
C10 C -0.2009(4) -0.0099(3) 0.2518(6) 0.0453(19) Uani 1 1 d . . . . .
C11 C -0.3886(4) 0.0056(2) 0.0827(5) 0.0352(16) Uani 1 1 d . . . . .
C12 C -0.0586(4) -0.0083(3) 0.2088(6) 0.048(2) Uani 1 1 d . . . . .
O3 O -0.0227(3) 0.0392(2) 0.2235(5) 0.071(2) Uani 1 1 d . . . . .
O4 O -0.0220(3) -0.0566(2) 0.2180(5) 0.0666(19) Uani 1 1 d . . . . .
O5 O -0.4383(3) 0.1178(2) -0.1496(4) 0.0503(13) Uani 1 1 d . . . . .
O6 O -0.5575(3) 0.1001(2) 0.0479(4) 0.0472(13) Uani 1 1 d . . . . .
O7 O -0.5438(3) 0.21297(19) -0.0634(4) 0.0545(15) Uani 1 1 d . . . . .
O8 O -0.6094(3) 0.1486(2) -0.1531(4) 0.0518(14) Uani 1 1 d . . . . .
C13 C -0.7669(4) 0.3446(3) -0.1711(5) 0.0355(16) Uani 1 1 d . . . . .
C14 C -0.6884(4) 0.3530(3) -0.1436(6) 0.048(2) Uani 1 1 d . . . . .
H14A H -0.669751 0.391513 -0.133283 0.058 Uiso 1 1 calc R U . . .
C15 C -0.6364(4) 0.3058(3) -0.1310(6) 0.050(2) Uani 1 1 d . . . . .
H15A H -0.583373 0.313043 -0.115208 0.060 Uiso 1 1 calc R U . . .
C16 C -0.6633(4) 0.2476(3) -0.1418(5) 0.0375(16) Uani 1 1 d . . . . .
C17 C -0.7736(4) 0.1780(3) -0.1860(6) 0.0415(18) Uani 1 1 d . . . . .
H17A H -0.739882 0.145642 -0.178352 0.050 Uiso 1 1 calc R U . . .
C18 C -0.8507(4) 0.1685(3) -0.2109(6) 0.050(2) Uani 1 1 d . . . . .
H18A H -0.869012 0.129940 -0.221460 0.059 Uiso 1 1 calc R U . . .
C19 C -0.9036(4) 0.2168(3) -0.2210(6) 0.0463(19) Uani 1 1 d . . . . .
H19A H -0.956612 0.209793 -0.237268 0.056 Uiso 1 1 calc R U . . .
C20 C -0.8776(4) 0.2733(3) -0.2071(5) 0.0384(16) Uani 1 1 d . . . . .
H20A H -0.913208 0.304613 -0.213425 0.046 Uiso 1 1 calc R U . . .
C21 C -0.7972(4) 0.2856(3) -0.1830(5) 0.0360(15) Uani 1 1 d . . . . .
C22 C -0.7431(4) 0.2361(2) -0.1714(5) 0.0332(15) Uani 1 1 d . . . . .
C23 C -0.8160(4) 0.3998(3) -0.1865(6) 0.0409(18) Uani 1 1 d . . . . .
C24 C -0.6031(4) 0.2000(3) -0.1191(6) 0.0406(17) Uani 1 1 d . . . . .
O9 O -0.8880(3) 0.39931(19) -0.2136(5) 0.0603(18) Uani 1 1 d . . . . .
O10 O -0.7816(3) 0.44924(18) -0.1732(4) 0.0515(15) Uani 1 1 d . . . . .
O11 O -0.8851(3) 0.61800(19) -0.2215(5) 0.0597(18) Uani 1 1 d . . . . .
O12 O -0.7796(3) 0.56730(19) -0.1802(5) 0.0606(17) Uani 1 1 d . . . . .
C25 C -0.7629(4) 0.6720(3) -0.1828(6) 0.0390(17) Uani 1 1 d . . . . .
C26 C -0.6852(4) 0.6632(3) -0.1538(7) 0.052(2) Uani 1 1 d . . . . .
H26A H -0.667183 0.624576 -0.142813 0.063 Uiso 1 1 calc R U . . .
C27 C -0.6328(4) 0.7102(3) -0.1405(6) 0.054(2) Uani 1 1 d . . . . .
H27A H -0.580199 0.702793 -0.122194 0.065 Uiso 1 1 calc R U . . .
C28 C -0.6587(4) 0.7682(3) -0.1545(5) 0.0423(17) Uani 1 1 d . . . . .
C29 C -0.7646(5) 0.8381(3) -0.2034(6) 0.054(2) Uani 1 1 d . . . . .
H29A H -0.729020 0.869385 -0.196127 0.065 Uiso 1 1 calc R U . . .
C30 C -0.8414(5) 0.8499(3) -0.2305(7) 0.058(2) Uani 1 1 d . . . . .
H30A H -0.858020 0.888880 -0.240655 0.070 Uiso 1 1 calc R U . . .
C31 C -0.8955(4) 0.8025(3) -0.2431(6) 0.054(2) Uani 1 1 d . . . . .
H31A H -0.947743 0.810359 -0.262346 0.065 Uiso 1 1 calc R U . . .
C32 C -0.8715(4) 0.7449(3) -0.2273(6) 0.0418(18) Uani 1 1 d . . . . .
H32A H -0.908027 0.714324 -0.235235 0.050 Uiso 1 1 calc R U . . .
C33 C -0.7918(4) 0.7310(3) -0.1988(5) 0.0339(15) Uani 1 1 d . . . . .
C34 C -0.7380(4) 0.7793(3) -0.1860(5) 0.0388(16) Uani 1 1 d . . . . .
C35 C -0.8124(4) 0.6174(3) -0.1951(6) 0.0449(19) Uani 1 1 d . . . . .
C36 C -0.6019(5) 0.8182(3) -0.1342(7) 0.053(2) Uani 1 1 d . . . . .
O13 O -0.5887(3) 0.83066(19) -0.0457(4) 0.0458(13) Uani 1 1 d . . . . .
O14 O -0.5708(5) 0.8427(4) -0.2018(6) 0.126(4) Uani 1 1 d . . . . .
O15 O -0.9262(3) 0.5107(2) -0.1045(4) 0.0522(13) Uani 1 1 d . . . . .
O16 O -0.8684(3) 0.5069(2) -0.3448(4) 0.0532(14) Uani 1 1 d . . . . .
U2 U -0.89694(2) 0.50893(2) -0.22483(2) 0.03296(9) Uani 1 1 d . . . . .
N1 N -0.3095(5) 0.7418(5) -0.0982(7) 0.092(3) Uani 1 1 d . . . . .
H1A H -0.352132 0.721865 -0.109649 0.110 Uiso 1 1 calc R U . . .
N2 N 0.2656(4) 0.7630(5) 0.0705(6) 0.083(3) Uani 1 1 d . . . . .
H2B H 0.310592 0.746529 0.083191 0.100 Uiso 1 1 calc R U . . .
C37 C -0.3120(6) 0.8024(7) -0.1008(8) 0.097(4) Uani 1 1 d . . . . .
H37A H -0.359813 0.821234 -0.116189 0.117 Uiso 1 1 calc R U . . .
C38 C -0.2463(6) 0.8363(6) -0.0813(8) 0.090(3) Uani 1 1 d . . . . .
H38A H -0.248838 0.877598 -0.081463 0.108 Uiso 1 1 calc R U . . .
C39 C -0.1727(5) 0.8056(5) -0.0605(7) 0.071(3) Uani 1 1 d . . . . .
C40 C -0.1728(5) 0.7446(5) -0.0591(7) 0.076(3) Uani 1 1 d . . . . .
H40A H -0.125917 0.724263 -0.045081 0.091 Uiso 1 1 calc R U . . .
C41 C -0.2414(6) 0.7129(5) -0.0780(8) 0.084(3) Uani 1 1 d . . . . .
H41A H -0.240543 0.671541 -0.076848 0.101 Uiso 1 1 calc R U . . .
C42 C -0.0997(5) 0.8420(4) -0.0415(7) 0.074(3) Uani 1 1 d . . . . .
H42A H -0.107178 0.867666 0.014225 0.089 Uiso 1 1 calc R U . . .
H42B H -0.093144 0.867334 -0.097935 0.089 Uiso 1 1 calc R U . . .
C43 C -0.0251(5) 0.8071(4) -0.0216(7) 0.070(3) Uani 1 1 d . . . . .
H43A H -0.014794 0.783920 -0.079342 0.084 Uiso 1 1 calc R U . . .
H43B H -0.032562 0.779573 0.031711 0.084 Uiso 1 1 calc R U . . .
C44 C 0.0471(5) 0.8466(4) 0.0054(8) 0.075(3) Uani 1 1 d . . . . .
H44A H 0.054002 0.873912 -0.048371 0.090 Uiso 1 1 calc R U . . .
H44B H 0.035729 0.870163 0.062294 0.090 Uiso 1 1 calc R U . . .
C45 C 0.1221(5) 0.8154(4) 0.0268(6) 0.059(2) Uani 1 1 d . . . . .
C46 C 0.1885(6) 0.8497(5) 0.0529(8) 0.080(3) Uani 1 1 d . . . . .
H46A H 0.183908 0.890864 0.054008 0.096 Uiso 1 1 calc R U . . .
C47 C 0.2593(7) 0.8247(6) 0.0765(8) 0.093(4) Uani 1 1 d . . . . .
H47A H 0.302552 0.847904 0.096222 0.111 Uiso 1 1 calc R U . . .
C48 C 0.2029(6) 0.7288(5) 0.0455(7) 0.079(3) Uani 1 1 d . . . . .
H48A H 0.207906 0.687714 0.043490 0.095 Uiso 1 1 calc R U . . .
C49 C 0.1316(5) 0.7551(4) 0.0229(7) 0.064(2) Uani 1 1 d . . . . .
H49A H 0.088591 0.731294 0.004348 0.077 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O6 1.731(5) . ?
U1 O5 1.759(5) . ?
U1 O13 2.326(4) 3_465 ?
U1 O2 2.329(4) 3_455 ?
U1 O1 2.346(4) . ?
U1 O7 2.463(4) . ?
U1 O8 2.474(4) . ?
U1 C24 2.846(6) . ?
O1 C11 1.255(8) . ?
O2 C11 1.275(8) . ?
C1 C2 1.379(11) . ?
C1 C9 1.422(10) . ?
C1 C11 1.488(8) . ?
C2 C3 1.430(9) . ?
C2 H2A 0.9300 . ?
C3 C4 1.343(10) . ?
C3 H3A 0.9300 . ?
C4 C10 1.437(11) . ?
C4 C12 1.496(9) . ?
C5 C6 1.344(15) . ?
C5 C10 1.422(12) . ?
C5 H5A 0.9300 . ?
C6 C7 1.406(15) . ?
C6 H6A 0.9300 . ?
C7 C8 1.338(13) . ?
C7 H7A 0.9300 . ?
C8 C9 1.410(12) . ?
C8 H8A 0.9300 . ?
C9 C10 1.440(9) . ?
C12 O3 1.241(8) . ?
C12 O4 1.255(8) . ?
C12 U2 2.847(7) 4_666 ?
O3 U2 2.465(4) 4_666 ?
O4 U2 2.469(4) 4_666 ?
O7 C24 1.262(8) . ?
O8 C24 1.248(8) . ?
C13 C14 1.379(8) . ?
C13 C21 1.431(8) . ?
C13 C23 1.505(8) . ?
C14 C15 1.387(9) . ?
C14 H14A 0.9300 . ?
C15 C16 1.393(9) . ?
C15 H15A 0.9300 . ?
C16 C22 1.417(8) . ?
C16 C24 1.503(8) . ?
C17 C18 1.354(9) . ?
C17 C22 1.417(8) . ?
C17 H17A 0.9300 . ?
C18 C19 1.412(9) . ?
C18 H18A 0.9300 . ?
C19 C20 1.357(9) . ?
C19 H19A 0.9300 . ?
C20 C21 1.416(8) . ?
C20 H20A 0.9300 . ?
C21 C22 1.447(8) . ?
C23 O9 1.260(8) . ?
C23 O10 1.265(7) . ?
C23 U2 2.849(6) . ?
O9 U2 2.475(4) . ?
O10 U2 2.448(4) . ?
O11 C35 1.268(8) . ?
O11 U2 2.463(4) . ?
O12 C35 1.268(7) . ?
O12 U2 2.437(4) . ?
C25 C26 1.373(9) . ?
C25 C33 1.427(8) . ?
C25 C35 1.495(8) . ?
C26 C27 1.390(9) . ?
C26 H26A 0.9300 . ?
C27 C28 1.387(10) . ?
C27 H27A 0.9300 . ?
C28 C34 1.416(9) . ?
C28 C36 1.498(9) . ?
C29 C30 1.363(11) . ?
C29 C34 1.415(9) . ?
C29 H29A 0.9300 . ?
C30 C31 1.413(10) . ?
C30 H30A 0.9300 . ?
C31 C32 1.371(9) . ?
C31 H31A 0.9300 . ?
C32 C33 1.424(8) . ?
C32 H32A 0.9300 . ?
C33 C34 1.424(8) . ?
C35 U2 2.849(6) . ?
C36 O14 1.221(10) . ?
C36 O13 1.250(9) . ?
O15 U2 1.745(5) . ?
O16 U2 1.736(6) . ?
N1 C41 1.344(12) . ?
N1 C37 1.365(15) . ?
N1 H1A 0.8600 . ?
N2 C48 1.344(12) . ?
N2 C47 1.393(14) . ?
N2 H2B 0.8600 . ?
C37 C38 1.367(15) . ?
C37 H37A 0.9300 . ?
C38 C39 1.443(12) . ?
C38 H38A 0.9300 . ?
C39 C40 1.374(14) . ?
C39 C42 1.498(13) . ?
C40 C41 1.379(13) . ?
C40 H40A 0.9300 . ?
C41 H41A 0.9300 . ?
C42 C43 1.504(11) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.545(12) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 C45 1.471(12) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 C49 1.368(12) . ?
C45 C46 1.398(12) . ?
C46 C47 1.351(14) . ?
C46 H46A 0.9300 . ?
C47 H47A 0.9300 . ?
C48 C49 1.368(12) . ?
C48 H48A 0.9300 . ?
C49 H49A 0.9300 . ?

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
O6 U1 O5 178.3(2) . . ?
O6 U1 O13 91.5(2) . 3_465 ?
O5 U1 O13 90.2(2) . 3_465 ?
O6 U1 O2 87.1(2) . 3_455 ?
O5 U1 O2 91.3(2) . 3_455 ?
O13 U1 O2 161.42(15) 3_465 3_455 ?
O6 U1 O1 93.8(2) . . ?
O5 U1 O1 86.7(2) . . ?
O13 U1 O1 77.15(16) 3_465 . ?
O2 U1 O1 84.44(15) 3_455 . ?
O6 U1 O7 88.6(2) . . ?
O5 U1 O7 91.9(2) . . ?
O13 U1 O7 71.70(15) 3_465 . ?
O2 U1 O7 126.74(14) 3_455 . ?
O1 U1 O7 148.81(15) . . ?
O6 U1 O8 90.8(2) . . ?
O5 U1 O8 88.2(2) . . ?
O13 U1 O8 123.59(15) 3_465 . ?
O2 U1 O8 74.97(15) 3_455 . ?
O1 U1 O8 158.67(16) . . ?
O7 U1 O8 52.03(15) . . ?
O6 U1 C24 87.4(2) . . ?
O5 U1 C24 92.3(2) . . ?
O13 U1 C24 97.95(17) 3_465 . ?
O2 U1 C24 100.49(17) 3_455 . ?
O1 U1 C24 174.99(17) . . ?
O7 U1 C24 26.26(16) . . ?
O8 U1 C24 25.95(17) . . ?
C11 O1 U1 142.3(5) . . ?
C11 O2 U1 126.5(4) . 3_455 ?
C2 C1 C9 120.5(6) . . ?
C2 C1 C11 116.3(7) . . ?
C9 C1 C11 123.2(7) . . ?
C1 C2 C3 121.3(7) . . ?
C1 C2 H2A 119.4 . . ?
C3 C2 H2A 119.4 . . ?
C4 C3 C2 119.5(8) . . ?
C4 C3 H3A 120.2 . . ?
C2 C3 H3A 120.2 . . ?
C3 C4 C10 121.5(6) . . ?
C3 C4 C12 119.7(7) . . ?
C10 C4 C12 118.7(7) . . ?
C6 C5 C10 121.9(9) . . ?
C6 C5 H5A 119.1 . . ?
C10 C5 H5A 119.1 . . ?
C5 C6 C7 119.4(10) . . ?
C5 C6 H6A 120.3 . . ?
C7 C6 H6A 120.3 . . ?
C8 C7 C6 121.3(11) . . ?
C8 C7 H7A 119.4 . . ?
C6 C7 H7A 119.4 . . ?
C7 C8 C9 121.9(9) . . ?
C7 C8 H8A 119.0 . . ?
C9 C8 H8A 119.0 . . ?
C8 C9 C1 124.4(7) . . ?
C8 C9 C10 117.4(7) . . ?
C1 C9 C10 118.0(7) . . ?
C5 C10 C4 122.7(7) . . ?
C5 C10 C9 118.1(8) . . ?
C4 C10 C9 119.2(7) . . ?
O1 C11 O2 122.9(5) . . ?
O1 C11 C1 117.2(6) . . ?
O2 C11 C1 119.9(6) . . ?
O3 C12 O4 119.4(6) . . ?
O3 C12 C4 119.9(6) . . ?
O4 C12 C4 120.7(5) . . ?
O3 C12 U2 59.7(3) . 4_666 ?
O4 C12 U2 59.9(3) . 4_666 ?
C4 C12 U2 177.9(6) . 4_666 ?
C12 O3 U2 94.6(4) . 4_666 ?
C12 O4 U2 94.0(4) . 4_666 ?
C24 O7 U1 94.1(4) . . ?
C24 O8 U1 93.9(4) . . ?
C14 C13 C21 119.7(5) . . ?
C14 C13 C23 116.5(5) . . ?
C21 C13 C23 123.8(5) . . ?
C13 C14 C15 122.0(6) . . ?
C13 C14 H14A 119.0 . . ?
C15 C14 H14A 119.0 . . ?
C14 C15 C16 120.2(6) . . ?
C14 C15 H15A 119.9 . . ?
C16 C15 H15A 119.9 . . ?
C15 C16 C22 120.3(5) . . ?
C15 C16 C24 115.6(5) . . ?
C22 C16 C24 124.1(6) . . ?
C18 C17 C22 121.6(6) . . ?
C18 C17 H17A 119.2 . . ?
C22 C17 H17A 119.2 . . ?
C17 C18 C19 120.4(6) . . ?
C17 C18 H18A 119.8 . . ?
C19 C18 H18A 119.8 . . ?
C20 C19 C18 120.4(6) . . ?
C20 C19 H19A 119.8 . . ?
C18 C19 H19A 119.8 . . ?
C19 C20 C21 121.2(6) . . ?
C19 C20 H20A 119.4 . . ?
C21 C20 H20A 119.4 . . ?
C20 C21 C13 123.0(5) . . ?
C20 C21 C22 118.4(5) . . ?
C13 C21 C22 118.6(5) . . ?
C16 C22 C17 123.1(5) . . ?
C16 C22 C21 119.0(5) . . ?
C17 C22 C21 117.9(5) . . ?
O9 C23 O10 119.0(5) . . ?
O9 C23 C13 123.8(6) . . ?
O10 C23 C13 117.2(6) . . ?
O9 C23 U2 60.1(3) . . ?
O10 C23 U2 58.9(3) . . ?
C13 C23 U2 174.6(5) . . ?
O8 C24 O7 119.2(6) . . ?
O8 C24 C16 122.7(6) . . ?
O7 C24 C16 118.1(6) . . ?
O8 C24 U1 60.1(3) . . ?
O7 C24 U1 59.7(3) . . ?
C16 C24 U1 171.8(5) . . ?
C23 O9 U2 93.7(4) . . ?
C23 O10 U2 94.8(4) . . ?
C35 O11 U2 94.1(4) . . ?
C35 O12 U2 95.3(4) . . ?
C26 C25 C33 119.8(5) . . ?
C26 C25 C35 116.1(6) . . ?
C33 C25 C35 124.1(5) . . ?
C25 C26 C27 121.8(6) . . ?
C25 C26 H26A 119.1 . . ?
C27 C26 H26A 119.1 . . ?
C28 C27 C26 120.1(6) . . ?
C28 C27 H27A 119.9 . . ?
C26 C27 H27A 119.9 . . ?
C27 C28 C34 119.8(6) . . ?
C27 C28 C36 118.9(6) . . ?
C34 C28 C36 121.2(6) . . ?
C30 C29 C34 121.3(6) . . ?
C30 C29 H29A 119.3 . . ?
C34 C29 H29A 119.3 . . ?
C29 C30 C31 119.6(7) . . ?
C29 C30 H30A 120.2 . . ?
C31 C30 H30A 120.2 . . ?
C32 C31 C30 120.5(7) . . ?
C32 C31 H31A 119.7 . . ?
C30 C31 H31A 119.7 . . ?
C31 C32 C33 121.4(6) . . ?
C31 C32 H32A 119.3 . . ?
C33 C32 H32A 119.3 . . ?
C34 C33 C32 117.4(6) . . ?
C34 C33 C25 118.5(6) . . ?
C32 C33 C25 124.0(5) . . ?
C29 C34 C28 120.4(6) . . ?
C29 C34 C33 119.7(6) . . ?
C28 C34 C33 119.9(6) . . ?
O11 C35 O12 118.0(6) . . ?
O11 C35 C25 123.8(6) . . ?
O12 C35 C25 118.2(6) . . ?
O11 C35 U2 59.6(3) . . ?
O12 C35 U2 58.4(3) . . ?
C25 C35 U2 175.7(5) . . ?
O14 C36 O13 124.6(7) . . ?
O14 C36 C28 120.1(8) . . ?
O13 C36 C28 115.2(7) . . ?
C36 O13 U1 137.8(5) . 3_465 ?
O16 U2 O15 179.6(3) . . ?
O16 U2 O12 88.9(2) . . ?
O15 U2 O12 91.5(2) . . ?
O16 U2 O10 89.7(2) . . ?
O15 U2 O10 90.5(2) . . ?
O12 U2 O10 65.93(15) . . ?
O16 U2 O11 91.0(2) . . ?
O15 U2 O11 89.2(2) . . ?
O12 U2 O11 52.65(15) . . ?
O10 U2 O11 118.54(15) . . ?
O16 U2 O3 90.2(2) . 4_465 ?
O15 U2 O3 89.4(2) . 4_465 ?
O12 U2 O3 173.34(15) . 4_465 ?
O10 U2 O3 120.67(15) . 4_465 ?
O11 U2 O3 120.78(15) . 4_465 ?
O16 U2 O4 89.8(2) . 4_465 ?
O15 U2 O4 90.0(2) . 4_465 ?
O12 U2 O4 121.58(15) . 4_465 ?
O10 U2 O4 172.46(15) . 4_465 ?
O11 U2 O4 68.99(15) . 4_465 ?
O3 U2 O4 51.81(15) 4_465 4_465 ?
O16 U2 O9 90.7(2) . . ?
O15 U2 O9 89.1(2) . . ?
O12 U2 O9 118.35(14) . . ?
O10 U2 O9 52.42(14) . . ?
O11 U2 O9 170.80(15) . . ?
O3 U2 O9 68.26(15) 4_465 . ?
O4 U2 O9 120.07(15) 4_465 . ?
O16 U2 C12 91.0(3) . 4_465 ?
O15 U2 C12 88.7(2) . 4_465 ?
O12 U2 C12 147.66(16) . 4_465 ?
O10 U2 C12 146.41(16) . 4_465 ?
O11 U2 C12 95.03(16) . 4_465 ?
O3 U2 C12 25.75(16) 4_465 4_465 ?
O4 U2 C12 26.09(16) 4_465 4_465 ?
O9 U2 C12 93.99(16) . 4_465 ?
O16 U2 C23 89.6(2) . . ?
O15 U2 C23 90.5(2) . . ?
O12 U2 C23 92.17(16) . . ?
O10 U2 C23 26.25(16) . . ?
O11 U2 C23 144.79(17) . . ?
O3 U2 C23 94.42(17) 4_465 . ?
O4 U2 C23 146.22(17) 4_465 . ?
O9 U2 C23 26.18(16) . . ?
C12 U2 C23 120.16(18) 4_465 . ?
O16 U2 C35 89.5(2) . . ?
O15 U2 C35 90.8(2) . . ?
O12 U2 C35 26.31(17) . . ?
O10 U2 C35 92.24(16) . . ?
O11 U2 C35 26.34(16) . . ?
O3 U2 C35 147.09(17) 4_465 . ?
O4 U2 C35 95.28(17) 4_465 . ?
O9 U2 C35 144.65(16) . . ?
C12 U2 C35 121.35(18) 4_465 . ?
C23 U2 C35 118.48(19) . . ?
C41 N1 C37 121.0(10) . . ?
C41 N1 H1A 119.5 . . ?
C37 N1 H1A 119.5 . . ?
C48 N2 C47 121.5(9) . . ?
C48 N2 H2B 119.3 . . ?
C47 N2 H2B 119.3 . . ?
N1 C37 C38 121.9(10) . . ?
N1 C37 H37A 119.1 . . ?
C38 C37 H37A 119.1 . . ?
C37 C38 C39 117.5(11) . . ?
C37 C38 H38A 121.2 . . ?
C39 C38 H38A 121.2 . . ?
C40 C39 C38 118.7(10) . . ?
C40 C39 C42 123.1(8) . . ?
C38 C39 C42 118.3(10) . . ?
C39 C40 C41 121.1(9) . . ?
C39 C40 H40A 119.5 . . ?
C41 C40 H40A 119.5 . . ?
N1 C41 C40 119.9(11) . . ?
N1 C41 H41A 120.1 . . ?
C40 C41 H41A 120.1 . . ?
C39 C42 C43 115.4(8) . . ?
C39 C42 H42A 108.4 . . ?
C43 C42 H42A 108.4 . . ?
C39 C42 H42B 108.4 . . ?
C43 C42 H42B 108.4 . . ?
H42A C42 H42B 107.5 . . ?
C42 C43 C44 113.3(8) . . ?
C42 C43 H43A 108.9 . . ?
C44 C43 H43A 108.9 . . ?
C42 C43 H43B 108.9 . . ?
C44 C43 H43B 108.9 . . ?
H43A C43 H43B 107.7 . . ?
C45 C44 C43 116.3(8) . . ?
C45 C44 H44A 108.2 . . ?
C43 C44 H44A 108.2 . . ?
C45 C44 H44B 108.2 . . ?
C43 C44 H44B 108.2 . . ?
H44A C44 H44B 107.4 . . ?
C49 C45 C46 117.5(9) . . ?
C49 C45 C44 124.7(8) . . ?
C46 C45 C44 117.8(9) . . ?
C47 C46 C45 121.8(10) . . ?
C47 C46 H46A 119.1 . . ?
C45 C46 H46A 119.1 . . ?
C46 C47 N2 118.1(10) . . ?
C46 C47 H47A 121.0 . . ?
N2 C47 H47A 121.0 . . ?
N2 C48 C49 119.4(10) . . ?
N2 C48 H48A 120.3 . . ?
C49 C48 H48A 120.3 . . ?
C48 C49 C45 121.6(9) . . ?
C48 C49 H49A 119.2 . . ?
C45 C49 H49A 119.2 . . ?

_refine_diff_density_max         1.518
_refine_diff_density_min         -1.518
_refine_diff_density_rms         0.161

####################################################################### 
# 
# 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_SHX97
_database_code_depnum_ccdc_archive 'CCDC 1575473'
_audit_update_record             
;
2017-09-20 deposited with the CCDC.
2018-02-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H18 O16 U2, C13 H16 N2, C2 H6 O'
_chemical_formula_sum            'C51 H40 N2 O17 U2'
_chemical_formula_weight         1428.91

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   16.7566(9)
_cell_length_b                   22.7781(9)
_cell_length_c                   13.8044(9)
_cell_angle_alpha                90
_cell_angle_beta                 92.711(5)
_cell_angle_gamma                90
_cell_volume                     5263.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    21137
_cell_measurement_theta_min      3.04
_cell_measurement_theta_max      25.39

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_F_000             2720
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.280
_exptl_absorpt_coefficient_mu    6.217
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.105
_exptl_absorpt_correction_T_max  0.175
_exptl_absorpt_process_details   ABSCOR(Higashi,1995)
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'rigaku r-axis rapid'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21137
_diffrn_reflns_av_unetI/netI     0.0938
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.041
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             9631
_reflns_number_gt                7394
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.000 357 179 ' '
2 1.000 1.000 0.500 357 178 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0652P)²+34.9391P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9592
_refine_ls_number_parameters     649
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0668
_refine_ls_wR_factor_ref         0.1652
_refine_ls_wR_factor_gt          0.1544
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 1.00228(2) 0.60785(2) 0.44970(3) 0.02398(15) Uani 1 1 d . U . . .
U2 U 0.60880(2) 1.00715(2) 0.27317(3) 0.02155(14) Uani 1 1 d . U . . .
O1 O 0.9574(4) 0.7094(3) 0.4364(6) 0.033(2) Uani 1 1 d . . . . .
O2 O 0.8873(5) 0.6473(3) 0.3515(7) 0.041(2) Uani 1 1 d . . . . .
O3 O 0.7226(5) 0.9483(3) 0.3316(6) 0.0351(19) Uani 1 1 d . U . . .
O4 O 0.6200(4) 0.9003(3) 0.2726(6) 0.0281(19) Uani 1 1 d . . . . .
C1 C 0.8362(7) 0.7475(5) 0.3611(8) 0.029(3) Uani 1 1 d . . . . .
C2 C 0.8651(6) 0.8027(5) 0.3734(9) 0.031(3) Uani 1 1 d . . . . .
H2A H 0.918718 0.808389 0.391493 0.037 Uiso 1 1 calc R U . . .
C3 C 0.8153(7) 0.8507(5) 0.3590(9) 0.030(3) Uani 1 1 d . U . . .
H3A H 0.835536 0.888341 0.369045 0.036 Uiso 1 1 calc R U . . .
C4 C 0.7365(6) 0.8436(4) 0.3302(8) 0.022(2) Uani 1 1 d . . . . .
C5 C 0.6204(6) 0.7743(4) 0.2930(7) 0.018(2) Uani 1 1 d . U . . .
H5A H 0.585112 0.805484 0.283636 0.021 Uiso 1 1 calc R U . . .
C6 C 0.5929(6) 0.7190(5) 0.2820(8) 0.028(3) Uani 1 1 d . . . . .
H6A H 0.539181 0.712775 0.265146 0.033 Uiso 1 1 calc R U . . .
C7 C 0.6433(7) 0.6714(5) 0.2954(8) 0.030(3) Uani 1 1 d . . . . .
H7A H 0.623623 0.633419 0.288380 0.037 Uiso 1 1 calc R U . . .
C8 C 0.7220(7) 0.6808(5) 0.3190(8) 0.025(2) Uani 1 1 d . . . . .
H8A H 0.754963 0.648133 0.327522 0.031 Uiso 1 1 calc R U . . .
C10 C 0.7567(6) 0.7364(5) 0.3313(8) 0.024(2) Uani 1 1 d . . . . .
C11 C 0.8969(7) 0.6985(5) 0.3831(8) 0.029(3) Uani 1 1 d . . . . .
C12 C 0.6907(7) 0.8986(5) 0.3097(8) 0.027(3) Uani 1 1 d . . . . .
O5 O 0.9405(4) 0.5255(3) 0.3830(5) 0.0251(17) Uani 1 1 d . . . . .
O6 O 0.9017(4) 0.4579(3) 0.4874(6) 0.0300(19) Uani 1 1 d . . . . .
O7 O 0.5158(4) 0.4610(3) 0.2939(6) 0.0296(18) Uani 1 1 d . . . . .
O8 O 0.5166(4) 0.5571(3) 0.2826(7) 0.041(2) Uani 1 1 d . . . . .
C13 C 0.8016(6) 0.5007(4) 0.3829(7) 0.020(2) Uani 1 1 d . U . . .
C14 C 0.7477(8) 0.4952(5) 0.4480(9) 0.034(3) Uani 1 1 d . . . . .
H14A H 0.763684 0.488466 0.512485 0.041 Uiso 1 1 calc R U . . .
C15 C 0.6653(7) 0.4995(5) 0.4211(10) 0.033(3) Uani 1 1 d . . . . .
H15A H 0.627952 0.496337 0.468575 0.040 Uiso 1 1 calc R U . . .
C16 C 0.6402(6) 0.5081(4) 0.3292(9) 0.027(3) Uani 1 1 d . . . . .
C17 C 0.6720(9) 0.5232(7) 0.1566(10) 0.051(4) Uani 1 1 d . . . . .
H17B H 0.617837 0.525899 0.139228 0.061 Uiso 1 1 calc R U . . .
C18 C 0.7262(11) 0.5277(10) 0.0868(12) 0.085(6) Uani 1 1 d . . . . .
H18A H 0.709172 0.533053 0.022278 0.102 Uiso 1 1 calc R U . . .
C19 C 0.8077(10) 0.5241(11) 0.1127(12) 0.095(8) Uani 1 1 d . . . . .
H19A H 0.844356 0.528304 0.064583 0.115 Uiso 1 1 calc R U . . .
C20 C 0.8361(8) 0.5146(8) 0.2078(10) 0.061(5) Uani 1 1 d . . . . .
H20A H 0.890570 0.511345 0.222756 0.073 Uiso 1 1 calc R U . . .
C21 C 0.6965(7) 0.5143(5) 0.2560(9) 0.029(3) Uani 1 1 d . . . . .
C22 C 0.7790(7) 0.5100(5) 0.2829(8) 0.027(3) Uani 1 1 d . . . . .
C23 C 0.8868(6) 0.4937(4) 0.4178(8) 0.021(2) Uani 1 1 d . U . . .
C24 C 0.5544(6) 0.5090(5) 0.3008(8) 0.026(3) Uani 1 1 d . . . . .
O9 O 1.0903(4) 0.6672(3) 0.5396(6) 0.0298(19) Uani 1 1 d . . . . .
O10 O 1.0503(8) 0.6762(6) 0.6895(10) 0.090(4) Uani 1 1 d . U . . .
O11 O 1.3825(4) 0.8854(3) 0.7130(6) 0.0276(18) Uani 1 1 d . . . . .
O12 O 1.0616(5) 0.6162(4) 0.3471(7) 0.042(2) Uani 1 1 d . . . . .
C25 C 1.1529(7) 0.7388(5) 0.6400(8) 0.031(3) Uani 1 1 d . . . . .
C26 C 1.1285(7) 0.7948(6) 0.6261(10) 0.040(3) Uani 1 1 d . . . . .
H26A H 1.075768 0.802683 0.606292 0.049 Uiso 1 1 calc R U . . .
C27 C 1.1822(7) 0.8404(6) 0.6415(9) 0.034(3) Uani 1 1 d . . . . .
H27A H 1.164965 0.878771 0.630422 0.041 Uiso 1 1 calc R U . . .
C28 C 1.2597(6) 0.8309(5) 0.6725(8) 0.027(3) Uani 1 1 d . . . . .
C29 C 1.3655(7) 0.7589(5) 0.7176(8) 0.028(3) Uani 1 1 d . . . . .
H29A H 1.401578 0.789434 0.729223 0.033 Uiso 1 1 calc R U . . .
C30 C 1.3906(7) 0.7016(6) 0.7306(9) 0.038(3) Uani 1 1 d . . . . .
H30A H 1.443384 0.693845 0.750344 0.045 Uiso 1 1 calc R U . . .
C31 C 1.3364(8) 0.6548(5) 0.7139(9) 0.038(3) Uani 1 1 d . . . . .
H31A H 1.353190 0.616138 0.721857 0.046 Uiso 1 1 calc R U . . .
C32 C 1.2592(8) 0.6671(5) 0.6862(8) 0.032(3) Uani 1 1 d . . . . .
H32A H 1.222923 0.636464 0.677110 0.039 Uiso 1 1 calc R U . . .
C33 C 1.2870(6) 0.7718(5) 0.6872(7) 0.022(2) Uani 1 1 d . . . . .
C34 C 1.2328(6) 0.7265(5) 0.6707(8) 0.024(2) Uani 1 1 d . . . . .
C35 C 1.0931(8) 0.6895(6) 0.6228(9) 0.039(3) Uani 1 1 d . . . . .
C36 C 1.3080(7) 0.8850(5) 0.6842(8) 0.028(3) Uani 1 1 d . . . . .
O13 O 0.9438(5) 0.5999(3) 0.5460(6) 0.0384(19) Uani 1 1 d . U . . .
O14 O 1.2763(5) 0.9340(4) 0.6714(7) 0.044(2) Uani 1 1 d . . . . .
O15 O 0.5722(5) 1.0059(4) 0.3875(7) 0.042(2) Uani 1 1 d . U . . .
O16 O 0.6464(5) 1.0097(4) 0.1574(7) 0.044(2) Uani 1 1 d . U . . .
N1 N 0.8098(7) 0.7591(6) 0.6016(9) 0.055(3) Uani 1 1 d . . . . .
H1A H 0.851848 0.780146 0.613045 0.066 Uiso 1 1 calc R U . . .
C9 C 0.7030(6) 0.7862(5) 0.3188(8) 0.023(2) Uani 1 1 d . . . . .
C37 C 0.8160(11) 0.6990(8) 0.6014(10) 0.063(5) Uani 1 1 d . . . . .
H37A H 0.865134 0.681115 0.614827 0.075 Uiso 1 1 calc R U . . .
C38 C 0.7496(9) 0.6658(7) 0.5815(10) 0.049(4) Uani 1 1 d . . . . .
H38A H 0.753975 0.625092 0.580633 0.058 Uiso 1 1 calc R U . . .
C39 C 0.6752(8) 0.6918(6) 0.5624(9) 0.041(3) Uani 1 1 d . . . . .
C40 C 0.6717(8) 0.7527(6) 0.5659(9) 0.042(3) Uani 1 1 d . . . . .
H40A H 0.622928 0.771717 0.555812 0.050 Uiso 1 1 calc R U . . .
C41 C 0.7400(8) 0.7850(7) 0.5843(10) 0.047(4) Uani 1 1 d . . . . .
H41A H 0.737061 0.825762 0.584511 0.057 Uiso 1 1 calc R U . . .
C42 C 0.6023(8) 0.6548(6) 0.5430(10) 0.045(4) Uani 1 1 d . . . . .
H42A H 0.594916 0.630009 0.598998 0.054 Uiso 1 1 calc R U . . .
H42B H 0.611461 0.629292 0.488376 0.054 Uiso 1 1 calc R U . . .
C43 C 0.5261(7) 0.6890(6) 0.5214(9) 0.035(3) Uani 1 1 d . . . . .
H43A H 0.534049 0.716050 0.468524 0.043 Uiso 1 1 calc R U . . .
H43B H 0.513512 0.711790 0.578015 0.043 Uiso 1 1 calc R U . . .
C44 C 0.4550(8) 0.6478(6) 0.4936(10) 0.043(3) Uani 1 1 d . . . . .
H44A H 0.469527 0.623842 0.439149 0.052 Uiso 1 1 calc R U . . .
H44B H 0.446973 0.621637 0.547706 0.052 Uiso 1 1 calc R U . . .
C45 C 0.3788(8) 0.6769(6) 0.4678(8) 0.034(3) Uani 1 1 d . . . . .
C46 C 0.3119(9) 0.6457(6) 0.4334(9) 0.042(3) Uani 1 1 d . . . . .
H46A H 0.317144 0.605250 0.426603 0.051 Uiso 1 1 calc R U . . .
C47 C 0.2414(8) 0.6692(6) 0.4096(9) 0.037(3) Uani 1 1 d . . . . .
H47A H 0.198574 0.645767 0.388433 0.045 Uiso 1 1 calc R U . . .
C48 C 0.2934(7) 0.7610(5) 0.4473(9) 0.033(3) Uani 1 1 d . . . . .
H48A H 0.286553 0.801486 0.450893 0.040 Uiso 1 1 calc R U . . .
C49 C 0.3660(7) 0.7361(5) 0.4738(9) 0.034(3) Uani 1 1 d . . . . .
H49A H 0.407613 0.760161 0.496443 0.041 Uiso 1 1 calc R U . . .
N2 N 0.2334(7) 0.7268(5) 0.4166(7) 0.042(3) Uani 1 1 d . . . . .
H2B H 0.187906 0.742538 0.400897 0.051 Uiso 1 1 calc R U . . .
C50 C 0.4459(10) 0.8912(6) 0.4374(10) 0.054(4) Uani 1 1 d . . . . .
H50A H 0.459556 0.917290 0.386037 0.081 Uiso 1 1 calc R U . . .
H50B H 0.424862 0.855355 0.410175 0.081 Uiso 1 1 calc R U . . .
H50C H 0.406491 0.909463 0.475672 0.081 Uiso 1 1 calc R U . . .
C51 C 0.5178(9) 0.8784(7) 0.4990(12) 0.058(4) Uani 1 1 d . . . . .
H51A H 0.557615 0.861227 0.458890 0.070 Uiso 1 1 calc R U . . .
H51B H 0.539285 0.915214 0.524240 0.070 Uiso 1 1 calc R U . . .
O17 O 0.5062(6) 0.8403(4) 0.5781(7) 0.056(3) Uani 1 1 d . . . . .
H17A H 0.472318 0.854157 0.612447 0.084 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O13 1.698(9) . ?
U1 O12 1.779(9) . ?
U1 O5 2.313(7) . ?
U1 O9 2.317(7) . ?
U1 O6 2.335(7) 3_766 ?
U1 O1 2.436(8) . ?
U1 O2 2.472(8) . ?
U1 C11 2.842(11) . ?
U2 O15 1.721(10) . ?
U2 O16 1.746(10) . ?
U2 O3 2.436(7) . ?
U2 O14 2.439(8) 3_776 ?
U2 O4 2.441(7) . ?
U2 O11 2.460(7) 3_776 ?
U2 O7 2.479(7) 2_655 ?
U2 O8 2.479(7) 2_655 ?
U2 C12 2.860(11) . ?
U2 C24 2.874(10) 2_655 ?
U2 C36 2.872(12) 3_776 ?
O1 C11 1.250(13) . ?
O2 C11 1.253(14) . ?
O3 C12 1.282(13) . ?
O4 C12 1.268(13) . ?
C1 C2 1.356(15) . ?
C1 C10 1.399(15) . ?
C1 C11 1.530(16) . ?
C2 C3 1.384(15) . ?
C2 H2A 0.9300 . ?
C3 C4 1.371(15) . ?
C3 H3A 0.9300 . ?
C4 C9 1.428(14) . ?
C4 C12 1.491(14) . ?
C5 C6 1.346(15) . ?
C5 C9 1.438(14) . ?
C5 H5A 0.9300 . ?
C6 C7 1.381(15) . ?
C6 H6A 0.9300 . ?
C7 C8 1.361(16) . ?
C7 H7A 0.9300 . ?
C8 C10 1.402(15) . ?
C8 H8A 0.9300 . ?
C10 C9 1.452(15) . ?
O5 C23 1.266(13) . ?
O6 C23 1.277(13) . ?
O7 C24 1.272(13) . ?
O8 C24 1.284(13) . ?
C13 C14 1.310(17) . ?
C13 C22 1.430(15) . ?
C13 C23 1.492(14) . ?
C14 C15 1.416(16) . ?
C14 H14A 0.9300 . ?
C15 C16 1.332(17) . ?
C15 H15A 0.9300 . ?
C16 C21 1.421(17) . ?
C16 C24 1.473(14) . ?
C17 C18 1.36(2) . ?
C17 C21 1.428(17) . ?
C17 H17B 0.9300 . ?
C18 C19 1.40(2) . ?
C18 H18A 0.9300 . ?
C19 C20 1.39(2) . ?
C19 H19A 0.9300 . ?
C20 C22 1.448(18) . ?
C20 H20A 0.9300 . ?
C21 C22 1.417(15) . ?
O9 C35 1.254(14) . ?
O10 C35 1.231(16) . ?
O11 C36 1.291(13) . ?
C25 C26 1.349(17) . ?
C25 C34 1.414(16) . ?
C25 C35 1.518(16) . ?
C26 C27 1.385(17) . ?
C26 H26A 0.9300 . ?
C27 C28 1.364(15) . ?
C27 H27A 0.9300 . ?
C28 C33 1.433(15) . ?
C28 C36 1.479(15) . ?
C29 C30 1.380(16) . ?
C29 C33 1.393(15) . ?
C29 H29A 0.9300 . ?
C30 C31 1.413(18) . ?
C30 H30A 0.9300 . ?
C31 C32 1.359(17) . ?
C31 H31A 0.9300 . ?
C32 C34 1.437(15) . ?
C32 H32A 0.9300 . ?
C33 C34 1.386(15) . ?
C36 O14 1.246(13) . ?
N1 C41 1.322(17) . ?
N1 C37 1.37(2) . ?
N1 H1A 0.8600 . ?
C37 C38 1.36(2) . ?
C37 H37A 0.9300 . ?
C38 C39 1.395(18) . ?
C38 H38A 0.9300 . ?
C39 C40 1.389(19) . ?
C39 C42 1.498(19) . ?
C40 C41 1.374(19) . ?
C40 H40A 0.9300 . ?
C41 H41A 0.9300 . ?
C42 C43 1.513(17) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.549(19) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 C45 1.467(17) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 C49 1.368(17) . ?
C45 C46 1.391(18) . ?
C46 C47 1.325(18) . ?
C46 H46A 0.9300 . ?
C47 N2 1.324(16) . ?
C47 H47A 0.9300 . ?
C48 N2 1.326(16) . ?
C48 C49 1.376(16) . ?
C48 H48A 0.9300 . ?
C49 H49A 0.9300 . ?
N2 H2B 0.8600 . ?
C50 C51 1.47(2) . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 O17 1.416(17) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
O17 H17A 0.8200 . ?

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
O13 U1 O12 178.7(4) . . ?
O13 U1 O5 87.7(3) . . ?
O12 U1 O5 91.6(3) . . ?
O13 U1 O9 91.1(3) . . ?
O12 U1 O9 89.9(3) . . ?
O5 U1 O9 161.5(3) . . ?
O13 U1 O6 93.1(3) . 3_766 ?
O12 U1 O6 87.9(4) . 3_766 ?
O5 U1 O6 85.2(2) . 3_766 ?
O9 U1 O6 76.4(3) . 3_766 ?
O13 U1 O1 88.4(3) . . ?
O12 U1 O1 91.2(3) . . ?
O5 U1 O1 127.6(2) . . ?
O9 U1 O1 70.9(3) . . ?
O6 U1 O1 147.3(2) 3_766 . ?
O13 U1 O2 90.2(4) . . ?
O12 U1 O2 88.6(4) . . ?
O5 U1 O2 75.8(3) . . ?
O9 U1 O2 122.8(3) . . ?
O6 U1 O2 160.5(3) 3_766 . ?
O1 U1 O2 52.0(3) . . ?
O13 U1 C11 87.6(4) . . ?
O12 U1 C11 91.5(4) . . ?
O5 U1 C11 101.6(3) . . ?
O9 U1 C11 96.8(3) . . ?
O6 U1 C11 173.2(3) 3_766 . ?
O1 U1 C11 26.0(3) . . ?
O2 U1 C11 26.1(3) . . ?
O15 U2 O16 179.0(4) . . ?
O15 U2 O3 89.7(4) . . ?
O16 U2 O3 90.6(4) . . ?
O15 U2 O14 91.8(4) . 3_776 ?
O16 U2 O14 87.4(4) . 3_776 ?
O3 U2 O14 66.7(3) . 3_776 ?
O15 U2 O4 91.0(3) . . ?
O16 U2 O4 89.9(3) . . ?
O3 U2 O4 52.7(2) . . ?
O14 U2 O4 119.3(3) 3_776 . ?
O15 U2 O11 88.2(3) . 3_776 ?
O16 U2 O11 90.9(4) . 3_776 ?
O3 U2 O11 118.6(3) . 3_776 ?
O14 U2 O11 52.1(3) 3_776 3_776 ?
O4 U2 O11 171.3(2) . 3_776 ?
O15 U2 O7 90.3(3) . 2_655 ?
O16 U2 O7 90.4(3) . 2_655 ?
O3 U2 O7 121.5(3) . 2_655 ?
O14 U2 O7 171.5(3) 3_776 2_655 ?
O4 U2 O7 68.9(2) . 2_655 ?
O11 U2 O7 119.8(2) 3_776 2_655 ?
O15 U2 O8 87.7(4) . 2_655 ?
O16 U2 O8 92.2(4) . 2_655 ?
O3 U2 O8 173.5(3) . 2_655 ?
O14 U2 O8 119.3(3) 3_776 2_655 ?
O4 U2 O8 121.4(2) . 2_655 ?
O11 U2 O8 67.3(2) 3_776 2_655 ?
O7 U2 O8 52.6(3) 2_655 2_655 ?
O15 U2 C12 90.7(4) . . ?
O16 U2 C12 90.0(4) . . ?
O3 U2 C12 26.5(3) . . ?
O14 U2 C12 93.1(3) 3_776 . ?
O4 U2 C12 26.2(3) . . ?
O11 U2 C12 145.1(3) 3_776 . ?
O7 U2 C12 95.0(3) 2_655 . ?
O8 U2 C12 147.5(3) 2_655 . ?
O15 U2 C24 87.3(4) . 2_655 ?
O16 U2 C24 93.0(4) . 2_655 ?
O3 U2 C24 147.4(3) . 2_655 ?
O14 U2 C24 145.8(3) 3_776 2_655 ?
O4 U2 C24 94.9(3) . 2_655 ?
O11 U2 C24 93.7(3) 3_776 2_655 ?
O7 U2 C24 26.2(3) 2_655 2_655 ?
O8 U2 C24 26.5(3) 2_655 2_655 ?
C12 U2 C24 121.1(3) . 2_655 ?
O15 U2 C36 91.0(4) . 3_776 ?
O16 U2 C36 88.1(4) . 3_776 ?
O3 U2 C36 92.2(3) . 3_776 ?
O14 U2 C36 25.5(3) 3_776 3_776 ?
O4 U2 C36 144.8(3) . 3_776 ?
O11 U2 C36 26.6(3) 3_776 3_776 ?
O7 U2 C36 146.3(3) 2_655 3_776 ?
O8 U2 C36 93.8(3) 2_655 3_776 ?
C12 U2 C36 118.6(3) . 3_776 ?
C24 U2 C36 120.3(3) 2_655 3_776 ?
C11 O1 U1 95.5(7) . . ?
C11 O2 U1 93.7(7) . . ?
C12 O3 U2 95.5(7) . . ?
C12 O4 U2 95.7(6) . . ?
C2 C1 C10 122.2(11) . . ?
C2 C1 C11 114.9(10) . . ?
C10 C1 C11 122.9(10) . . ?
C1 C2 C3 120.3(11) . . ?
C1 C2 H2A 119.8 . . ?
C3 C2 H2A 119.8 . . ?
C4 C3 C2 120.9(10) . . ?
C4 C3 H3A 119.5 . . ?
C2 C3 H3A 119.5 . . ?
C3 C4 C9 120.6(9) . . ?
C3 C4 C12 115.8(9) . . ?
C9 C4 C12 123.6(9) . . ?
C6 C5 C9 121.6(10) . . ?
C6 C5 H5A 119.2 . . ?
C9 C5 H5A 119.2 . . ?
C5 C6 C7 121.0(10) . . ?
C5 C6 H6A 119.5 . . ?
C7 C6 H6A 119.5 . . ?
C8 C7 C6 119.3(11) . . ?
C8 C7 H7A 120.3 . . ?
C6 C7 H7A 120.3 . . ?
C7 C8 C10 124.2(10) . . ?
C7 C8 H8A 117.9 . . ?
C10 C8 H8A 117.9 . . ?
C1 C10 C8 125.6(10) . . ?
C1 C10 C9 118.1(10) . . ?
C8 C10 C9 116.1(10) . . ?
O1 C11 O2 118.4(10) . . ?
O1 C11 C1 119.1(10) . . ?
O2 C11 C1 122.4(10) . . ?
O1 C11 U1 58.5(6) . . ?
O2 C11 U1 60.2(6) . . ?
C1 C11 U1 172.3(8) . . ?
O4 C12 O3 116.1(10) . . ?
O4 C12 C4 124.4(10) . . ?
O3 C12 C4 119.6(10) . . ?
O4 C12 U2 58.1(5) . . ?
O3 C12 U2 58.0(5) . . ?
C4 C12 U2 177.5(8) . . ?
C23 O5 U1 128.7(7) . . ?
C23 O6 U1 142.8(7) . 3_766 ?
C24 O7 U2 94.5(6) . 2_645 ?
C24 O8 U2 94.2(6) . 2_645 ?
C14 C13 C22 121.1(10) . . ?
C14 C13 C23 116.6(10) . . ?
C22 C13 C23 122.2(10) . . ?
C13 C14 C15 120.6(11) . . ?
C13 C14 H14A 119.7 . . ?
C15 C14 H14A 119.7 . . ?
C16 C15 C14 121.3(12) . . ?
C16 C15 H15A 119.3 . . ?
C14 C15 H15A 119.3 . . ?
C15 C16 C21 120.1(10) . . ?
C15 C16 C24 121.0(12) . . ?
C21 C16 C24 118.8(10) . . ?
C18 C17 C21 121.4(14) . . ?
C18 C17 H17B 119.3 . . ?
C21 C17 H17B 119.3 . . ?
C17 C18 C19 119.5(15) . . ?
C17 C18 H18A 120.3 . . ?
C19 C18 H18A 120.3 . . ?
C20 C19 C18 122.4(15) . . ?
C20 C19 H19A 118.8 . . ?
C18 C19 H19A 118.8 . . ?
C19 C20 C22 118.7(13) . . ?
C19 C20 H20A 120.7 . . ?
C22 C20 H20A 120.7 . . ?
C22 C21 C16 118.6(10) . . ?
C22 C21 C17 119.6(11) . . ?
C16 C21 C17 121.8(11) . . ?
C21 C22 C13 118.3(10) . . ?
C21 C22 C20 118.5(11) . . ?
C13 C22 C20 123.2(11) . . ?
O5 C23 O6 122.2(9) . . ?
O5 C23 C13 120.2(9) . . ?
O6 C23 C13 117.5(9) . . ?
O7 C24 O8 118.4(9) . . ?
O7 C24 C16 119.5(9) . . ?
O8 C24 C16 122.1(9) . . ?
O7 C24 U2 59.3(5) . 2_645 ?
O8 C24 U2 59.4(5) . 2_645 ?
C16 C24 U2 174.3(8) . 2_645 ?
C35 O9 U1 136.2(8) . . ?
C36 O11 U2 94.8(6) . 3_776 ?
C26 C25 C34 120.4(11) . . ?
C26 C25 C35 119.0(11) . . ?
C34 C25 C35 120.6(11) . . ?
C25 C26 C27 119.8(11) . . ?
C25 C26 H26A 120.1 . . ?
C27 C26 H26A 120.1 . . ?
C28 C27 C26 122.0(12) . . ?
C28 C27 H27A 119.0 . . ?
C26 C27 H27A 119.0 . . ?
C27 C28 C33 119.1(10) . . ?
C27 C28 C36 114.2(10) . . ?
C33 C28 C36 126.6(10) . . ?
C30 C29 C33 121.1(11) . . ?
C30 C29 H29A 119.5 . . ?
C33 C29 H29A 119.5 . . ?
C29 C30 C31 120.2(11) . . ?
C29 C30 H30A 119.9 . . ?
C31 C30 H30A 119.9 . . ?
C32 C31 C30 119.1(11) . . ?
C32 C31 H31A 120.4 . . ?
C30 C31 H31A 120.4 . . ?
C31 C32 C34 121.2(11) . . ?
C31 C32 H32A 119.4 . . ?
C34 C32 H32A 119.4 . . ?
C34 C33 C29 119.6(10) . . ?
C34 C33 C28 118.3(10) . . ?
C29 C33 C28 122.1(10) . . ?
C33 C34 C25 120.3(10) . . ?
C33 C34 C32 118.8(10) . . ?
C25 C34 C32 120.8(10) . . ?
O10 C35 O9 126.0(12) . . ?
O10 C35 C25 117.9(11) . . ?
O9 C35 C25 116.0(10) . . ?
O14 C36 O11 115.9(10) . . ?
O14 C36 C28 120.2(11) . . ?
O11 C36 C28 123.8(10) . . ?
O14 C36 U2 57.4(6) . 3_776 ?
O11 C36 U2 58.6(5) . 3_776 ?
C28 C36 U2 173.2(8) . 3_776 ?
C36 O14 U2 97.1(7) . 3_776 ?
C41 N1 C37 120.7(14) . . ?
C41 N1 H1A 119.7 . . ?
C37 N1 H1A 119.7 . . ?
C4 C9 C5 124.7(9) . . ?
C4 C9 C10 117.6(9) . . ?
C5 C9 C10 117.8(9) . . ?
C38 C37 N1 119.6(15) . . ?
C38 C37 H37A 120.2 . . ?
N1 C37 H37A 120.2 . . ?
C37 C38 C39 121.1(15) . . ?
C37 C38 H38A 119.5 . . ?
C39 C38 H38A 119.5 . . ?
C38 C39 C40 117.1(13) . . ?
C38 C39 C42 120.6(13) . . ?
C40 C39 C42 122.2(12) . . ?
C41 C40 C39 120.4(13) . . ?
C41 C40 H40A 119.8 . . ?
C39 C40 H40A 119.8 . . ?
N1 C41 C40 121.1(14) . . ?
N1 C41 H41A 119.4 . . ?
C40 C41 H41A 119.4 . . ?
C39 C42 C43 114.8(12) . . ?
C39 C42 H42A 108.6 . . ?
C43 C42 H42A 108.6 . . ?
C39 C42 H42B 108.6 . . ?
C43 C42 H42B 108.6 . . ?
H42A C42 H42B 107.5 . . ?
C42 C43 C44 111.7(11) . . ?
C42 C43 H43A 109.3 . . ?
C44 C43 H43A 109.3 . . ?
C42 C43 H43B 109.3 . . ?
C44 C43 H43B 109.3 . . ?
H43A C43 H43B 107.9 . . ?
C45 C44 C43 115.9(11) . . ?
C45 C44 H44A 108.3 . . ?
C43 C44 H44A 108.3 . . ?
C45 C44 H44B 108.3 . . ?
C43 C44 H44B 108.3 . . ?
H44A C44 H44B 107.4 . . ?
C49 C45 C46 113.5(12) . . ?
C49 C45 C44 124.5(12) . . ?
C46 C45 C44 122.0(13) . . ?
C47 C46 C45 124.9(14) . . ?
C47 C46 H46A 117.5 . . ?
C45 C46 H46A 117.5 . . ?
N2 C47 C46 118.4(13) . . ?
N2 C47 H47A 120.8 . . ?
C46 C47 H47A 120.8 . . ?
N2 C48 C49 119.3(12) . . ?
N2 C48 H48A 120.3 . . ?
C49 C48 H48A 120.3 . . ?
C45 C49 C48 122.0(12) . . ?
C45 C49 H49A 119.0 . . ?
C48 C49 H49A 119.0 . . ?
C47 N2 C48 121.9(12) . . ?
C47 N2 H2B 119.1 . . ?
C48 N2 H2B 119.1 . . ?
C51 C50 H50A 109.5 . . ?
C51 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C51 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
O17 C51 C50 115.4(12) . . ?
O17 C51 H51A 108.4 . . ?
C50 C51 H51A 108.4 . . ?
O17 C51 H51B 108.4 . . ?
C50 C51 H51B 108.4 . . ?
H51A C51 H51B 107.5 . . ?
C51 O17 H17A 109.5 . . ?

_refine_diff_density_max         4.890
_refine_diff_density_min         -1.958
_refine_diff_density_rms         0.245

