# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2016

####################################################################### 
# 
# 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_Complex_1
_database_code_depnum_ccdc_archive 'CCDC 1501011'
_audit_update_record             
;
2016-08-25 deposited with the CCDC.
2016-10-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H14 I4 N2 O6 U'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1172.00

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'
I I -0.4742 1.8119 '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                   7.6634(2)
_cell_length_b                   25.2373(7)
_cell_length_c                   15.2304(4)
_cell_angle_alpha                90
_cell_angle_beta                 101.744(4)
_cell_angle_gamma                90
_cell_volume                     2883.95(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    36674
_cell_measurement_theta_min      5.429
_cell_measurement_theta_max      46.132
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.699
_exptl_crystal_F_000             2096
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    9.950
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5538
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2015)'

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36165
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.586
_diffrn_reflns_theta_max         27.030
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6313
_reflns_number_gt                4776
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'

_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)+(0.0386P)²+14.4241P] 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         6313
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.0987
_refine_ls_wR_factor_gt          0.0890
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.27169(4) 0.13536(2) 0.56013(2) 0.03800(9) Uani 1 1 d . . . . .
I1 I 0.02266(8) 0.18389(3) 0.19983(4) 0.06013(17) Uani 1 1 d . . . . .
I3 I 0.55608(8) 0.29596(2) 0.78618(4) 0.06016(17) Uani 1 1 d . . . . .
I2 I -0.03171(12) 0.42304(3) 0.41948(6) 0.0934(3) Uani 1 1 d . . . . .
I4 I 0.53484(15) 0.08764(5) 1.08000(6) 0.1208(4) Uani 1 1 d . . . . .
O4 O 0.2125(8) 0.2257(2) 0.5107(4) 0.0583(16) Uani 1 1 d . . . . .
O2 O 0.4906(7) 0.1400(2) 0.5406(4) 0.0489(13) Uani 1 1 d . . . . .
O1 O 0.0530(7) 0.1323(2) 0.5791(3) 0.0479(13) Uani 1 1 d . . . . .
O3 O 0.1283(8) 0.1655(2) 0.4089(4) 0.0502(14) Uani 1 1 d . . . . .
N1 N 0.2349(8) 0.0355(2) 0.6041(4) 0.0430(15) Uani 1 1 d . . . . .
N2 N 0.2755(8) 0.0602(2) 0.4406(4) 0.0402(14) Uani 1 1 d . . . . .
O6 O 0.4170(8) 0.1173(2) 0.7160(4) 0.0530(14) Uani 1 1 d . . . . .
O5 O 0.3556(8) 0.1996(2) 0.6828(4) 0.0548(15) Uani 1 1 d . . . . .
C7 C 0.2914(11) -0.0294(3) 0.3955(6) 0.049(2) Uani 1 1 d . . . . .
H7 H 0.2833 -0.0651 0.4090 0.059 Uiso 1 1 calc R U . . .
C11 C 0.1394(11) 0.2138(3) 0.4325(5) 0.0447(18) Uani 1 1 d . . . . .
C22 C 0.5843(15) 0.1997(5) 1.0184(7) 0.077(3) Uani 1 1 d . . . . .
H22 H 0.6152 0.2067 1.0795 0.092 Uiso 1 1 calc R U . . .
C5 C 0.2361(9) -0.0058(3) 0.5479(5) 0.0407(17) Uani 1 1 d . . . . .
C4 C 0.2044(11) -0.0571(3) 0.5731(6) 0.052(2) Uani 1 1 d . . . . .
H4 H 0.2091 -0.0851 0.5338 0.062 Uiso 1 1 calc R U . . .
C12 C 0.0629(10) 0.2576(3) 0.3680(5) 0.0438(18) Uani 1 1 d . . . . .
C10 C 0.3072(12) 0.0745(3) 0.3604(6) 0.053(2) Uani 1 1 d . . . . .
H10 H 0.3133 0.1104 0.3477 0.063 Uiso 1 1 calc R U . . .
C19 C 0.4834(10) 0.1799(3) 0.8363(5) 0.0434(18) Uani 1 1 d . . . . .
C6 C 0.2685(9) 0.0081(3) 0.4581(5) 0.0383(17) Uani 1 1 d . . . . .
C3 C 0.1668(12) -0.0666(4) 0.6544(7) 0.061(2) Uani 1 1 d . . . . .
H3 H 0.1449 -0.1010 0.6713 0.073 Uiso 1 1 calc R U . . .
C13 C 0.0074(10) 0.2524(3) 0.2747(6) 0.048(2) Uani 1 1 d . . . . .
C14 C -0.0648(12) 0.2971(4) 0.2264(6) 0.058(2) Uani 1 1 d . . . . .
H14 H -0.1054 0.2940 0.1648 0.069 Uiso 1 1 calc R U . . .
C20 C 0.5380(11) 0.2305(4) 0.8675(5) 0.051(2) Uani 1 1 d . . . . .
C21 C 0.5895(13) 0.2395(4) 0.9586(6) 0.066(3) Uani 1 1 d . . . . .
H21 H 0.6280 0.2730 0.9793 0.079 Uiso 1 1 calc R U . . .
C8 C 0.3259(11) -0.0151(4) 0.3140(6) 0.056(2) Uani 1 1 d . . . . .
H8 H 0.3447 -0.0405 0.2727 0.067 Uiso 1 1 calc R U . . .
C1 C 0.1944(12) 0.0253(4) 0.6843(6) 0.055(2) Uani 1 1 d . . . . .
H1 H 0.1886 0.0535 0.7229 0.065 Uiso 1 1 calc R U . . .
C2 C 0.1609(11) -0.0251(4) 0.7119(6) 0.057(2) Uani 1 1 d . . . . .
H2 H 0.1351 -0.0308 0.7683 0.068 Uiso 1 1 calc R U . . .
C9 C 0.3315(12) 0.0380(4) 0.2955(6) 0.056(2) Uani 1 1 d . . . . .
H9 H 0.3513 0.0494 0.2403 0.067 Uiso 1 1 calc R U . . .
C15 C -0.0781(13) 0.3447(4) 0.2657(7) 0.064(3) Uani 1 1 d . . . . .
H15 H -0.1255 0.3737 0.2314 0.077 Uiso 1 1 calc R U . . .
C17 C 0.0490(11) 0.3061(3) 0.4086(6) 0.049(2) Uani 1 1 d . . . . .
H17 H 0.0862 0.3095 0.4703 0.059 Uiso 1 1 calc R U . . .
C23 C 0.5337(14) 0.1494(5) 0.9894(7) 0.071(3) Uani 1 1 d . . . . .
C16 C -0.0201(12) 0.3495(3) 0.3575(7) 0.058(2) Uani 1 1 d . . . . .
C24 C 0.4856(12) 0.1395(4) 0.8980(6) 0.055(2) Uani 1 1 d . . . . .
H24 H 0.4545 0.1053 0.8779 0.067 Uiso 1 1 calc R U . . .
C18 C 0.4155(11) 0.1653(3) 0.7398(5) 0.0452(18) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.759(5) . ?
U1 O2 1.766(6) . ?
U1 O4 2.415(5) . ?
U1 O6 2.451(5) . ?
U1 O5 2.458(5) . ?
U1 O3 2.463(5) . ?
U1 N2 2.632(6) . ?
U1 N1 2.638(6) . ?
U1 C11 2.816(7) . ?
U1 C18 2.836(8) . ?
I1 C13 2.087(9) . ?
I3 C20 2.087(9) . ?
I2 C16 2.092(10) . ?
I4 C23 2.082(10) . ?
O4 C11 1.246(9) . ?
O3 C11 1.269(9) . ?
N1 C5 1.349(10) . ?
N1 C1 1.345(10) . ?
N2 C6 1.345(9) . ?
N2 C10 1.342(10) . ?
O6 C18 1.265(10) . ?
O5 C18 1.246(9) . ?
C7 C8 1.368(12) . ?
C7 C6 1.380(10) . ?
C11 C12 1.515(10) . ?
C22 C21 1.360(15) . ?
C22 C23 1.374(15) . ?
C5 C4 1.386(11) . ?
C5 C6 1.482(11) . ?
C4 C3 1.349(13) . ?
C12 C17 1.385(11) . ?
C12 C13 1.404(11) . ?
C10 C9 1.392(12) . ?
C19 C20 1.395(12) . ?
C19 C24 1.384(11) . ?
C19 C18 1.503(11) . ?
C3 C2 1.372(13) . ?
C13 C14 1.398(11) . ?
C14 C15 1.355(14) . ?
C20 C21 1.383(12) . ?
C8 C9 1.372(13) . ?
C1 C2 1.381(11) . ?
C15 C16 1.384(14) . ?
C17 C16 1.384(11) . ?
C23 C24 1.388(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 178.7(2) . . ?
O1 U1 O4 88.2(2) . . ?
O2 U1 O4 90.6(2) . . ?
O1 U1 O6 95.3(2) . . ?
O2 U1 O6 85.1(2) . . ?
O4 U1 O6 119.80(18) . . ?
O1 U1 O5 90.8(2) . . ?
O2 U1 O5 88.5(2) . . ?
O4 U1 O5 67.53(18) . . ?
O6 U1 O5 52.38(18) . . ?
O1 U1 O3 84.8(2) . . ?
O2 U1 O3 94.6(2) . . ?
O4 U1 O3 52.90(18) . . ?
O6 U1 O3 172.71(18) . . ?
O5 U1 O3 120.34(18) . . ?
O1 U1 N2 103.1(2) . . ?
O2 U1 N2 77.7(2) . . ?
O4 U1 N2 119.49(19) . . ?
O6 U1 N2 117.96(19) . . ?
O5 U1 N2 164.2(2) . . ?
O3 U1 N2 68.99(19) . . ?
O1 U1 N1 76.2(2) . . ?
O2 U1 N1 105.0(2) . . ?
O4 U1 N1 163.4(2) . . ?
O6 U1 N1 68.13(19) . . ?
O5 U1 N1 117.54(19) . . ?
O3 U1 N1 118.84(19) . . ?
N2 U1 N1 60.3(2) . . ?
O1 U1 C11 85.6(2) . . ?
O2 U1 C11 93.4(2) . . ?
O4 U1 C11 26.2(2) . . ?
O6 U1 C11 146.0(2) . . ?
O5 U1 C11 93.6(2) . . ?
O3 U1 C11 26.8(2) . . ?
N2 U1 C11 94.7(2) . . ?
N1 U1 C11 143.6(2) . . ?
O1 U1 C18 92.8(2) . . ?
O2 U1 C18 87.1(2) . . ?
O4 U1 C18 93.5(2) . . ?
O6 U1 C18 26.4(2) . . ?
O5 U1 C18 26.0(2) . . ?
O3 U1 C18 146.3(2) . . ?
N2 U1 C18 143.3(2) . . ?
N1 U1 C18 92.9(2) . . ?
C11 U1 C18 119.6(2) . . ?
C11 O4 U1 95.2(5) . . ?
C11 O3 U1 92.3(5) . . ?
C5 N1 C1 117.4(7) . . ?
C5 N1 U1 124.2(5) . . ?
C1 N1 U1 118.0(5) . . ?
C6 N2 C10 117.7(7) . . ?
C6 N2 U1 124.2(5) . . ?
C10 N2 U1 117.7(5) . . ?
C18 O6 U1 94.0(5) . . ?
C18 O5 U1 94.2(5) . . ?
C8 C7 C6 121.4(8) . . ?
O4 C11 O3 119.6(7) . . ?
O4 C11 C12 118.9(7) . . ?
O3 C11 C12 121.5(7) . . ?
O4 C11 U1 58.7(4) . . ?
O3 C11 U1 60.9(4) . . ?
C12 C11 U1 176.5(6) . . ?
C21 C22 C23 120.8(9) . . ?
N1 C5 C4 121.5(8) . . ?
N1 C5 C6 115.2(6) . . ?
C4 C5 C6 123.3(7) . . ?
C3 C4 C5 120.2(8) . . ?
C17 C12 C13 120.0(7) . . ?
C17 C12 C11 114.2(7) . . ?
C13 C12 C11 125.7(8) . . ?
N2 C10 C9 122.9(8) . . ?
C20 C19 C24 118.8(7) . . ?
C20 C19 C18 125.3(7) . . ?
C24 C19 C18 115.9(7) . . ?
N2 C6 C7 121.3(7) . . ?
N2 C6 C5 115.8(6) . . ?
C7 C6 C5 122.9(7) . . ?
C4 C3 C2 119.4(8) . . ?
C14 C13 C12 117.5(8) . . ?
C14 C13 I1 116.2(7) . . ?
C12 C13 I1 126.3(6) . . ?
C15 C14 C13 122.7(9) . . ?
C21 C20 C19 119.8(9) . . ?
C21 C20 I3 115.2(7) . . ?
C19 C20 I3 125.0(6) . . ?
C22 C21 C20 120.6(10) . . ?
C7 C8 C9 117.6(8) . . ?
N1 C1 C2 123.0(9) . . ?
C3 C2 C1 118.5(9) . . ?
C8 C9 C10 119.1(9) . . ?
C14 C15 C16 119.2(8) . . ?
C12 C17 C16 120.3(8) . . ?
C22 C23 C24 119.3(10) . . ?
C22 C23 I4 121.1(8) . . ?
C24 C23 I4 119.6(9) . . ?
C17 C16 C15 120.3(9) . . ?
C17 C16 I2 119.7(7) . . ?
C15 C16 I2 120.0(7) . . ?
C19 C24 C23 120.7(9) . . ?
O5 C18 O6 119.3(7) . . ?
O5 C18 C19 121.1(7) . . ?
O6 C18 C19 119.6(7) . . ?
O5 C18 U1 59.8(4) . . ?
O6 C18 U1 59.5(4) . . ?
C19 C18 U1 177.1(6) . . ?

_refine_diff_density_max         3.190
_refine_diff_density_min         -2.601
_refine_diff_density_rms         0.163

_shelxl_version_number           2014-1


_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_2
_database_code_depnum_ccdc_archive 'CCDC 1501012'
_audit_update_record             
;
2016-08-25 deposited with the CCDC.
2016-10-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H24 I4 N4 O10 U2'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1680.27

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'
I I -0.4742 1.8119 '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                   9.2236(8)
_cell_length_b                   28.080(3)
_cell_length_c                   8.6636(8)
_cell_angle_alpha                90
_cell_angle_beta                 104.853(11)
_cell_angle_gamma                90
_cell_volume                     2168.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    26477
_cell_measurement_theta_min      4.569
_cell_measurement_theta_max      49.476
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.573
_exptl_crystal_F_000             1512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    10.362
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5322
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2015)'

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26125
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.450
_diffrn_reflns_theta_max         26.989
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4721
_reflns_number_gt                3597
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'

_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)+(0.0349P)²+5.9938P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4721
_refine_ls_number_parameters     266
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.0839
_refine_ls_wR_factor_gt          0.0755
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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 0.88857(3) 0.04070(2) 0.33551(3) 0.03429(9) Uani 1 1 d . . . . .
I1 I 1.52600(5) 0.14855(2) 0.40170(7) 0.05126(15) Uani 1 1 d . . . . .
I2 I 0.89701(9) 0.28664(3) 0.07198(10) 0.0978(3) Uani 1 1 d . . . . .
O2 O 0.9382(5) 0.00668(19) 0.1851(6) 0.0491(13) Uani 1 1 d . . . . .
O1 O 0.8278(5) 0.07722(18) 0.4712(6) 0.0448(12) Uani 1 1 d . . . . .
O5 O 0.8808(5) -0.02690(18) 0.4803(6) 0.0448(13) Uani 1 1 d D . . . .
C19 C 1.0661(9) 0.2006(3) 0.2280(9) 0.0483(19) Uani 1 1 d . . . . .
H19 H 0.9693 0.1902 0.2224 0.058 Uiso 1 1 calc R U . . .
C5 C 0.2573(9) 0.0735(3) -0.0032(11) 0.059(2) Uani 1 1 d . . . . .
H5 H 0.1537 0.0711 -0.0218 0.071 Uiso 1 1 calc R U . . .
N2 N 0.7236(6) 0.0862(2) 0.0942(7) 0.0421(14) Uani 1 1 d . . . . .
C8 C 0.5396(11) 0.1427(4) -0.1389(11) 0.075(3) Uani 1 1 d . . . . .
H8 H 0.4794 0.1617 -0.2178 0.090 Uiso 1 1 calc R U . . .
O4 O 1.2290(6) 0.11675(19) 0.5124(7) 0.0586(15) Uani 1 1 d . . . . .
O3 O 1.0447(5) 0.10271(19) 0.2938(6) 0.0497(13) Uani 1 1 d . . . . .
C11 C 0.5697(7) 0.0821(3) 0.0587(8) 0.0390(17) Uani 1 1 d . . . . .
N1 N 0.6040(6) 0.0170(2) 0.2460(7) 0.0381(14) Uani 1 1 d . . . . .
C12 C 0.5084(7) 0.0462(2) 0.1399(8) 0.0353(16) Uani 1 1 d . . . . .
C1 C 0.5437(8) -0.0162(3) 0.3188(9) 0.0439(18) Uani 1 1 d . . . . .
H1 H 0.6077 -0.0361 0.3911 0.053 Uiso 1 1 calc R U . . .
C6 C 0.3153(10) 0.1065(3) -0.0818(11) 0.062(2) Uani 1 1 d . . . . .
H6 H 0.2519 0.1266 -0.1538 0.074 Uiso 1 1 calc R U . . .
C14 C 1.1880(8) 0.1723(2) 0.2984(8) 0.0367(16) Uani 1 1 d . . . . .
C4 C 0.3511(8) 0.0419(3) 0.1086(9) 0.0449(19) Uani 1 1 d . . . . .
C3 C 0.2939(7) 0.0057(3) 0.1898(10) 0.053(2) Uani 1 1 d . . . . .
H3 H 0.1908 0.0017 0.1721 0.063 Uiso 1 1 calc R U . . .
C9 C 0.6925(11) 0.1463(3) -0.1054(12) 0.070(3) Uani 1 1 d . . . . .
H9 H 0.7370 0.1680 -0.1601 0.085 Uiso 1 1 calc R U . . .
C18 C 1.0892(10) 0.2447(3) 0.1660(10) 0.056(2) Uani 1 1 d . . . . .
C2 C 0.3885(8) -0.0228(3) 0.2926(10) 0.054(2) Uani 1 1 d . . . . .
H2 H 0.3516 -0.0468 0.3461 0.064 Uiso 1 1 calc R U . . .
C17 C 1.2289(10) 0.2599(3) 0.1657(11) 0.062(2) Uani 1 1 d . . . . .
H17 H 1.2423 0.2891 0.1210 0.074 Uiso 1 1 calc R U . . .
C10 C 0.7797(10) 0.1173(3) 0.0101(10) 0.060(2) Uani 1 1 d . . . . .
H10 H 0.8834 0.1197 0.0300 0.072 Uiso 1 1 calc R U . . .
C7 C 0.4753(9) 0.1108(3) -0.0553(9) 0.051(2) Uani 1 1 d . . . . .
C16 C 1.3498(9) 0.2316(3) 0.2318(10) 0.053(2) Uani 1 1 d . . . . .
H16 H 1.4455 0.2415 0.2298 0.064 Uiso 1 1 calc R U . . .
C13 C 1.1551(7) 0.1269(3) 0.3783(9) 0.0404(17) Uani 1 1 d . . . . .
C15 C 1.3316(8) 0.1882(2) 0.3018(9) 0.0397(17) Uani 1 1 d . . . . .
H50 H 0.815(15) -0.055(4) 0.46(2) 0.20(7) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.756(5) . ?
U1 O2 1.768(5) . ?
U1 O5 2.286(5) . ?
U1 O5 2.341(5) 3_756 ?
U1 O3 2.346(5) . ?
U1 N2 2.587(6) . ?
U1 N1 2.625(5) . ?
U1 U1 3.8168(6) 3_756 ?
I1 C15 2.100(7) . ?
I2 C18 2.111(8) . ?
O5 U1 2.341(5) 3_756 ?
C19 C14 1.384(10) . ?
C19 C18 1.386(11) . ?
C5 C6 1.340(12) . ?
C5 C4 1.430(11) . ?
N2 C10 1.324(10) . ?
N2 C11 1.378(8) . ?
C8 C9 1.368(13) . ?
C8 C7 1.378(13) . ?
O4 C13 1.220(8) . ?
O3 C13 1.285(8) . ?
C11 C7 1.394(10) . ?
C11 C12 1.427(10) . ?
N1 C1 1.324(9) . ?
N1 C12 1.371(9) . ?
C12 C4 1.411(9) . ?
C1 C2 1.403(9) . ?
C6 C7 1.440(11) . ?
C14 C15 1.390(10) . ?
C14 C13 1.520(10) . ?
C4 C3 1.412(11) . ?
C3 C2 1.341(12) . ?
C9 C10 1.377(11) . ?
C18 C17 1.358(12) . ?
C17 C16 1.369(11) . ?
C16 C15 1.389(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 174.9(2) . . ?
O1 U1 O5 93.3(2) . . ?
O2 U1 O5 90.4(2) . . ?
O1 U1 O5 91.8(2) . 3_756 ?
O2 U1 O5 92.9(2) . 3_756 ?
O5 U1 O5 68.87(19) . 3_756 ?
O1 U1 O3 89.1(2) . . ?
O2 U1 O3 90.1(2) . . ?
O5 U1 O3 143.86(16) . . ?
O5 U1 O3 75.02(17) 3_756 . ?
O1 U1 N2 91.7(2) . . ?
O2 U1 N2 83.2(2) . . ?
O5 U1 N2 139.40(17) . . ?
O5 U1 N2 151.18(18) 3_756 . ?
O3 U1 N2 76.44(18) . . ?
O1 U1 N1 83.1(2) . . ?
O2 U1 N1 94.2(2) . . ?
O5 U1 N1 77.41(17) . . ?
O5 U1 N1 145.54(18) 3_756 . ?
O3 U1 N1 138.54(18) . . ?
N2 U1 N1 63.26(18) . . ?
O1 U1 U1 93.05(16) . 3_756 ?
O2 U1 U1 92.02(18) . 3_756 ?
O5 U1 U1 34.91(11) . 3_756 ?
O5 U1 U1 33.97(12) 3_756 3_756 ?
O3 U1 U1 108.98(12) . 3_756 ?
N2 U1 U1 172.85(14) . 3_756 ?
N1 U1 U1 112.04(13) . 3_756 ?
U1 O5 U1 111.13(19) . 3_756 ?
C14 C19 C18 119.7(7) . . ?
C6 C5 C4 121.5(7) . . ?
C10 N2 C11 117.2(6) . . ?
C10 N2 U1 122.6(5) . . ?
C11 N2 U1 119.8(5) . . ?
C9 C8 C7 119.6(8) . . ?
C13 O3 U1 137.0(5) . . ?
N2 C11 C7 122.0(7) . . ?
N2 C11 C12 117.7(6) . . ?
C7 C11 C12 120.2(6) . . ?
C1 N1 C12 117.6(6) . . ?
C1 N1 U1 123.2(5) . . ?
C12 N1 U1 118.0(4) . . ?
N1 C12 C4 122.0(7) . . ?
N1 C12 C11 119.0(6) . . ?
C4 C12 C11 119.0(6) . . ?
N1 C1 C2 123.5(7) . . ?
C5 C6 C7 120.3(8) . . ?
C19 C14 C15 119.1(7) . . ?
C19 C14 C13 116.7(6) . . ?
C15 C14 C13 124.1(6) . . ?
C12 C4 C3 117.6(7) . . ?
C12 C4 C5 119.3(8) . . ?
C3 C4 C5 123.0(7) . . ?
C2 C3 C4 119.8(6) . . ?
C8 C9 C10 119.3(8) . . ?
C17 C18 C19 121.4(7) . . ?
C17 C18 I2 121.8(6) . . ?
C19 C18 I2 116.8(6) . . ?
C3 C2 C1 119.4(8) . . ?
C18 C17 C16 119.2(8) . . ?
N2 C10 C9 123.5(8) . . ?
C8 C7 C11 118.3(8) . . ?
C8 C7 C6 122.2(8) . . ?
C11 C7 C6 119.5(8) . . ?
C17 C16 C15 120.9(8) . . ?
O4 C13 O3 126.0(7) . . ?
O4 C13 C14 120.1(6) . . ?
O3 C13 C14 113.9(6) . . ?
C16 C15 C14 119.6(7) . . ?
C16 C15 I1 117.3(5) . . ?
C14 C15 I1 123.1(5) . . ?

_refine_diff_density_max         2.358
_refine_diff_density_min         -2.215
_refine_diff_density_rms         0.160

_shelxl_version_number           2014-1


_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_3
_database_code_depnum_ccdc_archive 'CCDC 1501013'
_audit_update_record             
;
2016-08-25 deposited with the CCDC.
2016-10-08 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H14 I4 N2 O6 U'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Rod
_exptl_crystal_colour            Yellow

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1196.02

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   19.2039(10)
_cell_length_b                   10.5773(5)
_cell_length_c                   28.8136(14)
_cell_angle_alpha                90
_cell_angle_beta                 96.772(7)
_cell_angle_gamma                90
_cell_volume                     5811.9(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    57468
_cell_measurement_theta_min      4.404
_cell_measurement_theta_max      52.787
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.734
_exptl_crystal_F_000             4288
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    9.878
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6140
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2015)'

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            55772
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.211
_diffrn_reflns_theta_max         27.445
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13238
_reflns_number_gt                9598
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'

_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)+(0.0244P)²+7.8368P] 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         13238
_refine_ls_number_parameters     703
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.0709
_refine_ls_wR_factor_gt          0.0628
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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 0.28136(2) 0.60207(2) 0.03222(2) 0.03292(6) Uani 1 1 d . . . . .
U1 U 0.52918(2) 0.52259(2) 0.28047(2) 0.03465(6) Uani 1 1 d . . . . .
I1 I 0.51684(3) 0.35337(4) 0.09715(2) 0.05909(13) Uani 1 1 d . . . . .
I6 I 0.11686(3) -0.06350(4) 0.06891(2) 0.06218(14) Uani 1 1 d . . . . .
I8 I 0.27910(3) 0.12371(4) -0.17497(2) 0.06775(15) Uani 1 1 d . . . . .
I2 I 0.54574(3) 1.00363(4) 0.07308(2) 0.06126(14) Uani 1 1 d . . . . .
I3 I 0.53074(3) 0.74034(5) 0.45845(2) 0.07409(17) Uani 1 1 d . . . . .
I5 I 0.29718(3) 0.39208(4) 0.20796(2) 0.07075(17) Uani 1 1 d . . . . .
I4 I 0.36133(3) 1.17983(4) 0.30597(2) 0.05900(13) Uani 1 1 d . . . . .
I7 I 0.27863(4) 0.77490(5) -0.14986(2) 0.07938(18) Uani 1 1 d . . . . .
O5 O 0.5020(2) 0.6216(4) 0.35523(13) 0.0453(11) Uani 1 1 d . . . . .
C37 C 0.3183(3) 0.9283(6) 0.0537(2) 0.0439(16) Uani 1 1 d . . . . .
C40 C 0.2169(3) 0.2911(5) 0.11580(18) 0.0322(13) Uani 1 1 d . . . . .
C39 C 0.2390(3) 0.4001(5) 0.0887(2) 0.0348(13) Uani 1 1 d . . . . .
O9 O 0.2557(2) 0.5052(4) 0.10717(13) 0.0408(10) Uani 1 1 d . . . . .
O8 O 0.1927(2) 0.6473(4) 0.02358(14) 0.0460(11) Uani 1 1 d . . . . .
O3 O 0.5398(2) 0.4759(4) 0.19726(14) 0.0502(12) Uani 1 1 d . . . . .
C14 C 0.5319(3) 0.6286(5) 0.13392(19) 0.0352(13) Uani 1 1 d . . . . .
N2 N 0.5659(3) 0.3740(5) 0.35480(18) 0.0475(14) Uani 1 1 d . . . . .
O6 O 0.4964(3) 0.7413(4) 0.29441(14) 0.0570(13) Uani 1 1 d . . . . .
C4 C 0.5799(3) 0.0673(6) 0.2968(3) 0.0494(17) Uani 1 1 d . . . . .
O12 O 0.2645(3) 0.4606(4) -0.03552(14) 0.0547(13) Uani 1 1 d . . . . .
O10 O 0.2417(3) 0.3859(4) 0.04565(14) 0.0537(12) Uani 1 1 d . . . . .
O2 O 0.4399(2) 0.4853(4) 0.27112(14) 0.0484(11) Uani 1 1 d . . . . .
C26 C 0.4294(3) 0.9313(5) 0.33328(19) 0.0362(14) Uani 1 1 d . . . . .
H26 H 0.4227 0.9189 0.3011 0.043 Uiso 1 1 calc R U . . .
C51 C 0.2846(3) 0.3190(5) -0.1650(2) 0.0377(14) Uani 1 1 d . . . . .
C28 C 0.3681(4) 0.7753(9) 0.1857(3) 0.072(2) Uani 1 1 d . . . . .
H28 H 0.3786 0.7380 0.2149 0.087 Uiso 1 1 calc R U . . .
O1 O 0.6191(2) 0.5578(4) 0.28990(14) 0.0514(12) Uani 1 1 d . . . . .
N3 N 0.3263(3) 0.7498(5) 0.10466(18) 0.0460(13) Uani 1 1 d . . . . .
O11 O 0.3009(2) 0.6487(4) -0.04973(14) 0.0480(11) Uani 1 1 d . . . . .
O7 O 0.3695(2) 0.5571(4) 0.04079(15) 0.0527(12) Uani 1 1 d . . . . .
N1 N 0.5470(3) 0.2768(5) 0.26702(19) 0.0519(14) Uani 1 1 d . . . . .
N4 N 0.2942(3) 0.8489(5) 0.01813(18) 0.0473(13) Uani 1 1 d . . . . .
O4 O 0.5221(3) 0.6713(4) 0.21399(14) 0.0600(13) Uani 1 1 d . . . . .
C21 C 0.4632(3) 0.8384(5) 0.36212(19) 0.0318(13) Uani 1 1 d . . . . .
C45 C 0.1819(3) 0.1945(5) 0.08995(19) 0.0359(14) Uani 1 1 d . . . . .
H45 H 0.1712 0.2046 0.0578 0.043 Uiso 1 1 calc R U . . .
C13 C 0.5305(3) 0.5870(6) 0.1842(2) 0.0391(14) Uani 1 1 d . . . . .
C5 C 0.6033(3) -0.0091(7) 0.3357(3) 0.0573(19) Uani 1 1 d . . . . .
H5 H 0.6111 -0.0948 0.3312 0.069 Uiso 1 1 calc R U . . .
C42 C 0.2105(3) 0.1620(6) 0.1848(2) 0.0469(16) Uani 1 1 d . . . . .
H42 H 0.2197 0.1518 0.2170 0.056 Uiso 1 1 calc R U . . .
C18 C 0.5414(3) 0.8073(6) 0.0831(2) 0.0433(15) Uani 1 1 d . . . . .
C29 C 0.3766(4) 0.9033(8) 0.1799(3) 0.068(2) Uani 1 1 d . . . . .
H29 H 0.3930 0.9537 0.2054 0.082 Uiso 1 1 calc R U . . .
C19 C 0.5350(3) 0.7578(6) 0.1264(2) 0.0421(15) Uani 1 1 d . . . . .
H19 H 0.5328 0.8125 0.1515 0.051 Uiso 1 1 calc R U . . .
C11 C 0.5793(3) 0.2482(6) 0.3486(2) 0.0414(15) Uani 1 1 d . . . . .
C52 C 0.2844(3) 0.3685(5) -0.1210(2) 0.0365(14) Uani 1 1 d . . . . .
H52 H 0.2833 0.3141 -0.0957 0.044 Uiso 1 1 calc R U . . .
C27 C 0.3432(4) 0.7024(8) 0.1468(2) 0.065(2) Uani 1 1 d . . . . .
H27 H 0.3383 0.6158 0.1509 0.078 Uiso 1 1 calc R U . . .
C17 C 0.5457(3) 0.7274(6) 0.0457(2) 0.0466(16) Uani 1 1 d . . . . .
H17 H 0.5515 0.7602 0.0165 0.056 Uiso 1 1 calc R U . . .
C32 C 0.3512(4) 1.1358(7) 0.0849(4) 0.070(2) Uani 1 1 d . . . . .
H32 H 0.3573 1.2218 0.0802 0.084 Uiso 1 1 calc R U . . .
C46 C 0.2836(3) 0.5404(6) -0.06383(19) 0.0359(13) Uani 1 1 d . . . . .
C44 C 0.1627(3) 0.0847(6) 0.1104(2) 0.0380(14) Uani 1 1 d . . . . .
C15 C 0.5330(3) 0.5483(6) 0.0956(2) 0.0388(14) Uani 1 1 d . . . . .
C38 C 0.3357(3) 0.8768(6) 0.0988(2) 0.0435(16) Uani 1 1 d . . . . .
C1 C 0.5344(4) 0.2247(7) 0.2247(3) 0.069(2) Uani 1 1 d . . . . .
H1 H 0.5190 0.2768 0.1996 0.083 Uiso 1 1 calc R U . . .
C23 C 0.4465(3) 0.9689(6) 0.4285(2) 0.0457(16) Uani 1 1 d . . . . .
H23 H 0.4508 0.9806 0.4607 0.055 Uiso 1 1 calc R U . . .
C48 C 0.2871(3) 0.5773(5) -0.1519(2) 0.0378(14) Uani 1 1 d . . . . .
C30 C 0.3608(3) 0.9568(7) 0.1359(3) 0.0544(19) Uani 1 1 d . . . . .
C36 C 0.2716(4) 0.8993(6) -0.0231(2) 0.060(2) Uani 1 1 d . . . . .
H36 H 0.2545 0.8452 -0.0472 0.073 Uiso 1 1 calc R U . . .
C6 C 0.6144(3) 0.0393(7) 0.3786(3) 0.060(2) Uani 1 1 d . . . . .
H6 H 0.6300 -0.0132 0.4036 0.072 Uiso 1 1 calc R U . . .
C47 C 0.2859(3) 0.4987(5) -0.11334(18) 0.0341(13) Uani 1 1 d . . . . .
C12 C 0.5686(3) 0.1971(6) 0.3027(2) 0.0422(15) Uani 1 1 d . . . . .
C43 C 0.1759(3) 0.0687(6) 0.1580(2) 0.0458(16) Uani 1 1 d . . . . .
H43 H 0.1616 -0.0047 0.1719 0.055 Uiso 1 1 calc R U . . .
C20 C 0.4889(3) 0.7274(6) 0.3366(2) 0.0386(14) Uani 1 1 d . . . . .
C10 C 0.5782(4) 0.4209(8) 0.3978(2) 0.067(2) Uani 1 1 d . . . . .
H10 H 0.5707 0.5068 0.4020 0.080 Uiso 1 1 calc R U . . .
C16 C 0.5414(3) 0.5990(6) 0.0520(2) 0.0450(16) Uani 1 1 d . . . . .
H16 H 0.5442 0.5452 0.0268 0.054 Uiso 1 1 calc R U . . .
C8 C 0.6143(4) 0.2235(8) 0.4319(3) 0.066(2) Uani 1 1 d . . . . .
H8 H 0.6303 0.1736 0.4575 0.079 Uiso 1 1 calc R U . . .
C34 C 0.2998(4) 1.1078(7) 0.0023(3) 0.067(2) Uani 1 1 d . . . . .
H34 H 0.3031 1.1939 -0.0036 0.080 Uiso 1 1 calc R U . . .
C7 C 0.6027(3) 0.1708(7) 0.3872(3) 0.0529(18) Uani 1 1 d . . . . .
C49 C 0.2885(3) 0.5268(6) -0.1958(2) 0.0484(17) Uani 1 1 d . . . . .
H49 H 0.2901 0.5807 -0.2211 0.058 Uiso 1 1 calc R U . . .
C35 C 0.2720(4) 1.0289(7) -0.0321(3) 0.068(2) Uani 1 1 d . . . . .
H35 H 0.2535 1.0605 -0.0611 0.082 Uiso 1 1 calc R U . . .
C50 C 0.2876(3) 0.3976(6) -0.2030(2) 0.0478(16) Uani 1 1 d . . . . .
H50 H 0.2889 0.3643 -0.2327 0.057 Uiso 1 1 calc R U . . .
C25 C 0.4061(3) 1.0407(5) 0.3519(2) 0.0394(14) Uani 1 1 d . . . . .
C22 C 0.4731(3) 0.8592(6) 0.41013(19) 0.0374(14) Uani 1 1 d . . . . .
C33 C 0.3238(3) 1.0600(6) 0.0467(3) 0.0529(18) Uani 1 1 d . . . . .
C41 C 0.2317(3) 0.2714(6) 0.1639(2) 0.0387(14) Uani 1 1 d . . . . .
C24 C 0.4139(3) 1.0598(6) 0.3994(2) 0.0433(15) Uani 1 1 d . . . . .
H24 H 0.3974 1.1336 0.4118 0.052 Uiso 1 1 calc R U . . .
C3 C 0.5663(4) 0.0176(7) 0.2517(3) 0.066(2) Uani 1 1 d . . . . .
H3 H 0.5731 -0.0680 0.2463 0.079 Uiso 1 1 calc R U . . .
C9 C 0.6019(4) 0.3481(8) 0.4374(3) 0.075(2) Uani 1 1 d . . . . .
H9 H 0.6089 0.3850 0.4669 0.089 Uiso 1 1 calc R U . . .
C31 C 0.3685(4) 1.0889(8) 0.1268(3) 0.068(2) Uani 1 1 d . . . . .
H31 H 0.3860 1.1424 0.1511 0.082 Uiso 1 1 calc R U . . .
C2 C 0.5433(5) 0.0959(7) 0.2162(3) 0.081(3) Uani 1 1 d . . . . .
H2 H 0.5332 0.0641 0.1861 0.097 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
U2 O7 1.748(4) . ?
U2 O8 1.758(4) . ?
U2 O12 2.450(4) . ?
U2 O10 2.455(4) . ?
U2 O11 2.484(4) . ?
U2 O9 2.492(4) . ?
U2 N4 2.658(5) . ?
U2 N3 2.668(5) . ?
U2 C46 2.849(6) . ?
U2 C39 2.861(6) . ?
U1 O2 1.749(4) . ?
U1 O1 1.757(4) . ?
U1 O6 2.443(4) . ?
U1 O4 2.470(4) . ?
U1 O3 2.480(4) . ?
U1 O5 2.505(4) . ?
U1 N1 2.657(5) . ?
U1 N2 2.683(5) . ?
U1 C13 2.860(6) . ?
U1 C20 2.864(6) . ?
I1 C15 2.086(6) . ?
I6 C44 2.101(6) . ?
I8 C51 2.087(6) . ?
I2 C18 2.099(6) . ?
I3 C22 2.093(6) . ?
I5 C41 2.108(6) . ?
I4 C25 2.094(6) . ?
I7 C48 2.098(6) . ?
O5 C20 1.254(7) . ?
C37 N4 1.363(8) . ?
C37 C38 1.413(9) . ?
C37 C33 1.413(9) . ?
C40 C45 1.390(8) . ?
C40 C41 1.398(7) . ?
C40 C39 1.483(7) . ?
C39 O9 1.257(6) . ?
C39 O10 1.257(6) . ?
O3 C13 1.241(7) . ?
C14 C19 1.387(8) . ?
C14 C15 1.394(7) . ?
C14 C13 1.517(8) . ?
N2 C10 1.331(8) . ?
N2 C11 1.371(7) . ?
O6 C20 1.249(7) . ?
C4 C3 1.397(10) . ?
C4 C12 1.404(8) . ?
C4 C5 1.410(9) . ?
O12 C46 1.258(7) . ?
C26 C25 1.372(8) . ?
C26 C21 1.396(8) . ?
C26 H26 0.9300 . ?
C51 C52 1.371(8) . ?
C51 C50 1.382(8) . ?
C28 C29 1.376(11) . ?
C28 C27 1.398(10) . ?
C28 H28 0.9300 . ?
N3 C27 1.319(8) . ?
N3 C38 1.369(8) . ?
O11 C46 1.247(7) . ?
N1 C1 1.332(8) . ?
N1 C12 1.356(8) . ?
N4 C36 1.327(8) . ?
O4 C13 1.262(7) . ?
C21 C22 1.391(7) . ?
C21 C20 1.499(8) . ?
C45 C44 1.373(8) . ?
C45 H45 0.9300 . ?
C5 C6 1.333(10) . ?
C5 H5 0.9300 . ?
C42 C41 1.387(8) . ?
C42 C43 1.376(9) . ?
C42 H42 0.9300 . ?
C18 C19 1.373(8) . ?
C18 C17 1.379(8) . ?
C29 C30 1.389(10) . ?
C29 H29 0.9300 . ?
C19 H19 0.9300 . ?
C11 C7 1.410(9) . ?
C11 C12 1.422(8) . ?
C52 C47 1.394(8) . ?
C52 H52 0.9300 . ?
C27 H27 0.9300 . ?
C17 C16 1.373(9) . ?
C17 H17 0.9300 . ?
C32 C31 1.312(11) . ?
C32 C33 1.412(10) . ?
C32 H32 0.9300 . ?
C46 C47 1.499(7) . ?
C44 C43 1.374(8) . ?
C15 C16 1.394(8) . ?
C38 C30 1.404(9) . ?
C1 C2 1.399(9) . ?
C1 H1 0.9300 . ?
C23 C24 1.376(8) . ?
C23 C22 1.397(8) . ?
C23 H23 0.9300 . ?
C48 C49 1.377(8) . ?
C48 C47 1.389(7) . ?
C30 C31 1.433(10) . ?
C36 C35 1.396(9) . ?
C36 H36 0.9300 . ?
C6 C7 1.435(10) . ?
C6 H6 0.9300 . ?
C43 H43 0.9300 . ?
C10 C9 1.406(10) . ?
C10 H10 0.9300 . ?
C16 H16 0.9300 . ?
C8 C9 1.351(11) . ?
C8 C7 1.398(10) . ?
C8 H8 0.9300 . ?
C34 C35 1.357(10) . ?
C34 C33 1.403(10) . ?
C34 H34 0.9300 . ?
C49 C50 1.382(9) . ?
C49 H49 0.9300 . ?
C35 H35 0.9300 . ?
C50 H50 0.9300 . ?
C25 C24 1.375(8) . ?
C24 H24 0.9300 . ?
C3 C2 1.350(11) . ?
C3 H3 0.9300 . ?
C9 H9 0.9300 . ?
C31 H31 0.9300 . ?
C2 H2 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
O7 U2 O8 180.0(2) . . ?
O7 U2 O12 88.93(19) . . ?
O8 U2 O12 91.06(18) . . ?
O7 U2 O10 92.15(19) . . ?
O8 U2 O10 87.86(18) . . ?
O12 U2 O10 62.78(13) . . ?
O7 U2 O11 86.33(18) . . ?
O8 U2 O11 93.65(17) . . ?
O12 U2 O11 52.01(13) . . ?
O10 U2 O11 114.79(13) . . ?
O7 U2 O9 93.03(17) . . ?
O8 U2 O9 86.99(16) . . ?
O12 U2 O9 114.72(13) . . ?
O10 U2 O9 51.94(13) . . ?
O11 U2 O9 166.71(13) . . ?
O7 U2 N4 100.56(19) . . ?
O8 U2 N4 79.44(18) . . ?
O12 U2 N4 118.95(15) . . ?
O10 U2 N4 167.14(16) . . ?
O11 U2 N4 68.45(14) . . ?
O9 U2 N4 124.59(14) . . ?
O7 U2 N3 80.24(19) . . ?
O8 U2 N3 99.77(18) . . ?
O12 U2 N3 168.82(16) . . ?
O10 U2 N3 120.00(14) . . ?
O11 U2 N3 123.80(15) . . ?
O9 U2 N3 69.00(14) . . ?
N4 U2 N3 61.11(16) . . ?
O7 U2 C46 87.10(18) . . ?
O8 U2 C46 92.88(18) . . ?
O12 U2 C46 26.11(14) . . ?
O10 U2 C46 88.88(15) . . ?
O11 U2 C46 25.91(14) . . ?
O9 U2 C46 140.81(15) . . ?
N4 U2 C46 93.69(16) . . ?
N3 U2 C46 148.60(16) . . ?
O7 U2 C39 92.99(19) . . ?
O8 U2 C39 87.03(17) . . ?
O12 U2 C39 88.72(15) . . ?
O10 U2 C39 25.94(14) . . ?
O11 U2 C39 140.72(15) . . ?
O9 U2 C39 26.00(13) . . ?
N4 U2 C39 149.07(16) . . ?
N3 U2 C39 94.57(16) . . ?
C46 U2 C39 114.82(17) . . ?
O2 U1 O1 179.2(2) . . ?
O2 U1 O6 88.38(18) . . ?
O1 U1 O6 92.4(2) . . ?
O2 U1 O4 93.48(19) . . ?
O1 U1 O4 87.04(19) . . ?
O6 U1 O4 62.15(13) . . ?
O2 U1 O3 89.83(17) . . ?
O1 U1 O3 90.01(17) . . ?
O6 U1 O3 113.57(13) . . ?
O4 U1 O3 51.71(13) . . ?
O2 U1 O5 85.83(17) . . ?
O1 U1 O5 94.53(17) . . ?
O6 U1 O5 51.60(13) . . ?
O4 U1 O5 113.74(13) . . ?
O3 U1 O5 164.58(14) . . ?
O2 U1 N1 84.13(19) . . ?
O1 U1 N1 95.1(2) . . ?
O6 U1 N1 172.19(17) . . ?
O4 U1 N1 120.42(15) . . ?
O3 U1 N1 68.73(15) . . ?
O5 U1 N1 125.32(15) . . ?
O2 U1 N2 98.71(18) . . ?
O1 U1 N2 80.76(18) . . ?
O6 U1 N2 118.17(14) . . ?
O4 U1 N2 167.80(17) . . ?
O3 U1 N2 127.68(15) . . ?
O5 U1 N2 67.68(14) . . ?
N1 U1 N2 61.11(16) . . ?
O2 U1 C13 91.43(18) . . ?
O1 U1 C13 88.77(18) . . ?
O6 U1 C13 88.04(16) . . ?
O4 U1 C13 26.09(15) . . ?
O3 U1 C13 25.63(14) . . ?
O5 U1 C13 139.57(16) . . ?
N1 U1 C13 94.33(17) . . ?
N2 U1 C13 151.93(17) . . ?
O2 U1 C20 86.12(18) . . ?
O1 U1 C20 94.52(19) . . ?
O6 U1 C20 25.69(14) . . ?
O4 U1 C20 87.84(16) . . ?
O3 U1 C20 139.04(16) . . ?
O5 U1 C20 25.92(14) . . ?
N1 U1 C20 150.54(17) . . ?
N2 U1 C20 93.18(16) . . ?
C13 U1 C20 113.66(18) . . ?
C20 O5 U1 93.3(3) . . ?
N4 C37 C38 118.5(6) . . ?
N4 C37 C33 121.6(6) . . ?
C38 C37 C33 119.8(6) . . ?
C45 C40 C41 116.8(5) . . ?
C45 C40 C39 116.1(5) . . ?
C41 C40 C39 126.9(5) . . ?
O9 C39 O10 119.0(5) . . ?
O9 C39 C40 122.7(5) . . ?
O10 C39 C40 118.3(5) . . ?
O9 C39 U2 60.3(3) . . ?
O10 C39 U2 58.7(3) . . ?
C40 C39 U2 177.0(4) . . ?
C39 O9 U2 93.7(3) . . ?
C13 O3 U1 94.6(3) . . ?
C19 C14 C15 118.2(5) . . ?
C19 C14 C13 116.1(5) . . ?
C15 C14 C13 125.7(5) . . ?
C10 N2 C11 117.9(6) . . ?
C10 N2 U1 121.8(5) . . ?
C11 N2 U1 120.0(4) . . ?
C20 O6 U1 96.3(4) . . ?
C3 C4 C12 117.7(7) . . ?
C3 C4 C5 122.0(7) . . ?
C12 C4 C5 120.3(7) . . ?
C46 O12 U2 94.9(3) . . ?
C39 O10 U2 95.4(3) . . ?
C25 C26 C21 120.7(5) . . ?
C25 C26 H26 119.6 . . ?
C21 C26 H26 119.6 . . ?
C52 C51 C50 120.5(6) . . ?
C52 C51 I8 120.0(4) . . ?
C50 C51 I8 119.5(4) . . ?
C29 C28 C27 118.7(7) . . ?
C29 C28 H28 120.7 . . ?
C27 C28 H28 120.7 . . ?
C27 N3 C38 117.7(6) . . ?
C27 N3 U2 121.3(5) . . ?
C38 N3 U2 120.9(4) . . ?
C46 O11 U2 93.6(3) . . ?
C1 N1 C12 116.2(6) . . ?
C1 N1 U1 121.7(5) . . ?
C12 N1 U1 122.1(4) . . ?
C36 N4 C37 118.2(6) . . ?
C36 N4 U2 120.3(4) . . ?
C37 N4 U2 121.3(4) . . ?
C13 O4 U1 94.5(4) . . ?
C22 C21 C26 118.7(5) . . ?
C22 C21 C20 126.7(5) . . ?
C26 C21 C20 114.6(5) . . ?
C44 C45 C40 121.9(5) . . ?
C44 C45 H45 119.0 . . ?
C40 C45 H45 119.0 . . ?
O3 C13 O4 119.2(5) . . ?
O3 C13 C14 123.1(5) . . ?
O4 C13 C14 117.6(6) . . ?
O3 C13 U1 59.8(3) . . ?
O4 C13 U1 59.4(3) . . ?
C14 C13 U1 176.9(4) . . ?
C6 C5 C4 121.2(7) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C41 C42 C43 120.0(6) . . ?
C41 C42 H42 120.0 . . ?
C43 C42 H42 120.0 . . ?
C19 C18 C17 119.7(6) . . ?
C19 C18 I2 120.8(5) . . ?
C17 C18 I2 119.5(4) . . ?
C30 C29 C28 119.6(7) . . ?
C30 C29 H29 120.2 . . ?
C28 C29 H29 120.2 . . ?
C18 C19 C14 121.9(6) . . ?
C18 C19 H19 119.1 . . ?
C14 C19 H19 119.1 . . ?
N2 C11 C7 120.5(6) . . ?
N2 C11 C12 118.8(6) . . ?
C7 C11 C12 120.7(6) . . ?
C51 C52 C47 121.4(5) . . ?
C51 C52 H52 119.3 . . ?
C47 C52 H52 119.3 . . ?
N3 C27 C28 123.6(8) . . ?
N3 C27 H27 118.2 . . ?
C28 C27 H27 118.2 . . ?
C16 C17 C18 119.6(6) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C31 C32 C33 122.3(8) . . ?
C31 C32 H32 118.9 . . ?
C33 C32 H32 118.9 . . ?
O11 C46 O12 119.4(5) . . ?
O11 C46 C47 122.9(5) . . ?
O12 C46 C47 117.6(5) . . ?
O11 C46 U2 60.5(3) . . ?
O12 C46 U2 59.0(3) . . ?
C47 C46 U2 176.0(4) . . ?
C45 C44 C43 120.4(6) . . ?
C45 C44 I6 120.2(4) . . ?
C43 C44 I6 119.4(4) . . ?
C14 C15 C16 119.6(6) . . ?
C14 C15 I1 124.7(4) . . ?
C16 C15 I1 115.7(4) . . ?
N3 C38 C37 118.1(6) . . ?
N3 C38 C30 122.4(6) . . ?
C37 C38 C30 119.5(6) . . ?
N1 C1 C2 123.4(7) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C24 C23 C22 120.7(6) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C49 C48 C47 120.4(6) . . ?
C49 C48 I7 114.9(4) . . ?
C47 C48 I7 124.4(4) . . ?
C29 C30 C38 118.0(7) . . ?
C29 C30 C31 123.3(7) . . ?
C38 C30 C31 118.8(7) . . ?
N4 C36 C35 123.6(7) . . ?
N4 C36 H36 118.2 . . ?
C35 C36 H36 118.2 . . ?
C5 C6 C7 121.3(7) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C48 C47 C52 117.8(5) . . ?
C48 C47 C46 126.1(5) . . ?
C52 C47 C46 116.0(5) . . ?
N1 C12 C4 123.7(6) . . ?
N1 C12 C11 117.8(6) . . ?
C4 C12 C11 118.5(6) . . ?
C44 C43 C42 119.5(6) . . ?
C44 C43 H43 120.2 . . ?
C42 C43 H43 120.2 . . ?
O6 C20 O5 118.7(6) . . ?
O6 C20 C21 117.9(5) . . ?
O5 C20 C21 123.4(5) . . ?
O6 C20 U1 58.0(3) . . ?
O5 C20 U1 60.8(3) . . ?
C21 C20 U1 174.7(4) . . ?
N2 C10 C9 123.8(7) . . ?
N2 C10 H10 118.1 . . ?
C9 C10 H10 118.1 . . ?
C17 C16 C15 121.0(6) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C9 C8 C7 119.0(7) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C35 C34 C33 120.3(7) . . ?
C35 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C8 C7 C11 119.8(7) . . ?
C8 C7 C6 122.2(7) . . ?
C11 C7 C6 118.0(7) . . ?
C48 C49 C50 121.3(6) . . ?
C48 C49 H49 119.3 . . ?
C50 C49 H49 119.3 . . ?
C34 C35 C36 118.5(7) . . ?
C34 C35 H35 120.7 . . ?
C36 C35 H35 120.7 . . ?
C51 C50 C49 118.5(6) . . ?
C51 C50 H50 120.7 . . ?
C49 C50 H50 120.7 . . ?
C26 C25 C24 120.7(6) . . ?
C26 C25 I4 118.3(4) . . ?
C24 C25 I4 121.0(4) . . ?
C21 C22 C23 119.6(5) . . ?
C21 C22 I3 124.5(4) . . ?
C23 C22 I3 115.8(4) . . ?
C34 C33 C32 124.0(7) . . ?
C34 C33 C37 117.6(7) . . ?
C32 C33 C37 118.4(7) . . ?
C42 C41 C40 121.2(6) . . ?
C42 C41 I5 115.4(4) . . ?
C40 C41 I5 123.0(4) . . ?
C25 C24 C23 119.5(6) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C2 C3 C4 118.9(7) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C8 C9 C10 119.0(8) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C32 C31 C30 121.1(8) . . ?
C32 C31 H31 119.4 . . ?
C30 C31 H31 119.4 . . ?
C3 C2 C1 120.0(8) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?

_refine_diff_density_max         1.683
_refine_diff_density_min         -2.089
_refine_diff_density_rms         0.141

_shelxl_version_number           2014-1


_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/n'
_symmetry_int_tables_number      14
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_4
_database_code_depnum_ccdc_archive 'CCDC 1501014'
_audit_update_record             
;
2016-08-25 deposited with the CCDC.
2016-10-08 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H17 I4 N3 O6 U'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1249.08

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'
I I -0.4742 1.8119 '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                   14.7607(9)
_cell_length_b                   16.8925(10)
_cell_length_c                   13.3636(8)
_cell_angle_alpha                90
_cell_angle_beta                 104.521(11)
_cell_angle_gamma                90
_cell_volume                     3225.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    30478
_cell_measurement_theta_min      4.399
_cell_measurement_theta_max      43.675
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.572
_exptl_crystal_F_000             2256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    8.906
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5856
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2015)'

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29830
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.425
_diffrn_reflns_theta_max         26.886
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6923
_reflns_number_gt                4780
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'

_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)+(0.0383P)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         6923
_refine_ls_number_parameters     388
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.0934
_refine_ls_wR_factor_gt          0.0803
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.34664(2) 0.07454(2) 0.16278(2) 0.02987(9) Uani 1 1 d . . . . .
I3 I 0.35900(5) -0.08173(4) 0.57286(5) 0.0618(2) Uani 1 1 d . . . . .
I4 I -0.03775(5) 0.13361(4) 0.33677(6) 0.0651(2) Uani 1 1 d . . . . .
I1 I 0.12341(4) 0.37846(4) 0.32925(5) 0.05727(19) Uani 1 1 d . . . . .
I2 I -0.13370(5) 0.13645(7) -0.05963(7) 0.1110(4) Uani 1 1 d . . . . .
O2 O 0.4113(4) 0.1034(3) 0.2867(4) 0.0415(13) Uani 1 1 d . . . . .
O1 O 0.2878(3) 0.0460(3) 0.0364(4) 0.0382(13) Uani 1 1 d . . . . .
O5 O 0.2686(4) -0.0159(3) 0.2359(4) 0.0416(13) Uani 1 1 d . . . . .
N1 N 0.3813(4) 0.2041(4) 0.0809(5) 0.0365(15) Uani 1 1 d . . . . .
O3 O 0.2216(4) 0.1517(3) 0.1680(4) 0.0432(14) Uani 1 1 d . . . . .
N3 N 0.4463(4) -0.0506(3) 0.1581(5) 0.0353(15) Uani 1 1 d . . . . .
O6 O 0.2874(5) -0.1238(3) 0.3319(4) 0.0560(17) Uani 1 1 d . . . . .
N2 N 0.5118(4) 0.0930(3) 0.1299(4) 0.0303(14) Uani 1 1 d . . . . .
C4 C 0.4902(7) 0.3064(5) 0.0703(7) 0.049(2) Uani 1 1 d . . . . .
H4 H 0.5518 0.3238 0.0828 0.059 Uiso 1 1 calc R U . . .
C17 C 0.0966(5) 0.2377(4) 0.1728(6) 0.0315(17) Uani 1 1 d . . . . .
C29 C 0.1321(5) 0.0301(4) 0.3419(6) 0.0379(19) Uani 1 1 d . . . . .
H29 H 0.1144 0.0373 0.2706 0.045 Uiso 1 1 calc R U . . .
C24 C 0.2101(5) -0.0149(4) 0.3852(6) 0.0352(18) Uani 1 1 d . . . . .
C10 C 0.5751(5) 0.0332(5) 0.1455(5) 0.0320(17) Uani 1 1 d . . . . .
C27 C 0.1050(6) 0.0558(5) 0.5088(7) 0.051(2) Uani 1 1 d . . . . .
H27 H 0.0703 0.0794 0.5499 0.061 Uiso 1 1 calc R U . . .
C3 C 0.4182(8) 0.3569(5) 0.0289(8) 0.058(3) Uani 1 1 d . . . . .
H3 H 0.4307 0.4090 0.0144 0.070 Uiso 1 1 calc R U . . .
C16 C 0.1975(6) 0.2129(5) 0.2122(7) 0.045(2) Uani 1 1 d . . . . .
C15 C 0.4074(6) -0.1215(5) 0.1587(6) 0.043(2) Uani 1 1 d . . . . .
H15 H 0.3448 -0.1241 0.1600 0.052 Uiso 1 1 calc R U . . .
C5 C 0.4709(5) 0.2286(4) 0.0937(5) 0.0338(18) Uani 1 1 d . . . . .
C22 C 0.0408(6) 0.1926(5) 0.0936(6) 0.042(2) Uani 1 1 d . . . . .
H22 H 0.0671 0.1504 0.0661 0.050 Uiso 1 1 calc R U . . .
C1 C 0.3117(6) 0.2536(5) 0.0381(6) 0.047(2) Uani 1 1 d . . . . .
H1 H 0.2504 0.2359 0.0276 0.057 Uiso 1 1 calc R U . . .
C14 C 0.4552(6) -0.1912(5) 0.1574(6) 0.046(2) Uani 1 1 d . . . . .
H14 H 0.4251 -0.2397 0.1565 0.055 Uiso 1 1 calc R U . . .
C9 C 0.6688(6) 0.0463(5) 0.1528(6) 0.043(2) Uani 1 1 d . . . . .
H9 H 0.7104 0.0039 0.1617 0.052 Uiso 1 1 calc R U . . .
C25 C 0.2361(6) -0.0243(5) 0.4927(6) 0.0401(19) Uani 1 1 d . . . . .
C18 C 0.0547(5) 0.3022(4) 0.2101(6) 0.0321(17) Uani 1 1 d . . . . .
O4 O 0.2505(5) 0.2505(5) 0.2779(7) 0.117(4) Uani 1 1 d . . . . .
C6 C 0.5437(6) 0.1672(5) 0.1226(6) 0.0381(19) Uani 1 1 d . . . . .
C20 C -0.0924(6) 0.2732(6) 0.0933(7) 0.055(3) Uani 1 1 d . . . . .
H20 H -0.1553 0.2852 0.0667 0.066 Uiso 1 1 calc R U . . .
C23 C 0.2608(5) -0.0564(5) 0.3146(6) 0.0362(19) Uani 1 1 d . . . . .
C11 C 0.5365(5) -0.0470(4) 0.1532(5) 0.0307(17) Uani 1 1 d . . . . .
C26 C 0.1840(6) 0.0106(5) 0.5526(7) 0.051(2) Uani 1 1 d . . . . .
H26 H 0.2018 0.0039 0.6239 0.061 Uiso 1 1 calc R U . . .
C28 C 0.0797(6) 0.0646(5) 0.4027(7) 0.046(2) Uani 1 1 d . . . . .
C12 C 0.5896(6) -0.1143(5) 0.1552(6) 0.044(2) Uani 1 1 d . . . . .
H12 H 0.6524 -0.1105 0.1550 0.053 Uiso 1 1 calc R U . . .
C2 C 0.3271(7) 0.3303(5) 0.0088(7) 0.061(3) Uani 1 1 d . . . . .
H2 H 0.2775 0.3627 -0.0235 0.074 Uiso 1 1 calc R U . . .
C19 C -0.0390(6) 0.3188(5) 0.1707(7) 0.047(2) Uani 1 1 d . . . . .
H19 H -0.0660 0.3612 0.1969 0.057 Uiso 1 1 calc R U . . .
C21 C -0.0540(6) 0.2101(6) 0.0550(6) 0.053(2) Uani 1 1 d . . . . .
C8 C 0.7003(6) 0.1225(6) 0.1470(7) 0.050(2) Uani 1 1 d . . . . .
H8 H 0.7634 0.1323 0.1529 0.060 Uiso 1 1 calc R U . . .
C13 C 0.5479(6) -0.1882(5) 0.1575(6) 0.044(2) Uani 1 1 d . . . . .
H13 H 0.5824 -0.2345 0.1591 0.052 Uiso 1 1 calc R U . . .
C7 C 0.6372(6) 0.1839(5) 0.1323(6) 0.047(2) Uani 1 1 d . . . . .
H7 H 0.6572 0.2358 0.1290 0.056 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.761(5) . ?
U1 O2 1.760(5) . ?
U1 O3 2.275(5) . ?
U1 O5 2.276(5) . ?
U1 N1 2.555(6) . ?
U1 N3 2.585(6) . ?
U1 N2 2.602(6) . ?
I3 C25 2.099(8) . ?
I4 C28 2.092(9) . ?
I1 C18 2.102(7) . ?
I2 C21 2.091(8) . ?
O5 C23 1.284(9) . ?
N1 C1 1.336(10) . ?
N1 C5 1.357(9) . ?
O3 C16 1.284(9) . ?
N3 C15 1.329(10) . ?
N3 C11 1.351(9) . ?
O6 C23 1.208(9) . ?
N2 C6 1.351(9) . ?
N2 C10 1.355(9) . ?
C4 C3 1.366(12) . ?
C4 C5 1.396(11) . ?
C17 C22 1.393(10) . ?
C17 C18 1.404(10) . ?
C17 C16 1.510(10) . ?
C29 C24 1.379(10) . ?
C29 C28 1.383(11) . ?
C24 C25 1.400(10) . ?
C24 C23 1.514(10) . ?
C10 C9 1.380(10) . ?
C10 C11 1.484(10) . ?
C27 C28 1.381(12) . ?
C27 C26 1.394(12) . ?
C3 C2 1.379(13) . ?
C16 O4 1.201(10) . ?
C15 C14 1.375(11) . ?
C5 C6 1.473(11) . ?
C22 C21 1.397(11) . ?
C1 C2 1.389(11) . ?
C14 C13 1.368(11) . ?
C9 C8 1.378(12) . ?
C25 C26 1.375(11) . ?
C18 C19 1.378(11) . ?
C6 C7 1.384(11) . ?
C20 C21 1.366(12) . ?
C20 C19 1.370(12) . ?
C11 C12 1.378(10) . ?
C12 C13 1.396(11) . ?
C8 C7 1.374(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 176.8(2) . . ?
O1 U1 O3 88.7(2) . . ?
O2 U1 O3 93.7(2) . . ?
O1 U1 O5 92.7(2) . . ?
O2 U1 O5 89.7(2) . . ?
O3 U1 O5 82.46(19) . . ?
O1 U1 N1 85.8(2) . . ?
O2 U1 N1 92.7(2) . . ?
O3 U1 N1 76.9(2) . . ?
O5 U1 N1 159.35(19) . . ?
O1 U1 N3 84.3(2) . . ?
O2 U1 N3 94.1(2) . . ?
O3 U1 N3 160.07(19) . . ?
O5 U1 N3 79.29(19) . . ?
N1 U1 N3 120.9(2) . . ?
O1 U1 N2 97.4(2) . . ?
O2 U1 N2 79.4(2) . . ?
O3 U1 N2 137.60(19) . . ?
O5 U1 N2 138.56(18) . . ?
N1 U1 N2 61.87(19) . . ?
N3 U1 N2 62.04(19) . . ?
C23 O5 U1 150.2(5) . . ?
C1 N1 C5 118.9(7) . . ?
C1 N1 U1 120.3(5) . . ?
C5 N1 U1 120.1(5) . . ?
C16 O3 U1 142.7(5) . . ?
C15 N3 C11 118.3(6) . . ?
C15 N3 U1 119.2(5) . . ?
C11 N3 U1 122.5(5) . . ?
C6 N2 C10 117.6(6) . . ?
C6 N2 U1 118.7(5) . . ?
C10 N2 U1 121.6(5) . . ?
C3 C4 C5 119.8(9) . . ?
C22 C17 C18 117.7(7) . . ?
C22 C17 C16 117.2(7) . . ?
C18 C17 C16 125.2(7) . . ?
C24 C29 C28 121.1(8) . . ?
C29 C24 C25 118.6(7) . . ?
C29 C24 C23 119.0(7) . . ?
C25 C24 C23 122.4(7) . . ?
N2 C10 C9 122.2(7) . . ?
N2 C10 C11 115.4(6) . . ?
C9 C10 C11 122.4(7) . . ?
C28 C27 C26 118.2(8) . . ?
C4 C3 C2 119.8(8) . . ?
O4 C16 O3 123.9(8) . . ?
O4 C16 C17 120.9(8) . . ?
O3 C16 C17 115.2(7) . . ?
N3 C15 C14 123.2(8) . . ?
N1 C5 C4 120.4(7) . . ?
N1 C5 C6 116.2(7) . . ?
C4 C5 C6 123.1(7) . . ?
C17 C22 C21 120.8(8) . . ?
N1 C1 C2 122.8(8) . . ?
C13 C14 C15 119.0(8) . . ?
C10 C9 C8 119.4(8) . . ?
C26 C25 C24 120.0(8) . . ?
C26 C25 I3 116.0(6) . . ?
C24 C25 I3 123.8(6) . . ?
C19 C18 C17 120.8(7) . . ?
C19 C18 I1 114.3(6) . . ?
C17 C18 I1 124.9(5) . . ?
N2 C6 C7 122.6(7) . . ?
N2 C6 C5 115.4(7) . . ?
C7 C6 C5 121.8(7) . . ?
C21 C20 C19 120.5(8) . . ?
O6 C23 O5 124.5(7) . . ?
O6 C23 C24 120.4(7) . . ?
O5 C23 C24 115.1(7) . . ?
N3 C11 C12 121.6(7) . . ?
N3 C11 C10 116.4(6) . . ?
C12 C11 C10 121.9(7) . . ?
C25 C26 C27 121.4(8) . . ?
C29 C28 C27 120.8(8) . . ?
C29 C28 I4 120.9(6) . . ?
C27 C28 I4 118.3(6) . . ?
C11 C12 C13 119.2(8) . . ?
C3 C2 C1 118.0(9) . . ?
C20 C19 C18 120.4(8) . . ?
C20 C21 C22 119.9(8) . . ?
C20 C21 I2 121.9(7) . . ?
C22 C21 I2 118.2(7) . . ?
C7 C8 C9 119.2(7) . . ?
C14 C13 C12 118.6(7) . . ?
C6 C7 C8 119.0(8) . . ?

_refine_diff_density_max         1.811
_refine_diff_density_min         -1.700
_refine_diff_density_rms         0.172

_shelxl_version_number           2014-1


_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_5
_database_code_depnum_ccdc_archive 'CCDC 1501015'
_audit_update_record             
;
2016-08-25 deposited with the CCDC.
2016-10-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H16 Cl I4 N3 O6 U'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1283.53

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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                   15.720(7)
_cell_length_b                   16.555(8)
_cell_length_c                   13.408(7)
_cell_angle_alpha                90
_cell_angle_beta                 106.011(6)
_cell_angle_gamma                90
_cell_volume                     3354(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    76001
_cell_measurement_theta_min      5.293
_cell_measurement_theta_max      49.919
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.542
_exptl_crystal_F_000             2320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    8.646
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5294
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   'TWINABS, Bruker-AXS (2008)'

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48616
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         1.825
_diffrn_reflns_theta_max         27.023
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.974
_reflns_number_total             7115
_reflns_number_gt                4767
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'

_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)+(0.0747P)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         7115
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0544
_refine_ls_wR_factor_ref         0.1436
_refine_ls_wR_factor_gt          0.1328
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.65937(2) -0.06969(2) 0.84929(3) 0.02841(12) Uani 1 1 d . . . . .
I1 I 0.86096(5) -0.38254(5) 0.68740(7) 0.0574(2) Uani 1 1 d . . . . .
I4 I 1.01019(6) -0.11885(7) 0.67361(9) 0.0775(3) Uani 1 1 d . . . . .
I3 I 0.62662(9) 0.08575(8) 0.41955(8) 0.1029(5) Uani 1 1 d . . . . .
I2 I 1.11664(6) -0.14288(10) 1.08513(9) 0.1040(5) Uani 1 1 d . . . . .
Cl1 Cl 0.2208(2) -0.1481(3) 0.8514(4) 0.0950(14) Uani 1 1 d . . . . .
O2 O 0.7171(4) -0.0358(4) 0.9740(5) 0.0367(16) Uani 1 1 d . . . . .
O1 O 0.5956(4) -0.1030(4) 0.7276(5) 0.0398(17) Uani 1 1 d . . . . .
O5 O 0.7249(4) 0.0217(4) 0.7680(6) 0.0375(16) Uani 1 1 d . . . . .
N3 N 0.6328(5) -0.2011(5) 0.9368(7) 0.040(2) Uani 1 1 d . . . . .
N2 N 0.5051(5) -0.0919(5) 0.8828(6) 0.0325(19) Uani 1 1 d . . . . .
C19 C 1.0196(7) -0.3243(7) 0.8496(10) 0.052(3) Uani 1 1 d . . . . .
H19 H 1.0440 -0.3682 0.8240 0.063 Uiso 1 1 calc R U . . .
O3 O 0.7790(4) -0.1462(5) 0.8449(6) 0.0466(19) Uani 1 1 d . . . . .
N1 N 0.5615(6) 0.0555(5) 0.8501(7) 0.035(2) Uani 1 1 d . . . . .
C20 C 1.0714(7) -0.2783(9) 0.9278(10) 0.057(3) Uani 1 1 d . . . . .
H20 H 1.1307 -0.2915 0.9555 0.068 Uiso 1 1 calc R U . . .
C21 C 1.0361(7) -0.2120(8) 0.9662(10) 0.056(3) Uani 1 1 d . . . . .
C4 C 0.4212(8) 0.1177(7) 0.8330(10) 0.053(3) Uani 1 1 d . . . . .
H4 H 0.3612 0.1124 0.8279 0.064 Uiso 1 1 calc R U . . .
C10 C 0.4792(7) -0.1676(6) 0.8933(8) 0.037(2) Uani 1 1 d . . . . .
C23 C 0.7159(7) 0.0585(7) 0.6820(9) 0.040(3) Uani 1 1 d . . . . .
C5 C 0.4755(6) 0.0493(6) 0.8487(8) 0.034(2) Uani 1 1 d . . . . .
C1 C 0.5949(8) 0.1286(6) 0.8449(9) 0.042(3) Uani 1 1 d . . . . .
H1 H 0.6548 0.1333 0.8495 0.050 Uiso 1 1 calc R U . . .
C27 C 0.8764(9) -0.0337(8) 0.4982(10) 0.063(4) Uani 1 1 d . . . . .
H27 H 0.9130 -0.0525 0.4594 0.075 Uiso 1 1 calc R U . . .
C9 C 0.3903(7) -0.1875(8) 0.8817(9) 0.049(3) Uani 1 1 d . . . . .
H9 H 0.3731 -0.2408 0.8866 0.059 Uiso 1 1 calc R U . . .
C17 C 0.8939(6) -0.2389(6) 0.8456(8) 0.036(2) Uani 1 1 d . . . . .
C25 C 0.7498(8) 0.0363(7) 0.5076(9) 0.048(3) Uani 1 1 d . . . . .
O6 O 0.6745(7) 0.1213(6) 0.6575(7) 0.084(3) Uani 1 1 d . . . . .
C11 C 0.5506(6) -0.2291(6) 0.9270(8) 0.033(2) Uani 1 1 d . . . . .
C7 C 0.3546(6) -0.0493(7) 0.8534(9) 0.043(3) Uani 1 1 d . . . . .
H7 H 0.3126 -0.0082 0.8420 0.052 Uiso 1 1 calc R U . . .
C16 C 0.7975(7) -0.2131(7) 0.8056(9) 0.043(3) Uani 1 1 d . . . . .
C18 C 0.9297(6) -0.3052(6) 0.8080(8) 0.036(2) Uani 1 1 d . . . . .
C2 C 0.5439(10) 0.1984(7) 0.8331(9) 0.057(3) Uani 1 1 d . . . . .
H2 H 0.5694 0.2488 0.8307 0.068 Uiso 1 1 calc R U . . .
C15 C 0.7006(7) -0.2528(7) 0.9794(8) 0.044(3) Uani 1 1 d . . . . .
H15 H 0.7584 -0.2353 0.9880 0.052 Uiso 1 1 calc R U . . .
C26 C 0.8031(9) 0.0069(8) 0.4498(10) 0.059(3) Uani 1 1 d . . . . .
H26 H 0.7884 0.0151 0.3785 0.071 Uiso 1 1 calc R U . . .
C6 C 0.4440(6) -0.0321(7) 0.8609(7) 0.033(2) Uani 1 1 d . . . . .
C24 C 0.7702(6) 0.0253(6) 0.6128(8) 0.034(2) Uani 1 1 d . . . . .
C12 C 0.5332(8) -0.3064(7) 0.9492(9) 0.048(3) Uani 1 1 d . . . . .
H12 H 0.4753 -0.3249 0.9355 0.057 Uiso 1 1 calc R U . . .
C28 C 0.8994(7) -0.0487(7) 0.6017(10) 0.047(3) Uani 1 1 d . . . . .
C3 C 0.4560(9) 0.1917(7) 0.8251(10) 0.055(3) Uani 1 1 d . . . . .
H3 H 0.4201 0.2373 0.8144 0.066 Uiso 1 1 calc R U . . .
O4 O 0.7429(6) -0.2551(7) 0.7455(9) 0.100(4) Uani 1 1 d . . . . .
C22 C 0.9471(7) -0.1940(7) 0.9255(8) 0.045(3) Uani 1 1 d . . . . .
H22 H 0.9228 -0.1508 0.9526 0.054 Uiso 1 1 calc R U . . .
C29 C 0.8458(6) -0.0195(6) 0.6603(8) 0.039(2) Uani 1 1 d . . . . .
H29 H 0.8603 -0.0296 0.7312 0.047 Uiso 1 1 calc R U . . .
C14 C 0.6870(9) -0.3283(7) 1.0097(10) 0.059(3) Uani 1 1 d . . . . .
H14 H 0.7350 -0.3606 1.0423 0.070 Uiso 1 1 calc R U . . .
C13 C 0.6040(9) -0.3570(8) 0.9927(11) 0.065(4) Uani 1 1 d . . . . .
H13 H 0.5944 -0.4100 1.0100 0.078 Uiso 1 1 calc R U . . .
C8 C 0.3310(7) -0.1272(8) 0.8631(9) 0.047(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.752(7) . ?
U1 O2 1.760(7) . ?
U1 O5 2.270(7) . ?
U1 O3 2.281(7) . ?
U1 N3 2.561(9) . ?
U1 N1 2.583(8) . ?
U1 N2 2.611(8) . ?
I1 C18 2.111(10) . ?
I4 C28 2.094(12) . ?
I3 C25 2.134(12) . ?
I2 C21 2.084(12) . ?
Cl1 C8 1.731(11) . ?
O5 C23 1.278(12) . ?
N3 C11 1.344(12) . ?
N3 C15 1.363(13) . ?
N2 C10 1.337(13) . ?
N2 C6 1.355(12) . ?
C19 C20 1.366(17) . ?
C19 C18 1.406(14) . ?
O3 C16 1.293(13) . ?
N1 C1 1.329(13) . ?
N1 C5 1.350(12) . ?
C20 C21 1.391(18) . ?
C21 C22 1.386(15) . ?
C4 C3 1.358(17) . ?
C4 C5 1.398(14) . ?
C10 C9 1.402(14) . ?
C10 C11 1.491(14) . ?
C23 O6 1.223(13) . ?
C23 C24 1.526(14) . ?
C5 C6 1.460(15) . ?
C1 C2 1.391(15) . ?
C27 C26 1.337(17) . ?
C27 C28 1.357(17) . ?
C9 C8 1.343(16) . ?
C17 C22 1.381(14) . ?
C17 C18 1.390(14) . ?
C17 C16 1.523(13) . ?
C25 C24 1.369(15) . ?
C25 C26 1.377(15) . ?
C11 C12 1.359(14) . ?
C7 C8 1.357(17) . ?
C7 C6 1.411(13) . ?
C16 O4 1.221(14) . ?
C2 C3 1.360(17) . ?
C15 C14 1.349(15) . ?
C24 C29 1.397(14) . ?
C12 C13 1.387(17) . ?
C28 C29 1.388(14) . ?
C14 C13 1.347(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 176.3(3) . . ?
O1 U1 O5 88.9(3) . . ?
O2 U1 O5 93.5(3) . . ?
O1 U1 O3 93.7(3) . . ?
O2 U1 O3 89.3(3) . . ?
O5 U1 O3 82.6(3) . . ?
O1 U1 N3 92.0(3) . . ?
O2 U1 N3 86.7(3) . . ?
O5 U1 N3 159.9(3) . . ?
O3 U1 N3 77.3(3) . . ?
O1 U1 N1 93.9(3) . . ?
O2 U1 N1 83.8(3) . . ?
O5 U1 N1 79.5(2) . . ?
O3 U1 N1 160.3(3) . . ?
N3 U1 N1 120.5(3) . . ?
O1 U1 N2 78.2(3) . . ?
O2 U1 N2 98.1(3) . . ?
O5 U1 N2 137.9(2) . . ?
O3 U1 N2 137.5(3) . . ?
N3 U1 N2 61.6(3) . . ?
N1 U1 N2 61.9(3) . . ?
C23 O5 U1 143.1(7) . . ?
C11 N3 C15 116.3(9) . . ?
C11 N3 U1 121.5(7) . . ?
C15 N3 U1 121.2(7) . . ?
C10 N2 C6 119.3(8) . . ?
C10 N2 U1 118.3(6) . . ?
C6 N2 U1 119.8(6) . . ?
C20 C19 C18 120.0(10) . . ?
C16 O3 U1 140.0(7) . . ?
C1 N1 C5 118.5(9) . . ?
C1 N1 U1 119.1(7) . . ?
C5 N1 U1 122.3(6) . . ?
C19 C20 C21 120.6(10) . . ?
C20 C21 C22 119.1(11) . . ?
C20 C21 I2 119.8(9) . . ?
C22 C21 I2 121.2(10) . . ?
C3 C4 C5 120.0(11) . . ?
N2 C10 C9 122.2(10) . . ?
N2 C10 C11 116.5(9) . . ?
C9 C10 C11 121.1(10) . . ?
O6 C23 O5 124.5(10) . . ?
O6 C23 C24 119.3(10) . . ?
O5 C23 C24 115.9(9) . . ?
N1 C5 C4 120.5(10) . . ?
N1 C5 C6 115.9(8) . . ?
C4 C5 C6 123.5(10) . . ?
N1 C1 C2 122.6(11) . . ?
C26 C27 C28 122.7(11) . . ?
C8 C9 C10 117.7(11) . . ?
C22 C17 C18 119.2(9) . . ?
C22 C17 C16 116.9(9) . . ?
C18 C17 C16 123.9(9) . . ?
C24 C25 C26 121.8(11) . . ?
C24 C25 I3 122.7(8) . . ?
C26 C25 I3 115.1(8) . . ?
N3 C11 C12 123.3(10) . . ?
N3 C11 C10 114.7(8) . . ?
C12 C11 C10 122.0(9) . . ?
C8 C7 C6 118.6(10) . . ?
O4 C16 O3 124.1(9) . . ?
O4 C16 C17 121.5(10) . . ?
O3 C16 C17 114.3(9) . . ?
C17 C18 C19 119.7(10) . . ?
C17 C18 I1 125.8(7) . . ?
C19 C18 I1 114.5(8) . . ?
C3 C2 C1 118.8(12) . . ?
C14 C15 N3 122.5(11) . . ?
C27 C26 C25 118.7(12) . . ?
N2 C6 C7 120.0(10) . . ?
N2 C6 C5 117.2(8) . . ?
C7 C6 C5 122.8(9) . . ?
C25 C24 C29 118.0(9) . . ?
C25 C24 C23 124.5(9) . . ?
C29 C24 C23 117.5(9) . . ?
C11 C12 C13 118.3(11) . . ?
C27 C28 C29 118.9(11) . . ?
C27 C28 I4 121.7(8) . . ?
C29 C28 I4 119.4(9) . . ?
C2 C3 C4 119.4(11) . . ?
C17 C22 C21 121.3(10) . . ?
C28 C29 C24 120.0(10) . . ?
C13 C14 C15 120.1(12) . . ?
C14 C13 C12 119.1(12) . . ?
C9 C8 C7 122.0(10) . . ?
C9 C8 Cl1 119.6(10) . . ?
C7 C8 Cl1 118.3(9) . . ?

_refine_diff_density_max         5.374
_refine_diff_density_min         -4.153
_refine_diff_density_rms         0.226

_shelxl_version_number           2014-1


_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration ?
####################################################################### 
# 
# 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_Complex_6
_database_code_depnum_ccdc_archive 'CCDC 1501016'
_audit_update_record             
;
2016-08-25 deposited with the CCDC.
2016-10-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H14 Br4 N2 O6 U'
_exptl_crystal_recrystallization_method Hydrothermal
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow

_diffrn_ambient_temperature      110(2)
_chemical_formula_weight         984.04

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'
Br Br -0.2901 2.4595 '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                   10.0684(18)
_cell_length_b                   11.644(2)
_cell_length_c                   12.261(2)
_cell_angle_alpha                91.165(3)
_cell_angle_beta                 113.983(2)
_cell_angle_gamma                90.210(3)
_cell_volume                     1312.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    12937
_cell_measurement_theta_min      4.428
_cell_measurement_theta_max      53.359
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.489
_exptl_crystal_F_000             904
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    12.311
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6221
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2015)'

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12936
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.749
_diffrn_reflns_theta_max         27.549
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             5958
_reflns_number_gt                4744
_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       'APEX, Bruker-AXS'
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_structure_solution    'SIR92 (Gualardi, 1994)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'WINGX (Farrugia, 2012)'
_computing_publication_material  'Crystal Maker (Palmer, 2009)'

_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)+(0.0289P)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         5958
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.0744
_refine_ls_wR_factor_gt          0.0689
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_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 0.38586(2) 0.16927(2) 0.66727(2) 0.01228(7) Uani 1 1 d . . . . .
Br1 Br 0.65972(7) -0.44922(6) 0.62513(6) 0.02348(16) Uani 1 1 d . . . . .
Br2 Br 1.09803(7) -0.18295(6) 0.98692(6) 0.02238(16) Uani 1 1 d . . . . .
Br4 Br 0.41530(8) 0.80845(6) 0.91326(6) 0.02817(17) Uani 1 1 d . . . . .
Br3 Br 0.95401(7) 0.59170(6) 1.13422(6) 0.02713(17) Uani 1 1 d . . . . .
O6 O 0.3778(4) 0.3783(4) 0.7056(4) 0.0185(10) Uani 1 1 d . . . . .
O2 O 0.3027(4) 0.1404(4) 0.7656(4) 0.0171(10) Uani 1 1 d . . . . .
O1 O 0.4709(4) 0.1973(4) 0.5698(4) 0.0173(10) Uani 1 1 d . . . . .
O4 O 0.6062(4) 0.0691(4) 0.7992(4) 0.0175(10) Uani 1 1 d . . . . .
O3 O 0.4323(4) -0.0379(4) 0.6691(4) 0.0177(10) Uani 1 1 d . . . . .
O5 O 0.5753(5) 0.2891(4) 0.8176(4) 0.0188(10) Uani 1 1 d . . . . .
N1 N 0.1179(5) 0.2489(5) 0.5435(5) 0.0179(12) Uani 1 1 d . . . . .
C18 C 0.5015(7) 0.3787(5) 0.7925(5) 0.0153(13) Uani 1 1 d . . . . .
N2 N 0.2061(5) 0.0549(4) 0.4722(4) 0.0142(11) Uani 1 1 d . . . . .
C7 C -0.0261(6) 0.0199(5) 0.3108(5) 0.0175(14) Uani 1 1 d . . . . .
H7 H -0.1227 0.0407 0.2711 0.021 Uiso 1 1 calc R U . . .
C6 C 0.0658(6) 0.0834(5) 0.4121(5) 0.0155(13) Uani 1 1 d . . . . .
C8 C 0.0258(7) -0.0730(6) 0.2699(6) 0.0207(15) Uani 1 1 d . . . . .
H8 H -0.0353 -0.1166 0.2041 0.025 Uiso 1 1 calc R U . . .
C23 C 0.5307(7) 0.6773(5) 0.9268(5) 0.0176(14) Uani 1 1 d . . . . .
C10 C 0.2557(7) -0.0335(6) 0.4274(5) 0.0210(15) Uani 1 1 d . . . . .
H10 H 0.3538 -0.0510 0.4654 0.025 Uiso 1 1 calc R U . . .
C11 C 0.5620(6) -0.0277(5) 0.7483(5) 0.0134(13) Uani 1 1 d . . . . .
C20 C 0.7027(7) 0.4870(5) 0.9509(5) 0.0156(13) Uani 1 1 d . . . . .
H20 H 0.7610 0.4230 0.9600 0.019 Uiso 1 1 calc R U . . .
C14 C 0.7195(7) -0.3135(5) 0.7208(5) 0.0161(13) Uani 1 1 d . . . . .
C21 C 0.7570(7) 0.5857(6) 1.0203(5) 0.0187(14) Uani 1 1 d . . . . .
C24 C 0.4726(6) 0.5814(5) 0.8542(5) 0.0138(13) Uani 1 1 d . . . . .
H24 H 0.3772 0.5809 0.7974 0.017 Uiso 1 1 calc R U . . .
C5 C 0.0156(6) 0.1846(5) 0.4582(5) 0.0156(13) Uani 1 1 d . . . . .
C3 C -0.1735(7) 0.3122(6) 0.4569(6) 0.0220(15) Uani 1 1 d . . . . .
H3 H -0.2709 0.3320 0.4289 0.026 Uiso 1 1 calc R U . . .
C16 C 0.9021(6) -0.2002(5) 0.8731(5) 0.0160(14) Uani 1 1 d . . . . .
C19 C 0.5597(7) 0.4859(5) 0.8678(5) 0.0150(13) Uani 1 1 d . . . . .
C12 C 0.6643(7) -0.1262(5) 0.7732(5) 0.0152(13) Uani 1 1 d . . . . .
C13 C 0.6196(7) -0.2257(5) 0.7026(5) 0.0165(14) Uani 1 1 d . . . . .
H13 H 0.5252 -0.2334 0.6446 0.020 Uiso 1 1 calc R U . . .
C1 C 0.0748(7) 0.3433(6) 0.5839(6) 0.0244(16) Uani 1 1 d . . . . .
H1 H 0.1451 0.3876 0.6437 0.029 Uiso 1 1 calc R U . . .
C15 C 0.8620(7) -0.3021(5) 0.8043(5) 0.0183(14) Uani 1 1 d . . . . .
H15 H 0.9288 -0.3601 0.8142 0.022 Uiso 1 1 calc R U . . .
C9 C 0.1701(7) -0.0999(6) 0.3284(6) 0.0207(15) Uani 1 1 d . . . . .
H9 H 0.2094 -0.1613 0.3023 0.025 Uiso 1 1 calc R U . . .
C17 C 0.8052(6) -0.1128(5) 0.8580(5) 0.0170(14) Uani 1 1 d . . . . .
H17 H 0.8341 -0.0455 0.9041 0.020 Uiso 1 1 calc R U . . .
C4 C -0.1322(7) 0.2155(6) 0.4137(6) 0.0226(15) Uani 1 1 d . . . . .
H4 H -0.2020 0.1700 0.3548 0.027 Uiso 1 1 calc R U . . .
C22 C 0.6719(7) 0.6826(5) 1.0105(5) 0.0188(14) Uani 1 1 d . . . . .
H22 H 0.7091 0.7479 1.0585 0.023 Uiso 1 1 calc R U . . .
C2 C -0.0692(7) 0.3789(6) 0.5416(6) 0.0256(16) Uani 1 1 d . . . . .
H2 H -0.0936 0.4465 0.5704 0.031 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 1.761(4) . ?
U1 O1 1.765(4) . ?
U1 O5 2.450(4) . ?
U1 O3 2.458(4) . ?
U1 O4 2.465(4) . ?
U1 O6 2.477(4) . ?
U1 N2 2.665(5) . ?
U1 N1 2.681(5) . ?
U1 C18 2.834(6) . ?
U1 C11 2.842(6) . ?
Br1 C14 1.891(6) . ?
Br2 C16 1.905(6) . ?
Br4 C23 1.891(6) . ?
Br3 C21 1.906(6) . ?
O6 C18 1.268(7) . ?
O4 C11 1.264(7) . ?
O3 C11 1.275(7) . ?
O5 C18 1.253(7) . ?
N1 C5 1.342(7) . ?
N1 C1 1.342(8) . ?
C18 C19 1.504(8) . ?
N2 C6 1.347(7) . ?
N2 C10 1.347(8) . ?
C7 C8 1.374(9) . ?
C7 C6 1.404(8) . ?
C6 C5 1.474(8) . ?
C8 C9 1.375(9) . ?
C23 C22 1.375(9) . ?
C23 C24 1.383(9) . ?
C10 C9 1.386(9) . ?
C11 C12 1.497(8) . ?
C20 C21 1.386(8) . ?
C20 C19 1.385(8) . ?
C14 C15 1.387(8) . ?
C14 C13 1.394(8) . ?
C21 C22 1.397(9) . ?
C24 C19 1.389(8) . ?
C5 C4 1.412(8) . ?
C3 C2 1.363(9) . ?
C3 C4 1.371(9) . ?
C16 C17 1.374(8) . ?
C16 C15 1.400(8) . ?
C12 C17 1.382(8) . ?
C12 C13 1.389(8) . ?
C1 C2 1.394(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U1 O1 179.4(2) . . ?
O2 U1 O5 92.21(17) . . ?
O1 U1 O5 87.53(17) . . ?
O2 U1 O3 86.35(17) . . ?
O1 U1 O3 93.25(16) . . ?
O5 U1 O3 116.59(13) . . ?
O2 U1 O4 90.18(17) . . ?
O1 U1 O4 89.18(17) . . ?
O5 U1 O4 63.81(14) . . ?
O3 U1 O4 52.81(13) . . ?
O2 U1 O6 90.43(17) . . ?
O1 U1 O6 89.88(17) . . ?
O5 U1 O6 52.65(13) . . ?
O3 U1 O6 168.69(13) . . ?
O4 U1 O6 116.44(13) . . ?
O2 U1 N2 100.27(17) . . ?
O1 U1 N2 80.00(17) . . ?
O5 U1 N2 167.43(15) . . ?
O3 U1 N2 66.10(14) . . ?
O4 U1 N2 117.10(14) . . ?
O6 U1 N2 125.18(14) . . ?
O2 U1 N1 79.13(17) . . ?
O1 U1 N1 101.50(18) . . ?
O5 U1 N1 121.57(15) . . ?
O3 U1 N1 120.24(15) . . ?
O4 U1 N1 167.97(15) . . ?
O6 U1 N1 69.58(14) . . ?
N2 U1 N1 60.33(15) . . ?
O2 U1 C18 90.37(18) . . ?
O1 U1 C18 89.65(18) . . ?
O5 U1 C18 26.16(15) . . ?
O3 U1 C18 142.50(16) . . ?
O4 U1 C18 89.90(16) . . ?
O6 U1 C18 26.54(15) . . ?
N2 U1 C18 150.63(17) . . ?
N1 U1 C18 95.61(17) . . ?
O2 U1 C11 89.90(18) . . ?
O1 U1 C11 89.52(18) . . ?
O5 U1 C11 90.16(15) . . ?
O3 U1 C11 26.58(14) . . ?
O4 U1 C11 26.35(14) . . ?
O6 U1 C11 142.79(15) . . ?
N2 U1 C11 91.26(16) . . ?
N1 U1 C11 146.45(16) . . ?
C18 U1 C11 116.25(17) . . ?
C18 O6 U1 92.6(4) . . ?
C11 O4 U1 93.7(3) . . ?
C11 O3 U1 93.8(4) . . ?
C18 O5 U1 94.3(4) . . ?
C5 N1 C1 117.7(5) . . ?
C5 N1 U1 121.5(4) . . ?
C1 N1 U1 119.1(4) . . ?
O5 C18 O6 120.2(6) . . ?
O5 C18 C19 119.4(6) . . ?
O6 C18 C19 120.4(5) . . ?
O5 C18 U1 59.5(3) . . ?
O6 C18 U1 60.8(3) . . ?
C19 C18 U1 174.8(4) . . ?
C6 N2 C10 117.1(5) . . ?
C6 N2 U1 122.9(4) . . ?
C10 N2 U1 120.0(4) . . ?
C8 C7 C6 120.5(6) . . ?
N2 C6 C7 121.2(6) . . ?
N2 C6 C5 116.4(5) . . ?
C7 C6 C5 122.4(5) . . ?
C7 C8 C9 118.5(6) . . ?
C22 C23 C24 122.6(6) . . ?
C22 C23 Br4 117.2(5) . . ?
C24 C23 Br4 120.2(5) . . ?
N2 C10 C9 124.3(6) . . ?
O4 C11 O3 119.2(5) . . ?
O4 C11 C12 120.3(5) . . ?
O3 C11 C12 120.3(5) . . ?
O4 C11 U1 59.9(3) . . ?
O3 C11 U1 59.6(3) . . ?
C12 C11 U1 169.3(4) . . ?
C21 C20 C19 118.4(6) . . ?
C15 C14 C13 121.5(6) . . ?
C15 C14 Br1 119.6(5) . . ?
C13 C14 Br1 118.8(5) . . ?
C20 C21 C22 122.3(6) . . ?
C20 C21 Br3 119.8(5) . . ?
C22 C21 Br3 117.9(5) . . ?
C23 C24 C19 118.7(6) . . ?
N1 C5 C4 120.7(6) . . ?
N1 C5 C6 116.8(5) . . ?
C4 C5 C6 122.4(5) . . ?
C2 C3 C4 118.9(6) . . ?
C17 C16 C15 121.7(5) . . ?
C17 C16 Br2 120.1(5) . . ?
C15 C16 Br2 118.2(4) . . ?
C24 C19 C20 120.8(6) . . ?
C24 C19 C18 121.0(6) . . ?
C20 C19 C18 118.2(5) . . ?
C17 C12 C13 121.3(6) . . ?
C17 C12 C11 119.5(5) . . ?
C13 C12 C11 119.0(5) . . ?
C12 C13 C14 118.5(6) . . ?
N1 C1 C2 123.8(6) . . ?
C14 C15 C16 117.9(6) . . ?
C8 C9 C10 118.4(6) . . ?
C16 C17 C12 119.1(6) . . ?
C3 C4 C5 120.4(6) . . ?
C23 C22 C21 117.1(6) . . ?
C3 C2 C1 118.4(6) . . ?

_refine_diff_density_max         1.131
_refine_diff_density_min         -1.365
_refine_diff_density_rms         0.215

_shelxl_version_number           2014-1


_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?


#===END
