# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2015

####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_Compound_1
_database_code_depnum_ccdc_archive 'CCDC 1025739'
_audit_update_record             
;
2014-09-23 deposited with the CCDC.
2014-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H16 Br2 N2 O6 U'
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow

_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         850.26

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                   8.9104(8)
_cell_length_b                   12.1555(10)
_cell_length_c                   13.0201(11)
_cell_angle_alpha                63.614(4)
_cell_angle_beta                 76.124(4)
_cell_angle_gamma                84.538(3)
_cell_volume                     1226.32(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    16445
_cell_measurement_theta_min      5.247
_cell_measurement_theta_max      54.977
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.303
_exptl_crystal_F_000             792
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    9.923
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6069
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS, 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            16445
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.790
_diffrn_reflns_theta_max         27.638
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5695
_reflns_number_gt                5111
_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-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Crystal Maker (Palmer, 2009)'
_computing_publication_material  'WINGX (Farrugia, 2012)'

_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)+(0.0184P)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         5695
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0255
_refine_ls_wR_factor_ref         0.0496
_refine_ls_wR_factor_gt          0.0481
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_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 0.25749(2) 0.56469(2) 0.24104(2) 0.01066(4) Uani 1 1 d . . . . .
Br1 Br 0.74953(5) -0.01736(3) 0.49205(4) 0.01983(9) Uani 1 1 d . . . . .
Br2 Br 0.77110(4) 0.73221(4) 0.39601(3) 0.01953(9) Uani 1 1 d . . . . .
O1 O 0.3736(3) 0.6201(2) 0.0956(2) 0.0164(6) Uani 1 1 d . . . . .
O4 O 0.4819(3) 0.5344(2) 0.3272(2) 0.0154(6) Uani 1 1 d . . . . .
O2 O 0.1351(3) 0.5075(2) 0.3831(2) 0.0148(6) Uani 1 1 d . . . . .
O3 O 0.4104(3) 0.3822(2) 0.3013(2) 0.0141(6) Uani 1 1 d . . . . .
O5 O 0.2555(3) 0.7513(2) 0.2335(2) 0.0191(6) Uani 1 1 d . . . . .
N1 N 0.0213(3) 0.6337(3) 0.1501(3) 0.0142(7) Uani 1 1 d . . . . .
N2 N 0.1302(3) 0.3998(3) 0.2120(3) 0.0122(6) Uani 1 1 d . . . . .
C23 C 0.6572(5) 0.8487(4) 0.2890(3) 0.0196(9) Uani 1 1 d . . . . .
O6 O 0.1912(4) 0.9478(3) 0.1516(3) 0.0318(8) Uani 1 1 d . . . . .
C12 C -0.0604(4) 0.5509(4) 0.1400(3) 0.0138(8) Uani 1 1 d . . . . .
C11 C -0.0041(4) 0.4277(3) 0.1730(3) 0.0123(8) Uani 1 1 d . . . . .
C16 C 0.7389(4) 0.1488(3) 0.4697(3) 0.0133(8) Uani 1 1 d . . . . .
C17 C 0.8451(4) 0.1934(4) 0.5045(3) 0.0148(8) Uani 1 1 d . . . . .
H17 H 0.9201 0.1423 0.5404 0.018 Uiso 1 1 calc R U . . .
C6 C -0.2246(4) 0.3780(4) 0.1170(3) 0.0194(9) Uani 1 1 d . . . . .
H6 H -0.2787 0.3209 0.1098 0.023 Uiso 1 1 calc R U . . .
C3 C -0.2464(4) 0.7056(4) 0.0617(3) 0.0184(9) Uani 1 1 d . . . . .
H3 H -0.3369 0.7298 0.0342 0.022 Uiso 1 1 calc R U . . .
C19 C 0.7248(4) 0.3913(3) 0.4326(3) 0.0135(8) Uani 1 1 d . . . . .
H19 H 0.7197 0.4729 0.4204 0.016 Uiso 1 1 calc R U . . .
C26 C 0.4969(6) 1.0179(4) 0.1327(4) 0.0297(11) Uani 1 1 d . . . . .
H26 H 0.4413 1.0760 0.0812 0.036 Uiso 1 1 calc R U . . .
C18 C 0.8380(4) 0.3155(4) 0.4849(3) 0.0153(8) Uani 1 1 d . . . . .
H18 H 0.9097 0.3468 0.5069 0.018 Uiso 1 1 calc R U . . .
C21 C 0.4354(5) 0.9007(4) 0.2046(3) 0.0188(9) Uani 1 1 d . . . . .
C24 C 0.7223(5) 0.9647(4) 0.2159(4) 0.0298(11) Uani 1 1 d . . . . .
H24 H 0.8180 0.9854 0.2197 0.036 Uiso 1 1 calc R U . . .
C2 C -0.1614(4) 0.7889(4) 0.0689(3) 0.0194(9) Uani 1 1 d . . . . .
H2 H -0.1911 0.8705 0.0438 0.023 Uiso 1 1 calc R U . . .
C4 C -0.1970(4) 0.5838(4) 0.0958(3) 0.0153(8) Uani 1 1 d . . . . .
C10 C 0.1830(4) 0.2852(3) 0.2404(3) 0.0159(8) Uani 1 1 d . . . . .
H10 H 0.2737 0.2648 0.2680 0.019 Uiso 1 1 calc R U . . .
C7 C -0.0855(4) 0.3420(4) 0.1611(3) 0.0144(8) Uani 1 1 d . . . . .
C1 C -0.0283(4) 0.7488(4) 0.1149(3) 0.0179(9) Uani 1 1 d . . . . .
H1 H 0.0279 0.8054 0.1211 0.021 Uiso 1 1 calc R U . . .
C13 C 0.4988(4) 0.4243(3) 0.3401(3) 0.0106(7) Uani 1 1 d . . . . .
C14 C 0.6194(4) 0.3450(3) 0.3986(3) 0.0100(7) Uani 1 1 d . . . . .
C8 C -0.0257(5) 0.2225(4) 0.1925(3) 0.0188(9) Uani 1 1 d . . . . .
H8 H -0.0774 0.1630 0.1870 0.023 Uiso 1 1 calc R U . . .
C20 C 0.2821(5) 0.8681(4) 0.1939(3) 0.0190(9) Uani 1 1 d . . . . .
C15 C 0.6254(4) 0.2220(3) 0.4169(3) 0.0112(7) Uani 1 1 d . . . . .
H15 H 0.5549 0.1907 0.3941 0.013 Uiso 1 1 calc R U . . .
C9 C 0.1090(4) 0.1951(4) 0.2309(3) 0.0171(8) Uani 1 1 d . . . . .
H9 H 0.1510 0.1173 0.2505 0.020 Uiso 1 1 calc R U . . .
C22 C 0.5166(4) 0.8154(3) 0.2833(3) 0.0150(8) Uani 1 1 d . . . . .
H22 H 0.4769 0.7364 0.3318 0.018 Uiso 1 1 calc R U . . .
C25 C 0.6395(6) 1.0494(4) 0.1365(4) 0.0362(12) Uani 1 1 d . . . . .
H25 H 0.6807 1.1275 0.0859 0.043 Uiso 1 1 calc R U . . .
C5 C -0.2770(4) 0.4928(4) 0.0863(3) 0.0175(9) Uani 1 1 d . . . . .
H5 H -0.3673 0.5140 0.0582 0.021 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 1.769(2) . ?
U1 O1 1.780(3) . ?
U1 O5 2.225(3) . ?
U1 O3 2.405(2) . ?
U1 O4 2.442(2) . ?
U1 N1 2.552(3) . ?
U1 N2 2.600(3) . ?
U1 C13 2.806(4) . ?
Br1 C16 1.905(4) . ?
Br2 C23 1.904(4) . ?
O4 C13 1.272(4) . ?
O3 C13 1.278(4) . ?
O5 C20 1.301(4) . ?
N1 C1 1.331(5) . ?
N1 C12 1.366(5) . ?
N2 C10 1.341(5) . ?
N2 C11 1.366(4) . ?
C23 C22 1.381(5) . ?
C23 C24 1.390(6) . ?
O6 C20 1.220(5) . ?
C12 C4 1.418(5) . ?
C12 C11 1.438(5) . ?
C11 C7 1.405(5) . ?
C16 C15 1.381(5) . ?
C16 C17 1.383(5) . ?
C17 C18 1.388(5) . ?
C17 H17 0.9300 . ?
C6 C5 1.340(6) . ?
C6 C7 1.440(5) . ?
C6 H6 0.9300 . ?
C3 C2 1.368(6) . ?
C3 C4 1.403(5) . ?
C3 H3 0.9300 . ?
C19 C14 1.384(5) . ?
C19 C18 1.388(5) . ?
C19 H19 0.9300 . ?
C26 C25 1.379(6) . ?
C26 C21 1.387(5) . ?
C26 H26 0.9300 . ?
C18 H18 0.9300 . ?
C21 C22 1.384(5) . ?
C21 C20 1.511(6) . ?
C24 C25 1.395(6) . ?
C24 H24 0.9300 . ?
C2 C1 1.405(5) . ?
C2 H2 0.9300 . ?
C4 C5 1.436(5) . ?
C10 C9 1.395(5) . ?
C10 H10 0.9300 . ?
C7 C8 1.411(5) . ?
C1 H1 0.9300 . ?
C13 C14 1.486(5) . ?
C14 C15 1.403(5) . ?
C8 C9 1.366(5) . ?
C8 H8 0.9300 . ?
C15 H15 0.9300 . ?
C9 H9 0.9300 . ?
C22 H22 0.9300 . ?
C25 H25 0.9300 . ?
C5 H5 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
O2 U1 O1 177.20(11) . . ?
O2 U1 O5 90.86(11) . . ?
O1 U1 O5 90.55(11) . . ?
O2 U1 O3 90.27(10) . . ?
O1 U1 O3 90.30(10) . . ?
O5 U1 O3 138.10(9) . . ?
O2 U1 O4 89.97(10) . . ?
O1 U1 O4 92.58(10) . . ?
O5 U1 O4 84.21(9) . . ?
O3 U1 O4 53.90(8) . . ?
O2 U1 N1 89.94(10) . . ?
O1 U1 N1 87.76(11) . . ?
O5 U1 N1 85.70(10) . . ?
O3 U1 N1 136.18(9) . . ?
O4 U1 N1 169.91(9) . . ?
O2 U1 N2 86.55(10) . . ?
O1 U1 N2 91.02(10) . . ?
O5 U1 N2 149.74(10) . . ?
O3 U1 N2 72.11(9) . . ?
O4 U1 N2 125.88(9) . . ?
N1 U1 N2 64.17(10) . . ?
O2 U1 C13 89.11(11) . . ?
O1 U1 C13 92.63(11) . . ?
O5 U1 C13 111.12(10) . . ?
O3 U1 C13 27.03(9) . . ?
O4 U1 C13 26.91(9) . . ?
N1 U1 C13 163.16(10) . . ?
N2 U1 C13 98.99(10) . . ?
C13 O4 U1 92.7(2) . . ?
C13 O3 U1 94.3(2) . . ?
C20 O5 U1 160.6(3) . . ?
C1 N1 C12 118.4(3) . . ?
C1 N1 U1 121.6(3) . . ?
C12 N1 U1 120.0(2) . . ?
C10 N2 C11 117.4(3) . . ?
C10 N2 U1 123.8(2) . . ?
C11 N2 U1 118.7(2) . . ?
C22 C23 C24 122.0(4) . . ?
C22 C23 Br2 120.0(3) . . ?
C24 C23 Br2 118.0(3) . . ?
N1 C12 C4 121.8(3) . . ?
N1 C12 C11 118.8(3) . . ?
C4 C12 C11 119.4(3) . . ?
N2 C11 C7 122.6(3) . . ?
N2 C11 C12 118.0(3) . . ?
C7 C11 C12 119.4(3) . . ?
C15 C16 C17 121.9(3) . . ?
C15 C16 Br1 118.2(3) . . ?
C17 C16 Br1 119.8(3) . . ?
C16 C17 C18 119.1(3) . . ?
C16 C17 H17 120.5 . . ?
C18 C17 H17 120.5 . . ?
C5 C6 C7 120.7(4) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 H6 119.7 . . ?
C2 C3 C4 120.0(4) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C14 C19 C18 119.7(3) . . ?
C14 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C25 C26 C21 120.9(4) . . ?
C25 C26 H26 119.6 . . ?
C21 C26 H26 119.6 . . ?
C17 C18 C19 120.4(3) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C22 C21 C26 119.4(4) . . ?
C22 C21 C20 121.4(4) . . ?
C26 C21 C20 119.2(4) . . ?
C23 C24 C25 117.9(4) . . ?
C23 C24 H24 121.1 . . ?
C25 C24 H24 121.1 . . ?
C3 C2 C1 118.7(4) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C3 C4 C12 117.8(4) . . ?
C3 C4 C5 123.0(4) . . ?
C12 C4 C5 119.2(4) . . ?
N2 C10 C9 123.5(4) . . ?
N2 C10 H10 118.3 . . ?
C9 C10 H10 118.3 . . ?
C11 C7 C8 118.0(3) . . ?
C11 C7 C6 119.8(4) . . ?
C8 C7 C6 122.2(4) . . ?
N1 C1 C2 123.2(4) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
O4 C13 O3 119.0(3) . . ?
O4 C13 C14 121.1(3) . . ?
O3 C13 C14 120.0(3) . . ?
O4 C13 U1 60.36(18) . . ?
O3 C13 U1 58.72(18) . . ?
C14 C13 U1 176.5(2) . . ?
C19 C14 C15 120.7(3) . . ?
C19 C14 C13 121.1(3) . . ?
C15 C14 C13 118.2(3) . . ?
C9 C8 C7 119.2(4) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
O6 C20 O5 123.6(4) . . ?
O6 C20 C21 121.0(4) . . ?
O5 C20 C21 115.4(3) . . ?
C16 C15 C14 118.2(3) . . ?
C16 C15 H15 120.9 . . ?
C14 C15 H15 120.9 . . ?
C8 C9 C10 119.3(4) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C23 C22 C21 119.4(4) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C26 C25 C24 120.4(4) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C6 C5 C4 121.5(4) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?

_refine_diff_density_max         0.939
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.147

_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 ?
####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_Compound_2
_database_code_depnum_ccdc_archive 'CCDC 1025740'
_audit_update_record             
;
2014-09-23 deposited with the CCDC.
2014-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H16 Br2 N2 O6 U'
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         850.26

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

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

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

_cell_length_a                   12.4466(8)
_cell_length_b                   21.6789(13)
_cell_length_c                   9.4110(6)
_cell_angle_alpha                90
_cell_angle_beta                 95.249(4)
_cell_angle_gamma                90
_cell_volume                     2528.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    34243
_cell_measurement_theta_min      4.735
_cell_measurement_theta_max      47.147
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.233
_exptl_crystal_F_000             1584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    9.624
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6051
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS, 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            25279
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.643
_diffrn_reflns_theta_max         27.974
_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             6099
_reflns_number_gt                4576
_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    'Crystal Maker (Palmer, 2009)'
_computing_publication_material  'WINGX (Farrugia, 2012)'

_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)+(0.0260P)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         6099
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0311
_refine_ls_wR_factor_ref         0.0623
_refine_ls_wR_factor_gt          0.0560
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_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 0.19607(2) 0.08861(2) 0.23512(2) 0.03020(6) Uani 1 1 d . . . . .
Br2 Br 0.52061(4) 0.45616(2) 0.17930(6) 0.05124(14) Uani 1 1 d . . . . .
Br1 Br 0.31416(6) -0.23444(3) -0.32590(7) 0.06907(18) Uani 1 1 d . . . . .
O2 O 0.2840(2) 0.06411(14) 0.3807(3) 0.0403(8) Uani 1 1 d . . . . .
O1 O 0.1082(3) 0.11560(15) 0.0907(3) 0.0439(8) Uani 1 1 d . . . . .
O5 O 0.3408(3) 0.15520(14) 0.1525(3) 0.0434(8) Uani 1 1 d . . . . .
O4 O 0.3133(2) 0.03621(13) 0.0648(3) 0.0393(8) Uani 1 1 d . . . . .
O6 O 0.2332(3) 0.19637(14) 0.2957(3) 0.0413(8) Uani 1 1 d . . . . .
O3 O 0.1864(3) -0.01661(14) 0.1542(3) 0.0457(8) Uani 1 1 d . . . . .
N1 N 0.0839(3) 0.13051(17) 0.4429(4) 0.0352(9) Uani 1 1 d . . . . .
C15 C 0.1984(4) -0.1126(2) -0.0416(5) 0.0472(13) Uani 1 1 d . . . . .
H15 H 0.1362 -0.1089 0.0054 0.057 Uiso 1 1 calc R U . . .
N2 N 0.0103(3) 0.03145(17) 0.2859(4) 0.0323(8) Uani 1 1 d . . . . .
C11 C -0.0561(3) 0.05764(19) 0.3754(4) 0.0289(10) Uani 1 1 d . . . . .
C21 C 0.3658(3) 0.2624(2) 0.2119(5) 0.0323(10) Uani 1 1 d . . . . .
C12 C -0.0171(3) 0.10929(19) 0.4605(4) 0.0297(10) Uani 1 1 d . . . . .
C3 C -0.0366(4) 0.1818(2) 0.6485(5) 0.0485(13) Uani 1 1 d . . . . .
H3 H -0.0771 0.2003 0.7151 0.058 Uiso 1 1 calc R U . . .
C9 C -0.1288(4) -0.0439(2) 0.2249(5) 0.0403(11) Uani 1 1 d . . . . .
H9 H -0.1503 -0.0791 0.1735 0.048 Uiso 1 1 calc R U . . .
C6 C -0.2254(4) 0.0642(2) 0.4886(5) 0.0428(12) Uani 1 1 d . . . . .
H6 H -0.2953 0.0501 0.4951 0.051 Uiso 1 1 calc R U . . .
C8 C -0.1948(4) -0.0173(2) 0.3133(5) 0.0413(12) Uani 1 1 d . . . . .
H8 H -0.2630 -0.0336 0.3217 0.050 Uiso 1 1 calc R U . . .
C10 C -0.0273(4) -0.0175(2) 0.2119(5) 0.0397(11) Uani 1 1 d . . . . .
H10 H 0.0163 -0.0353 0.1479 0.048 Uiso 1 1 calc R U . . .
C13 C 0.2616(4) -0.0136(2) 0.0713(5) 0.0357(11) Uani 1 1 d . . . . .
C23 C 0.4822(4) 0.3312(2) 0.0994(5) 0.0400(12) Uani 1 1 d . . . . .
H23 H 0.5288 0.3392 0.0298 0.048 Uiso 1 1 calc R U . . .
C25 C 0.3903(4) 0.3662(2) 0.2992(5) 0.0365(11) Uani 1 1 d . . . . .
H25 H 0.3773 0.3967 0.3649 0.044 Uiso 1 1 calc R U . . .
C22 C 0.4368(4) 0.2739(2) 0.1098(5) 0.0372(11) Uani 1 1 d . . . . .
H22 H 0.4538 0.2427 0.0480 0.045 Uiso 1 1 calc R U . . .
C5 C -0.1884(4) 0.1117(2) 0.5710(5) 0.0413(12) Uani 1 1 d . . . . .
H5 H -0.2322 0.1296 0.6345 0.050 Uiso 1 1 calc R U . . .
C20 C 0.3114(4) 0.2015(2) 0.2204(5) 0.0340(10) Uani 1 1 d . . . . .
C7 C -0.1604(3) 0.0347(2) 0.3918(5) 0.0327(10) Uani 1 1 d . . . . .
C1 C 0.1228(4) 0.1743(2) 0.5308(5) 0.0488(13) Uani 1 1 d . . . . .
H1 H 0.1922 0.1887 0.5215 0.059 Uiso 1 1 calc R U . . .
C24 C 0.4578(3) 0.3769(2) 0.1935(5) 0.0327(10) Uani 1 1 d . . . . .
C14 C 0.2790(4) -0.0686(2) -0.0192(5) 0.0361(11) Uani 1 1 d . . . . .
C18 C 0.3862(4) -0.1257(2) -0.1733(5) 0.0480(13) Uani 1 1 d . . . . .
H18 H 0.4501 -0.1312 -0.2159 0.058 Uiso 1 1 calc R U . . .
C4 C -0.0816(4) 0.1349(2) 0.5610(5) 0.0369(11) Uani 1 1 d . . . . .
C26 C 0.3425(4) 0.3087(2) 0.3045(5) 0.0335(10) Uani 1 1 d . . . . .
H26 H 0.2938 0.3013 0.3718 0.040 Uiso 1 1 calc R U . . .
C19 C 0.3737(4) -0.0757(2) -0.0850(5) 0.0429(12) Uani 1 1 d . . . . .
H19 H 0.4287 -0.0469 -0.0696 0.051 Uiso 1 1 calc R U . . .
C17 C 0.3028(4) -0.1672(2) -0.1972(5) 0.0447(13) Uani 1 1 d . . . . .
C16 C 0.2090(5) -0.1612(2) -0.1316(6) 0.0542(14) Uani 1 1 d . . . . .
H16 H 0.1537 -0.1899 -0.1482 0.065 Uiso 1 1 calc R U . . .
C2 C 0.0657(5) 0.2003(3) 0.6367(6) 0.0581(16) Uani 1 1 d . . . . .
H2 H 0.0977 0.2299 0.6982 0.070 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 1.755(3) . ?
U1 O1 1.764(3) . ?
U1 O3 2.404(3) . ?
U1 O6 2.439(3) . ?
U1 O5 2.488(3) . ?
U1 O4 2.533(3) . ?
U1 N1 2.664(4) . ?
U1 N2 2.705(4) . ?
U1 C20 2.847(4) . ?
U1 C13 2.860(5) . ?
Br2 C24 1.897(4) . ?
Br1 C17 1.908(5) . ?
O5 C20 1.262(5) . ?
O4 C13 1.261(5) . ?
O6 C20 1.261(5) . ?
O3 C13 1.274(5) . ?
N1 C1 1.323(6) . ?
N1 C12 1.363(5) . ?
C15 C16 1.367(7) . ?
C15 C14 1.385(6) . ?
C15 H15 0.9300 . ?
N2 C10 1.330(5) . ?
N2 C11 1.357(5) . ?
C11 C7 1.412(6) . ?
C11 C12 1.435(6) . ?
C21 C26 1.378(6) . ?
C21 C22 1.387(6) . ?
C21 C20 1.490(6) . ?
C12 C4 1.409(6) . ?
C3 C2 1.350(7) . ?
C3 C4 1.394(6) . ?
C3 H3 0.9300 . ?
C9 C8 1.351(7) . ?
C9 C10 1.402(6) . ?
C9 H9 0.9300 . ?
C6 C5 1.345(7) . ?
C6 C7 1.424(6) . ?
C6 H6 0.9300 . ?
C8 C7 1.393(6) . ?
C8 H8 0.9300 . ?
C10 H10 0.9300 . ?
C13 C14 1.493(6) . ?
C23 C22 1.371(6) . ?
C23 C24 1.382(6) . ?
C23 H23 0.9300 . ?
C25 C24 1.379(6) . ?
C25 C26 1.383(6) . ?
C25 H25 0.9300 . ?
C22 H22 0.9300 . ?
C5 C4 1.432(6) . ?
C5 H5 0.9300 . ?
C1 C2 1.394(7) . ?
C1 H1 0.9300 . ?
C14 C19 1.389(6) . ?
C18 C19 1.383(6) . ?
C18 C17 1.376(7) . ?
C18 H18 0.9300 . ?
C26 H26 0.9300 . ?
C19 H19 0.9300 . ?
C17 C16 1.376(7) . ?
C16 H16 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
O2 U1 O1 178.24(14) . . ?
O2 U1 O3 88.27(13) . . ?
O1 U1 O3 93.49(14) . . ?
O2 U1 O6 90.92(13) . . ?
O1 U1 O6 87.33(13) . . ?
O3 U1 O6 170.33(10) . . ?
O2 U1 O5 90.11(13) . . ?
O1 U1 O5 88.97(13) . . ?
O3 U1 O5 117.93(10) . . ?
O6 U1 O5 52.43(10) . . ?
O2 U1 O4 90.23(13) . . ?
O1 U1 O4 90.77(13) . . ?
O3 U1 O4 52.35(10) . . ?
O6 U1 O4 118.03(10) . . ?
O5 U1 O4 65.61(10) . . ?
O2 U1 N1 82.06(13) . . ?
O1 U1 N1 97.05(13) . . ?
O3 U1 N1 122.78(11) . . ?
O6 U1 N1 66.58(10) . . ?
O5 U1 N1 118.34(10) . . ?
O4 U1 N1 171.21(11) . . ?
O2 U1 N2 101.87(12) . . ?
O1 U1 N2 78.95(13) . . ?
O3 U1 N2 66.56(11) . . ?
O6 U1 N2 122.98(10) . . ?
O5 U1 N2 167.51(10) . . ?
O4 U1 N2 117.23(10) . . ?
N1 U1 N2 60.82(11) . . ?
O2 U1 C20 90.97(13) . . ?
O1 U1 C20 87.54(14) . . ?
O3 U1 C20 144.19(12) . . ?
O6 U1 C20 26.17(11) . . ?
O5 U1 C20 26.27(11) . . ?
O4 U1 C20 91.86(11) . . ?
N1 U1 C20 92.48(12) . . ?
N2 U1 C20 147.74(12) . . ?
O2 U1 C13 89.88(13) . . ?
O1 U1 C13 91.65(14) . . ?
O3 U1 C13 26.23(11) . . ?
O6 U1 C13 144.17(12) . . ?
O5 U1 C13 91.75(12) . . ?
O4 U1 C13 26.14(11) . . ?
N1 U1 C13 148.67(12) . . ?
N2 U1 C13 91.78(12) . . ?
C20 U1 C13 118.01(13) . . ?
C20 O5 U1 93.0(3) . . ?
C13 O4 U1 91.6(3) . . ?
C20 O6 U1 95.3(3) . . ?
C13 O3 U1 97.3(3) . . ?
C1 N1 C12 117.1(4) . . ?
C1 N1 U1 121.2(3) . . ?
C12 N1 U1 121.7(3) . . ?
C16 C15 C14 121.0(5) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C10 N2 C11 117.0(4) . . ?
C10 N2 U1 122.5(3) . . ?
C11 N2 U1 119.8(3) . . ?
N2 C11 C7 122.5(4) . . ?
N2 C11 C12 118.6(4) . . ?
C7 C11 C12 118.8(4) . . ?
C26 C21 C22 119.4(4) . . ?
C26 C21 C20 119.3(4) . . ?
C22 C21 C20 121.2(4) . . ?
N1 C12 C4 122.5(4) . . ?
N1 C12 C11 117.6(4) . . ?
C4 C12 C11 119.8(4) . . ?
C2 C3 C4 119.9(5) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C8 C9 C10 118.9(4) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C5 C6 C7 121.9(4) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C9 C8 C7 119.8(4) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
N2 C10 C9 123.7(4) . . ?
N2 C10 H10 118.1 . . ?
C9 C10 H10 118.1 . . ?
O4 C13 O3 118.7(4) . . ?
O4 C13 C14 123.7(4) . . ?
O3 C13 C14 117.5(4) . . ?
O4 C13 U1 62.3(2) . . ?
O3 C13 U1 56.5(2) . . ?
C14 C13 U1 171.8(3) . . ?
C22 C23 C24 119.2(4) . . ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 . . ?
C24 C25 C26 118.1(4) . . ?
C24 C25 H25 121.0 . . ?
C26 C25 H25 121.0 . . ?
C23 C22 C21 120.4(4) . . ?
C23 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C6 C5 C4 120.1(4) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
O5 C20 O6 119.3(4) . . ?
O5 C20 C21 121.6(4) . . ?
O6 C20 C21 119.1(4) . . ?
O5 C20 U1 60.8(2) . . ?
O6 C20 U1 58.5(2) . . ?
C21 C20 U1 176.8(3) . . ?
C8 C7 C11 117.9(4) . . ?
C8 C7 C6 122.5(4) . . ?
C11 C7 C6 119.5(4) . . ?
N1 C1 C2 123.8(5) . . ?
N1 C1 H1 118.1 . . ?
C2 C1 H1 118.1 . . ?
C25 C24 C23 121.7(4) . . ?
C25 C24 Br2 119.1(3) . . ?
C23 C24 Br2 119.2(3) . . ?
C15 C14 C19 119.2(4) . . ?
C15 C14 C13 119.7(4) . . ?
C19 C14 C13 121.1(4) . . ?
C19 C18 C17 119.0(5) . . ?
C19 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
C12 C4 C3 117.5(4) . . ?
C12 C4 C5 119.7(4) . . ?
C3 C4 C5 122.8(4) . . ?
C21 C26 C25 121.2(4) . . ?
C21 C26 H26 119.4 . . ?
C25 C26 H26 119.4 . . ?
C18 C19 C14 120.1(5) . . ?
C18 C19 H19 119.9 . . ?
C14 C19 H19 119.9 . . ?
C16 C17 C18 121.5(5) . . ?
C16 C17 Br1 118.2(4) . . ?
C18 C17 Br1 120.3(4) . . ?
C17 C16 C15 119.0(5) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
C3 C2 C1 119.0(5) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?

_refine_diff_density_max         0.597
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.123

_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/. 
# 
# Audit and citation data items have may 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_Compound_3
_database_code_depnum_ccdc_archive 'CCDC 1025741'
_audit_update_record             
;
2014-09-23 deposited with the CCDC.
2014-12-08 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H16 Br4 N2 O7 U'
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow

_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         1026.08

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'
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      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

_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'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   14.2282(8)
_cell_length_b                   6.5817(4)
_cell_length_c                   16.1780(9)
_cell_angle_alpha                90
_cell_angle_beta                 115.259(5)
_cell_angle_gamma                90
_cell_volume                     1370.15(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    18307
_cell_measurement_theta_min      5.029
_cell_measurement_theta_max      54.151
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.487
_exptl_crystal_F_000             948
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    11.805
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5319
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS, 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            18291
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.392
_diffrn_reflns_theta_max         27.603
_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             3465
_reflns_number_gt                2976
_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    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Crystal Maker (Palmer, 2009)'
_computing_publication_material  'WINGX (Farrugia, 2012)'

_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)+(0.0192P)²+1.0033P] 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         3465
_refine_ls_number_parameters     238
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0279
_refine_ls_wR_factor_ref         0.0543
_refine_ls_wR_factor_gt          0.0512
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.023
_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 0.74127(2) 0.7500 0.67332(2) 0.00778(6) Uani 1 2 d S T P . .
Br3 Br 0.65818(5) 0.7500 1.03232(4) 0.01887(15) Uani 1 2 d S T P . .
Br2 Br 0.96884(5) 0.7500 1.20907(4) 0.01941(15) Uani 1 2 d S T P . .
Br1 Br 1.29063(5) 0.7500 1.09320(4) 0.01886(15) Uani 1 2 d S T P . .
Br4 Br 0.22333(5) 0.7500 0.81702(5) 0.02428(17) Uani 1 2 d S T P . .
O3 O 0.7949(3) 0.7500 0.8380(3) 0.0118(9) Uani 1 2 d S T P . .
O1 O 0.7429(2) 0.4807(4) 0.67093(19) 0.0111(6) Uani 1 1 d . . . . .
O4 O 0.5849(3) 0.7500 0.6748(3) 0.0129(9) Uani 1 2 d S T P . .
O5 O 0.4134(3) 0.7500 0.5907(3) 0.0151(9) Uani 1 2 d S T P . .
O2 O 0.9193(3) 0.7500 0.7917(3) 0.0123(9) Uani 1 2 d S T P . .
OW1 O 0.8025(3) 0.2500 0.5233(3) 0.0214(11) Uani 1 2 d S T P . .
N2 N 0.6413(4) 0.7500 0.5004(3) 0.0098(10) Uani 1 2 d S T P . .
C2 C 1.0194(5) 0.7500 0.5778(4) 0.0142(13) Uani 1 2 d S T P . .
H2 H 1.0915 0.7500 0.6092 0.017 Uiso 1 2 calc R U P . .
N1 N 0.8536(4) 0.7500 0.5848(3) 0.0122(11) Uani 1 2 d S T P . .
C19 C 0.9372(4) 0.7500 1.0237(4) 0.0092(12) Uani 1 2 d S T P . .
H19 H 0.8669 0.7500 1.0106 0.011 Uiso 1 2 calc R U P . .
C11 C 0.6951(4) 0.7500 0.4470(4) 0.0090(12) Uani 1 2 d S T P . .
C8 C 0.5349(5) 0.7500 0.3105(4) 0.0129(13) Uani 1 2 d S T P . .
H8 H 0.4989 0.7500 0.2471 0.016 Uiso 1 2 calc R U P . .
C3 C 0.9728(5) 0.7500 0.4848(4) 0.0145(13) Uani 1 2 d S T P . .
H3 H 1.0126 0.7500 0.4517 0.017 Uiso 1 2 calc R U P . .
C4 C 0.8637(5) 0.7500 0.4394(4) 0.0128(13) Uani 1 2 d S T P . .
C20 C 0.4894(4) 0.7500 0.6650(4) 0.0107(12) Uani 1 2 d S T P . .
C22 C 0.5600(5) 0.7500 0.8378(4) 0.0121(13) Uani 1 2 d S T P . .
H22 H 0.6275 0.7500 0.8426 0.015 Uiso 1 2 calc R U P . .
C7 C 0.6440(4) 0.7500 0.3514(4) 0.0103(12) Uani 1 2 d S T P . .
C6 C 0.7033(5) 0.7500 0.2993(4) 0.0165(14) Uani 1 2 d S T P . .
H6 H 0.6697 0.7500 0.2358 0.020 Uiso 1 2 calc R U P . .
C5 C 0.8089(5) 0.7500 0.3422(5) 0.0191(14) Uani 1 2 d S T P . .
H5 H 0.8464 0.7500 0.3071 0.023 Uiso 1 2 calc R U P . .
C26 C 0.3747(5) 0.7500 0.7463(4) 0.0152(13) Uani 1 2 d S T P . .
H26 H 0.3177 0.7500 0.6895 0.018 Uiso 1 2 calc R U P . .
C12 C 0.8061(4) 0.7500 0.4915(4) 0.0092(12) Uani 1 2 d S T P . .
C13 C 0.8909(5) 0.7500 0.8562(4) 0.0095(12) Uani 1 2 d S T P . .
C23 C 0.5428(5) 0.7500 0.9148(4) 0.0121(13) Uani 1 2 d S T P . .
C16 C 1.1470(4) 0.7500 1.0639(4) 0.0119(13) Uani 1 2 d S T P . .
C9 C 0.4813(5) 0.7500 0.3631(4) 0.0115(13) Uani 1 2 d S T P . .
H9 H 0.4090 0.7500 0.3365 0.014 Uiso 1 2 calc R U P . .
C15 C 1.0748(5) 0.7500 0.9732(4) 0.0096(12) Uani 1 2 d S T P . .
H15 H 1.0963 0.7500 0.9264 0.012 Uiso 1 2 calc R U P . .
C25 C 0.3606(5) 0.7500 0.8248(4) 0.0154(14) Uani 1 2 d S T P . .
C14 C 0.9695(4) 0.7500 0.9536(4) 0.0084(12) Uani 1 2 d S TU P . .
C21 C 0.4755(5) 0.7500 0.7519(4) 0.0107(12) Uani 1 2 d S T P . .
C24 C 0.4429(5) 0.7500 0.9109(5) 0.0166(14) Uani 1 2 d S T P . .
H24 H 0.4321 0.7500 0.9637 0.020 Uiso 1 2 calc R U P . .
C10 C 0.5379(5) 0.7500 0.4580(4) 0.0131(13) Uani 1 2 d S T P . .
H10 H 0.5012 0.7500 0.4937 0.016 Uiso 1 2 calc R U P . .
C17 C 1.1170(4) 0.7500 1.1350(4) 0.0097(12) Uani 1 2 d S T P . .
H17 H 1.1660 0.7500 1.1956 0.012 Uiso 1 2 calc R U P . .
C18 C 1.0112(5) 0.7500 1.1125(4) 0.0105(12) Uani 1 2 d S TU P . .
C1 C 0.9577(4) 0.7500 0.6254(4) 0.0140(13) Uani 1 2 d S T P . .
H1 H 0.9906 0.7500 0.6889 0.017 Uiso 1 2 calc R U P . .


_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 1.773(3) 4_575 ?
U1 O1 1.773(3) . ?
U1 O4 2.235(4) . ?
U1 O3 2.438(4) . ?
U1 O2 2.438(4) . ?
U1 N2 2.540(5) . ?
U1 N1 2.561(5) . ?
U1 C13 2.813(6) . ?
Br3 C23 1.909(6) . ?
Br2 C18 1.899(6) . ?
Br1 C16 1.890(6) . ?
Br4 C25 1.903(6) . ?
O3 C13 1.267(7) . ?
O4 C20 1.299(7) . ?
O5 C20 1.227(7) . ?
O2 C13 1.271(7) . ?
N2 C10 1.332(7) . ?
N2 C11 1.378(7) . ?
C2 C3 1.361(9) . ?
C2 C1 1.393(8) . ?
C2 H2 0.9300 . ?
N1 C1 1.340(7) . ?
N1 C12 1.366(7) . ?
C19 C18 1.371(8) . ?
C19 C14 1.395(8) . ?
C19 H19 0.9300 . ?
C11 C7 1.400(8) . ?
C11 C12 1.430(8) . ?
C8 C9 1.364(8) . ?
C8 C7 1.404(8) . ?
C8 H8 0.9300 . ?
C3 C4 1.406(8) . ?
C3 H3 0.9300 . ?
C4 C12 1.404(8) . ?
C4 C5 1.426(9) . ?
C20 C21 1.501(8) . ?
C22 C23 1.370(8) . ?
C22 C21 1.397(8) . ?
C22 H22 0.9300 . ?
C7 C6 1.424(8) . ?
C6 C5 1.360(9) . ?
C6 H6 0.9300 . ?
C5 H5 0.9300 . ?
C26 C25 1.369(8) . ?
C26 C21 1.397(8) . ?
C26 H26 0.9300 . ?
C13 C14 1.493(8) . ?
C23 C24 1.395(8) . ?
C16 C17 1.388(8) . ?
C16 C15 1.386(8) . ?
C9 C10 1.396(8) . ?
C9 H9 0.9300 . ?
C15 C14 1.392(8) . ?
C15 H15 0.9300 . ?
C25 C24 1.386(9) . ?
C24 H24 0.9300 . ?
C10 H10 0.9300 . ?
C17 C18 1.389(8) . ?
C17 H17 0.9300 . ?
C1 H1 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
O1 U1 O1 176.57(18) 4_575 . ?
O1 U1 O4 91.30(9) 4_575 . ?
O1 U1 O4 91.30(9) . . ?
O1 U1 O3 91.32(9) 4_575 . ?
O1 U1 O3 91.32(9) . . ?
O4 U1 O3 80.64(14) . . ?
O1 U1 O2 89.90(9) 4_575 . ?
O1 U1 O2 89.90(9) . . ?
O4 U1 O2 134.18(14) . . ?
O3 U1 O2 53.55(13) . . ?
O1 U1 N2 88.99(9) 4_575 . ?
O1 U1 N2 88.99(9) . . ?
O4 U1 N2 85.39(15) . . ?
O3 U1 N2 166.02(14) . . ?
O2 U1 N2 140.43(14) . . ?
O1 U1 N1 88.31(9) 4_575 . ?
O1 U1 N1 88.31(9) . . ?
O4 U1 N1 150.19(16) . . ?
O3 U1 N1 129.18(15) . . ?
O2 U1 N1 75.63(15) . . ?
N2 U1 N1 64.80(16) . . ?
O1 U1 C13 90.68(9) 4_575 . ?
O1 U1 C13 90.68(9) . . ?
O4 U1 C13 107.37(16) . . ?
O3 U1 C13 26.73(15) . . ?
O2 U1 C13 26.82(15) . . ?
N2 U1 C13 167.25(16) . . ?
N1 U1 C13 102.45(17) . . ?
C13 O3 U1 93.4(3) . . ?
C20 O4 U1 173.1(4) . . ?
C13 O2 U1 93.2(3) . . ?
C10 N2 C11 117.6(5) . . ?
C10 N2 U1 123.0(4) . . ?
C11 N2 U1 119.4(4) . . ?
C3 C2 C1 119.1(6) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C1 N1 C12 117.6(5) . . ?
C1 N1 U1 123.3(4) . . ?
C12 N1 U1 119.1(4) . . ?
C18 C19 C14 118.7(5) . . ?
C18 C19 H19 120.7 . . ?
C14 C19 H19 120.7 . . ?
N2 C11 C7 121.8(5) . . ?
N2 C11 C12 118.3(5) . . ?
C7 C11 C12 119.8(5) . . ?
C9 C8 C7 120.4(6) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C2 C3 C4 119.1(6) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C12 C4 C3 118.9(6) . . ?
C12 C4 C5 118.5(5) . . ?
C3 C4 C5 122.6(6) . . ?
O5 C20 O4 123.9(6) . . ?
O5 C20 C21 120.4(5) . . ?
O4 C20 C21 115.8(5) . . ?
C23 C22 C21 119.5(6) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C11 C7 C8 118.0(5) . . ?
C11 C7 C6 119.6(5) . . ?
C8 C7 C6 122.4(6) . . ?
C5 C6 C7 120.2(6) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C6 C5 C4 121.8(6) . . ?
C6 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
C25 C26 C21 119.5(6) . . ?
C25 C26 H26 120.2 . . ?
C21 C26 H26 120.2 . . ?
N1 C12 C4 121.6(5) . . ?
N1 C12 C11 118.4(5) . . ?
C4 C12 C11 120.0(5) . . ?
O3 C13 O2 119.8(5) . . ?
O3 C13 C14 119.6(5) . . ?
O2 C13 C14 120.6(5) . . ?
O3 C13 U1 59.9(3) . . ?
O2 C13 U1 59.9(3) . . ?
C14 C13 U1 179.5(4) . . ?
C22 C23 C24 122.2(6) . . ?
C22 C23 Br3 119.6(5) . . ?
C24 C23 Br3 118.1(5) . . ?
C17 C16 C15 121.7(6) . . ?
C17 C16 Br1 118.3(4) . . ?
C15 C16 Br1 120.0(5) . . ?
C8 C9 C10 118.2(6) . . ?
C8 C9 H9 120.9 . . ?
C10 C9 H9 120.9 . . ?
C16 C15 C14 118.8(6) . . ?
C16 C15 H15 120.6 . . ?
C14 C15 H15 120.6 . . ?
C26 C25 C24 122.5(6) . . ?
C26 C25 Br4 119.5(5) . . ?
C24 C25 Br4 118.0(5) . . ?
C19 C14 C15 120.7(5) . . ?
C19 C14 C13 119.9(5) . . ?
C15 C14 C13 119.3(5) . . ?
C22 C21 C26 119.3(6) . . ?
C22 C21 C20 122.0(5) . . ?
C26 C21 C20 118.7(6) . . ?
C25 C24 C23 117.0(6) . . ?
C25 C24 H24 121.5 . . ?
C23 C24 H24 121.5 . . ?
N2 C10 C9 124.0(6) . . ?
N2 C10 H10 118.0 . . ?
C9 C10 H10 118.0 . . ?
C16 C17 C18 117.7(5) . . ?
C16 C17 H17 121.1 . . ?
C18 C17 H17 121.1 . . ?
C19 C18 C17 122.4(5) . . ?
C19 C18 Br2 119.3(4) . . ?
C17 C18 Br2 118.2(4) . . ?
N1 C1 C2 123.7(6) . . ?
N1 C1 H1 118.1 . . ?
C2 C1 H1 118.1 . . ?

_refine_diff_density_max         0.971
_refine_diff_density_min         -1.135
_refine_diff_density_rms         0.181

_shelxl_version_number           2013-4


_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/m'
_symmetry_int_tables_number      11
_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/. 
# 
# Audit and citation data items have may 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_Compound_4
_database_code_depnum_ccdc_archive 'CCDC 1025742'
_audit_update_record             
;
2014-09-23 deposited with the CCDC.
2014-12-08 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H32 N4 O20 U4'
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1696.69

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   7.576(6)
_cell_length_b                   15.177(6)
_cell_length_c                   16.860(7)
_cell_angle_alpha                90
_cell_angle_beta                 102.094(6)
_cell_angle_gamma                90
_cell_volume                     1895.6(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    40240
_cell_measurement_theta_min      4.942
_cell_measurement_theta_max      56.417
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.973
_exptl_crystal_F_000             1512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    17.121
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.2921
_exptl_absorpt_correction_T_max  0.7457
_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            40240
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_av_R_equivalents  0.0296
_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         1.824
_diffrn_reflns_theta_max         28.364
_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             4742
_reflns_number_gt                4166
_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    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Crystal Maker (Palmer, 2009)'
_computing_publication_material  'WINGX (Farrugia, 2012)'

_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)+(0.0205P)²+1.2508P] 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         4742
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0204
_refine_ls_wR_factor_ref         0.0453
_refine_ls_wR_factor_gt          0.0440
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O4 O 0.1890(4) 0.9272(2) 0.99798(19) 0.0332(7) Uani 1 1 d . . . . .
O1 O 0.4679(4) 1.23900(19) 0.95852(18) 0.0321(7) Uani 1 1 d . . . . .
O3 O 0.3568(4) 1.0549(2) 0.85075(18) 0.0331(7) Uani 1 1 d . . . . .
O2 O 0.2062(4) 1.1919(2) 1.10665(18) 0.0336(7) Uani 1 1 d . . . . .
N2 N 0.1146(5) 1.3169(2) 0.9319(2) 0.0302(8) Uani 1 1 d . . . . .
N1 N 0.3383(5) 1.3817(2) 1.0680(2) 0.0287(8) Uani 1 1 d . . . . .
O5 O 0.1258(4) 1.12124(18) 0.94955(17) 0.0259(6) Uani 1 1 d . . . . .
O6 O 0.4514(3) 1.07440(17) 1.03268(16) 0.0237(6) Uani 1 1 d . . . . .
OW1 O -0.0505(5) 0.9825(3) 0.8481(2) 0.0384(8) Uani 1 1 d . . . . .
O9 O 0.4092(5) 0.7651(2) 0.8629(2) 0.0454(9) Uani 1 1 d . . . . .
O8 O 0.2285(5) 0.8775(2) 0.8296(2) 0.0532(10) Uani 1 1 d . . . . .
C11 C 0.1429(5) 1.4052(3) 0.9377(3) 0.0266(9) Uani 1 1 d . . . . .
OW2 O 0.6962(5) 1.1188(3) 0.8340(2) 0.0586(10) Uani 1 1 d . . . . .
C12 C 0.2582(5) 1.4393(3) 1.0095(3) 0.0271(9) Uani 1 1 d . . . . .
C10 C 0.0054(6) 1.2864(3) 0.8652(3) 0.0381(11) Uani 1 1 d . . . . .
H10 H -0.0157 1.2260 0.8611 0.046 Uiso 1 1 calc R U . . .
C1 C 0.4364(6) 1.4147(3) 1.1358(3) 0.0356(10) Uani 1 1 d . . . . .
H1 H 0.4885 1.3756 1.1765 0.043 Uiso 1 1 calc R U . . .
C3 C 0.3920(7) 1.5622(3) 1.0903(3) 0.0387(11) Uani 1 1 d . . . . .
H3 H 0.4134 1.6223 1.0977 0.046 Uiso 1 1 calc R U . . .
C9 C -0.0788(7) 1.3398(4) 0.8016(3) 0.0427(12) Uani 1 1 d . . . . .
H9 H -0.1541 1.3153 0.7563 0.051 Uiso 1 1 calc R U . . .
C7 C 0.0616(6) 1.4640(3) 0.8756(3) 0.0357(11) Uani 1 1 d . . . . .
C8 C -0.0503(7) 1.4272(4) 0.8062(3) 0.0467(13) Uani 1 1 d . . . . .
H8 H -0.1046 1.4635 0.7635 0.056 Uiso 1 1 calc R U . . .
C2 C 0.4662(7) 1.5043(3) 1.1497(3) 0.0401(12) Uani 1 1 d . . . . .
H2 H 0.5356 1.5243 1.1985 0.048 Uiso 1 1 calc R U . . .
C4 C 0.2839(6) 1.5312(3) 1.0186(3) 0.0336(10) Uani 1 1 d . . . . .
C13 C 0.2736(6) 0.8006(3) 0.8210(3) 0.0281(9) Uani 1 1 d . . . . .
C6 C 0.0911(7) 1.5567(3) 0.8867(3) 0.0457(13) Uani 1 1 d . . . . .
H6 H 0.0356 1.5955 0.8463 0.055 Uiso 1 1 calc R U . . .
C14 C 0.1569(7) 0.7503(3) 0.7536(3) 0.0463(13) Uani 1 1 d . . . . .
H15A H 0.0399 0.7417 0.7658 0.069 Uiso 1 1 calc R U . . .
H15B H 0.2110 0.6941 0.7478 0.069 Uiso 1 1 calc R U . . .
H15C H 0.1448 0.7829 0.7039 0.069 Uiso 1 1 calc R U . . .
C5 C 0.1971(7) 1.5885(3) 0.9540(3) 0.0437(13) Uani 1 1 d . . . . .
H5 H 0.2152 1.6490 0.9593 0.052 Uiso 1 1 calc R U . . .
HW1 H -0.129(7) 1.017(3) 0.852(3) 0.041(16) Uiso 1 1 d . . . . .
HW2 H -0.111(8) 0.936(4) 0.863(4) 0.07(2) Uiso 1 1 d . . . . .
U1 U 0.33813(2) 1.21041(2) 1.03106(2) 0.02141(4) Uani 1 1 d . . . . .
U2 U 0.28151(2) 0.99224(2) 0.92762(2) 0.02033(4) 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
O4 U2 1.794(3) . ?
O1 U1 1.776(3) . ?
O3 U2 1.794(3) . ?
O2 U1 1.799(3) . ?
N2 C10 1.331(6) . ?
N2 C11 1.358(5) . ?
N2 U1 2.662(4) . ?
N1 C1 1.325(5) . ?
N1 C12 1.362(5) . ?
N1 U1 2.673(4) . ?
O5 U1 2.320(3) . ?
O5 U2 2.355(3) . ?
O6 U1 2.233(3) . ?
O6 U2 2.236(3) 3_677 ?
O6 U2 2.322(3) . ?
OW1 U2 2.595(4) . ?
O9 C13 1.242(5) . ?
O9 U1 2.359(3) 3_677 ?
O8 C13 1.234(5) . ?
O8 U2 2.376(3) . ?
C11 C7 1.416(6) . ?
C11 C12 1.432(6) . ?
C12 C4 1.413(6) . ?
C10 C9 1.388(6) . ?
C1 C2 1.391(6) . ?
C3 C2 1.361(7) . ?
C3 C4 1.393(7) . ?
C9 C8 1.344(7) . ?
C7 C8 1.409(7) . ?
C7 C6 1.430(7) . ?
C4 C5 1.439(7) . ?
C13 C14 1.494(6) . ?
C6 C5 1.336(7) . ?
U1 O9 2.359(3) 3_677 ?
U1 U2 3.7251(12) . ?
U2 O6 2.236(3) 3_677 ?
U2 U2 3.686(2) 3_677 ?

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
C10 N2 C11 117.7(4) . . ?
C10 N2 U1 121.4(3) . . ?
C11 N2 U1 118.9(3) . . ?
C1 N1 C12 117.8(4) . . ?
C1 N1 U1 122.8(3) . . ?
C12 N1 U1 118.5(3) . . ?
U1 O5 U2 105.66(11) . . ?
U1 O6 U2 137.99(12) . 3_677 ?
U1 O6 U2 109.69(11) . . ?
U2 O6 U2 107.92(11) 3_677 . ?
C13 O9 U1 143.7(3) . 3_677 ?
C13 O8 U2 139.9(3) . . ?
N2 C11 C7 122.1(4) . . ?
N2 C11 C12 118.5(4) . . ?
C7 C11 C12 119.4(4) . . ?
N1 C12 C4 121.7(4) . . ?
N1 C12 C11 118.7(4) . . ?
C4 C12 C11 119.6(4) . . ?
N2 C10 C9 123.6(5) . . ?
N1 C1 C2 123.8(4) . . ?
C2 C3 C4 119.9(4) . . ?
C8 C9 C10 119.3(5) . . ?
C8 C7 C11 117.2(4) . . ?
C8 C7 C6 123.3(4) . . ?
C11 C7 C6 119.5(4) . . ?
C9 C8 C7 120.1(5) . . ?
C3 C2 C1 118.7(5) . . ?
C3 C4 C12 118.0(4) . . ?
C3 C4 C5 123.0(4) . . ?
C12 C4 C5 118.9(4) . . ?
O8 C13 O9 124.1(4) . . ?
O8 C13 C14 116.0(4) . . ?
O9 C13 C14 119.9(4) . . ?
C5 C6 C7 121.0(4) . . ?
C6 C5 C4 121.5(5) . . ?
O1 U1 O2 174.81(14) . . ?
O1 U1 O6 88.15(12) . . ?
O2 U1 O6 96.66(12) . . ?
O1 U1 O5 98.61(13) . . ?
O2 U1 O5 84.80(13) . . ?
O6 U1 O5 71.64(10) . . ?
O1 U1 O9 90.31(15) . 3_677 ?
O2 U1 O9 88.30(15) . 3_677 ?
O6 U1 O9 83.57(10) . 3_677 ?
O5 U1 O9 153.23(10) . 3_677 ?
O1 U1 N2 77.89(13) . . ?
O2 U1 N2 99.50(14) . . ?
O6 U1 N2 139.52(10) . . ?
O5 U1 N2 73.20(11) . . ?
O9 U1 N2 133.53(11) 3_677 . ?
O1 U1 N1 87.11(13) . . ?
O2 U1 N1 87.71(13) . . ?
O6 U1 N1 156.15(10) . . ?
O5 U1 N1 132.20(10) . . ?
O9 U1 N1 73.10(11) 3_677 . ?
N2 U1 N1 61.67(11) . . ?
O1 U1 U2 85.46(10) . . ?
O2 U1 U2 99.57(10) . . ?
O6 U1 U2 35.94(7) . . ?
O5 U1 U2 37.49(7) . . ?
O9 U1 U2 119.39(8) 3_677 . ?
N2 U1 U2 104.45(8) . . ?
N1 U1 U2 165.45(7) . . ?
O3 U2 O4 175.03(13) . . ?
O3 U2 O6 92.94(12) . 3_677 ?
O4 U2 O6 90.44(12) . 3_677 ?
O3 U2 O6 93.27(13) . . ?
O4 U2 O6 91.24(12) . . ?
O6 U2 O6 72.08(11) 3_677 . ?
O3 U2 O5 85.31(12) . . ?
O4 U2 O5 94.33(13) . . ?
O6 U2 O5 141.35(9) 3_677 . ?
O6 U2 O5 69.48(10) . . ?
O3 U2 O8 85.37(14) . . ?
O4 U2 O8 91.39(15) . . ?
O6 U2 O8 83.53(10) 3_677 . ?
O6 U2 O8 155.49(11) . . ?
O5 U2 O8 134.53(11) . . ?
O3 U2 OW1 94.45(14) . . ?
O4 U2 OW1 80.77(13) . . ?
O6 U2 OW1 147.94(11) 3_677 . ?
O6 U2 OW1 138.32(11) . . ?
O5 U2 OW1 70.44(11) . . ?
O8 U2 OW1 66.08(12) . . ?
O3 U2 U2 93.84(10) . 3_677 ?
O4 U2 U2 91.05(10) . 3_677 ?
O6 U2 U2 36.83(7) 3_677 3_677 ?
O6 U2 U2 35.25(6) . 3_677 ?
O5 U2 U2 104.65(7) . 3_677 ?
O8 U2 U2 120.33(8) . 3_677 ?
OW1 U2 U2 169.95(9) . 3_677 ?
O3 U2 U1 81.03(10) . . ?
O4 U2 U1 101.64(10) . . ?
O6 U2 U1 104.69(7) 3_677 . ?
O6 U2 U1 34.36(6) . . ?
O5 U2 U1 36.84(7) . . ?
O8 U2 U1 164.39(9) . . ?
OW1 U2 U1 107.26(9) . . ?
U2 U2 U1 68.517(13) 3_677 . ?

_refine_diff_density_max         0.909
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.163

_shelxl_version_number           2013-4


_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/. 
# 
# Audit and citation data items have may 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_Compound_5
_database_code_depnum_ccdc_archive 'CCDC 1025743'
_audit_update_record             
;
2014-09-23 deposited with the CCDC.
2014-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H26 Br3 N3 O12 U2'
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1408.39

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                   8.1393(3)
_cell_length_b                   14.2487(4)
_cell_length_c                   17.1933(5)
_cell_angle_alpha                91.870(3)
_cell_angle_beta                 97.985(2)
_cell_angle_gamma                98.728(2)
_cell_volume                     1948.84(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    28493
_cell_measurement_theta_min      5.118
_cell_measurement_theta_max      53.100
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.400
_exptl_crystal_F_000             1296
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    11.441
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4689
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'SADABS, 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            28493
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.448
_diffrn_reflns_theta_max         29.054
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10273
_reflns_number_gt                7497
_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    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Crystal Maker (Palmer, 2009)'
_computing_publication_material  'WINGX (Farrugia, 2012)'

_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)+(0.0311P)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         10273
_refine_ls_number_parameters     505
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0724
_refine_ls_wR_factor_gt          0.0654
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_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
Br1 Br 0.34182(11) 0.34132(6) 0.37677(5) 0.0816(2) Uani 1 1 d . . . . .
Br2 Br -0.12062(10) 0.37335(5) 0.39861(5) 0.0789(2) Uani 1 1 d . . . . .
Br3 Br 0.13863(10) 1.07483(7) 0.45446(6) 0.0939(3) Uani 1 1 d . . . . .
O5 O 0.6977(4) 0.8037(2) 0.16576(19) 0.0314(8) Uani 1 1 d . . . . .
O2 O 0.9524(4) 0.7501(2) 0.0839(2) 0.0397(9) Uani 1 1 d . . . . .
O3 O 0.3306(4) 0.7643(2) 0.1587(2) 0.0429(9) Uani 1 1 d . . . . .
O6 O 0.6904(5) 0.5942(2) 0.1227(2) 0.0435(9) Uani 1 1 d . . . . .
O4 O 0.6272(5) 0.8016(3) 0.3306(2) 0.0504(10) Uani 1 1 d . . . . .
O1 O 0.5198(4) 0.7195(2) 0.0123(2) 0.0392(9) Uani 1 1 d . . . . .
N1 N 0.7802(5) 0.6008(3) -0.0455(2) 0.0350(10) Uani 1 1 d . . . . .
O8 O 0.3152(5) 0.6541(3) 0.3075(3) 0.0567(12) Uani 1 1 d . . . . .
O9 O 0.2329(4) 0.7917(2) 0.3195(2) 0.0414(9) Uani 1 1 d . . . . .
O7 O 0.5579(6) 0.6330(3) 0.2193(3) 0.0649(14) Uani 1 1 d . . . . .
N2 N 0.8264(5) 0.7847(3) -0.0822(2) 0.0306(9) Uani 1 1 d . . . . .
N3 N 0.7459(5) 0.9119(3) 0.0207(3) 0.0349(10) Uani 1 1 d . . . . .
O10 O 0.4901(5) 0.9416(2) 0.2435(2) 0.0442(9) Uani 1 1 d . . . . .
OW1 O 0.9879(5) 0.8951(3) 0.2510(2) 0.0495(10) Uani 1 1 d . . . . .
O11 O 0.7489(6) 1.0223(4) 0.2671(3) 0.0900(18) Uani 1 1 d . . . . .
C17 C 0.5818(6) 0.4736(3) 0.2035(3) 0.0325(11) Uani 1 1 d . . . . .
C16 C 0.6116(6) 0.5735(3) 0.1799(3) 0.0334(11) Uani 1 1 d . . . . .
C31 C 0.5607(7) 1.0539(3) 0.3528(3) 0.0344(12) Uani 1 1 d . . . . .
C32 C 0.3985(7) 1.0421(4) 0.3687(3) 0.0388(13) Uani 1 1 d . . . . .
H32 H 0.3130 1.0042 0.3350 0.047 Uiso 1 1 calc R U . . .
C5 C 0.8584(6) 0.6210(4) -0.1081(3) 0.0342(12) Uani 1 1 d . . . . .
C6 C 0.8789(6) 0.7209(4) -0.1297(3) 0.0360(12) Uani 1 1 d . . . . .
C15 C 0.7002(7) 0.9732(4) 0.0711(3) 0.0438(14) Uani 1 1 d . . . . .
H15 H 0.6698 0.9509 0.1181 0.053 Uiso 1 1 calc R U . . .
C11 C 0.7857(6) 0.9453(4) -0.0482(3) 0.0364(12) Uani 1 1 d . . . . .
C33 C 0.3641(8) 1.0871(4) 0.4352(4) 0.0495(15) Uani 1 1 d . . . . .
C18 C 0.4908(6) 0.4554(4) 0.2670(3) 0.0386(13) Uani 1 1 d . . . . .
H18 H 0.4529 0.5045 0.2928 0.046 Uiso 1 1 calc R U . . .
C10 C 0.8363(6) 0.8762(4) -0.1031(3) 0.0364(12) Uani 1 1 d . . . . .
C13 C 0.7335(8) 1.0994(4) -0.0136(4) 0.0524(16) Uani 1 1 d . . . . .
H13 H 0.7273 1.1621 -0.0255 0.063 Uiso 1 1 calc R U . . .
C23 C 0.2111(7) 0.7025(4) 0.3286(3) 0.0418(13) Uani 1 1 d . . . . .
C1 C 0.7489(7) 0.5099(4) -0.0278(3) 0.0415(13) Uani 1 1 d . . . . .
H1 H 0.6906 0.4952 0.0141 0.050 Uiso 1 1 calc R U . . .
C24 C 0.0654(7) 0.6531(4) 0.3631(3) 0.0426(13) Uani 1 1 d . . . . .
C7 C 0.9410(8) 0.7484(5) -0.1982(4) 0.0524(16) Uani 1 1 d . . . . .
H7 H 0.9771 0.7036 -0.2297 0.063 Uiso 1 1 calc R U . . .
C19 C 0.4594(7) 0.3640(4) 0.2901(4) 0.0485(15) Uani 1 1 d . . . . .
C3 C 0.8856(7) 0.4578(4) -0.1299(4) 0.0492(15) Uani 1 1 d . . . . .
H3 H 0.9254 0.4104 -0.1568 0.059 Uiso 1 1 calc R U . . .
C2 C 0.7985(7) 0.4364(4) -0.0686(4) 0.0491(15) Uani 1 1 d . . . . .
H2 H 0.7732 0.3739 -0.0546 0.059 Uiso 1 1 calc R U . . .
C4 C 0.9133(7) 0.5499(4) -0.1511(4) 0.0499(15) Uani 1 1 d . . . . .
H4 H 0.9685 0.5652 -0.1939 0.060 Uiso 1 1 calc R U . . .
C29 C -0.0498(7) 0.7030(4) 0.3909(4) 0.0523(16) Uani 1 1 d . . . . .
H29 H -0.0372 0.7689 0.3891 0.063 Uiso 1 1 calc R U . . .
C30 C 0.6057(8) 1.0042(4) 0.2829(4) 0.0470(15) Uani 1 1 d . . . . .
C12 C 0.7802(7) 1.0387(4) -0.0664(4) 0.0498(15) Uani 1 1 d . . . . .
H12 H 0.8081 1.0600 -0.1141 0.060 Uiso 1 1 calc R U . . .
C36 C 0.6871(7) 1.1107(4) 0.4038(4) 0.0489(15) Uani 1 1 d . . . . .
H36 H 0.7968 1.1204 0.3927 0.059 Uiso 1 1 calc R U . . .
C14 C 0.6959(8) 1.0673(4) 0.0571(4) 0.0516(16) Uani 1 1 d . . . . .
H14 H 0.6680 1.1082 0.0947 0.062 Uiso 1 1 calc R U . . .
C22 C 0.6338(7) 0.3991(4) 0.1658(4) 0.0474(15) Uani 1 1 d . . . . .
H22 H 0.6930 0.4105 0.1237 0.057 Uiso 1 1 calc R U . . .
C21 C 0.5989(8) 0.3071(4) 0.1901(4) 0.0551(17) Uani 1 1 d . . . . .
H21 H 0.6351 0.2575 0.1641 0.066 Uiso 1 1 calc R U . . .
C34 C 0.4870(9) 1.1420(5) 0.4869(4) 0.0594(17) Uani 1 1 d . . . . .
H34 H 0.4615 1.1714 0.5319 0.071 Uiso 1 1 calc R U . . .
C25 C 0.0461(8) 0.5554(4) 0.3664(3) 0.0500(15) Uani 1 1 d . . . . .
H25 H 0.1239 0.5216 0.3485 0.060 Uiso 1 1 calc R U . . .
C26 C -0.0910(8) 0.5085(4) 0.3967(4) 0.0515(16) Uani 1 1 d . . . . .
C9 C 0.8938(8) 0.9048(5) -0.1723(4) 0.0580(17) Uani 1 1 d . . . . .
H9 H 0.8948 0.9672 -0.1866 0.070 Uiso 1 1 calc R U . . .
C20 C 0.5110(8) 0.2890(4) 0.2523(4) 0.0595(18) Uani 1 1 d . . . . .
H20 H 0.4869 0.2275 0.2686 0.071 Uiso 1 1 calc R U . . .
C28 C -0.1850(8) 0.6530(5) 0.4215(4) 0.0639(19) Uani 1 1 d . . . . .
H28 H -0.2624 0.6864 0.4403 0.077 Uiso 1 1 calc R U . . .
C27 C -0.2071(8) 0.5553(5) 0.4246(4) 0.0616(19) Uani 1 1 d . . . . .
H27 H -0.2978 0.5225 0.4450 0.074 Uiso 1 1 calc R U . . .
C35 C 0.6493(9) 1.1524(5) 0.4706(4) 0.067(2) Uani 1 1 d . . . . .
H35 H 0.7350 1.1884 0.5055 0.080 Uiso 1 1 calc R U . . .
C8 C 0.9498(9) 0.8396(5) -0.2199(4) 0.0646(19) Uani 1 1 d . . . . .
H8 H 0.9923 0.8579 -0.2655 0.078 Uiso 1 1 calc R U . . .
U2 U 0.47919(2) 0.78109(2) 0.24468(2) 0.03006(6) Uani 1 1 d . . . . .
U1 U 0.73523(2) 0.73508(2) 0.05087(2) 0.02777(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C19 1.891(6) . ?
Br2 C26 1.907(6) . ?
Br3 C33 1.893(6) . ?
O5 U1 2.255(3) . ?
O5 U2 2.374(3) . ?
O2 U1 1.758(3) . ?
O3 U2 1.760(4) . ?
O6 C16 1.266(6) . ?
O6 U1 2.398(3) . ?
O4 U2 1.758(4) . ?
O1 U1 1.765(3) . ?
N1 C1 1.335(6) . ?
N1 C5 1.341(6) . ?
N1 U1 2.592(4) . ?
O8 C23 1.253(6) . ?
O8 U2 2.453(4) . ?
O9 C23 1.274(6) . ?
O9 U2 2.548(3) . ?
O7 C16 1.235(6) . ?
O7 U2 2.341(4) . ?
N2 C10 1.356(6) . ?
N2 C6 1.358(6) . ?
N2 U1 2.590(4) . ?
N3 C15 1.337(7) . ?
N3 C11 1.354(6) . ?
N3 U1 2.580(4) . ?
O10 C30 1.292(6) . ?
O10 U2 2.276(3) . ?
O11 C30 1.225(7) . ?
C17 C22 1.376(7) . ?
C17 C18 1.411(7) . ?
C17 C16 1.487(7) . ?
C31 C32 1.372(7) . ?
C31 C36 1.391(7) . ?
C31 C30 1.491(7) . ?
C32 C33 1.375(8) . ?
C32 H32 0.9300 . ?
C5 C4 1.397(7) . ?
C5 C6 1.474(7) . ?
C6 C7 1.390(7) . ?
C15 C14 1.375(7) . ?
C15 H15 0.9300 . ?
C11 C12 1.383(7) . ?
C11 C10 1.483(7) . ?
C33 C34 1.369(8) . ?
C18 C19 1.371(7) . ?
C18 H18 0.9300 . ?
C10 C9 1.389(7) . ?
C13 C12 1.364(8) . ?
C13 C14 1.370(8) . ?
C13 H13 0.9300 . ?
C23 C24 1.491(7) . ?
C23 U2 2.887(5) . ?
C1 C2 1.381(7) . ?
C1 H1 0.9300 . ?
C24 C25 1.380(8) . ?
C24 C29 1.385(8) . ?
C7 C8 1.357(9) . ?
C7 H7 0.9300 . ?
C19 C20 1.380(8) . ?
C3 C2 1.367(8) . ?
C3 C4 1.368(8) . ?
C3 H3 0.9300 . ?
C2 H2 0.9300 . ?
C4 H4 0.9300 . ?
C29 C28 1.394(8) . ?
C29 H29 0.9300 . ?
C12 H12 0.9300 . ?
C36 C35 1.368(8) . ?
C36 H36 0.9300 . ?
C14 H14 0.9300 . ?
C22 C21 1.388(8) . ?
C22 H22 0.9300 . ?
C21 C20 1.378(9) . ?
C21 H21 0.9300 . ?
C34 C35 1.376(9) . ?
C34 H34 0.9300 . ?
C25 C26 1.387(8) . ?
C25 H25 0.9300 . ?
C26 C27 1.365(9) . ?
C9 C8 1.386(9) . ?
C9 H9 0.9300 . ?
C20 H20 0.9300 . ?
C28 C27 1.381(9) . ?
C28 H28 0.9300 . ?
C27 H27 0.9300 . ?
C35 H35 0.9300 . ?
C8 H8 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
U1 O5 U2 133.45(14) . . ?
C16 O6 U1 132.9(3) . . ?
C1 N1 C5 117.9(4) . . ?
C1 N1 U1 120.5(3) . . ?
C5 N1 U1 120.9(3) . . ?
C23 O8 U2 97.0(3) . . ?
C23 O9 U2 91.9(3) . . ?
C16 O7 U2 154.8(4) . . ?
C10 N2 C6 118.4(4) . . ?
C10 N2 U1 121.1(3) . . ?
C6 N2 U1 120.2(3) . . ?
C15 N3 C11 117.3(4) . . ?
C15 N3 U1 120.6(3) . . ?
C11 N3 U1 122.0(3) . . ?
C30 O10 U2 125.7(4) . . ?
C22 C17 C18 119.2(5) . . ?
C22 C17 C16 123.7(5) . . ?
C18 C17 C16 117.1(4) . . ?
O7 C16 O6 123.2(5) . . ?
O7 C16 C17 116.6(5) . . ?
O6 C16 C17 120.1(4) . . ?
C32 C31 C36 119.7(5) . . ?
C32 C31 C30 121.2(5) . . ?
C36 C31 C30 119.0(5) . . ?
C31 C32 C33 119.1(5) . . ?
C31 C32 H32 120.5 . . ?
C33 C32 H32 120.5 . . ?
N1 C5 C4 121.2(5) . . ?
N1 C5 C6 116.5(4) . . ?
C4 C5 C6 122.3(5) . . ?
N2 C6 C7 120.9(5) . . ?
N2 C6 C5 117.4(4) . . ?
C7 C6 C5 121.6(5) . . ?
N3 C15 C14 123.5(5) . . ?
N3 C15 H15 118.2 . . ?
C14 C15 H15 118.2 . . ?
N3 C11 C12 121.8(5) . . ?
N3 C11 C10 116.3(4) . . ?
C12 C11 C10 121.8(5) . . ?
C34 C33 C32 122.2(6) . . ?
C34 C33 Br3 118.9(5) . . ?
C32 C33 Br3 118.9(5) . . ?
C19 C18 C17 118.8(5) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
N2 C10 C9 121.7(5) . . ?
N2 C10 C11 117.3(4) . . ?
C9 C10 C11 121.0(5) . . ?
C12 C13 C14 119.5(5) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
O8 C23 O9 119.1(5) . . ?
O8 C23 C24 118.6(5) . . ?
O9 C23 C24 122.4(5) . . ?
O8 C23 U2 57.5(3) . . ?
O9 C23 U2 61.9(3) . . ?
C24 C23 U2 172.7(4) . . ?
N1 C1 C2 123.5(5) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C25 C24 C29 120.1(5) . . ?
C25 C24 C23 118.5(5) . . ?
C29 C24 C23 121.4(5) . . ?
C8 C7 C6 121.0(6) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C18 C19 C20 122.2(6) . . ?
C18 C19 Br1 118.2(5) . . ?
C20 C19 Br1 119.6(5) . . ?
C2 C3 C4 119.1(5) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C3 C2 C1 118.4(6) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C3 C4 C5 119.7(5) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C24 C29 C28 119.0(6) . . ?
C24 C29 H29 120.5 . . ?
C28 C29 H29 120.5 . . ?
O11 C30 O10 123.6(5) . . ?
O11 C30 C31 119.3(5) . . ?
O10 C30 C31 117.1(5) . . ?
C13 C12 C11 119.4(6) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C35 C36 C31 119.7(5) . . ?
C35 C36 H36 120.2 . . ?
C31 C36 H36 120.2 . . ?
C13 C14 C15 118.4(6) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
C17 C22 C21 120.7(6) . . ?
C17 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C20 C21 C22 120.3(6) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C33 C34 C35 118.0(6) . . ?
C33 C34 H34 121.0 . . ?
C35 C34 H34 121.0 . . ?
C24 C25 C26 119.0(6) . . ?
C24 C25 H25 120.5 . . ?
C26 C25 H25 120.5 . . ?
C27 C26 C25 122.6(6) . . ?
C27 C26 Br2 118.5(5) . . ?
C25 C26 Br2 118.9(5) . . ?
C8 C9 C10 119.5(6) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C21 C20 C19 118.8(6) . . ?
C21 C20 H20 120.6 . . ?
C19 C20 H20 120.6 . . ?
C27 C28 C29 121.7(6) . . ?
C27 C28 H28 119.1 . . ?
C29 C28 H28 119.1 . . ?
C26 C27 C28 117.7(6) . . ?
C26 C27 H27 121.2 . . ?
C28 C27 H27 121.2 . . ?
C36 C35 C34 121.3(6) . . ?
C36 C35 H35 119.4 . . ?
C34 C35 H35 119.4 . . ?
C7 C8 C9 118.4(6) . . ?
C7 C8 H8 120.8 . . ?
C9 C8 H8 120.8 . . ?
O4 U2 O3 178.24(17) . . ?
O4 U2 O10 87.16(16) . . ?
O3 U2 O10 91.10(15) . . ?
O4 U2 O7 91.19(18) . . ?
O3 U2 O7 90.49(17) . . ?
O10 U2 O7 157.29(14) . . ?
O4 U2 O5 90.64(15) . . ?
O3 U2 O5 89.42(14) . . ?
O10 U2 O5 85.51(12) . . ?
O7 U2 O5 71.86(12) . . ?
O4 U2 O8 89.73(17) . . ?
O3 U2 O8 91.35(16) . . ?
O10 U2 O8 134.16(13) . . ?
O7 U2 O8 68.42(13) . . ?
O5 U2 O8 140.28(11) . . ?
O4 U2 O9 92.98(15) . . ?
O3 U2 O9 86.61(14) . . ?
O10 U2 O9 82.89(12) . . ?
O7 U2 O9 119.81(12) . . ?
O5 U2 O9 167.66(11) . . ?
O8 U2 O9 51.61(12) . . ?
O4 U2 C23 93.12(17) . . ?
O3 U2 C23 87.27(16) . . ?
O10 U2 C23 109.05(15) . . ?
O7 U2 C23 93.65(15) . . ?
O5 U2 C23 165.12(14) . . ?
O8 U2 C23 25.52(14) . . ?
O9 U2 C23 26.18(13) . . ?
O2 U1 O1 176.79(16) . . ?
O2 U1 O5 89.34(14) . . ?
O1 U1 O5 93.67(14) . . ?
O2 U1 O6 90.93(15) . . ?
O1 U1 O6 90.65(15) . . ?
O5 U1 O6 81.57(12) . . ?
O2 U1 N3 92.56(15) . . ?
O1 U1 N3 87.01(15) . . ?
O5 U1 N3 76.83(12) . . ?
O6 U1 N3 158.07(13) . . ?
O2 U1 N2 84.25(15) . . ?
O1 U1 N2 92.72(14) . . ?
O5 U1 N2 139.00(12) . . ?
O6 U1 N2 138.80(12) . . ?
N3 U1 N2 63.12(13) . . ?
O2 U1 N1 87.20(15) . . ?
O1 U1 N1 90.46(14) . . ?
O5 U1 N1 157.39(13) . . ?
O6 U1 N1 76.16(13) . . ?
N3 U1 N1 125.63(13) . . ?
N2 U1 N1 62.78(13) . . ?

_refine_diff_density_max         1.068
_refine_diff_density_min         -1.346
_refine_diff_density_rms         0.148

_shelxl_version_number           2013-4


_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_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/. 
# 
# Audit and citation data items have may 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_Compound_6
_database_code_depnum_ccdc_archive 'CCDC 1025744'
_audit_update_record             
;
2014-09-23 deposited with the CCDC.
2014-12-08 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H19 Br2 N3 O6 U'
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         903.32

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                   8.7005(4)
_cell_length_b                   10.3737(5)
_cell_length_c                   16.6960(8)
_cell_angle_alpha                107.848(4)
_cell_angle_beta                 95.093(4)
_cell_angle_gamma                95.359(3)
_cell_volume                     1417.13(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    19497
_cell_measurement_theta_min      4.739
_cell_measurement_theta_max      51.546
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.117
_exptl_crystal_F_000             848
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    8.595
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5736
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS, 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            19497
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.291
_diffrn_reflns_theta_max         28.019
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6817
_reflns_number_gt                5657
_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    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Crystal Maker (Palmer, 2009)'
_computing_publication_material  'WINGX (Farrugia, 2012)'

_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)+(0.0350P)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         6817
_refine_ls_number_parameters     370
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0695
_refine_ls_wR_factor_gt          0.0652
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.76321(7) 0.80459(6) 0.42431(3) 0.07292(17) Uani 1 1 d . . . . .
Br2 Br 0.22895(10) 0.44685(9) 0.35311(4) 0.1128(3) Uani 1 1 d . . . . .
O1 O 0.0832(4) 1.1828(3) 0.74864(19) 0.0509(8) Uani 1 1 d . . . . .
O2 O 0.3004(4) 1.0839(3) 0.90391(19) 0.0503(8) Uani 1 1 d . . . . .
O5 O 0.1547(4) 0.9093(3) 0.7330(2) 0.0557(8) Uani 1 1 d . . . . .
O3 O 0.4097(4) 1.1447(3) 0.7627(2) 0.0575(9) Uani 1 1 d . . . . .
N2 N 0.0772(4) 1.2682(4) 0.9563(2) 0.0420(8) Uani 1 1 d . . . . .
N1 N 0.2871(4) 1.3844(4) 0.8857(2) 0.0441(8) Uani 1 1 d . . . . .
N3 N -0.0713(4) 1.0281(4) 0.8526(2) 0.0439(8) Uani 1 1 d . . . . .
C20 C 0.6969(5) 0.9105(5) 0.5263(3) 0.0469(11) Uani 1 1 d . . . . .
C23 C 0.2163(5) 0.7968(5) 0.7237(3) 0.0492(11) Uani 1 1 d . . . . .
O6 O 0.2765(5) 0.7645(4) 0.7819(2) 0.0781(11) Uani 1 1 d . . . . .
C17 C 0.5993(5) 1.0753(5) 0.6712(3) 0.0415(10) Uani 1 1 d . . . . .
C24 C 0.2119(5) 0.7089(4) 0.6331(3) 0.0446(10) Uani 1 1 d . . . . .
C18 C 0.5028(5) 0.9630(4) 0.6185(3) 0.0460(11) Uani 1 1 d . . . . .
H18 H 0.4036 0.9431 0.6317 0.055 Uiso 1 1 calc R U . . .
O4 O 0.6444(4) 1.2594(5) 0.7986(2) 0.0950(15) Uani 1 1 d . . . . .
C25 C 0.1285(6) 0.7360(5) 0.5677(3) 0.0564(12) Uani 1 1 d . . . . .
H25 H 0.0689 0.8078 0.5798 0.068 Uiso 1 1 calc R U . . .
C16 C 0.5523(6) 1.1677(5) 0.7504(3) 0.0525(12) Uani 1 1 d . . . . .
C27 C 0.2184(6) 0.5520(5) 0.4672(3) 0.0606(13) Uani 1 1 d . . . . .
C29 C 0.2962(7) 0.5989(5) 0.6144(3) 0.0634(14) Uani 1 1 d . . . . .
H29 H 0.3499 0.5769 0.6581 0.076 Uiso 1 1 calc R U . . .
C26 C 0.1312(6) 0.6583(5) 0.4837(3) 0.0661(15) Uani 1 1 d . . . . .
H26 H 0.0752 0.6781 0.4398 0.079 Uiso 1 1 calc R U . . .
C21 C 0.7958(5) 1.0208(5) 0.5780(3) 0.0574(13) Uani 1 1 d . . . . .
H21 H 0.8952 1.0396 0.5647 0.069 Uiso 1 1 calc R U . . .
C19 C 0.5513(6) 0.8796(5) 0.5463(3) 0.0509(11) Uani 1 1 d . . . . .
H19 H 0.4860 0.8031 0.5115 0.061 Uiso 1 1 calc R U . . .
C22 C 0.7466(5) 1.1031(5) 0.6496(3) 0.0542(12) Uani 1 1 d . . . . .
H22 H 0.8129 1.1789 0.6844 0.065 Uiso 1 1 calc R U . . .
C10 C -0.0304(5) 1.2026(5) 0.9887(3) 0.0477(11) Uani 1 1 d . . . . .
C11 C -0.1272(5) 1.0818(4) 0.9271(3) 0.0446(10) Uani 1 1 d . . . . .
C5 C 0.2658(5) 1.4575(4) 0.9655(3) 0.0451(10) Uani 1 1 d . . . . .
C6 C 0.1580(5) 1.3876(5) 1.0068(3) 0.0454(10) Uani 1 1 d . . . . .
C1 C 0.3731(6) 1.4463(5) 0.8422(3) 0.0541(12) Uani 1 1 d . . . . .
H1 H 0.3857 1.3972 0.7869 0.065 Uiso 1 1 calc R U . . .
C15 C -0.1611(5) 0.9275(5) 0.7915(3) 0.0521(12) Uani 1 1 d . . . . .
H15 H -0.1232 0.8902 0.7401 0.062 Uiso 1 1 calc R U . . .
C4 C 0.3374(6) 1.5901(5) 1.0032(3) 0.0552(13) Uani 1 1 d . . . . .
H4 H 0.3237 1.6382 1.0586 0.066 Uiso 1 1 calc R U . . .
C14 C -0.3086(6) 0.8768(5) 0.8020(4) 0.0586(13) Uani 1 1 d . . . . .
H14 H -0.3685 0.8077 0.7580 0.070 Uiso 1 1 calc R U . . .
C2 C 0.4446(6) 1.5802(5) 0.8756(4) 0.0606(13) Uani 1 1 d . . . . .
H2 H 0.5013 1.6211 0.8433 0.073 Uiso 1 1 calc R U . . .
C12 C -0.2721(6) 1.0319(5) 0.9412(4) 0.0584(13) Uani 1 1 d . . . . .
H12 H -0.3071 1.0674 0.9937 0.070 Uiso 1 1 calc R U . . .
C3 C 0.4284(6) 1.6499(5) 0.9584(4) 0.0636(14) Uani 1 1 d . . . . .
H3 H 0.4795 1.7379 0.9839 0.076 Uiso 1 1 calc R U . . .
C7 C 0.1365(6) 1.4410(6) 1.0922(3) 0.0627(14) Uani 1 1 d . . . . .
H7 H 0.1933 1.5228 1.1265 0.075 Uiso 1 1 calc R U . . .
C9 C -0.0553(6) 1.2513(6) 1.0732(3) 0.0614(14) Uani 1 1 d . . . . .
H9 H -0.1284 1.2039 1.0947 0.074 Uiso 1 1 calc R U . . .
C28 C 0.3009(7) 0.5217(5) 0.5313(4) 0.0690(15) Uani 1 1 d . . . . .
H28 H 0.3599 0.4494 0.5189 0.083 Uiso 1 1 calc R U . . .
C8 C 0.0302(6) 1.3707(7) 1.1244(3) 0.0698(16) Uani 1 1 d . . . . .
H8 H 0.0159 1.4040 1.1813 0.084 Uiso 1 1 calc R U . . .
C13 C -0.3649(6) 0.9290(5) 0.8771(4) 0.0670(15) Uani 1 1 d . . . . .
H13 H -0.4636 0.8964 0.8853 0.080 Uiso 1 1 calc R U . . .
U1 U 0.19323(2) 1.12858(2) 0.82315(2) 0.03802(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C20 1.894(4) . ?
Br2 C27 1.898(5) . ?
O1 U1 1.760(3) . ?
O2 U1 1.773(3) . ?
O5 C23 1.301(6) . ?
O5 U1 2.285(3) . ?
O3 C16 1.288(5) . ?
O3 U1 2.230(3) . ?
N2 C10 1.353(6) . ?
N2 C6 1.353(6) . ?
N2 U1 2.600(3) . ?
N1 C1 1.338(6) . ?
N1 C5 1.355(5) . ?
N1 U1 2.558(4) . ?
N3 C11 1.353(5) . ?
N3 C15 1.340(6) . ?
N3 U1 2.587(3) . ?
C20 C21 1.369(7) . ?
C20 C19 1.372(6) . ?
C23 O6 1.213(6) . ?
C23 C24 1.503(6) . ?
C17 C18 1.377(6) . ?
C17 C22 1.390(6) . ?
C17 C16 1.492(6) . ?
C24 C25 1.372(6) . ?
C24 C29 1.384(6) . ?
C18 C19 1.377(6) . ?
C18 H18 0.9300 . ?
O4 C16 1.212(6) . ?
C25 C26 1.390(7) . ?
C25 H25 0.9300 . ?
C27 C26 1.370(7) . ?
C27 C28 1.367(7) . ?
C29 C28 1.380(7) . ?
C29 H29 0.9300 . ?
C26 H26 0.9300 . ?
C21 C22 1.369(6) . ?
C21 H21 0.9300 . ?
C19 H19 0.9300 . ?
C22 H22 0.9300 . ?
C10 C9 1.389(6) . ?
C10 C11 1.482(7) . ?
C11 C12 1.385(6) . ?
C5 C4 1.384(6) . ?
C5 C6 1.476(7) . ?
C6 C7 1.399(6) . ?
C1 C2 1.389(7) . ?
C1 H1 0.9300 . ?
C15 C14 1.387(7) . ?
C15 H15 0.9300 . ?
C4 C3 1.367(7) . ?
C4 H4 0.9300 . ?
C14 C13 1.360(7) . ?
C14 H14 0.9300 . ?
C2 C3 1.376(7) . ?
C2 H2 0.9300 . ?
C12 C13 1.387(7) . ?
C12 H12 0.9300 . ?
C3 H3 0.9300 . ?
C7 C8 1.372(8) . ?
C7 H7 0.9300 . ?
C9 C8 1.372(8) . ?
C9 H9 0.9300 . ?
C28 H28 0.9300 . ?
C8 H8 0.9300 . ?
C13 H13 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
C23 O5 U1 137.9(3) . . ?
C16 O3 U1 163.4(3) . . ?
C10 N2 C6 118.9(4) . . ?
C10 N2 U1 118.6(3) . . ?
C6 N2 U1 118.9(3) . . ?
C1 N1 C5 118.1(4) . . ?
C1 N1 U1 119.6(3) . . ?
C5 N1 U1 122.0(3) . . ?
C11 N3 C15 118.5(4) . . ?
C11 N3 U1 121.2(3) . . ?
C15 N3 U1 120.2(3) . . ?
C21 C20 C19 121.0(4) . . ?
C21 C20 Br1 118.3(3) . . ?
C19 C20 Br1 120.6(4) . . ?
O6 C23 O5 124.2(5) . . ?
O6 C23 C24 121.4(4) . . ?
O5 C23 C24 114.4(4) . . ?
C18 C17 C22 118.4(4) . . ?
C18 C17 C16 122.7(4) . . ?
C22 C17 C16 118.9(4) . . ?
C25 C24 C29 118.7(4) . . ?
C25 C24 C23 121.8(4) . . ?
C29 C24 C23 119.5(4) . . ?
C19 C18 C17 120.9(4) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C24 C25 C26 121.5(5) . . ?
C24 C25 H25 119.2 . . ?
C26 C25 H25 119.2 . . ?
O4 C16 O3 123.2(4) . . ?
O4 C16 C17 120.8(4) . . ?
O3 C16 C17 116.0(4) . . ?
C26 C27 C28 121.3(5) . . ?
C26 C27 Br2 119.4(4) . . ?
C28 C27 Br2 119.2(4) . . ?
C28 C29 C24 120.4(5) . . ?
C28 C29 H29 119.8 . . ?
C24 C29 H29 119.8 . . ?
C27 C26 C25 118.4(5) . . ?
C27 C26 H26 120.8 . . ?
C25 C26 H26 120.8 . . ?
C22 C21 C20 119.2(4) . . ?
C22 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?
C20 C19 C18 119.4(4) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C21 C22 C17 121.2(4) . . ?
C21 C22 H22 119.4 . . ?
C17 C22 H22 119.4 . . ?
N2 C10 C9 121.8(5) . . ?
N2 C10 C11 115.7(4) . . ?
C9 C10 C11 122.4(5) . . ?
N3 C11 C12 121.1(4) . . ?
N3 C11 C10 116.0(4) . . ?
C12 C11 C10 122.7(4) . . ?
N1 C5 C4 121.4(4) . . ?
N1 C5 C6 115.3(4) . . ?
C4 C5 C6 123.3(4) . . ?
N2 C6 C7 121.3(5) . . ?
N2 C6 C5 115.7(4) . . ?
C7 C6 C5 122.9(5) . . ?
N1 C1 C2 123.3(5) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
N3 C15 C14 122.4(5) . . ?
N3 C15 H15 118.8 . . ?
C14 C15 H15 118.8 . . ?
C3 C4 C5 119.4(5) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C13 C14 C15 119.5(5) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C3 C2 C1 117.6(5) . . ?
C3 C2 H2 121.2 . . ?
C1 C2 H2 121.2 . . ?
C11 C12 C13 119.9(5) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C4 C3 C2 120.2(5) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C8 C7 C6 118.8(5) . . ?
C8 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
C8 C9 C10 118.8(5) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
C27 C28 C29 119.7(5) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C7 C8 C9 120.4(5) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C14 C13 C12 118.6(5) . . ?
C14 C13 H13 120.7 . . ?
C12 C13 H13 120.7 . . ?
O1 U1 O2 175.92(13) . . ?
O1 U1 O3 92.60(14) . . ?
O2 U1 O3 89.56(13) . . ?
O1 U1 O5 90.64(13) . . ?
O2 U1 O5 93.03(13) . . ?
O3 U1 O5 84.28(12) . . ?
O1 U1 N1 82.12(13) . . ?
O2 U1 N1 94.91(13) . . ?
O3 U1 N1 78.72(12) . . ?
O5 U1 N1 161.15(12) . . ?
O1 U1 N3 85.71(13) . . ?
O2 U1 N3 93.44(13) . . ?
O3 U1 N3 159.99(12) . . ?
O5 U1 N3 75.81(11) . . ?
N1 U1 N3 120.63(11) . . ?
O1 U1 N2 96.97(13) . . ?
O2 U1 N2 79.12(12) . . ?
O3 U1 N2 137.43(12) . . ?
O5 U1 N2 136.69(12) . . ?
N1 U1 N2 61.84(11) . . ?
N3 U1 N2 62.45(11) . . ?

_refine_diff_density_max         1.023
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.105

_shelxl_version_number           2013-4


_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_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/. 
# 
# Audit and citation data items have may 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_Compound_7
_database_code_depnum_ccdc_archive 'CCDC 1025745'
_audit_update_record             
;
2014-09-23 deposited with the CCDC.
2014-12-08 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H17 Br4 N3 O6 U'
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow

_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         1061.12

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      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                   13.8471(10)
_cell_length_b                   17.0590(12)
_cell_length_c                   14.0709(10)
_cell_angle_alpha                90
_cell_angle_beta                 115.4880(10)
_cell_angle_gamma                90
_cell_volume                     3000.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    42515
_cell_measurement_theta_min      5.753
_cell_measurement_theta_max      55.047
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.349
_exptl_crystal_F_000             1968
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    10.785
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5489
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS, 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            41727
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.629
_diffrn_reflns_theta_max         28.398
_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             7528
_reflns_number_gt                6091
_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    'Crystal Maker (Palmer, 2009)'
_computing_publication_material  'WINGX (Farrugia, 2012)'

_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)+(0.0200P)²+1.6661P] 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         7528
_refine_ls_number_parameters     388
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0273
_refine_ls_wR_factor_ref         0.0538
_refine_ls_wR_factor_gt          0.0495
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_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 0.90687(2) 0.12840(2) 0.21065(2) 0.00840(4) Uani 1 1 d . . . . .
Br1 Br 0.35831(3) 0.07021(2) -0.07641(3) 0.01850(9) Uani 1 1 d . . . . .
Br2 Br 0.37746(3) 0.40150(2) -0.05902(3) 0.02128(10) Uani 1 1 d . . . . .
Br4 Br 0.30539(4) 0.28360(3) 0.15460(3) 0.02619(11) Uani 1 1 d . . . . .
Br3 Br 0.45543(4) -0.02829(3) 0.23358(4) 0.02876(11) Uani 1 1 d . . . . .
O2 O 0.9612(2) 0.22437(15) 0.2339(2) 0.0133(6) Uani 1 1 d . . . . .
O1 O 0.8617(2) 0.02975(15) 0.1877(2) 0.0142(6) Uani 1 1 d . . . . .
O4 O 0.7672(2) 0.28693(15) 0.0025(2) 0.0145(6) Uani 1 1 d . . . . .
O3 O 0.7706(2) 0.16243(15) 0.0552(2) 0.0119(6) Uani 1 1 d . . . . .
N3 N 0.9963(3) 0.11286(17) 0.0860(2) 0.0100(7) Uani 1 1 d . . . . .
N2 N 1.0883(2) 0.05457(17) 0.2823(2) 0.0091(6) Uani 1 1 d . . . . .
O5 O 0.7818(2) 0.15567(17) 0.2696(2) 0.0184(6) Uani 1 1 d . . . . .
N1 N 1.0039(3) 0.10686(17) 0.4111(2) 0.0109(7) Uani 1 1 d . . . . .
C22 C 0.5534(3) 0.3018(2) -0.0247(3) 0.0111(8) Uani 1 1 d . . . . .
H22 H 0.5908 0.3483 -0.0180 0.013 Uiso 1 1 calc R U . . .
O6 O 0.7379(2) 0.28182(17) 0.2750(2) 0.0216(7) Uani 1 1 d . . . . .
C5 C 1.0912(3) 0.0602(2) 0.4541(3) 0.0091(8) Uani 1 1 d . . . . .
C12 C 1.1320(3) 0.0581(2) 0.0427(3) 0.0127(8) Uani 1 1 d . . . . .
H12 H 1.1894 0.0240 0.0591 0.015 Uiso 1 1 calc R U . . .
C10 C 1.1222(3) 0.0253(2) 0.2128(3) 0.0099(8) Uani 1 1 d . . . . .
C6 C 1.1255(3) 0.0220(2) 0.3795(3) 0.0114(8) Uani 1 1 d . . . . .
C13 C 1.0934(3) 0.1020(2) -0.0494(3) 0.0136(8) Uani 1 1 d . . . . .
H13 H 1.1265 0.0988 -0.0944 0.016 Uiso 1 1 calc R U . . .
C16 C 0.7237(3) 0.2288(2) 0.0162(3) 0.0112(8) Uani 1 1 d . . . . .
C14 C 1.0063(3) 0.1502(2) -0.0739(3) 0.0142(8) Uani 1 1 d . . . . .
H14 H 0.9794 0.1798 -0.1354 0.017 Uiso 1 1 calc R U . . .
C1 C 0.9716(3) 0.1445(2) 0.4763(3) 0.0141(8) Uani 1 1 d . . . . .
H1 H 0.9113 0.1762 0.4471 0.017 Uiso 1 1 calc R U . . .
C3 C 1.1132(3) 0.0907(2) 0.6291(3) 0.0153(9) Uani 1 1 d . . . . .
H3 H 1.1499 0.0855 0.7018 0.018 Uiso 1 1 calc R U . . .
C7 C 1.1918(3) -0.0433(2) 0.4070(3) 0.0142(8) Uani 1 1 d . . . . .
H7 H 1.2155 -0.0654 0.4737 0.017 Uiso 1 1 calc R U . . .
C23 C 0.7162(3) 0.2119(2) 0.2648(3) 0.0144(8) Uani 1 1 d . . . . .
C11 C 1.0824(3) 0.0664(2) 0.1099(3) 0.0101(8) Uani 1 1 d . . . . .
C8 C 1.2220(3) -0.0750(2) 0.3334(3) 0.0148(8) Uani 1 1 d . . . . .
H8 H 1.2640 -0.1199 0.3492 0.018 Uiso 1 1 calc R U . . .
C18 C 0.5476(3) 0.1605(2) -0.0241(3) 0.0107(8) Uani 1 1 d . . . . .
H18 H 0.5817 0.1122 -0.0143 0.013 Uiso 1 1 calc R U . . .
C19 C 0.4393(3) 0.1644(2) -0.0506(3) 0.0125(8) Uani 1 1 d . . . . .
C24 C 0.6047(3) 0.1845(2) 0.2423(3) 0.0107(8) Uani 1 1 d . . . . .
C9 C 1.1894(3) -0.0394(2) 0.2362(3) 0.0130(8) Uani 1 1 d . . . . .
H9 H 1.2121 -0.0585 0.1873 0.016 Uiso 1 1 calc R U . . .
C20 C 0.3870(3) 0.2351(2) -0.0619(3) 0.0138(8) Uani 1 1 d . . . . .
H20 H 0.3143 0.2368 -0.0787 0.017 Uiso 1 1 calc R U . . .
C15 C 0.9598(3) 0.1535(2) -0.0045(3) 0.0131(8) Uani 1 1 d . . . . .
H15 H 0.9003 0.1854 -0.0213 0.016 Uiso 1 1 calc R U . . .
C29 C 0.5219(3) 0.2382(2) 0.2163(3) 0.0137(8) Uani 1 1 d . . . . .
H29 H 0.5347 0.2915 0.2134 0.016 Uiso 1 1 calc R U . . .
C4 C 1.1467(3) 0.0512(2) 0.5626(3) 0.0134(8) Uani 1 1 d . . . . .
H4 H 1.2063 0.0187 0.5905 0.016 Uiso 1 1 calc R U . . .
C27 C 0.3997(3) 0.1332(2) 0.2006(3) 0.0176(9) Uani 1 1 d . . . . .
H27 H 0.3313 0.1160 0.1871 0.021 Uiso 1 1 calc R U . . .
C21 C 0.4456(3) 0.3033(2) -0.0474(3) 0.0118(8) Uani 1 1 d . . . . .
C28 C 0.4204(3) 0.2119(2) 0.1948(3) 0.0149(9) Uani 1 1 d . . . . .
C25 C 0.5852(3) 0.1046(2) 0.2469(3) 0.0135(8) Uani 1 1 d . . . . .
H25 H 0.6401 0.0682 0.2630 0.016 Uiso 1 1 calc R U . . .
C2 C 1.0238(3) 0.1382(2) 0.5846(3) 0.0154(9) Uani 1 1 d . . . . .
H2 H 0.9992 0.1655 0.6270 0.019 Uiso 1 1 calc R U . . .
C17 C 0.6052(3) 0.2296(2) -0.0121(3) 0.0099(8) Uani 1 1 d . . . . .
C26 C 0.4834(3) 0.0805(2) 0.2270(3) 0.0168(9) 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 O2 1.772(3) . ?
U1 O1 1.776(3) . ?
U1 O3 2.265(3) . ?
U1 O5 2.268(3) . ?
U1 N3 2.560(3) . ?
U1 N1 2.576(3) . ?
U1 N2 2.595(3) . ?
Br1 C19 1.902(4) . ?
Br2 C21 1.895(4) . ?
Br4 C28 1.891(4) . ?
Br3 C26 1.907(4) . ?
O4 C16 1.218(4) . ?
O3 C16 1.303(4) . ?
N3 C11 1.348(5) . ?
N3 C15 1.342(5) . ?
N2 C10 1.350(5) . ?
N2 C6 1.356(5) . ?
O5 C23 1.302(5) . ?
N1 C1 1.344(5) . ?
N1 C5 1.353(5) . ?
C22 C21 1.385(5) . ?
C22 C17 1.396(5) . ?
C22 H22 0.9300 . ?
O6 C23 1.224(5) . ?
C5 C4 1.391(5) . ?
C5 C6 1.478(5) . ?
C12 C13 1.389(5) . ?
C12 C11 1.394(5) . ?
C12 H12 0.9300 . ?
C10 C9 1.389(5) . ?
C10 C11 1.485(5) . ?
C6 C7 1.388(5) . ?
C13 C14 1.376(5) . ?
C13 H13 0.9300 . ?
C16 C17 1.514(5) . ?
C14 C15 1.384(5) . ?
C14 H14 0.9300 . ?
C1 C2 1.381(5) . ?
C1 H1 0.9300 . ?
C3 C4 1.385(5) . ?
C3 C2 1.383(6) . ?
C3 H3 0.9300 . ?
C7 C8 1.383(5) . ?
C7 H7 0.9300 . ?
C23 C24 1.511(5) . ?
C8 C9 1.381(5) . ?
C8 H8 0.9300 . ?
C18 C19 1.382(5) . ?
C18 C17 1.392(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.381(5) . ?
C24 C29 1.388(5) . ?
C24 C25 1.396(5) . ?
C9 H9 0.9300 . ?
C20 C21 1.384(5) . ?
C20 H20 0.9300 . ?
C15 H15 0.9300 . ?
C29 C28 1.378(5) . ?
C29 H29 0.9300 . ?
C4 H4 0.9300 . ?
C27 C28 1.384(6) . ?
C27 C26 1.385(6) . ?
C27 H27 0.9300 . ?
C25 C26 1.376(6) . ?
C25 H25 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
O2 U1 O1 175.71(12) . . ?
O2 U1 O3 93.02(11) . . ?
O1 U1 O3 89.15(11) . . ?
O2 U1 O5 94.18(11) . . ?
O1 U1 O5 89.80(11) . . ?
O3 U1 O5 81.42(9) . . ?
O2 U1 N3 86.02(11) . . ?
O1 U1 N3 90.76(11) . . ?
O3 U1 N3 79.18(10) . . ?
O5 U1 N3 160.58(10) . . ?
O2 U1 N1 87.09(11) . . ?
O1 U1 N1 92.36(11) . . ?
O3 U1 N1 156.85(9) . . ?
O5 U1 N1 75.49(10) . . ?
N3 U1 N1 123.87(10) . . ?
O2 U1 N2 96.53(11) . . ?
O1 U1 N2 79.46(11) . . ?
O3 U1 N2 139.86(9) . . ?
O5 U1 N2 136.18(10) . . ?
N3 U1 N2 62.81(10) . . ?
N1 U1 N2 62.84(10) . . ?
C16 O3 U1 133.4(2) . . ?
C11 N3 C15 118.1(3) . . ?
C11 N3 U1 121.8(2) . . ?
C15 N3 U1 120.0(2) . . ?
C10 N2 C6 118.6(3) . . ?
C10 N2 U1 118.6(2) . . ?
C6 N2 U1 118.4(2) . . ?
C23 O5 U1 139.2(2) . . ?
C1 N1 C5 118.1(3) . . ?
C1 N1 U1 120.6(3) . . ?
C5 N1 U1 121.2(2) . . ?
C21 C22 C17 119.3(3) . . ?
C21 C22 H22 120.4 . . ?
C17 C22 H22 120.4 . . ?
N1 C5 C4 121.4(3) . . ?
N1 C5 C6 116.2(3) . . ?
C4 C5 C6 122.4(3) . . ?
C13 C12 C11 118.3(4) . . ?
C13 C12 H12 120.9 . . ?
C11 C12 H12 120.9 . . ?
N2 C10 C9 121.9(3) . . ?
N2 C10 C11 115.7(3) . . ?
C9 C10 C11 122.4(3) . . ?
N2 C6 C7 122.0(3) . . ?
N2 C6 C5 115.9(3) . . ?
C7 C6 C5 122.2(3) . . ?
C14 C13 C12 120.0(4) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
O4 C16 O3 125.7(4) . . ?
O4 C16 C17 120.3(3) . . ?
O3 C16 C17 114.0(3) . . ?
C13 C14 C15 118.1(4) . . ?
C13 C14 H14 121.0 . . ?
C15 C14 H14 121.0 . . ?
N1 C1 C2 123.1(4) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C4 C3 C2 118.3(4) . . ?
C4 C3 H3 120.9 . . ?
C2 C3 H3 120.9 . . ?
C8 C7 C6 118.8(4) . . ?
C8 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
O6 C23 O5 125.5(4) . . ?
O6 C23 C24 120.3(4) . . ?
O5 C23 C24 114.2(3) . . ?
N3 C11 C12 122.1(3) . . ?
N3 C11 C10 116.0(3) . . ?
C12 C11 C10 121.9(3) . . ?
C9 C8 C7 119.6(4) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C19 C18 C17 119.4(4) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C20 C19 C18 121.8(4) . . ?
C20 C19 Br1 118.6(3) . . ?
C18 C19 Br1 119.6(3) . . ?
C29 C24 C25 120.2(4) . . ?
C29 C24 C23 120.3(3) . . ?
C25 C24 C23 119.5(3) . . ?
C8 C9 C10 118.9(4) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C21 C20 C19 118.2(4) . . ?
C21 C20 H20 120.9 . . ?
C19 C20 H20 120.9 . . ?
N3 C15 C14 123.3(4) . . ?
N3 C15 H15 118.3 . . ?
C14 C15 H15 118.3 . . ?
C24 C29 C28 119.4(4) . . ?
C24 C29 H29 120.3 . . ?
C28 C29 H29 120.3 . . ?
C3 C4 C5 120.0(4) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C28 C27 C26 118.3(4) . . ?
C28 C27 H27 120.8 . . ?
C26 C27 H27 120.8 . . ?
C20 C21 C22 121.6(3) . . ?
C20 C21 Br2 119.5(3) . . ?
C22 C21 Br2 118.9(3) . . ?
C27 C28 C29 121.4(4) . . ?
C27 C28 Br4 118.4(3) . . ?
C29 C28 Br4 120.2(3) . . ?
C26 C25 C24 118.9(4) . . ?
C26 C25 H25 120.6 . . ?
C24 C25 H25 120.6 . . ?
C1 C2 C3 119.1(4) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C18 C17 C22 119.7(3) . . ?
C18 C17 C16 121.6(3) . . ?
C22 C17 C16 118.8(3) . . ?
C25 C26 C27 121.8(4) . . ?
C25 C26 Br3 119.5(3) . . ?
C27 C26 Br3 118.7(3) . . ?

_refine_diff_density_max         1.045
_refine_diff_density_min         -1.160
_refine_diff_density_rms         0.161

_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/. 
# 
# Audit and citation data items have may 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_Compound_8
_database_code_depnum_ccdc_archive 'CCDC 1025746'
_audit_update_record             
;
2014-09-23 deposited with the CCDC.
2014-12-08 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H26 Br3 N3 O12 U2'
_chemical_melting_point          ?

_exptl_crystal_description       Rod
_exptl_crystal_colour            Yellow

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1408.39

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      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                   20.6384(9)
_cell_length_b                   7.4578(3)
_cell_length_c                   26.5728(12)
_cell_angle_alpha                90
_cell_angle_beta                 105.647(6)
_cell_angle_gamma                90
_cell_volume                     3938.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    39751
_cell_measurement_theta_min      4.661
_cell_measurement_theta_max      45.326
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.375
_exptl_crystal_F_000             2592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    11.322
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5074
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS, 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            38110
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.115
_diffrn_reflns_theta_max         27.603
_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             9133
_reflns_number_gt                6727
_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-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Crystal Maker (Palmer, 2009)'
_computing_publication_material  'WINGX (Farrugia, 2012)'

_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)+(0.0626P)²+4.1171P] 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         9133
_refine_ls_number_parameters     505
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.1350
_refine_ls_wR_factor_gt          0.1195
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_restrained_S_all      1.762
_refine_ls_shift/su_max          0.020
_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 0.84493(2) 0.19599(4) 0.37096(2) 0.02733(10) Uani 1 1 d . . . . .
U2 U 0.71453(2) 0.15389(5) 0.46747(2) 0.03162(11) Uani 1 1 d . . . . .
Br1 Br 0.40545(7) -0.0021(2) 0.18444(7) 0.0870(5) Uani 1 1 d . . . . .
Br2 Br 0.51071(8) -0.6474(2) 0.61792(6) 0.0757(4) Uani 1 1 d . . . . .
Br3 Br 0.66128(16) 0.5654(7) 0.74698(12) 0.2246(13) Uani 1 1 d . U . . .
O1 O 0.8442(3) -0.0327(9) 0.3891(3) 0.0427(17) Uani 1 1 d . . . . .
C25 C 0.5975(5) -0.3847(13) 0.5170(4) 0.040(2) Uani 1 1 d . . . . .
H25 H 0.6162 -0.4165 0.4901 0.048 Uiso 1 1 calc R U . . .
O3 O 0.7785(4) -0.0011(9) 0.4932(3) 0.0481(18) Uani 1 1 d . . . . .
C26 C 0.5731(5) -0.5134(15) 0.5428(4) 0.044(3) Uani 1 1 d . . . . .
H26 H 0.5757 -0.6332 0.5339 0.053 Uiso 1 1 calc R U . . .
O2 O 0.8504(3) 0.4199(9) 0.3517(2) 0.0367(15) Uani 1 1 d . . . . .
O4 O 0.6503(4) 0.3100(10) 0.4403(3) 0.053(2) Uani 1 1 d . . . . .
O6 O 0.7318(3) 0.1525(9) 0.3195(2) 0.0376(16) Uani 1 1 d . . . . .
O7 O 0.6942(3) 0.0262(9) 0.3824(2) 0.0377(16) Uani 1 1 d . . . . .
N2 N 0.9655(4) 0.1317(10) 0.3646(3) 0.0322(18) Uani 1 1 d . . . . .
O9 O 0.6539(4) 0.0700(10) 0.5316(3) 0.053(2) Uani 1 1 d . . . . .
C18 C 0.6081(5) 0.0912(15) 0.2464(4) 0.041(2) Uani 1 1 d . . . . .
H18 H 0.6442 0.1237 0.2337 0.049 Uiso 1 1 calc R U . . .
O8 O 0.6359(4) -0.0943(10) 0.4605(3) 0.052(2) Uani 1 1 d . . . . .
N1 N 0.9406(4) 0.2399(10) 0.4543(3) 0.0327(18) Uani 1 1 d . . . . .
O10 O 0.7651(4) 0.3375(11) 0.5344(3) 0.059(2) Uani 1 1 d . . . . .
C32 C 0.7279(6) 0.361(2) 0.6265(5) 0.069(4) Uani 1 1 d . . . . .
H32 H 0.7285 0.2488 0.6111 0.083 Uiso 1 1 calc R U . . .
C1 C 0.9268(6) 0.3022(14) 0.4984(4) 0.044(3) Uani 1 1 d . . . . .
H1 H 0.8825 0.3289 0.4975 0.053 Uiso 1 1 calc R U . . .
C27 C 0.5449(5) -0.4687(15) 0.5818(4) 0.044(3) Uani 1 1 d . . . . .
C17 C 0.6174(5) 0.0595(13) 0.2993(4) 0.034(2) Uani 1 1 d . . . . .
C16 C 0.6859(5) 0.0831(13) 0.3363(4) 0.033(2) Uani 1 1 d . . . . .
C8 C 1.0892(6) -0.0009(19) 0.3611(6) 0.072(4) Uani 1 1 d . . . . .
H8 H 1.1308 -0.0470 0.3605 0.087 Uiso 1 1 calc R U . . .
O11 O 0.8043(6) 0.6121(14) 0.5444(4) 0.092(4) Uani 1 1 d . . . . .
N3 N 0.8572(4) 0.1187(13) 0.2796(3) 0.043(2) Uani 1 1 d . . . . .
C22 C 0.5642(5) 0.0125(14) 0.3185(4) 0.045(3) Uani 1 1 d . . . . .
H22 H 0.5709 -0.0089 0.3540 0.053 Uiso 1 1 calc R U . . .
C23 C 0.6292(5) -0.0708(14) 0.5061(4) 0.043(2) Uani 1 1 d . . . . .
C11 C 0.9186(5) 0.0754(13) 0.2723(4) 0.037(2) Uani 1 1 d . . . . .
C24 C 0.5946(5) -0.2055(15) 0.5304(4) 0.045(3) Uani 1 1 d . . . . .
C35 C 0.7159(9) 0.679(3) 0.6720(7) 0.102(6) Uani 1 1 d . U . . .
H35 H 0.7099 0.7885 0.6870 0.123 Uiso 1 1 calc R U . . .
C9 C 1.0368(6) -0.0030(16) 0.3170(5) 0.059(3) Uani 1 1 d . . . . .
H9 H 1.0423 -0.0511 0.2861 0.071 Uiso 1 1 calc R U . . .
C30 C 0.7756(6) 0.4888(16) 0.5586(4) 0.050(3) Uani 1 1 d . . . . .
C5 C 1.0052(5) 0.2002(12) 0.4567(4) 0.035(2) Uani 1 1 d . . . . .
C19 C 0.5439(5) 0.0737(17) 0.2126(4) 0.052(3) Uani 1 1 d . . . . .
H19 H 0.5368 0.0942 0.1770 0.063 Uiso 1 1 calc R U . . .
C31 C 0.7504(6) 0.5040(18) 0.6060(4) 0.053(3) Uani 1 1 d . . . . .
C10 C 0.9749(5) 0.0682(14) 0.3189(4) 0.041(2) Uani 1 1 d . . . . .
C6 C 1.0184(5) 0.1324(12) 0.4069(4) 0.036(2) Uani 1 1 d . . . . .
C15 C 0.8047(6) 0.1319(19) 0.2380(4) 0.059(4) Uani 1 1 d . . . . .
H15 H 0.7632 0.1616 0.2431 0.071 Uiso 1 1 calc R U . . .
C21 C 0.5000(5) -0.0026(16) 0.2839(5) 0.055(3) Uani 1 1 d . . . . .
H21 H 0.4633 -0.0322 0.2963 0.066 Uiso 1 1 calc R U . . .
C12 C 0.9238(6) 0.0462(16) 0.2218(4) 0.055(3) Uani 1 1 d . . . . .
H12 H 0.9651 0.0151 0.2165 0.066 Uiso 1 1 calc R U . . .
C3 C 1.0414(6) 0.2862(14) 0.5455(5) 0.051(3) Uani 1 1 d . . . . .
H3 H 1.0755 0.3021 0.5762 0.061 Uiso 1 1 calc R U . . .
C14 C 0.8083(6) 0.1040(17) 0.1875(4) 0.056(3) Uani 1 1 d . . . . .
H14 H 0.7701 0.1133 0.1594 0.067 Uiso 1 1 calc R U . . .
C2 C 0.9765(6) 0.3269(14) 0.5444(4) 0.047(3) Uani 1 1 d . . . . .
H2 H 0.9660 0.3704 0.5740 0.057 Uiso 1 1 calc R U . . .
C4 C 1.0566(6) 0.2227(14) 0.5021(4) 0.046(3) Uani 1 1 d . . . . .
H4 H 1.1008 0.1949 0.5028 0.055 Uiso 1 1 calc R U . . .
C28 C 0.5378(7) -0.2942(16) 0.5950(5) 0.061(4) Uani 1 1 d . . . . .
H28 H 0.5157 -0.2658 0.6202 0.074 Uiso 1 1 calc R U . . .
C20 C 0.4917(5) 0.0266(16) 0.2318(5) 0.053(3) Uani 1 1 d . . . . .
C29 C 0.5648(7) -0.1578(17) 0.5698(5) 0.063(4) Uani 1 1 d . . . . .
H29 H 0.5627 -0.0383 0.5792 0.076 Uiso 1 1 calc R U . . .
C36 C 0.7452(7) 0.671(2) 0.6266(7) 0.098(6) Uani 1 1 d . . . . .
H36 H 0.7593 0.7742 0.6129 0.118 Uiso 1 1 calc R U . . .
C13 C 0.8683(7) 0.0633(18) 0.1800(5) 0.062(4) Uani 1 1 d . . . . .
H13 H 0.8723 0.0465 0.1462 0.074 Uiso 1 1 calc R U . . .
C7 C 1.0805(5) 0.0684(15) 0.4061(5) 0.050(3) Uani 1 1 d . . . . .
H7 H 1.1163 0.0726 0.4361 0.060 Uiso 1 1 calc R U . . .
C33 C 0.7032(8) 0.377(3) 0.6713(6) 0.097(5) Uani 1 1 d . . . . .
H33 H 0.6903 0.2754 0.6866 0.116 Uiso 1 1 calc R U . . .
C34 C 0.6990(10) 0.531(3) 0.6900(8) 0.107(6) Uani 1 1 d . U . . .
O5 O 0.7877(3) 0.2983(8) 0.4257(2) 0.0322(15) Uani 1 1 d . . . . .
OW1 O 0.7778(5) 0.6477(10) 0.4384(3) 0.071(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 O2 1.759(7) . ?
U1 O1 1.774(7) . ?
U1 O5 2.241(6) . ?
U1 O6 2.388(6) . ?
U1 N1 2.561(8) . ?
U1 N3 2.575(8) . ?
U1 N2 2.583(8) . ?
U2 O3 1.749(7) . ?
U2 O4 1.766(7) . ?
U2 O10 2.263(7) . ?
U2 O5 2.361(6) . ?
U2 O7 2.383(6) . ?
U2 O8 2.435(7) . ?
U2 O9 2.451(7) . ?
U2 C23 2.818(11) . ?
Br1 C20 1.896(11) . ?
Br2 C27 1.887(11) . ?
Br3 C34 1.90(2) . ?
C25 C26 1.354(14) . ?
C25 C24 1.389(15) . ?
C26 C27 1.359(14) . ?
O6 C16 1.260(11) . ?
O7 C16 1.265(11) . ?
N2 C6 1.340(12) . ?
N2 C10 1.366(12) . ?
O9 C23 1.279(12) . ?
C18 C17 1.387(13) . ?
C18 C19 1.392(14) . ?
O8 C23 1.267(12) . ?
N1 C5 1.350(12) . ?
N1 C1 1.359(13) . ?
O10 C30 1.288(13) . ?
C32 C31 1.338(18) . ?
C32 C33 1.422(19) . ?
C1 C2 1.379(14) . ?
C27 C28 1.367(16) . ?
C17 C22 1.374(13) . ?
C17 C16 1.498(13) . ?
C8 C7 1.357(17) . ?
C8 C9 1.364(17) . ?
O11 C30 1.210(14) . ?
N3 C15 1.327(13) . ?
N3 C11 1.370(12) . ?
C22 C21 1.398(14) . ?
C23 C24 1.478(14) . ?
C11 C12 1.392(14) . ?
C11 C10 1.454(14) . ?
C24 C29 1.395(15) . ?
C35 C34 1.29(2) . ?
C35 C36 1.49(2) . ?
C9 C10 1.397(14) . ?
C30 C31 1.490(16) . ?
C5 C4 1.384(14) . ?
C5 C6 1.508(14) . ?
C19 C20 1.356(16) . ?
C31 C36 1.379(18) . ?
C6 C7 1.373(14) . ?
C15 C14 1.379(15) . ?
C21 C20 1.366(16) . ?
C12 C13 1.370(17) . ?
C3 C4 1.361(16) . ?
C3 C2 1.366(16) . ?
C14 C13 1.342(17) . ?
C28 C29 1.414(16) . ?
C33 C34 1.26(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U1 O1 176.3(3) . . ?
O2 U1 O5 87.3(3) . . ?
O1 U1 O5 96.1(3) . . ?
O2 U1 O6 95.3(3) . . ?
O1 U1 O6 86.9(3) . . ?
O5 U1 O6 79.2(2) . . ?
O2 U1 N1 92.0(3) . . ?
O1 U1 N1 87.1(3) . . ?
O5 U1 N1 79.2(2) . . ?
O6 U1 N1 156.8(2) . . ?
O2 U1 N3 84.7(3) . . ?
O1 U1 N3 92.9(3) . . ?
O5 U1 N3 153.2(3) . . ?
O6 U1 N3 76.1(2) . . ?
N1 U1 N3 126.6(3) . . ?
O2 U1 N2 91.1(3) . . ?
O1 U1 N2 85.3(3) . . ?
O5 U1 N2 142.3(2) . . ?
O6 U1 N2 138.4(2) . . ?
N1 U1 N2 63.2(2) . . ?
N3 U1 N2 63.6(3) . . ?
O3 U2 O4 178.9(3) . . ?
O3 U2 O10 87.4(3) . . ?
O4 U2 O10 93.3(4) . . ?
O3 U2 O5 88.5(3) . . ?
O4 U2 O5 90.7(3) . . ?
O10 U2 O5 82.8(2) . . ?
O3 U2 O7 91.6(3) . . ?
O4 U2 O7 87.5(3) . . ?
O10 U2 O7 155.8(3) . . ?
O5 U2 O7 73.0(2) . . ?
O3 U2 O8 86.8(3) . . ?
O4 U2 O8 93.4(3) . . ?
O10 U2 O8 132.5(3) . . ?
O5 U2 O8 144.0(2) . . ?
O7 U2 O8 71.4(2) . . ?
O3 U2 O9 91.9(3) . . ?
O4 U2 O9 89.1(3) . . ?
O10 U2 O9 79.8(3) . . ?
O5 U2 O9 162.5(2) . . ?
O7 U2 O9 124.4(2) . . ?
O8 U2 O9 53.4(2) . . ?
O3 U2 C23 86.8(3) . . ?
O4 U2 C23 93.8(3) . . ?
O10 U2 C23 105.9(3) . . ?
O5 U2 C23 169.8(3) . . ?
O7 U2 C23 98.1(3) . . ?
O8 U2 C23 26.7(3) . . ?
O9 U2 C23 27.0(3) . . ?
C26 C25 C24 120.3(10) . . ?
C25 C26 C27 120.5(10) . . ?
C16 O6 U1 124.4(6) . . ?
C16 O7 U2 136.7(6) . . ?
C6 N2 C10 117.9(8) . . ?
C6 N2 U1 121.8(6) . . ?
C10 N2 U1 119.6(6) . . ?
C23 O9 U2 92.7(6) . . ?
C17 C18 C19 119.1(10) . . ?
C23 O8 U2 93.7(6) . . ?
C5 N1 C1 117.9(8) . . ?
C5 N1 U1 122.3(6) . . ?
C1 N1 U1 119.8(6) . . ?
C30 O10 U2 154.5(8) . . ?
C31 C32 C33 121.1(16) . . ?
N1 C1 C2 122.0(11) . . ?
C26 C27 C28 121.8(10) . . ?
C26 C27 Br2 120.7(9) . . ?
C28 C27 Br2 117.4(8) . . ?
C22 C17 C18 120.8(9) . . ?
C22 C17 C16 119.6(9) . . ?
C18 C17 C16 119.5(9) . . ?
O6 C16 O7 124.1(8) . . ?
O6 C16 C17 118.9(8) . . ?
O7 C16 C17 116.9(8) . . ?
C7 C8 C9 119.9(11) . . ?
C15 N3 C11 118.6(9) . . ?
C15 N3 U1 120.2(7) . . ?
C11 N3 U1 121.0(6) . . ?
C17 C22 C21 119.2(10) . . ?
O8 C23 O9 119.2(10) . . ?
O8 C23 C24 120.9(10) . . ?
O9 C23 C24 119.9(9) . . ?
O8 C23 U2 59.6(5) . . ?
O9 C23 U2 60.3(5) . . ?
C24 C23 U2 170.6(8) . . ?
N3 C11 C12 119.2(10) . . ?
N3 C11 C10 116.5(9) . . ?
C12 C11 C10 124.3(10) . . ?
C25 C24 C29 119.8(10) . . ?
C25 C24 C23 118.8(10) . . ?
C29 C24 C23 121.1(11) . . ?
C34 C35 C36 118.3(16) . . ?
C8 C9 C10 119.0(11) . . ?
O11 C30 O10 122.7(11) . . ?
O11 C30 C31 121.2(11) . . ?
O10 C30 C31 116.1(11) . . ?
N1 C5 C4 121.9(10) . . ?
N1 C5 C6 116.2(8) . . ?
C4 C5 C6 121.9(9) . . ?
C20 C19 C18 119.7(11) . . ?
C32 C31 C36 119.2(14) . . ?
C32 C31 C30 121.4(12) . . ?
C36 C31 C30 119.2(14) . . ?
N2 C10 C9 121.1(10) . . ?
N2 C10 C11 118.2(9) . . ?
C9 C10 C11 120.8(10) . . ?
N2 C6 C7 122.5(10) . . ?
N2 C6 C5 116.0(8) . . ?
C7 C6 C5 121.4(10) . . ?
N3 C15 C14 123.6(12) . . ?
C20 C21 C22 119.3(11) . . ?
C13 C12 C11 120.1(11) . . ?
C4 C3 C2 120.5(10) . . ?
C13 C14 C15 118.2(12) . . ?
C1 C2 C3 118.7(11) . . ?
C3 C4 C5 118.9(11) . . ?
C27 C28 C29 118.7(11) . . ?
C19 C20 C21 121.9(10) . . ?
C19 C20 Br1 118.5(9) . . ?
C21 C20 Br1 119.6(9) . . ?
C24 C29 C28 118.8(12) . . ?
C31 C36 C35 116.8(17) . . ?
C14 C13 C12 120.2(11) . . ?
C8 C7 C6 119.5(11) . . ?
C34 C33 C32 119(2) . . ?
C33 C34 C35 125(2) . . ?
C33 C34 Br3 121.6(17) . . ?
C35 C34 Br3 112.8(17) . . ?
U1 O5 U2 131.7(3) . . ?

_refine_diff_density_max         4.462
_refine_diff_density_min         -2.757
_refine_diff_density_rms         0.234

_shelxl_version_number           2013-4


_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/. 
# 
# Audit and citation data items have may 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_Compound_9
_database_code_depnum_ccdc_archive 'CCDC 1025747'
_audit_update_record             
;
2014-09-23 deposited with the CCDC.
2014-12-08 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H23 Br3 Cl N3 O11 U2'
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1424.81

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'
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      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                   20.7772(8)
_cell_length_b                   7.9807(3)
_cell_length_c                   25.7089(10)
_cell_angle_alpha                90
_cell_angle_beta                 110.9250(10)
_cell_angle_gamma                90
_cell_volume                     3981.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    53197
_cell_measurement_theta_min      4.762
_cell_measurement_theta_max      52.653
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.377
_exptl_crystal_F_000             2616
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    11.263
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5983
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS, 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            51145
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.567
_diffrn_reflns_theta_max         27.671
_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             9289
_reflns_number_gt                7254
_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-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Crystal Maker (Palmer, 2009)'
_computing_publication_material  'WINGX (Farrugia, 2012)'

_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)+(0.0284P)²+7.0277P] 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         9289
_refine_ls_number_parameters     505
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0300
_refine_ls_wR_factor_ref         0.0664
_refine_ls_wR_factor_gt          0.0607
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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 0.33674(2) 0.66260(2) 0.33892(2) 0.03010(5) Uani 1 1 d . . . . .
U2 U 0.21913(2) 0.57305(2) 0.44352(2) 0.03331(6) Uani 1 1 d . . . . .
Br3 Br 0.21226(5) 0.82162(14) 0.69599(4) 0.1042(3) Uani 1 1 d . . . . .
Br1 Br -0.08444(4) 0.38011(12) 0.27058(4) 0.0912(3) Uani 1 1 d . . . . .
Br2 Br 0.03221(5) 0.21156(14) 0.63519(4) 0.1075(3) Uani 1 1 d . . . . .
Cl1 Cl 0.64132(8) 0.4200(3) 0.29667(8) 0.0774(6) Uani 1 1 d . . . . .
O1 O 0.33824(17) 0.4442(4) 0.34972(14) 0.0382(8) Uani 1 1 d . . . . .
O3 O 0.27248(18) 0.3943(5) 0.46086(14) 0.0422(9) Uani 1 1 d . . . . .
O5 O 0.29819(17) 0.7143(4) 0.40916(14) 0.0390(8) Uani 1 1 d . . . . .
O8 O 0.11576(19) 0.4031(5) 0.42465(16) 0.0498(10) Uani 1 1 d . . . . .
O7 O 0.18442(17) 0.5095(5) 0.34834(14) 0.0400(8) Uani 1 1 d . . . . .
O6 O 0.21432(17) 0.6591(5) 0.28825(14) 0.0412(9) Uani 1 1 d . . . . .
N3 N 0.3289(2) 0.6235(5) 0.23746(17) 0.0330(9) Uani 1 1 d . . . . .
O9 O 0.16654(19) 0.4877(5) 0.51021(15) 0.0445(9) Uani 1 1 d . . . . .
O11 O 0.3154(2) 0.9597(5) 0.49124(18) 0.0623(12) Uani 1 1 d . . . . .
O4 O 0.16709(19) 0.7529(5) 0.42718(16) 0.0494(10) Uani 1 1 d . . . . .
N2 N 0.4514(2) 0.6106(5) 0.32210(16) 0.0339(9) Uani 1 1 d . . . . .
C11 C 0.3843(3) 0.5837(6) 0.2241(2) 0.0341(11) Uani 1 1 d . . . . .
O10 O 0.2918(2) 0.7123(5) 0.52106(15) 0.0478(9) Uani 1 1 d . . . . .
O2 O 0.3413(2) 0.8790(5) 0.32825(17) 0.0495(10) Uani 1 1 d . . . . .
N1 N 0.4504(2) 0.6919(7) 0.42304(19) 0.0516(13) Uani 1 1 d . . . . .
C24 C 0.0619(3) 0.3304(6) 0.4897(2) 0.0395(12) Uani 1 1 d . . . . .
C4 C 0.5715(3) 0.6690(11) 0.4656(3) 0.078(2) Uani 1 1 d . . . . .
H4 H 0.6134 0.6397 0.4627 0.094 Uiso 1 1 calc R U . . .
C3 C 0.5695(4) 0.7254(13) 0.5151(3) 0.092(3) Uani 1 1 d . . . . .
H3 H 0.6098 0.7383 0.5458 0.110 Uiso 1 1 calc R U . . .
C5 C 0.5114(3) 0.6555(8) 0.4201(2) 0.0468(14) Uani 1 1 d . . . . .
C8 C 0.5690(3) 0.4956(9) 0.3068(3) 0.0532(15) Uani 1 1 d . . . . .
C17 C 0.0973(2) 0.5754(6) 0.2634(2) 0.0347(11) Uani 1 1 d . . . . .
C10 C 0.4503(2) 0.5656(6) 0.2710(2) 0.0361(12) Uani 1 1 d . . . . .
C16 C 0.1703(2) 0.5834(7) 0.3025(2) 0.0351(11) Uani 1 1 d . . . . .
C2 C 0.5078(4) 0.7620(13) 0.5185(3) 0.098(3) Uani 1 1 d . . . . .
H2 H 0.5050 0.7980 0.5521 0.117 Uiso 1 1 calc R U . . .
C14 C 0.2606(3) 0.6299(7) 0.1403(2) 0.0433(13) Uani 1 1 d . . . . .
H14 H 0.2176 0.6459 0.1127 0.052 Uiso 1 1 calc R U . . .
C31 C 0.2748(3) 0.9585(7) 0.5666(2) 0.0405(13) Uani 1 1 d . . . . .
C33 C 0.2370(3) 0.9488(9) 0.6437(3) 0.0585(17) Uani 1 1 d . . . . .
C12 C 0.3788(3) 0.5670(7) 0.1688(2) 0.0459(14) Uani 1 1 d . . . . .
H12 H 0.4174 0.5397 0.1602 0.055 Uiso 1 1 calc R U . . .
C35 C 0.2554(4) 1.2115(9) 0.6090(3) 0.073(2) Uani 1 1 d . . . . .
H35 H 0.2550 1.3279 0.6106 0.088 Uiso 1 1 calc R U . . .
C6 C 0.5115(3) 0.5986(7) 0.3651(2) 0.0405(13) Uani 1 1 d . . . . .
C36 C 0.2743(3) 1.1338(8) 0.5694(3) 0.0548(16) Uani 1 1 d . . . . .
H36 H 0.2869 1.1973 0.5443 0.066 Uiso 1 1 calc R U . . .
C18 C 0.0481(3) 0.5004(7) 0.2809(2) 0.0440(13) Uani 1 1 d . . . . .
H18 H 0.0606 0.4605 0.3172 0.053 Uiso 1 1 calc R U . . .
C30 C 0.2960(3) 0.8745(8) 0.5229(2) 0.0450(13) Uani 1 1 d . . . . .
C15 C 0.2688(3) 0.6453(7) 0.1958(2) 0.0422(13) Uani 1 1 d . . . . .
H15 H 0.2303 0.6723 0.2047 0.051 Uiso 1 1 calc R U . . .
C22 C 0.0769(3) 0.6380(8) 0.2094(2) 0.0490(15) Uani 1 1 d . . . . .
H22 H 0.1087 0.6907 0.1970 0.059 Uiso 1 1 calc R U . . .
C34 C 0.2369(4) 1.1201(9) 0.6463(3) 0.068(2) Uani 1 1 d . . . . .
H34 H 0.2244 1.1740 0.6733 0.082 Uiso 1 1 calc R U . . .
C7 C 0.5716(3) 0.5395(8) 0.3594(2) 0.0554(16) Uani 1 1 d . . . . .
H7 H 0.6123 0.5300 0.3901 0.066 Uiso 1 1 calc R U . . .
C23 C 0.1176(3) 0.4119(7) 0.4742(2) 0.0421(13) Uani 1 1 d . . . . .
C26 C 0.0184(3) 0.2402(8) 0.5584(3) 0.0544(16) Uani 1 1 d . . . . .
C19 C -0.0189(3) 0.4850(8) 0.2449(3) 0.0539(16) Uani 1 1 d . . . . .
C28 C -0.0492(3) 0.2021(9) 0.4637(3) 0.0653(18) Uani 1 1 d . . . . .
H28 H -0.0898 0.1665 0.4362 0.078 Uiso 1 1 calc R U . . .
C29 C 0.0020(3) 0.2736(8) 0.4486(3) 0.0528(15) Uani 1 1 d . . . . .
H29 H -0.0035 0.2837 0.4112 0.063 Uiso 1 1 calc R U . . .
C20 C -0.0387(3) 0.5442(10) 0.1919(3) 0.070(2) Uani 1 1 d . . . . .
H20 H -0.0842 0.5326 0.1678 0.084 Uiso 1 1 calc R U . . .
C13 C 0.3160(3) 0.5910(7) 0.1266(2) 0.0445(13) Uani 1 1 d . . . . .
H13 H 0.3118 0.5807 0.0894 0.053 Uiso 1 1 calc R U . . .
C27 C -0.0409(3) 0.1832(8) 0.5185(3) 0.0614(18) Uani 1 1 d . . . . .
H27 H -0.0750 0.1324 0.5285 0.074 Uiso 1 1 calc R U . . .
C1 C 0.4503(3) 0.7461(12) 0.4730(3) 0.086(3) Uani 1 1 d . . . . .
H1 H 0.4083 0.7738 0.4760 0.103 Uiso 1 1 calc R U . . .
C25 C 0.0702(3) 0.3163(7) 0.5452(2) 0.0463(14) Uani 1 1 d . . . . .
H25 H 0.1096 0.3569 0.5729 0.056 Uiso 1 1 calc R U . . .
C32 C 0.2550(3) 0.8657(8) 0.6036(2) 0.0460(14) Uani 1 1 d . . . . .
H32 H 0.2538 0.7493 0.6017 0.055 Uiso 1 1 calc R U . . .
C9 C 0.5085(3) 0.5082(8) 0.2623(2) 0.0481(14) Uani 1 1 d . . . . .
H9 H 0.5065 0.4787 0.2268 0.058 Uiso 1 1 calc R U . . .
C21 C 0.0088(4) 0.6212(10) 0.1742(3) 0.070(2) Uani 1 1 d . . . . .
H21 H -0.0049 0.6628 0.1381 0.084 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 1.757(4) . ?
U1 O1 1.763(3) . ?
U1 O5 2.260(3) . ?
U1 O6 2.409(3) . ?
U1 N3 2.574(4) . ?
U1 N1 2.581(5) . ?
U1 N2 2.603(4) . ?
U2 O4 1.755(4) . ?
U2 O3 1.764(4) . ?
U2 O10 2.310(4) . ?
U2 O7 2.346(3) . ?
U2 O5 2.406(3) . ?
U2 O9 2.436(3) . ?
U2 O8 2.438(4) . ?
U2 C23 2.814(5) . ?
Br3 C33 1.895(6) . ?
Br1 C19 1.906(6) . ?
Br2 C26 1.904(6) . ?
Cl1 C8 1.724(5) . ?
O8 C23 1.264(6) . ?
O7 C16 1.256(6) . ?
O6 C16 1.254(6) . ?
N3 C15 1.336(6) . ?
N3 C11 1.352(6) . ?
O9 C23 1.259(6) . ?
O11 C30 1.235(6) . ?
N2 C6 1.342(6) . ?
N2 C10 1.354(6) . ?
C11 C12 1.391(7) . ?
C11 C10 1.475(7) . ?
O10 C30 1.297(7) . ?
N1 C5 1.329(7) . ?
N1 C1 1.356(7) . ?
C24 C29 1.388(8) . ?
C24 C25 1.380(7) . ?
C24 C23 1.500(7) . ?
C4 C5 1.378(8) . ?
C4 C3 1.364(9) . ?
C4 H4 0.9300 . ?
C3 C2 1.347(10) . ?
C3 H3 0.9300 . ?
C5 C6 1.485(7) . ?
C8 C7 1.380(8) . ?
C8 C9 1.368(8) . ?
C17 C18 1.392(7) . ?
C17 C22 1.391(7) . ?
C17 C16 1.492(7) . ?
C10 C9 1.384(7) . ?
C2 C1 1.348(9) . ?
C2 H2 0.9300 . ?
C14 C13 1.356(7) . ?
C14 C15 1.380(7) . ?
C14 H14 0.9300 . ?
C31 C32 1.379(7) . ?
C31 C36 1.402(8) . ?
C31 C30 1.502(7) . ?
C33 C34 1.369(9) . ?
C33 C32 1.386(8) . ?
C12 C13 1.380(8) . ?
C12 H12 0.9300 . ?
C35 C36 1.364(9) . ?
C35 C34 1.363(10) . ?
C35 H35 0.9300 . ?
C6 C7 1.392(7) . ?
C36 H36 0.9300 . ?
C18 C19 1.376(8) . ?
C18 H18 0.9300 . ?
C15 H15 0.9300 . ?
C22 C21 1.387(8) . ?
C22 H22 0.9300 . ?
C34 H34 0.9300 . ?
C7 H7 0.9300 . ?
C26 C27 1.370(9) . ?
C26 C25 1.379(7) . ?
C19 C20 1.359(9) . ?
C28 C27 1.365(9) . ?
C28 C29 1.380(8) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C20 C21 1.370(10) . ?
C20 H20 0.9300 . ?
C13 H13 0.9300 . ?
C27 H27 0.9300 . ?
C1 H1 0.9300 . ?
C25 H25 0.9300 . ?
C32 H32 0.9300 . ?
C9 H9 0.9300 . ?
C21 H21 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
O2 U1 O1 175.89(16) . . ?
O2 U1 O5 89.98(15) . . ?
O1 U1 O5 92.64(14) . . ?
O2 U1 O6 91.88(16) . . ?
O1 U1 O6 91.69(14) . . ?
O5 U1 O6 80.05(12) . . ?
O2 U1 N3 87.02(15) . . ?
O1 U1 N3 91.78(14) . . ?
O5 U1 N3 156.93(13) . . ?
O6 U1 N3 77.20(12) . . ?
O2 U1 N1 87.55(18) . . ?
O1 U1 N1 89.89(16) . . ?
O5 U1 N1 78.07(13) . . ?
O6 U1 N1 158.10(13) . . ?
N3 U1 N1 124.59(13) . . ?
O2 U1 N2 91.53(15) . . ?
O1 U1 N2 84.43(14) . . ?
O5 U1 N2 140.24(12) . . ?
O6 U1 N2 139.56(12) . . ?
N3 U1 N2 62.76(12) . . ?
N1 U1 N2 62.32(13) . . ?
O4 U2 O3 179.0(2) . . ?
O4 U2 O10 88.27(17) . . ?
O3 U2 O10 90.76(15) . . ?
O4 U2 O7 89.63(16) . . ?
O3 U2 O7 91.15(14) . . ?
O10 U2 O7 150.06(12) . . ?
O4 U2 O5 88.39(14) . . ?
O3 U2 O5 91.26(14) . . ?
O10 U2 O5 76.70(12) . . ?
O7 U2 O5 73.39(11) . . ?
O4 U2 O9 90.24(15) . . ?
O3 U2 O9 89.74(15) . . ?
O10 U2 O9 81.16(13) . . ?
O7 U2 O9 128.72(12) . . ?
O5 U2 O9 157.85(13) . . ?
O4 U2 O8 89.06(16) . . ?
O3 U2 O8 91.71(15) . . ?
O10 U2 O8 134.19(12) . . ?
O7 U2 O8 75.61(12) . . ?
O5 U2 O8 148.90(12) . . ?
O9 U2 O8 53.12(12) . . ?
O4 U2 C23 88.92(16) . . ?
O3 U2 C23 91.49(16) . . ?
O10 U2 C23 107.58(15) . . ?
O7 U2 C23 102.23(15) . . ?
O5 U2 C23 174.88(14) . . ?
O9 U2 C23 26.51(14) . . ?
O8 U2 C23 26.63(14) . . ?
U1 O5 U2 133.73(16) . . ?
C23 O8 U2 93.5(3) . . ?
C16 O7 U2 139.4(3) . . ?
C16 O6 U1 125.9(3) . . ?
C15 N3 C11 117.7(4) . . ?
C15 N3 U1 119.9(3) . . ?
C11 N3 U1 122.4(3) . . ?
C23 O9 U2 93.7(3) . . ?
C6 N2 C10 118.0(4) . . ?
C6 N2 U1 120.7(3) . . ?
C10 N2 U1 120.3(3) . . ?
N3 C11 C12 121.1(5) . . ?
N3 C11 C10 116.2(4) . . ?
C12 C11 C10 122.7(5) . . ?
C30 O10 U2 121.8(4) . . ?
C5 N1 C1 116.7(5) . . ?
C5 N1 U1 122.6(4) . . ?
C1 N1 U1 120.8(4) . . ?
C29 C24 C25 120.5(5) . . ?
C29 C24 C23 120.4(5) . . ?
C25 C24 C23 119.0(5) . . ?
C5 C4 C3 119.8(6) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C2 C3 C4 118.7(7) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
N1 C5 C4 121.8(5) . . ?
N1 C5 C6 116.5(5) . . ?
C4 C5 C6 121.7(5) . . ?
C7 C8 C9 120.4(5) . . ?
C7 C8 Cl1 120.3(5) . . ?
C9 C8 Cl1 119.3(5) . . ?
C18 C17 C22 118.7(5) . . ?
C18 C17 C16 119.2(5) . . ?
C22 C17 C16 122.1(5) . . ?
N2 C10 C9 122.1(5) . . ?
N2 C10 C11 117.2(4) . . ?
C9 C10 C11 120.7(5) . . ?
O6 C16 O7 123.3(5) . . ?
O6 C16 C17 119.7(4) . . ?
O7 C16 C17 116.9(4) . . ?
C3 C2 C1 119.4(7) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C13 C14 C15 119.2(5) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C32 C31 C36 119.4(5) . . ?
C32 C31 C30 121.0(5) . . ?
C36 C31 C30 119.6(5) . . ?
C34 C33 C32 121.2(6) . . ?
C34 C33 Br3 119.8(5) . . ?
C32 C33 Br3 119.0(5) . . ?
C13 C12 C11 120.0(5) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C36 C35 C34 120.6(7) . . ?
C36 C35 H35 119.7 . . ?
C34 C35 H35 119.7 . . ?
N2 C6 C7 122.9(5) . . ?
N2 C6 C5 116.5(4) . . ?
C7 C6 C5 120.6(5) . . ?
C35 C36 C31 120.1(6) . . ?
C35 C36 H36 119.9 . . ?
C31 C36 H36 119.9 . . ?
C19 C18 C17 120.3(5) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
O11 C30 O10 123.9(5) . . ?
O11 C30 C31 120.0(5) . . ?
O10 C30 C31 116.1(5) . . ?
N3 C15 C14 123.5(5) . . ?
N3 C15 H15 118.3 . . ?
C14 C15 H15 118.3 . . ?
C21 C22 C17 119.5(6) . . ?
C21 C22 H22 120.3 . . ?
C17 C22 H22 120.3 . . ?
C35 C34 C33 119.7(6) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C8 C7 C6 117.7(5) . . ?
C8 C7 H7 121.1 . . ?
C6 C7 H7 121.1 . . ?
O9 C23 O8 119.5(5) . . ?
O9 C23 C24 120.8(5) . . ?
O8 C23 C24 119.7(5) . . ?
O9 C23 U2 59.8(2) . . ?
O8 C23 U2 59.8(3) . . ?
C24 C23 U2 178.2(4) . . ?
C27 C26 C25 122.2(6) . . ?
C27 C26 Br2 120.0(4) . . ?
C25 C26 Br2 117.8(5) . . ?
C20 C19 C18 121.1(6) . . ?
C20 C19 Br1 120.1(5) . . ?
C18 C19 Br1 118.8(5) . . ?
C27 C28 C29 120.6(7) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
C24 C29 C28 119.5(6) . . ?
C24 C29 H29 120.3 . . ?
C28 C29 H29 120.3 . . ?
C19 C20 C21 119.4(6) . . ?
C19 C20 H20 120.3 . . ?
C21 C20 H20 120.3 . . ?
C14 C13 C12 118.6(5) . . ?
C14 C13 H13 120.7 . . ?
C12 C13 H13 120.7 . . ?
C26 C27 C28 119.1(6) . . ?
C26 C27 H27 120.5 . . ?
C28 C27 H27 120.5 . . ?
N1 C1 C2 123.5(6) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C26 C25 C24 118.0(6) . . ?
C26 C25 H25 121.0 . . ?
C24 C25 H25 121.0 . . ?
C31 C32 C33 118.9(6) . . ?
C31 C32 H32 120.6 . . ?
C33 C32 H32 120.6 . . ?
C8 C9 C10 118.9(5) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C20 C21 C22 121.0(6) . . ?
C20 C21 H21 119.5 . . ?
C22 C21 H21 119.5 . . ?

_refine_diff_density_max         1.801
_refine_diff_density_min         -1.408
_refine_diff_density_rms         0.127

_shelxl_version_number           2013-4


_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/. 
# 
# Audit and citation data items have may 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_Compound_10
_database_code_depnum_ccdc_archive 'CCDC 1025748'
_audit_update_record             
;
2014-09-23 deposited with the CCDC.
2014-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H18 Br2 Cl N3 O6 U'
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         937.76

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'
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                   8.9940(3)
_cell_length_b                   10.4251(4)
_cell_length_c                   16.3687(6)
_cell_angle_alpha                104.094(2)
_cell_angle_beta                 94.879(2)
_cell_angle_gamma                96.417(3)
_cell_volume                     1469.19(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    20005
_cell_measurement_theta_min      4.589
_cell_measurement_theta_max      43.467
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.120
_exptl_crystal_F_000             880
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    8.382
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5942
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS, 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            20005
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.291
_diffrn_reflns_theta_max         27.821
_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             6939
_reflns_number_gt                4998
_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-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Crystal Maker (Palmer, 2009)'
_computing_publication_material  'WINGX (Farrugia, 2012)'

_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)+(0.0326P)²+1.0570P] 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         6939
_refine_ls_number_parameters     379
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.0859
_refine_ls_wR_factor_gt          0.0758
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_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 0.71649(2) 0.14183(2) 0.32723(2) 0.04497(9) Uani 1 1 d . . . . .
Br2 Br 1.27761(10) -0.17313(10) -0.05691(5) 0.0948(3) Uani 1 1 d . . . . .
Br1 Br 0.73808(15) -0.56351(14) -0.10759(7) 0.1425(5) Uani 1 1 d . . . . .
Cl1 Cl 0.4871(2) 0.4568(3) 0.71491(12) 0.0974(7) Uani 1 1 d . . . . .
O1 O 0.6123(4) 0.1914(4) 0.2474(2) 0.0552(10) Uani 1 1 d . . . . .
O6 O 1.1620(5) 0.2601(5) 0.3100(3) 0.0818(15) Uani 1 1 d . . . . .
C16 C 0.7507(7) -0.1751(6) 0.2427(4) 0.0541(16) Uani 1 1 d . . . . .
O2 O 0.8155(5) 0.1011(4) 0.4124(3) 0.0571(11) Uani 1 1 d . . . . .
O5 O 0.9294(5) 0.1606(4) 0.2667(3) 0.0652(12) Uani 1 1 d . . . . .
C13 C 0.1682(8) -0.0582(7) 0.3806(5) 0.070(2) Uani 1 1 d . . . . .
H13 H 0.0706 -0.0898 0.3877 0.084 Uiso 1 1 calc R U . . .
N1 N 0.8131(5) 0.3922(5) 0.3823(3) 0.0481(12) Uani 1 1 d . . . . .
N3 N 0.4586(5) 0.0392(5) 0.3586(3) 0.0498(12) Uani 1 1 d . . . . .
O3 O 0.6834(5) -0.0728(4) 0.2441(3) 0.0639(12) Uani 1 1 d . . . . .
N2 N 0.5944(5) 0.2798(5) 0.4525(3) 0.0432(11) Uani 1 1 d . . . . .
C8 C 0.5293(7) 0.3887(7) 0.6149(4) 0.0588(17) Uani 1 1 d . . . . .
C24 C 1.1194(6) 0.0904(6) 0.1825(4) 0.0444(13) Uani 1 1 d . . . . .
C5 C 0.7823(6) 0.4646(6) 0.4575(4) 0.0432(13) Uani 1 1 d . . . . .
C1 C 0.9058(7) 0.4525(6) 0.3379(4) 0.0554(16) Uani 1 1 d . . . . .
H1 H 0.9239 0.4045 0.2847 0.066 Uiso 1 1 calc R U . . .
C10 C 0.4843(7) 0.2176(6) 0.4856(4) 0.0494(15) Uani 1 1 d . . . . .
O4 O 0.8192(7) -0.1970(5) 0.3043(3) 0.0847(16) Uani 1 1 d . . . . .
C23 C 1.0709(7) 0.1769(7) 0.2597(4) 0.0541(16) Uani 1 1 d . . . . .
C6 C 0.6689(6) 0.3980(6) 0.4997(4) 0.0453(14) Uani 1 1 d . . . . .
C25 C 1.0218(7) -0.0149(6) 0.1305(4) 0.0561(16) Uani 1 1 d . . . . .
H25 H 0.9236 -0.0316 0.1429 0.067 Uiso 1 1 calc R U . . .
C7 C 0.6382(7) 0.4549(7) 0.5817(4) 0.0559(16) Uani 1 1 d . . . . .
H7 H 0.6909 0.5363 0.6130 0.067 Uiso 1 1 calc R U . . .
C11 C 0.3959(7) 0.0950(6) 0.4277(4) 0.0497(15) Uani 1 1 d . . . . .
C2 C 0.9736(7) 0.5810(7) 0.3681(4) 0.0593(17) Uani 1 1 d . . . . .
H2 H 1.0367 0.6195 0.3359 0.071 Uiso 1 1 calc R U . . .
C3 C 0.9481(7) 0.6536(6) 0.4469(4) 0.0577(17) Uani 1 1 d . . . . .
H3 H 0.9956 0.7406 0.4693 0.069 Uiso 1 1 calc R U . . .
C15 C 0.3763(7) -0.0642(6) 0.3014(4) 0.0600(17) Uani 1 1 d . . . . .
H15 H 0.4186 -0.1047 0.2535 0.072 Uiso 1 1 calc R U . . .
C9 C 0.4490(7) 0.2678(7) 0.5665(4) 0.0546(16) Uani 1 1 d . . . . .
H9 H 0.3736 0.2223 0.5884 0.066 Uiso 1 1 calc R U . . .
C22 C 0.8247(9) -0.3742(7) 0.1464(5) 0.077(2) Uani 1 1 d . . . . .
H22 H 0.8814 -0.3874 0.1932 0.092 Uiso 1 1 calc R U . . .
C26 C 1.0692(7) -0.0956(6) 0.0601(4) 0.0612(17) Uani 1 1 d . . . . .
H26 H 1.0037 -0.1667 0.0250 0.073 Uiso 1 1 calc R U . . .
C4 C 0.8504(7) 0.5940(6) 0.4915(4) 0.0534(15) Uani 1 1 d . . . . .
H4 H 0.8305 0.6412 0.5445 0.064 Uiso 1 1 calc R U . . .
C14 C 0.2311(8) -0.1132(7) 0.3107(5) 0.0666(19) Uani 1 1 d . . . . .
H14 H 0.1770 -0.1838 0.2689 0.080 Uiso 1 1 calc R U . . .
C17 C 0.7440(7) -0.2699(6) 0.1570(4) 0.0522(15) Uani 1 1 d . . . . .
C12 C 0.2527(7) 0.0466(7) 0.4413(5) 0.0647(19) Uani 1 1 d . . . . .
H12 H 0.2136 0.0843 0.4910 0.078 Uiso 1 1 calc R U . . .
C29 C 1.2647(7) 0.1138(7) 0.1634(4) 0.0630(18) Uani 1 1 d . . . . .
H29 H 1.3313 0.1846 0.1981 0.076 Uiso 1 1 calc R U . . .
C18 C 0.6591(8) -0.2533(7) 0.0865(5) 0.071(2) Uani 1 1 d . . . . .
H18 H 0.6027 -0.1828 0.0921 0.085 Uiso 1 1 calc R U . . .
C28 C 1.3120(8) 0.0327(8) 0.0933(5) 0.070(2) Uani 1 1 d . . . . .
H28 H 1.4103 0.0481 0.0807 0.084 Uiso 1 1 calc R U . . .
C27 C 1.2133(8) -0.0696(7) 0.0430(4) 0.0608(17) Uani 1 1 d . . . . .
C19 C 0.6579(9) -0.3394(9) 0.0091(5) 0.089(3) Uani 1 1 d . . . . .
H19 H 0.6011 -0.3275 -0.0380 0.107 Uiso 1 1 calc R U . . .
C21 C 0.8246(10) -0.4617(8) 0.0675(5) 0.086(2) Uani 1 1 d . . . . .
H21 H 0.8819 -0.5317 0.0611 0.103 Uiso 1 1 calc R U . . .
C20 C 0.7404(8) -0.4435(8) 0.0007(5) 0.079(2) 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 O2 1.754(4) . ?
U1 O1 1.755(4) . ?
U1 O5 2.240(4) . ?
U1 O3 2.290(4) . ?
U1 N1 2.568(5) . ?
U1 N3 2.589(5) . ?
U1 N2 2.604(4) . ?
Br2 C27 1.901(6) . ?
Br1 C20 1.901(7) . ?
Cl1 C8 1.712(6) . ?
O6 C23 1.217(7) . ?
C16 O4 1.220(7) . ?
C16 O3 1.280(7) . ?
C16 C17 1.498(9) . ?
O5 C23 1.284(7) . ?
C13 C14 1.350(9) . ?
C13 C12 1.384(10) . ?
C13 H13 0.9300 . ?
N1 C5 1.347(7) . ?
N1 C1 1.351(7) . ?
N3 C11 1.340(7) . ?
N3 C15 1.341(7) . ?
N2 C10 1.346(7) . ?
N2 C6 1.352(7) . ?
C8 C7 1.361(9) . ?
C8 C9 1.396(9) . ?
C24 C25 1.379(8) . ?
C24 C29 1.378(8) . ?
C24 C23 1.492(8) . ?
C5 C4 1.377(8) . ?
C5 C6 1.481(8) . ?
C1 C2 1.362(9) . ?
C1 H1 0.9300 . ?
C10 C9 1.379(8) . ?
C10 C11 1.490(8) . ?
C6 C7 1.393(8) . ?
C25 C26 1.382(8) . ?
C25 H25 0.9300 . ?
C7 H7 0.9300 . ?
C11 C12 1.386(8) . ?
C2 C3 1.379(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.378(8) . ?
C3 H3 0.9300 . ?
C15 C14 1.382(9) . ?
C15 H15 0.9300 . ?
C9 H9 0.9300 . ?
C22 C17 1.359(9) . ?
C22 C21 1.388(10) . ?
C22 H22 0.9300 . ?
C26 C27 1.361(9) . ?
C26 H26 0.9300 . ?
C4 H4 0.9300 . ?
C14 H14 0.9300 . ?
C17 C18 1.387(9) . ?
C12 H12 0.9300 . ?
C29 C28 1.380(9) . ?
C29 H29 0.9300 . ?
C18 C19 1.361(9) . ?
C18 H18 0.9300 . ?
C28 C27 1.356(9) . ?
C28 H28 0.9300 . ?
C19 C20 1.368(10) . ?
C19 H19 0.9300 . ?
C21 C20 1.341(10) . ?
C21 H21 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
O2 U1 O1 175.85(18) . . ?
O2 U1 O5 90.13(18) . . ?
O1 U1 O5 92.47(18) . . ?
O2 U1 O3 93.50(18) . . ?
O1 U1 O3 89.99(18) . . ?
O5 U1 O3 83.90(16) . . ?
O2 U1 N1 93.32(17) . . ?
O1 U1 N1 84.08(17) . . ?
O5 U1 N1 77.78(15) . . ?
O3 U1 N1 160.44(15) . . ?
O2 U1 N3 93.09(17) . . ?
O1 U1 N3 85.58(17) . . ?
O5 U1 N3 159.73(16) . . ?
O3 U1 N3 75.93(15) . . ?
N1 U1 N3 121.94(15) . . ?
O2 U1 N2 80.25(16) . . ?
O1 U1 N2 95.66(16) . . ?
O5 U1 N2 137.68(15) . . ?
O3 U1 N2 137.39(15) . . ?
N1 U1 N2 61.96(15) . . ?
N3 U1 N2 62.54(15) . . ?
O4 C16 O3 124.8(6) . . ?
O4 C16 C17 120.1(6) . . ?
O3 C16 C17 115.1(6) . . ?
C23 O5 U1 159.4(4) . . ?
C14 C13 C12 118.2(6) . . ?
C14 C13 H13 120.9 . . ?
C12 C13 H13 120.9 . . ?
C5 N1 C1 118.3(5) . . ?
C5 N1 U1 121.9(4) . . ?
C1 N1 U1 119.7(4) . . ?
C11 N3 C15 117.6(5) . . ?
C11 N3 U1 121.6(4) . . ?
C15 N3 U1 120.5(4) . . ?
C16 O3 U1 134.6(4) . . ?
C10 N2 C6 118.4(5) . . ?
C10 N2 U1 119.0(4) . . ?
C6 N2 U1 119.5(3) . . ?
C7 C8 C9 120.2(6) . . ?
C7 C8 Cl1 119.7(6) . . ?
C9 C8 Cl1 120.1(5) . . ?
C25 C24 C29 119.2(6) . . ?
C25 C24 C23 121.0(5) . . ?
C29 C24 C23 119.8(5) . . ?
N1 C5 C4 121.4(5) . . ?
N1 C5 C6 116.1(5) . . ?
C4 C5 C6 122.5(5) . . ?
N1 C1 C2 122.4(6) . . ?
N1 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
N2 C10 C9 122.4(6) . . ?
N2 C10 C11 116.0(5) . . ?
C9 C10 C11 121.5(5) . . ?
O6 C23 O5 123.6(6) . . ?
O6 C23 C24 120.5(5) . . ?
O5 C23 C24 115.9(5) . . ?
N2 C6 C7 122.2(6) . . ?
N2 C6 C5 115.5(5) . . ?
C7 C6 C5 122.3(6) . . ?
C24 C25 C26 120.3(6) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C8 C7 C6 118.5(6) . . ?
C8 C7 H7 120.7 . . ?
C6 C7 H7 120.7 . . ?
N3 C11 C12 121.8(6) . . ?
N3 C11 C10 116.1(5) . . ?
C12 C11 C10 122.0(6) . . ?
C1 C2 C3 119.5(6) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C2 C3 C4 118.4(6) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
N3 C15 C14 122.8(6) . . ?
N3 C15 H15 118.6 . . ?
C14 C15 H15 118.6 . . ?
C10 C9 C8 118.3(6) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
C17 C22 C21 121.6(7) . . ?
C17 C22 H22 119.2 . . ?
C21 C22 H22 119.2 . . ?
C27 C26 C25 119.0(6) . . ?
C27 C26 H26 120.5 . . ?
C25 C26 H26 120.5 . . ?
C5 C4 C3 119.9(6) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C13 C14 C15 119.8(7) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C22 C17 C18 118.1(6) . . ?
C22 C17 C16 120.1(6) . . ?
C18 C17 C16 121.8(6) . . ?
C11 C12 C13 119.7(7) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C28 C29 C24 120.4(6) . . ?
C28 C29 H29 119.8 . . ?
C24 C29 H29 119.8 . . ?
C19 C18 C17 120.4(7) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C27 C28 C29 119.2(6) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
C28 C27 C26 121.9(6) . . ?
C28 C27 Br2 118.3(5) . . ?
C26 C27 Br2 119.7(5) . . ?
C18 C19 C20 119.9(7) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C20 C21 C22 118.8(7) . . ?
C20 C21 H21 120.6 . . ?
C22 C21 H21 120.6 . . ?
C21 C20 C19 121.1(7) . . ?
C21 C20 Br1 119.2(6) . . ?
C19 C20 Br1 119.7(6) . . ?

_refine_diff_density_max         1.125
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.123

_shelxl_version_number           2013-4


_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_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/. 
# 
# Audit and citation data items have may 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_Compound_11
_database_code_depnum_ccdc_archive 'CCDC 1025749'
_audit_update_record             
;
2014-09-23 deposited with the CCDC.
2014-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H20 Br6 Cl N3 O11 U2'
_chemical_melting_point          ?

_exptl_crystal_description       Rod
_exptl_crystal_colour            Yellow

_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         1661.52

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'
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      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                   18.8629(13)
_cell_length_b                   8.6591(6)
_cell_length_c                   26.9328(19)
_cell_angle_alpha                90
_cell_angle_beta                 107.231(3)
_cell_angle_gamma                90
_cell_volume                     4201.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    41478
_cell_measurement_theta_min      5.220
_cell_measurement_theta_max      50.692
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.627
_exptl_crystal_F_000             3024
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    13.530
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4400
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   'SADABS, 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            39989
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_av_R_equivalents  0.0790
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.583
_diffrn_reflns_theta_max         27.277
_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             9431
_reflns_number_gt                6742
_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-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Crystal Maker (Palmer, 2009)'
_computing_publication_material  'WINGX (Farrugia, 2012)'

_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)+(0.0219P)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         9431
_refine_ls_number_parameters     532
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.0715
_refine_ls_wR_factor_gt          0.0628
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.009
_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 0.48841(2) 0.31331(3) 0.07638(2) 0.01052(7) Uani 1 1 d . . . . .
U2 U 0.27365(2) 0.19705(3) 0.08296(2) 0.01137(7) Uani 1 1 d . . . . .
Br2 Br 0.14898(4) -0.20935(9) -0.13365(3) 0.02344(18) Uani 1 1 d . . . . .
Br4 Br -0.08794(4) -0.22715(9) 0.09654(3) 0.02556(19) Uani 1 1 d . . . . .
Br3 Br -0.01713(5) -0.37959(9) -0.08750(3) 0.02802(19) Uani 1 1 d . . . . .
Br1 Br 0.37596(4) 0.04100(9) -0.20750(3) 0.02380(18) Uani 1 1 d . . . . .
Br6 Br 0.13601(5) 0.98134(10) 0.20881(3) 0.0382(2) Uani 1 1 d . . . . .
Br5 Br 0.03702(5) 0.38172(13) 0.22796(4) 0.0474(3) Uani 1 1 d . . . . .
Cl1 Cl 0.81509(10) 0.7212(2) 0.18111(7) 0.0242(4) Uani 1 1 d . . . . .
O1 O 0.4936(2) 0.1138(5) 0.08894(17) 0.0145(11) Uani 1 1 d . . . . .
O2 O 0.4875(2) 0.5130(5) 0.06403(17) 0.0155(11) Uani 1 1 d . . . . .
O5 O 0.3835(2) 0.3503(5) 0.09937(17) 0.0142(11) Uani 1 1 d . . . . .
O8 O 0.1948(2) 0.0010(5) 0.02753(18) 0.0157(11) Uani 1 1 d . . . . .
O9 O 0.1603(3) 0.0881(5) 0.09333(19) 0.0183(11) Uani 1 1 d . . . . .
O6 O 0.4131(3) 0.2538(5) -0.01032(17) 0.0144(11) Uani 1 1 d . . . . .
O3 O 0.3254(2) 0.0493(5) 0.12376(17) 0.0154(11) Uani 1 1 d . . . . .
O4 O 0.2236(2) 0.3469(5) 0.04298(19) 0.0185(12) Uani 1 1 d . . . . .
N3 N 0.5844(3) 0.2752(6) 0.0273(2) 0.0133(13) Uani 1 1 d . . . . .
O7 O 0.3271(3) 0.1345(5) 0.01763(18) 0.0168(11) Uani 1 1 d . . . . .
O11 O 0.3151(3) 0.5732(5) 0.14623(19) 0.0199(12) Uani 1 1 d . . . . .
N1 N 0.5300(3) 0.3326(6) 0.1760(2) 0.0125(13) Uani 1 1 d . . . . .
O10 O 0.2717(3) 0.3381(5) 0.15461(18) 0.0173(11) Uani 1 1 d . . . . .
N2 N 0.6236(3) 0.3977(6) 0.1219(2) 0.0110(12) Uani 1 1 d . . . . .
C28 C -0.0250(4) -0.2080(8) 0.0534(3) 0.0177(16) Uani 1 1 d . . . . .
C27 C -0.0408(4) -0.2897(8) 0.0078(3) 0.0191(17) Uani 1 1 d . . . . .
H27 H -0.0824 -0.3532 -0.0024 0.023 Uiso 1 1 calc R U . . .
C11 C 0.6477(3) 0.3601(7) 0.0399(2) 0.0089(14) Uani 1 1 d . U . . .
C3 C 0.5777(4) 0.3320(7) 0.2846(3) 0.0167(16) Uani 1 1 d . . . . .
H3 H 0.5931 0.3333 0.3207 0.020 Uiso 1 1 calc R U . . .
C10 C 0.6668(4) 0.4349(7) 0.0913(3) 0.0127(15) Uani 1 1 d . . . . .
C6 C 0.6407(4) 0.4563(7) 0.1703(3) 0.0126(15) Uani 1 1 d . . . . .
C22 C 0.2636(4) -0.0093(8) -0.0758(3) 0.0165(16) Uani 1 1 d . . . . .
H22 H 0.2407 -0.0199 -0.0497 0.020 Uiso 1 1 calc R U . . .
C14 C 0.6121(4) 0.1894(8) -0.0495(3) 0.0131(15) Uani 1 1 d . . . . .
H14 H 0.5994 0.1273 -0.0790 0.016 Uiso 1 1 calc R U . . .
C35 C 0.1484(4) 0.7665(8) 0.2015(3) 0.0227(18) Uani 1 1 d . . . . .
C13 C 0.6752(4) 0.2804(8) -0.0374(3) 0.0189(17) Uani 1 1 d . . . . .
H13 H 0.7049 0.2841 -0.0594 0.023 Uiso 1 1 calc R U . . .
C30 C 0.2711(4) 0.4859(8) 0.1587(3) 0.0149(16) Uani 1 1 d . . . . .
C16 C 0.3567(4) 0.1627(7) -0.0172(3) 0.0137(15) Uani 1 1 d . . . . .
C31 C 0.2114(4) 0.5497(8) 0.1793(3) 0.0148(16) Uani 1 1 d . . . . .
C19 C 0.3318(4) 0.0174(8) -0.1531(3) 0.0163(16) Uani 1 1 d . U . . .
C15 C 0.5684(4) 0.1938(7) -0.0161(3) 0.0148(15) Uani 1 1 d . . . . .
H15 H 0.5250 0.1356 -0.0248 0.018 Uiso 1 1 calc R U . . .
C12 C 0.6933(4) 0.3659(8) 0.0079(3) 0.0165(16) Uani 1 1 d . . . . .
H12 H 0.7357 0.4269 0.0170 0.020 Uiso 1 1 calc R U . . .
C7 C 0.6992(4) 0.5586(7) 0.1896(3) 0.0129(15) Uani 1 1 d . . . . .
H7 H 0.7089 0.6002 0.2228 0.016 Uiso 1 1 calc R U . . .
C8 C 0.7424(4) 0.5967(7) 0.1581(3) 0.0145(16) Uani 1 1 d . . . . .
C9 C 0.7267(3) 0.5352(7) 0.1087(3) 0.0118(15) Uani 1 1 d . . . . .
H9 H 0.7558 0.5604 0.0874 0.014 Uiso 1 1 calc R U . . .
C4 C 0.6188(4) 0.4043(8) 0.2564(3) 0.0139(15) Uani 1 1 d . . . . .
H4 H 0.6622 0.4567 0.2735 0.017 Uiso 1 1 calc R U . . .
C2 C 0.5125(4) 0.2572(8) 0.2570(3) 0.0182(17) Uani 1 1 d . . . . .
H2 H 0.4843 0.2044 0.2747 0.022 Uiso 1 1 calc R U . . .
C20 C 0.2690(4) -0.0756(8) -0.1621(3) 0.0189(17) Uani 1 1 d . . . . .
H20 H 0.2500 -0.1284 -0.1933 0.023 Uiso 1 1 calc R U . . .
C5 C 0.5949(4) 0.3980(7) 0.2029(3) 0.0132(15) Uani 1 1 d . . . . .
C1 C 0.4900(4) 0.2621(8) 0.2036(3) 0.0154(16) Uani 1 1 d . U . . .
H1 H 0.4454 0.2151 0.1857 0.019 Uiso 1 1 calc R U . . .
C17 C 0.3259(4) 0.0839(7) -0.0684(3) 0.0116(15) Uani 1 1 d . . . . .
C33 C 0.1077(4) 0.5130(9) 0.2112(3) 0.0246(19) Uani 1 1 d . . . . .
C18 C 0.3604(4) 0.0981(7) -0.1074(3) 0.0123(15) Uani 1 1 d . . . . .
H18 H 0.4019 0.1607 -0.1027 0.015 Uiso 1 1 calc R U . . .
C24 C 0.0836(4) -0.1041(8) 0.0384(3) 0.0143(16) Uani 1 1 d . . . . .
C25 C 0.0691(4) -0.1846(8) -0.0076(3) 0.0156(15) Uani 1 1 d . . . . .
H25 H 0.1009 -0.1780 -0.0282 0.019 Uiso 1 1 calc R U . . .
C23 C 0.1495(4) 0.0003(8) 0.0543(3) 0.0138(15) Uani 1 1 d . . . . .
C36 C 0.2038(4) 0.7084(9) 0.1829(3) 0.0216(17) Uani 1 1 d . . . . .
H36 H 0.2358 0.7751 0.1729 0.026 Uiso 1 1 calc R U . . .
C32 C 0.1641(4) 0.4509(9) 0.1937(3) 0.0199(17) Uani 1 1 d . . . . .
H32 H 0.1697 0.3445 0.1920 0.024 Uiso 1 1 calc R U . . .
C29 C 0.0361(4) -0.1119(8) 0.0693(3) 0.0150(16) Uani 1 1 d . . . . .
H29 H 0.0452 -0.0543 0.0997 0.018 Uiso 1 1 calc R U . . .
C21 C 0.2361(4) -0.0859(7) -0.1227(3) 0.0141(15) Uani 1 1 d . . . . .
C26 C 0.0061(4) -0.2756(8) -0.0225(3) 0.0181(17) Uani 1 1 d . . . . .
C34 C 0.0990(4) 0.6683(9) 0.2152(3) 0.0265(19) Uani 1 1 d . . . . .
H34 H 0.0609 0.7076 0.2269 0.032 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 1.758(4) . ?
U1 O2 1.760(4) . ?
U1 O5 2.264(4) . ?
U1 O6 2.402(5) . ?
U1 N3 2.560(5) . ?
U1 N1 2.568(6) . ?
U1 N2 2.587(5) . ?
U2 O4 1.769(5) . ?
U2 O3 1.778(5) . ?
U2 O10 2.293(4) . ?
U2 O7 2.336(4) . ?
U2 O5 2.390(4) . ?
U2 O9 2.428(4) . ?
U2 O8 2.451(4) . ?
U2 C23 2.813(7) . ?
Br2 C21 1.909(6) . ?
Br4 C28 1.899(7) . ?
Br3 C26 1.900(7) . ?
Br1 C19 1.898(7) . ?
Br6 C35 1.893(7) . ?
Br5 C33 1.906(8) . ?
Cl1 C8 1.710(7) . ?
O8 C23 1.272(8) . ?
O9 C23 1.263(8) . ?
O6 C16 1.294(8) . ?
N3 C15 1.321(8) . ?
N3 C11 1.357(8) . ?
O7 C16 1.248(8) . ?
O11 C30 1.240(8) . ?
N1 C5 1.349(8) . ?
N1 C1 1.351(8) . ?
O10 C30 1.285(8) . ?
N2 C6 1.346(8) . ?
N2 C10 1.356(8) . ?
C28 C27 1.371(10) . ?
C28 C29 1.382(9) . ?
C27 C26 1.377(10) . ?
C27 H27 0.9300 . ?
C11 C12 1.386(9) . ?
C11 C10 1.474(9) . ?
C3 C4 1.385(9) . ?
C3 C2 1.394(9) . ?
C3 H3 0.9300 . ?
C10 C9 1.392(9) . ?
C6 C7 1.391(9) . ?
C6 C5 1.491(9) . ?
C22 C21 1.385(9) . ?
C22 C17 1.392(9) . ?
C22 H22 0.9300 . ?
C14 C13 1.384(9) . ?
C14 C15 1.390(9) . ?
C14 H14 0.9300 . ?
C35 C36 1.381(10) . ?
C35 C34 1.390(10) . ?
C13 C12 1.381(9) . ?
C13 H13 0.9300 . ?
C30 C31 1.498(9) . ?
C16 C17 1.493(9) . ?
C31 C32 1.374(9) . ?
C31 C36 1.389(9) . ?
C19 C18 1.379(9) . ?
C19 C20 1.393(9) . ?
C15 H15 0.9300 . ?
C12 H12 0.9300 . ?
C7 C8 1.379(9) . ?
C7 H7 0.9300 . ?
C8 C9 1.381(9) . ?
C9 H9 0.9300 . ?
C4 C5 1.379(9) . ?
C4 H4 0.9300 . ?
C2 C1 1.376(9) . ?
C2 H2 0.9300 . ?
C20 C21 1.382(9) . ?
C20 H20 0.9300 . ?
C1 H1 0.9300 . ?
C17 C18 1.396(9) . ?
C33 C34 1.363(10) . ?
C33 C32 1.392(9) . ?
C18 H18 0.9300 . ?
C24 C25 1.377(9) . ?
C24 C29 1.396(9) . ?
C24 C23 1.492(9) . ?
C25 C26 1.382(9) . ?
C25 H25 0.9300 . ?
C36 H36 0.9300 . ?
C32 H32 0.9300 . ?
C29 H29 0.9300 . ?
C34 H34 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
O1 U1 O2 177.4(2) . . ?
O1 U1 O5 95.14(18) . . ?
O2 U1 O5 87.29(18) . . ?
O1 U1 O6 87.68(18) . . ?
O2 U1 O6 93.28(18) . . ?
O5 U1 O6 89.04(15) . . ?
O1 U1 N3 88.00(18) . . ?
O2 U1 N3 89.86(18) . . ?
O5 U1 N3 165.60(17) . . ?
O6 U1 N3 77.03(16) . . ?
O1 U1 N1 83.13(18) . . ?
O2 U1 N1 96.69(19) . . ?
O5 U1 N1 74.11(16) . . ?
O6 U1 N1 159.91(16) . . ?
N3 U1 N1 120.26(17) . . ?
O1 U1 N2 101.29(18) . . ?
O2 U1 N2 76.38(19) . . ?
O5 U1 N2 130.50(16) . . ?
O6 U1 N2 137.50(16) . . ?
N3 U1 N2 62.08(17) . . ?
N1 U1 N2 62.20(17) . . ?
O4 U2 O3 178.8(2) . . ?
O4 U2 O10 89.02(19) . . ?
O3 U2 O10 90.34(18) . . ?
O4 U2 O7 89.03(19) . . ?
O3 U2 O7 91.04(18) . . ?
O10 U2 O7 151.09(16) . . ?
O4 U2 O5 88.99(18) . . ?
O3 U2 O5 89.87(18) . . ?
O10 U2 O5 77.18(15) . . ?
O7 U2 O5 73.95(15) . . ?
O4 U2 O9 91.48(18) . . ?
O3 U2 O9 89.46(18) . . ?
O10 U2 O9 82.86(16) . . ?
O7 U2 O9 126.03(16) . . ?
O5 U2 O9 160.02(15) . . ?
O4 U2 O8 91.11(18) . . ?
O3 U2 O8 90.07(18) . . ?
O10 U2 O8 136.31(15) . . ?
O7 U2 O8 72.57(15) . . ?
O5 U2 O8 146.51(15) . . ?
O9 U2 O8 53.46(15) . . ?
O4 U2 C23 91.5(2) . . ?
O3 U2 C23 89.6(2) . . ?
O10 U2 C23 109.46(18) . . ?
O7 U2 C23 99.43(18) . . ?
O5 U2 C23 173.34(17) . . ?
O9 U2 C23 26.61(16) . . ?
O8 U2 C23 26.85(16) . . ?
U1 O5 U2 130.63(19) . . ?
C23 O8 U2 92.7(4) . . ?
C23 O9 U2 93.9(4) . . ?
C16 O6 U1 119.6(4) . . ?
C15 N3 C11 117.7(6) . . ?
C15 N3 U1 120.9(4) . . ?
C11 N3 U1 120.4(4) . . ?
C16 O7 U2 155.3(4) . . ?
C5 N1 C1 117.4(6) . . ?
C5 N1 U1 122.4(4) . . ?
C1 N1 U1 119.9(4) . . ?
C30 O10 U2 127.2(4) . . ?
C6 N2 C10 118.9(6) . . ?
C6 N2 U1 119.0(4) . . ?
C10 N2 U1 117.7(4) . . ?
C27 C28 C29 122.0(6) . . ?
C27 C28 Br4 119.5(5) . . ?
C29 C28 Br4 118.5(5) . . ?
C28 C27 C26 118.6(7) . . ?
C28 C27 H27 120.7 . . ?
C26 C27 H27 120.7 . . ?
N3 C11 C12 121.7(6) . . ?
N3 C11 C10 115.1(6) . . ?
C12 C11 C10 123.0(6) . . ?
C4 C3 C2 117.9(7) . . ?
C4 C3 H3 121.1 . . ?
C2 C3 H3 121.1 . . ?
N2 C10 C9 121.2(6) . . ?
N2 C10 C11 116.3(6) . . ?
C9 C10 C11 122.5(6) . . ?
N2 C6 C7 122.6(6) . . ?
N2 C6 C5 115.4(6) . . ?
C7 C6 C5 122.0(6) . . ?
C21 C22 C17 118.7(6) . . ?
C21 C22 H22 120.6 . . ?
C17 C22 H22 120.6 . . ?
C13 C14 C15 117.8(6) . . ?
C13 C14 H14 121.1 . . ?
C15 C14 H14 121.1 . . ?
C36 C35 C34 120.9(7) . . ?
C36 C35 Br6 121.7(6) . . ?
C34 C35 Br6 117.4(6) . . ?
C12 C13 C14 118.9(6) . . ?
C12 C13 H13 120.6 . . ?
C14 C13 H13 120.6 . . ?
O11 C30 O10 124.0(6) . . ?
O11 C30 C31 120.8(6) . . ?
O10 C30 C31 115.2(6) . . ?
O7 C16 O6 122.9(6) . . ?
O7 C16 C17 117.9(6) . . ?
O6 C16 C17 119.2(6) . . ?
C32 C31 C36 120.5(7) . . ?
C32 C31 C30 119.8(6) . . ?
C36 C31 C30 119.7(6) . . ?
C18 C19 C20 122.4(6) . . ?
C18 C19 Br1 119.3(5) . . ?
C20 C19 Br1 118.2(5) . . ?
N3 C15 C14 124.2(7) . . ?
N3 C15 H15 117.9 . . ?
C14 C15 H15 117.9 . . ?
C13 C12 C11 119.6(6) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C8 C7 C6 118.0(6) . . ?
C8 C7 H7 121.0 . . ?
C6 C7 H7 121.0 . . ?
C7 C8 C9 120.3(6) . . ?
C7 C8 Cl1 118.9(6) . . ?
C9 C8 Cl1 120.8(5) . . ?
C8 C9 C10 119.0(6) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C5 C4 C3 119.5(6) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C1 C2 C3 119.5(7) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C21 C20 C19 117.1(7) . . ?
C21 C20 H20 121.4 . . ?
C19 C20 H20 121.4 . . ?
N1 C5 C4 122.8(6) . . ?
N1 C5 C6 114.7(6) . . ?
C4 C5 C6 122.4(6) . . ?
N1 C1 C2 122.7(7) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C22 C17 C18 120.3(6) . . ?
C22 C17 C16 118.6(6) . . ?
C18 C17 C16 121.1(6) . . ?
C34 C33 C32 122.0(7) . . ?
C34 C33 Br5 117.4(6) . . ?
C32 C33 Br5 120.5(6) . . ?
C19 C18 C17 118.8(6) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
C25 C24 C29 121.4(6) . . ?
C25 C24 C23 119.5(6) . . ?
C29 C24 C23 119.0(6) . . ?
C24 C25 C26 118.4(6) . . ?
C24 C25 H25 120.8 . . ?
C26 C25 H25 120.8 . . ?
O9 C23 O8 119.9(6) . . ?
O9 C23 C24 121.3(6) . . ?
O8 C23 C24 118.8(6) . . ?
O9 C23 U2 59.4(3) . . ?
O8 C23 U2 60.5(3) . . ?
C24 C23 U2 179.2(5) . . ?
C35 C36 C31 119.4(7) . . ?
C35 C36 H36 120.3 . . ?
C31 C36 H36 120.3 . . ?
C31 C32 C33 118.7(7) . . ?
C31 C32 H32 120.6 . . ?
C33 C32 H32 120.6 . . ?
C28 C29 C24 117.9(6) . . ?
C28 C29 H29 121.1 . . ?
C24 C29 H29 121.1 . . ?
C20 C21 C22 122.6(6) . . ?
C20 C21 Br2 118.7(5) . . ?
C22 C21 Br2 118.8(5) . . ?
C27 C26 C25 121.8(7) . . ?
C27 C26 Br3 119.4(6) . . ?
C25 C26 Br3 118.8(5) . . ?
C33 C34 C35 118.4(7) . . ?
C33 C34 H34 120.8 . . ?
C35 C34 H34 120.8 . . ?

_refine_diff_density_max         1.614
_refine_diff_density_min         -1.613
_refine_diff_density_rms         0.234

_shelxl_version_number           2013-4


_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/. 
# 
# Audit and citation data items have may 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_Compound_12
_database_code_depnum_ccdc_archive 'CCDC 1025750'
_audit_update_record             
;
2014-09-23 deposited with the CCDC.
2014-12-08 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H25 Br3 Cl N3 O12 U2'
_chemical_melting_point          ?

_exptl_crystal_description       Rod
_exptl_crystal_colour            Yellow

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1442.83

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'
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      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                   20.7962(8)
_cell_length_b                   7.5283(6)
_cell_length_c                   26.7408(11)
_cell_angle_alpha                90
_cell_angle_beta                 106.168(5)
_cell_angle_gamma                90
_cell_volume                     4021.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    40651
_cell_measurement_theta_min      4.625
_cell_measurement_theta_max      43.117
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.383
_exptl_crystal_F_000             2656
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    11.157
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6078
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS, 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            38989
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.455
_diffrn_reflns_theta_max         27.579
_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             9288
_reflns_number_gt                6498
_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    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Crystal Maker (Palmer, 2009)'
_computing_publication_material  'WINGX (Farrugia, 2012)'

_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)+(0.0279P)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         9288
_refine_ls_number_parameters     514
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.0769
_refine_ls_wR_factor_gt          0.0671
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_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
O2 O 0.6589(2) 0.5208(6) 0.10834(17) 0.0389(11) Uani 1 1 d . . . . .
O5 O 0.7157(2) 0.1894(5) 0.07548(16) 0.0318(10) Uani 1 1 d . . . . .
N3 N 0.5631(3) 0.2508(7) 0.0448(2) 0.0320(13) Uani 1 1 d . . . . .
N2 N 0.5396(3) 0.3716(7) 0.1331(2) 0.0312(13) Uani 1 1 d . . . . .
O6 O 0.7715(2) 0.3456(6) 0.18055(16) 0.0385(11) Uani 1 1 d . . . . .
O4 O 0.7236(2) 0.4809(6) 0.00507(17) 0.0424(12) Uani 1 1 d . . . . .
O8 O 0.8659(3) 0.5816(7) 0.03921(19) 0.0524(14) Uani 1 1 d . . . . .
O7 O 0.8048(2) 0.4709(6) 0.11641(16) 0.0403(12) Uani 1 1 d . . . . .
O1 O 0.6523(2) 0.0775(6) 0.14839(16) 0.0359(11) Uani 1 1 d . . . . .
O3 O 0.8536(2) 0.1830(6) 0.0646(2) 0.0543(14) Uani 1 1 d . . . . .
O9 O 0.8511(3) 0.4089(7) -0.0290(2) 0.0562(15) Uani 1 1 d . . . . .
Br2 Br 0.99381(5) 1.11127(13) -0.11882(4) 0.0749(3) Uani 1 1 d . . . . .
Br1 Br 1.09325(5) 0.56420(14) 0.31192(4) 0.0921(4) Uani 1 1 d . . . . .
Br3 Br 0.83591(8) -0.1579(4) -0.23983(6) 0.2213(12) Uani 1 1 d . . . . .
N1 N 0.6471(3) 0.3806(7) 0.2186(2) 0.0371(14) Uani 1 1 d . . . . .
Cl1 Cl 0.34538(11) 0.6256(3) 0.13241(10) 0.0756(7) Uani 1 1 d . . . . .
O10 O 0.7440(3) 0.1336(7) -0.02900(19) 0.0549(14) Uani 1 1 d . . . . .
C11 C 0.4993(3) 0.2975(8) 0.0416(2) 0.0309(15) Uani 1 1 d . . . . .
C15 C 0.5758(4) 0.1838(9) 0.0016(3) 0.0403(17) Uani 1 1 d . . . . .
H15 H 0.6194 0.1519 0.0030 0.048 Uiso 1 1 calc R U . . .
C10 C 0.4872(3) 0.3741(8) 0.0899(3) 0.0336(16) Uani 1 1 d . . . . .
C13 C 0.4612(4) 0.2090(9) -0.0472(3) 0.048(2) Uani 1 1 d . . . . .
H13 H 0.4271 0.1947 -0.0779 0.057 Uiso 1 1 calc R U . . .
C8 C 0.4188(4) 0.5230(9) 0.1329(3) 0.0444(18) Uani 1 1 d . . . . .
C4 C 0.5814(4) 0.4625(10) 0.2745(3) 0.051(2) Uani 1 1 d . . . . .
H4 H 0.5399 0.4939 0.2787 0.061 Uiso 1 1 calc R U . . .
C9 C 0.4257(3) 0.4436(9) 0.0890(3) 0.0438(18) Uani 1 1 d . . . . .
H9 H 0.3898 0.4366 0.0591 0.053 Uiso 1 1 calc R U . . .
C14 C 0.5260(4) 0.1610(9) -0.0446(3) 0.0424(18) Uani 1 1 d . . . . .
H14 H 0.5362 0.1136 -0.0736 0.051 Uiso 1 1 calc R U . . .
C6 C 0.5310(3) 0.4429(8) 0.1773(3) 0.0370(16) Uani 1 1 d . . . . .
C1 C 0.6985(4) 0.3619(11) 0.2610(3) 0.051(2) Uani 1 1 d . . . . .
H1 H 0.7395 0.3276 0.2565 0.061 Uiso 1 1 calc R U . . .
C5 C 0.5877(3) 0.4321(9) 0.2247(3) 0.0370(16) Uani 1 1 d . . . . .
C12 C 0.4478(4) 0.2787(9) -0.0034(3) 0.0413(18) Uani 1 1 d . . . . .
H12 H 0.4045 0.3126 -0.0043 0.050 Uiso 1 1 calc R U . . .
C2 C 0.6949(4) 0.3900(11) 0.3108(3) 0.052(2) Uani 1 1 d . . . . .
H2 H 0.7319 0.3710 0.3393 0.063 Uiso 1 1 calc R U . . .
C7 C 0.4711(4) 0.5223(9) 0.1781(3) 0.0458(19) Uani 1 1 d . . . . .
H7 H 0.4663 0.5740 0.2084 0.055 Uiso 1 1 calc R U . . .
C16 C 0.8149(3) 0.4203(8) 0.1625(3) 0.0315(15) Uani 1 1 d . . . . .
O11 O 0.6871(3) -0.1167(8) -0.0430(2) 0.0766(19) Uani 1 1 d . . . . .
C24 C 0.9085(4) 0.6833(9) -0.0301(3) 0.0413(17) Uani 1 1 d . . . . .
C27 C 0.9604(4) 0.9350(10) -0.0819(3) 0.0470(19) Uani 1 1 d . . . . .
C30 C 0.7251(4) -0.0087(10) -0.0548(3) 0.0429(18) Uani 1 1 d . . . . .
C17 C 0.8831(3) 0.4498(8) 0.1993(2) 0.0297(15) Uani 1 1 d . . . . .
C25 C 0.9051(3) 0.8625(9) -0.0183(3) 0.0417(18) Uani 1 1 d . . . . .
H25 H 0.8849 0.8970 0.0071 0.050 Uiso 1 1 calc R U . . .
C18 C 0.8939(4) 0.4290(9) 0.2515(3) 0.0456(18) Uani 1 1 d . . . . .
H18 H 0.8592 0.3929 0.2648 0.055 Uiso 1 1 calc R U . . .
C22 C 0.9353(3) 0.5016(9) 0.1801(3) 0.0446(18) Uani 1 1 d . . . . .
H22 H 0.9278 0.5161 0.1444 0.053 Uiso 1 1 calc R U . . .
C19 C 0.9576(4) 0.4623(10) 0.2850(3) 0.050(2) Uani 1 1 d . . . . .
H19 H 0.9651 0.4491 0.3208 0.061 Uiso 1 1 calc R U . . .
C31 C 0.7517(4) -0.0391(11) -0.1003(3) 0.048(2) Uani 1 1 d . . . . .
C20 C 1.0079(4) 0.5132(10) 0.2659(3) 0.052(2) Uani 1 1 d . . . . .
C26 C 0.9317(3) 0.9888(10) -0.0440(3) 0.0454(19) Uani 1 1 d . . . . .
H26 H 0.9301 1.1086 -0.0359 0.054 Uiso 1 1 calc R U . . .
C28 C 0.9656(4) 0.7596(11) -0.0937(3) 0.060(2) Uani 1 1 d . . . . .
H28 H 0.9867 0.7267 -0.1187 0.073 Uiso 1 1 calc R U . . .
C21 C 0.9989(4) 0.5327(10) 0.2132(3) 0.056(2) Uani 1 1 d . . . . .
H21 H 1.0342 0.5655 0.2001 0.068 Uiso 1 1 calc R U . . .
C32 C 0.7800(4) 0.0961(12) -0.1220(3) 0.054(2) Uani 1 1 d . . . . .
H32 H 0.7827 0.2105 -0.1084 0.065 Uiso 1 1 calc R U . . .
C36 C 0.7488(4) -0.2080(12) -0.1211(4) 0.075(3) Uani 1 1 d . . . . .
H36 H 0.7296 -0.2993 -0.1068 0.090 Uiso 1 1 calc R U . . .
C23 C 0.8737(4) 0.5515(11) -0.0054(3) 0.0486(19) Uani 1 1 d . . . . .
C29 C 0.9390(4) 0.6319(11) -0.0680(3) 0.061(2) Uani 1 1 d . . . . .
H29 H 0.9415 0.5124 -0.0760 0.073 Uiso 1 1 calc R U . . .
C3 C 0.6353(4) 0.4467(11) 0.3172(3) 0.058(2) Uani 1 1 d . . . . .
H3 H 0.6315 0.4741 0.3502 0.070 Uiso 1 1 calc R U . . .
C35 C 0.7738(7) -0.244(2) -0.1629(5) 0.130(6) Uani 1 1 d . . . . .
H35 H 0.7722 -0.3584 -0.1766 0.156 Uiso 1 1 calc R U . . .
C33 C 0.8043(5) 0.0595(18) -0.1643(4) 0.091(4) Uani 1 1 d . . . . .
H33 H 0.8227 0.1501 -0.1796 0.110 Uiso 1 1 calc R U . . .
C34 C 0.8013(6) -0.106(3) -0.1831(5) 0.116(6) Uani 1 1 d . . . . .
OW1 O 0.7201(3) -0.1603(6) 0.0616(2) 0.0722(18) Uani 1 1 d . . . . .
U1 U 0.65896(2) 0.29812(3) 0.12793(2) 0.02861(7) Uani 1 1 d . . . . .
U2 U 0.78927(2) 0.33211(3) 0.03348(2) 0.03244(8) 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
O2 U1 1.756(4) . ?
O5 U1 2.226(4) . ?
O5 U2 2.390(4) . ?
N3 C15 1.351(8) . ?
N3 C11 1.353(8) . ?
N3 U1 2.564(5) . ?
N2 C6 1.354(8) . ?
N2 C10 1.350(8) . ?
N2 U1 2.585(5) . ?
O6 C16 1.266(7) . ?
O6 U1 2.398(4) . ?
O4 U2 1.765(4) . ?
O8 C23 1.269(8) . ?
O8 U2 2.440(4) . ?
O7 C16 1.252(7) . ?
O7 U2 2.391(4) . ?
O1 U1 1.766(4) . ?
O3 U2 1.767(5) . ?
O9 C23 1.267(8) . ?
O9 U2 2.445(5) . ?
Br2 C27 1.898(7) . ?
Br1 C20 1.895(7) . ?
Br3 C34 1.892(12) . ?
N1 C1 1.331(8) . ?
N1 C5 1.348(8) . ?
N1 U1 2.580(5) . ?
Cl1 C8 1.708(7) . ?
O10 C30 1.276(8) . ?
O10 U2 2.244(5) . ?
C11 C12 1.378(9) . ?
C11 C10 1.497(9) . ?
C15 C14 1.383(9) . ?
C15 H15 0.9300 . ?
C10 C9 1.375(9) . ?
C13 C14 1.378(10) . ?
C13 C12 1.381(10) . ?
C13 H13 0.9300 . ?
C8 C9 1.361(9) . ?
C8 C7 1.382(10) . ?
C4 C3 1.364(10) . ?
C4 C5 1.394(9) . ?
C4 H4 0.9300 . ?
C9 H9 0.9300 . ?
C14 H14 0.9300 . ?
C6 C7 1.387(9) . ?
C6 C5 1.475(9) . ?
C1 C2 1.370(10) . ?
C1 H1 0.9300 . ?
C12 H12 0.9300 . ?
C2 C3 1.367(10) . ?
C2 H2 0.9300 . ?
C7 H7 0.9300 . ?
C16 C17 1.500(8) . ?
O11 C30 1.235(8) . ?
C24 C29 1.391(10) . ?
C24 C25 1.392(9) . ?
C24 C23 1.487(9) . ?
C27 C28 1.369(10) . ?
C27 C26 1.372(10) . ?
C30 C31 1.486(10) . ?
C17 C18 1.359(9) . ?
C17 C22 1.380(9) . ?
C25 C26 1.376(9) . ?
C25 H25 0.9300 . ?
C18 C19 1.401(9) . ?
C18 H18 0.9300 . ?
C22 C21 1.391(9) . ?
C22 H22 0.9300 . ?
C19 C20 1.341(11) . ?
C19 H19 0.9300 . ?
C31 C32 1.382(11) . ?
C31 C36 1.383(10) . ?
C20 C21 1.377(11) . ?
C26 H26 0.9300 . ?
C28 C29 1.383(10) . ?
C28 H28 0.9300 . ?
C21 H21 0.9300 . ?
C32 C33 1.389(11) . ?
C32 H32 0.9300 . ?
C36 C35 1.384(15) . ?
C36 H36 0.9300 . ?
C23 U2 2.813(7) . ?
C29 H29 0.9300 . ?
C3 H3 0.9300 . ?
C35 C34 1.372(19) . ?
C35 H35 0.9300 . ?
C33 C34 1.337(17) . ?
C33 H33 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
U1 O5 U2 130.70(18) . . ?
C15 N3 C11 117.7(6) . . ?
C15 N3 U1 120.2(4) . . ?
C11 N3 U1 122.0(4) . . ?
C6 N2 C10 118.1(6) . . ?
C6 N2 U1 119.5(4) . . ?
C10 N2 U1 121.0(4) . . ?
C16 O6 U1 121.7(4) . . ?
C23 O8 U2 93.2(4) . . ?
C16 O7 U2 136.4(4) . . ?
C23 O9 U2 93.0(4) . . ?
C1 N1 C5 118.1(6) . . ?
C1 N1 U1 120.8(5) . . ?
C5 N1 U1 120.9(4) . . ?
C30 O10 U2 164.7(5) . . ?
N3 C11 C12 122.5(6) . . ?
N3 C11 C10 116.4(6) . . ?
C12 C11 C10 121.1(6) . . ?
N3 C15 C14 122.2(7) . . ?
N3 C15 H15 118.9 . . ?
C14 C15 H15 118.9 . . ?
N2 C10 C9 123.0(6) . . ?
N2 C10 C11 116.3(6) . . ?
C9 C10 C11 120.7(6) . . ?
C14 C13 C12 118.8(7) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
C9 C8 C7 120.4(7) . . ?
C9 C8 Cl1 120.1(6) . . ?
C7 C8 Cl1 119.5(6) . . ?
C3 C4 C5 120.7(7) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C8 C9 C10 118.2(7) . . ?
C8 C9 H9 120.9 . . ?
C10 C9 H9 120.9 . . ?
C13 C14 C15 119.5(7) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
N2 C6 C7 121.4(6) . . ?
N2 C6 C5 117.5(6) . . ?
C7 C6 C5 121.1(6) . . ?
N1 C1 C2 124.4(7) . . ?
N1 C1 H1 117.8 . . ?
C2 C1 H1 117.8 . . ?
N1 C5 C4 119.9(7) . . ?
N1 C5 C6 116.9(6) . . ?
C4 C5 C6 123.2(7) . . ?
C11 C12 C13 119.3(7) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
C3 C2 C1 117.8(7) . . ?
C3 C2 H2 121.1 . . ?
C1 C2 H2 121.1 . . ?
C8 C7 C6 118.6(7) . . ?
C8 C7 H7 120.7 . . ?
C6 C7 H7 120.7 . . ?
O7 C16 O6 124.6(6) . . ?
O7 C16 C17 118.0(6) . . ?
O6 C16 C17 117.4(6) . . ?
C29 C24 C25 119.8(7) . . ?
C29 C24 C23 121.0(7) . . ?
C25 C24 C23 119.0(6) . . ?
C28 C27 C26 122.3(7) . . ?
C28 C27 Br2 119.4(6) . . ?
C26 C27 Br2 118.4(6) . . ?
O11 C30 O10 122.4(7) . . ?
O11 C30 C31 121.2(7) . . ?
O10 C30 C31 116.3(7) . . ?
C18 C17 C22 119.5(6) . . ?
C18 C17 C16 120.8(6) . . ?
C22 C17 C16 119.7(6) . . ?
C26 C25 C24 120.2(7) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C17 C18 C19 119.5(7) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C17 C22 C21 121.1(7) . . ?
C17 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
C20 C19 C18 120.5(7) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C32 C31 C36 118.9(8) . . ?
C32 C31 C30 121.9(7) . . ?
C36 C31 C30 119.1(8) . . ?
C19 C20 C21 121.4(7) . . ?
C19 C20 Br1 120.0(7) . . ?
C21 C20 Br1 118.6(7) . . ?
C27 C26 C25 118.8(7) . . ?
C27 C26 H26 120.6 . . ?
C25 C26 H26 120.6 . . ?
C27 C28 C29 119.2(7) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
C20 C21 C22 117.9(7) . . ?
C20 C21 H21 121.0 . . ?
C22 C21 H21 121.0 . . ?
C31 C32 C33 119.4(9) . . ?
C31 C32 H32 120.3 . . ?
C33 C32 H32 120.3 . . ?
C31 C36 C35 121.5(11) . . ?
C31 C36 H36 119.2 . . ?
C35 C36 H36 119.2 . . ?
O9 C23 O8 119.5(7) . . ?
O9 C23 C24 120.2(6) . . ?
O8 C23 C24 120.3(7) . . ?
O9 C23 U2 60.2(4) . . ?
O8 C23 U2 60.0(4) . . ?
C24 C23 U2 170.9(5) . . ?
C28 C29 C24 119.6(7) . . ?
C28 C29 H29 120.2 . . ?
C24 C29 H29 120.2 . . ?
C2 C3 C4 119.0(7) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C34 C35 C36 117.3(12) . . ?
C34 C35 H35 121.3 . . ?
C36 C35 H35 121.3 . . ?
C34 C33 C32 120.1(12) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C35 122.7(13) . . ?
C33 C34 Br3 120.4(13) . . ?
C35 C34 Br3 116.9(12) . . ?
O2 U1 O1 175.14(19) . . ?
O2 U1 O5 96.87(18) . . ?
O1 U1 O5 87.18(17) . . ?
O2 U1 O6 87.26(17) . . ?
O1 U1 O6 96.12(17) . . ?
O5 U1 O6 79.76(15) . . ?
O2 U1 N3 86.44(18) . . ?
O1 U1 N3 91.66(18) . . ?
O5 U1 N3 79.81(16) . . ?
O6 U1 N3 157.72(16) . . ?
O2 U1 N1 93.34(19) . . ?
O1 U1 N1 84.19(18) . . ?
O5 U1 N1 152.46(16) . . ?
O6 U1 N1 75.25(16) . . ?
N3 U1 N1 126.45(17) . . ?
O2 U1 N2 83.71(18) . . ?
O1 U1 N2 91.44(17) . . ?
O5 U1 N2 142.99(15) . . ?
O6 U1 N2 137.03(16) . . ?
N3 U1 N2 63.25(17) . . ?
N1 U1 N2 63.52(17) . . ?
O4 U2 O3 177.3(2) . . ?
O4 U2 O10 89.3(2) . . ?
O3 U2 O10 91.9(2) . . ?
O4 U2 O5 88.19(18) . . ?
O3 U2 O5 89.58(19) . . ?
O10 U2 O5 81.95(16) . . ?
O4 U2 O7 90.60(18) . . ?
O3 U2 O7 87.2(2) . . ?
O10 U2 O7 154.44(16) . . ?
O5 U2 O7 72.50(14) . . ?
O4 U2 O8 87.24(19) . . ?
O3 U2 O8 93.6(2) . . ?
O10 U2 O8 133.67(17) . . ?
O5 U2 O8 143.97(15) . . ?
O7 U2 O8 71.84(15) . . ?
O4 U2 O9 92.7(2) . . ?
O3 U2 O9 89.9(2) . . ?
O10 U2 O9 80.79(17) . . ?
O5 U2 O9 162.71(15) . . ?
O7 U2 O9 124.74(16) . . ?
O8 U2 O9 53.29(16) . . ?
O4 U2 C23 87.5(2) . . ?
O3 U2 C23 94.5(2) . . ?
O10 U2 C23 106.9(2) . . ?
O5 U2 C23 170.06(19) . . ?
O7 U2 C23 98.60(19) . . ?
O8 U2 C23 26.77(18) . . ?
O9 U2 C23 26.74(18) . . ?

_refine_diff_density_max         1.094
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.167

_shelxl_version_number           2013-4


_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/n'
_symmetry_int_tables_number      14
_chemical_absolute_configuration ?

#===END
