# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H12 N2 O5 U'
_chemical_formula_weight         502.27

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   11.5887(3)
_cell_length_b                   13.7676(4)
_cell_length_c                   16.8921(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2695.11(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2651
_cell_measurement_theta_min      2.96
_cell_measurement_theta_max      26.00

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1840
_exptl_absorpt_coefficient_mu    12.065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0858
_exptl_absorpt_correction_T_max  0.2200
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS SMART APEX II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            9893
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2651
_reflns_number_gt                2033
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0227P)²+3.0474P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00009(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2651
_refine_ls_number_parameters     183
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0294
_refine_ls_wR_factor_ref         0.0620
_refine_ls_wR_factor_gt          0.0566
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.080782(18) 0.031154(16) 0.612884(13) 0.03680(10) Uani 1 1 d . . .
C1 C -0.1354(5) 0.2005(4) 0.5797(4) 0.0451(16) Uani 1 1 d . . .
H1 H -0.1205 0.1770 0.5291 0.054 Uiso 1 1 calc R . .
C2 C -0.2162(5) 0.2743(4) 0.5881(5) 0.0520(18) Uani 1 1 d . . .
H2 H -0.2542 0.2997 0.5442 0.062 Uiso 1 1 calc R . .
C3 C -0.2383(6) 0.3089(5) 0.6625(6) 0.059(2) Uani 1 1 d . . .
H3 H -0.2929 0.3576 0.6703 0.071 Uiso 1 1 calc R . .
C4 C -0.1789(5) 0.2708(5) 0.7254(4) 0.0517(18) Uani 1 1 d . . .
H4 H -0.1922 0.2942 0.7762 0.062 Uiso 1 1 calc R . .
C5 C -0.0990(4) 0.1971(4) 0.7134(4) 0.0338(14) Uani 1 1 d . . .
C6 C -0.0295(5) 0.1578(4) 0.7788(4) 0.0343(14) Uani 1 1 d . . .
C7 C -0.0556(6) 0.1767(5) 0.8579(4) 0.0527(18) Uani 1 1 d . . .
H7 H -0.1191 0.2147 0.8711 0.063 Uiso 1 1 calc R . .
C8 C 0.0132(6) 0.1387(6) 0.9161(4) 0.061(2) Uani 1 1 d . . .
H8 H -0.0040 0.1508 0.9690 0.074 Uiso 1 1 calc R . .
C9 C 0.1065(6) 0.0835(5) 0.8969(4) 0.0545(18) Uani 1 1 d . . .
H9 H 0.1543 0.0582 0.9361 0.065 Uiso 1 1 calc R . .
C10 C 0.1284(5) 0.0661(4) 0.8178(4) 0.0413(15) Uani 1 1 d . . .
H10 H 0.1923 0.0286 0.8045 0.050 Uiso 1 1 calc R . .
C11 C 0.2963(5) -0.0669(4) 0.6337(4) 0.0356(14) Uani 1 1 d . . .
C12 C 0.4057(5) -0.1206(5) 0.6456(4) 0.0507(18) Uani 1 1 d . . .
H12A H 0.3945 -0.1877 0.6322 0.076 Uiso 1 1 calc R . .
H12B H 0.4290 -0.1155 0.7000 0.076 Uiso 1 1 calc R . .
H12C H 0.4644 -0.0934 0.6122 0.076 Uiso 1 1 calc R . .
O1 O 0.1573(5) 0.1334(4) 0.5773(4) 0.090(2) Uani 1 1 d . . .
O2 O 0.0071(4) -0.0667(3) 0.6574(4) 0.0642(15) Uani 1 1 d . . .
O3 O 0.0476(7) -0.0313(7) 0.4901(4) 0.197(6) Uani 1 1 d . . .
O4 O 0.2580(4) -0.0112(3) 0.6862(2) 0.0453(10) Uani 1 1 d . . .
O5 O 0.2389(4) -0.0802(4) 0.5725(3) 0.0661(15) Uani 1 1 d . . .
N1 N -0.0780(4) 0.1615(3) 0.6404(3) 0.0338(11) Uani 1 1 d . . .
N2 N 0.0614(4) 0.1008(3) 0.7588(3) 0.0306(11) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
U1 0.03823(14) 0.05060(16) 0.02159(14) -0.00350(11) -0.00052(11) 0.01577(10)
C1 0.040(3) 0.055(4) 0.041(4) 0.004(3) -0.004(3) 0.002(3)
C2 0.044(4) 0.044(4) 0.068(5) 0.013(4) -0.016(4) 0.002(3)
C3 0.042(3) 0.045(4) 0.091(6) -0.016(4) -0.006(4) 0.015(3)
C4 0.043(4) 0.057(4) 0.054(5) -0.022(4) -0.001(4) 0.011(3)
C5 0.028(3) 0.033(3) 0.040(4) -0.008(3) 0.005(3) 0.000(2)
C6 0.037(3) 0.035(3) 0.031(4) -0.007(3) 0.004(3) -0.008(3)
C7 0.048(4) 0.071(4) 0.039(4) -0.012(4) 0.009(4) 0.005(3)
C8 0.068(5) 0.087(5) 0.029(4) -0.011(4) 0.004(4) 0.004(4)
C9 0.071(5) 0.065(4) 0.027(4) -0.003(4) -0.011(4) -0.006(4)
C10 0.044(3) 0.047(3) 0.033(4) -0.001(3) -0.006(3) 0.002(3)
C11 0.033(3) 0.038(3) 0.036(4) 0.003(3) 0.002(3) 0.003(3)
C12 0.043(4) 0.059(4) 0.050(4) -0.008(4) -0.004(3) 0.008(3)
O1 0.079(4) 0.085(4) 0.106(5) 0.068(4) 0.055(4) 0.031(3)
O2 0.046(2) 0.040(2) 0.107(5) -0.017(3) 0.008(3) -0.009(2)
O3 0.196(8) 0.313(12) 0.081(5) -0.122(7) -0.089(6) 0.207(8)
O4 0.041(2) 0.059(2) 0.036(2) -0.012(2) -0.002(2) 0.010(2)
O5 0.059(3) 0.097(4) 0.042(3) -0.028(3) -0.017(3) 0.044(3)
N1 0.028(2) 0.040(3) 0.034(3) 0.001(2) 0.002(2) 0.004(2)
N2 0.036(2) 0.028(2) 0.028(3) -0.004(2) -0.001(2) -0.003(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 1.763(5) . ?
U1 O1 1.769(5) . ?
U1 O3 2.278(6) . ?
U1 O3 2.289(6) 5_556 ?
U1 O4 2.468(4) . ?
U1 O5 2.485(4) . ?
U1 N1 2.613(4) . ?
U1 N2 2.654(5) . ?
C1 N1 1.335(8) . ?
C1 C2 1.389(8) . ?
C2 C3 1.369(11) . ?
C3 C4 1.371(10) . ?
C4 C5 1.389(8) . ?
C5 N1 1.348(7) . ?
C5 C6 1.471(8) . ?
C6 N2 1.356(7) . ?
C6 C7 1.395(9) . ?
C7 C8 1.368(10) . ?
C8 C9 1.362(9) . ?
C9 C10 1.382(9) . ?
C10 N2 1.351(7) . ?
C11 O5 1.244(7) . ?
C11 O4 1.252(7) . ?
C11 C12 1.481(8) . ?
O3 O3 1.438(11) 5_556 ?
O3 U1 2.289(6) 5_556 ?

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 174.6(3) . . ?
O2 U1 O3 91.0(4) . . ?
O1 U1 O3 94.3(4) . . ?
O2 U1 O3 90.6(4) . 5_556 ?
O1 U1 O3 93.8(4) . 5_556 ?
O3 U1 O3 36.7(3) . 5_556 ?
O2 U1 O4 90.47(19) . . ?
O1 U1 O4 86.7(2) . . ?
O3 U1 O4 120.55(17) . . ?
O3 U1 O4 157.26(17) 5_556 . ?
O2 U1 O5 90.2(2) . . ?
O1 U1 O5 91.6(2) . . ?
O3 U1 O5 69.01(17) . . ?
O3 U1 O5 105.72(18) 5_556 . ?
O4 U1 O5 51.56(15) . . ?
O2 U1 N1 96.19(17) . . ?
O1 U1 N1 82.35(18) . . ?
O3 U1 N1 107.60(17) . . ?
O3 U1 N1 71.16(18) 5_556 . ?
O4 U1 N1 131.24(14) . . ?
O5 U1 N1 172.92(17) . . ?
O2 U1 N2 80.7(2) . . ?
O1 U1 N2 94.0(2) . . ?
O3 U1 N2 165.4(2) . . ?
O3 U1 N2 130.57(18) 5_556 . ?
O4 U1 N2 71.95(13) . . ?
O5 U1 N2 122.72(14) . . ?
N1 U1 N2 61.74(14) . . ?
N1 C1 C2 123.4(7) . . ?
C3 C2 C1 118.4(7) . . ?
C2 C3 C4 119.0(6) . . ?
C3 C4 C5 120.1(7) . . ?
N1 C5 C4 121.3(6) . . ?
N1 C5 C6 117.1(5) . . ?
C4 C5 C6 121.6(6) . . ?
N2 C6 C7 121.0(6) . . ?
N2 C6 C5 116.8(5) . . ?
C7 C6 C5 122.2(6) . . ?
C8 C7 C6 119.4(6) . . ?
C9 C8 C7 120.4(7) . . ?
C8 C9 C10 118.2(7) . . ?
N2 C10 C9 123.2(6) . . ?
O5 C11 O4 119.3(5) . . ?
O5 C11 C12 119.7(6) . . ?
O4 C11 C12 120.9(6) . . ?
O3 O3 U1 72.1(5) 5_556 . ?
O3 O3 U1 71.2(5) 5_556 5_556 ?
U1 O3 U1 143.3(3) . 5_556 ?
C11 O4 U1 94.8(3) . . ?
C11 O5 U1 94.3(4) . . ?
C1 N1 C5 117.8(5) . . ?
C1 N1 U1 119.3(4) . . ?
C5 N1 U1 122.6(4) . . ?
C10 N2 C6 117.8(5) . . ?
C10 N2 U1 120.5(4) . . ?
C6 N2 U1 120.5(4) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.130
_database_code_depnum_ccdc_archive 'CCDC 1008960'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_x

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H10 N3 O10 U2'
_chemical_formula_weight         784.25

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   17.5227(16)
_cell_length_b                   11.7243(10)
_cell_length_c                   16.7131(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.255(2)
_cell_angle_gamma                90.00
_cell_volume                     3177.8(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1874
_cell_measurement_theta_min      2.14
_cell_measurement_theta_max      28.47

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2744
_exptl_absorpt_coefficient_mu    20.412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0612
_exptl_absorpt_correction_T_max  0.1203
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS SMART APEX II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            9773
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         28.47
_reflns_number_total             3896
_reflns_number_gt                2987
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0801P)²+404.0546P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3896
_refine_ls_number_parameters     209
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0609
_refine_ls_wR_factor_ref         0.1850
_refine_ls_wR_factor_gt          0.1731
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.047
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4129(11) 0.1964(14) 0.6039(12) 0.016(3) Uani 1 1 d U . .
C2 C 0.377(2) 0.131(3) 0.652(2) 0.075(11) Uani 1 1 d . . .
H2A H 0.4046 0.1462 0.7121 0.112 Uiso 1 1 calc R . .
H2B H 0.3823 0.0510 0.6410 0.112 Uiso 1 1 calc R . .
H2C H 0.3197 0.1497 0.6337 0.112 Uiso 1 1 calc R . .
C3 C 0.7728(17) 0.4778(17) 0.4267(17) 0.043(7) Uani 1 1 d . . .
C4 C 0.817(2) 0.536(3) 0.373(3) 0.088(15) Uani 1 1 d . . .
C5 C 0.784(2) 0.632(3) 0.328(3) 0.098(17) Uani 1 1 d . . .
H5A H 0.7797 0.6877 0.3688 0.117 Uiso 1 1 calc R . .
H5B H 0.7285 0.6139 0.2891 0.117 Uiso 1 1 calc R . .
C6 C 0.8243(14) 0.6916(18) 0.2749(16) 0.035(5) Uani 1 1 d . . .
N3 N 0.8710(16) 0.758(2) 0.1809(15) 0.053(6) Uani 1 1 d . . .
N2 N 0.8625(14) 0.7925(17) 0.3009(14) 0.043(5) Uani 1 1 d . . .
H2D H 0.8670 0.8264 0.3481 0.051 Uiso 1 1 calc R . .
O1 O 0.6553(9) 0.5581(15) 0.5753(11) 0.040(4) Uani 1 1 d . . .
O2 O 0.5280(10) 0.4838(16) 0.3586(11) 0.045(4) Uani 1 1 d . . .
O3 O 0.5231(8) 0.1644(13) 0.4411(11) 0.037(4) Uani 1 1 d . . .
O4 O 0.6444(11) 0.2622(15) 0.6534(11) 0.043(4) Uani 1 1 d . . .
O5 O 0.6532(8) 0.3364(11) 0.4856(10) 0.026(3) Uani 1 1 d . . .
O6 O 0.5187(8) 0.3903(11) 0.5162(10) 0.024(3) Uani 1 1 d . . .
O8 O 0.4766(15) 0.1570(17) 0.5925(19) 0.081(8) Uani 1 1 d . . .
O10 O 0.7112(14) 0.5278(15) 0.4250(15) 0.065(7) Uani 1 1 d . . .
C8 C 0.8298(15) 0.671(2) 0.2010(17) 0.042(6) Uani 1 1 d . . .
H8 H 0.8089 0.6068 0.1671 0.050 Uiso 1 1 calc R . .
C7 C 0.8921(16) 0.833(2) 0.2449(19) 0.051(7) Uani 1 1 d . . .
H7 H 0.9218 0.8998 0.2493 0.061 Uiso 1 1 calc R . .
U1 U 0.58230(4) 0.22083(6) 0.54662(5) 0.0211(2) Uani 1 1 d . . .
U2 U 0.58854(4) 0.52109(6) 0.46729(5) 0.0212(2) Uani 1 1 d . . .
N1 N 0.8909(11) 0.4824(15) 0.3858(12) 0.032(4) Uani 1 1 d U . .
H1A H 0.9317 0.5281 0.4196 0.039 Uiso 1 1 calc R . .
H1B H 0.8958 0.4785 0.3341 0.039 Uiso 1 1 calc R . .
O9 O 0.3908(17) 0.2903(17) 0.574(2) 0.112(12) Uani 1 1 d . . .
O7 O 0.7997(9) 0.3890(12) 0.4599(11) 0.034(4) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.016(3) 0.017(3) 0.017(3) -0.0001(10) 0.0066(16) 0.0006(10)
C2 0.09(3) 0.09(2) 0.07(2) 0.037(19) 0.06(2) 0.00(2)
C3 0.080(18) 0.016(10) 0.057(16) 0.016(10) 0.055(15) 0.026(11)
C4 0.08(2) 0.09(2) 0.15(3) 0.10(2) 0.10(2) 0.069(18)
C5 0.07(2) 0.10(2) 0.17(4) 0.11(3) 0.10(3) 0.069(19)
C6 0.037(12) 0.027(11) 0.048(14) 0.016(10) 0.023(11) 0.022(9)
N3 0.069(16) 0.066(15) 0.040(13) 0.018(11) 0.037(12) 0.012(13)
N2 0.063(14) 0.034(11) 0.037(12) 0.000(9) 0.025(11) -0.002(10)
O1 0.019(7) 0.049(10) 0.051(11) -0.013(8) 0.012(7) -0.005(7)
O2 0.038(9) 0.067(12) 0.030(9) -0.004(8) 0.013(7) 0.020(8)
O3 0.014(7) 0.037(8) 0.048(10) -0.010(7) -0.004(7) 0.009(6)
O4 0.040(9) 0.047(10) 0.037(10) -0.002(8) 0.009(8) 0.000(8)
O5 0.029(7) 0.017(6) 0.044(9) 0.009(6) 0.026(7) 0.009(5)
O6 0.023(7) 0.020(6) 0.044(9) -0.002(6) 0.027(7) -0.004(5)
O8 0.097(18) 0.038(11) 0.15(2) 0.029(13) 0.100(19) 0.018(11)
O10 0.104(16) 0.034(9) 0.097(16) 0.035(10) 0.085(15) 0.041(10)
C8 0.039(13) 0.038(13) 0.049(16) -0.013(11) 0.016(12) -0.012(10)
C7 0.037(14) 0.046(15) 0.053(17) 0.021(13) -0.001(12) -0.017(11)
U1 0.0186(3) 0.0177(3) 0.0299(4) 0.0043(3) 0.0125(3) 0.0022(3)
U2 0.0256(4) 0.0171(3) 0.0298(4) 0.0026(3) 0.0204(3) 0.0044(3)
N1 0.032(4) 0.032(4) 0.033(4) 0.0001(10) 0.0124(18) 0.0001(10)
O9 0.11(2) 0.033(11) 0.25(4) 0.061(16) 0.13(2) 0.027(12)
O7 0.028(7) 0.024(7) 0.065(11) 0.020(7) 0.034(8) 0.011(6)

_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
C1 O9 1.21(3) . ?
C1 O8 1.29(2) . ?
C1 C2 1.42(3) . ?
C3 O7 1.19(2) . ?
C3 O10 1.22(3) . ?
C3 C4 1.54(3) . ?
C4 C5 1.37(3) . ?
C4 N1 1.38(3) . ?
C5 C6 1.49(3) . ?
C6 C8 1.30(3) . ?
C6 N2 1.35(3) . ?
N3 C7 1.32(4) . ?
N3 C8 1.36(3) . ?
N2 C7 1.32(3) . ?
O1 U2 1.794(17) . ?
O2 U2 1.776(17) . ?
O3 U1 1.799(15) . ?
O4 U1 1.771(17) . ?
O5 U1 2.320(13) . ?
O5 U2 2.410(12) . ?
O6 U1 2.240(13) . ?
O6 U2 2.255(12) 5_666 ?
O6 U2 2.296(12) . ?
O8 U1 2.379(19) . ?
O10 U2 2.505(18) . ?
U1 O7 2.473(13) 7_656 ?
U1 N1 2.603(18) 7_656 ?
U2 O6 2.255(12) 5_666 ?
U2 O9 2.383(18) 5_666 ?
U2 U2 3.6931(13) 5_666 ?
N1 U1 2.603(18) 7_656 ?
O9 U2 2.383(18) 5_666 ?
O7 U1 2.473(13) 7_656 ?

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
O9 C1 O8 115.0(19) . . ?
O9 C1 C2 126(2) . . ?
O8 C1 C2 119(2) . . ?
O7 C3 O10 128(2) . . ?
O7 C3 C4 117.2(19) . . ?
O10 C3 C4 114.3(18) . . ?
C5 C4 N1 129(2) . . ?
C5 C4 C3 119(2) . . ?
N1 C4 C3 111.3(19) . . ?
C4 C5 C6 122(2) . . ?
C8 C6 N2 105(2) . . ?
C8 C6 C5 134(3) . . ?
N2 C6 C5 120(3) . . ?
C7 N3 C8 108(2) . . ?
C7 N2 C6 112(2) . . ?
U1 O5 U2 106.0(5) . . ?
U1 O6 U2 138.3(6) . 5_666 ?
U1 O6 U2 112.8(5) . . ?
U2 O6 U2 108.5(5) 5_666 . ?
C1 O8 U1 139.4(14) . . ?
C3 O10 U2 145.6(15) . . ?
C6 C8 N3 110(2) . . ?
N2 C7 N3 106(2) . . ?
O4 U1 O3 174.2(7) . . ?
O4 U1 O6 92.8(7) . . ?
O3 U1 O6 92.9(6) . . ?
O4 U1 O5 93.2(7) . . ?
O3 U1 O5 89.4(7) . . ?
O6 U1 O5 71.6(4) . . ?
O4 U1 O8 91.0(9) . . ?
O3 U1 O8 88.3(9) . . ?
O6 U1 O8 88.4(5) . . ?
O5 U1 O8 159.7(6) . . ?
O4 U1 O7 89.0(7) . 7_656 ?
O3 U1 O7 87.0(6) . 7_656 ?
O6 U1 O7 143.5(4) . 7_656 ?
O5 U1 O7 71.8(4) . 7_656 ?
O8 U1 O7 128.1(6) . 7_656 ?
O4 U1 N1 82.7(7) . 7_656 ?
O3 U1 N1 91.8(7) . 7_656 ?
O6 U1 N1 154.6(5) . 7_656 ?
O5 U1 N1 133.4(5) . 7_656 ?
O8 U1 N1 66.8(6) . 7_656 ?
O7 U1 N1 61.7(5) 7_656 7_656 ?
O2 U2 O1 176.4(7) . . ?
O2 U2 O6 92.0(6) . 5_666 ?
O1 U2 O6 91.2(6) . 5_666 ?
O2 U2 O6 90.4(7) . . ?
O1 U2 O6 92.1(7) . . ?
O6 U2 O6 71.5(5) 5_666 . ?
O2 U2 O9 91.8(11) . 5_666 ?
O1 U2 O9 87.3(11) . 5_666 ?
O6 U2 O9 80.3(6) 5_666 5_666 ?
O6 U2 O9 151.8(6) . 5_666 ?
O2 U2 O5 88.8(7) . . ?
O1 U2 O5 89.6(7) . . ?
O6 U2 O5 140.6(4) 5_666 . ?
O6 U2 O5 69.1(4) . . ?
O9 U2 O5 139.1(6) 5_666 . ?
O2 U2 O10 87.9(8) . . ?
O1 U2 O10 88.5(8) . . ?
O6 U2 O10 149.8(5) 5_666 . ?
O6 U2 O10 138.7(5) . . ?
O9 U2 O10 69.5(6) 5_666 . ?
O5 U2 O10 69.6(5) . . ?
O2 U2 U2 91.5(6) . 5_666 ?
O1 U2 U2 92.0(5) . 5_666 ?
O6 U2 U2 36.1(3) 5_666 5_666 ?
O6 U2 U2 35.4(3) . 5_666 ?
O9 U2 U2 116.4(5) 5_666 5_666 ?
O5 U2 U2 104.5(3) . 5_666 ?
O10 U2 U2 174.0(4) . 5_666 ?
C4 N1 U1 118.9(15) . 7_656 ?
C1 O9 U2 155(2) . 5_666 ?
C3 O7 U1 128.6(14) . 7_656 ?

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        28.47
_diffrn_measured_fraction_theta_full 0.968
_refine_diff_density_max         1.770
_refine_diff_density_min         -2.993
_refine_diff_density_rms         0.377
_database_code_depnum_ccdc_archive 'CCDC 1008961'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H14 N2 O6 U'
_chemical_formula_weight         544.30

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_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                   7.9487(5)
_cell_length_b                   19.0021(11)
_cell_length_c                   10.5863(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.6450(10)
_cell_angle_gamma                90.00
_cell_volume                     1591.22(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3212
_cell_measurement_theta_min      2.14
_cell_measurement_theta_max      28.30

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1008
_exptl_absorpt_coefficient_mu    10.232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.045
_exptl_absorpt_correction_T_max  0.293
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS SMART APEX II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            9876
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         28.30
_reflns_number_total             3893
_reflns_number_gt                2978
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0207P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3893
_refine_ls_number_parameters     210
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0285
_refine_ls_wR_factor_ref         0.0581
_refine_ls_wR_factor_gt          0.0533
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_restrained_S_all      0.989
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.28054(2) 0.830321(7) 0.159468(17) 0.03399(6) Uani 1 1 d . . .
C1 C 0.0830(6) 0.8860(2) -0.1299(5) 0.0423(12) Uani 1 1 d . . .
H1 H 0.0570 0.8383 -0.1281 0.051 Uiso 1 1 calc R . .
C2 C 0.0183(6) 0.9250(3) -0.2317(5) 0.0472(12) Uani 1 1 d . . .
H2 H -0.0512 0.9044 -0.2973 0.057 Uiso 1 1 calc R . .
C3 C 0.0573(7) 0.9948(3) -0.2356(5) 0.0507(13) Uani 1 1 d . . .
H3 H 0.0164 1.0222 -0.3047 0.061 Uiso 1 1 calc R . .
C4 C 0.1572(6) 1.0242(2) -0.1369(5) 0.0462(13) Uani 1 1 d . . .
H4 H 0.1852 1.0717 -0.1386 0.055 Uiso 1 1 calc R . .
C5 C 0.2163(5) 0.9827(2) -0.0341(4) 0.0338(10) Uani 1 1 d . . .
C6 C 0.3136(5) 1.0113(2) 0.0801(5) 0.0346(10) Uani 1 1 d . . .
C7 C 0.3684(6) 1.0804(2) 0.0889(5) 0.0456(13) Uani 1 1 d . . .
H7 H 0.3474 1.1103 0.0196 0.055 Uiso 1 1 calc R . .
C8 C 0.4528(7) 1.1050(2) 0.1984(5) 0.0519(14) Uani 1 1 d . . .
H8 H 0.4894 1.1515 0.2044 0.062 Uiso 1 1 calc R . .
C9 C 0.4826(7) 1.0603(3) 0.2990(6) 0.0542(14) Uani 1 1 d . . .
H9 H 0.5394 1.0756 0.3750 0.065 Uiso 1 1 calc R . .
C10 C 0.4265(7) 0.9917(2) 0.2854(5) 0.0495(13) Uani 1 1 d . . .
H10 H 0.4492 0.9611 0.3535 0.059 Uiso 1 1 calc R . .
C11 C 0.2799(6) 0.8067(2) 0.4249(5) 0.0401(11) Uani 1 1 d . . .
C12 C 0.2597(7) 0.7917(3) 0.5591(5) 0.0481(13) Uani 1 1 d . . .
H12A H 0.1905 0.7507 0.5646 0.072 Uiso 1 1 calc R . .
H12B H 0.2068 0.8312 0.5957 0.072 Uiso 1 1 calc R . .
H12C H 0.3687 0.7836 0.6043 0.072 Uiso 1 1 calc R . .
C13 C 0.2957(6) 0.7127(2) -0.0024(5) 0.0397(11) Uani 1 1 d . . .
C14 C 0.3077(7) 0.6508(3) -0.0886(5) 0.0563(15) Uani 1 1 d . . .
H14A H 0.2832 0.6084 -0.0444 0.085 Uiso 1 1 calc R . .
H14B H 0.4198 0.6481 -0.1146 0.085 Uiso 1 1 calc R . .
H14C H 0.2276 0.6562 -0.1620 0.085 Uiso 1 1 calc R . .
O1 O 0.0587(4) 0.82676(15) 0.1539(3) 0.0427(8) Uani 1 1 d . . .
O2 O 0.5020(4) 0.83399(14) 0.1677(3) 0.0428(8) Uani 1 1 d . . .
O3 O 0.3051(5) 0.75711(16) 0.3493(3) 0.0559(10) Uani 1 1 d . . .
O4 O 0.2680(4) 0.86891(16) 0.3814(3) 0.0476(9) Uani 1 1 d . . .
O5 O 0.2774(5) 0.70440(16) 0.1116(4) 0.0532(10) Uani 1 1 d . . .
O6 O 0.3054(5) 0.77433(16) -0.0471(3) 0.0475(9) Uani 1 1 d . . .
N1 N 0.1822(5) 0.91334(17) -0.0328(4) 0.0353(9) Uani 1 1 d . . .
N2 N 0.3411(5) 0.96684(19) 0.1794(4) 0.0395(9) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
U1 0.04185(11) 0.02462(9) 0.03613(11) 0.00052(8) 0.00707(7) 0.00188(7)
C1 0.043(3) 0.035(2) 0.047(3) 0.001(2) -0.001(2) 0.001(2)
C2 0.044(3) 0.054(3) 0.042(3) 0.000(3) -0.001(2) 0.007(2)
C3 0.054(3) 0.050(3) 0.047(3) 0.019(3) 0.003(3) 0.008(2)
C4 0.051(3) 0.037(3) 0.052(3) 0.011(2) 0.012(3) 0.000(2)
C5 0.035(3) 0.028(2) 0.041(3) 0.007(2) 0.014(2) 0.0035(18)
C6 0.035(2) 0.030(2) 0.041(3) -0.002(2) 0.013(2) 0.0020(19)
C7 0.055(3) 0.032(2) 0.053(3) -0.001(2) 0.015(3) -0.005(2)
C8 0.065(4) 0.030(2) 0.063(4) -0.008(3) 0.017(3) -0.014(2)
C9 0.064(4) 0.044(3) 0.054(4) -0.013(3) 0.004(3) -0.017(3)
C10 0.065(4) 0.036(3) 0.046(3) 0.005(2) 0.000(3) -0.006(2)
C11 0.044(3) 0.036(2) 0.040(3) 0.000(2) 0.001(2) -0.004(2)
C12 0.053(3) 0.049(3) 0.043(3) 0.006(3) 0.004(3) -0.003(2)
C13 0.037(3) 0.035(3) 0.047(3) -0.006(2) 0.001(2) 0.0033(19)
C14 0.070(4) 0.046(3) 0.052(4) -0.017(3) 0.001(3) 0.003(3)
O1 0.047(2) 0.0417(18) 0.040(2) 0.0003(16) 0.0082(15) -0.0051(14)
O2 0.0436(19) 0.0411(17) 0.043(2) -0.0038(16) 0.0008(15) 0.0073(14)
O3 0.093(3) 0.0337(18) 0.042(2) 0.0025(17) 0.010(2) 0.0096(18)
O4 0.072(2) 0.0303(17) 0.042(2) 0.0034(16) 0.0137(18) -0.0027(15)
O5 0.092(3) 0.0285(17) 0.041(2) -0.0016(16) 0.016(2) -0.0017(16)
O6 0.067(2) 0.0355(17) 0.040(2) -0.0013(16) 0.0071(17) 0.0065(16)
N1 0.038(2) 0.0273(18) 0.040(2) 0.0017(17) 0.0026(18) 0.0024(15)
N2 0.045(2) 0.0290(19) 0.045(3) -0.0019(18) 0.0053(19) -0.0013(16)

_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 1.760(3) . ?
U1 O3 2.437(3) . ?
U1 O5 2.445(3) . ?
U1 O6 2.457(3) . ?
U1 O4 2.472(3) . ?
U1 N1 2.632(4) . ?
U1 N2 2.643(4) . ?
C1 N1 1.338(6) . ?
C1 C2 1.367(7) . ?
C1 H1 0.9300 . ?
C2 C3 1.363(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.367(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.388(6) . ?
C4 H4 0.9300 . ?
C5 N1 1.346(5) . ?
C5 C6 1.474(6) . ?
C6 N2 1.349(6) . ?
C6 C7 1.383(6) . ?
C7 C8 1.364(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.366(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.380(6) . ?
C9 H9 0.9300 . ?
C10 N2 1.339(6) . ?
C10 H10 0.9300 . ?
C11 O3 1.265(5) . ?
C11 O4 1.269(5) . ?
C11 C12 1.472(7) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 O5 1.239(6) . ?
C13 O6 1.269(5) . ?
C13 C14 1.497(6) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U1 O1 179.08(15) . . ?
O2 U1 O3 89.03(14) . . ?
O1 U1 O3 90.26(14) . . ?
O2 U1 O5 92.23(13) . . ?
O1 U1 O5 88.03(13) . . ?
O3 U1 O5 67.09(12) . . ?
O2 U1 O6 83.88(14) . . ?
O1 U1 O6 96.97(14) . . ?
O3 U1 O6 118.69(11) . . ?
O5 U1 O6 52.55(11) . . ?
O2 U1 O4 94.30(14) . . ?
O1 U1 O4 84.81(14) . . ?
O3 U1 O4 52.62(10) . . ?
O5 U1 O4 119.12(11) . . ?
O6 U1 O4 171.24(10) . . ?
O2 U1 N1 103.57(13) . . ?
O1 U1 N1 77.10(13) . . ?
O3 U1 N1 166.82(12) . . ?
O5 U1 N1 115.46(12) . . ?
O6 U1 N1 67.36(11) . . ?
O4 U1 N1 121.35(11) . . ?
O2 U1 N2 77.47(12) . . ?
O1 U1 N2 102.39(12) . . ?
O3 U1 N2 119.69(12) . . ?
O5 U1 N2 167.14(12) . . ?
O6 U1 N2 117.77(11) . . ?
O4 U1 N2 69.95(11) . . ?
N1 U1 N2 60.76(12) . . ?
N1 C1 C2 122.9(4) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C3 C2 C1 118.8(5) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C2 C3 C4 119.4(5) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C3 C4 C5 119.6(4) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
N1 C5 C4 120.7(5) . . ?
N1 C5 C6 116.3(4) . . ?
C4 C5 C6 122.9(4) . . ?
N2 C6 C7 121.1(5) . . ?
N2 C6 C5 116.1(4) . . ?
C7 C6 C5 122.8(5) . . ?
C8 C7 C6 120.6(5) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C7 C8 C9 118.8(4) . . ?
C7 C8 H8 120.6 . . ?
C9 C8 H8 120.6 . . ?
C8 C9 C10 118.5(5) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
N2 C10 C9 123.5(5) . . ?
N2 C10 H10 118.2 . . ?
C9 C10 H10 118.2 . . ?
O3 C11 O4 118.3(4) . . ?
O3 C11 C12 120.4(4) . . ?
O4 C11 C12 121.3(4) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O5 C13 O6 119.8(4) . . ?
O5 C13 C14 121.0(4) . . ?
O6 C13 C14 119.2(5) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 O3 U1 95.3(3) . . ?
C11 O4 U1 93.5(3) . . ?
C13 O5 U1 94.5(3) . . ?
C13 O6 U1 93.1(3) . . ?
C1 N1 C5 118.5(4) . . ?
C1 N1 U1 118.0(3) . . ?
C5 N1 U1 123.4(3) . . ?
C10 N2 C6 117.5(4) . . ?
C10 N2 U1 119.1(3) . . ?
C6 N2 U1 122.5(3) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.125
_database_code_depnum_ccdc_archive 'CCDC 1008962'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_x

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C2 H10 N O10.50 U2'
_chemical_formula_weight         692.17

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   7.2325(16)
_cell_length_b                   16.469(4)
_cell_length_c                   17.315(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.814(3)
_cell_angle_gamma                90.00
_cell_volume                     2025.9(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1879
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      28.07

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2376
_exptl_absorpt_coefficient_mu    31.982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0510
_exptl_absorpt_correction_T_max  0.1140
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS SMART APEX II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            5702
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_sigmaI/netI    0.1106
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.39
_diffrn_reflns_theta_max         28.07
_reflns_number_total             2396
_reflns_number_gt                1608
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0330P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2396
_refine_ls_number_parameters     147
_refine_ls_number_restraints     29
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0505
_refine_ls_wR_factor_ref         0.1081
_refine_ls_wR_factor_gt          0.0939
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.25367(8) 0.36988(4) 0.28959(4) 0.01171(17) Uani 1 1 d . . .
U2 U 0.83552(9) 0.42811(4) 0.42410(4) 0.01728(19) Uani 1 1 d . . .
O1W O 0.8779(17) 0.3058(8) 0.6287(7) 0.030(3) Uani 1 1 d D . .
H1C H 0.801(7) 0.2719(15) 0.637(9) 0.045 Uiso 1 1 d D . .
H1D H 0.922(9) 0.335(6) 0.666(6) 0.045 Uiso 1 1 d D . .
O1 O 0.9178(19) 0.3375(8) 0.4755(7) 0.033(3) Uani 1 1 d . . .
O2 O 0.7358(17) 0.5161(7) 0.3735(8) 0.029(3) Uani 1 1 d . . .
O2W O 1.0000 0.4088(11) 0.7500 0.047(6) Uani 1 2 d S . .
H2C H 1.1074 0.4299 0.7630 0.070 Uiso 0.50 1 d PR . .
H2D H 0.9092 0.4386 0.7539 0.070 Uiso 0.50 1 d PRD . .
O3 O 0.2176(15) 0.2621(7) 0.2801(6) 0.013(3) Uani 1 1 d U . .
O4 O 0.3037(15) 0.4760(7) 0.3020(7) 0.020(3) Uani 1 1 d . . .
O5 O 1.1206(16) 0.4984(8) 0.4561(7) 0.026(3) Uani 1 1 d . . .
O6 O 0.5976(14) 0.3554(7) 0.3274(6) 0.013(3) Uani 1 1 d U . .
O7 O -0.0324(14) 0.3906(7) 0.3221(6) 0.013(3) Uani 1 1 d U . .
O8 O 0.5724(17) 0.4045(8) 0.4945(7) 0.026(3) Uani 1 1 d . . .
O9 O 0.3244(16) 0.3424(8) 0.4263(7) 0.021(3) Uani 1 1 d . . .
N1 N 0.503(2) 0.3493(10) 0.6363(9) 0.030(4) Uani 1 1 d . . .
H1A H 0.5989 0.3800 0.6360 0.036 Uiso 1 1 calc RD . .
H1B H 0.4801 0.3310 0.6801 0.036 Uiso 1 1 calc R . .
C1 C 0.427(3) 0.3629(11) 0.4887(10) 0.021(4) Uani 1 1 d U . .
C2 C 0.377(3) 0.3283(12) 0.5621(9) 0.025(5) Uani 1 1 d . . .
H2A H 0.2512 0.3462 0.5653 0.030 Uiso 1 1 calc R . .
H2B H 0.3739 0.2696 0.5573 0.030 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
U1 0.0078(3) 0.0165(4) 0.0112(3) 0.0004(3) 0.0026(2) -0.0001(3)
U2 0.0142(4) 0.0227(4) 0.0150(3) -0.0029(3) 0.0031(3) -0.0011(3)
O1W 0.024(8) 0.030(8) 0.033(8) 0.012(7) -0.002(6) -0.012(6)
O1 0.050(9) 0.026(8) 0.021(7) -0.006(6) 0.000(7) 0.016(7)
O2 0.030(8) 0.018(7) 0.035(8) 0.000(6) -0.007(6) 0.010(6)
O2W 0.049(14) 0.009(11) 0.085(18) 0.000 0.019(13) 0.000
O3 0.012(5) 0.020(6) 0.009(5) 0.000(4) 0.007(4) 0.002(4)
O4 0.005(6) 0.032(8) 0.024(7) 0.006(6) 0.002(5) -0.002(5)
O5 0.014(7) 0.036(8) 0.030(8) -0.014(6) 0.014(6) -0.011(6)
O6 0.005(5) 0.020(6) 0.015(5) -0.001(5) 0.004(4) 0.004(4)
O7 0.008(5) 0.020(6) 0.012(5) 0.001(4) 0.006(4) 0.001(4)
O8 0.019(7) 0.039(9) 0.024(7) -0.008(6) 0.011(6) -0.006(6)
O9 0.016(7) 0.038(8) 0.011(6) -0.006(6) 0.008(5) -0.003(6)
N1 0.030(10) 0.041(11) 0.020(9) 0.009(8) 0.008(8) -0.008(8)
C1 0.023(8) 0.026(8) 0.017(7) 0.004(6) 0.015(6) 0.004(7)
C2 0.039(12) 0.031(12) 0.006(9) -0.003(8) 0.006(9) 0.000(10)

_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 O4 1.789(12) . ?
U1 O3 1.797(11) . ?
U1 O7 2.270(10) . ?
U1 O7 2.293(11) 2 ?
U1 O9 2.370(12) . ?
U1 O6 2.462(10) . ?
U1 O6 2.477(10) 2_655 ?
U1 U1 3.6683(14) 2 ?
U1 U2 3.7591(12) 2_655 ?
U1 U1 4.0508(14) 2_655 ?
U2 O2 1.776(12) . ?
U2 O1 1.782(13) . ?
U2 O7 2.246(10) 1_655 ?
U2 O5 2.338(12) . ?
U2 O5 2.372(12) 5_766 ?
U2 O6 2.473(11) . ?
U2 O8 2.476(11) . ?
U2 U1 3.7591(12) 2_655 ?
U2 U2 3.9787(15) 5_766 ?
O1W H1C 0.818(10) . ?
O1W H1D 0.820(10) . ?
O2W H2C 0.8419 . ?
O2W H2D 0.8327 . ?
O5 U2 2.372(12) 5_766 ?
O6 U1 2.477(10) 2_655 ?
O7 U2 2.246(10) 1_455 ?
O7 U1 2.293(11) 2 ?
O8 C1 1.24(2) . ?
O9 C1 1.24(2) . ?
N1 C2 1.47(2) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
C1 C2 1.50(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?

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
O4 U1 O3 176.6(5) . . ?
O4 U1 O7 89.8(4) . . ?
O3 U1 O7 92.7(4) . . ?
O4 U1 O7 92.9(5) . 2 ?
O3 U1 O7 90.2(4) . 2 ?
O7 U1 O7 70.3(4) . 2 ?
O4 U1 O9 93.7(5) . . ?
O3 U1 O9 84.4(4) . . ?
O7 U1 O9 79.4(4) . . ?
O7 U1 O9 149.0(4) 2 . ?
O4 U1 O6 83.8(4) . . ?
O3 U1 O6 92.9(4) . . ?
O7 U1 O6 150.6(4) . . ?
O7 U1 O6 138.5(3) 2 . ?
O9 U1 O6 72.4(4) . . ?
O4 U1 O6 94.8(4) . 2_655 ?
O3 U1 O6 84.7(4) . 2_655 ?
O7 U1 O6 140.7(4) . 2_655 ?
O7 U1 O6 70.5(3) 2 2_655 ?
O9 U1 O6 138.9(4) . 2_655 ?
O6 U1 O6 68.7(4) . 2_655 ?
O4 U1 U1 102.2(3) . 2 ?
O3 U1 U1 81.3(3) . 2 ?
O7 U1 U1 36.7(3) . 2 ?
O7 U1 U1 36.3(2) 2 2 ?
O9 U1 U1 112.8(3) . 2 ?
O6 U1 U1 171.6(2) . 2 ?
O6 U1 U1 104.6(2) 2_655 2 ?
O4 U1 U2 82.1(4) . 2_655 ?
O3 U1 U2 99.6(3) . 2_655 ?
O7 U1 U2 102.1(3) . 2_655 ?
O7 U1 U2 33.7(2) 2 2_655 ?
O9 U1 U2 175.5(3) . 2_655 ?
O6 U1 U2 105.4(2) . 2_655 ?
O6 U1 U2 40.6(2) 2_655 2_655 ?
U1 U1 U2 69.95(2) 2 2_655 ?
O4 U1 U1 82.5(3) . 2_655 ?
O3 U1 U1 95.2(3) . 2_655 ?
O7 U1 U1 170.0(3) . 2_655 ?
O7 U1 U1 103.5(2) 2 2_655 ?
O9 U1 U1 107.4(3) . 2_655 ?
O6 U1 U1 35.0(2) . 2_655 ?
O6 U1 U1 34.8(2) 2_655 2_655 ?
U1 U1 U1 139.05(4) 2 2_655 ?
U2 U1 U1 70.50(2) 2_655 2_655 ?
O2 U2 O1 175.6(6) . . ?
O2 U2 O7 91.7(5) . 1_655 ?
O1 U2 O7 90.6(5) . 1_655 ?
O2 U2 O5 88.3(5) . . ?
O1 U2 O5 95.7(6) . . ?
O7 U2 O5 80.6(4) 1_655 . ?
O2 U2 O5 89.5(5) . 5_766 ?
O1 U2 O5 90.8(5) . 5_766 ?
O7 U2 O5 145.2(4) 1_655 5_766 ?
O5 U2 O5 64.7(5) . 5_766 ?
O2 U2 O6 84.0(5) . . ?
O1 U2 O6 93.3(5) . . ?
O7 U2 O6 71.3(4) 1_655 . ?
O5 U2 O6 150.5(4) . . ?
O5 U2 O6 143.3(4) 5_766 . ?
O2 U2 O8 95.3(5) . . ?
O1 U2 O8 80.7(5) . . ?
O7 U2 O8 145.4(4) 1_655 . ?
O5 U2 O8 133.3(4) . . ?
O5 U2 O8 68.8(4) 5_766 . ?
O6 U2 O8 75.9(4) . . ?
O2 U2 U1 75.1(4) . 2_655 ?
O1 U2 U1 104.9(4) . 2_655 ?
O7 U2 U1 34.5(3) 1_655 2_655 ?
O5 U2 U1 109.9(3) . 2_655 ?
O5 U2 U1 164.0(3) 5_766 2_655 ?
O6 U2 U1 40.6(2) . 2_655 ?
O8 U2 U1 116.0(3) . 2_655 ?
O2 U2 U2 88.7(4) . 5_766 ?
O1 U2 U2 93.8(4) . 5_766 ?
O7 U2 U2 113.2(3) 1_655 5_766 ?
O5 U2 U2 32.6(3) . 5_766 ?
O5 U2 U2 32.1(3) 5_766 5_766 ?
O6 U2 U2 171.6(2) . 5_766 ?
O8 U2 U2 100.8(3) . 5_766 ?
U1 U2 U2 140.63(3) 2_655 5_766 ?
H1C O1W H1D 116(2) . . ?
H2C O2W H2D 115.9 . . ?
U2 O5 U2 115.3(5) . 5_766 ?
U1 O6 U2 132.3(4) . . ?
U1 O6 U1 110.2(4) . 2_655 ?
U2 O6 U1 98.8(4) . 2_655 ?
U2 O7 U1 141.1(5) 1_455 . ?
U2 O7 U1 111.8(4) 1_455 2 ?
U1 O7 U1 107.0(4) . 2 ?
C1 O8 U2 139.7(11) . . ?
C1 O9 U1 143.3(12) . . ?
C2 N1 H1A 120.0 . . ?
C2 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
O9 C1 O8 125.5(16) . . ?
O9 C1 C2 115.9(16) . . ?
O8 C1 C2 118.4(17) . . ?
N1 C2 C1 116.4(16) . . ?
N1 C2 H2A 108.2 . . ?
C1 C2 H2A 108.2 . . ?
N1 C2 H2B 108.2 . . ?
C1 C2 H2B 108.2 . . ?
H2A C2 H2B 107.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1C N1 0.818(10) 2.50(2) 2.83(2) 105(2) .
O1W H1D O2W 0.820(10) 1.899(16) 2.716(17) 174(7) .
O2W H2D O4 0.83 2.17 2.914(16) 148.1 5_666
O2W H2C O4 0.84 2.13 2.914(16) 156.0 6_666
N1 H1A O1W 0.86 2.38 2.83(2) 113.2 .
N1 H1A O4 0.86 2.64 3.29(2) 132.7 5_666
N1 H1B O3 0.86 2.29 2.978(18) 137.2 7_556

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        28.07
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         2.482
_refine_diff_density_min         -2.536
_refine_diff_density_rms         0.558
_database_code_depnum_ccdc_archive 'CCDC 1008963'
