# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1057328'
_audit_update_record             
;
2015-04-01 deposited with the CCDC.
2015-05-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H8 O8 U'
_chemical_formula_weight         470.17

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'
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           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.7190(10)
_cell_length_b                   8.1323(13)
_cell_length_c                   10.5527(16)
_cell_angle_alpha                95.083(2)
_cell_angle_beta                 100.796(2)
_cell_angle_gamma                103.617(2)
_cell_volume                     545.14(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2858
_cell_measurement_theta_min      3.05
_cell_measurement_theta_max      30.87

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.864
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             424
_exptl_absorpt_coefficient_mu    14.916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1457
_exptl_absorpt_correction_T_max  0.3470
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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            2753
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.60
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1884
_reflns_number_gt                1796
_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)+(0.0560P)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     SHELXL
_refine_ls_extinction_coef       0.0154(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1884
_refine_ls_number_parameters     155
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0794
_refine_ls_wR_factor_gt          0.0786
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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 -0.2189(9) 0.0784(9) 0.0301(6) 0.0240(14) Uani 1 1 d . . .
C2 C -0.2881(9) 0.1392(9) 0.3064(6) 0.0228(14) Uani 1 1 d . . .
C3 C -0.2691(9) 0.2728(9) 0.2167(6) 0.0226(13) Uani 1 1 d . . .
C4 C -0.2851(11) 0.4316(10) 0.2665(7) 0.0317(16) Uani 1 1 d . . .
H4 H -0.3039 0.4507 0.3511 0.038 Uiso 1 1 calc R . .
C5 C -0.2729(11) 0.5626(10) 0.1893(8) 0.0364(18) Uani 1 1 d . . .
H5 H -0.2780 0.6705 0.2235 0.044 Uiso 1 1 calc R . .
C6 C -0.2537(12) 0.5325(10) 0.0644(9) 0.0388(18) Uani 1 1 d . . .
H6 H -0.2475 0.6201 0.0131 0.047 Uiso 1 1 calc R . .
C7 C -0.2433(11) 0.3733(10) 0.0121(7) 0.0338(16) Uani 1 1 d . . .
H7 H -0.2335 0.3537 -0.0744 0.041 Uiso 1 1 calc R . .
C8 C -0.2474(9) 0.2430(9) 0.0888(6) 0.0237(14) Uani 1 1 d . . .
O1 O 0.1232(9) -0.1418(7) 0.3124(6) 0.0304(12) Uani 1 1 d . . .
O1W O 0.3422(9) 0.6136(8) 0.4024(7) 0.0535(17) Uani 1 1 d . . .
H1WB H 0.2510 0.6578 0.3616 0.080 Uiso 1 1 d R . .
H1WC H 0.3467 0.6309 0.4837 0.080 Uiso 1 1 d R . .
O2 O 0.2242(8) 0.2800(7) 0.2380(5) 0.0266(11) Uani 1 1 d . . .
O3 O -0.1358(7) 0.0826(7) 0.3517(5) 0.0321(12) Uani 1 1 d . . .
O4 O -0.1248(7) -0.0090(6) 0.1012(4) 0.0247(10) Uani 1 1 d . . .
O5 O 0.2881(7) -0.0340(7) 0.0896(5) 0.0330(12) Uani 1 1 d . . .
O6 O 0.5388(7) 0.0889(6) 0.3399(4) 0.0255(10) Uani 1 1 d . . .
O7 O 0.2752(7) 0.1754(6) 0.5011(5) 0.0314(11) Uani 1 1 d . . .
H7A H 0.4075 0.1952 0.5259 0.047 Uiso 1 1 d R . .
H7B H 0.2383 0.2674 0.5143 0.047 Uiso 1 1 d R . .
U1 U 0.17405(3) 0.06728(2) 0.272122(18) 0.01755(17) 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 0.012(3) 0.037(4) 0.020(3) -0.001(3) 0.000(2) 0.005(3)
C2 0.017(3) 0.029(4) 0.020(3) -0.003(3) 0.003(2) 0.005(3)
C3 0.016(3) 0.027(4) 0.023(3) 0.003(3) 0.002(2) 0.003(2)
C4 0.029(4) 0.036(4) 0.031(4) -0.001(3) 0.011(3) 0.009(3)
C5 0.030(4) 0.022(4) 0.054(5) -0.001(3) 0.005(3) 0.004(3)
C6 0.035(4) 0.027(4) 0.059(5) 0.021(4) 0.015(4) 0.006(3)
C7 0.033(4) 0.041(4) 0.033(4) 0.016(3) 0.014(3) 0.012(3)
C8 0.014(3) 0.037(4) 0.021(3) 0.003(3) 0.004(2) 0.008(3)
O1 0.025(3) 0.028(3) 0.038(3) 0.010(2) 0.004(2) 0.006(2)
O1W 0.050(4) 0.038(3) 0.066(4) 0.001(3) -0.008(3) 0.016(3)
O2 0.025(3) 0.030(3) 0.027(3) 0.007(2) 0.007(2) 0.008(2)
O3 0.018(2) 0.053(3) 0.033(3) 0.018(2) 0.008(2) 0.018(2)
O4 0.020(2) 0.031(3) 0.020(2) 0.0004(19) -0.0052(18) 0.0081(19)
O5 0.023(2) 0.052(3) 0.025(3) -0.005(2) 0.0023(19) 0.017(2)
O6 0.014(2) 0.039(3) 0.025(2) 0.010(2) 0.0075(18) 0.0071(19)
O7 0.028(3) 0.037(3) 0.031(3) 0.003(2) 0.009(2) 0.012(2)
U1 0.0124(2) 0.0210(2) 0.0199(2) 0.00298(11) 0.00417(11) 0.00486(12)

_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 O5 1.250(8) 2 ?
C1 O4 1.263(8) . ?
C1 C8 1.494(9) . ?
C2 O3 1.250(8) . ?
C2 O6 1.265(8) 1_455 ?
C2 C3 1.502(10) . ?
C3 C4 1.386(10) . ?
C3 C8 1.390(9) . ?
C4 C5 1.394(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.354(12) . ?
C5 H5 0.9300 . ?
C6 C7 1.384(11) . ?
C6 H6 0.9300 . ?
C7 C8 1.387(10) . ?
C7 H7 0.9300 . ?
O1 U1 1.760(6) . ?
O1W H1WB 0.8500 . ?
O1W H1WC 0.8500 . ?
O2 U1 1.765(6) . ?
O3 U1 2.411(4) . ?
O4 U1 2.351(4) . ?
O5 C1 1.250(8) 2 ?
O5 U1 2.355(5) . ?
O6 C2 1.265(8) 1_655 ?
O6 U1 2.381(4) . ?
O7 U1 2.408(5) . ?
O7 H7A 0.8501 . ?
O7 H7B 0.8500 . ?

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
O5 C1 O4 122.6(6) 2 . ?
O5 C1 C8 117.7(6) 2 . ?
O4 C1 C8 119.7(6) . . ?
O3 C2 O6 120.1(7) . 1_455 ?
O3 C2 C3 121.6(6) . . ?
O6 C2 C3 118.3(6) 1_455 . ?
C4 C3 C8 120.0(6) . . ?
C4 C3 C2 115.8(6) . . ?
C8 C3 C2 124.1(6) . . ?
C3 C4 C5 119.8(7) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C6 C5 C4 120.0(7) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 120.9(7) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C6 C7 C8 120.0(7) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C3 119.3(7) . . ?
C7 C8 C1 117.5(6) . . ?
C3 C8 C1 123.2(6) . . ?
H1WB O1W H1WC 109.5 . . ?
C2 O3 U1 131.3(4) . . ?
C1 O4 U1 132.4(4) . . ?
C1 O5 U1 138.6(4) 2 . ?
C2 O6 U1 142.0(4) 1_655 . ?
U1 O7 H7A 109.3 . . ?
U1 O7 H7B 109.4 . . ?
H7A O7 H7B 109.5 . . ?
O1 U1 O2 177.72(19) . . ?
O1 U1 O4 91.1(2) . . ?
O2 U1 O4 90.0(2) . . ?
O1 U1 O5 88.4(2) . . ?
O2 U1 O5 93.8(2) . . ?
O4 U1 O5 74.65(16) . . ?
O1 U1 O6 88.4(2) . . ?
O2 U1 O6 91.7(2) . . ?
O4 U1 O6 147.38(15) . . ?
O5 U1 O6 72.73(15) . . ?
O1 U1 O7 89.0(2) . . ?
O2 U1 O7 88.9(2) . . ?
O4 U1 O7 140.05(16) . . ?
O5 U1 O7 145.25(16) . . ?
O6 U1 O7 72.56(15) . . ?
O1 U1 O3 84.9(2) . . ?
O2 U1 O3 93.6(2) . . ?
O4 U1 O3 69.10(16) . . ?
O5 U1 O3 142.94(17) . . ?
O6 U1 O3 143.17(16) . . ?
O7 U1 O3 71.13(16) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 C2 C3 C4 -112.3(7) . . . . ?
O6 C2 C3 C4 65.0(8) 1_455 . . . ?
O3 C2 C3 C8 70.9(9) . . . . ?
O6 C2 C3 C8 -111.8(7) 1_455 . . . ?
C8 C3 C4 C5 -1.9(10) . . . . ?
C2 C3 C4 C5 -178.9(6) . . . . ?
C3 C4 C5 C6 2.6(11) . . . . ?
C4 C5 C6 C7 -0.8(12) . . . . ?
C5 C6 C7 C8 -1.5(12) . . . . ?
C6 C7 C8 C3 2.1(10) . . . . ?
C6 C7 C8 C1 -175.3(6) . . . . ?
C4 C3 C8 C7 -0.4(10) . . . . ?
C2 C3 C8 C7 176.3(6) . . . . ?
C4 C3 C8 C1 176.9(6) . . . . ?
C2 C3 C8 C1 -6.4(9) . . . . ?
O5 C1 C8 C7 -32.7(9) 2 . . . ?
O4 C1 C8 C7 146.4(6) . . . . ?
O5 C1 C8 C3 149.9(6) 2 . . . ?
O4 C1 C8 C3 -31.0(9) . . . . ?
O6 C2 O3 U1 158.0(4) 1_455 . . . ?
C3 C2 O3 U1 -24.7(9) . . . . ?
O5 C1 O4 U1 138.6(5) 2 . . . ?
C8 C1 O4 U1 -40.4(8) . . . . ?
C1 O4 U1 O1 169.5(6) . . . . ?
C1 O4 U1 O2 -8.6(6) . . . . ?
C1 O4 U1 O5 -102.5(6) . . . . ?
C1 O4 U1 O6 -101.6(6) . . . . ?
C1 O4 U1 O7 79.7(6) . . . . ?
C1 O4 U1 O3 85.3(6) . . . . ?
C1 O5 U1 O1 99.8(8) 2 . . . ?
C1 O5 U1 O2 -80.8(8) 2 . . . ?
C1 O5 U1 O4 8.2(7) 2 . . . ?
C1 O5 U1 O6 -171.3(8) 2 . . . ?
C1 O5 U1 O7 -174.3(6) 2 . . . ?
C1 O5 U1 O3 20.4(9) 2 . . . ?
C2 O6 U1 O1 135.4(7) 1_655 . . . ?
C2 O6 U1 O2 -46.8(7) 1_655 . . . ?
C2 O6 U1 O4 45.8(8) 1_655 . . . ?
C2 O6 U1 O5 46.7(7) 1_655 . . . ?
C2 O6 U1 O7 -135.1(7) 1_655 . . . ?
C2 O6 U1 O3 -145.1(6) 1_655 . . . ?
C2 O3 U1 O1 -135.4(6) . . . . ?
C2 O3 U1 O2 46.3(6) . . . . ?
C2 O3 U1 O4 -42.3(6) . . . . ?
C2 O3 U1 O5 -54.9(7) . . . . ?
C2 O3 U1 O6 144.0(5) . . . . ?
C2 O3 U1 O7 133.9(6) . . . . ?

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 H1WB O1 0.85 2.07 2.866(8) 154.6 1_565
O7 H7A O1W 0.85 1.98 2.687(7) 140.7 2_666

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         2.194
_refine_diff_density_min         -3.490
_refine_diff_density_rms         0.239
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1057329'
_audit_update_record             
;
2015-04-07 deposited with the CCDC.
2015-05-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H24 O22 U2'
_chemical_formula_weight         1236.57

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.8418(5)
_cell_length_b                   10.4751(7)
_cell_length_c                   13.1315(9)
_cell_angle_alpha                86.1410(10)
_cell_angle_beta                 86.1060(10)
_cell_angle_gamma                71.2520(10)
_cell_volume                     888.09(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4146
_cell_measurement_theta_min      2.64
_cell_measurement_theta_max      30.32

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             576
_exptl_absorpt_coefficient_mu    9.199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1827
_exptl_absorpt_correction_T_max  0.5265
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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            4504
_diffrn_reflns_av_R_equivalents  0.0155
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.56
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3102
_reflns_number_gt                2949
_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)+(0.0237P)²+0.3660P] 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         3102
_refine_ls_number_parameters     255
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0187
_refine_ls_wR_factor_ref         0.0456
_refine_ls_wR_factor_gt          0.0450
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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 0.07994(2) 0.311686(13) 0.846997(9) 0.02152(6) Uani 1 1 d . . .
C1 C -0.0957(6) 0.6605(4) 0.8875(3) 0.0236(8) Uani 1 1 d . . .
C2 C -0.1526(6) 0.7773(4) 0.8109(3) 0.0204(8) Uani 1 1 d . . .
C3 C -0.2165(6) 0.9099(4) 0.8421(3) 0.0258(8) Uani 1 1 d . . .
H3 H -0.2245 0.9264 0.9113 0.031 Uiso 1 1 calc R . .
C4 C -0.2680(6) 1.0172(4) 0.7702(3) 0.0294(9) Uani 1 1 d . . .
H4 H -0.3103 1.1054 0.7912 0.035 Uiso 1 1 calc R . .
C5 C -0.2564(7) 0.9927(4) 0.6664(3) 0.0317(9) Uani 1 1 d . . .
H5 H -0.2899 1.0644 0.6180 0.038 Uiso 1 1 calc R . .
C6 C -0.1942(6) 0.8604(4) 0.6358(3) 0.0247(8) Uani 1 1 d . . .
C7 C -0.1414(6) 0.7529(4) 0.7080(3) 0.0247(8) Uani 1 1 d . . .
H7 H -0.0985 0.6646 0.6871 0.030 Uiso 1 1 calc R . .
C8 C -0.1839(7) 0.8290(4) 0.5265(3) 0.0328(10) Uani 1 1 d . . .
C9 C 0.2236(6) 0.0274(4) 0.8159(3) 0.0258(8) Uani 1 1 d . . .
C10 C 0.3001(6) -0.1223(4) 0.8103(3) 0.0214(8) Uani 1 1 d . . .
C11 C 0.3413(7) -0.1999(4) 0.9017(3) 0.0315(9) Uani 1 1 d . . .
H11 H 0.3174 -0.1576 0.9634 0.038 Uiso 1 1 calc R . .
C12 C 0.4171(7) -0.3385(4) 0.9012(3) 0.0338(10) Uani 1 1 d . . .
H12 H 0.4442 -0.3893 0.9625 0.041 Uiso 1 1 calc R . .
C13 C 0.4530(6) -0.4028(4) 0.8098(3) 0.0301(9) Uani 1 1 d . . .
H13 H 0.5054 -0.4964 0.8095 0.036 Uiso 1 1 calc R . .
C14 C 0.4104(6) -0.3263(4) 0.7182(3) 0.0261(8) Uani 1 1 d . . .
C15 C 0.3309(6) -0.1853(4) 0.7185(3) 0.0253(8) Uani 1 1 d . . .
H15 H 0.2992 -0.1344 0.6575 0.030 Uiso 1 1 calc R . .
C16 C 0.4516(7) -0.3975(4) 0.6220(3) 0.0349(10) Uani 1 1 d . . .
O1 O -0.1748(5) 0.3073(3) 0.8690(2) 0.0358(7) Uani 1 1 d . . .
O2 O 0.3332(5) 0.3147(3) 0.8206(2) 0.0388(7) Uani 1 1 d . . .
O3 O 0.1769(4) 0.1070(3) 0.73741(19) 0.0292(6) Uani 1 1 d . . .
O4 O 0.2051(5) 0.0771(3) 0.9027(2) 0.0372(7) Uani 1 1 d . . .
O5 O 0.1138(5) 0.3154(3) 1.0191(2) 0.0384(8) Uani 1 1 d . . .
O6 O -0.0340(5) 0.5440(3) 0.8563(2) 0.0356(7) Uani 1 1 d . . .
O7 O -0.0182(5) 0.3912(3) 0.6736(2) 0.0420(8) Uani 1 1 d . . .
H7A H -0.0657 0.4769 0.6707 0.063 Uiso 1 1 d R . .
H7C H -0.1106 0.3592 0.6573 0.063 Uiso 1 1 d R . .
O8 O -0.2040(7) 0.9344(3) 0.4624(2) 0.0595(11) Uani 1 1 d . . .
H8 H -0.1921 0.9103 0.4035 0.089 Uiso 1 1 calc R . .
O9 O -0.1622(6) 0.7165(3) 0.4992(2) 0.0503(9) Uani 1 1 d . . .
O10 O 0.3574(6) -0.3275(3) 0.5424(3) 0.0541(10) Uani 1 1 d . . .
H10 H 0.3865 -0.3746 0.4926 0.081 Uiso 1 1 calc R . .
O11 O 0.5678(5) -0.5150(3) 0.6168(2) 0.0458(8) 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 0.03277(9) 0.01363(8) 0.01653(8) -0.00098(5) -0.00175(6) -0.00495(6)
C1 0.031(2) 0.0175(19) 0.0202(19) 0.0013(15) -0.0047(15) -0.0051(16)
C2 0.0259(19) 0.0151(18) 0.0196(18) 0.0014(14) -0.0029(15) -0.0057(15)
C3 0.038(2) 0.021(2) 0.0178(19) -0.0010(15) -0.0012(16) -0.0088(17)
C4 0.041(2) 0.018(2) 0.029(2) -0.0013(17) -0.0008(18) -0.0095(18)
C5 0.043(2) 0.023(2) 0.028(2) 0.0044(17) -0.0020(18) -0.0097(18)
C6 0.034(2) 0.0200(19) 0.0184(18) 0.0028(15) -0.0017(15) -0.0066(16)
C7 0.031(2) 0.021(2) 0.0216(19) -0.0028(16) 0.0010(16) -0.0079(16)
C8 0.047(3) 0.031(2) 0.019(2) 0.0007(17) -0.0002(18) -0.010(2)
C9 0.034(2) 0.018(2) 0.025(2) -0.0016(16) -0.0005(16) -0.0066(16)
C10 0.0268(18) 0.0165(19) 0.0202(19) -0.0012(15) 0.0003(14) -0.0062(15)
C11 0.044(2) 0.022(2) 0.025(2) -0.0029(17) 0.0049(18) -0.0079(18)
C12 0.047(3) 0.021(2) 0.030(2) 0.0099(17) 0.0014(19) -0.0083(19)
C13 0.033(2) 0.0137(19) 0.042(2) 0.0000(17) 0.0009(18) -0.0058(16)
C14 0.027(2) 0.0183(19) 0.034(2) -0.0054(17) -0.0031(17) -0.0081(16)
C15 0.030(2) 0.0161(19) 0.029(2) 0.0008(16) -0.0041(16) -0.0056(16)
C16 0.038(2) 0.025(2) 0.040(2) -0.0105(19) -0.0062(19) -0.0051(19)
O1 0.0384(17) 0.0313(16) 0.0359(17) 0.0005(13) 0.0011(13) -0.0098(13)
O2 0.0370(17) 0.0306(17) 0.0492(19) -0.0021(14) 0.0028(14) -0.0123(14)
O3 0.0502(17) 0.0161(13) 0.0191(14) 0.0001(11) -0.0035(12) -0.0074(12)
O4 0.071(2) 0.0195(15) 0.0167(14) -0.0033(12) -0.0055(14) -0.0070(14)
O5 0.075(2) 0.0196(14) 0.0157(14) -0.0006(11) -0.0066(14) -0.0081(15)
O6 0.064(2) 0.0143(14) 0.0234(15) -0.0010(12) -0.0065(14) -0.0039(13)
O7 0.065(2) 0.0257(16) 0.0261(16) -0.0004(13) -0.0135(15) 0.0002(15)
O8 0.126(3) 0.0335(19) 0.0176(15) 0.0062(14) -0.0048(19) -0.025(2)
O9 0.094(3) 0.0334(19) 0.0228(16) -0.0037(14) 0.0009(16) -0.0197(18)
O10 0.077(2) 0.0313(18) 0.0391(19) -0.0149(15) -0.0213(18) 0.0107(17)
O11 0.059(2) 0.0277(17) 0.0398(18) -0.0138(14) -0.0133(15) 0.0057(15)

_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 1.753(3) . ?
U1 O1 1.762(3) . ?
U1 O5 2.292(3) . ?
U1 O6 2.313(3) . ?
U1 O4 2.407(3) . ?
U1 O7 2.433(3) . ?
U1 O3 2.545(2) . ?
C1 O6 1.245(5) . ?
C1 O5 1.258(5) 2_567 ?
C1 C2 1.498(5) . ?
C2 C7 1.384(5) . ?
C2 C3 1.397(5) . ?
C3 C4 1.388(6) . ?
C4 C5 1.396(6) . ?
C5 C6 1.391(6) . ?
C6 C7 1.393(5) . ?
C6 C8 1.486(5) . ?
C8 O9 1.215(5) . ?
C8 O8 1.319(5) . ?
C9 O4 1.268(5) . ?
C9 O3 1.272(5) . ?
C9 C10 1.490(5) . ?
C10 C15 1.384(5) . ?
C10 C11 1.396(6) . ?
C11 C12 1.376(6) . ?
C12 C13 1.385(6) . ?
C13 C14 1.393(6) . ?
C14 C15 1.400(5) . ?
C14 C16 1.475(6) . ?
C16 O11 1.235(5) . ?
C16 O10 1.315(5) . ?
O5 C1 1.258(5) 2_567 ?

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 177.99(12) . . ?
O2 U1 O5 91.30(14) . . ?
O1 U1 O5 90.66(13) . . ?
O2 U1 O6 89.91(13) . . ?
O1 U1 O6 90.74(13) . . ?
O5 U1 O6 83.35(10) . . ?
O2 U1 O4 91.10(13) . . ?
O1 U1 O4 88.98(13) . . ?
O5 U1 O4 75.77(9) . . ?
O6 U1 O4 159.12(10) . . ?
O2 U1 O7 92.27(14) . . ?
O1 U1 O7 86.03(13) . . ?
O5 U1 O7 159.79(10) . . ?
O6 U1 O7 76.77(10) . . ?
O4 U1 O7 124.02(9) . . ?
O2 U1 O3 86.73(12) . . ?
O1 U1 O3 91.73(12) . . ?
O5 U1 O3 127.92(9) . . ?
O6 U1 O3 148.58(9) . . ?
O4 U1 O3 52.27(8) . . ?
O7 U1 O3 72.17(9) . . ?
O6 C1 O5 122.8(4) . 2_567 ?
O6 C1 C2 118.7(3) . . ?
O5 C1 C2 118.5(3) 2_567 . ?
C7 C2 C3 119.9(4) . . ?
C7 C2 C1 119.3(3) . . ?
C3 C2 C1 120.7(3) . . ?
C4 C3 C2 120.1(3) . . ?
C3 C4 C5 120.0(4) . . ?
C6 C5 C4 119.6(4) . . ?
C5 C6 C7 120.4(3) . . ?
C5 C6 C8 121.7(4) . . ?
C7 C6 C8 118.0(3) . . ?
C2 C7 C6 120.0(3) . . ?
O9 C8 O8 123.3(4) . . ?
O9 C8 C6 122.7(4) . . ?
O8 C8 C6 114.0(4) . . ?
O4 C9 O3 118.7(3) . . ?
O4 C9 C10 118.4(3) . . ?
O3 C9 C10 122.9(3) . . ?
C15 C10 C11 119.8(3) . . ?
C15 C10 C9 122.3(3) . . ?
C11 C10 C9 117.9(3) . . ?
C12 C11 C10 120.6(4) . . ?
C11 C12 C13 120.3(4) . . ?
C12 C13 C14 119.6(4) . . ?
C13 C14 C15 120.3(4) . . ?
C13 C14 C16 118.4(3) . . ?
C15 C14 C16 121.3(4) . . ?
C10 C15 C14 119.5(4) . . ?
O11 C16 O10 122.5(4) . . ?
O11 C16 C14 122.0(4) . . ?
O10 C16 C14 115.6(3) . . ?
C9 O3 U1 91.2(2) . . ?
C9 O4 U1 97.8(2) . . ?
C1 O5 U1 167.2(3) 2_567 . ?
C1 O6 U1 163.8(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 C1 C2 C7 2.0(6) . . . . ?
O5 C1 C2 C7 -177.6(4) 2_567 . . . ?
O6 C1 C2 C3 -178.0(4) . . . . ?
O5 C1 C2 C3 2.5(6) 2_567 . . . ?
C7 C2 C3 C4 -0.2(6) . . . . ?
C1 C2 C3 C4 179.7(4) . . . . ?
C2 C3 C4 C5 0.1(6) . . . . ?
C3 C4 C5 C6 0.4(6) . . . . ?
C4 C5 C6 C7 -0.8(6) . . . . ?
C4 C5 C6 C8 178.6(4) . . . . ?
C3 C2 C7 C6 -0.2(6) . . . . ?
C1 C2 C7 C6 179.9(4) . . . . ?
C5 C6 C7 C2 0.7(6) . . . . ?
C8 C6 C7 C2 -178.7(4) . . . . ?
C5 C6 C8 O9 -168.0(4) . . . . ?
C7 C6 C8 O9 11.4(7) . . . . ?
C5 C6 C8 O8 10.8(6) . . . . ?
C7 C6 C8 O8 -169.8(4) . . . . ?
O4 C9 C10 C15 -178.0(4) . . . . ?
O3 C9 C10 C15 1.7(6) . . . . ?
O4 C9 C10 C11 2.0(6) . . . . ?
O3 C9 C10 C11 -178.3(4) . . . . ?
C15 C10 C11 C12 1.5(6) . . . . ?
C9 C10 C11 C12 -178.4(4) . . . . ?
C10 C11 C12 C13 -0.1(7) . . . . ?
C11 C12 C13 C14 -0.6(7) . . . . ?
C12 C13 C14 C15 -0.2(6) . . . . ?
C12 C13 C14 C16 179.6(4) . . . . ?
C11 C10 C15 C14 -2.3(6) . . . . ?
C9 C10 C15 C14 177.7(4) . . . . ?
C13 C14 C15 C10 1.6(6) . . . . ?
C16 C14 C15 C10 -178.1(4) . . . . ?
C13 C14 C16 O11 -18.7(7) . . . . ?
C15 C14 C16 O11 161.0(4) . . . . ?
C13 C14 C16 O10 161.5(4) . . . . ?
C15 C14 C16 O10 -18.7(6) . . . . ?
O4 C9 O3 U1 -0.2(4) . . . . ?
C10 C9 O3 U1 -180.0(4) . . . . ?
O2 U1 O3 C9 94.1(3) . . . . ?
O1 U1 O3 C9 -87.2(3) . . . . ?
O5 U1 O3 C9 5.0(3) . . . . ?
O6 U1 O3 C9 178.5(2) . . . . ?
O4 U1 O3 C9 0.1(2) . . . . ?
O7 U1 O3 C9 -172.5(3) . . . . ?
O3 C9 O4 U1 0.3(4) . . . . ?
C10 C9 O4 U1 180.0(3) . . . . ?
O2 U1 O4 C9 -85.2(3) . . . . ?
O1 U1 O4 C9 92.8(3) . . . . ?
O5 U1 O4 C9 -176.2(3) . . . . ?
O6 U1 O4 C9 -177.8(3) . . . . ?
O7 U1 O4 C9 8.3(3) . . . . ?
O3 U1 O4 C9 -0.1(2) . . . . ?
O2 U1 O5 C1 127.5(13) . . . 2_567 ?
O1 U1 O5 C1 -52.9(13) . . . 2_567 ?
O6 U1 O5 C1 37.8(13) . . . 2_567 ?
O4 U1 O5 C1 -141.7(13) . . . 2_567 ?
O7 U1 O5 C1 27.4(15) . . . 2_567 ?
O3 U1 O5 C1 -145.6(13) . . . 2_567 ?
O5 C1 O6 U1 3.5(13) 2_567 . . . ?
C2 C1 O6 U1 -176.0(8) . . . . ?
O2 U1 O6 C1 -102.6(11) . . . . ?
O1 U1 O6 C1 79.3(11) . . . . ?
O5 U1 O6 C1 -11.3(11) . . . . ?
O4 U1 O6 C1 -9.7(12) . . . . ?
O7 U1 O6 C1 165.1(11) . . . . ?
O3 U1 O6 C1 173.9(10) . . . . ?

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
O7 H7C O11 0.85 2.25 2.818(5) 124.4 1_465
O8 H8 O3 0.82 1.86 2.673(4) 168.3 2_566
O10 H10 O11 0.82 1.85 2.671(4) 175.1 2_646
C3 H3 O4 0.93 2.45 3.369(4) 168.8 2_567
C13 H13 O1 0.93 2.60 3.360(5) 139.6 1_645
C15 H15 O8 0.93 2.47 3.358(5) 159.3 2_566

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.105
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1057330'
_audit_update_record             
;
2015-04-01 deposited with the CCDC.
2015-05-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H18 N2 O8 U'
_chemical_formula_weight         580.33

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                   6.5012(10)
_cell_length_b                   9.5533(14)
_cell_length_c                   14.649(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.927(2)
_cell_angle_gamma                90.00
_cell_volume                     904.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2535
_cell_measurement_theta_min      2.80
_cell_measurement_theta_max      30.18

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.130
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             544
_exptl_absorpt_coefficient_mu    9.011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.012
_exptl_absorpt_correction_T_max  0.763
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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            4440
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.55
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1592
_reflns_number_gt                1199
_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)+(0.0289P)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         1592
_refine_ls_number_parameters     117
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0220
_refine_ls_wR_factor_ref         0.0530
_refine_ls_wR_factor_gt          0.0503
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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 0.0000 0.0000 0.5000 0.02659(10) Uani 1 2 d S . .
C1 C 0.3653(7) 0.1082(5) 0.3572(3) 0.0342(11) Uani 1 1 d . . .
H1 H 0.4527 0.0327 0.3721 0.041 Uiso 1 1 calc R . .
C2 C 0.2450(7) -0.2523(5) 0.4959(3) 0.0296(10) Uani 1 1 d . . .
C3 C 0.3765(7) -0.3806(4) 0.4976(3) 0.0268(10) Uani 1 1 d . . .
C4 C 0.3090(8) -0.5035(5) 0.5351(4) 0.0358(11) Uani 1 1 d . . .
H4 H 0.1817 -0.5063 0.5588 0.043 Uiso 1 1 calc R . .
C5 C 0.5672(7) -0.3769(5) 0.4628(4) 0.0339(11) Uani 1 1 d . . .
H5 H 0.6127 -0.2943 0.4380 0.041 Uiso 1 1 calc R . .
C7 C 0.2969(11) 0.3274(7) 0.2786(4) 0.073(2) Uani 1 1 d . . .
H7A H 0.2458 0.3257 0.2147 0.109 Uiso 1 1 calc R . .
H7B H 0.3792 0.4099 0.2913 0.109 Uiso 1 1 calc R . .
H7C H 0.1825 0.3282 0.3151 0.109 Uiso 1 1 calc R . .
C8 C 0.6126(11) 0.1887(8) 0.2565(5) 0.081(2) Uani 1 1 d . . .
H8A H 0.7058 0.2633 0.2762 0.121 Uiso 1 1 calc R . .
H8B H 0.5804 0.1932 0.1911 0.121 Uiso 1 1 calc R . .
H8C H 0.6765 0.1004 0.2730 0.121 Uiso 1 1 calc R . .
N1 N 0.4237(7) 0.2029(4) 0.3008(3) 0.0432(11) Uani 1 1 d . . .
O1 O 0.1634(5) 0.0613(4) 0.5961(2) 0.0383(8) Uani 1 1 d . . .
O2 O 0.0829(6) -0.2525(3) 0.5346(3) 0.0486(10) Uani 1 1 d . . .
O3 O 0.3015(5) -0.1415(3) 0.4594(2) 0.0394(9) Uani 1 1 d . . .
O4 O 0.1999(5) 0.1140(4) 0.3918(2) 0.0458(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 0.02405(14) 0.01494(14) 0.04155(15) 0.00096(12) 0.00706(9) 0.00843(10)
C1 0.036(3) 0.026(3) 0.041(3) -0.002(2) 0.006(2) 0.007(2)
C2 0.025(3) 0.018(2) 0.047(3) 0.000(2) 0.011(2) 0.0076(19)
C3 0.024(3) 0.012(2) 0.044(3) 0.002(2) 0.005(2) 0.0070(18)
C4 0.026(2) 0.025(3) 0.058(3) 0.000(2) 0.014(2) 0.011(2)
C5 0.028(3) 0.020(3) 0.056(3) 0.009(2) 0.013(2) 0.004(2)
C7 0.090(6) 0.051(4) 0.079(5) 0.030(3) 0.020(4) 0.021(3)
C8 0.064(5) 0.105(6) 0.080(5) 0.032(4) 0.035(4) 0.010(4)
N1 0.052(3) 0.038(3) 0.042(2) 0.013(2) 0.015(2) 0.006(2)
O1 0.036(2) 0.0253(17) 0.054(2) -0.0023(17) 0.0075(16) 0.0076(15)
O2 0.037(2) 0.0201(19) 0.093(3) 0.0125(19) 0.0288(19) 0.0151(16)
O3 0.035(2) 0.0170(18) 0.069(2) 0.0108(16) 0.0195(18) 0.0109(14)
O4 0.043(2) 0.031(2) 0.067(2) 0.0117(18) 0.0230(19) 0.0147(17)

_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) . ?
U1 O1 1.773(3) 3_556 ?
U1 O4 2.412(3) . ?
U1 O4 2.412(3) 3_556 ?
U1 O3 2.503(3) . ?
U1 O3 2.503(3) 3_556 ?
U1 O2 2.512(3) 3_556 ?
U1 O2 2.512(3) . ?
U1 C2 2.893(4) 3_556 ?
C1 O4 1.236(5) . ?
C1 N1 1.308(6) . ?
C2 O2 1.248(5) . ?
C2 O3 1.258(5) . ?
C2 C3 1.494(6) . ?
C3 C4 1.386(6) . ?
C3 C5 1.388(7) . ?
C4 C5 1.396(6) 3_646 ?
C5 C4 1.396(6) 3_646 ?
C7 N1 1.465(6) . ?
C8 N1 1.453(7) . ?

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 180.0 . 3_556 ?
O1 U1 O4 93.06(14) . . ?
O1 U1 O4 86.94(14) 3_556 . ?
O1 U1 O4 86.94(14) . 3_556 ?
O1 U1 O4 93.06(14) 3_556 3_556 ?
O4 U1 O4 180.00(13) . 3_556 ?
O1 U1 O3 86.99(13) . . ?
O1 U1 O3 93.00(13) 3_556 . ?
O4 U1 O3 66.36(11) . . ?
O4 U1 O3 113.64(11) 3_556 . ?
O1 U1 O3 93.00(13) . 3_556 ?
O1 U1 O3 87.00(13) 3_556 3_556 ?
O4 U1 O3 113.64(11) . 3_556 ?
O4 U1 O3 66.36(11) 3_556 3_556 ?
O3 U1 O3 179.999(1) . 3_556 ?
O1 U1 O2 86.63(15) . 3_556 ?
O1 U1 O2 93.37(15) 3_556 3_556 ?
O4 U1 O2 63.42(11) . 3_556 ?
O4 U1 O2 116.58(11) 3_556 3_556 ?
O3 U1 O2 128.87(10) . 3_556 ?
O3 U1 O2 51.13(10) 3_556 3_556 ?
O1 U1 O2 93.37(15) . . ?
O1 U1 O2 86.63(15) 3_556 . ?
O4 U1 O2 116.58(11) . . ?
O4 U1 O2 63.42(11) 3_556 . ?
O3 U1 O2 51.13(10) . . ?
O3 U1 O2 128.87(10) 3_556 . ?
O2 U1 O2 180.0 3_556 . ?
O1 U1 C2 89.67(14) . 3_556 ?
O1 U1 C2 90.33(14) 3_556 3_556 ?
O4 U1 C2 88.44(12) . 3_556 ?
O4 U1 C2 91.56(12) 3_556 3_556 ?
O3 U1 C2 154.33(12) . 3_556 ?
O3 U1 C2 25.67(11) 3_556 3_556 ?
O2 U1 C2 25.46(11) 3_556 3_556 ?
O2 U1 C2 154.54(11) . 3_556 ?
O4 C1 N1 123.3(5) . . ?
O2 C2 O3 119.5(4) . . ?
O2 C2 C3 120.0(4) . . ?
O3 C2 C3 120.4(4) . . ?
C4 C3 C5 119.9(4) . . ?
C4 C3 C2 119.8(4) . . ?
C5 C3 C2 120.3(4) . . ?
C3 C4 C5 119.7(5) . 3_646 ?
C3 C5 C4 120.4(4) . 3_646 ?
C1 N1 C8 122.1(5) . . ?
C1 N1 C7 120.6(5) . . ?
C8 N1 C7 117.3(5) . . ?
C2 O2 U1 94.6(3) . . ?
C2 O3 U1 94.8(3) . . ?
C1 O4 U1 143.1(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.369
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.107
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1057331'
_audit_update_record             
;
2015-04-01 deposited with the CCDC.
2015-05-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H10 O6 U'
_chemical_formula_weight         512.25

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'
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/m

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

_cell_length_a                   7.6328(12)
_cell_length_b                   17.461(3)
_cell_length_c                   5.3032(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.692(2)
_cell_angle_gamma                90.00
_cell_volume                     703.3(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2311
_cell_measurement_theta_min      2.92
_cell_measurement_theta_max      30.37

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             468
_exptl_absorpt_coefficient_mu    11.563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1951
_exptl_absorpt_correction_T_max  0.4581
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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            1738
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         2.33
_diffrn_reflns_theta_max         25.00
_reflns_number_total             649
_reflns_number_gt                649
_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)+(0.0419P)²+0.2899P] 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         649
_refine_ls_number_parameters     53
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0259
_refine_ls_wR_factor_ref         0.0660
_refine_ls_wR_factor_gt          0.0660
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_restrained_S_all      1.170
_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 0.0000 0.0000 0.0000 0.02816(19) Uani 1 4 d S . .
C1 C 0.0000 0.1270(5) 0.5000 0.0304(17) Uani 1 2 d S . .
C2 C 0.0000 0.2120(5) 0.5000 0.0293(17) Uani 1 2 d S . .
C3 C 0.0775(9) 0.2515(4) 0.7065(15) 0.0421(15) Uani 1 1 d . . .
H3 H 0.1294 0.2246 0.8458 0.050 Uiso 1 1 calc R . .
C4 C 0.0788(11) 0.3305(5) 0.709(2) 0.061(2) Uani 1 1 d . . .
H4 H 0.1316 0.3570 0.8485 0.074 Uiso 1 1 calc R . .
C5 C 0.0000 0.3698(6) 0.5000 0.068(4) Uani 1 2 d S . .
H5 H 0.0000 0.4231 0.5000 0.082 Uiso 1 2 calc SR . .
O1 O 0.2286(9) 0.0000 0.0908(17) 0.0490(18) Uani 1 2 d S . .
O2 O -0.0413(8) 0.0924(3) 0.2967(10) 0.0479(12) 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 0.0460(3) 0.0156(2) 0.0217(3) 0.000 -0.00221(17) 0.000
C1 0.043(4) 0.021(4) 0.028(4) 0.000 0.010(3) 0.000
C2 0.034(3) 0.022(4) 0.034(5) 0.000 0.012(3) 0.000
C3 0.051(3) 0.033(3) 0.042(4) -0.007(3) 0.005(3) -0.007(3)
C4 0.070(4) 0.035(4) 0.083(7) -0.024(4) 0.022(5) -0.014(3)
C5 0.072(7) 0.021(5) 0.117(13) 0.000 0.039(8) 0.000
O1 0.045(3) 0.037(4) 0.061(5) 0.000 -0.011(3) 0.000
O2 0.080(3) 0.029(2) 0.035(3) -0.011(2) 0.006(2) -0.002(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 O1 1.763(7) 5 ?
U1 O1 1.763(7) . ?
U1 O2 2.297(5) 6 ?
U1 O2 2.297(5) 5 ?
U1 O2 2.297(5) 2 ?
U1 O2 2.297(5) . ?
C1 O2 1.248(7) . ?
C1 O2 1.248(7) 2_556 ?
C1 C2 1.484(11) . ?
C2 C3 1.377(8) 2_556 ?
C2 C3 1.377(8) . ?
C3 C4 1.380(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.389(12) . ?
C4 H4 0.9300 . ?
C5 C4 1.389(12) 2_556 ?
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
O1 U1 O1 180.0 5 . ?
O1 U1 O2 89.3(3) 5 6 ?
O1 U1 O2 90.7(3) . 6 ?
O1 U1 O2 90.7(3) 5 5 ?
O1 U1 O2 89.3(3) . 5 ?
O2 U1 O2 90.7(3) 6 5 ?
O1 U1 O2 90.7(3) 5 2 ?
O1 U1 O2 89.3(3) . 2 ?
O2 U1 O2 180.00(17) 6 2 ?
O2 U1 O2 89.3(3) 5 2 ?
O1 U1 O2 89.3(3) 5 . ?
O1 U1 O2 90.7(3) . . ?
O2 U1 O2 89.3(3) 6 . ?
O2 U1 O2 180.0 5 . ?
O2 U1 O2 90.7(3) 2 . ?
O2 C1 O2 122.2(8) . 2_556 ?
O2 C1 C2 118.9(4) . . ?
O2 C1 C2 118.9(4) 2_556 . ?
C3 C2 C3 119.9(9) 2_556 . ?
C3 C2 C1 120.0(4) 2_556 . ?
C3 C2 C1 120.0(4) . . ?
C2 C3 C4 120.7(8) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C3 C4 C5 119.0(9) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C4 C5 C4 120.8(10) 2_556 . ?
C4 C5 H5 119.6 2_556 . ?
C4 C5 H5 119.6 . . ?
C1 O2 U1 153.0(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 C3 12.9(4) . . . 2_556 ?
O2 C1 C2 C3 -167.1(4) 2_556 . . 2_556 ?
O2 C1 C2 C3 -167.1(4) . . . . ?
O2 C1 C2 C3 12.9(4) 2_556 . . . ?
C3 C2 C3 C4 -0.1(5) 2_556 . . . ?
C1 C2 C3 C4 179.9(5) . . . . ?
C2 C3 C4 C5 0.3(10) . . . . ?
C3 C4 C5 C4 -0.1(5) . . . 2_556 ?
O2 C1 O2 U1 -46.8(9) 2_556 . . . ?
C2 C1 O2 U1 133.2(9) . . . . ?
O1 U1 O2 C1 153.1(10) 5 . . . ?
O1 U1 O2 C1 -26.9(10) . . . . ?
O2 U1 O2 C1 63.7(11) 6 . . . ?
O2 U1 O2 C1 -99(2) 5 . . . ?
O2 U1 O2 C1 -116.3(11) 2 . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.069
_refine_diff_density_min         -2.279
_refine_diff_density_rms         0.207
