# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_shx97
_database_code_depnum_ccdc_archive 'CCDC 1024949'
_audit_update_record             
;
2015-01-28 deposited with the CCDC.
2015-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H10 O13 U2, 9(H2 O)'
_chemical_formula_sum            'C16 H28 O22 U2'
_chemical_formula_weight         1048.3

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'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   9.6655(19)
_cell_length_b                   11.002(2)
_cell_length_c                   15.304(3)
_cell_angle_alpha                108.95(3)
_cell_angle_beta                 95.14(3)
_cell_angle_gamma                109.32(3)
_cell_volume                     1416.7(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    11274
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             788
_exptl_absorpt_coefficient_mu    11.465
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.146
_exptl_absorpt_correction_T_max  0.179
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295(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  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 0
_diffrn_standards_number         0
_diffrn_standards_interval_count image
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            11635
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_sigmaI/netI    0.0735
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         25.35
_reflns_number_total             5165
_reflns_number_gt                3859
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL-97

_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.The least-squares refinement
of the structural model was performed under geometry restraints and 
displacement parameter restraints such as ISOR, SHEL, FMAP and DFIX.
ISOR 0.01
SHEL 999 0.83
FMAP 2
DFIX 0.84 O9 H91 O9 H92
DFIX 1.4 H91 H92
;

_platon_squeeze_details          
;
The solvent molecules in the structure were highly disordered. Efforts to 
locate and refine the solvent peaks were in vain. The SQUEEZE routine was
used to remove the scattering from the highly disordered solvent molecules,
the 184 electrons can be accounted for by 9 water molecules per formula unit,
and the reported formula, formula weight, density, F(000), etc. include the
solvents.
;

_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)+(0.0862P)²+15.2636P] 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         5165
_refine_ls_number_parameters     286
_refine_ls_number_restraints     189
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0521
_refine_ls_wR_factor_ref         0.1778
_refine_ls_wR_factor_gt          0.1405
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.118
_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 0.88670(6) 0.18904(5) 0.11375(4) 0.0316(2) Uani 1 1 d U . .
U2 U 0.14972(7) -0.33593(6) 0.49976(4) 0.0479(2) Uani 1 1 d U . .
O1 O 1.0525(12) 0.2643(13) 0.1991(9) 0.056(3) Uani 1 1 d U . .
O2 O 0.7238(16) 0.1144(14) 0.0281(10) 0.072(4) Uani 1 1 d U . .
O3 O 0.8256(11) 0.3857(10) 0.2053(8) 0.038(2) Uani 1 1 d U . .
O4 O 0.9393(12) 0.4076(10) 0.0892(7) 0.040(2) Uani 1 1 d U . .
C1 C 0.8836(16) 0.4583(14) 0.1576(11) 0.037(3) Uani 1 1 d U . .
C2 C 0.8851(16) 0.6006(14) 0.1832(11) 0.034(3) Uani 1 1 d U . .
C3 C 0.9087(16) 0.6668(14) 0.1190(11) 0.034(3) Uani 1 1 d U . .
H3 H 0.9244 0.6215 0.0602 0.041 Uiso 1 1 calc R . .
C4 C 0.9091(16) 0.7981(14) 0.1420(11) 0.036(3) Uani 1 1 d U . .
C5 C 0.887(2) 0.8652(17) 0.2300(12) 0.052(4) Uani 1 1 d U . .
H5 H 0.8831 0.9528 0.2448 0.062 Uiso 1 1 calc R . .
C6 C 0.871(2) 0.8045(19) 0.2954(13) 0.057(4) Uani 1 1 d U . .
H6 H 0.8644 0.8535 0.3562 0.069 Uiso 1 1 calc R . .
C7 C 0.8632(19) 0.6670(16) 0.2699(12) 0.046(4) Uani 1 1 d U . .
H7 H 0.8436 0.6218 0.3119 0.055 Uiso 1 1 calc R . .
C8 C 0.9305(19) 0.8689(15) 0.0734(12) 0.044(4) Uani 1 1 d U . .
O5 O 0.9040(16) 0.9753(12) 0.0884(9) 0.062(3) Uani 1 1 d U . .
O6 O 0.9726(17) 0.8177(13) 0.0005(10) 0.067(3) Uani 1 1 d U . .
O7 O 0.2883(16) -0.3991(17) 0.5146(11) 0.082(4) Uani 1 1 d U . .
O8 O 0.0163(16) -0.2638(15) 0.4876(10) 0.074(4) Uani 1 1 d U . .
O9 O -0.0236(14) -0.5580(14) 0.4066(8) 0.060(3) Uani 1 1 d DU . .
H91 H 0.00(2) -0.58(2) 0.354(6) 0.090 Uiso 1 1 d D . .
H92 H -0.104(14) -0.54(2) 0.403(12) 0.090 Uiso 1 1 d D . .
O10 O 0.1760(12) -0.3698(12) 0.3362(8) 0.052(3) Uani 1 1 d U . .
O11 O 0.3253(15) -0.1717(14) 0.4452(10) 0.071(4) Uani 1 1 d U . .
C9 C 0.6785(17) 0.0796(16) 0.2729(11) 0.040(3) Uani 1 1 d U . .
C10 C 0.5515(15) -0.0535(14) 0.2462(10) 0.034(3) Uani 1 1 d U . .
C11 C 0.4805(16) -0.0905(15) 0.3139(11) 0.039(3) Uani 1 1 d U . .
H11 H 0.5158 -0.0317 0.3774 0.046 Uiso 1 1 calc R . .
C12 C 0.3579(15) -0.2139(15) 0.2877(11) 0.036(3) Uani 1 1 d U . .
C13 C 0.2999(19) -0.2982(18) 0.1923(12) 0.050(4) Uani 1 1 d U . .
H13 H 0.2158 -0.3802 0.1744 0.060 Uiso 1 1 calc R . .
C14 C 0.367(2) -0.2603(19) 0.1243(13) 0.057(5) Uani 1 1 d U . .
H14 H 0.3286 -0.3173 0.0606 0.068 Uiso 1 1 calc R . .
C15 C 0.4923(18) -0.1363(17) 0.1510(12) 0.048(4) Uani 1 1 d U . .
H15 H 0.5360 -0.1094 0.1051 0.057 Uiso 1 1 calc R . .
C16 C 0.2812(18) -0.2522(16) 0.3602(12) 0.046(4) Uani 1 1 d U . .
O12 O 0.7463(13) 0.1128(11) 0.2132(9) 0.051(3) Uani 1 1 d U . .
O13 O 0.724(2) 0.157(2) 0.3555(13) 0.112(6) Uani 1 1 d U . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 1.717(14) . ?
U1 O1 1.733(12) . ?
U1 O12 2.304(10) . ?
U1 O6 2.306(12) 2_765 ?
U1 O5 2.321(10) 1_545 ?
U1 O4 2.449(9) . ?
U1 O3 2.453(9) . ?
U1 C1 2.828(14) . ?
U2 O7 1.730(15) . ?
U2 O8 1.748(15) . ?
U2 O9 2.315(11) 2_546 ?
U2 O13 2.316(19) 2_656 ?
U2 O9 2.326(13) . ?
U2 O10 2.457(11) . ?
U2 O11 2.459(11) . ?
U2 C16 2.831(16) . ?
U2 U2 3.8100(18) 2_546 ?
O3 C1 1.281(16) . ?
O4 C1 1.271(17) . ?
C1 C2 1.479(18) . ?
C2 C7 1.36(2) . ?
C2 C3 1.393(19) . ?
C3 C4 1.370(18) . ?
C3 H3 0.9300 . ?
C4 C5 1.38(2) . ?
C4 C8 1.49(2) . ?
C5 C6 1.36(2) . ?
C5 H5 0.9300 . ?
C6 C7 1.41(2) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 O5 1.234(17) . ?
C8 O6 1.246(18) . ?
O5 U1 2.321(10) 1_565 ?
O6 U1 2.306(12) 2_765 ?
O9 U2 2.315(11) 2_546 ?
O9 H91 0.84(2) . ?
O9 H92 0.85(2) . ?
O10 C16 1.264(18) . ?
O11 C16 1.25(2) . ?
C9 O13 1.21(2) . ?
C9 O12 1.251(17) . ?
C9 C10 1.47(2) . ?
C10 C15 1.39(2) . ?
C10 C11 1.388(18) . ?
C11 C12 1.38(2) . ?
C11 H11 0.9300 . ?
C12 C13 1.39(2) . ?
C12 C16 1.48(2) . ?
C13 C14 1.38(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.40(2) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
O13 U2 2.316(19) 2_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
O2 U1 O1 179.3(6) . . ?
O2 U1 O12 88.1(6) . . ?
O1 U1 O12 92.5(5) . . ?
O2 U1 O6 90.6(6) . 2_765 ?
O1 U1 O6 88.6(6) . 2_765 ?
O12 U1 O6 158.3(4) . 2_765 ?
O2 U1 O5 92.0(6) . 1_545 ?
O1 U1 O5 87.8(5) . 1_545 ?
O12 U1 O5 77.8(4) . 1_545 ?
O6 U1 O5 80.6(4) 2_765 1_545 ?
O2 U1 O4 89.5(5) . . ?
O1 U1 O4 90.3(5) . . ?
O12 U1 O4 127.9(3) . . ?
O6 U1 O4 73.7(4) 2_765 . ?
O5 U1 O4 154.3(4) 1_545 . ?
O2 U1 O3 94.0(5) . . ?
O1 U1 O3 86.5(5) . . ?
O12 U1 O3 74.7(3) . . ?
O6 U1 O3 127.0(4) 2_765 . ?
O5 U1 O3 151.6(4) 1_545 . ?
O4 U1 O3 53.5(3) . . ?
O2 U1 C1 92.3(5) . . ?
O1 U1 C1 87.8(5) . . ?
O12 U1 C1 101.5(4) . . ?
O6 U1 C1 100.2(4) 2_765 . ?
O5 U1 C1 175.5(5) 1_545 . ?
O4 U1 C1 26.7(4) . . ?
O3 U1 C1 26.9(4) . . ?
O7 U2 O8 177.2(7) . . ?
O7 U2 O9 89.9(6) . 2_546 ?
O8 U2 O9 91.3(6) . 2_546 ?
O7 U2 O13 86.5(8) . 2_656 ?
O8 U2 O13 91.1(7) . 2_656 ?
O9 U2 O13 82.9(5) 2_546 2_656 ?
O7 U2 O9 91.6(6) . . ?
O8 U2 O9 91.3(6) . . ?
O9 U2 O9 69.6(5) 2_546 . ?
O13 U2 O9 152.5(5) 2_656 . ?
O7 U2 O10 89.8(6) . . ?
O8 U2 O10 90.6(5) . . ?
O9 U2 O10 143.9(4) 2_546 . ?
O13 U2 O10 133.1(4) 2_656 . ?
O9 U2 O10 74.3(4) . . ?
O7 U2 O11 87.8(6) . . ?
O8 U2 O11 90.3(6) . . ?
O9 U2 O11 163.4(5) 2_546 . ?
O13 U2 O11 80.6(5) 2_656 . ?
O9 U2 O11 126.8(4) . . ?
O10 U2 O11 52.6(4) . . ?
O7 U2 C16 88.3(6) . . ?
O8 U2 C16 90.8(6) . . ?
O9 U2 C16 170.1(5) 2_546 . ?
O13 U2 C16 106.7(5) 2_656 . ?
O9 U2 C16 100.7(4) . . ?
O10 U2 C16 26.5(4) . . ?
O11 U2 C16 26.1(4) . . ?
O7 U2 U2 90.9(5) . 2_546 ?
O8 U2 U2 91.6(5) . 2_546 ?
O9 U2 U2 34.9(3) 2_546 2_546 ?
O13 U2 U2 117.8(4) 2_656 2_546 ?
O9 U2 U2 34.7(3) . 2_546 ?
O10 U2 U2 109.0(3) . 2_546 ?
O11 U2 U2 161.5(3) . 2_546 ?
C16 U2 U2 135.4(3) . 2_546 ?
C1 O3 U1 93.1(8) . . ?
C1 O4 U1 93.6(8) . . ?
O4 C1 O3 119.8(12) . . ?
O4 C1 C2 120.9(12) . . ?
O3 C1 C2 119.3(13) . . ?
O4 C1 U1 59.8(7) . . ?
O3 C1 U1 60.0(7) . . ?
C2 C1 U1 178.3(11) . . ?
C7 C2 C3 119.9(13) . . ?
C7 C2 C1 119.9(13) . . ?
C3 C2 C1 120.2(13) . . ?
C4 C3 C2 120.5(13) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 119.4(14) . . ?
C3 C4 C8 121.1(13) . . ?
C5 C4 C8 119.5(13) . . ?
C6 C5 C4 120.9(15) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C7 119.4(16) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.3 . . ?
C2 C7 C6 119.7(16) . . ?
C2 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
O5 C8 O6 121.0(14) . . ?
O5 C8 C4 119.9(13) . . ?
O6 C8 C4 119.1(12) . . ?
C8 O5 U1 172.3(12) . 1_565 ?
C8 O6 U1 157.9(11) . 2_765 ?
U2 O9 U2 110.4(5) 2_546 . ?
U2 O9 H91 139(10) 2_546 . ?
U2 O9 H91 108(10) . . ?
U2 O9 H92 77(10) 2_546 . ?
U2 O9 H92 101(10) . . ?
H91 O9 H92 112(4) . . ?
C16 O10 U2 93.5(10) . . ?
C16 O11 U2 93.8(9) . . ?
O13 C9 O12 118.7(15) . . ?
O13 C9 C10 119.5(14) . . ?
O12 C9 C10 121.7(14) . . ?
C15 C10 C11 119.7(14) . . ?
C15 C10 C9 119.1(13) . . ?
C11 C10 C9 120.8(13) . . ?
C12 C11 C10 120.5(14) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 119.8(14) . . ?
C11 C12 C16 120.3(14) . . ?
C13 C12 C16 119.8(13) . . ?
C14 C13 C12 120.2(16) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 120.0(17) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C10 C15 C14 119.8(15) . . ?
C10 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
O11 C16 O10 120.0(14) . . ?
O11 C16 C12 120.2(13) . . ?
O10 C16 C12 119.6(14) . . ?
O11 C16 U2 60.1(8) . . ?
O10 C16 U2 60.0(8) . . ?
C12 C16 U2 175.7(12) . . ?
C9 O12 U1 175.2(12) . . ?
C9 O13 U2 167.0(13) . 2_656 ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.499 0.499 0.510 525 184 ' '
_platon_squeeze_void_probe_radius 1.20

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.528
_refine_diff_density_min         -3.378
_refine_diff_density_rms         0.331
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shx97
_database_code_depnum_ccdc_archive 'CCDC 1024950'
_audit_update_record             
;
2015-01-28 deposited with the CCDC.
2015-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H8 N2 O17 U2, C6 H16 N, H2 O'
_chemical_formula_sum            'C22 H26 N3 O18 U2'
_chemical_formula_weight         1096.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   10.663(2)
_cell_length_b                   11.090(2)
_cell_length_c                   14.718(3)
_cell_angle_alpha                106.88(3)
_cell_angle_beta                 95.76(3)
_cell_angle_gamma                112.99(3)
_cell_volume                     1487.4(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    14774
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1014
_exptl_absorpt_coefficient_mu    10.960
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.225
_exptl_absorpt_correction_T_max  0.300
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295(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  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 0
_diffrn_standards_number         0
_diffrn_standards_interval_count image
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            14776
_diffrn_reflns_av_R_equivalents  0.0928
_diffrn_reflns_av_sigmaI/netI    0.1009
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         27.48
_reflns_number_total             6754
_reflns_number_gt                5828
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL-97

_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.The least-squares refinement
of the structural model was performed under geometry restraints and 
displacement parameter restraints such as FMAP and DFIX.
FMAP 2
BOND $H
HTAB
DFIX 0.85 N3 H31
DFIX 1.89 O18 H31
DFIX 0.84 O18 H181 O18 O182
DFIX 1.40 H181 H182
;

_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)+(0.0365P)²+2.1101P] 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         6754
_refine_ls_number_parameters     409
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.0988
_refine_ls_wR_factor_gt          0.0934
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_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 0.60813(2) 0.830751(19) 0.889417(14) 0.01085(8) Uani 1 1 d . . .
U2 U 1.34101(2) 1.351379(19) 0.509817(13) 0.00980(8) Uani 1 1 d . . .
O1 O 0.4316(5) 0.7470(4) 0.8191(3) 0.0169(10) Uani 1 1 d . . .
O2 O 0.7837(5) 0.9143(4) 0.9612(3) 0.0171(10) Uani 1 1 d . . .
O3 O 0.6474(5) 0.6359(4) 0.7880(3) 0.0141(9) Uani 1 1 d . . .
O4 O 0.5732(5) 0.6122(4) 0.9181(3) 0.0182(10) Uani 1 1 d . . .
C1 C 0.6098(7) 0.5656(6) 0.8434(4) 0.0150(13) Uani 1 1 d . . .
C2 C 0.6100(7) 0.4215(5) 0.8152(4) 0.0122(13) Uani 1 1 d . . .
C3 C 0.6570(7) 0.3763(6) 0.7326(4) 0.0141(13) Uani 1 1 d . . .
H3A H 0.6849 0.4312 0.6944 0.017 Uiso 1 1 calc R . .
C4 C 0.6610(7) 0.2499(6) 0.7091(4) 0.0154(13) Uani 1 1 d . . .
C5 C 0.6262(7) 0.1667(6) 0.7667(4) 0.0131(13) Uani 1 1 d . . .
H5A H 0.6321 0.0818 0.7497 0.016 Uiso 1 1 calc R . .
C6 C 0.5824(7) 0.2150(5) 0.8504(4) 0.0124(13) Uani 1 1 d . . .
C7 C 0.5738(7) 0.3432(5) 0.8730(4) 0.0123(13) Uani 1 1 d . . .
H7A H 0.5431 0.3750 0.9281 0.015 Uiso 1 1 calc R . .
C8 C 0.5515(7) 0.1333(6) 0.9157(4) 0.0142(13) Uani 1 1 d . . .
O5 O 0.4686(6) 0.1498(5) 0.9684(3) 0.0217(11) Uani 1 1 d . . .
O6 O 0.6042(5) 0.0490(4) 0.9136(3) 0.0198(11) Uani 1 1 d . . .
N1 N 0.7009(6) 0.1967(5) 0.6189(3) 0.0149(11) Uani 1 1 d . . .
O7 O 0.6847(6) 0.0737(5) 0.5916(3) 0.0278(13) Uani 1 1 d . . .
O8 O 0.7503(5) 0.2759(4) 0.5756(3) 0.0201(11) Uani 1 1 d . . .
O9 O 1.4471(5) 1.2701(4) 0.5371(3) 0.0148(9) Uani 1 1 d . . .
O10 O 1.2327(5) 1.4304(4) 0.4822(3) 0.0162(10) Uani 1 1 d . . .
O11 O 0.6991(5) 0.8957(4) 0.7640(3) 0.0126(9) Uani 1 1 d . . .
O12 O 0.7868(5) 0.8364(4) 0.6367(3) 0.0145(10) Uani 1 1 d . . .
C9 C 0.7899(7) 0.9251(6) 0.7153(4) 0.0124(12) Uani 1 1 d . . .
C10 C 0.9097(6) 1.0669(5) 0.7510(4) 0.0107(12) Uani 1 1 d . . .
C11 C 0.9399(7) 1.1617(6) 0.8465(4) 0.0150(14) Uani 1 1 d . . .
H11A H 0.8840 1.1381 0.8890 0.018 Uiso 1 1 calc R . .
C12 C 1.0549(7) 1.2907(6) 0.8754(4) 0.0151(14) Uani 1 1 d . . .
C13 C 1.1414(7) 1.3314(6) 0.8165(4) 0.0150(13) Uani 1 1 d . . .
H13A H 1.2198 1.4181 0.8395 0.018 Uiso 1 1 calc R . .
C14 C 1.1081(7) 1.2378(6) 0.7201(4) 0.0129(13) Uani 1 1 d . . .
C15 C 0.9937(7) 1.1096(6) 0.6881(4) 0.0146(14) Uani 1 1 d . . .
H15A H 0.9712 1.0496 0.6236 0.017 Uiso 1 1 calc R . .
C16 C 1.1945(7) 1.2795(6) 0.6500(4) 0.0141(13) Uani 1 1 d . . .
O13 O 1.1488(5) 1.1980(4) 0.5605(3) 0.0168(11) Uani 1 1 d . . .
O14 O 1.3069(5) 1.3911(4) 0.6791(3) 0.0164(10) Uani 1 1 d . . .
N2 N 1.0851(6) 1.3901(5) 0.9757(4) 0.0179(13) Uani 1 1 d . . .
O15 O 1.1510(5) 1.5176(4) 0.9901(3) 0.0237(12) Uani 1 1 d . . .
O16 O 1.0444(6) 1.3454(5) 1.0388(3) 0.0302(14) Uani 1 1 d . . .
O17 O 1.5210(5) 1.5732(4) 0.5959(3) 0.0125(9) Uani 1 1 d . . .
H171 H 1.5690 1.5714 0.6412 0.015 Uiso 1 1 d R . .
H172 H 1.4890 1.6268 0.6174 0.015 Uiso 1 1 d R . .
O18 O 0.3947(5) 0.7691(5) 0.6261(3) 0.0212(11) Uani 1 1 d D . .
H181 H 0.3837 0.7847 0.5741 0.025 Uiso 1 1 d RD . .
H182 H 0.4723 0.8213 0.6613 0.025 Uiso 1 1 d RD . .
N3 N 0.1621(6) 0.7679(6) 0.6938(4) 0.0223(13) Uani 1 1 d D . .
H31 H 0.242(4) 0.772(8) 0.684(5) 0.027 Uiso 1 1 d D . .
C17 C 0.0591(8) 0.6183(7) 0.6489(5) 0.0258(16) Uani 1 1 d . . .
H17A H 0.0700 0.5798 0.5836 0.031 Uiso 1 1 calc R . .
H17B H -0.0349 0.6120 0.6424 0.031 Uiso 1 1 calc R . .
C18 C 0.0747(9) 0.5276(7) 0.7087(6) 0.0327(18) Uani 1 1 d . . .
H18A H 0.0046 0.4324 0.6763 0.039 Uiso 1 1 calc R . .
H18B H 0.0628 0.5642 0.7731 0.039 Uiso 1 1 calc R . .
H18C H 0.1663 0.5305 0.7134 0.039 Uiso 1 1 calc R . .
C19 C 0.1363(8) 0.8467(7) 0.6312(5) 0.0255(16) Uani 1 1 d . . .
H19A H 0.1240 0.7930 0.5631 0.031 Uiso 1 1 calc R . .
H19B H 0.0498 0.8541 0.6378 0.031 Uiso 1 1 calc R . .
C20 C 0.2531(9) 0.9915(8) 0.6575(6) 0.0334(19) Uani 1 1 d . . .
H20A H 0.2302 1.0360 0.6157 0.040 Uiso 1 1 calc R . .
H20B H 0.3387 0.9851 0.6490 0.040 Uiso 1 1 calc R . .
H20C H 0.2652 1.0460 0.7245 0.040 Uiso 1 1 calc R . .
C21 C 0.1693(7) 0.8331(7) 0.8002(4) 0.0220(15) Uani 1 1 d . . .
H21A H 0.2400 0.9301 0.8249 0.026 Uiso 1 1 calc R . .
H21B H 0.1987 0.7842 0.8362 0.026 Uiso 1 1 calc R . .
C22 C 0.0299(8) 0.8288(8) 0.8191(5) 0.0296(17) Uani 1 1 d . . .
H22A H 0.0404 0.8705 0.8881 0.036 Uiso 1 1 calc R . .
H22B H -0.0405 0.7331 0.7954 0.036 Uiso 1 1 calc R . .
H22C H 0.0018 0.8801 0.7856 0.036 Uiso 1 1 calc R . .


_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 1.778(5) . ?
U1 O1 1.779(5) . ?
U1 O5 2.306(4) 2_667 ?
U1 O11 2.335(4) . ?
U1 O6 2.360(4) 1_565 ?
U1 O3 2.456(4) . ?
U1 O4 2.472(4) . ?
U1 C1 2.827(6) . ?
U2 O9 1.780(5) . ?
U2 O10 1.781(5) . ?
U2 O17 2.314(4) . ?
U2 O12 2.330(4) 2_776 ?
U2 O17 2.353(4) 2_886 ?
U2 O13 2.444(4) . ?
U2 O14 2.491(4) . ?
U2 C16 2.822(5) . ?
U2 U2 3.8031(16) 2_886 ?
O3 C1 1.274(7) . ?
O4 C1 1.243(7) . ?
C1 C2 1.531(8) . ?
C2 C7 1.365(8) . ?
C2 C3 1.395(8) . ?
C3 C4 1.362(9) . ?
C3 H3A 0.9300 . ?
C4 C5 1.398(8) . ?
C4 N1 1.466(7) . ?
C5 C6 1.397(8) . ?
C5 H5A 0.9300 . ?
C6 C7 1.404(8) . ?
C6 C8 1.479(8) . ?
C7 H7A 0.9300 . ?
C8 O6 1.260(8) . ?
C8 O5 1.264(7) . ?
O5 U1 2.306(4) 2_667 ?
O6 U1 2.360(4) 1_545 ?
N1 O8 1.219(6) . ?
N1 O7 1.239(6) . ?
O11 C9 1.260(7) . ?
O12 C9 1.270(6) . ?
O12 U2 2.330(4) 2_776 ?
C9 C10 1.482(7) . ?
C10 C11 1.403(7) . ?
C10 C15 1.405(7) . ?
C11 C12 1.380(8) . ?
C11 H11A 0.9300 . ?
C12 C13 1.367(8) . ?
C12 N2 1.477(7) . ?
C13 C14 1.404(7) . ?
C13 H13A 0.9300 . ?
C14 C15 1.369(8) . ?
C14 C16 1.504(7) . ?
C15 H15A 0.9300 . ?
C16 O14 1.257(7) . ?
C16 O13 1.275(7) . ?
N2 O16 1.216(6) . ?
N2 O15 1.248(6) . ?
O17 U2 2.353(4) 2_886 ?
O17 H171 0.8100 . ?
O17 H172 0.7999 . ?
O18 H181 0.8385 . ?
O18 H182 0.8083 . ?
N3 C17 1.480(8) . ?
N3 C21 1.502(7) . ?
N3 C19 1.513(9) . ?
N3 H31 0.860(17) . ?
C17 C18 1.559(11) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C20 1.504(10) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.525(10) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 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 179.19(16) . . ?
O2 U1 O5 88.86(18) . 2_667 ?
O1 U1 O5 90.35(19) . 2_667 ?
O2 U1 O11 87.59(17) . . ?
O1 U1 O11 93.20(17) . . ?
O5 U1 O11 159.11(16) 2_667 . ?
O2 U1 O6 91.6(2) . 1_565 ?
O1 U1 O6 88.5(2) . 1_565 ?
O5 U1 O6 83.41(15) 2_667 1_565 ?
O11 U1 O6 76.12(14) . 1_565 ?
O2 U1 O3 90.87(18) . . ?
O1 U1 O3 89.50(18) . . ?
O5 U1 O3 127.71(14) 2_667 . ?
O11 U1 O3 72.95(14) . . ?
O6 U1 O3 148.84(12) 1_565 . ?
O2 U1 O4 89.99(18) . . ?
O1 U1 O4 89.67(19) . . ?
O5 U1 O4 74.93(15) 2_667 . ?
O11 U1 O4 125.63(13) . . ?
O6 U1 O4 158.24(12) 1_565 . ?
O3 U1 O4 52.78(12) . . ?
O2 U1 C1 90.6(2) . . ?
O1 U1 C1 89.4(2) . . ?
O5 U1 C1 100.96(16) 2_667 . ?
O11 U1 C1 99.66(15) . . ?
O6 U1 C1 175.16(14) 1_565 . ?
O3 U1 C1 26.75(14) . . ?
O4 U1 C1 26.03(14) . . ?
O9 U2 O10 179.18(17) . . ?
O9 U2 O17 91.74(18) . . ?
O10 U2 O17 89.02(18) . . ?
O9 U2 O12 91.55(18) . 2_776 ?
O10 U2 O12 87.94(18) . 2_776 ?
O17 U2 O12 150.76(13) . 2_776 ?
O9 U2 O17 89.36(17) . 2_886 ?
O10 U2 O17 91.19(17) . 2_886 ?
O17 U2 O17 70.85(15) . 2_886 ?
O12 U2 O17 80.15(13) 2_776 2_886 ?
O9 U2 O13 90.85(17) . . ?
O10 U2 O13 88.41(18) . . ?
O17 U2 O13 131.12(12) . . ?
O12 U2 O13 77.85(13) 2_776 . ?
O17 U2 O13 158.00(13) 2_886 . ?
O9 U2 O14 87.37(17) . . ?
O10 U2 O14 92.48(17) . . ?
O17 U2 O14 78.14(13) . . ?
O12 U2 O14 131.04(13) 2_776 . ?
O17 U2 O14 148.70(14) 2_886 . ?
O13 U2 O14 53.24(13) . . ?
O9 U2 C16 89.48(19) . . ?
O10 U2 C16 90.02(19) . . ?
O17 U2 C16 104.42(15) . . ?
O12 U2 C16 104.65(16) 2_776 . ?
O17 U2 C16 175.09(16) 2_886 . ?
O13 U2 C16 26.81(15) . . ?
O14 U2 C16 26.44(16) . . ?
O9 U2 U2 90.66(13) . 2_886 ?
O10 U2 U2 90.14(13) . 2_886 ?
O17 U2 U2 35.76(9) . 2_886 ?
O12 U2 U2 115.16(10) 2_776 2_886 ?
O17 U2 U2 35.09(10) 2_886 2_886 ?
O13 U2 U2 166.86(9) . 2_886 ?
O14 U2 U2 113.80(10) . 2_886 ?
C16 U2 U2 140.17(12) . 2_886 ?
C1 O3 U1 93.0(3) . . ?
C1 O4 U1 93.1(3) . . ?
O4 C1 O3 121.0(6) . . ?
O4 C1 C2 120.7(5) . . ?
O3 C1 C2 118.2(5) . . ?
O4 C1 U1 60.8(3) . . ?
O3 C1 U1 60.2(3) . . ?
C2 C1 U1 178.3(4) . . ?
C7 C2 C3 120.7(5) . . ?
C7 C2 C1 120.7(5) . . ?
C3 C2 C1 118.4(5) . . ?
C4 C3 C2 118.4(5) . . ?
C4 C3 H3A 120.8 . . ?
C2 C3 H3A 120.8 . . ?
C3 C4 C5 122.9(5) . . ?
C3 C4 N1 119.0(5) . . ?
C5 C4 N1 118.1(5) . . ?
C6 C5 C4 118.0(6) . . ?
C6 C5 H5A 121.0 . . ?
C4 C5 H5A 121.0 . . ?
C5 C6 C7 119.3(5) . . ?
C5 C6 C8 119.5(5) . . ?
C7 C6 C8 121.2(5) . . ?
C2 C7 C6 120.7(5) . . ?
C2 C7 H7A 119.6 . . ?
C6 C7 H7A 119.6 . . ?
O6 C8 O5 123.9(5) . . ?
O6 C8 C6 119.2(5) . . ?
O5 C8 C6 116.9(6) . . ?
C8 O5 U1 153.5(5) . 2_667 ?
C8 O6 U1 157.4(4) . 1_545 ?
O8 N1 O7 123.5(5) . . ?
O8 N1 C4 118.5(5) . . ?
O7 N1 C4 118.0(5) . . ?
C9 O11 U1 155.4(5) . . ?
C9 O12 U2 149.8(4) . 2_776 ?
O11 C9 O12 122.8(5) . . ?
O11 C9 C10 120.0(5) . . ?
O12 C9 C10 117.1(5) . . ?
C11 C10 C15 118.8(5) . . ?
C11 C10 C9 121.3(5) . . ?
C15 C10 C9 119.9(5) . . ?
C12 C11 C10 118.2(5) . . ?
C12 C11 H11A 120.9 . . ?
C10 C11 H11A 120.9 . . ?
C13 C12 C11 123.7(5) . . ?
C13 C12 N2 118.5(5) . . ?
C11 C12 N2 117.7(5) . . ?
C12 C13 C14 117.8(5) . . ?
C12 C13 H13A 121.1 . . ?
C14 C13 H13A 121.1 . . ?
C15 C14 C13 120.2(5) . . ?
C15 C14 C16 119.4(5) . . ?
C13 C14 C16 120.4(5) . . ?
C14 C15 C10 121.2(5) . . ?
C14 C15 H15A 119.4 . . ?
C10 C15 H15A 119.4 . . ?
O14 C16 O13 121.8(5) . . ?
O14 C16 C14 120.9(5) . . ?
O13 C16 C14 117.4(5) . . ?
O14 C16 U2 61.9(3) . . ?
O13 C16 U2 59.8(3) . . ?
C14 C16 U2 176.5(5) . . ?
C16 O13 U2 93.4(3) . . ?
C16 O14 U2 91.6(3) . . ?
O16 N2 O15 123.7(5) . . ?
O16 N2 C12 119.5(5) . . ?
O15 N2 C12 116.9(5) . . ?
U2 O17 U2 109.15(15) . 2_886 ?
U2 O17 H171 109.9 . . ?
U2 O17 H171 109.9 2_886 . ?
U2 O17 H172 109.8 . . ?
U2 O17 H172 109.8 2_886 . ?
H171 O17 H172 108.3 . . ?
H181 O18 H182 111.7 . . ?
C17 N3 C21 113.5(5) . . ?
C17 N3 C19 109.2(6) . . ?
C21 N3 C19 114.3(5) . . ?
C17 N3 H31 107(5) . . ?
C21 N3 H31 113(4) . . ?
C19 N3 H31 99(5) . . ?
N3 C17 C18 113.5(6) . . ?
N3 C17 H17A 108.9 . . ?
C18 C17 H17A 108.9 . . ?
N3 C17 H17B 108.9 . . ?
C18 C17 H17B 108.9 . . ?
H17A C17 H17B 107.7 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 N3 113.5(6) . . ?
C20 C19 H19A 108.9 . . ?
N3 C19 H19A 108.9 . . ?
C20 C19 H19B 108.9 . . ?
N3 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N3 C21 C22 113.2(6) . . ?
N3 C21 H21A 108.9 . . ?
C22 C21 H21A 108.9 . . ?
N3 C21 H21B 108.9 . . ?
C22 C21 H21B 108.9 . . ?
H21A C21 H21B 107.8 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         4.278
_refine_diff_density_min         -3.588
_refine_diff_density_rms         0.303
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shx97
_database_code_depnum_ccdc_archive 'CCDC 1024951'
_audit_update_record             
;
2015-01-28 deposited with the CCDC.
2015-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H12 N2 O13 U2, C6 H16 N'
_chemical_formula_sum            'C22 H28 N3 O13 U2'
_chemical_formula_weight         1018.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   9.6416(19)
_cell_length_b                   10.973(2)
_cell_length_c                   15.997(3)
_cell_angle_alpha                109.52(3)
_cell_angle_beta                 91.56(3)
_cell_angle_gamma                109.61(3)
_cell_volume                     1484.0(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    14242
_cell_measurement_theta_min      3.02
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.151
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             938
_exptl_absorpt_coefficient_mu    10.964
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.112
_exptl_absorpt_correction_T_max  0.191
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295(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  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 0
_diffrn_standards_number         0
_diffrn_standards_interval_count image
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            14242
_diffrn_reflns_av_R_equivalents  0.1198
_diffrn_reflns_av_sigmaI/netI    0.1581
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.48
_reflns_number_total             6699
_reflns_number_gt                3943
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL-97

_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.The least-squares refinement
of the structural model was performed under geometry restraints and 
displacement parameter restraints such as ISOR, SIMU, SADI, CONF and DFIX. 
ISOR 0.01 o2
CONF O9 C9 C10 C11
CONF O10 C9 C10 C15
CONF O12 C16 C14 C15
CONF O11 C16 C14 C13
CONF O4 C1 C2 C3
CONF O3 C1 C2 C7
CONF O5 C8 C6 C5
CONF O6 C8 C6 C7
SIMU 0.02 0.04 3.8 n3 > c22b
DFIX 1.42 0.01 n3 c17 n3 c19 n3 c21 n3 c17b n3 c19b n3 c21b
DFIX 1.55 0.01 c17 c18 c19 c20 c21 c22 c17b c18b c19b c20b c21b c22b
SADI 0.01 c17 c19 c17 c21 c19 c21 c17b c19b c17b c21b c19b c21b
SADI 0.01 n3 c18 n3 c20 n3 c22 n3 c18b n3 c20b n3 c22b
;

_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)+(0.0500P)²+18.0000P] 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     SHELXL
_refine_ls_extinction_coef       0.0019(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6699
_refine_ls_number_parameters     417
_refine_ls_number_restraints     438
_refine_ls_R_factor_all          0.1189
_refine_ls_R_factor_gt           0.0761
_refine_ls_wR_factor_ref         0.1980
_refine_ls_wR_factor_gt          0.1603
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      0.993
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001

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 0.10097(5) 0.29971(4) 0.37978(3) 0.03626(11) Uani 1 1 d . . .
U2 U 0.85495(5) 0.82900(4) -0.00320(3) 0.04236(13) Uani 1 1 d . . .
O1 O -0.0603(10) 0.2365(7) 0.3067(6) 0.055(2) Uani 1 1 d . . .
O2 O 0.2646(10) 0.3609(7) 0.4531(6) 0.049(2) Uani 1 1 d U . .
O3 O 0.1450(8) 0.0911(7) 0.2858(6) 0.047(2) Uani 1 1 d . . .
O4 O 0.0379(9) 0.0800(7) 0.4030(6) 0.045(2) Uani 1 1 d . . .
C1 C 0.0886(12) 0.0242(11) 0.3330(8) 0.039(3) Uani 1 1 d . . .
C2 C 0.0845(12) -0.1202(10) 0.3124(8) 0.037(3) Uani 1 1 d . . .
C3 C 0.0938(14) -0.1978(10) 0.2264(8) 0.049(3) Uani 1 1 d . . .
H31 H 0.1033 -0.1580 0.1829 0.058 Uiso 1 1 calc R . .
C4 C 0.0897(14) -0.3323(12) 0.2022(9) 0.048(3) Uani 1 1 d . . .
C5 C 0.0742(14) -0.3932(11) 0.2674(8) 0.052(3) Uani 1 1 d . . .
H51 H 0.0650 -0.4853 0.2524 0.062 Uiso 1 1 calc R . .
C6 C 0.0728(13) -0.3121(10) 0.3554(8) 0.046(3) Uani 1 1 d . . .
C7 C 0.0735(12) -0.1789(9) 0.3793(7) 0.036(3) Uani 1 1 d . . .
H71 H 0.0668 -0.1292 0.4379 0.044 Uiso 1 1 calc R . .
C8 C 0.0710(13) -0.3732(10) 0.4304(9) 0.045(3) Uani 1 1 d . . .
O5 O 0.0323(12) -0.3163(9) 0.4997(6) 0.075(3) Uani 1 1 d . . .
O6 O 0.1037(10) -0.4773(7) 0.4136(6) 0.062(2) Uani 1 1 d . . .
N1 N 0.0890(17) -0.4116(12) 0.1142(8) 0.095(5) Uani 1 1 d . . .
H13 H 0.0912 -0.3773 0.0729 0.114 Uiso 1 1 calc R . .
H12 H 0.0864 -0.4951 0.1007 0.114 Uiso 1 1 calc R . .
O7 O 0.9959(10) 0.7699(9) 0.0147(7) 0.067(3) Uani 1 1 d . . .
O8 O 0.7111(11) 0.8809(10) -0.0232(7) 0.069(3) Uani 1 1 d . . .
O9 O 0.6768(11) 0.6558(9) 0.0473(6) 0.066(3) Uani 1 1 d . . .
O10 O 0.8017(10) 0.8579(8) 0.1491(6) 0.050(2) Uani 1 1 d . . .
C9 C 0.7076(14) 0.7375(12) 0.1283(8) 0.045(3) Uani 1 1 d . . .
C10 C 0.6265(13) 0.6972(11) 0.1981(9) 0.047(3) Uani 1 1 d . . .
C11 C 0.6846(13) 0.7762(12) 0.2849(9) 0.044(3) Uani 1 1 d . . .
H111 H 0.7697 0.8559 0.2991 0.053 Uiso 1 1 calc R . .
C12 C 0.6160(14) 0.7380(12) 0.3548(8) 0.042(3) Uani 1 1 d . . .
C13 C 0.4874(13) 0.6202(11) 0.3308(9) 0.050(3) Uani 1 1 d . . .
H131 H 0.4392 0.5944 0.3752 0.060 Uiso 1 1 calc R . .
C14 C 0.4298(12) 0.5398(10) 0.2404(8) 0.040(3) Uani 1 1 d . . .
C15 C 0.5000(13) 0.5786(11) 0.1744(8) 0.040(3) Uani 1 1 d . . .
H151 H 0.4622 0.5252 0.1142 0.048 Uiso 1 1 calc R . .
C16 C 0.2901(12) 0.4113(11) 0.2160(8) 0.039(3) Uani 1 1 d . . .
O11 O 0.2245(11) 0.3605(9) 0.1389(6) 0.062(3) Uani 1 1 d . . .
O12 O 0.2437(9) 0.3679(7) 0.2770(6) 0.050(2) Uani 1 1 d . . .
N2 N 0.6784(14) 0.8168(13) 0.4428(9) 0.073(4) Uani 1 1 d . . .
H22 H 0.6378 0.7936 0.4851 0.088 Uiso 1 1 calc R . .
H21 H 0.7583 0.8894 0.4556 0.088 Uiso 1 1 calc R . .
O13 O 1.0023(10) 0.9439(7) -0.0864(6) 0.054(2) Uani 1 1 d . . .
H132 H 1.0471 0.9105 -0.1219 0.065 Uiso 1 1 d R . .
H133 H 0.9502 0.9436 -0.1263 0.065 Uiso 1 1 d R . .
N3 N 0.5877(6) 0.1515(4) 0.2450(3) 0.162(4) Uani 1 1 d DU . .
H3A H 0.6652 0.1576 0.2134 0.194 Uiso 0.546(12) 1 calc PR A 1
H3B H 0.5145 0.1163 0.1968 0.194 Uiso 0.454(12) 1 d PR A 2
C17 C 0.4539(11) 0.0575(7) 0.1843(7) 0.162(5) Uani 0.546(12) 1 d PDU A 1
H17A H 0.4327 0.1081 0.1493 0.194 Uiso 0.546(12) 1 calc PR A 1
H17B H 0.3764 0.0464 0.2216 0.194 Uiso 0.546(12) 1 calc PR A 1
C18 C 0.424(2) -0.0906(11) 0.1157(13) 0.154(8) Uani 0.546(12) 1 d PDU A 1
H18A H 0.3270 -0.1261 0.0803 0.232 Uiso 0.546(12) 1 calc PR A 1
H18B H 0.4271 -0.1504 0.1472 0.232 Uiso 0.546(12) 1 calc PR A 1
H18C H 0.4982 -0.0871 0.0771 0.232 Uiso 0.546(12) 1 calc PR A 1
C19 C 0.6132(12) 0.1004(8) 0.3129(5) 0.168(5) Uani 0.546(12) 1 d PDU A 1
H19A H 0.7111 0.1632 0.3464 0.202 Uiso 0.546(12) 1 calc PR A 1
H19B H 0.6236 0.0124 0.2811 0.202 Uiso 0.546(12) 1 calc PR A 1
C20 C 0.514(2) 0.0743(17) 0.3850(8) 0.172(8) Uani 0.546(12) 1 d PDU A 1
H20A H 0.5578 0.0374 0.4207 0.258 Uiso 0.546(12) 1 calc PR A 1
H20B H 0.4163 0.0092 0.3559 0.258 Uiso 0.546(12) 1 calc PR A 1
H20C H 0.5078 0.1603 0.4229 0.258 Uiso 0.546(12) 1 calc PR A 1
C21 C 0.5820(13) 0.2864(6) 0.2839(9) 0.162(5) Uani 0.546(12) 1 d PDU A 1
H21A H 0.5351 0.2859 0.3367 0.194 Uiso 0.546(12) 1 calc PR A 1
H21B H 0.5106 0.2903 0.2419 0.194 Uiso 0.546(12) 1 calc PR A 1
C22 C 0.711(2) 0.4293(8) 0.314(3) 0.162(8) Uani 0.546(12) 1 d PDU A 1
H22A H 0.6733 0.5015 0.3414 0.243 Uiso 0.546(12) 1 calc PR A 1
H22B H 0.7537 0.4422 0.2625 0.243 Uiso 0.546(12) 1 calc PR A 1
H22C H 0.7859 0.4328 0.3563 0.243 Uiso 0.546(12) 1 calc PR A 1
C17B C 0.7262(9) 0.2071(9) 0.2172(6) 0.172(5) Uani 0.454(12) 1 d PDU A 2
H17C H 0.7889 0.1637 0.2344 0.206 Uiso 0.454(12) 1 calc PR A 2
H17D H 0.7675 0.3041 0.2565 0.206 Uiso 0.454(12) 1 calc PR A 2
C18B C 0.7595(17) 0.207(3) 0.1234(8) 0.122(6) Uani 0.454(12) 1 d PDU A 2
H18D H 0.8601 0.2685 0.1285 0.183 Uiso 0.454(12) 1 calc PR A 2
H18E H 0.6918 0.2382 0.0988 0.183 Uiso 0.454(12) 1 calc PR A 2
H18F H 0.7472 0.1148 0.0847 0.183 Uiso 0.454(12) 1 calc PR A 2
C19B C 0.5827(12) 0.0384(7) 0.2714(7) 0.167(5) Uani 0.454(12) 1 d PDU A 2
H19C H 0.6843 0.0608 0.2975 0.201 Uiso 0.454(12) 1 calc PR A 2
H19D H 0.5621 -0.0405 0.2158 0.201 Uiso 0.454(12) 1 calc PR A 2
C20B C 0.483(3) -0.0190(14) 0.3347(10) 0.172(8) Uani 0.454(12) 1 d PDU A 2
H20D H 0.4991 -0.0998 0.3368 0.258 Uiso 0.454(12) 1 calc PR A 2
H20E H 0.3803 -0.0435 0.3124 0.258 Uiso 0.454(12) 1 calc PR A 2
H20F H 0.5088 0.0508 0.3939 0.258 Uiso 0.454(12) 1 calc PR A 2
C21B C 0.5590(12) 0.2564(9) 0.3151(7) 0.167(5) Uani 0.454(12) 1 d PDU A 2
H21C H 0.4740 0.2068 0.3374 0.201 Uiso 0.454(12) 1 calc PR A 2
H21D H 0.5234 0.3066 0.2854 0.201 Uiso 0.454(12) 1 calc PR A 2
C22B C 0.667(3) 0.3696(18) 0.4000(10) 0.176(8) Uani 0.454(12) 1 d PDU A 2
H22D H 0.6109 0.4100 0.4421 0.264 Uiso 0.454(12) 1 calc PR A 2
H22E H 0.7366 0.4405 0.3836 0.264 Uiso 0.454(12) 1 calc PR A 2
H22F H 0.7198 0.3286 0.4270 0.264 Uiso 0.454(12) 1 calc PR A 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 1.703(9) . ?
U1 O2 1.726(9) . ?
U1 O6 2.314(7) 1_565 ?
U1 O12 2.326(8) . ?
U1 O5 2.336(9) 2_556 ?
U1 O4 2.439(7) . ?
U1 O3 2.463(8) . ?
U1 C1 2.820(11) . ?
U2 O8 1.726(11) . ?
U2 O7 1.745(10) . ?
U2 O13 2.315(7) 2_775 ?
U2 O13 2.324(8) . ?
U2 O11 2.334(9) 2_665 ?
U2 O10 2.441(9) . ?
U2 O9 2.475(8) . ?
U2 C9 2.840(12) . ?
U2 U2 3.8208(17) 2_775 ?
O3 C1 1.236(13) . ?
O4 C1 1.281(14) . ?
C1 C2 1.493(15) . ?
C2 C3 1.378(16) . ?
C2 C7 1.412(15) . ?
C3 C4 1.381(16) . ?
C3 H31 0.9300 . ?
C4 N1 1.385(16) . ?
C4 C5 1.401(18) . ?
C5 C6 1.394(16) . ?
C5 H51 0.9300 . ?
C6 C7 1.379(14) . ?
C6 C8 1.555(18) . ?
C7 H71 0.9300 . ?
C8 O5 1.215(14) . ?
C8 O6 1.231(13) . ?
O5 U1 2.336(9) 2_556 ?
O6 U1 2.314(7) 1_545 ?
N1 H13 0.8600 . ?
N1 H12 0.8600 . ?
O9 C9 1.263(14) . ?
O10 C9 1.251(13) . ?
C9 C10 1.484(16) . ?
C10 C11 1.350(17) . ?
C10 C15 1.380(14) . ?
C11 C12 1.426(17) . ?
C11 H111 0.9300 . ?
C12 N2 1.372(16) . ?
C12 C13 1.386(15) . ?
C13 C14 1.397(17) . ?
C13 H131 0.9300 . ?
C14 C15 1.379(15) . ?
C14 C16 1.510(14) . ?
C15 H151 0.9300 . ?
C16 O11 1.221(15) . ?
C16 O12 1.254(14) . ?
O11 U2 2.334(9) 2_665 ?
N2 H22 0.8600 . ?
N2 H21 0.8600 . ?
O13 U2 2.315(7) 2_775 ?
O13 H132 0.7900 . ?
O13 H133 0.8000 . ?
N3 C17B 1.421(7) . ?
N3 C21 1.422(7) . ?
N3 C21B 1.424(7) . ?
N3 C19B 1.426(7) . ?
N3 C17 1.428(7) . ?
N3 C19 1.430(7) . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9099 . ?
C17 C18 1.550(8) . ?
C17 H3B 0.6725 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C20 1.555(9) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.546(9) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C17B C18B 1.542(8) . ?
C17B H17C 0.9700 . ?
C17B H17D 0.9700 . ?
C18B H18D 0.9600 . ?
C18B H18E 0.9600 . ?
C18B H18F 0.9600 . ?
C19B C20B 1.554(9) . ?
C19B H19C 0.9700 . ?
C19B H19D 0.9700 . ?
C20B H20D 0.9600 . ?
C20B H20E 0.9600 . ?
C20B H20F 0.9600 . ?
C21B C22B 1.549(9) . ?
C21B H21C 0.9700 . ?
C21B H21D 0.9700 . ?
C22B H22D 0.9600 . ?
C22B H22E 0.9600 . ?
C22B H22F 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
O1 U1 O2 179.0(3) . . ?
O1 U1 O6 89.7(3) . 1_565 ?
O2 U1 O6 91.3(4) . 1_565 ?
O1 U1 O12 92.1(4) . . ?
O2 U1 O12 88.0(4) . . ?
O6 U1 O12 79.0(3) 1_565 . ?
O1 U1 O5 90.4(4) . 2_556 ?
O2 U1 O5 89.9(4) . 2_556 ?
O6 U1 O5 80.2(3) 1_565 2_556 ?
O12 U1 O5 159.0(3) . 2_556 ?
O1 U1 O4 91.0(3) . . ?
O2 U1 O4 88.1(3) . . ?
O6 U1 O4 153.6(3) 1_565 . ?
O12 U1 O4 127.4(3) . . ?
O5 U1 O4 73.4(3) 2_556 . ?
O1 U1 O3 85.9(3) . . ?
O2 U1 O3 93.1(3) . . ?
O6 U1 O3 153.4(3) 1_565 . ?
O12 U1 O3 75.0(3) . . ?
O5 U1 O3 126.0(3) 2_556 . ?
O4 U1 O3 52.9(3) . . ?
O1 U1 C1 88.1(3) . . ?
O2 U1 C1 90.9(3) . . ?
O6 U1 C1 177.8(3) 1_565 . ?
O12 U1 C1 100.7(3) . . ?
O5 U1 C1 100.2(3) 2_556 . ?
O4 U1 C1 27.0(3) . . ?
O3 U1 C1 26.0(3) . . ?
O8 U2 O7 177.8(4) . . ?
O8 U2 O13 89.9(4) . 2_775 ?
O7 U2 O13 92.3(4) . 2_775 ?
O8 U2 O13 92.3(4) . . ?
O7 U2 O13 88.6(4) . . ?
O13 U2 O13 69.1(3) 2_775 . ?
O8 U2 O11 92.1(4) . 2_665 ?
O7 U2 O11 86.0(4) . 2_665 ?
O13 U2 O11 153.4(3) 2_775 2_665 ?
O13 U2 O11 84.3(3) . 2_665 ?
O8 U2 O10 89.8(4) . . ?
O7 U2 O10 90.7(4) . . ?
O13 U2 O10 73.5(3) 2_775 . ?
O13 U2 O10 142.5(3) . . ?
O11 U2 O10 133.0(3) 2_665 . ?
O8 U2 O9 88.1(4) . . ?
O7 U2 O9 90.5(4) . . ?
O13 U2 O9 125.8(3) 2_775 . ?
O13 U2 O9 165.1(3) . . ?
O11 U2 O9 80.8(3) 2_665 . ?
O10 U2 O9 52.4(3) . . ?
O8 U2 C9 89.0(4) . . ?
O7 U2 C9 90.5(4) . . ?
O13 U2 C9 99.5(3) 2_775 . ?
O13 U2 C9 168.5(3) . . ?
O11 U2 C9 107.1(3) 2_665 . ?
O10 U2 C9 26.0(3) . . ?
O9 U2 C9 26.4(3) . . ?
O8 U2 U2 91.3(3) . 2_775 ?
O7 U2 U2 90.6(3) . 2_775 ?
O13 U2 U2 34.6(2) 2_775 2_775 ?
O13 U2 U2 34.5(2) . 2_775 ?
O11 U2 U2 118.8(2) 2_665 2_775 ?
O10 U2 U2 108.10(18) . 2_775 ?
O9 U2 U2 160.5(2) . 2_775 ?
C9 U2 U2 134.1(2) . 2_775 ?
C1 O3 U1 93.4(7) . . ?
C1 O4 U1 93.4(6) . . ?
O3 C1 O4 120.3(10) . . ?
O3 C1 C2 121.0(10) . . ?
O4 C1 C2 118.6(10) . . ?
O3 C1 U1 60.7(6) . . ?
O4 C1 U1 59.7(6) . . ?
C2 C1 U1 177.5(9) . . ?
C3 C2 C7 118.9(10) . . ?
C3 C2 C1 119.5(11) . . ?
C7 C2 C1 121.5(10) . . ?
C2 C3 C4 122.8(12) . . ?
C2 C3 H31 118.6 . . ?
C4 C3 H31 118.6 . . ?
C3 C4 N1 121.7(12) . . ?
C3 C4 C5 118.8(11) . . ?
N1 C4 C5 119.3(11) . . ?
C6 C5 C4 118.3(10) . . ?
C6 C5 H51 120.8 . . ?
C4 C5 H51 120.8 . . ?
C7 C6 C5 122.8(11) . . ?
C7 C6 C8 118.1(10) . . ?
C5 C6 C8 119.0(10) . . ?
C6 C7 C2 118.1(10) . . ?
C6 C7 H71 120.9 . . ?
C2 C7 H71 120.9 . . ?
O5 C8 O6 125.5(13) . . ?
O5 C8 C6 116.7(10) . . ?
O6 C8 C6 117.7(11) . . ?
C8 O5 U1 157.0(8) . 2_556 ?
C8 O6 U1 165.5(8) . 1_545 ?
C4 N1 H13 120.0 . . ?
C4 N1 H12 120.0 . . ?
H13 N1 H12 120.0 . . ?
C9 O9 U2 93.2(7) . . ?
C9 O10 U2 95.1(7) . . ?
O10 C9 O9 119.3(11) . . ?
O10 C9 C10 119.2(11) . . ?
O9 C9 C10 121.3(10) . . ?
O10 C9 U2 58.9(6) . . ?
O9 C9 U2 60.5(6) . . ?
C10 C9 U2 176.2(9) . . ?
C11 C10 C15 121.5(11) . . ?
C11 C10 C9 117.8(10) . . ?
C15 C10 C9 120.6(11) . . ?
C10 C11 C12 120.2(10) . . ?
C10 C11 H111 119.9 . . ?
C12 C11 H111 119.9 . . ?
N2 C12 C13 122.1(12) . . ?
N2 C12 C11 119.8(11) . . ?
C13 C12 C11 118.1(11) . . ?
C12 C13 C14 120.5(11) . . ?
C12 C13 H131 119.7 . . ?
C14 C13 H131 119.7 . . ?
C15 C14 C13 119.9(9) . . ?
C15 C14 C16 120.6(11) . . ?
C13 C14 C16 119.5(10) . . ?
C10 C15 C14 119.7(11) . . ?
C10 C15 H151 120.1 . . ?
C14 C15 H151 120.1 . . ?
O11 C16 O12 123.8(10) . . ?
O11 C16 C14 117.9(11) . . ?
O12 C16 C14 118.2(11) . . ?
C16 O11 U2 147.7(9) . 2_665 ?
C16 O12 U1 164.3(8) . . ?
C12 N2 H22 120.0 . . ?
C12 N2 H21 120.0 . . ?
H22 N2 H21 120.0 . . ?
U2 O13 U2 110.9(3) 2_775 . ?
U2 O13 H132 111.6 2_775 . ?
U2 O13 H132 123.5 . . ?
U2 O13 H133 109.4 2_775 . ?
U2 O13 H133 109.4 . . ?
H132 O13 H133 89.4 . . ?
C17B N3 C21 90.8(7) . . ?
C17B N3 C21B 111.1(5) . . ?
C21 N3 C21B 28.0(8) . . ?
C17B N3 C19B 111.1(6) . . ?
C21 N3 C19B 138.5(7) . . ?
C21B N3 C19B 111.0(5) . . ?
C17B N3 C17 123.8(7) . . ?
C21 N3 C17 110.9(6) . . ?
C21B N3 C17 110.9(7) . . ?
C19B N3 C17 86.2(6) . . ?
C17B N3 C19 108.3(7) . . ?
C21 N3 C19 110.8(6) . . ?
C21B N3 C19 85.7(7) . . ?
C19B N3 C19 29.9(5) . . ?
C17 N3 C19 110.5(5) . . ?
C17B N3 H3A 19.2 . . ?
C21 N3 H3A 108.2 . . ?
C21B N3 H3A 130.2 . . ?
C19B N3 H3A 101.1 . . ?
C17 N3 H3A 108.2 . . ?
C19 N3 H3A 108.2 . . ?
C17B N3 H3B 108.0 . . ?
C21 N3 H3B 98.8 . . ?
C21B N3 H3B 108.9 . . ?
C19B N3 H3B 106.6 . . ?
C17 N3 H3B 21.7 . . ?
C19 N3 H3B 132.1 . . ?
H3A N3 H3B 96.5 . . ?
N3 C17 C18 127.9(10) . . ?
N3 C17 H3B 30.0 . . ?
C18 C17 H3B 131.6 . . ?
N3 C17 H17A 105.3 . . ?
C18 C17 H17A 105.3 . . ?
H3B C17 H17A 76.3 . . ?
N3 C17 H17B 105.3 . . ?
C18 C17 H17B 105.3 . . ?
H3B C17 H17B 120.9 . . ?
H17A C17 H17B 106.0 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 C20 127.8(9) . . ?
N3 C19 H19A 105.3 . . ?
C20 C19 H19A 105.3 . . ?
N3 C19 H19B 105.3 . . ?
C20 C19 H19B 105.3 . . ?
H19A C19 H19B 106.0 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N3 C21 C22 128.8(10) . . ?
N3 C21 H21A 105.1 . . ?
C22 C21 H21A 105.1 . . ?
N3 C21 H21B 105.1 . . ?
C22 C21 H21B 105.1 . . ?
H21A C21 H21B 105.9 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N3 C17B C18B 129.5(8) . . ?
N3 C17B H17C 104.9 . . ?
C18B C17B H17C 104.9 . . ?
N3 C17B H17D 104.9 . . ?
C18B C17B H17D 104.9 . . ?
H17C C17B H17D 105.8 . . ?
C17B C18B H18D 109.5 . . ?
C17B C18B H18E 109.5 . . ?
H18D C18B H18E 109.5 . . ?
C17B C18B H18F 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
N3 C19B C20B 128.1(9) . . ?
N3 C19B H19C 105.3 . . ?
C20B C19B H19C 105.3 . . ?
N3 C19B H19D 105.3 . . ?
C20B C19B H19D 105.3 . . ?
H19C C19B H19D 106.0 . . ?
C19B C20B H20D 109.5 . . ?
C19B C20B H20E 109.5 . . ?
H20D C20B H20E 109.5 . . ?
C19B C20B H20F 109.5 . . ?
H20D C20B H20F 109.5 . . ?
H20E C20B H20F 109.5 . . ?
N3 C21B C22B 128.5(10) . . ?
N3 C21B H21C 105.2 . . ?
C22B C21B H21C 105.2 . . ?
N3 C21B H21D 105.2 . . ?
C22B C21B H21D 105.2 . . ?
H21C C21B H21D 105.9 . . ?
C21B C22B H22D 109.5 . . ?
C21B C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C21B C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?

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
O9 C9 C10 C11 166.5(14) . . . . ?
O10 C9 C10 C15 165.2(13) . . . . ?
O12 C16 C14 C15 169.0(11) . . . . ?
O11 C16 C14 C13 164.4(12) . . . . ?
O4 C1 C2 C3 160.1(11) . . . . ?
O3 C1 C2 C7 156.3(11) . . . . ?
O5 C8 C6 C5 -161.9(12) . . . . ?
O6 C8 C6 C7 -164.1(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         4.049
_refine_diff_density_min         -3.583
_refine_diff_density_rms         0.370
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shx97
_database_code_depnum_ccdc_archive 'CCDC 1024952'
_audit_update_record             
;
2015-01-28 deposited with the CCDC.
2015-01-30 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C8 H4 O7 U),17(H2 O)'
_chemical_formula_sum            'C16 H42 O31 U2'
_chemical_formula_weight         1206.3

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/c
_symmetry_space_group_name_Hall  '-C 2yc'

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                   19.703(4)
_cell_length_b                   9.5197(19)
_cell_length_c                   20.127(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.26(3)
_cell_angle_gamma                90.00
_cell_volume                     3624.2(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    16567
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      27.44

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.350
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1640
_exptl_absorpt_coefficient_mu    8.971
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.043
_exptl_absorpt_correction_T_max  0.046
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295(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  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 0
_diffrn_standards_number         0
_diffrn_standards_interval_count image
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            16567
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         27.44
_reflns_number_total             4152
_reflns_number_gt                3038
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL-97

_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. The least-squares refinement
of the structural model was performed under geometry restraints and 
displacement parameter restraints such as ISOR, FMAP, MPLA and DFIX.  
BOND $H
ISOR 0.01 C2 O6
DFIX 0.84 O8 H81
DFIX 1.90 H61 H4
DFIX 0.84 O6 H61
FMAP 2
MPLA 3 O6 O7 C8
MPLA 3 C1 C2 C3 C4 C5 C6
MPLA 3 O4 O5 C7
;

_platon_squeeze_details          
;
The solvent molecules in the structure were highly disordered. Efforts to 
locate and refine the solvent peaks were in vain. The SQUEEZE routine was
used to remove the scattering from the highly disordered solvent molecules,
the 626 electrons can be accounted for by 15.65 (i.e. ~16) water molecules 
per formula unit, and the reported formula, formula weight, density, F(000),
etc. include the solvents.
;


_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)+(0.0756P)²+160.8163P] 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         4060
_refine_ls_number_parameters     156
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0576
_refine_ls_wR_factor_ref         0.1917
_refine_ls_wR_factor_gt          0.1451
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_restrained_S_all      1.162
_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
U U 0.10488(2) 0.63492(6) 0.11128(2) 0.0382(2) Uani 1 1 d . . .
O1 O 0.0511(6) 0.7865(14) 0.0971(5) 0.056(3) Uani 1 1 d . . .
O2 O 0.1584(5) 0.4834(15) 0.1258(6) 0.065(4) Uani 1 1 d . . .
O3 O 0.0932(4) 0.6200(10) 0.2192(4) 0.033(2) Uani 1 1 d . . .
C1 C 0.1179(6) 0.5382(15) 0.2761(6) 0.031(3) Uani 1 1 d . . .
C2 C 0.1802(6) 0.4646(15) 0.2902(6) 0.033(3) Uani 1 1 d U . .
H2 H 0.2063 0.4658 0.2583 0.040 Uiso 1 1 calc R . .
C3 C 0.2054(7) 0.3877(19) 0.3516(7) 0.050(4) Uani 1 1 d . . .
C4 C 0.1653(7) 0.3833(18) 0.3984(6) 0.047(4) Uani 1 1 d . . .
H4 H 0.1809 0.3312 0.4389 0.056 Uiso 1 1 calc RD . .
C5 C 0.1014(7) 0.4573(17) 0.3845(6) 0.040(3) Uani 1 1 d . . .
C6 C 0.0777(7) 0.5304(16) 0.3239(7) 0.036(3) Uani 1 1 d . . .
H6 H 0.0342 0.5758 0.3140 0.043 Uiso 1 1 calc R . .
C7 C 0.2699(8) 0.301(2) 0.3634(8) 0.057(5) Uani 1 1 d . . .
C8 C 0.0565(7) 0.4477(16) 0.4336(7) 0.039(3) Uani 1 1 d . . .
O4 O 0.2968(5) 0.2705(13) 0.3152(4) 0.051(3) Uani 1 1 d . . .
O5 O 0.3001(6) 0.2578(17) 0.4242(5) 0.077(5) Uani 1 1 d . . .
O6 O 0.0820(7) 0.3914(16) 0.4912(6) 0.069(3) Uani 1 1 d DU . .
H61 H 0.123(5) 0.354(19) 0.500(4) 0.083 Uiso 1 1 d D . .
O7 O -0.0045(5) 0.4945(12) 0.4149(5) 0.046(3) Uani 1 1 d . . .
O8 O 0.0000 0.830(2) 0.2500 0.110(11) Uani 1 2 d SD . .
H81 H 0.035(10) 0.78(3) 0.248(17) 0.132 Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U O2 1.763(13) . ?
U O1 1.765(13) . ?
U O3 2.251(8) . ?
U O7 2.323(8) 2 ?
U O6 2.344(11) 6_565 ?
U O4 2.450(8) 4 ?
U O5 2.477(10) 4 ?
U C7 2.851(16) 4 ?
O3 C1 1.359(15) . ?
C1 C2 1.371(16) . ?
C1 C6 1.409(17) . ?
C2 C3 1.40(2) . ?
C2 H2 0.9300 . ?
C3 C4 1.390(19) . ?
C3 C7 1.48(2) . ?
C4 C5 1.401(17) . ?
C4 H4 0.9300 . ?
C5 C6 1.368(19) . ?
C5 C8 1.504(17) . ?
C6 H6 0.9300 . ?
C7 O4 1.263(17) . ?
C7 O5 1.269(19) . ?
C7 U 2.851(16) 4_545 ?
C8 O7 1.236(15) . ?
C8 O6 1.248(17) . ?
O4 U 2.450(8) 4_545 ?
O5 U 2.477(10) 4_545 ?
O6 U 2.344(11) 6_566 ?
O6 H61 0.85(2) . ?
O7 U 2.323(8) 2 ?
O8 H81 0.84(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U O1 179.7(5) . . ?
O2 U O3 90.3(5) . . ?
O1 U O3 89.4(4) . . ?
O2 U O7 89.9(5) . 2 ?
O1 U O7 90.0(5) . 2 ?
O3 U O7 82.6(3) . 2 ?
O2 U O6 91.0(6) . 6_565 ?
O1 U O6 89.3(5) . 6_565 ?
O3 U O6 161.0(4) . 6_565 ?
O7 U O6 78.4(4) 2 6_565 ?
O2 U O4 89.7(5) . 4 ?
O1 U O4 90.2(5) . 4 ?
O3 U O4 74.2(3) . 4 ?
O7 U O4 156.8(3) 2 4 ?
O6 U O4 124.8(3) 6_565 4 ?
O2 U O5 88.2(6) . 4 ?
O1 U O5 92.0(5) . 4 ?
O3 U O5 126.7(3) . 4 ?
O7 U O5 150.6(3) 2 4 ?
O6 U O5 72.3(3) 6_565 4 ?
O4 U O5 52.5(3) 4 4 ?
O2 U C7 88.6(6) . 4 ?
O1 U C7 91.5(6) . 4 ?
O3 U C7 100.4(4) . 4 ?
O7 U C7 176.7(4) 2 4 ?
O6 U C7 98.6(4) 6_565 4 ?
O4 U C7 26.2(4) 4 4 ?
O5 U C7 26.4(4) 4 4 ?
C1 O3 U 137.8(8) . . ?
O3 C1 C2 123.8(11) . . ?
O3 C1 C6 117.9(11) . . ?
C2 C1 C6 118.3(11) . . ?
C1 C2 C3 121.7(11) . . ?
C1 C2 H2 119.1 . . ?
C3 C2 H2 119.1 . . ?
C4 C3 C2 118.9(12) . . ?
C4 C3 C7 120.0(15) . . ?
C2 C3 C7 120.8(13) . . ?
C3 C4 C5 119.9(12) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 119.9(12) . . ?
C6 C5 C8 120.0(11) . . ?
C4 C5 C8 120.0(12) . . ?
C5 C6 C1 121.2(11) . . ?
C5 C6 H6 119.4 . . ?
C1 C6 H6 119.4 . . ?
O4 C7 O5 119.0(14) . . ?
O4 C7 C3 122.0(15) . . ?
O5 C7 C3 119.0(13) . . ?
O4 C7 U 58.9(7) . 4_545 ?
O5 C7 U 60.1(8) . 4_545 ?
C3 C7 U 179.0(11) . 4_545 ?
O7 C8 O6 122.9(12) . . ?
O7 C8 C5 118.6(11) . . ?
O6 C8 C5 118.5(11) . . ?
C7 O4 U 95.0(9) . 4_545 ?
C7 O5 U 93.5(8) . 4_545 ?
C8 O6 U 156.1(11) . 6_566 ?
C8 O6 H61 119(3) . . ?
U O6 H61 82(3) 6_566 . ?
C8 O7 U 165.7(12) . 2 ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.009 -0.010 -0.012 1919 626 ' '
_platon_squeeze_void_probe_radius 1.20


_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        27.44
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         2.533
_refine_diff_density_min         -4.074
_refine_diff_density_rms         0.373
