# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global

_journal_coden_Cambridge         1350

loop_
_publ_author_name
'Pierre Thuery'
'Bernardo Masci'

_publ_contact_author_name        'Pierre Thuery'
_publ_contact_author_address     
;
IRAMIS
DSM
SCM, CNRS URA 331
CEA Saclay
Bat 125
Gif-sur-Yvette
91191
FRANCE
;

_publ_contact_author_email       PIERRE.THUERY@CEA.FR

_publ_requested_journal          CrystEngComm

_publ_section_title              
;
Hydrothermal synthesis of uranyl-organic frameworks
with pyrazine-2,3-dicarboxylate linkers
;

data_1
_database_code_depnum_ccdc_archive 'CCDC 678506'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H6 N2 O8 U'
_chemical_formula_weight         472.16

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   'P c'

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

_cell_length_a                   5.4220(3)
_cell_length_b                   6.2926(4)
_cell_length_c                   14.5732(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.472(4)
_cell_angle_gamma                90.00
_cell_volume                     491.79(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    16192
_cell_measurement_theta_min      2.83
_cell_measurement_theta_max      25.68

_exptl_crystal_description       needle
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             424
_exptl_absorpt_coefficient_mu    16.540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.263
_exptl_absorpt_correction_T_max  0.516
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 30 mm'
_diffrn_ambient_temperature      100(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  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two φ and five ω scans with 2° steps'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            16192
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.83
_diffrn_reflns_theta_max         25.68
_reflns_number_total             1786
_reflns_number_gt                1760
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'

_refine_special_details          
;
Structure solved by direct methods and subsequent Fourier-difference
synthesis. All non-hydrogen atoms were refined with anisotropic
displacement parameters. The H atoms bound to O atoms were found on a
Fourier-difference map and all the others were introduced at calculated
positions. All were treated as riding atoms with an isotropic displacement
parameter equal to 1.2 times that of the parent atom.
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)+(0.0256P)²+0.2330P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.482(8)
_refine_ls_number_reflns         1786
_refine_ls_number_parameters     155
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0154
_refine_ls_R_factor_gt           0.0151
_refine_ls_wR_factor_ref         0.0380
_refine_ls_wR_factor_gt          0.0378
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.106

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 0.56618(11) 0.698714(18) 0.93822(9) 0.00778(6) Uani 1 1 d . . .
O1 O 0.8516(8) 0.8289(6) 0.9684(3) 0.0137(8) Uani 1 1 d . . .
O2 O 0.2779(7) 0.5670(6) 0.9065(3) 0.0145(8) Uani 1 1 d . . .
O3 O 0.5190(8) 0.8569(6) 0.7896(3) 0.0154(8) Uani 1 1 d . . .
O4 O 0.6480(7) 0.9185(6) 0.6529(2) 0.0131(7) Uani 1 1 d . . .
O5 O 0.7389(6) 0.6138(5) 0.5066(2) 0.0112(7) Uani 1 1 d . . .
O6 O 1.1038(9) 0.7630(8) 0.5671(4) 0.0153(8) Uani 1 1 d . . .
O7 O 0.3853(7) 1.0535(5) 0.9505(2) 0.0116(7) Uani 1 1 d . . .
H7A H 0.4875 1.1833 0.9614 0.014 Uiso 1 1 d R . .
H7B H 0.2557 1.0967 0.9817 0.014 Uiso 1 1 d R . .
O8 O 0.4603(8) 0.7298(6) 1.0903(3) 0.0117(8) Uani 1 1 d . . .
H8A H 0.3582 0.6867 1.1294 0.014 Uiso 1 1 d R . .
H8B H 0.5268 0.8630 1.1156 0.014 Uiso 1 1 d R . .
N1 N 0.7615(7) 0.4883(7) 0.8077(3) 0.0102(8) Uani 1 1 d . . .
N2 N 1.0509(9) 0.3567(7) 0.6754(3) 0.0105(8) Uani 1 1 d . . .
C1 C 0.7710(9) 0.6008(8) 0.7298(3) 0.0094(9) Uani 1 1 d . . .
C2 C 0.9119(9) 0.5342(8) 0.6626(4) 0.0091(9) Uani 1 1 d . . .
C3 C 1.0367(10) 0.2416(10) 0.7518(5) 0.0090(10) Uani 1 1 d . . .
H3 H 1.1294 0.1173 0.7619 0.011 Uiso 1 1 calc R . .
C4 C 0.8861(13) 0.3043(7) 0.8167(4) 0.0105(12) Uani 1 1 d . . .
H4 H 0.8720 0.2167 0.8670 0.013 Uiso 1 1 calc R . .
C5 C 0.6340(11) 0.8096(7) 0.7218(4) 0.0105(12) Uani 1 1 d . . .
C6 C 0.9224(10) 0.6522(8) 0.5726(4) 0.0090(10) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U O1 1.749(4) . ?
U O2 1.769(4) . ?
U O5 2.337(3) 2_565 ?
U O3 2.363(4) . ?
U O8 2.378(4) . ?
U O7 2.456(3) . ?
U N1 2.662(4) . ?
O3 C5 1.278(7) . ?
O4 C5 1.227(7) . ?
O5 C6 1.300(6) . ?
O5 U 2.337(3) 2_564 ?
O6 C6 1.218(7) . ?
O7 H7A 0.9870 . ?
O7 H7B 0.9322 . ?
O8 H8A 0.8932 . ?
O8 H8B 0.9639 . ?
N1 C4 1.337(7) . ?
N1 C1 1.346(7) . ?
N2 C3 1.340(8) . ?
N2 C2 1.345(7) . ?
C1 C2 1.392(7) . ?
C1 C5 1.505(8) . ?
C2 C6 1.516(7) . ?
C3 C4 1.394(9) . ?
C3 H3 0.9300 . ?
C4 H4 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 U O2 179.41(17) . . ?
O1 U O5 90.15(16) . 2_565 ?
O2 U O5 90.02(15) . 2_565 ?
O1 U O3 90.30(18) . . ?
O2 U O3 89.18(16) . . ?
O5 U O3 136.70(13) 2_565 . ?
O1 U O8 93.07(18) . . ?
O2 U O8 87.52(16) . . ?
O5 U O8 78.95(13) 2_565 . ?
O3 U O8 144.21(14) . . ?
O1 U O7 84.49(15) . . ?
O2 U O7 95.63(14) . . ?
O5 U O7 150.83(12) 2_565 . ?
O3 U O7 72.14(12) . . ?
O8 U O7 72.75(13) . . ?
O1 U N1 88.97(16) . . ?
O2 U N1 90.54(15) . . ?
O5 U N1 73.13(13) 2_565 . ?
O3 U N1 63.59(14) . . ?
O8 U N1 152.01(14) . . ?
O7 U N1 135.18(13) . . ?
C5 O3 U 127.7(4) . . ?
C6 O5 U 133.4(3) . 2_564 ?
U O7 H7A 122.9 . . ?
U O7 H7B 129.7 . . ?
H7A O7 H7B 97.2 . . ?
U O8 H8A 145.8 . . ?
U O8 H8B 107.5 . . ?
H8A O8 H8B 104.6 . . ?
C4 N1 C1 117.2(5) . . ?
C4 N1 U 127.5(4) . . ?
C1 N1 U 114.2(3) . . ?
C3 N2 C2 117.7(5) . . ?
N1 C1 C2 121.9(5) . . ?
N1 C1 C5 116.4(5) . . ?
C2 C1 C5 121.6(5) . . ?
N2 C2 C1 120.5(5) . . ?
N2 C2 C6 115.8(4) . . ?
C1 C2 C6 123.8(4) . . ?
N2 C3 C4 121.5(5) . . ?
N2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
N1 C4 C3 121.1(5) . . ?
N1 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
O4 C5 O3 126.8(5) . . ?
O4 C5 C1 117.5(5) . . ?
O3 C5 C1 115.8(5) . . ?
O6 C6 O5 126.6(5) . . ?
O6 C6 C2 118.0(5) . . ?
O5 C6 C2 115.2(4) . . ?

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 H7A O5 0.99 1.91 2.875(5) 164.4 2_575
O7 H7B O6 0.93 1.82 2.705(6) 157.7 2_475
O8 H8A N2 0.89 1.91 2.752(6) 157.6 2_465
O8 H8B O4 0.96 1.59 2.548(5) 176.5 2_575

#===END

data_2
_database_code_depnum_ccdc_archive 'CCDC 678507'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H4 N2 O7 U'
_chemical_formula_weight         454.14

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   'C 2'

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'

_cell_length_a                   9.2125(6)
_cell_length_b                   11.6265(5)
_cell_length_c                   9.8446(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.397(3)
_cell_angle_gamma                90.00
_cell_volume                     1029.86(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    16046
_cell_measurement_theta_min      2.86
_cell_measurement_theta_max      25.67

_exptl_crystal_description       needle
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.929
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             808
_exptl_absorpt_coefficient_mu    15.784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.495
_exptl_absorpt_correction_T_max  0.623
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 30 mm'
_diffrn_ambient_temperature      100(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  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two φ and four ω scans with 2° steps'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            16046
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.86
_diffrn_reflns_theta_max         25.67
_reflns_number_total             1931
_reflns_number_gt                1878
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'

_refine_special_details          
;
Structure solved by direct methods and subsequent Fourier-difference
synthesis. All non-hydrogen atoms were refined with anisotropic
displacement parameters. The H atoms bound to O7 were found on a
Fourier-difference map and all the others were introduced at calculated
positions. All were treated as riding atoms with an isotropic displacement
parameter equal to 1.2 times that of the parent atom.
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)+(0.0277P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_chemical_absolute_configuration ad
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.011(9)
_refine_ls_number_reflns         1931
_refine_ls_number_parameters     146
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0185
_refine_ls_wR_factor_ref         0.0442
_refine_ls_wR_factor_gt          0.0439
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.67
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.605
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.130

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 0.228754(17) 0.4796 0.339436(15) 0.01480(7) Uani 1 1 d . . .
O1 O 0.4108(5) 0.4316(4) 0.3432(4) 0.0213(9) Uani 1 1 d . . .
O2 O 0.0465(5) 0.5242(3) 0.3413(4) 0.0212(9) Uani 1 1 d . . .
O3 O 0.1646(5) 0.2938(3) 0.4088(4) 0.0220(9) Uani 1 1 d . . .
O4 O 0.1663(5) 0.1485(3) 0.5536(4) 0.0195(9) Uani 1 1 d . . .
O5 O 0.2619(6) 0.1112(4) 0.8364(4) 0.0203(9) Uani 1 1 d . . .
O6 O 0.0528(5) 0.1927(4) 0.8750(4) 0.0204(9) Uani 1 1 d . . .
O7 O 0.1417(5) 0.3677(4) 0.1331(4) 0.0217(9) Uani 1 1 d . . .
H7A H 0.0717 0.3242 0.1632 0.026 Uiso 1 1 d R . .
H7B H 0.1698 0.3295 0.0668 0.026 Uiso 1 1 d R . .
N1 N 0.2594(5) 0.4428(4) 0.6097(6) 0.0157(10) Uani 1 1 d . . .
N2 N 0.2483(6) 0.3918(4) 0.8861(6) 0.0203(11) Uani 1 1 d . . .
C1 C 0.2245(7) 0.3360(5) 0.6487(6) 0.0165(11) Uani 1 1 d . . .
C2 C 0.2186(6) 0.3107(5) 0.7845(6) 0.0141(11) Uani 1 1 d . . .
C3 C 0.2921(6) 0.4957(7) 0.8497(6) 0.0176(15) Uani 1 1 d . . .
H3 H 0.3190 0.5523 0.9172 0.021 Uiso 1 1 calc R . .
C4 C 0.2979(7) 0.5201(5) 0.7105(7) 0.0193(13) Uani 1 1 d . . .
H4 H 0.3295 0.5924 0.6887 0.023 Uiso 1 1 calc R . .
C5 C 0.1828(6) 0.2528(5) 0.5298(6) 0.0147(12) Uani 1 1 d . . .
C6 C 0.1691(7) 0.1957(5) 0.8345(6) 0.0164(12) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U O1 1.761(4) . ?
U O2 1.761(4) . ?
U O5 2.326(4) 4_556 ?
U O4 2.338(4) 4_556 ?
U O3 2.379(4) . ?
U O7 2.400(4) . ?
U N1 2.650(5) . ?
O3 C5 1.260(7) . ?
O4 C5 1.250(7) . ?
O4 U 2.338(4) 4_546 ?
O5 C6 1.300(8) . ?
O5 U 2.326(4) 4_546 ?
O6 C6 1.222(7) . ?
O7 H7A 0.9181 . ?
O7 H7B 0.8734 . ?
N1 C4 1.330(8) . ?
N1 C1 1.358(8) . ?
N2 C3 1.346(9) . ?
N2 C2 1.360(8) . ?
C1 C2 1.381(8) . ?
C1 C5 1.504(8) . ?
C2 C6 1.527(8) . ?
C3 C4 1.411(8) . ?
C3 H3 0.9300 . ?
C4 H4 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 U O2 177.78(18) . . ?
O1 U O5 92.14(19) . 4_556 ?
O2 U O5 90.07(18) . 4_556 ?
O1 U O4 87.53(17) . 4_556 ?
O2 U O4 92.91(17) . 4_556 ?
O5 U O4 72.81(15) 4_556 4_556 ?
O1 U O3 90.01(18) . . ?
O2 U O3 88.20(17) . . ?
O5 U O3 149.62(15) 4_556 . ?
O4 U O3 137.56(14) 4_556 . ?
O1 U O7 89.43(18) . . ?
O2 U O7 91.27(18) . . ?
O5 U O7 77.63(15) 4_556 . ?
O4 U O7 150.14(14) 4_556 . ?
O3 U O7 72.09(14) . . ?
O1 U N1 91.83(17) . . ?
O2 U N1 86.19(17) . . ?
O5 U N1 147.20(14) 4_556 . ?
O4 U N1 74.85(14) 4_556 . ?
O3 U N1 62.89(14) . . ?
O7 U N1 134.96(14) . . ?
C5 O3 U 128.6(4) . . ?
C5 O4 U 147.5(4) . 4_546 ?
C6 O5 U 128.0(4) . 4_546 ?
U O7 H7A 99.0 . . ?
U O7 H7B 144.0 . . ?
H7A O7 H7B 107.6 . . ?
C4 N1 C1 116.6(5) . . ?
C4 N1 U 126.5(4) . . ?
C1 N1 U 116.8(4) . . ?
C3 N2 C2 116.8(5) . . ?
N1 C1 C2 121.9(5) . . ?
N1 C1 C5 113.9(5) . . ?
C2 C1 C5 124.0(5) . . ?
N2 C2 C1 121.4(5) . . ?
N2 C2 C6 113.4(5) . . ?
C1 C2 C6 125.1(5) . . ?
N2 C3 C4 121.0(6) . . ?
N2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
N1 C4 C3 122.0(6) . . ?
N1 C4 H4 119.0 . . ?
C3 C4 H4 119.0 . . ?
O4 C5 O3 123.1(5) . . ?
O4 C5 C1 120.0(5) . . ?
O3 C5 C1 116.9(5) . . ?
O6 C6 O5 126.4(6) . . ?
O6 C6 C2 118.3(5) . . ?
O5 C6 C2 115.1(5) . . ?

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 H7A O6 0.92 1.90 2.701(6) 144.7 2_556
O7 H7B N2 0.87 2.18 2.825(6) 130.0 1_554

#===END

data_3
_database_code_depnum_ccdc_archive 'CCDC 678508'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H7 Cs N4 O14 U2'
_chemical_formula_weight         1040.19

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'
Cs Cs -0.3680 2.1192 '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   'P 21/c'

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

_cell_length_a                   7.8884(5)
_cell_length_b                   30.599(2)
_cell_length_c                   8.2540(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.070(4)
_cell_angle_gamma                90.00
_cell_volume                     1992.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    46014
_cell_measurement_theta_min      3.26
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1832
_exptl_absorpt_coefficient_mu    18.121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.101
_exptl_absorpt_correction_T_max  0.404
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_special_details           'crystal-to-detector distance 40 mm'
_diffrn_ambient_temperature      100(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  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two φ and four ω scans with 2° steps'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            46014
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0526
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.26
_diffrn_reflns_theta_max         25.68
_reflns_number_total             3766
_reflns_number_gt                3290
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'

_refine_special_details          
;
The orthorhombic system can be ruled out on the basis of the
corresponding internal R factor of 0.61.
Structure solved by direct methods and subsequent Fourier-difference
synthesis. All non-hydrogen atoms were refined with anisotropic
displacement parameters. The H atoms bound to O atoms were found on a
Fourier-difference map and all the others were introduced at calculated
positions. All were treated as riding atoms with an isotropic displacement
parameter equal to 1.2 times that of the parent atom.
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)+(0.0257P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3766
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0257
_refine_ls_wR_factor_ref         0.0552
_refine_ls_wR_factor_gt          0.0533
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.215
_refine_diff_density_min         -1.542
_refine_diff_density_rms         0.296

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 0.73032(2) 0.117968(7) 0.38762(2) 0.01306(7) Uani 1 1 d . . .
U2 U 1.38436(2) 0.160372(7) 0.75357(2) 0.01286(7) Uani 1 1 d . . .
Cs Cs 0.95061(4) 0.085065(13) 0.92941(4) 0.02009(10) Uani 1 1 d . . .
O1 O 0.7942(4) 0.10270(14) 0.5852(4) 0.0171(9) Uani 1 1 d . . .
O2 O 0.6661(4) 0.13506(13) 0.1923(4) 0.0156(9) Uani 1 1 d . . .
O3 O 1.1712(4) 0.14930(13) 0.6990(4) 0.0159(9) Uani 1 1 d . . .
O4 O 1.5997(4) 0.16933(13) 0.8085(4) 0.0153(9) Uani 1 1 d . . .
O5 O 0.8266(4) 0.05248(13) 0.2809(4) 0.0161(9) Uani 1 1 d . . .
O6 O 0.8028(5) -0.01276(14) 0.1602(5) 0.0236(10) Uani 1 1 d . . .
O7 O 0.5706(5) -0.08476(14) 0.2578(4) 0.0193(9) Uani 1 1 d . . .
O8 O 0.4612(5) -0.06348(14) 0.0209(4) 0.0219(10) Uani 1 1 d . . .
O9 O 1.0143(4) 0.13456(14) 0.3143(4) 0.0159(9) Uani 1 1 d . . .
O10 O 1.2433(4) 0.17738(13) 0.2949(4) 0.0156(9) Uani 1 1 d . . .
O11 O 1.3456(4) 0.22661(13) 0.6017(4) 0.0138(9) Uani 1 1 d . . .
O12 O 1.3196(4) 0.28347(13) 0.4375(4) 0.0177(9) Uani 1 1 d . . .
O13 O 0.4914(4) 0.14829(13) 0.4919(4) 0.0141(9) Uani 1 1 d . . .
H13 H 0.4460 0.1673 0.4407 0.017 Uiso 1 1 d R . .
O14 O 1.3177(4) 0.12899(13) 1.0191(4) 0.0154(9) Uani 1 1 d . . .
H14A H 1.3519 0.1020 1.0213 0.019 Uiso 1 1 d R . .
H14B H 1.3039 0.1393 1.1186 0.019 Uiso 1 1 d R . .
N1 N 0.5050(5) 0.05570(16) 0.3541(5) 0.0135(10) Uani 1 1 d . . .
N2 N 0.2773(5) -0.01068(17) 0.2660(5) 0.0176(11) Uani 1 1 d . . .
N3 N 0.8325(5) 0.19809(16) 0.4404(5) 0.0139(10) Uani 1 1 d . . .
N4 N 0.9745(5) 0.27614(16) 0.5460(5) 0.0165(11) Uani 1 1 d . . .
C1 C 0.5585(7) 0.0194(2) 0.2820(6) 0.0137(13) Uani 1 1 d . . .
C2 C 0.4463(7) -0.0146(2) 0.2417(6) 0.0163(13) Uani 1 1 d . . .
C3 C 0.2267(7) 0.0257(2) 0.3364(6) 0.0172(13) Uani 1 1 d . . .
H3 H 0.1114 0.0293 0.3556 0.021 Uiso 1 1 calc R . .
C4 C 0.3370(7) 0.0591(2) 0.3837(6) 0.0183(13) Uani 1 1 d . . .
H4 H 0.2947 0.0838 0.4358 0.022 Uiso 1 1 calc R . .
C5 C 0.7441(7) 0.0182(2) 0.2350(6) 0.0181(14) Uani 1 1 d . . .
C6 C 0.4991(6) -0.0573(2) 0.1647(7) 0.0167(13) Uani 1 1 d . . .
C7 C 1.0012(6) 0.20469(19) 0.4328(6) 0.0141(13) Uani 1 1 d . . .
C8 C 1.0709(7) 0.2432(2) 0.4919(6) 0.0164(13) Uani 1 1 d . . .
C9 C 0.8084(7) 0.2697(2) 0.5438(6) 0.0185(14) Uani 1 1 d . . .
H9 H 0.7375 0.2924 0.5758 0.022 Uiso 1 1 calc R . .
C10 C 0.7357(7) 0.2303(2) 0.4957(6) 0.0174(14) Uani 1 1 d . . .
H10 H 0.6189 0.2265 0.5023 0.021 Uiso 1 1 calc R . .
C11 C 1.0963(7) 0.1694(2) 0.3411(6) 0.0153(13) Uani 1 1 d . . .
C12 C 1.2595(7) 0.2510(2) 0.5086(6) 0.0182(14) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 1.769(3) . ?
U1 O1 1.769(3) . ?
U1 O13 2.271(3) . ?
U1 O5 2.317(4) . ?
U1 O9 2.376(3) . ?
U1 N3 2.617(5) . ?
U1 N1 2.620(5) . ?
U1 Cs 4.2841(4) 1_554 ?
U1 Cs 4.9002(5) . ?
U2 O3 1.773(3) . ?
U2 O4 1.779(3) . ?
U2 O7 2.343(4) 3_756 ?
U2 O13 2.349(3) 1_655 ?
U2 O12 2.350(4) 4_566 ?
U2 O11 2.403(4) . ?
U2 O14 2.451(3) . ?
U2 Cs 4.3745(4) . ?
Cs O6 3.038(4) 3_756 ?
Cs O1 3.142(3) . ?
Cs O5 3.221(4) 1_556 ?
Cs O3 3.243(4) . ?
Cs O14 3.276(3) . ?
Cs N2 3.318(5) 3_656 ?
Cs O8 3.341(4) 3_656 ?
Cs O2 3.478(3) 1_556 ?
Cs O9 3.555(4) 1_556 ?
Cs O6 3.735(4) 1_556 ?
O5 C5 1.290(7) . ?
O6 C5 1.223(7) . ?
O7 C6 1.269(7) . ?
O8 C6 1.238(6) . ?
O9 C11 1.265(7) . ?
O10 C11 1.246(6) . ?
O11 C12 1.267(7) . ?
O12 C12 1.248(7) . ?
O13 H13 0.8039 . ?
O14 H14A 0.8696 . ?
O14 H14B 0.8865 . ?
N1 C1 1.329(7) . ?
N1 C4 1.352(6) . ?
N2 C3 1.318(7) . ?
N2 C2 1.354(7) . ?
N3 C10 1.328(7) . ?
N3 C7 1.347(6) . ?
N4 C9 1.325(7) . ?
N4 C8 1.340(7) . ?
C1 C2 1.406(8) . ?
C1 C5 1.515(7) . ?
C2 C6 1.512(8) . ?
C3 C4 1.398(8) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C7 C8 1.388(8) . ?
C7 C11 1.519(8) . ?
C8 C12 1.513(7) . ?
C9 C10 1.392(8) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U1 O1 178.10(18) . . ?
O2 U1 O13 89.30(14) . . ?
O1 U1 O13 89.67(14) . . ?
O2 U1 O5 90.17(15) . . ?
O1 U1 O5 91.65(16) . . ?
O13 U1 O5 140.33(13) . . ?
O2 U1 O9 88.50(14) . . ?
O1 U1 O9 91.34(14) . . ?
O13 U1 O9 142.41(14) . . ?
O5 U1 O9 77.20(13) . . ?
O2 U1 N3 87.86(16) . . ?
O1 U1 N3 90.38(17) . . ?
O13 U1 N3 79.04(13) . . ?
O5 U1 N3 140.57(12) . . ?
O9 U1 N3 63.38(13) . . ?
O2 U1 N1 85.71(15) . . ?
O1 U1 N1 95.61(16) . . ?
O13 U1 N1 76.93(13) . . ?
O5 U1 N1 63.48(13) . . ?
O9 U1 N1 140.19(14) . . ?
N3 U1 N1 155.18(14) . . ?
O3 U2 O4 177.85(18) . . ?
O3 U2 O7 86.84(16) . 3_756 ?
O4 U2 O7 91.01(16) . 3_756 ?
O3 U2 O13 94.48(14) . 1_655 ?
O4 U2 O13 85.09(14) . 1_655 ?
O7 U2 O13 75.70(13) 3_756 1_655 ?
O3 U2 O12 95.58(15) . 4_566 ?
O4 U2 O12 86.04(15) . 4_566 ?
O7 U2 O12 141.37(13) 3_756 4_566 ?
O13 U2 O12 141.98(13) 1_655 4_566 ?
O3 U2 O11 84.76(15) . . ?
O4 U2 O11 97.10(15) . . ?
O7 U2 O11 146.25(12) 3_756 . ?
O13 U2 O11 72.46(12) 1_655 . ?
O12 U2 O11 72.10(13) 4_566 . ?
O3 U2 O14 87.01(14) . . ?
O4 U2 O14 92.21(14) . . ?
O7 U2 O14 71.43(13) 3_756 . ?
O13 U2 O14 146.97(13) 1_655 . ?
O12 U2 O14 70.21(13) 4_566 . ?
O11 U2 O14 140.35(12) . . ?
O6 Cs O1 98.96(10) 3_756 . ?
O6 Cs O5 100.91(10) 3_756 1_556 ?
O1 Cs O5 138.43(9) . 1_556 ?
O6 Cs O3 87.39(10) 3_756 . ?
O1 Cs O3 64.91(9) . . ?
O5 Cs O3 151.60(9) 1_556 . ?
O6 Cs O14 77.75(10) 3_756 . ?
O1 Cs O14 118.67(9) . . ?
O5 Cs O14 101.11(9) 1_556 . ?
O3 Cs O14 53.79(9) . . ?
O6 Cs N2 74.26(11) 3_756 3_656 ?
O1 Cs N2 57.75(11) . 3_656 ?
O5 Cs N2 93.47(10) 1_556 3_656 ?
O3 Cs N2 114.93(10) . 3_656 ?
O14 Cs N2 150.41(10) . 3_656 ?
O6 Cs O8 120.59(10) 3_756 3_656 ?
O1 Cs O8 76.37(9) . 3_656 ?
O5 Cs O8 62.08(9) 1_556 3_656 ?
O3 Cs O8 135.59(9) . 3_656 ?
O14 Cs O8 155.87(9) . 3_656 ?
N2 Cs O8 52.96(10) 3_656 3_656 ?
O6 Cs O2 152.38(10) 3_756 1_556 ?
O1 Cs O2 103.62(9) . 1_556 ?
O5 Cs O2 51.49(9) 1_556 1_556 ?
O3 Cs O2 116.51(9) . 1_556 ?
O14 Cs O2 104.44(8) . 1_556 ?
N2 Cs O2 104.79(10) 3_656 1_556 ?
O8 Cs O2 51.83(9) 3_656 1_556 ?
O6 Cs O9 115.98(9) 3_756 1_556 ?
O1 Cs O9 142.16(10) . 1_556 ?
O5 Cs O9 50.92(9) 1_556 1_556 ?
O3 Cs O9 100.99(9) . 1_556 ?
O14 Cs O9 59.95(8) . 1_556 ?
N2 Cs O9 143.39(9) 3_656 1_556 ?
O8 Cs O9 96.37(8) 3_656 1_556 ?
O2 Cs O9 49.13(8) 1_556 1_556 ?
O6 Cs O6 74.98(10) 3_756 1_556 ?
O1 Cs O6 118.44(9) . 1_556 ?
O5 Cs O6 36.61(9) 1_556 1_556 ?
O3 Cs O6 162.33(9) . 1_556 ?
O14 Cs O6 119.33(9) . 1_556 ?
N2 Cs O6 61.89(10) 3_656 1_556 ?
O8 Cs O6 58.32(9) 3_656 1_556 ?
O2 Cs O6 80.34(9) 1_556 1_556 ?
O9 Cs O6 85.95(9) 1_556 1_556 ?
C5 Cs O6 19.05(10) 1_556 1_556 ?
C6 Cs O6 68.07(11) 3_656 1_556 ?
U1 O1 Cs 171.81(19) . . ?
U1 O2 Cs 104.73(14) . 1_554 ?
U2 O3 Cs 118.44(15) . . ?
C5 O5 U1 130.4(3) . . ?
C5 O5 Cs 98.1(3) . 1_554 ?
U1 O5 Cs 100.06(13) . 1_554 ?
C5 O6 Cs 158.5(4) . 3_756 ?
C5 O6 Cs 75.8(3) . 1_554 ?
Cs O6 Cs 105.02(10) 3_756 1_554 ?
C6 O7 U2 134.1(4) . 3_756 ?
C6 O8 Cs 98.4(3) . 3_656 ?
C11 O9 U1 128.1(3) . . ?
C11 O9 Cs 125.9(3) . 1_554 ?
U1 O9 Cs 90.25(11) . 1_554 ?
C12 O11 U2 151.7(4) . . ?
C12 O12 U2 165.7(4) . 4_565 ?
U1 O13 U2 135.40(16) . 1_455 ?
U1 O13 H13 117.7 . . ?
U2 O13 H13 102.1 1_455 . ?
U2 O14 Cs 98.58(11) . . ?
U2 O14 H14A 108.9 . . ?
Cs O14 H14A 83.6 . . ?
U2 O14 H14B 135.7 . . ?
Cs O14 H14B 104.2 . . ?
H14A O14 H14B 110.9 . . ?
C1 N1 C4 117.2(5) . . ?
C1 N1 U1 116.1(3) . . ?
C4 N1 U1 126.1(4) . . ?
C3 N2 C2 116.1(5) . . ?
C3 N2 Cs 129.0(3) . 3_656 ?
C2 N2 Cs 113.6(3) . 3_656 ?
C10 N3 C7 118.2(5) . . ?
C10 N3 U1 125.1(4) . . ?
C7 N3 U1 115.9(4) . . ?
C9 N4 C8 116.4(5) . . ?
N1 C1 C2 121.6(5) . . ?
N1 C1 C5 116.2(5) . . ?
C2 C1 C5 122.0(5) . . ?
N2 C2 C1 121.2(5) . . ?
N2 C2 C6 114.3(5) . . ?
C1 C2 C6 124.5(5) . . ?
N2 C3 C4 123.5(5) . . ?
N2 C3 H3 118.2 . . ?
C4 C3 H3 118.2 . . ?
N1 C4 C3 120.2(5) . . ?
N1 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
O6 C5 O5 125.9(5) . . ?
O6 C5 C1 120.9(6) . . ?
O5 C5 C1 113.1(5) . . ?
O8 C6 O7 125.9(6) . . ?
O8 C6 C2 117.9(5) . . ?
O7 C6 C2 116.1(5) . . ?
N3 C7 C8 120.1(5) . . ?
N3 C7 C11 113.9(5) . . ?
C8 C7 C11 125.7(5) . . ?
N4 C8 C7 122.0(5) . . ?
N4 C8 C12 114.2(5) . . ?
C7 C8 C12 123.7(5) . . ?
N4 C9 C10 122.7(5) . . ?
N4 C9 H9 118.6 . . ?
C10 C9 H9 118.6 . . ?
N3 C10 C9 120.2(5) . . ?
N3 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
O10 C11 O9 126.0(5) . . ?
O10 C11 C7 118.2(5) . . ?
O9 C11 C7 115.7(5) . . ?
O12 C12 O11 123.4(5) . . ?
O12 C12 C8 117.2(5) . . ?
O11 C12 C8 119.3(5) . . ?

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
O13 H13 O10 0.80 2.02 2.694(5) 140.7 1_455
O14 H14A O8 0.87 1.92 2.678(5) 144.9 3_756
O14 H14B O10 0.89 1.92 2.779(5) 161.1 1_556


