Supplementary information (ESI) for CrystEngComm
This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm
_journal_coden_cambridge         1350
_publ_contact_author_name        'Pierre Thuery'
_publ_contact_author_address     
;
CEA/Saclay, SCM (CNRS URA 331)
B\^at. 125
91191 Gif-sur-Yvette
France
;
_publ_contact_author_phone       '33 01 69 08 63 29'
_publ_contact_author_fax         '33 1 69 08 66 40'
_publ_contact_author_email       pierre.thuery@cea.fr

_publ_section_title              
;The first crystal structure of an actinide complex of
the macrocyclic ligand DOTA: a two dimensional uranyl-organic framework
;
_publ_author_name                'Pierre Thuery'

data_1
_database_code_depnum_ccdc_archive 'CCDC 673444'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H42 N4 O24 U2'
_chemical_formula_weight         1174.62

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 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                   6.7056(3)
_cell_length_b                   18.3989(10)
_cell_length_c                   27.4530(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.523(4)
_cell_angle_gamma                90.00
_cell_volume                     3383.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    136783
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2216
_exptl_absorpt_coefficient_mu    9.657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.302
_exptl_absorpt_correction_T_max  0.748
_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 \f and eight \w scans with 2\% steps'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            136783
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.21
_diffrn_reflns_theta_max         25.68
_reflns_number_total             6413
_reflns_number_gt                5193
_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          
;
Structure solved by Patterson map interpretation and subsequent
Fourier-difference synthesis. All non-hydrogen atoms were refined
with anisotropic displacement parameters, with restraints for the very
badly resolved water solvent molecules. All but two of these water
molecules were affected with 0.5 occupancy factors in order to
retain acceptable displacement parameters or because they are too close
to one another. The H atoms bound to the coordinated water O atoms and to
N 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 F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0393P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     heavy
_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         6413
_refine_ls_number_parameters     466
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0330
_refine_ls_wR_factor_ref         0.0779
_refine_ls_wR_factor_gt          0.0735
_refine_ls_goodness_of_fit_ref   1.025
_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 0.999
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.722
_refine_diff_density_min         -1.514
_refine_diff_density_rms         0.215

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 0.44700(3) 0.059591(14) 0.107774(9) 0.01933(8) Uani 1 1 d . . .
U2 U 0.50997(3) 0.021806(13) 0.385724(9) 0.01857(8) Uani 1 1 d . . .
O1 O 0.1940(6) 0.0318(3) 0.10336(18) 0.0260(11) Uani 1 1 d . . .
O2 O 0.7009(6) 0.0877(3) 0.11119(17) 0.0243(10) Uani 1 1 d . . .
O3 O 0.2507(6) 0.0036(2) 0.38039(17) 0.0228(10) Uani 1 1 d . . .
O4 O 0.7688(6) 0.0399(2) 0.39103(17) 0.0235(10) Uani 1 1 d . . .
O5 O 0.4030(6) 0.1105(3) 0.18352(17) 0.0246(11) Uani 1 1 d . . .
O6 O 0.3084(6) 0.1469(3) 0.25587(17) 0.0249(11) Uani 1 1 d . . .
O7 O 0.4510(6) 0.1435(2) 0.37013(17) 0.0225(10) Uani 1 1 d . . .
O8 O 0.3611(7) 0.2549(3) 0.3461(2) 0.0350(13) Uani 1 1 d . . .
O9 O 0.4761(6) 0.4649(2) 0.34050(17) 0.0221(10) Uani 1 1 d . . .
O10 O 0.3480(6) 0.4378(3) 0.26738(18) 0.0272(11) Uani 1 1 d . . .
O11 O 0.4328(6) 0.4097(2) 0.14718(16) 0.0232(10) Uani 1 1 d . . .
O12 O 0.3295(7) 0.3106(3) 0.1856(2) 0.0346(13) Uani 1 1 d . . .
O13 O 0.5222(7) -0.0449(3) 0.05585(17) 0.0273(11) Uani 1 1 d . . .
O14 O 0.4457(7) 0.0863(3) 0.02034(17) 0.0269(11) Uani 1 1 d . . .
O15 O 0.3335(8) 0.1812(3) 0.08920(19) 0.0406(14) Uani 1 1 d . . .
H15A H 0.4091 0.2193 0.1003 0.049 Uiso 1 1 d R . .
H15B H 0.2463 0.1996 0.0668 0.049 Uiso 1 1 d R . .
O16 O 0.4683(7) 0.0785(2) 0.46494(17) 0.0260(11) Uani 1 1 d . . .
O17 O 0.5372(7) -0.0634(2) 0.45432(16) 0.0260(11) Uani 1 1 d . . .
O18 O 0.5138(6) 0.0385(2) 0.29660(16) 0.0223(10) Uani 1 1 d . . .
H18A H 0.4501 0.0753 0.2784 0.027 Uiso 1 1 d R . .
H18B H 0.5559 0.0087 0.2722 0.027 Uiso 1 1 d R . .
N1 N -0.0514(7) 0.2024(3) 0.2171(2) 0.0198(12) Uani 1 1 d . . .
H1 H -0.0088 0.2346 0.2431 0.024 Uiso 1 1 d R . .
N2 N -0.0187(8) 0.2200(3) 0.3231(2) 0.0226(13) Uani 1 1 d . . .
N3 N -0.0022(7) 0.3803(3) 0.3066(2) 0.0193(12) Uani 1 1 d . . .
H3 H 0.0565 0.3558 0.2840 0.023 Uiso 1 1 d R . .
N4 N -0.0363(7) 0.3591(3) 0.1999(2) 0.0210(12) Uani 1 1 d . . .
C1 C -0.1435(10) 0.1497(4) 0.2500(3) 0.0236(15) Uani 1 1 d . . .
H1A H -0.0509 0.1102 0.2572 0.028 Uiso 1 1 calc R . .
H1B H -0.2627 0.1293 0.2341 0.028 Uiso 1 1 calc R . .
C2 C -0.1978(9) 0.1865(4) 0.2974(3) 0.0228(15) Uani 1 1 d . . .
H2A H -0.2969 0.2239 0.2903 0.027 Uiso 1 1 calc R . .
H2B H -0.2561 0.1510 0.3187 0.027 Uiso 1 1 calc R . .
C3 C -0.0838(10) 0.2758(4) 0.3605(2) 0.0222(15) Uani 1 1 d . . .
H3A H -0.1906 0.2553 0.3789 0.027 Uiso 1 1 calc R . .
H3B H 0.0275 0.2862 0.3831 0.027 Uiso 1 1 calc R . .
C4 C -0.1548(9) 0.3454(4) 0.3367(3) 0.0228(15) Uani 1 1 d . . .
H4A H -0.2730 0.3353 0.3162 0.027 Uiso 1 1 calc R . .
H4B H -0.1924 0.3792 0.3619 0.027 Uiso 1 1 calc R . .
C5 C -0.0981(10) 0.4345(4) 0.2737(3) 0.0238(15) Uani 1 1 d . . .
H5A H 0.0004 0.4702 0.2648 0.029 Uiso 1 1 calc R . .
H5B H -0.2013 0.4597 0.2908 0.029 Uiso 1 1 calc R . .
C6 C -0.1904(9) 0.3998(4) 0.2276(2) 0.0235(15) Uani 1 1 d . . .
H6A H -0.2953 0.3666 0.2363 0.028 Uiso 1 1 calc R . .
H6B H -0.2500 0.4373 0.2068 0.028 Uiso 1 1 calc R . .
C7 C -0.1370(9) 0.3079(4) 0.1631(3) 0.0217(15) Uani 1 1 d . . .
H7A H -0.2482 0.3327 0.1465 0.026 Uiso 1 1 calc R . .
H7B H -0.0428 0.2944 0.1389 0.026 Uiso 1 1 calc R . .
C8 C -0.2117(9) 0.2405(4) 0.1875(3) 0.0259(16) Uani 1 1 d . . .
H8A H -0.3188 0.2536 0.2084 0.031 Uiso 1 1 calc R . .
H8B H -0.2660 0.2074 0.1627 0.031 Uiso 1 1 calc R . .
C9 C 0.0862(9) 0.1664(4) 0.1852(3) 0.0246(15) Uani 1 1 d . . .
H9A H 0.1199 0.1998 0.1595 0.030 Uiso 1 1 calc R . .
H9B H 0.0194 0.1249 0.1701 0.030 Uiso 1 1 calc R . .
C10 C 0.2771(9) 0.1408(4) 0.2114(3) 0.0212(15) Uani 1 1 d . . .
C11 C 0.1105(9) 0.1636(4) 0.3472(3) 0.0231(15) Uani 1 1 d . . .
H11A H 0.1101 0.1203 0.3270 0.028 Uiso 1 1 calc R . .
H11B H 0.0572 0.1507 0.3783 0.028 Uiso 1 1 calc R . .
C12 C 0.3221(9) 0.1906(4) 0.3552(2) 0.0211(14) Uani 1 1 d . . .
C13 C 0.1549(9) 0.4139(4) 0.3375(2) 0.0215(14) Uani 1 1 d . . .
H13A H 0.1977 0.3790 0.3623 0.026 Uiso 1 1 calc R . .
H13B H 0.0978 0.4550 0.3540 0.026 Uiso 1 1 calc R . .
C14 C 0.3366(9) 0.4398(3) 0.3123(3) 0.0208(14) Uani 1 1 d . . .
C15 C 0.1030(9) 0.4091(4) 0.1743(3) 0.0235(15) Uani 1 1 d . . .
H15C H 0.1217 0.4536 0.1929 0.028 Uiso 1 1 calc R . .
H15D H 0.0457 0.4216 0.1424 0.028 Uiso 1 1 calc R . .
C16 C 0.3015(10) 0.3719(4) 0.1691(3) 0.0257(16) Uani 1 1 d . . .
C17 C 0.5221(9) -0.0383(4) 0.0100(3) 0.0230(15) Uani 1 1 d . . .
C18 C 0.4799(10) 0.0410(4) 0.5031(3) 0.0238(16) Uani 1 1 d . . .
O19 O 0.5757(13) 0.2864(4) 0.0637(4) 0.059(3) Uani 1 1 d U . .
O20 O 0.9709(16) 0.1362(8) 0.0376(5) 0.078(4) Uani 0.50 1 d PU . .
O21 O 0.5158(10) 0.3011(4) 0.4357(3) 0.078(2) Uani 1 1 d U . .
O22 O -0.067(2) 0.1467(8) -0.0350(5) 0.049(4) Uani 0.50 1 d P . .
O23 O 0.7969(16) 0.2501(7) -0.0087(4) 0.044(3) Uani 0.50 1 d P . .
O24 O 0.202(2) 0.2093(8) 0.4669(6) 0.054(4) Uani 0.50 1 d PU . .
O25 O 0.044(2) 0.1441(10) 0.4695(7) 0.069(5) Uani 0.50 1 d PU . .
O26 O -0.0636(17) 0.0095(8) 0.0086(5) 0.059(4) Uani 0.50 1 d PU . .
O27 O 0.990(3) 0.3616(13) 0.0445(8) 0.062(6) Uani 0.50 1 d PU . .
O28 O 0.0000 0.0000 0.5000 0.058(5) Uani 1 2 d SU . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
U1 0.01994(13) 0.01991(14) 0.01819(14) -0.00130(11) 0.00134(9) 0.00058(10)
U2 0.02024(13) 0.01851(14) 0.01697(14) -0.00015(10) 0.00068(9) -0.00111(10)
O1 0.021(2) 0.026(3) 0.031(3) 0.001(2) 0.000(2) -0.002(2)
O2 0.026(2) 0.024(3) 0.022(3) -0.003(2) 0.0058(19) 0.001(2)
O3 0.025(2) 0.021(3) 0.023(3) -0.001(2) -0.0007(19) 0.001(2)
O4 0.024(2) 0.021(3) 0.026(3) -0.002(2) 0.0012(19) -0.001(2)
O5 0.023(2) 0.029(3) 0.021(3) -0.003(2) -0.0035(19) 0.006(2)
O6 0.022(2) 0.032(3) 0.021(3) -0.002(2) -0.0002(19) 0.003(2)
O7 0.022(2) 0.021(3) 0.025(3) -0.001(2) -0.0018(19) -0.001(2)
O8 0.025(3) 0.022(3) 0.059(4) 0.002(3) 0.006(2) -0.001(2)
O9 0.020(2) 0.021(2) 0.025(3) 0.001(2) -0.0016(19) -0.0049(19)
O10 0.024(2) 0.033(3) 0.025(3) -0.001(2) 0.001(2) -0.004(2)
O11 0.024(2) 0.023(3) 0.023(3) 0.002(2) 0.0041(19) -0.002(2)
O12 0.023(2) 0.027(3) 0.054(4) 0.013(3) 0.005(2) 0.001(2)
O13 0.039(3) 0.021(3) 0.021(3) -0.001(2) 0.004(2) 0.007(2)
O14 0.041(3) 0.017(3) 0.023(3) 0.000(2) 0.006(2) 0.005(2)
O15 0.063(4) 0.030(3) 0.029(3) 0.003(2) 0.006(3) 0.021(3)
O16 0.040(3) 0.017(2) 0.021(3) 0.002(2) 0.003(2) 0.005(2)
O17 0.044(3) 0.018(3) 0.015(3) 0.003(2) 0.000(2) 0.001(2)
O18 0.030(2) 0.021(3) 0.016(2) 0.000(2) 0.0041(19) 0.000(2)
N1 0.021(3) 0.016(3) 0.022(3) -0.003(2) 0.000(2) 0.001(2)
N2 0.025(3) 0.015(3) 0.028(3) -0.006(2) 0.001(2) 0.001(2)
N3 0.023(3) 0.016(3) 0.020(3) 0.000(2) 0.007(2) 0.000(2)
N4 0.018(3) 0.024(3) 0.021(3) 0.001(3) 0.001(2) 0.000(2)
C1 0.024(3) 0.021(4) 0.026(4) 0.004(3) 0.002(3) -0.005(3)
C2 0.014(3) 0.025(4) 0.030(4) -0.001(3) -0.001(3) -0.007(3)
C3 0.023(3) 0.024(4) 0.020(4) -0.002(3) 0.003(3) -0.001(3)
C4 0.019(3) 0.022(4) 0.027(4) -0.003(3) 0.006(3) 0.002(3)
C5 0.027(3) 0.017(4) 0.028(4) -0.003(3) 0.006(3) 0.002(3)
C6 0.020(3) 0.030(4) 0.020(4) -0.005(3) -0.001(3) 0.001(3)
C7 0.020(3) 0.021(4) 0.024(4) -0.001(3) 0.000(3) 0.003(3)
C8 0.022(3) 0.026(4) 0.029(4) 0.002(3) 0.000(3) 0.007(3)
C9 0.025(3) 0.027(4) 0.021(4) -0.002(3) 0.000(3) 0.004(3)
C10 0.020(3) 0.018(4) 0.026(4) -0.003(3) 0.005(3) -0.004(3)
C11 0.030(3) 0.017(3) 0.022(4) 0.002(3) 0.005(3) 0.004(3)
C12 0.025(3) 0.020(4) 0.019(4) -0.004(3) 0.006(3) -0.003(3)
C13 0.023(3) 0.024(4) 0.018(4) 0.002(3) 0.003(3) -0.005(3)
C14 0.021(3) 0.015(3) 0.026(4) -0.003(3) -0.001(3) 0.006(3)
C15 0.020(3) 0.024(4) 0.026(4) -0.001(3) -0.002(3) 0.000(3)
C16 0.027(4) 0.024(4) 0.025(4) 0.004(3) -0.008(3) 0.000(3)
C17 0.023(3) 0.021(4) 0.025(4) -0.005(3) 0.006(3) -0.001(3)
C18 0.028(4) 0.021(4) 0.023(4) 0.000(3) 0.002(3) -0.001(3)
O19 0.057(5) 0.026(4) 0.095(7) 0.005(4) 0.005(5) 0.002(4)
O20 0.060(6) 0.101(8) 0.074(7) 0.022(6) 0.006(5) 0.009(6)
O21 0.070(4) 0.061(4) 0.103(6) -0.043(4) 0.021(4) -0.009(3)
O22 0.074(10) 0.039(9) 0.034(9) 0.024(7) 0.002(7) -0.002(8)
O23 0.048(6) 0.051(8) 0.033(7) 0.003(6) 0.009(5) 0.007(6)
O24 0.050(7) 0.058(8) 0.055(8) 0.001(6) 0.006(6) 0.000(6)
O25 0.070(8) 0.076(9) 0.063(8) 0.014(7) 0.006(7) -0.006(7)
O26 0.065(7) 0.062(7) 0.049(7) 0.017(6) -0.014(6) -0.025(7)
O27 0.067(9) 0.062(10) 0.057(9) 0.009(8) 0.005(8) 0.006(8)
O28 0.072(8) 0.052(8) 0.049(8) 0.009(7) -0.016(7) -0.016(7)

_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 1.771(4) . ?
U1 O2 1.778(4) . ?
U1 O9 2.293(5) 2_645 ?
U1 O5 2.312(5) . ?
U1 O15 2.411(5) . ?
U1 O14 2.450(5) . ?
U1 O13 2.459(5) . ?
U2 O4 1.767(4) . ?
U2 O3 1.770(4) . ?
U2 O11 2.291(5) 2_645 ?
U2 O7 2.310(5) . ?
U2 O16 2.439(5) . ?
U2 O17 2.451(4) . ?
U2 O18 2.467(4) . ?
O5 C10 1.292(7) . ?
O6 C10 1.234(8) . ?
O7 C12 1.279(8) . ?
O8 C12 1.239(8) . ?
O9 C14 1.274(8) . ?
O9 U1 2.293(5) 2_655 ?
O10 C14 1.240(8) . ?
O11 C16 1.292(8) . ?
O11 U2 2.291(5) 2_655 ?
O12 C16 1.227(8) . ?
O13 C17 1.264(8) . ?
O14 C17 1.240(8) 3_655 ?
O15 H15A 0.9095 . ?
O15 H15B 0.8963 . ?
O16 C18 1.255(8) . ?
O17 C18 1.248(8) 3_656 ?
O18 H18A 0.9333 . ?
O18 H18B 0.9195 . ?
N1 C9 1.458(8) . ?
N1 C1 1.479(8) . ?
N1 C8 1.494(8) . ?
N1 H1 0.9598 . ?
N2 C11 1.488(8) . ?
N2 C2 1.498(8) . ?
N2 C3 1.529(8) . ?
N3 C13 1.459(8) . ?
N3 C5 1.474(8) . ?
N3 C4 1.489(8) . ?
N3 H3 0.8765 . ?
N4 C15 1.507(8) . ?
N4 C6 1.507(8) . ?
N4 C7 1.519(8) . ?
C1 C2 1.525(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.505(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.526(9) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.506(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.516(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C11 C12 1.510(9) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C13 C14 1.505(8) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C15 C16 1.509(9) . ?
C15 H15C 0.9700 . ?
C15 H15D 0.9700 . ?
C17 O14 1.239(8) 3_655 ?
C17 C17 1.536(13) 3_655 ?
C18 O17 1.248(8) 3_656 ?
C18 C18 1.543(13) 3_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
O1 U1 O2 179.1(2) . . ?
O1 U1 O9 90.68(19) . 2_645 ?
O2 U1 O9 89.99(18) . 2_645 ?
O1 U1 O5 91.06(19) . . ?
O2 U1 O5 89.68(18) . . ?
O9 U1 O5 77.59(16) 2_645 . ?
O1 U1 O15 87.7(2) . . ?
O2 U1 O15 91.9(2) . . ?
O9 U1 O15 153.77(17) 2_645 . ?
O5 U1 O15 76.26(17) . . ?
O1 U1 O14 91.65(19) . . ?
O2 U1 O14 87.45(18) . . ?
O9 U1 O14 138.60(16) 2_645 . ?
O5 U1 O14 143.64(16) . . ?
O15 U1 O14 67.63(16) . . ?
O1 U1 O13 87.44(19) . . ?
O2 U1 O13 92.17(18) . . ?
O9 U1 O13 73.63(16) 2_645 . ?
O5 U1 O13 151.16(16) . . ?
O15 U1 O13 132.38(17) . . ?
O14 U1 O13 65.20(15) . . ?
O4 U2 O3 180.0(3) . . ?
O4 U2 O11 91.23(18) . 2_645 ?
O3 U2 O11 88.75(18) . 2_645 ?
O4 U2 O7 89.53(18) . . ?
O3 U2 O7 90.49(18) . . ?
O11 U2 O7 146.07(16) 2_645 . ?
O4 U2 O16 89.79(19) . . ?
O3 U2 O16 90.23(19) . . ?
O11 U2 O16 139.85(16) 2_645 . ?
O7 U2 O16 74.06(16) . . ?
O4 U2 O17 91.01(19) . . ?
O3 U2 O17 88.99(19) . . ?
O11 U2 O17 73.69(16) 2_645 . ?
O7 U2 O17 140.22(16) . . ?
O16 U2 O17 66.16(15) . . ?
O4 U2 O18 90.30(18) . . ?
O3 U2 O18 89.69(18) . . ?
O11 U2 O18 73.25(16) 2_645 . ?
O7 U2 O18 72.83(15) . . ?
O16 U2 O18 146.89(15) . . ?
O17 U2 O18 146.93(15) . . ?
C10 O5 U1 145.2(4) . . ?
C12 O7 U2 145.5(4) . . ?
C14 O9 U1 142.2(4) . 2_655 ?
C16 O11 U2 143.0(4) . 2_655 ?
C17 O13 U1 120.7(4) . . ?
C17 O14 U1 121.5(4) 3_655 . ?
U1 O15 H15A 118.5 . . ?
U1 O15 H15B 133.2 . . ?
H15A O15 H15B 106.1 . . ?
C18 O16 U2 120.3(4) . . ?
C18 O17 U2 120.1(4) 3_656 . ?
U2 O18 H18A 126.6 . . ?
U2 O18 H18B 131.6 . . ?
H18A O18 H18B 101.0 . . ?
C9 N1 C1 111.2(5) . . ?
C9 N1 C8 110.1(5) . . ?
C1 N1 C8 109.3(5) . . ?
C9 N1 H1 123.4 . . ?
C1 N1 H1 94.0 . . ?
C8 N1 H1 107.4 . . ?
C11 N2 C2 111.2(5) . . ?
C11 N2 C3 110.3(5) . . ?
C2 N2 C3 110.2(5) . . ?
C13 N3 C5 110.7(5) . . ?
C13 N3 C4 110.9(5) . . ?
C5 N3 C4 109.9(5) . . ?
C13 N3 H3 107.1 . . ?
C5 N3 H3 96.4 . . ?
C4 N3 H3 120.8 . . ?
C15 N4 C6 112.6(5) . . ?
C15 N4 C7 109.5(5) . . ?
C6 N4 C7 110.4(5) . . ?
N1 C1 C2 110.6(5) . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N2 C2 C1 111.6(5) . . ?
N2 C2 H2A 109.3 . . ?
C1 C2 H2A 109.3 . . ?
N2 C2 H2B 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
C4 C3 N2 112.0(6) . . ?
C4 C3 H3A 109.2 . . ?
N2 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
N2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
N3 C4 C3 113.3(5) . . ?
N3 C4 H4A 108.9 . . ?
C3 C4 H4A 108.9 . . ?
N3 C4 H4B 108.9 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
N3 C5 C6 112.1(5) . . ?
N3 C5 H5A 109.2 . . ?
C6 C5 H5A 109.2 . . ?
N3 C5 H5B 109.2 . . ?
C6 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
N4 C6 C5 111.3(5) . . ?
N4 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
N4 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C8 C7 N4 111.2(6) . . ?
C8 C7 H7A 109.4 . . ?
N4 C7 H7A 109.4 . . ?
C8 C7 H7B 109.4 . . ?
N4 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
N1 C8 C7 112.5(5) . . ?
N1 C8 H8A 109.1 . . ?
C7 C8 H8A 109.1 . . ?
N1 C8 H8B 109.1 . . ?
C7 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
N1 C9 C10 113.5(6) . . ?
N1 C9 H9A 108.9 . . ?
C10 C9 H9A 108.9 . . ?
N1 C9 H9B 108.9 . . ?
C10 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
O6 C10 O5 122.6(6) . . ?
O6 C10 C9 123.0(6) . . ?
O5 C10 C9 114.4(6) . . ?
N2 C11 C12 111.2(5) . . ?
N2 C11 H11A 109.4 . . ?
C12 C11 H11A 109.4 . . ?
N2 C11 H11B 109.4 . . ?
C12 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
O8 C12 O7 124.4(6) . . ?
O8 C12 C11 119.3(6) . . ?
O7 C12 C11 116.2(6) . . ?
N3 C13 C14 116.5(5) . . ?
N3 C13 H13A 108.2 . . ?
C14 C13 H13A 108.2 . . ?
N3 C13 H13B 108.2 . . ?
C14 C13 H13B 108.2 . . ?
H13A C13 H13B 107.3 . . ?
O10 C14 O9 122.7(6) . . ?
O10 C14 C13 122.3(6) . . ?
O9 C14 C13 115.0(6) . . ?
N4 C15 C16 109.6(6) . . ?
N4 C15 H15C 109.8 . . ?
C16 C15 H15C 109.8 . . ?
N4 C15 H15D 109.8 . . ?
C16 C15 H15D 109.8 . . ?
H15C C15 H15D 108.2 . . ?
O12 C16 O11 124.8(6) . . ?
O12 C16 C15 120.2(6) . . ?
O11 C16 C15 114.9(6) . . ?
O14 C17 O13 127.4(6) 3_655 . ?
O14 C17 C17 116.7(8) 3_655 3_655 ?
O13 C17 C17 115.9(7) . 3_655 ?
O17 C18 O16 126.5(6) 3_656 . ?
O17 C18 C18 116.8(8) 3_656 3_656 ?
O16 C18 C18 116.7(8) . 3_656 ?

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
O15 H15A O19 0.91 1.97 2.640(10) 129.2 .
O15 H15B O20 0.90 2.30 2.882(14) 122.6 1_455
O18 H18A O6 0.93 1.72 2.644(6) 168.1 .
O18 H18B O10 0.92 1.83 2.742(6) 169.6 2_645
N1 H1 N2 0.96 2.22 2.925(8) 129.8 .
N3 H3 N4 0.88 2.36 2.954(8) 124.9 .