# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global

_journal_coden_Cambridge         1350

loop_
_publ_author_name
'Pierre Thuery'

_publ_contact_author_name        'Pierre Thuery'
_publ_contact_author_email       THUERY@DRECAM.CEA.FR

_publ_section_title              
;
Uranyl ion complexes of cucurbit[7]uril with zero-,
one- and two-dimensionality
;

# Attachment 'CIF.txt'

data_1
_database_code_depnum_ccdc_archive 'CCDC 714212'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H66 N29 O35 Re U'
_chemical_formula_weight         1961.47

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'
Re Re -1.0185 7.2310 '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'

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

_cell_length_a                   15.9084(6)
_cell_length_b                   14.3646(6)
_cell_length_c                   16.7141(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.386(2)
_cell_angle_gamma                90.00
_cell_volume                     3421.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    96071
_cell_measurement_theta_min      2.93
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1936
_exptl_absorpt_coefficient_mu    4.245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.569
_exptl_absorpt_correction_T_max  0.844
_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 (380 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            96071
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.93
_diffrn_reflns_theta_max         25.68
_reflns_number_total             12904
_reflns_number_gt                11504
_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 direct methods and subsequent Fourier-difference
synthesis. All non-hydrogen atoms were refined with anisotropic
displacement parameters, with restraints for some badly behaving atoms,
particularly in the perrhenate counter ion and solvent water molecules.
Two water O atoms were given 0.5 occupancy factors in order to retain
acceptable 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. Some voids in the lattice likely indicate the presence of
other, unresolved solvent water molecules.
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)+(0.0861P)²+2.4968P] 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   -0.014(6)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         12904
_refine_ls_number_parameters     983
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1247
_refine_ls_wR_factor_gt          0.1205
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.199
_refine_diff_density_min         -1.623
_refine_diff_density_rms         0.140

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 0.89148(2) 0.854409(19) 0.71310(2) 0.02463(9) Uani 1 1 d . . .
Re Re 0.42670(3) 0.70414(3) 0.02096(3) 0.04872(14) Uani 1 1 d . . .
O1 O 0.7973(4) 0.8380(5) 0.6059(4) 0.0342(15) Uani 1 1 d . . .
O2 O 0.9941(4) 0.8704(4) 0.8155(4) 0.0325(15) Uani 1 1 d . . .
O3 O 0.8503(5) 0.9056(5) 0.8355(5) 0.0423(10) Uani 1 1 d U . .
O4 O 0.7267(5) 0.8981(6) 0.7126(5) 0.0451(11) Uani 1 1 d U . .
O5 O 0.7168(5) 0.9429(6) 0.8324(5) 0.0452(10) Uani 1 1 d U . .
O6 O 0.8396(5) 0.7210(4) 0.7620(5) 0.0347(15) Uani 1 1 d . . .
H6A H 0.8815 0.6928 0.8047 0.042 Uiso 1 1 d R . .
H6B H 0.8053 0.6753 0.7296 0.042 Uiso 1 1 d R . .
O7 O 0.8746(4) 1.0222(4) 0.7044(4) 0.0299(14) Uani 1 1 d . . .
H7A H 0.8917 1.0509 0.7553 0.036 Uiso 1 1 d R . .
H7B H 0.8180 1.0492 0.6699 0.036 Uiso 1 1 d R . .
O8 O 0.9797(4) 0.9141(4) 0.6370(4) 0.0280(13) Uani 1 1 d . . .
O9 O 1.1972(5) 1.2171(4) 0.5644(4) 0.0315(14) Uani 1 1 d . . .
O10 O 0.8412(5) 0.8973(5) 0.3818(5) 0.0411(17) Uani 1 1 d . . .
O11 O 1.0252(5) 1.2301(4) 0.3088(4) 0.0294(14) Uani 1 1 d . . .
O12 O 0.8928(7) 0.7984(6) 0.1969(6) 0.043(2) Uani 1 1 d . . .
O13 O 1.0077(5) 1.1637(4) 0.0958(4) 0.0313(14) Uani 1 1 d . . .
O14 O 1.0592(5) 0.6542(4) 0.1728(5) 0.0371(15) Uani 1 1 d . . .
O15 O 1.2059(5) 1.0407(4) 0.1460(5) 0.0345(15) Uani 1 1 d . . .
O16 O 1.2762(4) 0.6182(4) 0.3901(4) 0.0301(14) Uani 1 1 d . . .
O17 O 1.4324(4) 0.9972(4) 0.3574(4) 0.0304(14) Uani 1 1 d . . .
O18 O 1.3424(4) 0.6740(4) 0.6324(5) 0.0329(14) Uani 1 1 d . . .
O19 O 1.5162(5) 1.0458(4) 0.6090(5) 0.0329(14) Uani 1 1 d . . .
O20 O 1.2118(5) 0.8152(4) 0.7284(4) 0.0329(14) Uani 1 1 d . . .
O21 O 1.4207(5) 1.1660(4) 0.7161(5) 0.0336(15) Uani 1 1 d . . .
O22 O 0.4086(13) 0.6063(12) -0.0358(13) 0.139(6) Uani 1 1 d U . .
O23 O 0.5431(9) 0.7268(11) 0.0685(10) 0.112(4) Uani 1 1 d U . .
O24 O 0.3669(8) 0.7920(9) -0.0515(7) 0.084(3) Uani 1 1 d U . .
O25 O 0.3836(7) 0.6896(7) 0.0952(7) 0.072(3) Uani 1 1 d U . .
O26 O 0.7118(7) 0.6144(7) 0.6490(6) 0.077(3) Uani 1 1 d . . .
H26A H 0.6602 0.6089 0.6605 0.092 Uiso 1 1 d R . .
H26B H 0.6870 0.6436 0.5976 0.092 Uiso 1 1 d R . .
O27 O 1.1946(7) 0.7875(7) 0.4826(7) 0.069(2) Uani 1 1 d . . .
H27A H 1.2385 0.7344 0.4947 0.083 Uiso 1 1 d R . .
H27B H 1.1805 0.7894 0.4303 0.083 Uiso 1 1 d R . .
O28 O 1.3857(7) 0.5025(6) 0.7306(6) 0.062(2) Uani 1 1 d . . .
H28A H 1.3869 0.5504 0.7012 0.074 Uiso 1 1 d R . .
H28B H 1.3787 0.4608 0.6967 0.074 Uiso 1 1 d R . .
O29 O 1.3188(6) 1.1011(6) 0.5257(6) 0.055(2) Uani 1 1 d . . .
H29A H 1.2769 1.1363 0.5276 0.066 Uiso 1 1 d R . .
H29B H 1.3530 1.0780 0.5758 0.066 Uiso 1 1 d R . .
O30 O 1.3616(5) 1.3409(5) 0.6326(6) 0.054(2) Uani 1 1 d . . .
H30A H 1.3202 1.3126 0.6432 0.065 Uiso 1 1 d R . .
H30B H 1.3277 1.3775 0.5952 0.065 Uiso 1 1 d R . .
O31 O 0.5425(10) 0.5499(10) -0.1076(10) 0.115(4) Uani 1 1 d . . .
H31A H 0.5184 0.5736 -0.0686 0.137 Uiso 1 1 d R . .
H31B H 0.5040 0.4983 -0.1302 0.137 Uiso 1 1 d R . .
O32 O 0.6557(9) 0.8385(10) -0.0177(9) 0.110(4) Uani 1 1 d . . .
H32A H 0.7183 0.8354 0.0199 0.132 Uiso 1 1 d R . .
H32B H 0.6343 0.8744 0.0145 0.132 Uiso 1 1 d R . .
O33 O 0.2921(10) 0.9498(9) 0.0010(8) 0.096(4) Uani 1 1 d . . .
H33A H 0.3126 0.9037 -0.0173 0.115 Uiso 1 1 d R . .
H33B H 0.2370 0.9406 -0.0043 0.115 Uiso 1 1 d R . .
O34 O 1.1165(9) 0.8188(8) 0.3064(8) 0.088(3) Uani 1 1 d . . .
H34A H 1.0554 0.8186 0.2692 0.105 Uiso 1 1 d R . .
H34B H 1.1332 0.8674 0.2917 0.105 Uiso 1 1 d R . .
O35 O 1.3316(15) 1.1828(12) 0.1259(15) 0.074(5) Uani 0.50 1 d PU . .
H35A H 1.2802 1.1462 0.0981 0.089 Uiso 0.50 1 d PR . .
H35B H 1.3697 1.1681 0.1840 0.089 Uiso 0.50 1 d PR . .
O36 O 0.9011(11) 0.5048(13) 0.7270(11) 0.058(4) Uani 0.50 1 d PU . .
H36A H 0.9082 0.4812 0.6864 0.070 Uiso 0.50 1 d PR . .
H36B H 0.9343 0.5610 0.7233 0.070 Uiso 0.50 1 d PR . .
N1 N 0.7626(5) 0.9137(6) 0.7878(6) 0.0340(10) Uani 1 1 d . . .
N2 N 1.0866(5) 1.0327(5) 0.7033(5) 0.0267(16) Uani 1 1 d . . .
N3 N 0.9618(5) 1.0600(5) 0.5773(5) 0.0286(16) Uani 1 1 d . . .
N4 N 1.0484(5) 1.1844(5) 0.5478(5) 0.0274(16) Uani 1 1 d . . .
N5 N 1.1691(6) 1.1646(5) 0.6822(6) 0.0308(17) Uani 1 1 d . . .
N6 N 0.8622(6) 1.0532(5) 0.4167(6) 0.0304(17) Uani 1 1 d . . .
N7 N 0.8217(6) 1.0108(5) 0.2767(5) 0.0346(18) Uani 1 1 d . . .
N8 N 0.8847(6) 1.1501(5) 0.2444(6) 0.0299(16) Uani 1 1 d . . .
N9 N 0.9457(5) 1.1823(5) 0.3894(5) 0.0278(15) Uani 1 1 d . . .
N10 N 0.8400(6) 0.9475(5) 0.1513(6) 0.0329(17) Uani 1 1 d . . .
N11 N 0.9062(6) 0.8702(5) 0.0788(6) 0.0376(19) Uani 1 1 d . . .
N12 N 0.9544(6) 1.0178(5) 0.0407(5) 0.0298(16) Uani 1 1 d . . .
N13 N 0.8802(6) 1.0946(5) 0.1054(6) 0.0339(18) Uani 1 1 d . . .
N14 N 1.0375(6) 0.7819(5) 0.0824(6) 0.0359(18) Uani 1 1 d . . .
N15 N 1.1811(6) 0.7254(5) 0.1534(6) 0.0315(18) Uani 1 1 d . . .
N16 N 1.2371(6) 0.8832(5) 0.1535(6) 0.0328(18) Uani 1 1 d . . .
N17 N 1.0949(5) 0.9324(5) 0.0631(5) 0.0304(16) Uani 1 1 d . . .
N18 N 1.3208(5) 0.7040(5) 0.2956(5) 0.0266(15) Uani 1 1 d . . .
N19 N 1.4058(5) 0.7104(5) 0.4426(5) 0.0248(15) Uani 1 1 d . . .
N20 N 1.4766(4) 0.8579(6) 0.4318(4) 0.0258(13) Uani 1 1 d . . .
N21 N 1.3843(5) 0.8577(6) 0.2857(5) 0.0283(14) Uani 1 1 d . . .
N22 N 1.4582(5) 0.7351(5) 0.6009(5) 0.0303(17) Uani 1 1 d . . .
N23 N 1.4427(6) 0.7903(5) 0.7178(5) 0.0301(17) Uani 1 1 d . . .
N24 N 1.5141(5) 0.9371(5) 0.7110(6) 0.0296(17) Uani 1 1 d . . .
N25 N 1.5209(6) 0.8859(5) 0.5868(5) 0.0289(16) Uani 1 1 d . . .
N26 N 1.3604(5) 0.8836(5) 0.7819(5) 0.0284(16) Uani 1 1 d . . .
N27 N 1.2408(6) 0.9654(5) 0.7831(6) 0.0297(17) Uani 1 1 d . . .
N28 N 1.3225(5) 1.1051(5) 0.7724(5) 0.0281(16) Uani 1 1 d . . .
N29 N 1.4500(5) 1.0259(5) 0.7929(6) 0.0320(17) Uani 1 1 d . . .
C1 C 1.0078(6) 0.9960(6) 0.6390(6) 0.0228(17) Uani 1 1 d . . .
C2 C 1.0040(6) 1.1525(6) 0.6034(6) 0.0266(18) Uani 1 1 d . . .
H2 H 0.9609 1.1985 0.6080 0.032 Uiso 1 1 calc R . .
C3 C 1.0911(7) 1.1325(6) 0.6953(7) 0.030(2) Uani 1 1 d . . .
H3 H 1.0864 1.1651 0.7447 0.036 Uiso 1 1 calc R . .
C4 C 1.1453(7) 1.1928(6) 0.5938(6) 0.0276(19) Uani 1 1 d . . .
C5 C 0.8686(6) 1.0482(6) 0.5057(6) 0.0304(19) Uani 1 1 d . . .
H5A H 0.8282 1.0957 0.5114 0.036 Uiso 1 1 calc R . .
H5B H 0.8447 0.9882 0.5128 0.036 Uiso 1 1 calc R . .
C6 C 0.9984(7) 1.2386(6) 0.4675(7) 0.036(2) Uani 1 1 d . . .
H6C H 0.9556 1.2806 0.4767 0.043 Uiso 1 1 calc R . .
H6D H 1.0431 1.2762 0.4569 0.043 Uiso 1 1 calc R . .
C7 C 0.8417(8) 0.9765(6) 0.3607(7) 0.037(2) Uani 1 1 d . . .
C8 C 0.8186(7) 1.1087(6) 0.2726(6) 0.0309(19) Uani 1 1 d . . .
H8 H 0.7546 1.1313 0.2364 0.037 Uiso 1 1 calc R . .
C9 C 0.8564(6) 1.1408(6) 0.3698(6) 0.0278(19) Uani 1 1 d . . .
H9 H 0.8139 1.1852 0.3777 0.033 Uiso 1 1 calc R . .
C10 C 0.9565(7) 1.1904(6) 0.3135(6) 0.029(2) Uani 1 1 d . . .
C11 C 0.7813(8) 0.9537(6) 0.1995(7) 0.038(2) Uani 1 1 d . . .
H11A H 0.7203 0.9784 0.1593 0.045 Uiso 1 1 calc R . .
H11B H 0.7720 0.8916 0.2169 0.045 Uiso 1 1 calc R . .
C12 C 0.8614(7) 1.1716(6) 0.1519(6) 0.030(2) Uani 1 1 d . . .
H12A H 0.8974 1.2254 0.1502 0.036 Uiso 1 1 calc R . .
H12B H 0.7954 1.1878 0.1207 0.036 Uiso 1 1 calc R . .
C13 C 0.8811(9) 0.8672(7) 0.1491(8) 0.046(3) Uani 1 1 d . . .
C14 C 0.8779(7) 0.9553(6) 0.0308(7) 0.032(2) Uani 1 1 d . . .
H14 H 0.8358 0.9440 -0.0323 0.039 Uiso 1 1 calc R . .
C15 C 0.8258(7) 1.0090(6) 0.0778(6) 0.0285(18) Uani 1 1 d . . .
H15 H 0.7593 1.0200 0.0380 0.034 Uiso 1 1 calc R . .
C16 C 0.9536(7) 1.0971(6) 0.0821(6) 0.0287(19) Uani 1 1 d . . .
C17 C 0.9371(7) 0.7884(6) 0.0480(8) 0.037(2) Uani 1 1 d . . .
H17A H 0.9144 0.7332 0.0656 0.045 Uiso 1 1 calc R . .
H17B H 0.9091 0.7894 -0.0167 0.045 Uiso 1 1 calc R . .
C18 C 1.0228(6) 0.9993(6) 0.0068(6) 0.0301(19) Uani 1 1 d . . .
H18A H 1.0529 1.0572 0.0042 0.036 Uiso 1 1 calc R . .
H18B H 0.9906 0.9749 -0.0534 0.036 Uiso 1 1 calc R . .
C19 C 1.0904(6) 0.7150(6) 0.1407(6) 0.0275(18) Uani 1 1 d . . .
C20 C 1.1910(7) 0.7997(6) 0.1016(6) 0.031(2) Uani 1 1 d . . .
H20 H 1.2205 0.7789 0.0642 0.038 Uiso 1 1 calc R . .
C21 C 1.0903(6) 0.8330(6) 0.0454(6) 0.029(2) Uani 1 1 d . . .
H21 H 1.0685 0.8197 -0.0183 0.035 Uiso 1 1 calc R . .
C22 C 1.1825(7) 0.9610(7) 0.1231(6) 0.028(2) Uani 1 1 d . . .
C23 C 1.2567(6) 0.6636(5) 0.2106(6) 0.0241(17) Uani 1 1 d . . .
H23A H 1.2294 0.6079 0.2220 0.029 Uiso 1 1 calc R . .
H23B H 1.2922 0.6450 0.1788 0.029 Uiso 1 1 calc R . .
C24 C 1.3395(6) 0.8920(7) 0.1968(7) 0.031(2) Uani 1 1 d . . .
H24A H 1.3642 0.8588 0.1613 0.038 Uiso 1 1 calc R . .
H24B H 1.3556 0.9572 0.1973 0.038 Uiso 1 1 calc R . .
C25 C 1.3305(6) 0.6741(6) 0.3782(6) 0.0264(19) Uani 1 1 d . . .
C26 C 1.4640(6) 0.7590(6) 0.4081(7) 0.0256(18) Uani 1 1 d . . .
H26 H 1.5241 0.7274 0.4249 0.031 Uiso 1 1 calc R . .
C27 C 1.4033(6) 0.7586(6) 0.3072(6) 0.0257(18) Uani 1 1 d . . .
H27 H 1.4362 0.7305 0.2757 0.031 Uiso 1 1 calc R . .
C28 C 1.4315(6) 0.9129(6) 0.3586(7) 0.028(2) Uani 1 1 d . . .
C29 C 1.4492(6) 0.6705(6) 0.5326(6) 0.0270(18) Uani 1 1 d . . .
H29C H 1.4119 0.6180 0.5346 0.032 Uiso 1 1 calc R . .
H29D H 1.5110 0.6473 0.5449 0.032 Uiso 1 1 calc R . .
C30 C 1.5485(7) 0.8927(7) 0.5159(6) 0.0307(19) Uani 1 1 d . . .
H30C H 1.6058 0.8574 0.5321 0.037 Uiso 1 1 calc R . .
H30D H 1.5615 0.9573 0.5087 0.037 Uiso 1 1 calc R . .
C31 C 1.4074(6) 0.7285(5) 0.6487(6) 0.0263(18) Uani 1 1 d . . .
C32 C 1.5269(6) 0.8371(5) 0.7251(6) 0.0251(19) Uani 1 1 d . . .
H32 H 1.5824 0.8214 0.7804 0.030 Uiso 1 1 calc R . .
C33 C 1.5345(6) 0.8018(6) 0.6391(6) 0.0275(18) Uani 1 1 d . . .
H33 H 1.5955 0.7729 0.6541 0.033 Uiso 1 1 calc R . .
C34 C 1.5181(7) 0.9654(6) 0.6330(6) 0.0256(18) Uani 1 1 d . . .
C35 C 1.4118(8) 0.7982(5) 0.7864(7) 0.033(2) Uani 1 1 d . . .
H35C H 1.4661 0.7952 0.8442 0.040 Uiso 1 1 calc R . .
H35D H 1.3719 0.7455 0.7820 0.040 Uiso 1 1 calc R . .
C36 C 1.5325(7) 1.0010(6) 0.7835(7) 0.034(2) Uani 1 1 d . . .
H36C H 1.5775 0.9729 0.8388 0.041 Uiso 1 1 calc R . .
H36D H 1.5607 1.0571 0.7738 0.041 Uiso 1 1 calc R . .
C37 C 1.2646(7) 0.8812(5) 0.7590(6) 0.0256(19) Uani 1 1 d . . .
C38 C 1.3230(7) 1.0264(5) 0.8274(6) 0.0276(19) Uani 1 1 d . . .
H38 H 1.3314 1.0462 0.8866 0.033 Uiso 1 1 calc R . .
C39 C 1.4053(7) 0.9673(6) 0.8328(7) 0.034(2) Uani 1 1 d . . .
H39 H 1.4483 0.9521 0.8948 0.040 Uiso 1 1 calc R . .
C40 C 1.3989(7) 1.1038(6) 0.7559(7) 0.032(2) Uani 1 1 d . . .
C41 C 1.1508(6) 0.9803(6) 0.7821(6) 0.0286(19) Uani 1 1 d . . .
H41A H 1.1596 1.0141 0.8355 0.034 Uiso 1 1 calc R . .
H41B H 1.1229 0.9206 0.7831 0.034 Uiso 1 1 calc R . .
C42 C 1.2595(7) 1.1826(6) 0.7525(7) 0.032(2) Uani 1 1 d . . .
H42A H 1.2530 1.1990 0.8058 0.038 Uiso 1 1 calc R . .
H42B H 1.2864 1.2357 0.7364 0.038 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
U O1 1.767(6) . ?
U O2 1.779(6) . ?
U O11 2.348(5) 2_746 ?
U O6 2.371(5) . ?
U O7 2.422(5) . ?
U O8 2.431(6) . ?
U O3 2.518(7) . ?
U O4 2.691(7) . ?
Re O22 1.647(16) . ?
Re O25 1.676(9) . ?
Re O23 1.690(13) . ?
Re O24 1.715(10) . ?
O3 N1 1.268(10) . ?
O4 N1 1.148(11) . ?
O5 N1 1.321(10) . ?
O6 H6A 0.8334 . ?
O6 H6B 0.8716 . ?
O7 H7A 0.8723 . ?
O7 H7B 0.9125 . ?
O8 C1 1.253(10) . ?
O9 C4 1.187(11) . ?
O10 C7 1.191(11) . ?
O11 C10 1.267(11) . ?
O11 U 2.348(5) 2_756 ?
O12 C13 1.232(13) . ?
O13 C16 1.238(11) . ?
O14 C19 1.240(11) . ?
O15 C22 1.211(11) . ?
O16 C25 1.259(10) . ?
O17 C28 1.210(11) . ?
O18 C31 1.228(10) . ?
O19 C34 1.218(10) . ?
O20 C37 1.219(10) . ?
O21 C40 1.252(11) . ?
O26 H26A 0.9270 . ?
O26 H26B 0.8772 . ?
O27 H27A 0.9926 . ?
O27 H27B 0.8012 . ?
O28 H28A 0.8501 . ?
O28 H28B 0.7980 . ?
O29 H29A 0.8496 . ?
O29 H29B 0.8373 . ?
O30 H30A 0.8574 . ?
O30 H30B 0.8116 . ?
O31 H31A 0.9538 . ?
O31 H31B 0.9272 . ?
O32 H32A 0.9121 . ?
O32 H32B 0.9139 . ?
O33 H33A 0.8532 . ?
O33 H33B 0.8508 . ?
O34 H34A 0.8918 . ?
O34 H34B 0.8222 . ?
O35 H35A 0.9068 . ?
O35 H35B 0.9125 . ?
O36 H36A 0.8102 . ?
O36 H36B 0.9822 . ?
N2 C1 1.344(12) . ?
N2 C3 1.445(11) . ?
N2 C41 1.466(12) . ?
N3 C1 1.333(11) . ?
N3 C5 1.442(12) . ?
N3 C2 1.465(11) . ?
N4 C4 1.388(12) . ?
N4 C6 1.446(12) . ?
N4 C2 1.467(11) . ?
N5 C4 1.411(12) . ?
N5 C42 1.419(13) . ?
N5 C3 1.429(11) . ?
N6 C7 1.388(12) . ?
N6 C5 1.448(12) . ?
N6 C9 1.463(11) . ?
N7 C7 1.385(13) . ?
N7 C8 1.408(12) . ?
N7 C11 1.420(13) . ?
N8 C10 1.342(13) . ?
N8 C12 1.454(12) . ?
N8 C8 1.457(12) . ?
N9 C10 1.358(12) . ?
N9 C9 1.438(12) . ?
N9 C6 1.446(12) . ?
N10 C13 1.334(14) . ?
N10 C15 1.447(12) . ?
N10 C11 1.482(12) . ?
N11 C13 1.400(13) . ?
N11 C14 1.421(12) . ?
N11 C17 1.454(12) . ?
N12 C16 1.335(12) . ?
N12 C18 1.456(11) . ?
N12 C14 1.463(12) . ?
N13 C16 1.386(12) . ?
N13 C15 1.456(11) . ?
N13 C12 1.458(11) . ?
N14 C19 1.361(12) . ?
N14 C17 1.440(13) . ?
N14 C21 1.445(12) . ?
N15 C19 1.370(12) . ?
N15 C20 1.427(11) . ?
N15 C23 1.458(12) . ?
N16 C22 1.368(12) . ?
N16 C24 1.466(12) . ?
N16 C20 1.470(12) . ?
N17 C22 1.369(12) . ?
N17 C21 1.454(11) . ?
N17 C18 1.471(12) . ?
N18 C25 1.388(11) . ?
N18 C23 1.451(11) . ?
N18 C27 1.465(11) . ?
N19 C25 1.311(12) . ?
N19 C26 1.467(10) . ?
N19 C29 1.465(11) . ?
N20 C28 1.362(12) . ?
N20 C30 1.451(12) . ?
N20 C26 1.464(11) . ?
N21 C28 1.365(12) . ?
N21 C24 1.419(12) . ?
N21 C27 1.468(12) . ?
N22 C31 1.369(11) . ?
N22 C29 1.428(12) . ?
N22 C33 1.453(11) . ?
N23 C31 1.363(12) . ?
N23 C35 1.440(12) . ?
N23 C32 1.455(11) . ?
N24 C34 1.394(11) . ?
N24 C36 1.443(12) . ?
N24 C32 1.455(10) . ?
N25 C34 1.391(11) . ?
N25 C30 1.437(12) . ?
N25 C33 1.451(11) . ?
N26 C37 1.397(12) . ?
N26 C35 1.457(11) . ?
N26 C39 1.462(11) . ?
N27 C37 1.379(11) . ?
N27 C41 1.441(12) . ?
N27 C38 1.472(12) . ?
N28 C40 1.360(11) . ?
N28 C42 1.435(11) . ?
N28 C38 1.455(11) . ?
N29 C40 1.358(12) . ?
N29 C36 1.434(12) . ?
N29 C39 1.442(12) . ?
C2 C3 1.572(14) . ?
C2 H2 0.9800 . ?
C3 H3 0.9800 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C8 C9 1.531(13) . ?
C8 H8 0.9800 . ?
C9 H9 0.9800 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 C15 1.574(12) . ?
C14 H14 0.9800 . ?
C15 H15 0.9800 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C20 C21 1.530(13) . ?
C20 H20 0.9800 . ?
C21 H21 0.9800 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C26 C27 1.525(13) . ?
C26 H26 0.9800 . ?
C27 H27 0.9800 . ?
C29 H29C 0.9700 . ?
C29 H29D 0.9700 . ?
C30 H30C 0.9700 . ?
C30 H30D 0.9700 . ?
C32 C33 1.578(12) . ?
C32 H32 0.9800 . ?
C33 H33 0.9800 . ?
C35 H35C 0.9700 . ?
C35 H35D 0.9700 . ?
C36 H36C 0.9700 . ?
C36 H36D 0.9700 . ?
C38 C39 1.528(13) . ?
C38 H38 0.9800 . ?
C39 H39 0.9800 . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U O2 174.0(3) . . ?
O1 U O11 91.3(3) . 2_746 ?
O2 U O11 84.7(3) . 2_746 ?
O1 U O6 88.5(3) . . ?
O2 U O6 94.8(3) . . ?
O11 U O6 75.3(2) 2_746 . ?
O1 U O7 92.9(3) . . ?
O2 U O7 87.6(3) . . ?
O11 U O7 143.4(2) 2_746 . ?
O6 U O7 141.1(2) . . ?
O1 U O8 86.7(3) . . ?
O2 U O8 87.7(3) . . ?
O11 U O8 71.92(19) 2_746 . ?
O6 U O8 146.7(2) . . ?
O7 U O8 72.07(19) . . ?
O1 U O3 116.9(3) . . ?
O2 U O3 68.9(3) . . ?
O11 U O3 135.8(2) 2_746 . ?
O6 U O3 72.6(2) . . ?
O7 U O3 72.3(2) . . ?
O8 U O3 137.8(2) . . ?
O1 U O4 69.0(3) . . ?
O2 U O4 116.7(3) . . ?
O11 U O4 142.5(2) 2_746 . ?
O6 U O4 72.7(2) . . ?
O7 U O4 71.7(2) . . ?
O8 U O4 134.7(2) . . ?
O3 U O4 48.0(2) . . ?
O22 Re O25 107.2(8) . . ?
O22 Re O23 108.0(8) . . ?
O25 Re O23 113.5(6) . . ?
O22 Re O24 108.7(8) . . ?
O25 Re O24 109.5(4) . . ?
O23 Re O24 109.8(6) . . ?
N1 O3 U 97.3(5) . . ?
N1 O4 U 91.8(5) . . ?
U O6 H6A 114.9 . . ?
U O6 H6B 127.8 . . ?
H6A O6 H6B 102.0 . . ?
U O7 H7A 115.8 . . ?
U O7 H7B 120.9 . . ?
H7A O7 H7B 102.1 . . ?
C1 O8 U 126.8(5) . . ?
C10 O11 U 156.2(6) . 2_756 ?
H26A O26 H26B 100.9 . . ?
H27A O27 H27B 94.5 . . ?
H28A O28 H28B 103.3 . . ?
H29A O29 H29B 111.7 . . ?
H30A O30 H30B 99.0 . . ?
H31A O31 H31B 99.8 . . ?
H32A O32 H32B 101.5 . . ?
H33A O33 H33B 112.6 . . ?
H34A O34 H34B 101.0 . . ?
H35A O35 H35B 115.6 . . ?
H36A O36 H36B 90.7 . . ?
O4 N1 O3 122.9(8) . . ?
O4 N1 O5 123.3(8) . . ?
O3 N1 O5 113.8(8) . . ?
C1 N2 C3 112.5(8) . . ?
C1 N2 C41 123.2(7) . . ?
C3 N2 C41 123.3(8) . . ?
C1 N3 C5 124.7(7) . . ?
C1 N3 C2 111.9(8) . . ?
C5 N3 C2 121.4(7) . . ?
C4 N4 C6 119.0(7) . . ?
C4 N4 C2 113.8(7) . . ?
C6 N4 C2 122.3(7) . . ?
C4 N5 C42 121.1(7) . . ?
C4 N5 C3 113.9(8) . . ?
C42 N5 C3 124.1(8) . . ?
C7 N6 C5 122.8(8) . . ?
C7 N6 C9 112.4(8) . . ?
C5 N6 C9 123.6(8) . . ?
C7 N7 C8 113.1(8) . . ?
C7 N7 C11 121.6(8) . . ?
C8 N7 C11 122.8(8) . . ?
C10 N8 C12 122.8(8) . . ?
C10 N8 C8 110.9(8) . . ?
C12 N8 C8 123.5(8) . . ?
C10 N9 C9 110.2(8) . . ?
C10 N9 C6 122.1(7) . . ?
C9 N9 C6 123.8(7) . . ?
C13 N10 C15 113.5(8) . . ?
C13 N10 C11 120.1(8) . . ?
C15 N10 C11 121.8(8) . . ?
C13 N11 C14 111.3(8) . . ?
C13 N11 C17 122.7(8) . . ?
C14 N11 C17 124.5(9) . . ?
C16 N12 C18 122.6(8) . . ?
C16 N12 C14 112.5(8) . . ?
C18 N12 C14 124.9(8) . . ?
C16 N13 C15 112.9(7) . . ?
C16 N13 C12 121.9(7) . . ?
C15 N13 C12 125.1(7) . . ?
C19 N14 C17 123.7(8) . . ?
C19 N14 C21 111.9(8) . . ?
C17 N14 C21 123.3(8) . . ?
C19 N15 C20 112.3(8) . . ?
C19 N15 C23 122.8(7) . . ?
C20 N15 C23 124.9(8) . . ?
C22 N16 C24 119.7(7) . . ?
C22 N16 C20 112.3(8) . . ?
C24 N16 C20 121.0(7) . . ?
C22 N17 C21 112.8(7) . . ?
C22 N17 C18 121.5(7) . . ?
C21 N17 C18 123.8(8) . . ?
C25 N18 C23 124.7(7) . . ?
C25 N18 C27 109.6(7) . . ?
C23 N18 C27 122.9(7) . . ?
C25 N19 C26 111.9(7) . . ?
C25 N19 C29 122.0(7) . . ?
C26 N19 C29 119.9(7) . . ?
C28 N20 C30 123.0(8) . . ?
C28 N20 C26 111.5(7) . . ?
C30 N20 C26 123.4(8) . . ?
C28 N21 C24 123.6(8) . . ?
C28 N21 C27 111.9(7) . . ?
C24 N21 C27 123.1(8) . . ?
C31 N22 C29 123.1(7) . . ?
C31 N22 C33 112.5(7) . . ?
C29 N22 C33 123.2(7) . . ?
C31 N23 C35 124.7(7) . . ?
C31 N23 C32 112.9(7) . . ?
C35 N23 C32 121.6(8) . . ?
C34 N24 C36 121.6(7) . . ?
C34 N24 C32 112.2(7) . . ?
C36 N24 C32 122.0(8) . . ?
C34 N25 C30 120.0(7) . . ?
C34 N25 C33 112.4(7) . . ?
C30 N25 C33 122.3(7) . . ?
C37 N26 C35 120.8(7) . . ?
C37 N26 C39 111.8(7) . . ?
C35 N26 C39 122.9(8) . . ?
C37 N27 C41 121.8(7) . . ?
C37 N27 C38 111.8(7) . . ?
C41 N27 C38 125.0(7) . . ?
C40 N28 C42 124.0(7) . . ?
C40 N28 C38 111.2(8) . . ?
C42 N28 C38 123.8(7) . . ?
C40 N29 C36 123.2(7) . . ?
C40 N29 C39 111.9(7) . . ?
C36 N29 C39 124.6(8) . . ?
O8 C1 N3 124.1(8) . . ?
O8 C1 N2 125.8(8) . . ?
N3 C1 N2 110.1(7) . . ?
N3 C2 N4 112.4(7) . . ?
N3 C2 C3 102.3(7) . . ?
N4 C2 C3 102.3(7) . . ?
N3 C2 H2 113.0 . . ?
N4 C2 H2 113.0 . . ?
C3 C2 H2 113.0 . . ?
N5 C3 N2 114.6(8) . . ?
N5 C3 C2 103.8(7) . . ?
N2 C3 C2 102.3(7) . . ?
N5 C3 H3 111.8 . . ?
N2 C3 H3 111.8 . . ?
C2 C3 H3 111.8 . . ?
O9 C4 N4 127.0(9) . . ?
O9 C4 N5 127.3(9) . . ?
N4 C4 N5 105.7(7) . . ?
N3 C5 N6 115.0(7) . . ?
N3 C5 H5A 108.5 . . ?
N6 C5 H5A 108.5 . . ?
N3 C5 H5B 108.5 . . ?
N6 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
N9 C6 N4 113.3(7) . . ?
N9 C6 H6C 108.9 . . ?
N4 C6 H6C 108.9 . . ?
N9 C6 H6D 108.9 . . ?
N4 C6 H6D 108.9 . . ?
H6C C6 H6D 107.7 . . ?
O10 C7 N7 127.6(10) . . ?
O10 C7 N6 126.1(10) . . ?
N7 C7 N6 106.3(8) . . ?
N7 C8 N8 114.2(7) . . ?
N7 C8 C9 105.1(7) . . ?
N8 C8 C9 102.8(8) . . ?
N7 C8 H8 111.4 . . ?
N8 C8 H8 111.4 . . ?
C9 C8 H8 111.4 . . ?
N9 C9 N6 114.4(7) . . ?
N9 C9 C8 104.4(7) . . ?
N6 C9 C8 102.2(7) . . ?
N9 C9 H9 111.7 . . ?
N6 C9 H9 111.7 . . ?
C8 C9 H9 111.7 . . ?
O11 C10 N8 124.6(8) . . ?
O11 C10 N9 124.6(9) . . ?
N8 C10 N9 110.8(8) . . ?
N7 C11 N10 113.0(8) . . ?
N7 C11 H11A 109.0 . . ?
N10 C11 H11A 109.0 . . ?
N7 C11 H11B 109.0 . . ?
N10 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
N8 C12 N13 113.0(7) . . ?
N8 C12 H12A 109.0 . . ?
N13 C12 H12A 109.0 . . ?
N8 C12 H12B 109.0 . . ?
N13 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
O12 C13 N10 127.6(10) . . ?
O12 C13 N11 123.5(10) . . ?
N10 C13 N11 108.8(8) . . ?
N11 C14 N12 115.2(8) . . ?
N11 C14 C15 104.1(7) . . ?
N12 C14 C15 103.8(7) . . ?
N11 C14 H14 111.1 . . ?
N12 C14 H14 111.1 . . ?
C15 C14 H14 111.1 . . ?
N10 C15 N13 113.6(8) . . ?
N10 C15 C14 101.9(7) . . ?
N13 C15 C14 101.6(7) . . ?
N10 C15 H15 112.9 . . ?
N13 C15 H15 112.9 . . ?
C14 C15 H15 112.9 . . ?
O13 C16 N12 126.1(9) . . ?
O13 C16 N13 124.8(8) . . ?
N12 C16 N13 109.1(8) . . ?
N14 C17 N11 113.6(8) . . ?
N14 C17 H17A 108.8 . . ?
N11 C17 H17A 108.8 . . ?
N14 C17 H17B 108.8 . . ?
N11 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
N12 C18 N17 112.0(7) . . ?
N12 C18 H18A 109.2 . . ?
N17 C18 H18A 109.2 . . ?
N12 C18 H18B 109.2 . . ?
N17 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
O14 C19 N14 124.7(8) . . ?
O14 C19 N15 127.3(8) . . ?
N14 C19 N15 108.0(7) . . ?
N15 C20 N16 114.3(7) . . ?
N15 C20 C21 103.8(8) . . ?
N16 C20 C21 102.6(7) . . ?
N15 C20 H20 111.8 . . ?
N16 C20 H20 111.8 . . ?
C21 C20 H20 111.8 . . ?
N14 C21 N17 113.4(7) . . ?
N14 C21 C20 103.2(7) . . ?
N17 C21 C20 103.7(7) . . ?
N14 C21 H21 112.0 . . ?
N17 C21 H21 112.0 . . ?
C20 C21 H21 112.0 . . ?
O15 C22 N17 125.8(9) . . ?
O15 C22 N16 126.8(9) . . ?
N17 C22 N16 107.3(8) . . ?
N18 C23 N15 114.5(7) . . ?
N18 C23 H23A 108.6 . . ?
N15 C23 H23A 108.6 . . ?
N18 C23 H23B 108.6 . . ?
N15 C23 H23B 108.6 . . ?
H23A C23 H23B 107.6 . . ?
N21 C24 N16 114.6(7) . . ?
N21 C24 H24A 108.6 . . ?
N16 C24 H24A 108.6 . . ?
N21 C24 H24B 108.6 . . ?
N16 C24 H24B 108.6 . . ?
H24A C24 H24B 107.6 . . ?
O16 C25 N19 124.4(8) . . ?
O16 C25 N18 125.1(9) . . ?
N19 C25 N18 110.5(7) . . ?
N20 C26 N19 113.0(6) . . ?
N20 C26 C27 104.3(7) . . ?
N19 C26 C27 103.4(7) . . ?
N20 C26 H26 111.9 . . ?
N19 C26 H26 111.9 . . ?
C27 C26 H26 111.9 . . ?
N18 C27 N21 114.3(7) . . ?
N18 C27 C26 103.8(7) . . ?
N21 C27 C26 103.1(7) . . ?
N18 C27 H27 111.7 . . ?
N21 C27 H27 111.7 . . ?
C26 C27 H27 111.7 . . ?
O17 C28 N20 126.1(9) . . ?
O17 C28 N21 124.8(9) . . ?
N20 C28 N21 109.0(7) . . ?
N22 C29 N19 113.6(7) . . ?
N22 C29 H29C 108.8 . . ?
N19 C29 H29C 108.8 . . ?
N22 C29 H29D 108.8 . . ?
N19 C29 H29D 108.8 . . ?
H29C C29 H29D 107.7 . . ?
N25 C30 N20 112.2(7) . . ?
N25 C30 H30C 109.2 . . ?
N20 C30 H30C 109.2 . . ?
N25 C30 H30D 109.2 . . ?
N20 C30 H30D 109.2 . . ?
H30C C30 H30D 107.9 . . ?
O18 C31 N23 126.3(8) . . ?
O18 C31 N22 124.9(8) . . ?
N23 C31 N22 108.8(7) . . ?
N23 C32 N24 112.7(7) . . ?
N23 C32 C33 102.5(7) . . ?
N24 C32 C33 103.4(6) . . ?
N23 C32 H32 112.5 . . ?
N24 C32 H32 112.5 . . ?
C33 C32 H32 112.5 . . ?
N25 C33 N22 114.3(7) . . ?
N25 C33 C32 103.3(7) . . ?
N22 C33 C32 103.0(7) . . ?
N25 C33 H33 111.8 . . ?
N22 C33 H33 111.8 . . ?
C32 C33 H33 111.8 . . ?
O19 C34 N25 126.7(8) . . ?
O19 C34 N24 125.5(8) . . ?
N25 C34 N24 107.8(7) . . ?
N23 C35 N26 114.1(7) . . ?
N23 C35 H35C 108.7 . . ?
N26 C35 H35C 108.7 . . ?
N23 C35 H35D 108.7 . . ?
N26 C35 H35D 108.7 . . ?
H35C C35 H35D 107.6 . . ?
N29 C36 N24 113.4(8) . . ?
N29 C36 H36C 108.9 . . ?
N24 C36 H36C 108.9 . . ?
N29 C36 H36D 108.9 . . ?
N24 C36 H36D 108.9 . . ?
H36C C36 H36D 107.7 . . ?
O20 C37 N27 125.3(8) . . ?
O20 C37 N26 126.8(8) . . ?
N27 C37 N26 107.7(7) . . ?
N28 C38 N27 113.0(8) . . ?
N28 C38 C39 103.5(7) . . ?
N27 C38 C39 104.2(7) . . ?
N28 C38 H38 111.9 . . ?
N27 C38 H38 111.9 . . ?
C39 C38 H38 111.9 . . ?
N29 C39 N26 115.2(8) . . ?
N29 C39 C38 103.5(7) . . ?
N26 C39 C38 103.8(8) . . ?
N29 C39 H39 111.3 . . ?
N26 C39 H39 111.3 . . ?
C38 C39 H39 111.3 . . ?
O21 C40 N29 125.4(8) . . ?
O21 C40 N28 125.5(9) . . ?
N29 C40 N28 109.1(8) . . ?
N27 C41 N2 112.2(7) . . ?
N27 C41 H41A 109.2 . . ?
N2 C41 H41A 109.2 . . ?
N27 C41 H41B 109.2 . . ?
N2 C41 H41B 109.2 . . ?
H41A C41 H41B 107.9 . . ?
N5 C42 N28 113.4(7) . . ?
N5 C42 H42A 108.9 . . ?
N28 C42 H42A 108.9 . . ?
N5 C42 H42B 108.9 . . ?
N28 C42 H42B 108.9 . . ?
H42A C42 H42B 107.7 . . ?

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
O6 H6A O13 0.83 1.86 2.663(10) 163.0 2_746
O6 H6B O26 0.87 1.74 2.575(11) 161.2 .
O7 H7A O14 0.87 1.85 2.644(9) 150.7 2_756
O7 H7B O16 0.91 1.70 2.605(8) 169.5 2_756
O26 H26A O17 0.93 2.11 2.809(10) 131.6 2_746
O26 H26B O29 0.88 2.11 2.745(13) 128.6 2_746
O27 H27A O18 0.99 2.32 3.037(12) 128.0 .
O27 H27B O34 0.80 1.91 2.678(15) 161.7 .
O28 H28A O18 0.85 2.06 2.868(11) 158.2 .
O28 H28B O30 0.80 1.98 2.768(12) 168.2 1_545
O29 H29A O9 0.85 2.01 2.838(10) 166.0 .
O30 H30A O9 0.86 2.27 2.942(10) 135.3 .
O31 H31A O22 0.95 2.10 2.99(2) 153.0 .
O31 H31B O28 0.93 2.25 2.829(19) 119.8 1_454
O33 H33A O24 0.85 2.02 2.873(18) 175.9 .
O34 H34A O12 0.89 2.34 3.211(16) 167.1 .
O34 H34B O36 0.82 2.03 2.72(2) 140.4 2_756
O35 H35A O15 0.91 2.27 2.979(19) 134.2 .

#===END

data_2
_database_code_depnum_ccdc_archive 'CCDC 714213'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H80 N32 O55 U4'
_chemical_formula_weight         2865.50

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/c'

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

_cell_length_a                   29.9954(8)
_cell_length_b                   17.6794(7)
_cell_length_c                   20.5253(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 127.974(2)
_cell_angle_gamma                90.00
_cell_volume                     8580.2(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    121095
_cell_measurement_theta_min      3.05
_cell_measurement_theta_max      25.68

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5456
_exptl_absorpt_coefficient_mu    7.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.339
_exptl_absorpt_correction_T_max  0.465
_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 (400 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            121095
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         25.68
_reflns_number_total             8106
_reflns_number_gt                6653
_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 direct methods and subsequent Fourier-difference
synthesis. Three solvent water molecules (O24, O28, O29) were affected
with 0.5 occupancy factors in order to retain acceptable displacement
parameters. All non-hydrogen atoms were refined with anisotropic
displacement parameters. The H atoms bound to O atoms were found on a
Fourier-difference map, except those of one solvent water molecule (O25)
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)+(0.0522P)²+68.8977P] 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         8106
_refine_ls_number_parameters     613
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.1013
_refine_ls_wR_factor_gt          0.0970
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         3.042
_refine_diff_density_min         -2.469
_refine_diff_density_rms         0.163

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 0.336568(10) 0.438880(14) 0.793810(15) 0.02500(9) Uani 1 1 d . . .
U2 U 0.222102(10) 0.445509(14) 0.824652(15) 0.02575(9) Uani 1 1 d . . .
O1 O 0.3877(2) 0.4328(3) 0.9008(3) 0.0453(14) Uani 1 1 d . . .
O2 O 0.2859(2) 0.4449(4) 0.6848(3) 0.0469(16) Uani 1 1 d . . .
O3 O 0.2743(2) 0.4513(3) 0.9337(3) 0.0330(11) Uani 1 1 d . . .
O4 O 0.1676(2) 0.4434(3) 0.7165(3) 0.0373(13) Uani 1 1 d . . .
O5 O 0.27782(17) 0.5145(3) 0.8030(3) 0.0249(10) Uani 1 1 d . . .
H5 H 0.2553 0.5536 0.7678 0.030 Uiso 1 1 d R . .
O6 O 0.2768(2) 0.3677(3) 0.8067(3) 0.0409(13) Uani 1 1 d . . .
H6 H 0.2805 0.3131 0.8136 0.049 Uiso 1 1 d R . .
O7 O 0.3480(3) 0.3128(3) 0.7589(5) 0.075(2) Uani 1 1 d . . .
H7A H 0.3813 0.2894 0.7869 0.090 Uiso 1 1 d R . .
H7B H 0.3202 0.2806 0.7128 0.090 Uiso 1 1 d R . .
O8 O 0.3612(2) 0.5712(3) 0.7942(4) 0.0454(14) Uani 1 1 d . . .
H8A H 0.3871 0.5904 0.8024 0.055 Uiso 1 1 d R . .
H8B H 0.3336 0.5844 0.7413 0.055 Uiso 1 1 d R . .
O9 O 0.1995(2) 0.3175(3) 0.8401(4) 0.0438(13) Uani 1 1 d . . .
H9A H 0.2316 0.3066 0.8947 0.053 Uiso 1 1 d R . .
H9B H 0.2030 0.2849 0.8126 0.053 Uiso 1 1 d R . .
O10 O 0.20088(19) 0.5778(3) 0.8278(3) 0.0294(10) Uani 1 1 d . . .
H10A H 0.1596 0.5899 0.7797 0.035 Uiso 1 1 d R . .
H10B H 0.2085 0.5877 0.8774 0.035 Uiso 1 1 d R . .
O11 O 0.1469(3) 0.2058(5) 0.9587(4) 0.072(2) Uani 1 1 d . . .
O12 O 0.1642(3) 0.1647(4) 0.8759(5) 0.0703(19) Uani 1 1 d . . .
O13 O 0.0773(3) 0.1841(3) 0.8280(4) 0.0595(17) Uani 1 1 d . . .
O14 O 0.1889(2) 0.2790(3) 1.1186(4) 0.0566(17) Uani 1 1 d . . .
O15 O 0.2758(2) 0.3125(3) 1.2134(3) 0.0474(14) Uani 1 1 d . . .
O16 O 0.2072(2) 0.3925(3) 1.1667(3) 0.0397(12) Uani 1 1 d . . .
O17 O 0.41262(19) 0.4369(3) 0.7832(3) 0.0283(10) Uani 1 1 d . . .
O18 O 0.67276(19) 0.3267(3) 0.9017(3) 0.0314(10) Uani 1 1 d . . .
O19 O 0.51207(18) 0.3454(3) 0.9819(3) 0.0293(10) Uani 1 1 d . . .
O20 O 0.70834(19) 0.1296(3) 0.9598(3) 0.0303(11) Uani 1 1 d . . .
O21 O 0.52891(19) 0.1376(3) 1.0111(3) 0.0344(11) Uani 1 1 d . . .
O22 O 0.64694(18) -0.0491(3) 0.8357(3) 0.0267(10) Uani 1 1 d . . .
O23 O 0.46308(18) -0.0247(3) 0.8674(3) 0.0290(10) Uani 1 1 d . . .
O24 O 0.4454(5) 0.2405(8) 0.8552(7) 0.061(4) Uani 0.50 1 d P . .
H24A H 0.4362 0.2001 0.8269 0.073 Uiso 0.50 1 d PR . .
H24B H 0.4625 0.2762 0.8454 0.073 Uiso 0.50 1 d PR . .
O25 O 0.4491(2) 0.6318(3) 0.8188(4) 0.0562(16) Uani 1 1 d . . .
O26 O 0.0940(3) 0.6062(4) 0.7066(5) 0.091(3) Uani 1 1 d U . .
H26A H 0.0758 0.5515 0.6887 0.110 Uiso 1 1 d R . .
H26B H 0.1006 0.6086 0.6692 0.110 Uiso 1 1 d R . .
O27 O 0.2197(2) 0.3253(3) 0.9866(4) 0.0557(16) Uani 1 1 d . . .
H27A H 0.2071 0.2890 0.9962 0.067 Uiso 1 1 d R . .
H27B H 0.2491 0.3500 1.0388 0.067 Uiso 1 1 d R . .
O28 O 0.5438(4) 0.7009(6) 0.9498(6) 0.041(3) Uani 0.50 1 d PU . .
H28A H 0.5144 0.6772 0.9133 0.049 Uiso 0.50 1 d PR . .
H28B H 0.5754 0.6653 0.9713 0.049 Uiso 0.50 1 d PR . .
O29 O 0.0567(6) 0.5976(10) 0.8183(10) 0.088(5) Uani 0.50 1 d PU . .
H29A H 0.0502 0.5654 0.7785 0.105 Uiso 0.50 1 d PR . .
H29B H 0.0754 0.5608 0.8688 0.105 Uiso 0.50 1 d PR . .
N1 N 0.1294(3) 0.1868(4) 0.8879(5) 0.0532(19) Uani 1 1 d . . .
N2 N 0.2232(2) 0.3275(3) 1.1662(4) 0.0352(14) Uani 1 1 d . . .
N3 N 0.5004(2) 0.4778(3) 0.8301(3) 0.0230(11) Uani 1 1 d . . .
N4 N 0.5698(2) 0.4846(3) 0.8037(3) 0.0254(12) Uani 1 1 d . . .
N5 N 0.5663(2) 0.4226(3) 0.9658(3) 0.0258(12) Uani 1 1 d . . .
N6 N 0.6054(2) 0.3196(3) 1.0427(3) 0.0233(11) Uani 1 1 d . . .
N7 N 0.6734(2) 0.3157(3) 1.0141(3) 0.0236(11) Uani 1 1 d . . .
N8 N 0.6320(2) 0.4156(3) 0.9332(3) 0.0241(11) Uani 1 1 d . . .
N9 N 0.6181(2) 0.1845(3) 1.0660(3) 0.0257(12) Uani 1 1 d . . .
N10 N 0.5995(2) 0.0626(3) 1.0306(3) 0.0249(12) Uani 1 1 d . . .
N11 N 0.6723(2) 0.0582(3) 1.0127(3) 0.0216(11) Uani 1 1 d . . .
N12 N 0.6889(2) 0.1810(3) 1.0432(3) 0.0242(11) Uani 1 1 d . . .
N13 N 0.5586(2) -0.0522(3) 0.9493(3) 0.0244(12) Uani 1 1 d . . .
N14 N 0.5009(2) -0.1094(3) 0.8274(3) 0.0245(12) Uani 1 1 d . . .
N15 N 0.5780(2) -0.1236(3) 0.8188(3) 0.0252(12) Uani 1 1 d . . .
N16 N 0.6320(2) -0.0558(3) 0.9326(3) 0.0237(12) Uani 1 1 d . . .
C1 C 0.4448(3) 0.4637(4) 0.7707(4) 0.0228(14) Uani 1 1 d . . .
C2 C 0.5243(2) 0.5212(4) 0.7977(4) 0.0237(13) Uani 1 1 d . . .
H2 H 0.5345 0.5726 0.8202 0.028 Uiso 1 1 calc R . .
C3 C 0.5252(3) 0.4805(4) 0.9179(4) 0.0247(14) Uani 1 1 d . . .
H3A H 0.5430 0.5295 0.9402 0.030 Uiso 1 1 calc R . .
H3B H 0.4953 0.4756 0.9230 0.030 Uiso 1 1 calc R . .
C4 C 0.6269(2) 0.4762(4) 0.8811(4) 0.0259(14) Uani 1 1 d . . .
H4A H 0.6528 0.4665 0.8687 0.031 Uiso 1 1 calc R . .
H4B H 0.6382 0.5234 0.9116 0.031 Uiso 1 1 calc R . .
C5 C 0.5566(3) 0.3602(4) 0.9955(4) 0.0241(13) Uani 1 1 d . . .
C6 C 0.6247(3) 0.4274(4) 0.9960(4) 0.0240(13) Uani 1 1 d . . .
H6A H 0.6431 0.4740 1.0273 0.029 Uiso 1 1 calc R . .
C7 C 0.6525(2) 0.3560(4) 1.0513(4) 0.0239(13) Uani 1 1 d . . .
H7 H 0.6830 0.3694 1.1089 0.029 Uiso 1 1 calc R . .
C8 C 0.6605(3) 0.3493(4) 0.9447(4) 0.0269(14) Uani 1 1 d . . .
C9 C 0.6123(3) 0.2565(4) 1.0933(4) 0.0296(15) Uani 1 1 d . . .
H9C H 0.6456 0.2652 1.1499 0.036 Uiso 1 1 calc R . .
H9D H 0.5799 0.2544 1.0930 0.036 Uiso 1 1 calc R . .
C10 C 0.7144(2) 0.2543(4) 1.0562(4) 0.0267(14) Uani 1 1 d . . .
H10C H 0.7369 0.2528 1.0369 0.032 Uiso 1 1 calc R . .
H10D H 0.7397 0.2648 1.1150 0.032 Uiso 1 1 calc R . .
C11 C 0.5765(3) 0.1296(4) 1.0327(4) 0.0274(14) Uani 1 1 d . . .
C12 C 0.6720(3) 0.1544(4) 1.0922(4) 0.0219(13) Uani 1 1 d . . .
H12 H 0.7020 0.1616 1.1515 0.026 Uiso 1 1 calc R . .
C13 C 0.6591(3) 0.0697(3) 1.0690(4) 0.0219(13) Uani 1 1 d . . .
H13 H 0.6823 0.0373 1.1179 0.026 Uiso 1 1 calc R . .
C14 C 0.6918(3) 0.1240(4) 1.0010(4) 0.0230(13) Uani 1 1 d . . .
C15 C 0.5753(3) -0.0103(4) 1.0229(4) 0.0279(14) Uani 1 1 d . . .
H15A H 0.5423 -0.0034 1.0207 0.033 Uiso 1 1 calc R . .
H15B H 0.6025 -0.0401 1.0716 0.033 Uiso 1 1 calc R . .
C16 C 0.6835(2) -0.0156(4) 0.9975(4) 0.0246(14) Uani 1 1 d . . .
H16A H 0.7035 -0.0449 1.0482 0.029 Uiso 1 1 calc R . .
H16B H 0.7080 -0.0111 0.9817 0.029 Uiso 1 1 calc R . .
C17 C 0.5038(3) -0.0584(4) 0.8813(4) 0.0255(14) Uani 1 1 d . . .
C18 C 0.5968(2) -0.0987(4) 0.9461(4) 0.0225(13) Uani 1 1 d . . .
H18 H 0.6190 -0.1330 0.9936 0.027 Uiso 1 1 calc R . .
C19 C 0.5557(2) -0.1422(4) 0.8627(4) 0.0242(14) Uani 1 1 d . . .
H19 H 0.5562 -0.1968 0.8714 0.029 Uiso 1 1 calc R . .
C20 C 0.6208(3) -0.0738(3) 0.8594(4) 0.0216(13) Uani 1 1 d . . .
C21 C 0.4483(2) -0.1475(4) 0.7656(4) 0.0266(14) Uani 1 1 d . . .
H21A H 0.4220 -0.1386 0.7773 0.032 Uiso 1 1 calc R . .
H21B H 0.4553 -0.2015 0.7698 0.032 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 O1 1.743(5) . ?
U1 O2 1.772(5) . ?
U1 O5 2.309(4) . ?
U1 O6 2.335(5) . ?
U1 O17 2.422(4) . ?
U1 O7 2.430(6) . ?
U1 O8 2.451(5) . ?
U1 U2 3.8572(3) . ?
U2 O4 1.771(5) . ?
U2 O3 1.777(5) . ?
U2 O5 2.322(4) . ?
U2 O6 2.337(5) . ?
U2 O22 2.403(4) 3_455 ?
U2 O10 2.436(5) . ?
U2 O9 2.439(5) . ?
O5 H5 0.9251 . ?
O6 H6 0.9728 . ?
O7 H7A 0.8886 . ?
O7 H7B 0.9714 . ?
O8 H8A 0.7663 . ?
O8 H8B 0.9022 . ?
O9 H9A 0.9451 . ?
O9 H9B 0.8564 . ?
O10 H10A 1.0245 . ?
O10 H10B 0.9113 . ?
O11 N1 1.250(10) . ?
O12 N1 1.272(10) . ?
O13 N1 1.262(9) . ?
O14 N2 1.230(8) . ?
O15 N2 1.273(8) . ?
O16 N2 1.247(8) . ?
O17 C1 1.235(8) . ?
O18 C8 1.215(8) . ?
O19 C5 1.214(8) . ?
O20 C14 1.218(8) . ?
O21 C11 1.216(8) . ?
O22 C20 1.229(8) . ?
O22 U2 2.403(4) 3_545 ?
O23 C17 1.225(8) . ?
O24 H24A 0.8525 . ?
O24 H24B 0.9096 . ?
O26 H26A 1.0593 . ?
O26 H26B 0.9009 . ?
O27 H27A 0.8259 . ?
O27 H27B 0.9767 . ?
O28 H28A 0.8387 . ?
O28 H28B 0.9863 . ?
O29 H29A 0.9132 . ?
O29 H29B 1.0479 . ?
N3 C1 1.351(8) . ?
N3 C2 1.462(8) . ?
N3 C3 1.467(8) . ?
N4 C1 1.356(8) 2_656 ?
N4 C2 1.444(8) . ?
N4 C4 1.460(8) . ?
N5 C5 1.374(8) . ?
N5 C3 1.429(8) . ?
N5 C6 1.458(8) . ?
N6 C5 1.360(8) . ?
N6 C9 1.450(8) . ?
N6 C7 1.459(8) . ?
N7 C8 1.363(8) . ?
N7 C7 1.440(8) . ?
N7 C10 1.460(8) . ?
N8 C8 1.382(8) . ?
N8 C6 1.449(8) . ?
N8 C4 1.454(8) . ?
N9 C11 1.385(9) . ?
N9 C9 1.444(8) . ?
N9 C12 1.454(8) . ?
N10 C11 1.383(9) . ?
N10 C15 1.440(8) . ?
N10 C13 1.449(8) . ?
N11 C14 1.388(8) . ?
N11 C16 1.428(8) . ?
N11 C13 1.448(8) . ?
N12 C14 1.367(8) . ?
N12 C10 1.442(8) . ?
N12 C12 1.456(8) . ?
N13 C17 1.356(8) . ?
N13 C18 1.443(8) . ?
N13 C15 1.466(9) . ?
N14 C17 1.387(8) . ?
N14 C21 1.445(8) . ?
N14 C19 1.448(8) . ?
N15 C20 1.343(8) . ?
N15 C19 1.454(8) . ?
N15 C21 1.455(8) 2_656 ?
N16 C20 1.359(8) . ?
N16 C18 1.460(8) . ?
N16 C16 1.462(8) . ?
C1 N4 1.356(8) 2_656 ?
C2 C2 1.563(12) 2_656 ?
C2 H2 0.9800 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 C7 1.552(9) . ?
C6 H6A 0.9800 . ?
C7 H7 0.9800 . ?
C9 H9C 0.9700 . ?
C9 H9D 0.9700 . ?
C10 H10C 0.9700 . ?
C10 H10D 0.9700 . ?
C12 C13 1.547(9) . ?
C12 H12 0.9800 . ?
C13 H13 0.9800 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C18 C19 1.563(9) . ?
C18 H18 0.9800 . ?
C19 H19 0.9800 . ?
C21 N15 1.455(8) 2_656 ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2 178.6(2) . . ?
O1 U1 O5 93.2(2) . . ?
O2 U1 O5 87.9(2) . . ?
O1 U1 O6 88.0(2) . . ?
O2 U1 O6 93.1(2) . . ?
O5 U1 O6 67.97(17) . . ?
O1 U1 O17 88.0(2) . . ?
O2 U1 O17 90.6(2) . . ?
O5 U1 O17 145.45(16) . . ?
O6 U1 O17 146.54(16) . . ?
O1 U1 O7 98.1(3) . . ?
O2 U1 O7 81.4(3) . . ?
O5 U1 O7 143.95(18) . . ?
O6 U1 O7 78.30(19) . . ?
O17 U1 O7 69.40(18) . . ?
O1 U1 O8 91.4(3) . . ?
O2 U1 O8 88.2(2) . . ?
O5 U1 O8 72.01(17) . . ?
O6 U1 O8 139.87(18) . . ?
O17 U1 O8 73.44(17) . . ?
O7 U1 O8 141.2(2) . . ?
O4 U2 O3 176.6(2) . . ?
O4 U2 O5 89.38(19) . . ?
O3 U2 O5 91.76(19) . . ?
O4 U2 O6 89.2(2) . . ?
O3 U2 O6 94.2(2) . . ?
O5 U2 O6 67.73(17) . . ?
O4 U2 O22 85.58(19) . 3_455 ?
O3 U2 O22 91.70(19) . 3_455 ?
O5 U2 O22 145.57(15) . 3_455 ?
O6 U2 O22 145.98(16) . 3_455 ?
O4 U2 O10 89.9(2) . . ?
O3 U2 O10 87.3(2) . . ?
O5 U2 O10 74.45(15) . . ?
O6 U2 O10 142.17(17) . . ?
O22 U2 O10 71.52(15) 3_455 . ?
O4 U2 O9 91.6(2) . . ?
O3 U2 O9 89.4(2) . . ?
O5 U2 O9 143.38(16) . . ?
O6 U2 O9 75.68(17) . . ?
O22 U2 O9 70.89(16) 3_455 . ?
O10 U2 O9 142.15(17) . . ?
U1 O5 U2 112.76(19) . . ?
U1 O5 H5 126.5 . . ?
U2 O5 H5 106.1 . . ?
U1 O6 U2 111.3(2) . . ?
U1 O6 H6 121.5 . . ?
U2 O6 H6 126.3 . . ?
U1 O7 H7A 122.9 . . ?
U1 O7 H7B 129.1 . . ?
H7A O7 H7B 107.9 . . ?
U1 O8 H8A 133.5 . . ?
U1 O8 H8B 101.0 . . ?
H8A O8 H8B 101.8 . . ?
U2 O9 H9A 100.4 . . ?
U2 O9 H9B 112.5 . . ?
H9A O9 H9B 101.3 . . ?
U2 O10 H10A 110.8 . . ?
U2 O10 H10B 108.9 . . ?
H10A O10 H10B 111.1 . . ?
C1 O17 U1 155.9(4) . . ?
C20 O22 U2 152.5(4) . 3_545 ?
H24A O24 H24B 114.8 . . ?
H26A O26 H26B 94.8 . . ?
H27A O27 H27B 108.9 . . ?
H28A O28 H28B 105.9 . . ?
H29A O29 H29B 100.8 . . ?
O11 N1 O13 121.6(8) . . ?
O11 N1 O12 120.0(8) . . ?
O13 N1 O12 118.2(8) . . ?
O14 N2 O16 120.8(6) . . ?
O14 N2 O15 119.9(6) . . ?
O16 N2 O15 119.2(6) . . ?
C1 N3 C2 111.3(5) . . ?
C1 N3 C3 121.8(5) . . ?
C2 N3 C3 121.5(5) . . ?
C1 N4 C2 113.0(5) 2_656 . ?
C1 N4 C4 123.2(5) 2_656 . ?
C2 N4 C4 123.6(5) . . ?
C5 N5 C3 123.6(5) . . ?
C5 N5 C6 112.6(5) . . ?
C3 N5 C6 123.5(5) . . ?
C5 N6 C9 122.2(5) . . ?
C5 N6 C7 113.0(5) . . ?
C9 N6 C7 123.4(5) . . ?
C8 N7 C7 113.7(5) . . ?
C8 N7 C10 122.5(5) . . ?
C7 N7 C10 122.5(5) . . ?
C8 N8 C6 112.7(5) . . ?
C8 N8 C4 121.6(5) . . ?
C6 N8 C4 122.9(5) . . ?
C11 N9 C9 121.6(5) . . ?
C11 N9 C12 112.6(5) . . ?
C9 N9 C12 123.4(5) . . ?
C11 N10 C15 122.8(5) . . ?
C11 N10 C13 112.4(5) . . ?
C15 N10 C13 120.5(5) . . ?
C14 N11 C16 123.1(5) . . ?
C14 N11 C13 111.8(5) . . ?
C16 N11 C13 121.3(5) . . ?
C14 N12 C10 123.1(5) . . ?
C14 N12 C12 112.6(5) . . ?
C10 N12 C12 122.2(5) . . ?
C17 N13 C18 113.5(5) . . ?
C17 N13 C15 122.0(5) . . ?
C18 N13 C15 123.9(5) . . ?
C17 N14 C21 120.2(5) . . ?
C17 N14 C19 111.4(5) . . ?
C21 N14 C19 122.9(5) . . ?
C20 N15 C19 113.1(5) . . ?
C20 N15 C21 122.7(6) . 2_656 ?
C19 N15 C21 123.6(5) . 2_656 ?
C20 N16 C18 112.0(5) . . ?
C20 N16 C16 121.6(5) . . ?
C18 N16 C16 124.2(5) . . ?
O17 C1 N3 124.8(6) . . ?
O17 C1 N4 125.8(6) . 2_656 ?
N3 C1 N4 109.3(5) . 2_656 ?
N4 C2 N3 115.4(5) . . ?
N4 C2 C2 102.3(6) . 2_656 ?
N3 C2 C2 103.2(5) . 2_656 ?
N4 C2 H2 111.7 . . ?
N3 C2 H2 111.7 . . ?
C2 C2 H2 111.7 2_656 . ?
N5 C3 N3 113.1(5) . . ?
N5 C3 H3A 109.0 . . ?
N3 C3 H3A 109.0 . . ?
N5 C3 H3B 109.0 . . ?
N3 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
N8 C4 N4 113.3(5) . . ?
N8 C4 H4A 108.9 . . ?
N4 C4 H4A 108.9 . . ?
N8 C4 H4B 108.9 . . ?
N4 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
O19 C5 N6 126.9(6) . . ?
O19 C5 N5 124.9(6) . . ?
N6 C5 N5 108.2(5) . . ?
N8 C6 N5 114.4(5) . . ?
N8 C6 C7 103.2(5) . . ?
N5 C6 C7 103.1(5) . . ?
N8 C6 H6A 111.8 . . ?
N5 C6 H6A 111.8 . . ?
C7 C6 H6A 111.8 . . ?
N7 C7 N6 114.9(5) . . ?
N7 C7 C6 103.1(5) . . ?
N6 C7 C6 103.1(5) . . ?
N7 C7 H7 111.7 . . ?
N6 C7 H7 111.7 . . ?
C6 C7 H7 111.7 . . ?
O18 C8 N7 126.8(6) . . ?
O18 C8 N8 125.9(6) . . ?
N7 C8 N8 107.3(6) . . ?
N9 C9 N6 113.4(5) . . ?
N9 C9 H9C 108.9 . . ?
N6 C9 H9C 108.9 . . ?
N9 C9 H9D 108.9 . . ?
N6 C9 H9D 108.9 . . ?
H9C C9 H9D 107.7 . . ?
N12 C10 N7 113.7(5) . . ?
N12 C10 H10C 108.8 . . ?
N7 C10 H10C 108.8 . . ?
N12 C10 H10D 108.8 . . ?
N7 C10 H10D 108.8 . . ?
H10C C10 H10D 107.7 . . ?
O21 C11 N10 125.8(6) . . ?
O21 C11 N9 126.7(6) . . ?
N10 C11 N9 107.5(5) . . ?
N9 C12 N12 114.0(5) . . ?
N9 C12 C13 103.3(5) . . ?
N12 C12 C13 103.1(5) . . ?
N9 C12 H12 111.9 . . ?
N12 C12 H12 111.9 . . ?
C13 C12 H12 111.9 . . ?
N11 C13 N10 113.9(5) . . ?
N11 C13 C12 104.1(5) . . ?
N10 C13 C12 104.0(5) . . ?
N11 C13 H13 111.4 . . ?
N10 C13 H13 111.4 . . ?
C12 C13 H13 111.4 . . ?
O20 C14 N12 126.2(6) . . ?
O20 C14 N11 125.7(6) . . ?
N12 C14 N11 108.1(5) . . ?
N10 C15 N13 113.3(5) . . ?
N10 C15 H15A 108.9 . . ?
N13 C15 H15A 108.9 . . ?
N10 C15 H15B 108.9 . . ?
N13 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
N11 C16 N16 112.5(5) . . ?
N11 C16 H16A 109.1 . . ?
N16 C16 H16A 109.1 . . ?
N11 C16 H16B 109.1 . . ?
N16 C16 H16B 109.1 . . ?
H16A C16 H16B 107.8 . . ?
O23 C17 N13 127.1(6) . . ?
O23 C17 N14 124.4(6) . . ?
N13 C17 N14 108.4(6) . . ?
N13 C18 N16 113.5(5) . . ?
N13 C18 C19 102.5(5) . . ?
N16 C18 C19 102.8(5) . . ?
N13 C18 H18 112.4 . . ?
N16 C18 H18 112.4 . . ?
C19 C18 H18 112.4 . . ?
N14 C19 N15 114.3(5) . . ?
N14 C19 C18 103.8(5) . . ?
N15 C19 C18 102.4(5) . . ?
N14 C19 H19 111.9 . . ?
N15 C19 H19 111.9 . . ?
C18 C19 H19 111.9 . . ?
O22 C20 N15 125.9(6) . . ?
O22 C20 N16 124.8(6) . . ?
N15 C20 N16 109.3(5) . . ?
N14 C21 N15 114.1(5) . 2_656 ?
N14 C21 H21A 108.7 . . ?
N15 C21 H21A 108.7 2_656 . ?
N14 C21 H21B 108.7 . . ?
N15 C21 H21B 108.7 2_656 . ?
H21A C21 H21B 107.6 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5 O16 0.93 1.90 2.778(7) 157.9 6_565
O6 H6 O14 0.97 1.96 2.863(8) 152.6 7_557
O7 H7A O24 0.89 1.76 2.640(14) 170.2 .
O8 H8A O25 0.77 1.83 2.591(8) 176.7 .
O9 H9A O27 0.95 2.15 2.682(9) 114.3 .
O9 H9B O14 0.86 2.86 3.369(8) 120.2 7_557
O10 H10A O26 1.02 1.60 2.627(8) 177.2 .
O10 H10B O20 0.91 1.85 2.736(6) 163.1 3_455
O24 H24A O26 0.85 1.81 2.606(15) 154.4 4_546
O26 H26A O23 1.06 1.69 2.720(8) 163.4 4_556
O27 H27A O11 0.83 2.08 2.832(10) 151.9 .
O28 H28A O25 0.84 1.89 2.720(12) 170.6 .

#===END

data_3
_database_code_depnum_ccdc_archive 'CCDC 714214'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H68 N28 O35 U2'
_chemical_formula_weight         2025.32

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 c'

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

_cell_length_a                   17.8166(8)
_cell_length_b                   20.4976(9)
_cell_length_c                   19.1340(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.607(3)
_cell_angle_gamma                90.00
_cell_volume                     6987.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    86453
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      25.68

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3968
_exptl_absorpt_coefficient_mu    4.742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.494
_exptl_absorpt_correction_T_max  0.718
_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 (486 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            86453
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         25.68
_reflns_number_total             12947
_reflns_number_gt                11954
_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 direct methods and subsequent Fourier-difference
synthesis. All non-hydrogen atoms were refined with anisotropic
displacement parameters. Four solvent water molecules were given
occupancy parameters of 0.5 so as to retain acceptable displacement
parameters. Restraints on displacement parameters were applied for some
badly behaving atoms, particularly those of the solvent molecules. The H
atoms bound to O atoms were not found and only those of O5 and O6 were
introduced at ideal positions. The C-bound H atoms 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. Some
voids in the lattice likely indicate the presence of other, unresolved
water solvent molecules. The highest residual electron density peaks are
located near the U atoms as a result of imperfect absorption corrections.
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)+(0.0788P)²+71.9449P] 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   0.478(9)
_refine_ls_number_reflns         12947
_refine_ls_number_parameters     1001
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0608
_refine_ls_wR_factor_ref         0.1638
_refine_ls_wR_factor_gt          0.1611
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         4.376
_refine_diff_density_min         -1.807
_refine_diff_density_rms         0.225

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 0.38307(3) 0.67628(2) 0.32147(2) 0.02145(13) Uani 1 1 d . . .
U2 U 0.39815(3) 0.80074(3) 0.47018(3) 0.02874(15) Uani 1 1 d . . .
O1 O 0.4686(6) 0.6975(6) 0.2786(6) 0.033(3) Uani 1 1 d . . .
O2 O 0.2975(6) 0.6546(6) 0.3631(6) 0.033(2) Uani 1 1 d . . .
O3 O 0.4861(7) 0.8375(6) 0.4491(7) 0.045(3) Uani 1 1 d . . .
O4 O 0.3089(7) 0.7664(6) 0.4986(7) 0.046(3) Uani 1 1 d . . .
O5 O 0.3663(7) 0.7842(5) 0.3545(5) 0.032(2) Uani 1 1 d . . .
H5 H 0.3488 0.8168 0.3247 0.038 Uiso 1 1 calc R . .
O6 O 0.4360(6) 0.6980(5) 0.4303(6) 0.032(2) Uani 1 1 d . . .
H6 H 0.4678 0.6699 0.4547 0.038 Uiso 1 1 calc R . .
O7 O 0.4299(7) 0.5707(5) 0.3603(6) 0.034(3) Uani 1 1 d . . .
O8 O 0.3084(7) 0.7188(6) 0.2293(7) 0.044(3) Uani 1 1 d . . .
O9 O 0.3848(11) 0.8086(9) 0.1957(9) 0.079(5) Uani 1 1 d . . .
O10 O 0.4632(9) 0.7423(7) 0.5691(8) 0.064(4) Uani 1 1 d . . .
O11 O 0.3918(8) 0.8704(6) 0.5738(6) 0.044(3) Uani 1 1 d . . .
O12 O 0.3360(6) 0.9004(6) 0.4380(6) 0.036(3) Uani 1 1 d . . .
O13 O 0.3747(10) 0.9154(6) 0.3213(9) 0.059(4) Uani 1 1 d . . .
O14 O 0.3641(5) 0.5930(5) 0.2293(5) 0.0217(16) Uani 1 1 d . . .
O15 O 0.3737(6) 0.3936(5) 0.0167(5) 0.028(2) Uani 1 1 d . . .
O16 O 0.1899(6) 0.5370(5) 0.2947(6) 0.030(2) Uani 1 1 d . . .
O17 O 0.1719(8) 0.3288(7) 0.0644(7) 0.043(3) Uani 1 1 d . . .
O18 O 0.1585(6) 0.4111(5) 0.4269(6) 0.034(3) Uani 1 1 d . . .
O19 O 0.1465(6) 0.2073(6) 0.1859(6) 0.042(3) Uani 1 1 d . . .
O20 O 0.3119(6) 0.3090(5) 0.5166(5) 0.030(2) Uani 1 1 d . . .
O21 O 0.2964(6) 0.1004(6) 0.2904(5) 0.034(3) Uani 1 1 d . . .
O22 O 0.4997(6) 0.3118(5) 0.5095(5) 0.032(2) Uani 1 1 d . . .
O23 O 0.4895(6) 0.1088(5) 0.2777(5) 0.032(3) Uani 1 1 d . . .
O24 O 0.6161(6) 0.4258(5) 0.4040(6) 0.034(2) Uani 1 1 d . . .
O25 O 0.6149(6) 0.2329(7) 0.1588(6) 0.039(3) Uani 1 1 d . . .
O26 O 0.5501(6) 0.5451(5) 0.2788(5) 0.033(2) Uani 1 1 d . . .
O27 O 0.5620(6) 0.3551(6) 0.0389(6) 0.038(3) Uani 1 1 d . . .
O28 O 0.3126(7) 0.4957(7) 0.3782(10) 0.074(5) Uani 1 1 d . . .
O29 O 0.3159(13) 0.6876(10) 0.6358(10) 0.030(5) Uani 0.50 1 d PU . .
O30 O 0.2627(9) 0.8790(7) 0.6500(7) 0.057(4) Uani 1 1 d . . .
O31 O 0.5276(7) 0.8816(5) 0.6384(6) 0.038(3) Uani 1 1 d . . .
O32 O 0.3885(17) 0.9968(15) 0.2108(14) 0.051(7) Uani 0.50 1 d PU . .
O33 O 0.0382(9) 0.4914(8) 0.4810(8) 0.064(4) Uani 1 1 d . . .
O34 O 0.3426(11) 0.3661(8) 0.3823(9) 0.079(5) Uani 1 1 d . . .
O35 O 0.7058(11) 0.5188(9) 0.4763(10) 0.081(5) Uani 1 1 d U . .
O36 O 0.3609(17) 1.0117(13) 0.5536(14) 0.055(7) Uani 0.50 1 d PU . .
O37 O 0.3671(18) 0.5639(14) 0.7102(15) 0.060(7) Uani 0.50 1 d PU . .
N1 N 0.4194(7) 0.5753(5) 0.1255(6) 0.020(2) Uani 1 1 d . . .
N2 N 0.2952(7) 0.5725(6) 0.1318(6) 0.026(3) Uani 1 1 d . . .
N3 N 0.2983(7) 0.4833(6) 0.0466(7) 0.028(3) Uani 1 1 d . . .
N4 N 0.4216(7) 0.4939(7) 0.0305(6) 0.029(3) Uani 1 1 d . . .
N5 N 0.1829(8) 0.5258(7) 0.1731(7) 0.037(3) Uani 1 1 d . . .
N6 N 0.1123(7) 0.4615(7) 0.2410(7) 0.031(3) Uani 1 1 d . . .
N7 N 0.0981(8) 0.3817(8) 0.1444(7) 0.037(3) Uani 1 1 d . . .
N8 N 0.1798(8) 0.4395(7) 0.0843(7) 0.033(3) Uani 1 1 d . . .
N9 N 0.0946(7) 0.3760(8) 0.3293(7) 0.037(3) Uani 1 1 d . . .
N10 N 0.1410(7) 0.3015(6) 0.4026(6) 0.026(3) Uani 1 1 d . . .
N11 N 0.1348(7) 0.2203(6) 0.3078(7) 0.029(3) Uani 1 1 d . . .
N12 N 0.0917(8) 0.2973(7) 0.2330(8) 0.032(3) Uani 1 1 d . . .
N13 N 0.2269(7) 0.2321(6) 0.4667(6) 0.025(3) Uani 1 1 d . . .
N14 N 0.3398(7) 0.1988(6) 0.4944(7) 0.028(3) Uani 1 1 d . . .
N15 N 0.3354(7) 0.1168(6) 0.4044(6) 0.027(3) Uani 1 1 d . . .
N16 N 0.2255(6) 0.1555(6) 0.3696(7) 0.026(3) Uani 1 1 d . . .
N17 N 0.4771(7) 0.2045(7) 0.4872(7) 0.030(3) Uani 1 1 d . . .
N18 N 0.5792(7) 0.2480(6) 0.4437(7) 0.027(3) Uani 1 1 d . . .
N19 N 0.5727(8) 0.1677(6) 0.3469(6) 0.029(3) Uani 1 1 d . . .
N20 N 0.4725(7) 0.1222(6) 0.3931(6) 0.029(3) Uani 1 1 d . . .
N21 N 0.6534(7) 0.3229(6) 0.3758(7) 0.029(3) Uani 1 1 d . . .
N22 N 0.6708(7) 0.4012(7) 0.2976(6) 0.029(3) Uani 1 1 d . . .
N23 N 0.6750(7) 0.3237(6) 0.2006(6) 0.029(3) Uani 1 1 d . . .
N24 N 0.6399(7) 0.2458(6) 0.2753(8) 0.030(3) Uani 1 1 d . . .
N25 N 0.6338(7) 0.4875(7) 0.2159(7) 0.034(3) Uani 1 1 d . . .
N26 N 0.5478(8) 0.5437(6) 0.1574(6) 0.031(3) Uani 1 1 d . . .
N27 N 0.5511(7) 0.4662(7) 0.0612(6) 0.030(3) Uani 1 1 d . . .
N28 N 0.6387(7) 0.4091(6) 0.1181(7) 0.027(3) Uani 1 1 d . . .
C1 C 0.3299(8) 0.7587(7) 0.1831(8) 0.026(3) Uani 1 1 d . . .
H1 H 0.3090 0.7554 0.1385 0.031 Uiso 1 1 calc R . .
C2 C 0.3363(9) 0.9338(10) 0.3807(9) 0.042(4) Uani 1 1 d . . .
H2 H 0.3091 0.9725 0.3793 0.051 Uiso 1 1 calc R . .
C3 C 0.3601(8) 0.5859(7) 0.1689(7) 0.0211(16) Uani 1 1 d . . .
C4 C 0.3983(8) 0.5605(6) 0.0532(7) 0.021(3) Uani 1 1 d . . .
H4 H 0.4120 0.5949 0.0202 0.025 Uiso 1 1 calc R . .
C5 C 0.3115(9) 0.5495(8) 0.0587(7) 0.030(3) Uani 1 1 d . . .
H5A H 0.2846 0.5763 0.0242 0.036 Uiso 1 1 calc R . .
C6 C 0.3684(10) 0.4501(8) 0.0291(8) 0.032(4) Uani 1 1 d . . .
C7 C 0.2257(9) 0.5833(9) 0.1577(9) 0.035(4) Uani 1 1 d . . .
H7A H 0.1976 0.6094 0.1243 0.043 Uiso 1 1 calc R . .
H7B H 0.2309 0.6087 0.2002 0.043 Uiso 1 1 calc R . .
C8 C 0.2276(9) 0.4563(9) 0.0281(9) 0.038(4) Uani 1 1 d . . .
H8A H 0.2362 0.4173 0.0005 0.046 Uiso 1 1 calc R . .
H8B H 0.2013 0.4873 -0.0016 0.046 Uiso 1 1 calc R . .
C9 C 0.1638(8) 0.5075(8) 0.2417(7) 0.026(3) Uani 1 1 d . . .
C10 C 0.1367(9) 0.4882(7) 0.1255(7) 0.027(3) Uani 1 1 d . . .
H10 H 0.1074 0.5168 0.0946 0.032 Uiso 1 1 calc R . .
C11 C 0.0855(8) 0.4465(8) 0.1699(7) 0.026(3) Uani 1 1 d . . .
H11 H 0.0329 0.4593 0.1635 0.031 Uiso 1 1 calc R . .
C12 C 0.1542(9) 0.3771(10) 0.0936(8) 0.036(4) Uani 1 1 d . . .
C13 C 0.0726(10) 0.4413(8) 0.3052(9) 0.037(4) Uani 1 1 d . . .
H13A H 0.0832 0.4726 0.3420 0.044 Uiso 1 1 calc R . .
H13B H 0.0190 0.4418 0.2961 0.044 Uiso 1 1 calc R . .
C14 C 0.0619(9) 0.3223(8) 0.1698(8) 0.032(3) Uani 1 1 d . . .
H14A H 0.0090 0.3312 0.1762 0.038 Uiso 1 1 calc R . .
H14B H 0.0659 0.2889 0.1341 0.038 Uiso 1 1 calc R . .
C15 C 0.1343(9) 0.3675(9) 0.3909(8) 0.034(4) Uani 1 1 d . . .
C16 C 0.0620(8) 0.3179(8) 0.3019(8) 0.032(4) Uani 1 1 d . . .
H16 H 0.0070 0.3191 0.3024 0.038 Uiso 1 1 calc R . .
C17 C 0.0957(8) 0.2643(8) 0.3540(9) 0.031(4) Uani 1 1 d . . .
H17 H 0.0554 0.2415 0.3784 0.037 Uiso 1 1 calc R . .
C18 C 0.1274(8) 0.2384(8) 0.2360(8) 0.031(3) Uani 1 1 d . . .
C19 C 0.1608(9) 0.2748(8) 0.4662(8) 0.029(3) Uani 1 1 d . . .
H19A H 0.1184 0.2500 0.4832 0.034 Uiso 1 1 calc R . .
H19B H 0.1698 0.3102 0.4989 0.034 Uiso 1 1 calc R . .
C20 C 0.1577(11) 0.1553(8) 0.3286(9) 0.036(4) Uani 1 1 d . . .
H20A H 0.1179 0.1354 0.3555 0.043 Uiso 1 1 calc R . .
H20B H 0.1651 0.1290 0.2871 0.043 Uiso 1 1 calc R . .
C21 C 0.2941(9) 0.2538(7) 0.4952(8) 0.027(3) Uani 1 1 d . . .
C22 C 0.2262(9) 0.1648(7) 0.4471(8) 0.029(3) Uani 1 1 d . . .
H22 H 0.1862 0.1403 0.4701 0.035 Uiso 1 1 calc R . .
C23 C 0.3049(8) 0.1408(7) 0.4684(7) 0.024(3) Uani 1 1 d . . .
H23 H 0.3027 0.1067 0.5043 0.028 Uiso 1 1 calc R . .
C24 C 0.2862(9) 0.1241(8) 0.3479(8) 0.030(3) Uani 1 1 d . . .
C25 C 0.4107(9) 0.2014(8) 0.5311(8) 0.032(3) Uani 1 1 d . . .
H25A H 0.4148 0.1632 0.5607 0.038 Uiso 1 1 calc R . .
H25B H 0.4107 0.2394 0.5614 0.038 Uiso 1 1 calc R . .
C26 C 0.4058(8) 0.0806(7) 0.4007(9) 0.029(3) Uani 1 1 d . . .
H26A H 0.4031 0.0509 0.3613 0.035 Uiso 1 1 calc R . .
H26B H 0.4115 0.0546 0.4427 0.035 Uiso 1 1 calc R . .
C27 C 0.5161(9) 0.2607(7) 0.4834(7) 0.029(3) Uani 1 1 d . . .
C28 C 0.5124(9) 0.1501(7) 0.4564(8) 0.029(3) Uani 1 1 d . . .
H28 H 0.5256 0.1165 0.4908 0.035 Uiso 1 1 calc R . .
C29 C 0.5821(8) 0.1789(8) 0.4206(8) 0.028(3) Uani 1 1 d . . .
H29 H 0.6279 0.1578 0.4380 0.034 Uiso 1 1 calc R . .
C30 C 0.5107(9) 0.1325(7) 0.3334(9) 0.030(3) Uani 1 1 d . . .
C31 C 0.6411(9) 0.2905(8) 0.4417(9) 0.032(4) Uani 1 1 d . . .
H31A H 0.6859 0.2659 0.4537 0.038 Uiso 1 1 calc R . .
H31B H 0.6347 0.3236 0.4774 0.038 Uiso 1 1 calc R . .
C32 C 0.6294(9) 0.1801(8) 0.2975(9) 0.029(3) Uani 1 1 d . . .
H32A H 0.6187 0.1539 0.2563 0.035 Uiso 1 1 calc R . .
H32B H 0.6766 0.1647 0.3170 0.035 Uiso 1 1 calc R . .
C33 C 0.6435(9) 0.3883(7) 0.3627(8) 0.029(3) Uani 1 1 d . . .
C34 C 0.6882(8) 0.2914(8) 0.3159(8) 0.026(3) Uani 1 1 d . . .
H34 H 0.7346 0.2695 0.3306 0.031 Uiso 1 1 calc R . .
C35 C 0.7057(9) 0.3464(8) 0.2663(8) 0.029(3) Uani 1 1 d . . .
H35 H 0.7600 0.3530 0.2630 0.035 Uiso 1 1 calc R . .
C36 C 0.6419(8) 0.2624(8) 0.2064(7) 0.030(3) Uani 1 1 d . . .
C37 C 0.6810(9) 0.4690(7) 0.2723(8) 0.028(3) Uani 1 1 d . . .
H37A H 0.6725 0.4986 0.3109 0.033 Uiso 1 1 calc R . .
H37B H 0.7328 0.4743 0.2580 0.033 Uiso 1 1 calc R . .
C38 C 0.6866(8) 0.3570(9) 0.1346(8) 0.035(4) Uani 1 1 d . . .
H38A H 0.7378 0.3732 0.1343 0.042 Uiso 1 1 calc R . .
H38B H 0.6823 0.3249 0.0975 0.042 Uiso 1 1 calc R . .
C39 C 0.5743(8) 0.5268(7) 0.2232(8) 0.027(3) Uani 1 1 d . . .
C40 C 0.6483(10) 0.4776(8) 0.1417(9) 0.032(4) Uani 1 1 d . . .
H40 H 0.6989 0.4929 0.1305 0.039 Uiso 1 1 calc R . .
C41 C 0.5930(9) 0.5144(9) 0.1016(8) 0.036(4) Uani 1 1 d . . .
H41 H 0.6162 0.5475 0.0718 0.043 Uiso 1 1 calc R . .
C42 C 0.5831(8) 0.4042(8) 0.0699(7) 0.031(4) Uani 1 1 d . . .
C43 C 0.4955(8) 0.5965(8) 0.1442(8) 0.028(3) Uani 1 1 d . . .
H43A H 0.5147 0.6233 0.1066 0.034 Uiso 1 1 calc R . .
H43B H 0.4930 0.6236 0.1857 0.034 Uiso 1 1 calc R . .
C44 C 0.4975(9) 0.4807(11) 0.0076(10) 0.049(5) Uani 1 1 d . . .
H44A H 0.4958 0.4442 -0.0247 0.059 Uiso 1 1 calc R . .
H44B H 0.5152 0.5184 -0.0181 0.059 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 1.783(10) . ?
U1 O1 1.792(11) . ?
U1 O6 2.321(11) . ?
U1 O5 2.322(10) . ?
U1 O8 2.364(13) . ?
U1 O7 2.433(11) . ?
U1 O14 2.475(9) . ?
U1 U2 3.8289(7) . ?
U2 O3 1.790(12) . ?
U2 O4 1.827(12) . ?
U2 O5 2.304(10) . ?
U2 O6 2.342(11) . ?
U2 O12 2.401(11) . ?
U2 O11 2.446(12) . ?
U2 O10 2.513(15) . ?
O5 H5 0.9300 . ?
O6 H6 0.9300 . ?
O7 O28 2.619(16) . ?
O7 O26 2.712(16) . ?
O8 C1 1.27(2) . ?
O9 C1 1.43(2) . ?
O10 O27 2.729(19) 2_565 ?
O11 O31 2.715(18) . ?
O11 O30 2.74(2) . ?
O11 O36 2.97(3) . ?
O12 C2 1.29(2) . ?
O13 C2 1.39(2) . ?
O14 C3 1.165(17) . ?
O15 C6 1.185(19) . ?
O16 C9 1.265(18) . ?
O17 C12 1.18(2) . ?
O18 C15 1.205(19) . ?
O19 C18 1.20(2) . ?
O20 C21 1.243(19) . ?
O21 C24 1.218(19) . ?
O22 C27 1.198(18) . ?
O23 C30 1.227(18) . ?
O24 C33 1.208(19) . ?
O25 C36 1.191(19) . ?
O26 C39 1.213(18) . ?
O27 C42 1.225(19) . ?
N1 C3 1.37(2) . ?
N1 C4 1.461(17) . ?
N1 C43 1.464(19) . ?
N2 C7 1.36(2) . ?
N2 C3 1.379(18) . ?
N2 C5 1.506(18) . ?
N3 C5 1.397(19) . ?
N3 C8 1.42(2) . ?
N3 C6 1.465(19) . ?
N4 C6 1.31(2) . ?
N4 C44 1.45(2) . ?
N4 C4 1.493(18) . ?
N5 C9 1.41(2) . ?
N5 C7 1.44(2) . ?
N5 C10 1.444(19) . ?
N6 C9 1.32(2) . ?
N6 C11 1.470(18) . ?
N6 C13 1.48(2) . ?
N7 C12 1.40(2) . ?
N7 C11 1.43(2) . ?
N7 C14 1.46(2) . ?
N8 C12 1.37(2) . ?
N8 C8 1.42(2) . ?
N8 C10 1.49(2) . ?
N9 C15 1.38(2) . ?
N9 C16 1.42(2) . ?
N9 C13 1.47(2) . ?
N10 C19 1.38(2) . ?
N10 C15 1.38(2) . ?
N10 C17 1.443(19) . ?
N11 C18 1.43(2) . ?
N11 C20 1.45(2) . ?
N11 C17 1.447(19) . ?
N12 C18 1.36(2) . ?
N12 C14 1.41(2) . ?
N12 C16 1.49(2) . ?
N13 C21 1.38(2) . ?
N13 C22 1.430(19) . ?
N13 C19 1.47(2) . ?
N14 C21 1.391(19) . ?
N14 C23 1.429(19) . ?
N14 C25 1.44(2) . ?
N15 C24 1.39(2) . ?
N15 C23 1.432(18) . ?
N15 C26 1.459(18) . ?
N16 C24 1.33(2) . ?
N16 C20 1.43(2) . ?
N16 C22 1.495(19) . ?
N17 C27 1.35(2) . ?
N17 C28 1.41(2) . ?
N17 C25 1.46(2) . ?
N18 C27 1.39(2) . ?
N18 C31 1.41(2) . ?
N18 C29 1.485(19) . ?
N19 C30 1.34(2) . ?
N19 C32 1.41(2) . ?
N19 C29 1.436(18) . ?
N20 C30 1.35(2) . ?
N20 C26 1.471(19) . ?
N20 C28 1.509(18) . ?
N21 C33 1.374(19) . ?
N21 C31 1.44(2) . ?
N21 C34 1.459(19) . ?
N22 C33 1.37(2) . ?
N22 C35 1.42(2) . ?
N22 C37 1.483(19) . ?
N23 C36 1.39(2) . ?
N23 C35 1.442(17) . ?
N23 C38 1.45(2) . ?
N24 C36 1.36(2) . ?
N24 C32 1.42(2) . ?
N24 C34 1.485(19) . ?
N25 C39 1.34(2) . ?
N25 C37 1.413(19) . ?
N25 C40 1.46(2) . ?
N26 C39 1.385(19) . ?
N26 C43 1.449(19) . ?
N26 C41 1.472(19) . ?
N27 C42 1.40(2) . ?
N27 C44 1.42(2) . ?
N27 C41 1.457(19) . ?
N28 C42 1.351(19) . ?
N28 C38 1.40(2) . ?
N28 C40 1.484(19) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C4 C5 1.57(2) . ?
C4 H4 0.9800 . ?
C5 H5A 0.9800 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C10 C11 1.52(2) . ?
C10 H10 0.9800 . ?
C11 H11 0.9800 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C16 C17 1.60(2) . ?
C16 H16 0.9800 . ?
C17 H17 0.9800 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C22 C23 1.54(2) . ?
C22 H22 0.9800 . ?
C23 H23 0.9800 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C28 C29 1.54(2) . ?
C28 H28 0.9800 . ?
C29 H29 0.9800 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C34 C35 1.51(2) . ?
C34 H34 0.9800 . ?
C35 H35 0.9800 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C40 C41 1.45(3) . ?
C40 H40 0.9800 . ?
C41 H41 0.9800 . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U1 O1 179.2(6) . . ?
O2 U1 O6 89.3(5) . . ?
O1 U1 O6 91.4(5) . . ?
O2 U1 O5 90.1(5) . . ?
O1 U1 O5 90.3(5) . . ?
O6 U1 O5 68.0(4) . . ?
O2 U1 O8 87.0(5) . . ?
O1 U1 O8 92.5(5) . . ?
O6 U1 O8 145.0(4) . . ?
O5 U1 O8 77.2(4) . . ?
O2 U1 O7 86.3(5) . . ?
O1 U1 O7 93.7(5) . . ?
O6 U1 O7 76.2(4) . . ?
O5 U1 O7 144.1(4) . . ?
O8 U1 O7 138.1(4) . . ?
O2 U1 O14 92.1(5) . . ?
O1 U1 O14 87.2(4) . . ?
O6 U1 O14 145.4(3) . . ?
O5 U1 O14 146.6(3) . . ?
O8 U1 O14 69.6(4) . . ?
O7 U1 O14 69.4(3) . . ?
O3 U2 O4 175.4(6) . . ?
O3 U2 O5 93.0(5) . . ?
O4 U2 O5 91.3(5) . . ?
O3 U2 O6 92.8(5) . . ?
O4 U2 O6 90.3(5) . . ?
O5 U2 O6 67.9(4) . . ?
O3 U2 O12 89.2(5) . . ?
O4 U2 O12 90.2(5) . . ?
O5 U2 O12 76.7(4) . . ?
O6 U2 O12 144.7(4) . . ?
O3 U2 O11 89.1(5) . . ?
O4 U2 O11 86.3(5) . . ?
O5 U2 O11 148.3(4) . . ?
O6 U2 O11 143.6(4) . . ?
O12 U2 O11 71.7(4) . . ?
O3 U2 O10 88.5(6) . . ?
O4 U2 O10 89.3(6) . . ?
O5 U2 O10 139.5(4) . . ?
O6 U2 O10 71.6(4) . . ?
O12 U2 O10 143.7(4) . . ?
O11 U2 O10 72.1(4) . . ?
U2 O5 U1 111.7(4) . . ?
U2 O5 H5 124.1 . . ?
U1 O5 H5 124.1 . . ?
U1 O6 U2 110.4(4) . . ?
U1 O6 H6 124.8 . . ?
U2 O6 H6 124.8 . . ?
C1 O8 U1 125.9(10) . . ?
C2 O12 U2 131.4(10) . . ?
C3 O14 U1 143.1(9) . . ?
C39 O26 O7 148.8(10) . . ?
C3 N1 C4 114.6(12) . . ?
C3 N1 C43 121.5(12) . . ?
C4 N1 C43 121.4(12) . . ?
C7 N2 C3 122.9(12) . . ?
C7 N2 C5 125.3(12) . . ?
C3 N2 C5 111.8(12) . . ?
C5 N3 C8 124.7(13) . . ?
C5 N3 C6 110.3(13) . . ?
C8 N3 C6 121.2(13) . . ?
C6 N4 C44 122.9(15) . . ?
C6 N4 C4 115.5(12) . . ?
C44 N4 C4 121.4(14) . . ?
C9 N5 C7 122.8(13) . . ?
C9 N5 C10 107.7(14) . . ?
C7 N5 C10 127.6(13) . . ?
C9 N6 C11 112.2(12) . . ?
C9 N6 C13 122.1(13) . . ?
C11 N6 C13 123.7(12) . . ?
C12 N7 C11 114.4(14) . . ?
C12 N7 C14 119.5(15) . . ?
C11 N7 C14 125.9(13) . . ?
C12 N8 C8 121.8(15) . . ?
C12 N8 C10 112.5(13) . . ?
C8 N8 C10 123.7(14) . . ?
C15 N9 C16 114.4(15) . . ?
C15 N9 C13 121.1(15) . . ?
C16 N9 C13 122.7(14) . . ?
C19 N10 C15 123.8(13) . . ?
C19 N10 C17 119.8(14) . . ?
C15 N10 C17 111.6(13) . . ?
C18 N11 C20 121.8(13) . . ?
C18 N11 C17 112.6(13) . . ?
C20 N11 C17 122.9(14) . . ?
C18 N12 C14 121.9(14) . . ?
C18 N12 C16 112.5(14) . . ?
C14 N12 C16 121.5(14) . . ?
C21 N13 C22 114.8(12) . . ?
C21 N13 C19 120.2(12) . . ?
C22 N13 C19 124.6(12) . . ?
C21 N14 C23 115.1(13) . . ?
C21 N14 C25 118.4(13) . . ?
C23 N14 C25 125.2(12) . . ?
C24 N15 C23 112.6(12) . . ?
C24 N15 C26 123.5(12) . . ?
C23 N15 C26 123.4(12) . . ?
C24 N16 C20 120.8(14) . . ?
C24 N16 C22 111.9(13) . . ?
C20 N16 C22 122.8(13) . . ?
C27 N17 C28 114.9(13) . . ?
C27 N17 C25 119.3(13) . . ?
C28 N17 C25 125.0(13) . . ?
C27 N18 C31 122.7(13) . . ?
C27 N18 C29 111.8(12) . . ?
C31 N18 C29 123.6(12) . . ?
C30 N19 C32 124.1(13) . . ?
C30 N19 C29 111.2(13) . . ?
C32 N19 C29 123.4(13) . . ?
C30 N20 C26 126.0(13) . . ?
C30 N20 C28 112.4(13) . . ?
C26 N20 C28 121.0(13) . . ?
C33 N21 C31 125.9(13) . . ?
C33 N21 C34 110.1(13) . . ?
C31 N21 C34 123.5(13) . . ?
C33 N22 C35 113.1(13) . . ?
C33 N22 C37 121.7(12) . . ?
C35 N22 C37 123.1(13) . . ?
C36 N23 C35 112.2(12) . . ?
C36 N23 C38 123.9(12) . . ?
C35 N23 C38 123.4(13) . . ?
C36 N24 C32 122.0(14) . . ?
C36 N24 C34 109.2(12) . . ?
C32 N24 C34 121.1(13) . . ?
C39 N25 C37 123.2(14) . . ?
C39 N25 C40 109.5(13) . . ?
C37 N25 C40 126.5(14) . . ?
C39 N26 C43 123.9(12) . . ?
C39 N26 C41 111.9(13) . . ?
C43 N26 C41 122.3(13) . . ?
C42 N27 C44 122.9(13) . . ?
C42 N27 C41 110.3(12) . . ?
C44 N27 C41 125.1(15) . . ?
C42 N28 C38 122.6(13) . . ?
C42 N28 C40 111.0(14) . . ?
C38 N28 C40 125.8(13) . . ?
O8 C1 O9 123.6(15) . . ?
O8 C1 H1 118.2 . . ?
O9 C1 H1 118.2 . . ?
O12 C2 O13 123.9(15) . . ?
O12 C2 H2 118.0 . . ?
O13 C2 H2 118.0 . . ?
O14 C3 N2 125.3(13) . . ?
O14 C3 N1 125.6(13) . . ?
N2 C3 N1 107.7(12) . . ?
N1 C4 N4 113.4(11) . . ?
N1 C4 C5 102.1(11) . . ?
N4 C4 C5 99.6(11) . . ?
N1 C4 H4 113.5 . . ?
N4 C4 H4 113.5 . . ?
C5 C4 H4 113.5 . . ?
N3 C5 N2 115.0(13) . . ?
N3 C5 C4 107.1(13) . . ?
N2 C5 C4 102.6(10) . . ?
N3 C5 H5A 110.6 . . ?
N2 C5 H5A 110.6 . . ?
C4 C5 H5A 110.6 . . ?
O15 C6 N4 128.1(15) . . ?
O15 C6 N3 124.7(16) . . ?
N4 C6 N3 107.2(13) . . ?
N2 C7 N5 115.5(15) . . ?
N2 C7 H7A 108.4 . . ?
N5 C7 H7A 108.4 . . ?
N2 C7 H7B 108.4 . . ?
N5 C7 H7B 108.4 . . ?
H7A C7 H7B 107.5 . . ?
N3 C8 N8 116.4(15) . . ?
N3 C8 H8A 108.2 . . ?
N8 C8 H8A 108.2 . . ?
N3 C8 H8B 108.2 . . ?
N8 C8 H8B 108.2 . . ?
H8A C8 H8B 107.3 . . ?
O16 C9 N6 126.9(14) . . ?
O16 C9 N5 122.0(15) . . ?
N6 C9 N5 110.9(13) . . ?
N5 C10 N8 113.4(13) . . ?
N5 C10 C11 106.8(12) . . ?
N8 C10 C11 103.6(11) . . ?
N5 C10 H10 110.9 . . ?
N8 C10 H10 110.9 . . ?
C11 C10 H10 110.9 . . ?
N7 C11 N6 117.3(13) . . ?
N7 C11 C10 103.6(11) . . ?
N6 C11 C10 102.1(11) . . ?
N7 C11 H11 111.0 . . ?
N6 C11 H11 111.0 . . ?
C10 C11 H11 111.0 . . ?
O17 C12 N8 129.0(17) . . ?
O17 C12 N7 125.5(17) . . ?
N8 C12 N7 105.5(16) . . ?
N9 C13 N6 112.8(13) . . ?
N9 C13 H13A 109.0 . . ?
N6 C13 H13A 109.0 . . ?
N9 C13 H13B 109.0 . . ?
N6 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
N12 C14 N7 115.1(13) . . ?
N12 C14 H14A 108.5 . . ?
N7 C14 H14A 108.5 . . ?
N12 C14 H14B 108.5 . . ?
N7 C14 H14B 108.5 . . ?
H14A C14 H14B 107.5 . . ?
O18 C15 N10 127.3(16) . . ?
O18 C15 N9 124.9(17) . . ?
N10 C15 N9 107.8(14) . . ?
N9 C16 N12 114.6(13) . . ?
N9 C16 C17 101.4(12) . . ?
N12 C16 C17 102.9(12) . . ?
N9 C16 H16 112.4 . . ?
N12 C16 H16 112.4 . . ?
C17 C16 H16 112.4 . . ?
N10 C17 N11 117.0(12) . . ?
N10 C17 C16 104.1(12) . . ?
N11 C17 C16 103.2(13) . . ?
N10 C17 H17 110.7 . . ?
N11 C17 H17 110.7 . . ?
C16 C17 H17 110.7 . . ?
O19 C18 N12 124.8(15) . . ?
O19 C18 N11 127.1(15) . . ?
N12 C18 N11 108.1(14) . . ?
N10 C19 N13 116.2(12) . . ?
N10 C19 H19A 108.2 . . ?
N13 C19 H19A 108.2 . . ?
N10 C19 H19B 108.2 . . ?
N13 C19 H19B 108.2 . . ?
H19A C19 H19B 107.4 . . ?
N16 C20 N11 112.4(13) . . ?
N16 C20 H20A 109.1 . . ?
N11 C20 H20A 109.1 . . ?
N16 C20 H20B 109.1 . . ?
N11 C20 H20B 109.1 . . ?
H20A C20 H20B 107.8 . . ?
O20 C21 N13 129.7(14) . . ?
O20 C21 N14 126.4(15) . . ?
N13 C21 N14 103.9(13) . . ?
N13 C22 N16 112.6(12) . . ?
N13 C22 C23 103.5(12) . . ?
N16 C22 C23 102.8(11) . . ?
N13 C22 H22 112.4 . . ?
N16 C22 H22 112.4 . . ?
C23 C22 H22 112.4 . . ?
N14 C23 N15 114.6(12) . . ?
N14 C23 C22 102.6(12) . . ?
N15 C23 C22 103.6(11) . . ?
N14 C23 H23 111.8 . . ?
N15 C23 H23 111.8 . . ?
C22 C23 H23 111.8 . . ?
O21 C24 N16 127.2(16) . . ?
O21 C24 N15 124.0(15) . . ?
N16 C24 N15 108.6(13) . . ?
N14 C25 N17 115.7(12) . . ?
N14 C25 H25A 108.4 . . ?
N17 C25 H25A 108.4 . . ?
N14 C25 H25B 108.4 . . ?
N17 C25 H25B 108.4 . . ?
H25A C25 H25B 107.4 . . ?
N15 C26 N20 113.9(12) . . ?
N15 C26 H26A 108.8 . . ?
N20 C26 H26A 108.8 . . ?
N15 C26 H26B 108.8 . . ?
N20 C26 H26B 108.8 . . ?
H26A C26 H26B 107.7 . . ?
O22 C27 N17 126.7(15) . . ?
O22 C27 N18 126.4(15) . . ?
N17 C27 N18 106.9(13) . . ?
N17 C28 N20 115.2(12) . . ?
N17 C28 C29 104.3(12) . . ?
N20 C28 C29 99.4(12) . . ?
N17 C28 H28 112.3 . . ?
N20 C28 H28 112.3 . . ?
C29 C28 H28 112.3 . . ?
N19 C29 N18 116.2(13) . . ?
N19 C29 C28 106.8(12) . . ?
N18 C29 C28 101.7(11) . . ?
N19 C29 H29 110.6 . . ?
N18 C29 H29 110.6 . . ?
C28 C29 H29 110.6 . . ?
O23 C30 N19 128.7(15) . . ?
O23 C30 N20 121.2(14) . . ?
N19 C30 N20 110.0(13) . . ?
N18 C31 N21 115.8(14) . . ?
N18 C31 H31A 108.3 . . ?
N21 C31 H31A 108.3 . . ?
N18 C31 H31B 108.3 . . ?
N21 C31 H31B 108.3 . . ?
H31A C31 H31B 107.4 . . ?
N19 C32 N24 117.9(13) . . ?
N19 C32 H32A 107.8 . . ?
N24 C32 H32A 107.8 . . ?
N19 C32 H32B 107.8 . . ?
N24 C32 H32B 107.8 . . ?
H32A C32 H32B 107.2 . . ?
O24 C33 N22 128.4(14) . . ?
O24 C33 N21 123.6(15) . . ?
N22 C33 N21 108.0(13) . . ?
N21 C34 N24 116.2(12) . . ?
N21 C34 C35 104.9(13) . . ?
N24 C34 C35 105.3(12) . . ?
N21 C34 H34 110.1 . . ?
N24 C34 H34 110.1 . . ?
C35 C34 H34 110.1 . . ?
N22 C35 N23 117.4(13) . . ?
N22 C35 C34 103.3(13) . . ?
N23 C35 C34 103.2(12) . . ?
N22 C35 H35 110.8 . . ?
N23 C35 H35 110.8 . . ?
C34 C35 H35 110.8 . . ?
O25 C36 N24 126.8(16) . . ?
O25 C36 N23 124.4(14) . . ?
N24 C36 N23 108.6(13) . . ?
N25 C37 N22 115.3(12) . . ?
N25 C37 H37A 108.4 . . ?
N22 C37 H37A 108.4 . . ?
N25 C37 H37B 108.4 . . ?
N22 C37 H37B 108.4 . . ?
H37A C37 H37B 107.5 . . ?
N28 C38 N23 117.4(12) . . ?
N28 C38 H38A 107.9 . . ?
N23 C38 H38A 107.9 . . ?
N28 C38 H38B 107.9 . . ?
N23 C38 H38B 107.9 . . ?
H38A C38 H38B 107.2 . . ?
O26 C39 N25 124.6(15) . . ?
O26 C39 N26 126.8(14) . . ?
N25 C39 N26 108.6(13) . . ?
C41 C40 N25 108.3(13) . . ?
C41 C40 N28 104.8(13) . . ?
N25 C40 N28 113.9(15) . . ?
C41 C40 H40 109.9 . . ?
N25 C40 H40 109.9 . . ?
N28 C40 H40 109.9 . . ?
C40 C41 N27 105.6(14) . . ?
C40 C41 N26 101.7(13) . . ?
N27 C41 N26 112.3(13) . . ?
C40 C41 H41 112.2 . . ?
N27 C41 H41 112.2 . . ?
N26 C41 H41 112.2 . . ?
O27 C42 N28 127.6(17) . . ?
O27 C42 N27 124.4(14) . . ?
N28 C42 N27 108.0(12) . . ?
N26 C43 N1 114.4(13) . . ?
N26 C43 H43A 108.7 . . ?
N1 C43 H43A 108.7 . . ?
N26 C43 H43B 108.7 . . ?
N1 C43 H43B 108.7 . . ?
H43A C43 H43B 107.6 . . ?
N27 C44 N4 116.1(15) . . ?
N27 C44 H44A 108.3 . . ?
N4 C44 H44A 108.3 . . ?
N27 C44 H44B 108.3 . . ?
N4 C44 H44B 108.3 . . ?
H44A C44 H44B 107.4 . . ?

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
O5 H5 O13 0.93 2.07 2.766(17) 130.3 .
O6 H6 O27 0.93 2.37 3.231(16) 153.9 2_565


