# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'M Mazzanti'
_publ_contact_author_email       MARINELLA.MAZZANTI@CEA.FR

_publ_section_title              
;
Pentavalent Uranyl Stabilized by a Dianionic
Bulky Tetradentate Ligand
;
loop_
_publ_author_name
'M Mazzanti'
'Yaroslav Filinchuk'
'Pawel Horeglad'
'Gregory Nocton'
'Jacques Pecaut'

# Attachment 'cifB821398DR2.cif'

data_2
_database_code_depnum_ccdc_archive 'CCDC 711672'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40.50 H62.50 K N3 O4 U'
_chemical_formula_weight         932.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_int_tables_number      14

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                   11.7846(3)
_cell_length_b                   30.2442(5)
_cell_length_c                   13.0298(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.368(2)
_cell_angle_gamma                90.00
_cell_volume                     4536.26(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1878
_exptl_absorpt_coefficient_mu    3.707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'ABSPACK (Oxford Diffraction, 2006)'

_exptl_special_details           
;
ABSPACK does absorption correction and scaling of frames for the decaying
intensity of the synchrotron beam at the same time.
The transmition factors related to absorption exclusively can not
be determined in this precedure.
;

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.69408
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Beamline BM1A, SNBL-ESRF, Grenoble, France'
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_measurement_device_type  'MAR345 Image plate'
_diffrn_measurement_method       \f-scan
_diffrn_detector_area_resol_mean 6.67
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12949
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.73
_diffrn_reflns_theta_max         20.00
_reflns_number_total             3824
_reflns_number_gt                3242
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'MAR345 control software (MAR, 2002)'
_computing_cell_refinement       'CrysAlis (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction, 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXH-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
The highest peaks of residual electron density higher than 0.85 e/A3 are
located in the close vicinity of the uranium atoms.

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^)+(0.0478P)^2^+152.0692P] where P=(Fo^2^+2Fc^2^)/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         3824
_refine_ls_number_parameters     459
_refine_ls_number_restraints     432
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0641
_refine_ls_wR_factor_ref         0.1846
_refine_ls_wR_factor_gt          0.1726
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_restrained_S_all      1.157
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U U 0.69590(7) 0.22944(2) 0.05550(6) 0.0345(3) Uani 1 1 d U . .
K K 0.6254(5) 0.19851(13) 0.3130(4) 0.0509(13) Uani 1 1 d U . .
O1U O 0.7596(10) 0.2345(3) 0.1951(9) 0.034(3) Uani 1 1 d U . .
O2U O 0.6343(11) 0.2237(3) -0.0852(9) 0.035(3) Uani 1 1 d U . .
O1 O 0.7414(12) 0.3012(4) 0.0152(11) 0.049(3) Uani 1 1 d U . .
O2 O 0.5708(10) 0.1763(3) 0.1079(10) 0.037(3) Uani 1 1 d U . .
N1 N 0.9151(14) 0.2336(5) 0.0215(14) 0.044(3) Uani 1 1 d U . .
N2 N 0.7922(13) 0.1486(4) 0.0625(13) 0.038(3) Uani 1 1 d U . .
N3 N 0.5122(15) 0.2736(5) 0.0795(13) 0.044(3) Uani 1 1 d U . .
C1 C 0.923(2) 0.2631(6) -0.0700(18) 0.052(4) Uani 1 1 d U . .
H1A H 0.8605 0.2550 -0.1308 0.063 Uiso 1 1 calc R . .
H1B H 0.9983 0.2578 -0.0901 0.063 Uiso 1 1 calc R . .
C2 C 0.912(2) 0.3129(6) -0.0459(18) 0.054(5) Uani 1 1 d U . .
C3 C 0.996(2) 0.3411(7) -0.0722(16) 0.057(5) Uani 1 1 d U . .
H3 H 1.0576 0.3289 -0.0994 0.068 Uiso 1 1 calc R . .
C4 C 0.991(2) 0.3863(7) -0.0594(17) 0.062(5) Uani 1 1 d U . .
C5 C 0.902(2) 0.4019(7) -0.0170(18) 0.063(5) Uani 1 1 d U . .
H5 H 0.9022 0.4328 -0.0038 0.075 Uiso 1 1 calc R . .
C6 C 0.810(2) 0.3768(6) 0.0095(17) 0.055(4) Uani 1 1 d U . .
C7 C 0.8172(18) 0.3286(6) -0.0048(16) 0.044(4) Uani 1 1 d U . .
C8 C 1.084(2) 0.4182(8) -0.0850(19) 0.073(5) Uani 1 1 d U . .
C9 C 1.024(3) 0.4550(8) -0.157(2) 0.101(9) Uani 1 1 d U . .
H9A H 0.9744 0.4723 -0.1210 0.151 Uiso 1 1 calc R . .
H9B H 0.9767 0.4420 -0.2212 0.151 Uiso 1 1 calc R . .
H9C H 1.0831 0.4744 -0.1763 0.151 Uiso 1 1 calc R . .
C10 C 1.152(2) 0.4393(8) 0.017(2) 0.085(8) Uani 1 1 d U . .
H10A H 1.2106 0.4595 0.0015 0.128 Uiso 1 1 calc R . .
H10B H 1.1895 0.4160 0.0651 0.128 Uiso 1 1 calc R . .
H10C H 1.0979 0.4558 0.0511 0.128 Uiso 1 1 calc R . .
C11 C 1.173(3) 0.3934(8) -0.136(3) 0.111(9) Uani 1 1 d U . .
H11A H 1.1324 0.3785 -0.2006 0.166 Uiso 1 1 calc R . .
H11B H 1.2147 0.3714 -0.0871 0.166 Uiso 1 1 calc R . .
H11C H 1.2289 0.4147 -0.1539 0.166 Uiso 1 1 calc R . .
C12 C 0.710(2) 0.3949(6) 0.0573(18) 0.057(4) Uani 1 1 d U . .
C13 C 0.723(2) 0.3764(7) 0.1682(18) 0.070(7) Uani 1 1 d U . .
H13A H 0.7945 0.3874 0.2129 0.105 Uiso 1 1 calc R . .
H13B H 0.7250 0.3440 0.1657 0.105 Uiso 1 1 calc R . .
H13C H 0.6561 0.3858 0.1970 0.105 Uiso 1 1 calc R . .
C14 C 0.598(2) 0.3861(6) -0.0155(19) 0.063(5) Uani 1 1 d U . .
H14A H 0.5887 0.3541 -0.0269 0.095 Uiso 1 1 calc R . .
H14B H 0.5969 0.4008 -0.0827 0.095 Uiso 1 1 calc R . .
H14C H 0.5346 0.3974 0.0148 0.095 Uiso 1 1 calc R . .
C15 C 0.723(2) 0.4475(6) 0.068(2) 0.077(7) Uani 1 1 d U . .
H15A H 0.6612 0.4594 0.0994 0.115 Uiso 1 1 calc R . .
H15B H 0.7180 0.4605 -0.0017 0.115 Uiso 1 1 calc R . .
H15C H 0.7989 0.4547 0.1130 0.115 Uiso 1 1 calc R . .
C16 C 0.7794(17) 0.1243(6) 0.1591(16) 0.044(4) Uani 1 1 d U . .
H16A H 0.8001 0.1444 0.2201 0.052 Uiso 1 1 calc R . .
H16B H 0.8348 0.0993 0.1709 0.052 Uiso 1 1 calc R . .
C17 C 0.6575(18) 0.1066(5) 0.1534(15) 0.039(4) Uani 1 1 d U . .
C18 C 0.6462(19) 0.0601(6) 0.1764(16) 0.047(5) Uani 1 1 d U . .
H18 H 0.7137 0.0421 0.1936 0.056 Uiso 1 1 calc R . .
C19 C 0.537(2) 0.0415(6) 0.1735(17) 0.049(5) Uani 1 1 d U . .
C20 C 0.4429(19) 0.0694(6) 0.1459(17) 0.051(5) Uani 1 1 d U . .
H20 H 0.3684 0.0569 0.1434 0.061 Uiso 1 1 calc R . .
C21 C 0.4464(19) 0.1144(6) 0.1210(18) 0.050(5) Uani 1 1 d U . .
C22 C 0.5562(17) 0.1326(5) 0.1267(15) 0.036(4) Uani 1 1 d U . .
C23 C 0.527(2) -0.0070(6) 0.202(2) 0.066(5) Uani 1 1 d U . .
C24 C 0.408(3) -0.0245(7) 0.163(2) 0.112(10) Uani 1 1 d U . .
H24A H 0.4067 -0.0561 0.1786 0.168 Uiso 1 1 calc R . .
H24B H 0.3860 -0.0201 0.0864 0.168 Uiso 1 1 calc R . .
H24C H 0.3536 -0.0088 0.1966 0.168 Uiso 1 1 calc R . .
C25 C 0.604(4) -0.0350(8) 0.149(4) 0.178(14) Uani 1 1 d U . .
H25A H 0.6845 -0.0333 0.1882 0.267 Uiso 1 1 calc R . .
H25B H 0.5992 -0.0241 0.0770 0.267 Uiso 1 1 calc R . .
H25C H 0.5776 -0.0658 0.1457 0.267 Uiso 1 1 calc R . .
C26 C 0.563(3) -0.0128(8) 0.318(2) 0.107(10) Uani 1 1 d U . .
H26A H 0.5561 -0.0441 0.3354 0.161 Uiso 1 1 calc R . .
H26B H 0.5117 0.0049 0.3521 0.161 Uiso 1 1 calc R . .
H26C H 0.6431 -0.0031 0.3419 0.161 Uiso 1 1 calc R . .
C27 C 0.339(2) 0.1410(7) 0.084(2) 0.064(5) Uani 1 1 d U . .
C28 C 0.228(2) 0.1136(7) 0.081(3) 0.091(8) Uani 1 1 d U . .
H28A H 0.2304 0.0870 0.0385 0.137 Uiso 1 1 calc R . .
H28B H 0.1598 0.1313 0.0495 0.137 Uiso 1 1 calc R . .
H28C H 0.2235 0.1051 0.1525 0.137 Uiso 1 1 calc R . .
C29 C 0.339(2) 0.1798(6) 0.163(2) 0.071(6) Uani 1 1 d U . .
H29A H 0.3518 0.1681 0.2348 0.107 Uiso 1 1 calc R . .
H29B H 0.2641 0.1951 0.1460 0.107 Uiso 1 1 calc R . .
H29C H 0.4014 0.2006 0.1578 0.107 Uiso 1 1 calc R . .
C30 C 0.333(2) 0.1591(7) -0.025(2) 0.077(7) Uani 1 1 d U . .
H30A H 0.4046 0.1757 -0.0264 0.116 Uiso 1 1 calc R . .
H30B H 0.2661 0.1789 -0.0448 0.116 Uiso 1 1 calc R . .
H30C H 0.3256 0.1346 -0.0754 0.116 Uiso 1 1 calc R . .
C31 C 0.9447(18) 0.1894(6) -0.0054(17) 0.046(4) Uani 1 1 d U . .
H31A H 1.0280 0.1886 -0.0080 0.055 Uiso 1 1 calc R . .
H31B H 0.8992 0.1820 -0.0764 0.055 Uiso 1 1 calc R . .
C32 C 0.9217(17) 0.1548(6) 0.0715(18) 0.050(5) Uani 1 1 d U . .
H32A H 0.9570 0.1264 0.0572 0.060 Uiso 1 1 calc R . .
H32B H 0.9582 0.1640 0.1440 0.060 Uiso 1 1 calc R . .
C33 C 0.9976(19) 0.2499(7) 0.1208(18) 0.058(5) Uani 1 1 d U . .
H33A H 1.0773 0.2500 0.1099 0.087 Uiso 1 1 calc R . .
H33B H 0.9927 0.2303 0.1796 0.087 Uiso 1 1 calc R . .
H33C H 0.9758 0.2800 0.1369 0.087 Uiso 1 1 calc R . .
C34 C 0.7413(17) 0.1245(6) -0.0357(15) 0.039(4) Uani 1 1 d U . .
H34A H 0.7783 0.0954 -0.0348 0.058 Uiso 1 1 calc R . .
H34B H 0.7543 0.1414 -0.0962 0.058 Uiso 1 1 calc R . .
H34C H 0.6577 0.1207 -0.0409 0.058 Uiso 1 1 calc R . .
C41 C 0.503(2) 0.2930(6) 0.1739(17) 0.047(4) Uani 1 1 d U . .
H41 H 0.5686 0.2920 0.2309 0.056 Uiso 1 1 calc R . .
C42 C 0.404(2) 0.3136(7) 0.189(2) 0.067(6) Uani 1 1 d U . .
H42 H 0.4043 0.3292 0.2521 0.080 Uiso 1 1 calc R . .
C43 C 0.303(2) 0.3114(7) 0.109(2) 0.074(6) Uani 1 1 d U . .
H43 H 0.2336 0.3244 0.1197 0.089 Uiso 1 1 calc R . .
C44 C 0.304(2) 0.2910(7) 0.017(2) 0.075(6) Uani 1 1 d U . .
H44 H 0.2364 0.2885 -0.0375 0.089 Uiso 1 1 calc R . .
C45 C 0.4145(19) 0.2731(7) 0.0059(19) 0.056(5) Uani 1 1 d U . .
H45 H 0.4177 0.2597 -0.0595 0.067 Uiso 1 1 calc R . .
C51 C 0.036(4) 0.0054(14) 0.965(3) 0.070(14) Uiso 0.50 1 d PDU . .
H51A H 0.1118 0.0166 1.0055 0.084 Uiso 0.50 1 calc PR . .
H51B H 0.0515 -0.0213 0.9262 0.084 Uiso 0.50 1 calc PR . .
C52 C -0.021(3) 0.0403(14) 0.889(4) 0.076(14) Uiso 0.50 1 d PDU . .
H52A H -0.0444 0.0659 0.9272 0.092 Uiso 0.50 1 calc PR . .
H52B H -0.0917 0.0282 0.8419 0.092 Uiso 0.50 1 calc PR . .
C53 C 0.066(6) 0.054(2) 0.826(5) 0.16(3) Uiso 0.50 1 d PDU . .
H53A H 0.1448 0.0468 0.8646 0.242 Uiso 0.50 1 calc PR . .
H53B H 0.0611 0.0864 0.8142 0.242 Uiso 0.50 1 calc PR . .
H53C H 0.0503 0.0390 0.7580 0.242 Uiso 0.50 1 calc PR . .

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
U 0.0439(6) 0.0217(4) 0.0394(6) 0.0015(3) 0.0123(4) -0.0045(3)
K 0.079(4) 0.034(2) 0.044(3) -0.0023(19) 0.024(3) -0.008(2)
O1U 0.037(7) 0.032(6) 0.033(6) -0.001(4) 0.004(5) -0.007(5)
O2U 0.054(8) 0.020(6) 0.034(5) 0.001(4) 0.020(5) -0.013(5)
O1 0.049(8) 0.027(5) 0.069(9) 0.004(5) 0.009(7) -0.010(5)
O2 0.036(7) 0.025(5) 0.050(7) 0.008(5) 0.010(6) -0.004(4)
N1 0.040(6) 0.033(6) 0.065(9) 0.000(6) 0.022(6) -0.007(5)
N2 0.036(7) 0.029(6) 0.053(9) -0.003(5) 0.015(7) -0.004(5)
N3 0.048(6) 0.035(7) 0.049(9) 0.004(7) 0.012(6) 0.004(6)
C1 0.051(12) 0.037(6) 0.073(11) 0.009(7) 0.020(9) -0.001(7)
C2 0.062(12) 0.036(6) 0.067(13) 0.009(8) 0.019(10) -0.011(7)
C3 0.081(14) 0.052(7) 0.047(13) -0.002(10) 0.038(11) -0.023(9)
C4 0.097(13) 0.051(8) 0.043(13) 0.000(8) 0.029(10) -0.039(9)
C5 0.091(15) 0.036(9) 0.064(14) -0.011(10) 0.024(11) -0.031(8)
C6 0.085(11) 0.034(6) 0.051(12) -0.008(8) 0.027(9) -0.019(7)
C7 0.050(11) 0.029(6) 0.053(12) -0.001(8) 0.007(9) -0.011(6)
C8 0.102(16) 0.069(11) 0.049(13) 0.010(8) 0.020(10) -0.048(9)
C9 0.13(2) 0.087(16) 0.076(18) 0.037(13) 0.005(15) -0.056(13)
C10 0.08(2) 0.091(18) 0.075(15) 0.002(11) 0.001(12) -0.046(13)
C11 0.15(2) 0.074(16) 0.14(2) -0.005(14) 0.09(2) -0.065(13)
C12 0.097(12) 0.028(8) 0.055(11) -0.010(8) 0.033(9) -0.013(9)
C13 0.12(2) 0.044(11) 0.059(11) -0.009(9) 0.043(11) -0.026(13)
C14 0.091(12) 0.019(9) 0.083(14) -0.004(9) 0.027(11) 0.001(9)
C15 0.13(2) 0.029(8) 0.084(18) -0.014(9) 0.042(16) -0.018(10)
C16 0.051(8) 0.027(8) 0.048(9) 0.005(7) 0.000(9) -0.003(7)
C17 0.048(8) 0.026(7) 0.044(12) 0.003(7) 0.014(9) 0.000(6)
C18 0.059(10) 0.025(7) 0.057(13) 0.004(8) 0.014(11) 0.003(6)
C19 0.064(11) 0.025(7) 0.061(12) 0.000(7) 0.019(11) -0.008(5)
C20 0.060(11) 0.032(7) 0.075(15) 0.006(9) 0.044(12) -0.006(6)
C21 0.053(8) 0.027(7) 0.083(13) 0.008(8) 0.042(10) -0.002(5)
C22 0.049(7) 0.022(6) 0.042(10) 0.007(6) 0.022(9) 0.000(5)
C23 0.091(15) 0.031(8) 0.081(12) 0.014(9) 0.031(12) -0.008(7)
C24 0.145(18) 0.026(12) 0.13(2) 0.031(14) -0.042(17) -0.046(12)
C25 0.28(3) 0.029(12) 0.28(3) -0.01(2) 0.18(3) 0.011(19)
C26 0.15(3) 0.053(15) 0.093(13) 0.035(11) -0.021(15) -0.040(16)
C27 0.052(9) 0.043(9) 0.101(14) 0.010(8) 0.027(13) -0.002(7)
C28 0.059(10) 0.049(13) 0.17(3) 0.011(13) 0.039(16) -0.004(9)
C29 0.068(17) 0.038(11) 0.117(16) 0.009(10) 0.043(15) 0.013(9)
C30 0.080(19) 0.048(14) 0.094(13) 0.013(10) 0.000(13) -0.014(12)
C31 0.034(10) 0.035(7) 0.071(13) 0.002(6) 0.017(9) -0.006(7)
C32 0.035(8) 0.039(8) 0.072(14) 0.011(8) 0.007(9) 0.005(7)
C33 0.053(9) 0.046(11) 0.071(12) 0.001(9) 0.002(11) -0.008(10)
C34 0.043(12) 0.034(9) 0.052(10) -0.011(8) 0.040(9) -0.012(8)
C41 0.065(11) 0.033(10) 0.047(10) 0.006(8) 0.023(9) 0.006(9)
C42 0.076(14) 0.049(12) 0.078(14) -0.008(11) 0.023(9) 0.014(11)
C43 0.065(12) 0.043(12) 0.113(17) -0.012(11) 0.017(10) 0.015(11)
C44 0.059(10) 0.056(13) 0.099(15) -0.012(11) -0.004(12) 0.023(11)
C45 0.047(9) 0.052(12) 0.066(12) 0.000(10) 0.005(8) -0.002(9)

_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 O1U 1.819(12) . ?
U O2U 1.830(12) . ?
U O1 2.323(11) . ?
U O2 2.379(11) . ?
U N3 2.618(16) . ?
U N2 2.690(14) . ?
U N1 2.715(16) . ?
U K 3.781(4) 4_565 ?
K O1U 2.663(13) . ?
K O2U 2.691(11) 4_566 ?
K O1 2.695(15) 4_566 ?
K O2 2.697(13) . ?
K C7 3.02(2) 4_566 ?
K C14 3.46(2) 4_566 ?
K C2 3.50(2) 4_566 ?
K U 3.781(4) 4_566 ?
O2U K 2.691(11) 4_565 ?
O1 C7 1.29(2) . ?
O1 K 2.695(15) 4_565 ?
O2 C22 1.359(19) . ?
N1 C31 1.44(2) . ?
N1 C1 1.51(2) . ?
N1 C33 1.53(3) . ?
N2 C34 1.48(2) . ?
N2 C16 1.49(2) . ?
N2 C32 1.52(2) . ?
N3 C45 1.33(2) . ?
N3 C41 1.39(2) . ?
C1 C2 1.55(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.40(3) . ?
C2 C7 1.42(3) . ?
C2 K 3.50(2) 4_565 ?
C3 C4 1.38(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.36(3) . ?
C4 C8 1.55(3) . ?
C5 C6 1.43(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.47(3) . ?
C6 C12 1.55(3) . ?
C7 K 3.02(2) 4_565 ?
C8 C9 1.53(3) . ?
C8 C10 1.54(3) . ?
C8 C11 1.56(4) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C14 1.47(3) . ?
C12 C13 1.53(3) . ?
C12 C15 1.60(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 K 3.46(2) 4_565 ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.52(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C22 1.41(3) . ?
C17 C18 1.45(2) . ?
C18 C19 1.40(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.37(3) . ?
C19 C23 1.52(3) . ?
C20 C21 1.40(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.39(3) . ?
C21 C27 1.49(3) . ?
C23 C24 1.48(3) . ?
C23 C26 1.48(3) . ?
C23 C25 1.52(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C30 1.52(3) . ?
C27 C28 1.54(3) . ?
C27 C29 1.56(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.51(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C41 C42 1.37(3) . ?
C41 H41 0.9500 . ?
C42 C43 1.41(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.35(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.44(3) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C51 C52 1.508(10) . ?
C51 C51 1.42(8) 3_557 ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53 1.512(10) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?

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
O1U U O2U 178.9(6) . . ?
O1U U O1 94.7(5) . . ?
O2U U O1 85.6(5) . . ?
O1U U O2 85.3(5) . . ?
O2U U O2 94.9(4) . . ?
O1 U O2 152.1(4) . . ?
O1U U N3 90.7(5) . . ?
O2U U N3 90.4(5) . . ?
O1 U N3 77.7(5) . . ?
O2 U N3 74.4(4) . . ?
O1U U N2 87.8(5) . . ?
O2U U N2 91.2(5) . . ?
O1 U N2 137.8(5) . . ?
O2 U N2 70.0(4) . . ?
N3 U N2 144.4(5) . . ?
O1U U N1 87.5(5) . . ?
O2U U N1 91.6(5) . . ?
O1 U N1 69.3(5) . . ?
O2 U N1 138.4(4) . . ?
N3 U N1 146.7(4) . . ?
N2 U N1 68.8(4) . . ?
O1U U K 139.1(3) . 4_565 ?
O2U U K 41.3(3) . 4_565 ?
O1 U K 45.0(3) . 4_565 ?
O2 U K 126.2(3) . 4_565 ?
N3 U K 76.5(4) . 4_565 ?
N2 U K 124.6(3) . 4_565 ?
N1 U K 83.3(4) . 4_565 ?
O1U K O2U 87.8(4) . 4_566 ?
O1U K O1 108.9(4) . 4_566 ?
O2U K O1 63.8(4) 4_566 4_566 ?
O1U K O2 64.9(4) . . ?
O2U K O2 133.0(4) 4_566 . ?
O1 K O2 158.9(4) 4_566 . ?
O1U K C7 97.3(5) . 4_566 ?
O2U K C7 84.6(4) 4_566 4_566 ?
O1 K C7 25.2(4) 4_566 4_566 ?
O2 K C7 133.7(5) . 4_566 ?
O1U K C14 145.6(5) . 4_566 ?
O2U K C14 109.1(5) 4_566 4_566 ?
O1 K C14 57.9(5) 4_566 4_566 ?
O2 K C14 114.9(4) . 4_566 ?
C7 K C14 56.5(6) 4_566 4_566 ?
O1U K C2 73.6(5) . 4_566 ?
O2U K C2 84.0(4) 4_566 4_566 ?
O1 K C2 42.0(5) 4_566 4_566 ?
O2 K C2 119.6(5) . 4_566 ?
C7 K C2 23.8(5) 4_566 4_566 ?
C14 K C2 78.5(5) 4_566 4_566 ?
O1U K U 101.3(3) . 4_566 ?
O2U K U 26.6(2) 4_566 4_566 ?
O1 K U 37.5(2) 4_566 4_566 ?
O2 K U 159.2(3) . 4_566 ?
C7 K U 60.4(4) 4_566 4_566 ?
C14 K U 85.4(4) 4_566 4_566 ?
C2 K U 66.6(3) 4_566 4_566 ?
U O1U K 111.9(5) . . ?
U O2U K 112.1(5) . 4_565 ?
C7 O1 U 148.4(13) . . ?
C7 O1 K 91.6(12) . 4_565 ?
U O1 K 97.5(4) . 4_565 ?
C22 O2 U 144.9(11) . . ?
C22 O2 K 94.4(10) . . ?
U O2 K 94.9(4) . . ?
C31 N1 C1 107.2(15) . . ?
C31 N1 C33 111.3(16) . . ?
C1 N1 C33 110.1(15) . . ?
C31 N1 U 106.6(11) . . ?
C1 N1 U 112.2(12) . . ?
C33 N1 U 109.4(12) . . ?
C34 N2 C16 113.0(14) . . ?
C34 N2 C32 110.0(15) . . ?
C16 N2 C32 106.1(15) . . ?
C34 N2 U 109.1(11) . . ?
C16 N2 U 110.9(11) . . ?
C32 N2 U 107.5(10) . . ?
C45 N3 C41 115.1(19) . . ?
C45 N3 U 121.2(14) . . ?
C41 N3 U 123.0(14) . . ?
N1 C1 C2 113.2(17) . . ?
N1 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.8 . . ?
C3 C2 C7 122.6(19) . . ?
C3 C2 C1 117(2) . . ?
C7 C2 C1 120.3(17) . . ?
C3 C2 K 125.6(15) . 4_565 ?
C7 C2 K 58.7(12) . 4_565 ?
C1 C2 K 84.8(12) . 4_565 ?
C4 C3 C2 122(2) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C5 C4 C3 116.7(19) . . ?
C5 C4 C8 120(2) . . ?
C3 C4 C8 123(2) . . ?
C4 C5 C6 126.8(19) . . ?
C4 C5 H5 116.6 . . ?
C6 C5 H5 116.6 . . ?
C5 C6 C7 116(2) . . ?
C5 C6 C12 126.5(18) . . ?
C7 C6 C12 117.9(17) . . ?
O1 C7 C2 120.0(16) . . ?
O1 C7 C6 123.5(19) . . ?
C2 C7 C6 116.5(17) . . ?
O1 C7 K 63.2(10) . 4_565 ?
C2 C7 K 97.5(13) . 4_565 ?
C6 C7 K 108.4(14) . 4_565 ?
C9 C8 C10 108(2) . . ?
C9 C8 C11 110(2) . . ?
C10 C8 C11 107(2) . . ?
C9 C8 C4 110(2) . . ?
C10 C8 C4 109.3(19) . . ?
C11 C8 C4 112(2) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C14 C12 C13 116(2) . . ?
C14 C12 C6 109.4(19) . . ?
C13 C12 C6 109(2) . . ?
C14 C12 C15 107.0(19) . . ?
C13 C12 C15 107.1(17) . . ?
C6 C12 C15 108.5(17) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 K 110.9(13) . 4_565 ?
C12 C14 H14A 109.5 . . ?
K C14 H14A 36.4 4_565 . ?
C12 C14 H14B 109.5 . . ?
K C14 H14B 75.3 4_565 . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
K C14 H14C 134.7 4_565 . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N2 C16 C17 113.4(15) . . ?
N2 C16 H16A 108.9 . . ?
C17 C16 H16A 108.9 . . ?
N2 C16 H16B 108.9 . . ?
C17 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
C22 C17 C18 118.8(18) . . ?
C22 C17 C16 123.9(15) . . ?
C18 C17 C16 117.3(17) . . ?
C19 C18 C17 120.6(18) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C20 C19 C18 116.3(17) . . ?
C20 C19 C23 124(2) . . ?
C18 C19 C23 119.7(19) . . ?
C19 C20 C21 127(2) . . ?
C19 C20 H20 116.7 . . ?
C21 C20 H20 116.7 . . ?
C22 C21 C20 116.3(18) . . ?
C22 C21 C27 121.4(16) . . ?
C20 C21 C27 122.2(18) . . ?
O2 C22 C21 121.7(16) . . ?
O2 C22 C17 116.9(16) . . ?
C21 C22 C17 121.4(16) . . ?
C24 C23 C26 111(2) . . ?
C24 C23 C19 112(2) . . ?
C26 C23 C19 110.2(19) . . ?
C24 C23 C25 105(3) . . ?
C26 C23 C25 110(3) . . ?
C19 C23 C25 110(2) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C21 C27 C30 111(2) . . ?
C21 C27 C28 112.1(17) . . ?
C30 C27 C28 108(2) . . ?
C21 C27 C29 108(2) . . ?
C30 C27 C29 109.9(18) . . ?
C28 C27 C29 108(2) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N1 C31 C32 113.1(18) . . ?
N1 C31 H31A 109.0 . . ?
C32 C31 H31A 109.0 . . ?
N1 C31 H31B 109.0 . . ?
C32 C31 H31B 109.0 . . ?
H31A C31 H31B 107.8 . . ?
N2 C32 C31 110.7(16) . . ?
N2 C32 H32A 109.5 . . ?
C31 C32 H32A 109.5 . . ?
N2 C32 H32B 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 108.1 . . ?
N1 C33 H33A 109.5 . . ?
N1 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N1 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N2 C34 H34A 109.5 . . ?
N2 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N2 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C42 C41 N3 123(2) . . ?
C42 C41 H41 118.4 . . ?
N3 C41 H41 118.4 . . ?
C41 C42 C43 119(2) . . ?
C41 C42 H42 120.5 . . ?
C43 C42 H42 120.5 . . ?
C44 C43 C42 121(2) . . ?
C44 C43 H43 119.6 . . ?
C42 C43 H43 119.6 . . ?
C43 C44 C45 116(2) . . ?
C43 C44 H44 122.0 . . ?
C45 C44 H44 122.0 . . ?
N3 C45 C44 126(2) . . ?
N3 C45 H45 117.2 . . ?
C44 C45 H45 117.2 . . ?
C52 C51 C51 110(4) . 3_557 ?
C52 C51 H51A 109.7 . . ?
C51 C51 H51A 109.7 3_557 . ?
C52 C51 H51B 109.8 . . ?
C51 C51 H51B 109.7 3_557 . ?
H51A C51 H51B 108.2 . . ?
C51 C52 C53 106.8(14) . . ?
C51 C52 H52A 110.4 . . ?
C53 C52 H52A 110.4 . . ?
C51 C52 H52B 110.3 . . ?
C53 C52 H52B 110.4 . . ?
H52A C52 H52B 108.6 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.839
_diffrn_reflns_theta_full        20.00
_diffrn_measured_fraction_theta_full 0.839
_refine_diff_density_max         1.783
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.176

#===END

data_3
_database_code_depnum_ccdc_archive 'CCDC 711673'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40.50 H62.50 N3 O4 U'
_chemical_formula_weight         893.47

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'
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 1 21/c 1'

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                   19.6726(6)
_cell_length_b                   20.0780(6)
_cell_length_c                   11.4096(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.116(3)
_cell_angle_gamma                90.00
_cell_volume                     4422.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6467
_cell_measurement_theta_min      3.0488
_cell_measurement_theta_max      28.9707

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.3757
_exptl_crystal_size_mid          0.0338
_exptl_crystal_size_min          0.0171
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1802
_exptl_absorpt_coefficient_mu    3.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_process_details   'ABSPACK (Oxford Diffraction, 2006)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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  XCalibur-S
_diffrn_measurement_method       omega-scan
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
1 omega -5.00 47.00 1.0000 180.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 17.1550 -77.0000 240.0000 0.0000 0.0000 52

#__ type_ start__ end____ width___ exp.time_
2 omega 3.00 37.00 1.0000 180.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 17.1550 -135.0000 231.0000 0.0000 0.0000 34

#__ type_ start__ end____ width___ exp.time_
3 omega -42.00 7.00 1.0000 180.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -18.7175 45.0000 60.0000 0.0000 0.0000 49

#__ type_ start__ end____ width___ exp.time_
4 omega 3.00 43.00 1.0000 180.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -18.7175 -134.0000 62.0000 0.0000 0.0000 40

#__ type_ start__ end____ width___ exp.time_
5 omega -90.00 3.00 1.0000 180.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -18.7175 -45.0000 90.0000 0.0000 0.0000 93

#__ type_ start__ end____ width___ exp.time_
6 omega 4.00 46.00 1.0000 180.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -18.7175 0.0000 270.0000 0.0000 0.0000 42

;

_diffrn_detector_area_resol_mean 15.9653
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25664
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.1361
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         28.95
_reflns_number_total             9620
_reflns_number_gt                5228
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
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^)+(0.0280P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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         9620
_refine_ls_number_parameters     451
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.0745
_refine_ls_wR_factor_gt          0.0690
_refine_ls_goodness_of_fit_ref   0.808
_refine_ls_restrained_S_all      0.809
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U U 0.358500(12) 0.315957(12) 0.747385(18) 0.03186(7) Uani 1 1 d . . .
O1U O 0.36778(18) 0.3105(2) 0.5970(3) 0.0418(10) Uani 1 1 d . . .
O1 O 0.2490(2) 0.3440(2) 0.6906(3) 0.0425(11) Uani 1 1 d . . .
O2U O 0.34948(18) 0.3190(2) 0.9004(3) 0.0404(9) Uani 1 1 d . . .
O2 O 0.47102(19) 0.33923(19) 0.8024(3) 0.0376(11) Uani 1 1 d . . .
N1 N 0.2783(2) 0.2097(2) 0.7075(4) 0.0329(13) Uani 1 1 d . . .
N2 N 0.4309(2) 0.2046(2) 0.7937(4) 0.0330(13) Uani 1 1 d . . .
N3 N 0.3634(3) 0.4447(2) 0.7337(4) 0.0367(11) Uani 1 1 d . . .
C1 C 0.2337(3) 0.2144(3) 0.5855(5) 0.0384(17) Uani 1 1 d . . .
H1A H 0.2120 0.1715 0.5658 0.046 Uiso 1 1 calc R . .
H1B H 0.2636 0.2229 0.5287 0.046 Uiso 1 1 calc R . .
C2 C 0.1773(3) 0.2671(3) 0.5679(5) 0.0365(16) Uani 1 1 d . . .
C3 C 0.1158(3) 0.2518(4) 0.4914(5) 0.0462(19) Uani 1 1 d . . .
H3 H 0.1099 0.2094 0.4579 0.055 Uiso 1 1 calc R . .
C4 C 0.0625(4) 0.2980(4) 0.4631(6) 0.049(2) Uani 1 1 d . . .
C5 C 0.0722(3) 0.3581(4) 0.5223(6) 0.057(2) Uani 1 1 d . . .
H5 H 0.0364 0.3890 0.5076 0.069 Uiso 1 1 calc R . .
C6 C 0.1320(3) 0.3755(4) 0.6025(6) 0.0515(18) Uani 1 1 d . . .
C7 C 0.1876(3) 0.3301(3) 0.6206(5) 0.0381(16) Uani 1 1 d . . .
C8 C -0.0031(4) 0.2832(4) 0.3703(7) 0.064(2) Uani 1 1 d . . .
C9 C -0.0003(4) 0.3246(7) 0.2603(7) 0.123(4) Uani 1 1 d . . .
H9A H -0.0432 0.3200 0.2041 0.185 Uiso 1 1 calc R . .
H9B H 0.0372 0.3095 0.2245 0.185 Uiso 1 1 calc R . .
H9C H 0.0067 0.3706 0.2827 0.185 Uiso 1 1 calc R . .
C10 C -0.0661(4) 0.3066(6) 0.4124(8) 0.117(4) Uani 1 1 d . . .
H10A H -0.0654 0.3543 0.4178 0.176 Uiso 1 1 calc R . .
H10B H -0.0668 0.2879 0.4895 0.176 Uiso 1 1 calc R . .
H10C H -0.1066 0.2927 0.3568 0.176 Uiso 1 1 calc R . .
C11 C -0.0069(6) 0.2154(6) 0.3280(12) 0.200(8) Uani 1 1 d . . .
H11A H 0.0347 0.2046 0.2997 0.300 Uiso 1 1 calc R . .
H11B H -0.0461 0.2106 0.2640 0.300 Uiso 1 1 calc R . .
H11C H -0.0117 0.1859 0.3921 0.300 Uiso 1 1 calc R . .
C12 C 0.1395(4) 0.4439(4) 0.6651(7) 0.065(2) Uani 1 1 d . . .
C13 C 0.0693(4) 0.4803(5) 0.6452(8) 0.109(3) Uani 1 1 d . . .
H13A H 0.0742 0.5211 0.6899 0.164 Uiso 1 1 calc R . .
H13B H 0.0355 0.4525 0.6716 0.164 Uiso 1 1 calc R . .
H13C H 0.0546 0.4900 0.5618 0.164 Uiso 1 1 calc R . .
C14 C 0.1902(4) 0.4863(4) 0.6146(7) 0.085(3) Uani 1 1 d . . .
H14A H 0.2346 0.4647 0.6278 0.127 Uiso 1 1 calc R . .
H14B H 0.1945 0.5289 0.6534 0.127 Uiso 1 1 calc R . .
H14C H 0.1738 0.4923 0.5304 0.127 Uiso 1 1 calc R . .
C15 C 0.1628(4) 0.4352(4) 0.8001(7) 0.079(3) Uani 1 1 d . . .
H15A H 0.2039 0.4083 0.8160 0.119 Uiso 1 1 calc R . .
H15B H 0.1268 0.4138 0.8321 0.119 Uiso 1 1 calc R . .
H15C H 0.1725 0.4781 0.8368 0.119 Uiso 1 1 calc R . .
C16 C 0.4805(3) 0.2108(3) 0.9111(5) 0.0361(17) Uani 1 1 d . . .
H16A H 0.4978 0.1668 0.9358 0.043 Uiso 1 1 calc R . .
H16B H 0.4550 0.2268 0.9703 0.043 Uiso 1 1 calc R . .
C17 C 0.5417(3) 0.2563(3) 0.9122(5) 0.0338(16) Uani 1 1 d . . .
C18 C 0.6066(3) 0.2356(3) 0.9746(5) 0.0356(16) Uani 1 1 d . . .
H18 H 0.6105 0.1939 1.0109 0.043 Uiso 1 1 calc R . .
C19 C 0.6649(3) 0.2750(3) 0.9840(5) 0.0373(16) Uani 1 1 d . . .
C20 C 0.6564(3) 0.3366(3) 0.9269(5) 0.0375(16) Uani 1 1 d . . .
H20 H 0.6953 0.3635 0.9316 0.045 Uiso 1 1 calc R . .
C21 C 0.5935(3) 0.3609(3) 0.8630(5) 0.0332(15) Uani 1 1 d . . .
C22 C 0.5337(3) 0.3197(4) 0.8593(4) 0.0332(13) Uani 1 1 d . . .
C23 C 0.7346(3) 0.2523(4) 1.0606(5) 0.0410(17) Uani 1 1 d . . .
C24 C 0.7271(4) 0.2487(5) 1.1904(5) 0.081(3) Uani 1 1 d . . .
H24A H 0.7698 0.2335 1.2384 0.122 Uiso 1 1 calc R . .
H24B H 0.6906 0.2182 1.1980 0.122 Uiso 1 1 calc R . .
H24C H 0.7161 0.2921 1.2169 0.122 Uiso 1 1 calc R . .
C25 C 0.7535(3) 0.1849(4) 1.0205(5) 0.0630(18) Uani 1 1 d . . .
H25A H 0.7548 0.1862 0.9369 0.094 Uiso 1 1 calc R . .
H25B H 0.7196 0.1529 1.0342 0.094 Uiso 1 1 calc R . .
H25C H 0.7982 0.1723 1.0649 0.094 Uiso 1 1 calc R . .
C26 C 0.7930(3) 0.2988(4) 1.0502(6) 0.072(3) Uani 1 1 d . . .
H26A H 0.8356 0.2815 1.0956 0.107 Uiso 1 1 calc R . .
H26B H 0.7840 0.3419 1.0805 0.107 Uiso 1 1 calc R . .
H26C H 0.7969 0.3028 0.9678 0.107 Uiso 1 1 calc R . .
C27 C 0.5871(3) 0.4292(3) 0.8028(5) 0.0388(16) Uani 1 1 d . . .
C28 C 0.6571(3) 0.4641(3) 0.8117(6) 0.0568(19) Uani 1 1 d . . .
H28A H 0.6510 0.5044 0.7656 0.085 Uiso 1 1 calc R . .
H28B H 0.6885 0.4352 0.7814 0.085 Uiso 1 1 calc R . .
H28C H 0.6756 0.4745 0.8937 0.085 Uiso 1 1 calc R . .
C29 C 0.5418(3) 0.4750(3) 0.8604(5) 0.0453(17) Uani 1 1 d . . .
H29A H 0.5359 0.5165 0.8179 0.068 Uiso 1 1 calc R . .
H29B H 0.5635 0.4830 0.9420 0.068 Uiso 1 1 calc R . .
H29C H 0.4975 0.4546 0.8577 0.068 Uiso 1 1 calc R . .
C30 C 0.5566(3) 0.4212(3) 0.6688(5) 0.0490(18) Uani 1 1 d . . .
H30A H 0.5121 0.4002 0.6590 0.074 Uiso 1 1 calc R . .
H30B H 0.5871 0.3943 0.6323 0.074 Uiso 1 1 calc R . .
H30C H 0.5517 0.4643 0.6316 0.074 Uiso 1 1 calc R . .
C31 C 0.3210(3) 0.1483(3) 0.7065(5) 0.0414(16) Uani 1 1 d . . .
H31A H 0.3365 0.1451 0.6310 0.050 Uiso 1 1 calc R . .
H31B H 0.2930 0.1093 0.7145 0.050 Uiso 1 1 calc R . .
C32 C 0.3833(3) 0.1499(3) 0.8084(5) 0.0384(16) Uani 1 1 d . . .
H32A H 0.3677 0.1555 0.8834 0.046 Uiso 1 1 calc R . .
H32B H 0.4078 0.1078 0.8115 0.046 Uiso 1 1 calc R . .
C33 C 0.2338(3) 0.2029(3) 0.7974(5) 0.0467(19) Uani 1 1 d . . .
H33A H 0.2069 0.2427 0.7984 0.070 Uiso 1 1 calc R . .
H33B H 0.2623 0.1961 0.8748 0.070 Uiso 1 1 calc R . .
H33C H 0.2034 0.1655 0.7775 0.070 Uiso 1 1 calc R . .
C34 C 0.4702(3) 0.1890(4) 0.6982(4) 0.0391(14) Uani 1 1 d . . .
H34A H 0.4958 0.1485 0.7176 0.059 Uiso 1 1 calc R . .
H34B H 0.5016 0.2247 0.6916 0.059 Uiso 1 1 calc R . .
H34C H 0.4384 0.1836 0.6235 0.059 Uiso 1 1 calc R . .
C41 C 0.3521(3) 0.4837(3) 0.8219(5) 0.0402(17) Uani 1 1 d . . .
H41 H 0.3422 0.4639 0.8903 0.048 Uiso 1 1 calc R . .
C42 C 0.3545(3) 0.5529(3) 0.8169(5) 0.0432(16) Uani 1 1 d . . .
H42 H 0.3472 0.5787 0.8811 0.052 Uiso 1 1 calc R . .
C43 C 0.3677(3) 0.5820(3) 0.7157(6) 0.0496(18) Uani 1 1 d . . .
H43 H 0.3688 0.6282 0.7091 0.060 Uiso 1 1 calc R . .
C44 C 0.3791(4) 0.5424(4) 0.6245(6) 0.059(2) Uani 1 1 d . . .
H44 H 0.3884 0.5614 0.5549 0.071 Uiso 1 1 calc R . .
C45 C 0.3768(3) 0.4754(3) 0.6354(5) 0.0420(16) Uani 1 1 d . . .
H45 H 0.3848 0.4493 0.5722 0.050 Uiso 1 1 calc R . .
C51 C 0.0279(8) 0.5103(10) 0.0388(14) 0.106(6) Uiso 0.50 1 d PD . .
H51A H 0.0085 0.5311 0.1017 0.128 Uiso 0.50 1 calc PR . .
H51B H 0.0453 0.5468 -0.0028 0.128 Uiso 0.50 1 calc PR . .
C52 C 0.0927(10) 0.4775(9) 0.1050(19) 0.159(10) Uiso 0.50 1 d PD . .
H52A H 0.0810 0.4388 0.1480 0.190 Uiso 0.50 1 calc PR . .
H52B H 0.1213 0.4631 0.0494 0.190 Uiso 0.50 1 calc PR . .
C53 C 0.1310(10) 0.5276(13) 0.1908(18) 0.182(11) Uiso 0.50 1 d PD . .
H53A H 0.1539 0.5589 0.1480 0.273 Uiso 0.50 1 calc PR . .
H53B H 0.1647 0.5051 0.2496 0.273 Uiso 0.50 1 calc PR . .
H53C H 0.0988 0.5508 0.2296 0.273 Uiso 0.50 1 calc PR . .

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
U 0.02975(11) 0.03070(11) 0.03407(10) -0.00061(15) 0.00356(7) 0.00156(16)
O1U 0.036(2) 0.026(2) 0.058(2) 0.004(2) -0.0051(18) 0.004(2)
O1 0.033(2) 0.036(3) 0.055(3) -0.002(2) -0.001(2) 0.004(2)
O2U 0.043(2) 0.038(3) 0.041(2) -0.001(2) 0.0085(17) 0.000(2)
O2 0.032(2) 0.032(3) 0.048(2) 0.0034(19) 0.0038(19) 0.0029(18)
N1 0.029(3) 0.026(3) 0.043(3) 0.002(2) 0.005(3) -0.002(2)
N2 0.034(3) 0.033(4) 0.031(3) -0.002(2) 0.003(2) -0.003(2)
N3 0.034(3) 0.030(3) 0.045(3) 0.004(3) 0.006(2) 0.000(3)
C1 0.037(4) 0.036(4) 0.040(4) -0.011(3) 0.005(3) -0.008(3)
C2 0.029(4) 0.038(5) 0.043(4) 0.002(3) 0.008(3) 0.000(3)
C3 0.041(4) 0.042(5) 0.053(4) -0.004(3) 0.001(4) -0.007(4)
C4 0.038(4) 0.053(6) 0.051(4) 0.000(4) -0.004(3) 0.004(3)
C5 0.035(4) 0.047(5) 0.083(5) 0.005(4) -0.008(4) 0.012(3)
C6 0.037(4) 0.047(5) 0.066(4) -0.003(4) -0.002(3) 0.009(3)
C7 0.030(3) 0.038(5) 0.043(3) 0.000(3) -0.001(3) 0.000(3)
C8 0.037(4) 0.070(6) 0.074(5) 0.004(4) -0.013(4) -0.002(4)
C9 0.082(7) 0.187(13) 0.085(6) 0.011(8) -0.024(5) -0.034(8)
C10 0.041(5) 0.190(12) 0.112(7) -0.027(8) -0.005(5) -0.026(7)
C11 0.148(11) 0.093(10) 0.282(16) -0.057(10) -0.150(11) 0.016(8)
C12 0.046(5) 0.052(6) 0.090(6) -0.007(5) -0.007(4) 0.016(4)
C13 0.079(7) 0.078(7) 0.154(8) -0.036(6) -0.017(6) 0.034(5)
C14 0.078(6) 0.044(5) 0.116(7) 0.008(5) -0.022(5) -0.003(5)
C15 0.061(6) 0.077(7) 0.096(6) -0.032(5) 0.006(4) 0.021(5)
C16 0.036(4) 0.034(4) 0.035(3) 0.000(3) 0.001(3) -0.003(3)
C17 0.038(4) 0.030(4) 0.031(3) -0.001(3) -0.001(3) -0.001(3)
C18 0.043(4) 0.029(4) 0.035(3) 0.002(3) 0.006(3) -0.001(3)
C19 0.033(4) 0.047(5) 0.032(3) -0.001(3) 0.006(3) 0.003(3)
C20 0.029(3) 0.046(5) 0.038(3) -0.010(3) 0.010(3) -0.004(3)
C21 0.031(4) 0.038(4) 0.032(3) -0.004(3) 0.011(3) -0.004(3)
C22 0.029(3) 0.039(4) 0.030(3) -0.003(3) 0.001(2) 0.006(4)
C23 0.034(4) 0.048(5) 0.039(4) -0.002(3) 0.003(3) 0.005(3)
C24 0.051(5) 0.142(9) 0.042(4) 0.004(5) -0.014(4) 0.020(5)
C25 0.046(4) 0.070(5) 0.066(4) 0.008(5) -0.009(3) 0.009(5)
C26 0.035(4) 0.084(7) 0.087(5) 0.005(5) -0.011(4) 0.002(4)
C27 0.038(4) 0.032(4) 0.045(4) -0.002(3) 0.005(3) -0.005(3)
C28 0.049(4) 0.032(4) 0.090(5) 0.017(4) 0.016(4) -0.004(3)
C29 0.047(4) 0.037(4) 0.049(4) -0.004(3) 0.003(3) 0.000(3)
C30 0.060(5) 0.042(5) 0.046(4) 0.006(3) 0.012(3) 0.004(4)
C31 0.038(4) 0.036(4) 0.048(4) -0.003(3) 0.002(3) -0.002(3)
C32 0.040(4) 0.027(4) 0.045(4) 0.003(3) 0.002(3) -0.001(3)
C33 0.043(4) 0.051(5) 0.048(4) 0.001(3) 0.015(3) -0.008(3)
C34 0.039(3) 0.033(4) 0.044(3) -0.006(3) 0.004(3) 0.008(3)
C41 0.039(4) 0.048(5) 0.031(3) 0.001(3) 0.000(3) 0.007(3)
C42 0.044(4) 0.034(4) 0.047(4) -0.013(3) -0.002(3) 0.005(3)
C43 0.050(4) 0.025(4) 0.074(5) 0.000(3) 0.011(4) 0.001(3)
C44 0.075(5) 0.044(5) 0.064(5) 0.010(4) 0.027(4) 0.013(4)
C45 0.053(4) 0.036(4) 0.039(3) 0.000(3) 0.013(3) 0.003(3)

_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 O1U 1.764(4) . ?
U O2U 1.790(3) . ?
U O1 2.201(4) . ?
U O2 2.231(4) . ?
U N3 2.593(5) . ?
U N1 2.641(5) . ?
U N2 2.649(5) . ?
O1 C7 1.342(6) . ?
O2 C22 1.336(6) . ?
N1 C33 1.477(7) . ?
N1 C31 1.493(7) . ?
N1 C1 1.498(7) . ?
N2 C32 1.473(7) . ?
N2 C34 1.486(7) . ?
N2 C16 1.503(7) . ?
N3 C41 1.328(7) . ?
N3 C45 1.349(7) . ?
C1 C2 1.517(8) . ?
C2 C3 1.384(8) . ?
C2 C7 1.398(9) . ?
C3 C4 1.391(9) . ?
C4 C5 1.378(9) . ?
C4 C8 1.533(9) . ?
C5 C6 1.387(8) . ?
C6 C7 1.408(8) . ?
C6 C12 1.542(10) . ?
C8 C11 1.441(12) . ?
C8 C10 1.488(10) . ?
C8 C9 1.515(11) . ?
C12 C14 1.509(10) . ?
C12 C15 1.530(9) . ?
C12 C13 1.539(10) . ?
C16 C17 1.509(8) . ?
C17 C18 1.399(8) . ?
C17 C22 1.405(9) . ?
C18 C19 1.381(8) . ?
C19 C20 1.393(8) . ?
C19 C23 1.545(8) . ?
C20 C21 1.397(8) . ?
C21 C22 1.432(8) . ?
C21 C27 1.528(9) . ?
C23 C25 1.499(10) . ?
C23 C26 1.504(9) . ?
C23 C24 1.519(8) . ?
C27 C29 1.516(8) . ?
C27 C28 1.531(8) . ?
C27 C30 1.539(7) . ?
C31 C32 1.519(7) . ?
C41 C42 1.391(9) . ?
C42 C43 1.363(8) . ?
C43 C44 1.363(8) . ?
C44 C45 1.353(9) . ?
C51 C51 1.34(3) 3_565 ?
C51 C52 1.503(5) . ?
C52 C53 1.501(5) . ?

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
O1U U O2U 178.37(18) . . ?
O1U U O1 90.48(15) . . ?
O2U U O1 90.18(15) . . ?
O1U U O2 90.21(15) . . ?
O2U U O2 89.88(15) . . ?
O1 U O2 153.04(13) . . ?
O1U U N3 89.49(19) . . ?
O2U U N3 92.11(19) . . ?
O1 U N3 76.85(15) . . ?
O2 U N3 76.21(15) . . ?
O1U U N1 87.29(17) . . ?
O2U U N1 91.57(17) . . ?
O1 U N1 68.76(15) . . ?
O2 U N1 138.19(15) . . ?
N3 U N1 145.41(15) . . ?
O1U U N2 89.39(17) . . ?
O2U U N2 89.12(17) . . ?
O1 U N2 137.17(15) . . ?
O2 U N2 69.79(14) . . ?
N3 U N2 145.98(15) . . ?
N1 U N2 68.45(13) . . ?
C7 O1 U 147.0(4) . . ?
C22 O2 U 148.0(4) . . ?
C33 N1 C31 109.8(5) . . ?
C33 N1 C1 109.4(5) . . ?
C31 N1 C1 106.0(4) . . ?
C33 N1 U 111.6(3) . . ?
C31 N1 U 110.5(3) . . ?
C1 N1 U 109.4(3) . . ?
C32 N2 C34 110.9(5) . . ?
C32 N2 C16 106.2(4) . . ?
C34 N2 C16 109.4(4) . . ?
C32 N2 U 108.8(3) . . ?
C34 N2 U 111.6(3) . . ?
C16 N2 U 109.8(3) . . ?
C41 N3 C45 116.7(5) . . ?
C41 N3 U 121.9(4) . . ?
C45 N3 U 121.4(4) . . ?
N1 C1 C2 116.7(5) . . ?
C3 C2 C7 120.6(6) . . ?
C3 C2 C1 117.1(6) . . ?
C7 C2 C1 122.2(5) . . ?
C2 C3 C4 121.7(7) . . ?
C5 C4 C3 116.4(6) . . ?
C5 C4 C8 121.8(6) . . ?
C3 C4 C8 121.8(7) . . ?
C4 C5 C6 124.3(6) . . ?
C5 C6 C7 118.0(6) . . ?
C5 C6 C12 121.5(6) . . ?
C7 C6 C12 120.4(6) . . ?
O1 C7 C2 118.9(5) . . ?
O1 C7 C6 122.5(6) . . ?
C2 C7 C6 118.6(6) . . ?
C11 C8 C10 114.4(9) . . ?
C11 C8 C9 104.4(9) . . ?
C10 C8 C9 105.0(8) . . ?
C11 C8 C4 113.4(7) . . ?
C10 C8 C4 111.0(7) . . ?
C9 C8 C4 107.8(6) . . ?
C14 C12 C15 110.8(7) . . ?
C14 C12 C13 108.4(7) . . ?
C15 C12 C13 106.8(7) . . ?
C14 C12 C6 109.7(7) . . ?
C15 C12 C6 110.4(7) . . ?
C13 C12 C6 110.6(6) . . ?
N2 C16 C17 116.0(5) . . ?
C18 C17 C22 120.2(6) . . ?
C18 C17 C16 118.2(6) . . ?
C22 C17 C16 121.4(5) . . ?
C19 C18 C17 122.2(6) . . ?
C18 C19 C20 116.7(6) . . ?
C18 C19 C23 120.6(6) . . ?
C20 C19 C23 122.7(6) . . ?
C19 C20 C21 124.6(6) . . ?
C20 C21 C22 117.0(6) . . ?
C20 C21 C27 122.4(5) . . ?
C22 C21 C27 120.6(5) . . ?
O2 C22 C17 119.4(6) . . ?
O2 C22 C21 121.4(6) . . ?
C17 C22 C21 119.1(5) . . ?
C25 C23 C26 107.3(6) . . ?
C25 C23 C24 109.3(6) . . ?
C26 C23 C24 109.0(6) . . ?
C25 C23 C19 109.9(5) . . ?
C26 C23 C19 112.4(6) . . ?
C24 C23 C19 108.9(5) . . ?
C29 C27 C21 110.8(5) . . ?
C29 C27 C28 106.8(5) . . ?
C21 C27 C28 112.7(5) . . ?
C29 C27 C30 110.2(5) . . ?
C21 C27 C30 109.7(5) . . ?
C28 C27 C30 106.6(5) . . ?
N1 C31 C32 110.4(5) . . ?
N2 C32 C31 111.5(5) . . ?
N3 C41 C42 123.1(6) . . ?
C43 C42 C41 118.4(6) . . ?
C44 C43 C42 118.9(6) . . ?
C45 C44 C43 119.8(6) . . ?
N3 C45 C44 123.1(6) . . ?
C51 C51 C52 135(2) 3_565 . ?
C53 C52 C51 107.7(7) . . ?

_diffrn_measured_fraction_theta_max 0.821
_diffrn_reflns_theta_full        28.95
_diffrn_measured_fraction_theta_full 0.821
_refine_diff_density_max         1.907
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.111