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

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

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

_publ_section_title              
;
Structural variability in uranyl-lanthanide
heterometallic complexes with DOTA and oxalato ligands
;
_publ_author_name                'Pierre Thuery'

# Attachment 'CIF.txt'

data_1
_database_code_depnum_ccdc_archive 'CCDC 727650'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H48 N8 O24 Sm2 U2'
_chemical_formula_weight         1729.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   13.1889(6)
_cell_length_b                   8.6070(4)
_cell_length_c                   20.4006(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.461(3)
_cell_angle_gamma                90.00
_cell_volume                     2311.59(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    106009
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_exptl_absorpt_coefficient_mu    9.583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.167
_exptl_absorpt_correction_T_max  0.563
_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 eight ω scans with 2° steps (525 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            106009
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.57
_diffrn_reflns_theta_max         25.68
_reflns_number_total             4390
_reflns_number_gt                4106
_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. The H atoms were introduced at calculated
positions and 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)+(0.0298P)²+0.2958P] 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         4390
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0195
_refine_ls_wR_factor_ref         0.0477
_refine_ls_wR_factor_gt          0.0468
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.591
_refine_diff_density_min         -1.150
_refine_diff_density_rms         0.147

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 0.184471(9) 0.676570(13) 0.074869(5) 0.01411(5) Uani 1 1 d . . .
Sm Sm 0.366062(12) 0.419006(19) 0.331264(7) 0.01348(6) Uani 1 1 d . . .
O1 O 0.28507(17) 0.5497(3) 0.23739(10) 0.0179(5) Uani 1 1 d . . .
O2 O 0.15366(19) 0.6779(2) 0.18796(11) 0.0181(5) Uani 1 1 d . . .
O3 O 0.31606(18) 0.6430(3) 0.39333(11) 0.0171(5) Uani 1 1 d . . .
O4 O 0.28419(17) 0.7620(3) 0.48609(10) 0.0172(5) Uani 1 1 d . . .
O5 O 0.51562(17) 0.3865(3) 0.40319(10) 0.0167(5) Uani 1 1 d . . .
O6 O 0.66689(18) 0.2921(3) 0.38220(11) 0.0185(5) Uani 1 1 d . . .
O7 O 0.47302(18) 0.3070(3) 0.25844(11) 0.0178(5) Uani 1 1 d . . .
O8 O 0.51713(17) 0.1261(3) 0.18814(10) 0.0182(5) Uani 1 1 d . . .
O9 O 0.24064(17) 0.4899(3) 0.08390(10) 0.0181(5) Uani 1 1 d . . .
O10 O 0.12304(18) 0.8598(3) 0.06580(11) 0.0192(5) Uani 1 1 d . . .
O11 O 0.01752(18) 0.5570(3) 0.08194(11) 0.0215(5) Uani 1 1 d . . .
O12 O 0.10686(18) 0.5832(3) -0.03089(11) 0.0218(5) Uani 1 1 d . . .
N1 N 0.1617(2) 0.4260(3) 0.32814(13) 0.0167(6) Uani 1 1 d . . .
N2 N 0.3006(2) 0.3517(3) 0.44713(13) 0.0157(6) Uani 1 1 d . . .
N3 N 0.4136(2) 0.1196(3) 0.37011(12) 0.0168(6) Uani 1 1 d . . .
N4 N 0.2765(2) 0.1934(3) 0.25408(13) 0.0176(6) Uani 1 1 d . . .
C1 C 0.1283(3) 0.4253(4) 0.39710(15) 0.0168(7) Uani 1 1 d . . .
H1A H 0.0570 0.3974 0.3966 0.020 Uiso 1 1 calc R . .
H1B H 0.1358 0.5289 0.4155 0.020 Uiso 1 1 calc R . .
C2 C 0.1900(3) 0.3115(4) 0.44016(16) 0.0171(7) Uani 1 1 d . . .
H2A H 0.1631 0.3093 0.4834 0.020 Uiso 1 1 calc R . .
H2B H 0.1824 0.2082 0.4215 0.020 Uiso 1 1 calc R . .
C3 C 0.3599(3) 0.2207(4) 0.47819(15) 0.0185(7) Uani 1 1 d . . .
H3A H 0.3281 0.1887 0.5177 0.022 Uiso 1 1 calc R . .
H3B H 0.4279 0.2568 0.4910 0.022 Uiso 1 1 calc R . .
C4 C 0.3670(3) 0.0822(4) 0.43311(16) 0.0191(7) Uani 1 1 d . . .
H4A H 0.4070 0.0019 0.4558 0.023 Uiso 1 1 calc R . .
H4B H 0.2993 0.0409 0.4233 0.023 Uiso 1 1 calc R . .
C5 C 0.3779(3) -0.0006(4) 0.32125(16) 0.0181(7) Uani 1 1 d . . .
H5A H 0.3732 -0.1003 0.3431 0.022 Uiso 1 1 calc R . .
H5B H 0.4268 -0.0103 0.2879 0.022 Uiso 1 1 calc R . .
C6 C 0.2753(3) 0.0417(4) 0.28910(16) 0.0198(7) Uani 1 1 d . . .
H6A H 0.2539 -0.0391 0.2581 0.024 Uiso 1 1 calc R . .
H6B H 0.2259 0.0464 0.3224 0.024 Uiso 1 1 calc R . .
C7 C 0.1706(3) 0.2376(4) 0.23311(16) 0.0202(7) Uani 1 1 d . . .
H7A H 0.1360 0.1490 0.2127 0.024 Uiso 1 1 calc R . .
H7B H 0.1716 0.3201 0.2007 0.024 Uiso 1 1 calc R . .
C8 C 0.1120(3) 0.2928(4) 0.29163(17) 0.0203(7) Uani 1 1 d . . .
H8A H 0.0442 0.3236 0.2758 0.024 Uiso 1 1 calc R . .
H8B H 0.1055 0.2066 0.3217 0.024 Uiso 1 1 calc R . .
C9 C 0.1331(3) 0.5737(4) 0.29455(16) 0.0190(7) Uani 1 1 d . . .
H9A H 0.1432 0.6592 0.3252 0.023 Uiso 1 1 calc R . .
H9B H 0.0616 0.5706 0.2802 0.023 Uiso 1 1 calc R . .
C10 C 0.1961(3) 0.6014(4) 0.23545(15) 0.0174(7) Uani 1 1 d . . .
C11 C 0.3149(3) 0.4888(4) 0.49034(15) 0.0178(7) Uani 1 1 d . . .
H11A H 0.3822 0.4847 0.5122 0.021 Uiso 1 1 calc R . .
H11B H 0.2659 0.4848 0.5239 0.021 Uiso 1 1 calc R . .
C12 C 0.3027(2) 0.6413(4) 0.45351(16) 0.0164(7) Uani 1 1 d . . .
C13 C 0.5267(3) 0.1164(4) 0.37725(17) 0.0189(7) Uani 1 1 d . . .
H13A H 0.5525 0.0724 0.3378 0.023 Uiso 1 1 calc R . .
H13B H 0.5479 0.0494 0.4138 0.023 Uiso 1 1 calc R . .
C14 C 0.5728(3) 0.2767(4) 0.38883(15) 0.0175(7) Uani 1 1 d . . .
C15 C 0.3391(3) 0.1794(4) 0.19576(16) 0.0188(7) Uani 1 1 d . . .
H15A H 0.3171 0.2564 0.1632 0.023 Uiso 1 1 calc R . .
H15B H 0.3290 0.0774 0.1762 0.023 Uiso 1 1 calc R . .
C16 C 0.4516(3) 0.2029(4) 0.21515(16) 0.0167(7) Uani 1 1 d . . .
C17 C -0.0259(3) 0.4921(4) 0.03277(15) 0.0183(7) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U O9 1.775(2) . ?
U O10 1.777(2) . ?
U O6 2.322(2) 2_655 ?
U O4 2.362(2) 4_575 ?
U O2 2.367(2) . ?
U O11 2.443(2) . ?
U O12 2.466(2) . ?
Sm O7 2.319(2) . ?
Sm O5 2.403(2) . ?
Sm O8 2.404(2) 2_655 ?
Sm O1 2.414(2) . ?
Sm O3 2.420(2) . ?
Sm N2 2.630(3) . ?
Sm N1 2.693(3) . ?
Sm N4 2.724(3) . ?
Sm N3 2.757(3) . ?
O1 C10 1.254(4) . ?
O2 C10 1.273(4) . ?
O3 C12 1.251(4) . ?
O4 C12 1.265(4) . ?
O4 U 2.362(2) 4_576 ?
O5 C14 1.255(4) . ?
O6 C14 1.264(4) . ?
O6 U 2.322(2) 2_645 ?
O7 C16 1.278(4) . ?
O8 C16 1.243(4) . ?
O8 Sm 2.404(2) 2_645 ?
O11 C17 1.255(4) . ?
O12 C17 1.248(4) 3_565 ?
N1 C9 1.482(4) . ?
N1 C8 1.496(4) . ?
N1 C1 1.499(4) . ?
N2 C11 1.479(4) . ?
N2 C3 1.491(4) . ?
N2 C2 1.498(4) . ?
N3 C5 1.493(4) . ?
N3 C13 1.490(4) . ?
N3 C4 1.493(4) . ?
N4 C7 1.486(4) . ?
N4 C6 1.489(4) . ?
N4 C15 1.493(4) . ?
C1 C2 1.519(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.512(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.512(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.535(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.524(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C11 C12 1.516(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C13 C14 1.520(5) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C15 C16 1.526(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C17 O12 1.248(4) 3_565 ?
C17 C17 1.544(6) 3_565 ?

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
O9 U O10 177.56(10) . . ?
O9 U O6 90.62(9) . 2_655 ?
O10 U O6 91.64(10) . 2_655 ?
O9 U O4 91.95(9) . 4_575 ?
O10 U O4 89.61(9) . 4_575 ?
O6 U O4 72.35(8) 2_655 4_575 ?
O9 U O2 89.91(9) . . ?
O10 U O2 89.60(9) . . ?
O6 U O2 79.69(8) 2_655 . ?
O4 U O2 151.99(8) 4_575 . ?
O9 U O11 89.10(9) . . ?
O10 U O11 88.46(10) . . ?
O6 U O11 154.38(8) 2_655 . ?
O4 U O11 133.26(8) 4_575 . ?
O2 U O11 74.70(8) . . ?
O9 U O12 86.82(9) . . ?
O10 U O12 92.03(10) . . ?
O6 U O12 139.99(8) 2_655 . ?
O4 U O12 67.85(8) 4_575 . ?
O2 U O12 140.16(8) . . ?
O11 U O12 65.57(7) . . ?
O7 Sm O5 80.45(8) . . ?
O7 Sm O8 77.41(8) . 2_655 ?
O5 Sm O8 71.10(8) . 2_655 ?
O7 Sm O1 86.71(8) . . ?
O5 Sm O1 147.82(8) . . ?
O8 Sm O1 77.36(8) 2_655 . ?
O7 Sm O3 149.52(8) . . ?
O5 Sm O3 90.73(8) . . ?
O8 Sm O3 72.13(8) 2_655 . ?
O1 Sm O3 85.54(8) . . ?
O7 Sm N2 136.85(8) . . ?
O5 Sm N2 74.19(8) . . ?
O8 Sm N2 124.05(8) 2_655 . ?
O1 Sm N2 131.47(8) . . ?
O3 Sm N2 65.84(8) . . ?
O7 Sm N1 129.84(8) . . ?
O5 Sm N1 143.19(8) . . ?
O8 Sm N1 129.05(8) 2_655 . ?
O1 Sm N1 64.95(8) . . ?
O3 Sm N1 71.98(8) . . ?
N2 Sm N1 69.12(8) . . ?
O7 Sm N4 65.96(8) . . ?
O5 Sm N4 125.55(8) . . ?
O8 Sm N4 133.87(8) 2_655 . ?
O1 Sm N4 73.62(8) . . ?
O3 Sm N4 138.42(8) . . ?
N2 Sm N4 102.01(8) . . ?
N1 Sm N4 66.66(8) . . ?
O7 Sm N3 70.07(8) . . ?
O5 Sm N3 63.37(8) . . ?
O8 Sm N3 127.12(8) 2_655 . ?
O1 Sm N3 138.21(8) . . ?
O3 Sm N3 131.20(7) . . ?
N2 Sm N3 67.47(8) . . ?
N1 Sm N3 103.73(8) . . ?
N4 Sm N3 65.35(8) . . ?
C10 O1 Sm 124.0(2) . . ?
C10 O2 U 130.2(2) . . ?
C12 O3 Sm 124.3(2) . . ?
C12 O4 U 136.1(2) . 4_576 ?
C14 O5 Sm 115.3(2) . . ?
C14 O6 U 136.7(2) . 2_645 ?
C16 O7 Sm 128.1(2) . . ?
C16 O8 Sm 159.5(2) . 2_645 ?
C17 O11 U 120.6(2) . . ?
C17 O12 U 120.36(19) 3_565 . ?
C9 N1 C8 109.6(3) . . ?
C9 N1 C1 110.9(2) . . ?
C8 N1 C1 108.7(2) . . ?
C9 N1 Sm 104.85(19) . . ?
C8 N1 Sm 113.69(19) . . ?
C1 N1 Sm 109.15(19) . . ?
C11 N2 C3 107.8(2) . . ?
C11 N2 C2 109.2(3) . . ?
C3 N2 C2 110.4(3) . . ?
C11 N2 Sm 108.83(19) . . ?
C3 N2 Sm 110.87(19) . . ?
C2 N2 Sm 109.66(18) . . ?
C5 N3 C13 109.0(3) . . ?
C5 N3 C4 107.2(2) . . ?
C13 N3 C4 111.9(3) . . ?
C5 N3 Sm 113.50(18) . . ?
C13 N3 Sm 104.70(18) . . ?
C4 N3 Sm 110.52(18) . . ?
C7 N4 C6 109.0(3) . . ?
C7 N4 C15 110.3(3) . . ?
C6 N4 C15 109.5(3) . . ?
C7 N4 Sm 110.56(19) . . ?
C6 N4 Sm 111.39(19) . . ?
C15 N4 Sm 106.10(19) . . ?
N1 C1 C2 111.5(3) . . ?
N1 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
N2 C2 C1 113.0(3) . . ?
N2 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
N2 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
N2 C3 C4 112.8(3) . . ?
N2 C3 H3A 109.0 . . ?
C4 C3 H3A 109.0 . . ?
N2 C3 H3B 109.0 . . ?
C4 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
N3 C4 C3 113.4(3) . . ?
N3 C4 H4A 108.9 . . ?
C3 C4 H4A 108.9 . . ?
N3 C4 H4B 108.9 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
N3 C5 C6 111.1(3) . . ?
N3 C5 H5A 109.4 . . ?
C6 C5 H5A 109.4 . . ?
N3 C5 H5B 109.4 . . ?
C6 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
N4 C6 C5 112.6(3) . . ?
N4 C6 H6A 109.1 . . ?
C5 C6 H6A 109.1 . . ?
N4 C6 H6B 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
N4 C7 C8 111.3(3) . . ?
N4 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
N4 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
N1 C8 C7 113.5(3) . . ?
N1 C8 H8A 108.9 . . ?
C7 C8 H8A 108.9 . . ?
N1 C8 H8B 108.9 . . ?
C7 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
N1 C9 C10 111.4(3) . . ?
N1 C9 H9A 109.4 . . ?
C10 C9 H9A 109.4 . . ?
N1 C9 H9B 109.4 . . ?
C10 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
O1 C10 O2 125.1(3) . . ?
O1 C10 C9 118.3(3) . . ?
O2 C10 C9 116.6(3) . . ?
N2 C11 C12 112.9(3) . . ?
N2 C11 H11A 109.0 . . ?
C12 C11 H11A 109.0 . . ?
N2 C11 H11B 109.0 . . ?
C12 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
O3 C12 O4 123.3(3) . . ?
O3 C12 C11 118.7(3) . . ?
O4 C12 C11 117.9(3) . . ?
N3 C13 C14 112.8(3) . . ?
N3 C13 H13A 109.0 . . ?
C14 C13 H13A 109.0 . . ?
N3 C13 H13B 109.0 . . ?
C14 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
O5 C14 O6 123.6(3) . . ?
O5 C14 C13 118.7(3) . . ?
O6 C14 C13 117.7(3) . . ?
N4 C15 C16 111.0(3) . . ?
N4 C15 H15A 109.4 . . ?
C16 C15 H15A 109.4 . . ?
N4 C15 H15B 109.4 . . ?
C16 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
O8 C16 O7 123.3(3) . . ?
O8 C16 C15 120.4(3) . . ?
O7 C16 C15 116.3(3) . . ?
O12 C17 O11 127.1(3) 3_565 . ?
O12 C17 C17 116.2(3) 3_565 3_565 ?
O11 C17 C17 116.7(4) . 3_565 ?

#===END

data_2
_database_code_depnum_ccdc_archive 'CCDC 727651'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H48 Eu2 N8 O24 U2'
_chemical_formula_weight         1732.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   13.1694(13)
_cell_length_b                   8.6230(7)
_cell_length_c                   20.3522(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.309(6)
_cell_angle_gamma                90.00
_cell_volume                     2307.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    82004
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1620
_exptl_absorpt_coefficient_mu    9.774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.202
_exptl_absorpt_correction_T_max  0.746
_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 seven ω scans with 2° steps (479 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            82004
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         25.68
_reflns_number_total             4379
_reflns_number_gt                3518
_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. The H atoms were introduced at calculated
positions and 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)+(0.0352P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4379
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0702
_refine_ls_wR_factor_gt          0.0661
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_restrained_S_all      0.993
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.893
_refine_diff_density_min         -1.454
_refine_diff_density_rms         0.195

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 0.18475(2) 0.67646(3) 0.074504(12) 0.01774(8) Uani 1 1 d . . .
Eu Eu 0.36600(3) 0.41806(4) 0.331034(15) 0.01726(10) Uani 1 1 d . . .
O1 O 0.2855(4) 0.5482(5) 0.2373(2) 0.0213(10) Uani 1 1 d . . .
O2 O 0.1545(4) 0.6767(5) 0.1878(2) 0.0201(10) Uani 1 1 d . . .
O3 O 0.3161(4) 0.6419(5) 0.3923(2) 0.0209(10) Uani 1 1 d . . .
O4 O 0.2848(4) 0.7622(5) 0.4851(2) 0.0200(10) Uani 1 1 d . . .
O5 O 0.5147(4) 0.3872(5) 0.4030(2) 0.0194(10) Uani 1 1 d . . .
O6 O 0.6664(4) 0.2941(5) 0.3828(2) 0.0226(11) Uani 1 1 d . . .
O7 O 0.4736(4) 0.3070(5) 0.2585(2) 0.0197(10) Uani 1 1 d . . .
O8 O 0.5184(4) 0.1237(5) 0.1894(2) 0.0230(11) Uani 1 1 d . . .
O9 O 0.2414(4) 0.4913(5) 0.0835(2) 0.0223(11) Uani 1 1 d . . .
O10 O 0.1230(4) 0.8587(5) 0.0655(2) 0.0230(11) Uani 1 1 d . . .
O11 O 0.0178(4) 0.5571(5) 0.0821(2) 0.0246(11) Uani 1 1 d . . .
O12 O 0.1071(4) 0.5826(6) -0.0315(2) 0.0243(11) Uani 1 1 d . . .
N1 N 0.1620(4) 0.4258(6) 0.3285(3) 0.0211(13) Uani 1 1 d . . .
N2 N 0.3016(4) 0.3520(6) 0.4468(3) 0.0189(12) Uani 1 1 d . . .
N3 N 0.4132(4) 0.1202(6) 0.3705(3) 0.0205(12) Uani 1 1 d . . .
N4 N 0.2768(4) 0.1938(6) 0.2544(3) 0.0204(12) Uani 1 1 d . . .
C1 C 0.1287(5) 0.4254(8) 0.3975(3) 0.0221(15) Uani 1 1 d . . .
H1A H 0.0573 0.3973 0.3972 0.026 Uiso 1 1 calc R . .
H1B H 0.1360 0.5290 0.4158 0.026 Uiso 1 1 calc R . .
C2 C 0.1900(5) 0.3132(7) 0.4404(3) 0.0213(15) Uani 1 1 d . . .
H2A H 0.1635 0.3123 0.4839 0.026 Uiso 1 1 calc R . .
H2B H 0.1817 0.2097 0.4222 0.026 Uiso 1 1 calc R . .
C3 C 0.3601(6) 0.2218(7) 0.4786(3) 0.0229(16) Uani 1 1 d . . .
H3A H 0.3278 0.1909 0.5182 0.028 Uiso 1 1 calc R . .
H3B H 0.4283 0.2572 0.4914 0.028 Uiso 1 1 calc R . .
C4 C 0.3667(6) 0.0825(8) 0.4336(3) 0.0237(16) Uani 1 1 d . . .
H4A H 0.4068 0.0024 0.4563 0.028 Uiso 1 1 calc R . .
H4B H 0.2989 0.0414 0.4241 0.028 Uiso 1 1 calc R . .
C5 C 0.3776(5) -0.0010(7) 0.3216(3) 0.0202(15) Uani 1 1 d . . .
H5A H 0.3736 -0.1004 0.3435 0.024 Uiso 1 1 calc R . .
H5B H 0.4264 -0.0103 0.2878 0.024 Uiso 1 1 calc R . .
C6 C 0.2745(6) 0.0405(7) 0.2899(3) 0.0246(16) Uani 1 1 d . . .
H6A H 0.2529 -0.0401 0.2589 0.030 Uiso 1 1 calc R . .
H6B H 0.2254 0.0457 0.3235 0.030 Uiso 1 1 calc R . .
C7 C 0.1717(5) 0.2389(8) 0.2338(3) 0.0211(15) Uani 1 1 d . . .
H7A H 0.1372 0.1514 0.2125 0.025 Uiso 1 1 calc R . .
H7B H 0.1733 0.3224 0.2020 0.025 Uiso 1 1 calc R . .
C8 C 0.1121(6) 0.2915(8) 0.2918(3) 0.0253(16) Uani 1 1 d . . .
H8A H 0.0442 0.3217 0.2758 0.030 Uiso 1 1 calc R . .
H8B H 0.1058 0.2052 0.3218 0.030 Uiso 1 1 calc R . .
C9 C 0.1333(5) 0.5726(8) 0.2943(3) 0.0215(15) Uani 1 1 d . . .
H9A H 0.1421 0.6585 0.3249 0.026 Uiso 1 1 calc R . .
H9B H 0.0621 0.5684 0.2793 0.026 Uiso 1 1 calc R . .
C10 C 0.1980(6) 0.6004(7) 0.2355(3) 0.0218(16) Uani 1 1 d . . .
C11 C 0.3169(5) 0.4885(7) 0.4896(3) 0.0203(15) Uani 1 1 d . . .
H11A H 0.3850 0.4852 0.5103 0.024 Uiso 1 1 calc R . .
H11B H 0.2692 0.4839 0.5242 0.024 Uiso 1 1 calc R . .
C12 C 0.3025(5) 0.6413(8) 0.4529(3) 0.0205(15) Uani 1 1 d . . .
C13 C 0.5260(5) 0.1172(7) 0.3774(3) 0.0227(16) Uani 1 1 d . . .
H13A H 0.5518 0.0732 0.3378 0.027 Uiso 1 1 calc R . .
H13B H 0.5472 0.0504 0.4140 0.027 Uiso 1 1 calc R . .
C14 C 0.5724(6) 0.2777(8) 0.3889(3) 0.0235(16) Uani 1 1 d . . .
C15 C 0.3396(5) 0.1799(8) 0.1961(3) 0.0220(15) Uani 1 1 d . . .
H15A H 0.3186 0.2579 0.1638 0.026 Uiso 1 1 calc R . .
H15B H 0.3289 0.0787 0.1761 0.026 Uiso 1 1 calc R . .
C16 C 0.4533(6) 0.2010(7) 0.2162(3) 0.0203(15) Uani 1 1 d . . .
C17 C -0.0270(6) 0.4909(8) 0.0326(3) 0.0225(16) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U O9 1.767(4) . ?
U O10 1.774(4) . ?
U O6 2.331(5) 2_655 ?
U O2 2.362(4) . ?
U O4 2.368(4) 4_575 ?
U O11 2.441(5) . ?
U O12 2.471(4) . ?
Eu O7 2.312(4) . ?
Eu O8 2.389(4) 2_655 ?
Eu O5 2.392(5) . ?
Eu O1 2.406(4) . ?
Eu O3 2.410(4) . ?
Eu N2 2.612(5) . ?
Eu N1 2.685(6) . ?
Eu N4 2.710(5) . ?
Eu N3 2.751(5) . ?
O1 C10 1.236(9) . ?
O2 C10 1.281(8) . ?
O3 C12 1.257(8) . ?
O4 C12 1.260(8) . ?
O4 U 2.368(4) 4_576 ?
O5 C14 1.255(8) . ?
O6 C14 1.260(9) . ?
O6 U 2.331(5) 2_645 ?
O7 C16 1.272(8) . ?
O8 C16 1.237(8) . ?
O8 Eu 2.389(4) 2_645 ?
O11 C17 1.273(8) . ?
O12 C17 1.229(8) 3_565 ?
N1 C9 1.483(8) . ?
N1 C1 1.496(8) . ?
N1 C8 1.508(8) . ?
N2 C11 1.472(8) . ?
N2 C3 1.488(8) . ?
N2 C2 1.506(9) . ?
N3 C13 1.484(9) . ?
N3 C4 1.491(8) . ?
N3 C5 1.500(8) . ?
N4 C7 1.475(9) . ?
N4 C15 1.489(8) . ?
N4 C6 1.508(8) . ?
C1 C2 1.507(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.515(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.512(9) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.523(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.527(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C11 C12 1.521(9) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C13 C14 1.525(9) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C15 C16 1.540(10) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C17 O12 1.230(8) 3_565 ?
C17 C17 1.548(13) 3_565 ?

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
O9 U O10 177.7(2) . . ?
O9 U O6 90.79(19) . 2_655 ?
O10 U O6 91.35(19) . 2_655 ?
O9 U O2 89.64(18) . . ?
O10 U O2 89.89(18) . . ?
O6 U O2 79.67(16) 2_655 . ?
O9 U O4 91.79(18) . 4_575 ?
O10 U O4 89.68(18) . 4_575 ?
O6 U O4 72.32(16) 2_655 4_575 ?
O2 U O4 151.96(16) . 4_575 ?
O9 U O11 89.35(19) . . ?
O10 U O11 88.34(19) . . ?
O6 U O11 154.33(15) 2_655 . ?
O2 U O11 74.66(15) . . ?
O4 U O11 133.34(15) 4_575 . ?
O9 U O12 86.87(18) . . ?
O10 U O12 92.05(19) . . ?
O6 U O12 139.96(16) 2_655 . ?
O2 U O12 140.20(16) . . ?
O4 U O12 67.82(15) 4_575 . ?
O11 U O12 65.68(15) . . ?
O7 Eu O8 77.08(15) . 2_655 ?
O7 Eu O5 80.49(15) . . ?
O8 Eu O5 71.46(15) 2_655 . ?
O7 Eu O1 86.84(15) . . ?
O8 Eu O1 76.81(16) 2_655 . ?
O5 Eu O1 147.70(16) . . ?
O7 Eu O3 149.06(16) . . ?
O8 Eu O3 71.99(16) 2_655 . ?
O5 Eu O3 90.61(15) . . ?
O1 Eu O3 85.17(15) . . ?
O7 Eu N2 136.75(16) . . ?
O8 Eu N2 124.22(16) 2_655 . ?
O5 Eu N2 73.78(16) . . ?
O1 Eu N2 131.72(16) . . ?
O3 Eu N2 66.16(16) . . ?
O7 Eu N1 130.33(16) . . ?
O8 Eu N1 128.68(17) 2_655 . ?
O5 Eu N1 142.91(15) . . ?
O1 Eu N1 65.06(16) . . ?
O3 Eu N1 71.80(16) . . ?
N2 Eu N1 69.28(16) . . ?
O7 Eu N4 66.29(16) . . ?
O8 Eu N4 133.54(16) 2_655 . ?
O5 Eu N4 125.84(16) . . ?
O1 Eu N4 73.72(16) . . ?
O3 Eu N4 138.37(17) . . ?
N2 Eu N4 102.17(17) . . ?
N1 Eu N4 66.82(16) . . ?
O7 Eu N3 70.33(15) . . ?
O8 Eu N3 127.48(17) 2_655 . ?
O5 Eu N3 63.52(16) . . ?
O1 Eu N3 138.47(16) . . ?
O3 Eu N3 131.33(15) . . ?
N2 Eu N3 67.21(16) . . ?
N1 Eu N3 103.75(17) . . ?
N4 Eu N3 65.49(16) . . ?
C10 O1 Eu 124.1(4) . . ?
C10 O2 U 130.3(4) . . ?
C12 O3 Eu 124.3(4) . . ?
C12 O4 U 135.4(4) . 4_576 ?
C14 O5 Eu 115.4(4) . . ?
C14 O6 U 136.5(4) . 2_645 ?
C16 O7 Eu 128.1(5) . . ?
C16 O8 Eu 160.3(4) . 2_645 ?
C17 O11 U 121.1(4) . . ?
C17 O12 U 119.7(4) 3_565 . ?
C9 N1 C1 111.2(5) . . ?
C9 N1 C8 109.3(5) . . ?
C1 N1 C8 108.7(5) . . ?
C9 N1 Eu 105.0(4) . . ?
C1 N1 Eu 109.2(4) . . ?
C8 N1 Eu 113.4(4) . . ?
C11 N2 C3 107.2(5) . . ?
C11 N2 C2 109.1(5) . . ?
C3 N2 C2 110.4(5) . . ?
C11 N2 Eu 108.6(4) . . ?
C3 N2 Eu 111.7(4) . . ?
C2 N2 Eu 109.7(4) . . ?
C13 N3 C4 111.9(5) . . ?
C13 N3 C5 108.8(5) . . ?
C4 N3 C5 107.0(5) . . ?
C13 N3 Eu 104.6(4) . . ?
C4 N3 Eu 111.0(4) . . ?
C5 N3 Eu 113.6(4) . . ?
C7 N4 C15 110.5(5) . . ?
C7 N4 C6 108.9(5) . . ?
C15 N4 C6 109.8(5) . . ?
C7 N4 Eu 110.1(4) . . ?
C15 N4 Eu 105.9(4) . . ?
C6 N4 Eu 111.7(4) . . ?
N1 C1 C2 111.7(5) . . ?
N1 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 107.9 . . ?
N2 C2 C1 113.3(5) . . ?
N2 C2 H2A 108.9 . . ?
C1 C2 H2A 108.9 . . ?
N2 C2 H2B 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
N2 C3 C4 112.5(5) . . ?
N2 C3 H3A 109.1 . . ?
C4 C3 H3A 109.1 . . ?
N2 C3 H3B 109.1 . . ?
C4 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
N3 C4 C3 112.8(5) . . ?
N3 C4 H4A 109.0 . . ?
C3 C4 H4A 109.0 . . ?
N3 C4 H4B 109.0 . . ?
C3 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
N3 C5 C6 110.9(5) . . ?
N3 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
N4 C6 C5 111.7(6) . . ?
N4 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
N4 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
N4 C7 C8 112.1(6) . . ?
N4 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
N4 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
N1 C8 C7 112.5(6) . . ?
N1 C8 H8A 109.1 . . ?
C7 C8 H8A 109.1 . . ?
N1 C8 H8B 109.1 . . ?
C7 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
N1 C9 C10 111.2(5) . . ?
N1 C9 H9A 109.4 . . ?
C10 C9 H9A 109.4 . . ?
N1 C9 H9B 109.4 . . ?
C10 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
O1 C10 O2 125.7(6) . . ?
O1 C10 C9 118.8(6) . . ?
O2 C10 C9 115.4(6) . . ?
N2 C11 C12 113.2(5) . . ?
N2 C11 H11A 108.9 . . ?
C12 C11 H11A 108.9 . . ?
N2 C11 H11B 108.9 . . ?
C12 C11 H11B 108.9 . . ?
H11A C11 H11B 107.8 . . ?
O3 C12 O4 123.2(6) . . ?
O3 C12 C11 117.7(6) . . ?
O4 C12 C11 118.9(5) . . ?
N3 C13 C14 112.9(6) . . ?
N3 C13 H13A 109.0 . . ?
C14 C13 H13A 109.0 . . ?
N3 C13 H13B 109.0 . . ?
C14 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
O5 C14 O6 123.3(7) . . ?
O5 C14 C13 118.4(6) . . ?
O6 C14 C13 118.3(6) . . ?
N4 C15 C16 110.9(5) . . ?
N4 C15 H15A 109.5 . . ?
C16 C15 H15A 109.5 . . ?
N4 C15 H15B 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
O8 C16 O7 124.1(7) . . ?
O8 C16 C15 120.5(6) . . ?
O7 C16 C15 115.3(6) . . ?
O12 C17 O11 127.1(6) 3_565 . ?
O12 C17 C17 118.2(8) 3_565 3_565 ?
O11 C17 C17 114.7(8) . 3_565 ?

#===END

data_3
_database_code_depnum_ccdc_archive 'CCDC 727652'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H64 Gd2 N8 O44 U4'
_chemical_formula_weight         2603.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 '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'

_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                   43.698(2)
_cell_length_b                   8.3956(3)
_cell_length_c                   19.4670(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.999(2)
_cell_angle_gamma                90.00
_cell_volume                     6419.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    150622
_cell_measurement_theta_min      2.94
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.694
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4784
_exptl_absorpt_coefficient_mu    12.205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.408
_exptl_absorpt_correction_T_max  0.614
_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 eight ω scans with 2° steps (540 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            150622
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.94
_diffrn_reflns_theta_max         25.68
_reflns_number_total             6060
_reflns_number_gt                5057
_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. One uranyl group and the associated water
molecule are disordered over two positions (U2A and U2B) which were
refined with occupancy parameters constrained to sum to unity. The
two water solvent molecules were affected with 0.5 occupancy parameters
in order to retain acceptable displacement parameters. The H
atoms bound to O16 and O23 were found on a Fourier-difference map, but
the other O-bound H atoms were not found. 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.
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)+(0.0644P)²+131.1216P] 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         6060
_refine_ls_number_parameters     479
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0452
_refine_ls_wR_factor_ref         0.1222
_refine_ls_wR_factor_gt          0.1166
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.085
_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         4.565
_refine_diff_density_min         -2.393
_refine_diff_density_rms         0.253

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 0.811815(9) 0.41852(4) 0.485203(19) 0.02741(13) Uani 1 1 d . . .
U2A U 1.03680(2) 0.17798(11) 0.40930(4) 0.0313(3) Uani 0.5297(19) 1 d P . .
U2B U 1.02976(2) 0.93848(11) 0.39231(6) 0.0314(3) Uani 0.4703(19) 1 d P . .
Gd Gd 0.873309(11) 0.15924(5) 0.29910(2) 0.02198(13) Uani 1 1 d . . .
O1 O 0.84183(16) 0.2872(9) 0.3550(3) 0.0311(15) Uani 1 1 d . . .
O2 O 0.79656(18) 0.4125(9) 0.3508(4) 0.0331(16) Uani 1 1 d . . .
O3 O 0.86030(18) 0.3970(8) 0.2209(4) 0.0325(16) Uani 1 1 d . . .
O4 O 0.84902(19) 0.5171(9) 0.1110(4) 0.0374(17) Uani 1 1 d . . .
O5 O 0.92663(17) 0.1585(9) 0.2955(4) 0.0347(16) Uani 1 1 d . . .
O6 O 0.9782(3) 0.0560(16) 0.3415(7) 0.050(3) Uani 1 1 d . . .
O7 O 0.90434(19) 0.0555(10) 0.4227(4) 0.041(2) Uani 1 1 d . . .
O8 O 0.9094(3) -0.0703(17) 0.5265(7) 0.067(3) Uani 1 1 d . . .
O9 O 0.79355(18) 0.6107(9) 0.4714(4) 0.0343(16) Uani 1 1 d . . .
O10 O 0.82830(18) 0.2226(8) 0.4969(4) 0.0315(15) Uani 1 1 d . . .
O11A O 1.0331(3) 0.2136(18) 0.4943(8) 0.040(3) Uani 0.5297(19) 1 d P . .
O12A O 1.0430(4) 0.151(2) 0.3275(8) 0.051(4) Uani 0.5297(19) 1 d P . .
O11B O 1.0220(4) 0.929(2) 0.4741(10) 0.043(4) Uani 0.4703(19) 1 d P . .
O12B O 1.0367(4) 0.952(2) 0.3112(10) 0.050(5) Uani 0.4703(19) 1 d P . .
O13 O 0.9086(3) 0.3736(12) 0.3792(5) 0.065(3) Uani 1 1 d . . .
O14 O 0.75586(18) 0.2938(9) 0.4198(4) 0.0351(16) Uani 1 1 d . . .
O15 O 0.78528(18) 0.3429(9) 0.5695(4) 0.0354(17) Uani 1 1 d . . .
O16 O 0.8648(3) 0.5249(9) 0.4764(5) 0.051(2) Uani 1 1 d . . .
H16A H 0.8884 0.4879 0.5055 0.061 Uiso 1 1 d R . .
H16B H 0.8666 0.6243 0.4982 0.061 Uiso 1 1 d R . .
O17 O 1.0709(4) 0.4352(17) 0.4358(9) 0.064(4) Uani 1 1 d . . .
O18 O 1.0683(4) 0.7004(18) 0.4321(9) 0.074(4) Uani 1 1 d . . .
O19 O 1.0038(4) 0.4195(18) 0.3565(10) 0.075(4) Uani 1 1 d . . .
O20 O 1.0018(4) 0.6794(16) 0.3477(9) 0.069(4) Uani 1 1 d . . .
O21 O 1.0393(6) -0.109(3) 0.4307(16) 0.068(6) Uani 0.5297(19) 1 d PU . .
O22 O 1.0252(11) 1.238(6) 0.384(2) 0.084(12) Uani 0.4703(19) 1 d PU . .
O23 O 0.9718(6) 0.392(3) 0.4721(14) 0.087(7) Uani 0.50 1 d PU . .
H23A H 0.9769 0.2930 0.4791 0.104 Uiso 0.50 1 d PR . .
H23B H 0.9768 0.4240 0.4286 0.104 Uiso 0.50 1 d PR . .
O24 O 0.9352(8) 0.491(3) 0.2618(18) 0.043(7) Uani 0.50 1 d PU . .
N1 N 0.8062(2) 0.1640(15) 0.2115(5) 0.049(3) Uani 1 1 d . . .
N2 N 0.8597(2) 0.1027(10) 0.1572(5) 0.0287(18) Uani 1 1 d . . .
N3 N 0.8945(3) -0.1247(11) 0.2842(6) 0.056(3) Uani 1 1 d . . .
N4 N 0.8409(3) -0.0656(11) 0.3369(5) 0.046(3) Uani 1 1 d . . .
C1 C 0.7995(3) 0.175(2) 0.1286(6) 0.053(4) Uani 1 1 d . . .
H1A H 0.8034 0.2839 0.1171 0.064 Uiso 1 1 calc R . .
H1B H 0.7760 0.1484 0.0960 0.064 Uiso 1 1 calc R . .
C2 C 0.8230(3) 0.0624(17) 0.1124(6) 0.045(3) Uani 1 1 d . . .
H2A H 0.8191 -0.0455 0.1246 0.054 Uiso 1 1 calc R . .
H2B H 0.8173 0.0662 0.0583 0.054 Uiso 1 1 calc R . .
C3 C 0.8812(3) -0.0314(12) 0.1529(6) 0.035(2) Uani 1 1 d . . .
H3A H 0.9043 0.0062 0.1686 0.042 Uiso 1 1 calc R . .
H3B H 0.8725 -0.0676 0.1004 0.042 Uiso 1 1 calc R . .
C4 C 0.8815(4) -0.1680(14) 0.2027(7) 0.052(3) Uani 1 1 d . . .
H4A H 0.8586 -0.2090 0.1847 0.062 Uiso 1 1 calc R . .
H4B H 0.8956 -0.2525 0.1977 0.062 Uiso 1 1 calc R . .
C5 C 0.8822(5) -0.2491(17) 0.3230(9) 0.070(4) Uani 1 1 d . . .
H5A H 0.8844 -0.3539 0.3047 0.084 Uiso 1 1 calc R . .
H5B H 0.8966 -0.2461 0.3777 0.084 Uiso 1 1 calc R . .
C6 C 0.8470(5) -0.2239(18) 0.3088(9) 0.068(4) Uani 1 1 d . . .
H6A H 0.8403 -0.3081 0.3335 0.082 Uiso 1 1 calc R . .
H6B H 0.8326 -0.2314 0.2542 0.082 Uiso 1 1 calc R . .
C7 C 0.8033(3) -0.0310(19) 0.3047(8) 0.058(3) Uani 1 1 d . . .
H7A H 0.7914 -0.1254 0.3087 0.070 Uiso 1 1 calc R . .
H7B H 0.7994 0.0532 0.3342 0.070 Uiso 1 1 calc R . .
C8 C 0.7895(3) 0.019(2) 0.2227(7) 0.059(3) Uani 1 1 d . . .
H8A H 0.7927 -0.0679 0.1934 0.071 Uiso 1 1 calc R . .
H8B H 0.7653 0.0380 0.2030 0.071 Uiso 1 1 calc R . .
C9 C 0.7935(3) 0.3109(18) 0.2342(6) 0.050(3) Uani 1 1 d . . .
H9A H 0.7693 0.3007 0.2190 0.061 Uiso 1 1 calc R . .
H9B H 0.7969 0.4022 0.2078 0.061 Uiso 1 1 calc R . .
C10 C 0.8119(3) 0.3381(15) 0.3198(6) 0.037(3) Uani 1 1 d . . .
C11 C 0.8680(3) 0.2456(12) 0.1263(5) 0.031(2) Uani 1 1 d . . .
H11A H 0.8564 0.2424 0.0710 0.038 Uiso 1 1 calc R . .
H11B H 0.8923 0.2480 0.1414 0.038 Uiso 1 1 calc R . .
C12 C 0.8578(2) 0.3953(13) 0.1546(6) 0.032(2) Uani 1 1 d . . .
C13 C 0.9325(4) -0.1177(17) 0.3217(8) 0.061(4) Uani 1 1 d . . .
H13A H 0.9411 -0.1955 0.2977 0.073 Uiso 1 1 calc R . .
H13B H 0.9407 -0.1473 0.3750 0.073 Uiso 1 1 calc R . .
C14 C 0.9467(3) 0.0443(17) 0.3174(7) 0.051(3) Uani 1 1 d . . .
C15 C 0.8560(4) -0.0706(14) 0.4226(7) 0.049(3) Uani 1 1 d . . .
H15A H 0.8436 0.0025 0.4399 0.059 Uiso 1 1 calc R . .
H15B H 0.8533 -0.1769 0.4386 0.059 Uiso 1 1 calc R . .
C16 C 0.8922(3) -0.0281(16) 0.4590(7) 0.048(3) Uani 1 1 d . . .
C17 C 0.7414(3) 0.2348(12) 0.4567(5) 0.028(2) Uani 1 1 d . . .
C18 C 1.0552(5) 0.565(2) 0.4150(12) 0.056(5) Uani 1 1 d . . .
C19 C 1.0163(5) 0.557(3) 0.3681(12) 0.054(5) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O9 1.767(7) . ?
U1 O10 1.770(7) . ?
U1 O4 2.333(7) 6_566 ?
U1 O2 2.402(6) . ?
U1 O14 2.443(7) . ?
U1 O15 2.471(7) . ?
U1 O16 2.558(9) . ?
U2A O12A 1.744(14) . ?
U2A O11A 1.756(14) . ?
U2A O8 2.307(12) 5_756 ?
U2A O21 2.44(2) . ?
U2A O19 2.439(15) . ?
U2A O6 2.526(13) . ?
U2A O17 2.546(15) . ?
U2B O12B 1.737(17) . ?
U2B O11B 1.770(16) . ?
U2B O6 2.252(11) 1_565 ?
U2B O20 2.459(14) . ?
U2B O18 2.508(15) . ?
U2B O22 2.52(5) . ?
U2B O8 2.664(14) 5_766 ?
Gd O7 2.350(7) . ?
Gd O1 2.355(6) . ?
Gd O5 2.362(7) . ?
Gd O3 2.422(7) . ?
Gd O13 2.437(8) . ?
Gd N2 2.601(8) . ?
Gd N3 2.620(10) . ?
Gd N4 2.650(9) . ?
Gd N1 2.671(9) . ?
O1 C10 1.255(12) . ?
O2 C10 1.249(12) . ?
O3 C12 1.247(12) . ?
O4 C12 1.275(12) . ?
O4 U1 2.333(7) 6_565 ?
O5 C14 1.243(14) . ?
O5 O24 2.93(3) . ?
O6 C14 1.247(17) . ?
O6 U2B 2.252(11) 1_545 ?
O7 C16 1.266(14) . ?
O8 C16 1.247(16) . ?
O8 U2A 2.307(12) 5_756 ?
O8 U2B 2.664(14) 5_766 ?
O13 O23 2.56(3) . ?
O13 O24 3.14(3) . ?
O14 C17 1.248(11) . ?
O15 C17 1.236(12) 7_656 ?
O16 H16A 0.9829 . ?
O16 H16B 0.9243 . ?
O17 C18 1.25(2) . ?
O18 C18 1.25(2) . ?
O19 C19 1.25(2) . ?
O19 O24 2.81(4) . ?
O20 C19 1.18(2) . ?
O20 O24 3.08(3) . ?
O23 H23A 0.8591 . ?
O23 H23B 0.9984 . ?
N1 C8 1.484(18) . ?
N1 C9 1.496(17) . ?
N1 C1 1.513(13) . ?
N2 C11 1.458(13) . ?
N2 C2 1.491(13) . ?
N2 C3 1.492(13) . ?
N3 C4 1.478(16) . ?
N3 C13 1.49(2) . ?
N3 C5 1.519(17) . ?
N4 C15 1.502(15) . ?
N4 C6 1.505(17) . ?
N4 C7 1.509(18) . ?
C1 C2 1.527(18) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.497(15) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.45(2) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.498(19) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.515(14) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C11 C12 1.516(15) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C13 C14 1.51(2) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C15 C16 1.465(19) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C17 O15 1.236(12) 7_656 ?
C17 C17 1.536(18) 7_656 ?
C18 C19 1.54(3) . ?

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
O9 U1 O10 177.5(3) . . ?
O9 U1 O4 90.5(3) . 6_566 ?
O10 U1 O4 91.3(3) . 6_566 ?
O9 U1 O2 87.8(3) . . ?
O10 U1 O2 91.3(3) . . ?
O4 U1 O2 151.9(3) 6_566 . ?
O9 U1 O14 91.7(3) . . ?
O10 U1 O14 85.8(3) . . ?
O4 U1 O14 136.4(2) 6_566 . ?
O2 U1 O14 71.7(2) . . ?
O9 U1 O15 91.4(3) . . ?
O10 U1 O15 87.7(3) . . ?
O4 U1 O15 71.1(2) 6_566 . ?
O2 U1 O15 137.0(2) . . ?
O14 U1 O15 65.3(2) . . ?
O9 U1 O16 91.9(3) . . ?
O10 U1 O16 90.2(3) . . ?
O4 U1 O16 75.8(3) 6_566 . ?
O2 U1 O16 76.2(3) . . ?
O14 U1 O16 147.5(2) . . ?
O15 U1 O16 146.8(2) . . ?
O12A U2A O11A 176.0(7) . . ?
O12A U2A O8 85.0(6) . 5_756 ?
O11A U2A O8 92.8(5) . 5_756 ?
O12A U2A O21 90.7(9) . . ?
O11A U2A O21 91.3(8) . . ?
O8 U2A O21 64.0(6) 5_756 . ?
O12A U2A O19 91.4(7) . . ?
O11A U2A O19 88.5(6) . . ?
O8 U2A O19 145.8(5) 5_756 . ?
O21 U2A O19 150.1(7) . . ?
O12A U2A O6 89.9(6) . . ?
O11A U2A O6 94.1(5) . . ?
O8 U2A O6 133.0(5) 5_756 . ?
O21 U2A O6 69.4(6) . . ?
O19 U2A O6 80.8(5) . . ?
O12A U2A O17 89.1(7) . . ?
O11A U2A O17 87.3(6) . . ?
O8 U2A O17 81.7(5) 5_756 . ?
O21 U2A O17 145.6(6) . . ?
O19 U2A O17 64.2(5) . . ?
O6 U2A O17 145.0(4) . . ?
O12B U2B O6 96.4(6) . 1_565 ?
O11B U2B O6 82.2(6) . 1_565 ?
O12B U2B O20 89.7(8) . . ?
O11B U2B O20 90.9(7) . . ?
O6 U2B O20 89.2(5) 1_565 . ?
O12B U2B O18 88.4(7) . . ?
O11B U2B O18 93.1(7) . . ?
O6 U2B O18 153.1(5) 1_565 . ?
O20 U2B O18 64.3(5) . . ?
O12B U2B O22 85.4(12) . . ?
O11B U2B O22 93.4(11) . . ?
O6 U2B O22 59.9(10) 1_565 . ?
O20 U2B O22 147.8(10) . . ?
O18 U2B O22 147.0(10) . . ?
O12B U2B O8 89.2(6) . 5_766 ?
O11B U2B O8 91.2(6) . 5_766 ?
O6 U2B O8 128.6(5) 1_565 5_766 ?
O20 U2B O8 142.1(4) . 5_766 ?
O18 U2B O8 77.7(4) . 5_766 ?
O22 U2B O8 69.8(10) . 5_766 ?
O7 Gd O1 83.6(2) . . ?
O7 Gd O5 84.0(2) . . ?
O1 Gd O5 143.0(3) . . ?
O7 Gd O3 145.1(3) . . ?
O1 Gd O3 83.7(2) . . ?
O5 Gd O3 86.9(2) . . ?
O7 Gd O13 72.5(3) . . ?
O1 Gd O13 72.6(3) . . ?
O5 Gd O13 70.4(3) . . ?
O3 Gd O13 72.7(3) . . ?
O7 Gd N2 141.3(3) . . ?
O1 Gd N2 131.8(2) . . ?
O5 Gd N2 74.8(2) . . ?
O3 Gd N2 66.5(2) . . ?
O13 Gd N2 126.9(3) . . ?
O7 Gd N3 72.7(3) . . ?
O1 Gd N3 140.7(3) . . ?
O5 Gd N3 65.9(3) . . ?
O3 Gd N3 132.6(3) . . ?
O13 Gd N3 126.0(4) . . ?
N2 Gd N3 69.1(3) . . ?
O7 Gd N4 65.8(3) . . ?
O1 Gd N4 72.8(3) . . ?
O5 Gd N4 131.4(3) . . ?
O3 Gd N4 139.0(3) . . ?
O13 Gd N4 127.8(3) . . ?
N2 Gd N4 105.3(3) . . ?
N3 Gd N4 69.0(3) . . ?
O7 Gd N1 129.7(3) . . ?
O1 Gd N1 65.6(3) . . ?
O5 Gd N1 143.4(2) . . ?
O3 Gd N1 72.4(3) . . ?
O13 Gd N1 127.4(4) . . ?
N2 Gd N1 69.5(3) . . ?
N3 Gd N1 106.6(4) . . ?
N4 Gd N1 67.5(4) . . ?
C10 O1 Gd 125.6(6) . . ?
C10 O2 U1 125.9(6) . . ?
C12 O3 Gd 122.1(6) . . ?
C12 O4 U1 138.7(7) . 6_565 ?
C14 O5 Gd 123.4(8) . . ?
C14 O5 O24 132.2(10) . . ?
Gd O5 O24 103.2(7) . . ?
C14 O6 U2B 148.9(11) . 1_545 ?
C14 O6 U2A 157.9(11) . . ?
C16 O7 Gd 125.6(7) . . ?
C16 O8 U2A 133.2(9) . 5_756 ?
C16 O8 U2B 119.5(10) . 5_766 ?
Gd O13 O23 133.0(7) . . ?
Gd O13 O24 95.7(6) . . ?
O23 O13 O24 82.3(8) . . ?
C17 O14 U1 120.8(6) . . ?
C17 O15 U1 119.7(6) 7_656 . ?
U1 O16 H16A 127.0 . . ?
U1 O16 H16B 100.4 . . ?
H16A O16 H16B 99.5 . . ?
C18 O17 U2A 118.7(13) . . ?
C18 O18 U2B 118.4(13) . . ?
C19 O19 U2A 124.0(14) . . ?
C19 O20 U2B 122.8(14) . . ?
O13 O23 H23A 100.1 . . ?
O13 O23 H23B 89.2 . . ?
H23A O23 H23B 104.8 . . ?
C8 N1 C9 111.5(10) . . ?
C8 N1 C1 109.4(10) . . ?
C9 N1 C1 109.9(10) . . ?
C8 N1 Gd 111.4(8) . . ?
C9 N1 Gd 105.6(7) . . ?
C1 N1 Gd 109.0(6) . . ?
C11 N2 C2 110.2(9) . . ?
C11 N2 C3 108.7(7) . . ?
C2 N2 C3 109.8(8) . . ?
C11 N2 Gd 107.8(6) . . ?
C2 N2 Gd 110.4(6) . . ?
C3 N2 Gd 109.9(6) . . ?
C4 N3 C13 110.9(10) . . ?
C4 N3 C5 108.2(11) . . ?
C13 N3 C5 110.2(11) . . ?
C4 N3 Gd 110.7(8) . . ?
C13 N3 Gd 106.4(8) . . ?
C5 N3 Gd 110.5(8) . . ?
C15 N4 C6 108.6(10) . . ?
C15 N4 C7 109.5(9) . . ?
C6 N4 C7 110.7(11) . . ?
C15 N4 Gd 107.5(7) . . ?
C6 N4 Gd 109.0(7) . . ?
C7 N4 Gd 111.4(8) . . ?
N1 C1 C2 110.4(11) . . ?
N1 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N1 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N2 C2 C1 112.7(9) . . ?
N2 C2 H2A 109.1 . . ?
C1 C2 H2A 109.1 . . ?
N2 C2 H2B 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
N2 C3 C4 111.7(9) . . ?
N2 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
N2 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
N3 C4 C3 113.4(10) . . ?
N3 C4 H4A 108.9 . . ?
C3 C4 H4A 108.9 . . ?
N3 C4 H4B 108.9 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
C6 C5 N3 112.4(13) . . ?
C6 C5 H5A 109.1 . . ?
N3 C5 H5A 109.1 . . ?
C6 C5 H5B 109.1 . . ?
N3 C5 H5B 109.1 . . ?
H5A C5 H5B 107.8 . . ?
C5 C6 N4 113.6(12) . . ?
C5 C6 H6A 108.8 . . ?
N4 C6 H6A 108.8 . . ?
C5 C6 H6B 108.8 . . ?
N4 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
C8 C7 N4 110.5(10) . . ?
C8 C7 H7A 109.5 . . ?
N4 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
N1 C8 C7 113.1(10) . . ?
N1 C8 H8A 109.0 . . ?
C7 C8 H8A 109.0 . . ?
N1 C8 H8B 109.0 . . ?
C7 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
N1 C9 C10 111.2(10) . . ?
N1 C9 H9A 109.4 . . ?
C10 C9 H9A 109.4 . . ?
N1 C9 H9B 109.4 . . ?
C10 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
O2 C10 O1 123.9(9) . . ?
O2 C10 C9 117.8(9) . . ?
O1 C10 C9 118.3(9) . . ?
N2 C11 C12 111.4(8) . . ?
N2 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
N2 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
O3 C12 O4 122.9(10) . . ?
O3 C12 C11 118.6(9) . . ?
O4 C12 C11 118.3(9) . . ?
N3 C13 C14 113.8(10) . . ?
N3 C13 H13A 108.8 . . ?
C14 C13 H13A 108.8 . . ?
N3 C13 H13B 108.8 . . ?
C14 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
O5 C14 O6 124.5(14) . . ?
O5 C14 C13 117.8(11) . . ?
O6 C14 C13 117.5(12) . . ?
C16 C15 N4 112.6(9) . . ?
C16 C15 H15A 109.1 . . ?
N4 C15 H15A 109.1 . . ?
C16 C15 H15B 109.1 . . ?
N4 C15 H15B 109.1 . . ?
H15A C15 H15B 107.8 . . ?
O8 C16 O7 122.6(13) . . ?
O8 C16 C15 117.8(12) . . ?
O7 C16 C15 119.6(10) . . ?
O15 C17 O14 126.6(9) 7_656 . ?
O15 C17 C17 117.3(10) 7_656 7_656 ?
O14 C17 C17 116.1(11) . 7_656 ?
O18 C18 O17 125(2) . . ?
O18 C18 C19 117.1(18) . . ?
O17 C18 C19 117.4(17) . . ?
O20 C19 O19 127.9(19) . . ?
O20 C19 C18 116.7(19) . . ?
O19 C19 C18 115.4(18) . . ?

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
O16 H16A O17 0.98 1.76 2.591(17) 139.7 5_766
O23 H23A O11B 0.86 2.07 2.86(3) 154.4 5_766
O23 H23B O19 1.00 2.19 3.14(3) 156.4 .

#===END

data_4
_database_code_depnum_ccdc_archive 'CCDC 727653'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H27 Gd N4 O18 U2'
_chemical_formula_weight         1220.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 2/n'

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

_cell_length_a                   13.4846(13)
_cell_length_b                   6.6387(11)
_cell_length_c                   16.759(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.391(8)
_cell_angle_gamma                90.00
_cell_volume                     1396.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    61943
_cell_measurement_theta_min      3.07
_cell_measurement_theta_max      25.68

_exptl_crystal_description       platelet
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.902
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1110
_exptl_absorpt_coefficient_mu    14.001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.097
_exptl_absorpt_correction_T_max  0.326
_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 nine ω scans with 2° steps (543 frames)'
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            61943
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         25.68
_reflns_number_total             2637
_reflns_number_gt                2243
_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. The water solvent molecule was affected with
a 0.5 occupancy parameter in order to retain acceptable displacement
factors. The H atoms bound to O atoms were not found.
The C-bound H atoms were introduced at calculated positions and 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)+(0.1317P)²+43.3490P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0041(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2637
_refine_ls_number_parameters     201
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0802
_refine_ls_wR_factor_ref         0.2252
_refine_ls_wR_factor_gt          0.2183
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         4.709
_refine_diff_density_min         -5.085
_refine_diff_density_rms         0.378

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 0.74492(5) 0.48406(12) 0.61674(4) 0.0426(4) Uani 1 1 d . . .
Gd Gd 0.7500 0.7781(3) 0.2500 0.0508(5) Uani 1 2 d S . .
N1 N 0.7620(14) 1.002(3) 0.3776(9) 0.051(5) Uani 1 1 d . . .
N2 N 0.9150(14) 0.999(2) 0.2902(10) 0.048(4) Uani 1 1 d . . .
O1 O 0.8318(12) 0.618(3) 0.3841(8) 0.057(4) Uani 1 1 d . . .
O2 O 0.8260(12) 0.559(3) 0.5136(9) 0.069(5) Uani 1 1 d . . .
O3 O 0.8987(10) 0.616(2) 0.2377(8) 0.051(3) Uani 1 1 d . . .
O4 O 1.0688(13) 0.535(3) 0.3081(8) 0.061(4) Uani 1 1 d . . .
O5 O 0.7414(11) 0.219(3) 0.5912(9) 0.069(5) Uani 1 1 d . . .
O6 O 0.7453(12) 0.750(3) 0.6405(10) 0.068(5) Uani 1 1 d . . .
O7 O 0.6100(11) 0.532(2) 0.4732(9) 0.055(4) Uani 1 1 d . . .
O8 O 0.5610(11) 0.458(3) 0.6087(8) 0.060(4) Uani 1 1 d . . .
O9 O 0.7500 0.392(4) 0.7500 0.057(5) Uani 1 2 d S . .
O10 O 0.670(3) 1.012(4) 0.7253(18) 0.055(8) Uani 0.50 1 d P . .
C1 C 0.8698(16) 1.096(4) 0.4164(12) 0.051(5) Uani 1 1 d . . .
H1A H 0.9195 0.9978 0.4525 0.061 Uiso 1 1 calc R . .
H1B H 0.8664 1.2083 0.4521 0.061 Uiso 1 1 calc R . .
C2 C 0.9093(18) 1.168(4) 0.3481(13) 0.060(5) Uani 1 1 d . . .
H2A H 0.8618 1.2718 0.3142 0.072 Uiso 1 1 calc R . .
H2B H 0.9794 1.2272 0.3750 0.072 Uiso 1 1 calc R . .
C3 C 0.9246(16) 1.084(4) 0.2110(12) 0.056(5) Uani 1 1 d . . .
H3A H 0.9513 0.9801 0.1834 0.067 Uiso 1 1 calc R . .
H3B H 0.9768 1.1920 0.2273 0.067 Uiso 1 1 calc R . .
C4 C 0.8206(17) 1.167(4) 0.1462(13) 0.060(6) Uani 1 1 d . . .
H4A H 0.7961 1.2793 0.1709 0.072 Uiso 1 1 calc R . .
H4B H 0.8321 1.2135 0.0954 0.072 Uiso 1 1 calc R . .
C5 C 0.7426(16) 0.867(4) 0.4408(13) 0.055(5) Uani 1 1 d . . .
H5A H 0.6670 0.8384 0.4231 0.066 Uiso 1 1 calc R . .
H5B H 0.7655 0.9321 0.4964 0.066 Uiso 1 1 calc R . .
C6 C 0.8045(16) 0.669(4) 0.4474(12) 0.060(6) Uani 1 1 d . . .
C7 C 1.0094(18) 0.868(4) 0.3315(13) 0.062(6) Uani 1 1 d . . .
H7A H 1.0215 0.8529 0.3919 0.074 Uiso 1 1 calc R . .
H7B H 1.0721 0.9302 0.3266 0.074 Uiso 1 1 calc R . .
C8 C 0.9904(16) 0.663(3) 0.2881(11) 0.050(5) Uani 1 1 d . . .
C9 C 0.513(2) 0.520(3) 0.4606(14) 0.056(6) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U O6 1.808(19) . ?
U O5 1.81(2) . ?
U O9 2.292(7) . ?
U O4 2.367(16) 3_766 ?
U O2 2.409(15) . ?
U O8 2.441(14) . ?
U O7 2.451(13) . ?
Gd O3 2.351(14) . ?
Gd O3 2.351(14) 2_655 ?
Gd O1 2.364(14) . ?
Gd O1 2.364(14) 2_655 ?
Gd N2 2.541(17) 2_655 ?
Gd N2 2.541(17) . ?
Gd N1 2.559(16) . ?
Gd N1 2.559(16) 2_655 ?
N1 C5 1.48(3) . ?
N1 C1 1.50(3) . ?
N1 C4 1.51(3) 2_655 ?
N2 C7 1.48(3) . ?
N2 C3 1.49(3) . ?
N2 C2 1.51(3) . ?
O1 C6 1.29(2) . ?
O2 C6 1.27(3) . ?
O3 C8 1.26(2) . ?
O4 C8 1.30(3) . ?
O4 U 2.367(16) 3_766 ?
O7 C9 1.25(3) . ?
O8 C9 1.23(3) 3_666 ?
O9 U 2.292(7) 2_656 ?
C1 C2 1.51(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.53(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N1 1.51(3) 2_655 ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.54(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C7 C8 1.52(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C9 O8 1.23(3) 3_666 ?
C9 C9 1.51(4) 3_666 ?

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
O6 U O5 178.7(7) . . ?
O6 U O9 92.8(8) . . ?
O5 U O9 87.7(8) . . ?
O6 U O4 91.1(7) . 3_766 ?
O5 U O4 90.2(6) . 3_766 ?
O9 U O4 79.5(3) . 3_766 ?
O6 U O2 89.5(7) . . ?
O5 U O2 90.6(7) . . ?
O9 U O2 153.3(4) . . ?
O4 U O2 73.9(5) 3_766 . ?
O6 U O8 90.1(7) . . ?
O5 U O8 88.8(6) . . ?
O9 U O8 72.8(3) . . ?
O4 U O8 152.3(5) 3_766 . ?
O2 U O8 133.8(5) . . ?
O6 U O7 91.8(6) . . ?
O5 U O7 87.0(6) . . ?
O9 U O7 137.6(3) . . ?
O4 U O7 142.5(5) 3_766 . ?
O2 U O7 68.8(5) . . ?
O8 U O7 65.1(5) . . ?
O3 Gd O3 125.5(7) . 2_655 ?
O3 Gd O1 76.1(5) . . ?
O3 Gd O1 80.1(5) 2_655 . ?
O3 Gd O1 80.1(5) . 2_655 ?
O3 Gd O1 76.1(5) 2_655 2_655 ?
O1 Gd O1 126.6(8) . 2_655 ?
O3 Gd N2 159.0(5) . 2_655 ?
O3 Gd N2 66.1(5) 2_655 2_655 ?
O1 Gd N2 124.8(5) . 2_655 ?
O1 Gd N2 87.0(5) 2_655 2_655 ?
O3 Gd N2 66.1(5) . . ?
O3 Gd N2 159.0(5) 2_655 . ?
O1 Gd N2 87.0(5) . . ?
O1 Gd N2 124.8(5) 2_655 . ?
N2 Gd N2 109.6(8) 2_655 . ?
O3 Gd N1 122.9(5) . . ?
O3 Gd N1 89.3(5) 2_655 . ?
O1 Gd N1 66.5(5) . . ?
O1 Gd N1 157.0(5) 2_655 . ?
N2 Gd N1 70.7(5) 2_655 . ?
N2 Gd N1 70.3(5) . . ?
O3 Gd N1 89.3(5) . 2_655 ?
O3 Gd N1 122.9(5) 2_655 2_655 ?
O1 Gd N1 157.0(5) . 2_655 ?
O1 Gd N1 66.5(5) 2_655 2_655 ?
N2 Gd N1 70.3(5) 2_655 2_655 ?
N2 Gd N1 70.7(5) . 2_655 ?
N1 Gd N1 109.1(8) . 2_655 ?
C5 N1 C1 109.8(15) . . ?
C5 N1 C4 108.8(16) . 2_655 ?
C1 N1 C4 108.6(17) . 2_655 ?
C5 N1 Gd 105.9(12) . . ?
C1 N1 Gd 111.1(12) . . ?
C4 N1 Gd 112.6(11) 2_655 . ?
C7 N2 C3 107.4(17) . . ?
C7 N2 C2 111.8(16) . . ?
C3 N2 C2 109.3(17) . . ?
C7 N2 Gd 107.8(13) . . ?
C3 N2 Gd 109.6(12) . . ?
C2 N2 Gd 110.8(13) . . ?
C6 O1 Gd 119.4(14) . . ?
C6 O2 U 136.6(14) . . ?
C8 O3 Gd 119.3(13) . . ?
C8 O4 U 141.2(15) . 3_766 ?
C9 O7 U 121.0(13) . . ?
C9 O8 U 120.2(14) 3_666 . ?
U O9 U 149.1(12) . 2_656 ?
N1 C1 C2 111.1(16) . . ?
N1 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N2 C2 C1 111.5(19) . . ?
N2 C2 H2A 109.3 . . ?
C1 C2 H2A 109.3 . . ?
N2 C2 H2B 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
N2 C3 C4 114.4(17) . . ?
N2 C3 H3A 108.7 . . ?
C4 C3 H3A 108.7 . . ?
N2 C3 H3B 108.7 . . ?
C4 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
N1 C4 C3 109(2) 2_655 . ?
N1 C4 H4A 109.9 2_655 . ?
C3 C4 H4A 109.9 . . ?
N1 C4 H4B 109.9 2_655 . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
N1 C5 C6 109.5(16) . . ?
N1 C5 H5A 109.8 . . ?
C6 C5 H5A 109.8 . . ?
N1 C5 H5B 109.8 . . ?
C6 C5 H5B 109.8 . . ?
H5A C5 H5B 108.2 . . ?
O2 C6 O1 122(2) . . ?
O2 C6 C5 119.9(18) . . ?
O1 C6 C5 118(2) . . ?
N2 C7 C8 109.4(17) . . ?
N2 C7 H7A 109.8 . . ?
C8 C7 H7A 109.8 . . ?
N2 C7 H7B 109.8 . . ?
C8 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
O3 C8 O4 121(2) . . ?
O3 C8 C7 119.8(19) . . ?
O4 C8 C7 118.7(19) . . ?
O8 C9 O7 126(2) 3_666 . ?
O8 C9 C9 118(3) 3_666 3_666 ?
O7 C9 C9 115(3) . 3_666 ?


