# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2004

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

loop_
_publ_author_name
_publ_author_address
'Zhen-Tao Yu'
;     Department of Chemistry
Jilin University
Changchun, 130012
P. R. China
;
'Zuo-Lei Liao'
;     Department of Chemistry
Jilin University
Changchun, 130012
P. R. China
;
'Yu-Sheng Jiang'
;     Department of Chemistry
Jilin University
Changchun, 130012
P. R. China
;
'Guang-Hua Li'
;     Department of Chemistry
Jilin University
Changchun, 130012
P. R. China
;
;
Guo-Dong Li
;
;     Department of Chemistry
Jilin University
Changchun, 130012
P. R. China
;
'Jie-Sheng Chen'
;     Department of Chemistry
Jilin University
Changchun, 130012
P. R. China
;

_publ_contact_author_name        'ProfD Jie-Sheng Chen'
_publ_contact_author_address     
;
Changchun
CHINA
;

_publ_contact_author_email       CHEMCJ@MAIL.JLU.EDU.CN

_publ_section_title              
;
Construction of a Microporous Inorganic-Organic
Hybrid Compound with Uranyl Units
;
#============================================================
data_B406019A
_database_code_depnum_ccdc_archive 'CCDC 218126'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C19 H20 N3 Ni O16 U2.50'
_chemical_formula_sum            'C19 H20 N3 Ni O16 U2.50'
_chemical_formula_weight         1200.17

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'
Ni Ni 0.3393 1.1124 '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           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5466(2)
_cell_length_b                   10.8779(2)
_cell_length_c                   13.4741(3)
_cell_angle_alpha                89.1470(10)
_cell_angle_beta                 74.0720(10)
_cell_angle_gamma                80.1120(10)
_cell_volume                     1463.54(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1082
_exptl_absorpt_coefficient_mu    14.503
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.1725
_exptl_absorpt_correction_T_max  0.6486
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            7063
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4979
_reflns_number_gt                4579
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL

_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^)+(0.0641P)^2^+5.1898P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4979
_refine_ls_number_parameters     397
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0346
_refine_ls_wR_factor_ref         0.0958
_refine_ls_wR_factor_gt          0.0943
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.050
_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
U1 U 0.32979(3) 0.25184(2) 0.39469(2) 0.02220(11) Uani 1 1 d . . .
U2 U 0.5000 0.5000 0.5000 0.02563(13) Uani 1 2 d S . .
U3 U 0.55138(3) 0.13346(2) 0.55341(2) 0.01758(11) Uani 1 1 d . . .
Ni1 Ni 0.0000 0.0000 0.0000 0.0165(3) Uani 1 2 d S . .
Ni2 Ni 0.5000 0.0000 0.0000 0.0179(3) Uani 1 2 d S . .
O1 O 0.1873(5) 0.0186(5) 0.0033(4) 0.0238(12) Uani 1 1 d . . .
O2 O 0.3227(5) -0.0212(5) 0.1052(4) 0.0224(11) Uani 1 1 d . . .
O3 O 0.2305(6) 0.1078(5) 0.3190(5) 0.0356(15) Uani 1 1 d . . .
O4 O 0.2957(7) -0.0925(5) 0.3392(5) 0.0392(16) Uani 1 1 d . . .
O5 O 0.4554(7) 0.3097(5) 0.4870(5) 0.0372(16) Uani 1 1 d . . .
O6 O 0.4217(6) 0.0773(5) 0.4527(5) 0.0256(12) Uani 1 1 d . . .
O7 O 0.3342(8) 0.4816(6) 0.3884(6) 0.0480(19) Uani 1 1 d U . .
O8 O 0.4003(7) 0.6590(5) 0.3871(5) 0.0393(16) Uani 1 1 d . . .
O9 O 0.1886(7) 0.2720(6) 0.5081(5) 0.0394(16) Uani 1 1 d . . .
O10 O 0.4597(7) 0.2400(6) 0.2740(5) 0.0350(15) Uani 1 1 d . . .
O11 O 0.1469(7) 0.3580(6) 0.3113(5) 0.0405(16) Uani 1 1 d . . .
O12 O 0.6427(7) 0.4632(6) 0.3889(6) 0.0424(16) Uani 1 1 d . . .
O13 O 0.4119(6) 0.1466(6) 0.6675(5) 0.0334(14) Uani 1 1 d . . .
O14 O 0.6976(7) 0.1297(6) 0.4461(5) 0.0402(16) Uani 1 1 d . . .
O15 O 0.5630(6) 0.0424(6) 0.1265(4) 0.0301(13) Uani 1 1 d . . .
O1W O 0.8996(14) 0.2678(14) 0.3425(14) 0.058(4) Uani 0.50 1 d PU . .
O2W O 0.832(3) 0.613(3) 0.274(2) 0.048(7) Uani 0.25 1 d PU . .
O2W' O 0.915(3) 0.567(2) 0.3088(19) 0.038(6) Uani 0.25 1 d PU . .
N1 N -0.0179(6) -0.0318(5) 0.1542(5) 0.0173(13) Uani 1 1 d . . .
N2 N 0.5833(7) -0.1862(6) 0.0157(5) 0.0250(15) Uani 1 1 d . . .
N3 N 0.9251(7) -0.8045(6) 0.0356(5) 0.0264(15) Uani 1 1 d . . .
C1 C 0.0941(7) -0.0217(6) 0.1795(6) 0.0182(15) Uani 1 1 d . . .
C2 C 0.1033(8) -0.0314(6) 0.2807(6) 0.0187(15) Uani 1 1 d . . .
C3 C -0.0035(9) -0.0642(8) 0.3526(6) 0.0291(19) Uani 1 1 d . . .
H3 H 0.0016 -0.0772 0.4198 0.080 Uiso 1 1 calc . . .
C4 C -0.1204(9) -0.0788(8) 0.3277(6) 0.0272(18) Uani 1 1 d . . .
H4 H -0.1931 -0.1011 0.3767 0.080 Uiso 1 1 calc . . .
C5 C -0.1223(7) -0.0586(7) 0.2275(6) 0.0214(16) Uani 1 1 d . . .
H5 H -0.2005 -0.0639 0.2097 0.080 Uiso 1 1 calc . . .
C6 C 0.2117(7) -0.0048(7) 0.0898(6) 0.0198(16) Uani 1 1 d . . .
C7 C 0.2209(8) -0.0036(7) 0.3143(6) 0.0226(17) Uani 1 1 d . . .
C8 C 0.6619(9) -0.2546(8) -0.0674(6) 0.0300(19) Uani 1 1 d . . .
H8 H 0.6709 -0.2198 -0.1320 0.080 Uiso 1 1 calc . . .
C9 C 0.7297(10) -0.3727(8) -0.0626(7) 0.036(2) Uani 1 1 d . . .
H9 H 0.7848 -0.4150 -0.1226 0.080 Uiso 1 1 calc . . .
C10 C 0.7159(9) -0.4298(8) 0.0327(7) 0.0311(19) Uani 1 1 d . . .
C11 C 0.6351(11) -0.3591(9) 0.1198(7) 0.044(2) Uani 1 1 d . . .
H11 H 0.6246 -0.3916 0.1852 0.080 Uiso 1 1 calc . . .
C12 C 0.5704(10) -0.2395(8) 0.1077(7) 0.038(2) Uani 1 1 d . . .
H12 H 0.5154 -0.1942 0.1663 0.080 Uiso 1 1 calc . . .
C13 C 0.9761(9) -0.7203(8) -0.0311(7) 0.033(2) Uani 1 1 d . . .
H13 H 1.0593 -0.7453 -0.0783 0.080 Uiso 1 1 calc . . .
C14 C 0.9118(10) -0.5992(8) -0.0331(7) 0.035(2) Uani 1 1 d . . .
H14 H 0.9502 -0.5456 -0.0823 0.080 Uiso 1 1 calc . . .
C15 C 0.7883(9) -0.5569(8) 0.0389(7) 0.0305(19) Uani 1 1 d . . .
C16 C 0.7397(10) -0.6409(8) 0.1109(7) 0.037(2) Uani 1 1 d . . .
H16 H 0.6598 -0.6164 0.1619 0.080 Uiso 1 1 calc . . .
C17 C 0.8087(9) -0.7608(8) 0.1076(7) 0.034(2) Uani 1 1 d . . .
H17 H 0.7735 -0.8149 0.1576 0.080 Uiso 1 1 calc . . .
C18 C 0.3368(11) 0.5896(8) 0.3540(8) 0.042(2) Uani 1 1 d . . .
C19 C 0.2763(17) 0.6276(13) 0.2672(12) 0.076(4) Uani 1 1 d U . .
H19A H 0.2320 0.5629 0.2524 0.080 Uiso 1 1 calc . . .
H19B H 0.3456 0.6407 0.2069 0.080 Uiso 1 1 calc . . .
H19C H 0.2126 0.7035 0.2869 0.080 Uiso 1 1 calc . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
U1 0.0332(2) 0.01756(17) 0.02227(18) 0.00209(11) -0.01762(13) -0.00552(12)
U2 0.0395(3) 0.0153(2) 0.0304(2) 0.00145(16) -0.0226(2) -0.00600(17)
U3 0.02078(18) 0.01655(16) 0.01951(17) 0.00102(11) -0.01129(12) -0.00506(11)
Ni1 0.0126(6) 0.0234(7) 0.0153(6) 0.0017(5) -0.0071(5) -0.0031(5)
Ni2 0.0120(6) 0.0219(7) 0.0196(7) -0.0007(5) -0.0045(5) -0.0020(5)
O1 0.018(3) 0.040(3) 0.016(3) 0.004(2) -0.008(2) -0.007(2)
O2 0.011(3) 0.036(3) 0.022(3) 0.006(2) -0.007(2) -0.006(2)
O3 0.045(4) 0.024(3) 0.052(4) 0.001(3) -0.036(3) -0.007(3)
O4 0.047(4) 0.028(3) 0.062(4) 0.008(3) -0.044(4) -0.011(3)
O5 0.068(5) 0.015(3) 0.046(4) 0.003(2) -0.045(4) -0.007(3)
O6 0.033(3) 0.017(3) 0.036(3) 0.001(2) -0.024(3) -0.006(2)
O7 0.072(5) 0.027(3) 0.062(5) 0.008(3) -0.048(4) -0.008(3)
O8 0.068(5) 0.020(3) 0.048(4) 0.008(3) -0.044(4) -0.011(3)
O9 0.044(4) 0.038(4) 0.033(4) 0.006(3) -0.008(3) -0.001(3)
O10 0.043(4) 0.032(3) 0.033(3) 0.002(3) -0.011(3) -0.015(3)
O11 0.046(4) 0.041(4) 0.036(4) 0.012(3) -0.017(3) -0.004(3)
O12 0.048(4) 0.035(4) 0.044(4) 0.000(3) -0.013(3) -0.006(3)
O13 0.032(3) 0.040(4) 0.027(3) -0.002(3) -0.001(3) -0.013(3)
O14 0.033(4) 0.043(4) 0.040(4) 0.000(3) 0.002(3) -0.013(3)
O15 0.022(3) 0.043(3) 0.027(3) -0.007(3) -0.010(2) -0.005(3)
O1W 0.033(6) 0.047(7) 0.091(9) 0.026(6) -0.012(6) -0.011(5)
O2W 0.059(11) 0.045(10) 0.041(10) -0.001(8) -0.006(8) -0.021(8)
O2W' 0.037(9) 0.031(9) 0.032(9) -0.013(7) 0.013(7) -0.001(8)
N1 0.010(3) 0.022(3) 0.021(3) 0.002(2) -0.005(3) -0.004(2)
N2 0.024(4) 0.027(4) 0.022(4) -0.001(3) -0.006(3) 0.000(3)
N3 0.026(4) 0.028(4) 0.025(4) 0.003(3) -0.008(3) -0.002(3)
C1 0.016(4) 0.019(3) 0.021(4) -0.003(3) -0.008(3) -0.002(3)
C2 0.026(4) 0.014(3) 0.020(4) 0.001(3) -0.012(3) -0.004(3)
C3 0.031(5) 0.036(5) 0.021(4) 0.002(3) -0.010(4) -0.003(4)
C4 0.028(5) 0.035(4) 0.019(4) 0.005(3) -0.005(3) -0.010(4)
C5 0.015(4) 0.029(4) 0.020(4) 0.001(3) -0.003(3) -0.005(3)
C6 0.016(4) 0.021(4) 0.024(4) 0.001(3) -0.008(3) -0.006(3)
C7 0.026(4) 0.027(4) 0.021(4) -0.002(3) -0.013(3) -0.009(3)
C8 0.041(5) 0.031(4) 0.017(4) 0.001(3) -0.011(4) -0.002(4)
C9 0.046(6) 0.031(5) 0.025(4) -0.003(4) -0.008(4) 0.005(4)
C10 0.031(5) 0.026(4) 0.032(5) 0.007(3) -0.005(4) -0.001(4)
C11 0.062(7) 0.032(5) 0.025(5) 0.005(4) -0.001(5) 0.004(4)
C12 0.050(6) 0.033(5) 0.021(4) -0.002(4) -0.002(4) 0.004(4)
C13 0.028(5) 0.030(4) 0.036(5) -0.001(4) -0.002(4) -0.003(4)
C14 0.040(5) 0.023(4) 0.037(5) 0.000(4) -0.002(4) -0.005(4)
C15 0.035(5) 0.027(4) 0.029(4) 0.004(3) -0.008(4) -0.003(4)
C16 0.038(5) 0.031(5) 0.029(5) 0.003(4) 0.006(4) 0.005(4)
C17 0.037(5) 0.026(4) 0.033(5) 0.002(4) -0.006(4) 0.001(4)
C18 0.067(7) 0.018(4) 0.057(6) -0.001(4) -0.043(6) -0.009(4)
C19 0.103(8) 0.070(7) 0.087(8) 0.021(6) -0.068(7) -0.032(6)

_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 1.803(7) . ?
U1 O10 1.806(7) . ?
U1 O6 2.213(5) . ?
U1 O5 2.217(6) . ?
U1 O3 2.406(5) . ?
U1 O7 2.507(6) . ?
U1 O11 2.588(6) . ?
U1 U3 3.6498(4) . ?
U1 U2 3.9622(3) . ?
U2 O12 1.800(7) . ?
U2 O12 1.800(7) 2_666 ?
U2 O5 2.220(5) 2_666 ?
U2 O5 2.220(5) . ?
U2 O8 2.566(6) 2_666 ?
U2 O8 2.566(6) . ?
U2 O7 2.633(7) 2_666 ?
U2 O7 2.633(7) . ?
U2 C18 3.001(9) . ?
U2 C18 3.001(9) 2_666 ?
U2 U1 3.9622(3) 2_666 ?
U3 O14 1.796(6) . ?
U3 O13 1.800(6) . ?
U3 O6 2.261(5) 2_656 ?
U3 O5 2.297(5) . ?
U3 O6 2.326(5) . ?
U3 O4 2.431(6) 2_656 ?
U3 O8 2.584(6) 2_666 ?
U3 U3 3.7064(5) 2_656 ?
Ni1 O1 2.033(5) . ?
Ni1 O1 2.033(5) 2 ?
Ni1 N1 2.063(6) . ?
Ni1 N1 2.063(6) 2 ?
Ni1 N3 2.150(7) 1_465 ?
Ni1 N3 2.150(7) 2_645 ?
Ni2 O2 2.060(5) 2_655 ?
Ni2 O2 2.060(5) . ?
Ni2 O15 2.075(5) . ?
Ni2 O15 2.075(5) 2_655 ?
Ni2 N2 2.097(6) . ?
Ni2 N2 2.097(6) 2_655 ?
O1 C6 1.274(9) . ?
O2 C6 1.227(9) . ?
O3 C7 1.237(9) . ?
O4 C7 1.243(10) . ?
O4 U3 2.431(6) 2_656 ?
O6 U3 2.261(5) 2_656 ?
O7 C18 1.259(11) . ?
O8 C18 1.251(11) . ?
O8 U3 2.584(6) 2_666 ?
O2W O2W' 1.14(4) . ?
N1 C5 1.333(10) . ?
N1 C1 1.339(9) . ?
N2 C8 1.342(10) . ?
N2 C12 1.343(11) . ?
N3 C13 1.348(11) . ?
N3 C17 1.354(11) . ?
N3 Ni1 2.150(7) 1_645 ?
C1 C2 1.395(10) . ?
C1 C6 1.511(11) . ?
C2 C3 1.365(12) . ?
C2 C7 1.508(10) . ?
C3 C4 1.397(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.369(11) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C8 C9 1.369(12) . ?
C8 H8 0.9300 . ?
C9 C10 1.401(12) . ?
C9 H9 0.9300 . ?
C10 C11 1.395(13) . ?
C10 C15 1.473(11) . ?
C11 C12 1.391(13) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.378(12) . ?
C13 H13 0.9300 . ?
C14 C15 1.401(13) . ?
C14 H14 0.9300 . ?
C15 C16 1.378(12) . ?
C16 C17 1.375(12) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.499(15) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?

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 174.1(3) . . ?
O9 U1 O6 91.4(3) . . ?
O10 U1 O6 93.7(3) . . ?
O9 U1 O5 89.7(3) . . ?
O10 U1 O5 94.4(3) . . ?
O6 U1 O5 74.3(2) . . ?
O9 U1 O3 90.6(3) . . ?
O10 U1 O3 87.3(3) . . ?
O6 U1 O3 81.82(19) . . ?
O5 U1 O3 156.16(19) . . ?
O9 U1 O7 92.2(3) . . ?
O10 U1 O7 85.5(3) . . ?
O6 U1 O7 141.6(2) . . ?
O5 U1 O7 67.44(19) . . ?
O3 U1 O7 136.3(2) . . ?
O9 U1 O11 81.2(3) . . ?
O10 U1 O11 92.9(3) . . ?
O6 U1 O11 146.7(2) . . ?
O5 U1 O11 137.5(2) . . ?
O3 U1 O11 65.9(2) . . ?
O7 U1 O11 71.5(2) . . ?
O9 U1 U3 89.9(2) . . ?
O10 U1 U3 95.9(2) . . ?
O6 U1 U3 37.56(14) . . ?
O5 U1 U3 36.80(14) . . ?
O3 U1 U3 119.36(13) . . ?
O7 U1 U3 104.20(15) . . ?
O11 U1 U3 169.88(15) . . ?
O9 U1 U2 92.4(2) . . ?
O10 U1 U2 89.5(2) . . ?
O6 U1 U2 100.89(14) . . ?
O5 U1 U2 26.76(14) . . ?
O3 U1 U2 175.95(15) . . ?
O7 U1 U2 40.74(15) . . ?
O11 U1 U2 111.77(15) . . ?
U3 U1 U2 63.458(6) . . ?
O12 U2 O12 180.000(1) . 2_666 ?
O12 U2 O5 90.7(3) . 2_666 ?
O12 U2 O5 89.3(3) 2_666 2_666 ?
O12 U2 O5 89.3(3) . . ?
O12 U2 O5 90.7(3) 2_666 . ?
O5 U2 O5 180.000(1) 2_666 . ?
O12 U2 O8 93.7(3) . 2_666 ?
O12 U2 O8 86.3(3) 2_666 2_666 ?
O5 U2 O8 113.78(19) 2_666 2_666 ?
O5 U2 O8 66.22(19) . 2_666 ?
O12 U2 O8 86.3(3) . . ?
O12 U2 O8 93.7(3) 2_666 . ?
O5 U2 O8 66.22(19) 2_666 . ?
O5 U2 O8 113.78(19) . . ?
O8 U2 O8 180.0(2) 2_666 . ?
O12 U2 O7 88.6(3) . 2_666 ?
O12 U2 O7 91.4(3) 2_666 2_666 ?
O5 U2 O7 65.09(19) 2_666 2_666 ?
O5 U2 O7 114.91(19) . 2_666 ?
O8 U2 O7 49.06(19) 2_666 2_666 ?
O8 U2 O7 130.94(19) . 2_666 ?
O12 U2 O7 91.4(3) . . ?
O12 U2 O7 88.6(3) 2_666 . ?
O5 U2 O7 114.91(19) 2_666 . ?
O5 U2 O7 65.09(19) . . ?
O8 U2 O7 130.94(19) 2_666 . ?
O8 U2 O7 49.06(19) . . ?
O7 U2 O7 180.000(1) 2_666 . ?
O12 U2 C18 87.7(3) . . ?
O12 U2 C18 92.3(3) 2_666 . ?
O5 U2 C18 90.5(2) 2_666 . ?
O5 U2 C18 89.5(2) . . ?
O8 U2 C18 155.6(2) 2_666 . ?
O8 U2 C18 24.4(2) . . ?
O7 U2 C18 155.3(2) 2_666 . ?
O7 U2 C18 24.7(2) . . ?
O12 U2 C18 92.3(3) . 2_666 ?
O12 U2 C18 87.7(3) 2_666 2_666 ?
O5 U2 C18 89.5(2) 2_666 2_666 ?
O5 U2 C18 90.5(2) . 2_666 ?
O8 U2 C18 24.4(2) 2_666 2_666 ?
O8 U2 C18 155.6(2) . 2_666 ?
O7 U2 C18 24.7(2) 2_666 2_666 ?
O7 U2 C18 155.3(2) . 2_666 ?
C18 U2 C18 180.000(1) . 2_666 ?
O12 U2 U1 91.2(2) . 2_666 ?
O12 U2 U1 88.8(2) 2_666 2_666 ?
O5 U2 U1 26.72(15) 2_666 2_666 ?
O5 U2 U1 153.28(15) . 2_666 ?
O8 U2 U1 87.09(13) 2_666 2_666 ?
O8 U2 U1 92.91(13) . 2_666 ?
O7 U2 U1 38.42(13) 2_666 2_666 ?
O7 U2 U1 141.58(13) . 2_666 ?
C18 U2 U1 117.25(16) . 2_666 ?
C18 U2 U1 62.75(16) 2_666 2_666 ?
O12 U2 U1 88.8(2) . . ?
O12 U2 U1 91.2(2) 2_666 . ?
O5 U2 U1 153.28(15) 2_666 . ?
O5 U2 U1 26.72(15) . . ?
O8 U2 U1 92.91(13) 2_666 . ?
O8 U2 U1 87.09(13) . . ?
O7 U2 U1 141.58(13) 2_666 . ?
O7 U2 U1 38.42(13) . . ?
C18 U2 U1 62.75(16) . . ?
C18 U2 U1 117.25(16) 2_666 . ?
U1 U2 U1 180.0 2_666 . ?
O14 U3 O13 174.5(3) . . ?
O14 U3 O6 90.8(3) . 2_656 ?
O13 U3 O6 92.6(3) . 2_656 ?
O14 U3 O5 87.9(3) . . ?
O13 U3 O5 92.0(3) . . ?
O6 U3 O5 142.7(2) 2_656 . ?
O14 U3 O6 94.0(3) . . ?
O13 U3 O6 91.2(3) . . ?
O6 U3 O6 72.2(2) 2_656 . ?
O5 U3 O6 70.7(2) . . ?
O14 U3 O4 86.5(3) . 2_656 ?
O13 U3 O4 89.6(3) . 2_656 ?
O6 U3 O4 82.37(19) 2_656 2_656 ?
O5 U3 O4 134.6(2) . 2_656 ?
O6 U3 O4 154.59(19) . 2_656 ?
O14 U3 O8 87.3(3) . 2_666 ?
O13 U3 O8 87.6(3) . 2_666 ?
O6 U3 O8 152.23(19) 2_656 2_666 ?
O5 U3 O8 64.91(19) . 2_666 ?
O6 U3 O8 135.55(18) . 2_666 ?
O4 U3 O8 69.86(19) 2_656 2_666 ?
O14 U3 U1 91.8(2) . . ?
O13 U3 U1 91.3(2) . . ?
O6 U3 U1 107.61(13) 2_656 . ?
O5 U3 U1 35.32(14) . . ?
O6 U3 U1 35.43(13) . . ?
O4 U3 U1 169.92(14) 2_656 . ?
O8 U3 U1 100.14(13) 2_666 . ?
O14 U3 U3 93.0(2) . 2_656 ?
O13 U3 U3 92.4(2) . 2_656 ?
O6 U3 U3 36.71(13) 2_656 2_656 ?
O5 U3 U3 106.17(14) . 2_656 ?
O6 U3 U3 35.52(13) . 2_656 ?
O4 U3 U3 119.08(14) 2_656 2_656 ?
O8 U3 U3 171.07(13) 2_666 2_656 ?
U1 U3 U3 70.923(9) . 2_656 ?
O14 U3 U2 82.6(2) . . ?
O13 U3 U2 94.8(2) . . ?
O6 U3 U2 167.36(14) 2_656 . ?
O5 U3 U2 26.85(14) . . ?
O6 U3 U2 97.39(13) . . ?
O4 U3 U2 107.85(14) 2_656 . ?
O8 U3 U2 38.67(13) 2_666 . ?
U1 U3 U2 62.069(6) . . ?
U3 U3 U2 132.530(11) 2_656 . ?
O1 Ni1 O1 180.0 . 2 ?
O1 Ni1 N1 81.0(2) . . ?
O1 Ni1 N1 99.0(2) 2 . ?
O1 Ni1 N1 99.0(2) . 2 ?
O1 Ni1 N1 81.0(2) 2 2 ?
N1 Ni1 N1 180.0(3) . 2 ?
O1 Ni1 N3 92.1(2) . 1_465 ?
O1 Ni1 N3 87.9(2) 2 1_465 ?
N1 Ni1 N3 90.3(2) . 1_465 ?
N1 Ni1 N3 89.7(2) 2 1_465 ?
O1 Ni1 N3 87.9(2) . 2_645 ?
O1 Ni1 N3 92.1(2) 2 2_645 ?
N1 Ni1 N3 89.7(2) . 2_645 ?
N1 Ni1 N3 90.3(2) 2 2_645 ?
N3 Ni1 N3 180.0(4) 1_465 2_645 ?
O2 Ni2 O2 180.0(3) 2_655 . ?
O2 Ni2 O15 93.8(2) 2_655 . ?
O2 Ni2 O15 86.2(2) . . ?
O2 Ni2 O15 86.2(2) 2_655 2_655 ?
O2 Ni2 O15 93.8(2) . 2_655 ?
O15 Ni2 O15 180.0(3) . 2_655 ?
O2 Ni2 N2 89.1(2) 2_655 . ?
O2 Ni2 N2 90.9(2) . . ?
O15 Ni2 N2 86.7(2) . . ?
O15 Ni2 N2 93.3(2) 2_655 . ?
O2 Ni2 N2 90.9(2) 2_655 2_655 ?
O2 Ni2 N2 89.1(2) . 2_655 ?
O15 Ni2 N2 93.3(2) . 2_655 ?
O15 Ni2 N2 86.7(2) 2_655 2_655 ?
N2 Ni2 N2 180.0 . 2_655 ?
C6 O1 Ni1 114.4(5) . . ?
C6 O2 Ni2 126.4(5) . . ?
C7 O3 U1 143.1(5) . . ?
C7 O4 U3 139.6(5) . 2_656 ?
U1 O5 U2 126.5(3) . . ?
U1 O5 U3 107.9(2) . . ?
U2 O5 U3 125.3(3) . . ?
U1 O6 U3 145.1(3) . 2_656 ?
U1 O6 U3 107.0(2) . . ?
U3 O6 U3 107.8(2) 2_656 . ?
C18 O7 U1 160.4(7) . . ?
C18 O7 U2 94.2(5) . . ?
U1 O7 U2 100.8(2) . . ?
C18 O8 U2 97.7(5) . . ?
C18 O8 U3 156.5(6) . 2_666 ?
U2 O8 U3 102.4(2) . 2_666 ?
C5 N1 C1 118.7(6) . . ?
C5 N1 Ni1 129.3(5) . . ?
C1 N1 Ni1 111.9(5) . . ?
C8 N2 C12 116.9(7) . . ?
C8 N2 Ni2 120.0(5) . . ?
C12 N2 Ni2 122.9(5) . . ?
C13 N3 C17 115.8(7) . . ?
C13 N3 Ni1 119.0(5) . 1_645 ?
C17 N3 Ni1 123.3(6) . 1_645 ?
N1 C1 C2 122.5(7) . . ?
N1 C1 C6 115.1(6) . . ?
C2 C1 C6 122.4(7) . . ?
C3 C2 C1 116.8(7) . . ?
C3 C2 C7 119.4(7) . . ?
C1 C2 C7 123.8(7) . . ?
C2 C3 C4 121.7(7) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 H3 119.1 . . ?
C5 C4 C3 116.6(7) . . ?
C5 C4 H4 121.7 . . ?
C3 C4 H4 121.7 . . ?
N1 C5 C4 123.4(7) . . ?
N1 C5 H5 118.3 . . ?
C4 C5 H5 118.3 . . ?
O2 C6 O1 125.8(7) . . ?
O2 C6 C1 117.4(7) . . ?
O1 C6 C1 116.7(6) . . ?
O3 C7 O4 125.6(7) . . ?
O3 C7 C2 116.3(7) . . ?
O4 C7 C2 118.0(7) . . ?
N2 C8 C9 123.6(8) . . ?
N2 C8 H8 118.2 . . ?
C9 C8 H8 118.2 . . ?
C8 C9 C10 120.0(8) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C11 C10 C9 116.8(8) . . ?
C11 C10 C15 122.7(8) . . ?
C9 C10 C15 120.5(8) . . ?
C12 C11 C10 119.3(8) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
N2 C12 C11 123.3(8) . . ?
N2 C12 H12 118.3 . . ?
C11 C12 H12 118.3 . . ?
N3 C13 C14 123.5(8) . . ?
N3 C13 H13 118.2 . . ?
C14 C13 H13 118.2 . . ?
C13 C14 C15 119.9(8) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C16 C15 C14 116.5(8) . . ?
C16 C15 C10 123.6(8) . . ?
C14 C15 C10 119.8(8) . . ?
C17 C16 C15 120.4(8) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
N3 C17 C16 123.7(8) . . ?
N3 C17 H17 118.1 . . ?
C16 C17 H17 118.1 . . ?
O8 C18 O7 118.8(8) . . ?
O8 C18 C19 121.3(9) . . ?
O7 C18 C19 119.6(9) . . ?
O8 C18 U2 57.9(4) . . ?
O7 C18 U2 61.0(5) . . ?
C19 C18 U2 170.5(10) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.964
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.964
_refine_diff_density_max         2.842
_refine_diff_density_min         -1.942
_refine_diff_density_rms         0.253
#============================================================END