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

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Xian-He Bu'
_publ_contact_author_email       BUXH@NANKAI.EDU.CN

_publ_section_title              
;
Novel lanthanide-azido complexes: hydrothermal syntheses,
structures and magnetic properties
;
loop_
_publ_author_name
'Xian-He Bu'
'Bo-Wen Hu'
'Xin Hu'
'Fu-Chen Liu'
'Joan Ribas'
'Yong-Fei Zeng'
'Jiong-Peng Zhao'

# Attachment 'CIF.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 692690'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H18 Gd2 N6 O10'
_chemical_formula_weight         792.88

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'
Gd Gd -0.1653 3.9035 '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                   8.083(2)
_cell_length_b                   12.578(4)
_cell_length_c                   12.598(4)
_cell_angle_alpha                108.143(5)
_cell_angle_beta                 104.287(5)
_cell_angle_gamma                98.071(5)
_cell_volume                     1146.2(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1278
_cell_measurement_theta_min      3.2301
_cell_measurement_theta_max      23.2163

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             752
_exptl_absorpt_coefficient_mu    5.804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2226
_exptl_absorpt_correction_T_max  0.2933
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(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  'Bruker Smart APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            6158
_diffrn_reflns_av_R_equivalents  0.0854
_diffrn_reflns_av_sigmaI/netI    0.1261
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         25.50
_reflns_number_total             4163
_reflns_number_gt                2820
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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.
During the refinement, the command 'omit-3 51' was used to omit the poor
data above 51 degree. The command 'isor' was used to restrain the
lighter atoms (C, N) with ADP and NPD problems, which led to a relative
high restraint number 216.
All the pyridine groups were fixed with the "AFIX" command so as to get
the reasonable benzene ring.
The highest residual peak (3.717 eA3) is close to O10 and Gd1, but
featureless, which is probably due to the series termination errors.
;

_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^)+(0.0300P)^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         4163
_refine_ls_number_parameters     380
_refine_ls_number_restraints     216
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0550
_refine_ls_wR_factor_ref         0.1221
_refine_ls_wR_factor_gt          0.1140
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.016
_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
Gd1 Gd 0.03907(7) 0.85844(5) 0.40761(5) 0.01533(19) Uani 1 1 d . . .
Gd2 Gd 0.42170(7) 1.13027(5) 0.58061(5) 0.0170(2) Uani 1 1 d . . .
O1 O 0.2013(11) 0.7840(8) 0.5370(8) 0.028(2) Uani 1 1 d . B .
O2 O 0.4851(11) 0.7990(8) 0.5534(8) 0.036(3) Uani 1 1 d . . .
O3 O 0.5012(11) 1.0861(8) 0.7523(8) 0.030(2) Uani 1 1 d . . .
O4 O 0.4773(13) 1.2303(9) 0.9005(8) 0.039(3) Uani 1 1 d . . .
O5 O 0.6406(11) 1.2960(8) 0.7024(8) 0.040(3) Uani 1 1 d U A .
O6 O 0.9246(11) 1.3152(8) 0.7159(8) 0.033(2) Uani 1 1 d . . .
O1W O -0.0062(10) 0.8805(8) 0.2187(7) 0.025(2) Uani 1 1 d . . .
O7 O -0.2800(10) 0.7389(7) 0.2868(7) 0.025(2) Uani 1 1 d . . .
O9 O 0.1572(10) 1.0178(7) 0.5871(7) 0.019(2) Uani 1 1 d . . .
O10 O 0.3242(9) 0.9538(7) 0.4164(7) 0.018(2) Uani 1 1 d . . .
N4 N -0.1579(13) 0.8242(10) 0.5256(9) 0.028(3) Uani 1 1 d U . .
N5 N -0.1415(14) 0.7856(11) 0.6023(11) 0.035(3) Uani 1 1 d U . .
N6 N -0.1226(19) 0.7469(16) 0.6730(14) 0.076(5) Uani 1 1 d U . .
N2 N 0.8161(10) 1.0086(8) 1.1024(8) 0.042(3) Uani 1 1 d GU . .
C10 C 0.7524(11) 1.1032(8) 1.1422(7) 0.040(4) Uani 1 1 d GU . .
H10 H 0.7714 1.1390 1.2223 0.040 Uiso 1 1 calc R . .
C11 C 0.6610(11) 1.1454(8) 1.0647(7) 0.033(3) Uani 1 1 d GU . .
H11 H 0.6176 1.2099 1.0918 0.033 Uiso 1 1 calc R . .
C7 C 0.6332(10) 1.0929(8) 0.9473(7) 0.023(3) Uani 1 1 d GU . .
C8 C 0.6968(11) 0.9983(8) 0.9075(7) 0.032(3) Uani 1 1 d GU . .
H8 H 0.6778 0.9626 0.8274 0.032 Uiso 1 1 calc R . .
C9 C 0.7882(11) 0.9562(8) 0.9850(8) 0.038(3) Uani 1 1 d GU . .
H9 H 0.8316 0.8916 0.9579 0.038 Uiso 1 1 calc R . .
C12 C 0.5274(16) 1.1416(12) 0.8605(12) 0.026(3) Uani 1 1 d . . .
N3 N 0.890(3) 1.6747(17) 1.0193(17) 0.032(7) Uani 0.48(2) 1 d PGU A 1
C15 C 0.790(3) 1.5778(17) 1.0213(18) 0.042(9) Uani 0.48(2) 1 d PGU A 1
H15 H 0.7416 1.5831 1.0820 0.042 Uiso 0.48(2) 1 calc PR A 1
C14 C 0.761(3) 1.4730(18) 0.9335(17) 0.025(6) Uani 0.48(2) 1 d PGU A 1
H14 H 0.6936 1.4075 0.9348 0.025 Uiso 0.48(2) 1 calc PR A 1
C13 C 0.833(3) 1.4652(18) 0.8437(17) 0.025(6) Uani 0.48(2) 1 d PGU A 1
C16 C 0.933(3) 1.5621(18) 0.842(2) 0.029(6) Uani 0.48(2) 1 d PGU A 1
H16 H 0.9816 1.5568 0.7810 0.029 Uiso 0.48(2) 1 calc PR A 1
C17 C 0.962(3) 1.6669(18) 0.9295(19) 0.035(7) Uani 0.48(2) 1 d PGU A 1
H17 H 1.0295 1.7324 0.9282 0.035 Uiso 0.48(2) 1 calc PR A 1
N3A N 0.915(3) 1.6856(18) 1.0078(17) 0.046(8) Uani 0.52(2) 1 d PGU A 2
C15A C 0.747(3) 1.620(2) 0.9615(19) 0.060(12) Uani 0.52(2) 1 d PGU A 2
H15A H 0.6581 1.6485 0.9875 0.060 Uiso 0.52(2) 1 calc PR A 2
C14A C 0.710(3) 1.5143(19) 0.877(2) 0.046(8) Uani 0.52(2) 1 d PGU A 2
H14A H 0.5950 1.4698 0.8455 0.046 Uiso 0.52(2) 1 calc PR A 2
C13A C 0.840(2) 1.4734(18) 0.8393(17) 0.026(8) Uani 0.52(2) 1 d PGU A 2
C16A C 1.007(2) 1.5385(18) 0.8856(17) 0.034(7) Uani 0.52(2) 1 d PGU A 2
H16A H 1.0962 1.5104 0.8597 0.034 Uiso 0.52(2) 1 calc PR A 2
C17A C 1.045(3) 1.6446(16) 0.9699(17) 0.034(7) Uani 0.52(2) 1 d PGU A 2
H17A H 1.1593 1.6891 1.0016 0.034 Uiso 0.52(2) 1 calc PR A 2
C18 C 0.8007(17) 1.3503(11) 0.7456(11) 0.024(3) Uani 1 1 d . . .
N1 N 0.322(3) 0.4739(18) 0.6874(19) 0.037(7) Uani 0.440(16) 1 d PGU B 1
C3 C 0.172(3) 0.4864(18) 0.6184(19) 0.024(6) Uani 0.440(16) 1 d PGU B 1
H3 H 0.0672 0.4321 0.5955 0.024 Uiso 0.440(16) 1 calc PR B 1
C2 C 0.177(3) 0.5786(18) 0.5830(18) 0.020(6) Uani 0.440(16) 1 d PGU B 1
H2 H 0.0749 0.5871 0.5360 0.020 Uiso 0.440(16) 1 calc PR B 1
C1 C 0.331(2) 0.6582(18) 0.6166(17) 0.017(6) Uani 0.440(16) 1 d PGU B 1
C4 C 0.481(2) 0.6457(18) 0.6856(19) 0.029(7) Uani 0.440(16) 1 d PGU B 1
H4 H 0.5859 0.7000 0.7084 0.029 Uiso 0.440(16) 1 calc PR B 1
C5 C 0.476(2) 0.5536(18) 0.721(2) 0.036(7) Uani 0.440(16) 1 d PGU B 1
H5 H 0.5781 0.5450 0.7680 0.036 Uiso 0.440(16) 1 calc PR B 1
N1A N 0.332(3) 0.4559(16) 0.6555(17) 0.054(7) Uani 0.560(16) 1 d PGU B 2
C3A C 0.203(3) 0.5162(18) 0.6647(17) 0.048(6) Uani 0.560(16) 1 d PGU B 2
H3A H 0.1130 0.4924 0.6922 0.048 Uiso 0.560(16) 1 calc PR B 2
C2A C 0.207(2) 0.6119(17) 0.6332(17) 0.037(6) Uani 0.560(16) 1 d PGU B 2
H2A H 0.1204 0.6527 0.6394 0.037 Uiso 0.560(16) 1 calc PR B 2
C1A C 0.340(2) 0.6472(16) 0.5924(15) 0.028(6) Uani 0.560(16) 1 d PGU B 2
C4A C 0.469(2) 0.5869(17) 0.5832(17) 0.048(6) Uani 0.560(16) 1 d PGU B 2
H4A H 0.5590 0.6107 0.5557 0.048 Uiso 0.560(16) 1 calc PR B 2
C5A C 0.465(2) 0.4912(17) 0.6147(18) 0.052(7) Uani 0.560(16) 1 d PGU B 2
H5A H 0.5516 0.4505 0.6085 0.052 Uiso 0.560(16) 1 calc PR B 2
C6 C 0.3415(16) 0.7550(11) 0.5632(11) 0.020(3) Uani 1 1 d . . .

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
Gd1 0.0138(3) 0.0146(4) 0.0154(4) 0.0026(3) 0.0048(3) 0.0024(3)
Gd2 0.0128(3) 0.0149(4) 0.0189(4) 0.0019(3) 0.0035(3) 0.0014(3)
O1 0.033(5) 0.031(6) 0.041(6) 0.026(5) 0.022(4) 0.018(5)
O2 0.028(5) 0.037(6) 0.048(7) 0.022(5) 0.015(5) -0.003(5)
O3 0.024(5) 0.036(6) 0.027(6) 0.010(5) 0.006(4) 0.008(4)
O4 0.054(7) 0.039(7) 0.024(6) 0.006(5) 0.014(5) 0.021(5)
O5 0.020(5) 0.029(5) 0.047(6) -0.014(4) 0.009(4) -0.001(4)
O6 0.028(5) 0.030(6) 0.034(6) 0.002(5) 0.016(4) 0.000(5)
O1W 0.028(5) 0.029(6) 0.021(5) 0.011(4) 0.009(4) 0.006(4)
O7 0.024(5) 0.018(5) 0.026(5) 0.000(4) 0.007(4) 0.000(4)
O9 0.015(4) 0.022(5) 0.018(5) 0.005(4) 0.006(3) 0.001(4)
O10 0.008(4) 0.029(5) 0.016(5) 0.006(4) 0.005(3) 0.001(4)
N4 0.025(5) 0.037(6) 0.023(5) 0.009(5) 0.009(4) 0.009(5)
N5 0.022(5) 0.047(7) 0.037(6) 0.023(6) 0.004(5) 0.005(5)
N6 0.059(8) 0.098(9) 0.080(8) 0.059(8) 0.010(6) 0.010(7)
N2 0.035(7) 0.051(8) 0.042(6) 0.026(7) 0.007(6) 0.001(6)
C10 0.051(10) 0.043(9) 0.021(7) 0.015(6) 0.007(6) -0.004(7)
C11 0.037(8) 0.035(8) 0.025(7) 0.012(6) 0.011(6) 0.004(6)
C7 0.020(7) 0.032(8) 0.023(6) 0.016(6) 0.010(5) 0.003(5)
C8 0.032(8) 0.036(8) 0.035(7) 0.018(6) 0.010(6) 0.012(6)
C9 0.039(9) 0.040(9) 0.045(7) 0.027(7) 0.014(7) 0.011(7)
C12 0.016(7) 0.028(9) 0.034(9) 0.014(7) 0.010(6) -0.003(6)
N3 0.041(11) 0.029(8) 0.027(9) 0.009(7) 0.008(8) 0.011(7)
C15 0.06(2) 0.029(13) 0.042(19) 0.006(11) 0.030(17) 0.013(15)
C14 0.025(6) 0.025(6) 0.025(6) 0.009(2) 0.008(2) 0.0058(16)
C13 0.025(7) 0.025(7) 0.025(7) 0.009(3) 0.008(2) 0.0060(18)
C16 0.029(6) 0.029(6) 0.029(6) 0.010(2) 0.009(2) 0.0068(16)
C17 0.029(11) 0.031(8) 0.040(10) 0.005(7) 0.014(8) 0.002(7)
N3A 0.055(10) 0.040(10) 0.040(11) 0.015(7) 0.009(8) 0.012(7)
C15A 0.050(13) 0.06(2) 0.04(2) -0.016(16) 0.017(16) 0.020(14)
C14A 0.040(9) 0.048(10) 0.043(11) 0.000(7) 0.018(8) 0.016(8)
C13A 0.026(11) 0.029(15) 0.010(13) -0.003(10) -0.003(9) 0.009(8)
C16A 0.033(8) 0.035(10) 0.033(10) 0.014(7) 0.010(8) 0.004(7)
C17A 0.047(13) 0.029(13) 0.025(15) 0.017(9) 0.006(12) -0.004(11)
C18 0.032(8) 0.015(7) 0.027(8) 0.007(6) 0.012(6) 0.004(6)
N1 0.033(9) 0.036(10) 0.045(11) 0.019(8) 0.010(7) 0.007(7)
C3 0.027(8) 0.028(10) 0.021(10) 0.012(8) 0.013(7) 0.004(7)
C2 0.019(8) 0.023(9) 0.018(10) 0.005(8) 0.010(7) -0.002(7)
C1 0.017(6) 0.017(6) 0.017(6) 0.006(2) 0.005(2) 0.0041(17)
C4 0.022(8) 0.031(10) 0.035(11) 0.015(8) 0.004(7) 0.006(7)
C5 0.030(9) 0.035(10) 0.042(11) 0.019(8) 0.005(7) 0.011(7)
N1A 0.055(10) 0.046(10) 0.058(11) 0.022(8) 0.013(8) 0.011(7)
C3A 0.045(9) 0.051(10) 0.053(11) 0.026(8) 0.016(8) 0.005(7)
C2A 0.033(9) 0.036(9) 0.038(10) 0.007(8) 0.016(7) 0.004(7)
C1A 0.028(6) 0.028(6) 0.028(6) 0.010(2) 0.009(2) 0.0065(17)
C4A 0.045(9) 0.046(10) 0.057(11) 0.017(8) 0.022(8) 0.019(7)
C5A 0.051(9) 0.051(10) 0.060(12) 0.022(8) 0.018(8) 0.024(8)
C6 0.024(7) 0.017(7) 0.021(7) 0.002(6) 0.015(6) 0.008(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
Gd1 O1 2.345(9) . ?
Gd1 O6 2.359(10) 2_676 ?
Gd1 O9 2.369(8) . ?
Gd1 O9 2.373(9) 2_576 ?
Gd1 O10 2.403(7) . ?
Gd1 O1W 2.426(8) . ?
Gd1 N4 2.511(10) . ?
Gd1 O7 2.603(8) . ?
Gd1 Gd2 3.7845(14) 2_576 ?
Gd1 Gd1 3.8333(15) 2_576 ?
Gd1 Gd2 3.8819(12) . ?
Gd2 O5 2.337(8) . ?
Gd2 O3 2.359(9) . ?
Gd2 O2 2.363(9) 2_676 ?
Gd2 O10 2.382(8) . ?
Gd2 O9 2.426(7) . ?
Gd2 O10 2.436(8) 2_676 ?
Gd2 N4 2.465(11) 2_576 ?
Gd2 O7 2.564(9) 2_576 ?
Gd2 Gd1 3.7845(14) 2_576 ?
Gd2 Gd2 3.8412(15) 2_676 ?
O1 C6 1.238(15) . ?
O2 C6 1.266(13) . ?
O2 Gd2 2.363(9) 2_676 ?
O3 C12 1.270(15) . ?
O4 C12 1.242(17) . ?
O5 C18 1.269(14) . ?
O6 C18 1.242(15) . ?
O6 Gd1 2.359(10) 2_676 ?
O7 Gd2 2.564(9) 2_576 ?
O9 Gd1 2.373(9) 2_576 ?
O10 Gd2 2.436(8) 2_676 ?
N4 N5 1.197(15) . ?
N4 Gd2 2.465(11) 2_576 ?
N5 N6 1.132(17) . ?
N2 C9 1.363(5) . ?
N2 C10 1.364(5) . ?
C10 C11 1.363(5) . ?
C10 H10 0.9300 . ?
C11 C7 1.364(5) . ?
C11 H11 0.9300 . ?
C7 C8 1.363(5) . ?
C7 C12 1.550(16) . ?
C8 C9 1.364(5) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
N3 C15 1.376(14) . ?
N3 C17 1.376(14) . ?
C15 C14 1.376(14) . ?
C15 H15 0.9300 . ?
C14 C13 1.376(14) . ?
C14 H14 0.9300 . ?
C13 C16 1.376(14) . ?
C13 C18 1.52(2) . ?
C16 C17 1.376(14) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
N3A C15A 1.358(14) . ?
N3A C17A 1.358(14) . ?
C15A C14A 1.358(14) . ?
C15A H15A 0.9300 . ?
C14A C13A 1.358(14) . ?
C14A H14A 0.9300 . ?
C13A C16A 1.358(14) . ?
C13A C18 1.56(2) . ?
C16A C17A 1.358(14) . ?
C16A H16A 0.9300 . ?
C17A H17A 0.9300 . ?
N1 C3 1.365(14) . ?
N1 C5 1.365(14) . ?
C3 C2 1.365(14) . ?
C3 H3 0.9300 . ?
C2 C1 1.365(14) . ?
C2 H2 0.9300 . ?
C1 C4 1.365(14) . ?
C1 C6 1.56(2) . ?
C4 C5 1.365(14) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
N1A C3A 1.378(12) . ?
N1A C5A 1.378(12) . ?
C3A C2A 1.378(12) . ?
C3A H3A 0.9300 . ?
C2A C1A 1.378(12) . ?
C2A H2A 0.9300 . ?
C1A C4A 1.378(12) . ?
C1A C6 1.51(2) . ?
C4A C5A 1.378(12) . ?
C4A H4A 0.9300 . ?
C5A H5A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Gd1 O6 75.6(3) . 2_676 ?
O1 Gd1 O9 76.0(3) . . ?
O6 Gd1 O9 147.1(3) 2_676 . ?
O1 Gd1 O9 137.2(3) . 2_576 ?
O6 Gd1 O9 140.8(3) 2_676 2_576 ?
O9 Gd1 O9 72.1(3) . 2_576 ?
O1 Gd1 O10 83.7(3) . . ?
O6 Gd1 O10 89.3(3) 2_676 . ?
O9 Gd1 O10 71.4(3) . . ?
O9 Gd1 O10 111.5(3) 2_576 . ?
O1 Gd1 O1W 144.6(3) . . ?
O6 Gd1 O1W 75.7(3) 2_676 . ?
O9 Gd1 O1W 122.1(3) . . ?
O9 Gd1 O1W 77.8(3) 2_576 . ?
O10 Gd1 O1W 75.7(3) . . ?
O1 Gd1 N4 76.0(3) . . ?
O6 Gd1 N4 112.1(3) 2_676 . ?
O9 Gd1 N4 76.4(3) . . ?
O9 Gd1 N4 69.3(3) 2_576 . ?
O10 Gd1 N4 145.2(3) . . ?
O1W Gd1 N4 134.7(3) . . ?
O1 Gd1 O7 115.9(3) . . ?
O6 Gd1 O7 75.6(3) 2_676 . ?
O9 Gd1 O7 132.7(3) . . ?
O9 Gd1 O7 70.2(3) 2_576 . ?
O10 Gd1 O7 150.4(3) . . ?
O1W Gd1 O7 75.9(3) . . ?
N4 Gd1 O7 64.3(3) . . ?
O1 Gd1 Gd2 115.9(2) . 2_576 ?
O6 Gd1 Gd2 117.0(2) 2_676 2_576 ?
O9 Gd1 Gd2 90.37(19) . 2_576 ?
O9 Gd1 Gd2 38.45(18) 2_576 2_576 ?
O10 Gd1 Gd2 149.8(2) . 2_576 ?
O1W Gd1 Gd2 95.5(2) . 2_576 ?
N4 Gd1 Gd2 40.0(3) . 2_576 ?
O7 Gd1 Gd2 42.5(2) . 2_576 ?
O1 Gd1 Gd1 107.7(2) . 2_576 ?
O6 Gd1 Gd1 176.6(2) 2_676 2_576 ?
O9 Gd1 Gd1 36.1(2) . 2_576 ?
O9 Gd1 Gd1 36.03(18) 2_576 2_576 ?
O10 Gd1 Gd1 91.7(2) . 2_576 ?
O1W Gd1 Gd1 101.4(2) . 2_576 ?
N4 Gd1 Gd1 68.7(3) . 2_576 ?
O7 Gd1 Gd1 102.1(2) . 2_576 ?
Gd2 Gd1 Gd1 61.27(2) 2_576 2_576 ?
O1 Gd1 Gd2 82.8(2) . . ?
O6 Gd1 Gd2 122.9(2) 2_676 . ?
O9 Gd1 Gd2 36.45(18) . . ?
O9 Gd1 Gd2 87.99(18) 2_576 . ?
O10 Gd1 Gd2 35.6(2) . . ?
O1W Gd1 Gd2 95.82(19) . . ?
N4 Gd1 Gd2 112.8(2) . . ?
O7 Gd1 Gd2 157.8(2) . . ?
Gd2 Gd1 Gd2 120.01(2) 2_576 . ?
Gd1 Gd1 Gd2 58.75(2) 2_576 . ?
O5 Gd2 O3 80.4(3) . . ?
O5 Gd2 O2 76.6(3) . 2_676 ?
O3 Gd2 O2 147.7(3) . 2_676 ?
O5 Gd2 O10 149.8(3) . . ?
O3 Gd2 O10 107.8(3) . . ?
O2 Gd2 O10 82.7(3) 2_676 . ?
O5 Gd2 O9 138.3(3) . . ?
O3 Gd2 O9 73.3(3) . . ?
O2 Gd2 O9 138.0(3) 2_676 . ?
O10 Gd2 O9 70.7(3) . . ?
O5 Gd2 O10 81.6(3) . 2_676 ?
O3 Gd2 O10 71.1(3) . 2_676 ?
O2 Gd2 O10 83.2(3) 2_676 2_676 ?
O10 Gd2 O10 74.3(3) . 2_676 ?
O9 Gd2 O10 118.0(3) . 2_676 ?
O5 Gd2 N4 112.1(4) . 2_576 ?
O3 Gd2 N4 134.4(3) . 2_576 ?
O2 Gd2 N4 76.1(3) 2_676 2_576 ?
O10 Gd2 N4 83.4(3) . 2_576 ?
O9 Gd2 N4 69.2(3) . 2_576 ?
O10 Gd2 N4 151.3(3) 2_676 2_576 ?
O5 Gd2 O7 73.3(3) . 2_576 ?
O3 Gd2 O7 78.1(3) . 2_576 ?
O2 Gd2 O7 115.8(3) 2_676 2_576 ?
O10 Gd2 O7 136.4(2) . 2_576 ?
O9 Gd2 O7 70.1(3) . 2_576 ?
O10 Gd2 O7 142.9(3) 2_676 2_576 ?
N4 Gd2 O7 65.5(3) 2_576 2_576 ?
O5 Gd2 Gd1 115.7(2) . 2_576 ?
O3 Gd2 Gd1 93.6(2) . 2_576 ?
O2 Gd2 Gd1 116.8(2) 2_676 2_576 ?
O10 Gd2 Gd1 93.24(18) . 2_576 ?
O9 Gd2 Gd1 37.4(2) . 2_576 ?
O10 Gd2 Gd1 155.39(19) 2_676 2_576 ?
N4 Gd2 Gd1 40.9(2) 2_576 2_576 ?
O7 Gd2 Gd1 43.32(17) 2_576 2_576 ?
O5 Gd2 Gd2 116.3(2) . 2_676 ?
O3 Gd2 Gd2 89.1(2) . 2_676 ?
O2 Gd2 Gd2 81.1(3) 2_676 2_676 ?
O10 Gd2 Gd2 37.62(19) . 2_676 ?
O9 Gd2 Gd2 95.4(2) . 2_676 ?
O10 Gd2 Gd2 36.64(18) 2_676 2_676 ?
N4 Gd2 Gd2 119.0(3) 2_576 2_676 ?
O7 Gd2 Gd2 162.78(19) 2_576 2_676 ?
Gd1 Gd2 Gd2 127.71(3) 2_576 2_676 ?
O5 Gd2 Gd1 173.7(2) . . ?
O3 Gd2 Gd1 95.1(2) . . ?
O2 Gd2 Gd1 109.2(2) 2_676 . ?
O10 Gd2 Gd1 35.97(17) . . ?
O9 Gd2 Gd1 35.47(19) . . ?
O10 Gd2 Gd1 101.20(19) 2_676 . ?
N4 Gd2 Gd1 68.1(3) 2_576 . ?
O7 Gd2 Gd1 101.63(17) 2_576 . ?
Gd1 Gd2 Gd1 59.99(2) 2_576 . ?
Gd2 Gd2 Gd1 67.76(3) 2_676 . ?
C6 O1 Gd1 142.4(8) . . ?
C6 O2 Gd2 137.5(9) . 2_676 ?
C12 O3 Gd2 134.1(9) . . ?
C18 O5 Gd2 150.9(9) . . ?
C18 O6 Gd1 136.0(8) . 2_676 ?
Gd2 O7 Gd1 94.2(3) 2_576 . ?
Gd1 O9 Gd1 107.9(3) . 2_576 ?
Gd1 O9 Gd2 108.1(3) . . ?
Gd1 O9 Gd2 104.1(3) 2_576 . ?
Gd2 O10 Gd1 108.4(3) . . ?
Gd2 O10 Gd2 105.7(3) . 2_676 ?
Gd1 O10 Gd2 125.6(4) . 2_676 ?
N5 N4 Gd2 128.4(9) . 2_576 ?
N5 N4 Gd1 132.2(9) . . ?
Gd2 N4 Gd1 99.0(4) 2_576 . ?
N6 N5 N4 177.6(18) . . ?
C9 N2 C10 120.0 . . ?
C11 C10 N2 120.0 . . ?
C11 C10 H10 120.0 . . ?
N2 C10 H10 120.0 . . ?
C10 C11 C7 120.0 . . ?
C10 C11 H11 120.0 . . ?
C7 C11 H11 120.0 . . ?
C8 C7 C11 120.0 . . ?
C8 C7 C12 120.8(8) . . ?
C11 C7 C12 119.2(8) . . ?
C7 C8 C9 120.0 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
N2 C9 C8 120.0 . . ?
N2 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
O4 C12 O3 125.4(13) . . ?
O4 C12 C7 118.8(12) . . ?
O3 C12 C7 115.8(12) . . ?
C15 N3 C17 120.0 . . ?
N3 C15 C14 120.0 . . ?
N3 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C13 C14 C15 120.0 . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C16 C13 C14 120.0 . . ?
C16 C13 C18 119.5(13) . . ?
C14 C13 C18 120.5(13) . . ?
C13 C16 C17 120.0 . . ?
C13 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 N3 120.0 . . ?
C16 C17 H17 120.0 . . ?
N3 C17 H17 120.0 . . ?
C15A N3A C17A 120.0 . . ?
C14A C15A N3A 120.0 . . ?
C14A C15A H15A 120.0 . . ?
N3A C15A H15A 120.0 . . ?
C15A C14A C13A 120.0 . . ?
C15A C14A H14A 120.0 . . ?
C13A C14A H14A 120.0 . . ?
C14A C13A C16A 120.0 . . ?
C14A C13A C18 120.9(13) . . ?
C16A C13A C18 119.1(13) . . ?
C17A C16A C13A 120.0 . . ?
C17A C16A H16A 120.0 . . ?
C13A C16A H16A 120.0 . . ?
C16A C17A N3A 120.00(6) . . ?
C16A C17A H17A 120.0 . . ?
N3A C17A H17A 120.0 . . ?
O6 C18 O5 125.5(13) . . ?
O6 C18 C13 120.9(13) . . ?
O5 C18 C13 113.6(13) . . ?
O6 C18 C13A 118.6(12) . . ?
O5 C18 C13A 115.8(13) . . ?
C13 C18 C13A 5.0(12) . . ?
C3 N1 C5 120.0 . . ?
C2 C3 N1 120.0 . . ?
C2 C3 H3 120.0 . . ?
N1 C3 H3 120.0 . . ?
C1 C2 C3 120.0 . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C2 C1 C4 120.0 . . ?
C2 C1 C6 119.8(12) . . ?
C4 C1 C6 119.7(12) . . ?
C5 C4 C1 120.0 . . ?
C5 C4 H4 120.0 . . ?
C1 C4 H4 120.0 . . ?
C4 C5 N1 120.0 . . ?
C4 C5 H5 120.0 . . ?
N1 C5 H5 120.0 . . ?
C3A N1A C5A 120.0 . . ?
N1A C3A C2A 120.0 . . ?
N1A C3A H3A 120.0 . . ?
C2A C3A H3A 120.0 . . ?
C1A C2A C3A 120.0 . . ?
C1A C2A H2A 120.0 . . ?
C3A C2A H2A 120.0 . . ?
C4A C1A C2A 120.0 . . ?
C4A C1A C6 122.5(13) . . ?
C2A C1A C6 117.5(13) . . ?
C5A C4A C1A 120.0 . . ?
C5A C4A H4A 120.0 . . ?
C1A C4A H4A 120.0 . . ?
C4A C5A N1A 120.0 . . ?
C4A C5A H5A 120.0 . . ?
N1A C5A H5A 120.0 . . ?
O1 C6 O2 125.6(13) . . ?
O1 C6 C1A 118.8(12) . . ?
O2 C6 C1A 114.9(13) . . ?
O1 C6 C1 113.8(12) . . ?
O2 C6 C1 120.6(13) . . ?
C1A C6 C1 11.9(11) . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         3.717
_refine_diff_density_min         -1.862
_refine_diff_density_rms         0.294

#===END

data_2
_database_code_depnum_ccdc_archive 'CCDC 692691'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H18 Eu2 N6 O10'
_chemical_formula_weight         782.30

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'
Eu Eu -0.1578 3.6682 '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                   8.1279(9)
_cell_length_b                   12.5922(13)
_cell_length_c                   12.6120(13)
_cell_angle_alpha                108.094(2)
_cell_angle_beta                 104.365(2)
_cell_angle_gamma                98.055(2)
_cell_volume                     1155.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2170
_cell_measurement_theta_min      2.8203
_cell_measurement_theta_max      27.1607

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.32
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             748
_exptl_absorpt_coefficient_mu    5.447
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2252
_exptl_absorpt_correction_T_max  0.2746
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(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  'Bruker Smart APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            6328
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0850
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         25.50
_reflns_number_total             4209
_reflns_number_gt                3271
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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.
During the refinement, the command 'omit-3 51' was used to omit the poor
data above 51 degree. The command 'isor' was used to restrain the
lighter atoms (C, N) with ADP and NPD problems, which led to a relative
high restraint number 162.
All the pyridine groups were fixed with the "AFIX" command so as to get
the reasonable benzene ring.
The highest residual peak (1.837 eA3) is close to Eu1, but
featureless, which is probably due to the series termination errors.
;

_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^)+(0.0120P)^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         4209
_refine_ls_number_parameters     377
_refine_ls_number_restraints     162
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0376
_refine_ls_wR_factor_ref         0.0801
_refine_ls_wR_factor_gt          0.0754
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.003
_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
Eu1 Eu 0.03883(4) 0.85786(3) 0.40691(3) 0.01438(12) Uani 1 1 d . . .
Eu2 Eu 0.42219(4) 1.13061(3) 0.58073(3) 0.01618(12) Uani 1 1 d . . .
O1 O 0.2036(7) 0.7849(5) 0.5385(5) 0.0298(14) Uani 1 1 d . B .
O2 O 0.4839(7) 0.8002(5) 0.5538(5) 0.0339(16) Uani 1 1 d . . .
O3 O 0.4998(7) 1.0861(5) 0.7533(5) 0.0268(14) Uani 1 1 d . . .
O4 O 0.4772(8) 1.2292(5) 0.9021(5) 0.0368(16) Uani 1 1 d . . .
O5 O 0.6429(7) 1.2978(5) 0.7043(6) 0.0403(18) Uani 1 1 d . A .
O6 O 0.9221(6) 1.3194(5) 0.7164(5) 0.0266(14) Uani 1 1 d . . .
O1W O -0.0057(6) 0.8804(5) 0.2166(5) 0.0242(14) Uani 1 1 d . . .
O7 O -0.2802(6) 0.7388(4) 0.2866(4) 0.0207(13) Uani 1 1 d . . .
O9 O 0.1599(6) 1.0198(4) 0.5876(4) 0.0162(12) Uani 1 1 d . . .
O10 O 0.3238(6) 0.9532(4) 0.4159(4) 0.0146(12) Uani 1 1 d . . .
N4 N -0.1570(8) 0.8242(6) 0.5282(6) 0.0227(16) Uani 1 1 d U . .
N5 N -0.1399(8) 0.7870(7) 0.6035(7) 0.0344(19) Uani 1 1 d U . .
N6 N -0.1241(12) 0.7492(10) 0.6772(9) 0.073(3) Uani 1 1 d U . .
N2 N 0.8152(6) 1.0092(5) 1.1041(5) 0.0360(18) Uani 1 1 d GU . .
C10 C 0.7514(7) 1.1037(5) 1.1442(4) 0.037(2) Uani 1 1 d GU . .
H10 H 0.7698 1.1389 1.2241 0.037 Uiso 1 1 calc R . .
C11 C 0.6606(7) 1.1464(5) 1.0667(4) 0.030(2) Uani 1 1 d GU . .
H11 H 0.6172 1.2106 1.0939 0.030 Uiso 1 1 calc R . .
C7 C 0.6336(6) 1.0946(5) 0.9491(4) 0.0229(18) Uani 1 1 d GU . .
C8 C 0.6973(7) 1.0001(5) 0.9091(5) 0.034(2) Uani 1 1 d GU . .
H8 H 0.6790 0.9649 0.8291 0.034 Uiso 1 1 calc R . .
C9 C 0.7882(7) 0.9574(5) 0.9866(5) 0.041(2) Uani 1 1 d GU . .
H9 H 0.8316 0.8932 0.9593 0.041 Uiso 1 1 calc R . .
C12 C 0.5258(10) 1.1405(7) 0.8614(8) 0.025(2) Uani 1 1 d . . .
N3 N 0.8905(15) 1.6758(10) 1.0161(10) 0.032(5) Uani 0.487(17) 1 d PGU A 1
C15 C 0.7892(17) 1.5823(11) 1.0185(11) 0.032(5) Uani 0.487(17) 1 d PGU A 1
H15 H 0.7397 1.5893 1.0786 0.032 Uiso 0.487(17) 1 calc PR A 1
C14 C 0.7598(16) 1.4787(10) 0.9334(11) 0.027(5) Uani 0.487(17) 1 d PGU A 1
H14 H 0.6901 1.4144 0.9350 0.027 Uiso 0.487(17) 1 calc PR A 1
C13 C 0.8316(14) 1.4686(9) 0.8459(9) 0.013(5) Uani 0.487(17) 1 d PGU A 1
C17 C 0.9330(17) 1.5621(10) 0.8436(11) 0.026(5) Uani 0.487(17) 1 d PGU A 1
H17 H 0.9824 1.5551 0.7834 0.026 Uiso 0.487(17) 1 calc PR A 1
C16 C 0.9624(18) 1.6657(10) 0.9287(12) 0.031(5) Uani 0.487(17) 1 d PGU A 1
H16 H 1.0321 1.7300 0.9271 0.031 Uiso 0.487(17) 1 calc PR A 1
N3A N 0.9167(17) 1.6881(11) 1.0086(10) 0.049(6) Uani 0.513(17) 1 d PGU A 2
C15A C 0.7479(15) 1.6224(12) 0.9603(13) 0.047(6) Uani 0.513(17) 1 d PGU A 2
H15A H 0.6589 1.6501 0.9857 0.047 Uiso 0.513(17) 1 calc PR A 2
C14A C 0.7108(11) 1.5155(10) 0.8744(11) 0.043(6) Uani 0.513(17) 1 d PGU A 2
H14A H 0.5966 1.4711 0.8418 0.043 Uiso 0.513(17) 1 calc PR A 2
C13A C 0.8424(8) 1.4745(5) 0.8368(5) 0.025(6) Uani 0.513(17) 1 d PGU A 2
C17A C 1.0112(12) 1.5402(8) 0.8851(10) 0.028(4) Uani 0.513(17) 1 d PGU A 2
H17A H 1.1002 1.5124 0.8597 0.028 Uiso 0.513(17) 1 calc PR A 2
C16A C 1.0483(16) 1.6470(9) 0.9709(12) 0.041(5) Uani 0.513(17) 1 d PGU A 2
H16A H 1.1624 1.6915 1.0036 0.041 Uiso 0.513(17) 1 calc PR A 2
C18 C 0.7992(9) 1.3538(7) 0.7460(6) 0.0203(19) Uani 1 1 d GU . .
N1 N 0.3318(18) 0.4566(11) 0.6546(12) 0.032(4) Uani 0.501(11) 1 d PGU B 1
C3 C 0.2033(19) 0.5156(14) 0.6634(12) 0.023(4) Uani 0.501(11) 1 d PGU B 1
H3 H 0.1129 0.4904 0.6893 0.023 Uiso 0.501(11) 1 calc PR B 1
C2 C 0.208(2) 0.6119(14) 0.6341(13) 0.023(5) Uani 0.501(11) 1 d PGU B 1
H2 H 0.1208 0.6519 0.6401 0.023 Uiso 0.501(11) 1 calc PR B 1
C1 C 0.3412(19) 0.6491(13) 0.5960(13) 0.014(4) Uani 0.501(11) 1 d PGU B 1
C4 C 0.4697(15) 0.5901(12) 0.5872(12) 0.038(5) Uani 0.501(11) 1 d PGU B 1
H4 H 0.5601 0.6154 0.5613 0.038 Uiso 0.501(11) 1 calc PR B 1
C5 C 0.4650(15) 0.4939(11) 0.6165(13) 0.039(5) Uani 0.501(11) 1 d PGU B 1
H5 H 0.5522 0.4538 0.6105 0.039 Uiso 0.501(11) 1 calc PR B 1
N1A N 0.318(2) 0.4739(13) 0.6895(13) 0.045(5) Uani 0.499(11) 1 d PGU B 2
C3A C 0.173(2) 0.4876(14) 0.6195(13) 0.040(6) Uani 0.499(11) 1 d PGU B 2
H3A H 0.0671 0.4348 0.5964 0.040 Uiso 0.499(11) 1 calc PR B 2
C2A C 0.183(2) 0.5781(15) 0.5833(14) 0.034(6) Uani 0.499(11) 1 d PGU B 2
H2A H 0.0830 0.5876 0.5353 0.034 Uiso 0.499(11) 1 calc PR B 2
C1A C 0.337(2) 0.6550(13) 0.6170(13) 0.031(6) Uani 0.499(11) 1 d PGU B 2
C4A C 0.4820(17) 0.6413(13) 0.6869(13) 0.042(5) Uani 0.499(11) 1 d PGU B 2
H4A H 0.5881 0.6941 0.7101 0.042 Uiso 0.499(11) 1 calc PR B 2
C5A C 0.4725(16) 0.5507(12) 0.7232(13) 0.052(5) Uani 0.499(11) 1 d PGU B 2
H5A H 0.5721 0.5413 0.7712 0.052 Uiso 0.499(11) 1 calc PR B 2
C6 C 0.3435(10) 0.7552(7) 0.5634(7) 0.0204(18) Uani 1 1 d . . .

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
Eu1 0.0119(2) 0.0121(2) 0.0169(2) 0.00156(18) 0.00504(17) 0.00321(15)
Eu2 0.0109(2) 0.0135(2) 0.0199(3) 0.00121(19) 0.00392(17) 0.00260(16)
O1 0.033(3) 0.031(4) 0.039(4) 0.020(3) 0.019(3) 0.017(3)
O2 0.021(3) 0.035(4) 0.048(4) 0.021(3) 0.010(3) 0.001(3)
O3 0.028(3) 0.028(3) 0.020(3) 0.003(3) 0.007(3) 0.009(3)
O4 0.043(4) 0.034(4) 0.033(4) 0.011(3) 0.008(3) 0.018(3)
O5 0.018(3) 0.026(4) 0.054(4) -0.009(3) 0.007(3) -0.006(3)
O6 0.021(3) 0.021(3) 0.029(3) -0.005(3) 0.010(3) 0.003(2)
O1W 0.030(3) 0.023(3) 0.018(3) 0.004(3) 0.009(3) 0.008(2)
O7 0.017(3) 0.019(3) 0.020(3) 0.001(3) 0.002(2) 0.006(2)
O9 0.011(3) 0.011(3) 0.017(3) -0.006(2) 0.001(2) 0.004(2)
O10 0.009(2) 0.011(3) 0.018(3) 0.000(2) 0.000(2) 0.000(2)
N4 0.018(3) 0.034(4) 0.022(4) 0.014(3) 0.008(3) 0.010(3)
N5 0.014(3) 0.055(5) 0.038(5) 0.025(4) 0.007(3) 0.003(3)
N6 0.051(5) 0.113(7) 0.075(6) 0.065(6) 0.015(5) 0.013(5)
N2 0.023(4) 0.045(5) 0.046(4) 0.029(4) 0.008(4) 0.006(3)
C10 0.036(5) 0.046(6) 0.025(5) 0.013(4) 0.007(4) 0.004(4)
C11 0.028(5) 0.036(5) 0.021(5) 0.006(4) 0.008(4) 0.005(4)
C7 0.013(4) 0.025(4) 0.028(4) 0.011(4) 0.004(3) -0.003(3)
C8 0.034(5) 0.033(5) 0.037(5) 0.014(4) 0.012(4) 0.013(4)
C9 0.039(5) 0.037(6) 0.049(6) 0.016(5) 0.012(5) 0.019(4)
C12 0.023(4) 0.023(5) 0.028(5) 0.013(4) 0.004(4) -0.001(4)
N3 0.045(9) 0.022(7) 0.030(8) 0.006(6) 0.012(7) 0.015(6)
C15 0.052(12) 0.028(9) 0.022(11) 0.007(7) 0.025(9) 0.011(8)
C14 0.022(10) 0.037(9) 0.013(10) 0.000(7) 0.006(7) -0.001(8)
C13 0.011(8) 0.008(7) 0.013(8) -0.001(6) 0.000(6) 0.000(5)
C17 0.022(10) 0.016(8) 0.041(12) 0.007(7) 0.019(9) 0.002(7)
C16 0.022(8) 0.021(7) 0.045(8) 0.004(6) 0.014(7) -0.002(6)
N3A 0.058(8) 0.032(8) 0.049(10) 0.008(6) 0.007(7) 0.013(6)
C15A 0.063(9) 0.032(11) 0.053(15) 0.007(9) 0.038(11) 0.021(9)
C14A 0.029(9) 0.047(12) 0.038(13) -0.004(9) 0.006(9) 0.012(8)
C13A 0.027(8) 0.026(9) 0.024(9) 0.007(6) 0.010(7) 0.008(6)
C17A 0.031(8) 0.020(9) 0.025(10) 0.007(7) 0.006(8) -0.001(7)
C16A 0.050(8) 0.029(7) 0.038(9) 0.014(6) 0.004(7) 0.003(6)
C18 0.021(4) 0.025(4) 0.010(4) 0.002(3) 0.003(3) 0.005(3)
N1 0.040(7) 0.022(7) 0.033(8) 0.013(6) 0.006(6) 0.007(5)
C3 0.019(7) 0.027(8) 0.021(9) 0.011(7) 0.005(6) -0.007(6)
C2 0.024(11) 0.024(11) 0.031(14) 0.011(11) 0.020(10) 0.008(9)
C1 0.013(11) 0.022(12) 0.009(10) 0.008(9) 0.002(8) 0.000(7)
C4 0.027(7) 0.041(8) 0.053(9) 0.021(7) 0.019(7) 0.010(6)
C5 0.037(7) 0.039(8) 0.050(9) 0.021(7) 0.015(6) 0.023(6)
N1A 0.043(8) 0.048(9) 0.045(9) 0.021(7) 0.012(6) 0.005(6)
C3A 0.048(10) 0.035(13) 0.026(14) 0.007(11) 0.003(10) -0.006(10)
C2A 0.026(8) 0.028(13) 0.041(17) 0.004(11) 0.009(9) 0.007(8)
C1A 0.025(12) 0.024(13) 0.035(15) 0.001(11) 0.006(10) 0.009(8)
C4A 0.031(7) 0.048(8) 0.050(9) 0.026(7) 0.007(6) 0.006(6)
C5A 0.046(7) 0.057(9) 0.062(10) 0.034(7) 0.013(7) 0.014(6)
C6 0.027(5) 0.017(4) 0.015(4) 0.004(4) 0.006(4) 0.005(4)

_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
Eu1 O1 2.362(6) . ?
Eu1 O9 2.382(5) 2_576 ?
Eu1 O9 2.399(4) . ?
Eu1 O6 2.406(5) 2_676 ?
Eu1 O10 2.414(4) . ?
Eu1 O1W 2.448(6) . ?
Eu1 N4 2.544(6) . ?
Eu1 O7 2.611(5) . ?
Eu1 Eu2 3.8098(6) 2_576 ?
Eu1 Eu1 3.8567(8) 2_576 ?
Eu1 Eu2 3.9045(6) . ?
Eu1 Eu2 4.3250(7) 2_676 ?
Eu2 O2 2.365(6) 2_676 ?
Eu2 O5 2.366(5) . ?
Eu2 O3 2.372(6) . ?
Eu2 O10 2.396(4) . ?
Eu2 O9 2.415(5) . ?
Eu2 O10 2.444(5) 2_676 ?
Eu2 N4 2.493(7) 2_576 ?
Eu2 O7 2.572(5) 2_576 ?
Eu2 Eu1 3.8098(6) 2_576 ?
Eu2 Eu2 3.8534(8) 2_676 ?
Eu2 Eu1 4.3250(7) 2_676 ?
O1 C6 1.244(9) . ?
O2 C6 1.253(9) . ?
O2 Eu2 2.365(6) 2_676 ?
O3 C12 1.268(9) . ?
O4 C12 1.239(10) . ?
O5 C18 1.255(8) . ?
O6 C18 1.237(8) . ?
O6 Eu1 2.406(5) 2_676 ?
O7 Eu2 2.572(5) 2_576 ?
O9 Eu1 2.382(5) 2_576 ?
O10 Eu2 2.444(5) 2_676 ?
N4 N5 1.171(10) . ?
N4 Eu2 2.493(7) 2_576 ?
N5 N6 1.158(12) . ?
N2 C9 1.367(3) . ?
N2 C10 1.367(3) . ?
C10 C11 1.367(3) . ?
C10 H10 0.9300 . ?
C11 C7 1.367(3) . ?
C11 H11 0.9300 . ?
C7 C8 1.367(3) . ?
C7 C12 1.544(10) . ?
C8 C9 1.367(3) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
N3 C15 1.352(7) . ?
N3 C16 1.352(7) . ?
C15 C14 1.352(7) . ?
C15 H15 0.9300 . ?
C14 C13 1.352(7) . ?
C14 H14 0.9300 . ?
C13 C17 1.352(7) . ?
C13 C18 1.531(13) . ?
C17 C16 1.352(7) . ?
C17 H17 0.9300 . ?
C16 H16 0.9300 . ?
N3A C15A 1.376(5) . ?
N3A C16A 1.376(5) . ?
C15A C14A 1.376(5) . ?
C15A H15A 0.9300 . ?
C14A C13A 1.376(5) . ?
C14A H14A 0.9300 . ?
C13A C17A 1.376(5) . ?
C13A C18 1.521(5) . ?
C17A C16A 1.376(5) . ?
C17A H17A 0.9300 . ?
C16A H16A 0.9300 . ?
N1 C3 1.371(9) . ?
N1 C5 1.371(9) . ?
C3 C2 1.371(9) . ?
C3 H3 0.9300 . ?
C2 C1 1.371(9) . ?
C2 H2 0.9300 . ?
C1 C4 1.371(9) . ?
C1 C6 1.513(17) . ?
C4 C5 1.371(9) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
N1A C3A 1.353(10) . ?
N1A C5A 1.353(10) . ?
C3A C2A 1.353(10) . ?
C3A H3A 0.9300 . ?
C2A C1A 1.353(10) . ?
C2A H2A 0.9300 . ?
C1A C4A 1.353(10) . ?
C1A C6 1.607(18) . ?
C4A C5A 1.353(10) . ?
C4A H4A 0.9300 . ?
C5A H5A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Eu1 O9 136.66(18) . 2_576 ?
O1 Eu1 O9 75.61(19) . . ?
O9 Eu1 O9 72.47(18) 2_576 . ?
O1 Eu1 O6 75.3(2) . 2_676 ?
O9 Eu1 O6 141.26(17) 2_576 2_676 ?
O9 Eu1 O6 146.26(17) . 2_676 ?
O1 Eu1 O10 83.12(18) . . ?
O9 Eu1 O10 112.36(17) 2_576 . ?
O9 Eu1 O10 70.86(15) . . ?
O6 Eu1 O10 89.06(16) 2_676 . ?
O1 Eu1 O1W 144.60(18) . . ?
O9 Eu1 O1W 78.27(17) 2_576 . ?
O9 Eu1 O1W 121.54(18) . . ?
O6 Eu1 O1W 76.44(19) 2_676 . ?
O10 Eu1 O1W 75.56(17) . . ?
O1 Eu1 N4 75.8(2) . . ?
O9 Eu1 N4 68.8(2) 2_576 . ?
O9 Eu1 N4 76.49(19) . . ?
O6 Eu1 N4 112.0(2) 2_676 . ?
O10 Eu1 N4 144.62(19) . . ?
O1W Eu1 N4 135.37(19) . . ?
O1 Eu1 O7 116.54(19) . . ?
O9 Eu1 O7 69.39(15) 2_576 . ?
O9 Eu1 O7 132.84(15) . . ?
O6 Eu1 O7 76.37(16) 2_676 . ?
O10 Eu1 O7 150.60(17) . . ?
O1W Eu1 O7 76.25(17) . . ?
N4 Eu1 O7 64.60(18) . . ?
O1 Eu1 Eu2 115.97(13) . 2_576 ?
O9 Eu1 Eu2 37.73(12) 2_576 2_576 ?
O9 Eu1 Eu2 90.67(11) . 2_576 ?
O6 Eu1 Eu2 117.38(12) 2_676 2_576 ?
O10 Eu1 Eu2 149.86(12) . 2_576 ?
O1W Eu1 Eu2 95.80(12) . 2_576 ?
N4 Eu1 Eu2 40.35(15) . 2_576 ?
O7 Eu1 Eu2 42.30(10) . 2_576 ?
O1 Eu1 Eu1 107.13(13) . 2_576 ?
O9 Eu1 Eu1 36.39(11) 2_576 2_576 ?
O9 Eu1 Eu1 36.09(11) . 2_576 ?
O6 Eu1 Eu1 177.54(14) 2_676 2_576 ?
O10 Eu1 Eu1 91.78(11) . 2_576 ?
O1W Eu1 Eu1 101.53(13) . 2_576 ?
N4 Eu1 Eu1 68.37(16) . 2_576 ?
O7 Eu1 Eu1 101.86(11) . 2_576 ?
Eu2 Eu1 Eu1 61.229(11) 2_576 2_576 ?
O1 Eu1 Eu2 82.17(14) . . ?
O9 Eu1 Eu2 88.66(11) 2_576 . ?
O9 Eu1 Eu2 35.95(12) . . ?
O6 Eu1 Eu2 122.55(12) 2_676 . ?
O10 Eu1 Eu2 35.59(11) . . ?
O1W Eu1 Eu2 95.67(12) . . ?
N4 Eu1 Eu2 112.30(15) . . ?
O7 Eu1 Eu2 157.64(12) . . ?
Eu2 Eu1 Eu2 120.023(12) 2_576 . ?
Eu1 Eu1 Eu2 58.793(12) 2_576 . ?
O1 Eu1 Eu2 62.97(13) . 2_676 ?
O9 Eu1 Eu2 139.59(12) 2_576 2_676 ?
O9 Eu1 Eu2 84.61(11) . 2_676 ?
O6 Eu1 Eu2 67.12(12) 2_676 2_676 ?
O10 Eu1 Eu2 27.25(12) . 2_676 ?
O1W Eu1 Eu2 86.59(12) . 2_676 ?
N4 Eu1 Eu2 137.82(15) . 2_676 ?
O7 Eu1 Eu2 142.42(11) . 2_676 ?
Eu2 Eu1 Eu2 175.278(14) 2_576 2_676 ?
Eu1 Eu1 Eu2 114.325(14) 2_576 2_676 ?
Eu2 Eu1 Eu2 55.558(11) . 2_676 ?
O2 Eu2 O5 77.0(2) 2_676 . ?
O2 Eu2 O3 147.81(19) 2_676 . ?
O5 Eu2 O3 80.4(2) . . ?
O2 Eu2 O10 82.39(19) 2_676 . ?
O5 Eu2 O10 149.92(18) . . ?
O3 Eu2 O10 107.80(19) . . ?
O2 Eu2 O9 138.11(18) 2_676 . ?
O5 Eu2 O9 137.96(19) . . ?
O3 Eu2 O9 72.97(18) . . ?
O10 Eu2 O9 70.89(15) . . ?
O2 Eu2 O10 82.66(19) 2_676 2_676 ?
O5 Eu2 O10 81.33(18) . 2_676 ?
O3 Eu2 O10 71.48(17) . 2_676 ?
O10 Eu2 O10 74.47(16) . 2_676 ?
O9 Eu2 O10 118.44(17) . 2_676 ?
O2 Eu2 N4 76.2(2) 2_676 2_576 ?
O5 Eu2 N4 112.4(2) . 2_576 ?
O3 Eu2 N4 134.3(2) . 2_576 ?
O10 Eu2 N4 83.01(19) . 2_576 ?
O9 Eu2 N4 69.2(2) . 2_576 ?
O10 Eu2 N4 150.89(19) 2_676 2_576 ?
O2 Eu2 O7 116.5(2) 2_676 2_576 ?
O5 Eu2 O7 73.42(18) . 2_576 ?
O3 Eu2 O7 77.71(18) . 2_576 ?
O10 Eu2 O7 136.17(15) . 2_576 ?
O9 Eu2 O7 69.58(16) . 2_576 ?
O10 Eu2 O7 142.85(16) 2_676 2_576 ?
N4 Eu2 O7 65.89(19) 2_576 2_576 ?
O2 Eu2 Eu1 117.27(14) 2_676 2_576 ?
O5 Eu2 Eu1 115.63(14) . 2_576 ?
O3 Eu2 Eu1 93.08(13) . 2_576 ?
O10 Eu2 Eu1 93.20(10) . 2_576 ?
O9 Eu2 Eu1 37.12(12) . 2_576 ?
O10 Eu2 Eu1 155.46(12) 2_676 2_576 ?
N4 Eu2 Eu1 41.37(15) 2_576 2_576 ?
O7 Eu2 Eu1 43.09(11) 2_576 2_576 ?
O2 Eu2 Eu2 80.60(15) 2_676 2_676 ?
O5 Eu2 Eu2 116.27(14) . 2_676 ?
O3 Eu2 Eu2 89.35(13) . 2_676 ?
O10 Eu2 Eu2 37.66(11) . 2_676 ?
O9 Eu2 Eu2 95.65(11) . 2_676 ?
O10 Eu2 Eu2 36.81(10) 2_676 2_676 ?
N4 Eu2 Eu2 118.58(15) 2_576 2_676 ?
O7 Eu2 Eu2 162.57(13) 2_576 2_676 ?
Eu1 Eu2 Eu2 127.704(15) 2_576 2_676 ?
O2 Eu2 Eu1 109.05(14) 2_676 . ?
O5 Eu2 Eu1 173.56(16) . . ?
O3 Eu2 Eu1 94.89(13) . . ?
O10 Eu2 Eu1 35.88(11) . . ?
O9 Eu2 Eu1 35.67(11) . . ?
O10 Eu2 Eu1 101.40(11) 2_676 . ?
N4 Eu2 Eu1 67.83(16) 2_576 . ?
O7 Eu2 Eu1 101.40(11) 2_576 . ?
Eu1 Eu2 Eu1 59.977(12) 2_576 . ?
Eu2 Eu2 Eu1 67.761(13) 2_676 . ?
O2 Eu2 Eu1 63.88(14) 2_676 2_676 ?
O5 Eu2 Eu1 59.81(14) . 2_676 ?
O3 Eu2 Eu1 85.01(13) . 2_676 ?
O10 Eu2 Eu1 91.49(10) . 2_676 ?
O9 Eu2 Eu1 145.19(12) . 2_676 ?
O10 Eu2 Eu1 26.89(11) 2_676 2_676 ?
N4 Eu2 Eu1 140.07(16) 2_576 2_676 ?
O7 Eu2 Eu1 132.19(11) 2_576 2_676 ?
Eu1 Eu2 Eu1 175.278(14) 2_576 2_676 ?
Eu2 Eu2 Eu1 56.681(11) 2_676 2_676 ?
Eu1 Eu2 Eu1 124.442(11) . 2_676 ?
C6 O1 Eu1 142.0(5) . . ?
C6 O2 Eu2 138.1(5) . 2_676 ?
C12 O3 Eu2 134.8(6) . . ?
C18 O5 Eu2 152.0(5) . . ?
C18 O6 Eu1 136.1(5) . 2_676 ?
Eu2 O7 Eu1 94.62(15) 2_576 . ?
Eu1 O9 Eu1 107.53(18) 2_576 . ?
Eu1 O9 Eu2 105.1(2) 2_576 . ?
Eu1 O9 Eu2 108.38(18) . . ?
Eu2 O10 Eu1 108.53(18) . . ?
Eu2 O10 Eu2 105.53(16) . 2_676 ?
Eu1 O10 Eu2 125.9(2) . 2_676 ?
N5 N4 Eu2 129.0(5) . 2_576 ?
N5 N4 Eu1 132.2(6) . . ?
Eu2 N4 Eu1 98.3(2) 2_576 . ?
N6 N5 N4 179.3(11) . . ?
C9 N2 C10 120.0 . . ?
C11 C10 N2 120.0 . . ?
C11 C10 H10 120.0 . . ?
N2 C10 H10 120.0 . . ?
C7 C11 C10 120.0 . . ?
C7 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C8 C7 C11 120.0 . . ?
C8 C7 C12 120.0(5) . . ?
C11 C7 C12 119.9(5) . . ?
C7 C8 C9 120.0 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C8 C9 N2 120.0 . . ?
C8 C9 H9 120.0 . . ?
N2 C9 H9 120.0 . . ?
O4 C12 O3 125.5(8) . . ?
O4 C12 C7 117.6(7) . . ?
O3 C12 C7 116.9(7) . . ?
C15 N3 C16 120.0 . . ?
N3 C15 C14 120.0 . . ?
N3 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C13 C14 C15 120.0 . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C17 C13 C14 120.0 . . ?
C17 C13 C18 117.9(8) . . ?
C14 C13 C18 122.1(8) . . ?
C13 C17 C16 120.0 . . ?
C13 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C16 N3 120.0 . . ?
C17 C16 H16 120.0 . . ?
N3 C16 H16 120.0 . . ?
C15A N3A C16A 120.0 . . ?
C14A C15A N3A 120.0 . . ?
C14A C15A H15A 120.0 . . ?
N3A C15A H15A 120.0 . . ?
C15A C14A C13A 120.0 . . ?
C15A C14A H14A 120.0 . . ?
C13A C14A H14A 120.0 . . ?
C17A C13A C14A 120.0 . . ?
C17A C13A C18 121.0 . . ?
C14A C13A C18 118.9 . . ?
C13A C17A C16A 120.0 . . ?
C13A C17A H17A 120.0 . . ?
C16A C17A H17A 120.0 . . ?
C17A C16A N3A 120.0 . . ?
C17A C16A H16A 120.0 . . ?
N3A C16A H16A 120.0 . . ?
O6 C18 O5 124.8(7) . . ?
O6 C18 C13A 116.8(5) . . ?
O5 C18 C13A 118.4(5) . . ?
O6 C18 C13 120.8(7) . . ?
O5 C18 C13 114.3(7) . . ?
C13A C18 C13 7.0(5) . . ?
C3 N1 C5 120.0 . . ?
C2 C3 N1 120.0 . . ?
C2 C3 H3 120.0 . . ?
N1 C3 H3 120.0 . . ?
C1 C2 C3 120.0 . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C1 C2 120.0 . . ?
C4 C1 C6 120.8(10) . . ?
C2 C1 C6 119.2(10) . . ?
C5 C4 C1 120.0 . . ?
C5 C4 H4 120.0 . . ?
C1 C4 H4 120.0 . . ?
C4 C5 N1 120.0 . . ?
C4 C5 H5 120.0 . . ?
N1 C5 H5 120.0 . . ?
C3A N1A C5A 120.0 . . ?
N1A C3A C2A 120.0 . . ?
N1A C3A H3A 120.0 . . ?
C2A C3A H3A 120.0 . . ?
C1A C2A C3A 120.0 . . ?
C1A C2A H2A 120.0 . . ?
C3A C2A H2A 120.0 . . ?
C2A C1A C4A 120.0 . . ?
C2A C1A C6 117.7(10) . . ?
C4A C1A C6 122.1(10) . . ?
C5A C4A C1A 120.0 . . ?
C5A C4A H4A 120.0 . . ?
C1A C4A H4A 120.0 . . ?
C4A C5A N1A 120.0 . . ?
C4A C5A H5A 120.0 . . ?
N1A C5A H5A 120.0 . . ?
O1 C6 O2 125.0(8) . . ?
O1 C6 C1 118.0(8) . . ?
O2 C6 C1 116.7(9) . . ?
O1 C6 C1A 114.8(9) . . ?
O2 C6 C1A 120.1(9) . . ?
C1 C6 C1A 9.1(9) . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         1.837
_refine_diff_density_min         -1.179
_refine_diff_density_rms         0.192

#===END

data_3
_database_code_depnum_ccdc_archive 'CCDC 692692'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H18 N6 O10 Sm2'
_chemical_formula_weight         779.08

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'
Sm Sm -0.1638 3.4418 '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                   8.1650(5)
_cell_length_b                   12.5991(8)
_cell_length_c                   12.6299(8)
_cell_angle_alpha                108.0220(10)
_cell_angle_beta                 104.4420(10)
_cell_angle_gamma                98.0800(10)
_cell_volume                     1162.55(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4626
_cell_measurement_theta_min      2.81
_cell_measurement_theta_max      26.32

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             744
_exptl_absorpt_coefficient_mu    5.068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2700
_exptl_absorpt_correction_T_max  0.3311
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(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  'Bruker Smart APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            6288
_diffrn_reflns_av_R_equivalents  0.1306
_diffrn_reflns_av_sigmaI/netI    0.0792
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         25.50
_reflns_number_total             4227
_reflns_number_gt                3858
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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.
During the data collection, the precision of diffraction data is a little
poor because the quality of the single crystal is limited, leading to the
high Rint value (0.1306).
During the refinement, the command 'omit-3 51' was used to omit the poor
data above 51 degree. The command 'isor' was used to restrain the
lighter atoms (C, N) with ADP and NPD problems, which led to a relative
high restraint number 100.
The C13 and C13A atoms were just isotropically refined with fixed thermal
parameters because of their NPD problems during the anisotropically
refinement. The fixed thermal parameters are 1.2 times larger than the
normal C thermal parameters.
All the pyridine groups were fixed with the "AFIX" command so as to get
the reasonable benzene ring.
The highest residual peak (2.716 eA3) is close to Sm1, but
featureless, which is probably due to the series termination errors.
;

_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^)+(0.1000P)^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         4227
_refine_ls_number_parameters     368
_refine_ls_number_restraints     100
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1346
_refine_ls_wR_factor_gt          0.1314
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.021
_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
Sm1 Sm 0.03863(4) 0.85745(2) 0.40635(2) 0.01379(15) Uani 1 1 d . . .
Sm2 Sm 0.42277(4) 1.13103(3) 0.58107(3) 0.01568(15) Uani 1 1 d . . .
O1 O 0.2038(6) 0.7846(4) 0.5390(4) 0.0286(11) Uani 1 1 d . B .
O2 O 0.4824(7) 0.7981(5) 0.5548(5) 0.0363(12) Uani 1 1 d . . .
O3 O 0.5015(7) 1.0875(4) 0.7547(4) 0.0295(11) Uani 1 1 d . . .
O4 O 0.4747(7) 1.2304(4) 0.9018(4) 0.0377(12) Uani 1 1 d . . .
O5 O 0.6447(6) 1.2989(4) 0.7057(5) 0.0384(13) Uani 1 1 d . A .
O6 O 0.9240(6) 1.3198(4) 0.7169(4) 0.0310(11) Uani 1 1 d . . .
O1W O -0.0059(6) 0.8798(4) 0.2163(4) 0.0246(10) Uani 1 1 d . . .
O7 O -0.2792(6) 0.7395(4) 0.2860(4) 0.0215(9) Uani 1 1 d . . .
O9 O 0.1576(5) 1.0196(4) 0.5872(4) 0.0168(9) Uani 1 1 d . . .
O10 O 0.3238(5) 0.9534(4) 0.4150(4) 0.0182(9) Uani 1 1 d . . .
N4 N -0.1569(7) 0.8234(5) 0.5286(5) 0.0249(12) Uani 1 1 d . . .
N5 N -0.1404(8) 0.7838(6) 0.6029(5) 0.0348(16) Uani 1 1 d . . .
N6 N -0.1223(12) 0.7475(9) 0.6761(8) 0.074(3) Uani 1 1 d U . .
N2 N 0.8157(6) 1.0103(4) 1.1056(4) 0.0380(15) Uani 1 1 d GU . .
C10 C 0.7520(7) 1.1051(4) 1.1451(4) 0.0389(17) Uani 1 1 d GU . .
H10 H 0.7706 1.1407 1.2249 0.039 Uiso 1 1 calc R . .
C11 C 0.6610(6) 1.1474(4) 1.0669(4) 0.0305(15) Uani 1 1 d GU . .
H11 H 0.6178 1.2116 1.0937 0.031 Uiso 1 1 calc R . .
C7 C 0.6336(6) 1.0948(4) 0.9492(4) 0.0261(14) Uani 1 1 d GU . .
C8 C 0.6973(7) 0.9999(4) 0.9097(4) 0.0338(16) Uani 1 1 d GU . .
H8 H 0.6787 0.9643 0.8299 0.034 Uiso 1 1 calc R . .
C9 C 0.7883(6) 0.9577(4) 0.9879(4) 0.0381(17) Uani 1 1 d GU . .
H9 H 0.8315 0.8934 0.9611 0.038 Uiso 1 1 calc R . .
C12 C 0.5270(9) 1.1422(6) 0.8628(6) 0.0241(14) Uani 1 1 d . . .
N3 N 0.9208(16) 1.6882(9) 1.0110(9) 0.040(4) Uani 0.501(15) 1 d PGU A 1
C15 C 1.0490(17) 1.6460(9) 0.9721(10) 0.043(4) Uani 0.501(15) 1 d PGU A 1
H15 H 1.1629 1.6899 1.0031 0.043 Uiso 0.501(15) 1 calc PR A 1
C14 C 1.0095(15) 1.5392(10) 0.8877(10) 0.036(4) Uani 0.501(15) 1 d PGU A 1
H14 H 1.0967 1.5105 0.8612 0.036 Uiso 0.501(15) 1 calc PR A 1
C13 C 0.8420(14) 1.4746(10) 0.8422(10) 0.044 Uiso 0.501(15) 1 d PGU A 1
C17 C 0.7138(14) 1.5168(10) 0.8811(11) 0.045(5) Uani 0.501(15) 1 d PGU A 1
H17 H 0.5999 1.4729 0.8501 0.045 Uiso 0.501(15) 1 calc PR A 1
C16 C 0.7532(14) 1.6236(11) 0.9655(10) 0.044(5) Uani 0.501(15) 1 d PGU A 1
H16 H 0.6661 1.6523 0.9920 0.044 Uiso 0.501(15) 1 calc PR A 1
N3A N 0.8877(15) 1.6768(8) 1.0178(9) 0.033(4) Uani 0.499(15) 1 d PGU A 2
C15A C 0.9632(16) 1.6684(8) 0.9318(10) 0.036(4) Uani 0.499(15) 1 d PGU A 2
H15A H 1.0320 1.7335 0.9313 0.036 Uiso 0.499(15) 1 calc PR A 2
C14A C 0.9379(17) 1.5647(8) 0.8466(11) 0.036(4) Uani 0.499(15) 1 d PGU A 2
H14A H 0.9895 1.5590 0.7878 0.036 Uiso 0.499(15) 1 calc PR A 2
C13A C 0.8372(16) 1.4694(8) 0.8473(10) 0.043 Uiso 0.499(15) 1 d PGU A 2
C17A C 0.7617(14) 1.4778(9) 0.9333(9) 0.027(3) Uani 0.499(15) 1 d PGU A 2
H17A H 0.6929 1.4127 0.9338 0.027 Uiso 0.499(15) 1 calc PR A 2
C16A C 0.7869(15) 1.5815(9) 1.0185(9) 0.036(4) Uani 0.499(15) 1 d PGU A 2
H16A H 0.7354 1.5872 1.0773 0.036 Uiso 0.499(15) 1 calc PR A 2
C18 C 0.7976(9) 1.3537(6) 0.7482(6) 0.0217(13) Uani 1 1 d . . .
N1 N 0.3241(19) 0.4748(13) 0.6900(14) 0.044(5) Uani 0.484(15) 1 d PGU B 1
C3 C 0.177(2) 0.4875(13) 0.6217(13) 0.030(5) Uani 0.484(15) 1 d PGU B 1
H3 H 0.0716 0.4350 0.6014 0.030 Uiso 0.484(15) 1 calc PR B 1
C2 C 0.183(2) 0.5768(12) 0.5832(12) 0.028(4) Uani 0.484(15) 1 d PGU B 1
H2 H 0.0816 0.5855 0.5363 0.028 Uiso 0.484(15) 1 calc PR B 1
C1 C 0.3359(18) 0.6533(11) 0.6129(11) 0.027(5) Uani 0.484(15) 1 d PGU B 1
C5 C 0.4833(15) 0.6406(11) 0.6811(13) 0.043(4) Uani 0.484(15) 1 d PGU B 1
H5 H 0.5884 0.6930 0.7015 0.043 Uiso 0.484(15) 1 calc PR B 1
C4 C 0.4774(16) 0.5513(12) 0.7197(15) 0.064(7) Uani 0.484(15) 1 d PGU B 1
H4 H 0.5785 0.5426 0.7665 0.064 Uiso 0.484(15) 1 calc PR B 1
N1A N 0.3266(18) 0.4554(12) 0.6551(13) 0.037(4) Uani 0.516(15) 1 d PGU B 2
C3A C 0.197(2) 0.5147(13) 0.6618(12) 0.037(5) Uani 0.516(15) 1 d PGU B 2
H3A H 0.1055 0.4895 0.6867 0.037 Uiso 0.516(15) 1 calc PR B 2
C2A C 0.2026(19) 0.6116(13) 0.6316(11) 0.025(4) Uani 0.516(15) 1 d PGU B 2
H2A H 0.1154 0.6514 0.6361 0.025 Uiso 0.516(15) 1 calc PR B 2
C1A C 0.3384(16) 0.6491(11) 0.5946(11) 0.022(4) Uani 0.516(15) 1 d PGU B 2
C5A C 0.4683(14) 0.5898(10) 0.5879(13) 0.036(4) Uani 0.516(15) 1 d PGU B 2
H5A H 0.5595 0.6150 0.5630 0.036 Uiso 0.516(15) 1 calc PR B 2
C4A C 0.4624(15) 0.4929(11) 0.6181(14) 0.051(5) Uani 0.516(15) 1 d PGU B 2
H4A H 0.5496 0.4531 0.6136 0.051 Uiso 0.516(15) 1 calc PR B 2
C6 C 0.3427(8) 0.7535(5) 0.5628(5) 0.0184(13) Uani 1 1 d . . .

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
Sm1 0.0102(2) 0.0132(2) 0.0161(2) 0.00437(15) 0.00337(14) 0.00035(14)
Sm2 0.0097(2) 0.0143(2) 0.0195(2) 0.00414(16) 0.00278(14) -0.00041(14)
O1 0.022(3) 0.037(3) 0.038(3) 0.025(2) 0.011(2) 0.011(2)
O2 0.023(3) 0.042(3) 0.052(3) 0.029(3) 0.015(2) 0.001(2)
O3 0.033(3) 0.034(3) 0.021(2) 0.013(2) 0.002(2) 0.007(2)
O4 0.049(4) 0.033(3) 0.031(3) 0.011(2) 0.010(2) 0.016(3)
O5 0.012(3) 0.032(3) 0.052(3) -0.004(2) 0.008(2) -0.003(2)
O6 0.029(3) 0.019(2) 0.041(3) 0.003(2) 0.014(2) 0.004(2)
O1W 0.027(3) 0.027(3) 0.020(2) 0.011(2) 0.006(2) 0.004(2)
O7 0.014(2) 0.020(2) 0.026(2) 0.0051(19) 0.0040(18) -0.0011(18)
O9 0.013(2) 0.018(2) 0.017(2) 0.0075(18) 0.0018(17) 0.0011(17)
O10 0.013(2) 0.019(2) 0.019(2) 0.0067(18) 0.0027(17) -0.0006(17)
N4 0.015(3) 0.034(3) 0.029(3) 0.018(3) 0.006(2) 0.002(2)
N5 0.018(3) 0.058(5) 0.034(4) 0.028(3) 0.006(3) 0.003(3)
N6 0.053(5) 0.119(7) 0.070(5) 0.069(5) 0.017(4) 0.007(5)
N2 0.028(3) 0.047(4) 0.040(3) 0.026(3) 0.002(3) 0.003(3)
C10 0.035(4) 0.051(5) 0.033(4) 0.023(4) 0.007(3) 0.006(4)
C11 0.026(4) 0.033(4) 0.034(3) 0.019(3) 0.007(3) 0.003(3)
C7 0.017(3) 0.033(4) 0.032(3) 0.020(3) 0.004(3) 0.001(3)
C8 0.031(4) 0.037(4) 0.032(4) 0.015(3) 0.006(3) 0.003(3)
C9 0.035(4) 0.034(4) 0.049(4) 0.020(3) 0.011(4) 0.011(3)
C12 0.020(3) 0.026(4) 0.029(3) 0.016(3) 0.005(3) 0.003(3)
N3 0.052(7) 0.020(6) 0.036(8) 0.008(5) 0.004(6) 0.001(5)
C15 0.052(7) 0.035(7) 0.034(7) 0.011(5) 0.011(6) -0.001(6)
C14 0.039(9) 0.031(8) 0.047(10) 0.019(6) 0.024(8) 0.004(7)
C17 0.025(8) 0.047(9) 0.039(9) -0.009(7) -0.003(7) 0.013(7)
C16 0.046(8) 0.042(9) 0.034(9) -0.006(7) 0.009(8) 0.025(7)
N3A 0.037(7) 0.026(6) 0.024(7) -0.005(5) 0.010(6) 0.007(5)
C15A 0.037(8) 0.022(6) 0.040(7) 0.002(5) 0.013(6) -0.003(5)
C14A 0.046(11) 0.018(7) 0.049(10) 0.006(6) 0.033(9) 0.004(7)
C17A 0.027(8) 0.023(6) 0.031(7) 0.011(5) 0.006(6) 0.008(6)
C16A 0.041(7) 0.036(6) 0.028(6) 0.006(5) 0.012(6) 0.006(5)
C18 0.020(3) 0.019(3) 0.024(3) 0.004(3) 0.007(3) 0.007(3)
N1 0.043(10) 0.039(10) 0.060(14) 0.032(10) 0.017(8) 0.008(7)
C3 0.037(8) 0.020(9) 0.046(14) 0.016(10) 0.026(8) 0.010(7)
C2 0.032(7) 0.017(9) 0.029(11) 0.008(8) 0.002(8) 0.001(7)
C1 0.032(10) 0.011(9) 0.040(11) 0.009(8) 0.012(8) 0.008(7)
C5 0.031(6) 0.046(8) 0.056(9) 0.030(7) 0.005(6) 0.004(5)
C4 0.044(9) 0.056(14) 0.099(19) 0.053(14) 0.001(11) 0.008(8)
N1A 0.040(9) 0.023(7) 0.042(10) 0.017(7) -0.001(6) 0.000(6)
C3A 0.053(11) 0.031(10) 0.028(11) 0.010(9) 0.020(9) 0.001(8)
C2A 0.030(9) 0.030(10) 0.025(10) 0.012(8) 0.018(8) 0.013(8)
C1A 0.012(8) 0.035(11) 0.021(8) 0.020(8) -0.001(6) 0.002(6)
C5A 0.023(6) 0.036(7) 0.059(8) 0.025(6) 0.016(6) 0.009(5)
C4A 0.032(9) 0.045(10) 0.087(15) 0.041(11) 0.011(9) 0.016(8)
C6 0.018(3) 0.018(3) 0.019(3) 0.010(3) 0.003(2) 0.004(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
Sm1 O1 2.374(4) . ?
Sm1 O9 2.378(4) 2_576 ?
Sm1 O6 2.404(4) 2_676 ?
Sm1 O9 2.405(4) . ?
Sm1 O10 2.428(4) . ?
Sm1 O1W 2.446(4) . ?
Sm1 N4 2.562(5) . ?
Sm1 O7 2.609(4) . ?
Sm1 Sm2 3.8310(5) 2_576 ?
Sm1 Sm1 3.8755(6) 2_576 ?
Sm1 Sm2 3.9230(4) . ?
Sm2 O5 2.382(5) . ?
Sm2 O3 2.380(4) . ?
Sm2 O2 2.400(5) 2_676 ?
Sm2 O10 2.408(4) . ?
Sm2 O9 2.441(4) . ?
Sm2 O10 2.453(4) 2_676 ?
Sm2 N4 2.511(5) 2_576 ?
Sm2 O7 2.584(4) 2_576 ?
Sm2 Sm1 3.8310(5) 2_576 ?
Sm2 Sm2 3.8680(6) 2_676 ?
O1 C6 1.248(8) . ?
O2 C6 1.241(8) . ?
O2 Sm2 2.400(4) 2_676 ?
O3 C12 1.273(8) . ?
O4 C12 1.248(8) . ?
O5 C18 1.232(9) . ?
O6 C18 1.275(7) . ?
O6 Sm1 2.404(4) 2_676 ?
O7 Sm2 2.584(4) 2_576 ?
O9 Sm1 2.378(4) 2_576 ?
O10 Sm2 2.453(4) 2_676 ?
N4 N5 1.181(7) . ?
N4 Sm2 2.511(5) 2_576 ?
N5 N6 1.139(9) . ?
N2 C10 1.372(3) . ?
N2 C9 1.372(3) . ?
C10 C11 1.372(3) . ?
C10 H10 0.9300 . ?
C11 C7 1.372(3) . ?
C11 H11 0.9300 . ?
C7 C8 1.372(3) . ?
C7 C12 1.543(7) . ?
C8 C9 1.372(3) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
N3 C15 1.367(8) . ?
N3 C16 1.368(8) . ?
C15 C14 1.367(8) . ?
C15 H15 0.9300 . ?
C14 C13 1.367(8) . ?
C14 H14 0.9300 . ?
C13 C17 1.367(8) . ?
C13 C18 1.541(13) . ?
C17 C16 1.367(8) . ?
C17 H17 0.9300 . ?
C16 H16 0.9300 . ?
N3A C15A 1.361(7) . ?
N3A C16A 1.361(7) . ?
C15A C14A 1.361(7) . ?
C15A H15A 0.9300 . ?
C14A C13A 1.361(7) . ?
C14A H14A 0.9300 . ?
C13A C17A 1.361(7) . ?
C13A C18 1.528(12) . ?
C17A C16A 1.361(7) . ?
C17A H17A 0.9300 . ?
C16A H16A 0.9300 . ?
N1 C3 1.356(9) . ?
N1 C4 1.356(9) . ?
C3 C2 1.356(9) . ?
C3 H3 0.9300 . ?
C2 C1 1.356(9) . ?
C2 H2 0.9300 . ?
C1 C5 1.356(9) . ?
C1 C6 1.578(14) . ?
C5 C4 1.356(9) . ?
C5 H5 0.9300 . ?
C4 H4 0.9300 . ?
N1A C3A 1.385(9) . ?
N1A C4A 1.386(9) . ?
C3A C2A 1.385(9) . ?
C3A H3A 0.9300 . ?
C2A C1A 1.385(9) . ?
C2A H2A 0.9300 . ?
C1A C5A 1.385(9) . ?
C1A C6 1.488(14) . ?
C5A C4A 1.385(9) . ?
C5A H5A 0.9300 . ?
C4A H4A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Sm1 O9 136.29(15) . 2_576 ?
O1 Sm1 O6 75.53(17) . 2_676 ?
O9 Sm1 O6 141.41(16) 2_576 2_676 ?
O1 Sm1 O9 75.67(16) . . ?
O9 Sm1 O9 71.75(16) 2_576 . ?
O6 Sm1 O9 146.83(16) 2_676 . ?
O1 Sm1 O10 83.22(15) . . ?
O9 Sm1 O10 112.08(15) 2_576 . ?
O6 Sm1 O10 89.28(15) 2_676 . ?
O9 Sm1 O10 71.29(16) . . ?
O1 Sm1 O1W 144.65(16) . . ?
O9 Sm1 O1W 78.54(15) 2_576 . ?
O6 Sm1 O1W 76.33(16) 2_676 . ?
O9 Sm1 O1W 121.64(15) . . ?
O10 Sm1 O1W 75.45(15) . . ?
O1 Sm1 N4 75.62(16) . . ?
O9 Sm1 N4 68.92(15) 2_576 . ?
O6 Sm1 N4 111.87(17) 2_676 . ?
O9 Sm1 N4 76.12(16) . . ?
O10 Sm1 N4 144.61(16) . . ?
O1W Sm1 N4 135.55(17) . . ?
O1 Sm1 O7 116.88(16) . . ?
O9 Sm1 O7 69.50(14) 2_576 . ?
O6 Sm1 O7 76.31(15) 2_676 . ?
O9 Sm1 O7 132.32(14) . . ?
O10 Sm1 O7 150.40(14) . . ?
O1W Sm1 O7 76.06(15) . . ?
N4 Sm1 O7 64.79(16) . . ?
O1 Sm1 Sm2 115.88(11) . 2_576 ?
O9 Sm1 Sm2 37.93(10) 2_576 2_576 ?
O6 Sm1 Sm2 117.17(12) 2_676 2_576 ?
O9 Sm1 Sm2 90.21(10) . 2_576 ?
O10 Sm1 Sm2 149.81(10) . 2_576 ?
O1W Sm1 Sm2 95.88(11) . 2_576 ?
N4 Sm1 Sm2 40.46(12) . 2_576 ?
O7 Sm1 Sm2 42.21(9) . 2_576 ?
O1 Sm1 Sm1 106.86(12) . 2_576 ?
O9 Sm1 Sm1 36.10(10) 2_576 2_576 ?
O6 Sm1 Sm1 177.48(12) 2_676 2_576 ?
O9 Sm1 Sm1 35.65(10) . 2_576 ?
O10 Sm1 Sm1 91.81(10) . 2_576 ?
O1W Sm1 Sm1 101.74(11) . 2_576 ?
N4 Sm1 Sm1 68.31(13) . 2_576 ?
O7 Sm1 Sm1 101.70(9) . 2_576 ?
Sm2 Sm1 Sm1 61.198(8) 2_576 2_576 ?
O1 Sm1 Sm2 81.97(13) . . ?
O9 Sm1 Sm2 88.40(10) 2_576 . ?
O6 Sm1 Sm2 122.75(12) 2_676 . ?
O9 Sm1 Sm2 36.26(10) . . ?
O10 Sm1 Sm2 35.62(10) . . ?
O1W Sm1 Sm2 95.80(11) . . ?
N4 Sm1 Sm2 112.21(13) . . ?
O7 Sm1 Sm2 157.46(9) . . ?
Sm2 Sm1 Sm2 120.039(9) 2_576 . ?
Sm1 Sm1 Sm2 58.842(10) 2_576 . ?
O5 Sm2 O3 79.91(19) . . ?
O5 Sm2 O2 76.94(19) . 2_676 ?
O3 Sm2 O2 147.60(18) . 2_676 ?
O5 Sm2 O10 149.84(15) . . ?
O3 Sm2 O10 108.41(16) . . ?
O2 Sm2 O10 82.33(17) 2_676 . ?
O5 Sm2 O9 138.00(16) . . ?
O3 Sm2 O9 73.57(16) . . ?
O2 Sm2 O9 137.87(16) 2_676 . ?
O10 Sm2 O9 71.00(15) . . ?
O5 Sm2 O10 81.30(16) . 2_676 ?
O3 Sm2 O10 71.33(16) . 2_676 ?
O2 Sm2 O10 82.97(15) 2_676 2_676 ?
O10 Sm2 O10 74.57(16) . 2_676 ?
O9 Sm2 O10 118.58(14) . 2_676 ?
O5 Sm2 N4 112.57(18) . 2_576 ?
O3 Sm2 N4 134.44(17) . 2_576 ?
O2 Sm2 N4 76.12(17) 2_676 2_576 ?
O10 Sm2 N4 82.82(17) . 2_576 ?
O9 Sm2 N4 68.83(15) . 2_576 ?
O10 Sm2 N4 150.99(16) 2_676 2_576 ?
O5 Sm2 O7 73.87(15) . 2_576 ?
O3 Sm2 O7 77.38(15) . 2_576 ?
O2 Sm2 O7 116.69(16) 2_676 2_576 ?
O10 Sm2 O7 135.79(14) . 2_576 ?
O9 Sm2 O7 68.99(14) . 2_576 ?
O10 Sm2 O7 142.86(14) 2_676 2_576 ?
N4 Sm2 O7 65.86(16) 2_576 2_576 ?
O5 Sm2 Sm1 115.68(12) . 2_576 ?
O3 Sm2 Sm1 93.11(13) . 2_576 ?
O2 Sm2 Sm1 117.27(12) 2_676 2_576 ?
O10 Sm2 Sm1 93.21(10) . 2_576 ?
O9 Sm2 Sm1 36.79(10) . 2_576 ?
O10 Sm2 Sm1 155.24(10) 2_676 2_576 ?
N4 Sm2 Sm1 41.46(12) 2_576 2_576 ?
O7 Sm2 Sm1 42.71(10) 2_576 2_576 ?
O5 Sm2 Sm2 116.26(12) . 2_676 ?
O3 Sm2 Sm2 89.63(12) . 2_676 ?
O2 Sm2 Sm2 80.75(13) 2_676 2_676 ?
O10 Sm2 Sm2 37.69(10) . 2_676 ?
O9 Sm2 Sm2 95.78(10) . 2_676 ?
O10 Sm2 Sm2 36.88(10) 2_676 2_676 ?
N4 Sm2 Sm2 118.48(13) 2_576 2_676 ?
O7 Sm2 Sm2 162.15(9) 2_576 2_676 ?
Sm1 Sm2 Sm2 127.641(14) 2_576 2_676 ?
O5 Sm2 Sm1 173.54(13) . . ?
O3 Sm2 Sm1 95.29(13) . . ?
O2 Sm2 Sm1 109.14(14) 2_676 . ?
O10 Sm2 Sm1 35.96(10) . . ?
O9 Sm2 Sm1 35.63(10) . . ?
O10 Sm2 Sm1 101.35(10) 2_676 . ?
N4 Sm2 Sm1 67.78(13) 2_576 . ?
O7 Sm2 Sm1 100.97(10) 2_576 . ?
Sm1 Sm2 Sm1 59.961(9) 2_576 . ?
Sm2 Sm2 Sm1 67.717(11) 2_676 . ?
C6 O1 Sm1 141.7(4) . . ?
C6 O2 Sm2 137.2(4) . 2_676 ?
C12 O3 Sm2 134.8(4) . . ?
C18 O5 Sm2 152.4(4) . . ?
C18 O6 Sm1 135.3(4) . 2_676 ?
Sm2 O7 Sm1 95.08(14) 2_576 . ?
Sm1 O9 Sm1 108.25(16) 2_576 . ?
Sm1 O9 Sm2 105.29(16) 2_576 . ?
Sm1 O9 Sm2 108.11(16) . . ?
Sm2 O10 Sm1 108.42(16) . . ?
Sm2 O10 Sm2 105.43(16) . 2_676 ?
Sm1 O10 Sm2 125.58(18) . 2_676 ?
N5 N4 Sm2 129.1(5) . 2_576 ?
N5 N4 Sm1 132.1(5) . . ?
Sm2 N4 Sm1 98.08(17) 2_576 . ?
N6 N5 N4 178.6(9) . . ?
C10 N2 C9 120.0 . . ?
C11 C10 N2 120.0 . . ?
C11 C10 H10 120.0 . . ?
N2 C10 H10 120.0 . . ?
C10 C11 C7 120.0 . . ?
C10 C11 H11 120.0 . . ?
C7 C11 H11 120.0 . . ?
C11 C7 C8 120.0 . . ?
C11 C7 C12 119.0(4) . . ?
C8 C7 C12 121.0(4) . . ?
C9 C8 C7 120.0 . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 N2 120.0 . . ?
C8 C9 H9 120.0 . . ?
N2 C9 H9 120.0 . . ?
O4 C12 O3 124.7(6) . . ?
O4 C12 C7 119.4(6) . . ?
O3 C12 C7 115.9(5) . . ?
C15 N3 C16 120.0 . . ?
C14 C15 N3 120.0 . . ?
C14 C15 H15 120.0 . . ?
N3 C15 H15 120.0 . . ?
C15 C14 C13 120.0 . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C17 C13 C14 120.0 . . ?
C17 C13 C18 119.9(7) . . ?
C14 C13 C18 120.1(7) . . ?
C13 C17 C16 120.0 . . ?
C13 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C16 N3 120.0 . . ?
C17 C16 H16 120.0 . . ?
N3 C16 H16 120.0 . . ?
C15A N3A C16A 120.0 . . ?
N3A C15A C14A 120.0 . . ?
N3A C15A H15A 120.0 . . ?
C14A C15A H15A 120.0 . . ?
C15A C14A C13A 120.0 . . ?
C15A C14A H14A 120.0 . . ?
C13A C14A H14A 120.0 . . ?
C14A C13A C17A 120.0 . . ?
C14A C13A C18 120.8(6) . . ?
C17A C13A C18 119.1(6) . . ?
C16A C17A C13A 120.0 . . ?
C16A C17A H17A 120.0 . . ?
C13A C17A H17A 120.0 . . ?
C17A C16A N3A 120.0 . . ?
C17A C16A H16A 120.0 . . ?
N3A C16A H16A 120.0 . . ?
O5 C18 O6 124.8(6) . . ?
O5 C18 C13 118.8(6) . . ?
O6 C18 C13 116.3(7) . . ?
O5 C18 C13A 116.9(7) . . ?
O6 C18 C13A 118.2(7) . . ?
C13 C18 C13A 4.3(6) . . ?
C3 N1 C4 120.0 . . ?
N1 C3 C2 120.0 . . ?
N1 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C1 C2 C3 120.0 . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C5 C1 C2 120.0 . . ?
C5 C1 C6 120.4(8) . . ?
C2 C1 C6 119.5(8) . . ?
C1 C5 C4 120.0 . . ?
C1 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C4 N1 120.0 . . ?
C5 C4 H4 120.0 . . ?
N1 C4 H4 120.0 . . ?
C3A N1A C4A 120.0 . . ?
C2A C3A N1A 120.0 . . ?
C2A C3A H3A 120.0 . . ?
N1A C3A H3A 120.0 . . ?
C3A C2A C1A 120.0 . . ?
C3A C2A H2A 120.0 . . ?
C1A C2A H2A 120.0 . . ?
C5A C1A C2A 120.0 . . ?
C5A C1A C6 120.8(8) . . ?
C2A C1A C6 119.2(8) . . ?
C1A C5A C4A 120.0 . . ?
C1A C5A H5A 120.0 . . ?
C4A C5A H5A 120.0 . . ?
C5A C4A N1A 120.0 . . ?
C5A C4A H4A 120.0 . . ?
N1A C4A H4A 120.0 . . ?
O2 C6 O1 125.3(6) . . ?
O2 C6 C1A 116.7(7) . . ?
O1 C6 C1A 117.8(7) . . ?
O2 C6 C1 119.3(7) . . ?
O1 C6 C1 115.3(7) . . ?
C1A C6 C1 7.8(8) . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         2.670
_refine_diff_density_min         -3.559
_refine_diff_density_rms         0.305