# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Paul Kruger'
_publ_contact_author_email       PAUL.KRUGER@CANTERBURY.AC.NZ

_publ_section_title              
;
Synthesis and structural characterisation of
lanthanide coordination polymers featuring
4,4',6,6'-tetra-carboxy-2,2'-bipyridine and rare network topology
;
loop_
_publ_author_name
'Paul Kruger'
'Stuart Batten'
'Sandrine Goetz'
'Niamh R Kelly'

# Attachment 'B801985A__revised.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 677289'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            7
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H11 La N2 O11, H2 O'
_chemical_formula_sum            'C14 H13 La N2 O12'
_chemical_formula_weight         540.17

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'
La La -0.2871 2.4523 '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'

_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                   6.9628(3)
_cell_length_b                   11.0010(3)
_cell_length_c                   11.5319(5)
_cell_angle_alpha                79.8560(10)
_cell_angle_beta                 73.862(2)
_cell_angle_gamma                76.865(2)
_cell_volume                     820.27(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             528
_exptl_absorpt_coefficient_mu    2.682
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7814
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   TWINABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      153(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'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4505
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         30.49
_reflns_number_total             4505
_reflns_number_gt                4326
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXTL version 5.1 (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXTL version 5.1 (Sheldrick, 1998)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
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)+(0.0328P)²+0.1836P] where P=(Fo²+2Fc²)/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         4505
_refine_ls_number_parameters     290
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0228
_refine_ls_wR_factor_ref         0.0612
_refine_ls_wR_factor_gt          0.0606
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.056
_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
La1 La 0.666434(16) 0.467805(9) 0.243269(9) 0.01043(5) Uani 1 1 d . . .
N1 N 0.8962(3) 0.26612(16) 0.13068(16) 0.0122(3) Uani 1 1 d . . .
C1 C 0.9839(3) 0.28824(19) 0.01134(19) 0.0120(4) Uani 1 1 d . . .
C2 C 1.1260(3) 0.1984(2) -0.05363(19) 0.0135(4) Uani 1 1 d . . .
H2A H 1.1869 0.2175 -0.1376 0.016 Uiso 1 1 calc R . .
C3 C 1.1771(3) 0.0796(2) 0.0075(2) 0.0131(4) Uani 1 1 d . . .
C4 C 1.0821(3) 0.0543(2) 0.12961(19) 0.0133(4) Uani 1 1 d . . .
H4A H 1.1125 -0.0268 0.1725 0.016 Uiso 1 1 calc R . .
C5 C 0.9409(3) 0.15048(19) 0.18826(19) 0.0116(4) Uani 1 1 d . . .
C6 C 0.8276(3) 0.13036(19) 0.31751(19) 0.0112(4) Uani 1 1 d . . .
C7 C 0.8481(3) 0.01382(19) 0.38811(19) 0.0126(4) Uani 1 1 d . . .
H7A H 0.9335 -0.0578 0.3531 0.015 Uiso 1 1 calc R . .
C8 C 0.7430(3) 0.00270(19) 0.51015(19) 0.0117(4) Uani 1 1 d . . .
C9 C 0.6207(3) 0.10987(19) 0.55777(19) 0.0129(4) Uani 1 1 d . . .
H9A H 0.5523 0.1070 0.6416 0.016 Uiso 1 1 calc R . .
C10 C 0.6006(3) 0.22111(19) 0.48028(19) 0.0116(4) Uani 1 1 d . . .
N2 N 0.7001(3) 0.23236(16) 0.36277(16) 0.0111(3) Uani 1 1 d . . .
C11 C 0.4604(3) 0.33967(19) 0.52408(19) 0.0128(4) Uani 1 1 d . . .
O1 O 0.4162(2) 0.42620(14) 0.44211(14) 0.0140(3) Uani 1 1 d . . .
O2 O 0.3989(2) 0.34346(14) 0.63651(14) 0.0159(3) Uani 1 1 d . . .
C12 C 0.7670(3) -0.12561(19) 0.58599(19) 0.0128(4) Uani 1 1 d . . .
O3 O 0.6734(2) -0.13562(15) 0.69648(14) 0.0172(3) Uani 1 1 d . . .
O4 O 0.8810(3) -0.21469(15) 0.53235(15) 0.0186(3) Uani 1 1 d . . .
C13 C 1.3300(3) -0.0224(2) -0.05696(19) 0.0138(4) Uani 1 1 d . . .
O5 O 1.3814(3) -0.12481(16) -0.00506(16) 0.0231(4) Uani 1 1 d . . .
O6 O 1.3979(3) 0.01404(16) -0.17259(16) 0.0226(4) Uani 1 1 d . . .
H6 H 1.485(6) -0.043(4) -0.205(4) 0.048(11) Uiso 1 1 d . . .
C14 C 0.9165(3) 0.41794(19) -0.04957(19) 0.0123(4) Uani 1 1 d . . .
O7 O 1.0153(2) 0.44672(14) -0.15695(14) 0.0144(3) Uani 1 1 d . . .
O8 O 0.7668(2) 0.48816(14) 0.00914(14) 0.0145(3) Uani 1 1 d . . .
O1W O 0.4150(3) 0.37054(16) 0.18727(16) 0.0199(3) Uani 1 1 d D . .
H1W1 H 0.393(5) 0.2984(16) 0.210(3) 0.030 Uiso 1 1 d D . .
H2W1 H 0.354(4) 0.400(3) 0.133(2) 0.030 Uiso 1 1 d D . .
O2W O 0.4341(3) 0.65079(16) 0.15858(17) 0.0221(4) Uani 1 1 d D . .
H1W2 H 0.457(5) 0.701(3) 0.0955(19) 0.033 Uiso 1 1 d D . .
H2W2 H 0.325(3) 0.683(3) 0.203(2) 0.033 Uiso 1 1 d D . .
O3W O 0.8887(3) 0.43355(16) 0.39586(15) 0.0180(3) Uani 1 1 d D . .
H1W3 H 0.975(4) 0.372(2) 0.412(3) 0.027 Uiso 1 1 d D . .
H2W3 H 0.831(4) 0.464(3) 0.4607(17) 0.027 Uiso 1 1 d D . .
O4W O 0.0695(3) 0.7073(2) 0.3083(2) 0.0378(5) Uani 1 1 d D . .
H1W4 H 0.009(6) 0.653(3) 0.299(4) 0.057 Uiso 1 1 d D . .
H2W4 H 0.006(5) 0.733(4) 0.376(2) 0.057 Uiso 1 1 d 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
La1 O7 2.4855(15) 2_765 ?
La1 O1 2.5050(15) . ?
La1 O2W 2.5156(17) . ?
La1 O1W 2.5200(16) . ?
La1 O8 2.5763(15) . ?
La1 O3W 2.5782(17) . ?
La1 O2 2.5834(15) 2_666 ?
La1 N2 2.7036(17) . ?
La1 N1 2.7231(17) . ?
N1 C5 1.339(3) . ?
N1 C1 1.345(3) . ?
C1 C2 1.386(3) . ?
C1 C14 1.509(3) . ?
C2 C3 1.391(3) . ?
C2 H2A 0.9500 . ?
C3 C4 1.388(3) . ?
C3 C13 1.501(3) . ?
C4 C5 1.398(3) . ?
C4 H4A 0.9500 . ?
C5 C6 1.484(3) . ?
C6 N2 1.347(3) . ?
C6 C7 1.393(3) . ?
C7 C8 1.393(3) . ?
C7 H7A 0.9500 . ?
C8 C9 1.389(3) . ?
C8 C12 1.525(3) . ?
C9 C10 1.386(3) . ?
C9 H9A 0.9500 . ?
C10 N2 1.338(3) . ?
C10 C11 1.513(3) . ?
C11 O2 1.252(3) . ?
C11 O1 1.267(3) . ?
O2 La1 2.5834(15) 2_666 ?
C12 O4 1.249(3) . ?
C12 O3 1.258(3) . ?
C13 O5 1.206(3) . ?
C13 O6 1.307(3) . ?
O6 H6 0.83(4) . ?
C14 O8 1.252(3) . ?
C14 O7 1.263(2) . ?
O7 La1 2.4855(15) 2_765 ?
O1W H1W1 0.827(12) . ?
O1W H2W1 0.827(12) . ?
O2W H1W2 0.831(12) . ?
O2W H2W2 0.835(12) . ?
O3W H1W3 0.831(12) . ?
O3W H2W3 0.835(12) . ?
O4W H1W4 0.846(12) . ?
O4W H2W4 0.845(12) . ?

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
O7 La1 O1 140.76(5) 2_765 . ?
O7 La1 O2W 96.62(5) 2_765 . ?
O1 La1 O2W 95.80(5) . . ?
O7 La1 O1W 142.80(5) 2_765 . ?
O1 La1 O1W 76.42(5) . . ?
O2W La1 O1W 75.18(6) . . ?
O7 La1 O8 68.32(5) 2_765 . ?
O1 La1 O8 150.40(5) . . ?
O2W La1 O8 69.94(5) . . ?
O1W La1 O8 74.88(5) . . ?
O7 La1 O3W 67.26(5) 2_765 . ?
O1 La1 O3W 78.03(5) . . ?
O2W La1 O3W 135.88(6) . . ?
O1W La1 O3W 141.59(5) . . ?
O8 La1 O3W 130.41(5) . . ?
O7 La1 O2 77.79(5) 2_765 2_666 ?
O1 La1 O2 71.89(5) . 2_666 ?
O2W La1 O2 69.98(6) . 2_666 ?
O1W La1 O2 129.33(6) . 2_666 ?
O8 La1 O2 122.86(5) . 2_666 ?
O3W La1 O2 66.58(5) . 2_666 ?
O7 La1 N2 117.23(5) 2_765 . ?
O1 La1 N2 61.20(5) . . ?
O2W La1 N2 145.86(6) . . ?
O1W La1 N2 74.97(5) . . ?
O8 La1 N2 116.97(5) . . ?
O3W La1 N2 67.69(5) . . ?
O2 La1 N2 119.20(5) 2_666 . ?
O7 La1 N1 82.29(5) 2_765 . ?
O1 La1 N1 117.79(5) . . ?
O2W La1 N1 127.48(6) . . ?
O1W La1 N1 75.25(6) . . ?
O8 La1 N1 60.95(5) . . ?
O3W La1 N1 92.18(5) . . ?
O2 La1 N1 155.20(5) 2_666 . ?
N2 La1 N1 58.42(5) . . ?
C5 N1 C1 118.60(18) . . ?
C5 N1 La1 124.27(13) . . ?
C1 N1 La1 116.86(13) . . ?
N1 C1 C2 122.96(19) . . ?
N1 C1 C14 115.82(18) . . ?
C2 C1 C14 121.21(19) . . ?
C1 C2 C3 118.22(19) . . ?
C1 C2 H2A 120.9 . . ?
C3 C2 H2A 120.9 . . ?
C4 C3 C2 119.32(19) . . ?
C4 C3 C13 119.48(19) . . ?
C2 C3 C13 121.19(19) . . ?
C3 C4 C5 118.71(19) . . ?
C3 C4 H4A 120.6 . . ?
C5 C4 H4A 120.6 . . ?
N1 C5 C4 122.10(19) . . ?
N1 C5 C6 115.69(17) . . ?
C4 C5 C6 122.19(18) . . ?
N2 C6 C7 121.57(19) . . ?
N2 C6 C5 115.64(17) . . ?
C7 C6 C5 122.78(18) . . ?
C8 C7 C6 119.74(19) . . ?
C8 C7 H7A 120.1 . . ?
C6 C7 H7A 120.1 . . ?
C9 C8 C7 118.24(19) . . ?
C9 C8 C12 122.74(19) . . ?
C7 C8 C12 119.02(18) . . ?
C10 C9 C8 118.55(19) . . ?
C10 C9 H9A 120.7 . . ?
C8 C9 H9A 120.7 . . ?
N2 C10 C9 123.47(19) . . ?
N2 C10 C11 115.05(17) . . ?
C9 C10 C11 121.47(18) . . ?
C10 N2 C6 118.26(17) . . ?
C10 N2 La1 116.28(13) . . ?
C6 N2 La1 124.91(13) . . ?
O2 C11 O1 126.2(2) . . ?
O2 C11 C10 117.70(18) . . ?
O1 C11 C10 116.09(18) . . ?
C11 O1 La1 122.16(13) . . ?
C11 O2 La1 128.81(13) . 2_666 ?
O4 C12 O3 124.4(2) . . ?
O4 C12 C8 116.52(18) . . ?
O3 C12 C8 119.10(18) . . ?
O5 C13 O6 125.5(2) . . ?
O5 C13 C3 122.3(2) . . ?
O6 C13 C3 112.13(18) . . ?
C13 O6 H6 110(3) . . ?
O8 C14 O7 125.0(2) . . ?
O8 C14 C1 117.95(18) . . ?
O7 C14 C1 117.01(18) . . ?
C14 O7 La1 133.18(14) . 2_765 ?
C14 O8 La1 122.66(13) . . ?
La1 O1W H1W1 127(2) . . ?
La1 O1W H2W1 126(2) . . ?
H1W1 O1W H2W1 107(3) . . ?
La1 O2W H1W2 131(2) . . ?
La1 O2W H2W2 121(2) . . ?
H1W2 O2W H2W2 107(3) . . ?
La1 O3W H1W3 130(2) . . ?
La1 O3W H2W3 115(2) . . ?
H1W3 O3W H2W3 107(3) . . ?
H1W4 O4W H2W4 107(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O7 La1 N1 C5 119.38(17) 2_765 . . . ?
O1 La1 N1 C5 -24.93(18) . . . . ?
O2W La1 N1 C5 -148.17(15) . . . . ?
O1W La1 N1 C5 -90.53(17) . . . . ?
O8 La1 N1 C5 -171.19(18) . . . . ?
O3W La1 N1 C5 52.68(16) . . . . ?
O2 La1 N1 C5 82.7(2) 2_666 . . . ?
N2 La1 N1 C5 -9.32(15) . . . . ?
O7 La1 N1 C1 -54.51(15) 2_765 . . . ?
O1 La1 N1 C1 161.18(14) . . . . ?
O2W La1 N1 C1 37.94(17) . . . . ?
O1W La1 N1 C1 95.58(15) . . . . ?
O8 La1 N1 C1 14.92(13) . . . . ?
O3W La1 N1 C1 -121.21(15) . . . . ?
O2 La1 N1 C1 -91.20(18) 2_666 . . . ?
N2 La1 N1 C1 176.78(17) . . . . ?
C5 N1 C1 C2 -3.2(3) . . . . ?
La1 N1 C1 C2 171.08(16) . . . . ?
C5 N1 C1 C14 176.14(18) . . . . ?
La1 N1 C1 C14 -9.6(2) . . . . ?
N1 C1 C2 C3 1.1(3) . . . . ?
C14 C1 C2 C3 -178.21(19) . . . . ?
C1 C2 C3 C4 1.3(3) . . . . ?
C1 C2 C3 C13 -179.92(19) . . . . ?
C2 C3 C4 C5 -1.5(3) . . . . ?
C13 C3 C4 C5 179.72(19) . . . . ?
C1 N1 C5 C4 3.0(3) . . . . ?
La1 N1 C5 C4 -170.84(15) . . . . ?
C1 N1 C5 C6 -175.78(18) . . . . ?
La1 N1 C5 C6 10.4(2) . . . . ?
C3 C4 C5 N1 -0.7(3) . . . . ?
C3 C4 C5 C6 177.97(19) . . . . ?
N1 C5 C6 N2 -2.8(3) . . . . ?
C4 C5 C6 N2 178.43(19) . . . . ?
N1 C5 C6 C7 176.4(2) . . . . ?
C4 C5 C6 C7 -2.4(3) . . . . ?
N2 C6 C7 C8 -3.3(3) . . . . ?
C5 C6 C7 C8 177.56(19) . . . . ?
C6 C7 C8 C9 -0.4(3) . . . . ?
C6 C7 C8 C12 179.91(19) . . . . ?
C7 C8 C9 C10 3.4(3) . . . . ?
C12 C8 C9 C10 -176.90(19) . . . . ?
C8 C9 C10 N2 -3.1(3) . . . . ?
C8 C9 C10 C11 176.35(19) . . . . ?
C9 C10 N2 C6 -0.4(3) . . . . ?
C11 C10 N2 C6 -179.93(18) . . . . ?
C9 C10 N2 La1 -172.33(16) . . . . ?
C11 C10 N2 La1 8.2(2) . . . . ?
C7 C6 N2 C10 3.6(3) . . . . ?
C5 C6 N2 C10 -177.14(18) . . . . ?
C7 C6 N2 La1 174.80(15) . . . . ?
C5 C6 N2 La1 -6.0(2) . . . . ?
O7 La1 N2 C10 118.51(14) 2_765 . . . ?
O1 La1 N2 C10 -16.82(14) . . . . ?
O2W La1 N2 C10 -69.58(18) . . . . ?
O1W La1 N2 C10 -99.36(15) . . . . ?
O8 La1 N2 C10 -163.28(14) . . . . ?
O3W La1 N2 C10 71.45(15) . . . . ?
O2 La1 N2 C10 27.63(16) 2_666 . . . ?
N1 La1 N2 C10 178.94(17) . . . . ?
O7 La1 N2 C6 -52.81(17) 2_765 . . . ?
O1 La1 N2 C6 171.86(18) . . . . ?
O2W La1 N2 C6 119.11(16) . . . . ?
O1W La1 N2 C6 89.32(16) . . . . ?
O8 La1 N2 C6 25.40(18) . . . . ?
O3W La1 N2 C6 -99.87(17) . . . . ?
O2 La1 N2 C6 -143.68(15) 2_666 . . . ?
N1 La1 N2 C6 7.62(15) . . . . ?
N2 C10 C11 O2 -164.48(19) . . . . ?
C9 C10 C11 O2 16.0(3) . . . . ?
N2 C10 C11 O1 15.6(3) . . . . ?
C9 C10 C11 O1 -163.9(2) . . . . ?
O2 C11 O1 La1 144.89(18) . . . . ?
C10 C11 O1 La1 -35.2(2) . . . . ?
O7 La1 O1 C11 -70.92(18) 2_765 . . . ?
O2W La1 O1 C11 -178.84(16) . . . . ?
O1W La1 O1 C11 107.97(16) . . . . ?
O8 La1 O1 C11 122.43(16) . . . . ?
O3W La1 O1 C11 -43.10(15) . . . . ?
O2 La1 O1 C11 -112.12(16) 2_666 . . . ?
N2 La1 O1 C11 27.85(15) . . . . ?
N1 La1 O1 C11 43.01(17) . . . . ?
O1 C11 O2 La1 -36.1(3) . . . 2_666 ?
C10 C11 O2 La1 144.00(15) . . . 2_666 ?
C9 C8 C12 O4 179.8(2) . . . . ?
C7 C8 C12 O4 -0.5(3) . . . . ?
C9 C8 C12 O3 -0.3(3) . . . . ?
C7 C8 C12 O3 179.44(19) . . . . ?
C4 C3 C13 O5 -3.6(3) . . . . ?
C2 C3 C13 O5 177.6(2) . . . . ?
C4 C3 C13 O6 176.7(2) . . . . ?
C2 C3 C13 O6 -2.1(3) . . . . ?
N1 C1 C14 O8 -9.8(3) . . . . ?
C2 C1 C14 O8 169.51(19) . . . . ?
N1 C1 C14 O7 170.82(18) . . . . ?
C2 C1 C14 O7 -9.9(3) . . . . ?
O8 C14 O7 La1 95.8(2) . . . 2_765 ?
C1 C14 O7 La1 -84.9(2) . . . 2_765 ?
O7 C14 O8 La1 -154.05(16) . . . . ?
C1 C14 O8 La1 26.6(2) . . . . ?
O7 La1 O8 C14 71.09(15) 2_765 . . . ?
O1 La1 O8 C14 -117.95(16) . . . . ?
O2W La1 O8 C14 177.19(17) . . . . ?
O1W La1 O8 C14 -103.38(16) . . . . ?
O3W La1 O8 C14 43.33(17) . . . . ?
O2 La1 O8 C14 129.24(15) 2_666 . . . ?
N2 La1 O8 C14 -39.41(17) . . . . ?
N1 La1 O8 C14 -22.10(15) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O6 H6 O3 0.83(4) 1.74(4) 2.550(2) 166(4) 1_654
O1W H1W1 O3 0.827(12) 1.998(14) 2.811(2) 167(3) 2_656
O1W H2W1 O8 0.827(12) 2.123(13) 2.934(2) 167(3) 2_665
O2W H1W2 O5 0.831(12) 2.10(2) 2.850(2) 150(3) 1_465
O2W H2W2 O4W 0.835(12) 1.842(15) 2.652(3) 163(3) .
O3W H1W3 O4 0.831(12) 1.892(14) 2.709(2) 167(3) 2_756
O3W H2W3 O1 0.835(12) 2.033(18) 2.775(2) 148(3) 2_666
O4W H1W4 O7 0.846(12) 2.18(3) 2.887(3) 141(3) 2_665
O4W H2W4 O4 0.845(12) 1.899(13) 2.742(3) 176(4) 1_465

_diffrn_measured_fraction_theta_max 0.902
_diffrn_reflns_theta_full        30.49
_diffrn_measured_fraction_theta_full 0.902
_refine_diff_density_max         1.509
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.121

####END

data_2
_database_code_depnum_ccdc_archive 'CCDC 677290'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            8
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H9 La N2 O10'
_chemical_formula_sum            'C14 H9 La N2 O10'
_chemical_formula_weight         504.14

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'
La La -0.2871 2.4523 '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                   7.2471(5)
_cell_length_b                   9.9563(6)
_cell_length_c                   11.0922(7)
_cell_angle_alpha                71.4320(10)
_cell_angle_beta                 75.0060(10)
_cell_angle_gamma                78.6650(10)
_cell_volume                     727.14(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             488
_exptl_absorpt_coefficient_mu    3.007
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7375
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      153(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'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5729
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2554
_reflns_number_gt                2465
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXTL version 5.1 (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXTL version 5.1 (Sheldrick, 1998)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
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)+(0.0328P)²+2.2338P] where P=(Fo²+2Fc²)/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         2554
_refine_ls_number_parameters     259
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0728
_refine_ls_wR_factor_gt          0.0718
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_restrained_S_all      1.164
_refine_ls_shift/su_max          0.000
_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
La1 La -0.64962(4) 0.47067(3) 0.26928(2) 0.00944(10) Uani 1 1 d . . .
N1 N -0.7670(5) 0.2385(4) 0.4753(4) 0.0109(8) Uani 1 1 d . . .
C1 C -0.8664(6) 0.2674(5) 0.5853(4) 0.0108(9) Uani 1 1 d . . .
C2 C -0.9510(7) 0.1652(5) 0.6942(4) 0.0131(10) Uani 1 1 d . . .
H2 H -1.0244 0.1903 0.7700 0.016 Uiso 1 1 calc R . .
C3 C -0.9244(7) 0.0263(5) 0.6878(4) 0.0122(9) Uani 1 1 d . . .
C4 C -0.8172(7) -0.0059(5) 0.5745(4) 0.0125(9) Uani 1 1 d . . .
H4 H -0.7956 -0.1012 0.5691 0.015 Uiso 1 1 calc R . .
C5 C -0.7419(7) 0.1034(5) 0.4691(4) 0.0118(9) Uani 1 1 d . . .
C6 C -0.6227(7) 0.0766(5) 0.3470(4) 0.0120(9) Uani 1 1 d . . .
C7 C -0.5804(7) -0.0576(5) 0.3243(4) 0.0123(10) Uani 1 1 d . . .
H7 H -0.6294 -0.1383 0.3894 0.015 Uiso 1 1 calc R . .
C8 C -0.4669(6) -0.0729(5) 0.2068(4) 0.0113(9) Uani 1 1 d . . .
C9 C -0.4003(7) 0.0485(5) 0.1138(5) 0.0126(9) Uani 1 1 d . . .
H9 H -0.3253 0.0429 0.0312 0.015 Uiso 1 1 calc R . .
C10 C -0.4448(7) 0.1772(5) 0.1434(4) 0.0116(9) Uani 1 1 d . . .
N2 N -0.5523(5) 0.1926(4) 0.2567(4) 0.0110(8) Uani 1 1 d . . .
C11 C -0.3733(6) 0.3125(5) 0.0471(4) 0.0120(9) Uani 1 1 d . . .
O1 O -0.3831(5) 0.4147(3) 0.0954(3) 0.0129(7) Uani 1 1 d . . .
O2 O -0.3128(5) 0.3145(3) -0.0683(3) 0.0135(7) Uani 1 1 d . . .
C12 C -0.4151(7) -0.2200(5) 0.1828(4) 0.0124(10) Uani 1 1 d . . .
O3 O -0.2899(5) -0.2353(3) 0.0839(3) 0.0162(7) Uani 1 1 d . . .
O4 O -0.5034(5) -0.3184(3) 0.2651(3) 0.0156(7) Uani 1 1 d . . .
C13 C -1.0013(7) -0.0953(5) 0.8001(5) 0.0132(10) Uani 1 1 d D . .
O5 O -0.9566(5) -0.2175(3) 0.7923(3) 0.0193(8) Uani 1 1 d . . .
O6 O -1.1102(5) -0.0572(4) 0.8976(3) 0.0224(8) Uani 1 1 d D . .
H6 H -1.147(8) -0.128(4) 0.955(3) 0.027 Uiso 1 1 d D . .
C14 C -0.8740(6) 0.4188(5) 0.5880(4) 0.0104(9) Uani 1 1 d . . .
O7 O -0.9938(5) 0.4607(3) 0.6758(3) 0.0142(7) Uani 1 1 d . . .
O8 O -0.7549(5) 0.4936(3) 0.5003(3) 0.0134(7) Uani 1 1 d . . .
O1W O -0.8067(5) 0.4144(4) 0.1187(3) 0.0170(7) Uani 1 1 d D . .
H1W1 H -0.886(6) 0.362(5) 0.125(5) 0.020 Uiso 1 1 d D . .
H2W1 H -0.762(7) 0.445(5) 0.0411(18) 0.020 Uiso 1 1 d D . .
O2W O -0.3559(5) 0.3536(4) 0.3717(3) 0.0170(7) Uani 1 1 d D . .
H2W2 H -0.256(4) 0.334(6) 0.322(4) 0.020 Uiso 1 1 d D . .
H1W2 H -0.330(7) 0.402(5) 0.412(5) 0.020 Uiso 1 1 d 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
La1 O1 2.469(3) . ?
La1 O1W 2.496(3) . ?
La1 O7 2.504(3) 2_366 ?
La1 O4 2.515(3) 1_565 ?
La1 O8 2.548(3) . ?
La1 O2W 2.571(4) . ?
La1 O2 2.582(3) 2_465 ?
La1 N2 2.759(4) . ?
La1 N1 2.774(4) . ?
N1 C1 1.333(6) . ?
N1 C5 1.343(6) . ?
C1 C2 1.396(6) . ?
C1 C14 1.507(6) . ?
C2 C3 1.380(7) . ?
C3 C4 1.392(6) . ?
C3 C13 1.508(6) . ?
C4 C5 1.393(6) . ?
C5 C6 1.479(6) . ?
C6 N2 1.352(6) . ?
C6 C7 1.399(6) . ?
C7 C8 1.386(6) . ?
C8 C9 1.391(6) . ?
C8 C12 1.529(6) . ?
C9 C10 1.380(6) . ?
C10 N2 1.333(6) . ?
C10 C11 1.515(6) . ?
C11 O2 1.236(6) . ?
C11 O1 1.275(6) . ?
O2 La1 2.582(3) 2_465 ?
C12 O4 1.256(6) . ?
C12 O3 1.260(6) . ?
O4 La1 2.515(3) 1_545 ?
C13 O5 1.220(6) . ?
C13 O6 1.281(6) . ?
C14 O7 1.246(6) . ?
C14 O8 1.266(6) . ?
O7 La1 2.504(3) 2_366 ?

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 La1 O1W 74.74(11) . . ?
O1 La1 O7 143.01(11) . 2_366 ?
O1W La1 O7 70.00(11) . 2_366 ?
O1 La1 O4 91.73(10) . 1_565 ?
O1W La1 O4 135.09(11) . 1_565 ?
O7 La1 O4 105.29(11) 2_366 1_565 ?
O1 La1 O8 147.52(11) . . ?
O1W La1 O8 135.17(11) . . ?
O7 La1 O8 69.46(11) 2_366 . ?
O4 La1 O8 74.55(10) 1_565 . ?
O1 La1 O2W 72.45(11) . . ?
O1W La1 O2W 134.24(11) . . ?
O7 La1 O2W 142.80(11) 2_366 . ?
O4 La1 O2W 77.01(11) 1_565 . ?
O8 La1 O2W 75.78(11) . . ?
O1 La1 O2 76.14(10) . 2_465 ?
O1W La1 O2 67.94(11) . 2_465 ?
O7 La1 O2 80.56(10) 2_366 2_465 ?
O4 La1 O2 67.26(10) 1_565 2_465 ?
O8 La1 O2 122.21(10) . 2_465 ?
O2W La1 O2 130.97(11) . 2_465 ?
O1 La1 N2 60.53(10) . . ?
O1W La1 N2 66.40(12) . . ?
O7 La1 N2 112.66(11) 2_366 . ?
O4 La1 N2 141.72(11) 1_565 . ?
O8 La1 N2 113.96(11) . . ?
O2W La1 N2 69.96(11) . . ?
O2 La1 N2 123.05(10) 2_465 . ?
O1 La1 N1 115.68(10) . . ?
O1W La1 N1 93.54(11) . . ?
O7 La1 N1 77.88(11) 2_366 . ?
O4 La1 N1 130.12(11) 1_565 . ?
O8 La1 N1 59.83(10) . . ?
O2W La1 N1 73.45(11) . . ?
O2 La1 N1 155.46(11) 2_465 . ?
N2 La1 N1 57.09(11) . . ?
C1 N1 C5 118.7(4) . . ?
C1 N1 La1 116.2(3) . . ?
C5 N1 La1 124.9(3) . . ?
N1 C1 C2 123.5(4) . . ?
N1 C1 C14 115.3(4) . . ?
C2 C1 C14 121.1(4) . . ?
C3 C2 C1 117.6(4) . . ?
C2 C3 C4 119.4(4) . . ?
C2 C3 C13 123.0(4) . . ?
C4 C3 C13 117.6(4) . . ?
C3 C4 C5 119.2(4) . . ?
N1 C5 C4 121.5(4) . . ?
N1 C5 C6 116.2(4) . . ?
C4 C5 C6 122.2(4) . . ?
N2 C6 C7 121.2(4) . . ?
N2 C6 C5 115.0(4) . . ?
C7 C6 C5 123.9(4) . . ?
C8 C7 C6 119.9(4) . . ?
C7 C8 C9 118.0(4) . . ?
C7 C8 C12 120.2(4) . . ?
C9 C8 C12 121.8(4) . . ?
C10 C9 C8 119.1(4) . . ?
N2 C10 C9 123.3(4) . . ?
N2 C10 C11 115.2(4) . . ?
C9 C10 C11 121.5(4) . . ?
C10 N2 C6 118.5(4) . . ?
C10 N2 La1 115.1(3) . . ?
C6 N2 La1 125.8(3) . . ?
O2 C11 O1 126.4(4) . . ?
O2 C11 C10 118.4(4) . . ?
O1 C11 C10 115.2(4) . . ?
C11 O1 La1 124.0(3) . . ?
C11 O2 La1 126.8(3) . 2_465 ?
O4 C12 O3 124.4(4) . . ?
O4 C12 C8 116.4(4) . . ?
O3 C12 C8 119.2(4) . . ?
C12 O4 La1 138.4(3) . 1_545 ?
O5 C13 O6 126.0(4) . . ?
O5 C13 C3 119.6(4) . . ?
O6 C13 C3 114.4(4) . . ?
O7 C14 O8 125.0(4) . . ?
O7 C14 C1 118.4(4) . . ?
O8 C14 C1 116.6(4) . . ?
C14 O7 La1 137.4(3) . 2_366 ?
C14 O8 La1 123.0(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 La1 N1 C1 160.6(3) . . . . ?
O1W La1 N1 C1 -124.6(3) . . . . ?
O7 La1 N1 C1 -55.9(3) 2_366 . . . ?
O4 La1 N1 C1 44.0(4) 1_565 . . . ?
O8 La1 N1 C1 17.2(3) . . . . ?
O2W La1 N1 C1 100.1(3) . . . . ?
O2 La1 N1 C1 -85.0(4) 2_465 . . . ?
N2 La1 N1 C1 176.6(4) . . . . ?
O1 La1 N1 C5 -23.9(4) . . . . ?
O1W La1 N1 C5 50.9(4) . . . . ?
O7 La1 N1 C5 119.5(4) 2_366 . . . ?
O4 La1 N1 C5 -140.6(3) 1_565 . . . ?
O8 La1 N1 C5 -167.3(4) . . . . ?
O2W La1 N1 C5 -84.4(4) . . . . ?
O2 La1 N1 C5 90.5(4) 2_465 . . . ?
N2 La1 N1 C5 -7.9(3) . . . . ?
C5 N1 C1 C2 -1.8(7) . . . . ?
La1 N1 C1 C2 174.0(3) . . . . ?
C5 N1 C1 C14 175.2(4) . . . . ?
La1 N1 C1 C14 -9.0(5) . . . . ?
N1 C1 C2 C3 2.0(7) . . . . ?
C14 C1 C2 C3 -174.8(4) . . . . ?
C1 C2 C3 C4 -0.5(7) . . . . ?
C1 C2 C3 C13 177.6(4) . . . . ?
C2 C3 C4 C5 -1.1(7) . . . . ?
C13 C3 C4 C5 -179.3(4) . . . . ?
C1 N1 C5 C4 0.0(7) . . . . ?
La1 N1 C5 C4 -175.4(3) . . . . ?
C1 N1 C5 C6 -177.2(4) . . . . ?
La1 N1 C5 C6 7.4(6) . . . . ?
C3 C4 C5 N1 1.4(7) . . . . ?
C3 C4 C5 C6 178.5(4) . . . . ?
N1 C5 C6 N2 0.5(6) . . . . ?
C4 C5 C6 N2 -176.7(4) . . . . ?
N1 C5 C6 C7 179.4(4) . . . . ?
C4 C5 C6 C7 2.2(7) . . . . ?
N2 C6 C7 C8 -1.0(7) . . . . ?
C5 C6 C7 C8 -179.8(4) . . . . ?
C6 C7 C8 C9 -0.8(7) . . . . ?
C6 C7 C8 C12 178.2(4) . . . . ?
C7 C8 C9 C10 1.9(7) . . . . ?
C12 C8 C9 C10 -177.1(4) . . . . ?
C8 C9 C10 N2 -1.2(7) . . . . ?
C8 C9 C10 C11 178.8(4) . . . . ?
C9 C10 N2 C6 -0.6(7) . . . . ?
C11 C10 N2 C6 179.4(4) . . . . ?
C9 C10 N2 La1 -172.5(4) . . . . ?
C11 C10 N2 La1 7.4(5) . . . . ?
C7 C6 N2 C10 1.7(7) . . . . ?
C5 C6 N2 C10 -179.4(4) . . . . ?
C7 C6 N2 La1 172.7(3) . . . . ?
C5 C6 N2 La1 -8.4(6) . . . . ?
O1 La1 N2 C10 -16.9(3) . . . . ?
O1W La1 N2 C10 68.3(3) . . . . ?
O7 La1 N2 C10 122.4(3) 2_366 . . . ?
O4 La1 N2 C10 -65.6(4) 1_565 . . . ?
O8 La1 N2 C10 -160.9(3) . . . . ?
O2W La1 N2 C10 -97.6(3) . . . . ?
O2 La1 N2 C10 29.0(4) 2_465 . . . ?
N1 La1 N2 C10 179.6(4) . . . . ?
O1 La1 N2 C6 171.8(4) . . . . ?
O1W La1 N2 C6 -102.9(4) . . . . ?
O7 La1 N2 C6 -48.9(4) 2_366 . . . ?
O4 La1 N2 C6 123.1(3) 1_565 . . . ?
O8 La1 N2 C6 27.8(4) . . . . ?
O2W La1 N2 C6 91.2(4) . . . . ?
O2 La1 N2 C6 -142.3(3) 2_465 . . . ?
N1 La1 N2 C6 8.4(3) . . . . ?
N2 C10 C11 O2 -163.4(4) . . . . ?
C9 C10 C11 O2 16.6(7) . . . . ?
N2 C10 C11 O1 16.4(6) . . . . ?
C9 C10 C11 O1 -163.6(4) . . . . ?
O2 C11 O1 La1 142.2(4) . . . . ?
C10 C11 O1 La1 -37.6(5) . . . . ?
O1W La1 O1 C11 -41.8(3) . . . . ?
O7 La1 O1 C11 -59.7(4) 2_366 . . . ?
O4 La1 O1 C11 -178.3(3) 1_565 . . . ?
O8 La1 O1 C11 118.3(3) . . . . ?
O2W La1 O1 C11 105.9(3) . . . . ?
O2 La1 O1 C11 -112.3(4) 2_465 . . . ?
N2 La1 O1 C11 29.4(3) . . . . ?
N1 La1 O1 C11 44.8(4) . . . . ?
O1 C11 O2 La1 -35.2(7) . . . 2_465 ?
C10 C11 O2 La1 144.6(3) . . . 2_465 ?
C7 C8 C12 O4 10.5(7) . . . . ?
C9 C8 C12 O4 -170.6(4) . . . . ?
C7 C8 C12 O3 -169.7(4) . . . . ?
C9 C8 C12 O3 9.2(7) . . . . ?
O3 C12 O4 La1 -38.9(8) . . . 1_545 ?
C8 C12 O4 La1 140.9(4) . . . 1_545 ?
C2 C3 C13 O5 -172.8(5) . . . . ?
C4 C3 C13 O5 5.3(7) . . . . ?
C2 C3 C13 O6 6.8(7) . . . . ?
C4 C3 C13 O6 -175.1(4) . . . . ?
N1 C1 C14 O7 166.0(4) . . . . ?
C2 C1 C14 O7 -16.9(6) . . . . ?
N1 C1 C14 O8 -14.7(6) . . . . ?
C2 C1 C14 O8 162.4(4) . . . . ?
O8 C14 O7 La1 107.2(5) . . . 2_366 ?
C1 C14 O7 La1 -73.6(6) . . . 2_366 ?
O7 C14 O8 La1 -145.6(4) . . . . ?
C1 C14 O8 La1 35.1(5) . . . . ?
O1 La1 O8 C14 -119.0(3) . . . . ?
O1W La1 O8 C14 33.3(4) . . . . ?
O7 La1 O8 C14 59.8(3) 2_366 . . . ?
O4 La1 O8 C14 173.1(4) 1_565 . . . ?
O2W La1 O8 C14 -106.7(4) . . . . ?
O2 La1 O8 C14 123.5(3) 2_465 . . . ?
N2 La1 O8 C14 -46.7(4) . . . . ?
N1 La1 O8 C14 -27.8(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O6 H6 O3 0.824(19) 1.72(2) 2.509(4) 161(5) 1_456
O1W H1W1 O5 0.819(14) 1.87(2) 2.641(4) 157(5) 2_356
O1W H2W1 O1 0.816(14) 1.94(3) 2.661(4) 147(5) 2_465
O2W H2W2 O5 0.815(14) 2.14(2) 2.917(5) 160(5) 2_456
O2W H1W2 O8 0.820(14) 1.907(16) 2.724(5) 175(5) 2_466

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.806
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.135

####END

data_3
_database_code_depnum_ccdc_archive 'CCDC 677291'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            9
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H10 Eu N2 O12.50'
_chemical_formula_sum            'C14 H10 Eu N2 O12.50'
_chemical_formula_weight         558.20

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'
Eu Eu -0.1578 3.6682 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pnma

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

_cell_length_a                   21.9566(10)
_cell_length_b                   6.6188(3)
_cell_length_c                   11.3669(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1651.91(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1084
_exptl_absorpt_coefficient_mu    3.877
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7820
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      153(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'
_diffrn_measurement_method       'Omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12755
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         24.99
_reflns_number_total             1596
_reflns_number_gt                1570
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXTL version 5.1 (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXTL version 5.1 (Sheldrick, 1998)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
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)+(0.0000P)²+62.2209P] where P=(Fo²+2Fc²)/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         1596
_refine_ls_number_parameters     155
_refine_ls_number_restraints     136
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0619
_refine_ls_wR_factor_ref         0.1544
_refine_ls_wR_factor_gt          0.1542
_refine_ls_goodness_of_fit_ref   1.423
_refine_ls_restrained_S_all      1.364
_refine_ls_shift/su_max          0.000
_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 0.13148(3) -0.7500 0.46646(6) 0.0154(3) Uani 1 2 d S . .
N1 N 0.2448(6) -0.7500 0.4223(11) 0.021(3) Uani 1 2 d SU . .
C1 C 0.2625(7) -0.7500 0.3093(13) 0.020(4) Uani 1 2 d SU . .
C2 C 0.3226(7) -0.7500 0.2749(14) 0.029(4) Uani 1 2 d SU . .
H2A H 0.3336 -0.7500 0.1941 0.035 Uiso 1 2 calc SR . .
C3 C 0.3670(8) -0.7500 0.3631(14) 0.039(5) Uani 1 2 d SU . .
C4 C 0.3487(7) -0.7500 0.4815(15) 0.038(5) Uani 1 2 d SU . .
H4A H 0.3782 -0.7500 0.5427 0.046 Uiso 1 2 calc SR . .
C5 C 0.2870(7) -0.7500 0.5075(14) 0.025(4) Uani 1 2 d SU . .
C6 C 0.2641(7) -0.7500 0.6295(14) 0.023(4) Uani 1 2 d SU . .
C7 C 0.3016(6) -0.7500 0.7267(12) 0.010(3) Uiso 1 2 d SU . .
H7A H 0.3445 -0.7500 0.7168 0.012 Uiso 1 2 calc SR . .
C8 C 0.2769(7) -0.7500 0.8392(13) 0.018(3) Uani 1 2 d SU . .
C9 C 0.2143(7) -0.7500 0.8502(15) 0.025(4) Uani 1 2 d SU . .
H9A H 0.1960 -0.7500 0.9259 0.030 Uiso 1 2 calc SR . .
C10 C 0.1784(7) -0.7500 0.7494(13) 0.018(3) Uani 1 2 d SU . .
N2 N 0.2031(5) -0.7500 0.6403(11) 0.016(3) Uani 1 2 d SU . .
C11 C 0.1093(8) -0.785(5) 0.7506(16) 0.018(7) Uani 0.50 1 d PU . .
O1 O 0.0839(5) -0.7500 0.6510(10) 0.030(3) Uani 1 2 d SU . .
O2 O 0.0829(6) -0.7500 0.8457(12) 0.035(3) Uiso 1 2 d SU . .
C12 C 0.3205(7) -0.7500 0.9430(13) 0.022(4) Uani 1 2 d SU . .
O3 O 0.3377(4) -0.9165(14) 0.9806(7) 0.028(2) Uani 1 1 d U . .
C13 C 0.4330(9) -0.7500 0.3346(17) 0.031(4) Uiso 1 2 d SDU . .
O4 O 0.4675(7) -0.7500 0.4264(13) 0.043(4) Uiso 1 2 d SDU . .
H4 H 0.5049(11) -0.7500 0.410(6) 0.064 Uiso 1 2 d SD . .
O5 O 0.4515(7) -0.7500 0.2322(14) 0.047(4) Uiso 1 2 d SU . .
C14 C 0.2102(7) -0.7500 0.2218(13) 0.017(3) Uani 1 2 d SU . .
O6 O 0.2222(5) -0.7500 0.1155(9) 0.024(3) Uani 1 2 d SU . .
O7 O 0.1567(4) -0.7500 0.2650(9) 0.017(2) Uani 1 2 d SU . .
O1W O 0.0438(4) -0.9614(16) 0.4052(11) 0.050(3) Uani 1 1 d . . .
O2W O 0.0405(6) -0.331(2) 0.2232(11) 0.013(3) Uiso 0.50 1 d P . .
O3W O 0.0792(6) -0.832(2) 1.0856(11) 0.012(3) Uiso 0.50 1 d P . .


_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 O3 2.314(9) 7_665 ?
Eu1 O3 2.314(9) 2_534 ?
Eu1 O1 2.343(11) . ?
Eu1 O7 2.356(10) . ?
Eu1 O1W 2.480(9) . ?
Eu1 O1W 2.480(9) 8_545 ?
Eu1 N2 2.525(12) . ?
Eu1 N1 2.537(12) . ?
N1 C5 1.34(2) . ?
N1 C1 1.342(19) . ?
C1 C2 1.38(2) . ?
C1 C14 1.519(19) . ?
C2 C3 1.40(2) . ?
C2 H2A 0.9500 . ?
C3 C4 1.40(2) . ?
C3 C13 1.48(3) . ?
C4 C5 1.39(2) . ?
C4 H4A 0.9500 . ?
C5 C6 1.48(2) . ?
C6 N2 1.346(19) . ?
C6 C7 1.38(2) . ?
C7 C8 1.39(2) . ?
C7 H7A 0.9500 . ?
C8 C9 1.38(2) . ?
C8 C12 1.52(2) . ?
C9 C10 1.39(2) . ?
C9 H9A 0.9500 . ?
C10 N2 1.352(19) . ?
C10 C11 1.53(2) 8_545 ?
C10 C11 1.53(2) . ?
C11 C11 0.46(7) 8_545 ?
C11 O2 1.25(2) . ?
C11 O1 1.28(2) . ?
O1 C11 1.28(2) 8_545 ?
O2 C11 1.25(2) 8_545 ?
C12 O3 1.241(11) 8_545 ?
C12 O3 1.241(11) . ?
O3 Eu1 2.314(9) 2_535 ?
C13 O5 1.23(2) . ?
C13 O4 1.29(2) . ?
O4 H4 0.84(2) . ?
C14 O6 1.236(18) . ?
C14 O7 1.273(18) . ?
O2W O2W 1.08(3) 8 ?
O3W O3W 1.09(3) 8_545 ?

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
O3 Eu1 O3 145.0(4) 7_665 2_534 ?
O3 Eu1 O1 93.9(2) 7_665 . ?
O3 Eu1 O1 93.9(2) 2_534 . ?
O3 Eu1 O7 89.9(2) 7_665 . ?
O3 Eu1 O7 89.9(2) 2_534 . ?
O1 Eu1 O7 167.1(4) . . ?
O3 Eu1 O1W 141.7(3) 7_665 . ?
O3 Eu1 O1W 73.1(3) 2_534 . ?
O1 Eu1 O1W 84.5(4) . . ?
O7 Eu1 O1W 84.8(3) . . ?
O3 Eu1 O1W 73.1(3) 7_665 8_545 ?
O3 Eu1 O1W 141.7(3) 2_534 8_545 ?
O1 Eu1 O1W 84.5(4) . 8_545 ?
O7 Eu1 O1W 84.8(3) . 8_545 ?
O1W Eu1 O1W 68.7(4) . 8_545 ?
O3 Eu1 N2 76.3(2) 7_665 . ?
O3 Eu1 N2 76.3(2) 2_534 . ?
O1 Eu1 N2 65.0(4) . . ?
O7 Eu1 N2 127.9(4) . . ?
O1W Eu1 N2 134.7(3) . . ?
O1W Eu1 N2 134.7(3) 8_545 . ?
O3 Eu1 N1 74.1(2) 7_665 . ?
O3 Eu1 N1 74.1(2) 2_534 . ?
O1 Eu1 N1 127.9(4) . . ?
O7 Eu1 N1 65.0(4) . . ?
O1W Eu1 N1 134.9(3) . . ?
O1W Eu1 N1 134.9(3) 8_545 . ?
N2 Eu1 N1 62.9(4) . . ?
C5 N1 C1 119.3(13) . . ?
C5 N1 Eu1 122.4(10) . . ?
C1 N1 Eu1 118.3(9) . . ?
N1 C1 C2 123.4(14) . . ?
N1 C1 C14 114.0(13) . . ?
C2 C1 C14 122.6(14) . . ?
C1 C2 C3 117.7(15) . . ?
C1 C2 H2A 121.1 . . ?
C3 C2 H2A 121.1 . . ?
C2 C3 C4 119.2(16) . . ?
C2 C3 C13 121.6(15) . . ?
C4 C3 C13 119.2(15) . . ?
C5 C4 C3 118.9(15) . . ?
C5 C4 H4A 120.6 . . ?
C3 C4 H4A 120.6 . . ?
N1 C5 C4 121.5(14) . . ?
N1 C5 C6 116.3(13) . . ?
C4 C5 C6 122.2(14) . . ?
N2 C6 C7 121.4(14) . . ?
N2 C6 C5 115.2(14) . . ?
C7 C6 C5 123.4(14) . . ?
C6 C7 C8 120.4(14) . . ?
C6 C7 H7A 119.8 . . ?
C8 C7 H7A 119.8 . . ?
C9 C8 C7 118.2(14) . . ?
C9 C8 C12 123.8(14) . . ?
C7 C8 C12 118.0(13) . . ?
C8 C9 C10 119.3(15) . . ?
C8 C9 H9A 120.3 . . ?
C10 C9 H9A 120.3 . . ?
N2 C10 C9 121.9(15) . . ?
N2 C10 C11 113.9(14) . 8_545 ?
C9 C10 C11 123.5(14) . 8_545 ?
N2 C10 C11 113.9(14) . . ?
C9 C10 C11 123.5(14) . . ?
C6 N2 C10 118.8(13) . . ?
C6 N2 Eu1 123.2(10) . . ?
C10 N2 Eu1 117.9(10) . . ?
C11 C11 O2 79.3(16) 8_545 . ?
C11 C11 O1 79.6(15) 8_545 . ?
O2 C11 O1 121.9(17) . . ?
C11 C11 C10 81.3(13) 8_545 . ?
O2 C11 C10 116.1(17) . . ?
O1 C11 C10 113.2(16) . . ?
C11 O1 Eu1 126.6(10) . . ?
C11 O1 Eu1 126.6(10) 8_545 . ?
O3 C12 O3 125.4(14) 8_545 . ?
O3 C12 C8 117.3(7) 8_545 . ?
O3 C12 C8 117.3(7) . . ?
C12 O3 Eu1 155.8(8) . 2_535 ?
O5 C13 O4 124.8(18) . . ?
O5 C13 C3 121.9(17) . . ?
O4 C13 C3 113.4(16) . . ?
C13 O4 H4 113(5) . . ?
O6 C14 O7 124.9(13) . . ?
O6 C14 C1 118.7(13) . . ?
O7 C14 C1 116.4(12) . . ?
C14 O7 Eu1 126.3(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Eu1 N1 C5 82.5(2) 7_665 . . . ?
O3 Eu1 N1 C5 -82.5(2) 2_534 . . . ?
O1 Eu1 N1 C5 0.000(1) . . . . ?
O7 Eu1 N1 C5 180.000(1) . . . . ?
O1W Eu1 N1 C5 -127.2(4) . . . . ?
O1W Eu1 N1 C5 127.2(4) 8_545 . . . ?
N2 Eu1 N1 C5 0.000(1) . . . . ?
O3 Eu1 N1 C1 -97.5(2) 7_665 . . . ?
O3 Eu1 N1 C1 97.5(2) 2_534 . . . ?
O1 Eu1 N1 C1 180.0 . . . . ?
O7 Eu1 N1 C1 0.0 . . . . ?
O1W Eu1 N1 C1 52.8(4) . . . . ?
O1W Eu1 N1 C1 -52.8(4) 8_545 . . . ?
N2 Eu1 N1 C1 180.000(1) . . . . ?
C5 N1 C1 C2 0.000(2) . . . . ?
Eu1 N1 C1 C2 180.0 . . . . ?
C5 N1 C1 C14 180.000(1) . . . . ?
Eu1 N1 C1 C14 0.000(1) . . . . ?
N1 C1 C2 C3 0.000(2) . . . . ?
C14 C1 C2 C3 180.000(1) . . . . ?
C1 C2 C3 C4 0.000(2) . . . . ?
C1 C2 C3 C13 180.000(1) . . . . ?
C2 C3 C4 C5 0.000(2) . . . . ?
C13 C3 C4 C5 180.000(2) . . . . ?
C1 N1 C5 C4 0.000(2) . . . . ?
Eu1 N1 C5 C4 180.000(2) . . . . ?
C1 N1 C5 C6 180.000(2) . . . . ?
Eu1 N1 C5 C6 0.000(2) . . . . ?
C3 C4 C5 N1 0.000(2) . . . . ?
C3 C4 C5 C6 180.000(2) . . . . ?
N1 C5 C6 N2 0.000(2) . . . . ?
C4 C5 C6 N2 180.000(2) . . . . ?
N1 C5 C6 C7 180.000(2) . . . . ?
C4 C5 C6 C7 0.000(3) . . . . ?
N2 C6 C7 C8 0.000(4) . . . . ?
C5 C6 C7 C8 180.000(3) . . . . ?
C6 C7 C8 C9 0.000(4) . . . . ?
C6 C7 C8 C12 180.000(3) . . . . ?
C7 C8 C9 C10 0.000(4) . . . . ?
C12 C8 C9 C10 180.000(3) . . . . ?
C8 C9 C10 N2 0.000(4) . . . . ?
C8 C9 C10 C11 -169.6(15) . . . 8_545 ?
C8 C9 C10 C11 169.6(15) . . . . ?
C7 C6 N2 C10 0.000(4) . . . . ?
C5 C6 N2 C10 180.000(3) . . . . ?
C7 C6 N2 Eu1 180.000(2) . . . . ?
C5 C6 N2 Eu1 0.000(2) . . . . ?
C9 C10 N2 C6 0.000(4) . . . . ?
C11 C10 N2 C6 170.5(14) 8_545 . . . ?
C11 C10 N2 C6 -170.5(14) . . . . ?
C9 C10 N2 Eu1 180.000(3) . . . . ?
C11 C10 N2 Eu1 -9.5(14) 8_545 . . . ?
C11 C10 N2 Eu1 9.5(14) . . . . ?
O3 Eu1 N2 C6 -79.0(2) 7_665 . . . ?
O3 Eu1 N2 C6 79.0(2) 2_534 . . . ?
O1 Eu1 N2 C6 180.000(2) . . . . ?
O7 Eu1 N2 C6 0.000(2) . . . . ?
O1W Eu1 N2 C6 127.5(4) . . . . ?
O1W Eu1 N2 C6 -127.5(4) 8_545 . . . ?
N1 Eu1 N2 C6 0.000(2) . . . . ?
O3 Eu1 N2 C10 101.0(2) 7_665 . . . ?
O3 Eu1 N2 C10 -101.0(2) 2_534 . . . ?
O1 Eu1 N2 C10 0.000(2) . . . . ?
O7 Eu1 N2 C10 180.000(2) . . . . ?
O1W Eu1 N2 C10 -52.5(4) . . . . ?
O1W Eu1 N2 C10 52.5(4) 8_545 . . . ?
N1 Eu1 N2 C10 180.000(2) . . . . ?
N2 C10 C11 C11 -93.9(6) . . . 8_545 ?
C9 C10 C11 C11 95.8(9) . . . 8_545 ?
N2 C10 C11 O2 -167.4(18) . . . . ?
C9 C10 C11 O2 22(3) . . . . ?
C11 C10 C11 O2 -74(2) 8_545 . . . ?
N2 C10 C11 O1 -19(3) . . . . ?
C9 C10 C11 O1 170.5(13) . . . . ?
C11 C10 C11 O1 75(2) 8_545 . . . ?
O2 C11 O1 C11 70(3) . . . 8_545 ?
C10 C11 O1 C11 -76(2) . . . 8_545 ?
C11 C11 O1 Eu1 97.8(12) 8_545 . . . ?
O2 C11 O1 Eu1 168.2(16) . . . . ?
C10 C11 O1 Eu1 22(3) . . . . ?
O3 Eu1 O1 C11 -85.9(19) 7_665 . . . ?
O3 Eu1 O1 C11 60.0(19) 2_534 . . . ?
O7 Eu1 O1 C11 167.0(19) . . . . ?
O1W Eu1 O1 C11 132.5(19) . . . . ?
O1W Eu1 O1 C11 -158.4(19) 8_545 . . . ?
N2 Eu1 O1 C11 -13.0(19) . . . . ?
N1 Eu1 O1 C11 -13.0(19) . . . . ?
O3 Eu1 O1 C11 -60.0(19) 7_665 . . 8_545 ?
O3 Eu1 O1 C11 85.9(19) 2_534 . . 8_545 ?
O7 Eu1 O1 C11 -167.0(19) . . . 8_545 ?
O1W Eu1 O1 C11 158.4(19) . . . 8_545 ?
O1W Eu1 O1 C11 -132.5(19) 8_545 . . 8_545 ?
N2 Eu1 O1 C11 13.0(19) . . . 8_545 ?
N1 Eu1 O1 C11 13.0(19) . . . 8_545 ?
O1 C11 O2 C11 -71(3) . . . 8_545 ?
C10 C11 O2 C11 75(2) . . . 8_545 ?
C9 C8 C12 O3 -91.2(12) . . . 8_545 ?
C7 C8 C12 O3 88.8(12) . . . 8_545 ?
C9 C8 C12 O3 91.2(12) . . . . ?
C7 C8 C12 O3 -88.8(12) . . . . ?
O3 C12 O3 Eu1 -139.6(12) 8_545 . . 2_535 ?
C8 C12 O3 Eu1 38(3) . . . 2_535 ?
C2 C3 C13 O5 0.000(2) . . . . ?
C4 C3 C13 O5 180.000(2) . . . . ?
C2 C3 C13 O4 180.000(1) . . . . ?
C4 C3 C13 O4 0.000(2) . . . . ?
N1 C1 C14 O6 180.000(1) . . . . ?
C2 C1 C14 O6 0.000(1) . . . . ?
N1 C1 C14 O7 0.000(1) . . . . ?
C2 C1 C14 O7 180.0 . . . . ?
O6 C14 O7 Eu1 180.0 . . . . ?
C1 C14 O7 Eu1 0.0 . . . . ?
O3 Eu1 O7 C14 72.5(2) 7_665 . . . ?
O3 Eu1 O7 C14 -72.5(2) 2_534 . . . ?
O1 Eu1 O7 C14 180.000(1) . . . . ?
O1W Eu1 O7 C14 -145.5(2) . . . . ?
O1W Eu1 O7 C14 145.5(2) 8_545 . . . ?
N2 Eu1 O7 C14 0.0 . . . . ?
N1 Eu1 O7 C14 0.0 . . . . ?

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
O4 H4 O3W 0.84(2) 1.72(3) 2.517(19) 157(4) 6_657
O4 H4 O3W 0.84(2) 1.72(3) 2.517(19) 157(4) 3_536

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         2.197
_refine_diff_density_min         -1.749
_refine_diff_density_rms         0.260

####END

data_5
_database_code_depnum_ccdc_archive 'CCDC 677292'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            11
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H6 Eu N2 O9, C2 H8 N'
_chemical_formula_sum            'C16 H14 Eu N3 O9'
_chemical_formula_weight         544.26

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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   8.2797(4)
_cell_length_b                   16.7532(9)
_cell_length_c                   12.7089(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.5780(10)
_cell_angle_gamma                90.00
_cell_volume                     1747.47(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1064
_exptl_absorpt_coefficient_mu    3.650
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7486
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      153(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'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13473
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3064
_reflns_number_gt                2955
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXTL version 5.1 (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXTL version 5.1 (Sheldrick, 1998)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
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)+(0.0151P)²+2.0737P] where P=(Fo²+2Fc²)/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         3064
_refine_ls_number_parameters     278
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0172
_refine_ls_R_factor_gt           0.0164
_refine_ls_wR_factor_ref         0.0404
_refine_ls_wR_factor_gt          0.0400
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.104
_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 0.413742(13) 0.728233(6) 0.410989(8) 0.01070(5) Uani 1 1 d . . .
N1 N 0.4365(2) 0.61344(11) 0.27894(15) 0.0126(4) Uani 1 1 d . . .
C1 C 0.5052(3) 0.63325(14) 0.19297(18) 0.0134(5) Uani 1 1 d . . .
C2 C 0.5719(3) 0.57731(14) 0.13180(18) 0.0135(5) Uani 1 1 d . . .
H2 H 0.6224 0.5934 0.0723 0.016 Uiso 1 1 calc R . .
C3 C 0.5640(3) 0.49719(14) 0.15828(18) 0.0130(5) Uani 1 1 d . . .
C4 C 0.4840(3) 0.47539(13) 0.24390(17) 0.0122(5) Uani 1 1 d . . .
H4 H 0.4713 0.4208 0.2612 0.015 Uiso 1 1 calc R . .
C5 C 0.4234(3) 0.53547(14) 0.30329(18) 0.0117(5) Uani 1 1 d . . .
C6 C 0.3420(3) 0.52134(14) 0.40040(18) 0.0120(5) Uani 1 1 d . . .
C7 C 0.3097(3) 0.44593(14) 0.43826(18) 0.0134(5) Uani 1 1 d . . .
H7 H 0.3411 0.3992 0.4038 0.016 Uiso 1 1 calc R . .
C8 C 0.2299(3) 0.44049(14) 0.52833(18) 0.0133(5) Uani 1 1 d . . .
C9 C 0.1794(3) 0.51001(14) 0.57301(18) 0.0132(5) Uani 1 1 d . . .
H9 H 0.1173 0.5078 0.6307 0.016 Uiso 1 1 calc R . .
C10 C 0.2205(3) 0.58249(14) 0.53263(18) 0.0128(5) Uani 1 1 d . . .
N2 N 0.3042(2) 0.58875(12) 0.44972(15) 0.0125(4) Uani 1 1 d . . .
C11 C 0.1704(3) 0.66108(14) 0.57848(18) 0.0130(5) Uani 1 1 d . . .
C12 C 0.2020(3) 0.36085(15) 0.58006(18) 0.0145(5) Uani 1 1 d . . .
O1 O 0.2195(2) 0.72378(9) 0.53564(13) 0.0142(4) Uani 1 1 d . . .
O2 O 0.0852(2) 0.65840(10) 0.65112(14) 0.0201(4) Uani 1 1 d . . .
O4 O 0.3129(2) 0.30942(10) 0.57846(13) 0.0161(4) Uani 1 1 d . . .
C13 C 0.6493(3) 0.43663(14) 0.09630(18) 0.0137(5) Uani 1 1 d . . .
O5 O 0.5978(2) 0.36600(11) 0.09413(12) 0.0173(4) Uani 1 1 d . . .
O6 O 0.7628(2) 0.46231(11) 0.05073(16) 0.0259(4) Uani 1 1 d . . .
C14 C 0.5122(3) 0.72205(14) 0.17005(19) 0.0132(5) Uani 1 1 d . . .
O7 O 0.5532(2) 0.74221(11) 0.08233(12) 0.0147(3) Uani 1 1 d . . .
O8 O 0.4768(2) 0.76886(9) 0.24036(13) 0.0160(4) Uani 1 1 d . . .
O1W O 0.1484(2) 0.74124(12) 0.31295(15) 0.0207(4) Uani 1 1 d D . .
H2W1 H 0.068(3) 0.7171(18) 0.326(3) 0.035(10) Uiso 1 1 d D . .
H1W1 H 0.120(4) 0.7683(16) 0.2600(19) 0.027(9) Uiso 1 1 d D . .
N3 N 0.9912(3) 0.35465(17) 0.0129(3) 0.0420(8) Uani 1 1 d . . .
H1N3 H 0.908(4) 0.389(2) 0.024(2) 0.032(8) Uiso 1 1 d . . .
H2N3 H 0.952(4) 0.308(2) 0.027(3) 0.046(10) Uiso 1 1 d . . .
C15 C 1.0306(5) 0.3629(2) -0.0965(3) 0.0607(12) Uani 1 1 d . . .
H15C H 0.9330 0.3521 -0.1470 0.091 Uiso 1 1 calc R . .
H15B H 1.1164 0.3248 -0.1080 0.091 Uiso 1 1 calc R . .
H15A H 1.0686 0.4174 -0.1073 0.091 Uiso 1 1 calc R . .
C16 C 1.1295(4) 0.3708(2) 0.0958(3) 0.0515(10) Uani 1 1 d . . .
H16C H 1.0938 0.3651 0.1660 0.077 Uiso 1 1 calc R . .
H16B H 1.1692 0.4252 0.0876 0.077 Uiso 1 1 calc R . .
H16A H 1.2174 0.3327 0.0891 0.077 Uiso 1 1 calc R . .
O3 O 0.0759(2) 0.35387(11) 0.62158(16) 0.0248(4) 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
Eu1 O5 2.3106(18) 2_655 ?
Eu1 O4 2.3364(16) 3_666 ?
Eu1 O7 2.3784(16) 4_576 ?
Eu1 O1W 2.3887(18) . ?
Eu1 O8 2.3953(16) . ?
Eu1 O1 2.4026(16) . ?
Eu1 N1 2.5756(19) . ?
Eu1 N2 2.578(2) . ?
N1 C1 1.339(3) . ?
N1 C5 1.350(3) . ?
C1 C2 1.378(3) . ?
C1 C14 1.519(3) . ?
C2 C3 1.387(3) . ?
C3 C4 1.395(3) . ?
C3 C13 1.515(3) . ?
C4 C5 1.391(3) . ?
C5 C6 1.501(3) . ?
C6 N2 1.348(3) . ?
C6 C7 1.390(3) . ?
C7 C8 1.398(3) . ?
C8 C9 1.384(3) . ?
C8 C12 1.519(3) . ?
C9 C10 1.378(3) . ?
C10 N2 1.339(3) . ?
C10 C11 1.520(3) . ?
C11 O2 1.234(3) . ?
C11 O1 1.274(3) . ?
C12 O3 1.235(3) . ?
C12 O4 1.261(3) . ?
O4 Eu1 2.3364(16) 3_666 ?
C13 O6 1.244(3) . ?
C13 O5 1.257(3) . ?
O5 Eu1 2.3106(18) 2_645 ?
C14 O8 1.252(3) . ?
C14 O7 1.254(3) . ?
O7 Eu1 2.3784(16) 4_575 ?
N3 C16 1.476(5) . ?
N3 C15 1.476(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Eu1 O4 107.92(6) 2_655 3_666 ?
O5 Eu1 O7 80.28(6) 2_655 4_576 ?
O4 Eu1 O7 69.76(6) 3_666 4_576 ?
O5 Eu1 O1W 82.08(6) 2_655 . ?
O4 Eu1 O1W 150.70(6) 3_666 . ?
O7 Eu1 O1W 139.52(6) 4_576 . ?
O5 Eu1 O8 72.77(5) 2_655 . ?
O4 Eu1 O8 78.66(6) 3_666 . ?
O7 Eu1 O8 129.21(6) 4_576 . ?
O1W Eu1 O8 78.31(6) . . ?
O5 Eu1 O1 91.19(5) 2_655 . ?
O4 Eu1 O1 132.94(6) 3_666 . ?
O7 Eu1 O1 71.89(6) 4_576 . ?
O1W Eu1 O1 72.37(6) . . ?
O8 Eu1 O1 148.28(6) . . ?
O5 Eu1 N1 137.21(6) 2_655 . ?
O4 Eu1 N1 71.47(6) 3_666 . ?
O7 Eu1 N1 133.12(6) 4_576 . ?
O1W Eu1 N1 82.51(6) . . ?
O8 Eu1 N1 65.09(6) . . ?
O1 Eu1 N1 121.28(6) . . ?
O5 Eu1 N2 153.72(6) 2_655 . ?
O4 Eu1 N2 96.14(6) 3_666 . ?
O7 Eu1 N2 98.89(6) 4_576 . ?
O1W Eu1 N2 81.93(6) . . ?
O8 Eu1 N2 123.70(6) . . ?
O1 Eu1 N2 64.08(6) . . ?
N1 Eu1 N2 60.35(6) . . ?
C1 N1 C5 118.9(2) . . ?
C1 N1 Eu1 114.98(15) . . ?
C5 N1 Eu1 123.92(15) . . ?
N1 C1 C2 122.5(2) . . ?
N1 C1 C14 115.5(2) . . ?
C2 C1 C14 122.0(2) . . ?
C1 C2 C3 119.1(2) . . ?
C2 C3 C4 119.0(2) . . ?
C2 C3 C13 118.8(2) . . ?
C4 C3 C13 122.1(2) . . ?
C5 C4 C3 118.4(2) . . ?
N1 C5 C4 122.0(2) . . ?
N1 C5 C6 113.5(2) . . ?
C4 C5 C6 124.4(2) . . ?
N2 C6 C7 122.2(2) . . ?
N2 C6 C5 114.0(2) . . ?
C7 C6 C5 123.7(2) . . ?
C6 C7 C8 118.4(2) . . ?
C9 C8 C7 118.8(2) . . ?
C9 C8 C12 119.3(2) . . ?
C7 C8 C12 121.8(2) . . ?
C10 C9 C8 119.0(2) . . ?
N2 C10 C9 122.7(2) . . ?
N2 C10 C11 115.4(2) . . ?
C9 C10 C11 121.8(2) . . ?
C10 N2 C6 118.4(2) . . ?
C10 N2 Eu1 116.92(15) . . ?
C6 N2 Eu1 124.14(15) . . ?
O2 C11 O1 126.6(2) . . ?
O2 C11 C10 117.9(2) . . ?
O1 C11 C10 115.56(19) . . ?
O3 C12 O4 126.9(2) . . ?
O3 C12 C8 117.0(2) . . ?
O4 C12 C8 116.1(2) . . ?
C11 O1 Eu1 125.92(14) . . ?
C12 O4 Eu1 152.30(16) . 3_666 ?
O6 C13 O5 126.2(2) . . ?
O6 C13 C3 116.3(2) . . ?
O5 C13 C3 117.5(2) . . ?
C13 O5 Eu1 162.53(16) . 2_645 ?
O8 C14 O7 125.6(2) . . ?
O8 C14 C1 117.3(2) . . ?
O7 C14 C1 117.1(2) . . ?
C14 O7 Eu1 135.58(15) . 4_575 ?
C14 O8 Eu1 124.57(14) . . ?
C16 N3 C15 114.1(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5 Eu1 N1 C1 24.6(2) 2_655 . . . ?
O4 Eu1 N1 C1 -72.04(16) 3_666 . . . ?
O7 Eu1 N1 C1 -107.57(16) 4_576 . . . ?
O1W Eu1 N1 C1 94.31(16) . . . . ?
O8 Eu1 N1 C1 13.77(15) . . . . ?
O1 Eu1 N1 C1 158.38(15) . . . . ?
N2 Eu1 N1 C1 179.26(18) . . . . ?
O5 Eu1 N1 C5 -172.67(15) 2_655 . . . ?
O4 Eu1 N1 C5 90.69(18) 3_666 . . . ?
O7 Eu1 N1 C5 55.2(2) 4_576 . . . ?
O1W Eu1 N1 C5 -102.95(18) . . . . ?
O8 Eu1 N1 C5 176.50(19) . . . . ?
O1 Eu1 N1 C5 -38.89(19) . . . . ?
N2 Eu1 N1 C5 -18.01(16) . . . . ?
C5 N1 C1 C2 -3.9(3) . . . . ?
Eu1 N1 C1 C2 159.76(18) . . . . ?
C5 N1 C1 C14 178.8(2) . . . . ?
Eu1 N1 C1 C14 -17.5(2) . . . . ?
N1 C1 C2 C3 1.7(4) . . . . ?
C14 C1 C2 C3 178.8(2) . . . . ?
C1 C2 C3 C4 2.2(3) . . . . ?
C1 C2 C3 C13 -175.1(2) . . . . ?
C2 C3 C4 C5 -3.7(3) . . . . ?
C13 C3 C4 C5 173.5(2) . . . . ?
C1 N1 C5 C4 2.2(3) . . . . ?
Eu1 N1 C5 C4 -159.89(17) . . . . ?
C1 N1 C5 C6 -179.1(2) . . . . ?
Eu1 N1 C5 C6 18.8(3) . . . . ?
C3 C4 C5 N1 1.6(3) . . . . ?
C3 C4 C5 C6 -176.9(2) . . . . ?
N1 C5 C6 N2 -3.4(3) . . . . ?
C4 C5 C6 N2 175.2(2) . . . . ?
N1 C5 C6 C7 177.5(2) . . . . ?
C4 C5 C6 C7 -3.9(4) . . . . ?
N2 C6 C7 C8 2.4(3) . . . . ?
C5 C6 C7 C8 -178.6(2) . . . . ?
C6 C7 C8 C9 3.1(3) . . . . ?
C6 C7 C8 C12 -175.0(2) . . . . ?
C7 C8 C9 C10 -5.1(3) . . . . ?
C12 C8 C9 C10 173.1(2) . . . . ?
C8 C9 C10 N2 1.8(4) . . . . ?
C8 C9 C10 C11 -179.5(2) . . . . ?
C9 C10 N2 C6 3.6(3) . . . . ?
C11 C10 N2 C6 -175.2(2) . . . . ?
C9 C10 N2 Eu1 -168.66(17) . . . . ?
C11 C10 N2 Eu1 12.5(2) . . . . ?
C7 C6 N2 C10 -5.7(3) . . . . ?
C5 C6 N2 C10 175.2(2) . . . . ?
C7 C6 N2 Eu1 165.95(17) . . . . ?
C5 C6 N2 Eu1 -13.1(3) . . . . ?
O5 Eu1 N2 C10 -33.4(2) 2_655 . . . ?
O4 Eu1 N2 C10 123.01(16) 3_666 . . . ?
O7 Eu1 N2 C10 52.61(16) 4_576 . . . ?
O1W Eu1 N2 C10 -86.46(16) . . . . ?
O8 Eu1 N2 C10 -156.54(15) . . . . ?
O1 Eu1 N2 C10 -12.19(15) . . . . ?
N1 Eu1 N2 C10 -172.39(18) . . . . ?
O5 Eu1 N2 C6 154.78(16) 2_655 . . . ?
O4 Eu1 N2 C6 -48.78(18) 3_666 . . . ?
O7 Eu1 N2 C6 -119.19(17) 4_576 . . . ?
O1W Eu1 N2 C6 101.75(18) . . . . ?
O8 Eu1 N2 C6 31.7(2) . . . . ?
O1 Eu1 N2 C6 176.02(19) . . . . ?
N1 Eu1 N2 C6 15.81(16) . . . . ?
N2 C10 C11 O2 176.0(2) . . . . ?
C9 C10 C11 O2 -2.8(3) . . . . ?
N2 C10 C11 O1 -2.8(3) . . . . ?
C9 C10 C11 O1 178.3(2) . . . . ?
C9 C8 C12 O3 35.1(3) . . . . ?
C7 C8 C12 O3 -146.8(2) . . . . ?
C9 C8 C12 O4 -143.1(2) . . . . ?
C7 C8 C12 O4 35.1(3) . . . . ?
O2 C11 O1 Eu1 171.28(17) . . . . ?
C10 C11 O1 Eu1 -10.0(3) . . . . ?
O5 Eu1 O1 C11 -177.34(18) 2_655 . . . ?
O4 Eu1 O1 C11 -61.3(2) 3_666 . . . ?
O7 Eu1 O1 C11 -97.96(18) 4_576 . . . ?
O1W Eu1 O1 C11 101.36(19) . . . . ?
O8 Eu1 O1 C11 124.66(18) . . . . ?
N1 Eu1 O1 C11 32.0(2) . . . . ?
N2 Eu1 O1 C11 11.89(17) . . . . ?
O3 C12 O4 Eu1 -140.0(3) . . . 3_666 ?
C8 C12 O4 Eu1 37.9(4) . . . 3_666 ?
C2 C3 C13 O6 23.0(3) . . . . ?
C4 C3 C13 O6 -154.2(2) . . . . ?
C2 C3 C13 O5 -155.9(2) . . . . ?
C4 C3 C13 O5 26.9(3) . . . . ?
O6 C13 O5 Eu1 34.6(7) . . . 2_645 ?
C3 C13 O5 Eu1 -146.6(4) . . . 2_645 ?
N1 C1 C14 O8 10.5(3) . . . . ?
C2 C1 C14 O8 -166.8(2) . . . . ?
N1 C1 C14 O7 -169.7(2) . . . . ?
C2 C1 C14 O7 13.0(3) . . . . ?
O8 C14 O7 Eu1 -87.6(3) . . . 4_575 ?
C1 C14 O7 Eu1 92.6(3) . . . 4_575 ?
O7 C14 O8 Eu1 -176.33(17) . . . . ?
C1 C14 O8 Eu1 3.5(3) . . . . ?
O5 Eu1 O8 C14 178.7(2) 2_655 . . . ?
O4 Eu1 O8 C14 65.71(19) 3_666 . . . ?
O7 Eu1 O8 C14 117.46(19) 4_576 . . . ?
O1W Eu1 O8 C14 -96.06(19) . . . . ?
O1 Eu1 O8 C14 -118.71(19) . . . . ?
N1 Eu1 O8 C14 -8.97(18) . . . . ?
N2 Eu1 O8 C14 -24.1(2) . . . . ?

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
O1W H2W1 O3 0.819(18) 1.863(19) 2.662(2) 165(3) 3_566
O1W H1W1 O2 0.819(18) 1.844(18) 2.655(2) 170(3) 4_575
N3 H1N3 O6 0.92(3) 1.78(3) 2.702(3) 174(3) .
N3 H2N3 O1 0.87(4) 2.08(4) 2.819(3) 141(3) 2_645
N3 H2N3 O1W 0.87(4) 2.56(4) 3.243(4) 136(3) 2_645

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.079


####END

data_4
_database_code_depnum_ccdc_archive 'CCDC 683756'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            10
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H11 Gd N2 O13'
_chemical_formula_weight         572.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pnma

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

_cell_length_a                   21.9198(10)
_cell_length_b                   6.6040(3)
_cell_length_c                   11.3592(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1644.34(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1108
_exptl_absorpt_coefficient_mu    4.118
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8325
_exptl_absorpt_correction_T_max  1.0000
_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  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12536
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_sigmaI/netI    0.0134
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1588
_reflns_number_gt                1581
_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 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)+(0.0223P)²+73.6823P] where P=(Fo²+2Fc²)/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         1588
_refine_ls_number_parameters     125
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0650
_refine_ls_wR_factor_ref         0.1657
_refine_ls_wR_factor_gt          0.1657
_refine_ls_goodness_of_fit_ref   1.367
_refine_ls_restrained_S_all      1.367
_refine_ls_shift/su_max          0.117
_refine_ls_shift/su_mean         0.001

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 0.13186(3) 0.2500 0.03345(7) 0.0151(3) Uani 1 2 d S . .
N1 N 0.2447(6) 0.2500 0.0785(12) 0.025(4) Uani 1 2 d S . .
C1 C 0.2622(8) 0.2500 0.1913(16) 0.020(4) Uiso 1 2 d S . .
C2 C 0.3227(8) 0.2500 0.2248(16) 0.030(5) Uani 1 2 d S . .
H2A H 0.3334 0.2500 0.3040 0.036 Uiso 1 2 calc SR . .
C3 C 0.3669(10) 0.2500 0.1382(19) 0.033(5) Uiso 1 2 d S . .
C4 C 0.3486(8) 0.2500 0.0198(16) 0.043(7) Uani 1 2 d S . .
H4A H 0.3776 0.2500 -0.0400 0.052 Uiso 1 2 calc SR . .
C5 C 0.2873(8) 0.2500 -0.0070(15) 0.027(5) Uani 1 2 d S . .
C6 C 0.2639(8) 0.2500 -0.1295(16) 0.019(4) Uiso 1 2 d S . .
C7 C 0.3018(8) 0.2500 -0.2266(15) 0.016(4) Uiso 1 2 d S . .
H7A H 0.3439 0.2500 -0.2168 0.019 Uiso 1 2 calc SR . .
C8 C 0.2768(8) 0.2500 -0.3386(15) 0.017(4) Uiso 1 2 d S . .
C9 C 0.2143(8) 0.2500 -0.3491(17) 0.022(4) Uiso 1 2 d S . .
H9A H 0.1962 0.2500 -0.4231 0.027 Uiso 1 2 calc SR . .
C10 C 0.1784(8) 0.2500 -0.2483(14) 0.020(4) Uani 1 2 d S . .
N2 N 0.2036(6) 0.2500 -0.1403(13) 0.018(3) Uiso 1 2 d S . .
C11 C 0.1093(9) 0.2500 -0.2492(17) 0.026(4) Uiso 1 2 d S . .
O1 O 0.0837(6) 0.2500 -0.1495(11) 0.025(3) Uiso 1 2 d S . .
O2 O 0.0825(7) 0.2500 -0.3453(13) 0.038(4) Uiso 1 2 d S . .
C12 C 0.3202(8) 0.2500 -0.4432(15) 0.018(4) Uiso 1 2 d S . .
O3 O 0.3376(4) 0.0839(16) -0.4802(7) 0.029(2) Uani 1 1 d . . .
C13 C 0.4329(9) 0.2500 0.1666(15) 0.060(10) Uani 1 2 d S . .
O4 O 0.4681(7) 0.2500 0.0739(14) 0.042(4) Uiso 1 2 d S . .
O5 O 0.4513(8) 0.2500 0.2675(15) 0.049(4) Uiso 1 2 d S . .
C14 C 0.2102(8) 0.2500 0.2790(14) 0.019(4) Uani 1 2 d S . .
O6 O 0.2220(5) 0.2500 0.3845(10) 0.026(3) Uani 1 2 d S . .
O7 O 0.1563(5) 0.2500 0.2347(10) 0.021(3) Uani 1 2 d S . .
O1W O 0.0421(7) 0.446(3) 0.0729(16) 0.014(4) Uiso 0.50 1 d P . .
O1W' O 0.0461(7) 0.475(3) 0.1160(17) 0.015(4) Uiso 0.50 1 d P . .
O2W O 0.0788(7) 0.159(2) 0.4136(14) 0.086(5) Uiso 1 1 d . . .
O3W O 0.0407(7) 0.670(2) 0.2760(13) 0.016(3) Uiso 0.50 1 d P . .


_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 O3 2.310(10) 7_666 ?
Gd1 O3 2.310(10) 2 ?
Gd1 O1 2.331(13) . ?
Gd1 O7 2.348(11) . ?
Gd1 O1W 2.397(17) 8_565 ?
Gd1 O1W 2.397(17) . ?
Gd1 N2 2.523(14) . ?
Gd1 N1 2.526(14) . ?
Gd1 O1W' 2.572(18) 8_565 ?
Gd1 O1W' 2.572(18) . ?
N1 C1 1.34(2) . ?
N1 C5 1.35(2) . ?
C1 C2 1.38(2) . ?
C1 C14 1.51(2) . ?
C2 C3 1.38(3) . ?
C2 H2A 0.9300 . ?
C3 C4 1.40(3) . ?
C3 C13 1.48(3) . ?
C4 C5 1.38(3) . ?
C4 H4A 0.9300 . ?
C5 C6 1.48(2) . ?
C6 N2 1.33(2) . ?
C6 C7 1.38(2) . ?
C7 C8 1.39(2) . ?
C7 H7A 0.9300 . ?
C8 C9 1.37(2) . ?
C8 C12 1.52(2) . ?
C9 C10 1.39(2) . ?
C9 H9A 0.9300 . ?
C10 N2 1.34(2) . ?
C10 C11 1.52(3) . ?
C11 O2 1.24(2) . ?
C11 O1 1.26(2) . ?
C12 O3 1.235(12) 8_565 ?
C12 O3 1.235(12) . ?
O3 Gd1 2.310(10) 2_554 ?
C13 O5 1.21(2) . ?
C13 O4 1.31(2) . ?
C14 O6 1.23(2) . ?
C14 O7 1.28(2) . ?
O1W O1W' 0.53(2) . ?
O2W O2W 1.21(3) 8_565 ?
O3W O3W 1.05(3) 8_575 ?

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
O3 Gd1 O3 145.4(5) 7_666 2 ?
O3 Gd1 O1 94.1(2) 7_666 . ?
O3 Gd1 O1 94.1(2) 2 . ?
O3 Gd1 O7 90.0(2) 7_666 . ?
O3 Gd1 O7 90.0(2) 2 . ?
O1 Gd1 O7 166.3(4) . . ?
O3 Gd1 O1W 140.0(5) 7_666 8_565 ?
O3 Gd1 O1W 74.7(5) 2 8_565 ?
O1 Gd1 O1W 78.2(5) . 8_565 ?
O7 Gd1 O1W 90.3(5) . 8_565 ?
O3 Gd1 O1W 74.7(5) 7_666 . ?
O3 Gd1 O1W 140.0(5) 2 . ?
O1 Gd1 O1W 78.2(5) . . ?
O7 Gd1 O1W 90.3(5) . . ?
O1W Gd1 O1W 65.3(9) 8_565 . ?
O3 Gd1 N2 76.5(2) 7_666 . ?
O3 Gd1 N2 76.5(2) 2 . ?
O1 Gd1 N2 65.5(4) . . ?
O7 Gd1 N2 128.3(4) . . ?
O1W Gd1 N2 131.1(5) 8_565 . ?
O1W Gd1 N2 131.1(5) . . ?
O3 Gd1 N1 74.3(2) 7_666 . ?
O3 Gd1 N1 74.3(2) 2 . ?
O1 Gd1 N1 128.6(4) . . ?
O7 Gd1 N1 65.1(4) . . ?
O1W Gd1 N1 140.0(5) 8_565 . ?
O1W Gd1 N1 140.0(5) . . ?
N2 Gd1 N1 63.1(5) . . ?
O3 Gd1 O1W' 141.9(5) 7_666 8_565 ?
O3 Gd1 O1W' 71.7(5) 2 8_565 ?
O1 Gd1 O1W' 89.6(5) . 8_565 ?
O7 Gd1 O1W' 79.2(5) . 8_565 ?
O1W Gd1 O1W' 11.6(5) 8_565 8_565 ?
O1W Gd1 O1W' 69.1(5) . 8_565 ?
N2 Gd1 O1W' 137.8(4) . 8_565 ?
N1 Gd1 O1W' 129.9(5) . 8_565 ?
O3 Gd1 O1W' 71.7(5) 7_666 . ?
O3 Gd1 O1W' 141.9(5) 2 . ?
O1 Gd1 O1W' 89.6(5) . . ?
O7 Gd1 O1W' 79.2(5) . . ?
O1W Gd1 O1W' 69.1(5) 8_565 . ?
O1W Gd1 O1W' 11.6(5) . . ?
N2 Gd1 O1W' 137.8(4) . . ?
N1 Gd1 O1W' 129.9(5) . . ?
O1W' Gd1 O1W' 70.5(8) 8_565 . ?
C1 N1 C5 119.4(15) . . ?
C1 N1 Gd1 118.3(11) . . ?
C5 N1 Gd1 122.2(11) . . ?
N1 C1 C2 122.7(16) . . ?
N1 C1 C14 114.5(15) . . ?
C2 C1 C14 122.8(16) . . ?
C1 C2 C3 118.5(17) . . ?
C1 C2 H2A 120.8 . . ?
C3 C2 H2A 120.8 . . ?
C2 C3 C4 118.9(19) . . ?
C2 C3 C13 122.0(18) . . ?
C4 C3 C13 119.2(18) . . ?
C5 C4 C3 119.3(17) . . ?
C5 C4 H4A 120.3 . . ?
C3 C4 H4A 120.3 . . ?
N1 C5 C4 121.2(16) . . ?
N1 C5 C6 115.8(15) . . ?
C4 C5 C6 123.0(16) . . ?
N2 C6 C7 121.7(16) . . ?
N2 C6 C5 115.6(15) . . ?
C7 C6 C5 122.8(16) . . ?
C6 C7 C8 119.7(16) . . ?
C6 C7 H7A 120.1 . . ?
C8 C7 H7A 120.1 . . ?
C9 C8 C7 118.2(16) . . ?
C9 C8 C12 123.7(16) . . ?
C7 C8 C12 118.0(15) . . ?
C8 C9 C10 119.6(17) . . ?
C8 C9 H9A 120.2 . . ?
C10 C9 H9A 120.2 . . ?
N2 C10 C9 121.3(16) . . ?
N2 C10 C11 114.6(15) . . ?
C9 C10 C11 124.1(16) . . ?
C6 N2 C10 119.5(15) . . ?
C6 N2 Gd1 123.2(12) . . ?
C10 N2 Gd1 117.3(11) . . ?
O2 C11 O1 125.5(18) . . ?
O2 C11 C10 118.6(17) . . ?
O1 C11 C10 115.9(16) . . ?
C11 O1 Gd1 126.7(12) . . ?
O3 C12 O3 125.4(16) 8_565 . ?
O3 C12 C8 117.3(8) 8_565 . ?
O3 C12 C8 117.3(8) . . ?
C12 O3 Gd1 156.1(9) . 2_554 ?
O5 C13 O4 124(2) . . ?
O5 C13 C3 122.0(19) . . ?
O4 C13 C3 113.7(17) . . ?
O6 C14 O7 125.2(15) . . ?
O6 C14 C1 119.1(15) . . ?
O7 C14 C1 115.8(14) . . ?
C14 O7 Gd1 126.2(10) . . ?
O1W' O1W Gd1 103(3) . . ?
O1W O1W' Gd1 65(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Gd1 N1 C1 97.4(2) 7_666 . . . ?
O3 Gd1 N1 C1 -97.4(2) 2 . . . ?
O1 Gd1 N1 C1 180.0 . . . . ?
O7 Gd1 N1 C1 0.0 . . . . ?
O1W Gd1 N1 C1 -57.1(7) 8_565 . . . ?
O1W Gd1 N1 C1 57.1(7) . . . . ?
N2 Gd1 N1 C1 180.0 . . . . ?
O1W' Gd1 N1 C1 -48.8(6) 8_565 . . . ?
O1W' Gd1 N1 C1 48.8(6) . . . . ?
O3 Gd1 N1 C5 -82.6(2) 7_666 . . . ?
O3 Gd1 N1 C5 82.6(2) 2 . . . ?
O1 Gd1 N1 C5 0.0 . . . . ?
O7 Gd1 N1 C5 180.0 . . . . ?
O1W Gd1 N1 C5 122.9(7) 8_565 . . . ?
O1W Gd1 N1 C5 -122.9(7) . . . . ?
N2 Gd1 N1 C5 0.0 . . . . ?
O1W' Gd1 N1 C5 131.2(6) 8_565 . . . ?
O1W' Gd1 N1 C5 -131.2(6) . . . . ?
C5 N1 C1 C2 0.000(1) . . . . ?
Gd1 N1 C1 C2 180.0 . . . . ?
C5 N1 C1 C14 180.0 . . . . ?
Gd1 N1 C1 C14 0.0 . . . . ?
N1 C1 C2 C3 0.000(1) . . . . ?
C14 C1 C2 C3 180.000(1) . . . . ?
C1 C2 C3 C4 0.000(1) . . . . ?
C1 C2 C3 C13 180.0 . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C13 C3 C4 C5 180.0 . . . . ?
C1 N1 C5 C4 0.0 . . . . ?
Gd1 N1 C5 C4 180.0 . . . . ?
C1 N1 C5 C6 180.0 . . . . ?
Gd1 N1 C5 C6 0.0 . . . . ?
C3 C4 C5 N1 0.0 . . . . ?
C3 C4 C5 C6 180.0 . . . . ?
N1 C5 C6 N2 0.0 . . . . ?
C4 C5 C6 N2 180.0 . . . . ?
N1 C5 C6 C7 180.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
N2 C6 C7 C8 0.000(1) . . . . ?
C5 C6 C7 C8 180.000(1) . . . . ?
C6 C7 C8 C9 0.000(2) . . . . ?
C6 C7 C8 C12 180.000(1) . . . . ?
C7 C8 C9 C10 0.000(2) . . . . ?
C12 C8 C9 C10 180.000(1) . . . . ?
C8 C9 C10 N2 0.000(2) . . . . ?
C8 C9 C10 C11 180.000(2) . . . . ?
C7 C6 N2 C10 0.000(1) . . . . ?
C5 C6 N2 C10 180.0 . . . . ?
C7 C6 N2 Gd1 180.0 . . . . ?
C5 C6 N2 Gd1 0.0 . . . . ?
C9 C10 N2 C6 0.000(1) . . . . ?
C11 C10 N2 C6 180.0 . . . . ?
C9 C10 N2 Gd1 180.000(1) . . . . ?
C11 C10 N2 Gd1 0.0 . . . . ?
O3 Gd1 N2 C6 79.0(2) 7_666 . . . ?
O3 Gd1 N2 C6 -79.0(2) 2 . . . ?
O1 Gd1 N2 C6 180.0 . . . . ?
O7 Gd1 N2 C6 0.0 . . . . ?
O1W Gd1 N2 C6 -134.3(6) 8_565 . . . ?
O1W Gd1 N2 C6 134.3(6) . . . . ?
N1 Gd1 N2 C6 0.0 . . . . ?
O1W' Gd1 N2 C6 -120.9(7) 8_565 . . . ?
O1W' Gd1 N2 C6 120.9(7) . . . . ?
O3 Gd1 N2 C10 -101.0(2) 7_666 . . . ?
O3 Gd1 N2 C10 101.0(2) 2 . . . ?
O1 Gd1 N2 C10 0.0 . . . . ?
O7 Gd1 N2 C10 180.0 . . . . ?
O1W Gd1 N2 C10 45.7(6) 8_565 . . . ?
O1W Gd1 N2 C10 -45.7(6) . . . . ?
N1 Gd1 N2 C10 180.0 . . . . ?
O1W' Gd1 N2 C10 59.1(7) 8_565 . . . ?
O1W' Gd1 N2 C10 -59.1(7) . . . . ?
N2 C10 C11 O2 180.000(1) . . . . ?
C9 C10 C11 O2 0.000(2) . . . . ?
N2 C10 C11 O1 0.000(1) . . . . ?
C9 C10 C11 O1 180.000(1) . . . . ?
O2 C11 O1 Gd1 180.000(2) . . . . ?
C10 C11 O1 Gd1 0.000(1) . . . . ?
O3 Gd1 O1 C11 73.2(2) 7_666 . . . ?
O3 Gd1 O1 C11 -73.2(2) 2 . . . ?
O7 Gd1 O1 C11 180.000(1) . . . . ?
O1W Gd1 O1 C11 -146.6(4) 8_565 . . . ?
O1W Gd1 O1 C11 146.6(4) . . . . ?
N2 Gd1 O1 C11 0.000(1) . . . . ?
N1 Gd1 O1 C11 0.000(1) . . . . ?
O1W' Gd1 O1 C11 -144.8(4) 8_565 . . . ?
O1W' Gd1 O1 C11 144.8(4) . . . . ?
C9 C8 C12 O3 91.8(14) . . . 8_565 ?
C7 C8 C12 O3 -88.2(14) . . . 8_565 ?
C9 C8 C12 O3 -91.8(14) . . . . ?
C7 C8 C12 O3 88.2(14) . . . . ?
O3 C12 O3 Gd1 140.0(14) 8_565 . . 2_554 ?
C8 C12 O3 Gd1 -36(3) . . . 2_554 ?
C2 C3 C13 O5 0.000(1) . . . . ?
C4 C3 C13 O5 180.000(1) . . . . ?
C2 C3 C13 O4 180.0 . . . . ?
C4 C3 C13 O4 0.0 . . . . ?
N1 C1 C14 O6 180.0 . . . . ?
C2 C1 C14 O6 0.000(1) . . . . ?
N1 C1 C14 O7 0.000(1) . . . . ?
C2 C1 C14 O7 180.0 . . . . ?
O6 C14 O7 Gd1 180.000(1) . . . . ?
C1 C14 O7 Gd1 0.0 . . . . ?
O3 Gd1 O7 C14 -72.7(2) 7_666 . . . ?
O3 Gd1 O7 C14 72.7(2) 2 . . . ?
O1 Gd1 O7 C14 180.000(1) . . . . ?
O1W Gd1 O7 C14 147.4(4) 8_565 . . . ?
O1W Gd1 O7 C14 -147.4(4) . . . . ?
N2 Gd1 O7 C14 0.000(1) . . . . ?
N1 Gd1 O7 C14 0.0 . . . . ?
O1W' Gd1 O7 C14 144.0(4) 8_565 . . . ?
O1W' Gd1 O7 C14 -144.0(4) . . . . ?
O3 Gd1 O1W O1W' -73(3) 7_666 . . . ?
O3 Gd1 O1W O1W' 107(3) 2 . . . ?
O1 Gd1 O1W O1W' -171(3) . . . . ?
O7 Gd1 O1W O1W' 16(3) . . . . ?
O1W Gd1 O1W O1W' 107(3) 8_565 . . . ?
N2 Gd1 O1W O1W' -129(3) . . . . ?
N1 Gd1 O1W O1W' -33(4) . . . . ?
O1W' Gd1 O1W O1W' 95(3) 8_565 . . . ?
O3 Gd1 O1W' O1W 103(3) 7_666 . . . ?
O3 Gd1 O1W' O1W -87(3) 2 . . . ?
O1 Gd1 O1W' O1W 9(3) . . . . ?
O7 Gd1 O1W' O1W -163(3) . . . . ?
O1W Gd1 O1W' O1W -69(3) 8_565 . . . ?
N2 Gd1 O1W' O1W 60(4) . . . . ?
N1 Gd1 O1W' O1W 153(3) . . . . ?
O1W' Gd1 O1W' O1W -81(3) 8_565 . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         2.140
_refine_diff_density_min         -2.567
_refine_diff_density_rms         0.334

