# 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

_publ_contact_author_name        'La-Sheng Long'
_publ_contact_author_email       LSLONG@XMU.EDU.CN

_publ_section_title              
;
Influence of the Reaction Condition on the Shape of
Channel of 3d-4f Heterometallic Metal-organic Framework
;
loop_
_publ_author_name
'La-Sheng Long.'
'Rong-Bin Huantg.'
'Xiang-Jian Kong.'
'Mohamedally Kurmoo'
;
Yan-Ping Ren
;
'Lan-Sun Zheng.'

# Attachment 'complex1.cif'

data_complex1
_database_code_depnum_ccdc_archive 'CCDC 647829'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H24 La2 N3 Ni1.50 O22.50'
_chemical_formula_weight         972.26

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'
Ni Ni 0.3393 1.1124 '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                   7.2005(15)
_cell_length_b                   12.813(3)
_cell_length_c                   14.723(3)
_cell_angle_alpha                74.624(4)
_cell_angle_beta                 89.392(4)
_cell_angle_gamma                87.687(3)
_cell_volume                     1308.7(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    5146
_cell_measurement_theta_min      2.457
_cell_measurement_theta_max      28.363

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             942
_exptl_absorpt_coefficient_mu    4.376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3096
_exptl_absorpt_correction_T_max  0.8109
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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_%        ?
_diffrn_reflns_number            7030
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4976
_reflns_number_gt                4554
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_cell_refinement       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0536P)²+2.3558P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4976
_refine_ls_number_parameters     412
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.1046
_refine_ls_wR_factor_gt          0.1018
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.006
_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 0.25276(3) -0.874453(15) 0.324820(14) 0.00877(5) Uani 1 1 d . . .
La2 La -0.32524(3) -0.459426(15) 0.256796(14) 0.00920(5) Uani 1 1 d . . .
Ni1 Ni 0.0000 -0.5000 0.0000 0.01061(15) Uani 1 2 d S . .
Ni2 Ni -0.03715(6) -0.17330(3) 0.29993(3) 0.00945(11) Uani 1 1 d . . .
O1 O -0.4737(4) -0.9892(2) 0.3324(2) 0.0210(7) Uani 1 1 d . . .
O2 O -0.2552(4) -1.1161(2) 0.36349(18) 0.0149(6) Uani 1 1 d . . .
C1 C -0.3324(6) -1.0333(3) 0.2029(3) 0.0232(10) Uani 1 1 d . . .
H1A H -0.4441 -1.0604 0.1793 0.028 Uiso 1 1 calc R . .
H1B H -0.3256 -0.9553 0.1706 0.028 Uiso 1 1 calc R . .
C2 C -0.3531(5) -1.0466(3) 0.3067(3) 0.0153(9) Uani 1 1 d . . .
N1 N -0.1668(4) -1.0910(2) 0.1786(2) 0.0114(7) Uani 1 1 d . . .
H1C H -0.2018 -1.1393 0.1453 0.014 Uiso 1 1 calc R . .
C3 C -0.0273(6) -1.0197(3) 0.1251(3) 0.0162(9) Uani 1 1 d . . .
H3A H -0.0898 -0.9559 0.0816 0.019 Uiso 1 1 calc R . .
H3B H 0.0479 -1.0589 0.0870 0.019 Uiso 1 1 calc R . .
C4 C 0.0978(5) -0.9829(3) 0.1912(3) 0.0117(8) Uani 1 1 d . . .
O3 O 0.2148(4) -0.91370(19) 0.15973(18) 0.0141(6) Uani 1 1 d . . .
O4 O 0.0778(4) -1.0231(2) 0.27850(18) 0.0153(6) Uani 1 1 d . . .
O5 O 0.2169(4) -0.55861(19) 0.08813(18) 0.0146(6) Uani 1 1 d . . .
O6 O 0.4561(4) -0.5050(2) 0.1528(2) 0.0198(7) Uani 1 1 d . . .
C5 C 0.2970(6) -0.3734(3) 0.0368(3) 0.0200(10) Uani 1 1 d . . .
H5A H 0.2920 -0.3234 0.0779 0.024 Uiso 1 1 calc R . .
H5B H 0.4067 -0.3558 -0.0048 0.024 Uiso 1 1 calc R . .
C6 C 0.3225(5) -0.4860(3) 0.0967(3) 0.0130(8) Uani 1 1 d . . .
N2 N 0.1284(4) -0.3542(2) -0.0219(2) 0.0122(7) Uani 1 1 d . . .
H2A H 0.1599 -0.3284 -0.0851 0.015 Uiso 1 1 calc R . .
C7 C -0.0117(5) -0.2819(3) 0.0040(3) 0.0166(9) Uani 1 1 d . . .
H7A H -0.0876 -0.2460 -0.0521 0.020 Uiso 1 1 calc R . .
H7B H 0.0510 -0.2250 0.0249 0.020 Uiso 1 1 calc R . .
C8 C -0.1373(5) -0.3407(3) 0.0813(3) 0.0115(8) Uani 1 1 d . . .
O7 O -0.2439(4) -0.2890(2) 0.12132(19) 0.0183(7) Uani 1 1 d . . .
O8 O -0.1296(4) -0.44245(19) 0.10246(18) 0.0137(6) Uani 1 1 d . . .
O9 O 0.4322(4) -0.3273(2) 0.2591(2) 0.0241(7) Uani 1 1 d . . .
O10 O 0.1800(4) -0.2231(2) 0.2336(2) 0.0182(7) Uani 1 1 d . . .
C9 C 0.2647(6) -0.3119(3) 0.3914(3) 0.0203(10) Uani 1 1 d . . .
H9A H 0.2576 -0.3914 0.4161 0.024 Uiso 1 1 calc R . .
H9B H 0.3741 -0.2893 0.4205 0.024 Uiso 1 1 calc R . .
C10 C 0.2928(5) -0.2852(3) 0.2871(3) 0.0147(9) Uani 1 1 d . . .
N3 N 0.0964(4) -0.2600(2) 0.4198(2) 0.0114(7) Uani 1 1 d . . .
H3C H 0.1285 -0.2140 0.4560 0.014 Uiso 1 1 calc R . .
C11 C -0.0408(5) -0.3360(3) 0.4701(3) 0.0142(9) Uani 1 1 d . . .
H11A H -0.1167 -0.3013 0.5113 0.017 Uiso 1 1 calc R . .
H11B H 0.0246 -0.4009 0.5106 0.017 Uiso 1 1 calc R . .
C12 C -0.1654(5) -0.3696(3) 0.4036(3) 0.0114(8) Uani 1 1 d . . .
O11 O -0.1580(4) -0.31948(19) 0.31821(18) 0.0130(6) Uani 1 1 d . . .
O12 O -0.2721(4) -0.4448(2) 0.43265(18) 0.0159(6) Uani 1 1 d . . .
O13 O -0.0074(4) -0.54064(19) 0.31011(18) 0.0140(6) Uani 1 1 d . . .
O14 O 0.1952(4) -0.67979(19) 0.32903(18) 0.0121(6) Uani 1 1 d . . .
C13 C 0.0448(5) -0.6306(3) 0.3013(2) 0.0098(8) Uani 1 1 d . . .
C14 C -0.0876(5) -0.6902(3) 0.2535(2) 0.0109(8) Uani 1 1 d . . .
O15 O -0.2483(4) -0.64823(19) 0.23794(19) 0.0151(6) Uani 1 1 d . . .
O16 O -0.0262(4) -0.77230(19) 0.23309(18) 0.0143(6) Uani 1 1 d . . .
C15 C -0.0672(5) -0.9490(3) 0.4899(2) 0.0106(8) Uani 1 1 d . . .
O17 O -0.2149(3) -0.95823(19) 0.53506(18) 0.0131(6) Uani 1 1 d . . .
O18 O -0.0141(4) -0.86716(19) 0.43323(19) 0.0147(6) Uani 1 1 d . . .
O1W O 0.4395(4) -0.8480(2) 0.46389(18) 0.0156(6) Uani 1 1 d . . .
O2W O 0.4475(4) -0.7478(2) 0.20072(19) 0.0162(7) Uani 1 1 d . . .
O3W O -0.5328(4) -0.5739(2) 0.37809(19) 0.0191(7) Uani 1 1 d . . .
O4W O 0.4810(12) -0.8696(7) 0.0040(6) 0.054(2) Uani 0.50 1 d P . .
O4W' O 0.3624(19) -0.9465(9) 0.0003(8) 0.096(4) Uani 0.50 1 d P . .
O5W O 0.6534(19) -0.8771(7) -0.0440(8) 0.104(4) Uani 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
La1 O1 2.395(3) 1_655 ?
La1 O18 2.499(3) . ?
La1 O14 2.529(2) . ?
La1 O16 2.546(3) . ?
La1 O2W 2.549(3) . ?
La1 O1W 2.565(3) . ?
La1 O4 2.565(3) . ?
La1 O17 2.572(2) 2_536 ?
La1 O3 2.628(3) . ?
La1 C4 2.943(4) . ?
La2 O9 2.389(3) 1_455 ?
La2 O6 2.401(3) 1_455 ?
La2 O3W 2.511(3) . ?
La2 O13 2.520(3) . ?
La2 O15 2.546(3) . ?
La2 O11 2.558(3) . ?
La2 O7 2.619(3) . ?
La2 O8 2.625(3) . ?
La2 O12 2.677(3) . ?
La2 C12 2.966(4) . ?
La2 C8 2.971(4) . ?
Ni1 O5 2.029(3) . ?
Ni1 O5 2.029(3) 2_545 ?
Ni1 O8 2.048(3) 2_545 ?
Ni1 O8 2.048(3) . ?
Ni1 N2 2.064(3) . ?
Ni1 N2 2.064(3) 2_545 ?
Ni2 O10 2.005(3) . ?
Ni2 O2 2.029(3) 1_565 ?
Ni2 N1 2.033(3) 1_565 ?
Ni2 N3 2.045(3) . ?
Ni2 O11 2.049(3) . ?
Ni2 O4 2.071(3) 1_565 ?
O1 C2 1.236(5) . ?
O1 La1 2.395(3) 1_455 ?
O2 C2 1.248(4) . ?
O2 Ni2 2.029(3) 1_545 ?
C1 N1 1.467(5) . ?
C1 C2 1.498(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
N1 C3 1.463(5) . ?
N1 Ni2 2.033(3) 1_545 ?
N1 H1C 0.9300 . ?
C3 C4 1.510(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O3 1.243(4) . ?
C4 O4 1.260(4) . ?
O4 Ni2 2.071(3) 1_545 ?
O5 C6 1.258(5) . ?
O6 C6 1.248(5) . ?
O6 La2 2.401(3) 1_655 ?
C5 N2 1.472(5) . ?
C5 C6 1.483(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
N2 C7 1.458(5) . ?
N2 H2A 0.9300 . ?
C7 C8 1.503(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 O7 1.237(5) . ?
C8 O8 1.257(4) . ?
O9 C10 1.238(5) . ?
O9 La2 2.389(3) 1_655 ?
O10 C10 1.242(4) . ?
C9 N3 1.469(5) . ?
C9 C10 1.495(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
N3 C11 1.467(5) . ?
N3 H3C 0.9300 . ?
C11 C12 1.491(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 O12 1.239(4) . ?
C12 O11 1.252(4) . ?
O13 C13 1.236(4) . ?
O14 C13 1.247(4) . ?
C13 C14 1.532(5) . ?
C14 O16 1.233(5) . ?
C14 O15 1.253(4) . ?
C15 O18 1.227(4) . ?
C15 O17 1.241(4) . ?
C15 C15 1.558(7) 2_536 ?
O17 La1 2.572(2) 2_536 ?
O4W O4W' 1.342(15) . ?
O4W O5W 1.434(15) . ?

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 O18 134.68(9) 1_655 . ?
O1 La1 O14 133.93(9) 1_655 . ?
O18 La1 O14 71.73(8) . . ?
O1 La1 O16 149.88(9) 1_655 . ?
O18 La1 O16 69.47(9) . . ?
O14 La1 O16 63.01(8) . . ?
O1 La1 O2W 81.14(9) 1_655 . ?
O18 La1 O2W 139.95(8) . . ?
O14 La1 O2W 69.13(8) . . ?
O16 La1 O2W 85.39(8) . . ?
O1 La1 O1W 75.07(9) 1_655 . ?
O18 La1 O1W 82.20(9) . . ?
O14 La1 O1W 73.00(8) . . ?
O16 La1 O1W 133.01(8) . . ?
O2W La1 O1W 94.19(9) . . ?
O1 La1 O4 86.64(9) 1_655 . ?
O18 La1 O4 85.83(9) . . ?
O14 La1 O4 138.35(8) . . ?
O16 La1 O4 76.50(8) . . ?
O2W La1 O4 118.89(9) . . ?
O1W La1 O4 139.30(8) . . ?
O1 La1 O17 72.36(9) 1_655 2_536 ?
O18 La1 O17 63.40(8) . 2_536 ?
O14 La1 O17 125.51(8) . 2_536 ?
O16 La1 O17 121.71(8) . 2_536 ?
O2W La1 O17 152.37(8) . 2_536 ?
O1W La1 O17 71.83(8) . 2_536 ?
O4 La1 O17 68.02(8) . 2_536 ?
O1 La1 O3 82.82(9) 1_655 . ?
O18 La1 O3 123.14(9) . . ?
O14 La1 O3 116.02(8) . . ?
O16 La1 O3 67.21(8) . . ?
O2W La1 O3 69.36(8) . . ?
O1W La1 O3 154.36(9) . . ?
O4 La1 O3 49.72(8) . . ?
O17 La1 O3 113.77(8) 2_536 . ?
O1 La1 C4 87.86(10) 1_655 . ?
O18 La1 C4 102.86(10) . . ?
O14 La1 C4 127.48(9) . . ?
O16 La1 C4 66.35(9) . . ?
O2W La1 C4 94.27(10) . . ?
O1W La1 C4 159.51(9) . . ?
O4 La1 C4 25.27(9) . . ?
O17 La1 C4 92.46(9) 2_536 . ?
O3 La1 C4 24.96(9) . . ?
O9 La2 O6 80.18(10) 1_455 1_455 ?
O9 La2 O3W 80.95(9) 1_455 . ?
O6 La2 O3W 81.26(9) 1_455 . ?
O9 La2 O13 149.24(10) 1_455 . ?
O6 La2 O13 130.57(9) 1_455 . ?
O3W La2 O13 102.15(9) . . ?
O9 La2 O15 145.37(9) 1_455 . ?
O6 La2 O15 69.63(9) 1_455 . ?
O3W La2 O15 78.12(9) . . ?
O13 La2 O15 63.21(8) . . ?
O9 La2 O11 77.49(9) 1_455 . ?
O6 La2 O11 151.05(8) 1_455 . ?
O3W La2 O11 112.80(9) . . ?
O13 La2 O11 73.13(8) . . ?
O15 La2 O11 136.33(8) . . ?
O9 La2 O7 74.68(9) 1_455 . ?
O6 La2 O7 88.62(9) 1_455 . ?
O3W La2 O7 154.89(9) . . ?
O13 La2 O7 101.89(8) . . ?
O15 La2 O7 119.74(9) . . ?
O11 La2 O7 67.89(8) . . ?
O9 La2 O8 119.25(9) 1_455 . ?
O6 La2 O8 77.48(9) 1_455 . ?
O3W La2 O8 147.03(9) . . ?
O13 La2 O8 74.17(8) . . ?
O15 La2 O8 70.99(8) . . ?
O11 La2 O8 97.69(8) . . ?
O7 La2 O8 49.24(8) . . ?
O9 La2 O12 82.23(9) 1_455 . ?
O6 La2 O12 144.36(9) 1_455 . ?
O3W La2 O12 65.47(9) . . ?
O13 La2 O12 71.81(8) . . ?
O15 La2 O12 112.91(8) . . ?
O11 La2 O12 49.06(8) . . ?
O7 La2 O12 116.11(8) . . ?
O8 La2 O12 138.00(8) . . ?
O9 La2 C12 82.31(10) 1_455 . ?
O6 La2 C12 161.43(10) 1_455 . ?
O3W La2 C12 89.96(10) . . ?
O13 La2 C12 67.19(9) . . ?
O15 La2 C12 124.66(9) . . ?
O11 La2 C12 24.82(8) . . ?
O7 La2 C12 92.69(9) . . ?
O8 La2 C12 116.93(9) . . ?
O12 La2 C12 24.70(9) . . ?
O9 La2 C8 98.00(10) 1_455 . ?
O6 La2 C8 85.07(10) 1_455 . ?
O3W La2 C8 166.27(10) . . ?
O13 La2 C8 85.81(9) . . ?
O15 La2 C8 95.97(9) . . ?
O11 La2 C8 80.07(9) . . ?
O7 La2 C8 24.54(9) . . ?
O8 La2 C8 24.99(9) . . ?
O12 La2 C8 128.11(9) . . ?
C12 La2 C8 103.50(10) . . ?
O5 Ni1 O5 180.00(14) . 2_545 ?
O5 Ni1 O8 89.82(11) . 2_545 ?
O5 Ni1 O8 90.18(11) 2_545 2_545 ?
O5 Ni1 O8 90.18(11) . . ?
O5 Ni1 O8 89.82(11) 2_545 . ?
O8 Ni1 O8 180.0 2_545 . ?
O5 Ni1 N2 84.15(11) . . ?
O5 Ni1 N2 95.85(11) 2_545 . ?
O8 Ni1 N2 99.36(11) 2_545 . ?
O8 Ni1 N2 80.64(11) . . ?
O5 Ni1 N2 95.85(11) . 2_545 ?
O5 Ni1 N2 84.15(11) 2_545 2_545 ?
O8 Ni1 N2 80.64(11) 2_545 2_545 ?
O8 Ni1 N2 99.36(11) . 2_545 ?
N2 Ni1 N2 180.0 . 2_545 ?
O10 Ni2 O2 177.46(10) . 1_565 ?
O10 Ni2 N1 94.08(12) . 1_565 ?
O2 Ni2 N1 84.31(11) 1_565 1_565 ?
O10 Ni2 N3 84.35(12) . . ?
O2 Ni2 N3 97.29(12) 1_565 . ?
N1 Ni2 N3 178.08(12) 1_565 . ?
O10 Ni2 O11 90.98(11) . . ?
O2 Ni2 O11 91.21(11) 1_565 . ?
N1 Ni2 O11 98.77(11) 1_565 . ?
N3 Ni2 O11 80.17(11) . . ?
O10 Ni2 O4 89.79(11) . 1_565 ?
O2 Ni2 O4 87.99(11) 1_565 1_565 ?
N1 Ni2 O4 79.44(11) 1_565 1_565 ?
N3 Ni2 O4 101.64(11) . 1_565 ?
O11 Ni2 O4 178.10(10) . 1_565 ?
C2 O1 La1 158.7(3) . 1_455 ?
C2 O2 Ni2 112.4(3) . 1_545 ?
N1 C1 C2 113.2(3) . . ?
N1 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.8 . . ?
O1 C2 O2 122.5(4) . . ?
O1 C2 C1 117.4(3) . . ?
O2 C2 C1 120.0(4) . . ?
C3 N1 C1 114.0(3) . . ?
C3 N1 Ni2 105.1(2) . 1_545 ?
C1 N1 Ni2 108.4(2) . 1_545 ?
C3 N1 H1C 109.7 . . ?
C1 N1 H1C 109.7 . . ?
Ni2 N1 H1C 109.7 1_545 . ?
N1 C3 C4 110.2(3) . . ?
N1 C3 H3A 109.6 . . ?
C4 C3 H3A 109.6 . . ?
N1 C3 H3B 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
O3 C4 O4 121.5(3) . . ?
O3 C4 C3 120.4(3) . . ?
O4 C4 C3 118.1(3) . . ?
O3 C4 La1 63.2(2) . . ?
O4 C4 La1 60.33(19) . . ?
C3 C4 La1 164.6(3) . . ?
C4 O3 La1 91.8(2) . . ?
C4 O4 Ni2 108.6(2) . 1_545 ?
C4 O4 La1 94.4(2) . . ?
Ni2 O4 La1 155.78(12) 1_545 . ?
C6 O5 Ni1 113.0(2) . . ?
C6 O6 La2 154.4(3) . 1_655 ?
N2 C5 C6 114.1(3) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
O6 C6 O5 122.4(3) . . ?
O6 C6 C5 116.9(3) . . ?
O5 C6 C5 120.7(3) . . ?
C7 N2 C5 114.3(3) . . ?
C7 N2 Ni1 104.4(2) . . ?
C5 N2 Ni1 107.6(2) . . ?
C7 N2 H2A 110.1 . . ?
C5 N2 H2A 110.1 . . ?
Ni1 N2 H2A 110.1 . . ?
N2 C7 C8 112.4(3) . . ?
N2 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
N2 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.9 . . ?
O7 C8 O8 122.4(3) . . ?
O7 C8 C7 120.1(3) . . ?
O8 C8 C7 117.5(3) . . ?
O7 C8 La2 61.57(19) . . ?
O8 C8 La2 61.93(19) . . ?
C7 C8 La2 169.5(3) . . ?
C8 O7 La2 93.9(2) . . ?
C8 O8 Ni1 111.8(2) . . ?
C8 O8 La2 93.1(2) . . ?
Ni1 O8 La2 154.70(12) . . ?
C10 O9 La2 158.6(3) . 1_655 ?
C10 O10 Ni2 114.1(3) . . ?
N3 C9 C10 113.7(3) . . ?
N3 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
N3 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
O9 C10 O10 123.5(4) . . ?
O9 C10 C9 116.5(3) . . ?
O10 C10 C9 120.0(3) . . ?
C11 N3 C9 114.4(3) . . ?
C11 N3 Ni2 104.7(2) . . ?
C9 N3 Ni2 107.8(2) . . ?
C11 N3 H3C 109.9 . . ?
C9 N3 H3C 109.9 . . ?
Ni2 N3 H3C 109.9 . . ?
N3 C11 C12 111.6(3) . . ?
N3 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
N3 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
O12 C12 O11 121.7(3) . . ?
O12 C12 C11 120.5(3) . . ?
O11 C12 C11 117.8(3) . . ?
O12 C12 La2 64.5(2) . . ?
O11 C12 La2 59.02(19) . . ?
C11 C12 La2 165.7(3) . . ?
C12 O11 Ni2 111.3(2) . . ?
C12 O11 La2 96.2(2) . . ?
Ni2 O11 La2 152.40(12) . . ?
C12 O12 La2 90.8(2) . . ?
C13 O13 La2 121.6(2) . . ?
C13 O14 La1 120.9(2) . . ?
O13 C13 O14 126.6(3) . . ?
O13 C13 C14 117.8(3) . . ?
O14 C13 C14 115.6(3) . . ?
O16 C14 O15 126.8(4) . . ?
O16 C14 C13 117.7(3) . . ?
O15 C14 C13 115.5(3) . . ?
C14 O15 La2 121.0(2) . . ?
C14 O16 La1 118.1(2) . . ?
O18 C15 O17 126.7(3) . . ?
O18 C15 C15 116.8(4) . 2_536 ?
O17 C15 C15 116.5(4) . 2_536 ?
C15 O17 La1 118.8(2) . 2_536 ?
C15 O18 La1 121.5(2) . . ?
O4W' O4W O5W 114.0(9) . . ?

_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.967
_refine_diff_density_max         1.674
_refine_diff_density_min         -1.695
_refine_diff_density_rms         0.200

# Attachment 'complex1a.cif'

data_complex1a
_database_code_depnum_ccdc_archive 'CCDC 647830'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H21 La2 N3 Ni1.50 O21'
_chemical_formula_weight         945.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   7.2229(11)
_cell_length_b                   12.7689(19)
_cell_length_c                   14.766(2)
_cell_angle_alpha                74.862(2)
_cell_angle_beta                 89.617(2)
_cell_angle_gamma                87.493(2)
_cell_volume                     1313.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9275
_cell_measurement_theta_min      2.452
_cell_measurement_theta_max      28.316

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             912
_exptl_absorpt_coefficient_mu    4.353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4764
_exptl_absorpt_correction_T_max  0.8118
_exptl_absorpt_process_details   sadabs

_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_%        ?
_diffrn_reflns_number            9987
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.43
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5017
_reflns_number_gt                4787
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_cell_refinement       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0458P)²+0.9909P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5017
_refine_ls_number_parameters     385
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0270
_refine_ls_wR_factor_ref         0.0820
_refine_ls_wR_factor_gt          0.0806
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.135
_refine_ls_shift/su_max          0.009
_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
La1 La 0.248050(18) -0.875845(10) 0.323681(9) 0.01529(3) Uani 1 1 d . . .
La2 La -0.327989(18) -0.458788(11) 0.255449(10) 0.01628(3) Uani 1 1 d . . .
Ni1 Ni 0.0000 -0.5000 0.0000 0.01671(10) Uani 1 2 d S . .
Ni2 Ni -0.04092(4) -0.17396(2) 0.29893(2) 0.01584(8) Uani 1 1 d . . .
O1 O -0.4803(3) -0.99033(18) 0.33047(15) 0.0389(6) Uani 1 1 d . . .
O2 O -0.2561(3) -1.11455(15) 0.36212(13) 0.0260(5) Uani 1 1 d . . .
C1 C -0.3343(4) -1.0326(3) 0.2029(2) 0.0405(9) Uani 1 1 d . . .
H1A H -0.4442 -1.0575 0.1788 0.049 Uiso 1 1 calc R . .
H1B H -0.3258 -0.9559 0.1723 0.049 Uiso 1 1 calc R . .
C2 C -0.3561(4) -1.0466(2) 0.30567(19) 0.0228(6) Uani 1 1 d . . .
N1 N -0.1717(3) -1.09131(17) 0.17814(14) 0.0199(5) Uani 1 1 d . . .
H1C H -0.2073 -1.1386 0.1456 0.024 Uiso 1 1 calc R . .
C3 C -0.0319(4) -1.0220(2) 0.12566(19) 0.0265(7) Uani 1 1 d . . .
H3A H -0.0925 -0.9596 0.0825 0.032 Uiso 1 1 calc R . .
H3B H 0.0403 -1.0618 0.0890 0.032 Uiso 1 1 calc R . .
C4 C 0.0955(4) -0.9838(2) 0.18924(18) 0.0216(6) Uani 1 1 d . . .
O3 O 0.2061(3) -0.91471(15) 0.15715(14) 0.0291(5) Uani 1 1 d . . .
O4 O 0.0774(3) -1.02488(14) 0.27654(13) 0.0248(5) Uani 1 1 d . . .
O5 O 0.2150(3) -0.55750(15) 0.08866(13) 0.0258(5) Uani 1 1 d . . .
O6 O 0.4553(3) -0.50513(17) 0.15104(15) 0.0351(5) Uani 1 1 d . . .
C5 C 0.2965(4) -0.3733(2) 0.0356(2) 0.0335(8) Uani 1 1 d . . .
H5A H 0.2966 -0.3231 0.0749 0.040 Uiso 1 1 calc R . .
H5B H 0.4011 -0.3579 -0.0066 0.040 Uiso 1 1 calc R . .
C6 C 0.3218(3) -0.4862(2) 0.09632(18) 0.0235(6) Uani 1 1 d . . .
N2 N 0.1254(3) -0.35368(17) -0.02004(15) 0.0212(5) Uani 1 1 d . . .
H2A H 0.1531 -0.3276 -0.0818 0.025 Uiso 1 1 calc R . .
C7 C -0.0124(4) -0.2805(2) 0.0072(2) 0.0284(7) Uani 1 1 d . . .
H7A H -0.0853 -0.2426 -0.0474 0.034 Uiso 1 1 calc R . .
H7B H 0.0505 -0.2267 0.0300 0.034 Uiso 1 1 calc R . .
C8 C -0.1388(4) -0.3402(2) 0.08189(17) 0.0215(6) Uani 1 1 d . . .
O7 O -0.2441(3) -0.28836(15) 0.12170(14) 0.0302(5) Uani 1 1 d . . .
O8 O -0.1333(3) -0.44217(14) 0.10118(13) 0.0237(4) Uani 1 1 d . . .
O9 O 0.4258(3) -0.32916(18) 0.25721(16) 0.0403(6) Uani 1 1 d . . .
O10 O 0.1717(3) -0.22648(16) 0.23229(13) 0.0289(5) Uani 1 1 d . . .
C9 C 0.2617(4) -0.3114(3) 0.3896(2) 0.0359(8) Uani 1 1 d . . .
H9A H 0.2592 -0.3895 0.4150 0.043 Uiso 1 1 calc R . .
H9B H 0.3679 -0.2865 0.4167 0.043 Uiso 1 1 calc R . .
C10 C 0.2863(4) -0.2866(2) 0.2848(2) 0.0250(6) Uani 1 1 d . . .
N3 N 0.0941(3) -0.26151(17) 0.41818(15) 0.0196(5) Uani 1 1 d . . .
H3C H 0.1250 -0.2161 0.4535 0.023 Uiso 1 1 calc R . .
C11 C -0.0383(4) -0.3368(2) 0.46840(18) 0.0259(7) Uani 1 1 d . . .
H11A H -0.1092 -0.3032 0.5102 0.031 Uiso 1 1 calc R . .
H11B H 0.0276 -0.4008 0.5065 0.031 Uiso 1 1 calc R . .
C12 C -0.1683(4) -0.3700(2) 0.40340(18) 0.0220(6) Uani 1 1 d . . .
O11 O -0.1649(3) -0.31911(14) 0.31826(12) 0.0223(4) Uani 1 1 d . . .
O12 O -0.2726(3) -0.44495(16) 0.43249(13) 0.0292(5) Uani 1 1 d . . .
O13 O -0.0109(3) -0.54084(14) 0.30978(13) 0.0248(4) Uani 1 1 d . . .
O14 O 0.1908(2) -0.68016(14) 0.32924(13) 0.0205(4) Uani 1 1 d . . .
C13 C 0.0411(3) -0.63117(19) 0.30132(17) 0.0174(6) Uani 1 1 d . . .
C14 C -0.0912(3) -0.6900(2) 0.25318(17) 0.0187(6) Uani 1 1 d . . .
O15 O -0.2499(3) -0.64899(15) 0.23648(15) 0.0297(5) Uani 1 1 d . . .
O16 O -0.0309(3) -0.77322(15) 0.23253(13) 0.0264(5) Uani 1 1 d . . .
C15 C -0.0662(3) -0.94961(19) 0.49076(17) 0.0184(6) Uani 1 1 d . . .
O17 O -0.2112(2) -0.95775(15) 0.53649(13) 0.0236(4) Uani 1 1 d . . .
O18 O -0.0164(3) -0.86760(15) 0.43237(13) 0.0264(5) Uani 1 1 d . . .
O1W O 0.4356(3) -0.84850(16) 0.46207(13) 0.0291(5) Uani 1 1 d . . .
H1WA H 0.5399 -0.8829 0.4654 0.044 Uiso 1 1 d R . .
H1WB H 0.3780 -0.8734 0.5130 0.044 Uiso 1 1 d R . .
O2W O 0.4446(3) -0.75036(16) 0.20163(15) 0.0312(5) Uani 1 1 d . . .
H2WA H 0.5477 -0.7402 0.2247 0.047 Uiso 1 1 d R . .
H2WB H 0.3884 -0.6894 0.1786 0.047 Uiso 1 1 d R . .
O3W O -0.5307(3) -0.57510(18) 0.37547(15) 0.0382(6) Uani 1 1 d . . .
H3WA H -0.6325 -0.5864 0.3518 0.057 Uiso 1 1 d R . .
H3WB H -0.5522 -0.5480 0.4215 0.057 Uiso 1 1 d R . .


_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 2.3819(19) 1_655 ?
La1 O18 2.5030(19) . ?
La1 O14 2.5373(18) . ?
La1 O16 2.5442(18) . ?
La1 O2W 2.5471(19) . ?
La1 O4 2.5562(19) . ?
La1 O1W 2.566(2) . ?
La1 O17 2.5689(17) 2_536 ?
La1 O3 2.654(2) . ?
La1 C4 2.940(3) . ?
La2 O9 2.381(2) 1_455 ?
La2 O6 2.402(2) 1_455 ?
La2 O3W 2.504(2) . ?
La2 O13 2.5224(18) . ?
La2 O11 2.5476(19) . ?
La2 O15 2.555(2) . ?
La2 O7 2.6188(19) . ?
La2 O8 2.6350(18) . ?
La2 O12 2.699(2) . ?
La2 C12 2.971(3) . ?
La2 C8 2.972(3) . ?
Ni1 O5 2.0224(18) 2_545 ?
Ni1 O5 2.0224(18) . ?
Ni1 O8 2.0491(18) . ?
Ni1 O8 2.0491(18) 2_545 ?
Ni1 N2 2.062(2) . ?
Ni1 N2 2.062(2) 2_545 ?
Ni2 O10 2.0026(19) . ?
Ni2 O2 2.0268(18) 1_565 ?
Ni2 N1 2.035(2) 1_565 ?
Ni2 O11 2.0456(19) . ?
Ni2 N3 2.050(2) . ?
Ni2 O4 2.0671(19) 1_565 ?
O1 C2 1.237(3) . ?
O1 La1 2.3819(19) 1_455 ?
O2 C2 1.243(3) . ?
O2 Ni2 2.0268(18) 1_545 ?
C1 N1 1.461(4) . ?
C1 C2 1.490(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
N1 C3 1.454(3) . ?
N1 Ni2 2.035(2) 1_545 ?
N1 H1C 0.9100 . ?
C3 C4 1.502(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 O3 1.216(3) . ?
C4 O4 1.267(3) . ?
O4 Ni2 2.0671(19) 1_545 ?
O5 C6 1.247(3) . ?
O6 C6 1.236(3) . ?
O6 La2 2.402(2) 1_655 ?
C5 N2 1.464(4) . ?
C5 C6 1.490(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
N2 C7 1.461(3) . ?
N2 H2A 0.9100 . ?
C7 C8 1.497(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O7 1.231(3) . ?
C8 O8 1.257(3) . ?
O9 C10 1.241(3) . ?
O9 La2 2.381(2) 1_655 ?
O10 C10 1.233(3) . ?
C9 N3 1.454(4) . ?
C9 C10 1.507(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
N3 C11 1.445(3) . ?
N3 H3C 0.9100 . ?
C11 C12 1.498(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 O12 1.229(3) . ?
C12 O11 1.256(3) . ?
O13 C13 1.234(3) . ?
O14 C13 1.242(3) . ?
C13 C14 1.528(4) . ?
C14 O15 1.238(3) . ?
C14 O16 1.240(3) . ?
C15 O18 1.236(3) . ?
C15 O17 1.236(3) . ?
C15 C15 1.535(5) 2_536 ?
O17 La1 2.5689(17) 2_536 ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8499 . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8500 . ?
O3W H3WA 0.8499 . ?
O3W H3WB 0.8499 . ?

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 O18 134.79(6) 1_655 . ?
O1 La1 O14 133.77(7) 1_655 . ?
O18 La1 O14 71.47(6) . . ?
O1 La1 O16 149.74(7) 1_655 . ?
O18 La1 O16 69.64(6) . . ?
O14 La1 O16 63.24(6) . . ?
O1 La1 O2W 80.35(7) 1_655 . ?
O18 La1 O2W 140.26(6) . . ?
O14 La1 O2W 69.55(6) . . ?
O16 La1 O2W 86.14(6) . . ?
O1 La1 O4 86.10(7) 1_655 . ?
O18 La1 O4 86.69(6) . . ?
O14 La1 O4 139.02(6) . . ?
O16 La1 O4 76.89(6) . . ?
O2W La1 O4 118.80(7) . . ?
O1 La1 O1W 75.28(7) 1_655 . ?
O18 La1 O1W 81.97(7) . . ?
O14 La1 O1W 72.50(6) . . ?
O16 La1 O1W 132.84(6) . . ?
O2W La1 O1W 93.42(7) . . ?
O4 La1 O1W 139.54(6) . . ?
O1 La1 O17 72.81(6) 1_655 2_536 ?
O18 La1 O17 63.08(6) . 2_536 ?
O14 La1 O17 124.85(6) . 2_536 ?
O16 La1 O17 121.62(6) . 2_536 ?
O2W La1 O17 151.81(6) . 2_536 ?
O4 La1 O17 68.42(6) . 2_536 ?
O1W La1 O17 71.82(6) . 2_536 ?
O1 La1 O3 83.14(7) 1_655 . ?
O18 La1 O3 123.10(6) . . ?
O14 La1 O3 115.97(6) . . ?
O16 La1 O3 66.76(6) . . ?
O2W La1 O3 69.76(7) . . ?
O4 La1 O3 49.40(6) . . ?
O1W La1 O3 154.72(6) . . ?
O17 La1 O3 114.35(6) 2_536 . ?
O1 La1 C4 87.54(8) 1_655 . ?
O18 La1 C4 103.64(7) . . ?
O14 La1 C4 127.74(6) . . ?
O16 La1 C4 66.47(7) . . ?
O2W La1 C4 94.18(7) . . ?
O4 La1 C4 25.43(6) . . ?
O1W La1 C4 159.76(6) . . ?
O17 La1 C4 93.13(7) 2_536 . ?
O3 La1 C4 24.43(6) . . ?
O9 La2 O6 79.47(8) 1_455 1_455 ?
O9 La2 O3W 80.97(8) 1_455 . ?
O6 La2 O3W 81.41(7) 1_455 . ?
O9 La2 O13 150.15(8) 1_455 . ?
O6 La2 O13 130.37(7) 1_455 . ?
O3W La2 O13 101.26(7) . . ?
O9 La2 O11 78.29(7) 1_455 . ?
O6 La2 O11 151.26(6) 1_455 . ?
O3W La2 O11 112.58(7) . . ?
O13 La2 O11 73.38(6) . . ?
O9 La2 O15 144.23(7) 1_455 . ?
O6 La2 O15 69.43(7) 1_455 . ?
O3W La2 O15 77.38(7) . . ?
O13 La2 O15 63.16(6) . . ?
O11 La2 O15 136.54(6) . . ?
O9 La2 O7 75.77(7) 1_455 . ?
O6 La2 O7 89.20(7) 1_455 . ?
O3W La2 O7 156.16(7) . . ?
O13 La2 O7 101.50(6) . . ?
O11 La2 O7 67.83(6) . . ?
O15 La2 O7 119.71(7) . . ?
O9 La2 O8 119.40(7) 1_455 . ?
O6 La2 O8 77.13(7) 1_455 . ?
O3W La2 O8 146.39(7) . . ?
O13 La2 O8 74.57(6) . . ?
O11 La2 O8 98.36(6) . . ?
O15 La2 O8 71.02(6) . . ?
O7 La2 O8 49.07(6) . . ?
O9 La2 O12 83.17(7) 1_455 . ?
O6 La2 O12 144.70(7) 1_455 . ?
O3W La2 O12 65.58(7) . . ?
O13 La2 O12 71.22(6) . . ?
O11 La2 O12 48.75(6) . . ?
O15 La2 O12 112.47(6) . . ?
O7 La2 O12 115.95(6) . . ?
O8 La2 O12 137.95(6) . . ?
O9 La2 C12 83.48(8) 1_455 . ?
O6 La2 C12 161.84(7) 1_455 . ?
O3W La2 C12 89.83(7) . . ?
O13 La2 C12 66.85(7) . . ?
O11 La2 C12 24.82(6) . . ?
O15 La2 C12 124.23(7) . . ?
O7 La2 C12 92.64(7) . . ?
O8 La2 C12 117.24(7) . . ?
O12 La2 C12 24.44(6) . . ?
O9 La2 C8 98.75(7) 1_455 . ?
O6 La2 C8 85.36(7) 1_455 . ?
O3W La2 C8 166.60(7) . . ?
O13 La2 C8 85.70(6) . . ?
O11 La2 C8 80.28(7) . . ?
O15 La2 C8 96.00(7) . . ?
O7 La2 C8 24.40(7) . . ?
O8 La2 C8 24.98(6) . . ?
O12 La2 C8 127.79(7) . . ?
C12 La2 C8 103.48(7) . . ?
O5 Ni1 O5 180.0 2_545 . ?
O5 Ni1 O8 89.63(8) 2_545 . ?
O5 Ni1 O8 90.37(8) . . ?
O5 Ni1 O8 90.37(8) 2_545 2_545 ?
O5 Ni1 O8 89.63(8) . 2_545 ?
O8 Ni1 O8 180.0 . 2_545 ?
O5 Ni1 N2 96.13(8) 2_545 . ?
O5 Ni1 N2 83.87(8) . . ?
O8 Ni1 N2 80.47(8) . . ?
O8 Ni1 N2 99.53(8) 2_545 . ?
O5 Ni1 N2 83.87(8) 2_545 2_545 ?
O5 Ni1 N2 96.13(8) . 2_545 ?
O8 Ni1 N2 99.53(8) . 2_545 ?
O8 Ni1 N2 80.47(8) 2_545 2_545 ?
N2 Ni1 N2 180.00(12) . 2_545 ?
O10 Ni2 O2 177.52(7) . 1_565 ?
O10 Ni2 N1 93.87(8) . 1_565 ?
O2 Ni2 N1 84.19(8) 1_565 1_565 ?
O10 Ni2 O11 91.06(8) . . ?
O2 Ni2 O11 90.77(8) 1_565 . ?
N1 Ni2 O11 98.74(8) 1_565 . ?
O10 Ni2 N3 84.38(8) . . ?
O2 Ni2 N3 97.59(8) 1_565 . ?
N1 Ni2 N3 177.87(8) 1_565 . ?
O11 Ni2 N3 80.09(8) . . ?
O10 Ni2 O4 89.68(8) . 1_565 ?
O2 Ni2 O4 88.45(8) 1_565 1_565 ?
N1 Ni2 O4 79.50(8) 1_565 1_565 ?
O11 Ni2 O4 178.14(7) . 1_565 ?
N3 Ni2 O4 101.68(8) . 1_565 ?
C2 O1 La1 160.1(2) . 1_455 ?
C2 O2 Ni2 112.67(17) . 1_545 ?
N1 C1 C2 113.8(2) . . ?
N1 C1 H1A 108.8 . . ?
C2 C1 H1A 108.8 . . ?
N1 C1 H1B 108.8 . . ?
C2 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
O1 C2 O2 123.1(3) . . ?
O1 C2 C1 116.7(2) . . ?
O2 C2 C1 120.1(2) . . ?
C3 N1 C1 114.4(2) . . ?
C3 N1 Ni2 104.47(16) . 1_545 ?
C1 N1 Ni2 108.17(16) . 1_545 ?
C3 N1 H1C 109.9 . . ?
C1 N1 H1C 109.9 . . ?
Ni2 N1 H1C 109.9 1_545 . ?
N1 C3 C4 111.8(2) . . ?
N1 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
N1 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
O3 C4 O4 122.7(3) . . ?
O3 C4 C3 120.6(2) . . ?
O4 C4 C3 116.6(2) . . ?
O3 C4 La1 64.50(15) . . ?
O4 C4 La1 60.08(14) . . ?
C3 C4 La1 163.71(19) . . ?
C4 O3 La1 91.07(16) . . ?
C4 O4 Ni2 109.49(17) . 1_545 ?
C4 O4 La1 94.49(16) . . ?
Ni2 O4 La1 155.35(9) 1_545 . ?
C6 O5 Ni1 113.68(16) . . ?
C6 O6 La2 153.88(19) . 1_655 ?
N2 C5 C6 113.9(2) . . ?
N2 C5 H5A 108.8 . . ?
C6 C5 H5A 108.8 . . ?
N2 C5 H5B 108.8 . . ?
C6 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
O6 C6 O5 122.8(2) . . ?
O6 C6 C5 116.9(3) . . ?
O5 C6 C5 120.3(2) . . ?
C7 N2 C5 114.9(2) . . ?
C7 N2 Ni1 105.59(16) . . ?
C5 N2 Ni1 107.79(16) . . ?
C7 N2 H2A 109.5 . . ?
C5 N2 H2A 109.5 . . ?
Ni1 N2 H2A 109.5 . . ?
N2 C7 C8 111.9(2) . . ?
N2 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
N2 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
O7 C8 O8 122.6(2) . . ?
O7 C8 C7 119.3(2) . . ?
O8 C8 C7 118.2(2) . . ?
O7 C8 La2 61.50(13) . . ?
O8 C8 La2 62.32(13) . . ?
C7 C8 La2 168.71(19) . . ?
C8 O7 La2 94.10(15) . . ?
C8 O8 Ni1 112.19(16) . . ?
C8 O8 La2 92.70(15) . . ?
Ni1 O8 La2 154.96(8) . . ?
C10 O9 La2 159.21(19) . 1_655 ?
C10 O10 Ni2 114.17(18) . . ?
N3 C9 C10 113.9(2) . . ?
N3 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
N3 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
O10 C10 O9 124.0(3) . . ?
O10 C10 C9 119.8(2) . . ?
O9 C10 C9 116.1(2) . . ?
C11 N3 C9 115.1(2) . . ?
C11 N3 Ni2 105.43(16) . . ?
C9 N3 Ni2 107.69(16) . . ?
C11 N3 H3C 109.5 . . ?
C9 N3 H3C 109.5 . . ?
Ni2 N3 H3C 109.5 . . ?
N3 C11 C12 112.0(2) . . ?
N3 C11 H11A 109.2 . . ?
C12 C11 H11A 109.2 . . ?
N3 C11 H11B 109.2 . . ?
C12 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
O12 C12 O11 121.6(3) . . ?
O12 C12 C11 121.0(2) . . ?
O11 C12 C11 117.4(2) . . ?
O12 C12 La2 65.30(15) . . ?
O11 C12 La2 58.35(14) . . ?
C11 C12 La2 163.95(19) . . ?
C12 O11 Ni2 111.66(17) . . ?
C12 O11 La2 96.82(16) . . ?
Ni2 O11 La2 151.52(9) . . ?
C12 O12 La2 90.27(16) . . ?
C13 O13 La2 121.54(17) . . ?
C13 O14 La1 120.35(16) . . ?
O13 C13 O14 126.3(2) . . ?
O13 C13 C14 117.5(2) . . ?
O14 C13 C14 116.2(2) . . ?
O15 C14 O16 125.4(3) . . ?
O15 C14 C13 116.8(2) . . ?
O16 C14 C13 117.9(2) . . ?
C14 O15 La2 120.29(17) . . ?
C14 O16 La1 117.79(17) . . ?
O18 C15 O17 126.2(2) . . ?
O18 C15 C15 116.8(3) . 2_536 ?
O17 C15 C15 117.0(3) . 2_536 ?
C15 O17 La1 119.14(15) . 2_536 ?
C15 O18 La1 121.50(16) . . ?
La1 O1W H1WA 109.7 . . ?
La1 O1W H1WB 109.8 . . ?
H1WA O1W H1WB 108.2 . . ?
La1 O2W H2WA 111.3 . . ?
La1 O2W H2WB 111.6 . . ?
H2WA O2W H2WB 109.3 . . ?
La2 O3W H3WA 111.8 . . ?
La2 O3W H3WB 111.9 . . ?
H3WA O3W H3WB 109.6 . . ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         1.127
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.147

# Attachment 'complex2.cif'

data_complex2
_database_code_depnum_ccdc_archive 'CCDC 647831'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H23 N3 Nd2 Ni1.50 O22'
_chemical_formula_weight         973.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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                   7.1179(16)
_cell_length_b                   12.650(3)
_cell_length_c                   14.633(3)
_cell_angle_alpha                74.922(4)
_cell_angle_beta                 89.513(4)
_cell_angle_gamma                87.403(4)
_cell_volume                     1270.9(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    3592
_cell_measurement_theta_min      2.473
_cell_measurement_theta_max      28.310

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             944
_exptl_absorpt_coefficient_mu    5.227
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4885
_exptl_absorpt_correction_T_max  0.7444
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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_%        ?
_diffrn_reflns_number            6941
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.44
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4848
_reflns_number_gt                4427
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_cell_refinement       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0393P)²+3.0438P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4848
_refine_ls_number_parameters     403
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.0980
_refine_ls_wR_factor_gt          0.0946
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.005
_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
Nd1 Nd 0.24989(3) -0.875080(18) 0.326326(17) 0.00631(6) Uani 1 1 d . . .
Nd2 Nd -0.32195(3) -0.459808(18) 0.254793(17) 0.00689(6) Uani 1 1 d . . .
Ni1 Ni 0.0000 -0.5000 0.0000 0.00745(19) Uani 1 2 d S . .
Ni2 Ni -0.03682(8) -0.17326(4) 0.29976(4) 0.00701(13) Uani 1 1 d . . .
O1 O -0.4791(5) -0.9869(3) 0.3343(2) 0.0166(9) Uani 1 1 d . . .
O2 O -0.2569(5) -1.1163(3) 0.3642(2) 0.0113(8) Uani 1 1 d . . .
C1 C -0.3330(7) -1.0282(4) 0.2037(3) 0.0193(13) Uani 1 1 d . . .
H1A H -0.4470 -1.0521 0.1780 0.023 Uiso 1 1 calc R . .
H1B H -0.3224 -0.9489 0.1739 0.023 Uiso 1 1 calc R . .
C2 C -0.3554(6) -1.0453(4) 0.3079(3) 0.0091(11) Uani 1 1 d . . .
N1 N -0.1675(5) -1.0880(3) 0.1781(3) 0.0087(9) Uani 1 1 d . . .
H1C H -0.2048 -1.1360 0.1439 0.010 Uiso 1 1 calc R . .
C3 C -0.0251(7) -1.0176(4) 0.1255(3) 0.0141(12) Uani 1 1 d . . .
H3A H -0.0868 -0.9525 0.0817 0.017 Uiso 1 1 calc R . .
H3B H 0.0507 -1.0579 0.0874 0.017 Uiso 1 1 calc R . .
C4 C 0.1008(7) -0.9819(3) 0.1925(3) 0.0091(11) Uani 1 1 d . . .
O3 O 0.2195(5) -0.9133(2) 0.1619(2) 0.0109(8) Uani 1 1 d . . .
O4 O 0.0788(5) -1.0217(2) 0.2806(2) 0.0107(8) Uani 1 1 d . . .
O5 O 0.2213(5) -0.5598(2) 0.0881(2) 0.0115(8) Uani 1 1 d . . .
O6 O 0.4613(5) -0.5059(3) 0.1529(2) 0.0166(9) Uani 1 1 d . . .
C5 C 0.2981(7) -0.3727(4) 0.0382(4) 0.0146(12) Uani 1 1 d . . .
H5A H 0.2911 -0.3229 0.0804 0.018 Uiso 1 1 calc R . .
H5B H 0.4092 -0.3538 -0.0030 0.018 Uiso 1 1 calc R . .
C6 C 0.3271(6) -0.4874(4) 0.0975(3) 0.0085(6) Uani 1 1 d U . .
N2 N 0.1290(5) -0.3524(3) -0.0216(3) 0.0082(9) Uani 1 1 d . . .
H2A H 0.1611 -0.3262 -0.0850 0.010 Uiso 1 1 calc R . .
C7 C -0.0126(7) -0.2789(4) 0.0053(3) 0.0105(11) Uani 1 1 d . . .
H7A H -0.0883 -0.2409 -0.0511 0.013 Uiso 1 1 calc R . .
H7B H 0.0512 -0.2225 0.0280 0.013 Uiso 1 1 calc R . .
C8 C -0.1404(7) -0.3384(4) 0.0809(3) 0.0095(11) Uani 1 1 d . . .
O7 O -0.2522(5) -0.2884(3) 0.1208(2) 0.0136(8) Uani 1 1 d . . .
O8 O -0.1264(5) -0.4427(2) 0.1048(2) 0.0112(8) Uani 1 1 d . . .
O9 O 0.4351(5) -0.3317(3) 0.2571(3) 0.0184(9) Uani 1 1 d . . .
O10 O 0.1823(5) -0.2232(3) 0.2325(2) 0.0155(9) Uani 1 1 d . . .
C9 C 0.2684(7) -0.3141(4) 0.3912(4) 0.0150(12) Uani 1 1 d . . .
H9A H 0.2641 -0.3945 0.4167 0.018 Uiso 1 1 calc R . .
H9B H 0.3783 -0.2897 0.4200 0.018 Uiso 1 1 calc R . .
C10 C 0.2962(7) -0.2887(4) 0.2858(3) 0.0119(11) Uani 1 1 d . . .
N3 N 0.0991(5) -0.2632(3) 0.4196(3) 0.0101(9) Uani 1 1 d . . .
H3C H 0.1313 -0.2170 0.4565 0.012 Uiso 1 1 calc R . .
C11 C -0.0404(7) -0.3385(4) 0.4694(3) 0.0098(11) Uani 1 1 d . . .
H11A H -0.1165 -0.3029 0.5109 0.012 Uiso 1 1 calc R . .
H11B H 0.0247 -0.4048 0.5099 0.012 Uiso 1 1 calc R . .
C12 C -0.1679(7) -0.3713(4) 0.4009(3) 0.0103(11) Uani 1 1 d . . .
O11 O -0.1568(5) -0.3210(2) 0.3149(2) 0.0105(8) Uani 1 1 d . . .
O12 O -0.2735(5) -0.4479(2) 0.4289(2) 0.0119(8) Uani 1 1 d . . .
O13 O -0.0072(5) -0.5392(2) 0.3094(2) 0.0114(8) Uani 1 1 d . . .
O14 O 0.1962(4) -0.6823(2) 0.3318(2) 0.0087(8) Uani 1 1 d . . .
C13 C 0.0471(6) -0.6314(4) 0.3025(3) 0.0079(6) Uani 1 1 d U . .
C14 C -0.0871(6) -0.6904(4) 0.2535(3) 0.0078(6) Uani 1 1 d U . .
O15 O -0.2474(5) -0.6476(3) 0.2352(2) 0.0113(5) Uani 1 1 d U . .
O16 O -0.0259(5) -0.7753(2) 0.2340(2) 0.0100(8) Uani 1 1 d . . .
C15 C -0.0689(6) -0.9489(3) 0.4901(3) 0.0068(6) Uani 1 1 d U . .
O17 O -0.2170(4) -0.9581(2) 0.5350(2) 0.0092(8) Uani 1 1 d . . .
O18 O -0.0154(5) -0.8665(2) 0.4316(2) 0.0111(8) Uani 1 1 d . . .
O1W O 0.4337(5) -0.8457(2) 0.4605(2) 0.0112(8) Uani 1 1 d . . .
H1WA H 0.5380 -0.8801 0.4639 0.017 Uiso 1 1 d R . .
H1WB H 0.3761 -0.8706 0.5114 0.017 Uiso 1 1 d R . .
O2W O 0.4441(5) -0.7533(3) 0.2044(2) 0.0119(8) Uani 1 1 d . . .
H2WA H 0.5472 -0.7431 0.2275 0.018 Uiso 1 1 d R . .
H2WB H 0.3879 -0.6923 0.1814 0.018 Uiso 1 1 d R . .
O3W O -0.5192(5) -0.5760(3) 0.3724(2) 0.0176(9) Uani 1 1 d . . .
H3WA H -0.6210 -0.5873 0.3488 0.026 Uiso 1 1 d R . .
H3WB H -0.5408 -0.5489 0.4185 0.026 Uiso 1 1 d R . .
O4W O 1.374(2) -1.1150(7) 0.0355(8) 0.078(4) Uani 0.50 1 d P . .
O4W' O 1.5236(16) -1.1209(9) -0.0044(8) 0.061(4) Uani 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
Nd1 O1 2.325(3) 1_655 ?
Nd1 O18 2.443(3) . ?
Nd1 O14 2.473(3) . ?
Nd1 O1W 2.484(3) . ?
Nd1 O2W 2.487(3) . ?
Nd1 O16 2.491(3) . ?
Nd1 O4 2.497(3) . ?
Nd1 O17 2.537(3) 2_536 ?
Nd1 O3 2.588(3) . ?
Nd1 C4 2.885(5) . ?
Nd2 O9 2.322(3) 1_455 ?
Nd2 O6 2.348(4) 1_455 ?
Nd2 O3W 2.434(3) . ?
Nd2 O13 2.465(3) . ?
Nd2 O15 2.500(3) . ?
Nd2 O11 2.500(3) . ?
Nd2 O8 2.556(3) . ?
Nd2 O7 2.581(3) . ?
Nd2 O12 2.618(3) . ?
Nd2 C12 2.902(5) . ?
Nd2 C8 2.931(5) . ?
Ni1 O5 2.034(3) . ?
Ni1 O5 2.034(3) 2_545 ?
Ni1 O8 2.044(3) . ?
Ni1 O8 2.044(3) 2_545 ?
Ni1 N2 2.067(4) . ?
Ni1 N2 2.067(4) 2_545 ?
Ni2 O10 2.002(4) . ?
Ni2 O2 2.022(3) 1_565 ?
Ni2 N1 2.034(4) 1_565 ?
Ni2 N3 2.048(4) . ?
Ni2 O11 2.049(3) . ?
Ni2 O4 2.072(3) 1_565 ?
O1 C2 1.247(6) . ?
O1 Nd1 2.325(3) 1_455 ?
O2 C2 1.244(5) . ?
O2 Ni2 2.022(3) 1_545 ?
C1 N1 1.470(6) . ?
C1 C2 1.490(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
N1 C3 1.457(6) . ?
N1 Ni2 2.034(4) 1_545 ?
N1 H1C 0.9300 . ?
C3 C4 1.500(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O3 1.235(5) . ?
C4 O4 1.266(5) . ?
O4 Ni2 2.072(3) 1_545 ?
O5 C6 1.247(6) . ?
O6 C6 1.232(6) . ?
O6 Nd2 2.348(4) 1_655 ?
C5 N2 1.467(6) . ?
C5 C6 1.491(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
N2 C7 1.461(6) . ?
N2 H2A 0.9300 . ?
C7 C8 1.494(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 O7 1.230(6) . ?
C8 O8 1.274(5) . ?
O9 C10 1.230(6) . ?
O9 Nd2 2.322(3) 1_655 ?
O10 C10 1.252(5) . ?
C9 N3 1.449(6) . ?
C9 C10 1.504(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
N3 C11 1.462(6) . ?
N3 H3C 0.9300 . ?
C11 C12 1.505(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 O12 1.236(6) . ?
C12 O11 1.257(5) . ?
O13 C13 1.241(5) . ?
O14 C13 1.236(5) . ?
C13 C14 1.529(7) . ?
C14 O16 1.240(5) . ?
C14 O15 1.241(5) . ?
C15 O17 1.231(6) . ?
C15 O18 1.238(5) . ?
C15 C15 1.552(8) 2_536 ?
O17 Nd1 2.537(3) 2_536 ?
O1W H1WA 0.8382 . ?
O1W H1WB 0.8409 . ?
O2W H2WA 0.8393 . ?
O2W H2WB 0.8412 . ?
O3W H3WA 0.8394 . ?
O3W H3WB 0.8415 . ?
O4W O4W' 1.218(17) . ?

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 Nd1 O18 135.15(11) 1_655 . ?
O1 Nd1 O14 132.62(12) 1_655 . ?
O18 Nd1 O14 71.95(10) . . ?
O1 Nd1 O1W 74.96(12) 1_655 . ?
O18 Nd1 O1W 82.83(11) . . ?
O14 Nd1 O1W 71.51(10) . . ?
O1 Nd1 O2W 80.02(11) 1_655 . ?
O18 Nd1 O2W 140.69(10) . . ?
O14 Nd1 O2W 69.85(11) . . ?
O1W Nd1 O2W 93.60(11) . . ?
O1 Nd1 O16 149.33(12) 1_655 . ?
O18 Nd1 O16 69.73(10) . . ?
O14 Nd1 O16 64.47(10) . . ?
O1W Nd1 O16 133.29(11) . . ?
O2W Nd1 O16 85.64(10) . . ?
O1 Nd1 O4 87.15(12) 1_655 . ?
O18 Nd1 O4 85.74(11) . . ?
O14 Nd1 O4 139.21(10) . . ?
O1W Nd1 O4 140.21(10) . . ?
O2W Nd1 O4 118.30(11) . . ?
O16 Nd1 O4 75.99(10) . . ?
O1 Nd1 O17 72.00(11) 1_655 2_536 ?
O18 Nd1 O17 64.24(10) . 2_536 ?
O14 Nd1 O17 125.55(10) . 2_536 ?
O1W Nd1 O17 72.44(10) . 2_536 ?
O2W Nd1 O17 151.08(10) . 2_536 ?
O16 Nd1 O17 122.51(10) . 2_536 ?
O4 Nd1 O17 68.27(10) . 2_536 ?
O1 Nd1 O3 82.46(11) 1_655 . ?
O18 Nd1 O3 124.01(11) . . ?
O14 Nd1 O3 116.29(10) . . ?
O1W Nd1 O3 153.03(11) . . ?
O2W Nd1 O3 67.74(11) . . ?
O16 Nd1 O3 67.00(10) . . ?
O4 Nd1 O3 50.76(10) . . ?
O17 Nd1 O3 114.47(10) 2_536 . ?
O1 Nd1 C4 88.02(13) 1_655 . ?
O18 Nd1 C4 103.34(12) . . ?
O14 Nd1 C4 128.11(11) . . ?
O1W Nd1 C4 160.35(11) . . ?
O2W Nd1 C4 93.03(12) . . ?
O16 Nd1 C4 65.69(11) . . ?
O4 Nd1 C4 25.95(11) . . ?
O17 Nd1 C4 93.21(11) 2_536 . ?
O3 Nd1 C4 25.34(11) . . ?
O9 Nd2 O6 79.51(13) 1_455 1_455 ?
O9 Nd2 O3W 81.83(12) 1_455 . ?
O6 Nd2 O3W 80.94(12) 1_455 . ?
O9 Nd2 O13 149.16(12) 1_455 . ?
O6 Nd2 O13 131.32(11) 1_455 . ?
O3W Nd2 O13 100.67(11) . . ?
O9 Nd2 O15 143.92(12) 1_455 . ?
O6 Nd2 O15 68.96(11) 1_455 . ?
O3W Nd2 O15 76.43(11) . . ?
O13 Nd2 O15 64.43(11) . . ?
O9 Nd2 O11 78.41(12) 1_455 . ?
O6 Nd2 O11 151.19(10) 1_455 . ?
O3W Nd2 O11 113.75(12) . . ?
O13 Nd2 O11 72.45(10) . . ?
O15 Nd2 O11 136.86(10) . . ?
O9 Nd2 O8 119.66(11) 1_455 . ?
O6 Nd2 O8 78.38(12) 1_455 . ?
O3W Nd2 O8 146.28(11) . . ?
O13 Nd2 O8 74.43(11) . . ?
O15 Nd2 O8 71.40(10) . . ?
O11 Nd2 O8 96.83(11) . . ?
O9 Nd2 O7 73.74(11) 1_455 . ?
O6 Nd2 O7 88.06(11) 1_455 . ?
O3W Nd2 O7 154.68(11) . . ?
O13 Nd2 O7 103.69(10) . . ?
O15 Nd2 O7 120.65(11) . . ?
O11 Nd2 O7 68.11(10) . . ?
O8 Nd2 O7 50.18(10) . . ?
O9 Nd2 O12 82.58(12) 1_455 . ?
O6 Nd2 O12 143.17(12) 1_455 . ?
O3W Nd2 O12 64.77(11) . . ?
O13 Nd2 O12 71.25(11) . . ?
O15 Nd2 O12 112.59(10) . . ?
O11 Nd2 O12 50.37(10) . . ?
O8 Nd2 O12 138.20(11) . . ?
O7 Nd2 O12 117.27(10) . . ?
O9 Nd2 C12 82.63(13) 1_455 . ?
O6 Nd2 C12 160.86(13) 1_455 . ?
O3W Nd2 C12 89.80(13) . . ?
O13 Nd2 C12 66.72(12) . . ?
O15 Nd2 C12 125.19(11) . . ?
O11 Nd2 C12 25.54(11) . . ?
O8 Nd2 C12 116.93(12) . . ?
O7 Nd2 C12 93.53(12) . . ?
O12 Nd2 C12 25.19(11) . . ?
O9 Nd2 C8 97.42(12) 1_455 . ?
O6 Nd2 C8 85.25(13) 1_455 . ?
O3W Nd2 C8 166.07(13) . . ?
O13 Nd2 C8 87.14(12) . . ?
O15 Nd2 C8 97.00(12) . . ?
O11 Nd2 C8 79.51(12) . . ?
O8 Nd2 C8 25.69(11) . . ?
O7 Nd2 C8 24.75(11) . . ?
O12 Nd2 C8 129.05(12) . . ?
C12 Nd2 C8 103.94(13) . . ?
O5 Ni1 O5 180.0(3) . 2_545 ?
O5 Ni1 O8 89.37(13) . . ?
O5 Ni1 O8 90.63(13) 2_545 . ?
O5 Ni1 O8 90.63(13) . 2_545 ?
O5 Ni1 O8 89.37(13) 2_545 2_545 ?
O8 Ni1 O8 180.0 . 2_545 ?
O5 Ni1 N2 84.25(13) . . ?
O5 Ni1 N2 95.75(13) 2_545 . ?
O8 Ni1 N2 80.54(14) . . ?
O8 Ni1 N2 99.46(14) 2_545 . ?
O5 Ni1 N2 95.75(13) . 2_545 ?
O5 Ni1 N2 84.25(13) 2_545 2_545 ?
O8 Ni1 N2 99.46(14) . 2_545 ?
O8 Ni1 N2 80.54(14) 2_545 2_545 ?
N2 Ni1 N2 180.0 . 2_545 ?
O10 Ni2 O2 177.57(13) . 1_565 ?
O10 Ni2 N1 93.89(15) . 1_565 ?
O2 Ni2 N1 84.49(14) 1_565 1_565 ?
O10 Ni2 N3 84.24(15) . . ?
O2 Ni2 N3 97.42(14) 1_565 . ?
N1 Ni2 N3 177.83(16) 1_565 . ?
O10 Ni2 O11 90.36(14) . . ?
O2 Ni2 O11 91.67(13) 1_565 . ?
N1 Ni2 O11 98.87(14) 1_565 . ?
N3 Ni2 O11 80.08(14) . . ?
O10 Ni2 O4 89.92(14) . 1_565 ?
O2 Ni2 O4 88.00(13) 1_565 1_565 ?
N1 Ni2 O4 79.25(14) 1_565 1_565 ?
N3 Ni2 O4 101.80(14) . 1_565 ?
O11 Ni2 O4 178.11(13) . 1_565 ?
C2 O1 Nd1 158.2(3) . 1_455 ?
C2 O2 Ni2 112.2(3) . 1_545 ?
N1 C1 C2 113.3(4) . . ?
N1 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
O2 C2 O1 122.7(4) . . ?
O2 C2 C1 120.7(4) . . ?
O1 C2 C1 116.6(4) . . ?
C3 N1 C1 114.1(4) . . ?
C3 N1 Ni2 104.9(3) . 1_545 ?
C1 N1 Ni2 108.0(3) . 1_545 ?
C3 N1 H1C 109.9 . . ?
C1 N1 H1C 109.9 . . ?
Ni2 N1 H1C 109.9 1_545 . ?
N1 C3 C4 110.1(4) . . ?
N1 C3 H3A 109.6 . . ?
C4 C3 H3A 109.6 . . ?
N1 C3 H3B 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.2 . . ?
O3 C4 O4 121.3(4) . . ?
O3 C4 C3 120.2(4) . . ?
O4 C4 C3 118.4(4) . . ?
O3 C4 Nd1 63.7(3) . . ?
O4 C4 Nd1 59.6(2) . . ?
C3 C4 Nd1 163.8(3) . . ?
C4 O3 Nd1 90.9(3) . . ?
C4 O4 Ni2 107.7(3) . 1_545 ?
C4 O4 Nd1 94.4(3) . . ?
Ni2 O4 Nd1 156.56(15) 1_545 . ?
C6 O5 Ni1 113.2(3) . . ?
C6 O6 Nd2 154.4(3) . 1_655 ?
N2 C5 C6 114.9(4) . . ?
N2 C5 H5A 108.5 . . ?
C6 C5 H5A 108.5 . . ?
N2 C5 H5B 108.5 . . ?
C6 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
O6 C6 O5 123.1(4) . . ?
O6 C6 C5 116.7(4) . . ?
O5 C6 C5 120.2(4) . . ?
C7 N2 C5 113.7(4) . . ?
C7 N2 Ni1 104.6(3) . . ?
C5 N2 Ni1 107.1(3) . . ?
C7 N2 H2A 110.4 . . ?
C5 N2 H2A 110.4 . . ?
Ni1 N2 H2A 110.4 . . ?
N2 C7 C8 112.3(4) . . ?
N2 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
N2 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
O7 C8 O8 120.9(4) . . ?
O7 C8 C7 121.1(4) . . ?
O8 C8 C7 117.9(4) . . ?
O7 C8 Nd2 61.5(2) . . ?
O8 C8 Nd2 60.4(2) . . ?
C7 C8 Nd2 168.0(3) . . ?
C8 O7 Nd2 93.8(3) . . ?
C8 O8 Ni1 110.6(3) . . ?
C8 O8 Nd2 93.9(3) . . ?
Ni1 O8 Nd2 154.53(15) . . ?
C10 O9 Nd2 159.0(3) . 1_655 ?
C10 O10 Ni2 114.1(3) . . ?
N3 C9 C10 114.1(4) . . ?
N3 C9 H9A 108.7 . . ?
C10 C9 H9A 108.7 . . ?
N3 C9 H9B 108.7 . . ?
C10 C9 H9B 108.7 . . ?
H9A C9 H9B 107.6 . . ?
O9 C10 O10 123.5(5) . . ?
O9 C10 C9 117.3(4) . . ?
O10 C10 C9 119.2(4) . . ?
C9 N3 C11 115.6(4) . . ?
C9 N3 Ni2 108.1(3) . . ?
C11 N3 Ni2 104.6(3) . . ?
C9 N3 H3C 109.4 . . ?
C11 N3 H3C 109.4 . . ?
Ni2 N3 H3C 109.4 . . ?
N3 C11 C12 111.2(4) . . ?
N3 C11 H11A 109.4 . . ?
C12 C11 H11A 109.4 . . ?
N3 C11 H11B 109.4 . . ?
C12 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
O12 C12 O11 122.0(4) . . ?
O12 C12 C11 120.3(4) . . ?
O11 C12 C11 117.6(4) . . ?
O12 C12 Nd2 64.4(3) . . ?
O11 C12 Nd2 59.0(2) . . ?
C11 C12 Nd2 164.9(3) . . ?
C12 O11 Ni2 110.7(3) . . ?
C12 O11 Nd2 95.4(3) . . ?
Ni2 O11 Nd2 153.63(16) . . ?
C12 O12 Nd2 90.4(3) . . ?
C13 O13 Nd2 121.7(3) . . ?
C13 O14 Nd1 120.6(3) . . ?
O14 C13 O13 127.8(4) . . ?
O14 C13 C14 115.7(4) . . ?
O13 C13 C14 116.5(4) . . ?
O16 C14 O15 125.7(4) . . ?
O16 C14 C13 117.6(4) . . ?
O15 C14 C13 116.7(4) . . ?
C14 O15 Nd2 120.0(3) . . ?
C14 O16 Nd1 117.4(3) . . ?
O17 C15 O18 127.3(4) . . ?
O17 C15 C15 116.9(5) . 2_536 ?
O18 C15 C15 115.8(5) . 2_536 ?
C15 O17 Nd1 118.4(3) . 2_536 ?
C15 O18 Nd1 121.9(3) . . ?
Nd1 O1W H1WA 109.3 . . ?
Nd1 O1W H1WB 109.5 . . ?
H1WA O1W H1WB 107.9 . . ?
Nd1 O2W H2WA 110.7 . . ?
Nd1 O2W H2WB 111.5 . . ?
H2WA O2W H2WB 109.2 . . ?
Nd2 O3W H3WA 111.6 . . ?
Nd2 O3W H3WB 111.4 . . ?
H3WA O3W H3WB 109.9 . . ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         1.983
_refine_diff_density_min         -1.124
_refine_diff_density_rms         0.201

# Attachment 'complex3.cif'

data_complex3
_database_code_depnum_ccdc_archive 'CCDC 647832'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H23 Eu2 N3 Ni1.50 O22'
_chemical_formula_weight         989.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   7.0976(19)
_cell_length_b                   12.604(3)
_cell_length_c                   14.654(4)
_cell_angle_alpha                74.981(5)
_cell_angle_beta                 89.720(5)
_cell_angle_gamma                87.365(5)
_cell_volume                     1264.7(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    2975
_cell_measurement_theta_min      2.475
_cell_measurement_theta_max      27.942

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             956
_exptl_absorpt_coefficient_mu    6.107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4819
_exptl_absorpt_correction_T_max  0.7499
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      223(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_%        ?
_diffrn_reflns_number            6818
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.44
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4768
_reflns_number_gt                4079
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_cell_refinement       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0517P)²+0.4726P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4768
_refine_ls_number_parameters     394
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0430
_refine_ls_wR_factor_ref         0.1020
_refine_ls_wR_factor_gt          0.0977
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.015
_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
Eu1 Eu 0.24712(3) -0.876202(18) 0.327451(16) 0.00928(6) Uani 1 1 d . . .
Eu2 Eu -0.31977(3) -0.460899(18) 0.252987(17) 0.01079(6) Uani 1 1 d . . .
Ni1 Ni 0.0000 -0.5000 0.0000 0.0120(2) Uani 1 2 d S . .
Ni2 Ni -0.03610(9) -0.17337(5) 0.29875(5) 0.01551(16) Uani 1 1 d . . .
O1 O -0.4832(5) -0.9867(3) 0.3357(3) 0.0239(10) Uani 1 1 d . . .
O2 O -0.2601(5) -1.1176(3) 0.3640(2) 0.0219(10) Uani 1 1 d . . .
C1 C -0.3319(8) -1.0237(5) 0.2037(4) 0.0297(16) Uani 1 1 d . . .
H1A H -0.4462 -1.0424 0.1751 0.036 Uiso 1 1 calc R . .
H1B H -0.3145 -0.9450 0.1771 0.036 Uiso 1 1 calc R . .
C2 C -0.3598(7) -1.0450(4) 0.3083(4) 0.0171(13) Uani 1 1 d . . .
N1 N -0.1706(6) -1.0859(3) 0.1781(3) 0.0177(11) Uani 1 1 d . . .
H1C H -0.2101 -1.1326 0.1438 0.021 Uiso 1 1 calc R . .
C3 C -0.0242(8) -1.0169(4) 0.1268(4) 0.0205(13) Uani 1 1 d . . .
H3A H -0.0834 -0.9522 0.0825 0.025 Uiso 1 1 calc R . .
H3B H 0.0510 -1.0583 0.0903 0.025 Uiso 1 1 calc R . .
C4 C 0.1007(7) -0.9809(4) 0.1926(4) 0.0165(13) Uani 1 1 d . . .
O3 O 0.2224(5) -0.9130(3) 0.1633(3) 0.0212(9) Uani 1 1 d . . .
O4 O 0.0773(5) -1.0209(3) 0.2814(2) 0.0192(9) Uani 1 1 d . . .
O5 O 0.2228(5) -0.5597(3) 0.0878(2) 0.0171(9) Uani 1 1 d . . .
O6 O 0.4646(5) -0.5066(3) 0.1535(3) 0.0249(10) Uani 1 1 d . . .
C5 C 0.2978(8) -0.3722(4) 0.0382(4) 0.0219(14) Uani 1 1 d . . .
H5A H 0.2913 -0.3228 0.0800 0.026 Uiso 1 1 calc R . .
H5B H 0.4070 -0.3529 -0.0029 0.026 Uiso 1 1 calc R . .
C6 C 0.3303(7) -0.4865(4) 0.0971(4) 0.0151(12) Uani 1 1 d . . .
N2 N 0.1279(6) -0.3519(3) -0.0207(3) 0.0134(10) Uani 1 1 d . . .
H2A H 0.1592 -0.3258 -0.0832 0.016 Uiso 1 1 calc R . .
C7 C -0.0149(7) -0.2778(4) 0.0059(4) 0.0203(14) Uani 1 1 d . . .
H7A H -0.0904 -0.2401 -0.0499 0.024 Uiso 1 1 calc R . .
H7B H 0.0476 -0.2220 0.0290 0.024 Uiso 1 1 calc R . .
C8 C -0.1410(7) -0.3396(4) 0.0807(4) 0.0152(12) Uani 1 1 d . . .
O7 O -0.2560(6) -0.2882(3) 0.1200(3) 0.0249(10) Uani 1 1 d . . .
O8 O -0.1285(5) -0.4427(3) 0.1058(2) 0.0183(9) Uani 1 1 d . . .
O9 O 0.4387(5) -0.3343(3) 0.2562(3) 0.0263(10) Uani 1 1 d . . .
O10 O 0.1870(5) -0.2230(3) 0.2323(3) 0.0264(10) Uani 1 1 d . . .
C9 C 0.2699(8) -0.3155(5) 0.3894(4) 0.0276(15) Uani 1 1 d . . .
H9A H 0.2638 -0.3953 0.4139 0.033 Uiso 1 1 calc R . .
H9B H 0.3796 -0.2927 0.4186 0.033 Uiso 1 1 calc R . .
C10 C 0.2993(7) -0.2894(4) 0.2845(4) 0.0202(14) Uani 1 1 d . . .
N3 N 0.1007(6) -0.2633(3) 0.4183(3) 0.0165(11) Uani 1 1 d . . .
H3C H 0.1334 -0.2178 0.4550 0.020 Uiso 1 1 calc R . .
C11 C -0.0395(7) -0.3391(4) 0.4674(3) 0.0168(13) Uani 1 1 d . . .
H11A H -0.1158 -0.3037 0.5080 0.020 Uiso 1 1 calc R . .
H11B H 0.0252 -0.4049 0.5077 0.020 Uiso 1 1 calc R . .
C12 C -0.1656(8) -0.3723(4) 0.3991(4) 0.0197(13) Uani 1 1 d . . .
O11 O -0.1571(5) -0.3220(3) 0.3118(2) 0.0190(9) Uani 1 1 d . . .
O12 O -0.2724(5) -0.4487(3) 0.4260(3) 0.0253(10) Uani 1 1 d . . .
O13 O -0.0076(5) -0.5398(3) 0.3098(2) 0.0156(9) Uani 1 1 d . . .
O14 O 0.1962(5) -0.6837(3) 0.3334(2) 0.0139(8) Uani 1 1 d . . .
C13 C 0.0444(7) -0.6323(4) 0.3034(3) 0.0128(12) Uani 1 1 d . . .
C14 C -0.0875(7) -0.6909(4) 0.2532(3) 0.0125(12) Uani 1 1 d . . .
O15 O -0.2467(5) -0.6472(3) 0.2333(3) 0.0191(9) Uani 1 1 d . . .
O16 O -0.0246(5) -0.7780(3) 0.2348(2) 0.0157(9) Uani 1 1 d . . .
C15 C -0.0669(7) -0.9490(4) 0.4908(3) 0.0116(11) Uani 1 1 d . . .
O17 O -0.2189(5) -0.9574(3) 0.5357(2) 0.0146(9) Uani 1 1 d . . .
O18 O -0.0170(5) -0.8668(3) 0.4307(2) 0.0164(9) Uani 1 1 d . . .
O1W O 0.4318(5) -0.8467(3) 0.4581(3) 0.0190(9) Uani 1 1 d . . .
H1WA H 0.5361 -0.8811 0.4614 0.029 Uiso 1 1 d R . .
H1WB H 0.3742 -0.8716 0.5090 0.029 Uiso 1 1 d R . .
O2W O 0.4409(5) -0.7561(3) 0.2092(3) 0.0222(10) Uani 1 1 d . . .
H2WA H 0.5440 -0.7460 0.2322 0.033 Uiso 1 1 d R . .
H2WB H 0.3847 -0.6952 0.1861 0.033 Uiso 1 1 d R . .
O3W O -0.5084(5) -0.5787(3) 0.3687(3) 0.0283(11) Uani 1 1 d . . .
H3WA H -0.6102 -0.5900 0.3451 0.042 Uiso 1 1 d R . .
H3WB H -0.5299 -0.5516 0.4147 0.042 Uiso 1 1 d R . .
O4W O -0.5726(19) -1.1132(7) 0.0245(8) 0.203(5) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O1 2.300(4) 1_655 ?
Eu1 O18 2.421(3) . ?
Eu1 O1W 2.441(4) . ?
Eu1 O2W 2.448(3) . ?
Eu1 O16 2.456(3) . ?
Eu1 O14 2.461(3) . ?
Eu1 O4 2.466(4) . ?
Eu1 O17 2.513(3) 2_536 ?
Eu1 O3 2.573(4) . ?
Eu1 C4 2.867(6) . ?
Eu1 C14 3.237(5) . ?
Eu1 C15 3.246(5) . ?
Eu2 O9 2.296(4) 1_455 ?
Eu2 O6 2.310(4) 1_455 ?
Eu2 O3W 2.393(4) . ?
Eu2 O13 2.445(3) . ?
Eu2 O15 2.471(3) . ?
Eu2 O11 2.474(4) . ?
Eu2 O8 2.509(3) . ?
Eu2 O7 2.573(3) . ?
Eu2 O12 2.604(4) . ?
Eu2 C12 2.899(6) . ?
Eu2 C8 2.910(5) . ?
Eu2 C13 3.251(5) . ?
Eu2 H3WA 2.8036 . ?
Eu2 H3WB 2.8052 . ?
Ni1 O5 2.032(3) 2_545 ?
Ni1 O5 2.032(3) . ?
Ni1 N2 2.064(4) 2_545 ?
Ni1 N2 2.064(4) . ?
Ni1 O8 2.064(4) . ?
Ni1 O8 2.064(4) 2_545 ?
Ni2 O10 2.014(4) . ?
Ni2 N1 2.040(4) 1_565 ?
Ni2 O2 2.041(4) 1_565 ?
Ni2 N3 2.045(4) . ?
Ni2 O11 2.059(4) . ?
Ni2 O4 2.072(3) 1_565 ?
O1 C2 1.248(6) . ?
O1 Eu1 2.300(4) 1_455 ?
O2 C2 1.250(6) . ?
O2 Ni2 2.041(4) 1_545 ?
C1 N1 1.460(7) . ?
C1 C2 1.500(8) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
N1 C3 1.462(6) . ?
N1 Ni2 2.040(4) 1_545 ?
N1 H1C 0.9200 . ?
C3 C4 1.482(8) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 O3 1.240(6) . ?
C4 O4 1.280(6) . ?
O4 Ni2 2.072(3) 1_545 ?
O5 C6 1.258(6) . ?
O6 C6 1.239(6) . ?
O6 Eu2 2.310(4) 1_655 ?
C5 N2 1.460(7) . ?
C5 C6 1.484(7) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
N2 C7 1.465(7) . ?
N2 H2A 0.9200 . ?
C7 C8 1.490(7) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C8 O7 1.249(6) . ?
C8 O8 1.255(6) . ?
O9 C10 1.240(6) . ?
O9 Eu2 2.296(4) 1_655 ?
O10 C10 1.238(6) . ?
C9 N3 1.455(7) . ?
C9 C10 1.503(8) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
N3 C11 1.464(6) . ?
N3 H3C 0.9200 . ?
C11 C12 1.496(8) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 O12 1.235(6) . ?
C12 O11 1.275(6) . ?
O13 C13 1.232(6) . ?
O14 C13 1.252(6) . ?
C13 C14 1.522(7) . ?
C14 O15 1.236(6) . ?
C14 O16 1.258(6) . ?
C15 O18 1.238(5) . ?
C15 O17 1.255(6) . ?
C15 C15 1.528(9) 2_536 ?
O17 Eu1 2.513(3) 2_536 ?
O1W H1WA 0.8353 . ?
O1W H1WB 0.8427 . ?
O2W H2WA 0.8365 . ?
O2W H2WB 0.8380 . ?
O3W H3WA 0.8367 . ?
O3W H3WB 0.8416 . ?

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 O18 135.46(12) 1_655 . ?
O1 Eu1 O1W 74.39(13) 1_655 . ?
O18 Eu1 O1W 83.64(12) . . ?
O1 Eu1 O2W 79.58(12) 1_655 . ?
O18 Eu1 O2W 140.57(11) . . ?
O1W Eu1 O2W 92.42(12) . . ?
O1 Eu1 O16 148.83(13) 1_655 . ?
O18 Eu1 O16 70.03(12) . . ?
O1W Eu1 O16 134.06(12) . . ?
O2W Eu1 O16 85.82(12) . . ?
O1 Eu1 O14 131.91(13) 1_655 . ?
O18 Eu1 O14 72.06(11) . . ?
O1W Eu1 O14 71.12(11) . . ?
O2W Eu1 O14 69.60(12) . . ?
O16 Eu1 O14 65.32(11) . . ?
O1 Eu1 O4 87.48(13) 1_655 . ?
O18 Eu1 O4 85.84(12) . . ?
O1W Eu1 O4 140.81(11) . . ?
O2W Eu1 O4 118.55(12) . . ?
O16 Eu1 O4 75.52(12) . . ?
O14 Eu1 O4 139.55(12) . . ?
O1 Eu1 O17 71.46(12) 1_655 2_536 ?
O18 Eu1 O17 65.11(11) . 2_536 ?
O1W Eu1 O17 72.65(12) . 2_536 ?
O2W Eu1 O17 150.00(12) . 2_536 ?
O16 Eu1 O17 123.38(11) . 2_536 ?
O14 Eu1 O17 125.85(11) . 2_536 ?
O4 Eu1 O17 68.67(12) . 2_536 ?
O1 Eu1 O3 82.02(12) 1_655 . ?
O18 Eu1 O3 124.87(12) . . ?
O1W Eu1 O3 151.42(12) . . ?
O2W Eu1 O3 67.25(12) . . ?
O16 Eu1 O3 66.91(11) . . ?
O14 Eu1 O3 116.25(11) . . ?
O4 Eu1 O3 51.46(11) . . ?
O17 Eu1 O3 114.95(11) 2_536 . ?
O1 Eu1 C4 88.14(14) 1_655 . ?
O18 Eu1 C4 103.81(14) . . ?
O1W Eu1 C4 160.53(12) . . ?
O2W Eu1 C4 92.80(13) . . ?
O16 Eu1 C4 65.08(13) . . ?
O14 Eu1 C4 128.18(12) . . ?
O4 Eu1 C4 26.43(12) . . ?
O17 Eu1 C4 93.92(12) 2_536 . ?
O3 Eu1 C4 25.62(12) . . ?
O1 Eu1 C14 163.00(12) 1_655 . ?
O18 Eu1 C14 61.49(11) . . ?
O1W Eu1 C14 113.93(12) . . ?
O2W Eu1 C14 85.13(12) . . ?
O16 Eu1 C14 20.14(12) . . ?
O14 Eu1 C14 46.37(12) . . ?
O4 Eu1 C14 93.39(12) . . ?
O17 Eu1 C14 124.56(11) 2_536 . ?
O3 Eu1 C14 85.26(12) . . ?
C4 Eu1 C14 85.21(13) . . ?
O1 Eu1 C15 118.03(12) 1_655 . ?
O18 Eu1 C15 18.94(11) . . ?
O1W Eu1 C15 82.78(12) . . ?
O2W Eu1 C15 159.22(12) . . ?
O16 Eu1 C15 83.18(12) . . ?
O14 Eu1 C15 89.77(11) . . ?
O4 Eu1 C15 75.51(12) . . ?
O17 Eu1 C15 46.72(11) 2_536 . ?
O3 Eu1 C15 123.24(12) . . ?
C4 Eu1 C15 98.42(13) . . ?
C14 Eu1 C15 78.49(12) . . ?
O9 Eu2 O6 79.45(14) 1_455 1_455 ?
O9 Eu2 O3W 82.75(13) 1_455 . ?
O6 Eu2 O3W 80.87(14) 1_455 . ?
O9 Eu2 O13 148.36(14) 1_455 . ?
O6 Eu2 O13 132.15(13) 1_455 . ?
O3W Eu2 O13 98.98(12) . . ?
O9 Eu2 O15 143.68(13) 1_455 . ?
O6 Eu2 O15 68.85(12) 1_455 . ?
O3W Eu2 O15 75.32(13) . . ?
O13 Eu2 O15 65.04(12) . . ?
O9 Eu2 O11 78.09(13) 1_455 . ?
O6 Eu2 O11 150.84(12) 1_455 . ?
O3W Eu2 O11 114.21(13) . . ?
O13 Eu2 O11 72.40(12) . . ?
O15 Eu2 O11 137.41(12) . . ?
O9 Eu2 O8 119.69(12) 1_455 . ?
O6 Eu2 O8 78.82(13) 1_455 . ?
O3W Eu2 O8 145.82(13) . . ?
O13 Eu2 O8 75.51(12) . . ?
O15 Eu2 O8 71.82(11) . . ?
O11 Eu2 O8 96.51(12) . . ?
O9 Eu2 O7 73.24(12) 1_455 . ?
O6 Eu2 O7 87.99(13) 1_455 . ?
O3W Eu2 O7 155.04(13) . . ?
O13 Eu2 O7 105.01(12) . . ?
O15 Eu2 O7 121.21(12) . . ?
O11 Eu2 O7 67.86(12) . . ?
O8 Eu2 O7 50.49(11) . . ?
O9 Eu2 O12 82.02(13) 1_455 . ?
O6 Eu2 O12 142.56(13) 1_455 . ?
O3W Eu2 O12 64.66(13) . . ?
O13 Eu2 O12 70.64(12) . . ?
O15 Eu2 O12 112.85(12) . . ?
O11 Eu2 O12 50.72(11) . . ?
O8 Eu2 O12 138.43(12) . . ?
O7 Eu2 O12 117.19(12) . . ?
O9 Eu2 C12 82.39(15) 1_455 . ?
O6 Eu2 C12 160.46(15) 1_455 . ?
O3W Eu2 C12 89.78(14) . . ?
O13 Eu2 C12 66.07(14) . . ?
O15 Eu2 C12 125.38(13) . . ?
O11 Eu2 C12 25.93(12) . . ?
O8 Eu2 C12 116.91(14) . . ?
O7 Eu2 C12 93.65(13) . . ?
O12 Eu2 C12 25.21(12) . . ?
O9 Eu2 C8 97.63(14) 1_455 . ?
O6 Eu2 C8 85.51(14) 1_455 . ?
O3W Eu2 C8 166.09(14) . . ?
O13 Eu2 C8 88.02(13) . . ?
O15 Eu2 C8 97.12(13) . . ?
O11 Eu2 C8 79.31(13) . . ?
O8 Eu2 C8 25.41(12) . . ?
O7 Eu2 C8 25.38(13) . . ?
O12 Eu2 C8 129.23(13) . . ?
C12 Eu2 C8 104.08(15) . . ?
O9 Eu2 C13 164.93(14) 1_455 . ?
O6 Eu2 C13 113.73(13) 1_455 . ?
O3W Eu2 C13 91.93(12) . . ?
O13 Eu2 C13 19.04(12) . . ?
O15 Eu2 C13 46.01(12) . . ?
O11 Eu2 C13 91.43(12) . . ?
O8 Eu2 C13 71.84(11) . . ?
O7 Eu2 C13 113.02(12) . . ?
O12 Eu2 C13 82.96(12) . . ?
C12 Eu2 C13 83.50(14) . . ?
C8 Eu2 C13 90.92(13) . . ?
O9 Eu2 H3WA 76.5 1_455 . ?
O6 Eu2 H3WA 65.2 1_455 . ?
O3W Eu2 H3WA 16.2 . . ?
O13 Eu2 H3WA 112.2 . . ?
O15 Eu2 H3WA 74.5 . . ?
O11 Eu2 H3WA 125.9 . . ?
O8 Eu2 H3WA 137.5 . . ?
O7 Eu2 H3WA 142.7 . . ?
O12 Eu2 H3WA 78.9 . . ?
C12 Eu2 H3WA 103.5 . . ?
C8 Eu2 H3WA 150.7 . . ?
C13 Eu2 H3WA 101.8 . . ?
O9 Eu2 H3WB 74.0 1_455 . ?
O6 Eu2 H3WB 92.8 1_455 . ?
O3W Eu2 H3WB 16.3 . . ?
O13 Eu2 H3WB 99.1 . . ?
O15 Eu2 H3WB 89.9 . . ?
O11 Eu2 H3WB 98.6 . . ?
O8 Eu2 H3WB 161.6 . . ?
O7 Eu2 H3WB 146.5 . . ?
O12 Eu2 H3WB 50.6 . . ?
C12 Eu2 H3WB 75.2 . . ?
C8 Eu2 H3WB 171.7 . . ?
C13 Eu2 H3WB 97.2 . . ?
H3WA Eu2 H3WB 28.4 . . ?
O5 Ni1 O5 180.0 2_545 . ?
O5 Ni1 N2 84.11(15) 2_545 2_545 ?
O5 Ni1 N2 95.89(15) . 2_545 ?
O5 Ni1 N2 95.89(15) 2_545 . ?
O5 Ni1 N2 84.11(15) . . ?
N2 Ni1 N2 180.0 2_545 . ?
O5 Ni1 O8 90.51(15) 2_545 . ?
O5 Ni1 O8 89.49(14) . . ?
N2 Ni1 O8 99.51(15) 2_545 . ?
N2 Ni1 O8 80.49(15) . . ?
O5 Ni1 O8 89.49(14) 2_545 2_545 ?
O5 Ni1 O8 90.51(14) . 2_545 ?
N2 Ni1 O8 80.49(15) 2_545 2_545 ?
N2 Ni1 O8 99.51(15) . 2_545 ?
O8 Ni1 O8 180.0 . 2_545 ?
O10 Ni2 N1 95.21(16) . 1_565 ?
O10 Ni2 O2 178.04(15) . 1_565 ?
N1 Ni2 O2 83.78(16) 1_565 1_565 ?
O10 Ni2 N3 83.82(16) . . ?
N1 Ni2 N3 178.82(18) 1_565 . ?
O2 Ni2 N3 97.20(16) 1_565 . ?
O10 Ni2 O11 90.53(15) . . ?
N1 Ni2 O11 98.56(16) 1_565 . ?
O2 Ni2 O11 91.28(15) 1_565 . ?
N3 Ni2 O11 80.79(16) . . ?
O10 Ni2 O4 90.17(15) . 1_565 ?
N1 Ni2 O4 79.13(16) 1_565 1_565 ?
O2 Ni2 O4 87.99(15) 1_565 1_565 ?
N3 Ni2 O4 101.53(16) . 1_565 ?
O11 Ni2 O4 177.64(14) . 1_565 ?
C2 O1 Eu1 157.3(4) . 1_455 ?
C2 O2 Ni2 112.6(3) . 1_545 ?
N1 C1 C2 113.5(4) . . ?
N1 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
O1 C2 O2 122.8(5) . . ?
O1 C2 C1 117.1(5) . . ?
O2 C2 C1 120.1(5) . . ?
C1 N1 C3 113.7(4) . . ?
C1 N1 Ni2 108.8(3) . 1_545 ?
C3 N1 Ni2 103.4(3) . 1_545 ?
C1 N1 H1C 110.2 . . ?
C3 N1 H1C 110.2 . . ?
Ni2 N1 H1C 110.2 1_545 . ?
N1 C3 C4 111.1(4) . . ?
N1 C3 H3A 109.4 . . ?
C4 C3 H3A 109.4 . . ?
N1 C3 H3B 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
O3 C4 O4 120.7(5) . . ?
O3 C4 C3 121.5(5) . . ?
O4 C4 C3 117.8(4) . . ?
O3 C4 Eu1 63.8(3) . . ?
O4 C4 Eu1 59.0(3) . . ?
C3 C4 Eu1 163.7(4) . . ?
C4 O3 Eu1 90.6(3) . . ?
C4 O4 Ni2 107.1(3) . 1_545 ?
C4 O4 Eu1 94.5(3) . . ?
Ni2 O4 Eu1 156.73(17) 1_545 . ?
C6 O5 Ni1 113.4(3) . . ?
C6 O6 Eu2 153.8(3) . 1_655 ?
N2 C5 C6 115.6(4) . . ?
N2 C5 H5A 108.4 . . ?
C6 C5 H5A 108.4 . . ?
N2 C5 H5B 108.4 . . ?
C6 C5 H5B 108.4 . . ?
H5A C5 H5B 107.5 . . ?
O6 C6 O5 122.3(4) . . ?
O6 C6 C5 118.3(5) . . ?
O5 C6 C5 119.4(5) . . ?
C5 N2 C7 114.3(4) . . ?
C5 N2 Ni1 107.2(3) . . ?
C7 N2 Ni1 104.8(3) . . ?
C5 N2 H2A 110.1 . . ?
C7 N2 H2A 110.1 . . ?
Ni1 N2 H2A 110.1 . . ?
N2 C7 C8 111.0(4) . . ?
N2 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
N2 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
O7 C8 O8 120.1(4) . . ?
O7 C8 C7 119.7(4) . . ?
O8 C8 C7 120.2(5) . . ?
O7 C8 Eu2 62.0(2) . . ?
O8 C8 Eu2 59.1(3) . . ?
C7 C8 Eu2 167.9(4) . . ?
C8 O7 Eu2 92.6(3) . . ?
C8 O8 Ni1 109.1(3) . . ?
C8 O8 Eu2 95.5(3) . . ?
Ni1 O8 Eu2 154.46(16) . . ?
C10 O9 Eu2 160.1(4) . 1_655 ?
C10 O10 Ni2 114.9(4) . . ?
N3 C9 C10 114.7(4) . . ?
N3 C9 H9A 108.6 . . ?
C10 C9 H9A 108.6 . . ?
N3 C9 H9B 108.6 . . ?
C10 C9 H9B 108.6 . . ?
H9A C9 H9B 107.6 . . ?
O10 C10 O9 124.4(5) . . ?
O10 C10 C9 118.4(5) . . ?
O9 C10 C9 117.1(5) . . ?
C9 N3 C11 115.1(4) . . ?
C9 N3 Ni2 107.9(3) . . ?
C11 N3 Ni2 104.2(3) . . ?
C9 N3 H3C 109.8 . . ?
C11 N3 H3C 109.8 . . ?
Ni2 N3 H3C 109.8 . . ?
N3 C11 C12 111.4(4) . . ?
N3 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
N3 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
O12 C12 O11 120.4(5) . . ?
O12 C12 C11 120.9(5) . . ?
O11 C12 C11 118.6(5) . . ?
O12 C12 Eu2 63.9(3) . . ?
O11 C12 Eu2 58.1(3) . . ?
C11 C12 Eu2 165.2(4) . . ?
C12 O11 Ni2 109.1(3) . . ?
C12 O11 Eu2 96.0(3) . . ?
Ni2 O11 Eu2 154.74(17) . . ?
C12 O12 Eu2 90.9(3) . . ?
C13 O13 Eu2 120.6(3) . . ?
C13 O14 Eu1 119.8(3) . . ?
O13 C13 O14 126.9(5) . . ?
O13 C13 C14 117.4(4) . . ?
O14 C13 C14 115.8(4) . . ?
O13 C13 Eu2 40.3(2) . . ?
O14 C13 Eu2 166.9(4) . . ?
C14 C13 Eu2 77.1(3) . . ?
O13 C13 Eu1 166.6(4) . . ?
O14 C13 Eu1 40.8(2) . . ?
C14 C13 Eu1 75.3(3) . . ?
Eu2 C13 Eu1 151.47(17) . . ?
O15 C14 O16 126.2(5) . . ?
O15 C14 C13 116.3(4) . . ?
O16 C14 C13 117.5(4) . . ?
O15 C14 Eu1 161.0(3) . . ?
O16 C14 Eu1 42.2(2) . . ?
C13 C14 Eu1 77.6(3) . . ?
O15 C14 Eu2 40.9(2) . . ?
O16 C14 Eu2 165.1(4) . . ?
C13 C14 Eu2 75.9(3) . . ?
Eu1 C14 Eu2 152.51(18) . . ?
C14 O15 Eu2 119.9(3) . . ?
C14 O16 Eu1 117.6(3) . . ?
O18 C15 O17 126.2(4) . . ?
O18 C15 C15 116.6(5) . 2_536 ?
O17 C15 C15 117.2(5) . 2_536 ?
O18 C15 Eu1 39.4(2) . . ?
O17 C15 Eu1 162.7(3) . . ?
C15 C15 Eu1 77.8(4) 2_536 . ?
C15 O17 Eu1 117.1(3) . 2_536 ?
C15 O18 Eu1 121.6(3) . . ?
Eu1 O1W H1WA 109.7 . . ?
Eu1 O1W H1WB 108.9 . . ?
H1WA O1W H1WB 108.0 . . ?
Eu1 O2W H2WA 111.3 . . ?
Eu1 O2W H2WB 111.3 . . ?
H2WA O2W H2WB 109.1 . . ?
Eu2 O3W H3WA 111.0 . . ?
Eu2 O3W H3WB 110.8 . . ?
H3WA O3W H3WB 109.9 . . ?

_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.960
_refine_diff_density_max         1.917
_refine_diff_density_min         -1.220
_refine_diff_density_rms         0.214

# Attachment 'complex4.cif'

data_complex4
_database_code_depnum_ccdc_archive 'CCDC 647833'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H23 Gd2 N3 Ni1.50 O22'
_chemical_formula_weight         999.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   7.0723(14)
_cell_length_b                   12.517(3)
_cell_length_c                   14.536(3)
_cell_angle_alpha                74.901(4)
_cell_angle_beta                 89.669(4)
_cell_angle_gamma                87.133(4)
_cell_volume                     1240.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    4587
_cell_measurement_theta_min      2.496
_cell_measurement_theta_max      28.441

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             960
_exptl_absorpt_coefficient_mu    6.515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3557
_exptl_absorpt_correction_T_max  0.7806
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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_%        ?
_diffrn_reflns_number            6727
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.45
_diffrn_reflns_theta_max         25.99
_reflns_number_total             4716
_reflns_number_gt                4519
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_cell_refinement       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0556P)²+12.8032P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4716
_refine_ls_number_parameters     394
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.1087
_refine_ls_wR_factor_gt          0.1067
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.010
_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 Gd 0.24779(3) -0.876755(17) 0.327533(15) 0.00710(5) Uani 1 1 d . . .
EU2 Gd -0.31896(3) -0.462759(18) 0.253224(16) 0.00909(6) Uani 1 1 d . . .
Ni1 Ni 0.0000 -0.5000 0.0000 0.01018(19) Uani 1 2 d S . .
Ni2 Ni -0.03523(9) -0.17384(5) 0.29888(4) 0.01422(15) Uani 1 1 d . . .
O1 O -0.4828(5) -0.9891(3) 0.3362(3) 0.0178(9) Uani 1 1 d . . .
O2 O -0.2584(6) -1.1174(3) 0.3634(3) 0.0203(9) Uani 1 1 d . . .
C1 C -0.3319(8) -1.0242(5) 0.2029(4) 0.0265(15) Uani 1 1 d . . .
H1A H -0.4472 -1.0445 0.1745 0.032 Uiso 1 1 calc R . .
H1B H -0.3169 -0.9440 0.1753 0.032 Uiso 1 1 calc R . .
C2 C -0.3584(7) -1.0452(4) 0.3084(4) 0.0151(12) Uani 1 1 d . . .
N1 N -0.1682(7) -1.0859(4) 0.1770(3) 0.0174(10) Uani 1 1 d . . .
H1C H -0.2075 -1.1336 0.1423 0.021 Uiso 1 1 calc R . .
C3 C -0.0216(8) -1.0165(4) 0.1248(4) 0.0161(12) Uani 1 1 d . . .
H3A H -0.0817 -0.9503 0.0799 0.019 Uiso 1 1 calc R . .
H3B H 0.0545 -1.0586 0.0874 0.019 Uiso 1 1 calc R . .
C4 C 0.1040(7) -0.9814(4) 0.1921(4) 0.0134(11) Uani 1 1 d . . .
O3 O 0.2251(5) -0.9141(3) 0.1639(3) 0.0177(9) Uani 1 1 d . . .
O4 O 0.0777(5) -1.0198(3) 0.2810(2) 0.0147(8) Uani 1 1 d . . .
O5 O 0.2222(5) -0.5612(3) 0.0883(2) 0.0141(8) Uani 1 1 d . . .
O6 O 0.4669(5) -0.5077(3) 0.1536(3) 0.0166(8) Uani 1 1 d . . .
C5 C 0.2990(8) -0.3710(4) 0.0373(4) 0.0190(13) Uani 1 1 d . . .
H5A H 0.2937 -0.3204 0.0796 0.023 Uiso 1 1 calc R . .
H5B H 0.4091 -0.3522 -0.0052 0.023 Uiso 1 1 calc R . .
C6 C 0.3298(7) -0.4882(4) 0.0976(3) 0.0098(10) Uani 1 1 d . . .
N2 N 0.1283(6) -0.3517(3) -0.0204(3) 0.0101(9) Uani 1 1 d . . .
H2A H 0.1588 -0.3249 -0.0843 0.012 Uiso 1 1 calc R . .
C7 C -0.0164(8) -0.2771(4) 0.0065(4) 0.0187(13) Uani 1 1 d . . .
H7A H -0.0929 -0.2385 -0.0503 0.022 Uiso 1 1 calc R . .
H7B H 0.0461 -0.2205 0.0304 0.022 Uiso 1 1 calc R . .
C8 C -0.1419(8) -0.3394(4) 0.0810(4) 0.0166(12) Uani 1 1 d . . .
O7 O -0.2599(5) -0.2870(3) 0.1191(3) 0.0202(9) Uani 1 1 d . . .
O8 O -0.1281(5) -0.4430(3) 0.1065(2) 0.0121(8) Uani 1 1 d . . .
O9 O 0.4398(5) -0.3354(3) 0.2563(3) 0.0214(9) Uani 1 1 d . . .
O10 O 0.1858(5) -0.2242(3) 0.2312(3) 0.0206(9) Uani 1 1 d . . .
C9 C 0.2704(8) -0.3175(5) 0.3909(4) 0.0236(14) Uani 1 1 d . . .
H9A H 0.2649 -0.3989 0.4155 0.028 Uiso 1 1 calc R . .
H9B H 0.3813 -0.2945 0.4209 0.028 Uiso 1 1 calc R . .
C10 C 0.2999(7) -0.2905(4) 0.2858(4) 0.0171(12) Uani 1 1 d . . .
N3 N 0.0995(6) -0.2652(4) 0.4199(3) 0.0169(10) Uani 1 1 d . . .
H3C H 0.1318 -0.2190 0.4576 0.020 Uiso 1 1 calc R . .
C11 C -0.0393(8) -0.3410(4) 0.4686(4) 0.0183(13) Uani 1 1 d . . .
H11A H -0.1177 -0.3051 0.5098 0.022 Uiso 1 1 calc R . .
H11B H 0.0267 -0.4078 0.5098 0.022 Uiso 1 1 calc R . .
C12 C -0.1653(8) -0.3748(5) 0.3990(4) 0.0198(13) Uani 1 1 d . . .
O11 O -0.1551(5) -0.3234(3) 0.3123(3) 0.0172(9) Uani 1 1 d . . .
O12 O -0.2715(6) -0.4504(3) 0.4250(3) 0.0238(10) Uani 1 1 d . . .
O13 O -0.0074(5) -0.5394(3) 0.3089(2) 0.0126(8) Uani 1 1 d . . .
O14 O 0.1975(5) -0.6845(3) 0.3340(2) 0.0105(8) Uani 1 1 d . . .
C13 C 0.0465(7) -0.6327(4) 0.3036(3) 0.0077(6) Uani 1 1 d U . .
C14 C -0.0846(7) -0.6927(4) 0.2531(3) 0.0088(11) Uani 1 1 d . . .
O15 O -0.2441(5) -0.6480(3) 0.2324(3) 0.0163(9) Uani 1 1 d . . .
O16 O -0.0204(5) -0.7779(3) 0.2340(2) 0.0110(8) Uani 1 1 d . . .
C15 C -0.0692(7) -0.9484(3) 0.4894(3) 0.0072(10) Uani 1 1 d . . .
O17 O -0.2188(5) -0.9570(3) 0.5347(2) 0.0109(8) Uani 1 1 d . . .
O18 O -0.0168(5) -0.8665(3) 0.4298(2) 0.0124(8) Uani 1 1 d . . .
O1W O 0.4313(5) -0.8468(3) 0.4578(2) 0.0137(8) Uani 1 1 d . . .
H1WA H 0.5356 -0.8812 0.4611 0.021 Uiso 1 1 d R . .
H1WB H 0.3737 -0.8717 0.5087 0.021 Uiso 1 1 d R . .
O2W O 0.4419(5) -0.7582(3) 0.2109(2) 0.0121(8) Uani 1 1 d . . .
H2WA H 0.5450 -0.7480 0.2340 0.018 Uiso 1 1 d R . .
H2WB H 0.3857 -0.6972 0.1878 0.018 Uiso 1 1 d R . .
O3W O -0.5047(6) -0.5811(3) 0.3676(3) 0.0237(10) Uani 1 1 d . . .
H3WA H -0.6065 -0.5924 0.3440 0.035 Uiso 1 1 d R . .
H3WB H -0.5263 -0.5540 0.4137 0.035 Uiso 1 1 d R . .
O4W O 1.442(2) -1.1117(7) 0.0206(8) 0.184(5) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
EU1 O1 2.295(4) 1_655 ?
EU1 O18 2.402(3) . ?
EU1 O2W 2.414(3) . ?
EU1 O1W 2.420(4) . ?
EU1 O16 2.428(3) . ?
EU1 O14 2.441(3) . ?
EU1 O4 2.443(4) . ?
EU1 O17 2.500(3) 2_536 ?
EU1 O3 2.548(4) . ?
EU1 C4 2.851(5) . ?
EU2 O9 2.284(4) 1_455 ?
EU2 O6 2.289(4) 1_455 ?
EU2 O3W 2.360(4) . ?
EU2 O13 2.415(3) . ?
EU2 O15 2.447(4) . ?
EU2 O11 2.473(4) . ?
EU2 O8 2.482(3) . ?
EU2 O12 2.566(4) . ?
EU2 O7 2.581(4) . ?
EU2 C12 2.872(6) . ?
EU2 C8 2.891(5) . ?
Ni1 O5 2.024(3) 2_545 ?
Ni1 O5 2.024(3) . ?
Ni1 O8 2.054(3) 2_545 ?
Ni1 O8 2.054(3) . ?
Ni1 N2 2.058(4) . ?
Ni1 N2 2.058(4) 2_545 ?
Ni2 O10 2.004(4) . ?
Ni2 O2 2.021(4) 1_565 ?
Ni2 N1 2.034(4) 1_565 ?
Ni2 N3 2.043(4) . ?
Ni2 O11 2.056(4) . ?
Ni2 O4 2.076(4) 1_565 ?
O1 C2 1.229(7) . ?
O1 EU1 2.295(4) 1_455 ?
O2 C2 1.234(6) . ?
O2 Ni2 2.021(4) 1_545 ?
C1 N1 1.461(7) . ?
C1 C2 1.500(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
N1 C3 1.463(7) . ?
N1 Ni2 2.034(4) 1_545 ?
N1 H1C 0.9300 . ?
C3 C4 1.487(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O3 1.224(6) . ?
C4 O4 1.272(6) . ?
O4 Ni2 2.076(4) 1_545 ?
O5 C6 1.251(6) . ?
O6 C6 1.243(6) . ?
O6 EU2 2.289(4) 1_655 ?
C5 N2 1.447(7) . ?
C5 C6 1.507(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
N2 C7 1.471(7) . ?
N2 H2A 0.9300 . ?
C7 C8 1.479(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 O7 1.249(7) . ?
C8 O8 1.251(6) . ?
O9 C10 1.242(7) . ?
O9 EU2 2.284(4) 1_655 ?
O10 C10 1.252(6) . ?
C9 N3 1.459(7) . ?
C9 C10 1.492(8) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
N3 C11 1.449(7) . ?
N3 H3C 0.9300 . ?
C11 C12 1.505(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 O12 1.218(7) . ?
C12 O11 1.260(6) . ?
O13 C13 1.232(6) . ?
O14 C13 1.242(6) . ?
C13 C14 1.525(7) . ?
C14 O16 1.235(6) . ?
C14 O15 1.237(6) . ?
C15 O18 1.229(5) . ?
C15 O17 1.238(6) . ?
C15 C15 1.546(9) 2_536 ?
O17 EU1 2.500(3) 2_536 ?
O1W H1WA 0.8301 . ?
O1W H1WB 0.8368 . ?
O2W H2WA 0.8335 . ?
O2W H2WB 0.8310 . ?
O3W H3WA 0.8337 . ?
O3W H3WB 0.8352 . ?

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 O18 135.63(12) 1_655 . ?
O1 EU1 O2W 79.46(12) 1_655 . ?
O18 EU1 O2W 140.59(11) . . ?
O1 EU1 O1W 74.64(13) 1_655 . ?
O18 EU1 O1W 84.03(12) . . ?
O2W EU1 O1W 91.78(12) . . ?
O1 EU1 O16 148.54(12) 1_655 . ?
O18 EU1 O16 70.02(11) . . ?
O2W EU1 O16 85.93(11) . . ?
O1W EU1 O16 133.99(12) . . ?
O1 EU1 O14 132.02(13) 1_655 . ?
O18 EU1 O14 71.93(11) . . ?
O2W EU1 O14 69.75(11) . . ?
O1W EU1 O14 70.62(11) . . ?
O16 EU1 O14 65.53(11) . . ?
O1 EU1 O4 87.60(13) 1_655 . ?
O18 EU1 O4 85.53(12) . . ?
O2W EU1 O4 118.78(12) . . ?
O1W EU1 O4 141.37(11) . . ?
O16 EU1 O4 75.22(11) . . ?
O14 EU1 O4 139.37(11) . . ?
O1 EU1 O17 71.46(12) 1_655 2_536 ?
O18 EU1 O17 65.15(11) . 2_536 ?
O2W EU1 O17 149.72(11) . 2_536 ?
O1W EU1 O17 72.81(11) . 2_536 ?
O16 EU1 O17 123.62(11) . 2_536 ?
O14 EU1 O17 125.39(11) . 2_536 ?
O4 EU1 O17 69.05(11) . 2_536 ?
O1 EU1 O3 81.67(12) 1_655 . ?
O18 EU1 O3 124.73(12) . . ?
O2W EU1 O3 67.60(12) . . ?
O1W EU1 O3 151.18(12) . . ?
O16 EU1 O3 66.98(12) . . ?
O14 EU1 O3 116.76(11) . . ?
O4 EU1 O3 51.32(12) . . ?
O17 EU1 O3 114.96(12) 2_536 . ?
O1 EU1 C4 87.74(14) 1_655 . ?
O18 EU1 C4 103.82(13) . . ?
O2W EU1 C4 92.97(13) . . ?
O1W EU1 C4 160.58(13) . . ?
O16 EU1 C4 65.20(13) . . ?
O14 EU1 C4 128.57(12) . . ?
O4 EU1 C4 26.40(12) . . ?
O17 EU1 C4 94.12(13) 2_536 . ?
O3 EU1 C4 25.43(13) . . ?
O9 EU2 O6 79.47(14) 1_455 1_455 ?
O9 EU2 O3W 83.26(14) 1_455 . ?
O6 EU2 O3W 80.69(13) 1_455 . ?
O9 EU2 O13 147.95(13) 1_455 . ?
O6 EU2 O13 132.57(13) 1_455 . ?
O3W EU2 O13 99.51(13) . . ?
O9 EU2 O15 143.99(13) 1_455 . ?
O6 EU2 O15 68.88(12) 1_455 . ?
O3W EU2 O15 75.27(14) . . ?
O13 EU2 O15 65.52(12) . . ?
O9 EU2 O11 78.22(13) 1_455 . ?
O6 EU2 O11 150.85(12) 1_455 . ?
O3W EU2 O11 114.80(13) . . ?
O13 EU2 O11 71.64(12) . . ?
O15 EU2 O11 137.11(12) . . ?
O9 EU2 O8 119.36(12) 1_455 . ?
O6 EU2 O8 79.08(12) 1_455 . ?
O3W EU2 O8 145.79(13) . . ?
O13 EU2 O8 75.13(11) . . ?
O15 EU2 O8 71.81(12) . . ?
O11 EU2 O8 95.85(12) . . ?
O9 EU2 O12 82.03(14) 1_455 . ?
O6 EU2 O12 142.81(13) 1_455 . ?
O3W EU2 O12 65.26(13) . . ?
O13 EU2 O12 70.65(12) . . ?
O15 EU2 O12 113.30(12) . . ?
O11 EU2 O12 50.60(12) . . ?
O8 EU2 O12 137.96(12) . . ?
O9 EU2 O7 72.35(13) 1_455 . ?
O6 EU2 O7 87.62(12) 1_455 . ?
O3W EU2 O7 154.54(13) . . ?
O13 EU2 O7 105.02(11) . . ?
O15 EU2 O7 121.31(12) . . ?
O11 EU2 O7 67.87(12) . . ?
O8 EU2 O7 50.76(11) . . ?
O12 EU2 O7 116.87(12) . . ?
O9 EU2 C12 82.45(15) 1_455 . ?
O6 EU2 C12 160.59(15) 1_455 . ?
O3W EU2 C12 90.28(15) . . ?
O13 EU2 C12 65.69(14) . . ?
O15 EU2 C12 125.48(14) . . ?
O11 EU2 C12 25.92(13) . . ?
O8 EU2 C12 116.38(14) . . ?
O12 EU2 C12 25.09(14) . . ?
O7 EU2 C12 93.60(14) . . ?
O9 EU2 C8 97.09(14) 1_455 . ?
O6 EU2 C8 85.64(14) 1_455 . ?
O3W EU2 C8 166.03(15) . . ?
O13 EU2 C8 87.63(13) . . ?
O15 EU2 C8 97.18(14) . . ?
O11 EU2 C8 78.78(14) . . ?
O8 EU2 C8 25.50(13) . . ?
O12 EU2 C8 128.68(14) . . ?
O7 EU2 C8 25.60(14) . . ?
C12 EU2 C8 103.63(15) . . ?
O5 Ni1 O5 180.0(2) 2_545 . ?
O5 Ni1 O8 89.40(14) 2_545 2_545 ?
O5 Ni1 O8 90.60(14) . 2_545 ?
O5 Ni1 O8 90.60(14) 2_545 . ?
O5 Ni1 O8 89.40(14) . . ?
O8 Ni1 O8 180.0 2_545 . ?
O5 Ni1 N2 95.80(14) 2_545 . ?
O5 Ni1 N2 84.20(14) . . ?
O8 Ni1 N2 99.46(15) 2_545 . ?
O8 Ni1 N2 80.54(15) . . ?
O5 Ni1 N2 84.20(14) 2_545 2_545 ?
O5 Ni1 N2 95.80(14) . 2_545 ?
O8 Ni1 N2 80.54(15) 2_545 2_545 ?
O8 Ni1 N2 99.46(15) . 2_545 ?
N2 Ni1 N2 180.000(1) . 2_545 ?
O10 Ni2 O2 177.83(15) . 1_565 ?
O10 Ni2 N1 94.34(17) . 1_565 ?
O2 Ni2 N1 83.95(17) 1_565 1_565 ?
O10 Ni2 N3 84.75(17) . . ?
O2 Ni2 N3 96.99(17) 1_565 . ?
N1 Ni2 N3 178.68(19) 1_565 . ?
O10 Ni2 O11 90.04(16) . . ?
O2 Ni2 O11 91.53(16) 1_565 . ?
N1 Ni2 O11 98.82(17) 1_565 . ?
N3 Ni2 O11 80.24(16) . . ?
O10 Ni2 O4 90.59(16) . 1_565 ?
O2 Ni2 O4 87.78(15) 1_565 1_565 ?
N1 Ni2 O4 78.89(16) 1_565 1_565 ?
N3 Ni2 O4 102.05(16) . 1_565 ?
O11 Ni2 O4 177.66(14) . 1_565 ?
C2 O1 EU1 157.4(4) . 1_455 ?
C2 O2 Ni2 113.3(3) . 1_545 ?
N1 C1 C2 113.5(5) . . ?
N1 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
O1 C2 O2 122.8(5) . . ?
O1 C2 C1 117.4(5) . . ?
O2 C2 C1 119.8(5) . . ?
C1 N1 C3 114.5(4) . . ?
C1 N1 Ni2 108.3(3) . 1_545 ?
C3 N1 Ni2 103.9(3) . 1_545 ?
C1 N1 H1C 110.0 . . ?
C3 N1 H1C 110.0 . . ?
Ni2 N1 H1C 110.0 1_545 . ?
N1 C3 C4 110.4(4) . . ?
N1 C3 H3A 109.6 . . ?
C4 C3 H3A 109.6 . . ?
N1 C3 H3B 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
O3 C4 O4 120.1(5) . . ?
O3 C4 C3 121.7(5) . . ?
O4 C4 C3 118.2(4) . . ?
O3 C4 EU1 63.3(3) . . ?
O4 C4 EU1 58.6(3) . . ?
C3 C4 EU1 163.3(4) . . ?
C4 O3 EU1 91.2(3) . . ?
C4 O4 Ni2 106.7(3) . 1_545 ?
C4 O4 EU1 95.0(3) . . ?
Ni2 O4 EU1 156.30(17) 1_545 . ?
C6 O5 Ni1 113.2(3) . . ?
C6 O6 EU2 154.2(3) . 1_655 ?
N2 C5 C6 114.1(4) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
O6 C6 O5 123.1(4) . . ?
O6 C6 C5 116.9(4) . . ?
O5 C6 C5 119.9(4) . . ?
C5 N2 C7 114.7(4) . . ?
C5 N2 Ni1 108.2(3) . . ?
C7 N2 Ni1 104.5(3) . . ?
C5 N2 H2A 109.8 . . ?
C7 N2 H2A 109.8 . . ?
Ni1 N2 H2A 109.8 . . ?
N2 C7 C8 111.0(4) . . ?
N2 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
N2 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
O7 C8 O8 120.6(5) . . ?
O7 C8 C7 119.0(5) . . ?
O8 C8 C7 120.4(5) . . ?
O7 C8 EU2 63.2(3) . . ?
O8 C8 EU2 58.6(3) . . ?
C7 C8 EU2 167.8(4) . . ?
C8 O7 EU2 91.2(3) . . ?
C8 O8 Ni1 108.9(3) . . ?
C8 O8 EU2 95.9(3) . . ?
Ni1 O8 EU2 154.08(17) . . ?
C10 O9 EU2 159.4(4) . 1_655 ?
C10 O10 Ni2 113.5(4) . . ?
N3 C9 C10 114.5(4) . . ?
N3 C9 H9A 108.6 . . ?
C10 C9 H9A 108.6 . . ?
N3 C9 H9B 108.6 . . ?
C10 C9 H9B 108.6 . . ?
H9A C9 H9B 107.6 . . ?
O9 C10 O10 122.7(5) . . ?
O9 C10 C9 117.6(5) . . ?
O10 C10 C9 119.7(5) . . ?
C11 N3 C9 115.1(4) . . ?
C11 N3 Ni2 104.7(3) . . ?
C9 N3 Ni2 107.5(3) . . ?
C11 N3 H3C 109.8 . . ?
C9 N3 H3C 109.8 . . ?
Ni2 N3 H3C 109.8 . . ?
N3 C11 C12 111.5(4) . . ?
N3 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
N3 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
O12 C12 O11 120.8(6) . . ?
O12 C12 C11 121.4(5) . . ?
O11 C12 C11 117.8(5) . . ?
O12 C12 EU2 63.3(3) . . ?
O11 C12 EU2 59.1(3) . . ?
C11 C12 EU2 165.7(4) . . ?
C12 O11 Ni2 110.1(4) . . ?
C12 O11 EU2 95.0(3) . . ?
Ni2 O11 EU2 154.64(18) . . ?
C12 O12 EU2 91.6(3) . . ?
C13 O13 EU2 120.8(3) . . ?
C13 O14 EU1 119.6(3) . . ?
O13 C13 O14 127.7(5) . . ?
O13 C13 C14 117.1(4) . . ?
O14 C13 C14 115.2(4) . . ?
O16 C14 O15 126.4(5) . . ?
O16 C14 C13 117.6(4) . . ?
O15 C14 C13 115.9(4) . . ?
C14 O15 EU2 120.1(3) . . ?
C14 O16 EU1 117.5(3) . . ?
O18 C15 O17 127.3(4) . . ?
O18 C15 C15 116.0(5) . 2_536 ?
O17 C15 C15 116.7(5) . 2_536 ?
C15 O17 EU1 117.8(3) . 2_536 ?
C15 O18 EU1 122.0(3) . . ?
EU1 O1W H1WA 109.7 . . ?
EU1 O1W H1WB 108.7 . . ?
H1WA O1W H1WB 108.2 . . ?
EU1 O2W H2WA 112.0 . . ?
EU1 O2W H2WB 110.8 . . ?
H2WA O2W H2WB 109.1 . . ?
EU2 O3W H3WA 111.2 . . ?
EU2 O3W H3WB 110.3 . . ?
H3WA O3W H3WB 109.9 . . ?

_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         1.699
_refine_diff_density_min         -1.427
_refine_diff_density_rms         0.199

# Attachment 'complex5.cif'

data_complex5
_database_code_depnum_ccdc_archive 'CCDC 647834'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H28 N4 Ni2 O24 Pr2'
_chemical_formula_weight         1083.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 '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                   7.113(2)
_cell_length_b                   8.519(2)
_cell_length_c                   12.641(4)
_cell_angle_alpha                74.748(5)
_cell_angle_beta                 88.024(5)
_cell_angle_gamma                86.919(5)
_cell_volume                     737.8(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    3460
_cell_measurement_theta_min      2.481
_cell_measurement_theta_max      28.403

_exptl_crystal_description       stick
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             530
_exptl_absorpt_coefficient_mu    4.612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4168
_exptl_absorpt_correction_T_max  0.7384
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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_%        ?
_diffrn_reflns_number            3094
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         24.99
_reflns_number_total             2363
_reflns_number_gt                2310
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_cell_refinement       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0916P)²+1.4296P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2363
_refine_ls_number_parameters     238
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0371
_refine_ls_wR_factor_ref         0.1121
_refine_ls_wR_factor_gt          0.1110
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.005
_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
Pr1 Pr 0.20527(2) 0.06631(2) 0.685363(14) 0.00791(6) Uani 1 1 d . . .
Ni1 Ni -0.5000 0.0000 1.0000 0.00864(15) Uani 1 2 d S . .
Ni2 Ni -0.5000 0.5000 0.5000 0.00893(15) Uani 1 2 d S . .
O1 O -0.0521(4) 0.0665(4) 0.8023(2) 0.0216(7) Uani 1 1 d . . .
O2 O -0.2889(4) 0.1132(3) 0.9053(2) 0.0160(7) Uani 1 1 d . . .
C1 C -0.1953(6) -0.1596(5) 0.9136(4) 0.0242(11) Uani 1 1 d . . .
H1A H -0.2023 -0.2082 0.8509 0.029 Uiso 1 1 calc R . .
H1B H -0.0799 -0.2060 0.9541 0.029 Uiso 1 1 calc R . .
C2 C -0.1796(5) 0.0209(5) 0.8704(3) 0.0144(9) Uani 1 1 d . . .
N1 N -0.3577(4) -0.2052(4) 0.9855(3) 0.0112(7) Uani 1 1 d . . .
H1C H -0.3189 -0.2670 1.0540 0.013 Uiso 1 1 calc R . .
C3 C -0.4959(6) -0.2911(5) 0.9430(3) 0.0175(10) Uani 1 1 d . . .
H3A H -0.5694 -0.3581 1.0049 0.021 Uiso 1 1 calc R . .
H3B H -0.4300 -0.3653 0.9039 0.021 Uiso 1 1 calc R . .
C4 C -0.6264(6) -0.1764(5) 0.8668(3) 0.0145(9) Uani 1 1 d . . .
O3 O -0.7337(4) -0.2267(3) 0.8100(2) 0.0148(6) Uani 1 1 d . . .
O4 O -0.6214(4) -0.0277(3) 0.8623(2) 0.0137(6) Uani 1 1 d . . .
O5 O -0.0107(4) 0.2538(3) 0.5742(2) 0.0165(7) Uani 1 1 d . . .
O6 O -0.2661(4) 0.3580(3) 0.4869(2) 0.0112(6) Uani 1 1 d . . .
C5 C -0.1908(5) 0.4375(5) 0.6466(3) 0.0152(9) Uani 1 1 d . . .
H5A H -0.1938 0.3608 0.7206 0.018 Uiso 1 1 calc R . .
H5B H -0.0849 0.5095 0.6435 0.018 Uiso 1 1 calc R . .
C6 C -0.1554(5) 0.3426(5) 0.5633(3) 0.0124(9) Uani 1 1 d . . .
N2 N -0.3674(4) 0.5372(4) 0.6308(3) 0.0113(7) Uani 1 1 d . . .
H2A H -0.3416 0.6466 0.6176 0.014 Uiso 1 1 calc R . .
C7 C -0.5026(5) 0.4934(5) 0.7216(3) 0.0106(8) Uani 1 1 d . . .
H7A H -0.5822 0.5909 0.7251 0.013 Uiso 1 1 calc R . .
H7B H -0.4343 0.4552 0.7913 0.013 Uiso 1 1 calc R . .
C8 C -0.6244(5) 0.3633(5) 0.7088(3) 0.0133(9) Uani 1 1 d . . .
O7 O -0.6020(4) 0.3136(3) 0.6225(2) 0.0122(6) Uani 1 1 d . . .
O8 O -0.7397(4) 0.3012(3) 0.7810(2) 0.0143(6) Uani 1 1 d . . .
C9 C 0.5644(5) -0.0465(4) 0.5459(3) 0.0112(8) Uani 1 1 d . . .
O9 O 0.5093(4) -0.0599(4) 0.6404(2) 0.0165(7) Uani 1 1 d . . .
O10 O 0.7145(3) -0.1054(3) 0.5163(2) 0.0122(6) Uani 1 1 d . . .
O1W O 0.0427(4) -0.1412(3) 0.6244(2) 0.0159(7) Uani 1 1 d . . .
H1WA H 0.0715 -0.2226 0.6756 0.019 Uiso 1 1 d R . .
H1WB H -0.0739 -0.1497 0.6254 0.019 Uiso 1 1 d R . .
O2W O 0.0184(13) -0.4941(10) 0.8805(8) 0.060(3) Uani 0.50 1 d P . .
O2W' O 0.0964(16) -0.4498(14) 1.0947(7) 0.067(3) Uani 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
Pr1 O1 2.313(3) . ?
Pr1 O5 2.364(3) . ?
Pr1 O1W 2.460(3) . ?
Pr1 O9 2.479(3) . ?
Pr1 O7 2.511(3) 1_655 ?
Pr1 O4 2.512(3) 1_655 ?
Pr1 O10 2.531(3) 2_656 ?
Pr1 O3 2.600(3) 1_655 ?
Pr1 O8 2.647(3) 1_655 ?
Pr1 C4 2.898(4) 1_655 ?
Pr1 C8 2.951(4) 1_655 ?
Ni1 O2 2.011(3) 2_457 ?
Ni1 O2 2.011(3) . ?
Ni1 N1 2.020(3) . ?
Ni1 N1 2.020(3) 2_457 ?
Ni1 O4 2.042(3) . ?
Ni1 O4 2.042(3) 2_457 ?
Ni2 O6 2.032(3) . ?
Ni2 O6 2.032(3) 2_466 ?
Ni2 N2 2.035(3) 2_466 ?
Ni2 N2 2.035(3) . ?
Ni2 O7 2.049(3) . ?
Ni2 O7 2.049(3) 2_466 ?
O1 C2 1.234(5) . ?
O2 C2 1.228(5) . ?
C1 N1 1.449(5) . ?
C1 C2 1.499(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
N1 C3 1.453(5) . ?
N1 H1C 0.9300 . ?
C3 C4 1.488(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O3 1.232(5) . ?
C4 O4 1.255(5) . ?
C4 Pr1 2.898(4) 1_455 ?
O3 Pr1 2.600(3) 1_455 ?
O4 Pr1 2.512(3) 1_455 ?
O5 C6 1.234(5) . ?
O6 C6 1.243(5) . ?
C5 N2 1.467(5) . ?
C5 C6 1.494(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
N2 C7 1.455(5) . ?
N2 H2A 0.9300 . ?
C7 C8 1.488(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 O8 1.235(5) . ?
C8 O7 1.272(5) . ?
C8 Pr1 2.951(4) 1_455 ?
O7 Pr1 2.511(3) 1_455 ?
O8 Pr1 2.647(3) 1_455 ?
C9 O9 1.222(5) . ?
C9 O10 1.243(5) . ?
C9 C9 1.526(8) 2_656 ?
O10 Pr1 2.531(3) 2_656 ?
O1W H1WA 0.8360 . ?
O1W H1WB 0.8363 . ?
O2W O2W' 0.969(13) 2_547 ?
O2W' O2W 0.969(13) 2_547 ?

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 Pr1 O5 77.22(10) . . ?
O1 Pr1 O1W 85.46(11) . . ?
O5 Pr1 O1W 84.99(10) . . ?
O1 Pr1 O9 150.06(9) . . ?
O5 Pr1 O9 131.47(9) . . ?
O1W Pr1 O9 88.62(10) . . ?
O1 Pr1 O7 120.50(10) . 1_655 ?
O5 Pr1 O7 78.50(9) . 1_655 ?
O1W Pr1 O7 144.38(9) . 1_655 ?
O9 Pr1 O7 79.44(9) . 1_655 ?
O1 Pr1 O4 82.70(10) . 1_655 ?
O5 Pr1 O4 148.96(10) . 1_655 ?
O1W Pr1 O4 116.95(9) . 1_655 ?
O9 Pr1 O4 73.95(9) . 1_655 ?
O7 Pr1 O4 91.95(9) 1_655 1_655 ?
O1 Pr1 O10 140.62(9) . 2_656 ?
O5 Pr1 O10 68.71(9) . 2_656 ?
O1W Pr1 O10 72.76(9) . 2_656 ?
O9 Pr1 O10 63.48(8) . 2_656 ?
O7 Pr1 O10 71.87(9) 1_655 2_656 ?
O4 Pr1 O10 136.34(8) 1_655 2_656 ?
O1 Pr1 O3 83.05(9) . 1_655 ?
O5 Pr1 O3 146.80(9) . 1_655 ?
O1W Pr1 O3 66.90(9) . 1_655 ?
O9 Pr1 O3 67.69(9) . 1_655 ?
O7 Pr1 O3 134.70(9) 1_655 1_655 ?
O4 Pr1 O3 50.27(9) 1_655 1_655 ?
O10 Pr1 O3 115.78(9) 2_656 1_655 ?
O1 Pr1 O8 74.86(10) . 1_655 ?
O5 Pr1 O8 85.89(10) . 1_655 ?
O1W Pr1 O8 159.72(9) . 1_655 ?
O9 Pr1 O8 110.89(9) . 1_655 ?
O7 Pr1 O8 49.88(8) 1_655 1_655 ?
O4 Pr1 O8 65.99(9) 1_655 1_655 ?
O10 Pr1 O8 120.20(8) 2_656 1_655 ?
O3 Pr1 O8 114.46(9) 1_655 1_655 ?
O1 Pr1 C4 85.62(10) . 1_655 ?
O5 Pr1 C4 162.75(10) . 1_655 ?
O1W Pr1 C4 92.03(11) . 1_655 ?
O9 Pr1 C4 65.27(10) . 1_655 ?
O7 Pr1 C4 112.41(10) 1_655 1_655 ?
O4 Pr1 C4 25.57(11) 1_655 1_655 ?
O10 Pr1 C4 126.54(10) 2_656 1_655 ?
O3 Pr1 C4 25.15(11) 1_655 1_655 ?
O8 Pr1 C4 91.33(10) 1_655 1_655 ?
O1 Pr1 C8 98.40(11) . 1_655 ?
O5 Pr1 C8 83.62(11) . 1_655 ?
O1W Pr1 C8 166.84(10) . 1_655 ?
O9 Pr1 C8 93.99(10) . 1_655 ?
O7 Pr1 C8 25.32(10) 1_655 1_655 ?
O4 Pr1 C8 76.12(10) 1_655 1_655 ?
O10 Pr1 C8 96.88(10) 2_656 1_655 ?
O3 Pr1 C8 125.93(10) 1_655 1_655 ?
O8 Pr1 C8 24.74(9) 1_655 1_655 ?
C4 Pr1 C8 100.78(11) 1_655 1_655 ?
O2 Ni1 O2 180.0 2_457 . ?
O2 Ni1 N1 95.93(12) 2_457 . ?
O2 Ni1 N1 84.07(12) . . ?
O2 Ni1 N1 84.07(12) 2_457 2_457 ?
O2 Ni1 N1 95.93(12) . 2_457 ?
N1 Ni1 N1 180.00(18) . 2_457 ?
O2 Ni1 O4 91.04(11) 2_457 . ?
O2 Ni1 O4 88.96(11) . . ?
N1 Ni1 O4 80.47(12) . . ?
N1 Ni1 O4 99.53(12) 2_457 . ?
O2 Ni1 O4 88.96(11) 2_457 2_457 ?
O2 Ni1 O4 91.04(11) . 2_457 ?
N1 Ni1 O4 99.53(12) . 2_457 ?
N1 Ni1 O4 80.47(12) 2_457 2_457 ?
O4 Ni1 O4 180.000(1) . 2_457 ?
O6 Ni2 O6 180.0 . 2_466 ?
O6 Ni2 N2 95.95(12) . 2_466 ?
O6 Ni2 N2 84.05(12) 2_466 2_466 ?
O6 Ni2 N2 84.05(12) . . ?
O6 Ni2 N2 95.95(12) 2_466 . ?
N2 Ni2 N2 180.000(1) 2_466 . ?
O6 Ni2 O7 89.58(10) . . ?
O6 Ni2 O7 90.42(10) 2_466 . ?
N2 Ni2 O7 100.06(12) 2_466 . ?
N2 Ni2 O7 79.94(12) . . ?
O6 Ni2 O7 90.42(10) . 2_466 ?
O6 Ni2 O7 89.58(10) 2_466 2_466 ?
N2 Ni2 O7 79.94(12) 2_466 2_466 ?
N2 Ni2 O7 100.06(12) . 2_466 ?
O7 Ni2 O7 180.000(1) . 2_466 ?
C2 O1 Pr1 162.3(3) . . ?
C2 O2 Ni1 113.7(3) . . ?
N1 C1 C2 113.6(3) . . ?
N1 C1 H1A 108.8 . . ?
C2 C1 H1A 108.8 . . ?
N1 C1 H1B 108.8 . . ?
C2 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
O2 C2 O1 124.2(4) . . ?
O2 C2 C1 119.4(3) . . ?
O1 C2 C1 116.4(4) . . ?
C1 N1 C3 114.3(3) . . ?
C1 N1 Ni1 108.5(2) . . ?
C3 N1 Ni1 103.9(2) . . ?
C1 N1 H1C 110.0 . . ?
C3 N1 H1C 110.0 . . ?
Ni1 N1 H1C 110.0 . . ?
N1 C3 C4 111.6(3) . . ?
N1 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
N1 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
O3 C4 O4 121.8(4) . . ?
O3 C4 C3 120.7(4) . . ?
O4 C4 C3 117.5(4) . . ?
O3 C4 Pr1 63.8(2) . 1_455 ?
O4 C4 Pr1 59.8(2) . 1_455 ?
C3 C4 Pr1 165.5(3) . 1_455 ?
C4 O3 Pr1 91.1(2) . 1_455 ?
C4 O4 Ni1 109.8(2) . . ?
C4 O4 Pr1 94.7(2) . 1_455 ?
Ni1 O4 Pr1 155.29(13) . 1_455 ?
C6 O5 Pr1 151.0(3) . . ?
C6 O6 Ni2 113.2(2) . . ?
N2 C5 C6 113.5(3) . . ?
N2 C5 H5A 108.9 . . ?
C6 C5 H5A 108.9 . . ?
N2 C5 H5B 108.9 . . ?
C6 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
O5 C6 O6 123.4(4) . . ?
O5 C6 C5 116.3(4) . . ?
O6 C6 C5 120.3(3) . . ?
C7 N2 C5 114.2(3) . . ?
C7 N2 Ni2 104.7(2) . . ?
C5 N2 Ni2 108.5(2) . . ?
C7 N2 H2A 109.7 . . ?
C5 N2 H2A 109.7 . . ?
Ni2 N2 H2A 109.7 . . ?
N2 C7 C8 111.4(3) . . ?
N2 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
N2 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
O8 C8 O7 120.7(4) . . ?
O8 C8 C7 121.4(4) . . ?
O7 C8 C7 117.9(3) . . ?
O8 C8 Pr1 63.7(2) . 1_455 ?
O7 C8 Pr1 57.61(19) . 1_455 ?
C7 C8 Pr1 168.5(3) . 1_455 ?
C8 O7 Ni2 108.1(2) . . ?
C8 O7 Pr1 97.1(2) . 1_455 ?
Ni2 O7 Pr1 150.68(14) . 1_455 ?
C8 O8 Pr1 91.5(2) . 1_455 ?
O9 C9 O10 126.4(4) . . ?
O9 C9 C9 117.7(4) . 2_656 ?
O10 C9 C9 115.8(4) . 2_656 ?
C9 O9 Pr1 122.3(2) . . ?
C9 O10 Pr1 120.6(2) . 2_656 ?
Pr1 O1W H1WA 99.0 . . ?
Pr1 O1W H1WB 125.4 . . ?
H1WA O1W H1WB 99.4 . . ?

_diffrn_measured_fraction_theta_max 0.912
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.912
_refine_diff_density_max         3.127
_refine_diff_density_min         -2.314
_refine_diff_density_rms         0.210

# Attachment 'complex5a.cif'

data_complex5a
_database_code_depnum_ccdc_archive 'CCDC 647835'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H24 N4 Ni2 O22 Pr2'
_chemical_formula_weight         1047.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 '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                   7.153(2)
_cell_length_b                   8.569(3)
_cell_length_c                   12.570(4)
_cell_angle_alpha                75.026(6)
_cell_angle_beta                 87.787(6)
_cell_angle_gamma                85.779(6)
_cell_volume                     742.2(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2947
_cell_measurement_theta_min      2.466
_cell_measurement_theta_max      28.268

_exptl_crystal_description       stick
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             510
_exptl_absorpt_coefficient_mu    4.575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4467
_exptl_absorpt_correction_T_max  0.8382
_exptl_absorpt_process_details   sadabs

_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_%        ?
_diffrn_reflns_number            3141
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2411
_reflns_number_gt                2200
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_cell_refinement       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0916P)²+1.4296P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2411
_refine_ls_number_parameters     220
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1360
_refine_ls_wR_factor_gt          0.1329
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_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
Pr1 Pr 0.20721(6) 0.06611(6) 0.68689(3) 0.0156(2) Uani 1 1 d . . .
Ni1 Ni -0.5000 0.0000 1.0000 0.0158(4) Uani 1 2 d S . .
Ni2 Ni -0.5000 0.5000 0.5000 0.0158(4) Uani 1 2 d S . .
O1 O -0.0435(10) 0.0636(10) 0.8091(6) 0.0406(19) Uani 1 1 d . . .
O2 O -0.2915(9) 0.1119(8) 0.9051(5) 0.0255(14) Uani 1 1 d . . .
C1 C -0.1827(15) -0.1591(14) 0.9190(10) 0.043(3) Uani 1 1 d . . .
H1A H -0.1798 -0.2093 0.8580 0.051 Uiso 1 1 calc R . .
H1B H -0.0726 -0.2009 0.9628 0.051 Uiso 1 1 calc R . .
C2 C -0.1766(13) 0.0179(13) 0.8755(7) 0.028(2) Uani 1 1 d . . .
N1 N -0.3505(10) -0.2023(9) 0.9866(5) 0.0202(16) Uani 1 1 d . . .
H1C H -0.3159 -0.2614 1.0549 0.024 Uiso 1 1 calc R . .
C3 C -0.4823(14) -0.2914(11) 0.9423(8) 0.029(2) Uani 1 1 d . . .
H3A H -0.5521 -0.3586 1.0025 0.035 Uiso 1 1 calc R . .
H3B H -0.4133 -0.3616 0.9031 0.035 Uiso 1 1 calc R . .
C4 C -0.6137(13) -0.1786(11) 0.8670(7) 0.022(2) Uani 1 1 d . . .
O3 O -0.7187(10) -0.2290(8) 0.8102(6) 0.0324(16) Uani 1 1 d . . .
O4 O -0.6162(9) -0.0301(8) 0.8619(5) 0.0243(14) Uani 1 1 d . . .
O5 O -0.0138(9) 0.2480(9) 0.5783(5) 0.0344(17) Uani 1 1 d . . .
O6 O -0.2665(9) 0.3538(8) 0.4904(5) 0.0251(14) Uani 1 1 d . . .
C5 C -0.1930(13) 0.4396(14) 0.6459(8) 0.033(2) Uani 1 1 d . . .
H5A H -0.1859 0.3686 0.7197 0.040 Uiso 1 1 calc R . .
H5B H -0.0936 0.5133 0.6373 0.040 Uiso 1 1 calc R . .
C6 C -0.1598(12) 0.3408(12) 0.5660(7) 0.023(2) Uani 1 1 d . . .
N2 N -0.3724(10) 0.5333(9) 0.6351(5) 0.0172(15) Uani 1 1 d . . .
H2A H -0.3537 0.6401 0.6253 0.021 Uiso 1 1 calc R . .
C7 C -0.5057(13) 0.4829(12) 0.7235(7) 0.024(2) Uani 1 1 d . . .
H7A H -0.5855 0.5765 0.7303 0.028 Uiso 1 1 calc R . .
H7B H -0.4385 0.4421 0.7917 0.028 Uiso 1 1 calc R . .
C8 C -0.6241(12) 0.3580(10) 0.7091(7) 0.0177(18) Uani 1 1 d . . .
O7 O -0.6069(9) 0.3165(8) 0.6198(5) 0.0245(14) Uani 1 1 d . . .
O8 O -0.7354(9) 0.2951(8) 0.7816(5) 0.0281(15) Uani 1 1 d . . .
C9 C 0.5667(12) -0.0440(11) 0.5453(7) 0.0209(19) Uani 1 1 d . . .
O9 O 0.5130(10) -0.0588(9) 0.6406(5) 0.0355(18) Uani 1 1 d . . .
O10 O 0.7178(9) -0.1024(8) 0.5146(5) 0.0273(15) Uani 1 1 d . . .
O1W O 0.0418(11) -0.1374(9) 0.6256(6) 0.0374(18) Uani 1 1 d . . .
H1WA H 0.0706 -0.2188 0.6767 0.045 Uiso 1 1 d R . .
H1WB H -0.0748 -0.1459 0.6266 0.045 Uiso 1 1 d R . .


_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
Pr1 O1 2.313(6) . ?
Pr1 O5 2.344(6) . ?
Pr1 O1W 2.470(7) . ?
Pr1 O9 2.479(6) . ?
Pr1 O4 2.497(6) 1_655 ?
Pr1 O10 2.512(6) 2_656 ?
Pr1 O7 2.545(6) 1_655 ?
Pr1 O8 2.608(7) 1_655 ?
Pr1 O3 2.630(7) 1_655 ?
Pr1 C4 2.922(8) 1_655 ?
Pr1 C8 2.936(9) 1_655 ?
Ni1 N1 2.010(7) 2_457 ?
Ni1 N1 2.010(7) . ?
Ni1 O2 2.013(6) 2_457 ?
Ni1 O2 2.013(6) . ?
Ni1 O4 2.037(6) 2_457 ?
Ni1 O4 2.037(6) . ?
Ni2 O6 2.031(6) 2_466 ?
Ni2 O6 2.031(6) . ?
Ni2 O7 2.047(6) . ?
Ni2 O7 2.047(6) 2_466 ?
Ni2 N2 2.052(7) . ?
Ni2 N2 2.052(7) 2_466 ?
O1 C2 1.258(12) . ?
O2 C2 1.223(12) . ?
C1 N1 1.457(12) . ?
C1 C2 1.477(15) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
N1 C3 1.466(13) . ?
N1 H1C 0.9100 . ?
C3 C4 1.475(12) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 O3 1.228(11) . ?
C4 O4 1.256(11) . ?
C4 Pr1 2.922(8) 1_455 ?
O3 Pr1 2.630(7) 1_455 ?
O4 Pr1 2.497(6) 1_455 ?
O5 C6 1.254(11) . ?
O6 C6 1.219(10) . ?
C5 N2 1.455(11) . ?
C5 C6 1.475(14) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
N2 C7 1.435(11) . ?
N2 H2A 0.9100 . ?
C7 C8 1.463(13) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O8 1.228(11) . ?
C8 O7 1.261(11) . ?
C8 Pr1 2.937(9) 1_455 ?
O7 Pr1 2.545(6) 1_455 ?
O8 Pr1 2.608(7) 1_455 ?
C9 O9 1.222(11) . ?
C9 O10 1.247(11) . ?
C9 C9 1.520(17) 2_656 ?
O10 Pr1 2.512(6) 2_656 ?
O1W H1WA 0.8365 . ?
O1W H1WB 0.8424 . ?

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 Pr1 O5 78.0(3) . . ?
O1 Pr1 O1W 85.0(3) . . ?
O5 Pr1 O1W 83.2(3) . . ?
O1 Pr1 O9 148.8(3) . . ?
O5 Pr1 O9 132.0(2) . . ?
O1W Pr1 O9 90.2(3) . . ?
O1 Pr1 O4 81.8(2) . 1_655 ?
O5 Pr1 O4 150.0(2) . 1_655 ?
O1W Pr1 O4 117.1(2) . 1_655 ?
O9 Pr1 O4 73.0(2) . 1_655 ?
O1 Pr1 O10 141.6(2) . 2_656 ?
O5 Pr1 O10 68.9(2) . 2_656 ?
O1W Pr1 O10 72.6(2) . 2_656 ?
O9 Pr1 O10 63.8(2) . 2_656 ?
O4 Pr1 O10 136.0(2) 1_655 2_656 ?
O1 Pr1 O7 120.8(2) . 1_655 ?
O5 Pr1 O7 78.6(2) . 1_655 ?
O1W Pr1 O7 143.7(2) . 1_655 ?
O9 Pr1 O7 79.5(2) . 1_655 ?
O4 Pr1 O7 93.2(2) 1_655 1_655 ?
O10 Pr1 O7 71.7(2) 2_656 1_655 ?
O1 Pr1 O8 75.6(2) . 1_655 ?
O5 Pr1 O8 87.2(2) . 1_655 ?
O1W Pr1 O8 159.7(2) . 1_655 ?
O9 Pr1 O8 109.4(2) . 1_655 ?
O4 Pr1 O8 66.2(2) 1_655 1_655 ?
O10 Pr1 O8 120.2(2) 2_656 1_655 ?
O7 Pr1 O8 49.75(19) 1_655 1_655 ?
O1 Pr1 O3 83.1(3) . 1_655 ?
O5 Pr1 O3 146.6(2) . 1_655 ?
O1W Pr1 O3 67.8(2) . 1_655 ?
O9 Pr1 O3 66.6(2) . 1_655 ?
O4 Pr1 O3 49.7(2) 1_655 1_655 ?
O10 Pr1 O3 114.6(2) 2_656 1_655 ?
O7 Pr1 O3 134.8(2) 1_655 1_655 ?
O8 Pr1 O3 114.5(2) 1_655 1_655 ?
O1 Pr1 C4 85.1(3) . 1_655 ?
O5 Pr1 C4 162.9(2) . 1_655 ?
O1W Pr1 C4 92.6(3) . 1_655 ?
O9 Pr1 C4 64.3(2) . 1_655 ?
O4 Pr1 C4 25.3(2) 1_655 1_655 ?
O10 Pr1 C4 125.6(2) 2_656 1_655 ?
O7 Pr1 C4 113.1(2) 1_655 1_655 ?
O8 Pr1 C4 91.3(2) 1_655 1_655 ?
O3 Pr1 C4 24.8(2) 1_655 1_655 ?
O1 Pr1 C8 99.1(3) . 1_655 ?
O5 Pr1 C8 84.9(3) . 1_655 ?
O1W Pr1 C8 166.4(2) . 1_655 ?
O9 Pr1 C8 92.7(3) . 1_655 ?
O4 Pr1 C8 76.5(2) 1_655 1_655 ?
O10 Pr1 C8 96.9(2) 2_656 1_655 ?
O7 Pr1 C8 25.3(2) 1_655 1_655 ?
O8 Pr1 C8 24.7(2) 1_655 1_655 ?
O3 Pr1 C8 125.5(2) 1_655 1_655 ?
C4 Pr1 C8 100.7(2) 1_655 1_655 ?
N1 Ni1 N1 180.000(2) 2_457 . ?
N1 Ni1 O2 83.6(3) 2_457 2_457 ?
N1 Ni1 O2 96.4(3) . 2_457 ?
N1 Ni1 O2 96.4(3) 2_457 . ?
N1 Ni1 O2 83.6(3) . . ?
O2 Ni1 O2 180.0 2_457 . ?
N1 Ni1 O4 80.7(3) 2_457 2_457 ?
N1 Ni1 O4 99.3(3) . 2_457 ?
O2 Ni1 O4 88.8(3) 2_457 2_457 ?
O2 Ni1 O4 91.2(3) . 2_457 ?
N1 Ni1 O4 99.3(3) 2_457 . ?
N1 Ni1 O4 80.7(3) . . ?
O2 Ni1 O4 91.2(3) 2_457 . ?
O2 Ni1 O4 88.8(3) . . ?
O4 Ni1 O4 180.000(1) 2_457 . ?
O6 Ni2 O6 180.000(1) 2_466 . ?
O6 Ni2 O7 90.7(3) 2_466 . ?
O6 Ni2 O7 89.3(3) . . ?
O6 Ni2 O7 89.3(3) 2_466 2_466 ?
O6 Ni2 O7 90.7(3) . 2_466 ?
O7 Ni2 O7 180.0(3) . 2_466 ?
O6 Ni2 N2 96.3(3) 2_466 . ?
O6 Ni2 N2 83.7(3) . . ?
O7 Ni2 N2 80.2(3) . . ?
O7 Ni2 N2 99.8(3) 2_466 . ?
O6 Ni2 N2 83.7(3) 2_466 2_466 ?
O6 Ni2 N2 96.3(3) . 2_466 ?
O7 Ni2 N2 99.8(3) . 2_466 ?
O7 Ni2 N2 80.2(3) 2_466 2_466 ?
N2 Ni2 N2 180.000(1) . 2_466 ?
C2 O1 Pr1 162.6(8) . . ?
C2 O2 Ni1 113.0(6) . . ?
N1 C1 C2 111.9(8) . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
O2 C2 O1 123.1(10) . . ?
O2 C2 C1 121.5(8) . . ?
O1 C2 C1 115.4(9) . . ?
C1 N1 C3 115.3(8) . . ?
C1 N1 Ni1 109.6(6) . . ?
C3 N1 Ni1 104.4(6) . . ?
C1 N1 H1C 109.1 . . ?
C3 N1 H1C 109.1 . . ?
Ni1 N1 H1C 109.1 . . ?
N1 C3 C4 110.7(8) . . ?
N1 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
O3 C4 O4 120.6(8) . . ?
O3 C4 C3 120.6(8) . . ?
O4 C4 C3 118.8(8) . . ?
O3 C4 Pr1 64.2(5) . 1_455 ?
O4 C4 Pr1 58.1(4) . 1_455 ?
C3 C4 Pr1 166.3(7) . 1_455 ?
C4 O3 Pr1 91.0(5) . 1_455 ?
C4 O4 Ni1 109.2(5) . . ?
C4 O4 Pr1 96.6(5) . 1_455 ?
Ni1 O4 Pr1 153.8(3) . 1_455 ?
C6 O5 Pr1 152.6(6) . . ?
C6 O6 Ni2 113.1(6) . . ?
N2 C5 C6 114.4(8) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
O6 C6 O5 122.6(9) . . ?
O6 C6 C5 121.0(8) . . ?
O5 C6 C5 116.3(8) . . ?
C7 N2 C5 115.7(7) . . ?
C7 N2 Ni2 104.0(5) . . ?
C5 N2 Ni2 107.4(6) . . ?
C7 N2 H2A 109.8 . . ?
C5 N2 H2A 109.8 . . ?
Ni2 N2 H2A 109.8 . . ?
N2 C7 C8 114.0(7) . . ?
N2 C7 H7A 108.7 . . ?
C8 C7 H7A 108.7 . . ?
N2 C7 H7B 108.7 . . ?
C8 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
O8 C8 O7 121.1(8) . . ?
O8 C8 C7 121.3(8) . . ?
O7 C8 C7 117.6(7) . . ?
O8 C8 Pr1 62.5(5) . 1_455 ?
O7 C8 Pr1 59.7(4) . 1_455 ?
C7 C8 Pr1 168.7(6) . 1_455 ?
C8 O7 Ni2 109.5(6) . . ?
C8 O7 Pr1 94.9(5) . 1_455 ?
Ni2 O7 Pr1 153.3(3) . 1_455 ?
C8 O8 Pr1 92.8(5) . 1_455 ?
O9 C9 O10 126.1(8) . . ?
O9 C9 C9 117.7(9) . 2_656 ?
O10 C9 C9 116.1(9) . 2_656 ?
C9 O9 Pr1 121.8(6) . . ?
C9 O10 Pr1 120.5(5) . 2_656 ?
Pr1 O1W H1WA 99.1 . . ?
Pr1 O1W H1WB 127.0 . . ?
H1WA O1W H1WB 98.6 . . ?

_diffrn_measured_fraction_theta_max 0.924
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.924
_refine_diff_density_max         3.067
_refine_diff_density_min         -2.512
_refine_diff_density_rms         0.249

# Attachment 'complex6.cif'

data_complex6
_database_code_depnum_ccdc_archive 'CCDC 647836'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H14 La N2 Ni O12'
_chemical_formula_weight         539.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   7.2250(13)
_cell_length_b                   8.6469(16)
_cell_length_c                   12.836(2)
_cell_angle_alpha                74.971(3)
_cell_angle_beta                 87.847(3)
_cell_angle_gamma                86.518(3)
_cell_volume                     772.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    6065
_cell_measurement_theta_min      2.442
_cell_measurement_theta_max      28.385

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             526
_exptl_absorpt_coefficient_mu    4.014
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4217
_exptl_absorpt_correction_T_max  0.6445
_exptl_absorpt_process_details   sadabs

_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_%        ?
_diffrn_reflns_number            5910
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         25.99
_reflns_number_total             2952
_reflns_number_gt                2912
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_cell_refinement       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0340P)²+1.4002P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2952
_refine_ls_number_parameters     238
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0248
_refine_ls_wR_factor_ref         0.0654
_refine_ls_wR_factor_gt          0.0651
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.104
_refine_ls_shift/su_max          0.022
_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
La1 La 0.204798(16) 0.067170(14) 0.686207(9) 0.01699(3) Uani 1 1 d . . .
Ni1 Ni -0.5000 0.0000 1.0000 0.01815(9) Uani 1 2 d S . .
Ni2 Ni -0.5000 0.5000 0.5000 0.01861(9) Uani 1 2 d S . .
O1 O -0.0522(3) 0.0659(3) 0.80751(18) 0.0446(6) Uani 1 1 d . . .
O2 O -0.2914(3) 0.1124(2) 0.90613(16) 0.0321(5) Uani 1 1 d . . .
C1 C -0.1952(4) -0.1561(4) 0.9140(3) 0.0470(9) Uani 1 1 d . . .
H1A H -0.1998 -0.2019 0.8528 0.056 Uiso 1 1 calc R . .
H1B H -0.0840 -0.2009 0.9533 0.056 Uiso 1 1 calc R . .
C2 C -0.1810(4) 0.0211(3) 0.8732(2) 0.0285(6) Uani 1 1 d . . .
N1 N -0.3565(3) -0.2038(2) 0.98436(17) 0.0241(5) Uani 1 1 d . . .
H1C H -0.3188 -0.2633 1.0502 0.029 Uiso 1 1 calc R . .
C3 C -0.4897(4) -0.2897(3) 0.9420(2) 0.0320(6) Uani 1 1 d . . .
H3A H -0.5595 -0.3555 1.0014 0.038 Uiso 1 1 calc R . .
H3B H -0.4240 -0.3602 0.9037 0.038 Uiso 1 1 calc R . .
C4 C -0.6219(4) -0.1763(3) 0.8666(2) 0.0254(6) Uani 1 1 d . . .
O3 O -0.7258(3) -0.2261(2) 0.81058(16) 0.0335(5) Uani 1 1 d . . .
O4 O -0.6209(3) -0.0299(2) 0.86440(14) 0.0266(4) Uani 1 1 d . . .
O5 O -0.0178(3) 0.2520(3) 0.57481(16) 0.0380(5) Uani 1 1 d . . .
O6 O -0.2709(2) 0.3553(2) 0.48940(14) 0.0282(4) Uani 1 1 d . . .
C5 C -0.1956(4) 0.4391(3) 0.6440(2) 0.0314(6) Uani 1 1 d . . .
H5A H -0.1956 0.3674 0.7159 0.038 Uiso 1 1 calc R . .
H5B H -0.0938 0.5092 0.6387 0.038 Uiso 1 1 calc R . .
C6 C -0.1616(3) 0.3415(3) 0.5636(2) 0.0249(6) Uani 1 1 d . . .
N2 N -0.3698(3) 0.5370(2) 0.63007(16) 0.0221(5) Uani 1 1 d . . .
H2A H -0.3460 0.6424 0.6178 0.027 Uiso 1 1 calc R . .
C7 C -0.5024(4) 0.4925(3) 0.7205(2) 0.0272(6) Uani 1 1 d . . .
H7A H -0.5798 0.5863 0.7251 0.033 Uiso 1 1 calc R . .
H7B H -0.4354 0.4550 0.7872 0.033 Uiso 1 1 calc R . .
C8 C -0.6228(3) 0.3639(3) 0.7076(2) 0.0232(6) Uani 1 1 d . . .
O7 O -0.6069(3) 0.3198(2) 0.62091(14) 0.0269(4) Uani 1 1 d . . .
O8 O -0.7329(3) 0.3016(2) 0.78019(15) 0.0326(5) Uani 1 1 d . . .
C9 C 0.5657(3) -0.0459(3) 0.54503(19) 0.0215(5) Uani 1 1 d . . .
O9 O 0.5121(3) -0.0573(3) 0.63906(15) 0.0363(5) Uani 1 1 d . . .
O10 O 0.7136(2) -0.1031(2) 0.51517(14) 0.0269(4) Uani 1 1 d . . .
O1W O 0.0401(3) -0.1418(2) 0.62478(17) 0.0368(5) Uani 1 1 d . . .
H1WA H 0.0688 -0.2232 0.6759 0.044 Uiso 1 1 d R . .
H1WB H -0.0766 -0.1504 0.6258 0.044 Uiso 1 1 d R . .
O2W O -1.1091(17) 0.4296(12) 0.9019(6) 0.135(4) Uani 0.50 1 d P . .
O2W' O -0.9656(18) 0.5074(9) 0.8874(11) 0.218(5) Uani 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
La1 O1 2.377(2) . ?
La1 O5 2.4209(18) . ?
La1 O1W 2.525(2) . ?
La1 O9 2.5299(19) . ?
La1 O4 2.5721(17) 1_655 ?
La1 O10 2.5725(18) 2_656 ?
La1 O7 2.5787(18) 1_655 ?
La1 O3 2.6530(18) 1_655 ?
La1 O8 2.681(2) 1_655 ?
La1 C4 2.955(2) 1_655 ?
La1 C8 2.998(3) 1_655 ?
Ni1 O2 2.0253(18) . ?
Ni1 O2 2.0253(18) 2_457 ?
Ni1 N1 2.041(2) . ?
Ni1 N1 2.041(2) 2_457 ?
Ni1 O4 2.0578(18) 2_457 ?
Ni1 O4 2.0578(18) . ?
Ni2 O6 2.0356(17) . ?
Ni2 O6 2.0356(17) 2_466 ?
Ni2 N2 2.051(2) 2_466 ?
Ni2 N2 2.051(2) . ?
Ni2 O7 2.0581(17) 2_466 ?
Ni2 O7 2.0581(17) . ?
O1 C2 1.242(3) . ?
O2 C2 1.229(3) . ?
C1 N1 1.459(4) . ?
C1 C2 1.493(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
N1 C3 1.452(4) . ?
N1 H1C 0.9100 . ?
C3 C4 1.508(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 O3 1.227(3) . ?
C4 O4 1.259(3) . ?
C4 La1 2.955(2) 1_455 ?
O3 La1 2.6530(18) 1_455 ?
O4 La1 2.5721(17) 1_455 ?
O5 C6 1.247(3) . ?
O6 C6 1.238(3) . ?
C5 N2 1.463(3) . ?
C5 C6 1.498(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
N2 C7 1.463(3) . ?
N2 H2A 0.9100 . ?
C7 C8 1.498(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O8 1.236(3) . ?
C8 O7 1.266(3) . ?
C8 La1 2.998(3) 1_455 ?
O7 La1 2.5787(18) 1_455 ?
O8 La1 2.681(2) 1_455 ?
C9 O9 1.235(3) . ?
C9 O10 1.239(3) . ?
C9 C9 1.544(5) 2_656 ?
O10 La1 2.5725(18) 2_656 ?
O1W H1WA 0.8501 . ?
O1W H1WB 0.8499 . ?
O2W O2W' 1.252(16) . ?

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 O5 77.77(7) . . ?
O1 La1 O1W 85.56(8) . . ?
O5 La1 O1W 83.71(7) . . ?
O1 La1 O9 149.75(7) . . ?
O5 La1 O9 131.26(6) . . ?
O1W La1 O9 89.30(7) . . ?
O1 La1 O4 81.59(7) . 1_655 ?
O5 La1 O4 149.79(7) . 1_655 ?
O1W La1 O4 116.55(6) . 1_655 ?
O9 La1 O4 74.16(6) . 1_655 ?
O1 La1 O10 141.90(7) . 2_656 ?
O5 La1 O10 69.22(6) . 2_656 ?
O1W La1 O10 72.68(6) . 2_656 ?
O9 La1 O10 62.68(6) . 2_656 ?
O4 La1 O10 136.02(6) 1_655 2_656 ?
O1 La1 O7 120.16(7) . 1_655 ?
O5 La1 O7 78.54(7) . 1_655 ?
O1W La1 O7 144.02(6) . 1_655 ?
O9 La1 O7 79.64(7) . 1_655 ?
O4 La1 O7 93.33(6) 1_655 1_655 ?
O10 La1 O7 71.83(6) 2_656 1_655 ?
O1 La1 O3 83.10(7) . 1_655 ?
O5 La1 O3 146.69(7) . 1_655 ?
O1W La1 O3 67.71(6) . 1_655 ?
O9 La1 O3 67.44(6) . 1_655 ?
O4 La1 O3 49.19(6) 1_655 1_655 ?
O10 La1 O3 115.01(6) 2_656 1_655 ?
O7 La1 O3 134.77(6) 1_655 1_655 ?
O1 La1 O8 75.93(7) . 1_655 ?
O5 La1 O8 87.46(7) . 1_655 ?
O1W La1 O8 160.83(7) . 1_655 ?
O9 La1 O8 109.21(7) . 1_655 ?
O4 La1 O8 66.11(6) 1_655 1_655 ?
O10 La1 O8 119.74(6) 2_656 1_655 ?
O7 La1 O8 48.88(6) 1_655 1_655 ?
O3 La1 O8 114.08(6) 1_655 1_655 ?
O1 La1 C4 85.15(7) . 1_655 ?
O5 La1 C4 162.69(7) . 1_655 ?
O1W La1 C4 92.24(7) . 1_655 ?
O9 La1 C4 65.26(6) . 1_655 ?
O4 La1 C4 25.13(6) 1_655 1_655 ?
O10 La1 C4 125.60(6) 2_656 1_655 ?
O7 La1 C4 113.15(7) 1_655 1_655 ?
O3 La1 C4 24.53(7) 1_655 1_655 ?
O8 La1 C4 91.16(7) 1_655 1_655 ?
O1 La1 C8 99.00(8) . 1_655 ?
O5 La1 C8 84.83(7) . 1_655 ?
O1W La1 C8 166.48(6) . 1_655 ?
O9 La1 C8 92.88(7) . 1_655 ?
O4 La1 C8 76.83(6) 1_655 1_655 ?
O10 La1 C8 96.52(6) 2_656 1_655 ?
O7 La1 C8 24.80(6) 1_655 1_655 ?
O3 La1 C8 125.30(6) 1_655 1_655 ?
O8 La1 C8 24.32(6) 1_655 1_655 ?
C4 La1 C8 100.79(7) 1_655 1_655 ?
O2 Ni1 O2 180.0 . 2_457 ?
O2 Ni1 N1 83.98(8) . . ?
O2 Ni1 N1 96.02(8) 2_457 . ?
O2 Ni1 N1 96.02(8) . 2_457 ?
O2 Ni1 N1 83.98(8) 2_457 2_457 ?
N1 Ni1 N1 180.00(11) . 2_457 ?
O2 Ni1 O4 90.52(8) . 2_457 ?
O2 Ni1 O4 89.48(8) 2_457 2_457 ?
N1 Ni1 O4 99.94(8) . 2_457 ?
N1 Ni1 O4 80.06(8) 2_457 2_457 ?
O2 Ni1 O4 89.48(8) . . ?
O2 Ni1 O4 90.52(8) 2_457 . ?
N1 Ni1 O4 80.06(8) . . ?
N1 Ni1 O4 99.94(8) 2_457 . ?
O4 Ni1 O4 180.0 2_457 . ?
O6 Ni2 O6 180.000(1) . 2_466 ?
O6 Ni2 N2 95.99(8) . 2_466 ?
O6 Ni2 N2 84.01(8) 2_466 2_466 ?
O6 Ni2 N2 84.01(8) . . ?
O6 Ni2 N2 95.99(8) 2_466 . ?
N2 Ni2 N2 180.0 2_466 . ?
O6 Ni2 O7 90.20(7) . 2_466 ?
O6 Ni2 O7 89.80(7) 2_466 2_466 ?
N2 Ni2 O7 80.14(8) 2_466 2_466 ?
N2 Ni2 O7 99.86(8) . 2_466 ?
O6 Ni2 O7 89.80(7) . . ?
O6 Ni2 O7 90.20(7) 2_466 . ?
N2 Ni2 O7 99.86(8) 2_466 . ?
N2 Ni2 O7 80.14(8) . . ?
O7 Ni2 O7 180.00(8) 2_466 . ?
C2 O1 La1 162.6(2) . . ?
C2 O2 Ni1 113.67(17) . . ?
N1 C1 C2 114.2(2) . . ?
N1 C1 H1A 108.7 . . ?
C2 C1 H1A 108.7 . . ?
N1 C1 H1B 108.7 . . ?
C2 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
O2 C2 O1 124.1(3) . . ?
O2 C2 C1 119.9(2) . . ?
O1 C2 C1 116.0(3) . . ?
C3 N1 C1 114.8(2) . . ?
C3 N1 Ni1 104.63(15) . . ?
C1 N1 Ni1 107.82(16) . . ?
C3 N1 H1C 109.8 . . ?
C1 N1 H1C 109.8 . . ?
Ni1 N1 H1C 109.8 . . ?
N1 C3 C4 111.6(2) . . ?
N1 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
N1 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
O3 C4 O4 122.1(2) . . ?
O3 C4 C3 120.9(2) . . ?
O4 C4 C3 117.1(2) . . ?
O3 C4 La1 63.83(13) . 1_455 ?
O4 C4 La1 60.17(12) . 1_455 ?
C3 C4 La1 165.63(18) . 1_455 ?
C4 O3 La1 91.64(14) . 1_455 ?
C4 O4 Ni1 110.84(15) . . ?
C4 O4 La1 94.69(15) . 1_455 ?
Ni1 O4 La1 154.34(8) . 1_455 ?
C6 O5 La1 151.56(18) . . ?
C6 O6 Ni2 113.50(17) . . ?
N2 C5 C6 114.3(2) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
O6 C6 O5 123.4(3) . . ?
O6 C6 C5 120.1(2) . . ?
O5 C6 C5 116.5(2) . . ?
C5 N2 C7 114.19(19) . . ?
C5 N2 Ni2 107.89(17) . . ?
C7 N2 Ni2 105.14(15) . . ?
C5 N2 H2A 109.8 . . ?
C7 N2 H2A 109.8 . . ?
Ni2 N2 H2A 109.8 . . ?
N2 C7 C8 111.5(2) . . ?
N2 C7 H7A 109.3 . . ?
C8 C7 H7A 109.3 . . ?
N2 C7 H7B 109.3 . . ?
C8 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
O8 C8 O7 121.1(2) . . ?
O8 C8 C7 120.8(2) . . ?
O7 C8 C7 118.1(2) . . ?
O8 C8 La1 63.30(14) . 1_455 ?
O7 C8 La1 58.71(13) . 1_455 ?
C7 C8 La1 168.92(17) . 1_455 ?
C8 O7 Ni2 109.72(15) . . ?
C8 O7 La1 96.48(14) . 1_455 ?
Ni2 O7 La1 151.53(9) . 1_455 ?
C8 O8 La1 92.38(16) . 1_455 ?
O9 C9 O10 126.7(2) . . ?
O9 C9 C9 117.0(3) . 2_656 ?
O10 C9 C9 116.3(3) . 2_656 ?
C9 O9 La1 122.64(15) . . ?
C9 O10 La1 121.33(15) . 2_656 ?
La1 O1W H1WA 99.0 . . ?
La1 O1W H1WB 125.9 . . ?
H1WA O1W H1WB 99.2 . . ?

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.968
_refine_diff_density_max         0.936
_refine_diff_density_min         -1.064
_refine_diff_density_rms         0.108

# Attachment 'complex7.cif'

data_complex7
_database_code_depnum_ccdc_archive 'CCDC 647837'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H28 N4 Nd2 Ni2 O24'
_chemical_formula_weight         1090.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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                   7.1630(16)
_cell_length_b                   8.5771(19)
_cell_length_c                   12.728(3)
_cell_angle_alpha                74.789(4)
_cell_angle_beta                 87.820(4)
_cell_angle_gamma                86.685(4)
_cell_volume                     753.1(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    3846
_cell_measurement_theta_min      2.582
_cell_measurement_theta_max      28.299

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             532
_exptl_absorpt_coefficient_mu    4.730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4831
_exptl_absorpt_correction_T_max  0.7034
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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_%        ?
_diffrn_reflns_number            4036
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2847
_reflns_number_gt                2782
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_cell_refinement       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0667P)²+2.6202P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2847
_refine_ls_number_parameters     238
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.1011
_refine_ls_wR_factor_gt          0.1003
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.004
_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
Nd1 Nd 0.20601(2) 0.066780(19) 0.684964(13) 0.00755(5) Uani 1 1 d . . .
Ni1 Ni -0.5000 0.0000 1.0000 0.00840(14) Uani 1 2 d S . .
Ni2 Ni -0.5000 0.5000 0.5000 0.00871(14) Uani 1 2 d S . .
O1 O -0.0500(4) 0.0660(3) 0.8024(2) 0.0202(5) Uani 1 1 d U . .
O2 O -0.2878(4) 0.1139(3) 0.9058(2) 0.0157(6) Uani 1 1 d . . .
C1 C -0.1946(6) -0.1601(5) 0.9119(4) 0.0234(10) Uani 1 1 d . . .
H1A H -0.2025 -0.2068 0.8490 0.028 Uiso 1 1 calc R . .
H1B H -0.0797 -0.2074 0.9514 0.028 Uiso 1 1 calc R . .
C2 C -0.1784(5) 0.0200(5) 0.8703(3) 0.0146(8) Uani 1 1 d . . .
N1 N -0.3583(4) -0.2068(4) 0.9851(2) 0.0118(7) Uani 1 1 d . . .
H1C H -0.3195 -0.2684 1.0530 0.014 Uiso 1 1 calc R . .
C3 C -0.4960(5) -0.2923(4) 0.9422(3) 0.0155(8) Uani 1 1 d . . .
H3A H -0.5693 -0.3588 1.0035 0.019 Uiso 1 1 calc R . .
H3B H -0.4301 -0.3659 0.9033 0.019 Uiso 1 1 calc R . .
C4 C -0.6274(5) -0.1760(4) 0.8653(3) 0.0142(8) Uani 1 1 d . . .
O3 O -0.7344(4) -0.2235(3) 0.8082(2) 0.0150(6) Uani 1 1 d . . .
O4 O -0.6204(4) -0.0261(3) 0.8609(2) 0.0128(6) Uani 1 1 d . . .
O5 O -0.0098(4) 0.2535(3) 0.5742(2) 0.0178(6) Uani 1 1 d . . .
O6 O -0.2655(3) 0.3597(3) 0.4863(2) 0.0136(6) Uani 1 1 d . . .
C5 C -0.1915(5) 0.4370(5) 0.6473(3) 0.0162(8) Uani 1 1 d . . .
H5A H -0.1953 0.3601 0.7204 0.019 Uiso 1 1 calc R . .
H5B H -0.0862 0.5078 0.6450 0.019 Uiso 1 1 calc R . .
C6 C -0.1548(5) 0.3428(4) 0.5630(3) 0.0108(5) Uani 1 1 d U . .
N2 N -0.3676(4) 0.5374(4) 0.6317(2) 0.0112(7) Uani 1 1 d . . .
H2A H -0.3421 0.6460 0.6189 0.013 Uiso 1 1 calc R . .
C7 C -0.5036(5) 0.4930(4) 0.7226(3) 0.0134(8) Uani 1 1 d . . .
H7A H -0.5833 0.5897 0.7265 0.016 Uiso 1 1 calc R . .
H7B H -0.4362 0.4546 0.7919 0.016 Uiso 1 1 calc R . .
C8 C -0.6256(5) 0.3619(4) 0.7089(3) 0.0102(8) Uani 1 1 d . . .
O7 O -0.6021(4) 0.3128(3) 0.6228(2) 0.0130(6) Uani 1 1 d . . .
O8 O -0.7420(4) 0.3013(3) 0.7809(2) 0.0167(6) Uani 1 1 d . . .
C9 C 0.5646(5) -0.0464(4) 0.5457(3) 0.0114(8) Uani 1 1 d . . .
O9 O 0.5102(4) -0.0598(3) 0.6410(2) 0.0163(6) Uani 1 1 d . . .
O10 O 0.7150(3) -0.1054(3) 0.5155(2) 0.0119(6) Uani 1 1 d . . .
O1W O 0.0429(4) -0.1387(3) 0.6246(2) 0.0165(6) Uani 1 1 d . . .
H1WA H 0.0717 -0.2201 0.6758 0.020 Uiso 1 1 d R . .
H1WB H -0.0737 -0.1472 0.6256 0.020 Uiso 1 1 d R . .
O2W' O -0.9892(15) 0.5071(12) 0.8766(9) 0.070(3) Uani 0.50 1 d P . .
O2W O -1.1001(14) 0.4449(12) 0.9068(6) 0.056(3) Uani 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
Nd1 O1 2.320(3) . ?
Nd1 O5 2.374(3) . ?
Nd1 O1W 2.465(3) . ?
Nd1 O9 2.489(3) . ?
Nd1 O7 2.519(3) 1_655 ?
Nd1 O4 2.521(2) 1_655 ?
Nd1 O10 2.532(3) 2_656 ?
Nd1 O3 2.592(2) 1_655 ?
Nd1 O8 2.662(3) 1_655 ?
Nd1 C4 2.906(4) 1_655 ?
Nd1 C8 2.957(4) 1_655 ?
Ni1 O2 2.030(3) . ?
Ni1 O2 2.030(3) 2_457 ?
Ni1 N1 2.041(3) . ?
Ni1 N1 2.041(3) 2_457 ?
Ni1 O4 2.068(3) 2_457 ?
Ni1 O4 2.068(3) . ?
Ni2 O6 2.039(3) . ?
Ni2 O6 2.039(3) 2_466 ?
Ni2 N2 2.062(3) 2_466 ?
Ni2 N2 2.062(3) . ?
Ni2 O7 2.071(2) 2_466 ?
Ni2 O7 2.071(2) . ?
O1 C2 1.246(5) . ?
O2 C2 1.248(5) . ?
C1 N1 1.476(5) . ?
C1 C2 1.505(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
N1 C3 1.464(5) . ?
N1 H1C 0.9300 . ?
C3 C4 1.513(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O3 1.231(5) . ?
C4 O4 1.275(5) . ?
C4 Nd1 2.906(4) 1_455 ?
O3 Nd1 2.592(2) 1_455 ?
O4 Nd1 2.521(2) 1_455 ?
O5 C6 1.244(4) . ?
O6 C6 1.254(4) . ?
C5 N2 1.475(5) . ?
C5 C6 1.511(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
N2 C7 1.469(5) . ?
N2 H2A 0.9300 . ?
C7 C8 1.512(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 O8 1.243(4) . ?
C8 O7 1.277(5) . ?
C8 Nd1 2.957(4) 1_455 ?
O7 Nd1 2.519(3) 1_455 ?
O8 Nd1 2.662(3) 1_455 ?
C9 O9 1.237(4) . ?
C9 O10 1.254(4) . ?
C9 C9 1.535(7) 2_656 ?
O10 Nd1 2.532(3) 2_656 ?
O1W H1WA 0.8420 . ?
O1W H1WB 0.8424 . ?
O2W' O2W 0.991(13) . ?

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 Nd1 O5 77.53(9) . . ?
O1 Nd1 O1W 85.07(10) . . ?
O5 Nd1 O1W 84.60(9) . . ?
O1 Nd1 O9 149.45(9) . . ?
O5 Nd1 O9 131.78(9) . . ?
O1W Nd1 O9 89.18(9) . . ?
O1 Nd1 O7 120.67(9) . 1_655 ?
O5 Nd1 O7 78.72(9) . 1_655 ?
O1W Nd1 O7 144.63(9) . 1_655 ?
O9 Nd1 O7 79.44(9) . 1_655 ?
O1 Nd1 O4 82.60(9) . 1_655 ?
O5 Nd1 O4 149.00(9) . 1_655 ?
O1W Nd1 O4 117.31(8) . 1_655 ?
O9 Nd1 O4 73.51(8) . 1_655 ?
O7 Nd1 O4 91.55(8) 1_655 1_655 ?
O1 Nd1 O10 140.67(9) . 2_656 ?
O5 Nd1 O10 68.53(9) . 2_656 ?
O1W Nd1 O10 72.81(9) . 2_656 ?
O9 Nd1 O10 63.99(8) . 2_656 ?
O7 Nd1 O10 72.10(8) 1_655 2_656 ?
O4 Nd1 O10 136.38(8) 1_655 2_656 ?
O1 Nd1 O3 82.56(9) . 1_655 ?
O5 Nd1 O3 146.51(9) . 1_655 ?
O1W Nd1 O3 66.95(9) . 1_655 ?
O9 Nd1 O3 67.64(8) . 1_655 ?
O7 Nd1 O3 134.77(8) 1_655 1_655 ?
O4 Nd1 O3 50.58(8) 1_655 1_655 ?
O10 Nd1 O3 115.88(8) 2_656 1_655 ?
O1 Nd1 O8 74.63(9) . 1_655 ?
O5 Nd1 O8 85.83(9) . 1_655 ?
O1W Nd1 O8 159.01(9) . 1_655 ?
O9 Nd1 O8 111.02(9) . 1_655 ?
O7 Nd1 O8 50.04(8) 1_655 1_655 ?
O4 Nd1 O8 65.94(8) 1_655 1_655 ?
O10 Nd1 O8 120.45(8) 2_656 1_655 ?
O3 Nd1 O8 114.53(8) 1_655 1_655 ?
O1 Nd1 C4 85.19(10) . 1_655 ?
O5 Nd1 C4 162.61(10) . 1_655 ?
O1W Nd1 C4 91.98(10) . 1_655 ?
O9 Nd1 C4 65.02(9) . 1_655 ?
O7 Nd1 C4 112.51(10) 1_655 1_655 ?
O4 Nd1 C4 25.96(10) 1_655 1_655 ?
O10 Nd1 C4 126.66(9) 2_656 1_655 ?
O3 Nd1 C4 25.05(10) 1_655 1_655 ?
O8 Nd1 C4 91.59(10) 1_655 1_655 ?
O1 Nd1 C8 98.41(10) . 1_655 ?
O5 Nd1 C8 83.82(10) . 1_655 ?
O1W Nd1 C8 166.87(9) . 1_655 ?
O9 Nd1 C8 93.95(9) . 1_655 ?
O7 Nd1 C8 25.38(9) 1_655 1_655 ?
O4 Nd1 C8 75.77(9) 1_655 1_655 ?
O10 Nd1 C8 97.14(9) 2_656 1_655 ?
O3 Nd1 C8 125.95(9) 1_655 1_655 ?
O8 Nd1 C8 24.86(9) 1_655 1_655 ?
C4 Nd1 C8 100.90(10) 1_655 1_655 ?
O2 Ni1 O2 180.0 . 2_457 ?
O2 Ni1 N1 84.59(11) . . ?
O2 Ni1 N1 95.41(11) 2_457 . ?
O2 Ni1 N1 95.41(11) . 2_457 ?
O2 Ni1 N1 84.59(11) 2_457 2_457 ?
N1 Ni1 N1 180.00(16) . 2_457 ?
O2 Ni1 O4 91.05(10) . 2_457 ?
O2 Ni1 O4 88.95(10) 2_457 2_457 ?
N1 Ni1 O4 99.64(11) . 2_457 ?
N1 Ni1 O4 80.36(11) 2_457 2_457 ?
O2 Ni1 O4 88.95(10) . . ?
O2 Ni1 O4 91.05(10) 2_457 . ?
N1 Ni1 O4 80.36(11) . . ?
N1 Ni1 O4 99.64(11) 2_457 . ?
O4 Ni1 O4 180.000(1) 2_457 . ?
O6 Ni2 O6 180.000(1) . 2_466 ?
O6 Ni2 N2 95.96(11) . 2_466 ?
O6 Ni2 N2 84.04(11) 2_466 2_466 ?
O6 Ni2 N2 84.04(11) . . ?
O6 Ni2 N2 95.96(11) 2_466 . ?
N2 Ni2 N2 180.000(1) 2_466 . ?
O6 Ni2 O7 90.16(10) . 2_466 ?
O6 Ni2 O7 89.84(10) 2_466 2_466 ?
N2 Ni2 O7 79.96(11) 2_466 2_466 ?
N2 Ni2 O7 100.04(11) . 2_466 ?
O6 Ni2 O7 89.84(10) . . ?
O6 Ni2 O7 90.16(10) 2_466 . ?
N2 Ni2 O7 100.04(11) 2_466 . ?
N2 Ni2 O7 79.96(11) . . ?
O7 Ni2 O7 180.00(11) 2_466 . ?
C2 O1 Nd1 162.4(3) . . ?
C2 O2 Ni1 113.1(2) . . ?
N1 C1 C2 113.7(3) . . ?
N1 C1 H1A 108.8 . . ?
C2 C1 H1A 108.8 . . ?
N1 C1 H1B 108.8 . . ?
C2 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
O1 C2 O2 123.7(4) . . ?
O1 C2 C1 116.3(4) . . ?
O2 C2 C1 120.0(3) . . ?
C3 N1 C1 114.1(3) . . ?
C3 N1 Ni1 104.3(2) . . ?
C1 N1 Ni1 108.0(2) . . ?
C3 N1 H1C 110.1 . . ?
C1 N1 H1C 110.1 . . ?
Ni1 N1 H1C 110.1 . . ?
N1 C3 C4 111.6(3) . . ?
N1 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
N1 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
O3 C4 O4 121.4(3) . . ?
O3 C4 C3 121.5(3) . . ?
O4 C4 C3 117.1(3) . . ?
O3 C4 Nd1 63.08(19) . 1_455 ?
O4 C4 Nd1 59.91(18) . 1_455 ?
C3 C4 Nd1 165.5(3) . 1_455 ?
C4 O3 Nd1 91.9(2) . 1_455 ?
C4 O4 Ni1 109.7(2) . . ?
C4 O4 Nd1 94.1(2) . 1_455 ?
Ni1 O4 Nd1 155.75(12) . 1_455 ?
C6 O5 Nd1 151.3(2) . . ?
C6 O6 Ni2 113.5(2) . . ?
N2 C5 C6 113.6(3) . . ?
N2 C5 H5A 108.8 . . ?
C6 C5 H5A 108.8 . . ?
N2 C5 H5B 108.8 . . ?
C6 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
O5 C6 O6 124.0(3) . . ?
O5 C6 C5 115.9(3) . . ?
O6 C6 C5 120.1(3) . . ?
C7 N2 C5 114.1(3) . . ?
C7 N2 Ni2 104.6(2) . . ?
C5 N2 Ni2 108.3(2) . . ?
C7 N2 H2A 109.9 . . ?
C5 N2 H2A 109.9 . . ?
Ni2 N2 H2A 109.9 . . ?
N2 C7 C8 111.2(3) . . ?
N2 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
N2 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
O8 C8 O7 121.2(3) . . ?
O8 C8 C7 120.8(3) . . ?
O7 C8 C7 118.0(3) . . ?
O8 C8 Nd1 64.2(2) . 1_455 ?
O7 C8 Nd1 57.74(17) . 1_455 ?
C7 C8 Nd1 168.7(2) . 1_455 ?
C8 O7 Ni2 108.2(2) . . ?
C8 O7 Nd1 96.9(2) . 1_455 ?
Ni2 O7 Nd1 150.62(13) . 1_455 ?
C8 O8 Nd1 91.0(2) . 1_455 ?
O9 C9 O10 126.2(3) . . ?
O9 C9 C9 118.0(4) . 2_656 ?
O10 C9 C9 115.7(4) . 2_656 ?
C9 O9 Nd1 121.6(2) . . ?
C9 O10 Nd1 120.7(2) . 2_656 ?
Nd1 O1W H1WA 98.9 . . ?
Nd1 O1W H1WB 125.9 . . ?
H1WA O1W H1WB 99.4 . . ?

_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.959
_refine_diff_density_max         2.287
_refine_diff_density_min         -1.882
_refine_diff_density_rms         0.216

# Attachment 'complex8.cif'

data_complex8
_database_code_depnum_ccdc_archive 'CCDC 647838'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H28 Eu2 N4 Ni2 O24'
_chemical_formula_weight         1105.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   7.1243(19)
_cell_length_b                   8.578(2)
_cell_length_c                   12.695(3)
_cell_angle_alpha                74.769(4)
_cell_angle_beta                 87.335(5)
_cell_angle_gamma                86.314(5)
_cell_volume                     746.7(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3448
_cell_measurement_theta_min      2.590
_cell_measurement_theta_max      28.382

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             538
_exptl_absorpt_coefficient_mu    5.494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4380
_exptl_absorpt_correction_T_max  0.7707
_exptl_absorpt_process_details   sadabs

_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_%        ?
_diffrn_reflns_number            3774
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2805
_reflns_number_gt                2710
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_cell_refinement       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0548P)²+1.5040P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2805
_refine_ls_number_parameters     238
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.1169
_refine_ls_wR_factor_gt          0.1157
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.022
_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
Eu1 Eu 0.20705(3) 0.06775(2) 0.684172(15) 0.01376(6) Uani 1 1 d . . .
Ni1 Ni -0.5000 0.0000 1.0000 0.01517(18) Uani 1 2 d S . .
Ni2 Ni -0.5000 0.5000 0.5000 0.01575(18) Uani 1 2 d S . .
O1 O -0.0423(5) 0.0682(5) 0.8033(3) 0.0356(10) Uani 1 1 d . . .
O2 O -0.2825(5) 0.1130(4) 0.9079(3) 0.0252(8) Uani 1 1 d . . .
C1 C -0.1947(8) -0.1587(6) 0.9085(5) 0.0352(15) Uani 1 1 d . . .
H1A H -0.2055 -0.1997 0.8449 0.042 Uiso 1 1 calc R . .
H1B H -0.0816 -0.2096 0.9454 0.042 Uiso 1 1 calc R . .
C2 C -0.1735(7) 0.0204(6) 0.8713(4) 0.0231(11) Uani 1 1 d . . .
N1 N -0.3571(6) -0.2056(5) 0.9820(3) 0.0197(9) Uani 1 1 d . . .
H1C H -0.3184 -0.2673 1.0480 0.024 Uiso 1 1 calc R . .
C3 C -0.4955(8) -0.2883(6) 0.9396(4) 0.0244(12) Uani 1 1 d . . .
H3A H -0.5695 -0.3516 1.0000 0.029 Uiso 1 1 calc R . .
H3B H -0.4312 -0.3622 0.9020 0.029 Uiso 1 1 calc R . .
C4 C -0.6251(7) -0.1718(5) 0.8619(4) 0.0225(11) Uani 1 1 d . . .
O3 O -0.7329(5) -0.2207(4) 0.8065(3) 0.0277(9) Uani 1 1 d . . .
O4 O -0.6177(5) -0.0236(4) 0.8582(2) 0.0210(8) Uani 1 1 d . . .
O5 O -0.0115(5) 0.2450(5) 0.5761(3) 0.0320(10) Uani 1 1 d . . .
O6 O -0.2651(5) 0.3558(4) 0.4866(3) 0.0244(8) Uani 1 1 d . . .
C5 C -0.1907(7) 0.4344(6) 0.6468(4) 0.0270(12) Uani 1 1 d . . .
H5A H -0.1906 0.3613 0.7194 0.032 Uiso 1 1 calc R . .
H5B H -0.0877 0.5051 0.6412 0.032 Uiso 1 1 calc R . .
C6 C -0.1557(7) 0.3370(6) 0.5647(4) 0.0216(11) Uani 1 1 d . . .
N2 N -0.3691(6) 0.5335(4) 0.6335(3) 0.0183(9) Uani 1 1 d . . .
H2A H -0.3450 0.6397 0.6218 0.022 Uiso 1 1 calc R . .
C7 C -0.5073(7) 0.4890(6) 0.7233(4) 0.0245(12) Uani 1 1 d . . .
H7A H -0.5864 0.5839 0.7271 0.029 Uiso 1 1 calc R . .
H7B H -0.4425 0.4508 0.7916 0.029 Uiso 1 1 calc R . .
C8 C -0.6274(7) 0.3608(6) 0.7093(4) 0.0211(11) Uani 1 1 d . . .
O7 O -0.6075(5) 0.3126(4) 0.6227(3) 0.0222(8) Uani 1 1 d . . .
O8 O -0.7461(5) 0.3008(4) 0.7813(3) 0.0304(10) Uani 1 1 d . . .
C9 C 0.5654(7) -0.0460(5) 0.5455(3) 0.0177(11) Uani 1 1 d . . .
O9 O 0.5096(5) -0.0549(5) 0.6407(3) 0.0319(10) Uani 1 1 d . . .
O10 O 0.7160(5) -0.1052(4) 0.5158(3) 0.0216(8) Uani 1 1 d . . .
O1W O 0.0435(5) -0.1314(4) 0.6243(3) 0.0291(9) Uani 1 1 d . . .
H1WA H 0.0723 -0.2128 0.6754 0.035 Uiso 1 1 d R . .
H1WB H -0.0732 -0.1400 0.6253 0.035 Uiso 1 1 d R . .
O2W O -1.0994(19) 0.4258(17) 0.9106(8) 0.080(4) Uani 0.50 1 d P . .
O2W' O -1.021(3) 0.4920(18) 0.8854(13) 0.138(7) Uani 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 O1 2.279(4) . ?
Eu1 O5 2.327(3) . ?
Eu1 O1W 2.424(4) . ?
Eu1 O9 2.441(4) . ?
Eu1 O7 2.483(3) 1_655 ?
Eu1 O4 2.505(3) 1_655 ?
Eu1 O10 2.513(3) 2_656 ?
Eu1 O3 2.574(3) 1_655 ?
Eu1 O8 2.655(4) 1_655 ?
Eu1 C4 2.871(4) 1_655 ?
Eu1 C8 2.941(5) 1_655 ?
Eu1 H1WA 2.6785 . ?
Ni1 O2 2.034(3) 2_457 ?
Ni1 O2 2.034(3) . ?
Ni1 N1 2.039(4) . ?
Ni1 N1 2.039(4) 2_457 ?
Ni1 O4 2.083(3) 2_457 ?
Ni1 O4 2.083(3) . ?
Ni2 O6 2.044(3) . ?
Ni2 O6 2.044(3) 2_466 ?
Ni2 N2 2.065(4) . ?
Ni2 N2 2.065(4) 2_466 ?
Ni2 O7 2.081(3) . ?
Ni2 O7 2.081(3) 2_466 ?
O1 C2 1.255(6) . ?
O2 C2 1.237(6) . ?
C1 N1 1.460(6) . ?
C1 C2 1.500(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
N1 C3 1.451(7) . ?
N1 H1C 0.9100 . ?
C3 C4 1.508(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 O3 1.227(6) . ?
C4 O4 1.264(6) . ?
C4 Eu1 2.871(4) 1_455 ?
O3 Eu1 2.574(3) 1_455 ?
O4 Eu1 2.505(3) 1_455 ?
O5 C6 1.245(6) . ?
O6 C6 1.260(6) . ?
C5 N2 1.474(6) . ?
C5 C6 1.500(7) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
N2 C7 1.459(6) . ?
N2 H2A 0.9100 . ?
C7 C8 1.487(7) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O8 1.246(6) . ?
C8 O7 1.271(6) . ?
C8 Eu1 2.941(5) 1_455 ?
O7 Eu1 2.483(3) 1_455 ?
O8 Eu1 2.655(4) 1_455 ?
C9 O9 1.240(6) . ?
C9 O10 1.242(6) . ?
C9 C9 1.534(9) 2_656 ?
O10 Eu1 2.513(3) 2_656 ?
O1W H1WA 0.8409 . ?
O1W H1WB 0.8383 . ?
O2W O2W' 0.81(2) . ?

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 O5 77.72(13) . . ?
O1 Eu1 O1W 85.75(14) . . ?
O5 Eu1 O1W 82.27(13) . . ?
O1 Eu1 O9 148.95(12) . . ?
O5 Eu1 O9 132.28(12) . . ?
O1W Eu1 O9 90.40(14) . . ?
O1 Eu1 O7 119.29(13) . 1_655 ?
O5 Eu1 O7 79.74(13) . 1_655 ?
O1W Eu1 O7 144.66(12) . 1_655 ?
O9 Eu1 O7 79.84(12) . 1_655 ?
O1 Eu1 O4 81.86(13) . 1_655 ?
O5 Eu1 O4 149.83(12) . 1_655 ?
O1W Eu1 O4 118.25(11) . 1_655 ?
O9 Eu1 O4 72.92(11) . 1_655 ?
O7 Eu1 O4 91.37(11) 1_655 1_655 ?
O1 Eu1 O10 141.40(13) . 2_656 ?
O5 Eu1 O10 68.35(11) . 2_656 ?
O1W Eu1 O10 72.29(12) . 2_656 ?
O9 Eu1 O10 64.53(11) . 2_656 ?
O7 Eu1 O10 72.85(11) 1_655 2_656 ?
O4 Eu1 O10 136.43(11) 1_655 2_656 ?
O1 Eu1 O3 82.32(12) . 1_655 ?
O5 Eu1 O3 144.83(13) . 1_655 ?
O1W Eu1 O3 67.53(12) . 1_655 ?
O9 Eu1 O3 67.83(12) . 1_655 ?
O7 Eu1 O3 135.43(11) 1_655 1_655 ?
O4 Eu1 O3 50.95(11) 1_655 1_655 ?
O10 Eu1 O3 115.76(11) 2_656 1_655 ?
O1 Eu1 O8 73.01(13) . 1_655 ?
O5 Eu1 O8 87.01(13) . 1_655 ?
O1W Eu1 O8 157.85(13) . 1_655 ?
O9 Eu1 O8 111.02(13) . 1_655 ?
O7 Eu1 O8 50.13(11) 1_655 1_655 ?
O4 Eu1 O8 65.75(11) 1_655 1_655 ?
O10 Eu1 O8 121.30(11) 2_656 1_655 ?
O3 Eu1 O8 114.42(11) 1_655 1_655 ?
O1 Eu1 C4 84.74(14) . 1_655 ?
O5 Eu1 C4 162.06(13) . 1_655 ?
O1W Eu1 C4 92.82(13) . 1_655 ?
O9 Eu1 C4 64.66(13) . 1_655 ?
O7 Eu1 C4 112.69(13) 1_655 1_655 ?
O4 Eu1 C4 26.09(13) 1_655 1_655 ?
O10 Eu1 C4 126.62(12) 2_656 1_655 ?
O3 Eu1 C4 25.31(13) 1_655 1_655 ?
O8 Eu1 C4 91.47(13) 1_655 1_655 ?
O1 Eu1 C8 97.16(14) . 1_655 ?
O5 Eu1 C8 85.52(14) . 1_655 ?
O1W Eu1 C8 166.56(12) . 1_655 ?
O9 Eu1 C8 93.67(14) . 1_655 ?
O7 Eu1 C8 25.35(12) 1_655 1_655 ?
O4 Eu1 C8 75.19(12) 1_655 1_655 ?
O10 Eu1 C8 97.95(12) 2_656 1_655 ?
O3 Eu1 C8 125.81(12) 1_655 1_655 ?
O8 Eu1 C8 25.07(12) 1_655 1_655 ?
C4 Eu1 C8 100.50(14) 1_655 1_655 ?
O1 Eu1 H1WA 82.6 . . ?
O5 Eu1 H1WA 99.0 . . ?
O1W Eu1 H1WA 18.1 . . ?
O9 Eu1 H1WA 84.3 . . ?
O7 Eu1 H1WA 156.7 1_655 . ?
O4 Eu1 H1WA 100.2 1_655 . ?
O10 Eu1 H1WA 85.0 2_656 . ?
O3 Eu1 H1WA 49.5 1_655 . ?
O8 Eu1 H1WA 153.1 1_655 . ?
C4 Eu1 H1WA 74.8 1_655 . ?
C8 Eu1 H1WA 175.3 1_655 . ?
O2 Ni1 O2 180.00(13) 2_457 . ?
O2 Ni1 N1 96.02(14) 2_457 . ?
O2 Ni1 N1 83.98(14) . . ?
O2 Ni1 N1 83.98(14) 2_457 2_457 ?
O2 Ni1 N1 96.02(14) . 2_457 ?
N1 Ni1 N1 180.000(1) . 2_457 ?
O2 Ni1 O4 89.25(14) 2_457 2_457 ?
O2 Ni1 O4 90.75(14) . 2_457 ?
N1 Ni1 O4 100.40(14) . 2_457 ?
N1 Ni1 O4 79.60(14) 2_457 2_457 ?
O2 Ni1 O4 90.75(14) 2_457 . ?
O2 Ni1 O4 89.25(14) . . ?
N1 Ni1 O4 79.60(14) . . ?
N1 Ni1 O4 100.40(14) 2_457 . ?
O4 Ni1 O4 180.000(1) 2_457 . ?
O6 Ni2 O6 180.00(18) . 2_466 ?
O6 Ni2 N2 84.11(14) . . ?
O6 Ni2 N2 95.89(14) 2_466 . ?
O6 Ni2 N2 95.89(14) . 2_466 ?
O6 Ni2 N2 84.11(14) 2_466 2_466 ?
N2 Ni2 N2 180.000(1) . 2_466 ?
O6 Ni2 O7 89.70(13) . . ?
O6 Ni2 O7 90.30(13) 2_466 . ?
N2 Ni2 O7 79.79(14) . . ?
N2 Ni2 O7 100.21(14) 2_466 . ?
O6 Ni2 O7 90.30(13) . 2_466 ?
O6 Ni2 O7 89.70(13) 2_466 2_466 ?
N2 Ni2 O7 100.21(14) . 2_466 ?
N2 Ni2 O7 79.79(14) 2_466 2_466 ?
O7 Ni2 O7 180.00(14) . 2_466 ?
C2 O1 Eu1 161.5(4) . . ?
C2 O2 Ni1 113.3(3) . . ?
N1 C1 C2 114.1(4) . . ?
N1 C1 H1A 108.7 . . ?
C2 C1 H1A 108.7 . . ?
N1 C1 H1B 108.7 . . ?
C2 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
O2 C2 O1 123.3(5) . . ?
O2 C2 C1 119.9(4) . . ?
O1 C2 C1 116.8(5) . . ?
C3 N1 C1 114.3(4) . . ?
C3 N1 Ni1 103.9(3) . . ?
C1 N1 Ni1 108.2(3) . . ?
C3 N1 H1C 110.1 . . ?
C1 N1 H1C 110.1 . . ?
Ni1 N1 H1C 110.1 . . ?
N1 C3 C4 112.1(4) . . ?
N1 C3 H3A 109.2 . . ?
C4 C3 H3A 109.2 . . ?
N1 C3 H3B 109.2 . . ?
C4 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
O3 C4 O4 122.6(4) . . ?
O3 C4 C3 120.9(4) . . ?
O4 C4 C3 116.6(4) . . ?
O3 C4 Eu1 63.7(2) . 1_455 ?
O4 C4 Eu1 60.6(2) . 1_455 ?
C3 C4 Eu1 166.7(3) . 1_455 ?
C4 O3 Eu1 91.0(3) . 1_455 ?
C4 O4 Ni1 109.7(3) . . ?
C4 O4 Eu1 93.3(3) . 1_455 ?
Ni1 O4 Eu1 156.30(16) . 1_455 ?
C6 O5 Eu1 151.8(3) . . ?
C6 O6 Ni2 113.1(3) . . ?
N2 C5 C6 114.2(4) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
O5 C6 O6 123.3(5) . . ?
O5 C6 C5 116.5(4) . . ?
O6 C6 C5 120.1(4) . . ?
C7 N2 C5 115.5(4) . . ?
C7 N2 Ni2 104.4(3) . . ?
C5 N2 Ni2 108.0(3) . . ?
C7 N2 H2A 109.6 . . ?
C5 N2 H2A 109.6 . . ?
Ni2 N2 H2A 109.6 . . ?
N2 C7 C8 111.7(4) . . ?
N2 C7 H7A 109.3 . . ?
C8 C7 H7A 109.3 . . ?
N2 C7 H7B 109.3 . . ?
C8 C7 H7B 109.3 . . ?
H7A C7 H7B 107.9 . . ?
O8 C8 O7 120.1(5) . . ?
O8 C8 C7 120.7(5) . . ?
O7 C8 C7 119.2(4) . . ?
O8 C8 Eu1 64.5(3) . 1_455 ?
O7 C8 Eu1 56.7(2) . 1_455 ?
C7 C8 Eu1 168.4(3) . 1_455 ?
C8 O7 Ni2 107.7(3) . . ?
C8 O7 Eu1 97.9(3) . 1_455 ?
Ni2 O7 Eu1 151.31(17) . 1_455 ?
C8 O8 Eu1 90.4(3) . 1_455 ?
O9 C9 O10 126.8(4) . . ?
O9 C9 C9 116.9(5) . 2_656 ?
O10 C9 C9 116.4(5) . 2_656 ?
C9 O9 Eu1 122.3(3) . . ?
C9 O10 Eu1 119.9(3) . 2_656 ?
Eu1 O1W H1WA 98.3 . . ?
Eu1 O1W H1WB 126.8 . . ?
H1WA O1W H1WB 99.3 . . ?

_diffrn_measured_fraction_theta_max 0.954
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.954
_refine_diff_density_max         2.916
_refine_diff_density_min         -2.470
_refine_diff_density_rms         0.227

# Attachment 'complex9.cif'

data_complex9
_database_code_depnum_ccdc_archive 'CCDC 647839'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H18 Dy2 N2 Ni O20'
_chemical_formula_weight         893.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 '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                   7.4026(18)
_cell_length_b                   8.224(2)
_cell_length_c                   9.822(2)
_cell_angle_alpha                81.482(4)
_cell_angle_beta                 81.709(4)
_cell_angle_gamma                83.254(4)
_cell_volume                     582.3(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3423
_cell_measurement_theta_min      2.517
_cell_measurement_theta_max      28.375

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             424
_exptl_absorpt_coefficient_mu    7.248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4302
_exptl_absorpt_correction_T_max  0.6703
_exptl_absorpt_process_details   sadabs

_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_%        ?
_diffrn_reflns_number            4515
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.11
_diffrn_reflns_theta_max         25.99
_reflns_number_total             2237
_reflns_number_gt                2189
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_cell_refinement       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0555P)²+1.5124P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2237
_refine_ls_number_parameters     169
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.0915
_refine_ls_wR_factor_gt          0.0905
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.003

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
Dy1 Dy 0.32211(4) 0.39534(3) 0.78976(3) 0.01792(13) Uani 1 1 d . . .
Ni1 Ni 0.0000 0.0000 1.0000 0.0188(3) Uani 1 2 d S . .
O1 O 0.1418(7) 0.1586(6) 0.8569(5) 0.0285(11) Uani 1 1 d . . .
O2 O 0.2286(9) 0.2208(9) 0.6389(6) 0.0514(18) Uani 1 1 d . . .
C1 C 0.0435(13) -0.0021(13) 0.7071(9) 0.048(2) Uani 1 1 d . . .
H1A H -0.0188 0.0363 0.6262 0.057 Uiso 1 1 calc R . .
H1B H 0.1301 -0.0959 0.6862 0.057 Uiso 1 1 calc R . .
C2 C 0.1453(11) 0.1325(10) 0.7357(8) 0.0312(17) Uani 1 1 d . . .
N1 N -0.0895(7) -0.0540(7) 0.8235(6) 0.0209(11) Uani 1 1 d . . .
H1C H -0.0929 -0.1652 0.8303 0.025 Uiso 1 1 calc R . .
C3 C -0.2733(11) 0.0261(11) 0.8177(10) 0.044(2) Uani 1 1 d . . .
H3A H -0.3591 -0.0575 0.8382 0.052 Uiso 1 1 calc R . .
H3B H -0.2827 0.0803 0.7240 0.052 Uiso 1 1 calc R . .
C4 C -0.3270(10) 0.1489(9) 0.9146(7) 0.0280(15) Uani 1 1 d . . .
O3 O -0.4796(7) 0.2289(8) 0.9119(6) 0.0406(14) Uani 1 1 d . . .
O4 O -0.2229(7) 0.1655(7) 0.9996(5) 0.0327(12) Uani 1 1 d . . .
C5 C 0.0542(9) 0.4618(8) 1.0594(7) 0.0216(14) Uani 1 1 d . . .
O5 O 0.2106(6) 0.4006(6) 1.0281(5) 0.0262(11) Uani 1 1 d . . .
O6 O -0.0288(6) 0.4645(7) 1.1787(5) 0.0290(11) Uani 1 1 d . . .
C6 C 0.4156(9) 0.5588(8) 0.4860(7) 0.0227(14) Uani 1 1 d . . .
O7 O 0.2905(7) 0.5680(7) 0.5834(5) 0.0334(13) Uani 1 1 d . . .
O8 O 0.4174(7) 0.6375(6) 0.3668(5) 0.0293(11) Uani 1 1 d . . .
O1W O 0.4576(9) 0.6195(8) 0.8269(6) 0.0446(15) Uani 1 1 d . . .
H1WB H 0.5040 0.6679 0.7494 0.067 Uiso 1 1 d R . .
H1WA H 0.3767 0.6858 0.8660 0.067 Uiso 1 1 d R . .
O2W O 0.7656(9) 0.7102(8) 0.6526(6) 0.0495(16) Uani 1 1 d . . .
H2WA H 0.7611 0.7774 0.5783 0.074 Uiso 1 1 d R . .
H2WB H 0.8269 0.6206 0.6332 0.074 Uiso 1 1 d R . .


_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
Dy1 O3 2.240(5) 1_655 ?
Dy1 O1W 2.297(5) . ?
Dy1 O8 2.302(5) 2_666 ?
Dy1 O7 2.320(5) . ?
Dy1 O6 2.337(5) 2_567 ?
Dy1 O5 2.372(5) . ?
Dy1 O2 2.428(6) . ?
Dy1 O1 2.446(5) . ?
Dy1 C2 2.806(7) . ?
Ni1 O4 2.012(5) 2_557 ?
Ni1 O4 2.012(5) . ?
Ni1 O1 2.033(5) 2_557 ?
Ni1 O1 2.033(5) . ?
Ni1 N1 2.067(6) . ?
Ni1 N1 2.067(6) 2_557 ?
O1 C2 1.236(9) . ?
O2 C2 1.243(9) . ?
C1 N1 1.445(9) . ?
C1 C2 1.490(11) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
N1 C3 1.446(9) . ?
N1 H1C 0.9100 . ?
C3 C4 1.471(11) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 O3 1.240(9) . ?
C4 O4 1.246(9) . ?
O3 Dy1 2.240(5) 1_455 ?
C5 O5 1.223(8) . ?
C5 O6 1.244(8) . ?
C5 C5 1.528(12) 2_567 ?
O6 Dy1 2.337(5) 2_567 ?
C6 O7 1.236(8) . ?
C6 O8 1.251(8) . ?
C6 C6 1.519(13) 2_666 ?
O8 Dy1 2.302(5) 2_666 ?
O1W H1WB 0.8500 . ?
O1W H1WA 0.8501 . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8500 . ?

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 Dy1 O1W 89.5(2) 1_655 . ?
O3 Dy1 O8 75.73(18) 1_655 2_666 ?
O1W Dy1 O8 82.3(2) . 2_666 ?
O3 Dy1 O7 144.71(18) 1_655 . ?
O1W Dy1 O7 79.4(2) . . ?
O8 Dy1 O7 69.66(17) 2_666 . ?
O3 Dy1 O6 140.06(18) 1_655 2_567 ?
O1W Dy1 O6 92.1(2) . 2_567 ?
O8 Dy1 O6 143.96(17) 2_666 2_567 ?
O7 Dy1 O6 74.31(17) . 2_567 ?
O3 Dy1 O5 72.88(17) 1_655 . ?
O1W Dy1 O5 80.8(2) . . ?
O8 Dy1 O5 144.30(17) 2_666 . ?
O7 Dy1 O5 136.42(17) . . ?
O6 Dy1 O5 68.02(16) 2_567 . ?
O3 Dy1 O2 104.4(3) 1_655 . ?
O1W Dy1 O2 152.2(2) . . ?
O8 Dy1 O2 78.1(2) 2_666 . ?
O7 Dy1 O2 75.4(2) . . ?
O6 Dy1 O2 92.3(2) 2_567 . ?
O5 Dy1 O2 126.05(18) . . ?
O3 Dy1 O1 81.5(2) 1_655 . ?
O1W Dy1 O1 155.3(2) . . ?
O8 Dy1 O1 117.08(18) 2_666 . ?
O7 Dy1 O1 120.33(19) . . ?
O6 Dy1 O1 80.63(19) 2_567 . ?
O5 Dy1 O1 74.59(17) . . ?
O2 Dy1 O1 52.30(18) . . ?
O3 Dy1 C2 93.4(2) 1_655 . ?
O1W Dy1 C2 177.1(2) . . ?
O8 Dy1 C2 98.2(2) 2_666 . ?
O7 Dy1 C2 98.0(2) . . ?
O6 Dy1 C2 85.8(2) 2_567 . ?
O5 Dy1 C2 100.3(2) . . ?
O2 Dy1 C2 26.2(2) . . ?
O1 Dy1 C2 26.08(19) . . ?
O4 Ni1 O4 180.000(1) 2_557 . ?
O4 Ni1 O1 89.8(2) 2_557 2_557 ?
O4 Ni1 O1 90.2(2) . 2_557 ?
O4 Ni1 O1 90.2(2) 2_557 . ?
O4 Ni1 O1 89.8(2) . . ?
O1 Ni1 O1 180.0 2_557 . ?
O4 Ni1 N1 97.5(2) 2_557 . ?
O4 Ni1 N1 82.5(2) . . ?
O1 Ni1 N1 98.7(2) 2_557 . ?
O1 Ni1 N1 81.3(2) . . ?
O4 Ni1 N1 82.5(2) 2_557 2_557 ?
O4 Ni1 N1 97.5(2) . 2_557 ?
O1 Ni1 N1 81.3(2) 2_557 2_557 ?
O1 Ni1 N1 98.7(2) . 2_557 ?
N1 Ni1 N1 180.000(1) . 2_557 ?
C2 O1 Ni1 114.1(5) . . ?
C2 O1 Dy1 93.4(4) . . ?
Ni1 O1 Dy1 152.4(2) . . ?
C2 O2 Dy1 94.1(5) . . ?
N1 C1 C2 111.9(6) . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
O1 C2 O2 120.1(7) . . ?
O1 C2 C1 119.3(7) . . ?
O2 C2 C1 120.6(7) . . ?
O1 C2 Dy1 60.5(4) . . ?
O2 C2 Dy1 59.6(4) . . ?
C1 C2 Dy1 177.4(6) . . ?
C1 N1 C3 115.1(7) . . ?
C1 N1 Ni1 107.2(5) . . ?
C3 N1 Ni1 107.7(4) . . ?
C1 N1 H1C 108.9 . . ?
C3 N1 H1C 108.9 . . ?
Ni1 N1 H1C 108.9 . . ?
N1 C3 C4 113.9(6) . . ?
N1 C3 H3A 108.8 . . ?
C4 C3 H3A 108.8 . . ?
N1 C3 H3B 108.8 . . ?
C4 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
O3 C4 O4 122.0(7) . . ?
O3 C4 C3 118.1(7) . . ?
O4 C4 C3 119.9(6) . . ?
C4 O3 Dy1 148.7(5) . 1_455 ?
C4 O4 Ni1 114.1(5) . . ?
O5 C5 O6 126.7(6) . . ?
O5 C5 C5 117.2(7) . 2_567 ?
O6 C5 C5 116.0(7) . 2_567 ?
C5 O5 Dy1 118.7(4) . . ?
C5 O6 Dy1 119.7(4) . 2_567 ?
O7 C6 O8 126.4(6) . . ?
O7 C6 C6 116.9(7) . 2_666 ?
O8 C6 C6 116.7(7) . 2_666 ?
C6 O7 Dy1 118.2(4) . . ?
C6 O8 Dy1 118.4(4) . 2_666 ?
Dy1 O1W H1WB 109.3 . . ?
Dy1 O1W H1WA 109.1 . . ?
H1WB O1W H1WA 109.5 . . ?
H2WA O2W H2WB 108.8 . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         1.899
_refine_diff_density_min         -1.435
_refine_diff_density_rms         0.196


