# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

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#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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data_NiDy

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H33 Dy Fe N6 Ni O13, C2 H3 N'
_chemical_formula_sum            'C34 H36 Dy Fe N7 Ni O13'
_chemical_formula_weight         1027.74

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'
Fe Fe 0.3463 0.8444 '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                   12.208(5)
_cell_length_b                   12.313(5)
_cell_length_c                   12.459(5)
_cell_angle_alpha                97.914(5)
_cell_angle_beta                 92.016(5)
_cell_angle_gamma                99.686(5)
_cell_volume                     1825.3(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2275
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      27.54

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.870
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1026
_exptl_absorpt_coefficient_mu    3.006
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9397
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.1016
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         25.50
_reflns_number_total             6577
_reflns_number_gt                4655
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0980P)²+1.2840P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6577
_refine_ls_number_parameters     522
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0688
_refine_ls_wR_factor_ref         0.1874
_refine_ls_wR_factor_gt          0.1598
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.012
_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
Dy1 Dy 0.73149(4) 0.40908(4) 0.25073(4) 0.02317(19) Uani 1 1 d . . .
Ni1 Ni 0.53699(10) 0.17819(11) 0.16395(10) 0.0184(3) Uani 1 1 d . . .
Fe1 Fe 0.10765(12) -0.14148(13) 0.16716(13) 0.0257(4) Uani 1 1 d . . .
O1 O 0.6849(5) 0.2197(5) 0.2565(6) 0.0192(16) Uani 1 1 d . . .
O2 O 0.8729(6) 0.3169(6) 0.3524(6) 0.0276(19) Uani 1 1 d . . .
O3 O 0.5876(6) 0.3325(6) 0.1236(6) 0.0229(16) Uani 1 1 d U . .
O4 O 0.7214(6) 0.5053(6) 0.0846(6) 0.032(2) Uani 1 1 d . . .
O5 O 0.4573(5) 0.2484(6) 0.2889(5) 0.0186(16) Uani 1 1 d . . .
O6 O 0.5792(6) 0.4042(6) 0.3525(6) 0.0269(18) Uani 1 1 d . . .
O7 O 0.8572(8) 0.3365(8) 0.1222(8) 0.048(3) Uani 1 1 d . . .
O8 O 0.9194(6) 0.4948(6) 0.2245(7) 0.035(2) Uani 1 1 d . . .
O9 O 1.0346(9) 0.4120(9) 0.1298(11) 0.074(4) Uani 1 1 d . . .
O10 O 0.8060(6) 0.5337(6) 0.4244(6) 0.0290(19) Uani 1 1 d . . .
O11 O 0.7366(6) 0.6086(6) 0.2987(7) 0.0268(18) Uani 1 1 d . . .
O12 O 0.8242(7) 0.7130(7) 0.4434(7) 0.043(2) Uani 1 1 d . . .
O13 O 0.6216(6) 0.1151(6) 0.0348(6) 0.0226(17) Uani 1 1 d D . .
H13 H 0.6009 0.0476 0.0208 0.034 Uiso 1 1 calc RD . .
N1 N 0.4138(7) -0.0525(7) 0.1978(7) 0.023(2) Uani 1 1 d . . .
N2 N 0.5173(7) 0.0245(7) 0.2203(7) 0.021(2) Uani 1 1 d . . .
N3 N 0.3033(7) 0.0774(7) 0.0427(7) 0.023(2) Uani 1 1 d . . .
N4 N 0.3983(6) 0.1651(7) 0.0531(7) 0.0193(19) Uani 1 1 d . . .
N5 N 0.9420(9) 0.4141(9) 0.1554(10) 0.048(3) Uani 1 1 d . . .
N6 N 0.7889(8) 0.6204(8) 0.3893(8) 0.030(2) Uani 1 1 d . . .
N7 N 0.5142(15) 0.2165(11) 0.5814(11) 0.071(4) Uani 1 1 d . . .
C1 C 0.2491(9) -0.1423(9) 0.2601(9) 0.024(2) Uani 1 1 d . . .
C2 C 0.1551(9) -0.1489(10) 0.3243(9) 0.031(3) Uani 1 1 d . . .
H2 H 0.1448 -0.0959 0.3879 0.038 Uiso 1 1 calc R . .
C3 C 0.0785(10) -0.2471(10) 0.2799(10) 0.036(3) Uani 1 1 d . . .
H3 H 0.0059 -0.2725 0.3076 0.043 Uiso 1 1 calc R . .
C4 C 0.1235(9) -0.3002(9) 0.1894(10) 0.029(3) Uani 1 1 d . . .
H4 H 0.0880 -0.3689 0.1431 0.035 Uiso 1 1 calc R . .
C5 C 0.2278(9) -0.2351(9) 0.1743(10) 0.026(3) Uani 1 1 d . . .
H5 H 0.2777 -0.2520 0.1168 0.032 Uiso 1 1 calc R . .
C6 C 0.3493(9) -0.0543(9) 0.2760(9) 0.024(2) Uani 1 1 d . . .
C7 C 0.3660(9) 0.0204(9) 0.3816(9) 0.031(3) Uani 1 1 d . . .
H7A H 0.3913 -0.0185 0.4367 0.047 Uiso 1 1 calc R . .
H7B H 0.2968 0.0431 0.4007 0.047 Uiso 1 1 calc R . .
H7C H 0.4205 0.0849 0.3758 0.047 Uiso 1 1 calc R . .
C8 C 0.5937(8) -0.0155(9) 0.2657(8) 0.021(2) Uani 1 1 d . . .
H8 H 0.5753 -0.0892 0.2775 0.025 Uiso 1 1 calc R . .
C9 C 0.7058(8) 0.0407(10) 0.3009(9) 0.025(3) Uani 1 1 d . . .
C10 C 0.7765(9) -0.0254(10) 0.3457(9) 0.030(3) Uani 1 1 d . . .
H10 H 0.7524 -0.1015 0.3440 0.036 Uiso 1 1 calc R . .
C11 C 0.8791(9) 0.0234(10) 0.3905(9) 0.031(3) Uani 1 1 d . . .
H11 H 0.9247 -0.0201 0.4193 0.037 Uiso 1 1 calc R . .
C12 C 0.9178(9) 0.1380(10) 0.3945(9) 0.031(3) Uani 1 1 d . . .
H12 H 0.9885 0.1704 0.4246 0.037 Uiso 1 1 calc R . .
C13 C 0.8475(9) 0.2021(9) 0.3519(9) 0.027(3) Uani 1 1 d . . .
C14 C 0.7430(8) 0.1563(8) 0.2986(9) 0.020(2) Uani 1 1 d . . .
C15 C 0.9766(10) 0.3718(11) 0.4100(11) 0.045(3) Uani 1 1 d U . .
H15A H 0.9761 0.3574 0.4838 0.068 Uiso 1 1 calc R . .
H15B H 0.9851 0.4505 0.4089 0.068 Uiso 1 1 calc R . .
H15C H 1.0374 0.3438 0.3756 0.068 Uiso 1 1 calc R . .
C16 C 0.7981(10) 0.6029(9) 0.0637(11) 0.035(3) Uani 1 1 d . . .
H16A H 0.8341 0.5850 -0.0021 0.053 Uiso 1 1 calc R . .
H16B H 0.8531 0.6260 0.1230 0.053 Uiso 1 1 calc R . .
H16C H 0.7577 0.6623 0.0562 0.053 Uiso 1 1 calc R . .
C17 C 0.6448(10) 0.4554(9) 0.0011(9) 0.029(3) Uani 1 1 d . . .
C18 C 0.6342(12) 0.4884(10) -0.0986(10) 0.041(3) Uani 1 1 d . . .
H18 H 0.6829 0.5501 -0.1142 0.049 Uiso 1 1 calc R . .
C19 C 0.5540(11) 0.4337(10) -0.1762(10) 0.035(3) Uani 1 1 d . . .
H19 H 0.5494 0.4568 -0.2440 0.042 Uiso 1 1 calc R . .
C20 C 0.4793(10) 0.3425(9) -0.1516(10) 0.031(3) Uani 1 1 d . . .
H20 H 0.4236 0.3054 -0.2030 0.037 Uiso 1 1 calc R . .
C21 C 0.4876(9) 0.3068(9) -0.0506(9) 0.025(2) Uani 1 1 d . . .
C22 C 0.5709(9) 0.3618(8) 0.0259(9) 0.020(2) Uani 1 1 d . . .
C23 C 0.4049(8) 0.2124(8) -0.0310(9) 0.021(2) Uani 1 1 d . . .
H23 H 0.3507 0.1838 -0.0867 0.025 Uiso 1 1 calc R . .
C24 C 0.2233(8) 0.0889(9) 0.1054(9) 0.022(2) Uani 1 1 d . . .
C25 C 0.2167(9) 0.1915(10) 0.1842(10) 0.031(3) Uani 1 1 d . . .
H25A H 0.2831 0.2455 0.1832 0.046 Uiso 1 1 calc R . .
H25B H 0.2094 0.1722 0.2560 0.046 Uiso 1 1 calc R . .
H25C H 0.1532 0.2224 0.1637 0.046 Uiso 1 1 calc R . .
C26 C 0.1252(9) -0.0017(9) 0.0929(9) 0.027(3) Uani 1 1 d . . .
C27 C 0.1069(9) -0.1010(10) 0.0146(9) 0.027(3) Uani 1 1 d . . .
H27 H 0.1571 -0.1211 -0.0416 0.032 Uiso 1 1 calc R . .
C28 C 0.0036(9) -0.1636(10) 0.0322(9) 0.029(3) Uani 1 1 d U . .
H28 H -0.0305 -0.2355 -0.0094 0.035 Uiso 1 1 calc R . .
C29 C -0.0418(9) -0.1069(10) 0.1203(11) 0.035(3) Uani 1 1 d . . .
H29 H -0.1130 -0.1327 0.1505 0.042 Uiso 1 1 calc R . .
C30 C 0.0328(10) -0.0061(11) 0.1593(11) 0.037(3) Uani 1 1 d . . .
H30 H 0.0222 0.0498 0.2203 0.045 Uiso 1 1 calc R . .
C31 C 0.4865(9) 0.3377(9) 0.3489(9) 0.023(2) Uani 1 1 d . . .
C32 C 0.3995(11) 0.3749(10) 0.4239(12) 0.046(4) Uani 1 1 d . . .
H32A H 0.3411 0.3955 0.3817 0.068 Uiso 1 1 calc R . .
H32B H 0.4337 0.4377 0.4755 0.068 Uiso 1 1 calc R . .
H32C H 0.3690 0.3148 0.4616 0.068 Uiso 1 1 calc R . .
C33 C 0.5992(17) 0.2726(12) 0.5775(12) 0.058(5) Uani 1 1 d . . .
C34 C 0.7071(14) 0.3447(13) 0.5765(12) 0.057(4) Uani 1 1 d . . .
H34A H 0.7151 0.4042 0.6363 0.085 Uiso 1 1 calc R . .
H34B H 0.7118 0.3751 0.5095 0.085 Uiso 1 1 calc R . .
H34C H 0.7655 0.3021 0.5829 0.085 Uiso 1 1 calc R . .
H1 H 0.5852 0.1398 -0.0107 0.03(3) Uiso 1 1 d RD . .


_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 O6 2.284(7) . ?
Dy1 O3 2.306(7) . ?
Dy1 O1 2.317(7) . ?
Dy1 O8 2.412(7) . ?
Dy1 O11 2.437(7) . ?
Dy1 O7 2.440(9) . ?
Dy1 O10 2.518(7) . ?
Dy1 O4 2.532(8) . ?
Dy1 O2 2.603(8) . ?
Dy1 N5 2.863(11) . ?
Dy1 N6 2.882(9) . ?
Dy1 Ni1 3.4045(16) . ?
Ni1 O3 2.034(7) . ?
Ni1 O5 2.034(7) . ?
Ni1 O1 2.057(7) . ?
Ni1 O13 2.073(7) . ?
Ni1 N2 2.087(9) . ?
Ni1 N4 2.117(8) . ?
Fe1 C5 2.019(12) . ?
Fe1 C29 2.026(12) . ?
Fe1 C28 2.030(11) . ?
Fe1 C27 2.031(12) . ?
Fe1 C2 2.041(12) . ?
Fe1 C3 2.043(12) . ?
Fe1 C30 2.043(14) . ?
Fe1 C1 2.047(11) . ?
Fe1 C26 2.047(12) . ?
Fe1 C4 2.051(12) . ?
O1 C14 1.288(13) . ?
O2 C13 1.395(14) . ?
O2 C15 1.444(12) . ?
O3 C22 1.334(13) . ?
O4 C17 1.378(14) . ?
O4 C16 1.454(12) . ?
O5 C31 1.232(12) . ?
O6 C31 1.276(12) . ?
O7 N5 1.297(13) . ?
O8 N5 1.296(13) . ?
O9 N5 1.189(14) . ?
O10 N6 1.253(12) . ?
O11 N6 1.256(12) . ?
O12 N6 1.242(12) . ?
N1 C6 1.275(14) . ?
N1 N2 1.440(10) . ?
N2 C8 1.275(14) . ?
N3 C24 1.286(14) . ?
N3 N4 1.434(10) . ?
N4 C23 1.266(14) . ?
N7 C33 1.15(2) . ?
C1 C2 1.420(16) . ?
C1 C5 1.436(15) . ?
C1 C6 1.479(13) . ?
C2 C3 1.429(15) . ?
C3 C4 1.401(17) . ?
C4 C5 1.419(14) . ?
C6 C7 1.484(15) . ?
C8 C9 1.449(13) . ?
C9 C14 1.424(15) . ?
C9 C10 1.431(17) . ?
C10 C11 1.359(15) . ?
C11 C12 1.404(17) . ?
C12 C13 1.397(17) . ?
C13 C14 1.408(14) . ?
C17 C18 1.367(17) . ?
C17 C22 1.416(14) . ?
C18 C19 1.371(18) . ?
C19 C20 1.399(16) . ?
C20 C21 1.395(16) . ?
C21 C22 1.388(15) . ?
C21 C23 1.460(14) . ?
C24 C26 1.481(14) . ?
C24 C25 1.505(15) . ?
C26 C30 1.421(17) . ?
C26 C27 1.435(15) . ?
C27 C28 1.404(15) . ?
C28 C29 1.400(17) . ?
C29 C30 1.424(16) . ?
C31 C32 1.525(16) . ?
C33 C34 1.46(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
O6 Dy1 O3 77.7(3) . . ?
O6 Dy1 O1 79.2(3) . . ?
O3 Dy1 O1 70.6(3) . . ?
O6 Dy1 O8 148.6(3) . . ?
O3 Dy1 O8 129.5(3) . . ?
O1 Dy1 O8 121.5(3) . . ?
O6 Dy1 O11 81.0(3) . . ?
O3 Dy1 O11 110.6(3) . . ?
O1 Dy1 O11 159.3(3) . . ?
O8 Dy1 O11 74.6(3) . . ?
O6 Dy1 O7 156.8(3) . . ?
O3 Dy1 O7 87.5(3) . . ?
O1 Dy1 O7 79.1(3) . . ?
O8 Dy1 O7 53.4(3) . . ?
O11 Dy1 O7 121.4(3) . . ?
O6 Dy1 O10 76.9(2) . . ?
O3 Dy1 O10 150.9(3) . . ?
O1 Dy1 O10 117.7(3) . . ?
O8 Dy1 O10 72.4(3) . . ?
O11 Dy1 O10 51.2(3) . . ?
O7 Dy1 O10 120.9(3) . . ?
O6 Dy1 O4 115.1(3) . . ?
O3 Dy1 O4 64.0(2) . . ?
O1 Dy1 O4 126.6(2) . . ?
O8 Dy1 O4 73.5(3) . . ?
O11 Dy1 O4 67.9(3) . . ?
O7 Dy1 O4 72.6(3) . . ?
O10 Dy1 O4 115.6(3) . . ?
O6 Dy1 O2 106.2(3) . . ?
O3 Dy1 O2 131.0(2) . . ?
O1 Dy1 O2 62.7(2) . . ?
O8 Dy1 O2 69.8(3) . . ?
O11 Dy1 O2 118.2(2) . . ?
O7 Dy1 O2 70.5(3) . . ?
O10 Dy1 O2 70.4(2) . . ?
O4 Dy1 O2 138.6(3) . . ?
O6 Dy1 N5 170.7(3) . . ?
O3 Dy1 N5 110.7(3) . . ?
O1 Dy1 N5 99.4(3) . . ?
O8 Dy1 N5 26.7(3) . . ?
O11 Dy1 N5 99.2(3) . . ?
O7 Dy1 N5 26.8(3) . . ?
O10 Dy1 N5 95.9(3) . . ?
O4 Dy1 N5 73.2(3) . . ?
O2 Dy1 N5 65.4(3) . . ?
O6 Dy1 N6 79.6(2) . . ?
O3 Dy1 N6 133.8(3) . . ?
O1 Dy1 N6 141.9(3) . . ?
O8 Dy1 N6 69.8(3) . . ?
O11 Dy1 N6 25.6(3) . . ?
O7 Dy1 N6 123.2(3) . . ?
O10 Dy1 N6 25.7(3) . . ?
O4 Dy1 N6 91.1(3) . . ?
O2 Dy1 N6 93.8(3) . . ?
N5 Dy1 N6 96.5(3) . . ?
O6 Dy1 Ni1 68.71(17) . . ?
O3 Dy1 Ni1 35.57(18) . . ?
O1 Dy1 Ni1 36.23(17) . . ?
O8 Dy1 Ni1 142.19(19) . . ?
O11 Dy1 Ni1 137.48(18) . . ?
O7 Dy1 Ni1 88.8(2) . . ?
O10 Dy1 Ni1 139.55(18) . . ?
O4 Dy1 Ni1 98.24(16) . . ?
O2 Dy1 Ni1 98.91(15) . . ?
N5 Dy1 Ni1 115.5(2) . . ?
N6 Dy1 Ni1 147.99(19) . . ?
O3 Ni1 O5 88.9(3) . . ?
O3 Ni1 O1 81.5(3) . . ?
O5 Ni1 O1 90.1(3) . . ?
O3 Ni1 O13 88.1(3) . . ?
O5 Ni1 O13 176.9(3) . . ?
O1 Ni1 O13 89.2(3) . . ?
O3 Ni1 N2 168.4(3) . . ?
O5 Ni1 N2 93.0(3) . . ?
O1 Ni1 N2 87.1(3) . . ?
O13 Ni1 N2 89.9(3) . . ?
O3 Ni1 N4 86.7(3) . . ?
O5 Ni1 N4 92.4(3) . . ?
O1 Ni1 N4 167.9(3) . . ?
O13 Ni1 N4 87.7(3) . . ?
N2 Ni1 N4 104.6(3) . . ?
O3 Ni1 Dy1 41.3(2) . . ?
O5 Ni1 Dy1 80.70(18) . . ?
O1 Ni1 Dy1 41.74(19) . . ?
O13 Ni1 Dy1 96.83(19) . . ?
N2 Ni1 Dy1 127.9(2) . . ?
N4 Ni1 Dy1 127.2(2) . . ?
C5 Fe1 C29 156.1(5) . . ?
C5 Fe1 C28 120.0(5) . . ?
C29 Fe1 C28 40.4(5) . . ?
C5 Fe1 C27 105.5(5) . . ?
C29 Fe1 C27 68.3(5) . . ?
C28 Fe1 C27 40.5(4) . . ?
C5 Fe1 C2 69.1(5) . . ?
C29 Fe1 C2 123.7(5) . . ?
C28 Fe1 C2 157.3(4) . . ?
C27 Fe1 C2 161.9(4) . . ?
C5 Fe1 C3 68.3(5) . . ?
C29 Fe1 C3 106.9(5) . . ?
C28 Fe1 C3 119.7(4) . . ?
C27 Fe1 C3 154.6(5) . . ?
C2 Fe1 C3 41.0(4) . . ?
C5 Fe1 C30 160.5(4) . . ?
C29 Fe1 C30 41.0(5) . . ?
C28 Fe1 C30 68.6(5) . . ?
C27 Fe1 C30 69.0(5) . . ?
C2 Fe1 C30 110.1(5) . . ?
C3 Fe1 C30 124.7(5) . . ?
C5 Fe1 C1 41.3(4) . . ?
C29 Fe1 C1 160.7(5) . . ?
C28 Fe1 C1 158.5(5) . . ?
C27 Fe1 C1 124.1(4) . . ?
C2 Fe1 C1 40.6(4) . . ?
C3 Fe1 C1 68.4(4) . . ?
C30 Fe1 C1 125.3(4) . . ?
C5 Fe1 C26 123.1(5) . . ?
C29 Fe1 C26 68.3(5) . . ?
C28 Fe1 C26 68.4(4) . . ?
C27 Fe1 C26 41.2(4) . . ?
C2 Fe1 C26 126.4(4) . . ?
C3 Fe1 C26 162.3(5) . . ?
C30 Fe1 C26 40.7(5) . . ?
C1 Fe1 C26 110.2(4) . . ?
C5 Fe1 C4 40.8(4) . . ?
C29 Fe1 C4 120.5(5) . . ?
C28 Fe1 C4 104.0(5) . . ?
C27 Fe1 C4 119.3(5) . . ?
C2 Fe1 C4 68.5(5) . . ?
C3 Fe1 C4 40.0(5) . . ?
C30 Fe1 C4 158.4(5) . . ?
C1 Fe1 C4 68.6(4) . . ?
C26 Fe1 C4 157.3(5) . . ?
C14 O1 Ni1 129.6(6) . . ?
C14 O1 Dy1 128.1(6) . . ?
Ni1 O1 Dy1 102.0(3) . . ?
C13 O2 C15 115.5(10) . . ?
C13 O2 Dy1 117.4(6) . . ?
C15 O2 Dy1 127.1(7) . . ?
C22 O3 Ni1 125.2(6) . . ?
C22 O3 Dy1 127.1(6) . . ?
Ni1 O3 Dy1 103.2(3) . . ?
C17 O4 C16 116.1(9) . . ?
C17 O4 Dy1 118.0(6) . . ?
C16 O4 Dy1 125.5(7) . . ?
C31 O5 Ni1 129.0(7) . . ?
C31 O6 Dy1 133.9(7) . . ?
N5 O7 Dy1 95.1(7) . . ?
N5 O8 Dy1 96.4(6) . . ?
N6 O10 Dy1 93.6(6) . . ?
N6 O11 Dy1 97.4(6) . . ?
C6 N1 N2 114.9(8) . . ?
C8 N2 N1 113.7(9) . . ?
C8 N2 Ni1 125.8(7) . . ?
N1 N2 Ni1 120.1(7) . . ?
C24 N3 N4 118.2(9) . . ?
C23 N4 N3 110.9(8) . . ?
C23 N4 Ni1 121.8(7) . . ?
N3 N4 Ni1 124.2(6) . . ?
O9 N5 O8 120.9(10) . . ?
O9 N5 O7 124.6(11) . . ?
O8 N5 O7 114.4(10) . . ?
O9 N5 Dy1 170.3(12) . . ?
O8 N5 Dy1 56.8(5) . . ?
O7 N5 Dy1 58.1(6) . . ?
O12 N6 O10 119.9(10) . . ?
O12 N6 O11 122.9(10) . . ?
O10 N6 O11 117.2(9) . . ?
O12 N6 Dy1 173.2(8) . . ?
O10 N6 Dy1 60.7(5) . . ?
O11 N6 Dy1 57.0(5) . . ?
C2 C1 C5 107.4(9) . . ?
C2 C1 C6 126.6(10) . . ?
C5 C1 C6 126.0(10) . . ?
C2 C1 Fe1 69.4(7) . . ?
C5 C1 Fe1 68.3(6) . . ?
C6 C1 Fe1 126.1(8) . . ?
C1 C2 C3 107.6(10) . . ?
C1 C2 Fe1 69.9(6) . . ?
C3 C2 Fe1 69.6(7) . . ?
C4 C3 C2 108.8(10) . . ?
C4 C3 Fe1 70.3(7) . . ?
C2 C3 Fe1 69.4(7) . . ?
C3 C4 C5 108.0(10) . . ?
C3 C4 Fe1 69.7(7) . . ?
C5 C4 Fe1 68.4(6) . . ?
C4 C5 C1 108.1(10) . . ?
C4 C5 Fe1 70.8(7) . . ?
C1 C5 Fe1 70.4(7) . . ?
N1 C6 C1 116.0(9) . . ?
N1 C6 C7 126.9(9) . . ?
C1 C6 C7 117.1(10) . . ?
N2 C8 C9 127.4(10) . . ?
C14 C9 C10 121.0(9) . . ?
C14 C9 C8 123.0(11) . . ?
C10 C9 C8 115.9(10) . . ?
C11 C10 C9 119.7(11) . . ?
C10 C11 C12 121.5(12) . . ?
C13 C12 C11 118.3(10) . . ?
O2 C13 C12 125.0(9) . . ?
O2 C13 C14 111.8(10) . . ?
C12 C13 C14 123.2(10) . . ?
O1 C14 C13 119.9(9) . . ?
O1 C14 C9 124.0(9) . . ?
C13 C14 C9 116.0(10) . . ?
C18 C17 O4 126.6(10) . . ?
C18 C17 C22 119.5(11) . . ?
O4 C17 C22 114.0(10) . . ?
C17 C18 C19 122.2(11) . . ?
C18 C19 C20 118.7(12) . . ?
C21 C20 C19 120.5(11) . . ?
C22 C21 C20 119.8(10) . . ?
C22 C21 C23 123.3(10) . . ?
C20 C21 C23 116.9(10) . . ?
O3 C22 C21 124.4(9) . . ?
O3 C22 C17 116.3(9) . . ?
C21 C22 C17 119.3(10) . . ?
N4 C23 C21 127.5(10) . . ?
N3 C24 C26 117.7(9) . . ?
N3 C24 C25 125.2(9) . . ?
C26 C24 C25 116.9(9) . . ?
C30 C26 C27 107.8(9) . . ?
C30 C26 C24 125.2(10) . . ?
C27 C26 C24 126.9(10) . . ?
C30 C26 Fe1 69.5(7) . . ?
C27 C26 Fe1 68.8(7) . . ?
C24 C26 Fe1 126.2(8) . . ?
C28 C27 C26 107.7(10) . . ?
C28 C27 Fe1 69.7(7) . . ?
C26 C27 Fe1 70.0(6) . . ?
C29 C28 C27 108.6(10) . . ?
C29 C28 Fe1 69.7(7) . . ?
C27 C28 Fe1 69.8(7) . . ?
C28 C29 C30 108.8(11) . . ?
C28 C29 Fe1 70.0(7) . . ?
C30 C29 Fe1 70.2(7) . . ?
C26 C30 C29 107.1(11) . . ?
C26 C30 Fe1 69.8(7) . . ?
C29 C30 Fe1 68.9(7) . . ?
O5 C31 O6 127.5(10) . . ?
O5 C31 C32 115.9(9) . . ?
O6 C31 C32 116.6(10) . . ?
N7 C33 C34 178.1(17) . . ?

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.968
_refine_diff_density_max         3.126
_refine_diff_density_min         -1.678
_refine_diff_density_rms         0.235
_database_code_depnum_ccdc_archive 'CCDC 993944'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_NiTb

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H33 Fe N6 Ni O13 Tb, C2 H3 N'
_chemical_formula_sum            'C34 H36 Fe N7 Ni O13 Tb'
_chemical_formula_weight         1024.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
Tb Tb -0.1723 4.1537 '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                   12.293(5)
_cell_length_b                   12.354(5)
_cell_length_c                   12.498(5)
_cell_angle_alpha                98.128(5)
_cell_angle_beta                 91.977(5)
_cell_angle_gamma                99.904(5)
_cell_volume                     1847.6(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2963
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      27.14

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1024.0
_exptl_absorpt_coefficient_mu    2.861
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_T_max  0.772
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9912
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         25.50
_reflns_number_total             6705
_reflns_number_gt                5370
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0183P)²+19.4865P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6705
_refine_ls_number_parameters     522
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1256
_refine_ls_wR_factor_gt          0.0995
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.087
_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
Tb1 Tb 0.23204(3) 0.41062(3) 0.75017(3) 0.02695(13) Uani 1 1 d . . .
Ni1 Ni 0.03619(8) 0.17881(8) 0.66418(8) 0.0194(2) Uani 1 1 d . . .
Fe1 Fe -0.39133(9) -0.14117(10) 0.66629(10) 0.0262(3) Uani 1 1 d . . .
O10 O 0.3064(5) 0.5320(5) 0.9234(5) 0.0306(13) Uani 1 1 d . . .
O6 O 0.0784(4) 0.4040(4) 0.8512(4) 0.0269(13) Uani 1 1 d . . .
O8 O 0.4212(5) 0.4938(5) 0.7257(5) 0.0433(17) Uani 1 1 d . . .
O4 O 0.2206(5) 0.5045(5) 0.5839(5) 0.0310(14) Uani 1 1 d . . .
O13 O 0.1197(4) 0.1150(5) 0.5336(4) 0.0251(12) Uani 1 1 d DU . .
H13A H 0.1008 0.1382 0.4788 0.038 Uiso 1 1 calc RD . .
O3 O 0.0880(4) 0.3322(4) 0.6230(4) 0.0228(12) Uani 1 1 d . . .
C7 C -0.1317(7) 0.0214(7) 0.8821(6) 0.0272(19) Uani 1 1 d . . .
H7A H -0.0954 -0.0133 0.9337 0.041 Uiso 1 1 calc R . .
H7B H -0.2014 0.0353 0.9078 0.041 Uiso 1 1 calc R . .
H7C H -0.0860 0.0903 0.8730 0.041 Uiso 1 1 calc R . .
O1 O 0.1822(4) 0.2212(4) 0.7577(4) 0.0254(12) Uani 1 1 d . . .
O11 O 0.2379(5) 0.6124(5) 0.7978(4) 0.0300(13) Uani 1 1 d . . .
O2 O 0.3697(4) 0.3172(5) 0.8541(5) 0.0323(14) Uani 1 1 d . . .
O7 O 0.3543(6) 0.3334(6) 0.6197(6) 0.057(2) Uani 1 1 d . . .
O5 O -0.0420(4) 0.2494(4) 0.7875(4) 0.0236(12) Uani 1 1 d . . .
C21 C -0.0106(6) 0.3041(6) 0.4498(7) 0.0250(18) Uani 1 1 d . . .
N3 N -0.1971(5) 0.0762(5) 0.5440(5) 0.0217(14) Uani 1 1 d . . .
C34 C 0.0880(13) 0.2668(10) 0.0768(9) 0.059(3) Uani 1 1 d . . .
C9 C 0.2033(6) 0.0407(7) 0.7993(6) 0.0230(17) Uani 1 1 d . . .
C13 C 0.3465(7) 0.2030(7) 0.8509(7) 0.031(2) Uani 1 1 d . . .
C6 C -0.1509(6) -0.0547(6) 0.7747(6) 0.0201(17) Uani 1 1 d . . .
C24 C -0.2776(6) 0.0895(7) 0.6060(6) 0.0243(17) Uani 1 1 d . . .
N1 N -0.0853(5) -0.0529(5) 0.6958(5) 0.0223(14) Uani 1 1 d . . .
N2 N 0.0163(5) 0.0259(5) 0.7187(5) 0.0210(14) Uani 1 1 d . . .
C17 C 0.1428(7) 0.4537(7) 0.4985(7) 0.0282(19) Uani 1 1 d . . .
C31 C -0.0173(7) 0.3396(7) 0.8463(6) 0.030(2) Uani 1 1 d . . .
N4 N -0.1024(5) 0.1646(5) 0.5533(5) 0.0209(14) Uani 1 1 d . . .
C8 C 0.0910(6) -0.0143(7) 0.7640(6) 0.0232(17) Uani 1 1 d . . .
H8 H 0.0716 -0.0876 0.7759 0.028 Uiso 1 1 calc R . .
C26 C -0.3736(6) -0.0011(7) 0.5929(7) 0.0276(19) Uani 1 1 d . . .
C2 C -0.3438(7) -0.1498(7) 0.8222(7) 0.0299(19) Uani 1 1 d . . .
H2 H -0.3530 -0.0969 0.8861 0.036 Uiso 1 1 calc R . .
O12 O 0.3247(6) 0.7175(6) 0.9463(6) 0.0513(19) Uani 1 1 d . . .
C22 C 0.0742(6) 0.3613(6) 0.5273(6) 0.0198(16) Uani 1 1 d . . .
C1 C -0.2515(6) -0.1429(6) 0.7572(6) 0.0231(17) Uani 1 1 d . . .
C27 C -0.3919(7) -0.0982(7) 0.5145(7) 0.0292(19) Uani 1 1 d . . .
H27 H -0.3425 -0.1176 0.4579 0.035 Uiso 1 1 calc R . .
C5 C -0.2717(6) -0.2356(6) 0.6709(6) 0.0230(17) Uani 1 1 d . . .
H5 H -0.2222 -0.2519 0.6134 0.028 Uiso 1 1 calc R . .
C3 C -0.4206(7) -0.2452(7) 0.7781(7) 0.036(2) Uani 1 1 d . . .
H3 H -0.4928 -0.2694 0.8062 0.043 Uiso 1 1 calc R . .
C14 C 0.2409(6) 0.1554(7) 0.7986(6) 0.0262(18) Uani 1 1 d . . .
C20 C -0.0199(7) 0.3426(7) 0.3484(6) 0.0287(19) Uani 1 1 d . . .
H20 H -0.0754 0.3057 0.2971 0.034 Uiso 1 1 calc R . .
C11 C 0.3756(7) 0.0247(8) 0.8883(7) 0.033(2) Uani 1 1 d . . .
H11 H 0.4214 -0.0189 0.9152 0.040 Uiso 1 1 calc R . .
C16 C 0.2961(7) 0.6007(7) 0.5617(8) 0.034(2) Uani 1 1 d . . .
H16A H 0.3395 0.5793 0.5025 0.052 Uiso 1 1 calc R . .
H16B H 0.3441 0.6315 0.6248 0.052 Uiso 1 1 calc R . .
H16C H 0.2549 0.6553 0.5429 0.052 Uiso 1 1 calc R . .
C10 C 0.2722(7) -0.0235(7) 0.8439(7) 0.0278(19) Uani 1 1 d . . .
H10 H 0.2474 -0.0991 0.8432 0.033 Uiso 1 1 calc R . .
O9 O 0.5337(7) 0.4075(7) 0.6311(7) 0.070(2) Uani 1 1 d U . .
C32 C -0.1016(7) 0.3771(8) 0.9179(8) 0.043(2) Uani 1 1 d . . .
H32A H -0.1595 0.3964 0.8749 0.065 Uiso 1 1 calc R . .
H32B H -0.0677 0.4408 0.9685 0.065 Uiso 1 1 calc R . .
H32C H -0.1321 0.3182 0.9566 0.065 Uiso 1 1 calc R . .
C12 C 0.4131(7) 0.1401(8) 0.8937(7) 0.035(2) Uani 1 1 d . . .
H12 H 0.4825 0.1729 0.9260 0.042 Uiso 1 1 calc R . .
C19 C 0.0510(8) 0.4324(7) 0.3252(7) 0.035(2) Uani 1 1 d . . .
H19 H 0.0435 0.4564 0.2585 0.042 Uiso 1 1 calc R . .
C25 C -0.2819(6) 0.1919(7) 0.6856(7) 0.033(2) Uani 1 1 d . . .
H25A H -0.2149 0.2447 0.6849 0.049 Uiso 1 1 calc R . .
H25B H -0.2895 0.1722 0.7569 0.049 Uiso 1 1 calc R . .
H25C H -0.3440 0.2241 0.6658 0.049 Uiso 1 1 calc R . .
C4 C -0.3770(7) -0.3007(7) 0.6859(7) 0.033(2) Uani 1 1 d . . .
H4 H -0.4133 -0.3692 0.6398 0.039 Uiso 1 1 calc R . .
C28 C -0.4968(7) -0.1620(8) 0.5323(7) 0.037(2) Uani 1 1 d . . .
H28 H -0.5314 -0.2333 0.4901 0.044 Uiso 1 1 calc R . .
N6 N 0.2883(6) 0.6213(6) 0.8904(6) 0.0342(18) Uani 1 1 d . . .
C15 C 0.4744(8) 0.3729(8) 0.9111(9) 0.053(3) Uani 1 1 d . . .
H15A H 0.4738 0.3608 0.9853 0.080 Uiso 1 1 calc R . .
H15B H 0.4840 0.4511 0.9081 0.080 Uiso 1 1 calc R . .
H15C H 0.5342 0.3433 0.8775 0.080 Uiso 1 1 calc R . .
C29 C -0.5410(7) -0.1055(7) 0.6210(8) 0.036(2) Uani 1 1 d . . .
H29 H -0.6117 -0.1305 0.6515 0.044 Uiso 1 1 calc R . .
N7 N 0.0037(12) 0.2167(9) 0.0811(8) 0.078(4) Uani 1 1 d . . .
C23 C -0.0955(7) 0.2133(6) 0.4689(7) 0.0250(18) Uani 1 1 d . . .
H23 H -0.1510 0.1875 0.4142 0.030 Uiso 1 1 calc R . .
C18 C 0.1343(8) 0.4883(7) 0.4006(7) 0.035(2) Uani 1 1 d . . .
H18 H 0.1838 0.5488 0.3844 0.042 Uiso 1 1 calc R . .
C30 C -0.4660(7) -0.0065(7) 0.6588(7) 0.032(2) Uani 1 1 d . . .
H30 H -0.4756 0.0490 0.7203 0.039 Uiso 1 1 calc R . .
C33 C 0.1987(7) 0.3375(9) 0.0769(7) 0.068(4) Uani 1 1 d . . .
H33A H 0.1934 0.3964 0.0355 0.102 Uiso 1 1 calc R . .
H33B H 0.2497 0.2933 0.0453 0.102 Uiso 1 1 calc R . .
H33C H 0.2244 0.3687 0.1500 0.102 Uiso 1 1 calc R . .
N5 N 0.4389(7) 0.4167(8) 0.6548(6) 0.068(3) Uani 1 1 d R . .
H13B H 0.160(5) 0.062(4) 0.542(5) 0.009(18) Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O6 2.304(5) . ?
Tb1 O3 2.320(5) . ?
Tb1 O1 2.331(5) . ?
Tb1 O8 2.423(6) . ?
Tb1 O7 2.460(7) . ?
Tb1 O11 2.467(6) . ?
Tb1 O10 2.499(6) . ?
Tb1 O4 2.529(6) . ?
Tb1 O2 2.613(6) . ?
Tb1 N5 2.839(8) . ?
Tb1 N6 2.886(7) . ?
Tb1 Ni1 3.4252(14) . ?
Ni1 O5 2.017(5) . ?
Ni1 O3 2.036(5) . ?
Ni1 O1 2.055(5) . ?
Ni1 N2 2.076(6) . ?
Ni1 O13 2.091(6) . ?
Ni1 N4 2.126(6) . ?
Fe1 C3 2.028(9) . ?
Fe1 C5 2.032(8) . ?
Fe1 C1 2.033(8) . ?
Fe1 C2 2.038(8) . ?
Fe1 C28 2.041(9) . ?
Fe1 C27 2.041(9) . ?
Fe1 C29 2.044(9) . ?
Fe1 C30 2.045(9) . ?
Fe1 C26 2.053(8) . ?
Fe1 C4 2.057(9) . ?
O10 N6 1.281(9) . ?
O6 C31 1.296(10) . ?
O8 N5 1.258(10) . ?
O4 C17 1.409(10) . ?
O4 C16 1.443(9) . ?
O3 C22 1.310(9) . ?
C7 C6 1.512(10) . ?
O1 C14 1.318(10) . ?
O11 N6 1.275(9) . ?
O2 C13 1.385(10) . ?
O2 C15 1.460(10) . ?
O7 N5 1.344(10) . ?
O5 C31 1.229(10) . ?
C21 C22 1.417(11) . ?
C21 C20 1.423(11) . ?
C21 C23 1.447(11) . ?
N3 C24 1.296(10) . ?
N3 N4 1.442(8) . ?
C34 N7 1.119(16) . ?
C34 C33 1.485(17) . ?
C9 C10 1.407(11) . ?
C9 C14 1.414(11) . ?
C9 C8 1.454(10) . ?
C13 C12 1.366(12) . ?
C13 C14 1.424(11) . ?
C6 N1 1.294(10) . ?
C6 C1 1.488(9) . ?
C24 C26 1.467(11) . ?
C24 C25 1.504(11) . ?
N1 N2 1.438(8) . ?
N2 C8 1.269(10) . ?
C17 C18 1.358(12) . ?
C17 C22 1.396(10) . ?
C31 C32 1.484(12) . ?
N4 C23 1.285(10) . ?
C26 C27 1.417(12) . ?
C26 C30 1.423(12) . ?
C2 C3 1.408(12) . ?
C2 C1 1.416(11) . ?
O12 N6 1.289(9) . ?
C1 C5 1.439(11) . ?
C27 C28 1.433(11) . ?
C5 C4 1.435(10) . ?
C3 C4 1.425(13) . ?
C20 C19 1.360(12) . ?
C11 C10 1.369(11) . ?
C11 C12 1.413(13) . ?
O9 N5 1.232(11) . ?
C19 C18 1.385(13) . ?
C28 C29 1.401(13) . ?
C29 C30 1.410(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Tb1 O3 76.95(19) . . ?
O6 Tb1 O1 77.61(19) . . ?
O3 Tb1 O1 70.05(18) . . ?
O6 Tb1 O8 149.4(2) . . ?
O3 Tb1 O8 130.2(2) . . ?
O1 Tb1 O8 121.4(2) . . ?
O6 Tb1 O7 154.8(2) . . ?
O3 Tb1 O7 86.4(2) . . ?
O1 Tb1 O7 79.0(2) . . ?
O8 Tb1 O7 54.4(2) . . ?
O6 Tb1 O11 81.72(19) . . ?
O3 Tb1 O11 110.83(18) . . ?
O1 Tb1 O11 158.54(19) . . ?
O8 Tb1 O11 75.4(2) . . ?
O7 Tb1 O11 122.3(2) . . ?
O6 Tb1 O10 77.53(18) . . ?
O3 Tb1 O10 151.33(18) . . ?
O1 Tb1 O10 116.51(19) . . ?
O8 Tb1 O10 72.4(2) . . ?
O7 Tb1 O10 121.9(2) . . ?
O11 Tb1 O10 52.30(19) . . ?
O6 Tb1 O4 114.74(19) . . ?
O3 Tb1 O4 63.70(18) . . ?
O1 Tb1 O4 126.47(18) . . ?
O8 Tb1 O4 75.1(2) . . ?
O7 Tb1 O4 72.8(2) . . ?
O11 Tb1 O4 68.07(18) . . ?
O10 Tb1 O4 117.02(19) . . ?
O6 Tb1 O2 105.22(19) . . ?
O3 Tb1 O2 130.33(18) . . ?
O1 Tb1 O2 62.49(17) . . ?
O8 Tb1 O2 69.8(2) . . ?
O7 Tb1 O2 71.5(2) . . ?
O11 Tb1 O2 118.65(18) . . ?
O10 Tb1 O2 69.55(18) . . ?
O4 Tb1 O2 140.02(19) . . ?
O6 Tb1 N5 171.4(2) . . ?
O3 Tb1 N5 110.6(2) . . ?
O1 Tb1 N5 100.8(2) . . ?
O8 Tb1 N5 26.2(2) . . ?
O7 Tb1 N5 28.2(2) . . ?
O11 Tb1 N5 98.7(2) . . ?
O10 Tb1 N5 95.9(2) . . ?
O4 Tb1 N5 73.1(2) . . ?
O2 Tb1 N5 67.0(2) . . ?
O6 Tb1 N6 79.71(19) . . ?
O3 Tb1 N6 134.0(2) . . ?
O1 Tb1 N6 140.8(2) . . ?
O8 Tb1 N6 70.7(2) . . ?
O7 Tb1 N6 125.0(2) . . ?
O11 Tb1 N6 26.09(19) . . ?
O10 Tb1 N6 26.27(19) . . ?
O4 Tb1 N6 92.1(2) . . ?
O2 Tb1 N6 93.8(2) . . ?
N5 Tb1 N6 96.9(2) . . ?
O6 Tb1 Ni1 67.70(13) . . ?
O3 Tb1 Ni1 35.31(13) . . ?
O1 Tb1 Ni1 35.84(13) . . ?
O8 Tb1 Ni1 142.07(14) . . ?
O7 Tb1 Ni1 87.79(18) . . ?
O11 Tb1 Ni1 137.32(14) . . ?
O10 Tb1 Ni1 138.72(13) . . ?
O4 Tb1 Ni1 97.83(13) . . ?
O2 Tb1 Ni1 98.27(12) . . ?
N5 Tb1 Ni1 115.91(18) . . ?
N6 Tb1 Ni1 147.17(14) . . ?
O5 Ni1 O3 89.1(2) . . ?
O5 Ni1 O1 89.5(2) . . ?
O3 Ni1 O1 81.5(2) . . ?
O5 Ni1 N2 93.8(2) . . ?
O3 Ni1 N2 168.4(2) . . ?
O1 Ni1 N2 87.3(2) . . ?
O5 Ni1 O13 176.6(2) . . ?
O3 Ni1 O13 87.5(2) . . ?
O1 Ni1 O13 90.2(2) . . ?
N2 Ni1 O13 89.6(2) . . ?
O5 Ni1 N4 92.3(2) . . ?
O3 Ni1 N4 87.0(2) . . ?
O1 Ni1 N4 168.3(2) . . ?
N2 Ni1 N4 104.2(2) . . ?
O13 Ni1 N4 87.3(2) . . ?
O5 Ni1 Tb1 80.82(15) . . ?
O3 Ni1 Tb1 41.19(14) . . ?
O1 Ni1 Tb1 41.64(15) . . ?
N2 Ni1 Tb1 128.24(17) . . ?
O13 Ni1 Tb1 96.76(16) . . ?
N4 Ni1 Tb1 127.33(17) . . ?
C3 Fe1 C5 69.0(3) . . ?
C3 Fe1 C1 68.4(3) . . ?
C5 Fe1 C1 41.5(3) . . ?
C3 Fe1 C2 40.5(3) . . ?
C5 Fe1 C2 69.3(3) . . ?
C1 Fe1 C2 40.7(3) . . ?
C3 Fe1 C28 119.8(4) . . ?
C5 Fe1 C28 120.2(4) . . ?
C1 Fe1 C28 158.8(4) . . ?
C2 Fe1 C28 156.9(3) . . ?
C3 Fe1 C27 155.6(4) . . ?
C5 Fe1 C27 105.3(3) . . ?
C1 Fe1 C27 123.9(3) . . ?
C2 Fe1 C27 161.6(3) . . ?
C28 Fe1 C27 41.1(3) . . ?
C3 Fe1 C29 106.6(4) . . ?
C5 Fe1 C29 156.1(3) . . ?
C1 Fe1 C29 160.6(4) . . ?
C2 Fe1 C29 123.5(4) . . ?
C28 Fe1 C29 40.1(4) . . ?
C27 Fe1 C29 68.5(4) . . ?
C3 Fe1 C30 124.3(4) . . ?
C5 Fe1 C30 160.7(3) . . ?
C1 Fe1 C30 126.0(3) . . ?
C2 Fe1 C30 110.8(4) . . ?
C28 Fe1 C30 67.7(4) . . ?
C27 Fe1 C30 68.3(4) . . ?
C29 Fe1 C30 40.3(3) . . ?
C3 Fe1 C26 161.9(4) . . ?
C5 Fe1 C26 122.9(3) . . ?
C1 Fe1 C26 110.3(3) . . ?
C2 Fe1 C26 126.7(3) . . ?
C28 Fe1 C26 68.3(3) . . ?
C27 Fe1 C26 40.5(3) . . ?
C29 Fe1 C26 68.3(3) . . ?
C30 Fe1 C26 40.6(3) . . ?
C3 Fe1 C4 40.8(3) . . ?
C5 Fe1 C4 41.1(3) . . ?
C1 Fe1 C4 68.9(3) . . ?
C2 Fe1 C4 68.7(3) . . ?
C28 Fe1 C4 103.8(4) . . ?
C27 Fe1 C4 119.5(4) . . ?
C29 Fe1 C4 120.3(3) . . ?
C30 Fe1 C4 158.1(3) . . ?
C26 Fe1 C4 157.0(3) . . ?
N6 O10 Tb1 94.0(5) . . ?
C31 O6 Tb1 135.3(5) . . ?
N5 O8 Tb1 95.7(5) . . ?
C17 O4 C16 115.1(6) . . ?
C17 O4 Tb1 118.8(4) . . ?
C16 O4 Tb1 125.7(5) . . ?
C22 O3 Ni1 126.2(5) . . ?
C22 O3 Tb1 125.6(5) . . ?
Ni1 O3 Tb1 103.5(2) . . ?
C14 O1 Ni1 128.6(5) . . ?
C14 O1 Tb1 128.2(5) . . ?
Ni1 O1 Tb1 102.5(2) . . ?
N6 O11 Tb1 95.6(5) . . ?
C13 O2 C15 115.3(7) . . ?
C13 O2 Tb1 118.3(5) . . ?
C15 O2 Tb1 126.3(5) . . ?
N5 O7 Tb1 91.8(5) . . ?
C31 O5 Ni1 131.0(5) . . ?
C22 C21 C20 118.8(7) . . ?
C22 C21 C23 124.7(7) . . ?
C20 C21 C23 116.4(7) . . ?
C24 N3 N4 118.1(6) . . ?
N7 C34 C33 176.6(13) . . ?
C10 C9 C14 120.2(7) . . ?
C10 C9 C8 116.8(7) . . ?
C14 C9 C8 122.8(7) . . ?
C12 C13 O2 125.9(8) . . ?
C12 C13 C14 122.0(8) . . ?
O2 C13 C14 112.1(7) . . ?
N1 C6 C1 115.8(7) . . ?
N1 C6 C7 125.8(7) . . ?
C1 C6 C7 118.4(7) . . ?
N3 C24 C26 116.6(7) . . ?
N3 C24 C25 125.1(7) . . ?
C26 C24 C25 118.2(7) . . ?
C6 N1 N2 114.7(6) . . ?
C8 N2 N1 112.1(6) . . ?
C8 N2 Ni1 126.3(5) . . ?
N1 N2 Ni1 121.2(5) . . ?
C18 C17 C22 123.8(8) . . ?
C18 C17 O4 125.4(7) . . ?
C22 C17 O4 110.8(7) . . ?
O5 C31 O6 124.3(8) . . ?
O5 C31 C32 118.2(8) . . ?
O6 C31 C32 117.5(8) . . ?
C23 N4 N3 111.9(6) . . ?
C23 N4 Ni1 121.5(5) . . ?
N3 N4 Ni1 123.7(5) . . ?
N2 C8 C9 127.6(7) . . ?
C27 C26 C30 107.6(7) . . ?
C27 C26 C24 127.2(8) . . ?
C30 C26 C24 125.2(8) . . ?
C27 C26 Fe1 69.3(5) . . ?
C30 C26 Fe1 69.4(5) . . ?
C24 C26 Fe1 126.5(6) . . ?
C3 C2 C1 107.9(8) . . ?
C3 C2 Fe1 69.4(5) . . ?
C1 C2 Fe1 69.5(5) . . ?
O3 C22 C17 120.4(7) . . ?
O3 C22 C21 122.8(7) . . ?
C17 C22 C21 116.8(7) . . ?
C2 C1 C5 108.3(6) . . ?
C2 C1 C6 125.9(7) . . ?
C5 C1 C6 125.8(7) . . ?
C2 C1 Fe1 69.8(5) . . ?
C5 C1 Fe1 69.2(4) . . ?
C6 C1 Fe1 126.5(5) . . ?
C26 C27 C28 107.4(8) . . ?
C26 C27 Fe1 70.2(5) . . ?
C28 C27 Fe1 69.4(5) . . ?
C4 C5 C1 107.3(7) . . ?
C4 C5 Fe1 70.4(5) . . ?
C1 C5 Fe1 69.3(4) . . ?
C2 C3 C4 109.3(8) . . ?
C2 C3 Fe1 70.1(5) . . ?
C4 C3 Fe1 70.7(5) . . ?
O1 C14 C9 124.1(7) . . ?
O1 C14 C13 118.5(7) . . ?
C9 C14 C13 117.3(8) . . ?
C19 C20 C21 121.2(8) . . ?
C10 C11 C12 120.6(8) . . ?
C11 C10 C9 120.4(8) . . ?
C13 C12 C11 119.3(8) . . ?
C20 C19 C18 120.2(8) . . ?
C3 C4 C5 107.2(7) . . ?
C3 C4 Fe1 68.5(5) . . ?
C5 C4 Fe1 68.5(5) . . ?
C29 C28 C27 108.4(8) . . ?
C29 C28 Fe1 70.1(5) . . ?
C27 C28 Fe1 69.5(5) . . ?
O11 N6 O10 117.8(7) . . ?
O11 N6 O12 120.8(7) . . ?
O10 N6 O12 121.3(7) . . ?
O11 N6 Tb1 58.3(4) . . ?
O10 N6 Tb1 59.7(4) . . ?
O12 N6 Tb1 172.7(6) . . ?
C28 C29 C30 108.1(8) . . ?
C28 C29 Fe1 69.8(5) . . ?
C30 C29 Fe1 69.9(5) . . ?
N4 C23 C21 126.9(7) . . ?
C17 C18 C19 119.2(8) . . ?
C29 C30 C26 108.5(8) . . ?
C29 C30 Fe1 69.8(5) . . ?
C26 C30 Fe1 70.0(5) . . ?
O9 N5 O8 121.2(8) . . ?
O9 N5 O7 119.8(9) . . ?
O8 N5 O7 118.0(7) . . ?
O9 N5 Tb1 166.4(7) . . ?
O8 N5 Tb1 58.1(4) . . ?
O7 N5 Tb1 60.0(4) . . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         1.593
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.192
_database_code_depnum_ccdc_archive 'CCDC 993945'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_NiHo

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H33 Fe Ho N6 Ni O13, C2 H3 N'
_chemical_formula_sum            'C34 H36 Fe Ho N7 Ni O13'
_chemical_formula_weight         1030.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
Ho Ho -0.2175 4.6783 '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                   12.313(4)
_cell_length_b                   12.378(4)
_cell_length_c                   12.530(4)
_cell_angle_alpha                98.030(6)
_cell_angle_beta                 91.972(6)
_cell_angle_gamma                100.182(6)
_cell_volume                     1857.7(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9781
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      28.37

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          .07
_exptl_crystal_size_mid          .06
_exptl_crystal_size_min          .05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.842
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1028
_exptl_absorpt_coefficient_mu    3.072
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.6001
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  '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            29219
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         27.00
_reflns_number_total             8042
_reflns_number_gt                7104
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0024P)²+7.2417P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8042
_refine_ls_number_parameters     528
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.0648
_refine_ls_wR_factor_gt          0.0584
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.231165(14) 0.410184(14) 0.249324(15) 0.01909(5) Uani 1 1 d . . .
Fe1 Fe -0.39151(4) -0.14161(4) 0.16664(4) 0.01823(12) Uani 1 1 d . . .
Ni1 Ni 0.03651(3) 0.17917(3) 0.16394(4) 0.01346(10) Uani 1 1 d . . .
O4 O 0.2214(2) 0.5054(2) 0.0838(2) 0.0252(6) Uani 1 1 d . . .
O3 O 0.0890(2) 0.33285(19) 0.12324(19) 0.0167(5) Uani 1 1 d . . .
N3 N -0.1971(2) 0.0766(2) 0.0434(2) 0.0170(6) Uani 1 1 d . . .
O1 O 0.18264(19) 0.22274(19) 0.2567(2) 0.0182(5) Uani 1 1 d . . .
O2 O 0.3707(2) 0.3190(2) 0.3518(2) 0.0271(6) Uani 1 1 d . . .
C15 C 0.4753(4) 0.3749(4) 0.4060(4) 0.0431(13) Uani 1 1 d . . .
H15A H 0.4765 0.3629 0.4801 0.065 Uiso 1 1 calc R . .
H15B H 0.4843 0.4530 0.4029 0.065 Uiso 1 1 calc R . .
H15C H 0.5344 0.3458 0.3711 0.065 Uiso 1 1 calc R . .
O5 O -0.04192(19) 0.24956(19) 0.2869(2) 0.0180(5) Uani 1 1 d . . .
O6 O 0.0803(2) 0.4047(2) 0.3509(2) 0.0206(6) Uani 1 1 d . . .
O8 O 0.4180(2) 0.4946(2) 0.2231(3) 0.0366(8) Uani 1 1 d . . .
O7 O 0.3540(3) 0.3361(3) 0.1198(3) 0.0397(8) Uani 1 1 d . . .
O10 O 0.2340(2) 0.6084(2) 0.2977(2) 0.0256(6) Uani 1 1 d . . .
O11 O 0.3050(2) 0.5296(2) 0.4217(2) 0.0231(6) Uani 1 1 d . . .
O12 O 0.3214(3) 0.7141(3) 0.4460(3) 0.0457(9) Uani 1 1 d . . .
N1 N -0.0855(2) -0.0522(2) 0.1966(2) 0.0152(6) Uani 1 1 d . . .
N4 N -0.1026(2) 0.1646(2) 0.0535(2) 0.0147(6) Uani 1 1 d . . .
C14 C 0.2406(3) 0.1573(3) 0.2982(3) 0.0178(7) Uani 1 1 d . . .
O13 O 0.1204(2) 0.1160(2) 0.0333(2) 0.0189(5) Uani 1 1 d . . .
O9 O 0.5296(3) 0.4108(3) 0.1251(4) 0.0783(16) Uani 1 1 d . . .
N6 N 0.2866(3) 0.6179(3) 0.3891(3) 0.0275(8) Uani 1 1 d . . .
N7 N 0.9937(5) 0.7839(4) 0.4182(4) 0.0610(15) Uani 1 1 d . . .
C16 C 0.2969(4) 0.6026(3) 0.0640(4) 0.0321(10) Uani 1 1 d . . .
H1A H 0.3434 0.5821 0.0076 0.048 Uiso 1 1 calc R . .
H1B H 0.3417 0.6346 0.1288 0.048 Uiso 1 1 calc R . .
H1C H 0.2557 0.6558 0.0424 0.048 Uiso 1 1 calc R . .
C17 C 0.1446(3) 0.4543(3) -0.0001(3) 0.0215(8) Uani 1 1 d . . .
C22 C 0.0732(3) 0.3604(3) 0.0270(3) 0.0169(7) Uani 1 1 d . . .
N2 N 0.0154(2) 0.0267(2) 0.2187(2) 0.0153(6) Uani 1 1 d . . .
C6 C -0.1514(3) -0.0553(3) 0.2742(3) 0.0167(7) Uani 1 1 d . . .
C7 C -0.1325(3) 0.0202(3) 0.3817(3) 0.0219(8) Uani 1 1 d . . .
H6A H -0.1018 -0.0169 0.4345 0.033 Uiso 1 1 calc R . .
H6B H -0.2017 0.0383 0.4044 0.033 Uiso 1 1 calc R . .
H6C H -0.0822 0.0871 0.3743 0.033 Uiso 1 1 calc R . .
C1 C -0.2511(3) -0.1422(3) 0.2580(3) 0.0185(7) Uani 1 1 d . . .
C2 C -0.3446(3) -0.1498(3) 0.3228(3) 0.0231(8) Uani 1 1 d . . .
H8 H -0.3539 -0.0998 0.3830 0.028 Uiso 1 1 calc R . .
C3 C -0.4210(3) -0.2474(3) 0.2787(3) 0.0263(9) Uani 1 1 d . . .
H9 H -0.4889 -0.2725 0.3056 0.032 Uiso 1 1 calc R . .
C4 C -0.3762(3) -0.2998(3) 0.1871(3) 0.0250(9) Uani 1 1 d . . .
H10 H -0.4098 -0.3649 0.1432 0.030 Uiso 1 1 calc R . .
C5 C -0.2718(3) -0.2362(3) 0.1739(3) 0.0194(8) Uani 1 1 d . . .
H11 H -0.2245 -0.2524 0.1200 0.023 Uiso 1 1 calc R . .
C29 C -0.4962(3) -0.1636(3) 0.0324(3) 0.0271(9) Uani 1 1 d . . .
H12 H -0.5291 -0.2314 -0.0073 0.032 Uiso 1 1 calc R . .
C28 C -0.5411(3) -0.1067(3) 0.1207(4) 0.0278(9) Uani 1 1 d . . .
H13 H -0.6085 -0.1306 0.1491 0.033 Uiso 1 1 calc R . .
C27 C -0.4662(3) -0.0067(3) 0.1589(3) 0.0261(9) Uani 1 1 d . . .
H14 H -0.4758 0.0464 0.2164 0.031 Uiso 1 1 calc R . .
C26 C -0.3728(3) -0.0022(3) 0.0929(3) 0.0177(7) Uani 1 1 d . . .
C30 C -0.3923(3) -0.1001(3) 0.0140(3) 0.0226(8) Uani 1 1 d . . .
H16 H -0.3455 -0.1189 -0.0395 0.027 Uiso 1 1 calc R . .
C24 C -0.2762(3) 0.0888(3) 0.1043(3) 0.0175(7) Uani 1 1 d . . .
C23 C -0.0948(3) 0.2125(3) -0.0312(3) 0.0173(7) Uani 1 1 d . . .
H18 H -0.1494 0.1851 -0.0862 0.021 Uiso 1 1 calc R . .
C21 C -0.0107(3) 0.3043(3) -0.0511(3) 0.0187(7) Uani 1 1 d . . .
C20 C -0.0195(3) 0.3419(3) -0.1517(3) 0.0248(8) Uani 1 1 d . . .
H20 H -0.0749 0.3048 -0.2029 0.030 Uiso 1 1 calc R . .
C19 C 0.0521(4) 0.4320(3) -0.1752(3) 0.0300(9) Uani 1 1 d . . .
H21 H 0.0455 0.4553 -0.2421 0.036 Uiso 1 1 calc R . .
C18 C 0.1353(4) 0.4891(3) -0.0987(3) 0.0275(9) Uani 1 1 d . . .
H22 H 0.1840 0.5504 -0.1146 0.033 Uiso 1 1 calc R . .
C25 C -0.2816(3) 0.1909(3) 0.1844(3) 0.0222(8) Uani 1 1 d . . .
H23A H -0.2148 0.2444 0.1843 0.033 Uiso 1 1 calc R . .
H23B H -0.2896 0.1707 0.2553 0.033 Uiso 1 1 calc R . .
H23C H -0.3437 0.2225 0.1643 0.033 Uiso 1 1 calc R . .
C8 C 0.0917(3) -0.0134(3) 0.2638(3) 0.0181(7) Uani 1 1 d . . .
H24 H 0.0731 -0.0869 0.2753 0.022 Uiso 1 1 calc R . .
C9 C 0.2033(3) 0.0428(3) 0.2988(3) 0.0183(7) Uani 1 1 d . . .
C13 C 0.3469(3) 0.2052(3) 0.3491(3) 0.0228(8) Uani 1 1 d . . .
C12 C 0.4139(3) 0.1431(3) 0.3922(3) 0.0271(9) Uani 1 1 d . . .
H27 H 0.4834 0.1766 0.4237 0.033 Uiso 1 1 calc R . .
C11 C 0.3772(3) 0.0288(3) 0.3887(3) 0.0260(9) Uani 1 1 d . . .
H28 H 0.4230 -0.0140 0.4167 0.031 Uiso 1 1 calc R . .
C10 C 0.2738(3) -0.0201(3) 0.3441(3) 0.0232(8) Uani 1 1 d . . .
H29 H 0.2496 -0.0957 0.3436 0.028 Uiso 1 1 calc R . .
C31 C -0.0137(3) 0.3415(3) 0.3468(3) 0.0187(7) Uani 1 1 d . . .
C32 C -0.1003(3) 0.3796(4) 0.4180(4) 0.0360(11) Uani 1 1 d . . .
H31A H -0.1581 0.3974 0.3740 0.054 Uiso 1 1 calc R . .
H31B H -0.0671 0.4441 0.4677 0.054 Uiso 1 1 calc R . .
H31C H -0.1307 0.3214 0.4575 0.054 Uiso 1 1 calc R . .
N5 N 0.4371(3) 0.4156(3) 0.1533(4) 0.0508(12) Uani 1 1 d . . .
C33 C 0.9087(6) 0.7310(4) 0.4213(4) 0.0459(14) Uani 1 1 d . . .
C34 C 0.8005(5) 0.6627(5) 0.4241(5) 0.0542(15) Uani 1 1 d . . .
H34A H 0.7742 0.6285 0.3522 0.081 Uiso 1 1 calc R . .
H34B H 0.7500 0.7081 0.4537 0.081 Uiso 1 1 calc R . .
H34C H 0.8058 0.6062 0.4684 0.081 Uiso 1 1 calc R . .
H1 H 0.149(4) 0.062(4) 0.032(4) 0.036(14) Uiso 1 1 d . . .
H100 H 0.102(5) 0.118(5) -0.034(5) 0.07(2) Uiso 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
Ho1 O6 2.284(3) . ?
Ho1 O3 2.296(2) . ?
Ho1 O1 2.307(3) . ?
Ho1 O8 2.407(3) . ?
Ho1 O10 2.438(3) . ?
Ho1 O7 2.451(3) . ?
Ho1 O11 2.485(3) . ?
Ho1 O4 2.534(3) . ?
Ho1 O2 2.610(3) . ?
Ho1 N5 2.838(4) . ?
Ho1 N6 2.860(3) . ?
Fe1 C29 2.041(4) . ?
Fe1 C2 2.042(4) . ?
Fe1 C1 2.043(4) . ?
Fe1 C5 2.046(4) . ?
Fe1 C28 2.047(4) . ?
Fe1 C30 2.048(4) . ?
Fe1 C3 2.050(4) . ?
Fe1 C4 2.050(4) . ?
Fe1 C26 2.051(4) . ?
Fe1 C27 2.056(4) . ?
Ni1 O5 2.023(2) . ?
Ni1 O3 2.038(2) . ?
Ni1 O1 2.054(2) . ?
Ni1 N2 2.073(3) . ?
Ni1 O13 2.098(3) . ?
Ni1 N4 2.130(3) . ?
O4 C17 1.391(5) . ?
O4 C16 1.440(4) . ?
O3 C22 1.315(4) . ?
N3 C24 1.275(5) . ?
N3 N4 1.436(4) . ?
O1 C14 1.316(4) . ?
O2 C13 1.383(5) . ?
O2 C15 1.446(4) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
O5 C31 1.258(4) . ?
O6 C31 1.272(4) . ?
O8 N5 1.277(5) . ?
O7 N5 1.300(5) . ?
O10 N6 1.277(4) . ?
O11 N6 1.273(4) . ?
O12 N6 1.293(4) . ?
N1 C6 1.288(5) . ?
N1 N2 1.431(4) . ?
N4 C23 1.284(5) . ?
C14 C9 1.412(5) . ?
C14 C13 1.426(5) . ?
O13 H1 0.81(5) . ?
O13 H100 0.87(7) . ?
O9 N5 1.214(5) . ?
N7 C33 1.137(8) . ?
C16 H1A 0.9600 . ?
C16 H1B 0.9600 . ?
C16 H1C 0.9600 . ?
C17 C18 1.372(6) . ?
C17 C22 1.418(5) . ?
C22 C21 1.413(5) . ?
N2 C8 1.287(5) . ?
C6 C1 1.470(5) . ?
C6 C7 1.514(5) . ?
C7 H6A 0.9600 . ?
C7 H6B 0.9600 . ?
C7 H6C 0.9600 . ?
C1 C2 1.429(5) . ?
C1 C5 1.436(5) . ?
C2 C3 1.424(5) . ?
C2 H8 0.9300 . ?
C3 C4 1.416(6) . ?
C3 H9 0.9300 . ?
C4 C5 1.413(5) . ?
C4 H10 0.9300 . ?
C5 H11 0.9300 . ?
C29 C28 1.410(6) . ?
C29 C30 1.422(5) . ?
C29 H12 0.9300 . ?
C28 C27 1.418(5) . ?
C28 H13 0.9300 . ?
C27 C26 1.438(5) . ?
C27 H14 0.9300 . ?
C26 C30 1.432(5) . ?
C26 C24 1.473(5) . ?
C30 H16 0.9300 . ?
C24 C25 1.513(5) . ?
C23 C21 1.451(5) . ?
C23 H18 0.9300 . ?
C21 C20 1.411(5) . ?
C20 C19 1.367(6) . ?
C20 H20 0.9300 . ?
C19 C18 1.397(6) . ?
C19 H21 0.9300 . ?
C18 H22 0.9300 . ?
C25 H23A 0.9600 . ?
C25 H23B 0.9600 . ?
C25 H23C 0.9600 . ?
C8 C9 1.449(5) . ?
C8 H24 0.9300 . ?
C9 C10 1.418(5) . ?
C13 C12 1.369(6) . ?
C12 C11 1.401(6) . ?
C12 H27 0.9300 . ?
C11 C10 1.372(5) . ?
C11 H28 0.9300 . ?
C10 H29 0.9300 . ?
C31 C32 1.510(5) . ?
C32 H31A 0.9600 . ?
C32 H31B 0.9600 . ?
C32 H31C 0.9600 . ?
C33 C34 1.451(8) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Ho1 O3 77.86(9) . . ?
O6 Ho1 O1 78.36(9) . . ?
O3 Ho1 O1 70.43(8) . . ?
O6 Ho1 O8 148.85(9) . . ?
O3 Ho1 O8 129.36(10) . . ?
O1 Ho1 O8 121.60(9) . . ?
O6 Ho1 O10 80.15(9) . . ?
O3 Ho1 O10 110.27(9) . . ?
O1 Ho1 O10 157.80(9) . . ?
O8 Ho1 O10 76.04(9) . . ?
O6 Ho1 O7 156.09(9) . . ?
O3 Ho1 O7 86.63(10) . . ?
O1 Ho1 O7 79.35(10) . . ?
O8 Ho1 O7 53.72(10) . . ?
O10 Ho1 O7 122.70(10) . . ?
O6 Ho1 O11 76.63(9) . . ?
O3 Ho1 O11 151.47(9) . . ?
O1 Ho1 O11 116.08(9) . . ?
O8 Ho1 O11 73.01(9) . . ?
O10 Ho1 O11 52.64(9) . . ?
O7 Ho1 O11 121.53(10) . . ?
O6 Ho1 O4 115.24(9) . . ?
O3 Ho1 O4 63.97(8) . . ?
O1 Ho1 O4 126.91(8) . . ?
O8 Ho1 O4 73.81(11) . . ?
O10 Ho1 O4 68.20(9) . . ?
O7 Ho1 O4 72.46(11) . . ?
O11 Ho1 O4 116.99(9) . . ?
O6 Ho1 O2 105.67(10) . . ?
O3 Ho1 O2 130.89(8) . . ?
O1 Ho1 O2 62.86(8) . . ?
O8 Ho1 O2 69.76(11) . . ?
O10 Ho1 O2 118.66(8) . . ?
O7 Ho1 O2 71.15(11) . . ?
O11 Ho1 O2 69.14(8) . . ?
O4 Ho1 O2 139.00(9) . . ?
O6 Ho1 N5 171.14(13) . . ?
O3 Ho1 N5 110.05(11) . . ?
O1 Ho1 N5 100.20(10) . . ?
O8 Ho1 N5 26.59(10) . . ?
O10 Ho1 N5 100.17(10) . . ?
O7 Ho1 N5 27.23(10) . . ?
O11 Ho1 N5 96.44(11) . . ?
O4 Ho1 N5 72.70(13) . . ?
O2 Ho1 N5 66.30(13) . . ?
O6 Ho1 N6 78.71(9) . . ?
O3 Ho1 N6 134.05(9) . . ?
O1 Ho1 N6 140.49(10) . . ?
O8 Ho1 N6 71.01(9) . . ?
O10 Ho1 N6 26.37(10) . . ?
O7 Ho1 N6 124.69(10) . . ?
O11 Ho1 N6 26.37(10) . . ?
O4 Ho1 N6 92.03(10) . . ?
O2 Ho1 N6 93.40(9) . . ?
N5 Ho1 N6 97.59(10) . . ?
C29 Fe1 C2 156.89(15) . . ?
C29 Fe1 C1 158.55(16) . . ?
C2 Fe1 C1 40.94(15) . . ?
C29 Fe1 C5 120.44(16) . . ?
C2 Fe1 C5 68.74(16) . . ?
C1 Fe1 C5 41.13(14) . . ?
C29 Fe1 C28 40.35(17) . . ?
C2 Fe1 C28 123.41(17) . . ?
C1 Fe1 C28 160.67(16) . . ?
C5 Fe1 C28 156.30(15) . . ?
C29 Fe1 C30 40.71(15) . . ?
C2 Fe1 C30 162.10(14) . . ?
C1 Fe1 C30 123.96(15) . . ?
C5 Fe1 C30 105.89(16) . . ?
C28 Fe1 C30 68.40(17) . . ?
C29 Fe1 C3 119.62(15) . . ?
C2 Fe1 C3 40.72(14) . . ?
C1 Fe1 C3 68.55(15) . . ?
C5 Fe1 C3 68.05(16) . . ?
C28 Fe1 C3 106.79(17) . . ?
C30 Fe1 C3 154.79(15) . . ?
C29 Fe1 C4 103.93(16) . . ?
C2 Fe1 C4 68.52(16) . . ?
C1 Fe1 C4 68.67(14) . . ?
C5 Fe1 C4 40.35(14) . . ?
C28 Fe1 C4 120.76(15) . . ?
C30 Fe1 C4 119.18(16) . . ?
C3 Fe1 C4 40.41(16) . . ?
C29 Fe1 C26 68.48(15) . . ?
C2 Fe1 C26 126.71(14) . . ?
C1 Fe1 C26 109.97(14) . . ?
C5 Fe1 C26 123.14(14) . . ?
C28 Fe1 C26 68.50(15) . . ?
C30 Fe1 C26 40.89(14) . . ?
C3 Fe1 C26 162.48(16) . . ?
C4 Fe1 C26 156.70(16) . . ?
C29 Fe1 C27 68.14(16) . . ?
C2 Fe1 C27 110.50(17) . . ?
C1 Fe1 C27 125.71(15) . . ?
C5 Fe1 C27 160.96(14) . . ?
C28 Fe1 C27 40.45(15) . . ?
C30 Fe1 C27 68.70(16) . . ?
C3 Fe1 C27 124.65(17) . . ?
C4 Fe1 C27 158.43(15) . . ?
C26 Fe1 C27 40.99(15) . . ?
O5 Ni1 O3 88.96(10) . . ?
O5 Ni1 O1 89.66(10) . . ?
O3 Ni1 O1 80.89(10) . . ?
O5 Ni1 N2 93.55(11) . . ?
O3 Ni1 N2 168.44(11) . . ?
O1 Ni1 N2 87.84(10) . . ?
O5 Ni1 O13 176.40(11) . . ?
O3 Ni1 O13 87.45(10) . . ?
O1 Ni1 O13 90.07(11) . . ?
N2 Ni1 O13 90.03(12) . . ?
O5 Ni1 N4 92.01(11) . . ?
O3 Ni1 N4 87.24(10) . . ?
O1 Ni1 N4 167.98(11) . . ?
N2 Ni1 N4 103.93(11) . . ?
O13 Ni1 N4 87.52(11) . . ?
C17 O4 C16 116.5(3) . . ?
C17 O4 Ho1 117.9(2) . . ?
C16 O4 Ho1 125.3(2) . . ?
C22 O3 Ni1 124.9(2) . . ?
C22 O3 Ho1 127.1(2) . . ?
Ni1 O3 Ho1 103.49(11) . . ?
C24 N3 N4 118.0(3) . . ?
C14 O1 Ni1 128.2(2) . . ?
C14 O1 Ho1 128.7(2) . . ?
Ni1 O1 Ho1 102.62(10) . . ?
C13 O2 C15 115.9(3) . . ?
C13 O2 Ho1 117.6(2) . . ?
C15 O2 Ho1 126.4(3) . . ?
O2 C15 H15A 109.5 . . ?
O2 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O2 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C31 O5 Ni1 129.6(2) . . ?
C31 O6 Ho1 135.0(2) . . ?
N5 O8 Ho1 95.9(2) . . ?
N5 O7 Ho1 93.2(2) . . ?
N6 O10 Ho1 95.6(2) . . ?
N6 O11 Ho1 93.5(2) . . ?
C6 N1 N2 115.5(3) . . ?
C23 N4 N3 111.5(3) . . ?
C23 N4 Ni1 121.0(2) . . ?
N3 N4 Ni1 124.3(2) . . ?
O1 C14 C9 124.4(3) . . ?
O1 C14 C13 118.2(3) . . ?
C9 C14 C13 117.3(3) . . ?
Ni1 O13 H1 125(4) . . ?
Ni1 O13 H100 124(4) . . ?
H1 O13 H100 105(5) . . ?
O11 N6 O10 117.8(3) . . ?
O11 N6 O12 121.1(4) . . ?
O10 N6 O12 121.1(4) . . ?
O11 N6 Ho1 60.11(17) . . ?
O10 N6 Ho1 58.03(17) . . ?
O12 N6 Ho1 173.5(3) . . ?
O4 C16 H1A 109.5 . . ?
O4 C16 H1B 109.5 . . ?
H1A C16 H1B 109.5 . . ?
O4 C16 H1C 109.5 . . ?
H1A C16 H1C 109.5 . . ?
H1B C16 H1C 109.5 . . ?
C18 C17 O4 125.4(3) . . ?
C18 C17 C22 122.1(4) . . ?
O4 C17 C22 112.5(3) . . ?
O3 C22 C21 124.9(3) . . ?
O3 C22 C17 117.8(3) . . ?
C21 C22 C17 117.3(3) . . ?
C8 N2 N1 112.1(3) . . ?
C8 N2 Ni1 125.6(2) . . ?
N1 N2 Ni1 121.8(2) . . ?
N1 C6 C1 116.9(3) . . ?
N1 C6 C7 125.5(3) . . ?
C1 C6 C7 117.6(3) . . ?
C6 C7 H6A 109.5 . . ?
C6 C7 H6B 109.5 . . ?
H6A C7 H6B 109.5 . . ?
C6 C7 H6C 109.5 . . ?
H6A C7 H6C 109.5 . . ?
H6B C7 H6C 109.5 . . ?
C2 C1 C5 107.3(3) . . ?
C2 C1 C6 126.7(3) . . ?
C5 C1 C6 126.0(3) . . ?
C2 C1 Fe1 69.5(2) . . ?
C5 C1 Fe1 69.5(2) . . ?
C6 C1 Fe1 126.5(3) . . ?
C3 C2 C1 107.8(3) . . ?
C3 C2 Fe1 69.9(2) . . ?
C1 C2 Fe1 69.5(2) . . ?
C3 C2 H8 126.1 . . ?
C1 C2 H8 126.1 . . ?
Fe1 C2 H8 126.0 . . ?
C4 C3 C2 108.4(3) . . ?
C4 C3 Fe1 69.8(2) . . ?
C2 C3 Fe1 69.4(2) . . ?
C4 C3 H9 125.8 . . ?
C2 C3 H9 125.8 . . ?
Fe1 C3 H9 126.6 . . ?
C5 C4 C3 108.2(3) . . ?
C5 C4 Fe1 69.6(2) . . ?
C3 C4 Fe1 69.8(2) . . ?
C5 C4 H10 125.9 . . ?
C3 C4 H10 125.9 . . ?
Fe1 C4 H10 126.3 . . ?
C4 C5 C1 108.3(3) . . ?
C4 C5 Fe1 70.0(2) . . ?
C1 C5 Fe1 69.3(2) . . ?
C4 C5 H11 125.9 . . ?
C1 C5 H11 125.9 . . ?
Fe1 C5 H11 126.4 . . ?
C28 C29 C30 108.7(3) . . ?
C28 C29 Fe1 70.1(2) . . ?
C30 C29 Fe1 69.9(2) . . ?
C28 C29 H12 125.6 . . ?
C30 C29 H12 125.6 . . ?
Fe1 C29 H12 125.9 . . ?
C29 C28 C27 108.5(3) . . ?
C29 C28 Fe1 69.6(2) . . ?
C27 C28 Fe1 70.1(2) . . ?
C29 C28 H13 125.8 . . ?
C27 C28 H13 125.8 . . ?
Fe1 C28 H13 126.1 . . ?
C28 C27 C26 107.7(3) . . ?
C28 C27 Fe1 69.4(2) . . ?
C26 C27 Fe1 69.3(2) . . ?
C28 C27 H14 126.2 . . ?
C26 C27 H14 126.2 . . ?
Fe1 C27 H14 126.7 . . ?
C30 C26 C27 107.6(3) . . ?
C30 C26 C24 126.9(3) . . ?
C27 C26 C24 125.5(3) . . ?
C30 C26 Fe1 69.5(2) . . ?
C27 C26 Fe1 69.7(2) . . ?
C24 C26 Fe1 127.1(3) . . ?
C29 C30 C26 107.5(4) . . ?
C29 C30 Fe1 69.4(2) . . ?
C26 C30 Fe1 69.6(2) . . ?
C29 C30 H16 126.2 . . ?
C26 C30 H16 126.2 . . ?
Fe1 C30 H16 126.3 . . ?
N3 C24 C26 117.4(3) . . ?
N3 C24 C25 125.5(3) . . ?
C26 C24 C25 117.0(3) . . ?
N4 C23 C21 127.6(3) . . ?
N4 C23 H18 116.2 . . ?
C21 C23 H18 116.2 . . ?
C20 C21 C22 119.7(3) . . ?
C20 C21 C23 117.0(3) . . ?
C22 C21 C23 123.2(3) . . ?
C19 C20 C21 121.1(4) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 H20 119.4 . . ?
C20 C19 C18 120.1(4) . . ?
C20 C19 H21 120.0 . . ?
C18 C19 H21 120.0 . . ?
C17 C18 C19 119.7(4) . . ?
C17 C18 H22 120.1 . . ?
C19 C18 H22 120.1 . . ?
C24 C25 H23A 109.5 . . ?
C24 C25 H23B 109.5 . . ?
H23A C25 H23B 109.5 . . ?
C24 C25 H23C 109.5 . . ?
H23A C25 H23C 109.5 . . ?
H23B C25 H23C 109.5 . . ?
N2 C8 C9 127.4(3) . . ?
N2 C8 H24 116.3 . . ?
C9 C8 H24 116.3 . . ?
C14 C9 C10 119.5(3) . . ?
C14 C9 C8 123.2(3) . . ?
C10 C9 C8 117.1(3) . . ?
C12 C13 O2 125.4(3) . . ?
C12 C13 C14 122.3(4) . . ?
O2 C13 C14 112.3(3) . . ?
C13 C12 C11 119.6(3) . . ?
C13 C12 H27 120.2 . . ?
C11 C12 H27 120.2 . . ?
C10 C11 C12 120.1(4) . . ?
C10 C11 H28 119.9 . . ?
C12 C11 H28 119.9 . . ?
C11 C10 C9 121.1(4) . . ?
C11 C10 H29 119.5 . . ?
C9 C10 H29 119.5 . . ?
O5 C31 O6 125.5(3) . . ?
O5 C31 C32 116.5(3) . . ?
O6 C31 C32 118.0(3) . . ?
C31 C32 H31A 109.5 . . ?
C31 C32 H31B 109.5 . . ?
H31A C32 H31B 109.5 . . ?
C31 C32 H31C 109.5 . . ?
H31A C32 H31C 109.5 . . ?
H31B C32 H31C 109.5 . . ?
O9 N5 O8 121.7(4) . . ?
O9 N5 O7 121.3(4) . . ?
O8 N5 O7 116.8(4) . . ?
O9 N5 Ho1 170.3(5) . . ?
O8 N5 Ho1 57.53(19) . . ?
O7 N5 Ho1 59.6(2) . . ?
N7 C33 C34 179.4(6) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.244
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.121
_database_code_depnum_ccdc_archive 'CCDC 993946'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_NiGd

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H33 Fe Gd N6 Ni O13, C2 H3 N'
_chemical_formula_sum            'C34 H36 Fe Gd N7 Ni O13'
_chemical_formula_weight         1022.49

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'
Fe Fe 0.3463 0.8444 '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                   12.377(5)
_cell_length_b                   12.390(5)
_cell_length_c                   12.485(5)
_cell_angle_alpha                91.923(5)
_cell_angle_beta                 98.147(5)
_cell_angle_gamma                100.163(5)
_cell_volume                     1862.2(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3281
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      27.92

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1023.44
_exptl_absorpt_coefficient_mu    2.721
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.728406
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9993
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         25.50
_reflns_number_total             6767
_reflns_number_gt                5575
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0542P)²+2.9447P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6767
_refine_ls_number_parameters     504
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.1206
_refine_ls_wR_factor_gt          0.1128
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.91221(3) 0.23247(3) 0.24975(3) 0.02912(12) Uani 1 1 d . . .
Ni1 Ni 0.67940(6) 0.03585(6) 0.16399(6) 0.02062(19) Uani 1 1 d . . .
Fe1 Fe 0.35918(7) -0.38990(7) 0.16558(7) 0.0271(2) Uani 1 1 d . . .
O10 O 1.0342(4) 0.3057(4) 0.4245(4) 0.0409(6) Uani 1 1 d . . .
O6 O 0.9048(3) 0.0786(3) 0.3519(3) 0.0279(10) Uani 1 1 d . . .
O2 O 1.0050(3) 0.2197(4) 0.0822(4) 0.0329(11) Uani 1 1 d . . .
O3 O 0.7216(3) 0.1802(3) 0.2574(3) 0.0275(10) Uani 1 1 d . . .
O8 O 0.9949(4) 0.4220(4) 0.2235(4) 0.0498(15) Uani 1 1 d . . .
O13 O 0.6155(3) 0.1203(3) 0.0344(3) 0.0242(9) Uani 1 1 d D . .
H13 H 0.6315 0.0964 -0.0222 0.036 Uiso 1 1 calc RD . .
O4 O 0.8178(4) 0.3676(4) 0.3533(4) 0.0374(12) Uani 1 1 d . . .
O5 O 0.7495(3) -0.0421(3) 0.2872(3) 0.0236(9) Uani 1 1 d . . .
O1 O 0.8327(3) 0.0883(3) 0.1223(3) 0.0248(9) Uani 1 1 d . . .
N1 N 0.5766(4) -0.1962(4) 0.0436(4) 0.0257(12) Uani 1 1 d . . .
O11 O 1.1139(4) 0.2381(4) 0.2983(4) 0.0409(6) Uani 1 1 d . . .
C17 C 0.7036(6) 0.3437(5) 0.3490(5) 0.0315(15) Uani 1 1 d . . .
C21 C 0.5421(5) 0.2024(5) 0.2975(5) 0.0246(13) Uani 1 1 d . . .
C13 C 0.9531(5) 0.1431(5) -0.0019(5) 0.0291(15) Uani 1 1 d . . .
C33 C 0.7671(7) 0.0873(11) 0.5779(6) 0.064(3) Uani 1 1 d . . .
O7 O 0.8347(5) 0.3527(5) 0.1171(5) 0.0622(16) Uani 1 1 d . . .
N4 N 0.5272(4) 0.0147(4) 0.2185(4) 0.0217(11) Uani 1 1 d . . .
C24 C 0.4447(5) -0.1519(5) 0.2738(5) 0.0245(13) Uani 1 1 d . . .
N2 N 0.6644(4) -0.1022(4) 0.0533(4) 0.0229(11) Uani 1 1 d . . .
N3 N 0.4474(4) -0.0858(4) 0.1959(4) 0.0231(11) Uani 1 1 d . . .
C6 C 0.5902(5) -0.2750(5) 0.1053(5) 0.0244(13) Uani 1 1 d . . .
C14 C 0.8609(5) 0.0723(5) 0.0252(5) 0.0245(13) Uani 1 1 d . . .
C9 C 0.8042(5) -0.0111(5) -0.0519(5) 0.0282(14) Uani 1 1 d . . .
C19 C 0.5270(6) 0.3733(5) 0.3862(5) 0.0362(16) Uani 1 1 d . . .
H19 H 0.4837 0.4189 0.4132 0.043 Uiso 1 1 calc R . .
C27 C 0.3496(5) -0.3428(5) 0.3221(5) 0.0309(15) Uani 1 1 d . . .
H27 H 0.4019 -0.3524 0.3862 0.037 Uiso 1 1 calc R . .
O12 O 1.2196(4) 0.3234(4) 0.4491(4) 0.0409(6) Uani 1 1 d . . .
C1 C 0.4991(5) -0.3719(5) 0.0926(5) 0.0286(14) Uani 1 1 d . . .
C28 C 0.2524(6) -0.4204(6) 0.2765(6) 0.0376(17) Uani 1 1 d . . .
H28 H 0.2263 -0.4920 0.3040 0.045 Uiso 1 1 calc R . .
C31 C 0.8423(6) -0.0148(5) 0.3465(5) 0.0292(15) Uani 1 1 d . . .
C20 C 0.4784(6) 0.2703(5) 0.3411(5) 0.0328(15) Uani 1 1 d . . .
H20 H 0.4027 0.2458 0.3397 0.039 Uiso 1 1 calc R . .
C30 C 0.2651(5) -0.2717(5) 0.1711(5) 0.0276(14) Uani 1 1 d . . .
H30 H 0.2488 -0.2227 0.1133 0.033 Uiso 1 1 calc R . .
C12 C 0.9884(5) 0.1331(6) -0.1005(6) 0.0400(18) Uani 1 1 d . . .
H12A H 1.0493 0.1819 -0.1168 0.048 Uiso 1 1 calc R . .
C26 C 0.3582(5) -0.2505(5) 0.2568(5) 0.0250(14) Uani 1 1 d . . .
C10 C 0.8415(5) -0.0211(6) -0.1516(5) 0.0302(15) Uani 1 1 d . . .
H10 H 0.8042 -0.0766 -0.2025 0.036 Uiso 1 1 calc R . .
C11 C 0.9325(5) 0.0495(6) -0.1761(6) 0.0390(18) Uani 1 1 d . . .
H11 H 0.9565 0.0414 -0.2428 0.047 Uiso 1 1 calc R . .
C4 C 0.3391(6) -0.4947(5) 0.0328(6) 0.0379(17) Uani 1 1 d . . .
H4 H 0.2679 -0.5296 -0.0095 0.046 Uiso 1 1 calc R . .
C22 C 0.6565(5) 0.2380(5) 0.2984(5) 0.0242(14) Uani 1 1 d . . .
O9 O 0.9080(6) 0.5315(5) 0.1261(7) 0.104(3) Uani 1 1 d . . .
C7 C 0.6920(5) -0.2803(5) 0.1844(5) 0.0314(15) Uani 1 1 d . . .
H7A H 0.7234 -0.3420 0.1640 0.047 Uiso 1 1 calc R . .
H7B H 0.6724 -0.2883 0.2557 0.047 Uiso 1 1 calc R . .
H7C H 0.7453 -0.2139 0.1840 0.047 Uiso 1 1 calc R . .
C18 C 0.6411(6) 0.4098(6) 0.3916(6) 0.0363(17) Uani 1 1 d . . .
H18 H 0.6742 0.4786 0.4241 0.044 Uiso 1 1 calc R . .
C5 C 0.4028(6) -0.3905(5) 0.0145(5) 0.0318(15) Uani 1 1 d . . .
H5 H 0.3835 -0.3417 -0.0425 0.038 Uiso 1 1 calc R . .
C15 C 1.1017(6) 0.2958(6) 0.0612(6) 0.0421(19) Uani 1 1 d . . .
H15A H 1.1528 0.2557 0.0340 0.063 Uiso 1 1 calc R . .
H15B H 1.1372 0.3368 0.1273 0.063 Uiso 1 1 calc R . .
H15C H 1.0794 0.3454 0.0086 0.063 Uiso 1 1 calc R . .
C29 C 0.2008(6) -0.3749(6) 0.1850(6) 0.0347(16) Uani 1 1 d . . .
H29 H 0.1330 -0.4102 0.1375 0.042 Uiso 1 1 calc R . .
C16 C 0.8732(6) 0.4714(6) 0.4098(8) 0.062(3) Uani 1 1 d . . .
H16A H 0.8467 0.5308 0.3733 0.093 Uiso 1 1 calc R . .
H16B H 0.9518 0.4792 0.4105 0.093 Uiso 1 1 calc R . .
H16C H 0.8575 0.4727 0.4829 0.093 Uiso 1 1 calc R . .
C3 C 0.3956(6) -0.5381(6) 0.1230(6) 0.0414(18) Uani 1 1 d . . .
H3 H 0.3707 -0.6082 0.1541 0.050 Uiso 1 1 calc R . .
C8 C 0.7136(5) -0.0953(5) -0.0310(5) 0.0240(13) Uani 1 1 d . . .
H8 H 0.6880 -0.1511 -0.0850 0.029 Uiso 1 1 calc R . .
C23 C 0.4858(5) 0.0889(5) 0.2616(5) 0.0270(14) Uani 1 1 d . . .
H23 H 0.4121 0.0698 0.2719 0.032 Uiso 1 1 calc R . .
N5 N 0.9165(6) 0.4421(7) 0.1529(7) 0.078(3) Uani 1 1 d . . .
C34 C 0.8339(9) 0.1944(8) 0.5751(7) 0.069(3) Uani 1 1 d . . .
H34A H 0.8604 0.2246 0.6478 0.103 Uiso 1 1 calc R . .
H34B H 0.7899 0.2417 0.5372 0.103 Uiso 1 1 calc R . .
H34C H 0.8959 0.1884 0.5384 0.103 Uiso 1 1 calc R . .
N6 N 1.1220(5) 0.2883(5) 0.3908(5) 0.0409(6) Uani 1 1 d . . .
C25 C 0.5199(5) -0.1330(5) 0.3811(5) 0.0305(15) Uani 1 1 d . . .
H25A H 0.5863 -0.0821 0.3738 0.046 Uiso 1 1 calc R . .
H25B H 0.5390 -0.2015 0.4035 0.046 Uiso 1 1 calc R . .
H25C H 0.4825 -0.1034 0.4343 0.046 Uiso 1 1 calc R . .
N7 N 0.7146(7) 0.0030(9) 0.5804(6) 0.081(3) Uani 1 1 d . . .
C2 C 0.4948(6) -0.4625(5) 0.1602(6) 0.0367(16) Uani 1 1 d . . .
H2 H 0.5504 -0.4706 0.2222 0.044 Uiso 1 1 calc R . .
C32 C 0.8798(7) -0.1002(6) 0.4174(6) 0.050(2) Uani 1 1 d . . .
H32A H 0.8181 -0.1384 0.4480 0.075 Uiso 1 1 calc R . .
H32B H 0.9368 -0.0655 0.4746 0.075 Uiso 1 1 calc R . .
H32C H 0.9087 -0.1514 0.3750 0.075 Uiso 1 1 calc R . .
H100 H 0.5586 0.1535 0.0431 0.03(2) Uiso 1 1 d RD . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O6 2.325(4) . ?
Gd1 O1 2.331(4) . ?
Gd1 O3 2.350(4) . ?
Gd1 O8 2.442(5) . ?
Gd1 O7 2.471(6) . ?
Gd1 O11 2.472(5) . ?
Gd1 O10 2.513(5) . ?
Gd1 O2 2.538(4) . ?
Gd1 O4 2.610(5) . ?
Gd1 N6 2.883(6) . ?
Gd1 N5 2.896(8) . ?
Gd1 Ni1 3.4435(12) . ?
Ni1 O5 2.017(4) . ?
Ni1 O1 2.039(4) . ?
Ni1 O3 2.047(4) . ?
Ni1 N4 2.069(5) . ?
Ni1 O13 2.094(4) . ?
Ni1 N2 2.127(5) . ?
Fe1 C4 2.030(6) . ?
Fe1 C30 2.031(7) . ?
Fe1 C5 2.034(7) . ?
Fe1 C3 2.038(7) . ?
Fe1 C26 2.039(6) . ?
Fe1 C28 2.046(7) . ?
Fe1 C27 2.046(6) . ?
Fe1 C1 2.049(6) . ?
Fe1 C29 2.048(7) . ?
Fe1 C2 2.047(7) . ?
O10 N6 1.269(7) . ?
O6 C31 1.267(7) . ?
O2 C13 1.393(8) . ?
O2 C15 1.449(7) . ?
O3 C22 1.311(7) . ?
O8 N5 1.280(9) . ?
O4 C17 1.385(8) . ?
O4 C16 1.454(8) . ?
O5 C31 1.259(7) . ?
O1 C14 1.326(7) . ?
N1 C6 1.283(8) . ?
N1 N2 1.435(6) . ?
O11 N6 1.276(7) . ?
C17 C18 1.365(9) . ?
C17 C22 1.423(8) . ?
C21 C20 1.397(9) . ?
C21 C22 1.405(9) . ?
C21 C23 1.478(8) . ?
C13 C12 1.373(9) . ?
C13 C14 1.401(8) . ?
C33 N7 1.132(13) . ?
C33 C34 1.438(14) . ?
O7 N5 1.376(9) . ?
N4 C23 1.268(8) . ?
N4 N3 1.438(6) . ?
C24 N3 1.292(8) . ?
C24 C26 1.464(8) . ?
C24 C25 1.505(9) . ?
N2 C8 1.286(7) . ?
C6 C1 1.482(8) . ?
C6 C7 1.499(9) . ?
C14 C9 1.405(9) . ?
C9 C10 1.397(9) . ?
C9 C8 1.450(8) . ?
C19 C20 1.376(9) . ?
C19 C18 1.395(10) . ?
C27 C26 1.425(9) . ?
C27 C28 1.434(9) . ?
O12 N6 1.312(7) . ?
C1 C5 1.408(9) . ?
C1 C2 1.425(9) . ?
C28 C29 1.412(10) . ?
C31 C32 1.496(10) . ?
C30 C29 1.412(8) . ?
C30 C26 1.438(9) . ?
C12 C11 1.393(10) . ?
C10 C11 1.377(9) . ?
C4 C3 1.413(11) . ?
C4 C5 1.433(9) . ?
O9 N5 1.186(10) . ?
C3 C2 1.416(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Gd1 O1 76.78(14) . . ?
O6 Gd1 O3 77.00(15) . . ?
O1 Gd1 O3 69.45(14) . . ?
O6 Gd1 O8 149.98(15) . . ?
O1 Gd1 O8 129.98(16) . . ?
O3 Gd1 O8 121.61(16) . . ?
O6 Gd1 O7 154.45(17) . . ?
O1 Gd1 O7 85.94(18) . . ?
O3 Gd1 O7 79.38(17) . . ?
O8 Gd1 O7 54.20(18) . . ?
O6 Gd1 O11 81.53(15) . . ?
O1 Gd1 O11 110.94(15) . . ?
O3 Gd1 O11 157.84(16) . . ?
O8 Gd1 O11 76.08(16) . . ?
O7 Gd1 O11 122.69(18) . . ?
O6 Gd1 O10 77.23(15) . . ?
O1 Gd1 O10 150.95(16) . . ?
O3 Gd1 O10 116.53(15) . . ?
O8 Gd1 O10 73.29(16) . . ?
O7 Gd1 O10 122.77(19) . . ?
O11 Gd1 O10 52.14(16) . . ?
O6 Gd1 O2 114.52(15) . . ?
O1 Gd1 O2 63.41(13) . . ?
O3 Gd1 O2 125.93(14) . . ?
O8 Gd1 O2 75.42(17) . . ?
O7 Gd1 O2 72.55(18) . . ?
O11 Gd1 O2 68.58(15) . . ?
O10 Gd1 O2 117.53(15) . . ?
O6 Gd1 O4 104.93(15) . . ?
O1 Gd1 O4 129.74(14) . . ?
O3 Gd1 O4 62.51(14) . . ?
O8 Gd1 O4 70.13(18) . . ?
O7 Gd1 O4 71.99(18) . . ?
O11 Gd1 O4 119.06(15) . . ?
O10 Gd1 O4 70.03(15) . . ?
O2 Gd1 O4 140.55(15) . . ?
O6 Gd1 N6 79.61(15) . . ?
O1 Gd1 N6 134.16(16) . . ?
O3 Gd1 N6 140.55(16) . . ?
O8 Gd1 N6 71.45(16) . . ?
O7 Gd1 N6 125.56(19) . . ?
O11 Gd1 N6 26.16(16) . . ?
O10 Gd1 N6 26.06(16) . . ?
O2 Gd1 N6 92.66(16) . . ?
O4 Gd1 N6 94.08(16) . . ?
O6 Gd1 N5 171.1(2) . . ?
O1 Gd1 N5 110.7(2) . . ?
O3 Gd1 N5 100.79(19) . . ?
O8 Gd1 N5 26.00(17) . . ?
O7 Gd1 N5 28.3(2) . . ?
O11 Gd1 N5 99.58(19) . . ?
O10 Gd1 N5 96.4(2) . . ?
O2 Gd1 N5 73.9(2) . . ?
O4 Gd1 N5 66.7(2) . . ?
N6 Gd1 N5 97.45(19) . . ?
O6 Gd1 Ni1 67.39(10) . . ?
O1 Gd1 Ni1 35.12(10) . . ?
O3 Gd1 Ni1 35.42(10) . . ?
O8 Gd1 Ni1 141.75(11) . . ?
O7 Gd1 Ni1 87.65(15) . . ?
O11 Gd1 Ni1 136.98(11) . . ?
O10 Gd1 Ni1 138.27(11) . . ?
O2 Gd1 Ni1 97.40(10) . . ?
O4 Gd1 Ni1 97.86(10) . . ?
N6 Gd1 Ni1 146.78(12) . . ?
N5 Gd1 Ni1 115.75(15) . . ?
O5 Ni1 O1 89.41(16) . . ?
O5 Ni1 O3 89.69(17) . . ?
O1 Ni1 O3 81.48(17) . . ?
O5 Ni1 N4 93.50(18) . . ?
O1 Ni1 N4 168.50(18) . . ?
O3 Ni1 N4 87.41(18) . . ?
O5 Ni1 O13 176.82(16) . . ?
O1 Ni1 O13 87.42(16) . . ?
O3 Ni1 O13 89.57(17) . . ?
N4 Ni1 O13 89.55(18) . . ?
O5 Ni1 N2 92.03(18) . . ?
O1 Ni1 N2 87.26(18) . . ?
O3 Ni1 N2 168.60(18) . . ?
N4 Ni1 N2 103.73(19) . . ?
O13 Ni1 N2 88.10(18) . . ?
O5 Ni1 Gd1 81.20(11) . . ?
O1 Ni1 Gd1 41.12(12) . . ?
O3 Ni1 Gd1 41.71(12) . . ?
N4 Ni1 Gd1 128.47(14) . . ?
O13 Ni1 Gd1 96.20(11) . . ?
N2 Ni1 Gd1 127.55(13) . . ?
C4 Fe1 C30 120.9(3) . . ?
C4 Fe1 C5 41.3(2) . . ?
C30 Fe1 C5 105.9(3) . . ?
C4 Fe1 C3 40.7(3) . . ?
C30 Fe1 C3 156.9(3) . . ?
C5 Fe1 C3 69.1(3) . . ?
C4 Fe1 C26 159.3(3) . . ?
C30 Fe1 C26 41.4(2) . . ?
C5 Fe1 C26 123.9(2) . . ?
C3 Fe1 C26 159.6(3) . . ?
C4 Fe1 C28 119.1(3) . . ?
C30 Fe1 C28 68.6(3) . . ?
C5 Fe1 C28 155.0(3) . . ?
C3 Fe1 C28 105.9(3) . . ?
C26 Fe1 C28 69.1(2) . . ?
C4 Fe1 C27 156.5(3) . . ?
C30 Fe1 C27 68.8(3) . . ?
C5 Fe1 C27 161.8(2) . . ?
C3 Fe1 C27 122.7(3) . . ?
C26 Fe1 C27 40.8(2) . . ?
C28 Fe1 C27 41.0(2) . . ?
C4 Fe1 C1 68.2(3) . . ?
C30 Fe1 C1 123.1(2) . . ?
C5 Fe1 C1 40.4(3) . . ?
C3 Fe1 C1 68.5(3) . . ?
C26 Fe1 C1 110.1(2) . . ?
C28 Fe1 C1 162.5(3) . . ?
C27 Fe1 C1 126.9(3) . . ?
C4 Fe1 C29 104.3(3) . . ?
C30 Fe1 C29 40.5(2) . . ?
C5 Fe1 C29 119.7(3) . . ?
C3 Fe1 C29 121.0(3) . . ?
C26 Fe1 C29 68.7(3) . . ?
C28 Fe1 C29 40.4(3) . . ?
C27 Fe1 C29 68.3(3) . . ?
C1 Fe1 C29 156.9(3) . . ?
C4 Fe1 C2 68.2(3) . . ?
C30 Fe1 C2 160.4(2) . . ?
C5 Fe1 C2 68.6(3) . . ?
C3 Fe1 C2 40.6(3) . . ?
C26 Fe1 C2 125.0(3) . . ?
C28 Fe1 C2 124.5(3) . . ?
C27 Fe1 C2 110.3(3) . . ?
C1 Fe1 C2 40.7(3) . . ?
C29 Fe1 C2 158.7(3) . . ?
N6 O10 Gd1 93.5(4) . . ?
C31 O6 Gd1 135.4(4) . . ?
C13 O2 C15 116.6(5) . . ?
C13 O2 Gd1 118.6(3) . . ?
C15 O2 Gd1 124.4(4) . . ?
C22 O3 Ni1 128.8(4) . . ?
C22 O3 Gd1 127.7(3) . . ?
Ni1 O3 Gd1 102.87(18) . . ?
N5 O8 Gd1 97.2(4) . . ?
C17 O4 C16 115.7(6) . . ?
C17 O4 Gd1 118.2(4) . . ?
C16 O4 Gd1 125.9(4) . . ?
C31 O5 Ni1 129.6(4) . . ?
C14 O1 Ni1 125.3(4) . . ?
C14 O1 Gd1 126.6(3) . . ?
Ni1 O1 Gd1 103.77(17) . . ?
C6 N1 N2 117.7(5) . . ?
N6 O11 Gd1 95.2(4) . . ?
C18 C17 O4 125.4(6) . . ?
C18 C17 C22 122.3(6) . . ?
O4 C17 C22 112.3(6) . . ?
C20 C21 C22 120.7(6) . . ?
C20 C21 C23 116.7(6) . . ?
C22 C21 C23 122.3(6) . . ?
C12 C13 O2 125.0(6) . . ?
C12 C13 C14 122.0(6) . . ?
O2 C13 C14 113.0(5) . . ?
N7 C33 C34 179.7(11) . . ?
N5 O7 Gd1 93.3(4) . . ?
C23 N4 N3 111.1(5) . . ?
C23 N4 Ni1 126.2(4) . . ?
N3 N4 Ni1 122.1(4) . . ?
N3 C24 C26 116.7(5) . . ?
N3 C24 C25 125.3(5) . . ?
C26 C24 C25 118.0(5) . . ?
C8 N2 N1 111.8(5) . . ?
C8 N2 Ni1 121.2(4) . . ?
N1 N2 Ni1 124.3(4) . . ?
C24 N3 N4 115.4(5) . . ?
N1 C6 C1 116.7(6) . . ?
N1 C6 C7 125.9(5) . . ?
C1 C6 C7 117.3(5) . . ?
O1 C14 C13 117.8(5) . . ?
O1 C14 C9 124.2(5) . . ?
C13 C14 C9 118.1(6) . . ?
C10 C9 C14 119.4(6) . . ?
C10 C9 C8 116.7(6) . . ?
C14 C9 C8 123.6(6) . . ?
C20 C19 C18 120.3(7) . . ?
C26 C27 C28 108.2(6) . . ?
C26 C27 Fe1 69.3(3) . . ?
C28 C27 Fe1 69.5(4) . . ?
C5 C1 C2 108.4(6) . . ?
C5 C1 C6 126.9(6) . . ?
C2 C1 C6 124.7(6) . . ?
C5 C1 Fe1 69.2(4) . . ?
C2 C1 Fe1 69.6(4) . . ?
C6 C1 Fe1 126.5(4) . . ?
C29 C28 C27 107.7(6) . . ?
C29 C28 Fe1 69.9(4) . . ?
C27 C28 Fe1 69.5(4) . . ?
O5 C31 O6 125.5(6) . . ?
O5 C31 C32 116.5(6) . . ?
O6 C31 C32 118.0(6) . . ?
C19 C20 C21 120.4(6) . . ?
C29 C30 C26 108.2(6) . . ?
C29 C30 Fe1 70.4(4) . . ?
C26 C30 Fe1 69.6(4) . . ?
C13 C12 C11 119.6(6) . . ?
C27 C26 C30 107.2(5) . . ?
C27 C26 C24 126.7(6) . . ?
C30 C26 C24 126.1(6) . . ?
C27 C26 Fe1 69.9(4) . . ?
C30 C26 Fe1 69.0(4) . . ?
C24 C26 Fe1 126.7(4) . . ?
C11 C10 C9 121.3(6) . . ?
C10 C11 C12 119.6(6) . . ?
C3 C4 C5 108.5(6) . . ?
C3 C4 Fe1 70.0(4) . . ?
C5 C4 Fe1 69.5(4) . . ?
O3 C22 C21 124.5(5) . . ?
O3 C22 C17 118.7(6) . . ?
C21 C22 C17 116.8(6) . . ?
C17 C18 C19 119.5(6) . . ?
C1 C5 C4 107.3(6) . . ?
C1 C5 Fe1 70.4(4) . . ?
C4 C5 Fe1 69.2(4) . . ?
C30 C29 C28 108.8(6) . . ?
C30 C29 Fe1 69.1(4) . . ?
C28 C29 Fe1 69.7(4) . . ?
C4 C3 C2 107.7(6) . . ?
C4 C3 Fe1 69.4(4) . . ?
C2 C3 Fe1 70.1(4) . . ?
N2 C8 C9 127.9(5) . . ?
N4 C23 C21 127.1(6) . . ?
O9 N5 O8 123.8(8) . . ?
O9 N5 O7 121.1(8) . . ?
O8 N5 O7 114.8(7) . . ?
O9 N5 Gd1 169.0(8) . . ?
O8 N5 Gd1 56.8(4) . . ?
O7 N5 Gd1 58.4(4) . . ?
O10 N6 O11 118.9(5) . . ?
O10 N6 O12 120.6(6) . . ?
O11 N6 O12 120.5(6) . . ?
O10 N6 Gd1 60.5(3) . . ?
O11 N6 Gd1 58.7(3) . . ?
O12 N6 Gd1 173.8(4) . . ?
C3 C2 C1 108.1(6) . . ?
C3 C2 Fe1 69.4(4) . . ?
C1 C2 Fe1 69.7(4) . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         1.322
_refine_diff_density_min         -1.529
_refine_diff_density_rms         0.135
_database_code_depnum_ccdc_archive 'CCDC 993947'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_NiEr

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H33 Er Fe N6 Ni O13, C2 H3 N'
_chemical_formula_sum            'C34 H36 Er Fe N7 Ni O13'
_chemical_formula_weight         1032.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Fe Fe 0.3463 0.8444 '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'
Er Er -0.2586 4.9576 '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                   12.262(5)
_cell_length_b                   12.365(5)
_cell_length_c                   12.503(5)
_cell_angle_alpha                98.072(5)
_cell_angle_beta                 92.025(5)
_cell_angle_gamma                100.116(5)
_cell_volume                     1844.2(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2541
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      26.30

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1030
_exptl_absorpt_coefficient_mu    3.225
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.649764
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9813
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0753
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.16
_diffrn_reflns_theta_max         25.50
_reflns_number_total             6710
_reflns_number_gt                5112
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0934P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6710
_refine_ls_number_parameters     523
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.1579
_refine_ls_wR_factor_gt          0.1302
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.26912(3) 0.08990(3) 0.75103(3) 0.02699(16) Uani 1 1 d . . .
Ni1 Ni 0.46354(8) 0.32061(8) 0.83600(8) 0.0196(2) Uani 1 1 d . . .
Fe1 Fe 0.89167(10) 0.64171(10) 0.83346(10) 0.0256(3) Uani 1 1 d . . .
O1 O 0.4110(5) 0.1671(4) 0.8762(5) 0.0278(14) Uani 1 1 d . . .
O2 O 0.2789(4) -0.0054(4) 0.9156(5) 0.0267(14) Uani 1 1 d . . .
O7 O 0.1515(6) 0.1645(6) 0.8805(6) 0.052(2) Uani 1 1 d . . .
O8 O 0.0838(5) 0.0053(5) 0.7776(6) 0.0416(18) Uani 1 1 d . . .
O9 O -0.0274(7) 0.0887(7) 0.8772(9) 0.091(4) Uani 1 1 d . . .
O11 O 0.2668(5) -0.1075(5) 0.7034(5) 0.0307(14) Uani 1 1 d . . .
O12 O 0.1797(7) -0.2127(6) 0.5546(6) 0.062(2) Uani 1 1 d . . .
O10 O 0.1934(5) -0.0274(5) 0.5796(5) 0.0314(14) Uani 1 1 d . . .
O4 O 0.1287(5) 0.1803(5) 0.6492(5) 0.0335(15) Uani 1 1 d . . .
O3 O 0.3171(5) 0.2767(4) 0.7428(5) 0.0269(13) Uani 1 1 d . . .
O6 O 0.4194(4) 0.0951(4) 0.6496(5) 0.0262(13) Uani 1 1 d . . .
O5 O 0.5409(4) 0.2509(4) 0.7133(4) 0.0246(13) Uani 1 1 d . . .
O13 O 0.3816(4) 0.3843(4) 0.9660(4) 0.0223(12) Uani 1 1 d D . .
N1 N 0.6961(5) 0.4235(5) 0.9572(6) 0.0245(16) Uani 1 1 d . . .
N2 N 0.6035(5) 0.3348(5) 0.9473(5) 0.0231(15) Uani 1 1 d . . .
N6 N 0.2155(6) -0.1152(7) 0.6102(6) 0.038(2) Uani 1 1 d . . .
N5 N 0.0621(8) 0.0847(7) 0.8479(9) 0.060(3) Uani 1 1 d . . .
N4 N 0.4841(6) 0.4732(6) 0.7804(5) 0.0240(16) Uani 1 1 d . . .
N3 N 0.5850(5) 0.5526(5) 0.8023(5) 0.0189(14) Uani 1 1 d . . .
N7 N 0.4944(10) 0.2844(8) 0.4191(8) 0.060(3) Uani 1 1 d . . .
C1 C 0.8930(7) 0.6004(7) 0.9854(7) 0.0277(19) Uani 1 1 d . . .
H1 H 0.8440 0.6207 1.0421 0.033 Uiso 1 1 calc R . .
C2 C 0.9983(8) 0.6633(8) 0.9669(8) 0.037(2) Uani 1 1 d . . .
H2 H 1.0341 0.7347 1.0084 0.044 Uiso 1 1 calc R . .
C3 C 1.0392(7) 0.6074(8) 0.8788(9) 0.038(2) Uani 1 1 d . . .
H3 H 1.1095 0.6335 0.8476 0.046 Uiso 1 1 calc R . .
C4 C 0.9674(6) 0.5063(8) 0.8413(8) 0.033(2) Uani 1 1 d . . .
H4 H 0.9782 0.4509 0.7803 0.039 Uiso 1 1 calc R . .
C5 C 0.8730(7) 0.5014(7) 0.9068(7) 0.0265(19) Uani 1 1 d . . .
C6 C 0.7753(7) 0.4107(6) 0.8945(7) 0.0232(18) Uani 1 1 d . . .
C7 C 0.7823(7) 0.3094(7) 0.8154(8) 0.034(2) Uani 1 1 d . . .
H7A H 0.7156 0.2554 0.8150 0.051 Uiso 1 1 calc R . .
H7B H 0.8450 0.2786 0.8362 0.051 Uiso 1 1 calc R . .
H7C H 0.7907 0.3295 0.7443 0.051 Uiso 1 1 calc R . .
C8 C 0.5970(7) 0.2879(7) 1.0303(7) 0.0239(18) Uani 1 1 d . . .
H8 H 0.6531 0.3138 1.0846 0.029 Uiso 1 1 calc R . .
C9 C 0.5100(7) 0.1963(7) 1.0505(6) 0.0247(18) Uani 1 1 d . . .
C10 C 0.5185(8) 0.1581(7) 1.1505(7) 0.031(2) Uani 1 1 d . . .
H10 H 0.5746 0.1952 1.2014 0.037 Uiso 1 1 calc R . .
C11 C 0.4471(7) 0.0680(7) 1.1757(7) 0.031(2) Uani 1 1 d . . .
H11 H 0.4532 0.0458 1.2434 0.037 Uiso 1 1 calc R . .
C12 C 0.3655(9) 0.0106(7) 1.0981(7) 0.041(3) Uani 1 1 d . . .
H12 H 0.3185 -0.0524 1.1132 0.049 Uiso 1 1 calc R . .
C13 C 0.3535(7) 0.0456(6) 0.9998(7) 0.029(2) Uani 1 1 d . . .
C14 C 0.4279(6) 0.1392(6) 0.9744(6) 0.0231(18) Uani 1 1 d . . .
C15 C 0.2074(9) -0.1042(7) 0.9363(9) 0.046(3) Uani 1 1 d . . .
H15A H 0.2337 -0.1259 1.0019 0.069 Uiso 1 1 calc R . .
H15B H 0.2073 -0.1628 0.8771 0.069 Uiso 1 1 calc R . .
H15C H 0.1334 -0.0899 0.9438 0.069 Uiso 1 1 calc R . .
C16 C 0.0247(8) 0.1248(8) 0.5931(9) 0.052(3) Uani 1 1 d . . .
H16A H -0.0351 0.1548 0.6262 0.078 Uiso 1 1 calc R . .
H16B H 0.0147 0.0467 0.5970 0.078 Uiso 1 1 calc R . .
H16C H 0.0254 0.1359 0.5186 0.078 Uiso 1 1 calc R . .
C17 C 0.1533(7) 0.2940(7) 0.6517(7) 0.028(2) Uani 1 1 d . . .
C18 C 0.0858(7) 0.3557(7) 0.6094(8) 0.034(2) Uani 1 1 d . . .
H18 H 0.0156 0.3223 0.5789 0.040 Uiso 1 1 calc R . .
C19 C 0.1226(7) 0.4693(8) 0.6122(8) 0.034(2) Uani 1 1 d . . .
H19 H 0.0767 0.5123 0.5842 0.041 Uiso 1 1 calc R . .
C20 C 0.2281(8) 0.5182(8) 0.6569(7) 0.034(2) Uani 1 1 d . . .
H20 H 0.2530 0.5938 0.6574 0.041 Uiso 1 1 calc R . .
C21 C 0.2959(6) 0.4562(7) 0.7002(6) 0.0246(18) Uani 1 1 d . . .
C22 C 0.2596(6) 0.3417(6) 0.7017(6) 0.0192(17) Uani 1 1 d . . .
C23 C 0.4094(7) 0.5124(7) 0.7354(7) 0.0245(19) Uani 1 1 d . . .
H23 H 0.4285 0.5856 0.7232 0.029 Uiso 1 1 calc R . .
C24 C 0.6521(7) 0.5547(7) 0.7254(7) 0.028(2) Uani 1 1 d . . .
C25 C 0.6310(8) 0.4789(7) 0.6185(7) 0.034(2) Uani 1 1 d . . .
H25A H 0.5700 0.4197 0.6230 0.051 Uiso 1 1 calc R . .
H25B H 0.6962 0.4484 0.6015 0.051 Uiso 1 1 calc R . .
H25C H 0.6135 0.5204 0.5628 0.051 Uiso 1 1 calc R . .
C26 C 0.7513(7) 0.6420(7) 0.7420(7) 0.0262(19) Uani 1 1 d . . .
C27 C 0.7730(7) 0.7357(6) 0.8268(8) 0.0267(19) Uani 1 1 d . . .
H27 H 0.7236 0.7524 0.8843 0.032 Uiso 1 1 calc R . .
C28 C 0.8761(7) 0.7998(7) 0.8128(7) 0.033(2) Uani 1 1 d . . .
H28 H 0.9116 0.8680 0.8599 0.040 Uiso 1 1 calc R . .
C29 C 0.9220(8) 0.7481(7) 0.7207(7) 0.034(2) Uani 1 1 d . . .
H29 H 0.9944 0.7742 0.6934 0.041 Uiso 1 1 calc R . .
C30 C 0.8444(7) 0.6500(7) 0.6755(7) 0.034(2) Uani 1 1 d . . .
H30 H 0.8539 0.5973 0.6117 0.041 Uiso 1 1 calc R . .
C31 C 0.5137(8) 0.1582(7) 0.6532(7) 0.030(2) Uani 1 1 d . . .
C32 C 0.5992(8) 0.1185(9) 0.5835(9) 0.046(3) Uani 1 1 d . . .
H32A H 0.5661 0.0516 0.5365 0.068 Uiso 1 1 calc R . .
H32B H 0.6585 0.1037 0.6283 0.068 Uiso 1 1 calc R . .
H32C H 0.6281 0.1745 0.5407 0.068 Uiso 1 1 calc R . .
C33 C 0.3027(11) 0.1646(11) 0.4258(10) 0.065(4) Uani 1 1 d . . .
H33A H 0.2769 0.1272 0.3545 0.097 Uiso 1 1 calc R . .
H33B H 0.2508 0.2099 0.4531 0.097 Uiso 1 1 calc R . .
H33C H 0.3090 0.1106 0.4728 0.097 Uiso 1 1 calc R . .
C34 C 0.4070(9) 0.2319(9) 0.4214(7) 0.063(4) Uani 1 1 d . . .
H13A H 0.3154 0.4079 0.9880 0.12(6) Uiso 1 1 d RD . .
H13B H 0.3961 0.3751 1.0387 0.000(16) Uiso 1 1 d RD . .


_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
Er1 O6 2.270(5) . ?
Er1 O1 2.278(6) . ?
Er1 O3 2.299(5) . ?
Er1 O8 2.385(6) . ?
Er1 O7 2.401(7) . ?
Er1 O11 2.425(6) . ?
Er1 O10 2.465(6) . ?
Er1 O2 2.520(6) . ?
Er1 O4 2.599(6) . ?
Er1 N6 2.836(7) . ?
Er1 N5 2.846(9) . ?
Er1 Ni1 3.3957(14) . ?
Ni1 O5 2.004(5) . ?
Ni1 O1 2.033(6) . ?
Ni1 O3 2.051(6) . ?
Ni1 O13 2.074(5) . ?
Ni1 N4 2.079(7) . ?
Ni1 N2 2.137(7) . ?
Fe1 C3 2.009(10) . ?
Fe1 C27 2.022(8) . ?
Fe1 C26 2.033(9) . ?
Fe1 C1 2.035(9) . ?
Fe1 C2 2.041(10) . ?
Fe1 C28 2.048(9) . ?
Fe1 C5 2.056(9) . ?
Fe1 C29 2.060(9) . ?
Fe1 C30 2.060(9) . ?
Fe1 C4 2.064(9) . ?
O1 C14 1.340(10) . ?
O2 C13 1.373(10) . ?
O2 C15 1.433(9) . ?
O7 N5 1.349(11) . ?
O8 N5 1.294(10) . ?
O9 N5 1.176(11) . ?
O11 N6 1.288(10) . ?
O12 N6 1.299(10) . ?
O10 N6 1.270(10) . ?
O4 C17 1.381(11) . ?
O4 C16 1.443(9) . ?
O3 C22 1.303(10) . ?
O6 C31 1.272(10) . ?
O5 C31 1.263(10) . ?
N1 C6 1.287(10) . ?
N1 N2 1.422(8) . ?
N2 C8 1.257(11) . ?
N4 C23 1.259(11) . ?
N4 N3 1.430(8) . ?
N3 C24 1.287(10) . ?
N7 C34 1.154(14) . ?
C1 C2 1.429(12) . ?
C1 C5 1.437(11) . ?
C2 C3 1.375(13) . ?
C3 C4 1.406(12) . ?
C4 C5 1.439(12) . ?
C5 C6 1.478(11) . ?
C6 C7 1.499(11) . ?
C8 C9 1.470(11) . ?
C9 C14 1.382(11) . ?
C9 C10 1.404(12) . ?
C10 C11 1.372(12) . ?
C11 C12 1.391(13) . ?
C12 C13 1.371(13) . ?
C13 C14 1.424(11) . ?
C17 C18 1.361(13) . ?
C17 C22 1.416(11) . ?
C18 C19 1.394(13) . ?
C19 C20 1.389(12) . ?
C20 C21 1.371(13) . ?
C21 C22 1.411(11) . ?
C21 C23 1.464(11) . ?
C24 C26 1.465(11) . ?
C24 C25 1.507(11) . ?
C26 C30 1.434(12) . ?
C26 C27 1.436(11) . ?
C27 C28 1.399(11) . ?
C28 C29 1.421(13) . ?
C29 C30 1.436(11) . ?
C31 C32 1.492(13) . ?
C33 C34 1.406(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
O6 Er1 O1 77.9(2) . . ?
O6 Er1 O3 78.4(2) . . ?
O1 Er1 O3 70.6(2) . . ?
O6 Er1 O8 148.67(19) . . ?
O1 Er1 O8 129.3(2) . . ?
O3 Er1 O8 121.9(2) . . ?
O6 Er1 O7 155.3(2) . . ?
O1 Er1 O7 85.6(2) . . ?
O3 Er1 O7 79.0(2) . . ?
O8 Er1 O7 54.9(2) . . ?
O6 Er1 O11 80.10(19) . . ?
O1 Er1 O11 110.2(2) . . ?
O3 Er1 O11 157.8(2) . . ?
O8 Er1 O11 75.8(2) . . ?
O7 Er1 O11 123.2(2) . . ?
O6 Er1 O10 77.07(19) . . ?
O1 Er1 O10 152.2(2) . . ?
O3 Er1 O10 115.4(2) . . ?
O8 Er1 O10 72.6(2) . . ?
O7 Er1 O10 122.0(2) . . ?
O11 Er1 O10 53.5(2) . . ?
O6 Er1 O2 115.2(2) . . ?
O1 Er1 O2 64.27(19) . . ?
O3 Er1 O2 127.37(18) . . ?
O8 Er1 O2 73.4(2) . . ?
O7 Er1 O2 72.2(2) . . ?
O11 Er1 O2 67.82(19) . . ?
O10 Er1 O2 117.14(19) . . ?
O6 Er1 O4 105.9(2) . . ?
O1 Er1 O4 130.88(19) . . ?
O3 Er1 O4 62.80(19) . . ?
O8 Er1 O4 69.9(2) . . ?
O7 Er1 O4 71.7(2) . . ?
O11 Er1 O4 118.79(19) . . ?
O10 Er1 O4 68.41(19) . . ?
O2 Er1 O4 138.79(19) . . ?
O6 Er1 N6 78.01(19) . . ?
O1 Er1 N6 134.1(2) . . ?
O3 Er1 N6 139.6(2) . . ?
O8 Er1 N6 71.4(2) . . ?
O7 Er1 N6 126.3(2) . . ?
O11 Er1 N6 26.9(2) . . ?
O10 Er1 N6 26.6(2) . . ?
O2 Er1 N6 92.4(2) . . ?
O4 Er1 N6 93.2(2) . . ?
O6 Er1 N5 171.2(3) . . ?
O1 Er1 N5 110.0(3) . . ?
O3 Er1 N5 100.2(2) . . ?
O8 Er1 N5 26.8(2) . . ?
O7 Er1 N5 28.2(2) . . ?
O11 Er1 N5 100.2(2) . . ?
O10 Er1 N5 96.0(3) . . ?
O2 Er1 N5 72.7(3) . . ?
O4 Er1 N5 66.1(3) . . ?
N6 Er1 N5 98.2(2) . . ?
O6 Er1 Ni1 68.59(13) . . ?
O1 Er1 Ni1 35.54(15) . . ?
O3 Er1 Ni1 36.14(15) . . ?
O8 Er1 Ni1 142.15(14) . . ?
O7 Er1 Ni1 87.31(16) . . ?
O11 Er1 Ni1 136.49(14) . . ?
O10 Er1 Ni1 138.48(14) . . ?
O2 Er1 Ni1 98.63(12) . . ?
O4 Er1 Ni1 98.86(12) . . ?
N6 Er1 Ni1 146.43(15) . . ?
N5 Er1 Ni1 115.32(18) . . ?
O5 Ni1 O1 89.0(2) . . ?
O5 Ni1 O3 89.2(2) . . ?
O1 Ni1 O3 80.7(2) . . ?
O5 Ni1 O13 176.8(2) . . ?
O1 Ni1 O13 87.9(2) . . ?
O3 Ni1 O13 90.7(2) . . ?
O5 Ni1 N4 93.3(2) . . ?
O1 Ni1 N4 168.1(3) . . ?
O3 Ni1 N4 87.7(2) . . ?
O13 Ni1 N4 89.9(2) . . ?
O5 Ni1 N2 92.3(2) . . ?
O1 Ni1 N2 87.2(2) . . ?
O3 Ni1 N2 167.8(2) . . ?
O13 Ni1 N2 87.1(2) . . ?
N4 Ni1 N2 104.4(3) . . ?
O5 Ni1 Er1 80.66(15) . . ?
O1 Ni1 Er1 40.66(17) . . ?
O3 Ni1 Er1 41.37(16) . . ?
O13 Ni1 Er1 97.22(14) . . ?
N4 Ni1 Er1 128.29(19) . . ?
N2 Ni1 Er1 127.04(18) . . ?
C3 Fe1 C27 156.1(4) . . ?
C3 Fe1 C26 160.6(4) . . ?
C27 Fe1 C26 41.5(3) . . ?
C3 Fe1 C1 68.2(4) . . ?
C27 Fe1 C1 105.9(4) . . ?
C26 Fe1 C1 124.2(3) . . ?
C3 Fe1 C2 39.7(4) . . ?
C27 Fe1 C2 120.8(4) . . ?
C26 Fe1 C2 159.3(4) . . ?
C1 Fe1 C2 41.1(3) . . ?
C3 Fe1 C28 120.8(4) . . ?
C27 Fe1 C28 40.2(3) . . ?
C26 Fe1 C28 68.7(4) . . ?
C1 Fe1 C28 119.3(4) . . ?
C2 Fe1 C28 104.2(4) . . ?
C3 Fe1 C5 68.5(4) . . ?
C27 Fe1 C5 123.3(3) . . ?
C26 Fe1 C5 109.8(3) . . ?
C1 Fe1 C5 41.1(3) . . ?
C2 Fe1 C5 68.7(3) . . ?
C28 Fe1 C5 157.0(4) . . ?
C3 Fe1 C29 106.6(4) . . ?
C27 Fe1 C29 68.3(4) . . ?
C26 Fe1 C29 68.8(3) . . ?
C1 Fe1 C29 154.7(3) . . ?
C2 Fe1 C29 119.1(4) . . ?
C28 Fe1 C29 40.5(4) . . ?
C5 Fe1 C29 162.2(4) . . ?
C3 Fe1 C30 123.3(4) . . ?
C27 Fe1 C30 69.0(4) . . ?
C26 Fe1 C30 41.0(3) . . ?
C1 Fe1 C30 162.3(3) . . ?
C2 Fe1 C30 156.2(4) . . ?
C28 Fe1 C30 68.5(4) . . ?
C5 Fe1 C30 126.5(3) . . ?
C29 Fe1 C30 40.8(3) . . ?
C3 Fe1 C4 40.4(3) . . ?
C27 Fe1 C4 161.2(3) . . ?
C26 Fe1 C4 125.7(3) . . ?
C1 Fe1 C4 68.6(4) . . ?
C2 Fe1 C4 67.7(4) . . ?
C28 Fe1 C4 158.4(3) . . ?
C5 Fe1 C4 40.9(3) . . ?
C29 Fe1 C4 124.4(4) . . ?
C30 Fe1 C4 110.5(4) . . ?
C14 O1 Ni1 124.5(5) . . ?
C14 O1 Er1 127.2(5) . . ?
Ni1 O1 Er1 103.8(3) . . ?
C13 O2 C15 114.8(7) . . ?
C13 O2 Er1 118.1(5) . . ?
C15 O2 Er1 126.9(6) . . ?
N5 O7 Er1 94.6(5) . . ?
N5 O8 Er1 96.9(5) . . ?
N6 O11 Er1 94.6(5) . . ?
N6 O10 Er1 93.2(5) . . ?
C17 O4 C16 115.9(7) . . ?
C17 O4 Er1 117.2(5) . . ?
C16 O4 Er1 126.9(6) . . ?
C22 O3 Ni1 128.0(5) . . ?
C22 O3 Er1 129.0(5) . . ?
Ni1 O3 Er1 102.5(3) . . ?
C31 O6 Er1 135.1(5) . . ?
C31 O5 Ni1 130.2(5) . . ?
C6 N1 N2 116.9(6) . . ?
C8 N2 N1 111.6(7) . . ?
C8 N2 Ni1 121.7(5) . . ?
N1 N2 Ni1 123.3(5) . . ?
O10 N6 O11 118.6(7) . . ?
O10 N6 O12 121.8(8) . . ?
O11 N6 O12 119.4(9) . . ?
O10 N6 Er1 60.2(4) . . ?
O11 N6 Er1 58.5(4) . . ?
O12 N6 Er1 171.8(6) . . ?
O9 N5 O8 123.3(9) . . ?
O9 N5 O7 123.5(9) . . ?
O8 N5 O7 113.1(7) . . ?
O9 N5 Er1 171.6(10) . . ?
O8 N5 Er1 56.3(4) . . ?
O7 N5 Er1 57.2(4) . . ?
C23 N4 N3 111.8(7) . . ?
C23 N4 Ni1 125.9(6) . . ?
N3 N4 Ni1 121.9(5) . . ?
C24 N3 N4 115.7(6) . . ?
C2 C1 C5 107.6(8) . . ?
C2 C1 Fe1 69.7(5) . . ?
C5 C1 Fe1 70.2(5) . . ?
C3 C2 C1 107.9(8) . . ?
C3 C2 Fe1 68.9(6) . . ?
C1 C2 Fe1 69.3(5) . . ?
C2 C3 C4 110.5(8) . . ?
C2 C3 Fe1 71.4(6) . . ?
C4 C3 Fe1 71.9(5) . . ?
C3 C4 C5 107.1(8) . . ?
C3 C4 Fe1 67.7(6) . . ?
C5 C4 Fe1 69.3(5) . . ?
C1 C5 C4 106.8(7) . . ?
C1 C5 C6 127.4(7) . . ?
C4 C5 C6 125.8(7) . . ?
C1 C5 Fe1 68.7(5) . . ?
C4 C5 Fe1 69.9(5) . . ?
C6 C5 Fe1 126.6(6) . . ?
N1 C6 C5 117.0(7) . . ?
N1 C6 C7 126.5(7) . . ?
C5 C6 C7 116.4(7) . . ?
N2 C8 C9 126.7(8) . . ?
C14 C9 C10 118.4(8) . . ?
C14 C9 C8 124.4(8) . . ?
C10 C9 C8 116.9(8) . . ?
C11 C10 C9 122.3(9) . . ?
C10 C11 C12 118.7(9) . . ?
C13 C12 C11 120.9(8) . . ?
C12 C13 O2 126.5(7) . . ?
C12 C13 C14 120.0(8) . . ?
O2 C13 C14 113.4(7) . . ?
O1 C14 C9 124.2(7) . . ?
O1 C14 C13 116.1(7) . . ?
C9 C14 C13 119.6(8) . . ?
C18 C17 O4 125.0(8) . . ?
C18 C17 C22 122.3(8) . . ?
O4 C17 C22 112.7(8) . . ?
C17 C18 C19 119.5(8) . . ?
C20 C19 C18 119.8(9) . . ?
C21 C20 C19 120.8(9) . . ?
C20 C21 C22 120.7(8) . . ?
C20 C21 C23 116.8(8) . . ?
C22 C21 C23 122.3(8) . . ?
O3 C22 C21 125.1(7) . . ?
O3 C22 C17 118.0(7) . . ?
C21 C22 C17 116.8(8) . . ?
N4 C23 C21 127.7(8) . . ?
N3 C24 C26 116.7(7) . . ?
N3 C24 C25 124.3(8) . . ?
C26 C24 C25 118.8(8) . . ?
C30 C26 C27 107.4(7) . . ?
C30 C26 C24 126.0(7) . . ?
C27 C26 C24 126.6(7) . . ?
C30 C26 Fe1 70.5(5) . . ?
C27 C26 Fe1 68.9(5) . . ?
C24 C26 Fe1 126.4(7) . . ?
C28 C27 C26 108.6(8) . . ?
C28 C27 Fe1 70.9(5) . . ?
C26 C27 Fe1 69.7(5) . . ?
C27 C28 C29 108.7(8) . . ?
C27 C28 Fe1 68.9(5) . . ?
C29 C28 Fe1 70.2(5) . . ?
C28 C29 C30 108.0(8) . . ?
C28 C29 Fe1 69.3(5) . . ?
C30 C29 Fe1 69.6(5) . . ?
C26 C30 C29 107.4(8) . . ?
C26 C30 Fe1 68.5(5) . . ?
C29 C30 Fe1 69.6(5) . . ?
O5 C31 O6 124.7(8) . . ?
O5 C31 C32 117.7(8) . . ?
O6 C31 C32 117.6(8) . . ?
N7 C34 C33 177.6(11) . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         2.346
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.228
_database_code_depnum_ccdc_archive 'CCDC 993948'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_NiY

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H33 Fe N6 Ni O13 Y, C2 H3 N'
_chemical_formula_sum            'C34 H36 Fe N7 Ni O13 Y'
_chemical_formula_weight         955.16

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'
Fe Fe 0.3463 0.8444 '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'
Y Y -2.7962 3.5667 '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                   12.238(5)
_cell_length_b                   12.345(5)
_cell_length_c                   12.486(5)
_cell_angle_alpha                98.068(5)
_cell_angle_beta                 92.083(5)
_cell_angle_gamma                99.950(5)
_cell_volume                     1836.0(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6632
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      28.36

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             974.0
_exptl_absorpt_coefficient_mu    2.542
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.6408
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12772
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         25.50
_reflns_number_total             6789
_reflns_number_gt                5770
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0342P)²+2.7821P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6789
_refine_ls_number_parameters     523
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_ref         0.0867
_refine_ls_wR_factor_gt          0.0822
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C2 C 1.4666(3) 0.5069(3) 0.3402(3) 0.0228(7) Uani 1 1 d . . .
H2 H 1.4760 0.4514 0.2786 0.027 Uiso 1 1 calc R . .
Y1 Y 0.76865(3) 0.09105(3) 0.25035(3) 0.01989(9) Uani 1 1 d . . .
Ni1 Ni 0.96317(3) 0.32130(3) 0.33591(3) 0.01342(10) Uani 1 1 d . . .
Fe1 Fe 1.39209(4) 0.64160(4) 0.33310(4) 0.01773(12) Uani 1 1 d . . .
O11 O 0.69491(19) -0.02887(19) 0.07854(19) 0.0248(5) Uani 1 1 d . . .
O6 O 0.91998(19) 0.09641(18) 0.14906(18) 0.0210(5) Uani 1 1 d . . .
O4 O 0.62861(19) 0.1815(2) 0.1475(2) 0.0274(6) Uani 1 1 d . . .
O2 O 0.7787(2) -0.00509(19) 0.41550(19) 0.0248(5) Uani 1 1 d . . .
O10 O 0.7655(2) -0.10797(19) 0.20252(19) 0.0261(6) Uani 1 1 d . . .
O8 O 0.5816(2) 0.0059(2) 0.2760(2) 0.0351(7) Uani 1 1 d . . .
O13 O 0.87898(19) 0.38422(19) 0.46613(17) 0.0193(5) Uani 1 1 d . . .
H13A H 0.9085 0.3741 0.5230 0.029 Uiso 1 1 calc R . .
O3 O 0.81703(18) 0.27814(18) 0.24300(17) 0.0180(5) Uani 1 1 d . . .
N1 N 1.1974(2) 0.4235(2) 0.4566(2) 0.0171(6) Uani 1 1 d . . .
O1 O 0.91065(18) 0.16738(17) 0.37608(16) 0.0167(5) Uani 1 1 d . . .
O5 O 1.04237(18) 0.25149(17) 0.21254(16) 0.0165(5) Uani 1 1 d . . .
O7 O 0.6462(3) 0.1651(2) 0.3796(2) 0.0425(7) Uani 1 1 d . . .
N4 N 0.9840(2) 0.4738(2) 0.2814(2) 0.0145(5) Uani 1 1 d . . .
N3 N 1.0850(2) 0.5524(2) 0.3031(2) 0.0143(5) Uani 1 1 d . . .
C23 C 1.1512(3) 0.5555(3) 0.2250(2) 0.0166(7) Uani 1 1 d . . .
C8 C 1.0105(3) 0.1959(3) 0.5505(2) 0.0179(7) Uani 1 1 d . . .
C20 C 0.7955(3) 0.4579(3) 0.2002(2) 0.0189(7) Uani 1 1 d . . .
N2 N 1.1030(2) 0.3358(2) 0.4462(2) 0.0153(6) Uani 1 1 d . . .
C16 C 0.6527(3) 0.2960(3) 0.1498(3) 0.0230(8) Uani 1 1 d . . .
O12 O 0.6775(2) -0.2119(2) 0.0558(2) 0.0406(7) Uani 1 1 d . . .
C12 C 0.8553(3) 0.0459(3) 0.4998(3) 0.0214(7) Uani 1 1 d . . .
C27 C 1.0136(3) 0.1594(3) 0.1526(2) 0.0196(7) Uani 1 1 d . . .
C21 C 0.7581(3) 0.3435(3) 0.2009(2) 0.0184(7) Uani 1 1 d . . .
C1 C 1.3737(3) 0.5017(3) 0.4064(3) 0.0195(7) Uani 1 1 d . . .
C19 C 0.7254(3) 0.5208(3) 0.1549(3) 0.0233(8) Uani 1 1 d . . .
H19 H 0.7499 0.5965 0.1554 0.028 Uiso 1 1 calc R . .
C5 C 1.2773(3) 0.4107(3) 0.3943(3) 0.0175(7) Uani 1 1 d . . .
C9 C 1.0196(3) 0.1583(3) 0.6518(3) 0.0230(8) Uani 1 1 d . . .
H9 H 1.0750 0.1956 0.7035 0.028 Uiso 1 1 calc R . .
C25 C 1.2510(3) 0.6429(3) 0.2421(2) 0.0165(7) Uani 1 1 d . . .
C24 C 1.1326(3) 0.4805(3) 0.1188(3) 0.0219(7) Uani 1 1 d . . .
H24A H 1.0837 0.4128 0.1267 0.033 Uiso 1 1 calc R . .
H24B H 1.2024 0.4638 0.0952 0.033 Uiso 1 1 calc R . .
H24C H 1.0998 0.5168 0.0660 0.033 Uiso 1 1 calc R . .
C3 C 1.5424(3) 0.6061(3) 0.3780(3) 0.0273(8) Uani 1 1 d . . .
H3 H 1.6134 0.6312 0.3474 0.033 Uiso 1 1 calc R . .
C10 C 0.9474(3) 0.0672(3) 0.6748(3) 0.0281(8) Uani 1 1 d . . .
H10 H 0.9542 0.0438 0.7420 0.034 Uiso 1 1 calc R . .
N6 N 0.7129(2) -0.1176(2) 0.1110(2) 0.0272(7) Uani 1 1 d . . .
C14 C 0.7030(3) -0.1021(3) 0.4356(3) 0.0318(9) Uani 1 1 d . . .
H14A H 0.7444 -0.1554 0.4576 0.048 Uiso 1 1 calc R . .
H14B H 0.6579 -0.1343 0.3707 0.048 Uiso 1 1 calc R . .
H14C H 0.6561 -0.0812 0.4921 0.048 Uiso 1 1 calc R . .
C13 C 0.9264(3) 0.1396(3) 0.4734(2) 0.0171(7) Uani 1 1 d . . .
C18 C 0.6218(3) 0.4723(3) 0.1101(3) 0.0277(8) Uani 1 1 d . . .
H18 H 0.5757 0.5155 0.0821 0.033 Uiso 1 1 calc R . .
O9 O 0.4687(3) 0.0901(3) 0.3739(3) 0.0696(12) Uani 1 1 d . . .
C7 C 1.0949(3) 0.2876(3) 0.5310(2) 0.0176(7) Uani 1 1 d . . .
H7 H 1.1497 0.3147 0.5864 0.021 Uiso 1 1 calc R . .
C15 C 0.5235(3) 0.1270(3) 0.0929(4) 0.0445(12) Uani 1 1 d . . .
H15A H 0.4642 0.1560 0.1287 0.067 Uiso 1 1 calc R . .
H15B H 0.5143 0.0484 0.0947 0.067 Uiso 1 1 calc R . .
H15C H 0.5220 0.1402 0.0190 0.067 Uiso 1 1 calc R . .
C11 C 0.8643(3) 0.0100(3) 0.5988(3) 0.0279(8) Uani 1 1 d . . .
H11 H 0.8156 -0.0516 0.6144 0.033 Uiso 1 1 calc R . .
C4 C 1.4972(3) 0.6638(3) 0.4674(3) 0.0255(8) Uani 1 1 d . . .
H4 H 1.5317 0.7355 0.5094 0.031 Uiso 1 1 calc R . .
N7 N 0.9932(4) 0.2844(3) 0.9179(3) 0.0585(12) Uani 1 1 d . . .
C6 C 1.2823(3) 0.3090(3) 0.3146(3) 0.0218(7) Uani 1 1 d . . .
H6A H 1.2146 0.2562 0.3140 0.033 Uiso 1 1 calc R . .
H6B H 1.3441 0.2763 0.3353 0.033 Uiso 1 1 calc R . .
H6C H 1.2913 0.3293 0.2436 0.033 Uiso 1 1 calc R . .
C26 C 1.3766(3) 0.8000(3) 0.3122(3) 0.0259(8) Uani 1 1 d . . .
H26 H 1.4127 0.8684 0.3588 0.031 Uiso 1 1 calc R . .
C28 C 1.1009(3) 0.1222(3) 0.0816(3) 0.0342(9) Uani 1 1 d . . .
H28A H 1.1557 0.0980 0.1250 0.051 Uiso 1 1 calc R . .
H28B H 1.1358 0.1830 0.0473 0.051 Uiso 1 1 calc R . .
H28C H 1.0669 0.0618 0.0271 0.051 Uiso 1 1 calc R . .
C22 C 0.9074(3) 0.5142(3) 0.2358(2) 0.0170(7) Uani 1 1 d . . .
H22 H 0.9260 0.5878 0.2244 0.020 Uiso 1 1 calc R . .
C17 C 0.5852(3) 0.3581(3) 0.1062(3) 0.0266(8) Uani 1 1 d . . .
H17 H 0.5155 0.3246 0.0743 0.032 Uiso 1 1 calc R . .
N5 N 0.5616(3) 0.0850(3) 0.3457(3) 0.0511(11) Uani 1 1 d . . .
C29 C 0.9082(5) 0.2307(4) 0.9211(3) 0.0449(12) Uani 1 1 d . . .
C30 C 0.7995(4) 0.1609(4) 0.9235(4) 0.0530(13) Uani 1 1 d . . .
H30A H 0.7713 0.1305 0.8508 0.080 Uiso 1 1 calc R . .
H30B H 0.7493 0.2048 0.9575 0.080 Uiso 1 1 calc R . .
H30C H 0.8065 0.1014 0.9638 0.080 Uiso 1 1 calc R . .
C34 C 1.3930(3) 0.5998(3) 0.4852(3) 0.0209(7) Uani 1 1 d . . .
H34 H 1.3431 0.6196 0.5415 0.025 Uiso 1 1 calc R . .
C31 C 1.2716(3) 0.7359(3) 0.3270(3) 0.0205(7) Uani 1 1 d . . .
H31 H 1.2220 0.7527 0.3845 0.025 Uiso 1 1 calc R . .
C33 C 1.3445(3) 0.6501(3) 0.1764(3) 0.0228(7) Uani 1 1 d . . .
H33 H 1.3539 0.5973 0.1126 0.027 Uiso 1 1 calc R . .
C32 C 1.4216(3) 0.7468(3) 0.2207(3) 0.0275(8) Uani 1 1 d . . .
H32 H 1.4940 0.7723 0.1929 0.033 Uiso 1 1 calc R . .
H13B H 0.8529 0.4346 0.4647 0.024(11) 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
C2 C3 1.413(5) . ?
C2 C1 1.428(5) . ?
C2 Fe1 2.041(3) . ?
Y1 O6 2.277(2) . ?
Y1 O1 2.279(2) . ?
Y1 O3 2.299(2) . ?
Y1 O8 2.401(3) . ?
Y1 O7 2.434(3) . ?
Y1 O10 2.439(3) . ?
Y1 O11 2.473(2) . ?
Y1 O2 2.529(3) . ?
Y1 O4 2.596(3) . ?
Y1 N5 2.832(4) . ?
Y1 N6 2.859(3) . ?
Y1 Ni1 3.3930(11) . ?
Ni1 O5 2.020(2) . ?
Ni1 O1 2.036(2) . ?
Ni1 O3 2.043(2) . ?
Ni1 N4 2.069(3) . ?
Ni1 O13 2.086(2) . ?
Ni1 N2 2.123(3) . ?
Fe1 C4 2.034(3) . ?
Fe1 C25 2.036(3) . ?
Fe1 C31 2.036(3) . ?
Fe1 C34 2.037(3) . ?
Fe1 C3 2.040(4) . ?
Fe1 C33 2.043(3) . ?
Fe1 C32 2.043(4) . ?
Fe1 C26 2.049(4) . ?
Fe1 C1 2.049(3) . ?
O11 N6 1.271(4) . ?
O6 C27 1.264(4) . ?
O4 C16 1.389(4) . ?
O4 C15 1.443(4) . ?
O2 C12 1.386(4) . ?
O2 C14 1.440(4) . ?
O10 N6 1.271(4) . ?
O8 N5 1.277(4) . ?
O3 C21 1.319(4) . ?
N1 C5 1.289(4) . ?
N1 N2 1.429(4) . ?
O1 C13 1.324(4) . ?
O5 C27 1.257(4) . ?
O7 N5 1.314(4) . ?
N4 C22 1.286(4) . ?
N4 N3 1.424(3) . ?
N3 C23 1.291(4) . ?
C23 C25 1.471(4) . ?
C23 C24 1.493(4) . ?
C8 C13 1.401(5) . ?
C8 C9 1.414(5) . ?
C8 C7 1.448(4) . ?
C20 C19 1.405(5) . ?
C20 C21 1.409(5) . ?
C20 C22 1.448(4) . ?
N2 C7 1.285(4) . ?
C16 C17 1.367(5) . ?
C16 C21 1.410(5) . ?
O12 N6 1.264(4) . ?
C12 C11 1.377(5) . ?
C12 C13 1.409(5) . ?
C27 C28 1.504(5) . ?
C1 C34 1.428(5) . ?
C1 C5 1.469(4) . ?
C19 C18 1.368(5) . ?
C5 C6 1.500(4) . ?
C9 C10 1.376(5) . ?
C25 C33 1.430(5) . ?
C25 C31 1.430(5) . ?
C3 C4 1.420(5) . ?
C10 C11 1.388(5) . ?
C18 C17 1.398(5) . ?
O9 N5 1.212(5) . ?
C4 C34 1.422(5) . ?
N7 C29 1.138(6) . ?
C26 C32 1.415(5) . ?
C26 C31 1.421(5) . ?
C29 C30 1.459(7) . ?
C33 C32 1.418(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 C2 C1 108.4(3) . . ?
C3 C2 Fe1 69.7(2) . . ?
C1 C2 Fe1 69.86(19) . . ?
O6 Y1 O1 77.75(8) . . ?
O6 Y1 O3 78.27(8) . . ?
O1 Y1 O3 70.52(8) . . ?
O6 Y1 O8 148.64(8) . . ?
O1 Y1 O8 129.46(9) . . ?
O3 Y1 O8 121.99(8) . . ?
O6 Y1 O7 155.98(9) . . ?
O1 Y1 O7 86.59(9) . . ?
O3 Y1 O7 79.39(9) . . ?
O8 Y1 O7 54.12(9) . . ?
O6 Y1 O10 80.51(8) . . ?
O1 Y1 O10 110.16(8) . . ?
O3 Y1 O10 158.08(8) . . ?
O8 Y1 O10 75.42(8) . . ?
O7 Y1 O10 122.40(9) . . ?
O6 Y1 O11 76.78(8) . . ?
O1 Y1 O11 151.31(8) . . ?
O3 Y1 O11 116.38(8) . . ?
O8 Y1 O11 72.68(8) . . ?
O7 Y1 O11 121.66(9) . . ?
O10 Y1 O11 52.47(8) . . ?
O6 Y1 O2 115.11(8) . . ?
O1 Y1 O2 64.07(8) . . ?
O3 Y1 O2 127.18(7) . . ?
O8 Y1 O2 73.66(9) . . ?
O7 Y1 O2 72.58(9) . . ?
O10 Y1 O2 67.69(8) . . ?
O11 Y1 O2 116.43(8) . . ?
O6 Y1 O4 105.67(9) . . ?
O1 Y1 O4 131.18(8) . . ?
O3 Y1 O4 63.04(7) . . ?
O8 Y1 O4 69.91(9) . . ?
O7 Y1 O4 71.36(9) . . ?
O10 Y1 O4 118.49(8) . . ?
O11 Y1 O4 69.22(8) . . ?
O2 Y1 O4 139.10(8) . . ?
O6 Y1 N5 171.08(11) . . ?
O1 Y1 N5 110.31(10) . . ?
O3 Y1 N5 100.48(9) . . ?
O8 Y1 N5 26.64(9) . . ?
O7 Y1 N5 27.59(10) . . ?
O10 Y1 N5 99.63(9) . . ?
O11 Y1 N5 96.15(10) . . ?
O2 Y1 N5 72.78(11) . . ?
O4 Y1 N5 66.32(11) . . ?
O6 Y1 N6 78.99(8) . . ?
O1 Y1 N6 133.84(8) . . ?
O3 Y1 N6 140.77(8) . . ?
O8 Y1 N6 70.50(8) . . ?
O7 Y1 N6 124.58(9) . . ?
O10 Y1 N6 26.25(8) . . ?
O11 Y1 N6 26.31(8) . . ?
O2 Y1 N6 91.47(9) . . ?
O4 Y1 N6 93.38(9) . . ?
N5 Y1 N6 97.14(9) . . ?
O6 Y1 Ni1 68.42(6) . . ?
O1 Y1 Ni1 35.68(5) . . ?
O3 Y1 Ni1 35.99(5) . . ?
O8 Y1 Ni1 142.32(6) . . ?
O7 Y1 Ni1 88.23(7) . . ?
O10 Y1 Ni1 136.72(6) . . ?
O11 Y1 Ni1 138.65(6) . . ?
O2 Y1 Ni1 98.57(6) . . ?
O4 Y1 Ni1 98.96(6) . . ?
N5 Y1 Ni1 115.68(8) . . ?
N6 Y1 Ni1 147.17(6) . . ?
O5 Ni1 O1 89.16(9) . . ?
O5 Ni1 O3 89.71(9) . . ?
O1 Ni1 O3 80.77(9) . . ?
O5 Ni1 N4 93.31(10) . . ?
O1 Ni1 N4 168.36(10) . . ?
O3 Ni1 N4 87.87(9) . . ?
O5 Ni1 O13 176.64(9) . . ?
O1 Ni1 O13 87.50(9) . . ?
O3 Ni1 O13 90.03(9) . . ?
N4 Ni1 O13 90.03(10) . . ?
O5 Ni1 N2 91.86(10) . . ?
O1 Ni1 N2 87.51(9) . . ?
O3 Ni1 N2 168.15(9) . . ?
N4 Ni1 N2 103.76(10) . . ?
O13 Ni1 N2 87.72(10) . . ?
O5 Ni1 Y1 81.02(6) . . ?
O1 Ni1 Y1 40.76(6) . . ?
O3 Ni1 Y1 41.39(6) . . ?
N4 Ni1 Y1 128.52(7) . . ?
O13 Ni1 Y1 96.60(7) . . ?
N2 Ni1 Y1 127.41(7) . . ?
C4 Fe1 C25 158.27(14) . . ?
C4 Fe1 C31 120.02(14) . . ?
C25 Fe1 C31 41.12(13) . . ?
C4 Fe1 C34 40.88(13) . . ?
C25 Fe1 C34 123.79(13) . . ?
C31 Fe1 C34 105.51(14) . . ?
C4 Fe1 C3 40.79(15) . . ?
C25 Fe1 C3 160.55(14) . . ?
C31 Fe1 C3 156.44(14) . . ?
C34 Fe1 C3 68.72(14) . . ?
C4 Fe1 C2 68.48(14) . . ?
C25 Fe1 C2 125.69(13) . . ?
C31 Fe1 C2 160.62(13) . . ?
C34 Fe1 C2 68.71(14) . . ?
C3 Fe1 C2 40.51(14) . . ?
C4 Fe1 C33 156.85(14) . . ?
C25 Fe1 C33 41.05(13) . . ?
C31 Fe1 C33 69.06(14) . . ?
C34 Fe1 C33 161.98(13) . . ?
C3 Fe1 C33 123.13(15) . . ?
C2 Fe1 C33 110.42(14) . . ?
C4 Fe1 C32 119.52(14) . . ?
C25 Fe1 C32 68.65(13) . . ?
C31 Fe1 C32 68.69(15) . . ?
C34 Fe1 C32 155.09(14) . . ?
C3 Fe1 C32 106.43(15) . . ?
C2 Fe1 C32 124.38(15) . . ?
C33 Fe1 C32 40.60(13) . . ?
C4 Fe1 C26 103.85(14) . . ?
C25 Fe1 C26 68.52(13) . . ?
C31 Fe1 C26 40.71(13) . . ?
C34 Fe1 C26 119.49(14) . . ?
C3 Fe1 C26 120.74(14) . . ?
C2 Fe1 C26 158.40(14) . . ?
C33 Fe1 C26 68.31(14) . . ?
C32 Fe1 C26 40.47(15) . . ?
C4 Fe1 C1 68.75(13) . . ?
C25 Fe1 C1 109.95(13) . . ?
C31 Fe1 C1 122.85(13) . . ?
C34 Fe1 C1 40.92(13) . . ?
C3 Fe1 C1 68.61(14) . . ?
C2 Fe1 C1 40.87(13) . . ?
C33 Fe1 C1 126.60(13) . . ?
C32 Fe1 C1 162.07(14) . . ?
C26 Fe1 C1 157.05(14) . . ?
N6 O11 Y1 94.09(18) . . ?
C27 O6 Y1 135.2(2) . . ?
C16 O4 C15 115.3(3) . . ?
C16 O4 Y1 117.48(19) . . ?
C15 O4 Y1 127.1(2) . . ?
C12 O2 C14 116.2(3) . . ?
C12 O2 Y1 117.82(19) . . ?
C14 O2 Y1 125.6(2) . . ?
N6 O10 Y1 95.67(19) . . ?
N5 O8 Y1 95.9(2) . . ?
C21 O3 Ni1 128.6(2) . . ?
C21 O3 Y1 128.31(19) . . ?
Ni1 O3 Y1 102.63(9) . . ?
C5 N1 N2 117.7(3) . . ?
C13 O1 Ni1 124.74(19) . . ?
C13 O1 Y1 127.03(19) . . ?
Ni1 O1 Y1 103.56(9) . . ?
C27 O5 Ni1 129.1(2) . . ?
N5 O7 Y1 93.3(2) . . ?
C22 N4 N3 112.0(3) . . ?
C22 N4 Ni1 125.6(2) . . ?
N3 N4 Ni1 122.00(19) . . ?
C23 N3 N4 115.7(2) . . ?
N3 C23 C25 116.5(3) . . ?
N3 C23 C24 125.4(3) . . ?
C25 C23 C24 118.0(3) . . ?
C13 C8 C9 119.2(3) . . ?
C13 C8 C7 124.0(3) . . ?
C9 C8 C7 116.7(3) . . ?
C19 C20 C21 119.6(3) . . ?
C19 C20 C22 116.9(3) . . ?
C21 C20 C22 123.3(3) . . ?
C7 N2 N1 111.7(3) . . ?
C7 N2 Ni1 120.6(2) . . ?
N1 N2 Ni1 124.45(19) . . ?
C17 C16 O4 125.3(3) . . ?
C17 C16 C21 122.3(3) . . ?
O4 C16 C21 112.4(3) . . ?
C11 C12 O2 125.0(3) . . ?
C11 C12 C13 122.4(3) . . ?
O2 C12 C13 112.6(3) . . ?
O5 C27 O6 125.7(3) . . ?
O5 C27 C28 115.7(3) . . ?
O6 C27 C28 118.6(3) . . ?
O3 C21 C20 124.1(3) . . ?
O3 C21 C16 118.5(3) . . ?
C20 C21 C16 117.4(3) . . ?
C2 C1 C34 107.4(3) . . ?
C2 C1 C5 125.3(3) . . ?
C34 C1 C5 127.3(3) . . ?
C2 C1 Fe1 69.27(19) . . ?
C34 C1 Fe1 69.11(19) . . ?
C5 C1 Fe1 127.1(2) . . ?
C18 C19 C20 121.0(3) . . ?
N1 C5 C1 116.8(3) . . ?
N1 C5 C6 125.5(3) . . ?
C1 C5 C6 117.5(3) . . ?
C10 C9 C8 120.8(3) . . ?
C33 C25 C31 107.9(3) . . ?
C33 C25 C23 126.0(3) . . ?
C31 C25 C23 126.1(3) . . ?
C33 C25 Fe1 69.74(19) . . ?
C31 C25 Fe1 69.45(18) . . ?
C23 C25 Fe1 126.5(2) . . ?
C2 C3 C4 108.1(3) . . ?
C2 C3 Fe1 69.8(2) . . ?
C4 C3 Fe1 69.4(2) . . ?
C9 C10 C11 120.6(3) . . ?
O12 N6 O11 121.4(3) . . ?
O12 N6 O10 121.3(3) . . ?
O11 N6 O10 117.3(3) . . ?
O12 N6 Y1 172.9(2) . . ?
O11 N6 Y1 59.60(15) . . ?
O10 N6 Y1 58.07(15) . . ?
O1 C13 C8 124.2(3) . . ?
O1 C13 C12 117.7(3) . . ?
C8 C13 C12 118.1(3) . . ?
C19 C18 C17 120.0(3) . . ?
N2 C7 C8 127.7(3) . . ?
C12 C11 C10 118.9(3) . . ?
C3 C4 C34 108.2(3) . . ?
C3 C4 Fe1 69.9(2) . . ?
C34 C4 Fe1 69.68(19) . . ?
C32 C26 C31 108.5(3) . . ?
C32 C26 Fe1 69.6(2) . . ?
C31 C26 Fe1 69.17(19) . . ?
N4 C22 C20 127.3(3) . . ?
C16 C17 C18 119.4(3) . . ?
O9 N5 O8 122.1(3) . . ?
O9 N5 O7 121.5(3) . . ?
O8 N5 O7 116.2(3) . . ?
O9 N5 Y1 170.3(4) . . ?
O8 N5 Y1 57.49(17) . . ?
O7 N5 Y1 59.08(18) . . ?
N7 C29 C30 179.0(5) . . ?
C4 C34 C1 108.0(3) . . ?
C4 C34 Fe1 69.43(19) . . ?
C1 C34 Fe1 69.98(19) . . ?
C26 C31 C25 107.5(3) . . ?
C26 C31 Fe1 70.1(2) . . ?
C25 C31 Fe1 69.43(19) . . ?
C32 C33 C25 107.7(3) . . ?
C32 C33 Fe1 69.7(2) . . ?
C25 C33 Fe1 69.21(18) . . ?
C26 C32 C33 108.4(3) . . ?
C26 C32 Fe1 70.0(2) . . ?
C33 C32 Fe1 69.7(2) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.084
_database_code_depnum_ccdc_archive 'CCDC 993949'
