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

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#                                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
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data_complex-1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C100 H72 Dy2 N20 Ni8 O28, 2(Cl O4), 16(O)'
_chemical_formula_sum            'C100 H72 Cl2 Dy2 N20 Ni8 O52'
_chemical_formula_weight         3251.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_hall  '-P 2ybc'

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

_cell_length_a                   18.104(5)
_cell_length_b                   21.575(5)
_cell_length_c                   17.072(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 115.356(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     6026(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2578
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      27.68

_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.792

_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3236.0
_exptl_absorpt_coefficient_mu    2.589
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_T_max  0.774
_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            31306
_diffrn_reflns_av_R_equivalents  0.1331
_diffrn_reflns_av_unetI/netI     0.1727
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.89
_diffrn_reflns_theta_max         25.50
_reflns_number_total             11114
_reflns_number_gt                5052
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Due to the weak high-angle diffractions internal R-value is high.
 Actual molecular formula is C100 H108 Cl2 Dy2 N20 Ni8 O52 which differ from    calculated molecular formula because hydrogens of sixteen water molecules, 
 two -OH   and two oxime-OH could not be modeled.
 
 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)+(0.1565P)²+14.0103P] 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         11114
_refine_ls_number_parameters     796
_refine_ls_number_restraints     52
_refine_ls_R_factor_all          0.2186
_refine_ls_R_factor_gt           0.1124
_refine_ls_wR_factor_ref         0.3278
_refine_ls_wR_factor_gt          0.2641
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.008
_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
C1 C 0.6758(13) 0.4114(8) 0.7949(13) 0.054(5) Uani 1 1 d . . .
C2 C 0.7364(12) 0.3940(8) 0.7764(12) 0.051(5) Uani 1 1 d . . .
H2 H 0.7897 0.4047 0.8136 0.061 Uiso 1 1 calc R . .
C3 C 0.7210(13) 0.3589(8) 0.6997(13) 0.055(5) Uani 1 1 d . . .
H3 H 0.7636 0.3495 0.6851 0.066 Uiso 1 1 calc R . .
C4 C 0.6429(12) 0.3391(8) 0.6479(12) 0.055(5) Uani 1 1 d . . .
H4 H 0.6328 0.3154 0.5989 0.065 Uiso 1 1 calc R . .
C5 C 0.5763(11) 0.3553(8) 0.6698(12) 0.049(5) Uani 1 1 d . . .
C6 C 0.5943(11) 0.3922(7) 0.7444(11) 0.040(3) Uani 1 1 d . . .
C7 C 0.4958(13) 0.3357(8) 0.6209(13) 0.057(5) Uani 1 1 d . . .
H7 H 0.4826 0.3110 0.5721 0.069 Uiso 1 1 calc R . .
C8 C 0.4359(12) 0.3537(9) 0.6464(12) 0.055(5) Uani 1 1 d . . .
H8 H 0.3820 0.3410 0.6156 0.066 Uiso 1 1 calc R . .
C9 C 0.4587(12) 0.3916(8) 0.7203(12) 0.050(5) Uani 1 1 d . . .
C10 C 0.3994(11) 0.4162(8) 0.7495(12) 0.047(5) Uani 1 1 d . . .
H10 H 0.3447 0.4045 0.7236 0.057 Uiso 1 1 calc R . .
C11 C 0.5213(11) 0.6104(8) 0.9070(12) 0.047(5) Uani 1 1 d . . .
H11 H 0.5710 0.6248 0.9103 0.057 Uiso 1 1 calc R . .
C12 C 0.4447(11) 0.6429(8) 0.8566(12) 0.045(5) Uani 1 1 d . . .
C13 C 0.4333(12) 0.6955(8) 0.8033(12) 0.052(5) Uani 1 1 d . . .
H13 H 0.4775 0.7159 0.8007 0.062 Uiso 1 1 calc R . .
C14 C 0.3543(12) 0.7152(9) 0.7553(13) 0.056(5) Uani 1 1 d . . .
H14 H 0.3452 0.7487 0.7180 0.067 Uiso 1 1 calc R . .
C15 C 0.2881(12) 0.6872(8) 0.7606(12) 0.050(5) Uani 1 1 d . . .
C16 C 0.3066(11) 0.6368(8) 0.8199(12) 0.045(4) Uani 1 1 d . . .
C17 C 0.2454(11) 0.6034(9) 0.8307(11) 0.048(5) Uani 1 1 d . . .
C18 C 0.1640(14) 0.6213(10) 0.7824(13) 0.066(6) Uani 1 1 d . . .
H18 H 0.1221 0.6010 0.7898 0.079 Uiso 1 1 calc R . .
C19 C 0.1458(12) 0.6705(10) 0.7221(13) 0.059(5) Uani 1 1 d . . .
H19 H 0.0918 0.6805 0.6862 0.071 Uiso 1 1 calc R . .
C20 C 0.2092(13) 0.7037(9) 0.7171(14) 0.061(5) Uani 1 1 d . . .
H20 H 0.1966 0.7388 0.6822 0.074 Uiso 1 1 calc R . .
C21 C 0.4162(11) 0.6548(8) 1.0519(11) 0.044(4) Uani 1 1 d . . .
C22 C 0.4889(12) 0.6857(9) 1.0768(11) 0.054(5) Uani 1 1 d . . .
H22 H 0.5350 0.6631 1.0836 0.065 Uiso 1 1 calc R . .
C23 C 0.4970(13) 0.7488(8) 1.0922(12) 0.054(4) Uani 1 1 d . . .
H23 H 0.5479 0.7677 1.1110 0.065 Uiso 1 1 calc R . .
C24 C 0.4293(13) 0.7830(8) 1.0793(12) 0.054(4) Uani 1 1 d . . .
H24 H 0.4344 0.8256 1.0884 0.065 Uiso 1 1 calc R . .
C25 C 0.3536(12) 0.7558(7) 1.0531(11) 0.044(4) Uani 1 1 d . . .
C26 C 0.3478(12) 0.6927(8) 1.0389(11) 0.047(5) Uani 1 1 d . . .
C27 C 0.2808(14) 0.7855(9) 1.0376(13) 0.059(5) Uani 1 1 d . . .
H27 H 0.2811 0.8281 1.0457 0.071 Uiso 1 1 calc R . .
C28 C 0.2108(13) 0.7549(9) 1.0116(12) 0.057(5) Uani 1 1 d . . .
H28 H 0.1626 0.7764 0.9998 0.069 Uiso 1 1 calc R . .
C29 C 0.2092(12) 0.6901(8) 1.0017(11) 0.044(4) Uani 1 1 d . . .
C30 C 0.1362(12) 0.6513(9) 0.9741(12) 0.052(5) Uani 1 1 d . . .
H30 H 0.0844 0.6674 0.9603 0.062 Uiso 1 1 calc R . .
C31 C 0.4690(11) 0.4511(7) 1.2834(13) 0.043(4) Uani 1 1 d . . .
C32 C 0.5497(13) 0.4520(8) 1.3368(13) 0.057(5) Uani 1 1 d . . .
H32 H 0.5877 0.4575 1.3142 0.068 Uiso 1 1 calc R . .
C33 C 0.5767(14) 0.4446(8) 1.4279(15) 0.065(6) Uani 1 1 d . . .
H33 H 0.6325 0.4436 1.4632 0.078 Uiso 1 1 calc R . .
C34 C 0.5233(15) 0.4387(10) 1.4655(16) 0.073(6) Uani 1 1 d . . .
H34 H 0.5429 0.4356 1.5254 0.088 Uiso 1 1 calc R . .
C35 C 0.4383(13) 0.4375(8) 1.4122(15) 0.059(6) Uani 1 1 d . . .
C36 C 0.4146(12) 0.4428(8) 1.3217(13) 0.050(5) Uani 1 1 d . . .
C37 C 0.3741(14) 0.4336(9) 1.4392(15) 0.065(6) Uani 1 1 d . . .
H37 H 0.3871 0.4291 1.4978 0.079 Uiso 1 1 calc R . .
C38 C 0.2965(13) 0.4363(9) 1.3825(14) 0.060(5) Uani 1 1 d . . .
H38 H 0.2553 0.4338 1.4013 0.072 Uiso 1 1 calc R . .
C39 C 0.2765(12) 0.4430(8) 1.2937(14) 0.055(5) Uani 1 1 d . . .
C40 C 0.1982(12) 0.4433(8) 1.2235(13) 0.053(3) Uani 1 1 d . . .
H40 H 0.1522 0.4375 1.2337 0.063 Uiso 1 1 calc R . .
C41 C 0.1318(14) 0.3012(10) 0.9313(16) 0.069(5) Uani 1 1 d . . .
C42 C 0.1629(14) 0.2408(9) 0.9589(19) 0.084(8) Uani 1 1 d . . .
H42 H 0.2037 0.2329 1.0140 0.101 Uiso 1 1 calc R . .
C43 C 0.1261(18) 0.1918(11) 0.895(2) 0.095(10) Uani 1 1 d . . .
H43 H 0.1431 0.1512 0.9102 0.114 Uiso 1 1 calc R . .
C44 C 0.0669(17) 0.2034(12) 0.811(2) 0.089(9) Uani 1 1 d . . .
H44 H 0.0478 0.1706 0.7723 0.107 Uiso 1 1 calc R . .
C45 C 0.0356(16) 0.2618(12) 0.784(2) 0.084(7) Uani 1 1 d . . .
C46 C 0.0688(14) 0.3115(10) 0.8443(16) 0.069(5) Uani 1 1 d . . .
C47 C -0.0264(16) 0.2791(15) 0.7054(19) 0.094(8) Uani 1 1 d . . .
H47 H -0.0506 0.2478 0.6649 0.113 Uiso 1 1 calc R . .
C48 C -0.0550(16) 0.3366(14) 0.6823(18) 0.093(8) Uani 1 1 d . . .
H48 H -0.0962 0.3462 0.6281 0.111 Uiso 1 1 calc R . .
C49 C -0.0162(13) 0.3819(11) 0.7488(17) 0.069(4) Uani 1 1 d . . .
C50 C -0.0406(15) 0.4488(10) 0.7292(14) 0.073(6) Uani 1 1 d . . .
H50 H -0.0808 0.4621 0.6764 0.088 Uiso 1 1 calc R . .
Cl13 Cl 0.1886(7) 0.5121(6) 0.5212(8) 0.178(4) Uani 1 1 d DU . .
Dy1 Dy 0.11065(6) 0.44759(4) 0.93791(6) 0.0502(3) Uani 1 1 d . . .
N1 N 0.5337(9) 0.4100(6) 0.7648(9) 0.040(3) Uani 1 1 d . . .
N2 N 0.4276(9) 0.4554(6) 0.8143(10) 0.048(4) Uani 1 1 d . . .
N3 N 0.3816(9) 0.6156(6) 0.8626(9) 0.040(3) Uani 1 1 d . . .
N4 N 0.5167(8) 0.5616(6) 0.9458(10) 0.044(4) Uani 1 1 d . . .
N5 N 0.2777(9) 0.6615(6) 1.0159(9) 0.043(4) Uani 1 1 d . . .
N6 N 0.1496(9) 0.5927(7) 0.9706(9) 0.047(4) Uani 1 1 d . . .
N7 N 0.3349(10) 0.4453(7) 1.2693(11) 0.055(4) Uani 1 1 d . . .
N8 N 0.1896(10) 0.4517(6) 1.1447(11) 0.053(3) Uani 1 1 d . . .
N9 N 0.0430(11) 0.3685(8) 0.8254(13) 0.069(4) Uani 1 1 d . . .
N10 N -0.0012(9) 0.4854(7) 0.7915(11) 0.059(4) Uani 1 1 d . . .
Ni1 Ni 0.40180(14) 0.54142(9) 0.93599(15) 0.0409(6) Uani 1 1 d . . .
Ni2 Ni 0.44763(14) 0.53200(10) 1.13806(15) 0.0436(6) Uani 1 1 d . . .
Ni3 Ni 0.30262(14) 0.45499(10) 1.14162(16) 0.0462(6) Uani 1 1 d . . .
Ni4 Ni 0.26848(14) 0.56799(9) 1.00695(15) 0.0426(6) Uani 1 1 d . . .
O1 O 0.1672(8) 0.4611(5) 0.8355(9) 0.057(3) Uani 1 1 d . . .
H1A H 0.2118 0.4381 0.8499 0.085 Uiso 1 1 d R . .
H1B H 0.1320 0.4499 0.7825 0.085 Uiso 1 1 d R . .
O2 O -0.0221(9) 0.4414(6) 0.9355(9) 0.069(4) Uani 1 1 d . . .
H2A H -0.0197 0.4301 0.9873 0.104 Uiso 1 1 d R . .
H2B H -0.0482 0.4779 0.9219 0.104 Uiso 1 1 d R . .
O3 O -0.0206(9) 0.5475(7) 0.7754(10) 0.075(4) Uani 1 1 d U . .
O4 O 0.1597(8) 0.3507(6) 0.9798(10) 0.070(4) Uani 1 1 d . . .
O5 O 0.3014(8) 0.3602(5) 1.1162(9) 0.060(4) Uani 1 1 d . . .
H5A H 0.3251 0.3403 1.1637 0.090 Uiso 1 1 d R . .
H5B H 0.2519 0.3481 1.0900 0.090 Uiso 1 1 d R . .
O6 O 0.3149(7) 0.5505(5) 1.1365(7) 0.047(3) Uani 1 1 d . . .
O7 O 0.4367(7) 0.4565(5) 1.1976(8) 0.046(3) Uani 1 1 d . . .
O8 O 0.2507(7) 0.4726(5) 1.0119(7) 0.046(3) Uani 1 1 d . . .
O9 O 0.0844(7) 0.5538(5) 0.9404(7) 0.049(3) Uani 1 1 d . . .
O10 O 0.1164(8) 0.4536(6) 1.0769(9) 0.060(4) Uani 1 1 d . . .
O11 O 0.4155(7) 0.4757(5) 1.0260(8) 0.050(3) Uani 1 1 d . . .
O12 O 0.2657(7) 0.5571(5) 0.8882(8) 0.048(3) Uani 1 1 d . . .
O13 O 0.3736(7) 0.4778(6) 0.8425(9) 0.057(4) Uani 1 1 d . . .
O15 O 0.3019(10) 0.3753(7) 0.8882(11) 0.111(6) Uani 1 1 d G . .
O17 O 0.3076(8) 0.2501(7) 0.3854(10) 0.242(19) Uani 1 1 d G . .
O20 O 0.9981(14) 0.6057(17) 0.4910(18) 0.33(3) Uani 1 1 d G . .
O18 O 0.2500(8) 0.2798(9) 0.2260(9) 0.232(17) Uani 1 1 d G . .
O19 O 0.2302(10) 0.1834(10) 0.1902(11) 0.36(3) Uani 1 1 d G . .
O21 O 0.1297(12) 0.4729(9) 0.4586(14) 0.164(9) Uani 1 1 d DU . .
O22 O 0.2575(13) 0.4772(12) 0.5634(19) 0.277(16) Uani 1 1 d DU . .
O23 O 0.156(2) 0.5301(15) 0.5782(19) 0.327(19) Uani 1 1 d DU . .
O24 O 0.2009(15) 0.5644(9) 0.4821(16) 0.180(10) Uani 1 1 d DU . .
O25 O 0.9259(11) 0.6748(9) 0.8887(12) 0.112(6) Uani 1 1 d G . .
O26 O 0.4080(7) 0.5924(4) 1.0412(7) 0.039(3) Uani 1 1 d . . .
O27 O 0.0114(13) 0.7302(9) 0.5045(15) 0.140(7) Uani 1 1 d GU . .
O28 O 0.1061(16) 0.4398(9) 0.6630(13) 0.27(2) Uani 1 1 d G . .


_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
C1 C2 1.32(3) . ?
C1 O6 1.38(2) 3_667 ?
C1 C6 1.42(2) . ?
C2 C3 1.43(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.38(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.45(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.42(2) . ?
C5 C7 1.40(3) . ?
C6 N1 1.34(2) . ?
C7 C8 1.39(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.41(2) . ?
C8 H8 0.9300 . ?
C9 N1 1.30(2) . ?
C9 C10 1.46(2) . ?
C10 N2 1.31(2) . ?
C10 H10 0.9300 . ?
C11 N4 1.26(2) . ?
C11 C12 1.46(2) . ?
C11 H11 0.9300 . ?
C12 N3 1.33(2) . ?
C12 C13 1.41(2) . ?
C13 C14 1.38(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.38(3) . ?
C14 H14 0.9300 . ?
C15 C20 1.35(3) . ?
C15 C16 1.43(3) . ?
C16 N3 1.32(2) . ?
C16 C17 1.40(2) . ?
C17 O12 1.34(2) . ?
C17 C18 1.40(3) . ?
C18 C19 1.42(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.39(3) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 O26 1.357(19) . ?
C21 C22 1.37(2) . ?
C21 C26 1.42(2) . ?
C22 C23 1.38(2) . ?
C22 H22 0.9300 . ?
C23 C24 1.37(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.38(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.38(2) . ?
C25 C27 1.39(3) . ?
C26 N5 1.34(2) . ?
C27 C28 1.33(3) . ?
C27 H27 0.9300 . ?
C28 C29 1.41(2) . ?
C28 H28 0.9300 . ?
C29 N5 1.31(2) . ?
C29 C30 1.46(2) . ?
C30 N6 1.29(2) . ?
C30 H30 0.9300 . ?
C31 O7 1.33(2) . ?
C31 C32 1.35(3) . ?
C31 C36 1.41(3) . ?
C32 C33 1.42(3) . ?
C32 H32 0.9300 . ?
C33 C34 1.38(3) . ?
C33 H33 0.9300 . ?
C34 C35 1.41(3) . ?
C34 H34 0.9300 . ?
C35 C37 1.42(3) . ?
C35 C36 1.42(3) . ?
C36 N7 1.33(2) . ?
C37 C38 1.32(3) . ?
C37 H37 0.9300 . ?
C38 C39 1.41(3) . ?
C38 H38 0.9300 . ?
C39 N7 1.29(2) . ?
C39 C40 1.41(3) . ?
C40 N8 1.30(2) . ?
C40 H40 0.9300 . ?
C41 O4 1.31(2) . ?
C41 C42 1.42(3) . ?
C41 C46 1.45(3) . ?
C42 C43 1.46(3) . ?
C42 H42 0.9300 . ?
C43 C44 1.39(4) . ?
C43 H43 0.9300 . ?
C44 C45 1.38(3) . ?
C44 H44 0.9300 . ?
C45 C47 1.38(3) . ?
C45 C46 1.43(3) . ?
C46 N9 1.31(3) . ?
C47 C48 1.34(3) . ?
C47 H47 0.9300 . ?
C48 C49 1.43(3) . ?
C48 H48 0.9300 . ?
C49 N9 1.32(3) . ?
C49 C50 1.51(3) . ?
C50 N10 1.27(2) . ?
C50 H50 0.9300 . ?
Cl13 O22 1.368(15) . ?
Cl13 O24 1.377(14) . ?
Cl13 O23 1.391(16) . ?
Cl13 O21 1.420(14) . ?
Dy1 O4 2.265(14) . ?
Dy1 O10 2.334(14) . ?
Dy1 O9 2.344(12) . ?
Dy1 O8 2.360(12) . ?
Dy1 O1 2.391(12) . ?
Dy1 O2 2.391(14) . ?
Dy1 N9 2.467(18) . ?
Dy1 N10 2.585(17) . ?
N1 Ni2 1.987(14) 3_667 ?
N2 O13 1.349(18) . ?
N2 Ni2 2.065(15) 3_667 ?
N3 Ni1 1.968(14) . ?
N4 O11 1.372(17) 3_667 ?
N4 Ni1 2.061(13) . ?
N5 Ni4 2.025(13) . ?
N6 O9 1.358(17) . ?
N6 Ni4 2.039(15) . ?
N7 Ni3 2.011(17) . ?
N8 O10 1.336(19) . ?
N8 Ni3 2.070(16) . ?
N10 O3 1.381(19) . ?
Ni1 O13 1.998(12) . ?
Ni1 O11 2.026(12) . ?
Ni1 O26 2.068(11) . ?
Ni1 O12 2.265(12) . ?
Ni2 O7 1.974(11) . ?
Ni2 O26 1.983(10) . ?
Ni2 N1 1.987(14) 3_667 ?
Ni2 N2 2.065(15) 3_667 ?
Ni2 O11 2.126(11) . ?
Ni3 O8 2.038(12) . ?
Ni3 O6 2.078(11) . ?
Ni3 O5 2.089(12) . ?
Ni3 O7 2.195(12) . ?
Ni4 O12 2.020(13) . ?
Ni4 O6 2.036(12) . ?
Ni4 O8 2.090(11) . ?
Ni4 O26 2.394(11) . ?
O1 H1A 0.8880 . ?
O1 H1B 0.8889 . ?
O2 H2A 0.8988 . ?
O2 H2B 0.8970 . ?
O5 H5A 0.8535 . ?
O5 H5B 0.8535 . ?
O6 C1 1.38(2) 3_667 ?
O11 N4 1.372(17) 3_667 ?

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
C2 C1 O6 124.1(19) . 3_667 ?
C2 C1 C6 121.9(19) . . ?
O6 C1 C6 114.0(17) 3_667 . ?
C1 C2 C3 121(2) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 H2 119.6 . . ?
C4 C3 C2 119.7(19) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 120.0(19) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C7 119.1(17) . . ?
C6 C5 C4 118.1(17) . . ?
C7 C5 C4 122.9(18) . . ?
N1 C6 C5 119.7(16) . . ?
N1 C6 C1 120.9(16) . . ?
C5 C6 C1 119.4(17) . . ?
C8 C7 C5 118.9(17) . . ?
C8 C7 H7 120.5 . . ?
C5 C7 H7 120.5 . . ?
C7 C8 C9 118.4(18) . . ?
C7 C8 H8 120.8 . . ?
C9 C8 H8 120.8 . . ?
N1 C9 C8 122.2(18) . . ?
N1 C9 C10 115.1(15) . . ?
C8 C9 C10 122.6(18) . . ?
N2 C10 C9 116.4(16) . . ?
N2 C10 H10 121.8 . . ?
C9 C10 H10 121.8 . . ?
N4 C11 C12 116.7(17) . . ?
N4 C11 H11 121.6 . . ?
C12 C11 H11 121.6 . . ?
N3 C12 C13 120.9(17) . . ?
N3 C12 C11 111.8(16) . . ?
C13 C12 C11 127.2(16) . . ?
C14 C13 C12 117.3(17) . . ?
C14 C13 H13 121.3 . . ?
C12 C13 H13 121.3 . . ?
C15 C14 C13 122.4(19) . . ?
C15 C14 H14 118.8 . . ?
C13 C14 H14 118.8 . . ?
C20 C15 C14 126(2) . . ?
C20 C15 C16 117.7(19) . . ?
C14 C15 C16 115.8(18) . . ?
N3 C16 C17 115.9(17) . . ?
N3 C16 C15 122.0(17) . . ?
C17 C16 C15 121.8(17) . . ?
O12 C17 C18 121.8(18) . . ?
O12 C17 C16 119.8(16) . . ?
C18 C17 C16 118.4(19) . . ?
C17 C18 C19 119(2) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
C20 C19 C18 119.5(19) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C15 C20 C19 123(2) . . ?
C15 C20 H20 118.6 . . ?
C19 C20 H20 118.6 . . ?
O26 C21 C22 124.0(17) . . ?
O26 C21 C26 120.8(15) . . ?
C22 C21 C26 115.2(17) . . ?
C21 C22 C23 123(2) . . ?
C21 C22 H22 118.4 . . ?
C23 C22 H22 118.4 . . ?
C24 C23 C22 119.1(19) . . ?
C24 C23 H23 120.5 . . ?
C22 C23 H23 120.5 . . ?
C23 C24 C25 121.5(17) . . ?
C23 C24 H24 119.3 . . ?
C25 C24 H24 119.3 . . ?
C26 C25 C24 117.9(17) . . ?
C26 C25 C27 115.3(18) . . ?
C24 C25 C27 126.7(17) . . ?
N5 C26 C25 122.6(18) . . ?
N5 C26 C21 114.3(16) . . ?
C25 C26 C21 123.1(17) . . ?
C28 C27 C25 122.0(18) . . ?
C28 C27 H27 119.0 . . ?
C25 C27 H27 119.0 . . ?
C27 C28 C29 120.1(19) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
N5 C29 C28 118.4(17) . . ?
N5 C29 C30 116.3(15) . . ?
C28 C29 C30 125.3(18) . . ?
N6 C30 C29 114.4(16) . . ?
N6 C30 H30 122.8 . . ?
C29 C30 H30 122.8 . . ?
O7 C31 C32 125.6(17) . . ?
O7 C31 C36 117.2(16) . . ?
C32 C31 C36 117.2(18) . . ?
C31 C32 C33 120(2) . . ?
C31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C34 C33 C32 123(2) . . ?
C34 C33 H33 118.7 . . ?
C32 C33 H33 118.7 . . ?
C33 C34 C35 119(2) . . ?
C33 C34 H34 120.4 . . ?
C35 C34 H34 120.4 . . ?
C34 C35 C37 127(2) . . ?
C34 C35 C36 116(2) . . ?
C37 C35 C36 117(2) . . ?
N7 C36 C31 117.0(18) . . ?
N7 C36 C35 118.0(19) . . ?
C31 C36 C35 124.7(18) . . ?
C38 C37 C35 121(2) . . ?
C38 C37 H37 119.3 . . ?
C35 C37 H37 119.3 . . ?
C37 C38 C39 120(2) . . ?
C37 C38 H38 120.2 . . ?
C39 C38 H38 120.2 . . ?
N7 C39 C38 118.8(19) . . ?
N7 C39 C40 113(2) . . ?
C38 C39 C40 128.1(19) . . ?
N8 C40 C39 120.7(19) . . ?
N8 C40 H40 119.6 . . ?
C39 C40 H40 119.6 . . ?
O4 C41 C42 123(2) . . ?
O4 C41 C46 116(2) . . ?
C42 C41 C46 121(2) . . ?
C41 C42 C43 115(3) . . ?
C41 C42 H42 122.4 . . ?
C43 C42 H42 122.4 . . ?
C44 C43 C42 123(2) . . ?
C44 C43 H43 118.6 . . ?
C42 C43 H43 118.6 . . ?
C45 C44 C43 122(2) . . ?
C45 C44 H44 118.8 . . ?
C43 C44 H44 118.8 . . ?
C47 C45 C44 129(3) . . ?
C47 C45 C46 114(2) . . ?
C44 C45 C46 117(3) . . ?
N9 C46 C45 122(2) . . ?
N9 C46 C41 116(2) . . ?
C45 C46 C41 122(2) . . ?
C48 C47 C45 126(3) . . ?
C48 C47 H47 116.9 . . ?
C45 C47 H47 116.9 . . ?
C47 C48 C49 114(3) . . ?
C47 C48 H48 123.1 . . ?
C49 C48 H48 123.1 . . ?
N9 C49 C48 123(2) . . ?
N9 C49 C50 118(2) . . ?
C48 C49 C50 119(2) . . ?
N10 C50 C49 114(2) . . ?
N10 C50 H50 123.1 . . ?
C49 C50 H50 123.1 . . ?
O22 Cl13 O24 113.9(15) . . ?
O22 Cl13 O23 110.4(15) . . ?
O24 Cl13 O23 108.2(14) . . ?
O22 Cl13 O21 106.9(14) . . ?
O24 Cl13 O21 110.4(13) . . ?
O23 Cl13 O21 106.7(14) . . ?
O4 Dy1 O10 83.6(5) . . ?
O4 Dy1 O9 162.2(5) . . ?
O10 Dy1 O9 81.3(4) . . ?
O4 Dy1 O8 81.7(4) . . ?
O10 Dy1 O8 82.7(4) . . ?
O9 Dy1 O8 86.9(4) . . ?
O4 Dy1 O1 96.4(5) . . ?
O10 Dy1 O1 152.8(4) . . ?
O9 Dy1 O1 92.7(4) . . ?
O8 Dy1 O1 70.4(4) . . ?
O4 Dy1 O2 102.0(5) . . ?
O10 Dy1 O2 68.1(5) . . ?
O9 Dy1 O2 81.1(5) . . ?
O8 Dy1 O2 149.7(4) . . ?
O1 Dy1 O2 137.4(5) . . ?
O4 Dy1 N9 66.7(6) . . ?
O10 Dy1 N9 128.4(5) . . ?
O9 Dy1 N9 130.8(5) . . ?
O8 Dy1 N9 129.5(5) . . ?
O1 Dy1 N9 74.9(5) . . ?
O2 Dy1 N9 77.7(5) . . ?
O4 Dy1 N10 129.5(5) . . ?
O10 Dy1 N10 129.9(5) . . ?
O9 Dy1 N10 68.1(5) . . ?
O8 Dy1 N10 131.5(4) . . ?
O1 Dy1 N10 70.0(5) . . ?
O2 Dy1 N10 68.7(5) . . ?
N9 Dy1 N10 62.8(6) . . ?
C9 N1 C6 121.7(15) . . ?
C9 N1 Ni2 116.2(12) . 3_667 ?
C6 N1 Ni2 122.0(12) . 3_667 ?
C10 N2 O13 116.9(14) . . ?
C10 N2 Ni2 112.5(13) . 3_667 ?
O13 N2 Ni2 130.5(10) . 3_667 ?
C16 N3 C12 121.4(16) . . ?
C16 N3 Ni1 120.0(12) . . ?
C12 N3 Ni1 118.6(13) . . ?
C11 N4 O11 115.0(14) . 3_667 ?
C11 N4 Ni1 115.1(12) . . ?
O11 N4 Ni1 128.7(10) 3_667 . ?
C29 N5 C26 121.4(15) . . ?
C29 N5 Ni4 114.5(12) . . ?
C26 N5 Ni4 124.0(12) . . ?
C30 N6 O9 118.2(16) . . ?
C30 N6 Ni4 115.9(13) . . ?
O9 N6 Ni4 125.9(11) . . ?
C39 N7 C36 125.5(19) . . ?
C39 N7 Ni3 117.0(14) . . ?
C36 N7 Ni3 117.4(14) . . ?
C40 N8 O10 122.3(16) . . ?
C40 N8 Ni3 110.5(13) . . ?
O10 N8 Ni3 127.0(12) . . ?
C46 N9 C49 120(2) . . ?
C46 N9 Dy1 117.0(16) . . ?
C49 N9 Dy1 122.8(15) . . ?
C50 N10 O3 115.7(18) . . ?
C50 N10 Dy1 122.6(14) . . ?
O3 N10 Dy1 121.7(11) . . ?
N3 Ni1 O13 97.8(6) . . ?
N3 Ni1 O11 168.8(5) . . ?
O13 Ni1 O11 91.8(5) . . ?
N3 Ni1 N4 77.6(6) . . ?
O13 Ni1 N4 96.5(5) . . ?
O11 Ni1 N4 107.2(5) . . ?
N3 Ni1 O26 92.7(5) . . ?
O13 Ni1 O26 163.6(5) . . ?
O11 Ni1 O26 76.7(4) . . ?
N4 Ni1 O26 98.0(5) . . ?
N3 Ni1 O12 76.8(5) . . ?
O13 Ni1 O12 87.1(5) . . ?
O11 Ni1 O12 98.0(5) . . ?
N4 Ni1 O12 154.4(5) . . ?
O26 Ni1 O12 83.0(4) . . ?
O7 Ni2 O26 153.0(5) . . ?
O7 Ni2 N1 96.2(5) . 3_667 ?
O26 Ni2 N1 98.9(5) . 3_667 ?
O7 Ni2 N2 103.9(5) . 3_667 ?
O26 Ni2 N2 100.7(5) . 3_667 ?
N1 Ni2 N2 79.7(6) 3_667 3_667 ?
O7 Ni2 O11 86.7(5) . . ?
O26 Ni2 O11 76.3(4) . . ?
N1 Ni2 O11 173.6(5) 3_667 . ?
N2 Ni2 O11 105.1(5) 3_667 . ?
N7 Ni3 O8 169.2(6) . . ?
N7 Ni3 N8 78.5(7) . . ?
O8 Ni3 N8 91.9(6) . . ?
N7 Ni3 O6 99.3(5) . . ?
O8 Ni3 O6 77.1(4) . . ?
N8 Ni3 O6 99.2(5) . . ?
N7 Ni3 O5 95.5(6) . . ?
O8 Ni3 O5 89.9(5) . . ?
N8 Ni3 O5 92.8(5) . . ?
O6 Ni3 O5 162.5(5) . . ?
N7 Ni3 O7 77.0(6) . . ?
O8 Ni3 O7 112.3(5) . . ?
N8 Ni3 O7 155.5(6) . . ?
O6 Ni3 O7 83.4(4) . . ?
O5 Ni3 O7 91.0(5) . . ?
O12 Ni4 N5 99.1(5) . . ?
O12 Ni4 O6 152.8(5) . . ?
N5 Ni4 O6 96.9(5) . . ?
O12 Ni4 N6 99.0(5) . . ?
N5 Ni4 N6 78.7(6) . . ?
O6 Ni4 N6 105.7(5) . . ?
O12 Ni4 O8 89.3(5) . . ?
N5 Ni4 O8 170.8(5) . . ?
O6 Ni4 O8 76.9(4) . . ?
N6 Ni4 O8 96.3(5) . . ?
O12 Ni4 O26 80.8(4) . . ?
N5 Ni4 O26 73.6(5) . . ?
O6 Ni4 O26 82.8(4) . . ?
N6 Ni4 O26 151.9(5) . . ?
O8 Ni4 O26 111.8(4) . . ?
Dy1 O1 H1A 110.7 . . ?
Dy1 O1 H1B 111.6 . . ?
H1A O1 H1B 107.4 . . ?
Dy1 O2 H2A 111.9 . . ?
Dy1 O2 H2B 111.6 . . ?
H2A O2 H2B 106.9 . . ?
C41 O4 Dy1 124.0(15) . . ?
Ni3 O5 H5A 109.9 . . ?
Ni3 O5 H5B 109.0 . . ?
H5A O5 H5B 109.3 . . ?
C1 O6 Ni4 130.8(10) 3_667 . ?
C1 O6 Ni3 122.1(10) 3_667 . ?
Ni4 O6 Ni3 103.2(5) . . ?
C31 O7 Ni2 123.1(10) . . ?
C31 O7 Ni3 111.2(10) . . ?
Ni2 O7 Ni3 97.2(5) . . ?
Ni3 O8 Ni4 102.7(5) . . ?
Ni3 O8 Dy1 115.4(5) . . ?
Ni4 O8 Dy1 110.6(5) . . ?
N6 O9 Dy1 117.5(10) . . ?
N8 O10 Dy1 118.3(11) . . ?
N4 O11 Ni1 118.5(10) 3_667 . ?
N4 O11 Ni2 99.3(9) 3_667 . ?
Ni1 O11 Ni2 100.4(5) . . ?
C17 O12 Ni4 122.1(11) . . ?
C17 O12 Ni1 106.9(11) . . ?
Ni4 O12 Ni1 95.7(5) . . ?
N2 O13 Ni1 123.7(9) . . ?
C21 O26 Ni2 124.0(10) . . ?
C21 O26 Ni1 127.3(10) . . ?
Ni2 O26 Ni1 103.9(4) . . ?
C21 O26 Ni4 107.1(10) . . ?
Ni2 O26 Ni4 91.5(4) . . ?
Ni1 O26 Ni4 90.7(4) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         2.570
_refine_diff_density_min         -1.732
_refine_diff_density_rms         0.208

# start Validation Reply Form
_vrf_PLAT306_complex-1           
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O15 Check 
RESPONSE: Due to disorder of  water molecules their Hydrogen could not be 
located with out pointing in the wrong direction.
;
_vrf_PLAT342_complex-1           
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0320 Ang.  
RESPONSE: Disordered  carbon atoms in the structure leads to low bond 
precision and due to poor diffraction quality of the crystal it was not 
possible to model this disorder.
;
_database_code_depnum_ccdc_archive 'CCDC 986609'
#######################################################################
#
#                 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_complex-2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C102 H74 Gd2 N20 Ni8 O28, 2(N O3), 12(O)'
_chemical_formula_sum            'C102 H74 Gd2 N22 Ni8 O46'
_chemical_formula_weight         3127.86

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_hall  '-P 2ybc'


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

_cell_length_a                   18.148(5)
_cell_length_b                   21.542(6)
_cell_length_c                   17.094(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.989(5)
_cell_angle_gamma                90.00
_cell_volume                     6057(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1704
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      27.81

_exptl_crystal_description       Block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3120
_exptl_absorpt_coefficient_mu    2.387
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.716
_exptl_absorpt_correction_T_max  0.788
_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            30239
_diffrn_reflns_av_R_equivalents  0.1604
_diffrn_reflns_av_unetI/netI     0.2151
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.13
_diffrn_reflns_theta_max         25.03
_reflns_number_total             10614
_reflns_number_gt                4128
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Due to the weak high-angle diffractions internal R-value is high.
Actual molecular formula is C102 H104 Gd2 N22 Ni8 O46 which differ from calculated molecular formula because hydrogen of twelve water, two -OH, two oxime-OH and two coordinated MeOH could not be modeled.

 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)+(0.1260P)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         10614
_refine_ls_number_parameters     784
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.2288
_refine_ls_R_factor_gt           0.0931
_refine_ls_wR_factor_ref         0.2826
_refine_ls_wR_factor_gt          0.2138
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_restrained_S_all      0.979
_refine_ls_shift/su_max          0.003
_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
C1 C -0.0369(15) 1.0506(13) 0.7318(16) 0.096(7) Uani 1 1 d . . .
H1 H -0.0763 1.0366 0.6794 0.115 Uiso 1 1 calc R . .
C2 C -0.0173(16) 1.1155(13) 0.7439(17) 0.083(7) Uani 1 1 d . . .
C3 C -0.0536(14) 1.1614(11) 0.6838(16) 0.094(6) Uani 1 1 d . . .
H3 H -0.0952 1.1520 0.6302 0.113 Uiso 1 1 calc R . .
C4 C -0.0285(15) 1.2178(13) 0.7034(17) 0.094(6) Uani 1 1 d . . .
H4 H -0.0529 1.2482 0.6618 0.113 Uiso 1 1 calc R . .
C5 C 0.0346(17) 1.2370(14) 0.785(2) 0.104(8) Uani 1 1 d . . .
C6 C 0.0672(17) 1.1878(13) 0.842(2) 0.084(7) Uani 1 1 d . . .
C7 C 0.063(2) 1.2980(13) 0.809(2) 0.112(10) Uani 1 1 d . . .
H7 H 0.0430 1.3303 0.7692 0.135 Uiso 1 1 calc R . .
C8 C 0.122(2) 1.3093(13) 0.891(2) 0.115(10) Uani 1 1 d . . .
H8 H 0.1389 1.3499 0.9075 0.138 Uiso 1 1 calc R . .
C9 C 0.1561(15) 1.2621(10) 0.950(2) 0.112(10) Uani 1 1 d . . .
H9 H 0.1962 1.2705 1.0049 0.134 Uiso 1 1 calc R . .
C10 C 0.1287(16) 1.2008(10) 0.925(2) 0.079(7) Uani 1 1 d . . .
C11 C 0.2618(11) 0.8980(7) 1.2239(12) 0.056(5) Uani 1 1 d . . .
H11 H 0.2086 0.9091 1.1882 0.067 Uiso 1 1 calc R . .
C12 C 0.3239(11) 0.9144(8) 1.2034(11) 0.049(4) Uani 1 1 d . . .
C13 C 0.4040(12) 0.8951(6) 1.2565(10) 0.045(4) Uani 1 1 d . . .
C14 C 0.4214(13) 0.8580(8) 1.3318(11) 0.054(5) Uani 1 1 d . . .
C15 C 0.3554(15) 0.8436(8) 1.3525(14) 0.071(6) Uani 1 1 d . . .
H15 H 0.3651 0.8201 1.4015 0.085 Uiso 1 1 calc R . .
C16 C 0.2803(14) 0.8626(8) 1.3037(12) 0.061(5) Uani 1 1 d . . .
H16 H 0.2388 0.8534 1.3202 0.074 Uiso 1 1 calc R . .
C17 C 0.5399(12) 0.8967(7) 1.2791(11) 0.049(5) Uani 1 1 d . . .
C18 C 0.5604(12) 0.8587(7) 1.3527(12) 0.061(5) Uani 1 1 d . . .
H18 H 0.6142 0.8466 1.3835 0.073 Uiso 1 1 calc R . .
C19 C 0.5025(13) 0.8391(8) 1.3801(12) 0.061(5) Uani 1 1 d . . .
H19 H 0.5167 0.8142 1.4288 0.073 Uiso 1 1 calc R . .
C20 C 0.5975(13) 0.9205(8) 1.2500(13) 0.064(5) Uani 1 1 d . . .
H20 H 0.6524 0.9106 1.2774 0.076 Uiso 1 1 calc R . .
O11 O 0.9324(8) 0.8212(7) 0.8940(9) 0.146(7) Uani 1 1 d G . .
O9 O 0.1081(10) 0.0577(7) 0.6654(11) 0.267(18) Uani 1 1 d G . .
O6 O 0.0161(9) 0.7238(10) 0.0111(10) 0.261(15) Uani 1 1 d G . .
O8 O 0.6957(10) 0.7540(9) 0.1286(9) 0.269(14) Uani 1 1 d GU . .
O102 O 0.0064(11) 0.6075(9) 0.9959(13) 0.41(3) Uani 1 1 d G . .
C21 C 0.2485(12) 0.8931(9) 0.8345(12) 0.059(4) Uani 1 1 d . . .
C22 C 0.1691(12) 0.8747(8) 0.7861(11) 0.059(4) Uani 1 1 d . . .
H22 H 0.1269 0.8960 0.7915 0.071 Uiso 1 1 calc R . .
C23 C 0.1511(14) 0.8243(9) 0.7291(12) 0.076(6) Uani 1 1 d . . .
H23 H 0.0972 0.8128 0.6970 0.091 Uiso 1 1 calc R . .
C24 C 0.2106(12) 0.7928(8) 0.7205(12) 0.058(5) Uani 1 1 d . . .
H24 H 0.1973 0.7589 0.6834 0.070 Uiso 1 1 calc R . .
C25 C 0.2917(12) 0.8091(8) 0.7653(11) 0.049(4) Uani 1 1 d . . .
C26 C 0.3081(10) 0.8611(7) 0.8210(10) 0.046(4) Uani 1 1 d . . .
C27 C 0.4462(11) 0.8568(7) 0.8597(11) 0.048(3) Uani 1 1 d . . .
C28 C 0.4316(13) 0.8031(7) 0.8064(12) 0.059(5) Uani 1 1 d . . .
H28 H 0.4760 0.7824 0.8050 0.071 Uiso 1 1 calc R . .
C29 C 0.3566(12) 0.7810(8) 0.7580(12) 0.061(5) Uani 1 1 d . . .
H29 H 0.3489 0.7477 0.7207 0.073 Uiso 1 1 calc R . .
C30 C 0.5218(10) 0.8859(7) 0.9102(11) 0.048(3) Uani 1 1 d . . .
H30 H 0.5711 0.8694 0.9158 0.058 Uiso 1 1 calc R . .
C31 C 0.1398(13) 0.8486(10) 0.9752(12) 0.065(5) Uani 1 1 d . . .
H31 H 0.0881 0.8325 0.9607 0.078 Uiso 1 1 calc R . .
C32 C 0.2100(13) 0.8085(8) 1.0028(10) 0.055(5) Uani 1 1 d . . .
C33 C 0.2118(12) 0.7436(9) 1.0123(11) 0.055(5) Uani 1 1 d . . .
H33 H 0.1642 0.7214 0.9996 0.066 Uiso 1 1 calc R . .
C34 C 0.2820(17) 0.7149(9) 1.0393(12) 0.074(7) Uani 1 1 d . . .
H34 H 0.2830 0.6723 1.0482 0.089 Uiso 1 1 calc R . .
C35 C 0.3476(14) 0.8097(9) 1.0411(11) 0.066(6) Uani 1 1 d . . .
C36 C 0.3516(15) 0.7432(7) 1.0546(11) 0.053(5) Uani 1 1 d . . .
C37 C 0.4325(15) 0.7163(9) 1.0855(11) 0.066(6) Uani 1 1 d . . .
H37 H 0.4397 0.6743 1.0987 0.079 Uiso 1 1 calc R . .
C38 C 0.4951(14) 0.7506(9) 1.0950(11) 0.069(6) Uani 1 1 d . . .
H38 H 0.5452 0.7311 1.1124 0.083 Uiso 1 1 calc R . .
C39 C 0.4917(13) 0.8181(7) 1.0801(11) 0.058(5) Uani 1 1 d . . .
H39 H 0.5376 0.8406 1.0864 0.069 Uiso 1 1 calc R . .
C40 C 0.4192(11) 0.8456(8) 1.0571(10) 0.047(4) Uani 1 1 d . . .
C41 C 0.5327(12) 0.9499(7) 0.7179(14) 0.054(5) Uani 1 1 d . . .
C42 C 0.4538(11) 0.9487(7) 0.6642(12) 0.053(4) Uani 1 1 d . . .
H42 H 0.4146 0.9507 0.6857 0.063 Uiso 1 1 calc R . .
C43 C 0.4304(12) 0.9442(7) 0.5738(12) 0.061(5) Uani 1 1 d . . .
H43 H 0.3752 0.9469 0.5379 0.073 Uiso 1 1 calc R . .
C44 C 0.4809(13) 0.9366(8) 0.5364(12) 0.064(5) Uani 1 1 d . . .
H44 H 0.4617 0.9309 0.4771 0.077 Uiso 1 1 calc R . .
C45 C 0.5655(13) 0.9375(7) 0.5915(11) 0.060(5) Uani 1 1 d . . .
C46 C 0.5880(12) 0.9423(7) 0.6796(12) 0.053(5) Uani 1 1 d . . .
C47 C 0.6282(12) 0.9342(8) 0.5652(13) 0.063(5) Uani 1 1 d . . .
H47 H 0.6147 0.9312 0.5065 0.076 Uiso 1 1 calc R . .
C48 C 0.7081(12) 0.9351(7) 0.6209(11) 0.054(5) Uani 1 1 d . . .
H48 H 0.7491 0.9321 0.6021 0.065 Uiso 1 1 calc R . .
C49 C 0.7246(10) 0.9410(7) 0.7081(11) 0.050(4) Uani 1 1 d . . .
C50 C 0.8054(11) 0.9441(7) 0.7785(12) 0.056(5) Uani 1 1 d . . .
H50 H 0.8516 0.9404 0.7683 0.067 Uiso 1 1 calc R . .
C54 C 0.6716(12) 0.8159(8) 0.8294(13) 0.076(3) Uani 1 1 d U . .
H54A H 0.6203 0.8289 0.7853 0.114 Uiso 1 1 calc R . .
H54B H 0.6643 0.7784 0.8557 0.114 Uiso 1 1 calc R . .
H54C H 0.7092 0.8084 0.8043 0.114 Uiso 1 1 calc R . .
Gd1 Gd 0.11029(6) 1.05223(4) 0.93694(6) 0.0593(4) Uani 1 1 d . . .
N1 N -0.0015(10) 1.0134(10) 0.7909(11) 0.075(5) Uani 1 1 d . . .
N2 N 0.0397(11) 1.1298(9) 0.8207(13) 0.071(5) Uani 1 1 d . . .
N3 N 0.4649(10) 0.9127(5) 1.2343(9) 0.049(4) Uani 1 1 d . . .
N4 N 0.5697(9) 0.9558(6) 1.1848(9) 0.053(4) Uani 1 1 d . . .
N5 N 0.2762(10) 0.8402(6) 1.0174(8) 0.046(4) Uani 1 1 d . . .
N6 N 0.1507(9) 0.9070(7) 0.9714(8) 0.054(4) Uani 1 1 d . . .
N7 N 0.3848(9) 0.8835(5) 0.8668(8) 0.047(4) Uani 1 1 d . . .
N8 N 0.5174(8) 0.9366(6) 0.9473(8) 0.042(3) Uani 1 1 d . . .
N9 N 0.6685(9) 0.9448(6) 0.7355(9) 0.050(4) Uani 1 1 d . . .
N10 N 0.8112(9) 0.9520(6) 0.8559(10) 0.051(4) Uani 1 1 d . . .
N11 N 0.1952(7) 0.9901(6) 0.5192(7) 0.033(3) Uani 1 1 d D . .
Ni1 Ni 0.26837(14) 0.93234(9) 1.00732(14) 0.0487(6) Uani 1 1 d . . .
Ni2 Ni 0.40305(13) 0.95753(9) 0.93694(13) 0.0429(6) Uani 1 1 d . . .
Ni3 Ni 0.55372(14) 1.03050(9) 0.86284(14) 0.0476(6) Uani 1 1 d . . .
Ni4 Ni 0.69930(14) 0.95404(9) 0.86048(14) 0.0501(6) Uani 1 1 d . . .
O1 O 0.1677(7) 1.0382(5) 0.8347(8) 0.065(3) Uani 1 1 d . . .
H1A H 0.1907 1.0017 0.8413 0.098 Uiso 1 1 d R . .
H1B H 0.1300 1.0408 0.7818 0.098 Uiso 1 1 d R . .
O2 O -0.0244(7) 1.0585(6) 0.9349(8) 0.073(4) Uani 1 1 d . . .
H2A H -0.0469 1.0226 0.9243 0.110 Uiso 1 1 d R . .
H2B H -0.0201 1.0710 0.9843 0.110 Uiso 1 1 d R . .
O3 O 0.1993(13) 0.9362(8) 0.4956(18) 0.29(2) Uani 1 1 d D . .
O5 O 0.2549(11) 1.0213(11) 0.5636(15) 0.33(3) Uani 1 1 d D . .
O7 O 0.6953(11) 0.8817(7) 0.1095(12) 0.130(6) Uani 1 1 d G . .
O12 O 0.8843(7) 0.9527(5) 0.9223(8) 0.060(3) Uani 1 1 d . . .
O13 O -0.0199(8) 0.9505(7) 0.7744(9) 0.083(4) Uani 1 1 d . . .
O14 O 0.1559(9) 1.1516(6) 0.9776(9) 0.090(4) Uani 1 1 d . . .
O15 O 0.0851(7) 0.9433(6) 0.9398(7) 0.060(3) Uani 1 1 d . . .
O16 O 0.4061(6) 0.9082(4) 1.0419(7) 0.045(3) Uani 1 1 d . . .
O17 O 0.3131(7) 0.9500(4) 1.1367(7) 0.049(3) Uani 1 1 d . . .
O18 O 0.6237(7) 0.9780(5) 1.1567(7) 0.055(3) Uani 1 1 d . . .
O19 O 0.5858(7) 0.9753(4) 0.9742(7) 0.051(3) Uani 1 1 d . . .
O20 O 0.5656(7) 0.9548(5) 0.8054(8) 0.056(3) Uani 1 1 d . . .
O21 O 0.7017(8) 0.8614(5) 0.8907(9) 0.076(3) Uani 1 1 d . . .
O22 O 0.7487(7) 0.9728(5) 0.9900(7) 0.053(3) Uani 1 1 d . . .
O23 O 0.2678(7) 0.9426(5) 0.8895(7) 0.053(3) Uani 1 1 d . . .
O4 O 0.1351(13) 1.0236(10) 0.4708(16) 0.265(14) Uani 1 1 d DU . .


_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
C1 N1 1.24(2) . ?
C1 C2 1.44(3) . ?
C1 H1 0.9300 . ?
C2 N2 1.32(3) . ?
C2 C3 1.38(3) . ?
C3 C4 1.29(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.44(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.39(3) . ?
C5 C7 1.41(3) . ?
C6 N2 1.34(3) . ?
C6 C10 1.41(3) . ?
C7 C8 1.39(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.38(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.41(3) . ?
C9 H9 0.9300 . ?
C10 O14 1.34(2) . ?
C11 C12 1.36(2) . ?
C11 C16 1.47(2) . ?
C11 H11 0.9300 . ?
C12 O17 1.318(18) . ?
C12 C13 1.41(2) . ?
C13 N3 1.365(19) . ?
C13 C14 1.43(2) . ?
C14 C19 1.41(2) . ?
C14 C15 1.42(2) . ?
C15 C16 1.33(2) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 N3 1.29(2) . ?
C17 C18 1.41(2) . ?
C17 C20 1.43(2) . ?
C18 C19 1.39(2) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 N4 1.26(2) . ?
C20 H20 0.9300 . ?
C21 O23 1.37(2) . ?
C21 C22 1.38(2) . ?
C21 C26 1.38(2) . ?
C22 C23 1.40(2) . ?
C22 H22 0.9300 . ?
C23 C24 1.34(2) . ?
C23 H23 0.9300 . ?
C24 C25 1.39(2) . ?
C24 H24 0.9300 . ?
C25 C29 1.38(2) . ?
C25 C26 1.42(2) . ?
C26 N7 1.365(19) . ?
C27 N7 1.304(18) . ?
C27 C30 1.42(2) . ?
C27 C28 1.43(2) . ?
C28 C29 1.35(2) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 N8 1.282(17) . ?
C30 H30 0.9300 . ?
C31 N6 1.28(2) . ?
C31 C32 1.45(2) . ?
C31 H31 0.9300 . ?
C32 N5 1.31(2) . ?
C32 C33 1.41(2) . ?
C33 C34 1.31(2) . ?
C33 H33 0.9300 . ?
C34 C36 1.33(2) . ?
C34 H34 0.9300 . ?
C35 N5 1.35(2) . ?
C35 C40 1.43(2) . ?
C35 C36 1.45(2) . ?
C36 C37 1.45(3) . ?
C37 C38 1.31(2) . ?
C37 H37 0.9300 . ?
C38 C39 1.47(2) . ?
C38 H38 0.9300 . ?
C39 C40 1.34(2) . ?
C39 H39 0.9300 . ?
C40 O16 1.376(18) . ?
C41 C42 1.33(2) . ?
C41 O20 1.36(2) . ?
C41 C46 1.42(2) . ?
C42 C43 1.42(2) . ?
C42 H42 0.9300 . ?
C43 C44 1.33(2) . ?
C43 H43 0.9300 . ?
C44 C45 1.42(3) . ?
C44 H44 0.9300 . ?
C45 C46 1.39(2) . ?
C45 C47 1.39(2) . ?
C46 N9 1.37(2) . ?
C47 C48 1.36(2) . ?
C47 H47 0.9300 . ?
C48 C49 1.40(2) . ?
C48 H48 0.9300 . ?
C49 N9 1.290(18) . ?
C49 C50 1.45(2) . ?
C50 N10 1.29(2) . ?
C50 H50 0.9300 . ?
C54 O21 1.37(2) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
Gd1 O14 2.295(15) . ?
Gd1 O12 2.369(11) 3_677 ?
Gd1 O22 2.387(11) 3_677 ?
Gd1 O15 2.395(12) . ?
Gd1 O1 2.401(9) . ?
Gd1 O2 2.434(11) . ?
Gd1 N2 2.497(17) . ?
Gd1 N1 2.601(18) . ?
N1 O13 1.396(19) . ?
N3 Ni3 1.973(13) 3_677 ?
N4 O18 1.349(15) . ?
N4 Ni3 2.055(15) 3_677 ?
N5 Ni1 1.992(13) . ?
N6 O15 1.333(16) . ?
N6 Ni1 2.032(16) . ?
N7 Ni2 1.938(13) . ?
N8 O19 1.402(15) . ?
N8 Ni2 2.056(13) . ?
N9 Ni4 1.977(14) . ?
N10 O12 1.333(16) . ?
N10 Ni4 2.065(14) . ?
N11 O5 1.228(9) . ?
N11 O3 1.242(9) . ?
N11 O4 1.277(9) . ?
Ni1 O23 2.021(10) . ?
Ni1 O17 2.044(10) . ?
Ni1 O22 2.071(10) 3_677 ?
Ni1 O16 2.370(10) . ?
Ni2 O18 2.018(10) 3_677 ?
Ni2 O19 2.046(10) 3_677 ?
Ni2 O16 2.065(9) . ?
Ni2 O23 2.259(11) . ?
Ni3 O20 1.961(10) . ?
Ni3 N3 1.973(13) 3_677 ?
Ni3 O16 1.981(10) 3_677 ?
Ni3 N4 2.055(15) 3_677 ?
Ni3 O19 2.107(10) . ?
Ni4 O22 2.048(11) . ?
Ni4 O21 2.058(12) . ?
Ni4 O17 2.083(10) 3_677 ?
Ni4 O20 2.202(12) . ?
O1 H1A 0.8754 . ?
O1 H1B 0.8756 . ?
O2 H2A 0.8578 . ?
O2 H2B 0.8576 . ?
O12 Gd1 2.369(11) 3_677 ?
O16 Ni3 1.981(10) 3_677 ?
O17 Ni4 2.083(10) 3_677 ?
O18 Ni2 2.017(10) 3_677 ?
O19 Ni2 2.046(10) 3_677 ?
O22 Ni1 2.071(10) 3_677 ?
O22 Gd1 2.387(11) 3_677 ?

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
N1 C1 C2 120(2) . . ?
N1 C1 H1 119.9 . . ?
C2 C1 H1 119.9 . . ?
N2 C2 C3 120(3) . . ?
N2 C2 C1 114(2) . . ?
C3 C2 C1 126(3) . . ?
C4 C3 C2 119(3) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C3 C4 C5 125(3) . . ?
C3 C4 H4 117.6 . . ?
C5 C4 H4 117.6 . . ?
C6 C5 C7 121(3) . . ?
C6 C5 C4 113(3) . . ?
C7 C5 C4 126(3) . . ?
N2 C6 C5 121(3) . . ?
N2 C6 C10 120(2) . . ?
C5 C6 C10 118(3) . . ?
C8 C7 C5 119(3) . . ?
C8 C7 H7 120.3 . . ?
C5 C7 H7 120.3 . . ?
C9 C8 C7 122(3) . . ?
C9 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
C8 C9 C10 119(3) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
O14 C10 C9 124(3) . . ?
O14 C10 C6 115(2) . . ?
C9 C10 C6 121(2) . . ?
C12 C11 C16 118.9(18) . . ?
C12 C11 H11 120.5 . . ?
C16 C11 H11 120.5 . . ?
O17 C12 C11 122.5(17) . . ?
O17 C12 C13 117.6(14) . . ?
C11 C12 C13 119.9(16) . . ?
N3 C13 C12 118.3(15) . . ?
N3 C13 C14 120.6(17) . . ?
C12 C13 C14 121.2(16) . . ?
C19 C14 C15 125.0(17) . . ?
C19 C14 C13 117.8(16) . . ?
C15 C14 C13 117.2(19) . . ?
C16 C15 C14 121.8(18) . . ?
C16 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C15 C16 C11 120.9(17) . . ?
C15 C16 H16 119.6 . . ?
C11 C16 H16 119.6 . . ?
N3 C17 C18 119.9(16) . . ?
N3 C17 C20 115.9(16) . . ?
C18 C17 C20 124.2(19) . . ?
C19 C18 C17 121.7(18) . . ?
C19 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?
C18 C19 C14 117.8(17) . . ?
C18 C19 H19 121.1 . . ?
C14 C19 H19 121.1 . . ?
N4 C20 C17 116.4(18) . . ?
N4 C20 H20 121.8 . . ?
C17 C20 H20 121.8 . . ?
O23 C21 C22 122.4(16) . . ?
O23 C21 C26 120.9(18) . . ?
C22 C21 C26 116.6(18) . . ?
C21 C22 C23 121.1(18) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 H22 119.5 . . ?
C24 C23 C22 120.5(19) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C23 C24 C25 122.1(17) . . ?
C23 C24 H24 119.0 . . ?
C25 C24 H24 119.0 . . ?
C29 C25 C24 126.1(17) . . ?
C29 C25 C26 117.6(17) . . ?
C24 C25 C26 116.3(15) . . ?
N7 C26 C21 114.1(16) . . ?
N7 C26 C25 122.6(15) . . ?
C21 C26 C25 123.3(17) . . ?
N7 C27 C30 113.1(15) . . ?
N7 C27 C28 118.8(16) . . ?
C30 C27 C28 128.1(16) . . ?
C29 C28 C27 123.1(17) . . ?
C29 C28 H28 118.5 . . ?
C27 C28 H28 118.5 . . ?
C28 C29 C25 118.1(18) . . ?
C28 C29 H29 120.9 . . ?
C25 C29 H29 120.9 . . ?
N8 C30 C27 115.5(15) . . ?
N8 C30 H30 122.3 . . ?
C27 C30 H30 122.3 . . ?
N6 C31 C32 118.1(18) . . ?
N6 C31 H31 120.9 . . ?
C32 C31 H31 120.9 . . ?
N5 C32 C33 121.4(19) . . ?
N5 C32 C31 111.1(16) . . ?
C33 C32 C31 127.4(19) . . ?
C34 C33 C32 118.7(19) . . ?
C34 C33 H33 120.6 . . ?
C32 C33 H33 120.6 . . ?
C33 C34 C36 123.7(19) . . ?
C33 C34 H34 118.1 . . ?
C36 C34 H34 118.1 . . ?
N5 C35 C40 118.1(17) . . ?
N5 C35 C36 120.4(19) . . ?
C40 C35 C36 121.4(19) . . ?
C34 C36 C35 116(2) . . ?
C34 C36 C37 128.3(17) . . ?
C35 C36 C37 115.3(19) . . ?
C38 C37 C36 120.8(18) . . ?
C38 C37 H37 119.6 . . ?
C36 C37 H37 119.6 . . ?
C37 C38 C39 124.4(19) . . ?
C37 C38 H38 117.8 . . ?
C39 C38 H38 117.8 . . ?
C40 C39 C38 116.8(18) . . ?
C40 C39 H39 121.6 . . ?
C38 C39 H39 121.6 . . ?
C39 C40 O16 123.9(16) . . ?
C39 C40 C35 121.0(17) . . ?
O16 C40 C35 115.0(16) . . ?
C42 C41 O20 127.0(14) . . ?
C42 C41 C46 116.3(19) . . ?
O20 C41 C46 116.6(17) . . ?
C41 C42 C43 119.3(16) . . ?
C41 C42 H42 120.3 . . ?
C43 C42 H42 120.3 . . ?
C44 C43 C42 125.5(19) . . ?
C44 C43 H43 117.3 . . ?
C42 C43 H43 117.3 . . ?
C43 C44 C45 116.7(18) . . ?
C43 C44 H44 121.6 . . ?
C45 C44 H44 121.6 . . ?
C46 C45 C47 116.7(19) . . ?
C46 C45 C44 117.4(17) . . ?
C47 C45 C44 126.0(17) . . ?
N9 C46 C45 119.9(16) . . ?
N9 C46 C41 115.4(17) . . ?
C45 C46 C41 125(2) . . ?
C48 C47 C45 123.4(18) . . ?
C48 C47 H47 118.3 . . ?
C45 C47 H47 118.3 . . ?
C47 C48 C49 115.7(16) . . ?
C47 C48 H48 122.1 . . ?
C49 C48 H48 122.1 . . ?
N9 C49 C48 123.1(17) . . ?
N9 C49 C50 111.8(16) . . ?
C48 C49 C50 125.1(15) . . ?
N10 C50 C49 118.0(15) . . ?
N10 C50 H50 121.0 . . ?
C49 C50 H50 121.0 . . ?
O21 C54 H54A 109.5 . . ?
O21 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
O21 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
O14 Gd1 O12 83.1(4) . 3_677 ?
O14 Gd1 O22 83.3(4) . 3_677 ?
O12 Gd1 O22 83.3(4) 3_677 3_677 ?
O14 Gd1 O15 162.8(5) . . ?
O12 Gd1 O15 82.0(4) 3_677 . ?
O22 Gd1 O15 86.6(4) 3_677 . ?
O14 Gd1 O1 97.2(4) . . ?
O12 Gd1 O1 152.7(4) 3_677 . ?
O22 Gd1 O1 69.7(4) 3_677 . ?
O15 Gd1 O1 92.1(4) . . ?
O14 Gd1 O2 100.6(5) . . ?
O12 Gd1 O2 68.1(4) 3_677 . ?
O22 Gd1 O2 150.3(4) 3_677 . ?
O15 Gd1 O2 81.7(4) . . ?
O1 Gd1 O2 137.6(4) . . ?
O14 Gd1 N2 67.3(6) . . ?
O12 Gd1 N2 128.7(5) 3_677 . ?
O22 Gd1 N2 130.1(5) 3_677 . ?
O15 Gd1 N2 129.3(6) . . ?
O1 Gd1 N2 74.9(5) . . ?
O2 Gd1 N2 77.1(4) . . ?
O14 Gd1 N1 128.7(6) . . ?
O12 Gd1 N1 129.9(5) 3_677 . ?
O22 Gd1 N1 131.2(4) 3_677 . ?
O15 Gd1 N1 68.1(5) . . ?
O1 Gd1 N1 70.3(5) . . ?
O2 Gd1 N1 68.4(5) . . ?
N2 Gd1 N1 61.4(7) . . ?
C1 N1 O13 118(2) . . ?
C1 N1 Gd1 120.1(17) . . ?
O13 N1 Gd1 121.9(12) . . ?
C2 N2 C6 122(2) . . ?
C2 N2 Gd1 123.9(16) . . ?
C6 N2 Gd1 113.6(17) . . ?
C17 N3 C13 122.2(15) . . ?
C17 N3 Ni3 115.3(11) . 3_677 ?
C13 N3 Ni3 122.3(13) . 3_677 ?
C20 N4 O18 116.5(15) . . ?
C20 N4 Ni3 113.5(12) . 3_677 ?
O18 N4 Ni3 130.0(10) . 3_677 ?
C32 N5 C35 119.2(17) . . ?
C32 N5 Ni1 118.5(13) . . ?
C35 N5 Ni1 122.2(12) . . ?
C31 N6 O15 117.8(17) . . ?
C31 N6 Ni1 114.5(14) . . ?
O15 N6 Ni1 127.6(11) . . ?
C27 N7 C26 119.7(15) . . ?
C27 N7 Ni2 119.5(12) . . ?
C26 N7 Ni2 120.8(11) . . ?
C30 N8 O19 115.8(12) . . ?
C30 N8 Ni2 114.6(11) . . ?
O19 N8 Ni2 128.3(9) . . ?
C49 N9 C46 121.2(15) . . ?
C49 N9 Ni4 119.5(13) . . ?
C46 N9 Ni4 119.3(10) . . ?
C50 N10 O12 119.6(14) . . ?
C50 N10 Ni4 112.7(12) . . ?
O12 N10 Ni4 127.4(10) . . ?
O5 N11 O3 123.6(14) . . ?
O5 N11 O4 112.4(14) . . ?
O3 N11 O4 118.0(13) . . ?
N5 Ni1 O23 99.5(4) . . ?
N5 Ni1 N6 77.6(6) . . ?
O23 Ni1 N6 99.6(5) . . ?
N5 Ni1 O17 96.3(4) . . ?
O23 Ni1 O17 152.9(4) . . ?
N6 Ni1 O17 105.3(4) . . ?
N5 Ni1 O22 170.9(4) . 3_677 ?
O23 Ni1 O22 88.6(4) . 3_677 ?
N6 Ni1 O22 97.1(5) . 3_677 ?
O17 Ni1 O22 77.8(4) . 3_677 ?
N5 Ni1 O16 74.4(5) . . ?
O23 Ni1 O16 80.4(4) . . ?
N6 Ni1 O16 151.6(5) . . ?
O17 Ni1 O16 82.9(4) . . ?
O22 Ni1 O16 111.3(4) 3_677 . ?
N7 Ni2 O18 99.0(5) . 3_677 ?
N7 Ni2 O19 168.3(4) . 3_677 ?
O18 Ni2 O19 90.9(4) 3_677 3_677 ?
N7 Ni2 N8 77.0(6) . . ?
O18 Ni2 N8 96.7(4) 3_677 . ?
O19 Ni2 N8 108.2(5) 3_677 . ?
N7 Ni2 O16 92.8(4) . . ?
O18 Ni2 O16 162.2(4) 3_677 . ?
O19 Ni2 O16 76.2(4) 3_677 . ?
N8 Ni2 O16 99.0(4) . . ?
N7 Ni2 O23 77.6(5) . . ?
O18 Ni2 O23 87.3(4) 3_677 . ?
O19 Ni2 O23 96.8(4) 3_677 . ?
N8 Ni2 O23 154.6(5) . . ?
O16 Ni2 O23 82.2(4) . . ?
O20 Ni3 N3 96.3(5) . 3_677 ?
O20 Ni3 O16 152.3(5) . 3_677 ?
N3 Ni3 O16 98.7(5) 3_677 3_677 ?
O20 Ni3 N4 104.6(5) . 3_677 ?
N3 Ni3 N4 78.9(6) 3_677 3_677 ?
O16 Ni3 N4 101.0(5) 3_677 3_677 ?
O20 Ni3 O19 86.3(4) . . ?
N3 Ni3 O19 173.6(6) 3_677 . ?
O16 Ni3 O19 76.6(4) 3_677 . ?
N4 Ni3 O19 106.1(5) 3_677 . ?
N9 Ni4 O22 169.5(5) . . ?
N9 Ni4 O21 98.1(5) . . ?
O22 Ni4 O21 88.1(5) . . ?
N9 Ni4 N10 77.9(6) . . ?
O22 Ni4 N10 93.3(5) . . ?
O21 Ni4 N10 94.1(5) . . ?
N9 Ni4 O17 98.1(5) . 3_677 ?
O22 Ni4 O17 77.4(4) . 3_677 ?
O21 Ni4 O17 161.5(4) . 3_677 ?
N10 Ni4 O17 98.1(5) . 3_677 ?
N9 Ni4 O20 77.4(5) . . ?
O22 Ni4 O20 111.2(4) . . ?
O21 Ni4 O20 91.0(5) . . ?
N10 Ni4 O20 155.2(5) . . ?
O17 Ni4 O20 83.8(4) 3_677 . ?
Gd1 O1 H1A 110.5 . . ?
Gd1 O1 H1B 110.7 . . ?
H1A O1 H1B 108.2 . . ?
Gd1 O2 H2A 109.7 . . ?
Gd1 O2 H2B 109.3 . . ?
H2A O2 H2B 109.1 . . ?
N10 O12 Gd1 117.7(9) . 3_677 ?
C10 O14 Gd1 123.5(16) . . ?
N6 O15 Gd1 115.9(10) . . ?
C40 O16 Ni3 121.6(9) . 3_677 ?
C40 O16 Ni2 127.5(8) . . ?
Ni3 O16 Ni2 103.7(4) 3_677 . ?
C40 O16 Ni1 110.0(9) . . ?
Ni3 O16 Ni1 92.4(4) 3_677 . ?
Ni2 O16 Ni1 91.9(4) . . ?
C12 O17 Ni1 132.3(10) . . ?
C12 O17 Ni4 122.4(9) . 3_677 ?
Ni1 O17 Ni4 102.2(5) . 3_677 ?
N4 O18 Ni2 123.9(10) . 3_677 ?
N8 O19 Ni2 117.4(8) . 3_677 ?
N8 O19 Ni3 99.9(8) . . ?
Ni2 O19 Ni3 100.0(4) 3_677 . ?
C41 O20 Ni3 121.7(10) . . ?
C41 O20 Ni4 111.2(9) . . ?
Ni3 O20 Ni4 97.3(5) . . ?
C54 O21 Ni4 122.9(12) . . ?
Ni4 O22 Ni1 102.5(5) . 3_677 ?
Ni4 O22 Gd1 113.8(4) . 3_677 ?
Ni1 O22 Gd1 110.4(5) 3_677 3_677 ?
C21 O23 Ni1 119.5(9) . . ?
C21 O23 Ni2 106.4(10) . . ?
Ni1 O23 Ni2 96.4(5) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.431
_refine_diff_density_min         -1.298
_refine_diff_density_rms         0.161
# start Validation Reply Form
_vrf_PLAT026_complex-2           
;
PROBLEM: Ratio Observed / Unique Reflections too Low ....         39 %     
RESPONSE: Crystals were  poorly diffracting with many reflections missed.
;
_vrf_PLAT306_complex-2           
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O6 Check 
RESPONSE: Due to disorder of  water molecules their Hydrogen could not be located with out pointing in the wrong direction.
;
_vrf_PLAT342_complex-2           
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0318 Ang.  
RESPONSE: Disordered  carbon atoms in the structure leads to low bond precision and due to poor diffraction quality of the crystal it was not possible to model this disorder,
;
_database_code_depnum_ccdc_archive 'CCDC 986610'
#######################################################################
#
#                 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_complex-3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C102 H74 Ho2 N20 Ni8 O28, 2(Cl O4), 2(C H3 O), 8(O), 4(H2 O)'
_chemical_formula_sum            'C104 H88 Cl2 Ho2 N20 Ni8 O50'
_chemical_formula_weight         3288.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_hall  '-P 2ybc'

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

_cell_length_a                   18.181(5)
_cell_length_b                   21.581(5)
_cell_length_c                   17.132(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.918(5)
_cell_angle_gamma                90.00
_cell_volume                     6096(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2001
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      20.09

_exptl_crystal_description       Block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3288
_exptl_absorpt_coefficient_mu    2.631
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.486
_exptl_absorpt_correction_T_max  0.602
_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            31486
_diffrn_reflns_av_R_equivalents  0.1471
_diffrn_reflns_av_unetI/netI     0.1879
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.12
_diffrn_reflns_theta_max         25.03
_reflns_number_total             10733
_reflns_number_gt                4627
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'


_refine_special_details          
;
Due to the weak high-angle diffractions internal R-value is high.
Actual molecular formula is C104 H112 Cl2 Ho2 N20 Ni8 O50 which differ from calculated molecular formula because hydrogen of eight water, two -OH and two oxime-OH and two Me-OH could not be modeled.
 
 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)+(0.1018P)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         10733
_refine_ls_number_parameters     806
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.2002
_refine_ls_R_factor_gt           0.0852
_refine_ls_wR_factor_ref         0.2362
_refine_ls_wR_factor_gt          0.1804
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_restrained_S_all      0.972
_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
C1 C 0.8745(13) 0.1968(10) 0.5736(15) 0.090(3) Uani 1 1 d . . .
C2 C 0.8483(12) 0.2563(10) 0.5518(14) 0.090(3) Uani 1 1 d . . .
H2 H 0.8076 0.2644 0.4975 0.108 Uiso 1 1 calc R . .
C3 C 0.8817(12) 0.3061(10) 0.6102(14) 0.090(3) Uani 1 1 d . . .
H3 H 0.8653 0.3466 0.5932 0.108 Uiso 1 1 calc R . .
C4 C 0.9390(12) 0.2937(10) 0.6929(14) 0.090(3) Uani 1 1 d . . .
H4 H 0.9577 0.3261 0.7322 0.108 Uiso 1 1 calc R . .
C5 C 0.9697(13) 0.2341(10) 0.7193(16) 0.090(3) Uani 1 1 d . . .
C6 C 0.9365(13) 0.1853(11) 0.6588(15) 0.090(3) Uani 1 1 d . . .
C7 C 1.0296(14) 0.2160(15) 0.7990(14) 0.109(9) Uani 1 1 d . . .
H7 H 1.0526 0.2458 0.8418 0.131 Uiso 1 1 calc R . .
C8 C 1.0549(14) 0.1575(13) 0.8158(16) 0.101(8) Uani 1 1 d . . .
H8 H 1.0964 0.1473 0.8687 0.121 Uiso 1 1 calc R . .
C9 C 1.0193(12) 0.1115(12) 0.7541(13) 0.079(6) Uani 1 1 d . . .
C10 C 1.0402(11) 0.0453(10) 0.7733(11) 0.071(5) Uani 1 1 d . . .
H10A H 1.0772 0.0306 0.8264 0.085 Uiso 1 1 calc R . .
C11 C 0.3268(9) 0.0854(6) 0.7043(9) 0.039(4) Uani 1 1 d . . .
C12 C 0.2631(9) 0.1020(6) 0.7262(9) 0.044(4) Uani 1 1 d . . .
H12 H 0.2098 0.0909 0.6913 0.053 Uiso 1 1 calc R . .
C13 C 0.2820(11) 0.1358(7) 0.8021(10) 0.052(4) Uani 1 1 d . . .
H13 H 0.2397 0.1454 0.8171 0.063 Uiso 1 1 calc R . .
C14 C 0.3559(11) 0.1552(7) 0.8542(10) 0.056(5) Uani 1 1 d . . .
H14 H 0.3645 0.1773 0.9039 0.067 Uiso 1 1 calc R . .
C15 C 0.4231(10) 0.1411(6) 0.8323(9) 0.044(4) Uani 1 1 d . . .
C16 C 0.4046(9) 0.1059(6) 0.7565(9) 0.038(4) Uani 1 1 d . . .
C17 C 0.5035(11) 0.1579(7) 0.8796(9) 0.053(4) Uani 1 1 d . . .
H17 H 0.5172 0.1818 0.9290 0.064 Uiso 1 1 calc R . .
C18 C 0.5618(9) 0.1406(7) 0.8557(9) 0.047(4) Uani 1 1 d . . .
H18 H 0.6154 0.1525 0.8873 0.056 Uiso 1 1 calc R . .
C19 C 0.5394(9) 0.1035(6) 0.7807(9) 0.038(3) Uani 1 1 d . . .
C20 C 0.5973(10) 0.0788(6) 0.7504(9) 0.049(4) Uani 1 1 d . . .
H20 H 0.6522 0.0884 0.7778 0.058 Uiso 1 1 calc R . .
C21 C 0.5813(10) -0.1540(6) 0.4435(8) 0.042(4) Uani 1 1 d . . .
C22 C 0.5092(9) -0.1821(6) 0.4189(8) 0.037(3) Uani 1 1 d . . .
H22 H 0.4635 -0.1591 0.4113 0.044 Uiso 1 1 calc R . .
C23 C 0.5028(11) -0.2456(7) 0.4046(9) 0.050(4) Uani 1 1 d . . .
H23 H 0.4519 -0.2637 0.3871 0.060 Uiso 1 1 calc R . .
C24 C 0.5669(12) -0.2833(8) 0.4146(9) 0.058(5) Uani 1 1 d . . .
H24 H 0.5600 -0.3256 0.4038 0.069 Uiso 1 1 calc R . .
C25 C 0.6448(12) -0.2551(7) 0.4424(9) 0.049(4) Uani 1 1 d . . .
C26 C 0.6507(10) -0.1906(6) 0.4580(8) 0.041(4) Uani 1 1 d . . .
C27 C 0.7166(14) -0.2856(8) 0.4594(10) 0.068(5) Uani 1 1 d . . .
H27 H 0.7159 -0.3285 0.4529 0.081 Uiso 1 1 calc R . .
C28 C 0.7874(11) -0.2553(8) 0.4851(9) 0.055(5) Uani 1 1 d . . .
H28 H 0.8349 -0.2766 0.4946 0.066 Uiso 1 1 calc R . .
C29 C 0.7886(9) -0.1922(7) 0.4971(8) 0.041(4) Uani 1 1 d . . .
C30 C 0.8618(11) -0.1515(8) 0.5243(9) 0.059(5) Uani 1 1 d . . .
H30 H 0.9132 -0.1673 0.5368 0.071 Uiso 1 1 calc R . .
C31 C 0.5349(9) 0.0516(6) 0.2211(10) 0.044(4) Uani 1 1 d . . .
C32 C 0.4551(8) 0.0518(6) 0.1652(8) 0.040(4) Uani 1 1 d . . .
H32 H 0.4162 0.0485 0.1870 0.048 Uiso 1 1 calc R . .
C33 C 0.4297(10) 0.0566(6) 0.0763(10) 0.051(4) Uani 1 1 d . . .
H33 H 0.3744 0.0562 0.0408 0.062 Uiso 1 1 calc R . .
C34 C 0.4836(10) 0.0621(6) 0.0393(9) 0.049(4) Uani 1 1 d . . .
H34 H 0.4650 0.0655 -0.0200 0.058 Uiso 1 1 calc R . .
C35 C 0.5684(10) 0.0623(6) 0.0937(10) 0.047(4) Uani 1 1 d . . .
C36 C 0.5899(9) 0.0571(6) 0.1814(10) 0.043(4) Uani 1 1 d . . .
C37 C 0.7279(9) 0.0585(6) 0.2111(10) 0.043(4) Uani 1 1 d . . .
C38 C 0.8078(9) 0.0553(7) 0.2802(10) 0.053(4) Uani 1 1 d . . .
H38 H 0.8544 0.0582 0.2706 0.064 Uiso 1 1 calc R . .
C39 C 0.7094(10) 0.0627(7) 0.1235(10) 0.054(4) Uani 1 1 d . . .
H39 H 0.7506 0.0641 0.1049 0.064 Uiso 1 1 calc R . .
C40 C 0.6320(11) 0.0649(6) 0.0669(11) 0.054(4) Uani 1 1 d . . .
H40 H 0.6195 0.0682 0.0085 0.065 Uiso 1 1 calc R . .
C41 C 0.7540(9) -0.1077(6) 0.6665(8) 0.037(3) Uani 1 1 d . . .
C42 C 0.6910(9) -0.1391(7) 0.6775(9) 0.044(4) Uani 1 1 d . . .
C43 C 0.7070(10) -0.1910(7) 0.7315(9) 0.043(4) Uani 1 1 d . . .
C44 C 0.7873(10) -0.2093(7) 0.7768(9) 0.050(4) Uani 1 1 d . . .
H44 H 0.7991 -0.2439 0.8123 0.060 Uiso 1 1 calc R . .
C45 C 0.8487(12) -0.1774(9) 0.7700(11) 0.071(5) Uani 1 1 d . . .
H45 H 0.9022 -0.1890 0.8030 0.085 Uiso 1 1 calc R . .
C46 C 0.8318(9) -0.1272(8) 0.7135(9) 0.055(4) Uani 1 1 d . . .
H46 H 0.8743 -0.1068 0.7077 0.066 Uiso 1 1 calc R . .
C47 C 0.5221(10) 0.1129(7) 0.4086(9) 0.049(4) Uani 1 1 d . . .
H47 H 0.5709 0.1277 0.4108 0.058 Uiso 1 1 calc R . .
C48 C 0.4461(9) 0.1444(6) 0.3613(9) 0.037(3) Uani 1 1 d . . .
C49 C 0.4366(10) 0.1964(6) 0.3087(9) 0.047(4) Uani 1 1 d . . .
H49 H 0.4812 0.2154 0.3056 0.056 Uiso 1 1 calc R . .
C50 C 0.3599(11) 0.2180(7) 0.2622(9) 0.051(4) Uani 1 1 d . . .
H50 H 0.3521 0.2516 0.2255 0.062 Uiso 1 1 calc R . .
C51 C 0.6744(11) 0.1877(8) 0.3288(10) 0.071(3) Uani 1 1 d U . .
H51A H 0.6238 0.1756 0.2831 0.107 Uiso 1 1 calc R . .
H51B H 0.7137 0.1949 0.3060 0.107 Uiso 1 1 calc R . .
H51C H 0.6669 0.2251 0.3551 0.107 Uiso 1 1 calc R . .
C52 C 0.655(4) 0.244(3) 0.541(4) 0.40(5) Uani 1 1 d . . .
H52A H 0.6726 0.2113 0.5152 0.601 Uiso 1 1 calc R . .
H52B H 0.6675 0.2834 0.5228 0.601 Uiso 1 1 calc R . .
H52C H 0.5977 0.2412 0.5237 0.601 Uiso 1 1 calc R . .
O25 O 0.0108(15) 0.3937(18) 0.513(2) 0.323(16) Uani 1 1 d GU . .
O26 O 0.8134(18) 0.207(2) 0.807(2) 0.43(2) Uani 1 1 d GU . .
Cl1 Cl 0.7993(6) 0.9908(5) 0.9731(6) 0.156(3) Uani 1 1 d D . .
Ho1 Ho 0.89108(5) 0.04972(4) 0.56455(5) 0.0542(3) Uani 1 1 d . . .
N1 N 0.6697(8) 0.0557(5) 0.2369(7) 0.048(3) Uani 1 1 d . . .
N2 N 0.8110(7) 0.0478(5) 0.3572(8) 0.043(3) Uani 1 1 d . . .
N3 N 0.9606(9) 0.1268(8) 0.6794(9) 0.071(4) Uani 1 1 d . . .
N4 N 1.0013(9) 0.0108(8) 0.7085(9) 0.065(4) Uani 1 1 d . . .
N5 N 0.6157(8) -0.1173(5) 0.6342(7) 0.041(3) Uani 1 1 d . . .
N6 N 0.7218(8) -0.1603(6) 0.4806(7) 0.046(3) Uani 1 1 d . . .
N7 N 0.8494(8) -0.0938(6) 0.5291(8) 0.048(3) Uani 1 1 d . . .
N8 N 0.4649(7) 0.0873(5) 0.7341(6) 0.034(3) Uani 1 1 d . . .
N9 N 0.5689(7) 0.0429(5) 0.6840(7) 0.037(3) Uani 1 1 d . . .
N10 N 0.5179(7) 0.0629(5) 0.4475(7) 0.040(3) Uani 1 1 d . . .
Ni1 Ni 0.59657(10) -0.04228(8) 0.56279(11) 0.0347(4) Uani 1 1 d . . .
Ni2 Ni 0.55403(11) -0.03005(8) 0.36299(11) 0.0371(5) Uani 1 1 d . . .
Ni3 Ni 0.70052(11) 0.04552(8) 0.36232(11) 0.0420(5) Uani 1 1 d . . .
Ni4 Ni 0.73204(11) -0.06822(8) 0.49291(11) 0.0403(5) Uani 1 1 d . . .
O1 O 0.7325(5) -0.0585(4) 0.6111(6) 0.043(2) Uani 1 1 d . . .
O2 O 0.8673(11) 1.0230(10) 1.0396(13) 0.242(14) Uani 1 1 d D . .
O4 O 0.796(3) 0.9704(14) 0.8912(14) 0.43(3) Uani 1 1 d DU . .
O5 O 0.7955(13) 0.9379(9) 1.0218(13) 0.210(12) Uani 1 1 d D . .
O6 O 0.3142(5) 0.0499(4) 0.6359(5) 0.041(2) Uani 1 1 d . . .
O7 O 0.6232(6) 0.0223(4) 0.6559(5) 0.040(2) Uani 1 1 d . . .
O9 O 0.6962(8) 0.1173(7) 0.6065(8) 0.118(5) Uani 1 1 d GU . .
H9A H 0.7204 0.1365 0.6539 0.177 Uiso 1 1 d G . .
H9B H 0.6566 0.0970 0.6076 0.177 Uiso 1 1 d G . .
O8 O 0.8921(9) 0.0580(11) 0.8331(8) 0.233(12) Uani 1 1 d GU . .
O10 O 1.0183(7) -0.0515(6) 0.7226(7) 0.075(3) Uani 1 1 d . . .
O11 O 0.8448(7) 0.1476(5) 0.5223(7) 0.074(4) Uani 1 1 d . . .
O12 O 0.8348(6) 0.0366(5) 0.6654(6) 0.060(3) Uani 1 1 d . . .
H12A H 0.8068 0.0016 0.6558 0.090 Uiso 1 1 d R . .
H12B H 0.8732 0.0351 0.7190 0.090 Uiso 1 1 d R . .
O13 O 1.0229(6) 0.0570(5) 0.5648(7) 0.069(3) Uani 1 1 d . . .
H13A H 1.0544 0.0287 0.5983 0.104 Uiso 1 1 d R . .
H13B H 1.0196 0.0514 0.5133 0.104 Uiso 1 1 d R . .
O14 O 0.5935(5) -0.0926(4) 0.4572(5) 0.034(2) Uani 1 1 d . . .
O15 O 0.9143(6) -0.0555(5) 0.5598(6) 0.053(3) Uani 1 1 d . . .
O17 O 0.8845(6) 0.0455(5) 0.4246(6) 0.060(3) Uani 1 1 d . . .
O18 O 0.5846(6) 0.0246(4) 0.4741(5) 0.040(2) Uani 1 1 d . . .
O19 O 0.7032(7) 0.1386(5) 0.3931(7) 0.071(3) Uani 1 1 d . . .
O20 O 0.5654(5) 0.0452(4) 0.3045(6) 0.039(2) Uani 1 1 d . . .
O21 O 0.7508(6) 0.0261(4) 0.4899(6) 0.043(2) Uani 1 1 d . . .
O22 O 0.9334(8) 0.1814(8) 0.4011(10) 0.140(6) Uani 1 1 d GU . .
H22A H 0.9232 0.1488 0.4228 0.210 Uiso 1 1 d G . .
H22B H 0.8924 0.1907 0.3551 0.210 Uiso 1 1 d G . .
O23 O 0.0213(11) 0.2844(15) 0.5093(16) 0.245(12) Uani 1 1 d GU . .
O24 O 0.6987(17) 0.2393(17) 0.638(3) 0.294(18) Uani 1 1 d . . .
O3 O 0.7328(11) 1.0360(10) 0.9402(14) 0.216(10) Uani 1 1 d DU . .


_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
C1 O11 1.34(2) . ?
C1 C2 1.37(3) . ?
C1 C6 1.44(3) . ?
C2 C3 1.42(2) . ?
C3 C4 1.39(3) . ?
C4 C5 1.40(3) . ?
C5 C7 1.40(3) . ?
C5 C6 1.42(3) . ?
C6 N3 1.34(2) . ?
C7 C8 1.33(3) . ?
C8 C9 1.39(3) . ?
C9 N3 1.32(2) . ?
C9 C10 1.48(3) . ?
C10 N4 1.275(19) . ?
C11 O6 1.337(15) . ?
C11 C16 1.390(19) . ?
C11 C12 1.406(18) . ?
C12 C13 1.402(19) . ?
C13 C14 1.33(2) . ?
C14 C15 1.45(2) . ?
C15 C17 1.39(2) . ?
C15 C16 1.418(18) . ?
C16 N8 1.366(17) . ?
C17 C18 1.34(2) . ?
C18 C19 1.420(18) . ?
C19 N8 1.296(16) . ?
C19 C20 1.46(2) . ?
C20 N9 1.291(16) . ?
C21 C22 1.341(18) . ?
C21 O14 1.347(15) . ?
C21 C26 1.419(19) . ?
C22 C23 1.389(18) . ?
C23 C24 1.37(2) . ?
C24 C25 1.43(2) . ?
C25 C27 1.38(2) . ?
C25 C26 1.412(19) . ?
C26 N6 1.350(18) . ?
C27 C28 1.34(2) . ?
C28 C29 1.38(2) . ?
C29 N6 1.319(17) . ?
C29 C30 1.50(2) . ?
C30 N7 1.275(18) . ?
C31 O20 1.305(16) . ?
C31 C32 1.360(18) . ?
C31 C36 1.43(2) . ?
C32 C33 1.397(18) . ?
C33 C34 1.38(2) . ?
C34 C35 1.43(2) . ?
C35 C36 1.390(19) . ?
C35 C40 1.41(2) . ?
C36 N1 1.360(18) . ?
C37 N1 1.309(17) . ?
C37 C39 1.397(19) . ?
C37 C38 1.44(2) . ?
C38 N2 1.306(17) . ?
C39 C40 1.33(2) . ?
C41 C46 1.366(18) . ?
C41 O1 1.368(15) . ?
C41 C42 1.411(19) . ?
C42 N5 1.336(17) . ?
C42 C43 1.404(19) . ?
C43 C44 1.390(19) . ?
C43 C50 1.39(2) 3_656 ?
C44 C45 1.36(2) . ?
C45 C46 1.40(2) . ?
C47 N10 1.287(16) . ?
C47 C48 1.44(2) . ?
C48 N5 1.298(16) 3_656 ?
C48 C49 1.403(18) . ?
C49 C50 1.364(19) . ?
C50 C43 1.39(2) 3_656 ?
C51 O19 1.458(17) . ?
C52 O24 1.52(5) . ?
Cl1 O5 1.432(9) . ?
Cl1 O4 1.450(10) . ?
Cl1 O2 1.457(9) . ?
Cl1 O3 1.470(9) . ?
Ho1 O11 2.276(12) . ?
Ho1 O15 2.316(11) . ?
Ho1 O17 2.351(10) . ?
Ho1 O12 2.367(10) . ?
Ho1 O21 2.378(9) . ?
Ho1 O13 2.399(11) . ?
Ho1 N3 2.477(14) . ?
Ho1 N4 2.576(15) . ?
N1 Ni3 1.991(12) . ?
N2 O17 1.349(14) . ?
N2 Ni3 2.049(12) . ?
N4 O10 1.379(17) . ?
N5 C48 1.298(16) 3_656 ?
N5 Ni1 1.970(11) . ?
N6 Ni4 2.000(12) . ?
N7 O15 1.352(14) . ?
N7 Ni4 2.031(13) . ?
N8 Ni2 1.982(11) 3_656 ?
N9 O7 1.343(13) . ?
N9 Ni2 2.051(11) 3_656 ?
N10 O18 1.377(13) . ?
N10 Ni1 2.062(12) 3_656 ?
Ni1 O7 2.017(8) . ?
Ni1 O18 2.039(9) . ?
Ni1 N10 2.062(12) 3_656 ?
Ni1 O14 2.091(8) . ?
Ni1 O1 2.279(9) . ?
Ni2 O20 1.965(9) . ?
Ni2 N8 1.982(11) 3_656 ?
Ni2 O14 1.992(8) . ?
Ni2 N9 2.051(11) 3_656 ?
Ni2 O18 2.105(9) . ?
Ni3 O21 2.026(9) . ?
Ni3 O19 2.072(11) . ?
Ni3 O6 2.077(9) 3_656 ?
Ni3 O20 2.228(9) . ?
Ni4 O1 2.031(9) . ?
Ni4 O6 2.043(9) 3_656 ?
Ni4 O21 2.068(8) . ?
Ni4 O14 2.387(9) . ?
O6 Ni4 2.043(9) 3_656 ?
O6 Ni3 2.077(9) 3_656 ?

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
O11 C1 C2 125(2) . . ?
O11 C1 C6 117(2) . . ?
C2 C1 C6 118(2) . . ?
C1 C2 C3 122(2) . . ?
C4 C3 C2 119(2) . . ?
C3 C4 C5 122(2) . . ?
C7 C5 C4 128(2) . . ?
C7 C5 C6 115(2) . . ?
C4 C5 C6 117(2) . . ?
N3 C6 C5 121(2) . . ?
N3 C6 C1 117.4(19) . . ?
C5 C6 C1 121(2) . . ?
C8 C7 C5 122(2) . . ?
C7 C8 C9 120(2) . . ?
N3 C9 C8 119(2) . . ?
N3 C9 C10 118.9(17) . . ?
C8 C9 C10 122(2) . . ?
N4 C10 C9 111.9(17) . . ?
O6 C11 C16 119.9(13) . . ?
O6 C11 C12 121.6(14) . . ?
C16 C11 C12 118.5(14) . . ?
C13 C12 C11 118.2(14) . . ?
C14 C13 C12 124.7(15) . . ?
C13 C14 C15 118.9(14) . . ?
C17 C15 C16 117.4(14) . . ?
C17 C15 C14 126.0(14) . . ?
C16 C15 C14 116.6(15) . . ?
N8 C16 C11 116.5(13) . . ?
N8 C16 C15 120.5(14) . . ?
C11 C16 C15 122.9(14) . . ?
C18 C17 C15 121.5(14) . . ?
C17 C18 C19 118.1(14) . . ?
N8 C19 C18 122.4(13) . . ?
N8 C19 C20 114.0(12) . . ?
C18 C19 C20 123.6(13) . . ?
N9 C20 C19 116.9(14) . . ?
C22 C21 O14 124.5(14) . . ?
C22 C21 C26 118.9(13) . . ?
O14 C21 C26 116.6(13) . . ?
C21 C22 C23 120.1(15) . . ?
C24 C23 C22 123.9(16) . . ?
C23 C24 C25 117.5(15) . . ?
C27 C25 C26 116.2(17) . . ?
C27 C25 C24 125.7(16) . . ?
C26 C25 C24 118.0(15) . . ?
N6 C26 C25 121.2(15) . . ?
N6 C26 C21 117.0(13) . . ?
C25 C26 C21 121.6(16) . . ?
C28 C27 C25 121.8(17) . . ?
C27 C28 C29 118.9(16) . . ?
N6 C29 C28 121.9(16) . . ?
N6 C29 C30 112.3(14) . . ?
C28 C29 C30 125.6(15) . . ?
N7 C30 C29 115.7(14) . . ?
O20 C31 C32 127.3(14) . . ?
O20 C31 C36 118.0(13) . . ?
C32 C31 C36 114.7(14) . . ?
C31 C32 C33 122.1(14) . . ?
C34 C33 C32 122.3(15) . . ?
C33 C34 C35 118.9(14) . . ?
C36 C35 C40 117.3(15) . . ?
C36 C35 C34 116.1(14) . . ?
C40 C35 C34 126.6(15) . . ?
N1 C36 C35 119.3(14) . . ?
N1 C36 C31 114.8(13) . . ?
C35 C36 C31 125.9(15) . . ?
N1 C37 C39 120.2(15) . . ?
N1 C37 C38 113.6(14) . . ?
C39 C37 C38 126.2(14) . . ?
N2 C38 C37 115.9(13) . . ?
C40 C39 C37 119.2(15) . . ?
C39 C40 C35 121.4(15) . . ?
C46 C41 O1 124.8(14) . . ?
C46 C41 C42 118.1(13) . . ?
O1 C41 C42 117.1(13) . . ?
N5 C42 C43 121.7(14) . . ?
N5 C42 C41 117.2(13) . . ?
C43 C42 C41 121.1(14) . . ?
C44 C43 C50 125.7(14) . 3_656 ?
C44 C43 C42 118.1(15) . . ?
C50 C43 C42 116.1(14) 3_656 . ?
C45 C44 C43 121.1(15) . . ?
C44 C45 C46 120.2(16) . . ?
C41 C46 C45 121.2(15) . . ?
N10 C47 C48 115.8(14) . . ?
N5 C48 C49 121.5(14) 3_656 . ?
N5 C48 C47 113.7(13) 3_656 . ?
C49 C48 C47 124.5(14) . . ?
C50 C49 C48 117.9(14) . . ?
C49 C50 C43 121.5(14) . 3_656 ?
O5 Cl1 O4 109.3(9) . . ?
O5 Cl1 O2 99.2(14) . . ?
O4 Cl1 O2 125(2) . . ?
O5 Cl1 O3 121.2(15) . . ?
O4 Cl1 O3 98.0(17) . . ?
O2 Cl1 O3 105.8(9) . . ?
O11 Ho1 O15 161.2(3) . . ?
O11 Ho1 O17 81.9(4) . . ?
O15 Ho1 O17 81.8(3) . . ?
O11 Ho1 O12 97.3(4) . . ?
O15 Ho1 O12 92.8(3) . . ?
O17 Ho1 O12 152.6(3) . . ?
O11 Ho1 O21 81.9(3) . . ?
O15 Ho1 O21 86.6(3) . . ?
O17 Ho1 O21 82.0(3) . . ?
O12 Ho1 O21 70.8(3) . . ?
O11 Ho1 O13 100.1(4) . . ?
O15 Ho1 O13 82.4(4) . . ?
O17 Ho1 O13 68.1(4) . . ?
O12 Ho1 O13 138.1(4) . . ?
O21 Ho1 O13 149.2(3) . . ?
O11 Ho1 N3 68.1(5) . . ?
O15 Ho1 N3 130.2(5) . . ?
O17 Ho1 N3 128.7(4) . . ?
O12 Ho1 N3 74.5(4) . . ?
O21 Ho1 N3 130.1(4) . . ?
O13 Ho1 N3 77.3(4) . . ?
O11 Ho1 N4 129.9(5) . . ?
O15 Ho1 N4 68.6(4) . . ?
O17 Ho1 N4 130.4(4) . . ?
O12 Ho1 N4 70.3(4) . . ?
O21 Ho1 N4 132.1(4) . . ?
O13 Ho1 N4 69.3(4) . . ?
N3 Ho1 N4 61.8(6) . . ?
C37 N1 C36 122.7(13) . . ?
C37 N1 Ni3 118.0(11) . . ?
C36 N1 Ni3 119.3(10) . . ?
C38 N2 O17 118.4(12) . . ?
C38 N2 Ni3 114.8(9) . . ?
O17 N2 Ni3 126.7(9) . . ?
C9 N3 C6 122.3(19) . . ?
C9 N3 Ho1 122.6(14) . . ?
C6 N3 Ho1 115.1(13) . . ?
C10 N4 O10 114.5(16) . . ?
C10 N4 Ho1 124.5(14) . . ?
O10 N4 Ho1 120.8(10) . . ?
C48 N5 C42 121.3(13) 3_656 . ?
C48 N5 Ni1 118.4(11) 3_656 . ?
C42 N5 Ni1 120.3(10) . . ?
C29 N6 C26 119.5(13) . . ?
C29 N6 Ni4 117.3(11) . . ?
C26 N6 Ni4 123.1(10) . . ?
C30 N7 O15 118.2(14) . . ?
C30 N7 Ni4 116.0(12) . . ?
O15 N7 Ni4 125.7(9) . . ?
C19 N8 C16 120.1(12) . . ?
C19 N8 Ni2 116.8(9) . 3_656 ?
C16 N8 Ni2 122.9(9) . 3_656 ?
C20 N9 O7 115.7(12) . . ?
C20 N9 Ni2 113.1(11) . 3_656 ?
O7 N9 Ni2 131.2(8) . 3_656 ?
C47 N10 O18 116.0(13) . . ?
C47 N10 Ni1 114.5(11) . 3_656 ?
O18 N10 Ni1 128.0(8) . 3_656 ?
N5 Ni1 O7 99.0(4) . . ?
N5 Ni1 O18 168.4(4) . . ?
O7 Ni1 O18 90.8(3) . . ?
N5 Ni1 N10 77.5(5) . 3_656 ?
O7 Ni1 N10 96.6(4) . 3_656 ?
O18 Ni1 N10 107.6(4) . 3_656 ?
N5 Ni1 O14 92.5(4) . . ?
O7 Ni1 O14 162.4(4) . . ?
O18 Ni1 O14 76.6(3) . . ?
N10 Ni1 O14 99.0(4) 3_656 . ?
N5 Ni1 O1 76.6(4) . . ?
O7 Ni1 O1 87.5(4) . . ?
O18 Ni1 O1 97.9(4) . . ?
N10 Ni1 O1 154.1(4) 3_656 . ?
O14 Ni1 O1 82.2(3) . . ?
O20 Ni2 N8 96.0(4) . 3_656 ?
O20 Ni2 O14 153.4(4) . . ?
N8 Ni2 O14 97.7(4) 3_656 . ?
O20 Ni2 N9 104.1(4) . 3_656 ?
N8 Ni2 N9 79.1(5) 3_656 3_656 ?
O14 Ni2 N9 100.8(4) . 3_656 ?
O20 Ni2 O18 87.4(3) . . ?
N8 Ni2 O18 173.9(4) 3_656 . ?
O14 Ni2 O18 77.3(3) . . ?
N9 Ni2 O18 105.1(4) 3_656 . ?
N1 Ni3 O21 168.8(5) . . ?
N1 Ni3 N2 77.6(5) . . ?
O21 Ni3 N2 92.7(4) . . ?
N1 Ni3 O19 97.6(4) . . ?
O21 Ni3 O19 88.5(4) . . ?
N2 Ni3 O19 93.9(5) . . ?
N1 Ni3 O6 98.4(4) . 3_656 ?
O21 Ni3 O6 77.4(3) . 3_656 ?
N2 Ni3 O6 99.2(4) . 3_656 ?
O19 Ni3 O6 161.1(4) . 3_656 ?
N1 Ni3 O20 76.4(5) . . ?
O21 Ni3 O20 113.0(4) . . ?
N2 Ni3 O20 154.0(4) . . ?
O19 Ni3 O20 91.1(4) . . ?
O6 Ni3 O20 83.1(3) 3_656 . ?
N6 Ni4 N7 78.6(5) . . ?
N6 Ni4 O1 99.7(4) . . ?
N7 Ni4 O1 99.2(4) . . ?
N6 Ni4 O6 95.8(4) . 3_656 ?
N7 Ni4 O6 106.5(4) . 3_656 ?
O1 Ni4 O6 152.1(4) . 3_656 ?
N6 Ni4 O21 170.1(4) . . ?
N7 Ni4 O21 96.4(5) . . ?
O1 Ni4 O21 89.5(4) . . ?
O6 Ni4 O21 77.2(4) 3_656 . ?
N6 Ni4 O14 73.2(4) . . ?
N7 Ni4 O14 151.3(4) . . ?
O1 Ni4 O14 80.8(3) . . ?
O6 Ni4 O14 81.7(3) 3_656 . ?
O21 Ni4 O14 112.2(3) . . ?
C41 O1 Ni4 119.4(8) . . ?
C41 O1 Ni1 108.6(8) . . ?
Ni4 O1 Ni1 96.1(4) . . ?
C11 O6 Ni4 132.6(8) . 3_656 ?
C11 O6 Ni3 122.1(8) . 3_656 ?
Ni4 O6 Ni3 102.2(4) 3_656 3_656 ?
N9 O7 Ni1 123.0(7) . . ?
C1 O11 Ho1 122.3(13) . . ?
C21 O14 Ni2 123.4(7) . . ?
C21 O14 Ni1 127.1(8) . . ?
Ni2 O14 Ni1 102.6(4) . . ?
C21 O14 Ni4 109.9(8) . . ?
Ni2 O14 Ni4 92.2(3) . . ?
Ni1 O14 Ni4 91.3(3) . . ?
N7 O15 Ho1 118.1(8) . . ?
N2 O17 Ho1 118.6(8) . . ?
N10 O18 Ni1 118.3(7) . . ?
N10 O18 Ni2 100.2(6) . . ?
Ni1 O18 Ni2 100.5(4) . . ?
C51 O19 Ni3 123.4(9) . . ?
C31 O20 Ni2 124.0(8) . . ?
C31 O20 Ni3 111.5(8) . . ?
Ni2 O20 Ni3 96.3(4) . . ?
Ni3 O21 Ni4 103.1(4) . . ?
Ni3 O21 Ho1 115.5(4) . . ?
Ni4 O21 Ho1 110.4(4) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.441
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.165
# start Validation Reply Form
_vrf_PLAT306_complex-3           
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O8 Check 
RESPONSE: Due to disorder of  water molecules their Hydrogen could not be located with out pointing in the wrong direction.
;
_vrf_PLAT342_complex-3           
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0258 Ang.  
RESPONSE: Disordered  carbon atoms in the structure leads to low bond precision and due to poor diffraction quality of the crystal it was not possible to model this disorder.
;
_database_code_depnum_ccdc_archive 'CCDC 986611'
#######################################################################
#
#                 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_complex-4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C106 H78 N20 Ni8 O28 Tb2, 2(C H2 Cl2), 8(O)'
_chemical_formula_sum            'C108 H82 Cl4 N20 Ni8 O36 Tb2'
_chemical_formula_weight         3165.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_hall  '-P 2ybc'

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

_cell_length_a                   18.595(5)
_cell_length_b                   21.805(5)
_cell_length_c                   17.277(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 116.236(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     6284(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      4.11
_cell_measurement_theta_max      25.03

_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3160
_exptl_absorpt_coefficient_mu    2.448
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.710
_exptl_absorpt_correction_T_max  0.783
_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            31619
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_unetI/netI     0.0927
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.11
_diffrn_reflns_theta_max         25.03
_reflns_number_total             11049
_reflns_number_gt                7301
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Due to the weak high-angle diffractions internal R-value is high.
Actual molecular formula is C108 H106 Cl4 N20 Ni8 O36 Tb2 which differ from calculated molecular formula because hydrogen of eight water, two -OH and two oxime-OH and four coordinated Me-OH could not be modeled.

 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)+(0.1185P)²+106.2737P] 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         11049
_refine_ls_number_parameters     793
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1480
_refine_ls_R_factor_gt           0.1048
_refine_ls_wR_factor_ref         0.2915
_refine_ls_wR_factor_gt          0.2642
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.094
_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
C1 C -0.0457(11) 1.0349(9) -0.2824(12) 0.069(5) Uani 1 1 d . . .
H1A H -0.0856 1.0203 -0.3341 0.083 Uiso 1 1 calc R . .
C2 C -0.0263(11) 1.1008(9) -0.2669(11) 0.061(5) Uani 1 1 d . . .
C3 C -0.0706(13) 1.1450(11) -0.3275(13) 0.078(6) Uani 1 1 d . . .
H3 H -0.1128 1.1341 -0.3799 0.093 Uiso 1 1 calc R . .
C4 C -0.0503(15) 1.2032(13) -0.3079(15) 0.092(8) Uani 1 1 d . . .
H4 H -0.0810 1.2329 -0.3473 0.110 Uiso 1 1 calc R . .
C5 C 0.0131(14) 1.2225(10) -0.2329(16) 0.078(7) Uani 1 1 d . . .
C6 C 0.0382(14) 1.2822(10) -0.2106(16) 0.084(7) Uani 1 1 d . . .
H6 H 0.0122 1.3140 -0.2485 0.101 Uiso 1 1 calc R . .
C7 C 0.1030(14) 1.2949(9) -0.1306(16) 0.080(6) Uani 1 1 d . . .
H7 H 0.1197 1.3353 -0.1167 0.096 Uiso 1 1 calc R . .
C8 C 0.1439(12) 1.2478(9) -0.0701(13) 0.071(5) Uani 1 1 d . . .
H8 H 0.1855 1.2579 -0.0169 0.085 Uiso 1 1 calc R . .
C9 C 0.1222(11) 1.1878(8) -0.0900(13) 0.063(5) Uani 1 1 d . . .
C10 C 0.0552(10) 1.1735(9) -0.1750(12) 0.061(5) Uani 1 1 d . . .
C11 C 0.1899(10) 1.0462(8) 0.2060(12) 0.055(4) Uani 1 1 d . . .
H11 H 0.1431 1.0466 0.2130 0.066 Uiso 1 1 calc R . .
C12 C 0.2703(10) 1.0524(8) 0.2810(11) 0.053(4) Uani 1 1 d . . .
C13 C 0.2869(12) 1.0585(8) 0.3659(12) 0.058(4) Uani 1 1 d . . .
H13 H 0.2458 1.0602 0.3826 0.070 Uiso 1 1 calc R . .
C14 C 0.3657(12) 1.0621(8) 0.4263(11) 0.058(4) Uani 1 1 d . . .
H14 H 0.3781 1.0652 0.4845 0.070 Uiso 1 1 calc R . .
C15 C 0.4286(9) 1.0611(6) 0.4007(10) 0.042(3) Uani 1 1 d . . .
C16 C 0.5121(10) 1.0622(7) 0.4579(10) 0.049(4) Uani 1 1 d . . .
H16 H 0.5292 1.0658 0.5171 0.059 Uiso 1 1 calc R . .
C17 C 0.5671(9) 1.0577(6) 0.4250(9) 0.043(4) Uani 1 1 d . . .
H17 H 0.6215 1.0589 0.4624 0.052 Uiso 1 1 calc R . .
C18 C 0.5422(10) 1.0514(6) 0.3351(10) 0.045(4) Uani 1 1 d . . .
H18 H 0.5809 1.0478 0.3150 0.054 Uiso 1 1 calc R . .
C19 C 0.4617(9) 1.0503(6) 0.2762(9) 0.037(3) Uani 1 1 d . . .
C20 C 0.4056(9) 1.0553(7) 0.3115(10) 0.043(3) Uani 1 1 d . . .
C21 C 0.6015(8) 0.9245(6) 0.2515(8) 0.035(3) Uani 1 1 d . . .
H21 H 0.6558 0.9150 0.2787 0.042 Uiso 1 1 calc R . .
C22 C 0.5449(9) 0.8990(6) 0.2812(8) 0.036(3) Uani 1 1 d . . .
C23 C 0.5702(9) 0.8620(6) 0.3589(9) 0.044(4) Uani 1 1 d . . .
H23 H 0.6234 0.8506 0.3913 0.052 Uiso 1 1 calc R . .
C24 C 0.5120(10) 0.8450(6) 0.3814(9) 0.045(4) Uani 1 1 d . . .
H24 H 0.5269 0.8214 0.4310 0.054 Uiso 1 1 calc R . .
C25 C 0.4317(10) 0.8603(7) 0.3358(9) 0.047(4) Uani 1 1 d . . .
C26 C 0.3682(10) 0.8464(7) 0.3557(9) 0.046(4) Uani 1 1 d . . .
H26 H 0.3786 0.8246 0.4058 0.055 Uiso 1 1 calc R . .
C27 C 0.2920(10) 0.8638(7) 0.3036(11) 0.052(4) Uani 1 1 d . . .
H27 H 0.2517 0.8541 0.3195 0.063 Uiso 1 1 calc R . .
C28 C 0.2718(10) 0.8961(7) 0.2260(10) 0.049(4) Uani 1 1 d . . .
H28 H 0.2186 0.9060 0.1905 0.059 Uiso 1 1 calc R . .
C29 C 0.3316(9) 0.9133(6) 0.2026(9) 0.041(3) Uani 1 1 d . . .
C30 C 0.4113(8) 0.8960(6) 0.2573(8) 0.032(3) Uani 1 1 d . . .
C31 C 0.1468(10) 0.8393(8) -0.0296(10) 0.053(4) Uani 1 1 d . . .
H31 H 0.0967 0.8216 -0.0458 0.063 Uiso 1 1 calc R . .
C32 C 0.2220(9) 0.8033(7) 0.0044(9) 0.043(4) Uani 1 1 d . . .
C33 C 0.2262(11) 0.7382(8) 0.0199(10) 0.058(5) Uani 1 1 d . . .
H33 H 0.1807 0.7154 0.0103 0.070 Uiso 1 1 calc R . .
C34 C 0.2994(11) 0.7116(6) 0.0491(9) 0.051(4) Uani 1 1 d . . .
H34 H 0.3034 0.6698 0.0609 0.061 Uiso 1 1 calc R . .
C35 C 0.3688(10) 0.7433(6) 0.0625(9) 0.043(4) Uani 1 1 d . . .
C36 C 0.4477(10) 0.7183(6) 0.0938(9) 0.044(4) Uani 1 1 d . . .
H36 H 0.4572 0.6768 0.1069 0.053 Uiso 1 1 calc R . .
C37 C 0.5069(10) 0.7560(6) 0.1037(10) 0.047(4) Uani 1 1 d . . .
H37 H 0.5578 0.7391 0.1234 0.057 Uiso 1 1 calc R . .
C38 C 0.4994(9) 0.8197(6) 0.0869(9) 0.041(3) Uani 1 1 d . . .
H38 H 0.5439 0.8433 0.0952 0.049 Uiso 1 1 calc R . .
C39 C 0.4249(9) 0.8458(6) 0.0580(8) 0.040(3) Uani 1 1 d . . .
C40 C 0.3584(9) 0.8081(6) 0.0462(8) 0.034(3) Uani 1 1 d . . .
C41 C 0.2523(9) 0.8880(7) -0.1680(8) 0.040(3) Uani 1 1 d . . .
C42 C 0.1760(9) 0.8656(6) -0.2147(9) 0.045(4) Uani 1 1 d . . .
H42 H 0.1331 0.8849 -0.2109 0.053 Uiso 1 1 calc R . .
C43 C 0.1618(10) 0.8137(8) -0.2682(9) 0.051(4) Uani 1 1 d . . .
H43 H 0.1097 0.7995 -0.2996 0.062 Uiso 1 1 calc R . .
C44 C 0.2231(10) 0.7844(7) -0.2745(9) 0.049(4) Uani 1 1 d . . .
H44 H 0.2120 0.7501 -0.3098 0.059 Uiso 1 1 calc R . .
C45 C 0.3021(10) 0.8040(6) -0.2299(9) 0.044(4) Uani 1 1 d . . .
C46 C 0.3162(8) 0.8560(6) -0.1765(8) 0.038(3) Uani 1 1 d . . .
C47 C 0.4722(8) 1.1121(6) 0.0852(8) 0.034(3) Uani 1 1 d . . .
H47 H 0.4227 1.1262 0.0786 0.040 Uiso 1 1 calc R . .
C48 C 0.5455(8) 1.1457(6) 0.1338(8) 0.031(3) Uani 1 1 d . . .
C49 C 0.5552(9) 1.1973(6) 0.1851(9) 0.041(3) Uani 1 1 d . . .
H49 H 0.5105 1.2155 0.1864 0.049 Uiso 1 1 calc R . .
C50 C 0.6302(10) 1.2217(6) 0.2340(9) 0.045(4) Uani 1 1 d . . .
H50 H 0.6360 1.2551 0.2698 0.054 Uiso 1 1 calc R . .
C51 C 0.2704(11) 0.0412(10) 0.5483(13) 0.088(7) Uani 1 1 d D . .
H51A H 0.2972 0.0424 0.5112 0.105 Uiso 1 1 calc R . .
H51B H 0.3111 0.0401 0.6078 0.105 Uiso 1 1 calc R . .
C52 C 0.3196(12) 1.1832(7) 0.1600(11) 0.071(5) Uani 1 1 d D . .
H52A H 0.2781 1.1921 0.1772 0.107 Uiso 1 1 calc R . .
H52B H 0.3300 1.2190 0.1342 0.107 Uiso 1 1 calc R . .
H52C H 0.3675 1.1714 0.2097 0.107 Uiso 1 1 calc R . .
C53 C 0.1468(12) 1.0372(10) -0.2662(10) 0.074(3) Uani 1 1 d DU . .
H53A H 0.1174 1.0032 -0.3012 0.112 Uiso 1 1 calc R . .
H53B H 0.1957 1.0426 -0.2716 0.112 Uiso 1 1 calc R . .
H53C H 0.1150 1.0738 -0.2851 0.112 Uiso 1 1 calc R . .
C54 C -0.0423(12) 1.1154(8) -0.0667(15) 0.081(3) Uani 1 1 d DU . .
H54A H -0.0021 1.1308 -0.0129 0.121 Uiso 1 1 calc R . .
H54B H -0.0935 1.1158 -0.0658 0.121 Uiso 1 1 calc R . .
H54C H -0.0444 1.1409 -0.1131 0.121 Uiso 1 1 calc R . .
N1 N -0.0032(8) 0.9990(7) -0.2191(9) 0.056(4) Uani 1 1 d . . .
N2 N 0.0337(8) 1.1147(7) -0.1942(10) 0.059(4) Uani 1 1 d . . .
N3 N 0.1881(8) 1.0401(6) 0.1314(9) 0.051(3) Uani 1 1 d . . .
N4 N 0.3286(7) 1.0520(5) 0.2549(7) 0.041(3) Uani 1 1 d . . .
N5 N 0.5728(7) 0.9600(5) 0.1872(7) 0.035(3) Uani 1 1 d . . .
N6 N 0.4697(6) 0.9138(5) 0.2345(7) 0.031(2) Uani 1 1 d . . .
N7 N 0.1572(7) 0.9002(6) -0.0351(8) 0.046(3) Uani 1 1 d . . .
N8 N 0.2868(8) 0.8347(5) 0.0189(7) 0.040(3) Uani 1 1 d . . .
N9 N 0.3896(7) 0.8810(5) -0.1327(7) 0.035(3) Uani 1 1 d . . .
N10 N 0.4801(7) 1.0612(5) 0.0515(6) 0.036(3) Uani 1 1 d . . .
O1 O -0.0209(7) 0.9379(5) -0.2340(8) 0.063(3) Uani 1 1 d . . .
O2 O 0.1564(6) 1.1378(5) -0.0420(7) 0.060(3) Uani 1 1 d . . .
O3 O 0.1166(7) 1.0333(6) 0.0629(8) 0.066(3) Uani 1 1 d . . .
O4 O 0.4331(6) 1.0449(4) 0.1925(6) 0.038(2) Uani 1 1 d . . .
O5 O 0.6225(6) 0.9821(4) 0.1578(6) 0.038(2) Uani 1 1 d . . .
O6 O 0.3185(6) 0.9465(4) 0.1330(5) 0.034(2) Uani 1 1 d . . .
O7 O 0.0928(7) 0.9326(6) -0.0718(8) 0.071(4) Uani 1 1 d . . .
O8 O 0.4113(6) 0.9065(4) 0.0428(5) 0.036(2) Uani 1 1 d . . .
O9 O 0.2728(5) 0.9367(4) -0.1143(6) 0.036(2) Uani 1 1 d . . .
O10 O 0.4158(6) 1.0225(4) 0.0239(6) 0.036(2) Uani 1 1 d . . .
O11 O 0.2509(6) 1.0193(4) 0.0022(6) 0.038(2) Uani 1 1 d . . .
O12 O 0.1660(8) 1.0249(6) -0.1744(8) 0.074(3) Uani 1 1 d D . .
O13 O -0.0221(8) 1.0520(6) -0.0798(10) 0.081(3) Uani 1 1 d D . .
O14 O 0.2929(6) 1.1316(4) 0.0956(7) 0.047(2) Uani 1 1 d D . .
O15 O 0.3464(12) 0.2341(12) 0.9744(16) 0.171(11) Uani 1 1 d . . .
O16 O 0.6987(12) 0.8739(13) 0.1167(14) 0.166(10) Uani 1 1 d . . .
O17 O 0.0250(17) 0.669(3) 0.0188(19) 0.33(2) Uani 1 1 d U . .
O18 O 0.067(3) 0.189(2) 0.093(3) 0.37(3) Uani 1 1 d . . .
Cl1 Cl 0.2115(6) -0.0228(10) 0.5261(7) 0.294(11) Uani 1 1 d D . .
Cl2 Cl 0.212(2) 0.1054(12) 0.531(2) 0.58(3) Uani 1 1 d DU . .
Ni1 Ni 0.29873(11) 1.04056(8) 0.13088(11) 0.0371(4) Uani 1 1 d . . .
Ni2 Ni 0.44874(10) 0.96975(7) 0.13640(10) 0.0317(4) Uani 1 1 d . . .
Ni3 Ni 0.40549(10) 0.95532(7) -0.06375(10) 0.0281(4) Uani 1 1 d . . .
Ni4 Ni 0.27354(11) 0.92682(8) 0.00474(11) 0.0358(4) Uani 1 1 d . . .
Tb1 Tb 0.10898(4) 1.04027(4) -0.07637(5) 0.0492(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.29(2) . ?
C1 C2 1.48(3) . ?
C1 H1A 0.9300 . ?
C2 N2 1.29(2) . ?
C2 C3 1.39(2) . ?
C3 C4 1.32(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.38(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.38(3) . ?
C5 C10 1.44(2) . ?
C6 C7 1.40(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.42(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.37(3) . ?
C8 H8 0.9300 . ?
C9 O2 1.346(19) . ?
C9 C10 1.48(3) . ?
C10 N2 1.34(2) . ?
C11 N3 1.28(2) . ?
C11 C12 1.49(2) . ?
C11 H11 0.9300 . ?
C12 N4 1.347(19) . ?
C12 C13 1.36(2) . ?
C13 C14 1.38(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.42(2) . ?
C14 H14 0.9300 . ?
C15 C20 1.41(2) . ?
C15 C16 1.43(2) . ?
C16 C17 1.38(2) . ?
C16 H16 0.9300 . ?
C17 C18 1.42(2) . ?
C17 H17 0.9300 . ?
C18 C19 1.39(2) . ?
C18 H18 0.9300 . ?
C19 O4 1.308(16) . ?
C19 C20 1.43(2) . ?
C20 N4 1.331(19) . ?
C21 N5 1.263(16) . ?
C21 C22 1.469(19) . ?
C21 H21 0.9300 . ?
C22 N6 1.308(17) . ?
C22 C23 1.455(18) . ?
C23 C24 1.35(2) . ?
C23 H23 0.9300 . ?
C24 C25 1.39(2) . ?
C24 H24 0.9300 . ?
C25 C26 1.40(2) . ?
C25 C30 1.461(18) . ?
C26 C27 1.35(2) . ?
C26 H26 0.9300 . ?
C27 C28 1.41(2) . ?
C27 H27 0.9300 . ?
C28 C29 1.39(2) . ?
C28 H28 0.9300 . ?
C29 O6 1.332(17) . ?
C29 C30 1.41(2) . ?
C30 N6 1.365(17) . ?
C31 N7 1.35(2) . ?
C31 C32 1.48(2) . ?
C31 H31 0.9300 . ?
C32 N8 1.311(18) . ?
C32 C33 1.44(2) . ?
C33 C34 1.35(2) . ?
C33 H33 0.9300 . ?
C34 C35 1.39(2) . ?
C34 H34 0.9300 . ?
C35 C36 1.43(2) . ?
C35 C40 1.437(19) . ?
C36 C37 1.32(2) . ?
C36 H36 0.9300 . ?
C37 C38 1.413(19) . ?
C37 H37 0.9300 . ?
C38 C39 1.37(2) . ?
C38 H38 0.9300 . ?
C39 O8 1.353(16) . ?
C39 C40 1.42(2) . ?
C40 N8 1.332(18) . ?
C41 O9 1.349(16) . ?
C41 C42 1.37(2) . ?
C41 C46 1.44(2) . ?
C42 C43 1.41(2) . ?
C42 H42 0.9300 . ?
C43 C44 1.35(2) . ?
C43 H43 0.9300 . ?
C44 C45 1.39(2) . ?
C44 H44 0.9300 . ?
C45 C50 1.41(2) 3_675 ?
C45 C46 1.411(19) . ?
C46 N9 1.348(17) . ?
C47 N10 1.290(16) . ?
C47 C48 1.445(19) . ?
C47 H47 0.9300 . ?
C48 N9 1.348(17) 3_675 ?
C48 C49 1.394(18) . ?
C49 C50 1.38(2) . ?
C49 H49 0.9300 . ?
C50 C45 1.41(2) 3_675 ?
C50 H50 0.9300 . ?
C51 Cl1 1.711(16) . ?
C51 Cl2 1.720(17) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 O14 1.505(14) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 O12 1.490(15) . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 O13 1.476(15) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
N1 O1 1.370(18) . ?
N1 Tb1 2.587(14) . ?
N2 Tb1 2.494(13) . ?
N3 O3 1.342(17) . ?
N3 Ni1 2.061(13) . ?
N4 Ni1 1.977(11) . ?
N5 O5 1.326(14) . ?
N5 Ni2 2.084(11) . ?
N6 Ni2 1.983(11) . ?
N7 O7 1.290(16) . ?
N7 Ni4 2.043(12) . ?
N8 Ni4 2.026(11) . ?
N9 C48 1.348(17) 3_675 ?
N9 Ni3 1.955(11) . ?
N10 O10 1.365(14) . ?
N10 Ni3 2.074(12) 3_675 ?
O2 Tb1 2.279(12) . ?
O3 Tb1 2.352(12) . ?
O4 Ni2 1.990(9) . ?
O4 Ni1 2.244(10) . ?
O5 Ni3 2.006(9) 3_675 ?
O6 Ni4 2.038(9) . ?
O6 Ni1 2.082(8) . ?
O7 Tb1 2.372(13) . ?
O8 Ni2 2.001(8) . ?
O8 Ni3 2.087(8) . ?
O8 Ni4 2.388(10) . ?
O9 Ni4 2.062(9) . ?
O9 Ni3 2.261(9) . ?
O10 Ni3 2.054(9) . ?
O10 Ni2 2.104(9) . ?
O11 Ni1 2.049(10) . ?
O11 Ni4 2.058(8) . ?
O11 Tb1 2.418(9) . ?
O12 Tb1 2.385(12) . ?
O13 Tb1 2.425(13) . ?
O14 Ni1 2.065(9) . ?
Ni3 O5 2.006(9) 3_675 ?
Ni3 N10 2.074(12) 3_675 ?

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
N1 C1 C2 115.3(17) . . ?
N1 C1 H1A 122.3 . . ?
C2 C1 H1A 122.3 . . ?
N2 C2 C3 122.4(19) . . ?
N2 C2 C1 116.2(15) . . ?
C3 C2 C1 121.5(18) . . ?
C4 C3 C2 118(2) . . ?
C4 C3 H3 121.2 . . ?
C2 C3 H3 121.2 . . ?
C3 C4 C5 124.3(19) . . ?
C3 C4 H4 117.9 . . ?
C5 C4 H4 117.9 . . ?
C4 C5 C6 127(2) . . ?
C4 C5 C10 114(2) . . ?
C6 C5 C10 120(2) . . ?
C5 C6 C7 119.9(18) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 C8 122(2) . . ?
C6 C7 H7 119.0 . . ?
C8 C7 H7 119.0 . . ?
C9 C8 C7 120(2) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
O2 C9 C8 127.9(19) . . ?
O2 C9 C10 113.7(17) . . ?
C8 C9 C10 118.4(16) . . ?
N2 C10 C5 121.9(19) . . ?
N2 C10 C9 118.3(15) . . ?
C5 C10 C9 120(2) . . ?
N3 C11 C12 117.0(14) . . ?
N3 C11 H11 121.5 . . ?
C12 C11 H11 121.5 . . ?
N4 C12 C13 121.8(16) . . ?
N4 C12 C11 110.8(14) . . ?
C13 C12 C11 127.4(15) . . ?
C12 C13 C14 118.7(16) . . ?
C12 C13 H13 120.6 . . ?
C14 C13 H13 120.6 . . ?
C13 C14 C15 120.7(15) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C20 C15 C14 116.6(15) . . ?
C20 C15 C16 118.1(14) . . ?
C14 C15 C16 125.2(14) . . ?
C17 C16 C15 119.5(14) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C16 C17 C18 121.1(15) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C19 C18 C17 121.9(15) . . ?
C19 C18 H18 119.0 . . ?
C17 C18 H18 119.0 . . ?
O4 C19 C18 126.3(13) . . ?
O4 C19 C20 117.6(13) . . ?
C18 C19 C20 116.1(13) . . ?
N4 C20 C15 121.0(14) . . ?
N4 C20 C19 115.8(13) . . ?
C15 C20 C19 123.2(14) . . ?
N5 C21 C22 116.7(12) . . ?
N5 C21 H21 121.6 . . ?
C22 C21 H21 121.6 . . ?
N6 C22 C23 121.8(13) . . ?
N6 C22 C21 115.3(11) . . ?
C23 C22 C21 122.9(13) . . ?
C24 C23 C22 116.3(14) . . ?
C24 C23 H23 121.9 . . ?
C22 C23 H23 121.9 . . ?
C23 C24 C25 124.6(13) . . ?
C23 C24 H24 117.7 . . ?
C25 C24 H24 117.7 . . ?
C24 C25 C26 128.4(13) . . ?
C24 C25 C30 115.4(13) . . ?
C26 C25 C30 116.2(14) . . ?
C27 C26 C25 121.6(14) . . ?
C27 C26 H26 119.2 . . ?
C25 C26 H26 119.2 . . ?
C26 C27 C28 122.2(15) . . ?
C26 C27 H27 118.9 . . ?
C28 C27 H27 118.9 . . ?
C29 C28 C27 119.9(15) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
O6 C29 C28 123.9(14) . . ?
O6 C29 C30 117.9(12) . . ?
C28 C29 C30 118.1(13) . . ?
N6 C30 C29 117.8(11) . . ?
N6 C30 C25 120.3(12) . . ?
C29 C30 C25 121.9(13) . . ?
N7 C31 C32 114.2(13) . . ?
N7 C31 H31 122.9 . . ?
C32 C31 H31 122.9 . . ?
N8 C32 C33 120.6(15) . . ?
N8 C32 C31 115.2(13) . . ?
C33 C32 C31 124.2(14) . . ?
C34 C33 C32 117.0(15) . . ?
C34 C33 H33 121.5 . . ?
C32 C33 H33 121.5 . . ?
C33 C34 C35 123.8(14) . . ?
C33 C34 H34 118.1 . . ?
C35 C34 H34 118.1 . . ?
C34 C35 C36 126.7(13) . . ?
C34 C35 C40 114.8(14) . . ?
C36 C35 C40 118.4(14) . . ?
C37 C36 C35 118.0(13) . . ?
C37 C36 H36 121.0 . . ?
C35 C36 H36 121.0 . . ?
C36 C37 C38 125.7(15) . . ?
C36 C37 H37 117.1 . . ?
C38 C37 H37 117.1 . . ?
C39 C38 C37 118.3(14) . . ?
C39 C38 H38 120.9 . . ?
C37 C38 H38 120.9 . . ?
O8 C39 C38 123.3(14) . . ?
O8 C39 C40 117.5(13) . . ?
C38 C39 C40 119.2(13) . . ?
N8 C40 C39 117.9(12) . . ?
N8 C40 C35 121.7(13) . . ?
C39 C40 C35 120.4(13) . . ?
O9 C41 C42 126.0(14) . . ?
O9 C41 C46 117.1(12) . . ?
C42 C41 C46 116.9(13) . . ?
C41 C42 C43 121.0(15) . . ?
C41 C42 H42 119.5 . . ?
C43 C42 H42 119.5 . . ?
C44 C43 C42 120.8(15) . . ?
C44 C43 H43 119.6 . . ?
C42 C43 H43 119.6 . . ?
C43 C44 C45 122.2(14) . . ?
C43 C44 H44 118.9 . . ?
C45 C44 H44 118.9 . . ?
C44 C45 C50 126.8(13) . 3_675 ?
C44 C45 C46 117.0(14) . . ?
C50 C45 C46 116.1(14) 3_675 . ?
N9 C46 C45 122.8(14) . . ?
N9 C46 C41 115.0(12) . . ?
C45 C46 C41 122.1(13) . . ?
N10 C47 C48 115.6(12) . . ?
N10 C47 H47 122.2 . . ?
C48 C47 H47 122.2 . . ?
N9 C48 C49 119.5(12) 3_675 . ?
N9 C48 C47 113.1(11) 3_675 . ?
C49 C48 C47 127.1(12) . . ?
C50 C49 C48 120.9(14) . . ?
C50 C49 H49 119.6 . . ?
C48 C49 H49 119.6 . . ?
C49 C50 C45 120.0(13) . 3_675 ?
C49 C50 H50 120.0 . . ?
C45 C50 H50 120.0 3_675 . ?
Cl1 C51 Cl2 109.3(13) . . ?
Cl1 C51 H51A 109.8 . . ?
Cl2 C51 H51A 109.8 . . ?
Cl1 C51 H51B 109.8 . . ?
Cl2 C51 H51B 109.8 . . ?
H51A C51 H51B 108.3 . . ?
O14 C52 H52A 109.5 . . ?
O14 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
O14 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O12 C53 H53A 109.5 . . ?
O12 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
O12 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
O13 C54 H54A 109.5 . . ?
O13 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
O13 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C1 N1 O1 115.1(15) . . ?
C1 N1 Tb1 121.9(13) . . ?
O1 N1 Tb1 122.9(9) . . ?
C2 N2 C10 119.9(15) . . ?
C2 N2 Tb1 124.8(12) . . ?
C10 N2 Tb1 115.0(12) . . ?
C11 N3 O3 118.2(13) . . ?
C11 N3 Ni1 115.0(11) . . ?
O3 N3 Ni1 126.8(10) . . ?
C20 N4 C12 121.2(13) . . ?
C20 N4 Ni1 119.9(10) . . ?
C12 N4 Ni1 118.8(11) . . ?
C21 N5 O5 117.6(11) . . ?
C21 N5 Ni2 113.0(9) . . ?
O5 N5 Ni2 129.1(8) . . ?
C22 N6 C30 121.5(11) . . ?
C22 N6 Ni2 115.6(9) . . ?
C30 N6 Ni2 122.7(8) . . ?
O7 N7 C31 116.3(13) . . ?
O7 N7 Ni4 128.6(10) . . ?
C31 N7 Ni4 114.7(11) . . ?
C32 N8 C40 122.0(12) . . ?
C32 N8 Ni4 116.3(10) . . ?
C40 N8 Ni4 121.6(9) . . ?
C46 N9 C48 120.5(11) . 3_675 ?
C46 N9 Ni3 121.4(10) . . ?
C48 N9 Ni3 118.1(9) 3_675 . ?
C47 N10 O10 115.6(11) . . ?
C47 N10 Ni3 114.8(9) . 3_675 ?
O10 N10 Ni3 128.9(8) . 3_675 ?
C9 O2 Tb1 124.9(12) . . ?
N3 O3 Tb1 118.9(9) . . ?
C19 O4 Ni2 122.4(8) . . ?
C19 O4 Ni1 110.6(8) . . ?
Ni2 O4 Ni1 96.1(4) . . ?
N5 O5 Ni3 125.6(7) . 3_675 ?
C29 O6 Ni4 133.8(8) . . ?
C29 O6 Ni1 120.8(8) . . ?
Ni4 O6 Ni1 101.8(4) . . ?
N7 O7 Tb1 117.1(9) . . ?
C39 O8 Ni2 123.3(8) . . ?
C39 O8 Ni3 127.1(8) . . ?
Ni2 O8 Ni3 103.0(4) . . ?
C39 O8 Ni4 108.7(9) . . ?
Ni2 O8 Ni4 92.5(4) . . ?
Ni3 O8 Ni4 91.8(3) . . ?
C41 O9 Ni4 118.6(8) . . ?
C41 O9 Ni3 109.6(8) . . ?
Ni4 O9 Ni3 96.2(4) . . ?
N10 O10 Ni3 118.8(7) . . ?
N10 O10 Ni2 99.4(7) . . ?
Ni3 O10 Ni2 100.6(4) . . ?
Ni1 O11 Ni4 102.2(4) . . ?
Ni1 O11 Tb1 114.2(4) . . ?
Ni4 O11 Tb1 111.1(4) . . ?
C53 O12 Tb1 139.4(11) . . ?
C54 O13 Tb1 114.6(11) . . ?
C52 O14 Ni1 122.9(9) . . ?
N4 Ni1 O11 169.5(5) . . ?
N4 Ni1 N3 78.4(5) . . ?
O11 Ni1 N3 92.8(5) . . ?
N4 Ni1 O14 98.8(4) . . ?
O11 Ni1 O14 87.4(4) . . ?
N3 Ni1 O14 94.8(5) . . ?
N4 Ni1 O6 98.2(4) . . ?
O11 Ni1 O6 77.6(3) . . ?
N3 Ni1 O6 99.5(5) . . ?
O14 Ni1 O6 159.7(4) . . ?
N4 Ni1 O4 76.1(4) . . ?
O11 Ni1 O4 112.5(4) . . ?
N3 Ni1 O4 154.5(4) . . ?
O14 Ni1 O4 90.1(4) . . ?
O6 Ni1 O4 83.2(3) . . ?
N6 Ni2 O4 96.1(4) . . ?
N6 Ni2 O8 97.7(4) . . ?
O4 Ni2 O8 152.6(4) . . ?
N6 Ni2 N5 79.3(4) . . ?
O4 Ni2 N5 104.6(4) . . ?
O8 Ni2 N5 101.2(4) . . ?
N6 Ni2 O10 173.6(4) . . ?
O4 Ni2 O10 87.3(4) . . ?
O8 Ni2 O10 77.0(3) . . ?
N5 Ni2 O10 105.1(4) . . ?
N9 Ni3 O5 98.9(4) . 3_675 ?
N9 Ni3 O10 168.6(4) . . ?
O5 Ni3 O10 91.0(4) 3_675 . ?
N9 Ni3 N10 77.9(5) . 3_675 ?
O5 Ni3 N10 95.0(4) 3_675 3_675 ?
O10 Ni3 N10 106.9(4) . 3_675 ?
N9 Ni3 O8 92.8(4) . . ?
O5 Ni3 O8 162.7(4) 3_675 . ?
O10 Ni3 O8 76.2(3) . . ?
N10 Ni3 O8 99.8(4) 3_675 . ?
N9 Ni3 O9 76.7(4) . . ?
O5 Ni3 O9 87.8(4) 3_675 . ?
O10 Ni3 O9 98.3(3) . . ?
N10 Ni3 O9 154.6(4) 3_675 . ?
O8 Ni3 O9 82.6(3) . . ?
N8 Ni4 O6 96.2(4) . . ?
N8 Ni4 N7 79.3(5) . . ?
O6 Ni4 N7 106.9(4) . . ?
N8 Ni4 O11 171.1(4) . . ?
O6 Ni4 O11 78.4(4) . . ?
N7 Ni4 O11 95.4(5) . . ?
N8 Ni4 O9 99.8(4) . . ?
O6 Ni4 O9 151.8(4) . . ?
N7 Ni4 O9 98.9(4) . . ?
O11 Ni4 O9 88.0(4) . . ?
N8 Ni4 O8 74.0(4) . . ?
O6 Ni4 O8 82.2(3) . . ?
N7 Ni4 O8 152.6(4) . . ?
O11 Ni4 O8 111.9(3) . . ?
O9 Ni4 O8 80.1(3) . . ?
O2 Tb1 O3 87.2(4) . . ?
O2 Tb1 O7 162.8(4) . . ?
O3 Tb1 O7 81.6(5) . . ?
O2 Tb1 O12 94.3(5) . . ?
O3 Tb1 O12 150.7(4) . . ?
O7 Tb1 O12 89.3(5) . . ?
O2 Tb1 O11 80.2(3) . . ?
O3 Tb1 O11 81.7(3) . . ?
O7 Tb1 O11 85.3(3) . . ?
O12 Tb1 O11 69.8(4) . . ?
O2 Tb1 O13 100.1(4) . . ?
O3 Tb1 O13 68.7(4) . . ?
O7 Tb1 O13 88.0(4) . . ?
O12 Tb1 O13 139.0(5) . . ?
O11 Tb1 O13 150.4(4) . . ?
O2 Tb1 N2 67.5(5) . . ?
O3 Tb1 N2 129.5(5) . . ?
O7 Tb1 N2 129.6(5) . . ?
O12 Tb1 N2 77.1(4) . . ?
O11 Tb1 N2 131.3(4) . . ?
O13 Tb1 N2 73.5(5) . . ?
O2 Tb1 N1 129.0(4) . . ?
O3 Tb1 N1 127.7(4) . . ?
O7 Tb1 N1 68.1(4) . . ?
O12 Tb1 N1 72.5(4) . . ?
O11 Tb1 N1 133.6(4) . . ?
O13 Tb1 N1 68.6(5) . . ?
N2 Tb1 N1 61.5(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 N2 4(2) . . . . ?
N1 C1 C2 C3 -176.0(18) . . . . ?
N2 C2 C3 C4 -1(3) . . . . ?
C1 C2 C3 C4 178.6(19) . . . . ?
C2 C3 C4 C5 2(4) . . . . ?
C3 C4 C5 C6 178(2) . . . . ?
C3 C4 C5 C10 -2(3) . . . . ?
C4 C5 C6 C7 178(2) . . . . ?
C10 C5 C6 C7 -2(3) . . . . ?
C5 C6 C7 C8 -1(3) . . . . ?
C6 C7 C8 C9 2(3) . . . . ?
C7 C8 C9 O2 177.2(17) . . . . ?
C7 C8 C9 C10 -1(3) . . . . ?
C4 C5 C10 N2 1(3) . . . . ?
C6 C5 C10 N2 -179.2(17) . . . . ?
C4 C5 C10 C9 -177.0(17) . . . . ?
C6 C5 C10 C9 3(3) . . . . ?
O2 C9 C10 N2 2(2) . . . . ?
C8 C9 C10 N2 -179.7(16) . . . . ?
O2 C9 C10 C5 179.9(15) . . . . ?
C8 C9 C10 C5 -2(2) . . . . ?
N3 C11 C12 N4 2(2) . . . . ?
N3 C11 C12 C13 -179.1(17) . . . . ?
N4 C12 C13 C14 -2(3) . . . . ?
C11 C12 C13 C14 178.3(16) . . . . ?
C12 C13 C14 C15 2(3) . . . . ?
C13 C14 C15 C20 -1(2) . . . . ?
C13 C14 C15 C16 -177.5(15) . . . . ?
C20 C15 C16 C17 0(2) . . . . ?
C14 C15 C16 C17 176.6(14) . . . . ?
C15 C16 C17 C18 -1(2) . . . . ?
C16 C17 C18 C19 1(2) . . . . ?
C17 C18 C19 O4 179.6(12) . . . . ?
C17 C18 C19 C20 -0.6(19) . . . . ?
C14 C15 C20 N4 1(2) . . . . ?
C16 C15 C20 N4 177.8(13) . . . . ?
C14 C15 C20 C19 -176.5(14) . . . . ?
C16 C15 C20 C19 0(2) . . . . ?
O4 C19 C20 N4 2.2(19) . . . . ?
C18 C19 C20 N4 -177.7(12) . . . . ?
O4 C19 C20 C15 179.8(12) . . . . ?
C18 C19 C20 C15 0(2) . . . . ?
N5 C21 C22 N6 3.2(18) . . . . ?
N5 C21 C22 C23 -174.3(13) . . . . ?
N6 C22 C23 C24 -2(2) . . . . ?
C21 C22 C23 C24 175.7(13) . . . . ?
C22 C23 C24 C25 0(2) . . . . ?
C23 C24 C25 C26 -178.0(15) . . . . ?
C23 C24 C25 C30 2(2) . . . . ?
C24 C25 C26 C27 -178.9(15) . . . . ?
C30 C25 C26 C27 2(2) . . . . ?
C25 C26 C27 C28 1(2) . . . . ?
C26 C27 C28 C29 -3(2) . . . . ?
C27 C28 C29 O6 -176.5(13) . . . . ?
C27 C28 C29 C30 2(2) . . . . ?
O6 C29 C30 N6 -0.8(18) . . . . ?
C28 C29 C30 N6 -179.1(12) . . . . ?
O6 C29 C30 C25 179.2(12) . . . . ?
C28 C29 C30 C25 1(2) . . . . ?
C24 C25 C30 N6 -2.1(19) . . . . ?
C26 C25 C30 N6 177.5(12) . . . . ?
C24 C25 C30 C29 177.9(13) . . . . ?
C26 C25 C30 C29 -3(2) . . . . ?
N7 C31 C32 N8 -4.3(19) . . . . ?
N7 C31 C32 C33 176.8(14) . . . . ?
N8 C32 C33 C34 0(2) . . . . ?
C31 C32 C33 C34 178.4(14) . . . . ?
C32 C33 C34 C35 -2(2) . . . . ?
C33 C34 C35 C36 179.4(15) . . . . ?
C33 C34 C35 C40 2(2) . . . . ?
C34 C35 C36 C37 -178.9(14) . . . . ?
C40 C35 C36 C37 -2(2) . . . . ?
C35 C36 C37 C38 1(2) . . . . ?
C36 C37 C38 C39 0(2) . . . . ?
C37 C38 C39 O8 177.6(12) . . . . ?
C37 C38 C39 C40 0.1(19) . . . . ?
O8 C39 C40 N8 1.7(17) . . . . ?
C38 C39 C40 N8 179.4(12) . . . . ?
O8 C39 C40 C35 -179.0(11) . . . . ?
C38 C39 C40 C35 -1.3(18) . . . . ?
C34 C35 C40 N8 -1.1(18) . . . . ?
C36 C35 C40 N8 -178.4(12) . . . . ?
C34 C35 C40 C39 179.6(12) . . . . ?
C36 C35 C40 C39 2.3(18) . . . . ?
O9 C41 C42 C43 -179.3(13) . . . . ?
C46 C41 C42 C43 0(2) . . . . ?
C41 C42 C43 C44 1(2) . . . . ?
C42 C43 C44 C45 -1(2) . . . . ?
C43 C44 C45 C50 -177.6(15) . . . 3_675 ?
C43 C44 C45 C46 1(2) . . . . ?
C44 C45 C46 N9 -177.2(13) . . . . ?
C50 C45 C46 N9 1(2) 3_675 . . . ?
C44 C45 C46 C41 0(2) . . . . ?
C50 C45 C46 C41 178.2(12) 3_675 . . . ?
O9 C41 C46 N9 -3.6(17) . . . . ?
C42 C41 C46 N9 177.2(12) . . . . ?
O9 C41 C46 C45 179.2(12) . . . . ?
C42 C41 C46 C45 0(2) . . . . ?
N10 C47 C48 N9 2.7(16) . . . 3_675 ?
N10 C47 C48 C49 -171.4(12) . . . . ?
N9 C48 C49 C50 0.6(19) 3_675 . . . ?
C47 C48 C49 C50 174.3(13) . . . . ?
C48 C49 C50 C45 3(2) . . . 3_675 ?
C2 C1 N1 O1 -179.4(14) . . . . ?
C2 C1 N1 Tb1 -1(2) . . . . ?
C3 C2 N2 C10 0(3) . . . . ?
C1 C2 N2 C10 -179.8(16) . . . . ?
C3 C2 N2 Tb1 174.4(14) . . . . ?
C1 C2 N2 Tb1 -6(2) . . . . ?
C5 C10 N2 C2 0(3) . . . . ?
C9 C10 N2 C2 177.8(15) . . . . ?
C5 C10 N2 Tb1 -174.5(12) . . . . ?
C9 C10 N2 Tb1 3.0(19) . . . . ?
C12 C11 N3 O3 178.9(13) . . . . ?
C12 C11 N3 Ni1 -0.2(19) . . . . ?
C15 C20 N4 C12 -2(2) . . . . ?
C19 C20 N4 C12 175.9(13) . . . . ?
C15 C20 N4 Ni1 -177.6(10) . . . . ?
C19 C20 N4 Ni1 0.1(17) . . . . ?
C13 C12 N4 C20 2(2) . . . . ?
C11 C12 N4 C20 -178.2(13) . . . . ?
C13 C12 N4 Ni1 178.3(13) . . . . ?
C11 C12 N4 Ni1 -2.3(17) . . . . ?
C22 C21 N5 O5 -178.1(10) . . . . ?
C22 C21 N5 Ni2 -2.6(15) . . . . ?
C23 C22 N6 C30 1.1(19) . . . . ?
C21 C22 N6 C30 -176.5(11) . . . . ?
C23 C22 N6 Ni2 175.5(10) . . . . ?
C21 C22 N6 Ni2 -2.1(14) . . . . ?
C29 C30 N6 C22 -179.1(12) . . . . ?
C25 C30 N6 C22 0.9(18) . . . . ?
C29 C30 N6 Ni2 6.9(16) . . . . ?
C25 C30 N6 Ni2 -173.1(10) . . . . ?
C32 C31 N7 O7 173.7(13) . . . . ?
C32 C31 N7 Ni4 0.1(16) . . . . ?
C33 C32 N8 C40 2(2) . . . . ?
C31 C32 N8 C40 -177.2(12) . . . . ?
C33 C32 N8 Ni4 -174.6(11) . . . . ?
C31 C32 N8 Ni4 6.5(16) . . . . ?
C39 C40 N8 C32 178.4(12) . . . . ?
C35 C40 N8 C32 -0.9(19) . . . . ?
C39 C40 N8 Ni4 -5.5(16) . . . . ?
C35 C40 N8 Ni4 175.2(9) . . . . ?
C45 C46 N9 C48 -4.4(19) . . . 3_675 ?
C41 C46 N9 C48 178.3(11) . . . 3_675 ?
C45 C46 N9 Ni3 177.1(10) . . . . ?
C41 C46 N9 Ni3 -0.2(16) . . . . ?
C48 C47 N10 O10 164.9(10) . . . . ?
C48 C47 N10 Ni3 -6.5(14) . . . 3_675 ?
C8 C9 O2 Tb1 174.6(14) . . . . ?
C10 C9 O2 Tb1 -7.5(19) . . . . ?
C11 N3 O3 Tb1 168.9(11) . . . . ?
Ni1 N3 O3 Tb1 -12.2(16) . . . . ?
C18 C19 O4 Ni2 64.9(16) . . . . ?
C20 C19 O4 Ni2 -114.9(12) . . . . ?
C18 C19 O4 Ni1 176.8(11) . . . . ?
C20 C19 O4 Ni1 -3.0(14) . . . . ?
C21 N5 O5 Ni3 -174.4(9) . . . 3_675 ?
Ni2 N5 O5 Ni3 11.0(15) . . . 3_675 ?
C28 C29 O6 Ni4 -78.0(17) . . . . ?
C30 C29 O6 Ni4 103.8(13) . . . . ?
C28 C29 O6 Ni1 75.9(15) . . . . ?
C30 C29 O6 Ni1 -102.2(12) . . . . ?
C31 N7 O7 Tb1 177.1(10) . . . . ?
Ni4 N7 O7 Tb1 -10.2(17) . . . . ?
C38 C39 O8 Ni2 -69.5(15) . . . . ?
C40 C39 O8 Ni2 108.1(12) . . . . ?
C38 C39 O8 Ni3 77.1(15) . . . . ?
C40 C39 O8 Ni3 -105.3(12) . . . . ?
C38 C39 O8 Ni4 -175.6(10) . . . . ?
C40 C39 O8 Ni4 2.0(13) . . . . ?
C42 C41 O9 Ni4 75.0(16) . . . . ?
C46 C41 O9 Ni4 -104.1(12) . . . . ?
C42 C41 O9 Ni3 -175.9(12) . . . . ?
C46 C41 O9 Ni3 4.9(14) . . . . ?
C47 N10 O10 Ni3 160.5(9) . . . . ?
Ni3 N10 O10 Ni3 -29.6(12) 3_675 . . . ?
C47 N10 O10 Ni2 -91.8(10) . . . . ?
Ni3 N10 O10 Ni2 78.1(8) 3_675 . . . ?
C20 N4 Ni1 O11 145(2) . . . . ?
C12 N4 Ni1 O11 -31(3) . . . . ?
C20 N4 Ni1 N3 177.7(12) . . . . ?
C12 N4 Ni1 N3 1.8(11) . . . . ?
C20 N4 Ni1 O14 -89.2(11) . . . . ?
C12 N4 Ni1 O14 94.9(11) . . . . ?
C20 N4 Ni1 O6 79.6(11) . . . . ?
C12 N4 Ni1 O6 -96.3(11) . . . . ?
C20 N4 Ni1 O4 -1.3(10) . . . . ?
C12 N4 Ni1 O4 -177.2(12) . . . . ?
Ni4 O11 Ni1 N4 -69(2) . . . . ?
Tb1 O11 Ni1 N4 51(2) . . . . ?
Ni4 O11 Ni1 N3 -100.7(5) . . . . ?
Tb1 O11 Ni1 N3 19.4(5) . . . . ?
Ni4 O11 Ni1 O14 164.7(4) . . . . ?
Tb1 O11 Ni1 O14 -75.3(4) . . . . ?
Ni4 O11 Ni1 O6 -1.6(4) . . . . ?
Tb1 O11 Ni1 O6 118.5(4) . . . . ?
Ni4 O11 Ni1 O4 75.6(4) . . . . ?
Tb1 O11 Ni1 O4 -164.4(3) . . . . ?
C11 N3 Ni1 N4 -0.8(12) . . . . ?
O3 N3 Ni1 N4 -179.7(13) . . . . ?
C11 N3 Ni1 O11 173.6(12) . . . . ?
O3 N3 Ni1 O11 -5.4(12) . . . . ?
C11 N3 Ni1 O14 -98.7(12) . . . . ?
O3 N3 Ni1 O14 82.3(12) . . . . ?
C11 N3 Ni1 O6 95.7(12) . . . . ?
O3 N3 Ni1 O6 -83.3(12) . . . . ?
C11 N3 Ni1 O4 1.6(19) . . . . ?
O3 N3 Ni1 O4 -177.4(9) . . . . ?
C52 O14 Ni1 N4 8.2(13) . . . . ?
C52 O14 Ni1 O11 179.7(12) . . . . ?
C52 O14 Ni1 N3 87.1(12) . . . . ?
C52 O14 Ni1 O6 -138.2(14) . . . . ?
C52 O14 Ni1 O4 -67.8(12) . . . . ?
C29 O6 Ni1 N4 10.7(11) . . . . ?
Ni4 O6 Ni1 N4 171.8(5) . . . . ?
C29 O6 Ni1 O11 -159.5(10) . . . . ?
Ni4 O6 Ni1 O11 1.6(4) . . . . ?
C29 O6 Ni1 N3 -68.8(11) . . . . ?
Ni4 O6 Ni1 N3 92.3(5) . . . . ?
C29 O6 Ni1 O14 157.1(12) . . . . ?
Ni4 O6 Ni1 O14 -41.8(13) . . . . ?
C29 O6 Ni1 O4 85.6(10) . . . . ?
Ni4 O6 Ni1 O4 -113.3(4) . . . . ?
C19 O4 Ni1 N4 2.3(8) . . . . ?
Ni2 O4 Ni1 N4 130.4(5) . . . . ?
C19 O4 Ni1 O11 -171.4(8) . . . . ?
Ni2 O4 Ni1 O11 -43.4(4) . . . . ?
C19 O4 Ni1 N3 -0.1(15) . . . . ?
Ni2 O4 Ni1 N3 128.0(10) . . . . ?
C19 O4 Ni1 O14 101.3(8) . . . . ?
Ni2 O4 Ni1 O14 -130.7(4) . . . . ?
C19 O4 Ni1 O6 -97.9(8) . . . . ?
Ni2 O4 Ni1 O6 30.2(3) . . . . ?
C22 N6 Ni2 O4 -103.1(9) . . . . ?
C30 N6 Ni2 O4 71.2(10) . . . . ?
C22 N6 Ni2 O8 100.6(9) . . . . ?
C30 N6 Ni2 O8 -85.0(10) . . . . ?
C22 N6 Ni2 N5 0.6(9) . . . . ?
C30 N6 Ni2 N5 174.9(10) . . . . ?
C22 N6 Ni2 O10 135(3) . . . . ?
C30 N6 Ni2 O10 -51(4) . . . . ?
C19 O4 Ni2 N6 21.8(11) . . . . ?
Ni1 O4 Ni2 N6 -97.3(4) . . . . ?
C19 O4 Ni2 O8 141.7(10) . . . . ?
Ni1 O4 Ni2 O8 22.6(9) . . . . ?
C19 O4 Ni2 N5 -58.7(11) . . . . ?
Ni1 O4 Ni2 N5 -177.8(4) . . . . ?
C19 O4 Ni2 O10 -163.6(10) . . . . ?
Ni1 O4 Ni2 O10 77.3(4) . . . . ?
C39 O8 Ni2 N6 -17.1(11) . . . . ?
Ni3 O8 Ni2 N6 -170.3(4) . . . . ?
Ni4 O8 Ni2 N6 97.3(4) . . . . ?
C39 O8 Ni2 O4 -136.6(11) . . . . ?
Ni3 O8 Ni2 O4 70.2(9) . . . . ?
Ni4 O8 Ni2 O4 -22.3(9) . . . . ?
C39 O8 Ni2 N5 63.5(11) . . . . ?
Ni3 O8 Ni2 N5 -89.7(5) . . . . ?
Ni4 O8 Ni2 N5 177.9(4) . . . . ?
C39 O8 Ni2 O10 166.6(11) . . . . ?
Ni3 O8 Ni2 O10 13.4(4) . . . . ?
Ni4 O8 Ni2 O10 -79.1(3) . . . . ?
C21 N5 Ni2 N6 1.2(9) . . . . ?
O5 N5 Ni2 N6 176.0(11) . . . . ?
C21 N5 Ni2 O4 94.8(10) . . . . ?
O5 N5 Ni2 O4 -90.4(10) . . . . ?
C21 N5 Ni2 O8 -94.6(10) . . . . ?
O5 N5 Ni2 O8 80.2(10) . . . . ?
C21 N5 Ni2 O10 -174.0(9) . . . . ?
O5 N5 Ni2 O10 0.8(11) . . . . ?
N10 O10 Ni2 N6 -170(3) . . . . ?
Ni3 O10 Ni2 N6 -48(4) . . . . ?
N10 O10 Ni2 O4 67.4(7) . . . . ?
Ni3 O10 Ni2 O4 -170.8(4) . . . . ?
N10 O10 Ni2 O8 -135.3(7) . . . . ?
Ni3 O10 Ni2 O8 -13.5(4) . . . . ?
N10 O10 Ni2 N5 -36.9(8) . . . . ?
Ni3 O10 Ni2 N5 84.9(4) . . . . ?
C46 N9 Ni3 O5 -83.4(10) . . . 3_675 ?
C48 N9 Ni3 O5 98.0(9) 3_675 . . 3_675 ?
C46 N9 Ni3 O10 67(3) . . . . ?
C48 N9 Ni3 O10 -112(2) 3_675 . . . ?
C46 N9 Ni3 N10 -176.7(11) . . . 3_675 ?
C48 N9 Ni3 N10 4.7(9) 3_675 . . 3_675 ?
C46 N9 Ni3 O8 83.8(10) . . . . ?
C48 N9 Ni3 O8 -94.7(9) 3_675 . . . ?
C46 N9 Ni3 O9 2.1(9) . . . . ?
C48 N9 Ni3 O9 -176.4(10) 3_675 . . . ?
N10 O10 Ni3 N9 137(2) . . . . ?
Ni2 O10 Ni3 N9 30(2) . . . . ?
N10 O10 Ni3 O5 -71.9(8) . . . 3_675 ?
Ni2 O10 Ni3 O5 -178.9(4) . . . 3_675 ?
N10 O10 Ni3 N10 23.7(10) . . . 3_675 ?
Ni2 O10 Ni3 N10 -83.3(4) . . . 3_675 ?
N10 O10 Ni3 O8 119.9(8) . . . . ?
Ni2 O10 Ni3 O8 12.9(4) . . . . ?
N10 O10 Ni3 O9 -159.8(8) . . . . ?
Ni2 O10 Ni3 O9 93.2(4) . . . . ?
C39 O8 Ni3 N9 17.8(12) . . . . ?
Ni2 O8 Ni3 N9 169.6(5) . . . . ?
Ni4 O8 Ni3 N9 -97.4(4) . . . . ?
C39 O8 Ni3 O5 150.8(13) . . . 3_675 ?
Ni2 O8 Ni3 O5 -57.4(14) . . . 3_675 ?
Ni4 O8 Ni3 O5 35.6(14) . . . 3_675 ?
C39 O8 Ni3 O10 -165.6(12) . . . . ?
Ni2 O8 Ni3 O10 -13.7(4) . . . . ?
Ni4 O8 Ni3 O10 79.2(3) . . . . ?
C39 O8 Ni3 N10 -60.4(12) . . . 3_675 ?
Ni2 O8 Ni3 N10 91.5(5) . . . 3_675 ?
Ni4 O8 Ni3 N10 -175.6(4) . . . 3_675 ?
C39 O8 Ni3 O9 94.0(11) . . . . ?
Ni2 O8 Ni3 O9 -114.2(4) . . . . ?
Ni4 O8 Ni3 O9 -21.2(3) . . . . ?
C41 O9 Ni3 N9 -3.8(8) . . . . ?
Ni4 O9 Ni3 N9 119.6(4) . . . . ?
C41 O9 Ni3 O5 95.9(8) . . . 3_675 ?
Ni4 O9 Ni3 O5 -140.6(4) . . . 3_675 ?
C41 O9 Ni3 O10 -173.3(8) . . . . ?
Ni4 O9 Ni3 O10 -49.9(4) . . . . ?
C41 O9 Ni3 N10 -1.2(13) . . . 3_675 ?
Ni4 O9 Ni3 N10 122.3(8) . . . 3_675 ?
C41 O9 Ni3 O8 -98.5(8) . . . . ?
Ni4 O9 Ni3 O8 24.9(3) . . . . ?
C32 N8 Ni4 O6 101.0(10) . . . . ?
C40 N8 Ni4 O6 -75.2(10) . . . . ?
C32 N8 Ni4 N7 -5.0(10) . . . . ?
C40 N8 Ni4 N7 178.7(11) . . . . ?
C32 N8 Ni4 O11 49(3) . . . . ?
C40 N8 Ni4 O11 -127(3) . . . . ?
C32 N8 Ni4 O9 -102.3(10) . . . . ?
C40 N8 Ni4 O9 81.4(10) . . . . ?
C32 N8 Ni4 O8 -178.9(10) . . . . ?
C40 N8 Ni4 O8 4.8(9) . . . . ?
C29 O6 Ni4 N8 -17.0(13) . . . . ?
Ni1 O6 Ni4 N8 -174.4(5) . . . . ?
C29 O6 Ni4 N7 63.6(13) . . . . ?
Ni1 O6 Ni4 N7 -93.8(5) . . . . ?
C29 O6 Ni4 O11 155.8(13) . . . . ?
Ni1 O6 Ni4 O11 -1.6(4) . . . . ?
C29 O6 Ni4 O9 -141.4(12) . . . . ?
Ni1 O6 Ni4 O9 61.2(9) . . . . ?
C29 O6 Ni4 O8 -89.9(12) . . . . ?
Ni1 O6 Ni4 O8 112.7(4) . . . . ?
O7 N7 Ni4 N8 -170.2(14) . . . . ?
C31 N7 Ni4 N8 2.5(10) . . . . ?
O7 N7 Ni4 O6 96.5(13) . . . . ?
C31 N7 Ni4 O6 -90.8(11) . . . . ?
O7 N7 Ni4 O11 17.0(14) . . . . ?
C31 N7 Ni4 O11 -170.3(11) . . . . ?
O7 N7 Ni4 O9 -71.9(13) . . . . ?
C31 N7 Ni4 O9 100.9(11) . . . . ?
O7 N7 Ni4 O8 -157.4(11) . . . . ?
C31 N7 Ni4 O8 15.3(17) . . . . ?
Ni1 O11 Ni4 N8 55(3) . . . . ?
Tb1 O11 Ni4 N8 -67(3) . . . . ?
Ni1 O11 Ni4 O6 1.6(4) . . . . ?
Tb1 O11 Ni4 O6 -120.6(5) . . . . ?
Ni1 O11 Ni4 N7 107.8(5) . . . . ?
Tb1 O11 Ni4 N7 -14.4(5) . . . . ?
Ni1 O11 Ni4 O9 -153.5(4) . . . . ?
Tb1 O11 Ni4 O9 84.3(4) . . . . ?
Ni1 O11 Ni4 O8 -75.0(4) . . . . ?
Tb1 O11 Ni4 O8 162.8(3) . . . . ?
C41 O9 Ni4 N8 22.9(10) . . . . ?
Ni3 O9 Ni4 N8 -93.5(4) . . . . ?
C41 O9 Ni4 O6 146.5(9) . . . . ?
Ni3 O9 Ni4 O6 30.1(9) . . . . ?
C41 O9 Ni4 N7 -57.6(10) . . . . ?
Ni3 O9 Ni4 N7 -174.0(4) . . . . ?
C41 O9 Ni4 O11 -152.8(10) . . . . ?
Ni3 O9 Ni4 O11 90.8(4) . . . . ?
C41 O9 Ni4 O8 94.6(10) . . . . ?
Ni3 O9 Ni4 O8 -21.8(3) . . . . ?
C39 O8 Ni4 N8 -3.5(7) . . . . ?
Ni2 O8 Ni4 N8 -130.0(4) . . . . ?
Ni3 O8 Ni4 N8 126.9(4) . . . . ?
C39 O8 Ni4 O6 95.3(7) . . . . ?
Ni2 O8 Ni4 O6 -31.2(3) . . . . ?
Ni3 O8 Ni4 O6 -134.4(3) . . . . ?
C39 O8 Ni4 N7 -16.6(13) . . . . ?
Ni2 O8 Ni4 N7 -143.1(8) . . . . ?
Ni3 O8 Ni4 N7 113.8(9) . . . . ?
C39 O8 Ni4 O11 169.4(7) . . . . ?
Ni2 O8 Ni4 O11 42.9(4) . . . . ?
Ni3 O8 Ni4 O11 -60.2(4) . . . . ?
C39 O8 Ni4 O9 -106.8(8) . . . . ?
Ni2 O8 Ni4 O9 126.7(4) . . . . ?
Ni3 O8 Ni4 O9 23.6(3) . . . . ?
C9 O2 Tb1 O3 -128.4(13) . . . . ?
C9 O2 Tb1 O7 -177.8(15) . . . . ?
C9 O2 Tb1 O12 80.9(13) . . . . ?
C9 O2 Tb1 O11 149.5(13) . . . . ?
C9 O2 Tb1 O13 -60.6(13) . . . . ?
C9 O2 Tb1 N2 6.7(12) . . . . ?
C9 O2 Tb1 N1 10.0(14) . . . . ?
N3 O3 Tb1 O2 -60.7(11) . . . . ?
N3 O3 Tb1 O7 106.2(11) . . . . ?
N3 O3 Tb1 O12 33.1(16) . . . . ?
N3 O3 Tb1 O11 19.8(10) . . . . ?
N3 O3 Tb1 O13 -162.7(12) . . . . ?
N3 O3 Tb1 N2 -118.4(11) . . . . ?
N3 O3 Tb1 N1 160.0(10) . . . . ?
N7 O7 Tb1 O2 -34(2) . . . . ?
N7 O7 Tb1 O3 -83.8(11) . . . . ?
N7 O7 Tb1 O12 68.3(11) . . . . ?
N7 O7 Tb1 O11 -1.5(11) . . . . ?
N7 O7 Tb1 O13 -152.6(12) . . . . ?
N7 O7 Tb1 N2 140.9(10) . . . . ?
N7 O7 Tb1 N1 139.7(12) . . . . ?
C53 O12 Tb1 O2 -84.3(18) . . . . ?
C53 O12 Tb1 O3 -176.3(16) . . . . ?
C53 O12 Tb1 O7 112.5(18) . . . . ?
C53 O12 Tb1 O11 -162.3(19) . . . . ?
C53 O12 Tb1 O13 26(2) . . . . ?
C53 O12 Tb1 N2 -18.5(18) . . . . ?
C53 O12 Tb1 N1 45.3(18) . . . . ?
Ni1 O11 Tb1 O2 66.7(4) . . . . ?
Ni4 O11 Tb1 O2 -178.4(5) . . . . ?
Ni1 O11 Tb1 O3 -22.0(5) . . . . ?
Ni4 O11 Tb1 O3 93.0(5) . . . . ?
Ni1 O11 Tb1 O7 -104.1(5) . . . . ?
Ni4 O11 Tb1 O7 10.8(5) . . . . ?
Ni1 O11 Tb1 O12 164.9(5) . . . . ?
Ni4 O11 Tb1 O12 -80.2(5) . . . . ?
Ni1 O11 Tb1 O13 -26.7(9) . . . . ?
Ni4 O11 Tb1 O13 88.3(8) . . . . ?
Ni1 O11 Tb1 N2 114.7(6) . . . . ?
Ni4 O11 Tb1 N2 -130.4(6) . . . . ?
Ni1 O11 Tb1 N1 -157.5(5) . . . . ?
Ni4 O11 Tb1 N1 -42.6(7) . . . . ?
C54 O13 Tb1 O2 4.3(13) . . . . ?
C54 O13 Tb1 O3 87.2(13) . . . . ?
C54 O13 Tb1 O7 169.0(13) . . . . ?
C54 O13 Tb1 O12 -104.5(14) . . . . ?
C54 O13 Tb1 O11 92.2(14) . . . . ?
C54 O13 Tb1 N2 -58.5(13) . . . . ?
C54 O13 Tb1 N1 -123.8(14) . . . . ?
C2 N2 Tb1 O2 -179.2(15) . . . . ?
C10 N2 Tb1 O2 -4.7(11) . . . . ?
C2 N2 Tb1 O3 -113.2(14) . . . . ?
C10 N2 Tb1 O3 61.2(13) . . . . ?
C2 N2 Tb1 O7 2.5(16) . . . . ?
C10 N2 Tb1 O7 177.0(10) . . . . ?
C2 N2 Tb1 O12 80.6(14) . . . . ?
C10 N2 Tb1 O12 -104.9(12) . . . . ?
C2 N2 Tb1 O11 128.3(13) . . . . ?
C10 N2 Tb1 O11 -57.2(13) . . . . ?
C2 N2 Tb1 O13 -70.4(14) . . . . ?
C10 N2 Tb1 O13 104.0(12) . . . . ?
C2 N2 Tb1 N1 3.7(13) . . . . ?
C10 N2 Tb1 N1 178.2(13) . . . . ?
C1 N1 Tb1 O2 -4.7(16) . . . . ?
O1 N1 Tb1 O2 173.8(9) . . . . ?
C1 N1 Tb1 O3 118.4(14) . . . . ?
O1 N1 Tb1 O3 -63.1(12) . . . . ?
C1 N1 Tb1 O7 177.8(15) . . . . ?
O1 N1 Tb1 O7 -3.8(10) . . . . ?
C1 N1 Tb1 O12 -85.8(14) . . . . ?
O1 N1 Tb1 O12 92.7(11) . . . . ?
C1 N1 Tb1 O11 -122.6(13) . . . . ?
O1 N1 Tb1 O11 55.9(12) . . . . ?
C1 N1 Tb1 O13 81.1(14) . . . . ?
O1 N1 Tb1 O13 -100.5(11) . . . . ?
C1 N1 Tb1 N2 -1.2(13) . . . . ?
O1 N1 Tb1 N2 177.2(12) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         2.300
_refine_diff_density_min         -2.057
_refine_diff_density_rms         0.205
# start Validation Reply Form
_vrf_PLAT306_complex-4           
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O15 Check 
RESPONSE: Due to disorder of  water molecules their Hydrogen could not be located with out pointing in the wrong direction.
;
_vrf_PLAT342_complex-4           
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0263 Ang.  
RESPONSE: Disordered  carbon atoms in the structure leads to low bond precision and due to poor diffraction quality of the crystal it was not possible to model this disorder.
;
_vrf_PLAT411_complex-4           
;
PROBLEM: Short Inter H...H Contact  H14    ..  H51A    ..       1.83 Ang.  
RESPONSE: in 3D crystal packing two hydrogen is coming close to each other.
;
# end Validation Reply Form

_database_code_depnum_ccdc_archive 'CCDC 986612'
