# 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_shelxl

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C65.40 H72.20 N4 Ni4 O12.70'
_chemical_formula_weight         1352.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.0042(2)
_cell_length_b                   14.6854(3)
_cell_length_c                   18.3859(3)
_cell_angle_alpha                94.7490(10)
_cell_angle_beta                 95.5530(10)
_cell_angle_gamma                105.1460(10)
_cell_volume                     3094.15(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    28122
_cell_measurement_theta_min      6.56
_cell_measurement_theta_max      71.95

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1412
_exptl_absorpt_coefficient_mu    1.908
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.710
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36381
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         6.56
_diffrn_reflns_theta_max         64.00
_reflns_number_total             9690
_reflns_number_gt                7126
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1165P)²+1.9583P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9690
_refine_ls_number_parameters     927
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0639
_refine_ls_wR_factor_ref         0.2073
_refine_ls_wR_factor_gt          0.1741
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_restrained_S_all      1.134
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.44773(6) 0.15289(6) 0.28238(4) 0.0336(2) Uani 1 1 d . . .
Ni2 Ni 0.15984(6) 0.10152(6) 0.27578(4) 0.0341(2) Uani 1 1 d . . .
Ni3 Ni 0.28832(6) 0.12953(6) 0.13732(4) 0.0306(2) Uani 1 1 d . . .
Ni4 Ni 0.31093(6) 0.30511(6) 0.26666(4) 0.0343(2) Uani 1 1 d . . .
N1 N 0.4598(3) 0.0491(3) 0.34126(18) 0.0314(9) Uani 1 1 d . . .
O1 O 0.3010(2) 0.0553(2) 0.22913(15) 0.0301(7) Uani 1 1 d . . .
O2 O 0.5711(3) 0.2497(2) 0.34466(17) 0.0423(8) Uani 1 1 d . . .
C1 C 0.3092(4) -0.0318(3) 0.2447(2) 0.0311(10) Uani 1 1 d . . .
C2 C 0.2393(4) -0.1161(4) 0.2066(2) 0.0351(11) Uani 1 1 d . . .
C3 C 0.2480(4) -0.2047(4) 0.2245(2) 0.0365(11) Uani 1 1 d . . .
C4 C 0.3301(4) -0.2116(4) 0.2817(2) 0.0378(11) Uani 1 1 d . . .
C5 C 0.3441(5) -0.3070(4) 0.2986(3) 0.0568(15) Uani 1 1 d . . .
H5A H 0.2673 -0.3526 0.2951 0.074 Uiso 1 1 calc R . .
H5B H 0.3842 -0.3011 0.3485 0.074 Uiso 1 1 calc R . .
H5C H 0.3899 -0.3293 0.2633 0.074 Uiso 1 1 calc R . .
C6 C 0.3984(4) -0.1288(4) 0.3203(3) 0.0388(12) Uani 1 1 d . . .
C7 C 0.3893(4) -0.0396(4) 0.3048(2) 0.0329(11) Uani 1 1 d . . .
C8 C 0.5304(4) 0.0585(4) 0.4009(2) 0.0341(11) Uani 1 1 d . . .
C9 C 0.6081(4) 0.1461(4) 0.4355(2) 0.0329(11) Uani 1 1 d . . .
C10 C 0.6740(4) 0.1422(4) 0.5033(3) 0.0398(12) Uani 1 1 d . . .
C11 C 0.7484(5) 0.2204(4) 0.5429(3) 0.0480(14) Uani 1 1 d . . .
C12 C 0.7627(5) 0.3076(5) 0.5161(3) 0.0558(16) Uani 1 1 d . . .
C13 C 0.7033(5) 0.3151(5) 0.4495(3) 0.0556(15) Uani 1 1 d . . .
C14 C 0.6247(4) 0.2355(4) 0.4072(2) 0.0422(12) Uani 1 1 d . . .
N2 N 0.1608(3) 0.0351(3) 0.3646(2) 0.0384(10) Uani 1 1 d . . .
O3 O 0.3046(3) 0.1956(2) 0.33361(15) 0.0336(7) Uani 1 1 d . . .
O4 O 0.0351(3) -0.0013(2) 0.21873(16) 0.0390(8) Uani 1 1 d . . .
C15 C 0.3038(4) 0.1817(4) 0.4067(2) 0.0344(11) Uani 1 1 d . . .
C16 C 0.3736(5) 0.2465(4) 0.4622(2) 0.0434(13) Uani 1 1 d . . .
C17 C 0.3709(5) 0.2275(5) 0.5350(3) 0.0517(15) Uani 1 1 d . . .
C18 C 0.2982(5) 0.1436(5) 0.5545(2) 0.0500(15) Uani 1 1 d . . .
C19 C 0.2936(5) 0.1258(5) 0.6344(3) 0.0594(17) Uani 1 1 d . . .
H19A H 0.3454 0.1804 0.6660 0.077 Uiso 1 1 calc R . .
H19B H 0.3187 0.0687 0.6426 0.077 Uiso 1 1 calc R . .
H19C H 0.2139 0.1168 0.6461 0.077 Uiso 1 1 calc R . .
C20 C 0.2310(4) 0.0807(4) 0.4986(3) 0.0432(14) Uani 1 1 d . . .
C21 C 0.2322(4) 0.0966(4) 0.4247(2) 0.0352(11) Uani 1 1 d . . .
C22 C 0.1006(4) -0.0505(4) 0.3688(3) 0.0429(13) Uani 1 1 d . . .
C23 C 0.0200(4) -0.1119(4) 0.3109(3) 0.0390(12) Uani 1 1 d . . .
C24 C -0.0335(5) -0.2042(4) 0.3265(3) 0.0509(14) Uani 1 1 d . . .
C25 C -0.1128(5) -0.2695(5) 0.2770(3) 0.0597(16) Uani 1 1 d . . .
C26 C -0.1433(5) -0.2439(5) 0.2088(3) 0.0563(15) Uani 1 1 d . . .
C27 C -0.0929(5) -0.1534(4) 0.1915(3) 0.0495(14) Uani 1 1 d . . .
C28 C -0.0095(4) -0.0842(4) 0.2398(3) 0.0424(12) Uani 1 1 d . . .
N3 N 0.2497(3) 0.2116(3) 0.06358(19) 0.0338(9) Uani 1 1 d . . .
O5 O 0.1811(2) 0.1890(2) 0.19487(15) 0.0306(7) Uani 1 1 d . . .
O6 O 0.4111(3) 0.0977(2) 0.08506(15) 0.0343(7) Uani 1 1 d . . .
C29 C 0.1090(4) 0.2189(3) 0.1444(2) 0.0314(10) Uani 1 1 d . . .
C30 C 0.0044(4) 0.2341(4) 0.1593(3) 0.0395(12) Uani 1 1 d . . .
C31 C -0.0579(4) 0.2726(4) 0.1094(3) 0.0470(14) Uani 1 1 d . . .
C32 C -0.0196(4) 0.2955(4) 0.0420(2) 0.0391(12) Uani 1 1 d . . .
C33 C -0.0871(5) 0.3400(4) -0.0121(3) 0.0543(15) Uani 1 1 d . . .
H33A H -0.1706 0.3143 -0.0102 0.071 Uiso 1 1 calc R . .
H33B H -0.0690 0.3256 -0.0619 0.071 Uiso 1 1 calc R . .
H33C H -0.0652 0.4090 0.0009 0.071 Uiso 1 1 calc R . .
C34 C 0.0827(4) 0.2765(4) 0.0260(2) 0.0346(11) Uani 1 1 d . . .
C35 C 0.1480(4) 0.2379(3) 0.0761(2) 0.0311(10) Uani 1 1 d . . .
C36 C 0.3071(4) 0.2346(4) 0.0080(2) 0.0388(12) Uani 1 1 d . . .
C37 C 0.4074(4) 0.2053(4) -0.0082(2) 0.0389(12) Uani 1 1 d . . .
C38 C 0.4633(5) 0.2471(5) -0.0670(3) 0.0583(17) Uani 1 1 d . . .
C39 C 0.5613(5) 0.2259(5) -0.0885(3) 0.0688(19) Uani 1 1 d . . .
C40 C 0.6063(5) 0.1623(5) -0.0516(3) 0.0630(17) Uani 1 1 d . . .
C41 C 0.5551(5) 0.1218(5) 0.0055(3) 0.0481(14) Uani 1 1 d . . .
C42 C 0.4552(4) 0.1414(4) 0.0298(2) 0.0369(11) Uani 1 1 d . . .
N4 N 0.3423(3) 0.3941(3) 0.19027(19) 0.0358(9) Uani 1 1 d . . .
O7 O 0.4170(2) 0.2436(2) 0.21035(15) 0.0323(7) Uani 1 1 d . . .
O8 O 0.1924(3) 0.3613(3) 0.30442(17) 0.0481(9) Uani 1 1 d . . .
C43 C 0.4859(4) 0.3122(3) 0.1763(2) 0.0316(10) Uani 1 1 d . . .
C44 C 0.5932(4) 0.3078(4) 0.1571(3) 0.0427(12) Uani 1 1 d . . .
H44 H 0.6243 0.2577 0.1710 0.056 Uiso 1 1 calc R . .
C45 C 0.6550(4) 0.3755(4) 0.1179(3) 0.0451(13) Uani 1 1 d . . .
C46 C 0.6142(4) 0.4517(4) 0.0986(3) 0.0418(12) Uani 1 1 d . . .
C47 C 0.6831(5) 0.5239(4) 0.0543(3) 0.0584(16) Uani 1 1 d . . .
H47A H 0.6345 0.5633 0.0358 0.076 Uiso 1 1 calc R . .
H47B H 0.7075 0.4910 0.0127 0.076 Uiso 1 1 calc R . .
H47C H 0.7519 0.5643 0.0856 0.076 Uiso 1 1 calc R . .
C48 C 0.5081(4) 0.4586(4) 0.1206(2) 0.0385(12) Uani 1 1 d . . .
C49 C 0.4457(4) 0.3903(3) 0.1600(2) 0.0328(10) Uani 1 1 d . . .
C50 C 0.2782(4) 0.4485(4) 0.1703(2) 0.0372(11) Uani 1 1 d . . .
C51 C 0.1780(4) 0.4574(4) 0.2038(3) 0.0401(12) Uani 1 1 d . . .
C52 C 0.1124(5) 0.5126(4) 0.1691(3) 0.0506(14) Uani 1 1 d . . .
C53 C 0.0160(6) 0.5284(5) 0.1945(4) 0.0675(19) Uani 1 1 d . . .
C54 C -0.0201(7) 0.4891(6) 0.2569(4) 0.082(2) Uani 1 1 d . . .
C55 C 0.0409(6) 0.4358(6) 0.2927(4) 0.076(2) Uani 1 1 d . . .
C56 C 0.1410(5) 0.4169(4) 0.2676(3) 0.0495(14) Uani 1 1 d . . .
O9 O 0.4562(3) 0.3837(3) 0.33660(17) 0.0459(9) Uani 1 1 d . . .
H9O H 0.5105 0.3575 0.3356 0.060 Uiso 1 1 calc R . .
C57 C 0.5040(6) 0.4840(5) 0.3574(3) 0.0683(18) Uani 1 1 d . . .
H57A H 0.5258 0.4950 0.4113 0.082 Uiso 1 1 calc R . .
H57B H 0.4425 0.5160 0.3455 0.082 Uiso 1 1 calc R . .
C58 C 0.6066(8) 0.5290(7) 0.3220(5) 0.122(3) Uani 1 1 d . . .
H58A H 0.6368 0.5958 0.3424 0.146 Uiso 1 1 calc R . .
H58B H 0.5842 0.5253 0.2689 0.146 Uiso 1 1 calc R . .
H58C H 0.6668 0.4960 0.3311 0.146 Uiso 1 1 calc R . .
O10 O 0.5451(3) 0.0998(2) 0.20877(17) 0.0401(8) Uani 1 1 d . . .
H10O H 0.5264 0.1025 0.1639 0.052 Uiso 1 1 calc R . .
C59 C 0.6499(5) 0.0739(6) 0.2179(3) 0.077(2) Uani 1 1 d . . .
H59A H 0.7087 0.1201 0.1955 0.092 Uiso 1 1 calc R . .
H59B H 0.6763 0.0812 0.2713 0.092 Uiso 1 1 calc R . .
C60 C 0.6502(8) -0.0165(6) 0.1894(4) 0.108(3) Uani 1 1 d . . .
H60A H 0.7288 -0.0243 0.1988 0.129 Uiso 1 1 calc R . .
H60B H 0.6258 -0.0253 0.1363 0.129 Uiso 1 1 calc R . .
H60C H 0.5962 -0.0638 0.2130 0.129 Uiso 1 1 calc R . .
O11 O 0.0600(3) 0.1830(3) 0.32507(17) 0.0452(9) Uani 1 1 d . . .
H11O H 0.0786 0.2414 0.3208 0.059 Uiso 1 1 calc R . .
C61 C -0.0517(7) 0.1563(8) 0.3460(5) 0.120(3) Uani 1 1 d D . .
C62 C -0.0552(16) 0.1551(17) 0.4230(6) 0.118(9) Uiso 0.57(3) 1 d PD . .
C62A C -0.121(3) 0.212(2) 0.3748(19) 0.107(16) Uiso 0.25(2) 1 d PD . .
C62B C -0.096(2) 0.094(2) 0.3984(14) 0.042(12) Uiso 0.18(2) 1 d PD . .
O12 O 0.1385(3) 0.0218(2) 0.09270(16) 0.0386(8) Uani 1 1 d . . .
H12O H 0.0789 0.0206 0.1134 0.050 Uiso 1 1 calc R . .
C63 C 0.1119(5) -0.0527(4) 0.0342(3) 0.0563(15) Uani 1 1 d . . .
H63A H 0.0266 -0.0747 0.0205 0.068 Uiso 1 1 calc R . .
H63B H 0.1386 -0.1068 0.0507 0.068 Uiso 1 1 calc R . .
C64 C 0.1688(5) -0.0207(4) -0.0311(3) 0.0562(15) Uani 1 1 d . . .
H64A H 0.1485 -0.0732 -0.0708 0.073 Uiso 1 1 calc R . .
H64B H 0.2533 -0.0003 -0.0179 0.073 Uiso 1 1 calc R . .
H64C H 0.1420 0.0326 -0.0477 0.073 Uiso 1 1 calc R . .
O1E O 0.2323(10) 0.4433(8) 0.4597(6) 0.160(4) Uani 0.70 1 d PU . .
C1E C 0.1727(9) 0.3823(9) 0.5013(5) 0.084(3) Uani 0.70 1 d P . .
C2E C 0.0988(10) 0.4193(9) 0.5449(8) 0.118(5) Uani 0.70 1 d P . .
H2 H 0.187(4) -0.101(3) 0.166(2) 0.035(12) Uiso 1 1 d . . .
H3 H 0.191(4) -0.263(3) 0.196(2) 0.034(12) Uiso 1 1 d . . .
H6 H 0.449(4) -0.133(3) 0.355(3) 0.040(14) Uiso 1 1 d . . .
H8 H 0.541(3) 0.005(3) 0.422(2) 0.027(12) Uiso 1 1 d . . .
H10 H 0.661(4) 0.080(4) 0.522(2) 0.035(13) Uiso 1 1 d . . .
H11 H 0.784(5) 0.218(4) 0.586(3) 0.063(17) Uiso 1 1 d . . .
H12 H 0.825(5) 0.364(4) 0.538(3) 0.069(18) Uiso 1 1 d . . .
H13 H 0.726(4) 0.384(3) 0.431(2) 0.034(12) Uiso 1 1 d . . .
H16 H 0.427(4) 0.314(4) 0.452(3) 0.057(16) Uiso 1 1 d . . .
H17 H 0.425(4) 0.272(3) 0.567(2) 0.033(13) Uiso 1 1 d . . .
H20 H 0.176(4) 0.032(3) 0.505(2) 0.037 Uiso 1 1 d . . .
H22 H 0.106(4) -0.072(4) 0.421(3) 0.048(14) Uiso 1 1 d . . .
H24 H -0.007(4) -0.224(3) 0.373(3) 0.037(13) Uiso 1 1 d . . .
H25 H -0.153(5) -0.333(5) 0.277(3) 0.07(2) Uiso 1 1 d . . .
H26 H -0.201(4) -0.291(4) 0.176(3) 0.048(15) Uiso 1 1 d . . .
H27 H -0.113(4) -0.138(3) 0.150(3) 0.033(13) Uiso 1 1 d . . .
H30 H -0.021(4) 0.219(4) 0.199(3) 0.045(15) Uiso 1 1 d . . .
H31 H -0.124(4) 0.282(4) 0.123(3) 0.044(14) Uiso 1 1 d . . .
H34 H 0.102(4) 0.279(4) -0.020(3) 0.054(15) Uiso 1 1 d . . .
H36 H 0.286(4) 0.279(3) -0.028(3) 0.043(13) Uiso 1 1 d . . .
H38 H 0.432(4) 0.287(4) -0.092(3) 0.057(17) Uiso 1 1 d . . .
H39 H 0.596(5) 0.253(4) -0.136(3) 0.071(17) Uiso 1 1 d . . .
H40 H 0.696(5) 0.149(4) -0.063(3) 0.082(19) Uiso 1 1 d . . .
H41 H 0.582(5) 0.081(4) 0.024(3) 0.058(18) Uiso 1 1 d . . .
H45 H 0.730(4) 0.366(3) 0.099(2) 0.042(13) Uiso 1 1 d . . .
H48 H 0.478(4) 0.513(4) 0.113(2) 0.040(13) Uiso 1 1 d . . .
H50 H 0.303(3) 0.486(3) 0.126(2) 0.030(11) Uiso 1 1 d . . .
H52 H 0.143(4) 0.538(3) 0.125(3) 0.044(14) Uiso 1 1 d . . .
H53 H -0.032(5) 0.556(4) 0.164(3) 0.066(18) Uiso 1 1 d . . .
H54 H -0.094(7) 0.494(5) 0.275(4) 0.12(3) Uiso 1 1 d . . .
H55 H 0.010(6) 0.406(5) 0.328(4) 0.10(2) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2 1.956(3) . ?
Ni1 N1 1.968(4) . ?
Ni1 O7 2.029(3) . ?
Ni1 O1 2.057(3) . ?
Ni1 O10 2.101(3) . ?
Ni1 O3 2.239(3) . ?
Ni2 O4 1.969(3) . ?
Ni2 N2 1.971(4) . ?
Ni2 O5 2.036(3) . ?
Ni2 O3 2.050(3) . ?
Ni2 O11 2.114(3) . ?
Ni2 O1 2.204(3) . ?
Ni3 O6 1.968(3) . ?
Ni3 N3 1.987(4) . ?
Ni3 O5 2.059(3) . ?
Ni3 O1 2.099(3) . ?
Ni3 O12 2.103(3) . ?
Ni3 O7 2.206(3) . ?
Ni4 O8 1.975(3) . ?
Ni4 N4 1.993(4) . ?
Ni4 O7 2.052(3) . ?
Ni4 O9 2.073(3) . ?
Ni4 O3 2.095(3) . ?
Ni4 O5 2.218(3) . ?
N1 C8 1.293(5) . ?
N1 C7 1.426(6) . ?
O1 C1 1.359(5) . ?
O2 C14 1.322(5) . ?
C1 C2 1.389(6) . ?
C1 C7 1.425(6) . ?
C2 C3 1.396(7) . ?
C2 H2 1.00(4) . ?
C3 C4 1.399(6) . ?
C3 H3 1.01(4) . ?
C4 C6 1.371(7) . ?
C4 C5 1.507(7) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.393(7) . ?
C6 H6 0.85(5) . ?
C8 C9 1.432(7) . ?
C8 H8 0.94(4) . ?
C9 C14 1.424(7) . ?
C9 C10 1.424(6) . ?
C10 C11 1.359(7) . ?
C10 H10 0.98(5) . ?
C11 C12 1.385(8) . ?
C11 H11 0.86(6) . ?
C12 C13 1.384(7) . ?
C12 H12 0.98(6) . ?
C13 C14 1.411(7) . ?
C13 H13 1.08(5) . ?
N2 C22 1.289(6) . ?
N2 C21 1.421(6) . ?
O3 C15 1.377(5) . ?
O4 C28 1.302(6) . ?
C15 C16 1.380(7) . ?
C15 C21 1.404(7) . ?
C16 C17 1.392(7) . ?
C16 H16 1.07(6) . ?
C17 C18 1.408(8) . ?
C17 H17 0.92(4) . ?
C18 C20 1.361(7) . ?
C18 C19 1.516(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.398(6) . ?
C20 H20 0.86(5) . ?
C22 C23 1.438(7) . ?
C22 H22 1.03(5) . ?
C23 C24 1.406(7) . ?
C23 C28 1.441(6) . ?
C24 C25 1.366(8) . ?
C24 H24 0.97(5) . ?
C25 C26 1.381(8) . ?
C25 H25 0.93(6) . ?
C26 C27 1.387(8) . ?
C26 H26 0.96(5) . ?
C27 C28 1.404(7) . ?
C27 H27 0.85(5) . ?
N3 C36 1.306(6) . ?
N3 C35 1.405(5) . ?
O5 C29 1.383(5) . ?
O6 C42 1.326(5) . ?
C29 C30 1.380(6) . ?
C29 C35 1.407(6) . ?
C30 C31 1.376(7) . ?
C30 H30 0.84(5) . ?
C31 C32 1.399(7) . ?
C31 H31 0.89(5) . ?
C32 C34 1.381(6) . ?
C32 C33 1.517(6) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.402(6) . ?
C34 H34 0.90(5) . ?
C36 C37 1.428(6) . ?
C36 H36 1.03(5) . ?
C37 C42 1.418(6) . ?
C37 C38 1.426(7) . ?
C38 C39 1.379(8) . ?
C38 H38 0.91(6) . ?
C39 C40 1.386(8) . ?
C39 H39 1.06(6) . ?
C40 C41 1.368(7) . ?
C40 H40 1.18(6) . ?
C41 C42 1.409(7) . ?
C41 H41 0.83(6) . ?
N4 C50 1.296(6) . ?
N4 C49 1.421(5) . ?
O7 C43 1.365(5) . ?
O8 C56 1.333(6) . ?
C43 C44 1.384(6) . ?
C43 C49 1.398(6) . ?
C44 C45 1.376(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.392(7) . ?
C45 H45 1.04(4) . ?
C46 C48 1.399(7) . ?
C46 C47 1.513(7) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 C49 1.387(6) . ?
C48 H48 0.98(5) . ?
C50 C51 1.433(6) . ?
C50 H50 1.05(4) . ?
C51 C56 1.416(7) . ?
C51 C52 1.417(7) . ?
C52 C53 1.356(8) . ?
C52 H52 0.99(5) . ?
C53 C54 1.383(9) . ?
C53 H53 0.95(6) . ?
C54 C55 1.369(9) . ?
C54 H54 1.00(7) . ?
C55 C56 1.412(8) . ?
C55 H55 0.88(7) . ?
O9 C57 1.438(7) . ?
O9 H9O 0.8400 . ?
C57 C58 1.476(10) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
O10 C59 1.406(6) . ?
O10 H10O 0.8400 . ?
C59 C60 1.387(9) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
O11 C61 1.396(7) . ?
O11 H11O 0.8400 . ?
C61 C62 1.422(5) . ?
C61 C62B 1.424(5) . ?
C61 C62A 1.425(5) . ?
C62 C62B 0.95(3) . ?
C62 C62A 1.57(3) . ?
C62A C62B 1.91(4) . ?
O12 C63 1.418(6) . ?
O12 H12O 0.8400 . ?
C63 C64 1.488(7) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
O1E C1E 1.335(13) . ?
C1E C2E 1.430(14) . ?

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
O2 Ni1 N1 94.92(14) . . ?
O2 Ni1 O7 94.16(13) . . ?
N1 Ni1 O7 170.87(14) . . ?
O2 Ni1 O1 170.78(12) . . ?
N1 Ni1 O1 83.96(13) . . ?
O7 Ni1 O1 87.23(12) . . ?
O2 Ni1 O10 100.68(13) . . ?
N1 Ni1 O10 87.48(13) . . ?
O7 Ni1 O10 89.90(12) . . ?
O1 Ni1 O10 88.42(12) . . ?
O2 Ni1 O3 93.84(13) . . ?
N1 Ni1 O3 98.67(13) . . ?
O7 Ni1 O3 81.66(11) . . ?
O1 Ni1 O3 77.33(12) . . ?
O10 Ni1 O3 163.71(12) . . ?
O4 Ni2 N2 94.09(16) . . ?
O4 Ni2 O5 96.04(12) . . ?
N2 Ni2 O5 169.87(16) . . ?
O4 Ni2 O3 171.76(13) . . ?
N2 Ni2 O3 83.32(15) . . ?
O5 Ni2 O3 86.68(11) . . ?
O4 Ni2 O11 100.25(13) . . ?
N2 Ni2 O11 88.75(14) . . ?
O5 Ni2 O11 89.18(12) . . ?
O3 Ni2 O11 87.54(13) . . ?
O4 Ni2 O1 94.33(12) . . ?
N2 Ni2 O1 97.01(13) . . ?
O5 Ni2 O1 82.52(11) . . ?
O3 Ni2 O1 78.27(12) . . ?
O11 Ni2 O1 163.91(13) . . ?
O6 Ni3 N3 93.98(13) . . ?
O6 Ni3 O5 168.93(13) . . ?
N3 Ni3 O5 81.60(13) . . ?
O6 Ni3 O1 99.72(12) . . ?
N3 Ni3 O1 166.20(13) . . ?
O5 Ni3 O1 84.63(11) . . ?
O6 Ni3 O12 103.14(13) . . ?
N3 Ni3 O12 89.36(14) . . ?
O5 Ni3 O12 87.02(12) . . ?
O1 Ni3 O12 89.10(12) . . ?
O6 Ni3 O7 91.53(12) . . ?
N3 Ni3 O7 96.34(14) . . ?
O5 Ni3 O7 78.95(11) . . ?
O1 Ni3 O7 81.76(11) . . ?
O12 Ni3 O7 163.87(11) . . ?
O8 Ni4 N4 93.29(15) . . ?
O8 Ni4 O7 170.19(12) . . ?
N4 Ni4 O7 81.21(14) . . ?
O8 Ni4 O9 99.52(14) . . ?
N4 Ni4 O9 92.26(14) . . ?
O7 Ni4 O9 88.86(13) . . ?
O8 Ni4 O3 100.63(13) . . ?
N4 Ni4 O3 165.96(14) . . ?
O7 Ni4 O3 84.75(12) . . ?
O9 Ni4 O3 87.30(13) . . ?
O8 Ni4 O5 93.83(13) . . ?
N4 Ni4 O5 96.27(13) . . ?
O7 Ni4 O5 78.80(11) . . ?
O9 Ni4 O5 163.71(13) . . ?
O3 Ni4 O5 81.07(11) . . ?
C8 N1 C7 124.4(4) . . ?
C8 N1 Ni1 124.8(4) . . ?
C7 N1 Ni1 110.4(3) . . ?
C1 O1 Ni1 107.0(2) . . ?
C1 O1 Ni3 139.1(3) . . ?
Ni1 O1 Ni3 95.16(12) . . ?
C1 O1 Ni2 114.9(2) . . ?
Ni1 O1 Ni2 102.63(13) . . ?
Ni3 O1 Ni2 92.30(11) . . ?
C14 O2 Ni1 124.5(3) . . ?
O1 C1 C2 123.3(4) . . ?
O1 C1 C7 119.9(4) . . ?
C2 C1 C7 116.8(4) . . ?
C1 C2 C3 122.2(4) . . ?
C1 C2 H2 109(3) . . ?
C3 C2 H2 128(3) . . ?
C2 C3 C4 120.6(5) . . ?
C2 C3 H3 118(3) . . ?
C4 C3 H3 122(3) . . ?
C6 C4 C3 117.6(5) . . ?
C6 C4 C5 121.6(4) . . ?
C3 C4 C5 120.8(5) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 C7 122.9(4) . . ?
C4 C6 H6 118(3) . . ?
C7 C6 H6 119(3) . . ?
C6 C7 C1 119.8(5) . . ?
C6 C7 N1 125.7(4) . . ?
C1 C7 N1 114.3(4) . . ?
N1 C8 C9 125.3(5) . . ?
N1 C8 H8 120(3) . . ?
C9 C8 H8 114(3) . . ?
C14 C9 C10 118.1(5) . . ?
C14 C9 C8 125.3(4) . . ?
C10 C9 C8 116.6(4) . . ?
C11 C10 C9 122.7(5) . . ?
C11 C10 H10 120(3) . . ?
C9 C10 H10 117(3) . . ?
C10 C11 C12 119.1(5) . . ?
C10 C11 H11 122(4) . . ?
C12 C11 H11 118(4) . . ?
C13 C12 C11 120.6(6) . . ?
C13 C12 H12 116(3) . . ?
C11 C12 H12 123(3) . . ?
C12 C13 C14 121.7(6) . . ?
C12 C13 H13 115(2) . . ?
C14 C13 H13 123(2) . . ?
O2 C14 C13 117.5(5) . . ?
O2 C14 C9 124.8(4) . . ?
C13 C14 C9 117.7(4) . . ?
C22 N2 C21 124.5(4) . . ?
C22 N2 Ni2 124.9(3) . . ?
C21 N2 Ni2 110.5(3) . . ?
C15 O3 Ni2 107.8(3) . . ?
C15 O3 Ni4 139.3(3) . . ?
Ni2 O3 Ni4 96.50(11) . . ?
C15 O3 Ni1 113.6(2) . . ?
Ni2 O3 Ni1 101.64(13) . . ?
Ni4 O3 Ni1 91.89(11) . . ?
C28 O4 Ni2 125.6(3) . . ?
O3 C15 C16 122.4(4) . . ?
O3 C15 C21 118.3(4) . . ?
C16 C15 C21 119.3(4) . . ?
C15 C16 C17 119.8(6) . . ?
C15 C16 H16 122(3) . . ?
C17 C16 H16 118(3) . . ?
C16 C17 C18 122.0(5) . . ?
C16 C17 H17 113(3) . . ?
C18 C17 H17 124(3) . . ?
C20 C18 C17 116.9(4) . . ?
C20 C18 C19 122.0(6) . . ?
C17 C18 C19 121.1(5) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 C21 122.9(5) . . ?
C18 C20 H20 123(3) . . ?
C21 C20 H20 113(3) . . ?
C20 C21 C15 119.2(5) . . ?
C20 C21 N2 125.1(5) . . ?
C15 C21 N2 115.6(4) . . ?
N2 C22 C23 126.0(4) . . ?
N2 C22 H22 115(3) . . ?
C23 C22 H22 119(3) . . ?
C24 C23 C22 116.7(5) . . ?
C24 C23 C28 119.1(5) . . ?
C22 C23 C28 124.2(5) . . ?
C25 C24 C23 122.9(5) . . ?
C25 C24 H24 119(3) . . ?
C23 C24 H24 118(3) . . ?
C24 C25 C26 118.9(6) . . ?
C24 C25 H25 134(4) . . ?
C26 C25 H25 107(4) . . ?
C25 C26 C27 120.0(6) . . ?
C25 C26 H26 117(3) . . ?
C27 C26 H26 124(3) . . ?
C26 C27 C28 123.5(5) . . ?
C26 C27 H27 120(3) . . ?
C28 C27 H27 117(3) . . ?
O4 C28 C27 119.6(4) . . ?
O4 C28 C23 124.7(5) . . ?
C27 C28 C23 115.7(5) . . ?
C36 N3 C35 123.7(4) . . ?
C36 N3 Ni3 124.8(3) . . ?
C35 N3 Ni3 111.4(3) . . ?
C29 O5 Ni2 136.3(3) . . ?
C29 O5 Ni3 107.6(2) . . ?
Ni2 O5 Ni3 98.56(13) . . ?
C29 O5 Ni4 114.7(3) . . ?
Ni2 O5 Ni4 93.16(11) . . ?
Ni3 O5 Ni4 100.81(11) . . ?
C42 O6 Ni3 124.5(3) . . ?
C30 C29 O5 123.1(4) . . ?
C30 C29 C35 119.4(4) . . ?
O5 C29 C35 117.4(4) . . ?
C31 C30 C29 120.3(4) . . ?
C31 C30 H30 121(3) . . ?
C29 C30 H30 119(3) . . ?
C30 C31 C32 121.8(5) . . ?
C30 C31 H31 116(3) . . ?
C32 C31 H31 122(3) . . ?
C34 C32 C31 117.8(4) . . ?
C34 C32 C33 120.6(4) . . ?
C31 C32 C33 121.6(5) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 C35 121.5(4) . . ?
C32 C34 H34 120(3) . . ?
C35 C34 H34 118(3) . . ?
C34 C35 N3 125.7(4) . . ?
C34 C35 C29 119.2(4) . . ?
N3 C35 C29 115.0(4) . . ?
N3 C36 C37 125.1(4) . . ?
N3 C36 H36 122(3) . . ?
C37 C36 H36 113(3) . . ?
C42 C37 C38 119.0(4) . . ?
C42 C37 C36 125.7(4) . . ?
C38 C37 C36 115.3(5) . . ?
C39 C38 C37 121.7(6) . . ?
C39 C38 H38 119(3) . . ?
C37 C38 H38 119(3) . . ?
C38 C39 C40 118.8(5) . . ?
C38 C39 H39 119(3) . . ?
C40 C39 H39 122(3) . . ?
C41 C40 C39 120.8(5) . . ?
C41 C40 H40 117(3) . . ?
C39 C40 H40 121(3) . . ?
C40 C41 C42 122.7(5) . . ?
C40 C41 H41 118(4) . . ?
C42 C41 H41 119(4) . . ?
O6 C42 C41 118.2(4) . . ?
O6 C42 C37 124.7(4) . . ?
C41 C42 C37 117.1(4) . . ?
C50 N4 C49 124.0(4) . . ?
C50 N4 Ni4 125.3(3) . . ?
C49 N4 Ni4 110.7(3) . . ?
C43 O7 Ni1 134.4(3) . . ?
C43 O7 Ni4 107.7(3) . . ?
Ni1 O7 Ni4 99.55(12) . . ?
C43 O7 Ni3 115.9(2) . . ?
Ni1 O7 Ni3 92.72(13) . . ?
Ni4 O7 Ni3 101.42(12) . . ?
C56 O8 Ni4 123.8(3) . . ?
O7 C43 C44 123.0(4) . . ?
O7 C43 C49 118.2(4) . . ?
C44 C43 C49 118.8(4) . . ?
C45 C44 C43 120.4(5) . . ?
C45 C44 H44 119.8 . . ?
C43 C44 H44 119.8 . . ?
C44 C45 C46 121.5(5) . . ?
C44 C45 H45 118(3) . . ?
C46 C45 H45 120(3) . . ?
C45 C46 C48 118.2(5) . . ?
C45 C46 C47 120.3(5) . . ?
C48 C46 C47 121.5(5) . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C49 C48 C46 120.2(5) . . ?
C49 C48 H48 117(3) . . ?
C46 C48 H48 122(3) . . ?
C48 C49 C43 120.7(4) . . ?
C48 C49 N4 125.1(4) . . ?
C43 C49 N4 114.2(4) . . ?
N4 C50 C51 124.4(4) . . ?
N4 C50 H50 115(2) . . ?
C51 C50 H50 120(2) . . ?
C56 C51 C52 118.5(5) . . ?
C56 C51 C50 125.8(5) . . ?
C52 C51 C50 115.7(5) . . ?
C53 C52 C51 122.8(6) . . ?
C53 C52 H52 123(3) . . ?
C51 C52 H52 114(3) . . ?
C52 C53 C54 118.8(6) . . ?
C52 C53 H53 119(3) . . ?
C54 C53 H53 122(3) . . ?
C55 C54 C53 120.6(6) . . ?
C55 C54 H54 117(5) . . ?
C53 C54 H54 122(5) . . ?
C54 C55 C56 122.3(6) . . ?
C54 C55 H55 117(5) . . ?
C56 C55 H55 120(5) . . ?
O8 C56 C55 118.2(5) . . ?
O8 C56 C51 124.8(4) . . ?
C55 C56 C51 117.0(5) . . ?
C57 O9 Ni4 132.6(3) . . ?
C57 O9 H9O 109.5 . . ?
Ni4 O9 H9O 110.6 . . ?
O9 C57 C58 115.3(6) . . ?
O9 C57 H57A 108.4 . . ?
C58 C57 H57A 108.4 . . ?
O9 C57 H57B 108.4 . . ?
C58 C57 H57B 108.4 . . ?
H57A C57 H57B 107.5 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C59 O10 Ni1 133.3(3) . . ?
C59 O10 H10O 109.5 . . ?
Ni1 O10 H10O 116.2 . . ?
C60 C59 O10 118.3(7) . . ?
C60 C59 H59A 107.7 . . ?
O10 C59 H59A 107.7 . . ?
C60 C59 H59B 107.7 . . ?
O10 C59 H59B 107.7 . . ?
H59A C59 H59B 107.1 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C61 O11 Ni2 131.0(5) . . ?
C61 O11 H11O 109.5 . . ?
Ni2 O11 H11O 116.8 . . ?
O11 C61 C62 114.7(10) . . ?
O11 C61 C62B 129.6(13) . . ?
C62 C61 C62B 38.9(12) . . ?
O11 C61 C62A 130.6(17) . . ?
C62 C61 C62A 66.8(16) . . ?
C62B C61 C62A 84(2) . . ?
C62B C62 C61 70.7(7) . . ?
C62B C62 C62A 96(2) . . ?
C61 C62 C62A 56.7(8) . . ?
C61 C62A C62 56.5(8) . . ?
C61 C62A C62B 47.8(10) . . ?
C62 C62A C62B 29.5(10) . . ?
C62 C62B C61 70.4(7) . . ?
C62 C62B C62A 54.5(17) . . ?
C61 C62B C62A 47.8(10) . . ?
C63 O12 Ni3 135.1(3) . . ?
C63 O12 H12O 109.5 . . ?
Ni3 O12 H12O 115.4 . . ?
O12 C63 C64 111.1(5) . . ?
O12 C63 H63A 109.4 . . ?
C64 C63 H63A 109.4 . . ?
O12 C63 H63B 109.4 . . ?
C64 C63 H63B 109.4 . . ?
H63A C63 H63B 108.0 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
O1E C1E C2E 114.9(11) . . ?

_diffrn_measured_fraction_theta_max 0.944
_diffrn_reflns_theta_full        64.00
_diffrn_measured_fraction_theta_full 0.944
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.095


# start Validation Reply Form
_vrf_PLAT029_shelxl              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.590
RESPONSE: We have collected data to 2theta=143 deg trying to cover all
possibly accessible reciprocal space, but only those to 2theta=130 deg
were used in the refinement. This alert is due to instrument limitations
for triclinic crystals with small unit cell axis measured with Cu radiation.
;
_vrf_PLAT201_shelxl              
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) 
RESPONSE: The terminal ethanol atom C62 was found disordered over three 
positions and was refined isotropically using the restraint SUMP for the sum 
of the occupation factors which were refined to values 0.57, 0.28 and 0.18 
using free variables.
;
#===END
_database_code_depnum_ccdc_archive 'CCDC 1018616'
#######################################################################
#
#                 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_shelxl

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C68 H72 N8 Ni4 O12'
_chemical_formula_weight         1428.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3987(2)
_cell_length_b                   11.9871(2)
_cell_length_c                   12.9916(2)
_cell_angle_alpha                63.7240(10)
_cell_angle_beta                 82.2820(10)
_cell_angle_gamma                81.8030(10)
_cell_volume                     1570.38(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    18186
_cell_measurement_theta_min      6.73
_cell_measurement_theta_max      71.83

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            red-brown
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             744
_exptl_absorpt_coefficient_mu    1.925
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21294
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         6.73
_diffrn_reflns_theta_max         65.00
_reflns_number_total             5057
_reflns_number_gt                4022
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0583P)²+0.5879P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5057
_refine_ls_number_parameters     491
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0412
_refine_ls_wR_factor_ref         0.1146
_refine_ls_wR_factor_gt          0.1035
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.002
_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
Ni1 Ni 0.45513(4) 0.90416(4) 0.22591(4) 0.02322(16) Uani 1 1 d . . .
Ni2 Ni 0.42440(4) 0.90083(4) -0.00668(4) 0.02190(16) Uani 1 1 d . . .
N1 N 0.26157(19) 0.8455(2) 0.0332(2) 0.0253(6) Uani 1 1 d . . .
O1 O 0.44653(15) 0.78115(17) 0.16017(17) 0.0254(5) Uani 1 1 d . . .
O2 O 0.38197(15) 1.03595(17) -0.15995(17) 0.0244(5) Uani 1 1 d . . .
O3 O 0.40913(14) 1.03321(16) 0.06322(17) 0.0217(5) Uani 1 1 d . . .
C1 C 0.3541(2) 0.7081(3) 0.2043(3) 0.0250(7) Uani 1 1 d . . .
C2 C 0.3537(3) 0.6080(3) 0.3121(3) 0.0297(8) Uani 1 1 d . . .
C3 C 0.2611(3) 0.5327(3) 0.3530(3) 0.0344(8) Uani 1 1 d . . .
C4 C 0.1654(3) 0.5550(3) 0.2874(3) 0.0345(8) Uani 1 1 d . . .
C5 C 0.0659(3) 0.4705(3) 0.3314(3) 0.0502(10) Uani 1 1 d . . .
H5A H 0.0992 0.3838 0.3532 0.055 Uiso 1 1 calc R . .
H5B H 0.0117 0.4951 0.2709 0.055 Uiso 1 1 calc R . .
H5C H 0.0222 0.4778 0.3988 0.055 Uiso 1 1 calc R . .
C6 C 0.1646(3) 0.6562(3) 0.1815(3) 0.0301(8) Uani 1 1 d . . .
C7 C 0.2559(2) 0.7359(3) 0.1389(3) 0.0256(7) Uani 1 1 d . . .
C8 C 0.1723(3) 0.8988(3) -0.0264(3) 0.0312(8) Uani 1 1 d . . .
C9 C 0.1712(2) 1.0123(3) -0.1323(3) 0.0263(7) Uani 1 1 d . . .
C10 C 0.0593(3) 1.0620(3) -0.1759(3) 0.0327(8) Uani 1 1 d . . .
C11 C 0.0428(3) 1.1718(3) -0.2708(3) 0.0364(8) Uani 1 1 d . . .
C12 C 0.1412(3) 1.2378(3) -0.3285(3) 0.0346(8) Uani 1 1 d . . .
C13 C 0.2529(3) 1.1916(3) -0.2900(3) 0.0301(8) Uani 1 1 d . . .
C14 C 0.2722(2) 1.0788(3) -0.1938(3) 0.0239(7) Uani 1 1 d . . .
N2 N 0.28870(19) 0.9550(2) 0.2681(2) 0.0243(6) Uani 1 1 d . . .
O4 O 0.48271(16) 0.80389(18) 0.38457(18) 0.0291(5) Uani 1 1 d . . .
C15 C 0.3040(2) 1.1011(2) 0.0699(3) 0.0220(7) Uani 1 1 d . . .
C16 C 0.2596(3) 1.2037(3) -0.0229(3) 0.0261(7) Uani 1 1 d . . .
C17 C 0.1537(3) 1.2713(3) -0.0099(3) 0.0292(8) Uani 1 1 d . . .
C18 C 0.0909(2) 1.2389(3) 0.0976(3) 0.0281(7) Uani 1 1 d . . .
C19 C -0.0220(3) 1.3148(3) 0.1135(3) 0.0413(9) Uani 1 1 d . . .
H19A H -0.0237 1.3994 0.0507 0.045 Uiso 1 1 d . . .
H19B H -0.0246 1.3192 0.1873 0.045 Uiso 1 1 d . . .
H19C H -0.0910 1.2749 0.1127 0.045 Uiso 1 1 d . . .
C20 C 0.1348(3) 1.1356(3) 0.1908(3) 0.0291(8) Uani 1 1 d . . .
C21 C 0.2380(2) 1.0637(3) 0.1782(3) 0.0235(7) Uani 1 1 d . . .
C22 C 0.2280(2) 0.8934(3) 0.3648(3) 0.0279(7) Uani 1 1 d . . .
C23 C 0.2761(2) 0.7867(3) 0.4604(3) 0.0279(7) Uani 1 1 d . . .
C24 C 0.1964(3) 0.7186(3) 0.5529(3) 0.0362(8) Uani 1 1 d . . .
C25 C 0.2331(3) 0.6157(3) 0.6460(3) 0.0425(9) Uani 1 1 d . . .
C26 C 0.3555(3) 0.5780(4) 0.6526(3) 0.0415(9) Uani 1 1 d . . .
C27 C 0.4360(3) 0.6440(3) 0.5664(3) 0.0316(8) Uani 1 1 d . . .
C28 C 0.4005(2) 0.7479(3) 0.4668(3) 0.0274(7) Uani 1 1 d . . .
O5 O 0.48028(16) 0.76924(17) -0.07145(18) 0.0279(5) Uani 1 1 d . . .
N3 N 0.6072(2) 0.6004(2) -0.0607(2) 0.0335(7) Uani 1 1 d . . .
C29 C 0.5431(3) 0.6728(3) -0.0169(3) 0.0291(8) Uani 1 1 d . . .
C30 C 0.6873(3) 0.4949(3) 0.0076(3) 0.0449(9) Uani 1 1 d . . .
H30A H 0.6734 0.4207 -0.0008 0.049 Uiso 1 1 calc R . .
H30B H 0.6727 0.4790 0.0888 0.049 Uiso 1 1 calc R . .
H30C H 0.7698 0.5140 -0.0191 0.049 Uiso 1 1 calc R . .
C31 C 0.6127(4) 0.6366(4) -0.1831(3) 0.0600(11) Uani 1 1 d . . .
H31A H 0.6097 0.5626 -0.1962 0.066 Uiso 1 1 calc R . .
H31B H 0.6871 0.6743 -0.2199 0.066 Uiso 1 1 calc R . .
H31C H 0.5451 0.6973 -0.2160 0.066 Uiso 1 1 calc R . .
N4 N 0.7432(2) 0.9835(3) 0.4447(3) 0.0419(7) Uani 1 1 d . . .
O6 O 0.9111(2) 0.8810(3) 0.5328(3) 0.0672(8) Uani 1 1 d . . .
C32 C 0.8606(3) 0.9648(4) 0.4549(4) 0.0469(10) Uani 1 1 d . . .
C33 C 0.6652(3) 0.9001(4) 0.5328(4) 0.0704(13) Uani 1 1 d . . .
H33A H 0.6167 0.8668 0.4980 0.077 Uiso 1 1 calc R . .
H33B H 0.6132 0.9457 0.5708 0.077 Uiso 1 1 calc R . .
H33C H 0.7125 0.8311 0.5897 0.077 Uiso 1 1 calc R . .
C34 C 0.6891(3) 1.0877(4) 0.3495(3) 0.0579(11) Uani 1 1 d . . .
H34A H 0.6425 1.0566 0.3113 0.064 Uiso 1 1 calc R . .
H34B H 0.7514 1.1355 0.2944 0.064 Uiso 1 1 calc R . .
H34C H 0.6369 1.1419 0.3783 0.064 Uiso 1 1 calc R . .
H2 H 0.417(2) 0.595(2) 0.353(2) 0.017(7) Uiso 1 1 d . . .
H3 H 0.261(2) 0.467(2) 0.424(2) 0.014(7) Uiso 1 1 d . . .
H6 H 0.098(2) 0.675(2) 0.139(2) 0.026(8) Uiso 1 1 d . . .
H8 H 0.100(3) 0.863(3) 0.002(2) 0.032(8) Uiso 1 1 d . . .
H10 H -0.002(3) 1.019(3) -0.137(3) 0.036(9) Uiso 1 1 d . . .
H11 H -0.037(3) 1.200(3) -0.296(3) 0.043(9) Uiso 1 1 d . . .
H12 H 0.131(3) 1.320(3) -0.395(3) 0.033(9) Uiso 1 1 d . . .
H13 H 0.316(3) 1.238(3) -0.333(3) 0.050(10) Uiso 1 1 d . . .
H16 H 0.300(2) 1.231(2) -0.093(2) 0.016(7) Uiso 1 1 d . . .
H17 H 0.126(3) 1.336(3) -0.073(3) 0.027(9) Uiso 1 1 d . . .
H20 H 0.097(3) 1.117(3) 0.258(3) 0.029(9) Uiso 1 1 d . . .
H22 H 0.137(2) 0.919(2) 0.379(2) 0.028(8) Uiso 1 1 d . . .
H24 H 0.120(3) 0.741(3) 0.552(3) 0.032(9) Uiso 1 1 d . . .
H25 H 0.184(3) 0.565(3) 0.711(3) 0.068(12) Uiso 1 1 d . . .
H26 H 0.379(3) 0.504(3) 0.713(3) 0.038(10) Uiso 1 1 d . . .
H27 H 0.523(3) 0.624(3) 0.568(2) 0.034(8) Uiso 1 1 d . . .
H29 H 0.544(2) 0.643(2) 0.061(2) 0.019 Uiso 1 1 d . . .
H32 H 0.904(3) 1.027(4) 0.388(3) 0.067(13) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O4 1.914(2) . ?
Ni1 N2 1.989(2) . ?
Ni1 O1 2.0229(18) . ?
Ni1 O2 2.0263(18) 2_675 ?
Ni1 O3 2.075(2) . ?
Ni2 N1 1.985(2) . ?
Ni2 O2 2.001(2) . ?
Ni2 O1 2.027(2) . ?
Ni2 O3 2.0747(17) 2_675 ?
Ni2 O5 2.0848(18) . ?
Ni2 O3 2.1279(17) . ?
N1 C8 1.277(4) . ?
N1 C7 1.421(4) . ?
O1 C1 1.364(3) . ?
O2 C14 1.337(3) . ?
O2 Ni1 2.0263(18) 2_675 ?
O3 C15 1.365(3) . ?
O3 Ni2 2.0747(17) 2_675 ?
C1 C2 1.383(4) . ?
C1 C7 1.408(4) . ?
C2 C3 1.381(4) . ?
C2 H2 0.90(3) . ?
C3 C4 1.398(4) . ?
C3 H3 0.92(3) . ?
C4 C6 1.373(4) . ?
C4 C5 1.510(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.401(4) . ?
C6 H6 0.94(3) . ?
C8 C9 1.444(4) . ?
C8 H8 0.93(3) . ?
C9 C10 1.408(4) . ?
C9 C14 1.432(4) . ?
C10 C11 1.357(5) . ?
C10 H10 0.89(3) . ?
C11 C12 1.396(4) . ?
C11 H11 0.97(3) . ?
C12 C13 1.379(4) . ?
C12 H12 0.98(3) . ?
C13 C14 1.389(4) . ?
C13 H13 0.93(3) . ?
N2 C22 1.301(4) . ?
N2 C21 1.420(4) . ?
O4 C28 1.321(3) . ?
C15 C16 1.377(4) . ?
C15 C21 1.413(4) . ?
C16 C17 1.389(4) . ?
C16 H16 0.90(3) . ?
C17 C18 1.395(4) . ?
C17 H17 0.90(3) . ?
C18 C20 1.381(4) . ?
C18 C19 1.512(4) . ?
C19 H19A 0.9804 . ?
C19 H19B 0.9786 . ?
C19 H19C 0.9811 . ?
C20 C21 1.393(4) . ?
C20 H20 0.87(3) . ?
C22 C23 1.434(4) . ?
C22 H22 1.05(3) . ?
C23 C24 1.409(4) . ?
C23 C28 1.430(4) . ?
C24 C25 1.351(5) . ?
C24 H24 0.88(3) . ?
C25 C26 1.406(5) . ?
C25 H25 0.95(4) . ?
C26 C27 1.366(4) . ?
C26 H26 0.92(3) . ?
C27 C28 1.400(4) . ?
C27 H27 0.99(3) . ?
O5 C29 1.236(3) . ?
N3 C29 1.324(4) . ?
N3 C31 1.446(4) . ?
N3 C30 1.454(4) . ?
C29 H29 0.91(3) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
N4 C32 1.339(4) . ?
N4 C33 1.438(4) . ?
N4 C34 1.445(4) . ?
O6 C32 1.207(5) . ?
C32 H32 0.98(4) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?

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
O4 Ni1 N2 91.26(9) . . ?
O4 Ni1 O1 105.31(8) . . ?
N2 Ni1 O1 106.88(8) . . ?
O4 Ni1 O2 101.04(8) . 2_675 ?
N2 Ni1 O2 144.70(8) . 2_675 ?
O1 Ni1 O2 101.58(7) . 2_675 ?
O4 Ni1 O3 170.62(7) . . ?
N2 Ni1 O3 81.37(9) . . ?
O1 Ni1 O3 82.51(7) . . ?
O2 Ni1 O3 82.09(7) 2_675 . ?
N1 Ni2 O2 92.47(9) . . ?
N1 Ni2 O1 83.25(9) . . ?
O2 Ni2 O1 169.97(7) . . ?
N1 Ni2 O3 174.97(9) . 2_675 ?
O2 Ni2 O3 82.72(7) . 2_675 ?
O1 Ni2 O3 101.73(7) . 2_675 ?
N1 Ni2 O5 91.04(8) . . ?
O2 Ni2 O5 93.57(8) . . ?
O1 Ni2 O5 95.56(8) . . ?
O3 Ni2 O5 87.80(7) 2_675 . ?
N1 Ni2 O3 100.97(8) . . ?
O2 Ni2 O3 90.86(7) . . ?
O1 Ni2 O3 81.11(7) . . ?
O3 Ni2 O3 80.65(7) 2_675 . ?
O5 Ni2 O3 167.01(7) . . ?
C8 N1 C7 123.2(2) . . ?
C8 N1 Ni2 125.9(2) . . ?
C7 N1 Ni2 110.85(17) . . ?
C1 O1 Ni1 115.96(16) . . ?
C1 O1 Ni2 109.55(18) . . ?
Ni1 O1 Ni2 100.16(8) . . ?
C14 O2 Ni2 126.31(18) . . ?
C14 O2 Ni1 133.65(18) . 2_675 ?
Ni2 O2 Ni1 99.40(8) . 2_675 ?
C15 O3 Ni2 126.97(15) . 2_675 ?
C15 O3 Ni1 110.90(17) . . ?
Ni2 O3 Ni1 95.47(7) 2_675 . ?
C15 O3 Ni2 121.75(15) . . ?
Ni2 O3 Ni2 99.35(7) 2_675 . ?
Ni1 O3 Ni2 95.30(7) . . ?
O1 C1 C2 121.8(3) . . ?
O1 C1 C7 119.2(3) . . ?
C2 C1 C7 119.0(3) . . ?
C3 C2 C1 120.6(3) . . ?
C3 C2 H2 122.7(17) . . ?
C1 C2 H2 116.7(17) . . ?
C2 C3 C4 121.3(3) . . ?
C2 C3 H3 120.3(17) . . ?
C4 C3 H3 118.4(16) . . ?
C6 C4 C3 118.0(3) . . ?
C6 C4 C5 121.0(3) . . ?
C3 C4 C5 121.0(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 C7 122.0(3) . . ?
C4 C6 H6 118.4(17) . . ?
C7 C6 H6 119.5(17) . . ?
C6 C7 C1 119.0(3) . . ?
C6 C7 N1 126.6(3) . . ?
C1 C7 N1 114.4(2) . . ?
N1 C8 C9 126.0(3) . . ?
N1 C8 H8 117.6(18) . . ?
C9 C8 H8 116.4(18) . . ?
C10 C9 C14 118.1(3) . . ?
C10 C9 C8 116.0(3) . . ?
C14 C9 C8 125.9(3) . . ?
C11 C10 C9 122.9(3) . . ?
C11 C10 H10 120(2) . . ?
C9 C10 H10 117(2) . . ?
C10 C11 C12 118.6(3) . . ?
C10 C11 H11 118.3(19) . . ?
C12 C11 H11 123.1(19) . . ?
C13 C12 C11 120.5(3) . . ?
C13 C12 H12 119.2(17) . . ?
C11 C12 H12 120.3(17) . . ?
C12 C13 C14 121.9(3) . . ?
C12 C13 H13 117(2) . . ?
C14 C13 H13 121(2) . . ?
O2 C14 C13 120.3(2) . . ?
O2 C14 C9 121.8(3) . . ?
C13 C14 C9 117.9(3) . . ?
C22 N2 C21 122.0(2) . . ?
C22 N2 Ni1 124.9(2) . . ?
C21 N2 Ni1 112.97(17) . . ?
C28 O4 Ni1 124.97(19) . . ?
O3 C15 C16 123.4(3) . . ?
O3 C15 C21 117.9(3) . . ?
C16 C15 C21 118.7(2) . . ?
C15 C16 C17 120.7(3) . . ?
C15 C16 H16 121.1(17) . . ?
C17 C16 H16 118.2(18) . . ?
C16 C17 C18 121.1(3) . . ?
C16 C17 H17 118.5(19) . . ?
C18 C17 H17 120.4(19) . . ?
C20 C18 C17 118.4(3) . . ?
C20 C18 C19 120.1(3) . . ?
C17 C18 C19 121.5(3) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.6 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.4 . . ?
H19A C19 H19C 109.3 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 C21 121.2(3) . . ?
C18 C20 H20 118(2) . . ?
C21 C20 H20 121(2) . . ?
C20 C21 C15 119.8(3) . . ?
C20 C21 N2 125.3(3) . . ?
C15 C21 N2 114.9(2) . . ?
N2 C22 C23 124.4(3) . . ?
N2 C22 H22 121.5(15) . . ?
C23 C22 H22 114.1(15) . . ?
C24 C23 C28 118.9(3) . . ?
C24 C23 C22 118.0(3) . . ?
C28 C23 C22 123.1(3) . . ?
C25 C24 C23 122.3(3) . . ?
C25 C24 H24 117(2) . . ?
C23 C24 H24 121(2) . . ?
C24 C25 C26 118.8(3) . . ?
C24 C25 H25 127(2) . . ?
C26 C25 H25 115(2) . . ?
C27 C26 C25 120.7(4) . . ?
C27 C26 H26 121(2) . . ?
C25 C26 H26 118(2) . . ?
C26 C27 C28 121.9(3) . . ?
C26 C27 H27 124.0(17) . . ?
C28 C27 H27 114.0(17) . . ?
O4 C28 C27 118.8(3) . . ?
O4 C28 C23 123.9(3) . . ?
C27 C28 C23 117.3(3) . . ?
C29 O5 Ni2 121.16(19) . . ?
C29 N3 C31 119.8(3) . . ?
C29 N3 C30 121.6(3) . . ?
C31 N3 C30 117.9(3) . . ?
O5 C29 N3 125.4(3) . . ?
O5 C29 H29 120.1(17) . . ?
N3 C29 H29 114.4(17) . . ?
N3 C30 H30A 109.5 . . ?
N3 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N3 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N3 C31 H31A 109.5 . . ?
N3 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N3 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C32 N4 C33 119.9(4) . . ?
C32 N4 C34 122.8(3) . . ?
C33 N4 C34 117.3(3) . . ?
O6 C32 N4 126.1(4) . . ?
O6 C32 H32 122(2) . . ?
N4 C32 H32 112(2) . . ?
N4 C33 H33A 109.5 . . ?
N4 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N4 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N4 C34 H34A 109.5 . . ?
N4 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N4 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.945
_diffrn_reflns_theta_full        65.00
_diffrn_measured_fraction_theta_full 0.945
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.069

# start Validation Reply Form
_vrf_PLAT029_shelxl              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.590
RESPONSE: We have collected data to 2theta=143 deg trying to cover all
possibly accessible reciprocal space, but only those to 2theta=130 deg
were used in the refinement. This alert is due to instrument limitations
for triclinic crystals with small unit cell axis measured with Cu radiation.
;
#===END

_database_code_depnum_ccdc_archive 'CCDC 1018617'
#######################################################################
#
#                 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_shelxl

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C76 H92 Cl4 N4 Ni4 O22'
_chemical_formula_weight         1790.18

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.0498(6)
_cell_length_b                   11.4157(6)
_cell_length_c                   17.5861(10)
_cell_angle_alpha                99.067(2)
_cell_angle_beta                 94.192(3)
_cell_angle_gamma                113.463(2)
_cell_volume                     1986.76(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9833
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      32.98

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            olive-green
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             932
_exptl_absorpt_coefficient_mu    1.143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.669
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_process_details   Bruker-SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            52633
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6987
_reflns_number_gt                6410
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'

_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0230P)²+3.3225P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6987
_refine_ls_number_parameters     620
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_ref         0.0752
_refine_ls_wR_factor_gt          0.0732
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.48281(3) 0.42790(3) 0.204270(16) 0.01307(8) Uani 1 1 d . . .
Ni2 Ni 0.54631(3) 0.59274(3) 0.082592(16) 0.01068(8) Uani 1 1 d . . .
N1 N 0.4571(2) 0.54467(19) 0.29594(11) 0.0161(4) Uani 1 1 d . . .
O1 O 0.37472(15) 0.47882(15) 0.12590(9) 0.0134(3) Uani 1 1 d . . .
O2 O 0.57795(17) 0.36312(17) 0.27816(9) 0.0205(4) Uani 1 1 d . . .
O3 O 0.5843(2) 0.29245(18) 0.38779(10) 0.0288(4) Uani 1 1 d . . .
N11 N 0.54631(19) 0.76648(18) 0.12481(11) 0.0130(4) Uani 1 1 d . . .
O11 O 0.64356(15) 0.58611(15) 0.17929(9) 0.0145(3) Uani 1 1 d . . .
O12 O 0.45077(15) 0.57760(15) -0.02389(9) 0.0117(3) Uani 1 1 d . . .
O13 O 0.48676(16) 0.69659(15) -0.11604(9) 0.0154(3) Uani 1 1 d . . .
O21 O 0.31236(18) 0.26646(18) 0.21742(10) 0.0212(4) Uani 1 1 d . . .
O22 O 0.71766(16) 0.68812(16) 0.02998(10) 0.0154(3) Uani 1 1 d . . .
C1 C 0.2871(2) 0.5289(2) 0.14508(14) 0.0147(5) Uani 1 1 d . . .
C2 C 0.2048(2) 0.5424(2) 0.08552(15) 0.0176(5) Uani 1 1 d . . .
C3 C 0.1099(3) 0.5896(3) 0.10123(16) 0.0237(6) Uani 1 1 d . . .
C4 C 0.0935(3) 0.6269(3) 0.17764(16) 0.0285(6) Uani 1 1 d . . .
C5 C 0.1753(3) 0.6180(3) 0.23689(16) 0.0252(6) Uani 1 1 d . . .
C6 C 0.2727(2) 0.5698(2) 0.22323(14) 0.0179(5) Uani 1 1 d . . .
C7 C 0.3589(2) 0.5786(2) 0.29267(14) 0.0189(5) Uani 1 1 d . . .
C8 C 0.5411(2) 0.5859(2) 0.36966(14) 0.0180(5) Uani 1 1 d . . .
C9 C 0.5714(3) 0.7099(3) 0.41411(15) 0.0231(6) Uani 1 1 d . . .
C10 C 0.6498(3) 0.7532(3) 0.48626(16) 0.0270(6) Uani 1 1 d . . .
C11 C 0.6987(3) 0.6719(3) 0.51469(15) 0.0260(6) Uani 1 1 d . . .
C12 C 0.6734(3) 0.5510(3) 0.47152(15) 0.0233(6) Uani 1 1 d . . .
C13 C 0.5971(2) 0.5073(2) 0.39770(14) 0.0192(5) Uani 1 1 d . . .
C14 C 0.5837(2) 0.3784(2) 0.35173(14) 0.0206(5) Uani 1 1 d . . .
Cl1 Cl 0.79371(9) 0.72298(8) 0.60681(4) 0.0436(2) Uani 1 1 d . . .
C21 C 0.7215(2) 0.6909(2) 0.23259(13) 0.0153(5) Uani 1 1 d . . .
C22 C 0.8151(2) 0.6807(3) 0.28739(15) 0.0213(5) Uani 1 1 d . . .
C23 C 0.9000(3) 0.7863(3) 0.34306(16) 0.0294(6) Uani 1 1 d . . .
C24 C 0.8960(3) 0.9079(3) 0.34821(17) 0.0308(6) Uani 1 1 d . . .
C25 C 0.8057(3) 0.9206(3) 0.29579(15) 0.0234(6) Uani 1 1 d . . .
C26 C 0.7173(2) 0.8146(2) 0.23712(14) 0.0176(5) Uani 1 1 d . . .
C27 C 0.6301(2) 0.8445(2) 0.18542(14) 0.0162(5) Uani 1 1 d . . .
C28 C 0.4665(2) 0.8162(2) 0.08390(13) 0.0139(5) Uani 1 1 d . . .
C29 C 0.4231(2) 0.9038(2) 0.12499(15) 0.0184(5) Uani 1 1 d . . .
C30 C 0.3505(2) 0.9574(2) 0.08684(15) 0.0195(5) Uani 1 1 d . . .
C31 C 0.3207(2) 0.9239(2) 0.00655(15) 0.0176(5) Uani 1 1 d . . .
C32 C 0.3616(2) 0.8377(2) -0.03616(15) 0.0156(5) Uani 1 1 d . . .
C33 C 0.4322(2) 0.7802(2) 0.00192(13) 0.0131(5) Uani 1 1 d . . .
C34 C 0.4618(2) 0.6801(2) -0.05008(13) 0.0127(5) Uani 1 1 d . . .
Cl2 Cl 0.23205(6) 0.99385(6) -0.04200(4) 0.02282(14) Uani 1 1 d . . .
C41 C 0.1938(3) 0.2020(3) 0.16214(18) 0.0302(6) Uani 1 1 d . . .
C42 C 0.0918(3) 0.0868(3) 0.1867(2) 0.0393(8) Uani 1 1 d . . .
C43 C 0.8497(2) 0.7230(3) 0.06958(15) 0.0198(5) Uani 1 1 d . . .
C44 C 0.9573(3) 0.7895(3) 0.02347(17) 0.0240(6) Uani 1 1 d . . .
O23 O 0.7070(2) 0.1876(2) 0.22978(14) 0.0411(5) Uani 1 1 d . . .
C45 C 0.8355(4) 0.2916(4) 0.2315(3) 0.0715(13) Uani 1 1 d . . .
H45A H 0.8855 0.2585 0.1961 0.100 Uiso 1 1 calc R . .
H45B H 0.8220 0.3620 0.2108 0.100 Uiso 1 1 calc R . .
C46 C 0.9141(5) 0.3455(6) 0.3050(3) 0.108(2) Uani 1 1 d . . .
H46A H 0.9166 0.2753 0.3299 0.162 Uiso 1 1 calc R . .
H46B H 0.8758 0.3959 0.3374 0.162 Uiso 1 1 calc R . .
H46C H 1.0050 0.4030 0.2992 0.162 Uiso 1 1 calc R . .
O24 O 0.7115(3) 0.2935(3) 0.53204(14) 0.0477(6) Uani 1 1 d . . .
C47 C 0.8406(5) 0.3028(5) 0.5141(2) 0.0700(13) Uani 1 1 d . . .
H47A H 0.9043 0.3310 0.5629 0.098 Uiso 1 1 calc R . .
H47B H 0.8756 0.3688 0.4816 0.098 Uiso 1 1 calc R . .
C48 C 0.8290(6) 0.1773(6) 0.4727(3) 0.0936(17) Uani 1 1 d . . .
H48A H 0.7630 0.1477 0.4256 0.140 Uiso 1 1 calc R . .
H48B H 0.8005 0.1136 0.5064 0.140 Uiso 1 1 calc R . .
H48C H 0.9157 0.1859 0.4583 0.140 Uiso 1 1 calc R . .
O25 O 0.3878(2) 0.09004(19) 0.27731(12) 0.0310(5) Uani 1 1 d . . .
C49 C 0.3165(3) -0.0127(3) 0.31516(18) 0.0355(7) Uani 1 1 d . . .
H49A H 0.2528 -0.0886 0.2758 0.050 Uiso 1 1 calc R . .
H49B H 0.2647 0.0165 0.3513 0.050 Uiso 1 1 calc R . .
C50 C 0.4105(4) -0.0532(4) 0.3602(2) 0.0510(9) Uani 1 1 d . . .
H50A H 0.3585 -0.1275 0.3829 0.076 Uiso 1 1 calc R . .
H50B H 0.4689 0.0199 0.4019 0.076 Uiso 1 1 calc R . .
H50C H 0.4647 -0.0783 0.3249 0.076 Uiso 1 1 calc R . .
H2 H 0.218(2) 0.525(2) 0.0354(15) 0.009(6) Uiso 1 1 d . . .
H3 H 0.056(3) 0.596(3) 0.0593(16) 0.021(7) Uiso 1 1 d . . .
H4 H 0.027(3) 0.663(3) 0.1892(18) 0.035(8) Uiso 1 1 d . . .
H5 H 0.168(3) 0.646(3) 0.2918(18) 0.030(8) Uiso 1 1 d . . .
H7 H 0.341(2) 0.615(2) 0.3401(16) 0.015(6) Uiso 1 1 d . . .
H9 H 0.540(3) 0.765(3) 0.3938(16) 0.025(7) Uiso 1 1 d . . .
H10 H 0.668(3) 0.837(3) 0.5160(17) 0.026(7) Uiso 1 1 d . . .
H12 H 0.706(3) 0.496(3) 0.4905(17) 0.027(8) Uiso 1 1 d . . .
H22 H 0.816(3) 0.600(3) 0.2842(16) 0.023(7) Uiso 1 1 d . . .
H23 H 0.958(3) 0.775(3) 0.3779(18) 0.028(8) Uiso 1 1 d . . .
H24 H 0.952(3) 0.979(3) 0.3862(19) 0.037(9) Uiso 1 1 d . . .
H25 H 0.800(3) 0.998(3) 0.2977(15) 0.016(7) Uiso 1 1 d . . .
H27 H 0.641(2) 0.933(3) 0.1982(14) 0.010(6) Uiso 1 1 d . . .
H29 H 0.443(3) 0.926(3) 0.1796(18) 0.026(7) Uiso 1 1 d . . .
H30 H 0.323(3) 1.015(3) 0.1147(16) 0.019(7) Uiso 1 1 d . . .
H32 H 0.345(2) 0.819(2) -0.0866(16) 0.013(6) Uiso 1 1 d . . .
H21O H 0.331(4) 0.214(4) 0.232(2) 0.045(11) Uiso 1 1 d . . .
H22O H 0.710(3) 0.651(3) -0.0121(18) 0.018(8) Uiso 1 1 d . . .
H23O H 0.662(4) 0.223(4) 0.248(2) 0.067(14) Uiso 1 1 d . . .
H24O H 0.653(5) 0.276(5) 0.483(3) 0.114(19) Uiso 1 1 d . . .
H25O H 0.455(4) 0.144(4) 0.312(2) 0.049(11) Uiso 1 1 d . . .
H41A H 0.158(3) 0.261(3) 0.1604(16) 0.025(8) Uiso 1 1 d . . .
H41B H 0.219(3) 0.176(3) 0.108(2) 0.043(9) Uiso 1 1 d . . .
H42A H 0.014(4) 0.050(4) 0.150(2) 0.056(11) Uiso 1 1 d . . .
H42B H 0.127(4) 0.022(4) 0.194(2) 0.071(13) Uiso 1 1 d . . .
H42C H 0.069(4) 0.111(4) 0.233(2) 0.050(11) Uiso 1 1 d . . .
H43A H 0.858(3) 0.781(3) 0.1166(17) 0.025(7) Uiso 1 1 d . . .
H43B H 0.855(3) 0.645(3) 0.0825(15) 0.018(7) Uiso 1 1 d . . .
H44A H 0.950(3) 0.730(3) -0.0263(18) 0.030(8) Uiso 1 1 d . . .
H44B H 0.949(3) 0.865(3) 0.0095(18) 0.038(9) Uiso 1 1 d . . .
H44C H 1.043(3) 0.819(3) 0.0556(18) 0.037(9) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2 2.0156(17) . ?
Ni1 N1 2.0365(19) . ?
Ni1 O1 2.0563(16) . ?
Ni1 O13 2.0741(16) 2_665 ?
Ni1 O11 2.1022(16) . ?
Ni1 O21 2.1051(18) . ?
Ni2 O11 1.9726(16) . ?
Ni2 N11 2.0051(19) . ?
Ni2 O12 2.0284(15) . ?
Ni2 O12 2.0665(15) 2_665 ?
Ni2 O1 2.1039(16) . ?
Ni2 O22 2.1351(17) . ?
N1 C7 1.290(3) . ?
N1 C8 1.431(3) . ?
O1 C1 1.344(3) . ?
O2 C14 1.271(3) . ?
O3 C14 1.251(3) . ?
N11 C27 1.298(3) . ?
N11 C28 1.432(3) . ?
O11 C21 1.326(3) . ?
O12 C34 1.289(3) . ?
O12 Ni2 2.0665(15) 2_665 ?
O13 C34 1.238(3) . ?
O13 Ni1 2.0741(16) 2_665 ?
O21 C41 1.423(3) . ?
O21 H21O 0.78(4) . ?
O22 C43 1.440(3) . ?
O22 H22O 0.77(3) . ?
C1 C2 1.404(3) . ?
C1 C6 1.422(3) . ?
C2 C3 1.382(4) . ?
C2 H2 0.91(3) . ?
C3 C4 1.392(4) . ?
C3 H3 0.95(3) . ?
C4 C5 1.372(4) . ?
C4 H4 0.99(3) . ?
C5 C6 1.409(3) . ?
C5 H5 0.99(3) . ?
C6 C7 1.457(3) . ?
C7 H7 0.95(3) . ?
C8 C9 1.401(4) . ?
C8 C13 1.403(3) . ?
C9 C10 1.380(4) . ?
C9 H9 0.94(3) . ?
C10 C11 1.382(4) . ?
C10 H10 0.95(3) . ?
C11 C12 1.376(4) . ?
C11 Cl1 1.741(3) . ?
C12 C13 1.395(4) . ?
C12 H12 0.93(3) . ?
C13 C14 1.509(3) . ?
C21 C22 1.413(3) . ?
C21 C26 1.421(3) . ?
C22 C23 1.373(4) . ?
C22 H22 0.92(3) . ?
C23 C24 1.395(4) . ?
C23 H23 0.91(3) . ?
C24 C25 1.375(4) . ?
C24 H24 0.92(3) . ?
C25 C26 1.415(3) . ?
C25 H25 0.90(3) . ?
C26 C27 1.450(3) . ?
C27 H27 0.95(3) . ?
C28 C29 1.399(3) . ?
C28 C33 1.414(3) . ?
C29 C30 1.382(4) . ?
C29 H29 0.94(3) . ?
C30 C31 1.382(4) . ?
C30 H30 0.92(3) . ?
C31 C32 1.381(3) . ?
C31 Cl2 1.744(2) . ?
C32 C33 1.399(3) . ?
C32 H32 0.87(3) . ?
C33 C34 1.503(3) . ?
C41 C42 1.502(4) . ?
C41 H41A 0.91(3) . ?
C41 H41B 1.04(3) . ?
C42 H42A 0.94(4) . ?
C42 H42B 0.97(4) . ?
C42 H42C 0.91(4) . ?
C43 C44 1.504(4) . ?
C43 H43A 0.95(3) . ?
C43 H43B 0.97(3) . ?
C44 H44A 1.00(3) . ?
C44 H44B 0.97(3) . ?
C44 H44C 0.97(3) . ?
O23 C45 1.438(5) . ?
O23 H23O 0.81(4) . ?
C45 C46 1.401(6) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
O24 C47 1.450(5) . ?
O24 H24O 0.98(5) . ?
C47 C48 1.452(6) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
O25 C49 1.423(3) . ?
O25 H25O 0.86(4) . ?
C49 C50 1.516(5) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?

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
O2 Ni1 N1 90.18(7) . . ?
O2 Ni1 O1 175.42(7) . . ?
N1 Ni1 O1 92.11(7) . . ?
O2 Ni1 O13 86.16(6) . 2_665 ?
N1 Ni1 O13 176.30(7) . 2_665 ?
O1 Ni1 O13 91.49(6) . 2_665 ?
O2 Ni1 O11 101.27(7) . . ?
N1 Ni1 O11 91.72(7) . . ?
O1 Ni1 O11 82.63(6) . . ?
O13 Ni1 O11 89.59(6) 2_665 . ?
O2 Ni1 O21 83.70(7) . . ?
N1 Ni1 O21 91.49(8) . . ?
O1 Ni1 O21 92.28(7) . . ?
O13 Ni1 O21 87.50(7) 2_665 . ?
O11 Ni1 O21 174.08(7) . . ?
O11 Ni2 N11 94.60(7) . . ?
O11 Ni2 O12 171.92(6) . . ?
N11 Ni2 O12 93.34(7) . . ?
O11 Ni2 O12 92.18(6) . 2_665 ?
N11 Ni2 O12 171.70(7) . 2_665 ?
O12 Ni2 O12 79.79(6) . 2_665 ?
O11 Ni2 O1 84.62(6) . . ?
N11 Ni2 O1 96.80(7) . . ?
O12 Ni2 O1 95.93(6) . . ?
O12 Ni2 O1 88.59(6) 2_665 . ?
O11 Ni2 O22 96.76(7) . . ?
N11 Ni2 O22 89.51(7) . . ?
O12 Ni2 O22 81.80(6) . . ?
O12 Ni2 O22 84.93(6) 2_665 . ?
O1 Ni2 O22 173.42(6) . . ?
C7 N1 C8 115.9(2) . . ?
C7 N1 Ni1 122.00(17) . . ?
C8 N1 Ni1 121.92(15) . . ?
C1 O1 Ni1 124.00(14) . . ?
C1 O1 Ni2 119.24(14) . . ?
Ni1 O1 Ni2 92.62(6) . . ?
C14 O2 Ni1 127.91(16) . . ?
C27 N11 C28 117.2(2) . . ?
C27 N11 Ni2 120.96(16) . . ?
C28 N11 Ni2 121.35(15) . . ?
C21 O11 Ni2 123.74(15) . . ?
C21 O11 Ni1 123.41(14) . . ?
Ni2 O11 Ni1 95.11(6) . . ?
C34 O12 Ni2 120.99(14) . . ?
C34 O12 Ni2 128.50(14) . 2_665 ?
Ni2 O12 Ni2 100.21(6) . 2_665 ?
C34 O13 Ni1 128.65(15) . 2_665 ?
C41 O21 Ni1 125.02(16) . . ?
C41 O21 H21O 108(3) . . ?
Ni1 O21 H21O 112(3) . . ?
C43 O22 Ni2 120.50(15) . . ?
C43 O22 H22O 109(2) . . ?
Ni2 O22 H22O 111(2) . . ?
O1 C1 C2 119.1(2) . . ?
O1 C1 C6 123.4(2) . . ?
C2 C1 C6 117.5(2) . . ?
C3 C2 C1 121.9(2) . . ?
C3 C2 H2 118.9(15) . . ?
C1 C2 H2 119.0(15) . . ?
C2 C3 C4 120.7(2) . . ?
C2 C3 H3 119.1(16) . . ?
C4 C3 H3 120.2(16) . . ?
C5 C4 C3 118.4(2) . . ?
C5 C4 H4 120.6(18) . . ?
C3 C4 H4 121.0(18) . . ?
C4 C5 C6 122.6(2) . . ?
C4 C5 H5 120.7(17) . . ?
C6 C5 H5 116.7(17) . . ?
C5 C6 C1 118.9(2) . . ?
C5 C6 C7 115.1(2) . . ?
C1 C6 C7 125.7(2) . . ?
N1 C7 C6 127.4(2) . . ?
N1 C7 H7 117.5(16) . . ?
C6 C7 H7 115.1(16) . . ?
C9 C8 C13 119.0(2) . . ?
C9 C8 N1 119.0(2) . . ?
C13 C8 N1 121.9(2) . . ?
C10 C9 C8 121.2(3) . . ?
C10 C9 H9 119.5(18) . . ?
C8 C9 H9 119.2(18) . . ?
C9 C10 C11 119.0(3) . . ?
C9 C10 H10 120.2(18) . . ?
C11 C10 H10 120.8(18) . . ?
C12 C11 C10 121.1(2) . . ?
C12 C11 Cl1 119.3(2) . . ?
C10 C11 Cl1 119.6(2) . . ?
C11 C12 C13 120.5(2) . . ?
C11 C12 H12 121.5(18) . . ?
C13 C12 H12 118.0(18) . . ?
C12 C13 C8 119.0(2) . . ?
C12 C13 C14 117.0(2) . . ?
C8 C13 C14 124.0(2) . . ?
O3 C14 O2 122.4(2) . . ?
O3 C14 C13 118.7(2) . . ?
O2 C14 C13 118.8(2) . . ?
O11 C21 C22 118.9(2) . . ?
O11 C21 C26 123.3(2) . . ?
C22 C21 C26 117.7(2) . . ?
C23 C22 C21 121.6(3) . . ?
C23 C22 H22 121.6(18) . . ?
C21 C22 H22 116.9(18) . . ?
C22 C23 C24 121.1(3) . . ?
C22 C23 H23 118.8(19) . . ?
C24 C23 H23 120.0(19) . . ?
C25 C24 C23 118.6(3) . . ?
C25 C24 H24 120(2) . . ?
C23 C24 H24 121(2) . . ?
C24 C25 C26 122.1(3) . . ?
C24 C25 H25 120.8(17) . . ?
C26 C25 H25 117.1(17) . . ?
C25 C26 C21 118.9(2) . . ?
C25 C26 C27 115.4(2) . . ?
C21 C26 C27 125.7(2) . . ?
N11 C27 C26 127.0(2) . . ?
N11 C27 H27 119.6(15) . . ?
C26 C27 H27 113.3(15) . . ?
C29 C28 C33 118.8(2) . . ?
C29 C28 N11 119.9(2) . . ?
C33 C28 N11 121.2(2) . . ?
C30 C29 C28 121.3(2) . . ?
C30 C29 H29 119.3(18) . . ?
C28 C29 H29 119.5(18) . . ?
C29 C30 C31 119.3(2) . . ?
C29 C30 H30 120.3(17) . . ?
C31 C30 H30 120.4(17) . . ?
C32 C31 C30 121.3(2) . . ?
C32 C31 Cl2 119.29(19) . . ?
C30 C31 Cl2 119.44(18) . . ?
C31 C32 C33 120.0(2) . . ?
C31 C32 H32 121.2(17) . . ?
C33 C32 H32 118.8(17) . . ?
C32 C33 C28 119.3(2) . . ?
C32 C33 C34 115.2(2) . . ?
C28 C33 C34 125.5(2) . . ?
O13 C34 O12 124.2(2) . . ?
O13 C34 C33 119.0(2) . . ?
O12 C34 C33 116.63(19) . . ?
O21 C41 C42 112.5(2) . . ?
O21 C41 H41A 106.0(18) . . ?
C42 C41 H41A 107.0(18) . . ?
O21 C41 H41B 108.8(18) . . ?
C42 C41 H41B 111.8(18) . . ?
H41A C41 H41B 110(3) . . ?
C41 C42 H42A 110(2) . . ?
C41 C42 H42B 111(2) . . ?
H42A C42 H42B 111(3) . . ?
C41 C42 H42C 111(2) . . ?
H42A C42 H42C 108(3) . . ?
H42B C42 H42C 106(3) . . ?
O22 C43 C44 112.7(2) . . ?
O22 C43 H43A 105.3(17) . . ?
C44 C43 H43A 109.5(17) . . ?
O22 C43 H43B 109.0(16) . . ?
C44 C43 H43B 111.6(16) . . ?
H43A C43 H43B 108(2) . . ?
C43 C44 H44A 110.6(17) . . ?
C43 C44 H44B 110.7(19) . . ?
H44A C44 H44B 107(3) . . ?
C43 C44 H44C 108.2(19) . . ?
H44A C44 H44C 112(2) . . ?
H44B C44 H44C 108(3) . . ?
C45 O23 H23O 105(3) . . ?
C46 C45 O23 115.4(4) . . ?
C46 C45 H45A 108.4 . . ?
O23 C45 H45A 108.4 . . ?
C46 C45 H45B 108.4 . . ?
O23 C45 H45B 108.4 . . ?
H45A C45 H45B 107.5 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C47 O24 H24O 109(3) . . ?
O24 C47 C48 110.2(4) . . ?
O24 C47 H47A 109.6 . . ?
C48 C47 H47A 109.6 . . ?
O24 C47 H47B 109.6 . . ?
C48 C47 H47B 109.6 . . ?
H47A C47 H47B 108.1 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C49 O25 H25O 105(2) . . ?
O25 C49 C50 111.2(3) . . ?
O25 C49 H49A 109.4 . . ?
C50 C49 H49A 109.4 . . ?
O25 C49 H49B 109.4 . . ?
C50 C49 H49B 109.4 . . ?
H49A C49 H49B 108.0 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.355
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.062
_database_code_depnum_ccdc_archive 'CCDC 1018618'
