# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2014

#######################################################################
#
#                 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
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# 
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#  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.
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data_ap409a0m
#TrackingRef 'complex1.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C98 H108 N6 Ni8 O32'
_chemical_formula_weight         2351.58

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'

_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                   13.291(2)
_cell_length_b                   13.838(2)
_cell_length_c                   16.545(4)
_cell_angle_alpha                108.734(3)
_cell_angle_beta                 105.788(3)
_cell_angle_gamma                101.737(2)
_cell_volume                     2628.1(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3998
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      22.38

_exptl_crystal_description       prism
_exptl_crystal_colour            dark_green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1218
_exptl_absorpt_coefficient_mu    1.481
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.7561
_exptl_absorpt_correction_T_max  0.8907
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART Apex-II'
_diffrn_measurement_method       'Omega Scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17894
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0778
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.36
_diffrn_reflns_theta_max         27.56
_reflns_number_total             11581
_reflns_number_gt                7534
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex-II'
_computing_cell_refinement       'Bruker Apex-II'
_computing_data_reduction        'Bruker Apex-II'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL 6.31'
_computing_publication_material  'Bruker SHELXTL 6.31'

_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)+(0.0818P)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         11581
_refine_ls_number_parameters     655
_refine_ls_number_restraints     612
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0542
_refine_ls_wR_factor_ref         0.1603
_refine_ls_wR_factor_gt          0.1391
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.016
_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
Ni1 Ni -0.04670(4) 0.48171(4) 0.12754(4) 0.03315(15) Uani 1 1 d U . .
Ni2 Ni 0.17948(4) 0.49123(4) 0.06374(3) 0.03255(15) Uani 1 1 d U . .
Ni3 Ni 0.05741(4) 0.68403(4) 0.10305(4) 0.03418(15) Uani 1 1 d U . .
Ni4 Ni -0.16210(5) 0.65328(5) 0.13214(4) 0.03815(16) Uani 1 1 d U . .
N1 N -0.0977(3) 0.3185(3) 0.0656(2) 0.0400(8) Uani 1 1 d U . .
N4 N 0.2212(3) 0.7171(3) 0.1695(2) 0.0375(8) Uani 1 1 d U . .
N21 N 0.1761(3) 0.4697(3) 0.1783(2) 0.0355(8) Uani 1 1 d U . .
O1 O -0.1127(3) 0.2621(3) -0.0179(2) 0.0457(8) Uani 1 1 d U . .
O1A O 0.3281(13) 0.8409(13) 0.4949(10) 0.379(9) Uani 1 1 d D . .
H101 H 0.3319 0.7854 0.4416 0.569 Uiso 1 1 d RD . .
H102 H 0.2800 0.8642 0.4637 0.569 Uiso 1 1 d RD . .
O2A O -0.1308(8) 0.9911(8) 0.5137(9) 0.313(8) Uani 1 1 d D . .
H201 H -0.1379 0.9901 0.4532 0.021(10) Uiso 1 1 d RD . .
H202 H -0.0863 0.9446 0.5127 0.054(15) Uiso 1 1 d RD . .
O4 O 0.2723(2) 0.6476(2) 0.1490(2) 0.0410(7) Uani 1 1 d U . .
O8 O -0.1006(3) 0.4359(3) 0.2225(2) 0.0454(8) Uani 1 1 d U . .
O19 O -0.3180(3) 0.6534(3) 0.0607(3) 0.0618(10) Uani 1 1 d U . .
O21 O 0.1003(2) 0.4873(3) 0.2120(2) 0.0413(7) Uani 1 1 d U . .
O28 O 0.3286(2) 0.4566(3) 0.1107(2) 0.0415(7) Uani 1 1 d U . .
O48 O 0.1050(3) 0.8462(3) 0.1856(2) 0.0455(7) Uani 1 1 d U . .
O61 O -0.2183(3) 0.6271(3) 0.2288(2) 0.0537(8) Uani 1 1 d U . .
O62 O -0.1708(4) 0.7947(4) 0.3314(3) 0.0941(15) Uani 1 1 d U . .
O71 O -0.0108(2) 0.6428(2) 0.18965(18) 0.0358(6) Uani 1 1 d U . .
O72 O -0.1927(2) 0.4926(2) 0.05206(19) 0.0343(6) Uani 1 1 d U . .
O73 O -0.1026(2) 0.6659(2) 0.03100(19) 0.0350(6) Uani 1 1 d U . .
O74 O -0.1127(3) 0.8200(3) 0.2013(2) 0.0598(9) Uani 1 1 d DU . .
H74 H -0.1166 0.8283 0.2466 0.090 Uiso 1 1 d RD . .
O81 O 0.0355(2) 0.5250(2) 0.04941(17) 0.0312(6) Uani 1 1 d U . .
C1 C -0.1331(4) 0.2654(4) 0.1123(3) 0.0450(10) Uani 1 1 d U . .
C2 C -0.1917(4) 0.1496(4) 0.0701(3) 0.0493(11) Uani 1 1 d U . .
C3 C -0.1527(6) 0.0746(5) 0.0173(5) 0.0760(17) Uani 1 1 d U . .
H3 H -0.0862 0.0983 0.0103 0.091 Uiso 1 1 calc R . .
C4 C -0.2122(7) -0.0328(5) -0.0236(5) 0.090(2) Uani 1 1 d U . .
H4 H -0.1851 -0.0810 -0.0581 0.107 Uiso 1 1 calc R . .
C5 C -0.3097(7) -0.0708(6) -0.0149(5) 0.093(2) Uani 1 1 d U . .
H5 H -0.3487 -0.1441 -0.0426 0.111 Uiso 1 1 calc R . .
C6 C -0.3490(6) -0.0003(6) 0.0346(5) 0.0848(19) Uani 1 1 d U . .
H6 H -0.4158 -0.0257 0.0405 0.102 Uiso 1 1 calc R . .
C7 C -0.2919(5) 0.1088(5) 0.0768(4) 0.0686(15) Uani 1 1 d U . .
H7 H -0.3212 0.1555 0.1102 0.082 Uiso 1 1 calc R . .
C8 C -0.1145(4) 0.3388(4) 0.2053(3) 0.0433(10) Uani 1 1 d U . .
C9 C -0.1068(4) 0.3019(5) 0.2812(4) 0.0527(12) Uani 1 1 d U . .
C10 C -0.0820(5) 0.2087(5) 0.2793(4) 0.0718(16) Uani 1 1 d U . .
H10 H -0.0762 0.1628 0.2269 0.086 Uiso 1 1 calc R . .
C11 C -0.0662(6) 0.1845(6) 0.3553(5) 0.094(2) Uani 1 1 d U . .
H11 H -0.0483 0.1227 0.3544 0.113 Uiso 1 1 calc R . .
C12 C -0.0765(6) 0.2511(7) 0.4327(5) 0.097(2) Uani 1 1 d U . .
H12 H -0.0668 0.2335 0.4834 0.116 Uiso 1 1 calc R . .
C13 C -0.1007(6) 0.3420(7) 0.4350(5) 0.093(2) Uani 1 1 d U . .
H13 H -0.1079 0.3867 0.4873 0.112 Uiso 1 1 calc R . .
C14 C -0.1147(5) 0.3684(5) 0.3608(4) 0.0684(16) Uani 1 1 d U . .
H14 H -0.1298 0.4319 0.3636 0.082 Uiso 1 1 calc R . .
C19 C -0.3896(6) 0.6972(8) 0.0910(5) 0.120(3) Uani 1 1 d U . .
H19A H -0.4545 0.6822 0.0398 0.180 Uiso 1 1 calc R . .
H19B H -0.3556 0.7737 0.1235 0.180 Uiso 1 1 calc R . .
H19C H -0.4097 0.6669 0.1313 0.180 Uiso 1 1 calc R . .
C21 C 0.2647(3) 0.4609(4) 0.2304(3) 0.0364(9) Uani 1 1 d U . .
C22 C 0.2871(4) 0.4780(4) 0.3270(3) 0.0388(10) Uani 1 1 d U . .
C23 C 0.2053(4) 0.4326(4) 0.3541(3) 0.0473(11) Uani 1 1 d U . .
H23 H 0.1366 0.3875 0.3105 0.057 Uiso 1 1 calc R . .
C24 C 0.2268(5) 0.4548(5) 0.4454(3) 0.0575(13) Uani 1 1 d U . .
H24 H 0.1718 0.4244 0.4629 0.069 Uiso 1 1 calc R . .
C25 C 0.3262(5) 0.5202(5) 0.5105(4) 0.0666(15) Uani 1 1 d U . .
H25 H 0.3398 0.5337 0.5719 0.080 Uiso 1 1 calc R . .
C26 C 0.4058(5) 0.5656(5) 0.4845(4) 0.0712(16) Uani 1 1 d U . .
H26 H 0.4735 0.6122 0.5290 0.085 Uiso 1 1 calc R . .
C27 C 0.3881(4) 0.5437(4) 0.3932(3) 0.0548(13) Uani 1 1 d U . .
H27 H 0.4444 0.5734 0.3766 0.066 Uiso 1 1 calc R . .
C28 C 0.3387(4) 0.4387(4) 0.1816(3) 0.0393(10) Uani 1 1 d U . .
C29 C 0.4224(3) 0.3873(4) 0.2091(3) 0.0394(10) Uani 1 1 d U . .
C30 C 0.4015(4) 0.3112(4) 0.2453(3) 0.0460(11) Uani 1 1 d U . .
H30 H 0.3370 0.2965 0.2573 0.055 Uiso 1 1 calc R . .
C31 C 0.4756(5) 0.2571(5) 0.2635(4) 0.0596(14) Uani 1 1 d U . .
H31 H 0.4600 0.2038 0.2852 0.071 Uiso 1 1 calc R . .
C32 C 0.5723(5) 0.2831(5) 0.2491(4) 0.0645(15) Uani 1 1 d U . .
H32 H 0.6236 0.2486 0.2633 0.077 Uiso 1 1 calc R . .
C33 C 0.5950(5) 0.3581(6) 0.2146(4) 0.0687(16) Uani 1 1 d U . .
H33 H 0.6611 0.3742 0.2051 0.082 Uiso 1 1 calc R . .
C34 C 0.5203(4) 0.4102(5) 0.1936(4) 0.0572(13) Uani 1 1 d U . .
H34 H 0.5353 0.4607 0.1689 0.069 Uiso 1 1 calc R . .
C41 C 0.2781(4) 0.8195(4) 0.2147(3) 0.0432(10) Uani 1 1 d U . .
C42 C 0.3988(4) 0.8621(4) 0.2404(4) 0.0534(12) Uani 1 1 d U . .
C43 C 0.4711(5) 0.8259(5) 0.2916(4) 0.0731(16) Uani 1 1 d U . .
H43 H 0.4440 0.7739 0.3113 0.088 Uiso 1 1 calc R . .
C44 C 0.5814(6) 0.8662(7) 0.3130(6) 0.104(2) Uani 1 1 d U . .
H44 H 0.6288 0.8416 0.3481 0.124 Uiso 1 1 calc R . .
C45 C 0.6242(7) 0.9403(8) 0.2854(7) 0.120(3) Uani 1 1 d U . .
H45 H 0.7001 0.9674 0.3016 0.144 Uiso 1 1 calc R . .
C46 C 0.5542(7) 0.9757(7) 0.2327(6) 0.106(2) Uani 1 1 d U . .
H46 H 0.5829 1.0267 0.2126 0.128 Uiso 1 1 calc R . .
C47 C 0.4397(6) 0.9356(5) 0.2089(5) 0.0784(17) Uani 1 1 d U . .
H47 H 0.3923 0.9587 0.1723 0.094 Uiso 1 1 calc R . .
C48 C 0.2066(4) 0.8852(4) 0.2281(3) 0.0435(10) Uani 1 1 d U . .
C49 C 0.2493(4) 1.0001(4) 0.2925(3) 0.0513(12) Uani 1 1 d U . .
C50 C 0.3407(5) 1.0414(5) 0.3717(4) 0.0652(14) Uani 1 1 d U . .
H50 H 0.3820 0.9978 0.3844 0.078 Uiso 1 1 calc R . .
C51 C 0.3716(6) 1.1472(5) 0.4328(5) 0.0830(18) Uani 1 1 d U . .
H51 H 0.4333 1.1746 0.4865 0.100 Uiso 1 1 calc R . .
C52 C 0.3110(6) 1.2108(5) 0.4137(5) 0.088(2) Uani 1 1 d U . .
H52 H 0.3321 1.2820 0.4548 0.106 Uiso 1 1 calc R . .
C53 C 0.2196(6) 1.1721(5) 0.3353(6) 0.087(2) Uani 1 1 d U . .
H53 H 0.1789 1.2165 0.3232 0.104 Uiso 1 1 calc R . .
C54 C 0.1885(5) 1.0660(4) 0.2740(5) 0.0677(15) Uani 1 1 d U . .
H54 H 0.1267 1.0390 0.2205 0.081 Uiso 1 1 calc R . .
C61 C -0.2075(5) 0.6939(6) 0.3043(4) 0.0681(15) Uani 1 1 d U . .
C62 C -0.2388(8) 0.6508(7) 0.3694(5) 0.117(3) Uani 1 1 d U . .
H62A H -0.2272 0.7096 0.4249 0.176 Uiso 1 1 calc R . .
H62B H -0.1942 0.6075 0.3831 0.176 Uiso 1 1 calc R . .
H62C H -0.3152 0.6076 0.3418 0.176 Uiso 1 1 calc R . .
C71 C 0.0473(4) 0.6912(5) 0.2861(3) 0.0563(13) Uani 1 1 d U . .
H71A H 0.0599 0.7675 0.3079 0.084 Uiso 1 1 calc R . .
H71B H 0.1169 0.6779 0.3000 0.084 Uiso 1 1 calc R . .
H71C H 0.0045 0.6610 0.3156 0.084 Uiso 1 1 calc R . .
C72 C -0.2931(4) 0.4185(5) 0.0380(4) 0.0565(13) Uani 1 1 d U . .
H72A H -0.2925 0.4159 0.0954 0.085 Uiso 1 1 calc R . .
H72B H -0.3010 0.3483 -0.0039 0.085 Uiso 1 1 calc R . .
H72C H -0.3537 0.4411 0.0130 0.085 Uiso 1 1 calc R . .
C73 C -0.1159(4) 0.7484(4) 0.0001(4) 0.0513(12) Uani 1 1 d U . .
H73A H -0.1927 0.7338 -0.0326 0.077 Uiso 1 1 calc R . .
H73B H -0.0757 0.7510 -0.0398 0.077 Uiso 1 1 calc R . .
H73C H -0.0882 0.8164 0.0517 0.077 Uiso 1 1 calc R . .
C74 C -0.141(3) 0.9134(14) 0.208(2) 0.61(3) Uani 1 1 d DU . .
H74A H -0.0933 0.9711 0.2652 0.911 Uiso 1 1 calc R . .
H74B H -0.2162 0.9008 0.2041 0.911 Uiso 1 1 calc R . .
H74C H -0.1329 0.9324 0.1584 0.911 Uiso 1 1 calc R . .
H19 H -0.340(8) 0.610(9) -0.012(8) 0.21(4) 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 O71 2.021(3) . ?
Ni1 N1 2.031(4) . ?
Ni1 O21 2.040(3) . ?
Ni1 O81 2.055(3) . ?
Ni1 O72 2.066(3) . ?
Ni1 O8 2.110(3) . ?
Ni2 N21 2.022(3) . ?
Ni2 O81 2.031(3) . ?
Ni2 O72 2.048(3) 2_565 ?
Ni2 O4 2.050(3) . ?
Ni2 O73 2.065(3) 2_565 ?
Ni2 O28 2.132(3) . ?
Ni3 O81 2.015(3) . ?
Ni3 O1 2.024(3) 2_565 ?
Ni3 N4 2.031(4) . ?
Ni3 O71 2.055(3) . ?
Ni3 O73 2.054(3) . ?
Ni3 O48 2.070(3) . ?
Ni4 O71 2.034(3) . ?
Ni4 O61 2.040(3) . ?
Ni4 O73 2.075(3) . ?
Ni4 O72 2.076(3) . ?
Ni4 O74 2.084(4) . ?
Ni4 O19 2.088(3) . ?
N1 O1 1.285(4) . ?
N1 C1 1.334(5) . ?
N4 O4 1.297(4) . ?
N4 C41 1.309(6) . ?
N21 O21 1.305(4) . ?
N21 C21 1.311(5) . ?
O1 Ni3 2.024(3) 2_565 ?
O1A H101 0.9873 . ?
O1A H102 0.8887 . ?
O2A H201 0.9754 . ?
O2A H202 0.9574 . ?
O8 C8 1.243(5) . ?
O19 C19 1.351(6) . ?
O19 H19 1.09(11) . ?
O28 C28 1.254(5) . ?
O48 C48 1.246(5) . ?
O61 C61 1.242(7) . ?
O62 C61 1.259(8) . ?
O71 C71 1.423(5) . ?
O72 C72 1.417(6) . ?
O72 Ni2 2.048(3) 2_565 ?
O73 C73 1.416(5) . ?
O73 Ni2 2.065(3) 2_565 ?
O74 C74 1.398(13) . ?
O74 H74 0.7395 . ?
O81 O81 1.487(5) 2_565 ?
C1 C2 1.463(7) . ?
C1 C8 1.465(7) . ?
C2 C7 1.386(7) . ?
C2 C3 1.411(7) . ?
C3 C4 1.371(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.360(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.350(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.382(9) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.487(6) . ?
C9 C10 1.387(7) . ?
C9 C14 1.389(7) . ?
C10 C11 1.374(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.377(10) . ?
C11 H11 0.9300 . ?
C12 C13 1.352(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.367(7) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C21 C28 1.452(6) . ?
C21 C22 1.472(5) . ?
C22 C27 1.375(6) . ?
C22 C23 1.394(6) . ?
C23 C24 1.375(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.356(8) . ?
C24 H24 0.9300 . ?
C25 C26 1.359(8) . ?
C25 H25 0.9300 . ?
C26 C27 1.383(7) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.485(6) . ?
C29 C30 1.385(6) . ?
C29 C34 1.387(6) . ?
C30 C31 1.380(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.369(7) . ?
C31 H31 0.9300 . ?
C32 C33 1.357(8) . ?
C32 H32 0.9300 . ?
C33 C34 1.375(7) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C41 C48 1.454(6) . ?
C41 C42 1.479(7) . ?
C42 C47 1.367(8) . ?
C42 C43 1.385(8) . ?
C43 C44 1.358(8) . ?
C43 H43 0.9300 . ?
C44 C45 1.338(12) . ?
C44 H44 0.9300 . ?
C45 C46 1.372(12) . ?
C45 H45 0.9300 . ?
C46 C47 1.404(9) . ?
C46 H46 0.9300 . ?
C47 H47 0.9300 . ?
C48 C49 1.484(7) . ?
C49 C50 1.375(8) . ?
C49 C54 1.386(7) . ?
C50 C51 1.382(8) . ?
C50 H50 0.9300 . ?
C51 C52 1.361(9) . ?
C51 H51 0.9300 . ?
C52 C53 1.371(10) . ?
C52 H52 0.9300 . ?
C53 C54 1.387(8) . ?
C53 H53 0.9300 . ?
C54 H54 0.9300 . ?
C61 C62 1.498(8) . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C71 H71A 0.9600 . ?
C71 H71B 0.9600 . ?
C71 H71C 0.9600 . ?
C72 H72A 0.9600 . ?
C72 H72B 0.9600 . ?
C72 H72C 0.9600 . ?
C73 H73A 0.9600 . ?
C73 H73B 0.9600 . ?
C73 H73C 0.9600 . ?
C74 H74 1.5599 . ?
C74 H74A 0.9600 . ?
C74 H74B 0.9600 . ?
C74 H74C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O71 Ni1 N1 174.40(13) . . ?
O71 Ni1 O21 91.47(12) . . ?
N1 Ni1 O21 92.53(13) . . ?
O71 Ni1 O81 82.17(11) . . ?
N1 Ni1 O81 101.88(13) . . ?
O21 Ni1 O81 87.91(11) . . ?
O71 Ni1 O72 82.54(11) . . ?
N1 Ni1 O72 93.33(13) . . ?
O21 Ni1 O72 173.76(12) . . ?
O81 Ni1 O72 92.96(10) . . ?
O71 Ni1 O8 99.08(12) . . ?
N1 Ni1 O8 77.73(13) . . ?
O21 Ni1 O8 80.74(12) . . ?
O81 Ni1 O8 168.60(11) . . ?
O72 Ni1 O8 98.44(11) . . ?
N21 Ni2 O81 89.13(11) . . ?
N21 Ni2 O72 175.39(12) . 2_565 ?
O81 Ni2 O72 95.36(10) . 2_565 ?
N21 Ni2 O4 86.29(13) . . ?
O81 Ni2 O4 92.62(11) . . ?
O72 Ni2 O4 94.52(12) 2_565 . ?
N21 Ni2 O73 99.36(13) . 2_565 ?
O81 Ni2 O73 93.44(11) . 2_565 ?
O72 Ni2 O73 79.38(11) 2_565 2_565 ?
O4 Ni2 O73 171.77(11) . 2_565 ?
N21 Ni2 O28 76.66(12) . . ?
O81 Ni2 O28 165.66(10) . . ?
O72 Ni2 O28 98.89(11) 2_565 . ?
O4 Ni2 O28 84.67(12) . . ?
O73 Ni2 O28 90.79(11) 2_565 . ?
O81 Ni3 O1 103.45(12) . 2_565 ?
O81 Ni3 N4 91.35(13) . . ?
O1 Ni3 N4 82.27(13) 2_565 . ?
O81 Ni3 O71 82.33(11) . . ?
O1 Ni3 O71 172.49(12) 2_565 . ?
N4 Ni3 O71 102.57(12) . . ?
O81 Ni3 O73 93.59(11) . . ?
O1 Ni3 O73 91.60(12) 2_565 . ?
N4 Ni3 O73 172.89(13) . . ?
O71 Ni3 O73 83.17(11) . . ?
O81 Ni3 O48 166.34(11) . . ?
O1 Ni3 O48 83.97(13) 2_565 . ?
N4 Ni3 O48 78.16(14) . . ?
O71 Ni3 O48 91.36(12) . . ?
O73 Ni3 O48 97.69(12) . . ?
O71 Ni4 O61 94.12(12) . . ?
O71 Ni4 O73 83.15(11) . . ?
O61 Ni4 O73 174.60(12) . . ?
O71 Ni4 O72 81.98(11) . . ?
O61 Ni4 O72 96.53(13) . . ?
O73 Ni4 O72 78.50(11) . . ?
O71 Ni4 O74 94.02(13) . . ?
O61 Ni4 O74 92.75(14) . . ?
O73 Ni4 O74 92.09(13) . . ?
O72 Ni4 O74 170.12(12) . . ?
O71 Ni4 O19 174.32(13) . . ?
O61 Ni4 O19 89.62(14) . . ?
O73 Ni4 O19 92.77(13) . . ?
O72 Ni4 O19 93.35(14) . . ?
O74 Ni4 O19 90.07(15) . . ?
O1 N1 C1 116.8(4) . . ?
O1 N1 Ni1 126.3(3) . . ?
C1 N1 Ni1 116.3(3) . . ?
O4 N4 C41 119.4(4) . . ?
O4 N4 Ni3 122.5(3) . . ?
C41 N4 Ni3 115.4(3) . . ?
O21 N21 C21 118.1(3) . . ?
O21 N21 Ni2 122.1(2) . . ?
C21 N21 Ni2 118.1(3) . . ?
N1 O1 Ni3 126.4(3) . 2_565 ?
H101 O1A H102 97.2 . . ?
H201 O2A H202 95.4 . . ?
N4 O4 Ni2 118.2(3) . . ?
C8 O8 Ni1 111.4(3) . . ?
C19 O19 Ni4 130.8(4) . . ?
C19 O19 H19 119(5) . . ?
Ni4 O19 H19 110(5) . . ?
N21 O21 Ni1 118.9(2) . . ?
C28 O28 Ni2 111.8(3) . . ?
C48 O48 Ni3 112.2(3) . . ?
C61 O61 Ni4 128.2(4) . . ?
C71 O71 Ni1 116.9(3) . . ?
C71 O71 Ni4 121.7(3) . . ?
Ni1 O71 Ni4 98.43(13) . . ?
C71 O71 Ni3 120.7(3) . . ?
Ni1 O71 Ni3 97.41(11) . . ?
Ni4 O71 Ni3 96.58(11) . . ?
C72 O72 Ni2 114.9(3) . 2_565 ?
C72 O72 Ni1 118.2(3) . . ?
Ni2 O72 Ni1 109.32(12) 2_565 . ?
C72 O72 Ni4 117.0(3) . . ?
Ni2 O72 Ni4 98.76(12) 2_565 . ?
Ni1 O72 Ni4 95.65(12) . . ?
C73 O73 Ni3 114.9(3) . . ?
C73 O73 Ni2 117.3(3) . 2_565 ?
Ni3 O73 Ni2 109.22(12) . 2_565 ?
C73 O73 Ni4 118.7(3) . . ?
Ni3 O73 Ni4 95.30(11) . . ?
Ni2 O73 Ni4 98.22(12) 2_565 . ?
C74 O74 Ni4 145.6(12) . . ?
C74 O74 H74 88.1 . . ?
Ni4 O74 H74 104.4 . . ?
O81 O81 Ni3 111.0(2) 2_565 . ?
O81 O81 Ni2 108.7(2) 2_565 . ?
Ni3 O81 Ni2 113.08(13) . . ?
O81 O81 Ni1 111.5(3) 2_565 . ?
Ni3 O81 Ni1 97.59(11) . . ?
Ni2 O81 Ni1 114.60(12) . . ?
N1 C1 C2 122.2(4) . . ?
N1 C1 C8 111.5(4) . . ?
C2 C1 C8 126.1(4) . . ?
C7 C2 C3 116.6(5) . . ?
C7 C2 C1 121.0(5) . . ?
C3 C2 C1 122.4(5) . . ?
C4 C3 C2 120.4(6) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C5 C4 C3 121.7(6) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
C6 C5 C4 118.8(6) . . ?
C6 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
C5 C6 C7 121.4(7) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C6 C7 C2 121.0(6) . . ?
C6 C7 H7 119.5 . . ?
C2 C7 H7 119.5 . . ?
O8 C8 C1 119.3(4) . . ?
O8 C8 C9 118.6(4) . . ?
C1 C8 C9 122.1(4) . . ?
C10 C9 C14 118.3(5) . . ?
C10 C9 C8 122.9(5) . . ?
C14 C9 C8 118.5(5) . . ?
C11 C10 C9 119.8(6) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C12 C11 C10 120.5(6) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C13 C12 C11 120.1(6) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 120.2(7) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C13 C14 C9 121.0(6) . . ?
C13 C14 H14 119.5 . . ?
C9 C14 H14 119.5 . . ?
O19 C19 H19A 109.5 . . ?
O19 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O19 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N21 C21 C28 110.9(3) . . ?
N21 C21 C22 123.5(4) . . ?
C28 C21 C22 125.5(4) . . ?
C27 C22 C23 118.5(4) . . ?
C27 C22 C21 120.4(4) . . ?
C23 C22 C21 121.0(4) . . ?
C24 C23 C22 119.8(5) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C25 C24 C23 121.5(5) . . ?
C25 C24 H24 119.2 . . ?
C23 C24 H24 119.2 . . ?
C24 C25 C26 119.0(5) . . ?
C24 C25 H25 120.5 . . ?
C26 C25 H25 120.5 . . ?
C25 C26 C27 121.2(6) . . ?
C25 C26 H26 119.4 . . ?
C27 C26 H26 119.4 . . ?
C22 C27 C26 120.0(5) . . ?
C22 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
O28 C28 C21 120.1(4) . . ?
O28 C28 C29 117.8(4) . . ?
C21 C28 C29 121.9(4) . . ?
C30 C29 C34 119.0(4) . . ?
C30 C29 C28 120.8(4) . . ?
C34 C29 C28 120.1(4) . . ?
C31 C30 C29 120.5(4) . . ?
C31 C30 H30 119.7 . . ?
C29 C30 H30 119.7 . . ?
C32 C31 C30 119.0(5) . . ?
C32 C31 H31 120.5 . . ?
C30 C31 H31 120.5 . . ?
C33 C32 C31 121.4(5) . . ?
C33 C32 H32 119.3 . . ?
C31 C32 H32 119.3 . . ?
C32 C33 C34 120.1(5) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C33 C34 C29 119.9(5) . . ?
C33 C34 H34 120.0 . . ?
C29 C34 H34 120.0 . . ?
N4 C41 C48 111.5(4) . . ?
N4 C41 C42 123.4(4) . . ?
C48 C41 C42 124.9(4) . . ?
C47 C42 C43 119.1(6) . . ?
C47 C42 C41 118.9(5) . . ?
C43 C42 C41 121.9(5) . . ?
C44 C43 C42 120.1(7) . . ?
C44 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
C45 C44 C43 122.1(8) . . ?
C45 C44 H44 119.0 . . ?
C43 C44 H44 119.0 . . ?
C44 C45 C46 119.0(8) . . ?
C44 C45 H45 120.5 . . ?
C46 C45 H45 120.5 . . ?
C45 C46 C47 120.5(8) . . ?
C45 C46 H46 119.7 . . ?
C47 C46 H46 119.7 . . ?
C42 C47 C46 119.1(7) . . ?
C42 C47 H47 120.4 . . ?
C46 C47 H47 120.4 . . ?
O48 C48 C41 120.7(4) . . ?
O48 C48 C49 116.7(4) . . ?
C41 C48 C49 122.6(4) . . ?
C50 C49 C54 119.2(5) . . ?
C50 C49 C48 123.2(5) . . ?
C54 C49 C48 117.4(5) . . ?
C49 C50 C51 120.7(6) . . ?
C49 C50 H50 119.7 . . ?
C51 C50 H50 119.7 . . ?
C52 C51 C50 119.4(7) . . ?
C52 C51 H51 120.3 . . ?
C50 C51 H51 120.3 . . ?
C51 C52 C53 121.4(7) . . ?
C51 C52 H52 119.3 . . ?
C53 C52 H52 119.3 . . ?
C52 C53 C54 119.2(7) . . ?
C52 C53 H53 120.4 . . ?
C54 C53 H53 120.4 . . ?
C53 C54 C49 120.1(6) . . ?
C53 C54 H54 119.9 . . ?
C49 C54 H54 119.9 . . ?
O61 C61 O62 125.7(5) . . ?
O61 C61 C62 117.1(7) . . ?
O62 C61 C62 117.2(6) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
O71 C71 H71A 109.5 . . ?
O71 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
O71 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
O72 C72 H72A 109.5 . . ?
O72 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
O72 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
O73 C73 H73A 109.5 . . ?
O73 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
O73 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
O74 C74 H74 28.3 . . ?
O74 C74 H74A 109.5 . . ?
H74 C74 H74A 91.0 . . ?
O74 C74 H74B 109.5 . . ?
H74 C74 H74B 97.4 . . ?
H74A C74 H74B 109.5 . . ?
O74 C74 H74C 109.5 . . ?
H74 C74 H74C 137.4 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.952
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.952
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.096
_database_code_depnum_ccdc_archive 'CCDC 894474'
#######################################################################
#
#                 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_ap510_0m
#TrackingRef 'complex2.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C110 H112 N6 Ni8 O30'
_chemical_formula_weight         2467.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   13.259(2)
_cell_length_b                   28.761(5)
_cell_length_c                   15.273(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.829(2)
_cell_angle_gamma                90.00
_cell_volume                     5655.0(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4180
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      24.17

_exptl_crystal_description       prism
_exptl_crystal_colour            dark_green
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2556
_exptl_absorpt_coefficient_mu    1.379
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5951
_exptl_absorpt_correction_T_max  0.8520
_exptl_absorpt_process_details   'Bruker Apex-II'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21909
_diffrn_reflns_av_R_equivalents  0.0920
_diffrn_reflns_av_sigmaI/netI    0.1137
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         24.17
_reflns_number_total             8862
_reflns_number_gt                5175
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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)+(0.0783P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       none
_refine_ls_number_reflns         8862
_refine_ls_number_parameters     734
_refine_ls_number_restraints     760
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.0631
_refine_ls_wR_factor_ref         0.1743
_refine_ls_wR_factor_gt          0.1463
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      0.977
_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
Ni3 Ni 0.33985(7) 0.48723(3) 0.88900(5) 0.0480(3) Uani 1 1 d U . .
Ni1 Ni 0.52088(7) 0.55295(3) 0.88232(5) 0.0469(3) Uani 1 1 d U . .
Ni4 Ni 0.30232(7) 0.59262(3) 0.86891(5) 0.0524(3) Uani 1 1 d U . .
Ni2 Ni 0.57900(7) 0.43816(3) 0.93626(5) 0.0470(3) Uani 1 1 d U . .
C48 C 0.2033(6) 0.4435(3) 0.7405(4) 0.0601(17) Uani 1 1 d U B .
C1A C 0.0333(13) 0.7055(5) 0.4960(11) 0.176(6) Uani 1 1 d U . .
C41 C 0.2942(6) 0.4133(2) 0.7590(4) 0.0593(17) Uani 1 1 d U B .
C49 C 0.1175(7) 0.4386(2) 0.6580(5) 0.0657(19) Uani 1 1 d U . .
C54 C 0.0200(7) 0.4558(3) 0.6581(6) 0.086(2) Uani 1 1 d U . .
H54 H 0.0091 0.4695 0.7102 0.103 Uiso 1 1 calc R . .
C53 C -0.0600(7) 0.4532(3) 0.5838(7) 0.097(3) Uani 1 1 d U . .
H53 H -0.1256 0.4640 0.5857 0.116 Uiso 1 1 calc R . .
C52 C -0.0431(8) 0.4345(3) 0.5058(6) 0.097(3) Uani 1 1 d U . .
H52 H -0.0980 0.4324 0.4550 0.116 Uiso 1 1 calc R . .
C51 C 0.0509(8) 0.4190(3) 0.5015(6) 0.104(3) Uani 1 1 d U . .
H51 H 0.0619 0.4076 0.4475 0.125 Uiso 1 1 calc R . .
C50 C 0.1322(7) 0.4201(3) 0.5788(5) 0.083(2) Uani 1 1 d U . .
H50 H 0.1969 0.4082 0.5768 0.099 Uiso 1 1 calc R . .
C42 C 0.2980(8) 0.3651(3) 0.7244(5) 0.081(2) Uani 1 1 d U . .
C47 C 0.2275(10) 0.3345(3) 0.7345(8) 0.131(4) Uani 1 1 d U B .
H47 H 0.1751 0.3394 0.7645 0.158 Uiso 1 1 calc R A 1
C46 C 0.249(3) 0.2858(14) 0.684(3) 0.130(9) Uiso 0.50 1 d PU B 1
H46 H 0.1964 0.2636 0.6704 0.156 Uiso 0.50 1 calc PR B 1
C45 C 0.346(3) 0.2765(11) 0.662(3) 0.144(8) Uani 0.50 1 d PU B 1
H45 H 0.3680 0.2462 0.6562 0.173 Uiso 0.50 1 calc PR B 1
C44 C 0.402(2) 0.3114(8) 0.6493(17) 0.114(7) Uani 0.50 1 d PU B 1
H44 H 0.4536 0.3072 0.6186 0.137 Uiso 0.50 1 calc PR B 1
C43 C 0.385(4) 0.3552(18) 0.681(4) 0.104(7) Uani 0.50 1 d PU B 1
H43 H 0.4301 0.3793 0.6754 0.125 Uiso 0.50 1 calc PR B 1
C46A C 0.209(2) 0.2884(7) 0.7262(19) 0.130(7) Uani 0.50 1 d PU B 2
H46A H 0.1574 0.2711 0.7423 0.156 Uiso 0.50 1 calc PR B 2
C45A C 0.287(3) 0.2738(14) 0.689(3) 0.147(8) Uani 0.50 1 d PU B 2
H45A H 0.2981 0.2419 0.6894 0.176 Uiso 0.50 1 calc PR B 2
C44A C 0.341(3) 0.2966(9) 0.655(3) 0.120(7) Uani 0.50 1 d PU B 2
H44A H 0.3683 0.2847 0.6088 0.144 Uiso 0.50 1 calc PR B 2
C43A C 0.364(4) 0.3469(18) 0.689(4) 0.109(6) Uani 0.50 1 d PU B 2
H43A H 0.4238 0.3626 0.6842 0.130 Uiso 0.50 1 calc PR B 2
C8 C 0.6525(7) 0.6131(2) 0.8178(5) 0.0616(18) Uani 1 1 d U B .
C1 C 0.7137(6) 0.6029(2) 0.9125(5) 0.0594(17) Uani 1 1 d U . .
C9 C 0.7021(8) 0.6340(3) 0.7495(5) 0.079(2) Uani 1 1 d U . .
C14 C 0.6379(9) 0.6440(4) 0.6667(7) 0.133(4) Uani 1 1 d U . .
H14 H 0.5668 0.6390 0.6569 0.160 Uiso 1 1 calc R . .
C13 C 0.6789(13) 0.6617(5) 0.5970(9) 0.167(5) Uani 1 1 d U . .
H13 H 0.6349 0.6686 0.5413 0.200 Uiso 1 1 calc R . .
C12 C 0.7858(14) 0.6692(5) 0.6109(10) 0.167(5) Uani 1 1 d U . .
H12 H 0.8141 0.6817 0.5660 0.200 Uiso 1 1 calc R . .
C11 C 0.8444(12) 0.6579(5) 0.6895(9) 0.169(5) Uani 1 1 d U . .
H11 H 0.9158 0.6619 0.6987 0.203 Uiso 1 1 calc R . .
C10 C 0.8064(10) 0.6401(4) 0.7609(7) 0.140(4) Uani 1 1 d U . .
H10 H 0.8519 0.6327 0.8155 0.168 Uiso 1 1 calc R . .
C2 C 0.8078(7) 0.6270(3) 0.9622(5) 0.076(2) Uani 1 1 d U . .
C7 C 0.8029(11) 0.6725(4) 0.9834(8) 0.140(4) Uani 1 1 d U . .
H7 H 0.7402 0.6883 0.9648 0.168 Uiso 1 1 calc R . .
C6 C 0.8889(14) 0.6960(5) 1.0321(11) 0.173(6) Uani 1 1 d U . .
H6 H 0.8838 0.7275 1.0442 0.208 Uiso 1 1 calc R . .
C5 C 0.9791(14) 0.6742(6) 1.0619(10) 0.173(6) Uani 1 1 d U . .
H5 H 1.0374 0.6899 1.0947 0.208 Uiso 1 1 calc R . .
C4 C 0.9825(11) 0.6297(6) 1.0431(10) 0.171(5) Uani 1 1 d U . .
H4 H 1.0452 0.6141 1.0636 0.205 Uiso 1 1 calc R . .
C3 C 0.9009(9) 0.6056(5) 0.9963(9) 0.150(5) Uani 1 1 d U . .
H3 H 0.9078 0.5739 0.9869 0.180 Uiso 1 1 calc R . .
C28 C 0.6898(6) 0.3978(2) 0.8160(4) 0.0561(17) Uani 1 1 d U B .
C21 C 0.6561(5) 0.4429(2) 0.7747(4) 0.0519(16) Uani 1 1 d U . .
C29 C 0.7496(6) 0.3643(2) 0.7762(4) 0.0557(17) Uani 1 1 d U . .
C34 C 0.7356(6) 0.3167(3) 0.7896(5) 0.070(2) Uani 1 1 d U . .
H34 H 0.6866 0.3069 0.8201 0.084 Uiso 1 1 calc R . .
C33 C 0.7949(8) 0.2846(3) 0.7575(6) 0.087(3) Uani 1 1 d U . .
H33 H 0.7856 0.2531 0.7669 0.105 Uiso 1 1 calc R . .
C32 C 0.8675(8) 0.2982(3) 0.7118(6) 0.091(3) Uani 1 1 d U . .
H32 H 0.9064 0.2763 0.6895 0.109 Uiso 1 1 calc R . .
C31 C 0.8814(7) 0.3452(3) 0.6998(6) 0.090(3) Uani 1 1 d U . .
H31 H 0.9306 0.3550 0.6694 0.108 Uiso 1 1 calc R . .
C30 C 0.8236(6) 0.3778(3) 0.7322(5) 0.073(2) Uani 1 1 d U . .
H30 H 0.8349 0.4093 0.7243 0.088 Uiso 1 1 calc R . .
C22 C 0.6599(7) 0.4594(3) 0.6824(4) 0.067(2) Uani 1 1 d U . .
C27 C 0.6184(6) 0.4336(3) 0.6063(5) 0.081(2) Uani 1 1 d U . .
H27 H 0.5923 0.4041 0.6122 0.098 Uiso 1 1 calc R . .
C26 C 0.6150(9) 0.4511(4) 0.5211(6) 0.122(4) Uani 1 1 d U . .
H26 H 0.5867 0.4334 0.4701 0.147 Uiso 1 1 calc R . .
C25 C 0.6531(12) 0.4941(5) 0.5126(7) 0.142(5) Uani 1 1 d U . .
H25 H 0.6473 0.5063 0.4553 0.171 Uiso 1 1 calc R . .
C24 C 0.7001(10) 0.5202(4) 0.5865(7) 0.127(4) Uani 1 1 d U . .
H24 H 0.7296 0.5488 0.5794 0.152 Uiso 1 1 calc R . .
C23 C 0.7026(8) 0.5027(3) 0.6723(5) 0.089(3) Uani 1 1 d U . .
H23 H 0.7329 0.5202 0.7231 0.107 Uiso 1 1 calc R . .
C61 C 0.2823(7) 0.6507(3) 0.7020(5) 0.0666(19) Uani 1 1 d U . .
C73 C 0.1984(6) 0.5325(3) 0.9868(5) 0.073(2) Uani 1 1 d U B .
H73A H 0.1830 0.5589 1.0198 0.109 Uiso 1 1 calc R . .
H73B H 0.2050 0.5053 1.0241 0.109 Uiso 1 1 calc R . .
H73C H 0.1433 0.5280 0.9338 0.109 Uiso 1 1 calc R . .
C72 C 0.4908(6) 0.6438(2) 0.9758(5) 0.0641(19) Uani 1 1 d U B .
H72A H 0.5015 0.6580 0.9218 0.096 Uiso 1 1 calc R . .
H72B H 0.5558 0.6419 1.0198 0.096 Uiso 1 1 calc R . .
H72C H 0.4428 0.6622 0.9992 0.096 Uiso 1 1 calc R . .
C71 C 0.3561(6) 0.5376(2) 0.7156(4) 0.064(2) Uani 1 1 d U B .
H71A H 0.2837 0.5323 0.6895 0.097 Uiso 1 1 calc R . .
H71B H 0.3958 0.5120 0.7013 0.097 Uiso 1 1 calc R . .
H71C H 0.3775 0.5658 0.6917 0.097 Uiso 1 1 calc R . .
C74 C 0.0548(9) 0.5806(9) 0.7926(14) 0.315(13) Uani 1 1 d DU B .
H74A H 0.0096 0.5723 0.7358 0.472 Uiso 1 1 calc R . .
H74B H 0.0383 0.6113 0.8090 0.472 Uiso 1 1 calc R . .
H74C H 0.0458 0.5589 0.8380 0.472 Uiso 1 1 calc R . .
C19 C 0.201(4) 0.6870(12) 0.9264(14) 0.098(11) Uani 0.45 1 d PU B 3
H19A H 0.1782 0.6980 0.9778 0.147 Uiso 0.45 1 calc PR B 3
H19B H 0.1445 0.6881 0.8739 0.147 Uiso 0.45 1 calc PR B 3
H19C H 0.2567 0.7065 0.9172 0.147 Uiso 0.45 1 calc PR B 3
C19A C 0.179(3) 0.6796(11) 0.8980(16) 0.110(9) Uani 0.55 1 d PU B 4
H19D H 0.1551 0.6979 0.9417 0.164 Uiso 0.55 1 calc PR B 4
H19E H 0.1198 0.6686 0.8532 0.164 Uiso 0.55 1 calc PR B 4
H19F H 0.2217 0.6983 0.8696 0.164 Uiso 0.55 1 calc PR B 4
C62 C 0.3380(7) 0.6791(3) 0.6455(5) 0.070(2) Uani 1 1 d U . .
C63 C 0.4133(8) 0.7100(3) 0.6842(6) 0.092(3) Uani 1 1 d U . .
H63 H 0.4325 0.7130 0.7466 0.110 Uiso 1 1 calc R . .
C64 C 0.4617(9) 0.7372(3) 0.6309(7) 0.110(3) Uani 1 1 d U . .
H64 H 0.5109 0.7592 0.6575 0.132 Uiso 1 1 calc R . .
C65 C 0.4366(10) 0.7315(4) 0.5388(7) 0.112(3) Uani 1 1 d U . .
H65 H 0.4704 0.7490 0.5033 0.135 Uiso 1 1 calc R . .
C66 C 0.3638(9) 0.7008(4) 0.5004(7) 0.112(3) Uani 1 1 d U . .
H66 H 0.3477 0.6967 0.4382 0.135 Uiso 1 1 calc R . .
C67 C 0.3127(9) 0.6755(3) 0.5523(5) 0.102(3) Uani 1 1 d U . .
H67 H 0.2599 0.6553 0.5244 0.122 Uiso 1 1 calc R . .
N4 N 0.3744(5) 0.43180(19) 0.8186(3) 0.0507(13) Uani 1 1 d U . .
N1 N 0.6642(5) 0.57214(18) 0.9524(3) 0.0552(13) Uani 1 1 d U . .
N21 N 0.6150(4) 0.46945(19) 0.8281(3) 0.0497(13) Uani 1 1 d U B .
O48 O 0.1981(4) 0.47660(17) 0.7929(3) 0.0622(12) Uani 1 1 d U . .
O1A O 0.0343(7) 0.6973(3) 0.5906(7) 0.167(3) Uani 1 1 d U . .
O4 O 0.4591(4) 0.40815(15) 0.8438(3) 0.0522(11) Uani 1 1 d U B .
O81 O 0.4915(3) 0.49481(13) 0.9504(2) 0.0445(10) Uani 1 1 d U . .
O8 O 0.5601(4) 0.60204(16) 0.7952(3) 0.0612(12) Uani 1 1 d U . .
O1 O 0.7089(4) 0.56169(15) 1.0355(3) 0.0604(12) Uani 1 1 d U . .
O28 O 0.6663(4) 0.38675(14) 0.8889(3) 0.0577(12) Uani 1 1 d U . .
O21 O 0.5805(4) 0.50999(15) 0.7997(3) 0.0546(11) Uani 1 1 d U . .
O61 O 0.3289(4) 0.64326(15) 0.7829(3) 0.0651(13) Uani 1 1 d U . .
O62 O 0.1920(5) 0.6357(2) 0.6637(4) 0.0961(18) Uani 1 1 d U . .
O73 O 0.2932(3) 0.54033(13) 0.9609(3) 0.0479(10) Uani 1 1 d U . .
O72 O 0.4489(3) 0.59749(14) 0.9552(2) 0.0483(10) Uani 1 1 d U . .
O71 O 0.3731(3) 0.54160(14) 0.8119(2) 0.0479(10) Uani 1 1 d U . .
O74 O 0.1561(4) 0.57932(18) 0.7855(3) 0.0740(14) Uani 1 1 d DU . .
O19 O 0.2370(4) 0.64084(16) 0.9417(3) 0.0724(14) Uani 1 1 d U . .


_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
Ni3 O81 2.016(4) . ?
Ni3 O1 2.021(4) 3_667 ?
Ni3 N4 2.035(5) . ?
Ni3 O73 2.061(4) . ?
Ni3 O71 2.067(4) . ?
Ni3 O48 2.112(5) . ?
Ni1 N1 2.022(6) . ?
Ni1 O71 2.023(4) . ?
Ni1 O21 2.054(4) . ?
Ni1 O81 2.055(4) . ?
Ni1 O72 2.074(4) . ?
Ni1 O8 2.089(4) . ?
Ni4 O71 2.045(4) . ?
Ni4 O61 2.047(4) . ?
Ni4 O72 2.076(4) . ?
Ni4 O73 2.081(4) . ?
Ni4 O74 2.085(5) . ?
Ni4 O19 2.090(5) . ?
Ni2 N21 2.036(5) . ?
Ni2 O81 2.042(4) . ?
Ni2 O4 2.048(4) . ?
Ni2 O72 2.056(4) 3_667 ?
Ni2 O73 2.109(4) 3_667 ?
Ni2 O28 2.109(4) . ?
C48 O48 1.256(8) . ?
C48 C41 1.458(10) . ?
C48 C49 1.488(10) . ?
C1A O1A 1.461(16) . ?
C41 N4 1.334(8) . ?
C41 C42 1.488(11) . ?
C49 C50 1.379(10) . ?
C49 C54 1.384(11) . ?
C54 C53 1.357(11) . ?
C53 C52 1.375(13) . ?
C52 C51 1.340(12) . ?
C51 C50 1.396(11) . ?
C42 C43A 1.25(5) . ?
C42 C47 1.321(13) . ?
C42 C43 1.49(4) . ?
C47 C46A 1.35(2) . ?
C47 C46 1.65(4) . ?
C46 C45 1.43(5) . ?
C45 C44 1.29(4) . ?
C44 C43 1.39(5) . ?
C46A C45A 1.35(5) . ?
C45A C44A 1.18(5) . ?
C44A C43A 1.55(6) . ?
C8 O8 1.232(8) . ?
C8 C9 1.487(10) . ?
C8 C1 1.509(10) . ?
C1 N1 1.331(8) . ?
C1 C2 1.469(11) . ?
C9 C10 1.364(13) . ?
C9 C14 1.375(12) . ?
C14 C13 1.402(13) . ?
C13 C12 1.399(18) . ?
C12 C11 1.305(19) . ?
C11 C10 1.402(14) . ?
C2 C7 1.354(12) . ?
C2 C3 1.367(13) . ?
C7 C6 1.380(17) . ?
C6 C5 1.33(2) . ?
C5 C4 1.316(19) . ?
C4 C3 1.339(15) . ?
C28 O28 1.267(7) . ?
C28 C21 1.464(9) . ?
C28 C29 1.468(9) . ?
C21 N21 1.326(7) . ?
C21 C22 1.500(8) . ?
C29 C30 1.371(9) . ?
C29 C34 1.404(9) . ?
C34 C33 1.377(10) . ?
C33 C32 1.374(11) . ?
C32 C31 1.383(11) . ?
C31 C30 1.375(10) . ?
C22 C27 1.377(10) . ?
C22 C23 1.394(10) . ?
C27 C26 1.385(12) . ?
C26 C25 1.355(15) . ?
C25 C24 1.373(16) . ?
C24 C23 1.397(11) . ?
C61 O61 1.260(8) . ?
C61 O62 1.274(9) . ?
C61 C62 1.505(10) . ?
C73 O73 1.422(8) . ?
C72 O72 1.449(7) . ?
C71 O71 1.439(6) . ?
C74 O74 1.373(12) . ?
C19 O19 1.41(3) . ?
C19A O19 1.43(3) . ?
C62 C63 1.361(11) . ?
C62 C67 1.386(10) . ?
C63 C64 1.391(12) . ?
C64 C65 1.375(14) . ?
C65 C66 1.336(14) . ?
C66 C67 1.370(12) . ?
N4 O4 1.290(6) . ?
N1 O1 1.301(6) . ?
N21 O21 1.289(6) . ?
O81 O81 1.508(7) 3_667 ?
O1 Ni3 2.021(4) 3_667 ?
O73 Ni2 2.109(4) 3_667 ?
O72 Ni2 2.056(4) 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
O81 Ni3 O1 103.24(17) . 3_667 ?
O81 Ni3 N4 90.28(19) . . ?
O1 Ni3 N4 84.21(19) 3_667 . ?
O81 Ni3 O73 93.72(16) . . ?
O1 Ni3 O73 91.94(17) 3_667 . ?
N4 Ni3 O73 175.0(2) . . ?
O81 Ni3 O71 81.85(16) . . ?
O1 Ni3 O71 172.98(18) 3_667 . ?
N4 Ni3 O71 100.73(18) . . ?
O73 Ni3 O71 82.83(16) . . ?
O81 Ni3 O48 163.98(16) . . ?
O1 Ni3 O48 86.75(18) 3_667 . ?
N4 Ni3 O48 78.2(2) . . ?
O73 Ni3 O48 98.47(18) . . ?
O71 Ni3 O48 89.38(17) . . ?
N1 Ni1 O71 173.40(19) . . ?
N1 Ni1 O21 92.2(2) . . ?
O71 Ni1 O21 92.44(17) . . ?
N1 Ni1 O81 102.86(19) . . ?
O71 Ni1 O81 82.00(16) . . ?
O21 Ni1 O81 88.21(16) . . ?
N1 Ni1 O72 92.43(19) . . ?
O71 Ni1 O72 82.73(16) . . ?
O21 Ni1 O72 174.52(17) . . ?
O81 Ni1 O72 93.65(15) . . ?
N1 Ni1 O8 78.8(2) . . ?
O71 Ni1 O8 97.33(18) . . ?
O21 Ni1 O8 79.89(18) . . ?
O81 Ni1 O8 168.05(16) . . ?
O72 Ni1 O8 98.10(17) . . ?
O71 Ni4 O61 94.03(17) . . ?
O71 Ni4 O72 82.15(16) . . ?
O61 Ni4 O72 94.62(18) . . ?
O71 Ni4 O73 82.86(15) . . ?
O61 Ni4 O73 173.60(19) . . ?
O72 Ni4 O73 79.43(16) . . ?
O71 Ni4 O74 93.60(19) . . ?
O61 Ni4 O74 90.9(2) . . ?
O72 Ni4 O74 173.22(18) . . ?
O73 Ni4 O74 94.84(19) . . ?
O71 Ni4 O19 173.22(16) . . ?
O61 Ni4 O19 91.49(18) . . ?
O72 Ni4 O19 93.50(18) . . ?
O73 Ni4 O19 91.25(17) . . ?
O74 Ni4 O19 90.2(2) . . ?
N21 Ni2 O81 89.00(18) . . ?
N21 Ni2 O4 85.47(19) . . ?
O81 Ni2 O4 92.40(17) . . ?
N21 Ni2 O72 175.4(2) . 3_667 ?
O81 Ni2 O72 95.54(15) . 3_667 ?
O4 Ni2 O72 94.93(17) . 3_667 ?
N21 Ni2 O73 99.90(19) . 3_667 ?
O81 Ni2 O73 93.62(15) . 3_667 ?
O4 Ni2 O73 171.99(17) . 3_667 ?
O72 Ni2 O73 79.24(16) 3_667 3_667 ?
N21 Ni2 O28 77.14(19) . . ?
O81 Ni2 O28 165.50(15) . . ?
O4 Ni2 O28 82.39(18) . . ?
O72 Ni2 O28 98.38(16) 3_667 . ?
O73 Ni2 O28 92.96(17) 3_667 . ?
O48 C48 C41 119.8(6) . . ?
O48 C48 C49 117.6(7) . . ?
C41 C48 C49 122.5(6) . . ?
N4 C41 C48 112.4(6) . . ?
N4 C41 C42 121.7(7) . . ?
C48 C41 C42 125.6(7) . . ?
C50 C49 C54 117.8(8) . . ?
C50 C49 C48 122.6(8) . . ?
C54 C49 C48 119.4(7) . . ?
C53 C54 C49 121.6(9) . . ?
C54 C53 C52 119.3(10) . . ?
C51 C52 C53 121.3(9) . . ?
C52 C51 C50 119.4(9) . . ?
C49 C50 C51 120.5(9) . . ?
C43A C42 C47 111(2) . . ?
C43A C42 C41 129(2) . . ?
C47 C42 C41 119.7(10) . . ?
C43A C42 C43 14(4) . . ?
C47 C42 C43 125(2) . . ?
C41 C42 C43 115.5(19) . . ?
C42 C47 C46A 139.5(18) . . ?
C42 C47 C46 107.9(17) . . ?
C46A C47 C46 33.8(17) . . ?
C45 C46 C47 122(3) . . ?
C44 C45 C46 118(3) . . ?
C45 C44 C43 121(3) . . ?
C44 C43 C42 122(3) . . ?
C47 C46A C45A 102(3) . . ?
C44A C45A C46A 128(4) . . ?
C45A C44A C43A 118(4) . . ?
C42 C43A C44A 116(3) . . ?
O8 C8 C9 119.0(7) . . ?
O8 C8 C1 119.2(6) . . ?
C9 C8 C1 121.7(7) . . ?
N1 C1 C2 121.8(7) . . ?
N1 C1 C8 110.9(6) . . ?
C2 C1 C8 126.8(7) . . ?
C10 C9 C14 118.5(9) . . ?
C10 C9 C8 124.6(9) . . ?
C14 C9 C8 116.7(9) . . ?
C9 C14 C13 120.5(12) . . ?
C12 C13 C14 120.2(13) . . ?
C11 C12 C13 117.4(12) . . ?
C12 C11 C10 124.1(14) . . ?
C9 C10 C11 119.3(12) . . ?
C7 C2 C3 115.7(11) . . ?
C7 C2 C1 119.8(10) . . ?
C3 C2 C1 124.3(9) . . ?
C2 C7 C6 121.4(14) . . ?
C5 C6 C7 120.9(16) . . ?
C4 C5 C6 117.3(17) . . ?
C5 C4 C3 123.7(17) . . ?
C4 C3 C2 120.8(13) . . ?
O28 C28 C21 119.2(6) . . ?
O28 C28 C29 118.1(6) . . ?
C21 C28 C29 122.8(6) . . ?
N21 C21 C28 111.9(5) . . ?
N21 C21 C22 120.5(6) . . ?
C28 C21 C22 127.5(6) . . ?
C30 C29 C34 118.9(7) . . ?
C30 C29 C28 122.5(7) . . ?
C34 C29 C28 118.4(6) . . ?
C33 C34 C29 119.8(8) . . ?
C32 C33 C34 121.2(8) . . ?
C33 C32 C31 118.6(8) . . ?
C30 C31 C32 121.1(8) . . ?
C29 C30 C31 120.5(8) . . ?
C27 C22 C23 118.7(7) . . ?
C27 C22 C21 121.8(7) . . ?
C23 C22 C21 119.5(6) . . ?
C22 C27 C26 121.0(9) . . ?
C25 C26 C27 119.4(10) . . ?
C26 C25 C24 121.8(10) . . ?
C25 C24 C23 118.7(11) . . ?
C22 C23 C24 120.3(9) . . ?
O61 C61 O62 125.4(7) . . ?
O61 C61 C62 117.5(7) . . ?
O62 C61 C62 117.1(7) . . ?
C63 C62 C67 117.8(8) . . ?
C63 C62 C61 121.1(7) . . ?
C67 C62 C61 121.1(8) . . ?
C62 C63 C64 120.4(9) . . ?
C65 C64 C63 119.9(11) . . ?
C66 C65 C64 120.1(10) . . ?
C65 C66 C67 120.2(10) . . ?
C66 C67 C62 121.5(10) . . ?
O4 N4 C41 119.2(6) . . ?
O4 N4 Ni3 123.0(4) . . ?
C41 N4 Ni3 115.4(5) . . ?
O1 N1 C1 116.1(6) . . ?
O1 N1 Ni1 127.2(4) . . ?
C1 N1 Ni1 116.3(5) . . ?
O21 N21 C21 118.6(5) . . ?
O21 N21 Ni2 122.7(4) . . ?
C21 N21 Ni2 117.1(4) . . ?
C48 O48 Ni3 112.2(5) . . ?
N4 O4 Ni2 117.4(3) . . ?
O81 O81 Ni3 112.5(4) 3_667 . ?
O81 O81 Ni2 108.1(3) 3_667 . ?
Ni3 O81 Ni2 113.16(17) . . ?
O81 O81 Ni1 110.3(3) 3_667 . ?
Ni3 O81 Ni1 98.14(16) . . ?
Ni2 O81 Ni1 114.49(19) . . ?
C8 O8 Ni1 112.3(4) . . ?
N1 O1 Ni3 125.8(4) . 3_667 ?
C28 O28 Ni2 113.3(4) . . ?
N21 O21 Ni1 119.7(3) . . ?
C61 O61 Ni4 129.0(5) . . ?
C73 O73 Ni3 115.3(4) . . ?
C73 O73 Ni4 120.0(4) . . ?
Ni3 O73 Ni4 95.87(16) . . ?
C73 O73 Ni2 116.5(4) . 3_667 ?
Ni3 O73 Ni2 108.92(19) . 3_667 ?
Ni4 O73 Ni2 97.17(17) . 3_667 ?
C72 O72 Ni2 114.7(3) . 3_667 ?
C72 O72 Ni1 118.9(4) . . ?
Ni2 O72 Ni1 108.62(18) 3_667 . ?
C72 O72 Ni4 116.9(4) . . ?
Ni2 O72 Ni4 99.03(18) 3_667 . ?
Ni1 O72 Ni4 95.66(16) . . ?
C71 O71 Ni1 116.8(4) . . ?
C71 O71 Ni4 121.1(4) . . ?
Ni1 O71 Ni4 98.21(16) . . ?
C71 O71 Ni3 121.3(4) . . ?
Ni1 O71 Ni3 97.50(16) . . ?
Ni4 O71 Ni3 96.78(16) . . ?
C74 O74 Ni4 137.0(9) . . ?
C19 O19 C19A 20.8(19) . . ?
C19 O19 Ni4 134.6(13) . . ?
C19A O19 Ni4 121.0(11) . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        24.17
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.084
_database_code_depnum_ccdc_archive 'CCDC 894475'
#######################################################################
#
#                 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_brech27
#TrackingRef 'complex3.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'Ni8,(C14 H10 N O2)6,(C7 H4 Cl O)2,O2(C H3 O)6 ,C H4 O)2,H2 0)2'
_chemical_formula_sum            'C106 H98 Cl2 N6 Ni8 O28'
_chemical_formula_weight         2444.48

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'
Cl Cl 0.1484 0.1585 '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'

_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                   13.372(10)
_cell_length_b                   14.701(11)
_cell_length_c                   15.110(11)
_cell_angle_alpha                94.446(6)
_cell_angle_beta                 108.768(13)
_cell_angle_gamma                104.964(10)
_cell_volume                     2675(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    8405
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      28.1

_exptl_crystal_description       Prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1258
_exptl_absorpt_coefficient_mu    1.504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  confocal
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26876
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.54
_diffrn_reflns_theta_max         25.37
_reflns_number_total             9695
_reflns_number_gt                9124
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Corp., 2004)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0933P)²+4.8133P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9695
_refine_ls_number_parameters     676
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0601
_refine_ls_wR_factor_ref         0.1669
_refine_ls_wR_factor_gt          0.1644
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.063
_refine_ls_shift/su_mean         0.002

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 0.03235(4) 0.59954(3) 0.64695(3) 0.03127(15) Uani 1 1 d . . .
Ni2 Ni -0.12026(4) 0.36841(3) 0.53408(3) 0.03190(15) Uani 1 1 d . . .
Ni3 Ni 0.15726(4) 0.46351(3) 0.60225(3) 0.03102(14) Uani 1 1 d . . .
Ni4 Ni 0.27920(4) 0.67707(3) 0.67793(3) 0.03396(15) Uani 1 1 d . . .
O1 O -0.1643(2) 0.6286(2) 0.4999(2) 0.0394(6) Uani 1 1 d . . .
N1 N -0.1022(3) 0.6446(2) 0.5890(2) 0.0360(7) Uani 1 1 d . . .
C1 C -0.1204(3) 0.7040(3) 0.6474(3) 0.0406(9) Uani 1 1 d . . .
C2 C -0.2073(4) 0.7527(4) 0.6137(3) 0.0521(11) Uani 1 1 d . . .
C3 C -0.3168(5) 0.7004(5) 0.5665(5) 0.0754(17) Uani 1 1 d . . .
H3A H -0.3376 0.6325 0.5572 0.091 Uiso 1 1 calc R . .
O4 O -0.0157(2) 0.29836(19) 0.61067(19) 0.0380(6) Uani 1 1 d . . .
N4 N 0.0888(3) 0.3459(2) 0.6477(2) 0.0348(7) Uani 1 1 d . . .
C4 C -0.3962(6) 0.7457(8) 0.5328(6) 0.101(3) Uani 1 1 d . . .
H4A H -0.4709 0.7092 0.4983 0.121 Uiso 1 1 calc R . .
C5 C -0.3667(8) 0.8435(8) 0.5493(6) 0.128(4) Uani 1 1 d . . .
H5A H -0.4218 0.8749 0.5289 0.153 Uiso 1 1 calc R . .
C6 C -0.2610(10) 0.8949(9) 0.5939(8) 0.134(3) Uani 1 1 d U . .
H6A H -0.2417 0.9627 0.6054 0.161 Uiso 1 1 calc R . .
C7 C -0.1772(7) 0.8498(5) 0.6244(7) 0.125(4) Uani 1 1 d . . .
H7A H -0.1015 0.8866 0.6517 0.150 Uiso 1 1 calc R . .
O8 O 0.0442(2) 0.69744(19) 0.7601(2) 0.0371(6) Uani 1 1 d . . .
C8 C -0.0404(3) 0.7226(3) 0.7446(3) 0.0390(9) Uani 1 1 d . . .
C9 C -0.0586(4) 0.7706(3) 0.8249(3) 0.0447(10) Uani 1 1 d . . .
C10 C -0.1630(4) 0.7574(4) 0.8296(4) 0.0646(14) Uani 1 1 d . . .
H10A H -0.2263 0.7183 0.7786 0.077 Uiso 1 1 calc R . .
C11 C -0.1754(5) 0.8010(5) 0.9087(4) 0.0745(17) Uani 1 1 d . . .
H11A H -0.2472 0.7907 0.9121 0.089 Uiso 1 1 calc R . .
C12 C -0.0849(5) 0.8587(5) 0.9817(4) 0.0761(18) Uani 1 1 d . . .
H12A H -0.0940 0.8898 1.0349 0.091 Uiso 1 1 calc R . .
C13 C 0.0197(5) 0.8719(5) 0.9784(4) 0.0770(18) Uani 1 1 d . . .
H13A H 0.0826 0.9113 1.0297 0.092 Uiso 1 1 calc R . .
C14 C 0.0331(4) 0.8278(4) 0.9003(3) 0.0558(12) Uani 1 1 d . . .
H14A H 0.1053 0.8368 0.8983 0.067 Uiso 1 1 calc R . .
O19 O 0.3790(2) 0.7842(2) 0.6354(2) 0.0426(7) Uani 1 1 d . . .
O21 O -0.0515(2) 0.50601(19) 0.7107(2) 0.0390(6) Uani 1 1 d . . .
N21 N -0.1221(3) 0.4257(2) 0.6597(2) 0.0346(7) Uani 1 1 d . . .
C21 C -0.1844(3) 0.3710(3) 0.6992(3) 0.0387(9) Uani 1 1 d . . .
C22 C -0.1746(4) 0.3981(3) 0.7982(3) 0.0507(11) Uani 1 1 d . . .
C23 C -0.1807(5) 0.4884(4) 0.8286(4) 0.0686(16) Uani 1 1 d . . .
H23A H -0.1975 0.5293 0.7840 0.082 Uiso 1 1 calc R . .
C24 C -0.1625(7) 0.5183(5) 0.9225(5) 0.101(3) Uani 1 1 d . . .
H24A H -0.1667 0.5796 0.9423 0.121 Uiso 1 1 calc R . .
C25 C -0.1386(7) 0.4608(6) 0.9866(5) 0.113(3) Uani 1 1 d . . .
H25A H -0.1256 0.4824 1.0514 0.135 Uiso 1 1 calc R . .
C26 C -0.1327(6) 0.3710(6) 0.9596(4) 0.099(3) Uani 1 1 d . . .
H26A H -0.1171 0.3310 1.0055 0.119 Uiso 1 1 calc R . .
C27 C -0.1496(5) 0.3386(4) 0.8643(4) 0.0680(16) Uani 1 1 d . . .
H27A H -0.1442 0.2775 0.8454 0.082 Uiso 1 1 calc R . .
O28 O -0.2443(2) 0.26193(19) 0.5559(2) 0.0386(6) Uani 1 1 d . . .
C28 C -0.2561(3) 0.2824(3) 0.6339(3) 0.0381(9) Uani 1 1 d . . .
C29 C -0.3462(3) 0.2155(3) 0.6542(3) 0.0376(8) Uani 1 1 d . . .
C30 C -0.4046(4) 0.2475(3) 0.7060(3) 0.0448(10) Uani 1 1 d . . .
H30A H -0.3858 0.3136 0.7304 0.054 Uiso 1 1 calc R . .
C31 C -0.4895(4) 0.1823(3) 0.7212(4) 0.0536(11) Uani 1 1 d . . .
H31A H -0.5298 0.2040 0.7554 0.064 Uiso 1 1 calc R . .
C32 C -0.5164(4) 0.0866(4) 0.6874(4) 0.0565(12) Uani 1 1 d . . .
H32A H -0.5744 0.0423 0.6991 0.068 Uiso 1 1 calc R . .
C33 C -0.4590(4) 0.0541(3) 0.6361(4) 0.0522(11) Uani 1 1 d . . .
H33A H -0.4777 -0.0123 0.6129 0.063 Uiso 1 1 calc R . .
C34 C -0.3747(3) 0.1185(3) 0.6190(3) 0.0424(9) Uani 1 1 d . . .
H34A H -0.3361 0.0965 0.5831 0.051 Uiso 1 1 calc R . .
C41 C 0.1588(4) 0.3057(3) 0.7011(3) 0.0454(10) Uani 1 1 d . . .
C42 C 0.1304(5) 0.2061(3) 0.7183(4) 0.0667(16) Uani 1 1 d . . .
C43 C 0.0456(6) 0.1704(5) 0.7459(4) 0.086(2) Uani 1 1 d . . .
H43A H -0.0005 0.2078 0.7535 0.103 Uiso 1 1 calc R . .
C44 C 0.0242(7) 0.0697(5) 0.7649(5) 0.091(2) Uani 1 1 d . . .
H44A H -0.0360 0.0401 0.7837 0.109 Uiso 1 1 calc R . .
C45 C 0.0942(6) 0.0250(5) 0.7539(5) 0.087(2) Uani 1 1 d . . .
H45A H 0.0847 -0.0365 0.7713 0.104 Uiso 1 1 calc R . .
C46 C 0.1793(6) 0.0560(5) 0.7206(6) 0.094(2) Uani 1 1 d . . .
H46A H 0.2221 0.0168 0.7096 0.113 Uiso 1 1 calc R . .
C47 C 0.1968(5) 0.1478(4) 0.7048(5) 0.081(2) Uani 1 1 d . . .
H47A H 0.2560 0.1744 0.6838 0.097 Uiso 1 1 calc R . .
O48 O 0.2985(2) 0.4356(2) 0.6934(2) 0.0403(6) Uani 1 1 d . . .
C48 C 0.2722(4) 0.3687(3) 0.7356(3) 0.0423(9) Uani 1 1 d . . .
C49 C 0.3576(4) 0.3579(3) 0.8229(3) 0.0508(11) Uani 1 1 d . . .
C50 C 0.3302(5) 0.3229(4) 0.8963(4) 0.0720(17) Uani 1 1 d . . .
H50A H 0.2546 0.3011 0.8904 0.086 Uiso 1 1 calc R . .
C51 C 0.4125(7) 0.3192(5) 0.9797(4) 0.091(2) Uani 1 1 d . . .
H51A H 0.3930 0.2962 1.0308 0.109 Uiso 1 1 calc R . .
C52 C 0.5218(6) 0.3487(5) 0.9876(5) 0.085(2) Uani 1 1 d . . .
H52A H 0.5774 0.3436 1.0432 0.102 Uiso 1 1 calc R . .
C53 C 0.5513(6) 0.3857(5) 0.9155(5) 0.084(2) Uani 1 1 d . . .
H53A H 0.6272 0.4075 0.9223 0.101 Uiso 1 1 calc R . .
C54 C 0.4692(4) 0.3911(4) 0.8317(4) 0.0652(14) Uani 1 1 d . . .
H54A H 0.4890 0.4170 0.7819 0.078 Uiso 1 1 calc R . .
O61 O 0.3120(2) 0.7644(2) 0.8005(2) 0.0416(7) Uani 1 1 d . . .
C61 C 0.3397(3) 0.8544(3) 0.8166(3) 0.0405(9) Uani 1 1 d . . .
O62 O 0.3655(4) 0.9069(2) 0.7610(3) 0.0661(10) Uani 1 1 d . . .
C62 C 0.3416(3) 0.9015(3) 0.9089(3) 0.0392(9) Uani 1 1 d . . .
C63 C 0.3231(4) 0.8490(3) 0.9767(3) 0.0435(9) Uani 1 1 d . . .
H63A H 0.3102 0.7817 0.9652 0.052 Uiso 1 1 calc R . .
C64 C 0.3228(4) 0.8922(3) 1.0610(3) 0.0515(11) Uani 1 1 d . . .
H64A H 0.3113 0.8554 1.1078 0.062 Uiso 1 1 calc R . .
Cl65 Cl 0.33184(15) 1.04439(11) 1.17968(10) 0.0722(4) Uani 1 1 d . . .
C65 C 0.3396(4) 0.9890(3) 1.0763(3) 0.0501(11) Uani 1 1 d . . .
C66 C 0.3622(4) 1.0444(3) 1.0112(4) 0.0549(12) Uani 1 1 d . . .
H66A H 0.3764 1.1117 1.0237 0.066 Uiso 1 1 calc R . .
C67 C 0.3641(4) 1.0010(3) 0.9284(3) 0.0486(10) Uani 1 1 d . . .
H67A H 0.3807 1.0387 0.8837 0.058 Uiso 1 1 calc R . .
O71 O 0.1760(2) 0.56783(19) 0.70978(18) 0.0326(6) Uani 1 1 d . . .
C71 C 0.1974(4) 0.5528(3) 0.8057(3) 0.0391(9) Uani 1 1 d . . .
H71A H 0.2034 0.6112 0.8455 0.059 Uiso 1 1 calc R . .
H71B H 0.2669 0.5366 0.8290 0.059 Uiso 1 1 calc R . .
H71C H 0.1366 0.5001 0.8082 0.059 Uiso 1 1 calc R . .
O72 O 0.1307(2) 0.69535(18) 0.59465(19) 0.0336(6) Uani 1 1 d . . .
C72 C 0.1189(4) 0.7922(3) 0.5990(4) 0.0555(12) Uani 1 1 d . . .
H72A H 0.0450 0.7896 0.5562 0.083 Uiso 1 1 calc R . .
H72B H 0.1752 0.8339 0.5796 0.083 Uiso 1 1 calc R . .
H72C H 0.1285 0.8176 0.6641 0.083 Uiso 1 1 calc R . .
O73 O 0.2361(2) 0.57791(19) 0.55653(19) 0.0337(6) Uani 1 1 d . . .
C73 C 0.3218(4) 0.5638(4) 0.5240(4) 0.0535(11) Uani 1 1 d . . .
H73A H 0.2888 0.5152 0.4663 0.080 Uiso 1 1 calc R . .
H73B H 0.3743 0.5424 0.5734 0.080 Uiso 1 1 calc R . .
H73C H 0.3608 0.6241 0.5103 0.080 Uiso 1 1 calc R . .
O74 O 0.4143(2) 0.6271(2) 0.7503(2) 0.0448(7) Uani 1 1 d . . .
C74 C 0.5247(4) 0.6651(4) 0.7537(4) 0.0644(14) Uani 1 1 d . . .
H74A H 0.5712 0.6300 0.7914 0.097 Uiso 1 1 calc R . .
H74B H 0.5530 0.7328 0.7830 0.097 Uiso 1 1 calc R . .
H74C H 0.5261 0.6586 0.6891 0.097 Uiso 1 1 calc R . .
O81 O 0.0077(2) 0.48494(19) 0.54712(18) 0.0324(6) 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
Ni1 N1 2.033(4) . ?
Ni1 O71 2.041(3) . ?
Ni1 O21 2.045(3) . ?
Ni1 O72 2.055(3) . ?
Ni1 O81 2.055(3) . ?
Ni1 O8 2.084(3) . ?
Ni2 N21 2.026(4) . ?
Ni2 O81 2.029(3) . ?
Ni2 O72 2.039(3) 2_566 ?
Ni2 O4 2.060(3) . ?
Ni2 O73 2.081(3) 2_566 ?
Ni2 O28 2.098(3) . ?
Ni3 O1 2.015(3) 2_566 ?
Ni3 N4 2.018(3) . ?
Ni3 O81 2.022(3) . ?
Ni3 O73 2.037(3) . ?
Ni3 O71 2.051(3) . ?
Ni3 O48 2.109(3) . ?
Ni4 O61 2.022(3) . ?
Ni4 O71 2.030(3) . ?
Ni4 O73 2.072(3) . ?
Ni4 O19 2.073(3) . ?
Ni4 O72 2.078(3) . ?
Ni4 O74 2.130(3) . ?
O1 N1 1.300(4) . ?
O1 Ni3 2.015(3) 2_566 ?
N1 C1 1.316(5) . ?
C1 C8 1.467(6) . ?
C1 C2 1.493(6) . ?
C2 C7 1.359(9) . ?
C2 C3 1.380(8) . ?
C3 C4 1.379(9) . ?
C3 H3A 0.9500 . ?
O4 N4 1.298(4) . ?
N4 C41 1.322(5) . ?
C4 C5 1.369(13) . ?
C4 H4A 0.9500 . ?
C5 C6 1.334(14) . ?
C5 H5A 0.9500 . ?
C6 C7 1.417(12) . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9500 . ?
O8 C8 1.237(5) . ?
C8 C9 1.475(6) . ?
C9 C10 1.385(7) . ?
C9 C14 1.389(7) . ?
C10 C11 1.390(7) . ?
C10 H10A 0.9500 . ?
C11 C12 1.366(8) . ?
C11 H11A 0.9500 . ?
C12 C13 1.379(8) . ?
C12 H12A 0.9500 . ?
C13 C14 1.388(7) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
O21 N21 1.301(4) . ?
N21 C21 1.321(5) . ?
C21 C28 1.461(6) . ?
C21 C22 1.472(6) . ?
C22 C27 1.395(8) . ?
C22 C23 1.402(8) . ?
C23 C24 1.375(8) . ?
C23 H23A 0.9500 . ?
C24 C25 1.351(12) . ?
C24 H24A 0.9500 . ?
C25 C26 1.380(12) . ?
C25 H25A 0.9500 . ?
C26 C27 1.407(9) . ?
C26 H26A 0.9500 . ?
C27 H27A 0.9500 . ?
O28 C28 1.262(5) . ?
C28 C29 1.479(5) . ?
C29 C34 1.390(6) . ?
C29 C30 1.403(6) . ?
C30 C31 1.378(6) . ?
C30 H30A 0.9500 . ?
C31 C32 1.371(7) . ?
C31 H31A 0.9500 . ?
C32 C33 1.390(7) . ?
C32 H32A 0.9500 . ?
C33 C34 1.382(6) . ?
C33 H33A 0.9500 . ?
C34 H34A 0.9500 . ?
C41 C48 1.457(6) . ?
C41 C42 1.481(6) . ?
C42 C43 1.329(10) . ?
C42 C47 1.432(9) . ?
C43 C44 1.502(9) . ?
C43 H43A 0.9500 . ?
C44 C45 1.318(11) . ?
C44 H44A 0.9500 . ?
C45 C46 1.376(11) . ?
C45 H45A 0.9500 . ?
C46 C47 1.362(9) . ?
C46 H46A 0.9500 . ?
C47 H47A 0.9500 . ?
O48 C48 1.249(5) . ?
C48 C49 1.491(6) . ?
C49 C50 1.372(8) . ?
C49 C54 1.403(8) . ?
C50 C51 1.397(8) . ?
C50 H50A 0.9500 . ?
C51 C52 1.375(11) . ?
C51 H51A 0.9500 . ?
C52 C53 1.376(11) . ?
C52 H52A 0.9500 . ?
C53 C54 1.408(8) . ?
C53 H53A 0.9500 . ?
C54 H54A 0.9500 . ?
O61 C61 1.259(5) . ?
C61 O62 1.252(5) . ?
C61 C62 1.498(6) . ?
C62 C63 1.376(6) . ?
C62 C67 1.402(6) . ?
C63 C64 1.381(7) . ?
C63 H63A 0.9500 . ?
C64 C65 1.372(7) . ?
C64 H64A 0.9500 . ?
Cl65 C65 1.750(5) . ?
C65 C66 1.383(7) . ?
C66 C67 1.370(7) . ?
C66 H66A 0.9500 . ?
C67 H67A 0.9500 . ?
O71 C71 1.430(5) . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
O72 C72 1.472(6) . ?
O72 Ni2 2.039(3) 2_566 ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
O73 C73 1.438(5) . ?
O73 Ni2 2.081(3) 2_566 ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
O74 C74 1.419(6) . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
O81 O81 1.491(5) 2_566 ?

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 Ni1 O71 174.49(12) . . ?
N1 Ni1 O21 91.16(13) . . ?
O71 Ni1 O21 92.31(12) . . ?
N1 Ni1 O72 93.60(13) . . ?
O71 Ni1 O72 82.69(12) . . ?
O21 Ni1 O72 174.23(11) . . ?
N1 Ni1 O81 102.89(12) . . ?
O71 Ni1 O81 81.52(11) . . ?
O21 Ni1 O81 87.94(12) . . ?
O72 Ni1 O81 94.16(11) . . ?
N1 Ni1 O8 78.33(13) . . ?
O71 Ni1 O8 97.94(11) . . ?
O21 Ni1 O8 81.83(12) . . ?
O72 Ni1 O8 95.94(12) . . ?
O81 Ni1 O8 169.73(10) . . ?
N21 Ni2 O81 88.53(12) . . ?
N21 Ni2 O72 175.59(12) . 2_566 ?
O81 Ni2 O72 95.55(11) . 2_566 ?
N21 Ni2 O4 87.06(13) . . ?
O81 Ni2 O4 92.34(12) . . ?
O72 Ni2 O4 94.42(12) 2_566 . ?
N21 Ni2 O73 98.80(13) . 2_566 ?
O81 Ni2 O73 92.85(11) . 2_566 ?
O72 Ni2 O73 79.37(12) 2_566 2_566 ?
O4 Ni2 O73 172.27(11) . 2_566 ?
N21 Ni2 O28 77.46(12) . . ?
O81 Ni2 O28 165.70(11) . . ?
O72 Ni2 O28 98.54(11) 2_566 . ?
O4 Ni2 O28 84.22(12) . . ?
O73 Ni2 O28 92.10(12) 2_566 . ?
O1 Ni3 N4 85.69(14) 2_566 . ?
O1 Ni3 O81 105.00(12) 2_566 . ?
N4 Ni3 O81 90.51(13) . . ?
O1 Ni3 O73 91.55(12) 2_566 . ?
N4 Ni3 O73 175.56(12) . . ?
O81 Ni3 O73 93.56(11) . . ?
O1 Ni3 O71 170.91(11) 2_566 . ?
N4 Ni3 O71 100.16(13) . . ?
O81 Ni3 O71 82.05(11) . . ?
O73 Ni3 O71 82.17(12) . . ?
O1 Ni3 O48 86.38(12) 2_566 . ?
N4 Ni3 O48 78.24(13) . . ?
O81 Ni3 O48 163.48(11) . . ?
O73 Ni3 O48 98.14(12) . . ?
O71 Ni3 O48 88.00(12) . . ?
O61 Ni4 O71 92.80(12) . . ?
O61 Ni4 O73 174.65(11) . . ?
O71 Ni4 O73 81.85(12) . . ?
O61 Ni4 O19 90.93(13) . . ?
O71 Ni4 O19 175.96(11) . . ?
O73 Ni4 O19 94.42(12) . . ?
O61 Ni4 O72 100.71(12) . . ?
O71 Ni4 O72 82.40(12) . . ?
O73 Ni4 O72 78.68(11) . . ?
O19 Ni4 O72 95.41(12) . . ?
O61 Ni4 O74 88.33(13) . . ?
O71 Ni4 O74 89.09(13) . . ?
O73 Ni4 O74 91.55(12) . . ?
O19 Ni4 O74 92.55(13) . . ?
O72 Ni4 O74 167.82(11) . . ?
N1 O1 Ni3 124.8(2) . 2_566 ?
O1 N1 C1 117.2(3) . . ?
O1 N1 Ni1 127.0(3) . . ?
C1 N1 Ni1 115.4(3) . . ?
N1 C1 C8 112.6(4) . . ?
N1 C1 C2 122.0(4) . . ?
C8 C1 C2 125.1(4) . . ?
C7 C2 C3 119.6(6) . . ?
C7 C2 C1 119.5(5) . . ?
C3 C2 C1 120.8(5) . . ?
C4 C3 C2 120.6(7) . . ?
C4 C3 H3A 119.7 . . ?
C2 C3 H3A 119.7 . . ?
N4 O4 Ni2 116.9(2) . . ?
O4 N4 C41 119.3(3) . . ?
O4 N4 Ni3 122.8(2) . . ?
C41 N4 Ni3 115.9(3) . . ?
C3 C4 C5 119.6(8) . . ?
C3 C4 H4A 120.2 . . ?
C5 C4 H4A 120.2 . . ?
C6 C5 C4 120.3(8) . . ?
C6 C5 H5A 119.9 . . ?
C4 C5 H5A 119.9 . . ?
C5 C6 C7 120.9(10) . . ?
C5 C6 H6A 119.5 . . ?
C7 C6 H6A 119.5 . . ?
C2 C7 C6 118.7(8) . . ?
C2 C7 H7A 120.6 . . ?
C6 C7 H7A 120.7 . . ?
C8 O8 Ni1 112.1(3) . . ?
O8 C8 C1 119.7(4) . . ?
O8 C8 C9 119.0(4) . . ?
C1 C8 C9 121.4(4) . . ?
C10 C9 C14 119.0(4) . . ?
C10 C9 C8 122.5(4) . . ?
C14 C9 C8 118.4(4) . . ?
C9 C10 C11 120.3(5) . . ?
C9 C10 H10A 119.8 . . ?
C11 C10 H10A 119.9 . . ?
C12 C11 C10 120.2(5) . . ?
C12 C11 H11A 119.9 . . ?
C10 C11 H11A 119.9 . . ?
C11 C12 C13 120.1(5) . . ?
C11 C12 H12A 119.9 . . ?
C13 C12 H12A 119.9 . . ?
C12 C13 C14 120.1(5) . . ?
C12 C13 H13A 120.0 . . ?
C14 C13 H13A 120.0 . . ?
C13 C14 C9 120.2(5) . . ?
C13 C14 H14A 119.9 . . ?
C9 C14 H14A 119.9 . . ?
N21 O21 Ni1 118.8(2) . . ?
O21 N21 C21 118.0(3) . . ?
O21 N21 Ni2 123.2(2) . . ?
C21 N21 Ni2 117.7(3) . . ?
N21 C21 C28 111.2(4) . . ?
N21 C21 C22 121.8(4) . . ?
C28 C21 C22 126.9(4) . . ?
C27 C22 C23 119.2(5) . . ?
C27 C22 C21 120.8(5) . . ?
C23 C22 C21 119.7(4) . . ?
C24 C23 C22 120.6(7) . . ?
C24 C23 H23A 119.7 . . ?
C22 C23 H23A 119.7 . . ?
C25 C24 C23 120.3(7) . . ?
C25 C24 H24A 119.9 . . ?
C23 C24 H24A 119.9 . . ?
C24 C25 C26 121.0(6) . . ?
C24 C25 H25A 119.5 . . ?
C26 C25 H25A 119.5 . . ?
C25 C26 C27 120.2(7) . . ?
C25 C26 H26A 119.9 . . ?
C27 C26 H26A 119.9 . . ?
C22 C27 C26 118.7(7) . . ?
C22 C27 H27A 120.7 . . ?
C26 C27 H27A 120.7 . . ?
C28 O28 Ni2 112.8(2) . . ?
O28 C28 C21 120.1(4) . . ?
O28 C28 C29 117.6(4) . . ?
C21 C28 C29 122.2(4) . . ?
C34 C29 C30 119.6(4) . . ?
C34 C29 C28 118.5(4) . . ?
C30 C29 C28 121.9(4) . . ?
C31 C30 C29 119.5(4) . . ?
C31 C30 H30A 120.2 . . ?
C29 C30 H30A 120.2 . . ?
C32 C31 C30 120.7(5) . . ?
C32 C31 H31A 119.6 . . ?
C30 C31 H31A 119.6 . . ?
C31 C32 C33 120.2(4) . . ?
C31 C32 H32A 119.9 . . ?
C33 C32 H32A 119.9 . . ?
C34 C33 C32 119.9(4) . . ?
C34 C33 H33A 120.0 . . ?
C32 C33 H33A 120.0 . . ?
C33 C34 C29 120.0(4) . . ?
C33 C34 H34A 120.0 . . ?
C29 C34 H34A 120.0 . . ?
N4 C41 C48 111.8(4) . . ?
N4 C41 C42 125.6(4) . . ?
C48 C41 C42 122.4(4) . . ?
C43 C42 C47 119.9(6) . . ?
C43 C42 C41 121.6(6) . . ?
C47 C42 C41 118.5(6) . . ?
C42 C43 C44 118.5(8) . . ?
C42 C43 H43A 120.8 . . ?
C44 C43 H43A 120.8 . . ?
C45 C44 C43 115.8(8) . . ?
C45 C44 H44A 122.1 . . ?
C43 C44 H44A 122.1 . . ?
C44 C45 C46 128.4(7) . . ?
C44 C45 H45A 115.8 . . ?
C46 C45 H45A 115.8 . . ?
C47 C46 C45 114.0(8) . . ?
C47 C46 H46A 123.0 . . ?
C45 C46 H46A 123.0 . . ?
C46 C47 C42 123.3(8) . . ?
C46 C47 H47A 118.4 . . ?
C42 C47 H47A 118.4 . . ?
C48 O48 Ni3 111.2(3) . . ?
O48 C48 C41 119.7(4) . . ?
O48 C48 C49 118.7(4) . . ?
C41 C48 C49 121.6(4) . . ?
C50 C49 C54 119.9(5) . . ?
C50 C49 C48 121.8(5) . . ?
C54 C49 C48 118.2(5) . . ?
C49 C50 C51 120.6(7) . . ?
C49 C50 H50A 119.7 . . ?
C51 C50 H50A 119.7 . . ?
C52 C51 C50 119.8(7) . . ?
C52 C51 H51A 120.1 . . ?
C50 C51 H51A 120.1 . . ?
C53 C52 C51 120.6(6) . . ?
C53 C52 H52A 119.7 . . ?
C51 C52 H52A 119.7 . . ?
C52 C53 C54 120.1(7) . . ?
C52 C53 H53A 120.0 . . ?
C54 C53 H53A 120.0 . . ?
C49 C54 C53 119.1(6) . . ?
C49 C54 H54A 120.5 . . ?
C53 C54 H54A 120.5 . . ?
C61 O61 Ni4 128.1(3) . . ?
O62 C61 O61 124.6(4) . . ?
O62 C61 C62 118.0(4) . . ?
O61 C61 C62 117.3(4) . . ?
C63 C62 C67 118.6(4) . . ?
C63 C62 C61 121.2(4) . . ?
C67 C62 C61 120.2(4) . . ?
C62 C63 C64 121.1(4) . . ?
C62 C63 H63A 119.4 . . ?
C64 C63 H63A 119.4 . . ?
C65 C64 C63 119.0(4) . . ?
C65 C64 H64A 120.5 . . ?
C63 C64 H64A 120.5 . . ?
C64 C65 C66 121.2(4) . . ?
C64 C65 Cl65 119.9(4) . . ?
C66 C65 Cl65 118.9(4) . . ?
C67 C66 C65 119.2(4) . . ?
C67 C66 H66A 120.4 . . ?
C65 C66 H66A 120.4 . . ?
C66 C67 C62 120.6(4) . . ?
C66 C67 H67A 119.7 . . ?
C62 C67 H67A 119.7 . . ?
C71 O71 Ni4 120.8(2) . . ?
C71 O71 Ni1 115.6(2) . . ?
Ni4 O71 Ni1 97.70(12) . . ?
C71 O71 Ni3 122.5(2) . . ?
Ni4 O71 Ni3 97.56(12) . . ?
Ni1 O71 Ni3 97.65(12) . . ?
O71 C71 H71A 109.5 . . ?
O71 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
O71 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C72 O72 Ni2 115.8(3) . 2_566 ?
C72 O72 Ni1 116.1(3) . . ?
Ni2 O72 Ni1 108.72(13) 2_566 . ?
C72 O72 Ni4 118.8(3) . . ?
Ni2 O72 Ni4 98.86(12) 2_566 . ?
Ni1 O72 Ni4 95.73(12) . . ?
O72 C72 H72A 109.5 . . ?
O72 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
O72 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C73 O73 Ni3 114.8(3) . . ?
C73 O73 Ni4 119.0(3) . . ?
Ni3 O73 Ni4 96.67(12) . . ?
C73 O73 Ni2 116.1(3) . 2_566 ?
Ni3 O73 Ni2 109.85(13) . 2_566 ?
Ni4 O73 Ni2 97.71(12) . 2_566 ?
O73 C73 H73A 109.5 . . ?
O73 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
O73 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C74 O74 Ni4 125.1(3) . . ?
O74 C74 H74A 109.5 . . ?
O74 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
O74 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
O81 O81 Ni3 110.9(2) 2_566 . ?
O81 O81 Ni2 109.3(2) 2_566 . ?
Ni3 O81 Ni2 113.10(13) . . ?
O81 O81 Ni1 109.7(2) 2_566 . ?
Ni3 O81 Ni1 98.16(11) . . ?
Ni2 O81 Ni1 115.27(13) . . ?

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
Ni3 O1 N1 C1 -177.2(3) 2_566 . . . ?
Ni3 O1 N1 Ni1 10.2(4) 2_566 . . . ?
O71 Ni1 N1 O1 120.9(12) . . . . ?
O21 Ni1 N1 O1 -110.0(3) . . . . ?
O72 Ni1 N1 O1 73.3(3) . . . . ?
O81 Ni1 N1 O1 -21.9(3) . . . . ?
O8 Ni1 N1 O1 168.6(3) . . . . ?
O71 Ni1 N1 C1 -51.9(13) . . . . ?
O21 Ni1 N1 C1 77.3(3) . . . . ?
O72 Ni1 N1 C1 -99.5(3) . . . . ?
O81 Ni1 N1 C1 165.4(3) . . . . ?
O8 Ni1 N1 C1 -4.2(3) . . . . ?
O1 N1 C1 C8 -175.6(3) . . . . ?
Ni1 N1 C1 C8 -2.1(5) . . . . ?
O1 N1 C1 C2 -0.9(6) . . . . ?
Ni1 N1 C1 C2 172.5(3) . . . . ?
N1 C1 C2 C7 -117.6(7) . . . . ?
C8 C1 C2 C7 56.3(8) . . . . ?
N1 C1 C2 C3 58.3(7) . . . . ?
C8 C1 C2 C3 -127.8(5) . . . . ?
C7 C2 C3 C4 -2.0(11) . . . . ?
C1 C2 C3 C4 -177.9(6) . . . . ?
N21 Ni2 O4 N4 -83.4(3) . . . . ?
O81 Ni2 O4 N4 5.0(3) . . . . ?
O72 Ni2 O4 N4 100.8(3) 2_566 . . . ?
O73 Ni2 O4 N4 137.1(7) 2_566 . . . ?
O28 Ni2 O4 N4 -161.1(3) . . . . ?
Ni2 O4 N4 C41 177.0(3) . . . . ?
Ni2 O4 N4 Ni3 -19.4(4) . . . . ?
O1 Ni3 N4 O4 -82.6(3) 2_566 . . . ?
O81 Ni3 N4 O4 22.4(3) . . . . ?
O73 Ni3 N4 O4 -134.2(14) . . . . ?
O71 Ni3 N4 O4 104.4(3) . . . . ?
O48 Ni3 N4 O4 -169.8(3) . . . . ?
O1 Ni3 N4 C41 81.5(3) 2_566 . . . ?
O81 Ni3 N4 C41 -173.5(3) . . . . ?
O73 Ni3 N4 C41 29.9(17) . . . . ?
O71 Ni3 N4 C41 -91.4(3) . . . . ?
O48 Ni3 N4 C41 -5.7(3) . . . . ?
C2 C3 C4 C5 -2.4(12) . . . . ?
C3 C4 C5 C6 3.1(15) . . . . ?
C4 C5 C6 C7 0.5(17) . . . . ?
C3 C2 C7 C6 5.5(13) . . . . ?
C1 C2 C7 C6 -178.6(8) . . . . ?
C5 C6 C7 C2 -4.9(17) . . . . ?
N1 Ni1 O8 C8 10.8(3) . . . . ?
O71 Ni1 O8 C8 -173.3(3) . . . . ?
O21 Ni1 O8 C8 -82.1(3) . . . . ?
O72 Ni1 O8 C8 103.2(3) . . . . ?
O81 Ni1 O8 C8 -87.1(7) . . . . ?
Ni1 O8 C8 C1 -15.8(5) . . . . ?
Ni1 O8 C8 C9 164.0(3) . . . . ?
N1 C1 C8 O8 12.5(6) . . . . ?
C2 C1 C8 O8 -161.9(4) . . . . ?
N1 C1 C8 C9 -167.3(4) . . . . ?
C2 C1 C8 C9 18.3(7) . . . . ?
O8 C8 C9 C10 -145.0(5) . . . . ?
C1 C8 C9 C10 34.7(7) . . . . ?
O8 C8 C9 C14 32.1(6) . . . . ?
C1 C8 C9 C14 -148.2(4) . . . . ?
C14 C9 C10 C11 0.1(9) . . . . ?
C8 C9 C10 C11 177.3(5) . . . . ?
C9 C10 C11 C12 1.1(11) . . . . ?
C10 C11 C12 C13 -1.7(12) . . . . ?
C11 C12 C13 C14 1.0(11) . . . . ?
C12 C13 C14 C9 0.3(10) . . . . ?
C10 C9 C14 C13 -0.9(8) . . . . ?
C8 C9 C14 C13 -178.1(5) . . . . ?
N1 Ni1 O21 N21 78.1(3) . . . . ?
O71 Ni1 O21 N21 -106.2(3) . . . . ?
O72 Ni1 O21 N21 -136.2(10) . . . . ?
O81 Ni1 O21 N21 -24.7(3) . . . . ?
O8 Ni1 O21 N21 156.1(3) . . . . ?
Ni1 O21 N21 C21 -172.7(3) . . . . ?
Ni1 O21 N21 Ni2 20.0(4) . . . . ?
O81 Ni2 N21 O21 -2.5(3) . . . . ?
O72 Ni2 N21 O21 -160.3(14) 2_566 . . . ?
O4 Ni2 N21 O21 89.9(3) . . . . ?
O73 Ni2 N21 O21 -95.2(3) 2_566 . . . ?
O28 Ni2 N21 O21 174.6(3) . . . . ?
O81 Ni2 N21 C21 -169.9(3) . . . . ?
O72 Ni2 N21 C21 32.3(17) 2_566 . . . ?
O4 Ni2 N21 C21 -77.5(3) . . . . ?
O73 Ni2 N21 C21 97.4(3) 2_566 . . . ?
O28 Ni2 N21 C21 7.2(3) . . . . ?
O21 N21 C21 C28 -178.0(3) . . . . ?
Ni2 N21 C21 C28 -10.0(5) . . . . ?
O21 N21 C21 C22 -0.7(6) . . . . ?
Ni2 N21 C21 C22 167.4(3) . . . . ?
N21 C21 C22 C27 -122.0(5) . . . . ?
C28 C21 C22 C27 54.9(7) . . . . ?
N21 C21 C22 C23 52.3(7) . . . . ?
C28 C21 C22 C23 -130.8(5) . . . . ?
C27 C22 C23 C24 -0.1(9) . . . . ?
C21 C22 C23 C24 -174.5(5) . . . . ?
C22 C23 C24 C25 -0.1(11) . . . . ?
C23 C24 C25 C26 -0.5(13) . . . . ?
C24 C25 C26 C27 1.2(12) . . . . ?
C23 C22 C27 C26 0.8(8) . . . . ?
C21 C22 C27 C26 175.1(5) . . . . ?
C25 C26 C27 C22 -1.3(10) . . . . ?
N21 Ni2 O28 C28 -2.5(3) . . . . ?
O81 Ni2 O28 C28 9.1(6) . . . . ?
O72 Ni2 O28 C28 179.4(3) 2_566 . . . ?
O4 Ni2 O28 C28 85.8(3) . . . . ?
O73 Ni2 O28 C28 -101.1(3) 2_566 . . . ?
Ni2 O28 C28 C21 -2.1(5) . . . . ?
Ni2 O28 C28 C29 176.1(3) . . . . ?
N21 C21 C28 O28 7.9(6) . . . . ?
C22 C21 C28 O28 -169.3(4) . . . . ?
N21 C21 C28 C29 -170.1(4) . . . . ?
C22 C21 C28 C29 12.7(7) . . . . ?
O28 C28 C29 C34 32.4(6) . . . . ?
C21 C28 C29 C34 -149.5(4) . . . . ?
O28 C28 C29 C30 -146.2(4) . . . . ?
C21 C28 C29 C30 31.9(6) . . . . ?
C34 C29 C30 C31 0.0(7) . . . . ?
C28 C29 C30 C31 178.6(4) . . . . ?
C29 C30 C31 C32 0.9(8) . . . . ?
C30 C31 C32 C33 -0.8(8) . . . . ?
C31 C32 C33 C34 -0.1(8) . . . . ?
C32 C33 C34 C29 1.0(7) . . . . ?
C30 C29 C34 C33 -0.9(7) . . . . ?
C28 C29 C34 C33 -179.6(4) . . . . ?
O4 N4 C41 C48 179.3(3) . . . . ?
Ni3 N4 C41 C48 14.6(5) . . . . ?
O4 N4 C41 C42 4.5(7) . . . . ?
Ni3 N4 C41 C42 -160.2(4) . . . . ?
N4 C41 C42 C43 -50.4(8) . . . . ?
C48 C41 C42 C43 135.4(5) . . . . ?
N4 C41 C42 C47 129.8(5) . . . . ?
C48 C41 C42 C47 -44.5(7) . . . . ?
C47 C42 C43 C44 1.8(8) . . . . ?
C41 C42 C43 C44 -178.1(5) . . . . ?
C42 C43 C44 C45 1.2(9) . . . . ?
C43 C44 C45 C46 -5.3(12) . . . . ?
C44 C45 C46 C47 5.8(12) . . . . ?
C45 C46 C47 C42 -2.1(10) . . . . ?
C43 C42 C47 C46 -1.3(9) . . . . ?
C41 C42 C47 C46 178.6(6) . . . . ?
O1 Ni3 O48 C48 -92.1(3) 2_566 . . . ?
N4 Ni3 O48 C48 -5.8(3) . . . . ?
O81 Ni3 O48 C48 42.2(5) . . . . ?
O73 Ni3 O48 C48 176.8(3) . . . . ?
O71 Ni3 O48 C48 95.0(3) . . . . ?
Ni3 O48 C48 C41 15.9(5) . . . . ?
Ni3 O48 C48 C49 -161.7(3) . . . . ?
N4 C41 C48 O48 -21.0(6) . . . . ?
C42 C41 C48 O48 154.0(5) . . . . ?
N4 C41 C48 C49 156.6(4) . . . . ?
C42 C41 C48 C49 -28.4(7) . . . . ?
O48 C48 C49 C50 147.6(5) . . . . ?
C41 C48 C49 C50 -30.0(7) . . . . ?
O48 C48 C49 C54 -27.7(6) . . . . ?
C41 C48 C49 C54 154.7(4) . . . . ?
C54 C49 C50 C51 -0.7(9) . . . . ?
C48 C49 C50 C51 -175.9(5) . . . . ?
C49 C50 C51 C52 -1.4(10) . . . . ?
C50 C51 C52 C53 2.6(10) . . . . ?
C51 C52 C53 C54 -1.7(10) . . . . ?
C50 C49 C54 C53 1.6(8) . . . . ?
C48 C49 C54 C53 177.0(5) . . . . ?
C52 C53 C54 C49 -0.5(9) . . . . ?
O71 Ni4 O61 C61 -152.6(3) . . . . ?
O73 Ni4 O61 C61 -152.9(11) . . . . ?
O19 Ni4 O61 C61 25.8(4) . . . . ?
O72 Ni4 O61 C61 -69.9(4) . . . . ?
O74 Ni4 O61 C61 118.4(4) . . . . ?
Ni4 O61 C61 O62 -9.5(7) . . . . ?
Ni4 O61 C61 C62 170.4(3) . . . . ?
O62 C61 C62 C63 -174.6(4) . . . . ?
O61 C61 C62 C63 5.4(6) . . . . ?
O62 C61 C62 C67 4.4(6) . . . . ?
O61 C61 C62 C67 -175.5(4) . . . . ?
C67 C62 C63 C64 2.1(7) . . . . ?
C61 C62 C63 C64 -178.8(4) . . . . ?
C62 C63 C64 C65 1.1(7) . . . . ?
C63 C64 C65 C66 -3.4(8) . . . . ?
C63 C64 C65 Cl65 176.4(4) . . . . ?
C64 C65 C66 C67 2.4(8) . . . . ?
Cl65 C65 C66 C67 -177.4(4) . . . . ?
C65 C66 C67 C62 1.0(8) . . . . ?
C63 C62 C67 C66 -3.2(7) . . . . ?
C61 C62 C67 C66 177.7(4) . . . . ?
O61 Ni4 O71 C71 -34.8(3) . . . . ?
O73 Ni4 O71 C71 145.2(3) . . . . ?
O19 Ni4 O71 C71 167.5(15) . . . . ?
O72 Ni4 O71 C71 -135.2(3) . . . . ?
O74 Ni4 O71 C71 53.5(3) . . . . ?
O61 Ni4 O71 Ni1 91.19(13) . . . . ?
O73 Ni4 O71 Ni1 -88.83(12) . . . . ?
O19 Ni4 O71 Ni1 -66.5(16) . . . . ?
O72 Ni4 O71 Ni1 -9.25(11) . . . . ?
O74 Ni4 O71 Ni1 179.48(12) . . . . ?
O61 Ni4 O71 Ni3 -169.98(12) . . . . ?
O73 Ni4 O71 Ni3 10.00(11) . . . . ?
O19 Ni4 O71 Ni3 32.3(17) . . . . ?
O72 Ni4 O71 Ni3 89.58(12) . . . . ?
O74 Ni4 O71 Ni3 -81.69(13) . . . . ?
N1 Ni1 O71 C71 90.9(12) . . . . ?
O21 Ni1 O71 C71 -38.2(3) . . . . ?
O72 Ni1 O71 C71 138.9(3) . . . . ?
O81 Ni1 O71 C71 -125.7(3) . . . . ?
O8 Ni1 O71 C71 43.9(3) . . . . ?
N1 Ni1 O71 Ni4 -38.6(13) . . . . ?
O21 Ni1 O71 Ni4 -167.75(11) . . . . ?
O72 Ni1 O71 Ni4 9.35(11) . . . . ?
O81 Ni1 O71 Ni4 104.69(12) . . . . ?
O8 Ni1 O71 Ni4 -85.68(13) . . . . ?
N1 Ni1 O71 Ni3 -137.4(12) . . . . ?
O21 Ni1 O71 Ni3 93.50(13) . . . . ?
O72 Ni1 O71 Ni3 -89.40(12) . . . . ?
O81 Ni1 O71 Ni3 5.94(9) . . . . ?
O8 Ni1 O71 Ni3 175.57(10) . . . . ?
O1 Ni3 O71 C71 -97.6(7) 2_566 . . . ?
N4 Ni3 O71 C71 31.9(3) . . . . ?
O81 Ni3 O71 C71 121.0(3) . . . . ?
O73 Ni3 O71 C71 -144.3(3) . . . . ?
O48 Ni3 O71 C71 -45.8(3) . . . . ?
O1 Ni3 O71 Ni4 36.5(7) 2_566 . . . ?
N4 Ni3 O71 Ni4 166.01(12) . . . . ?
O81 Ni3 O71 Ni4 -104.90(12) . . . . ?
O73 Ni3 O71 Ni4 -10.17(11) . . . . ?
O48 Ni3 O71 Ni4 88.33(13) . . . . ?
O1 Ni3 O71 Ni1 135.4(7) 2_566 . . . ?
N4 Ni3 O71 Ni1 -95.11(13) . . . . ?
O81 Ni3 O71 Ni1 -6.03(10) . . . . ?
O73 Ni3 O71 Ni1 88.71(12) . . . . ?
O48 Ni3 O71 Ni1 -172.79(12) . . . . ?
N1 Ni1 O72 C72 40.8(3) . . . . ?
O71 Ni1 O72 C72 -135.1(3) . . . . ?
O21 Ni1 O72 C72 -104.8(11) . . . . ?
O81 Ni1 O72 C72 144.0(3) . . . . ?
O8 Ni1 O72 C72 -37.8(3) . . . . ?
N1 Ni1 O72 Ni2 -91.80(15) . . . 2_566 ?
O71 Ni1 O72 Ni2 92.30(14) . . . 2_566 ?
O21 Ni1 O72 Ni2 122.6(11) . . . 2_566 ?
O81 Ni1 O72 Ni2 11.42(14) . . . 2_566 ?
O8 Ni1 O72 Ni2 -170.42(12) . . . 2_566 ?
N1 Ni1 O72 Ni4 166.81(12) . . . . ?
O71 Ni1 O72 Ni4 -9.09(10) . . . . ?
O21 Ni1 O72 Ni4 21.2(11) . . . . ?
O81 Ni1 O72 Ni4 -89.97(12) . . . . ?
O8 Ni1 O72 Ni4 88.19(12) . . . . ?
O61 Ni4 O72 C72 41.7(3) . . . . ?
O71 Ni4 O72 C72 133.2(3) . . . . ?
O73 Ni4 O72 C72 -143.7(3) . . . . ?
O19 Ni4 O72 C72 -50.2(3) . . . . ?
O74 Ni4 O72 C72 179.2(5) . . . . ?
O61 Ni4 O72 Ni2 167.71(11) . . . 2_566 ?
O71 Ni4 O72 Ni2 -100.86(12) . . . 2_566 ?
O73 Ni4 O72 Ni2 -17.70(11) . . . 2_566 ?
O19 Ni4 O72 Ni2 75.73(13) . . . 2_566 ?
O74 Ni4 O72 Ni2 -54.9(6) . . . 2_566 ?
O61 Ni4 O72 Ni1 -82.28(13) . . . . ?
O71 Ni4 O72 Ni1 9.15(11) . . . . ?
O73 Ni4 O72 Ni1 92.30(12) . . . . ?
O19 Ni4 O72 Ni1 -174.26(11) . . . . ?
O74 Ni4 O72 Ni1 55.1(6) . . . . ?
O1 Ni3 O73 C73 -37.2(3) 2_566 . . . ?
N4 Ni3 O73 C73 14.3(16) . . . . ?
O81 Ni3 O73 C73 -142.3(3) . . . . ?
O71 Ni3 O73 C73 136.2(3) . . . . ?
O48 Ni3 O73 C73 49.4(3) . . . . ?
O1 Ni3 O73 Ni4 -163.46(12) 2_566 . . . ?
N4 Ni3 O73 Ni4 -112.0(15) . . . . ?
O81 Ni3 O73 Ni4 91.40(11) . . . . ?
O71 Ni3 O73 Ni4 9.94(11) . . . . ?
O48 Ni3 O73 Ni4 -76.90(12) . . . . ?
O1 Ni3 O73 Ni2 95.83(14) 2_566 . . 2_566 ?
N4 Ni3 O73 Ni2 147.3(15) . . . 2_566 ?
O81 Ni3 O73 Ni2 -9.30(14) . . . 2_566 ?
O71 Ni3 O73 Ni2 -90.77(14) . . . 2_566 ?
O48 Ni3 O73 Ni2 -177.61(12) . . . 2_566 ?
O61 Ni4 O73 C73 -133.1(12) . . . . ?
O71 Ni4 O73 C73 -133.3(3) . . . . ?
O19 Ni4 O73 C73 48.2(3) . . . . ?
O72 Ni4 O73 C73 142.9(3) . . . . ?
O74 Ni4 O73 C73 -44.4(3) . . . . ?
O61 Ni4 O73 Ni3 -9.8(13) . . . . ?
O71 Ni4 O73 Ni3 -10.05(11) . . . . ?
O19 Ni4 O73 Ni3 171.49(11) . . . . ?
O72 Ni4 O73 Ni3 -93.87(12) . . . . ?
O74 Ni4 O73 Ni3 78.81(13) . . . . ?
O61 Ni4 O73 Ni2 101.3(12) . . . 2_566 ?
O71 Ni4 O73 Ni2 101.10(13) . . . 2_566 ?
O19 Ni4 O73 Ni2 -77.36(13) . . . 2_566 ?
O72 Ni4 O73 Ni2 17.28(10) . . . 2_566 ?
O74 Ni4 O73 Ni2 -170.04(12) . . . 2_566 ?
O61 Ni4 O74 C74 -92.8(4) . . . . ?
O71 Ni4 O74 C74 174.4(4) . . . . ?
O73 Ni4 O74 C74 92.6(4) . . . . ?
O19 Ni4 O74 C74 -1.9(4) . . . . ?
O72 Ni4 O74 C74 128.9(6) . . . . ?
O1 Ni3 O81 O81 -53.4(3) 2_566 . . 2_566 ?
N4 Ni3 O81 O81 -139.0(3) . . . 2_566 ?
O73 Ni3 O81 O81 39.2(3) . . . 2_566 ?
O71 Ni3 O81 O81 120.8(3) . . . 2_566 ?
O48 Ni3 O81 O81 174.3(3) . . . 2_566 ?
O1 Ni3 O81 Ni2 69.85(15) 2_566 . . . ?
N4 Ni3 O81 Ni2 -15.83(14) . . . . ?
O73 Ni3 O81 Ni2 162.41(13) . . . . ?
O71 Ni3 O81 Ni2 -116.01(14) . . . . ?
O48 Ni3 O81 Ni2 -62.5(4) . . . . ?
O1 Ni3 O81 Ni1 -168.15(10) 2_566 . . . ?
N4 Ni3 O81 Ni1 106.18(13) . . . . ?
O73 Ni3 O81 Ni1 -75.59(12) . . . . ?
O71 Ni3 O81 Ni1 5.99(10) . . . . ?
O48 Ni3 O81 Ni1 59.5(4) . . . . ?
N21 Ni2 O81 O81 -139.3(3) . . . 2_566 ?
O72 Ni2 O81 O81 39.0(3) 2_566 . . 2_566 ?
O4 Ni2 O81 O81 133.7(3) . . . 2_566 ?
O73 Ni2 O81 O81 -40.5(3) 2_566 . . 2_566 ?
O28 Ni2 O81 O81 -150.6(4) . . . 2_566 ?
N21 Ni2 O81 Ni3 96.64(15) . . . . ?
O72 Ni2 O81 Ni3 -85.03(14) 2_566 . . . ?
O4 Ni2 O81 Ni3 9.64(14) . . . . ?
O73 Ni2 O81 Ni3 -164.63(13) 2_566 . . . ?
O28 Ni2 O81 Ni3 85.3(5) . . . . ?
N21 Ni2 O81 Ni1 -15.20(15) . . . . ?
O72 Ni2 O81 Ni1 163.13(13) 2_566 . . . ?
O4 Ni2 O81 Ni1 -102.19(14) . . . . ?
O73 Ni2 O81 Ni1 83.54(14) 2_566 . . . ?
O28 Ni2 O81 Ni1 -26.6(5) . . . . ?
N1 Ni1 O81 O81 54.9(3) . . . 2_566 ?
O71 Ni1 O81 O81 -121.8(3) . . . 2_566 ?
O21 Ni1 O81 O81 145.6(3) . . . 2_566 ?
O72 Ni1 O81 O81 -39.8(3) . . . 2_566 ?
O8 Ni1 O81 O81 150.5(5) . . . 2_566 ?
N1 Ni1 O81 Ni3 170.60(11) . . . . ?
O71 Ni1 O81 Ni3 -6.03(10) . . . . ?
O21 Ni1 O81 Ni3 -98.68(12) . . . . ?
O72 Ni1 O81 Ni3 75.94(12) . . . . ?
O8 Ni1 O81 Ni3 -93.7(6) . . . . ?
N1 Ni1 O81 Ni2 -69.01(16) . . . . ?
O71 Ni1 O81 Ni2 114.37(15) . . . . ?
O21 Ni1 O81 Ni2 21.72(14) . . . . ?
O72 Ni1 O81 Ni2 -163.67(13) . . . . ?
O8 Ni1 O81 Ni2 26.7(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.459
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.108
_database_code_depnum_ccdc_archive 'CCDC 894476'
#######################################################################
#
#                 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_eb1089
#TrackingRef 'complex4.cif'

_audit_creation_date             12-07-19
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'eb1089 in P-1'
_chemical_name_systematic        ?
_chemical_melting_point          ?
_chemical_compound_source        G.Papaefstathiou

_exptl_crystal_recrystallization_method 
;
Et2O diffusion of a MeOH/DCM solution.
;
#end of refcif
_cell_length_a                   12.8976(6)
_cell_length_b                   13.0924(6)
_cell_length_c                   16.4651(6)
_cell_angle_alpha                98.686(3)
_cell_angle_beta                 99.661(3)
_cell_angle_gamma                90.904(3)
_cell_volume                     2707.0(2)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni -3.0029 0.5091 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            1

# Given Formula = C122 Cl2 N10 Ni5 O24
# Dc = 1.44 Fooo = 1204.00 Mu = 20.79 M = 1176.93
# Found Formula = C117 H112 Cl2 N8 Ni5 O20
# Dc = 1.42 FOOO = 1204.00 Mu = 20.07 M = 1157.34

_chemical_formula_sum            'C117 H112 Cl2 N8 Ni5 O20'
_chemical_formula_moiety         '[Ni5(aboH)6(abo)2].4MeOH.1CH2Cl2'
_chemical_formula_weight         2314.67


_cell_measurement_temperature    150.0
_cell_measurement_reflns_used    23087
_cell_measurement_theta_min      2.7544
_cell_measurement_theta_max      73.8570

_exptl_crystal_description       Block
_exptl_crystal_colour            Orange
_exptl_crystal_size_min          0.03
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_max          0.04

_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             1204
_exptl_absorpt_coefficient_mu    2.007

# Sheldrick geometric approximatio 0.92 0.94
_exptl_absorpt_correction_T_min  0.63551
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      150.0
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_reflns_number            54794
_reflns_number_total             9656
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_sigmaI/netI    0.1107

# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 9656
# Theoretical number of reflections is about 21969


_diffrn_reflns_theta_min         2.756
_diffrn_reflns_theta_max         73.953
_diffrn_measured_fraction_theta_max 0.881

_diffrn_reflns_theta_full        73.953
_diffrn_measured_fraction_theta_full 0.881


_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       20
_reflns_limit_h_min              -16
_reflns_limit_h_max              15
_reflns_limit_k_min              -16
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              20

_oxford_diffrn_Wilson_B_factor   2.87
_oxford_diffrn_Wilson_scale      0.09

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.74
_refine_diff_density_max         1.71


# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold


# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         9648
_refine_ls_number_restraints     2
_refine_ls_number_parameters     700
_oxford_refine_ls_R_factor_ref   0.0829
_refine_ls_wR_factor_ref         0.2087
_refine_ls_goodness_of_fit_ref   0.9640
_refine_ls_shift/su_max          0.0053546
_refine_ls_shift/su_mean         0.0000614


# The values computed with all filters except I/sigma
_oxford_reflns_number_all        9648
_refine_ls_R_factor_all          0.0829
_refine_ls_wR_factor_all         0.2087

# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7753
_refine_ls_R_factor_gt           0.0686
_refine_ls_wR_factor_gt          0.1827

# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    'see above notes' #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)]
where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)²]²
Ai are:
0.390E+04 0.651E+04 0.406E+04 0.173E+04 383.
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ni1 Ni 0.5000 0.0000 0.5000 0.0285 1.0000 Uani S . . . . .
Ni2 Ni 0.55065(5) -0.07340(5) 0.31415(4) 0.0285 1.0000 Uani . . . . . .
Ni3 Ni 0.51086(5) 0.10341(5) 0.23205(4) 0.0301 1.0000 Uani . . . . . .
Cl1 Cl 0.1431(3) -0.3333(3) 0.1949(3) 0.0899 0.5000 Uani D . . . . .
Cl2 Cl 0.1150(4) -0.5113(5) 0.0694(3) 0.1323 0.5000 Uani D . . . . .
O3 O 0.4910(2) -0.1080(2) 0.41367(17) 0.0325 1.0000 Uani . . . . . .
O13 O 0.3588(2) -0.0373(2) 0.60566(16) 0.0324 1.0000 Uani . . . . . .
O21 O 0.5948(2) -0.0077(2) 0.21638(17) 0.0316 1.0000 Uani . . . . . .
O25 O 0.6029(2) 0.2765(2) 0.1832(2) 0.0406 1.0000 Uani . . . . . .
O38 O 0.4229(2) 0.0203(2) 0.27325(17) 0.0325 1.0000 Uani . . . . . .
O48 O 0.4349(2) 0.3006(2) 0.23275(19) 0.0377 1.0000 Uani . . . . . .
O55 O 0.6573(2) -0.1912(2) 0.30972(19) 0.0442 1.0000 Uani . . . . . .
O65 O 0.3793(3) -0.1724(3) 0.1818(2) 0.0573 1.0000 Uani . . . . . .
O75 O 0.8186(3) -0.1946(3) 0.4309(3) 0.0694 1.0000 Uani . . . . . .
O77 O 0.8477(3) 0.0090(3) 0.4394(4) 0.0909 1.0000 Uani . . . . . .
N12 N 0.3994(2) -0.0733(2) 0.53636(19) 0.0297 1.0000 Uani . . . . . .
N24 N 0.6110(3) 0.1761(3) 0.1932(2) 0.0336 1.0000 Uani . . . . . .
N47 N 0.4202(3) 0.2067(3) 0.2535(2) 0.0335 1.0000 Uani . . . . . .
N64 N 0.4762(3) -0.1899(3) 0.2268(2) 0.0335 1.0000 Uani . . . . . .
C4 C 0.4193(3) -0.1896(3) 0.4166(2) 0.0329 1.0000 Uani . . . . . .
C5 C 0.4743(3) -0.2916(3) 0.4202(2) 0.0321 1.0000 Uani . . . . . .
C6 C 0.5718(3) -0.2938(3) 0.4718(3) 0.0383 1.0000 Uani . . . . . .
C7 C 0.6206(4) -0.3873(4) 0.4760(3) 0.0445 1.0000 Uani . . . . . .
C8 C 0.5736(4) -0.4780(3) 0.4303(3) 0.0443 1.0000 Uani . . . . . .
C9 C 0.4769(4) -0.4768(3) 0.3800(3) 0.0414 1.0000 Uani . . . . . .
C10 C 0.4274(3) -0.3839(3) 0.3745(3) 0.0369 1.0000 Uani . . . . . .
C11 C 0.3662(3) -0.1627(3) 0.4923(2) 0.0318 1.0000 Uani . . . . . .
C14 C 0.2889(3) -0.2351(3) 0.5125(3) 0.0372 1.0000 Uani . . . . . .
C15 C 0.2931(4) -0.2537(4) 0.5942(3) 0.0505 1.0000 Uani . . . . . .
C16 C 0.2271(5) -0.3273(4) 0.6131(4) 0.0685 1.0000 Uani . . . . . .
C17 C 0.1526(5) -0.3813(4) 0.5486(5) 0.0763 1.0000 Uani . . . . . .
C18 C 0.1477(4) -0.3631(4) 0.4676(5) 0.0663 1.0000 Uani . . . . . .
C19 C 0.2146(4) -0.2901(4) 0.4490(3) 0.0487 1.0000 Uani . . . . . .
C22 C 0.6895(3) 0.0147(3) 0.1901(2) 0.0319 1.0000 Uani . . . . . .
C23 C 0.6930(3) 0.1271(3) 0.1773(3) 0.0345 1.0000 Uani . . . . . .
C26 C 0.7805(4) 0.1719(3) 0.1448(3) 0.0455 1.0000 Uani . . . . . .
C27 C 0.8822(5) 0.1786(6) 0.1902(5) 0.0801 1.0000 Uani . . . . . .
C28 C 0.9639(6) 0.2168(7) 0.1560(7) 0.1075 1.0000 Uani . . . . . .
C29 C 0.9461(8) 0.2477(6) 0.0802(9) 0.1212 1.0000 Uani . . . . . .
C30 C 0.8454(8) 0.2375(8) 0.0354(9) 0.1489 1.0000 Uani . . . . . .
C31 C 0.7623(6) 0.1996(7) 0.0662(5) 0.0958 1.0000 Uani . . . . . .
C32 C 0.6987(3) -0.0549(3) 0.1086(3) 0.0337 1.0000 Uani . . . . . .
C33 C 0.7966(4) -0.0740(4) 0.0866(3) 0.0446 1.0000 Uani . . . . . .
C34 C 0.8056(4) -0.1352(4) 0.0113(3) 0.0561 1.0000 Uani . . . . . .
C35 C 0.7179(5) -0.1785(4) -0.0419(3) 0.0543 1.0000 Uani . . . . . .
C36 C 0.6198(5) -0.1596(4) -0.0200(3) 0.0545 1.0000 Uani . . . . . .
C37 C 0.6103(4) -0.0974(4) 0.0540(3) 0.0459 1.0000 Uani . . . . . .
C39 C 0.3435(3) 0.0756(3) 0.3102(2) 0.0315 1.0000 Uani . . . . . .
C40 C 0.2395(3) 0.0148(3) 0.2804(3) 0.0368 1.0000 Uani . . . . . .
C41 C 0.1910(4) 0.0049(4) 0.1978(3) 0.0475 1.0000 Uani . . . . . .
C42 C 0.0972(4) -0.0533(5) 0.1702(4) 0.0686 1.0000 Uani . . . . . .
C43 C 0.0532(5) -0.1027(5) 0.2277(5) 0.0776 1.0000 Uani . . . . . .
C44 C 0.1022(4) -0.0935(5) 0.3089(5) 0.0727 1.0000 Uani . . . . . .
C45 C 0.1953(4) -0.0360(4) 0.3354(4) 0.0496 1.0000 Uani . . . . . .
C46 C 0.3416(3) 0.1848(3) 0.2885(2) 0.0317 1.0000 Uani . . . . . .
C49 C 0.2568(3) 0.2548(3) 0.3080(3) 0.0349 1.0000 Uani . . . . . .
C50 C 0.1952(3) 0.2328(4) 0.3652(3) 0.0436 1.0000 Uani . . . . . .
C51 C 0.1115(4) 0.2945(4) 0.3816(3) 0.0506 1.0000 Uani . . . . . .
C52 C 0.0889(4) 0.3787(4) 0.3423(4) 0.0535 1.0000 Uani . . . . . .
C53 C 0.1506(4) 0.4029(4) 0.2863(4) 0.0544 1.0000 Uani . . . . . .
C54 C 0.2344(3) 0.3423(3) 0.2688(3) 0.0421 1.0000 Uani . . . . . .
C56 C 0.6152(4) -0.2948(4) 0.2679(3) 0.0489 1.0000 Uani . . . . . .
C57 C 0.7008(3) -0.3494(3) 0.2267(2) 0.0349 1.0000 Uani . . . . . .
C58 C 0.7229(5) -0.4502(5) 0.2417(4) 0.0628 1.0000 Uani . . . . . .
C59 C 0.8053(5) -0.5042(5) 0.2084(4) 0.0679 1.0000 Uani . . . . . .
C60 C 0.8580(5) -0.4520(4) 0.1629(4) 0.0632 1.0000 Uani . . . . . .
C61 C 0.8383(5) -0.3512(5) 0.1470(4) 0.0660 1.0000 Uani . . . . . .
C62 C 0.7591(4) -0.3016(5) 0.1797(3) 0.0602 1.0000 Uani . . . . . .
C63 C 0.5165(4) -0.2751(4) 0.2065(3) 0.0429 1.0000 Uani . . . . . .
C66 C 0.4678(4) -0.3600(3) 0.1397(3) 0.0435 1.0000 Uani . . . . . .
C67 C 0.4307(4) -0.3380(4) 0.0601(3) 0.0474 1.0000 Uani . . . . . .
C68 C 0.3824(5) -0.4161(4) -0.0021(3) 0.0576 1.0000 Uani . . . . . .
C69 C 0.3697(5) -0.5136(5) 0.0147(3) 0.0651 1.0000 Uani . . . . . .
C70 C 0.4071(5) -0.5371(4) 0.0940(3) 0.0605 1.0000 Uani . . . . . .
C71 C 0.4567(4) -0.4595(4) 0.1558(3) 0.0520 1.0000 Uani . . . . . .
C73 C 0.1862(10) -0.4183(8) 0.1316(8) 0.1112 0.5000 Uani D . . . . .
C76 C 0.8954(5) -0.2565(5) 0.4004(4) 0.0702 1.0000 Uani . . . . . .
C78 C 0.9188(4) 0.0724(5) 0.4191(5) 0.0712 1.0000 Uani . . . . . .
H41 H 0.3670 -0.1972 0.3678 0.0389 1.0000 Uiso R . . . . .
H61 H 0.6043 -0.2317 0.5040 0.0459 1.0000 Uiso R . . . . .
H71 H 0.6874 -0.3884 0.5105 0.0527 1.0000 Uiso R . . . . .
H81 H 0.6076 -0.5414 0.4338 0.0530 1.0000 Uiso R . . . . .
H91 H 0.4441 -0.5394 0.3490 0.0498 1.0000 Uiso R . . . . .
H101 H 0.3611 -0.3833 0.3394 0.0441 1.0000 Uiso R . . . . .
H151 H 0.3422 -0.2146 0.6377 0.0602 1.0000 Uiso R . . . . .
H161 H 0.2323 -0.3415 0.6685 0.0824 1.0000 Uiso R . . . . .
H171 H 0.1046 -0.4305 0.5606 0.0923 1.0000 Uiso R . . . . .
H181 H 0.0977 -0.4013 0.4242 0.0787 1.0000 Uiso R . . . . .
H191 H 0.2104 -0.2775 0.3933 0.0577 1.0000 Uiso R . . . . .
H221 H 0.7469 0.0039 0.2318 0.0383 1.0000 Uiso R . . . . .
H271 H 0.8959 0.1571 0.2434 0.0955 1.0000 Uiso R . . . . .
H281 H 1.0336 0.2216 0.1865 0.1288 1.0000 Uiso R . . . . .
H291 H 1.0019 0.2759 0.0583 0.1439 1.0000 Uiso R . . . . .
H301 H 0.8327 0.2570 -0.0186 0.1811 1.0000 Uiso R . . . . .
H311 H 0.6934 0.1930 0.0341 0.1129 1.0000 Uiso R . . . . .
H331 H 0.8583 -0.0449 0.1233 0.0538 1.0000 Uiso R . . . . .
H341 H 0.8732 -0.1468 -0.0031 0.0676 1.0000 Uiso R . . . . .
H351 H 0.7241 -0.2211 -0.0928 0.0653 1.0000 Uiso R . . . . .
H361 H 0.5582 -0.1895 -0.0564 0.0650 1.0000 Uiso R . . . . .
H371 H 0.5424 -0.0838 0.0673 0.0551 1.0000 Uiso R . . . . .
H391 H 0.3609 0.0800 0.3691 0.0375 1.0000 Uiso R . . . . .
H411 H 0.2222 0.0379 0.1597 0.0565 1.0000 Uiso R . . . . .
H421 H 0.0632 -0.0592 0.1137 0.0818 1.0000 Uiso R . . . . .
H431 H -0.0108 -0.1428 0.2098 0.0927 1.0000 Uiso R . . . . .
H441 H 0.0718 -0.1268 0.3472 0.0873 1.0000 Uiso R . . . . .
H451 H 0.2294 -0.0309 0.3917 0.0595 1.0000 Uiso R . . . . .
H501 H 0.2100 0.1751 0.3933 0.0520 1.0000 Uiso R . . . . .
H511 H 0.0698 0.2781 0.4206 0.0606 1.0000 Uiso R . . . . .
H521 H 0.0314 0.4198 0.3533 0.0642 1.0000 Uiso R . . . . .
H531 H 0.1357 0.4616 0.2594 0.0650 1.0000 Uiso R . . . . .
H541 H 0.2765 0.3601 0.2305 0.0506 1.0000 Uiso R . . . . .
H561 H 0.5959 -0.3334 0.3078 0.0598 1.0000 Uiso R . . . . .
H581 H 0.6823 -0.4828 0.2744 0.0765 1.0000 Uiso R . . . . .
H591 H 0.8219 -0.5723 0.2180 0.0816 1.0000 Uiso R . . . . .
H601 H 0.9132 -0.4860 0.1397 0.0752 1.0000 Uiso R . . . . .
H611 H 0.8786 -0.3183 0.1143 0.0805 1.0000 Uiso R . . . . .
H621 H 0.7440 -0.2333 0.1700 0.0726 1.0000 Uiso R . . . . .
H671 H 0.4382 -0.2697 0.0482 0.0567 1.0000 Uiso R . . . . .
H681 H 0.3577 -0.4013 -0.0566 0.0678 1.0000 Uiso R . . . . .
H691 H 0.3360 -0.5663 -0.0281 0.0778 1.0000 Uiso R . . . . .
H701 H 0.3982 -0.6053 0.1056 0.0719 1.0000 Uiso R . . . . .
H711 H 0.4831 -0.4752 0.2097 0.0617 1.0000 Uiso R . . . . .
H731 H 0.2386 -0.4518 0.1646 0.1311 0.5000 Uiso R . . . . .
H732 H 0.2183 -0.3811 0.0965 0.1311 0.5000 Uiso R . . . . .
H750 H 0.7667 -0.1936 0.3917 0.0833 1.0000 Uiso R . . . . .
H770 H 0.7825 0.0180 0.4251 0.1070 1.0000 Uiso R . . . . .
H650 H 0.3255 -0.2092 0.1847 0.0682 1.0000 Uiso R . . . . .
H781 H 0.9878 0.0527 0.4392 0.0856 1.0000 Uiso R . . . . .
H782 H 0.9096 0.1414 0.4437 0.0856 1.0000 Uiso R . . . . .
H783 H 0.9090 0.0682 0.3602 0.0856 1.0000 Uiso R . . . . .
H761 H 0.9537 -0.2580 0.4439 0.0834 1.0000 Uiso R . . . . .
H762 H 0.8668 -0.3248 0.3808 0.0834 1.0000 Uiso R . . . . .
H763 H 0.9180 -0.2286 0.3560 0.0834 1.0000 Uiso R . . . . .
H481 H 0.4870 0.3129 0.2097 0.0447 1.0000 Uiso R . . . . .
H252 H 0.6539 0.3122 0.2147 0.0489 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          3.92(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 . O3 2_656 1.834(2) yes
Ni1 . N12 2_656 1.832(3) yes
Ni1 . O3 . 1.834(2) yes
Ni1 . N12 . 1.832(3) yes
Ni2 . O13 2_656 2.015(3) yes
Ni2 . O3 . 2.029(3) yes
Ni2 . O21 . 2.090(3) yes
Ni2 . O38 . 2.148(3) yes
Ni2 . O55 . 2.083(3) yes
Ni2 . N64 . 2.036(3) yes
Ni3 . O21 . 1.839(3) yes
Ni3 . O38 . 1.837(3) yes
Ni3 . N24 . 1.846(3) yes
Ni3 . N47 . 1.834(3) yes
Cl1 . C73 . 1.581(9) yes
Cl2 . C73 . 1.627(8) yes
O3 . C4 . 1.414(5) yes
O13 . N12 . 1.358(4) yes
O21 . C22 . 1.404(5) yes
O25 . N24 . 1.352(5) yes
O25 . H252 . 0.850 no
O38 . C39 . 1.429(4) yes
O48 . N47 . 1.343(4) yes
O48 . H481 . 0.850 no
O55 . C56 . 1.477(5) yes
O65 . N64 . 1.382(4) yes
O65 . H650 . 0.850 no
O75 . C76 . 1.399(7) yes
O75 . H750 . 0.850 no
O77 . C78 . 1.343(8) yes
O77 . H770 . 0.850 no
N12 . C11 . 1.305(5) yes
N24 . C23 . 1.289(5) yes
N47 . C46 . 1.296(5) yes
N64 . C63 . 1.261(6) yes
C4 . C5 . 1.526(5) yes
C4 . C11 . 1.519(5) yes
C4 . H41 . 0.950 no
C5 . C6 . 1.398(6) yes
C5 . C10 . 1.393(5) yes
C6 . C7 . 1.392(6) yes
C6 . H61 . 0.950 no
C7 . C8 . 1.378(6) yes
C7 . H71 . 0.950 no
C8 . C9 . 1.378(7) yes
C8 . H81 . 0.950 no
C9 . C10 . 1.391(6) yes
C9 . H91 . 0.950 no
C10 . H101 . 0.950 no
C11 . C14 . 1.476(6) yes
C14 . C15 . 1.395(7) yes
C14 . C19 . 1.394(6) yes
C15 . C16 . 1.380(7) yes
C15 . H151 . 0.950 no
C16 . C17 . 1.400(9) yes
C16 . H161 . 0.950 no
C17 . C18 . 1.382(10) yes
C17 . H171 . 0.950 no
C18 . C19 . 1.380(8) yes
C18 . H181 . 0.950 no
C19 . H191 . 0.950 no
C22 . C23 . 1.519(6) yes
C22 . C32 . 1.527(5) yes
C22 . H221 . 0.950 no
C23 . C26 . 1.476(6) yes
C26 . C27 . 1.390(8) yes
C26 . C31 . 1.380(9) yes
C27 . C28 . 1.395(11) yes
C27 . H271 . 0.950 no
C28 . C29 . 1.353(15) yes
C28 . H281 . 0.950 no
C29 . C30 . 1.376(17) yes
C29 . H291 . 0.950 no
C30 . C31 . 1.377(10) yes
C30 . H301 . 0.950 no
C31 . H311 . 0.950 no
C32 . C33 . 1.387(6) yes
C32 . C37 . 1.379(6) yes
C33 . C34 . 1.394(6) yes
C33 . H331 . 0.950 no
C34 . C35 . 1.366(8) yes
C34 . H341 . 0.950 no
C35 . C36 . 1.389(8) yes
C35 . H351 . 0.950 no
C36 . C37 . 1.384(7) yes
C36 . H361 . 0.950 no
C37 . H371 . 0.950 no
C39 . C40 . 1.517(5) yes
C39 . C46 . 1.524(6) yes
C39 . H391 . 0.950 no
C40 . C41 . 1.384(7) yes
C40 . C45 . 1.390(7) yes
C41 . C42 . 1.391(7) yes
C41 . H411 . 0.950 no
C42 . C43 . 1.411(10) yes
C42 . H421 . 0.950 no
C43 . C44 . 1.366(10) yes
C43 . H431 . 0.950 no
C44 . C45 . 1.376(8) yes
C44 . H441 . 0.950 no
C45 . H451 . 0.950 no
C46 . C49 . 1.484(5) yes
C49 . C50 . 1.389(7) yes
C49 . C54 . 1.408(6) yes
C50 . C51 . 1.397(6) yes
C50 . H501 . 0.950 no
C51 . C52 . 1.371(8) yes
C51 . H511 . 0.950 no
C52 . C53 . 1.382(8) yes
C52 . H521 . 0.950 no
C53 . C54 . 1.394(6) yes
C53 . H531 . 0.950 no
C54 . H541 . 0.950 no
C56 . C57 . 1.523(6) yes
C56 . C63 . 1.538(7) yes
C56 . H561 . 0.950 no
C57 . C58 . 1.404(7) yes
C57 . C62 . 1.372(8) yes
C58 . C59 . 1.425(8) yes
C58 . H581 . 0.950 no
C59 . C60 . 1.343(9) yes
C59 . H591 . 0.950 no
C60 . C61 . 1.403(9) yes
C60 . H601 . 0.950 no
C61 . C62 . 1.361(8) yes
C61 . H611 . 0.950 no
C62 . H621 . 0.950 no
C63 . C66 . 1.489(5) yes
C66 . C67 . 1.392(7) yes
C66 . C71 . 1.377(7) yes
C67 . C68 . 1.390(6) yes
C67 . H671 . 0.950 no
C68 . C69 . 1.358(8) yes
C68 . H681 . 0.950 no
C69 . C70 . 1.396(8) yes
C69 . H691 . 0.950 no
C70 . C71 . 1.388(7) yes
C70 . H701 . 0.950 no
C71 . H711 . 0.950 no
C73 . H731 . 0.950 no
C73 . H732 . 0.950 no
C76 . H761 . 0.950 no
C76 . H762 . 0.950 no
C76 . H763 . 0.950 no
C78 . H781 . 0.950 no
C78 . H782 . 0.950 no
C78 . H783 . 0.950 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 2_656 Ni1 . N12 2_656 85.76(13) yes
O3 2_656 Ni1 . O3 . 179.994 yes
N12 2_656 Ni1 . O3 . 94.24(13) yes
O3 2_656 Ni1 . N12 . 94.24(13) yes
N12 2_656 Ni1 . N12 . 179.994 yes
O3 . Ni1 . N12 . 85.76(13) yes
O13 2_656 Ni2 . O3 . 86.98(11) yes
O13 2_656 Ni2 . O21 . 88.23(11) yes
O3 . Ni2 . O21 . 167.39(11) yes
O13 2_656 Ni2 . O38 . 98.24(11) yes
O3 . Ni2 . O38 . 94.90(11) yes
O21 . Ni2 . O38 . 74.26(11) yes
O13 2_656 Ni2 . O55 . 99.52(11) yes
O3 . Ni2 . O55 . 96.79(13) yes
O21 . Ni2 . O55 . 95.50(13) yes
O38 . Ni2 . O55 . 159.18(11) yes
O13 2_656 Ni2 . N64 . 172.58(13) yes
O3 . Ni2 . N64 . 98.31(13) yes
O21 . Ni2 . N64 . 87.62(13) yes
O38 . Ni2 . N64 . 86.54(12) yes
O55 . Ni2 . N64 . 74.77(12) yes
O21 . Ni3 . O38 . 88.21(12) yes
O21 . Ni3 . N24 . 85.57(13) yes
O38 . Ni3 . N24 . 173.39(13) yes
O21 . Ni3 . N47 . 174.39(14) yes
O38 . Ni3 . N47 . 86.28(14) yes
N24 . Ni3 . N47 . 99.89(15) yes
Ni2 . O3 . Ni1 . 114.07(13) yes
Ni2 . O3 . C4 . 128.4(2) yes
Ni1 . O3 . C4 . 114.8(2) yes
Ni2 2_656 O13 . N12 . 114.3(2) yes
Ni2 . O21 . Ni3 . 93.34(12) yes
Ni2 . O21 . C22 . 136.4(2) yes
Ni3 . O21 . C22 . 114.7(2) yes
N24 . O25 . H252 . 109.5 no
Ni2 . O38 . Ni3 . 91.55(11) yes
Ni2 . O38 . C39 . 136.3(2) yes
Ni3 . O38 . C39 . 113.3(2) yes
N47 . O48 . H481 . 120.1 no
Ni2 . O55 . C56 . 116.8(3) yes
N64 . O65 . H650 . 119.7 no
C76 . O75 . H750 . 109.0 no
C78 . O77 . H770 . 119.4 no
O13 . N12 . Ni1 . 122.5(2) yes
O13 . N12 . C11 . 120.1(3) yes
Ni1 . N12 . C11 . 117.4(3) yes
O25 . N24 . Ni3 . 123.3(3) yes
O25 . N24 . C23 . 120.1(3) yes
Ni3 . N24 . C23 . 116.6(3) yes
O48 . N47 . Ni3 . 120.9(3) yes
O48 . N47 . C46 . 121.9(3) yes
Ni3 . N47 . C46 . 117.3(3) yes
O65 . N64 . Ni2 . 118.6(2) yes
O65 . N64 . C63 . 117.4(3) yes
Ni2 . N64 . C63 . 123.8(3) yes
O3 . C4 . C5 . 111.4(3) yes
O3 . C4 . C11 . 109.2(3) yes
C5 . C4 . C11 . 110.1(3) yes
O3 . C4 . H41 . 108.7 no
C5 . C4 . H41 . 108.7 no
C11 . C4 . H41 . 108.6 no
C4 . C5 . C6 . 120.0(3) yes
C4 . C5 . C10 . 121.0(4) yes
C6 . C5 . C10 . 119.0(4) yes
C5 . C6 . C7 . 119.7(4) yes
C5 . C6 . H61 . 120.1 no
C7 . C6 . H61 . 120.2 no
C6 . C7 . C8 . 120.7(4) yes
C6 . C7 . H71 . 119.5 no
C8 . C7 . H71 . 119.8 no
C7 . C8 . C9 . 120.0(4) yes
C7 . C8 . H81 . 119.9 no
C9 . C8 . H81 . 120.0 no
C8 . C9 . C10 . 120.0(4) yes
C8 . C9 . H91 . 120.0 no
C10 . C9 . H91 . 120.0 no
C5 . C10 . C9 . 120.5(4) yes
C5 . C10 . H101 . 119.7 no
C9 . C10 . H101 . 119.7 no
C4 . C11 . N12 . 112.8(4) yes
C4 . C11 . C14 . 121.3(3) yes
N12 . C11 . C14 . 125.8(4) yes
C11 . C14 . C15 . 120.6(4) yes
C11 . C14 . C19 . 120.0(4) yes
C15 . C14 . C19 . 119.3(4) yes
C14 . C15 . C16 . 121.3(5) yes
C14 . C15 . H151 . 119.3 no
C16 . C15 . H151 . 119.4 no
C15 . C16 . C17 . 118.6(6) yes
C15 . C16 . H161 . 120.9 no
C17 . C16 . H161 . 120.6 no
C16 . C17 . C18 . 120.5(5) yes
C16 . C17 . H171 . 120.0 no
C18 . C17 . H171 . 119.6 no
C17 . C18 . C19 . 120.7(5) yes
C17 . C18 . H181 . 119.6 no
C19 . C18 . H181 . 119.7 no
C14 . C19 . C18 . 119.7(5) yes
C14 . C19 . H191 . 120.1 no
C18 . C19 . H191 . 120.2 no
O21 . C22 . C23 . 109.2(3) yes
O21 . C22 . C32 . 110.7(3) yes
C23 . C22 . C32 . 109.5(3) yes
O21 . C22 . H221 . 109.1 no
C23 . C22 . H221 . 109.1 no
C32 . C22 . H221 . 109.2 no
C22 . C23 . N24 . 113.8(4) yes
C22 . C23 . C26 . 121.7(3) yes
N24 . C23 . C26 . 124.4(4) yes
C23 . C26 . C27 . 120.3(5) yes
C23 . C26 . C31 . 119.4(5) yes
C27 . C26 . C31 . 120.0(6) yes
C26 . C27 . C28 . 118.8(8) yes
C26 . C27 . H271 . 120.6 no
C28 . C27 . H271 . 120.6 no
C27 . C28 . C29 . 121.5(9) yes
C27 . C28 . H281 . 119.4 no
C29 . C28 . H281 . 119.1 no
C28 . C29 . C30 . 118.6(8) yes
C28 . C29 . H291 . 120.8 no
C30 . C29 . H291 . 120.5 no
C29 . C30 . C31 . 122.0(10) yes
C29 . C30 . H301 . 119.1 no
C31 . C30 . H301 . 118.9 no
C26 . C31 . C30 . 118.9(9) yes
C26 . C31 . H311 . 120.5 no
C30 . C31 . H311 . 120.6 no
C22 . C32 . C33 . 120.4(4) yes
C22 . C32 . C37 . 121.1(4) yes
C33 . C32 . C37 . 118.5(4) yes
C32 . C33 . C34 . 120.8(4) yes
C32 . C33 . H331 . 119.6 no
C34 . C33 . H331 . 119.6 no
C33 . C34 . C35 . 120.5(5) yes
C33 . C34 . H341 . 119.7 no
C35 . C34 . H341 . 119.8 no
C34 . C35 . C36 . 118.8(4) yes
C34 . C35 . H351 . 120.4 no
C36 . C35 . H351 . 120.8 no
C35 . C36 . C37 . 121.0(5) yes
C35 . C36 . H361 . 119.5 no
C37 . C36 . H361 . 119.5 no
C36 . C37 . C32 . 120.5(5) yes
C36 . C37 . H371 . 119.8 no
C32 . C37 . H371 . 119.7 no
O38 . C39 . C40 . 108.3(3) yes
O38 . C39 . C46 . 109.2(3) yes
C40 . C39 . C46 . 113.4(3) yes
O38 . C39 . H391 . 108.6 no
C40 . C39 . H391 . 108.6 no
C46 . C39 . H391 . 108.7 no
C39 . C40 . C41 . 120.6(4) yes
C39 . C40 . C45 . 119.7(4) yes
C41 . C40 . C45 . 119.6(4) yes
C40 . C41 . C42 . 120.4(6) yes
C40 . C41 . H411 . 119.8 no
C42 . C41 . H411 . 119.8 no
C41 . C42 . C43 . 118.7(6) yes
C41 . C42 . H421 . 120.4 no
C43 . C42 . H421 . 120.8 no
C42 . C43 . C44 . 120.5(5) yes
C42 . C43 . H431 . 119.7 no
C44 . C43 . H431 . 119.8 no
C43 . C44 . C45 . 120.2(6) yes
C43 . C44 . H441 . 119.8 no
C45 . C44 . H441 . 119.9 no
C40 . C45 . C44 . 120.5(6) yes
C40 . C45 . H451 . 119.8 no
C44 . C45 . H451 . 119.7 no
C39 . C46 . N47 . 112.8(3) yes
C39 . C46 . C49 . 121.0(4) yes
N47 . C46 . C49 . 126.2(4) yes
C46 . C49 . C50 . 119.4(4) yes
C46 . C49 . C54 . 122.3(4) yes
C50 . C49 . C54 . 118.3(4) yes
C49 . C50 . C51 . 120.6(5) yes
C49 . C50 . H501 . 119.6 no
C51 . C50 . H501 . 119.8 no
C50 . C51 . C52 . 120.8(5) yes
C50 . C51 . H511 . 119.6 no
C52 . C51 . H511 . 119.6 no
C51 . C52 . C53 . 119.4(4) yes
C51 . C52 . H521 . 120.3 no
C53 . C52 . H521 . 120.3 no
C52 . C53 . C54 . 120.8(5) yes
C52 . C53 . H531 . 119.7 no
C54 . C53 . H531 . 119.6 no
C49 . C54 . C53 . 120.1(5) yes
C49 . C54 . H541 . 119.9 no
C53 . C54 . H541 . 120.0 no
O55 . C56 . C57 . 108.3(4) yes
O55 . C56 . C63 . 105.1(4) yes
C57 . C56 . C63 . 114.3(4) yes
O55 . C56 . H561 . 109.6 no
C57 . C56 . H561 . 109.6 no
C63 . C56 . H561 . 109.7 no
C56 . C57 . C58 . 117.7(4) yes
C56 . C57 . C62 . 122.3(4) yes
C58 . C57 . C62 . 119.9(5) yes
C57 . C58 . C59 . 120.9(6) yes
C57 . C58 . H581 . 119.5 no
C59 . C58 . H581 . 119.7 no
C58 . C59 . C60 . 115.3(6) yes
C58 . C59 . H591 . 122.3 no
C60 . C59 . H591 . 122.4 no
C59 . C60 . C61 . 125.4(6) yes
C59 . C60 . H601 . 117.3 no
C61 . C60 . H601 . 117.3 no
C60 . C61 . C62 . 117.9(6) yes
C60 . C61 . H611 . 121.3 no
C62 . C61 . H611 . 120.8 no
C57 . C62 . C61 . 120.7(6) yes
C57 . C62 . H621 . 119.6 no
C61 . C62 . H621 . 119.7 no
C56 . C63 . N64 . 113.7(4) yes
C56 . C63 . C66 . 119.7(4) yes
N64 . C63 . C66 . 125.8(4) yes
C63 . C66 . C67 . 119.4(4) yes
C63 . C66 . C71 . 121.1(4) yes
C67 . C66 . C71 . 119.5(4) yes
C66 . C67 . C68 . 119.8(5) yes
C66 . C67 . H671 . 120.2 no
C68 . C67 . H671 . 120.0 no
C67 . C68 . C69 . 120.4(5) yes
C67 . C68 . H681 . 119.9 no
C69 . C68 . H681 . 119.7 no
C68 . C69 . C70 . 120.5(5) yes
C68 . C69 . H691 . 119.8 no
C70 . C69 . H691 . 119.7 no
C69 . C70 . C71 . 119.2(5) yes
C69 . C70 . H701 . 120.3 no
C71 . C70 . H701 . 120.5 no
C70 . C71 . C66 . 120.6(5) yes
C70 . C71 . H711 . 119.6 no
C66 . C71 . H711 . 119.8 no
Cl2 . C73 . Cl1 . 125.0(8) yes
Cl2 . C73 . H731 . 105.2 no
Cl1 . C73 . H731 . 105.6 no
Cl2 . C73 . H732 . 105.6 no
Cl1 . C73 . H732 . 105.5 no
H731 . C73 . H732 . 109.5 no
O75 . C76 . H761 . 109.4 no
O75 . C76 . H762 . 109.6 no
H761 . C76 . H762 . 109.5 no
O75 . C76 . H763 . 109.4 no
H761 . C76 . H763 . 109.5 no
H762 . C76 . H763 . 109.5 no
O77 . C78 . H781 . 109.6 no
O77 . C78 . H782 . 109.3 no
H781 . C78 . H782 . 109.5 no
O77 . C78 . H783 . 109.6 no
H781 . C78 . H783 . 109.5 no
H782 . C78 . H783 . 109.5 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 19/07/12 at 17:27:49
#
#LIST 12
BLOCK SCALE X'S, U'S
RIDE O ( 25,X'S) H ( 252,X'S)
RIDE O ( 48,X'S) H ( 481,X'S)
RIDE O ( 65,X'S) H ( 650,X'S)
RIDE O ( 75,X'S) H ( 750,X'S)
RIDE O ( 77,X'S) H ( 770,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 7,X'S) H ( 71,X'S)
RIDE C ( 8,X'S) H ( 81,X'S)
RIDE C ( 9,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 101,X'S)
RIDE C ( 15,X'S) H ( 151,X'S)
RIDE C ( 16,X'S) H ( 161,X'S)
RIDE C ( 17,X'S) H ( 171,X'S)
RIDE C ( 18,X'S) H ( 181,X'S)
RIDE C ( 19,X'S) H ( 191,X'S)
RIDE C ( 22,X'S) H ( 221,X'S)
RIDE C ( 27,X'S) H ( 271,X'S)
RIDE C ( 28,X'S) H ( 281,X'S)
RIDE C ( 29,X'S) H ( 291,X'S)
RIDE C ( 30,X'S) H ( 301,X'S)
RIDE C ( 31,X'S) H ( 311,X'S)
RIDE C ( 33,X'S) H ( 331,X'S)
RIDE C ( 34,X'S) H ( 341,X'S)
RIDE C ( 35,X'S) H ( 351,X'S)
RIDE C ( 36,X'S) H ( 361,X'S)
RIDE C ( 37,X'S) H ( 371,X'S)
RIDE C ( 39,X'S) H ( 391,X'S)
RIDE C ( 41,X'S) H ( 411,X'S)
RIDE C ( 42,X'S) H ( 421,X'S)
RIDE C ( 43,X'S) H ( 431,X'S)
RIDE C ( 44,X'S) H ( 441,X'S)
RIDE C ( 45,X'S) H ( 451,X'S)
RIDE C ( 50,X'S) H ( 501,X'S)
RIDE C ( 51,X'S) H ( 511,X'S)
RIDE C ( 52,X'S) H ( 521,X'S)
RIDE C ( 53,X'S) H ( 531,X'S)
RIDE C ( 54,X'S) H ( 541,X'S)
RIDE C ( 56,X'S) H ( 561,X'S)
RIDE C ( 58,X'S) H ( 581,X'S)
RIDE C ( 59,X'S) H ( 591,X'S)
RIDE C ( 60,X'S) H ( 601,X'S)
RIDE C ( 61,X'S) H ( 611,X'S)
RIDE C ( 62,X'S) H ( 621,X'S)
RIDE C ( 67,X'S) H ( 671,X'S)
RIDE C ( 68,X'S) H ( 681,X'S)
RIDE C ( 69,X'S) H ( 691,X'S)
RIDE C ( 70,X'S) H ( 701,X'S)
RIDE C ( 71,X'S) H ( 711,X'S)
RIDE C ( 73,X'S) H ( 731,X'S) H ( 732,X'S)
RIDE C ( 76,X'S) H ( 761,X'S) H ( 762,X'S) H ( 763,X'S)
RIDE C ( 78,X'S) H ( 781,X'S) H ( 782,X'S) H ( 783,X'S)
END
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 19/07/12 at 17:27:49
#
#LIST 16
DIST 0.0, 0.01 = MEAN CL(1) TO C(73) , CL(2) TO C(73)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
-2 -1 2 x .
-3 0 4 x .
-2 -3 5 x .
0 2 0 x .
-3 0 10 x .
-1 -9 3 x .
-1 1 1 x .
2 3 12 x .


_database_code_depnum_ccdc_archive 'CCDC 894477'
