# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_zl55-2
_database_code_depnum_ccdc_archive 'CCDC 1060742'
_audit_update_record             
;
2015-04-21 deposited with the CCDC.
2016-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H58 Ni5 O38'
_chemical_formula_weight         1680.61

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'
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           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   7.812(3)
_cell_length_b                   11.688(4)
_cell_length_c                   17.770(6)
_cell_angle_alpha                90.927(5)
_cell_angle_beta                 93.857(5)
_cell_angle_gamma                107.518(5)
_cell_volume                     1542.6(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.809
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             862
_exptl_absorpt_coefficient_mu    1.608
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.6892
_exptl_absorpt_correction_T_max  0.7392
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15903
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5357
_reflns_number_gt                4403
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_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 > 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)+(0.0001P)²+62.6455P] 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         5357
_refine_ls_number_parameters     469
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0978
_refine_ls_wR_factor_ref         0.2570
_refine_ls_wR_factor_gt          0.2494
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_restrained_S_all      1.129
_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 0.5000 0.5000 0.5000 0.0117(5) Uani 1 2 d S . .
Ni2 Ni 0.3130(2) 0.65870(14) 0.37118(9) 0.0171(4) Uani 1 1 d . . .
Ni3 Ni 0.2660(2) 0.24910(13) 0.60196(8) 0.0142(4) Uani 1 1 d . . .
O1 O 0.3024(11) 0.3951(7) 0.4210(4) 0.0170(18) Uani 1 1 d U . .
O2 O 0.3023(12) 0.4952(7) 0.3153(5) 0.0214(19) Uani 1 1 d . . .
O3 O 0.1098(13) -0.0367(8) 0.4285(5) 0.026(2) Uani 1 1 d U . .
O4 O -0.0820(12) -0.1380(8) 0.3348(5) 0.024(2) Uani 1 1 d . . .
O5 O -0.3666(18) 0.0435(10) -0.1348(6) 0.054(4) Uani 1 1 d . . .
H5 H -0.4136 0.0562 -0.1752 0.080 Uiso 1 1 calc R . .
O6 O -0.1610(18) 0.2125(12) -0.1577(6) 0.058(4) Uani 1 1 d . . .
O7 O 0.3039(11) 0.5221(7) 0.5650(4) 0.0156(17) Uani 1 1 d . . .
O8 O 0.2401(12) 0.3938(7) 0.6580(5) 0.0213(19) Uani 1 1 d . . .
O9 O 0.366(2) 0.9414(11) 0.6169(7) 0.064(4) Uani 1 1 d U . .
O10 O 0.4671(14) 1.0260(8) 0.7297(5) 0.030(2) Uani 1 1 d U . .
O11 O 0.5509(15) 0.6766(10) 1.1753(5) 0.040(3) Uani 1 1 d . . .
O12 O 0.292(2) 0.5260(11) 1.1636(6) 0.059(4) Uani 1 1 d . . .
H12 H 0.3018 0.5317 1.2099 0.088 Uiso 1 1 calc R . .
O13 O 0.4893(11) 0.3474(7) 0.5525(4) 0.0157(17) Uani 1 1 d . . .
H13A H 0.4858 0.3121 0.5119 0.024 Uiso 1 1 d R . .
O14 O 0.1247(13) 0.6769(10) 0.2919(6) 0.034(2) Uani 1 1 d . . .
H14A H 0.1257 0.7196 0.2556 0.051 Uiso 1 1 d R . .
H14B H 0.0193 0.6414 0.2984 0.051 Uiso 1 1 d R . .
O15 O 0.1117(13) 0.5743(9) 0.4384(5) 0.030(2) Uani 1 1 d . . .
H15A H 0.0058 0.5324 0.4352 0.046 Uiso 1 1 d R . .
H15B H 0.1509 0.5738 0.4826 0.046 Uiso 1 1 d R . .
O16 O 0.3228(13) 0.8184(9) 0.4297(7) 0.037(3) Uani 1 1 d . . .
H16A H 0.4253 0.8648 0.4356 0.056 Uiso 1 1 d R . .
H16B H 0.2573 0.8571 0.4135 0.056 Uiso 1 1 d R . .
O17 O 0.5327(11) 0.7594(7) 0.3135(5) 0.0186(18) Uani 1 1 d . . .
H17A H 0.5227 0.8254 0.3034 0.028 Uiso 1 1 d R . .
H17B H 0.5550 0.7293 0.2748 0.028 Uiso 1 1 d R . .
O18 O 0.0742(12) 0.2633(8) 0.5169(5) 0.023(2) Uani 1 1 d . . .
H18A H 0.1460 0.3040 0.4865 0.034 Uiso 1 1 d R . .
H18B H -0.0123 0.2719 0.5374 0.034 Uiso 1 1 d R . .
O19 O 0.3011(12) 0.1061(8) 0.5433(5) 0.027(2) Uani 1 1 d . . .
H19A H 0.2495 0.0670 0.5051 0.041 Uiso 1 1 d R . .
H19B H 0.3128 0.0585 0.5752 0.041 Uiso 1 1 d R . .
C1 C 0.0323(17) 0.1574(11) 0.1979(7) 0.020(3) Uani 1 1 d . . .
C2 C 0.1162(17) 0.2701(11) 0.2350(7) 0.020(3) Uani 1 1 d . . .
H2 H 0.1243 0.3395 0.2088 0.024 Uiso 1 1 calc R . .
C3 C 0.1866(16) 0.2801(10) 0.3092(7) 0.016(2) Uani 1 1 d . . .
C4 C 0.1691(17) 0.1770(11) 0.3481(7) 0.019(3) Uani 1 1 d . . .
H4 H 0.2214 0.1819 0.3971 0.023 Uiso 1 1 calc R . .
C5 C 0.0728(16) 0.0641(10) 0.3144(7) 0.017(2) Uani 1 1 d . . .
C6 C 0.0076(17) 0.0554(11) 0.2405(7) 0.021(3) Uani 1 1 d U . .
H6 H -0.0539 -0.0196 0.2183 0.025 Uiso 1 1 calc R . .
C7 C 0.2693(16) 0.3993(10) 0.3493(7) 0.016(2) Uani 1 1 d . . .
C8 C 0.0326(16) -0.0436(11) 0.3630(7) 0.018(3) Uani 1 1 d . . .
C9 C -0.0334(19) 0.1480(11) 0.1172(7) 0.022(3) Uani 1 1 d . . .
C10 C -0.179(2) 0.0539(12) 0.0888(8) 0.032(3) Uani 1 1 d . . .
H10 H -0.2350 -0.0067 0.1202 0.038 Uiso 1 1 calc R . .
C11 C -0.242(2) 0.0493(13) 0.0129(8) 0.034(4) Uani 1 1 d . . .
H11 H -0.3416 -0.0139 -0.0054 0.041 Uiso 1 1 calc R . .
C12 C -0.1613(19) 0.1354(13) -0.0343(7) 0.026(3) Uani 1 1 d . . .
C13 C -0.013(2) 0.2284(13) -0.0070(8) 0.035(4) Uani 1 1 d . . .
H13 H 0.0461 0.2864 -0.0395 0.042 Uiso 1 1 calc R . .
C14 C 0.049(2) 0.2358(13) 0.0673(8) 0.038(4) Uani 1 1 d . . .
H14 H 0.1468 0.3003 0.0851 0.045 Uiso 1 1 calc R . .
C15 C -0.226(2) 0.1341(13) -0.1152(8) 0.033(3) Uani 1 1 d . . .
C16 C 0.3521(18) 0.6757(11) 0.8168(7) 0.021(3) Uani 1 1 d . . .
C17 C 0.3066(18) 0.5794(11) 0.7655(7) 0.021(3) Uani 1 1 d . . .
H17 H 0.2783 0.5015 0.7823 0.025 Uiso 1 1 calc R . .
C18 C 0.3031(16) 0.5995(10) 0.6873(6) 0.015(2) Uani 1 1 d . . .
C19 C 0.3347(17) 0.7149(11) 0.6628(7) 0.020(3) Uani 1 1 d . . .
H19 H 0.3293 0.7278 0.6113 0.024 Uiso 1 1 calc R . .
C20 C 0.3746(19) 0.8125(11) 0.7141(7) 0.022(3) Uani 1 1 d . . .
C21 C 0.3852(17) 0.7922(11) 0.7905(7) 0.019(3) Uani 1 1 d . . .
H21 H 0.4149 0.8570 0.8250 0.022 Uiso 1 1 calc R . .
C22 C 0.2778(15) 0.4977(10) 0.6322(6) 0.013(2) Uani 1 1 d . . .
C23 C 0.406(2) 0.9362(12) 0.6861(8) 0.029(3) Uani 1 1 d U . .
C24 C 0.3653(19) 0.6571(11) 0.8988(7) 0.023(3) Uani 1 1 d . . .
C25 C 0.502(2) 0.7343(13) 0.9445(8) 0.033(3) Uani 1 1 d . . .
H25 H 0.5842 0.7981 0.9232 0.040 Uiso 1 1 calc R . .
C26 C 0.5215(19) 0.7193(12) 1.0214(7) 0.028(3) Uani 1 1 d . . .
H26 H 0.6149 0.7728 1.0511 0.033 Uiso 1 1 calc R . .
C27 C 0.401(2) 0.6243(12) 1.0538(7) 0.028(3) Uani 1 1 d . . .
C28 C 0.259(2) 0.5456(12) 1.0090(8) 0.033(4) Uani 1 1 d . . .
H28 H 0.1767 0.4826 1.0308 0.040 Uiso 1 1 calc R . .
C29 C 0.242(2) 0.5615(12) 0.9320(7) 0.030(3) Uani 1 1 d . . .
H29 H 0.1475 0.5087 0.9023 0.036 Uiso 1 1 calc R . .
C30 C 0.424(2) 0.6125(12) 1.1364(8) 0.029(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O13 2.008(8) . ?
Ni1 O13 2.008(8) 2_666 ?
Ni1 O7 2.052(8) . ?
Ni1 O7 2.052(8) 2_666 ?
Ni1 O1 2.090(8) 2_666 ?
Ni1 O1 2.090(8) . ?
Ni2 O13 2.004(8) 2_666 ?
Ni2 O14 2.028(10) . ?
Ni2 O15 2.057(9) . ?
Ni2 O16 2.100(10) . ?
Ni2 O17 2.107(9) . ?
Ni2 O2 2.116(9) . ?
Ni3 O8 2.019(9) . ?
Ni3 O4 2.039(9) 2_556 ?
Ni3 O13 2.042(8) . ?
Ni3 O19 2.053(10) . ?
Ni3 O18 2.100(9) . ?
Ni3 O17 2.126(9) 2_666 ?
O1 C7 1.288(14) . ?
O2 C7 1.249(14) . ?
O3 C8 1.264(15) . ?
O4 C8 1.264(15) . ?
O4 Ni3 2.039(9) 2_556 ?
O5 C15 1.299(18) . ?
O5 H5 0.8200 . ?
O6 C15 1.208(18) . ?
O7 C22 1.249(14) . ?
O8 C22 1.262(14) . ?
O9 C23 1.255(18) . ?
O10 C23 1.245(16) . ?
O11 C30 1.211(18) . ?
O12 C30 1.330(18) . ?
O12 H12 0.8200 . ?
O13 Ni2 2.004(8) 2_666 ?
O13 H13A 0.8199 . ?
O14 H14A 0.8201 . ?
O14 H14B 0.8200 . ?
O15 H15A 0.8223 . ?
O15 H15B 0.8235 . ?
O16 H16A 0.8200 . ?
O16 H16B 0.8200 . ?
O17 Ni3 2.126(8) 2_666 ?
O17 H17A 0.8201 . ?
O17 H17B 0.8200 . ?
O18 H18A 0.8501 . ?
O18 H18B 0.8200 . ?
O19 H19A 0.8201 . ?
O19 H19B 0.8200 . ?
C1 C6 1.393(17) . ?
C1 C2 1.411(17) . ?
C1 C9 1.481(17) . ?
C2 C3 1.383(17) . ?
C2 H2 0.9300 . ?
C3 C4 1.375(17) . ?
C3 C7 1.493(16) . ?
C4 C5 1.408(17) . ?
C4 H4 0.9300 . ?
C5 C6 1.368(17) . ?
C5 C8 1.504(16) . ?
C6 H6 0.9300 . ?
C9 C10 1.382(19) . ?
C9 C14 1.401(19) . ?
C10 C11 1.399(19) . ?
C10 H10 0.9300 . ?
C11 C12 1.353(19) . ?
C11 H11 0.9300 . ?
C12 C13 1.383(19) . ?
C12 C15 1.490(18) . ?
C13 C14 1.367(19) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C16 C17 1.381(17) . ?
C16 C21 1.402(17) . ?
C16 C24 1.478(17) . ?
C17 C18 1.412(16) . ?
C17 H17 0.9300 . ?
C18 C19 1.380(17) . ?
C18 C22 1.486(15) . ?
C19 C20 1.394(18) . ?
C19 H19 0.9300 . ?
C20 C21 1.382(17) . ?
C20 C23 1.491(18) . ?
C21 H21 0.9300 . ?
C24 C25 1.38(2) . ?
C24 C29 1.407(19) . ?
C25 C26 1.384(19) . ?
C25 H25 0.9300 . ?
C26 C27 1.382(19) . ?
C26 H26 0.9300 . ?
C27 C28 1.40(2) . ?
C27 C30 1.480(18) . ?
C28 C29 1.387(18) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?

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
O13 Ni1 O13 179.998(2) . 2_666 ?
O13 Ni1 O7 89.2(3) . . ?
O13 Ni1 O7 90.8(3) 2_666 . ?
O13 Ni1 O7 90.8(3) . 2_666 ?
O13 Ni1 O7 89.2(3) 2_666 2_666 ?
O7 Ni1 O7 179.998(2) . 2_666 ?
O13 Ni1 O1 92.9(3) . 2_666 ?
O13 Ni1 O1 87.1(3) 2_666 2_666 ?
O7 Ni1 O1 89.8(3) . 2_666 ?
O7 Ni1 O1 90.2(3) 2_666 2_666 ?
O13 Ni1 O1 87.1(3) . . ?
O13 Ni1 O1 92.9(3) 2_666 . ?
O7 Ni1 O1 90.2(3) . . ?
O7 Ni1 O1 89.8(3) 2_666 . ?
O1 Ni1 O1 179.999(1) 2_666 . ?
O13 Ni2 O14 175.8(4) 2_666 . ?
O13 Ni2 O15 93.7(4) 2_666 . ?
O14 Ni2 O15 89.7(4) . . ?
O13 Ni2 O16 84.9(4) 2_666 . ?
O14 Ni2 O16 92.8(4) . . ?
O15 Ni2 O16 86.4(4) . . ?
O13 Ni2 O17 82.0(3) 2_666 . ?
O14 Ni2 O17 94.4(4) . . ?
O15 Ni2 O17 173.1(4) . . ?
O16 Ni2 O17 87.8(4) . . ?
O13 Ni2 O2 94.1(3) 2_666 . ?
O14 Ni2 O2 88.3(4) . . ?
O15 Ni2 O2 92.3(4) . . ?
O16 Ni2 O2 178.3(4) . . ?
O17 Ni2 O2 93.4(3) . . ?
O8 Ni3 O4 90.4(4) . 2_556 ?
O8 Ni3 O13 93.2(3) . . ?
O4 Ni3 O13 167.6(4) 2_556 . ?
O8 Ni3 O19 177.8(4) . . ?
O4 Ni3 O19 91.7(4) 2_556 . ?
O13 Ni3 O19 84.6(4) . . ?
O8 Ni3 O18 90.4(4) . . ?
O4 Ni3 O18 94.6(4) 2_556 . ?
O13 Ni3 O18 97.3(3) . . ?
O19 Ni3 O18 89.9(4) . . ?
O8 Ni3 O17 88.9(4) . 2_666 ?
O4 Ni3 O17 87.5(3) 2_556 2_666 ?
O13 Ni3 O17 80.7(3) . 2_666 ?
O19 Ni3 O17 90.6(3) . 2_666 ?
O18 Ni3 O17 177.8(3) . 2_666 ?
C7 O1 Ni1 134.1(7) . . ?
C7 O2 Ni2 121.3(8) . . ?
C8 O4 Ni3 121.8(8) . 2_556 ?
C15 O5 H5 109.5 . . ?
C22 O7 Ni1 129.9(8) . . ?
C22 O8 Ni3 124.1(8) . . ?
C30 O12 H12 109.5 . . ?
Ni2 O13 Ni1 120.5(4) 2_666 . ?
Ni2 O13 Ni3 101.7(3) 2_666 . ?
Ni1 O13 Ni3 122.6(4) . . ?
Ni2 O13 H13A 115.8 2_666 . ?
Ni1 O13 H13A 90.8 . . ?
Ni3 O13 H13A 104.9 . . ?
Ni2 O14 H14A 134.9 . . ?
Ni2 O14 H14B 116.9 . . ?
H14A O14 H14B 107.7 . . ?
Ni2 O15 H15A 140.6 . . ?
Ni2 O15 H15B 111.5 . . ?
H15A O15 H15B 107.2 . . ?
Ni2 O16 H16A 112.3 . . ?
Ni2 O16 H16B 118.6 . . ?
H16A O16 H16B 107.2 . . ?
Ni2 O17 Ni3 95.7(3) . 2_666 ?
Ni2 O17 H17A 111.0 . . ?
Ni3 O17 H17A 118.4 2_666 . ?
Ni2 O17 H17B 117.9 . . ?
Ni3 O17 H17B 106.3 2_666 . ?
H17A O17 H17B 107.7 . . ?
Ni3 O18 H18A 98.3 . . ?
Ni3 O18 H18B 107.8 . . ?
H18A O18 H18B 134.5 . . ?
Ni3 O19 H19A 133.2 . . ?
Ni3 O19 H19B 105.8 . . ?
H19A O19 H19B 107.7 . . ?
C6 C1 C2 117.7(11) . . ?
C6 C1 C9 121.0(11) . . ?
C2 C1 C9 121.2(11) . . ?
C3 C2 C1 121.9(11) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
C4 C3 C2 118.6(11) . . ?
C4 C3 C7 119.4(10) . . ?
C2 C3 C7 121.9(11) . . ?
C3 C4 C5 120.6(11) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C6 C5 C4 120.0(11) . . ?
C6 C5 C8 121.4(11) . . ?
C4 C5 C8 118.4(10) . . ?
C5 C6 C1 120.9(11) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.5 . . ?
O2 C7 O1 123.1(11) . . ?
O2 C7 C3 121.9(11) . . ?
O1 C7 C3 115.0(10) . . ?
O4 C8 O3 123.3(11) . . ?
O4 C8 C5 116.3(10) . . ?
O3 C8 C5 120.4(11) . . ?
C10 C9 C14 117.7(12) . . ?
C10 C9 C1 121.5(11) . . ?
C14 C9 C1 120.8(12) . . ?
C9 C10 C11 120.4(12) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C12 C11 C10 120.9(12) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C11 C12 C13 119.3(12) . . ?
C11 C12 C15 122.5(13) . . ?
C13 C12 C15 118.3(13) . . ?
C14 C13 C12 120.6(13) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C13 C14 C9 121.1(13) . . ?
C13 C14 H14 119.5 . . ?
C9 C14 H14 119.5 . . ?
O6 C15 O5 122.9(13) . . ?
O6 C15 C12 123.8(14) . . ?
O5 C15 C12 113.2(12) . . ?
C17 C16 C21 119.3(11) . . ?
C17 C16 C24 120.8(11) . . ?
C21 C16 C24 119.9(11) . . ?
C16 C17 C18 119.9(11) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C19 C18 C17 119.6(11) . . ?
C19 C18 C22 120.3(10) . . ?
C17 C18 C22 119.9(11) . . ?
C18 C19 C20 121.0(11) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 H19 119.5 . . ?
C21 C20 C19 118.8(11) . . ?
C21 C20 C23 121.3(11) . . ?
C19 C20 C23 119.9(11) . . ?
C20 C21 C16 121.3(11) . . ?
C20 C21 H21 119.4 . . ?
C16 C21 H21 119.4 . . ?
O7 C22 O8 125.3(11) . . ?
O7 C22 C18 117.6(10) . . ?
O8 C22 C18 117.0(10) . . ?
O10 C23 O9 123.8(13) . . ?
O10 C23 C20 121.0(12) . . ?
O9 C23 C20 115.1(12) . . ?
C25 C24 C29 118.5(12) . . ?
C25 C24 C16 119.8(12) . . ?
C29 C24 C16 121.7(12) . . ?
C24 C25 C26 121.8(13) . . ?
C24 C25 H25 119.1 . . ?
C26 C25 H25 119.1 . . ?
C27 C26 C25 119.7(13) . . ?
C27 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
C26 C27 C28 119.8(12) . . ?
C26 C27 C30 118.2(12) . . ?
C28 C27 C30 121.9(13) . . ?
C29 C28 C27 119.9(13) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C28 C29 C24 120.3(13) . . ?
C28 C29 H29 119.9 . . ?
C24 C29 H29 119.9 . . ?
O11 C30 O12 123.5(13) . . ?
O11 C30 C27 122.5(13) . . ?
O12 C30 C27 114.0(12) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O19 H19B O9 0.82 1.71 2.499(14) 160.8 1_545
O19 H19A O3 0.82 1.86 2.676(12) 171.3 .
O18 H18B O16 0.82 2.45 3.174(13) 147.5 2_566
O18 H18B O15 0.82 2.21 2.848(13) 134.9 2_566
O18 H18A O1 0.85 1.85 2.700(12) 179.0 .
O17 H17B O11 0.82 1.86 2.653(13) 163.2 1_554
O17 H17A O10 0.82 1.82 2.636(12) 169.9 2_676
O16 H16B O3 0.82 1.96 2.708(14) 151.8 1_565
O16 H16A O19 0.82 2.07 2.807(14) 149.8 2_666
O15 H15B O7 0.82 2.04 2.797(13) 152.4 .
O15 H15A O7 0.82 2.31 3.096(13) 160.3 2_566
O14 H14B O8 0.82 2.14 2.923(13) 158.8 2_566
O14 H14A O6 0.82 1.93 2.722(14) 162.9 2_565
O12 H12 O2 0.82 1.93 2.723(13) 163.3 1_556
O5 H5 O10 0.82 1.85 2.632(13) 159.3 1_444

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.968
_refine_diff_density_min         -1.434
_refine_diff_density_rms         0.194
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_zh119-2
_database_code_depnum_ccdc_archive 'CCDC 1060743'
_audit_update_record             
;
2015-04-21 deposited with the CCDC.
2016-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H18 Ni2 O12'
_chemical_formula_weight         507.71

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'
Ni Ni 0.3393 1.1124 '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'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   7.8760(10)
_cell_length_b                   10.4299(13)
_cell_length_c                   12.2338(16)
_cell_angle_alpha                98.828(2)
_cell_angle_beta                 91.679(2)
_cell_angle_gamma                107.982(2)
_cell_volume                     941.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             520
_exptl_absorpt_coefficient_mu    2.064
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10152
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         25.05
_reflns_number_total             3339
_reflns_number_gt                2722
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_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 > 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)+(0.0408P)²+0.2746P] 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         3339
_refine_ls_number_parameters     280
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0320
_refine_ls_wR_factor_ref         0.0816
_refine_ls_wR_factor_gt          0.0753
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.037
_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
Ni1 Ni 0.50937(5) 0.01811(4) 0.62913(3) 0.01531(13) Uani 1 1 d . . .
Ni2 Ni 0.46231(5) 0.26893(4) 0.55423(3) 0.01659(13) Uani 1 1 d . . .
O1 O 0.4006(3) 0.1032(2) 0.76640(19) 0.0262(6) Uani 1 1 d . . .
O2 O 0.3249(3) 0.2601(2) 0.68886(19) 0.0262(6) Uani 1 1 d . . .
O7 O 0.3795(3) 0.0654(2) 0.50073(18) 0.0175(5) Uani 1 1 d . . .
H7A H 0.2734 0.0196 0.4959 0.026 Uiso 1 1 d R . .
O10 O 0.5514(3) 0.4785(2) 0.6194(2) 0.0275(6) Uani 1 1 d . . .
H10A H 0.6435 0.5254 0.5973 0.041 Uiso 1 1 d R . .
H10B H 0.4772 0.5186 0.6162 0.041 Uiso 1 1 d R . .
O9 O 0.2314(3) 0.2850(2) 0.47342(19) 0.0239(5) Uani 1 1 d . . .
H9A H 0.1919 0.2248 0.4191 0.036 Uiso 1 1 d R . .
H9B H 0.1642 0.2654 0.5225 0.036 Uiso 1 1 d R . .
O3 O 0.3292(3) 0.7830(2) 1.36574(18) 0.0192(5) Uani 1 1 d . . .
O4 O 0.0655(3) 0.8022(2) 1.4130(2) 0.0290(6) Uani 1 1 d . . .
O5 O -0.3012(3) 0.1488(2) 1.35510(19) 0.0225(5) Uani 1 1 d . . .
O6 O -0.3851(3) 0.3281(2) 1.42790(19) 0.0227(5) Uani 1 1 d . . .
O8 O 0.6694(3) -0.0276(3) 0.7468(2) 0.0385(7) Uani 1 1 d . . .
H8A H 0.7697 -0.0317 0.7346 0.058 Uiso 1 1 d R . .
H8B H 0.6809 0.0299 0.8028 0.058 Uiso 1 1 d R . .
C9 C 0.1428(4) 0.5347(3) 1.2257(3) 0.0211(8) Uani 1 1 d . . .
H9 H 0.2391 0.5917 1.1960 0.025 Uiso 1 1 calc R . .
C1 C 0.3363(4) 0.2003(3) 0.7689(3) 0.0210(8) Uani 1 1 d . . .
C12 C -0.0683(4) 0.5025(3) 1.3638(3) 0.0200(7) Uani 1 1 d . . .
H12 H -0.1181 0.5380 1.4245 0.024 Uiso 1 1 calc R . .
C5 C 0.1362(5) 0.3462(3) 1.0708(3) 0.0241(8) Uani 1 1 d . . .
C14 C -0.2874(4) 0.2732(3) 1.3708(3) 0.0180(7) Uani 1 1 d . . .
C10 C 0.0757(4) 0.5869(3) 1.3200(3) 0.0180(7) Uani 1 1 d . . .
C2 C 0.2659(5) 0.2486(4) 0.8737(3) 0.0229(8) Uani 1 1 d . . .
C3 C 0.2563(5) 0.3805(4) 0.8945(3) 0.0323(9) Uani 1 1 d . . .
H3 H 0.2909 0.4369 0.8418 0.039 Uiso 1 1 calc R . .
C11 C 0.1601(4) 0.7354(3) 1.3711(3) 0.0185(7) Uani 1 1 d . . .
C8 C 0.0689(5) 0.3986(3) 1.1746(3) 0.0211(8) Uani 1 1 d . . .
C15 C -0.0709(4) 0.3147(3) 1.2232(3) 0.0215(8) Uani 1 1 d . . .
H15 H -0.1200 0.2229 1.1917 0.026 Uiso 1 1 calc R . .
C13 C -0.1386(4) 0.3656(3) 1.3178(3) 0.0173(7) Uani 1 1 d . . .
C7 C 0.2063(6) 0.1654(4) 0.9517(3) 0.0390(11) Uani 1 1 d . . .
H7 H 0.2096 0.0760 0.9390 0.047 Uiso 1 1 calc R . .
C6 C 0.1418(6) 0.2130(4) 1.0481(3) 0.0410(11) Uani 1 1 d . . .
H6 H 0.1013 0.1547 1.0988 0.049 Uiso 1 1 calc R . .
C4 C 0.1961(5) 0.4296(4) 0.9924(3) 0.0316(9) Uani 1 1 d . . .
H4 H 0.1958 0.5198 1.0058 0.038 Uiso 1 1 calc R . .
O11 O 1.0070(3) 0.0415(3) 0.3362(2) 0.0420(7) Uani 1 1 d . . .
H11A H 0.9917 -0.0310 0.3588 0.063 Uiso 1 1 d R . .
H11B H 0.9144 0.0612 0.3435 0.063 Uiso 1 1 d R . .
O12 O 0.6793(12) 0.1616(10) 0.9505(7) 0.094(3) Uani 0.50 1 d PU A -1
H12A H 0.6141 0.0921 0.9694 0.141 Uiso 0.50 1 d PR A -1
H12B H 0.6537 0.2264 0.9845 0.141 Uiso 0.50 1 d PR A -1
O13 O 0.5158(15) 0.2400(13) 0.1398(10) 0.054(3) Uani 0.25 1 d PU . .
H13A H 0.5136 0.2378 0.2042 0.081 Uiso 0.25 1 d PR . .
H13B H 0.5544 0.1829 0.1071 0.081 Uiso 0.25 1 d PR . .
O14 O 0.560(2) 0.0551(18) 0.9484(11) 0.069(4) Uani 0.25 1 d PU . .
H14A H 0.5332 0.1175 0.9274 0.104 Uiso 0.25 1 d PR . .
H14B H 0.4786 -0.0162 0.9261 0.104 Uiso 0.25 1 d PR . .


_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 O5 2.029(2) 2_557 ?
Ni1 O7 2.044(2) 2_656 ?
Ni1 O7 2.052(2) . ?
Ni1 O3 2.062(2) 2_667 ?
Ni1 O8 2.089(3) . ?
Ni1 O1 2.107(2) . ?
Ni2 O2 1.996(2) . ?
Ni2 O7 2.013(2) . ?
Ni2 O6 2.039(2) 1_654 ?
Ni2 O10 2.095(2) . ?
Ni2 O9 2.108(2) . ?
Ni2 O3 2.137(2) 2_667 ?
O1 C1 1.261(4) . ?
O2 C1 1.254(4) . ?
O7 Ni1 2.044(2) 2_656 ?
O7 H7A 0.8199 . ?
O10 H10A 0.8199 . ?
O10 H10B 0.8200 . ?
O9 H9A 0.8200 . ?
O9 H9B 0.8198 . ?
O3 C11 1.277(4) . ?
O3 Ni1 2.062(2) 2_667 ?
O3 Ni2 2.137(2) 2_667 ?
O4 C11 1.239(4) . ?
O5 C14 1.252(4) . ?
O5 Ni1 2.029(2) 2_557 ?
O6 C14 1.260(4) . ?
O6 Ni2 2.039(2) 1_456 ?
O8 H8A 0.8213 . ?
O8 H8B 0.8206 . ?
C9 C10 1.389(4) . ?
C9 C8 1.393(5) . ?
C9 H9 0.9300 . ?
C1 C2 1.490(5) . ?
C12 C13 1.381(5) . ?
C12 C10 1.383(4) . ?
C12 H12 0.9300 . ?
C5 C6 1.388(5) . ?
C5 C4 1.390(5) . ?
C5 C8 1.483(4) . ?
C14 C13 1.504(4) . ?
C10 C11 1.508(4) . ?
C2 C7 1.383(5) . ?
C2 C3 1.385(5) . ?
C3 C4 1.384(5) . ?
C3 H3 0.9300 . ?
C8 C15 1.390(5) . ?
C15 C13 1.388(4) . ?
C15 H15 0.9300 . ?
C7 C6 1.381(5) . ?
C7 H7 0.9300 . ?
C6 H6 0.9300 . ?
C4 H4 0.9300 . ?
O11 H11A 0.8201 . ?
O11 H11B 0.8199 . ?
O12 H12A 0.8196 . ?
O12 H12B 0.8201 . ?
O12 H14A 1.1087 . ?
O13 H13A 0.7924 . ?
O13 H13B 0.8089 . ?
O14 H12A 0.5066 . ?
O14 H14A 0.8187 . ?
O14 H14B 0.8210 . ?

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
O5 Ni1 O7 99.37(9) 2_557 2_656 ?
O5 Ni1 O7 93.99(9) 2_557 . ?
O7 Ni1 O7 80.87(9) 2_656 . ?
O5 Ni1 O3 163.00(9) 2_557 2_667 ?
O7 Ni1 O3 96.00(9) 2_656 2_667 ?
O7 Ni1 O3 81.28(9) . 2_667 ?
O5 Ni1 O8 90.84(10) 2_557 . ?
O7 Ni1 O8 92.73(10) 2_656 . ?
O7 Ni1 O8 172.54(9) . . ?
O3 Ni1 O8 95.66(10) 2_667 . ?
O5 Ni1 O1 80.85(9) 2_557 . ?
O7 Ni1 O1 178.24(9) 2_656 . ?
O7 Ni1 O1 100.86(9) . . ?
O3 Ni1 O1 84.01(9) 2_667 . ?
O8 Ni1 O1 85.51(10) . . ?
O2 Ni2 O7 95.22(9) . . ?
O2 Ni2 O6 166.00(10) . 1_654 ?
O7 Ni2 O6 98.66(9) . 1_654 ?
O2 Ni2 O10 82.41(10) . . ?
O7 Ni2 O10 176.58(9) . . ?
O6 Ni2 O10 83.81(9) 1_654 . ?
O2 Ni2 O9 85.52(9) . . ?
O7 Ni2 O9 90.54(9) . . ?
O6 Ni2 O9 92.46(9) 1_654 . ?
O10 Ni2 O9 91.72(9) . . ?
O2 Ni2 O3 91.97(9) . 2_667 ?
O7 Ni2 O3 80.37(9) . 2_667 ?
O6 Ni2 O3 92.19(9) 1_654 2_667 ?
O10 Ni2 O3 97.22(9) . 2_667 ?
O9 Ni2 O3 170.33(9) . 2_667 ?
C1 O1 Ni1 125.7(2) . . ?
C1 O2 Ni2 128.7(2) . . ?
Ni2 O7 Ni1 120.66(10) . 2_656 ?
Ni2 O7 Ni1 96.05(9) . . ?
Ni1 O7 Ni1 99.13(9) 2_656 . ?
Ni2 O7 H7A 121.8 . . ?
Ni1 O7 H7A 106.6 2_656 . ?
Ni1 O7 H7A 108.6 . . ?
Ni2 O10 H10A 117.3 . . ?
Ni2 O10 H10B 116.0 . . ?
H10A O10 H10B 107.1 . . ?
Ni2 O9 H9A 112.4 . . ?
Ni2 O9 H9B 97.2 . . ?
H9A O9 H9B 106.9 . . ?
C11 O3 Ni1 129.9(2) . 2_667 ?
C11 O3 Ni2 128.8(2) . 2_667 ?
Ni1 O3 Ni2 92.06(9) 2_667 2_667 ?
C14 O5 Ni1 130.9(2) . 2_557 ?
C14 O6 Ni2 131.6(2) . 1_456 ?
Ni1 O8 H8A 121.8 . . ?
Ni1 O8 H8B 106.3 . . ?
H8A O8 H8B 107.2 . . ?
C10 C9 C8 121.3(3) . . ?
C10 C9 H9 119.3 . . ?
C8 C9 H9 119.3 . . ?
O2 C1 O1 125.0(3) . . ?
O2 C1 C2 116.4(3) . . ?
O1 C1 C2 118.6(3) . . ?
C13 C12 C10 120.3(3) . . ?
C13 C12 H12 119.8 . . ?
C10 C12 H12 119.8 . . ?
C6 C5 C4 117.6(3) . . ?
C6 C5 C8 121.7(3) . . ?
C4 C5 C8 120.7(3) . . ?
O5 C14 O6 126.1(3) . . ?
O5 C14 C13 116.7(3) . . ?
O6 C14 C13 117.2(3) . . ?
C12 C10 C9 119.4(3) . . ?
C12 C10 C11 121.6(3) . . ?
C9 C10 C11 119.0(3) . . ?
C7 C2 C3 118.0(3) . . ?
C7 C2 C1 122.2(3) . . ?
C3 C2 C1 119.8(3) . . ?
C4 C3 C2 121.1(3) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
O4 C11 O3 124.9(3) . . ?
O4 C11 C10 119.9(3) . . ?
O3 C11 C10 115.2(3) . . ?
C15 C8 C9 118.0(3) . . ?
C15 C8 C5 121.4(3) . . ?
C9 C8 C5 120.6(3) . . ?
C13 C15 C8 121.2(3) . . ?
C13 C15 H15 119.4 . . ?
C8 C15 H15 119.4 . . ?
C12 C13 C15 119.6(3) . . ?
C12 C13 C14 119.7(3) . . ?
C15 C13 C14 120.7(3) . . ?
C6 C7 C2 121.0(3) . . ?
C6 C7 H7 119.5 . . ?
C2 C7 H7 119.5 . . ?
C7 C6 C5 121.4(3) . . ?
C7 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
C3 C4 C5 120.9(3) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
H11A O11 H11B 107.0 . . ?
H12A O12 H12B 107.2 . . ?
H12A O12 H14A 55.3 . . ?
H12B O12 H14A 84.6 . . ?
H13A O13 H13B 112.4 . . ?
H12A O14 H14A 85.9 . . ?
H12A O14 H14B 165.3 . . ?
H14A O14 H14B 107.7 . . ?

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
O5 Ni1 O1 C1 -117.3(3) 2_557 . . . ?
O7 Ni1 O1 C1 145(3) 2_656 . . . ?
O7 Ni1 O1 C1 -25.0(3) . . . . ?
O3 Ni1 O1 C1 54.9(3) 2_667 . . . ?
O8 Ni1 O1 C1 151.1(3) . . . . ?
O7 Ni2 O2 C1 60.1(3) . . . . ?
O6 Ni2 O2 C1 -127.6(4) 1_654 . . . ?
O10 Ni2 O2 C1 -117.4(3) . . . . ?
O9 Ni2 O2 C1 150.2(3) . . . . ?
O3 Ni2 O2 C1 -20.4(3) 2_667 . . . ?
O2 Ni2 O7 Ni1 -171.49(12) . . . 2_656 ?
O6 Ni2 O7 Ni1 10.39(14) 1_654 . . 2_656 ?
O10 Ni2 O7 Ni1 -125.6(15) . . . 2_656 ?
O9 Ni2 O7 Ni1 102.96(12) . . . 2_656 ?
O3 Ni2 O7 Ni1 -80.37(12) 2_667 . . 2_656 ?
O2 Ni2 O7 Ni1 -67.12(10) . . . . ?
O6 Ni2 O7 Ni1 114.76(9) 1_654 . . . ?
O10 Ni2 O7 Ni1 -21.2(15) . . . . ?
O9 Ni2 O7 Ni1 -152.67(9) . . . . ?
O3 Ni2 O7 Ni1 23.99(8) 2_667 . . . ?
O5 Ni1 O7 Ni2 138.70(9) 2_557 . . . ?
O7 Ni1 O7 Ni2 -122.44(12) 2_656 . . . ?
O3 Ni1 O7 Ni2 -24.86(9) 2_667 . . . ?
O8 Ni1 O7 Ni2 -91.1(8) . . . . ?
O1 Ni1 O7 Ni2 57.27(10) . . . . ?
O5 Ni1 O7 Ni1 -98.86(9) 2_557 . . 2_656 ?
O7 Ni1 O7 Ni1 0.0 2_656 . . 2_656 ?
O3 Ni1 O7 Ni1 97.58(9) 2_667 . . 2_656 ?
O8 Ni1 O7 Ni1 31.3(8) . . . 2_656 ?
O1 Ni1 O7 Ni1 179.70(9) . . . 2_656 ?
Ni2 O2 C1 O1 -21.0(5) . . . . ?
Ni2 O2 C1 C2 159.7(2) . . . . ?
Ni1 O1 C1 O2 1.1(5) . . . . ?
Ni1 O1 C1 C2 -179.5(2) . . . . ?
Ni1 O5 C14 O6 19.9(5) 2_557 . . . ?
Ni1 O5 C14 C13 -161.0(2) 2_557 . . . ?
Ni2 O6 C14 O5 23.3(5) 1_456 . . . ?
Ni2 O6 C14 C13 -155.8(2) 1_456 . . . ?
C13 C12 C10 C9 3.5(5) . . . . ?
C13 C12 C10 C11 -177.5(3) . . . . ?
C8 C9 C10 C12 -0.5(5) . . . . ?
C8 C9 C10 C11 -179.5(3) . . . . ?
O2 C1 C2 C7 154.7(4) . . . . ?
O1 C1 C2 C7 -24.7(5) . . . . ?
O2 C1 C2 C3 -24.3(5) . . . . ?
O1 C1 C2 C3 156.3(4) . . . . ?
C7 C2 C3 C4 2.7(6) . . . . ?
C1 C2 C3 C4 -178.3(3) . . . . ?
Ni1 O3 C11 O4 -22.7(5) 2_667 . . . ?
Ni2 O3 C11 O4 114.2(3) 2_667 . . . ?
Ni1 O3 C11 C10 156.3(2) 2_667 . . . ?
Ni2 O3 C11 C10 -66.8(4) 2_667 . . . ?
C12 C10 C11 O4 -35.1(5) . . . . ?
C9 C10 C11 O4 143.9(3) . . . . ?
C12 C10 C11 O3 145.8(3) . . . . ?
C9 C10 C11 O3 -35.2(4) . . . . ?
C10 C9 C8 C15 -2.2(5) . . . . ?
C10 C9 C8 C5 176.9(3) . . . . ?
C6 C5 C8 C15 -34.9(6) . . . . ?
C4 C5 C8 C15 145.0(4) . . . . ?
C6 C5 C8 C9 146.0(4) . . . . ?
C4 C5 C8 C9 -34.1(5) . . . . ?
C9 C8 C15 C13 1.8(5) . . . . ?
C5 C8 C15 C13 -177.3(3) . . . . ?
C10 C12 C13 C15 -3.8(5) . . . . ?
C10 C12 C13 C14 176.1(3) . . . . ?
C8 C15 C13 C12 1.1(5) . . . . ?
C8 C15 C13 C14 -178.8(3) . . . . ?
O5 C14 C13 C12 -154.1(3) . . . . ?
O6 C14 C13 C12 25.1(5) . . . . ?
O5 C14 C13 C15 25.9(5) . . . . ?
O6 C14 C13 C15 -155.0(3) . . . . ?
C3 C2 C7 C6 -1.0(6) . . . . ?
C1 C2 C7 C6 180.0(4) . . . . ?
C2 C7 C6 C5 -0.7(7) . . . . ?
C4 C5 C6 C7 0.7(6) . . . . ?
C8 C5 C6 C7 -179.4(4) . . . . ?
C2 C3 C4 C5 -2.8(6) . . . . ?
C6 C5 C4 C3 1.0(6) . . . . ?
C8 C5 C4 C3 -178.9(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7A O4 0.82 2.40 3.091(3) 142.6 1_544
O10 H10A O9 0.82 2.24 2.944(3) 144.8 2_666
O10 H10B O6 0.82 2.08 2.840(3) 153.7 2_567
O9 H9A O11 0.82 2.10 2.853(4) 152.9 1_455
O9 H9B O2 0.82 2.38 2.788(3) 111.4 .
O9 H9B O4 0.82 1.97 2.738(3) 156.8 2_567
O8 H8A O11 0.82 2.01 2.808(4) 165.0 2_756
O8 H8B O12 0.82 2.10 2.914(9) 172.9 .
O8 H8B O14 0.82 2.06 2.737(13) 139.3 .
O11 H11A O4 0.82 2.18 2.954(4) 157.1 1_644
O11 H11B O5 0.82 2.16 2.971(3) 169.5 1_654
O13 H13A O8 0.79 2.40 2.834(12) 115.8 2_656
O13 H13B O12 0.81 2.19 2.816(16) 134.4 1_554
O13 H13B O14 0.81 2.19 2.90(2) 146.5 1_554
O13 H13B O14 0.81 2.34 2.97(2) 134.3 2_656
O14 H14A O1 0.82 2.16 2.713(14) 124.5 .
O14 H14B O12 0.82 2.40 2.93(2) 122.4 2_657
O14 H14B O13 0.82 2.36 2.97(2) 130.8 2_656

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.05
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.083
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_B-ZH27-15
_database_code_depnum_ccdc_archive 'CCDC 1433662'
_audit_update_record             
;
2015-10-28 deposited with the CCDC.
2016-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H48 N8 Ni7 O25'
_chemical_formula_weight         1643.99

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   31.086(6)
_cell_length_b                   12.676(3)
_cell_length_c                   16.113(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.06(3)
_cell_angle_gamma                90
_cell_volume                     6209(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_F_000             3344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    2.167
_shelx_estimated_absorpt_T_min   0.613
_shelx_estimated_absorpt_T_max   0.671
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.720
_diffrn_radiation_type           synchrotron
_diffrn_source                   ?
_diffrn_measurement_device_type  mar
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9556
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.110
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_full        25.050
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measured_fraction_theta_full 0.944
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_Laue_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_point_group_measured_fraction_full 0.944
_reflns_number_total             4997
_reflns_number_gt                4319
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1058P)²+0.4180P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4997
_refine_ls_number_parameters     428
_refine_ls_number_restraints     144
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.1009
_refine_ls_wR_factor_ref         0.3006
_refine_ls_wR_factor_gt          0.2946
_refine_ls_goodness_of_fit_ref   2.273
_refine_ls_restrained_S_all      2.326
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.58349(3) 0.77661(9) 0.68735(8) 0.0168(4) Uani 1 1 d . U . A 4
Ni2 Ni 0.50627(3) 0.79254(9) 0.54125(7) 0.0163(4) Uani 1 1 d . . . A 4
Ni3 Ni 0.5000 0.29722(13) 0.2500 0.0162(4) Uani 1 2 d S TU P A 4
Ni4 Ni 0.95034(3) 0.50432(10) 0.49259(8) 0.0225(4) Uani 1 1 d . . . A 4
O1 O 0.61193(19) 0.7145(5) 0.5957(4) 0.0177(14) Uani 1 1 d . U . A 4
O2 O 0.55264(19) 0.7158(5) 0.4884(4) 0.0188(14) Uani 1 1 d . U . A 4
O3 O 0.5444(2) 0.4109(5) 0.2972(4) 0.0239(15) Uani 1 1 d . . . A 4
O4 O 0.60664(18) 0.3486(5) 0.2645(4) 0.0227(15) Uani 1 1 d . . . A 4
O5 O 0.89745(19) 0.5771(6) 0.5355(5) 0.0257(16) Uani 1 1 d . . . A 4
O6 O 0.88685(19) 0.4422(6) 0.4481(5) 0.0298(17) Uani 1 1 d . U . A 4
O7 O 0.55329(19) 0.8958(5) 0.6093(4) 0.0202(14) Uani 1 1 d . . . A 4
H7A H 0.5366 0.9179 0.6415 0.030 Uiso 1 1 d R U . A 4
O8 O 0.99558(18) 0.4090(5) 0.4538(4) 0.0208(15) Uani 1 1 d . . . A 4
H8A H 0.9875 0.4160 0.4005 0.031 Uiso 1 1 d R U . A 4
O9 O 0.47625(19) 0.2972(5) 0.3557(4) 0.0192(14) Uani 1 1 d . . . A 4
H9A H 0.4784 0.3743 0.3633 0.029 Uiso 1 1 d R U . A 4
O10 O 0.45173(19) 0.1798(5) 0.2149(4) 0.0189(14) Uani 1 1 d . . . A 4
O11 O 0.45967(19) 0.1131(5) 0.0907(4) 0.0214(14) Uani 1 1 d . . . A 4
N1 N 0.6399(2) 0.8602(7) 0.7366(5) 0.0236(18) Uani 1 1 d . . . A 4
N2 N 0.7098(3) 0.8998(8) 0.7895(6) 0.041(2) Uani 1 1 d . U . A 4
N3 N 0.8925(3) 0.8696(8) 0.9116(6) 0.036(2) Uani 1 1 d . U . A 4
N4 N 0.9575(2) 0.8056(6) 0.9748(5) 0.0189(17) Uani 1 1 d . . . A 4
C1 C 0.5917(3) 0.6911(7) 0.5241(6) 0.019(2) Uani 1 1 d . U . A 4
C2 C 0.6149(3) 0.6229(7) 0.4716(6) 0.0195(19) Uani 1 1 d . U . A 4
C3 C 0.5908(3) 0.5541(7) 0.4092(6) 0.021(2) Uani 1 1 d . . . A 4
H3 H 0.5596 0.5564 0.3969 0.026 Uiso 1 1 calc R U . A 4
C4 C 0.6118(3) 0.4854(7) 0.3673(6) 0.0175(19) Uani 1 1 d . . . A 4
C5 C 0.6575(3) 0.4810(9) 0.3826(7) 0.032(2) Uani 1 1 d . . . A 4
H5 H 0.6716 0.4326 0.3518 0.038 Uiso 1 1 calc R U . A 4
C6 C 0.6827(3) 0.5467(8) 0.4424(7) 0.028(2) Uani 1 1 d . U . A 4
C7 C 0.6616(3) 0.6160(8) 0.4884(6) 0.022(2) Uani 1 1 d . . . A 4
H7 H 0.6786 0.6588 0.5315 0.026 Uiso 1 1 calc R U . A 4
C8 C 0.5850(3) 0.4073(8) 0.3043(6) 0.020(2) Uani 1 1 d . U . A 4
C9 C 0.73206(16) 0.5396(7) 0.4549(6) 0.035(3) Uani 1 1 d G U . A 4
C10 C 0.7587(2) 0.6114(6) 0.5072(6) 0.053(3) Uani 1 1 d G U . A 4
H10 H 0.7458 0.6651 0.5352 0.064 Uiso 1 1 calc R U . A 4
C11 C 0.8042(2) 0.6047(7) 0.5186(6) 0.070(5) Uani 1 1 d G . . A 4
H11 H 0.8223 0.6538 0.5544 0.085 Uiso 1 1 calc R U . A 4
C12 C 0.82304(17) 0.5262(7) 0.4777(6) 0.030(2) Uani 1 1 d G U . A 4
C13 C 0.7964(3) 0.4544(8) 0.4253(7) 0.100(6) Uani 1 1 d G U . A 4
H13 H 0.8093 0.4008 0.3973 0.120 Uiso 1 1 calc R U . A 4
C14 C 0.7509(2) 0.4611(8) 0.4139(7) 0.106(7) Uani 1 1 d G U . A 4
H14 H 0.7328 0.4120 0.3781 0.128 Uiso 1 1 calc R U . A 4
C15 C 0.8723(3) 0.5139(8) 0.4864(7) 0.025(2) Uani 1 1 d . . . A 4
C16 C 0.6439(3) 0.9689(10) 0.7456(9) 0.048(4) Uani 1 1 d . . . A 4
H16 H 0.6205 1.0180 0.7305 0.057 Uiso 1 1 calc R U . A 4
C17 C 0.6866(4) 0.9944(11) 0.7795(10) 0.059(4) Uani 1 1 d . . . A 4
H17 H 0.6982 1.0629 0.7936 0.071 Uiso 1 1 calc R U . A 4
C18 C 0.6793(3) 0.8232(10) 0.7638(8) 0.040(3) Uani 1 1 d . U . A 4
H18 H 0.6861 0.7501 0.7657 0.048 Uiso 1 1 calc R U . A 4
C25 C 0.9145(3) 0.7916(8) 0.9606(7) 0.030(2) Uani 1 1 d . U . A 4
H25 H 0.9006 0.7339 0.9821 0.036 Uiso 1 1 calc R U . A 4
C22 C 0.84575(19) 0.8808(8) 0.8846(7) 0.057(4) Uani 1 1 d G . . A 4
C23 C 0.8177(3) 0.8084(8) 0.9106(8) 0.095(6) Uani 1 1 d G U . A 4
H23 H 0.8294 0.7532 0.9485 0.114 Uiso 1 1 calc R U . A 4
C24 C 0.7725(3) 0.8167(9) 0.8810(8) 0.089(6) Uani 1 1 d G U . A 4
H24 H 0.7533 0.7673 0.8987 0.107 Uiso 1 1 calc R U . A 4
C19 C 0.75537(17) 0.8975(9) 0.8255(7) 0.063(5) Uani 1 1 d G . . A 4
C20 C 0.7835(2) 0.9699(7) 0.7995(7) 0.068(5) Uani 1 1 d G . . A 4
H20 H 0.7718 1.0251 0.7616 0.082 Uiso 1 1 calc R U . A 4
C21 C 0.8286(2) 0.9616(8) 0.8291(7) 0.066(5) Uani 1 1 d G . . A 4
H21 H 0.8478 1.0111 0.8114 0.079 Uiso 1 1 calc R U . A 4
C26 C 0.9241(3) 0.9419(10) 0.8957(8) 0.041(3) Uani 1 1 d . U . A 4
H26 H 0.9191 1.0053 0.8637 0.049 Uiso 1 1 calc R U . A 4
C27 C 0.9629(3) 0.9021(10) 0.9356(8) 0.036(3) Uani 1 1 d . . . A 4
H27 H 0.9905 0.9350 0.9370 0.043 Uiso 1 1 calc R U . A 4
C28 C 0.4419(3) 0.1171(8) 0.1536(6) 0.021(2) Uani 1 1 d . . . A 4
H28 H 0.4204 0.0667 0.1549 0.025 Uiso 1 1 d R U . A 4
O12 O 0.4179(8) 0.7978(14) 0.1906(14) 0.070(6) Uani 0.5 1 d . U P B 4
H12A H 0.4032 0.7969 0.1397 0.104 Uiso 0.5 1 d R U P B 4
H12B H 0.4036 0.7623 0.2206 0.104 Uiso 0.5 1 d R U P B 4
O13 O 0.4717(7) 0.9285(15) 0.2890(13) 0.075(7) Uani 0.5 1 d . . P C 4
H13A H 0.4850 0.9779 0.2691 0.113 Uiso 0.5 1 d R U P C 4
H13B H 0.4490 0.9548 0.3026 0.113 Uiso 0.5 1 d R U P C 4
O14 O 0.5000 0.640(2) 0.2500 0.075(9) Uani 0.5 2 d S TU P D 4
H14A H 0.5195 0.6018 0.2397 0.075 Uiso 0.5 1 d R U P D 4
O15 O 0.4604(17) 0.824(5) 0.286(3) 0.093(16) Uani 0.25 1 d . U P E -1
H15A H 0.4802 0.7856 0.3101 0.140 Uiso 0.25 1 d R U P E -1
H15B H 0.4372 0.7920 0.2822 0.140 Uiso 0.25 1 d R U P E -1


_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 O1 2.031(6) . ?
Ni1 O4 2.052(7) 6_566 ?
Ni1 N1 2.059(7) . ?
Ni1 O7 2.062(6) . ?
Ni1 O9 2.066(6) 5_666 ?
Ni1 O10 2.169(6) 5_666 ?
Ni1 Ni2 2.9975(18) . ?
Ni2 O9 1.993(6) 5_666 ?
Ni2 O8 2.020(7) 3_455 ?
Ni2 O2 2.064(6) . ?
Ni2 N4 2.076(8) 8_465 ?
Ni2 O7 2.093(6) . ?
Ni2 O11 2.156(6) 6_566 ?
Ni3 O9 1.992(7) 2_655 ?
Ni3 O9 1.992(7) . ?
Ni3 O3 2.029(7) . ?
Ni3 O3 2.029(7) 2_655 ?
Ni3 O10 2.105(6) 2_655 ?
Ni3 O10 2.105(6) . ?
Ni4 O8 2.043(6) 5_766 ?
Ni4 O8 2.049(6) . ?
Ni4 O7 2.057(7) 7_666 ?
Ni4 O6 2.107(6) . ?
Ni4 O5 2.123(6) . ?
Ni4 O11 2.147(7) 8_556 ?
Ni4 C15 2.410(9) . ?
O1 C1 1.230(11) . ?
O2 C1 1.269(10) . ?
O3 C8 1.246(11) . ?
O4 C8 1.264(12) . ?
O4 Ni1 2.052(7) 6_565 ?
O5 C15 1.273(12) . ?
O6 C15 1.236(13) . ?
O7 Ni4 2.057(7) 7_666 ?
O7 H7A 0.8549 . ?
O8 Ni2 2.019(7) 3_545 ?
O8 Ni4 2.043(6) 5_766 ?
O8 H8A 0.8466 . ?
O9 Ni2 1.993(6) 5_666 ?
O9 Ni1 2.066(6) 5_666 ?
O9 H9A 0.9849 . ?
O10 C28 1.256(11) . ?
O10 Ni1 2.169(6) 5_666 ?
O11 C28 1.251(11) . ?
O11 Ni4 2.147(7) 8_455 ?
O11 Ni2 2.156(6) 6_565 ?
N1 C18 1.300(13) . ?
N1 C16 1.389(15) . ?
N2 C18 1.360(15) . ?
N2 C17 1.390(17) . ?
N2 C19 1.414(10) . ?
N3 C25 1.359(14) . ?
N3 C26 1.407(15) . ?
N3 C22 1.433(10) . ?
N4 C25 1.322(12) . ?
N4 C27 1.403(14) . ?
N4 Ni2 2.076(8) 8_566 ?
C1 C2 1.497(13) . ?
C2 C3 1.421(13) . ?
C2 C7 1.422(12) . ?
C3 C4 1.352(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(13) . ?
C4 C8 1.534(12) . ?
C5 C6 1.386(15) . ?
C5 H5 0.9500 . ?
C6 C7 1.399(14) . ?
C6 C9 1.507(10) . ?
C7 H7 0.9500 . ?
C9 C10 1.3900 . ?
C9 C14 1.3900 . ?
C10 C11 1.3900 . ?
C10 H10 0.9500 . ?
C11 C12 1.3900 . ?
C11 H11 0.9500 . ?
C12 C13 1.3900 . ?
C12 C15 1.517(10) . ?
C13 C14 1.3900 . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C16 C17 1.365(15) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C25 H25 0.9500 . ?
C22 C23 1.3900 . ?
C22 C21 1.3900 . ?
C23 C24 1.3900 . ?
C23 H23 0.9500 . ?
C24 C19 1.3900 . ?
C24 H24 0.9500 . ?
C19 C20 1.3900 . ?
C20 C21 1.3900 . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C26 C27 1.340(15) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 H28 0.9281 . ?
O12 H12A 0.8500 . ?
O12 H12B 0.8499 . ?
O13 H13A 0.8499 . ?
O13 H13B 0.8501 . ?
O14 H14A 0.8193 . ?
O15 H15A 0.8182 . ?
O15 H15B 0.8205 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O4 89.4(3) . 6_566 ?
O1 Ni1 N1 90.9(3) . . ?
O4 Ni1 N1 90.1(3) 6_566 . ?
O1 Ni1 O7 93.0(3) . . ?
O4 Ni1 O7 173.6(2) 6_566 . ?
N1 Ni1 O7 95.8(3) . . ?
O1 Ni1 O9 94.5(3) . 5_666 ?
O4 Ni1 O9 91.7(2) 6_566 5_666 ?
N1 Ni1 O9 174.4(3) . 5_666 ?
O7 Ni1 O9 82.2(2) . 5_666 ?
O1 Ni1 O10 171.4(2) . 5_666 ?
O4 Ni1 O10 85.6(3) 6_566 5_666 ?
N1 Ni1 O10 96.2(3) . 5_666 ?
O7 Ni1 O10 91.3(3) . 5_666 ?
O9 Ni1 O10 78.7(2) 5_666 5_666 ?
O1 Ni1 Ni2 81.61(17) . . ?
O4 Ni1 Ni2 130.54(18) 6_566 . ?
N1 Ni1 Ni2 138.2(2) . . ?
O7 Ni1 Ni2 44.24(17) . . ?
O9 Ni1 Ni2 41.47(18) 5_666 . ?
O10 Ni1 Ni2 96.32(16) 5_666 . ?
O9 Ni2 O8 167.2(3) 5_666 3_455 ?
O9 Ni2 O2 89.0(3) 5_666 . ?
O8 Ni2 O2 94.8(3) 3_455 . ?
O9 Ni2 N4 97.5(3) 5_666 8_465 ?
O8 Ni2 N4 94.7(3) 3_455 8_465 ?
O2 Ni2 N4 90.1(3) . 8_465 ?
O9 Ni2 O7 83.2(2) 5_666 . ?
O8 Ni2 O7 84.5(3) 3_455 . ?
O2 Ni2 O7 92.2(2) . . ?
N4 Ni2 O7 177.6(3) 8_465 . ?
O9 Ni2 O11 95.5(3) 5_666 6_566 ?
O8 Ni2 O11 80.1(2) 3_455 6_566 ?
O2 Ni2 O11 174.3(3) . 6_566 ?
N4 Ni2 O11 92.8(3) 8_465 6_566 ?
O7 Ni2 O11 84.8(2) . 6_566 ?
O9 Ni2 Ni1 43.34(17) 5_666 . ?
O8 Ni2 Ni1 125.82(17) 3_455 . ?
O2 Ni2 Ni1 77.21(17) . . ?
N4 Ni2 Ni1 138.0(2) 8_465 . ?
O7 Ni2 Ni1 43.42(17) . . ?
O11 Ni2 Ni1 103.69(17) 6_566 . ?
O9 Ni3 O9 180.0(4) 2_655 . ?
O9 Ni3 O3 88.6(3) 2_655 . ?
O9 Ni3 O3 91.4(3) . . ?
O9 Ni3 O3 91.4(3) 2_655 2_655 ?
O9 Ni3 O3 88.6(3) . 2_655 ?
O3 Ni3 O3 89.5(4) . 2_655 ?
O9 Ni3 O10 81.9(2) 2_655 2_655 ?
O9 Ni3 O10 98.1(2) . 2_655 ?
O3 Ni3 O10 90.6(3) . 2_655 ?
O3 Ni3 O10 173.2(3) 2_655 2_655 ?
O9 Ni3 O10 98.1(2) 2_655 . ?
O9 Ni3 O10 81.9(2) . . ?
O3 Ni3 O10 173.2(3) . . ?
O3 Ni3 O10 90.6(3) 2_655 . ?
O10 Ni3 O10 90.0(4) 2_655 . ?
O8 Ni4 O8 83.7(3) 5_766 . ?
O8 Ni4 O7 84.8(3) 5_766 7_666 ?
O8 Ni4 O7 92.7(3) . 7_666 ?
O8 Ni4 O6 167.1(3) 5_766 . ?
O8 Ni4 O6 109.2(3) . . ?
O7 Ni4 O6 93.9(3) 7_666 . ?
O8 Ni4 O5 104.7(3) 5_766 . ?
O8 Ni4 O5 169.5(3) . . ?
O7 Ni4 O5 94.3(3) 7_666 . ?
O6 Ni4 O5 62.6(3) . . ?
O8 Ni4 O11 95.1(2) 5_766 8_556 ?
O8 Ni4 O11 79.6(2) . 8_556 ?
O7 Ni4 O11 172.3(3) 7_666 8_556 ?
O6 Ni4 O11 88.0(3) . 8_556 ?
O5 Ni4 O11 93.2(3) . 8_556 ?
O8 Ni4 C15 136.3(3) 5_766 . ?
O8 Ni4 C15 140.0(3) . . ?
O7 Ni4 C15 92.8(3) 7_666 . ?
O6 Ni4 C15 30.8(3) . . ?
O5 Ni4 C15 31.8(3) . . ?
O11 Ni4 C15 92.6(3) 8_556 . ?
C1 O1 Ni1 124.1(6) . . ?
C1 O2 Ni2 127.8(6) . . ?
C8 O3 Ni3 127.3(6) . . ?
C8 O4 Ni1 127.3(5) . 6_565 ?
C15 O5 Ni4 86.6(6) . . ?
C15 O6 Ni4 88.2(6) . . ?
Ni4 O7 Ni1 151.6(3) 7_666 . ?
Ni4 O7 Ni2 92.9(2) 7_666 . ?
Ni1 O7 Ni2 92.3(3) . . ?
Ni4 O7 H7A 110.1 7_666 . ?
Ni1 O7 H7A 97.3 . . ?
Ni2 O7 H7A 94.5 . . ?
Ni2 O8 Ni4 95.6(2) 3_545 5_766 ?
Ni2 O8 Ni4 104.0(3) 3_545 . ?
Ni4 O8 Ni4 96.3(3) 5_766 . ?
Ni2 O8 H8A 139.0 3_545 . ?
Ni4 O8 H8A 114.5 5_766 . ?
Ni4 O8 H8A 99.8 . . ?
Ni3 O9 Ni2 128.8(3) . 5_666 ?
Ni3 O9 Ni1 100.4(3) . 5_666 ?
Ni2 O9 Ni1 95.2(3) 5_666 5_666 ?
Ni3 O9 H9A 94.5 . . ?
Ni2 O9 H9A 117.5 5_666 . ?
Ni1 O9 H9A 121.6 5_666 . ?
C28 O10 Ni3 134.5(6) . . ?
C28 O10 Ni1 131.0(5) . 5_666 ?
Ni3 O10 Ni1 93.7(2) . 5_666 ?
C28 O11 Ni4 127.6(6) . 8_455 ?
C28 O11 Ni2 136.1(6) . 6_565 ?
Ni4 O11 Ni2 96.3(3) 8_455 6_565 ?
C18 N1 C16 105.3(9) . . ?
C18 N1 Ni1 127.7(8) . . ?
C16 N1 Ni1 127.0(6) . . ?
C18 N2 C17 105.6(9) . . ?
C18 N2 C19 133.3(11) . . ?
C17 N2 C19 121.0(10) . . ?
C25 N3 C26 107.1(9) . . ?
C25 N3 C22 127.1(9) . . ?
C26 N3 C22 125.7(9) . . ?
C25 N4 C27 104.6(8) . . ?
C25 N4 Ni2 127.7(7) . 8_566 ?
C27 N4 Ni2 127.7(6) . 8_566 ?
O1 C1 O2 128.3(9) . . ?
O1 C1 C2 117.1(7) . . ?
O2 C1 C2 114.6(8) . . ?
C3 C2 C7 117.6(9) . . ?
C3 C2 C1 120.5(8) . . ?
C7 C2 C1 121.5(8) . . ?
C4 C3 C2 120.6(8) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 121.3(9) . . ?
C3 C4 C8 119.6(8) . . ?
C5 C4 C8 119.0(9) . . ?
C6 C5 C4 120.5(10) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C7 119.1(9) . . ?
C5 C6 C9 117.9(9) . . ?
C7 C6 C9 123.0(8) . . ?
C6 C7 C2 120.8(9) . . ?
C6 C7 H7 119.6 . . ?
C2 C7 H7 119.6 . . ?
O3 C8 O4 127.8(8) . . ?
O3 C8 C4 116.0(8) . . ?
O4 C8 C4 116.2(7) . . ?
C10 C9 C14 120.0 . . ?
C10 C9 C6 120.1(6) . . ?
C14 C9 C6 119.9(6) . . ?
C9 C10 C11 120.0 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 120.0 . . ?
C11 C12 C15 123.3(7) . . ?
C13 C12 C15 116.7(7) . . ?
C12 C13 C14 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C9 120.0 . . ?
C13 C14 H14 120.0 . . ?
C9 C14 H14 120.0 . . ?
O6 C15 O5 122.2(8) . . ?
O6 C15 C12 119.8(9) . . ?
O5 C15 C12 118.0(9) . . ?
O6 C15 Ni4 60.9(5) . . ?
O5 C15 Ni4 61.6(5) . . ?
C12 C15 Ni4 175.8(7) . . ?
C17 C16 N1 109.6(10) . . ?
C17 C16 H16 125.2 . . ?
N1 C16 H16 125.2 . . ?
C16 C17 N2 106.2(11) . . ?
C16 C17 H17 126.9 . . ?
N2 C17 H17 126.9 . . ?
N1 C18 N2 113.2(11) . . ?
N1 C18 H18 123.4 . . ?
N2 C18 H18 123.4 . . ?
N4 C25 N3 111.8(10) . . ?
N4 C25 H25 124.1 . . ?
N3 C25 H25 124.1 . . ?
C23 C22 C21 120.0 . . ?
C23 C22 N3 120.3(7) . . ?
C21 C22 N3 119.7(7) . . ?
C24 C23 C22 120.0 . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C19 120.0 . . ?
C23 C24 H24 120.0 . . ?
C19 C24 H24 120.0 . . ?
C20 C19 C24 120.0 . . ?
C20 C19 N2 120.1(7) . . ?
C24 C19 N2 119.7(7) . . ?
C19 C20 C21 120.0 . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C20 C21 C22 120.0 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C27 C26 N3 105.1(10) . . ?
C27 C26 H26 127.4 . . ?
N3 C26 H26 127.4 . . ?
C26 C27 N4 111.3(9) . . ?
C26 C27 H27 124.3 . . ?
N4 C27 H27 124.3 . . ?
O11 C28 O10 126.0(9) . . ?
O11 C28 H28 115.5 . . ?
O10 C28 H28 118.4 . . ?
H12A O12 H12B 107.7 . . ?
H13A O13 H13B 107.7 . . ?
H15A O15 H15B 107.3 . . ?

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
Ni1 O1 C1 O2 13.1(14) . . . . ?
Ni1 O1 C1 C2 -165.6(6) . . . . ?
Ni2 O2 C1 O1 -6.6(14) . . . . ?
Ni2 O2 C1 C2 172.1(6) . . . . ?
O1 C1 C2 C3 151.1(9) . . . . ?
O2 C1 C2 C3 -27.7(13) . . . . ?
O1 C1 C2 C7 -21.8(13) . . . . ?
O2 C1 C2 C7 159.3(9) . . . . ?
C7 C2 C3 C4 -0.6(14) . . . . ?
C1 C2 C3 C4 -173.8(9) . . . . ?
C2 C3 C4 C5 -1.1(15) . . . . ?
C2 C3 C4 C8 176.3(8) . . . . ?
C3 C4 C5 C6 0.7(16) . . . . ?
C8 C4 C5 C6 -176.7(10) . . . . ?
C4 C5 C6 C7 1.4(17) . . . . ?
C4 C5 C6 C9 -178.9(10) . . . . ?
C5 C6 C7 C2 -3.0(16) . . . . ?
C9 C6 C7 C2 177.2(9) . . . . ?
C3 C2 C7 C6 2.6(15) . . . . ?
C1 C2 C7 C6 175.8(9) . . . . ?
Ni3 O3 C8 O4 21.2(15) . . . . ?
Ni3 O3 C8 C4 -160.4(6) . . . . ?
Ni1 O4 C8 O3 -9.9(15) 6_565 . . . ?
Ni1 O4 C8 C4 171.6(6) 6_565 . . . ?
C3 C4 C8 O3 -1.7(14) . . . . ?
C5 C4 C8 O3 175.8(9) . . . . ?
C3 C4 C8 O4 176.9(9) . . . . ?
C5 C4 C8 O4 -5.6(14) . . . . ?
C5 C6 C9 C10 173.1(9) . . . . ?
C7 C6 C9 C10 -7.2(15) . . . . ?
C5 C6 C9 C14 -6.9(13) . . . . ?
C7 C6 C9 C14 172.8(9) . . . . ?
C14 C9 C10 C11 0.0 . . . . ?
C6 C9 C10 C11 -180.0(9) . . . . ?
C9 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C10 C11 C12 C15 179.7(9) . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C15 C12 C13 C14 -179.7(8) . . . . ?
C12 C13 C14 C9 0.0 . . . . ?
C10 C9 C14 C13 0.0 . . . . ?
C6 C9 C14 C13 180.0(9) . . . . ?
Ni4 O6 C15 O5 -6.8(10) . . . . ?
Ni4 O6 C15 C12 175.3(8) . . . . ?
Ni4 O5 C15 O6 6.8(10) . . . . ?
Ni4 O5 C15 C12 -175.3(8) . . . . ?
C11 C12 C15 O6 180.0(8) . . . . ?
C13 C12 C15 O6 -0.3(12) . . . . ?
C11 C12 C15 O5 2.0(13) . . . . ?
C13 C12 C15 O5 -178.3(8) . . . . ?
C18 N1 C16 C17 -0.5(16) . . . . ?
Ni1 N1 C16 C17 -179.0(9) . . . . ?
N1 C16 C17 N2 1.7(17) . . . . ?
C18 N2 C17 C16 -2.2(16) . . . . ?
C19 N2 C17 C16 -178.4(11) . . . . ?
C16 N1 C18 N2 -0.9(14) . . . . ?
Ni1 N1 C18 N2 177.5(7) . . . . ?
C17 N2 C18 N1 2.0(15) . . . . ?
C19 N2 C18 N1 177.5(11) . . . . ?
C27 N4 C25 N3 3.1(13) . . . . ?
Ni2 N4 C25 N3 -177.4(7) 8_566 . . . ?
C26 N3 C25 N4 -2.4(14) . . . . ?
C22 N3 C25 N4 -179.1(10) . . . . ?
C25 N3 C22 C23 1.8(16) . . . . ?
C26 N3 C22 C23 -174.4(10) . . . . ?
C25 N3 C22 C21 -175.2(10) . . . . ?
C26 N3 C22 C21 8.6(16) . . . . ?
C21 C22 C23 C24 0.0 . . . . ?
N3 C22 C23 C24 -177.0(11) . . . . ?
C22 C23 C24 C19 0.0 . . . . ?
C23 C24 C19 C20 0.0 . . . . ?
C23 C24 C19 N2 174.1(12) . . . . ?
C18 N2 C19 C20 139.5(12) . . . . ?
C17 N2 C19 C20 -45.6(16) . . . . ?
C18 N2 C19 C24 -34.6(17) . . . . ?
C17 N2 C19 C24 140.3(11) . . . . ?
C24 C19 C20 C21 0.0 . . . . ?
N2 C19 C20 C21 -174.1(12) . . . . ?
C19 C20 C21 C22 0.0 . . . . ?
C23 C22 C21 C20 0.0 . . . . ?
N3 C22 C21 C20 177.0(11) . . . . ?
C25 N3 C26 C27 0.5(14) . . . . ?
C22 N3 C26 C27 177.3(11) . . . . ?
N3 C26 C27 N4 1.4(14) . . . . ?
C25 N4 C27 C26 -2.8(13) . . . . ?
Ni2 N4 C27 C26 177.7(8) 8_566 . . . ?
Ni4 O11 C28 O10 171.3(7) 8_455 . . . ?
Ni2 O11 C28 O10 -8.7(15) 6_565 . . . ?
Ni3 O10 C28 O11 -3.4(15) . . . . ?
Ni1 O10 C28 O11 164.1(7) 5_666 . . . ?

_refine_diff_density_max         3.535
_refine_diff_density_min         -1.342
_refine_diff_density_rms         0.282

