# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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
#  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_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H54 N4 Ni3 O10'
_chemical_formula_weight         902.98

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                   9.450(3)
_cell_length_b                   18.825(6)
_cell_length_c                   12.001(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.273(8)
_cell_angle_gamma                90.00
_cell_volume                     2049.3(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9913
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       hexagonal
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             948
_exptl_absorpt_coefficient_mu    1.423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6587
_exptl_absorpt_correction_T_max  0.6914
_exptl_absorpt_process_details   SADABS

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26684
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         27.39
_reflns_number_total             4581
_reflns_number_gt                3896
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0800P)²+0.0550P] 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         4581
_refine_ls_number_parameters     252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.1081
_refine_ls_wR_factor_gt          0.1011
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_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
Ni2 Ni 0.5000 0.0000 0.0000 0.03437(12) Uani 1 2 d S . .
Ni1 Ni 0.51989(3) 0.143660(11) 0.121476(19) 0.03556(11) Uani 1 1 d . . .
O1 O 0.40203(15) 0.09944(7) -0.02882(11) 0.0405(3) Uani 1 1 d . . .
O2 O 0.66711(14) 0.06316(7) 0.11190(11) 0.0391(3) Uani 1 1 d . . .
O3 O 0.71010(18) 0.16679(7) 0.04835(13) 0.0497(4) Uani 1 1 d . . .
O4 O 0.39963(18) 0.09020(7) 0.20847(12) 0.0479(4) Uani 1 1 d . . .
O5 O 0.41075(17) -0.01756(7) 0.13327(12) 0.0467(3) Uani 1 1 d . . .
N2 N 0.6377(2) 0.20171(10) 0.27629(15) 0.0508(4) Uani 1 1 d . . .
N1 N 0.4036(2) 0.23253(9) 0.08438(16) 0.0477(4) Uani 1 1 d . . .
C9 C 0.6115(4) 0.27588(12) 0.2349(2) 0.0707(8) Uani 1 1 d . . .
H9A H 0.6701 0.2861 0.1822 0.085 Uiso 1 1 calc R . .
H9B H 0.6419 0.3081 0.3004 0.085 Uiso 1 1 calc R . .
C8 C 0.4526(3) 0.28713(12) 0.1743(2) 0.0660(7) Uani 1 1 d . . .
H8A H 0.3951 0.2841 0.2296 0.079 Uiso 1 1 calc R . .
H8B H 0.4383 0.3340 0.1392 0.079 Uiso 1 1 calc R . .
C7 C 0.3025(3) 0.24550(11) -0.0081(2) 0.0517(5) Uani 1 1 d . . .
H7 H 0.2605 0.2905 -0.0142 0.062 Uiso 1 1 calc R . .
C6 C 0.2456(2) 0.19831(11) -0.10451(19) 0.0472(5) Uani 1 1 d . . .
C1 C 0.2968(2) 0.12790(10) -0.11142(17) 0.0397(4) Uani 1 1 d . . .
C2 C 0.2302(3) 0.08896(12) -0.21275(19) 0.0551(6) Uani 1 1 d . . .
H2 H 0.2627 0.0432 -0.2210 0.066 Uiso 1 1 calc R . .
C3 C 0.1177(3) 0.11767(15) -0.2997(2) 0.0772(9) Uani 1 1 d . . .
H3 H 0.0737 0.0901 -0.3644 0.093 Uiso 1 1 calc R . .
C4 C 0.0684(3) 0.18552(17) -0.2940(3) 0.0857(9) Uani 1 1 d . . .
H4 H -0.0070 0.2042 -0.3542 0.103 Uiso 1 1 calc R . .
C5 C 0.1324(3) 0.22493(14) -0.1984(3) 0.0701(7) Uani 1 1 d . . .
H5 H 0.1003 0.2713 -0.1946 0.084 Uiso 1 1 calc R . .
C10 C 0.7965(3) 0.18817(19) 0.3227(3) 0.0794(9) Uani 1 1 d . . .
H10A H 0.8453 0.2265 0.3728 0.095 Uiso 1 1 calc R . .
H10B H 0.8429 0.1818 0.2607 0.095 Uiso 1 1 calc R . .
C11 C 0.7994(4) 0.1193(2) 0.3912(3) 0.0975(12) Uani 1 1 d . . .
H11A H 0.7916 0.0781 0.3412 0.117 Uiso 1 1 calc R . .
H11B H 0.8894 0.1157 0.4543 0.117 Uiso 1 1 calc R . .
C12 C 0.6682(5) 0.1252(2) 0.4365(3) 0.0989(12) Uani 1 1 d . . .
H12A H 0.6987 0.1318 0.5200 0.119 Uiso 1 1 calc R . .
H12B H 0.6087 0.0824 0.4188 0.119 Uiso 1 1 calc R . .
C13 C 0.5825(4) 0.18791(15) 0.3780(2) 0.0707(8) Uani 1 1 d . . .
H13A H 0.4778 0.1775 0.3538 0.085 Uiso 1 1 calc R . .
H13B H 0.5995 0.2286 0.4295 0.085 Uiso 1 1 calc R . .
C14 C 0.7469(2) 0.10419(10) 0.06919(17) 0.0406(4) Uani 1 1 d . . .
C15 C 0.8881(3) 0.07391(13) 0.0553(3) 0.0645(7) Uani 1 1 d . . .
H15A H 0.9396 0.0510 0.1277 0.077 Uiso 1 1 calc R . .
H15B H 0.8629 0.0372 -0.0037 0.077 Uiso 1 1 calc R . .
C16 C 0.9899(4) 0.12221(18) 0.0244(4) 0.1008(12) Uani 1 1 d . . .
H16A H 0.9496 0.1375 -0.0545 0.151 Uiso 1 1 calc R . .
H16B H 1.0821 0.0985 0.0322 0.151 Uiso 1 1 calc R . .
H16C H 1.0055 0.1627 0.0750 0.151 Uiso 1 1 calc R . .
C17 C 0.3751(2) 0.02481(11) 0.20075(17) 0.0449(4) Uani 1 1 d . . .
C18 C 0.2935(4) -0.00689(14) 0.2809(3) 0.0804(10) Uani 1 1 d . . .
H18A H 0.2048 -0.0294 0.2334 0.096 Uiso 1 1 calc R . .
H18B H 0.3548 -0.0440 0.3262 0.096 Uiso 1 1 calc R . .
C19 C 0.2504(5) 0.04221(17) 0.3626(3) 0.0959(11) Uani 1 1 d . . .
H19A H 0.3355 0.0535 0.4256 0.144 Uiso 1 1 calc R . .
H19B H 0.1774 0.0199 0.3926 0.144 Uiso 1 1 calc R . .
H19C H 0.2105 0.0850 0.3225 0.144 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni2 O5 2.0333(14) . ?
Ni2 O5 2.0333(14) 3_655 ?
Ni2 O1 2.0741(14) 3_655 ?
Ni2 O1 2.0741(14) . ?
Ni2 O2 2.1266(13) . ?
Ni2 O2 2.1266(13) 3_655 ?
Ni1 N1 1.9828(18) . ?
Ni1 O4 2.0148(14) . ?
Ni1 O1 2.0152(14) . ?
Ni1 O2 2.0820(14) . ?
Ni1 N2 2.1738(17) . ?
Ni1 O3 2.2526(16) . ?
O1 C1 1.306(2) . ?
O2 C14 1.282(2) . ?
O3 C14 1.234(2) . ?
O4 C17 1.251(2) . ?
O5 C17 1.248(2) . ?
N2 C10 1.470(4) . ?
N2 C13 1.478(3) . ?
N2 C9 1.479(3) . ?
N1 C7 1.269(3) . ?
N1 C8 1.468(3) . ?
C9 C8 1.489(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C7 C6 1.438(3) . ?
C7 H7 0.9300 . ?
C6 C5 1.410(3) . ?
C6 C1 1.422(3) . ?
C1 C2 1.408(3) . ?
C2 C3 1.374(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.368(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.358(4) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C10 C11 1.532(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.491(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.492(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.503(3) . ?
C15 C16 1.445(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.514(3) . ?
C18 C19 1.485(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 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
O5 Ni2 O5 180.0 . 3_655 ?
O5 Ni2 O1 89.21(5) . 3_655 ?
O5 Ni2 O1 90.79(5) 3_655 3_655 ?
O5 Ni2 O1 90.79(5) . . ?
O5 Ni2 O1 89.21(5) 3_655 . ?
O1 Ni2 O1 180.0 3_655 . ?
O5 Ni2 O2 89.57(6) . . ?
O5 Ni2 O2 90.43(6) 3_655 . ?
O1 Ni2 O2 100.46(5) 3_655 . ?
O1 Ni2 O2 79.54(5) . . ?
O5 Ni2 O2 90.43(6) . 3_655 ?
O5 Ni2 O2 89.57(6) 3_655 3_655 ?
O1 Ni2 O2 79.54(5) 3_655 3_655 ?
O1 Ni2 O2 100.46(5) . 3_655 ?
O2 Ni2 O2 180.0 . 3_655 ?
N1 Ni1 O4 100.37(7) . . ?
N1 Ni1 O1 90.86(7) . . ?
O4 Ni1 O1 90.40(6) . . ?
N1 Ni1 O2 159.85(6) . . ?
O4 Ni1 O2 98.49(6) . . ?
O1 Ni1 O2 81.96(5) . . ?
N1 Ni1 N2 83.49(8) . . ?
O4 Ni1 N2 92.08(7) . . ?
O1 Ni1 N2 174.16(6) . . ?
O2 Ni1 N2 102.89(7) . . ?
N1 Ni1 O3 101.66(7) . . ?
O4 Ni1 O3 157.81(6) . . ?
O1 Ni1 O3 91.86(6) . . ?
O2 Ni1 O3 60.05(5) . . ?
N2 Ni1 O3 87.85(7) . . ?
C1 O1 Ni1 128.48(13) . . ?
C1 O1 Ni2 134.91(13) . . ?
Ni1 O1 Ni2 96.58(6) . . ?
C14 O2 Ni1 93.47(11) . . ?
C14 O2 Ni2 120.01(12) . . ?
Ni1 O2 Ni2 93.00(6) . . ?
C14 O3 Ni1 86.95(12) . . ?
C17 O4 Ni1 124.95(13) . . ?
C17 O5 Ni2 130.79(13) . . ?
C10 N2 C13 102.5(2) . . ?
C10 N2 C9 110.3(2) . . ?
C13 N2 C9 112.3(2) . . ?
C10 N2 Ni1 117.42(15) . . ?
C13 N2 Ni1 113.75(15) . . ?
C9 N2 Ni1 100.97(14) . . ?
C7 N1 C8 120.90(19) . . ?
C7 N1 Ni1 126.37(15) . . ?
C8 N1 Ni1 112.62(16) . . ?
N2 C9 C8 110.4(2) . . ?
N2 C9 H9A 109.6 . . ?
C8 C9 H9A 109.6 . . ?
N2 C9 H9B 109.6 . . ?
C8 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
N1 C8 C9 109.08(19) . . ?
N1 C8 H8A 109.9 . . ?
C9 C8 H8A 109.9 . . ?
N1 C8 H8B 109.9 . . ?
C9 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
N1 C7 C6 127.23(19) . . ?
N1 C7 H7 116.4 . . ?
C6 C7 H7 116.4 . . ?
C5 C6 C1 118.6(2) . . ?
C5 C6 C7 116.9(2) . . ?
C1 C6 C7 124.49(19) . . ?
O1 C1 C2 120.20(19) . . ?
O1 C1 C6 122.51(19) . . ?
C2 C1 C6 117.29(19) . . ?
C3 C2 C1 120.9(2) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C4 C3 C2 122.1(3) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C5 C4 C3 118.3(2) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
C4 C5 C6 122.6(2) . . ?
C4 C5 H5 118.7 . . ?
C6 C5 H5 118.7 . . ?
N2 C10 C11 102.3(2) . . ?
N2 C10 H10A 111.3 . . ?
C11 C10 H10A 111.3 . . ?
N2 C10 H10B 111.3 . . ?
C11 C10 H10B 111.3 . . ?
H10A C10 H10B 109.2 . . ?
C12 C11 C10 103.9(3) . . ?
C12 C11 H11A 111.0 . . ?
C10 C11 H11A 111.0 . . ?
C12 C11 H11B 111.0 . . ?
C10 C11 H11B 111.0 . . ?
H11A C11 H11B 109.0 . . ?
C11 C12 C13 106.5(3) . . ?
C11 C12 H12A 110.4 . . ?
C13 C12 H12A 110.4 . . ?
C11 C12 H12B 110.4 . . ?
C13 C12 H12B 110.4 . . ?
H12A C12 H12B 108.6 . . ?
N2 C13 C12 104.9(3) . . ?
N2 C13 H13A 110.8 . . ?
C12 C13 H13A 110.8 . . ?
N2 C13 H13B 110.8 . . ?
C12 C13 H13B 110.8 . . ?
H13A C13 H13B 108.8 . . ?
O3 C14 O2 119.49(18) . . ?
O3 C14 C15 123.25(19) . . ?
O2 C14 C15 117.11(18) . . ?
C16 C15 C14 117.7(2) . . ?
C16 C15 H15A 107.9 . . ?
C14 C15 H15A 107.9 . . ?
C16 C15 H15B 107.9 . . ?
C14 C15 H15B 107.9 . . ?
H15A C15 H15B 107.2 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O5 C17 O4 126.76(18) . . ?
O5 C17 C18 116.01(19) . . ?
O4 C17 C18 117.23(19) . . ?
C19 C18 C17 117.2(2) . . ?
C19 C18 H18A 108.0 . . ?
C17 C18 H18A 108.0 . . ?
C19 C18 H18B 108.0 . . ?
C17 C18 H18B 108.0 . . ?
H18A C18 H18B 107.2 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        27.39
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.059
_database_code_depnum_ccdc_archive 'CCDC 986865'
#######################################################################
#
#                 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_added_by_encifer


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H57 N5 Ni3 O10'
_chemical_formula_weight         1136.20

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

_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                   13.709(3)
_cell_length_b                   14.024(3)
_cell_length_c                   16.630(4)
_cell_angle_alpha                111.754(3)
_cell_angle_beta                 95.086(4)
_cell_angle_gamma                111.703(3)
_cell_volume                     2663.2(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1686
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      18.07

_exptl_crystal_description       hexagonal
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1184
_exptl_absorpt_coefficient_mu    1.112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7608
_exptl_absorpt_correction_T_max  0.8082
_exptl_absorpt_process_details   SADABS

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19449
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_sigmaI/netI    0.1730
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         25.56
_reflns_number_total             9770
_reflns_number_gt                4066
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0800P)²+0.5000P] 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         9770
_refine_ls_number_parameters     629
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1943
_refine_ls_R_factor_gt           0.0849
_refine_ls_wR_factor_ref         0.2378
_refine_ls_wR_factor_gt          0.1932
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5745(11) 0.5792(11) -0.1466(11) 0.1184(17) Uani 1 1 d . . .
C2 C 0.4690(10) 0.5818(10) -0.1718(9) 0.1184(17) Uani 1 1 d . . .
H2 H 0.4173 0.5633 -0.1407 0.142 Uiso 1 1 calc R . .
C3 C 0.4436(9) 0.6115(10) -0.2416(7) 0.094(4) Uani 1 1 d . . .
H3 H 0.3786 0.6164 -0.2543 0.112 Uiso 1 1 calc R . .
C4 C 0.5199(11) 0.6327(12) -0.2898(7) 0.111(5) Uani 1 1 d . . .
H4 H 0.5049 0.6501 -0.3368 0.134 Uiso 1 1 calc R . .
C5 C 0.6118(10) 0.6287(9) -0.2707(7) 0.088(3) Uani 1 1 d . . .
H5 H 0.6612 0.6444 -0.3042 0.106 Uiso 1 1 calc R . .
C6 C 0.6383(9) 0.6023(8) -0.2034(7) 0.077(3) Uani 1 1 d . . .
C7 C 0.7484(9) 0.6074(9) -0.1835(7) 0.076(3) Uani 1 1 d . . .
H7 H 0.7869 0.6116 -0.2263 0.092 Uiso 1 1 calc R . .
C8 C 0.9081(10) 0.6285(12) -0.1027(9) 0.119(5) Uani 1 1 d . . .
H8A H 0.9533 0.7087 -0.0847 0.143 Uiso 1 1 calc R . .
H8B H 0.9203 0.5847 -0.1582 0.143 Uiso 1 1 calc R . .
C9 C 0.9376(11) 0.5967(15) -0.0336(11) 0.149(6) Uani 1 1 d . . .
H9A H 0.9091 0.5143 -0.0594 0.179 Uiso 1 1 calc R . .
H9B H 1.0162 0.6280 -0.0151 0.179 Uiso 1 1 calc R . .
C10 C 0.9686(11) 0.7553(12) 0.1059(11) 0.1184(17) Uani 1 1 d . . .
H10A H 1.0411 0.7787 0.0968 0.142 Uiso 1 1 calc R . .
H10B H 0.9378 0.8032 0.0958 0.142 Uiso 1 1 calc R . .
C11 C 0.9725(16) 0.7640(14) 0.1943(11) 0.192(8) Uani 1 1 d . . .
H11A H 0.9284 0.8009 0.2213 0.230 Uiso 1 1 calc R . .
H11B H 1.0467 0.8082 0.2317 0.230 Uiso 1 1 calc R . .
C12 C 0.9293(19) 0.6463(17) 0.1852(12) 0.235(12) Uani 1 1 d . . .
H12A H 0.9802 0.6398 0.2249 0.282 Uiso 1 1 calc R . .
H12B H 0.8609 0.6269 0.2019 0.282 Uiso 1 1 calc R . .
C13 C 0.9139(10) 0.5753(12) 0.1006(10) 0.124(5) Uani 1 1 d . . .
H13A H 0.8498 0.5042 0.0828 0.149 Uiso 1 1 calc R . .
H13B H 0.9763 0.5589 0.0937 0.149 Uiso 1 1 calc R . .
C14 C 0.6124(8) 0.3480(8) -0.0545(5) 0.053(2) Uani 1 1 d . . .
C15 C 0.6037(9) 0.2304(9) -0.0832(6) 0.062(3) Uani 1 1 d . . .
C16 C 0.6861(9) 0.2034(10) -0.1085(6) 0.078(3) Uani 1 1 d . . .
H16 H 0.7500 0.2593 -0.1078 0.093 Uiso 1 1 calc R . .
C17 C 0.6741(14) 0.0919(13) -0.1355(8) 0.113(5) Uani 1 1 d . . .
H17 H 0.7312 0.0745 -0.1503 0.136 Uiso 1 1 calc R . .
C18 C 0.5804(15) 0.0094(13) -0.1400(9) 0.126(6) Uani 1 1 d . . .
H18 H 0.5717 -0.0654 -0.1604 0.152 Uiso 1 1 calc R . .
C19 C 0.4993(14) 0.0356(11) -0.1150(9) 0.122(5) Uani 1 1 d . . .
H19 H 0.4347 -0.0218 -0.1183 0.146 Uiso 1 1 calc R . .
C20 C 0.5104(11) 0.1487(11) -0.0835(8) 0.099(4) Uani 1 1 d . . .
H20 H 0.4555 0.1668 -0.0636 0.118 Uiso 1 1 calc R . .
C21 C 0.6943(8) 0.7144(10) 0.1154(6) 0.065(3) Uani 1 1 d . . .
C22 C 0.6771(8) 0.7907(9) 0.2001(6) 0.066(3) Uani 1 1 d . . .
C23 C 0.7382(9) 0.9055(10) 0.2369(8) 0.093(4) Uani 1 1 d . . .
H23 H 0.7895 0.9377 0.2102 0.112 Uiso 1 1 calc R . .
C24 C 0.7229(10) 0.9733(10) 0.3144(10) 0.109(4) Uani 1 1 d . . .
H24 H 0.7672 1.0513 0.3421 0.131 Uiso 1 1 calc R . .
C25 C 0.6438(12) 0.9275(14) 0.3510(8) 0.112(5) Uani 1 1 d . . .
H25 H 0.6311 0.9748 0.4011 0.134 Uiso 1 1 calc R . .
C26 C 0.5836(9) 0.8132(11) 0.3147(7) 0.084(3) Uani 1 1 d . . .
H26 H 0.5315 0.7825 0.3415 0.101 Uiso 1 1 calc R . .
C27 C 0.5983(7) 0.7410(9) 0.2381(6) 0.063(3) Uani 1 1 d . . .
H27 H 0.5571 0.6624 0.2130 0.076 Uiso 1 1 calc R . .
C28 C -0.0768(7) 0.3235(8) 0.2973(6) 0.057(2) Uani 1 1 d . . .
C29 C -0.1253(7) 0.3849(9) 0.2711(6) 0.070(3) Uani 1 1 d . . .
H29 H -0.1197 0.4533 0.3142 0.083 Uiso 1 1 calc R . .
C30 C -0.1794(9) 0.3466(11) 0.1852(7) 0.093(4) Uani 1 1 d . . .
H30 H -0.2110 0.3884 0.1706 0.111 Uiso 1 1 calc R . .
C31 C -0.1887(11) 0.2461(14) 0.1185(8) 0.115(5) Uani 1 1 d . . .
H31 H -0.2275 0.2195 0.0598 0.138 Uiso 1 1 calc R . .
C32 C -0.1410(10) 0.1882(11) 0.1397(7) 0.107(4) Uani 1 1 d . . .
H32 H -0.1454 0.1222 0.0941 0.128 Uiso 1 1 calc R . .
C33 C -0.0848(8) 0.2217(9) 0.2269(6) 0.073(3) Uani 1 1 d . . .
C34 C -0.0375(10) 0.1525(9) 0.2405(8) 0.087(4) Uani 1 1 d . . .
H34 H -0.0452 0.0904 0.1891 0.105 Uiso 1 1 calc R . .
C35 C 0.0607(10) 0.0879(11) 0.3147(9) 0.1184(17) Uani 1 1 d . . .
H35A H 0.0708 0.0508 0.2560 0.142 Uiso 1 1 calc R . .
H35B H 0.0125 0.0295 0.3292 0.142 Uiso 1 1 calc R . .
C36 C 0.1715(10) 0.1579(11) 0.3859(9) 0.1184(17) Uani 1 1 d . . .
H36A H 0.2214 0.2139 0.3701 0.142 Uiso 1 1 calc R . .
H36B H 0.2035 0.1083 0.3904 0.142 Uiso 1 1 calc R . .
C37 C 0.2669(10) 0.2937(11) 0.5323(9) 0.1184(17) Uani 1 1 d . . .
H37A H 0.3033 0.3589 0.5202 0.142 Uiso 1 1 calc R . .
H37B H 0.3102 0.2519 0.5295 0.142 Uiso 1 1 calc R . .
C38 C 0.2221(11) 0.3254(12) 0.6263(10) 0.1184(17) Uani 1 1 d . . .
H38A H 0.2750 0.3432 0.6787 0.142 Uiso 1 1 calc R . .
H38B H 0.2008 0.3870 0.6378 0.142 Uiso 1 1 calc R . .
C39 C 0.1259(11) 0.2119(14) 0.5956(9) 0.148(6) Uani 1 1 d . . .
H39A H 0.0654 0.2258 0.6141 0.177 Uiso 1 1 calc R . .
H39B H 0.1435 0.1721 0.6273 0.177 Uiso 1 1 calc R . .
C40 C 0.0863(11) 0.1300(12) 0.4927(10) 0.1184(17) Uani 1 1 d . . .
H40A H 0.1091 0.0691 0.4764 0.142 Uiso 1 1 calc R . .
H40B H 0.0088 0.1002 0.4676 0.142 Uiso 1 1 calc R . .
C41 C 0.2118(7) 0.4918(8) 0.4835(6) 0.049(2) Uani 1 1 d . . .
C42 C 0.3042(7) 0.6093(8) 0.5201(6) 0.055(2) Uani 1 1 d . . .
C43 C 0.3880(8) 0.6307(10) 0.4800(7) 0.078(3) Uani 1 1 d . . .
H43 H 0.3887 0.5722 0.4301 0.093 Uiso 1 1 calc R . .
C44 C 0.4701(9) 0.7381(12) 0.5136(9) 0.097(4) Uani 1 1 d . . .
H44 H 0.5256 0.7537 0.4853 0.116 Uiso 1 1 calc R . .
C45 C 0.4705(9) 0.8230(11) 0.5893(9) 0.104(4) Uani 1 1 d . . .
H45 H 0.5291 0.8948 0.6142 0.124 Uiso 1 1 calc R . .
C46 C 0.3882(9) 0.8042(9) 0.6278(7) 0.083(3) Uani 1 1 d . . .
H46 H 0.3870 0.8634 0.6769 0.100 Uiso 1 1 calc R . .
C47 C 0.3050(7) 0.6954(9) 0.5935(7) 0.064(3) Uani 1 1 d . . .
H47 H 0.2487 0.6809 0.6211 0.077 Uiso 1 1 calc R . .
C48 C -0.0949(7) 0.3024(8) 0.5425(5) 0.048(2) Uani 1 1 d . . .
C49 C -0.1696(6) 0.2516(8) 0.5910(5) 0.049(2) Uani 1 1 d . . .
C50 C -0.2089(8) 0.3162(9) 0.6514(6) 0.070(3) Uani 1 1 d . . .
H50 H -0.1876 0.3922 0.6629 0.084 Uiso 1 1 calc R . .
C51 C -0.2801(9) 0.2689(11) 0.6951(7) 0.083(3) Uani 1 1 d . . .
H51 H -0.3041 0.3133 0.7377 0.100 Uiso 1 1 calc R . .
C52 C -0.3147(9) 0.1548(12) 0.6743(7) 0.094(4) Uani 1 1 d . . .
H52 H -0.3668 0.1208 0.6996 0.113 Uiso 1 1 calc R . .
C53 C -0.2734(9) 0.0917(10) 0.6173(8) 0.088(3) Uani 1 1 d . . .
H53 H -0.2934 0.0164 0.6075 0.106 Uiso 1 1 calc R . .
C54 C -0.2015(7) 0.1385(8) 0.5735(6) 0.067(3) Uani 1 1 d . . .
H54 H -0.1753 0.0944 0.5330 0.080 Uiso 1 1 calc R . .
C55 C 0.2866(16) 0.1182(13) 0.0476(10) 0.163(7) Uani 1 1 d . . .
H55A H 0.2644 0.1239 -0.0062 0.245 Uiso 1 1 calc R . .
H55B H 0.3206 0.0674 0.0352 0.245 Uiso 1 1 calc R . .
H55C H 0.3373 0.1923 0.0928 0.245 Uiso 1 1 calc R . .
C56 C 0.194(2) 0.0752(19) 0.0787(15) 0.179(9) Uani 1 1 d . . .
N1 N 0.7948(7) 0.6068(7) -0.1166(6) 0.073(2) Uani 1 1 d . . .
N2 N 0.8993(7) 0.6340(8) 0.0446(6) 0.087(3) Uani 1 1 d . . .
N3 N 0.0142(7) 0.1639(7) 0.3137(6) 0.073(2) Uani 1 1 d . . .
N4 N 0.1478(7) 0.2182(7) 0.4766(6) 0.083(3) Uani 1 1 d . . .
N5 N 0.125(2) 0.041(2) 0.1029(18) 0.292(14) Uani 1 1 d . . .
Ni1 Ni 0.73334(9) 0.58913(10) -0.01603(8) 0.0622(4) Uani 1 1 d . . .
Ni2 Ni 0.5000 0.5000 0.0000 0.0485(4) Uani 1 2 d S . .
Ni3 Ni 0.05895(9) 0.29846(9) 0.43211(7) 0.0527(4) Uani 1 1 d . . .
Ni4 Ni 0.0000 0.5000 0.5000 0.0446(4) Uani 1 2 d S . .
O1 O 0.5866(4) 0.5489(5) -0.0880(4) 0.0659(17) Uani 1 1 d . . .
O2 O 0.6561(5) 0.6067(5) 0.0921(4) 0.0597(16) Uani 1 1 d . . .
O3 O 0.7503(5) 0.7578(5) 0.0723(4) 0.0768(19) Uani 1 1 d . . .
O4 O 0.7014(5) 0.4236(5) -0.0550(4) 0.0673(17) Uani 1 1 d . . .
O5 O 0.4658(5) 0.6340(5) 0.0327(4) 0.0585(16) Uani 1 1 d . . .
O6 O -0.0296(4) 0.3597(4) 0.3822(3) 0.0514(15) Uani 1 1 d . . .
O7 O 0.1407(4) 0.4740(4) 0.5286(3) 0.0500(14) Uani 1 1 d . . .
O8 O 0.2063(5) 0.4120(5) 0.4149(4) 0.0665(17) Uani 1 1 d . . .
O9 O -0.0567(4) 0.2408(5) 0.4921(4) 0.0547(15) Uani 1 1 d . . .
O10 O -0.0751(4) 0.4028(5) 0.5574(3) 0.0509(14) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.221(13) . ?
C1 C6 1.388(15) . ?
C1 C2 1.487(16) . ?
C2 C3 1.428(14) . ?
C2 H2 0.9300 . ?
C3 C4 1.385(13) . ?
C3 H3 0.9300 . ?
C4 C5 1.298(14) . ?
C4 H4 0.9300 . ?
C5 C6 1.362(13) . ?
C5 H5 0.9300 . ?
C6 C7 1.486(14) . ?
C7 N1 1.236(11) . ?
C7 H7 0.9300 . ?
C8 N1 1.448(12) . ?
C8 C9 1.453(15) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.435(14) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.424(17) . ?
C10 N2 1.477(15) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.475(19) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.330(18) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.498(14) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 O5 1.242(9) 2_665 ?
C14 O4 1.290(10) . ?
C14 C15 1.491(12) . ?
C15 C20 1.363(13) . ?
C15 C16 1.372(12) . ?
C16 C17 1.396(15) . ?
C16 H16 0.9300 . ?
C17 C18 1.347(17) . ?
C17 H17 0.9300 . ?
C18 C19 1.348(17) . ?
C18 H18 0.9300 . ?
C19 C20 1.416(15) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 O3 1.244(10) . ?
C21 O2 1.285(11) . ?
C21 C22 1.521(13) . ?
C22 C23 1.360(13) . ?
C22 C27 1.393(11) . ?
C23 C24 1.378(14) . ?
C23 H23 0.9300 . ?
C24 C25 1.360(16) . ?
C24 H24 0.9300 . ?
C25 C26 1.353(15) . ?
C25 H25 0.9300 . ?
C26 C27 1.390(13) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 O6 1.316(9) . ?
C28 C29 1.424(12) . ?
C28 C33 1.429(12) . ?
C29 C30 1.352(12) . ?
C29 H29 0.9300 . ?
C30 C31 1.384(16) . ?
C30 H30 0.9300 . ?
C31 C32 1.333(17) . ?
C31 H31 0.9300 . ?
C32 C33 1.395(14) . ?
C32 H32 0.9300 . ?
C33 C34 1.421(15) . ?
C34 N3 1.275(13) . ?
C34 H34 0.9300 . ?
C35 N3 1.434(13) . ?
C35 C36 1.547(16) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 N4 1.562(14) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 N4 1.540(14) . ?
C37 C38 1.696(16) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.503(17) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.569(17) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 N4 1.352(13) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 O8 1.239(9) . ?
C41 O7 1.290(9) . ?
C41 C42 1.506(11) . ?
C42 C47 1.358(12) . ?
C42 C43 1.372(11) . ?
C43 C44 1.363(13) . ?
C43 H43 0.9300 . ?
C44 C45 1.374(15) . ?
C44 H44 0.9300 . ?
C45 C46 1.336(13) . ?
C45 H45 0.9300 . ?
C46 C47 1.381(12) . ?
C46 H46 0.9300 . ?
C47 H47 0.9300 . ?
C48 O10 1.251(9) . ?
C48 O9 1.265(9) . ?
C48 C49 1.496(11) . ?
C49 C50 1.380(11) . ?
C49 C54 1.382(11) . ?
C50 C51 1.388(12) . ?
C50 H50 0.9300 . ?
C51 C52 1.379(14) . ?
C51 H51 0.9300 . ?
C52 C53 1.358(14) . ?
C52 H52 0.9300 . ?
C53 C54 1.392(12) . ?
C53 H53 0.9300 . ?
C54 H54 0.9300 . ?
C55 C56 1.43(2) . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 N5 1.08(2) . ?
N1 Ni1 1.992(8) . ?
N2 Ni1 2.157(9) . ?
N3 Ni3 1.998(8) . ?
N4 Ni3 2.184(8) . ?
Ni1 O1 2.007(6) . ?
Ni1 O4 2.020(6) . ?
Ni1 O2 2.148(6) . ?
Ni1 O3 2.183(6) . ?
Ni2 O5 1.997(6) . ?
Ni2 O5 1.997(6) 2_665 ?
Ni2 O1 2.114(6) . ?
Ni2 O1 2.114(6) 2_665 ?
Ni2 O2 2.125(6) 2_665 ?
Ni2 O2 2.125(6) . ?
Ni3 O6 2.005(5) . ?
Ni3 O9 2.024(5) . ?
Ni3 O7 2.146(5) . ?
Ni3 O8 2.182(6) . ?
Ni4 O10 1.983(5) . ?
Ni4 O10 1.983(5) 2_566 ?
Ni4 O6 2.071(5) . ?
Ni4 O6 2.071(5) 2_566 ?
Ni4 O7 2.136(5) 2_566 ?
O5 C14 1.242(9) 2_665 ?

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 C1 C6 131.6(13) . . ?
O1 C1 C2 117.6(12) . . ?
C6 C1 C2 110.5(12) . . ?
C3 C2 C1 122.8(12) . . ?
C3 C2 H2 118.6 . . ?
C1 C2 H2 118.6 . . ?
C4 C3 C2 117.1(10) . . ?
C4 C3 H3 121.4 . . ?
C2 C3 H3 121.4 . . ?
C5 C4 C3 121.5(10) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
C4 C5 C6 122.2(11) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C5 C6 C1 125.7(12) . . ?
C5 C6 C7 117.8(10) . . ?
C1 C6 C7 116.2(11) . . ?
N1 C7 C6 127.6(9) . . ?
N1 C7 H7 116.2 . . ?
C6 C7 H7 116.2 . . ?
N1 C8 C9 109.7(9) . . ?
N1 C8 H8A 109.7 . . ?
C9 C8 H8A 109.7 . . ?
N1 C8 H8B 109.7 . . ?
C9 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
N2 C9 C8 115.1(12) . . ?
N2 C9 H9A 108.5 . . ?
C8 C9 H9A 108.5 . . ?
N2 C9 H9B 108.5 . . ?
C8 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C11 C10 N2 106.0(11) . . ?
C11 C10 H10A 110.5 . . ?
N2 C10 H10A 110.5 . . ?
C11 C10 H10B 110.5 . . ?
N2 C10 H10B 110.5 . . ?
H10A C10 H10B 108.7 . . ?
C10 C11 C12 106.2(14) . . ?
C10 C11 H11A 110.5 . . ?
C12 C11 H11A 110.5 . . ?
C10 C11 H11B 110.5 . . ?
C12 C11 H11B 110.5 . . ?
H11A C11 H11B 108.7 . . ?
C13 C12 C11 109.1(17) . . ?
C13 C12 H12A 109.9 . . ?
C11 C12 H12A 109.9 . . ?
C13 C12 H12B 109.9 . . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
C12 C13 N2 106.6(14) . . ?
C12 C13 H13A 110.4 . . ?
N2 C13 H13A 110.4 . . ?
C12 C13 H13B 110.4 . . ?
N2 C13 H13B 110.4 . . ?
H13A C13 H13B 108.6 . . ?
O5 C14 O4 124.9(9) 2_665 . ?
O5 C14 C15 118.3(9) 2_665 . ?
O4 C14 C15 116.8(9) . . ?
C20 C15 C16 120.0(11) . . ?
C20 C15 C14 118.0(10) . . ?
C16 C15 C14 122.0(10) . . ?
C15 C16 C17 120.0(12) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C18 C17 C16 120.5(15) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C17 C18 C19 119.7(15) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C18 C19 C20 121.3(15) . . ?
C18 C19 H19 119.4 . . ?
C20 C19 H19 119.4 . . ?
C15 C20 C19 118.4(12) . . ?
C15 C20 H20 120.8 . . ?
C19 C20 H20 120.8 . . ?
O3 C21 O2 120.8(9) . . ?
O3 C21 C22 119.6(10) . . ?
O2 C21 C22 119.5(9) . . ?
C23 C22 C27 121.4(10) . . ?
C23 C22 C21 119.6(10) . . ?
C27 C22 C21 119.0(10) . . ?
C22 C23 C24 118.9(11) . . ?
C22 C23 H23 120.6 . . ?
C24 C23 H23 120.6 . . ?
C25 C24 C23 120.9(12) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C26 C25 C24 120.1(12) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C25 C26 C27 121.1(11) . . ?
C25 C26 H26 119.5 . . ?
C27 C26 H26 119.5 . . ?
C26 C27 C22 117.5(10) . . ?
C26 C27 H27 121.2 . . ?
C22 C27 H27 121.2 . . ?
O6 C28 C29 120.5(8) . . ?
O6 C28 C33 123.5(9) . . ?
C29 C28 C33 116.0(9) . . ?
C30 C29 C28 121.8(10) . . ?
C30 C29 H29 119.1 . . ?
C28 C29 H29 119.1 . . ?
C29 C30 C31 121.2(12) . . ?
C29 C30 H30 119.4 . . ?
C31 C30 H30 119.4 . . ?
C32 C31 C30 118.9(12) . . ?
C32 C31 H31 120.6 . . ?
C30 C31 H31 120.6 . . ?
C31 C32 C33 123.2(13) . . ?
C31 C32 H32 118.4 . . ?
C33 C32 H32 118.4 . . ?
C32 C33 C34 117.7(11) . . ?
C32 C33 C28 118.9(11) . . ?
C34 C33 C28 123.4(9) . . ?
N3 C34 C33 128.9(10) . . ?
N3 C34 H34 115.6 . . ?
C33 C34 H34 115.6 . . ?
N3 C35 C36 108.4(11) . . ?
N3 C35 H35A 110.0 . . ?
C36 C35 H35A 110.0 . . ?
N3 C35 H35B 110.0 . . ?
C36 C35 H35B 110.0 . . ?
H35A C35 H35B 108.4 . . ?
C35 C36 N4 106.3(9) . . ?
C35 C36 H36A 110.5 . . ?
N4 C36 H36A 110.5 . . ?
C35 C36 H36B 110.5 . . ?
N4 C36 H36B 110.5 . . ?
H36A C36 H36B 108.7 . . ?
N4 C37 C38 88.8(9) . . ?
N4 C37 H37A 113.8 . . ?
C38 C37 H37A 113.8 . . ?
N4 C37 H37B 113.8 . . ?
C38 C37 H37B 113.8 . . ?
H37A C37 H37B 111.1 . . ?
C39 C38 C37 97.2(11) . . ?
C39 C38 H38A 112.3 . . ?
C37 C38 H38A 112.3 . . ?
C39 C38 H38B 112.3 . . ?
C37 C38 H38B 112.3 . . ?
H38A C38 H38B 109.9 . . ?
C38 C39 C40 117.4(13) . . ?
C38 C39 H39A 107.9 . . ?
C40 C39 H39A 107.9 . . ?
C38 C39 H39B 107.9 . . ?
C40 C39 H39B 107.9 . . ?
H39A C39 H39B 107.2 . . ?
N4 C40 C39 89.2(11) . . ?
N4 C40 H40A 113.8 . . ?
C39 C40 H40A 113.8 . . ?
N4 C40 H40B 113.8 . . ?
C39 C40 H40B 113.8 . . ?
H40A C40 H40B 111.0 . . ?
O8 C41 O7 120.1(8) . . ?
O8 C41 C42 121.8(8) . . ?
O7 C41 C42 118.0(8) . . ?
C47 C42 C43 119.4(9) . . ?
C47 C42 C41 119.9(8) . . ?
C43 C42 C41 120.7(9) . . ?
C44 C43 C42 119.8(11) . . ?
C44 C43 H43 120.1 . . ?
C42 C43 H43 120.1 . . ?
C43 C44 C45 119.7(10) . . ?
C43 C44 H44 120.1 . . ?
C45 C44 H44 120.1 . . ?
C46 C45 C44 121.2(11) . . ?
C46 C45 H45 119.4 . . ?
C44 C45 H45 119.4 . . ?
C45 C46 C47 118.8(11) . . ?
C45 C46 H46 120.6 . . ?
C47 C46 H46 120.6 . . ?
C42 C47 C46 121.0(9) . . ?
C42 C47 H47 119.5 . . ?
C46 C47 H47 119.5 . . ?
O10 C48 O9 126.6(8) . . ?
O10 C48 C49 116.3(8) . . ?
O9 C48 C49 117.1(8) . . ?
C50 C49 C54 119.9(8) . . ?
C50 C49 C48 120.2(8) . . ?
C54 C49 C48 119.8(8) . . ?
C49 C50 C51 120.5(10) . . ?
C49 C50 H50 119.7 . . ?
C51 C50 H50 119.7 . . ?
C52 C51 C50 118.9(10) . . ?
C52 C51 H51 120.5 . . ?
C50 C51 H51 120.5 . . ?
C53 C52 C51 120.7(10) . . ?
C53 C52 H52 119.6 . . ?
C51 C52 H52 119.6 . . ?
C52 C53 C54 120.6(11) . . ?
C52 C53 H53 119.7 . . ?
C54 C53 H53 119.7 . . ?
C49 C54 C53 119.1(9) . . ?
C49 C54 H54 120.4 . . ?
C53 C54 H54 120.4 . . ?
C56 C55 H55A 109.5 . . ?
C56 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C56 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
N5 C56 C55 178(3) . . ?
C7 N1 C8 119.7(9) . . ?
C7 N1 Ni1 126.9(7) . . ?
C8 N1 Ni1 113.3(7) . . ?
C9 N2 C10 111.7(11) . . ?
C9 N2 C13 109.4(11) . . ?
C10 N2 C13 102.2(9) . . ?
C9 N2 Ni1 100.9(7) . . ?
C10 N2 Ni1 117.0(8) . . ?
C13 N2 Ni1 115.8(7) . . ?
C34 N3 C35 121.4(11) . . ?
C34 N3 Ni3 124.5(8) . . ?
C35 N3 Ni3 113.4(8) . . ?
C40 N4 C37 119.1(10) . . ?
C40 N4 C36 103.0(10) . . ?
C37 N4 C36 97.3(8) . . ?
C40 N4 Ni3 115.0(7) . . ?
C37 N4 Ni3 117.9(6) . . ?
C36 N4 Ni3 98.3(6) . . ?
N1 Ni1 O1 88.9(3) . . ?
N1 Ni1 O4 97.0(3) . . ?
O1 Ni1 O4 92.5(2) . . ?
N1 Ni1 O2 164.3(3) . . ?
O1 Ni1 O2 83.4(2) . . ?
O4 Ni1 O2 97.0(2) . . ?
N1 Ni1 N2 82.8(4) . . ?
O1 Ni1 N2 171.6(3) . . ?
O4 Ni1 N2 88.3(3) . . ?
O2 Ni1 N2 104.8(3) . . ?
N1 Ni1 O3 105.7(3) . . ?
O1 Ni1 O3 91.4(2) . . ?
O4 Ni1 O3 157.0(2) . . ?
O2 Ni1 O3 61.0(2) . . ?
N2 Ni1 O3 91.1(3) . . ?
O5 Ni2 O5 179.998(1) . 2_665 ?
O5 Ni2 O1 90.1(2) . . ?
O5 Ni2 O1 89.9(2) 2_665 . ?
O5 Ni2 O1 89.9(2) . 2_665 ?
O5 Ni2 O1 90.1(2) 2_665 2_665 ?
O1 Ni2 O1 179.999(1) . 2_665 ?
O5 Ni2 O2 90.1(2) . 2_665 ?
O5 Ni2 O2 89.9(2) 2_665 2_665 ?
O1 Ni2 O2 98.5(2) . 2_665 ?
O1 Ni2 O2 81.5(2) 2_665 2_665 ?
O5 Ni2 O2 89.9(2) . . ?
O5 Ni2 O2 90.1(2) 2_665 . ?
O1 Ni2 O2 81.5(2) . . ?
O1 Ni2 O2 98.5(2) 2_665 . ?
O2 Ni2 O2 179.998(1) 2_665 . ?
N3 Ni3 O6 91.5(3) . . ?
N3 Ni3 O9 102.4(3) . . ?
O6 Ni3 O9 90.5(2) . . ?
N3 Ni3 O7 157.2(3) . . ?
O6 Ni3 O7 81.0(2) . . ?
O9 Ni3 O7 99.2(2) . . ?
N3 Ni3 O8 98.1(3) . . ?
O6 Ni3 O8 91.0(2) . . ?
O9 Ni3 O8 159.4(2) . . ?
O7 Ni3 O8 60.8(2) . . ?
N3 Ni3 N4 83.9(4) . . ?
O6 Ni3 N4 175.2(3) . . ?
O9 Ni3 N4 89.3(3) . . ?
O7 Ni3 N4 103.8(3) . . ?
O8 Ni3 N4 90.9(3) . . ?
O10 Ni4 O10 179.999(1) . 2_566 ?
O10 Ni4 O6 92.3(2) . . ?
O10 Ni4 O6 87.7(2) 2_566 . ?
O10 Ni4 O6 87.7(2) . 2_566 ?
O10 Ni4 O6 92.3(2) 2_566 2_566 ?
O6 Ni4 O6 179.999(1) . 2_566 ?
O10 Ni4 O7 90.6(2) . 2_566 ?
O10 Ni4 O7 89.4(2) 2_566 2_566 ?
O6 Ni4 O7 100.2(2) . 2_566 ?
O6 Ni4 O7 79.8(2) 2_566 2_566 ?
C1 O1 Ni1 123.0(8) . . ?
C1 O1 Ni2 138.6(8) . . ?
Ni1 O1 Ni2 95.5(3) . . ?
C21 O2 Ni2 117.8(5) . . ?
C21 O2 Ni1 89.4(5) . . ?
Ni2 O2 Ni1 91.1(2) . . ?
C21 O3 Ni1 88.9(6) . . ?
C14 O4 Ni1 123.9(6) . . ?
C14 O5 Ni2 134.1(6) 2_665 . ?
C28 O6 Ni3 127.1(5) . . ?
C28 O6 Ni4 134.8(5) . . ?
Ni3 O6 Ni4 97.6(2) . . ?
C41 O7 Ni3 89.6(5) . . ?
C41 O8 Ni3 89.4(5) . . ?
C48 O9 Ni3 123.5(5) . . ?
C48 O10 Ni4 132.1(5) . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        25.56
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         1.774
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.106
_database_code_depnum_ccdc_archive 'CCDC 986866'
#######################################################################
#
#                 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_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H56 N6 Ni3 O10'
_chemical_formula_weight         957.04

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                   9.2422(16)
_cell_length_b                   11.427(2)
_cell_length_c                   11.940(2)
_cell_angle_alpha                71.389(7)
_cell_angle_beta                 86.472(7)
_cell_angle_gamma                68.480(6)
_cell_volume                     1109.5(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2661
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      24.91

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             502
_exptl_absorpt_coefficient_mu    1.320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7423
_exptl_absorpt_correction_T_max  0.7970
_exptl_absorpt_process_details   'SADABS (Sheldrick 2008)'

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12958
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_av_sigmaI/netI    0.0770
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         26.50
_reflns_number_total             4552
_reflns_number_gt                3038
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)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       ?
_refine_ls_number_reflns         4552
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.1337
_refine_ls_wR_factor_gt          0.1098
_refine_ls_goodness_of_fit_ref   0.833
_refine_ls_restrained_S_all      0.833
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2425(4) 0.7525(3) 0.8312(3) 0.0440(8) Uani 1 1 d . . .
C2 C 0.2441(5) 0.8318(3) 0.9000(4) 0.0572(10) Uani 1 1 d . . .
H2 H 0.3152 0.7955 0.9651 0.069 Uiso 1 1 calc R . .
C3 C 0.1441(6) 0.9605(4) 0.8737(4) 0.0754(13) Uani 1 1 d . . .
H3 H 0.1466 1.0094 0.9221 0.090 Uiso 1 1 calc R . .
C4 C 0.0395(6) 1.0191(4) 0.7766(5) 0.0919(17) Uani 1 1 d . . .
H4 H -0.0272 1.1073 0.7585 0.110 Uiso 1 1 calc R . .
C5 C 0.0355(6) 0.9452(4) 0.7074(5) 0.0787(13) Uani 1 1 d . . .
H5 H -0.0355 0.9845 0.6420 0.094 Uiso 1 1 calc R . .
C6 C 0.1336(4) 0.8138(3) 0.7314(3) 0.0519(9) Uani 1 1 d . . .
C7 C 0.1182(5) 0.7487(4) 0.6491(3) 0.0571(9) Uani 1 1 d . . .
H7 H 0.0451 0.7999 0.5855 0.069 Uiso 1 1 calc R . .
C8 C 0.1701(6) 0.5771(4) 0.5615(4) 0.0747(13) Uani 1 1 d . . .
H8A H 0.0669 0.6288 0.5226 0.090 Uiso 1 1 calc R . .
H8B H 0.2464 0.5833 0.5026 0.090 Uiso 1 1 calc R . .
C9 C 0.1868(6) 0.4384(5) 0.6180(5) 0.0822(15) Uani 1 1 d . . .
H9A H 0.1775 0.4016 0.5572 0.099 Uiso 1 1 calc R . .
H9B H 0.1020 0.4354 0.6695 0.099 Uiso 1 1 calc R . .
C10 C 0.3159(6) 0.2310(5) 0.7673(4) 0.0776(14) Uani 1 1 d . . .
H10A H 0.2828 0.1895 0.7197 0.093 Uiso 1 1 calc R . .
H10B H 0.2352 0.2540 0.8209 0.093 Uiso 1 1 calc R . .
C11 C 0.4651(8) 0.1348(5) 0.8375(5) 0.0968(18) Uani 1 1 d . . .
H11A H 0.4961 0.1754 0.8871 0.116 Uiso 1 1 calc R . .
H11B H 0.4483 0.0565 0.8888 0.116 Uiso 1 1 calc R . .
C12 C 0.5927(7) 0.0948(5) 0.7584(6) 0.1041(19) Uani 1 1 d . . .
H12A H 0.5681 0.0445 0.7156 0.125 Uiso 1 1 calc R . .
H12B H 0.6896 0.0388 0.8056 0.125 Uiso 1 1 calc R . .
C13 C 0.6113(6) 0.2168(4) 0.6718(5) 0.0804(14) Uani 1 1 d . . .
H13A H 0.6547 0.2572 0.7142 0.096 Uiso 1 1 calc R . .
H13B H 0.6845 0.1905 0.6145 0.096 Uiso 1 1 calc R . .
C14 C 0.4623(5) 0.3161(4) 0.6082(4) 0.0647(11) Uani 1 1 d . . .
H14A H 0.4278 0.2803 0.5560 0.078 Uiso 1 1 calc R . .
H14B H 0.4801 0.3950 0.5595 0.078 Uiso 1 1 calc R . .
C15 C 0.6404(4) 0.4480(3) 0.7816(3) 0.0431(8) Uani 1 1 d . . .
C16 C 0.8122(5) 0.4165(5) 0.7889(4) 0.0724(12) Uani 1 1 d . . .
H16A H 0.8626 0.3595 0.7427 0.109 Uiso 1 1 calc R . .
H16B H 0.8519 0.3725 0.8700 0.109 Uiso 1 1 calc R . .
H16C H 0.8324 0.4972 0.7589 0.109 Uiso 1 1 calc R . .
C17 C 0.7480(4) 0.6159(3) 0.9895(3) 0.0446(8) Uani 1 1 d . . .
C18 C 0.8484(5) 0.6843(4) 0.9128(4) 0.0645(11) Uani 1 1 d . . .
H18A H 0.8116 0.7143 0.8313 0.097 Uiso 1 1 calc R . .
H18B H 0.9544 0.6232 0.9226 0.097 Uiso 1 1 calc R . .
H18C H 0.8430 0.7590 0.9357 0.097 Uiso 1 1 calc R . .
C19 C 0.3634(6) 0.1591(5) 0.4023(4) 0.0733(12) Uani 1 1 d . . .
C20 C 0.4988(5) 0.1706(4) 0.3417(4) 0.0716(12) Uani 1 1 d . . .
H20A H 0.5278 0.2346 0.3611 0.107 Uiso 1 1 calc R . .
H20B H 0.4761 0.1988 0.2578 0.107 Uiso 1 1 calc R . .
H20C H 0.5831 0.0860 0.3655 0.107 Uiso 1 1 calc R . .
N1 N 0.1947(4) 0.6282(3) 0.6550(3) 0.0542(8) Uani 1 1 d . . .
N2 N 0.3366(4) 0.3543(3) 0.6882(3) 0.0521(8) Uani 1 1 d . . .
N3 N 0.2595(6) 0.1505(6) 0.4513(5) 0.1250(19) Uani 1 1 d . . .
Ni1 Ni 0.35418(5) 0.49302(4) 0.77855(3) 0.03949(16) Uani 1 1 d . . .
Ni2 Ni 0.5000 0.5000 1.0000 0.03586(17) Uani 1 2 d S . .
O1 O 0.3415(3) 0.6295(2) 0.8579(2) 0.0447(5) Uani 1 1 d . . .
O2 O 0.5746(3) 0.4007(2) 0.87271(19) 0.0409(5) Uani 1 1 d . . .
O3 O 0.5608(3) 0.5156(2) 0.6865(2) 0.0542(6) Uani 1 1 d . . .
O4 O 0.2205(3) 0.4245(2) 0.9002(2) 0.0493(6) Uani 1 1 d . . .
O5 O 0.6414(3) 0.6048(2) 0.93854(19) 0.0451(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.312(4) . ?
C1 C2 1.408(5) . ?
C1 C6 1.423(5) . ?
C2 C3 1.363(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.376(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.367(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.385(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.450(5) . ?
C7 N1 1.276(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.463(6) . ?
C8 N1 1.477(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.482(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.497(5) . ?
C10 C11 1.501(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.495(8) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.508(7) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.481(6) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 N2 1.487(5) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 O3 1.246(4) . ?
C15 O2 1.277(4) . ?
C15 C16 1.496(5) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 O5 1.253(4) . ?
C17 O4 1.262(4) 2_667 ?
C17 C18 1.511(5) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 N3 1.113(6) . ?
C19 C20 1.433(6) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
N1 Ni1 1.969(3) . ?
N2 Ni1 2.237(3) . ?
Ni1 O4 2.003(2) . ?
Ni1 O1 2.034(2) . ?
Ni1 O2 2.115(2) . ?
Ni1 O3 2.201(2) . ?
Ni2 O5 2.037(2) . ?
Ni2 O5 2.038(2) 2_667 ?
Ni2 O1 2.080(2) . ?
Ni2 O1 2.080(2) 2_667 ?
Ni2 O2 2.115(2) . ?
Ni2 O2 2.115(2) 2_667 ?
O4 C17 1.262(4) 2_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
O1 C1 C2 120.3(3) . . ?
O1 C1 C6 122.9(3) . . ?
C2 C1 C6 116.8(3) . . ?
C3 C2 C1 121.7(4) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
C2 C3 C4 121.1(4) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C5 C4 C3 118.8(4) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
C4 C5 C6 122.2(4) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C5 C6 C1 119.4(4) . . ?
C5 C6 C7 116.1(4) . . ?
C1 C6 C7 124.5(3) . . ?
N1 C7 C6 126.6(4) . . ?
N1 C7 H7 116.7 . . ?
C6 C7 H7 116.7 . . ?
C9 C8 N1 107.7(3) . . ?
C9 C8 H8A 110.2 . . ?
N1 C8 H8A 110.2 . . ?
C9 C8 H8B 110.2 . . ?
N1 C8 H8B 110.2 . . ?
H8A C8 H8B 108.5 . . ?
C8 C9 N2 113.9(3) . . ?
C8 C9 H9A 108.8 . . ?
N2 C9 H9A 108.8 . . ?
C8 C9 H9B 108.8 . . ?
N2 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
N2 C10 C11 110.9(4) . . ?
N2 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.0 . . ?
C12 C11 C10 111.4(4) . . ?
C12 C11 H11A 109.3 . . ?
C10 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C11 C12 C13 109.8(4) . . ?
C11 C12 H12A 109.7 . . ?
C13 C12 H12A 109.7 . . ?
C11 C12 H12B 109.7 . . ?
C13 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
C14 C13 C12 112.8(4) . . ?
C14 C13 H13A 109.0 . . ?
C12 C13 H13A 109.0 . . ?
C14 C13 H13B 109.0 . . ?
C12 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
C13 C14 N2 113.6(4) . . ?
C13 C14 H14A 108.9 . . ?
N2 C14 H14A 108.9 . . ?
C13 C14 H14B 108.9 . . ?
N2 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
O3 C15 O2 119.2(3) . . ?
O3 C15 C16 121.1(4) . . ?
O2 C15 C16 119.7(4) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O5 C17 O4 126.0(3) . 2_667 ?
O5 C17 C18 117.5(3) . . ?
O4 C17 C18 116.4(3) 2_667 . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 C20 178.5(5) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C7 N1 C8 120.4(3) . . ?
C7 N1 Ni1 127.1(3) . . ?
C8 N1 Ni1 112.5(3) . . ?
C9 N2 C14 109.9(3) . . ?
C9 N2 C10 106.7(3) . . ?
C14 N2 C10 108.4(3) . . ?
C9 N2 Ni1 99.5(2) . . ?
C14 N2 Ni1 115.8(2) . . ?
C10 N2 Ni1 115.7(2) . . ?
N1 Ni1 O4 100.85(12) . . ?
N1 Ni1 O1 90.98(11) . . ?
O4 Ni1 O1 89.55(9) . . ?
N1 Ni1 O2 155.91(11) . . ?
O4 Ni1 O2 101.39(9) . . ?
O1 Ni1 O2 80.07(9) . . ?
N1 Ni1 O3 97.82(12) . . ?
O4 Ni1 O3 161.27(10) . . ?
O1 Ni1 O3 91.68(9) . . ?
O2 Ni1 O3 60.50(9) . . ?
N1 Ni1 N2 83.82(12) . . ?
O4 Ni1 N2 86.90(10) . . ?
O1 Ni1 N2 173.04(11) . . ?
O2 Ni1 N2 106.50(10) . . ?
O3 Ni1 N2 93.60(10) . . ?
O5 Ni2 O5 179.999(1) . 2_667 ?
O5 Ni2 O1 88.61(9) . . ?
O5 Ni2 O1 91.39(9) 2_667 . ?
O5 Ni2 O1 91.39(9) . 2_667 ?
O5 Ni2 O1 88.61(9) 2_667 2_667 ?
O1 Ni2 O1 179.999(1) . 2_667 ?
O5 Ni2 O2 90.72(8) . . ?
O5 Ni2 O2 89.28(8) 2_667 . ?
O1 Ni2 O2 79.05(9) . . ?
O1 Ni2 O2 100.95(9) 2_667 . ?
O5 Ni2 O2 89.28(8) . 2_667 ?
O5 Ni2 O2 90.72(8) 2_667 2_667 ?
O1 Ni2 O2 100.95(9) . 2_667 ?
O1 Ni2 O2 79.05(9) 2_667 2_667 ?
O2 Ni2 O2 180.00(12) . 2_667 ?
C1 O1 Ni1 127.6(2) . . ?
C1 O1 Ni2 134.8(2) . . ?
Ni1 O1 Ni2 96.79(9) . . ?
C15 O2 Ni1 91.7(2) . . ?
C15 O2 Ni2 120.53(17) . . ?
Ni1 O2 Ni2 93.33(9) . . ?
C15 O3 Ni1 88.6(2) . . ?
C17 O4 Ni1 124.3(2) 2_667 . ?
C17 O5 Ni2 131.5(2) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.072
_database_code_depnum_ccdc_archive 'CCDC 986867'
#######################################################################
#
#                 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_4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H58 N4 Ni3 O10'
_chemical_formula_weight         931.03

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                   9.721(2)
_cell_length_b                   18.581(4)
_cell_length_c                   12.238(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.402(8)
_cell_angle_gamma                90.00
_cell_volume                     2141.1(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9976
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      29.11

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             980
_exptl_absorpt_coefficient_mu    1.365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7354
_exptl_absorpt_correction_T_max  0.7720
_exptl_absorpt_process_details   'SADABS (Sheldrick 2008)'

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26726
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         27.00
_reflns_number_total             4635
_reflns_number_gt                3873
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)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       ?
_refine_ls_number_reflns         4635
_refine_ls_number_parameters     261
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0300
_refine_ls_wR_factor_ref         0.1186
_refine_ls_wR_factor_gt          0.1045
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_restrained_S_all      0.949
_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
Ni2 Ni 0.5000 1.0000 1.0000 0.03346(13) Uani 1 2 d S . .
Ni1 Ni 0.48548(3) 0.853802(12) 0.88554(2) 0.03494(12) Uani 1 1 d . . .
O2 O 0.65683(14) 1.06395(7) 1.10720(12) 0.0382(3) Uani 1 1 d . . .
O4 O 0.61447(16) 0.90534(7) 0.80573(12) 0.0437(4) Uani 1 1 d . . .
O5 O 0.40368(17) 0.98421(8) 1.12728(13) 0.0451(4) Uani 1 1 d . . .
N1 N 0.6043(2) 0.76621(9) 0.92058(16) 0.0433(4) Uani 1 1 d . . .
O1 O 0.59087(15) 0.89957(7) 1.03246(11) 0.0394(3) Uani 1 1 d . . .
N2 N 0.3770(2) 0.79337(9) 0.73236(16) 0.0470(4) Uani 1 1 d . . .
C10 C 0.4391(3) 0.80784(15) 0.6351(2) 0.0605(7) Uani 1 1 d . . .
H10A H 0.4138 0.7690 0.5809 0.073 Uiso 1 1 calc R . .
H10B H 0.5418 0.8090 0.6613 0.073 Uiso 1 1 calc R . .
C11 C 0.3876(3) 0.87849(18) 0.5776(2) 0.0749(8) Uani 1 1 d . . .
H11A H 0.4194 0.9178 0.6300 0.090 Uiso 1 1 calc R . .
H11B H 0.4288 0.8852 0.5138 0.090 Uiso 1 1 calc R . .
C12 C 0.2281(4) 0.8805(2) 0.5373(3) 0.0945(11) Uani 1 1 d . . .
H12A H 0.1957 0.8445 0.4792 0.113 Uiso 1 1 calc R . .
H12B H 0.1974 0.9274 0.5056 0.113 Uiso 1 1 calc R . .
C13 C 0.1665(3) 0.86560(18) 0.6368(3) 0.0795(9) Uani 1 1 d . . .
H13A H 0.1913 0.9046 0.6907 0.095 Uiso 1 1 calc R . .
H13B H 0.0638 0.8637 0.6113 0.095 Uiso 1 1 calc R . .
C14 C 0.2203(3) 0.79590(15) 0.6938(2) 0.0632(7) Uani 1 1 d . . .
H14A H 0.1803 0.7891 0.7582 0.076 Uiso 1 1 calc R . .
H14B H 0.1879 0.7565 0.6417 0.076 Uiso 1 1 calc R . .
C9 C 0.4132(3) 0.71905(12) 0.7729(2) 0.0625(7) Uani 1 1 d . . .
H9A H 0.3902 0.6863 0.7093 0.075 Uiso 1 1 calc R . .
H9B H 0.3562 0.7058 0.8245 0.075 Uiso 1 1 calc R . .
C8 C 0.5682(3) 0.71134(12) 0.8320(2) 0.0601(7) Uani 1 1 d . . .
H8A H 0.5864 0.6637 0.8649 0.072 Uiso 1 1 calc R . .
H8B H 0.6260 0.7177 0.7785 0.072 Uiso 1 1 calc R . .
C7 C 0.7037(2) 0.75534(11) 1.0073(2) 0.0481(5) Uani 1 1 d . . .
H7 H 0.7496 0.7111 1.0112 0.058 Uiso 1 1 calc R . .
C6 C 0.7545(2) 0.80335(12) 1.10099(19) 0.0449(5) Uani 1 1 d . . .
C1 C 0.6968(2) 0.87325(10) 1.11049(17) 0.0367(4) Uani 1 1 d . . .
C2 C 0.7582(3) 0.91325(12) 1.20757(19) 0.0492(5) Uani 1 1 d . . .
H2 H 0.7223 0.9586 1.2166 0.059 Uiso 1 1 calc R . .
C3 C 0.8699(3) 0.88702(15) 1.2894(2) 0.0692(8) Uani 1 1 d . . .
H3 H 0.9102 0.9156 1.3515 0.083 Uiso 1 1 calc R . .
C4 C 0.9237(3) 0.81891(16) 1.2813(3) 0.0798(9) Uani 1 1 d . . .
H4 H 0.9973 0.8008 1.3384 0.096 Uiso 1 1 calc R . .
C5 C 0.8664(3) 0.77911(14) 1.1882(3) 0.0661(7) Uani 1 1 d . . .
H5 H 0.9035 0.7336 1.1821 0.079 Uiso 1 1 calc R . .
O3 O 0.29667(17) 0.83076(8) 0.95366(14) 0.0480(4) Uani 1 1 d . . .
C15 C 0.2621(2) 0.89408(11) 0.93331(18) 0.0409(4) Uani 1 1 d . . .
C16 C 0.1236(3) 0.92512(14) 0.9455(3) 0.0637(7) Uani 1 1 d . . .
H16A H 0.1447 0.9633 1.0013 0.076 Uiso 1 1 calc R . .
H16B H 0.0757 0.9469 0.8741 0.076 Uiso 1 1 calc R . .
C17 C 0.0249(4) 0.87475(19) 0.9782(4) 0.1059(14) Uani 1 1 d . . .
H17A H 0.0166 0.8322 0.9326 0.159 Uiso 1 1 calc R . .
H17B H -0.0666 0.8970 0.9672 0.159 Uiso 1 1 calc R . .
H17C H 0.0600 0.8621 1.0562 0.159 Uiso 1 1 calc R . .
C18 C 0.3613(2) 1.02848(11) 1.18794(18) 0.0418(5) Uani 1 1 d . . .
C19 C 0.2698(4) 0.99894(14) 1.2623(3) 0.0745(9) Uani 1 1 d . . .
H19A H 0.1863 0.9768 1.2137 0.089 Uiso 1 1 calc R . .
H19B H 0.3229 0.9612 1.3093 0.089 Uiso 1 1 calc R . .
C20 C 0.2218(4) 1.05085(17) 1.3367(3) 0.0909(11) Uani 1 1 d . . .
H20A H 0.2987 1.0610 1.4010 0.136 Uiso 1 1 calc R . .
H20B H 0.1438 1.0306 1.3614 0.136 Uiso 1 1 calc R . .
H20C H 0.1918 1.0946 1.2959 0.136 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni2 O5 2.0285(15) . ?
Ni2 O5 2.0285(15) 3_677 ?
Ni2 O1 2.0605(13) . ?
Ni2 O1 2.0606(13) 3_677 ?
Ni2 O2 2.1124(14) 3_677 ?
Ni2 O2 2.1125(14) . ?
Ni1 N1 1.9801(18) . ?
Ni1 O4 2.0130(14) . ?
Ni1 O1 2.0223(14) . ?
Ni1 O2 2.0781(14) 3_677 ?
Ni1 N2 2.2143(18) . ?
Ni1 O3 2.2380(16) . ?
Ni1 C15 2.500(2) . ?
O2 C15 1.292(2) 3_677 ?
O2 Ni1 2.0781(14) 3_677 ?
O4 C18 1.251(2) 3_677 ?
O5 C18 1.245(3) . ?
N1 C7 1.261(3) . ?
N1 C8 1.466(3) . ?
O1 C1 1.312(2) . ?
N2 C14 1.480(3) . ?
N2 C9 1.480(3) . ?
N2 C10 1.486(3) . ?
C10 C11 1.515(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.506(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.511(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.502(4) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C9 C8 1.507(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C7 C6 1.440(3) . ?
C7 H7 0.9300 . ?
C6 C5 1.395(3) . ?
C6 C1 1.431(3) . ?
C1 C2 1.403(3) . ?
C2 C3 1.371(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.382(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.357(4) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
O3 C15 1.232(3) . ?
C15 O2 1.292(2) 3_677 ?
C15 C16 1.505(3) . ?
C16 C17 1.466(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 O4 1.251(2) 3_677 ?
C18 C19 1.525(3) . ?
C19 C20 1.479(4) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 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
O5 Ni2 O5 179.999(1) . 3_677 ?
O5 Ni2 O1 88.77(6) . . ?
O5 Ni2 O1 91.23(6) 3_677 . ?
O5 Ni2 O1 91.23(6) . 3_677 ?
O5 Ni2 O1 88.77(6) 3_677 3_677 ?
O1 Ni2 O1 179.999(1) . 3_677 ?
O5 Ni2 O2 89.76(6) . 3_677 ?
O5 Ni2 O2 90.24(6) 3_677 3_677 ?
O1 Ni2 O2 79.57(5) . 3_677 ?
O1 Ni2 O2 100.43(5) 3_677 3_677 ?
O5 Ni2 O2 90.24(6) . . ?
O5 Ni2 O2 89.76(6) 3_677 . ?
O1 Ni2 O2 100.43(5) . . ?
O1 Ni2 O2 79.57(5) 3_677 . ?
O2 Ni2 O2 180.00(6) 3_677 . ?
N1 Ni1 O4 95.50(7) . . ?
N1 Ni1 O1 90.79(7) . . ?
O4 Ni1 O1 89.57(6) . . ?
N1 Ni1 O2 162.54(7) . 3_677 ?
O4 Ni1 O2 99.94(6) . 3_677 ?
O1 Ni1 O2 81.26(6) . 3_677 ?
N1 Ni1 N2 84.02(8) . . ?
O4 Ni1 N2 93.05(7) . . ?
O1 Ni1 N2 174.39(6) . . ?
O2 Ni1 N2 103.14(7) 3_677 . ?
N1 Ni1 O3 104.50(7) . . ?
O4 Ni1 O3 159.93(6) . . ?
O1 Ni1 O3 91.73(6) . . ?
O2 Ni1 O3 60.55(5) 3_677 . ?
N2 Ni1 O3 87.51(7) . . ?
N1 Ni1 C15 133.57(7) . . ?
O4 Ni1 C15 130.78(6) . . ?
O1 Ni1 C15 86.77(6) . . ?
O2 Ni1 C15 31.08(6) 3_677 . ?
N2 Ni1 C15 95.24(7) . . ?
O3 Ni1 C15 29.48(6) . . ?
C15 O2 Ni1 92.79(12) 3_677 3_677 ?
C15 O2 Ni2 121.07(13) 3_677 . ?
Ni1 O2 Ni2 93.15(6) 3_677 . ?
C18 O4 Ni1 124.60(13) 3_677 . ?
C18 O5 Ni2 130.29(13) . . ?
C7 N1 C8 120.22(19) . . ?
C7 N1 Ni1 126.69(15) . . ?
C8 N1 Ni1 113.09(15) . . ?
C1 O1 Ni1 128.51(13) . . ?
C1 O1 Ni2 134.34(13) . . ?
Ni1 O1 Ni2 96.39(6) . . ?
C14 N2 C9 106.1(2) . . ?
C14 N2 C10 109.3(2) . . ?
C9 N2 C10 109.1(2) . . ?
C14 N2 Ni1 119.31(15) . . ?
C9 N2 Ni1 99.55(14) . . ?
C10 N2 Ni1 112.56(14) . . ?
N2 C10 C11 112.1(2) . . ?
N2 C10 H10A 109.2 . . ?
C11 C10 H10A 109.2 . . ?
N2 C10 H10B 109.2 . . ?
C11 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C12 C11 C10 111.6(3) . . ?
C12 C11 H11A 109.3 . . ?
C10 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C11 C12 C13 108.3(3) . . ?
C11 C12 H12A 110.0 . . ?
C13 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
C13 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
C14 C13 C12 111.8(3) . . ?
C14 C13 H13A 109.3 . . ?
C12 C13 H13A 109.3 . . ?
C14 C13 H13B 109.3 . . ?
C12 C13 H13B 109.3 . . ?
H13A C13 H13B 107.9 . . ?
N2 C14 C13 112.8(2) . . ?
N2 C14 H14A 109.0 . . ?
C13 C14 H14A 109.0 . . ?
N2 C14 H14B 109.0 . . ?
C13 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
N2 C9 C8 112.0(2) . . ?
N2 C9 H9A 109.2 . . ?
C8 C9 H9A 109.2 . . ?
N2 C9 H9B 109.2 . . ?
C8 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
N1 C8 C9 108.38(19) . . ?
N1 C8 H8A 110.0 . . ?
C9 C8 H8A 110.0 . . ?
N1 C8 H8B 110.0 . . ?
C9 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
N1 C7 C6 127.60(19) . . ?
N1 C7 H7 116.2 . . ?
C6 C7 H7 116.2 . . ?
C5 C6 C1 118.5(2) . . ?
C5 C6 C7 117.2(2) . . ?
C1 C6 C7 124.3(2) . . ?
O1 C1 C2 120.69(19) . . ?
O1 C1 C6 122.11(19) . . ?
C2 C1 C6 117.20(19) . . ?
C3 C2 C1 121.6(2) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
C2 C3 C4 121.2(3) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 118.4(2) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
C4 C5 C6 123.1(2) . . ?
C4 C5 H5 118.5 . . ?
C6 C5 H5 118.5 . . ?
C15 O3 Ni1 87.13(13) . . ?
O3 C15 O2 119.47(19) . 3_677 ?
O3 C15 C16 123.5(2) . . ?
O2 C15 C16 116.90(19) 3_677 . ?
O3 C15 Ni1 63.39(11) . . ?
O2 C15 Ni1 56.13(10) 3_677 . ?
C16 C15 Ni1 171.08(17) . . ?
C17 C16 C15 116.4(2) . . ?
C17 C16 H16A 108.2 . . ?
C15 C16 H16A 108.2 . . ?
C17 C16 H16B 108.2 . . ?
C15 C16 H16B 108.2 . . ?
H16A C16 H16B 107.3 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O5 C18 O4 126.99(19) . 3_677 ?
O5 C18 C19 116.55(19) . . ?
O4 C18 C19 116.46(19) 3_677 . ?
C20 C19 C18 116.9(2) . . ?
C20 C19 H19A 108.1 . . ?
C18 C19 H19A 108.1 . . ?
C20 C19 H19B 108.1 . . ?
C18 C19 H19B 108.1 . . ?
H19A C19 H19B 107.3 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.052
_database_code_depnum_ccdc_archive 'CCDC 986868'
#######################################################################
#
#                 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_added_by_encifer
_audit_creation_date             2014-05-29
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4844)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C56 H58 N4 Ni3 O10,C H2 Cl2'
_chemical_formula_sum            'C57 H60 Cl2 N4 Ni3 O10'
_chemical_formula_weight         1208.12
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 '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'
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C2/c '
_space_group_name_Hall           '-C 2yc'
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                   21.737(17)
_cell_length_b                   10.824(8)
_cell_length_c                   23.427(18)
_cell_angle_alpha                90
_cell_angle_beta                 103.020(9)
_cell_angle_gamma                90
_cell_volume                     5370(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6712
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      24.97
_shelx_estimated_absorpt_T_max   0.812
_shelx_estimated_absorpt_T_min   0.753
_exptl_absorpt_coefficient_mu    1.204
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7702
_exptl_absorpt_correction_T_max  0.8263
_exptl_absorpt_process_details   'SADABS (Sheldrick 2008)'

_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            19507
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.148
_diffrn_reflns_theta_min         1.784
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4191
_reflns_number_total             5239
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         5239
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0427
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0542P)²+9.1343P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1178
_refine_special_details          
;
 DCM molecule Cl(1)C(29)H₂Cl(2) is disordered equally between two 
positions related by crystallographic twofold axis, which were refined 
with 50% occupancies.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl2-C29 \\sim Cl1-C29
 with sigma of 0.01
3. Others
 Fixed Sof: C29(0.5) H29A(0.5) H29B(0.5) Cl1(0.5) Cl2(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C29(H29A,H29B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C17(H17), C18(H18), C19(H19),
 C20(H20), C21(H21), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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
C1 C 0.17949(16) 0.4978(3) 0.51022(13) 0.0398(7) Uani 1 1 d . . . . .
C2 C 0.12333(16) 0.4558(3) 0.47352(15) 0.0480(8) Uani 1 1 d . . . . .
H2 H 0.1235 0.3825 0.4529 0.058 Uiso 1 1 calc R . . . .
C3 C 0.06832(18) 0.5206(4) 0.46745(17) 0.0579(9) Uani 1 1 d . . . . .
H3 H 0.0315 0.4896 0.4435 0.069 Uiso 1 1 calc R . . . .
C4 C 0.06650(19) 0.6315(4) 0.49631(19) 0.0643(10) Uani 1 1 d . . . . .
H4 H 0.0286 0.6738 0.4931 0.077 Uiso 1 1 calc R . . . .
C5 C 0.12080(19) 0.6773(3) 0.52929(17) 0.0561(9) Uani 1 1 d . . . . .
H5 H 0.1199 0.7531 0.5477 0.067 Uiso 1 1 calc R . . . .
C6 C 0.17835(16) 0.6148(3) 0.53672(13) 0.0439(7) Uani 1 1 d . . . . .
C7 C 0.23255(19) 0.6747(3) 0.57206(14) 0.0509(9) Uani 1 1 d . . . . .
H7 H 0.2266 0.7541 0.5850 0.061 Uiso 1 1 calc R . . . .
C8 C 0.3371(2) 0.6987(4) 0.6272(2) 0.0767(13) Uani 1 1 d . . . . .
H8A H 0.3381 0.6752 0.6674 0.092 Uiso 1 1 calc R . . . .
H8B H 0.3287 0.7867 0.6232 0.092 Uiso 1 1 calc R . . . .
C9 C 0.3973(2) 0.6706(4) 0.6131(2) 0.0775(13) Uani 1 1 d . . . . .
H9A H 0.4308 0.7077 0.6426 0.093 Uiso 1 1 calc R . . . .
H9B H 0.3982 0.7083 0.5757 0.093 Uiso 1 1 calc R . . . .
C10 C 0.4317(2) 0.4802(5) 0.66787(15) 0.0705(12) Uani 1 1 d . . . . .
H10A H 0.3976 0.4825 0.6883 0.085 Uiso 1 1 calc R . . . .
H10B H 0.4666 0.5280 0.6904 0.085 Uiso 1 1 calc R . . . .
C11 C 0.4524(2) 0.3504(5) 0.6642(2) 0.0925(17) Uani 1 1 d . . . . .
H11A H 0.4170 0.3015 0.6433 0.111 Uiso 1 1 calc R . . . .
H11B H 0.4658 0.3168 0.7034 0.111 Uiso 1 1 calc R . . . .
C12 C 0.5059(2) 0.3409(5) 0.6333(3) 0.0950(17) Uani 1 1 d . . . . .
H12A H 0.5431 0.3817 0.6563 0.114 Uiso 1 1 calc R . . . .
H12B H 0.5162 0.2548 0.6288 0.114 Uiso 1 1 calc R . . . .
C13 C 0.4870(2) 0.3996(5) 0.5755(2) 0.0853(15) Uani 1 1 d . . . . .
H13A H 0.4542 0.3505 0.5508 0.102 Uiso 1 1 calc R . . . .
H13B H 0.5230 0.4013 0.5573 0.102 Uiso 1 1 calc R . . . .
C14 C 0.46349(19) 0.5276(4) 0.57914(18) 0.0679(12) Uani 1 1 d . . . . .
H14A H 0.4495 0.5603 0.5398 0.081 Uiso 1 1 calc R . . . .
H14B H 0.4981 0.5788 0.5996 0.081 Uiso 1 1 calc R . . . .
C15 C 0.34511(14) 0.4130(3) 0.46810(12) 0.0377(7) Uani 1 1 d . . . . .
C16 C 0.36212(14) 0.3696(3) 0.41374(12) 0.0391(7) Uani 1 1 d . . . . .
C17 C 0.35668(17) 0.4470(4) 0.36652(14) 0.0514(8) Uani 1 1 d . . . . .
H17 H 0.3431 0.5278 0.3690 0.062 Uiso 1 1 calc R . . . .
C18 C 0.3712(2) 0.4060(4) 0.31565(15) 0.0660(11) Uani 1 1 d . . . . .
H18 H 0.3659 0.4582 0.2834 0.079 Uiso 1 1 calc R . . . .
C19 C 0.3931(2) 0.2891(5) 0.31228(17) 0.0710(12) Uani 1 1 d . . . . .
H19 H 0.4038 0.2621 0.2781 0.085 Uiso 1 1 calc R . . . .
C20 C 0.3994(2) 0.2118(4) 0.35914(18) 0.0699(12) Uani 1 1 d . . . . .
H20 H 0.4148 0.1321 0.3570 0.084 Uiso 1 1 calc R . . . .
C21 C 0.38331(18) 0.2511(3) 0.40946(15) 0.0535(9) Uani 1 1 d . . . . .
H21 H 0.3867 0.1971 0.4409 0.064 Uiso 1 1 calc R . . . .
C22 C 0.29180(14) 0.2639(3) 0.62950(13) 0.0378(7) Uani 1 1 d . . . . .
C23 C 0.29945(15) 0.1973(3) 0.68645(13) 0.0430(7) Uani 1 1 d . . . . .
C24 C 0.3084(2) 0.2600(4) 0.73831(15) 0.0717(13) Uani 1 1 d . . . . .
H24 H 0.3101 0.3458 0.7383 0.086 Uiso 1 1 calc R . . . .
C25 C 0.3148(3) 0.1982(5) 0.79002(18) 0.0965(17) Uani 1 1 d . . . . .
H25 H 0.3206 0.2424 0.8249 0.116 Uiso 1 1 calc R . . . .
C26 C 0.3127(3) 0.0732(5) 0.79113(19) 0.0879(15) Uani 1 1 d . . . . .
H26 H 0.3164 0.0316 0.8265 0.106 Uiso 1 1 calc R . . . .
C27 C 0.3051(2) 0.0088(4) 0.74011(19) 0.0764(13) Uani 1 1 d . . . . .
H27 H 0.3045 -0.0771 0.7407 0.092 Uiso 1 1 calc R . . . .
C28 C 0.29834(18) 0.0703(3) 0.68774(16) 0.0562(9) Uani 1 1 d . . . . .
H28 H 0.2930 0.0258 0.6530 0.067 Uiso 1 1 calc R . . . .
C29 C 0.4802(5) 0.0457(11) 0.7554(4) 0.111(4) Uiso 0.5 1 d . . . A -1
H29A H 0.4407 0.0594 0.7671 0.134 Uiso 0.5 1 calc R . . A -1
H29B H 0.5004 0.1253 0.7545 0.134 Uiso 0.5 1 calc R . . A -1
Cl1 Cl 0.4646(6) -0.0138(10) 0.6885(4) 0.182(4) Uani 0.5 1 d . . . A -1
N1 N 0.28773(14) 0.6306(3) 0.58749(12) 0.0476(7) Uani 1 1 d . . . . .
N2 N 0.41031(14) 0.5366(3) 0.60980(12) 0.0504(7) Uani 1 1 d . . . . .
Ni1 Ni 0.31713(2) 0.47337(4) 0.56206(2) 0.03680(13) Uani 1 1 d . . . . .
Ni2 Ni 0.2500 0.2500 0.5000 0.03449(15) Uani 1 2 d S T P . .
O1 O 0.23009(10) 0.42891(19) 0.51916(9) 0.0422(5) Uani 1 1 d . . . . .
O2 O 0.33915(10) 0.33332(18) 0.50709(8) 0.0376(5) Uani 1 1 d . . . . .
O3 O 0.33876(12) 0.5246(2) 0.47758(9) 0.0478(6) Uani 1 1 d . . . . .
O5 O 0.22513(10) 0.2981(2) 0.41575(8) 0.0420(5) Uani 1 1 d . . . . .
O4 O 0.30452(11) 0.3772(2) 0.63197(9) 0.0453(5) Uani 1 1 d . . . . .
Cl2 Cl 0.5272(5) -0.0443(11) 0.8063(4) 0.215(6) Uani 0.5 1 d . . . A -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
C1 C2 1.401(5) . ?
C1 C6 1.413(4) . ?
C1 O1 1.306(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.366(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.383(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.351(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.398(5) . ?
C6 C7 1.434(5) . ?
C7 H7 0.9300 . ?
C7 N1 1.266(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.453(6) . ?
C8 N1 1.453(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 N2 1.483(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.483(7) . ?
C10 N2 1.468(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.505(7) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.468(7) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.487(7) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 N2 1.495(5) . ?
C15 C16 1.481(4) . ?
C15 Ni1 2.499(3) . ?
C15 O2 1.284(4) . ?
C15 O3 1.241(4) . ?
C16 C17 1.371(4) . ?
C16 C21 1.374(5) . ?
C17 H17 0.9300 . ?
C17 C18 1.373(5) . ?
C18 H18 0.9300 . ?
C18 C19 1.361(6) . ?
C19 H19 0.9300 . ?
C19 C20 1.363(6) . ?
C20 H20 0.9300 . ?
C20 C21 1.371(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.493(4) . ?
C22 O5 1.239(4) 7_556 ?
C22 O4 1.256(4) . ?
C23 C24 1.367(5) . ?
C23 C28 1.375(5) . ?
C24 H24 0.9300 . ?
C24 C25 1.363(6) . ?
C25 H25 0.9300 . ?
C25 C26 1.355(7) . ?
C26 H26 0.9300 . ?
C26 C27 1.361(6) . ?
C27 H27 0.9300 . ?
C27 C28 1.374(5) . ?
C28 H28 0.9300 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 Cl1 1.656(9) . ?
C29 Cl2 1.693(9) . ?
N1 Ni1 1.957(3) . ?
N2 Ni1 2.191(3) . ?
Ni1 O1 1.991(2) . ?
Ni1 O2 2.113(2) . ?
Ni1 O3 2.206(3) . ?
Ni1 O4 2.011(2) . ?
Ni2 O1 2.056(2) . ?
Ni2 O1 2.056(2) 7_556 ?
Ni2 O2 2.110(2) 7_556 ?
Ni2 O2 2.110(2) . ?
Ni2 O5 1.995(2) . ?
Ni2 O5 1.995(2) 7_556 ?
O5 C22 1.239(4) 7_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 117.5(3) . . ?
O1 C1 C2 119.9(3) . . ?
O1 C1 C6 122.6(3) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 C1 121.2(3) . . ?
C3 C2 H2 119.4 . . ?
C2 C3 H3 119.5 . . ?
C2 C3 C4 121.1(4) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 H4 120.6 . . ?
C5 C4 C3 118.7(4) . . ?
C5 C4 H4 120.6 . . ?
C4 C5 H5 118.8 . . ?
C4 C5 C6 122.4(4) . . ?
C6 C5 H5 118.8 . . ?
C1 C6 C7 124.5(3) . . ?
C5 C6 C1 118.9(3) . . ?
C5 C6 C7 116.7(3) . . ?
C6 C7 H7 116.7 . . ?
N1 C7 C6 126.6(3) . . ?
N1 C7 H7 116.7 . . ?
H8A C8 H8B 108.3 . . ?
C9 C8 H8A 109.9 . . ?
C9 C8 H8B 109.9 . . ?
N1 C8 H8A 109.9 . . ?
N1 C8 H8B 109.9 . . ?
N1 C8 C9 108.7(3) . . ?
C8 C9 H9A 108.7 . . ?
C8 C9 H9B 108.7 . . ?
C8 C9 N2 114.1(4) . . ?
H9A C9 H9B 107.6 . . ?
N2 C9 H9A 108.7 . . ?
N2 C9 H9B 108.7 . . ?
H10A C10 H10B 107.9 . . ?
C11 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
N2 C10 H10A 109.2 . . ?
N2 C10 H10B 109.2 . . ?
N2 C10 C11 112.2(4) . . ?
C10 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
C10 C11 C12 111.7(4) . . ?
H11A C11 H11B 107.9 . . ?
C12 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C11 C12 H12A 109.8 . . ?
C11 C12 H12B 109.8 . . ?
H12A C12 H12B 108.3 . . ?
C13 C12 C11 109.2(4) . . ?
C13 C12 H12A 109.8 . . ?
C13 C12 H12B 109.8 . . ?
C12 C13 H13A 109.2 . . ?
C12 C13 H13B 109.2 . . ?
C12 C13 C14 112.2(4) . . ?
H13A C13 H13B 107.9 . . ?
C14 C13 H13A 109.2 . . ?
C14 C13 H13B 109.2 . . ?
C13 C14 H14A 108.8 . . ?
C13 C14 H14B 108.8 . . ?
C13 C14 N2 113.7(3) . . ?
H14A C14 H14B 107.7 . . ?
N2 C14 H14A 108.8 . . ?
N2 C14 H14B 108.8 . . ?
C16 C15 Ni1 176.5(2) . . ?
O2 C15 C16 118.9(3) . . ?
O2 C15 Ni1 57.69(15) . . ?
O3 C15 C16 121.5(3) . . ?
O3 C15 Ni1 61.92(15) . . ?
O3 C15 O2 119.6(3) . . ?
C17 C16 C15 120.4(3) . . ?
C17 C16 C21 118.7(3) . . ?
C21 C16 C15 120.8(3) . . ?
C16 C17 H17 119.7 . . ?
C16 C17 C18 120.5(4) . . ?
C18 C17 H17 119.7 . . ?
C17 C18 H18 119.9 . . ?
C19 C18 C17 120.2(4) . . ?
C19 C18 H18 119.9 . . ?
C18 C19 H19 120.1 . . ?
C18 C19 C20 119.8(4) . . ?
C20 C19 H19 120.1 . . ?
C19 C20 H20 119.9 . . ?
C19 C20 C21 120.2(4) . . ?
C21 C20 H20 119.9 . . ?
C16 C21 H21 119.8 . . ?
C20 C21 C16 120.5(4) . . ?
C20 C21 H21 119.8 . . ?
O5 C22 C23 117.1(3) 7_556 . ?
O5 C22 O4 126.1(3) 7_556 . ?
O4 C22 C23 116.9(3) . . ?
C24 C23 C22 121.3(3) . . ?
C24 C23 C28 118.4(3) . . ?
C28 C23 C22 120.2(3) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 C23 120.8(4) . . ?
C25 C24 H24 119.6 . . ?
C24 C25 H25 119.7 . . ?
C26 C25 C24 120.6(4) . . ?
C26 C25 H25 119.7 . . ?
C25 C26 H26 120.2 . . ?
C25 C26 C27 119.5(4) . . ?
C27 C26 H26 120.2 . . ?
C26 C27 H27 119.9 . . ?
C26 C27 C28 120.2(4) . . ?
C28 C27 H27 119.9 . . ?
C23 C28 H28 119.8 . . ?
C27 C28 C23 120.3(4) . . ?
C27 C28 H28 119.8 . . ?
H29A C29 H29B 107.7 . . ?
Cl1 C29 H29A 108.8 . . ?
Cl1 C29 H29B 108.8 . . ?
Cl1 C29 Cl2 113.9(8) . . ?
Cl2 C29 H29A 108.8 . . ?
Cl2 C29 H29B 108.8 . . ?
C7 N1 C8 120.5(3) . . ?
C7 N1 Ni1 126.5(2) . . ?
C8 N1 Ni1 113.1(3) . . ?
C9 N2 C14 105.4(3) . . ?
C9 N2 Ni1 99.6(2) . . ?
C10 N2 C9 112.5(3) . . ?
C10 N2 C14 107.4(3) . . ?
C10 N2 Ni1 114.0(2) . . ?
C14 N2 Ni1 117.4(2) . . ?
N1 Ni1 C15 131.01(11) . . ?
N1 Ni1 N2 84.29(12) . . ?
N1 Ni1 O1 91.46(11) . . ?
N1 Ni1 O2 160.69(10) . . ?
N1 Ni1 O3 101.81(11) . . ?
N1 Ni1 O4 95.07(11) . . ?
N2 Ni1 C15 98.67(11) . . ?
N2 Ni1 O3 91.14(11) . . ?
O1 Ni1 C15 83.35(10) . . ?
O1 Ni1 N2 175.64(10) . . ?
O1 Ni1 O2 80.72(9) . . ?
O1 Ni1 O3 88.75(10) . . ?
O1 Ni1 O4 89.87(10) . . ?
O2 Ni1 C15 30.91(9) . . ?
O2 Ni1 N2 103.01(11) . . ?
O2 Ni1 O3 60.66(9) . . ?
O3 Ni1 C15 29.76(9) . . ?
O4 Ni1 C15 133.41(10) . . ?
O4 Ni1 N2 91.49(11) . . ?
O4 Ni1 O2 102.49(10) . . ?
O4 Ni1 O3 163.09(9) . . ?
O1 Ni2 O1 180.0 7_556 . ?
O1 Ni2 O2 79.33(9) . . ?
O1 Ni2 O2 100.67(9) 7_556 . ?
O1 Ni2 O2 100.67(9) . 7_556 ?
O1 Ni2 O2 79.33(9) 7_556 7_556 ?
O2 Ni2 O2 180.00(10) . 7_556 ?
O5 Ni2 O1 86.94(9) . . ?
O5 Ni2 O1 93.06(9) . 7_556 ?
O5 Ni2 O1 86.94(9) 7_556 7_556 ?
O5 Ni2 O1 93.06(9) 7_556 . ?
O5 Ni2 O2 90.32(8) . . ?
O5 Ni2 O2 90.32(8) 7_556 7_556 ?
O5 Ni2 O2 89.68(8) . 7_556 ?
O5 Ni2 O2 89.68(8) 7_556 . ?
O5 Ni2 O5 180.0 . 7_556 ?
C1 O1 Ni1 127.8(2) . . ?
C1 O1 Ni2 135.5(2) . . ?
Ni1 O1 Ni2 96.61(10) . . ?
C15 O2 Ni1 91.40(18) . . ?
C15 O2 Ni2 117.99(18) . . ?
Ni2 O2 Ni1 91.40(9) . . ?
C15 O3 Ni1 88.33(18) . . ?
C22 O5 Ni2 131.9(2) 7_556 . ?
C22 O4 Ni1 122.48(19) . . ?

_database_code_depnum_ccdc_archive 'CCDC 986869'
#######################################################################
#
#                 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_6

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H54 N4 Ni3 O12'
_chemical_formula_weight         934.98

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                   9.5838(3)
_cell_length_b                   18.8156(7)
_cell_length_c                   11.9457(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.1170(10)
_cell_angle_gamma                90.00
_cell_volume                     2069.44(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7867
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      28.99

_exptl_crystal_description       hexagonal
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             980
_exptl_absorpt_coefficient_mu    1.416
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7275
_exptl_absorpt_correction_T_max  0.7847
_exptl_absorpt_process_details   'SADABS (Sheldrick 2008)'

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29489
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         30.90
_reflns_number_total             6458
_reflns_number_gt                4934
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)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       ?
_refine_ls_number_reflns         6458
_refine_ls_number_parameters     261
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.1185
_refine_ls_wR_factor_gt          0.1029
_refine_ls_goodness_of_fit_ref   0.835
_refine_ls_restrained_S_all      0.835
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.29827(19) 0.87287(9) -0.11239(14) 0.0315(3) Uani 1 1 d . . .
C2 C 0.2311(2) 0.91222(10) -0.21335(17) 0.0444(5) Uani 1 1 d . . .
H2 H 0.2653 0.9575 -0.2223 0.053 Uiso 1 1 calc R . .
C3 C 0.1157(3) 0.88508(12) -0.2993(2) 0.0574(6) Uani 1 1 d . . .
H3 H 0.0714 0.9131 -0.3635 0.069 Uiso 1 1 calc R . .
C4 C 0.0648(3) 0.81707(14) -0.2916(2) 0.0639(7) Uani 1 1 d . . .
H4 H -0.0110 0.7986 -0.3509 0.077 Uiso 1 1 calc R . .
C5 C 0.1283(2) 0.77756(12) -0.1951(2) 0.0527(5) Uani 1 1 d . . .
H5 H 0.0939 0.7318 -0.1896 0.063 Uiso 1 1 calc R . .
C6 C 0.2438(2) 0.80314(10) -0.10347(16) 0.0362(4) Uani 1 1 d . . .
C7 C 0.2983(2) 0.75594(9) -0.00626(17) 0.0387(4) Uani 1 1 d . . .
H7 H 0.2536 0.7118 -0.0109 0.046 Uiso 1 1 calc R . .
C8 C 0.4427(3) 0.71451(10) 0.1769(2) 0.0489(5) Uani 1 1 d . . .
H8A H 0.4245 0.6674 0.1431 0.059 Uiso 1 1 calc R . .
H8B H 0.3859 0.7204 0.2320 0.059 Uiso 1 1 calc R . .
C9 C 0.6023(3) 0.72320(10) 0.23826(19) 0.0498(5) Uani 1 1 d . . .
H9A H 0.6292 0.6910 0.3042 0.060 Uiso 1 1 calc R . .
H9B H 0.6589 0.7108 0.1852 0.060 Uiso 1 1 calc R . .
C10 C 0.7974(3) 0.80329(13) 0.3218(2) 0.0534(5) Uani 1 1 d . . .
H10A H 0.8378 0.7987 0.2562 0.064 Uiso 1 1 calc R . .
H10B H 0.8351 0.7647 0.3755 0.064 Uiso 1 1 calc R . .
C11 C 0.8442(3) 0.87236(15) 0.3815(2) 0.0664(7) Uani 1 1 d . . .
H11A H 0.9495 0.8741 0.4071 0.080 Uiso 1 1 calc R . .
H11B H 0.8108 0.9109 0.3266 0.080 Uiso 1 1 calc R . .
C12 C 0.6355(3) 0.88064(15) 0.4387(2) 0.0616(7) Uani 1 1 d . . .
H12A H 0.6021 0.9192 0.3838 0.074 Uiso 1 1 calc R . .
H12B H 0.5963 0.8883 0.5043 0.074 Uiso 1 1 calc R . .
C13 C 0.5791(3) 0.81173(12) 0.38118(17) 0.0494(5) Uani 1 1 d . . .
H13A H 0.6074 0.7734 0.4372 0.059 Uiso 1 1 calc R . .
H13B H 0.4738 0.8133 0.3553 0.059 Uiso 1 1 calc R . .
C14 C 0.3668(2) 0.97370(10) 0.19577(16) 0.0369(4) Uani 1 1 d . . .
C15 C 0.2767(4) 1.00443(13) 0.2702(2) 0.0635(7) Uani 1 1 d . . .
H15A H 0.3274 1.0457 0.3105 0.076 Uiso 1 1 calc R . .
H15B H 0.1856 1.0210 0.2186 0.076 Uiso 1 1 calc R . .
C16 C 0.2427(4) 0.95641(16) 0.3590(3) 0.0817(10) Uani 1 1 d . . .
H16A H 0.2026 0.9127 0.3224 0.123 Uiso 1 1 calc R . .
H16B H 0.1736 0.9791 0.3920 0.123 Uiso 1 1 calc R . .
H16C H 0.3301 0.9466 0.4195 0.123 Uiso 1 1 calc R . .
C17 C 0.2548(2) 1.10368(9) -0.07211(16) 0.0350(4) Uani 1 1 d . . .
C18 C 0.1151(2) 1.07299(12) -0.0601(2) 0.0536(5) Uani 1 1 d . . .
H18A H 0.0628 1.0527 -0.1346 0.064 Uiso 1 1 calc R . .
H18B H 0.1386 1.0343 -0.0043 0.064 Uiso 1 1 calc R . .
C19 C 0.0171(4) 1.12183(17) -0.0235(4) 0.0924(11) Uani 1 1 d . . .
H19A H 0.0630 1.1386 0.0539 0.139 Uiso 1 1 calc R . .
H19B H -0.0712 1.0974 -0.0242 0.139 Uiso 1 1 calc R . .
H19C H -0.0048 1.1615 -0.0761 0.139 Uiso 1 1 calc R . .
N1 N 0.40178(18) 0.76814(8) 0.08585(14) 0.0357(3) Uani 1 1 d . . .
N2 N 0.63625(18) 0.79739(8) 0.27965(13) 0.0383(3) Uani 1 1 d . . .
Ni1 Ni 0.51903(2) 0.856343(10) 0.120814(18) 0.02896(8) Uani 1 1 d . . .
Ni2 Ni 0.5000 1.0000 0.0000 0.02915(9) Uani 1 2 d S . .
O1 O 0.40649(14) 0.90035(6) -0.03140(10) 0.0343(3) Uani 1 1 d . . .
O4 O 0.39347(16) 0.90814(7) 0.20455(11) 0.0381(3) Uani 1 1 d . . .
O5 O 0.40616(16) 1.01661(7) 0.13023(12) 0.0400(3) Uani 1 1 d . . .
O3 O 0.70917(16) 0.83339(7) 0.05105(13) 0.0419(3) Uani 1 1 d . . .
O2 O 0.33658(14) 1.06242(6) -0.11345(11) 0.0330(3) Uani 1 1 d . . .
O6 O 0.7894(2) 0.88210(11) 0.47827(15) 0.0735(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
C1 O1 1.312(2) . ?
C1 C2 1.409(3) . ?
C1 C6 1.427(3) . ?
C2 C3 1.382(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.382(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.365(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.408(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.440(3) . ?
C7 N1 1.281(2) . ?
C7 H7 0.9300 . ?
C8 N1 1.456(2) . ?
C8 C9 1.510(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.487(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.490(3) . ?
C10 C11 1.490(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 O6 1.408(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 O6 1.419(4) . ?
C12 C13 1.496(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.488(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 O5 1.254(2) . ?
C14 O4 1.258(2) . ?
C14 C15 1.515(3) . ?
C15 C16 1.497(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 O3 1.240(2) 3_675 ?
C17 O2 1.295(2) . ?
C17 C18 1.501(3) . ?
C17 Ni1 2.5107(19) 3_675 ?
C18 C19 1.465(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
N1 Ni1 1.9827(15) . ?
N2 Ni1 2.2156(15) . ?
Ni1 O1 2.0165(12) . ?
Ni1 O4 2.0166(13) . ?
Ni1 O2 2.0801(12) 3_675 ?
Ni1 O3 2.2461(15) . ?
Ni1 C17 2.5107(19) 3_675 ?
Ni2 O5 2.0257(13) . ?
Ni2 O5 2.0257(13) 3_675 ?
Ni2 O1 2.0670(12) 3_675 ?
Ni2 O1 2.0671(12) . ?
Ni2 O2 2.1191(12) 3_675 ?
Ni2 O2 2.1191(12) . ?
O3 C17 1.240(2) 3_675 ?
O2 Ni1 2.0800(12) 3_675 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 120.24(16) . . ?
O1 C1 C6 122.54(16) . . ?
C2 C1 C6 117.22(16) . . ?
C3 C2 C1 121.5(2) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
C2 C3 C4 121.1(2) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 118.6(2) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
C4 C5 C6 122.7(2) . . ?
C4 C5 H5 118.6 . . ?
C6 C5 H5 118.6 . . ?
C5 C6 C1 118.77(18) . . ?
C5 C6 C7 116.56(17) . . ?
C1 C6 C7 124.67(16) . . ?
N1 C7 C6 127.12(16) . . ?
N1 C7 H7 116.4 . . ?
C6 C7 H7 116.4 . . ?
N1 C8 C9 108.32(16) . . ?
N1 C8 H8A 110.0 . . ?
C9 C8 H8A 110.0 . . ?
N1 C8 H8B 110.0 . . ?
C9 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
N2 C9 C8 111.22(17) . . ?
N2 C9 H9A 109.4 . . ?
C8 C9 H9A 109.4 . . ?
N2 C9 H9B 109.4 . . ?
C8 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
N2 C10 C11 111.9(2) . . ?
N2 C10 H10A 109.2 . . ?
C11 C10 H10A 109.2 . . ?
N2 C10 H10B 109.2 . . ?
C11 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
O6 C11 C10 112.0(2) . . ?
O6 C11 H11A 109.2 . . ?
C10 C11 H11A 109.2 . . ?
O6 C11 H11B 109.2 . . ?
C10 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
O6 C12 C13 112.3(2) . . ?
O6 C12 H12A 109.1 . . ?
C13 C12 H12A 109.1 . . ?
O6 C12 H12B 109.1 . . ?
C13 C12 H12B 109.1 . . ?
H12A C12 H12B 107.9 . . ?
N2 C13 C12 111.31(19) . . ?
N2 C13 H13A 109.4 . . ?
C12 C13 H13A 109.4 . . ?
N2 C13 H13B 109.4 . . ?
C12 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
O5 C14 O4 126.43(18) . . ?
O5 C14 C15 116.10(17) . . ?
O4 C14 C15 117.46(18) . . ?
C16 C15 C14 117.2(2) . . ?
C16 C15 H15A 108.0 . . ?
C14 C15 H15A 108.0 . . ?
C16 C15 H15B 108.0 . . ?
C14 C15 H15B 108.0 . . ?
H15A C15 H15B 107.2 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O3 C17 O2 119.09(17) 3_675 . ?
O3 C17 C18 123.62(18) 3_675 . ?
O2 C17 C18 117.16(16) . . ?
O3 C17 Ni1 63.32(10) 3_675 3_675 ?
O2 C17 Ni1 55.81(9) . 3_675 ?
C18 C17 Ni1 171.04(15) . 3_675 ?
C19 C18 C17 116.8(2) . . ?
C19 C18 H18A 108.1 . . ?
C17 C18 H18A 108.1 . . ?
C19 C18 H18B 108.1 . . ?
C17 C18 H18B 108.1 . . ?
H18A C18 H18B 107.3 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C7 N1 C8 120.12(16) . . ?
C7 N1 Ni1 126.10(13) . . ?
C8 N1 Ni1 113.78(13) . . ?
C9 N2 C13 110.20(17) . . ?
C9 N2 C10 107.06(17) . . ?
C13 N2 C10 107.01(17) . . ?
C9 N2 Ni1 99.97(11) . . ?
C13 N2 Ni1 113.17(12) . . ?
C10 N2 Ni1 118.94(13) . . ?
N1 Ni1 O1 91.36(6) . . ?
N1 Ni1 O4 97.33(6) . . ?
O1 Ni1 O4 90.31(5) . . ?
N1 Ni1 O2 161.99(6) . 3_675 ?
O1 Ni1 O2 81.70(5) . 3_675 ?
O4 Ni1 O2 99.29(5) . 3_675 ?
N1 Ni1 N2 83.35(6) . . ?
O1 Ni1 N2 174.20(5) . . ?
O4 Ni1 N2 92.73(6) . . ?
O2 Ni1 N2 102.65(6) 3_675 . ?
N1 Ni1 O3 103.39(6) . . ?
O1 Ni1 O3 91.74(5) . . ?
O4 Ni1 O3 159.11(5) . . ?
O2 Ni1 O3 60.52(5) 3_675 . ?
N2 Ni1 O3 87.18(6) . . ?
N1 Ni1 C17 132.63(6) . 3_675 ?
O1 Ni1 C17 87.02(6) . 3_675 ?
O4 Ni1 C17 129.99(6) . 3_675 ?
O2 Ni1 C17 30.99(5) 3_675 3_675 ?
N2 Ni1 C17 94.78(6) . 3_675 ?
O3 Ni1 C17 29.54(5) . 3_675 ?
O5 Ni2 O5 180.00(8) . 3_675 ?
O5 Ni2 O1 89.04(5) . 3_675 ?
O5 Ni2 O1 90.96(5) 3_675 3_675 ?
O5 Ni2 O1 90.96(5) . . ?
O5 Ni2 O1 89.04(5) 3_675 . ?
O1 Ni2 O1 180.0 3_675 . ?
O5 Ni2 O2 90.07(5) . 3_675 ?
O5 Ni2 O2 89.93(5) 3_675 3_675 ?
O1 Ni2 O2 100.39(5) 3_675 3_675 ?
O1 Ni2 O2 79.61(5) . 3_675 ?
O5 Ni2 O2 89.93(5) . . ?
O5 Ni2 O2 90.07(5) 3_675 . ?
O1 Ni2 O2 79.61(5) 3_675 . ?
O1 Ni2 O2 100.39(5) . . ?
O2 Ni2 O2 180.0 3_675 . ?
C1 O1 Ni1 128.20(11) . . ?
C1 O1 Ni2 134.86(11) . . ?
Ni1 O1 Ni2 96.45(5) . . ?
C14 O4 Ni1 124.62(12) . . ?
C14 O5 Ni2 130.93(12) . . ?
C17 O3 Ni1 87.14(11) 3_675 . ?
C17 O2 Ni1 93.20(10) . 3_675 ?
C17 O2 Ni2 120.44(11) . . ?
Ni1 O2 Ni2 92.98(5) 3_675 . ?
C11 O6 C12 108.30(18) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        30.90
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.061
_database_code_depnum_ccdc_archive 'CCDC 986870'
#######################################################################
#
#                 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_added_by_encifer

_audit_creation_date             2014-05-27
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C54 H54 N4 Ni3 O12,3(C H2 Cl2)'
_chemical_formula_sum            'C57 H60 Cl6 N4 Ni3 O12'
_chemical_formula_weight         1381.92
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 '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'
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        P2(1)/n
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.9987(16)
_cell_length_b                   19.977(3)
_cell_length_c                   15.049(2)
_cell_angle_alpha                90
_cell_angle_beta                 109.934(4)
_cell_angle_gamma                90
_cell_volume                     3108.5(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5140
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      22.94
_exptl_crystal_description       block
_exptl_crystal_colour            green
_shelx_estimated_absorpt_T_max   0.810
_shelx_estimated_absorpt_T_min   0.775
_exptl_absorpt_coefficient_mu    1.219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7882
_exptl_absorpt_correction_T_max  0.8216
_exptl_absorpt_process_details   'SADABS (Sheldrick 2008)'
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37221
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.841
_diffrn_reflns_theta_min         1.764
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'fine-focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4034
_reflns_number_total             5991
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         5991
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0509
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0810P)²+1.8460P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1567
_refine_special_details          
;
One DCM molecule is disordered between 4 alternative orientations: (i) 
Cl(3), its inversion equivalent and C(29) (with attached hydrogens), 
(ii) Cl(3) and the inversion equivalents of Cl(3) and C(29), 
(iii) Cl(4)C(30)Cl(5) and (iv) its inversion equivalent, with 
contributions of 35%, 35%, 15%, and 15%, respectively. 
The morpholinyl-methyl moiety, C(9)N(2)C(10)C(11)O(6)C(12)C(13), 
is disordered equally between two orientations, A and B.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 Cl5-Cl3
 1.54 with sigma of 0.02
 C9A-C8 \\sim C9B-C8
 with sigma of 0.02
 N2A-C9A \\sim N2B-C9B
 with sigma of 0.02
 N2B-C13A \\sim N2B-C10B \\sim N2A-C13B \\sim N2A-C10A
 with sigma of 0.02
 O6A-C12B \\sim O6B-C12A \\sim O6B-C11B \\sim O6A-C11A
 with sigma of 0.02
 C13B-C12B \\sim C13A-C12A \\sim C11B-C10B \\sim C11A-C10A
 with sigma of 0.02
 C30-Cl4 \\sim C30-Cl5
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N2A) = Uanis(N2B)
Uanis(O6A) = Uanis(O6B)
Uanis(C10B) = Uanis(C10A)
Uanis(C13B) = Uanis(C13A)
Uanis(C12B) = Uanis(C12A)
Uanis(C11B) = Uanis(C11A)
Uiso(Cl5) = Uiso(Cl4)
4. Others
 Fixed Sof: H8AA(0.5) H8AB(0.5) H8BC(0.5) H8BD(0.5) C10B(0.5) H10A(0.5)
 H10B(0.5) C11B(0.5) H11A(0.5) H11B(0.5) C12B(0.5) H12A(0.5) H12B(0.5)
 C13B(0.5) H13A(0.5) H13B(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5) C9B(0.5) H9BA(0.5)
 H9BB(0.5) N2A(0.5) O6B(0.5) Cl3(0.7) Cl5(0.15) C13A(0.5) H13C(0.5) H13D(0.5)
 C10A(0.5) H10C(0.5) H10D(0.5) C12A(0.5) H12C(0.5) H12D(0.5) C11A(0.5)
 H11C(0.5) H11D(0.5) O6A(0.5) N2B(0.5) Cl4(0.15) C29(0.35) H29A(0.35)
 H29B(0.35) C30(0.15) H30A(0.15) H30B(0.15)
5.a Riding coordinates:
 C8(H8AA,H8AB,H8BC,H8BD), C9A(H9AA,H9AB), C9B(H9BA,H9BB), C29(H29A,H29B),
 C30(H30A,H30B)
5.b Secondary CH2 refined with riding coordinates:
 C10B(H10A,H10B), C11B(H11A,H11B), C12B(H12A,H12B), C13B(H13A,H13B), C28(H28A,
 H28B), C13A(H13C,H13D), C10A(H10C,H10D), C12A(H12C,H12D), C11A(H11C,H11D)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
C1 C 0.2252(4) 0.93639(17) 0.4508(3) 0.0462(9) Uani 1 1 d . . . . .
C2 C 0.2229(4) 0.9156(2) 0.3612(3) 0.0581(11) Uani 1 1 d . . . . .
H2 H 0.2917 0.9263 0.3411 0.070 Uiso 1 1 calc R . . . .
C3 C 0.1202(5) 0.8795(2) 0.3027(4) 0.0753(14) Uani 1 1 d . . . . .
H3 H 0.1207 0.8666 0.2434 0.090 Uiso 1 1 calc R . . . .
C4 C 0.0168(5) 0.8620(3) 0.3296(4) 0.0869(16) Uani 1 1 d . . . . .
H4 H -0.0498 0.8355 0.2909 0.104 Uiso 1 1 calc R . . . .
C5 C 0.0146(5) 0.8844(3) 0.4138(4) 0.0804(15) Uani 1 1 d . . . . .
H5 H -0.0575 0.8751 0.4307 0.096 Uiso 1 1 calc R . . . .
C6 C 0.1167(4) 0.9213(2) 0.4769(3) 0.0561(10) Uani 1 1 d . . . . .
C7 C 0.1018(5) 0.9398(2) 0.5648(4) 0.0651(12) Uani 1 1 d . . . . .
H7 H 0.0212 0.9322 0.5702 0.078 Uiso 1 1 calc R . . . .
C8 C 0.1610(6) 0.9789(3) 0.7236(4) 0.0833(16) Uani 1 1 d . . . . .
H8AA_a H 0.0858 0.9534 0.7230 0.100 Uiso 0.5 1 d R . . A 1
H8AB_a H 0.1449 1.0262 0.7289 0.100 Uiso 0.5 1 d R . . A 1
H8BC_b H 0.1708 0.9379 0.7598 0.100 Uiso 0.5 1 d R . . B 2
H8BD_b H 0.0728 0.9949 0.7070 0.100 Uiso 0.5 1 d R . . B 2
C10B_b C 0.4429(15) 0.9578(9) 0.8667(11) 0.082(4) Uani 0.5 1 d . . . C 2
H10A_b H 0.4212 0.9647 0.9233 0.098 Uiso 0.5 1 calc R . . C 2
H10B_b H 0.4088 0.9148 0.8393 0.098 Uiso 0.5 1 calc R . . C 2
C11B_b C 0.5853(15) 0.9608(9) 0.8887(16) 0.098(5) Uani 0.5 1 d . . . C 2
H11A_b H 0.6250 0.9253 0.9332 0.118 Uiso 0.5 1 calc R . . C 2
H11B_b H 0.6034 0.9517 0.8311 0.118 Uiso 0.5 1 calc R . . C 2
C12B_a C 0.5353(17) 1.0858(12) 0.8503(16) 0.106(6) Uani 0.5 1 d . . . D 1
H12A_a H 0.5511 1.0855 0.7907 0.127 Uiso 0.5 1 calc R . . D 1
H12B_a H 0.5363 1.1320 0.8703 0.127 Uiso 0.5 1 calc R . . D 1
C13B_a C 0.4041(14) 1.0570(6) 0.8349(9) 0.072(3) Uani 0.5 1 d . . . D 1
H13A_a H 0.3873 1.0565 0.8941 0.086 Uiso 0.5 1 calc R . . D 1
H13B_a H 0.3387 1.0845 0.7903 0.086 Uiso 0.5 1 calc R . . D 1
C14 C 0.5554(4) 0.90928(19) 0.6687(3) 0.0512(10) Uani 1 1 d . . . . .
C15 C 0.6719(4) 0.8672(2) 0.6939(3) 0.0534(10) Uani 1 1 d . . . . .
C16 C 0.7788(4) 0.8866(2) 0.6716(4) 0.0705(13) Uani 1 1 d . . . . .
H16 H 0.7780 0.9273 0.6413 0.085 Uiso 1 1 calc R . . . .
C17 C 0.8865(5) 0.8460(3) 0.6939(4) 0.0949(19) Uani 1 1 d . . . . .
H17 H 0.9570 0.8588 0.6771 0.114 Uiso 1 1 calc R . . . .
C18 C 0.8899(6) 0.7869(3) 0.7409(5) 0.101(2) Uani 1 1 d . . . . .
H18 H 0.9628 0.7598 0.7564 0.121 Uiso 1 1 calc R . . . .
C19 C 0.7852(6) 0.7679(3) 0.7651(5) 0.104(2) Uani 1 1 d . . . . .
H19 H 0.7878 0.7282 0.7978 0.125 Uiso 1 1 calc R . . . .
C20 C 0.6765(5) 0.8077(3) 0.7409(4) 0.0804(15) Uani 1 1 d . . . . .
H20 H 0.6054 0.7942 0.7566 0.097 Uiso 1 1 calc R . . . .
C21 C 0.3944(4) 1.11711(19) 0.5749(3) 0.0470(9) Uani 1 1 d . . . . .
C22 C 0.3622(4) 1.19051(19) 0.5663(3) 0.0531(10) Uani 1 1 d . . . . .
C23 C 0.4120(6) 1.2313(2) 0.5133(4) 0.0864(16) Uani 1 1 d . . . . .
H23 H 0.4672 1.2142 0.4840 0.104 Uiso 1 1 calc R . . . .
C24 C 0.3778(8) 1.2991(3) 0.5043(5) 0.120(3) Uani 1 1 d . . . . .
H24 H 0.4097 1.3274 0.4684 0.145 Uiso 1 1 calc R . . . .
C25 C 0.2968(8) 1.3236(3) 0.5490(5) 0.116(3) Uani 1 1 d . . . . .
H25 H 0.2744 1.3687 0.5431 0.139 Uiso 1 1 calc R . . . .
C26 C 0.2497(6) 1.2835(3) 0.6006(5) 0.100(2) Uani 1 1 d . . . . .
H26 H 0.1944 1.3008 0.6298 0.120 Uiso 1 1 calc R . . . .
C27 C 0.2827(5) 1.2174(2) 0.6107(4) 0.0745(14) Uani 1 1 d . . . . .
H27 H 0.2510 1.1901 0.6480 0.089 Uiso 1 1 calc R . . . .
C28 C 0.2524(8) 0.7627(3) 0.5629(6) 0.138(3) Uani 1 1 d . . . . .
H28A H 0.2008 0.7778 0.5001 0.165 Uiso 1 1 calc R . . . .
H28B H 0.3230 0.7941 0.5886 0.165 Uiso 1 1 calc R . . . .
C9A_a C 0.2731(10) 0.9581(5) 0.8008(7) 0.073(3) Uani 0.5 1 d . . . D 1
H9AA_a H 0.2605 0.9702 0.8595 0.088 Uiso 0.5 1 d R . . D 1
H9AB_a H 0.2807 0.9099 0.7976 0.088 Uiso 0.5 1 d R . . D 1
C9B_b C 0.2491(10) 1.0284(6) 0.7800(8) 0.084(3) Uani 0.5 1 d . . . C 2
H9BA_b H 0.2268 1.0714 0.7488 0.101 Uiso 0.5 1 d R . . C 2
H9BB_b H 0.2399 1.0306 0.8418 0.101 Uiso 0.5 1 d R . . C 2
Cl1 Cl 0.3126(4) 0.68671(14) 0.5555(3) 0.2149(14) Uani 1 1 d . . . . .
Cl2 Cl 0.1605(5) 0.76143(16) 0.6321(4) 0.280(2) Uani 1 1 d . . . . .
N1 N 0.1885(4) 0.96588(18) 0.6367(3) 0.0588(9) Uani 1 1 d . . . . .
N2A_a N 0.3968(12) 0.9873(5) 0.7974(12) 0.060(2) Uani 0.5 1 d . . . D 1
Ni1 Ni 0.36822(5) 0.98478(2) 0.64646(3) 0.04719(18) Uani 1 1 d . . . . .
Ni2 Ni 0.5000 1.0000 0.5000 0.0408(2) Uani 1 2 d S T P . .
O1 O 0.3245(3) 0.97064(13) 0.50632(18) 0.0479(6) Uani 1 1 d . . . . .
O6B_b O 0.645(3) 1.0225(8) 0.927(2) 0.118(5) Uani 0.5 1 d . . . C 2
O3 O 0.4524(3) 0.88744(14) 0.6762(2) 0.0616(8) Uani 1 1 d . . . . .
O2 O 0.5611(3) 0.97102(12) 0.64500(17) 0.0476(6) Uani 1 1 d . . . . .
O4 O 0.3456(3) 1.08335(14) 0.6252(2) 0.0579(7) Uani 1 1 d . . . . .
O5 O 0.5351(3) 0.90531(12) 0.46820(18) 0.0492(6) Uani 1 1 d . . . . .
Cl3_a Cl 0.0008(6) 1.0247(3) 0.9101(4) 0.183(2) Uani 0.7 1 d D . . E 1
Cl5 Cl -0.051(2) 0.9555(9) 0.8950(18) 0.190(8) Uiso 0.15 1 d D . . F -2
C13A_b C 0.4620(14) 1.0767(6) 0.8325(9) 0.072(3) Uani 0.5 1 d . . . C 2
H13C_b H 0.4292 1.1114 0.7852 0.086 Uiso 0.5 1 calc R . . C 2
H13D_b H 0.4456 1.0908 0.8891 0.086 Uiso 0.5 1 calc R . . C 2
C10A_a C 0.5074(14) 0.9514(9) 0.8668(11) 0.082(4) Uani 0.5 1 d . . . D 1
H10C_a H 0.5119 0.9068 0.8423 0.098 Uiso 0.5 1 calc R . . D 1
H10D_a H 0.4887 0.9461 0.9249 0.098 Uiso 0.5 1 calc R . . D 1
C12A_b C 0.6030(16) 1.0705(11) 0.8544(16) 0.106(6) Uani 0.5 1 d . . . C 2
H12C_b H 0.6220 1.0559 0.7990 0.127 Uiso 0.5 1 calc R . . C 2
H12D_b H 0.6455 1.1131 0.8752 0.127 Uiso 0.5 1 calc R . . C 2
C11A_a C 0.6381(17) 0.9832(8) 0.8906(17) 0.098(5) Uani 0.5 1 d . . . D 1
H11C_a H 0.7001 0.9583 0.9414 0.118 Uiso 0.5 1 calc R . . D 1
H11D_a H 0.6656 0.9812 0.8359 0.118 Uiso 0.5 1 calc R . . D 1
O6A_a O 0.637(3) 1.0507(8) 0.919(2) 0.118(5) Uani 0.5 1 d . . . D 1
N2B_b N 0.3900(12) 1.0133(4) 0.7971(12) 0.060(2) Uani 0.5 1 d . . . C 2
Cl4 Cl -0.004(4) 1.0129(18) 1.088(2) 0.190(8) Uiso 0.15 1 d . . . F -2
C29_a C -0.043(3) 0.9600(16) 0.967(3) 0.157(10) Uiso 0.35 1 d . . . E 1
H29A_a H -0.0013 0.9195 0.9583 0.188 Uiso 0.35 1 d R . . E 1
H29B_a H -0.1345 0.9536 0.9408 0.188 Uiso 0.35 1 d R . . E 1
C30 C -0.022(6) 1.029(3) 0.968(3) 0.124(18) Uiso 0.15 1 d . . . F -2
H30A H 0.0569 1.0483 0.9648 0.149 Uiso 0.15 1 d R . . F -2
H30B H -0.0917 1.0603 0.9405 0.149 Uiso 0.15 1 d R . . F -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.403(6) . ?
C1 C6 1.411(6) . ?
C1 O1 1.318(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.376(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.376(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.353(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.406(6) . ?
C6 C7 1.435(6) . ?
C7 H7 0.9300 . ?
C7 N1 1.284(6) . ?
C8 H8AA_a 0.9703 . ?
C8 H8AB_a 0.9698 . ?
C8 H8BC_b 0.9704 . ?
C8 H8BD_b 0.9699 . ?
C8 C9A_a 1.438(11) . ?
C8 C9B_b 1.441(11) . ?
C8 N1 1.463(6) . ?
C10B_b H10A_b 0.9700 . ?
C10B_b H10B_b 0.9700 . ?
C10B_b C11B_b 1.488(14) . ?
C10B_b N2B_b 1.500(13) . ?
C11B_b H11A_b 0.9700 . ?
C11B_b H11B_b 0.9700 . ?
C11B_b O6B_b 1.424(14) . ?
C12B_a H12A_a 0.9700 . ?
C12B_a H12B_a 0.9700 . ?
C12B_a C13B_a 1.496(14) . ?
C12B_a O6A_a 1.417(15) . ?
C13B_a H13A_a 0.9700 . ?
C13B_a H13B_a 0.9700 . ?
C13B_a N2A_a 1.494(11) . ?
C14 C15 1.470(6) . ?
C14 Ni1 2.481(4) . ?
C14 O3 1.255(5) . ?
C14 O2 1.291(4) . ?
C15 C16 1.384(6) . ?
C15 C20 1.375(6) . ?
C16 H16 0.9300 . ?
C16 C17 1.379(7) . ?
C17 H17 0.9300 . ?
C17 C18 1.370(7) . ?
C18 H18 0.9300 . ?
C18 C19 1.373(8) . ?
C19 H19 0.9300 . ?
C19 C20 1.377(7) . ?
C20 H20 0.9300 . ?
C21 C22 1.504(5) . ?
C21 O4 1.262(5) . ?
C21 O5 1.251(5) 3_676 ?
C22 C23 1.378(6) . ?
C22 C27 1.378(6) . ?
C23 H23 0.9300 . ?
C23 C24 1.398(7) . ?
C24 H24 0.9300 . ?
C24 C25 1.376(10) . ?
C25 H25 0.9300 . ?
C25 C26 1.337(9) . ?
C26 H26 0.9300 . ?
C26 C27 1.364(7) . ?
C27 H27 0.9300 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 Cl1 1.675(7) . ?
C28 Cl2 1.680(8) . ?
C9A_a H9AA_a 0.9701 . ?
C9A_a H9AB_a 0.9702 . ?
C9A_a N2A_a 1.496(13) . ?
C9B_b H9BA_b 0.9699 . ?
C9B_b H9BB_b 0.9702 . ?
C9B_b N2B_b 1.512(13) . ?
N1 Ni1 1.968(4) . ?
N2A_a Ni1 2.185(17) . ?
N2A_a C10A_a 1.490(13) . ?
Ni1 O1 2.017(3) . ?
Ni1 O3 2.134(3) . ?
Ni1 O2 2.146(3) . ?
Ni1 O4 1.997(3) . ?
Ni1 N2B_b 2.269(16) . ?
Ni2 O1 2.051(3) . ?
Ni2 O1 2.050(3) 3_676 ?
Ni2 O2 2.133(2) . ?
Ni2 O2 2.133(2) 3_676 ?
Ni2 O5 2.021(2) 3_676 ?
Ni2 O5 2.021(2) . ?
O6B_b C12A_b 1.409(15) . ?
O5 C21 1.251(5) 3_676 ?
Cl3_a C29_a 1.71(3) . ?
Cl3_a C29_a 1.77(3) 3_577 ?
Cl5 C30 1.78(4) . ?
C13A_b H13C_b 0.9700 . ?
C13A_b H13D_b 0.9700 . ?
C13A_b C12A_b 1.477(14) . ?
C13A_b N2B_b 1.493(12) . ?
C10A_a H10C_a 0.9700 . ?
C10A_a H10D_a 0.9700 . ?
C10A_a C11A_a 1.499(14) . ?
C12A_b H12C_b 0.9700 . ?
C12A_b H12D_b 0.9700 . ?
C11A_a H11C_a 0.9700 . ?
C11A_a H11D_a 0.9700 . ?
C11A_a O6A_a 1.414(14) . ?
Cl4 C30 1.78(4) . ?
C29_a Cl3_a 1.77(3) 3_577 ?
C29_a C29_a 1.94(6) 3_577 ?
C29_a H29A_a 0.9601 . ?
C29_a H29B_a 0.9600 . ?
C30 H30A 0.9699 . ?
C30 H30B 0.9699 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 117.7(4) . . ?
O1 C1 C2 120.1(4) . . ?
O1 C1 C6 122.1(4) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 C1 120.8(4) . . ?
C3 C2 H2 119.6 . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.7(5) . . ?
C4 C3 H3 119.1 . . ?
C3 C4 H4 120.9 . . ?
C5 C4 C3 118.2(5) . . ?
C5 C4 H4 120.9 . . ?
C4 C5 H5 118.6 . . ?
C4 C5 C6 122.7(5) . . ?
C6 C5 H5 118.6 . . ?
C1 C6 C7 125.1(4) . . ?
C5 C6 C1 118.7(4) . . ?
C5 C6 C7 116.2(4) . . ?
C6 C7 H7 116.7 . . ?
N1 C7 C6 126.5(4) . . ?
N1 C7 H7 116.7 . . ?
H8AA_a C8 H8AB_a 109.5 . . ?
H8BC_b C8 H8BD_b 109.4 . . ?
C9A_a C8 H8AA_a 110.4 . . ?
C9A_a C8 H8AB_a 110.2 . . ?
C9A_a C8 N1 106.8(5) . . ?
C9B_b C8 H8BC_b 109.0 . . ?
C9B_b C8 H8BD_b 109.8 . . ?
C9B_b C8 N1 110.3(5) . . ?
N1 C8 H8AA_a 109.6 . . ?
N1 C8 H8AB_a 110.3 . . ?
N1 C8 H8BC_b 109.5 . . ?
N1 C8 H8BD_b 108.8 . . ?
H10A_b C10B_b H10B_b 108.9 . . ?
C11B_b C10B_b H10A_b 110.8 . . ?
C11B_b C10B_b H10B_b 110.8 . . ?
C11B_b C10B_b N2B_b 104.7(13) . . ?
N2B_b C10B_b H10A_b 110.8 . . ?
N2B_b C10B_b H10B_b 110.8 . . ?
C10B_b C11B_b H11A_b 108.4 . . ?
C10B_b C11B_b H11B_b 108.4 . . ?
H11A_b C11B_b H11B_b 107.4 . . ?
O6B_b C11B_b C10B_b 116(2) . . ?
O6B_b C11B_b H11A_b 108.4 . . ?
O6B_b C11B_b H11B_b 108.4 . . ?
H12A_a C12B_a H12B_a 107.7 . . ?
C13B_a C12B_a H12A_a 108.8 . . ?
C13B_a C12B_a H12B_a 108.8 . . ?
O6A_a C12B_a H12A_a 108.8 . . ?
O6A_a C12B_a H12B_a 108.8 . . ?
O6A_a C12B_a C13B_a 114(2) . . ?
C12B_a C13B_a H13A_a 109.7 . . ?
C12B_a C13B_a H13B_a 109.7 . . ?
H13A_a C13B_a H13B_a 108.2 . . ?
N2A_a C13B_a C12B_a 110.0(14) . . ?
N2A_a C13B_a H13A_a 109.7 . . ?
N2A_a C13B_a H13B_a 109.7 . . ?
C15 C14 Ni1 173.0(3) . . ?
O3 C14 C15 120.8(4) . . ?
O3 C14 Ni1 59.3(2) . . ?
O3 C14 O2 119.1(4) . . ?
O2 C14 C15 119.9(4) . . ?
O2 C14 Ni1 59.9(2) . . ?
C16 C15 C14 121.0(4) . . ?
C20 C15 C14 120.2(4) . . ?
C20 C15 C16 118.8(4) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 C15 120.4(4) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 H17 119.9 . . ?
C18 C17 C16 120.1(5) . . ?
C18 C17 H17 119.9 . . ?
C17 C18 H18 120.1 . . ?
C17 C18 C19 119.8(5) . . ?
C19 C18 H18 120.1 . . ?
C18 C19 H19 119.9 . . ?
C18 C19 C20 120.1(5) . . ?
C20 C19 H19 119.9 . . ?
C15 C20 C19 120.7(5) . . ?
C15 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
O4 C21 C22 115.9(4) . . ?
O5 C21 C22 118.3(4) 3_676 . ?
O5 C21 O4 125.8(4) 3_676 . ?
C23 C22 C21 119.9(4) . . ?
C27 C22 C21 120.6(4) . . ?
C27 C22 C23 119.6(4) . . ?
C22 C23 H23 120.6 . . ?
C22 C23 C24 118.8(6) . . ?
C24 C23 H23 120.6 . . ?
C23 C24 H24 120.2 . . ?
C25 C24 C23 119.7(6) . . ?
C25 C24 H24 120.2 . . ?
C24 C25 H25 119.5 . . ?
C26 C25 C24 120.9(6) . . ?
C26 C25 H25 119.5 . . ?
C25 C26 H26 119.9 . . ?
C25 C26 C27 120.2(6) . . ?
C27 C26 H26 119.9 . . ?
C22 C27 H27 119.6 . . ?
C26 C27 C22 120.8(6) . . ?
C26 C27 H27 119.6 . . ?
H28A C28 H28B 108.0 . . ?
Cl1 C28 H28A 109.4 . . ?
Cl1 C28 H28B 109.4 . . ?
Cl1 C28 Cl2 111.3(4) . . ?
Cl2 C28 H28A 109.4 . . ?
Cl2 C28 H28B 109.4 . . ?
C8 C9A_a H9AA_a 108.3 . . ?
C8 C9A_a H9AB_a 108.2 . . ?
C8 C9A_a N2A_a 113.5(9) . . ?
H9AA_a C9A_a H9AB_a 109.4 . . ?
N2A_a C9A_a H9AA_a 110.4 . . ?
N2A_a C9A_a H9AB_a 106.9 . . ?
C8 C9B_b H9BA_b 108.3 . . ?
C8 C9B_b H9BB_b 109.1 . . ?
C8 C9B_b N2B_b 114.1(8) . . ?
H9BA_b C9B_b H9BB_b 109.5 . . ?
N2B_b C9B_b H9BA_b 109.5 . . ?
N2B_b C9B_b H9BB_b 106.4 . . ?
C7 N1 C8 120.3(4) . . ?
C7 N1 Ni1 125.5(3) . . ?
C8 N1 Ni1 114.0(3) . . ?
C13B_a N2A_a C9A_a 106.4(10) . . ?
C13B_a N2A_a Ni1 112.6(10) . . ?
C9A_a N2A_a Ni1 102.5(8) . . ?
C10A_a N2A_a C13B_a 105.0(13) . . ?
C10A_a N2A_a C9A_a 108.8(10) . . ?
C10A_a N2A_a Ni1 120.7(9) . . ?
N1 Ni1 C14 131.27(14) . . ?
N1 Ni1 N2A_a 82.4(3) . . ?
N1 Ni1 O1 91.11(13) . . ?
N1 Ni1 O3 101.16(13) . . ?
N1 Ni1 O2 161.00(13) . . ?
N1 Ni1 O4 96.33(13) . . ?
N1 Ni1 N2B_b 83.4(3) . . ?
N2A_a Ni1 C14 93.2(3) . . ?
O1 Ni1 C14 86.95(12) . . ?
O1 Ni1 N2A_a 171.4(3) . . ?
O1 Ni1 O3 91.35(11) . . ?
O1 Ni1 O2 81.70(10) . . ?
O1 Ni1 N2B_b 170.4(3) . . ?
O3 Ni1 C14 30.39(11) . . ?
O3 Ni1 N2A_a 84.5(3) . . ?
O3 Ni1 O2 61.72(10) . . ?
O3 Ni1 N2B_b 97.4(3) . . ?
O2 Ni1 C14 31.35(11) . . ?
O2 Ni1 N2A_a 102.8(3) . . ?
O2 Ni1 N2B_b 105.9(3) . . ?
O4 Ni1 C14 132.32(13) . . ?
O4 Ni1 N2A_a 96.3(3) . . ?
O4 Ni1 O1 89.90(11) . . ?
O4 Ni1 O3 162.44(12) . . ?
O4 Ni1 O2 101.19(11) . . ?
O4 Ni1 N2B_b 83.0(3) . . ?
N2B_b Ni1 C14 102.6(3) . . ?
O1 Ni2 O1 180.0 3_676 . ?
O1 Ni2 O2 98.75(10) 3_676 . ?
O1 Ni2 O2 81.25(10) . . ?
O1 Ni2 O2 98.75(10) . 3_676 ?
O1 Ni2 O2 81.25(10) 3_676 3_676 ?
O2 Ni2 O2 180.0 3_676 . ?
O5 Ni2 O1 90.13(10) . . ?
O5 Ni2 O1 90.14(10) 3_676 3_676 ?
O5 Ni2 O1 89.87(10) 3_676 . ?
O5 Ni2 O1 89.86(10) . 3_676 ?
O5 Ni2 O2 88.24(10) 3_676 3_676 ?
O5 Ni2 O2 91.76(10) 3_676 . ?
O5 Ni2 O2 91.76(10) . 3_676 ?
O5 Ni2 O2 88.24(10) . . ?
O5 Ni2 O5 180.0 3_676 . ?
C1 O1 Ni1 125.9(2) . . ?
C1 O1 Ni2 135.2(2) . . ?
Ni1 O1 Ni2 96.65(11) . . ?
C12A_b O6B_b C11B_b 107(2) . . ?
C14 O3 Ni1 90.3(2) . . ?
C14 O2 Ni1 88.8(2) . . ?
C14 O2 Ni2 120.9(2) . . ?
Ni2 O2 Ni1 90.47(10) . . ?
C21 O4 Ni1 124.6(2) . . ?
C21 O5 Ni2 131.3(2) 3_676 . ?
C29_a Cl3_a C29_a 67.8(17) . 3_577 ?
H13C_b C13A_b H13D_b 107.7 . . ?
C12A_b C13A_b H13C_b 108.9 . . ?
C12A_b C13A_b H13D_b 108.9 . . ?
C12A_b C13A_b N2B_b 113.3(12) . . ?
N2B_b C13A_b H13C_b 108.9 . . ?
N2B_b C13A_b H13D_b 108.9 . . ?
N2A_a C10A_a H10C_a 108.1 . . ?
N2A_a C10A_a H10D_a 108.1 . . ?
N2A_a C10A_a C11A_a 116.8(14) . . ?
H10C_a C10A_a H10D_a 107.3 . . ?
C11A_a C10A_a H10C_a 108.1 . . ?
C11A_a C10A_a H10D_a 108.1 . . ?
O6B_b C12A_b C13A_b 106(2) . . ?
O6B_b C12A_b H12C_b 110.5 . . ?
O6B_b C12A_b H12D_b 110.5 . . ?
C13A_b C12A_b H12C_b 110.5 . . ?
C13A_b C12A_b H12D_b 110.5 . . ?
H12C_b C12A_b H12D_b 108.7 . . ?
C10A_a C11A_a H11C_a 109.3 . . ?
C10A_a C11A_a H11D_a 109.3 . . ?
H11C_a C11A_a H11D_a 108.0 . . ?
O6A_a C11A_a C10A_a 112(2) . . ?
O6A_a C11A_a H11C_a 109.3 . . ?
O6A_a C11A_a H11D_a 109.3 . . ?
C11A_a O6A_a C12B_a 110(2) . . ?
C10B_b N2B_b C9B_b 113.4(12) . . ?
C10B_b N2B_b Ni1 113.3(8) . . ?
C9B_b N2B_b Ni1 97.3(8) . . ?
C13A_b N2B_b C10B_b 110.3(13) . . ?
C13A_b N2B_b C9B_b 106.2(8) . . ?
C13A_b N2B_b Ni1 115.6(10) . . ?
Cl3_a C29_a Cl3_a 112.2(17) . 3_577 ?
Cl3_a C29_a C29_a 54.7(17) 3_577 3_577 ?
Cl3_a C29_a C29_a 57.5(17) . 3_577 ?
Cl3_a C29_a H29A_a 109.1 3_577 . ?
Cl3_a C29_a H29A_a 109.6 . . ?
Cl3_a C29_a H29B_a 108.8 3_577 . ?
Cl3_a C29_a H29B_a 108.9 . . ?
C29_a C29_a H29A_a 126.5 3_577 . ?
C29_a C29_a H29B_a 125.4 3_577 . ?
H29A_a C29_a H29B_a 108.1 . . ?
Cl5 C30 H30A 106.3 . . ?
Cl5 C30 H30B 109.2 . . ?
Cl4 C30 Cl5 114(4) . . ?
Cl4 C30 H30A 109.0 . . ?
Cl4 C30 H30B 109.8 . . ?
H30A C30 H30B 107.8 . . ?

_database_code_depnum_ccdc_archive 'CCDC 986871'
#######################################################################
#
#                 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_986872

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H60 Cl4 N6 Ni3 O14'
_chemical_formula_weight         1383.05

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                   11.2050(18)
_cell_length_b                   12.005(2)
_cell_length_c                   13.346(2)
_cell_angle_alpha                107.023(5)
_cell_angle_beta                 103.618(6)
_cell_angle_gamma                104.109(5)
_cell_volume                     1571.0(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.77
_cell_measurement_theta_max      25.18

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             714
_exptl_absorpt_coefficient_mu    1.127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7897
_exptl_absorpt_correction_T_max  0.8229
_exptl_absorpt_process_details   'SADABS (Sheldrick 2008)'

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18341
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         25.30
_reflns_number_total             5675
_reflns_number_gt                4626
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+1.2058P] 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         5675
_refine_ls_number_parameters     395
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0482
_refine_ls_wR_factor_ref         0.1619
_refine_ls_wR_factor_gt          0.1503
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.1166(4) 0.7959(3) 0.5273(3) 0.0488(8) Uani 1 1 d . . .
C2 C 1.2062(4) 0.8266(4) 0.4738(4) 0.0576(10) Uani 1 1 d . . .
H2 H 1.2081 0.8915 0.4489 0.069 Uiso 1 1 calc R . .
C3 C 1.2918(5) 0.7632(4) 0.4571(4) 0.0724(12) Uani 1 1 d . . .
H3 H 1.3508 0.7862 0.4221 0.087 Uiso 1 1 calc R . .
C4 C 1.2897(5) 0.6655(5) 0.4923(5) 0.0812(14) Uani 1 1 d . . .
H4 H 1.3469 0.6223 0.4805 0.097 Uiso 1 1 calc R . .
C5 C 1.2047(5) 0.6330(5) 0.5438(5) 0.0796(14) Uani 1 1 d . . .
H5 H 1.2040 0.5668 0.5667 0.096 Uiso 1 1 calc R . .
C6 C 1.1162(4) 0.6963(4) 0.5641(4) 0.0581(10) Uani 1 1 d . . .
C7 C 1.0319(5) 0.6554(4) 0.6223(4) 0.0669(11) Uani 1 1 d . . .
H7 H 1.0348 0.5845 0.6364 0.080 Uiso 1 1 calc R . .
C8 C 0.8810(6) 0.6565(5) 0.7194(5) 0.0844(16) Uani 1 1 d . . .
H8A H 0.9198 0.6040 0.7491 0.101 Uiso 1 1 calc R . .
H8B H 0.7917 0.6080 0.6724 0.101 Uiso 1 1 calc R . .
C9 C 0.8845(6) 0.7658(5) 0.8123(4) 0.0773(14) Uani 1 1 d . . .
H9A H 0.8332 0.7371 0.8547 0.093 Uiso 1 1 calc R . .
H9B H 0.9737 0.8100 0.8617 0.093 Uiso 1 1 calc R . .
C10 C 0.6870(5) 0.7974(5) 0.7187(4) 0.0733(13) Uani 1 1 d . . .
H10A H 0.6636 0.7259 0.6513 0.088 Uiso 1 1 calc R . .
H10B H 0.6508 0.7698 0.7699 0.088 Uiso 1 1 calc R . .
C11 C 0.6302(5) 0.8886(7) 0.6921(5) 0.0945(17) Uani 1 1 d . . .
H11A H 0.6643 0.9142 0.6390 0.113 Uiso 1 1 calc R . .
H11B H 0.5364 0.8501 0.6583 0.113 Uiso 1 1 calc R . .
C12 C 0.7962(6) 1.0520(5) 0.8328(5) 0.0870(15) Uani 1 1 d . . .
H12A H 0.8181 1.1263 0.8972 0.104 Uiso 1 1 calc R . .
H12B H 0.8273 1.0762 0.7777 0.104 Uiso 1 1 calc R . .
C13 C 0.8634(5) 0.9674(4) 0.8657(4) 0.0682(11) Uani 1 1 d . . .
H13A H 0.9570 1.0098 0.8951 0.082 Uiso 1 1 calc R . .
H13B H 0.8361 0.9470 0.9238 0.082 Uiso 1 1 calc R . .
C14 C 0.6058(3) 0.7488(3) 0.3510(3) 0.0462(8) Uani 1 1 d . . .
C15 C 0.5291(4) 0.6269(4) 0.3216(4) 0.0579(10) Uani 1 1 d . . .
C16 C 0.4097(4) 0.5757(5) 0.2374(4) 0.0782(14) Uani 1 1 d . . .
H16 H 0.3594 0.4938 0.2185 0.094 Uiso 1 1 calc R . .
C17 C 0.3658(5) 0.6438(6) 0.1824(4) 0.0864(16) Uani 1 1 d . . .
H17 H 0.2853 0.6083 0.1261 0.104 Uiso 1 1 calc R . .
C18 C 0.4381(5) 0.7643(5) 0.2084(4) 0.0802(14) Uani 1 1 d . . .
H18 H 0.4075 0.8108 0.1703 0.096 Uiso 1 1 calc R . .
C19 C 0.5582(4) 0.8161(4) 0.2928(4) 0.0606(10) Uani 1 1 d . . .
H19 H 0.6078 0.8979 0.3106 0.073 Uiso 1 1 calc R . .
C20 C 0.7378(3) 0.8136(3) 0.4394(3) 0.0452(8) Uani 1 1 d . . .
C21 C 1.1553(4) 1.2126(4) 0.7995(3) 0.0625(10) Uani 1 1 d . . .
C22 C 1.2652(4) 1.2677(4) 0.8956(3) 0.0625(11) Uani 1 1 d . . .
C23 C 1.3305(6) 1.3924(5) 0.9368(5) 0.0971(18) Uani 1 1 d . . .
H23 H 1.4010 1.4273 1.0025 0.117 Uiso 1 1 calc R . .
C24 C 1.2953(7) 1.4663(6) 0.8846(6) 0.115(2) Uani 1 1 d . . .
H24 H 1.3452 1.5494 0.9096 0.137 Uiso 1 1 calc R . .
C25 C 1.1843(7) 1.4153(5) 0.7941(5) 0.108(2) Uani 1 1 d . . .
H25 H 1.1554 1.4668 0.7616 0.129 Uiso 1 1 calc R . .
C26 C 1.1133(6) 1.2907(4) 0.7492(4) 0.0795(14) Uani 1 1 d . . .
H26 H 1.0389 1.2588 0.6868 0.095 Uiso 1 1 calc R . .
C27 C 1.0773(4) 1.0810(4) 0.7444(3) 0.0583(10) Uani 1 1 d . . .
C28 C 0.3050(10) 0.8179(11) 0.8726(8) 0.147(3) Uani 1 1 d . . .
C29 C 0.3757(9) 0.8883(10) 0.8283(8) 0.167(4) Uani 1 1 d . . .
H29A H 0.4121 0.8389 0.7820 0.250 Uiso 1 1 calc R . .
H29B H 0.4449 0.9572 0.8872 0.250 Uiso 1 1 calc R . .
H29C H 0.3198 0.9183 0.7847 0.250 Uiso 1 1 calc R . .
Cl1 Cl 0.57618(15) 0.53162(12) 0.38529(14) 0.0978(5) Uani 1 1 d . . .
Cl2 Cl 1.32444(15) 1.18483(16) 0.96826(12) 0.1036(5) Uani 1 1 d . . .
N1 N 0.9551(4) 0.7051(3) 0.6559(3) 0.0604(9) Uani 1 1 d . . .
N2 N 0.8324(3) 0.8511(3) 0.7692(3) 0.0537(8) Uani 1 1 d . . .
N3 N 0.2401(11) 0.7586(10) 0.9080(8) 0.185(4) Uani 1 1 d . . .
Ni1 Ni 0.93400(4) 0.86114(4) 0.64724(4) 0.04448(17) Uani 1 1 d . . .
Ni2 Ni 1.0000 1.0000 0.5000 0.04084(19) Uani 1 2 d S . .
O1 O 1.0349(2) 0.8564(2) 0.5404(2) 0.0487(6) Uani 1 1 d . . .
O2 O 0.9762(2) 1.0470(2) 0.65955(19) 0.0442(5) Uani 1 1 d . . .
O3 O 1.1050(3) 0.9996(3) 0.7810(3) 0.0697(8) Uani 1 1 d . . .
O4 O 0.7632(2) 0.7798(3) 0.5198(2) 0.0559(7) Uani 1 1 d . . .
O5 O 0.8108(2) 0.9013(2) 0.4262(2) 0.0493(6) Uani 1 1 d . . .
O6 O 0.6597(4) 0.9941(4) 0.7888(4) 0.0987(12) Uani 1 1 d . . .
O7A O 0.012(2) 0.3958(14) 0.008(2) 0.193(8) Uani 0.60 1 d PD . .
O7B O 0.0108(19) 0.434(2) 0.009(3) 0.25(3) Uani 0.40 1 d PD . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.311(4) . ?
C1 C2 1.401(5) . ?
C1 C6 1.419(5) . ?
C2 C3 1.380(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.383(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.348(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.417(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.442(6) . ?
C7 N1 1.254(6) . ?
C7 H7 0.9300 . ?
C8 N1 1.460(5) . ?
C8 C9 1.503(7) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.483(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.480(8) . ?
C10 N2 1.496(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 O6 1.420(7) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 O6 1.410(7) . ?
C12 C13 1.506(7) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.492(5) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C19 1.387(5) . ?
C14 C15 1.389(5) . ?
C14 C20 1.505(5) . ?
C15 C16 1.384(6) . ?
C15 Cl1 1.720(4) . ?
C16 C17 1.353(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.368(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.391(6) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 O5 1.251(4) . ?
C20 O4 1.252(4) . ?
C21 C22 1.400(6) . ?
C21 C26 1.410(7) . ?
C21 C27 1.464(6) . ?
C22 C23 1.368(7) . ?
C22 Cl2 1.719(5) . ?
C23 C24 1.353(9) . ?
C23 H23 0.9300 . ?
C24 C25 1.367(9) . ?
C24 H24 0.9300 . ?
C25 C26 1.378(7) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 O2 1.278(5) . ?
C27 O3 1.283(5) . ?
C27 Ni1 2.485(4) . ?
C28 N3 1.168(13) . ?
C28 C29 1.371(14) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
N1 Ni1 1.977(3) . ?
N2 Ni1 2.210(3) . ?
Ni1 O1 2.014(2) . ?
Ni1 O4 2.023(3) . ?
Ni1 O2 2.112(2) . ?
Ni1 O3 2.173(3) . ?
Ni2 O5 1.994(2) . ?
Ni2 O5 1.994(2) 2_776 ?
Ni2 O1 2.047(2) 2_776 ?
Ni2 O1 2.047(2) . ?
Ni2 O2 2.136(2) . ?
Ni2 O2 2.136(2) 2_776 ?
O7B O7B 1.74(4) 2_565 ?

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 C1 C2 120.6(3) . . ?
O1 C1 C6 121.8(3) . . ?
C2 C1 C6 117.6(4) . . ?
C3 C2 C1 121.9(4) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
C2 C3 C4 120.1(4) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 119.8(4) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 122.2(4) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C5 C6 C1 118.5(4) . . ?
C5 C6 C7 117.3(4) . . ?
C1 C6 C7 124.2(4) . . ?
N1 C7 C6 127.1(4) . . ?
N1 C7 H7 116.5 . . ?
C6 C7 H7 116.5 . . ?
N1 C8 C9 107.1(4) . . ?
N1 C8 H8A 110.3 . . ?
C9 C8 H8A 110.3 . . ?
N1 C8 H8B 110.3 . . ?
C9 C8 H8B 110.3 . . ?
H8A C8 H8B 108.6 . . ?
N2 C9 C8 111.3(4) . . ?
N2 C9 H9A 109.4 . . ?
C8 C9 H9A 109.4 . . ?
N2 C9 H9B 109.4 . . ?
C8 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
C11 C10 N2 111.6(4) . . ?
C11 C10 H10A 109.3 . . ?
N2 C10 H10A 109.3 . . ?
C11 C10 H10B 109.3 . . ?
N2 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
O6 C11 C10 111.4(4) . . ?
O6 C11 H11A 109.3 . . ?
C10 C11 H11A 109.3 . . ?
O6 C11 H11B 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
O6 C12 C13 111.5(4) . . ?
O6 C12 H12A 109.3 . . ?
C13 C12 H12A 109.3 . . ?
O6 C12 H12B 109.3 . . ?
C13 C12 H12B 109.3 . . ?
H12A C12 H12B 108.0 . . ?
N2 C13 C12 111.4(4) . . ?
N2 C13 H13A 109.3 . . ?
C12 C13 H13A 109.3 . . ?
N2 C13 H13B 109.3 . . ?
C12 C13 H13B 109.3 . . ?
H13A C13 H13B 108.0 . . ?
C19 C14 C15 117.4(4) . . ?
C19 C14 C20 117.1(3) . . ?
C15 C14 C20 125.5(3) . . ?
C16 C15 C14 120.7(4) . . ?
C16 C15 Cl1 116.6(3) . . ?
C14 C15 Cl1 122.7(3) . . ?
C17 C16 C15 120.5(4) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C17 C18 120.9(4) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C17 C18 C19 118.9(5) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
C14 C19 C18 121.6(4) . . ?
C14 C19 H19 119.2 . . ?
C18 C19 H19 119.2 . . ?
O5 C20 O4 126.1(3) . . ?
O5 C20 C14 115.1(3) . . ?
O4 C20 C14 118.8(3) . . ?
C22 C21 C26 117.5(4) . . ?
C22 C21 C27 127.1(4) . . ?
C26 C21 C27 115.4(4) . . ?
C23 C22 C21 120.8(5) . . ?
C23 C22 Cl2 116.6(4) . . ?
C21 C22 Cl2 122.6(3) . . ?
C24 C23 C22 121.7(6) . . ?
C24 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
C23 C24 C25 118.1(6) . . ?
C23 C24 H24 120.9 . . ?
C25 C24 H24 120.9 . . ?
C24 C25 C26 122.8(6) . . ?
C24 C25 H25 118.6 . . ?
C26 C25 H25 118.6 . . ?
C25 C26 C21 118.8(5) . . ?
C25 C26 H26 120.6 . . ?
C21 C26 H26 120.6 . . ?
O2 C27 O3 119.1(4) . . ?
O2 C27 C21 118.9(4) . . ?
O3 C27 C21 122.0(4) . . ?
O2 C27 Ni1 58.19(19) . . ?
O3 C27 Ni1 60.9(2) . . ?
C21 C27 Ni1 176.7(3) . . ?
N3 C28 C29 177.1(12) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C7 N1 C8 120.7(4) . . ?
C7 N1 Ni1 126.4(3) . . ?
C8 N1 Ni1 112.6(3) . . ?
C9 N2 C13 107.6(3) . . ?
C9 N2 C10 110.4(4) . . ?
C13 N2 C10 107.2(3) . . ?
C9 N2 Ni1 99.9(2) . . ?
C13 N2 Ni1 117.5(2) . . ?
C10 N2 Ni1 113.8(3) . . ?
N1 Ni1 O1 90.06(12) . . ?
N1 Ni1 O4 95.61(14) . . ?
O1 Ni1 O4 90.95(11) . . ?
N1 Ni1 O2 161.86(13) . . ?
O1 Ni1 O2 81.70(10) . . ?
O4 Ni1 O2 100.63(10) . . ?
N1 Ni1 O3 102.16(14) . . ?
O1 Ni1 O3 90.19(11) . . ?
O4 Ni1 O3 162.19(12) . . ?
O2 Ni1 O3 61.98(11) . . ?
N1 Ni1 N2 83.83(13) . . ?
O1 Ni1 N2 173.62(11) . . ?
O4 Ni1 N2 91.47(12) . . ?
O2 Ni1 N2 103.64(11) . . ?
O3 Ni1 N2 89.31(12) . . ?
N1 Ni1 C27 132.64(15) . . ?
O1 Ni1 C27 85.09(12) . . ?
O4 Ni1 C27 131.48(13) . . ?
O2 Ni1 C27 30.93(11) . . ?
O3 Ni1 C27 31.05(12) . . ?
N2 Ni1 C27 97.70(13) . . ?
O5 Ni2 O5 180.0 . 2_776 ?
O5 Ni2 O1 89.34(10) . 2_776 ?
O5 Ni2 O1 90.66(10) 2_776 2_776 ?
O5 Ni2 O1 90.66(10) . . ?
O5 Ni2 O1 89.34(10) 2_776 . ?
O1 Ni2 O1 180.00(14) 2_776 . ?
O5 Ni2 O2 91.13(10) . . ?
O5 Ni2 O2 88.87(10) 2_776 . ?
O1 Ni2 O2 99.62(9) 2_776 . ?
O1 Ni2 O2 80.38(9) . . ?
O5 Ni2 O2 88.87(10) . 2_776 ?
O5 Ni2 O2 91.13(10) 2_776 2_776 ?
O1 Ni2 O2 80.38(9) 2_776 2_776 ?
O1 Ni2 O2 99.62(9) . 2_776 ?
O2 Ni2 O2 179.998(1) . 2_776 ?
C1 O1 Ni1 126.9(2) . . ?
C1 O1 Ni2 134.9(2) . . ?
Ni1 O1 Ni2 96.56(10) . . ?
C27 O2 Ni1 90.9(2) . . ?
C27 O2 Ni2 117.8(2) . . ?
Ni1 O2 Ni2 91.06(9) . . ?
C27 O3 Ni1 88.1(2) . . ?
C20 O4 Ni1 123.4(2) . . ?
C20 O5 Ni2 132.4(2) . . ?
C12 O6 C11 108.1(4) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.30
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.076
_database_code_depnum_ccdc_archive 'CCDC 986872'
