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

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

data_comp1_rev
_database_code_depnum_ccdc_archive 'CCDC 1448720'
_audit_update_record             
;
2016-05-20 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;

# ========================================================================= #

_audit_creation_method           'SHELXL-2014/7 and enCIFer'
_shelx_SHELXL_version_number     2014/7
_audit_creation_date             '19 May 2016'

# ========================================================================= #

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C77 H58 Cl4 N4 Ni5 O17, 5(C H4 O), 2(C6 H14)'
_chemical_formula_sum            'C94 H106 Cl4 N4 Ni5 O22'
_chemical_formula_weight         2079.17

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.472(2)
_cell_length_b                   14.473(2)
_cell_length_c                   24.048(4)
_cell_angle_alpha                101.736(8)
_cell_angle_beta                 96.477(8)
_cell_angle_gamma                116.529(7)
_cell_volume                     4291.5(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9189
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      29.61

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_F_000             2164
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.282
_shelx_estimated_absorpt_T_min   0.883
_shelx_estimated_absorpt_T_max   0.939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_process_details   
; 
'SADABS V2012/1 (Bruker AXS Inc.)' 
;


_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            110715
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.639
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992


_reflns_number_total             16187
_reflns_number_gt                13656
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 (Bruker AXS Inc., 2012)'
_computing_cell_refinement       'SAINT (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT (Bruker AXS Inc., 2012)'
_computing_structure_solution    'SHELXS (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2014)'


_refine_special_details          
;
 All non-hydrogen atoms were refined anisotropically.
 
 Hydrogen atoms were placed geometrically on the carbon atoms and refined
 with a riding model.
 
 Hydrogen atoms on the methanol molecules molecules were found
 in the Fourier difference map, their distance fixed, and refined with 
 a riding model.
 
 The cell contains a void with a considerable number of solvent molecules. 
 Four MeOH solvent molecules were unequivocally identified and refined,
 and the attempts to model and refine the remaining solvent molecules in the
 overlapping electronic density revealed to be unsuccessful. It was not possible
 to found a model chemically reasonable. Consequently, the residual density
 was processed with the solvent-masking procedure [PLATON SQUEEZE; Reference to 
 van der Sluis, P. & Spek, A. L., Acta Cryst. 1990, A46, 194-201] indicating 
 118 electrons per formula unit. This value as assigned to one MeOH 
 (18 electrons) and two hexane (C6H14; 50 electrons) molecules, which 
 were considered in the molecular formula of the compound and 
 in the final refinement cycles.
;


# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: The ratio of given/expected molecular weight as
         calculated from the _atom_site* data lies outside
         the range 0.90 <> 1.10
RESPONSE: One MeOH and two hexane molecules have been estimated 
          after SQUEEZE use; these molecules were not modelated
          but were considered in the final formula of the compound
;
# end Validation Reply Form

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0714P)²+31.3910P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16187
_refine_ls_number_parameters     1058
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0657
_refine_ls_wR_factor_ref         0.1623
_refine_ls_wR_factor_gt          0.1539
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_restrained_S_all      0.935
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.31569(4) 0.49128(4) 0.24062(2) 0.01493(14) Uani 1 1 d . . . . .
Ni2 Ni 0.13517(4) 0.27958(4) 0.16562(2) 0.01514(14) Uani 1 1 d . . . . .
Ni3 Ni 0.28076(5) 0.53553(5) 0.36004(3) 0.01843(15) Uani 1 1 d . . . . .
Ni4 Ni 0.47223(4) 0.71196(5) 0.32229(3) 0.01566(14) Uani 1 1 d . . . . .
Ni5 Ni 0.30239(5) 0.43465(5) 0.10756(3) 0.01704(14) Uani 1 1 d . . . . .
Cl1 Cl 0.88243(14) 0.57574(13) 0.39058(9) 0.0536(5) Uani 1 1 d . . . . .
Cl2 Cl -0.00866(11) -0.01481(10) 0.36028(6) 0.0323(3) Uani 1 1 d . . . . .
Cl3 Cl 0.63858(15) 0.96713(16) 0.09962(9) 0.0769(8) Uani 1 1 d . . . . .
Cl4 Cl -0.23598(14) 0.47546(15) 0.20334(9) 0.0556(5) Uani 1 1 d . . . . .
O1 O 0.2962(2) 0.3644(2) 0.17330(13) 0.0168(7) Uani 1 1 d . . . . .
O2 O 0.1543(2) 0.4235(2) 0.21772(14) 0.0170(7) Uani 1 1 d . . . . .
O3 O 0.1163(3) 0.4476(3) 0.30701(15) 0.0248(8) Uani 1 1 d . . . . .
O4 O 0.3140(2) 0.6159(2) 0.29921(14) 0.0172(7) Uani 1 1 d . . . . .
O5 O 0.4752(2) 0.5748(2) 0.27987(14) 0.0170(7) Uani 1 1 d . . . . .
O6 O 0.5673(3) 0.5191(3) 0.22673(15) 0.0267(8) Uani 1 1 d . . . . .
O7 O 0.4718(3) 0.8499(3) 0.35736(15) 0.0212(7) Uani 1 1 d . . . . .
O8 O 0.4369(3) 0.6445(3) 0.39329(14) 0.0208(7) Uani 1 1 d . . . . .
O9 O 0.2940(2) 0.4131(2) 0.30403(14) 0.0174(7) Uani 1 1 d . . . . .
O10 O 0.1706(3) 0.2508(3) 0.24546(14) 0.0200(7) Uani 1 1 d . . . . .
O11 O 0.4610(3) 0.7331(3) 0.23315(14) 0.0217(7) Uani 1 1 d . . . . .
O12 O 0.3349(3) 0.5679(3) 0.17848(14) 0.0200(7) Uani 1 1 d . . . . .
O13 O 0.1437(3) 0.3466(3) 0.09507(14) 0.0202(7) Uani 1 1 d . . . . .
O14 O 0.4675(3) 0.5070(3) 0.12514(16) 0.0262(8) Uani 1 1 d D . . . .
H14E H 0.486(5) 0.510(5) 0.1603(12) 0.039 Uiso 1 1 d D U . . .
O15 O 0.3016(3) 0.3204(3) 0.03886(16) 0.0283(8) Uani 1 1 d D . . . .
H15E H 0.276(5) 0.257(2) 0.042(3) 0.042 Uiso 1 1 d D U . . .
O16 O 0.2335(3) 0.6276(3) 0.41167(18) 0.0372(10) Uani 1 1 d D . . . .
H16E H 0.269(5) 0.6959(17) 0.421(3) 0.056 Uiso 1 1 d D U . . .
O17 O 0.1083(3) 0.1328(3) 0.12343(14) 0.0209(7) Uani 1 1 d . . . . .
N1 N 0.6315(3) 0.7950(3) 0.34204(17) 0.0170(8) Uani 1 1 d . . . . .
N2 N 0.2911(3) 0.4559(3) 0.41861(17) 0.0210(9) Uani 1 1 d . . . . .
N3 N 0.2817(3) 0.5277(3) 0.06151(17) 0.0217(9) Uani 1 1 d . . . . .
N4 N -0.0209(3) 0.2102(3) 0.16864(17) 0.0180(8) Uani 1 1 d . . . . .
C1 C 0.0910(4) 0.4177(4) 0.2520(2) 0.0209(10) Uani 1 1 d . . . . .
C2 C 0.5600(4) 0.5725(4) 0.2718(2) 0.0171(10) Uani 1 1 d . . . . .
C3 C 0.6568(4) 0.6353(4) 0.3212(2) 0.0174(10) Uani 1 1 d . . . . .
C4 C 0.6926(4) 0.7430(4) 0.3544(2) 0.0165(9) Uani 1 1 d . . . . .
C5 C 0.6848(4) 0.8970(4) 0.3448(2) 0.0176(10) Uani 1 1 d . . . . .
H5 H 0.7587 0.9256 0.3469 0.021 Uiso 1 1 calc R U . . .
C6 C 0.6432(4) 0.9694(4) 0.3451(2) 0.0165(9) Uani 1 1 d . . . . .
C7 C 0.5421(4) 0.9452(4) 0.3563(2) 0.0212(10) Uani 1 1 d . . . . .
C8 C 0.5160(4) 1.0309(4) 0.3694(2) 0.0297(12) Uani 1 1 d . . . . .
H8 H 0.4492 1.0157 0.3780 0.036 Uiso 1 1 calc R U . . .
C9 C 0.5836(5) 1.1323(4) 0.3697(3) 0.0339(13) Uani 1 1 d . . . . .
H9 H 0.5637 1.1867 0.3796 0.041 Uiso 1 1 calc R U . . .
C10 C 0.6832(5) 1.1598(4) 0.3558(3) 0.0333(13) Uani 1 1 d . . . . .
C11 C 0.7143(4) 1.0781(4) 0.3420(2) 0.0229(11) Uani 1 1 d . . . . .
C12 C 0.8124(4) 1.1070(4) 0.3260(3) 0.0304(12) Uani 1 1 d . . . . .
H12 H 0.8339 1.0540 0.3152 0.036 Uiso 1 1 calc R U . . .
C13 C 0.8777(5) 1.2120(5) 0.3258(3) 0.0457(16) Uani 1 1 d . . . . .
H13 H 0.9438 1.2302 0.3154 0.055 Uiso 1 1 calc R U . . .
C14 C 0.8479(6) 1.2916(5) 0.3407(4) 0.0520(19) Uani 1 1 d . . . . .
H14 H 0.8937 1.3635 0.3409 0.062 Uiso 1 1 calc R U . . .
C15 C 0.7533(6) 1.2656(5) 0.3548(3) 0.0493(18) Uani 1 1 d . . . . .
H15 H 0.7332 1.3200 0.3643 0.059 Uiso 1 1 calc R U . . .
C16 C 0.7859(4) 0.7963(4) 0.3980(2) 0.0203(10) Uani 1 1 d . . . . .
H16 H 0.8085 0.8676 0.4209 0.024 Uiso 1 1 calc R U . . .
C17 C 0.8459(4) 0.7466(4) 0.4082(2) 0.0285(12) Uani 1 1 d . . . . .
H17 H 0.9111 0.7843 0.4369 0.034 Uiso 1 1 calc R U . . .
C18 C 0.8094(4) 0.6410(4) 0.3761(2) 0.0291(12) Uani 1 1 d . . . . .
C19 C 0.7176(4) 0.5856(4) 0.3325(2) 0.0232(11) Uani 1 1 d . . . . .
H19 H 0.6958 0.5140 0.3103 0.028 Uiso 1 1 calc R U . . .
C20 C 0.4818(4) 0.6774(4) 0.4490(2) 0.0225(11) Uani 1 1 d . . . . .
C21 C 0.4461(4) 0.6138(4) 0.4873(2) 0.0217(10) Uani 1 1 d . . . . .
C22 C 0.3659(4) 0.5011(4) 0.4658(2) 0.0209(10) Uani 1 1 d . . . . .
H22 H 0.3686 0.4557 0.4887 0.025 Uiso 1 1 calc R U . . .
C23 C 0.2210(4) 0.3417(4) 0.4047(2) 0.0208(10) Uani 1 1 d . . . . .
C24 C 0.1856(4) 0.2774(4) 0.3465(2) 0.0180(10) Uani 1 1 d . . . . .
C25 C 0.2185(4) 0.3161(4) 0.2944(2) 0.0160(9) Uani 1 1 d . . . . .
C26 C 0.1147(4) 0.1674(4) 0.3333(2) 0.0200(10) Uani 1 1 d . . . . .
H26 H 0.0896 0.1234 0.2940 0.024 Uiso 1 1 calc R U . . .
C27 C 0.0811(4) 0.1229(4) 0.3779(2) 0.0235(11) Uani 1 1 d . . . . .
C28 C 0.1147(4) 0.1844(4) 0.4352(2) 0.0307(12) Uani 1 1 d . . . . .
H28 H 0.0910 0.1525 0.4652 0.037 Uiso 1 1 calc R U . . .
C29 C 0.1839(5) 0.2938(5) 0.4483(2) 0.0334(13) Uani 1 1 d . . . . .
H29 H 0.2066 0.3372 0.4876 0.040 Uiso 1 1 calc R U . . .
C30 C 0.4980(4) 0.6575(4) 0.5491(2) 0.0205(10) Uani 1 1 d . . . . .
C31 C 0.5869(4) 0.7640(4) 0.5701(2) 0.0231(11) Uani 1 1 d . . . . .
C32 C 0.6220(4) 0.8236(4) 0.5296(2) 0.0238(11) Uani 1 1 d . . . . .
H32 H 0.6817 0.8938 0.5430 0.029 Uiso 1 1 calc R U . . .
C33 C 0.5722(4) 0.7826(4) 0.4720(2) 0.0230(11) Uani 1 1 d . . . . .
H33 H 0.5983 0.8249 0.4463 0.028 Uiso 1 1 calc R U . . .
C34 C 0.6353(4) 0.8097(4) 0.6309(2) 0.0262(11) Uani 1 1 d . . . . .
H34 H 0.6930 0.8811 0.6444 0.031 Uiso 1 1 calc R U . . .
C35 C 0.6008(5) 0.7536(5) 0.6703(2) 0.0308(12) Uani 1 1 d . . . . .
H35 H 0.6344 0.7850 0.7107 0.037 Uiso 1 1 calc R U . . .
C36 C 0.5150(5) 0.6490(5) 0.6499(2) 0.0328(13) Uani 1 1 d . . . . .
H36 H 0.4909 0.6090 0.6769 0.039 Uiso 1 1 calc R U . . .
C37 C 0.4650(4) 0.6028(4) 0.5919(2) 0.0286(12) Uani 1 1 d . . . . .
H37 H 0.4063 0.5319 0.5799 0.034 Uiso 1 1 calc R U . . .
C38 C 0.4065(4) 0.6653(4) 0.1850(2) 0.0202(10) Uani 1 1 d . . . . .
C39 C 0.0738(4) 0.3313(4) 0.0499(2) 0.0200(10) Uani 1 1 d . . . . .
C40 C 0.0944(4) 0.4018(4) 0.0140(2) 0.0195(10) Uani 1 1 d . . . . .
C41 C 0.1915(4) 0.5022(4) 0.0283(2) 0.0222(10) Uani 1 1 d . . . . .
H41 H 0.1895 0.5556 0.0116 0.027 Uiso 1 1 calc R U . . .
C42 C 0.3670(4) 0.6343(4) 0.0724(2) 0.0236(11) Uani 1 1 d . . . . .
C43 C 0.4263(4) 0.6999(4) 0.1297(2) 0.0213(10) Uani 1 1 d . . . . .
C44 C 0.5089(4) 0.8023(4) 0.1373(3) 0.0306(12) Uani 1 1 d . . . . .
H44 H 0.5485 0.8475 0.1755 0.037 Uiso 1 1 calc R U . . .
C45 C 0.5339(5) 0.8388(5) 0.0891(3) 0.0404(16) Uani 1 1 d . . . . .
C46 C 0.4775(5) 0.7750(5) 0.0331(3) 0.0430(16) Uani 1 1 d . . . . .
H46 H 0.4959 0.8010 0.0005 0.052 Uiso 1 1 calc R U . . .
C47 C 0.3942(5) 0.6732(5) 0.0248(3) 0.0353(14) Uani 1 1 d . . . . .
H47 H 0.3550 0.6292 -0.0137 0.042 Uiso 1 1 calc R U . . .
C48 C 0.0110(4) 0.3783(4) -0.0350(2) 0.0256(11) Uani 1 1 d . . . . .
C49 C -0.0912(4) 0.2894(4) -0.0450(2) 0.0263(11) Uani 1 1 d . . . . .
C50 C -0.1079(4) 0.2214(5) -0.0083(2) 0.0312(12) Uani 1 1 d . . . . .
H50 H -0.1761 0.1608 -0.0151 0.037 Uiso 1 1 calc R U . . .
C51 C -0.0287(4) 0.2399(4) 0.0367(2) 0.0241(11) Uani 1 1 d . . . . .
H51 H -0.0428 0.1908 0.0595 0.029 Uiso 1 1 calc R U . . .
C52 C -0.1736(5) 0.2666(5) -0.0922(2) 0.0329(13) Uani 1 1 d . . . . .
H52 H -0.2418 0.2063 -0.0984 0.039 Uiso 1 1 calc R U . . .
C53 C -0.1559(5) 0.3305(5) -0.1288(2) 0.0391(15) Uani 1 1 d . . . . .
H53 H -0.2118 0.3151 -0.1600 0.047 Uiso 1 1 calc R U . . .
C54 C -0.0557(5) 0.4182(5) -0.1202(3) 0.0388(14) Uani 1 1 d . . . . .
H54 H -0.0438 0.4626 -0.1457 0.047 Uiso 1 1 calc R U . . .
C55 C 0.0266(5) 0.4414(5) -0.0751(2) 0.0318(13) Uani 1 1 d . . . . .
H55 H 0.0948 0.5005 -0.0707 0.038 Uiso 1 1 calc R U . . .
C56 C 0.5316(6) 0.4956(8) 0.0870(3) 0.075(3) Uani 1 1 d . . . . .
H56A H 0.5194 0.4214 0.0771 0.112 Uiso 1 1 calc R U . . .
H56B H 0.6065 0.5451 0.1061 0.112 Uiso 1 1 calc R U . . .
H56C H 0.5133 0.5126 0.0513 0.112 Uiso 1 1 calc R U . . .
C57 C 0.2793(6) 0.3146(5) -0.0214(2) 0.0421(15) Uani 1 1 d . . . . .
H57A H 0.2025 0.2825 -0.0362 0.063 Uiso 1 1 calc R U . . .
H57B H 0.3054 0.2701 -0.0435 0.063 Uiso 1 1 calc R U . . .
H57C H 0.3149 0.3873 -0.0260 0.063 Uiso 1 1 calc R U . . .
C58 C 0.2515(4) 0.6630(4) 0.2801(2) 0.0249(11) Uani 1 1 d . . . . .
H58A H 0.2128 0.6734 0.3097 0.037 Uiso 1 1 calc R U . . .
H58B H 0.2007 0.6150 0.2431 0.037 Uiso 1 1 calc R U . . .
H58C H 0.2984 0.7328 0.2746 0.037 Uiso 1 1 calc R U . . .
C59 C 0.1568(8) 0.5935(7) 0.4444(5) 0.080(3) Uani 1 1 d . . . . .
H59A H 0.1104 0.5154 0.4289 0.120 Uiso 1 1 calc R U . . .
H59B H 0.1143 0.6302 0.4420 0.120 Uiso 1 1 calc R U . . .
H59C H 0.1920 0.6109 0.4853 0.120 Uiso 1 1 calc R U . . .
C60 C -0.0213(4) 0.3737(4) 0.2196(2) 0.0234(11) Uani 1 1 d . . . . .
C61 C -0.0727(4) 0.2737(4) 0.1764(2) 0.0200(10) Uani 1 1 d . . . . .
C62 C -0.0730(4) 0.1111(4) 0.1704(2) 0.0178(10) Uani 1 1 d . . . . .
H62 H -0.1417 0.0890 0.1779 0.021 Uiso 1 1 calc R U . . .
C63 C -0.0387(4) 0.0313(4) 0.1623(2) 0.0173(10) Uani 1 1 d . . . . .
C64 C 0.0507(4) 0.0469(4) 0.1392(2) 0.0195(10) Uani 1 1 d . . . . .
C65 C 0.0812(4) -0.0361(4) 0.1314(2) 0.0285(12) Uani 1 1 d . . . . .
H65 H 0.1416 -0.0263 0.1161 0.034 Uiso 1 1 calc R U . . .
C66 C 0.0249(5) -0.1275(4) 0.1457(2) 0.0301(12) Uani 1 1 d . . . . .
H66 H 0.0477 -0.1802 0.1408 0.036 Uiso 1 1 calc R U . . .
C67 C -0.0668(4) -0.1482(4) 0.1678(2) 0.0239(11) Uani 1 1 d . . . . .
C68 C -0.1011(4) -0.0688(4) 0.1760(2) 0.0212(10) Uani 1 1 d . . . . .
C69 C -0.1937(4) -0.0931(4) 0.1975(2) 0.0236(11) Uani 1 1 d . . . . .
H69 H -0.2185 -0.0419 0.2033 0.028 Uiso 1 1 calc R U . . .
C70 C -0.2494(4) -0.1900(4) 0.2102(2) 0.0276(12) Uani 1 1 d . . . . .
H70 H -0.3117 -0.2044 0.2244 0.033 Uiso 1 1 calc R U . . .
C71 C -0.2143(5) -0.2664(4) 0.2023(3) 0.0327(13) Uani 1 1 d . . . . .
H71 H -0.2523 -0.3324 0.2113 0.039 Uiso 1 1 calc R U . . .
C72 C -0.1253(5) -0.2459(4) 0.1815(3) 0.0315(12) Uani 1 1 d . . . . .
H72 H -0.1019 -0.2983 0.1761 0.038 Uiso 1 1 calc R U . . .
C73 C -0.1733(4) 0.2371(4) 0.1412(3) 0.0289(12) Uani 1 1 d . . . . .
H73 H -0.2070 0.1700 0.1116 0.035 Uiso 1 1 calc R U . . .
C74 C -0.2229(4) 0.2994(5) 0.1499(3) 0.0351(14) Uani 1 1 d . . . . .
H74 H -0.2909 0.2758 0.1262 0.042 Uiso 1 1 calc R U . . .
C75 C -0.1724(5) 0.3975(5) 0.1936(3) 0.0340(13) Uani 1 1 d . . . . .
C76 C -0.0730(4) 0.4345(4) 0.2294(2) 0.0288(12) Uani 1 1 d . . . . .
H76 H -0.0412 0.5000 0.2600 0.035 Uiso 1 1 calc R U . . .
C77 C 0.3526(4) 0.3048(4) 0.1804(2) 0.0225(10) Uani 1 1 d . . . . .
H77A H 0.3928 0.3064 0.1501 0.034 Uiso 1 1 calc R U . . .
H77B H 0.3016 0.2299 0.1769 0.034 Uiso 1 1 calc R U . . .
H77C H 0.4016 0.3377 0.2190 0.034 Uiso 1 1 calc R U . . .
O18 O 0.2165(3) 0.1215(3) 0.04416(16) 0.0321(9) Uani 1 1 d . . . . .
H18E H 0.1847 0.1232 0.0711 0.048 Uiso 1 1 calc R U . . .
C78 C 0.1413(6) 0.0552(6) -0.0094(3) 0.057(2) Uani 1 1 d . . . . .
H78A H 0.1025 0.0912 -0.0216 0.085 Uiso 1 1 calc R U . . .
H78B H 0.0913 -0.0137 -0.0042 0.085 Uiso 1 1 calc R U . . .
H78C H 0.1782 0.0423 -0.0394 0.085 Uiso 1 1 calc R U . . .
O19 O 0.1032(6) 0.9421(6) 0.4851(3) 0.093(2) Uani 1 1 d . . . . .
H19E H 0.1157 0.9312 0.4518 0.139 Uiso 1 1 calc R U . . .
C79 C 0.1363(8) 0.8907(10) 0.5166(4) 0.091(3) Uani 1 1 d . . . . .
H79A H 0.2139 0.9251 0.5253 0.137 Uiso 1 1 calc R U . . .
H79B H 0.1062 0.8151 0.4942 0.137 Uiso 1 1 calc R U . . .
H79C H 0.1126 0.8947 0.5532 0.137 Uiso 1 1 calc R U . . .
O20 O 0.3286(3) 0.8339(3) 0.41931(19) 0.0420(10) Uani 1 1 d . . . . .
H20E H 0.3759 0.8406 0.4007 0.063 Uiso 1 1 calc R U . . .
C80 C 0.3765(7) 0.8844(7) 0.4795(4) 0.068(2) Uani 1 1 d . . . . .
H80A H 0.3930 0.9600 0.4888 0.103 Uiso 1 1 calc R U . . .
H80B H 0.4421 0.8806 0.4889 0.103 Uiso 1 1 calc R U . . .
H80C H 0.3276 0.8476 0.5024 0.103 Uiso 1 1 calc R U . . .
O21 O 0.1727(6) 0.8874(6) 0.3820(3) 0.094(2) Uani 1 1 d . . . . .
H21E H 0.2052 0.8606 0.3983 0.113 Uiso 1 1 calc R U . . .
C81 C 0.1006(12) 0.8099(12) 0.3286(6) 0.146(6) Uani 1 1 d . . . . .
H81A H 0.0435 0.8266 0.3182 0.219 Uiso 1 1 calc R U . . .
H81B H 0.0703 0.7376 0.3338 0.219 Uiso 1 1 calc R U . . .
H81C H 0.1390 0.8128 0.2974 0.219 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O12 2.008(3) . ?
Ni1 O2 2.040(3) . ?
Ni1 O9 2.049(3) . ?
Ni1 O5 2.058(3) . ?
Ni1 O4 2.062(3) . ?
Ni1 O1 2.073(3) . ?
Ni1 Ni3 2.9634(10) . ?
Ni2 O17 1.997(3) . ?
Ni2 N4 2.038(4) . ?
Ni2 O1 2.056(3) . ?
Ni2 O2 2.081(3) . ?
Ni2 O10 2.102(3) . ?
Ni2 O13 2.108(3) . ?
Ni3 O4 2.019(3) . ?
Ni3 N2 2.025(4) . ?
Ni3 O16 2.030(4) . ?
Ni3 O8 2.032(3) . ?
Ni3 O9 2.093(3) . ?
Ni3 O3 2.205(4) . ?
Ni4 O7 2.006(3) . ?
Ni4 N1 2.008(4) . ?
Ni4 O4 2.010(3) . ?
Ni4 O5 2.061(3) . ?
Ni4 O8 2.135(3) . ?
Ni4 O11 2.224(3) . ?
Ni5 N3 2.006(4) . ?
Ni5 O13 2.016(3) . ?
Ni5 O1 2.036(3) . ?
Ni5 O15 2.081(4) . ?
Ni5 O14 2.084(4) . ?
Ni5 O12 2.126(3) . ?
Cl1 C18 1.753(5) . ?
Cl2 C27 1.748(5) . ?
Cl3 C45 1.738(6) . ?
Cl4 C75 1.745(5) . ?
O1 C77 1.448(6) . ?
O2 C1 1.287(6) . ?
O3 C1 1.259(6) . ?
O4 C58 1.442(6) . ?
O5 C2 1.276(6) . ?
O6 C2 1.242(6) . ?
O7 C7 1.305(6) . ?
O8 C20 1.309(6) . ?
O9 C25 1.288(5) . ?
O10 C25 1.240(6) . ?
O11 C38 1.252(6) . ?
O12 C38 1.286(6) . ?
O13 C39 1.306(6) . ?
O14 C56 1.412(8) . ?
O14 H14E 0.84(2) . ?
O15 C57 1.427(7) . ?
O15 H15E 0.85(2) . ?
O16 C59 1.401(8) . ?
O16 H16E 0.85(2) . ?
O17 C64 1.312(6) . ?
N1 C5 1.308(6) . ?
N1 C4 1.436(6) . ?
N2 C22 1.294(6) . ?
N2 C23 1.441(6) . ?
N3 C41 1.302(6) . ?
N3 C42 1.426(6) . ?
N4 C62 1.302(6) . ?
N4 C61 1.421(6) . ?
C1 C60 1.499(7) . ?
C2 C3 1.500(6) . ?
C3 C19 1.399(7) . ?
C3 C4 1.419(7) . ?
C4 C16 1.392(7) . ?
C5 C6 1.422(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.417(7) . ?
C6 C11 1.469(7) . ?
C7 C8 1.436(7) . ?
C8 C9 1.349(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.413(8) . ?
C9 H9 0.9500 . ?
C10 C15 1.418(8) . ?
C10 C11 1.435(7) . ?
C11 C12 1.413(7) . ?
C12 C13 1.386(8) . ?
C12 H12 0.9500 . ?
C13 C14 1.398(9) . ?
C13 H13 0.9500 . ?
C14 C15 1.351(9) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.384(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.385(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.378(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.411(7) . ?
C20 C33 1.432(7) . ?
C21 C22 1.450(7) . ?
C21 C30 1.454(7) . ?
C22 H22 0.9500 . ?
C23 C29 1.398(7) . ?
C23 C24 1.404(7) . ?
C24 C26 1.396(7) . ?
C24 C25 1.513(6) . ?
C26 C27 1.387(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.374(8) . ?
C28 C29 1.385(8) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 C37 1.421(7) . ?
C30 C31 1.433(7) . ?
C31 C32 1.419(7) . ?
C31 C34 1.424(7) . ?
C32 C33 1.358(7) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 C35 1.364(8) . ?
C34 H34 0.9500 . ?
C35 C36 1.399(8) . ?
C35 H35 0.9500 . ?
C36 C37 1.370(8) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C43 1.525(7) . ?
C39 C40 1.421(7) . ?
C39 C51 1.422(7) . ?
C40 C41 1.438(7) . ?
C40 C48 1.453(7) . ?
C41 H41 0.9500 . ?
C42 C47 1.396(7) . ?
C42 C43 1.419(7) . ?
C43 C44 1.385(7) . ?
C44 C45 1.387(8) . ?
C44 H44 0.9500 . ?
C45 C46 1.381(9) . ?
C46 C47 1.379(8) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C48 C49 1.413(8) . ?
C48 C55 1.428(8) . ?
C49 C50 1.411(8) . ?
C49 C52 1.417(7) . ?
C50 C51 1.373(7) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 C53 1.366(9) . ?
C52 H52 0.9500 . ?
C53 C54 1.392(9) . ?
C53 H53 0.9500 . ?
C54 C55 1.383(8) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 C76 1.390(7) . ?
C60 C61 1.407(7) . ?
C61 C73 1.403(7) . ?
C62 C63 1.435(7) . ?
C62 H62 0.9500 . ?
C63 C64 1.409(7) . ?
C63 C68 1.455(7) . ?
C64 C65 1.440(7) . ?
C65 C66 1.349(7) . ?
C65 H65 0.9500 . ?
C66 C67 1.414(7) . ?
C66 H66 0.9500 . ?
C67 C72 1.418(7) . ?
C67 C68 1.429(7) . ?
C68 C69 1.413(7) . ?
C69 C70 1.390(7) . ?
C69 H69 0.9500 . ?
C70 C71 1.399(8) . ?
C70 H70 0.9500 . ?
C71 C72 1.365(8) . ?
C71 H71 0.9500 . ?
C72 H72 0.9500 . ?
C73 C74 1.381(8) . ?
C73 H73 0.9500 . ?
C74 C75 1.395(8) . ?
C74 H74 0.9500 . ?
C75 C76 1.394(8) . ?
C76 H76 0.9500 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
O18 C78 1.418(8) . ?
O18 H18E 0.8400 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
O19 C79 1.349(12) . ?
O19 H19E 0.8400 . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
O20 C80 1.414(9) . ?
O20 H20E 0.8400 . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
O21 C81 1.436(13) . ?
O21 H21E 0.8400 . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O12 Ni1 O2 92.61(13) . . ?
O12 Ni1 O9 179.14(13) . . ?
O2 Ni1 O9 86.62(13) . . ?
O12 Ni1 O5 92.89(13) . . ?
O2 Ni1 O5 168.18(13) . . ?
O9 Ni1 O5 87.81(13) . . ?
O12 Ni1 O4 91.95(13) . . ?
O2 Ni1 O4 86.79(12) . . ?
O9 Ni1 O4 87.63(13) . . ?
O5 Ni1 O4 82.58(12) . . ?
O12 Ni1 O1 83.36(13) . . ?
O2 Ni1 O1 85.40(13) . . ?
O9 Ni1 O1 96.94(12) . . ?
O5 Ni1 O1 105.63(13) . . ?
O4 Ni1 O1 170.69(12) . . ?
O12 Ni1 Ni3 134.61(10) . . ?
O2 Ni1 Ni3 82.52(9) . . ?
O9 Ni1 Ni3 44.92(9) . . ?
O5 Ni1 Ni3 86.17(9) . . ?
O4 Ni1 Ni3 42.87(9) . . ?
O1 Ni1 Ni3 140.41(9) . . ?
O17 Ni2 N4 87.35(14) . . ?
O17 Ni2 O1 99.34(13) . . ?
N4 Ni2 O1 172.13(14) . . ?
O17 Ni2 O2 172.57(13) . . ?
N4 Ni2 O2 88.11(14) . . ?
O1 Ni2 O2 84.80(12) . . ?
O17 Ni2 O10 89.47(13) . . ?
N4 Ni2 O10 88.75(14) . . ?
O1 Ni2 O10 87.20(13) . . ?
O2 Ni2 O10 84.55(13) . . ?
O17 Ni2 O13 99.49(13) . . ?
N4 Ni2 O13 105.33(14) . . ?
O1 Ni2 O13 77.78(12) . . ?
O2 Ni2 O13 87.38(13) . . ?
O10 Ni2 O13 163.54(13) . . ?
O4 Ni3 N2 161.97(15) . . ?
O4 Ni3 O16 98.45(15) . . ?
N2 Ni3 O16 94.66(17) . . ?
O4 Ni3 O8 78.06(13) . . ?
N2 Ni3 O8 89.08(15) . . ?
O16 Ni3 O8 92.55(16) . . ?
O4 Ni3 O9 87.59(13) . . ?
N2 Ni3 O9 82.21(14) . . ?
O16 Ni3 O9 166.96(15) . . ?
O8 Ni3 O9 100.03(13) . . ?
O4 Ni3 O3 85.49(13) . . ?
N2 Ni3 O3 107.73(15) . . ?
O16 Ni3 O3 86.41(16) . . ?
O8 Ni3 O3 163.19(13) . . ?
O9 Ni3 O3 82.53(13) . . ?
O4 Ni3 Ni1 44.02(9) . . ?
N2 Ni3 Ni1 125.10(12) . . ?
O16 Ni3 Ni1 140.09(13) . . ?
O8 Ni3 Ni1 91.54(9) . . ?
O9 Ni3 Ni1 43.72(9) . . ?
O3 Ni3 Ni1 78.77(9) . . ?
O7 Ni4 N1 88.36(14) . . ?
O7 Ni4 O4 97.27(13) . . ?
N1 Ni4 O4 174.37(14) . . ?
O7 Ni4 O5 174.99(14) . . ?
N1 Ni4 O5 90.61(14) . . ?
O4 Ni4 O5 83.78(13) . . ?
O7 Ni4 O8 97.08(13) . . ?
N1 Ni4 O8 103.51(14) . . ?
O4 Ni4 O8 75.89(13) . . ?
O5 Ni4 O8 87.93(13) . . ?
O7 Ni4 O11 92.81(13) . . ?
N1 Ni4 O11 92.46(14) . . ?
O4 Ni4 O11 87.27(13) . . ?
O5 Ni4 O11 82.33(12) . . ?
O8 Ni4 O11 161.39(12) . . ?
N3 Ni5 O13 89.83(15) . . ?
N3 Ni5 O1 158.37(15) . . ?
O13 Ni5 O1 80.38(13) . . ?
N3 Ni5 O15 98.06(16) . . ?
O13 Ni5 O15 90.40(14) . . ?
O1 Ni5 O15 101.22(14) . . ?
N3 Ni5 O14 98.76(16) . . ?
O13 Ni5 O14 171.24(14) . . ?
O1 Ni5 O14 92.09(13) . . ?
O15 Ni5 O14 86.67(15) . . ?
N3 Ni5 O12 81.54(15) . . ?
O13 Ni5 O12 100.59(13) . . ?
O1 Ni5 O12 81.39(12) . . ?
O15 Ni5 O12 169.00(14) . . ?
O14 Ni5 O12 82.54(14) . . ?
C77 O1 Ni5 122.4(3) . . ?
C77 O1 Ni2 114.9(3) . . ?
Ni5 O1 Ni2 101.38(14) . . ?
C77 O1 Ni1 121.6(3) . . ?
Ni5 O1 Ni1 97.86(13) . . ?
Ni2 O1 Ni1 93.20(13) . . ?
C1 O2 Ni1 127.4(3) . . ?
C1 O2 Ni2 117.7(3) . . ?
Ni1 O2 Ni2 93.47(13) . . ?
C1 O3 Ni3 124.6(3) . . ?
C58 O4 Ni4 116.3(3) . . ?
C58 O4 Ni3 122.0(3) . . ?
Ni4 O4 Ni3 104.96(14) . . ?
C58 O4 Ni1 119.4(3) . . ?
Ni4 O4 Ni1 96.07(13) . . ?
Ni3 O4 Ni1 93.11(13) . . ?
C2 O5 Ni1 138.1(3) . . ?
C2 O5 Ni4 123.7(3) . . ?
Ni1 O5 Ni4 94.66(13) . . ?
C7 O7 Ni4 125.0(3) . . ?
C20 O8 Ni3 122.9(3) . . ?
C20 O8 Ni4 133.9(3) . . ?
Ni3 O8 Ni4 100.14(14) . . ?
C25 O9 Ni1 121.9(3) . . ?
C25 O9 Ni3 116.9(3) . . ?
Ni1 O9 Ni3 91.35(13) . . ?
C25 O10 Ni2 129.2(3) . . ?
C38 O11 Ni4 129.8(3) . . ?
C38 O12 Ni1 125.3(3) . . ?
C38 O12 Ni5 123.9(3) . . ?
Ni1 O12 Ni5 97.04(13) . . ?
C39 O13 Ni5 125.2(3) . . ?
C39 O13 Ni2 134.0(3) . . ?
Ni5 O13 Ni2 100.31(14) . . ?
C56 O14 Ni5 127.9(4) . . ?
C56 O14 H14E 118(4) . . ?
Ni5 O14 H14E 105(4) . . ?
C57 O15 Ni5 125.4(3) . . ?
C57 O15 H15E 108(4) . . ?
Ni5 O15 H15E 117(5) . . ?
C59 O16 Ni3 127.1(4) . . ?
C59 O16 H16E 112(5) . . ?
Ni3 O16 H16E 120(5) . . ?
C64 O17 Ni2 122.3(3) . . ?
C5 N1 C4 116.7(4) . . ?
C5 N1 Ni4 123.0(3) . . ?
C4 N1 Ni4 120.2(3) . . ?
C22 N2 C23 117.7(4) . . ?
C22 N2 Ni3 122.4(3) . . ?
C23 N2 Ni3 119.4(3) . . ?
C41 N3 C42 117.9(4) . . ?
C41 N3 Ni5 124.0(3) . . ?
C42 N3 Ni5 117.5(3) . . ?
C62 N4 C61 117.3(4) . . ?
C62 N4 Ni2 122.1(3) . . ?
C61 N4 Ni2 120.1(3) . . ?
O3 C1 O2 126.5(5) . . ?
O3 C1 C60 120.9(4) . . ?
O2 C1 C60 112.6(4) . . ?
O6 C2 O5 124.8(4) . . ?
O6 C2 C3 117.4(4) . . ?
O5 C2 C3 117.7(4) . . ?
C19 C3 C4 118.9(4) . . ?
C19 C3 C2 117.2(4) . . ?
C4 C3 C2 123.8(4) . . ?
C16 C4 C3 119.8(4) . . ?
C16 C4 N1 121.2(4) . . ?
C3 C4 N1 119.0(4) . . ?
N1 C5 C6 126.6(4) . . ?
N1 C5 H5 116.7 . . ?
C6 C5 H5 116.7 . . ?
C7 C6 C5 122.0(4) . . ?
C7 C6 C11 119.5(4) . . ?
C5 C6 C11 117.9(4) . . ?
O7 C7 C6 123.8(4) . . ?
O7 C7 C8 117.7(5) . . ?
C6 C7 C8 118.5(4) . . ?
C9 C8 C7 122.1(5) . . ?
C9 C8 H8 119.0 . . ?
C7 C8 H8 119.0 . . ?
C8 C9 C10 121.9(5) . . ?
C8 C9 H9 119.1 . . ?
C10 C9 H9 119.1 . . ?
C9 C10 C15 122.0(5) . . ?
C9 C10 C11 119.1(5) . . ?
C15 C10 C11 118.9(5) . . ?
C12 C11 C10 117.8(5) . . ?
C12 C11 C6 123.5(4) . . ?
C10 C11 C6 118.7(5) . . ?
C13 C12 C11 120.7(5) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C12 C13 C14 121.0(6) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C15 C14 C13 119.5(6) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C10 122.0(6) . . ?
C14 C15 H15 119.0 . . ?
C10 C15 H15 119.0 . . ?
C17 C16 C4 120.7(5) . . ?
C17 C16 H16 119.7 . . ?
C4 C16 H16 119.7 . . ?
C16 C17 C18 118.9(5) . . ?
C16 C17 H17 120.5 . . ?
C18 C17 H17 120.5 . . ?
C19 C18 C17 122.0(5) . . ?
C19 C18 Cl1 118.7(4) . . ?
C17 C18 Cl1 119.3(4) . . ?
C18 C19 C3 119.6(5) . . ?
C18 C19 H19 120.2 . . ?
C3 C19 H19 120.2 . . ?
O8 C20 C21 123.1(4) . . ?
O8 C20 C33 118.4(4) . . ?
C21 C20 C33 118.5(5) . . ?
C20 C21 C22 121.5(5) . . ?
C20 C21 C30 119.8(4) . . ?
C22 C21 C30 118.3(4) . . ?
N2 C22 C21 126.9(5) . . ?
N2 C22 H22 116.6 . . ?
C21 C22 H22 116.6 . . ?
C29 C23 C24 119.0(5) . . ?
C29 C23 N2 120.9(4) . . ?
C24 C23 N2 120.0(4) . . ?
C26 C24 C23 119.6(4) . . ?
C26 C24 C25 114.7(4) . . ?
C23 C24 C25 125.7(4) . . ?
O10 C25 O9 125.0(4) . . ?
O10 C25 C24 116.9(4) . . ?
O9 C25 C24 118.1(4) . . ?
C27 C26 C24 119.6(5) . . ?
C27 C26 H26 120.2 . . ?
C24 C26 H26 120.2 . . ?
C28 C27 C26 121.8(5) . . ?
C28 C27 Cl2 119.5(4) . . ?
C26 C27 Cl2 118.8(4) . . ?
C27 C28 C29 118.7(5) . . ?
C27 C28 H28 120.6 . . ?
C29 C28 H28 120.6 . . ?
C28 C29 C23 121.4(5) . . ?
C28 C29 H29 119.3 . . ?
C23 C29 H29 119.3 . . ?
C37 C30 C31 116.1(4) . . ?
C37 C30 C21 124.5(5) . . ?
C31 C30 C21 119.4(4) . . ?
C32 C31 C34 121.4(5) . . ?
C32 C31 C30 118.6(4) . . ?
C34 C31 C30 119.9(5) . . ?
C33 C32 C31 121.6(5) . . ?
C33 C32 H32 119.2 . . ?
C31 C32 H32 119.2 . . ?
C32 C33 C20 122.0(5) . . ?
C32 C33 H33 119.0 . . ?
C20 C33 H33 119.0 . . ?
C35 C34 C31 121.7(5) . . ?
C35 C34 H34 119.1 . . ?
C31 C34 H34 119.1 . . ?
C34 C35 C36 118.5(5) . . ?
C34 C35 H35 120.7 . . ?
C36 C35 H35 120.7 . . ?
C37 C36 C35 121.6(5) . . ?
C37 C36 H36 119.2 . . ?
C35 C36 H36 119.2 . . ?
C36 C37 C30 122.1(5) . . ?
C36 C37 H37 119.0 . . ?
C30 C37 H37 119.0 . . ?
O11 C38 O12 124.7(4) . . ?
O11 C38 C43 118.0(4) . . ?
O12 C38 C43 117.3(4) . . ?
O13 C39 C40 123.5(4) . . ?
O13 C39 C51 117.9(4) . . ?
C40 C39 C51 118.6(4) . . ?
C39 C40 C41 122.0(4) . . ?
C39 C40 C48 119.3(4) . . ?
C41 C40 C48 118.3(4) . . ?
N3 C41 C40 127.0(5) . . ?
N3 C41 H41 116.5 . . ?
C40 C41 H41 116.5 . . ?
C47 C42 C43 119.6(5) . . ?
C47 C42 N3 118.5(5) . . ?
C43 C42 N3 121.9(4) . . ?
C44 C43 C42 119.1(5) . . ?
C44 C43 C38 116.4(4) . . ?
C42 C43 C38 124.5(4) . . ?
C43 C44 C45 120.0(5) . . ?
C43 C44 H44 120.0 . . ?
C45 C44 H44 120.0 . . ?
C46 C45 C44 121.3(5) . . ?
C46 C45 Cl3 119.4(4) . . ?
C44 C45 Cl3 119.2(5) . . ?
C47 C46 C45 119.4(5) . . ?
C47 C46 H46 120.3 . . ?
C45 C46 H46 120.3 . . ?
C46 C47 C42 120.6(5) . . ?
C46 C47 H47 119.7 . . ?
C42 C47 H47 119.7 . . ?
C49 C48 C55 116.7(5) . . ?
C49 C48 C40 120.3(5) . . ?
C55 C48 C40 123.0(5) . . ?
C50 C49 C48 118.3(5) . . ?
C50 C49 C52 120.9(5) . . ?
C48 C49 C52 120.7(5) . . ?
C51 C50 C49 122.2(5) . . ?
C51 C50 H50 118.9 . . ?
C49 C50 H50 118.9 . . ?
C50 C51 C39 121.2(5) . . ?
C50 C51 H51 119.4 . . ?
C39 C51 H51 119.4 . . ?
C53 C52 C49 120.7(6) . . ?
C53 C52 H52 119.7 . . ?
C49 C52 H52 119.7 . . ?
C52 C53 C54 119.8(5) . . ?
C52 C53 H53 120.1 . . ?
C54 C53 H53 120.1 . . ?
C55 C54 C53 120.8(6) . . ?
C55 C54 H54 119.6 . . ?
C53 C54 H54 119.6 . . ?
C54 C55 C48 121.2(6) . . ?
C54 C55 H55 119.4 . . ?
C48 C55 H55 119.4 . . ?
O14 C56 H56A 109.5 . . ?
O14 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
O14 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
O15 C57 H57A 109.5 . . ?
O15 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
O15 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
O4 C58 H58A 109.5 . . ?
O4 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
O4 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
O16 C59 H59A 109.5 . . ?
O16 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
O16 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C76 C60 C61 119.6(5) . . ?
C76 C60 C1 120.1(5) . . ?
C61 C60 C1 120.1(4) . . ?
C73 C61 C60 120.7(4) . . ?
C73 C61 N4 120.3(4) . . ?
C60 C61 N4 119.0(4) . . ?
N4 C62 C63 127.5(4) . . ?
N4 C62 H62 116.3 . . ?
C63 C62 H62 116.3 . . ?
C64 C63 C62 121.1(4) . . ?
C64 C63 C68 120.3(4) . . ?
C62 C63 C68 118.6(4) . . ?
O17 C64 C63 124.0(4) . . ?
O17 C64 C65 117.1(4) . . ?
C63 C64 C65 118.9(4) . . ?
C66 C65 C64 120.6(5) . . ?
C66 C65 H65 119.7 . . ?
C64 C65 H65 119.7 . . ?
C65 C66 C67 122.7(5) . . ?
C65 C66 H66 118.7 . . ?
C67 C66 H66 118.7 . . ?
C66 C67 C72 121.3(5) . . ?
C66 C67 C68 119.0(4) . . ?
C72 C67 C68 119.7(5) . . ?
C69 C68 C67 117.3(4) . . ?
C69 C68 C63 124.3(4) . . ?
C67 C68 C63 118.4(4) . . ?
C70 C69 C68 121.5(5) . . ?
C70 C69 H69 119.2 . . ?
C68 C69 H69 119.2 . . ?
C69 C70 C71 120.4(5) . . ?
C69 C70 H70 119.8 . . ?
C71 C70 H70 119.8 . . ?
C72 C71 C70 119.7(5) . . ?
C72 C71 H71 120.1 . . ?
C70 C71 H71 120.1 . . ?
C71 C72 C67 121.4(5) . . ?
C71 C72 H72 119.3 . . ?
C67 C72 H72 119.3 . . ?
C74 C73 C61 119.4(5) . . ?
C74 C73 H73 120.3 . . ?
C61 C73 H73 120.3 . . ?
C73 C74 C75 119.6(5) . . ?
C73 C74 H74 120.2 . . ?
C75 C74 H74 120.2 . . ?
C76 C75 C74 121.8(5) . . ?
C76 C75 Cl4 119.4(4) . . ?
C74 C75 Cl4 118.8(4) . . ?
C60 C76 C75 118.8(5) . . ?
C60 C76 H76 120.6 . . ?
C75 C76 H76 120.6 . . ?
O1 C77 H77A 109.5 . . ?
O1 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
O1 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
C78 O18 H18E 109.5 . . ?
O18 C78 H78A 109.5 . . ?
O18 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
O18 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C79 O19 H19E 109.5 . . ?
O19 C79 H79A 109.5 . . ?
O19 C79 H79B 109.5 . . ?
H79A C79 H79B 109.5 . . ?
O19 C79 H79C 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C80 O20 H20E 109.5 . . ?
O20 C80 H80A 109.5 . . ?
O20 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
O20 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
C81 O21 H21E 109.5 . . ?
O21 C81 H81A 109.5 . . ?
O21 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
O21 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni3 O3 C1 O2 7.2(7) . . . . ?
Ni3 O3 C1 C60 -170.4(3) . . . . ?
Ni1 O2 C1 O3 -4.5(7) . . . . ?
Ni2 O2 C1 O3 114.6(5) . . . . ?
Ni1 O2 C1 C60 173.3(3) . . . . ?
Ni2 O2 C1 C60 -67.5(4) . . . . ?
Ni1 O5 C2 O6 11.7(8) . . . . ?
Ni4 O5 C2 O6 -141.2(4) . . . . ?
Ni1 O5 C2 C3 -165.6(3) . . . . ?
Ni4 O5 C2 C3 41.5(5) . . . . ?
O6 C2 C3 C19 -40.3(6) . . . . ?
O5 C2 C3 C19 137.2(4) . . . . ?
O6 C2 C3 C4 136.0(5) . . . . ?
O5 C2 C3 C4 -46.5(6) . . . . ?
C19 C3 C4 C16 -1.2(7) . . . . ?
C2 C3 C4 C16 -177.4(4) . . . . ?
C19 C3 C4 N1 178.7(4) . . . . ?
C2 C3 C4 N1 2.5(7) . . . . ?
C5 N1 C4 C16 38.2(6) . . . . ?
Ni4 N1 C4 C16 -141.3(4) . . . . ?
C5 N1 C4 C3 -141.7(4) . . . . ?
Ni4 N1 C4 C3 38.8(5) . . . . ?
C4 N1 C5 C6 -167.6(4) . . . . ?
Ni4 N1 C5 C6 11.9(7) . . . . ?
N1 C5 C6 C7 15.5(7) . . . . ?
N1 C5 C6 C11 -173.4(4) . . . . ?
Ni4 O7 C7 C6 -18.2(6) . . . . ?
Ni4 O7 C7 C8 164.0(4) . . . . ?
C5 C6 C7 O7 -12.2(7) . . . . ?
C11 C6 C7 O7 176.8(4) . . . . ?
C5 C6 C7 C8 165.6(5) . . . . ?
C11 C6 C7 C8 -5.3(7) . . . . ?
O7 C7 C8 C9 179.7(5) . . . . ?
C6 C7 C8 C9 1.7(8) . . . . ?
C7 C8 C9 C10 1.6(9) . . . . ?
C8 C9 C10 C15 178.5(6) . . . . ?
C8 C9 C10 C11 -1.1(9) . . . . ?
C9 C10 C11 C12 177.5(5) . . . . ?
C15 C10 C11 C12 -2.1(9) . . . . ?
C9 C10 C11 C6 -2.6(8) . . . . ?
C15 C10 C11 C6 177.8(6) . . . . ?
C7 C6 C11 C12 -174.3(5) . . . . ?
C5 C6 C11 C12 14.4(7) . . . . ?
C7 C6 C11 C10 5.8(7) . . . . ?
C5 C6 C11 C10 -165.5(5) . . . . ?
C10 C11 C12 C13 2.2(9) . . . . ?
C6 C11 C12 C13 -177.7(6) . . . . ?
C11 C12 C13 C14 -0.8(10) . . . . ?
C12 C13 C14 C15 -0.8(12) . . . . ?
C13 C14 C15 C10 0.9(12) . . . . ?
C9 C10 C15 C14 -179.0(7) . . . . ?
C11 C10 C15 C14 0.6(11) . . . . ?
C3 C4 C16 C17 2.0(7) . . . . ?
N1 C4 C16 C17 -177.9(4) . . . . ?
C4 C16 C17 C18 -2.8(8) . . . . ?
C16 C17 C18 C19 2.9(8) . . . . ?
C16 C17 C18 Cl1 -177.7(4) . . . . ?
C17 C18 C19 C3 -2.1(8) . . . . ?
Cl1 C18 C19 C3 178.4(4) . . . . ?
C4 C3 C19 C18 1.3(7) . . . . ?
C2 C3 C19 C18 177.7(5) . . . . ?
Ni3 O8 C20 C21 28.2(6) . . . . ?
Ni4 O8 C20 C21 -175.9(3) . . . . ?
Ni3 O8 C20 C33 -152.6(4) . . . . ?
Ni4 O8 C20 C33 3.3(7) . . . . ?
O8 C20 C21 C22 8.8(8) . . . . ?
C33 C20 C21 C22 -170.4(5) . . . . ?
O8 C20 C21 C30 -177.9(4) . . . . ?
C33 C20 C21 C30 2.9(7) . . . . ?
C23 N2 C22 C21 178.6(5) . . . . ?
Ni3 N2 C22 C21 6.1(7) . . . . ?
C20 C21 C22 N2 -28.5(8) . . . . ?
C30 C21 C22 N2 158.2(5) . . . . ?
C22 N2 C23 C29 41.0(7) . . . . ?
Ni3 N2 C23 C29 -146.3(4) . . . . ?
C22 N2 C23 C24 -141.6(5) . . . . ?
Ni3 N2 C23 C24 31.2(6) . . . . ?
C29 C23 C24 C26 -0.2(7) . . . . ?
N2 C23 C24 C26 -177.7(4) . . . . ?
C29 C23 C24 C25 -179.4(5) . . . . ?
N2 C23 C24 C25 3.1(7) . . . . ?
Ni2 O10 C25 O9 -31.7(6) . . . . ?
Ni2 O10 C25 C24 148.8(3) . . . . ?
Ni1 O9 C25 O10 19.9(6) . . . . ?
Ni3 O9 C25 O10 130.2(4) . . . . ?
Ni1 O9 C25 C24 -160.6(3) . . . . ?
Ni3 O9 C25 C24 -50.3(5) . . . . ?
C26 C24 C25 O10 8.5(6) . . . . ?
C23 C24 C25 O10 -172.3(5) . . . . ?
C26 C24 C25 O9 -171.1(4) . . . . ?
C23 C24 C25 O9 8.1(7) . . . . ?
C23 C24 C26 C27 -0.7(7) . . . . ?
C25 C24 C26 C27 178.6(4) . . . . ?
C24 C26 C27 C28 0.8(8) . . . . ?
C24 C26 C27 Cl2 179.4(4) . . . . ?
C26 C27 C28 C29 0.1(8) . . . . ?
Cl2 C27 C28 C29 -178.5(5) . . . . ?
C27 C28 C29 C23 -1.1(9) . . . . ?
C24 C23 C29 C28 1.2(8) . . . . ?
N2 C23 C29 C28 178.6(5) . . . . ?
C20 C21 C30 C37 176.4(5) . . . . ?
C22 C21 C30 C37 -10.2(7) . . . . ?
C20 C21 C30 C31 -1.7(7) . . . . ?
C22 C21 C30 C31 171.8(5) . . . . ?
C37 C30 C31 C32 -178.6(5) . . . . ?
C21 C30 C31 C32 -0.3(7) . . . . ?
C37 C30 C31 C34 -1.2(7) . . . . ?
C21 C30 C31 C34 177.0(4) . . . . ?
C34 C31 C32 C33 -176.2(5) . . . . ?
C30 C31 C32 C33 1.1(7) . . . . ?
C31 C32 C33 C20 0.1(8) . . . . ?
O8 C20 C33 C32 178.6(5) . . . . ?
C21 C20 C33 C32 -2.2(8) . . . . ?
C32 C31 C34 C35 178.9(5) . . . . ?
C30 C31 C34 C35 1.6(8) . . . . ?
C31 C34 C35 C36 -0.7(8) . . . . ?
C34 C35 C36 C37 -0.6(9) . . . . ?
C35 C36 C37 C30 0.9(9) . . . . ?
C31 C30 C37 C36 0.0(8) . . . . ?
C21 C30 C37 C36 -178.1(5) . . . . ?
Ni4 O11 C38 O12 7.9(7) . . . . ?
Ni4 O11 C38 C43 -171.8(3) . . . . ?
Ni1 O12 C38 O11 -14.6(7) . . . . ?
Ni5 O12 C38 O11 -145.7(4) . . . . ?
Ni1 O12 C38 C43 165.1(3) . . . . ?
Ni5 O12 C38 C43 34.0(6) . . . . ?
Ni5 O13 C39 C40 -22.9(6) . . . . ?
Ni2 O13 C39 C40 166.6(3) . . . . ?
Ni5 O13 C39 C51 158.0(3) . . . . ?
Ni2 O13 C39 C51 -12.5(7) . . . . ?
O13 C39 C40 C41 -6.4(8) . . . . ?
C51 C39 C40 C41 172.7(5) . . . . ?
O13 C39 C40 C48 -179.5(4) . . . . ?
C51 C39 C40 C48 -0.3(7) . . . . ?
C42 N3 C41 C40 -176.8(5) . . . . ?
Ni5 N3 C41 C40 -6.0(7) . . . . ?
C39 C40 C41 N3 22.5(8) . . . . ?
C48 C40 C41 N3 -164.4(5) . . . . ?
C41 N3 C42 C47 -52.2(7) . . . . ?
Ni5 N3 C42 C47 136.4(4) . . . . ?
C41 N3 C42 C43 129.6(5) . . . . ?
Ni5 N3 C42 C43 -41.8(6) . . . . ?
C47 C42 C43 C44 1.2(8) . . . . ?
N3 C42 C43 C44 179.3(5) . . . . ?
C47 C42 C43 C38 -178.1(5) . . . . ?
N3 C42 C43 C38 0.1(8) . . . . ?
O11 C38 C43 C44 4.4(7) . . . . ?
O12 C38 C43 C44 -175.3(5) . . . . ?
O11 C38 C43 C42 -176.4(5) . . . . ?
O12 C38 C43 C42 3.9(7) . . . . ?
C42 C43 C44 C45 -1.0(8) . . . . ?
C38 C43 C44 C45 178.3(5) . . . . ?
C43 C44 C45 C46 0.2(10) . . . . ?
C43 C44 C45 Cl3 -179.5(5) . . . . ?
C44 C45 C46 C47 0.4(11) . . . . ?
Cl3 C45 C46 C47 -179.8(5) . . . . ?
C45 C46 C47 C42 -0.3(10) . . . . ?
C43 C42 C47 C46 -0.5(9) . . . . ?
N3 C42 C47 C46 -178.8(6) . . . . ?
C39 C40 C48 C49 3.3(7) . . . . ?
C41 C40 C48 C49 -170.0(5) . . . . ?
C39 C40 C48 C55 -176.5(5) . . . . ?
C41 C40 C48 C55 10.2(7) . . . . ?
C55 C48 C49 C50 176.2(5) . . . . ?
C40 C48 C49 C50 -3.6(7) . . . . ?
C55 C48 C49 C52 -1.1(7) . . . . ?
C40 C48 C49 C52 179.1(5) . . . . ?
C48 C49 C50 C51 1.0(8) . . . . ?
C52 C49 C50 C51 178.2(5) . . . . ?
C49 C50 C51 C39 2.0(8) . . . . ?
O13 C39 C51 C50 176.9(5) . . . . ?
C40 C39 C51 C50 -2.3(8) . . . . ?
C50 C49 C52 C53 -177.5(5) . . . . ?
C48 C49 C52 C53 -0.3(8) . . . . ?
C49 C52 C53 C54 0.8(9) . . . . ?
C52 C53 C54 C55 0.2(9) . . . . ?
C53 C54 C55 C48 -1.7(9) . . . . ?
C49 C48 C55 C54 2.1(8) . . . . ?
C40 C48 C55 C54 -178.1(5) . . . . ?
O3 C1 C60 C76 56.5(7) . . . . ?
O2 C1 C60 C76 -121.4(5) . . . . ?
O3 C1 C60 C61 -127.4(5) . . . . ?
O2 C1 C60 C61 54.7(6) . . . . ?
C76 C60 C61 C73 3.3(8) . . . . ?
C1 C60 C61 C73 -172.8(5) . . . . ?
C76 C60 C61 N4 -177.2(5) . . . . ?
C1 C60 C61 N4 6.7(7) . . . . ?
C62 N4 C61 C73 -53.9(6) . . . . ?
Ni2 N4 C61 C73 133.8(4) . . . . ?
C62 N4 C61 C60 126.6(5) . . . . ?
Ni2 N4 C61 C60 -45.7(6) . . . . ?
C61 N4 C62 C63 178.3(5) . . . . ?
Ni2 N4 C62 C63 -9.5(7) . . . . ?
N4 C62 C63 C64 -13.4(8) . . . . ?
N4 C62 C63 C68 169.4(5) . . . . ?
Ni2 O17 C64 C63 34.8(6) . . . . ?
Ni2 O17 C64 C65 -145.9(4) . . . . ?
C62 C63 C64 O17 -0.2(7) . . . . ?
C68 C63 C64 O17 177.0(4) . . . . ?
C62 C63 C64 C65 -179.4(5) . . . . ?
C68 C63 C64 C65 -2.3(7) . . . . ?
O17 C64 C65 C66 -179.0(5) . . . . ?
C63 C64 C65 C66 0.4(8) . . . . ?
C64 C65 C66 C67 1.1(9) . . . . ?
C65 C66 C67 C72 178.9(6) . . . . ?
C65 C66 C67 C68 -0.7(9) . . . . ?
C66 C67 C68 C69 179.3(5) . . . . ?
C72 C67 C68 C69 -0.3(7) . . . . ?
C66 C67 C68 C63 -1.2(7) . . . . ?
C72 C67 C68 C63 179.2(5) . . . . ?
C64 C63 C68 C69 -177.9(5) . . . . ?
C62 C63 C68 C69 -0.6(7) . . . . ?
C64 C63 C68 C67 2.7(7) . . . . ?
C62 C63 C68 C67 179.9(4) . . . . ?
C67 C68 C69 C70 0.1(7) . . . . ?
C63 C68 C69 C70 -179.4(5) . . . . ?
C68 C69 C70 C71 0.3(8) . . . . ?
C69 C70 C71 C72 -0.5(9) . . . . ?
C70 C71 C72 C67 0.2(9) . . . . ?
C66 C67 C72 C71 -179.4(6) . . . . ?
C68 C67 C72 C71 0.2(9) . . . . ?
C60 C61 C73 C74 -1.2(8) . . . . ?
N4 C61 C73 C74 179.3(5) . . . . ?
C61 C73 C74 C75 -0.3(9) . . . . ?
C73 C74 C75 C76 -0.5(9) . . . . ?
C73 C74 C75 Cl4 179.4(5) . . . . ?
C61 C60 C76 C75 -4.0(8) . . . . ?
C1 C60 C76 C75 172.1(5) . . . . ?
C74 C75 C76 C60 2.6(9) . . . . ?
Cl4 C75 C76 C60 -177.3(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O14 H14E O6 0.84(2) 1.82(3) 2.625(5) 160(6) .
O15 H15E O18 0.85(2) 1.77(2) 2.615(5) 177(7) .
O16 H16E O20 0.85(2) 1.80(3) 2.625(6) 164(7) .
O18 H18E O17 0.84 1.79 2.624(5) 172.9 .
O19 H19E O21 0.84 2.06 2.872(10) 162.9 .
O20 H20E O7 0.84 1.80 2.641(5) 177.0 .
O21 H21E O20 0.84 2.02 2.807(8) 155.1 .

_refine_diff_density_max         1.273
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.110





#=============================================================================#
#    Luis Cunha-Silva @ REQUIMTE / LAQV & DQB FCUP  *  19/05/2016  *   END    #
#=============================================================================#
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_comp2_rev
_database_code_depnum_ccdc_archive 'CCDC 1448721'
_audit_update_record             
;
2016-05-20 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;

# ========================================================================= #

_audit_creation_method           'SHELXL-2014/7 and enCIFer'
_shelx_SHELXL_version_number     2014/7
_audit_creation_date             '19 May 2016'

# ========================================================================= #


_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H70 Cl4 N8 Ni5 O18, 3(C3 H7 N O)'
_chemical_formula_sum            'C93 H91 Cl4 N11 Ni5 O21'
_chemical_formula_weight         2134.11

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.1417(10)
_cell_length_b                   14.1587(10)
_cell_length_c                   14.7117(11)
_cell_angle_alpha                92.408(2)
_cell_angle_beta                 99.389(2)
_cell_angle_gamma                116.998(2)
_cell_volume                     2566.8(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8253
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      28.42

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_F_000             1102
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    1.075
_shelx_estimated_absorpt_T_min   0.739
_shelx_estimated_absorpt_T_max   0.968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_process_details   
; 
'SADABS V2012/1 (Bruker AXS Inc.)' 
;


_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20519
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.977
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.027
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measured_fraction_theta_full 0.924
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_Laue_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_point_group_measured_fraction_full 0.924


_reflns_number_total             8395
_reflns_number_gt                7062
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 (Bruker AXS Inc., 2012)'
_computing_cell_refinement       'SAINT (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT (Bruker AXS Inc., 2012)'
_computing_structure_solution    'SHELXS (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2014)'


_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0722P)²+26.5167P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8395
_refine_ls_number_parameters     607
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0974
_refine_ls_wR_factor_ref         0.2268
_refine_ls_wR_factor_gt          0.2184
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_restrained_S_all      1.170
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.5000 0.0000 0.0108(3) Uani 1 2 d S . P . .
Ni2 Ni 0.26885(8) 0.39960(7) -0.11519(6) 0.0133(2) Uani 1 1 d . . . . .
Ni3 Ni 0.33513(8) 0.32313(8) 0.07662(6) 0.0150(3) Uani 1 1 d . . . . .
Cl1 Cl 0.3211(3) 0.6780(2) 0.44932(19) 0.0582(8) Uani 1 1 d . . . . .
Cl2 Cl 0.3427(2) 0.85211(19) -0.35563(16) 0.0367(6) Uani 1 1 d . . . . .
O1 O 0.3735(4) 0.3521(4) -0.0506(3) 0.0137(11) Uani 1 1 d . . . . .
H1 H 0.3874 0.2994 -0.0861 0.016 Uiso 1 1 calc R U . . .
O2 O 0.3977(4) 0.5535(4) -0.0661(3) 0.0127(10) Uani 1 1 d . . . . .
O3 O 0.5213(4) 0.6895(4) -0.1230(4) 0.0189(12) Uani 1 1 d . . . . .
O4 O 0.2128(4) 0.3618(4) 0.0045(4) 0.0174(11) Uani 1 1 d . . . . .
O5 O 0.4288(4) 0.4832(4) 0.1106(3) 0.0144(11) Uani 1 1 d . . . . .
O6 O 0.4864(5) 0.6524(5) 0.1695(4) 0.0311(14) Uani 1 1 d . . . . .
O7 O 0.2515(4) 0.1638(4) 0.0586(4) 0.0209(12) Uani 1 1 d . . . . .
O8 O 0.3256(4) 0.4282(4) -0.2371(3) 0.0191(12) Uani 1 1 d . . . . .
O9 O 0.1472(5) 0.2540(4) -0.1851(4) 0.0242(13) Uani 1 1 d . . . . .
N1 N 0.1838(5) 0.4813(5) -0.1403(4) 0.0169(14) Uani 1 1 d . . . . .
N2 N 0.3078(5) 0.3236(5) 0.2088(4) 0.0197(14) Uani 1 1 d . . . . .
N3 N 0.3729(6) 0.3956(6) -0.3696(5) 0.0301(17) Uani 1 1 d . . . . .
N4 N 0.0394(5) 0.0783(5) -0.1801(5) 0.0239(15) Uani 1 1 d . . . . .
C1 C 0.4262(6) 0.6283(6) -0.1188(5) 0.0138(16) Uani 1 1 d . . . . .
C2 C 0.3363(6) 0.6390(6) -0.1814(5) 0.0162(16) Uani 1 1 d . . . . .
C3 C 0.2248(7) 0.5731(7) -0.1894(5) 0.0213(18) Uani 1 1 d . . . . .
C4 C 0.1023(6) 0.4632(7) -0.1038(5) 0.0199(17) Uani 1 1 d . . . . .
H4 H 0.0705 0.5091 -0.1152 0.024 Uiso 1 1 calc R U . . .
C5 C 0.0527(6) 0.3800(6) -0.0466(5) 0.0192(17) Uani 1 1 d . . . . .
C6 C 0.1138(6) 0.3401(6) 0.0085(5) 0.0125(15) Uani 1 1 d . . . . .
C7 C 0.4304(6) 0.5536(7) 0.1692(5) 0.0193(17) Uani 1 1 d . . . . .
C8 C 0.3638(7) 0.5165(7) 0.2428(5) 0.0231(18) Uani 1 1 d . . . . .
C9 C 0.3040(7) 0.4107(6) 0.2560(5) 0.0196(17) Uani 1 1 d . . . . .
C10 C 0.3090(6) 0.2487(6) 0.2551(5) 0.0192(17) Uani 1 1 d . . . . .
H10 H 0.3131 0.2597 0.3201 0.023 Uiso 1 1 calc R U . . .
C11 C 0.3048(6) 0.1512(6) 0.2196(5) 0.0156(16) Uani 1 1 d . . . . .
C12 C 0.2688(6) 0.1100(6) 0.1234(6) 0.0197(17) Uani 1 1 d . . . . .
C13 C 0.2453(7) 0.0022(7) 0.0958(6) 0.029(2) Uani 1 1 d . . . . .
H13 H 0.2160 -0.0276 0.0324 0.034 Uiso 1 1 calc R U . . .
C14 C 0.2638(7) -0.0589(6) 0.1584(6) 0.0259(19) Uani 1 1 d . . . . .
H14 H 0.2467 -0.1303 0.1373 0.031 Uiso 1 1 calc R U . . .
C15 C 0.3078(7) -0.0193(6) 0.2541(6) 0.0228(18) Uani 1 1 d . . . . .
C16 C 0.3287(6) 0.0868(6) 0.2865(5) 0.0191(17) Uani 1 1 d . . . . .
C17 C 0.3748(7) 0.1237(7) 0.3807(6) 0.0250(19) Uani 1 1 d . . . . .
H17 H 0.3931 0.1948 0.4037 0.030 Uiso 1 1 calc R U . . .
C18 C 0.3944(8) 0.0608(8) 0.4404(6) 0.035(2) Uani 1 1 d . . . . .
H18 H 0.4237 0.0888 0.5042 0.042 Uiso 1 1 calc R U . . .
C19 C 0.3726(8) -0.0438(8) 0.4109(7) 0.037(2) Uani 1 1 d . . . . .
H19 H 0.3862 -0.0862 0.4543 0.045 Uiso 1 1 calc R U . . .
C20 C 0.3327(7) -0.0830(7) 0.3214(6) 0.030(2) Uani 1 1 d . . . . .
H20 H 0.3202 -0.1529 0.3006 0.036 Uiso 1 1 calc R U . . .
C21 C 0.2357(7) 0.3883(7) 0.3218(6) 0.027(2) Uani 1 1 d . . . . .
H21 H 0.1887 0.3159 0.3269 0.033 Uiso 1 1 calc R U . . .
C22 C 0.2357(8) 0.4676(7) 0.3779(6) 0.032(2) Uani 1 1 d . . . . .
H22 H 0.1887 0.4513 0.4208 0.038 Uiso 1 1 calc R U . . .
C23 C 0.3072(9) 0.5738(8) 0.3704(6) 0.037(2) Uani 1 1 d . . . . .
C24 C 0.3663(8) 0.5991(7) 0.3020(6) 0.028(2) Uani 1 1 d . . . . .
H24 H 0.4089 0.6718 0.2945 0.033 Uiso 1 1 calc R U . . .
C25 C 0.0643(6) 0.2757(6) 0.0784(6) 0.0217(17) Uani 1 1 d . . . . .
H25 H 0.1050 0.2501 0.1182 0.026 Uiso 1 1 calc R U . . .
C26 C -0.0375(7) 0.2507(7) 0.0891(6) 0.0228(18) Uani 1 1 d . . . . .
H26 H -0.0655 0.2097 0.1368 0.027 Uiso 1 1 calc R U . . .
C27 C -0.1030(6) 0.2847(6) 0.0301(5) 0.0198(17) Uani 1 1 d . . . . .
C28 C -0.0581(6) 0.3495(6) -0.0391(5) 0.0199(17) Uani 1 1 d . . . . .
C29 C -0.1274(7) 0.3784(7) -0.0977(6) 0.0263(19) Uani 1 1 d . . . . .
H29 H -0.1007 0.4202 -0.1454 0.032 Uiso 1 1 calc R U . . .
C30 C -0.2316(7) 0.3486(8) -0.0885(6) 0.033(2) Uani 1 1 d . . . . .
H30 H -0.2753 0.3706 -0.1289 0.039 Uiso 1 1 calc R U . . .
C31 C -0.2741(7) 0.2858(7) -0.0197(6) 0.029(2) Uani 1 1 d . . . . .
H31 H -0.3463 0.2657 -0.0132 0.035 Uiso 1 1 calc R U . . .
C32 C -0.2116(7) 0.2537(7) 0.0378(6) 0.0259(19) Uani 1 1 d . . . . .
H32 H -0.2411 0.2100 0.0836 0.031 Uiso 1 1 calc R U . . .
C33 C 0.1516(7) 0.5935(8) -0.2503(6) 0.034(2) Uani 1 1 d . . . . .
H33 H 0.0760 0.5478 -0.2573 0.040 Uiso 1 1 calc R U . . .
C34 C 0.1871(8) 0.6790(8) -0.3007(7) 0.036(2) Uani 1 1 d . . . . .
H34 H 0.1364 0.6924 -0.3415 0.043 Uiso 1 1 calc R U . . .
C35 C 0.2966(8) 0.7444(7) -0.2914(6) 0.029(2) Uani 1 1 d . . . . .
C36 C 0.3708(7) 0.7258(6) -0.2333(5) 0.0206(17) Uani 1 1 d . . . . .
H36 H 0.4461 0.7718 -0.2280 0.025 Uiso 1 1 calc R U . . .
C37 C 0.3287(7) 0.3656(7) -0.2958(5) 0.0223(18) Uani 1 1 d . . . . .
H37 H 0.2978 0.2920 -0.2880 0.027 Uiso 1 1 calc R U . . .
C38 C 0.3685(9) 0.3173(10) -0.4405(7) 0.050(3) Uani 1 1 d . . . . .
H38A H 0.3432 0.2475 -0.4180 0.074 Uiso 1 1 calc R U . . .
H38B H 0.4410 0.3404 -0.4536 0.074 Uiso 1 1 calc R U . . .
H38C H 0.3184 0.3116 -0.4975 0.074 Uiso 1 1 calc R U . . .
C39 C 0.4190(9) 0.5072(9) -0.3847(7) 0.043(3) Uani 1 1 d . . . . .
H39A H 0.3706 0.5159 -0.4355 0.065 Uiso 1 1 calc R U . . .
H39B H 0.4900 0.5296 -0.4008 0.065 Uiso 1 1 calc R U . . .
H39C H 0.4274 0.5513 -0.3278 0.065 Uiso 1 1 calc R U . . .
C40 C 0.1204(7) 0.1721(7) -0.1448(5) 0.0208(18) Uani 1 1 d . . . . .
H40 H 0.1616 0.1785 -0.0849 0.025 Uiso 1 1 calc R U . . .
C41 C 0.0140(8) -0.0138(7) -0.1304(7) 0.038(2) Uani 1 1 d . . . . .
H41A H 0.0674 0.0065 -0.0721 0.057 Uiso 1 1 calc R U . . .
H41B H 0.0159 -0.0709 -0.1687 0.057 Uiso 1 1 calc R U . . .
H41C H -0.0586 -0.0391 -0.1168 0.057 Uiso 1 1 calc R U . . .
C42 C -0.0280(9) 0.0632(9) -0.2692(7) 0.049(3) Uani 1 1 d . . . . .
H42A H -0.0974 0.0580 -0.2607 0.073 Uiso 1 1 calc R U . . .
H42B H -0.0408 -0.0028 -0.3052 0.073 Uiso 1 1 calc R U . . .
H42C H 0.0082 0.1240 -0.3024 0.073 Uiso 1 1 calc R U . . .
O12 O -0.0100(19) 0.1656(19) 0.3147(15) 0.091(6) Uiso 0.5 1 d . . P . .
N7 N -0.053(2) 0.087(2) 0.4350(17) 0.073(6) Uiso 0.5 1 d . . P . .
C51 C -0.072(3) 0.117(3) 0.363(2) 0.079(8) Uiso 0.5 1 d . . P . .
H51 H -0.1458 0.1003 0.3414 0.095 Uiso 0.5 1 calc R U P . .
C50 C 0.057(3) 0.115(3) 0.475(2) 0.103(11) Uiso 0.5 1 d . . P . .
H50A H 0.1052 0.1650 0.4385 0.154 Uiso 0.5 1 calc R U P A 2
H50B H 0.0664 0.0504 0.4739 0.154 Uiso 0.5 1 calc R U P A 2
H50C H 0.0752 0.1488 0.5389 0.154 Uiso 0.5 1 calc R U P A 2
C49 C -0.141(4) 0.016(4) 0.482(3) 0.150(17) Uiso 0.5 1 d . . P . .
H49A H -0.1087 0.0000 0.5394 0.225 Uiso 0.25 1 calc R U P . .
H49B H -0.1824 0.0521 0.4957 0.225 Uiso 0.25 1 calc R U P . .
H49C H -0.1887 -0.0509 0.4402 0.225 Uiso 0.25 1 calc R U P . .
H49D H -0.2112 0.0008 0.4442 0.225 Uiso 0.25 1 calc R U P . .
H49E H -0.1374 -0.0513 0.4878 0.225 Uiso 0.25 1 calc R U P . .
H49F H -0.1312 0.0517 0.5433 0.225 Uiso 0.25 1 calc R U P . .
N5 N 0.6103(15) 0.9224(14) 0.1775(12) 0.044(4) Uiso 0.5 1 d . . P . .
O10 O 0.6395(18) 0.8782(18) 0.3098(15) 0.090(6) Uiso 0.5 1 d . . P . .
C44 C 0.698(2) 0.935(2) 0.1556(19) 0.067(7) Uiso 0.5 1 d . . P . .
H44A H 0.7486 1.0116 0.1619 0.101 Uiso 0.5 1 calc R U P . .
H44B H 0.6829 0.9032 0.0911 0.101 Uiso 0.5 1 calc R U P . .
H44C H 0.7303 0.9001 0.1968 0.101 Uiso 0.5 1 calc R U P . .
C45 C 0.569(3) 0.897(3) 0.248(2) 0.089(9) Uiso 0.5 1 d . . P . .
H45 H 0.5017 0.8923 0.2570 0.107 Uiso 0.5 1 calc R U P . .
C43 C 0.548(4) 0.953(4) 0.113(3) 0.145(17) Uiso 0.5 1 d . . P . .
H43A H 0.5865 1.0305 0.1128 0.217 Uiso 0.5 1 calc R U P . .
H43B H 0.4782 0.9337 0.1313 0.217 Uiso 0.5 1 calc R U P . .
H43C H 0.5350 0.9161 0.0513 0.217 Uiso 0.5 1 calc R U P . .
N6 N -0.0100(17) 0.3450(17) 0.6046(13) 0.057(5) Uiso 0.5 1 d . . P . .
C48 C 0.0902(18) 0.3594(18) 0.6133(15) 0.043(5) Uiso 0.5 1 d . . P . .
H48 H 0.1220 0.3491 0.6716 0.052 Uiso 0.5 1 calc R U P . .
O11 O 0.137(2) 0.380(2) 0.5650(17) 0.106(7) Uiso 0.5 1 d . . P . .
C47 C -0.068(2) 0.311(2) 0.6794(16) 0.055(6) Uiso 0.5 1 d . . P . .
H47A H -0.0165 0.3202 0.7367 0.082 Uiso 0.5 1 calc R U P . .
H47B H -0.1220 0.2357 0.6636 0.082 Uiso 0.5 1 calc R U P . .
H47C H -0.1040 0.3546 0.6885 0.082 Uiso 0.5 1 calc R U P . .
C46 C -0.034(5) 0.414(5) 0.524(4) 0.19(2) Uiso 0.5 1 d . . P . .
H46A H -0.0464 0.4700 0.5527 0.283 Uiso 0.5 1 calc R U P . .
H46B H -0.0975 0.3663 0.4767 0.283 Uiso 0.5 1 calc R U P . .
H46C H 0.0294 0.4476 0.4947 0.283 Uiso 0.5 1 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O5 2.017(5) . ?
Ni1 O5 2.017(5) 2_665 ?
Ni1 O1 2.043(5) 2_665 ?
Ni1 O1 2.043(5) . ?
Ni1 O2 2.052(4) 2_665 ?
Ni1 O2 2.052(4) . ?
Ni1 Ni3 2.9616(9) 2_665 ?
Ni1 Ni3 2.9616(9) . ?
Ni2 O1 2.011(5) . ?
Ni2 N1 2.018(6) . ?
Ni2 O4 2.042(5) . ?
Ni2 O8 2.064(5) . ?
Ni2 O9 2.072(6) . ?
Ni2 O2 2.104(5) . ?
Ni3 O7 1.996(5) . ?
Ni3 O5 2.026(5) . ?
Ni3 O1 2.040(5) . ?
Ni3 N2 2.044(6) . ?
Ni3 O3 2.122(5) 2_665 ?
Ni3 O4 2.175(5) . ?
Cl1 C23 1.756(9) . ?
Cl2 C35 1.750(8) . ?
O1 H1 1.0000 . ?
O2 C1 1.291(8) . ?
O3 C1 1.240(9) . ?
O3 Ni3 2.122(5) 2_665 ?
O4 C6 1.301(8) . ?
O5 C7 1.279(9) . ?
O6 C7 1.256(10) . ?
O7 C12 1.305(9) . ?
O8 C37 1.231(9) . ?
O9 C40 1.253(9) . ?
N1 C4 1.277(10) . ?
N1 C3 1.442(10) . ?
N2 C10 1.289(10) . ?
N2 C9 1.416(10) . ?
N3 C37 1.331(10) . ?
N3 C39 1.453(12) . ?
N3 C38 1.463(12) . ?
N4 C40 1.309(11) . ?
N4 C42 1.432(12) . ?
N4 C41 1.450(11) . ?
C1 C2 1.514(10) . ?
C2 C3 1.402(11) . ?
C2 C36 1.410(10) . ?
C3 C33 1.397(11) . ?
C4 C5 1.452(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.407(10) . ?
C5 C28 1.449(11) . ?
C6 C25 1.453(10) . ?
C7 C8 1.506(11) . ?
C8 C9 1.387(12) . ?
C8 C24 1.412(11) . ?
C9 C21 1.422(11) . ?
C10 C11 1.428(11) . ?
C10 H10 0.9500 . ?
C11 C12 1.425(11) . ?
C11 C16 1.470(10) . ?
C12 C13 1.431(12) . ?
C13 C14 1.364(11) . ?
C13 H13 0.9500 . ?
C14 C15 1.419(12) . ?
C14 H14 0.9500 . ?
C15 C16 1.436(11) . ?
C15 C20 1.471(11) . ?
C16 C17 1.398(12) . ?
C17 C18 1.359(11) . ?
C17 H17 0.9500 . ?
C18 C19 1.402(14) . ?
C18 H18 0.9500 . ?
C19 C20 1.332(13) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.365(12) . ?
C21 H21 0.9500 . ?
C22 C23 1.402(14) . ?
C22 H22 0.9500 . ?
C23 C24 1.368(12) . ?
C24 H24 0.9500 . ?
C25 C26 1.356(11) . ?
C25 H25 0.9500 . ?
C26 C27 1.421(11) . ?
C26 H26 0.9500 . ?
C27 C32 1.419(11) . ?
C27 C28 1.429(11) . ?
C28 C29 1.411(11) . ?
C29 C30 1.368(12) . ?
C29 H29 0.9500 . ?
C30 C31 1.402(13) . ?
C30 H30 0.9500 . ?
C31 C32 1.363(12) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C34 1.383(12) . ?
C33 H33 0.9500 . ?
C34 C35 1.376(13) . ?
C34 H34 0.9500 . ?
C35 C36 1.371(11) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40 0.9500 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
O12 C51 1.20(3) . ?
N7 C51 1.20(3) . ?
N7 C50 1.42(4) . ?
N7 C49 1.49(5) . ?
C51 H51 0.9500 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C49 H49D 0.9800 . ?
C49 H49E 0.9800 . ?
C49 H49F 0.9800 . ?
N5 C45 1.26(3) . ?
N5 C44 1.27(3) . ?
N5 C43 1.40(4) . ?
O10 C45 1.36(4) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45 0.9500 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
N6 C48 1.32(3) . ?
N6 C47 1.44(3) . ?
N6 C46 1.66(5) . ?
C48 O11 1.01(3) . ?
C48 H48 0.9500 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Ni1 O5 180.0 . 2_665 ?
O5 Ni1 O1 95.9(2) . 2_665 ?
O5 Ni1 O1 84.1(2) 2_665 2_665 ?
O5 Ni1 O1 84.1(2) . . ?
O5 Ni1 O1 95.9(2) 2_665 . ?
O1 Ni1 O1 180.0 2_665 . ?
O5 Ni1 O2 90.67(18) . 2_665 ?
O5 Ni1 O2 89.33(18) 2_665 2_665 ?
O1 Ni1 O2 83.92(19) 2_665 2_665 ?
O1 Ni1 O2 96.08(19) . 2_665 ?
O5 Ni1 O2 89.33(18) . . ?
O5 Ni1 O2 90.67(18) 2_665 . ?
O1 Ni1 O2 96.08(19) 2_665 . ?
O1 Ni1 O2 83.92(19) . . ?
O2 Ni1 O2 180.00(19) 2_665 . ?
O5 Ni1 Ni3 136.98(14) . 2_665 ?
O5 Ni1 Ni3 43.02(14) 2_665 2_665 ?
O1 Ni1 Ni3 43.46(13) 2_665 2_665 ?
O1 Ni1 Ni3 136.54(13) . 2_665 ?
O2 Ni1 Ni3 96.67(13) 2_665 2_665 ?
O2 Ni1 Ni3 83.33(13) . 2_665 ?
O5 Ni1 Ni3 43.02(14) . . ?
O5 Ni1 Ni3 136.98(14) 2_665 . ?
O1 Ni1 Ni3 136.54(13) 2_665 . ?
O1 Ni1 Ni3 43.46(13) . . ?
O2 Ni1 Ni3 83.33(13) 2_665 . ?
O2 Ni1 Ni3 96.67(13) . . ?
Ni3 Ni1 Ni3 180.0 2_665 . ?
O1 Ni2 N1 160.8(2) . . ?
O1 Ni2 O4 79.54(19) . . ?
N1 Ni2 O4 89.8(2) . . ?
O1 Ni2 O8 97.9(2) . . ?
N1 Ni2 O8 93.4(2) . . ?
O4 Ni2 O8 176.2(2) . . ?
O1 Ni2 O9 99.8(2) . . ?
N1 Ni2 O9 96.1(2) . . ?
O4 Ni2 O9 90.2(2) . . ?
O8 Ni2 O9 87.5(2) . . ?
O1 Ni2 O2 83.40(19) . . ?
N1 Ni2 O2 82.6(2) . . ?
O4 Ni2 O2 99.2(2) . . ?
O8 Ni2 O2 83.2(2) . . ?
O9 Ni2 O2 170.5(2) . . ?
O7 Ni3 O5 172.9(2) . . ?
O7 Ni3 O1 101.4(2) . . ?
O5 Ni3 O1 83.9(2) . . ?
O7 Ni3 N2 88.9(2) . . ?
O5 Ni3 N2 85.9(2) . . ?
O1 Ni3 N2 169.6(2) . . ?
O7 Ni3 O3 88.8(2) . 2_665 ?
O5 Ni3 O3 86.4(2) . 2_665 ?
O1 Ni3 O3 90.64(19) . 2_665 ?
N2 Ni3 O3 91.1(2) . 2_665 ?
O7 Ni3 O4 100.1(2) . . ?
O5 Ni3 O4 85.7(2) . . ?
O1 Ni3 O4 75.85(18) . . ?
N2 Ni3 O4 101.0(2) . . ?
O3 Ni3 O4 165.00(19) 2_665 . ?
O7 Ni3 Ni1 140.64(16) . . ?
O5 Ni3 Ni1 42.78(13) . . ?
O1 Ni3 Ni1 43.54(14) . . ?
N2 Ni3 Ni1 127.20(19) . . ?
O3 Ni3 Ni1 76.83(14) 2_665 . ?
O4 Ni3 Ni1 88.74(13) . . ?
Ni2 O1 Ni3 105.0(2) . . ?
Ni2 O1 Ni1 97.9(2) . . ?
Ni3 O1 Ni1 93.0(2) . . ?
Ni2 O1 H1 118.8 . . ?
Ni3 O1 H1 118.8 . . ?
Ni1 O1 H1 118.8 . . ?
C1 O2 Ni1 123.9(5) . . ?
C1 O2 Ni2 121.7(5) . . ?
Ni1 O2 Ni2 94.74(19) . . ?
C1 O3 Ni3 130.0(4) . 2_665 ?
C6 O4 Ni2 120.8(4) . . ?
C6 O4 Ni3 136.6(4) . . ?
Ni2 O4 Ni3 99.3(2) . . ?
C7 O5 Ni1 130.5(5) . . ?
C7 O5 Ni3 134.2(5) . . ?
Ni1 O5 Ni3 94.2(2) . . ?
C12 O7 Ni3 119.8(5) . . ?
C37 O8 Ni2 129.4(5) . . ?
C40 O9 Ni2 119.4(5) . . ?
C4 N1 C3 118.0(6) . . ?
C4 N1 Ni2 121.9(5) . . ?
C3 N1 Ni2 119.4(5) . . ?
C10 N2 C9 118.5(7) . . ?
C10 N2 Ni3 118.3(5) . . ?
C9 N2 Ni3 122.5(5) . . ?
C37 N3 C39 119.7(7) . . ?
C37 N3 C38 121.4(8) . . ?
C39 N3 C38 118.7(8) . . ?
C40 N4 C42 121.1(7) . . ?
C40 N4 C41 121.3(7) . . ?
C42 N4 C41 117.6(8) . . ?
O3 C1 O2 124.5(6) . . ?
O3 C1 C2 118.3(6) . . ?
O2 C1 C2 117.1(7) . . ?
C3 C2 C36 118.8(7) . . ?
C3 C2 C1 125.9(7) . . ?
C36 C2 C1 115.3(7) . . ?
C33 C3 C2 119.1(7) . . ?
C33 C3 N1 119.1(7) . . ?
C2 C3 N1 121.7(7) . . ?
N1 C4 C5 127.1(7) . . ?
N1 C4 H4 116.4 . . ?
C5 C4 H4 116.4 . . ?
C6 C5 C28 120.8(7) . . ?
C6 C5 C4 121.2(7) . . ?
C28 C5 C4 117.6(6) . . ?
O4 C6 C5 124.6(6) . . ?
O4 C6 C25 118.4(6) . . ?
C5 C6 C25 116.9(6) . . ?
O6 C7 O5 123.3(7) . . ?
O6 C7 C8 118.1(7) . . ?
O5 C7 C8 118.6(7) . . ?
C9 C8 C24 119.9(8) . . ?
C9 C8 C7 125.1(7) . . ?
C24 C8 C7 115.0(8) . . ?
C8 C9 N2 124.0(7) . . ?
C8 C9 C21 118.1(7) . . ?
N2 C9 C21 117.9(7) . . ?
N2 C10 C11 127.2(7) . . ?
N2 C10 H10 116.4 . . ?
C11 C10 H10 116.4 . . ?
C12 C11 C10 122.3(7) . . ?
C12 C11 C16 119.3(7) . . ?
C10 C11 C16 118.1(7) . . ?
O7 C12 C11 123.6(7) . . ?
O7 C12 C13 117.6(7) . . ?
C11 C12 C13 118.8(7) . . ?
C14 C13 C12 121.6(8) . . ?
C14 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
C13 C14 C15 122.1(8) . . ?
C13 C14 H14 118.9 . . ?
C15 C14 H14 118.9 . . ?
C14 C15 C16 118.7(7) . . ?
C14 C15 C20 122.4(7) . . ?
C16 C15 C20 118.8(7) . . ?
C17 C16 C15 116.9(7) . . ?
C17 C16 C11 124.0(7) . . ?
C15 C16 C11 119.1(7) . . ?
C18 C17 C16 122.0(8) . . ?
C18 C17 H17 119.0 . . ?
C16 C17 H17 119.0 . . ?
C17 C18 C19 122.2(9) . . ?
C17 C18 H18 118.9 . . ?
C19 C18 H18 118.9 . . ?
C20 C19 C18 119.2(8) . . ?
C20 C19 H19 120.4 . . ?
C18 C19 H19 120.4 . . ?
C19 C20 C15 120.8(8) . . ?
C19 C20 H20 119.6 . . ?
C15 C20 H20 119.6 . . ?
C22 C21 C9 122.1(8) . . ?
C22 C21 H21 119.0 . . ?
C9 C21 H21 119.0 . . ?
C21 C22 C23 118.0(8) . . ?
C21 C22 H22 121.0 . . ?
C23 C22 H22 121.0 . . ?
C24 C23 C22 121.6(8) . . ?
C24 C23 Cl1 118.6(8) . . ?
C22 C23 Cl1 119.8(7) . . ?
C23 C24 C8 119.6(9) . . ?
C23 C24 H24 120.2 . . ?
C8 C24 H24 120.2 . . ?
C26 C25 C6 122.7(7) . . ?
C26 C25 H25 118.6 . . ?
C6 C25 H25 118.6 . . ?
C25 C26 C27 121.1(7) . . ?
C25 C26 H26 119.4 . . ?
C27 C26 H26 119.4 . . ?
C32 C27 C26 121.3(7) . . ?
C32 C27 C28 120.0(7) . . ?
C26 C27 C28 118.7(7) . . ?
C29 C28 C27 116.5(7) . . ?
C29 C28 C5 123.9(7) . . ?
C27 C28 C5 119.6(7) . . ?
C30 C29 C28 122.5(8) . . ?
C30 C29 H29 118.8 . . ?
C28 C29 H29 118.8 . . ?
C29 C30 C31 120.4(8) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
C32 C31 C30 119.8(7) . . ?
C32 C31 H31 120.1 . . ?
C30 C31 H31 120.1 . . ?
C31 C32 C27 120.8(8) . . ?
C31 C32 H32 119.6 . . ?
C27 C32 H32 119.6 . . ?
C34 C33 C3 121.2(9) . . ?
C34 C33 H33 119.4 . . ?
C3 C33 H33 119.4 . . ?
C35 C34 C33 119.4(8) . . ?
C35 C34 H34 120.3 . . ?
C33 C34 H34 120.3 . . ?
C36 C35 C34 121.0(7) . . ?
C36 C35 Cl2 119.1(7) . . ?
C34 C35 Cl2 119.8(6) . . ?
C35 C36 C2 120.5(8) . . ?
C35 C36 H36 119.7 . . ?
C2 C36 H36 119.7 . . ?
O8 C37 N3 123.4(8) . . ?
O8 C37 H37 118.3 . . ?
N3 C37 H37 118.3 . . ?
N3 C38 H38A 109.5 . . ?
N3 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
N3 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N3 C39 H39A 109.5 . . ?
N3 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
N3 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O9 C40 N4 124.2(7) . . ?
O9 C40 H40 117.9 . . ?
N4 C40 H40 117.9 . . ?
N4 C41 H41A 109.5 . . ?
N4 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
N4 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N4 C42 H42A 109.5 . . ?
N4 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N4 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C51 N7 C50 119(3) . . ?
C51 N7 C49 121(3) . . ?
C50 N7 C49 119(3) . . ?
N7 C51 O12 128(3) . . ?
N7 C51 H51 116.1 . . ?
O12 C51 H51 116.1 . . ?
N7 C50 H50A 109.5 . . ?
N7 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
N7 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N7 C49 H49A 109.5 . . ?
N7 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
N7 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
N7 C49 H49D 109.5 . . ?
H49A C49 H49D 141.1 . . ?
H49B C49 H49D 56.3 . . ?
H49C C49 H49D 56.3 . . ?
N7 C49 H49E 109.5 . . ?
H49A C49 H49E 56.3 . . ?
H49B C49 H49E 141.1 . . ?
H49C C49 H49E 56.3 . . ?
H49D C49 H49E 109.5 . . ?
N7 C49 H49F 109.5 . . ?
H49A C49 H49F 56.3 . . ?
H49B C49 H49F 56.3 . . ?
H49C C49 H49F 141.1 . . ?
H49D C49 H49F 109.5 . . ?
H49E C49 H49F 109.5 . . ?
C45 N5 C44 135(3) . . ?
C45 N5 C43 111(3) . . ?
C44 N5 C43 114(3) . . ?
N5 C44 H44A 109.5 . . ?
N5 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
N5 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N5 C45 O10 106(3) . . ?
N5 C45 H45 126.8 . . ?
O10 C45 H45 126.8 . . ?
N5 C43 H43A 109.5 . . ?
N5 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N5 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C48 N6 C47 121(2) . . ?
C48 N6 C46 110(3) . . ?
C47 N6 C46 125(3) . . ?
O11 C48 N6 127(3) . . ?
O11 C48 H48 116.3 . . ?
N6 C48 H48 116.3 . . ?
N6 C47 H47A 109.5 . . ?
N6 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
N6 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
N6 C46 H46A 109.5 . . ?
N6 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
N6 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni3 O3 C1 O2 16.1(11) 2_665 . . . ?
Ni3 O3 C1 C2 -162.2(5) 2_665 . . . ?
Ni1 O2 C1 O3 -13.6(10) . . . . ?
Ni2 O2 C1 O3 -135.8(6) . . . . ?
Ni1 O2 C1 C2 164.7(4) . . . . ?
Ni2 O2 C1 C2 42.5(8) . . . . ?
O3 C1 C2 C3 176.4(7) . . . . ?
O2 C1 C2 C3 -2.0(11) . . . . ?
O3 C1 C2 C36 -5.6(10) . . . . ?
O2 C1 C2 C36 176.0(6) . . . . ?
C36 C2 C3 C33 1.9(12) . . . . ?
C1 C2 C3 C33 179.9(8) . . . . ?
C36 C2 C3 N1 178.3(7) . . . . ?
C1 C2 C3 N1 -3.8(12) . . . . ?
C4 N1 C3 C33 -44.5(11) . . . . ?
Ni2 N1 C3 C33 144.6(7) . . . . ?
C4 N1 C3 C2 139.2(8) . . . . ?
Ni2 N1 C3 C2 -31.8(10) . . . . ?
C3 N1 C4 C5 -175.7(8) . . . . ?
Ni2 N1 C4 C5 -5.0(12) . . . . ?
N1 C4 C5 C6 28.7(13) . . . . ?
N1 C4 C5 C28 -159.0(8) . . . . ?
Ni2 O4 C6 C5 -27.4(9) . . . . ?
Ni3 O4 C6 C5 177.8(5) . . . . ?
Ni2 O4 C6 C25 156.6(5) . . . . ?
Ni3 O4 C6 C25 1.9(11) . . . . ?
C28 C5 C6 O4 178.5(7) . . . . ?
C4 C5 C6 O4 -9.5(12) . . . . ?
C28 C5 C6 C25 -5.5(11) . . . . ?
C4 C5 C6 C25 166.5(7) . . . . ?
Ni1 O5 C7 O6 -4.4(10) . . . . ?
Ni3 O5 C7 O6 -169.1(5) . . . . ?
Ni1 O5 C7 C8 176.9(4) . . . . ?
Ni3 O5 C7 C8 12.1(10) . . . . ?
O6 C7 C8 C9 -175.2(7) . . . . ?
O5 C7 C8 C9 3.7(11) . . . . ?
O6 C7 C8 C24 3.9(10) . . . . ?
O5 C7 C8 C24 -177.3(7) . . . . ?
C24 C8 C9 N2 -171.2(7) . . . . ?
C7 C8 C9 N2 7.8(12) . . . . ?
C24 C8 C9 C21 8.0(11) . . . . ?
C7 C8 C9 C21 -173.0(7) . . . . ?
C10 N2 C9 C8 138.7(8) . . . . ?
Ni3 N2 C9 C8 -31.5(10) . . . . ?
C10 N2 C9 C21 -40.5(10) . . . . ?
Ni3 N2 C9 C21 149.3(6) . . . . ?
C9 N2 C10 C11 175.1(8) . . . . ?
Ni3 N2 C10 C11 -14.3(11) . . . . ?
N2 C10 C11 C12 -17.8(13) . . . . ?
N2 C10 C11 C16 168.1(8) . . . . ?
Ni3 O7 C12 C11 28.7(10) . . . . ?
Ni3 O7 C12 C13 -154.3(6) . . . . ?
C10 C11 C12 O7 9.9(12) . . . . ?
C16 C11 C12 O7 -176.0(7) . . . . ?
C10 C11 C12 C13 -167.0(8) . . . . ?
C16 C11 C12 C13 7.0(11) . . . . ?
O7 C12 C13 C14 178.1(8) . . . . ?
C11 C12 C13 C14 -4.8(12) . . . . ?
C12 C13 C14 C15 -0.3(14) . . . . ?
C13 C14 C15 C16 2.9(13) . . . . ?
C13 C14 C15 C20 -177.1(8) . . . . ?
C14 C15 C16 C17 -178.3(8) . . . . ?
C20 C15 C16 C17 1.7(11) . . . . ?
C14 C15 C16 C11 -0.5(12) . . . . ?
C20 C15 C16 C11 179.5(7) . . . . ?
C12 C11 C16 C17 173.2(8) . . . . ?
C10 C11 C16 C17 -12.6(11) . . . . ?
C12 C11 C16 C15 -4.5(11) . . . . ?
C10 C11 C16 C15 169.8(7) . . . . ?
C15 C16 C17 C18 -3.1(13) . . . . ?
C11 C16 C17 C18 179.2(8) . . . . ?
C16 C17 C18 C19 2.0(15) . . . . ?
C17 C18 C19 C20 0.8(15) . . . . ?
C18 C19 C20 C15 -2.2(14) . . . . ?
C14 C15 C20 C19 -179.1(9) . . . . ?
C16 C15 C20 C19 0.9(13) . . . . ?
C8 C9 C21 C22 -6.6(12) . . . . ?
N2 C9 C21 C22 172.7(8) . . . . ?
C9 C21 C22 C23 -1.1(13) . . . . ?
C21 C22 C23 C24 7.6(14) . . . . ?
C21 C22 C23 Cl1 -173.1(7) . . . . ?
C22 C23 C24 C8 -6.1(14) . . . . ?
Cl1 C23 C24 C8 174.5(6) . . . . ?
C9 C8 C24 C23 -1.9(12) . . . . ?
C7 C8 C24 C23 179.0(8) . . . . ?
O4 C6 C25 C26 178.7(8) . . . . ?
C5 C6 C25 C26 2.5(12) . . . . ?
C6 C25 C26 C27 1.4(13) . . . . ?
C25 C26 C27 C32 176.5(8) . . . . ?
C25 C26 C27 C28 -2.2(12) . . . . ?
C32 C27 C28 C29 -0.6(11) . . . . ?
C26 C27 C28 C29 178.1(7) . . . . ?
C32 C27 C28 C5 -179.6(7) . . . . ?
C26 C27 C28 C5 -0.9(11) . . . . ?
C6 C5 C28 C29 -174.1(8) . . . . ?
C4 C5 C28 C29 13.7(12) . . . . ?
C6 C5 C28 C27 4.9(11) . . . . ?
C4 C5 C28 C27 -167.4(7) . . . . ?
C27 C28 C29 C30 1.3(13) . . . . ?
C5 C28 C29 C30 -179.7(9) . . . . ?
C28 C29 C30 C31 -0.8(14) . . . . ?
C29 C30 C31 C32 -0.5(14) . . . . ?
C30 C31 C32 C27 1.2(13) . . . . ?
C26 C27 C32 C31 -179.3(8) . . . . ?
C28 C27 C32 C31 -0.6(12) . . . . ?
C2 C3 C33 C34 -1.8(14) . . . . ?
N1 C3 C33 C34 -178.3(9) . . . . ?
C3 C33 C34 C35 0.7(15) . . . . ?
C33 C34 C35 C36 0.4(15) . . . . ?
C33 C34 C35 Cl2 179.4(8) . . . . ?
C34 C35 C36 C2 -0.3(13) . . . . ?
Cl2 C35 C36 C2 -179.3(6) . . . . ?
C3 C2 C36 C35 -0.9(12) . . . . ?
C1 C2 C36 C35 -179.1(7) . . . . ?
Ni2 O8 C37 N3 -176.3(6) . . . . ?
C39 N3 C37 O8 -1.2(13) . . . . ?
C38 N3 C37 O8 -176.1(8) . . . . ?
Ni2 O9 C40 N4 174.6(6) . . . . ?
C42 N4 C40 O9 -1.5(12) . . . . ?
C41 N4 C40 O9 178.9(8) . . . . ?
C50 N7 C51 O12 4(5) . . . . ?
C49 N7 C51 O12 -173(4) . . . . ?
C44 N5 C45 O10 -2(5) . . . . ?
C43 N5 C45 O10 -175(3) . . . . ?
C47 N6 C48 O11 178(3) . . . . ?
C46 N6 C48 O11 -25(4) . . . . ?

_refine_diff_density_max         1.699
_refine_diff_density_min         -1.008
_refine_diff_density_rms         0.145

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

data_comp3_rev
_database_code_depnum_ccdc_archive 'CCDC 1448722'
_audit_update_record             
;
2016-05-20 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;

# ========================================================================= #

_audit_creation_method           'SHELXL-2014/7 and enCIFer'
_shelx_SHELXL_version_number     2014/7
_audit_creation_date             '19 May 2016'

# ========================================================================= #


_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C78 H58 Cl5 N5 Ni5 O16, C4 H10 O, 3(C2 H3 N), 4(C H4 O)'
_chemical_formula_sum            'C94 H96 Cl5 N9 Ni5 O21'
_chemical_formula_weight         2158.59

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   17.414(4)
_cell_length_b                   17.728(4)
_cell_length_c                   18.040(4)
_cell_angle_alpha                69.585(9)
_cell_angle_beta                 84.074(9)
_cell_angle_gamma                65.021(9)
_cell_volume                     4724.9(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9304
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      30.64

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_F_000             2232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    1.195
_shelx_estimated_absorpt_T_min   0.708
_shelx_estimated_absorpt_T_max   0.870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_process_details   
; 
'SADABS V2012/1 (Bruker AXS Inc.)' 
;


_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            128931
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.644
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.995


_reflns_number_total             21557
_reflns_number_gt                18848
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 (Bruker AXS Inc., 2012)'
_computing_cell_refinement       'SAINT (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT (Bruker AXS Inc., 2012)'
_computing_structure_solution    'SHELXS (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2014)'


_refine_special_details          
;
Besides several solvent molecules identified and refined in this 
structure, it was not possible to found chemically reasonable 
models to resolve the remaining amount of overlapping electronic 
density. Consequently, the solvent-masking procedure implemented 
in PLATON (SQUEEZE) was utilized, pointing to ca 65 additional 
electrons per formula unit. This evaluation suggest the existence 
of extra solvent that would be 1.5 MeCN and 2 MeOH, which were 
accounted for the terminal refinement cycles and for the final 
molecular formula of the compound: 3*4(MeCN)*4(MeOH)*Et2O
;




_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0963P)²+16.5262P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         21557
_refine_ls_number_parameters     1164
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0401
_refine_ls_wR_factor_ref         0.1227
_refine_ls_wR_factor_gt          0.1134
_refine_ls_goodness_of_fit_ref   0.728
_refine_ls_restrained_S_all      0.728
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.23109(2) 0.39724(2) 0.33057(2) 0.01393(7) Uani 1 1 d . . . . .
Ni2 Ni 0.11241(2) 0.36404(2) 0.47312(2) 0.01472(7) Uani 1 1 d . . . . .
Ni3 Ni 0.41975(2) 0.31075(2) 0.36625(2) 0.01445(7) Uani 1 1 d . . . . .
Ni4 Ni 0.33756(2) 0.51382(2) 0.26939(2) 0.01807(7) Uani 1 1 d . . . . .
Ni5 Ni 0.16092(2) 0.38790(2) 0.16394(2) 0.01484(7) Uani 1 1 d . . . . .
Cl1 Cl 0.10719(4) 0.49750(4) 0.36688(3) 0.02000(12) Uani 1 1 d . . . . .
Cl2 Cl -0.10649(6) 0.17859(7) 0.37089(5) 0.0472(2) Uani 1 1 d . . . . .
Cl3 Cl 0.53990(5) 0.17635(6) 0.02524(4) 0.04131(19) Uani 1 1 d . . . . .
Cl4 Cl 0.04085(6) 0.85031(6) -0.03365(6) 0.0540(2) Uani 1 1 d . . . . .
Cl5 Cl 0.46582(4) 0.04079(6) 0.75218(4) 0.04012(19) Uani 1 1 d . . . . .
O1 O 0.23554(10) 0.31293(11) 0.44480(9) 0.0164(3) Uani 1 1 d . . . . .
O2 O 0.37530(10) 0.23841(11) 0.46474(9) 0.0180(3) Uani 1 1 d . . . . .
O3 O 0.32103(10) 0.42576(11) 0.36958(9) 0.0161(3) Uani 1 1 d . . . . .
O4 O 0.24815(10) 0.48820(11) 0.22747(9) 0.0176(3) Uani 1 1 d . . . . .
O5 O 0.15291(11) 0.51371(11) 0.13873(10) 0.0196(3) Uani 1 1 d . . . . .
O6 O 0.15629(10) 0.35374(11) 0.28492(9) 0.0160(3) Uani 1 1 d . . . . .
O7 O 0.09433(11) 0.31047(12) 0.39626(10) 0.0200(3) Uani 1 1 d . . . . .
O8 O 0.17080(11) 0.40806(11) 0.04723(10) 0.0204(3) Uani 1 1 d . . . . .
O9 O 0.29300(10) 0.32724(11) 0.17768(10) 0.0185(3) Uani 1 1 d . . . . .
O10 O 0.33490(10) 0.30761(11) 0.29873(9) 0.0151(3) Uani 1 1 d . . . . .
O11 O 0.50808(11) 0.29578(11) 0.43856(10) 0.0203(3) Uani 1 1 d . . . . .
O12 O 0.02944(11) 0.45258(12) 0.15372(12) 0.0249(4) Uani 1 1 d D . . . .
H12E H -0.004(2) 0.447(2) 0.1264(19) 0.037 Uiso 1 1 d D U . . .
O13 O 0.44169(11) 0.40522(11) 0.26853(10) 0.0205(3) Uani 1 1 d . . . . .
O14 O 0.41344(14) 0.55324(14) 0.31391(13) 0.0310(4) Uani 1 1 d D . . . .
H14E H 0.453(2) 0.512(2) 0.347(2) 0.047 Uiso 1 1 d D U . . .
O15 O -0.01080(10) 0.40226(11) 0.49142(10) 0.0188(3) Uani 1 1 d . . . . .
O16 O 0.12247(11) 0.42577(12) 0.54888(10) 0.0204(3) Uani 1 1 d D . . . .
H16E H 0.0888(18) 0.4781(13) 0.5309(19) 0.031 Uiso 1 1 d D U . . .
N1 N 0.15523(13) 0.27381(13) 0.17381(11) 0.0174(4) Uani 1 1 d . . . . .
N2 N 0.50243(12) 0.19973(13) 0.34852(11) 0.0160(4) Uani 1 1 d . . . . .
N3 N 0.35409(13) 0.56900(14) 0.15411(13) 0.0214(4) Uani 1 1 d . . . . .
N4 N 0.23100(16) 0.62314(16) 0.28124(14) 0.0297(5) Uani 1 1 d . . . . .
N5 N 0.13785(12) 0.24809(13) 0.56182(11) 0.0167(4) Uani 1 1 d . . . . .
C1 C 0.30215(15) 0.25380(15) 0.48760(13) 0.0159(4) Uani 1 1 d . . . . .
C2 C 0.20216(15) 0.53470(15) 0.16368(14) 0.0172(4) Uani 1 1 d . . . . .
C3 C 0.11099(14) 0.31485(15) 0.32677(13) 0.0165(4) Uani 1 1 d . . . . .
C4 C 0.07311(15) 0.27004(16) 0.29325(14) 0.0185(5) Uani 1 1 d . . . . .
C5 C 0.09737(15) 0.24733(15) 0.22440(14) 0.0182(4) Uani 1 1 d . . . . .
C6 C 0.20033(16) 0.22571(16) 0.13092(14) 0.0201(5) Uani 1 1 d . . . . .
H6 H 0.2056 0.1666 0.1473 0.024 Uiso 1 1 calc R U . . .
C7 C 0.24229(16) 0.25447(17) 0.06151(14) 0.0219(5) Uani 1 1 d . . . . .
C8 C 0.21736(15) 0.34559(17) 0.01936(14) 0.0204(5) Uani 1 1 d . . . . .
C9 C 0.24205(19) 0.3716(2) -0.06100(16) 0.0300(6) Uani 1 1 d . . . . .
H9 H 0.2247 0.4327 -0.0907 0.036 Uiso 1 1 calc R U . . .
C10 C 0.2898(2) 0.3103(2) -0.09497(16) 0.0327(6) Uani 1 1 d . . . . .
H10 H 0.3036 0.3296 -0.1486 0.039 Uiso 1 1 calc R U . . .
C11 C 0.31965(19) 0.2183(2) -0.05281(17) 0.0308(6) Uani 1 1 d . . . . .
C12 C 0.29755(18) 0.18924(19) 0.02646(16) 0.0278(6) Uani 1 1 d . . . . .
C13 C 0.3312(2) 0.0976(2) 0.06779(18) 0.0400(8) Uani 1 1 d . . . . .
H13 H 0.3203 0.0765 0.1221 0.048 Uiso 1 1 calc R U . . .
C14 C 0.3796(3) 0.0380(2) 0.0307(2) 0.0530(10) Uani 1 1 d . . . . .
H14 H 0.4001 -0.0237 0.0593 0.064 Uiso 1 1 calc R U . . .
C15 C 0.3987(2) 0.0671(3) -0.0481(2) 0.0502(9) Uani 1 1 d . . . . .
H15 H 0.4317 0.0255 -0.0733 0.060 Uiso 1 1 calc R U . . .
C16 C 0.3702(2) 0.1550(2) -0.08892(19) 0.0403(7) Uani 1 1 d . . . . .
H16 H 0.3844 0.1746 -0.1425 0.048 Uiso 1 1 calc R U . . .
C17 C 0.05728(18) 0.20323(18) 0.20301(16) 0.0258(5) Uani 1 1 d . . . . .
H17 H 0.0730 0.1881 0.1564 0.031 Uiso 1 1 calc R U . . .
C18 C -0.0042(2) 0.1812(2) 0.24764(17) 0.0309(6) Uani 1 1 d . . . . .
H18 H -0.0300 0.1506 0.2325 0.037 Uiso 1 1 calc R U . . .
C19 C -0.02758(18) 0.2043(2) 0.31474(17) 0.0288(6) Uani 1 1 d . . . . .
C20 C 0.00982(17) 0.24770(18) 0.33767(16) 0.0249(5) Uani 1 1 d . . . . .
H20 H -0.0073 0.2628 0.3842 0.030 Uiso 1 1 calc R U . . .
C21 C 0.34831(14) 0.29536(15) 0.23168(13) 0.0152(4) Uani 1 1 d . . . . .
C22 C 0.43725(15) 0.23804(15) 0.21706(13) 0.0168(4) Uani 1 1 d . . . . .
C23 C 0.50789(15) 0.19195(15) 0.27231(13) 0.0172(4) Uani 1 1 d . . . . .
C24 C 0.54992(14) 0.13314(16) 0.40750(14) 0.0171(4) Uani 1 1 d . . . . .
H24 H 0.5768 0.0772 0.4004 0.021 Uiso 1 1 calc R U . . .
C25 C 0.56510(14) 0.13722(15) 0.48271(13) 0.0165(4) Uani 1 1 d . . . . .
C26 C 0.54915(15) 0.21842(16) 0.49180(14) 0.0182(4) Uani 1 1 d . . . . .
C27 C 0.58131(17) 0.21654(18) 0.56264(16) 0.0243(5) Uani 1 1 d . . . . .
H27 H 0.5734 0.2708 0.5680 0.029 Uiso 1 1 calc R U . . .
C28 C 0.62273(17) 0.13987(18) 0.62230(15) 0.0252(5) Uani 1 1 d . . . . .
H28 H 0.6437 0.1415 0.6680 0.030 Uiso 1 1 calc R U . . .
C29 C 0.63522(15) 0.05744(17) 0.61758(14) 0.0203(5) Uani 1 1 d . . . . .
C30 C 0.60509(15) 0.05573(16) 0.54821(14) 0.0188(5) Uani 1 1 d . . . . .
C31 C 0.61309(16) -0.02699(17) 0.54797(15) 0.0228(5) Uani 1 1 d . . . . .
H31 H 0.5922 -0.0301 0.5030 0.027 Uiso 1 1 calc R U . . .
C32 C 0.65076(18) -0.10331(18) 0.61195(16) 0.0277(6) Uani 1 1 d . . . . .
H32 H 0.6551 -0.1580 0.6104 0.033 Uiso 1 1 calc R U . . .
C33 C 0.68261(18) -0.10112(18) 0.67887(16) 0.0286(6) Uani 1 1 d . . . . .
H33 H 0.7094 -0.1541 0.7221 0.034 Uiso 1 1 calc R U . . .
C34 C 0.67497(17) -0.02229(19) 0.68159(15) 0.0264(5) Uani 1 1 d . . . . .
H34 H 0.6966 -0.0208 0.7270 0.032 Uiso 1 1 calc R U . . .
C35 C 0.58698(16) 0.14411(17) 0.24825(15) 0.0231(5) Uani 1 1 d . . . . .
H35 H 0.6349 0.1144 0.2845 0.028 Uiso 1 1 calc R U . . .
C36 C 0.59724(17) 0.13895(18) 0.17295(16) 0.0264(5) Uani 1 1 d . . . . .
H36 H 0.6515 0.1061 0.1575 0.032 Uiso 1 1 calc R U . . .
C37 C 0.52741(17) 0.18227(18) 0.12049(15) 0.0246(5) Uani 1 1 d . . . . .
C38 C 0.44844(16) 0.23072(17) 0.14138(14) 0.0217(5) Uani 1 1 d . . . . .
H38 H 0.4013 0.2593 0.1044 0.026 Uiso 1 1 calc R U . . .
C39 C -0.02134(18) 0.5078(2) 0.19704(19) 0.0348(7) Uani 1 1 d . . . . .
H39A H -0.0465 0.4751 0.2401 0.052 Uiso 1 1 calc R U . . .
H39B H -0.0666 0.5601 0.1617 0.052 Uiso 1 1 calc R U . . .
H39C H 0.0139 0.5263 0.2193 0.052 Uiso 1 1 calc R U . . .
C40 C 0.20626(16) 0.62175(16) 0.11429(14) 0.0205(5) Uani 1 1 d . . . . .
C41 C 0.28001(16) 0.63598(17) 0.10781(15) 0.0225(5) Uani 1 1 d . . . . .
C42 C 0.42378(17) 0.54288(17) 0.11831(15) 0.0237(5) Uani 1 1 d . . . . .
H42 H 0.4220 0.5730 0.0630 0.028 Uiso 1 1 calc R U . . .
C43 C 0.50343(16) 0.47265(18) 0.15435(15) 0.0223(5) Uani 1 1 d . . . . .
C44 C 0.50865(16) 0.40598(17) 0.22777(15) 0.0203(5) Uani 1 1 d . . . . .
C45 C 0.58924(17) 0.33532(18) 0.25787(16) 0.0259(5) Uani 1 1 d . . . . .
H45 H 0.5934 0.2910 0.3077 0.031 Uiso 1 1 calc R U . . .
C46 C 0.66024(17) 0.32997(19) 0.21674(17) 0.0288(6) Uani 1 1 d . . . . .
H46 H 0.7128 0.2816 0.2383 0.035 Uiso 1 1 calc R U . . .
C47 C 0.65788(17) 0.39468(19) 0.14259(16) 0.0264(5) Uani 1 1 d . . . . .
C48 C 0.57955(17) 0.46754(18) 0.11099(15) 0.0245(5) Uani 1 1 d . . . . .
C49 C 0.58017(19) 0.5337(2) 0.03849(17) 0.0309(6) Uani 1 1 d . . . . .
H49 H 0.5287 0.5833 0.0160 0.037 Uiso 1 1 calc R U . . .
C50 C 0.6547(2) 0.5267(2) 0.00039(17) 0.0345(7) Uani 1 1 d . . . . .
H50 H 0.6537 0.5715 -0.0480 0.041 Uiso 1 1 calc R U . . .
C51 C 0.73141(19) 0.4545(2) 0.03216(18) 0.0330(6) Uani 1 1 d . . . . .
H51 H 0.7822 0.4504 0.0055 0.040 Uiso 1 1 calc R U . . .
C52 C 0.73302(18) 0.3895(2) 0.10194(18) 0.0311(6) Uani 1 1 d . . . . .
H52 H 0.7852 0.3404 0.1233 0.037 Uiso 1 1 calc R U . . .
C53 C 0.2792(2) 0.71657(19) 0.05719(18) 0.0328(6) Uani 1 1 d . . . . .
H53 H 0.3296 0.7261 0.0525 0.039 Uiso 1 1 calc R U . . .
C54 C 0.2061(2) 0.7827(2) 0.0139(2) 0.0412(8) Uani 1 1 d . . . . .
H54 H 0.2059 0.8375 -0.0203 0.049 Uiso 1 1 calc R U . . .
C55 C 0.13348(19) 0.76823(19) 0.02088(18) 0.0339(6) Uani 1 1 d . . . . .
C56 C 0.13244(17) 0.68865(17) 0.07048(15) 0.0243(5) Uani 1 1 d . . . . .
H56 H 0.0818 0.6798 0.0746 0.029 Uiso 1 1 calc R U . . .
C57 C 0.3809(4) 0.6320(3) 0.3357(4) 0.0741(14) Uani 1 1 d . . . . .
H57A H 0.3465 0.6831 0.2911 0.111 Uiso 1 1 calc R U . . .
H57B H 0.4284 0.6415 0.3493 0.111 Uiso 1 1 calc R U . . .
H57C H 0.3459 0.6247 0.3815 0.111 Uiso 1 1 calc R U . . .
C58 C 0.1607(2) 0.6708(2) 0.27565(19) 0.0432(8) Uani 1 1 d . . . . .
C59 C 0.0693(3) 0.7263(3) 0.2673(3) 0.0697(13) Uani 1 1 d . . . . .
H59A H 0.0478 0.7392 0.2141 0.104 Uiso 1 1 calc R U . . .
H59B H 0.0587 0.7817 0.2752 0.104 Uiso 1 1 calc R U . . .
H59C H 0.0403 0.6950 0.3069 0.104 Uiso 1 1 calc R U . . .
C60 C 0.31013(18) 0.44609(18) 0.44092(15) 0.0258(5) Uani 1 1 d . . . . .
H60A H 0.3634 0.4436 0.4573 0.039 Uiso 1 1 calc R U . . .
H60B H 0.2943 0.4030 0.4827 0.039 Uiso 1 1 calc R U . . .
H60C H 0.2653 0.5056 0.4318 0.039 Uiso 1 1 calc R U . . .
C61 C 0.29349(15) 0.20025(15) 0.57135(14) 0.0178(4) Uani 1 1 d . . . . .
C62 C 0.21712(15) 0.19973(16) 0.60580(14) 0.0188(5) Uani 1 1 d . . . . .
C63 C 0.08264(15) 0.21379(16) 0.57949(14) 0.0197(5) Uani 1 1 d . . . . .
H63 H 0.1018 0.1551 0.6161 0.024 Uiso 1 1 calc R U . . .
C64 C -0.00382(15) 0.25450(16) 0.54991(14) 0.0194(5) Uani 1 1 d . . . . .
C65 C -0.04652(15) 0.34728(17) 0.51079(14) 0.0197(5) Uani 1 1 d . . . . .
C66 C -0.13593(17) 0.38436(19) 0.49334(19) 0.0312(6) Uani 1 1 d . . . . .
H66 H -0.1653 0.4463 0.4678 0.037 Uiso 1 1 calc R U . . .
C67 C -0.17948(18) 0.3332(2) 0.5125(2) 0.0381(7) Uani 1 1 d . . . . .
H67 H -0.2389 0.3604 0.5004 0.046 Uiso 1 1 calc R U . . .
C68 C -0.13941(18) 0.2403(2) 0.54986(19) 0.0310(6) Uani 1 1 d . . . . .
C69 C -0.05135(17) 0.19989(18) 0.56840(16) 0.0253(5) Uani 1 1 d . . . . .
C70 C -0.0139(2) 0.1068(2) 0.6037(2) 0.0381(7) Uani 1 1 d . . . . .
H70 H 0.0455 0.0768 0.6158 0.046 Uiso 1 1 calc R U . . .
C71 C -0.0624(2) 0.0586(2) 0.6209(3) 0.0526(10) Uani 1 1 d . . . . .
H71 H -0.0356 -0.0039 0.6448 0.063 Uiso 1 1 calc R U . . .
C72 C -0.1491(2) 0.0995(2) 0.6039(3) 0.0523(10) Uani 1 1 d . . . . .
H72 H -0.1818 0.0655 0.6170 0.063 Uiso 1 1 calc R U . . .
C73 C -0.1871(2) 0.1886(2) 0.5684(2) 0.0443(8) Uani 1 1 d . . . . .
H73 H -0.2464 0.2168 0.5557 0.053 Uiso 1 1 calc R U . . .
C74 C 0.21999(16) 0.15233(17) 0.68689(15) 0.0236(5) Uani 1 1 d . . . . .
H74 H 0.1686 0.1539 0.7112 0.028 Uiso 1 1 calc R U . . .
C75 C 0.29505(18) 0.10368(19) 0.73228(15) 0.0281(6) Uani 1 1 d . . . . .
H75 H 0.2954 0.0721 0.7871 0.034 Uiso 1 1 calc R U . . .
C76 C 0.37003(17) 0.10151(18) 0.69673(15) 0.0257(5) Uani 1 1 d . . . . .
C77 C 0.36933(16) 0.14876(17) 0.61757(14) 0.0222(5) Uani 1 1 d . . . . .
H77 H 0.4214 0.1463 0.5941 0.027 Uiso 1 1 calc R U . . .
C78 C 0.1137(2) 0.3940(2) 0.63275(17) 0.0392(7) Uani 1 1 d . . . . .
H78A H 0.0698 0.3713 0.6434 0.059 Uiso 1 1 calc R U . . .
H78B H 0.0975 0.4425 0.6536 0.059 Uiso 1 1 calc R U . . .
H78C H 0.1678 0.3465 0.6586 0.059 Uiso 1 1 calc R U . . .
N6 N 0.2352(2) -0.0312(3) 0.6116(2) 0.0759(13) Uani 1 1 d . . . . .
C80 C 0.2046(2) 0.0109(3) 0.5503(2) 0.0462(8) Uani 1 1 d . . . . .
C81 C 0.1643(2) 0.0677(3) 0.4721(2) 0.0493(9) Uani 1 1 d . . . . .
H81A H 0.1502 0.1294 0.4655 0.074 Uiso 1 1 calc R U . . .
H81B H 0.1122 0.0612 0.4664 0.074 Uiso 1 1 calc R U . . .
H81C H 0.2031 0.0508 0.4316 0.074 Uiso 1 1 calc R U . . .
N7 N 0.4110(7) 0.8069(7) 0.1742(4) 0.159(3) Uani 1 1 d . . . . .
C82 C 0.4578(6) 0.7438(5) 0.1734(4) 0.0461(17) Uani 0.5 1 d . . P . .
C83 C 0.5165(5) 0.6647(5) 0.1754(4) 0.0454(16) Uani 0.5 1 d . . P . .
H83A H 0.5359 0.6675 0.1219 0.068 Uiso 0.5 1 calc R U P . .
H83B H 0.4921 0.6210 0.1949 0.068 Uiso 0.5 1 calc R U P . .
H83C H 0.5646 0.6475 0.2107 0.068 Uiso 0.5 1 calc R U P . .
O17 O 0.93567(14) 0.44099(15) 0.05863(13) 0.0368(5) Uani 1 1 d . . . . .
H17A H 0.9052 0.4887 0.0241 0.044 Uiso 1 1 calc R U . . .
C79 C 0.9853(2) 0.3789(2) 0.0216(2) 0.0429(8) Uani 1 1 d . . . . .
H79A H 1.0456 0.3611 0.0327 0.064 Uiso 1 1 calc R U . . .
H79B H 0.9725 0.4057 -0.0357 0.064 Uiso 1 1 calc R U . . .
H79C H 0.9724 0.3269 0.0422 0.064 Uiso 1 1 calc R U . . .
O18 O 0.6955(4) 0.5676(4) 0.2989(3) 0.1294(19) Uani 1 1 d . . . . .
C86 C 0.7776(6) 0.4424(6) 0.2684(5) 0.113(2) Uani 1 1 d . . . . .
C87 C 0.6049(7) 0.6851(6) 0.3449(6) 0.151(4) Uani 1 1 d . . . . .
C88 C 0.7733(5) 0.5138(7) 0.2853(4) 0.067(3) Uani 0.5 1 d . . P A 1
C89 C 0.6853(6) 0.6377(7) 0.3330(6) 0.061(2) Uani 0.5 1 d . . P A 1
C88B C 0.6932(8) 0.4747(9) 0.3266(10) 0.104(5) Uani 0.5 1 d . . P A 2
C89B C 0.5990(12) 0.6505(11) 0.2893(15) 0.159(9) Uani 0.5 1 d . . P A 2
O19 O 0.5173(3) 0.4388(3) 0.4300(2) 0.0280(8) Uiso 0.5 1 d D . P B 1
C90 C 0.6049(6) 0.4271(6) 0.4092(5) 0.057(2) Uiso 0.5 1 d D . P B 1
O20 O 0.5553(4) 0.4265(4) 0.4024(4) 0.0598(14) Uiso 0.5 1 d D . P C 2
C91 C 0.5632(9) 0.4496(9) 0.4625(8) 0.094(4) Uiso 0.5 1 d D . P C 2
C85 C 0.1684(6) 0.9625(7) 0.1648(6) 0.126(3) Uiso 1 1 d . . . . .
N11 N 0.1638(8) 1.0280(9) 0.1447(7) 0.210(5) Uiso 1 1 d . . . . .
C84 C 0.1788(11) 0.8772(11) 0.1890(10) 0.257(8) Uiso 1 1 d . . . . .
H84A H 0.1398 0.8718 0.1577 0.385 Uiso 1 1 calc R U . . .
H84B H 0.1668 0.8584 0.2452 0.385 Uiso 1 1 calc R U . . .
H84C H 0.2374 0.8396 0.1818 0.385 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O10 2.0295(16) . ?
Ni1 O1 2.0671(16) . ?
Ni1 O4 2.0847(16) . ?
Ni1 O3 2.0854(17) . ?
Ni1 O6 2.1170(17) . ?
Ni1 Cl1 2.3505(7) . ?
Ni2 O15 1.9884(17) . ?
Ni2 N5 2.016(2) . ?
Ni2 O1 2.0337(17) . ?
Ni2 O7 2.0456(18) . ?
Ni2 O16 2.0860(18) . ?
Ni2 Cl1 2.4435(8) . ?
Ni3 O11 1.9916(18) . ?
Ni3 N2 2.000(2) . ?
Ni3 O10 2.0391(17) . ?
Ni3 O3 2.0542(17) . ?
Ni3 O2 2.0893(16) . ?
Ni3 O13 2.0976(17) . ?
Ni4 N3 2.015(2) . ?
Ni4 O13 2.0154(18) . ?
Ni4 O3 2.0225(16) . ?
Ni4 O14 2.066(2) . ?
Ni4 O4 2.0695(17) . ?
Ni4 N4 2.101(2) . ?
Ni5 O8 2.0105(17) . ?
Ni5 N1 2.012(2) . ?
Ni5 O6 2.0542(16) . ?
Ni5 O5 2.0600(18) . ?
Ni5 O12 2.0769(19) . ?
Ni5 O9 2.0858(17) . ?
Cl2 C19 1.744(3) . ?
Cl3 C37 1.744(3) . ?
Cl4 C55 1.742(3) . ?
Cl5 C76 1.738(3) . ?
O1 C1 1.278(3) . ?
O2 C1 1.243(3) . ?
O3 C60 1.428(3) . ?
O4 C2 1.271(3) . ?
O5 C2 1.242(3) . ?
O6 C3 1.281(3) . ?
O7 C3 1.240(3) . ?
O8 C8 1.297(3) . ?
O9 C21 1.243(3) . ?
O10 C21 1.283(3) . ?
O11 C26 1.307(3) . ?
O12 C39 1.418(3) . ?
O12 H12E 0.851(18) . ?
O13 C44 1.315(3) . ?
O14 C57 1.447(5) . ?
O14 H14E 0.844(19) . ?
O15 C65 1.299(3) . ?
O16 C78 1.435(3) . ?
O16 H16E 0.825(18) . ?
N1 C6 1.308(3) . ?
N1 C5 1.407(3) . ?
N2 C24 1.300(3) . ?
N2 C23 1.419(3) . ?
N3 C42 1.295(3) . ?
N3 C41 1.417(3) . ?
N4 C58 1.148(4) . ?
N5 C63 1.300(3) . ?
N5 C62 1.422(3) . ?
C1 C61 1.510(3) . ?
C2 C40 1.517(3) . ?
C3 C4 1.514(3) . ?
C4 C20 1.407(3) . ?
C4 C5 1.407(3) . ?
C5 C17 1.405(4) . ?
C6 C7 1.429(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.412(4) . ?
C7 C12 1.452(4) . ?
C8 C9 1.439(3) . ?
C9 C10 1.359(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.417(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.414(4) . ?
C11 C16 1.419(4) . ?
C12 C13 1.407(4) . ?
C13 C14 1.378(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.391(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.356(5) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.380(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.380(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.373(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.508(3) . ?
C22 C38 1.402(3) . ?
C22 C23 1.418(3) . ?
C23 C35 1.397(3) . ?
C24 C25 1.440(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.412(3) . ?
C25 C30 1.448(3) . ?
C26 C27 1.432(3) . ?
C27 C28 1.356(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.416(4) . ?
C28 H28 0.9500 . ?
C29 C34 1.418(4) . ?
C29 C30 1.420(3) . ?
C30 C31 1.415(4) . ?
C31 C32 1.382(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.399(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.365(4) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C36 1.381(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.381(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.376(4) . ?
C38 H38 0.9500 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.396(4) . ?
C40 C56 1.397(4) . ?
C41 C53 1.397(4) . ?
C42 C43 1.435(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.415(3) . ?
C43 C48 1.453(3) . ?
C44 C45 1.425(4) . ?
C45 C46 1.360(4) . ?
C45 H45 0.9500 . ?
C46 C47 1.417(4) . ?
C46 H46 0.9500 . ?
C47 C52 1.416(4) . ?
C47 C48 1.419(4) . ?
C48 C49 1.423(4) . ?
C49 C50 1.382(4) . ?
C49 H49 0.9500 . ?
C50 C51 1.398(5) . ?
C50 H50 0.9500 . ?
C51 C52 1.371(4) . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
C53 C54 1.383(4) . ?
C53 H53 0.9500 . ?
C54 C55 1.378(5) . ?
C54 H54 0.9500 . ?
C55 C56 1.389(4) . ?
C56 H56 0.9500 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 C59 1.465(6) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C77 1.397(3) . ?
C61 C62 1.411(3) . ?
C62 C74 1.404(3) . ?
C63 C64 1.432(3) . ?
C63 H63 0.9500 . ?
C64 C65 1.422(3) . ?
C64 C69 1.459(3) . ?
C65 C66 1.431(4) . ?
C66 C67 1.351(4) . ?
C66 H66 0.9500 . ?
C67 C68 1.416(4) . ?
C67 H67 0.9500 . ?
C68 C69 1.410(4) . ?
C68 C73 1.418(4) . ?
C69 C70 1.414(4) . ?
C70 C71 1.381(4) . ?
C70 H70 0.9500 . ?
C71 C72 1.385(5) . ?
C71 H71 0.9500 . ?
C72 C73 1.359(5) . ?
C72 H72 0.9500 . ?
C73 H73 0.9500 . ?
C74 C75 1.378(4) . ?
C74 H74 0.9500 . ?
C75 C76 1.385(4) . ?
C75 H75 0.9500 . ?
C76 C77 1.379(3) . ?
C77 H77 0.9500 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
N6 C80 1.129(5) . ?
C80 C81 1.454(5) . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
N7 C82 1.074(11) . ?
C82 C83 1.331(11) . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
O17 C79 1.412(4) . ?
O17 H17A 0.8400 . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
O18 C88 1.344(9) . ?
O18 C89 1.509(11) . ?
O18 C88B 1.562(13) . ?
O18 C89B 1.676(18) . ?
C86 C88 1.375(13) . ?
C86 C88B 1.726(16) . ?
C87 C89 1.335(13) . ?
C87 C89B 1.38(2) . ?
O19 C90 1.475(9) . ?
O20 C91 1.323(12) . ?
C85 N11 1.058(13) . ?
C85 C84 1.356(16) . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 Ni1 O1 94.43(7) . . ?
O10 Ni1 O4 84.33(7) . . ?
O1 Ni1 O4 165.79(7) . . ?
O10 Ni1 O3 83.13(7) . . ?
O1 Ni1 O3 87.61(7) . . ?
O4 Ni1 O3 78.18(7) . . ?
O10 Ni1 O6 87.82(7) . . ?
O1 Ni1 O6 93.37(7) . . ?
O4 Ni1 O6 100.71(7) . . ?
O3 Ni1 O6 170.95(6) . . ?
O10 Ni1 Cl1 177.32(5) . . ?
O1 Ni1 Cl1 84.95(5) . . ?
O4 Ni1 Cl1 96.91(5) . . ?
O3 Ni1 Cl1 99.43(5) . . ?
O6 Ni1 Cl1 89.61(5) . . ?
O15 Ni2 N5 90.34(8) . . ?
O15 Ni2 O1 170.46(7) . . ?
N5 Ni2 O1 87.82(7) . . ?
O15 Ni2 O7 87.13(7) . . ?
N5 Ni2 O7 89.47(8) . . ?
O1 Ni2 O7 83.50(7) . . ?
O15 Ni2 O16 89.62(7) . . ?
N5 Ni2 O16 92.86(8) . . ?
O1 Ni2 O16 99.82(7) . . ?
O7 Ni2 O16 176.01(7) . . ?
O15 Ni2 Cl1 99.04(5) . . ?
N5 Ni2 Cl1 170.37(6) . . ?
O1 Ni2 Cl1 83.27(5) . . ?
O7 Ni2 Cl1 93.14(5) . . ?
O16 Ni2 Cl1 85.09(5) . . ?
O11 Ni3 N2 87.73(8) . . ?
O11 Ni3 O10 172.09(7) . . ?
N2 Ni3 O10 86.12(7) . . ?
O11 Ni3 O3 102.56(7) . . ?
N2 Ni3 O3 169.68(7) . . ?
O10 Ni3 O3 83.68(7) . . ?
O11 Ni3 O2 87.92(7) . . ?
N2 Ni3 O2 91.13(7) . . ?
O10 Ni3 O2 87.23(7) . . ?
O3 Ni3 O2 89.95(7) . . ?
O11 Ni3 O13 95.70(7) . . ?
N2 Ni3 O13 100.06(8) . . ?
O10 Ni3 O13 90.28(7) . . ?
O3 Ni3 O13 78.47(7) . . ?
O2 Ni3 O13 168.36(7) . . ?
N3 Ni4 O13 87.35(8) . . ?
N3 Ni4 O3 159.33(8) . . ?
O13 Ni4 O3 81.14(7) . . ?
N3 Ni4 O14 96.46(9) . . ?
O13 Ni4 O14 88.57(8) . . ?
O3 Ni4 O14 100.33(8) . . ?
N3 Ni4 O4 84.98(8) . . ?
O13 Ni4 O4 98.93(7) . . ?
O3 Ni4 O4 79.96(7) . . ?
O14 Ni4 O4 172.43(8) . . ?
N3 Ni4 N4 97.36(9) . . ?
O13 Ni4 N4 174.90(8) . . ?
O3 Ni4 N4 94.92(8) . . ?
O14 Ni4 N4 88.97(9) . . ?
O4 Ni4 N4 83.48(9) . . ?
O8 Ni5 N1 86.38(8) . . ?
O8 Ni5 O6 174.16(7) . . ?
N1 Ni5 O6 88.42(7) . . ?
O8 Ni5 O5 87.24(7) . . ?
N1 Ni5 O5 170.83(7) . . ?
O6 Ni5 O5 98.23(7) . . ?
O8 Ni5 O12 93.14(7) . . ?
N1 Ni5 O12 90.77(8) . . ?
O6 Ni5 O12 89.58(7) . . ?
O5 Ni5 O12 83.00(7) . . ?
O8 Ni5 O9 88.86(7) . . ?
N1 Ni5 O9 91.77(8) . . ?
O6 Ni5 O9 88.65(6) . . ?
O5 Ni5 O9 94.68(7) . . ?
O12 Ni5 O9 176.86(7) . . ?
Ni1 Cl1 Ni2 83.04(3) . . ?
C1 O1 Ni2 130.90(15) . . ?
C1 O1 Ni1 126.68(14) . . ?
Ni2 O1 Ni1 101.64(7) . . ?
C1 O2 Ni3 130.54(15) . . ?
C60 O3 Ni4 117.92(15) . . ?
C60 O3 Ni3 118.67(15) . . ?
Ni4 O3 Ni3 100.59(7) . . ?
C60 O3 Ni1 120.22(15) . . ?
Ni4 O3 Ni1 101.70(7) . . ?
Ni3 O3 Ni1 93.24(7) . . ?
C2 O4 Ni4 126.54(15) . . ?
C2 O4 Ni1 130.65(15) . . ?
Ni4 O4 Ni1 100.16(7) . . ?
C2 O5 Ni5 126.89(15) . . ?
C3 O6 Ni5 124.37(15) . . ?
C3 O6 Ni1 124.45(15) . . ?
Ni5 O6 Ni1 111.10(7) . . ?
C3 O7 Ni2 135.95(16) . . ?
C8 O8 Ni5 122.71(15) . . ?
C21 O9 Ni5 137.76(15) . . ?
C21 O10 Ni1 128.29(15) . . ?
C21 O10 Ni3 126.09(14) . . ?
Ni1 O10 Ni3 95.38(7) . . ?
C26 O11 Ni3 119.49(15) . . ?
C39 O12 Ni5 125.50(17) . . ?
C39 O12 H12E 108(3) . . ?
Ni5 O12 H12E 126(2) . . ?
C44 O13 Ni4 124.89(16) . . ?
C44 O13 Ni3 133.88(16) . . ?
Ni4 O13 Ni3 99.37(7) . . ?
C57 O14 Ni4 123.5(3) . . ?
C57 O14 H14E 110(3) . . ?
Ni4 O14 H14E 115(3) . . ?
C65 O15 Ni2 121.92(15) . . ?
C78 O16 Ni2 122.92(18) . . ?
C78 O16 H16E 109(2) . . ?
Ni2 O16 H16E 107(2) . . ?
C6 N1 C5 118.6(2) . . ?
C6 N1 Ni5 121.87(17) . . ?
C5 N1 Ni5 119.44(16) . . ?
C24 N2 C23 119.5(2) . . ?
C24 N2 Ni3 120.02(16) . . ?
C23 N2 Ni3 120.43(15) . . ?
C42 N3 C41 118.2(2) . . ?
C42 N3 Ni4 125.65(18) . . ?
C41 N3 Ni4 115.84(16) . . ?
C58 N4 Ni4 156.5(3) . . ?
C63 N5 C62 117.6(2) . . ?
C63 N5 Ni2 120.81(17) . . ?
C62 N5 Ni2 121.60(16) . . ?
O2 C1 O1 123.5(2) . . ?
O2 C1 C61 117.0(2) . . ?
O1 C1 C61 119.5(2) . . ?
O5 C2 O4 124.1(2) . . ?
O5 C2 C40 117.0(2) . . ?
O4 C2 C40 118.9(2) . . ?
O7 C3 O6 124.2(2) . . ?
O7 C3 C4 114.7(2) . . ?
O6 C3 C4 121.1(2) . . ?
C20 C4 C5 118.6(2) . . ?
C20 C4 C3 115.4(2) . . ?
C5 C4 C3 125.9(2) . . ?
C17 C5 N1 119.7(2) . . ?
C17 C5 C4 118.5(2) . . ?
N1 C5 C4 121.6(2) . . ?
N1 C6 C7 125.6(2) . . ?
N1 C6 H6 117.2 . . ?
C7 C6 H6 117.2 . . ?
C8 C7 C6 120.4(2) . . ?
C8 C7 C12 120.3(2) . . ?
C6 C7 C12 118.1(2) . . ?
O8 C8 C7 124.3(2) . . ?
O8 C8 C9 117.4(2) . . ?
C7 C8 C9 118.2(2) . . ?
C10 C9 C8 121.0(3) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C9 C10 C11 122.0(3) . . ?
C9 C10 H10 119.0 . . ?
C11 C10 H10 119.0 . . ?
C12 C11 C10 119.1(3) . . ?
C12 C11 C16 119.5(3) . . ?
C10 C11 C16 121.3(3) . . ?
C13 C12 C11 117.8(3) . . ?
C13 C12 C7 123.2(2) . . ?
C11 C12 C7 119.1(3) . . ?
C14 C13 C12 121.1(3) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 C15 120.7(3) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C16 C15 C14 119.9(3) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C15 C16 C11 120.9(3) . . ?
C15 C16 H16 119.5 . . ?
C11 C16 H16 119.5 . . ?
C18 C17 C5 122.1(3) . . ?
C18 C17 H17 119.0 . . ?
C5 C17 H17 119.0 . . ?
C19 C18 C17 118.7(3) . . ?
C19 C18 H18 120.7 . . ?
C17 C18 H18 120.7 . . ?
C20 C19 C18 121.2(2) . . ?
C20 C19 Cl2 119.6(2) . . ?
C18 C19 Cl2 119.2(2) . . ?
C19 C20 C4 120.9(2) . . ?
C19 C20 H20 119.5 . . ?
C4 C20 H20 119.5 . . ?
O9 C21 O10 124.6(2) . . ?
O9 C21 C22 117.4(2) . . ?
O10 C21 C22 118.0(2) . . ?
C38 C22 C23 118.8(2) . . ?
C38 C22 C21 115.1(2) . . ?
C23 C22 C21 126.1(2) . . ?
C35 C23 C22 118.8(2) . . ?
C35 C23 N2 118.9(2) . . ?
C22 C23 N2 122.0(2) . . ?
N2 C24 C25 125.3(2) . . ?
N2 C24 H24 117.3 . . ?
C25 C24 H24 117.3 . . ?
C26 C25 C24 121.3(2) . . ?
C26 C25 C30 119.2(2) . . ?
C24 C25 C30 119.2(2) . . ?
O11 C26 C25 124.0(2) . . ?
O11 C26 C27 117.6(2) . . ?
C25 C26 C27 118.4(2) . . ?
C28 C27 C26 122.1(2) . . ?
C28 C27 H27 118.9 . . ?
C26 C27 H27 118.9 . . ?
C27 C28 C29 121.1(2) . . ?
C27 C28 H28 119.5 . . ?
C29 C28 H28 119.5 . . ?
C28 C29 C34 121.0(2) . . ?
C28 C29 C30 118.9(2) . . ?
C34 C29 C30 120.0(2) . . ?
C31 C30 C29 117.3(2) . . ?
C31 C30 C25 122.8(2) . . ?
C29 C30 C25 119.9(2) . . ?
C32 C31 C30 121.2(2) . . ?
C32 C31 H31 119.4 . . ?
C30 C31 H31 119.4 . . ?
C31 C32 C33 120.9(3) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 H32 119.6 . . ?
C34 C33 C32 119.5(2) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
C33 C34 C29 121.0(2) . . ?
C33 C34 H34 119.5 . . ?
C29 C34 H34 119.5 . . ?
C36 C35 C23 121.6(2) . . ?
C36 C35 H35 119.2 . . ?
C23 C35 H35 119.2 . . ?
C37 C36 C35 118.9(2) . . ?
C37 C36 H36 120.5 . . ?
C35 C36 H36 120.5 . . ?
C38 C37 C36 121.5(2) . . ?
C38 C37 Cl3 119.3(2) . . ?
C36 C37 Cl3 119.2(2) . . ?
C37 C38 C22 120.3(2) . . ?
C37 C38 H38 119.9 . . ?
C22 C38 H38 119.9 . . ?
O12 C39 H39A 109.5 . . ?
O12 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
O12 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C41 C40 C56 119.5(2) . . ?
C41 C40 C2 123.5(2) . . ?
C56 C40 C2 116.9(2) . . ?
C40 C41 C53 119.6(2) . . ?
C40 C41 N3 119.4(2) . . ?
C53 C41 N3 121.0(2) . . ?
N3 C42 C43 126.1(2) . . ?
N3 C42 H42 116.9 . . ?
C43 C42 H42 116.9 . . ?
C44 C43 C42 121.8(2) . . ?
C44 C43 C48 119.7(2) . . ?
C42 C43 C48 118.3(2) . . ?
O13 C44 C43 122.6(2) . . ?
O13 C44 C45 118.5(2) . . ?
C43 C44 C45 118.9(2) . . ?
C46 C45 C44 121.4(2) . . ?
C46 C45 H45 119.3 . . ?
C44 C45 H45 119.3 . . ?
C45 C46 C47 121.7(3) . . ?
C45 C46 H46 119.1 . . ?
C47 C46 H46 119.1 . . ?
C52 C47 C46 120.9(3) . . ?
C52 C47 C48 120.0(3) . . ?
C46 C47 C48 119.1(2) . . ?
C47 C48 C49 117.7(2) . . ?
C47 C48 C43 119.2(2) . . ?
C49 C48 C43 123.1(3) . . ?
C50 C49 C48 120.9(3) . . ?
C50 C49 H49 119.6 . . ?
C48 C49 H49 119.6 . . ?
C49 C50 C51 120.9(3) . . ?
C49 C50 H50 119.6 . . ?
C51 C50 H50 119.6 . . ?
C52 C51 C50 119.7(3) . . ?
C52 C51 H51 120.1 . . ?
C50 C51 H51 120.1 . . ?
C51 C52 C47 120.9(3) . . ?
C51 C52 H52 119.6 . . ?
C47 C52 H52 119.6 . . ?
C54 C53 C41 120.8(3) . . ?
C54 C53 H53 119.6 . . ?
C41 C53 H53 119.6 . . ?
C55 C54 C53 119.2(3) . . ?
C55 C54 H54 120.4 . . ?
C53 C54 H54 120.4 . . ?
C54 C55 C56 121.3(3) . . ?
C54 C55 Cl4 120.0(2) . . ?
C56 C55 Cl4 118.7(2) . . ?
C55 C56 C40 119.6(3) . . ?
C55 C56 H56 120.2 . . ?
C40 C56 H56 120.2 . . ?
O14 C57 H57A 109.5 . . ?
O14 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
O14 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
N4 C58 C59 175.3(4) . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
O3 C60 H60A 109.5 . . ?
O3 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
O3 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C77 C61 C62 118.9(2) . . ?
C77 C61 C1 115.0(2) . . ?
C62 C61 C1 126.1(2) . . ?
C74 C62 C61 118.3(2) . . ?
C74 C62 N5 119.6(2) . . ?
C61 C62 N5 122.1(2) . . ?
N5 C63 C64 127.3(2) . . ?
N5 C63 H63 116.3 . . ?
C64 C63 H63 116.3 . . ?
C65 C64 C63 121.9(2) . . ?
C65 C64 C69 119.4(2) . . ?
C63 C64 C69 118.3(2) . . ?
O15 C65 C64 124.8(2) . . ?
O15 C65 C66 116.8(2) . . ?
C64 C65 C66 118.4(2) . . ?
C67 C66 C65 121.5(3) . . ?
C67 C66 H66 119.3 . . ?
C65 C66 H66 119.3 . . ?
C66 C67 C68 122.1(3) . . ?
C66 C67 H67 118.9 . . ?
C68 C67 H67 118.9 . . ?
C69 C68 C67 119.0(3) . . ?
C69 C68 C73 120.4(3) . . ?
C67 C68 C73 120.5(3) . . ?
C68 C69 C70 116.9(3) . . ?
C68 C69 C64 119.5(2) . . ?
C70 C69 C64 123.6(3) . . ?
C71 C70 C69 121.1(3) . . ?
C71 C70 H70 119.5 . . ?
C69 C70 H70 119.5 . . ?
C70 C71 C72 121.4(3) . . ?
C70 C71 H71 119.3 . . ?
C72 C71 H71 119.3 . . ?
C73 C72 C71 119.3(3) . . ?
C73 C72 H72 120.4 . . ?
C71 C72 H72 120.4 . . ?
C72 C73 C68 121.0(3) . . ?
C72 C73 H73 119.5 . . ?
C68 C73 H73 119.5 . . ?
C75 C74 C62 122.1(2) . . ?
C75 C74 H74 119.0 . . ?
C62 C74 H74 119.0 . . ?
C74 C75 C76 118.9(2) . . ?
C74 C75 H75 120.5 . . ?
C76 C75 H75 120.5 . . ?
C77 C76 C75 120.5(2) . . ?
C77 C76 Cl5 119.3(2) . . ?
C75 C76 Cl5 120.2(2) . . ?
C76 C77 C61 121.2(2) . . ?
C76 C77 H77 119.4 . . ?
C61 C77 H77 119.4 . . ?
O16 C78 H78A 109.5 . . ?
O16 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
O16 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
N6 C80 C81 178.1(5) . . ?
C80 C81 H81A 109.5 . . ?
C80 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
C80 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
N7 C82 C83 177.8(10) . . ?
C82 C83 H83A 109.5 . . ?
C82 C83 H83B 109.5 . . ?
H83A C83 H83B 109.5 . . ?
C82 C83 H83C 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
C79 O17 H17A 109.5 . . ?
O17 C79 H79A 109.5 . . ?
O17 C79 H79B 109.5 . . ?
H79A C79 H79B 109.5 . . ?
O17 C79 H79C 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C88 O18 C89 120.0(8) . . ?
C88B O18 C89B 113.0(9) . . ?
O18 C88 C86 115.5(10) . . ?
C87 C89 O18 113.7(8) . . ?
O18 C88B C86 88.6(7) . . ?
C87 C89B O18 102.1(11) . . ?
N11 C85 C84 176.8(16) . . ?
C85 C84 H84A 109.5 . . ?
C85 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
C85 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni3 O2 C1 O1 13.1(4) . . . . ?
Ni3 O2 C1 C61 -165.40(15) . . . . ?
Ni2 O1 C1 O2 -168.79(17) . . . . ?
Ni1 O1 C1 O2 -0.8(3) . . . . ?
Ni2 O1 C1 C61 9.7(3) . . . . ?
Ni1 O1 C1 C61 177.70(15) . . . . ?
Ni5 O5 C2 O4 -24.5(3) . . . . ?
Ni5 O5 C2 C40 155.94(16) . . . . ?
Ni4 O4 C2 O5 175.53(16) . . . . ?
Ni1 O4 C2 O5 -26.7(3) . . . . ?
Ni4 O4 C2 C40 -4.9(3) . . . . ?
Ni1 O4 C2 C40 152.88(16) . . . . ?
Ni2 O7 C3 O6 7.4(4) . . . . ?
Ni2 O7 C3 C4 -172.46(16) . . . . ?
Ni5 O6 C3 O7 -164.45(17) . . . . ?
Ni1 O6 C3 O7 12.2(3) . . . . ?
Ni5 O6 C3 C4 15.4(3) . . . . ?
Ni1 O6 C3 C4 -167.94(15) . . . . ?
O7 C3 C4 C20 13.8(3) . . . . ?
O6 C3 C4 C20 -166.1(2) . . . . ?
O7 C3 C4 C5 -164.3(2) . . . . ?
O6 C3 C4 C5 15.8(4) . . . . ?
C6 N1 C5 C17 -31.7(3) . . . . ?
Ni5 N1 C5 C17 144.3(2) . . . . ?
C6 N1 C5 C4 153.5(2) . . . . ?
Ni5 N1 C5 C4 -30.5(3) . . . . ?
C20 C4 C5 C17 0.0(4) . . . . ?
C3 C4 C5 C17 178.0(2) . . . . ?
C20 C4 C5 N1 174.8(2) . . . . ?
C3 C4 C5 N1 -7.2(4) . . . . ?
C5 N1 C6 C7 160.6(2) . . . . ?
Ni5 N1 C6 C7 -15.3(3) . . . . ?
N1 C6 C7 C8 -19.8(4) . . . . ?
N1 C6 C7 C12 173.1(2) . . . . ?
Ni5 O8 C8 C7 22.7(3) . . . . ?
Ni5 O8 C8 C9 -159.97(19) . . . . ?
C6 C7 C8 O8 15.7(4) . . . . ?
C12 C7 C8 O8 -177.4(2) . . . . ?
C6 C7 C8 C9 -161.6(2) . . . . ?
C12 C7 C8 C9 5.3(4) . . . . ?
O8 C8 C9 C10 -179.1(3) . . . . ?
C7 C8 C9 C10 -1.5(4) . . . . ?
C8 C9 C10 C11 -1.9(5) . . . . ?
C9 C10 C11 C12 1.5(5) . . . . ?
C9 C10 C11 C16 -179.3(3) . . . . ?
C10 C11 C12 C13 -177.3(3) . . . . ?
C16 C11 C12 C13 3.5(5) . . . . ?
C10 C11 C12 C7 2.3(4) . . . . ?
C16 C11 C12 C7 -176.9(3) . . . . ?
C8 C7 C12 C13 173.9(3) . . . . ?
C6 C7 C12 C13 -18.9(4) . . . . ?
C8 C7 C12 C11 -5.7(4) . . . . ?
C6 C7 C12 C11 161.5(3) . . . . ?
C11 C12 C13 C14 -4.1(5) . . . . ?
C7 C12 C13 C14 176.4(3) . . . . ?
C12 C13 C14 C15 2.1(7) . . . . ?
C13 C14 C15 C16 0.6(7) . . . . ?
C14 C15 C16 C11 -1.1(6) . . . . ?
C12 C11 C16 C15 -1.0(5) . . . . ?
C10 C11 C16 C15 179.9(3) . . . . ?
N1 C5 C17 C18 -175.5(2) . . . . ?
C4 C5 C17 C18 -0.5(4) . . . . ?
C5 C17 C18 C19 0.8(4) . . . . ?
C17 C18 C19 C20 -0.7(5) . . . . ?
C17 C18 C19 Cl2 178.9(2) . . . . ?
C18 C19 C20 C4 0.1(4) . . . . ?
Cl2 C19 C20 C4 -179.5(2) . . . . ?
C5 C4 C20 C19 0.2(4) . . . . ?
C3 C4 C20 C19 -178.0(2) . . . . ?
Ni5 O9 C21 O10 -14.5(4) . . . . ?
Ni5 O9 C21 C22 165.30(17) . . . . ?
Ni1 O10 C21 O9 -12.9(3) . . . . ?
Ni3 O10 C21 O9 -149.19(18) . . . . ?
Ni1 O10 C21 C22 167.34(15) . . . . ?
Ni3 O10 C21 C22 31.0(3) . . . . ?
O9 C21 C22 C38 3.1(3) . . . . ?
O10 C21 C22 C38 -177.1(2) . . . . ?
O9 C21 C22 C23 -176.4(2) . . . . ?
O10 C21 C22 C23 3.4(3) . . . . ?
C38 C22 C23 C35 2.9(4) . . . . ?
C21 C22 C23 C35 -177.7(2) . . . . ?
C38 C22 C23 N2 176.8(2) . . . . ?
C21 C22 C23 N2 -3.8(4) . . . . ?
C24 N2 C23 C35 -36.9(3) . . . . ?
Ni3 N2 C23 C35 145.09(19) . . . . ?
C24 N2 C23 C22 149.2(2) . . . . ?
Ni3 N2 C23 C22 -28.8(3) . . . . ?
C23 N2 C24 C25 165.5(2) . . . . ?
Ni3 N2 C24 C25 -16.4(3) . . . . ?
N2 C24 C25 C26 -18.3(4) . . . . ?
N2 C24 C25 C30 167.7(2) . . . . ?
Ni3 O11 C26 C25 29.2(3) . . . . ?
Ni3 O11 C26 C27 -152.30(18) . . . . ?
C24 C25 C26 O11 11.1(4) . . . . ?
C30 C25 C26 O11 -174.9(2) . . . . ?
C24 C25 C26 C27 -167.4(2) . . . . ?
C30 C25 C26 C27 6.5(3) . . . . ?
O11 C26 C27 C28 178.2(2) . . . . ?
C25 C26 C27 C28 -3.2(4) . . . . ?
C26 C27 C28 C29 -0.8(4) . . . . ?
C27 C28 C29 C34 -177.0(3) . . . . ?
C27 C28 C29 C30 1.3(4) . . . . ?
C28 C29 C30 C31 -175.5(2) . . . . ?
C34 C29 C30 C31 2.8(3) . . . . ?
C28 C29 C30 C25 2.2(3) . . . . ?
C34 C29 C30 C25 -179.5(2) . . . . ?
C26 C25 C30 C31 171.4(2) . . . . ?
C24 C25 C30 C31 -14.5(3) . . . . ?
C26 C25 C30 C29 -6.1(3) . . . . ?
C24 C25 C30 C29 168.0(2) . . . . ?
C29 C30 C31 C32 -1.7(4) . . . . ?
C25 C30 C31 C32 -179.2(2) . . . . ?
C30 C31 C32 C33 -0.4(4) . . . . ?
C31 C32 C33 C34 1.2(4) . . . . ?
C32 C33 C34 C29 0.0(4) . . . . ?
C28 C29 C34 C33 176.2(3) . . . . ?
C30 C29 C34 C33 -2.1(4) . . . . ?
C22 C23 C35 C36 -1.7(4) . . . . ?
N2 C23 C35 C36 -175.8(2) . . . . ?
C23 C35 C36 C37 0.0(4) . . . . ?
C35 C36 C37 C38 0.5(4) . . . . ?
C35 C36 C37 Cl3 179.8(2) . . . . ?
C36 C37 C38 C22 0.7(4) . . . . ?
Cl3 C37 C38 C22 -178.6(2) . . . . ?
C23 C22 C38 C37 -2.4(4) . . . . ?
C21 C22 C38 C37 178.1(2) . . . . ?
O5 C2 C40 C41 -146.6(2) . . . . ?
O4 C2 C40 C41 33.8(3) . . . . ?
O5 C2 C40 C56 30.2(3) . . . . ?
O4 C2 C40 C56 -149.5(2) . . . . ?
C56 C40 C41 C53 -0.5(4) . . . . ?
C2 C40 C41 C53 176.1(3) . . . . ?
C56 C40 C41 N3 178.1(2) . . . . ?
C2 C40 C41 N3 -5.2(4) . . . . ?
C42 N3 C41 C40 127.2(3) . . . . ?
Ni4 N3 C41 C40 -46.5(3) . . . . ?
C42 N3 C41 C53 -54.2(4) . . . . ?
Ni4 N3 C41 C53 132.1(2) . . . . ?
C41 N3 C42 C43 -176.1(2) . . . . ?
Ni4 N3 C42 C43 -3.1(4) . . . . ?
N3 C42 C43 C44 20.3(4) . . . . ?
N3 C42 C43 C48 -163.8(3) . . . . ?
Ni4 O13 C44 C43 -31.2(3) . . . . ?
Ni3 O13 C44 C43 167.76(18) . . . . ?
Ni4 O13 C44 C45 150.69(19) . . . . ?
Ni3 O13 C44 C45 -10.4(4) . . . . ?
C42 C43 C44 O13 -1.8(4) . . . . ?
C48 C43 C44 O13 -177.6(2) . . . . ?
C42 C43 C44 C45 176.3(3) . . . . ?
C48 C43 C44 C45 0.5(4) . . . . ?
O13 C44 C45 C46 176.8(3) . . . . ?
C43 C44 C45 C46 -1.4(4) . . . . ?
C44 C45 C46 C47 0.7(5) . . . . ?
C45 C46 C47 C52 177.8(3) . . . . ?
C45 C46 C47 C48 0.8(4) . . . . ?
C52 C47 C48 C49 -0.2(4) . . . . ?
C46 C47 C48 C49 176.8(3) . . . . ?
C52 C47 C48 C43 -178.7(3) . . . . ?
C46 C47 C48 C43 -1.7(4) . . . . ?
C44 C43 C48 C47 1.0(4) . . . . ?
C42 C43 C48 C47 -174.9(2) . . . . ?
C44 C43 C48 C49 -177.4(3) . . . . ?
C42 C43 C48 C49 6.7(4) . . . . ?
C47 C48 C49 C50 0.2(4) . . . . ?
C43 C48 C49 C50 178.6(3) . . . . ?
C48 C49 C50 C51 -0.1(5) . . . . ?
C49 C50 C51 C52 0.1(5) . . . . ?
C50 C51 C52 C47 -0.2(5) . . . . ?
C46 C47 C52 C51 -176.7(3) . . . . ?
C48 C47 C52 C51 0.3(4) . . . . ?
C40 C41 C53 C54 0.5(5) . . . . ?
N3 C41 C53 C54 -178.1(3) . . . . ?
C41 C53 C54 C55 -0.2(5) . . . . ?
C53 C54 C55 C56 0.0(5) . . . . ?
C53 C54 C55 Cl4 -179.6(3) . . . . ?
C54 C55 C56 C40 0.0(5) . . . . ?
Cl4 C55 C56 C40 179.5(2) . . . . ?
C41 C40 C56 C55 0.2(4) . . . . ?
C2 C40 C56 C55 -176.6(3) . . . . ?
O2 C1 C61 C77 9.3(3) . . . . ?
O1 C1 C61 C77 -169.3(2) . . . . ?
O2 C1 C61 C62 -172.1(2) . . . . ?
O1 C1 C61 C62 9.3(4) . . . . ?
C77 C61 C62 C74 4.6(4) . . . . ?
C1 C61 C62 C74 -173.9(2) . . . . ?
C77 C61 C62 N5 -177.9(2) . . . . ?
C1 C61 C62 N5 3.6(4) . . . . ?
C63 N5 C62 C74 -36.8(3) . . . . ?
Ni2 N5 C62 C74 144.9(2) . . . . ?
C63 N5 C62 C61 145.7(2) . . . . ?
Ni2 N5 C62 C61 -32.6(3) . . . . ?
C62 N5 C63 C64 172.3(2) . . . . ?
Ni2 N5 C63 C64 -9.4(3) . . . . ?
N5 C63 C64 C65 -15.6(4) . . . . ?
N5 C63 C64 C69 171.1(2) . . . . ?
Ni2 O15 C65 C64 25.4(3) . . . . ?
Ni2 O15 C65 C66 -156.77(19) . . . . ?
C63 C64 C65 O15 6.8(4) . . . . ?
C69 C64 C65 O15 180.0(2) . . . . ?
C63 C64 C65 C66 -171.0(2) . . . . ?
C69 C64 C65 C66 2.2(4) . . . . ?
O15 C65 C66 C67 -178.7(3) . . . . ?
C64 C65 C66 C67 -0.7(4) . . . . ?
C65 C66 C67 C68 -0.7(5) . . . . ?
C66 C67 C68 C69 0.5(5) . . . . ?
C66 C67 C68 C73 -179.4(3) . . . . ?
C67 C68 C69 C70 -178.3(3) . . . . ?
C73 C68 C69 C70 1.7(5) . . . . ?
C67 C68 C69 C64 1.0(4) . . . . ?
C73 C68 C69 C64 -179.1(3) . . . . ?
C65 C64 C69 C68 -2.4(4) . . . . ?
C63 C64 C69 C68 171.1(2) . . . . ?
C65 C64 C69 C70 176.9(3) . . . . ?
C63 C64 C69 C70 -9.7(4) . . . . ?
C68 C69 C70 C71 -1.7(5) . . . . ?
C64 C69 C70 C71 179.1(3) . . . . ?
C69 C70 C71 C72 0.3(6) . . . . ?
C70 C71 C72 C73 1.2(7) . . . . ?
C71 C72 C73 C68 -1.3(7) . . . . ?
C69 C68 C73 C72 -0.2(6) . . . . ?
C67 C68 C73 C72 179.7(4) . . . . ?
C61 C62 C74 C75 -3.0(4) . . . . ?
N5 C62 C74 C75 179.4(3) . . . . ?
C62 C74 C75 C76 0.0(4) . . . . ?
C74 C75 C76 C77 1.3(5) . . . . ?
C74 C75 C76 Cl5 -180.0(2) . . . . ?
C75 C76 C77 C61 0.4(4) . . . . ?
Cl5 C76 C77 C61 -178.3(2) . . . . ?
C62 C61 C77 C76 -3.4(4) . . . . ?
C1 C61 C77 C76 175.3(2) . . . . ?
C89 O18 C88 C86 168.4(7) . . . . ?
C88 O18 C89 C87 -178.7(8) . . . . ?
C89B O18 C88B C86 145.2(10) . . . . ?
C88B O18 C89B C87 117.3(14) . . . . ?

_refine_diff_density_max         1.387
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.081




#=============================================================================#
#    Luis Cunha-Silva @ REQUIMTE / LAQV & DQB FCUP  *  18/05/2016  *   END    #
#=============================================================================#

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

data_comp3_rev
_database_code_depnum_ccdc_archive 'CCDC 1448723'
_audit_update_record             
;
2016-05-20 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;

# ========================================================================= #

_audit_creation_method           'SHELXL-2014/7 and enCIFer'
_shelx_SHELXL_version_number     2014/7
_audit_creation_date             '19 May 2016'

# ========================================================================= #


_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C108 H70 Cl6 N6 Ni6 O24, 2(C6 H16 N), 8(C H2 Cl2)'
_chemical_formula_sum            'C128 H118 Cl22 N8 Ni6 O24'
_chemical_formula_weight         3284.46

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   14.7531(12)
_cell_length_b                   18.2554(16)
_cell_length_c                   26.332(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.008(4)
_cell_angle_gamma                90
_cell_volume                     7004.4(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8348
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      28.46

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_F_000             3352
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    1.280
_shelx_estimated_absorpt_T_min   0.663
_shelx_estimated_absorpt_T_max   0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_process_details   
; 
'SADABS V2012/1 (Bruker AXS Inc.)' 
;


_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            109393
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.540
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.027
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994


_reflns_number_total             12298
_reflns_number_gt                11343
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 (Bruker AXS Inc., 2012)'
_computing_cell_refinement       'SAINT (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT (Bruker AXS Inc., 2012)'
_computing_structure_solution    'SHELXS (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2014)'


_refine_special_details          
;
 In this structure have been clearly found and refined 
 6 dichloromethane (DCM) solvent molecules per formula. 
 Various attempts to model and refine the remaining solvent 
 molecules in the overlapping electronic density revealed to 
 be unsuccessful. It was not possible to found a model chemically 
 reasonable. Consequently, the residual density was processed 
 with the solvent-masking procedure (PLATON SQUEEZE), pointing 
 to the existence of two additional DCM molecules. The located 
 solvent and these two extra molecules were then considered in 
 the molecular formula of the compound and in the final 
 refinement cycles of this crystal structure.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1374P)²+150.0885P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12298
_refine_ls_number_parameters     839
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0986
_refine_ls_wR_factor_ref         0.2603
_refine_ls_wR_factor_gt          0.2556
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_restrained_S_all      0.916
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.97533(6) -0.07634(5) 0.01455(3) 0.0121(2) Uani 1 1 d . . . . .
Ni2 Ni 0.85555(6) 0.06985(5) 0.06661(3) 0.0127(2) Uani 1 1 d . . . . .
Ni3 Ni 0.92881(6) -0.22811(5) 0.04853(3) 0.0148(2) Uani 1 1 d . . . . .
Cl1 Cl 0.71205(17) -0.13323(12) 0.25582(8) 0.0339(5) Uani 1 1 d . . . . .
Cl2 Cl 0.80679(17) 0.42718(11) 0.11027(9) 0.0383(6) Uani 1 1 d . . . . .
Cl3 Cl 0.49583(15) 0.34250(11) 0.05677(9) 0.0342(5) Uani 1 1 d . . . . .
O1 O 0.9186(3) 0.0251(3) 0.01104(17) 0.0127(10) Uani 1 1 d D . . . .
H1 H 0.879(4) 0.021(4) -0.0158(18) 0.012(19) Uiso 1 1 d D . . . .
O2 O 0.8129(3) -0.0344(3) 0.08911(19) 0.0170(11) Uani 1 1 d . . . . .
O3 O 0.8675(3) -0.1255(3) 0.04478(18) 0.0136(10) Uani 1 1 d . . . . .
O4 O 0.8797(4) -0.2496(3) -0.02601(19) 0.0198(11) Uani 1 1 d . . . . .
O5 O 0.8909(4) 0.1764(3) 0.04749(19) 0.0186(11) Uani 1 1 d . . . . .
O6 O 0.9638(3) 0.1794(3) -0.02037(18) 0.0144(10) Uani 1 1 d . . . . .
O7 O 1.0134(4) 0.1976(3) -0.12154(19) 0.0197(11) Uani 1 1 d . . . . .
O8 O 0.7404(3) 0.0724(3) 0.01399(19) 0.0189(11) Uani 1 1 d . . . . .
O9 O 0.5980(4) 0.0997(3) -0.0190(2) 0.0270(13) Uani 1 1 d . . . . .
O10 O 0.9667(3) 0.0603(3) 0.12162(19) 0.0186(11) Uani 1 1 d . . . . .
O11 O 1.0417(4) -0.0639(3) 0.08983(19) 0.0185(11) Uani 1 1 d D . . . .
H1W H 1.032(6) -0.103(2) 0.106(3) 0.028 Uiso 1 1 d D U . . .
H2W H 1.022(6) -0.024(2) 0.102(3) 0.028 Uiso 1 1 d D U . . .
O12 O 0.9080(3) -0.1076(3) -0.05839(19) 0.0164(10) Uani 1 1 d D . . . .
H3W H 0.879(5) -0.148(3) -0.062(3) 0.025 Uiso 1 1 d D U . . .
H4W H 0.949(4) -0.101(4) -0.078(3) 0.025 Uiso 1 1 d D U . . .
N1 N 0.8072(4) -0.2632(3) 0.0640(2) 0.0186(13) Uani 1 1 d . . . . .
N2 N 0.9907(4) 0.3174(3) -0.0604(2) 0.0202(13) Uani 1 1 d . . . . .
N3 N 0.7884(4) 0.1183(3) 0.1189(2) 0.0151(12) Uani 1 1 d . . . . .
C1 C 0.8260(5) -0.1000(4) 0.0809(3) 0.0143(14) Uani 1 1 d . . . . .
C2 C 0.8406(6) -0.3127(4) -0.0382(3) 0.0214(16) Uani 1 1 d . . . . .
C3 C 0.7804(5) -0.3481(4) -0.0082(3) 0.0236(17) Uani 1 1 d . . . . .
C4 C 0.7568(5) -0.3121(4) 0.0373(3) 0.0171(15) Uani 1 1 d . . . . .
H4 H 0.7006 -0.3253 0.0482 0.020 Uiso 1 1 calc R U . . .
C5 C 0.7752(5) -0.2310(4) 0.1072(3) 0.0184(15) Uani 1 1 d . . . . .
C6 C 0.7868(5) -0.1545(4) 0.1162(3) 0.0166(15) Uani 1 1 d . . . . .
C7 C 0.7646(5) -0.1256(4) 0.1616(3) 0.0189(15) Uani 1 1 d . . . . .
H7 H 0.7713 -0.0745 0.1681 0.023 Uiso 1 1 calc R U . . .
C8 C 0.7331(5) -0.1704(4) 0.1976(3) 0.0232(17) Uani 1 1 d . . . . .
C9 C 0.7205(6) -0.2445(4) 0.1891(3) 0.0258(17) Uani 1 1 d . . . . .
H9 H 0.6970 -0.2746 0.2134 0.031 Uiso 1 1 calc R U . . .
C10 C 0.7432(5) -0.2742(4) 0.1436(3) 0.0238(17) Uani 1 1 d . . . . .
H10 H 0.7364 -0.3254 0.1377 0.029 Uiso 1 1 calc R U . . .
C11 C 0.7363(6) -0.4162(4) -0.0252(3) 0.0282(18) Uani 1 1 d . . . . .
C12 C 0.7549(7) -0.4485(5) -0.0720(4) 0.035(2) Uani 1 1 d . . . . .
C13 C 0.8173(8) -0.4117(5) -0.1001(3) 0.039(2) Uani 1 1 d . . . . .
H13 H 0.8318 -0.4335 -0.1306 0.047 Uiso 1 1 calc R U . . .
C14 C 0.8558(6) -0.3476(5) -0.0843(3) 0.0300(19) Uani 1 1 d . . . . .
H14 H 0.8950 -0.3244 -0.1048 0.036 Uiso 1 1 calc R U . . .
C15 C 0.7159(9) -0.5170(5) -0.0875(4) 0.049(3) Uani 1 1 d . . . . .
H15 H 0.7314 -0.5392 -0.1176 0.059 Uiso 1 1 calc R U . . .
C16 C 0.6567(9) -0.5527(6) -0.0608(5) 0.058(3) Uani 1 1 d . . . . .
H16 H 0.6291 -0.5978 -0.0727 0.070 Uiso 1 1 calc R U . . .
C17 C 0.6382(8) -0.5204(5) -0.0150(4) 0.045(3) Uani 1 1 d . . . . .
H17 H 0.5975 -0.5445 0.0041 0.054 Uiso 1 1 calc R U . . .
C18 C 0.6769(6) -0.4552(5) 0.0029(4) 0.033(2) Uani 1 1 d . . . . .
H18 H 0.6639 -0.4359 0.0345 0.040 Uiso 1 1 calc R U . . .
C19 C 0.9248(5) 0.2097(4) 0.0137(3) 0.0132(14) Uani 1 1 d . . . . .
C20 C 0.9149(5) 0.2935(4) 0.0148(3) 0.0156(14) Uani 1 1 d . . . . .
C21 C 0.9448(5) 0.3433(4) -0.0195(3) 0.0195(15) Uani 1 1 d . . . . .
C22 C 0.9758(5) 0.3500(4) -0.1051(3) 0.0213(16) Uani 1 1 d . . . . .
H22 H 0.9403 0.3937 -0.1085 0.026 Uiso 1 1 calc R U . . .
C23 C 1.0109(6) 0.3226(5) -0.1495(3) 0.0242(17) Uani 1 1 d . . . . .
C24 C 1.0203(5) 0.2464(5) -0.1572(3) 0.0229(17) Uani 1 1 d . . . . .
C25 C 1.0333(6) 0.2212(5) -0.2077(3) 0.0288(18) Uani 1 1 d . . . . .
H25 H 1.0333 0.1701 -0.2145 0.035 Uiso 1 1 calc R U . . .
C26 C 1.0456(6) 0.2692(6) -0.2453(3) 0.039(2) Uani 1 1 d . . . . .
H26 H 1.0567 0.2506 -0.2775 0.046 Uiso 1 1 calc R U . . .
C27 C 1.0424(6) 0.3467(6) -0.2383(3) 0.035(2) Uani 1 1 d . . . . .
C28 C 1.0233(6) 0.3735(5) -0.1900(3) 0.0306(19) Uani 1 1 d . . . . .
C29 C 1.0217(8) 0.4504(6) -0.1841(4) 0.045(3) Uani 1 1 d . . . . .
H29 H 1.0081 0.4700 -0.1527 0.054 Uiso 1 1 calc R U . . .
C30 C 1.0387(9) 0.4976(7) -0.2216(4) 0.060(4) Uani 1 1 d . . . . .
H30 H 1.0366 0.5489 -0.2159 0.072 Uiso 1 1 calc R U . . .
C31 C 1.0592(8) 0.4714(7) -0.2681(4) 0.056(3) Uani 1 1 d . . . . .
H31 H 1.0726 0.5044 -0.2938 0.067 Uiso 1 1 calc R U . . .
C32 C 1.0596(7) 0.3973(7) -0.2761(3) 0.046(3) Uani 1 1 d . . . . .
H32 H 1.0719 0.3793 -0.3082 0.055 Uiso 1 1 calc R U . . .
C33 C 0.9324(6) 0.4177(4) -0.0132(3) 0.0258(17) Uani 1 1 d . . . . .
H33 H 0.9539 0.4508 -0.0365 0.031 Uiso 1 1 calc R U . . .
C34 C 0.8897(6) 0.4456(4) 0.0260(3) 0.0295(19) Uani 1 1 d . . . . .
H34 H 0.8807 0.4967 0.0296 0.035 Uiso 1 1 calc R U . . .
C35 C 0.8602(6) 0.3945(4) 0.0600(3) 0.0256(18) Uani 1 1 d . . . . .
C36 C 0.8720(5) 0.3209(4) 0.0543(3) 0.0205(16) Uani 1 1 d . . . . .
H36 H 0.8505 0.2879 0.0777 0.025 Uiso 1 1 calc R U . . .
C37 C 0.6688(5) 0.1091(4) 0.0134(3) 0.0190(15) Uani 1 1 d . . . . .
C38 C 0.6625(5) 0.1689(4) 0.0540(3) 0.0159(14) Uani 1 1 d . . . . .
C39 C 0.7191(5) 0.1725(4) 0.1029(3) 0.0160(14) Uani 1 1 d . . . . .
C40 C 0.8080(5) 0.1054(4) 0.1679(3) 0.0187(16) Uani 1 1 d . . . . .
H40 H 0.7670 0.1251 0.1888 0.022 Uiso 1 1 calc R U . . .
C41 C 0.8852(5) 0.0643(4) 0.1942(3) 0.0169(15) Uani 1 1 d . . . . .
C42 C 0.9628(5) 0.0490(4) 0.1706(3) 0.0197(16) Uani 1 1 d . . . . .
C43 C 1.0430(6) 0.0203(6) 0.2022(3) 0.035(2) Uani 1 1 d . . . . .
H43 H 1.0963 0.0124 0.1868 0.042 Uiso 1 1 calc R U . . .
C44 C 1.0470(7) 0.0035(7) 0.2534(4) 0.047(3) Uani 1 1 d . . . . .
H44 H 1.1013 -0.0163 0.2727 0.056 Uiso 1 1 calc R U . . .
C45 C 0.9663(6) 0.0169(6) 0.2773(3) 0.036(2) Uani 1 1 d . . . . .
C46 C 0.8860(6) 0.0463(4) 0.2481(3) 0.0208(16) Uani 1 1 d . . . . .
C47 C 0.8098(6) 0.0555(4) 0.2735(3) 0.0205(16) Uani 1 1 d . . . . .
H47 H 0.7543 0.0746 0.2550 0.025 Uiso 1 1 calc R U . . .
C48 C 0.8136(7) 0.0376(4) 0.3249(3) 0.0282(19) Uani 1 1 d . . . . .
H48 H 0.7614 0.0456 0.3412 0.034 Uiso 1 1 calc R U . . .
C49 C 0.8925(7) 0.0082(5) 0.3528(3) 0.037(2) Uani 1 1 d . . . . .
H49 H 0.8936 -0.0053 0.3877 0.045 Uiso 1 1 calc R U . . .
C50 C 0.9692(8) -0.0013(6) 0.3299(3) 0.045(3) Uani 1 1 d . . . . .
H50 H 1.0240 -0.0201 0.3492 0.054 Uiso 1 1 calc R U . . .
C51 C 0.7078(6) 0.2321(4) 0.1344(3) 0.0214(16) Uani 1 1 d . . . . .
H51 H 0.7476 0.2369 0.1663 0.026 Uiso 1 1 calc R U . . .
C52 C 0.6406(6) 0.2847(4) 0.1210(3) 0.0230(17) Uani 1 1 d . . . . .
H52 H 0.6341 0.3245 0.1434 0.028 Uiso 1 1 calc R U . . .
C53 C 0.5836(5) 0.2785(4) 0.0748(3) 0.0242(17) Uani 1 1 d . . . . .
C54 C 0.5949(5) 0.2216(4) 0.0415(3) 0.0222(16) Uani 1 1 d . . . . .
H54 H 0.5556 0.2187 0.0093 0.027 Uiso 1 1 calc R U . . .
N4 N 0.3891(5) 0.0304(4) 0.0692(3) 0.0359(18) Uani 1 1 d . . . . .
H4A H 0.3859 -0.0161 0.0490 0.043 Uiso 1 1 calc R U . . .
C58 C 0.4865(8) 0.0529(6) 0.0799(6) 0.070(4) Uani 1 1 d . . . . .
H58A H 0.5001 0.0812 0.0499 0.084 Uiso 1 1 calc R U . . .
H58B H 0.4938 0.0868 0.1096 0.084 Uiso 1 1 calc R U . . .
C59 C 0.5560(7) -0.0040(7) 0.0908(4) 0.054(3) Uani 1 1 d . . . . .
H59A H 0.5441 -0.0329 0.1204 0.081 Uiso 1 1 calc R U . . .
H59B H 0.6168 0.0187 0.0986 0.081 Uiso 1 1 calc R U . . .
H59C H 0.5538 -0.0360 0.0607 0.081 Uiso 1 1 calc R U . . .
C60 C 0.3303(10) 0.0817(7) 0.0401(5) 0.062(3) Uani 1 1 d . . . . .
H60A H 0.2667 0.0628 0.0366 0.074 Uiso 1 1 calc R U . . .
H60B H 0.3470 0.0841 0.0052 0.074 Uiso 1 1 calc R U . . .
C61 C 0.3309(12) 0.1593(9) 0.0612(7) 0.092(5) Uani 1 1 d . U . . .
H61A H 0.2751 0.1849 0.0455 0.137 Uiso 1 1 calc R U . . .
H61B H 0.3849 0.1854 0.0532 0.137 Uiso 1 1 calc R U . . .
H61C H 0.3331 0.1575 0.0986 0.137 Uiso 1 1 calc R U . . .
C62 C 0.3652(9) 0.0111(8) 0.1242(5) 0.060(3) Uani 1 1 d . . . . .
H62A H 0.4094 -0.0253 0.1414 0.072 Uiso 1 1 calc R U . . .
H62B H 0.3689 0.0557 0.1458 0.072 Uiso 1 1 calc R U . . .
C63 C 0.2703(8) -0.0194(7) 0.1172(4) 0.051(3) Uani 1 1 d . . . . .
H63A H 0.2261 0.0196 0.1058 0.076 Uiso 1 1 calc R U . . .
H63B H 0.2578 -0.0394 0.1500 0.076 Uiso 1 1 calc R U . . .
H63C H 0.2646 -0.0584 0.0914 0.076 Uiso 1 1 calc R U . . .
Cl4 Cl 0.2311(2) 0.2626(2) 0.42728(14) 0.0690(9) Uani 1 1 d . . . . .
Cl5 Cl 0.2558(3) 0.1960(2) 0.33004(15) 0.0762(10) Uani 1 1 d . . . . .
C55 C 0.2795(9) 0.2748(7) 0.3721(5) 0.063(3) Uani 1 1 d . . . . .
H55A H 0.3467 0.2813 0.3814 0.075 Uiso 1 1 calc R U . . .
H55B H 0.2540 0.3195 0.3539 0.075 Uiso 1 1 calc R U . . .
Cl6 Cl 0.0236(3) 0.3309(2) 0.33215(16) 0.0867(11) Uani 1 1 d . . . . .
Cl7 Cl -0.0099(3) 0.1991(2) 0.3890(3) 0.158(3) Uani 1 1 d . . . . .
C56 C -0.0118(9) 0.2957(7) 0.3878(6) 0.071(4) Uani 1 1 d . . . . .
H56A H -0.0749 0.3129 0.3895 0.086 Uiso 1 1 calc R U . . .
H56B H 0.0290 0.3147 0.4184 0.086 Uiso 1 1 calc R U . . .
Cl8 Cl -0.0233(3) 0.2583(3) 0.1810(3) 0.132(2) Uani 1 1 d . . . . .
Cl9 Cl 0.1447(6) 0.1869(3) 0.1808(2) 0.138(2) Uani 1 1 d . . . . .
C57 C 0.0614(13) 0.2210(13) 0.2225(6) 0.115(8) Uani 1 1 d . . . . .
H57A H 0.0382 0.1801 0.2416 0.138 Uiso 1 1 calc R U . . .
H57B H 0.0905 0.2579 0.2474 0.138 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.026(5) 3_755 ?
Ni1 O1 2.028(5) . ?
Ni1 O6 2.080(5) 3_755 ?
Ni1 O11 2.081(5) . ?
Ni1 O3 2.090(5) . ?
Ni1 O12 2.099(5) . ?
Ni2 O8 2.017(5) . ?
Ni2 O10 2.018(5) . ?
Ni2 N3 2.021(6) . ?
Ni2 O1 2.025(5) . ?
Ni2 O5 2.095(5) . ?
Ni2 O2 2.118(5) . ?
Ni3 N1 2.007(6) . ?
Ni3 N2 2.013(6) 3_755 ?
Ni3 O4 2.022(5) . ?
Ni3 O6 2.054(5) 3_755 ?
Ni3 O7 2.054(5) 3_755 ?
Ni3 O3 2.075(5) . ?
Cl1 C8 1.749(8) . ?
Cl2 C35 1.747(8) . ?
Cl3 C53 1.753(8) . ?
O1 Ni1 2.026(5) 3_755 ?
O1 H1 0.85(2) . ?
O2 C1 1.238(9) . ?
O3 C1 1.296(8) . ?
O4 C2 1.305(9) . ?
O5 C19 1.245(9) . ?
O6 C19 1.267(9) . ?
O6 Ni3 2.054(5) 3_755 ?
O6 Ni1 2.079(5) 3_755 ?
O7 C24 1.310(9) . ?
O7 Ni3 2.054(5) 3_755 ?
O8 C37 1.250(9) . ?
O9 C37 1.253(9) . ?
O10 C42 1.318(9) . ?
O11 H1W 0.86(2) . ?
O11 H2W 0.86(2) . ?
O12 H3W 0.85(2) . ?
O12 H4W 0.85(2) . ?
N1 C4 1.295(10) . ?
N1 C5 1.423(9) . ?
N2 C22 1.309(10) . ?
N2 C21 1.437(10) . ?
N2 Ni3 2.013(6) 3_755 ?
N3 C40 1.299(10) . ?
N3 C39 1.437(9) . ?
C1 C6 1.534(10) . ?
C2 C14 1.420(11) . ?
C2 C3 1.432(11) . ?
C3 C11 1.441(12) . ?
C3 C4 1.456(11) . ?
C4 H4 0.9500 . ?
C5 C10 1.380(11) . ?
C5 C6 1.423(11) . ?
C6 C7 1.393(10) . ?
C7 C8 1.385(11) . ?
C7 H7 0.9500 . ?
C8 C9 1.379(12) . ?
C9 C10 1.403(11) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C18 1.423(13) . ?
C11 C12 1.433(13) . ?
C12 C15 1.409(13) . ?
C12 C13 1.434(14) . ?
C13 C14 1.339(13) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.371(17) . ?
C15 H15 0.9500 . ?
C16 C17 1.406(17) . ?
C16 H16 0.9500 . ?
C17 C18 1.371(13) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.538(10) . ?
C20 C36 1.393(10) . ?
C20 C21 1.400(10) . ?
C21 C33 1.384(11) . ?
C22 C23 1.440(11) . ?
C22 H22 0.9500 . ?
C23 C24 1.416(12) . ?
C23 C28 1.446(11) . ?
C24 C25 1.447(11) . ?
C25 C26 1.357(13) . ?
C25 H25 0.9500 . ?
C26 C27 1.429(15) . ?
C26 H26 0.9500 . ?
C27 C32 1.410(13) . ?
C27 C28 1.432(13) . ?
C28 C29 1.412(14) . ?
C29 C30 1.363(13) . ?
C29 H29 0.9500 . ?
C30 C31 1.391(18) . ?
C30 H30 0.9500 . ?
C31 C32 1.370(18) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C34 1.388(12) . ?
C33 H33 0.9500 . ?
C34 C35 1.409(12) . ?
C34 H34 0.9500 . ?
C35 C36 1.366(11) . ?
C36 H36 0.9500 . ?
C37 C38 1.541(10) . ?
C38 C54 1.388(10) . ?
C38 C39 1.421(10) . ?
C39 C51 1.395(10) . ?
C40 C41 1.446(11) . ?
C40 H40 0.9500 . ?
C41 C42 1.412(10) . ?
C41 C46 1.456(10) . ?
C42 C43 1.434(12) . ?
C43 C44 1.376(13) . ?
C43 H43 0.9500 . ?
C44 C45 1.452(13) . ?
C44 H44 0.9500 . ?
C45 C46 1.413(12) . ?
C45 C50 1.417(12) . ?
C46 C47 1.406(11) . ?
C47 C48 1.384(11) . ?
C47 H47 0.9500 . ?
C48 C49 1.384(14) . ?
C48 H48 0.9500 . ?
C49 C50 1.374(14) . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?
C51 C52 1.385(11) . ?
C51 H51 0.9500 . ?
C52 C53 1.370(12) . ?
C52 H52 0.9500 . ?
C53 C54 1.388(11) . ?
C54 H54 0.9500 . ?
N4 C60 1.417(14) . ?
N4 C58 1.479(13) . ?
N4 C62 1.582(14) . ?
N4 H4A 1.0000 . ?
C58 C59 1.455(17) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 C61 1.521(19) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 C63 1.492(17) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
Cl4 C55 1.732(13) . ?
Cl5 C55 1.815(15) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
Cl6 C56 1.752(16) . ?
Cl7 C56 1.765(14) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
Cl8 C57 1.67(2) . ?
Cl9 C57 1.88(2) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 84.1(2) 3_755 . ?
O1 Ni1 O6 95.45(19) 3_755 3_755 ?
O1 Ni1 O6 178.1(2) . 3_755 ?
O1 Ni1 O11 89.6(2) 3_755 . ?
O1 Ni1 O11 94.2(2) . . ?
O6 Ni1 O11 84.0(2) 3_755 . ?
O1 Ni1 O3 176.71(19) 3_755 . ?
O1 Ni1 O3 94.40(19) . . ?
O6 Ni1 O3 85.91(19) 3_755 . ?
O11 Ni1 O3 87.5(2) . . ?
O1 Ni1 O12 95.79(19) 3_755 . ?
O1 Ni1 O12 94.25(19) . . ?
O6 Ni1 O12 87.6(2) 3_755 . ?
O11 Ni1 O12 170.4(2) . . ?
O3 Ni1 O12 87.25(19) . . ?
O8 Ni2 O10 175.5(2) . . ?
O8 Ni2 N3 90.4(2) . . ?
O10 Ni2 N3 88.8(2) . . ?
O8 Ni2 O1 86.9(2) . . ?
O10 Ni2 O1 94.0(2) . . ?
N3 Ni2 O1 176.6(2) . . ?
O8 Ni2 O5 91.6(2) . . ?
O10 Ni2 O5 92.7(2) . . ?
N3 Ni2 O5 85.7(2) . . ?
O1 Ni2 O5 92.35(19) . . ?
O8 Ni2 O2 87.6(2) . . ?
O10 Ni2 O2 88.0(2) . . ?
N3 Ni2 O2 90.2(2) . . ?
O1 Ni2 O2 91.73(19) . . ?
O5 Ni2 O2 175.79(19) . . ?
N1 Ni3 N2 103.6(2) . 3_755 ?
N1 Ni3 O4 86.5(2) . . ?
N2 Ni3 O4 96.1(2) 3_755 . ?
N1 Ni3 O6 167.6(2) . 3_755 ?
N2 Ni3 O6 86.4(2) 3_755 3_755 ?
O4 Ni3 O6 85.0(2) . 3_755 ?
N1 Ni3 O7 98.6(2) . 3_755 ?
N2 Ni3 O7 85.8(2) 3_755 3_755 ?
O4 Ni3 O7 174.0(2) . 3_755 ?
O6 Ni3 O7 89.4(2) 3_755 3_755 ?
N1 Ni3 O3 84.3(2) . . ?
N2 Ni3 O3 168.7(2) 3_755 . ?
O4 Ni3 O3 92.4(2) . . ?
O6 Ni3 O3 86.97(19) 3_755 . ?
O7 Ni3 O3 85.1(2) 3_755 . ?
Ni2 O1 Ni1 121.4(2) . 3_755 ?
Ni2 O1 Ni1 124.6(2) . . ?
Ni1 O1 Ni1 95.9(2) 3_755 . ?
Ni2 O1 H1 107(5) . . ?
Ni1 O1 H1 103(5) 3_755 . ?
Ni1 O1 H1 101(5) . . ?
C1 O2 Ni2 139.4(5) . . ?
C1 O3 Ni3 122.8(4) . . ?
C1 O3 Ni1 126.9(4) . . ?
Ni3 O3 Ni1 93.08(19) . . ?
C2 O4 Ni3 119.2(5) . . ?
C19 O5 Ni2 140.2(5) . . ?
C19 O6 Ni3 121.9(4) . 3_755 ?
C19 O6 Ni1 125.6(4) . 3_755 ?
Ni3 O6 Ni1 94.01(19) 3_755 3_755 ?
C24 O7 Ni3 114.8(5) . 3_755 ?
C37 O8 Ni2 129.8(5) . . ?
C42 O10 Ni2 124.2(5) . . ?
Ni1 O11 H1W 108(6) . . ?
Ni1 O11 H2W 109(6) . . ?
H1W O11 H2W 114(4) . . ?
Ni1 O12 H3W 119(6) . . ?
Ni1 O12 H4W 103(5) . . ?
H3W O12 H4W 117(4) . . ?
C4 N1 C5 119.0(6) . . ?
C4 N1 Ni3 124.4(5) . . ?
C5 N1 Ni3 116.7(5) . . ?
C22 N2 C21 119.5(7) . . ?
C22 N2 Ni3 121.3(5) . 3_755 ?
C21 N2 Ni3 119.1(5) . 3_755 ?
C40 N3 C39 117.0(6) . . ?
C40 N3 Ni2 122.7(5) . . ?
C39 N3 Ni2 120.3(5) . . ?
O2 C1 O3 125.5(6) . . ?
O2 C1 C6 115.9(6) . . ?
O3 C1 C6 118.5(6) . . ?
O4 C2 C14 118.9(7) . . ?
O4 C2 C3 123.4(7) . . ?
C14 C2 C3 117.7(7) . . ?
C2 C3 C11 120.4(7) . . ?
C2 C3 C4 120.0(7) . . ?
C11 C3 C4 119.4(7) . . ?
N1 C4 C3 124.5(7) . . ?
N1 C4 H4 117.7 . . ?
C3 C4 H4 117.7 . . ?
C10 C5 N1 120.7(7) . . ?
C10 C5 C6 119.3(7) . . ?
N1 C5 C6 119.5(6) . . ?
C7 C6 C5 118.5(7) . . ?
C7 C6 C1 115.9(6) . . ?
C5 C6 C1 125.6(6) . . ?
C8 C7 C6 120.8(7) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
C9 C8 C7 121.4(7) . . ?
C9 C8 Cl1 118.9(6) . . ?
C7 C8 Cl1 119.7(6) . . ?
C8 C9 C10 118.2(7) . . ?
C8 C9 H9 120.9 . . ?
C10 C9 H9 120.9 . . ?
C5 C10 C9 121.8(7) . . ?
C5 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
C18 C11 C12 117.2(8) . . ?
C18 C11 C3 123.8(8) . . ?
C12 C11 C3 119.0(8) . . ?
C15 C12 C11 119.4(9) . . ?
C15 C12 C13 122.2(9) . . ?
C11 C12 C13 118.4(8) . . ?
C14 C13 C12 121.7(8) . . ?
C14 C13 H13 119.1 . . ?
C12 C13 H13 119.1 . . ?
C13 C14 C2 122.7(8) . . ?
C13 C14 H14 118.6 . . ?
C2 C14 H14 118.6 . . ?
C16 C15 C12 122.6(10) . . ?
C16 C15 H15 118.7 . . ?
C12 C15 H15 118.7 . . ?
C15 C16 C17 117.7(9) . . ?
C15 C16 H16 121.2 . . ?
C17 C16 H16 121.2 . . ?
C18 C17 C16 122.2(10) . . ?
C18 C17 H17 118.9 . . ?
C16 C17 H17 118.9 . . ?
C17 C18 C11 120.9(10) . . ?
C17 C18 H18 119.6 . . ?
C11 C18 H18 119.6 . . ?
O5 C19 O6 124.8(6) . . ?
O5 C19 C20 115.0(6) . . ?
O6 C19 C20 120.2(6) . . ?
C36 C20 C21 118.4(7) . . ?
C36 C20 C19 115.3(6) . . ?
C21 C20 C19 126.4(6) . . ?
C33 C21 C20 119.9(7) . . ?
C33 C21 N2 119.9(7) . . ?
C20 C21 N2 120.2(6) . . ?
N2 C22 C23 122.9(7) . . ?
N2 C22 H22 118.6 . . ?
C23 C22 H22 118.6 . . ?
C24 C23 C22 120.9(7) . . ?
C24 C23 C28 120.0(8) . . ?
C22 C23 C28 118.5(8) . . ?
O7 C24 C23 123.0(7) . . ?
O7 C24 C25 118.6(8) . . ?
C23 C24 C25 118.3(7) . . ?
C26 C25 C24 121.2(9) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C25 C26 C27 122.3(9) . . ?
C25 C26 H26 118.9 . . ?
C27 C26 H26 118.9 . . ?
C32 C27 C26 122.9(9) . . ?
C32 C27 C28 119.1(10) . . ?
C26 C27 C28 118.0(8) . . ?
C29 C28 C27 116.6(8) . . ?
C29 C28 C23 123.4(8) . . ?
C27 C28 C23 119.9(8) . . ?
C30 C29 C28 122.7(11) . . ?
C30 C29 H29 118.7 . . ?
C28 C29 H29 118.7 . . ?
C29 C30 C31 120.7(12) . . ?
C29 C30 H30 119.6 . . ?
C31 C30 H30 119.6 . . ?
C32 C31 C30 118.8(10) . . ?
C32 C31 H31 120.6 . . ?
C30 C31 H31 120.6 . . ?
C31 C32 C27 122.1(10) . . ?
C31 C32 H32 118.9 . . ?
C27 C32 H32 118.9 . . ?
C21 C33 C34 122.1(8) . . ?
C21 C33 H33 118.9 . . ?
C34 C33 H33 118.9 . . ?
C33 C34 C35 117.0(7) . . ?
C33 C34 H34 121.5 . . ?
C35 C34 H34 121.5 . . ?
C36 C35 C34 121.5(7) . . ?
C36 C35 Cl2 120.0(6) . . ?
C34 C35 Cl2 118.5(6) . . ?
C35 C36 C20 121.1(7) . . ?
C35 C36 H36 119.5 . . ?
C20 C36 H36 119.5 . . ?
O8 C37 O9 123.2(7) . . ?
O8 C37 C38 121.0(6) . . ?
O9 C37 C38 115.9(6) . . ?
C54 C38 C39 118.8(7) . . ?
C54 C38 C37 116.4(7) . . ?
C39 C38 C37 124.8(6) . . ?
C51 C39 C38 117.8(7) . . ?
C51 C39 N3 120.6(7) . . ?
C38 C39 N3 121.6(6) . . ?
N3 C40 C41 127.3(6) . . ?
N3 C40 H40 116.3 . . ?
C41 C40 H40 116.3 . . ?
C42 C41 C40 121.6(6) . . ?
C42 C41 C46 120.0(7) . . ?
C40 C41 C46 118.1(6) . . ?
O10 C42 C41 124.2(7) . . ?
O10 C42 C43 117.7(7) . . ?
C41 C42 C43 118.0(7) . . ?
C44 C43 C42 123.6(8) . . ?
C44 C43 H43 118.2 . . ?
C42 C43 H43 118.2 . . ?
C43 C44 C45 118.4(9) . . ?
C43 C44 H44 120.8 . . ?
C45 C44 H44 120.8 . . ?
C46 C45 C50 121.0(8) . . ?
C46 C45 C44 120.2(8) . . ?
C50 C45 C44 118.8(9) . . ?
C47 C46 C45 116.8(7) . . ?
C47 C46 C41 123.5(7) . . ?
C45 C46 C41 119.7(7) . . ?
C48 C47 C46 121.5(8) . . ?
C48 C47 H47 119.2 . . ?
C46 C47 H47 119.2 . . ?
C49 C48 C47 120.9(8) . . ?
C49 C48 H48 119.6 . . ?
C47 C48 H48 119.6 . . ?
C50 C49 C48 119.8(8) . . ?
C50 C49 H49 120.1 . . ?
C48 C49 H49 120.1 . . ?
C49 C50 C45 119.9(9) . . ?
C49 C50 H50 120.1 . . ?
C45 C50 H50 120.1 . . ?
C52 C51 C39 122.4(7) . . ?
C52 C51 H51 118.8 . . ?
C39 C51 H51 118.8 . . ?
C53 C52 C51 119.0(7) . . ?
C53 C52 H52 120.5 . . ?
C51 C52 H52 120.5 . . ?
C52 C53 C54 120.4(7) . . ?
C52 C53 Cl3 120.7(6) . . ?
C54 C53 Cl3 118.9(6) . . ?
C53 C54 C38 121.4(7) . . ?
C53 C54 H54 119.3 . . ?
C38 C54 H54 119.3 . . ?
C60 N4 C58 114.4(9) . . ?
C60 N4 C62 115.9(9) . . ?
C58 N4 C62 103.7(9) . . ?
C60 N4 H4A 107.5 . . ?
C58 N4 H4A 107.5 . . ?
C62 N4 H4A 107.5 . . ?
C59 C58 N4 118.2(10) . . ?
C59 C58 H58A 107.8 . . ?
N4 C58 H58A 107.8 . . ?
C59 C58 H58B 107.8 . . ?
N4 C58 H58B 107.8 . . ?
H58A C58 H58B 107.1 . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
N4 C60 C61 116.7(11) . . ?
N4 C60 H60A 108.1 . . ?
C61 C60 H60A 108.1 . . ?
N4 C60 H60B 108.1 . . ?
C61 C60 H60B 108.1 . . ?
H60A C60 H60B 107.3 . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C63 C62 N4 108.1(10) . . ?
C63 C62 H62A 110.1 . . ?
N4 C62 H62A 110.1 . . ?
C63 C62 H62B 110.1 . . ?
N4 C62 H62B 110.1 . . ?
H62A C62 H62B 108.4 . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
Cl4 C55 Cl5 110.1(7) . . ?
Cl4 C55 H55A 109.6 . . ?
Cl5 C55 H55A 109.6 . . ?
Cl4 C55 H55B 109.6 . . ?
Cl5 C55 H55B 109.6 . . ?
H55A C55 H55B 108.2 . . ?
Cl6 C56 Cl7 112.1(9) . . ?
Cl6 C56 H56A 109.2 . . ?
Cl7 C56 H56A 109.2 . . ?
Cl6 C56 H56B 109.2 . . ?
Cl7 C56 H56B 109.2 . . ?
H56A C56 H56B 107.9 . . ?
Cl8 C57 Cl9 104.1(9) . . ?
Cl8 C57 H57A 110.9 . . ?
Cl9 C57 H57A 110.9 . . ?
Cl8 C57 H57B 110.9 . . ?
Cl9 C57 H57B 110.9 . . ?
H57A C57 H57B 109.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni2 O2 C1 O3 -11.8(12) . . . . ?
Ni2 O2 C1 C6 170.0(5) . . . . ?
Ni3 O3 C1 O2 156.9(6) . . . . ?
Ni1 O3 C1 O2 32.5(10) . . . . ?
Ni3 O3 C1 C6 -25.0(8) . . . . ?
Ni1 O3 C1 C6 -149.3(5) . . . . ?
Ni3 O4 C2 C14 -141.8(6) . . . . ?
Ni3 O4 C2 C3 40.0(10) . . . . ?
O4 C2 C3 C11 177.2(7) . . . . ?
C14 C2 C3 C11 -1.0(11) . . . . ?
O4 C2 C3 C4 2.9(12) . . . . ?
C14 C2 C3 C4 -175.3(7) . . . . ?
C5 N1 C4 C3 178.7(7) . . . . ?
Ni3 N1 C4 C3 -0.7(10) . . . . ?
C2 C3 C4 N1 -25.1(11) . . . . ?
C11 C3 C4 N1 160.5(7) . . . . ?
C4 N1 C5 C10 49.1(10) . . . . ?
Ni3 N1 C5 C10 -131.5(7) . . . . ?
C4 N1 C5 C6 -138.6(7) . . . . ?
Ni3 N1 C5 C6 40.8(9) . . . . ?
C10 C5 C6 C7 -0.4(11) . . . . ?
N1 C5 C6 C7 -172.8(7) . . . . ?
C10 C5 C6 C1 176.8(7) . . . . ?
N1 C5 C6 C1 4.4(11) . . . . ?
O2 C1 C6 C7 -17.6(9) . . . . ?
O3 C1 C6 C7 164.0(6) . . . . ?
O2 C1 C6 C5 165.1(7) . . . . ?
O3 C1 C6 C5 -13.2(11) . . . . ?
C5 C6 C7 C8 0.8(11) . . . . ?
C1 C6 C7 C8 -176.7(7) . . . . ?
C6 C7 C8 C9 -1.6(12) . . . . ?
C6 C7 C8 Cl1 176.4(6) . . . . ?
C7 C8 C9 C10 1.9(12) . . . . ?
Cl1 C8 C9 C10 -176.0(6) . . . . ?
N1 C5 C10 C9 173.2(7) . . . . ?
C6 C5 C10 C9 0.9(12) . . . . ?
C8 C9 C10 C5 -1.6(12) . . . . ?
C2 C3 C11 C18 179.0(8) . . . . ?
C4 C3 C11 C18 -6.7(12) . . . . ?
C2 C3 C11 C12 1.1(12) . . . . ?
C4 C3 C11 C12 175.4(8) . . . . ?
C18 C11 C12 C15 -1.4(13) . . . . ?
C3 C11 C12 C15 176.6(9) . . . . ?
C18 C11 C12 C13 -177.6(9) . . . . ?
C3 C11 C12 C13 0.4(13) . . . . ?
C15 C12 C13 C14 -178.2(10) . . . . ?
C11 C12 C13 C14 -2.1(15) . . . . ?
C12 C13 C14 C2 2.3(16) . . . . ?
O4 C2 C14 C13 -179.0(9) . . . . ?
C3 C2 C14 C13 -0.7(13) . . . . ?
C11 C12 C15 C16 3.5(17) . . . . ?
C13 C12 C15 C16 179.5(11) . . . . ?
C12 C15 C16 C17 -2.9(18) . . . . ?
C15 C16 C17 C18 0.3(18) . . . . ?
C16 C17 C18 C11 1.7(16) . . . . ?
C12 C11 C18 C17 -1.1(13) . . . . ?
C3 C11 C18 C17 -178.9(9) . . . . ?
Ni2 O5 C19 O6 -11.4(12) . . . . ?
Ni2 O5 C19 C20 167.5(5) . . . . ?
Ni3 O6 C19 O5 -147.3(6) 3_755 . . . ?
Ni1 O6 C19 O5 -24.2(10) 3_755 . . . ?
Ni3 O6 C19 C20 33.9(8) 3_755 . . . ?
Ni1 O6 C19 C20 157.0(5) 3_755 . . . ?
O5 C19 C20 C36 1.9(10) . . . . ?
O6 C19 C20 C36 -179.2(7) . . . . ?
O5 C19 C20 C21 -178.3(7) . . . . ?
O6 C19 C20 C21 0.6(11) . . . . ?
C36 C20 C21 C33 0.9(11) . . . . ?
C19 C20 C21 C33 -179.0(7) . . . . ?
C36 C20 C21 N2 179.1(7) . . . . ?
C19 C20 C21 N2 -0.8(12) . . . . ?
C22 N2 C21 C33 -38.4(11) . . . . ?
Ni3 N2 C21 C33 145.0(6) 3_755 . . . ?
C22 N2 C21 C20 143.4(7) . . . . ?
Ni3 N2 C21 C20 -33.3(9) 3_755 . . . ?
C21 N2 C22 C23 -172.9(7) . . . . ?
Ni3 N2 C22 C23 3.7(10) 3_755 . . . ?
N2 C22 C23 C24 33.3(12) . . . . ?
N2 C22 C23 C28 -155.9(8) . . . . ?
Ni3 O7 C24 C23 -38.8(9) 3_755 . . . ?
Ni3 O7 C24 C25 144.5(6) 3_755 . . . ?
C22 C23 C24 O7 -12.0(12) . . . . ?
C28 C23 C24 O7 177.3(7) . . . . ?
C22 C23 C24 C25 164.7(7) . . . . ?
C28 C23 C24 C25 -6.0(11) . . . . ?
O7 C24 C25 C26 -176.6(8) . . . . ?
C23 C24 C25 C26 6.5(12) . . . . ?
C24 C25 C26 C27 -2.7(13) . . . . ?
C25 C26 C27 C32 176.7(9) . . . . ?
C25 C26 C27 C28 -1.6(13) . . . . ?
C32 C27 C28 C29 1.0(13) . . . . ?
C26 C27 C28 C29 179.3(9) . . . . ?
C32 C27 C28 C23 -176.4(8) . . . . ?
C26 C27 C28 C23 2.0(12) . . . . ?
C24 C23 C28 C29 -175.3(9) . . . . ?
C22 C23 C28 C29 13.8(13) . . . . ?
C24 C23 C28 C27 1.8(12) . . . . ?
C22 C23 C28 C27 -169.1(8) . . . . ?
C27 C28 C29 C30 -1.1(15) . . . . ?
C23 C28 C29 C30 176.1(10) . . . . ?
C28 C29 C30 C31 -0.2(18) . . . . ?
C29 C30 C31 C32 1.6(18) . . . . ?
C30 C31 C32 C27 -1.7(16) . . . . ?
C26 C27 C32 C31 -177.9(10) . . . . ?
C28 C27 C32 C31 0.4(14) . . . . ?
C20 C21 C33 C34 -0.9(13) . . . . ?
N2 C21 C33 C34 -179.2(8) . . . . ?
C21 C33 C34 C35 0.9(13) . . . . ?
C33 C34 C35 C36 -0.9(13) . . . . ?
C33 C34 C35 Cl2 179.5(7) . . . . ?
C34 C35 C36 C20 0.9(13) . . . . ?
Cl2 C35 C36 C20 -179.5(6) . . . . ?
C21 C20 C36 C35 -0.9(12) . . . . ?
C19 C20 C36 C35 179.0(7) . . . . ?
Ni2 O8 C37 O9 -172.1(5) . . . . ?
Ni2 O8 C37 C38 7.1(10) . . . . ?
O8 C37 C38 C54 159.7(7) . . . . ?
O9 C37 C38 C54 -21.0(10) . . . . ?
O8 C37 C38 C39 -21.7(11) . . . . ?
O9 C37 C38 C39 157.6(7) . . . . ?
C54 C38 C39 C51 -4.4(10) . . . . ?
C37 C38 C39 C51 177.0(7) . . . . ?
C54 C38 C39 N3 178.0(6) . . . . ?
C37 C38 C39 N3 -0.5(11) . . . . ?
C40 N3 C39 C51 31.9(9) . . . . ?
Ni2 N3 C39 C51 -144.8(6) . . . . ?
C40 N3 C39 C38 -150.6(7) . . . . ?
Ni2 N3 C39 C38 32.7(8) . . . . ?
C39 N3 C40 C41 -167.7(7) . . . . ?
Ni2 N3 C40 C41 8.9(10) . . . . ?
N3 C40 C41 C42 16.9(12) . . . . ?
N3 C40 C41 C46 -170.0(7) . . . . ?
Ni2 O10 C42 C41 -20.7(10) . . . . ?
Ni2 O10 C42 C43 160.3(6) . . . . ?
C40 C41 C42 O10 -10.4(12) . . . . ?
C46 C41 C42 O10 176.8(7) . . . . ?
C40 C41 C42 C43 168.6(8) . . . . ?
C46 C41 C42 C43 -4.3(11) . . . . ?
O10 C42 C43 C44 -177.6(9) . . . . ?
C41 C42 C43 C44 3.4(14) . . . . ?
C42 C43 C44 C45 -1.3(17) . . . . ?
C43 C44 C45 C46 0.2(17) . . . . ?
C43 C44 C45 C50 178.9(11) . . . . ?
C50 C45 C46 C47 -0.7(14) . . . . ?
C44 C45 C46 C47 178.1(9) . . . . ?
C50 C45 C46 C41 -179.9(9) . . . . ?
C44 C45 C46 C41 -1.2(14) . . . . ?
C42 C41 C46 C47 -175.9(7) . . . . ?
C40 C41 C46 C47 11.0(11) . . . . ?
C42 C41 C46 C45 3.3(12) . . . . ?
C40 C41 C46 C45 -169.8(8) . . . . ?
C45 C46 C47 C48 0.8(12) . . . . ?
C41 C46 C47 C48 180.0(7) . . . . ?
C46 C47 C48 C49 -1.5(12) . . . . ?
C47 C48 C49 C50 2.0(14) . . . . ?
C48 C49 C50 C45 -1.9(16) . . . . ?
C46 C45 C50 C49 1.2(17) . . . . ?
C44 C45 C50 C49 -177.5(11) . . . . ?
C38 C39 C51 C52 3.8(11) . . . . ?
N3 C39 C51 C52 -178.6(7) . . . . ?
C39 C51 C52 C53 -0.6(12) . . . . ?
C51 C52 C53 C54 -2.0(12) . . . . ?
C51 C52 C53 Cl3 178.5(6) . . . . ?
C52 C53 C54 C38 1.3(12) . . . . ?
Cl3 C53 C54 C38 -179.2(6) . . . . ?
C39 C38 C54 C53 2.0(11) . . . . ?
C37 C38 C54 C53 -179.3(7) . . . . ?
C60 N4 C58 C59 -156.4(12) . . . . ?
C62 N4 C58 C59 76.5(14) . . . . ?
C58 N4 C60 C61 -55.2(17) . . . . ?
C62 N4 C60 C61 65.4(16) . . . . ?
C60 N4 C62 C63 59.2(13) . . . . ?
C58 N4 C62 C63 -174.6(10) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4 H4A O8 1.00 2.51 3.264(9) 131.8 3_655
N4 H4A O9 1.00 1.75 2.739(9) 169.2 3_655
O11 H1W O7 0.86(2) 1.92(3) 2.744(7) 161(9) 3_755
O11 H2W O10 0.86(2) 1.86(2) 2.712(7) 172(9) .
O12 H3W O4 0.85(2) 2.08(6) 2.781(7) 140(8) .
O12 H4W O10 0.85(2) 1.98(3) 2.811(7) 165(7) 3_755

_refine_diff_density_max         3.081
_refine_diff_density_min         -1.837
_refine_diff_density_rms         0.163




#=============================================================================#
#    Luis Cunha-Silva @ REQUIMTE / LAQV & DQB FCUP  *  11/05/2016  *   END    #
#=============================================================================#
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_comp_5
_database_code_depnum_ccdc_archive 'CCDC 1448724'
_audit_update_record             
;
2016-01-20 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;

# ========================================================================= #

_audit_creation_method           'SHELXL-2014/7 and enCIFer'
_shelx_SHELXL_version_number     2014/7
_audit_creation_date             '20 January 2016'

# ========================================================================= #

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C38 H28 Cl2 N2 Na2 Ni O8, C38 H32 Cl2 N2 Na2 Ni O10'
_chemical_formula_sum            'C76 H60 Cl4 N4 Na4 Ni2 O18'
_chemical_formula_weight         1668.46

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.5505(16)
_cell_length_b                   18.877(4)
_cell_length_c                   26.086(6)
_cell_angle_alpha                79.415(11)
_cell_angle_beta                 86.090(10)
_cell_angle_gamma                89.411(10)
_cell_volume                     3646.2(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9793
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      26.49

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_F_000             1712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.762
_shelx_estimated_absorpt_T_min   0.766
_shelx_estimated_absorpt_T_max   0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_process_details   
; 
'SADABS V2012/1 (Bruker AXS Inc.)' 
;


_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            83856
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.698
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.027
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             12700
_reflns_number_gt                11079
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX2 (Bruker AXS Inc., 2012)'
_computing_cell_refinement       'SAINT (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT (Bruker AXS Inc., 2012)'
_computing_structure_solution    'SHELXS (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2014)'


_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+12.2636P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12700
_refine_ls_number_parameters     1034
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0607
_refine_ls_wR_factor_ref         0.1221
_refine_ls_wR_factor_gt          0.1179
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_restrained_S_all      4.456
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.72458(6) 0.18244(3) 0.51973(2) 0.01665(12) Uani 1 1 d . . . . .
Cl1 Cl 1.2811(2) 0.25009(9) 0.28355(5) 0.0605(4) Uani 1 1 d . . . . .
Cl2 Cl 0.17608(18) 0.16326(7) 0.75006(4) 0.0433(3) Uani 1 1 d . . . . .
Na1 Na 0.2997(2) -0.00139(8) 0.49702(6) 0.0228(3) Uani 1 1 d . . . . .
Na2 Na -0.0311(2) 0.05398(9) 0.58365(6) 0.0242(4) Uani 1 1 d . . . . .
O1 O 0.8161(4) 0.17325(15) 0.59345(11) 0.0240(6) Uani 1 1 d . . . . .
O2 O 0.8917(4) 0.10453(14) 0.49896(10) 0.0201(6) Uani 1 1 d . . . . .
O3 O 1.0618(4) 0.05632(15) 0.44174(11) 0.0271(7) Uani 1 1 d . . . . .
O4 O 0.2624(4) 0.06818(15) 0.56516(12) 0.0260(7) Uani 1 1 d . . . . .
O5 O 0.5463(4) 0.09846(14) 0.54434(11) 0.0216(6) Uani 1 1 d . . . . .
O6 O 0.6363(4) 0.20279(14) 0.44667(11) 0.0205(6) Uani 1 1 d . . . . .
O7 O 0.5067(4) 0.07233(15) 0.43918(11) 0.0255(7) Uani 1 1 d D . . . .
H4 H 0.507(7) 0.1161(13) 0.4432(19) 0.038 Uiso 1 1 d D U . . .
O8 O -0.2055(6) 0.04750(19) 0.65968(14) 0.0518(10) Uani 1 1 d D . . . .
H5 H -0.218(9) 0.0916(14) 0.647(2) 0.078 Uiso 1 1 d D U . . .
N1 N 0.9356(4) 0.24944(17) 0.49572(14) 0.0213(7) Uani 1 1 d . . . . .
N2 N 0.5276(4) 0.24994(17) 0.53711(13) 0.0181(7) Uani 1 1 d . . . . .
C1 C 1.1787(6) 0.2508(3) 0.34560(18) 0.0355(11) Uani 1 1 d . . . . .
C2 C 1.1451(6) 0.3150(3) 0.36206(19) 0.0398(12) Uani 1 1 d . . . . .
H2 H 1.1768 0.3594 0.3399 0.048 Uiso 1 1 calc R U . . .
C3 C 1.0644(6) 0.3139(2) 0.41154(19) 0.0315(11) Uani 1 1 d . . . . .
H3 H 1.0404 0.3582 0.4229 0.038 Uiso 1 1 calc R U . . .
C4 C 1.0178(5) 0.2497(2) 0.44491(16) 0.0230(9) Uani 1 1 d . . . . .
C5 C 1.0480(5) 0.1841(2) 0.42719(16) 0.0214(9) Uani 1 1 d . . . . .
C6 C 1.1309(6) 0.1858(3) 0.37720(17) 0.0292(10) Uani 1 1 d . . . . .
H6 H 1.1543 0.1421 0.3650 0.035 Uiso 1 1 calc R U . . .
C7 C 0.9969(5) 0.1101(2) 0.45777(16) 0.0204(9) Uani 1 1 d . . . . .
C8 C 0.9980(5) 0.2913(2) 0.52420(18) 0.0252(10) Uani 1 1 d . . . . .
H8 H 1.0914 0.3232 0.5087 0.030 Uiso 1 1 calc R U . . .
C9 C 0.9381(6) 0.2937(2) 0.57731(19) 0.0287(10) Uani 1 1 d . . . . .
C10 C 0.8584(6) 0.2324(2) 0.60963(17) 0.0267(10) Uani 1 1 d . . . . .
C11 C 0.8245(7) 0.2349(3) 0.66447(19) 0.0378(12) Uani 1 1 d . . . . .
H11 H 0.7700 0.1946 0.6871 0.045 Uiso 1 1 calc R U . . .
C12 C 0.8690(7) 0.2938(3) 0.6846(2) 0.0487(15) Uani 1 1 d . . . . .
H12 H 0.8447 0.2932 0.7209 0.058 Uiso 1 1 calc R U . . .
C13 C 0.9504(7) 0.3558(3) 0.6530(2) 0.0481(15) Uani 1 1 d . . . . .
C14 C 0.9965(8) 0.4165(4) 0.6744(3) 0.069(2) Uani 1 1 d . . . . .
H14 H 0.9746 0.4154 0.7109 0.082 Uiso 1 1 calc R U . . .
C15 C 1.0717(8) 0.4765(4) 0.6437(4) 0.077(3) Uani 1 1 d . . . . .
H15 H 1.1031 0.5164 0.6587 0.093 Uiso 1 1 calc R U . . .
C16 C 1.1017(7) 0.4784(3) 0.5904(3) 0.070(2) Uani 1 1 d . . . . .
H16 H 1.1518 0.5199 0.5683 0.083 Uiso 1 1 calc R U . . .
C17 C 1.0583(7) 0.4200(3) 0.5705(3) 0.0545(17) Uani 1 1 d . . . . .
H17 H 1.0806 0.4225 0.5339 0.065 Uiso 1 1 calc DR U . . .
C18 C 0.9827(6) 0.3559(3) 0.5995(2) 0.0380(13) Uani 1 1 d . . . . .
C19 C 0.3968(5) 0.1053(2) 0.56828(15) 0.0201(9) Uani 1 1 d . . . . .
C20 C 0.3778(5) 0.1605(2) 0.60393(15) 0.0189(8) Uani 1 1 d . . . . .
C21 C 0.2926(5) 0.1407(2) 0.65375(16) 0.0241(9) Uani 1 1 d . . . . .
H21 H 0.2471 0.0933 0.6649 0.029 Uiso 1 1 calc R U . . .
C22 C 0.2748(6) 0.1903(2) 0.68666(16) 0.0273(10) Uani 1 1 d . . . . .
C23 C 0.3314(6) 0.2606(2) 0.67077(17) 0.0287(10) Uani 1 1 d . . . . .
H23 H 0.3151 0.2943 0.6936 0.034 Uiso 1 1 calc R U . . .
C24 C 0.4124(6) 0.2813(2) 0.62116(17) 0.0265(10) Uani 1 1 d . . . . .
H24 H 0.4506 0.3298 0.6098 0.032 Uiso 1 1 calc R U . . .
C25 C 0.4388(5) 0.2319(2) 0.58749(15) 0.0192(8) Uani 1 1 d . . . . .
C26 C 0.4805(5) 0.3063(2) 0.50494(16) 0.0209(9) Uani 1 1 d . . . . .
H26 H 0.4007 0.3388 0.5184 0.025 Uiso 1 1 calc R U . . .
C27 C 0.5384(5) 0.3238(2) 0.45090(16) 0.0202(9) Uani 1 1 d . . . . .
C28 C 0.6050(5) 0.2686(2) 0.42388(16) 0.0203(9) Uani 1 1 d . . . . .
C29 C 0.6358(6) 0.2859(2) 0.36805(17) 0.0262(10) Uani 1 1 d . . . . .
H29 H 0.6803 0.2496 0.3497 0.031 Uiso 1 1 calc R U . . .
C30 C 0.6032(6) 0.3525(2) 0.34078(17) 0.0305(10) Uani 1 1 d . . . . .
H30 H 0.6266 0.3618 0.3039 0.037 Uiso 1 1 calc R U . . .
C31 C 0.5347(6) 0.4089(2) 0.36588(17) 0.0274(10) Uani 1 1 d . . . . .
C32 C 0.4952(7) 0.4781(3) 0.33718(19) 0.0361(11) Uani 1 1 d . . . . .
H32 H 0.5154 0.4874 0.3002 0.043 Uiso 1 1 calc R U . . .
C33 C 0.4287(7) 0.5312(2) 0.3619(2) 0.0383(12) Uani 1 1 d . . . . .
H33 H 0.4027 0.5771 0.3420 0.046 Uiso 1 1 calc R U . . .
C34 C 0.3986(6) 0.5184(2) 0.4163(2) 0.0357(11) Uani 1 1 d . . . . .
H34 H 0.3512 0.5557 0.4332 0.043 Uiso 1 1 calc R U . . .
C35 C 0.4369(6) 0.4527(2) 0.44567(19) 0.0294(10) Uani 1 1 d . . . . .
H35 H 0.4193 0.4456 0.4827 0.035 Uiso 1 1 calc R U . . .
C36 C 0.5028(5) 0.3949(2) 0.42131(17) 0.0234(9) Uani 1 1 d . . . . .
C72 C 0.5255(7) 0.0725(3) 0.38438(17) 0.0351(11) Uani 1 1 d . . . . .
H72A H 0.4476 0.0356 0.3760 0.053 Uiso 1 1 calc R U . . .
H72B H 0.6490 0.0619 0.3743 0.053 Uiso 1 1 calc R U . . .
H72C H 0.4927 0.1199 0.3652 0.053 Uiso 1 1 calc R U . . .
C73 C -0.2812(9) 0.0262(4) 0.7103(2) 0.0659(19) Uani 1 1 d . . . . .
H73A H -0.2533 -0.0246 0.7230 0.099 Uiso 1 1 calc R U . . .
H73B H -0.4102 0.0323 0.7103 0.099 Uiso 1 1 calc R U . . .
H73C H -0.2333 0.0559 0.7333 0.099 Uiso 1 1 calc R U . . .
Ni2 Ni 0.23128(6) 0.29737(3) 1.03759(2) 0.01607(12) Uani 1 1 d . . . . .
Cl3 Cl 0.5006(2) 0.36737(8) 0.76981(5) 0.0605(4) Uani 1 1 d . . . . .
Cl4 Cl -0.1152(2) 0.11440(8) 1.28691(5) 0.0487(3) Uani 1 1 d . . . . .
O10 O 0.3815(4) 0.38730(14) 1.00871(11) 0.0202(6) Uani 1 1 d . . . . .
O11 O 0.0827(4) 0.35199(15) 1.08649(11) 0.0260(7) Uani 1 1 d . . . . .
O12 O 0.3893(4) 0.26698(14) 1.09776(11) 0.0221(6) Uani 1 1 d . . . . .
O13 O -0.0664(7) 0.36065(19) 1.16115(15) 0.0713(15) Uani 1 1 d . . . . .
O14 O 0.4783(5) 0.39063(18) 1.12575(13) 0.0452(10) Uani 1 1 d D . . . .
H1 H 0.461(8) 0.3486(17) 1.120(2) 0.068 Uiso 1 1 d D U . . .
O18 O 0.9181(8) 0.5127(2) 0.8511(2) 0.090(2) Uani 1 1 d D . . . .
H7 H 0.964(13) 0.554(5) 0.845(4) 0.136 Uiso 1 1 d . U . . .
O19 O 0.0702(3) 0.32961(13) 0.97723(10) 0.0186(6) Uani 1 1 d . . . . .
N3 N 0.4116(4) 0.24469(16) 0.99640(12) 0.0175(7) Uani 1 1 d . . . . .
N4 N 0.0543(4) 0.21575(16) 1.05962(12) 0.0169(7) Uani 1 1 d . . . . .
C37 C 0.4428(8) 0.4022(2) 0.9622(2) 0.0447(15) Uani 1 1 d . . . . .
C38 C 0.4519(6) 0.3483(2) 0.92585(17) 0.0274(10) Uani 1 1 d . . . . .
C39 C 0.4720(7) 0.3752(2) 0.87263(19) 0.0391(13) Uani 1 1 d . . . . .
H39 H 0.4804 0.4259 0.8609 0.047 Uiso 1 1 calc R U . . .
C40 C 0.4801(6) 0.3310(2) 0.83668(17) 0.0333(11) Uani 1 1 d . . . . .
C41 C 0.4708(6) 0.2564(2) 0.85197(17) 0.0280(10) Uani 1 1 d . . . . .
H41 H 0.4768 0.2257 0.8268 0.034 Uiso 1 1 calc R U . . .
C42 C 0.4524(6) 0.2283(2) 0.90483(16) 0.0229(9) Uani 1 1 d . . . . .
H42 H 0.4468 0.1776 0.9161 0.028 Uiso 1 1 calc R U . . .
C43 C 0.4419(5) 0.2730(2) 0.94227(16) 0.0195(8) Uani 1 1 d . . . . .
C44 C 0.4945(5) 0.1868(2) 1.01709(16) 0.0198(9) Uani 1 1 d . . . . .
H44 H 0.5660 0.1628 0.9942 0.024 Uiso 1 1 calc R U . . .
C45 C 0.4861(5) 0.1562(2) 1.07209(16) 0.0189(8) Uani 1 1 d . . . . .
C46 C 0.4432(5) 0.2007(2) 1.10983(16) 0.0203(9) Uani 1 1 d . . . . .
C47 C 0.4669(6) 0.1724(2) 1.16390(17) 0.0259(9) Uani 1 1 d . . . . .
H47 H 0.4412 0.2022 1.1891 0.031 Uiso 1 1 calc R U . . .
C48 C 0.5252(6) 0.1041(2) 1.17986(17) 0.0257(9) Uani 1 1 d . . . . .
H48 H 0.5383 0.0870 1.2160 0.031 Uiso 1 1 calc R U . . .
C49 C 0.5674(5) 0.0574(2) 1.14345(17) 0.0229(9) Uani 1 1 d . . . . .
C50 C 0.5485(5) 0.0833(2) 1.08912(16) 0.0214(9) Uani 1 1 d . . . . .
C51 C 0.5922(5) 0.0357(2) 1.05447(17) 0.0236(9) Uani 1 1 d . . . . .
H51 H 0.5730 0.0502 1.0185 0.028 Uiso 1 1 calc R U . . .
C52 C 0.6626(6) -0.0318(2) 1.07178(18) 0.0256(10) Uani 1 1 d . . . . .
H52 H 0.6965 -0.0619 1.0474 0.031 Uiso 1 1 calc R U . . .
C53 C 0.6840(6) -0.0558(2) 1.12483(19) 0.0292(10) Uani 1 1 d . . . . .
H53 H 0.7327 -0.1021 1.1365 0.035 Uiso 1 1 calc R U . . .
C54 C 0.6346(6) -0.0124(2) 1.16012(18) 0.0279(10) Uani 1 1 d . . . . .
H54 H 0.6458 -0.0297 1.1963 0.033 Uiso 1 1 calc R U . . .
C55 C 0.0031(6) 0.3240(2) 1.12996(17) 0.0309(10) Uani 1 1 d . . . . .
C56 C -0.0084(5) 0.2427(2) 1.14746(16) 0.0225(9) Uani 1 1 d . . . . .
C57 C -0.0499(6) 0.2177(2) 1.20072(16) 0.0277(10) Uani 1 1 d . . . . .
H57 H -0.0718 0.2511 1.2236 0.033 Uiso 1 1 calc R U . . .
C58 C -0.0590(6) 0.1444(3) 1.22008(17) 0.0305(10) Uani 1 1 d . . . . .
C59 C -0.0270(6) 0.0940(2) 1.18804(17) 0.0279(10) Uani 1 1 d . . . . .
H59 H -0.0301 0.0439 1.2022 0.033 Uiso 1 1 calc R U . . .
C60 C 0.0094(5) 0.1182(2) 1.13516(16) 0.0228(9) Uani 1 1 d . . . . .
H60 H 0.0297 0.0842 1.1127 0.027 Uiso 1 1 calc R U . . .
C61 C 0.0171(5) 0.1919(2) 1.11409(15) 0.0189(8) Uani 1 1 d . . . . .
C62 C -0.0129(5) 0.2093(2) 0.97083(15) 0.0179(8) Uani 1 1 d . . . . .
C63 C -0.1001(5) 0.0866(2) 0.95569(17) 0.0226(9) Uani 1 1 d . . . . .
H63 H -0.0787 0.0662 0.9908 0.027 Uiso 1 1 calc R U . . .
C64 C -0.0677(5) 0.1614(2) 0.93719(16) 0.0200(9) Uani 1 1 d . . . . .
C65 C -0.1617(6) 0.0433(2) 0.92381(18) 0.0272(10) Uani 1 1 d . . . . .
H65 H -0.1873 -0.0059 0.9376 0.033 Uiso 1 1 calc R U . . .
C66 C -0.1872(6) 0.0710(2) 0.87106(18) 0.0298(10) Uani 1 1 d . . . . .
H66 H -0.2302 0.0407 0.8493 0.036 Uiso 1 1 calc R U . . .
C67 C -0.1498(6) 0.1418(2) 0.85134(17) 0.0278(10) Uani 1 1 d . . . . .
H67 H -0.1645 0.1602 0.8155 0.033 Uiso 1 1 calc R U . . .
C68 C -0.0892(5) 0.1883(2) 0.88368(16) 0.0233(9) Uani 1 1 d . . . . .
C69 C -0.0548(6) 0.2632(2) 0.86362(17) 0.0290(10) Uani 1 1 d . . . . .
H69 H -0.0696 0.2821 0.8278 0.035 Uiso 1 1 calc R U . . .
C70 C -0.0012(6) 0.3074(2) 0.89531(17) 0.0274(10) Uani 1 1 d . . . . .
H70 H 0.0216 0.3567 0.8808 0.033 Uiso 1 1 calc R U . . .
C71 C 0.0221(5) 0.2827(2) 0.94934(16) 0.0191(8) Uani 1 1 d . . . . .
C74 C 0.4948(9) 0.3866(3) 1.1791(2) 0.0549(15) Uani 1 1 d . . . . .
H74A H 0.5333 0.4335 1.1855 0.082 Uiso 1 1 calc R U . . .
H74B H 0.5829 0.3499 1.1912 0.082 Uiso 1 1 calc R U . . .
H74C H 0.3800 0.3737 1.1982 0.082 Uiso 1 1 calc R U . . .
C75 C 0.9062(15) 0.4843(4) 0.8060(4) 0.122(4) Uani 1 1 d . . . . .
H75A H 0.8375 0.4394 0.8142 0.183 Uiso 1 1 calc R U . . .
H75B H 1.0256 0.4745 0.7919 0.183 Uiso 1 1 calc R U . . .
H75C H 0.8470 0.5191 0.7800 0.183 Uiso 1 1 calc R U . . .
C5RH C -0.0247(5) 0.1850(2) 1.02685(15) 0.0182(8) Uani 1 1 d . . . . .
H5RH H -0.0951 0.1435 1.0406 0.022 Uiso 1 1 calc R U . . .
O15 O 0.8762(9) 0.5226(3) 1.0607(3) 0.0285(14) Uani 0.5 1 d . . P A 1
O20 O 0.7403(8) 0.3362(3) 1.0441(3) 0.0313(15) Uani 0.5 1 d . . P A 1
Na3A Na 0.6915(6) 0.5387(2) 0.93208(18) 0.0285(9) Uani 0.5 1 d . . P A 1
Na4A Na 0.6381(4) 0.44699(17) 1.04959(13) 0.0245(7) Uani 0.5 1 d . . P A 1
O9A O 0.5630(8) 0.4557(3) 0.9535(2) 0.0235(13) Uani 0.5 1 d . . P A 1
O16 O 0.7630(10) 0.3996(6) 1.0051(4) 0.074(3) Uani 0.5 1 d . . P A 2
O17 O 1.0026(8) 0.4766(3) 0.9651(2) 0.0275(13) Uani 0.5 1 d . . P A 2
Na3B Na 0.7768(6) 0.5366(2) 0.91659(17) 0.0257(9) Uani 0.5 1 d . . P A 2
Na4B Na 0.7709(5) 0.44325(17) 1.08292(13) 0.0281(8) Uani 0.5 1 d . . P A 2
O9B O 0.4396(8) 0.4688(3) 0.9341(2) 0.0250(13) Uani 0.5 1 d . . P A 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
Ni1 N2 2.030(3) . ?
Ni1 O6 2.031(3) . ?
Ni1 N1 2.036(3) . ?
Ni1 O2 2.052(3) . ?
Ni1 O1 2.064(3) . ?
Ni1 O5 2.071(3) . ?
Ni1 Na2 3.3026(18) 1_655 ?
Ni1 Na1 3.5323(17) 2_656 ?
Cl1 C1 1.748(5) . ?
Cl2 C22 1.755(4) . ?
Na1 O7 2.368(3) . ?
Na1 O4 2.397(3) . ?
Na1 O2 2.419(3) 2_656 ?
Na1 O7 2.484(3) 2_656 ?
Na1 O3 2.496(3) 1_455 ?
Na1 O5 2.527(3) 2_656 ?
Na1 Na1 3.041(3) 2_656 ?
Na1 C7 3.076(4) 2_656 ?
Na1 Na2 3.304(2) 2_556 ?
Na1 Ni1 3.5322(17) 2_656 ?
Na2 O4 2.243(3) . ?
Na2 O8 2.289(4) . ?
Na2 O3 2.316(3) 2_656 ?
Na2 O2 2.350(3) 1_455 ?
Na2 O1 2.566(3) 1_455 ?
Na2 Ni1 3.3026(18) 1_455 ?
Na2 Na1 3.304(2) 2_556 ?
Na2 H5 2.30(7) . ?
O1 C10 1.314(5) . ?
O1 Na2 2.566(3) 1_655 ?
O2 C7 1.281(5) . ?
O2 Na2 2.350(3) 1_655 ?
O2 Na1 2.419(3) 2_656 ?
O3 C7 1.250(5) . ?
O3 Na2 2.316(3) 2_656 ?
O3 Na1 2.496(3) 1_655 ?
O4 C19 1.254(5) . ?
O5 C19 1.270(5) . ?
O5 Na1 2.527(3) 2_656 ?
O6 C28 1.302(5) . ?
O7 C72 1.426(5) . ?
O7 Na1 2.484(3) 2_656 ?
O7 H4 0.852(19) . ?
O8 C73 1.393(6) . ?
O8 H5 0.84(2) . ?
N1 C8 1.292(5) . ?
N1 C4 1.424(5) . ?
N2 C26 1.292(5) . ?
N2 C25 1.419(5) . ?
C1 C2 1.373(7) . ?
C1 C6 1.382(6) . ?
C2 C3 1.386(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.409(6) . ?
C5 C6 1.402(6) . ?
C5 C7 1.516(6) . ?
C6 H6 0.9500 . ?
C7 Na1 3.076(4) 2_656 ?
C8 C9 1.436(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.414(7) . ?
C9 C18 1.453(6) . ?
C10 C11 1.445(6) . ?
C11 C12 1.368(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.422(9) . ?
C12 H12 0.9500 . ?
C13 C18 1.399(8) . ?
C13 C14 1.421(7) . ?
C14 C15 1.364(11) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(10) . ?
C15 H15 0.9500 . ?
C16 C17 1.354(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.407(8) . ?
C17 H17 0.9500 . ?
C19 C20 1.519(5) . ?
C20 C21 1.398(6) . ?
C20 C25 1.408(6) . ?
C21 C22 1.382(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.378(6) . ?
C23 C24 1.383(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.398(6) . ?
C24 H24 0.9500 . ?
C26 C27 1.427(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.430(6) . ?
C27 C36 1.453(5) . ?
C28 C29 1.436(6) . ?
C29 C30 1.355(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.425(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.421(6) . ?
C31 C36 1.426(6) . ?
C32 C33 1.362(7) . ?
C32 H32 0.9500 . ?
C33 C34 1.400(7) . ?
C33 H33 0.9500 . ?
C34 C35 1.371(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.429(6) . ?
C35 H35 0.9500 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
Ni2 N4 2.025(3) . ?
Ni2 O12 2.032(3) . ?
Ni2 N3 2.040(3) . ?
Ni2 O10 2.047(3) . ?
Ni2 O11 2.052(3) . ?
Ni2 O19 2.055(3) . ?
Ni2 Na3A 3.398(4) 2_667 ?
Ni2 Na3B 3.552(4) 2_667 ?
Cl3 C40 1.750(4) . ?
Cl4 C58 1.755(4) . ?
O10 C37 1.251(5) . ?
O10 Na3A 2.303(5) 2_667 ?
O10 Na4A 2.632(4) . ?
O10 Na3B 2.822(5) 2_667 ?
O11 C55 1.272(5) . ?
O11 Na3B 2.351(5) 2_667 ?
O11 Na3A 2.645(5) 2_667 ?
O11 Na4B 2.899(4) 1_455 ?
O12 C46 1.300(5) . ?
O13 C55 1.248(5) . ?
O13 Na4B 2.690(6) 1_455 ?
O14 C74 1.395(6) . ?
O14 Na3A 2.278(6) 2_667 ?
O14 Na4A 2.336(5) . ?
O14 Na4B 2.534(5) . ?
O14 Na3B 2.548(6) 2_667 ?
O14 H1 0.85(2) . ?
O18 C75 1.388(9) . ?
O18 Na3B 2.070(8) . ?
O18 Na3A 2.739(8) . ?
O18 H7 0.85(9) . ?
O19 C71 1.314(5) . ?
N3 C44 1.301(5) . ?
N3 C43 1.419(5) . ?
N4 C5RH 1.298(5) . ?
N4 C61 1.419(5) . ?
C37 O9B 1.335(7) . ?
C37 O9A 1.342(7) . ?
C37 C38 1.512(6) . ?
C37 Na4A 2.871(5) 2_667 ?
C38 C39 1.387(6) . ?
C38 C43 1.408(5) . ?
C39 C40 1.364(7) . ?
C39 H39 0.9500 . ?
C40 C41 1.393(6) . ?
C41 C42 1.381(6) . ?
C41 H41 0.9500 . ?
C42 C43 1.401(6) . ?
C42 H42 0.9500 . ?
C44 C45 1.442(6) . ?
C44 H44 0.9500 . ?
C45 C46 1.427(6) . ?
C45 C50 1.450(5) . ?
C46 C47 1.436(6) . ?
C47 C48 1.359(6) . ?
C47 H47 0.9500 . ?
C48 C49 1.429(6) . ?
C48 H48 0.9500 . ?
C49 C54 1.411(6) . ?
C49 C50 1.428(6) . ?
C50 C51 1.409(6) . ?
C51 C52 1.383(6) . ?
C51 H51 0.9500 . ?
C52 C53 1.395(6) . ?
C52 H52 0.9500 . ?
C53 C54 1.372(6) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C55 C56 1.521(6) . ?
C55 Na4B 2.973(6) 1_455 ?
C55 Na3B 3.130(6) 2_667 ?
C56 C57 1.398(6) . ?
C56 C61 1.413(6) . ?
C57 C58 1.385(6) . ?
C57 H57 0.9500 . ?
C58 C59 1.387(6) . ?
C59 C60 1.381(6) . ?
C59 H59 0.9500 . ?
C60 C61 1.398(6) . ?
C60 H60 0.9500 . ?
C62 C71 1.415(5) . ?
C62 C5RH 1.446(6) . ?
C62 C64 1.452(5) . ?
C63 C65 1.373(6) . ?
C63 C64 1.425(6) . ?
C63 H63 0.9500 . ?
C64 C68 1.414(6) . ?
C65 C66 1.405(6) . ?
C65 H65 0.9500 . ?
C66 C67 1.365(6) . ?
C66 H66 0.9500 . ?
C67 C68 1.424(6) . ?
C67 H67 0.9500 . ?
C68 C69 1.434(6) . ?
C69 C70 1.360(6) . ?
C69 H69 0.9500 . ?
C70 C71 1.423(6) . ?
C70 H70 0.9500 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C5RH H5RH 0.9500 . ?
O15 Na4A 2.373(7) . ?
O20 Na4A 2.248(7) . ?
Na3A O9A 1.828(7) . ?
Na3A O14 2.278(6) 2_667 ?
Na3A O10 2.303(5) 2_667 ?
Na3A Na4A 2.523(6) 2_667 ?
Na3A O11 2.645(5) 2_667 ?
Na3A Ni2 3.398(4) 2_667 ?
Na4A O9A 2.365(7) 2_667 ?
Na4A Na3A 2.523(6) 2_667 ?
Na4A O9A 2.582(7) . ?
Na4A C37 2.871(5) 2_667 ?
Na4A Na4A 3.715(7) 2_667 ?
Na4A H1 2.65(6) . ?
O9A Na4A 2.365(7) 2_667 ?
O16 Na4B 2.331(8) . ?
O17 Na3B 2.349(7) . ?
O17 Na4B 2.418(7) 2_767 ?
Na3B O11 2.350(5) 2_667 ?
Na3B O14 2.548(6) 2_667 ?
Na3B O10 2.822(5) 2_667 ?
Na3B O9B 2.833(8) . ?
Na3B C55 3.130(6) 2_667 ?
Na3B Na4B 3.441(6) 2_767 ?
Na3B Ni2 3.552(4) 2_667 ?
Na3B Na4B 4.149(6) 2_667 ?
Na3B H7 2.23(10) . ?
Na4B O9B 2.292(7) 2_667 ?
Na4B O17 2.418(7) 2_767 ?
Na4B O13 2.690(6) 1_655 ?
Na4B O11 2.899(4) 1_655 ?
Na4B C55 2.973(6) 1_655 ?
Na4B Na3B 3.441(6) 2_767 ?
Na4B Na3B 4.149(6) 2_667 ?
O9B Na4B 2.292(7) 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
N2 Ni1 O6 84.98(12) . . ?
N2 Ni1 N1 103.56(13) . . ?
O6 Ni1 N1 90.70(13) . . ?
N2 Ni1 O2 170.81(12) . . ?
O6 Ni1 O2 90.29(11) . . ?
N1 Ni1 O2 84.34(12) . . ?
N2 Ni1 O1 91.40(12) . . ?
O6 Ni1 O1 174.02(11) . . ?
N1 Ni1 O1 85.51(13) . . ?
O2 Ni1 O1 93.93(11) . . ?
N2 Ni1 O5 87.40(12) . . ?
O6 Ni1 O5 92.50(11) . . ?
N1 Ni1 O5 168.82(12) . . ?
O2 Ni1 O5 84.94(11) . . ?
O1 Ni1 O5 92.09(11) . . ?
N2 Ni1 Na2 137.46(10) . 1_655 ?
O6 Ni1 Na2 134.07(8) . 1_655 ?
N1 Ni1 Na2 93.57(10) . 1_655 ?
O2 Ni1 Na2 44.92(8) . 1_655 ?
O1 Ni1 Na2 50.99(8) . 1_655 ?
O5 Ni1 Na2 76.55(8) . 1_655 ?
N2 Ni1 Na1 129.68(9) . 2_656 ?
O6 Ni1 Na1 83.00(8) . 2_656 ?
N1 Ni1 Na1 125.22(10) . 2_656 ?
O2 Ni1 Na1 41.61(8) . 2_656 ?
O1 Ni1 Na1 102.96(8) . 2_656 ?
O5 Ni1 Na1 44.80(8) . 2_656 ?
Na2 Ni1 Na1 57.70(4) 1_655 2_656 ?
O7 Na1 O4 99.82(11) . . ?
O7 Na1 O2 141.00(12) . 2_656 ?
O4 Na1 O2 118.48(11) . 2_656 ?
O7 Na1 O7 102.43(10) . 2_656 ?
O4 Na1 O7 81.09(11) . 2_656 ?
O2 Na1 O7 91.09(11) 2_656 2_656 ?
O7 Na1 O3 87.72(11) . 1_455 ?
O4 Na1 O3 98.04(11) . 1_455 ?
O2 Na1 O3 80.38(10) 2_656 1_455 ?
O7 Na1 O3 169.83(12) 2_656 1_455 ?
O7 Na1 O5 81.53(10) . 2_656 ?
O4 Na1 O5 151.59(12) . 2_656 ?
O2 Na1 O5 68.47(10) 2_656 2_656 ?
O7 Na1 O5 71.00(10) 2_656 2_656 ?
O3 Na1 O5 110.37(11) 1_455 2_656 ?
O7 Na1 Na1 52.92(9) . 2_656 ?
O4 Na1 Na1 90.37(10) . 2_656 ?
O2 Na1 Na1 128.37(11) 2_656 2_656 ?
O7 Na1 Na1 49.51(8) 2_656 2_656 ?
O3 Na1 Na1 140.63(11) 1_455 2_656 ?
O5 Na1 Na1 67.63(8) 2_656 2_656 ?
O7 Na1 C7 163.23(12) . 2_656 ?
O4 Na1 C7 95.23(11) . 2_656 ?
O2 Na1 C7 23.26(10) 2_656 2_656 ?
O7 Na1 C7 87.13(11) 2_656 2_656 ?
O3 Na1 C7 82.86(11) 1_455 2_656 ?
O5 Na1 C7 88.76(11) 2_656 2_656 ?
Na1 Na1 C7 134.80(11) 2_656 2_656 ?
O7 Na1 Na2 102.56(9) . 2_556 ?
O4 Na1 Na2 134.34(9) . 2_556 ?
O2 Na1 Na2 45.28(7) 2_656 2_556 ?
O7 Na1 Na2 130.68(9) 2_656 2_556 ?
O3 Na1 Na2 44.41(7) 1_455 2_556 ?
O5 Na1 Na2 71.54(8) 2_656 2_556 ?
Na1 Na1 Na2 134.56(9) 2_656 2_556 ?
C7 Na1 Na2 61.18(8) 2_656 2_556 ?
O7 Na1 Ni1 115.74(9) . 2_656 ?
O4 Na1 Ni1 139.53(9) . 2_656 ?
O2 Na1 Ni1 34.29(7) 2_656 2_656 ?
O7 Na1 Ni1 73.24(8) 2_656 2_656 ?
O3 Na1 Ni1 101.87(8) 1_455 2_656 ?
O5 Na1 Ni1 35.28(6) 2_656 2_656 ?
Na1 Na1 Ni1 95.89(7) 2_656 2_656 ?
C7 Na1 Ni1 53.48(8) 2_656 2_656 ?
Na2 Na1 Ni1 57.66(4) 2_556 2_656 ?
O4 Na2 O8 132.38(16) . . ?
O4 Na2 O3 98.20(12) . 2_656 ?
O8 Na2 O3 105.76(14) . 2_656 ?
O4 Na2 O2 95.00(12) . 1_455 ?
O8 Na2 O2 126.84(14) . 1_455 ?
O3 Na2 O2 85.66(11) 2_656 1_455 ?
O4 Na2 O1 111.82(11) . 1_455 ?
O8 Na2 O1 66.33(12) . 1_455 ?
O3 Na2 O1 145.42(12) 2_656 1_455 ?
O2 Na2 O1 75.33(10) 1_455 1_455 ?
O4 Na2 Ni1 114.50(9) . 1_455 ?
O8 Na2 Ni1 92.91(11) . 1_455 ?
O3 Na2 Ni1 113.34(9) 2_656 1_455 ?
O2 Na2 Ni1 38.07(7) 1_455 1_455 ?
O1 Na2 Ni1 38.68(7) 1_455 1_455 ?
O4 Na2 Na1 123.03(10) . 2_556 ?
O8 Na2 Na1 103.49(13) . 2_556 ?
O3 Na2 Na1 48.94(8) 2_656 2_556 ?
O2 Na2 Na1 47.01(8) 1_455 2_556 ?
O1 Na2 Na1 98.50(8) 1_455 2_556 ?
Ni1 Na2 Na1 64.64(4) 1_455 2_556 ?
O4 Na2 H5 131.1(17) . . ?
O8 Na2 H5 21.2(6) . . ?
O3 Na2 H5 122.9(12) 2_656 . ?
O2 Na2 H5 111.9(12) 1_455 . ?
O1 Na2 H5 45.2(6) 1_455 . ?
Ni1 Na2 H5 74.9(11) 1_455 . ?
Na1 Na2 H5 104.7(17) 2_556 . ?
C10 O1 Ni1 118.4(3) . . ?
C10 O1 Na2 136.5(2) . 1_655 ?
Ni1 O1 Na2 90.33(11) . 1_655 ?
C7 O2 Ni1 126.9(2) . . ?
C7 O2 Na2 124.6(2) . 1_655 ?
Ni1 O2 Na2 97.01(11) . 1_655 ?
C7 O2 Na1 108.5(2) . 2_656 ?
Ni1 O2 Na1 104.10(12) . 2_656 ?
Na2 O2 Na1 87.71(10) 1_655 2_656 ?
C7 O3 Na2 151.2(3) . 2_656 ?
C7 O3 Na1 112.0(3) . 1_655 ?
Na2 O3 Na1 86.65(11) 2_656 1_655 ?
C19 O4 Na2 146.1(3) . . ?
C19 O4 Na1 112.7(3) . . ?
Na2 O4 Na1 99.10(12) . . ?
C19 O5 Ni1 123.7(2) . . ?
C19 O5 Na1 135.9(2) . 2_656 ?
Ni1 O5 Na1 99.92(11) . 2_656 ?
C28 O6 Ni1 120.4(2) . . ?
C72 O7 Na1 123.2(3) . . ?
C72 O7 Na1 123.4(3) . 2_656 ?
Na1 O7 Na1 77.58(10) . 2_656 ?
C72 O7 H4 107(3) . . ?
Na1 O7 H4 114(3) . . ?
Na1 O7 H4 109(3) 2_656 . ?
C73 O8 Na2 163.4(4) . . ?
C73 O8 H5 115(5) . . ?
Na2 O8 H5 80(5) . . ?
C8 N1 C4 118.8(4) . . ?
C8 N1 Ni1 123.4(3) . . ?
C4 N1 Ni1 117.8(3) . . ?
C26 N2 C25 120.0(3) . . ?
C26 N2 Ni1 123.6(3) . . ?
C25 N2 Ni1 116.4(2) . . ?
C2 C1 C6 121.0(4) . . ?
C2 C1 Cl1 120.2(4) . . ?
C6 C1 Cl1 118.7(4) . . ?
C1 C2 C3 119.0(4) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C2 C3 C4 121.7(4) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C3 C4 C5 119.0(4) . . ?
C3 C4 N1 121.0(4) . . ?
C5 C4 N1 119.9(4) . . ?
C6 C5 C4 118.7(4) . . ?
C6 C5 C7 115.9(4) . . ?
C4 C5 C7 125.3(4) . . ?
C1 C6 C5 120.5(4) . . ?
C1 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
O3 C7 O2 122.4(4) . . ?
O3 C7 C5 118.0(4) . . ?
O2 C7 C5 119.6(3) . . ?
O3 C7 Na1 81.8(2) . 2_656 ?
O2 C7 Na1 48.20(18) . 2_656 ?
C5 C7 Na1 148.0(3) . 2_656 ?
N1 C8 C9 125.5(4) . . ?
N1 C8 H8 117.3 . . ?
C9 C8 H8 117.3 . . ?
C10 C9 C8 120.2(4) . . ?
C10 C9 C18 120.1(4) . . ?
C8 C9 C18 119.1(4) . . ?
O1 C10 C9 124.6(4) . . ?
O1 C10 C11 118.0(4) . . ?
C9 C10 C11 117.4(4) . . ?
C12 C11 C10 121.6(5) . . ?
C12 C11 H11 119.2 . . ?
C10 C11 H11 119.2 . . ?
C11 C12 C13 122.1(5) . . ?
C11 C12 H12 119.0 . . ?
C13 C12 H12 119.0 . . ?
C18 C13 C14 120.5(6) . . ?
C18 C13 C12 118.0(5) . . ?
C14 C13 C12 121.5(6) . . ?
C15 C14 C13 121.3(7) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C14 C15 C16 119.2(6) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
C17 C16 C15 119.0(7) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
C16 C17 C18 125.3(7) . . ?
C16 C17 H17 117.4 . . ?
C18 C17 H17 117.4 . . ?
C13 C18 C17 114.7(5) . . ?
C13 C18 C9 120.9(5) . . ?
C17 C18 C9 124.4(5) . . ?
O4 C19 O5 124.1(4) . . ?
O4 C19 C20 117.1(4) . . ?
O5 C19 C20 118.8(3) . . ?
C21 C20 C25 119.1(4) . . ?
C21 C20 C19 119.2(4) . . ?
C25 C20 C19 121.7(3) . . ?
C22 C21 C20 119.9(4) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C23 C22 C21 121.6(4) . . ?
C23 C22 Cl2 119.3(3) . . ?
C21 C22 Cl2 119.1(3) . . ?
C22 C23 C24 119.1(4) . . ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 . . ?
C23 C24 C25 120.9(4) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C24 C25 C20 119.4(4) . . ?
C24 C25 N2 122.8(4) . . ?
C20 C25 N2 117.7(3) . . ?
N2 C26 C27 125.3(4) . . ?
N2 C26 H26 117.4 . . ?
C27 C26 H26 117.4 . . ?
C26 C27 C28 120.2(3) . . ?
C26 C27 C36 119.7(4) . . ?
C28 C27 C36 119.4(4) . . ?
O6 C28 C27 124.0(4) . . ?
O6 C28 C29 117.5(4) . . ?
C27 C28 C29 118.5(4) . . ?
C30 C29 C28 121.8(4) . . ?
C30 C29 H29 119.1 . . ?
C28 C29 H29 119.1 . . ?
C29 C30 C31 121.8(4) . . ?
C29 C30 H30 119.1 . . ?
C31 C30 H30 119.1 . . ?
C32 C31 C30 121.9(4) . . ?
C32 C31 C36 119.3(4) . . ?
C30 C31 C36 118.8(4) . . ?
C33 C32 C31 121.0(5) . . ?
C33 C32 H32 119.5 . . ?
C31 C32 H32 119.5 . . ?
C32 C33 C34 120.2(4) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
C35 C34 C33 120.8(5) . . ?
C35 C34 H34 119.6 . . ?
C33 C34 H34 119.6 . . ?
C34 C35 C36 120.9(5) . . ?
C34 C35 H35 119.6 . . ?
C36 C35 H35 119.6 . . ?
C31 C36 C35 117.8(4) . . ?
C31 C36 C27 119.7(4) . . ?
C35 C36 C27 122.5(4) . . ?
O7 C72 H72A 109.5 . . ?
O7 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
O7 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
O8 C73 H73A 109.5 . . ?
O8 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
O8 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
N4 Ni2 O12 95.87(12) . . ?
N4 Ni2 N3 97.82(13) . . ?
O12 Ni2 N3 84.83(12) . . ?
N4 Ni2 O10 171.52(12) . . ?
O12 Ni2 O10 92.19(11) . . ?
N3 Ni2 O10 85.49(12) . . ?
N4 Ni2 O11 86.77(12) . . ?
O12 Ni2 O11 86.73(12) . . ?
N3 Ni2 O11 170.76(13) . . ?
O10 Ni2 O11 91.09(11) . . ?
N4 Ni2 O19 84.50(12) . . ?
O12 Ni2 O19 179.05(11) . . ?
N3 Ni2 O19 95.99(12) . . ?
O10 Ni2 O19 87.39(11) . . ?
O11 Ni2 O19 92.42(11) . . ?
N4 Ni2 Na3A 137.72(12) . 2_667 ?
O12 Ni2 Na3A 80.55(11) . 2_667 ?
N3 Ni2 Na3A 123.44(12) . 2_667 ?
O10 Ni2 Na3A 41.42(11) . 2_667 ?
O11 Ni2 Na3A 51.08(12) . 2_667 ?
O19 Ni2 Na3A 98.58(10) . 2_667 ?
N4 Ni2 Na3B 125.93(11) . 2_667 ?
O12 Ni2 Na3B 82.74(10) . 2_667 ?
N3 Ni2 Na3B 135.41(12) . 2_667 ?
O10 Ni2 Na3B 52.56(11) . 2_667 ?
O11 Ni2 Na3B 39.17(11) . 2_667 ?
O19 Ni2 Na3B 96.34(10) . 2_667 ?
C37 O10 Ni2 122.9(3) . . ?
C37 O10 Na3A 130.4(3) . 2_667 ?
Ni2 O10 Na3A 102.57(16) . 2_667 ?
C37 O10 Na4A 96.8(3) . . ?
Ni2 O10 Na4A 130.71(14) . . ?
Na3A O10 Na4A 61.07(15) 2_667 . ?
C37 O10 Na3B 136.7(3) . 2_667 ?
Ni2 O10 Na3B 92.28(13) . 2_667 ?
C55 O11 Ni2 125.8(3) . . ?
C55 O11 Na3B 116.3(3) . 2_667 ?
Ni2 O11 Na3B 107.35(17) . 2_667 ?
C55 O11 Na3A 127.7(3) . 2_667 ?
Ni2 O11 Na3A 91.78(15) . 2_667 ?
C55 O11 Na4B 80.8(3) . 1_455 ?
Ni2 O11 Na4B 138.29(15) . 1_455 ?
Na3B O11 Na4B 81.17(15) 2_667 1_455 ?
C46 O12 Ni2 120.8(2) . . ?
C55 O13 Na4B 90.4(3) . 1_455 ?
C74 O14 Na3A 132.1(4) . 2_667 ?
C74 O14 Na4A 134.8(4) . . ?
Na3A O14 Na4A 66.29(17) 2_667 . ?
C74 O14 Na4B 104.5(3) . . ?
C74 O14 Na3B 118.7(4) . 2_667 ?
Na4B O14 Na3B 109.45(17) . 2_667 ?
C74 O14 H1 109(4) . . ?
Na3A O14 H1 103(4) 2_667 . ?
Na4A O14 H1 103(4) . . ?
Na4B O14 H1 112(4) . . ?
Na3B O14 H1 103(4) 2_667 . ?
C75 O18 Na3B 144.6(6) . . ?
C75 O18 Na3A 136.9(6) . . ?
C75 O18 H7 113(7) . . ?
Na3B O18 H7 90(7) . . ?
Na3A O18 H7 95(7) . . ?
C71 O19 Ni2 119.6(2) . . ?
C44 N3 C43 119.8(3) . . ?
C44 N3 Ni2 123.3(3) . . ?
C43 N3 Ni2 116.8(2) . . ?
C5RH N4 C61 119.4(3) . . ?
C5RH N4 Ni2 123.6(3) . . ?
C61 N4 Ni2 117.1(2) . . ?
O10 C37 O9B 122.6(4) . . ?
O10 C37 O9A 113.4(5) . . ?
O10 C37 C38 123.1(4) . . ?
O9B C37 C38 109.3(5) . . ?
O9A C37 C38 118.0(4) . . ?
O10 C37 Na4A 94.7(3) . 2_667 ?
O9A C37 Na4A 54.7(3) . 2_667 ?
C38 C37 Na4A 134.5(4) . 2_667 ?
C39 C38 C43 118.0(4) . . ?
C39 C38 C37 117.3(4) . . ?
C43 C38 C37 124.6(4) . . ?
C40 C39 C38 121.7(4) . . ?
C40 C39 H39 119.1 . . ?
C38 C39 H39 119.1 . . ?
C39 C40 C41 121.3(4) . . ?
C39 C40 Cl3 120.2(4) . . ?
C41 C40 Cl3 118.5(4) . . ?
C42 C41 C40 117.9(4) . . ?
C42 C41 H41 121.0 . . ?
C40 C41 H41 121.0 . . ?
C41 C42 C43 121.6(4) . . ?
C41 C42 H42 119.2 . . ?
C43 C42 H42 119.2 . . ?
C42 C43 C38 119.4(4) . . ?
C42 C43 N3 121.7(3) . . ?
C38 C43 N3 118.7(4) . . ?
N3 C44 C45 125.0(4) . . ?
N3 C44 H44 117.5 . . ?
C45 C44 H44 117.5 . . ?
C46 C45 C44 120.0(3) . . ?
C46 C45 C50 119.6(4) . . ?
C44 C45 C50 119.7(4) . . ?
O12 C46 C45 123.5(4) . . ?
O12 C46 C47 117.7(4) . . ?
C45 C46 C47 118.8(4) . . ?
C48 C47 C46 121.6(4) . . ?
C48 C47 H47 119.2 . . ?
C46 C47 H47 119.2 . . ?
C47 C48 C49 121.4(4) . . ?
C47 C48 H48 119.3 . . ?
C49 C48 H48 119.3 . . ?
C54 C49 C50 119.7(4) . . ?
C54 C49 C48 121.0(4) . . ?
C50 C49 C48 119.2(4) . . ?
C51 C50 C49 117.5(4) . . ?
C51 C50 C45 123.1(4) . . ?
C49 C50 C45 119.4(4) . . ?
C52 C51 C50 121.4(4) . . ?
C52 C51 H51 119.3 . . ?
C50 C51 H51 119.3 . . ?
C51 C52 C53 120.5(4) . . ?
C51 C52 H52 119.8 . . ?
C53 C52 H52 119.8 . . ?
C54 C53 C52 119.8(4) . . ?
C54 C53 H53 120.1 . . ?
C52 C53 H53 120.1 . . ?
C53 C54 C49 121.0(4) . . ?
C53 C54 H54 119.5 . . ?
C49 C54 H54 119.5 . . ?
O13 C55 O11 122.9(4) . . ?
O13 C55 C56 115.9(4) . . ?
O11 C55 C56 121.1(4) . . ?
O13 C55 Na4B 64.8(3) . 1_455 ?
O11 C55 Na4B 74.2(3) . 1_455 ?
C56 C55 Na4B 137.8(3) . 1_455 ?
O13 C55 Na3B 85.2(3) . 2_667 ?
O11 C55 Na3B 42.3(2) . 2_667 ?
C56 C55 Na3B 150.5(3) . 2_667 ?
Na4B C55 Na3B 68.58(14) 1_455 2_667 ?
C57 C56 C61 118.7(4) . . ?
C57 C56 C55 116.3(4) . . ?
C61 C56 C55 125.0(4) . . ?
C58 C57 C56 120.0(4) . . ?
C58 C57 H57 120.0 . . ?
C56 C57 H57 120.0 . . ?
C57 C58 C59 121.8(4) . . ?
C57 C58 Cl4 119.1(4) . . ?
C59 C58 Cl4 119.1(3) . . ?
C60 C59 C58 118.6(4) . . ?
C60 C59 H59 120.7 . . ?
C58 C59 H59 120.7 . . ?
C59 C60 C61 121.2(4) . . ?
C59 C60 H60 119.4 . . ?
C61 C60 H60 119.4 . . ?
C60 C61 C56 119.7(4) . . ?
C60 C61 N4 120.4(3) . . ?
C56 C61 N4 119.9(3) . . ?
C71 C62 C5RH 120.3(3) . . ?
C71 C62 C64 119.4(4) . . ?
C5RH C62 C64 119.4(3) . . ?
C65 C63 C64 121.3(4) . . ?
C65 C63 H63 119.3 . . ?
C64 C63 H63 119.3 . . ?
C68 C64 C63 117.3(4) . . ?
C68 C64 C62 120.1(4) . . ?
C63 C64 C62 122.5(4) . . ?
C63 C65 C66 120.8(4) . . ?
C63 C65 H65 119.6 . . ?
C66 C65 H65 119.6 . . ?
C67 C66 C65 119.5(4) . . ?
C67 C66 H66 120.3 . . ?
C65 C66 H66 120.3 . . ?
C66 C67 C68 121.0(4) . . ?
C66 C67 H67 119.5 . . ?
C68 C67 H67 119.5 . . ?
C64 C68 C67 119.9(4) . . ?
C64 C68 C69 118.7(4) . . ?
C67 C68 C69 121.3(4) . . ?
C70 C69 C68 120.7(4) . . ?
C70 C69 H69 119.7 . . ?
C68 C69 H69 119.7 . . ?
C69 C70 C71 122.5(4) . . ?
C69 C70 H70 118.8 . . ?
C71 C70 H70 118.8 . . ?
O19 C71 C62 123.1(4) . . ?
O19 C71 C70 118.3(3) . . ?
C62 C71 C70 118.6(4) . . ?
O14 C74 H74A 109.5 . . ?
O14 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
O14 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
O18 C75 H75A 109.5 . . ?
O18 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
O18 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
N4 C5RH C62 124.5(4) . . ?
N4 C5RH H5RH 117.7 . . ?
C62 C5RH H5RH 117.7 . . ?
O9A Na3A O14 104.8(3) . 2_667 ?
O9A Na3A O10 106.8(3) . 2_667 ?
O14 Na3A O10 88.60(19) 2_667 2_667 ?
O9A Na3A Na4A 63.5(2) . 2_667 ?
O14 Na3A Na4A 57.97(16) 2_667 2_667 ?
O10 Na3A Na4A 65.92(16) 2_667 2_667 ?
O9A Na3A O11 169.7(3) . 2_667 ?
O14 Na3A O11 85.51(17) 2_667 2_667 ?
O10 Na3A O11 72.14(14) 2_667 2_667 ?
Na4A Na3A O11 123.36(19) 2_667 2_667 ?
O9A Na3A O18 105.4(3) . . ?
O14 Na3A O18 90.1(2) 2_667 . ?
O10 Na3A O18 146.9(2) 2_667 . ?
Na4A Na3A O18 137.8(2) 2_667 . ?
O11 Na3A O18 74.82(17) 2_667 . ?
O9A Na3A Ni2 142.8(3) . 2_667 ?
O14 Na3A Ni2 79.85(14) 2_667 2_667 ?
O10 Na3A Ni2 36.02(9) 2_667 2_667 ?
Na4A Na3A Ni2 90.78(14) 2_667 2_667 ?
O11 Na3A Ni2 37.14(8) 2_667 2_667 ?
O18 Na3A Ni2 111.45(17) . 2_667 ?
O20 Na4A O14 85.5(2) . . ?
O20 Na4A O9A 159.0(3) . 2_667 ?
O14 Na4A O9A 88.0(2) . 2_667 ?
O20 Na4A O15 109.9(3) . . ?
O14 Na4A O15 116.4(2) . . ?
O9A Na4A O15 90.9(2) 2_667 . ?
O20 Na4A Na3A 117.7(2) . 2_667 ?
O14 Na4A Na3A 55.74(16) . 2_667 ?
O9A Na4A Na3A 43.78(17) 2_667 2_667 ?
O15 Na4A Na3A 129.8(2) . 2_667 ?
O20 Na4A O9A 85.8(2) . . ?
O14 Na4A O9A 128.9(2) . . ?
O9A Na4A O9A 82.8(2) 2_667 . ?
O15 Na4A O9A 113.9(2) . . ?
Na3A Na4A O9A 85.18(19) 2_667 . ?
O20 Na4A O10 75.83(19) . . ?
O14 Na4A O10 79.92(14) . . ?
O9A Na4A O10 83.37(18) 2_667 . ?
O15 Na4A O10 162.6(2) . . ?
Na3A Na4A O10 53.01(13) 2_667 . ?
O9A Na4A O10 49.13(15) . . ?
O20 Na4A C37 168.1(2) . 2_667 ?
O14 Na4A C37 106.37(17) . 2_667 ?
O9A Na4A C37 27.60(18) 2_667 2_667 ?
O15 Na4A C37 64.4(2) . 2_667 ?
Na3A Na4A C37 71.18(16) 2_667 2_667 ?
O9A Na4A C37 87.2(2) . 2_667 ?
O10 Na4A C37 106.56(18) . 2_667 ?
O20 Na4A Na4A 122.9(2) . 2_667 ?
O14 Na4A Na4A 114.42(18) . 2_667 ?
O9A Na4A Na4A 43.60(16) 2_667 2_667 ?
O15 Na4A Na4A 106.9(2) . 2_667 ?
Na3A Na4A Na4A 58.79(14) 2_667 2_667 ?
O9A Na4A Na4A 39.17(15) . 2_667 ?
O10 Na4A Na4A 58.10(10) . 2_667 ?
C37 Na4A Na4A 53.24(15) 2_667 2_667 ?
O20 Na4A H1 69.8(10) . . ?
O14 Na4A H1 18.2(8) . . ?
O9A Na4A H1 99.8(12) 2_667 . ?
O15 Na4A H1 129.4(12) . . ?
Na3A Na4A H1 60.4(14) 2_667 . ?
O9A Na4A H1 116.5(11) . . ?
O10 Na4A H1 68.0(12) . . ?
C37 Na4A H1 122.1(10) 2_667 . ?
Na4A Na4A H1 114.7(14) 2_667 . ?
C37 O9A Na3A 167.4(6) . . ?
C37 O9A Na4A 97.7(4) . 2_667 ?
Na3A O9A Na4A 72.7(2) . 2_667 ?
C37 O9A Na4A 96.7(4) . . ?
Na3A O9A Na4A 92.7(3) . . ?
Na4A O9A Na4A 97.2(2) 2_667 . ?
Na3B O17 Na4B 92.4(2) . 2_767 ?
O18 Na3B O17 86.5(3) . . ?
O18 Na3B O11 95.3(2) . 2_667 ?
O17 Na3B O11 90.7(2) . 2_667 ?
O18 Na3B O14 100.5(2) . 2_667 ?
O17 Na3B O14 172.6(3) . 2_667 ?
O11 Na3B O14 86.26(16) 2_667 2_667 ?
O18 Na3B O10 162.2(2) . 2_667 ?
O17 Na3B O10 99.6(2) . 2_667 ?
O11 Na3B O10 68.20(14) 2_667 2_667 ?
O14 Na3B O10 72.92(15) 2_667 2_667 ?
O18 Na3B O9B 112.3(2) . . ?
O17 Na3B O9B 115.5(2) . . ?
O11 Na3B O9B 142.1(2) 2_667 . ?
O14 Na3B O9B 64.24(17) 2_667 . ?
O10 Na3B O9B 80.20(17) 2_667 . ?
O18 Na3B C55 75.0(2) . 2_667 ?
O17 Na3B C55 96.2(2) . 2_667 ?
O11 Na3B C55 21.37(11) 2_667 2_667 ?
O14 Na3B C55 83.38(16) 2_667 2_667 ?
O10 Na3B C55 87.68(14) 2_667 2_667 ?
O9B Na3B C55 147.5(2) . 2_667 ?
O18 Na3B Na4B 65.79(19) . 2_767 ?
O17 Na3B Na4B 44.60(18) . 2_767 ?
O11 Na3B Na4B 56.37(13) 2_667 2_767 ?
O14 Na3B Na4B 136.51(17) 2_667 2_767 ?
O10 Na3B Na4B 107.22(15) 2_667 2_767 ?
O9B Na3B Na4B 158.96(19) . 2_767 ?
C55 Na3B Na4B 53.56(12) 2_667 2_767 ?
O18 Na3B Ni2 127.5(2) . 2_667 ?
O17 Na3B Ni2 100.2(2) . 2_667 ?
O11 Na3B Ni2 33.48(9) 2_667 2_667 ?
O14 Na3B Ni2 73.62(12) 2_667 2_667 ?
O10 Na3B Ni2 35.16(7) 2_667 2_667 ?
O9B Na3B Ni2 111.08(18) . 2_667 ?
C55 Na3B Ni2 52.54(10) 2_667 2_667 ?
Na4B Na3B Ni2 83.06(10) 2_767 2_667 ?
O18 Na3B Na4B 119.4(2) . 2_667 ?
O17 Na3B Na4B 142.0(2) . 2_667 ?
O11 Na3B Na4B 111.99(16) 2_667 2_667 ?
O14 Na3B Na4B 35.16(11) 2_667 2_667 ?
O10 Na3B Na4B 64.51(11) 2_667 2_667 ?
O9B Na3B Na4B 31.76(13) . 2_667 ?
C55 Na3B Na4B 116.17(15) 2_667 2_667 ?
Na4B Na3B Na4B 168.33(16) 2_767 2_667 ?
Ni2 Na3B Na4B 85.80(10) 2_667 2_667 ?
O18 Na3B H7 22(2) . . ?
O17 Na3B H7 90(2) . . ?
O11 Na3B H7 73(2) 2_667 . ?
O14 Na3B H7 96(2) 2_667 . ?
O10 Na3B H7 140(2) 2_667 . ?
O9B Na3B H7 130(3) . . ?
C55 Na3B H7 53(2) 2_667 . ?
Na4B Na3B H7 55(2) 2_767 . ?
Ni2 Na3B H7 105(2) 2_667 . ?
Na4B Na3B H7 125(2) 2_667 . ?
O9B Na4B O16 97.4(3) 2_667 . ?
O9B Na4B O17 90.7(2) 2_667 2_767 ?
O16 Na4B O17 84.2(3) . 2_767 ?
O9B Na4B O14 72.83(19) 2_667 . ?
O16 Na4B O14 97.7(3) . . ?
O17 Na4B O14 163.5(2) 2_767 . ?
O9B Na4B O13 142.8(2) 2_667 1_655 ?
O16 Na4B O13 117.0(3) . 1_655 ?
O17 Na4B O13 105.7(2) 2_767 1_655 ?
O14 Na4B O13 88.05(16) . 1_655 ?
O9B Na4B O11 167.5(2) 2_667 1_655 ?
O16 Na4B O11 78.3(2) . 1_655 ?
O17 Na4B O11 77.31(18) 2_767 1_655 ?
O14 Na4B O11 119.15(16) . 1_655 ?
O13 Na4B O11 46.49(11) 1_655 1_655 ?
O9B Na4B C55 166.6(2) 2_667 1_655 ?
O16 Na4B C55 92.9(3) . 1_655 ?
O17 Na4B C55 98.8(2) 2_767 1_655 ?
O14 Na4B C55 97.42(16) . 1_655 ?
O13 Na4B C55 24.81(11) 1_655 1_655 ?
O11 Na4B C55 24.99(11) 1_655 1_655 ?
O9B Na4B Na3B 128.3(2) 2_667 2_767 ?
O16 Na4B Na3B 98.5(2) . 2_767 ?
O17 Na4B Na3B 43.01(16) 2_767 2_767 ?
O14 Na4B Na3B 150.93(16) . 2_767 ?
O13 Na4B Na3B 63.08(14) 1_655 2_767 ?
O11 Na4B Na3B 42.46(10) 1_655 2_767 ?
C55 Na4B Na3B 57.86(13) 1_655 2_767 ?
O9B Na4B Na3B 40.59(17) 2_667 2_667 ?
O16 Na4B Na3B 87.8(2) . 2_667 ?
O17 Na4B Na3B 128.90(18) 2_767 2_667 ?
O14 Na4B Na3B 35.39(11) . 2_667 ?
O13 Na4B Na3B 122.58(16) 1_655 2_667 ?
O11 Na4B Na3B 149.17(13) 1_655 2_667 ?
C55 Na4B Na3B 131.99(15) 1_655 2_667 ?
Na3B Na4B Na3B 168.32(16) 2_767 2_667 ?
C37 O9B Na4B 135.6(5) . 2_667 ?
C37 O9B Na3B 113.6(4) . . ?
Na4B O9B Na3B 107.7(2) 2_667 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 1.0(7) . . . . ?
Cl1 C1 C2 C3 -179.7(4) . . . . ?
C1 C2 C3 C4 0.4(7) . . . . ?
C2 C3 C4 C5 -2.2(6) . . . . ?
C2 C3 C4 N1 179.8(4) . . . . ?
C8 N1 C4 C3 -44.5(6) . . . . ?
Ni1 N1 C4 C3 135.6(3) . . . . ?
C8 N1 C4 C5 137.5(4) . . . . ?
Ni1 N1 C4 C5 -42.4(5) . . . . ?
C3 C4 C5 C6 2.6(6) . . . . ?
N1 C4 C5 C6 -179.3(4) . . . . ?
C3 C4 C5 C7 -177.0(4) . . . . ?
N1 C4 C5 C7 1.0(6) . . . . ?
C2 C1 C6 C5 -0.6(7) . . . . ?
Cl1 C1 C6 C5 -179.8(3) . . . . ?
C4 C5 C6 C1 -1.3(6) . . . . ?
C7 C5 C6 C1 178.4(4) . . . . ?
Na2 O3 C7 O2 53.3(8) 2_656 . . . ?
Na1 O3 C7 O2 -73.9(4) 1_655 . . . ?
Na2 O3 C7 C5 -127.4(5) 2_656 . . . ?
Na1 O3 C7 C5 105.4(3) 1_655 . . . ?
Na2 O3 C7 Na1 26.0(5) 2_656 . . 2_656 ?
Na1 O3 C7 Na1 -101.17(16) 1_655 . . 2_656 ?
Ni1 O2 C7 O3 -162.5(3) . . . . ?
Na2 O2 C7 O3 62.9(5) 1_655 . . . ?
Na1 O2 C7 O3 -37.5(4) 2_656 . . . ?
Ni1 O2 C7 C5 18.3(5) . . . . ?
Na2 O2 C7 C5 -116.4(3) 1_655 . . . ?
Na1 O2 C7 C5 143.2(3) 2_656 . . . ?
Ni1 O2 C7 Na1 -125.0(3) . . . 2_656 ?
Na2 O2 C7 Na1 100.4(3) 1_655 . . 2_656 ?
C6 C5 C7 O3 14.0(5) . . . . ?
C4 C5 C7 O3 -166.3(4) . . . . ?
C6 C5 C7 O2 -166.7(4) . . . . ?
C4 C5 C7 O2 13.0(6) . . . . ?
C6 C5 C7 Na1 -109.1(5) . . . 2_656 ?
C4 C5 C7 Na1 70.5(7) . . . 2_656 ?
C4 N1 C8 C9 -175.4(4) . . . . ?
Ni1 N1 C8 C9 4.4(6) . . . . ?
N1 C8 C9 C10 26.0(6) . . . . ?
N1 C8 C9 C18 -162.6(4) . . . . ?
Ni1 O1 C10 C9 -35.8(5) . . . . ?
Na2 O1 C10 C9 89.5(5) 1_655 . . . ?
Ni1 O1 C10 C11 145.3(3) . . . . ?
Na2 O1 C10 C11 -89.3(5) 1_655 . . . ?
C8 C9 C10 O1 -7.5(6) . . . . ?
C18 C9 C10 O1 -178.8(4) . . . . ?
C8 C9 C10 C11 171.3(4) . . . . ?
C18 C9 C10 C11 0.0(6) . . . . ?
O1 C10 C11 C12 178.3(4) . . . . ?
C9 C10 C11 C12 -0.6(6) . . . . ?
C10 C11 C12 C13 0.2(7) . . . . ?
C11 C12 C13 C18 0.9(7) . . . . ?
C11 C12 C13 C14 -179.8(5) . . . . ?
C18 C13 C14 C15 0.5(8) . . . . ?
C12 C13 C14 C15 -178.8(5) . . . . ?
C13 C14 C15 C16 0.7(9) . . . . ?
C14 C15 C16 C17 -1.2(9) . . . . ?
C15 C16 C17 C18 0.3(9) . . . . ?
C14 C13 C18 C17 -1.3(7) . . . . ?
C12 C13 C18 C17 178.1(5) . . . . ?
C14 C13 C18 C9 179.2(5) . . . . ?
C12 C13 C18 C9 -1.4(7) . . . . ?
C16 C17 C18 C13 0.9(8) . . . . ?
C16 C17 C18 C9 -179.6(5) . . . . ?
C10 C9 C18 C13 1.0(6) . . . . ?
C8 C9 C18 C13 -170.4(4) . . . . ?
C10 C9 C18 C17 -178.4(4) . . . . ?
C8 C9 C18 C17 10.2(7) . . . . ?
Na2 O4 C19 O5 -169.5(3) . . . . ?
Na1 O4 C19 O5 -11.0(5) . . . . ?
Na2 O4 C19 C20 11.8(7) . . . . ?
Na1 O4 C19 C20 170.3(3) . . . . ?
Ni1 O5 C19 O4 149.8(3) . . . . ?
Na1 O5 C19 O4 -20.6(6) 2_656 . . . ?
Ni1 O5 C19 C20 -31.5(5) . . . . ?
Na1 O5 C19 C20 158.1(3) 2_656 . . . ?
O4 C19 C20 C21 45.2(5) . . . . ?
O5 C19 C20 C21 -133.6(4) . . . . ?
O4 C19 C20 C25 -132.7(4) . . . . ?
O5 C19 C20 C25 48.5(5) . . . . ?
C25 C20 C21 C22 -2.2(6) . . . . ?
C19 C20 C21 C22 179.8(4) . . . . ?
C20 C21 C22 C23 3.2(6) . . . . ?
C20 C21 C22 Cl2 -177.2(3) . . . . ?
C21 C22 C23 C24 -1.8(7) . . . . ?
Cl2 C22 C23 C24 178.7(3) . . . . ?
C22 C23 C24 C25 -0.7(6) . . . . ?
C23 C24 C25 C20 1.6(6) . . . . ?
C23 C24 C25 N2 -177.3(4) . . . . ?
C21 C20 C25 C24 -0.2(6) . . . . ?
C19 C20 C25 C24 177.7(4) . . . . ?
C21 C20 C25 N2 178.9(4) . . . . ?
C19 C20 C25 N2 -3.2(6) . . . . ?
C26 N2 C25 C24 -50.9(5) . . . . ?
Ni1 N2 C25 C24 129.9(3) . . . . ?
C26 N2 C25 C20 130.1(4) . . . . ?
Ni1 N2 C25 C20 -49.1(4) . . . . ?
C25 N2 C26 C27 -169.3(4) . . . . ?
Ni1 N2 C26 C27 9.9(6) . . . . ?
N2 C26 C27 C28 21.7(6) . . . . ?
N2 C26 C27 C36 -168.4(4) . . . . ?
Ni1 O6 C28 C27 -34.0(5) . . . . ?
Ni1 O6 C28 C29 147.5(3) . . . . ?
C26 C27 C28 O6 -8.0(6) . . . . ?
C36 C27 C28 O6 -178.0(4) . . . . ?
C26 C27 C28 C29 170.4(4) . . . . ?
C36 C27 C28 C29 0.5(6) . . . . ?
O6 C28 C29 C30 178.4(4) . . . . ?
C27 C28 C29 C30 -0.1(6) . . . . ?
C28 C29 C30 C31 -0.7(7) . . . . ?
C29 C30 C31 C32 -178.0(4) . . . . ?
C29 C30 C31 C36 1.1(7) . . . . ?
C30 C31 C32 C33 179.6(4) . . . . ?
C36 C31 C32 C33 0.5(7) . . . . ?
C31 C32 C33 C34 0.2(7) . . . . ?
C32 C33 C34 C35 0.6(7) . . . . ?
C33 C34 C35 C36 -2.1(7) . . . . ?
C32 C31 C36 C35 -1.9(6) . . . . ?
C30 C31 C36 C35 179.0(4) . . . . ?
C32 C31 C36 C27 178.4(4) . . . . ?
C30 C31 C36 C27 -0.7(6) . . . . ?
C34 C35 C36 C31 2.8(6) . . . . ?
C34 C35 C36 C27 -177.6(4) . . . . ?
C26 C27 C36 C31 -170.0(4) . . . . ?
C28 C27 C36 C31 -0.1(6) . . . . ?
C26 C27 C36 C35 10.3(6) . . . . ?
C28 C27 C36 C35 -179.7(4) . . . . ?
Ni2 O10 C37 O9B 137.1(5) . . . . ?
Na3B O10 C37 O9B -2.1(9) 2_667 . . . ?
Ni2 O10 C37 O9A -168.6(4) . . . . ?
Na3A O10 C37 O9A 38.2(7) 2_667 . . . ?
Na4A O10 C37 O9A -19.2(5) . . . . ?
Ni2 O10 C37 C38 -15.3(7) . . . . ?
Na3A O10 C37 C38 -168.5(4) 2_667 . . . ?
Na4A O10 C37 C38 134.1(5) . . . . ?
Na3B O10 C37 C38 -154.4(3) 2_667 . . . ?
Ni2 O10 C37 Na4A 138.0(2) . . . 2_667 ?
Na3A O10 C37 Na4A -15.2(5) 2_667 . . 2_667 ?
Na4A O10 C37 Na4A -72.7(2) . . . 2_667 ?
O10 C37 C38 C39 161.4(5) . . . . ?
O9B C37 C38 C39 5.9(7) . . . . ?
O9A C37 C38 C39 -46.4(8) . . . . ?
Na4A C37 C38 C39 20.4(7) 2_667 . . . ?
O10 C37 C38 C43 -18.8(8) . . . . ?
O9B C37 C38 C43 -174.3(5) . . . . ?
O9A C37 C38 C43 133.4(5) . . . . ?
Na4A C37 C38 C43 -159.8(4) 2_667 . . . ?
C43 C38 C39 C40 0.7(7) . . . . ?
C37 C38 C39 C40 -179.4(5) . . . . ?
C38 C39 C40 C41 -0.8(8) . . . . ?
C38 C39 C40 Cl3 178.6(4) . . . . ?
C39 C40 C41 C42 0.2(7) . . . . ?
Cl3 C40 C41 C42 -179.2(3) . . . . ?
C40 C41 C42 C43 0.5(6) . . . . ?
C41 C42 C43 C38 -0.6(6) . . . . ?
C41 C42 C43 N3 175.9(4) . . . . ?
C39 C38 C43 C42 0.0(6) . . . . ?
C37 C38 C43 C42 -179.8(4) . . . . ?
C39 C38 C43 N3 -176.6(4) . . . . ?
C37 C38 C43 N3 3.6(6) . . . . ?
C44 N3 C43 C42 42.7(5) . . . . ?
Ni2 N3 C43 C42 -135.7(3) . . . . ?
C44 N3 C43 C38 -140.8(4) . . . . ?
Ni2 N3 C43 C38 40.8(4) . . . . ?
C43 N3 C44 C45 174.7(4) . . . . ?
Ni2 N3 C44 C45 -6.9(5) . . . . ?
N3 C44 C45 C46 -24.4(6) . . . . ?
N3 C44 C45 C50 165.4(4) . . . . ?
Ni2 O12 C46 C45 35.4(5) . . . . ?
Ni2 O12 C46 C47 -147.1(3) . . . . ?
C44 C45 C46 O12 8.6(6) . . . . ?
C50 C45 C46 O12 178.8(4) . . . . ?
C44 C45 C46 C47 -168.9(4) . . . . ?
C50 C45 C46 C47 1.4(6) . . . . ?
O12 C46 C47 C48 -179.0(4) . . . . ?
C45 C46 C47 C48 -1.4(6) . . . . ?
C46 C47 C48 C49 0.6(7) . . . . ?
C47 C48 C49 C54 177.4(4) . . . . ?
C47 C48 C49 C50 0.3(6) . . . . ?
C54 C49 C50 C51 2.5(6) . . . . ?
C48 C49 C50 C51 179.7(4) . . . . ?
C54 C49 C50 C45 -177.5(4) . . . . ?
C48 C49 C50 C45 -0.4(6) . . . . ?
C46 C45 C50 C51 179.5(4) . . . . ?
C44 C45 C50 C51 -10.3(6) . . . . ?
C46 C45 C50 C49 -0.5(6) . . . . ?
C44 C45 C50 C49 169.8(3) . . . . ?
C49 C50 C51 C52 -4.4(6) . . . . ?
C45 C50 C51 C52 175.6(4) . . . . ?
C50 C51 C52 C53 3.1(6) . . . . ?
C51 C52 C53 C54 0.2(6) . . . . ?
C52 C53 C54 C49 -2.1(6) . . . . ?
C50 C49 C54 C53 0.6(6) . . . . ?
C48 C49 C54 C53 -176.5(4) . . . . ?
Na4B O13 C55 O11 48.5(5) 1_455 . . . ?
Na4B O13 C55 C56 -133.0(4) 1_455 . . . ?
Na4B O13 C55 Na3B 68.57(16) 1_455 . . 2_667 ?
Ni2 O11 C55 O13 170.7(4) . . . . ?
Na3B O11 C55 O13 30.6(7) 2_667 . . . ?
Na3A O11 C55 O13 43.4(7) 2_667 . . . ?
Na4B O11 C55 O13 -44.7(5) 1_455 . . . ?
Ni2 O11 C55 C56 -7.9(6) . . . . ?
Na3B O11 C55 C56 -147.9(3) 2_667 . . . ?
Na3A O11 C55 C56 -135.1(4) 2_667 . . . ?
Na4B O11 C55 C56 136.8(4) 1_455 . . . ?
Ni2 O11 C55 Na4B -144.6(3) . . . 1_455 ?
Na3B O11 C55 Na4B 75.3(2) 2_667 . . 1_455 ?
Ni2 O11 C55 Na3B 140.1(4) . . . 2_667 ?
Na4B O11 C55 Na3B -75.3(2) 1_455 . . 2_667 ?
O13 C55 C56 C57 -16.9(7) . . . . ?
O11 C55 C56 C57 161.7(4) . . . . ?
Na4B C55 C56 C57 -97.1(5) 1_455 . . . ?
Na3B C55 C56 C57 115.1(6) 2_667 . . . ?
O13 C55 C56 C61 162.2(5) . . . . ?
O11 C55 C56 C61 -19.2(7) . . . . ?
Na4B C55 C56 C61 82.0(6) 1_455 . . . ?
Na3B C55 C56 C61 -65.8(8) 2_667 . . . ?
C61 C56 C57 C58 2.3(6) . . . . ?
C55 C56 C57 C58 -178.5(4) . . . . ?
C56 C57 C58 C59 0.3(7) . . . . ?
C56 C57 C58 Cl4 -178.9(3) . . . . ?
C57 C58 C59 C60 -2.0(7) . . . . ?
Cl4 C58 C59 C60 177.2(3) . . . . ?
C58 C59 C60 C61 1.0(6) . . . . ?
C59 C60 C61 C56 1.6(6) . . . . ?
C59 C60 C61 N4 -179.9(4) . . . . ?
C57 C56 C61 C60 -3.3(6) . . . . ?
C55 C56 C61 C60 177.7(4) . . . . ?
C57 C56 C61 N4 178.2(4) . . . . ?
C55 C56 C61 N4 -0.9(6) . . . . ?
C5RH N4 C61 C60 44.5(5) . . . . ?
Ni2 N4 C61 C60 -135.4(3) . . . . ?
C5RH N4 C61 C56 -136.9(4) . . . . ?
Ni2 N4 C61 C56 43.1(4) . . . . ?
C65 C63 C64 C68 -4.5(6) . . . . ?
C65 C63 C64 C62 176.2(4) . . . . ?
C71 C62 C64 C68 -1.2(6) . . . . ?
C5RH C62 C64 C68 168.1(4) . . . . ?
C71 C62 C64 C63 178.1(4) . . . . ?
C5RH C62 C64 C63 -12.6(6) . . . . ?
C64 C63 C65 C66 2.9(6) . . . . ?
C63 C65 C66 C67 0.2(7) . . . . ?
C65 C66 C67 C68 -1.4(7) . . . . ?
C63 C64 C68 C67 3.2(6) . . . . ?
C62 C64 C68 C67 -177.5(4) . . . . ?
C63 C64 C68 C69 -179.0(4) . . . . ?
C62 C64 C68 C69 0.4(6) . . . . ?
C66 C67 C68 C64 -0.3(6) . . . . ?
C66 C67 C68 C69 -178.1(4) . . . . ?
C64 C68 C69 C70 0.5(6) . . . . ?
C67 C68 C69 C70 178.3(4) . . . . ?
C68 C69 C70 C71 -0.6(7) . . . . ?
Ni2 O19 C71 C62 35.4(5) . . . . ?
Ni2 O19 C71 C70 -146.6(3) . . . . ?
C5RH C62 C71 O19 10.0(6) . . . . ?
C64 C62 C71 O19 179.2(3) . . . . ?
C5RH C62 C71 C70 -168.0(4) . . . . ?
C64 C62 C71 C70 1.2(6) . . . . ?
C69 C70 C71 O19 -178.4(4) . . . . ?
C69 C70 C71 C62 -0.3(6) . . . . ?
C61 N4 C5RH C62 173.0(3) . . . . ?
Ni2 N4 C5RH C62 -7.1(5) . . . . ?
C71 C62 C5RH N4 -26.5(6) . . . . ?
C64 C62 C5RH N4 164.3(4) . . . . ?
O10 C37 O9A Na3A -118(2) . . . . ?
C38 C37 O9A Na3A 87(2) . . . . ?
Na4A C37 O9A Na3A -39(2) 2_667 . . . ?
O10 C37 O9A Na4A -78.6(5) . . . 2_667 ?
C38 C37 O9A Na4A 126.6(5) . . . 2_667 ?
O10 C37 O9A Na4A 19.6(5) . . . . ?
C38 C37 O9A Na4A -135.2(4) . . . . ?
Na4A C37 O9A Na4A 98.3(3) 2_667 . . . ?
O14 Na3A O9A C37 -1(2) 2_667 . . . ?
O10 Na3A O9A C37 92(2) 2_667 . . . ?
Na4A Na3A O9A C37 41(2) 2_667 . . . ?
O11 Na3A O9A C37 175.1(15) 2_667 . . . ?
O18 Na3A O9A C37 -95(2) . . . . ?
Ni2 Na3A O9A C37 92(2) 2_667 . . . ?
O14 Na3A O9A Na4A -41.9(2) 2_667 . . 2_667 ?
O10 Na3A O9A Na4A 51.2(2) 2_667 . . 2_667 ?
O11 Na3A O9A Na4A 133.8(17) 2_667 . . 2_667 ?
O18 Na3A O9A Na4A -136.1(2) . . . 2_667 ?
Ni2 Na3A O9A Na4A 50.8(4) 2_667 . . 2_667 ?
O14 Na3A O9A Na4A -138.6(2) 2_667 . . . ?
O10 Na3A O9A Na4A -45.6(3) 2_667 . . . ?
Na4A Na3A O9A Na4A -96.7(2) 2_667 . . . ?
O11 Na3A O9A Na4A 37.1(18) 2_667 . . . ?
O18 Na3A O9A Na4A 127.1(2) . . . . ?
Ni2 Na3A O9A Na4A -45.9(5) 2_667 . . . ?
O10 C37 O9B Na4B -49.3(10) . . . 2_667 ?
C38 C37 O9B Na4B 106.4(6) . . . 2_667 ?
O10 C37 O9B Na3B 107.2(6) . . . . ?
C38 C37 O9B Na3B -97.1(5) . . . . ?

_refine_diff_density_max         0.745
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.080

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
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data_comp_6
_database_code_depnum_ccdc_archive 'CCDC 1448725'
_audit_update_record             
;
2016-01-20 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C116 H96 Cl10 N6 Ni6 O27.29'
_chemical_formula_weight         2717.42

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 'Calculated using XDISP in WinGX (Farrugia, 1999)'
H H 0.0000 0.0000 'Calculated using XDISP in WinGX (Farrugia, 1999)'
N N 0.0076 0.0040 'Calculated using XDISP in WinGX (Farrugia, 1999)'
O O 0.0132 0.0074 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Cl Cl 0.1697 0.1896 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Ni Ni 0.3262 1.3024 'Calculated using XDISP in WinGX (Farrugia, 1999)'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

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

_cell_length_a                   27.5171(11)
_cell_length_b                   27.7084(10)
_cell_length_c                   31.0222(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     23653.0(16)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9637
_cell_measurement_theta_min      2.2955
_cell_measurement_theta_max      24.099

_exptl_crystal_description       lath
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_F_000             11123
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.561
_shelx_estimated_absorpt_T_min   0.847
_shelx_estimated_absorpt_T_max   0.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_process_details   'SADABS-2014/5 - Bruker AXS, Madison WI'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_source                   
;
Advanced Light Source, station 11.3.1
;
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            226986
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_av_R_equivalents  0.0981
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.149
_diffrn_reflns_theta_max         24.191
_diffrn_reflns_theta_full        24.191
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             14570
_reflns_number_gt                11211
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2 Bruker-AXS, Madison WI'
_computing_cell_refinement       'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_structure_solution    'SHELXT 2014/4 Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2013)'
_computing_molecular_graphics    
;
Bruker SHELXTL Bruker-AXS, Madison WI
and local programs
;
_computing_publication_material  'Bruker SHELXTL Bruker-AXS, Madison WI'


_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. All non-hydrogen atoms were 
 refined anisotropically.
 Hydrogen atoms were placed geometrically on the carbon atoms and refined
 with a riding model.
 Hydrogen atoms on the bound methanol molecules and water molecules were found
 in the Fourier difference map, their distance fixed, and refined with a riding model.
 Hydrogen atoms on the free water molecule could not be found and were therefore left out
 of the model, but left in the formula for accuracy.
 One of the dichloromethane positions is disordered and suitable restraints and constraints
 were use to model this disorder (SADI/SIMU/DELU/EXYZ/EADP). Similarly, one of the attached
 ligands appears to be in motion or disordered over multiple positions, SIMU and DELU were
 used to better model the displacement parameters.
 The diffraction quality is poor (~0.95 Ang) and also contains a weaker second crystal domain
 which was ignored. Due to this, there is additional residual density in non chemically sesnsible
 locations, as well as a larger (130) number of systematic abscence violations.
 The cell contains a void with an unknown number and type of solvent molecules. 
 The solvents used in the crystal growth were both methanol and dichloromethane.
 Attempts were made to model these into the overlapping density; however, no
 chemically reasonable model could be found. Thus the residual density was treated
 with the program SQUEEZE [Reference to van der Sluis, P. & Spek, A. L., Acta Cryst. 
 1990, A46, 194-201] as implemented in Platon [Reference to Spek, A. L., Acta Cryst. 
 2009, D65, 148-155] which allows for the mathematical compensation of the electron 
 contribution of disordered solvent contained in the voids to the calculated 
 diffraction intensities.

# Solvent Accessible Volume =    1416.7
# Electrons Found in S.A.V. =     251.0
;

# start Validation Reply Form
_vrf_THETM01_pp140d              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Diffract data trimmed to 0.95 Ang with Rmerge <0.35 and I/sig > 2
;
_vrf_PLAT234_pp140d              
;
PROBLEM: Large Hirshfeld Difference O24    --  C114    ..       0.36 Ang.  
RESPONSE: bound methanol which is likely disordered
;
_vrf_PLAT220_pp140d              
;
PROBLEM: Large Non-Solvent  C     Ueq(max)/Ueq(min) Range        6.5 Ratio 
RESPONSE: Some of the bound ligands (methanol and main ligand) are either
 in motion or disordered over many positions.
;
_vrf_PLAT222_pp140d              
;
PROBLEM: Large Non-Solvent  H     Uiso(max)/Uiso(min) ...        7.6 Ratio 
RESPONSE: Some of the bound ligands (methanol and main ligand) are either
 in motion or disordered over many positions.
;
_vrf_PLAT242_pp140d              
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        O24 Check 
RESPONSE: bound methanol which is likely disordered
;
_vrf_PLAT341_pp140d              
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01602 Ang.  
RESPONSE: low resolution dataset plagued with unresolved twinning and
 lots of disorder
;
# end Validation Reply Form

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0721P)²+329.1099P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14570
_refine_ls_number_parameters     1537
_refine_ls_number_restraints     584
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0803
_refine_ls_wR_factor_ref         0.2190
_refine_ls_wR_factor_gt          0.1958
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.085
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.27290(4) 0.67434(4) 0.40643(4) 0.0305(3) Uani 1 1 d . . . . .
Ni2 Ni 0.35390(5) 0.56974(4) 0.36225(4) 0.0364(3) Uani 1 1 d . . . . .
Ni3 Ni 0.33302(5) 0.69001(4) 0.24681(4) 0.0350(3) Uani 1 1 d . . . . .
Ni4 Ni 0.27337(5) 0.56821(4) 0.21127(4) 0.0385(3) Uani 1 1 d . . . . .
Ni5 Ni 0.14509(4) 0.66381(4) 0.27940(4) 0.0338(3) Uani 1 1 d . . . . .
Ni6 Ni 0.16223(5) 0.55093(4) 0.35139(4) 0.0390(3) Uani 1 1 d . . . . .
O1W O 0.2980(2) 0.6212(2) 0.36420(19) 0.0345(15) Uani 1 1 d . . . . .
H1W H 0.2993 0.6393 0.3421 0.041 Uiso 1 1 d R U . . .
H2W H 0.2775 0.5991 0.3587 0.041 Uiso 1 1 d R U . . .
O2W O 0.2918(2) 0.6258(2) 0.25037(19) 0.0351(15) Uani 1 1 d . . . . .
H3W H 0.2007 0.6301 0.3249 0.042 Uiso 1 1 d R U . . .
H4W H 0.2005 0.5975 0.2941 0.042 Uiso 1 1 d R U . . .
O3W O 0.1807(2) 0.6100(2) 0.31335(19) 0.0336(15) Uani 1 1 d . . . . .
H5W H 0.2656 0.6356 0.2641 0.040 Uiso 1 1 d R U . . .
H6W H 0.3030 0.6087 0.2717 0.040 Uiso 1 1 d R U . . .
Cl1 Cl 0.04604(11) 0.80090(12) 0.44269(11) 0.0699(9) Uani 1 1 d . . . . .
N1 N 0.2482(3) 0.7273(2) 0.4422(2) 0.0318(18) Uani 1 1 d . . . . .
O1 O 0.1508(2) 0.7066(2) 0.3350(2) 0.0358(15) Uani 1 1 d . . . . .
O2 O 0.2175(2) 0.6774(2) 0.36488(18) 0.0299(14) Uani 1 1 d . . . . .
O3 O 0.3279(2) 0.6661(2) 0.44675(19) 0.0356(15) Uani 1 1 d . . . . .
C1 C 0.1796(4) 0.7049(3) 0.3661(3) 0.033(2) Uani 1 1 d . . . . .
C2 C 0.1674(4) 0.7326(3) 0.4059(3) 0.033(2) Uani 1 1 d . . . . .
C3 C 0.1203(4) 0.7514(3) 0.4075(3) 0.043(3) Uani 1 1 d . . . . .
H3A H 0.0996 0.7481 0.3832 0.051 Uiso 1 1 calc R U . . .
C4 C 0.1034(4) 0.7748(4) 0.4438(4) 0.049(3) Uani 1 1 d . . . . .
C5 C 0.1317(4) 0.7776(4) 0.4800(4) 0.051(3) Uani 1 1 d . . . . .
H5A H 0.1193 0.7918 0.5056 0.061 Uiso 1 1 calc R U . . .
C6 C 0.1780(4) 0.7598(3) 0.4790(3) 0.042(3) Uani 1 1 d . . . . .
H6A H 0.1973 0.7614 0.5044 0.050 Uiso 1 1 calc R U . . .
C7 C 0.1977(3) 0.7395(3) 0.4422(3) 0.031(2) Uani 1 1 d . . . . .
C8 C 0.2783(4) 0.7562(3) 0.4623(3) 0.033(2) Uani 1 1 d . . . . .
H8A H 0.2651 0.7853 0.4735 0.040 Uiso 1 1 calc R U . . .
C9 C 0.3287(4) 0.7483(3) 0.4690(3) 0.033(2) Uani 1 1 d . . . . .
C10 C 0.3510(4) 0.7027(3) 0.4626(3) 0.038(2) Uani 1 1 d . . . . .
C11 C 0.4005(4) 0.6961(4) 0.4743(3) 0.046(3) Uani 1 1 d . . . . .
H11A H 0.4154 0.6656 0.4696 0.055 Uiso 1 1 calc R U . . .
C12 C 0.4273(4) 0.7326(4) 0.4921(3) 0.047(3) Uani 1 1 d . . . . .
H12A H 0.4603 0.7268 0.4996 0.057 Uiso 1 1 calc R U . . .
C13 C 0.4068(4) 0.7789(4) 0.4997(3) 0.043(3) Uani 1 1 d . . . . .
C14 C 0.4337(5) 0.8152(5) 0.5185(4) 0.059(3) Uani 1 1 d . . . . .
H14A H 0.4665 0.8091 0.5261 0.071 Uiso 1 1 calc R U . . .
C15 C 0.4140(5) 0.8601(4) 0.5264(4) 0.061(3) Uani 1 1 d . . . . .
H15A H 0.4329 0.8843 0.5403 0.073 Uiso 1 1 calc R U . . .
C16 C 0.3670(5) 0.8695(4) 0.5141(4) 0.056(3) Uani 1 1 d . . . . .
H16A H 0.3534 0.9005 0.5193 0.067 Uiso 1 1 calc R U . . .
C17 C 0.3392(4) 0.8345(4) 0.4944(3) 0.046(3) Uani 1 1 d . . . . .
H17A H 0.3072 0.8421 0.4851 0.055 Uiso 1 1 calc R U . . .
C18 C 0.3576(4) 0.7875(3) 0.4876(3) 0.037(2) Uani 1 1 d . . . . .
Cl2 Cl 0.35066(15) 0.33858(11) 0.26512(12) 0.0853(12) Uani 1 1 d . . . . .
N2 N 0.4052(3) 0.5214(3) 0.3503(3) 0.045(2) Uani 1 1 d . . . . .
O4 O 0.3239(3) 0.5222(2) 0.2382(2) 0.0471(18) Uani 1 1 d . . . . .
O5 O 0.3347(2) 0.5616(2) 0.2995(2) 0.0394(16) Uani 1 1 d . . . . .
O6 O 0.4024(3) 0.6213(2) 0.3475(2) 0.0422(17) Uani 1 1 d . . . . .
C19 C 0.3389(4) 0.5243(4) 0.2762(3) 0.045(3) Uani 1 1 d . . . . .
C20 C 0.3599(4) 0.4786(4) 0.2944(4) 0.053(3) Uani 1 1 d . . . . .
C21 C 0.3479(5) 0.4351(4) 0.2756(4) 0.063(3) Uani 1 1 d . . . . .
H21 H 0.3273 0.4348 0.2509 0.075 Uiso 1 1 calc R U . . .
C22 C 0.3649(5) 0.3923(4) 0.2916(4) 0.064(4) Uani 1 1 d . . . . .
C23 C 0.3938(5) 0.3904(4) 0.3281(4) 0.066(4) Uani 1 1 d . . . . .
H23A H 0.4041 0.3604 0.3397 0.079 Uiso 1 1 calc R U . . .
C24 C 0.4070(4) 0.4333(4) 0.3470(4) 0.054(3) Uani 1 1 d . . . . .
H24A H 0.4273 0.4328 0.3718 0.064 Uiso 1 1 calc R U . . .
C25 C 0.3913(4) 0.4774(4) 0.3307(3) 0.045(3) Uani 1 1 d . . . . .
C26 C 0.4512(4) 0.5291(4) 0.3572(3) 0.045(3) Uani 1 1 d . . . . .
H26A H 0.4731 0.5032 0.3519 0.054 Uiso 1 1 calc R U . . .
C27 C 0.4708(4) 0.5733(4) 0.3720(3) 0.043(3) Uani 1 1 d . . . . .
C28 C 0.4464(4) 0.6175(4) 0.3639(3) 0.047(3) Uani 1 1 d . . . . .
C29 C 0.4716(5) 0.6612(4) 0.3723(4) 0.058(3) Uani 1 1 d . . . . .
H29A H 0.4571 0.6912 0.3647 0.069 Uiso 1 1 calc R U . . .
C30 C 0.5163(5) 0.6607(5) 0.3910(4) 0.062(3) Uani 1 1 d . . . . .
H30A H 0.5320 0.6906 0.3969 0.074 Uiso 1 1 calc R U . . .
C31 C 0.5404(4) 0.6171(5) 0.4019(4) 0.059(3) Uani 1 1 d . . . . .
C32 C 0.5866(5) 0.6166(7) 0.4235(4) 0.080(4) Uani 1 1 d . . . . .
H32A H 0.6025 0.6461 0.4302 0.096 Uiso 1 1 calc R U . . .
C33 C 0.6067(6) 0.5751(7) 0.4339(5) 0.097(5) Uani 1 1 d . . . . .
H33A H 0.6370 0.5755 0.4487 0.116 Uiso 1 1 calc R U . . .
C34 C 0.5864(5) 0.5317(6) 0.4244(5) 0.083(4) Uani 1 1 d . . . . .
H34A H 0.6026 0.5027 0.4320 0.100 Uiso 1 1 calc R U . . .
C35 C 0.5420(4) 0.5302(5) 0.4038(4) 0.064(3) Uani 1 1 d . . . . .
H35A H 0.5275 0.4999 0.3973 0.077 Uiso 1 1 calc R U . . .
C36 C 0.5178(4) 0.5735(5) 0.3922(4) 0.057(3) Uani 1 1 d . . . . .
Cl3 Cl 0.46955(19) 0.82336(19) 0.40465(11) 0.131(2) Uani 1 1 d . . . . .
N3 N 0.3691(3) 0.7519(3) 0.2486(3) 0.042(2) Uani 1 1 d . . . . .
O7 O 0.3151(2) 0.7251(2) 0.3745(2) 0.0343(15) Uani 1 1 d . . . . .
O8 O 0.3187(2) 0.6929(2) 0.30954(18) 0.0300(14) Uani 1 1 d . . . . .
O9 O 0.3470(2) 0.6846(2) 0.1846(2) 0.0434(17) Uani 1 1 d . . . . .
C37 C 0.3325(4) 0.7234(3) 0.3374(3) 0.034(2) Uani 1 1 d . . . . .
C38 C 0.3749(4) 0.7559(4) 0.3276(3) 0.040(2) Uani 1 1 d . . . . .
C39 C 0.3978(4) 0.7745(4) 0.3636(3) 0.056(3) Uani 1 1 d . . . . .
H39A H 0.3850 0.7688 0.3916 0.067 Uiso 1 1 calc R U . . .
C40 C 0.4398(5) 0.8016(5) 0.3581(4) 0.076(4) Uani 1 1 d . . . . .
C41 C 0.4591(5) 0.8107(5) 0.3185(4) 0.074(4) Uani 1 1 d . . . . .
H41A H 0.4884 0.8285 0.3157 0.089 Uiso 1 1 calc R U . . .
C42 C 0.4356(5) 0.7937(4) 0.2831(4) 0.061(3) Uani 1 1 d . . . . .
H42A H 0.4486 0.8001 0.2553 0.073 Uiso 1 1 calc R U . . .
C43 C 0.3923(4) 0.7669(4) 0.2866(3) 0.049(3) Uani 1 1 d . . . . .
C44 C 0.3684(4) 0.7804(4) 0.2159(3) 0.044(3) Uani 1 1 d . . . . .
H44A H 0.3814 0.8118 0.2203 0.053 Uiso 1 1 calc R U . . .
C45 C 0.3501(4) 0.7703(4) 0.1736(3) 0.044(3) Uani 1 1 d . . . . .
C46 C 0.3429(4) 0.7225(4) 0.1600(3) 0.044(3) Uani 1 1 d . . . . .
C47 C 0.3298(4) 0.7143(4) 0.1153(3) 0.048(3) Uani 1 1 d . . . . .
H47A H 0.3256 0.6821 0.1056 0.058 Uiso 1 1 calc R U . . .
C48 C 0.3234(4) 0.7506(5) 0.0871(4) 0.060(3) Uani 1 1 d . . . . .
H48A H 0.3141 0.7436 0.0583 0.072 Uiso 1 1 calc R U . . .
C49 C 0.3305(4) 0.7997(4) 0.0999(3) 0.049(3) Uani 1 1 d . . . . .
C50 C 0.3258(4) 0.8371(5) 0.0703(4) 0.065(4) Uani 1 1 d . . . . .
H50A H 0.3169 0.8300 0.0414 0.078 Uiso 1 1 calc R U . . .
C51 C 0.3339(5) 0.8837(5) 0.0822(4) 0.071(4) Uani 1 1 d . . . . .
H51A H 0.3316 0.9088 0.0615 0.085 Uiso 1 1 calc R U . . .
C52 C 0.3454(4) 0.8947(5) 0.1247(4) 0.062(3) Uani 1 1 d . . . . .
H52A H 0.3505 0.9273 0.1328 0.075 Uiso 1 1 calc R U . . .
C53 C 0.3494(4) 0.8588(4) 0.1550(4) 0.054(3) Uani 1 1 d . . . . .
H53A H 0.3563 0.8671 0.1841 0.065 Uiso 1 1 calc R U . . .
C54 C 0.3434(4) 0.8096(4) 0.1434(3) 0.049(3) Uani 1 1 d . . . . .
Cl4 Cl 0.22173(14) 0.32745(9) 0.27280(10) 0.0714(10) Uani 1 1 d . . . . .
N4 N 0.2455(3) 0.5130(3) 0.1796(2) 0.041(2) Uani 1 1 d . . . . .
O10 O 0.1757(3) 0.5056(2) 0.2990(2) 0.0456(18) Uani 1 1 d . . . . .
O11 O 0.2248(2) 0.5522(2) 0.25968(19) 0.0383(16) Uani 1 1 d . . . . .
O12 O 0.2243(2) 0.6087(2) 0.17968(19) 0.0391(16) Uani 1 1 d . . . . .
C55 C 0.2055(4) 0.5117(3) 0.2690(3) 0.038(3) Uani 1 1 d . . . . .
C56 C 0.2206(4) 0.4674(3) 0.2437(3) 0.043(3) Uani 1 1 d . . . . .
C57 C 0.2142(4) 0.4240(3) 0.2647(3) 0.048(3) Uani 1 1 d . . . . .
H57A H 0.1996 0.4233 0.2924 0.058 Uiso 1 1 calc R U . . .
C58 C 0.2292(5) 0.3813(3) 0.2453(4) 0.060(4) Uani 1 1 d . . . . .
C59 C 0.2507(4) 0.3820(4) 0.2046(3) 0.053(3) Uani 1 1 d . . . . .
H59A H 0.2616 0.3528 0.1917 0.063 Uiso 1 1 calc R U . . .
C60 C 0.2558(4) 0.4245(3) 0.1834(4) 0.050(3) Uani 1 1 d . . . . .
H60A H 0.2703 0.4247 0.1556 0.060 Uiso 1 1 calc R U . . .
C61 C 0.2403(4) 0.4683(3) 0.2017(3) 0.048(3) Uani 1 1 d . . . . .
C62 C 0.2336(4) 0.5161(3) 0.1393(3) 0.041(3) Uani 1 1 d . . . . .
H62A H 0.2254 0.4873 0.1244 0.050 Uiso 1 1 calc R U . . .
C63 C 0.2322(4) 0.5604(3) 0.1162(3) 0.038(2) Uani 1 1 d . . . . .
C64 C 0.2252(4) 0.6044(3) 0.1380(3) 0.037(2) Uani 1 1 d . . . . .
C65 C 0.2153(4) 0.6459(4) 0.1129(4) 0.049(3) Uani 1 1 d . . . . .
H65A H 0.2082 0.6752 0.1274 0.059 Uiso 1 1 calc R U . . .
C66 C 0.2156(4) 0.6458(4) 0.0693(3) 0.049(3) Uani 1 1 d . . . . .
H66A H 0.2098 0.6749 0.0540 0.059 Uiso 1 1 calc R U . . .
C67 C 0.2245(4) 0.6025(4) 0.0466(3) 0.044(3) Uani 1 1 d . . . . .
C68 C 0.2234(5) 0.6014(4) 0.0013(4) 0.067(4) Uani 1 1 d . . . . .
H68A H 0.2166 0.6302 -0.0141 0.080 Uiso 1 1 calc R U . . .
C69 C 0.2318(7) 0.5598(5) -0.0208(4) 0.097(6) Uani 1 1 d . . . . .
H69A H 0.2291 0.5592 -0.0513 0.116 Uiso 1 1 calc R U . . .
C70 C 0.2444(7) 0.5178(5) 0.0020(4) 0.091(5) Uani 1 1 d . . . . .
H70A H 0.2527 0.4892 -0.0132 0.109 Uiso 1 1 calc R U . . .
C71 C 0.2449(5) 0.5182(4) 0.0457(4) 0.065(4) Uani 1 1 d . . . . .
H71A H 0.2529 0.4894 0.0606 0.078 Uiso 1 1 calc R U . . .
C72 C 0.2340(4) 0.5600(4) 0.0698(3) 0.047(3) Uani 1 1 d . . . . .
Cl5 Cl 0.20029(13) 0.80818(11) 0.09262(10) 0.0678(9) Uani 1 1 d . . . . .
N5 N 0.1154(3) 0.7187(3) 0.2483(3) 0.0437(10) Uani 1 1 d . U . . .
O13 O 0.2686(2) 0.7241(2) 0.2270(2) 0.0362(11) Uani 1 1 d . U . . .
O14 O 0.2120(2) 0.6806(2) 0.2594(2) 0.0353(11) Uani 1 1 d . U . . .
O15 O 0.0795(2) 0.6428(3) 0.2996(2) 0.0485(12) Uani 1 1 d . U . . .
C73 C 0.2248(4) 0.7133(3) 0.2331(3) 0.0366(9) Uani 1 1 d . U . . .
C74 C 0.1878(4) 0.7379(3) 0.2052(3) 0.0400(9) Uani 1 1 d . U . . .
C75 C 0.2060(4) 0.7607(3) 0.1684(3) 0.0423(11) Uani 1 1 d . U . . .
H75A H 0.2402 0.7626 0.1644 0.051 Uiso 1 1 calc R U . . .
C76 C 0.1754(4) 0.7806(3) 0.1377(3) 0.0442(11) Uani 1 1 d . U . . .
C77 C 0.1268(4) 0.7777(3) 0.1424(3) 0.0451(11) Uani 1 1 d . U . . .
H77A H 0.1061 0.7905 0.1208 0.054 Uiso 1 1 calc R U . . .
C78 C 0.1073(4) 0.7564(3) 0.1780(3) 0.0440(11) Uani 1 1 d . U . . .
H78A H 0.0729 0.7542 0.1806 0.053 Uiso 1 1 calc R U . . .
C79 C 0.1370(4) 0.7376(3) 0.2110(3) 0.0423(9) Uani 1 1 d . U . . .
C80 C 0.0767(4) 0.7388(4) 0.2640(3) 0.0475(11) Uani 1 1 d . U . . .
H80A H 0.0662 0.7676 0.2503 0.057 Uiso 1 1 calc R U . . .
C81 C 0.0478(4) 0.7226(4) 0.3000(4) 0.0513(10) Uani 1 1 d . U . . .
C82 C 0.0492(4) 0.6750(4) 0.3137(4) 0.0509(10) Uani 1 1 d . U . . .
C83 C 0.0163(4) 0.6600(4) 0.3483(4) 0.0543(11) Uani 1 1 d . U . . .
H83A H 0.0174 0.6276 0.3582 0.065 Uiso 1 1 calc R U . . .
C84 C -0.0149(4) 0.6905(4) 0.3661(4) 0.0575(12) Uani 1 1 d . U . . .
H84A H -0.0375 0.6790 0.3869 0.069 Uiso 1 1 calc R U . . .
C85 C -0.0151(4) 0.7387(4) 0.3550(4) 0.0588(11) Uani 1 1 d . U . . .
C86 C -0.0451(4) 0.7733(4) 0.3778(4) 0.0618(12) Uani 1 1 d . U . . .
H86A H -0.0665 0.7626 0.3998 0.074 Uiso 1 1 calc R U . . .
C87 C -0.0430(4) 0.8202(5) 0.3681(4) 0.0626(13) Uani 1 1 d . U . . .
H87A H -0.0624 0.8421 0.3842 0.075 Uiso 1 1 calc R U . . .
C88 C -0.0138(4) 0.8383(5) 0.3359(4) 0.0616(13) Uani 1 1 d . U . . .
H88A H -0.0136 0.8718 0.3297 0.074 Uiso 1 1 calc R U . . .
C89 C 0.0160(4) 0.8058(4) 0.3119(4) 0.0593(12) Uani 1 1 d . U . . .
H89A H 0.0364 0.8176 0.2895 0.071 Uiso 1 1 calc R U . . .
C90 C 0.0150(4) 0.7569(4) 0.3216(4) 0.0565(10) Uani 1 1 d . U . . .
Cl6 Cl 0.28624(13) 0.32967(9) 0.37137(10) 0.0620(8) Uani 1 1 d . U . . .
N6 N 0.1579(4) 0.4982(3) 0.3951(3) 0.0532(11) Uani 1 1 d . U . . .
O16 O 0.3056(3) 0.5147(2) 0.3779(2) 0.0437(11) Uani 1 1 d . U . . .
O17 O 0.2356(3) 0.5504(2) 0.3631(2) 0.0413(11) Uani 1 1 d . U . . .
O18 O 0.1484(3) 0.5963(2) 0.3995(2) 0.0573(13) Uani 1 1 d . U . . .
C91 C 0.2603(4) 0.5139(3) 0.3723(3) 0.0432(10) Uani 1 1 d . U . . .
C92 C 0.2370(4) 0.4641(3) 0.3759(3) 0.0466(9) Uani 1 1 d . U . . .
C93 C 0.2663(4) 0.4244(3) 0.3695(3) 0.0485(11) Uani 1 1 d . U . . .
H93A H 0.2993 0.4286 0.3613 0.058 Uiso 1 1 calc R U . . .
C94 C 0.2476(5) 0.3781(3) 0.3752(3) 0.0509(11) Uani 1 1 d . U . . .
C95 C 0.1993(4) 0.3712(4) 0.3851(3) 0.0515(11) Uani 1 1 d . U . . .
H95A H 0.1864 0.3395 0.3875 0.062 Uiso 1 1 calc R U . . .
C96 C 0.1699(5) 0.4106(3) 0.3914(3) 0.0506(11) Uani 1 1 d . U . . .
H96A H 0.1368 0.4060 0.3990 0.061 Uiso 1 1 calc R U . . .
C97 C 0.1882(4) 0.4575(3) 0.3868(3) 0.0497(10) Uani 1 1 d . U . . .
C98 C 0.1368(5) 0.5007(4) 0.4317(4) 0.0591(11) Uani 1 1 d . U . . .
H98A H 0.1386 0.4730 0.4497 0.071 Uiso 1 1 calc R U . . .
C99 C 0.1104(5) 0.5416(4) 0.4481(4) 0.0652(11) Uani 1 1 d . U . . .
C100 C 0.1187(5) 0.5874(4) 0.4317(4) 0.0621(11) Uani 1 1 d . U . . .
C101 C 0.0971(5) 0.6282(4) 0.4523(4) 0.0661(13) Uani 1 1 d . U . . .
H10D H 0.1019 0.6595 0.4406 0.079 Uiso 1 1 calc R U . . .
C102 C 0.0703(5) 0.6226(4) 0.4879(4) 0.0721(13) Uani 1 1 d . U . . .
H10E H 0.0567 0.6503 0.5014 0.087 Uiso 1 1 calc R U . . .
C103 C 0.0617(6) 0.5774(4) 0.5058(4) 0.0773(12) Uani 1 1 d . U . . .
C104 C 0.0343(6) 0.5738(5) 0.5461(5) 0.0836(14) Uani 1 1 d . U . . .
H10F H 0.0261 0.6021 0.5617 0.100 Uiso 1 1 calc R U . . .
C105 C 0.0202(6) 0.5283(5) 0.5616(5) 0.0867(15) Uani 1 1 d . U . . .
H10G H -0.0042 0.5249 0.5830 0.104 Uiso 1 1 calc R U . . .
C106 C 0.0438(6) 0.4883(5) 0.5440(5) 0.0858(15) Uani 1 1 d . U . . .
H10H H 0.0429 0.4584 0.5590 0.103 Uiso 1 1 calc R U . . .
C107 C 0.0690(6) 0.4911(5) 0.5044(5) 0.0816(14) Uani 1 1 d . U . . .
H10I H 0.0778 0.4625 0.4895 0.098 Uiso 1 1 calc R U . . .
C108 C 0.0809(5) 0.5366(4) 0.4870(4) 0.0751(12) Uani 1 1 d . U . . .
Cl3S Cl 0.46030(15) 0.59468(15) 0.54049(12) 0.0903(10) Uani 1 1 d D U . . .
Cl4S Cl 0.54924(15) 0.53831(17) 0.53760(13) 0.0982(10) Uani 1 1 d D U . . .
C2S C 0.5097(4) 0.5765(5) 0.5076(4) 0.0942(11) Uani 1 1 d D U . . .
H2SA H 0.5278 0.6053 0.4976 0.113 Uiso 1 1 calc R U . . .
H2SB H 0.4974 0.5591 0.4820 0.113 Uiso 1 1 calc R U . . .
Cl1S Cl 0.0818(3) 0.4163(3) 0.2659(3) 0.1547(8) Uani 0.564(8) 1 d D U P A 1
Cl2S Cl 0.0845(4) 0.4746(4) 0.1935(4) 0.1533(11) Uani 0.564(8) 1 d D U P A 1
C1S C 0.0823(16) 0.4784(5) 0.2508(5) 0.1543(9) Uani 0.564(8) 1 d D U P A 1
H1SA H 0.1112 0.4952 0.2625 0.185 Uiso 0.564(8) 1 calc R U P A 1
H1SB H 0.0526 0.4952 0.2608 0.185 Uiso 0.564(8) 1 calc R U P A 1
C109 C 0.2248(4) 0.6219(4) 0.4843(3) 0.047(3) Uani 1 1 d . . . . .
H10A H 0.2553 0.6277 0.4997 0.071 Uiso 1 1 calc R U . . .
H10B H 0.2109 0.5911 0.4937 0.071 Uiso 1 1 calc R U . . .
H10C H 0.2019 0.6480 0.4905 0.071 Uiso 1 1 calc R U . . .
O19 O 0.2341(2) 0.6201(2) 0.43903(19) 0.0375(16) Uani 1 1 d . . . . .
H19 H 0.2077 0.6219 0.4255 0.045 Uiso 1 1 calc R U . . .
C110 C 0.3555(6) 0.5502(5) 0.4591(4) 0.089(5) Uani 1 1 d . . . . .
H11B H 0.3221 0.5562 0.4685 0.133 Uiso 1 1 calc R U . . .
H11C H 0.3777 0.5548 0.4836 0.133 Uiso 1 1 calc R U . . .
H11D H 0.3584 0.5171 0.4484 0.133 Uiso 1 1 calc R U . . .
O20 O 0.3675(2) 0.5821(2) 0.42665(19) 0.0407(17) Uani 1 1 d . . . . .
H20 H 0.3533 0.6085 0.4308 0.049 Uiso 1 1 calc R U . . .
C111 C 0.4407(4) 0.6555(6) 0.2467(4) 0.076(4) Uani 1 1 d . . . . .
H11E H 0.4385 0.6610 0.2155 0.114 Uiso 1 1 calc R U . . .
H11F H 0.4602 0.6266 0.2522 0.114 Uiso 1 1 calc R U . . .
H11G H 0.4562 0.6834 0.2604 0.114 Uiso 1 1 calc R U . . .
O21 O 0.3938(2) 0.6492(3) 0.2638(2) 0.0482(18) Uani 1 1 d . . . . .
H21A H 0.3950 0.6507 0.2908 0.058 Uiso 1 1 calc R U . . .
C112 C 0.3675(7) 0.5694(7) 0.1527(7) 0.146(9) Uani 1 1 d . . . . .
H11H H 0.3858 0.5915 0.1341 0.219 Uiso 1 1 calc R U . . .
H11I H 0.3578 0.5409 0.1360 0.219 Uiso 1 1 calc R U . . .
H11J H 0.3879 0.5594 0.1770 0.219 Uiso 1 1 calc R U . . .
O22 O 0.3257(3) 0.5929(3) 0.1684(2) 0.0494(19) Uani 1 1 d . . . . .
H22 H 0.3319 0.6223 0.1724 0.059 Uiso 1 1 calc R U . . .
C113 C 0.1010(4) 0.6132(5) 0.1989(4) 0.064(3) Uani 1 1 d . . . . .
H11K H 0.0734 0.6307 0.2113 0.096 Uiso 1 1 calc R U . . .
H11L H 0.0923 0.5791 0.1954 0.096 Uiso 1 1 calc R U . . .
H11M H 0.1092 0.6270 0.1707 0.096 Uiso 1 1 calc R U . . .
O23 O 0.1415(3) 0.6171(2) 0.2268(2) 0.0413(17) Uani 1 1 d . . . . .
H23 H 0.1669 0.6206 0.2121 0.050 Uiso 1 1 calc R U . . .
C114 C 0.0524(8) 0.5308(8) 0.3427(10) 0.202(14) Uani 1 1 d . . . . .
H11N H 0.0619 0.4978 0.3504 0.303 Uiso 1 1 calc R U . . .
H11O H 0.0287 0.5299 0.3192 0.303 Uiso 1 1 calc R U . . .
H11P H 0.0379 0.5467 0.3679 0.303 Uiso 1 1 calc R U . . .
O24 O 0.0920(3) 0.5556(3) 0.3300(3) 0.060(2) Uani 1 1 d . . . . .
H24 H 0.0833 0.5817 0.3186 0.072 Uiso 1 1 calc R U . . .
C3S C 0.0861(9) 0.4736(19) 0.240(3) 0.1543(9) Uani 0.215(8) 1 d D U P B 2
H3SA H 0.1045 0.4707 0.2127 0.185 Uiso 0.215(8) 1 calc R U P B 2
H3SB H 0.1031 0.4969 0.2589 0.185 Uiso 0.215(8) 1 calc R U P B 2
Cl5S Cl 0.0256(7) 0.4935(6) 0.2295(7) 0.1544(8) Uani 0.215(8) 1 d D U P B 2
Cl6S Cl 0.0818(3) 0.4163(3) 0.2659(3) 0.1547(8) Uani 0.215(8) 1 d D U P B 2
C7S C 0.0256(7) 0.4935(6) 0.2295(7) 0.1544(8) Uani 0.219(6) 1 d D U P C 3
H7SA H 0.0227 0.4928 0.1977 0.185 Uiso 0.219(6) 1 calc R U P C 3
H7SB H 0.0577 0.5070 0.2374 0.185 Uiso 0.219(6) 1 calc R U P C 3
Cl7S Cl 0.0175(10) 0.4345(6) 0.2520(9) 0.1547(10) Uani 0.219(6) 1 d D U P C 3
Cl8S Cl -0.0227(9) 0.5282(8) 0.2531(10) 0.1547(11) Uani 0.219(6) 1 d D U P C 3
O4W O 0.0455(9) 0.4343(9) 0.3363(8) 0.050(10) Uiso 0.29(2) 1 d . . P D 4


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.962(7) . ?
Ni1 O3 1.977(6) . ?
Ni1 O2 1.999(6) . ?
Ni1 O7 2.075(6) . ?
Ni1 O1W 2.088(6) . ?
Ni1 O19 2.103(6) . ?
Ni2 N2 1.980(9) . ?
Ni2 O6 2.008(7) . ?
Ni2 O5 2.028(6) . ?
Ni2 O20 2.061(6) . ?
Ni2 O16 2.080(7) . ?
Ni2 O1W 2.099(6) . ?
Ni3 O9 1.974(7) . ?
Ni3 N3 1.982(8) . ?
Ni3 O8 1.987(6) . ?
Ni3 O21 2.087(7) . ?
Ni3 O13 2.099(6) . ?
Ni3 O2W 2.112(6) . ?
Ni4 N4 1.973(8) . ?
Ni4 O12 2.011(6) . ?
Ni4 O11 2.059(7) . ?
Ni4 O4 2.064(7) . ?
Ni4 O2W 2.069(6) . ?
Ni4 O22 2.077(7) . ?
Ni5 N5 1.978(8) . ?
Ni5 O14 1.998(7) . ?
Ni5 O15 1.999(7) . ?
Ni5 O3W 2.073(6) . ?
Ni5 O23 2.085(6) . ?
Ni5 O1 2.100(6) . ?
Ni6 O18 1.988(7) . ?
Ni6 N6 1.999(8) . ?
Ni6 O24 2.048(7) . ?
Ni6 O17 2.051(7) . ?
Ni6 O3W 2.080(6) . ?
Ni6 O10 2.087(7) . ?
O1W H1W 0.8494 . ?
O1W H2W 0.8499 . ?
O2W H5W 0.8799 . ?
O2W H6W 0.8695 . ?
O3W H3W 0.8599 . ?
O3W H4W 0.8787 . ?
Cl1 C4 1.737(10) . ?
N1 C8 1.308(11) . ?
N1 C7 1.429(12) . ?
O1 C1 1.248(11) . ?
O2 C1 1.292(11) . ?
O3 C10 1.292(11) . ?
C1 C2 1.491(13) . ?
C2 C3 1.398(14) . ?
C2 C7 1.415(13) . ?
C3 C4 1.379(14) . ?
C3 H3A 0.9500 . ?
C4 C5 1.369(15) . ?
C5 C6 1.367(14) . ?
C5 H5A 0.9500 . ?
C6 C7 1.383(13) . ?
C6 H6A 0.9500 . ?
C8 C9 1.420(13) . ?
C8 H8A 0.9500 . ?
C9 C10 1.418(13) . ?
C9 C18 1.466(13) . ?
C10 C11 1.422(14) . ?
C11 C12 1.367(14) . ?
C11 H11A 0.9500 . ?
C12 C13 1.423(15) . ?
C12 H12A 0.9500 . ?
C13 C14 1.377(15) . ?
C13 C18 1.423(14) . ?
C14 C15 1.379(17) . ?
C14 H14A 0.9500 . ?
C15 C16 1.375(16) . ?
C15 H15A 0.9500 . ?
C16 C17 1.379(14) . ?
C16 H16A 0.9500 . ?
C17 C18 1.412(14) . ?
C17 H17A 0.9500 . ?
Cl2 C22 1.746(11) . ?
N2 C26 1.300(13) . ?
N2 C25 1.417(13) . ?
O4 C19 1.250(12) . ?
O5 C19 1.269(11) . ?
O6 C28 1.317(12) . ?
C19 C20 1.501(14) . ?
C20 C21 1.381(15) . ?
C20 C25 1.421(14) . ?
C21 C22 1.368(15) . ?
C21 H21 0.9500 . ?
C22 C23 1.382(16) . ?
C23 C24 1.374(15) . ?
C23 H23A 0.9500 . ?
C24 C25 1.390(14) . ?
C24 H24A 0.9500 . ?
C26 C27 1.415(15) . ?
C26 H26A 0.9500 . ?
C27 C28 1.419(15) . ?
C27 C36 1.440(15) . ?
C28 C29 1.419(15) . ?
C29 C30 1.361(17) . ?
C29 H29A 0.9500 . ?
C30 C31 1.420(17) . ?
C30 H30A 0.9500 . ?
C31 C36 1.391(17) . ?
C31 C32 1.436(17) . ?
C32 C33 1.32(2) . ?
C32 H32A 0.9500 . ?
C33 C34 1.36(2) . ?
C33 H33A 0.9500 . ?
C34 C35 1.380(17) . ?
C34 H34A 0.9500 . ?
C35 C36 1.417(17) . ?
C35 H35A 0.9500 . ?
Cl3 C40 1.766(11) . ?
N3 C44 1.286(13) . ?
N3 C43 1.403(13) . ?
O7 C37 1.249(11) . ?
O8 C37 1.268(10) . ?
O9 C46 1.303(12) . ?
C37 C38 1.504(14) . ?
C38 C39 1.380(14) . ?
C38 C43 1.395(14) . ?
C39 C40 1.388(16) . ?
C39 H39A 0.9500 . ?
C40 C41 1.362(16) . ?
C41 C42 1.360(16) . ?
C41 H41A 0.9500 . ?
C42 C43 1.407(16) . ?
C42 H42A 0.9500 . ?
C44 C45 1.432(14) . ?
C44 H44A 0.9500 . ?
C45 C46 1.406(15) . ?
C45 C54 1.447(15) . ?
C46 C47 1.451(14) . ?
C47 C48 1.345(15) . ?
C47 H47A 0.9500 . ?
C48 C49 1.430(17) . ?
C48 H48A 0.9500 . ?
C49 C50 1.390(16) . ?
C49 C54 1.423(15) . ?
C50 C51 1.363(19) . ?
C50 H50A 0.9500 . ?
C51 C52 1.388(18) . ?
C51 H51A 0.9500 . ?
C52 C53 1.372(16) . ?
C52 H52A 0.9500 . ?
C53 C54 1.420(16) . ?
C53 H53A 0.9500 . ?
Cl4 C58 1.732(11) . ?
N4 C62 1.295(12) . ?
N4 C61 1.423(12) . ?
O10 C55 1.254(12) . ?
O11 C55 1.272(12) . ?
O12 C64 1.298(11) . ?
C55 C56 1.515(13) . ?
C56 C57 1.380(14) . ?
C56 C61 1.410(15) . ?
C57 C58 1.390(15) . ?
C57 H57A 0.9500 . ?
C58 C59 1.394(17) . ?
C59 C60 1.357(15) . ?
C59 H59A 0.9500 . ?
C60 C61 1.407(14) . ?
C60 H60A 0.9500 . ?
C62 C63 1.423(14) . ?
C62 H62A 0.9500 . ?
C63 C64 1.407(13) . ?
C63 C72 1.439(14) . ?
C64 C65 1.415(14) . ?
C65 C66 1.352(15) . ?
C65 H65A 0.9500 . ?
C66 C67 1.413(14) . ?
C66 H66A 0.9500 . ?
C67 C68 1.404(15) . ?
C67 C72 1.407(15) . ?
C68 C69 1.360(17) . ?
C68 H68A 0.9500 . ?
C69 C70 1.405(19) . ?
C69 H69A 0.9500 . ?
C70 C71 1.355(16) . ?
C70 H70A 0.9500 . ?
C71 C72 1.410(15) . ?
C71 H71A 0.9500 . ?
Cl5 C76 1.734(11) . ?
N5 C80 1.297(13) . ?
N5 C79 1.403(13) . ?
O13 C73 1.257(11) . ?
O14 C73 1.267(11) . ?
O15 C82 1.295(12) . ?
C73 C74 1.502(14) . ?
C74 C75 1.396(14) . ?
C74 C79 1.410(14) . ?
C75 C76 1.387(14) . ?
C75 H75A 0.9500 . ?
C76 C77 1.348(15) . ?
C77 C78 1.362(14) . ?
C77 H77A 0.9500 . ?
C78 C79 1.409(14) . ?
C78 H78A 0.9500 . ?
C80 C81 1.443(16) . ?
C80 H80A 0.9500 . ?
C81 C82 1.384(16) . ?
C81 C90 1.471(15) . ?
C82 C83 1.465(16) . ?
C83 C84 1.327(15) . ?
C83 H83A 0.9500 . ?
C84 C85 1.380(17) . ?
C84 H84A 0.9500 . ?
C85 C90 1.418(17) . ?
C85 C86 1.450(16) . ?
C86 C87 1.334(17) . ?
C86 H86A 0.9500 . ?
C87 C88 1.376(17) . ?
C87 H87A 0.9500 . ?
C88 C89 1.426(16) . ?
C88 H88A 0.9500 . ?
C89 C90 1.390(17) . ?
C89 H89A 0.9500 . ?
Cl6 C94 1.716(11) . ?
N6 C98 1.277(14) . ?
N6 C97 1.426(14) . ?
O16 C91 1.259(12) . ?
O17 C91 1.252(11) . ?
O18 C100 1.315(13) . ?
C91 C92 1.525(14) . ?
C92 C93 1.377(14) . ?
C92 C97 1.397(16) . ?
C93 C94 1.394(14) . ?
C93 H93A 0.9500 . ?
C94 C95 1.378(16) . ?
C95 C96 1.371(15) . ?
C95 H95A 0.9500 . ?
C96 C97 1.401(14) . ?
C96 H96A 0.9500 . ?
C98 C99 1.439(16) . ?
C98 H98A 0.9500 . ?
C99 C100 1.386(16) . ?
C99 C108 1.459(17) . ?
C100 C101 1.428(16) . ?
C101 C102 1.339(16) . ?
C101 H10D 0.9500 . ?
C102 C103 1.391(17) . ?
C102 H10E 0.9500 . ?
C103 C108 1.379(17) . ?
C103 C104 1.461(18) . ?
C104 C105 1.403(18) . ?
C104 H10F 0.9500 . ?
C105 C106 1.396(18) . ?
C105 H10G 0.9500 . ?
C106 C107 1.412(18) . ?
C106 H10H 0.9500 . ?
C107 C108 1.411(17) . ?
C107 H10I 0.9500 . ?
Cl3S C2S 1.773(9) . ?
Cl4S C2S 1.780(10) . ?
C2S H2SA 0.9900 . ?
C2S H2SB 0.9900 . ?
Cl1S C1S 1.783(11) . ?
Cl2S C1S 1.784(11) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C109 O19 1.427(11) . ?
C109 H10A 0.9800 . ?
C109 H10B 0.9800 . ?
C109 H10C 0.9800 . ?
O19 H19 0.8400 . ?
C110 O20 1.380(14) . ?
C110 H11B 0.9800 . ?
C110 H11C 0.9800 . ?
C110 H11D 0.9800 . ?
O20 H20 0.8400 . ?
C111 O21 1.407(13) . ?
C111 H11E 0.9800 . ?
C111 H11F 0.9800 . ?
C111 H11G 0.9800 . ?
O21 H21A 0.8400 . ?
C112 O22 1.409(17) . ?
C112 H11H 0.9800 . ?
C112 H11I 0.9800 . ?
C112 H11J 0.9800 . ?
O22 H22 0.8400 . ?
C113 O23 1.416(12) . ?
C113 H11K 0.9800 . ?
C113 H11L 0.9800 . ?
C113 H11M 0.9800 . ?
O23 H23 0.8400 . ?
C114 O24 1.35(2) . ?
C114 H11N 0.9800 . ?
C114 H11O 0.9800 . ?
C114 H11P 0.9800 . ?
O24 H24 0.8400 . ?
C3S Cl6S 1.784(12) . ?
C3S Cl5S 1.785(12) . ?
C3S H3SA 0.9900 . ?
C3S H3SB 0.9900 . ?
C7S Cl7S 1.793(11) . ?
C7S Cl8S 1.795(11) . ?
C7S H7SA 0.9900 . ?
C7S H7SB 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 O3 89.6(3) . . ?
N1 Ni1 O2 94.0(3) . . ?
O3 Ni1 O2 175.8(2) . . ?
N1 Ni1 O7 87.5(3) . . ?
O3 Ni1 O7 87.2(3) . . ?
O2 Ni1 O7 95.2(2) . . ?
N1 Ni1 O1W 175.6(3) . . ?
O3 Ni1 O1W 93.6(2) . . ?
O2 Ni1 O1W 82.9(2) . . ?
O7 Ni1 O1W 89.6(2) . . ?
N1 Ni1 O19 95.0(3) . . ?
O3 Ni1 O19 90.1(3) . . ?
O2 Ni1 O19 87.3(2) . . ?
O7 Ni1 O19 176.4(3) . . ?
O1W Ni1 O19 88.0(2) . . ?
N2 Ni2 O6 87.9(3) . . ?
N2 Ni2 O5 86.1(3) . . ?
O6 Ni2 O5 91.9(3) . . ?
N2 Ni2 O20 99.4(3) . . ?
O6 Ni2 O20 89.0(3) . . ?
O5 Ni2 O20 174.4(3) . . ?
N2 Ni2 O16 90.2(3) . . ?
O6 Ni2 O16 178.1(3) . . ?
O5 Ni2 O16 88.6(3) . . ?
O20 Ni2 O16 90.7(3) . . ?
N2 Ni2 O1W 170.9(3) . . ?
O6 Ni2 O1W 90.6(3) . . ?
O5 Ni2 O1W 84.9(2) . . ?
O20 Ni2 O1W 89.6(2) . . ?
O16 Ni2 O1W 91.3(3) . . ?
O9 Ni3 N3 89.8(3) . . ?
O9 Ni3 O8 177.9(3) . . ?
N3 Ni3 O8 92.2(3) . . ?
O9 Ni3 O21 92.8(3) . . ?
N3 Ni3 O21 93.5(3) . . ?
O8 Ni3 O21 86.2(3) . . ?
O9 Ni3 O13 85.0(3) . . ?
N3 Ni3 O13 92.4(3) . . ?
O8 Ni3 O13 95.8(2) . . ?
O21 Ni3 O13 173.7(3) . . ?
O9 Ni3 O2W 95.2(3) . . ?
N3 Ni3 O2W 174.8(3) . . ?
O8 Ni3 O2W 82.9(2) . . ?
O21 Ni3 O2W 87.7(3) . . ?
O13 Ni3 O2W 86.6(2) . . ?
N4 Ni4 O12 85.9(3) . . ?
N4 Ni4 O11 86.8(3) . . ?
O12 Ni4 O11 92.3(3) . . ?
N4 Ni4 O4 89.1(3) . . ?
O12 Ni4 O4 174.1(3) . . ?
O11 Ni4 O4 90.6(3) . . ?
N4 Ni4 O2W 170.4(3) . . ?
O12 Ni4 O2W 91.1(2) . . ?
O11 Ni4 O2W 84.2(2) . . ?
O4 Ni4 O2W 94.3(2) . . ?
N4 Ni4 O22 101.9(3) . . ?
O12 Ni4 O22 88.2(3) . . ?
O11 Ni4 O22 171.4(3) . . ?
O4 Ni4 O22 89.8(3) . . ?
O2W Ni4 O22 87.2(3) . . ?
N5 Ni5 O14 92.9(3) . . ?
N5 Ni5 O15 90.2(3) . . ?
O14 Ni5 O15 176.5(3) . . ?
N5 Ni5 O3W 175.5(3) . . ?
O14 Ni5 O3W 83.7(2) . . ?
O15 Ni5 O3W 93.4(3) . . ?
N5 Ni5 O23 94.3(3) . . ?
O14 Ni5 O23 86.9(3) . . ?
O15 Ni5 O23 91.3(3) . . ?
O3W Ni5 O23 88.5(2) . . ?
N5 Ni5 O1 89.9(3) . . ?
O14 Ni5 O1 93.1(2) . . ?
O15 Ni5 O1 88.5(3) . . ?
O3W Ni5 O1 87.3(2) . . ?
O23 Ni5 O1 175.8(2) . . ?
O18 Ni6 N6 86.7(3) . . ?
O18 Ni6 O24 91.3(3) . . ?
N6 Ni6 O24 102.2(4) . . ?
O18 Ni6 O17 93.5(3) . . ?
N6 Ni6 O17 86.1(3) . . ?
O24 Ni6 O17 170.7(3) . . ?
O18 Ni6 O3W 88.6(3) . . ?
N6 Ni6 O3W 167.2(3) . . ?
O24 Ni6 O3W 89.9(3) . . ?
O17 Ni6 O3W 82.3(2) . . ?
O18 Ni6 O10 177.5(3) . . ?
N6 Ni6 O10 95.7(3) . . ?
O24 Ni6 O10 87.3(3) . . ?
O17 Ni6 O10 87.6(3) . . ?
O3W Ni6 O10 89.3(3) . . ?
Ni1 O1W Ni2 137.7(3) . . ?
Ni1 O1W H1W 96.0 . . ?
Ni2 O1W H1W 110.2 . . ?
Ni1 O1W H2W 114.5 . . ?
Ni2 O1W H2W 89.5 . . ?
H1W O1W H2W 107.0 . . ?
Ni4 O2W Ni3 138.7(3) . . ?
Ni4 O2W H5W 108.6 . . ?
Ni3 O2W H5W 102.0 . . ?
Ni4 O2W H6W 96.3 . . ?
Ni3 O2W H6W 108.1 . . ?
H5W O2W H6W 95.1 . . ?
Ni5 O3W Ni6 137.6(3) . . ?
Ni5 O3W H3W 92.6 . . ?
Ni6 O3W H3W 115.5 . . ?
Ni5 O3W H4W 103.3 . . ?
Ni6 O3W H4W 103.2 . . ?
H3W O3W H4W 98.2 . . ?
C8 N1 C7 118.0(7) . . ?
C8 N1 Ni1 120.5(6) . . ?
C7 N1 Ni1 120.9(6) . . ?
C1 O1 Ni5 131.4(6) . . ?
C1 O2 Ni1 128.4(6) . . ?
C10 O3 Ni1 121.7(6) . . ?
O1 C1 O2 120.8(8) . . ?
O1 C1 C2 118.5(9) . . ?
O2 C1 C2 120.6(8) . . ?
C3 C2 C7 117.9(8) . . ?
C3 C2 C1 115.5(9) . . ?
C7 C2 C1 126.6(9) . . ?
C4 C3 C2 121.1(10) . . ?
C4 C3 H3A 119.4 . . ?
C2 C3 H3A 119.4 . . ?
C5 C4 C3 120.3(10) . . ?
C5 C4 Cl1 120.7(8) . . ?
C3 C4 Cl1 119.0(8) . . ?
C6 C5 C4 119.4(10) . . ?
C6 C5 H5A 120.3 . . ?
C4 C5 H5A 120.3 . . ?
C5 C6 C7 122.1(10) . . ?
C5 C6 H6A 118.9 . . ?
C7 C6 H6A 118.9 . . ?
C6 C7 C2 118.7(9) . . ?
C6 C7 N1 118.5(8) . . ?
C2 C7 N1 122.8(8) . . ?
N1 C8 C9 126.4(8) . . ?
N1 C8 H8A 116.8 . . ?
C9 C8 H8A 116.8 . . ?
C10 C9 C8 122.6(9) . . ?
C10 C9 C18 118.7(9) . . ?
C8 C9 C18 118.3(8) . . ?
O3 C10 C9 122.7(9) . . ?
O3 C10 C11 117.9(9) . . ?
C9 C10 C11 119.5(9) . . ?
C12 C11 C10 121.7(10) . . ?
C12 C11 H11A 119.1 . . ?
C10 C11 H11A 119.1 . . ?
C11 C12 C13 121.3(10) . . ?
C11 C12 H12A 119.3 . . ?
C13 C12 H12A 119.3 . . ?
C14 C13 C12 121.0(10) . . ?
C14 C13 C18 120.0(11) . . ?
C12 C13 C18 118.9(9) . . ?
C13 C14 C15 121.6(11) . . ?
C13 C14 H14A 119.2 . . ?
C15 C14 H14A 119.2 . . ?
C16 C15 C14 119.4(10) . . ?
C16 C15 H15A 120.3 . . ?
C14 C15 H15A 120.3 . . ?
C15 C16 C17 120.7(11) . . ?
C15 C16 H16A 119.6 . . ?
C17 C16 H16A 119.6 . . ?
C16 C17 C18 121.1(10) . . ?
C16 C17 H17A 119.4 . . ?
C18 C17 H17A 119.4 . . ?
C17 C18 C13 117.1(9) . . ?
C17 C18 C9 123.2(9) . . ?
C13 C18 C9 119.8(9) . . ?
C26 N2 C25 118.3(9) . . ?
C26 N2 Ni2 123.6(7) . . ?
C25 N2 Ni2 118.0(7) . . ?
C19 O4 Ni4 125.0(6) . . ?
C19 O5 Ni2 127.9(6) . . ?
C28 O6 Ni2 117.8(6) . . ?
O4 C19 O5 123.2(9) . . ?
O4 C19 C20 116.2(9) . . ?
O5 C19 C20 120.5(9) . . ?
C21 C20 C25 117.3(9) . . ?
C21 C20 C19 119.1(9) . . ?
C25 C20 C19 123.6(9) . . ?
C22 C21 C20 121.4(11) . . ?
C22 C21 H21 119.3 . . ?
C20 C21 H21 119.3 . . ?
C21 C22 C23 121.9(10) . . ?
C21 C22 Cl2 119.3(9) . . ?
C23 C22 Cl2 118.8(8) . . ?
C24 C23 C22 117.8(10) . . ?
C24 C23 H23A 121.1 . . ?
C22 C23 H23A 121.1 . . ?
C23 C24 C25 121.5(10) . . ?
C23 C24 H24A 119.2 . . ?
C25 C24 H24A 119.2 . . ?
C24 C25 N2 121.1(9) . . ?
C24 C25 C20 119.9(9) . . ?
N2 C25 C20 119.0(9) . . ?
N2 C26 C27 124.4(9) . . ?
N2 C26 H26A 117.8 . . ?
C27 C26 H26A 117.8 . . ?
C26 C27 C28 120.7(9) . . ?
C26 C27 C36 119.1(10) . . ?
C28 C27 C36 119.9(10) . . ?
O6 C28 C29 116.9(10) . . ?
O6 C28 C27 124.7(9) . . ?
C29 C28 C27 118.3(10) . . ?
C30 C29 C28 120.8(12) . . ?
C30 C29 H29A 119.6 . . ?
C28 C29 H29A 119.6 . . ?
C29 C30 C31 122.1(11) . . ?
C29 C30 H30A 118.9 . . ?
C31 C30 H30A 118.9 . . ?
C36 C31 C30 118.7(11) . . ?
C36 C31 C32 119.2(13) . . ?
C30 C31 C32 122.0(13) . . ?
C33 C32 C31 119.6(15) . . ?
C33 C32 H32A 120.2 . . ?
C31 C32 H32A 120.2 . . ?
C32 C33 C34 123.1(15) . . ?
C32 C33 H33A 118.5 . . ?
C34 C33 H33A 118.5 . . ?
C33 C34 C35 119.6(15) . . ?
C33 C34 H34A 120.2 . . ?
C35 C34 H34A 120.2 . . ?
C34 C35 C36 120.4(14) . . ?
C34 C35 H35A 119.8 . . ?
C36 C35 H35A 119.8 . . ?
C31 C36 C35 118.1(11) . . ?
C31 C36 C27 119.9(11) . . ?
C35 C36 C27 122.0(11) . . ?
C44 N3 C43 119.1(9) . . ?
C44 N3 Ni3 120.2(7) . . ?
C43 N3 Ni3 120.5(7) . . ?
C37 O7 Ni1 129.1(6) . . ?
C37 O8 Ni3 129.3(6) . . ?
C46 O9 Ni3 119.6(6) . . ?
O7 C37 O8 122.5(9) . . ?
O7 C37 C38 117.5(8) . . ?
O8 C37 C38 119.7(8) . . ?
C39 C38 C43 120.0(9) . . ?
C39 C38 C37 114.5(9) . . ?
C43 C38 C37 125.5(9) . . ?
C38 C39 C40 118.9(10) . . ?
C38 C39 H39A 120.5 . . ?
C40 C39 H39A 120.5 . . ?
C41 C40 C39 122.4(10) . . ?
C41 C40 Cl3 119.5(10) . . ?
C39 C40 Cl3 118.2(9) . . ?
C42 C41 C40 118.6(11) . . ?
C42 C41 H41A 120.7 . . ?
C40 C41 H41A 120.7 . . ?
C41 C42 C43 121.6(11) . . ?
C41 C42 H42A 119.2 . . ?
C43 C42 H42A 119.2 . . ?
C38 C43 N3 123.1(9) . . ?
C38 C43 C42 118.4(10) . . ?
N3 C43 C42 118.6(10) . . ?
N3 C44 C45 127.4(10) . . ?
N3 C44 H44A 116.3 . . ?
C45 C44 H44A 116.3 . . ?
C46 C45 C44 120.6(9) . . ?
C46 C45 C54 119.8(9) . . ?
C44 C45 C54 119.3(10) . . ?
O9 C46 C45 125.0(9) . . ?
O9 C46 C47 117.1(10) . . ?
C45 C46 C47 117.9(10) . . ?
C48 C47 C46 122.6(11) . . ?
C48 C47 H47A 118.7 . . ?
C46 C47 H47A 118.7 . . ?
C47 C48 C49 120.8(10) . . ?
C47 C48 H48A 119.6 . . ?
C49 C48 H48A 119.6 . . ?
C50 C49 C54 120.4(12) . . ?
C50 C49 C48 120.8(11) . . ?
C54 C49 C48 118.8(10) . . ?
C51 C50 C49 120.8(12) . . ?
C51 C50 H50A 119.6 . . ?
C49 C50 H50A 119.6 . . ?
C50 C51 C52 120.1(12) . . ?
C50 C51 H51A 119.9 . . ?
C52 C51 H51A 119.9 . . ?
C53 C52 C51 120.7(13) . . ?
C53 C52 H52A 119.6 . . ?
C51 C52 H52A 119.6 . . ?
C52 C53 C54 120.9(11) . . ?
C52 C53 H53A 119.6 . . ?
C54 C53 H53A 119.6 . . ?
C53 C54 C49 116.9(10) . . ?
C53 C54 C45 123.0(10) . . ?
C49 C54 C45 120.1(10) . . ?
C62 N4 C61 119.8(8) . . ?
C62 N4 Ni4 121.9(7) . . ?
C61 N4 Ni4 118.3(6) . . ?
C55 O10 Ni6 127.8(6) . . ?
C55 O11 Ni4 128.8(6) . . ?
C64 O12 Ni4 114.9(6) . . ?
O10 C55 O11 124.2(9) . . ?
O10 C55 C56 117.0(9) . . ?
O11 C55 C56 118.8(10) . . ?
C57 C56 C61 120.0(9) . . ?
C57 C56 C55 115.3(10) . . ?
C61 C56 C55 124.7(9) . . ?
C56 C57 C58 120.0(11) . . ?
C56 C57 H57A 120.0 . . ?
C58 C57 H57A 120.0 . . ?
C57 C58 C59 120.5(10) . . ?
C57 C58 Cl4 119.0(10) . . ?
C59 C58 Cl4 120.5(8) . . ?
C60 C59 C58 119.6(9) . . ?
C60 C59 H59A 120.2 . . ?
C58 C59 H59A 120.2 . . ?
C59 C60 C61 121.5(11) . . ?
C59 C60 H60A 119.2 . . ?
C61 C60 H60A 119.2 . . ?
C60 C61 C56 118.3(9) . . ?
C60 C61 N4 121.7(10) . . ?
C56 C61 N4 119.9(8) . . ?
N4 C62 C63 123.4(9) . . ?
N4 C62 H62A 118.3 . . ?
C63 C62 H62A 118.3 . . ?
C64 C63 C62 120.6(8) . . ?
C64 C63 C72 119.6(9) . . ?
C62 C63 C72 119.6(8) . . ?
O12 C64 C63 124.2(8) . . ?
O12 C64 C65 117.9(9) . . ?
C63 C64 C65 117.7(9) . . ?
C66 C65 C64 123.2(10) . . ?
C66 C65 H65A 118.4 . . ?
C64 C65 H65A 118.4 . . ?
C65 C66 C67 120.1(10) . . ?
C65 C66 H66A 119.9 . . ?
C67 C66 H66A 119.9 . . ?
C68 C67 C72 119.9(10) . . ?
C68 C67 C66 121.0(10) . . ?
C72 C67 C66 119.1(9) . . ?
C69 C68 C67 121.3(12) . . ?
C69 C68 H68A 119.4 . . ?
C67 C68 H68A 119.4 . . ?
C68 C69 C70 119.3(12) . . ?
C68 C69 H69A 120.3 . . ?
C70 C69 H69A 120.3 . . ?
C71 C70 C69 119.9(12) . . ?
C71 C70 H70A 120.0 . . ?
C69 C70 H70A 120.0 . . ?
C70 C71 C72 122.4(12) . . ?
C70 C71 H71A 118.8 . . ?
C72 C71 H71A 118.8 . . ?
C67 C72 C71 117.0(10) . . ?
C67 C72 C63 119.9(9) . . ?
C71 C72 C63 123.1(10) . . ?
C80 N5 C79 119.8(9) . . ?
C80 N5 Ni5 119.1(8) . . ?
C79 N5 Ni5 121.0(7) . . ?
C73 O13 Ni3 131.2(6) . . ?
C73 O14 Ni5 128.5(6) . . ?
C82 O15 Ni5 119.0(7) . . ?
O13 C73 O14 122.3(9) . . ?
O13 C73 C74 117.1(9) . . ?
O14 C73 C74 120.4(9) . . ?
C75 C74 C79 117.6(9) . . ?
C75 C74 C73 115.6(9) . . ?
C79 C74 C73 126.7(9) . . ?
C76 C75 C74 121.6(10) . . ?
C76 C75 H75A 119.2 . . ?
C74 C75 H75A 119.2 . . ?
C77 C76 C75 120.2(10) . . ?
C77 C76 Cl5 120.4(8) . . ?
C75 C76 Cl5 119.4(9) . . ?
C76 C77 C78 120.4(10) . . ?
C76 C77 H77A 119.8 . . ?
C78 C77 H77A 119.8 . . ?
C77 C78 C79 121.3(10) . . ?
C77 C78 H78A 119.4 . . ?
C79 C78 H78A 119.4 . . ?
N5 C79 C78 119.4(10) . . ?
N5 C79 C74 121.8(9) . . ?
C78 C79 C74 118.7(10) . . ?
N5 C80 C81 127.6(10) . . ?
N5 C80 H80A 116.2 . . ?
C81 C80 H80A 116.2 . . ?
C82 C81 C80 121.2(10) . . ?
C82 C81 C90 119.5(11) . . ?
C80 C81 C90 119.3(10) . . ?
O15 C82 C81 124.8(11) . . ?
O15 C82 C83 116.6(10) . . ?
C81 C82 C83 118.5(10) . . ?
C84 C83 C82 121.7(12) . . ?
C84 C83 H83A 119.2 . . ?
C82 C83 H83A 119.2 . . ?
C83 C84 C85 121.0(12) . . ?
C83 C84 H84A 119.5 . . ?
C85 C84 H84A 119.5 . . ?
C84 C85 C90 121.6(11) . . ?
C84 C85 C86 121.4(12) . . ?
C90 C85 C86 117.0(12) . . ?
C87 C86 C85 120.6(13) . . ?
C87 C86 H86A 119.7 . . ?
C85 C86 H86A 119.7 . . ?
C86 C87 C88 122.9(12) . . ?
C86 C87 H87A 118.5 . . ?
C88 C87 H87A 118.5 . . ?
C87 C88 C89 119.0(12) . . ?
C87 C88 H88A 120.5 . . ?
C89 C88 H88A 120.5 . . ?
C90 C89 C88 119.4(12) . . ?
C90 C89 H89A 120.3 . . ?
C88 C89 H89A 120.3 . . ?
C89 C90 C85 121.0(11) . . ?
C89 C90 C81 121.3(11) . . ?
C85 C90 C81 117.5(11) . . ?
C98 N6 C97 118.1(9) . . ?
C98 N6 Ni6 126.2(8) . . ?
C97 N6 Ni6 114.9(7) . . ?
C91 O16 Ni2 127.9(6) . . ?
C91 O17 Ni6 125.5(6) . . ?
C100 O18 Ni6 124.8(7) . . ?
O17 C91 O16 123.6(9) . . ?
O17 C91 C92 121.4(10) . . ?
O16 C91 C92 115.0(9) . . ?
C93 C92 C97 119.5(9) . . ?
C93 C92 C91 117.8(10) . . ?
C97 C92 C91 122.6(9) . . ?
C92 C93 C94 120.0(11) . . ?
C92 C93 H93A 120.0 . . ?
C94 C93 H93A 120.0 . . ?
C95 C94 C93 120.9(10) . . ?
C95 C94 Cl6 120.4(8) . . ?
C93 C94 Cl6 118.8(10) . . ?
C96 C95 C94 119.3(10) . . ?
C96 C95 H95A 120.3 . . ?
C94 C95 H95A 120.3 . . ?
C95 C96 C97 120.8(11) . . ?
C95 C96 H96A 119.6 . . ?
C97 C96 H96A 119.6 . . ?
C92 C97 C96 119.5(10) . . ?
C92 C97 N6 120.1(9) . . ?
C96 C97 N6 120.3(11) . . ?
N6 C98 C99 125.9(10) . . ?
N6 C98 H98A 117.0 . . ?
C99 C98 H98A 117.0 . . ?
C100 C99 C98 120.6(11) . . ?
C100 C99 C108 118.7(11) . . ?
C98 C99 C108 119.9(10) . . ?
O18 C100 C99 123.6(11) . . ?
O18 C100 C101 116.7(10) . . ?
C99 C100 C101 119.5(11) . . ?
C102 C101 C100 120.5(11) . . ?
C102 C101 H10D 119.8 . . ?
C100 C101 H10D 119.8 . . ?
C101 C102 C103 121.9(12) . . ?
C101 C102 H10E 119.1 . . ?
C103 C102 H10E 119.1 . . ?
C108 C103 C102 120.2(12) . . ?
C108 C103 C104 120.3(12) . . ?
C102 C103 C104 119.4(12) . . ?
C105 C104 C103 119.8(13) . . ?
C105 C104 H10F 120.1 . . ?
C103 C104 H10F 120.1 . . ?
C106 C105 C104 116.8(13) . . ?
C106 C105 H10G 121.6 . . ?
C104 C105 H10G 121.6 . . ?
C105 C106 C107 121.6(13) . . ?
C105 C106 H10H 119.2 . . ?
C107 C106 H10H 119.2 . . ?
C108 C107 C106 119.9(13) . . ?
C108 C107 H10I 120.1 . . ?
C106 C107 H10I 120.1 . . ?
C103 C108 C107 118.7(12) . . ?
C103 C108 C99 119.2(11) . . ?
C107 C108 C99 122.0(12) . . ?
Cl3S C2S Cl4S 109.7(7) . . ?
Cl3S C2S H2SA 109.7 . . ?
Cl4S C2S H2SA 109.7 . . ?
Cl3S C2S H2SB 109.7 . . ?
Cl4S C2S H2SB 109.7 . . ?
H2SA C2S H2SB 108.2 . . ?
Cl1S C1S Cl2S 101.8(10) . . ?
Cl1S C1S H1SA 111.4 . . ?
Cl2S C1S H1SA 111.4 . . ?
Cl1S C1S H1SB 111.4 . . ?
Cl2S C1S H1SB 111.4 . . ?
H1SA C1S H1SB 109.3 . . ?
O19 C109 H10A 109.5 . . ?
O19 C109 H10B 109.5 . . ?
H10A C109 H10B 109.5 . . ?
O19 C109 H10C 109.5 . . ?
H10A C109 H10C 109.5 . . ?
H10B C109 H10C 109.5 . . ?
C109 O19 Ni1 122.6(6) . . ?
C109 O19 H19 109.5 . . ?
Ni1 O19 H19 99.0 . . ?
O20 C110 H11B 109.5 . . ?
O20 C110 H11C 109.5 . . ?
H11B C110 H11C 109.5 . . ?
O20 C110 H11D 109.5 . . ?
H11B C110 H11D 109.5 . . ?
H11C C110 H11D 109.5 . . ?
C110 O20 Ni2 123.9(7) . . ?
C110 O20 H20 109.5 . . ?
Ni2 O20 H20 102.0 . . ?
O21 C111 H11E 109.5 . . ?
O21 C111 H11F 109.5 . . ?
H11E C111 H11F 109.5 . . ?
O21 C111 H11G 109.5 . . ?
H11E C111 H11G 109.5 . . ?
H11F C111 H11G 109.5 . . ?
C111 O21 Ni3 124.9(7) . . ?
C111 O21 H21A 109.5 . . ?
Ni3 O21 H21A 104.9 . . ?
O22 C112 H11H 109.5 . . ?
O22 C112 H11I 109.5 . . ?
H11H C112 H11I 109.5 . . ?
O22 C112 H11J 109.5 . . ?
H11H C112 H11J 109.5 . . ?
H11I C112 H11J 109.5 . . ?
C112 O22 Ni4 129.3(10) . . ?
C112 O22 H22 109.5 . . ?
Ni4 O22 H22 111.5 . . ?
O23 C113 H11K 109.5 . . ?
O23 C113 H11L 109.5 . . ?
H11K C113 H11L 109.5 . . ?
O23 C113 H11M 109.5 . . ?
H11K C113 H11M 109.5 . . ?
H11L C113 H11M 109.5 . . ?
C113 O23 Ni5 124.3(7) . . ?
C113 O23 H23 109.5 . . ?
Ni5 O23 H23 108.3 . . ?
O24 C114 H11N 109.5 . . ?
O24 C114 H11O 109.5 . . ?
H11N C114 H11O 109.5 . . ?
O24 C114 H11P 109.5 . . ?
H11N C114 H11P 109.5 . . ?
H11O C114 H11P 109.5 . . ?
C114 O24 Ni6 129.4(12) . . ?
C114 O24 H24 109.5 . . ?
Ni6 O24 H24 117.3 . . ?
Cl6S C3S Cl5S 107.2(11) . . ?
Cl6S C3S H3SA 110.3 . . ?
Cl5S C3S H3SA 110.3 . . ?
Cl6S C3S H3SB 110.3 . . ?
Cl5S C3S H3SB 110.3 . . ?
H3SA C3S H3SB 108.5 . . ?
Cl7S C7S Cl8S 103.7(11) . . ?
Cl7S C7S H7SA 111.0 . . ?
Cl8S C7S H7SA 111.0 . . ?
Cl7S C7S H7SB 111.0 . . ?
Cl8S C7S H7SB 111.0 . . ?
H7SA C7S H7SB 109.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni5 O1 C1 O2 10.3(13) . . . . ?
Ni5 O1 C1 C2 -165.4(6) . . . . ?
Ni1 O2 C1 O1 171.4(6) . . . . ?
Ni1 O2 C1 C2 -12.9(11) . . . . ?
O1 C1 C2 C3 10.7(12) . . . . ?
O2 C1 C2 C3 -165.0(8) . . . . ?
O1 C1 C2 C7 -172.2(8) . . . . ?
O2 C1 C2 C7 12.1(13) . . . . ?
C7 C2 C3 C4 -1.9(14) . . . . ?
C1 C2 C3 C4 175.4(9) . . . . ?
C2 C3 C4 C5 -3.7(16) . . . . ?
C2 C3 C4 Cl1 175.9(8) . . . . ?
C3 C4 C5 C6 4.2(17) . . . . ?
Cl1 C4 C5 C6 -175.4(8) . . . . ?
C4 C5 C6 C7 1.0(16) . . . . ?
C5 C6 C7 C2 -6.6(14) . . . . ?
C5 C6 C7 N1 172.3(9) . . . . ?
C3 C2 C7 C6 6.9(13) . . . . ?
C1 C2 C7 C6 -170.1(9) . . . . ?
C3 C2 C7 N1 -171.9(8) . . . . ?
C1 C2 C7 N1 11.0(14) . . . . ?
C8 N1 C7 C6 -37.4(12) . . . . ?
Ni1 N1 C7 C6 151.4(7) . . . . ?
C8 N1 C7 C2 141.5(9) . . . . ?
Ni1 N1 C7 C2 -29.8(11) . . . . ?
C7 N1 C8 C9 174.4(8) . . . . ?
Ni1 N1 C8 C9 -14.3(12) . . . . ?
N1 C8 C9 C10 -14.0(14) . . . . ?
N1 C8 C9 C18 172.7(8) . . . . ?
Ni1 O3 C10 C9 28.6(12) . . . . ?
Ni1 O3 C10 C11 -152.1(7) . . . . ?
C8 C9 C10 O3 6.0(14) . . . . ?
C18 C9 C10 O3 179.3(8) . . . . ?
C8 C9 C10 C11 -173.3(9) . . . . ?
C18 C9 C10 C11 0.0(13) . . . . ?
O3 C10 C11 C12 -178.5(9) . . . . ?
C9 C10 C11 C12 0.8(15) . . . . ?
C10 C11 C12 C13 -0.1(16) . . . . ?
C11 C12 C13 C14 178.8(10) . . . . ?
C11 C12 C13 C18 -1.3(15) . . . . ?
C12 C13 C14 C15 -179.3(11) . . . . ?
C18 C13 C14 C15 0.7(16) . . . . ?
C13 C14 C15 C16 -2.2(18) . . . . ?
C14 C15 C16 C17 0.6(18) . . . . ?
C15 C16 C17 C18 2.4(17) . . . . ?
C16 C17 C18 C13 -3.7(15) . . . . ?
C16 C17 C18 C9 176.5(10) . . . . ?
C14 C13 C18 C17 2.2(14) . . . . ?
C12 C13 C18 C17 -177.8(9) . . . . ?
C14 C13 C18 C9 -178.0(9) . . . . ?
C12 C13 C18 C9 2.0(14) . . . . ?
C10 C9 C18 C17 178.4(9) . . . . ?
C8 C9 C18 C17 -8.0(14) . . . . ?
C10 C9 C18 C13 -1.3(13) . . . . ?
C8 C9 C18 C13 172.2(9) . . . . ?
Ni4 O4 C19 O5 -18.7(16) . . . . ?
Ni4 O4 C19 C20 157.5(8) . . . . ?
Ni2 O5 C19 O4 176.7(8) . . . . ?
Ni2 O5 C19 C20 0.7(15) . . . . ?
O4 C19 C20 C21 -20.7(17) . . . . ?
O5 C19 C20 C21 155.6(12) . . . . ?
O4 C19 C20 C25 160.1(11) . . . . ?
O5 C19 C20 C25 -23.6(18) . . . . ?
C25 C20 C21 C22 1(2) . . . . ?
C19 C20 C21 C22 -178.2(13) . . . . ?
C20 C21 C22 C23 2(2) . . . . ?
C20 C21 C22 Cl2 -177.3(11) . . . . ?
C21 C22 C23 C24 -3(2) . . . . ?
Cl2 C22 C23 C24 176.2(10) . . . . ?
C22 C23 C24 C25 1(2) . . . . ?
C23 C24 C25 N2 -179.8(11) . . . . ?
C23 C24 C25 C20 1.7(18) . . . . ?
C26 N2 C25 C24 52.2(15) . . . . ?
Ni2 N2 C25 C24 -131.9(9) . . . . ?
C26 N2 C25 C20 -129.4(11) . . . . ?
Ni2 N2 C25 C20 46.6(13) . . . . ?
C21 C20 C25 C24 -2.8(18) . . . . ?
C19 C20 C25 C24 176.4(11) . . . . ?
C21 C20 C25 N2 178.8(11) . . . . ?
C19 C20 C25 N2 -2.1(18) . . . . ?
C25 N2 C26 C27 172.6(9) . . . . ?
Ni2 N2 C26 C27 -3.2(14) . . . . ?
N2 C26 C27 C28 -26.3(16) . . . . ?
N2 C26 C27 C36 158.9(10) . . . . ?
Ni2 O6 C28 C29 -149.4(7) . . . . ?
Ni2 O6 C28 C27 33.5(12) . . . . ?
C26 C27 C28 O6 8.5(16) . . . . ?
C36 C27 C28 O6 -176.7(9) . . . . ?
C26 C27 C28 C29 -168.6(10) . . . . ?
C36 C27 C28 C29 6.2(15) . . . . ?
O6 C28 C29 C30 177.1(10) . . . . ?
C27 C28 C29 C30 -5.5(16) . . . . ?
C28 C29 C30 C31 1.7(18) . . . . ?
C29 C30 C31 C36 1.5(18) . . . . ?
C29 C30 C31 C32 -177.0(11) . . . . ?
C36 C31 C32 C33 0(2) . . . . ?
C30 C31 C32 C33 178.3(14) . . . . ?
C31 C32 C33 C34 1(2) . . . . ?
C32 C33 C34 C35 -1(3) . . . . ?
C33 C34 C35 C36 0(2) . . . . ?
C30 C31 C36 C35 -179.3(11) . . . . ?
C32 C31 C36 C35 -0.7(17) . . . . ?
C30 C31 C36 C27 -0.8(16) . . . . ?
C32 C31 C36 C27 177.8(10) . . . . ?
C34 C35 C36 C31 0.6(17) . . . . ?
C34 C35 C36 C27 -177.9(11) . . . . ?
C26 C27 C36 C31 171.7(10) . . . . ?
C28 C27 C36 C31 -3.1(15) . . . . ?
C26 C27 C36 C35 -9.8(15) . . . . ?
C28 C27 C36 C35 175.3(10) . . . . ?
Ni1 O7 C37 O8 14.4(13) . . . . ?
Ni1 O7 C37 C38 -159.3(6) . . . . ?
Ni3 O8 C37 O7 169.0(6) . . . . ?
Ni3 O8 C37 C38 -17.4(12) . . . . ?
O7 C37 C38 C39 16.3(14) . . . . ?
O8 C37 C38 C39 -157.6(10) . . . . ?
O7 C37 C38 C43 -165.2(10) . . . . ?
O8 C37 C38 C43 20.9(15) . . . . ?
C43 C38 C39 C40 -4.0(18) . . . . ?
C37 C38 C39 C40 174.6(11) . . . . ?
C38 C39 C40 C41 0(2) . . . . ?
C38 C39 C40 Cl3 -178.0(10) . . . . ?
C39 C40 C41 C42 2(2) . . . . ?
Cl3 C40 C41 C42 -179.8(12) . . . . ?
C40 C41 C42 C43 -1(2) . . . . ?
C39 C38 C43 N3 -175.7(10) . . . . ?
C37 C38 C43 N3 5.9(17) . . . . ?
C39 C38 C43 C42 5.2(17) . . . . ?
C37 C38 C43 C42 -173.2(10) . . . . ?
C44 N3 C43 C38 142.9(11) . . . . ?
Ni3 N3 C43 C38 -32.0(14) . . . . ?
C44 N3 C43 C42 -38.0(15) . . . . ?
Ni3 N3 C43 C42 147.1(9) . . . . ?
C41 C42 C43 C38 -3.0(19) . . . . ?
C41 C42 C43 N3 177.9(12) . . . . ?
C43 N3 C44 C45 174.6(10) . . . . ?
Ni3 N3 C44 C45 -10.5(15) . . . . ?
N3 C44 C45 C46 -18.2(17) . . . . ?
N3 C44 C45 C54 167.7(10) . . . . ?
Ni3 O9 C46 C45 29.2(13) . . . . ?
Ni3 O9 C46 C47 -150.5(7) . . . . ?
C44 C45 C46 O9 7.4(16) . . . . ?
C54 C45 C46 O9 -178.5(9) . . . . ?
C44 C45 C46 C47 -172.9(9) . . . . ?
C54 C45 C46 C47 1.2(15) . . . . ?
O9 C46 C47 C48 178.3(10) . . . . ?
C45 C46 C47 C48 -1.4(16) . . . . ?
C46 C47 C48 C49 1.6(17) . . . . ?
C47 C48 C49 C50 177.3(11) . . . . ?
C47 C48 C49 C54 -1.5(17) . . . . ?
C54 C49 C50 C51 0.6(18) . . . . ?
C48 C49 C50 C51 -178.2(11) . . . . ?
C49 C50 C51 C52 -2.1(19) . . . . ?
C50 C51 C52 C53 0.8(19) . . . . ?
C51 C52 C53 C54 2.0(18) . . . . ?
C52 C53 C54 C49 -3.4(16) . . . . ?
C52 C53 C54 C45 176.2(10) . . . . ?
C50 C49 C54 C53 2.1(15) . . . . ?
C48 C49 C54 C53 -179.1(10) . . . . ?
C50 C49 C54 C45 -177.5(10) . . . . ?
C48 C49 C54 C45 1.3(15) . . . . ?
C46 C45 C54 C53 179.2(10) . . . . ?
C44 C45 C54 C53 -6.6(16) . . . . ?
C46 C45 C54 C49 -1.2(15) . . . . ?
C44 C45 C54 C49 173.0(10) . . . . ?
Ni6 O10 C55 O11 -17.6(14) . . . . ?
Ni6 O10 C55 C56 160.0(6) . . . . ?
Ni4 O11 C55 O10 -179.2(7) . . . . ?
Ni4 O11 C55 C56 3.3(12) . . . . ?
O10 C55 C56 C57 -22.0(13) . . . . ?
O11 C55 C56 C57 155.7(9) . . . . ?
O10 C55 C56 C61 158.5(10) . . . . ?
O11 C55 C56 C61 -23.9(15) . . . . ?
C61 C56 C57 C58 2.9(16) . . . . ?
C55 C56 C57 C58 -176.7(10) . . . . ?
C56 C57 C58 C59 -0.1(17) . . . . ?
C56 C57 C58 Cl4 178.9(9) . . . . ?
C57 C58 C59 C60 -1.5(18) . . . . ?
Cl4 C58 C59 C60 179.5(9) . . . . ?
C58 C59 C60 C61 0.4(17) . . . . ?
C59 C60 C61 C56 2.4(17) . . . . ?
C59 C60 C61 N4 -179.9(10) . . . . ?
C57 C56 C61 C60 -4.0(16) . . . . ?
C55 C56 C61 C60 175.5(10) . . . . ?
C57 C56 C61 N4 178.2(10) . . . . ?
C55 C56 C61 N4 -2.3(16) . . . . ?
C62 N4 C61 C60 45.5(15) . . . . ?
Ni4 N4 C61 C60 -132.1(9) . . . . ?
C62 N4 C61 C56 -136.7(10) . . . . ?
Ni4 N4 C61 C56 45.6(13) . . . . ?
C61 N4 C62 C63 172.3(10) . . . . ?
Ni4 N4 C62 C63 -10.1(14) . . . . ?
N4 C62 C63 C64 -24.8(16) . . . . ?
N4 C62 C63 C72 160.3(10) . . . . ?
Ni4 O12 C64 C63 39.7(12) . . . . ?
Ni4 O12 C64 C65 -144.6(8) . . . . ?
C62 C63 C64 O12 6.9(16) . . . . ?
C72 C63 C64 O12 -178.2(9) . . . . ?
C62 C63 C64 C65 -168.7(10) . . . . ?
C72 C63 C64 C65 6.1(15) . . . . ?
O12 C64 C65 C66 179.5(10) . . . . ?
C63 C64 C65 C66 -4.6(16) . . . . ?
C64 C65 C66 C67 2.1(17) . . . . ?
C65 C66 C67 C68 177.9(11) . . . . ?
C65 C66 C67 C72 -1.3(16) . . . . ?
C72 C67 C68 C69 -1(2) . . . . ?
C66 C67 C68 C69 -179.9(14) . . . . ?
C67 C68 C69 C70 -4(2) . . . . ?
C68 C69 C70 C71 4(3) . . . . ?
C69 C70 C71 C72 -1(3) . . . . ?
C68 C67 C72 C71 3.7(17) . . . . ?
C66 C67 C72 C71 -177.0(11) . . . . ?
C68 C67 C72 C63 -176.2(11) . . . . ?
C66 C67 C72 C63 3.1(16) . . . . ?
C70 C71 C72 C67 -3(2) . . . . ?
C70 C71 C72 C63 177.1(14) . . . . ?
C64 C63 C72 C67 -5.6(15) . . . . ?
C62 C63 C72 C67 169.3(10) . . . . ?
C64 C63 C72 C71 174.5(11) . . . . ?
C62 C63 C72 C71 -10.6(17) . . . . ?
Ni3 O13 C73 O14 10.5(13) . . . . ?
Ni3 O13 C73 C74 -164.5(6) . . . . ?
Ni5 O14 C73 O13 171.3(6) . . . . ?
Ni5 O14 C73 C74 -13.8(12) . . . . ?
O13 C73 C74 C75 15.5(12) . . . . ?
O14 C73 C74 C75 -159.6(8) . . . . ?
O13 C73 C74 C79 -168.5(9) . . . . ?
O14 C73 C74 C79 16.4(14) . . . . ?
C79 C74 C75 C76 -2.8(14) . . . . ?
C73 C74 C75 C76 173.6(8) . . . . ?
C74 C75 C76 C77 -1.0(15) . . . . ?
C74 C75 C76 Cl5 -179.7(7) . . . . ?
C75 C76 C77 C78 1.9(15) . . . . ?
Cl5 C76 C77 C78 -179.4(8) . . . . ?
C76 C77 C78 C79 1.0(15) . . . . ?
C80 N5 C79 C78 -36.8(13) . . . . ?
Ni5 N5 C79 C78 146.9(7) . . . . ?
C80 N5 C79 C74 144.2(9) . . . . ?
Ni5 N5 C79 C74 -32.2(12) . . . . ?
C77 C78 C79 N5 176.2(9) . . . . ?
C77 C78 C79 C74 -4.8(14) . . . . ?
C75 C74 C79 N5 -175.5(8) . . . . ?
C73 C74 C79 N5 8.6(15) . . . . ?
C75 C74 C79 C78 5.5(13) . . . . ?
C73 C74 C79 C78 -170.4(9) . . . . ?
C79 N5 C80 C81 175.4(9) . . . . ?
Ni5 N5 C80 C81 -8.2(14) . . . . ?
N5 C80 C81 C82 -21.0(16) . . . . ?
N5 C80 C81 C90 161.2(10) . . . . ?
Ni5 O15 C82 C81 29.5(13) . . . . ?
Ni5 O15 C82 C83 -146.8(7) . . . . ?
C80 C81 C82 O15 8.3(16) . . . . ?
C90 C81 C82 O15 -173.9(9) . . . . ?
C80 C81 C82 C83 -175.4(9) . . . . ?
C90 C81 C82 C83 2.4(15) . . . . ?
O15 C82 C83 C84 177.6(10) . . . . ?
C81 C82 C83 C84 1.0(16) . . . . ?
C82 C83 C84 C85 -4.9(17) . . . . ?
C83 C84 C85 C90 5.3(17) . . . . ?
C83 C84 C85 C86 -172.7(10) . . . . ?
C84 C85 C86 C87 176.4(11) . . . . ?
C90 C85 C86 C87 -1.7(16) . . . . ?
C85 C86 C87 C88 1.7(18) . . . . ?
C86 C87 C88 C89 -0.8(18) . . . . ?
C87 C88 C89 C90 0.0(16) . . . . ?
C88 C89 C90 C85 -0.1(17) . . . . ?
C88 C89 C90 C81 -175.3(10) . . . . ?
C84 C85 C90 C89 -177.2(11) . . . . ?
C86 C85 C90 C89 0.9(16) . . . . ?
C84 C85 C90 C81 -1.8(16) . . . . ?
C86 C85 C90 C81 176.3(9) . . . . ?
C82 C81 C90 C89 173.4(10) . . . . ?
C80 C81 C90 C89 -8.8(16) . . . . ?
C82 C81 C90 C85 -2.0(15) . . . . ?
C80 C81 C90 C85 175.9(9) . . . . ?
Ni6 O17 C91 O16 177.6(7) . . . . ?
Ni6 O17 C91 C92 -0.1(13) . . . . ?
Ni2 O16 C91 O17 -13.4(14) . . . . ?
Ni2 O16 C91 C92 164.4(6) . . . . ?
O17 C91 C92 C93 155.5(10) . . . . ?
O16 C91 C92 C93 -22.4(14) . . . . ?
O17 C91 C92 C97 -26.8(15) . . . . ?
O16 C91 C92 C97 155.3(10) . . . . ?
C97 C92 C93 C94 -1.9(15) . . . . ?
C91 C92 C93 C94 175.8(9) . . . . ?
C92 C93 C94 C95 3.3(16) . . . . ?
C92 C93 C94 Cl6 -174.7(8) . . . . ?
C93 C94 C95 C96 -3.2(16) . . . . ?
Cl6 C94 C95 C96 174.8(8) . . . . ?
C94 C95 C96 C97 1.7(16) . . . . ?
C93 C92 C97 C96 0.5(16) . . . . ?
C91 C92 C97 C96 -177.2(9) . . . . ?
C93 C92 C97 N6 177.5(9) . . . . ?
C91 C92 C97 N6 -0.1(16) . . . . ?
C95 C96 C97 C92 -0.4(16) . . . . ?
C95 C96 C97 N6 -177.4(10) . . . . ?
C98 N6 C97 C92 -122.5(12) . . . . ?
Ni6 N6 C97 C92 47.7(12) . . . . ?
C98 N6 C97 C96 54.5(15) . . . . ?
Ni6 N6 C97 C96 -135.3(9) . . . . ?
C97 N6 C98 C99 171.1(12) . . . . ?
Ni6 N6 C98 C99 2.1(19) . . . . ?
N6 C98 C99 C100 -21(2) . . . . ?
N6 C98 C99 C108 169.3(13) . . . . ?
Ni6 O18 C100 C99 30.6(18) . . . . ?
Ni6 O18 C100 C101 -154.1(9) . . . . ?
C98 C99 C100 O18 4(2) . . . . ?
C108 C99 C100 O18 173.3(13) . . . . ?
C98 C99 C100 C101 -171.6(13) . . . . ?
C108 C99 C100 C101 -2(2) . . . . ?
O18 C100 C101 C102 -173.5(13) . . . . ?
C99 C100 C101 C102 2(2) . . . . ?
C100 C101 C102 C103 -1(2) . . . . ?
C101 C102 C103 C108 0(2) . . . . ?
C101 C102 C103 C104 176.6(15) . . . . ?
C108 C103 C104 C105 -11(2) . . . . ?
C102 C103 C104 C105 172.1(15) . . . . ?
C103 C104 C105 C106 16(2) . . . . ?
C104 C105 C106 C107 -19(3) . . . . ?
C105 C106 C107 C108 15(3) . . . . ?
C102 C103 C108 C107 -176.1(15) . . . . ?
C104 C103 C108 C107 7(2) . . . . ?
C102 C103 C108 C99 0(2) . . . . ?
C104 C103 C108 C99 -176.5(14) . . . . ?
C106 C107 C108 C103 -9(2) . . . . ?
C106 C107 C108 C99 174.7(15) . . . . ?
C100 C99 C108 C103 1(2) . . . . ?
C98 C99 C108 C103 170.6(14) . . . . ?
C100 C99 C108 C107 177.0(14) . . . . ?
C98 C99 C108 C107 -13(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W O8 0.85 1.87 2.672(8) 156.1 .
O1W H2W O16 0.85 2.53 2.988(8) 114.5 .
O1W H2W O17 0.85 1.78 2.607(9) 163.9 .
O3W H3W O2 0.86 1.86 2.659(8) 153.0 .
O3W H4W O11 0.88 1.78 2.609(8) 156.6 .
O2W H5W O14 0.88 1.94 2.685(8) 141.7 .
O2W H6W O5 0.87 1.79 2.623(8) 159.5 .
O19 H19 O18 0.84 1.95 2.739(10) 155.0 .
O20 H20 O3 0.84 1.81 2.645(8) 171.7 .
O21 H21A O6 0.84 1.95 2.719(9) 152.1 .
O22 H22 O9 0.84 1.81 2.653(10) 176.1 .
O23 H23 O12 0.84 1.90 2.716(10) 163.3 .
O24 H24 O15 0.84 1.80 2.616(10) 165.2 .

_refine_diff_density_max         1.017
_refine_diff_density_min         -1.731
_refine_diff_density_rms         0.119



