# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_added_by_encifer
_database_code_depnum_ccdc_archive 'CCDC 1418422'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2015-12-08 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            'C46 H71 Cl4 N13 Ni2 O13'
_chemical_formula_weight         1273.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.3126(2)
_cell_length_b                   20.4330(3)
_cell_length_c                   23.8954(5)
_cell_angle_alpha                90
_cell_angle_beta                 99.7407(18)
_cell_angle_gamma                90
_cell_volume                     5925.02(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    12011
_cell_measurement_theta_min      4.250
_cell_measurement_theta_max      75.230

_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_F_000             2664
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    3.029
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23826
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.642
_diffrn_reflns_theta_max         76.371
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             12011
_reflns_number_gt                10646
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_solution    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (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)+(0.0920P)²+8.5053P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12011
_refine_ls_number_parameters     727
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0561
_refine_ls_wR_factor_ref         0.1653
_refine_ls_wR_factor_gt          0.1591
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_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 0.01099(4) 0.65925(2) 0.22055(2) 0.01635(12) Uani 1 1 d . . . . .
Ni2 Ni 0.38578(4) 0.83838(2) 0.17416(2) 0.01797(12) Uani 1 1 d . . . . .
Cl3 Cl 0.91170(5) 0.90199(3) 0.28960(3) 0.02523(15) Uani 1 1 d . . . . .
Cl4 Cl 0.19491(6) 0.84600(4) 0.16343(3) 0.03117(17) Uani 1 1 d . . . . .
Cl5 Cl 0.25877(7) 0.53260(4) 0.44377(3) 0.03660(19) Uani 1 1 d . . . . .
Cl6 Cl 0.66247(12) 0.71484(8) 0.05351(6) 0.0271(3) Uani 0.7 1 d . . P . .
O1 O 0.14738(16) 0.70629(10) 0.20240(9) 0.0251(4) Uani 1 1 d . . . . .
H1A H 0.2001 0.7038 0.2308 0.038 Uiso 1 1 d R U . . .
H1B H 0.1325 0.7467 0.1952 0.038 Uiso 1 1 d R U . . .
N2 N -0.12715(18) 0.60893(11) 0.23577(10) 0.0195(4) Uani 1 1 d . . . . .
N3 N 0.50590(19) 0.90253(11) 0.15677(10) 0.0215(5) Uani 1 1 d . . . . .
N4 N 0.51732(18) 0.77440(11) 0.19808(9) 0.0190(4) Uani 1 1 d . . . . .
H4 H 0.5248 0.7481 0.1637 0.023 Uiso 1 1 calc R U . . .
N5 N 0.09833(17) 0.57539(10) 0.25540(9) 0.0170(4) Uani 1 1 d . . . . .
H5 H 0.0960 0.5428 0.2240 0.020 Uiso 1 1 calc R U . . .
N6 N -0.00182(18) 0.70716(11) 0.30184(9) 0.0194(4) Uani 1 1 d . . . . .
H6 H -0.0205 0.7534 0.2904 0.023 Uiso 1 1 calc R U . . .
N7 N -0.03827(18) 0.62192(11) 0.13597(9) 0.0191(4) Uani 1 1 d . . . . .
H7 H -0.0825 0.6582 0.1152 0.023 Uiso 1 1 calc R U . . .
N8 N 0.39864(19) 0.89280(11) 0.25125(10) 0.0217(5) Uani 1 1 d . . . . .
H8 H 0.4684 0.8799 0.2766 0.026 Uiso 1 1 calc R U . . .
C9 C 0.0779(2) 0.66404(13) 0.06914(11) 0.0208(5) Uani 1 1 d . . . . .
C10 C 0.4438(2) 0.66822(13) 0.22893(11) 0.0188(5) Uani 1 1 d . . . . .
C11 C 0.2982(2) 0.59574(13) 0.24872(11) 0.0197(5) Uani 1 1 d . . . . .
C12 C 0.1889(2) 0.74642(13) 0.35064(11) 0.0199(5) Uani 1 1 d . . . . .
C13 C 0.3648(2) 0.65094(13) 0.26157(11) 0.0191(5) Uani 1 1 d . . . . .
H13 H 0.3560 0.6772 0.2933 0.023 Uiso 1 1 calc R U . . .
N14 N 0.35760(18) 0.82445(11) 0.08404(9) 0.0200(4) Uani 1 1 d . . . . .
H14 H 0.2864 0.8478 0.0710 0.024 Uiso 1 1 calc R U . . .
C15 C 0.3001(2) 0.83303(13) 0.31948(12) 0.0228(5) Uani 1 1 d . . . . .
O16 O 0.9001(2) 0.83928(11) 0.31483(12) 0.0441(6) Uani 1 1 d . . . . .
C17 C 0.1401(2) 0.77579(14) 0.01486(11) 0.0229(5) Uani 1 1 d . . . . .
H17 H 0.1609 0.8137 -0.0038 0.027 Uiso 1 1 calc R U . . .
C18 C 0.0798(2) 0.71454(13) 0.35472(11) 0.0217(5) Uani 1 1 d . . . . .
H18A H 0.0952 0.6704 0.3713 0.026 Uiso 1 1 calc R U . . .
H18B H 0.0447 0.7402 0.3819 0.026 Uiso 1 1 calc R U . . .
C19 C 0.3130(2) 0.55675(13) 0.20290(12) 0.0221(5) Uani 1 1 d . . . . .
H19 H 0.2685 0.5190 0.1937 0.027 Uiso 1 1 calc R U . . .
O20 O 0.7416(2) 0.66531(16) 0.05455(11) 0.0498(7) Uani 1 1 d . . . . .
C21 C -0.1204(2) 0.56923(14) 0.13971(12) 0.0223(5) Uani 1 1 d . . . . .
H21A H -0.0825 0.5283 0.1541 0.027 Uiso 1 1 calc R U . . .
H21B H -0.1642 0.5605 0.1018 0.027 Uiso 1 1 calc R U . . .
O22 O 1.0091(2) 0.90270(13) 0.26415(14) 0.0485(7) Uani 1 1 d . . . . .
C23 C -0.0919(2) 0.54767(13) 0.26794(12) 0.0208(5) Uani 1 1 d . . . . .
H23A H -0.1045 0.5099 0.2417 0.025 Uiso 1 1 calc R U . . .
H23B H -0.1378 0.5414 0.2977 0.025 Uiso 1 1 calc R U . . .
N24 N -0.0740(2) 0.74645(12) 0.18461(11) 0.0288(5) Uani 1 1 d . . . . .
C25 C 0.4582(2) 0.62834(14) 0.18346(12) 0.0235(5) Uani 1 1 d . . . . .
H25 H 0.5128 0.6390 0.1612 0.028 Uiso 1 1 calc R U . . .
C26 C 0.2145(2) 0.57821(13) 0.28596(11) 0.0203(5) Uani 1 1 d . . . . .
H26A H 0.2342 0.5351 0.3037 0.024 Uiso 1 1 calc R U . . .
H26B H 0.2191 0.6109 0.3169 0.024 Uiso 1 1 calc R U . . .
C27 C 0.2204(2) 0.73852(13) 0.04892(11) 0.0196(5) Uani 1 1 d . . . . .
O28 O 0.8176(2) 0.91633(13) 0.24738(11) 0.0404(6) Uani 1 1 d . . . . .
C29 C 0.5167(2) 0.72698(13) 0.24540(11) 0.0200(5) Uani 1 1 d . . . . .
H29A H 0.4914 0.7497 0.2774 0.024 Uiso 1 1 calc R U . . .
H29B H 0.5930 0.7117 0.2588 0.024 Uiso 1 1 calc R U . . .
N30 N 0.3779(2) 0.40003(15) 0.15729(12) 0.0362(6) Uani 1 1 d . . . . .
C31 C 0.3931(2) 0.57304(14) 0.17051(12) 0.0240(5) Uani 1 1 d . . . . .
H31 H 0.4033 0.5462 0.1394 0.029 Uiso 1 1 calc R U . . .
O32 O 0.6170(3) 0.71488(17) 0.10517(13) 0.0573(8) Uani 1 1 d . . . . .
O33 O 0.9197(2) 0.95221(11) 0.33271(11) 0.0391(5) Uani 1 1 d . . . . .
C34 C 0.5140(2) 0.95795(14) 0.19811(12) 0.0248(6) Uani 1 1 d . . . . .
H34A H 0.5189 0.9998 0.1778 0.030 Uiso 1 1 calc R U . . .
H34B H 0.5818 0.9531 0.2267 0.030 Uiso 1 1 calc R U . . .
C35 C 0.2003(2) 0.79962(13) 0.31505(11) 0.0214(5) Uani 1 1 d . . . . .
H35 H 0.1393 0.8131 0.2876 0.026 Uiso 1 1 calc R U . . .
C36 C -0.1842(2) 0.65538(14) 0.26848(13) 0.0239(6) Uani 1 1 d . . . . .
H36A H -0.2460 0.6328 0.2820 0.029 Uiso 1 1 calc R U . . .
H36B H -0.2150 0.6919 0.2435 0.029 Uiso 1 1 calc R U . . .
C37 C 0.2802(2) 0.72591(14) 0.38927(11) 0.0241(5) Uani 1 1 d . . . . .
H37 H 0.2741 0.6891 0.4128 0.029 Uiso 1 1 calc R U . . .
C38 C -0.0006(2) 0.70198(15) 0.03486(12) 0.0251(6) Uani 1 1 d . . . . .
H38 H -0.0760 0.6896 0.0297 0.030 Uiso 1 1 calc R U . . .
C39 C 0.0301(2) 0.75762(15) 0.00811(12) 0.0260(6) Uani 1 1 d . . . . .
H39 H -0.0243 0.7833 -0.0149 0.031 Uiso 1 1 calc R U . . .
C40 C 0.1885(2) 0.68291(13) 0.07595(11) 0.0198(5) Uani 1 1 d . . . . .
H40 H 0.2428 0.6575 0.0993 0.024 Uiso 1 1 calc R U . . .
C41 C -0.0863(3) 0.79236(17) 0.15783(15) 0.0351(7) Uani 1 1 d . . . . .
C42 C -0.1058(2) 0.68222(14) 0.31874(12) 0.0234(5) Uani 1 1 d . . . . .
H42A H -0.1422 0.7182 0.3362 0.028 Uiso 1 1 calc R U . . .
H42B H -0.0876 0.6473 0.3475 0.028 Uiso 1 1 calc R U . . .
C43 C 0.6124(2) 0.86645(14) 0.16329(12) 0.0242(5) Uani 1 1 d . . . . .
H43A H 0.6745 0.8975 0.1724 0.029 Uiso 1 1 calc R U . . .
H43B H 0.6191 0.8440 0.1273 0.029 Uiso 1 1 calc R U . . .
C44 C 0.0426(2) 0.60404(14) 0.09857(12) 0.0234(5) Uani 1 1 d . . . . .
H44A H 0.0089 0.5719 0.0698 0.028 Uiso 1 1 calc R U . . .
H44B H 0.1080 0.5834 0.1216 0.028 Uiso 1 1 calc R U . . .
C45 C -0.1947(2) 0.59263(14) 0.17997(12) 0.0229(5) Uani 1 1 d . . . . .
H45A H -0.2361 0.6318 0.1640 0.028 Uiso 1 1 calc R U . . .
H45B H -0.2485 0.5580 0.1849 0.028 Uiso 1 1 calc R U . . .
C46 C 0.3894(2) 0.81273(15) 0.35946(13) 0.0279(6) Uani 1 1 d . . . . .
H46 H 0.4572 0.8359 0.3634 0.033 Uiso 1 1 calc R U . . .
C47 C 0.4394(2) 0.86415(14) 0.05963(12) 0.0243(6) Uani 1 1 d . . . . .
H47A H 0.4076 0.8781 0.0206 0.029 Uiso 1 1 calc R U . . .
H47B H 0.5061 0.8377 0.0578 0.029 Uiso 1 1 calc R U . . .
C48 C 0.3397(2) 0.75905(14) 0.05619(12) 0.0226(5) Uani 1 1 d . . . . .
H48A H 0.3859 0.7261 0.0795 0.027 Uiso 1 1 calc R U . . .
H48B H 0.3630 0.7607 0.0185 0.027 Uiso 1 1 calc R U . . .
C49 C 0.3086(3) 0.89454(14) 0.28559(13) 0.0278(6) Uani 1 1 d . . . . .
H49A H 0.2377 0.9017 0.2599 0.033 Uiso 1 1 calc R U . . .
H49B H 0.3208 0.9322 0.3120 0.033 Uiso 1 1 calc R U . . .
C50 C 0.6167(2) 0.81686(14) 0.21031(12) 0.0228(5) Uani 1 1 d . . . . .
H50A H 0.6841 0.7899 0.2127 0.027 Uiso 1 1 calc R U . . .
H50B H 0.6185 0.8395 0.2471 0.027 Uiso 1 1 calc R U . . .
C51 C 0.4142(2) 0.95926(13) 0.22780(13) 0.0242(5) Uani 1 1 d . . . . .
H51A H 0.4255 0.9918 0.2589 0.029 Uiso 1 1 calc R U . . .
H51B H 0.3478 0.9719 0.2005 0.029 Uiso 1 1 calc R U . . .
O52 O 0.3492(3) 0.56382(15) 0.42302(13) 0.0519(7) Uani 1 1 d . . . . .
C53 C 0.4699(2) 0.92395(14) 0.09697(12) 0.0251(6) Uani 1 1 d . . . . .
H53A H 0.5302 0.9483 0.0836 0.030 Uiso 1 1 calc R U . . .
H53B H 0.4055 0.9534 0.0946 0.030 Uiso 1 1 calc R U . . .
O54 O 0.2301(3) 0.47434(15) 0.41279(17) 0.0703(10) Uani 1 1 d . . . . .
C55 C 0.0288(2) 0.54905(12) 0.29549(11) 0.0193(5) Uani 1 1 d . . . . .
H55A H 0.0377 0.5767 0.3300 0.023 Uiso 1 1 calc R U . . .
H55B H 0.0533 0.5042 0.3071 0.023 Uiso 1 1 calc R U . . .
C56 C 0.3082(3) 0.39023(16) 0.12132(14) 0.0323(7) Uani 1 1 d . . . . .
C57 C -0.0996(4) 0.8521(2) 0.1242(2) 0.0586(12) Uani 1 1 d . . . . .
H57A H -0.1653 0.8484 0.0947 0.088 Uiso 1 1 calc R U . . .
H57B H -0.0345 0.8588 0.1062 0.088 Uiso 1 1 calc R U . . .
H57C H -0.1081 0.8894 0.1488 0.088 Uiso 1 1 calc R U . . .
O58 O 0.1657(3) 0.57603(15) 0.43468(15) 0.0626(9) Uani 1 1 d . . . . .
C59 C 0.3799(3) 0.75867(16) 0.39374(13) 0.0290(6) Uani 1 1 d . . . . .
H59 H 0.4416 0.7442 0.4202 0.035 Uiso 1 1 calc R U . . .
O60 O 0.5845(3) 0.7169(2) 0.00527(15) 0.0797(12) Uani 1 1 d . . . . .
O61 O 0.2853(4) 0.5198(2) 0.50274(15) 0.0928(16) Uani 1 1 d . . . . .
C62 C 0.2177(3) 0.3758(3) 0.07536(16) 0.0517(10) Uani 1 1 d . . . . .
H62A H 0.2467 0.3549 0.0440 0.078 Uiso 1 1 calc R U . . .
H62B H 0.1802 0.4166 0.0620 0.078 Uiso 1 1 calc R U . . .
H62C H 0.1654 0.3463 0.0892 0.078 Uiso 1 1 calc R U . . .
O78 O 0.7214(4) 0.7757(2) 0.0560(2) 0.0658(13) Uani 0.7 1 d . . P . .
C66 C 0.0930(5) 0.0500(3) 0.0584(2) 0.0676(13) Uani 1 1 d . . . . .
N71 N 0.1056(5) 0.1048(3) 0.0488(3) 0.0965(18) Uani 1 1 d . . . . .
C98 C 0.0754(6) -0.0195(3) 0.0715(2) 0.0733(15) Uani 1 1 d . . . . .
H98A H 0.0739 -0.0459 0.0371 0.110 Uiso 1 1 calc R U . . .
H98B H 0.0051 -0.0241 0.0852 0.110 Uiso 1 1 calc R U . . .
H98C H 0.1355 -0.0345 0.1009 0.110 Uiso 1 1 calc R U . . .
Cl1 Cl 0.6386(3) 0.6905(2) 0.05788(16) 0.0293(7) Uani 0.3 1 d . . P . .
C2 C 0.3652(5) 0.1045(2) 0.1049(2) 0.0654(14) Uani 1 1 d . . . . .
C3 C 0.1476(5) 0.8921(2) 0.43311(18) 0.0571(11) Uani 1 1 d . . . . .
H3A H 0.2032 0.8930 0.4082 0.086 Uiso 1 1 calc R U . . .
H3B H 0.0747 0.9006 0.4107 0.086 Uiso 1 1 calc R U . . .
H3C H 0.1477 0.8490 0.4511 0.086 Uiso 1 1 calc R U . . .
C4 C 0.3842(4) 0.1227(3) 0.0505(2) 0.0604(12) Uani 1 1 d . . . . .
H4A H 0.3339 0.0985 0.0216 0.091 Uiso 1 1 calc R U . . .
H4B H 0.4606 0.1125 0.0470 0.091 Uiso 1 1 calc R U . . .
H4C H 0.3714 0.1698 0.0451 0.091 Uiso 1 1 calc R U . . .
C5 C 0.1727(8) 0.9412(2) 0.4758(3) 0.106(3) Uani 1 1 d . . . . .
N1AA N 0.3551(7) 0.0900(3) 0.1494(3) 0.127(3) Uani 1 1 d . . . . .
N0AA N 0.1856(13) 0.9799(3) 0.5084(3) 0.237(8) Uani 1 1 d . . . . .
O11 O 0.5831(14) 0.6298(7) 0.0595(6) 0.092(5) Uani 0.3 1 d . . 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 O1 2.044(2) . ?
Ni1 N2 2.072(2) . ?
Ni1 N5 2.117(2) . ?
Ni1 N7 2.149(2) . ?
Ni1 N24 2.169(2) . ?
Ni1 N6 2.205(2) . ?
Ni2 N3 2.070(2) . ?
Ni2 N4 2.085(2) . ?
Ni2 N8 2.135(2) . ?
Ni2 N14 2.141(2) . ?
Ni2 Cl4 2.3257(8) . ?
Cl3 O28 1.432(2) . ?
Cl3 O22 1.434(3) . ?
Cl3 O16 1.434(2) . ?
Cl3 O33 1.445(2) . ?
Cl5 O54 1.415(3) . ?
Cl5 O61 1.416(3) . ?
Cl5 O58 1.437(3) . ?
Cl5 O52 1.442(3) . ?
Cl6 Cl1 0.596(3) . ?
Cl6 O60 1.370(3) . ?
Cl6 O20 1.403(3) . ?
Cl6 O78 1.437(5) . ?
Cl6 O32 1.439(3) . ?
Cl6 O11 2.010(12) . ?
O1 H1A 0.8578 . ?
O1 H1B 0.8576 . ?
N2 C36 1.480(3) . ?
N2 C45 1.485(3) . ?
N2 C23 1.495(3) . ?
N3 C53 1.488(3) . ?
N3 C43 1.490(4) . ?
N3 C34 1.495(4) . ?
N4 C50 1.488(3) . ?
N4 C29 1.490(3) . ?
N4 H4 1.0000 . ?
N5 C55 1.489(3) . ?
N5 C26 1.493(3) . ?
N5 H5 1.0000 . ?
N6 C18 1.483(3) . ?
N6 C42 1.495(3) . ?
N6 H6 1.0000 . ?
N7 C21 1.490(3) . ?
N7 C44 1.492(3) . ?
N7 H7 1.0000 . ?
N8 C49 1.487(4) . ?
N8 C51 1.494(3) . ?
N8 H8 1.0000 . ?
C9 C38 1.392(4) . ?
C9 C40 1.398(4) . ?
C9 C44 1.513(4) . ?
C10 C13 1.391(4) . ?
C10 C25 1.393(4) . ?
C10 C29 1.511(4) . ?
C11 C19 1.391(4) . ?
C11 C13 1.398(4) . ?
C11 C26 1.514(4) . ?
C12 C37 1.393(4) . ?
C12 C35 1.402(4) . ?
C12 C18 1.511(4) . ?
C13 H13 0.9500 . ?
N14 C47 1.487(3) . ?
N14 C48 1.493(3) . ?
N14 H14 1.0000 . ?
C15 C46 1.393(4) . ?
C15 C35 1.394(4) . ?
C15 C49 1.508(4) . ?
C17 C39 1.387(4) . ?
C17 C27 1.395(4) . ?
C17 H17 0.9500 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C31 1.393(4) . ?
C19 H19 0.9500 . ?
O20 Cl1 1.384(4) . ?
C21 C45 1.513(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C23 C55 1.519(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
N24 C41 1.131(4) . ?
C25 C31 1.390(4) . ?
C25 H25 0.9500 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C40 1.396(4) . ?
C27 C48 1.510(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
N30 C56 1.125(4) . ?
C31 H31 0.9500 . ?
O32 Cl1 1.303(5) . ?
C34 C51 1.520(4) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35 0.9500 . ?
C36 C42 1.511(4) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C59 1.386(4) . ?
C37 H37 0.9500 . ?
C38 C39 1.388(4) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 C57 1.457(5) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C50 1.507(4) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C59 1.392(4) . ?
C46 H46 0.9500 . ?
C47 C53 1.522(4) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 C62 1.456(5) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C59 H59 0.9500 . ?
O60 Cl1 1.426(5) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
O78 Cl1 2.023(6) . ?
C66 N71 1.158(8) . ?
C66 C98 1.477(8) . ?
C98 H98A 0.9800 . ?
C98 H98B 0.9800 . ?
C98 H98C 0.9800 . ?
Cl1 O11 1.419(12) . ?
C2 N1AA 1.132(7) . ?
C2 C4 1.408(6) . ?
C3 C5 1.427(8) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 N0AA 1.102(8) . ?

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 N2 177.42(9) . . ?
O1 Ni1 N5 94.77(8) . . ?
N2 Ni1 N5 84.65(9) . . ?
O1 Ni1 N7 94.51(8) . . ?
N2 Ni1 N7 83.08(9) . . ?
N5 Ni1 N7 97.27(8) . . ?
O1 Ni1 N24 83.59(10) . . ?
N2 Ni1 N24 96.99(10) . . ?
N5 Ni1 N24 178.36(10) . . ?
N7 Ni1 N24 83.03(9) . . ?
O1 Ni1 N6 99.32(8) . . ?
N2 Ni1 N6 83.25(9) . . ?
N5 Ni1 N6 96.89(8) . . ?
N7 Ni1 N6 159.27(9) . . ?
N24 Ni1 N6 83.25(9) . . ?
N3 Ni2 N4 84.48(9) . . ?
N3 Ni2 N8 83.81(9) . . ?
N4 Ni2 N8 98.58(9) . . ?
N3 Ni2 N14 83.22(9) . . ?
N4 Ni2 N14 100.29(9) . . ?
N8 Ni2 N14 155.90(9) . . ?
N3 Ni2 Cl4 132.71(7) . . ?
N4 Ni2 Cl4 142.74(7) . . ?
N8 Ni2 Cl4 89.22(7) . . ?
N14 Ni2 Cl4 84.79(6) . . ?
O28 Cl3 O22 109.55(17) . . ?
O28 Cl3 O16 110.66(17) . . ?
O22 Cl3 O16 109.71(15) . . ?
O28 Cl3 O33 107.84(15) . . ?
O22 Cl3 O33 109.52(18) . . ?
O16 Cl3 O33 109.54(16) . . ?
O54 Cl5 O61 111.1(2) . . ?
O54 Cl5 O58 108.5(2) . . ?
O61 Cl5 O58 108.0(3) . . ?
O54 Cl5 O52 109.4(2) . . ?
O61 Cl5 O52 111.2(2) . . ?
O58 Cl5 O52 108.50(19) . . ?
Cl1 Cl6 O60 83.0(5) . . ?
Cl1 Cl6 O20 75.9(5) . . ?
O60 Cl6 O20 115.0(2) . . ?
Cl1 Cl6 O78 167.6(6) . . ?
O60 Cl6 O78 106.5(3) . . ?
O20 Cl6 O78 106.2(3) . . ?
Cl1 Cl6 O32 64.9(5) . . ?
O60 Cl6 O32 113.8(2) . . ?
O20 Cl6 O32 110.80(19) . . ?
O78 Cl6 O32 103.4(3) . . ?
Cl1 Cl6 O11 6.3(6) . . ?
O60 Cl6 O11 78.9(6) . . ?
O20 Cl6 O11 73.8(5) . . ?
O78 Cl6 O11 173.7(5) . . ?
O32 Cl6 O11 71.0(4) . . ?
Ni1 O1 H1A 110.0 . . ?
Ni1 O1 H1B 109.9 . . ?
H1A O1 H1B 108.9 . . ?
C36 N2 C45 112.0(2) . . ?
C36 N2 C23 112.8(2) . . ?
C45 N2 C23 110.1(2) . . ?
C36 N2 Ni1 104.57(16) . . ?
C45 N2 Ni1 107.78(16) . . ?
C23 N2 Ni1 109.27(15) . . ?
C53 N3 C43 111.1(2) . . ?
C53 N3 C34 112.8(2) . . ?
C43 N3 C34 110.3(2) . . ?
C53 N3 Ni2 105.79(16) . . ?
C43 N3 Ni2 108.16(16) . . ?
C34 N3 Ni2 108.48(16) . . ?
C50 N4 C29 109.8(2) . . ?
C50 N4 Ni2 105.26(16) . . ?
C29 N4 Ni2 120.85(16) . . ?
C50 N4 H4 106.7 . . ?
C29 N4 H4 106.7 . . ?
Ni2 N4 H4 106.7 . . ?
C55 N5 C26 107.89(19) . . ?
C55 N5 Ni1 103.67(15) . . ?
C26 N5 Ni1 122.82(16) . . ?
C55 N5 H5 107.2 . . ?
C26 N5 H5 107.2 . . ?
Ni1 N5 H5 107.2 . . ?
C18 N6 C42 107.0(2) . . ?
C18 N6 Ni1 131.07(17) . . ?
C42 N6 Ni1 106.18(16) . . ?
C18 N6 H6 103.1 . . ?
C42 N6 H6 103.1 . . ?
Ni1 N6 H6 103.1 . . ?
C21 N7 C44 112.8(2) . . ?
C21 N7 Ni1 106.64(16) . . ?
C44 N7 Ni1 122.64(17) . . ?
C21 N7 H7 104.3 . . ?
C44 N7 H7 104.3 . . ?
Ni1 N7 H7 104.3 . . ?
C49 N8 C51 109.9(2) . . ?
C49 N8 Ni2 122.35(18) . . ?
C51 N8 Ni2 98.35(16) . . ?
C49 N8 H8 108.4 . . ?
C51 N8 H8 108.4 . . ?
Ni2 N8 H8 108.4 . . ?
C38 C9 C40 118.7(3) . . ?
C38 C9 C44 119.9(2) . . ?
C40 C9 C44 121.3(2) . . ?
C13 C10 C25 118.8(2) . . ?
C13 C10 C29 119.8(2) . . ?
C25 C10 C29 121.3(2) . . ?
C19 C11 C13 119.0(2) . . ?
C19 C11 C26 121.3(2) . . ?
C13 C11 C26 119.6(2) . . ?
C37 C12 C35 118.9(3) . . ?
C37 C12 C18 117.0(2) . . ?
C35 C12 C18 123.7(2) . . ?
C10 C13 C11 121.4(2) . . ?
C10 C13 H13 119.3 . . ?
C11 C13 H13 119.3 . . ?
C47 N14 C48 111.8(2) . . ?
C47 N14 Ni2 108.46(17) . . ?
C48 N14 Ni2 123.64(17) . . ?
C47 N14 H14 103.5 . . ?
C48 N14 H14 103.5 . . ?
Ni2 N14 H14 103.5 . . ?
C46 C15 C35 119.3(3) . . ?
C46 C15 C49 119.9(3) . . ?
C35 C15 C49 120.5(3) . . ?
C39 C17 C27 120.2(3) . . ?
C39 C17 H17 119.9 . . ?
C27 C17 H17 119.9 . . ?
N6 C18 C12 118.1(2) . . ?
N6 C18 H18A 107.8 . . ?
C12 C18 H18A 107.8 . . ?
N6 C18 H18B 107.8 . . ?
C12 C18 H18B 107.8 . . ?
H18A C18 H18B 107.1 . . ?
C11 C19 C31 120.0(3) . . ?
C11 C19 H19 120.0 . . ?
C31 C19 H19 120.0 . . ?
Cl1 O20 Cl6 24.70(14) . . ?
N7 C21 C45 107.4(2) . . ?
N7 C21 H21A 110.2 . . ?
C45 C21 H21A 110.2 . . ?
N7 C21 H21B 110.2 . . ?
C45 C21 H21B 110.2 . . ?
H21A C21 H21B 108.5 . . ?
N2 C23 C55 112.7(2) . . ?
N2 C23 H23A 109.1 . . ?
C55 C23 H23A 109.1 . . ?
N2 C23 H23B 109.1 . . ?
C55 C23 H23B 109.1 . . ?
H23A C23 H23B 107.8 . . ?
C41 N24 Ni1 156.2(3) . . ?
C31 C25 C10 120.3(2) . . ?
C31 C25 H25 119.9 . . ?
C10 C25 H25 119.9 . . ?
N5 C26 C11 114.4(2) . . ?
N5 C26 H26A 108.7 . . ?
C11 C26 H26A 108.7 . . ?
N5 C26 H26B 108.7 . . ?
C11 C26 H26B 108.7 . . ?
H26A C26 H26B 107.6 . . ?
C17 C27 C40 119.2(2) . . ?
C17 C27 C48 119.7(2) . . ?
C40 C27 C48 121.2(2) . . ?
N4 C29 C10 113.5(2) . . ?
N4 C29 H29A 108.9 . . ?
C10 C29 H29A 108.9 . . ?
N4 C29 H29B 108.9 . . ?
C10 C29 H29B 108.9 . . ?
H29A C29 H29B 107.7 . . ?
C25 C31 C19 120.4(3) . . ?
C25 C31 H31 119.8 . . ?
C19 C31 H31 119.8 . . ?
Cl1 O32 Cl6 24.47(16) . . ?
N3 C34 C51 110.7(2) . . ?
N3 C34 H34A 109.5 . . ?
C51 C34 H34A 109.5 . . ?
N3 C34 H34B 109.5 . . ?
C51 C34 H34B 109.5 . . ?
H34A C34 H34B 108.1 . . ?
C15 C35 C12 120.7(3) . . ?
C15 C35 H35 119.6 . . ?
C12 C35 H35 119.6 . . ?
N2 C36 C42 110.8(2) . . ?
N2 C36 H36A 109.5 . . ?
C42 C36 H36A 109.5 . . ?
N2 C36 H36B 109.5 . . ?
C42 C36 H36B 109.5 . . ?
H36A C36 H36B 108.1 . . ?
C59 C37 C12 120.7(3) . . ?
C59 C37 H37 119.7 . . ?
C12 C37 H37 119.7 . . ?
C39 C38 C9 120.7(3) . . ?
C39 C38 H38 119.6 . . ?
C9 C38 H38 119.6 . . ?
C17 C39 C38 120.2(3) . . ?
C17 C39 H39 119.9 . . ?
C38 C39 H39 119.9 . . ?
C27 C40 C9 121.0(3) . . ?
C27 C40 H40 119.5 . . ?
C9 C40 H40 119.5 . . ?
N24 C41 C57 178.6(5) . . ?
N6 C42 C36 111.7(2) . . ?
N6 C42 H42A 109.3 . . ?
C36 C42 H42A 109.3 . . ?
N6 C42 H42B 109.3 . . ?
C36 C42 H42B 109.3 . . ?
H42A C42 H42B 107.9 . . ?
N3 C43 C50 109.3(2) . . ?
N3 C43 H43A 109.8 . . ?
C50 C43 H43A 109.8 . . ?
N3 C43 H43B 109.8 . . ?
C50 C43 H43B 109.8 . . ?
H43A C43 H43B 108.3 . . ?
N7 C44 C9 110.7(2) . . ?
N7 C44 H44A 109.5 . . ?
C9 C44 H44A 109.5 . . ?
N7 C44 H44B 109.5 . . ?
C9 C44 H44B 109.5 . . ?
H44A C44 H44B 108.1 . . ?
N2 C45 C21 109.6(2) . . ?
N2 C45 H45A 109.8 . . ?
C21 C45 H45A 109.8 . . ?
N2 C45 H45B 109.8 . . ?
C21 C45 H45B 109.8 . . ?
H45A C45 H45B 108.2 . . ?
C59 C46 C15 120.3(3) . . ?
C59 C46 H46 119.9 . . ?
C15 C46 H46 119.9 . . ?
N14 C47 C53 108.9(2) . . ?
N14 C47 H47A 109.9 . . ?
C53 C47 H47A 109.9 . . ?
N14 C47 H47B 109.9 . . ?
C53 C47 H47B 109.9 . . ?
H47A C47 H47B 108.3 . . ?
N14 C48 C27 111.5(2) . . ?
N14 C48 H48A 109.3 . . ?
C27 C48 H48A 109.3 . . ?
N14 C48 H48B 109.3 . . ?
C27 C48 H48B 109.3 . . ?
H48A C48 H48B 108.0 . . ?
N8 C49 C15 113.7(2) . . ?
N8 C49 H49A 108.8 . . ?
C15 C49 H49A 108.8 . . ?
N8 C49 H49B 108.8 . . ?
C15 C49 H49B 108.8 . . ?
H49A C49 H49B 107.7 . . ?
N4 C50 C43 108.8(2) . . ?
N4 C50 H50A 109.9 . . ?
C43 C50 H50A 109.9 . . ?
N4 C50 H50B 109.9 . . ?
C43 C50 H50B 109.9 . . ?
H50A C50 H50B 108.3 . . ?
N8 C51 C34 108.9(2) . . ?
N8 C51 H51A 109.9 . . ?
C34 C51 H51A 109.9 . . ?
N8 C51 H51B 109.9 . . ?
C34 C51 H51B 109.9 . . ?
H51A C51 H51B 108.3 . . ?
N3 C53 C47 109.3(2) . . ?
N3 C53 H53A 109.8 . . ?
C47 C53 H53A 109.8 . . ?
N3 C53 H53B 109.8 . . ?
C47 C53 H53B 109.8 . . ?
H53A C53 H53B 108.3 . . ?
N5 C55 C23 110.8(2) . . ?
N5 C55 H55A 109.5 . . ?
C23 C55 H55A 109.5 . . ?
N5 C55 H55B 109.5 . . ?
C23 C55 H55B 109.5 . . ?
H55A C55 H55B 108.1 . . ?
N30 C56 C62 178.5(4) . . ?
C41 C57 H57A 109.5 . . ?
C41 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C41 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C37 C59 C46 120.0(3) . . ?
C37 C59 H59 120.0 . . ?
C46 C59 H59 120.0 . . ?
Cl6 O60 Cl1 24.51(14) . . ?
C56 C62 H62A 109.5 . . ?
C56 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C56 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
Cl6 O78 Cl1 3.64(16) . . ?
N71 C66 C98 178.7(7) . . ?
C66 C98 H98A 109.5 . . ?
C66 C98 H98B 109.5 . . ?
H98A C98 H98B 109.5 . . ?
C66 C98 H98C 109.5 . . ?
H98A C98 H98C 109.5 . . ?
H98B C98 H98C 109.5 . . ?
Cl6 Cl1 O32 90.6(5) . . ?
Cl6 Cl1 O20 79.4(5) . . ?
O32 Cl1 O20 121.1(3) . . ?
Cl6 Cl1 O11 171.1(8) . . ?
O32 Cl1 O11 98.1(6) . . ?
O20 Cl1 O11 97.4(8) . . ?
Cl6 Cl1 O60 72.5(5) . . ?
O32 Cl1 O60 119.1(3) . . ?
O20 Cl1 O60 112.7(3) . . ?
O11 Cl1 O60 101.5(8) . . ?
Cl6 Cl1 O78 8.8(4) . . ?
O32 Cl1 O78 82.4(3) . . ?
O20 Cl1 O78 81.3(3) . . ?
O11 Cl1 O78 178.6(8) . . ?
O60 Cl1 O78 79.4(3) . . ?
N1AA C2 C4 176.8(8) . . ?
C5 C3 H3A 109.5 . . ?
C5 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C5 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N0AA C5 C3 175.8(13) . . ?
Cl1 O11 Cl6 2.6(2) . . ?

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
C25 C10 C13 C11 -1.8(4) . . . . ?
C29 C10 C13 C11 -178.0(2) . . . . ?
C19 C11 C13 C10 1.2(4) . . . . ?
C26 C11 C13 C10 179.0(2) . . . . ?
C42 N6 C18 C12 -173.2(2) . . . . ?
Ni1 N6 C18 C12 56.1(3) . . . . ?
C37 C12 C18 N6 -149.1(2) . . . . ?
C35 C12 C18 N6 38.3(4) . . . . ?
C13 C11 C19 C31 -0.2(4) . . . . ?
C26 C11 C19 C31 -177.9(2) . . . . ?
O60 Cl6 O20 Cl1 -75.1(5) . . . . ?
O78 Cl6 O20 Cl1 167.3(6) . . . . ?
O32 Cl6 O20 Cl1 55.7(5) . . . . ?
O11 Cl6 O20 Cl1 -6.1(6) . . . . ?
C44 N7 C21 C45 178.3(2) . . . . ?
Ni1 N7 C21 C45 40.9(2) . . . . ?
C36 N2 C23 C55 -98.5(3) . . . . ?
C45 N2 C23 C55 135.5(2) . . . . ?
Ni1 N2 C23 C55 17.3(3) . . . . ?
C13 C10 C25 C31 1.2(4) . . . . ?
C29 C10 C25 C31 177.4(2) . . . . ?
C55 N5 C26 C11 172.5(2) . . . . ?
Ni1 N5 C26 C11 -67.3(3) . . . . ?
C19 C11 C26 N5 -60.8(3) . . . . ?
C13 C11 C26 N5 121.4(3) . . . . ?
C39 C17 C27 C40 0.0(4) . . . . ?
C39 C17 C27 C48 -179.6(2) . . . . ?
C50 N4 C29 C10 -160.2(2) . . . . ?
Ni2 N4 C29 C10 77.0(2) . . . . ?
C13 C10 C29 N4 -127.6(2) . . . . ?
C25 C10 C29 N4 56.3(3) . . . . ?
C10 C25 C31 C19 -0.2(4) . . . . ?
C11 C19 C31 C25 -0.3(4) . . . . ?
O60 Cl6 O32 Cl1 69.3(5) . . . . ?
O20 Cl6 O32 Cl1 -62.2(5) . . . . ?
O78 Cl6 O32 Cl1 -175.6(6) . . . . ?
O11 Cl6 O32 Cl1 1.3(7) . . . . ?
C53 N3 C34 C51 101.6(3) . . . . ?
C43 N3 C34 C51 -133.6(2) . . . . ?
Ni2 N3 C34 C51 -15.3(3) . . . . ?
C46 C15 C35 C12 0.6(4) . . . . ?
C49 C15 C35 C12 -173.4(2) . . . . ?
C37 C12 C35 C15 -2.2(4) . . . . ?
C18 C12 C35 C15 170.2(2) . . . . ?
C45 N2 C36 C42 -167.9(2) . . . . ?
C23 N2 C36 C42 67.2(3) . . . . ?
Ni1 N2 C36 C42 -51.5(2) . . . . ?
C35 C12 C37 C59 1.9(4) . . . . ?
C18 C12 C37 C59 -171.0(3) . . . . ?
C40 C9 C38 C39 -0.2(4) . . . . ?
C44 C9 C38 C39 179.2(3) . . . . ?
C27 C17 C39 C38 -0.5(4) . . . . ?
C9 C38 C39 C17 0.6(4) . . . . ?
C17 C27 C40 C9 0.3(4) . . . . ?
C48 C27 C40 C9 180.0(2) . . . . ?
C38 C9 C40 C27 -0.2(4) . . . . ?
C44 C9 C40 C27 -179.6(2) . . . . ?
C18 N6 C42 C36 -164.4(2) . . . . ?
Ni1 N6 C42 C36 -20.9(2) . . . . ?
N2 C36 C42 N6 49.8(3) . . . . ?
C53 N3 C43 C50 -149.9(2) . . . . ?
C34 N3 C43 C50 84.3(3) . . . . ?
Ni2 N3 C43 C50 -34.2(3) . . . . ?
C21 N7 C44 C9 147.5(2) . . . . ?
Ni1 N7 C44 C9 -82.8(3) . . . . ?
C38 C9 C44 N7 -58.1(3) . . . . ?
C40 C9 C44 N7 121.3(3) . . . . ?
C36 N2 C45 C21 157.1(2) . . . . ?
C23 N2 C45 C21 -76.5(3) . . . . ?
Ni1 N2 C45 C21 42.7(2) . . . . ?
N7 C21 C45 N2 -56.9(3) . . . . ?
C35 C15 C46 C59 1.5(4) . . . . ?
C49 C15 C46 C59 175.5(3) . . . . ?
C48 N14 C47 C53 -169.2(2) . . . . ?
Ni2 N14 C47 C53 -29.5(3) . . . . ?
C47 N14 C48 C27 -142.0(2) . . . . ?
Ni2 N14 C48 C27 85.4(3) . . . . ?
C17 C27 C48 N14 62.4(3) . . . . ?
C40 C27 C48 N14 -117.2(3) . . . . ?
C51 N8 C49 C15 -169.7(2) . . . . ?
Ni2 N8 C49 C15 76.0(3) . . . . ?
C46 C15 C49 N8 59.3(4) . . . . ?
C35 C15 C49 N8 -126.8(3) . . . . ?
C29 N4 C50 C43 -177.2(2) . . . . ?
Ni2 N4 C50 C43 -45.7(2) . . . . ?
N3 C43 C50 N4 54.6(3) . . . . ?
C49 N8 C51 C34 174.2(2) . . . . ?
Ni2 N8 C51 C34 -56.9(2) . . . . ?
N3 C34 C51 N8 51.3(3) . . . . ?
C43 N3 C53 C47 68.0(3) . . . . ?
C34 N3 C53 C47 -167.6(2) . . . . ?
Ni2 N3 C53 C47 -49.1(2) . . . . ?
N14 C47 C53 N3 53.4(3) . . . . ?
C26 N5 C55 C23 177.5(2) . . . . ?
Ni1 N5 C55 C23 45.8(2) . . . . ?
N2 C23 C55 N5 -44.0(3) . . . . ?
C12 C37 C59 C46 0.1(4) . . . . ?
C15 C46 C59 C37 -1.8(4) . . . . ?
O20 Cl6 O60 Cl1 70.8(5) . . . . ?
O78 Cl6 O60 Cl1 -171.8(6) . . . . ?
O32 Cl6 O60 Cl1 -58.6(5) . . . . ?
O11 Cl6 O60 Cl1 4.8(6) . . . . ?
O60 Cl6 O78 Cl1 139(3) . . . . ?
O20 Cl6 O78 Cl1 -98(3) . . . . ?
O32 Cl6 O78 Cl1 19(2) . . . . ?
O60 Cl6 Cl1 O32 -120.4(3) . . . . ?
O20 Cl6 Cl1 O32 121.5(3) . . . . ?
O78 Cl6 Cl1 O32 20(3) . . . . ?
O11 Cl6 Cl1 O32 -169(6) . . . . ?
O60 Cl6 Cl1 O20 118.1(2) . . . . ?
O78 Cl6 Cl1 O20 -101(2) . . . . ?
O32 Cl6 Cl1 O20 -121.5(3) . . . . ?
O11 Cl6 Cl1 O20 70(6) . . . . ?
O20 Cl6 Cl1 O60 -118.1(2) . . . . ?
O78 Cl6 Cl1 O60 141(2) . . . . ?
O32 Cl6 Cl1 O60 120.4(3) . . . . ?
O11 Cl6 Cl1 O60 -49(6) . . . . ?
O60 Cl6 Cl1 O78 -141(2) . . . . ?
O20 Cl6 Cl1 O78 101(2) . . . . ?
O32 Cl6 Cl1 O78 -20(3) . . . . ?
O11 Cl6 Cl1 O78 171(5) . . . . ?
Cl6 O32 Cl1 O20 78.0(5) . . . . ?
Cl6 O32 Cl1 O11 -178.3(10) . . . . ?
Cl6 O32 Cl1 O60 -70.2(5) . . . . ?
Cl6 O32 Cl1 O78 3.0(4) . . . . ?
Cl6 O20 Cl1 O32 -84.3(6) . . . . ?
Cl6 O20 Cl1 O11 171.6(9) . . . . ?
Cl6 O20 Cl1 O60 65.8(5) . . . . ?
Cl6 O20 Cl1 O78 -8.7(4) . . . . ?
Cl6 O60 Cl1 O32 80.7(6) . . . . ?
Cl6 O60 Cl1 O20 -70.1(5) . . . . ?
Cl6 O60 Cl1 O11 -173.2(8) . . . . ?
Cl6 O60 Cl1 O78 5.7(4) . . . . ?
O32 Cl1 O11 Cl6 169(7) . . . . ?
O20 Cl1 O11 Cl6 -68(6) . . . . ?
O60 Cl1 O11 Cl6 47(6) . . . . ?

_refine_diff_density_max         1.891
_refine_diff_density_min         -1.298
_refine_diff_density_rms         0.090

####################################################################### 
# 
# 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_added_by_encifer
_database_code_depnum_ccdc_archive 'CCDC 1418423'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2015-12-08 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            'C50 H83 Cl4 N9 Ni2 O13'
_chemical_formula_weight         1277.47

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/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.0625(17)
_cell_length_b                   23.576(2)
_cell_length_c                   21.767(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.325(13)
_cell_angle_gamma                90
_cell_volume                     7185.4(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    373(2)
_cell_measurement_reflns_used    11282
_cell_measurement_theta_min      1.868
_cell_measurement_theta_max      24.216

_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_F_000             2696
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    0.728
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      373(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            54008
_diffrn_reflns_av_unetI/netI     0.1454
_diffrn_reflns_av_R_equivalents  0.0806
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.868
_diffrn_reflns_theta_max         24.216
_diffrn_reflns_theta_full        24.216
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.975
_reflns_number_total             11282
_reflns_number_gt                5191
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_solution    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (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)+(0.0200P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11282
_refine_ls_number_parameters     750
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0463
_refine_ls_wR_factor_ref         0.0806
_refine_ls_wR_factor_gt          0.0755
_refine_ls_goodness_of_fit_ref   0.814
_refine_ls_restrained_S_all      0.814
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.28542(4) 0.29279(2) 0.83277(2) 0.03766(15) Uani 1 1 d . . . . .
Ni2 Ni -0.03329(4) 0.46357(2) 0.85299(2) 0.04034(16) Uani 1 1 d . . . . .
Cl3 Cl 0.11543(7) 0.44678(4) 0.90840(5) 0.0440(3) Uani 1 1 d . . . . .
Cl4 Cl 0.38870(9) 0.60923(6) 1.08129(7) 0.0624(4) Uani 1 1 d . . . . .
Cl1 Cl 0.18831(16) 0.04462(8) 0.86527(8) 0.0973(6) Uani 1 1 d . . . . .
O0AA O 0.17377(18) 0.34768(10) 0.82646(11) 0.0407(7) Uani 1 1 d . . . . .
H0AA H 0.1668 0.3626 0.7903 0.061 Uiso 1 1 d R U . . .
H0AB H 0.1843 0.3743 0.8533 0.061 Uiso 1 1 d R U . . .
N4AA N 0.2265(2) 0.24203(13) 0.75821(15) 0.0412(9) Uani 1 1 d . . . . .
H4AA H 0.2538 0.2556 0.7211 0.049 Uiso 1 1 calc R U . . .
N4 N -0.1034(2) 0.41947(14) 0.92176(15) 0.0433(9) Uani 1 1 d . . . . .
H4 H -0.1635 0.4038 0.9024 0.052 Uiso 1 1 calc R U . . .
N5AA N -0.1337(2) 0.52544(15) 0.86500(15) 0.0466(10) Uani 1 1 d . . . . .
N6AA N 0.2438(2) 0.23863(14) 0.90826(15) 0.0429(9) Uani 1 1 d . . . . .
H6AA H 0.2491 0.2644 0.9438 0.051 Uiso 1 1 calc R U . . .
N7AA N 0.4005(2) 0.23701(14) 0.83642(16) 0.0439(9) Uani 1 1 d . . . . .
N8AA N 0.3752(2) 0.34393(13) 0.77891(15) 0.0437(9) Uani 1 1 d . . . . .
H8AA H 0.4055 0.3712 0.8086 0.052 Uiso 1 1 calc R U . . .
N9AA N 0.0408(2) 0.53164(14) 0.81241(15) 0.0447(9) Uani 1 1 d . . . . .
H9AA H 0.0966 0.5382 0.8419 0.054 Uiso 1 1 calc R U . . .
C9AA C 0.0500(3) 0.29525(19) 0.93366(17) 0.0416(11) Uani 1 1 d . . . . .
H9AB H 0.1027 0.3152 0.9513 0.050 Uiso 1 1 calc R U . . .
C1AA C 0.0704(3) 0.28727(18) 0.71721(19) 0.0434(11) Uani 1 1 d . . . . .
N13 N -0.1263(2) 0.44058(14) 0.77674(15) 0.0452(9) Uani 1 1 d . . . . .
H13 H -0.1047 0.4609 0.7413 0.054 Uiso 1 1 calc R U . . .
C14 C 0.0465(3) 0.36241(19) 0.64029(19) 0.0479(12) Uani 1 1 d . . . . .
C2AA C -0.0556(3) 0.37539(17) 0.96236(18) 0.0447(12) Uani 1 1 d . . . . .
H2AA H -0.0932 0.3692 0.9969 0.054 Uiso 1 1 calc R U . . .
H2AB H 0.0063 0.3897 0.9788 0.054 Uiso 1 1 calc R U . . .
N16 N 0.3372(2) 0.34690(15) 0.90611(16) 0.0414(9) Uani 1 1 d . . . . .
C17 C -0.1195(3) 0.28874(19) 0.90708(18) 0.0447(11) Uani 1 1 d . . . . .
H17 H -0.1799 0.3048 0.9074 0.054 Uiso 1 1 calc R U . . .
C3AA C 0.3063(3) 0.43758(18) 0.74663(18) 0.0409(11) Uani 1 1 d . . . . .
O19 O 0.3064(3) 0.62624(15) 1.1060(2) 0.1179(17) Uani 1 1 d . . . . .
C20 C 0.0610(3) 0.24068(19) 0.90894(19) 0.0432(11) Uani 1 1 d . . . . .
C7AA C 0.1846(3) 0.50657(19) 0.75994(19) 0.0413(11) Uani 1 1 d . . . . .
O22 O 0.4263(3) 0.65360(14) 1.04696(15) 0.0845(11) Uani 1 1 d . . . . .
C23 C -0.0044(3) 0.30931(17) 0.74802(18) 0.0419(11) Uani 1 1 d . . . . .
H23 H -0.0210 0.2918 0.7838 0.050 Uiso 1 1 calc R U . . .
C24 C -0.1111(3) 0.23471(19) 0.8820(2) 0.0493(12) Uani 1 1 d . . . . .
C25 C 0.2114(3) 0.45417(19) 0.74046(18) 0.0439(11) Uani 1 1 d . . . . .
H25 H 0.1651 0.4294 0.7228 0.053 Uiso 1 1 calc R U . . .
C26 C -0.1800(3) 0.51317(19) 0.9222(2) 0.0521(13) Uani 1 1 d . . . . .
H26A H -0.2448 0.5002 0.9112 0.063 Uiso 1 1 calc R U . . .
H26B H -0.1831 0.5477 0.9461 0.063 Uiso 1 1 calc R U . . .
C27 C 0.3512(3) 0.52844(19) 0.7937(2) 0.0464(12) Uani 1 1 d . . . . .
C28 C -0.0413(3) 0.31911(18) 0.93141(18) 0.0410(11) Uani 1 1 d . . . . .
C29 C 0.3234(3) 0.19750(18) 0.92366(19) 0.0490(12) Uani 1 1 d . . . . .
H29A H 0.3066 0.1611 0.9048 0.059 Uiso 1 1 calc R U . . .
H29B H 0.3320 0.1921 0.9680 0.059 Uiso 1 1 calc R U . . .
C30 C 0.0932(3) 0.31422(18) 0.66326(18) 0.0454(12) Uani 1 1 d . . . . .
H30 H 0.1418 0.2991 0.6420 0.054 Uiso 1 1 calc R U . . .
C31 C 0.3756(3) 0.47479(19) 0.7727(2) 0.0488(12) Uani 1 1 d . . . . .
H31 H 0.4394 0.4637 0.7763 0.059 Uiso 1 1 calc R U . . .
C32 C -0.0539(3) 0.35704(18) 0.72579(19) 0.0428(11) Uani 1 1 d . . . . .
C33 C -0.0188(3) 0.21199(19) 0.88341(19) 0.0462(11) Uani 1 1 d . . . . .
H33 H -0.0109 0.1763 0.8665 0.055 Uiso 1 1 calc R U . . .
C34 C 0.2545(3) 0.54293(18) 0.78634(18) 0.0431(11) Uani 1 1 d . . . . .
H34 H 0.2362 0.5784 0.7997 0.052 Uiso 1 1 calc R U . . .
C35 C 0.1230(3) 0.23471(17) 0.74180(19) 0.0448(12) Uani 1 1 d . . . . .
H35A H 0.0942 0.2218 0.7781 0.054 Uiso 1 1 calc R U . . .
H35B H 0.1139 0.2050 0.7109 0.054 Uiso 1 1 calc R U . . .
C36 C -0.0283(3) 0.38300(19) 0.67195(19) 0.0497(12) Uani 1 1 d . . . . .
H36 H -0.0620 0.4148 0.6568 0.060 Uiso 1 1 calc R U . . .
C37 C 0.4157(3) 0.21817(19) 0.9013(2) 0.0506(12) Uani 1 1 d . . . . .
H37A H 0.4405 0.2494 0.9270 0.061 Uiso 1 1 calc R U . . .
H37B H 0.4625 0.1878 0.9048 0.061 Uiso 1 1 calc R U . . .
C38 C -0.2053(3) 0.52533(19) 0.8102(2) 0.0559(13) Uani 1 1 d . . . . .
H38A H -0.1828 0.5486 0.7778 0.067 Uiso 1 1 calc R U . . .
H38B H -0.2652 0.5410 0.8212 0.067 Uiso 1 1 calc R U . . .
C39 C -0.2204(3) 0.46508(19) 0.78772(19) 0.0494(12) Uani 1 1 d . . . . .
H39A H -0.2497 0.4428 0.8184 0.059 Uiso 1 1 calc R U . . .
H39B H -0.2625 0.4647 0.7498 0.059 Uiso 1 1 calc R U . . .
C40 C 0.4546(3) 0.30647(17) 0.7633(2) 0.0490(12) Uani 1 1 d . . . . .
H40A H 0.5085 0.3293 0.7533 0.059 Uiso 1 1 calc R U . . .
H40B H 0.4340 0.2834 0.7276 0.059 Uiso 1 1 calc R U . . .
C41 C 0.1544(3) 0.20811(19) 0.9153(2) 0.0543(12) Uani 1 1 d . . . . .
H41A H 0.1604 0.1905 0.9558 0.065 Uiso 1 1 calc R U . . .
H41B H 0.1493 0.1777 0.8851 0.065 Uiso 1 1 calc R U . . .
O43 O 0.3738(3) 0.55927(15) 1.04580(18) 0.1097(15) Uani 1 1 d . . . . .
C44 C 0.2691(3) 0.18473(16) 0.77295(19) 0.0440(12) Uani 1 1 d . . . . .
H44A H 0.2588 0.1604 0.7370 0.053 Uiso 1 1 calc R U . . .
H44B H 0.2378 0.1676 0.8062 0.053 Uiso 1 1 calc R U . . .
C45 C 0.3751(3) 0.42709(18) 0.9856(2) 0.0578(14) Uani 1 1 d . . . . .
H45A H 0.3404 0.4606 0.9721 0.087 Uiso 1 1 calc R U . . .
H45B H 0.4423 0.4350 0.9891 0.087 Uiso 1 1 calc R U . . .
H45C H 0.3564 0.4155 1.0250 0.087 Uiso 1 1 calc R U . . .
O46 O 0.2750(3) 0.06408(14) 0.84339(18) 0.0967(13) Uani 1 1 d . . . . .
C47 C -0.1260(3) 0.46868(18) 0.96084(19) 0.0500(12) Uani 1 1 d . . . . .
H47A H -0.0673 0.4848 0.9802 0.060 Uiso 1 1 calc R U . . .
H47B H -0.1642 0.4560 0.9931 0.060 Uiso 1 1 calc R U . . .
C49 C 0.3358(3) 0.37930(17) 0.7263(2) 0.0513(13) Uani 1 1 d . . . . .
H49A H 0.2808 0.3603 0.7053 0.062 Uiso 1 1 calc R U . . .
H49B H 0.3836 0.3833 0.6971 0.062 Uiso 1 1 calc R U . . .
O50 O 0.4579(3) 0.59682(17) 1.1328(2) 0.1236(17) Uani 1 1 d . . . . .
C51 C -0.1369(3) 0.37972(17) 0.75787(19) 0.0459(12) Uani 1 1 d . . . . .
H51A H -0.1950 0.3756 0.7305 0.055 Uiso 1 1 calc R U . . .
H51B H -0.1439 0.3569 0.7943 0.055 Uiso 1 1 calc R U . . .
C54 C 0.3749(3) 0.18962(17) 0.7918(2) 0.0475(12) Uani 1 1 d . . . . .
H54A H 0.3974 0.1541 0.8104 0.057 Uiso 1 1 calc R U . . .
H54B H 0.4079 0.1955 0.7551 0.057 Uiso 1 1 calc R U . . .
C57 C 0.0823(3) 0.52511(18) 0.75196(19) 0.0495(12) Uani 1 1 d . . . . .
H57A H 0.0778 0.5610 0.7301 0.059 Uiso 1 1 calc R U . . .
H57B H 0.0452 0.4974 0.7270 0.059 Uiso 1 1 calc R U . . .
C58 C 0.3544(3) 0.3823(2) 0.9415(2) 0.0414(11) Uani 1 1 d . . . . .
C59 C 0.4841(3) 0.26861(18) 0.8184(2) 0.0524(13) Uani 1 1 d . . . . .
H59A H 0.5329 0.2422 0.8079 0.063 Uiso 1 1 calc R U . . .
H59B H 0.5106 0.2916 0.8528 0.063 Uiso 1 1 calc R U . . .
C65 C -0.0174(3) 0.58466(18) 0.8163(2) 0.0594(14) Uani 1 1 d . . . . .
H65A H -0.0582 0.5899 0.7783 0.071 Uiso 1 1 calc R U . . .
H65B H 0.0245 0.6173 0.8222 0.071 Uiso 1 1 calc R U . . .
C66 C -0.0774(3) 0.57957(17) 0.8697(2) 0.0559(13) Uani 1 1 d . . . . .
H66A H -0.0365 0.5800 0.9081 0.067 Uiso 1 1 calc R U . . .
H66B H -0.1206 0.6116 0.8698 0.067 Uiso 1 1 calc R U . . .
O69 O 0.1879(4) 0.05466(17) 0.92637(17) 0.1343(18) Uani 1 1 d . . . . .
Cl5 Cl 0.29331(11) 0.29583(6) 0.09047(6) 0.0651(4) Uani 1 1 d . . . . .
O1AA O 0.3162(3) 0.25329(14) 0.13503(14) 0.0784(11) Uani 1 1 d . . . . .
C4AA C 0.0706(4) 0.3909(2) 0.58037(19) 0.0584(14) Uani 1 1 d . . . . .
C5AA C 0.4262(3) 0.56955(19) 0.8237(2) 0.0566(13) Uani 1 1 d . . . . .
O2AA O 0.2995(3) 0.34965(15) 0.11616(17) 0.0993(13) Uani 1 1 d . . . . .
C8AA C 0.4127(4) 0.62845(19) 0.7950(3) 0.0789(17) Uani 1 1 d . . . . .
H8AB H 0.4196 0.6263 0.7516 0.118 Uiso 1 1 calc R U . . .
H8AC H 0.4600 0.6538 0.8142 0.118 Uiso 1 1 calc R U . . .
H8AD H 0.3501 0.6423 0.8012 0.118 Uiso 1 1 calc R U . . .
C6 C -0.2000(4) 0.2028(2) 0.8541(2) 0.0660(14) Uani 1 1 d . . . . .
C7 C 0.1758(4) 0.3812(2) 0.5694(2) 0.0705(16) Uani 1 1 d . . . . .
H7A H 0.2162 0.3953 0.6041 0.106 Uiso 1 1 calc R U . . .
H7B H 0.1899 0.4010 0.5327 0.106 Uiso 1 1 calc R U . . .
H7C H 0.1872 0.3414 0.5645 0.106 Uiso 1 1 calc R U . . .
C8 C 0.0526(5) 0.4554(2) 0.5803(2) 0.113(3) Uani 1 1 d . . . . .
H8A H -0.0145 0.4625 0.5813 0.170 Uiso 1 1 calc R U . . .
H8B H 0.0739 0.4718 0.5436 0.170 Uiso 1 1 calc R U . . .
H8C H 0.0870 0.4722 0.6159 0.170 Uiso 1 1 calc R U . . .
C9 C 0.0078(4) 0.3639(3) 0.5270(2) 0.102(2) Uani 1 1 d . . . . .
H9A H 0.0221 0.3242 0.5249 0.154 Uiso 1 1 calc R U . . .
H9B H 0.0203 0.3819 0.4889 0.154 Uiso 1 1 calc R U . . .
H9C H -0.0582 0.3688 0.5336 0.154 Uiso 1 1 calc R U . . .
C10 C 0.4131(5) 0.5745(2) 0.8927(3) 0.122(3) Uani 1 1 d . . . . .
H10A H 0.3478 0.5835 0.8978 0.183 Uiso 1 1 calc R U . . .
H10B H 0.4538 0.6039 0.9107 0.183 Uiso 1 1 calc R U . . .
H10C H 0.4296 0.5391 0.9127 0.183 Uiso 1 1 calc R U . . .
C11 C -0.2763(4) 0.2018(3) 0.9004(3) 0.113(2) Uani 1 1 d . . . . .
H11A H -0.2496 0.1855 0.9387 0.170 Uiso 1 1 calc R U . . .
H11B H -0.3297 0.1794 0.8840 0.170 Uiso 1 1 calc R U . . .
H11C H -0.2972 0.2398 0.9076 0.170 Uiso 1 1 calc R U . . .
C6AA C -0.2500(4) 0.2369(3) 0.8000(3) 0.115(2) Uani 1 1 d . . . . .
H6AB H -0.2640 0.2744 0.8138 0.173 Uiso 1 1 calc R U . . .
H6AC H -0.3083 0.2183 0.7852 0.173 Uiso 1 1 calc R U . . .
H6AD H -0.2088 0.2393 0.7673 0.173 Uiso 1 1 calc R U . . .
C15 C 0.5273(4) 0.5513(2) 0.8174(3) 0.126(3) Uani 1 1 d . . . . .
H15A H 0.5392 0.5156 0.8379 0.188 Uiso 1 1 calc R U . . .
H15B H 0.5706 0.5794 0.8358 0.188 Uiso 1 1 calc R U . . .
H15C H 0.5368 0.5474 0.7745 0.188 Uiso 1 1 calc R U . . .
C18 C -0.1815(4) 0.1445(3) 0.8383(4) 0.193(5) Uani 1 1 d . . . . .
H18A H -0.1418 0.1436 0.8047 0.289 Uiso 1 1 calc R U . . .
H18B H -0.2408 0.1257 0.8262 0.289 Uiso 1 1 calc R U . . .
H18C H -0.1495 0.1256 0.8734 0.289 Uiso 1 1 calc R U . . .
O3AA O 0.1515(9) -0.0054(6) 0.8422(5) 0.075(4) Uani 0.5 1 d . . P A 2
O4AA O 0.3191(9) 0.2890(4) 0.0348(3) 0.081(3) Uani 0.5 1 d . . P B 1
O3 O 0.3870(7) 0.2972(5) 0.0565(5) 0.107(4) Uani 0.5 1 d . . P B 2
O4 O 0.1084(10) 0.0903(4) 0.8307(7) 0.098(4) Uani 0.5 1 d . . P A 2
O5 O 0.2251(8) 0.2807(4) 0.0475(4) 0.103(3) Uani 0.5 1 d . . P B 2
O6 O 0.1798(7) 0.2938(4) 0.0839(4) 0.091(3) Uani 0.5 1 d . . P B 1
O1 O 0.1184(10) 0.0518(8) 0.8288(6) 0.126(6) Uani 0.5 1 d . . P A 1
O2 O 0.2084(9) -0.0217(6) 0.8628(7) 0.119(5) Uani 0.5 1 d . . P A 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O0AA 2.029(3) . ?
Ni1 N7AA 2.081(3) . ?
Ni1 N16 2.119(4) . ?
Ni1 N4AA 2.122(3) . ?
Ni1 N8AA 2.167(3) . ?
Ni1 N6AA 2.203(3) . ?
Ni2 N5AA 2.064(3) . ?
Ni2 N13 2.087(3) . ?
Ni2 N4 2.137(3) . ?
Ni2 N9AA 2.147(3) . ?
Ni2 Cl3 2.3488(13) . ?
Cl4 O19 1.380(3) . ?
Cl4 O43 1.413(3) . ?
Cl4 O22 1.416(3) . ?
Cl4 O50 1.445(4) . ?
Cl1 O1 1.217(12) . ?
Cl1 O69 1.351(3) . ?
Cl1 O3AA 1.364(11) . ?
Cl1 O46 1.426(4) . ?
Cl1 O2 1.590(16) . ?
Cl1 O4 1.684(12) . ?
O0AA H0AA 0.8597 . ?
O0AA H0AB 0.8604 . ?
N4AA C35 1.476(5) . ?
N4AA C44 1.501(4) . ?
N4AA H4AA 0.9800 . ?
N4 C2AA 1.484(5) . ?
N4 C47 1.490(4) . ?
N4 H4 0.9800 . ?
N5AA C26 1.485(5) . ?
N5AA C38 1.488(5) . ?
N5AA C66 1.501(5) . ?
N6AA C41 1.468(5) . ?
N6AA C29 1.495(5) . ?
N6AA H6AA 0.9800 . ?
N7AA C59 1.475(5) . ?
N7AA C37 1.477(5) . ?
N7AA C54 1.502(5) . ?
N8AA C49 1.482(5) . ?
N8AA C40 1.488(4) . ?
N8AA H8AA 0.9800 . ?
N9AA C57 1.496(5) . ?
N9AA C65 1.501(5) . ?
N9AA H9AA 0.9800 . ?
C9AA C28 1.397(5) . ?
C9AA C20 1.409(5) . ?
C9AA H9AB 0.9300 . ?
C1AA C23 1.398(5) . ?
C1AA C30 1.399(5) . ?
C1AA C35 1.515(5) . ?
N13 C39 1.484(5) . ?
N13 C51 1.496(5) . ?
N13 H13 0.9800 . ?
C14 C30 1.382(5) . ?
C14 C36 1.397(5) . ?
C14 C4AA 1.532(6) . ?
C2AA C28 1.510(5) . ?
C2AA H2AA 0.9700 . ?
C2AA H2AB 0.9700 . ?
N16 C58 1.147(5) . ?
C17 C28 1.377(5) . ?
C17 C24 1.395(5) . ?
C17 H17 0.9300 . ?
C3AA C25 1.386(5) . ?
C3AA C31 1.392(6) . ?
C3AA C49 1.513(5) . ?
C20 C33 1.381(6) . ?
C20 C41 1.517(6) . ?
C7AA C25 1.370(5) . ?
C7AA C34 1.388(5) . ?
C7AA C57 1.499(5) . ?
C23 C32 1.387(5) . ?
C23 H23 0.9300 . ?
C24 C33 1.403(6) . ?
C24 C6 1.535(6) . ?
C25 H25 0.9300 . ?
C26 C47 1.506(5) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C34 1.396(5) . ?
C27 C31 1.398(5) . ?
C27 C5AA 1.533(6) . ?
C29 C37 1.509(5) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 C36 1.399(5) . ?
C32 C51 1.512(5) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36 0.9300 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.511(5) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 C59 1.522(5) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C44 C54 1.511(5) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 C58 1.438(6) . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C65 C66 1.502(5) . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
Cl5 O4AA 1.307(7) . ?
Cl5 O5 1.325(7) . ?
Cl5 O2AA 1.386(3) . ?
Cl5 O1AA 1.411(3) . ?
Cl5 O3 1.570(8) . ?
Cl5 O6 1.591(9) . ?
C4AA C9 1.531(7) . ?
C4AA C7 1.538(6) . ?
C4AA C8 1.543(6) . ?
C5AA C15 1.504(6) . ?
C5AA C8AA 1.527(6) . ?
C5AA C10 1.534(7) . ?
C8AA H8AB 0.9600 . ?
C8AA H8AC 0.9600 . ?
C8AA H8AD 0.9600 . ?
C6 C18 1.447(7) . ?
C6 C11 1.539(7) . ?
C6 C6AA 1.541(7) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C6AA H6AB 0.9600 . ?
C6AA H6AC 0.9600 . ?
C6AA H6AD 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O0AA Ni1 N7AA 178.24(12) . . ?
O0AA Ni1 N16 82.91(11) . . ?
N7AA Ni1 N16 98.07(13) . . ?
O0AA Ni1 N4AA 93.60(11) . . ?
N7AA Ni1 N4AA 85.41(13) . . ?
N16 Ni1 N4AA 176.50(13) . . ?
O0AA Ni1 N8AA 95.42(11) . . ?
N7AA Ni1 N8AA 83.25(13) . . ?
N16 Ni1 N8AA 84.04(13) . . ?
N4AA Ni1 N8AA 96.07(12) . . ?
O0AA Ni1 N6AA 99.35(11) . . ?
N7AA Ni1 N6AA 82.24(13) . . ?
N16 Ni1 N6AA 83.30(13) . . ?
N4AA Ni1 N6AA 97.56(13) . . ?
N8AA Ni1 N6AA 159.18(13) . . ?
N5AA Ni2 N13 84.18(13) . . ?
N5AA Ni2 N4 83.66(13) . . ?
N13 Ni2 N4 97.75(13) . . ?
N5AA Ni2 N9AA 83.54(13) . . ?
N13 Ni2 N9AA 99.15(13) . . ?
N4 Ni2 N9AA 157.60(12) . . ?
N5AA Ni2 Cl3 129.88(10) . . ?
N13 Ni2 Cl3 145.79(9) . . ?
N4 Ni2 Cl3 90.29(10) . . ?
N9AA Ni2 Cl3 83.95(10) . . ?
O19 Cl4 O43 111.6(3) . . ?
O19 Cl4 O22 111.0(2) . . ?
O43 Cl4 O22 111.8(2) . . ?
O19 Cl4 O50 106.5(3) . . ?
O43 Cl4 O50 108.1(3) . . ?
O22 Cl4 O50 107.6(2) . . ?
O1 Cl1 O69 122.7(8) . . ?
O69 Cl1 O3AA 118.5(6) . . ?
O1 Cl1 O46 113.7(7) . . ?
O69 Cl1 O46 110.7(3) . . ?
O3AA Cl1 O46 117.6(5) . . ?
O1 Cl1 O2 104.5(9) . . ?
O69 Cl1 O2 102.9(6) . . ?
O46 Cl1 O2 98.3(5) . . ?
O69 Cl1 O4 105.4(6) . . ?
O3AA Cl1 O4 100.0(8) . . ?
O46 Cl1 O4 101.6(6) . . ?
Ni1 O0AA H0AA 110.1 . . ?
Ni1 O0AA H0AB 109.6 . . ?
H0AA O0AA H0AB 108.9 . . ?
C35 N4AA C44 108.2(3) . . ?
C35 N4AA Ni1 123.9(2) . . ?
C44 N4AA Ni1 103.0(2) . . ?
C35 N4AA H4AA 106.9 . . ?
C44 N4AA H4AA 106.9 . . ?
Ni1 N4AA H4AA 106.9 . . ?
C2AA N4 C47 108.3(3) . . ?
C2AA N4 Ni2 123.0(2) . . ?
C47 N4 Ni2 99.1(2) . . ?
C2AA N4 H4 108.5 . . ?
C47 N4 H4 108.5 . . ?
Ni2 N4 H4 108.5 . . ?
C26 N5AA C38 110.7(3) . . ?
C26 N5AA C66 112.2(3) . . ?
C38 N5AA C66 111.7(3) . . ?
C26 N5AA Ni2 109.1(3) . . ?
C38 N5AA Ni2 108.5(2) . . ?
C66 N5AA Ni2 104.3(2) . . ?
C41 N6AA C29 106.8(3) . . ?
C41 N6AA Ni1 130.7(3) . . ?
C29 N6AA Ni1 107.3(2) . . ?
C41 N6AA H6AA 102.9 . . ?
C29 N6AA H6AA 102.9 . . ?
Ni1 N6AA H6AA 102.9 . . ?
C59 N7AA C37 111.0(3) . . ?
C59 N7AA C54 110.6(3) . . ?
C37 N7AA C54 113.6(3) . . ?
C59 N7AA Ni1 107.9(2) . . ?
C37 N7AA Ni1 105.6(2) . . ?
C54 N7AA Ni1 107.9(3) . . ?
C49 N8AA C40 113.0(3) . . ?
C49 N8AA Ni1 122.5(3) . . ?
C40 N8AA Ni1 106.3(2) . . ?
C49 N8AA H8AA 104.4 . . ?
C40 N8AA H8AA 104.4 . . ?
Ni1 N8AA H8AA 104.4 . . ?
C57 N9AA C65 113.3(3) . . ?
C57 N9AA Ni2 121.9(3) . . ?
C65 N9AA Ni2 108.1(2) . . ?
C57 N9AA H9AA 103.8 . . ?
C65 N9AA H9AA 103.8 . . ?
Ni2 N9AA H9AA 103.8 . . ?
C28 C9AA C20 119.2(4) . . ?
C28 C9AA H9AB 120.4 . . ?
C20 C9AA H9AB 120.4 . . ?
C23 C1AA C30 118.4(4) . . ?
C23 C1AA C35 119.9(4) . . ?
C30 C1AA C35 121.7(4) . . ?
C39 N13 C51 110.5(3) . . ?
C39 N13 Ni2 105.9(2) . . ?
C51 N13 Ni2 120.4(3) . . ?
C39 N13 H13 106.4 . . ?
C51 N13 H13 106.4 . . ?
Ni2 N13 H13 106.4 . . ?
C30 C14 C36 117.5(4) . . ?
C30 C14 C4AA 122.2(4) . . ?
C36 C14 C4AA 120.2(4) . . ?
N4 C2AA C28 114.9(3) . . ?
N4 C2AA H2AA 108.5 . . ?
C28 C2AA H2AA 108.5 . . ?
N4 C2AA H2AB 108.5 . . ?
C28 C2AA H2AB 108.5 . . ?
H2AA C2AA H2AB 107.5 . . ?
C58 N16 Ni1 168.8(4) . . ?
C28 C17 C24 122.1(4) . . ?
C28 C17 H17 118.9 . . ?
C24 C17 H17 118.9 . . ?
C25 C3AA C31 119.5(4) . . ?
C25 C3AA C49 121.0(4) . . ?
C31 C3AA C49 119.4(4) . . ?
C33 C20 C9AA 119.1(4) . . ?
C33 C20 C41 116.9(4) . . ?
C9AA C20 C41 123.5(4) . . ?
C25 C7AA C34 118.7(4) . . ?
C25 C7AA C57 121.0(4) . . ?
C34 C7AA C57 120.2(4) . . ?
C32 C23 C1AA 120.7(4) . . ?
C32 C23 H23 119.7 . . ?
C1AA C23 H23 119.7 . . ?
C17 C24 C33 116.8(4) . . ?
C17 C24 C6 120.4(4) . . ?
C33 C24 C6 122.7(4) . . ?
C7AA C25 C3AA 120.9(4) . . ?
C7AA C25 H25 119.5 . . ?
C3AA C25 H25 119.5 . . ?
N5AA C26 C47 111.5(3) . . ?
N5AA C26 H26A 109.3 . . ?
C47 C26 H26A 109.3 . . ?
N5AA C26 H26B 109.3 . . ?
C47 C26 H26B 109.3 . . ?
H26A C26 H26B 108.0 . . ?
C34 C27 C31 116.7(4) . . ?
C34 C27 C5AA 121.2(4) . . ?
C31 C27 C5AA 122.1(4) . . ?
C17 C28 C9AA 120.2(4) . . ?
C17 C28 C2AA 119.6(4) . . ?
C9AA C28 C2AA 119.9(4) . . ?
N6AA C29 C37 111.5(3) . . ?
N6AA C29 H29A 109.3 . . ?
C37 C29 H29A 109.3 . . ?
N6AA C29 H29B 109.3 . . ?
C37 C29 H29B 109.3 . . ?
H29A C29 H29B 108.0 . . ?
C14 C30 C1AA 122.6(4) . . ?
C14 C30 H30 118.7 . . ?
C1AA C30 H30 118.7 . . ?
C3AA C31 C27 121.3(4) . . ?
C3AA C31 H31 119.4 . . ?
C27 C31 H31 119.4 . . ?
C23 C32 C36 119.2(4) . . ?
C23 C32 C51 120.7(4) . . ?
C36 C32 C51 120.1(4) . . ?
C20 C33 C24 122.5(4) . . ?
C20 C33 H33 118.7 . . ?
C24 C33 H33 118.7 . . ?
C7AA C34 C27 122.8(4) . . ?
C7AA C34 H34 118.6 . . ?
C27 C34 H34 118.6 . . ?
N4AA C35 C1AA 115.3(3) . . ?
N4AA C35 H35A 108.4 . . ?
C1AA C35 H35A 108.4 . . ?
N4AA C35 H35B 108.4 . . ?
C1AA C35 H35B 108.4 . . ?
H35A C35 H35B 107.5 . . ?
C14 C36 C32 121.7(4) . . ?
C14 C36 H36 119.2 . . ?
C32 C36 H36 119.2 . . ?
N7AA C37 C29 110.7(3) . . ?
N7AA C37 H37A 109.5 . . ?
C29 C37 H37A 109.5 . . ?
N7AA C37 H37B 109.5 . . ?
C29 C37 H37B 109.5 . . ?
H37A C37 H37B 108.1 . . ?
N5AA C38 C39 109.0(3) . . ?
N5AA C38 H38A 109.9 . . ?
C39 C38 H38A 109.9 . . ?
N5AA C38 H38B 109.9 . . ?
C39 C38 H38B 109.9 . . ?
H38A C38 H38B 108.3 . . ?
N13 C39 C38 108.5(3) . . ?
N13 C39 H39A 110.0 . . ?
C38 C39 H39A 110.0 . . ?
N13 C39 H39B 110.0 . . ?
C38 C39 H39B 110.0 . . ?
H39A C39 H39B 108.4 . . ?
N8AA C40 C59 108.8(3) . . ?
N8AA C40 H40A 109.9 . . ?
C59 C40 H40A 109.9 . . ?
N8AA C40 H40B 109.9 . . ?
C59 C40 H40B 109.9 . . ?
H40A C40 H40B 108.3 . . ?
N6AA C41 C20 119.0(4) . . ?
N6AA C41 H41A 107.6 . . ?
C20 C41 H41A 107.6 . . ?
N6AA C41 H41B 107.6 . . ?
C20 C41 H41B 107.6 . . ?
H41A C41 H41B 107.0 . . ?
N4AA C44 C54 110.7(3) . . ?
N4AA C44 H44A 109.5 . . ?
C54 C44 H44A 109.5 . . ?
N4AA C44 H44B 109.5 . . ?
C54 C44 H44B 109.5 . . ?
H44A C44 H44B 108.1 . . ?
C58 C45 H45A 109.5 . . ?
C58 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C58 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N4 C47 C26 110.3(3) . . ?
N4 C47 H47A 109.6 . . ?
C26 C47 H47A 109.6 . . ?
N4 C47 H47B 109.6 . . ?
C26 C47 H47B 109.6 . . ?
H47A C47 H47B 108.1 . . ?
N8AA C49 C3AA 112.1(3) . . ?
N8AA C49 H49A 109.2 . . ?
C3AA C49 H49A 109.2 . . ?
N8AA C49 H49B 109.2 . . ?
C3AA C49 H49B 109.2 . . ?
H49A C49 H49B 107.9 . . ?
N13 C51 C32 113.8(3) . . ?
N13 C51 H51A 108.8 . . ?
C32 C51 H51A 108.8 . . ?
N13 C51 H51B 108.8 . . ?
C32 C51 H51B 108.8 . . ?
H51A C51 H51B 107.7 . . ?
N7AA C54 C44 113.8(3) . . ?
N7AA C54 H54A 108.8 . . ?
C44 C54 H54A 108.8 . . ?
N7AA C54 H54B 108.8 . . ?
C44 C54 H54B 108.8 . . ?
H54A C54 H54B 107.7 . . ?
N9AA C57 C7AA 112.1(3) . . ?
N9AA C57 H57A 109.2 . . ?
C7AA C57 H57A 109.2 . . ?
N9AA C57 H57B 109.2 . . ?
C7AA C57 H57B 109.2 . . ?
H57A C57 H57B 107.9 . . ?
N16 C58 C45 179.4(5) . . ?
N7AA C59 C40 109.9(4) . . ?
N7AA C59 H59A 109.7 . . ?
C40 C59 H59A 109.7 . . ?
N7AA C59 H59B 109.7 . . ?
C40 C59 H59B 109.7 . . ?
H59A C59 H59B 108.2 . . ?
N9AA C65 C66 109.0(4) . . ?
N9AA C65 H65A 109.9 . . ?
C66 C65 H65A 109.9 . . ?
N9AA C65 H65B 109.9 . . ?
C66 C65 H65B 109.9 . . ?
H65A C65 H65B 108.3 . . ?
N5AA C66 C65 110.2(3) . . ?
N5AA C66 H66A 109.6 . . ?
C65 C66 H66A 109.6 . . ?
N5AA C66 H66B 109.6 . . ?
C65 C66 H66B 109.6 . . ?
H66A C66 H66B 108.1 . . ?
O4AA Cl5 O2AA 118.3(5) . . ?
O5 Cl5 O2AA 123.0(5) . . ?
O4AA Cl5 O1AA 119.0(5) . . ?
O5 Cl5 O1AA 113.5(5) . . ?
O2AA Cl5 O1AA 111.8(2) . . ?
O5 Cl5 O3 104.9(7) . . ?
O2AA Cl5 O3 98.4(5) . . ?
O1AA Cl5 O3 101.0(4) . . ?
O4AA Cl5 O6 106.0(7) . . ?
O2AA Cl5 O6 95.0(4) . . ?
O1AA Cl5 O6 101.8(4) . . ?
C9 C4AA C14 107.9(4) . . ?
C9 C4AA C7 108.4(4) . . ?
C14 C4AA C7 111.1(4) . . ?
C9 C4AA C8 109.0(4) . . ?
C14 C4AA C8 112.6(4) . . ?
C7 C4AA C8 107.8(5) . . ?
C15 C5AA C8AA 107.7(4) . . ?
C15 C5AA C27 113.6(4) . . ?
C8AA C5AA C27 110.3(4) . . ?
C15 C5AA C10 108.1(5) . . ?
C8AA C5AA C10 108.0(4) . . ?
C27 C5AA C10 108.9(4) . . ?
C5AA C8AA H8AB 109.5 . . ?
C5AA C8AA H8AC 109.5 . . ?
H8AB C8AA H8AC 109.5 . . ?
C5AA C8AA H8AD 109.5 . . ?
H8AB C8AA H8AD 109.5 . . ?
H8AC C8AA H8AD 109.5 . . ?
C18 C6 C24 113.7(5) . . ?
C18 C6 C11 107.1(5) . . ?
C24 C6 C11 109.9(4) . . ?
C18 C6 C6AA 113.1(5) . . ?
C24 C6 C6AA 110.1(4) . . ?
C11 C6 C6AA 102.3(5) . . ?
C4AA C7 H7A 109.5 . . ?
C4AA C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4AA C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4AA C8 H8A 109.5 . . ?
C4AA C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4AA C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4AA C9 H9A 109.5 . . ?
C4AA C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C4AA C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5AA C10 H10A 109.5 . . ?
C5AA C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C5AA C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C6 C11 H11A 109.5 . . ?
C6 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C6 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C6 C6AA H6AB 109.5 . . ?
C6 C6AA H6AC 109.5 . . ?
H6AB C6AA H6AC 109.5 . . ?
C6 C6AA H6AD 109.5 . . ?
H6AB C6AA H6AD 109.5 . . ?
H6AC C6AA H6AD 109.5 . . ?
C5AA C15 H15A 109.5 . . ?
C5AA C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C5AA C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C6 C18 H18A 109.5 . . ?
C6 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C6 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 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
C47 N4 C2AA C28 171.2(3) . . . . ?
Ni2 N4 C2AA C28 -74.4(4) . . . . ?
C28 C9AA C20 C33 -0.4(6) . . . . ?
C28 C9AA C20 C41 -172.8(4) . . . . ?
C30 C1AA C23 C32 -0.6(6) . . . . ?
C35 C1AA C23 C32 -179.4(4) . . . . ?
C28 C17 C24 C33 0.9(6) . . . . ?
C28 C17 C24 C6 -178.7(4) . . . . ?
C34 C7AA C25 C3AA -0.2(6) . . . . ?
C57 C7AA C25 C3AA 178.6(4) . . . . ?
C31 C3AA C25 C7AA -0.3(6) . . . . ?
C49 C3AA C25 C7AA 178.8(4) . . . . ?
C38 N5AA C26 C47 132.3(4) . . . . ?
C66 N5AA C26 C47 -102.0(4) . . . . ?
Ni2 N5AA C26 C47 13.0(4) . . . . ?
C24 C17 C28 C9AA -2.4(6) . . . . ?
C24 C17 C28 C2AA -175.2(4) . . . . ?
C20 C9AA C28 C17 2.1(6) . . . . ?
C20 C9AA C28 C2AA 174.9(3) . . . . ?
N4 C2AA C28 C17 -61.6(5) . . . . ?
N4 C2AA C28 C9AA 125.5(4) . . . . ?
C41 N6AA C29 C37 164.0(4) . . . . ?
Ni1 N6AA C29 C37 20.2(4) . . . . ?
C36 C14 C30 C1AA -2.2(6) . . . . ?
C4AA C14 C30 C1AA -178.6(4) . . . . ?
C23 C1AA C30 C14 1.7(6) . . . . ?
C35 C1AA C30 C14 -179.6(4) . . . . ?
C25 C3AA C31 C27 0.9(6) . . . . ?
C49 C3AA C31 C27 -178.3(4) . . . . ?
C34 C27 C31 C3AA -0.8(6) . . . . ?
C5AA C27 C31 C3AA 178.8(4) . . . . ?
C1AA C23 C32 C36 0.1(6) . . . . ?
C1AA C23 C32 C51 177.9(4) . . . . ?
C9AA C20 C33 C24 -1.1(6) . . . . ?
C41 C20 C33 C24 171.8(4) . . . . ?
C17 C24 C33 C20 0.9(6) . . . . ?
C6 C24 C33 C20 -179.5(4) . . . . ?
C25 C7AA C34 C27 0.3(6) . . . . ?
C57 C7AA C34 C27 -178.5(4) . . . . ?
C31 C27 C34 C7AA 0.3(6) . . . . ?
C5AA C27 C34 C7AA -179.3(4) . . . . ?
C44 N4AA C35 C1AA -172.1(3) . . . . ?
Ni1 N4AA C35 C1AA 67.6(4) . . . . ?
C23 C1AA C35 N4AA -120.3(4) . . . . ?
C30 C1AA C35 N4AA 61.0(5) . . . . ?
C30 C14 C36 C32 1.6(6) . . . . ?
C4AA C14 C36 C32 178.2(4) . . . . ?
C23 C32 C36 C14 -0.6(6) . . . . ?
C51 C32 C36 C14 -178.5(4) . . . . ?
C59 N7AA C37 C29 167.6(3) . . . . ?
C54 N7AA C37 C29 -67.1(4) . . . . ?
Ni1 N7AA C37 C29 50.9(4) . . . . ?
N6AA C29 C37 N7AA -48.4(5) . . . . ?
C26 N5AA C38 C39 -84.4(4) . . . . ?
C66 N5AA C38 C39 149.7(3) . . . . ?
Ni2 N5AA C38 C39 35.3(4) . . . . ?
C51 N13 C39 C38 176.7(3) . . . . ?
Ni2 N13 C39 C38 44.8(4) . . . . ?
N5AA C38 C39 N13 -54.4(4) . . . . ?
C49 N8AA C40 C59 -175.3(3) . . . . ?
Ni1 N8AA C40 C59 -38.2(4) . . . . ?
C29 N6AA C41 C20 174.0(4) . . . . ?
Ni1 N6AA C41 C20 -54.1(5) . . . . ?
C33 C20 C41 N6AA 146.3(4) . . . . ?
C9AA C20 C41 N6AA -41.1(6) . . . . ?
C35 N4AA C44 C54 -178.5(3) . . . . ?
Ni1 N4AA C44 C54 -45.9(3) . . . . ?
C2AA N4 C47 C26 -176.6(3) . . . . ?
Ni2 N4 C47 C26 54.1(3) . . . . ?
N5AA C26 C47 N4 -47.8(5) . . . . ?
C40 N8AA C49 C3AA -144.1(4) . . . . ?
Ni1 N8AA C49 C3AA 86.7(4) . . . . ?
C25 C3AA C49 N8AA -114.3(4) . . . . ?
C31 C3AA C49 N8AA 64.8(5) . . . . ?
C39 N13 C51 C32 160.7(3) . . . . ?
Ni2 N13 C51 C32 -75.4(4) . . . . ?
C23 C32 C51 N13 124.2(4) . . . . ?
C36 C32 C51 N13 -58.0(5) . . . . ?
C59 N7AA C54 C44 -135.8(4) . . . . ?
C37 N7AA C54 C44 98.7(4) . . . . ?
Ni1 N7AA C54 C44 -18.0(4) . . . . ?
N4AA C44 C54 N7AA 44.9(5) . . . . ?
C65 N9AA C57 C7AA 135.8(4) . . . . ?
Ni2 N9AA C57 C7AA -92.4(4) . . . . ?
C25 C7AA C57 N9AA 113.1(4) . . . . ?
C34 C7AA C57 N9AA -68.1(5) . . . . ?
C37 N7AA C59 C40 -157.9(3) . . . . ?
C54 N7AA C59 C40 75.1(4) . . . . ?
Ni1 N7AA C59 C40 -42.6(4) . . . . ?
N8AA C40 C59 N7AA 55.5(4) . . . . ?
C57 N9AA C65 C66 164.3(4) . . . . ?
Ni2 N9AA C65 C66 26.0(4) . . . . ?
C26 N5AA C66 C65 169.4(4) . . . . ?
C38 N5AA C66 C65 -65.5(5) . . . . ?
Ni2 N5AA C66 C65 51.5(4) . . . . ?
N9AA C65 C66 N5AA -52.7(5) . . . . ?
C30 C14 C4AA C9 89.4(5) . . . . ?
C36 C14 C4AA C9 -87.0(5) . . . . ?
C30 C14 C4AA C7 -29.3(6) . . . . ?
C36 C14 C4AA C7 154.3(4) . . . . ?
C30 C14 C4AA C8 -150.3(5) . . . . ?
C36 C14 C4AA C8 33.3(7) . . . . ?
C34 C27 C5AA C15 -169.6(5) . . . . ?
C31 C27 C5AA C15 10.8(6) . . . . ?
C34 C27 C5AA C8AA -48.6(6) . . . . ?
C31 C27 C5AA C8AA 131.8(4) . . . . ?
C34 C27 C5AA C10 69.8(5) . . . . ?
C31 C27 C5AA C10 -109.8(5) . . . . ?
C17 C24 C6 C18 -171.5(6) . . . . ?
C33 C24 C6 C18 8.9(8) . . . . ?
C17 C24 C6 C11 -51.6(6) . . . . ?
C33 C24 C6 C11 128.8(5) . . . . ?
C17 C24 C6 C6AA 60.4(6) . . . . ?
C33 C24 C6 C6AA -119.2(5) . . . . ?

_refine_diff_density_max         0.599
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.056

####################################################################### 
# 
# 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_added_by_encifer
_database_code_depnum_ccdc_archive 'CCDC 1418424'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2015-12-08 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            'C41 H63 Cl3 N10 Ni2 O12'
_chemical_formula_weight         1111.78

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/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   17.1218(13)
_cell_length_b                   15.9325(14)
_cell_length_c                   19.4659(15)
_cell_angle_alpha                90
_cell_angle_beta                 115.046(8)
_cell_angle_gamma                90
_cell_volume                     4810.8(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9334
_cell_measurement_theta_min      2.119
_cell_measurement_theta_max      25.984

_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_F_000             2328
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.020
_shelx_estimated_absorpt_T_min   0.822
_shelx_estimated_absorpt_T_max   0.905
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37246
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.119
_diffrn_reflns_theta_max         25.984
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9334
_reflns_number_gt                6692
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_solution    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (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)+(0.0524P)²] 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         9334
_refine_ls_number_parameters     624
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0342
_refine_ls_wR_factor_ref         0.0876
_refine_ls_wR_factor_gt          0.0834
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_restrained_S_all      0.961
_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 0.15737(2) 0.31370(2) 0.44419(2) 0.01547(8) Uani 1 1 d . . . . .
Ni2 Ni 0.30082(2) 0.61556(2) 0.66203(2) 0.01940(8) Uani 1 1 d . . . . .
Cl3 Cl 0.39597(4) 0.25315(4) 0.31823(3) 0.02840(15) Uani 1 1 d . . . . .
Cl4 Cl 0.13108(4) 0.67213(4) 0.59738(4) 0.02761(14) Uani 1 1 d . . . . .
O6 O 0.26795(11) 0.51155(10) 0.59947(9) 0.0208(4) Uani 1 1 d . . . . .
O7 O 0.21892(11) 0.40353(10) 0.52136(8) 0.0195(4) Uani 1 1 d . . . . .
O8 O 0.04134(11) 0.39039(11) 0.40553(10) 0.0226(4) Uani 1 1 d . . . . .
H8A H -0.0010 0.3606 0.4044 0.034 Uiso 1 1 d R U . . .
O9 O 0.45963(14) 0.31403(13) 0.36235(11) 0.0420(5) Uani 1 1 d . . . . .
O10 O 0.12880(12) 0.50604(12) 0.51425(11) 0.0311(5) Uani 1 1 d . . . . .
O11 O 0.34165(13) 0.23350(13) 0.35514(11) 0.0394(5) Uani 1 1 d . . . . .
N12 N 0.10268(13) 0.21467(12) 0.36837(10) 0.0191(4) Uani 1 1 d . . . . .
N13 N 0.27401(13) 0.24549(12) 0.47569(10) 0.0180(4) Uani 1 1 d . . . . .
H13 H 0.3004 0.2646 0.4413 0.022 Uiso 1 1 calc R U . . .
N14 N 0.43495(13) 0.58445(12) 0.71048(11) 0.0211(4) Uani 1 1 d . . . . .
H14 H 0.4598 0.6105 0.6774 0.025 Uiso 1 1 calc R U . . .
N15 N 0.25910(14) 0.57448(13) 0.74606(11) 0.0227(4) Uani 1 1 d . . . . .
H15 H 0.1963 0.5888 0.7225 0.027 Uiso 1 1 calc R U . . .
N16 N 0.16184(13) 0.37333(12) 0.34550(10) 0.0195(4) Uani 1 1 d . . . . .
H16 H 0.1132 0.4145 0.3286 0.023 Uiso 1 1 calc R U . . .
N17 N 0.34118(14) 0.72204(13) 0.73106(12) 0.0251(5) Uani 1 1 d . . . . .
C18 C 0.21286(17) 0.68081(16) 0.40049(14) 0.0260(6) Uani 1 1 d . . . . .
H18 H 0.2070 0.7378 0.4120 0.031 Uiso 1 1 calc R U . . .
N19 N 0.09820(14) 0.24756(12) 0.50866(10) 0.0214(4) Uani 1 1 d . . . . .
H19 H 0.0447 0.2810 0.4971 0.026 Uiso 1 1 calc R U . . .
C20 C 0.17139(16) 0.15212(15) 0.37787(14) 0.0234(5) Uani 1 1 d . . . . .
H20A H 0.1922 0.1617 0.3382 0.028 Uiso 1 1 calc R U . . .
H20B H 0.1464 0.0950 0.3706 0.028 Uiso 1 1 calc R U . . .
C21 C 0.27815(16) 0.63151(15) 0.45275(13) 0.0214(5) Uani 1 1 d . . . . .
O22 O 0.34649(17) 0.28616(16) 0.24463(12) 0.0600(7) Uani 1 1 d . . . . .
N23 N 0.30283(14) 0.69743(12) 0.57656(11) 0.0227(5) Uani 1 1 d . . . . .
H23 H 0.2409 0.7083 0.5423 0.027 Uiso 1 1 calc R U . . .
C24 C 0.29466(19) 0.63349(18) 0.81131(15) 0.0330(7) Uani 1 1 d . . . . .
H24A H 0.3538 0.6162 0.8462 0.040 Uiso 1 1 calc R U . . .
H24B H 0.2584 0.6325 0.8397 0.040 Uiso 1 1 calc R U . . .
O25 O 0.43825(15) 0.17776(14) 0.31168(14) 0.0505(6) Uani 1 1 d . . . . .
C26 C 0.40398(16) 0.37722(15) 0.63309(12) 0.0200(5) Uani 1 1 d . . . . .
H26 H 0.3698 0.3641 0.6594 0.024 Uiso 1 1 calc R U . . .
C27 C 0.28466(16) 0.54771(15) 0.43556(13) 0.0204(5) Uani 1 1 d . . . . .
H27 H 0.3279 0.5132 0.4716 0.024 Uiso 1 1 calc R U . . .
C28 C 0.13543(19) 0.23962(16) 0.59273(13) 0.0261(6) Uani 1 1 d . . . . .
H28A H 0.1976 0.2263 0.6123 0.031 Uiso 1 1 calc R U . . .
H28B H 0.1069 0.1927 0.6065 0.031 Uiso 1 1 calc R U . . .
C29 C 0.03291(17) 0.17807(16) 0.38517(14) 0.0253(6) Uani 1 1 d . . . . .
H29A H 0.0155 0.1231 0.3595 0.030 Uiso 1 1 calc R U . . .
H29B H -0.0179 0.2156 0.3655 0.030 Uiso 1 1 calc R U . . .
C30 C 0.06346(19) 0.16665(15) 0.46998(14) 0.0273(6) Uani 1 1 d . . . . .
H30A H 0.0148 0.1482 0.4811 0.033 Uiso 1 1 calc R U . . .
H30B H 0.1088 0.1230 0.4887 0.033 Uiso 1 1 calc R U . . .
C31 C 0.12416(17) 0.31913(15) 0.62925(12) 0.0209(5) Uani 1 1 d . . . . .
C32 C 0.45845(16) 0.44677(15) 0.65565(13) 0.0206(5) Uani 1 1 d . . . . .
C33 C 0.18307(16) 0.43768(15) 0.71412(12) 0.0207(5) Uani 1 1 d . . . . .
C34 C 0.47237(18) 0.62987(17) 0.78376(14) 0.0276(6) Uani 1 1 d . . . . .
H34A H 0.5359 0.6320 0.8026 0.033 Uiso 1 1 calc R U . . .
H34B H 0.4586 0.5993 0.8216 0.033 Uiso 1 1 calc R U . . .
C35 C 0.19436(17) 0.36476(15) 0.67940(13) 0.0216(5) Uani 1 1 d . . . . .
H35 H 0.2511 0.3460 0.6903 0.026 Uiso 1 1 calc R U . . .
C36 C 0.02947(17) 0.42005(15) 0.64726(13) 0.0229(5) Uani 1 1 d . . . . .
H36 H -0.0272 0.4393 0.6359 0.028 Uiso 1 1 calc R U . . .
C37 C 0.16452(18) 0.56465(17) 0.31459(14) 0.0280(6) Uani 1 1 d . . . . .
H37 H 0.1260 0.5423 0.2670 0.034 Uiso 1 1 calc R U . . .
C38 C 0.39838(15) 0.32655(15) 0.57305(12) 0.0197(5) Uani 1 1 d . . . . .
C39 C 0.15652(18) 0.64721(17) 0.33195(15) 0.0294(6) Uani 1 1 d . . . . .
H39 H 0.1120 0.6811 0.2966 0.035 Uiso 1 1 calc R U . . .
C40 C 0.50259(18) 0.41521(17) 0.55594(15) 0.0296(6) Uani 1 1 d . . . . .
H40 H 0.5362 0.4284 0.5291 0.035 Uiso 1 1 calc R U . . .
C41 C 0.23632(18) 0.42329(15) 0.34743(15) 0.0261(6) Uani 1 1 d . . . . .
H41A H 0.2385 0.4199 0.2975 0.031 Uiso 1 1 calc R U . . .
H41B H 0.2906 0.3995 0.3860 0.031 Uiso 1 1 calc R U . . .
C42 C 0.09996(17) 0.46454(15) 0.69772(13) 0.0226(5) Uani 1 1 d . . . . .
H42 H 0.0913 0.5137 0.7212 0.027 Uiso 1 1 calc R U . . .
C43 C 0.31550(19) 0.79492(16) 0.67971(16) 0.0321(6) Uani 1 1 d . . . . .
H43A H 0.3460 0.8457 0.7075 0.038 Uiso 1 1 calc R U . . .
H43B H 0.2527 0.8046 0.6611 0.038 Uiso 1 1 calc R U . . .
C44 C 0.04113(17) 0.34735(16) 0.61315(13) 0.0229(5) Uani 1 1 d . . . . .
H44 H -0.0075 0.3169 0.5789 0.027 Uiso 1 1 calc R U . . .
C45 C 0.50822(17) 0.46548(16) 0.61654(15) 0.0279(6) Uani 1 1 d . . . . .
H45 H 0.5460 0.5124 0.6312 0.034 Uiso 1 1 calc R U . . .
C46 C 0.22856(16) 0.51388(15) 0.36617(13) 0.0215(5) Uani 1 1 d . . . . .
C47 C 0.34281(17) 0.66919(17) 0.52548(14) 0.0276(6) Uani 1 1 d . . . . .
H47A H 0.3880 0.6271 0.5524 0.033 Uiso 1 1 calc R U . . .
H47B H 0.3709 0.7178 0.5134 0.033 Uiso 1 1 calc R U . . .
C48 C 0.20929(15) 0.47255(14) 0.54707(12) 0.0171(5) Uani 1 1 d . . . . .
C49 C 0.34385(16) 0.24821(15) 0.55450(13) 0.0232(5) Uani 1 1 d . . . . .
H49A H 0.3818 0.1989 0.5621 0.028 Uiso 1 1 calc R U . . .
H49B H 0.3173 0.2433 0.5907 0.028 Uiso 1 1 calc R U . . .
C51 C 0.44832(17) 0.34616(16) 0.53453(13) 0.0238(5) Uani 1 1 d . . . . .
H51 H 0.4452 0.3121 0.4934 0.029 Uiso 1 1 calc R U . . .
C52 C 0.43676(17) 0.71866(17) 0.77466(15) 0.0290(6) Uani 1 1 d . . . . .
H52A H 0.4527 0.7433 0.8255 0.035 Uiso 1 1 calc R U . . .
H52B H 0.4638 0.7532 0.7483 0.035 Uiso 1 1 calc R U . . .
C53 C 0.46674(18) 0.49590(16) 0.72460(13) 0.0260(6) Uani 1 1 d . . . . .
H53A H 0.4347 0.4657 0.7491 0.031 Uiso 1 1 calc R U . . .
H53B H 0.5283 0.4967 0.7610 0.031 Uiso 1 1 calc R U . . .
C54 C 0.29621(19) 0.72120(18) 0.78214(16) 0.0341(7) Uani 1 1 d . . . . .
H54A H 0.2364 0.7417 0.7541 0.041 Uiso 1 1 calc R U . . .
H54B H 0.3263 0.7594 0.8255 0.041 Uiso 1 1 calc R U . . .
C55 C 0.06775(17) 0.25153(15) 0.29086(13) 0.0235(5) Uani 1 1 d . . . . .
H55A H 0.0143 0.2831 0.2812 0.028 Uiso 1 1 calc R U . . .
H55B H 0.0533 0.2061 0.2528 0.028 Uiso 1 1 calc R U . . .
C56 C 0.25935(17) 0.48585(17) 0.77026(14) 0.0272(6) Uani 1 1 d . . . . .
H56A H 0.2579 0.4848 0.8205 0.033 Uiso 1 1 calc R U . . .
H56B H 0.3133 0.4582 0.7753 0.033 Uiso 1 1 calc R U . . .
C57 C 0.24750(17) 0.15710(15) 0.45546(14) 0.0254(6) Uani 1 1 d . . . . .
H57A H 0.2312 0.1320 0.4941 0.031 Uiso 1 1 calc R U . . .
H57B H 0.2965 0.1246 0.4549 0.031 Uiso 1 1 calc R U . . .
C58 C 0.3376(2) 0.77924(16) 0.61235(16) 0.0318(6) Uani 1 1 d . . . . .
H58A H 0.3130 0.8247 0.5746 0.038 Uiso 1 1 calc R U . . .
H58B H 0.4010 0.7798 0.6299 0.038 Uiso 1 1 calc R U . . .
C59 C 0.13386(18) 0.30993(16) 0.28339(13) 0.0263(6) Uani 1 1 d . . . . .
H59A H 0.1843 0.2771 0.2863 0.032 Uiso 1 1 calc R U . . .
H59B H 0.1083 0.3386 0.2336 0.032 Uiso 1 1 calc R U . . .
C61 C 0.1431(3) 0.5307(3) 0.1049(2) 0.0709(12) Uani 1 1 d . . . . .
H61A H 0.1145 0.5448 0.0508 0.106 Uiso 1 1 calc R U . . .
H61B H 0.1487 0.5813 0.1351 0.106 Uiso 1 1 calc R U . . .
H61C H 0.1088 0.4888 0.1168 0.106 Uiso 1 1 calc R U . . .
N63 N 0.5186(3) 0.1326(3) 0.5213(2) 0.0833(12) Uani 1 1 d . . . . .
C64 C 0.5471(3) 0.0934(3) 0.4892(2) 0.0602(10) Uani 1 1 d . . . . .
N65 N 0.2926(3) 0.4712(3) 0.1331(2) 0.0902(12) Uani 1 1 d . . . . .
C66 C 0.2274(3) 0.4970(2) 0.1222(2) 0.0550(9) Uani 1 1 d . . . . .
C67 C 0.5859(3) 0.0416(3) 0.4503(3) 0.0822(14) Uani 1 1 d . . . . .
H67A H 0.5674 0.0618 0.3981 0.123 Uiso 1 1 calc R U . . .
H67B H 0.5676 -0.0168 0.4494 0.123 Uiso 1 1 calc R U . . .
H67C H 0.6488 0.0450 0.4770 0.123 Uiso 1 1 calc R U . . .
Cl1 Cl 0.09212(7) 0.90470(5) 0.38971(6) 0.0602(3) Uani 1 1 d . . . . .
O0AA O 0.1001(2) 0.86758(19) 0.32728(17) 0.0805(9) Uani 1 1 d . . . . .
O3 O 0.1697(3) 0.9462(2) 0.43060(19) 0.1083(13) Uani 1 1 d . . . . .
H10 H 0.127(2) 0.550(2) 0.5344(19) 0.046(10) Uiso 1 1 d . . . . .
H8B H 0.054(2) 0.429(2) 0.4321(19) 0.043(10) Uiso 1 1 d . . . . .
O1 O 0.0778(4) 0.8400(2) 0.4310(3) 0.163(2) Uani 1 1 d . . . . .
O2 O 0.0279(3) 0.9619(2) 0.3681(5) 0.243(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O7 2.0187(15) . ?
Ni1 N12 2.0915(19) . ?
Ni1 N13 2.123(2) . ?
Ni1 N16 2.1735(19) . ?
Ni1 O8 2.1772(18) . ?
Ni1 N19 2.1881(19) . ?
Ni2 O6 1.9913(15) . ?
Ni2 N17 2.092(2) . ?
Ni2 N23 2.126(2) . ?
Ni2 N14 2.139(2) . ?
Ni2 N15 2.145(2) . ?
Cl3 O22 1.421(2) . ?
Cl3 O11 1.4299(19) . ?
Cl3 O25 1.436(2) . ?
Cl3 O9 1.4401(19) . ?
O6 C48 1.252(3) . ?
O7 C48 1.248(3) . ?
O8 H8A 0.8595 . ?
O8 H8B 0.78(3) . ?
O10 C48 1.359(3) . ?
O10 H10 0.80(3) . ?
N12 C29 1.485(3) . ?
N12 C55 1.488(3) . ?
N12 C20 1.492(3) . ?
N13 C57 1.481(3) . ?
N13 C49 1.494(3) . ?
N13 H13 1.0000 . ?
N14 C34 1.482(3) . ?
N14 C53 1.495(3) . ?
N14 H14 1.0000 . ?
N15 C24 1.488(3) . ?
N15 C56 1.488(3) . ?
N15 H15 1.0000 . ?
N16 C41 1.490(3) . ?
N16 C59 1.490(3) . ?
N16 H16 1.0000 . ?
N17 C43 1.473(3) . ?
N17 C52 1.492(3) . ?
N17 C54 1.493(3) . ?
C18 C39 1.381(4) . ?
C18 C21 1.392(3) . ?
C18 H18 0.9500 . ?
N19 C30 1.484(3) . ?
N19 C28 1.489(3) . ?
N19 H19 1.0000 . ?
C20 C57 1.523(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C27 1.392(3) . ?
C21 C47 1.504(3) . ?
N23 C58 1.479(3) . ?
N23 C47 1.495(3) . ?
N23 H23 1.0000 . ?
C24 C54 1.513(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C26 C38 1.390(3) . ?
C26 C32 1.394(3) . ?
C26 H26 0.9500 . ?
C27 C46 1.393(3) . ?
C27 H27 0.9500 . ?
C28 C31 1.505(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.517(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C35 1.390(4) . ?
C31 C44 1.394(4) . ?
C32 C45 1.394(4) . ?
C32 C53 1.508(3) . ?
C33 C42 1.387(4) . ?
C33 C35 1.398(3) . ?
C33 C56 1.510(3) . ?
C34 C52 1.521(4) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35 0.9500 . ?
C36 C42 1.386(4) . ?
C36 C44 1.391(3) . ?
C36 H36 0.9500 . ?
C37 C39 1.379(4) . ?
C37 C46 1.390(4) . ?
C37 H37 0.9500 . ?
C38 C51 1.391(3) . ?
C38 C49 1.508(3) . ?
C39 H39 0.9500 . ?
C40 C51 1.385(4) . ?
C40 C45 1.395(4) . ?
C40 H40 0.9500 . ?
C41 C46 1.508(3) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42 0.9500 . ?
C43 C58 1.532(4) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C51 H51 0.9500 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C59 1.519(4) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C61 C66 1.438(6) . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
N63 C64 1.130(5) . ?
C64 C67 1.457(6) . ?
N65 C66 1.123(5) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
Cl1 O2 1.350(4) . ?
Cl1 O1 1.391(3) . ?
Cl1 O3 1.393(4) . ?
Cl1 O0AA 1.410(3) . ?

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
O7 Ni1 N12 175.33(7) . . ?
O7 Ni1 N13 90.98(7) . . ?
N12 Ni1 N13 84.44(8) . . ?
O7 Ni1 N16 98.35(7) . . ?
N12 Ni1 N16 83.03(7) . . ?
N13 Ni1 N16 95.63(8) . . ?
O7 Ni1 O8 88.39(7) . . ?
N12 Ni1 O8 96.26(8) . . ?
N13 Ni1 O8 174.93(7) . . ?
N16 Ni1 O8 79.48(7) . . ?
O7 Ni1 N19 97.89(7) . . ?
N12 Ni1 N19 82.17(7) . . ?
N13 Ni1 N19 101.26(8) . . ?
N16 Ni1 N19 156.28(8) . . ?
O8 Ni1 N19 83.82(7) . . ?
O6 Ni2 N17 177.18(8) . . ?
O6 Ni2 N23 97.23(7) . . ?
N17 Ni2 N23 83.95(8) . . ?
O6 Ni2 N14 92.84(7) . . ?
N17 Ni2 N14 84.47(8) . . ?
N23 Ni2 N14 96.73(8) . . ?
O6 Ni2 N15 96.51(7) . . ?
N17 Ni2 N15 83.33(8) . . ?
N23 Ni2 N15 154.78(8) . . ?
N14 Ni2 N15 103.59(8) . . ?
O22 Cl3 O11 110.53(15) . . ?
O22 Cl3 O25 109.14(15) . . ?
O11 Cl3 O25 108.73(13) . . ?
O22 Cl3 O9 109.24(14) . . ?
O11 Cl3 O9 109.69(12) . . ?
O25 Cl3 O9 109.50(14) . . ?
C48 O6 Ni2 146.38(16) . . ?
C48 O7 Ni1 143.84(16) . . ?
Ni1 O8 H8A 109.6 . . ?
Ni1 O8 H8B 105(3) . . ?
H8A O8 H8B 117.1 . . ?
C48 O10 H10 110(2) . . ?
C29 N12 C55 111.3(2) . . ?
C29 N12 C20 112.08(19) . . ?
C55 N12 C20 110.28(18) . . ?
C29 N12 Ni1 107.60(14) . . ?
C55 N12 Ni1 106.59(14) . . ?
C20 N12 Ni1 108.81(14) . . ?
C57 N13 C49 108.82(18) . . ?
C57 N13 Ni1 105.37(15) . . ?
C49 N13 Ni1 121.86(15) . . ?
C57 N13 H13 106.6 . . ?
C49 N13 H13 106.6 . . ?
Ni1 N13 H13 106.6 . . ?
C34 N14 C53 107.97(19) . . ?
C34 N14 Ni2 104.91(15) . . ?
C53 N14 Ni2 122.61(16) . . ?
C34 N14 H14 106.8 . . ?
C53 N14 H14 106.8 . . ?
Ni2 N14 H14 106.8 . . ?
C24 N15 C56 112.59(19) . . ?
C24 N15 Ni2 108.07(15) . . ?
C56 N15 Ni2 124.99(16) . . ?
C24 N15 H15 102.7 . . ?
C56 N15 H15 102.7 . . ?
Ni2 N15 H15 102.7 . . ?
C41 N16 C59 111.11(19) . . ?
C41 N16 Ni1 124.14(15) . . ?
C59 N16 Ni1 107.53(14) . . ?
C41 N16 H16 104.0 . . ?
C59 N16 H16 104.0 . . ?
Ni1 N16 H16 104.0 . . ?
C43 N17 C52 110.8(2) . . ?
C43 N17 C54 111.7(2) . . ?
C52 N17 C54 111.8(2) . . ?
C43 N17 Ni2 106.32(15) . . ?
C52 N17 Ni2 108.71(15) . . ?
C54 N17 Ni2 107.29(15) . . ?
C39 C18 C21 120.2(2) . . ?
C39 C18 H18 119.9 . . ?
C21 C18 H18 119.9 . . ?
C30 N19 C28 112.14(19) . . ?
C30 N19 Ni1 108.10(14) . . ?
C28 N19 Ni1 125.76(16) . . ?
C30 N19 H19 102.5 . . ?
C28 N19 H19 102.5 . . ?
Ni1 N19 H19 102.5 . . ?
N12 C20 C57 112.75(19) . . ?
N12 C20 H20A 109.0 . . ?
C57 C20 H20A 109.0 . . ?
N12 C20 H20B 109.0 . . ?
C57 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
C27 C21 C18 119.1(2) . . ?
C27 C21 C47 120.5(2) . . ?
C18 C21 C47 120.4(2) . . ?
C58 N23 C47 111.8(2) . . ?
C58 N23 Ni2 107.99(15) . . ?
C47 N23 Ni2 119.96(16) . . ?
C58 N23 H23 105.3 . . ?
C47 N23 H23 105.3 . . ?
Ni2 N23 H23 105.3 . . ?
N15 C24 C54 109.2(2) . . ?
N15 C24 H24A 109.8 . . ?
C54 C24 H24A 109.8 . . ?
N15 C24 H24B 109.8 . . ?
C54 C24 H24B 109.8 . . ?
H24A C24 H24B 108.3 . . ?
C38 C26 C32 121.7(2) . . ?
C38 C26 H26 119.2 . . ?
C32 C26 H26 119.2 . . ?
C21 C27 C46 120.8(2) . . ?
C21 C27 H27 119.6 . . ?
C46 C27 H27 119.6 . . ?
N19 C28 C31 111.5(2) . . ?
N19 C28 H28A 109.3 . . ?
C31 C28 H28A 109.3 . . ?
N19 C28 H28B 109.3 . . ?
C31 C28 H28B 109.3 . . ?
H28A C28 H28B 108.0 . . ?
N12 C29 C30 110.4(2) . . ?
N12 C29 H29A 109.6 . . ?
C30 C29 H29A 109.6 . . ?
N12 C29 H29B 109.6 . . ?
C30 C29 H29B 109.6 . . ?
H29A C29 H29B 108.1 . . ?
N19 C30 C29 109.11(19) . . ?
N19 C30 H30A 109.9 . . ?
C29 C30 H30A 109.9 . . ?
N19 C30 H30B 109.9 . . ?
C29 C30 H30B 109.9 . . ?
H30A C30 H30B 108.3 . . ?
C35 C31 C44 119.0(2) . . ?
C35 C31 C28 121.8(2) . . ?
C44 C31 C28 119.2(2) . . ?
C45 C32 C26 118.7(2) . . ?
C45 C32 C53 121.7(2) . . ?
C26 C32 C53 119.4(2) . . ?
C42 C33 C35 118.9(2) . . ?
C42 C33 C56 119.9(2) . . ?
C35 C33 C56 121.2(2) . . ?
N14 C34 C52 110.7(2) . . ?
N14 C34 H34A 109.5 . . ?
C52 C34 H34A 109.5 . . ?
N14 C34 H34B 109.5 . . ?
C52 C34 H34B 109.5 . . ?
H34A C34 H34B 108.1 . . ?
C31 C35 C33 121.2(2) . . ?
C31 C35 H35 119.4 . . ?
C33 C35 H35 119.4 . . ?
C42 C36 C44 120.4(2) . . ?
C42 C36 H36 119.8 . . ?
C44 C36 H36 119.8 . . ?
C39 C37 C46 120.5(2) . . ?
C39 C37 H37 119.7 . . ?
C46 C37 H37 119.7 . . ?
C26 C38 C51 118.9(2) . . ?
C26 C38 C49 119.8(2) . . ?
C51 C38 C49 121.1(2) . . ?
C37 C39 C18 120.3(2) . . ?
C37 C39 H39 119.8 . . ?
C18 C39 H39 119.8 . . ?
C51 C40 C45 120.5(2) . . ?
C51 C40 H40 119.7 . . ?
C45 C40 H40 119.7 . . ?
N16 C41 C46 110.8(2) . . ?
N16 C41 H41A 109.5 . . ?
C46 C41 H41A 109.5 . . ?
N16 C41 H41B 109.5 . . ?
C46 C41 H41B 109.5 . . ?
H41A C41 H41B 108.1 . . ?
C36 C42 C33 120.4(2) . . ?
C36 C42 H42 119.8 . . ?
C33 C42 H42 119.8 . . ?
N17 C43 C58 110.0(2) . . ?
N17 C43 H43A 109.7 . . ?
C58 C43 H43A 109.7 . . ?
N17 C43 H43B 109.7 . . ?
C58 C43 H43B 109.7 . . ?
H43A C43 H43B 108.2 . . ?
C36 C44 C31 120.0(2) . . ?
C36 C44 H44 120.0 . . ?
C31 C44 H44 120.0 . . ?
C32 C45 C40 120.0(2) . . ?
C32 C45 H45 120.0 . . ?
C40 C45 H45 120.0 . . ?
C37 C46 C27 119.0(2) . . ?
C37 C46 C41 120.4(2) . . ?
C27 C46 C41 120.6(2) . . ?
N23 C47 C21 112.6(2) . . ?
N23 C47 H47A 109.1 . . ?
C21 C47 H47A 109.1 . . ?
N23 C47 H47B 109.1 . . ?
C21 C47 H47B 109.1 . . ?
H47A C47 H47B 107.8 . . ?
O7 C48 O6 124.6(2) . . ?
O7 C48 O10 115.9(2) . . ?
O6 C48 O10 119.5(2) . . ?
N13 C49 C38 114.52(19) . . ?
N13 C49 H49A 108.6 . . ?
C38 C49 H49A 108.6 . . ?
N13 C49 H49B 108.6 . . ?
C38 C49 H49B 108.6 . . ?
H49A C49 H49B 107.6 . . ?
C40 C51 C38 120.2(2) . . ?
C40 C51 H51 119.9 . . ?
C38 C51 H51 119.9 . . ?
N17 C52 C34 112.9(2) . . ?
N17 C52 H52A 109.0 . . ?
C34 C52 H52A 109.0 . . ?
N17 C52 H52B 109.0 . . ?
C34 C52 H52B 109.0 . . ?
H52A C52 H52B 107.8 . . ?
N14 C53 C32 115.9(2) . . ?
N14 C53 H53A 108.3 . . ?
C32 C53 H53A 108.3 . . ?
N14 C53 H53B 108.3 . . ?
C32 C53 H53B 108.3 . . ?
H53A C53 H53B 107.4 . . ?
N17 C54 C24 110.7(2) . . ?
N17 C54 H54A 109.5 . . ?
C24 C54 H54A 109.5 . . ?
N17 C54 H54B 109.5 . . ?
C24 C54 H54B 109.5 . . ?
H54A C54 H54B 108.1 . . ?
N12 C55 C59 110.0(2) . . ?
N12 C55 H55A 109.7 . . ?
C59 C55 H55A 109.7 . . ?
N12 C55 H55B 109.7 . . ?
C59 C55 H55B 109.7 . . ?
H55A C55 H55B 108.2 . . ?
N15 C56 C33 111.6(2) . . ?
N15 C56 H56A 109.3 . . ?
C33 C56 H56A 109.3 . . ?
N15 C56 H56B 109.3 . . ?
C33 C56 H56B 109.3 . . ?
H56A C56 H56B 108.0 . . ?
N13 C57 C20 110.5(2) . . ?
N13 C57 H57A 109.5 . . ?
C20 C57 H57A 109.5 . . ?
N13 C57 H57B 109.5 . . ?
C20 C57 H57B 109.5 . . ?
H57A C57 H57B 108.1 . . ?
N23 C58 C43 110.5(2) . . ?
N23 C58 H58A 109.5 . . ?
C43 C58 H58A 109.5 . . ?
N23 C58 H58B 109.5 . . ?
C43 C58 H58B 109.5 . . ?
H58A C58 H58B 108.1 . . ?
N16 C59 C55 109.52(19) . . ?
N16 C59 H59A 109.8 . . ?
C55 C59 H59A 109.8 . . ?
N16 C59 H59B 109.8 . . ?
C55 C59 H59B 109.8 . . ?
H59A C59 H59B 108.2 . . ?
C66 C61 H61A 109.5 . . ?
C66 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C66 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
N63 C64 C67 178.0(5) . . ?
N65 C66 C61 177.5(5) . . ?
C64 C67 H67A 109.5 . . ?
C64 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C64 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
O2 Cl1 O1 111.1(3) . . ?
O2 Cl1 O3 108.2(3) . . ?
O1 Cl1 O3 112.4(3) . . ?
O2 Cl1 O0AA 112.2(4) . . ?
O1 Cl1 O0AA 107.0(2) . . ?
O3 Cl1 O0AA 105.9(2) . . ?

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
C29 N12 C20 C57 -95.8(2) . . . . ?
C55 N12 C20 C57 139.6(2) . . . . ?
Ni1 N12 C20 C57 23.0(2) . . . . ?
C39 C18 C21 C27 -1.3(4) . . . . ?
C39 C18 C21 C47 176.4(2) . . . . ?
C56 N15 C24 C54 177.2(2) . . . . ?
Ni2 N15 C24 C54 35.1(3) . . . . ?
C18 C21 C27 C46 2.0(3) . . . . ?
C47 C21 C27 C46 -175.7(2) . . . . ?
C30 N19 C28 C31 -147.7(2) . . . . ?
Ni1 N19 C28 C31 77.3(3) . . . . ?
C55 N12 C29 C30 -161.8(2) . . . . ?
C20 N12 C29 C30 74.2(2) . . . . ?
Ni1 N12 C29 C30 -45.4(2) . . . . ?
C28 N19 C30 C29 -175.8(2) . . . . ?
Ni1 N19 C30 C29 -33.0(2) . . . . ?
N12 C29 C30 N19 53.2(3) . . . . ?
N19 C28 C31 C35 -118.3(2) . . . . ?
N19 C28 C31 C44 62.5(3) . . . . ?
C38 C26 C32 C45 0.1(4) . . . . ?
C38 C26 C32 C53 -175.7(2) . . . . ?
C53 N14 C34 C52 -175.3(2) . . . . ?
Ni2 N14 C34 C52 -43.1(2) . . . . ?
C44 C31 C35 C33 0.5(3) . . . . ?
C28 C31 C35 C33 -178.7(2) . . . . ?
C42 C33 C35 C31 -0.1(3) . . . . ?
C56 C33 C35 C31 178.3(2) . . . . ?
C32 C26 C38 C51 -0.2(3) . . . . ?
C32 C26 C38 C49 175.3(2) . . . . ?
C46 C37 C39 C18 0.9(4) . . . . ?
C21 C18 C39 C37 -0.1(4) . . . . ?
C59 N16 C41 C46 141.9(2) . . . . ?
Ni1 N16 C41 C46 -87.4(2) . . . . ?
C44 C36 C42 C33 0.8(3) . . . . ?
C35 C33 C42 C36 -0.5(3) . . . . ?
C56 C33 C42 C36 -178.9(2) . . . . ?
C52 N17 C43 C58 73.5(3) . . . . ?
C54 N17 C43 C58 -161.2(2) . . . . ?
Ni2 N17 C43 C58 -44.4(2) . . . . ?
C42 C36 C44 C31 -0.4(3) . . . . ?
C35 C31 C44 C36 -0.2(3) . . . . ?
C28 C31 C44 C36 179.0(2) . . . . ?
C26 C32 C45 C40 0.3(4) . . . . ?
C53 C32 C45 C40 175.9(2) . . . . ?
C51 C40 C45 C32 -0.5(4) . . . . ?
C39 C37 C46 C27 -0.2(4) . . . . ?
C39 C37 C46 C41 179.1(2) . . . . ?
C21 C27 C46 C37 -1.3(4) . . . . ?
C21 C27 C46 C41 179.4(2) . . . . ?
N16 C41 C46 C37 -68.8(3) . . . . ?
N16 C41 C46 C27 110.5(3) . . . . ?
C58 N23 C47 C21 -138.4(2) . . . . ?
Ni2 N23 C47 C21 93.6(2) . . . . ?
C27 C21 C47 N23 -116.8(3) . . . . ?
C18 C21 C47 N23 65.5(3) . . . . ?
Ni1 O7 C48 O6 179.95(17) . . . . ?
Ni1 O7 C48 O10 -0.4(4) . . . . ?
Ni2 O6 C48 O7 176.42(18) . . . . ?
Ni2 O6 C48 O10 -3.2(4) . . . . ?
C57 N13 C49 C38 159.3(2) . . . . ?
Ni1 N13 C49 C38 -77.9(2) . . . . ?
C26 C38 C49 N13 121.7(2) . . . . ?
C51 C38 C49 N13 -63.0(3) . . . . ?
C45 C40 C51 C38 0.4(4) . . . . ?
C26 C38 C51 C40 0.0(4) . . . . ?
C49 C38 C51 C40 -175.5(2) . . . . ?
C43 N17 C52 C34 -140.5(2) . . . . ?
C54 N17 C52 C34 94.3(3) . . . . ?
Ni2 N17 C52 C34 -24.0(2) . . . . ?
N14 C34 C52 N17 46.7(3) . . . . ?
C34 N14 C53 C32 -162.3(2) . . . . ?
Ni2 N14 C53 C32 75.8(3) . . . . ?
C45 C32 C53 N14 69.1(3) . . . . ?
C26 C32 C53 N14 -115.3(3) . . . . ?
C43 N17 C54 C24 157.8(2) . . . . ?
C52 N17 C54 C24 -77.4(3) . . . . ?
Ni2 N17 C54 C24 41.7(3) . . . . ?
N15 C24 C54 N17 -52.4(3) . . . . ?
C29 N12 C55 C59 163.4(2) . . . . ?
C20 N12 C55 C59 -71.6(2) . . . . ?
Ni1 N12 C55 C59 46.4(2) . . . . ?
C24 N15 C56 C33 146.2(2) . . . . ?
Ni2 N15 C56 C33 -79.2(3) . . . . ?
C42 C33 C56 N15 -59.1(3) . . . . ?
C35 C33 C56 N15 122.5(2) . . . . ?
C49 N13 C57 C20 175.5(2) . . . . ?
Ni1 N13 C57 C20 43.2(2) . . . . ?
N12 C20 C57 N13 -45.9(3) . . . . ?
C47 N23 C58 C43 -164.3(2) . . . . ?
Ni2 N23 C58 C43 -30.2(3) . . . . ?
N17 C43 C58 N23 51.3(3) . . . . ?
C41 N16 C59 C55 171.2(2) . . . . ?
Ni1 N16 C59 C55 32.3(2) . . . . ?
N12 C55 C59 N16 -53.8(3) . . . . ?

_refine_diff_density_max         0.670
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.068

####################################################################### 
# 
# 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_added_by_encifer
_database_code_depnum_ccdc_archive 'CCDC 1418425'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2015-12-08 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            'C42 H63 Cl3 N14 Ni2 O12'
_chemical_formula_weight         1179.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   11.1608(3)
_cell_length_b                   15.0248(3)
_cell_length_c                   16.3126(3)
_cell_angle_alpha                112.1643(18)
_cell_angle_beta                 91.4575(18)
_cell_angle_gamma                94.8008(17)
_cell_volume                     2519.60(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    10101
_cell_measurement_theta_min      3.192
_cell_measurement_theta_max      67.684

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_F_000             1232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    3.026
_shelx_estimated_absorpt_T_min   0.694
_shelx_estimated_absorpt_T_max   0.752
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            47338
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.192
_diffrn_reflns_theta_max         74.271
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10101
_reflns_number_gt                8943
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_solution    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (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)+(0.0653P)²+2.3875P] 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         10101
_refine_ls_number_parameters     714
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1252
_refine_ls_wR_factor_gt          0.1199
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.34107(4) 0.71920(3) 0.30362(2) 0.01950(10) Uani 1 1 d . . . . .
Ni2 Ni 0.25463(4) 0.27793(3) 0.16353(2) 0.02286(11) Uani 1 1 d . . . . .
N6 N 0.14533(19) 0.26552(14) 0.04432(12) 0.0243(4) Uani 1 1 d . . . . .
H6 H 0.2025 0.2933 0.0119 0.029 Uiso 1 1 calc R U . . .
N9 N 0.2414(2) 0.12767(14) 0.10170(13) 0.0266(4) Uani 1 1 d . . . . .
N11 N 0.23849(18) 0.73640(13) 0.20075(12) 0.0216(4) Uani 1 1 d . . . . .
H11 H 0.1592 0.7579 0.2236 0.026 Uiso 1 1 calc R U . . .
N12 N 0.4027(2) 0.25391(14) 0.23770(13) 0.0266(4) Uani 1 1 d . . . . .
H12 H 0.4748 0.2632 0.2056 0.032 Uiso 1 1 calc R U . . .
N13 N 0.30595(17) 0.49944(13) 0.23633(11) 0.0203(4) Uani 1 1 d . . . . .
N14 N 0.26968(19) 0.42247(14) 0.23056(13) 0.0261(4) Uani 1 1 d . . . . .
N15 N 0.34340(19) 0.57708(14) 0.24253(13) 0.0242(4) Uani 1 1 d . . . . .
N16 N 0.51134(18) 0.73118(13) 0.37063(12) 0.0212(4) Uani 1 1 d . . . . .
H16 H 0.5667 0.7036 0.3221 0.025 Uiso 1 1 calc R U . . .
N18 N 0.4011(2) 0.31007(15) 0.08963(13) 0.0272(4) Uani 1 1 d . . . . .
N20 N 0.22184(18) 0.74943(14) 0.40386(12) 0.0222(4) Uani 1 1 d . . . . .
H20 H 0.2664 0.7489 0.4576 0.027 Uiso 1 1 calc R U . . .
N21 N 0.37591(18) 0.87017(13) 0.34632(12) 0.0226(4) Uani 1 1 d . . . . .
C22 C 0.1200(2) 0.59357(17) 0.40345(15) 0.0242(5) Uani 1 1 d . . . . .
N24 N 0.1153(2) 0.25313(15) 0.23992(13) 0.0282(4) Uani 1 1 d . . . . .
H24 H 0.1538 0.2417 0.2906 0.034 Uiso 1 1 calc R U . . .
C25 C 0.1253(2) 0.48127(17) 0.08266(14) 0.0227(4) Uani 1 1 d . . . . .
H25 H 0.1994 0.4594 0.0595 0.027 Uiso 1 1 calc R U . . .
C27 C 0.1129(2) 0.58026(17) 0.11827(14) 0.0221(4) Uani 1 1 d . . . . .
C28 C 0.0793(2) 0.41875(18) 0.34947(16) 0.0271(5) Uani 1 1 d . . . . .
C29 C 0.5625(2) 0.57806(17) 0.38304(14) 0.0223(4) Uani 1 1 d . . . . .
C30 C 0.5302(2) 0.67947(17) 0.43167(14) 0.0240(5) Uani 1 1 d . . . . .
H30A H 0.4556 0.6769 0.4626 0.029 Uiso 1 1 calc R U . . .
H30B H 0.5954 0.7162 0.4770 0.029 Uiso 1 1 calc R U . . .
C32 C 0.4878(2) 0.49832(17) 0.38146(14) 0.0229(4) Uani 1 1 d . . . . .
H32 H 0.4148 0.5076 0.4109 0.027 Uiso 1 1 calc R U . . .
C33 C 0.6697(2) 0.56403(18) 0.33975(15) 0.0262(5) Uani 1 1 d . . . . .
H33 H 0.7212 0.6181 0.3407 0.031 Uiso 1 1 calc R U . . .
C34 C 0.4371(3) 0.31702(17) 0.33208(15) 0.0287(5) Uani 1 1 d . . . . .
H34A H 0.4788 0.2802 0.3613 0.034 Uiso 1 1 calc R U . . .
H34B H 0.3638 0.3382 0.3638 0.034 Uiso 1 1 calc R U . . .
C35 C 0.5088(2) 0.89103(16) 0.36161(15) 0.0249(5) Uani 1 1 d . . . . .
H35A H 0.5299 0.9611 0.3949 0.030 Uiso 1 1 calc R U . . .
H35B H 0.5463 0.8726 0.3039 0.030 Uiso 1 1 calc R U . . .
C36 C 0.0297(2) 0.41423(17) 0.08076(14) 0.0242(5) Uani 1 1 d . . . . .
C37 C 0.4715(2) 0.36429(18) 0.08018(15) 0.0266(5) Uani 1 1 d . . . . .
C38 C 0.0030(2) 0.61124(17) 0.15049(14) 0.0248(5) Uani 1 1 d . . . . .
H38 H -0.0070 0.6782 0.1732 0.030 Uiso 1 1 calc R U . . .
N39 N 1.0192(3) 0.8680(2) 0.22590(17) 0.0483(7) Uani 1 1 d . . . . .
C40 C 0.6269(2) 0.39180(18) 0.29446(15) 0.0275(5) Uani 1 1 d . . . . .
H40 H 0.6496 0.3285 0.2647 0.033 Uiso 1 1 calc R U . . .
C41 C 0.3087(2) 0.81811(16) 0.18774(15) 0.0249(5) Uani 1 1 d . . . . .
H41A H 0.2641 0.8374 0.1448 0.030 Uiso 1 1 calc R U . . .
H41B H 0.3873 0.7985 0.1641 0.030 Uiso 1 1 calc R U . . .
C42 C 0.5194(2) 0.40449(17) 0.33681(14) 0.0249(5) Uani 1 1 d . . . . .
C43 C 0.3138(2) 0.91229(17) 0.42964(15) 0.0267(5) Uani 1 1 d . . . . .
H43A H 0.2977 0.9792 0.4392 0.032 Uiso 1 1 calc R U . . .
H43B H 0.3658 0.9144 0.4805 0.032 Uiso 1 1 calc R U . . .
C44 C 0.7012(2) 0.47119(19) 0.29536(15) 0.0274(5) Uani 1 1 d . . . . .
H44 H 0.7738 0.4619 0.2655 0.033 Uiso 1 1 calc R U . . .
C45 C -0.0784(2) 0.44704(18) 0.11541(15) 0.0266(5) Uani 1 1 d . . . . .
H45 H -0.1433 0.4020 0.1155 0.032 Uiso 1 1 calc R U . . .
C46 C 0.0270(2) 0.32518(19) 0.27694(17) 0.0312(5) Uani 1 1 d . . . . .
H46A H -0.0389 0.2956 0.3008 0.037 Uiso 1 1 calc R U . . .
H46B H -0.0088 0.3402 0.2281 0.037 Uiso 1 1 calc R U . . .
C47 C 0.0737(2) 0.50574(18) 0.33793(15) 0.0251(5) Uani 1 1 d . . . . .
H47 H 0.0375 0.5051 0.2843 0.030 Uiso 1 1 calc R U . . .
C48 C 0.1062(2) 0.68647(17) 0.39062(15) 0.0250(5) Uani 1 1 d . . . . .
H48A H 0.0711 0.6709 0.3299 0.030 Uiso 1 1 calc R U . . .
H48B H 0.0488 0.7229 0.4328 0.030 Uiso 1 1 calc R U . . .
C50 C 0.1961(2) 0.85110(17) 0.42347(15) 0.0263(5) Uani 1 1 d . . . . .
H50A H 0.1564 0.8765 0.4802 0.032 Uiso 1 1 calc R U . . .
H50B H 0.1412 0.8534 0.3758 0.032 Uiso 1 1 calc R U . . .
C51 C 0.0496(3) 0.16014(19) 0.17990(18) 0.0344(6) Uani 1 1 d . . . . .
H51A H 0.0004 0.1712 0.1339 0.041 Uiso 1 1 calc R U . . .
H51B H -0.0056 0.1348 0.2144 0.041 Uiso 1 1 calc R U . . .
C52 C 0.5591(3) 0.4364(2) 0.07002(19) 0.0343(6) Uani 1 1 d . . . . .
H52A H 0.5600 0.4273 0.0073 0.051 Uiso 1 1 calc R U . . .
H52B H 0.6392 0.4293 0.0912 0.051 Uiso 1 1 calc R U . . .
H52C H 0.5369 0.5012 0.1047 0.051 Uiso 1 1 calc R U . . .
C53 C -0.0917(2) 0.54517(19) 0.14974(15) 0.0268(5) Uani 1 1 d . . . . .
H53 H -0.1659 0.5670 0.1727 0.032 Uiso 1 1 calc R U . . .
C54 C 0.3541(3) 0.09375(17) 0.12354(17) 0.0312(5) Uani 1 1 d . . . . .
H54A H 0.4182 0.1039 0.0862 0.037 Uiso 1 1 calc R U . . .
H54B H 0.3410 0.0238 0.1113 0.037 Uiso 1 1 calc R U . . .
N55 N 0.3422(3) 0.8428(2) 0.60413(17) 0.0451(6) Uani 1 1 d . . . . .
C56 C 0.5572(2) 0.83514(16) 0.41374(16) 0.0258(5) Uani 1 1 d . . . . .
H56A H 0.6464 0.8421 0.4162 0.031 Uiso 1 1 calc R U . . .
H56B H 0.5315 0.8617 0.4752 0.031 Uiso 1 1 calc R U . . .
C57 C 0.3927(3) 0.14946(17) 0.22111(17) 0.0306(5) Uani 1 1 d . . . . .
H57A H 0.3324 0.1347 0.2589 0.037 Uiso 1 1 calc R U . . .
H57B H 0.4713 0.1309 0.2353 0.037 Uiso 1 1 calc R U . . .
C58 C 0.1725(2) 0.59349(18) 0.48181(15) 0.0294(5) Uani 1 1 d . . . . .
H58 H 0.2045 0.6527 0.5272 0.035 Uiso 1 1 calc R U . . .
C59 C 0.1781(3) 0.5074(2) 0.49379(16) 0.0338(6) Uani 1 1 d . . . . .
H59 H 0.2147 0.5080 0.5473 0.041 Uiso 1 1 calc R U . . .
C60 C 0.1281(3) 0.16018(17) -0.01375(16) 0.0304(5) Uani 1 1 d . . . . .
H60A H 0.1275 0.1527 -0.0767 0.036 Uiso 1 1 calc R U . . .
H60B H 0.0492 0.1318 -0.0038 0.036 Uiso 1 1 calc R U . . .
C61 C 0.2262(3) 0.10643(17) 0.00487(16) 0.0308(5) Uani 1 1 d . . . . .
H61A H 0.2058 0.0362 -0.0279 0.037 Uiso 1 1 calc R U . . .
H61B H 0.3029 0.1256 -0.0161 0.037 Uiso 1 1 calc R U . . .
C62 C 0.1307(3) 0.41972(19) 0.42821(16) 0.0314(5) Uani 1 1 d . . . . .
H62 H 0.1336 0.3612 0.4375 0.038 Uiso 1 1 calc R U . . .
C63 C 0.2151(2) 0.65134(16) 0.11535(14) 0.0233(5) Uani 1 1 d . . . . .
H63A H 0.2891 0.6180 0.1008 0.028 Uiso 1 1 calc R U . . .
H63B H 0.1957 0.6742 0.0675 0.028 Uiso 1 1 calc R U . . .
C64 C 0.3076(3) 0.8868(2) 0.6702(2) 0.0392(6) Uani 1 1 d . . . . .
C65 C 0.3281(2) 0.90227(16) 0.27701(15) 0.0265(5) Uani 1 1 d . . . . .
H65A H 0.3856 0.9535 0.2719 0.032 Uiso 1 1 calc R U . . .
H65B H 0.2508 0.9297 0.2946 0.032 Uiso 1 1 calc R U . . .
C66 C 0.0318(2) 0.30606(17) 0.03580(16) 0.0285(5) Uani 1 1 d . . . . .
H66A H -0.0324 0.2748 0.0596 0.034 Uiso 1 1 calc R U . . .
H66B H 0.0105 0.2875 -0.0282 0.034 Uiso 1 1 calc R U . . .
C67 C 0.1363(3) 0.08626(18) 0.13563(17) 0.0339(6) Uani 1 1 d . . . . .
H67A H 0.1663 0.0602 0.1788 0.041 Uiso 1 1 calc R U . . .
H67B H 0.0926 0.0320 0.0856 0.041 Uiso 1 1 calc R U . . .
C69 C 0.9565(3) 0.8947(2) 0.2790(2) 0.0429(7) Uani 1 1 d . . . . .
C72 C 0.2629(5) 0.9439(3) 0.7562(3) 0.0758(14) Uani 1 1 d . . . . .
H72A H 0.1828 0.9619 0.7470 0.114 Uiso 1 1 calc R U . . .
H72B H 0.3182 1.0024 0.7858 0.114 Uiso 1 1 calc R U . . .
H72C H 0.2580 0.9054 0.7932 0.114 Uiso 1 1 calc R U . . .
C73 C 0.8722(4) 0.9245(3) 0.3512(2) 0.0589(9) Uani 1 1 d . . . . .
H73A H 0.7895 0.9006 0.3264 0.088 Uiso 1 1 calc R U . . .
H73B H 0.8793 0.9951 0.3795 0.088 Uiso 1 1 calc R U . . .
H73C H 0.8922 0.8974 0.3953 0.088 Uiso 1 1 calc R U . . .
Cl1 Cl 0.34562(5) 0.27913(4) 0.84078(3) 0.02585(13) Uani 1 1 d . . . . .
Cl2 Cl 0.12237(10) 0.14945(8) 0.43204(7) 0.0272(2) Uani 0.85 1 d . . P A 1
Cl3 Cl 0.2778(4) 0.8163(4) 0.9323(4) 0.0246(6) Uani 0.5 1 d . . P B 1
O5 O 0.27961(19) 0.27264(16) 0.76146(12) 0.0404(5) Uani 1 1 d . . . . .
O7 O 0.46870(18) 0.31591(14) 0.83679(14) 0.0383(4) Uani 1 1 d . . . . .
O8 O 0.29386(19) 0.34421(15) 0.91748(12) 0.0363(4) Uani 1 1 d . . . . .
O9 O 0.2026(2) 0.87501(14) 0.98859(16) 0.0458(5) Uani 1 1 d . . . . .
O10 O 0.0057(2) 0.16634(17) 0.40003(15) 0.0473(5) Uani 1 1 d . . . . .
O1 O 0.3445(2) 0.18543(15) 0.84457(15) 0.0446(5) Uani 1 1 d . . . . .
O2 O 0.1161(3) 0.0569(2) 0.4377(2) 0.0510(7) Uani 0.85 1 d . . P A 1
O3 O 0.1519(2) 0.22155(19) 0.51916(17) 0.0463(6) Uani 0.85 1 d . . P A 1
O6 O 0.2120(3) 0.1624(3) 0.3771(2) 0.0866(11) Uani 1 1 d . . . . .
O4 O 0.3073(3) 0.7388(2) 0.9548(3) 0.0787(10) Uani 1 1 d . . . . .
O11 O 0.2127(3) 0.7675(3) 0.8485(2) 0.0351(8) Uani 0.5 1 d . . P B 1
O12 O 0.3807(4) 0.8782(4) 0.9248(4) 0.0492(11) Uani 0.5 1 d . . P B 1
Cl4 Cl 0.3075(4) 0.8250(4) 0.9454(4) 0.0333(9) Uani 0.5 1 d . . P B 2
O13 O 0.4108(5) 0.8651(4) 1.0104(3) 0.0597(13) Uani 0.5 1 d . . P B 2
O14 O 0.3458(7) 0.8345(6) 0.8674(4) 0.080(2) Uani 0.5 1 d . . P B 2
Cl5 Cl 0.0920(7) 0.1285(5) 0.3989(5) 0.0373(15) Uani 0.15 1 d . . P A 2
O16 O 0.100(2) 0.0541(13) 0.3152(13) 0.084(7) Uani 0.15 1 d . . P A 2
O15A O 0.124(4) 0.121(3) 0.483(3) 0.063(10) Uiso 0.075 1 d . . P A 2
O15B O 0.082(2) 0.089(2) 0.4644(18) 0.021(5) Uiso 0.075 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 N15 1.9895(19) . ?
Ni1 N20 2.074(2) . ?
Ni1 N21 2.1043(19) . ?
Ni1 N11 2.1149(19) . ?
Ni1 N16 2.1278(19) . ?
Ni2 N14 2.019(2) . ?
Ni2 N9 2.087(2) . ?
Ni2 N24 2.112(2) . ?
Ni2 N12 2.157(2) . ?
Ni2 N18 2.183(2) . ?
Ni2 N6 2.207(2) . ?
N6 C66 1.477(3) . ?
N6 C60 1.499(3) . ?
N6 H6 1.0000 . ?
N9 C54 1.479(4) . ?
N9 C61 1.491(3) . ?
N9 C67 1.497(3) . ?
N11 C41 1.487(3) . ?
N11 C63 1.492(3) . ?
N11 H11 1.0000 . ?
N12 C57 1.482(3) . ?
N12 C34 1.491(3) . ?
N12 H12 1.0000 . ?
N13 N14 1.161(3) . ?
N13 N15 1.172(3) . ?
N16 C56 1.488(3) . ?
N16 C30 1.497(3) . ?
N16 H16 1.0000 . ?
N18 C37 1.139(3) . ?
N20 C50 1.493(3) . ?
N20 C48 1.495(3) . ?
N20 H20 1.0000 . ?
N21 C43 1.483(3) . ?
N21 C35 1.485(3) . ?
N21 C65 1.490(3) . ?
C22 C58 1.393(3) . ?
C22 C47 1.394(3) . ?
C22 C48 1.507(3) . ?
N24 C51 1.486(3) . ?
N24 C46 1.491(3) . ?
N24 H24 1.0000 . ?
C25 C36 1.396(3) . ?
C25 C27 1.398(3) . ?
C25 H25 0.9500 . ?
C27 C38 1.393(3) . ?
C27 C63 1.510(3) . ?
C28 C62 1.388(4) . ?
C28 C47 1.395(4) . ?
C28 C46 1.513(3) . ?
C29 C32 1.393(3) . ?
C29 C33 1.396(4) . ?
C29 C30 1.509(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C32 C42 1.401(3) . ?
C32 H32 0.9500 . ?
C33 C44 1.388(4) . ?
C33 H33 0.9500 . ?
C34 C42 1.515(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C56 1.520(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C45 1.393(4) . ?
C36 C66 1.512(3) . ?
C37 C52 1.457(4) . ?
C38 C53 1.385(4) . ?
C38 H38 0.9500 . ?
N39 C69 1.103(4) . ?
C40 C44 1.390(4) . ?
C40 C42 1.390(4) . ?
C40 H40 0.9500 . ?
C41 C65 1.522(3) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C43 C50 1.518(4) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44 0.9500 . ?
C45 C53 1.388(4) . ?
C45 H45 0.9500 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 H47 0.9500 . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C67 1.517(4) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53 0.9500 . ?
C54 C57 1.523(3) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
N55 C64 1.128(4) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 C59 1.385(4) . ?
C58 H58 0.9500 . ?
C59 C62 1.397(4) . ?
C59 H59 0.9500 . ?
C60 C61 1.503(4) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 H62 0.9500 . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 C72 1.467(5) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C69 C73 1.483(5) . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
Cl1 O1 1.431(2) . ?
Cl1 O8 1.4365(19) . ?
Cl1 O5 1.4391(19) . ?
Cl1 O7 1.450(2) . ?
Cl2 O6 1.410(3) . ?
Cl2 O2 1.425(3) . ?
Cl2 O3 1.434(3) . ?
Cl2 O10 1.467(2) . ?
Cl3 O9 1.370(7) . ?
Cl3 O4 1.408(7) . ?
Cl3 O11 1.427(5) . ?
Cl3 O12 1.453(7) . ?
O9 Cl4 1.490(6) . ?
O10 Cl5 1.155(8) . ?
O6 Cl5 1.492(8) . ?
O4 Cl4 1.361(7) . ?
Cl4 O14 1.407(9) . ?
Cl4 O13 1.469(6) . ?
Cl5 O15B 1.41(3) . ?
Cl5 O16 1.411(16) . ?
Cl5 O15A 1.45(4) . ?
O15A O15B 0.63(4) . ?

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
N15 Ni1 N20 110.12(8) . . ?
N15 Ni1 N21 164.78(8) . . ?
N20 Ni1 N21 85.02(8) . . ?
N15 Ni1 N11 95.42(8) . . ?
N20 Ni1 N11 102.00(8) . . ?
N21 Ni1 N11 82.43(7) . . ?
N15 Ni1 N16 91.21(8) . . ?
N20 Ni1 N16 103.79(7) . . ?
N21 Ni1 N16 83.39(8) . . ?
N11 Ni1 N16 149.24(8) . . ?
N14 Ni2 N9 176.45(8) . . ?
N14 Ni2 N24 93.35(8) . . ?
N9 Ni2 N24 84.80(8) . . ?
N14 Ni2 N12 94.90(8) . . ?
N9 Ni2 N12 82.36(8) . . ?
N24 Ni2 N12 97.42(8) . . ?
N14 Ni2 N18 84.15(8) . . ?
N9 Ni2 N18 97.64(8) . . ?
N24 Ni2 N18 177.32(8) . . ?
N12 Ni2 N18 81.85(8) . . ?
N14 Ni2 N6 100.33(8) . . ?
N9 Ni2 N6 82.97(8) . . ?
N24 Ni2 N6 99.16(8) . . ?
N12 Ni2 N6 156.70(8) . . ?
N18 Ni2 N6 82.28(8) . . ?
C66 N6 C60 106.90(19) . . ?
C66 N6 Ni2 130.46(15) . . ?
C60 N6 Ni2 106.51(15) . . ?
C66 N6 H6 103.3 . . ?
C60 N6 H6 103.3 . . ?
Ni2 N6 H6 103.3 . . ?
C54 N9 C61 111.2(2) . . ?
C54 N9 C67 110.1(2) . . ?
C61 N9 C67 112.8(2) . . ?
C54 N9 Ni2 108.52(15) . . ?
C61 N9 Ni2 105.38(14) . . ?
C67 N9 Ni2 108.61(15) . . ?
C41 N11 C63 111.11(17) . . ?
C41 N11 Ni1 102.91(13) . . ?
C63 N11 Ni1 117.67(14) . . ?
C41 N11 H11 108.3 . . ?
C63 N11 H11 108.3 . . ?
Ni1 N11 H11 108.3 . . ?
C57 N12 C34 113.26(18) . . ?
C57 N12 Ni2 107.51(15) . . ?
C34 N12 Ni2 122.66(16) . . ?
C57 N12 H12 103.7 . . ?
C34 N12 H12 103.7 . . ?
Ni2 N12 H12 103.7 . . ?
N14 N13 N15 179.4(3) . . ?
N13 N14 Ni2 149.83(18) . . ?
N13 N15 Ni1 148.05(18) . . ?
C56 N16 C30 110.98(17) . . ?
C56 N16 Ni1 108.92(14) . . ?
C30 N16 Ni1 121.56(15) . . ?
C56 N16 H16 104.6 . . ?
C30 N16 H16 104.6 . . ?
Ni1 N16 H16 104.6 . . ?
C37 N18 Ni2 149.8(2) . . ?
C50 N20 C48 109.74(18) . . ?
C50 N20 Ni1 105.09(14) . . ?
C48 N20 Ni1 119.89(14) . . ?
C50 N20 H20 107.2 . . ?
C48 N20 H20 107.2 . . ?
Ni1 N20 H20 107.2 . . ?
C43 N21 C35 111.80(18) . . ?
C43 N21 C65 110.78(19) . . ?
C35 N21 C65 112.15(19) . . ?
C43 N21 Ni1 106.63(14) . . ?
C35 N21 Ni1 105.69(13) . . ?
C65 N21 Ni1 109.49(14) . . ?
C58 C22 C47 118.7(2) . . ?
C58 C22 C48 121.4(2) . . ?
C47 C22 C48 119.8(2) . . ?
C51 N24 C46 109.1(2) . . ?
C51 N24 Ni2 103.63(15) . . ?
C46 N24 Ni2 121.02(16) . . ?
C51 N24 H24 107.5 . . ?
C46 N24 H24 107.5 . . ?
Ni2 N24 H24 107.5 . . ?
C36 C25 C27 120.6(2) . . ?
C36 C25 H25 119.7 . . ?
C27 C25 H25 119.7 . . ?
C38 C27 C25 119.2(2) . . ?
C38 C27 C63 120.9(2) . . ?
C25 C27 C63 119.8(2) . . ?
C62 C28 C47 119.4(2) . . ?
C62 C28 C46 121.0(2) . . ?
C47 C28 C46 119.6(2) . . ?
C32 C29 C33 119.5(2) . . ?
C32 C29 C30 121.1(2) . . ?
C33 C29 C30 119.4(2) . . ?
N16 C30 C29 112.25(18) . . ?
N16 C30 H30A 109.2 . . ?
C29 C30 H30A 109.2 . . ?
N16 C30 H30B 109.2 . . ?
C29 C30 H30B 109.2 . . ?
H30A C30 H30B 107.9 . . ?
C29 C32 C42 120.6(2) . . ?
C29 C32 H32 119.7 . . ?
C42 C32 H32 119.7 . . ?
C44 C33 C29 120.1(2) . . ?
C44 C33 H33 120.0 . . ?
C29 C33 H33 120.0 . . ?
N12 C34 C42 110.05(19) . . ?
N12 C34 H34A 109.6 . . ?
C42 C34 H34A 109.6 . . ?
N12 C34 H34B 109.6 . . ?
C42 C34 H34B 109.6 . . ?
H34A C34 H34B 108.2 . . ?
N21 C35 C56 110.32(19) . . ?
N21 C35 H35A 109.6 . . ?
C56 C35 H35A 109.6 . . ?
N21 C35 H35B 109.6 . . ?
C56 C35 H35B 109.6 . . ?
H35A C35 H35B 108.1 . . ?
C45 C36 C25 119.2(2) . . ?
C45 C36 C66 116.8(2) . . ?
C25 C36 C66 123.8(2) . . ?
N18 C37 C52 178.0(3) . . ?
C53 C38 C27 120.5(2) . . ?
C53 C38 H38 119.7 . . ?
C27 C38 H38 119.7 . . ?
C44 C40 C42 120.4(2) . . ?
C44 C40 H40 119.8 . . ?
C42 C40 H40 119.8 . . ?
N11 C41 C65 108.21(18) . . ?
N11 C41 H41A 110.1 . . ?
C65 C41 H41A 110.1 . . ?
N11 C41 H41B 110.1 . . ?
C65 C41 H41B 110.1 . . ?
H41A C41 H41B 108.4 . . ?
C40 C42 C32 119.2(2) . . ?
C40 C42 C34 119.7(2) . . ?
C32 C42 C34 121.1(2) . . ?
N21 C43 C50 109.39(18) . . ?
N21 C43 H43A 109.8 . . ?
C50 C43 H43A 109.8 . . ?
N21 C43 H43B 109.8 . . ?
C50 C43 H43B 109.8 . . ?
H43A C43 H43B 108.2 . . ?
C33 C44 C40 120.3(2) . . ?
C33 C44 H44 119.8 . . ?
C40 C44 H44 119.8 . . ?
C53 C45 C36 120.4(2) . . ?
C53 C45 H45 119.8 . . ?
C36 C45 H45 119.8 . . ?
N24 C46 C28 114.6(2) . . ?
N24 C46 H46A 108.6 . . ?
C28 C46 H46A 108.6 . . ?
N24 C46 H46B 108.6 . . ?
C28 C46 H46B 108.6 . . ?
H46A C46 H46B 107.6 . . ?
C22 C47 C28 121.4(2) . . ?
C22 C47 H47 119.3 . . ?
C28 C47 H47 119.3 . . ?
N20 C48 C22 113.7(2) . . ?
N20 C48 H48A 108.8 . . ?
C22 C48 H48A 108.8 . . ?
N20 C48 H48B 108.8 . . ?
C22 C48 H48B 108.8 . . ?
H48A C48 H48B 107.7 . . ?
N20 C50 C43 108.9(2) . . ?
N20 C50 H50A 109.9 . . ?
C43 C50 H50A 109.9 . . ?
N20 C50 H50B 109.9 . . ?
C43 C50 H50B 109.9 . . ?
H50A C50 H50B 108.3 . . ?
N24 C51 C67 111.2(2) . . ?
N24 C51 H51A 109.4 . . ?
C67 C51 H51A 109.4 . . ?
N24 C51 H51B 109.4 . . ?
C67 C51 H51B 109.4 . . ?
H51A C51 H51B 108.0 . . ?
C37 C52 H52A 109.5 . . ?
C37 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C37 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C38 C53 C45 120.1(2) . . ?
C38 C53 H53 120.0 . . ?
C45 C53 H53 120.0 . . ?
N9 C54 C57 109.5(2) . . ?
N9 C54 H54A 109.8 . . ?
C57 C54 H54A 109.8 . . ?
N9 C54 H54B 109.8 . . ?
C57 C54 H54B 109.8 . . ?
H54A C54 H54B 108.2 . . ?
N16 C56 C35 109.90(18) . . ?
N16 C56 H56A 109.7 . . ?
C35 C56 H56A 109.7 . . ?
N16 C56 H56B 109.7 . . ?
C35 C56 H56B 109.7 . . ?
H56A C56 H56B 108.2 . . ?
N12 C57 C54 107.88(19) . . ?
N12 C57 H57A 110.1 . . ?
C54 C57 H57A 110.1 . . ?
N12 C57 H57B 110.1 . . ?
C54 C57 H57B 110.1 . . ?
H57A C57 H57B 108.4 . . ?
C59 C58 C22 120.2(2) . . ?
C59 C58 H58 119.9 . . ?
C22 C58 H58 119.9 . . ?
C58 C59 C62 120.8(2) . . ?
C58 C59 H59 119.6 . . ?
C62 C59 H59 119.6 . . ?
N6 C60 C61 111.7(2) . . ?
N6 C60 H60A 109.3 . . ?
C61 C60 H60A 109.3 . . ?
N6 C60 H60B 109.3 . . ?
C61 C60 H60B 109.3 . . ?
H60A C60 H60B 107.9 . . ?
N9 C61 C60 110.6(2) . . ?
N9 C61 H61A 109.5 . . ?
C60 C61 H61A 109.5 . . ?
N9 C61 H61B 109.5 . . ?
C60 C61 H61B 109.5 . . ?
H61A C61 H61B 108.1 . . ?
C28 C62 C59 119.5(2) . . ?
C28 C62 H62 120.2 . . ?
C59 C62 H62 120.2 . . ?
N11 C63 C27 112.80(18) . . ?
N11 C63 H63A 109.0 . . ?
C27 C63 H63A 109.0 . . ?
N11 C63 H63B 109.0 . . ?
C27 C63 H63B 109.0 . . ?
H63A C63 H63B 107.8 . . ?
N55 C64 C72 179.8(4) . . ?
N21 C65 C41 110.77(18) . . ?
N21 C65 H65A 109.5 . . ?
C41 C65 H65A 109.5 . . ?
N21 C65 H65B 109.5 . . ?
C41 C65 H65B 109.5 . . ?
H65A C65 H65B 108.1 . . ?
N6 C66 C36 117.51(19) . . ?
N6 C66 H66A 107.9 . . ?
C36 C66 H66A 107.9 . . ?
N6 C66 H66B 107.9 . . ?
C36 C66 H66B 107.9 . . ?
H66A C66 H66B 107.2 . . ?
N9 C67 C51 112.7(2) . . ?
N9 C67 H67A 109.1 . . ?
C51 C67 H67A 109.1 . . ?
N9 C67 H67B 109.1 . . ?
C51 C67 H67B 109.1 . . ?
H67A C67 H67B 107.8 . . ?
N39 C69 C73 176.2(4) . . ?
C64 C72 H72A 109.5 . . ?
C64 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C64 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C69 C73 H73A 109.5 . . ?
C69 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C69 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
O1 Cl1 O8 110.38(12) . . ?
O1 Cl1 O5 110.00(14) . . ?
O8 Cl1 O5 109.95(12) . . ?
O1 Cl1 O7 109.33(13) . . ?
O8 Cl1 O7 109.70(12) . . ?
O5 Cl1 O7 107.43(13) . . ?
O6 Cl2 O2 113.1(2) . . ?
O6 Cl2 O3 107.2(2) . . ?
O2 Cl2 O3 108.36(19) . . ?
O6 Cl2 O10 109.11(18) . . ?
O2 Cl2 O10 110.77(18) . . ?
O3 Cl2 O10 108.16(15) . . ?
O9 Cl3 O4 114.2(5) . . ?
O9 Cl3 O11 107.7(3) . . ?
O4 Cl3 O11 102.0(4) . . ?
O9 Cl3 O12 107.1(5) . . ?
O4 Cl3 O12 114.7(4) . . ?
O11 Cl3 O12 110.9(5) . . ?
O4 Cl4 O14 120.3(6) . . ?
O4 Cl4 O13 90.5(4) . . ?
O14 Cl4 O13 105.4(5) . . ?
O4 Cl4 O9 109.8(4) . . ?
O14 Cl4 O9 119.3(5) . . ?
O13 Cl4 O9 106.3(4) . . ?
O10 Cl5 O15B 106.0(12) . . ?
O10 Cl5 O16 110.6(12) . . ?
O15B Cl5 O16 109.8(17) . . ?
O10 Cl5 O15A 113.4(18) . . ?
O15B Cl5 O15A 25.3(17) . . ?
O16 Cl5 O15A 124(2) . . ?
O10 Cl5 O6 124.1(6) . . ?
O15B Cl5 O6 121.2(12) . . ?
O16 Cl5 O6 81.4(12) . . ?
O15A Cl5 O6 100(2) . . ?
O15B O15A Cl5 74(5) . . ?
O15A O15B Cl5 81(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
C36 C25 C27 C38 -1.2(3) . . . . ?
C36 C25 C27 C63 -176.79(19) . . . . ?
C56 N16 C30 C29 -143.2(2) . . . . ?
Ni1 N16 C30 C29 86.7(2) . . . . ?
C32 C29 C30 N16 -117.1(2) . . . . ?
C33 C29 C30 N16 63.6(3) . . . . ?
C33 C29 C32 C42 -0.1(3) . . . . ?
C30 C29 C32 C42 -179.36(19) . . . . ?
C32 C29 C33 C44 0.2(3) . . . . ?
C30 C29 C33 C44 179.5(2) . . . . ?
C57 N12 C34 C42 143.7(2) . . . . ?
Ni2 N12 C34 C42 -84.6(2) . . . . ?
C43 N21 C35 C56 69.5(2) . . . . ?
C65 N21 C35 C56 -165.34(18) . . . . ?
Ni1 N21 C35 C56 -46.1(2) . . . . ?
C27 C25 C36 C45 -0.4(3) . . . . ?
C27 C25 C36 C66 174.0(2) . . . . ?
C25 C27 C38 C53 1.9(3) . . . . ?
C63 C27 C38 C53 177.5(2) . . . . ?
C63 N11 C41 C65 179.46(19) . . . . ?
Ni1 N11 C41 C65 -53.7(2) . . . . ?
C44 C40 C42 C32 -0.9(3) . . . . ?
C44 C40 C42 C34 177.6(2) . . . . ?
C29 C32 C42 C40 0.4(3) . . . . ?
C29 C32 C42 C34 -178.0(2) . . . . ?
N12 C34 C42 C40 -57.6(3) . . . . ?
N12 C34 C42 C32 120.9(2) . . . . ?
C35 N21 C43 C50 -150.94(19) . . . . ?
C65 N21 C43 C50 83.2(2) . . . . ?
Ni1 N21 C43 C50 -35.9(2) . . . . ?
C29 C33 C44 C40 -0.6(3) . . . . ?
C42 C40 C44 C33 1.0(3) . . . . ?
C25 C36 C45 C53 1.3(3) . . . . ?
C66 C36 C45 C53 -173.5(2) . . . . ?
C51 N24 C46 C28 171.5(2) . . . . ?
Ni2 N24 C46 C28 -68.6(3) . . . . ?
C62 C28 C46 N24 -61.3(3) . . . . ?
C47 C28 C46 N24 120.1(3) . . . . ?
C58 C22 C47 C28 -0.2(4) . . . . ?
C48 C22 C47 C28 -176.7(2) . . . . ?
C62 C28 C47 C22 0.8(4) . . . . ?
C46 C28 C47 C22 179.5(2) . . . . ?
C50 N20 C48 C22 -158.97(19) . . . . ?
Ni1 N20 C48 C22 79.3(2) . . . . ?
C58 C22 C48 N20 55.6(3) . . . . ?
C47 C22 C48 N20 -128.0(2) . . . . ?
C48 N20 C50 C43 -175.67(18) . . . . ?
Ni1 N20 C50 C43 -45.5(2) . . . . ?
N21 C43 C50 N20 56.2(2) . . . . ?
C46 N24 C51 C67 176.2(2) . . . . ?
Ni2 N24 C51 C67 46.0(2) . . . . ?
C27 C38 C53 C45 -1.0(3) . . . . ?
C36 C45 C53 C38 -0.6(3) . . . . ?
C61 N9 C54 C57 157.4(2) . . . . ?
C67 N9 C54 C57 -76.8(2) . . . . ?
Ni2 N9 C54 C57 42.0(2) . . . . ?
C30 N16 C56 C35 -165.23(19) . . . . ?
Ni1 N16 C56 C35 -28.8(2) . . . . ?
N21 C35 C56 N16 51.3(3) . . . . ?
C34 N12 C57 C54 178.5(2) . . . . ?
Ni2 N12 C57 C54 39.8(2) . . . . ?
N9 C54 C57 N12 -55.4(3) . . . . ?
C47 C22 C58 C59 0.0(4) . . . . ?
C48 C22 C58 C59 176.5(2) . . . . ?
C22 C58 C59 C62 -0.5(4) . . . . ?
C66 N6 C60 C61 -167.0(2) . . . . ?
Ni2 N6 C60 C61 -24.2(2) . . . . ?
C54 N9 C61 C60 -167.2(2) . . . . ?
C67 N9 C61 C60 68.5(3) . . . . ?
Ni2 N9 C61 C60 -49.8(2) . . . . ?
N6 C60 C61 N9 50.8(3) . . . . ?
C47 C28 C62 C59 -1.3(4) . . . . ?
C46 C28 C62 C59 -180.0(3) . . . . ?
C58 C59 C62 C28 1.2(4) . . . . ?
C41 N11 C63 C27 -161.30(19) . . . . ?
Ni1 N11 C63 C27 80.5(2) . . . . ?
C38 C27 C63 N11 48.8(3) . . . . ?
C25 C27 C63 N11 -135.7(2) . . . . ?
C43 N21 C65 C41 -136.4(2) . . . . ?
C35 N21 C65 C41 97.9(2) . . . . ?
Ni1 N21 C65 C41 -19.1(2) . . . . ?
N11 C41 C65 N21 50.0(3) . . . . ?
C60 N6 C66 C36 -173.8(2) . . . . ?
Ni2 N6 C66 C36 55.7(3) . . . . ?
C45 C36 C66 N6 -145.7(2) . . . . ?
C25 C36 C66 N6 39.7(3) . . . . ?
C54 N9 C67 C51 136.5(2) . . . . ?
C61 N9 C67 C51 -98.7(3) . . . . ?
Ni2 N9 C67 C51 17.8(3) . . . . ?
N24 C51 C67 N9 -44.5(3) . . . . ?
O10 Cl5 O15A O15B 78(5) . . . . ?
O16 Cl5 O15A O15B -61(6) . . . . ?
O6 Cl5 O15A O15B -148(5) . . . . ?
O10 Cl5 O15B O15A -111(5) . . . . ?
O16 Cl5 O15B O15A 129(5) . . . . ?
O6 Cl5 O15B O15A 38(6) . . . . ?

_refine_diff_density_max         1.323
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.075

####################################################################### 
# 
# 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_added_by_encifer
_database_code_depnum_ccdc_archive 'CCDC 1418426'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2015-12-08 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            'C4 H14 Ni O8'
_chemical_formula_weight         248.86

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   4.74771(14)
_cell_length_b                   11.7147(3)
_cell_length_c                   8.3144(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.055(3)
_cell_angle_gamma                90
_cell_volume                     461.78(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1788
_cell_measurement_theta_min      3.007
_cell_measurement_theta_max      26.000

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_F_000             260
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    2.116
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8698
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.007
_diffrn_reflns_theta_max         36.613
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.785
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.785
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.785
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1788
_reflns_number_gt                1376
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_solution    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (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)+(0.0282P)²+0.1523P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1788
_refine_ls_number_parameters     64
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0370
_refine_ls_wR_factor_ref         0.0715
_refine_ls_wR_factor_gt          0.0652
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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 0.0000 0.5000 0.5000 0.01174(9) Uani 1 2 d S . P . .
O2 O 0.2332(2) 0.45308(10) 0.70219(14) 0.0164(2) Uani 1 1 d . . . . .
H2A H 0.4096 0.4739 0.6966 0.025 Uiso 1 1 d R U . . .
H2B H 0.2300 0.3789 0.7152 0.025 Uiso 1 1 d R U . . .
O3 O 0.2822(2) 0.42024(9) 0.35235(14) 0.0150(2) Uani 1 1 d . . . . .
H3A H 0.1924 0.3752 0.2859 0.023 Uiso 1 1 d R U . . .
H3B H 0.4033 0.3810 0.4097 0.023 Uiso 1 1 d R U . . .
O4 O 0.2320(2) 0.64895(9) 0.49230(14) 0.0158(2) Uani 1 1 d . . . . .
O5 O -0.0760(3) 0.75824(10) 0.35219(16) 0.0220(3) Uani 1 1 d . . . . .
C6 C 0.1384(3) 0.74618(13) 0.4450(2) 0.0143(3) Uani 1 1 d . . . . .
C7 C 0.2927(4) 0.84984(14) 0.5087(2) 0.0220(4) Uani 1 1 d . . . . .
H7A H 0.2415 0.9158 0.4407 0.033 Uiso 1 1 calc R U . . .
H7B H 0.4964 0.8367 0.5076 0.033 Uiso 1 1 calc R U . . .
H7C H 0.2409 0.8648 0.6192 0.033 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 O2 2.0386(11) . ?
Ni1 O2 2.0386(11) 3_566 ?
Ni1 O4 2.0663(11) 3_566 ?
Ni1 O4 2.0664(11) . ?
Ni1 O3 2.0856(11) 3_566 ?
Ni1 O3 2.0856(11) . ?
O2 H2A 0.8756 . ?
O2 H2B 0.8756 . ?
O3 H3A 0.8601 . ?
O3 H3B 0.8603 . ?
O4 C6 1.2770(18) . ?
O5 C6 1.252(2) . ?
C6 C7 1.500(2) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 O2 180.0 . 3_566 ?
O2 Ni1 O4 90.79(4) . 3_566 ?
O2 Ni1 O4 89.21(5) 3_566 3_566 ?
O2 Ni1 O4 89.21(4) . . ?
O2 Ni1 O4 90.79(4) 3_566 . ?
O4 Ni1 O4 180.0 3_566 . ?
O2 Ni1 O3 88.46(5) . 3_566 ?
O2 Ni1 O3 91.54(5) 3_566 3_566 ?
O4 Ni1 O3 89.99(4) 3_566 3_566 ?
O4 Ni1 O3 90.01(4) . 3_566 ?
O2 Ni1 O3 91.54(5) . . ?
O2 Ni1 O3 88.46(5) 3_566 . ?
O4 Ni1 O3 90.01(4) 3_566 . ?
O4 Ni1 O3 89.99(4) . . ?
O3 Ni1 O3 180.0 3_566 . ?
Ni1 O2 H2A 111.1 . . ?
Ni1 O2 H2B 110.9 . . ?
H2A O2 H2B 107.8 . . ?
Ni1 O3 H3A 109.9 . . ?
Ni1 O3 H3B 110.2 . . ?
H3A O3 H3B 108.8 . . ?
C6 O4 Ni1 125.82(10) . . ?
O5 C6 O4 123.27(14) . . ?
O5 C6 C7 119.45(14) . . ?
O4 C6 C7 117.27(14) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 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
Ni1 O4 C6 O5 -23.1(2) . . . . ?
Ni1 O4 C6 C7 155.48(12) . . . . ?

_refine_diff_density_max         0.516
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.109

####################################################################### 
# 
# 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_added_by_encifer
_database_code_depnum_ccdc_archive 'CCDC 1418427'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2015-12-08 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            'C54 H87 Cl3 N14 Ni2 O12'
_chemical_formula_weight         1348.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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+1/2, -z'

_cell_length_a                   12.7102(6)
_cell_length_b                   12.8900(5)
_cell_length_c                   19.9985(9)
_cell_angle_alpha                90
_cell_angle_beta                 102.464(4)
_cell_angle_gamma                90
_cell_volume                     3199.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9639
_cell_measurement_theta_min      3.541
_cell_measurement_theta_max      74.435

_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_F_000             1424
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.452
_shelx_estimated_absorpt_T_min   0.741
_shelx_estimated_absorpt_T_max   0.792
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13871
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.561
_diffrn_reflns_theta_max         74.435
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9639
_reflns_number_gt                8548
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.912
_reflns_Friedel_fraction_max     0.965
_reflns_Friedel_fraction_full    0.999

_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_solution    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0436P)²+3.2768P] 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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.58(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9639
_refine_ls_number_parameters     779
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.1157
_refine_ls_wR_factor_gt          0.1109
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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 0.36391(7) 0.44042(6) 0.80461(4) 0.01772(19) Uani 1 1 d . . . . .
Ni2 Ni -0.05704(7) 0.65006(7) 0.66252(4) 0.01738(18) Uani 1 1 d . . . . .
Cl3 Cl 0.78088(11) 0.37599(10) 0.71860(7) 0.0256(3) Uani 1 1 d . . . . .
Cl4 Cl 0.86852(11) 0.65074(12) 0.37919(6) 0.0288(3) Uani 1 1 d . . . . .
Cl5 Cl 0.66390(11) 0.72361(12) 0.94486(7) 0.0304(3) Uani 1 1 d . . . . .
O6 O 0.8041(4) 0.4600(4) 0.7677(2) 0.0354(10) Uani 1 1 d . . . . .
O7 O 0.5522(4) 0.6957(4) 0.9354(2) 0.0418(11) Uani 1 1 d . . . . .
N8 N 0.0572(3) 0.5583(4) 0.7127(2) 0.0219(9) Uani 1 1 d . . . . .
N9 N -0.0652(3) 0.5704(3) 0.5681(2) 0.0190(9) Uani 1 1 d . . . . .
H9 H -0.0480 0.6203 0.5337 0.023 Uiso 1 1 calc R U . . .
N10 N 0.2393(4) 0.5282(4) 0.7611(2) 0.0220(9) Uani 1 1 d . . . . .
N11 N 0.1485(4) 0.5425(4) 0.7369(2) 0.0186(8) Uani 1 1 d . . . . .
N12 N 0.4976(3) 0.3561(3) 0.8527(2) 0.0187(9) Uani 1 1 d . . . . .
O13 O 0.9251(4) 0.7098(3) 0.4377(2) 0.0309(9) Uani 1 1 d . . . . .
O14 O 0.8695(3) 0.3594(4) 0.6869(2) 0.0389(11) Uani 1 1 d . . . . .
N15 N -0.1154(4) 0.6724(3) 0.7520(2) 0.0209(9) Uani 1 1 d . . . . .
H15 H -0.1268 0.6009 0.7685 0.025 Uiso 1 1 calc R U . . .
N16 N -0.2097(3) 0.7052(4) 0.6133(2) 0.0206(9) Uani 1 1 d . . . . .
N17 N 0.4754(3) 0.5582(4) 0.7965(2) 0.0191(9) Uani 1 1 d . . . . .
H17 H 0.4879 0.6006 0.8394 0.023 Uiso 1 1 calc R U . . .
O18 O 0.6867(3) 0.4021(4) 0.6671(2) 0.0381(11) Uani 1 1 d . . . . .
C19 C 0.2130(4) 0.8660(4) 0.7344(3) 0.0187(10) Uani 1 1 d . . . . .
H19 H 0.1599 0.9182 0.7331 0.022 Uiso 1 1 calc R U . . .
N20 N 0.2452(4) 0.3223(4) 0.8121(2) 0.0239(10) Uani 1 1 d . . . . .
N21 N 0.3531(4) 0.4744(4) 0.9082(2) 0.0223(9) Uani 1 1 d . . . . .
H21 H 0.2986 0.4243 0.9185 0.027 Uiso 1 1 calc R U . . .
O22 O 0.7599(5) 0.2842(4) 0.7543(3) 0.0441(12) Uani 1 1 d . . . . .
C23 C 0.3029(4) 0.4436(4) 0.6048(2) 0.0205(10) Uani 1 1 d . . . . .
C24 C 0.1956(4) 0.4340(4) 0.6087(2) 0.0178(9) Uani 1 1 d . . . . .
H24 H 0.1761 0.3865 0.6402 0.021 Uiso 1 1 calc R U . . .
C25 C 0.4564(4) 0.4423(5) 0.9531(3) 0.0243(11) Uani 1 1 d . . . . .
H25A H 0.4471 0.4322 1.0006 0.029 Uiso 1 1 calc R U . . .
H25B H 0.5119 0.4964 0.9535 0.029 Uiso 1 1 calc R U . . .
N26 N 0.3847(3) 0.3454(3) 0.7142(2) 0.0192(9) Uani 1 1 d . . . . .
H26 H 0.3202 0.2989 0.7059 0.023 Uiso 1 1 calc R U . . .
C27 C -0.1834(4) 0.5469(5) 0.5503(3) 0.0243(11) Uani 1 1 d . . . . .
H27A H -0.2024 0.5002 0.5852 0.029 Uiso 1 1 calc R U . . .
H27B H -0.2022 0.5117 0.5053 0.029 Uiso 1 1 calc R U . . .
C28 C 0.1950(4) 0.5814(4) 0.9166(3) 0.0218(11) Uani 1 1 d . . . . .
C29 C -0.2456(4) 0.6479(5) 0.5477(3) 0.0247(11) Uani 1 1 d . . . . .
H29A H -0.2331 0.6910 0.5092 0.030 Uiso 1 1 calc R U . . .
H29B H -0.3237 0.6331 0.5401 0.030 Uiso 1 1 calc R U . . .
C30 C 0.1331(4) 0.6498(5) 0.8698(2) 0.0216(10) Uani 1 1 d . . . . .
H30 H 0.1671 0.6958 0.8439 0.026 Uiso 1 1 calc R U . . .
O31 O 0.8888(6) 0.5443(4) 0.3921(3) 0.0677(19) Uani 1 1 d . . . . .
C32 C 0.5978(4) 0.4169(4) 0.8496(3) 0.0220(11) Uani 1 1 d . . . . .
H32A H 0.6536 0.3689 0.8401 0.026 Uiso 1 1 calc R U . . .
H32B H 0.6261 0.4496 0.8947 0.026 Uiso 1 1 calc R U . . .
C33 C 0.4538(4) 0.6305(4) 0.7368(3) 0.0204(11) Uani 1 1 d . . . . .
H33A H 0.4326 0.5890 0.6944 0.024 Uiso 1 1 calc R U . . .
H33B H 0.5217 0.6669 0.7348 0.024 Uiso 1 1 calc R U . . .
C34 C 0.0224(4) 0.6502(5) 0.8613(2) 0.0221(10) Uani 1 1 d . . . . .
C35 C 0.0329(5) 0.5118(5) 0.9454(3) 0.0255(12) Uani 1 1 d . . . . .
N36 N -0.0026(4) 0.7946(3) 0.6424(2) 0.0202(9) Uani 1 1 d . . . . .
H36 H 0.0021 0.8389 0.6840 0.024 Uiso 1 1 calc R U . . .
O37 O 0.7567(5) 0.6719(5) 0.3689(4) 0.0652(18) Uani 1 1 d . . . . .
C38 C 0.3147(5) 0.8938(4) 0.9122(3) 0.0243(11) Uani 1 1 d . . . . .
H38A H 0.3259 0.9455 0.9490 0.036 Uiso 1 1 calc R U . . .
H38B H 0.3696 0.8394 0.9235 0.036 Uiso 1 1 calc R U . . .
H38C H 0.2430 0.8629 0.9072 0.036 Uiso 1 1 calc R U . . .
C39 C -0.0015(4) 0.4740(4) 0.5668(3) 0.0187(10) Uani 1 1 d . . . . .
H39A H -0.0342 0.4335 0.5254 0.022 Uiso 1 1 calc R U . . .
H39B H -0.0058 0.4313 0.6073 0.022 Uiso 1 1 calc R U . . .
C40 C 0.3810(4) 0.7862(4) 0.7883(3) 0.0197(10) Uani 1 1 d . . . . .
H40 H 0.4437 0.7841 0.8242 0.024 Uiso 1 1 calc R U . . .
C41 C 0.4906(4) 0.3412(5) 0.9249(3) 0.0240(11) Uani 1 1 d . . . . .
H41A H 0.5616 0.3193 0.9524 0.029 Uiso 1 1 calc R U . . .
H41B H 0.4375 0.2862 0.9280 0.029 Uiso 1 1 calc R U . . .
C42 C 0.5766(4) 0.5004(4) 0.7949(3) 0.0204(10) Uani 1 1 d . . . . .
H42A H 0.6380 0.5494 0.8024 0.025 Uiso 1 1 calc R U . . .
H42B H 0.5705 0.4681 0.7494 0.025 Uiso 1 1 calc R U . . .
C43 C 0.1440(4) 0.5130(5) 0.9538(3) 0.0244(11) Uani 1 1 d . . . . .
H43 H 0.1864 0.4666 0.9855 0.029 Uiso 1 1 calc R U . . .
C44 C -0.2254(4) 0.7189(5) 0.7335(3) 0.0227(11) Uani 1 1 d . . . . .
H44A H -0.2200 0.7955 0.7353 0.027 Uiso 1 1 calc R U . . .
H44B H -0.2683 0.6962 0.7667 0.027 Uiso 1 1 calc R U . . .
C45 C 0.2305(6) 0.6161(5) 0.3915(3) 0.0354(14) Uani 1 1 d . . . . .
H45A H 0.2482 0.6652 0.3582 0.053 Uiso 1 1 calc R U . . .
H45B H 0.1521 0.6125 0.3861 0.053 Uiso 1 1 calc R U . . .
H45C H 0.2584 0.5473 0.3838 0.053 Uiso 1 1 calc R U . . .
C46 C 0.1033(4) 0.7973(4) 0.6225(3) 0.0196(10) Uani 1 1 d . . . . .
H46A H 0.1086 0.8625 0.5972 0.024 Uiso 1 1 calc R U . . .
H46B H 0.1068 0.7388 0.5909 0.024 Uiso 1 1 calc R U . . .
C47 C 0.4760(4) 0.2720(4) 0.7396(3) 0.0225(11) Uani 1 1 d . . . . .
H47A H 0.5430 0.3005 0.7292 0.027 Uiso 1 1 calc R U . . .
H47B H 0.4607 0.2047 0.7156 0.027 Uiso 1 1 calc R U . . .
C48 C 0.1162(4) 0.4939(4) 0.5667(2) 0.0176(10) Uani 1 1 d . . . . .
C49 C 0.3163(5) 0.5779(5) 0.9267(3) 0.0250(11) Uani 1 1 d . . . . .
H49A H 0.3402 0.6318 0.8980 0.030 Uiso 1 1 calc R U . . .
H49B H 0.3495 0.5933 0.9752 0.030 Uiso 1 1 calc R U . . .
C50 C 0.3674(4) 0.7111(4) 0.7377(3) 0.0204(10) Uani 1 1 d . . . . .
C51 C 0.1986(4) 0.7904(4) 0.6825(3) 0.0180(10) Uani 1 1 d . . . . .
C52 C -0.0273(4) 0.5815(5) 0.8991(3) 0.0241(11) Uani 1 1 d . . . . .
H52 H -0.1035 0.5825 0.8931 0.029 Uiso 1 1 calc R U . . .
C53 C 0.3302(4) 0.5144(4) 0.5583(3) 0.0216(11) Uani 1 1 d . . . . .
H53 H 0.4037 0.5214 0.5560 0.026 Uiso 1 1 calc R U . . .
C54 C 0.2821(4) 0.6528(5) 0.4646(3) 0.0240(10) Uani 1 1 d . . . . .
C55 C 0.3236(4) 0.9461(4) 0.8449(3) 0.0224(10) Uani 1 1 d . . . . .
C56 C 0.2746(4) 0.7139(4) 0.6843(3) 0.0187(10) Uani 1 1 d . . . . .
H56 H 0.2646 0.6627 0.6493 0.022 Uiso 1 1 calc R U . . .
C57 C 0.4378(5) 0.9925(5) 0.8535(3) 0.0289(12) Uani 1 1 d . . . . .
H57A H 0.4915 0.9373 0.8655 0.043 Uiso 1 1 calc R U . . .
H57B H 0.4492 1.0448 0.8899 0.043 Uiso 1 1 calc R U . . .
H57C H 0.4451 1.0250 0.8104 0.043 Uiso 1 1 calc R U . . .
C58 C 0.2379(6) 0.7601(5) 0.4755(3) 0.0339(14) Uani 1 1 d . . . . .
H58A H 0.1590 0.7571 0.4669 0.051 Uiso 1 1 calc R U . . .
H58B H 0.2598 0.8096 0.4439 0.051 Uiso 1 1 calc R U . . .
H58C H 0.2664 0.7824 0.5228 0.051 Uiso 1 1 calc R U . . .
O59 O 0.7178(5) 0.6613(7) 0.9072(4) 0.095(3) Uani 1 1 d . . . . .
C61 C 0.3049(4) 0.8653(4) 0.7881(3) 0.0201(10) Uani 1 1 d . . . . .
C62 C -0.0465(5) 0.7259(5) 0.8128(3) 0.0248(11) Uani 1 1 d . . . . .
H62A H -0.0935 0.7643 0.8378 0.030 Uiso 1 1 calc R U . . .
H62B H 0.0008 0.7768 0.7967 0.030 Uiso 1 1 calc R U . . .
C63 C -0.1975(4) 0.8178(4) 0.6014(3) 0.0229(11) Uani 1 1 d . . . . .
H63A H -0.2050 0.8573 0.6426 0.027 Uiso 1 1 calc R U . . .
H63B H -0.2545 0.8411 0.5624 0.027 Uiso 1 1 calc R U . . .
C64 C -0.0232(4) 0.4411(6) 0.9884(3) 0.0338(14) Uani 1 1 d . . . . .
C65 C 0.3925(4) 0.3763(4) 0.6439(3) 0.0213(10) Uani 1 1 d . . . . .
H65A H 0.3957 0.3124 0.6169 0.026 Uiso 1 1 calc R U . . .
H65B H 0.4615 0.4136 0.6469 0.026 Uiso 1 1 calc R U . . .
C66 C 0.1454(4) 0.5625(4) 0.5197(2) 0.0184(10) Uani 1 1 d . . . . .
H66 H 0.0911 0.6014 0.4901 0.022 Uiso 1 1 calc R U . . .
C67 C 0.1608(5) 0.2922(5) 0.8140(3) 0.0310(13) Uani 1 1 d . . . . .
O68 O 0.7131(5) 0.7362(10) 1.0127(3) 0.106(4) Uani 1 1 d . . . . .
C69 C 0.2532(5) 0.5748(4) 0.5154(3) 0.0222(11) Uani 1 1 d . . . . .
O70 O 0.9047(7) 0.6845(7) 0.3203(3) 0.090(3) Uani 1 1 d . . . . .
C72 C 0.2426(5) 1.0348(5) 0.8305(3) 0.0304(13) Uani 1 1 d . . . . .
H72A H 0.2591 1.0858 0.8677 0.046 Uiso 1 1 calc R U . . .
H72B H 0.1697 1.0076 0.8274 0.046 Uiso 1 1 calc R U . . .
H72C H 0.2468 1.0682 0.7871 0.046 Uiso 1 1 calc R U . . .
C73 C -0.2804(4) 0.6849(5) 0.6621(3) 0.0245(11) Uani 1 1 d . . . . .
H73A H -0.2971 0.6099 0.6622 0.029 Uiso 1 1 calc R U . . .
H73B H -0.3490 0.7231 0.6473 0.029 Uiso 1 1 calc R U . . .
C74 C 0.4920(5) 0.2551(4) 0.8164(3) 0.0233(11) Uani 1 1 d . . . . .
H74A H 0.4314 0.2137 0.8261 0.028 Uiso 1 1 calc R U . . .
H74B H 0.5594 0.2158 0.8332 0.028 Uiso 1 1 calc R U . . .
C75 C 0.4039(5) 0.6618(6) 0.4702(4) 0.0425(16) Uani 1 1 d . . . . .
H75A H 0.4184 0.7168 0.4396 0.064 Uiso 1 1 calc R U . . .
H75B H 0.4318 0.5957 0.4570 0.064 Uiso 1 1 calc R U . . .
H75C H 0.4393 0.6786 0.5175 0.064 Uiso 1 1 calc R U . . .
C76 C -0.1318(6) 0.4038(7) 0.9480(4) 0.0446(18) Uani 1 1 d . . . . .
H76A H -0.1226 0.3714 0.9053 0.067 Uiso 1 1 calc R U . . .
H76B H -0.1811 0.4629 0.9374 0.067 Uiso 1 1 calc R U . . .
H76C H -0.1617 0.3529 0.9752 0.067 Uiso 1 1 calc R U . . .
C77 C -0.0882(4) 0.8380(4) 0.5861(3) 0.0245(11) Uani 1 1 d . . . . .
H77A H -0.0838 0.8052 0.5421 0.029 Uiso 1 1 calc R U . . .
H77B H -0.0773 0.9136 0.5821 0.029 Uiso 1 1 calc R U . . .
O78 O 0.6677(6) 0.8274(6) 0.9184(7) 0.131(5) Uani 1 1 d . . . . .
C82 C -0.0417(8) 0.5074(9) 1.0497(4) 0.068(3) Uani 1 1 d . . . . .
H82A H -0.0939 0.5624 1.0328 0.102 Uiso 1 1 calc R U . . .
H82B H 0.0267 0.5385 1.0731 0.102 Uiso 1 1 calc R U . . .
H82C H -0.0695 0.4631 1.0818 0.102 Uiso 1 1 calc R U . . .
C89 C 0.0559(6) 0.2531(7) 0.8176(5) 0.052(2) Uani 1 1 d . . . . .
H89A H 0.0579 0.2265 0.8638 0.079 Uiso 1 1 calc R U . . .
H89B H 0.0356 0.1970 0.7842 0.079 Uiso 1 1 calc R U . . .
H89C H 0.0028 0.3092 0.8073 0.079 Uiso 1 1 calc R U . . .
C91 C 0.0458(7) 0.3502(9) 1.0159(6) 0.076(4) Uani 1 1 d . . . . .
H91A H 0.1165 0.3748 1.0407 0.114 Uiso 1 1 calc R U . . .
H91B H 0.0549 0.3055 0.9779 0.114 Uiso 1 1 calc R U . . .
H91C H 0.0113 0.3107 1.0472 0.114 Uiso 1 1 calc R U . . .
N1 N -0.0603(7) 0.9652(5) 0.7438(4) 0.066(2) Uani 1 1 d . . . . .
C2 C 0.5065(7) 0.9379(7) 0.6610(4) 0.0542(19) Uani 1 1 d . . . . .
C3 C 0.3978(6) 0.9639(7) 0.6308(5) 0.056(2) Uani 1 1 d . . . . .
H3A H 0.3494 0.9280 0.6553 0.084 Uiso 1 1 calc R U . . .
H3B H 0.3812 0.9425 0.5826 0.084 Uiso 1 1 calc R U . . .
H3C H 0.3878 1.0390 0.6337 0.084 Uiso 1 1 calc R U . . .
C4 C -0.1313(9) 1.0004(7) 0.7724(5) 0.066(3) Uani 1 1 d . . . . .
C5 C -0.2165(9) 1.0454(9) 0.8010(6) 0.083(3) Uani 1 1 d . . . . .
H5A H -0.2436 0.9934 0.8288 0.125 Uiso 1 1 calc R U . . .
H5B H -0.2753 1.0683 0.7637 0.125 Uiso 1 1 calc R U . . .
H5C H -0.1881 1.1050 0.8297 0.125 Uiso 1 1 calc R U . . .
N6 N 0.5941(7) 0.9153(9) 0.6850(5) 0.089(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N10 1.988(5) . ?
Ni1 N12 2.071(4) . ?
Ni1 N17 2.107(4) . ?
Ni1 N21 2.151(4) . ?
Ni1 N20 2.172(5) . ?
Ni1 N26 2.246(4) . ?
Ni2 N8 1.970(4) . ?
Ni2 N36 2.058(5) . ?
Ni2 N15 2.100(4) . ?
Ni2 N16 2.101(4) . ?
Ni2 N9 2.132(4) . ?
Cl3 O14 1.423(4) . ?
Cl3 O22 1.436(5) . ?
Cl3 O18 1.440(5) . ?
Cl3 O6 1.449(4) . ?
Cl4 O31 1.410(6) . ?
Cl4 O37 1.419(6) . ?
Cl4 O70 1.423(6) . ?
Cl4 O13 1.450(4) . ?
Cl5 O68 1.375(6) . ?
Cl5 O59 1.380(6) . ?
Cl5 O7 1.437(5) . ?
Cl5 O78 1.444(9) . ?
N8 N11 1.175(7) . ?
N9 C39 1.487(7) . ?
N9 C27 1.498(7) . ?
N9 H9 1.0000 . ?
N10 N11 1.166(7) . ?
N12 C41 1.479(6) . ?
N12 C74 1.485(7) . ?
N12 C32 1.508(7) . ?
N15 C44 1.492(7) . ?
N15 C62 1.504(6) . ?
N15 H15 1.0000 . ?
N16 C73 1.484(7) . ?
N16 C63 1.485(7) . ?
N16 C29 1.488(7) . ?
N17 C33 1.493(7) . ?
N17 C42 1.493(7) . ?
N17 H17 1.0000 . ?
C19 C51 1.406(7) . ?
C19 C61 1.407(7) . ?
C19 H19 0.9500 . ?
N20 C67 1.148(8) . ?
N21 C25 1.480(7) . ?
N21 C49 1.488(7) . ?
N21 H21 1.0000 . ?
C23 C24 1.388(8) . ?
C23 C53 1.398(8) . ?
C23 C65 1.510(7) . ?
C24 C48 1.398(7) . ?
C24 H24 0.9500 . ?
C25 C41 1.520(8) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
N26 C65 1.485(7) . ?
N26 C47 1.498(7) . ?
N26 H26 1.0000 . ?
C27 C29 1.519(8) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C30 1.397(8) . ?
C28 C43 1.400(8) . ?
C28 C49 1.512(8) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C34 1.381(8) . ?
C30 H30 0.9500 . ?
C32 C42 1.516(7) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C50 1.515(7) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C52 1.400(8) . ?
C34 C62 1.514(8) . ?
C35 C43 1.386(8) . ?
C35 C52 1.394(8) . ?
C35 C64 1.531(8) . ?
N36 C46 1.484(7) . ?
N36 C77 1.494(6) . ?
N36 H36 1.0000 . ?
C38 C55 1.531(7) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C48 1.519(7) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C50 1.383(7) . ?
C40 C61 1.405(7) . ?
C40 H40 0.9500 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43 0.9500 . ?
C44 C73 1.513(7) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C54 1.542(8) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C51 1.513(7) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C74 1.520(8) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C66 1.398(7) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C56 1.410(7) . ?
C51 C56 1.376(7) . ?
C52 H52 0.9500 . ?
C53 C69 1.392(8) . ?
C53 H53 0.9500 . ?
C54 C58 1.526(8) . ?
C54 C69 1.530(8) . ?
C54 C75 1.532(8) . ?
C55 C61 1.521(7) . ?
C55 C72 1.525(8) . ?
C55 C57 1.545(8) . ?
C56 H56 0.9500 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 C77 1.508(8) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 C91 1.497(11) . ?
C64 C76 1.519(9) . ?
C64 C82 1.553(11) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 C69 1.401(8) . ?
C66 H66 0.9500 . ?
C67 C89 1.442(10) . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
C77 H77A 0.9900 . ?
C77 H77B 0.9900 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C89 H89A 0.9800 . ?
C89 H89B 0.9800 . ?
C89 H89C 0.9800 . ?
C91 H91A 0.9800 . ?
C91 H91B 0.9800 . ?
C91 H91C 0.9800 . ?
N1 C4 1.253(14) . ?
C2 N6 1.151(12) . ?
C2 C3 1.423(12) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.450(16) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 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
N10 Ni1 N12 176.88(19) . . ?
N10 Ni1 N17 92.38(19) . . ?
N12 Ni1 N17 85.17(18) . . ?
N10 Ni1 N21 95.48(19) . . ?
N12 Ni1 N21 82.88(17) . . ?
N17 Ni1 N21 96.38(17) . . ?
N10 Ni1 N20 85.96(19) . . ?
N12 Ni1 N20 96.47(18) . . ?
N17 Ni1 N20 178.31(19) . . ?
N21 Ni1 N20 83.47(18) . . ?
N10 Ni1 N26 100.30(17) . . ?
N12 Ni1 N26 81.97(16) . . ?
N17 Ni1 N26 97.66(17) . . ?
N21 Ni1 N26 158.35(18) . . ?
N20 Ni1 N26 82.97(17) . . ?
N8 Ni2 N36 113.64(19) . . ?
N8 Ni2 N15 90.31(18) . . ?
N36 Ni2 N15 103.80(18) . . ?
N8 Ni2 N16 161.05(19) . . ?
N36 Ni2 N16 85.28(18) . . ?
N15 Ni2 N16 83.83(17) . . ?
N8 Ni2 N9 92.95(18) . . ?
N36 Ni2 N9 102.52(17) . . ?
N15 Ni2 N9 149.56(18) . . ?
N16 Ni2 N9 83.36(17) . . ?
O14 Cl3 O22 110.3(3) . . ?
O14 Cl3 O18 109.4(3) . . ?
O22 Cl3 O18 109.4(3) . . ?
O14 Cl3 O6 110.4(3) . . ?
O22 Cl3 O6 108.2(3) . . ?
O18 Cl3 O6 109.1(3) . . ?
O31 Cl4 O37 110.6(4) . . ?
O31 Cl4 O70 111.7(5) . . ?
O37 Cl4 O70 108.3(5) . . ?
O31 Cl4 O13 108.9(3) . . ?
O37 Cl4 O13 108.9(3) . . ?
O70 Cl4 O13 108.4(4) . . ?
O68 Cl5 O59 115.7(6) . . ?
O68 Cl5 O7 112.7(4) . . ?
O59 Cl5 O7 112.0(4) . . ?
O68 Cl5 O78 102.0(8) . . ?
O59 Cl5 O78 106.3(7) . . ?
O7 Cl5 O78 107.1(4) . . ?
N11 N8 Ni2 150.2(4) . . ?
C39 N9 C27 110.4(4) . . ?
C39 N9 Ni2 119.7(3) . . ?
C27 N9 Ni2 99.4(3) . . ?
C39 N9 H9 108.9 . . ?
C27 N9 H9 108.9 . . ?
Ni2 N9 H9 108.9 . . ?
N11 N10 Ni1 153.6(4) . . ?
N10 N11 N8 179.1(6) . . ?
C41 N12 C74 110.9(4) . . ?
C41 N12 C32 109.6(4) . . ?
C74 N12 C32 112.9(4) . . ?
C41 N12 Ni1 107.8(3) . . ?
C74 N12 Ni1 106.6(3) . . ?
C32 N12 Ni1 108.9(3) . . ?
C44 N15 C62 111.5(4) . . ?
C44 N15 Ni2 109.1(3) . . ?
C62 N15 Ni2 120.1(3) . . ?
C44 N15 H15 104.9 . . ?
C62 N15 H15 104.9 . . ?
Ni2 N15 H15 104.9 . . ?
C73 N16 C63 112.1(4) . . ?
C73 N16 C29 112.2(4) . . ?
C63 N16 C29 111.5(4) . . ?
C73 N16 Ni2 105.1(3) . . ?
C63 N16 Ni2 106.7(3) . . ?
C29 N16 Ni2 108.7(3) . . ?
C33 N17 C42 107.8(4) . . ?
C33 N17 Ni1 120.1(3) . . ?
C42 N17 Ni1 103.8(3) . . ?
C33 N17 H17 108.2 . . ?
C42 N17 H17 108.2 . . ?
Ni1 N17 H17 108.2 . . ?
C51 C19 C61 121.0(5) . . ?
C51 C19 H19 119.5 . . ?
C61 C19 H19 119.5 . . ?
C67 N20 Ni1 155.0(5) . . ?
C25 N21 C49 112.6(4) . . ?
C25 N21 Ni1 107.2(3) . . ?
C49 N21 Ni1 120.7(3) . . ?
C25 N21 H21 105.0 . . ?
C49 N21 H21 105.0 . . ?
Ni1 N21 H21 105.0 . . ?
C24 C23 C53 119.0(5) . . ?
C24 C23 C65 124.1(5) . . ?
C53 C23 C65 116.8(5) . . ?
C23 C24 C48 120.5(5) . . ?
C23 C24 H24 119.8 . . ?
C48 C24 H24 119.8 . . ?
N21 C25 C41 107.5(4) . . ?
N21 C25 H25A 110.2 . . ?
C41 C25 H25A 110.2 . . ?
N21 C25 H25B 110.2 . . ?
C41 C25 H25B 110.2 . . ?
H25A C25 H25B 108.5 . . ?
C65 N26 C47 106.6(4) . . ?
C65 N26 Ni1 131.3(3) . . ?
C47 N26 Ni1 106.7(3) . . ?
C65 N26 H26 103.0 . . ?
C47 N26 H26 103.0 . . ?
Ni1 N26 H26 103.0 . . ?
N9 C27 C29 108.8(5) . . ?
N9 C27 H27A 109.9 . . ?
C29 C27 H27A 109.9 . . ?
N9 C27 H27B 109.9 . . ?
C29 C27 H27B 109.9 . . ?
H27A C27 H27B 108.3 . . ?
C30 C28 C43 119.7(5) . . ?
C30 C28 C49 121.2(5) . . ?
C43 C28 C49 119.0(5) . . ?
N16 C29 C27 109.7(4) . . ?
N16 C29 H29A 109.7 . . ?
C27 C29 H29A 109.7 . . ?
N16 C29 H29B 109.7 . . ?
C27 C29 H29B 109.7 . . ?
H29A C29 H29B 108.2 . . ?
C34 C30 C28 119.7(5) . . ?
C34 C30 H30 120.1 . . ?
C28 C30 H30 120.1 . . ?
N12 C32 C42 112.2(4) . . ?
N12 C32 H32A 109.2 . . ?
C42 C32 H32A 109.2 . . ?
N12 C32 H32B 109.2 . . ?
C42 C32 H32B 109.2 . . ?
H32A C32 H32B 107.9 . . ?
N17 C33 C50 115.3(4) . . ?
N17 C33 H33A 108.5 . . ?
C50 C33 H33A 108.5 . . ?
N17 C33 H33B 108.5 . . ?
C50 C33 H33B 108.5 . . ?
H33A C33 H33B 107.5 . . ?
C30 C34 C52 119.9(5) . . ?
C30 C34 C62 120.9(5) . . ?
C52 C34 C62 119.1(5) . . ?
C43 C35 C52 118.2(5) . . ?
C43 C35 C64 121.6(5) . . ?
C52 C35 C64 120.1(5) . . ?
C46 N36 C77 110.2(4) . . ?
C46 N36 Ni2 115.9(3) . . ?
C77 N36 Ni2 105.4(3) . . ?
C46 N36 H36 108.4 . . ?
C77 N36 H36 108.4 . . ?
Ni2 N36 H36 108.4 . . ?
C55 C38 H38A 109.5 . . ?
C55 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C55 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N9 C39 C48 113.5(4) . . ?
N9 C39 H39A 108.9 . . ?
C48 C39 H39A 108.9 . . ?
N9 C39 H39B 108.9 . . ?
C48 C39 H39B 108.9 . . ?
H39A C39 H39B 107.7 . . ?
C50 C40 C61 121.9(5) . . ?
C50 C40 H40 119.1 . . ?
C61 C40 H40 119.1 . . ?
N12 C41 C25 109.5(4) . . ?
N12 C41 H41A 109.8 . . ?
C25 C41 H41A 109.8 . . ?
N12 C41 H41B 109.8 . . ?
C25 C41 H41B 109.8 . . ?
H41A C41 H41B 108.2 . . ?
N17 C42 C32 111.0(4) . . ?
N17 C42 H42A 109.4 . . ?
C32 C42 H42A 109.4 . . ?
N17 C42 H42B 109.4 . . ?
C32 C42 H42B 109.4 . . ?
H42A C42 H42B 108.0 . . ?
C35 C43 C28 121.2(5) . . ?
C35 C43 H43 119.4 . . ?
C28 C43 H43 119.4 . . ?
N15 C44 C73 109.6(4) . . ?
N15 C44 H44A 109.8 . . ?
C73 C44 H44A 109.8 . . ?
N15 C44 H44B 109.8 . . ?
C73 C44 H44B 109.8 . . ?
H44A C44 H44B 108.2 . . ?
C54 C45 H45A 109.5 . . ?
C54 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C54 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N36 C46 C51 113.7(4) . . ?
N36 C46 H46A 108.8 . . ?
C51 C46 H46A 108.8 . . ?
N36 C46 H46B 108.8 . . ?
C51 C46 H46B 108.8 . . ?
H46A C46 H46B 107.7 . . ?
N26 C47 C74 111.0(4) . . ?
N26 C47 H47A 109.4 . . ?
C74 C47 H47A 109.4 . . ?
N26 C47 H47B 109.4 . . ?
C74 C47 H47B 109.4 . . ?
H47A C47 H47B 108.0 . . ?
C66 C48 C24 119.4(5) . . ?
C66 C48 C39 120.8(5) . . ?
C24 C48 C39 119.3(5) . . ?
N21 C49 C28 111.1(4) . . ?
N21 C49 H49A 109.4 . . ?
C28 C49 H49A 109.4 . . ?
N21 C49 H49B 109.4 . . ?
C28 C49 H49B 109.4 . . ?
H49A C49 H49B 108.0 . . ?
C40 C50 C56 119.2(5) . . ?
C40 C50 C33 120.8(5) . . ?
C56 C50 C33 119.9(5) . . ?
C56 C51 C19 119.9(5) . . ?
C56 C51 C46 120.0(5) . . ?
C19 C51 C46 120.0(5) . . ?
C35 C52 C34 121.2(5) . . ?
C35 C52 H52 119.4 . . ?
C34 C52 H52 119.4 . . ?
C69 C53 C23 122.1(5) . . ?
C69 C53 H53 118.9 . . ?
C23 C53 H53 118.9 . . ?
C58 C54 C69 110.6(5) . . ?
C58 C54 C75 108.6(6) . . ?
C69 C54 C75 112.7(5) . . ?
C58 C54 C45 108.6(5) . . ?
C69 C54 C45 108.3(5) . . ?
C75 C54 C45 108.0(5) . . ?
C61 C55 C72 112.5(4) . . ?
C61 C55 C38 109.0(4) . . ?
C72 C55 C38 108.8(5) . . ?
C61 C55 C57 109.8(4) . . ?
C72 C55 C57 108.1(5) . . ?
C38 C55 C57 108.6(4) . . ?
C51 C56 C50 120.4(5) . . ?
C51 C56 H56 119.8 . . ?
C50 C56 H56 119.8 . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C54 C58 H58A 109.5 . . ?
C54 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C54 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C40 C61 C19 117.7(5) . . ?
C40 C61 C55 119.9(5) . . ?
C19 C61 C55 122.4(5) . . ?
N15 C62 C34 112.2(5) . . ?
N15 C62 H62A 109.2 . . ?
C34 C62 H62A 109.2 . . ?
N15 C62 H62B 109.2 . . ?
C34 C62 H62B 109.2 . . ?
H62A C62 H62B 107.9 . . ?
N16 C63 C77 109.6(4) . . ?
N16 C63 H63A 109.8 . . ?
C77 C63 H63A 109.8 . . ?
N16 C63 H63B 109.8 . . ?
C77 C63 H63B 109.8 . . ?
H63A C63 H63B 108.2 . . ?
C91 C64 C76 109.9(7) . . ?
C91 C64 C35 111.4(5) . . ?
C76 C64 C35 111.7(5) . . ?
C91 C64 C82 108.5(7) . . ?
C76 C64 C82 108.6(6) . . ?
C35 C64 C82 106.5(6) . . ?
N26 C65 C23 116.6(4) . . ?
N26 C65 H65A 108.2 . . ?
C23 C65 H65A 108.2 . . ?
N26 C65 H65B 108.2 . . ?
C23 C65 H65B 108.2 . . ?
H65A C65 H65B 107.3 . . ?
C48 C66 C69 121.2(5) . . ?
C48 C66 H66 119.4 . . ?
C69 C66 H66 119.4 . . ?
N20 C67 C89 178.7(8) . . ?
C53 C69 C66 117.8(5) . . ?
C53 C69 C54 122.6(5) . . ?
C66 C69 C54 119.6(5) . . ?
C55 C72 H72A 109.5 . . ?
C55 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C55 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
N16 C73 C44 110.3(4) . . ?
N16 C73 H73A 109.6 . . ?
C44 C73 H73A 109.6 . . ?
N16 C73 H73B 109.6 . . ?
C44 C73 H73B 109.6 . . ?
H73A C73 H73B 108.1 . . ?
N12 C74 C47 110.5(4) . . ?
N12 C74 H74A 109.6 . . ?
C47 C74 H74A 109.6 . . ?
N12 C74 H74B 109.6 . . ?
C47 C74 H74B 109.6 . . ?
H74A C74 H74B 108.1 . . ?
C54 C75 H75A 109.5 . . ?
C54 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C54 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C64 C76 H76A 109.5 . . ?
C64 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C64 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
N36 C77 C63 109.6(4) . . ?
N36 C77 H77A 109.7 . . ?
C63 C77 H77A 109.7 . . ?
N36 C77 H77B 109.7 . . ?
C63 C77 H77B 109.7 . . ?
H77A C77 H77B 108.2 . . ?
C64 C82 H82A 109.5 . . ?
C64 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C64 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C67 C89 H89A 109.5 . . ?
C67 C89 H89B 109.5 . . ?
H89A C89 H89B 109.5 . . ?
C67 C89 H89C 109.5 . . ?
H89A C89 H89C 109.5 . . ?
H89B C89 H89C 109.5 . . ?
C64 C91 H91A 109.5 . . ?
C64 C91 H91B 109.5 . . ?
H91A C91 H91B 109.5 . . ?
C64 C91 H91C 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
N6 C2 C3 179.0(12) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 C5 175.7(10) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

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
C53 C23 C24 C48 0.3(8) . . . . ?
C65 C23 C24 C48 -174.8(5) . . . . ?
C49 N21 C25 C41 -174.6(4) . . . . ?
Ni1 N21 C25 C41 -39.5(5) . . . . ?
C39 N9 C27 C29 -176.4(4) . . . . ?
Ni2 N9 C27 C29 56.9(4) . . . . ?
C73 N16 C29 C27 -95.5(5) . . . . ?
C63 N16 C29 C27 137.8(5) . . . . ?
Ni2 N16 C29 C27 20.4(5) . . . . ?
N9 C27 C29 N16 -54.4(6) . . . . ?
C43 C28 C30 C34 0.8(8) . . . . ?
C49 C28 C30 C34 179.4(5) . . . . ?
C41 N12 C32 C42 -136.3(5) . . . . ?
C74 N12 C32 C42 99.5(5) . . . . ?
Ni1 N12 C32 C42 -18.7(5) . . . . ?
C42 N17 C33 C50 -168.1(4) . . . . ?
Ni1 N17 C33 C50 73.5(5) . . . . ?
C28 C30 C34 C52 -0.5(8) . . . . ?
C28 C30 C34 C62 177.9(5) . . . . ?
C27 N9 C39 C48 165.7(4) . . . . ?
Ni2 N9 C39 C48 -80.0(5) . . . . ?
C74 N12 C41 C25 -159.8(4) . . . . ?
C32 N12 C41 C25 74.9(5) . . . . ?
Ni1 N12 C41 C25 -43.5(5) . . . . ?
N21 C25 C41 N12 56.4(6) . . . . ?
C33 N17 C42 C32 -173.9(4) . . . . ?
Ni1 N17 C42 C32 -45.6(4) . . . . ?
N12 C32 C42 N17 44.6(6) . . . . ?
C52 C35 C43 C28 -0.6(9) . . . . ?
C64 C35 C43 C28 -176.9(6) . . . . ?
C30 C28 C43 C35 -0.2(8) . . . . ?
C49 C28 C43 C35 -178.8(5) . . . . ?
C62 N15 C44 C73 164.1(5) . . . . ?
Ni2 N15 C44 C73 29.1(5) . . . . ?
C77 N36 C46 C51 160.2(4) . . . . ?
Ni2 N36 C46 C51 -80.3(5) . . . . ?
C65 N26 C47 C74 166.6(4) . . . . ?
Ni1 N26 C47 C74 22.7(5) . . . . ?
C23 C24 C48 C66 1.0(7) . . . . ?
C23 C24 C48 C39 173.7(5) . . . . ?
N9 C39 C48 C66 -50.8(6) . . . . ?
N9 C39 C48 C24 136.6(5) . . . . ?
C25 N21 C49 C28 -144.0(5) . . . . ?
Ni1 N21 C49 C28 87.7(5) . . . . ?
C30 C28 C49 N21 -118.0(5) . . . . ?
C43 C28 C49 N21 60.6(6) . . . . ?
C61 C40 C50 C56 0.1(8) . . . . ?
C61 C40 C50 C33 176.3(5) . . . . ?
N17 C33 C50 C40 64.1(7) . . . . ?
N17 C33 C50 C56 -119.7(5) . . . . ?
C61 C19 C51 C56 0.6(8) . . . . ?
C61 C19 C51 C46 -175.5(5) . . . . ?
N36 C46 C51 C56 124.4(5) . . . . ?
N36 C46 C51 C19 -59.5(6) . . . . ?
C43 C35 C52 C34 0.9(9) . . . . ?
C64 C35 C52 C34 177.2(6) . . . . ?
C30 C34 C52 C35 -0.3(8) . . . . ?
C62 C34 C52 C35 -178.7(5) . . . . ?
C24 C23 C53 C69 -0.6(8) . . . . ?
C65 C23 C53 C69 174.8(5) . . . . ?
C19 C51 C56 C50 -0.3(8) . . . . ?
C46 C51 C56 C50 175.7(5) . . . . ?
C40 C50 C56 C51 -0.1(8) . . . . ?
C33 C50 C56 C51 -176.2(5) . . . . ?
C50 C40 C61 C19 0.1(8) . . . . ?
C50 C40 C61 C55 -180.0(5) . . . . ?
C51 C19 C61 C40 -0.5(7) . . . . ?
C51 C19 C61 C55 179.6(5) . . . . ?
C72 C55 C61 C40 171.0(5) . . . . ?
C38 C55 C61 C40 -68.3(6) . . . . ?
C57 C55 C61 C40 50.6(6) . . . . ?
C72 C55 C61 C19 -9.2(7) . . . . ?
C38 C55 C61 C19 111.6(5) . . . . ?
C57 C55 C61 C19 -129.6(5) . . . . ?
C44 N15 C62 C34 140.1(5) . . . . ?
Ni2 N15 C62 C34 -90.4(5) . . . . ?
C30 C34 C62 N15 112.5(6) . . . . ?
C52 C34 C62 N15 -69.1(6) . . . . ?
C73 N16 C63 C77 149.4(4) . . . . ?
C29 N16 C63 C77 -83.8(5) . . . . ?
Ni2 N16 C63 C77 34.8(5) . . . . ?
C43 C35 C64 C91 -23.1(10) . . . . ?
C52 C35 C64 C91 160.7(7) . . . . ?
C43 C35 C64 C76 -146.5(6) . . . . ?
C52 C35 C64 C76 37.3(9) . . . . ?
C43 C35 C64 C82 95.1(8) . . . . ?
C52 C35 C64 C82 -81.1(7) . . . . ?
C47 N26 C65 C23 174.9(4) . . . . ?
Ni1 N26 C65 C23 -53.7(6) . . . . ?
C24 C23 C65 N26 -36.5(7) . . . . ?
C53 C23 C65 N26 148.3(5) . . . . ?
C24 C48 C66 C69 -2.0(7) . . . . ?
C39 C48 C66 C69 -174.6(5) . . . . ?
C23 C53 C69 C66 -0.3(8) . . . . ?
C23 C53 C69 C54 179.7(5) . . . . ?
C48 C66 C69 C53 1.7(8) . . . . ?
C48 C66 C69 C54 -178.4(5) . . . . ?
C58 C54 C69 C53 -125.8(6) . . . . ?
C75 C54 C69 C53 -4.0(8) . . . . ?
C45 C54 C69 C53 115.3(6) . . . . ?
C58 C54 C69 C66 54.3(7) . . . . ?
C75 C54 C69 C66 176.0(5) . . . . ?
C45 C54 C69 C66 -64.6(7) . . . . ?
C63 N16 C73 C44 -69.4(6) . . . . ?
C29 N16 C73 C44 164.2(5) . . . . ?
Ni2 N16 C73 C44 46.2(5) . . . . ?
N15 C44 C73 N16 -51.5(6) . . . . ?
C41 N12 C74 C47 168.3(4) . . . . ?
C32 N12 C74 C47 -68.2(5) . . . . ?
Ni1 N12 C74 C47 51.3(5) . . . . ?
N26 C47 C74 N12 -50.1(6) . . . . ?
C46 N36 C77 C63 170.1(4) . . . . ?
Ni2 N36 C77 C63 44.4(5) . . . . ?
N16 C63 C77 N36 -54.6(6) . . . . ?

_refine_diff_density_max         0.619
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.069

