# 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_Ni1
_database_code_depnum_ccdc_archive 'CCDC 1062047'
_audit_update_record             
;
2015-04-26 deposited with the CCDC.
2015-07-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H40 Cl4 N4 Ni2'
_chemical_formula_weight         787.94

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   15.376(3)
_cell_length_b                   10.184(2)
_cell_length_c                   22.865(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.27(3)
_cell_angle_gamma                90.00
_cell_volume                     3498.9(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.36
_cell_measurement_theta_max      27.52

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.643
_exptl_crystal_size_mid          0.397
_exptl_crystal_size_min          0.264
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1632
_exptl_absorpt_coefficient_mu    1.414
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6133

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            24004
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.36
_diffrn_reflns_theta_max         27.52
_reflns_number_total             7980
_reflns_number_gt                7481
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'


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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0424P)²+4.9897P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7980
_refine_ls_number_parameters     419
_refine_ls_number_restraints     540
_refine_ls_R_factor_ref          0.0488
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.1128
_refine_ls_wR_factor_gt          0.1083
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.27257(2) 0.05806(3) 0.192794(14) 0.01655(9) Uani 1 1 d U . .
Ni2 Ni 0.23887(2) -0.10807(3) 0.317729(14) 0.01694(9) Uani 1 1 d U . .
Cl4 Cl 0.34931(4) -0.08756(7) 0.40159(3) 0.02689(15) Uani 1 1 d U . .
Cl2 Cl 0.15375(4) 0.03303(7) 0.11542(3) 0.02676(15) Uani 1 1 d U . .
Cl3 Cl 0.22875(5) 0.11221(6) 0.28225(3) 0.02683(15) Uani 1 1 d U . .
Cl1 Cl 0.28831(5) -0.16073(7) 0.23023(3) 0.03263(17) Uani 1 1 d U . .
N1 N 0.28686(13) 0.2523(2) 0.17009(10) 0.0175(4) Uani 1 1 d U . .
N2 N 0.37495(13) 0.0443(2) 0.14891(9) 0.0159(4) Uani 1 1 d U . .
N4 N 0.12631(13) -0.0960(2) 0.35156(9) 0.0163(4) Uani 1 1 d U . .
N3 N 0.22011(13) -0.3031(2) 0.33694(10) 0.0177(4) Uani 1 1 d U . .
C4 C 0.33998(16) 0.3830(3) 0.09712(11) 0.0190(5) Uani 1 1 d U . .
C6 C 0.39772(15) 0.1519(2) 0.12716(11) 0.0149(4) Uani 1 1 d U . .
C21 C 0.15961(15) -0.3194(2) 0.37145(11) 0.0157(5) Uani 1 1 d U . .
C27 C 0.07126(15) 0.0184(2) 0.35096(11) 0.0168(5) Uani 1 1 d U . .
C5 C 0.34026(15) 0.2679(2) 0.13055(11) 0.0159(5) Uani 1 1 d U . .
C22 C 0.09920(15) -0.2043(2) 0.36997(11) 0.0160(5) Uani 1 1 d U . .
C23 C 0.01016(15) -0.2256(3) 0.38527(12) 0.0199(5) Uani 1 1 d U . .
H23A H -0.0156 -0.3084 0.3664 0.024 Uiso 1 1 calc R . .
H23B H -0.0300 -0.1531 0.3680 0.024 Uiso 1 1 calc R . .
C17 C 0.27383(18) -0.4024(3) 0.33031(13) 0.0247(6) Uani 1 1 d U . .
H17 H 0.3157 -0.3904 0.3056 0.030 Uiso 1 1 calc R . .
C12A C 0.5190(2) -0.0082(3) 0.24809(13) 0.0316(6) Uani 1 1 d U . .
H12A H 0.5294 0.0810 0.2351 0.047 Uiso 1 1 calc R . .
H12B H 0.5723 -0.0397 0.2761 0.047 Uiso 1 1 calc R . .
H12C H 0.4685 -0.0078 0.2680 0.047 Uiso 1 1 calc R . .
C12 C 0.49880(17) -0.0972(3) 0.19472(12) 0.0209(5) Uani 1 1 d U . .
C11 C 0.42773(15) -0.0711(2) 0.14672(11) 0.0164(5) Uani 1 1 d U . .
C28A C -0.0094(2) -0.0424(3) 0.24654(13) 0.0314(6) Uani 1 1 d U . .
H28A H 0.0438 -0.0386 0.2294 0.047 Uiso 1 1 calc R . .
H28B H -0.0611 -0.0118 0.2168 0.047 Uiso 1 1 calc R . .
H28C H -0.0194 -0.1330 0.2579 0.047 Uiso 1 1 calc R . .
C28 C 0.00359(16) 0.0438(3) 0.30082(12) 0.0203(5) Uani 1 1 d U . .
C3 C 0.28564(17) 0.4846(3) 0.10948(13) 0.0244(5) Uani 1 1 d U . .
H3 H 0.2838 0.5651 0.0883 0.029 Uiso 1 1 calc R . .
C20 C 0.15543(16) -0.4329(3) 0.40473(11) 0.0190(5) Uani 1 1 d U . .
C15 C 0.45858(18) -0.2653(3) 0.09640(13) 0.0248(6) Uani 1 1 d U . .
H15 H 0.4449 -0.3239 0.0634 0.030 Uiso 1 1 calc R . .
C7 C 0.48012(16) 0.1698(3) 0.10286(13) 0.0231(5) Uani 1 1 d U . .
H7A H 0.5203 0.0944 0.1157 0.028 Uiso 1 1 calc R . .
H7B H 0.5112 0.2501 0.1207 0.028 Uiso 1 1 calc R . .
C32 C 0.08737(17) 0.1004(3) 0.40112(12) 0.0214(5) Uani 1 1 d U . .
C14 C 0.53059(19) -0.2911(3) 0.14221(13) 0.0272(6) Uani 1 1 d U . .
H14 H 0.5668 -0.3657 0.1401 0.033 Uiso 1 1 calc R . .
C30 C -0.03833(19) 0.2325(3) 0.35273(14) 0.0285(6) Uani 1 1 d U . .
H30 H -0.0773 0.3043 0.3540 0.034 Uiso 1 1 calc R . .
C26 C 0.09819(18) -0.4473(3) 0.45071(13) 0.0250(6) Uani 1 1 d U . .
H26A H 0.1240 -0.5166 0.4796 0.030 Uiso 1 1 calc R . .
H26B H 0.0381 -0.4767 0.4302 0.030 Uiso 1 1 calc R . .
C9 C 0.38806(19) 0.2750(3) 0.00861(13) 0.0272(6) Uani 1 1 d U . .
H9A H 0.3305 0.2293 0.0055 0.033 Uiso 1 1 calc R . .
H9B H 0.3931 0.3011 -0.0323 0.033 Uiso 1 1 calc R . .
C10 C 0.38916(17) 0.3983(3) 0.04700(12) 0.0225(5) Uani 1 1 d U . .
H10A H 0.4517 0.4221 0.0644 0.027 Uiso 1 1 calc R . .
H10B H 0.3622 0.4717 0.0209 0.027 Uiso 1 1 calc R . .
C29 C -0.05102(18) 0.1515(3) 0.30303(13) 0.0270(6) Uani 1 1 d U . .
H29 H -0.0980 0.1700 0.2698 0.032 Uiso 1 1 calc R . .
C19 C 0.21187(18) -0.5361(3) 0.39644(13) 0.0256(6) Uani 1 1 d U . .
H19 H 0.2101 -0.6166 0.4172 0.031 Uiso 1 1 calc R . .
C25 C 0.08923(18) -0.3210(3) 0.48533(12) 0.0267(6) Uani 1 1 d U . .
H25A H 0.0784 -0.3442 0.5252 0.032 Uiso 1 1 calc R . .
H25B H 0.1459 -0.2716 0.4915 0.032 Uiso 1 1 calc R . .
C31 C 0.03158(19) 0.2080(3) 0.40049(13) 0.0268(6) Uani 1 1 d U . .
H31 H 0.0417 0.2662 0.4337 0.032 Uiso 1 1 calc R . .
C1 C 0.23500(17) 0.3508(3) 0.18047(13) 0.0232(5) Uani 1 1 d U . .
H1 H 0.1976 0.3385 0.2082 0.028 Uiso 1 1 calc R . .
C24 C 0.01359(17) -0.2329(3) 0.45297(12) 0.0238(5) Uani 1 1 d U . .
H24A H 0.0217 -0.1434 0.4701 0.029 Uiso 1 1 calc R . .
H24B H -0.0438 -0.2674 0.4596 0.029 Uiso 1 1 calc R . .
C8 C 0.46341(19) 0.1811(3) 0.03432(13) 0.0285(6) Uani 1 1 d U . .
H8A H 0.5186 0.2117 0.0229 0.034 Uiso 1 1 calc R . .
H8B H 0.4490 0.0931 0.0165 0.034 Uiso 1 1 calc R . .
C16 C 0.40547(16) -0.1548(3) 0.09760(12) 0.0192(5) Uani 1 1 d U . .
C13 C 0.55011(18) -0.2083(3) 0.19120(13) 0.0264(6) Uani 1 1 d U . .
H13 H 0.5993 -0.2276 0.2229 0.032 Uiso 1 1 calc R . .
C2 C 0.23452(19) 0.4703(3) 0.15187(14) 0.0280(6) Uani 1 1 d U . .
H2 H 0.1997 0.5412 0.1612 0.034 Uiso 1 1 calc R . .
C18 C 0.27033(18) -0.5217(3) 0.35818(14) 0.0276(6) Uani 1 1 d U . .
H18 H 0.3071 -0.5925 0.3514 0.033 Uiso 1 1 calc R . .
C16A C 0.32694(18) -0.1278(3) 0.04749(14) 0.0315(7) Uani 1 1 d U . .
H16A H 0.2728 -0.1222 0.0636 0.047 Uiso 1 1 calc R . .
H16B H 0.3207 -0.1991 0.0181 0.047 Uiso 1 1 calc R . .
H16C H 0.3361 -0.0446 0.0281 0.047 Uiso 1 1 calc R . .
C32A C 0.16193(19) 0.0746(3) 0.45375(14) 0.0317(7) Uani 1 1 d U . .
H32A H 0.1500 -0.0066 0.4736 0.048 Uiso 1 1 calc R . .
H32B H 0.1667 0.1480 0.4820 0.048 Uiso 1 1 calc R . .
H32C H 0.2179 0.0657 0.4401 0.048 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 2.044(2) . ?
Ni1 N1 2.068(2) . ?
Ni1 Cl2 2.2713(11) . ?
Ni1 Cl3 2.3511(8) . ?
Ni1 Cl1 2.3808(9) . ?
Ni2 N4 2.044(2) . ?
Ni2 N3 2.068(2) . ?
Ni2 Cl4 2.2848(11) . ?
Ni2 Cl1 2.3485(9) . ?
Ni2 Cl3 2.3795(8) . ?
N1 C1 1.334(3) . ?
N1 C5 1.354(3) . ?
N2 C6 1.283(3) . ?
N2 C11 1.435(3) . ?
N4 C22 1.282(3) . ?
N4 C27 1.438(3) . ?
N3 C17 1.334(3) . ?
N3 C21 1.352(3) . ?
C4 C3 1.396(4) . ?
C4 C5 1.399(4) . ?
C4 C10 1.509(3) . ?
C6 C5 1.487(3) . ?
C6 C7 1.499(3) . ?
C21 C20 1.394(4) . ?
C21 C22 1.491(3) . ?
C27 C32 1.397(4) . ?
C27 C28 1.399(4) . ?
C22 C23 1.499(3) . ?
C23 C24 1.539(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C17 C18 1.378(4) . ?
C17 H17 0.9500 . ?
C12A C12 1.499(4) . ?
C12A H12A 0.9800 . ?
C12A H12B 0.9800 . ?
C12A H12C 0.9800 . ?
C12 C13 1.391(4) . ?
C12 C11 1.400(3) . ?
C11 C16 1.394(4) . ?
C28A C28 1.498(4) . ?
C28A H28A 0.9800 . ?
C28A H28B 0.9800 . ?
C28A H28C 0.9800 . ?
C28 C29 1.389(4) . ?
C3 C2 1.379(4) . ?
C3 H3 0.9500 . ?
C20 C19 1.401(4) . ?
C20 C26 1.515(3) . ?
C15 C14 1.378(4) . ?
C15 C16 1.394(4) . ?
C15 H15 0.9500 . ?
C7 C8 1.538(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C32 C31 1.390(4) . ?
C32 C32A 1.498(4) . ?
C14 C13 1.383(4) . ?
C14 H14 0.9500 . ?
C30 C31 1.382(4) . ?
C30 C29 1.384(4) . ?
C30 H30 0.9500 . ?
C26 C25 1.532(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C9 C8 1.521(4) . ?
C9 C10 1.530(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C29 H29 0.9500 . ?
C19 C18 1.389(4) . ?
C19 H19 0.9500 . ?
C25 C24 1.529(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C31 H31 0.9500 . ?
C1 C2 1.381(4) . ?
C1 H1 0.9500 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C16 C16A 1.503(4) . ?
C13 H13 0.9500 . ?
C2 H2 0.9500 . ?
C18 H18 0.9500 . ?
C16A H16A 0.9800 . ?
C16A H16B 0.9800 . ?
C16A H16C 0.9800 . ?
C32A H32A 0.9800 . ?
C32A H32B 0.9800 . ?
C32A H32C 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
N2 Ni1 N1 78.96(8) . . ?
N2 Ni1 Cl2 100.71(6) . . ?
N1 Ni1 Cl2 91.30(6) . . ?
N2 Ni1 Cl3 146.76(7) . . ?
N1 Ni1 Cl3 93.41(6) . . ?
Cl2 Ni1 Cl3 111.85(3) . . ?
N2 Ni1 Cl1 94.71(6) . . ?
N1 Ni1 Cl1 167.71(6) . . ?
Cl2 Ni1 Cl1 100.28(3) . . ?
Cl3 Ni1 Cl1 86.15(3) . . ?
N4 Ni2 N3 79.05(8) . . ?
N4 Ni2 Cl4 102.41(6) . . ?
N3 Ni2 Cl4 91.26(6) . . ?
N4 Ni2 Cl1 142.15(7) . . ?
N3 Ni2 Cl1 92.67(6) . . ?
Cl4 Ni2 Cl1 114.74(3) . . ?
N4 Ni2 Cl3 94.18(6) . . ?
N3 Ni2 Cl3 167.47(6) . . ?
Cl4 Ni2 Cl3 100.55(3) . . ?
Cl1 Ni2 Cl3 86.24(3) . . ?
Ni1 Cl3 Ni2 93.75(3) . . ?
Ni2 Cl1 Ni1 93.78(3) . . ?
C1 N1 C5 120.1(2) . . ?
C1 N1 Ni1 125.11(17) . . ?
C5 N1 Ni1 113.07(16) . . ?
C6 N2 C11 118.9(2) . . ?
C6 N2 Ni1 115.69(16) . . ?
C11 N2 Ni1 125.02(15) . . ?
C22 N4 C27 117.9(2) . . ?
C22 N4 Ni2 115.64(17) . . ?
C27 N4 Ni2 126.10(16) . . ?
C17 N3 C21 119.5(2) . . ?
C17 N3 Ni2 125.87(17) . . ?
C21 N3 Ni2 112.70(16) . . ?
C3 C4 C5 116.3(2) . . ?
C3 C4 C10 119.7(2) . . ?
C5 C4 C10 123.9(2) . . ?
N2 C6 C5 116.4(2) . . ?
N2 C6 C7 124.7(2) . . ?
C5 C6 C7 118.8(2) . . ?
N3 C21 C20 122.5(2) . . ?
N3 C21 C22 113.2(2) . . ?
C20 C21 C22 124.3(2) . . ?
C32 C27 C28 122.3(2) . . ?
C32 C27 N4 118.3(2) . . ?
C28 C27 N4 119.4(2) . . ?
N1 C5 C4 122.1(2) . . ?
N1 C5 C6 113.1(2) . . ?
C4 C5 C6 124.8(2) . . ?
N4 C22 C21 116.1(2) . . ?
N4 C22 C23 125.3(2) . . ?
C21 C22 C23 118.5(2) . . ?
C22 C23 C24 113.8(2) . . ?
C22 C23 H23A 108.8 . . ?
C24 C23 H23A 108.8 . . ?
C22 C23 H23B 108.8 . . ?
C24 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
N3 C17 C18 122.0(2) . . ?
N3 C17 H17 119.0 . . ?
C18 C17 H17 119.0 . . ?
C12 C12A H12A 109.5 . . ?
C12 C12A H12B 109.5 . . ?
H12A C12A H12B 109.5 . . ?
C12 C12A H12C 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
C13 C12 C11 117.8(3) . . ?
C13 C12 C12A 121.1(2) . . ?
C11 C12 C12A 121.0(2) . . ?
C16 C11 C12 122.2(2) . . ?
C16 C11 N2 119.0(2) . . ?
C12 C11 N2 118.8(2) . . ?
C28 C28A H28A 109.5 . . ?
C28 C28A H28B 109.5 . . ?
H28A C28A H28B 109.5 . . ?
C28 C28A H28C 109.5 . . ?
H28A C28A H28C 109.5 . . ?
H28B C28A H28C 109.5 . . ?
C29 C28 C27 117.8(3) . . ?
C29 C28 C28A 121.2(2) . . ?
C27 C28 C28A 121.1(2) . . ?
C2 C3 C4 121.3(3) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C21 C20 C19 116.5(2) . . ?
C21 C20 C26 124.1(2) . . ?
C19 C20 C26 119.3(2) . . ?
C14 C15 C16 121.2(3) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 H15 119.4 . . ?
C6 C7 C8 114.6(2) . . ?
C6 C7 H7A 108.6 . . ?
C8 C7 H7A 108.6 . . ?
C6 C7 H7B 108.6 . . ?
C8 C7 H7B 108.6 . . ?
H7A C7 H7B 107.6 . . ?
C31 C32 C27 117.5(2) . . ?
C31 C32 C32A 120.8(3) . . ?
C27 C32 C32A 121.8(2) . . ?
C15 C14 C13 120.1(3) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C31 C30 C29 119.4(3) . . ?
C31 C30 H30 120.3 . . ?
C29 C30 H30 120.3 . . ?
C20 C26 C25 114.0(2) . . ?
C20 C26 H26A 108.8 . . ?
C25 C26 H26A 108.8 . . ?
C20 C26 H26B 108.8 . . ?
C25 C26 H26B 108.8 . . ?
H26A C26 H26B 107.6 . . ?
C8 C9 C10 112.3(2) . . ?
C8 C9 H9A 109.1 . . ?
C10 C9 H9A 109.1 . . ?
C8 C9 H9B 109.1 . . ?
C10 C9 H9B 109.1 . . ?
H9A C9 H9B 107.9 . . ?
C4 C10 C9 113.9(2) . . ?
C4 C10 H10A 108.8 . . ?
C9 C10 H10A 108.8 . . ?
C4 C10 H10B 108.8 . . ?
C9 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
C30 C29 C28 121.3(3) . . ?
C30 C29 H29 119.3 . . ?
C28 C29 H29 119.3 . . ?
C18 C19 C20 120.5(3) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 H19 119.7 . . ?
C24 C25 C26 112.6(2) . . ?
C24 C25 H25A 109.1 . . ?
C26 C25 H25A 109.1 . . ?
C24 C25 H25B 109.1 . . ?
C26 C25 H25B 109.1 . . ?
H25A C25 H25B 107.8 . . ?
C30 C31 C32 121.7(3) . . ?
C30 C31 H31 119.2 . . ?
C32 C31 H31 119.2 . . ?
N1 C1 C2 121.5(2) . . ?
N1 C1 H1 119.3 . . ?
C2 C1 H1 119.3 . . ?
C25 C24 C23 112.0(2) . . ?
C25 C24 H24A 109.2 . . ?
C23 C24 H24A 109.2 . . ?
C25 C24 H24B 109.2 . . ?
C23 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
C9 C8 C7 112.9(2) . . ?
C9 C8 H8A 109.0 . . ?
C7 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
C7 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C11 C16 C15 117.7(2) . . ?
C11 C16 C16A 121.5(2) . . ?
C15 C16 C16A 120.8(3) . . ?
C14 C13 C12 120.9(3) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C3 C2 C1 118.6(3) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C17 C18 C19 118.6(3) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 H18 120.7 . . ?
C16 C16A H16A 109.5 . . ?
C16 C16A H16B 109.5 . . ?
H16A C16A H16B 109.5 . . ?
C16 C16A H16C 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
C32 C32A H32A 109.5 . . ?
C32 C32A H32B 109.5 . . ?
H32A C32A H32B 109.5 . . ?
C32 C32A H32C 109.5 . . ?
H32A C32A H32C 109.5 . . ?
H32B C32A H32C 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
N2 Ni1 Cl3 Ni2 -94.88(11) . . . . ?
N1 Ni1 Cl3 Ni2 -169.86(6) . . . . ?
Cl2 Ni1 Cl3 Ni2 97.37(3) . . . . ?
Cl1 Ni1 Cl3 Ni2 -2.16(3) . . . . ?
N4 Ni2 Cl3 Ni1 -139.87(6) . . . . ?
N3 Ni2 Cl3 Ni1 -83.2(3) . . . . ?
Cl4 Ni2 Cl3 Ni1 116.67(3) . . . . ?
Cl1 Ni2 Cl3 Ni1 2.19(3) . . . . ?
N4 Ni2 Cl1 Ni1 89.80(11) . . . . ?
N3 Ni2 Cl1 Ni1 165.33(6) . . . . ?
Cl4 Ni2 Cl1 Ni1 -102.05(3) . . . . ?
Cl3 Ni2 Cl1 Ni1 -2.17(3) . . . . ?
N2 Ni1 Cl1 Ni2 148.87(6) . . . . ?
N1 Ni1 Cl1 Ni2 90.5(3) . . . . ?
Cl2 Ni1 Cl1 Ni2 -109.33(3) . . . . ?
Cl3 Ni1 Cl1 Ni2 2.19(3) . . . . ?
N2 Ni1 N1 C1 176.3(2) . . . . ?
Cl2 Ni1 N1 C1 75.7(2) . . . . ?
Cl3 Ni1 N1 C1 -36.3(2) . . . . ?
Cl1 Ni1 N1 C1 -123.8(3) . . . . ?
N2 Ni1 N1 C5 11.55(16) . . . . ?
Cl2 Ni1 N1 C5 -89.11(16) . . . . ?
Cl3 Ni1 N1 C5 158.91(16) . . . . ?
Cl1 Ni1 N1 C5 71.4(4) . . . . ?
N1 Ni1 N2 C6 -2.20(18) . . . . ?
Cl2 Ni1 N2 C6 87.03(18) . . . . ?
Cl3 Ni1 N2 C6 -81.4(2) . . . . ?
Cl1 Ni1 N2 C6 -171.56(17) . . . . ?
N1 Ni1 N2 C11 170.6(2) . . . . ?
Cl2 Ni1 N2 C11 -100.14(19) . . . . ?
Cl3 Ni1 N2 C11 91.4(2) . . . . ?
Cl1 Ni1 N2 C11 1.27(19) . . . . ?
N3 Ni2 N4 C22 2.41(18) . . . . ?
Cl4 Ni2 N4 C22 -86.47(18) . . . . ?
Cl1 Ni2 N4 C22 82.5(2) . . . . ?
Cl3 Ni2 N4 C22 171.77(18) . . . . ?
N3 Ni2 N4 C27 -171.0(2) . . . . ?
Cl4 Ni2 N4 C27 100.08(19) . . . . ?
Cl1 Ni2 N4 C27 -90.9(2) . . . . ?
Cl3 Ni2 N4 C27 -1.7(2) . . . . ?
N4 Ni2 N3 C17 -176.9(2) . . . . ?
Cl4 Ni2 N3 C17 -74.5(2) . . . . ?
Cl1 Ni2 N3 C17 40.3(2) . . . . ?
Cl3 Ni2 N3 C17 125.0(3) . . . . ?
N4 Ni2 N3 C21 -12.79(16) . . . . ?
Cl4 Ni2 N3 C21 89.62(17) . . . . ?
Cl1 Ni2 N3 C21 -155.55(16) . . . . ?
Cl3 Ni2 N3 C21 -70.9(4) . . . . ?
C11 N2 C6 C5 179.8(2) . . . . ?
Ni1 N2 C6 C5 -6.9(3) . . . . ?
C11 N2 C6 C7 -4.4(4) . . . . ?
Ni1 N2 C6 C7 168.9(2) . . . . ?
C17 N3 C21 C20 5.3(4) . . . . ?
Ni2 N3 C21 C20 -159.9(2) . . . . ?
C17 N3 C21 C22 -174.7(2) . . . . ?
Ni2 N3 C21 C22 20.0(3) . . . . ?
C22 N4 C27 C32 92.6(3) . . . . ?
Ni2 N4 C27 C32 -94.1(3) . . . . ?
C22 N4 C27 C28 -87.1(3) . . . . ?
Ni2 N4 C27 C28 86.3(3) . . . . ?
C1 N1 C5 C4 -3.4(4) . . . . ?
Ni1 N1 C5 C4 162.20(19) . . . . ?
C1 N1 C5 C6 176.3(2) . . . . ?
Ni1 N1 C5 C6 -18.0(2) . . . . ?
C3 C4 C5 N1 3.9(4) . . . . ?
C10 C4 C5 N1 -171.7(2) . . . . ?
C3 C4 C5 C6 -175.8(2) . . . . ?
C10 C4 C5 C6 8.5(4) . . . . ?
N2 C6 C5 N1 16.9(3) . . . . ?
C7 C6 C5 N1 -159.2(2) . . . . ?
N2 C6 C5 C4 -163.3(2) . . . . ?
C7 C6 C5 C4 20.6(4) . . . . ?
C27 N4 C22 C21 -178.3(2) . . . . ?
Ni2 N4 C22 C21 7.7(3) . . . . ?
C27 N4 C22 C23 6.5(4) . . . . ?
Ni2 N4 C22 C23 -167.47(19) . . . . ?
N3 C21 C22 N4 -18.8(3) . . . . ?
C20 C21 C22 N4 161.1(2) . . . . ?
N3 C21 C22 C23 156.7(2) . . . . ?
C20 C21 C22 C23 -23.4(4) . . . . ?
N4 C22 C23 C24 -105.1(3) . . . . ?
C21 C22 C23 C24 79.9(3) . . . . ?
C21 N3 C17 C18 -0.7(4) . . . . ?
Ni2 N3 C17 C18 162.5(2) . . . . ?
C13 C12 C11 C16 2.6(4) . . . . ?
C12A C12 C11 C16 -177.5(2) . . . . ?
C13 C12 C11 N2 -178.9(2) . . . . ?
C12A C12 C11 N2 1.0(4) . . . . ?
C6 N2 C11 C16 -91.2(3) . . . . ?
Ni1 N2 C11 C16 96.1(2) . . . . ?
C6 N2 C11 C12 90.1(3) . . . . ?
Ni1 N2 C11 C12 -82.5(3) . . . . ?
C32 C27 C28 C29 -2.8(4) . . . . ?
N4 C27 C28 C29 176.9(2) . . . . ?
C32 C27 C28 C28A 177.1(2) . . . . ?
N4 C27 C28 C28A -3.2(4) . . . . ?
C5 C4 C3 C2 -0.8(4) . . . . ?
C10 C4 C3 C2 175.1(3) . . . . ?
N3 C21 C20 C19 -5.9(4) . . . . ?
C22 C21 C20 C19 174.2(2) . . . . ?
N3 C21 C20 C26 170.6(2) . . . . ?
C22 C21 C20 C26 -9.3(4) . . . . ?
N2 C6 C7 C8 107.3(3) . . . . ?
C5 C6 C7 C8 -77.0(3) . . . . ?
C28 C27 C32 C31 1.8(4) . . . . ?
N4 C27 C32 C31 -177.9(2) . . . . ?
C28 C27 C32 C32A -178.0(3) . . . . ?
N4 C27 C32 C32A 2.3(4) . . . . ?
C16 C15 C14 C13 1.5(4) . . . . ?
C21 C20 C26 C25 -34.6(4) . . . . ?
C19 C20 C26 C25 141.9(3) . . . . ?
C3 C4 C10 C9 -137.9(3) . . . . ?
C5 C4 C10 C9 37.6(4) . . . . ?
C8 C9 C10 C4 -86.7(3) . . . . ?
C31 C30 C29 C28 1.8(4) . . . . ?
C27 C28 C29 C30 0.9(4) . . . . ?
C28A C28 C29 C30 -178.9(3) . . . . ?
C21 C20 C19 C18 2.0(4) . . . . ?
C26 C20 C19 C18 -174.7(3) . . . . ?
C20 C26 C25 C24 86.3(3) . . . . ?
C29 C30 C31 C32 -2.9(4) . . . . ?
C27 C32 C31 C30 1.1(4) . . . . ?
C32A C32 C31 C30 -179.1(3) . . . . ?
C5 N1 C1 C2 -0.3(4) . . . . ?
Ni1 N1 C1 C2 -164.2(2) . . . . ?
C26 C25 C24 C23 -42.0(3) . . . . ?
C22 C23 C24 C25 -45.7(3) . . . . ?
C10 C9 C8 C7 40.2(3) . . . . ?
C6 C7 C8 C9 46.5(3) . . . . ?
C12 C11 C16 C15 -2.2(4) . . . . ?
N2 C11 C16 C15 179.3(2) . . . . ?
C12 C11 C16 C16A 177.8(2) . . . . ?
N2 C11 C16 C16A -0.8(4) . . . . ?
C14 C15 C16 C11 0.1(4) . . . . ?
C14 C15 C16 C16A -179.8(3) . . . . ?
C15 C14 C13 C12 -1.1(4) . . . . ?
C11 C12 C13 C14 -0.9(4) . . . . ?
C12A C12 C13 C14 179.2(3) . . . . ?
C4 C3 C2 C1 -2.7(4) . . . . ?
N1 C1 C2 C3 3.4(4) . . . . ?
N3 C17 C18 C19 -3.1(4) . . . . ?
C20 C19 C18 C17 2.3(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.102
####################################################################### 
# 
# 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_Ni3
_database_code_depnum_ccdc_archive 'CCDC 1062048'
_audit_update_record             
;
2015-04-26 deposited with the CCDC.
2015-07-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H56 Cl4 N4 Ni2'
_chemical_formula_weight         900.15

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   10.330(2)
_cell_length_b                   14.356(3)
_cell_length_c                   14.999(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.47(3)
_cell_angle_gamma                90.00
_cell_volume                     2153.8(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.99
_cell_measurement_theta_max      27.50

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.638
_exptl_crystal_size_mid          0.591
_exptl_crystal_size_min          0.174
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             944
_exptl_absorpt_coefficient_mu    1.158
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7191

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            11130
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4924
_reflns_number_gt                4462
_reflns_threshold_expression     >2sigma(I)


_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'


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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0760P)²+1.1597P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4924
_refine_ls_number_parameters     248
_refine_ls_number_restraints     318
_refine_ls_R_factor_ref          0.0501
_refine_ls_R_factor_gt           0.0449
_refine_ls_wR_factor_ref         0.1385
_refine_ls_wR_factor_gt          0.1303
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.89371(3) 0.45249(2) 0.05957(2) 0.02711(12) Uani 1 1 d U . .
Cl1 Cl 1.12283(7) 0.45153(5) 0.07426(5) 0.0458(2) Uani 1 1 d U . .
Cl2 Cl 0.86111(7) 0.56659(4) 0.15722(5) 0.04098(18) Uani 1 1 d U . .
N2 N 0.88992(19) 0.34585(12) 0.15250(13) 0.0241(4) Uani 1 1 d U . .
N1 N 0.7020(2) 0.40565(13) 0.01607(14) 0.0260(4) Uani 1 1 d U . .
C11 C 1.0085(2) 0.30111(16) 0.20848(16) 0.0278(5) Uani 1 1 d U . .
C1 C 0.6146(2) 0.42745(17) -0.06261(17) 0.0303(5) Uani 1 1 d U . .
H1 H 0.6454 0.4595 -0.1088 0.036 Uiso 1 1 calc R . .
C5 C 0.6598(2) 0.35893(15) 0.08217(16) 0.0261(5) Uani 1 1 d U . .
C6 C 0.7721(2) 0.32388(15) 0.15784(16) 0.0258(4) Uani 1 1 d U . .
C7 C 0.7423(3) 0.26052(17) 0.22942(19) 0.0348(5) Uani 1 1 d U . .
H7A H 0.8276 0.2365 0.2684 0.042 Uiso 1 1 calc R . .
H7B H 0.6903 0.2066 0.1984 0.042 Uiso 1 1 calc R . .
C3 C 0.4346(3) 0.36377(17) -0.0103(2) 0.0351(5) Uani 1 1 d U . .
H3 H 0.3420 0.3511 -0.0193 0.042 Uiso 1 1 calc R . .
C4 C 0.5242(2) 0.34024(16) 0.07356(18) 0.0313(5) Uani 1 1 d U . .
C2 C 0.4796(3) 0.40478(17) -0.07940(19) 0.0334(5) Uani 1 1 d U . .
H2 H 0.4200 0.4175 -0.1375 0.040 Uiso 1 1 calc R . .
C16 C 1.0583(3) 0.22512(19) 0.16936(17) 0.0337(5) Uani 1 1 d U . .
C12 C 1.0728(3) 0.33563(18) 0.29557(17) 0.0360(6) Uani 1 1 d U . .
C16A C 0.9860(3) 0.1841(2) 0.07748(19) 0.0434(7) Uani 1 1 d U . .
H16A H 0.9093 0.2261 0.0499 0.052 Uiso 1 1 calc R . .
C12A C 1.0173(4) 0.41533(18) 0.33994(19) 0.0438(7) Uani 1 1 d U . .
H12A H 0.9286 0.4329 0.2988 0.053 Uiso 1 1 calc R . .
C10 C 0.4663(3) 0.3044(2) 0.1500(2) 0.0474(7) Uani 1 1 d U . .
H10A H 0.4797 0.2362 0.1558 0.057 Uiso 1 1 calc R . .
H10B H 0.3690 0.3167 0.1343 0.057 Uiso 1 1 calc R . .
C14 C 1.2453(3) 0.2190(2) 0.3046(2) 0.0500(8) Uani 1 1 d U . .
H14 H 1.3272 0.1917 0.3372 0.060 Uiso 1 1 calc R . .
C8 C 0.6639(3) 0.3077(2) 0.2912(2) 0.0437(7) Uani 1 1 d U . .
H8A H 0.6472 0.2610 0.3356 0.052 Uiso 1 1 calc R . .
H8B H 0.7207 0.3571 0.3271 0.052 Uiso 1 1 calc R . .
C15 C 1.1781(3) 0.1852(2) 0.2191(2) 0.0431(6) Uani 1 1 d U . .
H15 H 1.2142 0.1336 0.1937 0.052 Uiso 1 1 calc R . .
C13 C 1.1919(3) 0.2926(2) 0.3418(2) 0.0458(7) Uani 1 1 d U . .
H13 H 1.2376 0.3150 0.4009 0.055 Uiso 1 1 calc R . .
C9 C 0.5315(3) 0.3505(2) 0.2421(2) 0.0504(8) Uani 1 1 d U . .
H9A H 0.5455 0.4173 0.2313 0.061 Uiso 1 1 calc R . .
H9B H 0.4693 0.3462 0.2826 0.061 Uiso 1 1 calc R . .
C12C C 0.9952(4) 0.3863(2) 0.4332(2) 0.0597(10) Uani 1 1 d U . .
H12B H 0.9458 0.3273 0.4264 0.089 Uiso 1 1 calc R . .
H12C H 0.9437 0.4345 0.4553 0.089 Uiso 1 1 calc R . .
H12D H 1.0818 0.3783 0.4776 0.089 Uiso 1 1 calc R . .
C16B C 1.0759(4) 0.1798(3) 0.0103(2) 0.0663(10) Uani 1 1 d U . .
H16B H 1.1125 0.2418 0.0044 0.099 Uiso 1 1 calc R . .
H16C H 1.0234 0.1587 -0.0501 0.099 Uiso 1 1 calc R . .
H16D H 1.1494 0.1360 0.0337 0.099 Uiso 1 1 calc R . .
C16C C 0.9288(4) 0.0893(3) 0.0912(3) 0.0692(11) Uani 1 1 d U . .
H16F H 1.0018 0.0464 0.1182 0.104 Uiso 1 1 calc R . .
H16G H 0.8782 0.0649 0.0316 0.104 Uiso 1 1 calc R . .
H16E H 0.8693 0.0953 0.1325 0.104 Uiso 1 1 calc R . .
C12B C 1.1092(4) 0.5006(2) 0.3502(2) 0.0607(10) Uani 1 1 d U . .
H12E H 1.1960 0.4856 0.3919 0.091 Uiso 1 1 calc R . .
H12F H 1.0685 0.5527 0.3755 0.091 Uiso 1 1 calc R . .
H12G H 1.1219 0.5180 0.2898 0.091 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 2.038(2) . ?
Ni1 N2 2.0774(18) . ?
Ni1 Cl2 2.2778(8) . ?
Ni1 Cl1 2.3216(8) . ?
Ni1 Cl1 2.4053(8) 3_765 ?
Cl1 Ni1 2.4053(8) 3_765 ?
N2 C6 1.279(3) . ?
N2 C11 1.451(3) . ?
N1 C1 1.331(3) . ?
N1 C5 1.356(3) . ?
C11 C16 1.396(3) . ?
C11 C12 1.400(3) . ?
C1 C2 1.392(3) . ?
C1 H1 0.9500 . ?
C5 C4 1.401(3) . ?
C5 C6 1.493(3) . ?
C6 C7 1.497(3) . ?
C7 C8 1.533(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C3 C2 1.370(4) . ?
C3 C4 1.404(4) . ?
C3 H3 0.9500 . ?
C4 C10 1.510(4) . ?
C2 H2 0.9500 . ?
C16 C15 1.399(4) . ?
C16 C16A 1.513(4) . ?
C12 C13 1.396(4) . ?
C12 C12A 1.508(4) . ?
C16A C16C 1.519(5) . ?
C16A C16B 1.533(4) . ?
C16A H16A 1.0000 . ?
C12A C12C 1.530(4) . ?
C12A C12B 1.534(4) . ?
C12A H12A 1.0000 . ?
C10 C9 1.527(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C14 C13 1.372(5) . ?
C14 C15 1.385(4) . ?
C14 H14 0.9500 . ?
C8 C9 1.512(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C15 H15 0.9500 . ?
C13 H13 0.9500 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C12C H12B 0.9800 . ?
C12C H12C 0.9800 . ?
C12C H12D 0.9800 . ?
C16B H16B 0.9800 . ?
C16B H16C 0.9800 . ?
C16B H16D 0.9800 . ?
C16C H16F 0.9800 . ?
C16C H16G 0.9800 . ?
C16C H16E 0.9800 . ?
C12B H12E 0.9800 . ?
C12B H12F 0.9800 . ?
C12B H12G 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
N1 Ni1 N2 77.99(8) . . ?
N1 Ni1 Cl2 98.92(6) . . ?
N2 Ni1 Cl2 93.89(6) . . ?
N1 Ni1 Cl1 156.13(6) . . ?
N2 Ni1 Cl1 96.99(6) . . ?
Cl2 Ni1 Cl1 104.73(4) . . ?
N1 Ni1 Cl1 93.50(6) . 3_765 ?
N2 Ni1 Cl1 166.60(6) . 3_765 ?
Cl2 Ni1 Cl1 97.68(3) . 3_765 ?
Cl1 Ni1 Cl1 86.60(4) . 3_765 ?
Ni1 Cl1 Ni1 93.40(4) . 3_765 ?
C6 N2 C11 122.27(19) . . ?
C6 N2 Ni1 113.67(16) . . ?
C11 N2 Ni1 124.04(14) . . ?
C1 N1 C5 119.6(2) . . ?
C1 N1 Ni1 126.53(16) . . ?
C5 N1 Ni1 113.15(16) . . ?
C16 C11 C12 122.0(2) . . ?
C16 C11 N2 116.7(2) . . ?
C12 C11 N2 121.2(2) . . ?
N1 C1 C2 122.1(2) . . ?
N1 C1 H1 118.9 . . ?
C2 C1 H1 118.9 . . ?
N1 C5 C4 121.6(2) . . ?
N1 C5 C6 113.09(19) . . ?
C4 C5 C6 125.1(2) . . ?
N2 C6 C5 116.10(19) . . ?
N2 C6 C7 124.4(2) . . ?
C5 C6 C7 119.4(2) . . ?
C6 C7 C8 113.6(2) . . ?
C6 C7 H7A 108.9 . . ?
C8 C7 H7A 108.9 . . ?
C6 C7 H7B 108.9 . . ?
C8 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
C2 C3 C4 120.6(2) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 117.1(2) . . ?
C5 C4 C10 124.9(2) . . ?
C3 C4 C10 117.8(2) . . ?
C3 C2 C1 118.5(2) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C11 C16 C15 117.8(2) . . ?
C11 C16 C16A 122.5(2) . . ?
C15 C16 C16A 119.7(2) . . ?
C13 C12 C11 117.4(3) . . ?
C13 C12 C12A 120.1(3) . . ?
C11 C12 C12A 122.4(3) . . ?
C16 C16A C16C 110.2(3) . . ?
C16 C16A C16B 111.9(3) . . ?
C16C C16A C16B 111.9(3) . . ?
C16 C16A H16A 107.5 . . ?
C16C C16A H16A 107.5 . . ?
C16B C16A H16A 107.5 . . ?
C12 C12A C12C 110.9(2) . . ?
C12 C12A C12B 110.8(3) . . ?
C12C C12A C12B 110.9(2) . . ?
C12 C12A H12A 108.0 . . ?
C12C C12A H12A 108.0 . . ?
C12B C12A H12A 108.0 . . ?
C4 C10 C9 111.8(2) . . ?
C4 C10 H10A 109.3 . . ?
C9 C10 H10A 109.3 . . ?
C4 C10 H10B 109.3 . . ?
C9 C10 H10B 109.3 . . ?
H10A C10 H10B 107.9 . . ?
C13 C14 C15 119.1(3) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C9 C8 C7 115.8(2) . . ?
C9 C8 H8A 108.3 . . ?
C7 C8 H8A 108.3 . . ?
C9 C8 H8B 108.3 . . ?
C7 C8 H8B 108.3 . . ?
H8A C8 H8B 107.4 . . ?
C14 C15 C16 121.4(3) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
C14 C13 C12 122.2(3) . . ?
C14 C13 H13 118.9 . . ?
C12 C13 H13 118.9 . . ?
C8 C9 C10 113.9(3) . . ?
C8 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
C8 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C12A C12C H12B 109.5 . . ?
C12A C12C H12C 109.5 . . ?
H12B C12C H12C 109.5 . . ?
C12A C12C H12D 109.5 . . ?
H12B C12C H12D 109.5 . . ?
H12C C12C H12D 109.5 . . ?
C16A C16B H16B 109.5 . . ?
C16A C16B H16C 109.5 . . ?
H16B C16B H16C 109.5 . . ?
C16A C16B H16D 109.5 . . ?
H16B C16B H16D 109.5 . . ?
H16C C16B H16D 109.5 . . ?
C16A C16C H16F 109.5 . . ?
C16A C16C H16G 109.5 . . ?
H16F C16C H16G 109.5 . . ?
C16A C16C H16E 109.5 . . ?
H16F C16C H16E 109.5 . . ?
H16G C16C H16E 109.5 . . ?
C12A C12B H12E 109.5 . . ?
C12A C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
C12A C12B H12G 109.5 . . ?
H12E C12B H12G 109.5 . . ?
H12F C12B H12G 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
N1 Ni1 Cl1 Ni1 90.98(14) . . . 3_765 ?
N2 Ni1 Cl1 Ni1 167.04(6) . . . 3_765 ?
Cl2 Ni1 Cl1 Ni1 -97.05(4) . . . 3_765 ?
Cl1 Ni1 Cl1 Ni1 0.0 3_765 . . 3_765 ?
N1 Ni1 N2 C6 -20.06(16) . . . . ?
Cl2 Ni1 N2 C6 78.24(16) . . . . ?
Cl1 Ni1 N2 C6 -176.39(15) . . . . ?
Cl1 Ni1 N2 C6 -71.5(3) 3_765 . . . ?
N1 Ni1 N2 C11 161.43(18) . . . . ?
Cl2 Ni1 N2 C11 -100.27(17) . . . . ?
Cl1 Ni1 N2 C11 5.11(17) . . . . ?
Cl1 Ni1 N2 C11 110.0(3) 3_765 . . . ?
N2 Ni1 N1 C1 -168.3(2) . . . . ?
Cl2 Ni1 N1 C1 99.60(19) . . . . ?
Cl1 Ni1 N1 C1 -88.3(2) . . . . ?
Cl1 Ni1 N1 C1 1.26(19) 3_765 . . . ?
N2 Ni1 N1 C5 21.50(15) . . . . ?
Cl2 Ni1 N1 C5 -70.62(15) . . . . ?
Cl1 Ni1 N1 C5 101.52(18) . . . . ?
Cl1 Ni1 N1 C5 -168.96(14) 3_765 . . . ?
C6 N2 C11 C16 93.8(3) . . . . ?
Ni1 N2 C11 C16 -87.8(2) . . . . ?
C6 N2 C11 C12 -89.1(3) . . . . ?
Ni1 N2 C11 C12 89.3(2) . . . . ?
C5 N1 C1 C2 0.8(3) . . . . ?
Ni1 N1 C1 C2 -168.86(18) . . . . ?
C1 N1 C5 C4 -6.0(3) . . . . ?
Ni1 N1 C5 C4 164.99(17) . . . . ?
C1 N1 C5 C6 169.0(2) . . . . ?
Ni1 N1 C5 C6 -20.1(2) . . . . ?
C11 N2 C6 C5 -166.29(19) . . . . ?
Ni1 N2 C6 C5 15.2(2) . . . . ?
C11 N2 C6 C7 8.6(3) . . . . ?
Ni1 N2 C6 C7 -169.90(18) . . . . ?
N1 C5 C6 N2 3.1(3) . . . . ?
C4 C5 C6 N2 177.8(2) . . . . ?
N1 C5 C6 C7 -172.1(2) . . . . ?
C4 C5 C6 C7 2.6(3) . . . . ?
N2 C6 C7 C8 118.3(3) . . . . ?
C5 C6 C7 C8 -67.0(3) . . . . ?
N1 C5 C4 C3 6.1(3) . . . . ?
C6 C5 C4 C3 -168.2(2) . . . . ?
N1 C5 C4 C10 -168.5(2) . . . . ?
C6 C5 C4 C10 17.1(4) . . . . ?
C2 C3 C4 C5 -1.2(4) . . . . ?
C2 C3 C4 C10 173.8(2) . . . . ?
C4 C3 C2 C1 -3.7(4) . . . . ?
N1 C1 C2 C3 4.0(4) . . . . ?
C12 C11 C16 C15 -1.7(4) . . . . ?
N2 C11 C16 C15 175.3(2) . . . . ?
C12 C11 C16 C16A 176.8(2) . . . . ?
N2 C11 C16 C16A -6.1(4) . . . . ?
C16 C11 C12 C13 1.7(4) . . . . ?
N2 C11 C12 C13 -175.3(2) . . . . ?
C16 C11 C12 C12A -177.7(2) . . . . ?
N2 C11 C12 C12A 5.4(4) . . . . ?
C11 C16 C16A C16C -109.2(3) . . . . ?
C15 C16 C16A C16C 69.3(4) . . . . ?
C11 C16 C16A C16B 125.5(3) . . . . ?
C15 C16 C16A C16B -55.9(4) . . . . ?
C13 C12 C12A C12C -57.1(4) . . . . ?
C11 C12 C12A C12C 122.2(3) . . . . ?
C13 C12 C12A C12B 66.5(3) . . . . ?
C11 C12 C12A C12B -114.2(3) . . . . ?
C5 C4 C10 C9 40.1(4) . . . . ?
C3 C4 C10 C9 -134.5(3) . . . . ?
C6 C7 C8 C9 57.2(3) . . . . ?
C13 C14 C15 C16 0.9(5) . . . . ?
C11 C16 C15 C14 0.4(4) . . . . ?
C16A C16 C15 C14 -178.2(3) . . . . ?
C15 C14 C13 C12 -1.0(4) . . . . ?
C11 C12 C13 C14 -0.3(4) . . . . ?
C12A C12 C13 C14 179.1(3) . . . . ?
C7 C8 C9 C10 26.9(4) . . . . ?
C4 C10 C9 C8 -81.7(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.199

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.163 0.432 0.637 10.7 2.3
2 0.336 0.932 0.863 10.7 2.2
3 0.663 0.068 0.137 10.7 2.3
4 0.837 0.568 0.363 10.7 2.1
_platon_squeeze_details          
; ?
;
#==END
