# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_aa2
_database_code_depnum_ccdc_archive 'CCDC 910520'
_audit_update_record             
;
2012-11-12 deposited with the CCDC.
2015-03-18 downloaded from the CCDC.
;
#TrackingRef '2.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H29 Cl2 N5 Ni O5'
_chemical_formula_sum            'C29 H29 Cl2 N5 Ni O5'
_chemical_formula_weight         657.18

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   22.221(4)
_cell_length_b                   15.276(3)
_cell_length_c                   17.848(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.16(3)
_cell_angle_gamma                90.00
_cell_volume                     5899(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            Blue
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2720
_exptl_absorpt_coefficient_mu    0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7181
_exptl_absorpt_correction_T_max  0.9166
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16912
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         25.01
_reflns_number_total             5164
_reflns_number_gt                4234
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0422P)²+8.6451P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5164
_refine_ls_number_parameters     388
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0550
_refine_ls_wR_factor_ref         0.1283
_refine_ls_wR_factor_gt          0.1207
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.128
_refine_ls_shift/su_mean         0.003

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 0.22156(2) -0.04765(3) 0.06565(3) 0.03108(16) Uani 1 1 d . . .
Cl1 Cl 0.21972(5) -0.19006(6) 0.11862(6) 0.0430(3) Uani 1 1 d . . .
Cl2 Cl 0.08205(5) 0.71745(7) 0.62418(7) 0.0547(3) Uani 1 1 d . . .
O1 O 0.0460(2) 0.7061(3) 0.5481(3) 0.1159(16) Uani 1 1 d . . .
O2 O 0.08463(18) 0.8089(2) 0.6374(3) 0.0947(13) Uani 1 1 d . . .
O3 O 0.0552(3) 0.6764(4) 0.6756(4) 0.173(3) Uani 1 1 d . . .
O4 O 0.14235(17) 0.6868(2) 0.6257(3) 0.0920(13) Uani 1 1 d . . .
O5 O 0.9874(9) 0.4656(7) 0.7001(7) 0.378(9) Uani 1 1 d D . .
N1 N 0.16708(14) -0.09110(18) -0.03748(18) 0.0362(7) Uani 1 1 d . . .
N2 N 0.13252(14) -0.03041(18) 0.08449(19) 0.0378(8) Uani 1 1 d . . .
N3 N 0.26595(14) 0.00890(18) 0.16916(17) 0.0340(7) Uani 1 1 d . . .
N4 N 0.23669(14) 0.09209(17) 0.03244(17) 0.0319(7) Uani 1 1 d . . .
N5 N 0.30458(14) -0.06161(18) 0.03430(17) 0.0340(7) Uani 1 1 d . . .
C1 C 0.18631(19) -0.1187(2) -0.0984(2) 0.0430(10) Uani 1 1 d . . .
H1 H 0.2278 -0.1116 -0.0986 0.052 Uiso 1 1 calc R . .
C2 C 0.1486(2) -0.1570(3) -0.1612(2) 0.0527(11) Uani 1 1 d . . .
H2 H 0.1642 -0.1751 -0.2027 0.063 Uiso 1 1 calc R . .
C3 C 0.0879(2) -0.1680(3) -0.1618(3) 0.0573(12) Uani 1 1 d . . .
H3 H 0.0612 -0.1938 -0.2037 0.069 Uiso 1 1 calc R . .
C4 C 0.0664(2) -0.1401(3) -0.0992(3) 0.0518(11) Uani 1 1 d . . .
H4 H 0.0250 -0.1467 -0.0985 0.062 Uiso 1 1 calc R . .
C5 C 0.10724(18) -0.1021(2) -0.0372(2) 0.0391(9) Uani 1 1 d . . .
C6 C 0.08876(17) -0.0726(2) 0.0325(2) 0.0384(9) Uani 1 1 d . . .
C7 C 0.0307(2) -0.0872(3) 0.0461(3) 0.0529(11) Uani 1 1 d . . .
H7 H 0.0013 -0.1181 0.0104 0.064 Uiso 1 1 calc R . .
C8 C 0.0165(2) -0.0564(3) 0.1115(3) 0.0571(12) Uani 1 1 d . . .
H8 H -0.0226 -0.0653 0.1206 0.069 Uiso 1 1 calc R . .
C9 C 0.0609(2) -0.0121(3) 0.1640(3) 0.0548(12) Uani 1 1 d . . .
H9 H 0.0522 0.0100 0.2089 0.066 Uiso 1 1 calc R . .
C10 C 0.1179(2) -0.0013(2) 0.1489(2) 0.0455(10) Uani 1 1 d . . .
H10 H 0.1481 0.0278 0.1850 0.055 Uiso 1 1 calc R . .
C11 C 0.29856(18) -0.0323(2) 0.2312(2) 0.0403(9) Uani 1 1 d . . .
H11 H 0.3041 -0.0924 0.2286 0.048 Uiso 1 1 calc R . .
C12 C 0.3243(2) 0.0100(3) 0.2988(2) 0.0471(10) Uani 1 1 d . . .
H12 H 0.3473 -0.0206 0.3406 0.056 Uiso 1 1 calc R . .
C13 C 0.3151(2) 0.0986(3) 0.3030(2) 0.0501(11) Uani 1 1 d . . .
H13 H 0.3307 0.1288 0.3486 0.060 Uiso 1 1 calc R . .
C14 C 0.2826(2) 0.1421(3) 0.2395(2) 0.0448(10) Uani 1 1 d . . .
H14 H 0.2761 0.2022 0.2415 0.054 Uiso 1 1 calc R . .
C15 C 0.25957(17) 0.0961(2) 0.1726(2) 0.0349(9) Uani 1 1 d . . .
C16 C 0.22506(18) 0.1389(2) 0.1006(2) 0.0372(9) Uani 1 1 d . . .
H16A H 0.1812 0.1384 0.0992 0.045 Uiso 1 1 calc R . .
H16B H 0.2381 0.1994 0.0997 0.045 Uiso 1 1 calc R . .
C17 C 0.33246(19) -0.1381(2) 0.0292(2) 0.0422(10) Uani 1 1 d . . .
H17 H 0.3123 -0.1895 0.0368 0.051 Uiso 1 1 calc R . .
C18 C 0.3893(2) -0.1435(3) 0.0131(3) 0.0521(11) Uani 1 1 d . . .
H18 H 0.4075 -0.1978 0.0098 0.063 Uiso 1 1 calc R . .
C19 C 0.4194(2) -0.0681(3) 0.0018(3) 0.0574(12) Uani 1 1 d . . .
H19 H 0.4583 -0.0704 -0.0093 0.069 Uiso 1 1 calc R . .
C20 C 0.39112(19) 0.0106(3) 0.0071(2) 0.0472(10) Uani 1 1 d . . .
H20 H 0.4107 0.0626 -0.0002 0.057 Uiso 1 1 calc R . .
C21 C 0.33393(17) 0.0120(2) 0.0232(2) 0.0318(8) Uani 1 1 d . . .
C22 C 0.30375(17) 0.0977(2) 0.0334(2) 0.0359(9) Uani 1 1 d . . .
H22A H 0.3251 0.1232 0.0820 0.043 Uiso 1 1 calc R . .
H22B H 0.3090 0.1372 -0.0072 0.043 Uiso 1 1 calc R . .
C23 C 0.19806(17) 0.1219(2) -0.0393(2) 0.0337(8) Uani 1 1 d . . .
C24 C 0.14467(18) 0.1699(2) -0.0426(2) 0.0423(10) Uani 1 1 d . . .
H24 H 0.1317 0.1817 0.0023 0.051 Uiso 1 1 calc R . .
C25 C 0.11058(19) 0.2004(3) -0.1120(2) 0.0469(10) Uani 1 1 d . . .
H25 H 0.0753 0.2333 -0.1125 0.056 Uiso 1 1 calc R . .
C26 C 0.12691(19) 0.1838(2) -0.1805(2) 0.0415(10) Uani 1 1 d . . .
C27 C 0.0900(2) 0.2203(3) -0.2555(3) 0.0592(12) Uani 1 1 d . . .
H27A H 0.0509 0.1908 -0.2695 0.089 Uiso 1 1 calc R . .
H27B H 0.1124 0.2115 -0.2951 0.089 Uiso 1 1 calc R . .
H27C H 0.0834 0.2818 -0.2498 0.089 Uiso 1 1 calc R . .
C28 C 0.1793(2) 0.1341(3) -0.1763(2) 0.0478(10) Uani 1 1 d . . .
H28 H 0.1916 0.1208 -0.2214 0.057 Uiso 1 1 calc R . .
C29 C 0.2140(2) 0.1035(2) -0.1076(2) 0.0447(10) Uani 1 1 d . . .
H29 H 0.2489 0.0697 -0.1073 0.054 Uiso 1 1 calc R . .
H5A H 1.008(2) 0.489(3) 0.664(3) 0.060(15) Uiso 1 1 d D . .
H5B H 0.9683(17) 0.5014(19) 0.718(2) 0.026(9) Uiso 1 1 d 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 N5 2.057(3) . ?
Ni1 N1 2.069(3) . ?
Ni1 N3 2.074(3) . ?
Ni1 N2 2.098(3) . ?
Ni1 N4 2.261(3) . ?
Ni1 Cl1 2.3761(10) . ?
Cl2 O3 1.357(4) . ?
Cl2 O4 1.414(4) . ?
Cl2 O2 1.416(3) . ?
Cl2 O1 1.421(4) . ?
O5 O5 1.74(3) 2_756 ?
N1 C1 1.325(5) . ?
N1 C5 1.341(5) . ?
N2 C10 1.340(5) . ?
N2 C6 1.346(5) . ?
N3 C11 1.335(5) . ?
N3 C15 1.342(4) . ?
N4 C23 1.443(4) . ?
N4 C16 1.484(4) . ?
N4 C22 1.489(5) . ?
N5 C17 1.335(5) . ?
N5 C21 1.338(4) . ?
C1 C2 1.369(6) . ?
C2 C3 1.356(6) . ?
C3 C4 1.378(6) . ?
C4 C5 1.387(5) . ?
C5 C6 1.467(6) . ?
C6 C7 1.384(5) . ?
C7 C8 1.360(6) . ?
C8 C9 1.373(6) . ?
C9 C10 1.365(6) . ?
C11 C12 1.372(5) . ?
C12 C13 1.374(6) . ?
C13 C14 1.370(6) . ?
C14 C15 1.381(5) . ?
C15 C16 1.489(5) . ?
C17 C18 1.359(6) . ?
C18 C19 1.370(6) . ?
C19 C20 1.370(6) . ?
C20 C21 1.365(5) . ?
C21 C22 1.500(5) . ?
C23 C29 1.373(5) . ?
C23 C24 1.385(5) . ?
C24 C25 1.376(6) . ?
C25 C26 1.377(6) . ?
C26 C28 1.378(6) . ?
C26 C27 1.508(6) . ?
C28 C29 1.373(5) . ?

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
N5 Ni1 N1 95.98(12) . . ?
N5 Ni1 N3 90.65(12) . . ?
N1 Ni1 N3 171.65(12) . . ?
N5 Ni1 N2 173.53(12) . . ?
N1 Ni1 N2 78.50(13) . . ?
N3 Ni1 N2 94.57(13) . . ?
N5 Ni1 N4 80.24(11) . . ?
N1 Ni1 N4 99.29(11) . . ?
N3 Ni1 N4 76.79(11) . . ?
N2 Ni1 N4 97.21(11) . . ?
N5 Ni1 Cl1 96.37(8) . . ?
N1 Ni1 Cl1 90.04(8) . . ?
N3 Ni1 Cl1 94.28(8) . . ?
N2 Ni1 Cl1 87.07(8) . . ?
N4 Ni1 Cl1 170.34(8) . . ?
O3 Cl2 O4 113.2(4) . . ?
O3 Cl2 O2 110.6(3) . . ?
O4 Cl2 O2 108.8(2) . . ?
O3 Cl2 O1 110.6(4) . . ?
O4 Cl2 O1 107.7(3) . . ?
O2 Cl2 O1 105.8(3) . . ?
C1 N1 C5 117.9(3) . . ?
C1 N1 Ni1 126.9(3) . . ?
C5 N1 Ni1 114.7(3) . . ?
C10 N2 C6 118.2(4) . . ?
C10 N2 Ni1 126.9(3) . . ?
C6 N2 Ni1 112.9(3) . . ?
C11 N3 C15 118.2(3) . . ?
C11 N3 Ni1 127.0(2) . . ?
C15 N3 Ni1 114.8(2) . . ?
C23 N4 C16 113.3(3) . . ?
C23 N4 C22 112.6(3) . . ?
C16 N4 C22 108.9(3) . . ?
C23 N4 Ni1 115.9(2) . . ?
C16 N4 Ni1 100.1(2) . . ?
C22 N4 Ni1 105.04(19) . . ?
C17 N5 C21 118.4(3) . . ?
C17 N5 Ni1 124.6(3) . . ?
C21 N5 Ni1 116.8(2) . . ?
N1 C1 C2 123.8(4) . . ?
C3 C2 C1 118.8(4) . . ?
C2 C3 C4 118.8(4) . . ?
C3 C4 C5 119.4(4) . . ?
N1 C5 C4 121.2(4) . . ?
N1 C5 C6 115.7(3) . . ?
C4 C5 C6 123.1(4) . . ?
N2 C6 C7 120.8(4) . . ?
N2 C6 C5 115.7(3) . . ?
C7 C6 C5 123.5(4) . . ?
C8 C7 C6 120.1(4) . . ?
C7 C8 C9 119.1(4) . . ?
C10 C9 C8 118.6(4) . . ?
N2 C10 C9 123.1(4) . . ?
N3 C11 C12 123.1(3) . . ?
C11 C12 C13 118.4(4) . . ?
C14 C13 C12 119.3(4) . . ?
C13 C14 C15 119.4(4) . . ?
N3 C15 C14 121.5(3) . . ?
N3 C15 C16 115.9(3) . . ?
C14 C15 C16 122.6(3) . . ?
N4 C16 C15 110.1(3) . . ?
N5 C17 C18 122.4(4) . . ?
C17 C18 C19 119.3(4) . . ?
C18 C19 C20 118.6(4) . . ?
C21 C20 C19 119.6(4) . . ?
N5 C21 C20 121.7(3) . . ?
N5 C21 C22 118.0(3) . . ?
C20 C21 C22 120.2(3) . . ?
N4 C22 C21 115.0(3) . . ?
C29 C23 C24 117.5(4) . . ?
C29 C23 N4 120.1(3) . . ?
C24 C23 N4 122.4(3) . . ?
C25 C24 C23 120.6(4) . . ?
C24 C25 C26 122.3(4) . . ?
C25 C26 C28 116.3(4) . . ?
C25 C26 C27 121.4(4) . . ?
C28 C26 C27 122.3(4) . . ?
C29 C28 C26 122.2(4) . . ?
C23 C29 C28 121.1(4) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.063
####################################################################### 
# 
# 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_bb
_database_code_depnum_ccdc_archive 'CCDC 910521'
_audit_update_record             
;
2012-11-12 deposited with the CCDC.
2015-03-18 downloaded from the CCDC.
;
#TrackingRef '3.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H27 Cl2 N5 Ni O7'
_chemical_formula_sum            'C31 H27 Cl2 N5 Ni O7'
_chemical_formula_weight         711.17

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/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                   7.6563(3)
_cell_length_b                   35.2380(17)
_cell_length_c                   12.7241(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.532(4)
_cell_angle_gamma                90.00
_cell_volume                     3214.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    4309
_cell_measurement_theta_min      2.4298
_cell_measurement_theta_max      28.9742

_exptl_crystal_description       Prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1464
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_T_max  0.9522
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      113(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  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12479
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         25.01
_reflns_number_total             5668
_reflns_number_gt                4312
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0532P)²+4.8603P] 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         5668
_refine_ls_number_parameters     416
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0592
_refine_ls_wR_factor_ref         0.1447
_refine_ls_wR_factor_gt          0.1319
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.004
_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 0.29012(7) 0.102720(14) 0.94536(4) 0.02887(17) Uani 1 1 d . . .
Cl1 Cl 0.56542(15) 0.06492(3) 1.01090(10) 0.0456(3) Uani 1 1 d . . .
Cl2 Cl 0.77069(18) 0.15891(4) 0.43359(11) 0.0579(4) Uani 1 1 d . . .
O1 O 0.7681(8) 0.14071(19) 0.3374(4) 0.134(2) Uani 1 1 d . . .
O2 O 0.7425(10) 0.1325(2) 0.5080(5) 0.157(3) Uani 1 1 d . . .
O3 O 0.9322(9) 0.1780(3) 0.4860(5) 0.201(4) Uani 1 1 d . . .
O4 O 0.6166(12) 0.1801(2) 0.4079(10) 0.247(5) Uani 1 1 d . . .
O5 O 0.826(2) 0.0410(5) 0.4347(15) 0.411(10) Uani 1 1 d . . .
O6 O 0.5512(13) 0.0015(2) 0.1911(9) 0.225(4) Uani 1 1 d . . .
N1 N 0.4486(4) 0.15280(9) 0.9814(3) 0.0308(8) Uani 1 1 d . . .
N2 N 0.3273(5) 0.11250(10) 0.7926(3) 0.0349(8) Uani 1 1 d . . .
N3 N 0.1060(5) 0.05767(10) 0.8821(3) 0.0373(8) Uani 1 1 d . . .
N4 N 0.0085(4) 0.13160(9) 0.8855(3) 0.0296(8) Uani 1 1 d . . .
N5 N 0.2367(4) 0.10416(9) 1.0936(3) 0.0314(8) Uani 1 1 d . . .
C1 C 0.5234(6) 0.17076(12) 1.0786(4) 0.0381(10) Uani 1 1 d . . .
H1 H 0.5109 0.1599 1.1440 0.046 Uiso 1 1 calc R . .
C2 C 0.6205(6) 0.20520(14) 1.0885(4) 0.0490(12) Uani 1 1 d . . .
H2 H 0.6753 0.2169 1.1598 0.059 Uiso 1 1 calc R . .
C3 C 0.6355(6) 0.22154(14) 0.9958(5) 0.0517(13) Uani 1 1 d . . .
H3 H 0.6966 0.2453 1.0013 0.062 Uiso 1 1 calc R . .
C4 C 0.5751(7) 0.21740(15) 0.7900(5) 0.0563(14) Uani 1 1 d . . .
H4 H 0.6284 0.2417 0.7895 0.068 Uiso 1 1 calc R . .
C5 C 0.5150(7) 0.19689(16) 0.6947(5) 0.0586(14) Uani 1 1 d . . .
H5 H 0.5281 0.2069 0.6286 0.070 Uiso 1 1 calc R . .
C6 C 0.3804(7) 0.13653(16) 0.5970(4) 0.0560(14) Uani 1 1 d . . .
H6 H 0.3947 0.1446 0.5292 0.067 Uiso 1 1 calc R . .
C7 C 0.3097(8) 0.10178(17) 0.6041(4) 0.0590(14) Uani 1 1 d . . .
H7 H 0.2785 0.0850 0.5419 0.071 Uiso 1 1 calc R . .
C8 C 0.2825(7) 0.09058(14) 0.7025(4) 0.0487(12) Uani 1 1 d . . .
H8 H 0.2299 0.0663 0.7049 0.058 Uiso 1 1 calc R . .
C9 C 0.5604(6) 0.20329(12) 0.8916(4) 0.0406(11) Uani 1 1 d . . .
C10 C 0.4702(5) 0.16842(12) 0.8895(3) 0.0316(9) Uani 1 1 d . . .
C11 C 0.4060(5) 0.14653(12) 0.7884(3) 0.0334(10) Uani 1 1 d . . .
C12 C 0.4322(6) 0.16047(14) 0.6909(4) 0.0431(11) Uani 1 1 d . . .
C13 C 0.1532(8) 0.28850(14) 0.8120(6) 0.0723(17) Uani 1 1 d . . .
H13A H 0.2884 0.2906 0.8307 0.108 Uiso 1 1 calc R . .
H13B H 0.1136 0.3055 0.8604 0.108 Uiso 1 1 calc R . .
H13C H 0.0895 0.2956 0.7333 0.108 Uiso 1 1 calc R . .
C14 C 0.1036(6) 0.24784(13) 0.8298(4) 0.0458(12) Uani 1 1 d . . .
C15 C 0.0482(6) 0.22241(13) 0.7422(4) 0.0451(12) Uani 1 1 d . . .
H15 H 0.0363 0.2309 0.6691 0.054 Uiso 1 1 calc R . .
C16 C 0.0092(6) 0.18475(12) 0.7575(4) 0.0375(10) Uani 1 1 d . . .
H16 H -0.0305 0.1680 0.6950 0.045 Uiso 1 1 calc R . .
C17 C 0.0281(5) 0.17155(11) 0.8633(3) 0.0317(9) Uani 1 1 d . . .
C18 C 0.0811(6) 0.19695(12) 0.9516(4) 0.0378(10) Uani 1 1 d . . .
H18 H 0.0928 0.1886 1.0247 0.045 Uiso 1 1 calc R . .
C19 C 0.1172(6) 0.23456(13) 0.9345(4) 0.0452(12) Uani 1 1 d . . .
H19 H 0.1521 0.2516 0.9963 0.054 Uiso 1 1 calc R . .
C20 C -0.0731(5) 0.12491(13) 0.9738(3) 0.0367(10) Uani 1 1 d . . .
H20A H -0.1623 0.1035 0.9500 0.044 Uiso 1 1 calc R . .
H20B H -0.1444 0.1477 0.9797 0.044 Uiso 1 1 calc R . .
C21 C 0.0669(6) 0.11610(11) 1.0880(3) 0.0310(9) Uani 1 1 d . . .
C22 C 0.0165(7) 0.11873(13) 1.1818(4) 0.0427(11) Uani 1 1 d . . .
H22 H -0.1050 0.1270 1.1753 0.051 Uiso 1 1 calc R . .
C23 C 0.1443(7) 0.10929(14) 1.2845(4) 0.0500(13) Uani 1 1 d . . .
H23 H 0.1125 0.1111 1.3501 0.060 Uiso 1 1 calc R . .
C24 C 0.3186(7) 0.09728(14) 1.2918(4) 0.0470(12) Uani 1 1 d . . .
H24 H 0.4090 0.0907 1.3623 0.056 Uiso 1 1 calc R . .
C25 C 0.3602(6) 0.09494(12) 1.1951(4) 0.0397(11) Uani 1 1 d . . .
H25 H 0.4808 0.0865 1.2002 0.048 Uiso 1 1 calc R . .
C26 C -0.0956(6) 0.10891(12) 0.7851(4) 0.0426(11) Uani 1 1 d . . .
H26A H -0.0530 0.1156 0.7224 0.051 Uiso 1 1 calc R . .
H26B H -0.2304 0.1147 0.7617 0.051 Uiso 1 1 calc R . .
C27 C -0.0643(6) 0.06730(12) 0.8109(4) 0.0414(11) Uani 1 1 d . . .
C28 C -0.1969(8) 0.04047(15) 0.7614(5) 0.0737(18) Uani 1 1 d . . .
H28 H -0.3165 0.0477 0.7112 0.088 Uiso 1 1 calc R . .
C29 C -0.1545(9) 0.00292(17) 0.7854(6) 0.094(2) Uani 1 1 d . . .
H29 H -0.2449 -0.0160 0.7514 0.113 Uiso 1 1 calc R . .
C30 C 0.0174(8) -0.00726(15) 0.8581(5) 0.0734(18) Uani 1 1 d . . .
H30 H 0.0488 -0.0332 0.8753 0.088 Uiso 1 1 calc R . .
C31 C 0.1428(7) 0.02091(13) 0.9055(4) 0.0499(12) Uani 1 1 d . . .
H31 H 0.2617 0.0141 0.9575 0.060 Uiso 1 1 calc R . .
O7 O 0.646(3) 0.9968(6) 0.4409(18) 0.71(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 N5 2.066(3) . ?
Ni1 N3 2.088(3) . ?
Ni1 N2 2.090(3) . ?
Ni1 N1 2.099(3) . ?
Ni1 N4 2.261(3) . ?
Ni1 Cl1 2.3831(11) . ?
Cl2 O4 1.335(7) . ?
Cl2 O3 1.359(5) . ?
Cl2 O1 1.376(5) . ?
Cl2 O2 1.398(6) . ?
N1 C1 1.327(5) . ?
N1 C10 1.354(5) . ?
N2 C8 1.324(5) . ?
N2 C11 1.351(5) . ?
N3 C31 1.337(5) . ?
N3 C27 1.344(5) . ?
N4 C17 1.454(5) . ?
N4 C26 1.481(5) . ?
N4 C20 1.482(5) . ?
N5 C21 1.344(5) . ?
N5 C25 1.345(5) . ?
C1 C2 1.405(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.353(7) . ?
C2 H2 0.9500 . ?
C3 C9 1.402(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.346(7) . ?
C4 C9 1.427(7) . ?
C4 H4 0.9500 . ?
C5 C12 1.425(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.355(7) . ?
C6 C12 1.402(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.396(7) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.406(6) . ?
C10 C11 1.431(6) . ?
C11 C12 1.412(6) . ?
C13 C14 1.519(6) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.376(7) . ?
C14 C19 1.381(6) . ?
C15 C16 1.388(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.383(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.381(6) . ?
C18 C19 1.386(6) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.505(6) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.381(6) . ?
C22 C23 1.371(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.371(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.377(6) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.504(6) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.368(6) . ?
C28 C29 1.371(8) . ?
C28 H28 0.9500 . ?
C29 C30 1.365(8) . ?
C29 H29 0.9500 . ?
C30 C31 1.366(7) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?

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
N5 Ni1 N3 92.74(14) . . ?
N5 Ni1 N2 168.63(14) . . ?
N3 Ni1 N2 93.47(14) . . ?
N5 Ni1 N1 93.67(13) . . ?
N3 Ni1 N1 169.67(13) . . ?
N2 Ni1 N1 78.92(13) . . ?
N5 Ni1 N4 79.96(12) . . ?
N3 Ni1 N4 77.12(12) . . ?
N2 Ni1 N4 92.16(12) . . ?
N1 Ni1 N4 96.03(12) . . ?
N5 Ni1 Cl1 97.36(10) . . ?
N3 Ni1 Cl1 96.01(10) . . ?
N2 Ni1 Cl1 91.45(10) . . ?
N1 Ni1 Cl1 91.20(9) . . ?
N4 Ni1 Cl1 172.42(9) . . ?
O4 Cl2 O3 114.7(6) . . ?
O4 Cl2 O1 107.8(5) . . ?
O3 Cl2 O1 113.2(4) . . ?
O4 Cl2 O2 101.8(6) . . ?
O3 Cl2 O2 109.1(4) . . ?
O1 Cl2 O2 109.6(4) . . ?
C1 N1 C10 117.9(4) . . ?
C1 N1 Ni1 129.2(3) . . ?
C10 N1 Ni1 112.9(3) . . ?
C8 N2 C11 117.9(4) . . ?
C8 N2 Ni1 129.1(3) . . ?
C11 N2 Ni1 113.0(3) . . ?
C31 N3 C27 118.3(4) . . ?
C31 N3 Ni1 126.1(3) . . ?
C27 N3 Ni1 115.6(3) . . ?
C17 N4 C26 114.6(3) . . ?
C17 N4 C20 113.6(3) . . ?
C26 N4 C20 109.0(3) . . ?
C17 N4 Ni1 110.5(2) . . ?
C26 N4 Ni1 102.0(2) . . ?
C20 N4 Ni1 106.2(2) . . ?
C21 N5 C25 117.9(4) . . ?
C21 N5 Ni1 117.1(3) . . ?
C25 N5 Ni1 125.0(3) . . ?
N1 C1 C2 122.4(4) . . ?
N1 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
C3 C2 C1 119.6(5) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C2 C3 C9 119.8(4) . . ?
C2 C3 H3 120.1 . . ?
C9 C3 H3 120.1 . . ?
C5 C4 C9 121.2(5) . . ?
C5 C4 H4 119.4 . . ?
C9 C4 H4 119.4 . . ?
C4 C5 C12 121.5(5) . . ?
C4 C5 H5 119.3 . . ?
C12 C5 H5 119.3 . . ?
C7 C6 C12 119.1(4) . . ?
C7 C6 H6 120.4 . . ?
C12 C6 H6 120.4 . . ?
C6 C7 C8 120.3(5) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
N2 C8 C7 122.4(5) . . ?
N2 C8 H8 118.8 . . ?
C7 C8 H8 118.8 . . ?
C3 C9 C10 117.0(4) . . ?
C3 C9 C4 124.1(5) . . ?
C10 C9 C4 118.8(4) . . ?
N1 C10 C9 123.2(4) . . ?
N1 C10 C11 116.8(4) . . ?
C9 C10 C11 120.0(4) . . ?
N2 C11 C12 123.1(4) . . ?
N2 C11 C10 117.4(4) . . ?
C12 C11 C10 119.5(4) . . ?
C6 C12 C11 117.1(5) . . ?
C6 C12 C5 124.1(4) . . ?
C11 C12 C5 118.8(5) . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C19 117.3(4) . . ?
C15 C14 C13 121.1(5) . . ?
C19 C14 C13 121.7(5) . . ?
C14 C15 C16 122.0(4) . . ?
C14 C15 H15 119.0 . . ?
C16 C15 H15 119.0 . . ?
C17 C16 C15 120.2(4) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C18 C17 C16 118.3(4) . . ?
C18 C17 N4 119.3(4) . . ?
C16 C17 N4 122.2(4) . . ?
C17 C18 C19 120.6(4) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C14 C19 C18 121.6(4) . . ?
C14 C19 H19 119.2 . . ?
C18 C19 H19 119.2 . . ?
N4 C20 C21 114.7(3) . . ?
N4 C20 H20A 108.6 . . ?
C21 C20 H20A 108.6 . . ?
N4 C20 H20B 108.6 . . ?
C21 C20 H20B 108.6 . . ?
H20A C20 H20B 107.6 . . ?
N5 C21 C22 122.2(4) . . ?
N5 C21 C20 117.7(4) . . ?
C22 C21 C20 120.1(4) . . ?
C23 C22 C21 119.0(4) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
C22 C23 C24 119.4(4) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 H23 120.3 . . ?
C23 C24 C25 118.8(4) . . ?
C23 C24 H24 120.6 . . ?
C25 C24 H24 120.6 . . ?
N5 C25 C24 122.6(4) . . ?
N5 C25 H25 118.7 . . ?
C24 C25 H25 118.7 . . ?
N4 C26 C27 110.0(3) . . ?
N4 C26 H26A 109.7 . . ?
C27 C26 H26A 109.7 . . ?
N4 C26 H26B 109.7 . . ?
C27 C26 H26B 109.7 . . ?
H26A C26 H26B 108.2 . . ?
N3 C27 C28 121.6(4) . . ?
N3 C27 C26 115.8(4) . . ?
C28 C27 C26 122.5(4) . . ?
C27 C28 C29 119.0(5) . . ?
C27 C28 H28 120.5 . . ?
C29 C28 H28 120.5 . . ?
C30 C29 C28 120.1(5) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C29 C30 C31 118.0(5) . . ?
C29 C30 H30 121.0 . . ?
C31 C30 H30 121.0 . . ?
N3 C31 C30 123.0(5) . . ?
N3 C31 H31 118.5 . . ?
C30 C31 H31 118.5 . . ?

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
N5 Ni1 N1 C1 15.8(3) . . . . ?
N3 Ni1 N1 C1 144.0(7) . . . . ?
N2 Ni1 N1 C1 -172.9(4) . . . . ?
N4 Ni1 N1 C1 96.1(3) . . . . ?
Cl1 Ni1 N1 C1 -81.6(3) . . . . ?
N5 Ni1 N1 C10 -162.5(3) . . . . ?
N3 Ni1 N1 C10 -34.4(9) . . . . ?
N2 Ni1 N1 C10 8.8(3) . . . . ?
N4 Ni1 N1 C10 -82.2(3) . . . . ?
Cl1 Ni1 N1 C10 100.0(2) . . . . ?
N5 Ni1 N2 C8 -137.2(6) . . . . ?
N3 Ni1 N2 C8 -14.3(4) . . . . ?
N1 Ni1 N2 C8 172.8(4) . . . . ?
N4 Ni1 N2 C8 -91.5(4) . . . . ?
Cl1 Ni1 N2 C8 81.8(4) . . . . ?
N5 Ni1 N2 C11 41.7(8) . . . . ?
N3 Ni1 N2 C11 164.6(3) . . . . ?
N1 Ni1 N2 C11 -8.3(3) . . . . ?
N4 Ni1 N2 C11 87.4(3) . . . . ?
Cl1 Ni1 N2 C11 -99.3(3) . . . . ?
N5 Ni1 N3 C31 -81.9(4) . . . . ?
N2 Ni1 N3 C31 107.7(4) . . . . ?
N1 Ni1 N3 C31 149.9(7) . . . . ?
N4 Ni1 N3 C31 -160.9(4) . . . . ?
Cl1 Ni1 N3 C31 15.8(4) . . . . ?
N5 Ni1 N3 C27 98.4(3) . . . . ?
N2 Ni1 N3 C27 -72.0(3) . . . . ?
N1 Ni1 N3 C27 -29.8(9) . . . . ?
N4 Ni1 N3 C27 19.4(3) . . . . ?
Cl1 Ni1 N3 C27 -163.9(3) . . . . ?
N5 Ni1 N4 C17 107.8(3) . . . . ?
N3 Ni1 N4 C17 -157.0(3) . . . . ?
N2 Ni1 N4 C17 -64.0(3) . . . . ?
N1 Ni1 N4 C17 15.1(3) . . . . ?
Cl1 Ni1 N4 C17 177.7(5) . . . . ?
N5 Ni1 N4 C26 -130.0(3) . . . . ?
N3 Ni1 N4 C26 -34.8(3) . . . . ?
N2 Ni1 N4 C26 58.3(3) . . . . ?
N1 Ni1 N4 C26 137.3(3) . . . . ?
Cl1 Ni1 N4 C26 -60.1(8) . . . . ?
N5 Ni1 N4 C20 -15.8(2) . . . . ?
N3 Ni1 N4 C20 79.3(3) . . . . ?
N2 Ni1 N4 C20 172.4(3) . . . . ?
N1 Ni1 N4 C20 -108.5(3) . . . . ?
Cl1 Ni1 N4 C20 54.0(8) . . . . ?
N3 Ni1 N5 C21 -69.3(3) . . . . ?
N2 Ni1 N5 C21 53.7(8) . . . . ?
N1 Ni1 N5 C21 102.6(3) . . . . ?
N4 Ni1 N5 C21 7.1(3) . . . . ?
Cl1 Ni1 N5 C21 -165.7(3) . . . . ?
N3 Ni1 N5 C25 112.4(3) . . . . ?
N2 Ni1 N5 C25 -124.6(6) . . . . ?
N1 Ni1 N5 C25 -75.8(3) . . . . ?
N4 Ni1 N5 C25 -171.2(4) . . . . ?
Cl1 Ni1 N5 C25 15.9(3) . . . . ?
C10 N1 C1 C2 0.9(6) . . . . ?
Ni1 N1 C1 C2 -177.4(3) . . . . ?
N1 C1 C2 C3 1.7(7) . . . . ?
C1 C2 C3 C9 -2.5(7) . . . . ?
C9 C4 C5 C12 0.8(8) . . . . ?
C12 C6 C7 C8 2.3(8) . . . . ?
C11 N2 C8 C7 -1.5(7) . . . . ?
Ni1 N2 C8 C7 177.4(4) . . . . ?
C6 C7 C8 N2 -1.5(8) . . . . ?
C2 C3 C9 C10 0.7(6) . . . . ?
C2 C3 C9 C4 -177.5(4) . . . . ?
C5 C4 C9 C3 173.9(5) . . . . ?
C5 C4 C9 C10 -4.2(7) . . . . ?
C1 N1 C10 C9 -2.8(6) . . . . ?
Ni1 N1 C10 C9 175.7(3) . . . . ?
C1 N1 C10 C11 173.4(3) . . . . ?
Ni1 N1 C10 C11 -8.0(4) . . . . ?
C3 C9 C10 N1 2.1(6) . . . . ?
C4 C9 C10 N1 -179.7(4) . . . . ?
C3 C9 C10 C11 -174.1(4) . . . . ?
C4 C9 C10 C11 4.2(6) . . . . ?
C8 N2 C11 C12 3.8(6) . . . . ?
Ni1 N2 C11 C12 -175.3(3) . . . . ?
C8 N2 C11 C10 -174.2(4) . . . . ?
Ni1 N2 C11 C10 6.8(4) . . . . ?
N1 C10 C11 N2 0.9(5) . . . . ?
C9 C10 C11 N2 177.3(4) . . . . ?
N1 C10 C11 C12 -177.2(3) . . . . ?
C9 C10 C11 C12 -0.8(6) . . . . ?
C7 C6 C12 C11 -0.2(7) . . . . ?
C7 C6 C12 C5 177.3(5) . . . . ?
N2 C11 C12 C6 -2.9(6) . . . . ?
C10 C11 C12 C6 175.0(4) . . . . ?
N2 C11 C12 C5 179.4(4) . . . . ?
C10 C11 C12 C5 -2.6(6) . . . . ?
C4 C5 C12 C6 -174.8(5) . . . . ?
C4 C5 C12 C11 2.7(7) . . . . ?
C19 C14 C15 C16 -0.7(7) . . . . ?
C13 C14 C15 C16 177.5(4) . . . . ?
C14 C15 C16 C17 -1.0(7) . . . . ?
C15 C16 C17 C18 1.8(6) . . . . ?
C15 C16 C17 N4 -173.3(4) . . . . ?
C26 N4 C17 C18 164.4(4) . . . . ?
C20 N4 C17 C18 38.1(5) . . . . ?
Ni1 N4 C17 C18 -81.1(4) . . . . ?
C26 N4 C17 C16 -20.6(5) . . . . ?
C20 N4 C17 C16 -146.8(4) . . . . ?
Ni1 N4 C17 C16 94.0(4) . . . . ?
C16 C17 C18 C19 -1.0(6) . . . . ?
N4 C17 C18 C19 174.2(4) . . . . ?
C15 C14 C19 C18 1.5(7) . . . . ?
C13 C14 C19 C18 -176.6(4) . . . . ?
C17 C18 C19 C14 -0.7(7) . . . . ?
C17 N4 C20 C21 -99.2(4) . . . . ?
C26 N4 C20 C21 131.7(4) . . . . ?
Ni1 N4 C20 C21 22.4(4) . . . . ?
C25 N5 C21 C22 -0.6(6) . . . . ?
Ni1 N5 C21 C22 -179.1(3) . . . . ?
C25 N5 C21 C20 -177.7(4) . . . . ?
Ni1 N5 C21 C20 3.9(5) . . . . ?
N4 C20 C21 N5 -19.2(5) . . . . ?
N4 C20 C21 C22 163.7(4) . . . . ?
N5 C21 C22 C23 0.8(7) . . . . ?
C20 C21 C22 C23 177.7(4) . . . . ?
C21 C22 C23 C24 -0.4(7) . . . . ?
C22 C23 C24 C25 -0.2(7) . . . . ?
C21 N5 C25 C24 0.1(6) . . . . ?
Ni1 N5 C25 C24 178.4(3) . . . . ?
C23 C24 C25 N5 0.3(7) . . . . ?
C17 N4 C26 C27 164.9(4) . . . . ?
C20 N4 C26 C27 -66.5(4) . . . . ?
Ni1 N4 C26 C27 45.6(4) . . . . ?
C31 N3 C27 C28 -1.2(7) . . . . ?
Ni1 N3 C27 C28 178.5(4) . . . . ?
C31 N3 C27 C26 -178.2(4) . . . . ?
Ni1 N3 C27 C26 1.5(5) . . . . ?
N4 C26 C27 N3 -34.7(6) . . . . ?
N4 C26 C27 C28 148.3(5) . . . . ?
N3 C27 C28 C29 0.2(9) . . . . ?
C26 C27 C28 C29 176.9(6) . . . . ?
C27 C28 C29 C30 0.3(11) . . . . ?
C28 C29 C30 C31 0.3(11) . . . . ?
C27 N3 C31 C30 1.9(8) . . . . ?
Ni1 N3 C31 C30 -177.8(4) . . . . ?
C29 C30 C31 N3 -1.4(10) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.071
####################################################################### 
# 
# 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_aa4
_database_code_depnum_ccdc_archive 'CCDC 910522'
_audit_update_record             
;
2012-11-12 deposited with the CCDC.
2015-03-18 downloaded from the CCDC.
;
#TrackingRef '4.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H31 Cl2 N7 Ni O5'
_chemical_formula_sum            'C34 H31 Cl2 N7 Ni O5'
_chemical_formula_weight         747.25

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   7.5420(15)
_cell_length_b                   11.202(2)
_cell_length_c                   19.311(4)
_cell_angle_alpha                97.04(3)
_cell_angle_beta                 90.51(3)
_cell_angle_gamma                90.79(3)
_cell_volume                     1619.0(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            Blue
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             772
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9248
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0944
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.19
_diffrn_reflns_theta_max         25.01
_reflns_number_total             5689
_reflns_number_gt                3689
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0778P)²+0.3193P] 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         5689
_refine_ls_number_parameters     445
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0710
_refine_ls_wR_factor_ref         0.1738
_refine_ls_wR_factor_gt          0.1533
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          1.343
_refine_ls_shift/su_mean         0.031

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 0.28534(8) 0.34302(6) 0.31904(3) 0.0347(2) Uani 1 1 d . . .
Cl1 Cl 0.52780(19) 0.34103(17) 0.39766(8) 0.0638(5) Uani 1 1 d . . .
Cl2 Cl 0.0248(3) 0.80559(14) 0.22108(8) 0.0619(5) Uani 1 1 d . . .
O1 O 0.0401(10) 0.7016(4) 0.1718(3) 0.117(2) Uani 1 1 d . . .
O2 O 0.0557(11) 0.9056(5) 0.1887(3) 0.134(3) Uani 1 1 d . . .
O3 O 0.1490(11) 0.8029(7) 0.2764(3) 0.158(3) Uani 1 1 d . . .
O4 O -0.1362(9) 0.8051(7) 0.2516(4) 0.166(3) Uani 1 1 d . . .
O5 O 0.490(3) 0.192(2) 0.5880(14) 0.498(19) Uani 1 1 d . . .
H5 H 0.3959 0.1575 0.5946 0.748 Uiso 1 1 calc R . .
N1 N 0.4184(5) 0.4501(4) 0.2550(2) 0.0376(10) Uani 1 1 d . . .
N2 N 0.4014(5) 0.2134(4) 0.2459(2) 0.0352(10) Uani 1 1 d . . .
N5 N 0.1362(6) 0.2127(4) 0.3603(2) 0.0403(11) Uani 1 1 d . . .
N6 N 0.0286(5) 0.3539(4) 0.2593(2) 0.0340(10) Uani 1 1 d . . .
N7 N 0.1614(5) 0.4860(4) 0.3774(2) 0.0376(11) Uani 1 1 d . . .
C1 C 0.4344(8) 0.5690(6) 0.2622(3) 0.0543(16) Uani 1 1 d . . .
H1 H 0.3859 0.6126 0.3014 0.065 Uiso 1 1 calc R . .
C2 C 0.5202(8) 0.6315(5) 0.2142(3) 0.0598(17) Uani 1 1 d . . .
H2 H 0.5333 0.7147 0.2227 0.072 Uiso 1 1 calc R . .
C3 C 0.5845(8) 0.5708(5) 0.1550(3) 0.0519(15) Uani 1 1 d . . .
H3 H 0.6389 0.6122 0.1219 0.062 Uiso 1 1 calc R . .
N3 N 0.6912(7) 0.4277(4) 0.0295(2) 0.0535(13) Uani 1 1 d . . .
C4 C 0.7363(8) 0.3563(7) -0.0267(3) 0.0600(18) Uani 1 1 d . . .
H4 H 0.7791 0.3913 -0.0646 0.072 Uiso 1 1 calc R . .
C5 C 0.7236(8) 0.2327(6) -0.0326(3) 0.0564(17) Uani 1 1 d . . .
H5A H 0.7593 0.1877 -0.0736 0.068 Uiso 1 1 calc R . .
N4 N 0.6625(6) 0.1768(4) 0.0182(2) 0.0514(13) Uani 1 1 d . . .
C6 C 0.5386(8) 0.0640(5) 0.1337(3) 0.0569(17) Uani 1 1 d . . .
H6 H 0.5826 0.0135 0.0962 0.068 Uiso 1 1 calc R . .
C7 C 0.4689(9) 0.0180(6) 0.1894(3) 0.0610(18) Uani 1 1 d . . .
H7 H 0.4680 -0.0646 0.1910 0.073 Uiso 1 1 calc R . .
C8 C 0.3992(8) 0.0938(5) 0.2438(3) 0.0493(15) Uani 1 1 d . . .
H8 H 0.3483 0.0600 0.2808 0.059 Uiso 1 1 calc R . .
C14 C 0.4766(6) 0.2596(5) 0.1916(3) 0.0325(12) Uani 1 1 d . . .
C9 C 0.4867(6) 0.3891(5) 0.1969(2) 0.0340(12) Uani 1 1 d . . .
C10 C 0.5685(6) 0.4455(5) 0.1442(3) 0.0366(13) Uani 1 1 d . . .
C11 C 0.6269(7) 0.3733(5) 0.0821(3) 0.0384(13) Uani 1 1 d . . .
C12 C 0.6151(7) 0.2474(5) 0.0764(3) 0.0439(14) Uani 1 1 d . . .
C13 C 0.5433(7) 0.1888(5) 0.1337(3) 0.0385(13) Uani 1 1 d . . .
C15 C 0.2006(9) 0.1344(6) 0.4018(3) 0.0552(17) Uani 1 1 d . . .
H15 H 0.3158 0.1465 0.4191 0.066 Uiso 1 1 calc R . .
C16 C 0.1056(11) 0.0389(6) 0.4196(3) 0.069(2) Uani 1 1 d . . .
H16 H 0.1539 -0.0115 0.4494 0.083 Uiso 1 1 calc R . .
C17 C -0.0619(12) 0.0183(7) 0.3929(4) 0.082(2) Uani 1 1 d . . .
H17 H -0.1280 -0.0480 0.4030 0.098 Uiso 1 1 calc R . .
C18 C -0.1306(9) 0.0970(6) 0.3511(3) 0.0636(18) Uani 1 1 d . . .
H18 H -0.2450 0.0852 0.3329 0.076 Uiso 1 1 calc R . .
C19 C -0.0294(7) 0.1938(5) 0.3362(3) 0.0412(13) Uani 1 1 d . . .
C20 C -0.1050(7) 0.2837(5) 0.2940(3) 0.0452(14) Uani 1 1 d . . .
H20A H -0.1832 0.2421 0.2585 0.054 Uiso 1 1 calc R . .
H20B H -0.1763 0.3392 0.3242 0.054 Uiso 1 1 calc R . .
C21 C -0.0129(8) 0.4836(5) 0.2727(3) 0.0443(14) Uani 1 1 d . . .
H21A H -0.1361 0.4954 0.2608 0.053 Uiso 1 1 calc R . .
H21B H 0.0603 0.5282 0.2434 0.053 Uiso 1 1 calc R . .
C22 C 0.0199(7) 0.5303(5) 0.3475(3) 0.0395(13) Uani 1 1 d . . .
C23 C -0.0828(9) 0.6188(6) 0.3817(3) 0.0592(18) Uani 1 1 d . . .
H23 H -0.1833 0.6453 0.3603 0.071 Uiso 1 1 calc R . .
C24 C -0.0342(10) 0.6676(6) 0.4486(3) 0.0677(19) Uani 1 1 d . . .
H24 H -0.1004 0.7283 0.4727 0.081 Uiso 1 1 calc R . .
C25 C 0.1128(9) 0.6247(6) 0.4784(3) 0.0615(18) Uani 1 1 d . . .
H25 H 0.1495 0.6567 0.5231 0.074 Uiso 1 1 calc R . .
C26 C 0.2050(8) 0.5345(5) 0.4420(3) 0.0491(15) Uani 1 1 d . . .
H26 H 0.3037 0.5052 0.4632 0.059 Uiso 1 1 calc R . .
C27 C 0.0495(6) 0.3090(5) 0.1866(3) 0.0356(12) Uani 1 1 d . . .
C28 C 0.0458(7) 0.1865(5) 0.1658(3) 0.0432(14) Uani 1 1 d . . .
H28 H 0.0157 0.1343 0.1979 0.052 Uiso 1 1 calc R . .
C29 C 0.0856(7) 0.1405(5) 0.0990(3) 0.0485(15) Uani 1 1 d . . .
H29 H 0.0811 0.0576 0.0868 0.058 Uiso 1 1 calc R . .
C30 C 0.1323(7) 0.2134(6) 0.0490(3) 0.0456(14) Uani 1 1 d . . .
C31 C 0.1833(9) 0.1632(6) -0.0232(3) 0.0654(19) Uani 1 1 d . . .
H31A H 0.1967 0.0777 -0.0255 0.098 Uiso 1 1 calc R . .
H31B H 0.2935 0.1993 -0.0350 0.098 Uiso 1 1 calc R . .
H31C H 0.0926 0.1804 -0.0556 0.098 Uiso 1 1 calc R . .
C32 C 0.1281(7) 0.3359(5) 0.0691(3) 0.0457(14) Uani 1 1 d . . .
H32 H 0.1533 0.3878 0.0363 0.055 Uiso 1 1 calc R . .
C33 C 0.0874(7) 0.3846(5) 0.1367(3) 0.0403(13) Uani 1 1 d . . .
H33 H 0.0857 0.4676 0.1485 0.048 Uiso 1 1 calc R . .
C34 C 0.548(2) 0.1510(12) 0.5382(11) 0.258(12) Uani 1 1 d . . .
H34A H 0.6745 0.1634 0.5400 0.387 Uiso 1 1 calc R . .
H34B H 0.4994 0.1878 0.5001 0.387 Uiso 1 1 calc R . .
H34C H 0.5217 0.0663 0.5316 0.387 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 N5 2.071(5) . ?
Ni1 N1 2.081(4) . ?
Ni1 N7 2.080(4) . ?
Ni1 N2 2.103(4) . ?
Ni1 N6 2.257(4) . ?
Ni1 Cl1 2.3685(16) . ?
Cl2 O4 1.354(6) . ?
Cl2 O2 1.367(5) . ?
Cl2 O1 1.418(5) . ?
Cl2 O3 1.418(7) . ?
O5 C34 1.11(3) . ?
O5 H5 0.8389 . ?
N1 C1 1.326(7) . ?
N1 C9 1.350(6) . ?
N2 C8 1.336(6) . ?
N2 C14 1.350(6) . ?
N5 C19 1.334(7) . ?
N5 C15 1.350(7) . ?
N6 C27 1.443(6) . ?
N6 C21 1.483(6) . ?
N6 C20 1.483(6) . ?
N7 C26 1.335(6) . ?
N7 C22 1.338(6) . ?
C1 C2 1.388(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.354(8) . ?
C2 H2 0.9300 . ?
C3 C10 1.397(7) . ?
C3 H3 0.9300 . ?
N3 C4 1.317(7) . ?
N3 C11 1.338(6) . ?
C4 C5 1.377(8) . ?
C4 H4 0.9300 . ?
C5 N4 1.311(7) . ?
C5 H5A 0.9300 . ?
N4 C12 1.346(7) . ?
C6 C7 1.355(8) . ?
C6 C13 1.398(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.380(8) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C14 C13 1.391(7) . ?
C14 C9 1.443(7) . ?
C9 C10 1.404(7) . ?
C10 C11 1.438(7) . ?
C11 C12 1.403(8) . ?
C12 C13 1.458(7) . ?
C15 C16 1.360(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.366(10) . ?
C16 H16 0.9300 . ?
C17 C18 1.370(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.378(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.487(7) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.493(7) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.374(7) . ?
C23 C24 1.383(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.365(9) . ?
C24 H24 0.9300 . ?
C25 C26 1.362(8) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C28 1.382(7) . ?
C27 C33 1.387(7) . ?
C28 C29 1.367(7) . ?
C28 H28 0.9300 . ?
C29 C30 1.384(8) . ?
C29 H29 0.9300 . ?
C30 C32 1.381(8) . ?
C30 C31 1.494(7) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C33 1.390(7) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 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
N5 Ni1 N1 166.27(16) . . ?
N5 Ni1 N7 94.28(17) . . ?
N1 Ni1 N7 94.76(17) . . ?
N5 Ni1 N2 91.67(17) . . ?
N1 Ni1 N2 78.13(17) . . ?
N7 Ni1 N2 170.57(15) . . ?
N5 Ni1 N6 79.79(16) . . ?
N1 Ni1 N6 92.00(15) . . ?
N7 Ni1 N6 78.08(16) . . ?
N2 Ni1 N6 95.82(15) . . ?
N5 Ni1 Cl1 95.86(13) . . ?
N1 Ni1 Cl1 93.73(12) . . ?
N7 Ni1 Cl1 94.38(12) . . ?
N2 Ni1 Cl1 92.28(12) . . ?
N6 Ni1 Cl1 170.90(11) . . ?
O4 Cl2 O2 113.1(5) . . ?
O4 Cl2 O1 109.5(4) . . ?
O2 Cl2 O1 109.2(3) . . ?
O4 Cl2 O3 105.1(5) . . ?
O2 Cl2 O3 109.4(5) . . ?
O1 Cl2 O3 110.5(4) . . ?
C34 O5 H5 112.9 . . ?
C1 N1 C9 117.2(5) . . ?
C1 N1 Ni1 128.2(4) . . ?
C9 N1 Ni1 114.5(3) . . ?
C8 N2 C14 117.1(5) . . ?
C8 N2 Ni1 128.9(4) . . ?
C14 N2 Ni1 113.9(3) . . ?
C19 N5 C15 117.3(5) . . ?
C19 N5 Ni1 117.0(3) . . ?
C15 N5 Ni1 125.0(4) . . ?
C27 N6 C21 114.4(4) . . ?
C27 N6 C20 112.4(4) . . ?
C21 N6 C20 109.3(4) . . ?
C27 N6 Ni1 111.0(3) . . ?
C21 N6 Ni1 102.5(3) . . ?
C20 N6 Ni1 106.4(3) . . ?
C26 N7 C22 117.3(5) . . ?
C26 N7 Ni1 126.6(4) . . ?
C22 N7 Ni1 116.1(3) . . ?
N1 C1 C2 123.2(6) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C3 C2 C1 119.7(6) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.1 . . ?
C2 C3 C10 119.4(6) . . ?
C2 C3 H3 120.3 . . ?
C10 C3 H3 120.3 . . ?
C4 N3 C11 116.0(5) . . ?
N3 C4 C5 123.7(6) . . ?
N3 C4 H4 118.2 . . ?
C5 C4 H4 118.2 . . ?
N4 C5 C4 121.7(6) . . ?
N4 C5 H5A 119.1 . . ?
C4 C5 H5A 119.1 . . ?
C5 N4 C12 115.9(5) . . ?
C7 C6 C13 118.8(6) . . ?
C7 C6 H6 120.6 . . ?
C13 C6 H6 120.6 . . ?
C6 C7 C8 120.1(6) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
N2 C8 C7 122.9(5) . . ?
N2 C8 H8 118.5 . . ?
C7 C8 H8 118.5 . . ?
N2 C14 C13 123.2(5) . . ?
N2 C14 C9 116.0(4) . . ?
C13 C14 C9 120.7(5) . . ?
N1 C9 C10 123.3(5) . . ?
N1 C9 C14 116.4(4) . . ?
C10 C9 C14 120.2(5) . . ?
C3 C10 C9 117.1(5) . . ?
C3 C10 C11 123.6(5) . . ?
C9 C10 C11 119.3(5) . . ?
N3 C11 C12 120.4(5) . . ?
N3 C11 C10 119.2(5) . . ?
C12 C11 C10 120.4(5) . . ?
N4 C12 C11 122.2(5) . . ?
N4 C12 C13 117.7(5) . . ?
C11 C12 C13 120.0(5) . . ?
C14 C13 C6 117.8(5) . . ?
C14 C13 C12 119.0(5) . . ?
C6 C13 C12 123.2(5) . . ?
N5 C15 C16 123.3(6) . . ?
N5 C15 H15 118.4 . . ?
C16 C15 H15 118.3 . . ?
C15 C16 C17 118.9(6) . . ?
C15 C16 H16 120.6 . . ?
C17 C16 H16 120.5 . . ?
C16 C17 C18 118.8(7) . . ?
C16 C17 H17 120.6 . . ?
C18 C17 H17 120.6 . . ?
C17 C18 C19 119.6(7) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
N5 C19 C18 122.0(5) . . ?
N5 C19 C20 117.6(5) . . ?
C18 C19 C20 120.4(5) . . ?
N6 C20 C19 114.7(4) . . ?
N6 C20 H20A 108.6 . . ?
C19 C20 H20A 108.6 . . ?
N6 C20 H20B 108.6 . . ?
C19 C20 H20B 108.6 . . ?
H20A C20 H20B 107.6 . . ?
N6 C21 C22 110.7(4) . . ?
N6 C21 H21A 109.5 . . ?
C22 C21 H21A 109.5 . . ?
N6 C21 H21B 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 108.1 . . ?
N7 C22 C23 122.6(5) . . ?
N7 C22 C21 115.7(5) . . ?
C23 C22 C21 121.6(5) . . ?
C22 C23 C24 118.9(6) . . ?
C22 C23 H23 120.6 . . ?
C24 C23 H23 120.6 . . ?
C25 C24 C23 118.6(6) . . ?
C25 C24 H24 120.7 . . ?
C23 C24 H24 120.7 . . ?
C24 C25 C26 119.1(6) . . ?
C24 C25 H25 120.4 . . ?
C26 C25 H25 120.5 . . ?
N7 C26 C25 123.5(5) . . ?
N7 C26 H26 118.2 . . ?
C25 C26 H26 118.2 . . ?
C28 C27 C33 117.9(5) . . ?
C28 C27 N6 119.8(5) . . ?
C33 C27 N6 122.1(5) . . ?
C29 C28 C27 121.3(5) . . ?
C29 C28 H28 119.4 . . ?
C27 C28 H28 119.4 . . ?
C28 C29 C30 122.1(5) . . ?
C28 C29 H29 118.9 . . ?
C30 C29 H29 118.9 . . ?
C32 C30 C29 116.4(5) . . ?
C32 C30 C31 121.4(6) . . ?
C29 C30 C31 122.2(6) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.4 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 C33 122.4(5) . . ?
C30 C32 H32 118.8 . . ?
C33 C32 H32 118.8 . . ?
C27 C33 C32 119.8(5) . . ?
C27 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
O5 C34 H34A 108.4 . . ?
O5 C34 H34B 110.8 . . ?
H34A C34 H34B 109.5 . . ?
O5 C34 H34C 109.2 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 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
N5 Ni1 N1 C1 141.5(7) . . . . ?
N7 Ni1 N1 C1 10.5(5) . . . . ?
N2 Ni1 N1 C1 -175.8(5) . . . . ?
N6 Ni1 N1 C1 88.7(5) . . . . ?
Cl1 Ni1 N1 C1 -84.3(5) . . . . ?
N5 Ni1 N1 C9 -34.2(9) . . . . ?
N7 Ni1 N1 C9 -165.2(3) . . . . ?
N2 Ni1 N1 C9 8.5(3) . . . . ?
N6 Ni1 N1 C9 -87.0(3) . . . . ?
Cl1 Ni1 N1 C9 100.0(3) . . . . ?
N5 Ni1 N2 C8 -13.0(5) . . . . ?
N1 Ni1 N2 C8 176.3(5) . . . . ?
N7 Ni1 N2 C8 -142.1(9) . . . . ?
N6 Ni1 N2 C8 -92.9(5) . . . . ?
Cl1 Ni1 N2 C8 82.9(4) . . . . ?
N5 Ni1 N2 C14 161.9(3) . . . . ?
N1 Ni1 N2 C14 -8.8(3) . . . . ?
N7 Ni1 N2 C14 32.8(12) . . . . ?
N6 Ni1 N2 C14 82.0(3) . . . . ?
Cl1 Ni1 N2 C14 -102.2(3) . . . . ?
N1 Ni1 N5 C19 -54.0(9) . . . . ?
N7 Ni1 N5 C19 77.1(4) . . . . ?
N2 Ni1 N5 C19 -95.6(4) . . . . ?
N6 Ni1 N5 C19 0.0(4) . . . . ?
Cl1 Ni1 N5 C19 171.9(4) . . . . ?
N1 Ni1 N5 C15 116.0(7) . . . . ?
N7 Ni1 N5 C15 -112.9(4) . . . . ?
N2 Ni1 N5 C15 74.4(4) . . . . ?
N6 Ni1 N5 C15 170.0(4) . . . . ?
Cl1 Ni1 N5 C15 -18.0(4) . . . . ?
N5 Ni1 N6 C27 -110.8(3) . . . . ?
N1 Ni1 N6 C27 58.1(3) . . . . ?
N7 Ni1 N6 C27 152.6(3) . . . . ?
N2 Ni1 N6 C27 -20.2(3) . . . . ?
Cl1 Ni1 N6 C27 -172.9(6) . . . . ?
N5 Ni1 N6 C21 126.6(3) . . . . ?
N1 Ni1 N6 C21 -64.5(3) . . . . ?
N7 Ni1 N6 C21 29.9(3) . . . . ?
N2 Ni1 N6 C21 -142.8(3) . . . . ?
Cl1 Ni1 N6 C21 64.5(9) . . . . ?
N5 Ni1 N6 C20 11.8(3) . . . . ?
N1 Ni1 N6 C20 -179.3(3) . . . . ?
N7 Ni1 N6 C20 -84.8(3) . . . . ?
N2 Ni1 N6 C20 102.4(3) . . . . ?
Cl1 Ni1 N6 C20 -50.3(9) . . . . ?
N5 Ni1 N7 C26 86.1(5) . . . . ?
N1 Ni1 N7 C26 -104.2(5) . . . . ?
N2 Ni1 N7 C26 -144.9(9) . . . . ?
N6 Ni1 N7 C26 164.7(5) . . . . ?
Cl1 Ni1 N7 C26 -10.1(5) . . . . ?
N5 Ni1 N7 C22 -91.3(4) . . . . ?
N1 Ni1 N7 C22 78.4(4) . . . . ?
N2 Ni1 N7 C22 37.7(12) . . . . ?
N6 Ni1 N7 C22 -12.7(4) . . . . ?
Cl1 Ni1 N7 C22 172.5(4) . . . . ?
C9 N1 C1 C2 -1.4(8) . . . . ?
Ni1 N1 C1 C2 -177.0(4) . . . . ?
N1 C1 C2 C3 3.2(10) . . . . ?
C1 C2 C3 C10 -2.0(9) . . . . ?
C11 N3 C4 C5 -1.3(9) . . . . ?
N3 C4 C5 N4 0.8(10) . . . . ?
C4 C5 N4 C12 -0.7(9) . . . . ?
C13 C6 C7 C8 2.0(10) . . . . ?
C14 N2 C8 C7 -0.2(8) . . . . ?
Ni1 N2 C8 C7 174.5(4) . . . . ?
C6 C7 C8 N2 -2.2(10) . . . . ?
C8 N2 C14 C13 2.9(7) . . . . ?
Ni1 N2 C14 C13 -172.7(4) . . . . ?
C8 N2 C14 C9 -176.5(4) . . . . ?
Ni1 N2 C14 C9 7.9(5) . . . . ?
C1 N1 C9 C10 -1.6(7) . . . . ?
Ni1 N1 C9 C10 174.6(4) . . . . ?
C1 N1 C9 C14 176.8(4) . . . . ?
Ni1 N1 C9 C14 -7.0(5) . . . . ?
N2 C14 C9 N1 -0.7(6) . . . . ?
C13 C14 C9 N1 179.9(4) . . . . ?
N2 C14 C9 C10 177.7(4) . . . . ?
C13 C14 C9 C10 -1.7(7) . . . . ?
C2 C3 C10 C9 -0.7(8) . . . . ?
C2 C3 C10 C11 177.8(5) . . . . ?
N1 C9 C10 C3 2.6(7) . . . . ?
C14 C9 C10 C3 -175.7(4) . . . . ?
N1 C9 C10 C11 -175.9(4) . . . . ?
C14 C9 C10 C11 5.8(7) . . . . ?
C4 N3 C11 C12 1.7(8) . . . . ?
C4 N3 C11 C10 -177.6(5) . . . . ?
C3 C10 C11 N3 -4.0(8) . . . . ?
C9 C10 C11 N3 174.4(5) . . . . ?
C3 C10 C11 C12 176.6(5) . . . . ?
C9 C10 C11 C12 -4.9(7) . . . . ?
C5 N4 C12 C11 1.1(8) . . . . ?
C5 N4 C12 C13 178.9(5) . . . . ?
N3 C11 C12 N4 -1.7(8) . . . . ?
C10 C11 C12 N4 177.6(5) . . . . ?
N3 C11 C12 C13 -179.4(5) . . . . ?
C10 C11 C12 C13 0.0(8) . . . . ?
N2 C14 C13 C6 -3.0(8) . . . . ?
C9 C14 C13 C6 176.3(5) . . . . ?
N2 C14 C13 C12 177.4(5) . . . . ?
C9 C14 C13 C12 -3.3(7) . . . . ?
C7 C6 C13 C14 0.5(9) . . . . ?
C7 C6 C13 C12 -179.9(6) . . . . ?
N4 C12 C13 C14 -173.6(5) . . . . ?
C11 C12 C13 C14 4.2(8) . . . . ?
N4 C12 C13 C6 6.8(8) . . . . ?
C11 C12 C13 C6 -175.5(5) . . . . ?
C19 N5 C15 C16 0.1(8) . . . . ?
Ni1 N5 C15 C16 -169.9(5) . . . . ?
N5 C15 C16 C17 1.8(10) . . . . ?
C15 C16 C17 C18 -2.2(10) . . . . ?
C16 C17 C18 C19 0.8(10) . . . . ?
C15 N5 C19 C18 -1.6(8) . . . . ?
Ni1 N5 C19 C18 169.2(4) . . . . ?
C15 N5 C19 C20 176.4(5) . . . . ?
Ni1 N5 C19 C20 -12.8(6) . . . . ?
C17 C18 C19 N5 1.1(9) . . . . ?
C17 C18 C19 C20 -176.8(6) . . . . ?
C27 N6 C20 C19 100.2(5) . . . . ?
C21 N6 C20 C19 -131.6(5) . . . . ?
Ni1 N6 C20 C19 -21.5(5) . . . . ?
N5 C19 C20 N6 24.2(7) . . . . ?
C18 C19 C20 N6 -157.8(5) . . . . ?
C27 N6 C21 C22 -163.3(4) . . . . ?
C20 N6 C21 C22 69.5(5) . . . . ?
Ni1 N6 C21 C22 -43.1(5) . . . . ?
C26 N7 C22 C23 -2.5(8) . . . . ?
Ni1 N7 C22 C23 175.2(5) . . . . ?
C26 N7 C22 C21 173.4(5) . . . . ?
Ni1 N7 C22 C21 -8.9(6) . . . . ?
N6 C21 C22 N7 37.8(7) . . . . ?
N6 C21 C22 C23 -146.3(6) . . . . ?
N7 C22 C23 C24 2.7(10) . . . . ?
C21 C22 C23 C24 -173.0(6) . . . . ?
C22 C23 C24 C25 -0.9(11) . . . . ?
C23 C24 C25 C26 -0.9(11) . . . . ?
C22 N7 C26 C25 0.6(9) . . . . ?
Ni1 N7 C26 C25 -176.8(5) . . . . ?
C24 C25 C26 N7 1.1(10) . . . . ?
C21 N6 C27 C28 -164.5(5) . . . . ?
C20 N6 C27 C28 -39.0(6) . . . . ?
Ni1 N6 C27 C28 80.1(5) . . . . ?
C21 N6 C27 C33 20.7(7) . . . . ?
C20 N6 C27 C33 146.2(5) . . . . ?
Ni1 N6 C27 C33 -94.8(5) . . . . ?
C33 C27 C28 C29 2.7(8) . . . . ?
N6 C27 C28 C29 -172.3(5) . . . . ?
C27 C28 C29 C30 0.4(9) . . . . ?
C28 C29 C30 C32 -3.2(8) . . . . ?
C28 C29 C30 C31 177.3(5) . . . . ?
C29 C30 C32 C33 2.9(8) . . . . ?
C31 C30 C32 C33 -177.5(5) . . . . ?
C28 C27 C33 C32 -2.9(8) . . . . ?
N6 C27 C33 C32 172.0(4) . . . . ?
C30 C32 C33 C27 0.1(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.457
_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_cc
_database_code_depnum_ccdc_archive 'CCDC 910523'
_audit_update_record             
;
2012-11-12 deposited with the CCDC.
2015-03-18 downloaded from the CCDC.
;
#TrackingRef '5.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H29 Cl2 N7 Ni O5'
_chemical_formula_sum            'C37 H29 Cl2 N7 Ni O5'
_chemical_formula_weight         781.26

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/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                   7.5063(15)
_cell_length_b                   22.913(5)
_cell_length_c                   20.750(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.90(3)
_cell_angle_gamma                90.00
_cell_volume                     3564.2(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    5802
_cell_measurement_theta_min      2.8365
_cell_measurement_theta_max      29.1868

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1608
_exptl_absorpt_coefficient_mu    0.748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_T_max  0.9707
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26371
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.84
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6271
_reflns_number_gt                4937
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1030P)²+4.3028P] 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         6271
_refine_ls_number_parameters     470
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0629
_refine_ls_wR_factor_ref         0.1897
_refine_ls_wR_factor_gt          0.1753
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.002

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 0.68579(7) 0.83579(2) 0.00541(3) 0.0388(2) Uani 1 1 d . . .
Cl1 Cl 0.43713(15) 0.89545(5) -0.02226(8) 0.0655(4) Uani 1 1 d . . .
Cl2 Cl 0.97957(19) 0.81238(6) 0.27893(6) 0.0629(4) Uani 1 1 d . . .
O1 O 0.8359(7) 0.8079(3) 0.3183(2) 0.1147(18) Uani 1 1 d . . .
O2 O 0.9806(11) 0.7656(2) 0.2357(2) 0.141(3) Uani 1 1 d . . .
O3 O 0.9667(7) 0.86424(18) 0.2419(2) 0.0957(14) Uani 1 1 d . . .
O4 O 1.1382(9) 0.8097(4) 0.3180(3) 0.153(3) Uani 1 1 d . . .
O5 O 0.2755(11) 0.9551(7) 0.2914(7) 0.317(8) Uani 1 1 d . . .
N1 N 0.5804(5) 0.80980(14) 0.09212(17) 0.0406(8) Uani 1 1 d . . .
N2 N 0.5592(4) 0.75677(15) -0.02182(16) 0.0396(8) Uani 1 1 d . . .
N3 N 0.3637(5) 0.63931(17) 0.19671(19) 0.0524(10) Uani 1 1 d . . .
N4 N 0.3631(5) 0.58096(16) 0.0767(2) 0.0534(10) Uani 1 1 d . . .
N5 N 0.8353(5) 0.90388(14) 0.04834(17) 0.0423(8) Uani 1 1 d . . .
N6 N 0.9548(4) 0.79200(14) 0.02810(16) 0.0389(8) Uani 1 1 d . . .
N7 N 0.8008(5) 0.84467(16) -0.08235(17) 0.0464(9) Uani 1 1 d . . .
C1 C 0.5745(7) 0.8398(2) 0.1467(2) 0.0524(12) Uani 1 1 d . . .
H1 H 0.6180 0.8788 0.1476 0.063 Uiso 1 1 calc R . .
C2 C 0.5082(7) 0.8171(2) 0.2020(2) 0.0593(13) Uani 1 1 d . . .
H2 H 0.5033 0.8406 0.2396 0.071 Uiso 1 1 calc R . .
C3 C 0.4492(7) 0.7604(2) 0.2026(2) 0.0543(12) Uani 1 1 d . . .
H3 H 0.4066 0.7437 0.2408 0.065 Uiso 1 1 calc R . .
C4 C 0.2895(8) 0.5494(2) 0.2478(3) 0.0730(16) Uani 1 1 d . . .
H4 H 0.2861 0.5683 0.2884 0.088 Uiso 1 1 calc R . .
C5 C 0.2586(8) 0.4912(3) 0.2428(4) 0.0833(19) Uani 1 1 d . . .
H5 H 0.2334 0.4698 0.2804 0.100 Uiso 1 1 calc R . .
C6 C 0.2626(8) 0.4619(3) 0.1843(4) 0.0835(19) Uani 1 1 d . . .
H6 H 0.2392 0.4212 0.1822 0.100 Uiso 1 1 calc R . .
C7 C 0.3001(8) 0.4917(2) 0.1299(3) 0.0736(16) Uani 1 1 d . . .
H7 H 0.3073 0.4713 0.0903 0.088 Uiso 1 1 calc R . .
C8 C 0.4250(6) 0.6444(2) -0.0382(2) 0.0519(11) Uani 1 1 d . . .
H8 H 0.3789 0.6060 -0.0443 0.062 Uiso 1 1 calc R . .
C9 C 0.4751(7) 0.6764(2) -0.0895(2) 0.0534(12) Uani 1 1 d . . .
H9 H 0.4636 0.6607 -0.1318 0.064 Uiso 1 1 calc R . .
C10 C 0.5424(6) 0.7317(2) -0.0797(2) 0.0469(10) Uani 1 1 d . . .
H10 H 0.5788 0.7530 -0.1160 0.056 Uiso 1 1 calc R . .
C11 C 0.5060(5) 0.72548(16) 0.02922(19) 0.0350(8) Uani 1 1 d . . .
C12 C 0.5150(5) 0.75527(17) 0.09148(19) 0.0360(9) Uani 1 1 d . . .
C13 C 0.4530(5) 0.72805(18) 0.1463(2) 0.0414(9) Uani 1 1 d . . .
C14 C 0.4016(6) 0.66661(17) 0.1421(2) 0.0418(10) Uani 1 1 d . . .
C15 C 0.3997(5) 0.63708(18) 0.0819(2) 0.0426(10) Uani 1 1 d . . .
C16 C 0.4428(6) 0.66895(18) 0.0241(2) 0.0436(10) Uani 1 1 d . . .
C17 C 0.3270(6) 0.5815(2) 0.1917(3) 0.0556(12) Uani 1 1 d . . .
C18 C 0.3284(6) 0.5521(2) 0.1318(3) 0.0562(12) Uani 1 1 d . . .
C19 C 0.7938(6) 0.96084(18) 0.0457(2) 0.0503(11) Uani 1 1 d . . .
H19 H 0.6865 0.9725 0.0230 0.060 Uiso 1 1 calc R . .
C20 C 0.9005(7) 1.0028(2) 0.0744(3) 0.0611(13) Uani 1 1 d . . .
H20 H 0.8662 1.0427 0.0726 0.073 Uiso 1 1 calc R . .
C21 C 1.0574(8) 0.9865(2) 0.1060(3) 0.0654(14) Uani 1 1 d . . .
H21 H 1.1341 1.0150 0.1257 0.078 Uiso 1 1 calc R . .
C22 C 1.1021(7) 0.9287(2) 0.1089(2) 0.0565(12) Uani 1 1 d . . .
H22 H 1.2108 0.9165 0.1302 0.068 Uiso 1 1 calc R . .
C23 C 0.9873(6) 0.88836(18) 0.0806(2) 0.0430(10) Uani 1 1 d . . .
C24 C 1.0192(6) 0.82396(18) 0.0878(2) 0.0458(10) Uani 1 1 d . . .
H24A H 1.1483 0.8166 0.0961 0.055 Uiso 1 1 calc R . .
H24B H 0.9559 0.8092 0.1252 0.055 Uiso 1 1 calc R . .
C25 C 0.9412(5) 0.73003(17) 0.0369(2) 0.0377(9) Uani 1 1 d . . .
C26 C 0.9246(6) 0.70459(19) 0.0969(2) 0.0472(10) Uani 1 1 d . . .
H26 H 0.9329 0.7282 0.1346 0.057 Uiso 1 1 calc R . .
C27 C 0.8959(7) 0.6450(2) 0.1025(2) 0.0515(11) Uani 1 1 d . . .
H27 H 0.8835 0.6287 0.1441 0.062 Uiso 1 1 calc R . .
C28 C 0.8850(6) 0.6086(2) 0.0492(2) 0.0535(12) Uani 1 1 d . . .
C29 C 0.8445(9) 0.5449(2) 0.0565(3) 0.0751(16) Uani 1 1 d . . .
H29A H 0.9164 0.5290 0.0931 0.113 Uiso 1 1 calc R . .
H29B H 0.8731 0.5242 0.0170 0.113 Uiso 1 1 calc R . .
H29C H 0.7176 0.5399 0.0641 0.113 Uiso 1 1 calc R . .
C30 C 0.9100(6) 0.6341(2) -0.0100(2) 0.0525(11) Uani 1 1 d . . .
H30 H 0.9085 0.6101 -0.0474 0.063 Uiso 1 1 calc R . .
C31 C 0.9370(6) 0.6934(2) -0.0165(2) 0.0482(11) Uani 1 1 d . . .
H31 H 0.9529 0.7093 -0.0580 0.058 Uiso 1 1 calc R . .
C32 C 1.0701(6) 0.8088(2) -0.0251(2) 0.0462(10) Uani 1 1 d . . .
H32A H 1.1468 0.7752 -0.0351 0.055 Uiso 1 1 calc R . .
H32B H 1.1493 0.8411 -0.0100 0.055 Uiso 1 1 calc R . .
C33 C 0.9702(6) 0.82766(17) -0.0861(2) 0.0428(10) Uani 1 1 d . . .
C34 C 1.0571(8) 0.8304(2) -0.1434(2) 0.0604(13) Uani 1 1 d . . .
H34 H 1.1787 0.8191 -0.1445 0.073 Uiso 1 1 calc R . .
C35 C 0.9680(10) 0.8493(3) -0.1979(3) 0.0724(16) Uani 1 1 d . . .
H35 H 1.0255 0.8508 -0.2377 0.087 Uiso 1 1 calc R . .
C36 C 0.7919(9) 0.8664(2) -0.1947(3) 0.0728(17) Uani 1 1 d . . .
H36 H 0.7268 0.8798 -0.2323 0.087 Uiso 1 1 calc R . .
C37 C 0.7122(7) 0.8640(2) -0.1367(2) 0.0602(13) Uani 1 1 d . . .
H37 H 0.5916 0.8761 -0.1346 0.072 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 N7 2.064(4) . ?
Ni1 N1 2.089(3) . ?
Ni1 N5 2.094(3) . ?
Ni1 N2 2.108(3) . ?
Ni1 N6 2.283(3) . ?
Ni1 Cl1 2.3609(13) . ?
Cl2 O1 1.389(5) . ?
Cl2 O2 1.398(4) . ?
Cl2 O4 1.407(6) . ?
Cl2 O3 1.416(4) . ?
N1 C1 1.328(6) . ?
N1 C12 1.342(5) . ?
N2 C10 1.332(5) . ?
N2 C11 1.356(5) . ?
N3 C14 1.338(5) . ?
N3 C17 1.356(6) . ?
N4 C15 1.318(5) . ?
N4 C18 1.357(6) . ?
N5 C23 1.341(5) . ?
N5 C19 1.342(5) . ?
N6 C25 1.436(5) . ?
N6 C32 1.488(5) . ?
N6 C24 1.497(5) . ?
N7 C33 1.336(6) . ?
N7 C37 1.354(6) . ?
C1 C2 1.375(7) . ?
C2 C3 1.374(7) . ?
C3 C13 1.385(6) . ?
C4 C5 1.357(8) . ?
C4 C17 1.417(7) . ?
C5 C6 1.388(9) . ?
C6 C7 1.359(8) . ?
C7 C18 1.401(7) . ?
C8 C9 1.361(7) . ?
C8 C16 1.411(6) . ?
C9 C10 1.374(6) . ?
C11 C16 1.382(5) . ?
C11 C12 1.460(5) . ?
C12 C13 1.397(6) . ?
C13 C14 1.461(6) . ?
C14 C15 1.419(6) . ?
C15 C16 1.455(6) . ?
C17 C18 1.413(7) . ?
C19 C20 1.368(7) . ?
C20 C21 1.370(7) . ?
C21 C22 1.367(7) . ?
C22 C23 1.374(6) . ?
C23 C24 1.501(6) . ?
C25 C26 1.385(6) . ?
C25 C31 1.389(6) . ?
C26 C27 1.388(6) . ?
C27 C28 1.385(7) . ?
C28 C30 1.381(7) . ?
C28 C29 1.501(7) . ?
C30 C31 1.380(6) . ?
C32 C33 1.501(6) . ?
C33 C34 1.387(7) . ?
C34 C35 1.356(8) . ?
C35 C36 1.384(9) . ?
C36 C37 1.373(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
N7 Ni1 N1 168.98(14) . . ?
N7 Ni1 N5 93.59(14) . . ?
N1 Ni1 N5 93.68(13) . . ?
N7 Ni1 N2 92.94(13) . . ?
N1 Ni1 N2 78.51(13) . . ?
N5 Ni1 N2 168.01(13) . . ?
N7 Ni1 N6 79.63(14) . . ?
N1 Ni1 N6 93.83(13) . . ?
N5 Ni1 N6 77.88(13) . . ?
N2 Ni1 N6 93.44(13) . . ?
N7 Ni1 Cl1 95.12(11) . . ?
N1 Ni1 Cl1 92.59(10) . . ?
N5 Ni1 Cl1 94.14(10) . . ?
N2 Ni1 Cl1 95.28(10) . . ?
N6 Ni1 Cl1 170.06(9) . . ?
O1 Cl2 O2 110.5(4) . . ?
O1 Cl2 O4 108.5(4) . . ?
O2 Cl2 O4 107.7(5) . . ?
O1 Cl2 O3 110.4(3) . . ?
O2 Cl2 O3 107.3(3) . . ?
O4 Cl2 O3 112.4(4) . . ?
C1 N1 C12 117.6(4) . . ?
C1 N1 Ni1 128.1(3) . . ?
C12 N1 Ni1 114.3(3) . . ?
C10 N2 C11 117.3(4) . . ?
C10 N2 Ni1 129.3(3) . . ?
C11 N2 Ni1 113.0(3) . . ?
C14 N3 C17 116.3(4) . . ?
C15 N4 C18 117.0(4) . . ?
C23 N5 C19 117.9(4) . . ?
C23 N5 Ni1 116.0(3) . . ?
C19 N5 Ni1 126.0(3) . . ?
C25 N6 C32 113.5(3) . . ?
C25 N6 C24 113.6(3) . . ?
C32 N6 C24 108.2(3) . . ?
C25 N6 Ni1 113.1(2) . . ?
C32 N6 Ni1 106.0(2) . . ?
C24 N6 Ni1 101.6(2) . . ?
C33 N7 C37 118.4(4) . . ?
C33 N7 Ni1 117.7(3) . . ?
C37 N7 Ni1 123.8(3) . . ?
N1 C1 C2 123.0(4) . . ?
C3 C2 C1 119.7(4) . . ?
C2 C3 C13 118.6(4) . . ?
C5 C4 C17 119.2(6) . . ?
C4 C5 C6 122.1(5) . . ?
C7 C6 C5 119.8(5) . . ?
C6 C7 C18 120.7(6) . . ?
C9 C8 C16 118.9(4) . . ?
C8 C9 C10 119.8(4) . . ?
N2 C10 C9 123.2(4) . . ?
N2 C11 C16 123.3(4) . . ?
N2 C11 C12 116.2(3) . . ?
C16 C11 C12 120.4(4) . . ?
N1 C12 C13 123.0(4) . . ?
N1 C12 C11 116.4(3) . . ?
C13 C12 C11 120.6(4) . . ?
C3 C13 C12 118.0(4) . . ?
C3 C13 C14 123.3(4) . . ?
C12 C13 C14 118.7(4) . . ?
N3 C14 C15 121.9(4) . . ?
N3 C14 C13 117.8(4) . . ?
C15 C14 C13 120.2(4) . . ?
N4 C15 C14 122.0(4) . . ?
N4 C15 C16 118.4(4) . . ?
C14 C15 C16 119.6(4) . . ?
C11 C16 C8 117.4(4) . . ?
C11 C16 C15 119.8(4) . . ?
C8 C16 C15 122.7(4) . . ?
N3 C17 C18 121.5(4) . . ?
N3 C17 C4 119.5(5) . . ?
C18 C17 C4 119.0(5) . . ?
N4 C18 C7 119.5(5) . . ?
N4 C18 C17 121.3(4) . . ?
C7 C18 C17 119.2(5) . . ?
N5 C19 C20 122.3(4) . . ?
C19 C20 C21 119.2(5) . . ?
C22 C21 C20 119.2(5) . . ?
C21 C22 C23 119.0(5) . . ?
N5 C23 C22 122.3(4) . . ?
N5 C23 C24 115.9(4) . . ?
C22 C23 C24 121.7(4) . . ?
N6 C24 C23 110.8(3) . . ?
C26 C25 C31 117.5(4) . . ?
C26 C25 N6 122.7(4) . . ?
C31 C25 N6 119.7(4) . . ?
C25 C26 C27 120.7(4) . . ?
C28 C27 C26 121.9(4) . . ?
C30 C28 C27 116.8(4) . . ?
C30 C28 C29 122.6(5) . . ?
C27 C28 C29 120.6(5) . . ?
C31 C30 C28 122.0(4) . . ?
C30 C31 C25 121.0(4) . . ?
N6 C32 C33 114.5(3) . . ?
N7 C33 C34 121.8(4) . . ?
N7 C33 C32 118.1(4) . . ?
C34 C33 C32 119.9(4) . . ?
C35 C34 C33 119.7(6) . . ?
C34 C35 C36 118.9(5) . . ?
C37 C36 C35 119.4(5) . . ?
N7 C37 C36 121.7(5) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.425
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.082



