# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2010

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Kouki Matsubara'
_publ_contact_author_email       KMATSUBA@FUKUOKA-U.AC.JP

_publ_section_title              
;
A New Aspect of Nickel-Catalyzed Grignard Cross-Coupling
Reactions: Selective Synthesis, Structure, and Catalytic Behavior of a
T-Shape Three-Coordinate Nickel(I) Chloride Bearing a Bullky NHC Ligand
;
loop_
_publ_author_name
'Kouki Matsubara'
'Taisuke Matsumoto'
'Satoshi Miyazaki'

# Attachment 'Xray.cif'

data_2(hexane)
_database_code_depnum_ccdc_archive 'CCDC 737686'
#TrackingRef 'Xray.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H86 Cl N4 Ni'
_chemical_formula_weight         957.49

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'
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           Orthorhombic
_symmetry_space_group_name_H-M   P212121

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

_cell_length_a                   12.976(4)
_cell_length_b                   20.197(7)
_cell_length_c                   21.226(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5563(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    14513
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2076
_exptl_absorpt_coefficient_mu    0.436
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_absorpt_correction_T_min  0.9374
_exptl_absorpt_correction_T_max  0.9828

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71070
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 7.31
_diffrn_reflns_number            45580
_diffrn_reflns_av_R_equivalents  0.0900
_diffrn_reflns_av_sigmaI/netI    0.0861
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         27.48
_reflns_number_total             12669
_reflns_number_gt                10177
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrystalClear
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_structure_solution    SIR2002
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP III (Farrujia, 1998)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0805P)^2^+2.5822P] where P=(Fo^2^+2Fc^2^)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.009(15)
_refine_ls_number_reflns         12669
_refine_ls_number_parameters     596
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0691
_refine_ls_wR_factor_ref         0.1820
_refine_ls_wR_factor_gt          0.1704
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_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 0.75047(3) 0.005689(17) 0.28983(2) 0.01556(12) Uani 1 1 d . . .
Cl1 Cl 0.75453(8) 0.00631(4) 0.18167(4) 0.0264(2) Uani 1 1 d . . .
N1 N 0.6977(2) 0.14989(14) 0.27920(14) 0.0178(6) Uani 1 1 d . . .
N2 N 0.8505(2) 0.13623(14) 0.31453(14) 0.0164(6) Uani 1 1 d . . .
N3 N 0.8004(2) -0.14015(13) 0.28383(15) 0.0174(6) Uani 1 1 d . . .
N4 N 0.6476(2) -0.12244(14) 0.31620(15) 0.0186(6) Uani 1 1 d . . .
C1 C 0.7637(3) 0.10142(15) 0.29928(15) 0.0151(7) Uani 1 1 d . . .
C2 C 0.7447(3) 0.21191(15) 0.28048(17) 0.0228(7) Uani 1 1 d . . .
H1 H 0.7144 0.2528 0.2685 0.027 Uiso 1 1 calc R . .
C3 C 0.8403(3) 0.20293(17) 0.30164(18) 0.0230(8) Uani 1 1 d . . .
H2 H 0.8916 0.2360 0.3069 0.028 Uiso 1 1 calc R . .
C4 C 0.5912(3) 0.14358(16) 0.26144(18) 0.0179(7) Uani 1 1 d . . .
C5 C 0.5171(3) 0.13393(17) 0.30930(18) 0.0194(8) Uani 1 1 d . . .
C6 C 0.4145(3) 0.13269(19) 0.2914(2) 0.0257(8) Uani 1 1 d . . .
H3 H 0.3628 0.1263 0.3225 0.031 Uiso 1 1 calc R . .
C7 C 0.3856(3) 0.14067(19) 0.22880(19) 0.0241(8) Uani 1 1 d . . .
H4 H 0.3147 0.1393 0.2178 0.029 Uiso 1 1 calc R . .
C8 C 0.4588(3) 0.15066(19) 0.18219(19) 0.0231(9) Uani 1 1 d . . .
H5 H 0.4376 0.1563 0.1397 0.028 Uiso 1 1 calc R . .
C9 C 0.5648(3) 0.15258(17) 0.19751(18) 0.0205(8) Uani 1 1 d . . .
C10 C 0.5483(3) 0.12960(19) 0.37856(18) 0.0228(8) Uani 1 1 d . . .
H6 H 0.6091 0.0993 0.3814 0.027 Uiso 1 1 calc R . .
C11 C 0.4635(3) 0.1011(3) 0.4204(2) 0.0367(11) Uani 1 1 d . . .
H7 H 0.4196 0.1372 0.4358 0.044 Uiso 1 1 calc R . .
H8 H 0.4946 0.0780 0.4562 0.044 Uiso 1 1 calc R . .
H9 H 0.4217 0.0699 0.3959 0.044 Uiso 1 1 calc R . .
C12 C 0.5806(4) 0.1968(2) 0.4055(2) 0.0439(12) Uani 1 1 d . . .
H10 H 0.6550 0.2028 0.3999 0.053 Uiso 1 1 calc R . .
H11 H 0.5638 0.1985 0.4505 0.053 Uiso 1 1 calc R . .
H12 H 0.5438 0.2322 0.3834 0.053 Uiso 1 1 calc R . .
C13 C 0.6431(3) 0.16637(19) 0.14678(19) 0.0239(8) Uani 1 1 d . . .
H13 H 0.7129 0.1563 0.1642 0.029 Uiso 1 1 calc R . .
C14 C 0.6265(3) 0.1225(2) 0.0880(2) 0.0341(10) Uani 1 1 d . . .
H14 H 0.6655 0.0813 0.0927 0.041 Uiso 1 1 calc R . .
H15 H 0.6504 0.1462 0.0504 0.041 Uiso 1 1 calc R . .
H16 H 0.5530 0.1123 0.0836 0.041 Uiso 1 1 calc R . .
C15 C 0.6410(4) 0.2399(2) 0.1280(2) 0.0395(11) Uani 1 1 d . . .
H17 H 0.7109 0.2544 0.1172 0.047 Uiso 1 1 calc R . .
H18 H 0.6151 0.2664 0.1633 0.047 Uiso 1 1 calc R . .
H19 H 0.5958 0.2458 0.0914 0.047 Uiso 1 1 calc R . .
C16 C 0.9491(3) 0.11012(17) 0.33593(18) 0.0171(7) Uani 1 1 d . . .
C17 C 0.9689(3) 0.11166(18) 0.40043(19) 0.0208(8) Uani 1 1 d . . .
C18 C 1.0704(3) 0.0962(2) 0.41988(19) 0.0244(9) Uani 1 1 d . . .
H20 H 1.0879 0.0970 0.4633 0.029 Uiso 1 1 calc R . .
C19 C 1.1446(3) 0.0798(2) 0.3750(2) 0.0286(9) Uani 1 1 d . . .
H21 H 1.2129 0.0704 0.3883 0.034 Uiso 1 1 calc R . .
C20 C 1.1212(3) 0.07692(19) 0.3118(2) 0.0245(8) Uani 1 1 d . . .
H22 H 1.1725 0.0639 0.2824 0.029 Uiso 1 1 calc R . .
C21 C 1.0218(3) 0.09312(16) 0.29034(19) 0.0196(7) Uani 1 1 d . . .
C22 C 0.8886(3) 0.1302(2) 0.4498(2) 0.0317(10) Uani 1 1 d . . .
H23 H 0.8190 0.1264 0.4299 0.038 Uiso 1 1 calc R . .
C23 C 0.8911(4) 0.0838(3) 0.5073(3) 0.0564(15) Uani 1 1 d . . .
H24 H 0.8444 0.0464 0.5001 0.068 Uiso 1 1 calc R . .
H25 H 0.8691 0.1083 0.5448 0.068 Uiso 1 1 calc R . .
H26 H 0.9614 0.0673 0.5135 0.068 Uiso 1 1 calc R . .
C24 C 0.9023(5) 0.2005(3) 0.4715(3) 0.0709(19) Uani 1 1 d . . .
H27 H 0.9495 0.2016 0.5075 0.085 Uiso 1 1 calc R . .
H28 H 0.8354 0.2188 0.4840 0.085 Uiso 1 1 calc R . .
H29 H 0.9310 0.2271 0.4370 0.085 Uiso 1 1 calc R . .
C25 C 0.9974(3) 0.09420(18) 0.22048(18) 0.0219(8) Uani 1 1 d . . .
H30 H 0.9209 0.0975 0.2159 0.026 Uiso 1 1 calc R . .
C26 C 1.0320(4) 0.0312(2) 0.1874(2) 0.0329(10) Uani 1 1 d . . .
H31 H 1.1029 0.0366 0.1723 0.040 Uiso 1 1 calc R . .
H32 H 0.9864 0.0223 0.1516 0.040 Uiso 1 1 calc R . .
H33 H 1.0290 -0.0060 0.2170 0.040 Uiso 1 1 calc R . .
C27 C 1.0447(4) 0.1553(2) 0.1900(2) 0.0311(10) Uani 1 1 d . . .
H34 H 0.9950 0.1918 0.1912 0.037 Uiso 1 1 calc R . .
H35 H 1.0627 0.1454 0.1462 0.037 Uiso 1 1 calc R . .
H36 H 1.1070 0.1680 0.2132 0.037 Uiso 1 1 calc R . .
C28 C 0.7357(3) -0.08953(15) 0.29924(16) 0.0176(7) Uani 1 1 d . . .
C29 C 0.7541(3) -0.20140(16) 0.29082(19) 0.0288(8) Uani 1 1 d . . .
H37 H 0.7844 -0.2434 0.2827 0.035 Uiso 1 1 calc R . .
C30 C 0.6580(3) -0.18981(18) 0.3113(2) 0.0282(9) Uani 1 1 d . . .
H38 H 0.6070 -0.2221 0.3207 0.034 Uiso 1 1 calc R . .
C31 C 0.9075(3) -0.13567(16) 0.26604(18) 0.0173(7) Uani 1 1 d . . .
C32 C 0.9810(3) -0.12959(18) 0.3149(2) 0.0245(8) Uani 1 1 d . . .
C33 C 1.0842(3) -0.12809(19) 0.2974(2) 0.0285(9) Uani 1 1 d . . .
H39 H 1.1354 -0.1236 0.3291 0.034 Uiso 1 1 calc R . .
C34 C 1.1145(3) -0.13286(18) 0.2355(2) 0.0255(8) Uani 1 1 d . . .
H40 H 1.1856 -0.1307 0.2251 0.031 Uiso 1 1 calc R . .
C35 C 1.0421(3) -0.14075(19) 0.1884(2) 0.0234(8) Uani 1 1 d . . .
H41 H 1.0640 -0.1449 0.1458 0.028 Uiso 1 1 calc R . .
C36 C 0.9358(3) -0.14269(17) 0.20278(18) 0.0203(8) Uani 1 1 d . . .
C37 C 0.9495(3) -0.1296(2) 0.38371(19) 0.0280(9) Uani 1 1 d . . .
H42 H 0.8727 -0.1330 0.3856 0.034 Uiso 1 1 calc R . .
C38 C 0.9946(4) -0.1888(2) 0.4192(2) 0.0431(12) Uani 1 1 d . . .
H43 H 0.9468 -0.2263 0.4166 0.052 Uiso 1 1 calc R . .
H44 H 1.0051 -0.1769 0.4635 0.052 Uiso 1 1 calc R . .
H45 H 1.0608 -0.2012 0.4003 0.052 Uiso 1 1 calc R . .
C39 C 0.9806(5) -0.0648(2) 0.4153(2) 0.0552(15) Uani 1 1 d . . .
H46 H 1.0500 -0.0693 0.4331 0.066 Uiso 1 1 calc R . .
H47 H 0.9317 -0.0544 0.4490 0.066 Uiso 1 1 calc R . .
H48 H 0.9802 -0.0290 0.3841 0.066 Uiso 1 1 calc R . .
C40 C 0.8571(3) -0.1540(2) 0.1501(2) 0.0286(9) Uani 1 1 d . . .
H49 H 0.7888 -0.1374 0.1652 0.034 Uiso 1 1 calc R . .
C41 C 0.8464(4) -0.2290(2) 0.1366(2) 0.0427(12) Uani 1 1 d . . .
H50 H 0.8956 -0.2418 0.1037 0.051 Uiso 1 1 calc R . .
H51 H 0.7762 -0.2385 0.1223 0.051 Uiso 1 1 calc R . .
H52 H 0.8608 -0.2540 0.1751 0.051 Uiso 1 1 calc R . .
C42 C 0.8850(4) -0.1161(2) 0.0901(2) 0.0386(11) Uani 1 1 d . . .
H53 H 0.8534 -0.0720 0.0913 0.046 Uiso 1 1 calc R . .
H54 H 0.8593 -0.1403 0.0533 0.046 Uiso 1 1 calc R . .
H55 H 0.9600 -0.1116 0.0872 0.046 Uiso 1 1 calc R . .
C43 C 0.5495(3) -0.09464(17) 0.33451(18) 0.0193(8) Uani 1 1 d . . .
C44 C 0.4788(3) -0.08012(17) 0.28566(18) 0.0198(7) Uani 1 1 d . . .
C45 C 0.3800(3) -0.06154(19) 0.3045(2) 0.0255(8) Uani 1 1 d . . .
H56 H 0.3310 -0.0493 0.2734 0.031 Uiso 1 1 calc R . .
C46 C 0.3513(3) -0.0604(2) 0.3676(2) 0.0277(9) Uani 1 1 d . . .
H57 H 0.2822 -0.0502 0.3789 0.033 Uiso 1 1 calc R . .
C47 C 0.4231(3) -0.0740(2) 0.4138(2) 0.0286(9) Uani 1 1 d . . .
H58 H 0.4032 -0.0713 0.4568 0.034 Uiso 1 1 calc R . .
C48 C 0.5252(3) -0.09182(19) 0.39883(19) 0.0223(8) Uani 1 1 d . . .
C49 C 0.5091(3) -0.08553(18) 0.21710(19) 0.0232(8) Uani 1 1 d . . .
H59 H 0.5860 -0.0871 0.2149 0.028 Uiso 1 1 calc R . .
C50 C 0.4726(4) -0.0253(2) 0.1787(2) 0.0343(10) Uani 1 1 d . . .
H60 H 0.4035 -0.0339 0.1620 0.041 Uiso 1 1 calc R . .
H61 H 0.5205 -0.0175 0.1438 0.041 Uiso 1 1 calc R . .
H62 H 0.4707 0.0139 0.2060 0.041 Uiso 1 1 calc R . .
C51 C 0.4674(4) -0.1498(2) 0.1892(2) 0.0377(11) Uani 1 1 d . . .
H63 H 0.5187 -0.1850 0.1945 0.045 Uiso 1 1 calc R . .
H64 H 0.4531 -0.1435 0.1443 0.045 Uiso 1 1 calc R . .
H65 H 0.4037 -0.1622 0.2111 0.045 Uiso 1 1 calc R . .
C52 C 0.6041(3) -0.1039(2) 0.4500(2) 0.0281(9) Uani 1 1 d . . .
H66 H 0.6643 -0.1265 0.4299 0.034 Uiso 1 1 calc R . .
C53 C 0.5658(4) -0.1487(3) 0.5017(3) 0.068(2) Uani 1 1 d . . .
H67 H 0.5330 -0.1221 0.5347 0.081 Uiso 1 1 calc R . .
H68 H 0.6240 -0.1732 0.5197 0.081 Uiso 1 1 calc R . .
H69 H 0.5155 -0.1800 0.4844 0.081 Uiso 1 1 calc R . .
C54 C 0.6423(6) -0.0392(3) 0.4761(4) 0.111(3) Uani 1 1 d . . .
H70 H 0.7038 -0.0252 0.4529 0.134 Uiso 1 1 calc R . .
H71 H 0.6596 -0.0447 0.5208 0.134 Uiso 1 1 calc R . .
H72 H 0.5884 -0.0055 0.4718 0.134 Uiso 1 1 calc R . .
C55 C 1.2483(4) 0.1271(2) 0.5574(2) 0.0396(10) Uani 1 1 d . . .
H73 H 1.2933 0.1429 0.5235 0.047 Uiso 1 1 calc R . .
H74 H 1.2530 0.1573 0.5934 0.047 Uiso 1 1 calc R . .
H75 H 1.1770 0.1256 0.5424 0.047 Uiso 1 1 calc R . .
C56 C 1.2817(3) 0.0585(2) 0.5775(2) 0.0399(11) Uani 1 1 d . . .
H76 H 1.2677 0.0533 0.6230 0.048 Uiso 1 1 calc R . .
H77 H 1.3570 0.0545 0.5712 0.048 Uiso 1 1 calc R . .
C57 C 1.2287(3) 0.0029(2) 0.54216(18) 0.0328(10) Uani 1 1 d . . .
H78 H 1.1532 0.0086 0.5461 0.039 Uiso 1 1 calc R . .
H79 H 1.2463 0.0065 0.4969 0.039 Uiso 1 1 calc R . .
C58 C 1.2571(4) -0.0656(2) 0.56489(18) 0.0332(9) Uani 1 1 d . . .
H80 H 1.2363 -0.0700 0.6096 0.040 Uiso 1 1 calc R . .
H81 H 1.3330 -0.0705 0.5630 0.040 Uiso 1 1 calc R . .
C59 C 1.2082(3) -0.1214(2) 0.5275(2) 0.0348(10) Uani 1 1 d . . .
H82 H 1.2243 -0.1150 0.4823 0.042 Uiso 1 1 calc R . .
H83 H 1.1325 -0.1189 0.5324 0.042 Uiso 1 1 calc R . .
C60 C 1.2441(4) -0.1898(2) 0.5473(2) 0.0438(11) Uani 1 1 d . . .
H84 H 1.3048 -0.2024 0.5226 0.053 Uiso 1 1 calc R . .
H85 H 1.1887 -0.2219 0.5400 0.053 Uiso 1 1 calc R . .
H86 H 1.2620 -0.1894 0.5922 0.053 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0134(2) 0.01199(18) 0.0213(2) 0.00126(14) 0.0002(2) -0.00012(19)
Cl1 0.0333(5) 0.0219(4) 0.0240(4) 0.0013(3) -0.0006(4) 0.0012(5)
N1 0.0154(15) 0.0138(13) 0.0242(17) 0.0034(11) 0.0000(13) 0.0004(11)
N2 0.0140(15) 0.0145(13) 0.0207(15) 0.0007(12) -0.0002(12) 0.0008(11)
N3 0.0144(15) 0.0115(13) 0.0263(17) 0.0011(12) 0.0058(13) 0.0016(11)
N4 0.0139(15) 0.0150(14) 0.0268(17) 0.0013(12) 0.0041(13) -0.0005(11)
C1 0.0145(18) 0.0142(13) 0.0167(16) -0.0011(11) 0.0024(14) 0.0014(13)
C2 0.0213(19) 0.0143(14) 0.033(2) 0.0011(12) -0.006(2) -0.0002(16)
C3 0.0198(19) 0.0159(16) 0.033(2) -0.0012(15) -0.0021(17) -0.0003(14)
C4 0.0170(19) 0.0145(15) 0.0222(18) -0.0002(14) -0.0049(15) 0.0012(13)
C5 0.0167(19) 0.0154(15) 0.026(2) 0.0000(14) 0.0034(16) 0.0022(13)
C6 0.021(2) 0.0250(18) 0.031(2) -0.0004(17) -0.0013(18) 0.0051(15)
C7 0.0127(18) 0.0283(19) 0.031(2) -0.0029(17) -0.0033(16) 0.0023(14)
C8 0.027(2) 0.0220(19) 0.0200(19) -0.0022(15) -0.0123(17) 0.0042(16)
C9 0.0173(19) 0.0189(16) 0.025(2) 0.0008(14) -0.0015(16) 0.0058(14)
C10 0.023(2) 0.025(2) 0.020(2) 0.0005(15) -0.0003(16) 0.0044(16)
C11 0.035(3) 0.050(3) 0.025(2) 0.004(2) 0.000(2) -0.003(2)
C12 0.066(3) 0.041(3) 0.025(2) -0.003(2) -0.006(2) -0.015(2)
C13 0.021(2) 0.026(2) 0.025(2) 0.0044(16) -0.0001(16) 0.0006(16)
C14 0.034(3) 0.046(3) 0.023(2) -0.0016(18) 0.0018(19) 0.010(2)
C15 0.045(3) 0.036(2) 0.037(3) 0.011(2) 0.010(2) 0.004(2)
C16 0.0121(18) 0.0130(16) 0.026(2) 0.0030(14) -0.0054(15) -0.0022(13)
C17 0.0173(19) 0.0188(17) 0.026(2) 0.0012(15) 0.0003(16) 0.0032(14)
C18 0.018(2) 0.034(2) 0.020(2) 0.0046(16) -0.0078(16) -0.0033(16)
C19 0.015(2) 0.030(2) 0.041(3) 0.0082(18) 0.0008(18) -0.0030(15)
C20 0.0140(19) 0.0278(19) 0.032(2) 0.0077(16) 0.0041(16) 0.0021(15)
C21 0.0166(18) 0.0153(15) 0.027(2) 0.0052(15) 0.0024(16) 0.0008(13)
C22 0.022(2) 0.039(2) 0.034(2) -0.0044(19) 0.0006(18) -0.0006(18)
C23 0.054(3) 0.069(4) 0.046(3) 0.008(3) 0.022(3) 0.011(3)
C24 0.094(5) 0.055(4) 0.064(4) -0.021(3) 0.036(4) 0.011(3)
C25 0.020(2) 0.0203(17) 0.025(2) -0.0010(14) 0.0037(15) -0.0037(14)
C26 0.040(3) 0.026(2) 0.033(2) -0.0021(18) 0.006(2) -0.0012(18)
C27 0.036(3) 0.028(2) 0.029(2) 0.0066(18) 0.000(2) -0.0080(18)
C28 0.0175(19) 0.0166(14) 0.0188(17) -0.0010(12) -0.0006(15) 0.0003(13)
C29 0.029(2) 0.0117(14) 0.046(2) 0.0030(14) 0.013(2) 0.0017(16)
C30 0.020(2) 0.0165(17) 0.048(3) 0.0069(17) 0.0115(19) -0.0038(15)
C31 0.0150(18) 0.0139(14) 0.0231(18) 0.0031(14) 0.0001(15) 0.0003(12)
C32 0.025(2) 0.0178(17) 0.031(2) -0.0017(16) -0.0006(17) 0.0041(15)
C33 0.0123(19) 0.0250(19) 0.048(3) -0.0019(19) -0.0051(18) 0.0033(14)
C34 0.0156(19) 0.0196(17) 0.041(2) -0.0003(17) 0.0072(18) 0.0026(14)
C35 0.024(2) 0.0198(18) 0.027(2) -0.0011(16) 0.0076(17) 0.0026(15)
C36 0.0195(19) 0.0161(16) 0.025(2) 0.0019(14) 0.0024(16) 0.0035(13)
C37 0.025(2) 0.036(2) 0.023(2) -0.0016(17) -0.0043(17) 0.0044(17)
C38 0.076(4) 0.021(2) 0.032(2) 0.0008(18) 0.005(2) 0.003(2)
C39 0.106(5) 0.027(2) 0.032(3) -0.002(2) 0.000(3) 0.003(3)
C40 0.028(2) 0.028(2) 0.030(2) -0.0104(17) 0.0024(18) 0.0041(17)
C41 0.049(3) 0.033(2) 0.046(3) -0.014(2) -0.009(2) -0.004(2)
C42 0.046(3) 0.046(3) 0.023(2) -0.0020(19) 0.001(2) 0.009(2)
C43 0.0156(19) 0.0162(16) 0.026(2) -0.0019(14) 0.0014(15) -0.0019(14)
C44 0.0156(18) 0.0206(16) 0.0232(19) -0.0032(15) 0.0014(16) -0.0028(13)
C45 0.019(2) 0.0239(18) 0.033(2) -0.0019(16) -0.0084(17) 0.0014(15)
C46 0.015(2) 0.035(2) 0.033(2) -0.0061(18) 0.0024(17) 0.0015(16)
C47 0.025(2) 0.031(2) 0.030(2) -0.0027(17) 0.0051(18) 0.0017(17)
C48 0.017(2) 0.0246(19) 0.025(2) 0.0033(16) 0.0066(16) -0.0001(15)
C49 0.020(2) 0.0245(18) 0.025(2) -0.0031(15) -0.0003(16) -0.0049(14)
C50 0.039(3) 0.037(2) 0.027(2) 0.0035(18) -0.0022(19) 0.001(2)
C51 0.051(3) 0.033(2) 0.029(2) -0.0054(19) 0.000(2) -0.014(2)
C52 0.024(2) 0.032(2) 0.029(2) 0.0035(17) 0.0020(18) 0.0043(17)
C53 0.039(3) 0.105(5) 0.059(4) 0.049(4) 0.004(3) 0.008(3)
C54 0.146(7) 0.037(3) 0.151(7) 0.003(4) -0.123(6) -0.012(4)
C55 0.036(2) 0.044(2) 0.038(2) 0.0010(18) -0.006(2) -0.009(3)
C56 0.032(3) 0.047(3) 0.041(3) 0.006(2) -0.009(2) 0.0007(19)
C57 0.031(3) 0.050(3) 0.0176(18) 0.0030(17) -0.0023(16) 0.0002(19)
C58 0.029(2) 0.050(2) 0.0196(19) 0.0029(16) 0.001(2) -0.001(2)
C59 0.028(2) 0.048(3) 0.028(2) 0.0023(19) 0.0014(18) -0.0096(19)
C60 0.039(3) 0.049(3) 0.043(3) 0.000(2) 0.003(3) -0.002(3)

_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 C28 1.943(3) . ?
Ni1 C1 1.952(3) . ?
Ni1 Cl1 2.2966(12) . ?
N1 C1 1.369(4) . ?
N1 C2 1.394(4) . ?
N1 C4 1.439(5) . ?
N2 C1 1.367(4) . ?
N2 C3 1.381(4) . ?
N2 C16 1.456(4) . ?
N3 C28 1.363(4) . ?
N3 C29 1.383(4) . ?
N3 C31 1.443(4) . ?
N4 C28 1.370(4) . ?
N4 C30 1.371(5) . ?
N4 C43 1.445(5) . ?
C2 C3 1.331(5) . ?
C4 C9 1.411(5) . ?
C4 C5 1.412(5) . ?
C5 C6 1.385(5) . ?
C5 C10 1.527(5) . ?
C6 C7 1.390(6) . ?
C7 C8 1.386(6) . ?
C8 C9 1.414(5) . ?
C9 C13 1.506(5) . ?
C10 C11 1.526(6) . ?
C10 C12 1.532(6) . ?
C13 C15 1.539(6) . ?
C13 C14 1.545(6) . ?
C16 C17 1.393(5) . ?
C16 C21 1.395(5) . ?
C17 C18 1.415(5) . ?
C17 C22 1.525(6) . ?
C18 C19 1.395(6) . ?
C19 C20 1.376(6) . ?
C20 C21 1.406(5) . ?
C21 C25 1.517(5) . ?
C22 C24 1.504(7) . ?
C22 C23 1.538(7) . ?
C25 C26 1.521(5) . ?
C25 C27 1.522(5) . ?
C29 C30 1.342(5) . ?
C31 C36 1.400(5) . ?
C31 C32 1.414(5) . ?
C32 C33 1.391(5) . ?
C32 C37 1.517(6) . ?
C33 C34 1.374(6) . ?
C34 C35 1.382(6) . ?
C35 C36 1.413(5) . ?
C36 C40 1.532(6) . ?
C37 C39 1.524(6) . ?
C37 C38 1.531(6) . ?
C40 C42 1.530(6) . ?
C40 C41 1.548(6) . ?
C43 C48 1.402(5) . ?
C43 C44 1.415(5) . ?
C44 C45 1.394(5) . ?
C44 C49 1.511(5) . ?
C45 C46 1.390(6) . ?
C46 C47 1.381(6) . ?
C47 C48 1.409(5) . ?
C48 C52 1.512(6) . ?
C49 C51 1.526(5) . ?
C49 C50 1.539(6) . ?
C52 C54 1.504(7) . ?
C52 C53 1.507(6) . ?
C55 C56 1.513(6) . ?
C56 C57 1.515(6) . ?
C57 C58 1.512(6) . ?
C58 C59 1.516(6) . ?
C59 C60 1.518(6) . ?

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
C28 Ni1 C1 168.18(15) . . ?
C28 Ni1 Cl1 96.34(10) . . ?
C1 Ni1 Cl1 95.47(10) . . ?
C1 N1 C2 111.3(3) . . ?
C1 N1 C4 128.3(3) . . ?
C2 N1 C4 120.4(3) . . ?
C1 N2 C3 112.1(3) . . ?
C1 N2 C16 127.7(3) . . ?
C3 N2 C16 120.0(3) . . ?
C28 N3 C29 112.2(3) . . ?
C28 N3 C31 127.5(3) . . ?
C29 N3 C31 120.2(3) . . ?
C28 N4 C30 112.3(3) . . ?
C28 N4 C43 128.1(3) . . ?
C30 N4 C43 119.5(3) . . ?
N2 C1 N1 102.8(3) . . ?
N2 C1 Ni1 127.4(2) . . ?
N1 C1 Ni1 128.4(3) . . ?
C3 C2 N1 107.0(3) . . ?
C2 C3 N2 106.8(3) . . ?
C9 C4 C5 123.0(3) . . ?
C9 C4 N1 118.3(3) . . ?
C5 C4 N1 118.5(3) . . ?
C6 C5 C4 117.3(4) . . ?
C6 C5 C10 121.2(4) . . ?
C4 C5 C10 121.4(3) . . ?
C5 C6 C7 121.3(4) . . ?
C8 C7 C6 121.0(4) . . ?
C7 C8 C9 120.4(4) . . ?
C4 C9 C8 117.0(4) . . ?
C4 C9 C13 123.2(3) . . ?
C8 C9 C13 119.8(3) . . ?
C11 C10 C5 113.0(3) . . ?
C11 C10 C12 108.3(4) . . ?
C5 C10 C12 112.4(3) . . ?
C9 C13 C15 110.7(3) . . ?
C9 C13 C14 112.2(3) . . ?
C15 C13 C14 109.9(4) . . ?
C17 C16 C21 124.2(3) . . ?
C17 C16 N2 117.4(3) . . ?
C21 C16 N2 117.9(3) . . ?
C16 C17 C18 117.0(4) . . ?
C16 C17 C22 123.7(3) . . ?
C18 C17 C22 119.3(4) . . ?
C19 C18 C17 119.7(4) . . ?
C20 C19 C18 121.6(4) . . ?
C19 C20 C21 120.5(4) . . ?
C16 C21 C20 117.0(4) . . ?
C16 C21 C25 122.2(3) . . ?
C20 C21 C25 120.8(3) . . ?
C24 C22 C17 111.1(4) . . ?
C24 C22 C23 109.3(4) . . ?
C17 C22 C23 112.4(4) . . ?
C21 C25 C26 112.2(3) . . ?
C21 C25 C27 110.0(3) . . ?
C26 C25 C27 111.3(3) . . ?
N3 C28 N4 102.3(3) . . ?
N3 C28 Ni1 131.0(3) . . ?
N4 C28 Ni1 126.1(2) . . ?
C30 C29 N3 106.4(3) . . ?
C29 C30 N4 106.8(3) . . ?
C36 C31 C32 122.4(3) . . ?
C36 C31 N3 119.9(3) . . ?
C32 C31 N3 117.6(3) . . ?
C33 C32 C31 117.1(4) . . ?
C33 C32 C37 121.1(4) . . ?
C31 C32 C37 121.6(3) . . ?
C34 C33 C32 121.9(4) . . ?
C33 C34 C35 120.4(4) . . ?
C34 C35 C36 120.6(4) . . ?
C31 C36 C35 117.5(4) . . ?
C31 C36 C40 122.7(3) . . ?
C35 C36 C40 119.8(4) . . ?
C32 C37 C39 110.6(4) . . ?
C32 C37 C38 111.8(4) . . ?
C39 C37 C38 110.7(4) . . ?
C42 C40 C36 112.1(4) . . ?
C42 C40 C41 110.9(4) . . ?
C36 C40 C41 109.9(4) . . ?
C48 C43 C44 124.1(3) . . ?
C48 C43 N4 118.4(3) . . ?
C44 C43 N4 117.0(3) . . ?
C45 C44 C43 116.1(4) . . ?
C45 C44 C49 122.3(3) . . ?
C43 C44 C49 121.5(3) . . ?
C46 C45 C44 121.9(4) . . ?
C47 C46 C45 120.0(4) . . ?
C46 C47 C48 121.7(4) . . ?
C43 C48 C47 116.1(4) . . ?
C43 C48 C52 122.8(3) . . ?
C47 C48 C52 121.0(4) . . ?
C44 C49 C51 110.0(3) . . ?
C44 C49 C50 111.9(3) . . ?
C51 C49 C50 111.0(4) . . ?
C54 C52 C53 111.2(5) . . ?
C54 C52 C48 110.3(4) . . ?
C53 C52 C48 113.4(4) . . ?
C55 C56 C57 114.2(4) . . ?
C58 C57 C56 114.2(3) . . ?
C57 C58 C59 114.3(4) . . ?
C58 C59 C60 113.8(4) . . ?

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
C3 N2 C1 N1 -2.7(4) . . . . ?
C16 N2 C1 N1 -176.7(3) . . . . ?
C3 N2 C1 Ni1 164.4(3) . . . . ?
C16 N2 C1 Ni1 -9.5(5) . . . . ?
C2 N1 C1 N2 1.8(4) . . . . ?
C4 N1 C1 N2 -174.9(3) . . . . ?
C2 N1 C1 Ni1 -165.2(3) . . . . ?
C4 N1 C1 Ni1 18.1(5) . . . . ?
C28 Ni1 C1 N2 80.3(8) . . . . ?
Cl1 Ni1 C1 N2 -101.5(3) . . . . ?
C28 Ni1 C1 N1 -115.7(7) . . . . ?
Cl1 Ni1 C1 N1 62.5(3) . . . . ?
C1 N1 C2 C3 -0.3(4) . . . . ?
C4 N1 C2 C3 176.7(3) . . . . ?
N1 C2 C3 N2 -1.4(4) . . . . ?
C1 N2 C3 C2 2.7(4) . . . . ?
C16 N2 C3 C2 177.2(3) . . . . ?
C1 N1 C4 C9 -111.2(4) . . . . ?
C2 N1 C4 C9 72.3(4) . . . . ?
C1 N1 C4 C5 73.8(5) . . . . ?
C2 N1 C4 C5 -102.7(4) . . . . ?
C9 C4 C5 C6 0.8(5) . . . . ?
N1 C4 C5 C6 175.5(3) . . . . ?
C9 C4 C5 C10 -175.3(3) . . . . ?
N1 C4 C5 C10 -0.5(5) . . . . ?
C4 C5 C6 C7 0.0(5) . . . . ?
C10 C5 C6 C7 176.0(3) . . . . ?
C5 C6 C7 C8 -0.5(6) . . . . ?
C6 C7 C8 C9 0.3(6) . . . . ?
C5 C4 C9 C8 -0.9(5) . . . . ?
N1 C4 C9 C8 -175.7(3) . . . . ?
C5 C4 C9 C13 176.7(3) . . . . ?
N1 C4 C9 C13 1.9(5) . . . . ?
C7 C8 C9 C4 0.3(5) . . . . ?
C7 C8 C9 C13 -177.4(3) . . . . ?
C6 C5 C10 C11 19.5(5) . . . . ?
C4 C5 C10 C11 -164.6(3) . . . . ?
C6 C5 C10 C12 -103.5(4) . . . . ?
C4 C5 C10 C12 72.4(5) . . . . ?
C4 C9 C13 C15 -103.7(4) . . . . ?
C8 C9 C13 C15 73.9(5) . . . . ?
C4 C9 C13 C14 133.1(4) . . . . ?
C8 C9 C13 C14 -49.3(5) . . . . ?
C1 N2 C16 C17 -99.4(4) . . . . ?
C3 N2 C16 C17 87.1(4) . . . . ?
C1 N2 C16 C21 88.5(4) . . . . ?
C3 N2 C16 C21 -85.1(4) . . . . ?
C21 C16 C17 C18 1.4(5) . . . . ?
N2 C16 C17 C18 -170.2(3) . . . . ?
C21 C16 C17 C22 -179.8(4) . . . . ?
N2 C16 C17 C22 8.6(5) . . . . ?
C16 C17 C18 C19 -0.6(6) . . . . ?
C22 C17 C18 C19 -179.4(4) . . . . ?
C17 C18 C19 C20 -1.3(6) . . . . ?
C18 C19 C20 C21 2.5(6) . . . . ?
C17 C16 C21 C20 -0.3(5) . . . . ?
N2 C16 C21 C20 171.3(3) . . . . ?
C17 C16 C21 C25 -178.1(3) . . . . ?
N2 C16 C21 C25 -6.5(5) . . . . ?
C19 C20 C21 C16 -1.7(5) . . . . ?
C19 C20 C21 C25 176.2(3) . . . . ?
C16 C17 C22 C24 -100.7(5) . . . . ?
C18 C17 C22 C24 78.1(5) . . . . ?
C16 C17 C22 C23 136.5(4) . . . . ?
C18 C17 C22 C23 -44.7(5) . . . . ?
C16 C21 C25 C26 -132.0(4) . . . . ?
C20 C21 C25 C26 50.2(5) . . . . ?
C16 C21 C25 C27 103.5(4) . . . . ?
C20 C21 C25 C27 -74.3(4) . . . . ?
C29 N3 C28 N4 0.2(4) . . . . ?
C31 N3 C28 N4 -175.7(3) . . . . ?
C29 N3 C28 Ni1 -171.9(3) . . . . ?
C31 N3 C28 Ni1 12.2(6) . . . . ?
C30 N4 C28 N3 0.0(4) . . . . ?
C43 N4 C28 N3 -176.8(3) . . . . ?
C30 N4 C28 Ni1 172.5(3) . . . . ?
C43 N4 C28 Ni1 -4.3(5) . . . . ?
C1 Ni1 C28 N3 -117.2(7) . . . . ?
Cl1 Ni1 C28 N3 64.5(3) . . . . ?
C1 Ni1 C28 N4 72.4(8) . . . . ?
Cl1 Ni1 C28 N4 -105.8(3) . . . . ?
C28 N3 C29 C30 -0.2(5) . . . . ?
C31 N3 C29 C30 176.0(3) . . . . ?
N3 C29 C30 N4 0.2(5) . . . . ?
C28 N4 C30 C29 -0.1(5) . . . . ?
C43 N4 C30 C29 177.0(3) . . . . ?
C28 N3 C31 C36 -103.9(4) . . . . ?
C29 N3 C31 C36 80.5(4) . . . . ?
C28 N3 C31 C32 81.2(5) . . . . ?
C29 N3 C31 C32 -94.4(4) . . . . ?
C36 C31 C32 C33 2.6(5) . . . . ?
N3 C31 C32 C33 177.4(3) . . . . ?
C36 C31 C32 C37 -173.2(3) . . . . ?
N3 C31 C32 C37 1.6(5) . . . . ?
C31 C32 C33 C34 -0.6(6) . . . . ?
C37 C32 C33 C34 175.3(4) . . . . ?
C32 C33 C34 C35 -1.3(6) . . . . ?
C33 C34 C35 C36 1.3(6) . . . . ?
C32 C31 C36 C35 -2.6(5) . . . . ?
N3 C31 C36 C35 -177.3(3) . . . . ?
C32 C31 C36 C40 175.8(3) . . . . ?
N3 C31 C36 C40 1.1(5) . . . . ?
C34 C35 C36 C31 0.6(5) . . . . ?
C34 C35 C36 C40 -177.8(3) . . . . ?
C33 C32 C37 C39 65.0(5) . . . . ?
C31 C32 C37 C39 -119.4(4) . . . . ?
C33 C32 C37 C38 -58.8(5) . . . . ?
C31 C32 C37 C38 116.8(4) . . . . ?
C31 C36 C40 C42 141.2(4) . . . . ?
C35 C36 C40 C42 -40.5(5) . . . . ?
C31 C36 C40 C41 -95.1(4) . . . . ?
C35 C36 C40 C41 83.3(5) . . . . ?
C28 N4 C43 C48 -100.8(5) . . . . ?
C30 N4 C43 C48 82.6(5) . . . . ?
C28 N4 C43 C44 87.3(5) . . . . ?
C30 N4 C43 C44 -89.3(4) . . . . ?
C48 C43 C44 C45 0.5(5) . . . . ?
N4 C43 C44 C45 171.9(3) . . . . ?
C48 C43 C44 C49 -178.7(3) . . . . ?
N4 C43 C44 C49 -7.2(5) . . . . ?
C43 C44 C45 C46 -2.9(5) . . . . ?
C49 C44 C45 C46 176.2(3) . . . . ?
C44 C45 C46 C47 4.0(6) . . . . ?
C45 C46 C47 C48 -2.5(6) . . . . ?
C44 C43 C48 C47 0.8(6) . . . . ?
N4 C43 C48 C47 -170.5(3) . . . . ?
C44 C43 C48 C52 -176.5(3) . . . . ?
N4 C43 C48 C52 12.2(5) . . . . ?
C46 C47 C48 C43 0.2(6) . . . . ?
C46 C47 C48 C52 177.6(4) . . . . ?
C45 C44 C49 C51 -77.7(5) . . . . ?
C43 C44 C49 C51 101.4(4) . . . . ?
C45 C44 C49 C50 46.2(5) . . . . ?
C43 C44 C49 C50 -134.7(4) . . . . ?
C43 C48 C52 C54 99.7(6) . . . . ?
C47 C48 C52 C54 -77.5(6) . . . . ?
C43 C48 C52 C53 -134.8(5) . . . . ?
C47 C48 C52 C53 48.1(6) . . . . ?
C55 C56 C57 C58 -176.4(4) . . . . ?
C56 C57 C58 C59 -177.1(4) . . . . ?
C57 C58 C59 C60 175.3(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.075
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.078

#===END

data_2(THF)
_database_code_depnum_ccdc_archive 'CCDC 737687'
#TrackingRef 'Xray.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C62 H88 Cl N4 Ni O2'
_chemical_formula_weight         1015.52

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   'P 1 21/n 1'

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                   12.197(3)
_cell_length_b                   21.922(5)
_cell_length_c                   21.563(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.719(2)
_cell_angle_gamma                90.00
_cell_volume                     5763(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    13366
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2196
_exptl_absorpt_coefficient_mu    0.428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_T_max  0.996

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71070
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 7.31
_diffrn_reflns_number            45886
_diffrn_reflns_av_R_equivalents  0.0883
_diffrn_reflns_av_sigmaI/netI    0.0819
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         27.48
_reflns_number_total             13005
_reflns_number_gt                10089
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       CrystalClear
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_structure_solution    SIR2002
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP III (Farrujia, 1998)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0614P)^2^+7.5681P] where P=(Fo^2^+2Fc^2^)/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         13005
_refine_ls_number_parameters     632
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0754
_refine_ls_wR_factor_ref         0.1840
_refine_ls_wR_factor_gt          0.1698
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_restrained_S_all      1.116
_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 0.34149(3) 0.210664(17) 0.674215(17) 0.01561(11) Uani 1 1 d . . .
Cl1 Cl 0.25893(7) 0.13214(4) 0.72654(4) 0.0318(2) Uani 1 1 d . . .
O1 O -0.0850(3) 0.41472(14) 0.62049(16) 0.0624(10) Uani 1 1 d . . .
O2 O -0.3803(4) 0.6319(2) 0.6596(2) 0.0950(14) Uani 1 1 d . . .
N1 N 0.14600(19) 0.20816(11) 0.58548(11) 0.0157(5) Uani 1 1 d . . .
N2 N 0.1501(2) 0.28958(11) 0.64008(11) 0.0163(5) Uani 1 1 d . . .
N3 N 0.5273(2) 0.20389(11) 0.76943(11) 0.0176(5) Uani 1 1 d . . .
N4 N 0.5723(2) 0.16721(12) 0.68213(11) 0.0190(5) Uani 1 1 d . . .
C1 C 0.2101(2) 0.23812(13) 0.62901(13) 0.0154(6) Uani 1 1 d . . .
C2 C 0.0504(2) 0.24032(13) 0.57095(14) 0.0191(6) Uani 1 1 d . . .
H2 H -0.0060 0.2283 0.5421 0.023 Uiso 1 1 calc R . .
C3 C 0.0524(2) 0.29128(14) 0.60511(15) 0.0203(6) Uani 1 1 d . . .
H3 H -0.0018 0.3223 0.6054 0.024 Uiso 1 1 calc R . .
C4 C 0.1713(2) 0.15367(13) 0.55077(14) 0.0187(6) Uani 1 1 d . . .
C5 C 0.1153(3) 0.09963(14) 0.56371(14) 0.0209(6) Uani 1 1 d . . .
C6 C 0.1319(3) 0.04986(15) 0.52428(16) 0.0271(7) Uani 1 1 d . . .
H6 H 0.0948 0.0125 0.5315 0.032 Uiso 1 1 calc R . .
C7 C 0.2012(3) 0.05429(16) 0.47511(17) 0.0315(8) Uani 1 1 d . . .
H7 H 0.2115 0.0200 0.4490 0.038 Uiso 1 1 calc R . .
C8 C 0.2558(3) 0.10817(16) 0.46332(15) 0.0287(7) Uani 1 1 d . . .
H8 H 0.3039 0.1103 0.4296 0.034 Uiso 1 1 calc R . .
C9 C 0.2410(2) 0.15962(14) 0.50064(14) 0.0209(6) Uani 1 1 d . . .
C10 C 0.0370(3) 0.09384(15) 0.61668(15) 0.0247(7) Uani 1 1 d . . .
H10 H 0.0540 0.1273 0.6470 0.030 Uiso 1 1 calc R . .
C11 C -0.0823(3) 0.10146(17) 0.59364(18) 0.0329(8) Uani 1 1 d . . .
H11A H -0.1026 0.1447 0.5952 0.040 Uiso 1 1 calc R . .
H11B H -0.1305 0.0778 0.6202 0.040 Uiso 1 1 calc R . .
H11C H -0.0900 0.0867 0.5508 0.040 Uiso 1 1 calc R . .
C12 C 0.0506(3) 0.03277(17) 0.65079(19) 0.0400(9) Uani 1 1 d . . .
H12A H 0.0014 0.0024 0.6316 0.048 Uiso 1 1 calc R . .
H12B H 0.0325 0.0380 0.6944 0.048 Uiso 1 1 calc R . .
H12C H 0.1267 0.0188 0.6482 0.048 Uiso 1 1 calc R . .
C13 C 0.2943(3) 0.21988(15) 0.48450(15) 0.0233(7) Uani 1 1 d . . .
H13 H 0.3126 0.2417 0.5242 0.028 Uiso 1 1 calc R . .
C14 C 0.2149(3) 0.26005(18) 0.44650(19) 0.0389(9) Uani 1 1 d . . .
H14A H 0.2232 0.2517 0.4022 0.047 Uiso 1 1 calc R . .
H14B H 0.2313 0.3031 0.4549 0.047 Uiso 1 1 calc R . .
H14C H 0.1395 0.2511 0.4580 0.047 Uiso 1 1 calc R . .
C15 C 0.4004(3) 0.21220(19) 0.4493(2) 0.0431(10) Uani 1 1 d . . .
H15A H 0.4407 0.1767 0.4656 0.052 Uiso 1 1 calc R . .
H15B H 0.4457 0.2488 0.4547 0.052 Uiso 1 1 calc R . .
H15C H 0.3827 0.2061 0.4051 0.052 Uiso 1 1 calc R . .
C16 C 0.1818(2) 0.34111(13) 0.67773(14) 0.0183(6) Uani 1 1 d . . .
C17 C 0.2260(3) 0.39173(14) 0.64751(15) 0.0233(7) Uani 1 1 d . . .
C18 C 0.2445(3) 0.44428(15) 0.68265(17) 0.0277(7) Uani 1 1 d . . .
H18 H 0.2736 0.4794 0.6634 0.033 Uiso 1 1 calc R . .
C19 C 0.2215(3) 0.44629(16) 0.74429(17) 0.0323(8) Uani 1 1 d . . .
H19 H 0.2344 0.4828 0.7672 0.039 Uiso 1 1 calc R . .
C20 C 0.1795(3) 0.39541(16) 0.77376(16) 0.0279(7) Uani 1 1 d . . .
H20 H 0.1654 0.3973 0.8168 0.033 Uiso 1 1 calc R . .
C21 C 0.1576(2) 0.34142(14) 0.74091(14) 0.0207(6) Uani 1 1 d . . .
C22 C 0.2530(3) 0.39032(16) 0.57924(16) 0.0304(8) Uani 1 1 d . . .
H22 H 0.2289 0.3498 0.5624 0.036 Uiso 1 1 calc R . .
C23 C 0.1926(5) 0.4385(2) 0.5426(2) 0.0678(16) Uani 1 1 d . . .
H23A H 0.1222 0.4221 0.5272 0.081 Uiso 1 1 calc R . .
H23B H 0.2365 0.4510 0.5075 0.081 Uiso 1 1 calc R . .
H23C H 0.1797 0.4738 0.5693 0.081 Uiso 1 1 calc R . .
C24 C 0.3757(4) 0.3948(4) 0.5719(3) 0.108(3) Uani 1 1 d . . .
H24A H 0.3969 0.4377 0.5682 0.130 Uiso 1 1 calc R . .
H24B H 0.3963 0.3727 0.5344 0.130 Uiso 1 1 calc R . .
H24C H 0.4135 0.3767 0.6082 0.130 Uiso 1 1 calc R . .
C25 C 0.1034(3) 0.28724(16) 0.77075(15) 0.0257(7) Uani 1 1 d . . .
H25 H 0.1233 0.2499 0.7470 0.031 Uiso 1 1 calc R . .
C26 C 0.1405(3) 0.2780(2) 0.83830(18) 0.0422(10) Uani 1 1 d . . .
H26A H 0.2048 0.2511 0.8402 0.051 Uiso 1 1 calc R . .
H26B H 0.0809 0.2594 0.8612 0.051 Uiso 1 1 calc R . .
H26C H 0.1597 0.3175 0.8569 0.051 Uiso 1 1 calc R . .
C27 C -0.0226(3) 0.2944(2) 0.76675(19) 0.0411(10) Uani 1 1 d . . .
H27A H -0.0473 0.3160 0.8036 0.049 Uiso 1 1 calc R . .
H27B H -0.0568 0.2539 0.7647 0.049 Uiso 1 1 calc R . .
H27C H -0.0435 0.3177 0.7295 0.049 Uiso 1 1 calc R . .
C28 C 0.4885(2) 0.19741(13) 0.70944(13) 0.0166(6) Uani 1 1 d . . .
C29 C 0.6305(3) 0.17804(15) 0.77834(15) 0.0247(7) Uani 1 1 d . . .
H29 H 0.6731 0.1770 0.8159 0.030 Uiso 1 1 calc R . .
C30 C 0.6581(3) 0.15495(16) 0.72378(15) 0.0259(7) Uani 1 1 d . . .
H30 H 0.7242 0.1341 0.7151 0.031 Uiso 1 1 calc R . .
C31 C 0.4815(2) 0.24083(14) 0.81753(14) 0.0191(6) Uani 1 1 d . . .
C32 C 0.5019(3) 0.30409(14) 0.81593(15) 0.0229(7) Uani 1 1 d . . .
C33 C 0.4665(3) 0.33906(16) 0.86548(16) 0.0288(7) Uani 1 1 d . . .
H33 H 0.4781 0.3819 0.8653 0.035 Uiso 1 1 calc R . .
C34 C 0.4150(3) 0.31261(16) 0.91480(15) 0.0266(7) Uani 1 1 d . . .
H34 H 0.3909 0.3373 0.9480 0.032 Uiso 1 1 calc R . .
C35 C 0.3983(3) 0.24984(15) 0.91599(14) 0.0235(7) Uani 1 1 d . . .
H35 H 0.3640 0.2320 0.9505 0.028 Uiso 1 1 calc R . .
C36 C 0.4311(2) 0.21261(14) 0.86745(14) 0.0199(6) Uani 1 1 d . . .
C37 C 0.5655(3) 0.33359(16) 0.76468(16) 0.0294(7) Uani 1 1 d . . .
H37 H 0.5824 0.3014 0.7335 0.035 Uiso 1 1 calc R . .
C38 C 0.6734(4) 0.3600(4) 0.7892(3) 0.094(2) Uani 1 1 d . . .
H38A H 0.6625 0.4026 0.8014 0.113 Uiso 1 1 calc R . .
H38B H 0.7278 0.3581 0.7567 0.113 Uiso 1 1 calc R . .
H38C H 0.6997 0.3364 0.8252 0.113 Uiso 1 1 calc R . .
C39 C 0.5004(4) 0.3828(3) 0.7320(3) 0.0744(18) Uani 1 1 d . . .
H39A H 0.4579 0.3650 0.6973 0.089 Uiso 1 1 calc R . .
H39B H 0.5505 0.4137 0.7164 0.089 Uiso 1 1 calc R . .
H39C H 0.4505 0.4017 0.7611 0.089 Uiso 1 1 calc R . .
C40 C 0.4163(3) 0.14374(15) 0.87144(15) 0.0247(7) Uani 1 1 d . . .
H40 H 0.4303 0.1260 0.8297 0.030 Uiso 1 1 calc R . .
C41 C 0.4996(3) 0.11628(17) 0.91791(19) 0.0375(9) Uani 1 1 d . . .
H41A H 0.5730 0.1318 0.9094 0.045 Uiso 1 1 calc R . .
H41B H 0.4991 0.0717 0.9140 0.045 Uiso 1 1 calc R . .
H41C H 0.4801 0.1277 0.9601 0.045 Uiso 1 1 calc R . .
C42 C 0.3000(3) 0.12654(17) 0.88878(17) 0.0350(8) Uani 1 1 d . . .
H42A H 0.2960 0.1239 0.9340 0.042 Uiso 1 1 calc R . .
H42B H 0.2807 0.0870 0.8703 0.042 Uiso 1 1 calc R . .
H42C H 0.2486 0.1577 0.8732 0.042 Uiso 1 1 calc R . .
C43 C 0.5830(2) 0.15134(15) 0.61743(14) 0.0199(6) Uani 1 1 d . . .
C44 C 0.5601(3) 0.09154(15) 0.59892(14) 0.0214(6) Uani 1 1 d . . .
C45 C 0.5902(3) 0.07492(16) 0.53940(15) 0.0269(7) Uani 1 1 d . . .
H45 H 0.5756 0.0346 0.5253 0.032 Uiso 1 1 calc R . .
C46 C 0.6406(3) 0.11555(16) 0.50034(15) 0.0279(7) Uani 1 1 d . . .
H46 H 0.6632 0.1025 0.4607 0.033 Uiso 1 1 calc R . .
C47 C 0.6581(3) 0.17487(16) 0.51905(15) 0.0260(7) Uani 1 1 d . . .
H47 H 0.6904 0.2029 0.4914 0.031 Uiso 1 1 calc R . .
C48 C 0.6293(2) 0.19468(16) 0.57801(15) 0.0241(7) Uani 1 1 d . . .
C49 C 0.5019(3) 0.04629(15) 0.63951(15) 0.0249(7) Uani 1 1 d . . .
H49 H 0.4924 0.0655 0.6811 0.030 Uiso 1 1 calc R . .
C50 C 0.5684(4) -0.01222(19) 0.6488(2) 0.0465(11) Uani 1 1 d . . .
H50A H 0.5479 -0.0415 0.6162 0.056 Uiso 1 1 calc R . .
H50B H 0.5530 -0.0298 0.6894 0.056 Uiso 1 1 calc R . .
H50C H 0.6467 -0.0029 0.6469 0.056 Uiso 1 1 calc R . .
C51 C 0.3886(3) 0.03227(17) 0.61166(17) 0.0336(8) Uani 1 1 d . . .
H51A H 0.3510 0.0705 0.6008 0.040 Uiso 1 1 calc R . .
H51B H 0.3458 0.0099 0.6420 0.040 Uiso 1 1 calc R . .
H51C H 0.3959 0.0074 0.5742 0.040 Uiso 1 1 calc R . .
C52 C 0.6487(3) 0.26035(16) 0.59838(17) 0.0309(8) Uani 1 1 d . . .
H52 H 0.6004 0.2693 0.6339 0.037 Uiso 1 1 calc R . .
C53 C 0.7665(4) 0.2698(2) 0.6197(3) 0.0727(18) Uani 1 1 d . . .
H53A H 0.7740 0.2612 0.6643 0.087 Uiso 1 1 calc R . .
H53B H 0.7880 0.3121 0.6119 0.087 Uiso 1 1 calc R . .
H53C H 0.8139 0.2421 0.5970 0.087 Uiso 1 1 calc R . .
C54 C 0.6220(4) 0.30602(19) 0.5465(2) 0.0514(12) Uani 1 1 d . . .
H54A H 0.6879 0.3135 0.5227 0.062 Uiso 1 1 calc R . .
H54B H 0.5972 0.3444 0.5646 0.062 Uiso 1 1 calc R . .
H54C H 0.5639 0.2894 0.5190 0.062 Uiso 1 1 calc R . .
C55 C -0.1562(4) 0.4455(2) 0.5791(2) 0.0469(10) Uani 1 1 d . . .
H55A H -0.1949 0.4164 0.5510 0.056 Uiso 1 1 calc R . .
H55B H -0.1156 0.4752 0.5539 0.056 Uiso 1 1 calc R . .
C56 C -0.2353(5) 0.4774(3) 0.6198(3) 0.0751(17) Uani 1 1 d . . .
H56A H -0.2975 0.4505 0.6298 0.090 Uiso 1 1 calc R . .
H56B H -0.2642 0.5150 0.5997 0.090 Uiso 1 1 calc R . .
C57 C -0.1667(5) 0.4924(2) 0.6772(3) 0.0642(15) Uani 1 1 d . . .
H57A H -0.1447 0.5359 0.6774 0.077 Uiso 1 1 calc R . .
H57B H -0.2076 0.4838 0.7152 0.077 Uiso 1 1 calc R . .
C58 C -0.0686(5) 0.4516(2) 0.6732(3) 0.0695(16) Uani 1 1 d . . .
H58A H -0.0011 0.4763 0.6694 0.083 Uiso 1 1 calc R . .
H58B H -0.0609 0.4260 0.7109 0.083 Uiso 1 1 calc R . .
C59 C -0.4328(6) 0.6209(3) 0.6034(3) 0.082(2) Uani 1 1 d . . .
H59A H -0.3783 0.6104 0.5720 0.098 Uiso 1 1 calc R . .
H59B H -0.4726 0.6580 0.5893 0.098 Uiso 1 1 calc R . .
C60 C -0.5089(4) 0.5713(3) 0.6100(3) 0.0647(14) Uani 1 1 d . . .
H60A H -0.4807 0.5340 0.5901 0.078 Uiso 1 1 calc R . .
H60B H -0.5808 0.5817 0.5904 0.078 Uiso 1 1 calc R . .
C61 C -0.5198(4) 0.5616(2) 0.6784(2) 0.0573(13) Uani 1 1 d . . .
H61A H -0.5964 0.5680 0.6909 0.069 Uiso 1 1 calc R . .
H61B H -0.4964 0.5199 0.6906 0.069 Uiso 1 1 calc R . .
C62 C -0.4464(6) 0.6077(4) 0.7064(3) 0.108(3) Uani 1 1 d . . .
H62A H -0.4900 0.6406 0.7251 0.130 Uiso 1 1 calc R . .
H62B H -0.3996 0.5889 0.7394 0.130 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.01504(19) 0.0173(2) 0.01442(19) -0.00135(15) -0.00142(13) 0.00182(14)
Cl1 0.0295(4) 0.0366(5) 0.0290(4) 0.0110(4) -0.0059(3) -0.0102(4)
O1 0.082(2) 0.0416(17) 0.062(2) -0.0132(16) -0.0176(18) 0.0328(17)
O2 0.081(3) 0.105(3) 0.100(3) -0.001(3) 0.017(3) -0.048(3)
N1 0.0163(11) 0.0159(12) 0.0148(12) -0.0011(10) -0.0029(9) 0.0019(9)
N2 0.0158(11) 0.0161(12) 0.0169(12) -0.0015(10) -0.0028(9) 0.0010(9)
N3 0.0168(12) 0.0194(13) 0.0163(12) -0.0039(10) -0.0024(9) 0.0040(10)
N4 0.0171(12) 0.0242(14) 0.0156(12) -0.0045(10) -0.0019(9) 0.0034(10)
C1 0.0192(14) 0.0128(14) 0.0141(13) 0.0000(11) 0.0020(11) -0.0013(11)
C2 0.0194(14) 0.0164(15) 0.0210(15) -0.0022(12) -0.0058(12) 0.0016(12)
C3 0.0183(14) 0.0180(15) 0.0241(16) 0.0006(13) -0.0057(12) 0.0030(12)
C4 0.0220(15) 0.0159(14) 0.0177(14) -0.0037(12) -0.0059(11) 0.0003(12)
C5 0.0233(15) 0.0172(15) 0.0218(15) -0.0006(12) -0.0061(12) 0.0003(12)
C6 0.0279(17) 0.0216(17) 0.0312(18) -0.0083(14) -0.0058(14) -0.0007(13)
C7 0.038(2) 0.0243(18) 0.0320(19) -0.0140(15) -0.0006(15) 0.0031(15)
C8 0.0302(17) 0.0336(19) 0.0223(17) -0.0083(14) 0.0022(13) 0.0050(15)
C9 0.0194(14) 0.0243(16) 0.0188(15) -0.0033(13) -0.0032(11) 0.0034(12)
C10 0.0276(17) 0.0193(16) 0.0271(17) -0.0021(13) 0.0006(13) -0.0048(13)
C11 0.0286(18) 0.0273(18) 0.043(2) 0.0006(16) 0.0020(15) -0.0031(14)
C12 0.046(2) 0.032(2) 0.042(2) 0.0108(17) -0.0024(18) -0.0011(17)
C13 0.0223(15) 0.0275(17) 0.0200(15) 0.0001(13) 0.0007(12) 0.0013(13)
C14 0.0321(19) 0.040(2) 0.045(2) 0.0162(18) 0.0001(17) -0.0027(17)
C15 0.0270(19) 0.047(2) 0.056(3) 0.001(2) 0.0083(18) -0.0005(17)
C16 0.0180(14) 0.0155(14) 0.0213(15) -0.0071(12) -0.0035(11) 0.0013(11)
C17 0.0222(15) 0.0199(16) 0.0275(17) -0.0014(13) -0.0013(13) -0.0002(12)
C18 0.0270(17) 0.0204(16) 0.0356(19) -0.0011(14) -0.0020(14) -0.0029(13)
C19 0.0341(19) 0.0245(18) 0.038(2) -0.0166(16) -0.0059(15) -0.0018(14)
C20 0.0308(17) 0.0299(18) 0.0226(16) -0.0111(14) -0.0027(13) 0.0030(14)
C21 0.0175(14) 0.0230(16) 0.0216(15) -0.0076(13) -0.0008(11) 0.0023(12)
C22 0.040(2) 0.0248(18) 0.0267(18) 0.0018(14) 0.0032(15) -0.0046(15)
C23 0.119(5) 0.051(3) 0.032(2) 0.001(2) -0.017(3) 0.018(3)
C24 0.049(3) 0.231(9) 0.046(3) 0.013(4) 0.022(3) -0.012(4)
C25 0.0278(17) 0.0300(18) 0.0196(16) 0.0001(14) 0.0024(13) 0.0037(14)
C26 0.036(2) 0.057(3) 0.033(2) 0.0133(19) -0.0029(16) 0.0037(18)
C27 0.031(2) 0.055(3) 0.037(2) 0.0101(19) -0.0031(16) -0.0113(18)
C28 0.0170(14) 0.0161(14) 0.0169(14) -0.0008(11) 0.0020(11) 0.0005(11)
C29 0.0224(16) 0.0274(17) 0.0238(16) -0.0042(13) -0.0072(12) 0.0072(13)
C30 0.0213(15) 0.0302(18) 0.0260(17) -0.0054(14) -0.0044(13) 0.0089(13)
C31 0.0177(14) 0.0222(16) 0.0173(14) -0.0028(12) -0.0027(11) 0.0021(12)
C32 0.0275(16) 0.0201(16) 0.0210(15) -0.0022(13) 0.0000(13) 0.0021(13)
C33 0.0334(18) 0.0237(17) 0.0293(18) -0.0051(14) 0.0000(14) 0.0038(14)
C34 0.0302(17) 0.0277(17) 0.0216(16) -0.0087(14) -0.0015(13) 0.0044(14)
C35 0.0233(16) 0.0310(18) 0.0160(15) -0.0036(13) -0.0013(12) 0.0019(13)
C36 0.0179(14) 0.0231(16) 0.0185(15) -0.0024(12) -0.0043(11) 0.0019(12)
C37 0.039(2) 0.0239(17) 0.0259(17) -0.0020(14) 0.0050(15) -0.0004(15)
C38 0.048(3) 0.170(7) 0.064(4) 0.051(4) -0.010(3) -0.042(4)
C39 0.057(3) 0.100(4) 0.067(3) 0.056(3) 0.018(3) 0.028(3)
C40 0.0326(18) 0.0219(16) 0.0196(16) -0.0021(13) -0.0005(13) -0.0005(13)
C41 0.043(2) 0.0273(19) 0.041(2) 0.0047(17) -0.0092(17) 0.0044(16)
C42 0.044(2) 0.0296(19) 0.0316(19) -0.0005(16) 0.0043(16) -0.0107(16)
C43 0.0144(13) 0.0292(17) 0.0163(14) -0.0039(13) 0.0026(11) 0.0061(12)
C44 0.0222(15) 0.0234(16) 0.0187(15) -0.0019(13) 0.0006(12) 0.0060(12)
C45 0.0320(18) 0.0277(18) 0.0212(16) -0.0052(14) 0.0051(13) 0.0016(14)
C46 0.0286(17) 0.037(2) 0.0183(16) -0.0033(14) 0.0066(13) 0.0060(15)
C47 0.0247(16) 0.0311(18) 0.0224(16) -0.0005(14) 0.0053(13) -0.0005(14)
C48 0.0160(14) 0.0327(18) 0.0236(16) -0.0020(14) 0.0015(12) 0.0020(13)
C49 0.0355(18) 0.0216(16) 0.0177(15) -0.0019(13) 0.0050(13) 0.0024(14)
C50 0.050(2) 0.040(2) 0.051(3) 0.020(2) 0.012(2) 0.0159(19)
C51 0.039(2) 0.034(2) 0.0281(18) 0.0004(16) 0.0034(15) -0.0051(16)
C52 0.0296(18) 0.0296(19) 0.0340(19) -0.0031(15) 0.0089(15) -0.0079(15)
C53 0.050(3) 0.036(2) 0.129(5) 0.000(3) -0.039(3) -0.012(2)
C54 0.076(3) 0.029(2) 0.050(3) 0.0004(19) 0.004(2) 0.000(2)
C55 0.045(2) 0.048(3) 0.048(3) 0.003(2) -0.003(2) 0.005(2)
C56 0.059(3) 0.103(5) 0.064(3) 0.027(3) 0.011(3) 0.033(3)
C57 0.086(4) 0.041(3) 0.067(3) -0.001(2) 0.024(3) 0.010(3)
C58 0.086(4) 0.060(3) 0.061(3) -0.011(3) -0.026(3) 0.030(3)
C59 0.122(5) 0.073(4) 0.050(3) 0.008(3) 0.010(3) -0.050(4)
C60 0.044(3) 0.083(4) 0.067(3) -0.023(3) 0.002(2) 0.002(3)
C61 0.051(3) 0.044(3) 0.078(4) 0.002(2) 0.011(2) -0.013(2)
C62 0.135(6) 0.129(6) 0.060(4) 0.011(4) -0.002(4) -0.100(5)

_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 C1 1.947(3) . ?
Ni1 C28 1.948(3) . ?
Ni1 Cl1 2.3062(10) . ?
O1 C55 1.399(5) . ?
O1 C58 1.404(6) . ?
O2 C59 1.375(7) . ?
O2 C62 1.413(7) . ?
N1 C1 1.371(4) . ?
N1 C2 1.391(4) . ?
N1 C4 1.448(4) . ?
N2 C1 1.369(4) . ?
N2 C3 1.391(4) . ?
N2 C16 1.437(4) . ?
N3 C28 1.371(4) . ?
N3 C29 1.389(4) . ?
N3 C31 1.441(4) . ?
N4 C28 1.365(4) . ?
N4 C30 1.386(4) . ?
N4 C43 1.447(4) . ?
C2 C3 1.338(4) . ?
C4 C5 1.399(4) . ?
C4 C9 1.401(4) . ?
C5 C6 1.401(4) . ?
C5 C10 1.516(4) . ?
C6 C7 1.379(5) . ?
C7 C8 1.384(5) . ?
C8 C9 1.400(4) . ?
C9 C13 1.517(5) . ?
C10 C11 1.533(5) . ?
C10 C12 1.534(5) . ?
C13 C14 1.528(5) . ?
C13 C15 1.529(5) . ?
C16 C17 1.402(4) . ?
C16 C21 1.403(4) . ?
C17 C18 1.394(5) . ?
C17 C22 1.519(5) . ?
C18 C19 1.367(5) . ?
C19 C20 1.389(5) . ?
C20 C21 1.401(4) . ?
C21 C25 1.513(5) . ?
C22 C23 1.498(6) . ?
C22 C24 1.513(6) . ?
C25 C26 1.526(5) . ?
C25 C27 1.544(5) . ?
C29 C30 1.333(5) . ?
C31 C36 1.400(4) . ?
C31 C32 1.409(4) . ?
C32 C33 1.394(4) . ?
C32 C37 1.514(5) . ?
C33 C34 1.379(5) . ?
C34 C35 1.391(5) . ?
C35 C36 1.395(4) . ?
C36 C40 1.523(4) . ?
C37 C39 1.501(6) . ?
C37 C38 1.519(6) . ?
C40 C42 1.525(5) . ?
C40 C41 1.529(5) . ?
C43 C44 1.396(4) . ?
C43 C48 1.404(5) . ?
C44 C45 1.394(4) . ?
C44 C49 1.514(4) . ?
C45 C46 1.383(5) . ?
C46 C47 1.376(5) . ?
C47 C48 1.398(4) . ?
C48 C52 1.522(5) . ?
C49 C51 1.522(5) . ?
C49 C50 1.528(5) . ?
C52 C53 1.510(6) . ?
C52 C54 1.528(6) . ?
C55 C56 1.497(7) . ?
C56 C57 1.510(8) . ?
C57 C58 1.499(7) . ?
C59 C60 1.440(7) . ?
C60 C61 1.501(7) . ?
C61 C62 1.467(7) . ?

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
C1 Ni1 C28 167.42(12) . . ?
C1 Ni1 Cl1 96.35(9) . . ?
C28 Ni1 Cl1 96.22(9) . . ?
C55 O1 C58 108.0(3) . . ?
C59 O2 C62 107.5(4) . . ?
C1 N1 C2 111.6(2) . . ?
C1 N1 C4 128.6(2) . . ?
C2 N1 C4 119.5(2) . . ?
C1 N2 C3 112.4(2) . . ?
C1 N2 C16 127.5(2) . . ?
C3 N2 C16 119.8(2) . . ?
C28 N3 C29 111.9(2) . . ?
C28 N3 C31 127.4(2) . . ?
C29 N3 C31 119.9(2) . . ?
C28 N4 C30 112.0(3) . . ?
C28 N4 C43 128.5(2) . . ?
C30 N4 C43 119.3(2) . . ?
N2 C1 N1 102.6(2) . . ?
N2 C1 Ni1 127.1(2) . . ?
N1 C1 Ni1 129.7(2) . . ?
C3 C2 N1 107.3(3) . . ?
C2 C3 N2 106.1(3) . . ?
C5 C4 C9 122.9(3) . . ?
C5 C4 N1 118.9(3) . . ?
C9 C4 N1 117.8(3) . . ?
C4 C5 C6 117.3(3) . . ?
C4 C5 C10 122.9(3) . . ?
C6 C5 C10 119.8(3) . . ?
C7 C6 C5 120.9(3) . . ?
C6 C7 C8 120.7(3) . . ?
C7 C8 C9 120.7(3) . . ?
C8 C9 C4 117.4(3) . . ?
C8 C9 C13 120.4(3) . . ?
C4 C9 C13 122.1(3) . . ?
C5 C10 C11 111.1(3) . . ?
C5 C10 C12 111.9(3) . . ?
C11 C10 C12 109.8(3) . . ?
C9 C13 C14 110.9(3) . . ?
C9 C13 C15 113.1(3) . . ?
C14 C13 C15 109.2(3) . . ?
C17 C16 C21 122.8(3) . . ?
C17 C16 N2 117.4(3) . . ?
C21 C16 N2 119.4(3) . . ?
C18 C17 C16 117.4(3) . . ?
C18 C17 C22 120.5(3) . . ?
C16 C17 C22 122.1(3) . . ?
C19 C18 C17 121.4(3) . . ?
C18 C19 C20 120.5(3) . . ?
C19 C20 C21 121.0(3) . . ?
C20 C21 C16 116.9(3) . . ?
C20 C21 C25 121.8(3) . . ?
C16 C21 C25 121.1(3) . . ?
C23 C22 C24 111.8(5) . . ?
C23 C22 C17 112.2(3) . . ?
C24 C22 C17 110.2(3) . . ?
C21 C25 C26 112.9(3) . . ?
C21 C25 C27 110.1(3) . . ?
C26 C25 C27 109.5(3) . . ?
N4 C28 N3 102.5(2) . . ?
N4 C28 Ni1 126.6(2) . . ?
N3 C28 Ni1 129.7(2) . . ?
C30 C29 N3 106.5(3) . . ?
C29 C30 N4 107.0(3) . . ?
C36 C31 C32 122.4(3) . . ?
C36 C31 N3 119.6(3) . . ?
C32 C31 N3 117.6(3) . . ?
C33 C32 C31 117.6(3) . . ?
C33 C32 C37 120.1(3) . . ?
C31 C32 C37 122.2(3) . . ?
C34 C33 C32 121.2(3) . . ?
C33 C34 C35 120.0(3) . . ?
C34 C35 C36 121.3(3) . . ?
C35 C36 C31 117.4(3) . . ?
C35 C36 C40 120.0(3) . . ?
C31 C36 C40 122.5(3) . . ?
C39 C37 C32 112.0(3) . . ?
C39 C37 C38 109.3(4) . . ?
C32 C37 C38 111.5(3) . . ?
C36 C40 C42 111.8(3) . . ?
C36 C40 C41 110.5(3) . . ?
C42 C40 C41 110.3(3) . . ?
C44 C43 C48 122.9(3) . . ?
C44 C43 N4 118.6(3) . . ?
C48 C43 N4 118.1(3) . . ?
C45 C44 C43 116.9(3) . . ?
C45 C44 C49 120.1(3) . . ?
C43 C44 C49 122.9(3) . . ?
C46 C45 C44 121.8(3) . . ?
C47 C46 C45 119.9(3) . . ?
C46 C47 C48 121.3(3) . . ?
C47 C48 C43 117.2(3) . . ?
C47 C48 C52 121.0(3) . . ?
C43 C48 C52 121.8(3) . . ?
C44 C49 C51 109.9(3) . . ?
C44 C49 C50 111.7(3) . . ?
C51 C49 C50 110.8(3) . . ?
C53 C52 C48 110.9(3) . . ?
C53 C52 C54 108.3(4) . . ?
C48 C52 C54 112.4(3) . . ?
O1 C55 C56 104.6(4) . . ?
C55 C56 C57 103.3(4) . . ?
C58 C57 C56 104.3(4) . . ?
O1 C58 C57 107.2(4) . . ?
O2 C59 C60 109.3(5) . . ?
C59 C60 C61 106.3(4) . . ?
C62 C61 C60 103.5(4) . . ?
O2 C62 C61 108.8(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
C3 N2 C1 N1 0.4(3) . . . . ?
C16 N2 C1 N1 -173.7(3) . . . . ?
C3 N2 C1 Ni1 -171.4(2) . . . . ?
C16 N2 C1 Ni1 14.6(4) . . . . ?
C2 N1 C1 N2 -0.2(3) . . . . ?
C4 N1 C1 N2 173.0(3) . . . . ?
C2 N1 C1 Ni1 171.2(2) . . . . ?
C4 N1 C1 Ni1 -15.6(4) . . . . ?
C28 Ni1 C1 N2 -75.3(6) . . . . ?
Cl1 Ni1 C1 N2 106.1(2) . . . . ?
C28 Ni1 C1 N1 115.2(5) . . . . ?
Cl1 Ni1 C1 N1 -63.5(3) . . . . ?
C1 N1 C2 C3 0.0(3) . . . . ?
C4 N1 C2 C3 -173.9(3) . . . . ?
N1 C2 C3 N2 0.2(3) . . . . ?
C1 N2 C3 C2 -0.4(4) . . . . ?
C16 N2 C3 C2 174.2(3) . . . . ?
C1 N1 C4 C5 110.5(3) . . . . ?
C2 N1 C4 C5 -76.8(4) . . . . ?
C1 N1 C4 C9 -77.2(4) . . . . ?
C2 N1 C4 C9 95.5(3) . . . . ?
C9 C4 C5 C6 0.5(5) . . . . ?
N1 C4 C5 C6 172.3(3) . . . . ?
C9 C4 C5 C10 -177.9(3) . . . . ?
N1 C4 C5 C10 -6.0(4) . . . . ?
C4 C5 C6 C7 0.4(5) . . . . ?
C10 C5 C6 C7 178.8(3) . . . . ?
C5 C6 C7 C8 -0.3(5) . . . . ?
C6 C7 C8 C9 -0.8(5) . . . . ?
C7 C8 C9 C4 1.6(5) . . . . ?
C7 C8 C9 C13 -175.3(3) . . . . ?
C5 C4 C9 C8 -1.4(5) . . . . ?
N1 C4 C9 C8 -173.4(3) . . . . ?
C5 C4 C9 C13 175.3(3) . . . . ?
N1 C4 C9 C13 3.4(4) . . . . ?
C4 C5 C10 C11 98.2(4) . . . . ?
C6 C5 C10 C11 -80.1(4) . . . . ?
C4 C5 C10 C12 -138.7(3) . . . . ?
C6 C5 C10 C12 43.0(4) . . . . ?
C8 C9 C13 C14 94.7(4) . . . . ?
C4 C9 C13 C14 -81.9(4) . . . . ?
C8 C9 C13 C15 -28.3(4) . . . . ?
C4 C9 C13 C15 155.0(3) . . . . ?
C1 N2 C16 C17 96.2(4) . . . . ?
C3 N2 C16 C17 -77.4(4) . . . . ?
C1 N2 C16 C21 -90.2(4) . . . . ?
C3 N2 C16 C21 96.1(3) . . . . ?
C21 C16 C17 C18 -0.8(5) . . . . ?
N2 C16 C17 C18 172.5(3) . . . . ?
C21 C16 C17 C22 179.2(3) . . . . ?
N2 C16 C17 C22 -7.5(4) . . . . ?
C16 C17 C18 C19 0.6(5) . . . . ?
C22 C17 C18 C19 -179.4(3) . . . . ?
C17 C18 C19 C20 0.4(5) . . . . ?
C18 C19 C20 C21 -1.3(5) . . . . ?
C19 C20 C21 C16 1.0(5) . . . . ?
C19 C20 C21 C25 -175.0(3) . . . . ?
C17 C16 C21 C20 0.0(5) . . . . ?
N2 C16 C21 C20 -173.2(3) . . . . ?
C17 C16 C21 C25 176.1(3) . . . . ?
N2 C16 C21 C25 2.9(4) . . . . ?
C18 C17 C22 C23 -58.3(5) . . . . ?
C16 C17 C22 C23 121.6(4) . . . . ?
C18 C17 C22 C24 67.0(5) . . . . ?
C16 C17 C22 C24 -113.0(5) . . . . ?
C20 C21 C25 C26 -37.3(4) . . . . ?
C16 C21 C25 C26 146.9(3) . . . . ?
C20 C21 C25 C27 85.4(4) . . . . ?
C16 C21 C25 C27 -90.5(4) . . . . ?
C30 N4 C28 N3 0.8(3) . . . . ?
C43 N4 C28 N3 -174.9(3) . . . . ?
C30 N4 C28 Ni1 -167.7(2) . . . . ?
C43 N4 C28 Ni1 16.7(4) . . . . ?
C29 N3 C28 N4 -0.5(3) . . . . ?
C31 N3 C28 N4 169.3(3) . . . . ?
C29 N3 C28 Ni1 167.4(2) . . . . ?
C31 N3 C28 Ni1 -22.8(4) . . . . ?
C1 Ni1 C28 N4 -79.4(6) . . . . ?
Cl1 Ni1 C28 N4 99.2(3) . . . . ?
C1 Ni1 C28 N3 115.3(5) . . . . ?
Cl1 Ni1 C28 N3 -66.0(3) . . . . ?
C28 N3 C29 C30 0.1(4) . . . . ?
C31 N3 C29 C30 -170.6(3) . . . . ?
N3 C29 C30 N4 0.4(4) . . . . ?
C28 N4 C30 C29 -0.8(4) . . . . ?
C43 N4 C30 C29 175.3(3) . . . . ?
C28 N3 C31 C36 109.7(3) . . . . ?
C29 N3 C31 C36 -81.2(4) . . . . ?
C28 N3 C31 C32 -78.0(4) . . . . ?
C29 N3 C31 C32 91.0(4) . . . . ?
C36 C31 C32 C33 -2.2(5) . . . . ?
N3 C31 C32 C33 -174.2(3) . . . . ?
C36 C31 C32 C37 174.4(3) . . . . ?
N3 C31 C32 C37 2.3(4) . . . . ?
C31 C32 C33 C34 1.0(5) . . . . ?
C37 C32 C33 C34 -175.6(3) . . . . ?
C32 C33 C34 C35 0.6(5) . . . . ?
C33 C34 C35 C36 -1.1(5) . . . . ?
C34 C35 C36 C31 0.1(4) . . . . ?
C34 C35 C36 C40 177.3(3) . . . . ?
C32 C31 C36 C35 1.6(4) . . . . ?
N3 C31 C36 C35 173.5(3) . . . . ?
C32 C31 C36 C40 -175.6(3) . . . . ?
N3 C31 C36 C40 -3.7(4) . . . . ?
C33 C32 C37 C39 -60.6(5) . . . . ?
C31 C32 C37 C39 123.0(4) . . . . ?
C33 C32 C37 C38 62.2(5) . . . . ?
C31 C32 C37 C38 -114.2(5) . . . . ?
C35 C36 C40 C42 50.2(4) . . . . ?
C31 C36 C40 C42 -132.7(3) . . . . ?
C35 C36 C40 C41 -73.0(4) . . . . ?
C31 C36 C40 C41 104.0(3) . . . . ?
C28 N4 C43 C44 -101.3(4) . . . . ?
C30 N4 C43 C44 83.3(4) . . . . ?
C28 N4 C43 C48 86.6(4) . . . . ?
C30 N4 C43 C48 -88.8(4) . . . . ?
C48 C43 C44 C45 3.0(5) . . . . ?
N4 C43 C44 C45 -168.6(3) . . . . ?
C48 C43 C44 C49 -174.9(3) . . . . ?
N4 C43 C44 C49 13.5(4) . . . . ?
C43 C44 C45 C46 0.1(5) . . . . ?
C49 C44 C45 C46 178.1(3) . . . . ?
C44 C45 C46 C47 -2.7(5) . . . . ?
C45 C46 C47 C48 2.3(5) . . . . ?
C46 C47 C48 C43 0.7(5) . . . . ?
C46 C47 C48 C52 -179.9(3) . . . . ?
C44 C43 C48 C47 -3.5(5) . . . . ?
N4 C43 C48 C47 168.2(3) . . . . ?
C44 C43 C48 C52 177.2(3) . . . . ?
N4 C43 C48 C52 -11.1(4) . . . . ?
C45 C44 C49 C51 -66.4(4) . . . . ?
C43 C44 C49 C51 111.5(3) . . . . ?
C45 C44 C49 C50 57.0(4) . . . . ?
C43 C44 C49 C50 -125.1(4) . . . . ?
C47 C48 C52 C53 -80.9(5) . . . . ?
C43 C48 C52 C53 98.4(4) . . . . ?
C47 C48 C52 C54 40.4(5) . . . . ?
C43 C48 C52 C54 -140.3(3) . . . . ?
C58 O1 C55 C56 -36.3(6) . . . . ?
O1 C55 C56 C57 32.5(5) . . . . ?
C55 C56 C57 C58 -17.3(6) . . . . ?
C55 O1 C58 C57 25.0(6) . . . . ?
C56 C57 C58 O1 -3.4(6) . . . . ?
C62 O2 C59 C60 -21.5(8) . . . . ?
O2 C59 C60 C61 13.3(7) . . . . ?
C59 C60 C61 C62 -0.3(7) . . . . ?
C59 O2 C62 C61 21.3(8) . . . . ?
C60 C61 C62 O2 -12.4(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.080

#===END