Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Euan Brechin'
_publ_contact_author_email       EBRECHIN@STAFFMAIL.ED.AC.UK

_publ_section_title              
;
Using pyridine amidoximes in 3d-metal cluster
chemistry: a novel ferromagnetic Ni12 complex from the use of
pyridine-2-amidoxime
;
loop_
_publ_author_name
'Euan Brechin'
'Filipe A. Almeida Paz'
'Luis Cunha-Silva'
'Marco Evangelisti'
'Leigh F Jones'
;
N.Matamoros-Salvador
;
'Tuyen D Nguyen'
'Constantina Papatriantafyllopoulou'
'Spyros Perlepes'
;
J.Rocha
;

data_1
_database_code_depnum_ccdc_archive 'CCDC 678537'

# =======================================================================

_audit_creation_method           'SHELXL-97, manual editing plus enCIFer'
_audit_creation_date             '09 january 2008'

# =======================================================================

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C74 H74 C12 N36 Ni12 O14, 5(C H4 O), 4(Cl)'
_chemical_formula_sum            'C79 H94 Cl6 N36 Ni12 O19'
_chemical_formula_weight         2769.12

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'
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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.8718(8)
_cell_length_b                   15.1738(7)
_cell_length_c                   15.3809(8)
_cell_angle_alpha                60.525(2)
_cell_angle_beta                 73.084(3)
_cell_angle_gamma                69.854(2)
_cell_volume                     2805.3(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9871
_cell_measurement_theta_min      2.72
_cell_measurement_theta_max      29.77

_exptl_crystal_description       Prism
_exptl_crystal_colour            Brown
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1410
_exptl_absorpt_coefficient_mu    2.182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6695
_exptl_absorpt_correction_T_max  0.8279
_exptl_absorpt_process_details   
;
SADABS (Sheldrick, 1997)
;

_exptl_special_details           
;
See details in the main paper
;

_diffrn_ambient_temperature      150(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 X8 Kappa CCD APEX II'
_diffrn_measurement_method       'omega/phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            147901
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.52
_diffrn_reflns_theta_max         29.13
_reflns_number_total             14885
_reflns_number_gt                11216
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_cell_refinement       'APEX2 '
_computing_data_reduction        'SAINT+ (Bruker, 1997-2005)'
_computing_structure_solution    'SHELXTL (Bruker 2001)'
_computing_structure_refinement  'SHELXTL '
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'SHELXTL '

_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^)+(0.1196P)^2^+18.5443P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14885
_refine_ls_number_parameters     721
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0596
_refine_ls_wR_factor_ref         0.2210
_refine_ls_wR_factor_gt          0.2006
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.07120(4) -0.05698(4) 0.40077(4) 0.01192(14) Uani 1 1 d . . .
Ni2 Ni 0.01048(4) 0.09888(5) 0.18347(5) 0.01454(14) Uani 1 1 d . . .
Ni3 Ni -0.13070(4) 0.20394(4) 0.38310(4) 0.01386(14) Uani 1 1 d . . .
Ni4 Ni 0.16182(4) 0.14813(4) 0.30909(4) 0.01234(14) Uani 1 1 d . . .
Ni5 Ni 0.08173(5) 0.31930(5) 0.07836(5) 0.01620(15) Uani 1 1 d . . .
Ni6 Ni -0.22934(4) 0.00972(5) 0.46416(5) 0.01419(14) Uani 1 1 d . . .
Cl1 Cl -0.15314(11) 0.20332(12) 0.11900(11) 0.0330(3) Uani 1 1 d . . .
O1 O 0.2015(2) -0.1439(3) 0.4714(2) 0.0145(6) Uani 1 1 d . . .
O2 O 0.1386(2) 0.0023(3) 0.2562(2) 0.0147(6) Uani 1 1 d . . .
O3 O 0.0908(3) 0.1465(3) 0.0470(3) 0.0198(7) Uani 1 1 d . . .
O4 O 0.0657(2) 0.0817(2) 0.3936(2) 0.0130(6) Uani 1 1 d . . .
O5 O 0.0104(3) 0.2316(3) 0.1821(3) 0.0174(7) Uani 1 1 d . . .
O6 O -0.1232(2) 0.0627(3) 0.3943(3) 0.0154(6) Uani 1 1 d . . .
O1M O -0.2490(3) 0.2613(3) 0.3044(3) 0.0311(9) Uani 1 1 d D . .
H1M H -0.218(5) 0.233(6) 0.257(5) 0.047 Uiso 1 1 d D . .
N1 N 0.3432(3) 0.0333(3) 0.4562(3) 0.0190(8) Uani 1 1 d . . .
N2 N 0.2583(3) -0.0846(3) 0.4623(3) 0.0159(8) Uani 1 1 d . . .
N3 N 0.3726(3) -0.1410(4) 0.3474(4) 0.0227(9) Uani 1 1 d D . .
H3A H 0.333(4) -0.178(5) 0.354(4) 0.034 Uiso 1 1 d D . .
H3B H 0.413(4) -0.124(5) 0.288(3) 0.034 Uiso 1 1 d D . .
N4 N 0.2687(3) 0.2007(3) 0.2179(3) 0.0169(8) Uani 1 1 d . . .
N5 N 0.1926(3) 0.0674(3) 0.2403(3) 0.0135(7) Uani 1 1 d . . .
N6 N 0.2988(3) 0.0219(3) 0.1138(3) 0.0196(8) Uani 1 1 d D . .
H6A H 0.266(3) -0.027(3) 0.136(5) 0.029 Uiso 1 1 d D . .
H6B H 0.3620(13) 0.001(4) 0.092(5) 0.029 Uiso 1 1 d D . .
N7 N 0.1729(3) 0.3895(3) -0.0238(3) 0.0212(9) Uani 1 1 d . . .
N8 N 0.1266(3) 0.2282(3) 0.0191(3) 0.0175(8) Uani 1 1 d . . .
N9 N 0.2334(3) 0.1899(4) -0.1116(4) 0.0246(9) Uani 1 1 d D . .
H9A H 0.207(4) 0.135(3) -0.081(5) 0.037 Uiso 1 1 d D . .
H9B H 0.2983(9) 0.172(4) -0.125(5) 0.037 Uiso 1 1 d D . .
N10 N -0.0755(3) 0.1954(3) 0.5951(3) 0.0151(8) Uani 1 1 d . . .
N11 N 0.0038(3) 0.1281(3) 0.4568(3) 0.0133(7) Uani 1 1 d . . .
N12 N 0.1186(3) 0.2255(3) 0.3834(3) 0.0163(8) Uani 1 1 d D . .
H12A H 0.144(4) 0.270(4) 0.385(5) 0.024 Uiso 1 1 d D . .
N13 N -0.1544(3) 0.3524(3) 0.3709(3) 0.0163(8) Uani 1 1 d . . .
N14 N -0.0509(3) 0.2714(3) 0.2489(3) 0.0152(8) Uani 1 1 d . . .
N15 N 0.0229(3) 0.4066(3) 0.1410(3) 0.0205(9) Uani 1 1 d D . .
H15A H 0.023(5) 0.469(2) 0.133(5) 0.031 Uiso 1 1 d D . .
N16 N 0.0039(3) -0.0279(3) 0.1740(3) 0.0169(8) Uani 1 1 d . . .
N17 N -0.0651(3) 0.0217(3) 0.3257(3) 0.0145(8) Uani 1 1 d . . .
N18 N -0.1919(3) -0.0575(3) 0.3821(3) 0.0180(8) Uani 1 1 d D . .
H18A H -0.225(4) -0.107(4) 0.410(5) 0.027 Uiso 1 1 d D . .
C1 C 0.3785(4) 0.1052(4) 0.4543(5) 0.0261(11) Uani 1 1 d . . .
H1 H 0.3467 0.1362 0.4993 0.031 Uiso 1 1 calc R . .
C2 C 0.4603(5) 0.1346(5) 0.3882(5) 0.0349(14) Uani 1 1 d . . .
H2 H 0.4829 0.1870 0.3863 0.042 Uiso 1 1 calc R . .
C3 C 0.5088(4) 0.0867(5) 0.3246(5) 0.0353(14) Uani 1 1 d . . .
H3 H 0.5661 0.1046 0.2804 0.042 Uiso 1 1 calc R . .
C4 C 0.4731(4) 0.0123(4) 0.3260(4) 0.0258(11) Uani 1 1 d . . .
H4 H 0.5047 -0.0207 0.2825 0.031 Uiso 1 1 calc R . .
C5 C 0.3896(3) -0.0123(4) 0.3931(4) 0.0177(9) Uani 1 1 d . . .
C6 C 0.3394(3) -0.0842(4) 0.3999(4) 0.0169(9) Uani 1 1 d . . .
C7 C 0.3011(4) 0.2776(4) 0.2081(4) 0.0253(11) Uani 1 1 d . . .
H7 H 0.2704 0.3097 0.2525 0.030 Uiso 1 1 calc R . .
C8 C 0.3780(5) 0.3121(5) 0.1354(5) 0.0352(14) Uani 1 1 d . . .
H8 H 0.3991 0.3674 0.1296 0.042 Uiso 1 1 calc R . .
C9 C 0.4240(5) 0.2643(5) 0.0710(5) 0.0335(14) Uani 1 1 d . . .
H9 H 0.4770 0.2865 0.0208 0.040 Uiso 1 1 calc R . .
C10 C 0.3915(4) 0.1841(4) 0.0811(4) 0.0234(11) Uani 1 1 d . . .
H10 H 0.4218 0.1502 0.0382 0.028 Uiso 1 1 calc R . .
C11 C 0.3135(4) 0.1541(4) 0.1552(4) 0.0176(9) Uani 1 1 d . . .
C12 C 0.2680(3) 0.0749(4) 0.1706(3) 0.0143(8) Uani 1 1 d . . .
C13 C 0.1922(5) 0.4775(4) -0.0411(4) 0.0287(12) Uani 1 1 d . . .
H13 H 0.1527 0.5147 -0.0031 0.034 Uiso 1 1 calc R . .
C14 C 0.2681(5) 0.5156(5) -0.1129(5) 0.0348(14) Uani 1 1 d . . .
H14 H 0.2807 0.5777 -0.1234 0.042 Uiso 1 1 calc R . .
C15 C 0.3250(5) 0.4625(5) -0.1686(5) 0.0347(14) Uani 1 1 d . . .
H15 H 0.3783 0.4867 -0.2167 0.042 Uiso 1 1 calc R . .
C16 C 0.3043(4) 0.3732(5) -0.1542(4) 0.0282(12) Uani 1 1 d . . .
H16 H 0.3413 0.3370 -0.1938 0.034 Uiso 1 1 calc R . .
C17 C 0.2286(4) 0.3387(4) -0.0809(4) 0.0208(10) Uani 1 1 d . . .
C18 C 0.1974(4) 0.2465(4) -0.0562(4) 0.0194(10) Uani 1 1 d . . .
C19 C -0.1329(4) 0.2350(4) 0.6591(4) 0.0176(9) Uani 1 1 d . . .
H19 H -0.1780 0.1984 0.7107 0.021 Uiso 1 1 calc R . .
C20 C -0.1278(4) 0.3288(4) 0.6517(4) 0.0227(10) Uani 1 1 d . . .
H20 H -0.1703 0.3569 0.6963 0.027 Uiso 1 1 calc R . .
C21 C -0.0601(4) 0.3797(4) 0.5784(4) 0.0245(11) Uani 1 1 d . . .
H21 H -0.0538 0.4422 0.5738 0.029 Uiso 1 1 calc R . .
C22 C -0.0010(4) 0.3393(4) 0.5114(4) 0.0195(10) Uani 1 1 d . . .
H22 H 0.0457 0.3736 0.4602 0.023 Uiso 1 1 calc R . .
C23 C -0.0121(3) 0.2475(3) 0.5212(4) 0.0149(9) Uani 1 1 d . . .
C24 C 0.0414(3) 0.2004(3) 0.4500(3) 0.0134(8) Uani 1 1 d . . .
C25 C -0.2150(4) 0.3915(4) 0.4332(4) 0.0206(10) Uani 1 1 d . . .
H25 H -0.2545 0.3499 0.4884 0.025 Uiso 1 1 calc R . .
C26 C -0.2228(4) 0.4913(4) 0.4206(4) 0.0279(12) Uani 1 1 d . . .
H26 H -0.2661 0.5170 0.4667 0.033 Uiso 1 1 calc R . .
C27 C -0.1657(4) 0.5522(4) 0.3390(4) 0.0275(12) Uani 1 1 d . . .
H27 H -0.1689 0.6201 0.3290 0.033 Uiso 1 1 calc R . .
C28 C -0.1037(4) 0.5128(4) 0.2721(4) 0.0249(11) Uani 1 1 d . . .
H28 H -0.0646 0.5534 0.2154 0.030 Uiso 1 1 calc R . .
C29 C -0.1005(4) 0.4133(4) 0.2900(4) 0.0181(9) Uani 1 1 d . . .
C30 C -0.0393(3) 0.3640(4) 0.2229(4) 0.0163(9) Uani 1 1 d . . .
C31 C 0.0549(4) -0.0594(4) 0.1023(4) 0.0214(10) Uani 1 1 d . . .
H31 H 0.1024 -0.0243 0.0536 0.026 Uiso 1 1 calc R . .
C32 C 0.0397(4) -0.1426(4) 0.0977(4) 0.0251(11) Uani 1 1 d . . .
H32 H 0.0767 -0.1645 0.0469 0.030 Uiso 1 1 calc R . .
C33 C -0.0304(4) -0.1928(4) 0.1684(4) 0.0246(11) Uani 1 1 d . . .
H33 H -0.0427 -0.2488 0.1658 0.029 Uiso 1 1 calc R . .
C34 C -0.0825(4) -0.1608(4) 0.2430(4) 0.0227(10) Uani 1 1 d . . .
H34 H -0.1308 -0.1942 0.2921 0.027 Uiso 1 1 calc R . .
C35 C -0.0621(4) -0.0784(4) 0.2440(4) 0.0175(9) Uani 1 1 d . . .
C36 C -0.1099(4) -0.0384(4) 0.3209(4) 0.0162(9) Uani 1 1 d . . .
C1M C -0.3447(6) 0.2626(8) 0.3312(7) 0.070(3) Uani 1 1 d . . .
H2M H -0.3529 0.1930 0.3527 0.105 Uiso 1 1 calc R . .
H3M H -0.3787 0.3132 0.2733 0.105 Uiso 1 1 calc R . .
H4M H -0.3715 0.2825 0.3870 0.105 Uiso 1 1 calc R . .
Cl2 Cl 0.23077(11) 0.39533(12) 0.38115(12) 0.0335(3) Uani 1 1 d . . .
Cl3 Cl 0.47083(11) 0.11244(16) -0.14364(14) 0.0441(4) Uani 1 1 d . . .
O2M O -0.2731(3) -0.2363(4) 0.4053(3) 0.0359(10) Uani 1 1 d . . .
H5M H -0.2731 -0.2607 0.4676 0.054 Uiso 1 1 calc R . .
C2M C -0.3586(6) -0.2387(6) 0.3896(7) 0.053(2) Uani 1 1 d . . .
H6M H -0.4124 -0.2179 0.4357 0.079 Uiso 1 1 calc R . .
H7M H -0.3553 -0.3096 0.4022 0.079 Uiso 1 1 calc R . .
H8M H -0.3689 -0.1904 0.3197 0.079 Uiso 1 1 calc R . .
O3M O 0.0655(3) 0.6206(3) 0.0858(3) 0.0363(10) Uani 1 1 d . . .
H9M H 0.0773 0.6688 0.0285 0.054 Uiso 1 1 calc R . .
C3M C 0.1442(6) 0.5824(7) 0.1399(7) 0.055(2) Uani 1 1 d . . .
H10M H 0.1686 0.6409 0.1267 0.082 Uiso 1 1 calc R . .
H11M H 0.1962 0.5336 0.1179 0.082 Uiso 1 1 calc R . .
H12M H 0.1222 0.5464 0.2124 0.082 Uiso 1 1 calc R . .
O4M O 0.5300(12) 0.4670(13) -0.0616(13) 0.086(4) Uiso 0.50 1 d P . .
H13M H 0.5467 0.4800 -0.1230 0.129 Uiso 0.50 1 calc PR . .
C4M C 0.5975(16) 0.4101(18) -0.0166(17) 0.074(6) Uiso 0.50 1 d P . .
H14M H 0.6513 0.4442 -0.0446 0.111 Uiso 0.50 1 calc PR . .
H15M H 0.6181 0.3449 -0.0237 0.111 Uiso 0.50 1 calc PR . .
H16M H 0.5779 0.3947 0.0550 0.111 Uiso 0.50 1 calc PR . .

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 0.0154(3) 0.0101(3) 0.0117(3) -0.0066(2) 0.0015(2) -0.0048(2)
Ni2 0.0178(3) 0.0148(3) 0.0129(3) -0.0081(2) 0.0009(2) -0.0056(2)
Ni3 0.0165(3) 0.0119(3) 0.0133(3) -0.0066(2) 0.0008(2) -0.0044(2)
Ni4 0.0141(3) 0.0112(3) 0.0129(3) -0.0070(2) 0.0022(2) -0.0051(2)
Ni5 0.0192(3) 0.0136(3) 0.0135(3) -0.0060(2) 0.0022(2) -0.0051(2)
Ni6 0.0147(3) 0.0146(3) 0.0155(3) -0.0086(2) 0.0010(2) -0.0054(2)
Cl1 0.0394(8) 0.0329(7) 0.0273(7) -0.0141(6) -0.0045(6) -0.0084(6)
O1 0.0146(15) 0.0158(15) 0.0162(16) -0.0088(13) 0.0008(12) -0.0071(12)
O2 0.0165(16) 0.0157(15) 0.0150(16) -0.0090(13) 0.0027(12) -0.0080(12)
O3 0.0238(18) 0.0228(17) 0.0163(17) -0.0115(14) 0.0037(14) -0.0106(14)
O4 0.0152(15) 0.0121(14) 0.0137(15) -0.0087(12) 0.0037(12) -0.0057(12)
O5 0.0230(17) 0.0152(15) 0.0143(16) -0.0090(13) 0.0052(13) -0.0075(13)
O6 0.0180(16) 0.0155(15) 0.0164(16) -0.0111(13) 0.0026(13) -0.0062(12)
O1M 0.031(2) 0.029(2) 0.037(2) -0.0149(18) -0.0109(18) -0.0058(17)
N1 0.017(2) 0.021(2) 0.021(2) -0.0106(17) -0.0020(16) -0.0053(16)
N2 0.0167(19) 0.0163(18) 0.0149(19) -0.0064(15) -0.0001(15) -0.0065(15)
N3 0.021(2) 0.026(2) 0.024(2) -0.0162(19) 0.0071(17) -0.0092(17)
N4 0.0180(19) 0.0152(18) 0.0169(19) -0.0069(16) 0.0007(15) -0.0062(15)
N5 0.0140(18) 0.0124(17) 0.0136(18) -0.0056(15) 0.0005(14) -0.0047(14)
N6 0.017(2) 0.025(2) 0.021(2) -0.0162(18) 0.0025(16) -0.0057(16)
N7 0.025(2) 0.018(2) 0.015(2) -0.0053(16) 0.0010(17) -0.0062(17)
N8 0.0169(19) 0.0182(19) 0.0137(18) -0.0052(16) 0.0001(15) -0.0046(15)
N9 0.023(2) 0.032(2) 0.020(2) -0.016(2) 0.0062(18) -0.0088(19)
N10 0.0180(19) 0.0114(17) 0.0157(19) -0.0067(15) -0.0004(15) -0.0039(14)
N11 0.0176(19) 0.0126(17) 0.0114(17) -0.0079(14) 0.0035(14) -0.0060(14)
N12 0.0182(19) 0.0146(18) 0.0181(19) -0.0092(16) 0.0031(15) -0.0079(15)
N13 0.0169(19) 0.0131(17) 0.0178(19) -0.0082(16) -0.0012(15) -0.0012(15)
N14 0.0169(19) 0.0142(18) 0.0139(18) -0.0093(15) 0.0020(15) -0.0019(14)
N15 0.026(2) 0.0143(18) 0.019(2) -0.0092(16) 0.0052(17) -0.0071(16)
N16 0.020(2) 0.0166(18) 0.0157(19) -0.0087(16) -0.0027(15) -0.0032(15)
N17 0.0171(19) 0.0158(18) 0.0127(18) -0.0094(15) 0.0030(14) -0.0056(15)
N18 0.019(2) 0.0179(19) 0.021(2) -0.0103(17) 0.0002(16) -0.0078(16)
C1 0.024(3) 0.028(3) 0.032(3) -0.017(2) 0.002(2) -0.012(2)
C2 0.029(3) 0.039(3) 0.047(4) -0.026(3) 0.007(3) -0.020(3)
C3 0.024(3) 0.041(3) 0.044(4) -0.022(3) 0.008(3) -0.018(3)
C4 0.019(2) 0.028(3) 0.029(3) -0.013(2) 0.004(2) -0.009(2)
C5 0.015(2) 0.021(2) 0.017(2) -0.0089(19) -0.0031(18) -0.0033(18)
C6 0.016(2) 0.015(2) 0.019(2) -0.0080(18) -0.0018(18) -0.0024(17)
C7 0.027(3) 0.025(3) 0.028(3) -0.014(2) 0.007(2) -0.016(2)
C8 0.040(3) 0.035(3) 0.039(3) -0.020(3) 0.013(3) -0.028(3)
C9 0.034(3) 0.041(3) 0.031(3) -0.018(3) 0.014(2) -0.026(3)
C10 0.024(3) 0.028(3) 0.023(3) -0.016(2) 0.004(2) -0.011(2)
C11 0.018(2) 0.020(2) 0.016(2) -0.0078(19) 0.0004(18) -0.0073(18)
C12 0.013(2) 0.014(2) 0.014(2) -0.0076(17) -0.0010(16) -0.0009(16)
C13 0.037(3) 0.021(2) 0.025(3) -0.011(2) 0.005(2) -0.012(2)
C14 0.044(4) 0.027(3) 0.030(3) -0.011(2) 0.007(3) -0.019(3)
C15 0.037(3) 0.034(3) 0.026(3) -0.008(3) 0.012(2) -0.022(3)
C16 0.029(3) 0.026(3) 0.025(3) -0.011(2) 0.005(2) -0.009(2)
C17 0.019(2) 0.022(2) 0.016(2) -0.0063(19) 0.0002(18) -0.0043(19)
C18 0.018(2) 0.022(2) 0.015(2) -0.0078(19) 0.0001(18) -0.0034(18)
C19 0.021(2) 0.016(2) 0.016(2) -0.0101(18) 0.0000(18) -0.0035(18)
C20 0.031(3) 0.019(2) 0.023(3) -0.016(2) 0.001(2) -0.005(2)
C21 0.034(3) 0.016(2) 0.029(3) -0.014(2) 0.000(2) -0.010(2)
C22 0.026(3) 0.016(2) 0.022(2) -0.0118(19) 0.003(2) -0.0101(19)
C23 0.018(2) 0.0119(19) 0.017(2) -0.0081(17) -0.0005(17) -0.0051(16)
C24 0.016(2) 0.0105(19) 0.013(2) -0.0045(16) -0.0020(16) -0.0040(16)
C25 0.024(2) 0.016(2) 0.020(2) -0.0098(19) 0.0001(19) -0.0014(18)
C26 0.034(3) 0.019(2) 0.029(3) -0.016(2) 0.000(2) 0.000(2)
C27 0.038(3) 0.015(2) 0.028(3) -0.013(2) 0.000(2) -0.003(2)
C28 0.031(3) 0.016(2) 0.023(3) -0.007(2) 0.002(2) -0.007(2)
C29 0.021(2) 0.013(2) 0.019(2) -0.0077(18) -0.0026(19) -0.0024(17)
C30 0.019(2) 0.0118(19) 0.016(2) -0.0060(17) -0.0020(18) -0.0017(17)
C31 0.027(3) 0.022(2) 0.017(2) -0.012(2) -0.0031(19) -0.003(2)
C32 0.034(3) 0.024(3) 0.023(3) -0.018(2) -0.005(2) -0.002(2)
C33 0.029(3) 0.023(2) 0.030(3) -0.019(2) -0.005(2) -0.005(2)
C34 0.026(3) 0.021(2) 0.026(3) -0.014(2) -0.004(2) -0.007(2)
C35 0.019(2) 0.016(2) 0.020(2) -0.0114(19) -0.0023(18) -0.0032(17)
C36 0.020(2) 0.0122(19) 0.017(2) -0.0070(17) -0.0027(18) -0.0030(17)
C1M 0.040(4) 0.075(6) 0.060(5) 0.004(5) -0.015(4) -0.020(4)
Cl2 0.0361(8) 0.0315(7) 0.0362(8) -0.0177(6) -0.0049(6) -0.0076(6)
Cl3 0.0260(7) 0.0626(11) 0.0404(9) -0.0316(8) 0.0008(6) 0.0022(7)
O2M 0.046(3) 0.034(2) 0.030(2) -0.014(2) -0.005(2) -0.013(2)
C2M 0.050(4) 0.045(4) 0.076(6) -0.037(4) -0.023(4) 0.002(3)
O3M 0.047(3) 0.028(2) 0.034(2) -0.0106(19) -0.010(2) -0.0102(19)
C3M 0.062(5) 0.055(5) 0.066(5) -0.041(4) -0.033(4) 0.007(4)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O4 2.026(3) . ?
Ni1 O2 2.028(3) . ?
Ni1 N10 2.049(4) 2_556 ?
Ni1 N11 2.071(4) 2_556 ?
Ni1 O1 2.175(3) . ?
Ni1 N17 2.282(4) . ?
Ni2 O3 1.999(3) . ?
Ni2 O5 2.003(3) . ?
Ni2 N16 2.035(4) . ?
Ni2 N17 2.091(4) . ?
Ni2 O2 2.176(3) . ?
Ni2 Cl1 2.5723(17) . ?
Ni3 N14 2.012(4) . ?
Ni3 O6 2.030(3) . ?
Ni3 O1 2.057(3) 2_556 ?
Ni3 N13 2.076(4) . ?
Ni3 O1M 2.113(4) . ?
Ni3 N11 2.250(4) . ?
Ni4 O4 1.835(3) . ?
Ni4 N5 1.854(4) . ?
Ni4 N12 1.863(4) . ?
Ni4 N4 1.898(4) . ?
Ni5 O5 1.827(3) . ?
Ni5 N15 1.848(4) . ?
Ni5 N8 1.854(4) . ?
Ni5 N7 1.885(4) . ?
Ni6 O6 1.824(3) . ?
Ni6 N2 1.845(4) 2_556 ?
Ni6 N18 1.847(4) . ?
Ni6 N1 1.887(4) 2_556 ?
O1 N2 1.368(5) . ?
O1 Ni3 2.057(3) 2_556 ?
O2 N5 1.369(5) . ?
O3 N8 1.342(5) . ?
O4 N11 1.412(5) . ?
O5 N14 1.393(5) . ?
O6 N17 1.412(5) . ?
O1M C1M 1.357(9) . ?
O1M H1M 0.95(8) . ?
N1 C1 1.350(7) . ?
N1 C5 1.355(7) . ?
N1 Ni6 1.887(4) 2_556 ?
N2 C6 1.305(6) . ?
N2 Ni6 1.845(4) 2_556 ?
N3 C6 1.341(7) . ?
N3 H3A 0.90(7) . ?
N3 H3B 0.90(5) . ?
N4 C7 1.338(6) . ?
N4 C11 1.359(7) . ?
N5 C12 1.300(6) . ?
N6 C12 1.350(6) . ?
N6 H6A 0.90(5) . ?
N6 H6B 0.90(5) . ?
N7 C13 1.344(7) . ?
N7 C17 1.363(7) . ?
N8 C18 1.305(6) . ?
N9 C18 1.375(7) . ?
N9 H9A 0.90(6) . ?
N9 H9B 0.90(6) . ?
N10 C19 1.341(6) . ?
N10 C23 1.345(6) . ?
N10 Ni1 2.049(4) 2_556 ?
N11 C24 1.344(6) . ?
N11 Ni1 2.071(4) 2_556 ?
N12 C24 1.322(6) . ?
N12 H12A 0.89(7) . ?
N13 C25 1.331(6) . ?
N13 C29 1.358(6) . ?
N14 C30 1.318(6) . ?
N15 C30 1.339(6) . ?
N15 H15A 0.89(5) . ?
N16 C35 1.343(6) . ?
N16 C31 1.343(7) . ?
N17 C36 1.338(6) . ?
N18 C36 1.328(6) . ?
N18 H18A 0.90(7) . ?
C1 C2 1.385(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.390(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.392(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.394(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.469(7) . ?
C7 C8 1.388(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.395(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.383(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.392(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.465(7) . ?
C13 C14 1.387(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.373(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.390(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.378(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.461(7) . ?
C19 C20 1.397(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.379(8) . ?
C20 H20 0.9500 . ?
C21 C22 1.391(7) . ?
C21 H21 0.9500 . ?
C22 C23 1.389(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.487(6) . ?
C25 C26 1.396(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.388(8) . ?
C26 H26 0.9500 . ?
C27 C28 1.394(8) . ?
C27 H27 0.9500 . ?
C28 C29 1.380(7) . ?
C28 H28 0.9500 . ?
C29 C30 1.482(7) . ?
C31 C32 1.394(7) . ?
C31 H31 0.9500 . ?
C32 C33 1.386(8) . ?
C32 H32 0.9500 . ?
C33 C34 1.387(8) . ?
C33 H33 0.9500 . ?
C34 C35 1.391(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.482(7) . ?
C1M H2M 0.9800 . ?
C1M H3M 0.9800 . ?
C1M H4M 0.9800 . ?
O2M C2M 1.376(9) . ?
O2M H5M 0.8400 . ?
C2M H6M 0.9800 . ?
C2M H7M 0.9800 . ?
C2M H8M 0.9800 . ?
O3M C3M 1.423(9) . ?
O3M H9M 0.8400 . ?
C3M H10M 0.9800 . ?
C3M H11M 0.9800 . ?
C3M H12M 0.9800 . ?
O4M C4M 1.20(2) . ?
O4M H13M 0.8400 . ?
C4M H14M 0.9800 . ?
C4M H15M 0.9800 . ?
C4M H16M 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ni1 O2 84.04(13) . . ?
O4 Ni1 N10 178.65(15) . 2_556 ?
O2 Ni1 N10 95.08(15) . 2_556 ?
O4 Ni1 N11 102.23(14) . 2_556 ?
O2 Ni1 N11 172.80(14) . 2_556 ?
N10 Ni1 N11 78.59(16) 2_556 2_556 ?
O4 Ni1 O1 96.56(13) . . ?
O2 Ni1 O1 96.87(13) . . ?
N10 Ni1 O1 84.55(14) 2_556 . ?
N11 Ni1 O1 86.03(14) 2_556 . ?
O4 Ni1 N17 88.34(14) . . ?
O2 Ni1 N17 83.16(14) . . ?
N10 Ni1 N17 90.55(15) 2_556 . ?
N11 Ni1 N17 93.39(15) 2_556 . ?
O1 Ni1 N17 175.08(13) . . ?
O3 Ni2 O5 86.65(14) . . ?
O3 Ni2 N16 91.04(15) . . ?
O5 Ni2 N16 174.84(16) . . ?
O3 Ni2 N17 169.20(15) . . ?
O5 Ni2 N17 103.78(14) . . ?
N16 Ni2 N17 78.79(16) . . ?
O3 Ni2 O2 91.61(14) . . ?
O5 Ni2 O2 97.16(14) . . ?
N16 Ni2 O2 87.51(15) . . ?
N17 Ni2 O2 84.39(14) . . ?
O3 Ni2 Cl1 95.39(12) . . ?
O5 Ni2 Cl1 83.96(11) . . ?
N16 Ni2 Cl1 91.68(12) . . ?
N17 Ni2 Cl1 88.60(12) . . ?
O2 Ni2 Cl1 172.97(10) . . ?
N14 Ni3 O6 104.18(15) . . ?
N14 Ni3 O1 170.96(15) . 2_556 ?
O6 Ni3 O1 82.48(13) . 2_556 ?
N14 Ni3 N13 78.43(16) . . ?
O6 Ni3 N13 173.74(15) . . ?
O1 Ni3 N13 95.57(15) 2_556 . ?
N14 Ni3 O1M 87.56(17) . . ?
O6 Ni3 O1M 86.18(15) . . ?
O1 Ni3 O1M 99.11(16) 2_556 . ?
N13 Ni3 O1M 88.27(16) . . ?
N14 Ni3 N11 89.71(15) . . ?
O6 Ni3 N11 87.39(14) . . ?
O1 Ni3 N11 84.44(13) 2_556 . ?
N13 Ni3 N11 98.37(15) . . ?
O1M Ni3 N11 172.17(16) . . ?
O4 Ni4 N5 89.92(15) . . ?
O4 Ni4 N12 84.47(16) . . ?
N5 Ni4 N12 174.08(17) . . ?
O4 Ni4 N4 172.17(16) . . ?
N5 Ni4 N4 82.78(17) . . ?
N12 Ni4 N4 102.92(18) . . ?
O5 Ni5 N15 84.49(17) . . ?
O5 Ni5 N8 90.35(16) . . ?
N15 Ni5 N8 173.23(19) . . ?
O5 Ni5 N7 170.28(18) . . ?
N15 Ni5 N7 102.09(19) . . ?
N8 Ni5 N7 83.59(19) . . ?
O6 Ni6 N2 89.68(16) . 2_556 ?
O6 Ni6 N18 84.87(16) . . ?
N2 Ni6 N18 174.41(18) 2_556 . ?
O6 Ni6 N1 172.74(17) . 2_556 ?
N2 Ni6 N1 83.11(18) 2_556 2_556 ?
N18 Ni6 N1 102.32(18) . 2_556 ?
N2 O1 Ni3 110.1(3) . 2_556 ?
N2 O1 Ni1 115.3(3) . . ?
Ni3 O1 Ni1 95.81(13) 2_556 . ?
N5 O2 Ni1 112.2(3) . . ?
N5 O2 Ni2 107.5(2) . . ?
Ni1 O2 Ni2 98.07(14) . . ?
N8 O3 Ni2 115.8(3) . . ?
N11 O4 Ni4 114.1(2) . . ?
N11 O4 Ni1 127.4(2) . . ?
Ni4 O4 Ni1 117.90(16) . . ?
N14 O5 Ni5 114.6(3) . . ?
N14 O5 Ni2 124.5(3) . . ?
Ni5 O5 Ni2 120.32(17) . . ?
N17 O6 Ni6 114.2(3) . . ?
N17 O6 Ni3 125.3(3) . . ?
Ni6 O6 Ni3 115.96(17) . . ?
C1M O1M Ni3 135.3(5) . . ?
C1M O1M H1M 112(5) . . ?
Ni3 O1M H1M 97(5) . . ?
C1 N1 C5 119.3(4) . . ?
C1 N1 Ni6 126.7(4) . 2_556 ?
C5 N1 Ni6 114.0(3) . 2_556 ?
C6 N2 O1 117.6(4) . . ?
C6 N2 Ni6 118.2(3) . 2_556 ?
O1 N2 Ni6 124.1(3) . 2_556 ?
C6 N3 H3A 116(4) . . ?
C6 N3 H3B 124(4) . . ?
H3A N3 H3B 113(6) . . ?
C7 N4 C11 118.7(4) . . ?
C7 N4 Ni4 127.6(4) . . ?
C11 N4 Ni4 113.7(3) . . ?
C12 N5 O2 117.6(4) . . ?
C12 N5 Ni4 118.5(3) . . ?
O2 N5 Ni4 123.8(3) . . ?
C12 N6 H6A 111(4) . . ?
C12 N6 H6B 123(4) . . ?
H6A N6 H6B 113(5) . . ?
C13 N7 C17 118.3(5) . . ?
C13 N7 Ni5 127.7(4) . . ?
C17 N7 Ni5 113.8(3) . . ?
C18 N8 O3 118.2(4) . . ?
C18 N8 Ni5 116.9(4) . . ?
O3 N8 Ni5 124.9(3) . . ?
C18 N9 H9A 108(4) . . ?
C18 N9 H9B 115(4) . . ?
H9A N9 H9B 113(6) . . ?
C19 N10 C23 119.4(4) . . ?
C19 N10 Ni1 126.1(3) . 2_556 ?
C23 N10 Ni1 114.4(3) . 2_556 ?
C24 N11 O4 109.1(3) . . ?
C24 N11 Ni1 111.9(3) . 2_556 ?
O4 N11 Ni1 128.2(3) . 2_556 ?
C24 N11 Ni3 110.7(3) . . ?
O4 N11 Ni3 100.8(2) . . ?
Ni1 N11 Ni3 93.15(15) 2_556 . ?
C24 N12 Ni4 111.1(3) . . ?
C24 N12 H12A 117(4) . . ?
Ni4 N12 H12A 131(4) . . ?
C25 N13 C29 118.7(4) . . ?
C25 N13 Ni3 127.0(3) . . ?
C29 N13 Ni3 114.3(3) . . ?
C30 N14 O5 109.9(4) . . ?
C30 N14 Ni3 117.7(3) . . ?
O5 N14 Ni3 131.4(3) . . ?
C30 N15 Ni5 110.7(3) . . ?
C30 N15 H15A 110(4) . . ?
Ni5 N15 H15A 139(4) . . ?
C35 N16 C31 119.5(4) . . ?
C35 N16 Ni2 114.6(3) . . ?
C31 N16 Ni2 125.8(4) . . ?
C36 N17 O6 109.2(4) . . ?
C36 N17 Ni2 109.6(3) . . ?
O6 N17 Ni2 128.2(3) . . ?
C36 N17 Ni1 118.4(3) . . ?
O6 N17 Ni1 97.5(2) . . ?
Ni2 N17 Ni1 93.02(15) . . ?
C36 N18 Ni6 111.2(3) . . ?
C36 N18 H18A 139(4) . . ?
Ni6 N18 H18A 106(4) . . ?
N1 C1 C2 121.4(5) . . ?
N1 C1 H1 119.3 . . ?
C2 C1 H1 119.3 . . ?
C1 C2 C3 119.4(5) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 H2 120.3 . . ?
C2 C3 C4 119.7(5) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 117.9(5) . . ?
C3 C4 H4 121.0 . . ?
C5 C4 H4 121.0 . . ?
N1 C5 C4 122.3(5) . . ?
N1 C5 C6 112.8(4) . . ?
C4 C5 C6 124.8(5) . . ?
N2 C6 N3 124.4(5) . . ?
N2 C6 C5 111.6(4) . . ?
N3 C6 C5 124.0(4) . . ?
N4 C7 C8 122.2(5) . . ?
N4 C7 H7 118.9 . . ?
C8 C7 H7 118.9 . . ?
C7 C8 C9 119.1(5) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 H8 120.5 . . ?
C10 C9 C8 119.2(5) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
C9 C10 C11 118.6(5) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 H10 120.7 . . ?
N4 C11 C10 122.2(5) . . ?
N4 C11 C12 113.2(4) . . ?
C10 C11 C12 124.5(5) . . ?
N5 C12 N6 125.3(4) . . ?
N5 C12 C11 111.7(4) . . ?
N6 C12 C11 122.9(4) . . ?
N7 C13 C14 121.9(5) . . ?
N7 C13 H13 119.1 . . ?
C14 C13 H13 119.1 . . ?
C15 C14 C13 119.3(6) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 C16 119.7(5) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C17 C16 C15 118.2(5) . . ?
C17 C16 H16 120.9 . . ?
C15 C16 H16 120.9 . . ?
N7 C17 C16 122.5(5) . . ?
N7 C17 C18 112.3(4) . . ?
C16 C17 C18 125.1(5) . . ?
N8 C18 N9 123.2(5) . . ?
N8 C18 C17 113.1(5) . . ?
N9 C18 C17 123.5(4) . . ?
N10 C19 C20 121.6(5) . . ?
N10 C19 H19 119.2 . . ?
C20 C19 H19 119.2 . . ?
C21 C20 C19 118.8(5) . . ?
C21 C20 H20 120.6 . . ?
C19 C20 H20 120.6 . . ?
C20 C21 C22 119.8(5) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 H21 120.1 . . ?
C23 C22 C21 118.3(5) . . ?
C23 C22 H22 120.8 . . ?
C21 C22 H22 120.8 . . ?
N10 C23 C22 122.1(4) . . ?
N10 C23 C24 114.4(4) . . ?
C22 C23 C24 123.5(4) . . ?
N12 C24 N11 120.4(4) . . ?
N12 C24 C23 125.4(4) . . ?
N11 C24 C23 114.2(4) . . ?
N13 C25 C26 122.5(5) . . ?
N13 C25 H25 118.7 . . ?
C26 C25 H25 118.7 . . ?
C27 C26 C25 118.4(5) . . ?
C27 C26 H26 120.8 . . ?
C25 C26 H26 120.8 . . ?
C26 C27 C28 119.4(5) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 H27 120.3 . . ?
C29 C28 C27 118.5(5) . . ?
C29 C28 H28 120.7 . . ?
C27 C28 H28 120.7 . . ?
N13 C29 C28 122.4(5) . . ?
N13 C29 C30 114.2(4) . . ?
C28 C29 C30 123.4(5) . . ?
N14 C30 N15 120.2(4) . . ?
N14 C30 C29 114.5(4) . . ?
N15 C30 C29 125.3(4) . . ?
N16 C31 C32 121.5(5) . . ?
N16 C31 H31 119.3 . . ?
C32 C31 H31 119.3 . . ?
C33 C32 C31 118.9(5) . . ?
C33 C32 H32 120.5 . . ?
C31 C32 H32 120.5 . . ?
C32 C33 C34 119.6(5) . . ?
C32 C33 H33 120.2 . . ?
C34 C33 H33 120.2 . . ?
C33 C34 C35 118.3(5) . . ?
C33 C34 H34 120.9 . . ?
C35 C34 H34 120.9 . . ?
N16 C35 C34 122.2(5) . . ?
N16 C35 C36 113.8(4) . . ?
C34 C35 C36 124.0(5) . . ?
N18 C36 N17 120.1(4) . . ?
N18 C36 C35 124.6(4) . . ?
N17 C36 C35 115.4(4) . . ?
O1M C1M H2M 109.5 . . ?
O1M C1M H3M 109.5 . . ?
H2M C1M H3M 109.5 . . ?
O1M C1M H4M 109.5 . . ?
H2M C1M H4M 109.5 . . ?
H3M C1M H4M 109.5 . . ?
C2M O2M H5M 109.5 . . ?
O2M C2M H6M 109.5 . . ?
O2M C2M H7M 109.5 . . ?
H6M C2M H7M 109.5 . . ?
O2M C2M H8M 109.5 . . ?
H6M C2M H8M 109.5 . . ?
H7M C2M H8M 109.5 . . ?
C3M O3M H9M 109.5 . . ?
O3M C3M H10M 109.5 . . ?
O3M C3M H11M 109.5 . . ?
H10M C3M H11M 109.5 . . ?
O3M C3M H12M 109.5 . . ?
H10M C3M H12M 109.5 . . ?
H11M C3M H12M 109.5 . . ?
C4M O4M H13M 109.5 . . ?
O4M C4M H14M 109.5 . . ?
O4M C4M H15M 109.5 . . ?
H14M C4M H15M 109.5 . . ?
O4M C4M H16M 109.5 . . ?
H14M C4M H16M 109.5 . . ?
H15M C4M H16M 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
O4 Ni1 O1 N2 -19.7(3) . . . . ?
O2 Ni1 O1 N2 65.1(3) . . . . ?
N10 Ni1 O1 N2 159.6(3) 2_556 . . . ?
N11 Ni1 O1 N2 -121.5(3) 2_556 . . . ?
O4 Ni1 O1 Ni3 95.86(13) . . . 2_556 ?
O2 Ni1 O1 Ni3 -179.39(12) . . . 2_556 ?
N10 Ni1 O1 Ni3 -84.91(15) 2_556 . . 2_556 ?
N11 Ni1 O1 Ni3 -6.01(14) 2_556 . . 2_556 ?
O4 Ni1 O2 N5 32.3(3) . . . . ?
N10 Ni1 O2 N5 -148.7(3) 2_556 . . . ?
O1 Ni1 O2 N5 -63.6(3) . . . . ?
N17 Ni1 O2 N5 121.4(3) . . . . ?
O4 Ni1 O2 Ni2 -80.36(14) . . . . ?
N10 Ni1 O2 Ni2 98.62(15) 2_556 . . . ?
O1 Ni1 O2 Ni2 -176.28(12) . . . . ?
N17 Ni1 O2 Ni2 8.67(13) . . . . ?
O3 Ni2 O2 N5 64.2(3) . . . . ?
O5 Ni2 O2 N5 -22.6(3) . . . . ?
N16 Ni2 O2 N5 155.2(3) . . . . ?
N17 Ni2 O2 N5 -125.8(3) . . . . ?
O3 Ni2 O2 Ni1 -179.39(14) . . . . ?
O5 Ni2 O2 Ni1 93.78(14) . . . . ?
N16 Ni2 O2 Ni1 -88.42(16) . . . . ?
N17 Ni2 O2 Ni1 -9.45(15) . . . . ?
O5 Ni2 O3 N8 12.0(3) . . . . ?
N16 Ni2 O3 N8 -172.6(3) . . . . ?
N17 Ni2 O3 N8 -153.1(7) . . . . ?
O2 Ni2 O3 N8 -85.1(3) . . . . ?
Cl1 Ni2 O3 N8 95.6(3) . . . . ?
N5 Ni4 O4 N11 -170.0(3) . . . . ?
N12 Ni4 O4 N11 8.1(3) . . . . ?
N5 Ni4 O4 Ni1 18.5(2) . . . . ?
N12 Ni4 O4 Ni1 -163.4(2) . . . . ?
O2 Ni1 O4 N11 160.6(3) . . . . ?
N11 Ni1 O4 N11 -15.8(4) 2_556 . . . ?
O1 Ni1 O4 N11 -103.2(3) . . . . ?
N17 Ni1 O4 N11 77.3(3) . . . . ?
O2 Ni1 O4 Ni4 -29.20(19) . . . . ?
N11 Ni1 O4 Ni4 154.40(19) 2_556 . . . ?
O1 Ni1 O4 Ni4 67.06(19) . . . . ?
N17 Ni1 O4 Ni4 -112.5(2) . . . . ?
N15 Ni5 O5 N14 2.5(3) . . . . ?
N8 Ni5 O5 N14 -173.1(3) . . . . ?
N15 Ni5 O5 Ni2 174.4(2) . . . . ?
N8 Ni5 O5 Ni2 -1.2(2) . . . . ?
O3 Ni2 O5 N14 166.3(4) . . . . ?
N17 Ni2 O5 N14 -16.6(4) . . . . ?
O2 Ni2 O5 N14 -102.5(3) . . . . ?
Cl1 Ni2 O5 N14 70.5(3) . . . . ?
O3 Ni2 O5 Ni5 -4.9(2) . . . . ?
N17 Ni2 O5 Ni5 172.3(2) . . . . ?
O2 Ni2 O5 Ni5 86.4(2) . . . . ?
Cl1 Ni2 O5 Ni5 -100.6(2) . . . . ?
N2 Ni6 O6 N17 175.7(3) 2_556 . . . ?
N18 Ni6 O6 N17 -5.5(3) . . . . ?
N2 Ni6 O6 Ni3 -27.0(2) 2_556 . . . ?
N18 Ni6 O6 Ni3 151.8(2) . . . . ?
N14 Ni3 O6 N17 6.0(4) . . . . ?
O1 Ni3 O6 N17 -167.8(3) 2_556 . . . ?
O1M Ni3 O6 N17 92.5(3) . . . . ?
N11 Ni3 O6 N17 -83.0(3) . . . . ?
N14 Ni3 O6 Ni6 -148.53(19) . . . . ?
O1 Ni3 O6 Ni6 37.70(18) 2_556 . . . ?
O1M Ni3 O6 Ni6 -62.0(2) . . . . ?
N11 Ni3 O6 Ni6 122.4(2) . . . . ?
N14 Ni3 O1M C1M -174.5(8) . . . . ?
O6 Ni3 O1M C1M 81.1(8) . . . . ?
O1 Ni3 O1M C1M -0.6(8) 2_556 . . . ?
N13 Ni3 O1M C1M -96.0(8) . . . . ?
Ni3 O1 N2 C6 146.4(4) 2_556 . . . ?
Ni1 O1 N2 C6 -106.6(4) . . . . ?
Ni3 O1 N2 Ni6 -31.2(4) 2_556 . . 2_556 ?
Ni1 O1 N2 Ni6 75.8(4) . . . 2_556 ?
N5 Ni4 N4 C7 175.9(5) . . . . ?
N12 Ni4 N4 C7 -2.4(5) . . . . ?
N5 Ni4 N4 C11 -2.3(3) . . . . ?
N12 Ni4 N4 C11 179.3(3) . . . . ?
Ni1 O2 N5 C12 151.4(3) . . . . ?
Ni2 O2 N5 C12 -101.9(4) . . . . ?
Ni1 O2 N5 Ni4 -30.8(4) . . . . ?
Ni2 O2 N5 Ni4 75.9(3) . . . . ?
O4 Ni4 N5 C12 -173.9(4) . . . . ?
N4 Ni4 N5 C12 3.2(4) . . . . ?
O4 Ni4 N5 O2 8.3(3) . . . . ?
N4 Ni4 N5 O2 -174.6(4) . . . . ?
N15 Ni5 N7 C13 3.3(5) . . . . ?
N8 Ni5 N7 C13 179.6(5) . . . . ?
N15 Ni5 N7 C17 178.6(4) . . . . ?
N8 Ni5 N7 C17 -5.1(4) . . . . ?
Ni2 O3 N8 C18 163.5(4) . . . . ?
Ni2 O3 N8 Ni5 -17.5(5) . . . . ?
O5 Ni5 N8 C18 -169.4(4) . . . . ?
N7 Ni5 N8 C18 3.0(4) . . . . ?
O5 Ni5 N8 O3 11.6(4) . . . . ?
N7 Ni5 N8 O3 -176.0(4) . . . . ?
Ni4 O4 N11 C24 -10.0(4) . . . . ?
Ni1 O4 N11 C24 160.5(3) . . . . ?
Ni4 O4 N11 Ni1 -150.7(2) . . . 2_556 ?
Ni1 O4 N11 Ni1 19.8(5) . . . 2_556 ?
Ni4 O4 N11 Ni3 106.5(2) . . . . ?
Ni1 O4 N11 Ni3 -83.0(3) . . . . ?
N14 Ni3 N11 C24 64.1(3) . . . . ?
O6 Ni3 N11 C24 168.3(3) . . . . ?
O1 Ni3 N11 C24 -109.0(3) 2_556 . . . ?
N13 Ni3 N11 C24 -14.2(3) . . . . ?
N14 Ni3 N11 O4 -51.2(2) . . . . ?
O6 Ni3 N11 O4 53.0(2) . . . . ?
O1 Ni3 N11 O4 135.7(2) 2_556 . . . ?
N13 Ni3 N11 O4 -129.5(2) . . . . ?
N14 Ni3 N11 Ni1 178.90(15) . . . 2_556 ?
O6 Ni3 N11 Ni1 -76.89(14) . . . 2_556 ?
O1 Ni3 N11 Ni1 5.80(14) 2_556 . . 2_556 ?
N13 Ni3 N11 Ni1 100.64(16) . . . 2_556 ?
O4 Ni4 N12 C24 -4.3(3) . . . . ?
N4 Ni4 N12 C24 178.4(3) . . . . ?
N14 Ni3 N13 C25 174.1(5) . . . . ?
O1 Ni3 N13 C25 -12.7(4) 2_556 . . . ?
O1M Ni3 N13 C25 86.3(4) . . . . ?
N11 Ni3 N13 C25 -97.9(4) . . . . ?
N14 Ni3 N13 C29 -6.1(3) . . . . ?
O1 Ni3 N13 C29 167.0(3) 2_556 . . . ?
O1M Ni3 N13 C29 -94.0(4) . . . . ?
N11 Ni3 N13 C29 81.8(4) . . . . ?
Ni5 O5 N14 C30 -2.8(5) . . . . ?
Ni2 O5 N14 C30 -174.3(3) . . . . ?
Ni5 O5 N14 Ni3 -170.9(2) . . . . ?
Ni2 O5 N14 Ni3 17.5(6) . . . . ?
O6 Ni3 N14 C30 -177.2(4) . . . . ?
N13 Ni3 N14 C30 8.6(4) . . . . ?
O1M Ni3 N14 C30 97.4(4) . . . . ?
N11 Ni3 N14 C30 -90.0(4) . . . . ?
O6 Ni3 N14 O5 -9.9(4) . . . . ?
N13 Ni3 N14 O5 176.0(4) . . . . ?
O1M Ni3 N14 O5 -95.3(4) . . . . ?
N11 Ni3 N14 O5 77.4(4) . . . . ?
O5 Ni5 N15 C30 -1.6(4) . . . . ?
N7 Ni5 N15 C30 -174.4(4) . . . . ?
O3 Ni2 N16 C35 -167.0(4) . . . . ?
N17 Ni2 N16 C35 16.7(3) . . . . ?
O2 Ni2 N16 C35 101.4(4) . . . . ?
Cl1 Ni2 N16 C35 -71.6(3) . . . . ?
O3 Ni2 N16 C31 9.0(4) . . . . ?
N17 Ni2 N16 C31 -167.3(4) . . . . ?
O2 Ni2 N16 C31 -82.5(4) . . . . ?
Cl1 Ni2 N16 C31 104.5(4) . . . . ?
Ni6 O6 N17 C36 7.2(4) . . . . ?
Ni3 O6 N17 C36 -147.8(3) . . . . ?
Ni6 O6 N17 Ni2 143.8(2) . . . . ?
Ni3 O6 N17 Ni2 -11.2(5) . . . . ?
Ni6 O6 N17 Ni1 -116.4(2) . . . . ?
Ni3 O6 N17 Ni1 88.7(3) . . . . ?
O3 Ni2 N17 C36 -44.6(10) . . . . ?
O5 Ni2 N17 C36 150.7(3) . . . . ?
N16 Ni2 N17 C36 -24.7(3) . . . . ?
O2 Ni2 N17 C36 -113.3(3) . . . . ?
Cl1 Ni2 N17 C36 67.3(3) . . . . ?
O3 Ni2 N17 O6 178.9(7) . . . . ?
O5 Ni2 N17 O6 14.3(4) . . . . ?
N16 Ni2 N17 O6 -161.2(4) . . . . ?
O2 Ni2 N17 O6 110.3(4) . . . . ?
Cl1 Ni2 N17 O6 -69.2(4) . . . . ?
O3 Ni2 N17 Ni1 77.0(9) . . . . ?
O5 Ni2 N17 Ni1 -87.70(16) . . . . ?
N16 Ni2 N17 Ni1 96.88(16) . . . . ?
O2 Ni2 N17 Ni1 8.32(13) . . . . ?
Cl1 Ni2 N17 Ni1 -171.13(11) . . . . ?
O4 Ni1 N17 C36 -170.5(3) . . . . ?
O2 Ni1 N17 C36 105.3(4) . . . . ?
N10 Ni1 N17 C36 10.2(4) 2_556 . . . ?
N11 Ni1 N17 C36 -68.4(4) 2_556 . . . ?
O4 Ni1 N17 O6 -53.9(2) . . . . ?
O2 Ni1 N17 O6 -138.1(2) . . . . ?
N10 Ni1 N17 O6 126.8(2) 2_556 . . . ?
N11 Ni1 N17 O6 48.2(2) 2_556 . . . ?
O4 Ni1 N17 Ni2 75.24(14) . . . . ?
O2 Ni1 N17 Ni2 -8.95(14) . . . . ?
N10 Ni1 N17 Ni2 -104.00(16) 2_556 . . . ?
N11 Ni1 N17 Ni2 177.40(14) 2_556 . . . ?
O6 Ni6 N18 C36 2.6(3) . . . . ?
N1 Ni6 N18 C36 -178.5(3) 2_556 . . . ?
C5 N1 C1 C2 1.1(8) . . . . ?
Ni6 N1 C1 C2 -176.3(5) 2_556 . . . ?
N1 C1 C2 C3 -2.1(10) . . . . ?
C1 C2 C3 C4 2.0(10) . . . . ?
C2 C3 C4 C5 -0.8(9) . . . . ?
C1 N1 C5 C4 0.0(8) . . . . ?
Ni6 N1 C5 C4 177.8(4) 2_556 . . . ?
C1 N1 C5 C6 -176.8(5) . . . . ?
Ni6 N1 C5 C6 1.0(5) 2_556 . . . ?
C3 C4 C5 N1 -0.2(8) . . . . ?
C3 C4 C5 C6 176.2(5) . . . . ?
O1 N2 C6 N3 -2.8(7) . . . . ?
Ni6 N2 C6 N3 175.0(4) 2_556 . . . ?
O1 N2 C6 C5 176.4(4) . . . . ?
Ni6 N2 C6 C5 -5.9(5) 2_556 . . . ?
N1 C5 C6 N2 3.0(6) . . . . ?
C4 C5 C6 N2 -173.7(5) . . . . ?
N1 C5 C6 N3 -177.9(5) . . . . ?
C4 C5 C6 N3 5.4(8) . . . . ?
C11 N4 C7 C8 0.8(9) . . . . ?
Ni4 N4 C7 C8 -177.3(5) . . . . ?
N4 C7 C8 C9 -0.8(10) . . . . ?
C7 C8 C9 C10 0.2(10) . . . . ?
C8 C9 C10 C11 0.2(10) . . . . ?
C7 N4 C11 C10 -0.4(8) . . . . ?
Ni4 N4 C11 C10 178.0(4) . . . . ?
C7 N4 C11 C12 -177.2(5) . . . . ?
Ni4 N4 C11 C12 1.2(5) . . . . ?
C9 C10 C11 N4 -0.1(8) . . . . ?
C9 C10 C11 C12 176.3(5) . . . . ?
O2 N5 C12 N6 -1.4(7) . . . . ?
Ni4 N5 C12 N6 -179.4(4) . . . . ?
O2 N5 C12 C11 174.6(4) . . . . ?
Ni4 N5 C12 C11 -3.3(5) . . . . ?
N4 C11 C12 N5 1.2(6) . . . . ?
C10 C11 C12 N5 -175.5(5) . . . . ?
N4 C11 C12 N6 177.4(4) . . . . ?
C10 C11 C12 N6 0.7(8) . . . . ?
C17 N7 C13 C14 -1.8(9) . . . . ?
Ni5 N7 C13 C14 173.4(5) . . . . ?
N7 C13 C14 C15 0.5(10) . . . . ?
C13 C14 C15 C16 1.7(10) . . . . ?
C14 C15 C16 C17 -2.4(10) . . . . ?
C13 N7 C17 C16 1.0(8) . . . . ?
Ni5 N7 C17 C16 -174.8(4) . . . . ?
C13 N7 C17 C18 -178.1(5) . . . . ?
Ni5 N7 C17 C18 6.1(6) . . . . ?
C15 C16 C17 N7 1.1(9) . . . . ?
C15 C16 C17 C18 -179.9(6) . . . . ?
O3 N8 C18 N9 3.7(7) . . . . ?
Ni5 N8 C18 N9 -175.4(4) . . . . ?
O3 N8 C18 C17 178.6(4) . . . . ?
Ni5 N8 C18 C17 -0.4(6) . . . . ?
N7 C17 C18 N8 -3.7(6) . . . . ?
C16 C17 C18 N8 177.2(5) . . . . ?
N7 C17 C18 N9 171.2(5) . . . . ?
C16 C17 C18 N9 -7.8(8) . . . . ?
C23 N10 C19 C20 -0.7(7) . . . . ?
Ni1 N10 C19 C20 177.8(4) 2_556 . . . ?
N10 C19 C20 C21 -1.9(8) . . . . ?
C19 C20 C21 C22 2.4(8) . . . . ?
C20 C21 C22 C23 -0.4(8) . . . . ?
C19 N10 C23 C22 2.9(7) . . . . ?
Ni1 N10 C23 C22 -175.9(4) 2_556 . . . ?
C19 N10 C23 C24 -175.1(4) . . . . ?
Ni1 N10 C23 C24 6.2(5) 2_556 . . . ?
C21 C22 C23 N10 -2.3(8) . . . . ?
C21 C22 C23 C24 175.5(5) . . . . ?
Ni4 N12 C24 N11 -0.6(6) . . . . ?
Ni4 N12 C24 C23 -179.5(4) . . . . ?
O4 N11 C24 N12 6.8(6) . . . . ?
Ni1 N11 C24 N12 154.4(4) 2_556 . . . ?
Ni3 N11 C24 N12 -103.2(4) . . . . ?
O4 N11 C24 C23 -174.1(4) . . . . ?
Ni1 N11 C24 C23 -26.5(5) 2_556 . . . ?
Ni3 N11 C24 C23 75.9(4) . . . . ?
N10 C23 C24 N12 -167.1(4) . . . . ?
C22 C23 C24 N12 15.0(8) . . . . ?
N10 C23 C24 N11 13.9(6) . . . . ?
C22 C23 C24 N11 -164.0(5) . . . . ?
C29 N13 C25 C26 -2.4(8) . . . . ?
Ni3 N13 C25 C26 177.3(4) . . . . ?
N13 C25 C26 C27 0.8(9) . . . . ?
C25 C26 C27 C28 0.7(9) . . . . ?
C26 C27 C28 C29 -0.7(9) . . . . ?
C25 N13 C29 C28 2.4(8) . . . . ?
Ni3 N13 C29 C28 -177.3(4) . . . . ?
C25 N13 C29 C30 -177.0(4) . . . . ?
Ni3 N13 C29 C30 3.3(5) . . . . ?
C27 C28 C29 N13 -0.9(8) . . . . ?
C27 C28 C29 C30 178.5(5) . . . . ?
O5 N14 C30 N15 1.5(6) . . . . ?
Ni3 N14 C30 N15 171.4(4) . . . . ?
O5 N14 C30 C29 -179.3(4) . . . . ?
Ni3 N14 C30 C29 -9.4(6) . . . . ?
Ni5 N15 C30 N14 0.5(6) . . . . ?
Ni5 N15 C30 C29 -178.7(4) . . . . ?
N13 C29 C30 N14 3.7(6) . . . . ?
C28 C29 C30 N14 -175.7(5) . . . . ?
N13 C29 C30 N15 -177.1(5) . . . . ?
C28 C29 C30 N15 3.5(8) . . . . ?
C35 N16 C31 C32 1.1(7) . . . . ?
Ni2 N16 C31 C32 -174.8(4) . . . . ?
N16 C31 C32 C33 0.6(8) . . . . ?
C31 C32 C33 C34 -1.1(8) . . . . ?
C32 C33 C34 C35 0.0(8) . . . . ?
C31 N16 C35 C34 -2.3(7) . . . . ?
Ni2 N16 C35 C34 174.0(4) . . . . ?
C31 N16 C35 C36 177.5(4) . . . . ?
Ni2 N16 C35 C36 -6.2(5) . . . . ?
C33 C34 C35 N16 1.8(8) . . . . ?
C33 C34 C35 C36 -178.0(5) . . . . ?
Ni6 N18 C36 N17 1.1(6) . . . . ?
Ni6 N18 C36 C35 -178.3(4) . . . . ?
O6 N17 C36 N18 -5.3(6) . . . . ?
Ni2 N17 C36 N18 -150.3(4) . . . . ?
Ni1 N17 C36 N18 104.8(4) . . . . ?
O6 N17 C36 C35 174.1(4) . . . . ?
Ni2 N17 C36 C35 29.1(5) . . . . ?
Ni1 N17 C36 C35 -75.8(5) . . . . ?
N16 C35 C36 N18 163.2(5) . . . . ?
C34 C35 C36 N18 -17.0(8) . . . . ?
N16 C35 C36 N17 -16.2(6) . . . . ?
C34 C35 C36 N17 163.6(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1M H1M Cl1 0.95(8) 2.26(8) 3.190(5) 167(7) .
N3 H3B Cl3 0.90(5) 2.35(5) 3.247(5) 169(6) 2_655
N6 H6B Cl3 0.90(5) 2.57(4) 3.359(5) 146(6) 2_655
N9 H9B Cl3 0.90(6) 2.39(4) 3.284(5) 174(6) .
N12 H12A Cl2 0.89(7) 2.61(7) 3.501(4) 176(6) .
N15 H15A O3M 0.89(5) 2.30(6) 3.172(6) 164(6) .
N18 H18A O2M 0.90(7) 2.35(7) 3.162(6) 151(6) .
O2M H5M Cl2 0.84 2.30 3.060(5) 151.4 2_556
O3M H9M Cl1 0.84 2.42 3.238(5) 163.8 2_565

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        29.13
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         4.818
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.208

# Attachment '1_squeeze_revised.cif'

data_1_squeeze
_database_code_depnum_ccdc_archive 'CCDC 678538'

# =======================================================================

_audit_creation_method           'SHELXL-97, manual editing plus enCIFer'
_audit_creation_date             '09 january 2008'

# =======================================================================

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C74 H74 C12 N36 Ni12 O14, 5(C H4 O), 4(Cl)'
_chemical_formula_sum            'C79 H94 Cl6 N36 Ni12 O19'
_chemical_formula_weight         2769.12

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'
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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.8718(8)
_cell_length_b                   15.1738(7)
_cell_length_c                   15.3809(8)
_cell_angle_alpha                60.525(2)
_cell_angle_beta                 73.084(3)
_cell_angle_gamma                69.854(2)
_cell_volume                     2805.3(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9871
_cell_measurement_theta_min      2.72
_cell_measurement_theta_max      29.77

_exptl_crystal_description       Prism
_exptl_crystal_colour            Brown
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1410
_exptl_absorpt_coefficient_mu    2.182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6695
_exptl_absorpt_correction_T_max  0.8279
_exptl_absorpt_process_details   
;
SADABS (Sheldrick, 1997)
;

_exptl_special_details           
;
See details in the main paper
;

_diffrn_ambient_temperature      150(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 X8 Kappa CCD APEX II'
_diffrn_measurement_method       'omega/phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            147901
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.52
_diffrn_reflns_theta_max         29.13
_reflns_number_total             14885
_reflns_number_gt                11471
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_cell_refinement       'APEX2 '
_computing_data_reduction        'SAINT+ (Bruker, 1997-2005)'
_computing_structure_solution    'SHELXTL (Bruker 2001)'
_computing_structure_refinement  'SHELXTL '
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'SHELXTL '

_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.

A considerable smeared-out electron density was found in the empty spaces
available in the structure which prevented a sensible location and refinement
of additional solvent molecules. Searches for the total potential solvent area
using thesoftware package <i> PLATON </i> revealed the presence of a large
cavity centered at (1/2; 1/2; 1/2) with an internal volume of
<i>ca.</i> 418\%A^3^ (<i>ca.</i> 15% of the total volume of the unit cell). The
original data set was then mathematically treated using the <i>SQUEEZE</i>
subroutines in order to remove the contribution of these highly disordered
molecules in the solvent-accessible volume. It was estimated that the
<i>ca.</i> 15% empty volume would contain <i>ca.</i> 181 electrons. Taking into
consideration that small solvent molecules should occupying average
<i>ca.</i> 40\%A^3^, it is thus feasible to assume that approximately 10
additional methanol molecules are still located in the empty spaces of the
structure (<i>i.e.</i>, <i>n</i>\\simeq10). The calculated solvent-free
reflection list was than used for further structural refinement.
;

_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^)+(0.0647P)^2^+2.2028P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14885
_refine_ls_number_parameters     721
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0412
_refine_ls_wR_factor_ref         0.1257
_refine_ls_wR_factor_gt          0.1203
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.124
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.07116(2) -0.05695(2) 0.40075(2) 0.01202(8) Uani 1 1 d . . .
Ni2 Ni 0.01048(3) 0.09885(3) 0.18348(3) 0.01481(9) Uani 1 1 d . . .
Ni3 Ni -0.13069(3) 0.20392(3) 0.38312(3) 0.01404(9) Uani 1 1 d . . .
Ni4 Ni 0.16178(2) 0.14810(2) 0.30914(3) 0.01248(8) Uani 1 1 d . . .
Ni5 Ni 0.08166(3) 0.31928(3) 0.07838(3) 0.01640(9) Uani 1 1 d . . .
Ni6 Ni -0.22934(2) 0.00970(3) 0.46419(3) 0.01444(9) Uani 1 1 d . . .
Cl1 Cl -0.15309(7) 0.20314(7) 0.11906(6) 0.03417(19) Uani 1 1 d . . .
O1 O 0.20129(13) -0.14380(14) 0.47109(14) 0.0146(4) Uani 1 1 d . . .
O2 O 0.13849(13) 0.00248(14) 0.25607(14) 0.0149(4) Uani 1 1 d . . .
O3 O 0.09077(15) 0.14652(16) 0.04710(15) 0.0202(4) Uani 1 1 d . . .
O4 O 0.06597(13) 0.08183(14) 0.39340(14) 0.0132(4) Uani 1 1 d . . .
O5 O 0.01069(14) 0.23142(15) 0.18224(14) 0.0178(4) Uani 1 1 d . . .
O6 O -0.12322(14) 0.06245(14) 0.39446(14) 0.0153(4) Uani 1 1 d . . .
O1M O -0.24932(17) 0.26150(18) 0.30485(18) 0.0308(5) Uani 1 1 d D . .
H1M H -0.229(3) 0.237(3) 0.254(2) 0.046 Uiso 1 1 d D . .
N1 N 0.34326(17) 0.03335(18) 0.45622(18) 0.0191(5) Uani 1 1 d . . .
N2 N 0.25814(16) -0.08454(18) 0.46211(17) 0.0157(5) Uani 1 1 d . . .
N3 N 0.37292(19) -0.1412(2) 0.3472(2) 0.0235(6) Uani 1 1 d D . .
H3A H 0.337(2) -0.179(2) 0.348(2) 0.035 Uiso 1 1 d D . .
H3B H 0.4230(17) -0.133(3) 0.2961(19) 0.035 Uiso 1 1 d D . .
N4 N 0.26892(17) 0.20090(18) 0.21780(18) 0.0171(5) Uani 1 1 d . . .
N5 N 0.19276(16) 0.06734(17) 0.24045(17) 0.0138(4) Uani 1 1 d . . .
N6 N 0.29884(18) 0.02143(19) 0.11402(19) 0.0199(5) Uani 1 1 d D . .
H6A H 0.2658(17) -0.025(2) 0.129(3) 0.030 Uiso 1 1 d D . .
H6B H 0.3618(9) 0.003(2) 0.092(3) 0.030 Uiso 1 1 d D . .
N7 N 0.17299(18) 0.38954(19) -0.02387(18) 0.0214(5) Uani 1 1 d . . .
N8 N 0.12669(17) 0.22815(18) 0.01930(18) 0.0176(5) Uani 1 1 d . . .
N9 N 0.23359(19) 0.1901(2) -0.1115(2) 0.0251(6) Uani 1 1 d D . .
H9A H 0.216(2) 0.1293(15) -0.083(3) 0.038 Uiso 1 1 d D . .
H9B H 0.2974(9) 0.184(2) -0.135(3) 0.038 Uiso 1 1 d D . .
N10 N -0.07558(16) 0.19544(17) 0.59496(17) 0.0147(5) Uani 1 1 d . . .
N11 N 0.00376(16) 0.12815(17) 0.45690(17) 0.0132(4) Uani 1 1 d . . .
N12 N 0.11866(17) 0.22531(17) 0.38341(18) 0.0163(5) Uani 1 1 d D . .
H12A H 0.145(2) 0.266(2) 0.391(3) 0.024 Uiso 1 1 d D . .
N13 N -0.15426(17) 0.35247(17) 0.37065(18) 0.0163(5) Uani 1 1 d . . .
N14 N -0.05085(17) 0.27162(17) 0.24897(17) 0.0154(5) Uani 1 1 d . . .
N15 N 0.02293(18) 0.40652(18) 0.14094(19) 0.0208(5) Uani 1 1 d D . .
H15A H 0.028(3) 0.4690(14) 0.129(3) 0.031 Uiso 1 1 d D . .
N16 N 0.00407(17) -0.02774(18) 0.17416(18) 0.0175(5) Uani 1 1 d . . .
N17 N -0.06483(16) 0.02175(17) 0.32562(17) 0.0144(5) Uani 1 1 d . . .
N18 N -0.19176(17) -0.05719(18) 0.38191(18) 0.0182(5) Uani 1 1 d D . .
H18A H -0.222(2) -0.090(2) 0.369(3) 0.027 Uiso 1 1 d D . .
C1 C 0.3787(2) 0.1053(2) 0.4538(3) 0.0253(7) Uani 1 1 d . . .
H1 H 0.3466 0.1371 0.4981 0.030 Uiso 1 1 calc R . .
C2 C 0.4609(2) 0.1340(3) 0.3882(3) 0.0347(8) Uani 1 1 d . . .
H2 H 0.4841 0.1857 0.3868 0.042 Uiso 1 1 calc R . .
C3 C 0.5087(2) 0.0870(3) 0.3249(3) 0.0353(8) Uani 1 1 d . . .
H3 H 0.5657 0.1053 0.2804 0.042 Uiso 1 1 calc R . .
C4 C 0.4733(2) 0.0126(2) 0.3263(2) 0.0260(7) Uani 1 1 d . . .
H4 H 0.5052 -0.0205 0.2830 0.031 Uiso 1 1 calc R . .
C5 C 0.3899(2) -0.0120(2) 0.3927(2) 0.0187(6) Uani 1 1 d . . .
C6 C 0.3391(2) -0.0841(2) 0.3999(2) 0.0169(6) Uani 1 1 d . . .
C7 C 0.3013(2) 0.2774(2) 0.2078(2) 0.0253(7) Uani 1 1 d . . .
H7 H 0.2704 0.3100 0.2516 0.030 Uiso 1 1 calc R . .
C8 C 0.3785(3) 0.3108(3) 0.1357(3) 0.0343(8) Uani 1 1 d . . .
H8 H 0.4004 0.3654 0.1304 0.041 Uiso 1 1 calc R . .
C9 C 0.4234(3) 0.2638(3) 0.0712(3) 0.0339(8) Uani 1 1 d . . .
H9 H 0.4757 0.2869 0.0204 0.041 Uiso 1 1 calc R . .
C10 C 0.3918(2) 0.1838(2) 0.0814(2) 0.0238(6) Uani 1 1 d . . .
H10 H 0.4226 0.1495 0.0390 0.029 Uiso 1 1 calc R . .
C11 C 0.3142(2) 0.1543(2) 0.1549(2) 0.0173(6) Uani 1 1 d . . .
C12 C 0.26824(19) 0.0744(2) 0.1709(2) 0.0155(5) Uani 1 1 d . . .
C13 C 0.1923(3) 0.4774(2) -0.0412(2) 0.0293(7) Uani 1 1 d . . .
H13 H 0.1530 0.5146 -0.0031 0.035 Uiso 1 1 calc R . .
C14 C 0.2677(3) 0.5154(3) -0.1130(3) 0.0352(8) Uani 1 1 d . . .
H14 H 0.2798 0.5778 -0.1237 0.042 Uiso 1 1 calc R . .
C15 C 0.3254(3) 0.4628(3) -0.1692(3) 0.0348(8) Uani 1 1 d . . .
H15 H 0.3783 0.4875 -0.2178 0.042 Uiso 1 1 calc R . .
C16 C 0.3052(2) 0.3731(2) -0.1538(2) 0.0276(7) Uani 1 1 d . . .
H16 H 0.3433 0.3359 -0.1923 0.033 Uiso 1 1 calc R . .
C17 C 0.2284(2) 0.3386(2) -0.0811(2) 0.0210(6) Uani 1 1 d . . .
C18 C 0.1974(2) 0.2465(2) -0.0561(2) 0.0195(6) Uani 1 1 d . . .
C19 C -0.1333(2) 0.2351(2) 0.6591(2) 0.0175(6) Uani 1 1 d . . .
H19 H -0.1788 0.1988 0.7105 0.021 Uiso 1 1 calc R . .
C20 C -0.1276(2) 0.3284(2) 0.6517(2) 0.0224(6) Uani 1 1 d . . .
H20 H -0.1697 0.3562 0.6966 0.027 Uiso 1 1 calc R . .
C21 C -0.0601(2) 0.3799(2) 0.5782(2) 0.0250(7) Uani 1 1 d . . .
H21 H -0.0542 0.4426 0.5733 0.030 Uiso 1 1 calc R . .
C22 C -0.0012(2) 0.3394(2) 0.5116(2) 0.0197(6) Uani 1 1 d . . .
H22 H 0.0456 0.3738 0.4604 0.024 Uiso 1 1 calc R . .
C23 C -0.0120(2) 0.2474(2) 0.5211(2) 0.0153(5) Uani 1 1 d . . .
C24 C 0.04152(19) 0.20045(19) 0.4502(2) 0.0131(5) Uani 1 1 d . . .
C25 C -0.2152(2) 0.3917(2) 0.4336(2) 0.0211(6) Uani 1 1 d . . .
H25 H -0.2544 0.3500 0.4892 0.025 Uiso 1 1 calc R . .
C26 C -0.2227(2) 0.4913(2) 0.4204(2) 0.0271(7) Uani 1 1 d . . .
H26 H -0.2661 0.5172 0.4663 0.033 Uiso 1 1 calc R . .
C27 C -0.1662(2) 0.5518(2) 0.3393(2) 0.0278(7) Uani 1 1 d . . .
H27 H -0.1697 0.6199 0.3291 0.033 Uiso 1 1 calc R . .
C28 C -0.1039(2) 0.5126(2) 0.2725(2) 0.0249(7) Uani 1 1 d . . .
H28 H -0.0648 0.5534 0.2160 0.030 Uiso 1 1 calc R . .
C29 C -0.1003(2) 0.4131(2) 0.2902(2) 0.0181(6) Uani 1 1 d . . .
C30 C -0.0390(2) 0.3641(2) 0.2229(2) 0.0167(6) Uani 1 1 d . . .
C31 C 0.0550(2) -0.0602(2) 0.1028(2) 0.0216(6) Uani 1 1 d . . .
H31 H 0.1029 -0.0256 0.0543 0.026 Uiso 1 1 calc R . .
C32 C 0.0396(2) -0.1429(2) 0.0980(2) 0.0254(7) Uani 1 1 d . . .
H32 H 0.0767 -0.1650 0.0474 0.030 Uiso 1 1 calc R . .
C33 C -0.0305(2) -0.1924(2) 0.1680(2) 0.0242(6) Uani 1 1 d . . .
H33 H -0.0431 -0.2481 0.1652 0.029 Uiso 1 1 calc R . .
C34 C -0.0826(2) -0.1603(2) 0.2427(2) 0.0214(6) Uani 1 1 d . . .
H34 H -0.1310 -0.1936 0.2917 0.026 Uiso 1 1 calc R . .
C35 C -0.0621(2) -0.0782(2) 0.2440(2) 0.0180(6) Uani 1 1 d . . .
C36 C -0.1102(2) -0.0382(2) 0.3208(2) 0.0163(5) Uani 1 1 d . . .
C1M C -0.3450(3) 0.2632(4) 0.3322(4) 0.0762(17) Uani 1 1 d . . .
H2M H -0.3533 0.1928 0.3581 0.114 Uiso 1 1 calc R . .
H3M H -0.3786 0.3105 0.2734 0.114 Uiso 1 1 calc R . .
H4M H -0.3722 0.2876 0.3850 0.114 Uiso 1 1 calc R . .
Cl2 Cl 0.23067(6) 0.39536(7) 0.38113(7) 0.03395(19) Uani 1 1 d . . .
Cl3 Cl 0.47073(6) 0.11211(9) -0.14337(8) 0.0450(2) Uani 1 1 d . . .
O2M O -0.27285(18) -0.23687(19) 0.40564(19) 0.0352(6) Uani 1 1 d . . .
H5M H -0.2658 -0.2733 0.4667 0.053 Uiso 1 1 calc R . .
C2M C -0.3596(3) -0.2411(3) 0.3916(4) 0.0539(12) Uani 1 1 d . . .
H6M H -0.4134 -0.2177 0.4361 0.081 Uiso 1 1 calc R . .
H7M H -0.3566 -0.3130 0.4076 0.081 Uiso 1 1 calc R . .
H8M H -0.3696 -0.1956 0.3211 0.081 Uiso 1 1 calc R . .
O3M O 0.06536(19) 0.62089(19) 0.08552(19) 0.0366(6) Uani 1 1 d . . .
H9M H 0.0757 0.6722 0.0304 0.055 Uiso 1 1 calc R . .
C3M C 0.1440(3) 0.5817(4) 0.1413(4) 0.0545(12) Uani 1 1 d . . .
H10M H 0.1700 0.6395 0.1267 0.082 Uiso 1 1 calc R . .
H11M H 0.1951 0.5307 0.1215 0.082 Uiso 1 1 calc R . .
H12M H 0.1206 0.5480 0.2138 0.082 Uiso 1 1 calc R . .
O4M O 0.5339(6) 0.4677(6) -0.0653(6) 0.089(2) Uiso 0.50 1 d P . .
H13M H 0.5358 0.4589 -0.1157 0.133 Uiso 0.50 1 calc PR . .
C4M C 0.6078(7) 0.4068(7) -0.0218(7) 0.057(2) Uiso 0.50 1 d P . .
H14M H 0.6495 0.4481 -0.0281 0.086 Uiso 0.50 1 calc PR . .
H15M H 0.6440 0.3599 -0.0536 0.086 Uiso 0.50 1 calc PR . .
H16M H 0.5866 0.3655 0.0499 0.086 Uiso 0.50 1 calc PR . .

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 0.01538(17) 0.01038(15) 0.01170(17) -0.00658(13) 0.00151(13) -0.00491(13)
Ni2 0.01828(18) 0.01513(17) 0.01300(17) -0.00822(14) 0.00095(14) -0.00578(13)
Ni3 0.01662(18) 0.01202(16) 0.01369(17) -0.00671(14) 0.00063(13) -0.00439(13)
Ni4 0.01400(17) 0.01145(16) 0.01323(17) -0.00723(13) 0.00219(13) -0.00511(13)
Ni5 0.01945(19) 0.01379(16) 0.01369(18) -0.00603(14) 0.00227(14) -0.00529(13)
Ni6 0.01492(18) 0.01475(16) 0.01579(18) -0.00877(14) 0.00114(13) -0.00562(13)
Cl1 0.0407(5) 0.0342(4) 0.0286(4) -0.0148(4) -0.0046(4) -0.0089(4)
O1 0.0144(9) 0.0163(9) 0.0168(10) -0.0097(8) 0.0012(7) -0.0070(7)
O2 0.0163(9) 0.0159(9) 0.0161(10) -0.0095(8) 0.0026(8) -0.0083(7)
O3 0.0231(11) 0.0234(10) 0.0179(10) -0.0125(9) 0.0051(8) -0.0112(8)
O4 0.0162(9) 0.0122(8) 0.0138(9) -0.0092(7) 0.0041(7) -0.0059(7)
O5 0.0229(10) 0.0161(9) 0.0147(10) -0.0093(8) 0.0049(8) -0.0076(8)
O6 0.0175(10) 0.0154(9) 0.0157(10) -0.0103(8) 0.0030(8) -0.0063(7)
O1M 0.0289(12) 0.0302(12) 0.0374(14) -0.0153(11) -0.0117(11) -0.0054(10)
N1 0.0172(12) 0.0205(12) 0.0216(13) -0.0106(10) -0.0014(10) -0.0059(9)
N2 0.0165(11) 0.0164(11) 0.0152(11) -0.0072(9) -0.0008(9) -0.0060(9)
N3 0.0213(13) 0.0278(13) 0.0239(14) -0.0167(12) 0.0085(11) -0.0104(11)
N4 0.0181(12) 0.0161(11) 0.0172(12) -0.0080(10) 0.0006(9) -0.0059(9)
N5 0.0146(11) 0.0128(10) 0.0140(11) -0.0060(9) 0.0006(9) -0.0053(8)
N6 0.0170(12) 0.0254(13) 0.0220(13) -0.0166(11) 0.0032(10) -0.0060(10)
N7 0.0247(13) 0.0180(11) 0.0165(12) -0.0058(10) 0.0020(10) -0.0063(10)
N8 0.0181(12) 0.0170(11) 0.0152(11) -0.0063(10) -0.0006(9) -0.0041(9)
N9 0.0238(14) 0.0305(14) 0.0222(14) -0.0161(12) 0.0069(11) -0.0094(11)
N10 0.0180(11) 0.0120(10) 0.0146(11) -0.0068(9) -0.0014(9) -0.0035(9)
N11 0.0166(11) 0.0135(10) 0.0115(11) -0.0087(9) 0.0035(9) -0.0054(9)
N12 0.0187(12) 0.0141(11) 0.0181(12) -0.0087(10) 0.0014(9) -0.0071(9)
N13 0.0171(12) 0.0131(10) 0.0168(12) -0.0076(9) -0.0011(9) -0.0012(9)
N14 0.0169(11) 0.0153(11) 0.0138(11) -0.0092(9) 0.0010(9) -0.0019(9)
N15 0.0253(13) 0.0131(11) 0.0201(12) -0.0078(10) 0.0041(10) -0.0053(10)
N16 0.0209(12) 0.0169(11) 0.0161(12) -0.0091(10) -0.0021(10) -0.0039(9)
N17 0.0170(11) 0.0148(10) 0.0133(11) -0.0093(9) 0.0025(9) -0.0050(9)
N18 0.0199(12) 0.0197(12) 0.0200(12) -0.0111(10) -0.0008(10) -0.0085(10)
C1 0.0231(16) 0.0263(15) 0.0319(17) -0.0162(14) 0.0016(13) -0.0112(12)
C2 0.0292(18) 0.0401(19) 0.045(2) -0.0251(18) 0.0070(16) -0.0204(15)
C3 0.0262(17) 0.0398(19) 0.042(2) -0.0192(17) 0.0089(15) -0.0200(15)
C4 0.0188(15) 0.0286(16) 0.0289(17) -0.0146(14) 0.0039(13) -0.0069(12)
C5 0.0171(14) 0.0203(13) 0.0184(14) -0.0080(12) -0.0042(11) -0.0035(11)
C6 0.0172(13) 0.0148(12) 0.0189(14) -0.0087(11) -0.0019(11) -0.0029(10)
C7 0.0262(16) 0.0248(15) 0.0277(17) -0.0140(13) 0.0055(13) -0.0133(13)
C8 0.0376(19) 0.0335(18) 0.040(2) -0.0198(16) 0.0102(16) -0.0256(16)
C9 0.0325(18) 0.042(2) 0.0299(18) -0.0171(16) 0.0128(15) -0.0250(16)
C10 0.0231(15) 0.0286(16) 0.0221(15) -0.0146(13) 0.0040(12) -0.0098(12)
C11 0.0162(13) 0.0196(13) 0.0160(14) -0.0078(11) 0.0001(11) -0.0061(11)
C12 0.0150(13) 0.0149(12) 0.0153(13) -0.0077(11) -0.0018(10) -0.0006(10)
C13 0.0387(19) 0.0215(15) 0.0248(17) -0.0099(13) 0.0048(14) -0.0123(13)
C14 0.046(2) 0.0270(17) 0.0295(18) -0.0102(15) 0.0074(16) -0.0198(15)
C15 0.0353(19) 0.0348(18) 0.0265(17) -0.0075(15) 0.0101(15) -0.0209(15)
C16 0.0279(17) 0.0268(16) 0.0218(16) -0.0091(13) 0.0035(13) -0.0077(13)
C17 0.0195(14) 0.0228(14) 0.0153(14) -0.0059(12) -0.0013(11) -0.0037(11)
C18 0.0184(14) 0.0211(14) 0.0157(14) -0.0074(12) -0.0007(11) -0.0035(11)
C19 0.0196(14) 0.0176(13) 0.0170(14) -0.0110(11) 0.0007(11) -0.0037(11)
C20 0.0284(16) 0.0200(14) 0.0227(15) -0.0170(12) 0.0020(12) -0.0032(12)
C21 0.0347(17) 0.0161(13) 0.0296(17) -0.0147(13) -0.0004(14) -0.0085(12)
C22 0.0251(15) 0.0164(13) 0.0205(15) -0.0109(12) 0.0033(12) -0.0096(11)
C23 0.0180(13) 0.0125(12) 0.0167(13) -0.0073(11) -0.0003(11) -0.0054(10)
C24 0.0165(13) 0.0094(11) 0.0138(13) -0.0050(10) -0.0023(10) -0.0036(9)
C25 0.0241(15) 0.0172(13) 0.0193(15) -0.0101(12) 0.0005(12) -0.0018(11)
C26 0.0323(18) 0.0200(14) 0.0271(17) -0.0160(13) 0.0000(14) 0.0012(12)
C27 0.0389(19) 0.0145(13) 0.0278(17) -0.0126(13) -0.0002(14) -0.0029(12)
C28 0.0316(17) 0.0153(13) 0.0236(16) -0.0075(12) 0.0010(13) -0.0068(12)
C29 0.0208(14) 0.0132(12) 0.0190(14) -0.0072(11) -0.0031(11) -0.0023(10)
C30 0.0190(14) 0.0121(12) 0.0163(13) -0.0056(11) -0.0029(11) -0.0015(10)
C31 0.0258(15) 0.0230(14) 0.0172(14) -0.0119(12) -0.0012(12) -0.0040(12)
C32 0.0339(18) 0.0255(15) 0.0213(16) -0.0175(13) -0.0033(13) -0.0018(13)
C33 0.0313(17) 0.0227(14) 0.0277(16) -0.0170(13) -0.0056(13) -0.0067(12)
C34 0.0251(15) 0.0200(14) 0.0250(15) -0.0135(12) -0.0038(12) -0.0063(12)
C35 0.0199(14) 0.0162(13) 0.0196(14) -0.0094(11) -0.0048(11) -0.0025(11)
C36 0.0192(14) 0.0127(12) 0.0173(14) -0.0070(11) -0.0030(11) -0.0033(10)
C1M 0.048(3) 0.074(4) 0.071(4) 0.005(3) -0.020(3) -0.022(3)
Cl2 0.0363(5) 0.0320(4) 0.0367(5) -0.0178(4) -0.0046(4) -0.0081(3)
Cl3 0.0262(4) 0.0638(6) 0.0412(5) -0.0317(5) 0.0006(4) 0.0022(4)
O2M 0.0429(15) 0.0336(13) 0.0321(13) -0.0146(11) -0.0047(11) -0.0128(11)
C2M 0.054(3) 0.043(2) 0.077(3) -0.036(2) -0.025(2) 0.0023(19)
O3M 0.0468(15) 0.0276(12) 0.0340(14) -0.0094(11) -0.0098(12) -0.0104(11)
C3M 0.060(3) 0.058(3) 0.063(3) -0.041(2) -0.029(2) 0.004(2)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O4 2.0279(18) . ?
Ni1 O2 2.0293(19) . ?
Ni1 N10 2.048(2) 2_556 ?
Ni1 N11 2.070(2) 2_556 ?
Ni1 O1 2.1705(19) . ?
Ni1 N17 2.278(2) . ?
Ni2 O3 1.998(2) . ?
Ni2 O5 2.0033(19) . ?
Ni2 N16 2.031(2) . ?
Ni2 N17 2.089(2) . ?
Ni2 O2 2.1729(19) . ?
Ni2 Cl1 2.5713(10) . ?
Ni3 N14 2.013(2) . ?
Ni3 O6 2.0320(18) . ?
Ni3 O1 2.0589(19) 2_556 ?
Ni3 N13 2.076(2) . ?
Ni3 O1M 2.113(2) . ?
Ni3 N11 2.250(2) . ?
Ni4 O4 1.8306(18) . ?
Ni4 N5 1.853(2) . ?
Ni4 N12 1.861(2) . ?
Ni4 N4 1.903(2) . ?
Ni5 O5 1.8263(19) . ?
Ni5 N15 1.846(2) . ?
Ni5 N8 1.852(2) . ?
Ni5 N7 1.887(2) . ?
Ni6 O6 1.8227(18) . ?
Ni6 N18 1.846(2) . ?
Ni6 N2 1.846(2) 2_556 ?
Ni6 N1 1.888(2) 2_556 ?
O1 N2 1.370(3) . ?
O1 Ni3 2.0589(19) 2_556 ?
O2 N5 1.371(3) . ?
O3 N8 1.343(3) . ?
O4 N11 1.416(3) . ?
O5 N14 1.396(3) . ?
O6 N17 1.413(3) . ?
O1M C1M 1.356(5) . ?
O1M H1M 0.96(4) . ?
N1 C1 1.348(4) . ?
N1 C5 1.359(4) . ?
N1 Ni6 1.888(2) 2_556 ?
N2 C6 1.301(4) . ?
N2 Ni6 1.846(2) 2_556 ?
N3 C6 1.347(4) . ?
N3 H3A 0.90(3) . ?
N3 H3B 0.90(3) . ?
N4 C7 1.329(4) . ?
N4 C11 1.362(4) . ?
N5 C12 1.299(3) . ?
N6 C12 1.352(4) . ?
N6 H6A 0.90(3) . ?
N6 H6B 0.90(3) . ?
N7 C13 1.342(4) . ?
N7 C17 1.364(4) . ?
N8 C18 1.305(4) . ?
N9 C18 1.371(4) . ?
N9 H9A 0.90(3) . ?
N9 H9B 0.90(3) . ?
N10 C19 1.345(4) . ?
N10 C23 1.347(3) . ?
N10 Ni1 2.048(2) 2_556 ?
N11 C24 1.345(3) . ?
N11 Ni1 2.070(2) 2_556 ?
N12 C24 1.321(3) . ?
N12 H12A 0.90(4) . ?
N13 C25 1.341(4) . ?
N13 C29 1.353(4) . ?
N14 C30 1.318(3) . ?
N15 C30 1.336(4) . ?
N15 H15A 0.90(3) . ?
N16 C35 1.343(4) . ?
N16 C31 1.346(4) . ?
N17 C36 1.344(3) . ?
N18 C36 1.322(4) . ?
N18 H18A 0.89(3) . ?
C1 C2 1.385(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.375(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.389(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.388(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.477(4) . ?
C7 C8 1.383(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.386(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.372(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.382(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.475(4) . ?
C13 C14 1.381(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.377(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.386(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.459(4) . ?
C19 C20 1.393(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.381(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.386(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.391(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.483(4) . ?
C25 C26 1.389(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.378(5) . ?
C26 H26 0.9500 . ?
C27 C28 1.392(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.380(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.483(4) . ?
C31 C32 1.390(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.378(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.388(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.391(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.479(4) . ?
C1M H2M 0.9800 . ?
C1M H3M 0.9800 . ?
C1M H4M 0.9800 . ?
O2M C2M 1.396(5) . ?
O2M H5M 0.8400 . ?
C2M H6M 0.9800 . ?
C2M H7M 0.9800 . ?
C2M H8M 0.9800 . ?
O3M C3M 1.435(5) . ?
O3M H9M 0.8400 . ?
C3M H10M 0.9800 . ?
C3M H11M 0.9800 . ?
C3M H12M 0.9800 . ?
O4M C4M 1.276(11) . ?
O4M H13M 0.8400 . ?
C4M H14M 0.9800 . ?
C4M H15M 0.9800 . ?
C4M H16M 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ni1 O2 83.91(7) . . ?
O4 Ni1 N10 178.74(8) . 2_556 ?
O2 Ni1 N10 95.16(8) . 2_556 ?
O4 Ni1 N11 102.37(8) . 2_556 ?
O2 Ni1 N11 172.77(8) . 2_556 ?
N10 Ni1 N11 78.50(9) 2_556 2_556 ?
O4 Ni1 O1 96.55(7) . . ?
O2 Ni1 O1 96.87(7) . . ?
N10 Ni1 O1 84.40(8) 2_556 . ?
N11 Ni1 O1 86.05(8) 2_556 . ?
O4 Ni1 N17 88.36(8) . . ?
O2 Ni1 N17 83.05(8) . . ?
N10 Ni1 N17 90.68(9) 2_556 . ?
N11 Ni1 N17 93.47(9) 2_556 . ?
O1 Ni1 N17 175.06(7) . . ?
O3 Ni2 O5 86.63(8) . . ?
O3 Ni2 N16 91.08(9) . . ?
O5 Ni2 N16 175.01(9) . . ?
O3 Ni2 N17 169.24(8) . . ?
O5 Ni2 N17 103.72(8) . . ?
N16 Ni2 N17 78.82(9) . . ?
O3 Ni2 O2 91.60(8) . . ?
O5 Ni2 O2 97.00(8) . . ?
N16 Ni2 O2 87.48(8) . . ?
N17 Ni2 O2 84.33(8) . . ?
O3 Ni2 Cl1 95.38(6) . . ?
O5 Ni2 Cl1 84.12(6) . . ?
N16 Ni2 Cl1 91.69(7) . . ?
N17 Ni2 Cl1 88.67(7) . . ?
O2 Ni2 Cl1 172.98(5) . . ?
N14 Ni3 O6 104.31(8) . . ?
N14 Ni3 O1 170.76(8) . 2_556 ?
O6 Ni3 O1 82.49(7) . 2_556 ?
N14 Ni3 N13 78.24(9) . . ?
O6 Ni3 N13 173.75(9) . . ?
O1 Ni3 N13 95.64(8) 2_556 . ?
N14 Ni3 O1M 87.74(9) . . ?
O6 Ni3 O1M 86.34(8) . . ?
O1 Ni3 O1M 99.06(9) 2_556 . ?
N13 Ni3 O1M 88.08(9) . . ?
N14 Ni3 N11 89.73(9) . . ?
O6 Ni3 N11 87.41(8) . . ?
O1 Ni3 N11 84.28(8) 2_556 . ?
N13 Ni3 N11 98.36(9) . . ?
O1M Ni3 N11 172.46(9) . . ?
O4 Ni4 N5 89.97(9) . . ?
O4 Ni4 N12 84.44(9) . . ?
N5 Ni4 N12 174.14(10) . . ?
O4 Ni4 N4 172.22(9) . . ?
N5 Ni4 N4 82.77(10) . . ?
N12 Ni4 N4 102.89(10) . . ?
O5 Ni5 N15 84.52(10) . . ?
O5 Ni5 N8 90.34(9) . . ?
N15 Ni5 N8 173.30(11) . . ?
O5 Ni5 N7 170.12(10) . . ?
N15 Ni5 N7 102.09(11) . . ?
N8 Ni5 N7 83.57(11) . . ?
O6 Ni6 N18 84.70(9) . . ?
O6 Ni6 N2 89.69(9) . 2_556 ?
N18 Ni6 N2 174.26(10) . 2_556 ?
O6 Ni6 N1 172.83(10) . 2_556 ?
N18 Ni6 N1 102.40(10) . 2_556 ?
N2 Ni6 N1 83.19(10) 2_556 2_556 ?
N2 O1 Ni3 109.92(15) . 2_556 ?
N2 O1 Ni1 115.38(14) . . ?
Ni3 O1 Ni1 95.88(7) 2_556 . ?
N5 O2 Ni1 112.03(15) . . ?
N5 O2 Ni2 107.79(14) . . ?
Ni1 O2 Ni2 98.10(8) . . ?
N8 O3 Ni2 115.79(16) . . ?
N11 O4 Ni4 114.23(14) . . ?
N11 O4 Ni1 127.11(14) . . ?
Ni4 O4 Ni1 118.02(9) . . ?
N14 O5 Ni5 114.48(15) . . ?
N14 O5 Ni2 124.59(15) . . ?
Ni5 O5 Ni2 120.32(10) . . ?
N17 O6 Ni6 114.48(14) . . ?
N17 O6 Ni3 125.01(14) . . ?
Ni6 O6 Ni3 115.92(9) . . ?
C1M O1M Ni3 135.1(3) . . ?
C1M O1M H1M 104(2) . . ?
Ni3 O1M H1M 107(2) . . ?
C1 N1 C5 118.8(3) . . ?
C1 N1 Ni6 127.0(2) . 2_556 ?
C5 N1 Ni6 114.09(19) . 2_556 ?
C6 N2 O1 117.5(2) . . ?
C6 N2 Ni6 118.27(19) . 2_556 ?
O1 N2 Ni6 124.19(17) . 2_556 ?
C6 N3 H3A 121.4(19) . . ?
C6 N3 H3B 125.1(19) . . ?
H3A N3 H3B 111.3(15) . . ?
C7 N4 C11 118.4(2) . . ?
C7 N4 Ni4 127.8(2) . . ?
C11 N4 Ni4 113.81(18) . . ?
C12 N5 O2 117.4(2) . . ?
C12 N5 Ni4 118.81(19) . . ?
O2 N5 Ni4 123.78(16) . . ?
C12 N6 H6A 116(2) . . ?
C12 N6 H6B 121(2) . . ?
H6A N6 H6B 113.7(16) . . ?
C13 N7 C17 118.4(3) . . ?
C13 N7 Ni5 127.8(2) . . ?
C17 N7 Ni5 113.7(2) . . ?
C18 N8 O3 118.1(2) . . ?
C18 N8 Ni5 117.0(2) . . ?
O3 N8 Ni5 124.88(17) . . ?
C18 N9 H9A 115(2) . . ?
C18 N9 H9B 114(2) . . ?
H9A N9 H9B 112.9(16) . . ?
C19 N10 C23 119.5(2) . . ?
C19 N10 Ni1 126.02(19) . 2_556 ?
C23 N10 Ni1 114.41(18) . 2_556 ?
C24 N11 O4 108.9(2) . . ?
C24 N11 Ni1 111.91(17) . 2_556 ?
O4 N11 Ni1 128.29(15) . 2_556 ?
C24 N11 Ni3 110.79(17) . . ?
O4 N11 Ni3 100.79(14) . . ?
Ni1 N11 Ni3 93.20(9) 2_556 . ?
C24 N12 Ni4 111.35(18) . . ?
C24 N12 H12A 114(2) . . ?
Ni4 N12 H12A 133(2) . . ?
C25 N13 C29 118.7(2) . . ?
C25 N13 Ni3 126.82(19) . . ?
C29 N13 Ni3 114.49(18) . . ?
C30 N14 O5 109.9(2) . . ?
C30 N14 Ni3 117.95(19) . . ?
O5 N14 Ni3 131.15(16) . . ?
C30 N15 Ni5 110.84(18) . . ?
C30 N15 H15A 115(2) . . ?
Ni5 N15 H15A 134(2) . . ?
C35 N16 C31 119.0(3) . . ?
C35 N16 Ni2 114.61(19) . . ?
C31 N16 Ni2 126.3(2) . . ?
C36 N17 O6 108.8(2) . . ?
C36 N17 Ni2 109.55(18) . . ?
O6 N17 Ni2 128.43(15) . . ?
C36 N17 Ni1 118.58(17) . . ?
O6 N17 Ni1 97.55(14) . . ?
Ni2 N17 Ni1 93.18(9) . . ?
C36 N18 Ni6 111.54(19) . . ?
C36 N18 H18A 115(2) . . ?
Ni6 N18 H18A 133(2) . . ?
N1 C1 C2 121.6(3) . . ?
N1 C1 H1 119.2 . . ?
C2 C1 H1 119.2 . . ?
C3 C2 C1 119.5(3) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 119.8(3) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 118.2(3) . . ?
C5 C4 H4 120.9 . . ?
C3 C4 H4 120.9 . . ?
N1 C5 C4 122.1(3) . . ?
N1 C5 C6 112.4(2) . . ?
C4 C5 C6 125.4(3) . . ?
N2 C6 N3 124.8(3) . . ?
N2 C6 C5 111.8(2) . . ?
N3 C6 C5 123.4(3) . . ?
N4 C7 C8 122.1(3) . . ?
N4 C7 H7 118.9 . . ?
C8 C7 H7 118.9 . . ?
C7 C8 C9 119.2(3) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C10 C9 C8 119.5(3) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C9 C10 C11 118.4(3) . . ?
C9 C10 H10 120.8 . . ?
C11 C10 H10 120.8 . . ?
N4 C11 C10 122.5(3) . . ?
N4 C11 C12 112.7(2) . . ?
C10 C11 C12 124.7(3) . . ?
N5 C12 N6 125.4(3) . . ?
N5 C12 C11 111.7(2) . . ?
N6 C12 C11 122.8(2) . . ?
N7 C13 C14 121.8(3) . . ?
N7 C13 H13 119.1 . . ?
C14 C13 H13 119.1 . . ?
C15 C14 C13 120.0(3) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 119.0(3) . . ?
C14 C15 H15 120.5 . . ?
C16 C15 H15 120.5 . . ?
C15 C16 C17 118.7(3) . . ?
C15 C16 H16 120.6 . . ?
C17 C16 H16 120.6 . . ?
N7 C17 C16 122.1(3) . . ?
N7 C17 C18 112.4(2) . . ?
C16 C17 C18 125.5(3) . . ?
N8 C18 N9 123.5(3) . . ?
N8 C18 C17 113.1(3) . . ?
N9 C18 C17 123.3(3) . . ?
N10 C19 C20 121.3(3) . . ?
N10 C19 H19 119.4 . . ?
C20 C19 H19 119.4 . . ?
C21 C20 C19 119.3(3) . . ?
C21 C20 H20 120.4 . . ?
C19 C20 H20 120.4 . . ?
C20 C21 C22 119.5(3) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
C21 C22 C23 118.6(3) . . ?
C21 C22 H22 120.7 . . ?
C23 C22 H22 120.7 . . ?
N10 C23 C22 121.8(3) . . ?
N10 C23 C24 114.4(2) . . ?
C22 C23 C24 123.8(2) . . ?
N12 C24 N11 120.2(2) . . ?
N12 C24 C23 125.7(2) . . ?
N11 C24 C23 114.1(2) . . ?
N13 C25 C26 122.2(3) . . ?
N13 C25 H25 118.9 . . ?
C26 C25 H25 118.9 . . ?
C27 C26 C25 118.8(3) . . ?
C27 C26 H26 120.6 . . ?
C25 C26 H26 120.6 . . ?
C26 C27 C28 119.6(3) . . ?
C26 C27 H27 120.2 . . ?
C28 C27 H27 120.2 . . ?
C29 C28 C27 118.5(3) . . ?
C29 C28 H28 120.7 . . ?
C27 C28 H28 120.7 . . ?
N13 C29 C28 122.3(3) . . ?
N13 C29 C30 114.3(2) . . ?
C28 C29 C30 123.4(3) . . ?
N14 C30 N15 120.2(3) . . ?
N14 C30 C29 114.1(2) . . ?
N15 C30 C29 125.7(2) . . ?
N16 C31 C32 121.9(3) . . ?
N16 C31 H31 119.1 . . ?
C32 C31 H31 119.1 . . ?
C33 C32 C31 118.9(3) . . ?
C33 C32 H32 120.6 . . ?
C31 C32 H32 120.6 . . ?
C32 C33 C34 119.7(3) . . ?
C32 C33 H33 120.2 . . ?
C34 C33 H33 120.2 . . ?
C33 C34 C35 118.4(3) . . ?
C33 C34 H34 120.8 . . ?
C35 C34 H34 120.8 . . ?
N16 C35 C34 122.1(3) . . ?
N16 C35 C36 113.9(2) . . ?
C34 C35 C36 124.0(3) . . ?
N18 C36 N17 120.0(3) . . ?
N18 C36 C35 124.9(2) . . ?
N17 C36 C35 115.0(2) . . ?
O1M C1M H2M 109.5 . . ?
O1M C1M H3M 109.5 . . ?
H2M C1M H3M 109.5 . . ?
O1M C1M H4M 109.5 . . ?
H2M C1M H4M 109.5 . . ?
H3M C1M H4M 109.5 . . ?
C2M O2M H5M 109.5 . . ?
O2M C2M H6M 109.5 . . ?
O2M C2M H7M 109.5 . . ?
H6M C2M H7M 109.5 . . ?
O2M C2M H8M 109.5 . . ?
H6M C2M H8M 109.5 . . ?
H7M C2M H8M 109.5 . . ?
C3M O3M H9M 109.5 . . ?
O3M C3M H10M 109.5 . . ?
O3M C3M H11M 109.5 . . ?
H10M C3M H11M 109.5 . . ?
O3M C3M H12M 109.5 . . ?
H10M C3M H12M 109.5 . . ?
H11M C3M H12M 109.5 . . ?
C4M O4M H13M 109.5 . . ?
O4M C4M H14M 109.5 . . ?
O4M C4M H15M 109.5 . . ?
H14M C4M H15M 109.5 . . ?
O4M C4M H16M 109.5 . . ?
H14M C4M H16M 109.5 . . ?
H15M C4M H16M 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
O4 Ni1 O1 N2 -19.44(17) . . . . ?
O2 Ni1 O1 N2 65.18(17) . . . . ?
N10 Ni1 O1 N2 159.72(17) 2_556 . . . ?
N11 Ni1 O1 N2 -121.46(17) 2_556 . . . ?
O4 Ni1 O1 Ni3 95.89(8) . . . 2_556 ?
O2 Ni1 O1 Ni3 -179.49(7) . . . 2_556 ?
N10 Ni1 O1 Ni3 -84.95(8) 2_556 . . 2_556 ?
N11 Ni1 O1 Ni3 -6.13(8) 2_556 . . 2_556 ?
O4 Ni1 O2 N5 32.50(15) . . . . ?
N10 Ni1 O2 N5 -148.35(16) 2_556 . . . ?
O1 Ni1 O2 N5 -63.39(16) . . . . ?
N17 Ni1 O2 N5 121.59(16) . . . . ?
O4 Ni1 O2 Ni2 -80.49(8) . . . . ?
N10 Ni1 O2 Ni2 98.66(9) 2_556 . . . ?
O1 Ni1 O2 Ni2 -176.38(7) . . . . ?
N17 Ni1 O2 Ni2 8.60(8) . . . . ?
O3 Ni2 O2 N5 64.29(15) . . . . ?
O5 Ni2 O2 N5 -22.52(16) . . . . ?
N16 Ni2 O2 N5 155.29(16) . . . . ?
N17 Ni2 O2 N5 -125.69(16) . . . . ?
O3 Ni2 O2 Ni1 -179.38(8) . . . . ?
O5 Ni2 O2 Ni1 93.81(8) . . . . ?
N16 Ni2 O2 Ni1 -88.37(9) . . . . ?
N17 Ni2 O2 Ni1 -9.36(8) . . . . ?
O5 Ni2 O3 N8 11.98(18) . . . . ?
N16 Ni2 O3 N8 -172.46(18) . . . . ?
N17 Ni2 O3 N8 -152.5(4) . . . . ?
O2 Ni2 O3 N8 -84.94(18) . . . . ?
Cl1 Ni2 O3 N8 95.74(17) . . . . ?
N5 Ni4 O4 N11 -170.09(16) . . . . ?
N12 Ni4 O4 N11 8.14(16) . . . . ?
N5 Ni4 O4 Ni1 18.37(12) . . . . ?
N12 Ni4 O4 Ni1 -163.40(12) . . . . ?
O2 Ni1 O4 N11 160.45(19) . . . . ?
N11 Ni1 O4 N11 -15.9(2) 2_556 . . . ?
O1 Ni1 O4 N11 -103.30(18) . . . . ?
N17 Ni1 O4 N11 77.27(19) . . . . ?
O2 Ni1 O4 Ni4 -29.24(11) . . . . ?
N11 Ni1 O4 Ni4 154.38(11) 2_556 . . . ?
O1 Ni1 O4 Ni4 67.01(11) . . . . ?
N17 Ni1 O4 Ni4 -112.42(11) . . . . ?
N15 Ni5 O5 N14 2.70(18) . . . . ?
N8 Ni5 O5 N14 -172.99(18) . . . . ?
N15 Ni5 O5 Ni2 174.20(14) . . . . ?
N8 Ni5 O5 Ni2 -1.49(13) . . . . ?
O3 Ni2 O5 N14 166.0(2) . . . . ?
N17 Ni2 O5 N14 -17.0(2) . . . . ?
O2 Ni2 O5 N14 -102.82(19) . . . . ?
Cl1 Ni2 O5 N14 70.21(18) . . . . ?
O3 Ni2 O5 Ni5 -4.62(12) . . . . ?
N17 Ni2 O5 Ni5 172.43(12) . . . . ?
O2 Ni2 O5 Ni5 86.58(12) . . . . ?
Cl1 Ni2 O5 Ni5 -100.39(11) . . . . ?
N18 Ni6 O6 N17 -5.58(17) . . . . ?
N2 Ni6 O6 N17 175.65(17) 2_556 . . . ?
N18 Ni6 O6 Ni3 151.69(12) . . . . ?
N2 Ni6 O6 Ni3 -27.08(12) 2_556 . . . ?
N14 Ni3 O6 N17 6.1(2) . . . . ?
O1 Ni3 O6 N17 -167.54(19) 2_556 . . . ?
O1M Ni3 O6 N17 92.81(19) . . . . ?
N11 Ni3 O6 N17 -82.98(18) . . . . ?
N14 Ni3 O6 Ni6 -148.49(11) . . . . ?
O1 Ni3 O6 Ni6 37.88(10) 2_556 . . . ?
O1M Ni3 O6 Ni6 -61.76(12) . . . . ?
N11 Ni3 O6 Ni6 122.45(11) . . . . ?
N14 Ni3 O1M C1M -174.0(4) . . . . ?
O6 Ni3 O1M C1M 81.5(4) . . . . ?
O1 Ni3 O1M C1M -0.3(4) 2_556 . . . ?
N13 Ni3 O1M C1M -95.7(4) . . . . ?
Ni3 O1 N2 C6 146.3(2) 2_556 . . . ?
Ni1 O1 N2 C6 -106.7(2) . . . . ?
Ni3 O1 N2 Ni6 -31.3(2) 2_556 . . 2_556 ?
Ni1 O1 N2 Ni6 75.7(2) . . . 2_556 ?
N5 Ni4 N4 C7 175.9(3) . . . . ?
N12 Ni4 N4 C7 -2.6(3) . . . . ?
N5 Ni4 N4 C11 -2.3(2) . . . . ?
N12 Ni4 N4 C11 179.23(19) . . . . ?
Ni1 O2 N5 C12 151.20(19) . . . . ?
Ni2 O2 N5 C12 -102.0(2) . . . . ?
Ni1 O2 N5 Ni4 -31.2(2) . . . . ?
Ni2 O2 N5 Ni4 75.65(19) . . . . ?
O4 Ni4 N5 C12 -173.8(2) . . . . ?
N4 Ni4 N5 C12 3.4(2) . . . . ?
O4 Ni4 N5 O2 8.6(2) . . . . ?
N4 Ni4 N5 O2 -174.2(2) . . . . ?
N15 Ni5 N7 C13 3.2(3) . . . . ?
N8 Ni5 N7 C13 179.6(3) . . . . ?
N15 Ni5 N7 C17 178.9(2) . . . . ?
N8 Ni5 N7 C17 -4.8(2) . . . . ?
Ni2 O3 N8 C18 163.6(2) . . . . ?
Ni2 O3 N8 Ni5 -17.7(3) . . . . ?
O5 Ni5 N8 C18 -169.4(2) . . . . ?
N7 Ni5 N8 C18 2.8(2) . . . . ?
O5 Ni5 N8 O3 12.0(2) . . . . ?
N7 Ni5 N8 O3 -175.8(2) . . . . ?
Ni4 O4 N11 C24 -10.1(2) . . . . ?
Ni1 O4 N11 C24 160.53(17) . . . . ?
Ni4 O4 N11 Ni1 -150.66(13) . . . 2_556 ?
Ni1 O4 N11 Ni1 20.0(3) . . . 2_556 ?
Ni4 O4 N11 Ni3 106.46(12) . . . . ?
Ni1 O4 N11 Ni3 -82.91(17) . . . . ?
N14 Ni3 N11 C24 63.97(19) . . . . ?
O6 Ni3 N11 C24 168.30(18) . . . . ?
O1 Ni3 N11 C24 -108.99(18) 2_556 . . . ?
N13 Ni3 N11 C24 -14.10(19) . . . . ?
N14 Ni3 N11 O4 -51.16(14) . . . . ?
O6 Ni3 N11 O4 53.18(13) . . . . ?
O1 Ni3 N11 O4 135.89(14) 2_556 . . . ?
N13 Ni3 N11 O4 -129.23(13) . . . . ?
N14 Ni3 N11 Ni1 178.86(9) . . . 2_556 ?
O6 Ni3 N11 Ni1 -76.80(8) . . . 2_556 ?
O1 Ni3 N11 Ni1 5.91(8) 2_556 . . 2_556 ?
N13 Ni3 N11 Ni1 100.79(9) . . . 2_556 ?
O4 Ni4 N12 C24 -4.25(19) . . . . ?
N4 Ni4 N12 C24 178.40(19) . . . . ?
N14 Ni3 N13 C25 174.5(3) . . . . ?
O1 Ni3 N13 C25 -12.6(2) 2_556 . . . ?
O1M Ni3 N13 C25 86.4(2) . . . . ?
N11 Ni3 N13 C25 -97.6(2) . . . . ?
N14 Ni3 N13 C29 -6.4(2) . . . . ?
O1 Ni3 N13 C29 166.6(2) 2_556 . . . ?
O1M Ni3 N13 C29 -94.5(2) . . . . ?
N11 Ni3 N13 C29 81.6(2) . . . . ?
Ni5 O5 N14 C30 -3.2(3) . . . . ?
Ni2 O5 N14 C30 -174.27(18) . . . . ?
Ni5 O5 N14 Ni3 -171.07(13) . . . . ?
Ni2 O5 N14 Ni3 17.8(3) . . . . ?
O6 Ni3 N14 C30 -177.0(2) . . . . ?
N13 Ni3 N14 C30 8.8(2) . . . . ?
O1M Ni3 N14 C30 97.3(2) . . . . ?
N11 Ni3 N14 C30 -89.8(2) . . . . ?
O6 Ni3 N14 O5 -9.9(2) . . . . ?
N13 Ni3 N14 O5 175.9(2) . . . . ?
O1M Ni3 N14 O5 -95.6(2) . . . . ?
N11 Ni3 N14 O5 77.3(2) . . . . ?
O5 Ni5 N15 C30 -1.6(2) . . . . ?
N7 Ni5 N15 C30 -174.1(2) . . . . ?
O3 Ni2 N16 C35 -166.9(2) . . . . ?
N17 Ni2 N16 C35 16.9(2) . . . . ?
O2 Ni2 N16 C35 101.6(2) . . . . ?
Cl1 Ni2 N16 C35 -71.4(2) . . . . ?
O3 Ni2 N16 C31 9.2(2) . . . . ?
N17 Ni2 N16 C31 -167.1(3) . . . . ?
O2 Ni2 N16 C31 -82.3(2) . . . . ?
Cl1 Ni2 N16 C31 104.6(2) . . . . ?
Ni6 O6 N17 C36 7.3(2) . . . . ?
Ni3 O6 N17 C36 -147.57(18) . . . . ?
Ni6 O6 N17 Ni2 143.46(14) . . . . ?
Ni3 O6 N17 Ni2 -11.4(3) . . . . ?
Ni6 O6 N17 Ni1 -116.37(12) . . . . ?
Ni3 O6 N17 Ni1 88.74(15) . . . . ?
O3 Ni2 N17 C36 -45.5(6) . . . . ?
O5 Ni2 N17 C36 150.53(18) . . . . ?
N16 Ni2 N17 C36 -25.07(18) . . . . ?
O2 Ni2 N17 C36 -113.62(18) . . . . ?
Cl1 Ni2 N17 C36 66.92(18) . . . . ?
O3 Ni2 N17 O6 178.7(4) . . . . ?
O5 Ni2 N17 O6 14.7(2) . . . . ?
N16 Ni2 N17 O6 -160.9(2) . . . . ?
O2 Ni2 N17 O6 110.5(2) . . . . ?
Cl1 Ni2 N17 O6 -69.0(2) . . . . ?
O3 Ni2 N17 Ni1 76.4(5) . . . . ?
O5 Ni2 N17 Ni1 -87.59(9) . . . . ?
N16 Ni2 N17 Ni1 96.81(9) . . . . ?
O2 Ni2 N17 Ni1 8.26(7) . . . . ?
Cl1 Ni2 N17 Ni1 -171.20(6) . . . . ?
O4 Ni1 N17 C36 -170.5(2) . . . . ?
O2 Ni1 N17 C36 105.5(2) . . . . ?
N10 Ni1 N17 C36 10.3(2) 2_556 . . . ?
N11 Ni1 N17 C36 -68.2(2) 2_556 . . . ?
O4 Ni1 N17 O6 -54.25(13) . . . . ?
O2 Ni1 N17 O6 -138.31(14) . . . . ?
N10 Ni1 N17 O6 126.57(14) 2_556 . . . ?
N11 Ni1 N17 O6 48.05(14) 2_556 . . . ?
O4 Ni1 N17 Ni2 75.19(8) . . . . ?
O2 Ni1 N17 Ni2 -8.87(8) . . . . ?
N10 Ni1 N17 Ni2 -103.98(9) 2_556 . . . ?
N11 Ni1 N17 Ni2 177.49(8) 2_556 . . . ?
O6 Ni6 N18 C36 2.5(2) . . . . ?
N1 Ni6 N18 C36 -178.57(19) 2_556 . . . ?
C5 N1 C1 C2 0.2(5) . . . . ?
Ni6 N1 C1 C2 -176.7(3) 2_556 . . . ?
N1 C1 C2 C3 -1.1(5) . . . . ?
C1 C2 C3 C4 1.0(6) . . . . ?
C2 C3 C4 C5 -0.2(5) . . . . ?
C1 N1 C5 C4 0.6(4) . . . . ?
Ni6 N1 C5 C4 178.0(2) 2_556 . . . ?
C1 N1 C5 C6 -176.5(3) . . . . ?
Ni6 N1 C5 C6 0.9(3) 2_556 . . . ?
C3 C4 C5 N1 -0.6(5) . . . . ?
C3 C4 C5 C6 176.1(3) . . . . ?
O1 N2 C6 N3 -3.1(4) . . . . ?
Ni6 N2 C6 N3 174.7(2) 2_556 . . . ?
O1 N2 C6 C5 176.3(2) . . . . ?
Ni6 N2 C6 C5 -5.9(3) 2_556 . . . ?
N1 C5 C6 N2 3.1(3) . . . . ?
C4 C5 C6 N2 -173.9(3) . . . . ?
N1 C5 C6 N3 -177.5(3) . . . . ?
C4 C5 C6 N3 5.5(5) . . . . ?
C11 N4 C7 C8 0.3(5) . . . . ?
Ni4 N4 C7 C8 -177.8(3) . . . . ?
N4 C7 C8 C9 0.4(6) . . . . ?
C7 C8 C9 C10 -1.3(6) . . . . ?
C8 C9 C10 C11 1.4(5) . . . . ?
C7 N4 C11 C10 -0.2(4) . . . . ?
Ni4 N4 C11 C10 178.2(2) . . . . ?
C7 N4 C11 C12 -177.3(3) . . . . ?
Ni4 N4 C11 C12 1.1(3) . . . . ?
C9 C10 C11 N4 -0.7(5) . . . . ?
C9 C10 C11 C12 176.1(3) . . . . ?
O2 N5 C12 N6 -1.4(4) . . . . ?
Ni4 N5 C12 N6 -179.2(2) . . . . ?
O2 N5 C12 C11 174.2(2) . . . . ?
Ni4 N5 C12 C11 -3.5(3) . . . . ?
N4 C11 C12 N5 1.4(3) . . . . ?
C10 C11 C12 N5 -175.6(3) . . . . ?
N4 C11 C12 N6 177.2(3) . . . . ?
C10 C11 C12 N6 0.2(4) . . . . ?
C17 N7 C13 C14 -1.8(5) . . . . ?
Ni5 N7 C13 C14 173.7(3) . . . . ?
N7 C13 C14 C15 0.1(6) . . . . ?
C13 C14 C15 C16 1.3(6) . . . . ?
C14 C15 C16 C17 -1.0(5) . . . . ?
C13 N7 C17 C16 2.1(4) . . . . ?
Ni5 N7 C17 C16 -174.0(2) . . . . ?
C13 N7 C17 C18 -178.2(3) . . . . ?
Ni5 N7 C17 C18 5.7(3) . . . . ?
C15 C16 C17 N7 -0.7(5) . . . . ?
C15 C16 C17 C18 179.6(3) . . . . ?
O3 N8 C18 N9 3.3(4) . . . . ?
Ni5 N8 C18 N9 -175.4(2) . . . . ?
O3 N8 C18 C17 178.3(2) . . . . ?
Ni5 N8 C18 C17 -0.4(3) . . . . ?
N7 C17 C18 N8 -3.5(4) . . . . ?
C16 C17 C18 N8 176.2(3) . . . . ?
N7 C17 C18 N9 171.5(3) . . . . ?
C16 C17 C18 N9 -8.8(5) . . . . ?
C23 N10 C19 C20 -0.9(4) . . . . ?
Ni1 N10 C19 C20 177.4(2) 2_556 . . . ?
N10 C19 C20 C21 -1.3(5) . . . . ?
C19 C20 C21 C22 1.7(5) . . . . ?
C20 C21 C22 C23 -0.1(5) . . . . ?
C19 N10 C23 C22 2.7(4) . . . . ?
Ni1 N10 C23 C22 -175.8(2) 2_556 . . . ?
C19 N10 C23 C24 -175.1(2) . . . . ?
Ni1 N10 C23 C24 6.4(3) 2_556 . . . ?
C21 C22 C23 N10 -2.2(4) . . . . ?
C21 C22 C23 C24 175.4(3) . . . . ?
Ni4 N12 C24 N11 -0.7(3) . . . . ?
Ni4 N12 C24 C23 -179.4(2) . . . . ?
O4 N11 C24 N12 6.9(3) . . . . ?
Ni1 N11 C24 N12 154.4(2) 2_556 . . . ?
Ni3 N11 C24 N12 -103.1(2) . . . . ?
O4 N11 C24 C23 -174.2(2) . . . . ?
Ni1 N11 C24 C23 -26.7(3) 2_556 . . . ?
Ni3 N11 C24 C23 75.8(2) . . . . ?
N10 C23 C24 N12 -167.3(3) . . . . ?
C22 C23 C24 N12 14.9(4) . . . . ?
N10 C23 C24 N11 13.9(3) . . . . ?
C22 C23 C24 N11 -163.9(3) . . . . ?
C29 N13 C25 C26 -1.7(4) . . . . ?
Ni3 N13 C25 C26 177.5(2) . . . . ?
N13 C25 C26 C27 0.5(5) . . . . ?
C25 C26 C27 C28 0.6(5) . . . . ?
C26 C27 C28 C29 -0.5(5) . . . . ?
C25 N13 C29 C28 1.8(4) . . . . ?
Ni3 N13 C29 C28 -177.4(2) . . . . ?
C25 N13 C29 C30 -177.3(3) . . . . ?
Ni3 N13 C29 C30 3.5(3) . . . . ?
C27 C28 C29 N13 -0.8(5) . . . . ?
C27 C28 C29 C30 178.2(3) . . . . ?
O5 N14 C30 N15 2.0(4) . . . . ?
Ni3 N14 C30 N15 171.6(2) . . . . ?
O5 N14 C30 C29 -179.2(2) . . . . ?
Ni3 N14 C30 C29 -9.5(3) . . . . ?
Ni5 N15 C30 N14 0.1(3) . . . . ?
Ni5 N15 C30 C29 -178.6(2) . . . . ?
N13 C29 C30 N14 3.6(4) . . . . ?
C28 C29 C30 N14 -175.4(3) . . . . ?
N13 C29 C30 N15 -177.5(3) . . . . ?
C28 C29 C30 N15 3.4(5) . . . . ?
C35 N16 C31 C32 1.5(4) . . . . ?
Ni2 N16 C31 C32 -174.5(2) . . . . ?
N16 C31 C32 C33 0.5(5) . . . . ?
C31 C32 C33 C34 -1.3(5) . . . . ?
C32 C33 C34 C35 0.2(5) . . . . ?
C31 N16 C35 C34 -2.7(4) . . . . ?
Ni2 N16 C35 C34 173.7(2) . . . . ?
C31 N16 C35 C36 177.5(2) . . . . ?
Ni2 N16 C35 C36 -6.1(3) . . . . ?
C33 C34 C35 N16 1.9(4) . . . . ?
C33 C34 C35 C36 -178.3(3) . . . . ?
Ni6 N18 C36 N17 1.3(3) . . . . ?
Ni6 N18 C36 C35 -178.5(2) . . . . ?
O6 N17 C36 N18 -5.6(3) . . . . ?
Ni2 N17 C36 N18 -150.4(2) . . . . ?
Ni1 N17 C36 N18 104.5(3) . . . . ?
O6 N17 C36 C35 174.3(2) . . . . ?
Ni2 N17 C36 C35 29.5(3) . . . . ?
Ni1 N17 C36 C35 -75.6(3) . . . . ?
N16 C35 C36 N18 163.4(3) . . . . ?
C34 C35 C36 N18 -16.5(4) . . . . ?
N16 C35 C36 N17 -16.5(4) . . . . ?
C34 C35 C36 N17 163.7(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1M H1M Cl1 0.96(4) 2.27(3) 3.199(3) 166(3) .
N3 H3B Cl3 0.90(3) 2.36(3) 3.246(3) 167(3) 2_655
N6 H6B Cl3 0.89(3) 2.58(2) 3.357(3) 145(3) 2_655
N9 H9B Cl3 0.90(3) 2.421(16) 3.282(3) 160(3) .
N12 H12A Cl2 0.90(4) 2.62(3) 3.503(2) 171(3) .
N15 H15A O3M 0.90(3) 2.28(3) 3.175(3) 171(3) .
N18 H18A O2M 0.89(3) 2.344(18) 3.170(3) 153(3) .
O2M H5M Cl2 0.84 2.23 3.054(3) 168.4 2_556
O3M H9M Cl1 0.84 2.42 3.237(3) 163.5 2_565

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        29.13
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.213
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.114

# ===== END ===== #