# Electronic Supplementary Material (ESI) for RSC Advances
# This journal is © The Royal Society of Chemistry 2012


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#  This CIF contains data from an original supplementary publication 
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#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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data_11jlm001_0m
_database_code_depnum_ccdc_archive 'CCDC 817179'
#TrackingRef '- NiN6-0-D.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H32 N8 Ni O4 S2, 2(N O3), 4(H2 O)'
_chemical_formula_sum            'C28 H40 N10 Ni O14 S2'
_chemical_formula_weight         863.53

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   24.196(3)
_cell_length_b                   9.5392(12)
_cell_length_c                   16.684(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.545(2)
_cell_angle_gamma                90.00
_cell_volume                     3772.9(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5160
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      30.29

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1800
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6625
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_process_details   'Apex2 v2011.2-0 (Bruker, 2011)'

_exptl_special_details           
;
Reflection -1 1 1 was obstructed by the beam stop and was omitted from
the refinement.
The methoxy methyl group is disordered over two equally occupied
positions. In one of the two positions the methyl group is in close
contact with its symmetry equivalent in a neighboring molecule, which
is the cause of the disorder.
;

_diffrn_ambient_temperature      100(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 AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41409
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.70
_diffrn_reflns_theta_max         31.37
_reflns_number_total             5861
_reflns_number_gt                4754
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Apex2 v2011.2-0 (Bruker, 2011)'
_computing_cell_refinement       'Apex2 v2011.2-0'
_computing_data_reduction        'Apex2 v2011.2-0'
_computing_structure_solution    
'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL 6.14'
_computing_molecular_graphics    'SHELXTL 6.14'
_computing_publication_material  'SHELXTL 6.14'

_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^)+(0.0415P)^2^+4.8385P] 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         5861
_refine_ls_number_parameters     274
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0380
_refine_ls_wR_factor_ref         0.1003
_refine_ls_wR_factor_gt          0.0895
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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 0.5000 0.45112(3) 0.7500 0.01921(8) Uani 1 2 d S . .
C1 C 0.38630(7) 0.30370(17) 0.69131(10) 0.0227(3) Uani 1 1 d . . .
C2 C 0.32709(8) 0.1328(2) 0.73953(12) 0.0348(4) Uani 1 1 d . . .
H2A H 0.3178 0.1834 0.7863 0.052 Uiso 1 1 calc R . .
H2B H 0.3608 0.0755 0.7580 0.052 Uiso 1 1 calc R . .
H2C H 0.2954 0.0722 0.7154 0.052 Uiso 1 1 calc R . .
C3 C 0.29293(8) 0.2622(2) 0.60702(11) 0.0349(4) Uani 1 1 d . . .
H3A H 0.3055 0.2341 0.5570 0.052 Uiso 1 1 calc R . .
H3B H 0.2842 0.3626 0.6047 0.052 Uiso 1 1 calc R . .
H3C H 0.2591 0.2089 0.6118 0.052 Uiso 1 1 calc R . .
C4 C 0.44771(7) 0.55180(17) 0.58032(10) 0.0242(3) Uani 1 1 d . . .
H4 H 0.4168 0.5533 0.5352 0.029 Uiso 1 1 calc R . .
C5 C 0.54296(7) 0.65870(16) 0.64387(9) 0.0205(3) Uani 1 1 d . . .
C6 C 0.49470(7) 0.64386(17) 0.57678(9) 0.0210(3) Uani 1 1 d . . .
C7 C 0.49262(7) 0.72340(17) 0.50743(10) 0.0237(3) Uani 1 1 d . . .
H7 H 0.4607 0.7153 0.4641 0.028 Uiso 1 1 calc R . .
C8 C 0.53646(7) 0.81714(17) 0.49829(9) 0.0222(3) Uani 1 1 d . . .
C9 C 0.53413(7) 0.90270(17) 0.42873(10) 0.0245(3) Uani 1 1 d . . .
H9 H 0.5024 0.8982 0.3849 0.029 Uiso 1 1 calc R . .
C10 C 0.57786(8) 0.99273(18) 0.42433(10) 0.0255(3) Uani 1 1 d . A .
C11 C 0.62529(8) 0.9986(2) 0.48878(11) 0.0303(4) Uani 1 1 d . . .
H11 H 0.6554 1.0606 0.4852 0.036 Uiso 1 1 calc R . .
C12 C 0.62835(8) 0.9152(2) 0.55693(11) 0.0295(4) Uani 1 1 d . . .
H12 H 0.6606 0.9190 0.6000 0.035 Uiso 1 1 calc R . .
C13 C 0.58374(7) 0.82501(17) 0.56223(9) 0.0231(3) Uani 1 1 d . . .
C14 C 0.52997(17) 1.0733(4) 0.2930(2) 0.0320(8) Uani 0.50 1 d P A -1
H14A H 0.4949 1.0878 0.3130 0.048 Uiso 0.50 1 calc PR A -1
H14B H 0.5288 0.9817 0.2662 0.048 Uiso 0.50 1 calc PR A -1
H14C H 0.5340 1.1471 0.2538 0.048 Uiso 0.50 1 calc PR A -1
C14B C 0.61731(16) 1.1733(4) 0.3539(2) 0.0287(7) Uani 0.50 1 d P A 2
H15D H 0.6515 1.1233 0.3472 0.043 Uiso 0.50 1 calc PR A 2
H15E H 0.6253 1.2286 0.4044 0.043 Uiso 0.50 1 calc PR A 2
H15F H 0.6050 1.2358 0.3071 0.043 Uiso 0.50 1 calc PR A 2
N1 N 0.33779(6) 0.23358(16) 0.67818(9) 0.0269(3) Uani 1 1 d . . .
N2 N 0.39498(6) 0.39276(15) 0.63099(8) 0.0227(3) Uani 1 1 d . . .
H2 H 0.3689 0.4022 0.5863 0.027 Uiso 1 1 calc R . .
N3 N 0.44444(5) 0.46789(14) 0.63977(8) 0.0198(2) Uani 1 1 d . . .
N4 N 0.58486(6) 0.74426(15) 0.63119(8) 0.0242(3) Uani 1 1 d . . .
H4A H 0.6153 0.7489 0.6700 0.029 Uiso 1 1 calc R . .
N5 N 0.31479(6) 0.54515(17) 0.42857(9) 0.0312(3) Uani 1 1 d . . .
O1 O 0.54842(5) 0.60104(12) 0.71219(7) 0.0242(2) Uani 1 1 d . . .
O2 O 0.57528(6) 1.07799(14) 0.35812(8) 0.0323(3) Uani 1 1 d . . .
O3 O 0.29250(7) 0.55472(16) 0.35495(9) 0.0445(4) Uani 1 1 d . . .
O4 O 0.33330(6) 0.43032(15) 0.45858(8) 0.0351(3) Uani 1 1 d . . .
O5 O 0.31931(7) 0.65289(17) 0.47300(9) 0.0453(4) Uani 1 1 d . . .
O6 O 0.26237(8) 0.64193(19) 0.60854(9) 0.0475(4) Uani 1 1 d D . .
H6A H 0.2846(11) 0.639(3) 0.5745(16) 0.071 Uiso 1 1 d D . .
H6B H 0.2388(11) 0.709(3) 0.5918(18) 0.071 Uiso 1 1 d D . .
O7 O 0.31160(6) 0.29873(19) 0.27236(9) 0.0437(4) Uani 1 1 d D . .
H7A H 0.3005(11) 0.298(3) 0.2197(11) 0.066 Uiso 1 1 d D . .
H7B H 0.3080(12) 0.383(2) 0.2907(18) 0.066 Uiso 1 1 d D . .
S1 S 0.435090(18) 0.28328(5) 0.77893(3) 0.02732(10) Uani 1 1 d . . .

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 0.02338(14) 0.01853(14) 0.01424(13) 0.000 0.00021(10) 0.000
C1 0.0243(7) 0.0226(7) 0.0210(7) 0.0010(6) 0.0043(6) -0.0001(6)
C2 0.0311(9) 0.0404(10) 0.0316(9) 0.0108(8) 0.0031(7) -0.0093(8)
C3 0.0266(9) 0.0470(11) 0.0279(9) 0.0087(8) -0.0019(7) -0.0093(8)
C4 0.0240(7) 0.0281(8) 0.0183(7) 0.0024(6) -0.0007(6) -0.0026(6)
C5 0.0248(7) 0.0199(7) 0.0160(6) -0.0021(5) 0.0020(5) 0.0000(6)
C6 0.0244(7) 0.0220(7) 0.0158(6) -0.0006(5) 0.0018(5) 0.0004(6)
C7 0.0269(8) 0.0248(7) 0.0172(7) 0.0008(6) -0.0012(6) -0.0014(6)
C8 0.0290(8) 0.0203(7) 0.0168(7) -0.0008(5) 0.0029(6) -0.0003(6)
C9 0.0308(8) 0.0230(7) 0.0183(7) 0.0015(6) 0.0017(6) -0.0015(6)
C10 0.0358(9) 0.0212(7) 0.0195(7) 0.0020(6) 0.0053(6) -0.0014(6)
C11 0.0359(9) 0.0276(8) 0.0268(8) 0.0011(7) 0.0049(7) -0.0091(7)
C12 0.0314(9) 0.0322(9) 0.0226(8) 0.0014(7) 0.0001(6) -0.0086(7)
C13 0.0296(8) 0.0222(7) 0.0167(7) 0.0006(6) 0.0026(6) -0.0021(6)
C14 0.048(2) 0.0241(16) 0.0229(16) 0.0055(13) 0.0060(15) 0.0013(14)
C14B 0.0382(19) 0.0234(15) 0.0248(16) 0.0039(12) 0.0069(14) -0.0027(14)
N1 0.0250(7) 0.0326(8) 0.0223(7) 0.0043(6) 0.0026(5) -0.0053(6)
N2 0.0220(6) 0.0265(7) 0.0175(6) 0.0029(5) -0.0010(5) -0.0037(5)
N3 0.0201(6) 0.0205(6) 0.0182(6) -0.0016(5) 0.0025(5) -0.0008(5)
N4 0.0264(7) 0.0276(7) 0.0168(6) 0.0009(5) -0.0001(5) -0.0057(5)
N5 0.0280(7) 0.0392(9) 0.0243(7) -0.0016(6) 0.0001(6) -0.0034(6)
O1 0.0302(6) 0.0253(6) 0.0153(5) 0.0027(4) 0.0004(4) -0.0044(5)
O2 0.0451(8) 0.0271(6) 0.0238(6) 0.0062(5) 0.0049(5) -0.0068(5)
O3 0.0537(9) 0.0476(9) 0.0251(7) 0.0043(6) -0.0088(6) -0.0040(7)
O4 0.0386(7) 0.0374(7) 0.0257(6) 0.0028(5) -0.0020(5) -0.0046(6)
O5 0.0481(9) 0.0461(9) 0.0377(8) -0.0137(7) -0.0014(6) 0.0076(7)
O6 0.0584(10) 0.0510(10) 0.0299(7) 0.0021(7) 0.0014(7) 0.0130(8)
O7 0.0350(7) 0.0666(11) 0.0255(7) 0.0006(7) -0.0035(6) -0.0072(7)
S1 0.0291(2) 0.0281(2) 0.02141(19) 0.00751(15) -0.00309(15) -0.00470(16)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.0275(12) 2_656 ?
Ni1 O1 2.0276(12) . ?
Ni1 N3 2.0556(13) . ?
Ni1 N3 2.0556(13) 2_656 ?
Ni1 S1 2.3594(5) . ?
Ni1 S1 2.3594(5) 2_656 ?
C1 N1 1.331(2) . ?
C1 N2 1.365(2) . ?
C1 S1 1.6964(16) . ?
C2 N1 1.464(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 N1 1.465(2) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 N3 1.289(2) . ?
C4 C6 1.447(2) . ?
C4 H4 0.9500 . ?
C5 O1 1.2487(18) . ?
C5 N4 1.351(2) . ?
C5 C6 1.454(2) . ?
C6 C7 1.376(2) . ?
C7 C8 1.419(2) . ?
C7 H7 0.9500 . ?
C8 C13 1.401(2) . ?
C8 C9 1.411(2) . ?
C9 C10 1.376(2) . ?
C9 H9 0.9500 . ?
C10 O2 1.363(2) . ?
C10 C11 1.408(2) . ?
C11 C12 1.377(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.397(2) . ?
C12 H12 0.9500 . ?
C13 N4 1.380(2) . ?
C14 O2 1.381(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C14B O2 1.376(4) . ?
C14B H15D 0.9800 . ?
C14B H15E 0.9800 . ?
C14B H15F 0.9800 . ?
N2 N3 1.3775(18) . ?
N2 H2 0.8800 . ?
N4 H4A 0.8800 . ?
N5 O3 1.242(2) . ?
N5 O4 1.250(2) . ?
N5 O5 1.259(2) . ?
O6 H6A 0.857(17) . ?
O6 H6B 0.867(17) . ?
O7 H7A 0.865(17) . ?
O7 H7B 0.874(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 90.29(7) 2_656 . ?
O1 Ni1 N3 84.74(5) 2_656 . ?
O1 Ni1 N3 88.96(5) . . ?
O1 Ni1 N3 88.96(5) 2_656 2_656 ?
O1 Ni1 N3 84.74(5) . 2_656 ?
N3 Ni1 N3 171.08(7) . 2_656 ?
O1 Ni1 S1 88.01(4) 2_656 . ?
O1 Ni1 S1 172.74(3) . . ?
N3 Ni1 S1 83.85(4) . . ?
N3 Ni1 S1 102.28(4) 2_656 . ?
O1 Ni1 S1 172.74(3) 2_656 2_656 ?
O1 Ni1 S1 88.01(4) . 2_656 ?
N3 Ni1 S1 102.28(4) . 2_656 ?
N3 Ni1 S1 83.85(4) 2_656 2_656 ?
S1 Ni1 S1 94.53(3) . 2_656 ?
N1 C1 N2 116.89(14) . . ?
N1 C1 S1 121.53(13) . . ?
N2 C1 S1 121.58(12) . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N3 C4 C6 125.29(14) . . ?
N3 C4 H4 117.4 . . ?
C6 C4 H4 117.4 . . ?
O1 C5 N4 117.62(14) . . ?
O1 C5 C6 125.58(15) . . ?
N4 C5 C6 116.79(14) . . ?
C7 C6 C4 118.16(14) . . ?
C7 C6 C5 118.84(14) . . ?
C4 C6 C5 122.98(14) . . ?
C6 C7 C8 122.38(15) . . ?
C6 C7 H7 118.8 . . ?
C8 C7 H7 118.8 . . ?
C13 C8 C9 119.17(15) . . ?
C13 C8 C7 117.77(14) . . ?
C9 C8 C7 123.06(15) . . ?
C10 C9 C8 120.02(15) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
O2 C10 C9 120.30(15) . . ?
O2 C10 C11 119.56(16) . . ?
C9 C10 C11 120.14(15) . . ?
C12 C11 C10 120.55(16) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C13 119.57(16) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
N4 C13 C12 120.67(15) . . ?
N4 C13 C8 118.78(14) . . ?
C12 C13 C8 120.54(15) . . ?
O2 C14 H14A 109.5 . . ?
O2 C14 H14B 109.5 . . ?
O2 C14 H14C 109.5 . . ?
O2 C14B H15D 109.5 . . ?
O2 C14B H15E 109.5 . . ?
H15D C14B H15E 109.5 . . ?
O2 C14B H15F 109.5 . . ?
H15D C14B H15F 109.5 . . ?
H15E C14B H15F 109.5 . . ?
C1 N1 C2 119.25(14) . . ?
C1 N1 C3 121.73(14) . . ?
C2 N1 C3 118.85(14) . . ?
C1 N2 N3 120.26(13) . . ?
C1 N2 H2 119.9 . . ?
N3 N2 H2 119.9 . . ?
C4 N3 N2 115.28(13) . . ?
C4 N3 Ni1 127.36(11) . . ?
N2 N3 Ni1 116.96(10) . . ?
C5 N4 C13 125.28(14) . . ?
C5 N4 H4A 117.4 . . ?
C13 N4 H4A 117.4 . . ?
O3 N5 O4 120.70(16) . . ?
O3 N5 O5 119.45(17) . . ?
O4 N5 O5 119.85(15) . . ?
C5 O1 Ni1 129.24(10) . . ?
C10 O2 C14B 121.40(19) . . ?
C10 O2 C14 121.2(2) . . ?
C14B O2 C14 117.4(2) . . ?
H6A O6 H6B 106(3) . . ?
H7A O7 H7B 109(3) . . ?
C1 S1 Ni1 97.04(6) . . ?

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
N3 C4 C6 C7 177.60(16) . . . . ?
N3 C4 C6 C5 -4.2(3) . . . . ?
O1 C5 C6 C7 174.55(16) . . . . ?
N4 C5 C6 C7 -4.2(2) . . . . ?
O1 C5 C6 C4 -3.7(3) . . . . ?
N4 C5 C6 C4 177.55(15) . . . . ?
C4 C6 C7 C8 179.73(15) . . . . ?
C5 C6 C7 C8 1.4(2) . . . . ?
C6 C7 C8 C13 1.4(2) . . . . ?
C6 C7 C8 C9 -177.88(16) . . . . ?
C13 C8 C9 C10 -0.2(2) . . . . ?
C7 C8 C9 C10 179.12(16) . . . . ?
C8 C9 C10 O2 -178.50(15) . . . . ?
C8 C9 C10 C11 0.7(3) . . . . ?
O2 C10 C11 C12 178.85(17) . . . . ?
C9 C10 C11 C12 -0.4(3) . . . . ?
C10 C11 C12 C13 -0.5(3) . . . . ?
C11 C12 C13 N4 -177.56(17) . . . . ?
C11 C12 C13 C8 1.1(3) . . . . ?
C9 C8 C13 N4 177.93(15) . . . . ?
C7 C8 C13 N4 -1.4(2) . . . . ?
C9 C8 C13 C12 -0.7(3) . . . . ?
C7 C8 C13 C12 179.96(16) . . . . ?
N2 C1 N1 C2 177.84(16) . . . . ?
S1 C1 N1 C2 -2.1(2) . . . . ?
N2 C1 N1 C3 -7.0(2) . . . . ?
S1 C1 N1 C3 173.04(14) . . . . ?
N1 C1 N2 N3 -179.32(14) . . . . ?
S1 C1 N2 N3 0.7(2) . . . . ?
C6 C4 N3 N2 178.28(15) . . . . ?
C6 C4 N3 Ni1 5.9(2) . . . . ?
C1 N2 N3 C4 -178.15(15) . . . . ?
C1 N2 N3 Ni1 -4.89(19) . . . . ?
O1 Ni1 N3 C4 88.93(14) 2_656 . . . ?
O1 Ni1 N3 C4 -1.45(14) . . . . ?
S1 Ni1 N3 C4 177.49(14) . . . . ?
S1 Ni1 N3 C4 -89.19(14) 2_656 . . . ?
O1 Ni1 N3 N2 -83.39(11) 2_656 . . . ?
O1 Ni1 N3 N2 -173.77(11) . . . . ?
S1 Ni1 N3 N2 5.17(10) . . . . ?
S1 Ni1 N3 N2 98.49(10) 2_656 . . . ?
O1 C5 N4 C13 -174.38(15) . . . . ?
C6 C5 N4 C13 4.5(2) . . . . ?
C12 C13 N4 C5 176.94(16) . . . . ?
C8 C13 N4 C5 -1.7(3) . . . . ?
N4 C5 O1 Ni1 -172.34(11) . . . . ?
C6 C5 O1 Ni1 8.9(2) . . . . ?
O1 Ni1 O1 C5 -90.60(14) 2_656 . . . ?
N3 Ni1 O1 C5 -5.86(14) . . . . ?
N3 Ni1 O1 C5 -179.53(15) 2_656 . . . ?
S1 Ni1 O1 C5 96.47(14) 2_656 . . . ?
C9 C10 O2 C14B 177.1(2) . . . . ?
C11 C10 O2 C14B -2.1(3) . . . . ?
C9 C10 O2 C14 -2.1(3) . . . . ?
C11 C10 O2 C14 178.7(2) . . . . ?
N1 C1 S1 Ni1 -177.02(14) . . . . ?
N2 C1 S1 Ni1 3.00(14) . . . . ?
O1 Ni1 S1 C1 81.05(7) 2_656 . . . ?
N3 Ni1 S1 C1 -3.88(7) . . . . ?
N3 Ni1 S1 C1 169.55(7) 2_656 . . . ?
S1 Ni1 S1 C1 -105.77(6) 2_656 . . . ?

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
N2 H2 O4 0.88 2.15 2.9852(19) 158.4 .
N4 H4A O7 0.88 1.89 2.724(2) 157.3 5_666
O6 H6A O5 0.857(17) 2.040(19) 2.876(2) 165(3) .
O6 H6B O5 0.867(17) 2.066(18) 2.917(2) 167(3) 7_566
O6 H6B O3 0.867(17) 2.59(2) 3.291(2) 139(3) 7_566
O7 H7A O6 0.865(17) 1.984(19) 2.812(2) 160(3) 6_565
O7 H7B O3 0.874(17) 2.031(19) 2.886(2) 166(3) .

_diffrn_measured_fraction_theta_max 0.946
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.067