# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Long-guan Zhu'
_publ_contact_author_email       LGZHU@YAHOO.COM

_publ_section_title              
;
Synthesis, supramolecular structures
and catalytic properties of nickel(II) 3-sulfobenzoate
complexes with chelating amine ligands
;
loop_
_publ_author_name
'Long-guan Zhu.'
'Xiao-He Miao.'

# Attachment 'cifs-checked-new.cif'

data_comp-1
_database_code_depnum_ccdc_archive 'CCDC 697402'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H16 N2 Ni O7 S, O'
_chemical_formula_sum            'C19 H18 N2 Ni O8 S'
_chemical_formula_weight         493.12

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'
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   14.3015(11)
_cell_length_b                   7.5361(6)
_cell_length_c                   18.7339(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.6780(10)
_cell_angle_gamma                90.00
_cell_volume                     1923.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    5327
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      28.26

_exptl_crystal_description       block
_exptl_crystal_colour            green-blue
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1016
_exptl_absorpt_coefficient_mu    1.171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(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 SMART area-detector diffractometer'
_diffrn_measurement_method       '\f and \w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10070
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.28
_diffrn_reflns_theta_max         25.60
_reflns_number_total             3624
_reflns_number_gt                3358
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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.

The O1w is isotropically refined. Hydrogen atoms on carbon atoms were
placed in idealized positions and refined as riding atoms,
with C-H = 0.93 \%A and Uiso(H) = 1.2Ueq(C). Hydrogen atoms on O6 and O7
were added according to the Fourier map with the restriction of
O-H = 0.85 \%A and Uiso(H) = 1.2 Ueq(O). H atoms on O1w were not added.
;

_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^)+(0.0414P)^2^+1.6454P] 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         3624
_refine_ls_number_parameters     287
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_ref         0.1016
_refine_ls_wR_factor_gt          0.1000
_refine_ls_goodness_of_fit_ref   1.246
_refine_ls_restrained_S_all      1.246
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         <0.001

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 0.27699(2) 0.91930(5) 0.200383(18) 0.02482(13) Uani 1 1 d . . .
S1 S 0.34958(5) 0.97593(9) 0.65328(3) 0.02291(17) Uani 1 1 d . . .
N1 N 0.22939(17) 0.9391(3) 0.08432(13) 0.0292(5) Uani 1 1 d . . .
N2 N 0.14379(17) 0.7898(3) 0.17761(13) 0.0310(5) Uani 1 1 d . . .
O1 O 0.31732(17) 0.8760(3) 0.31156(11) 0.0394(5) Uani 1 1 d . . .
O2 O 0.25800(19) 1.1082(4) 0.35708(12) 0.0534(7) Uani 1 1 d . . .
O3 O 0.35407(14) 0.8196(3) 0.69986(10) 0.0304(4) Uani 1 1 d . . .
O4 O 0.25323(14) 1.0565(3) 0.62619(11) 0.0334(5) Uani 1 1 d . . .
O5 O 0.42542(15) 1.1023(3) 0.69215(11) 0.0329(5) Uani 1 1 d . . .
O6 O 0.40706(15) 1.0403(3) 0.20662(13) 0.0389(5) Uani 1 1 d D . .
O7 O 0.20555(16) 1.1569(3) 0.21015(11) 0.0349(5) Uani 1 1 d D . .
C1 C 0.2725(2) 1.0192(4) 0.03926(17) 0.0378(7) Uani 1 1 d . . .
H1 H 0.3328 1.0743 0.0604 0.045 Uiso 1 1 calc R . .
C2 C 0.2311(3) 1.0237(5) -0.03770(19) 0.0491(9) Uani 1 1 d . . .
H2 H 0.2631 1.0810 -0.0676 0.059 Uiso 1 1 calc R . .
C3 C 0.1424(3) 0.9428(5) -0.06946(18) 0.0492(9) Uani 1 1 d . . .
H3 H 0.1140 0.9450 -0.1212 0.059 Uiso 1 1 calc R . .
C4 C 0.0944(2) 0.8570(4) -0.02439(17) 0.0387(7) Uani 1 1 d . . .
C5 C -0.0002(3) 0.7748(5) -0.0514(2) 0.0499(10) Uani 1 1 d . . .
H5 H -0.0322 0.7720 -0.1026 0.060 Uiso 1 1 calc R . .
C6 C -0.0439(2) 0.7014(5) -0.0041(2) 0.0507(10) Uani 1 1 d . . .
H6 H -0.1052 0.6486 -0.0235 0.061 Uiso 1 1 calc R . .
C7 C 0.0020(2) 0.7030(4) 0.07480(19) 0.0400(8) Uani 1 1 d . . .
C8 C -0.0400(3) 0.6335(5) 0.1274(2) 0.0552(10) Uani 1 1 d . . .
H8A H -0.1016 0.5806 0.1113 0.066 Uiso 1 1 calc R . .
C9 C 0.0090(3) 0.6431(6) 0.2015(2) 0.0600(10) Uani 1 1 d . . .
H9 H -0.0190 0.5975 0.2364 0.072 Uiso 1 1 calc R . .
C10 C 0.1019(3) 0.7218(5) 0.2253(2) 0.0459(8) Uani 1 1 d . . .
H10 H 0.1352 0.7265 0.2763 0.055 Uiso 1 1 calc R . .
C11 C 0.1416(2) 0.8605(4) 0.05329(15) 0.0295(6) Uani 1 1 d . . .
C12 C 0.0949(2) 0.7815(4) 0.10317(16) 0.0297(6) Uani 1 1 d . . .
C13 C 0.3067(2) 0.9695(4) 0.36411(15) 0.0294(6) Uani 1 1 d . . .
C14 C 0.3601(2) 0.9038(4) 0.44212(15) 0.0273(6) Uani 1 1 d . . .
C15 C 0.3324(2) 0.9627(4) 0.50307(15) 0.0264(6) Uani 1 1 d . . .
H15 H 0.2806 1.0421 0.4961 0.032 Uiso 1 1 calc R . .
C16 C 0.3824(2) 0.9023(3) 0.57417(14) 0.0242(6) Uani 1 1 d . . .
C17 C 0.4609(2) 0.7870(4) 0.58575(16) 0.0306(6) Uani 1 1 d . . .
H17 H 0.4946 0.7485 0.6339 0.037 Uiso 1 1 calc R . .
C18 C 0.4885(2) 0.7297(4) 0.52542(16) 0.0340(7) Uani 1 1 d . . .
H18 H 0.5414 0.6527 0.5328 0.041 Uiso 1 1 calc R . .
C19 C 0.4375(2) 0.7865(4) 0.45335(16) 0.0317(6) Uani 1 1 d . . .
H19 H 0.4556 0.7453 0.4126 0.038 Uiso 1 1 calc R . .
O1W O 0.3191(7) 0.4858(14) 0.3268(6) 0.289(5) Uiso 1 1 d . . .
H6A H 0.4497(19) 0.994(3) 0.2428(13) 0.047 Uiso 1 1 d D . .
H6B H 0.412(2) 1.1515(13) 0.2087(16) 0.037 Uiso 1 1 d D . .
H7A H 0.225(2) 1.250(3) 0.1937(14) 0.042 Uiso 1 1 d D . .
H7B H 0.221(2) 1.165(4) 0.2577(6) 0.042 Uiso 1 1 d 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 0.0269(2) 0.0259(2) 0.0195(2) 0.00098(14) 0.00382(14) -0.00189(14)
S1 0.0260(3) 0.0224(3) 0.0191(3) -0.0007(3) 0.0050(3) 0.0019(3)
N1 0.0303(13) 0.0299(13) 0.0253(12) 0.0027(10) 0.0055(10) 0.0047(10)
N2 0.0307(12) 0.0322(13) 0.0304(13) 0.0000(10) 0.0095(10) -0.0036(11)
O1 0.0569(14) 0.0380(12) 0.0203(10) -0.0023(9) 0.0071(9) 0.0091(10)
O2 0.0687(17) 0.0648(17) 0.0267(11) 0.0056(11) 0.0147(11) 0.0350(14)
O3 0.0399(11) 0.0287(11) 0.0235(10) 0.0009(8) 0.0107(8) -0.0024(9)
O4 0.0310(11) 0.0425(12) 0.0255(10) -0.0010(9) 0.0068(8) 0.0098(9)
O5 0.0364(11) 0.0231(10) 0.0337(11) -0.0046(8) 0.0024(9) -0.0001(8)
O6 0.0298(11) 0.0245(11) 0.0517(14) 0.0080(10) -0.0035(10) -0.0039(9)
O7 0.0406(12) 0.0326(11) 0.0304(11) 0.0045(9) 0.0093(9) 0.0033(10)
C1 0.0400(17) 0.0424(18) 0.0337(16) 0.0099(14) 0.0154(14) 0.0067(14)
C2 0.062(2) 0.058(2) 0.0340(17) 0.0147(16) 0.0244(17) 0.0180(19)
C3 0.066(2) 0.056(2) 0.0209(15) 0.0006(15) 0.0061(15) 0.0228(19)
C4 0.0445(18) 0.0370(17) 0.0276(15) -0.0063(13) 0.0006(13) 0.0147(14)
C5 0.048(2) 0.047(2) 0.0366(18) -0.0162(16) -0.0138(16) 0.0148(17)
C6 0.0327(17) 0.043(2) 0.061(2) -0.0178(18) -0.0085(16) 0.0018(15)
C7 0.0278(15) 0.0295(16) 0.056(2) -0.0075(15) 0.0032(14) 0.0012(13)
C8 0.0336(18) 0.047(2) 0.083(3) -0.005(2) 0.0154(19) -0.0129(16)
C9 0.052(2) 0.062(3) 0.073(3) 0.007(2) 0.028(2) -0.017(2)
C10 0.0461(19) 0.051(2) 0.0433(19) 0.0053(16) 0.0181(16) -0.0094(16)
C11 0.0309(15) 0.0269(14) 0.0266(14) -0.0022(12) 0.0025(12) 0.0085(12)
C12 0.0280(14) 0.0227(14) 0.0346(15) -0.0031(12) 0.0040(12) 0.0037(11)
C13 0.0313(15) 0.0345(16) 0.0234(14) -0.0001(12) 0.0097(12) 0.0007(13)
C14 0.0299(15) 0.0306(15) 0.0223(13) -0.0008(11) 0.0092(11) -0.0029(12)
C15 0.0271(14) 0.0248(14) 0.0262(14) -0.0003(11) 0.0064(11) 0.0036(11)
C16 0.0290(14) 0.0240(14) 0.0210(13) -0.0013(11) 0.0100(11) -0.0011(11)
C17 0.0319(15) 0.0322(16) 0.0261(14) 0.0024(12) 0.0066(12) 0.0043(12)
C18 0.0324(15) 0.0358(16) 0.0350(16) 0.0001(13) 0.0120(13) 0.0099(13)
C19 0.0344(15) 0.0363(16) 0.0277(14) -0.0043(12) 0.0144(12) 0.0010(13)

_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 2.012(2) . ?
Ni1 O6 2.043(2) . ?
Ni1 N2 2.066(2) . ?
Ni1 N1 2.077(2) . ?
Ni1 O7 2.097(2) . ?
Ni1 O3 2.1129(19) 4_575 ?
S1 O4 1.449(2) . ?
S1 O3 1.456(2) . ?
S1 O5 1.461(2) . ?
S1 C16 1.774(3) . ?
N1 C1 1.332(4) . ?
N1 C11 1.349(4) . ?
N2 C10 1.322(4) . ?
N2 C12 1.358(4) . ?
O1 C13 1.257(3) . ?
O2 C13 1.241(4) . ?
O3 Ni1 2.1129(19) 4_576 ?
O6 H6A 0.838(10) . ?
O6 H6B 0.841(10) . ?
O7 H7A 0.845(10) . ?
O7 H7B 0.853(10) . ?
C1 C2 1.383(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.370(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.398(5) . ?
C3 H3 0.9300 . ?
C4 C11 1.406(4) . ?
C4 C5 1.433(5) . ?
C5 C6 1.347(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.424(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.402(5) . ?
C7 C12 1.403(4) . ?
C8 C9 1.354(6) . ?
C8 H8A 0.9300 . ?
C9 C10 1.398(5) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.433(4) . ?
C13 C14 1.512(4) . ?
C14 C19 1.383(4) . ?
C14 C15 1.390(4) . ?
C15 C16 1.384(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.383(4) . ?
C17 C18 1.375(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.393(4) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?

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 O6 92.49(9) . . ?
O1 Ni1 N2 95.37(10) . . ?
O6 Ni1 N2 171.48(10) . . ?
O1 Ni1 N1 174.35(9) . . ?
O6 Ni1 N1 91.79(9) . . ?
N2 Ni1 N1 80.16(9) . . ?
O1 Ni1 O7 92.42(8) . . ?
O6 Ni1 O7 94.20(9) . . ?
N2 Ni1 O7 88.76(9) . . ?
N1 Ni1 O7 90.95(9) . . ?
O1 Ni1 O3 83.15(8) . 4_575 ?
O6 Ni1 O3 85.03(8) . 4_575 ?
N2 Ni1 O3 92.64(9) . 4_575 ?
N1 Ni1 O3 93.55(8) . 4_575 ?
O7 Ni1 O3 175.46(8) . 4_575 ?
O4 S1 O3 114.41(12) . . ?
O4 S1 O5 112.61(12) . . ?
O3 S1 O5 109.74(12) . . ?
O4 S1 C16 107.66(12) . . ?
O3 S1 C16 105.86(12) . . ?
O5 S1 C16 105.97(13) . . ?
C1 N1 C11 118.4(3) . . ?
C1 N1 Ni1 128.9(2) . . ?
C11 N1 Ni1 112.69(19) . . ?
C10 N2 C12 118.6(3) . . ?
C10 N2 Ni1 128.5(2) . . ?
C12 N2 Ni1 112.84(19) . . ?
C13 O1 Ni1 130.9(2) . . ?
S1 O3 Ni1 139.84(12) . 4_576 ?
Ni1 O6 H6A 107(2) . . ?
Ni1 O6 H6B 121(2) . . ?
H6A O6 H6B 110.4(16) . . ?
Ni1 O7 H7A 117(2) . . ?
Ni1 O7 H7B 100(2) . . ?
H7A O7 H7B 108.2(16) . . ?
N1 C1 C2 122.5(3) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C3 C2 C1 119.3(3) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 120.2(3) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C3 C4 C11 116.5(3) . . ?
C3 C4 C5 124.8(3) . . ?
C11 C4 C5 118.6(3) . . ?
C6 C5 C4 121.5(3) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C6 C7 121.2(3) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C8 C7 C12 116.7(3) . . ?
C8 C7 C6 124.5(3) . . ?
C12 C7 C6 118.8(3) . . ?
C9 C8 C7 120.1(3) . . ?
C9 C8 H8A 119.9 . . ?
C7 C8 H8A 119.9 . . ?
C8 C9 C10 119.7(4) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
N2 C10 C9 122.0(3) . . ?
N2 C10 H10 119.0 . . ?
C9 C10 H10 119.0 . . ?
N1 C11 C4 123.1(3) . . ?
N1 C11 C12 117.3(2) . . ?
C4 C11 C12 119.6(3) . . ?
N2 C12 C7 122.7(3) . . ?
N2 C12 C11 117.0(2) . . ?
C7 C12 C11 120.2(3) . . ?
O2 C13 O1 125.9(3) . . ?
O2 C13 C14 118.7(3) . . ?
O1 C13 C14 115.4(3) . . ?
C19 C14 C15 119.6(3) . . ?
C19 C14 C13 120.2(2) . . ?
C15 C14 C13 120.2(2) . . ?
C16 C15 C14 119.5(3) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C17 C16 C15 121.0(2) . . ?
C17 C16 S1 118.2(2) . . ?
C15 C16 S1 120.7(2) . . ?
C18 C17 C16 119.3(3) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C17 C18 C19 120.2(3) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C14 C19 C18 120.2(3) . . ?
C14 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?

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
O6 Ni1 N1 C1 -5.0(3) . . . . ?
N2 Ni1 N1 C1 177.8(3) . . . . ?
O7 Ni1 N1 C1 89.2(3) . . . . ?
O3 Ni1 N1 C1 -90.1(3) 4_575 . . . ?
O6 Ni1 N1 C11 176.27(19) . . . . ?
N2 Ni1 N1 C11 -0.92(19) . . . . ?
O7 Ni1 N1 C11 -89.50(19) . . . . ?
O3 Ni1 N1 C11 91.15(19) 4_575 . . . ?
O1 Ni1 N2 C10 5.8(3) . . . . ?
N1 Ni1 N2 C10 -177.7(3) . . . . ?
O7 Ni1 N2 C10 -86.5(3) . . . . ?
O3 Ni1 N2 C10 89.2(3) 4_575 . . . ?
O1 Ni1 N2 C12 -176.14(19) . . . . ?
N1 Ni1 N2 C12 0.37(19) . . . . ?
O7 Ni1 N2 C12 91.5(2) . . . . ?
O3 Ni1 N2 C12 -92.8(2) 4_575 . . . ?
O6 Ni1 O1 C13 90.1(3) . . . . ?
N2 Ni1 O1 C13 -93.2(3) . . . . ?
O7 Ni1 O1 C13 -4.2(3) . . . . ?
O3 Ni1 O1 C13 174.8(3) 4_575 . . . ?
O4 S1 O3 Ni1 47.2(2) . . . 4_576 ?
O5 S1 O3 Ni1 174.91(17) . . . 4_576 ?
C16 S1 O3 Ni1 -71.2(2) . . . 4_576 ?
C11 N1 C1 C2 -0.4(5) . . . . ?
Ni1 N1 C1 C2 -179.1(2) . . . . ?
N1 C1 C2 C3 -0.1(5) . . . . ?
C1 C2 C3 C4 0.1(5) . . . . ?
C2 C3 C4 C11 0.4(5) . . . . ?
C2 C3 C4 C5 177.3(3) . . . . ?
C3 C4 C5 C6 -177.0(3) . . . . ?
C11 C4 C5 C6 -0.1(5) . . . . ?
C4 C5 C6 C7 0.2(5) . . . . ?
C5 C6 C7 C8 178.3(3) . . . . ?
C5 C6 C7 C12 -0.6(5) . . . . ?
C12 C7 C8 C9 -0.3(5) . . . . ?
C6 C7 C8 C9 -179.2(4) . . . . ?
C7 C8 C9 C10 -0.3(6) . . . . ?
C12 N2 C10 C9 -0.4(5) . . . . ?
Ni1 N2 C10 C9 177.6(3) . . . . ?
C8 C9 C10 N2 0.7(6) . . . . ?
C1 N1 C11 C4 1.0(4) . . . . ?
Ni1 N1 C11 C4 179.8(2) . . . . ?
C1 N1 C11 C12 -177.5(3) . . . . ?
Ni1 N1 C11 C12 1.3(3) . . . . ?
C3 C4 C11 N1 -1.0(4) . . . . ?
C5 C4 C11 N1 -178.1(3) . . . . ?
C3 C4 C11 C12 177.5(3) . . . . ?
C5 C4 C11 C12 0.4(4) . . . . ?
C10 N2 C12 C7 -0.3(4) . . . . ?
Ni1 N2 C12 C7 -178.6(2) . . . . ?
C10 N2 C12 C11 178.5(3) . . . . ?
Ni1 N2 C12 C11 0.2(3) . . . . ?
C8 C7 C12 N2 0.6(4) . . . . ?
C6 C7 C12 N2 179.6(3) . . . . ?
C8 C7 C12 C11 -178.1(3) . . . . ?
C6 C7 C12 C11 0.9(4) . . . . ?
N1 C11 C12 N2 -1.1(4) . . . . ?
C4 C11 C12 N2 -179.6(3) . . . . ?
N1 C11 C12 C7 177.8(3) . . . . ?
C4 C11 C12 C7 -0.8(4) . . . . ?
Ni1 O1 C13 O2 7.8(5) . . . . ?
Ni1 O1 C13 C14 -171.48(19) . . . . ?
O2 C13 C14 C19 -159.8(3) . . . . ?
O1 C13 C14 C19 19.6(4) . . . . ?
O2 C13 C14 C15 19.4(4) . . . . ?
O1 C13 C14 C15 -161.2(3) . . . . ?
C19 C14 C15 C16 -0.3(4) . . . . ?
C13 C14 C15 C16 -179.5(3) . . . . ?
C14 C15 C16 C17 1.3(4) . . . . ?
C14 C15 C16 S1 179.6(2) . . . . ?
O4 S1 C16 C17 -165.9(2) . . . . ?
O3 S1 C16 C17 -43.2(3) . . . . ?
O5 S1 C16 C17 73.4(2) . . . . ?
O4 S1 C16 C15 15.7(3) . . . . ?
O3 S1 C16 C15 138.5(2) . . . . ?
O5 S1 C16 C15 -105.0(2) . . . . ?
C15 C16 C17 C18 -0.9(4) . . . . ?
S1 C16 C17 C18 -179.2(2) . . . . ?
C16 C17 C18 C19 -0.4(5) . . . . ?
C15 C14 C19 C18 -1.0(4) . . . . ?
C13 C14 C19 C18 178.2(3) . . . . ?
C17 C18 C19 C14 1.4(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
O6 H6A O5 0.838(10) 1.97(3) 2.780(3) 163(3) 3_676
O6 H6B O5 0.841(10) 1.900(12) 2.728(3) 168(3) 4_585
O7 H7A O4 0.845(10) 2.051(11) 2.873(3) 164(3) 4_585
O7 H7B O2 0.853(10) 1.825(12) 2.650(3) 162(3) .

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.60
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.078

data_comp-2
_database_code_depnum_ccdc_archive 'CCDC 697403'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H22 N4 Ni O6 S, H2 O'
_chemical_formula_sum            'C31 H24 N4 Ni O7 S'
_chemical_formula_weight         655.31

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           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                   8.5583(7)
_cell_length_b                   11.6900(9)
_cell_length_c                   16.0260(13)
_cell_angle_alpha                69.9820(10)
_cell_angle_beta                 78.5200(10)
_cell_angle_gamma                78.3490(10)
_cell_volume                     1460.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2384
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      23.57

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             676
_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(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 SMART area-detector diffractometer'
_diffrn_measurement_method       '\f and \w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7736
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         25.10
_reflns_number_total             5098
_reflns_number_gt                4261
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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.

Hydrogen atoms on carbon atoms were
placed in idealized positions and refined as riding atoms,
with C-H = 0.93 \%A and Uiso(H) = 1.2Ueq(C). Hydrogen atoms on water
molecules were added according to the Fourier map with the restriction of
O-H = 0.85 \%A and Uiso(H) = 1.2 Ueq(O).
;

_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^)+(0.0992P)^2^+1.1944P] 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         5098
_refine_ls_number_parameters     409
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0766
_refine_ls_wR_factor_ref         0.1936
_refine_ls_wR_factor_gt          0.1843
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_restrained_S_all      1.116
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         <0.001

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 0.27227(7) 0.20402(5) 0.73800(4) 0.0408(2) Uani 1 1 d . . .
S1 S 0.0157(2) -0.36731(12) 0.76903(10) 0.0648(4) Uani 1 1 d . . .
O1 O 0.1459(4) 0.0846(3) 0.7192(2) 0.0483(8) Uani 1 1 d . . .
O2 O -0.0506(7) 0.2091(4) 0.6517(5) 0.142(3) Uani 1 1 d . . .
O3 O 0.1484(10) -0.3726(5) 0.8054(7) 0.202(5) Uani 1 1 d . . .
O4 O -0.1236(9) -0.3927(5) 0.8311(4) 0.153(3) Uani 1 1 d . . .
O5 O 0.0389(10) -0.4389(4) 0.7128(4) 0.147(3) Uani 1 1 d . . .
O6 O 0.1219(5) 0.3522(3) 0.6693(3) 0.0640(10) Uani 1 1 d D . .
O7 O -0.2374(10) -0.4487(6) 1.0188(4) 0.136(2) Uani 1 1 d D . .
N1 N 0.4223(5) 0.2175(4) 0.6153(3) 0.0520(10) Uani 1 1 d . . .
N2 N 0.4237(5) 0.3235(4) 0.7387(3) 0.0498(10) Uani 1 1 d . . .
N3 N 0.1464(5) 0.1973(4) 0.8647(3) 0.0514(10) Uani 1 1 d . . .
N4 N 0.4002(5) 0.0456(4) 0.8171(3) 0.0458(9) Uani 1 1 d . . .
C1 C 0.4168(7) 0.1675(6) 0.5544(4) 0.0689(15) Uani 1 1 d . . .
H1 H 0.3473 0.1098 0.5681 0.083 Uiso 1 1 calc R . .
C2 C 0.5101(9) 0.1964(8) 0.4695(4) 0.085(2) Uani 1 1 d . . .
H2 H 0.5006 0.1595 0.4281 0.102 Uiso 1 1 calc R . .
C3 C 0.6143(9) 0.2786(7) 0.4481(4) 0.086(2) Uani 1 1 d . . .
H3 H 0.6766 0.2985 0.3919 0.103 Uiso 1 1 calc R . .
C4 C 0.6276(7) 0.3339(5) 0.5120(4) 0.0703(18) Uani 1 1 d . . .
C5 C 0.7338(8) 0.4200(7) 0.4986(6) 0.093(3) Uani 1 1 d . . .
H5 H 0.8014 0.4424 0.4443 0.112 Uiso 1 1 calc R . .
C6 C 0.7395(8) 0.4694(6) 0.5616(6) 0.092(3) Uani 1 1 d . . .
H6 H 0.8101 0.5256 0.5504 0.111 Uiso 1 1 calc R . .
C7 C 0.6383(7) 0.4370(5) 0.6459(5) 0.0693(17) Uani 1 1 d . . .
C8 C 0.6381(8) 0.4858(6) 0.7144(6) 0.086(2) Uani 1 1 d . . .
H8 H 0.7110 0.5387 0.7074 0.104 Uiso 1 1 calc R . .
C9 C 0.5315(9) 0.4562(6) 0.7913(6) 0.086(2) Uani 1 1 d . . .
H9 H 0.5305 0.4886 0.8370 0.104 Uiso 1 1 calc R . .
C10 C 0.4235(7) 0.3759(5) 0.7999(4) 0.0671(15) Uani 1 1 d . . .
H10 H 0.3479 0.3586 0.8513 0.081 Uiso 1 1 calc R . .
C11 C 0.5259(6) 0.2995(5) 0.5959(3) 0.0543(13) Uani 1 1 d . . .
C12 C 0.5299(6) 0.3546(4) 0.6626(4) 0.0533(13) Uani 1 1 d . . .
C13 C 0.0230(7) 0.2749(6) 0.8875(4) 0.0703(16) Uani 1 1 d . . .
H13 H -0.0159 0.3432 0.8423 0.084 Uiso 1 1 calc R . .
C14 C -0.0503(10) 0.2602(8) 0.9738(6) 0.094(2) Uani 1 1 d . . .
H14 H -0.1357 0.3179 0.9862 0.112 Uiso 1 1 calc R . .
C16 C 0.1322(8) 0.0749(7) 1.0208(4) 0.0738(18) Uani 1 1 d . . .
C17 C 0.1950(11) -0.0315(8) 1.0850(4) 0.094(2) Uani 1 1 d . . .
H17 H 0.1499 -0.0469 1.1449 0.112 Uiso 1 1 calc R . .
C18 C 0.3171(10) -0.1110(8) 1.0627(4) 0.090(2) Uani 1 1 d . . .
H18 H 0.3542 -0.1811 1.1071 0.108 Uiso 1 1 calc R . .
C19 C 0.3941(8) -0.0904(6) 0.9699(4) 0.0699(17) Uani 1 1 d . . .
C20 C 0.5191(9) -0.1702(6) 0.9408(5) 0.087(2) Uani 1 1 d . . .
H20 H 0.5600 -0.2429 0.9817 0.105 Uiso 1 1 calc R . .
C21 C 0.5806(8) -0.1425(6) 0.8539(5) 0.084(2) Uani 1 1 d . . .
H21 H 0.6640 -0.1960 0.8343 0.101 Uiso 1 1 calc R . .
C22 C 0.5188(7) -0.0322(5) 0.7922(4) 0.0643(15) Uani 1 1 d . . .
H22 H 0.5631 -0.0138 0.7321 0.077 Uiso 1 1 calc R . .
C23 C 0.2014(6) 0.0990(5) 0.9303(3) 0.0524(13) Uani 1 1 d . . .
C24 C 0.3355(6) 0.0156(5) 0.9050(3) 0.0493(12) Uani 1 1 d . . .
C25 C 0.0284(6) 0.1079(4) 0.6786(4) 0.0526(13) Uani 1 1 d . . .
C26 C -0.0243(5) 0.0028(4) 0.6625(3) 0.0423(10) Uani 1 1 d . . .
C27 C 0.0255(6) -0.1183(4) 0.7107(3) 0.0443(11) Uani 1 1 d . . .
H27 H 0.0983 -0.1353 0.7510 0.053 Uiso 1 1 calc R . .
C28 C -0.0310(6) -0.2136(4) 0.7000(3) 0.0503(12) Uani 1 1 d . . .
C29 C -0.1328(7) -0.1872(5) 0.6353(4) 0.0679(16) Uani 1 1 d . . .
H29 H -0.1697 -0.2508 0.6259 0.081 Uiso 1 1 calc R . .
C30 C -0.1780(8) -0.0675(6) 0.5858(4) 0.0710(16) Uani 1 1 d . . .
H30 H -0.2429 -0.0506 0.5416 0.085 Uiso 1 1 calc R . .
C31 C -0.1287(6) 0.0274(5) 0.6006(4) 0.0567(13) Uani 1 1 d . . .
H31 H -0.1653 0.1084 0.5691 0.068 Uiso 1 1 calc R . .
C15 C 0.0006(9) 0.1641(9) 1.0390(5) 0.093(2) Uani 1 1 d . . .
H15 H -0.0494 0.1539 1.0977 0.111 Uiso 1 1 calc R . .
H6A H 0.087(5) 0.417(3) 0.684(4) 0.076 Uiso 1 1 d D . .
H6B H 0.044(4) 0.319(4) 0.667(4) 0.076 Uiso 1 1 d D . .
H7A H -0.291(12) -0.478(8) 0.993(7) 0.168 Uiso 1 1 d D . .
H7B H -0.189(11) -0.509(5) 1.057(5) 0.168 Uiso 1 1 d 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 0.0516(4) 0.0310(3) 0.0404(4) -0.0096(2) -0.0030(3) -0.0135(3)
S1 0.0871(11) 0.0317(7) 0.0745(10) -0.0180(6) -0.0037(8) -0.0115(7)
O1 0.061(2) 0.0280(16) 0.062(2) -0.0131(14) -0.0202(17) -0.0096(14)
O2 0.169(5) 0.035(2) 0.263(8) -0.043(3) -0.161(6) 0.018(3)
O3 0.210(7) 0.047(3) 0.346(11) 0.037(5) -0.200(8) -0.025(4)
O4 0.186(6) 0.072(3) 0.120(5) 0.011(3) 0.066(4) 0.007(4)
O5 0.277(8) 0.038(3) 0.116(4) -0.039(3) 0.006(5) -0.007(4)
O6 0.080(3) 0.0321(19) 0.081(3) -0.0153(18) -0.020(2) -0.0076(18)
O7 0.159(7) 0.141(5) 0.089(4) -0.033(4) -0.023(4) 0.023(5)
N1 0.058(2) 0.051(3) 0.043(2) -0.0102(19) -0.0025(19) -0.011(2)
N2 0.061(3) 0.037(2) 0.053(2) -0.0093(18) -0.010(2) -0.0175(19)
N3 0.052(2) 0.052(3) 0.056(3) -0.027(2) 0.007(2) -0.021(2)
N4 0.050(2) 0.042(2) 0.045(2) -0.0101(17) -0.0070(18) -0.0135(18)
C1 0.072(4) 0.079(4) 0.058(3) -0.028(3) -0.008(3) -0.008(3)
C2 0.085(5) 0.109(6) 0.052(4) -0.026(4) -0.006(3) 0.004(4)
C3 0.080(5) 0.093(5) 0.049(4) -0.002(3) -0.001(3) 0.022(4)
C4 0.055(3) 0.055(3) 0.064(4) 0.014(3) 0.004(3) 0.006(3)
C5 0.068(4) 0.064(5) 0.098(6) 0.021(4) 0.012(4) -0.006(4)
C6 0.053(4) 0.054(4) 0.133(7) 0.015(4) -0.001(4) -0.016(3)
C7 0.056(3) 0.038(3) 0.100(5) 0.003(3) -0.018(3) -0.012(3)
C8 0.076(4) 0.048(4) 0.134(7) -0.006(4) -0.033(4) -0.027(3)
C9 0.107(5) 0.055(4) 0.116(6) -0.028(4) -0.048(5) -0.019(4)
C10 0.079(4) 0.049(3) 0.076(4) -0.011(3) -0.017(3) -0.022(3)
C11 0.047(3) 0.047(3) 0.051(3) 0.002(2) -0.003(2) 0.001(2)
C12 0.049(3) 0.035(3) 0.064(3) 0.003(2) -0.013(2) -0.006(2)
C13 0.075(4) 0.063(4) 0.083(4) -0.042(3) 0.011(3) -0.022(3)
C14 0.093(5) 0.104(6) 0.099(6) -0.063(5) 0.022(5) -0.029(5)
C16 0.080(4) 0.100(5) 0.051(3) -0.023(3) 0.003(3) -0.050(4)
C17 0.111(6) 0.126(7) 0.048(4) -0.014(4) -0.001(4) -0.058(5)
C18 0.107(6) 0.100(6) 0.049(4) 0.020(4) -0.024(4) -0.047(5)
C19 0.070(4) 0.067(4) 0.068(4) 0.001(3) -0.020(3) -0.027(3)
C20 0.090(5) 0.066(4) 0.085(5) 0.010(4) -0.028(4) -0.010(4)
C21 0.060(4) 0.063(4) 0.116(6) -0.017(4) -0.023(4) 0.012(3)
C22 0.060(3) 0.058(3) 0.068(4) -0.018(3) -0.001(3) -0.004(3)
C23 0.061(3) 0.062(3) 0.042(3) -0.016(2) 0.000(2) -0.035(3)
C24 0.050(3) 0.053(3) 0.044(3) -0.001(2) -0.013(2) -0.023(2)
C25 0.063(3) 0.028(2) 0.069(3) -0.013(2) -0.023(3) -0.004(2)
C26 0.050(3) 0.033(2) 0.046(3) -0.016(2) -0.009(2) -0.004(2)
C27 0.054(3) 0.036(2) 0.046(3) -0.017(2) -0.009(2) -0.005(2)
C28 0.062(3) 0.035(3) 0.059(3) -0.022(2) -0.003(2) -0.009(2)
C29 0.082(4) 0.051(3) 0.089(4) -0.034(3) -0.027(3) -0.013(3)
C30 0.083(4) 0.070(4) 0.075(4) -0.028(3) -0.034(3) -0.013(3)
C31 0.065(3) 0.047(3) 0.060(3) -0.013(2) -0.020(3) -0.006(2)
C15 0.090(5) 0.137(7) 0.072(5) -0.063(5) 0.028(4) -0.049(5)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O6 2.056(4) . ?
Ni1 O1 2.058(3) . ?
Ni1 N3 2.084(4) . ?
Ni1 N4 2.088(4) . ?
Ni1 N2 2.093(4) . ?
Ni1 N1 2.099(4) . ?
S1 O3 1.358(6) . ?
S1 O5 1.389(5) . ?
S1 O4 1.403(6) . ?
S1 C28 1.771(5) . ?
O1 C25 1.240(6) . ?
O2 C25 1.219(6) . ?
O6 H6A 0.85(4) . ?
O6 H6B 0.85(4) . ?
O7 H7A 0.86(10) . ?
O7 H7B 0.86(8) . ?
N1 C1 1.310(7) . ?
N1 C11 1.354(7) . ?
N2 C10 1.322(7) . ?
N2 C12 1.354(6) . ?
N3 C13 1.327(7) . ?
N3 C23 1.342(7) . ?
N4 C22 1.316(7) . ?
N4 C24 1.359(6) . ?
C1 C2 1.402(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.354(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.419(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.423(10) . ?
C4 C11 1.425(7) . ?
C5 C6 1.337(11) . ?
C5 H5 0.9300 . ?
C6 C7 1.426(10) . ?
C6 H6 0.9300 . ?
C7 C12 1.395(7) . ?
C7 C8 1.400(10) . ?
C8 C9 1.363(10) . ?
C8 H8 0.9300 . ?
C9 C10 1.403(8) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.433(8) . ?
C13 C14 1.368(9) . ?
C13 H13 0.9300 . ?
C14 C15 1.313(11) . ?
C14 H14 0.9300 . ?
C16 C17 1.404(10) . ?
C16 C23 1.406(7) . ?
C16 C15 1.430(10) . ?
C17 C18 1.331(11) . ?
C17 H17 0.9300 . ?
C18 C19 1.460(9) . ?
C18 H18 0.9300 . ?
C19 C20 1.388(9) . ?
C19 C24 1.394(7) . ?
C20 C21 1.337(10) . ?
C20 H20 0.9300 . ?
C21 C22 1.407(8) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C24 1.437(7) . ?
C25 C26 1.506(6) . ?
C26 C31 1.385(7) . ?
C26 C27 1.387(6) . ?
C27 C28 1.373(6) . ?
C27 H27 0.9300 . ?
C28 C29 1.400(8) . ?
C29 C30 1.372(8) . ?
C29 H29 0.9300 . ?
C30 C31 1.369(8) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C15 H15 0.9300 . ?

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
O6 Ni1 O1 90.66(14) . . ?
O6 Ni1 N3 95.25(17) . . ?
O1 Ni1 N3 94.69(14) . . ?
O6 Ni1 N4 173.18(15) . . ?
O1 Ni1 N4 85.17(14) . . ?
N3 Ni1 N4 79.75(16) . . ?
O6 Ni1 N2 89.69(15) . . ?
O1 Ni1 N2 171.09(15) . . ?
N3 Ni1 N2 94.14(16) . . ?
N4 Ni1 N2 95.27(15) . . ?
O6 Ni1 N1 87.46(16) . . ?
O1 Ni1 N1 91.88(15) . . ?
N3 Ni1 N1 172.86(16) . . ?
N4 Ni1 N1 98.05(16) . . ?
N2 Ni1 N1 79.24(17) . . ?
O3 S1 O5 114.1(6) . . ?
O3 S1 O4 114.9(6) . . ?
O5 S1 O4 109.0(5) . . ?
O3 S1 C28 107.1(3) . . ?
O5 S1 C28 105.5(3) . . ?
O4 S1 C28 105.4(3) . . ?
C25 O1 Ni1 129.1(3) . . ?
Ni1 O6 H6A 124(4) . . ?
Ni1 O6 H6B 103(4) . . ?
H6A O6 H6B 111(5) . . ?
H7A O7 H7B 108(9) . . ?
C1 N1 C11 118.3(5) . . ?
C1 N1 Ni1 128.8(4) . . ?
C11 N1 Ni1 112.5(3) . . ?
C10 N2 C12 117.3(5) . . ?
C10 N2 Ni1 129.2(4) . . ?
C12 N2 Ni1 113.4(3) . . ?
C13 N3 C23 117.7(5) . . ?
C13 N3 Ni1 129.1(4) . . ?
C23 N3 Ni1 113.2(3) . . ?
C22 N4 C24 117.9(4) . . ?
C22 N4 Ni1 129.2(4) . . ?
C24 N4 Ni1 112.4(3) . . ?
N1 C1 C2 123.4(6) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C3 C2 C1 119.6(7) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C2 C3 C4 119.5(6) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C3 C4 C5 125.1(7) . . ?
C3 C4 C11 116.5(6) . . ?
C5 C4 C11 118.4(7) . . ?
C6 C5 C4 122.0(7) . . ?
C6 C5 H5 119.0 . . ?
C4 C5 H5 119.0 . . ?
C5 C6 C7 120.7(7) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 H6 119.7 . . ?
C12 C7 C8 116.5(6) . . ?
C12 C7 C6 120.0(7) . . ?
C8 C7 C6 123.4(7) . . ?
C9 C8 C7 120.3(6) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C8 C9 C10 118.5(7) . . ?
C8 C9 H9 120.8 . . ?
C10 C9 H9 120.8 . . ?
N2 C10 C9 123.3(6) . . ?
N2 C10 H10 118.3 . . ?
C9 C10 H10 118.3 . . ?
N1 C11 C4 122.6(6) . . ?
N1 C11 C12 117.9(4) . . ?
C4 C11 C12 119.5(5) . . ?
N2 C12 C7 124.0(6) . . ?
N2 C12 C11 116.6(4) . . ?
C7 C12 C11 119.4(5) . . ?
N3 C13 C14 123.6(7) . . ?
N3 C13 H13 118.2 . . ?
C14 C13 H13 118.2 . . ?
C15 C14 C13 119.7(7) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C17 C16 C23 119.1(7) . . ?
C17 C16 C15 125.4(7) . . ?
C23 C16 C15 115.6(6) . . ?
C18 C17 C16 121.9(6) . . ?
C18 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
C17 C18 C19 121.4(6) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 H18 119.3 . . ?
C20 C19 C24 117.2(6) . . ?
C20 C19 C18 125.0(6) . . ?
C24 C19 C18 117.8(6) . . ?
C21 C20 C19 120.1(6) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C22 119.8(6) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 H21 120.1 . . ?
N4 C22 C21 122.0(6) . . ?
N4 C22 H22 119.0 . . ?
C21 C22 H22 119.0 . . ?
N3 C23 C16 122.7(6) . . ?
N3 C23 C24 117.4(4) . . ?
C16 C23 C24 119.9(5) . . ?
N4 C24 C19 122.9(5) . . ?
N4 C24 C23 117.2(4) . . ?
C19 C24 C23 119.9(5) . . ?
O2 C25 O1 125.4(5) . . ?
O2 C25 C26 116.8(5) . . ?
O1 C25 C26 117.8(4) . . ?
C31 C26 C27 119.3(4) . . ?
C31 C26 C25 119.5(4) . . ?
C27 C26 C25 121.2(4) . . ?
C28 C27 C26 121.0(4) . . ?
C28 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
C27 C28 C29 118.9(5) . . ?
C27 C28 S1 121.4(4) . . ?
C29 C28 S1 119.7(4) . . ?
C30 C29 C28 119.9(5) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C31 C30 C29 120.8(5) . . ?
C31 C30 H30 119.6 . . ?
C29 C30 H30 119.6 . . ?
C30 C31 C26 120.0(5) . . ?
C30 C31 H31 120.0 . . ?
C26 C31 H31 120.0 . . ?
C14 C15 C16 120.7(6) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?

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
O6 Ni1 O1 C25 1.3(5) . . . . ?
N3 Ni1 O1 C25 96.6(5) . . . . ?
N4 Ni1 O1 C25 175.9(5) . . . . ?
N1 Ni1 O1 C25 -86.2(5) . . . . ?
O6 Ni1 N1 C1 -87.7(5) . . . . ?
O1 Ni1 N1 C1 2.9(5) . . . . ?
N4 Ni1 N1 C1 88.3(5) . . . . ?
N2 Ni1 N1 C1 -177.8(5) . . . . ?
O6 Ni1 N1 C11 85.2(3) . . . . ?
O1 Ni1 N1 C11 175.8(3) . . . . ?
N4 Ni1 N1 C11 -98.8(3) . . . . ?
N2 Ni1 N1 C11 -5.0(3) . . . . ?
O6 Ni1 N2 C10 92.3(5) . . . . ?
N3 Ni1 N2 C10 -2.9(5) . . . . ?
N4 Ni1 N2 C10 -83.0(5) . . . . ?
N1 Ni1 N2 C10 179.8(5) . . . . ?
O6 Ni1 N2 C12 -83.9(3) . . . . ?
N3 Ni1 N2 C12 -179.1(3) . . . . ?
N4 Ni1 N2 C12 100.8(3) . . . . ?
N1 Ni1 N2 C12 3.6(3) . . . . ?
O6 Ni1 N3 C13 -6.5(5) . . . . ?
O1 Ni1 N3 C13 -97.6(4) . . . . ?
N4 Ni1 N3 C13 178.2(5) . . . . ?
N2 Ni1 N3 C13 83.6(5) . . . . ?
O6 Ni1 N3 C23 173.2(3) . . . . ?
O1 Ni1 N3 C23 82.1(3) . . . . ?
N4 Ni1 N3 C23 -2.1(3) . . . . ?
N2 Ni1 N3 C23 -96.7(3) . . . . ?
O1 Ni1 N4 C22 79.8(5) . . . . ?
N3 Ni1 N4 C22 175.5(5) . . . . ?
N2 Ni1 N4 C22 -91.2(5) . . . . ?
N1 Ni1 N4 C22 -11.4(5) . . . . ?
O1 Ni1 N4 C24 -92.3(3) . . . . ?
N3 Ni1 N4 C24 3.4(3) . . . . ?
N2 Ni1 N4 C24 96.7(3) . . . . ?
N1 Ni1 N4 C24 176.5(3) . . . . ?
C11 N1 C1 C2 -1.4(8) . . . . ?
Ni1 N1 C1 C2 171.1(4) . . . . ?
N1 C1 C2 C3 1.1(10) . . . . ?
C1 C2 C3 C4 0.1(10) . . . . ?
C2 C3 C4 C5 179.0(6) . . . . ?
C2 C3 C4 C11 -0.9(8) . . . . ?
C3 C4 C5 C6 179.5(6) . . . . ?
C11 C4 C5 C6 -0.6(9) . . . . ?
C4 C5 C6 C7 0.2(11) . . . . ?
C5 C6 C7 C12 -1.1(9) . . . . ?
C5 C6 C7 C8 -179.8(6) . . . . ?
C12 C7 C8 C9 -2.5(9) . . . . ?
C6 C7 C8 C9 176.2(6) . . . . ?
C7 C8 C9 C10 0.2(10) . . . . ?
C12 N2 C10 C9 -3.0(8) . . . . ?
Ni1 N2 C10 C9 -179.1(4) . . . . ?
C8 C9 C10 N2 2.7(9) . . . . ?
C1 N1 C11 C4 0.5(7) . . . . ?
Ni1 N1 C11 C4 -173.2(4) . . . . ?
C1 N1 C11 C12 179.4(5) . . . . ?
Ni1 N1 C11 C12 5.7(5) . . . . ?
C3 C4 C11 N1 0.7(7) . . . . ?
C5 C4 C11 N1 -179.3(5) . . . . ?
C3 C4 C11 C12 -178.3(5) . . . . ?
C5 C4 C11 C12 1.8(7) . . . . ?
C10 N2 C12 C7 0.4(7) . . . . ?
Ni1 N2 C12 C7 177.1(4) . . . . ?
C10 N2 C12 C11 -178.4(4) . . . . ?
Ni1 N2 C12 C11 -1.7(5) . . . . ?
C8 C7 C12 N2 2.3(8) . . . . ?
C6 C7 C12 N2 -176.5(5) . . . . ?
C8 C7 C12 C11 -178.9(5) . . . . ?
C6 C7 C12 C11 2.4(8) . . . . ?
N1 C11 C12 N2 -2.8(6) . . . . ?
C4 C11 C12 N2 176.2(4) . . . . ?
N1 C11 C12 C7 178.3(4) . . . . ?
C4 C11 C12 C7 -2.7(7) . . . . ?
C23 N3 C13 C14 0.2(8) . . . . ?
Ni1 N3 C13 C14 179.8(5) . . . . ?
N3 C13 C14 C15 -0.7(11) . . . . ?
C23 C16 C17 C18 -0.7(10) . . . . ?
C15 C16 C17 C18 179.4(7) . . . . ?
C16 C17 C18 C19 1.0(11) . . . . ?
C17 C18 C19 C20 -178.2(7) . . . . ?
C17 C18 C19 C24 0.0(10) . . . . ?
C24 C19 C20 C21 1.5(10) . . . . ?
C18 C19 C20 C21 179.7(6) . . . . ?
C19 C20 C21 C22 0.2(11) . . . . ?
C24 N4 C22 C21 -1.2(8) . . . . ?
Ni1 N4 C22 C21 -172.9(4) . . . . ?
C20 C21 C22 N4 -0.4(10) . . . . ?
C13 N3 C23 C16 1.0(7) . . . . ?
Ni1 N3 C23 C16 -178.8(4) . . . . ?
C13 N3 C23 C24 -179.8(4) . . . . ?
Ni1 N3 C23 C24 0.5(5) . . . . ?
C17 C16 C23 N3 178.7(5) . . . . ?
C15 C16 C23 N3 -1.4(8) . . . . ?
C17 C16 C23 C24 -0.6(8) . . . . ?
C15 C16 C23 C24 179.3(5) . . . . ?
C22 N4 C24 C19 3.0(7) . . . . ?
Ni1 N4 C24 C19 176.1(4) . . . . ?
C22 N4 C24 C23 -177.3(5) . . . . ?
Ni1 N4 C24 C23 -4.2(5) . . . . ?
C20 C19 C24 N4 -3.2(8) . . . . ?
C18 C19 C24 N4 178.4(5) . . . . ?
C20 C19 C24 C23 177.1(5) . . . . ?
C18 C19 C24 C23 -1.2(8) . . . . ?
N3 C23 C24 N4 2.6(6) . . . . ?
C16 C23 C24 N4 -178.1(4) . . . . ?
N3 C23 C24 C19 -177.7(5) . . . . ?
C16 C23 C24 C19 1.5(7) . . . . ?
Ni1 O1 C25 O2 -11.0(9) . . . . ?
Ni1 O1 C25 C26 170.4(3) . . . . ?
O2 C25 C26 C31 16.1(8) . . . . ?
O1 C25 C26 C31 -165.2(5) . . . . ?
O2 C25 C26 C27 -161.7(6) . . . . ?
O1 C25 C26 C27 17.1(7) . . . . ?
C31 C26 C27 C28 -2.0(7) . . . . ?
C25 C26 C27 C28 175.8(5) . . . . ?
C26 C27 C28 C29 3.8(8) . . . . ?
C26 C27 C28 S1 -173.6(4) . . . . ?
O3 S1 C28 C27 -20.0(7) . . . . ?
O5 S1 C28 C27 -142.0(5) . . . . ?
O4 S1 C28 C27 102.8(6) . . . . ?
O3 S1 C28 C29 162.6(6) . . . . ?
O5 S1 C28 C29 40.6(6) . . . . ?
O4 S1 C28 C29 -74.6(6) . . . . ?
C27 C28 C29 C30 -1.8(9) . . . . ?
S1 C28 C29 C30 175.6(5) . . . . ?
C28 C29 C30 C31 -2.0(10) . . . . ?
C29 C30 C31 C26 3.9(9) . . . . ?
C27 C26 C31 C30 -1.9(8) . . . . ?
C25 C26 C31 C30 -179.7(5) . . . . ?
C13 C14 C15 C16 0.2(11) . . . . ?
C17 C16 C15 C14 -179.3(7) . . . . ?
C23 C16 C15 C14 0.8(10) . . . . ?

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
O6 H6A O5 0.85(4) 1.84(4) 2.687(6) 173(5) 1_565
O6 H6B O2 0.85(4) 1.76(5) 2.558(6) 157(5) .
O7 H7A O4 0.86(10) 2.66(11) 2.859(9) 95(8) .
O7 H7B O3 0.86(8) 2.22(5) 3.010(9) 155(10) 2_547

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.090

data_comp-3
_database_code_depnum_ccdc_archive 'CCDC 697404'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H24 N6 Ni, 2(C7 H5 O5 S), 9(H2 O), O'
_chemical_formula_sum            'C50 H54 N6 Ni O20 S2'
_chemical_formula_weight         1181.82

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           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                   12.875(3)
_cell_length_b                   14.763(4)
_cell_length_c                   15.643(4)
_cell_angle_alpha                107.090(4)
_cell_angle_beta                 94.328(4)
_cell_angle_gamma                106.234(4)
_cell_volume                     2688.2(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4598
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      22.75

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1232
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(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 SMART area-detector diffractometer'
_diffrn_measurement_method       '\f and \w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19953
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.38
_diffrn_reflns_theta_max         25.20
_reflns_number_total             9619
_reflns_number_gt                7498
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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.

Hydrogen atoms on carbon atoms were
placed in idealized positions and refined as riding atoms,
with C-H = 0.93 \%A and Uiso(H) = 1.2Ueq(C). O10w is disordered and
hydrogen atoms on this atom were not added. H atoms on other water
molecules were added according to the Fourier map with the restriction of
O-H = 0.85 \%A and Uiso(H) = 1.2 Ueq(O).
;

_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^)+(0.0612P)^2^+1.0359P] 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         9619
_refine_ls_number_parameters     776
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0578
_refine_ls_wR_factor_ref         0.1430
_refine_ls_wR_factor_gt          0.1321
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         <0.001

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 0.87285(3) 0.69528(3) 0.70738(3) 0.03363(14) Uani 1 1 d . . .
S1 S 0.56093(8) 0.13660(8) 0.86520(9) 0.0639(3) Uani 1 1 d . . .
S2 S 0.18576(8) 0.27067(8) 0.75005(7) 0.0543(3) Uani 1 1 d . . .
N1 N 1.0121(2) 0.81736(19) 0.72469(17) 0.0368(6) Uani 1 1 d . . .
N2 N 0.9901(2) 0.6559(2) 0.77603(18) 0.0378(6) Uani 1 1 d . . .
N3 N 0.8190(2) 0.75547(19) 0.82884(18) 0.0365(6) Uani 1 1 d . . .
N4 N 0.7636(2) 0.7601(2) 0.66263(18) 0.0387(7) Uani 1 1 d . . .
N5 N 0.7541(2) 0.5544(2) 0.68061(18) 0.0386(6) Uani 1 1 d . . .
N6 N 0.8928(2) 0.6197(2) 0.57626(18) 0.0391(7) Uani 1 1 d . . .
O1 O 0.9863(2) 0.0053(2) 0.89347(19) 0.0657(8) Uani 1 1 d . . .
O2 O 0.8929(2) 0.0515(2) 1.00316(19) 0.0654(8) Uani 1 1 d . . .
H2C H 0.9371 0.0356 1.0314 0.098 Uiso 1 1 calc R . .
O3 O 0.6041(3) 0.2439(2) 0.9091(3) 0.1066(14) Uani 1 1 d . . .
O4 O 0.4792(3) 0.1043(3) 0.7854(3) 0.1060(13) Uani 1 1 d . . .
O5 O 0.5253(2) 0.0866(2) 0.9288(2) 0.0724(8) Uani 1 1 d . . .
O6 O 0.5124(2) 0.58339(19) 0.61463(19) 0.0642(8) Uani 1 1 d . . .
H6C H 0.5340 0.5814 0.5663 0.096 Uiso 1 1 calc R . .
O7 O 0.4022(2) 0.4328(2) 0.53208(18) 0.0678(8) Uani 1 1 d . . .
O8 O 0.1844(2) 0.2034(2) 0.66160(19) 0.0719(9) Uani 1 1 d . . .
O9 O 0.2382(3) 0.2467(2) 0.8216(2) 0.0820(10) Uani 1 1 d . . .
O10 O 0.0805(2) 0.2801(3) 0.7635(2) 0.0916(11) Uani 1 1 d . . .
O1W O 0.4593(3) 0.3503(2) 0.9105(3) 0.0798(10) Uani 1 1 d D . .
O2W O 0.6107(2) 0.5427(2) 0.9344(2) 0.0759(9) Uani 1 1 d D . .
O3W O 0.8142(3) 0.3462(2) 0.8724(3) 0.0774(9) Uani 1 1 d D . .
O4W O 0.8827(3) 0.3146(3) 0.6998(2) 0.0854(10) Uani 1 1 d D . .
O5W O 0.0070(3) 0.3075(3) 0.9348(2) 0.0806(9) Uani 1 1 d D . .
O6W O 0.8201(3) 0.5324(2) 0.9571(3) 0.0917(11) Uani 1 1 d D . .
O7W O 0.3971(4) 0.1637(4) 0.6500(3) 0.1190(15) Uani 1 1 d D . .
O8W O 0.8234(4) 0.1672(4) 0.5240(3) 0.1242(15) Uani 1 1 d D . .
O9W O 0.0027(6) 0.0992(5) 0.5182(3) 0.1537(19) Uani 1 1 d D . .
O10W O 0.5939(7) 0.0352(7) 0.4636(7) 0.185(5) Uani 0.760(13) 1 d PU A 1
O10' O 0.6215(11) 0.0804(11) 0.3940(13) 0.086(7) Uani 0.240(13) 1 d PU A 2
C1 C 1.0243(3) 0.8939(3) 0.6950(2) 0.0478(9) Uani 1 1 d . . .
H1 H 0.9644 0.8959 0.6594 0.057 Uiso 1 1 calc R . .
C2 C 1.1225(4) 0.9721(3) 0.7146(3) 0.0613(11) Uani 1 1 d . . .
H2 H 1.1275 1.0242 0.6916 0.074 Uiso 1 1 calc R . .
C3 C 1.2102(3) 0.9716(3) 0.7670(3) 0.0631(12) Uani 1 1 d . . .
H3 H 1.2756 1.0242 0.7817 0.076 Uiso 1 1 calc R . .
C4 C 1.2021(3) 0.8910(3) 0.7991(3) 0.0511(10) Uani 1 1 d . . .
C5 C 1.2900(3) 0.8827(3) 0.8553(3) 0.0639(12) Uani 1 1 d . . .
H5 H 1.3574 0.9330 0.8719 0.077 Uiso 1 1 calc R . .
C6 C 1.2774(3) 0.8042(4) 0.8844(3) 0.0633(12) Uani 1 1 d . . .
H6 H 1.3359 0.8015 0.9212 0.076 Uiso 1 1 calc R . .
C7 C 1.1756(3) 0.7244(3) 0.8600(2) 0.0486(9) Uani 1 1 d . . .
C8 C 1.1575(3) 0.6412(3) 0.8894(3) 0.0595(11) Uani 1 1 d . . .
H8 H 1.2121 0.6367 0.9289 0.071 Uiso 1 1 calc R . .
C9 C 1.0594(3) 0.5670(3) 0.8596(3) 0.0583(11) Uani 1 1 d . . .
H9 H 1.0471 0.5106 0.8774 0.070 Uiso 1 1 calc R . .
C10 C 0.9777(3) 0.5761(3) 0.8023(2) 0.0474(9) Uani 1 1 d . . .
H10 H 0.9115 0.5242 0.7814 0.057 Uiso 1 1 calc R . .
C11 C 1.1006(3) 0.8147(2) 0.7751(2) 0.0389(8) Uani 1 1 d . . .
C12 C 1.0885(3) 0.7295(3) 0.8043(2) 0.0390(8) Uani 1 1 d . . .
C13 C 0.8496(3) 0.7568(3) 0.9123(2) 0.0454(9) Uani 1 1 d . . .
H13 H 0.9098 0.7362 0.9234 0.055 Uiso 1 1 calc R . .
C14 C 0.7958(3) 0.7874(3) 0.9835(2) 0.0541(10) Uani 1 1 d . . .
H14 H 0.8200 0.7871 1.0410 0.065 Uiso 1 1 calc R . .
C15 C 0.7081(4) 0.8175(3) 0.9693(3) 0.0585(11) Uani 1 1 d . . .
H15 H 0.6712 0.8371 1.0167 0.070 Uiso 1 1 calc R . .
C16 C 0.6727(3) 0.8192(2) 0.8831(3) 0.0464(9) Uani 1 1 d . . .
C17 C 0.5838(3) 0.8526(3) 0.8619(3) 0.0590(11) Uani 1 1 d . . .
H17 H 0.5424 0.8711 0.9061 0.071 Uiso 1 1 calc R . .
C18 C 0.5584(3) 0.8579(3) 0.7785(3) 0.0589(11) Uani 1 1 d . . .
H18 H 0.5001 0.8805 0.7667 0.071 Uiso 1 1 calc R . .
C19 C 0.6189(3) 0.8298(3) 0.7087(3) 0.0472(9) Uani 1 1 d . . .
C20 C 0.6009(3) 0.8397(3) 0.6236(3) 0.0610(11) Uani 1 1 d . . .
H20 H 0.5461 0.8654 0.6096 0.073 Uiso 1 1 calc R . .
C21 C 0.6634(4) 0.8118(3) 0.5609(3) 0.0632(12) Uani 1 1 d . . .
H21 H 0.6528 0.8197 0.5044 0.076 Uiso 1 1 calc R . .
C22 C 0.7441(3) 0.7710(3) 0.5822(2) 0.0502(9) Uani 1 1 d . . .
H22 H 0.7854 0.7507 0.5384 0.060 Uiso 1 1 calc R . .
C23 C 0.7321(3) 0.7873(2) 0.8145(2) 0.0377(8) Uani 1 1 d . . .
C24 C 0.7038(3) 0.7919(2) 0.7261(2) 0.0377(8) Uani 1 1 d . . .
C25 C 0.6887(3) 0.5212(3) 0.7339(3) 0.0473(9) Uani 1 1 d . . .
H25 H 0.6885 0.5659 0.7899 0.057 Uiso 1 1 calc R . .
C26 C 0.6206(3) 0.4231(3) 0.7104(3) 0.0596(11) Uani 1 1 d . . .
H26 H 0.5779 0.4027 0.7508 0.072 Uiso 1 1 calc R . .
C27 C 0.6170(3) 0.3571(3) 0.6278(3) 0.0636(12) Uani 1 1 d . . .
H27 H 0.5707 0.2916 0.6107 0.076 Uiso 1 1 calc R . .
C28 C 0.6837(3) 0.3887(3) 0.5687(3) 0.0518(10) Uani 1 1 d . . .
C29 C 0.6865(4) 0.3258(3) 0.4801(3) 0.0688(13) Uani 1 1 d . . .
H29 H 0.6420 0.2594 0.4597 0.083 Uiso 1 1 calc R . .
C30 C 0.7510(4) 0.3598(3) 0.4265(3) 0.0676(12) Uani 1 1 d . . .
H30 H 0.7492 0.3170 0.3689 0.081 Uiso 1 1 calc R . .
C31 C 0.8230(3) 0.4604(3) 0.4552(2) 0.0508(10) Uani 1 1 d . . .
C32 C 0.8940(4) 0.5005(4) 0.4029(3) 0.0652(12) Uani 1 1 d . . .
H32 H 0.8936 0.4615 0.3441 0.078 Uiso 1 1 calc R . .
C33 C 0.9632(4) 0.5951(3) 0.4367(3) 0.0603(11) Uani 1 1 d . . .
H33 H 1.0115 0.6210 0.4022 0.072 Uiso 1 1 calc R . .
C34 C 0.9608(3) 0.6533(3) 0.5246(2) 0.0505(9) Uani 1 1 d . . .
H34 H 1.0089 0.7183 0.5479 0.061 Uiso 1 1 calc R . .
C35 C 0.7523(3) 0.4885(2) 0.5985(2) 0.0394(8) Uani 1 1 d . . .
C36 C 0.8244(3) 0.5244(2) 0.5422(2) 0.0393(8) Uani 1 1 d . . .
C37 C 0.9109(3) 0.0379(3) 0.9221(3) 0.0467(9) Uani 1 1 d . . .
C38 C 0.8389(3) 0.0626(2) 0.8604(3) 0.0442(9) Uani 1 1 d . . .
C39 C 0.7453(3) 0.0842(2) 0.8868(3) 0.0436(8) Uani 1 1 d . . .
H39 H 0.7296 0.0860 0.9442 0.052 Uiso 1 1 calc R . .
C40 C 0.6765(3) 0.1028(3) 0.8274(3) 0.0484(9) Uani 1 1 d . . .
C41 C 0.6989(4) 0.1007(3) 0.7423(3) 0.0634(12) Uani 1 1 d . . .
H41 H 0.6516 0.1130 0.7025 0.076 Uiso 1 1 calc R . .
C42 C 0.7926(4) 0.0801(3) 0.7165(3) 0.0663(12) Uani 1 1 d . . .
H42 H 0.8087 0.0792 0.6594 0.080 Uiso 1 1 calc R . .
C43 C 0.8621(3) 0.0609(3) 0.7756(3) 0.0556(10) Uani 1 1 d . . .
H43 H 0.9248 0.0467 0.7581 0.067 Uiso 1 1 calc R . .
C44 C 0.4337(3) 0.5011(3) 0.6037(3) 0.0464(9) Uani 1 1 d . . .
C45 C 0.3869(3) 0.4939(3) 0.6852(2) 0.0428(8) Uani 1 1 d . . .
C46 C 0.3145(3) 0.4027(3) 0.6805(2) 0.0445(9) Uani 1 1 d . . .
H46 H 0.2947 0.3497 0.6261 0.053 Uiso 1 1 calc R . .
C47 C 0.2719(3) 0.3901(3) 0.7552(2) 0.0424(8) Uani 1 1 d . . .
C48 C 0.3008(3) 0.4690(3) 0.8365(3) 0.0538(10) Uani 1 1 d . . .
H48 H 0.2717 0.4607 0.8873 0.065 Uiso 1 1 calc R . .
C49 C 0.3731(3) 0.5602(3) 0.8414(3) 0.0592(11) Uani 1 1 d . . .
H49 H 0.3926 0.6132 0.8957 0.071 Uiso 1 1 calc R . .
C50 C 0.4165(3) 0.5730(3) 0.7661(3) 0.0522(10) Uani 1 1 d . . .
H50 H 0.4653 0.6343 0.7696 0.063 Uiso 1 1 calc R . .
H9A H -0.023(6) 0.066(5) 0.554(4) 0.184 Uiso 1 1 d D . .
H6A H 0.870(2) 0.581(2) 0.993(3) 0.110 Uiso 1 1 d D . .
H1A H 0.498(3) 0.313(2) 0.912(3) 0.096 Uiso 1 1 d D . .
H1B H 0.3969(18) 0.316(3) 0.879(3) 0.096 Uiso 1 1 d D . .
H5A H 0.029(3) 0.288(4) 0.8844(16) 0.096 Uiso 1 1 d D . .
H5B H -0.049(3) 0.325(4) 0.923(3) 0.096 Uiso 1 1 d D . .
H8A H 0.826(5) 0.180(5) 0.475(3) 0.152 Uiso 1 1 d D . .
H8B H 0.757(2) 0.138(5) 0.526(4) 0.152 Uiso 1 1 d D . .
H2A H 0.587(3) 0.580(2) 0.975(2) 0.091 Uiso 1 1 d D . .
H2B H 0.567(3) 0.4832(12) 0.918(3) 0.091 Uiso 1 1 d D . .
H3B H 0.755(2) 0.311(2) 0.882(3) 0.093 Uiso 1 1 d D . .
H3A H 0.821(3) 0.4075(10) 0.899(3) 0.093 Uiso 1 1 d D . .
H9B H 0.062(4) 0.145(4) 0.548(4) 0.184 Uiso 1 1 d D . .
H4A H 0.847(3) 0.320(4) 0.743(2) 0.102 Uiso 1 1 d D . .
H4B H 0.942(2) 0.305(4) 0.716(3) 0.102 Uiso 1 1 d D . .
H6B H 0.762(2) 0.547(3) 0.951(3) 0.110 Uiso 1 1 d D . .
H7B H 0.3292(14) 0.155(5) 0.651(4) 0.145 Uiso 1 1 d D . .
H7A H 0.428(4) 0.165(5) 0.701(2) 0.145 Uiso 1 1 d 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 0.0308(2) 0.0333(2) 0.0330(2) 0.00850(18) 0.00722(17) 0.00649(18)
S1 0.0319(5) 0.0560(7) 0.1085(9) 0.0358(6) 0.0032(6) 0.0140(5)
S2 0.0465(6) 0.0599(6) 0.0534(6) 0.0249(5) 0.0136(5) 0.0043(5)
N1 0.0370(16) 0.0333(15) 0.0350(15) 0.0084(12) 0.0088(13) 0.0053(12)
N2 0.0328(15) 0.0403(16) 0.0405(16) 0.0133(13) 0.0106(13) 0.0106(13)
N3 0.0382(16) 0.0316(15) 0.0364(16) 0.0101(12) 0.0088(13) 0.0061(12)
N4 0.0363(16) 0.0369(16) 0.0383(16) 0.0100(13) 0.0039(13) 0.0076(13)
N5 0.0320(15) 0.0409(16) 0.0397(16) 0.0132(13) 0.0058(13) 0.0070(12)
N6 0.0405(16) 0.0411(16) 0.0363(16) 0.0113(13) 0.0114(13) 0.0144(13)
O1 0.0558(17) 0.084(2) 0.0652(18) 0.0145(15) 0.0129(14) 0.0440(16)
O2 0.0576(18) 0.091(2) 0.0600(19) 0.0253(16) 0.0108(15) 0.0422(16)
O3 0.0547(19) 0.055(2) 0.218(4) 0.042(2) 0.038(2) 0.0284(16)
O4 0.0463(19) 0.159(4) 0.127(3) 0.082(3) -0.0074(19) 0.025(2)
O5 0.0510(17) 0.079(2) 0.096(2) 0.0365(18) 0.0195(16) 0.0242(15)
O6 0.0602(18) 0.0553(17) 0.0632(18) 0.0234(14) 0.0121(14) -0.0074(14)
O7 0.0666(19) 0.0650(19) 0.0482(17) 0.0182(15) 0.0075(14) -0.0145(15)
O8 0.078(2) 0.0581(18) 0.0594(18) 0.0131(15) 0.0156(16) -0.0032(15)
O9 0.084(2) 0.081(2) 0.080(2) 0.0515(18) -0.0006(18) 0.0020(18)
O10 0.0462(18) 0.106(3) 0.120(3) 0.042(2) 0.0322(19) 0.0100(17)
O1W 0.064(2) 0.0587(19) 0.105(3) 0.0020(18) -0.0043(19) 0.0329(16)
O2W 0.058(2) 0.080(2) 0.081(2) 0.0123(19) 0.0184(17) 0.0221(17)
O3W 0.061(2) 0.0558(18) 0.109(3) 0.0175(19) 0.0313(19) 0.0141(16)
O4W 0.084(3) 0.095(3) 0.090(3) 0.049(2) 0.025(2) 0.026(2)
O5W 0.065(2) 0.094(3) 0.072(2) 0.0143(19) 0.0122(17) 0.0234(19)
O6W 0.056(2) 0.065(2) 0.127(3) -0.003(2) 0.011(2) 0.0157(17)
O7W 0.103(3) 0.198(5) 0.095(3) 0.080(3) 0.034(3) 0.069(4)
O8W 0.140(4) 0.116(4) 0.114(4) 0.047(3) -0.005(3) 0.034(3)
O9W 0.160(5) 0.145(5) 0.109(4) -0.006(3) -0.043(3) 0.045(4)
O10W 0.163(6) 0.182(7) 0.167(7) -0.021(5) 0.015(5) 0.075(5)
O10' 0.068(8) 0.068(8) 0.101(11) -0.016(6) 0.005(6) 0.039(6)
C1 0.048(2) 0.041(2) 0.051(2) 0.0138(18) 0.0126(18) 0.0094(17)
C2 0.069(3) 0.043(2) 0.071(3) 0.023(2) 0.026(2) 0.007(2)
C3 0.047(2) 0.049(2) 0.076(3) 0.012(2) 0.017(2) -0.0058(19)
C4 0.036(2) 0.048(2) 0.055(2) 0.0030(19) 0.0139(18) 0.0037(17)
C5 0.032(2) 0.066(3) 0.073(3) 0.003(2) 0.010(2) 0.004(2)
C6 0.033(2) 0.084(3) 0.061(3) 0.007(2) 0.0023(19) 0.019(2)
C7 0.035(2) 0.064(3) 0.046(2) 0.0090(19) 0.0091(17) 0.0212(18)
C8 0.049(2) 0.086(3) 0.057(3) 0.026(2) 0.010(2) 0.040(2)
C9 0.058(3) 0.071(3) 0.065(3) 0.034(2) 0.020(2) 0.036(2)
C10 0.045(2) 0.047(2) 0.054(2) 0.0196(18) 0.0156(18) 0.0161(18)
C11 0.0313(18) 0.042(2) 0.0362(18) 0.0041(15) 0.0126(15) 0.0076(15)
C12 0.0309(18) 0.048(2) 0.0356(18) 0.0073(16) 0.0117(15) 0.0146(16)
C13 0.053(2) 0.039(2) 0.041(2) 0.0125(16) 0.0091(17) 0.0106(17)
C14 0.072(3) 0.050(2) 0.036(2) 0.0136(18) 0.018(2) 0.012(2)
C15 0.070(3) 0.049(2) 0.054(3) 0.0116(19) 0.035(2) 0.015(2)
C16 0.042(2) 0.0344(19) 0.057(2) 0.0099(17) 0.0220(18) 0.0048(16)
C17 0.044(2) 0.043(2) 0.083(3) 0.010(2) 0.028(2) 0.0108(18)
C18 0.036(2) 0.044(2) 0.090(3) 0.013(2) 0.011(2) 0.0123(18)
C19 0.0306(19) 0.0347(19) 0.068(3) 0.0131(18) -0.0015(18) 0.0038(15)
C20 0.049(2) 0.048(2) 0.079(3) 0.018(2) -0.013(2) 0.014(2)
C21 0.068(3) 0.060(3) 0.053(3) 0.021(2) -0.014(2) 0.010(2)
C22 0.051(2) 0.050(2) 0.041(2) 0.0120(18) 0.0013(18) 0.0074(18)
C23 0.0313(18) 0.0264(17) 0.049(2) 0.0081(15) 0.0107(15) 0.0036(14)
C24 0.0306(18) 0.0283(17) 0.048(2) 0.0106(15) 0.0042(15) 0.0027(14)
C25 0.038(2) 0.049(2) 0.052(2) 0.0194(18) 0.0079(17) 0.0064(17)
C26 0.043(2) 0.060(3) 0.076(3) 0.037(2) 0.011(2) 0.003(2)
C27 0.048(2) 0.044(2) 0.086(3) 0.022(2) -0.001(2) -0.0022(19)
C28 0.039(2) 0.040(2) 0.063(3) 0.0071(19) -0.0068(19) 0.0059(17)
C29 0.062(3) 0.038(2) 0.079(3) -0.007(2) -0.006(3) 0.006(2)
C30 0.066(3) 0.056(3) 0.058(3) -0.012(2) -0.004(2) 0.021(2)
C31 0.047(2) 0.061(3) 0.040(2) 0.0026(18) 0.0017(18) 0.026(2)
C32 0.071(3) 0.084(3) 0.040(2) 0.002(2) 0.014(2) 0.041(3)
C33 0.066(3) 0.076(3) 0.049(2) 0.025(2) 0.027(2) 0.029(2)
C34 0.054(2) 0.056(2) 0.046(2) 0.0181(19) 0.0187(19) 0.0199(19)
C35 0.0320(18) 0.0380(19) 0.044(2) 0.0086(16) -0.0023(15) 0.0116(15)
C36 0.0381(19) 0.0379(19) 0.0385(19) 0.0047(15) 0.0021(15) 0.0161(16)
C37 0.036(2) 0.041(2) 0.054(2) 0.0064(18) 0.0030(18) 0.0098(17)
C38 0.041(2) 0.0339(19) 0.053(2) 0.0096(16) 0.0065(17) 0.0110(16)
C39 0.0363(19) 0.0376(19) 0.056(2) 0.0153(17) 0.0053(17) 0.0106(16)
C40 0.040(2) 0.0347(19) 0.069(3) 0.0210(19) 0.0026(19) 0.0067(16)
C41 0.067(3) 0.046(2) 0.081(3) 0.032(2) 0.000(2) 0.015(2)
C42 0.084(3) 0.060(3) 0.066(3) 0.031(2) 0.022(3) 0.025(2)
C43 0.059(3) 0.045(2) 0.067(3) 0.020(2) 0.018(2) 0.0187(19)
C44 0.039(2) 0.046(2) 0.050(2) 0.0212(19) 0.0029(17) 0.0023(17)
C45 0.0357(19) 0.042(2) 0.050(2) 0.0188(17) 0.0041(16) 0.0085(16)
C46 0.042(2) 0.049(2) 0.039(2) 0.0149(17) 0.0037(16) 0.0113(17)
C47 0.0329(18) 0.051(2) 0.046(2) 0.0183(18) 0.0063(16) 0.0146(16)
C48 0.055(2) 0.062(3) 0.052(2) 0.019(2) 0.022(2) 0.027(2)
C49 0.060(3) 0.055(3) 0.053(2) 0.000(2) 0.009(2) 0.022(2)
C50 0.048(2) 0.042(2) 0.062(3) 0.0121(19) 0.006(2) 0.0121(18)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 2.090(3) . ?
Ni1 N2 2.093(3) . ?
Ni1 N4 2.093(3) . ?
Ni1 N6 2.101(3) . ?
Ni1 N3 2.105(3) . ?
Ni1 N5 2.110(3) . ?
S1 O5 1.434(3) . ?
S1 O4 1.436(3) . ?
S1 O3 1.450(3) . ?
S1 C40 1.785(4) . ?
S2 O10 1.425(3) . ?
S2 O8 1.442(3) . ?
S2 O9 1.444(3) . ?
S2 C47 1.776(4) . ?
N1 C1 1.318(4) . ?
N1 C11 1.353(4) . ?
N2 C10 1.331(4) . ?
N2 C12 1.358(4) . ?
N3 C13 1.328(4) . ?
N3 C23 1.357(4) . ?
N4 C22 1.328(4) . ?
N4 C24 1.357(4) . ?
N5 C25 1.326(4) . ?
N5 C35 1.359(4) . ?
N6 C34 1.329(4) . ?
N6 C36 1.355(4) . ?
O1 C37 1.255(4) . ?
O2 C37 1.275(4) . ?
O2 H2C 0.8200 . ?
O6 C44 1.302(4) . ?
O6 H6C 0.8200 . ?
O7 C44 1.215(4) . ?
O1W H1A 0.84(4) . ?
O1W H1B 0.84(3) . ?
O2W H2A 0.85(3) . ?
O2W H2B 0.85(3) . ?
O3W H3B 0.85(3) . ?
O3W H3A 0.85(3) . ?
O4W H4A 0.84(4) . ?
O4W H4B 0.85(3) . ?
O5W H5A 0.86(3) . ?
O5W H5B 0.86(5) . ?
O6W H6A 0.83(4) . ?
O6W H6B 0.84(3) . ?
O7W H7B 0.85(3) . ?
O7W H7A 0.86(4) . ?
O8W H8A 0.84(5) . ?
O8W H8B 0.85(5) . ?
O9W H9A 0.87(7) . ?
O9W H9B 0.85(6) . ?
C1 C2 1.394(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.347(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.404(6) . ?
C3 H3 0.9300 . ?
C4 C11 1.405(5) . ?
C4 C5 1.435(6) . ?
C5 C6 1.338(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.431(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.401(6) . ?
C7 C12 1.401(5) . ?
C8 C9 1.361(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.393(5) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.433(5) . ?
C13 C14 1.386(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.350(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.400(5) . ?
C15 H15 0.9300 . ?
C16 C23 1.409(4) . ?
C16 C17 1.420(5) . ?
C17 C18 1.350(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.420(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.390(6) . ?
C19 C24 1.403(5) . ?
C20 C21 1.359(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.404(5) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C24 1.430(5) . ?
C25 C26 1.390(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.358(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.400(6) . ?
C27 H27 0.9300 . ?
C28 C35 1.404(5) . ?
C28 C29 1.432(6) . ?
C29 C30 1.328(6) . ?
C29 H29 0.9300 . ?
C30 C31 1.430(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.396(6) . ?
C31 C36 1.405(5) . ?
C32 C33 1.350(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.400(5) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 C36 1.429(5) . ?
C37 C38 1.478(5) . ?
C38 C43 1.375(5) . ?
C38 C39 1.392(5) . ?
C39 C40 1.374(5) . ?
C39 H39 0.9300 . ?
C40 C41 1.377(6) . ?
C41 C42 1.384(6) . ?
C41 H41 0.9300 . ?
C42 C43 1.381(6) . ?
C42 H42 0.9300 . ?
C43 H43 0.9300 . ?
C44 C45 1.469(5) . ?
C45 C46 1.384(5) . ?
C45 C50 1.386(5) . ?
C46 C47 1.368(5) . ?
C46 H46 0.9300 . ?
C47 C48 1.389(5) . ?
C48 C49 1.382(5) . ?
C48 H48 0.9300 . ?
C49 C50 1.381(5) . ?
C49 H49 0.9300 . ?
C50 H50 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N2 79.70(11) . . ?
N1 Ni1 N4 94.44(11) . . ?
N2 Ni1 N4 168.31(10) . . ?
N1 Ni1 N6 92.98(10) . . ?
N2 Ni1 N6 95.73(10) . . ?
N4 Ni1 N6 94.66(11) . . ?
N1 Ni1 N3 97.10(10) . . ?
N2 Ni1 N3 91.66(10) . . ?
N4 Ni1 N3 78.95(11) . . ?
N6 Ni1 N3 168.43(11) . . ?
N1 Ni1 N5 168.06(10) . . ?
N2 Ni1 N5 92.14(11) . . ?
N4 Ni1 N5 95.08(11) . . ?
N6 Ni1 N5 79.08(11) . . ?
N3 Ni1 N5 91.79(10) . . ?
O5 S1 O4 112.3(2) . . ?
O5 S1 O3 111.3(2) . . ?
O4 S1 O3 114.8(2) . . ?
O5 S1 C40 107.55(18) . . ?
O4 S1 C40 106.1(2) . . ?
O3 S1 C40 104.06(17) . . ?
O10 S2 O8 113.0(2) . . ?
O10 S2 O9 113.1(2) . . ?
O8 S2 O9 111.7(2) . . ?
O10 S2 C47 106.91(19) . . ?
O8 S2 C47 106.06(17) . . ?
O9 S2 C47 105.33(17) . . ?
C1 N1 C11 117.6(3) . . ?
C1 N1 Ni1 129.8(2) . . ?
C11 N1 Ni1 112.6(2) . . ?
C10 N2 C12 117.9(3) . . ?
C10 N2 Ni1 129.3(2) . . ?
C12 N2 Ni1 112.4(2) . . ?
C13 N3 C23 117.6(3) . . ?
C13 N3 Ni1 129.8(2) . . ?
C23 N3 Ni1 112.3(2) . . ?
C22 N4 C24 117.8(3) . . ?
C22 N4 Ni1 129.2(3) . . ?
C24 N4 Ni1 113.0(2) . . ?
C25 N5 C35 117.5(3) . . ?
C25 N5 Ni1 129.4(2) . . ?
C35 N5 Ni1 112.9(2) . . ?
C34 N6 C36 118.1(3) . . ?
C34 N6 Ni1 128.9(3) . . ?
C36 N6 Ni1 113.1(2) . . ?
C37 O2 H2C 109.5 . . ?
C44 O6 H6C 109.5 . . ?
H1A O1W H1B 110(4) . . ?
H2A O2W H2B 109(4) . . ?
H3B O3W H3A 108(4) . . ?
H4A O4W H4B 109(4) . . ?
H5A O5W H5B 106(4) . . ?
H6A O6W H6B 111(4) . . ?
H7B O7W H7A 109(5) . . ?
H8A O8W H8B 109(6) . . ?
H9A O9W H9B 107(6) . . ?
N1 C1 C2 123.2(4) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C3 C2 C1 119.6(4) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C2 C3 C4 119.4(4) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C3 C4 C11 117.2(4) . . ?
C3 C4 C5 124.2(4) . . ?
C11 C4 C5 118.6(4) . . ?
C6 C5 C4 121.6(4) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C5 C6 C7 121.3(4) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C8 C7 C12 117.7(3) . . ?
C8 C7 C6 123.7(4) . . ?
C12 C7 C6 118.6(4) . . ?
C9 C8 C7 119.5(4) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C8 C9 C10 119.5(4) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
N2 C10 C9 122.8(4) . . ?
N2 C10 H10 118.6 . . ?
C9 C10 H10 118.6 . . ?
N1 C11 C4 122.8(3) . . ?
N1 C11 C12 117.6(3) . . ?
C4 C11 C12 119.6(3) . . ?
N2 C12 C7 122.5(3) . . ?
N2 C12 C11 117.2(3) . . ?
C7 C12 C11 120.3(3) . . ?
N3 C13 C14 122.9(4) . . ?
N3 C13 H13 118.6 . . ?
C14 C13 H13 118.6 . . ?
C15 C14 C13 119.8(4) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C16 120.0(4) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C23 116.6(3) . . ?
C15 C16 C17 124.4(4) . . ?
C23 C16 C17 119.0(4) . . ?
C18 C17 C16 121.2(4) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C17 C18 C19 121.3(4) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 H18 119.3 . . ?
C20 C19 C24 117.3(4) . . ?
C20 C19 C18 123.8(4) . . ?
C24 C19 C18 118.9(4) . . ?
C21 C20 C19 120.0(4) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C22 119.4(4) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
N4 C22 C21 122.4(4) . . ?
N4 C22 H22 118.8 . . ?
C21 C22 H22 118.8 . . ?
N3 C23 C16 123.1(3) . . ?
N3 C23 C24 117.3(3) . . ?
C16 C23 C24 119.5(3) . . ?
N4 C24 C19 123.1(3) . . ?
N4 C24 C23 117.0(3) . . ?
C19 C24 C23 119.9(3) . . ?
N5 C25 C26 123.4(4) . . ?
N5 C25 H25 118.3 . . ?
C26 C25 H25 118.3 . . ?
C27 C26 C25 119.4(4) . . ?
C27 C26 H26 120.3 . . ?
C25 C26 H26 120.3 . . ?
C26 C27 C28 119.4(4) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 H27 120.3 . . ?
C27 C28 C35 117.6(4) . . ?
C27 C28 C29 124.2(4) . . ?
C35 C28 C29 118.2(4) . . ?
C30 C29 C28 121.7(4) . . ?
C30 C29 H29 119.1 . . ?
C28 C29 H29 119.1 . . ?
C29 C30 C31 121.6(4) . . ?
C29 C30 H30 119.2 . . ?
C31 C30 H30 119.2 . . ?
C32 C31 C36 116.8(4) . . ?
C32 C31 C30 124.5(4) . . ?
C36 C31 C30 118.7(4) . . ?
C33 C32 C31 120.9(4) . . ?
C33 C32 H32 119.6 . . ?
C31 C32 H32 119.6 . . ?
C32 C33 C34 118.7(4) . . ?
C32 C33 H33 120.6 . . ?
C34 C33 H33 120.6 . . ?
N6 C34 C33 122.8(4) . . ?
N6 C34 H34 118.6 . . ?
C33 C34 H34 118.6 . . ?
N5 C35 C28 122.6(3) . . ?
N5 C35 C36 117.2(3) . . ?
C28 C35 C36 120.2(3) . . ?
N6 C36 C31 122.7(3) . . ?
N6 C36 C35 117.7(3) . . ?
C31 C36 C35 119.6(3) . . ?
O1 C37 O2 123.0(4) . . ?
O1 C37 C38 119.6(4) . . ?
O2 C37 C38 117.4(3) . . ?
C43 C38 C39 119.9(4) . . ?
C43 C38 C37 120.1(3) . . ?
C39 C38 C37 119.9(3) . . ?
C40 C39 C38 119.4(4) . . ?
C40 C39 H39 120.3 . . ?
C38 C39 H39 120.3 . . ?
C39 C40 C41 120.9(4) . . ?
C39 C40 S1 118.5(3) . . ?
C41 C40 S1 120.5(3) . . ?
C40 C41 C42 119.5(4) . . ?
C40 C41 H41 120.2 . . ?
C42 C41 H41 120.2 . . ?
C43 C42 C41 120.0(4) . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C38 C43 C42 120.2(4) . . ?
C38 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
O7 C44 O6 123.1(3) . . ?
O7 C44 C45 121.3(3) . . ?
O6 C44 C45 115.6(3) . . ?
C46 C45 C50 119.9(3) . . ?
C46 C45 C44 117.7(3) . . ?
C50 C45 C44 122.3(3) . . ?
C47 C46 C45 120.4(3) . . ?
C47 C46 H46 119.8 . . ?
C45 C46 H46 119.8 . . ?
C46 C47 C48 120.1(3) . . ?
C46 C47 S2 119.9(3) . . ?
C48 C47 S2 119.9(3) . . ?
C49 C48 C47 119.6(4) . . ?
C49 C48 H48 120.2 . . ?
C47 C48 H48 120.2 . . ?
C50 C49 C48 120.4(4) . . ?
C50 C49 H49 119.8 . . ?
C48 C49 H49 119.8 . . ?
C49 C50 C45 119.6(4) . . ?
C49 C50 H50 120.2 . . ?
C45 C50 H50 120.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Ni1 N1 C1 175.8(3) . . . . ?
N4 Ni1 N1 C1 -14.4(3) . . . . ?
N6 Ni1 N1 C1 80.5(3) . . . . ?
N3 Ni1 N1 C1 -93.8(3) . . . . ?
N5 Ni1 N1 C1 128.3(5) . . . . ?
N2 Ni1 N1 C11 -5.1(2) . . . . ?
N4 Ni1 N1 C11 164.7(2) . . . . ?
N6 Ni1 N1 C11 -100.3(2) . . . . ?
N3 Ni1 N1 C11 85.3(2) . . . . ?
N5 Ni1 N1 C11 -52.5(6) . . . . ?
N1 Ni1 N2 C10 178.9(3) . . . . ?
N4 Ni1 N2 C10 118.3(5) . . . . ?
N6 Ni1 N2 C10 -89.1(3) . . . . ?
N3 Ni1 N2 C10 82.0(3) . . . . ?
N5 Ni1 N2 C10 -9.8(3) . . . . ?
N1 Ni1 N2 C12 6.4(2) . . . . ?
N4 Ni1 N2 C12 -54.3(6) . . . . ?
N6 Ni1 N2 C12 98.4(2) . . . . ?
N3 Ni1 N2 C12 -90.6(2) . . . . ?
N5 Ni1 N2 C12 177.6(2) . . . . ?
N1 Ni1 N3 C13 -83.8(3) . . . . ?
N2 Ni1 N3 C13 -4.0(3) . . . . ?
N4 Ni1 N3 C13 -177.0(3) . . . . ?
N6 Ni1 N3 C13 125.8(5) . . . . ?
N5 Ni1 N3 C13 88.2(3) . . . . ?
N1 Ni1 N3 C23 103.9(2) . . . . ?
N2 Ni1 N3 C23 -176.3(2) . . . . ?
N4 Ni1 N3 C23 10.7(2) . . . . ?
N6 Ni1 N3 C23 -46.6(6) . . . . ?
N5 Ni1 N3 C23 -84.1(2) . . . . ?
N1 Ni1 N4 C22 76.3(3) . . . . ?
N2 Ni1 N4 C22 135.6(5) . . . . ?
N6 Ni1 N4 C22 -17.1(3) . . . . ?
N3 Ni1 N4 C22 172.7(3) . . . . ?
N5 Ni1 N4 C22 -96.5(3) . . . . ?
N1 Ni1 N4 C24 -105.8(2) . . . . ?
N2 Ni1 N4 C24 -46.5(6) . . . . ?
N6 Ni1 N4 C24 160.8(2) . . . . ?
N3 Ni1 N4 C24 -9.4(2) . . . . ?
N5 Ni1 N4 C24 81.4(2) . . . . ?
N1 Ni1 N5 C25 128.0(5) . . . . ?
N2 Ni1 N5 C25 81.5(3) . . . . ?
N4 Ni1 N5 C25 -89.3(3) . . . . ?
N6 Ni1 N5 C25 177.0(3) . . . . ?
N3 Ni1 N5 C25 -10.2(3) . . . . ?
N1 Ni1 N5 C35 -47.1(6) . . . . ?
N2 Ni1 N5 C35 -93.6(2) . . . . ?
N4 Ni1 N5 C35 95.6(2) . . . . ?
N6 Ni1 N5 C35 1.8(2) . . . . ?
N3 Ni1 N5 C35 174.7(2) . . . . ?
N1 Ni1 N6 C34 -10.1(3) . . . . ?
N2 Ni1 N6 C34 -90.0(3) . . . . ?
N4 Ni1 N6 C34 84.6(3) . . . . ?
N3 Ni1 N6 C34 140.6(5) . . . . ?
N5 Ni1 N6 C34 178.9(3) . . . . ?
N1 Ni1 N6 C36 170.8(2) . . . . ?
N2 Ni1 N6 C36 90.8(2) . . . . ?
N4 Ni1 N6 C36 -94.5(2) . . . . ?
N3 Ni1 N6 C36 -38.6(6) . . . . ?
N5 Ni1 N6 C36 -0.2(2) . . . . ?
C11 N1 C1 C2 -1.2(5) . . . . ?
Ni1 N1 C1 C2 178.0(3) . . . . ?
N1 C1 C2 C3 -0.7(6) . . . . ?
C1 C2 C3 C4 1.7(6) . . . . ?
C2 C3 C4 C11 -0.7(6) . . . . ?
C2 C3 C4 C5 -179.9(4) . . . . ?
C3 C4 C5 C6 179.6(4) . . . . ?
C11 C4 C5 C6 0.4(6) . . . . ?
C4 C5 C6 C7 0.6(6) . . . . ?
C5 C6 C7 C8 -179.2(4) . . . . ?
C5 C6 C7 C12 0.2(6) . . . . ?
C12 C7 C8 C9 3.3(5) . . . . ?
C6 C7 C8 C9 -177.3(4) . . . . ?
C7 C8 C9 C10 -1.6(6) . . . . ?
C12 N2 C10 C9 2.4(5) . . . . ?
Ni1 N2 C10 C9 -169.9(3) . . . . ?
C8 C9 C10 N2 -1.3(6) . . . . ?
C1 N1 C11 C4 2.2(5) . . . . ?
Ni1 N1 C11 C4 -177.1(3) . . . . ?
C1 N1 C11 C12 -177.6(3) . . . . ?
Ni1 N1 C11 C12 3.1(3) . . . . ?
C3 C4 C11 N1 -1.2(5) . . . . ?
C5 C4 C11 N1 178.0(3) . . . . ?
C3 C4 C11 C12 178.6(3) . . . . ?
C5 C4 C11 C12 -2.2(5) . . . . ?
C10 N2 C12 C7 -0.5(5) . . . . ?
Ni1 N2 C12 C7 173.0(3) . . . . ?
C10 N2 C12 C11 179.7(3) . . . . ?
Ni1 N2 C12 C11 -6.8(3) . . . . ?
C8 C7 C12 N2 -2.3(5) . . . . ?
C6 C7 C12 N2 178.3(3) . . . . ?
C8 C7 C12 C11 177.5(3) . . . . ?
C6 C7 C12 C11 -1.9(5) . . . . ?
N1 C11 C12 N2 2.6(4) . . . . ?
C4 C11 C12 N2 -177.2(3) . . . . ?
N1 C11 C12 C7 -177.2(3) . . . . ?
C4 C11 C12 C7 3.0(5) . . . . ?
C23 N3 C13 C14 1.1(5) . . . . ?
Ni1 N3 C13 C14 -170.9(3) . . . . ?
N3 C13 C14 C15 0.1(6) . . . . ?
C13 C14 C15 C16 -1.0(6) . . . . ?
C14 C15 C16 C23 0.7(5) . . . . ?
C14 C15 C16 C17 -177.9(4) . . . . ?
C15 C16 C17 C18 175.9(4) . . . . ?
C23 C16 C17 C18 -2.7(5) . . . . ?
C16 C17 C18 C19 0.5(6) . . . . ?
C17 C18 C19 C20 -175.8(4) . . . . ?
C17 C18 C19 C24 2.6(5) . . . . ?
C24 C19 C20 C21 0.9(5) . . . . ?
C18 C19 C20 C21 179.3(4) . . . . ?
C19 C20 C21 C22 1.5(6) . . . . ?
C24 N4 C22 C21 -1.2(5) . . . . ?
Ni1 N4 C22 C21 176.6(3) . . . . ?
C20 C21 C22 N4 -1.4(6) . . . . ?
C13 N3 C23 C16 -1.3(5) . . . . ?
Ni1 N3 C23 C16 172.1(2) . . . . ?
C13 N3 C23 C24 176.1(3) . . . . ?
Ni1 N3 C23 C24 -10.5(3) . . . . ?
C15 C16 C23 N3 0.4(5) . . . . ?
C17 C16 C23 N3 179.1(3) . . . . ?
C15 C16 C23 C24 -176.9(3) . . . . ?
C17 C16 C23 C24 1.8(5) . . . . ?
C22 N4 C24 C19 3.8(5) . . . . ?
Ni1 N4 C24 C19 -174.3(2) . . . . ?
C22 N4 C24 C23 -175.0(3) . . . . ?
Ni1 N4 C24 C23 6.9(3) . . . . ?
C20 C19 C24 N4 -3.7(5) . . . . ?
C18 C19 C24 N4 177.8(3) . . . . ?
C20 C19 C24 C23 175.1(3) . . . . ?
C18 C19 C24 C23 -3.4(5) . . . . ?
N3 C23 C24 N4 2.6(4) . . . . ?
C16 C23 C24 N4 -179.9(3) . . . . ?
N3 C23 C24 C19 -176.3(3) . . . . ?
C16 C23 C24 C19 1.2(5) . . . . ?
C35 N5 C25 C26 0.9(5) . . . . ?
Ni1 N5 C25 C26 -174.0(3) . . . . ?
N5 C25 C26 C27 -2.0(6) . . . . ?
C25 C26 C27 C28 1.3(6) . . . . ?
C26 C27 C28 C35 0.3(6) . . . . ?
C26 C27 C28 C29 -179.9(4) . . . . ?
C27 C28 C29 C30 179.6(4) . . . . ?
C35 C28 C29 C30 -0.5(6) . . . . ?
C28 C29 C30 C31 1.5(7) . . . . ?
C29 C30 C31 C32 179.0(4) . . . . ?
C29 C30 C31 C36 -0.4(6) . . . . ?
C36 C31 C32 C33 2.5(6) . . . . ?
C30 C31 C32 C33 -176.9(4) . . . . ?
C31 C32 C33 C34 -1.5(6) . . . . ?
C36 N6 C34 C33 1.0(5) . . . . ?
Ni1 N6 C34 C33 -178.1(3) . . . . ?
C32 C33 C34 N6 -0.4(6) . . . . ?
C25 N5 C35 C28 0.8(5) . . . . ?
Ni1 N5 C35 C28 176.5(3) . . . . ?
C25 N5 C35 C36 -178.9(3) . . . . ?
Ni1 N5 C35 C36 -3.1(4) . . . . ?
C27 C28 C35 N5 -1.4(5) . . . . ?
C29 C28 C35 N5 178.8(3) . . . . ?
C27 C28 C35 C36 178.3(3) . . . . ?
C29 C28 C35 C36 -1.6(5) . . . . ?
C34 N6 C36 C31 0.1(5) . . . . ?
Ni1 N6 C36 C31 179.4(3) . . . . ?
C34 N6 C36 C35 179.4(3) . . . . ?
Ni1 N6 C36 C35 -1.4(4) . . . . ?
C32 C31 C36 N6 -1.9(5) . . . . ?
C30 C31 C36 N6 177.5(3) . . . . ?
C32 C31 C36 C35 178.9(3) . . . . ?
C30 C31 C36 C35 -1.7(5) . . . . ?
N5 C35 C36 N6 3.1(4) . . . . ?
C28 C35 C36 N6 -176.6(3) . . . . ?
N5 C35 C36 C31 -177.7(3) . . . . ?
C28 C35 C36 C31 2.7(5) . . . . ?
O1 C37 C38 C43 -7.5(5) . . . . ?
O2 C37 C38 C43 172.3(3) . . . . ?
O1 C37 C38 C39 170.3(3) . . . . ?
O2 C37 C38 C39 -9.9(5) . . . . ?
C43 C38 C39 C40 0.5(5) . . . . ?
C37 C38 C39 C40 -177.2(3) . . . . ?
C38 C39 C40 C41 -0.2(5) . . . . ?
C38 C39 C40 S1 -176.8(3) . . . . ?
O5 S1 C40 C39 -32.0(3) . . . . ?
O4 S1 C40 C39 -152.4(3) . . . . ?
O3 S1 C40 C39 86.1(3) . . . . ?
O5 S1 C40 C41 151.4(3) . . . . ?
O4 S1 C40 C41 31.1(4) . . . . ?
O3 S1 C40 C41 -90.4(4) . . . . ?
C39 C40 C41 C42 -0.4(6) . . . . ?
S1 C40 C41 C42 176.1(3) . . . . ?
C40 C41 C42 C43 0.6(6) . . . . ?
C39 C38 C43 C42 -0.3(6) . . . . ?
C37 C38 C43 C42 177.5(4) . . . . ?
C41 C42 C43 C38 -0.3(6) . . . . ?
O7 C44 C45 C46 7.1(5) . . . . ?
O6 C44 C45 C46 -170.9(3) . . . . ?
O7 C44 C45 C50 -175.9(4) . . . . ?
O6 C44 C45 C50 6.1(5) . . . . ?
C50 C45 C46 C47 0.0(5) . . . . ?
C44 C45 C46 C47 177.1(3) . . . . ?
C45 C46 C47 C48 0.2(5) . . . . ?
C45 C46 C47 S2 -176.2(3) . . . . ?
O10 S2 C47 C46 -116.6(3) . . . . ?
O8 S2 C47 C46 4.3(3) . . . . ?
O9 S2 C47 C46 122.8(3) . . . . ?
O10 S2 C47 C48 67.0(3) . . . . ?
O8 S2 C47 C48 -172.1(3) . . . . ?
O9 S2 C47 C48 -53.6(3) . . . . ?
C46 C47 C48 C49 -0.2(6) . . . . ?
S2 C47 C48 C49 176.1(3) . . . . ?
C47 C48 C49 C50 0.0(6) . . . . ?
C48 C49 C50 C45 0.2(6) . . . . ?
C46 C45 C50 C49 -0.3(5) . . . . ?
C44 C45 C50 C49 -177.2(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
O2 H2C O1 0.82 1.81 2.624(4) 168.7 2_757
O6 H6C O7 0.82 1.79 2.596(4) 169.7 2_666
O6W H6A O5W 0.83(4) 1.92(3) 2.746(5) 174(5) 2_667
O1W H1A O3 0.84(4) 1.92(4) 2.750(4) 171(5) .
O1W H1B O9 0.84(3) 2.01(3) 2.845(4) 170(4) .
O5W H5A O10 0.86(3) 2.031(18) 2.863(5) 163(4) .
O5W H5B O3W 0.86(5) 2.02(4) 2.863(5) 169(4) 1_455
O2W H2A O1W 0.85(3) 2.011(16) 2.840(5) 167(5) 2_667
O2W H2B O1W 0.85(3) 2.028(16) 2.859(5) 166(4) .
O3W H3A O6W 0.85(3) 1.80(3) 2.654(4) 174(4) .
O9W H9B O8 0.85(6) 2.08(4) 2.835(5) 148(6) .
O4W H4A O3W 0.84(4) 2.04(2) 2.852(5) 160(4) .
O4W H4B O10 0.85(3) 2.05(4) 2.894(5) 175(4) 1_655
O6W H6B O2W 0.84(3) 1.926(16) 2.745(5) 164(5) .
O7W H7B O8 0.85(3) 2.18(3) 2.964(5) 154(6) .
O7W H7A O4 0.86(4) 1.97(3) 2.766(5) 154(7) .

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.059

data_comp-4
_database_code_depnum_ccdc_archive 'CCDC 697405'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H16 N2 Ni O7 S, H2 O'
_chemical_formula_sum            'C17 H18 N2 Ni O8 S'
_chemical_formula_weight         469.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'

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

_cell_length_a                   7.989(4)
_cell_length_b                   15.006(7)
_cell_length_c                   8.168(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.145(8)
_cell_angle_gamma                90.00
_cell_volume                     925.1(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4031
_cell_measurement_theta_min      2.64
_cell_measurement_theta_max      28.30

_exptl_crystal_description       block
_exptl_crystal_colour            blue-green
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             484
_exptl_absorpt_coefficient_mu    1.212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_T_max  0.781
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(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 SMART area-detector diffractometer'
_diffrn_measurement_method       '\f and \w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5586
_diffrn_reflns_av_R_equivalents  0.0159
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.64
_diffrn_reflns_theta_max         27.09
_reflns_number_total             3799
_reflns_number_gt                3661
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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.

Hydrogen atoms on carbon atoms were
placed in idealized positions and refined as riding atoms,
with C-H = 0.93 \%A and Uiso(H) = 1.2Ueq(C). Hydrogen atoms on water
molecules were added according to the Fourier map with the restriction
of O-H = 0.85 \%A and Uiso(H) = 1.2 Ueq(O).
;

_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^)+(0.0379P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.044(10)
_refine_ls_number_reflns         3799
_refine_ls_number_parameters     280
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0270
_refine_ls_wR_factor_ref         0.0668
_refine_ls_wR_factor_gt          0.0662
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_restrained_S_all      0.879
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         <0.001

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 0.64677(4) 0.983456(19) 0.61501(3) 0.02422(8) Uani 1 1 d . . .
S1 S 1.26568(7) 1.06542(4) 1.62929(7) 0.02601(13) Uani 1 1 d . . .
N1 N 0.4802(3) 0.93685(13) 0.3815(2) 0.0275(4) Uani 1 1 d . . .
N2 N 0.6819(3) 1.07973(13) 0.4502(3) 0.0274(4) Uani 1 1 d . . .
O1 O 0.8204(2) 1.03632(12) 0.8306(2) 0.0316(4) Uani 1 1 d . . .
O2 O 0.7999(3) 0.94231(13) 1.0327(2) 0.0448(5) Uani 1 1 d . . .
O3 O 1.2045(2) 0.97563(15) 1.6452(2) 0.0360(4) Uani 1 1 d . . .
O4 O 1.2083(3) 1.13072(13) 1.7293(2) 0.0400(4) Uani 1 1 d . . .
O5 O 1.4573(2) 1.06897(12) 1.6682(2) 0.0318(4) Uani 1 1 d . . .
O6 O 0.5619(3) 0.88599(12) 0.7527(2) 0.0331(4) Uani 1 1 d D . .
O7 O 0.8570(2) 0.90502(13) 0.6008(2) 0.0351(4) Uani 1 1 d D . .
O1W O 0.8386(5) 0.82016(16) 0.3034(3) 0.0728(8) Uani 1 1 d D . .
C1 C 0.3842(4) 0.86252(19) 0.3562(4) 0.0399(6) Uani 1 1 d . . .
H1 H 0.3964 0.8252 0.4503 0.048 Uiso 1 1 calc R . .
C2 C 0.2683(4) 0.8386(2) 0.1977(4) 0.0452(7) Uani 1 1 d . . .
H2 H 0.2033 0.7862 0.1844 0.054 Uiso 1 1 calc R . .
C3 C 0.2500(4) 0.8942(2) 0.0582(4) 0.0431(7) Uani 1 1 d . . .
H3 H 0.1707 0.8802 -0.0505 0.052 Uiso 1 1 calc R . .
C4 C 0.3502(3) 0.9703(2) 0.0818(3) 0.0371(6) Uani 1 1 d . . .
H4 H 0.3401 1.0083 -0.0110 0.045 Uiso 1 1 calc R . .
C5 C 0.4667(3) 0.9902(2) 0.2452(3) 0.0283(5) Uani 1 1 d . . .
C6 C 0.5790(3) 1.07034(16) 0.2839(3) 0.0272(5) Uani 1 1 d . . .
C7 C 0.5799(4) 1.13390(19) 0.1608(4) 0.0391(6) Uani 1 1 d . . .
H7 H 0.5091 1.1267 0.0458 0.047 Uiso 1 1 calc R . .
C8 C 0.6869(4) 1.2076(2) 0.2109(4) 0.0461(7) Uani 1 1 d . . .
H8 H 0.6880 1.2510 0.1300 0.055 Uiso 1 1 calc R . .
C9 C 0.7913(4) 1.21689(18) 0.3795(4) 0.0415(6) Uani 1 1 d . . .
H9 H 0.8643 1.2663 0.4153 0.050 Uiso 1 1 calc R . .
C10 C 0.7859(4) 1.15087(16) 0.4964(3) 0.0330(5) Uani 1 1 d . . .
H10 H 0.8577 1.1566 0.6114 0.040 Uiso 1 1 calc R . .
C11 C 0.8596(3) 1.01054(16) 0.9846(3) 0.0267(5) Uani 1 1 d . . .
C12 C 0.9888(3) 1.06844(16) 1.1176(3) 0.0257(5) Uani 1 1 d . . .
C13 C 1.0539(3) 1.04254(15) 1.2909(3) 0.0250(5) Uani 1 1 d . . .
H13 H 1.0170 0.9893 1.3264 0.030 Uiso 1 1 calc R . .
C14 C 1.1732(3) 1.09657(16) 1.4088(3) 0.0265(5) Uani 1 1 d . . .
C15 C 1.2271(4) 1.17731(17) 1.3584(3) 0.0334(5) Uani 1 1 d . . .
H15 H 1.3058 1.2139 1.4400 0.040 Uiso 1 1 calc R . .
C16 C 1.1632(4) 1.20260(18) 1.1875(3) 0.0361(6) Uani 1 1 d . . .
H16 H 1.1982 1.2564 1.1526 0.043 Uiso 1 1 calc R . .
C17 C 1.0467(4) 1.14765(17) 1.0679(3) 0.0316(5) Uani 1 1 d . . .
H17 H 1.0062 1.1642 0.9518 0.038 Uiso 1 1 calc R . .
H7A H 0.838(3) 0.8788(18) 0.505(2) 0.042 Uiso 1 1 d D . .
H6A H 0.636(3) 0.892(2) 0.8549(19) 0.040 Uiso 1 1 d D . .
H6B H 0.4633(19) 0.906(2) 0.753(3) 0.040 Uiso 1 1 d D . .
H1A H 0.790(5) 0.7698(14) 0.270(5) 0.087 Uiso 1 1 d D . .
H1B H 0.816(6) 0.854(2) 0.216(3) 0.087 Uiso 1 1 d D . .
H7B H 0.955(2) 0.9322(18) 0.625(3) 0.042 Uiso 1 1 d 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 0.02462(14) 0.02644(14) 0.01902(13) 0.00165(11) 0.00366(10) -0.00247(13)
S1 0.0240(3) 0.0337(3) 0.0181(2) -0.0013(2) 0.0039(2) 0.0004(2)
N1 0.0287(11) 0.0293(10) 0.0239(10) -0.0005(8) 0.0077(8) -0.0037(8)
N2 0.0279(10) 0.0282(10) 0.0271(10) 0.0003(8) 0.0102(8) 0.0008(8)
O1 0.0298(9) 0.0398(10) 0.0200(8) 0.0025(7) 0.0012(7) -0.0062(7)
O2 0.0547(13) 0.0429(10) 0.0256(9) 0.0060(8) -0.0022(8) -0.0207(9)
O3 0.0338(9) 0.0451(10) 0.0263(8) 0.0052(9) 0.0061(7) -0.0065(10)
O4 0.0422(11) 0.0513(11) 0.0271(9) -0.0032(8) 0.0122(8) 0.0080(9)
O5 0.0244(9) 0.0374(9) 0.0303(9) -0.0039(7) 0.0045(7) 0.0007(7)
O6 0.0346(10) 0.0323(9) 0.0287(9) 0.0045(7) 0.0054(8) -0.0033(8)
O7 0.0333(10) 0.0335(9) 0.0380(10) -0.0026(8) 0.0108(8) -0.0011(8)
O1W 0.130(3) 0.0476(14) 0.0392(12) 0.0022(10) 0.0263(15) -0.0097(15)
C1 0.0485(16) 0.0363(14) 0.0330(13) -0.0016(10) 0.0108(12) -0.0090(12)
C2 0.0450(16) 0.0426(15) 0.0437(16) -0.0129(12) 0.0087(13) -0.0118(13)
C3 0.0400(15) 0.0540(17) 0.0282(13) -0.0134(12) 0.0015(11) 0.0054(14)
C4 0.0389(13) 0.0467(17) 0.0222(11) -0.0015(11) 0.0052(10) 0.0091(13)
C5 0.0295(11) 0.0347(12) 0.0208(10) -0.0006(10) 0.0084(8) 0.0062(12)
C6 0.0277(11) 0.0324(12) 0.0235(11) 0.0033(9) 0.0110(9) 0.0054(10)
C7 0.0444(16) 0.0453(15) 0.0291(13) 0.0098(11) 0.0141(12) 0.0058(13)
C8 0.0577(19) 0.0362(15) 0.0533(19) 0.0156(13) 0.0303(16) 0.0049(13)
C9 0.0435(16) 0.0273(13) 0.0589(19) 0.0043(12) 0.0239(14) -0.0021(12)
C10 0.0318(13) 0.0327(13) 0.0349(13) -0.0023(10) 0.0113(11) -0.0018(11)
C11 0.0218(11) 0.0326(13) 0.0235(12) -0.0014(8) 0.0044(9) 0.0027(9)
C12 0.0255(11) 0.0277(11) 0.0230(10) -0.0006(9) 0.0065(9) 0.0049(10)
C13 0.0241(11) 0.0279(12) 0.0220(11) -0.0008(8) 0.0062(9) -0.0007(9)
C14 0.0237(12) 0.0350(12) 0.0212(10) -0.0008(9) 0.0081(9) 0.0019(9)
C15 0.0357(14) 0.0335(13) 0.0280(12) -0.0049(9) 0.0064(11) -0.0082(11)
C16 0.0425(15) 0.0308(13) 0.0340(14) 0.0034(10) 0.0112(11) -0.0051(11)
C17 0.0351(14) 0.0359(13) 0.0221(11) 0.0024(9) 0.0069(10) 0.0023(11)

_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 2.0130(18) . ?
Ni1 N2 2.056(2) . ?
Ni1 N1 2.057(2) . ?
Ni1 O7 2.085(2) . ?
Ni1 O6 2.0891(18) . ?
Ni1 O5 2.1346(19) 1_454 ?
S1 O4 1.4431(19) . ?
S1 O3 1.454(2) . ?
S1 O5 1.4592(19) . ?
S1 C14 1.771(2) . ?
N1 C1 1.331(3) . ?
N1 C5 1.347(3) . ?
N2 C10 1.329(3) . ?
N2 C6 1.344(3) . ?
O1 C11 1.253(3) . ?
O2 C11 1.247(3) . ?
O5 Ni1 2.1346(19) 1_656 ?
O6 H6A 0.857(10) . ?
O6 H6B 0.843(10) . ?
O7 H7A 0.844(19) . ?
O7 H7B 0.844(10) . ?
O1W H1A 0.85(3) . ?
O1W H1B 0.85(3) . ?
C1 C2 1.370(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.381(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.372(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.386(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.472(4) . ?
C6 C7 1.388(3) . ?
C7 C8 1.375(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.363(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.386(4) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.505(3) . ?
C12 C17 1.384(4) . ?
C12 C13 1.393(3) . ?
C13 C14 1.375(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.392(4) . ?
C15 C16 1.373(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.380(4) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?

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 N2 95.35(8) . . ?
O1 Ni1 N1 174.61(7) . . ?
N2 Ni1 N1 79.48(8) . . ?
O1 Ni1 O7 86.27(8) . . ?
N2 Ni1 O7 94.29(8) . . ?
N1 Ni1 O7 92.54(8) . . ?
O1 Ni1 O6 93.27(8) . . ?
N2 Ni1 O6 169.32(8) . . ?
N1 Ni1 O6 92.04(8) . . ?
O7 Ni1 O6 92.55(8) . . ?
O1 Ni1 O5 85.19(8) . 1_454 ?
N2 Ni1 O5 88.22(8) . 1_454 ?
N1 Ni1 O5 96.13(8) . 1_454 ?
O7 Ni1 O5 171.29(7) . 1_454 ?
O6 Ni1 O5 86.23(8) . 1_454 ?
O4 S1 O3 113.60(12) . . ?
O4 S1 O5 110.94(12) . . ?
O3 S1 O5 111.95(11) . . ?
O4 S1 C14 107.00(12) . . ?
O3 S1 C14 107.18(11) . . ?
O5 S1 C14 105.65(11) . . ?
C1 N1 C5 118.9(2) . . ?
C1 N1 Ni1 126.41(17) . . ?
C5 N1 Ni1 114.62(17) . . ?
C10 N2 C6 119.3(2) . . ?
C10 N2 Ni1 125.81(17) . . ?
C6 N2 Ni1 114.74(16) . . ?
C11 O1 Ni1 129.06(16) . . ?
S1 O5 Ni1 134.20(11) . 1_656 ?
Ni1 O6 H6A 102(2) . . ?
Ni1 O6 H6B 103(2) . . ?
H6A O6 H6B 108.0(15) . . ?
Ni1 O7 H7A 114(2) . . ?
Ni1 O7 H7B 114(2) . . ?
H7A O7 H7B 108.7(15) . . ?
H1A O1W H1B 108.1(17) . . ?
N1 C1 C2 122.9(3) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C1 C2 C3 118.6(3) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
C4 C3 C2 119.2(3) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 119.4(3) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 121.0(3) . . ?
N1 C5 C6 115.47(19) . . ?
C4 C5 C6 123.5(2) . . ?
N2 C6 C7 120.9(2) . . ?
N2 C6 C5 115.5(2) . . ?
C7 C6 C5 123.6(2) . . ?
C8 C7 C6 119.2(3) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C9 C8 C7 119.8(3) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 118.4(3) . . ?
C8 C9 H9 120.8 . . ?
C10 C9 H9 120.8 . . ?
N2 C10 C9 122.4(3) . . ?
N2 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
O2 C11 O1 125.1(2) . . ?
O2 C11 C12 119.3(2) . . ?
O1 C11 C12 115.7(2) . . ?
C17 C12 C13 119.2(2) . . ?
C17 C12 C11 120.0(2) . . ?
C13 C12 C11 120.8(2) . . ?
C14 C13 C12 119.3(2) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C13 C14 C15 121.1(2) . . ?
C13 C14 S1 121.26(18) . . ?
C15 C14 S1 117.63(18) . . ?
C16 C15 C14 119.5(2) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C15 C16 C17 119.6(2) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C16 C17 C12 121.2(2) . . ?
C16 C17 H17 119.4 . . ?
C12 C17 H17 119.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Ni1 N1 C1 178.6(2) . . . . ?
O7 Ni1 N1 C1 84.7(2) . . . . ?
O6 Ni1 N1 C1 -8.0(2) . . . . ?
O5 Ni1 N1 C1 -94.4(2) 1_454 . . . ?
N2 Ni1 N1 C5 -3.61(16) . . . . ?
O7 Ni1 N1 C5 -97.50(17) . . . . ?
O6 Ni1 N1 C5 169.85(17) . . . . ?
O5 Ni1 N1 C5 83.43(17) 1_454 . . . ?
O1 Ni1 N2 C10 -2.3(2) . . . . ?
N1 Ni1 N2 C10 179.2(2) . . . . ?
O7 Ni1 N2 C10 -89.0(2) . . . . ?
O6 Ni1 N2 C10 141.4(4) . . . . ?
O5 Ni1 N2 C10 82.7(2) 1_454 . . . ?
O1 Ni1 N2 C6 -177.66(16) . . . . ?
N1 Ni1 N2 C6 3.90(16) . . . . ?
O7 Ni1 N2 C6 95.69(17) . . . . ?
O6 Ni1 N2 C6 -34.0(5) . . . . ?
O5 Ni1 N2 C6 -92.67(17) 1_454 . . . ?
N2 Ni1 O1 C11 177.4(2) . . . . ?
O7 Ni1 O1 C11 -88.6(2) . . . . ?
O6 Ni1 O1 C11 3.7(2) . . . . ?
O5 Ni1 O1 C11 89.6(2) 1_454 . . . ?
O4 S1 O5 Ni1 166.86(13) . . . 1_656 ?
O3 S1 O5 Ni1 38.81(17) . . . 1_656 ?
C14 S1 O5 Ni1 -77.52(16) . . . 1_656 ?
C5 N1 C1 C2 -1.7(4) . . . . ?
Ni1 N1 C1 C2 176.1(2) . . . . ?
N1 C1 C2 C3 -0.1(5) . . . . ?
C1 C2 C3 C4 1.1(4) . . . . ?
C2 C3 C4 C5 -0.4(4) . . . . ?
C1 N1 C5 C4 2.4(4) . . . . ?
Ni1 N1 C5 C4 -175.62(19) . . . . ?
C1 N1 C5 C6 -179.2(2) . . . . ?
Ni1 N1 C5 C6 2.8(3) . . . . ?
C3 C4 C5 N1 -1.3(4) . . . . ?
C3 C4 C5 C6 -179.6(2) . . . . ?
C10 N2 C6 C7 -0.2(4) . . . . ?
Ni1 N2 C6 C7 175.49(19) . . . . ?
C10 N2 C6 C5 -179.2(2) . . . . ?
Ni1 N2 C6 C5 -3.6(3) . . . . ?
N1 C5 C6 N2 0.5(3) . . . . ?
C4 C5 C6 N2 178.9(2) . . . . ?
N1 C5 C6 C7 -178.5(2) . . . . ?
C4 C5 C6 C7 -0.2(4) . . . . ?
N2 C6 C7 C8 -0.5(4) . . . . ?
C5 C6 C7 C8 178.5(2) . . . . ?
C6 C7 C8 C9 0.6(4) . . . . ?
C7 C8 C9 C10 -0.1(4) . . . . ?
C6 N2 C10 C9 0.7(4) . . . . ?
Ni1 N2 C10 C9 -174.40(19) . . . . ?
C8 C9 C10 N2 -0.6(4) . . . . ?
Ni1 O1 C11 O2 3.0(4) . . . . ?
Ni1 O1 C11 C12 -176.82(15) . . . . ?
O2 C11 C12 C17 -175.4(2) . . . . ?
O1 C11 C12 C17 4.4(3) . . . . ?
O2 C11 C12 C13 5.7(4) . . . . ?
O1 C11 C12 C13 -174.5(2) . . . . ?
C17 C12 C13 C14 0.4(3) . . . . ?
C11 C12 C13 C14 179.3(2) . . . . ?
C12 C13 C14 C15 1.3(4) . . . . ?
C12 C13 C14 S1 -177.97(17) . . . . ?
O4 S1 C14 C13 -116.8(2) . . . . ?
O3 S1 C14 C13 5.4(2) . . . . ?
O5 S1 C14 C13 124.9(2) . . . . ?
O4 S1 C14 C15 63.9(2) . . . . ?
O3 S1 C14 C15 -173.93(19) . . . . ?
O5 S1 C14 C15 -54.4(2) . . . . ?
C13 C14 C15 C16 -1.5(4) . . . . ?
S1 C14 C15 C16 177.8(2) . . . . ?
C14 C15 C16 C17 -0.1(4) . . . . ?
C15 C16 C17 C12 1.8(4) . . . . ?
C13 C12 C17 C16 -2.0(4) . . . . ?
C11 C12 C17 C16 179.1(2) . . . . ?

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
O7 H7A O1W 0.844(19) 1.867(12) 2.704(3) 170(3) .
O6 H6A O2 0.857(10) 1.770(15) 2.590(3) 159(3) .
O6 H6B O3 0.843(10) 2.224(14) 3.014(3) 156(3) 1_454
O1W H1A O4 0.85(3) 2.09(2) 2.868(3) 152(4) 2_747
O1W H1B O2 0.85(3) 1.97(3) 2.810(3) 171(4) 1_554
O7 H7B O3 0.844(10) 2.056(13) 2.881(3) 166(3) 1_554

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.09
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.054

data_comp-5
_database_code_depnum_ccdc_archive 'CCDC 697406'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C30 H24 N6 Ni), C7 H5 O5 S, 3(N O3), 8(H2 O), O'
_chemical_formula_sum            'C67 H71 N15 Ni2 O23 S'
_chemical_formula_weight         1603.87

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   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   22.7084(12)
_cell_length_b                   13.3203(7)
_cell_length_c                   24.1383(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.8210(10)
_cell_angle_gamma                90.00
_cell_volume                     7292.6(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3336
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(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 SMART area-detector diffractometer'
_diffrn_measurement_method       '\f and \w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            52787
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.20
_diffrn_reflns_theta_max         25.20
_reflns_number_total             13110
_reflns_number_gt                9796
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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.

Hydrogen atoms on carbon atoms were placed in idealized positions and
refined as riding atoms, with C-H = 0.93 \%A and Uiso(H) = 1.2Ueq(C).
Hydrogen atoms on O8w were not added. H atoms on other water molecules and
hydroxyl were added according to the Fourier map with the restriction of
O-H = 0.85 \%A and Uiso(H) = 1.2 Ueq(O).
;

_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^)+(0.0715P)^2^+4.7081P] 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         13110
_refine_ls_number_parameters     1021
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0493
_refine_ls_wR_factor_ref         0.1392
_refine_ls_wR_factor_gt          0.1246
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      0.995
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         <0.001

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 0.240420(17) 0.21505(3) 0.165739(16) 0.03760(12) Uani 1 1 d . . .
Ni2 Ni 0.243523(17) 0.16675(3) 0.833268(16) 0.03796(12) Uani 1 1 d . . .
S1 S 0.92446(4) 0.33351(7) 0.03730(4) 0.0546(2) Uani 1 1 d . . .
N1 N 0.28426(11) 0.1298(2) 0.10776(11) 0.0434(6) Uani 1 1 d . . .
N2 N 0.19444(11) 0.07886(19) 0.16812(11) 0.0422(6) Uani 1 1 d . . .
N3 N 0.28504(11) 0.34663(18) 0.14838(11) 0.0416(6) Uani 1 1 d . . .
N4 N 0.18355(11) 0.2799(2) 0.10566(11) 0.0426(6) Uani 1 1 d . . .
N5 N 0.29689(11) 0.16698(19) 0.23196(11) 0.0435(6) Uani 1 1 d . . .
N6 N 0.19769(11) 0.26984(19) 0.23377(11) 0.0422(6) Uani 1 1 d . . .
N7 N 0.30387(12) 0.2463(2) 0.88530(11) 0.0478(7) Uani 1 1 d . . .
N8 N 0.20000(11) 0.30305(19) 0.84182(11) 0.0423(6) Uani 1 1 d . . .
N9 N 0.20599(11) 0.0997(2) 0.90119(10) 0.0422(6) Uani 1 1 d . . .
N10 N 0.29135(11) 0.03266(19) 0.84018(11) 0.0438(6) Uani 1 1 d . . .
N11 N 0.18095(11) 0.10947(19) 0.77523(11) 0.0420(6) Uani 1 1 d . . .
N12 N 0.27839(12) 0.2109(2) 0.75917(11) 0.0453(6) Uani 1 1 d . . .
N13 N 0.49091(16) 0.2484(3) 0.21967(15) 0.0689(9) Uani 1 1 d . . .
N14 N 0.0037(2) 0.1657(4) 0.3107(3) 0.1008(15) Uani 1 1 d . . .
N15 N 0.3496(2) 0.6720(3) 0.98169(17) 0.0753(10) Uani 1 1 d . . .
O1 O 0.95633(13) -0.0247(2) -0.06020(11) 0.0692(7) Uani 1 1 d . . .
O2 O 1.01542(12) 0.0060(2) -0.12902(11) 0.0693(7) Uani 1 1 d . . .
H2C H 1.0146 -0.0554 -0.1320 0.104 Uiso 1 1 calc RD . .
O3 O 0.92848(15) 0.2559(2) 0.07793(12) 0.0892(10) Uani 1 1 d . . .
O4 O 0.86512(12) 0.3624(3) 0.02099(14) 0.0873(10) Uani 1 1 d . . .
O5 O 0.95989(13) 0.4208(2) 0.05315(12) 0.0763(8) Uani 1 1 d . . .
O6 O 0.4771(3) 0.2133(3) 0.17400(16) 0.148(2) Uani 1 1 d . . .
O7 O 0.52662(16) 0.2058(3) 0.25016(15) 0.1062(12) Uani 1 1 d . . .
O8 O 0.46701(17) 0.3231(3) 0.23423(18) 0.1199(14) Uani 1 1 d . . .
O9 O 0.0344(2) 0.1126(5) 0.2865(3) 0.186(3) Uani 1 1 d . . .
O10 O -0.0290(2) 0.2140(4) 0.2840(4) 0.210(3) Uani 1 1 d . . .
O11 O 0.0109(4) 0.1664(9) 0.3585(3) 0.292(6) Uani 1 1 d . . .
O12 O 0.3915(2) 0.6351(4) 0.9599(2) 0.1467(18) Uani 1 1 d . . .
O13 O 0.30041(16) 0.6457(3) 0.96589(14) 0.0925(10) Uani 1 1 d . . .
O14 O 0.35670(18) 0.7366(3) 1.01864(16) 0.1108(12) Uani 1 1 d . . .
O1W O 0.77753(14) 0.2652(3) 0.95751(12) 0.0795(8) Uani 1 1 d D . .
O2W O 0.95940(18) 0.4103(3) 0.25238(16) 0.1093(12) Uani 1 1 d D . .
O3W O 0.02811(15) 0.4276(4) 0.15689(14) 0.1081(12) Uani 1 1 d D . .
O4W O 0.4714(2) 0.8302(3) 0.98930(19) 0.1166(13) Uani 1 1 d D . .
O5W O 0.99221(19) 0.8251(3) 0.83757(18) 0.1098(12) Uani 1 1 d D . .
O6W O 0.4599(2) 0.2989(4) 0.07183(16) 0.1162(13) Uani 1 1 d D . .
O7W O 0.0226(2) 0.5073(3) 0.33542(18) 0.1128(12) Uani 1 1 d D . .
O8W O 0.5327(2) 0.9694(4) 0.0612(2) 0.1612(19) Uani 1 1 d . . .
O9W O 0.0203(2) 0.0126(5) 0.4429(3) 0.184(2) Uani 1 1 d D . .
C1 C 0.33186(16) 0.1579(3) 0.08025(15) 0.0539(9) Uani 1 1 d . . .
H1 H 0.3439 0.2246 0.0826 0.065 Uiso 1 1 calc R . .
C2 C 0.36322(17) 0.0936(3) 0.04928(16) 0.0631(10) Uani 1 1 d . . .
H2 H 0.3958 0.1161 0.0309 0.076 Uiso 1 1 calc R . .
C3 C 0.34586(18) -0.0053(3) 0.04560(16) 0.0647(10) Uani 1 1 d . . .
H3 H 0.3669 -0.0509 0.0251 0.078 Uiso 1 1 calc R . .
C4 C 0.29714(16) -0.0357(3) 0.07265(15) 0.0545(9) Uani 1 1 d . . .
H4 H 0.2843 -0.1019 0.0699 0.065 Uiso 1 1 calc R . .
C5 C 0.26723(13) 0.0330(2) 0.10406(13) 0.0412(7) Uani 1 1 d . . .
C6 C 0.21515(13) 0.0060(2) 0.13568(13) 0.0414(7) Uani 1 1 d . . .
C7 C 0.18896(15) -0.0884(2) 0.13299(16) 0.0523(9) Uani 1 1 d . . .
H7 H 0.2039 -0.1383 0.1107 0.063 Uiso 1 1 calc R . .
C8 C 0.14077(16) -0.1069(3) 0.16368(17) 0.0586(10) Uani 1 1 d . . .
H8 H 0.1228 -0.1696 0.1623 0.070 Uiso 1 1 calc R . .
C9 C 0.11937(15) -0.0329(3) 0.19626(16) 0.0545(9) Uani 1 1 d . . .
H9 H 0.0867 -0.0441 0.2171 0.065 Uiso 1 1 calc R . .
C10 C 0.14744(14) 0.0587(3) 0.19747(14) 0.0494(8) Uani 1 1 d . . .
H10 H 0.1330 0.1091 0.2198 0.059 Uiso 1 1 calc R . .
C11 C 0.33789(15) 0.3738(3) 0.17030(15) 0.0530(9) Uani 1 1 d . . .
H11 H 0.3551 0.3350 0.1987 0.064 Uiso 1 1 calc R . .
C12 C 0.36776(17) 0.4563(3) 0.15277(17) 0.0614(10) Uani 1 1 d . . .
H12 H 0.4042 0.4734 0.1693 0.074 Uiso 1 1 calc R . .
C13 C 0.34323(19) 0.5128(3) 0.11075(19) 0.0685(11) Uani 1 1 d . . .
H13 H 0.3629 0.5687 0.0979 0.082 Uiso 1 1 calc R . .
C14 C 0.28889(18) 0.4861(3) 0.08745(16) 0.0603(10) Uani 1 1 d . . .
H14 H 0.2715 0.5240 0.0587 0.072 Uiso 1 1 calc R . .
C15 C 0.26029(14) 0.4023(2) 0.10713(13) 0.0434(7) Uani 1 1 d . . .
C16 C 0.20197(14) 0.3675(3) 0.08452(13) 0.0456(8) Uani 1 1 d . . .
C17 C 0.16780(17) 0.4200(3) 0.04543(15) 0.0628(10) Uani 1 1 d . . .
H17 H 0.1814 0.4800 0.0310 0.075 Uiso 1 1 calc R . .
C18 C 0.11327(19) 0.3826(4) 0.02793(18) 0.0735(12) Uani 1 1 d . . .
H18 H 0.0895 0.4175 0.0020 0.088 Uiso 1 1 calc R . .
C19 C 0.09469(17) 0.2939(3) 0.04915(17) 0.0661(11) Uani 1 1 d . . .
H19 H 0.0583 0.2672 0.0376 0.079 Uiso 1 1 calc R . .
C20 C 0.13064(15) 0.2443(3) 0.08798(15) 0.0556(9) Uani 1 1 d . . .
H20 H 0.1177 0.1839 0.1024 0.067 Uiso 1 1 calc R . .
C21 C 0.34916(15) 0.1213(3) 0.22839(16) 0.0537(9) Uani 1 1 d . . .
H21 H 0.3645 0.1137 0.1936 0.064 Uiso 1 1 calc R . .
C22 C 0.38093(16) 0.0855(3) 0.27399(17) 0.0600(10) Uani 1 1 d . . .
H22 H 0.4176 0.0558 0.2702 0.072 Uiso 1 1 calc R . .
C23 C 0.35808(17) 0.0939(3) 0.32489(17) 0.0610(10) Uani 1 1 d . . .
H23 H 0.3781 0.0674 0.3561 0.073 Uiso 1 1 calc R . .
C24 C 0.30495(16) 0.1423(3) 0.32942(15) 0.0550(9) Uani 1 1 d . . .
H24 H 0.2892 0.1503 0.3640 0.066 Uiso 1 1 calc R . .
C25 C 0.27526(14) 0.1789(2) 0.28233(13) 0.0414(7) Uani 1 1 d . . .
C26 C 0.21882(14) 0.2349(2) 0.28321(13) 0.0419(7) Uani 1 1 d . . .
C27 C 0.18946(16) 0.2503(3) 0.33126(15) 0.0540(9) Uani 1 1 d . . .
H27 H 0.2046 0.2254 0.3650 0.065 Uiso 1 1 calc R . .
C28 C 0.13731(18) 0.3032(3) 0.32826(17) 0.0646(11) Uani 1 1 d . . .
H28 H 0.1167 0.3139 0.3601 0.078 Uiso 1 1 calc R . .
C29 C 0.11600(16) 0.3398(3) 0.27855(17) 0.0603(10) Uani 1 1 d . . .
H29 H 0.0811 0.3764 0.2761 0.072 Uiso 1 1 calc R . .
C30 C 0.14682(15) 0.3218(3) 0.23230(16) 0.0524(9) Uani 1 1 d . . .
H30 H 0.1320 0.3465 0.1984 0.063 Uiso 1 1 calc R . .
C31 C 0.35713(16) 0.2153(3) 0.90430(16) 0.0616(10) Uani 1 1 d . . .
H31 H 0.3701 0.1521 0.8938 0.074 Uiso 1 1 calc R . .
C32 C 0.3937(2) 0.2730(4) 0.93873(19) 0.0797(13) Uani 1 1 d . . .
H32 H 0.4307 0.2496 0.9507 0.096 Uiso 1 1 calc R . .
C33 C 0.3746(2) 0.3643(4) 0.9548(2) 0.0944(16) Uani 1 1 d . . .
H33 H 0.3984 0.4043 0.9782 0.113 Uiso 1 1 calc R . .
C34 C 0.3198(2) 0.3974(3) 0.93612(18) 0.0766(12) Uani 1 1 d . . .
H34 H 0.3060 0.4595 0.9473 0.092 Uiso 1 1 calc R . .
C35 C 0.28547(15) 0.3375(3) 0.90064(14) 0.0491(8) Uani 1 1 d . . .
C36 C 0.22717(15) 0.3692(2) 0.87718(14) 0.0476(8) Uani 1 1 d . . .
C37 C 0.20150(19) 0.4603(3) 0.88895(17) 0.0639(10) Uani 1 1 d . . .
H37 H 0.2201 0.5043 0.9141 0.077 Uiso 1 1 calc R . .
C38 C 0.14801(19) 0.4855(3) 0.86309(18) 0.0675(11) Uani 1 1 d . . .
H38 H 0.1304 0.5468 0.8704 0.081 Uiso 1 1 calc R . .
C39 C 0.12126(16) 0.4195(3) 0.82658(16) 0.0571(9) Uani 1 1 d . . .
H39 H 0.0855 0.4354 0.8083 0.069 Uiso 1 1 calc R . .
C40 C 0.14834(15) 0.3292(3) 0.81747(14) 0.0488(8) Uani 1 1 d . . .
H40 H 0.1297 0.2841 0.7931 0.059 Uiso 1 1 calc R . .
C41 C 0.15960(15) 0.1331(3) 0.92820(14) 0.0526(9) Uani 1 1 d . . .
H41 H 0.1437 0.1952 0.9183 0.063 Uiso 1 1 calc R . .
C42 C 0.13458(16) 0.0805(3) 0.96956(15) 0.0628(10) Uani 1 1 d . . .
H42 H 0.1023 0.1061 0.9871 0.075 Uiso 1 1 calc R . .
C43 C 0.15783(17) -0.0102(3) 0.98448(15) 0.0653(11) Uani 1 1 d . . .
H43 H 0.1417 -0.0475 1.0126 0.078 Uiso 1 1 calc R . .
C44 C 0.20564(16) -0.0465(3) 0.95755(14) 0.0574(9) Uani 1 1 d . . .
H44 H 0.2219 -0.1086 0.9672 0.069 Uiso 1 1 calc R . .
C45 C 0.22914(14) 0.0101(2) 0.91623(13) 0.0430(7) Uani 1 1 d . . .
C46 C 0.27990(14) -0.0227(2) 0.88500(13) 0.0430(7) Uani 1 1 d . . .
C47 C 0.31469(17) -0.1045(3) 0.90044(16) 0.0593(10) Uani 1 1 d . . .
H47 H 0.3066 -0.1416 0.9318 0.071 Uiso 1 1 calc R . .
C48 C 0.36111(18) -0.1304(3) 0.86917(18) 0.0664(11) Uani 1 1 d . . .
H48 H 0.3852 -0.1844 0.8795 0.080 Uiso 1 1 calc R . .
C49 C 0.37155(16) -0.0765(3) 0.82283(17) 0.0608(10) Uani 1 1 d . . .
H49 H 0.4020 -0.0942 0.8004 0.073 Uiso 1 1 calc R . .
C50 C 0.33618(15) 0.0046(3) 0.80983(15) 0.0546(9) Uani 1 1 d . . .
H50 H 0.3438 0.0419 0.7784 0.066 Uiso 1 1 calc R . .
C51 C 0.13030(15) 0.0625(3) 0.78593(16) 0.0546(9) Uani 1 1 d . . .
H51 H 0.1223 0.0496 0.8227 0.065 Uiso 1 1 calc R . .
C52 C 0.08990(18) 0.0326(3) 0.74521(19) 0.0710(11) Uani 1 1 d . . .
H52 H 0.0550 0.0015 0.7542 0.085 Uiso 1 1 calc R . .
C53 C 0.1020(2) 0.0496(4) 0.6910(2) 0.0831(13) Uani 1 1 d . . .
H53 H 0.0755 0.0294 0.6625 0.100 Uiso 1 1 calc R . .
C54 C 0.15372(19) 0.0968(3) 0.67903(17) 0.0704(11) Uani 1 1 d . . .
H54 H 0.1626 0.1086 0.6424 0.084 Uiso 1 1 calc R . .
C55 C 0.19234(15) 0.1266(2) 0.72200(14) 0.0465(8) Uani 1 1 d . . .
C56 C 0.24733(15) 0.1827(2) 0.71297(14) 0.0462(8) Uani 1 1 d . . .
C57 C 0.26653(19) 0.2055(3) 0.66096(15) 0.0628(10) Uani 1 1 d . . .
H57 H 0.2444 0.1860 0.6293 0.075 Uiso 1 1 calc R . .
C58 C 0.3186(2) 0.2574(3) 0.65629(18) 0.0699(12) Uani 1 1 d . . .
H58 H 0.3323 0.2724 0.6216 0.084 Uiso 1 1 calc R . .
C59 C 0.34986(18) 0.2863(3) 0.70333(19) 0.0689(11) Uani 1 1 d . . .
H59 H 0.3850 0.3217 0.7012 0.083 Uiso 1 1 calc R . .
C60 C 0.32866(16) 0.2622(3) 0.75378(16) 0.0585(9) Uani 1 1 d . . .
H60 H 0.3500 0.2823 0.7857 0.070 Uiso 1 1 calc R . .
C61 C 0.98375(15) 0.0335(3) -0.08727(14) 0.0519(9) Uani 1 1 d . . .
C62 C 0.98296(13) 0.1441(3) -0.07874(13) 0.0450(8) Uani 1 1 d . . .
C63 C 0.96036(14) 0.1814(3) -0.03065(13) 0.0452(8) Uani 1 1 d . . .
H63 H 0.9487 0.1375 -0.0033 0.054 Uiso 1 1 calc R . .
C64 C 0.95515(14) 0.2843(3) -0.02320(13) 0.0450(8) Uani 1 1 d . . .
C65 C 0.97297(15) 0.3502(3) -0.06383(15) 0.0541(9) Uani 1 1 d . . .
H65 H 0.9699 0.4192 -0.0589 0.065 Uiso 1 1 calc R . .
C66 C 0.99522(17) 0.3120(3) -0.11147(16) 0.0603(10) Uani 1 1 d . . .
H66 H 1.0069 0.3557 -0.1389 0.072 Uiso 1 1 calc R . .
C67 C 1.00041(15) 0.2103(3) -0.11904(15) 0.0549(9) Uani 1 1 d . . .
H67 H 1.0157 0.1858 -0.1514 0.066 Uiso 1 1 calc R . .
H1B H 0.8103(8) 0.281(4) 0.9733(16) 0.095 Uiso 1 1 d D . .
H1A H 0.7502(11) 0.280(4) 0.9790(14) 0.095 Uiso 1 1 d D . .
H2A H 0.964(3) 0.3518(19) 0.2679(19) 0.131 Uiso 1 1 d D . .
H2B H 0.941(2) 0.401(3) 0.2215(12) 0.131 Uiso 1 1 d D . .
H3B H 0.0054(17) 0.422(5) 0.1281(11) 0.130 Uiso 1 1 d D . .
H3A H 0.0071(17) 0.428(5) 0.1852(11) 0.130 Uiso 1 1 d D . .
H4A H 0.486(3) 0.789(3) 0.9661(17) 0.139 Uiso 1 1 d D . .
H4B H 0.464(3) 0.796(4) 1.0185(14) 0.139 Uiso 1 1 d D . .
H5A H 0.991(2) 0.807(4) 0.8036(8) 0.131 Uiso 1 1 d D . .
H5B H 1.0255(12) 0.8066(13) 0.8520(18) 0.131 Uiso 1 1 d D . .
H6B H 0.486(2) 0.345(4) 0.067(2) 0.139 Uiso 1 1 d D . .
H6A H 0.463(3) 0.283(4) 0.1062(8) 0.139 Uiso 1 1 d D . .
H7B H 0.019(3) 0.5709(9) 0.338(2) 0.136 Uiso 1 1 d D . .
H7A H 0.006(3) 0.481(3) 0.3632(17) 0.136 Uiso 1 1 d D . .
H9A H -0.009(2) -0.023(2) 0.452(4) 0.222 Uiso 1 1 d D . .
H9B H 0.008(3) 0.069(3) 0.431(4) 0.222 Uiso 1 1 d 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 0.0358(2) 0.0344(2) 0.0423(2) 0.00091(17) -0.00063(16) 0.00057(16)
Ni2 0.0370(2) 0.0386(2) 0.0385(2) 0.00166(17) 0.00422(16) 0.00027(17)
S1 0.0505(5) 0.0619(6) 0.0516(5) -0.0024(4) 0.0056(4) 0.0019(4)
N1 0.0419(15) 0.0439(16) 0.0446(15) 0.0015(12) 0.0050(12) 0.0009(12)
N2 0.0400(14) 0.0395(15) 0.0472(15) 0.0015(12) 0.0019(12) -0.0033(12)
N3 0.0440(15) 0.0342(14) 0.0463(15) 0.0002(12) -0.0005(12) -0.0022(11)
N4 0.0384(14) 0.0457(16) 0.0431(15) -0.0003(12) -0.0028(12) 0.0048(12)
N5 0.0416(15) 0.0375(14) 0.0511(16) 0.0035(12) -0.0016(12) 0.0012(12)
N6 0.0427(15) 0.0367(14) 0.0467(15) -0.0013(12) -0.0027(12) 0.0039(11)
N7 0.0440(16) 0.0519(17) 0.0469(16) 0.0042(13) -0.0029(13) -0.0028(13)
N8 0.0445(15) 0.0404(15) 0.0421(15) -0.0005(12) 0.0036(12) 0.0021(12)
N9 0.0416(15) 0.0477(16) 0.0378(14) 0.0023(12) 0.0075(12) -0.0014(12)
N10 0.0432(15) 0.0429(15) 0.0459(15) 0.0018(12) 0.0079(12) 0.0043(12)
N11 0.0429(15) 0.0378(14) 0.0457(16) -0.0017(12) 0.0052(12) -0.0027(12)
N12 0.0434(15) 0.0457(16) 0.0471(16) 0.0057(13) 0.0066(12) -0.0013(12)
N13 0.068(2) 0.076(2) 0.063(2) -0.0061(19) 0.0030(18) 0.0169(19)
N14 0.070(3) 0.094(3) 0.139(5) -0.008(3) 0.008(3) -0.002(3)
N15 0.085(3) 0.066(2) 0.075(3) 0.004(2) 0.004(2) 0.005(2)
O1 0.087(2) 0.0569(16) 0.0658(17) 0.0039(13) 0.0286(15) -0.0039(14)
O2 0.0706(17) 0.0729(18) 0.0671(17) -0.0071(14) 0.0305(14) -0.0004(14)
O3 0.118(3) 0.086(2) 0.0671(19) 0.0163(16) 0.0391(18) 0.0182(19)
O4 0.0545(17) 0.105(2) 0.102(2) -0.035(2) -0.0009(16) 0.0118(16)
O5 0.0774(19) 0.080(2) 0.0710(18) -0.0167(15) 0.0008(15) -0.0173(16)
O6 0.266(6) 0.103(3) 0.070(2) -0.012(2) -0.036(3) 0.019(3)
O7 0.096(3) 0.131(3) 0.091(2) -0.003(2) -0.009(2) 0.057(2)
O8 0.103(3) 0.105(3) 0.149(4) -0.037(3) -0.016(2) 0.055(2)
O9 0.114(4) 0.174(5) 0.267(7) -0.075(5) -0.014(4) 0.018(4)
O10 0.110(4) 0.125(4) 0.385(10) 0.044(5) -0.084(5) 0.030(3)
O11 0.261(9) 0.481(16) 0.141(6) -0.056(8) 0.072(6) -0.119(9)
O12 0.101(3) 0.168(4) 0.172(4) -0.071(4) 0.021(3) -0.002(3)
O13 0.087(2) 0.101(3) 0.089(2) -0.0166(19) -0.0047(19) -0.001(2)
O14 0.136(3) 0.096(3) 0.099(3) -0.035(2) -0.005(2) -0.006(2)
O1W 0.081(2) 0.084(2) 0.073(2) -0.0258(16) -0.0059(16) 0.0009(18)
O2W 0.101(3) 0.132(3) 0.095(3) 0.011(2) 0.003(2) 0.041(2)
O3W 0.089(2) 0.158(4) 0.075(2) -0.005(3) -0.0212(18) -0.015(3)
O4W 0.118(3) 0.114(3) 0.116(3) -0.017(2) -0.004(3) -0.007(3)
O5W 0.133(3) 0.072(2) 0.125(3) -0.008(2) 0.023(3) 0.019(2)
O6W 0.131(4) 0.141(4) 0.075(2) -0.003(2) -0.005(2) -0.009(3)
O7W 0.122(3) 0.097(3) 0.121(3) -0.002(2) 0.022(2) 0.020(3)
O8W 0.165(4) 0.166(5) 0.152(4) -0.043(4) 0.004(3) 0.026(4)
O9W 0.147(4) 0.217(7) 0.191(6) 0.018(5) 0.042(4) 0.049(5)
C1 0.054(2) 0.050(2) 0.059(2) 0.0022(17) 0.0113(18) -0.0034(17)
C2 0.056(2) 0.073(3) 0.062(2) 0.001(2) 0.0199(19) 0.002(2)
C3 0.065(2) 0.068(3) 0.063(2) -0.015(2) 0.013(2) 0.010(2)
C4 0.060(2) 0.046(2) 0.057(2) -0.0095(17) 0.0010(18) 0.0040(17)
C5 0.0419(18) 0.0388(17) 0.0420(17) -0.0019(14) -0.0064(14) 0.0032(14)
C6 0.0401(17) 0.0380(17) 0.0449(18) 0.0016(14) -0.0086(14) 0.0019(14)
C7 0.049(2) 0.0367(18) 0.070(2) -0.0016(16) -0.0081(18) 0.0002(15)
C8 0.047(2) 0.044(2) 0.083(3) 0.0120(19) -0.0121(19) -0.0083(16)
C9 0.0413(19) 0.056(2) 0.065(2) 0.0170(19) -0.0030(17) -0.0066(17)
C10 0.0455(19) 0.049(2) 0.054(2) 0.0036(16) 0.0047(16) -0.0042(16)
C11 0.050(2) 0.048(2) 0.060(2) -0.0003(17) -0.0042(17) -0.0060(16)
C12 0.055(2) 0.057(2) 0.073(3) -0.006(2) 0.0042(19) -0.0166(18)
C13 0.075(3) 0.046(2) 0.086(3) 0.008(2) 0.019(2) -0.011(2)
C14 0.070(3) 0.047(2) 0.065(2) 0.0131(18) 0.011(2) 0.0046(19)
C15 0.0473(19) 0.0361(17) 0.0472(19) 0.0024(14) 0.0058(15) 0.0048(14)
C16 0.0488(19) 0.0459(19) 0.0420(18) -0.0001(15) 0.0017(15) 0.0127(15)
C17 0.068(3) 0.063(2) 0.057(2) 0.0102(19) -0.0048(19) 0.017(2)
C18 0.067(3) 0.085(3) 0.066(3) 0.003(2) -0.019(2) 0.029(2)
C19 0.045(2) 0.083(3) 0.068(3) -0.011(2) -0.0164(19) 0.012(2)
C20 0.043(2) 0.066(2) 0.057(2) -0.0041(18) -0.0072(17) 0.0015(17)
C21 0.0433(19) 0.053(2) 0.064(2) 0.0032(18) -0.0014(17) 0.0095(16)
C22 0.045(2) 0.055(2) 0.078(3) 0.007(2) -0.0111(19) 0.0075(17)
C23 0.060(2) 0.054(2) 0.066(3) 0.0138(19) -0.021(2) 0.0021(18)
C24 0.060(2) 0.053(2) 0.051(2) 0.0087(17) -0.0082(17) -0.0017(18)
C25 0.0436(18) 0.0352(17) 0.0447(18) 0.0014(14) -0.0056(14) -0.0061(13)
C26 0.0445(18) 0.0361(17) 0.0445(18) -0.0023(14) -0.0029(14) -0.0035(14)
C27 0.056(2) 0.061(2) 0.044(2) -0.0020(17) 0.0025(16) -0.0043(18)
C28 0.059(2) 0.078(3) 0.058(2) -0.017(2) 0.0156(19) -0.006(2)
C29 0.048(2) 0.060(2) 0.073(3) -0.009(2) 0.0055(19) 0.0108(18)
C30 0.048(2) 0.052(2) 0.057(2) -0.0040(17) -0.0007(17) 0.0089(16)
C31 0.050(2) 0.066(2) 0.067(2) 0.008(2) -0.0090(19) -0.0015(19)
C32 0.063(3) 0.093(4) 0.080(3) 0.013(3) -0.027(2) -0.013(2)
C33 0.097(4) 0.082(3) 0.100(4) -0.005(3) -0.044(3) -0.021(3)
C34 0.087(3) 0.065(3) 0.076(3) -0.012(2) -0.019(2) -0.007(2)
C35 0.053(2) 0.050(2) 0.0443(19) 0.0016(16) 0.0002(16) -0.0062(16)
C36 0.056(2) 0.0432(19) 0.0438(19) 0.0002(15) 0.0061(16) -0.0013(16)
C37 0.077(3) 0.049(2) 0.066(2) -0.0146(19) 0.007(2) 0.001(2)
C38 0.070(3) 0.052(2) 0.082(3) -0.007(2) 0.016(2) 0.016(2)
C39 0.050(2) 0.056(2) 0.067(2) 0.0105(19) 0.0126(18) 0.0115(18)
C40 0.047(2) 0.047(2) 0.052(2) 0.0034(16) 0.0001(16) 0.0030(15)
C41 0.047(2) 0.062(2) 0.049(2) -0.0033(17) 0.0114(16) 0.0038(17)
C42 0.047(2) 0.098(3) 0.044(2) -0.003(2) 0.0144(17) -0.005(2)
C43 0.059(2) 0.091(3) 0.047(2) 0.016(2) 0.0069(18) -0.017(2)
C44 0.056(2) 0.064(2) 0.052(2) 0.0168(18) -0.0005(17) -0.0075(18)
C45 0.0442(18) 0.0448(19) 0.0395(17) 0.0030(14) -0.0015(14) -0.0051(15)
C46 0.0423(18) 0.0408(18) 0.0456(18) 0.0009(15) -0.0018(14) -0.0020(14)
C47 0.066(2) 0.049(2) 0.063(2) 0.0113(18) 0.0007(19) 0.0079(18)
C48 0.063(3) 0.049(2) 0.086(3) -0.002(2) -0.006(2) 0.0149(19)
C49 0.049(2) 0.060(2) 0.074(3) -0.014(2) 0.0072(19) 0.0107(18)
C50 0.050(2) 0.058(2) 0.057(2) 0.0004(17) 0.0137(17) 0.0102(17)
C51 0.050(2) 0.051(2) 0.063(2) -0.0019(17) 0.0047(17) -0.0065(17)
C52 0.059(2) 0.066(3) 0.087(3) -0.007(2) -0.006(2) -0.016(2)
C53 0.083(3) 0.085(3) 0.078(3) -0.008(3) -0.024(3) -0.020(3)
C54 0.082(3) 0.078(3) 0.050(2) -0.004(2) -0.007(2) -0.009(2)
C55 0.0487(19) 0.0437(19) 0.0470(19) -0.0043(15) 0.0018(15) 0.0024(15)
C56 0.051(2) 0.0445(19) 0.0435(19) 0.0041(15) 0.0078(15) 0.0104(15)
C57 0.076(3) 0.067(3) 0.046(2) 0.0027(18) 0.0138(19) 0.011(2)
C58 0.078(3) 0.074(3) 0.061(3) 0.019(2) 0.031(2) 0.013(2)
C59 0.059(2) 0.069(3) 0.081(3) 0.022(2) 0.027(2) -0.001(2)
C60 0.052(2) 0.060(2) 0.064(2) 0.0102(19) 0.0080(18) -0.0080(18)
C61 0.047(2) 0.065(2) 0.0429(19) 0.0005(17) 0.0042(16) 0.0013(17)
C62 0.0339(17) 0.059(2) 0.0422(18) 0.0027(15) 0.0022(14) -0.0041(15)
C63 0.0385(18) 0.059(2) 0.0383(17) 0.0084(15) 0.0014(14) -0.0063(15)
C64 0.0363(17) 0.055(2) 0.0433(18) 0.0053(15) -0.0046(14) -0.0028(15)
C65 0.053(2) 0.055(2) 0.055(2) 0.0076(17) -0.0004(17) -0.0053(17)
C66 0.059(2) 0.068(3) 0.054(2) 0.0196(19) 0.0114(18) -0.0092(19)
C67 0.044(2) 0.077(3) 0.044(2) 0.0051(18) 0.0073(15) -0.0073(18)

_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 N3 2.078(3) . ?
Ni1 N6 2.080(3) . ?
Ni1 N4 2.081(3) . ?
Ni1 N1 2.092(3) . ?
Ni1 N2 2.095(3) . ?
Ni1 N5 2.099(3) . ?
Ni2 N12 2.076(3) . ?
Ni2 N8 2.082(3) . ?
Ni2 N9 2.085(2) . ?
Ni2 N11 2.090(3) . ?
Ni2 N10 2.093(3) . ?
Ni2 N7 2.100(3) . ?
S1 O3 1.425(3) . ?
S1 O4 1.438(3) . ?
S1 O5 1.455(3) . ?
S1 C64 1.774(3) . ?
N1 C1 1.349(4) . ?
N1 C5 1.349(4) . ?
N2 C10 1.337(4) . ?
N2 C6 1.346(4) . ?
N3 C11 1.337(4) . ?
N3 C15 1.343(4) . ?
N4 C20 1.342(4) . ?
N4 C16 1.349(4) . ?
N5 C21 1.340(4) . ?
N5 C25 1.343(4) . ?
N6 C30 1.346(4) . ?
N6 C26 1.347(4) . ?
N7 C31 1.338(4) . ?
N7 C35 1.343(4) . ?
N8 C40 1.332(4) . ?
N8 C36 1.354(4) . ?
N9 C41 1.342(4) . ?
N9 C45 1.347(4) . ?
N10 C50 1.336(4) . ?
N10 C46 1.345(4) . ?
N11 C55 1.342(4) . ?
N11 C51 1.346(4) . ?
N12 C60 1.342(4) . ?
N12 C56 1.343(4) . ?
N13 O8 1.194(4) . ?
N13 O7 1.209(4) . ?
N13 O6 1.224(5) . ?
N14 O10 1.157(6) . ?
N14 O11 1.157(8) . ?
N14 O9 1.170(6) . ?
N15 O12 1.213(5) . ?
N15 O13 1.215(5) . ?
N15 O14 1.244(5) . ?
O1 C61 1.206(4) . ?
O2 C61 1.318(4) . ?
O2 H2C 0.8200 . ?
O1W H1B 0.85(3) . ?
O1W H1A 0.85(3) . ?
O2W H2A 0.87(3) . ?
O2W H2B 0.85(3) . ?
O3W H3B 0.85(3) . ?
O3W H3A 0.85(3) . ?
O4W H4A 0.86(5) . ?
O4W H4B 0.86(4) . ?
O5W H5A 0.853(10) . ?
O5W H5B 0.85(3) . ?
O6W H6B 0.87(5) . ?
O6W H6A 0.856(10) . ?
O7W H7B 0.854(10) . ?
O7W H7A 0.86(5) . ?
O9W H9A 0.86(5) . ?
O9W H9B 0.85(5) . ?
C1 C2 1.361(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.377(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.373(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.386(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.483(4) . ?
C6 C7 1.390(4) . ?
C7 C8 1.374(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.365(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.377(5) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.369(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.360(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.377(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.387(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.482(5) . ?
C16 C17 1.382(5) . ?
C17 C18 1.381(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.363(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.381(5) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C22 1.372(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.362(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.377(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.382(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.484(4) . ?
C26 C27 1.381(5) . ?
C27 C28 1.377(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.362(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.368(5) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 C32 1.379(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.354(7) . ?
C32 H32 0.9300 . ?
C33 C34 1.375(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.383(5) . ?
C34 H34 0.9300 . ?
C35 C36 1.476(5) . ?
C36 C37 1.382(5) . ?
C37 C38 1.379(6) . ?
C37 H37 0.9300 . ?
C38 C39 1.366(5) . ?
C38 H38 0.9300 . ?
C39 C40 1.373(5) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
C41 C42 1.366(5) . ?
C41 H41 0.9300 . ?
C42 C43 1.360(6) . ?
C42 H42 0.9300 . ?
C43 C44 1.380(5) . ?
C43 H43 0.9300 . ?
C44 C45 1.379(5) . ?
C44 H44 0.9300 . ?
C45 C46 1.474(5) . ?
C46 C47 1.387(5) . ?
C47 C48 1.370(5) . ?
C47 H47 0.9300 . ?
C48 C49 1.360(6) . ?
C48 H48 0.9300 . ?
C49 C50 1.374(5) . ?
C49 H49 0.9300 . ?
C50 H50 0.9300 . ?
C51 C52 1.370(5) . ?
C51 H51 0.9300 . ?
C52 C53 1.370(6) . ?
C52 H52 0.9300 . ?
C53 C54 1.375(6) . ?
C53 H53 0.9300 . ?
C54 C55 1.383(5) . ?
C54 H54 0.9300 . ?
C55 C56 1.481(5) . ?
C56 C57 1.383(5) . ?
C57 C58 1.379(6) . ?
C57 H57 0.9300 . ?
C58 C59 1.364(6) . ?
C58 H58 0.9300 . ?
C59 C60 1.369(5) . ?
C59 H59 0.9300 . ?
C60 H60 0.9300 . ?
C61 C62 1.488(5) . ?
C62 C63 1.385(4) . ?
C62 C67 1.386(5) . ?
C63 C64 1.387(5) . ?
C63 H63 0.9300 . ?
C64 C65 1.391(5) . ?
C65 C66 1.376(5) . ?
C65 H65 0.9300 . ?
C66 C67 1.373(5) . ?
C66 H66 0.9300 . ?
C67 H67 0.9300 . ?

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
N3 Ni1 N6 96.56(10) . . ?
N3 Ni1 N4 78.54(10) . . ?
N6 Ni1 N4 96.14(10) . . ?
N3 Ni1 N1 94.01(10) . . ?
N6 Ni1 N1 167.01(10) . . ?
N4 Ni1 N1 93.35(10) . . ?
N3 Ni1 N2 169.93(10) . . ?
N6 Ni1 N2 91.70(10) . . ?
N4 Ni1 N2 94.90(10) . . ?
N1 Ni1 N2 78.63(10) . . ?
N3 Ni1 N5 97.19(10) . . ?
N6 Ni1 N5 78.29(10) . . ?
N4 Ni1 N5 172.65(10) . . ?
N1 Ni1 N5 92.92(10) . . ?
N2 Ni1 N5 90.09(10) . . ?
N12 Ni2 N8 92.37(10) . . ?
N12 Ni2 N9 170.54(11) . . ?
N8 Ni2 N9 94.64(10) . . ?
N12 Ni2 N11 78.55(10) . . ?
N8 Ni2 N11 94.27(10) . . ?
N9 Ni2 N11 94.59(10) . . ?
N12 Ni2 N10 95.28(10) . . ?
N8 Ni2 N10 169.49(10) . . ?
N9 Ni2 N10 78.61(10) . . ?
N11 Ni2 N10 94.30(10) . . ?
N12 Ni2 N7 96.14(11) . . ?
N8 Ni2 N7 78.43(11) . . ?
N9 Ni2 N7 91.48(10) . . ?
N11 Ni2 N7 170.88(11) . . ?
N10 Ni2 N7 93.57(11) . . ?
O3 S1 O4 114.2(2) . . ?
O3 S1 O5 112.5(2) . . ?
O4 S1 O5 110.90(19) . . ?
O3 S1 C64 106.48(17) . . ?
O4 S1 C64 105.93(17) . . ?
O5 S1 C64 106.09(16) . . ?
C1 N1 C5 117.8(3) . . ?
C1 N1 Ni1 126.8(2) . . ?
C5 N1 Ni1 114.8(2) . . ?
C10 N2 C6 118.3(3) . . ?
C10 N2 Ni1 126.9(2) . . ?
C6 N2 Ni1 114.8(2) . . ?
C11 N3 C15 118.6(3) . . ?
C11 N3 Ni1 125.9(2) . . ?
C15 N3 Ni1 115.2(2) . . ?
C20 N4 C16 118.4(3) . . ?
C20 N4 Ni1 126.2(2) . . ?
C16 N4 Ni1 115.4(2) . . ?
C21 N5 C25 118.5(3) . . ?
C21 N5 Ni1 126.8(2) . . ?
C25 N5 Ni1 114.6(2) . . ?
C30 N6 C26 118.0(3) . . ?
C30 N6 Ni1 126.4(2) . . ?
C26 N6 Ni1 114.7(2) . . ?
C31 N7 C35 118.3(3) . . ?
C31 N7 Ni2 127.0(3) . . ?
C35 N7 Ni2 114.8(2) . . ?
C40 N8 C36 118.1(3) . . ?
C40 N8 Ni2 126.6(2) . . ?
C36 N8 Ni2 115.2(2) . . ?
C41 N9 C45 117.9(3) . . ?
C41 N9 Ni2 127.0(2) . . ?
C45 N9 Ni2 115.0(2) . . ?
C50 N10 C46 118.1(3) . . ?
C50 N10 Ni2 126.9(2) . . ?
C46 N10 Ni2 114.3(2) . . ?
C55 N11 C51 118.0(3) . . ?
C55 N11 Ni2 115.0(2) . . ?
C51 N11 Ni2 126.9(2) . . ?
C60 N12 C56 118.4(3) . . ?
C60 N12 Ni2 126.2(2) . . ?
C56 N12 Ni2 115.4(2) . . ?
O8 N13 O7 120.8(4) . . ?
O8 N13 O6 118.9(4) . . ?
O7 N13 O6 120.2(4) . . ?
O10 N14 O11 127.3(9) . . ?
O10 N14 O9 116.1(8) . . ?
O11 N14 O9 116.5(9) . . ?
O12 N15 O13 118.4(4) . . ?
O12 N15 O14 121.0(5) . . ?
O13 N15 O14 120.6(4) . . ?
C61 O2 H2C 109.5 . . ?
H1B O1W H1A 108.5(17) . . ?
H2A O2W H2B 107(4) . . ?
H3B O3W H3A 108.3(17) . . ?
H4A O4W H4B 107(5) . . ?
H5A O5W H5B 107(4) . . ?
H6B O6W H6A 106(5) . . ?
H7B O7W H7A 108(5) . . ?
H9A O9W H9B 109(6) . . ?
N1 C1 C2 123.4(3) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C1 C2 C3 118.8(4) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C4 C3 C2 119.1(3) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 119.6(3) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
N1 C5 C4 121.4(3) . . ?
N1 C5 C6 115.5(3) . . ?
C4 C5 C6 123.1(3) . . ?
N2 C6 C7 121.2(3) . . ?
N2 C6 C5 115.8(3) . . ?
C7 C6 C5 123.0(3) . . ?
C8 C7 C6 119.2(3) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C9 C8 C7 119.8(3) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 118.3(3) . . ?
C8 C9 H9 120.8 . . ?
C10 C9 H9 120.8 . . ?
N2 C10 C9 123.2(3) . . ?
N2 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
N3 C11 C12 122.9(3) . . ?
N3 C11 H11 118.5 . . ?
C12 C11 H11 118.5 . . ?
C13 C12 C11 118.9(4) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C12 C13 C14 119.2(4) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?
C13 C14 C15 119.5(4) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
N3 C15 C14 120.8(3) . . ?
N3 C15 C16 115.7(3) . . ?
C14 C15 C16 123.4(3) . . ?
N4 C16 C17 121.5(3) . . ?
N4 C16 C15 114.8(3) . . ?
C17 C16 C15 123.7(3) . . ?
C18 C17 C16 119.4(4) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C19 C18 C17 119.2(4) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?
C18 C19 C20 119.1(4) . . ?
C18 C19 H19 120.4 . . ?
C20 C19 H19 120.4 . . ?
N4 C20 C19 122.5(4) . . ?
N4 C20 H20 118.8 . . ?
C19 C20 H20 118.8 . . ?
N5 C21 C22 122.6(4) . . ?
N5 C21 H21 118.7 . . ?
C22 C21 H21 118.7 . . ?
C23 C22 C21 119.1(3) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
C22 C23 C24 119.0(3) . . ?
C22 C23 H23 120.5 . . ?
C24 C23 H23 120.5 . . ?
C23 C24 C25 119.6(4) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
N5 C25 C24 121.2(3) . . ?
N5 C25 C26 115.3(3) . . ?
C24 C25 C26 123.5(3) . . ?
N6 C26 C27 121.8(3) . . ?
N6 C26 C25 115.5(3) . . ?
C27 C26 C25 122.7(3) . . ?
C28 C27 C26 118.8(3) . . ?
C28 C27 H27 120.6 . . ?
C26 C27 H27 120.6 . . ?
C29 C28 C27 119.8(4) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C30 118.9(3) . . ?
C28 C29 H29 120.6 . . ?
C30 C29 H29 120.6 . . ?
N6 C30 C29 122.8(3) . . ?
N6 C30 H30 118.6 . . ?
C29 C30 H30 118.6 . . ?
N7 C31 C32 122.8(4) . . ?
N7 C31 H31 118.6 . . ?
C32 C31 H31 118.6 . . ?
C33 C32 C31 118.7(4) . . ?
C33 C32 H32 120.6 . . ?
C31 C32 H32 120.6 . . ?
C32 C33 C34 119.5(4) . . ?
C32 C33 H33 120.3 . . ?
C34 C33 H33 120.3 . . ?
C33 C34 C35 119.4(4) . . ?
C33 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
N7 C35 C34 121.3(3) . . ?
N7 C35 C36 116.0(3) . . ?
C34 C35 C36 122.7(3) . . ?
N8 C36 C37 121.2(3) . . ?
N8 C36 C35 115.3(3) . . ?
C37 C36 C35 123.5(3) . . ?
C38 C37 C36 119.4(4) . . ?
C38 C37 H37 120.3 . . ?
C36 C37 H37 120.3 . . ?
C39 C38 C37 119.3(4) . . ?
C39 C38 H38 120.4 . . ?
C37 C38 H38 120.4 . . ?
C38 C39 C40 118.6(4) . . ?
C38 C39 H39 120.7 . . ?
C40 C39 H39 120.7 . . ?
N8 C40 C39 123.4(3) . . ?
N8 C40 H40 118.3 . . ?
C39 C40 H40 118.3 . . ?
N9 C41 C42 123.3(4) . . ?
N9 C41 H41 118.3 . . ?
C42 C41 H41 118.3 . . ?
C43 C42 C41 118.7(4) . . ?
C43 C42 H42 120.7 . . ?
C41 C42 H42 120.7 . . ?
C42 C43 C44 119.4(3) . . ?
C42 C43 H43 120.3 . . ?
C44 C43 H43 120.3 . . ?
C45 C44 C43 119.4(4) . . ?
C45 C44 H44 120.3 . . ?
C43 C44 H44 120.3 . . ?
N9 C45 C44 121.3(3) . . ?
N9 C45 C46 115.4(3) . . ?
C44 C45 C46 123.3(3) . . ?
N10 C46 C47 121.1(3) . . ?
N10 C46 C45 115.9(3) . . ?
C47 C46 C45 123.0(3) . . ?
C48 C47 C46 119.6(4) . . ?
C48 C47 H47 120.2 . . ?
C46 C47 H47 120.2 . . ?
C49 C48 C47 119.3(4) . . ?
C49 C48 H48 120.3 . . ?
C47 C48 H48 120.3 . . ?
C48 C49 C50 118.7(4) . . ?
C48 C49 H49 120.7 . . ?
C50 C49 H49 120.7 . . ?
N10 C50 C49 123.2(3) . . ?
N10 C50 H50 118.4 . . ?
C49 C50 H50 118.4 . . ?
N11 C51 C52 123.1(4) . . ?
N11 C51 H51 118.5 . . ?
C52 C51 H51 118.5 . . ?
C53 C52 C51 118.6(4) . . ?
C53 C52 H52 120.7 . . ?
C51 C52 H52 120.7 . . ?
C52 C53 C54 119.3(4) . . ?
C52 C53 H53 120.3 . . ?
C54 C53 H53 120.3 . . ?
C53 C54 C55 119.4(4) . . ?
C53 C54 H54 120.3 . . ?
C55 C54 H54 120.3 . . ?
N11 C55 C54 121.6(3) . . ?
N11 C55 C56 115.5(3) . . ?
C54 C55 C56 122.9(3) . . ?
N12 C56 C57 121.1(3) . . ?
N12 C56 C55 115.5(3) . . ?
C57 C56 C55 123.4(3) . . ?
C58 C57 C56 119.6(4) . . ?
C58 C57 H57 120.2 . . ?
C56 C57 H57 120.2 . . ?
C59 C58 C57 119.1(4) . . ?
C59 C58 H58 120.5 . . ?
C57 C58 H58 120.5 . . ?
C58 C59 C60 118.9(4) . . ?
C58 C59 H59 120.6 . . ?
C60 C59 H59 120.6 . . ?
N12 C60 C59 122.9(4) . . ?
N12 C60 H60 118.5 . . ?
C59 C60 H60 118.5 . . ?
O1 C61 O2 123.4(4) . . ?
O1 C61 C62 123.4(3) . . ?
O2 C61 C62 113.1(3) . . ?
C63 C62 C67 119.3(3) . . ?
C63 C62 C61 118.7(3) . . ?
C67 C62 C61 121.9(3) . . ?
C62 C63 C64 120.1(3) . . ?
C62 C63 H63 120.0 . . ?
C64 C63 H63 120.0 . . ?
C63 C64 C65 120.1(3) . . ?
C63 C64 S1 120.7(2) . . ?
C65 C64 S1 119.1(3) . . ?
C66 C65 C64 119.2(3) . . ?
C66 C65 H65 120.4 . . ?
C64 C65 H65 120.4 . . ?
C67 C66 C65 120.9(3) . . ?
C67 C66 H66 119.6 . . ?
C65 C66 H66 119.6 . . ?
C66 C67 C62 120.4(3) . . ?
C66 C67 H67 119.8 . . ?
C62 C67 H67 119.8 . . ?

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 Ni1 N1 C1 10.7(3) . . . . ?
N6 Ni1 N1 C1 -133.7(4) . . . . ?
N4 Ni1 N1 C1 89.4(3) . . . . ?
N2 Ni1 N1 C1 -176.2(3) . . . . ?
N5 Ni1 N1 C1 -86.7(3) . . . . ?
N3 Ni1 N1 C5 -178.9(2) . . . . ?
N6 Ni1 N1 C5 36.7(6) . . . . ?
N4 Ni1 N1 C5 -100.2(2) . . . . ?
N2 Ni1 N1 C5 -5.9(2) . . . . ?
N5 Ni1 N1 C5 83.6(2) . . . . ?
N3 Ni1 N2 C10 -132.9(5) . . . . ?
N6 Ni1 N2 C10 12.3(3) . . . . ?
N4 Ni1 N2 C10 -84.0(3) . . . . ?
N1 Ni1 N2 C10 -176.5(3) . . . . ?
N5 Ni1 N2 C10 90.6(3) . . . . ?
N3 Ni1 N2 C6 46.2(7) . . . . ?
N6 Ni1 N2 C6 -168.6(2) . . . . ?
N4 Ni1 N2 C6 95.1(2) . . . . ?
N1 Ni1 N2 C6 2.7(2) . . . . ?
N5 Ni1 N2 C6 -90.3(2) . . . . ?
N6 Ni1 N3 C11 87.9(3) . . . . ?
N4 Ni1 N3 C11 -177.2(3) . . . . ?
N1 Ni1 N3 C11 -84.6(3) . . . . ?
N2 Ni1 N3 C11 -127.2(6) . . . . ?
N5 Ni1 N3 C11 8.9(3) . . . . ?
N6 Ni1 N3 C15 -99.5(2) . . . . ?
N4 Ni1 N3 C15 -4.5(2) . . . . ?
N1 Ni1 N3 C15 88.1(2) . . . . ?
N2 Ni1 N3 C15 45.5(7) . . . . ?
N5 Ni1 N3 C15 -178.5(2) . . . . ?
N3 Ni1 N4 C20 -175.9(3) . . . . ?
N6 Ni1 N4 C20 -80.5(3) . . . . ?
N1 Ni1 N4 C20 90.7(3) . . . . ?
N2 Ni1 N4 C20 11.8(3) . . . . ?
N3 Ni1 N4 C16 1.8(2) . . . . ?
N6 Ni1 N4 C16 97.3(2) . . . . ?
N1 Ni1 N4 C16 -91.6(2) . . . . ?
N2 Ni1 N4 C16 -170.4(2) . . . . ?
N3 Ni1 N5 C21 -79.3(3) . . . . ?
N6 Ni1 N5 C21 -174.5(3) . . . . ?
N1 Ni1 N5 C21 15.1(3) . . . . ?
N2 Ni1 N5 C21 93.7(3) . . . . ?
N3 Ni1 N5 C25 105.0(2) . . . . ?
N6 Ni1 N5 C25 9.8(2) . . . . ?
N1 Ni1 N5 C25 -160.5(2) . . . . ?
N2 Ni1 N5 C25 -81.9(2) . . . . ?
N3 Ni1 N6 C30 84.2(3) . . . . ?
N4 Ni1 N6 C30 5.1(3) . . . . ?
N1 Ni1 N6 C30 -131.5(4) . . . . ?
N2 Ni1 N6 C30 -90.0(3) . . . . ?
N5 Ni1 N6 C30 -179.7(3) . . . . ?
N3 Ni1 N6 C26 -107.2(2) . . . . ?
N4 Ni1 N6 C26 173.7(2) . . . . ?
N1 Ni1 N6 C26 37.1(6) . . . . ?
N2 Ni1 N6 C26 78.6(2) . . . . ?
N5 Ni1 N6 C26 -11.2(2) . . . . ?
N12 Ni2 N7 C31 -85.8(3) . . . . ?
N8 Ni2 N7 C31 -177.0(3) . . . . ?
N9 Ni2 N7 C31 88.6(3) . . . . ?
N10 Ni2 N7 C31 9.9(3) . . . . ?
N12 Ni2 N7 C35 94.7(2) . . . . ?
N8 Ni2 N7 C35 3.5(2) . . . . ?
N9 Ni2 N7 C35 -90.9(2) . . . . ?
N10 Ni2 N7 C35 -169.6(2) . . . . ?
N12 Ni2 N8 C40 81.8(3) . . . . ?
N9 Ni2 N8 C40 -91.8(3) . . . . ?
N11 Ni2 N8 C40 3.1(3) . . . . ?
N10 Ni2 N8 C40 -141.4(5) . . . . ?
N7 Ni2 N8 C40 177.6(3) . . . . ?
N12 Ni2 N8 C36 -100.2(2) . . . . ?
N9 Ni2 N8 C36 86.2(2) . . . . ?
N11 Ni2 N8 C36 -178.9(2) . . . . ?
N10 Ni2 N8 C36 36.6(7) . . . . ?
N7 Ni2 N8 C36 -4.4(2) . . . . ?
N8 Ni2 N9 C41 13.7(3) . . . . ?
N11 Ni2 N9 C41 -80.9(3) . . . . ?
N10 Ni2 N9 C41 -174.4(3) . . . . ?
N7 Ni2 N9 C41 92.3(3) . . . . ?
N8 Ni2 N9 C45 -171.1(2) . . . . ?
N11 Ni2 N9 C45 94.2(2) . . . . ?
N10 Ni2 N9 C45 0.8(2) . . . . ?
N7 Ni2 N9 C45 -92.6(2) . . . . ?
N12 Ni2 N10 C50 10.9(3) . . . . ?
N8 Ni2 N10 C50 -125.7(5) . . . . ?
N9 Ni2 N10 C50 -176.4(3) . . . . ?
N11 Ni2 N10 C50 89.8(3) . . . . ?
N7 Ni2 N10 C50 -85.6(3) . . . . ?
N12 Ni2 N10 C46 -178.8(2) . . . . ?
N8 Ni2 N10 C46 44.6(7) . . . . ?
N9 Ni2 N10 C46 -6.1(2) . . . . ?
N11 Ni2 N10 C46 -99.9(2) . . . . ?
N7 Ni2 N10 C46 84.7(2) . . . . ?
N12 Ni2 N11 C55 0.3(2) . . . . ?
N8 Ni2 N11 C55 91.9(2) . . . . ?
N9 Ni2 N11 C55 -173.1(2) . . . . ?
N10 Ni2 N11 C55 -94.2(2) . . . . ?
N12 Ni2 N11 C51 -176.4(3) . . . . ?
N8 Ni2 N11 C51 -84.8(3) . . . . ?
N9 Ni2 N11 C51 10.2(3) . . . . ?
N10 Ni2 N11 C51 89.1(3) . . . . ?
N8 Ni2 N12 C60 86.5(3) . . . . ?
N11 Ni2 N12 C60 -179.6(3) . . . . ?
N10 Ni2 N12 C60 -86.3(3) . . . . ?
N7 Ni2 N12 C60 7.9(3) . . . . ?
N8 Ni2 N12 C56 -94.8(2) . . . . ?
N11 Ni2 N12 C56 -0.9(2) . . . . ?
N10 Ni2 N12 C56 92.4(2) . . . . ?
N7 Ni2 N12 C56 -173.4(2) . . . . ?
C5 N1 C1 C2 0.0(5) . . . . ?
Ni1 N1 C1 C2 170.1(3) . . . . ?
N1 C1 C2 C3 -0.1(6) . . . . ?
C1 C2 C3 C4 0.8(6) . . . . ?
C2 C3 C4 C5 -1.5(6) . . . . ?
C1 N1 C5 C4 -0.6(5) . . . . ?
Ni1 N1 C5 C4 -171.9(2) . . . . ?
C1 N1 C5 C6 179.2(3) . . . . ?
Ni1 N1 C5 C6 7.9(3) . . . . ?
C3 C4 C5 N1 1.4(5) . . . . ?
C3 C4 C5 C6 -178.5(3) . . . . ?
C10 N2 C6 C7 -0.7(5) . . . . ?
Ni1 N2 C6 C7 -179.9(2) . . . . ?
C10 N2 C6 C5 179.8(3) . . . . ?
Ni1 N2 C6 C5 0.6(3) . . . . ?
N1 C5 C6 N2 -5.7(4) . . . . ?
C4 C5 C6 N2 174.1(3) . . . . ?
N1 C5 C6 C7 174.8(3) . . . . ?
C4 C5 C6 C7 -5.4(5) . . . . ?
N2 C6 C7 C8 0.6(5) . . . . ?
C5 C6 C7 C8 -180.0(3) . . . . ?
C6 C7 C8 C9 -0.1(5) . . . . ?
C7 C8 C9 C10 -0.4(5) . . . . ?
C6 N2 C10 C9 0.2(5) . . . . ?
Ni1 N2 C10 C9 179.3(2) . . . . ?
C8 C9 C10 N2 0.3(5) . . . . ?
C15 N3 C11 C12 0.4(5) . . . . ?
Ni1 N3 C11 C12 172.8(3) . . . . ?
N3 C11 C12 C13 -0.8(6) . . . . ?
C11 C12 C13 C14 0.7(6) . . . . ?
C12 C13 C14 C15 -0.1(6) . . . . ?
C11 N3 C15 C14 0.2(5) . . . . ?
Ni1 N3 C15 C14 -173.0(3) . . . . ?
C11 N3 C15 C16 179.6(3) . . . . ?
Ni1 N3 C15 C16 6.4(3) . . . . ?
C13 C14 C15 N3 -0.4(5) . . . . ?
C13 C14 C15 C16 -179.6(3) . . . . ?
C20 N4 C16 C17 -0.3(5) . . . . ?
Ni1 N4 C16 C17 -178.2(3) . . . . ?
C20 N4 C16 C15 178.8(3) . . . . ?
Ni1 N4 C16 C15 0.9(3) . . . . ?
N3 C15 C16 N4 -4.8(4) . . . . ?
C14 C15 C16 N4 174.5(3) . . . . ?
N3 C15 C16 C17 174.2(3) . . . . ?
C14 C15 C16 C17 -6.4(5) . . . . ?
N4 C16 C17 C18 0.7(5) . . . . ?
C15 C16 C17 C18 -178.3(3) . . . . ?
C16 C17 C18 C19 -0.8(6) . . . . ?
C17 C18 C19 C20 0.6(6) . . . . ?
C16 N4 C20 C19 0.0(5) . . . . ?
Ni1 N4 C20 C19 177.8(3) . . . . ?
C18 C19 C20 N4 -0.2(6) . . . . ?
C25 N5 C21 C22 0.8(5) . . . . ?
Ni1 N5 C21 C22 -174.7(3) . . . . ?
N5 C21 C22 C23 1.8(6) . . . . ?
C21 C22 C23 C24 -2.9(6) . . . . ?
C22 C23 C24 C25 1.6(5) . . . . ?
C21 N5 C25 C24 -2.1(5) . . . . ?
Ni1 N5 C25 C24 173.9(2) . . . . ?
C21 N5 C25 C26 176.9(3) . . . . ?
Ni1 N5 C25 C26 -7.1(3) . . . . ?
C23 C24 C25 N5 0.9(5) . . . . ?
C23 C24 C25 C26 -178.0(3) . . . . ?
C30 N6 C26 C27 0.7(5) . . . . ?
Ni1 N6 C26 C27 -168.9(3) . . . . ?
C30 N6 C26 C25 -179.5(3) . . . . ?
Ni1 N6 C26 C25 10.9(3) . . . . ?
N5 C25 C26 N6 -2.5(4) . . . . ?
C24 C25 C26 N6 176.5(3) . . . . ?
N5 C25 C26 C27 177.4(3) . . . . ?
C24 C25 C26 C27 -3.7(5) . . . . ?
N6 C26 C27 C28 -0.2(5) . . . . ?
C25 C26 C27 C28 180.0(3) . . . . ?
C26 C27 C28 C29 -0.5(6) . . . . ?
C27 C28 C29 C30 0.9(6) . . . . ?
C26 N6 C30 C29 -0.3(5) . . . . ?
Ni1 N6 C30 C29 167.9(3) . . . . ?
C28 C29 C30 N6 -0.4(6) . . . . ?
C35 N7 C31 C32 -0.1(6) . . . . ?
Ni2 N7 C31 C32 -179.6(3) . . . . ?
N7 C31 C32 C33 1.1(7) . . . . ?
C31 C32 C33 C34 -0.5(8) . . . . ?
C32 C33 C34 C35 -1.0(8) . . . . ?
C31 N7 C35 C34 -1.4(5) . . . . ?
Ni2 N7 C35 C34 178.1(3) . . . . ?
C31 N7 C35 C36 178.3(3) . . . . ?
Ni2 N7 C35 C36 -2.2(4) . . . . ?
C33 C34 C35 N7 2.0(6) . . . . ?
C33 C34 C35 C36 -177.7(4) . . . . ?
C40 N8 C36 C37 1.7(5) . . . . ?
Ni2 N8 C36 C37 -176.5(3) . . . . ?
C40 N8 C36 C35 -177.2(3) . . . . ?
Ni2 N8 C36 C35 4.6(4) . . . . ?
N7 C35 C36 N8 -1.6(4) . . . . ?
C34 C35 C36 N8 178.1(3) . . . . ?
N7 C35 C36 C37 179.5(3) . . . . ?
C34 C35 C36 C37 -0.8(6) . . . . ?
N8 C36 C37 C38 -1.8(6) . . . . ?
C35 C36 C37 C38 177.0(4) . . . . ?
C36 C37 C38 C39 0.4(6) . . . . ?
C37 C38 C39 C40 0.9(6) . . . . ?
C36 N8 C40 C39 -0.3(5) . . . . ?
Ni2 N8 C40 C39 177.7(3) . . . . ?
C38 C39 C40 N8 -1.1(5) . . . . ?
C45 N9 C41 C42 -0.6(5) . . . . ?
Ni2 N9 C41 C42 174.4(3) . . . . ?
N9 C41 C42 C43 0.3(6) . . . . ?
C41 C42 C43 C44 -0.1(6) . . . . ?
C42 C43 C44 C45 0.3(6) . . . . ?
C41 N9 C45 C44 0.8(5) . . . . ?
Ni2 N9 C45 C44 -174.8(3) . . . . ?
C41 N9 C45 C46 179.9(3) . . . . ?
Ni2 N9 C45 C46 4.2(3) . . . . ?
C43 C44 C45 N9 -0.7(5) . . . . ?
C43 C44 C45 C46 -179.7(3) . . . . ?
C50 N10 C46 C47 2.1(5) . . . . ?
Ni2 N10 C46 C47 -169.2(3) . . . . ?
C50 N10 C46 C45 -178.6(3) . . . . ?
Ni2 N10 C46 C45 10.2(3) . . . . ?
N9 C45 C46 N10 -9.7(4) . . . . ?
C44 C45 C46 N10 169.3(3) . . . . ?
N9 C45 C46 C47 169.6(3) . . . . ?
C44 C45 C46 C47 -11.3(5) . . . . ?
N10 C46 C47 C48 -0.8(5) . . . . ?
C45 C46 C47 C48 179.9(3) . . . . ?
C46 C47 C48 C49 -1.3(6) . . . . ?
C47 C48 C49 C50 2.1(6) . . . . ?
C46 N10 C50 C49 -1.2(5) . . . . ?
Ni2 N10 C50 C49 168.8(3) . . . . ?
C48 C49 C50 N10 -0.9(6) . . . . ?
C55 N11 C51 C52 -0.8(5) . . . . ?
Ni2 N11 C51 C52 175.8(3) . . . . ?
N11 C51 C52 C53 1.3(6) . . . . ?
C51 C52 C53 C54 -0.8(7) . . . . ?
C52 C53 C54 C55 -0.3(7) . . . . ?
C51 N11 C55 C54 -0.3(5) . . . . ?
Ni2 N11 C55 C54 -177.3(3) . . . . ?
C51 N11 C55 C56 177.3(3) . . . . ?
Ni2 N11 C55 C56 0.3(4) . . . . ?
C53 C54 C55 N11 0.8(6) . . . . ?
C53 C54 C55 C56 -176.6(4) . . . . ?
C60 N12 C56 C57 0.2(5) . . . . ?
Ni2 N12 C56 C57 -178.6(3) . . . . ?
C60 N12 C56 C55 -179.9(3) . . . . ?
Ni2 N12 C56 C55 1.4(4) . . . . ?
N11 C55 C56 N12 -1.1(4) . . . . ?
C54 C55 C56 N12 176.5(3) . . . . ?
N11 C55 C56 C57 178.8(3) . . . . ?
C54 C55 C56 C57 -3.6(5) . . . . ?
N12 C56 C57 C58 0.5(5) . . . . ?
C55 C56 C57 C58 -179.4(3) . . . . ?
C56 C57 C58 C59 -0.8(6) . . . . ?
C57 C58 C59 C60 0.5(6) . . . . ?
C56 N12 C60 C59 -0.6(5) . . . . ?
Ni2 N12 C60 C59 178.0(3) . . . . ?
C58 C59 C60 N12 0.3(6) . . . . ?
O1 C61 C62 C63 14.2(5) . . . . ?
O2 C61 C62 C63 -168.6(3) . . . . ?
O1 C61 C62 C67 -161.4(3) . . . . ?
O2 C61 C62 C67 15.8(5) . . . . ?
C67 C62 C63 C64 0.2(5) . . . . ?
C61 C62 C63 C64 -175.5(3) . . . . ?
C62 C63 C64 C65 -0.4(5) . . . . ?
C62 C63 C64 S1 178.3(2) . . . . ?
O3 S1 C64 C63 19.9(3) . . . . ?
O4 S1 C64 C63 -102.1(3) . . . . ?
O5 S1 C64 C63 140.0(3) . . . . ?
O3 S1 C64 C65 -161.4(3) . . . . ?
O4 S1 C64 C65 76.6(3) . . . . ?
O5 S1 C64 C65 -41.3(3) . . . . ?
C63 C64 C65 C66 0.6(5) . . . . ?
S1 C64 C65 C66 -178.2(3) . . . . ?
C64 C65 C66 C67 -0.5(6) . . . . ?
C65 C66 C67 C62 0.3(6) . . . . ?
C63 C62 C67 C66 -0.2(5) . . . . ?
C61 C62 C67 C66 175.4(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
O2 H2C O5W 0.82 1.82 2.587(5) 156.1 1_544
O1W H1B O4 0.85(3) 1.97(2) 2.772(4) 156(4) 1_556
O1W H1A O13 0.85(3) 2.05(4) 2.878(5) 163(4) 3_667
O1W H1A O14 0.85(3) 2.44(3) 3.130(5) 139(3) 3_667
O1W H1A N15 0.85(3) 2.58(3) 3.407(5) 164(4) 3_667
O2W H2A O10 0.87(3) 1.881(18) 2.733(7) 166(5) 1_655
O3W H3B O5 0.85(3) 2.05(3) 2.880(4) 171(5) 1_455
O3W H3A O2W 0.85(3) 2.01(3) 2.856(6) 173(6) 1_455
O4W H4A O6W 0.86(5) 1.96(5) 2.792(7) 162(7) 3_666
O4W H4B O14 0.86(4) 2.57(6) 3.004(6) 112(5) .
O5W H5A O10 0.853(10) 2.34(3) 3.134(10) 155(5) 3_666
O5W H5A O9 0.853(10) 2.46(4) 3.137(9) 137(5) 3_666
O5W H5B O3 0.85(3) 2.11(3) 2.865(6) 146(5) 3_766
O6W H6B O9W 0.87(5) 2.26(5) 2.907(8) 133(6) 2
O6W H6A O6 0.856(10) 1.89(2) 2.728(6) 164(6) .
O7W H7B O6 0.854(10) 1.921(15) 2.754(6) 165(5) 2
O7W H7A O8W 0.86(5) 2.07(5) 2.892(6) 160(5) 2_545
O9W H9A O9W 0.86(5) 2.57(8) 2.966(15) 109(7) 3_556

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.057
#===END