# 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        'Liya Wang'
_publ_contact_author_email       WLYA@LYNU.EDU.CN

_publ_section_title              
;
Dicarboxylate anion-dependent assembly of Ni(II)
coordination polymers with 4,4'-dipyridyl sulfide
;
loop_
_publ_author_name
'Liya Wang.'
'Stuart Batten'
'Jiang-Liang Hu.'
'Lu-Fang Ma.'
'Jian-ge Wang.'
;
Yao-Yu Wang
;

data_a
_database_code_depnum_ccdc_archive 'CCDC 701845'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H38 N4 Ni2 O15 S2'
_chemical_formula_weight         948.24

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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.2688(10)
_cell_length_b                   11.1859(10)
_cell_length_c                   18.4444(17)
_cell_angle_alpha                80.2550(10)
_cell_angle_beta                 83.1220(10)
_cell_angle_gamma                89.7290(10)
_cell_volume                     2072.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    6504
_cell_measurement_theta_min      0.00
_cell_measurement_theta_max      0.00

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             980
_exptl_absorpt_coefficient_mu    1.081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6199
_exptl_absorpt_correction_T_max  0.8417
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      291(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15524
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         25.50
_reflns_number_total             7684
_reflns_number_gt                6395
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0499P)²+1.8609P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7684
_refine_ls_number_parameters     532
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0371
_refine_ls_wR_factor_ref         0.1036
_refine_ls_wR_factor_gt          0.0969
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.49722(3) 0.44443(3) 0.286042(18) 0.02795(10) Uani 1 1 d . . .
Ni2 Ni 0.52187(3) 0.94796(3) -0.162951(17) 0.02786(10) Uani 1 1 d . . .
S1 S 0.00603(8) 1.29304(8) -0.10288(7) 0.0610(3) Uani 1 1 d . . .
S2 S -0.04082(8) 0.67910(9) 0.44066(5) 0.0550(2) Uani 1 1 d . . .
O6 O 0.67788(19) 0.84737(18) -0.20536(11) 0.0400(5) Uani 1 1 d . . .
H11W H 0.6573 0.7745 -0.2037 0.060 Uiso 1 1 d R . .
H12W H 0.6905 0.8823 -0.2495 0.060 Uiso 1 1 d R . .
O7 O 0.66056(19) 0.34960(18) 0.24669(10) 0.0365(4) Uani 1 1 d . . .
H13W H 0.6434 0.3048 0.2163 0.055 Uiso 1 1 d R . .
H14W H 0.6735 0.3039 0.2860 0.055 Uiso 1 1 d R . .
O8 O 0.45179(19) 0.30803(18) 0.37062(11) 0.0407(5) Uani 1 1 d . . .
O9 O 0.6500(2) 0.2351(2) 0.38887(11) 0.0443(5) Uani 1 1 d . . .
O10 O 0.6766(2) 0.0056(2) 0.65979(11) 0.0536(6) Uani 1 1 d . . .
O11 O 0.4927(2) 0.0216(2) 0.73416(10) 0.0457(5) Uani 1 1 d . . .
O12 O 0.50060(19) 0.56087(17) 0.18272(10) 0.0358(4) Uani 1 1 d . . .
O13 O 0.38400(19) 0.39182(16) 0.20646(10) 0.0334(4) Uani 1 1 d . . .
O14 O 0.50921(19) 0.83220(17) -0.05950(10) 0.0363(5) Uani 1 1 d . . .
O15 O 0.39426(18) 0.78927(16) -0.14474(9) 0.0322(4) Uani 1 1 d . . .
N1 N -0.3729(2) 0.5350(2) 0.33535(12) 0.0324(5) Uani 1 1 d . . .
N2 N 0.3306(2) 0.5281(2) 0.33069(12) 0.0321(5) Uani 1 1 d . . .
N3 N -0.3401(2) 1.0671(2) -0.14134(12) 0.0321(5) Uani 1 1 d . . .
N4 N 0.3575(2) 1.0476(2) -0.13233(12) 0.0306(5) Uani 1 1 d . . .
C1 C 0.5301(3) 0.2423(2) 0.40822(15) 0.0325(6) Uani 1 1 d . . .
C2 C 0.4681(3) 0.1738(2) 0.48115(14) 0.0295(6) Uani 1 1 d . . .
C3 C 0.3327(3) 0.1555(3) 0.49274(15) 0.0352(6) Uani 1 1 d . . .
H3 H 0.2823 0.1840 0.4549 0.042 Uiso 1 1 calc R . .
C4 C 0.2727(3) 0.0955(3) 0.55968(16) 0.0398(7) Uani 1 1 d . . .
H4 H 0.1828 0.0800 0.5663 0.048 Uiso 1 1 calc R . .
C5 C 0.3468(3) 0.0583(3) 0.61724(15) 0.0373(6) Uani 1 1 d . . .
H5 H 0.3056 0.0219 0.6633 0.045 Uiso 1 1 calc R . .
C6 C 0.4818(3) 0.0749(2) 0.60685(14) 0.0308(6) Uani 1 1 d . . .
C7 C 0.5428(3) 0.1301(2) 0.53785(14) 0.0294(6) Uani 1 1 d . . .
H7A H 0.6337 0.1378 0.5296 0.035 Uiso 1 1 calc R . .
C8 C 0.5588(3) 0.0303(2) 0.67101(15) 0.0345(6) Uani 1 1 d . . .
C9 C 0.3284(3) 0.6354(3) 0.35319(16) 0.0364(6) Uani 1 1 d . . .
H9 H 0.4066 0.6795 0.3473 0.044 Uiso 1 1 calc R . .
C10 C 0.2165(3) 0.6845(3) 0.38464(18) 0.0409(7) Uani 1 1 d . . .
H10 H 0.2195 0.7603 0.3989 0.049 Uiso 1 1 calc R . .
C11 C 0.0992(3) 0.6190(3) 0.39477(17) 0.0386(7) Uani 1 1 d . . .
C12 C 0.1004(3) 0.5069(3) 0.37243(17) 0.0416(7) Uani 1 1 d . . .
H12 H 0.0239 0.4603 0.3787 0.050 Uiso 1 1 calc R . .
C13 C 0.2161(3) 0.4656(3) 0.34089(17) 0.0387(7) Uani 1 1 d . . .
H13 H 0.2154 0.3904 0.3258 0.046 Uiso 1 1 calc R . .
C14 C -0.2698(3) 0.5934(3) 0.29314(17) 0.0438(7) Uani 1 1 d . . .
H14 H -0.2677 0.6042 0.2419 0.053 Uiso 1 1 calc R . .
C15 C -0.1668(3) 0.6382(3) 0.32231(19) 0.0492(8) Uani 1 1 d . . .
H15 H -0.0968 0.6784 0.2912 0.059 Uiso 1 1 calc R . .
C16 C -0.1684(3) 0.6230(3) 0.39807(17) 0.0389(7) Uani 1 1 d . . .
C17 C -0.2762(3) 0.5657(3) 0.44210(16) 0.0415(7) Uani 1 1 d . . .
H17 H -0.2818 0.5560 0.4935 0.050 Uiso 1 1 calc R . .
C18 C -0.3750(3) 0.5235(3) 0.40861(16) 0.0390(7) Uani 1 1 d . . .
H18 H -0.4471 0.4849 0.4386 0.047 Uiso 1 1 calc R . .
C19 C 0.4216(3) 0.4896(2) 0.16336(14) 0.0281(6) Uani 1 1 d . . .
C20 C 0.3675(3) 0.5225(2) 0.09089(14) 0.0269(5) Uani 1 1 d . . .
C21 C 0.2616(3) 0.4591(3) 0.07496(16) 0.0353(6) Uani 1 1 d . . .
H21 H 0.2257 0.3928 0.1087 0.042 Uiso 1 1 calc R . .
C22 C 0.2093(3) 0.4946(3) 0.00877(16) 0.0390(7) Uani 1 1 d . . .
H22 H 0.1375 0.4527 -0.0014 0.047 Uiso 1 1 calc R . .
C23 C 0.2638(3) 0.5921(3) -0.04211(15) 0.0356(6) Uani 1 1 d . . .
H23 H 0.2292 0.6148 -0.0867 0.043 Uiso 1 1 calc R . .
C24 C 0.3700(3) 0.6565(2) -0.02681(14) 0.0270(5) Uani 1 1 d . . .
C25 C 0.4209(2) 0.6212(2) 0.03995(14) 0.0274(5) Uani 1 1 d . . .
H25 H 0.4915 0.6640 0.0507 0.033 Uiso 1 1 calc R . .
C26 C 0.4279(3) 0.7645(2) -0.07981(14) 0.0292(6) Uani 1 1 d . . .
C27 C 0.3563(3) 1.1371(3) -0.09323(17) 0.0415(7) Uani 1 1 d . . .
H27 H 0.4316 1.1512 -0.0723 0.050 Uiso 1 1 calc R . .
C28 C 0.2511(3) 1.2097(3) -0.0819(2) 0.0484(8) Uani 1 1 d . . .
H28 H 0.2554 1.2706 -0.0537 0.058 Uiso 1 1 calc R . .
C29 C 0.1379(3) 1.1916(3) -0.11302(17) 0.0371(6) Uani 1 1 d . . .
C30 C 0.1374(3) 1.0987(3) -0.15377(19) 0.0477(8) Uani 1 1 d . . .
H30 H 0.0634 1.0829 -0.1754 0.057 Uiso 1 1 calc R . .
C31 C 0.2475(3) 1.0304(3) -0.16185(18) 0.0449(8) Uani 1 1 d . . .
H31 H 0.2458 0.9683 -0.1895 0.054 Uiso 1 1 calc R . .
C32 C -0.3109(3) 1.1760(3) -0.18110(19) 0.0489(8) Uani 1 1 d . . .
H32 H -0.3634 1.2064 -0.2175 0.059 Uiso 1 1 calc R . .
C33 C -0.2065(3) 1.2466(3) -0.1713(2) 0.0507(8) Uani 1 1 d . . .
H33 H -0.1885 1.3217 -0.2013 0.061 Uiso 1 1 calc R . .
C34 C -0.1300(3) 1.2049(3) -0.11681(18) 0.0410(7) Uani 1 1 d . . .
C35 C -0.1635(4) 1.0951(4) -0.0731(2) 0.0665(11) Uani 1 1 d . . .
H35 H -0.1167 1.0657 -0.0338 0.080 Uiso 1 1 calc R . .
C36 C -0.2664(4) 1.0290(3) -0.0877(2) 0.0586(10) Uani 1 1 d . . .
H36 H -0.2857 0.9534 -0.0585 0.070 Uiso 1 1 calc R . .
O1 O 0.9202(4) -0.0008(6) 0.5725(3) 0.182(3) Uani 1 1 d . . .
H2W H 0.9565 -0.0533 0.5498 0.273 Uiso 1 1 d R . .
H1W H 0.8493 -0.0291 0.5963 0.273 Uiso 1 1 d R . .
O2 O 0.9581(8) 0.0490(9) 0.7137(4) 0.277(4) Uani 1 1 d . . .
H3W H 0.9417 0.0373 0.6716 0.416 Uiso 1 1 d R . .
H4W H 0.9606 -0.0196 0.7411 0.416 Uiso 1 1 d R . .
O3 O 0.9627(11) -0.1610(10) 0.8268(11) 0.513(12) Uani 1 1 d . . .
H6W H 1.0133 -0.1880 0.7945 0.770 Uiso 1 1 d R . .
H5W H 0.8834 -0.1581 0.8178 0.770 Uiso 1 1 d R . .
O4 O 1.0943(5) -0.2215(6) 0.5836(5) 0.247(4) Uani 1 1 d . . .
H8W H 1.1749 -0.2291 0.5850 0.370 Uiso 1 1 d R . .
H7W H 1.0606 -0.2460 0.5487 0.370 Uiso 1 1 d R . .
O5 O 1.0377(8) -0.3409(13) 0.7679(7) 0.420(9) Uani 1 1 d . . .
H10W H 1.0281 -0.3718 0.7293 0.630 Uiso 1 1 d R . .
H9W H 1.1210 -0.3438 0.7637 0.630 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O8 2.0015(19) . ?
Ni1 N1 2.061(2) 1_655 ?
Ni1 N2 2.096(2) . ?
Ni1 O7 2.1018(19) . ?
Ni1 O12 2.1152(18) . ?
Ni1 O13 2.1355(18) . ?
Ni1 C19 2.451(3) . ?
Ni2 O11 1.9935(19) 1_564 ?
Ni2 N3 2.067(2) 1_655 ?
Ni2 N4 2.092(2) . ?
Ni2 O6 2.104(2) . ?
Ni2 O14 2.1072(18) . ?
Ni2 O15 2.1669(18) . ?
Ni2 C26 2.468(3) . ?
S1 C29 1.775(3) . ?
S1 C34 1.782(3) . ?
S2 C11 1.769(3) . ?
S2 C16 1.774(3) . ?
O6 H11W 0.8376 . ?
O6 H12W 0.8358 . ?
O7 H13W 0.8464 . ?
O7 H14W 0.8370 . ?
O8 C1 1.274(3) . ?
O9 C1 1.246(3) . ?
O10 C8 1.240(4) . ?
O11 C8 1.265(3) . ?
O11 Ni2 1.9935(19) 1_546 ?
O12 C19 1.262(3) . ?
O13 C19 1.270(3) . ?
O14 C26 1.260(3) . ?
O15 C26 1.271(3) . ?
N1 C18 1.333(4) . ?
N1 C14 1.338(4) . ?
N1 Ni1 2.061(2) 1_455 ?
N2 C9 1.334(4) . ?
N2 C13 1.348(4) . ?
N3 C32 1.327(4) . ?
N3 C36 1.330(4) . ?
N3 Ni2 2.067(2) 1_455 ?
N4 C27 1.328(4) . ?
N4 C31 1.339(4) . ?
C1 C2 1.501(4) . ?
C2 C3 1.392(4) . ?
C2 C7 1.392(4) . ?
C3 C4 1.377(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.386(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.386(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.392(4) . ?
C6 C8 1.515(4) . ?
C7 H7A 0.9300 . ?
C9 C10 1.378(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.390(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.383(4) . ?
C12 C13 1.372(4) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.375(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.377(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.383(4) . ?
C17 C18 1.373(4) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.497(3) . ?
C20 C21 1.387(4) . ?
C20 C25 1.390(4) . ?
C21 C22 1.388(4) . ?
C21 H21 0.9300 . ?
C22 C23 1.385(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.392(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.390(3) . ?
C24 C26 1.496(4) . ?
C25 H25 0.9300 . ?
C27 C28 1.365(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.387(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.382(4) . ?
C30 C31 1.369(4) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 C33 1.382(4) . ?
C32 H32 0.9300 . ?
C33 C34 1.368(4) . ?
C33 H33 0.9300 . ?
C34 C35 1.370(5) . ?
C35 C36 1.371(5) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
O1 H2W 0.8380 . ?
O1 H1W 0.8378 . ?
O2 H3W 0.8437 . ?
O2 H4W 0.8463 . ?
O3 H6W 0.8376 . ?
O3 H5W 0.8498 . ?
O4 H8W 0.8345 . ?
O4 H7W 0.8500 . ?
O5 H10W 0.8583 . ?
O5 H9W 0.8504 . ?

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
O8 Ni1 N1 97.39(9) . 1_655 ?
O8 Ni1 N2 85.44(9) . . ?
N1 Ni1 N2 94.73(9) 1_655 . ?
O8 Ni1 O7 90.61(8) . . ?
N1 Ni1 O7 86.26(8) 1_655 . ?
N2 Ni1 O7 176.02(8) . . ?
O8 Ni1 O12 162.19(8) . . ?
N1 Ni1 O12 100.39(8) 1_655 . ?
N2 Ni1 O12 91.89(8) . . ?
O7 Ni1 O12 91.72(8) . . ?
O8 Ni1 O13 100.12(8) . . ?
N1 Ni1 O13 162.37(8) 1_655 . ?
N2 Ni1 O13 88.71(8) . . ?
O7 Ni1 O13 91.50(7) . . ?
O12 Ni1 O13 62.17(7) . . ?
O8 Ni1 C19 131.25(9) . . ?
N1 Ni1 C19 131.37(9) 1_655 . ?
N2 Ni1 C19 89.66(9) . . ?
O7 Ni1 C19 92.58(8) . . ?
O12 Ni1 C19 30.99(8) . . ?
O13 Ni1 C19 31.19(8) . . ?
O11 Ni2 N3 101.02(9) 1_564 1_655 ?
O11 Ni2 N4 84.12(8) 1_564 . ?
N3 Ni2 N4 96.20(9) 1_655 . ?
O11 Ni2 O6 89.96(8) 1_564 . ?
N3 Ni2 O6 87.98(8) 1_655 . ?
N4 Ni2 O6 173.31(8) . . ?
O11 Ni2 O14 162.42(9) 1_564 . ?
N3 Ni2 O14 96.56(8) 1_655 . ?
N4 Ni2 O14 93.84(8) . . ?
O6 Ni2 O14 90.86(8) . . ?
O11 Ni2 O15 100.77(8) 1_564 . ?
N3 Ni2 O15 158.13(8) 1_655 . ?
N4 Ni2 O15 87.89(8) . . ?
O6 Ni2 O15 90.17(7) . . ?
O14 Ni2 O15 61.67(7) . . ?
O11 Ni2 C26 131.74(9) 1_564 . ?
N3 Ni2 C26 127.24(9) 1_655 . ?
N4 Ni2 C26 90.70(9) . . ?
O6 Ni2 C26 90.92(8) . . ?
O14 Ni2 C26 30.69(8) . . ?
O15 Ni2 C26 30.98(7) . . ?
C29 S1 C34 101.92(14) . . ?
C11 S2 C16 101.39(13) . . ?
Ni2 O6 H11W 112.6 . . ?
Ni2 O6 H12W 101.2 . . ?
H11W O6 H12W 109.8 . . ?
Ni1 O7 H13W 113.3 . . ?
Ni1 O7 H14W 99.9 . . ?
H13W O7 H14W 107.3 . . ?
C1 O8 Ni1 127.79(18) . . ?
C8 O11 Ni2 135.03(19) . 1_546 ?
C19 O12 Ni1 89.37(15) . . ?
C19 O13 Ni1 88.26(15) . . ?
C26 O14 Ni2 90.69(15) . . ?
C26 O15 Ni2 87.70(15) . . ?
C18 N1 C14 117.4(2) . . ?
C18 N1 Ni1 122.95(19) . 1_455 ?
C14 N1 Ni1 118.90(19) . 1_455 ?
C9 N2 C13 116.8(2) . . ?
C9 N2 Ni1 125.94(19) . . ?
C13 N2 Ni1 117.17(19) . . ?
C32 N3 C36 116.5(3) . . ?
C32 N3 Ni2 125.0(2) . 1_455 ?
C36 N3 Ni2 118.2(2) . 1_455 ?
C27 N4 C31 116.4(2) . . ?
C27 N4 Ni2 125.67(19) . . ?
C31 N4 Ni2 117.44(19) . . ?
O9 C1 O8 124.5(3) . . ?
O9 C1 C2 120.7(2) . . ?
O8 C1 C2 114.8(2) . . ?
C3 C2 C7 119.3(2) . . ?
C3 C2 C1 119.3(2) . . ?
C7 C2 C1 121.4(2) . . ?
C4 C3 C2 120.6(3) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 119.7(3) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C6 C5 C4 120.6(3) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C7 119.3(2) . . ?
C5 C6 C8 118.6(2) . . ?
C7 C6 C8 122.0(2) . . ?
C2 C7 C6 120.2(3) . . ?
C2 C7 H7A 119.9 . . ?
C6 C7 H7A 119.9 . . ?
O10 C8 O11 125.0(3) . . ?
O10 C8 C6 120.7(2) . . ?
O11 C8 C6 114.3(3) . . ?
N2 C9 C10 123.6(3) . . ?
N2 C9 H9 118.2 . . ?
C10 C9 H9 118.2 . . ?
C9 C10 C11 118.9(3) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.5 . . ?
C12 C11 C10 118.1(3) . . ?
C12 C11 S2 123.6(2) . . ?
C10 C11 S2 118.2(2) . . ?
C13 C12 C11 119.1(3) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
N2 C13 C12 123.5(3) . . ?
N2 C13 H13 118.3 . . ?
C12 C13 H13 118.3 . . ?
N1 C14 C15 122.8(3) . . ?
N1 C14 H14 118.6 . . ?
C15 C14 H14 118.6 . . ?
C14 C15 C16 119.3(3) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C15 C16 C17 118.2(3) . . ?
C15 C16 S2 122.5(2) . . ?
C17 C16 S2 119.2(2) . . ?
C18 C17 C16 118.8(3) . . ?
C18 C17 H17 120.6 . . ?
C16 C17 H17 120.6 . . ?
N1 C18 C17 123.4(3) . . ?
N1 C18 H18 118.3 . . ?
C17 C18 H18 118.3 . . ?
O12 C19 O13 120.1(2) . . ?
O12 C19 C20 120.1(2) . . ?
O13 C19 C20 119.7(2) . . ?
O12 C19 Ni1 59.63(13) . . ?
O13 C19 Ni1 60.55(13) . . ?
C20 C19 Ni1 175.79(19) . . ?
C21 C20 C25 119.5(2) . . ?
C21 C20 C19 121.1(2) . . ?
C25 C20 C19 119.4(2) . . ?
C20 C21 C22 120.1(3) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C23 C22 C21 120.2(3) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C22 C23 C24 120.3(2) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C25 C24 C23 119.2(2) . . ?
C25 C24 C26 119.5(2) . . ?
C23 C24 C26 121.3(2) . . ?
C24 C25 C20 120.8(2) . . ?
C24 C25 H25 119.6 . . ?
C20 C25 H25 119.6 . . ?
O14 C26 O15 119.9(2) . . ?
O14 C26 C24 119.6(2) . . ?
O15 C26 C24 120.4(2) . . ?
O14 C26 Ni2 58.62(13) . . ?
O15 C26 Ni2 61.32(13) . . ?
C24 C26 Ni2 177.56(19) . . ?
N4 C27 C28 123.9(3) . . ?
N4 C27 H27 118.1 . . ?
C28 C27 H27 118.1 . . ?
C27 C28 C29 119.4(3) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 H28 120.3 . . ?
C30 C29 C28 117.5(3) . . ?
C30 C29 S1 123.7(2) . . ?
C28 C29 S1 118.7(2) . . ?
C31 C30 C29 119.0(3) . . ?
C31 C30 H30 120.5 . . ?
C29 C30 H30 120.5 . . ?
N4 C31 C30 123.9(3) . . ?
N4 C31 H31 118.0 . . ?
C30 C31 H31 118.0 . . ?
N3 C32 C33 123.4(3) . . ?
N3 C32 H32 118.3 . . ?
C33 C32 H32 118.3 . . ?
C34 C33 C32 119.2(3) . . ?
C34 C33 H33 120.4 . . ?
C32 C33 H33 120.4 . . ?
C33 C34 C35 117.7(3) . . ?
C33 C34 S1 120.4(2) . . ?
C35 C34 S1 121.8(3) . . ?
C34 C35 C36 119.5(3) . . ?
C34 C35 H35 120.2 . . ?
C36 C35 H35 120.2 . . ?
N3 C36 C35 123.5(3) . . ?
N3 C36 H36 118.3 . . ?
C35 C36 H36 118.3 . . ?
H2W O1 H1W 109.3 . . ?
H3W O2 H4W 107.8 . . ?
H6W O3 H5W 113.2 . . ?
H8W O4 H7W 118.4 . . ?
H10W O5 H9W 96.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Ni1 O8 C1 -48.3(2) 1_655 . . . ?
N2 Ni1 O8 C1 -142.5(2) . . . . ?
O7 Ni1 O8 C1 38.0(2) . . . . ?
O12 Ni1 O8 C1 135.5(3) . . . . ?
O13 Ni1 O8 C1 129.6(2) . . . . ?
C19 Ni1 O8 C1 131.9(2) . . . . ?
O8 Ni1 O12 C19 -5.3(4) . . . . ?
N1 Ni1 O12 C19 178.65(16) 1_655 . . . ?
N2 Ni1 O12 C19 -86.19(16) . . . . ?
O7 Ni1 O12 C19 92.13(16) . . . . ?
O13 Ni1 O12 C19 1.35(15) . . . . ?
O8 Ni1 O13 C19 176.61(15) . . . . ?
N1 Ni1 O13 C19 -10.1(3) 1_655 . . . ?
N2 Ni1 O13 C19 91.48(16) . . . . ?
O7 Ni1 O13 C19 -92.50(15) . . . . ?
O12 Ni1 O13 C19 -1.34(15) . . . . ?
O11 Ni2 O14 C26 2.3(4) 1_564 . . . ?
N3 Ni2 O14 C26 -178.41(16) 1_655 . . . ?
N4 Ni2 O14 C26 84.89(17) . . . . ?
O6 Ni2 O14 C26 -90.35(16) . . . . ?
O15 Ni2 O14 C26 -0.62(15) . . . . ?
O11 Ni2 O15 C26 -178.50(15) 1_564 . . . ?
N3 Ni2 O15 C26 6.5(3) 1_655 . . . ?
N4 Ni2 O15 C26 -94.89(16) . . . . ?
O6 Ni2 O15 C26 91.51(15) . . . . ?
O14 Ni2 O15 C26 0.62(15) . . . . ?
O8 Ni1 N2 C9 121.3(2) . . . . ?
N1 Ni1 N2 C9 24.2(2) 1_655 . . . ?
O7 Ni1 N2 C9 128.5(11) . . . . ?
O12 Ni1 N2 C9 -76.4(2) . . . . ?
O13 Ni1 N2 C9 -138.5(2) . . . . ?
C19 Ni1 N2 C9 -107.3(2) . . . . ?
O8 Ni1 N2 C13 -55.4(2) . . . . ?
N1 Ni1 N2 C13 -152.5(2) 1_655 . . . ?
O7 Ni1 N2 C13 -48.2(12) . . . . ?
O12 Ni1 N2 C13 106.9(2) . . . . ?
O13 Ni1 N2 C13 44.8(2) . . . . ?
C19 Ni1 N2 C13 76.0(2) . . . . ?
O11 Ni2 N4 C27 -116.2(2) 1_564 . . . ?
N3 Ni2 N4 C27 -15.7(2) 1_655 . . . ?
O6 Ni2 N4 C27 -144.1(6) . . . . ?
O14 Ni2 N4 C27 81.3(2) . . . . ?
O15 Ni2 N4 C27 142.8(2) . . . . ?
C26 Ni2 N4 C27 111.9(2) . . . . ?
O11 Ni2 N4 C31 55.2(2) 1_564 . . . ?
N3 Ni2 N4 C31 155.7(2) 1_655 . . . ?
O6 Ni2 N4 C31 27.3(8) . . . . ?
O14 Ni2 N4 C31 -107.2(2) . . . . ?
O15 Ni2 N4 C31 -45.8(2) . . . . ?
C26 Ni2 N4 C31 -76.7(2) . . . . ?
Ni1 O8 C1 O9 -15.8(4) . . . . ?
Ni1 O8 C1 C2 162.45(18) . . . . ?
O9 C1 C2 C3 -162.2(3) . . . . ?
O8 C1 C2 C3 19.4(4) . . . . ?
O9 C1 C2 C7 19.0(4) . . . . ?
O8 C1 C2 C7 -159.4(2) . . . . ?
C7 C2 C3 C4 0.4(4) . . . . ?
C1 C2 C3 C4 -178.5(3) . . . . ?
C2 C3 C4 C5 3.2(4) . . . . ?
C3 C4 C5 C6 -3.6(5) . . . . ?
C4 C5 C6 C7 0.3(4) . . . . ?
C4 C5 C6 C8 -178.7(3) . . . . ?
C3 C2 C7 C6 -3.7(4) . . . . ?
C1 C2 C7 C6 175.1(2) . . . . ?
C5 C6 C7 C2 3.4(4) . . . . ?
C8 C6 C7 C2 -177.7(2) . . . . ?
Ni2 O11 C8 O10 -11.4(5) 1_546 . . . ?
Ni2 O11 C8 C6 168.7(2) 1_546 . . . ?
C5 C6 C8 O10 156.0(3) . . . . ?
C7 C6 C8 O10 -23.0(4) . . . . ?
C5 C6 C8 O11 -24.2(4) . . . . ?
C7 C6 C8 O11 156.9(3) . . . . ?
C13 N2 C9 C10 -0.9(4) . . . . ?
Ni1 N2 C9 C10 -177.6(2) . . . . ?
N2 C9 C10 C11 0.9(5) . . . . ?
C9 C10 C11 C12 -0.2(5) . . . . ?
C9 C10 C11 S2 176.0(2) . . . . ?
C16 S2 C11 C12 -34.9(3) . . . . ?
C16 S2 C11 C10 149.2(3) . . . . ?
C10 C11 C12 C13 -0.5(5) . . . . ?
S2 C11 C12 C13 -176.4(2) . . . . ?
C9 N2 C13 C12 0.2(4) . . . . ?
Ni1 N2 C13 C12 177.2(2) . . . . ?
C11 C12 C13 N2 0.5(5) . . . . ?
C18 N1 C14 C15 1.6(5) . . . . ?
Ni1 N1 C14 C15 -168.5(3) 1_455 . . . ?
N1 C14 C15 C16 0.0(5) . . . . ?
C14 C15 C16 C17 -1.8(5) . . . . ?
C14 C15 C16 S2 -179.3(3) . . . . ?
C11 S2 C16 C15 -51.9(3) . . . . ?
C11 S2 C16 C17 130.6(3) . . . . ?
C15 C16 C17 C18 1.8(5) . . . . ?
S2 C16 C17 C18 179.5(2) . . . . ?
C14 N1 C18 C17 -1.6(5) . . . . ?
Ni1 N1 C18 C17 168.2(2) 1_455 . . . ?
C16 C17 C18 N1 -0.2(5) . . . . ?
Ni1 O12 C19 O13 -2.3(3) . . . . ?
Ni1 O12 C19 C20 175.1(2) . . . . ?
Ni1 O13 C19 O12 2.3(2) . . . . ?
Ni1 O13 C19 C20 -175.2(2) . . . . ?
O8 Ni1 C19 O12 177.87(14) . . . . ?
N1 Ni1 C19 O12 -1.8(2) 1_655 . . . ?
N2 Ni1 C19 O12 94.24(16) . . . . ?
O7 Ni1 C19 O12 -89.06(16) . . . . ?
O13 Ni1 C19 O12 -177.7(2) . . . . ?
O8 Ni1 C19 O13 -4.4(2) . . . . ?
N1 Ni1 C19 O13 175.93(14) 1_655 . . . ?
N2 Ni1 C19 O13 -88.07(16) . . . . ?
O7 Ni1 C19 O13 88.64(15) . . . . ?
O12 Ni1 C19 O13 177.7(2) . . . . ?
O8 Ni1 C19 C20 90(3) . . . . ?
N1 Ni1 C19 C20 -89(3) 1_655 . . . ?
N2 Ni1 C19 C20 7(3) . . . . ?
O7 Ni1 C19 C20 -177(3) . . . . ?
O12 Ni1 C19 C20 -87(3) . . . . ?
O13 Ni1 C19 C20 95(3) . . . . ?
O12 C19 C20 C21 -166.8(3) . . . . ?
O13 C19 C20 C21 10.7(4) . . . . ?
Ni1 C19 C20 C21 -82(3) . . . . ?
O12 C19 C20 C25 10.7(4) . . . . ?
O13 C19 C20 C25 -171.9(2) . . . . ?
Ni1 C19 C20 C25 96(3) . . . . ?
C25 C20 C21 C22 -0.3(4) . . . . ?
C19 C20 C21 C22 177.1(3) . . . . ?
C20 C21 C22 C23 1.0(5) . . . . ?
C21 C22 C23 C24 -1.0(5) . . . . ?
C22 C23 C24 C25 0.3(4) . . . . ?
C22 C23 C24 C26 -178.1(3) . . . . ?
C23 C24 C25 C20 0.4(4) . . . . ?
C26 C24 C25 C20 178.8(2) . . . . ?
C21 C20 C25 C24 -0.4(4) . . . . ?
C19 C20 C25 C24 -177.9(2) . . . . ?
Ni2 O14 C26 O15 1.1(3) . . . . ?
Ni2 O14 C26 C24 -178.0(2) . . . . ?
Ni2 O15 C26 O14 -1.1(3) . . . . ?
Ni2 O15 C26 C24 178.0(2) . . . . ?
C25 C24 C26 O14 -9.8(4) . . . . ?
C23 C24 C26 O14 168.5(3) . . . . ?
C25 C24 C26 O15 171.1(2) . . . . ?
C23 C24 C26 O15 -10.6(4) . . . . ?
C25 C24 C26 Ni2 -54(5) . . . . ?
C23 C24 C26 Ni2 124(4) . . . . ?
O11 Ni2 C26 O14 -179.09(15) 1_564 . . . ?
N3 Ni2 C26 O14 2.0(2) 1_655 . . . ?
N4 Ni2 C26 O14 -96.35(16) . . . . ?
O6 Ni2 C26 O14 90.14(16) . . . . ?
O15 Ni2 C26 O14 178.9(3) . . . . ?
O11 Ni2 C26 O15 2.0(2) 1_564 . . . ?
N3 Ni2 C26 O15 -176.95(14) 1_655 . . . ?
N4 Ni2 C26 O15 84.72(15) . . . . ?
O6 Ni2 C26 O15 -88.79(15) . . . . ?
O14 Ni2 C26 O15 -178.9(3) . . . . ?
O11 Ni2 C26 C24 -134(4) 1_564 . . . ?
N3 Ni2 C26 C24 47(4) 1_655 . . . ?
N4 Ni2 C26 C24 -51(4) . . . . ?
O6 Ni2 C26 C24 135(4) . . . . ?
O14 Ni2 C26 C24 45(4) . . . . ?
O15 Ni2 C26 C24 -136(5) . . . . ?
C31 N4 C27 C28 0.3(5) . . . . ?
Ni2 N4 C27 C28 171.7(3) . . . . ?
N4 C27 C28 C29 -0.6(5) . . . . ?
C27 C28 C29 C30 0.7(5) . . . . ?
C27 C28 C29 S1 -175.9(3) . . . . ?
C34 S1 C29 C30 25.4(3) . . . . ?
C34 S1 C29 C28 -158.2(3) . . . . ?
C28 C29 C30 C31 -0.4(5) . . . . ?
S1 C29 C30 C31 176.0(3) . . . . ?
C27 N4 C31 C30 0.0(5) . . . . ?
Ni2 N4 C31 C30 -172.2(3) . . . . ?
C29 C30 C31 N4 0.1(5) . . . . ?
C36 N3 C32 C33 2.9(5) . . . . ?
Ni2 N3 C32 C33 -171.1(3) 1_455 . . . ?
N3 C32 C33 C34 -1.6(6) . . . . ?
C32 C33 C34 C35 -1.7(5) . . . . ?
C32 C33 C34 S1 179.6(3) . . . . ?
C29 S1 C34 C33 -122.9(3) . . . . ?
C29 S1 C34 C35 58.4(3) . . . . ?
C33 C34 C35 C36 3.4(6) . . . . ?
S1 C34 C35 C36 -177.8(3) . . . . ?
C32 N3 C36 C35 -1.0(6) . . . . ?
Ni2 N3 C36 C35 173.4(3) 1_455 . . . ?
C34 C35 C36 N3 -2.2(7) . . . . ?

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 H12W O10 0.84 2.00 2.800(3) 159.9 1_564
O7 H13W O15 0.85 1.90 2.742(3) 177.4 2_665
O7 H14W O9 0.84 1.91 2.707(3) 158.4 .
O1 H2W O4 0.84 2.39 3.034(9) 134.0 .
O1 H2W O1 0.84 2.43 2.961(10) 121.8 2_756
O1 H1W O10 0.84 2.08 2.816(5) 146.6 .
O2 H3W O1 0.84 1.98 2.824(8) 173.9 .
O2 H4W O3 0.85 2.04 2.870(17) 166.4 .
O3 H6W O5 0.84 1.87 2.519(17) 133.9 .
O3 H5W O6 0.85 2.20 3.051(11) 179.4 1_546
O4 H8W O9 0.83 1.91 2.732(5) 166.2 2_756
O4 H7W S2 0.85 2.61 3.463(6) 179.4 1_645
O5 H9W O7 0.85 2.23 3.081(9) 179.4 2_756

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.063

# Attachment '2.cif'

data_b
_database_code_depnum_ccdc_archive 'CCDC 701846'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H26 N6 Ni2 O14 S2'
_chemical_formula_weight         948.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   P2/n

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

_cell_length_a                   14.3584(14)
_cell_length_b                   8.2781(8)
_cell_length_c                   15.8981(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.7350(10)
_cell_angle_gamma                90.00
_cell_volume                     1885.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    6302
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      28.02

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.41
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             968
_exptl_absorpt_coefficient_mu    1.189
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.5941
_exptl_absorpt_correction_T_max  0.6383
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      291(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13517
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         25.50
_reflns_number_total             3504
_reflns_number_gt                3157
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.7500P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    CONSTR
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3504
_refine_ls_number_parameters     272
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0268
_refine_ls_wR_factor_ref         0.0942
_refine_ls_wR_factor_gt          0.0879
_refine_ls_goodness_of_fit_ref   0.735
_refine_ls_restrained_S_all      0.735
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.7500 0.72217(4) 1.2500 0.02295(12) Uani 1 2 d S . .
Ni2 Ni 0.7500 0.24878(4) 0.7500 0.02719(13) Uani 1 2 d S . .
S1 S 1.04475(5) 0.73099(7) 0.97408(4) 0.04790(18) Uani 1 1 d . . .
O1 O 0.63149(9) 0.65651(17) 1.17995(8) 0.0337(3) Uani 1 1 d . . .
O2 O 0.76140(9) 0.53202(17) 1.15171(9) 0.0383(3) Uani 1 1 d . . .
O3 O 0.69000(11) 0.25382(17) 0.86195(9) 0.0399(4) Uani 1 1 d . . .
O4 O 0.56350(9) 0.09528(16) 0.84502(8) 0.0342(3) Uani 1 1 d . . .
O5 O 0.32576(9) 0.1641(2) 1.06030(9) 0.0501(4) Uani 1 1 d . . .
O6 O 0.37542(10) 0.24900(17) 1.18355(9) 0.0385(4) Uani 1 1 d . . .
O7 O 0.84237(12) 0.06311(18) 0.79484(9) 0.0468(4) Uani 1 1 d . . .
H1W H 0.8805 0.0478 0.7582 0.070 Uiso 1 1 d R . .
H2W H 0.8132 -0.0204 0.8046 0.070 Uiso 1 1 d R . .
N1 N 0.84667(10) 0.41882(19) 0.80565(10) 0.0292(3) Uani 1 1 d . . .
N2 N 1.18709(10) 1.10664(18) 0.81880(9) 0.0293(3) Uani 1 1 d . . .
N3 N 0.38595(11) 0.2247(2) 1.10898(10) 0.0297(4) Uani 1 1 d . . .
C1 C 0.67424(13) 0.5439(2) 1.14365(11) 0.0280(4) Uani 1 1 d . . .
C2 C 0.61593(12) 0.4239(2) 1.09303(11) 0.0268(4) Uani 1 1 d . . .
C3 C 0.53048(12) 0.3798(2) 1.12156(11) 0.0282(4) Uani 1 1 d . . .
H3 H 0.5105 0.4227 1.1714 0.034 Uiso 1 1 calc R . .
C4 C 0.47536(13) 0.2713(2) 1.07506(12) 0.0257(4) Uani 1 1 d . . .
C5 C 0.49997(13) 0.2092(2) 0.99862(11) 0.0250(4) Uani 1 1 d . . .
H5A H 0.4601 0.1404 0.9672 0.030 Uiso 1 1 calc R . .
C6 C 0.58652(13) 0.25339(19) 0.97035(11) 0.0254(4) Uani 1 1 d . . .
C7 C 0.64470(12) 0.3573(2) 1.01858(11) 0.0273(4) Uani 1 1 d . . .
H7A H 0.7034 0.3825 1.0008 0.033 Uiso 1 1 calc R . .
C8 C 0.61482(12) 0.1934(2) 0.88524(10) 0.0266(4) Uani 1 1 d . . .
C9 C 0.81561(13) 0.5344(2) 0.85511(13) 0.0370(5) Uani 1 1 d . . .
H9 H 0.7514 0.5478 0.8567 0.044 Uiso 1 1 calc R . .
C10 C 0.87354(14) 0.6359(3) 0.90437(14) 0.0400(5) Uani 1 1 d . . .
H10 H 0.8486 0.7149 0.9379 0.048 Uiso 1 1 calc R . .
C11 C 0.96925(14) 0.6169(2) 0.90250(12) 0.0352(4) Uani 1 1 d . . .
C12 C 1.00312(13) 0.4999(3) 0.85020(12) 0.0362(4) Uani 1 1 d . . .
H12 H 1.0670 0.4856 0.8469 0.043 Uiso 1 1 calc R . .
C13 C 0.94021(13) 0.4046(2) 0.80309(12) 0.0329(4) Uani 1 1 d . . .
H13 H 0.9634 0.3267 0.7678 0.040 Uiso 1 1 calc R . .
C14 C 1.21414(14) 1.0736(3) 0.89897(12) 0.0379(5) Uani 1 1 d . . .
H14 H 1.2635 1.1325 0.9244 0.046 Uiso 1 1 calc R . .
C15 C 1.17277(15) 0.9567(3) 0.94614(12) 0.0394(5) Uani 1 1 d . . .
H15 H 1.1941 0.9370 1.0017 0.047 Uiso 1 1 calc R . .
C16 C 1.09872(13) 0.8692(2) 0.90865(12) 0.0310(4) Uani 1 1 d . . .
C17 C 1.07071(14) 0.9006(2) 0.82504(12) 0.0373(5) Uani 1 1 d . . .
H17 H 1.0223 0.8423 0.7977 0.045 Uiso 1 1 calc R . .
C18 C 1.11622(13) 1.0201(2) 0.78331(12) 0.0355(4) Uani 1 1 d . . .
H18 H 1.0966 1.0416 0.7275 0.043 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 2.0369(15) 3_777 ?
Ni1 N2 2.0369(15) 4_576 ?
Ni1 O1 2.0456(13) 2_657 ?
Ni1 O1 2.0456(13) . ?
Ni1 O2 2.2315(13) 2_657 ?
Ni1 O2 2.2315(13) . ?
Ni1 C1 2.4453(18) . ?
Ni1 C1 2.4453(18) 2_657 ?
Ni2 O3 2.0276(14) . ?
Ni2 O3 2.0277(14) 2_656 ?
Ni2 O7 2.1229(15) . ?
Ni2 O7 2.1229(15) 2_656 ?
Ni2 N1 2.1286(16) . ?
Ni2 N1 2.1286(16) 2_656 ?
S1 C16 1.7600(19) . ?
S1 C11 1.789(2) . ?
O1 C1 1.274(2) . ?
O2 C1 1.254(2) . ?
O3 C8 1.267(2) . ?
O4 C8 1.245(2) . ?
O5 N3 1.229(2) . ?
O6 N3 1.222(2) . ?
O7 H1W 0.8351 . ?
O7 H2W 0.8283 . ?
N1 C9 1.334(3) . ?
N1 C13 1.351(2) . ?
N2 C14 1.336(2) . ?
N2 C18 1.339(2) . ?
N2 Ni1 2.0369(15) 3_777 ?
N3 C4 1.476(2) . ?
C1 C2 1.499(2) . ?
C2 C3 1.385(3) . ?
C2 C7 1.393(2) . ?
C3 C4 1.380(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.386(3) . ?
C5 C6 1.397(3) . ?
C5 H5A 0.9300 . ?
C6 C7 1.394(3) . ?
C6 C8 1.521(2) . ?
C7 H7A 0.9300 . ?
C9 C10 1.388(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.385(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.386(3) . ?
C12 C13 1.382(3) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.382(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.388(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.388(3) . ?
C17 C18 1.379(3) . ?
C17 H17 0.9300 . ?
C18 H18 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
N2 Ni1 N2 91.83(9) 3_777 4_576 ?
N2 Ni1 O1 95.45(6) 3_777 2_657 ?
N2 Ni1 O1 105.95(6) 4_576 2_657 ?
N2 Ni1 O1 105.95(6) 3_777 . ?
N2 Ni1 O1 95.45(6) 4_576 . ?
O1 Ni1 O1 149.18(8) 2_657 . ?
N2 Ni1 O2 157.23(5) 3_777 2_657 ?
N2 Ni1 O2 93.41(6) 4_576 2_657 ?
O1 Ni1 O2 61.82(5) 2_657 2_657 ?
O1 Ni1 O2 95.59(5) . 2_657 ?
N2 Ni1 O2 93.41(6) 3_777 . ?
N2 Ni1 O2 157.23(5) 4_576 . ?
O1 Ni1 O2 95.59(5) 2_657 . ?
O1 Ni1 O2 61.81(5) . . ?
O2 Ni1 O2 90.28(8) 2_657 . ?
N2 Ni1 C1 103.97(6) 3_777 . ?
N2 Ni1 C1 126.74(6) 4_576 . ?
O1 Ni1 C1 122.21(6) 2_657 . ?
O1 Ni1 C1 31.39(6) . . ?
O2 Ni1 C1 90.51(6) 2_657 . ?
O2 Ni1 C1 30.66(5) . . ?
N2 Ni1 C1 126.74(6) 3_777 2_657 ?
N2 Ni1 C1 103.97(6) 4_576 2_657 ?
O1 Ni1 C1 31.39(6) 2_657 2_657 ?
O1 Ni1 C1 122.21(6) . 2_657 ?
O2 Ni1 C1 30.66(5) 2_657 2_657 ?
O2 Ni1 C1 90.52(6) . 2_657 ?
C1 Ni1 C1 105.78(9) . 2_657 ?
O3 Ni2 O3 177.64(8) . 2_656 ?
O3 Ni2 O7 90.69(6) . . ?
O3 Ni2 O7 91.02(6) 2_656 . ?
O3 Ni2 O7 91.02(6) . 2_656 ?
O3 Ni2 O7 90.68(6) 2_656 2_656 ?
O7 Ni2 O7 87.22(9) . 2_656 ?
O3 Ni2 N1 85.66(6) . . ?
O3 Ni2 N1 92.78(6) 2_656 . ?
O7 Ni2 N1 87.88(7) . . ?
O7 Ni2 N1 174.05(6) 2_656 . ?
O3 Ni2 N1 92.77(6) . 2_656 ?
O3 Ni2 N1 85.66(6) 2_656 2_656 ?
O7 Ni2 N1 174.05(6) . 2_656 ?
O7 Ni2 N1 87.88(7) 2_656 2_656 ?
N1 Ni2 N1 97.20(8) . 2_656 ?
C16 S1 C11 103.83(9) . . ?
C1 O1 Ni1 91.87(11) . . ?
C1 O2 Ni1 84.13(10) . . ?
C8 O3 Ni2 131.86(12) . . ?
Ni2 O7 H1W 107.4 . . ?
Ni2 O7 H2W 110.8 . . ?
H1W O7 H2W 111.5 . . ?
C9 N1 C13 116.83(17) . . ?
C9 N1 Ni2 119.05(12) . . ?
C13 N1 Ni2 123.52(13) . . ?
C14 N2 C18 117.25(16) . . ?
C14 N2 Ni1 122.89(12) . 3_777 ?
C18 N2 Ni1 119.85(12) . 3_777 ?
O6 N3 O5 123.51(16) . . ?
O6 N3 C4 118.50(16) . . ?
O5 N3 C4 117.99(16) . . ?
O2 C1 O1 121.22(16) . . ?
O2 C1 C2 121.44(16) . . ?
O1 C1 C2 117.32(16) . . ?
O2 C1 Ni1 65.20(10) . . ?
O1 C1 Ni1 56.73(9) . . ?
C2 C1 Ni1 168.15(13) . . ?
C3 C2 C7 119.48(16) . . ?
C3 C2 C1 118.34(15) . . ?
C7 C2 C1 122.17(16) . . ?
C4 C3 C2 119.07(16) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 122.75(17) . . ?
C3 C4 N3 117.17(16) . . ?
C5 C4 N3 120.06(16) . . ?
C4 C5 C6 117.89(17) . . ?
C4 C5 H5A 121.1 . . ?
C6 C5 H5A 121.1 . . ?
C7 C6 C5 119.89(16) . . ?
C7 C6 C8 120.37(16) . . ?
C5 C6 C8 119.69(16) . . ?
C2 C7 C6 120.77(16) . . ?
C2 C7 H7A 119.6 . . ?
C6 C7 H7A 119.6 . . ?
O4 C8 O3 126.48(16) . . ?
O4 C8 C6 119.10(16) . . ?
O3 C8 C6 114.40(15) . . ?
N1 C9 C10 123.77(18) . . ?
N1 C9 H9 118.1 . . ?
C10 C9 H9 118.1 . . ?
C11 C10 C9 118.58(19) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C10 C11 C12 118.64(18) . . ?
C10 C11 S1 119.17(17) . . ?
C12 C11 S1 121.94(16) . . ?
C13 C12 C11 118.80(18) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
N1 C13 C12 123.34(18) . . ?
N1 C13 H13 118.3 . . ?
C12 C13 H13 118.3 . . ?
N2 C14 C15 123.54(17) . . ?
N2 C14 H14 118.2 . . ?
C15 C14 H14 118.2 . . ?
C14 C15 C16 118.45(17) . . ?
C14 C15 H15 120.8 . . ?
C16 C15 H15 120.8 . . ?
C17 C16 C15 118.66(17) . . ?
C17 C16 S1 125.21(15) . . ?
C15 C16 S1 116.08(14) . . ?
C18 C17 C16 118.57(17) . . ?
C18 C17 H17 120.7 . . ?
C16 C17 H17 120.7 . . ?
N2 C18 C17 123.52(17) . . ?
N2 C18 H18 118.2 . . ?
C17 C18 H18 118.2 . . ?

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 O1 C1 90.78(12) 3_777 . . . ?
N2 Ni1 O1 C1 -175.74(11) 4_576 . . . ?
O1 Ni1 O1 C1 -41.43(10) 2_657 . . . ?
O2 Ni1 O1 C1 -81.77(11) 2_657 . . . ?
O2 Ni1 O1 C1 5.54(10) . . . . ?
C1 Ni1 O1 C1 -65.46(15) 2_657 . . . ?
N2 Ni1 O2 C1 -111.94(11) 3_777 . . . ?
N2 Ni1 O2 C1 -9.0(2) 4_576 . . . ?
O1 Ni1 O2 C1 152.23(11) 2_657 . . . ?
O1 Ni1 O2 C1 -5.66(10) . . . . ?
O2 Ni1 O2 C1 90.53(11) 2_657 . . . ?
C1 Ni1 O2 C1 121.20(11) 2_657 . . . ?
O3 Ni2 O3 C8 123.24(18) 2_656 . . . ?
O7 Ni2 O3 C8 -100.34(19) . . . . ?
O7 Ni2 O3 C8 -13.10(19) 2_656 . . . ?
N1 Ni2 O3 C8 171.84(19) . . . . ?
N1 Ni2 O3 C8 74.82(19) 2_656 . . . ?
O3 Ni2 N1 C9 -39.45(15) . . . . ?
O3 Ni2 N1 C9 138.78(15) 2_656 . . . ?
O7 Ni2 N1 C9 -130.30(15) . . . . ?
O7 Ni2 N1 C9 -95.7(5) 2_656 . . . ?
N1 Ni2 N1 C9 52.80(13) 2_656 . . . ?
O3 Ni2 N1 C13 131.41(15) . . . . ?
O3 Ni2 N1 C13 -50.36(14) 2_656 . . . ?
O7 Ni2 N1 C13 40.56(14) . . . . ?
O7 Ni2 N1 C13 75.2(6) 2_656 . . . ?
N1 Ni2 N1 C13 -136.33(16) 2_656 . . . ?
Ni1 O2 C1 O1 9.39(17) . . . . ?
Ni1 O2 C1 C2 -168.86(16) . . . . ?
Ni1 O1 C1 O2 -10.21(18) . . . . ?
Ni1 O1 C1 C2 168.11(14) . . . . ?
N2 Ni1 C1 O2 72.58(12) 3_777 . . . ?
N2 Ni1 C1 O2 175.68(10) 4_576 . . . ?
O1 Ni1 C1 O2 -33.23(13) 2_657 . . . ?
O1 Ni1 C1 O2 170.39(17) . . . . ?
O2 Ni1 C1 O2 -89.68(12) 2_657 . . . ?
C1 Ni1 C1 O2 -62.73(10) 2_657 . . . ?
N2 Ni1 C1 O1 -97.81(11) 3_777 . . . ?
N2 Ni1 C1 O1 5.29(13) 4_576 . . . ?
O1 Ni1 C1 O1 156.38(9) 2_657 . . . ?
O2 Ni1 C1 O1 99.93(11) 2_657 . . . ?
O2 Ni1 C1 O1 -170.39(17) . . . . ?
C1 Ni1 C1 O1 126.88(12) 2_657 . . . ?
N2 Ni1 C1 C2 -160.8(6) 3_777 . . . ?
N2 Ni1 C1 C2 -57.7(7) 4_576 . . . ?
O1 Ni1 C1 C2 93.4(6) 2_657 . . . ?
O1 Ni1 C1 C2 -63.0(6) . . . . ?
O2 Ni1 C1 C2 36.9(6) 2_657 . . . ?
O2 Ni1 C1 C2 126.6(7) . . . . ?
C1 Ni1 C1 C2 63.9(6) 2_657 . . . ?
O2 C1 C2 C3 142.81(19) . . . . ?
O1 C1 C2 C3 -35.5(2) . . . . ?
Ni1 C1 C2 C3 21.5(7) . . . . ?
O2 C1 C2 C7 -37.7(3) . . . . ?
O1 C1 C2 C7 143.98(18) . . . . ?
Ni1 C1 C2 C7 -159.0(6) . . . . ?
C7 C2 C3 C4 -0.4(3) . . . . ?
C1 C2 C3 C4 179.06(16) . . . . ?
C2 C3 C4 C5 -2.9(3) . . . . ?
C2 C3 C4 N3 178.50(17) . . . . ?
O6 N3 C4 C3 -18.3(2) . . . . ?
O5 N3 C4 C3 161.29(18) . . . . ?
O6 N3 C4 C5 163.06(17) . . . . ?
O5 N3 C4 C5 -17.4(3) . . . . ?
C3 C4 C5 C6 3.2(3) . . . . ?
N3 C4 C5 C6 -178.21(16) . . . . ?
C4 C5 C6 C7 -0.3(3) . . . . ?
C4 C5 C6 C8 -177.64(16) . . . . ?
C3 C2 C7 C6 3.3(3) . . . . ?
C1 C2 C7 C6 -176.17(16) . . . . ?
C5 C6 C7 C2 -2.9(3) . . . . ?
C8 C6 C7 C2 174.41(17) . . . . ?
Ni2 O3 C8 O4 9.9(3) . . . . ?
Ni2 O3 C8 C6 -168.71(12) . . . . ?
C7 C6 C8 O4 176.98(17) . . . . ?
C5 C6 C8 O4 -5.7(3) . . . . ?
C7 C6 C8 O3 -4.3(3) . . . . ?
C5 C6 C8 O3 173.06(17) . . . . ?
C13 N1 C9 C10 -1.5(3) . . . . ?
Ni2 N1 C9 C10 169.95(17) . . . . ?
N1 C9 C10 C11 0.0(3) . . . . ?
C9 C10 C11 C12 1.3(3) . . . . ?
C9 C10 C11 S1 -173.13(16) . . . . ?
C16 S1 C11 C10 -110.60(17) . . . . ?
C16 S1 C11 C12 75.13(18) . . . . ?
C10 C11 C12 C13 -1.1(3) . . . . ?
S1 C11 C12 C13 173.17(15) . . . . ?
C9 N1 C13 C12 1.7(3) . . . . ?
Ni2 N1 C13 C12 -169.32(15) . . . . ?
C11 C12 C13 N1 -0.4(3) . . . . ?
C18 N2 C14 C15 -0.3(3) . . . . ?
Ni1 N2 C14 C15 -179.30(17) 3_777 . . . ?
N2 C14 C15 C16 -0.4(3) . . . . ?
C14 C15 C16 C17 1.3(3) . . . . ?
C14 C15 C16 S1 -176.28(17) . . . . ?
C11 S1 C16 C17 12.7(2) . . . . ?
C11 S1 C16 C15 -169.88(17) . . . . ?
C15 C16 C17 C18 -1.5(3) . . . . ?
S1 C16 C17 C18 175.84(17) . . . . ?
C14 N2 C18 C17 0.0(3) . . . . ?
Ni1 N2 C18 C17 179.11(16) 3_777 . . . ?
C16 C17 C18 N2 0.9(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
O7 H1W O4 0.84 1.91 2.690(2) 153.9 2_656

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.061

# Attachment '3.cif'

data_c
_database_code_depnum_ccdc_archive 'CCDC 701847'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H22 N4 Ni O6 S2'
_chemical_formula_weight         633.33

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   P2(1)/c

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

_cell_length_a                   10.117(4)
_cell_length_b                   19.692(8)
_cell_length_c                   15.346(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.672(4)
_cell_angle_gamma                90.00
_cell_volume                     2929(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    5219
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      28.15

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1304
_exptl_absorpt_coefficient_mu    0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6845
_exptl_absorpt_correction_T_max  0.8333
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      291(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22057
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.34
_diffrn_reflns_theta_max         25.50
_reflns_number_total             5446
_reflns_number_gt                4829
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0325P)²+1.9066P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5446
_refine_ls_number_parameters     371
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0296
_refine_ls_wR_factor_ref         0.0750
_refine_ls_wR_factor_gt          0.0714
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.48207(3) 0.009444(11) 0.241134(16) 0.02702(8) Uani 1 1 d . . .
S1 S -0.09779(7) 0.13922(4) -0.03665(6) 0.0747(2) Uani 1 1 d . . .
S2 S 1.08067(6) -0.12910(3) 0.47083(4) 0.04575(15) Uani 1 1 d . . .
O1 O 0.50565(15) 0.09585(6) 0.32011(8) 0.0321(3) Uani 1 1 d . . .
O2 O 0.52248(18) 0.17635(7) 0.22176(9) 0.0433(4) Uani 1 1 d . . .
O3 O 0.53384(15) 0.41863(6) 0.32399(9) 0.0327(3) Uani 1 1 d . . .
O4 O 0.4553(3) 0.44128(8) 0.44140(13) 0.0806(7) Uani 1 1 d . . .
O5 O 0.4994(2) 0.21643(7) 0.60388(9) 0.0519(4) Uani 1 1 d . . .
H5 H 0.5062 0.2492 0.6378 0.078 Uiso 1 1 calc R . .
O6 O 0.59601(16) 0.05360(7) 0.16301(9) 0.0399(3) Uani 1 1 d . . .
H1W H 0.5798 0.0944 0.1581 0.060 Uiso 1 1 d R . .
H2W H 0.5779 0.0352 0.1119 0.060 Uiso 1 1 d R . .
N1 N 0.29511(18) 0.04758(8) 0.15143(11) 0.0363(4) Uani 1 1 d . . .
N2 N 0.0238(3) 0.31275(18) -0.1931(2) 0.1038(10) Uani 1 1 d U . .
N3 N 0.66983(17) -0.02862(8) 0.32591(11) 0.0315(4) Uani 1 1 d . . .
N4 N 1.36162(16) -0.03466(8) 0.31866(10) 0.0295(3) Uani 1 1 d . . .
C1 C 0.50535(19) 0.20990(9) 0.36763(12) 0.0254(4) Uani 1 1 d . . .
C2 C 0.50064(19) 0.27858(9) 0.34621(12) 0.0269(4) Uani 1 1 d . . .
H2 H 0.5025 0.2923 0.2886 0.032 Uiso 1 1 calc R . .
C3 C 0.4931(2) 0.32671(9) 0.41059(12) 0.0284(4) Uani 1 1 d . . .
C4 C 0.4889(2) 0.30627(9) 0.49622(12) 0.0332(4) Uani 1 1 d . . .
H4 H 0.4798 0.3385 0.5384 0.040 Uiso 1 1 calc R . .
C5 C 0.4982(2) 0.23818(9) 0.51929(12) 0.0325(4) Uani 1 1 d . . .
C6 C 0.5048(2) 0.18991(9) 0.45467(12) 0.0303(4) Uani 1 1 d . . .
H6A H 0.5088 0.1440 0.4695 0.036 Uiso 1 1 calc R . .
C7 C 0.51164(19) 0.15709(9) 0.29734(12) 0.0271(4) Uani 1 1 d . . .
C8 C 0.4915(2) 0.40158(9) 0.39035(13) 0.0370(5) Uani 1 1 d . . .
C9 C 0.2093(3) 0.08615(12) 0.18201(16) 0.0507(6) Uani 1 1 d . . .
H9 H 0.2308 0.0939 0.2443 0.061 Uiso 1 1 calc R . .
C10 C 0.0910(3) 0.11504(14) 0.12674(18) 0.0577(7) Uani 1 1 d . . .
H10 H 0.0344 0.1415 0.1513 0.069 Uiso 1 1 calc R . .
C11 C 0.0582(2) 0.10399(13) 0.03470(17) 0.0516(6) Uani 1 1 d . . .
C12 C 0.1439(3) 0.06304(14) 0.00214(16) 0.0552(6) Uani 1 1 d . . .
H12 H 0.1230 0.0536 -0.0597 0.066 Uiso 1 1 calc R . .
C13 C 0.2611(2) 0.03618(11) 0.06223(14) 0.0438(5) Uani 1 1 d . . .
H13 H 0.3187 0.0090 0.0394 0.053 Uiso 1 1 calc R . .
C14 C 0.1203(4) 0.2748(2) -0.1363(3) 0.1086(13) Uani 1 1 d U . .
H14 H 0.2122 0.2854 -0.1300 0.130 Uiso 1 1 calc R . .
C15 C 0.0940(3) 0.22168(18) -0.0869(2) 0.0785(9) Uani 1 1 d U . .
H15 H 0.1660 0.1974 -0.0481 0.094 Uiso 1 1 calc R . .
C16 C -0.0407(2) 0.20467(13) -0.09552(15) 0.0488(6) Uani 1 1 d U . .
C17 C -0.1422(3) 0.24337(13) -0.15365(17) 0.0538(6) Uani 1 1 d U . .
H17 H -0.2349 0.2340 -0.1611 0.065 Uiso 1 1 calc R . .
C18 C -0.1050(3) 0.29538(17) -0.2000(2) 0.0742(8) Uani 1 1 d U . .
H18 H -0.1750 0.3205 -0.2392 0.089 Uiso 1 1 calc R . .
C19 C 0.7893(2) 0.00361(10) 0.33441(15) 0.0385(5) Uani 1 1 d . . .
H19 H 0.7861 0.0470 0.3101 0.046 Uiso 1 1 calc R . .
C20 C 0.9162(2) -0.02368(11) 0.37692(16) 0.0416(5) Uani 1 1 d . . .
H20 H 0.9963 0.0009 0.3809 0.050 Uiso 1 1 calc R . .
C21 C 0.9236(2) -0.08812(10) 0.41373(14) 0.0361(5) Uani 1 1 d . . .
C22 C 0.8005(2) -0.12136(11) 0.40756(16) 0.0419(5) Uani 1 1 d . . .
H22 H 0.8009 -0.1642 0.4332 0.050 Uiso 1 1 calc R . .
C23 C 0.6780(2) -0.09055(10) 0.36327(15) 0.0375(5) Uani 1 1 d . . .
H23 H 0.5964 -0.1138 0.3590 0.045 Uiso 1 1 calc R . .
C24 C 1.2763(3) -0.08545(13) 0.28435(17) 0.0557(7) Uani 1 1 d . . .
H24 H 1.2744 -0.1020 0.2272 0.067 Uiso 1 1 calc R . .
C25 C 1.1904(3) -0.11504(13) 0.32852(17) 0.0568(7) Uani 1 1 d . . .
H25 H 1.1324 -0.1505 0.3016 0.068 Uiso 1 1 calc R . .
C26 C 1.1915(2) -0.09163(10) 0.41240(14) 0.0350(4) Uani 1 1 d . . .
C27 C 1.2809(3) -0.04011(12) 0.44939(14) 0.0469(6) Uani 1 1 d . . .
H27 H 1.2866 -0.0237 0.5072 0.056 Uiso 1 1 calc R . .
C28 C 1.3620(2) -0.01283(11) 0.40007(14) 0.0397(5) Uani 1 1 d . . .
H28 H 1.4204 0.0230 0.4255 0.048 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O3 2.0325(14) 2_645 ?
Ni1 O1 2.0627(13) . ?
Ni1 O6 2.0773(14) . ?
Ni1 N3 2.1083(18) . ?
Ni1 N4 2.1181(16) 1_455 ?
Ni1 N1 2.1313(18) . ?
S1 C16 1.764(3) . ?
S1 C11 1.783(2) . ?
S2 C21 1.773(2) . ?
S2 C26 1.784(2) . ?
O1 C7 1.262(2) . ?
O2 C7 1.255(2) . ?
O3 C8 1.258(2) . ?
O3 Ni1 2.0325(14) 2_655 ?
O4 C8 1.234(2) . ?
O5 C5 1.364(2) . ?
O5 H5 0.8200 . ?
O6 H1W 0.8200 . ?
O6 H2W 0.8361 . ?
N1 C13 1.331(3) . ?
N1 C9 1.336(3) . ?
N2 C18 1.321(4) . ?
N2 C14 1.336(4) . ?
N3 C19 1.338(3) . ?
N3 C23 1.340(2) . ?
N4 C28 1.320(2) . ?
N4 C24 1.328(3) . ?
N4 Ni1 2.1181(16) 1_655 ?
C1 C2 1.389(3) . ?
C1 C6 1.394(3) . ?
C1 C7 1.513(2) . ?
C2 C3 1.387(2) . ?
C2 H2 0.9300 . ?
C3 C4 1.387(3) . ?
C3 C8 1.506(3) . ?
C4 C5 1.383(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.389(3) . ?
C6 H6A 0.9300 . ?
C9 C10 1.376(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.372(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.378(4) . ?
C12 C13 1.382(3) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.361(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.373(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.380(3) . ?
C17 C18 1.360(4) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.372(3) . ?
C19 H19 0.9300 . ?
C20 C21 1.382(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.386(3) . ?
C22 C23 1.372(3) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.375(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.364(3) . ?
C25 H25 0.9300 . ?
C26 C27 1.369(3) . ?
C27 C28 1.376(3) . ?
C27 H27 0.9300 . ?
C28 H28 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
O3 Ni1 O1 173.84(5) 2_645 . ?
O3 Ni1 O6 93.63(6) 2_645 . ?
O1 Ni1 O6 90.23(6) . . ?
O3 Ni1 N3 85.46(6) 2_645 . ?
O1 Ni1 N3 89.93(6) . . ?
O6 Ni1 N3 87.36(7) . . ?
O3 Ni1 N4 86.46(6) 2_645 1_455 ?
O1 Ni1 N4 89.80(6) . 1_455 ?
O6 Ni1 N4 178.66(6) . 1_455 ?
N3 Ni1 N4 93.98(7) . 1_455 ?
O3 Ni1 N1 93.56(6) 2_645 . ?
O1 Ni1 N1 91.17(6) . . ?
O6 Ni1 N1 90.94(7) . . ?
N3 Ni1 N1 177.98(6) . . ?
N4 Ni1 N1 87.72(7) 1_455 . ?
C16 S1 C11 103.68(12) . . ?
C21 S2 C26 99.61(10) . . ?
C7 O1 Ni1 129.22(12) . . ?
C8 O3 Ni1 129.44(12) . 2_655 ?
C5 O5 H5 109.5 . . ?
Ni1 O6 H1W 109.5 . . ?
Ni1 O6 H2W 110.6 . . ?
H1W O6 H2W 110.8 . . ?
C13 N1 C9 117.1(2) . . ?
C13 N1 Ni1 121.61(15) . . ?
C9 N1 Ni1 121.28(15) . . ?
C18 N2 C14 115.3(3) . . ?
C19 N3 C23 116.55(18) . . ?
C19 N3 Ni1 121.36(13) . . ?
C23 N3 Ni1 121.44(14) . . ?
C28 N4 C24 116.47(17) . . ?
C28 N4 Ni1 123.50(13) . 1_655 ?
C24 N4 Ni1 119.98(14) . 1_655 ?
C2 C1 C6 119.49(16) . . ?
C2 C1 C7 120.40(15) . . ?
C6 C1 C7 120.11(16) . . ?
C3 C2 C1 120.12(16) . . ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 . . ?
C4 C3 C2 119.97(16) . . ?
C4 C3 C8 118.56(16) . . ?
C2 C3 C8 121.45(16) . . ?
C5 C4 C3 120.38(16) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
O5 C5 C4 121.97(16) . . ?
O5 C5 C6 118.40(16) . . ?
C4 C5 C6 119.63(17) . . ?
C5 C6 C1 120.33(17) . . ?
C5 C6 H6A 119.8 . . ?
C1 C6 H6A 119.8 . . ?
O2 C7 O1 124.67(16) . . ?
O2 C7 C1 118.95(15) . . ?
O1 C7 C1 116.38(15) . . ?
O4 C8 O3 125.21(18) . . ?
O4 C8 C3 118.48(17) . . ?
O3 C8 C3 116.22(16) . . ?
N1 C9 C10 123.8(2) . . ?
N1 C9 H9 118.1 . . ?
C10 C9 H9 118.1 . . ?
C11 C10 C9 118.6(2) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C10 C11 C12 118.3(2) . . ?
C10 C11 S1 118.7(2) . . ?
C12 C11 S1 122.9(2) . . ?
C11 C12 C13 119.4(2) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
N1 C13 C12 122.7(2) . . ?
N1 C13 H13 118.6 . . ?
C12 C13 H13 118.6 . . ?
N2 C14 C15 124.7(3) . . ?
N2 C14 H14 117.6 . . ?
C15 C14 H14 117.6 . . ?
C14 C15 C16 118.8(3) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?
C15 C16 C17 117.5(3) . . ?
C15 C16 S1 126.2(2) . . ?
C17 C16 S1 116.26(19) . . ?
C18 C17 C16 119.2(3) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
N2 C18 C17 124.6(3) . . ?
N2 C18 H18 117.7 . . ?
C17 C18 H18 117.7 . . ?
N3 C19 C20 123.83(19) . . ?
N3 C19 H19 118.1 . . ?
C20 C19 H19 118.1 . . ?
C19 C20 C21 119.16(19) . . ?
C19 C20 H20 120.4 . . ?
C21 C20 H20 120.4 . . ?
C20 C21 C22 117.61(19) . . ?
C20 C21 S2 123.73(16) . . ?
C22 C21 S2 118.63(16) . . ?
C23 C22 C21 119.42(19) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
N3 C23 C22 123.40(19) . . ?
N3 C23 H23 118.3 . . ?
C22 C23 H23 118.3 . . ?
N4 C24 C25 123.7(2) . . ?
N4 C24 H24 118.2 . . ?
C25 C24 H24 118.2 . . ?
C26 C25 C24 119.1(2) . . ?
C26 C25 H25 120.4 . . ?
C24 C25 H25 120.4 . . ?
C25 C26 C27 117.86(19) . . ?
C25 C26 S2 119.89(17) . . ?
C27 C26 S2 122.24(16) . . ?
C26 C27 C28 119.25(19) . . ?
C26 C27 H27 120.4 . . ?
C28 C27 H27 120.4 . . ?
N4 C28 C27 123.59(19) . . ?
N4 C28 H28 118.2 . . ?
C27 C28 H28 118.2 . . ?

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
O3 Ni1 O1 C7 163.0(5) 2_645 . . . ?
O6 Ni1 O1 C7 34.16(17) . . . . ?
N3 Ni1 O1 C7 121.52(17) . . . . ?
N4 Ni1 O1 C7 -144.50(17) 1_455 . . . ?
N1 Ni1 O1 C7 -56.78(17) . . . . ?
O3 Ni1 N1 C13 -40.41(17) 2_645 . . . ?
O1 Ni1 N1 C13 143.53(16) . . . . ?
O6 Ni1 N1 C13 53.28(17) . . . . ?
N3 Ni1 N1 C13 20.5(18) . . . . ?
N4 Ni1 N1 C13 -126.72(17) 1_455 . . . ?
O3 Ni1 N1 C9 142.10(17) 2_645 . . . ?
O1 Ni1 N1 C9 -33.96(18) . . . . ?
O6 Ni1 N1 C9 -124.21(18) . . . . ?
N3 Ni1 N1 C9 -157.0(17) . . . . ?
N4 Ni1 N1 C9 55.79(18) 1_455 . . . ?
O3 Ni1 N3 C19 121.79(16) 2_645 . . . ?
O1 Ni1 N3 C19 -62.30(16) . . . . ?
O6 Ni1 N3 C19 27.93(16) . . . . ?
N4 Ni1 N3 C19 -152.09(16) 1_455 . . . ?
N1 Ni1 N3 C19 60.8(18) . . . . ?
O3 Ni1 N3 C23 -48.58(15) 2_645 . . . ?
O1 Ni1 N3 C23 127.33(15) . . . . ?
O6 Ni1 N3 C23 -142.44(15) . . . . ?
N4 Ni1 N3 C23 37.54(15) 1_455 . . . ?
N1 Ni1 N3 C23 -109.6(17) . . . . ?
C6 C1 C2 C3 -1.1(3) . . . . ?
C7 C1 C2 C3 179.20(17) . . . . ?
C1 C2 C3 C4 -0.7(3) . . . . ?
C1 C2 C3 C8 178.44(18) . . . . ?
C2 C3 C4 C5 2.8(3) . . . . ?
C8 C3 C4 C5 -176.3(2) . . . . ?
C3 C4 C5 O5 177.6(2) . . . . ?
C3 C4 C5 C6 -3.2(3) . . . . ?
O5 C5 C6 C1 -179.33(19) . . . . ?
C4 C5 C6 C1 1.5(3) . . . . ?
C2 C1 C6 C5 0.6(3) . . . . ?
C7 C1 C6 C5 -179.62(18) . . . . ?
Ni1 O1 C7 O2 -10.1(3) . . . . ?
Ni1 O1 C7 C1 170.05(12) . . . . ?
C2 C1 C7 O2 5.0(3) . . . . ?
C6 C1 C7 O2 -174.71(19) . . . . ?
C2 C1 C7 O1 -175.08(17) . . . . ?
C6 C1 C7 O1 5.2(3) . . . . ?
Ni1 O3 C8 O4 -15.7(4) 2_655 . . . ?
Ni1 O3 C8 C3 167.70(13) 2_655 . . . ?
C4 C3 C8 O4 -16.3(3) . . . . ?
C2 C3 C8 O4 164.6(2) . . . . ?
C4 C3 C8 O3 160.6(2) . . . . ?
C2 C3 C8 O3 -18.5(3) . . . . ?
C13 N1 C9 C10 -1.1(4) . . . . ?
Ni1 N1 C9 C10 176.5(2) . . . . ?
N1 C9 C10 C11 -0.1(4) . . . . ?
C9 C10 C11 C12 1.5(4) . . . . ?
C9 C10 C11 S1 178.1(2) . . . . ?
C16 S1 C11 C10 109.2(2) . . . . ?
C16 S1 C11 C12 -74.4(2) . . . . ?
C10 C11 C12 C13 -1.8(4) . . . . ?
S1 C11 C12 C13 -178.22(19) . . . . ?
C9 N1 C13 C12 0.8(3) . . . . ?
Ni1 N1 C13 C12 -176.81(18) . . . . ?
C11 C12 C13 N1 0.7(4) . . . . ?
C18 N2 C14 C15 -0.4(7) . . . . ?
N2 C14 C15 C16 0.5(7) . . . . ?
C14 C15 C16 C17 -0.6(5) . . . . ?
C14 C15 C16 S1 -178.6(3) . . . . ?
C11 S1 C16 C15 1.0(3) . . . . ?
C11 S1 C16 C17 -177.07(19) . . . . ?
C15 C16 C17 C18 0.7(4) . . . . ?
S1 C16 C17 C18 178.9(2) . . . . ?
C14 N2 C18 C17 0.4(6) . . . . ?
C16 C17 C18 N2 -0.6(5) . . . . ?
C23 N3 C19 C20 1.3(3) . . . . ?
Ni1 N3 C19 C20 -169.54(17) . . . . ?
N3 C19 C20 C21 -0.1(3) . . . . ?
C19 C20 C21 C22 -1.6(3) . . . . ?
C19 C20 C21 S2 -179.70(17) . . . . ?
C26 S2 C21 C20 -30.1(2) . . . . ?
C26 S2 C21 C22 151.86(18) . . . . ?
C20 C21 C22 C23 2.1(3) . . . . ?
S2 C21 C22 C23 -179.71(17) . . . . ?
C19 N3 C23 C22 -0.7(3) . . . . ?
Ni1 N3 C23 C22 170.07(17) . . . . ?
C21 C22 C23 N3 -1.0(3) . . . . ?
C28 N4 C24 C25 0.4(4) . . . . ?
Ni1 N4 C24 C25 -177.2(2) 1_655 . . . ?
N4 C24 C25 C26 0.0(4) . . . . ?
C24 C25 C26 C27 -1.2(4) . . . . ?
C24 C25 C26 S2 179.8(2) . . . . ?
C21 S2 C26 C25 -79.3(2) . . . . ?
C21 S2 C26 C27 101.8(2) . . . . ?
C25 C26 C27 C28 2.0(4) . . . . ?
S2 C26 C27 C28 -179.05(18) . . . . ?
C24 N4 C28 C27 0.5(3) . . . . ?
Ni1 N4 C28 C27 178.01(18) 1_655 . . . ?
C26 C27 C28 N4 -1.7(4) . . . . ?

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 H2W O4 0.84 2.59 3.290(3) 141.4 4_565
O6 H2W O4 0.84 2.01 2.693(2) 138.3 2_645
O6 H1W O2 0.82 2.05 2.756(2) 143.4 .
O5 H5 O2 0.82 1.93 2.746(2) 177.5 4_566

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.044

# Attachment '4.cif'

data_e
_database_code_depnum_ccdc_archive 'CCDC 701848'

_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            'C44 H42N4 Ni2O9 S2'

_chemical_formula_weight         952.36

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   Cc

loop_

_symmetry_equiv_pos_as_xyz

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

_cell_length_a                   15.3099(10)

_cell_length_b                   27.9468(18)

_cell_length_c                   15.7112(10)

_cell_angle_alpha                90.00

_cell_angle_beta                 114.8620(10)

_cell_angle_gamma                90.00

_cell_volume                     6099.2(7)

_cell_formula_units_Z            4

_cell_measurement_temperature    291(2)

_cell_measurement_reflns_used    9065

_cell_measurement_theta_min      2.55

_cell_measurement_theta_max      25.92

_exptl_crystal_description       block

_exptl_crystal_colour            blue

_exptl_crystal_size_max          0.44

_exptl_crystal_size_mid          0.32

_exptl_crystal_size_min          0.31

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.037

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             1976

_exptl_absorpt_coefficient_mu    0.728

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.7380

_exptl_absorpt_correction_T_max  0.8078

_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;

?

;

_diffrn_ambient_temperature      291(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  'CCD area detector'

_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         0

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            22314

_diffrn_reflns_av_R_equivalents  0.0287

_diffrn_reflns_av_sigmaI/netI    0.0450

_diffrn_reflns_limit_h_min       -18

_diffrn_reflns_limit_h_max       18

_diffrn_reflns_limit_k_min       -33

_diffrn_reflns_limit_k_max       33

_diffrn_reflns_limit_l_min       -18

_diffrn_reflns_limit_l_max       19

_diffrn_reflns_theta_min         2.55

_diffrn_reflns_theta_max         25.50

_reflns_number_total             10908

_reflns_number_gt                10042

_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'

_computing_cell_refinement       'Bruker SMART'

_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics    'Bruker SHELXTL'

_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;

Refinement of F² against ALL reflections. The weighted R-factor wR and

goodness of fit S are based on F², conventional R-factors R are based

on F, with F set to zero for negative F². The threshold expression of

F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² are statistically about twice as large as those based on F, and R-

factors based on ALL data will be even larger.The carbon atoms of tert-butyl
groups have departed into two parts and their site occupation was
refined by programme. The restraints are needed to
restrict the large Ueq of tert-butyl groups.

;

_refine_ls_structure_factor_coef Fsqd

_refine_ls_matrix_type           full

_refine_ls_weighting_scheme      calc

_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1061P)²+2.3998P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct

_atom_sites_solution_secondary   difmap

_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    constr

_refine_ls_extinction_method     none

_refine_ls_extinction_coef       ?

_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'

_refine_ls_abs_structure_Flack   0.003(14)

_refine_ls_number_reflns         10908

_refine_ls_number_parameters     570

_refine_ls_number_restraints     237

_refine_ls_R_factor_all          0.0591

_refine_ls_R_factor_gt           0.0543

_refine_ls_wR_factor_ref         0.1506

_refine_ls_wR_factor_gt          0.1458

_refine_ls_goodness_of_fit_ref   1.067

_refine_ls_restrained_S_all      1.088

_refine_ls_shift/su_max          0.001

_refine_ls_shift/su_mean         0.000

loop_

_atom_site_label

_atom_site_type_symbol

_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z

_atom_site_U_iso_or_equiv

_atom_site_adp_type

_atom_site_occupancy

_atom_site_symmetry_multiplicity

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_assembly

_atom_site_disorder_group

C10 C 0.5395(16) 0.0090(8) 0.2055(14) 0.129(5) Uani 0.562(11) 1 d PDU A 1
H10A H 0.6053 -0.0009 0.2259 0.193 Uiso 0.562(11) 1 calc PR A 1
H10B H 0.5362 0.0433 0.2050 0.193 Uiso 0.562(11) 1 calc PR A 1
H10C H 0.5020 -0.0030 0.1435 0.193 Uiso 0.562(11) 1 calc PR A 1
C11 C 0.545(2) 0.0179(8) 0.3637(12) 0.179(6) Uani 0.562(11) 1 d PDU A 1
H11A H 0.6095 0.0065 0.4000 0.268 Uiso 0.562(11) 1 calc PR A 1
H11B H 0.5076 0.0140 0.3989 0.268 Uiso 0.562(11) 1 calc PR A 1
H11C H 0.5475 0.0511 0.3494 0.268 Uiso 0.562(11) 1 calc PR A 1
C12 C 0.535(2) -0.0620(5) 0.2953(17) 0.148(5) Uani 0.562(11) 1 d PDU A 1
H12A H 0.6036 -0.0623 0.3288 0.223 Uiso 0.562(11) 1 calc PR A 1
H12B H 0.5163 -0.0799 0.2382 0.223 Uiso 0.562(11) 1 calc PR A 1
H12C H 0.5065 -0.0763 0.3334 0.223 Uiso 0.562(11) 1 calc PR A 1
C10' C 0.544(2) 0.0376(7) 0.2697(19) 0.129(5) Uani 0.438(11) 1 d PDU A 2
H10D H 0.6070 0.0397 0.3210 0.193 Uiso 0.438(11) 1 calc PR A 2
H10E H 0.5041 0.0627 0.2748 0.193 Uiso 0.438(11) 1 calc PR A 2
H10F H 0.5504 0.0408 0.2115 0.193 Uiso 0.438(11) 1 calc PR A 2
C11' C 0.548(3) -0.0336(10) 0.3687(13) 0.179(6) Uani 0.438(11) 1 d PDU A 2
H11D H 0.5618 -0.0665 0.3622 0.268 Uiso 0.438(11) 1 calc PR A 2
H11E H 0.5051 -0.0318 0.3994 0.268 Uiso 0.438(11) 1 calc PR A 2
H11F H 0.6063 -0.0169 0.4055 0.268 Uiso 0.438(11) 1 calc PR A 2
C12' C 0.500(3) -0.0439(9) 0.1958(17) 0.148(5) Uani 0.438(11) 1 d PDU A 2
H12D H 0.5613 -0.0595 0.2168 0.223 Uiso 0.438(11) 1 calc PR A 2
H12E H 0.4885 -0.0256 0.1404 0.223 Uiso 0.438(11) 1 calc PR A 2
H12F H 0.4502 -0.0674 0.1819 0.223 Uiso 0.438(11) 1 calc PR A 2
C22 C -0.3487(8) 0.2690(4) -0.0686(5) 0.106(3) Uani 0.923(10) 1 d PDU B 1
H22A H -0.3263 0.3002 -0.0757 0.158 Uiso 0.923(10) 1 calc PR B 1
H22B H -0.2946 0.2482 -0.0378 0.158 Uiso 0.923(10) 1 calc PR B 1
H22C H -0.3850 0.2714 -0.0317 0.158 Uiso 0.923(10) 1 calc PR B 1
C23 C -0.4415(7) 0.1958(3) -0.1542(7) 0.109(3) Uani 0.923(10) 1 d PDU B 1
H23A H -0.4714 0.1955 -0.1114 0.163 Uiso 0.923(10) 1 calc PR B 1
H23B H -0.3846 0.1764 -0.1297 0.163 Uiso 0.923(10) 1 calc PR B 1
H23C H -0.4856 0.1834 -0.2138 0.163 Uiso 0.923(10) 1 calc PR B 1
C24 C -0.5044(6) 0.2787(4) -0.2146(7) 0.108(3) Uani 0.923(10) 1 d PDU B 1
H24A H -0.5394 0.2793 -0.1762 0.161 Uiso 0.923(10) 1 calc PR B 1
H24B H -0.5442 0.2652 -0.2746 0.161 Uiso 0.923(10) 1 calc PR B 1
H24C H -0.4866 0.3107 -0.2228 0.161 Uiso 0.923(10) 1 calc PR B 1
C22' C -0.3620(12) 0.2179(4) -0.0774(6) 0.106(3) Uani 0.077(10) 1 d PDU B 2
H22D H -0.2937 0.2199 -0.0576 0.158 Uiso 0.077(10) 1 calc PR B 2
H22E H -0.3822 0.1851 -0.0905 0.158 Uiso 0.077(10) 1 calc PR B 2
H22F H -0.3781 0.2297 -0.0284 0.158 Uiso 0.077(10) 1 calc PR B 2
C23' C -0.5145(6) 0.2272(4) -0.2190(13) 0.109(3) Uani 0.077(10) 1 d PDU B 2
H23D H -0.5560 0.2506 -0.2616 0.163 Uiso 0.077(10) 1 calc PR B 2
H23E H -0.5396 0.2183 -0.1746 0.163 Uiso 0.077(10) 1 calc PR B 2
H23F H -0.5112 0.1995 -0.2536 0.163 Uiso 0.077(10) 1 calc PR B 2
C24' C -0.4232(10) 0.2988(5) -0.1360(9) 0.108(3) Uani 0.077(10) 1 d PDU B 2
H24D H -0.4640 0.2985 -0.1033 0.161 Uiso 0.077(10) 1 calc PR B 2
H24E H -0.4510 0.3192 -0.1900 0.161 Uiso 0.077(10) 1 calc PR B 2
H24F H -0.3607 0.3107 -0.0950 0.161 Uiso 0.077(10) 1 calc PR B 2
Ni1 Ni -0.00008(4) 0.118199(18) -0.05227(4) 0.02424(14) Uani 1 1 d . . .
Ni2 Ni 0.21592(3) 0.140853(18) -0.07066(3) 0.02415(14) Uani 1 1 d . . .
S1 S 0.68448(9) 0.18504(5) 0.13051(10) 0.0451(3) Uani 1 1 d U . .
S2 S -0.23921(14) 0.07197(8) 0.20661(15) 0.0788(7) Uani 1 1 d U . .
O1 O 0.0988(2) 0.07122(13) 0.0347(2) 0.0382(8) Uani 1 1 d . . .
O2 O 0.2368(3) 0.08753(13) 0.0237(3) 0.0428(8) Uani 1 1 d . . .
O3 O 0.1035(3) -0.05758(16) 0.2638(3) 0.0581(12) Uani 1 1 d . . .
O4 O 0.2454(2) -0.09261(12) 0.3452(2) 0.0372(8) Uani 1 1 d . . .
O5 O -0.1114(2) 0.16299(13) -0.1362(2) 0.0392(8) Uani 1 1 d . . .
O6 O -0.0684(3) 0.18801(16) -0.2478(3) 0.0532(10) Uani 1 1 d . . .
O7 O -0.2944(2) 0.30844(12) -0.4817(2) 0.0356(7) Uani 1 1 d . . .
O8 O -0.4303(3) 0.32599(14) -0.4688(3) 0.0444(9) Uani 1 1 d . . .
O9 O 0.0677(2) 0.12709(11) -0.1431(2) 0.0277(6) Uani 1 1 d . . .
H9A H 0.0375 0.1534 -0.1856 0.042 Uiso 1 1 d R . .
H9B H 0.0586 0.0983 -0.1804 0.042 Uiso 1 1 d R . .
N1 N -0.0752(3) 0.10911(14) 0.0326(3) 0.0309(8) Uani 1 1 d . . .
N2 N -0.0758(3) -0.05875(14) 0.3682(3) 0.0344(9) Uani 1 1 d . . .
N3 N 0.3637(3) 0.15414(14) -0.0067(2) 0.0290(8) Uani 1 1 d . . .
N4 N 0.7020(3) 0.30503(14) 0.3326(3) 0.0334(8) Uani 1 1 d . . .
C1 C 0.1873(3) 0.06593(16) 0.0576(3) 0.0309(10) Uani 1 1 d . . .
C2 C 0.2381(4) 0.02982(18) 0.1334(4) 0.0393(11) Uani 1 1 d . . .
C3 C 0.1911(3) 0.00233(17) 0.1730(3) 0.0327(10) Uani 1 1 d . . .
H3 H 0.1251 0.0060 0.1535 0.039 Uiso 1 1 calc R . .
C4 C 0.2413(4) -0.03128(19) 0.2425(4) 0.0416(12) Uani 1 1 d . . .
C5 C 0.3408(5) -0.0352(3) 0.2695(6) 0.082(3) Uani 1 1 d . . .
H5 H 0.3747 -0.0576 0.3154 0.098 Uiso 1 1 calc R . .
C6 C 0.3898(5) -0.0089(4) 0.2335(7) 0.097(3) Uani 1 1 d U A .
C7 C 0.3376(4) 0.0251(3) 0.1651(6) 0.084(3) Uani 1 1 d . . .
H7 H 0.3700 0.0448 0.1404 0.101 Uiso 1 1 calc R . .
C8 C 0.1926(4) -0.06304(18) 0.2874(3) 0.0368(11) Uani 1 1 d . . .
C9 C 0.4998(7) -0.0107(4) 0.2724(8) 0.118(3) Uani 1 1 d DU . .
C13 C -0.1228(3) 0.18763(17) -0.2068(3) 0.0338(10) Uani 1 1 d . . .
C14 C -0.2131(4) 0.21826(19) -0.2445(4) 0.0406(11) Uani 1 1 d . . .
C15 C -0.2383(3) 0.24633(18) -0.3256(3) 0.0339(10) Uani 1 1 d . . .
H15 H -0.1991 0.2467 -0.3576 0.041 Uiso 1 1 calc R . .
C16 C -0.3209(4) 0.27307(19) -0.3573(4) 0.0380(11) Uani 1 1 d . . .
C17 C -0.3792(5) 0.2731(3) -0.3086(5) 0.0615(18) Uani 1 1 d . . .
H17 H -0.4352 0.2913 -0.3306 0.074 Uiso 1 1 calc R . .
C18 C -0.3543(5) 0.2471(3) -0.2303(5) 0.074(2) Uani 1 1 d D B .
C19 C -0.2708(5) 0.2199(3) -0.1967(5) 0.0647(19) Uani 1 1 d . . .
H19 H -0.2534 0.2026 -0.1415 0.078 Uiso 1 1 calc R . .
C20 C -0.3512(3) 0.30472(16) -0.4434(3) 0.0284(9) Uani 1 1 d . . .
C21 C -0.4138(5) 0.2483(2) -0.1669(5) 0.093(3) Uani 1 1 d D . .
C25 C -0.1713(4) 0.10771(19) -0.0065(4) 0.0400(11) Uani 1 1 d . . .
H25 H -0.2042 0.1156 -0.0696 0.048 Uiso 1 1 calc R . .
C26 C -0.2238(4) 0.09493(19) 0.0435(4) 0.0395(11) Uani 1 1 d . . .
H26 H -0.2906 0.0931 0.0143 0.047 Uiso 1 1 calc R . .
C27 C -0.1740(4) 0.0850(2) 0.1382(4) 0.0458(13) Uani 1 1 d . . .
C28 C -0.0765(5) 0.0885(3) 0.1782(4) 0.0571(16) Uani 1 1 d . . .
H28 H -0.0418 0.0828 0.2420 0.069 Uiso 1 1 calc R . .
C29 C -0.0295(4) 0.1004(2) 0.1234(3) 0.0423(11) Uani 1 1 d . . .
H29 H 0.0373 0.1025 0.1515 0.051 Uiso 1 1 calc R . .
C30 C -0.1744(4) 0.0204(2) 0.2682(4) 0.0506(14) Uani 1 1 d . . .
C31 C -0.1676(5) -0.0206(3) 0.2242(4) 0.0615(17) Uani 1 1 d . . .
H31 H -0.1964 -0.0223 0.1591 0.074 Uiso 1 1 calc R . .
C32 C -0.1187(4) -0.0590(2) 0.2753(4) 0.0485(13) Uani 1 1 d . . .
H32 H -0.1152 -0.0866 0.2438 0.058 Uiso 1 1 calc R . .
C33 C -0.0825(4) -0.01857(18) 0.4121(4) 0.0484(13) Uani 1 1 d . . .
H33 H -0.0528 -0.0179 0.4773 0.058 Uiso 1 1 calc R . .
C34 C -0.1314(5) 0.0217(2) 0.3652(5) 0.0617(17) Uani 1 1 d . . .
H34 H -0.1353 0.0489 0.3977 0.074 Uiso 1 1 calc R . .
C35 C 0.3958(3) 0.19829(17) 0.0165(3) 0.0357(10) Uani 1 1 d . . .
H35 H 0.3509 0.2228 0.0030 0.043 Uiso 1 1 calc R . .
C36 C 0.4920(4) 0.20996(19) 0.0595(4) 0.0383(11) Uani 1 1 d . . .
H36 H 0.5113 0.2416 0.0742 0.046 Uiso 1 1 calc R . .
C37 C 0.5594(4) 0.17367(18) 0.0805(3) 0.0340(10) Uani 1 1 d . . .
C38 C 0.5269(4) 0.12704(17) 0.0558(3) 0.0360(10) Uani 1 1 d . . .
H38 H 0.5701 0.1018 0.0680 0.043 Uiso 1 1 calc R . .
C39 C 0.4277(4) 0.11907(17) 0.0123(4) 0.0356(10) Uani 1 1 d . . .
H39 H 0.4056 0.0879 -0.0040 0.043 Uiso 1 1 calc R . .
C40 C 0.6904(3) 0.23220(18) 0.2093(3) 0.0367(11) Uani 1 1 d . . .
C41 C 0.7439(4) 0.2710(2) 0.2145(4) 0.0484(13) Uani 1 1 d . . .
H41 H 0.7779 0.2735 0.1776 0.058 Uiso 1 1 calc R . .
C42 C 0.7478(4) 0.3076(2) 0.2760(4) 0.0432(12) Uani 1 1 d . . .
H42 H 0.7834 0.3349 0.2781 0.052 Uiso 1 1 calc R . .
C43 C 0.6504(4) 0.26552(19) 0.3270(4) 0.0428(12) Uani 1 1 d . . .
H43 H 0.6175 0.2634 0.3650 0.051 Uiso 1 1 calc R . .
C44 C 0.6436(4) 0.2278(2) 0.2678(4) 0.0464(13) Uani 1 1 d . . .
H44 H 0.6088 0.2004 0.2671 0.056 Uiso 1 1 calc R . .


_geom_special_details            
;

All esds (except the esd in the dihedral angle between two l.s. planes)

are estimated using the full covariance matrix. The cell esds are taken

into account individually in the estimation of esds in distances, angles

and torsion angles; correlations between esds in cell parameters are only

used when they are defined by crystal symmetry. An approximate (isotropic)

treatment of cell esds is used for estimating esds involving l.s. planes.

;

loop_

_geom_bond_atom_site_label_1

_geom_bond_atom_site_label_2

_geom_bond_distance

_geom_bond_site_symmetry_2

_geom_bond_publ_flag

C10 C9 1.521(9) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C9 1.530(10) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C9 1.520(10) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C10' C9 1.522(10) . ?
C10' H10D 0.9600 . ?
C10' H10E 0.9600 . ?
C10' H10F 0.9600 . ?
C11' C9 1.517(10) . ?
C11' H11D 0.9600 . ?
C11' H11E 0.9600 . ?
C11' H11F 0.9600 . ?
C12' C9 1.519(10) . ?
C12' H12D 0.9600 . ?
C12' H12E 0.9600 . ?
C12' H12F 0.9600 . ?
C22 C21 1.555(8) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C21 1.563(7) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 C21 1.527(7) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C22' C21 1.547(9) . ?
C22' H22D 0.9600 . ?
C22' H22E 0.9600 . ?
C22' H22F 0.9600 . ?
C23' C21 1.527(9) . ?
C23' H23D 0.9600 . ?
C23' H23E 0.9600 . ?
C23' H23F 0.9600 . ?
C24' C21 1.519(9) . ?
C24' H24D 0.9600 . ?
C24' H24E 0.9600 . ?
C24' H24F 0.9600 . ?
Ni1 O8 2.029(3) 4 ?
Ni1 O1 2.035(3) . ?
Ni1 O5 2.078(3) . ?
Ni1 O9 2.103(3) . ?
Ni1 N2 2.109(4) 2_554 ?
Ni1 N1 2.110(4) . ?
Ni2 O2 2.030(3) . ?
Ni2 O7 2.043(3) 4 ?
Ni2 O4 2.066(3) 2_554 ?
Ni2 N3 2.087(4) . ?
Ni2 N4 2.091(4) 4_454 ?
Ni2 O9 2.102(3) . ?
S1 C37 1.766(5) . ?
S1 C40 1.784(5) . ?
S2 C27 1.785(5) . ?
S2 C30 1.787(5) . ?
O1 C1 1.256(6) . ?
O2 C1 1.250(6) . ?
O3 C8 1.264(6) . ?
O4 C8 1.243(6) . ?
O4 Ni2 2.066(3) 2 ?
O5 C13 1.254(6) . ?
O6 C13 1.249(6) . ?
O7 C20 1.251(5) . ?
O7 Ni2 2.043(3) 4_454 ?
O8 C20 1.254(6) . ?
O8 Ni1 2.029(3) 4_454 ?
O9 H9A 0.9700 . ?
O9 H9B 0.9700 . ?
N1 C29 1.321(6) . ?
N1 C25 1.336(7) . ?
N2 C32 1.324(7) . ?
N2 C33 1.345(7) . ?
N2 Ni1 2.109(4) 2 ?
N3 C35 1.321(6) . ?
N3 C39 1.328(6) . ?
N4 C43 1.340(7) . ?
N4 C42 1.346(7) . ?
N4 Ni2 2.091(4) 4 ?
C1 C2 1.503(6) . ?
C2 C3 1.368(7) . ?
C2 C7 1.396(8) . ?
C3 C4 1.400(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.403(8) . ?
C4 C8 1.511(7) . ?
C5 C6 1.335(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.405(9) . ?
C6 C9 1.532(11) . ?
C7 H7 0.9300 . ?
C13 C14 1.519(7) . ?
C14 C19 1.379(8) . ?
C14 C15 1.406(6) . ?
C15 C16 1.369(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.398(7) . ?
C16 C20 1.517(6) . ?
C17 C18 1.341(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.387(9) . ?
C18 C21 1.608(9) . ?
C19 H19 0.9300 . ?
C25 C26 1.388(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.384(8) . ?
C26 H26 0.9300 . ?
C27 C28 1.359(9) . ?
C28 C29 1.374(8) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 C31 1.364(10) . ?
C30 C34 1.383(9) . ?
C31 C32 1.360(9) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 C34 1.381(8) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 C36 1.377(7) . ?
C35 H35 0.9300 . ?
C36 C37 1.384(7) . ?
C36 H36 0.9300 . ?
C37 C38 1.391(7) . ?
C38 C39 1.396(7) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C40 C41 1.341(7) . ?
C40 C44 1.389(8) . ?
C41 C42 1.389(8) . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?
C43 C44 1.380(7) . ?
C43 H43 0.9300 . ?
C44 H44 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

C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C10' H10D 109.5 . . ?
C9 C10' H10E 109.5 . . ?
H10D C10' H10E 109.5 . . ?
C9 C10' H10F 109.5 . . ?
H10D C10' H10F 109.5 . . ?
H10E C10' H10F 109.5 . . ?
C9 C11' H11D 109.5 . . ?
C9 C11' H11E 109.5 . . ?
H11D C11' H11E 109.5 . . ?
C9 C11' H11F 109.5 . . ?
H11D C11' H11F 109.5 . . ?
H11E C11' H11F 109.5 . . ?
C9 C12' H12D 109.5 . . ?
C9 C12' H12E 109.5 . . ?
H12D C12' H12E 109.5 . . ?
C9 C12' H12F 109.5 . . ?
H12D C12' H12F 109.5 . . ?
H12E C12' H12F 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C22' H22D 109.5 . . ?
C21 C22' H22E 109.5 . . ?
H22D C22' H22E 109.5 . . ?
C21 C22' H22F 109.5 . . ?
H22D C22' H22F 109.5 . . ?
H22E C22' H22F 109.5 . . ?
C21 C23' H23D 109.5 . . ?
C21 C23' H23E 109.5 . . ?
H23D C23' H23E 109.5 . . ?
C21 C23' H23F 109.5 . . ?
H23D C23' H23F 109.5 . . ?
H23E C23' H23F 109.5 . . ?
C21 C24' H24D 109.5 . . ?
C21 C24' H24E 109.5 . . ?
H24D C24' H24E 109.5 . . ?
C21 C24' H24F 109.5 . . ?
H24D C24' H24F 109.5 . . ?
H24E C24' H24F 109.5 . . ?
O8 Ni1 O1 91.21(16) 4 . ?
O8 Ni1 O5 90.90(16) 4 . ?
O1 Ni1 O5 173.90(14) . . ?
O8 Ni1 O9 94.09(13) 4 . ?
O1 Ni1 O9 95.25(13) . . ?
O5 Ni1 O9 90.31(13) . . ?
O8 Ni1 N2 176.05(16) 4 2_554 ?
O1 Ni1 N2 87.58(16) . 2_554 ?
O5 Ni1 N2 89.94(15) . 2_554 ?
O9 Ni1 N2 89.77(14) . 2_554 ?
O8 Ni1 N1 87.90(15) 4 . ?
O1 Ni1 N1 86.99(14) . . ?
O5 Ni1 N1 87.37(14) . . ?
O9 Ni1 N1 176.96(15) . . ?
N2 Ni1 N1 88.28(16) 2_554 . ?
O2 Ni2 O7 92.48(16) . 4 ?
O2 Ni2 O4 88.76(15) . 2_554 ?
O7 Ni2 O4 172.25(13) 4 2_554 ?
O2 Ni2 N3 88.46(14) . . ?
O7 Ni2 N3 85.85(14) 4 . ?
O4 Ni2 N3 86.54(14) 2_554 . ?
O2 Ni2 N4 176.82(16) . 4_454 ?
O7 Ni2 N4 88.98(14) 4 4_454 ?
O4 Ni2 N4 89.41(16) 2_554 4_454 ?
N3 Ni2 N4 88.83(15) . 4_454 ?
O2 Ni2 O9 93.65(13) . . ?
O7 Ni2 O9 96.94(13) 4 . ?
O4 Ni2 O9 90.62(13) 2_554 . ?
N3 Ni2 O9 176.42(13) . . ?
N4 Ni2 O9 88.98(14) 4_454 . ?
C37 S1 C40 99.8(2) . . ?
C27 S2 C30 99.6(2) . . ?
C1 O1 Ni1 132.6(3) . . ?
C1 O2 Ni2 136.8(3) . . ?
C8 O4 Ni2 130.6(3) . 2 ?
C13 O5 Ni1 131.6(3) . . ?
C20 O7 Ni2 131.0(3) . 4_454 ?
C20 O8 Ni1 138.2(3) . 4_454 ?
Ni1 O9 Ni2 112.50(14) . . ?
Ni1 O9 H9A 109.1 . . ?
Ni2 O9 H9A 109.2 . . ?
Ni1 O9 H9B 109.0 . . ?
Ni2 O9 H9B 109.1 . . ?
H9A O9 H9B 107.9 . . ?
C29 N1 C25 118.2(4) . . ?
C29 N1 Ni1 121.5(3) . . ?
C25 N1 Ni1 120.0(3) . . ?
C32 N2 C33 117.4(5) . . ?
C32 N2 Ni1 122.9(4) . 2 ?
C33 N2 Ni1 119.7(3) . 2 ?
C35 N3 C39 118.3(4) . . ?
C35 N3 Ni2 120.1(3) . . ?
C39 N3 Ni2 121.7(3) . . ?
C43 N4 C42 117.2(4) . . ?
C43 N4 Ni2 121.4(3) . 4 ?
C42 N4 Ni2 121.3(3) . 4 ?
O2 C1 O1 126.5(4) . . ?
O2 C1 C2 117.2(4) . . ?
O1 C1 C2 116.2(4) . . ?
C3 C2 C7 119.2(5) . . ?
C3 C2 C1 122.8(4) . . ?
C7 C2 C1 118.0(5) . . ?
C2 C3 C4 120.7(4) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 117.3(5) . . ?
C5 C4 C8 119.9(5) . . ?
C3 C4 C8 122.8(4) . . ?
C6 C5 C4 124.2(6) . . ?
C6 C5 H5 117.9 . . ?
C4 C5 H5 117.9 . . ?
C5 C6 C7 117.1(6) . . ?
C5 C6 C9 122.2(6) . . ?
C7 C6 C9 120.3(6) . . ?
C2 C7 C6 121.5(6) . . ?
C2 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
O4 C8 O3 125.8(4) . . ?
O4 C8 C4 115.8(4) . . ?
O3 C8 C4 118.4(4) . . ?
C11' C9 C10 132.5(19) . . ?
C11' C9 C6 113.7(17) . . ?
C10 C9 C6 113.8(11) . . ?
C11' C9 C10' 111.5(10) . . ?
C10 C9 C10' 49.0(11) . . ?
C6 C9 C10' 113.0(13) . . ?
C11' C9 C12 52.6(12) . . ?
C10 C9 C12 107.6(9) . . ?
C6 C9 C12 110.1(13) . . ?
C10' C9 C12 136.5(16) . . ?
C11' C9 C12' 111.9(10) . . ?
C10 C9 C12' 62.6(11) . . ?
C6 C9 C12' 94.1(15) . . ?
C10' C9 C12' 111.6(10) . . ?
C12 C9 C12' 59.6(11) . . ?
C11' C9 C11 56.4(11) . . ?
C10 C9 C11 107.5(9) . . ?
C6 C9 C11 110.4(15) . . ?
C10' C9 C11 61.9(11) . . ?
C12 C9 C11 107.2(9) . . ?
C12' C9 C11 155.4(19) . . ?
O6 C13 O5 125.9(4) . . ?
O6 C13 C14 119.3(4) . . ?
O5 C13 C14 114.8(4) . . ?
C19 C14 C15 118.8(5) . . ?
C19 C14 C13 119.5(4) . . ?
C15 C14 C13 121.7(4) . . ?
C16 C15 C14 119.5(4) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C15 C16 C17 120.5(5) . . ?
C15 C16 C20 122.1(4) . . ?
C17 C16 C20 117.4(4) . . ?
C18 C17 C16 120.1(5) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 120.4(5) . . ?
C17 C18 C21 122.7(5) . . ?
C19 C18 C21 116.7(5) . . ?
C14 C19 C18 120.7(5) . . ?
C14 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
O7 C20 O8 125.5(4) . . ?
O7 C20 C16 117.6(4) . . ?
O8 C20 C16 116.9(4) . . ?
C24' C21 C23' 108.7(8) . . ?
C24' C21 C24 56.8(3) . . ?
C23' C21 C24 56.5(3) . . ?
C24' C21 C22' 107.5(8) . . ?
C23' C21 C22' 106.9(7) . . ?
C24 C21 C22' 139.8(9) . . ?
C24' C21 C22 56.3(3) . . ?
C23' C21 C22 139.2(9) . . ?
C24 C21 C22 110.6(5) . . ?
C22' C21 C22 55.4(3) . . ?
C24' C21 C23 139.8(10) . . ?
C23' C21 C23 55.9(3) . . ?
C24 C21 C23 110.2(5) . . ?
C22' C21 C23 55.3(3) . . ?
C22 C21 C23 108.5(5) . . ?
C24' C21 C18 111.9(8) . . ?
C23' C21 C18 111.5(8) . . ?
C24 C21 C18 110.0(5) . . ?
C22' C21 C18 110.1(7) . . ?
C22 C21 C18 109.2(5) . . ?
C23 C21 C18 108.2(5) . . ?
N1 C25 C26 122.4(5) . . ?
N1 C25 H25 118.8 . . ?
C26 C25 H25 118.8 . . ?
C27 C26 C25 118.1(5) . . ?
C27 C26 H26 120.9 . . ?
C25 C26 H26 120.9 . . ?
C28 C27 C26 119.0(5) . . ?
C28 C27 S2 121.4(4) . . ?
C26 C27 S2 119.5(4) . . ?
C27 C28 C29 119.4(5) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 H28 120.3 . . ?
N1 C29 C28 122.8(5) . . ?
N1 C29 H29 118.6 . . ?
C28 C29 H29 118.6 . . ?
C31 C30 C34 118.6(5) . . ?
C31 C30 S2 123.1(5) . . ?
C34 C30 S2 118.3(5) . . ?
C30 C31 C32 120.2(6) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
N2 C32 C31 122.8(6) . . ?
N2 C32 H32 118.6 . . ?
C31 C32 H32 118.6 . . ?
N2 C33 C34 123.2(5) . . ?
N2 C33 H33 118.4 . . ?
C34 C33 H33 118.4 . . ?
C33 C34 C30 117.8(6) . . ?
C33 C34 H34 121.1 . . ?
C30 C34 H34 121.1 . . ?
N3 C35 C36 123.6(4) . . ?
N3 C35 H35 118.2 . . ?
C36 C35 H35 118.2 . . ?
C35 C36 C37 118.7(5) . . ?
C35 C36 H36 120.7 . . ?
C37 C36 H36 120.7 . . ?
C36 C37 C38 118.4(5) . . ?
C36 C37 S1 122.3(4) . . ?
C38 C37 S1 119.1(4) . . ?
C37 C38 C39 118.3(5) . . ?
C37 C38 H38 120.8 . . ?
C39 C38 H38 120.8 . . ?
N3 C39 C38 122.7(4) . . ?
N3 C39 H39 118.7 . . ?
C38 C39 H39 118.7 . . ?
C41 C40 C44 120.2(5) . . ?
C41 C40 S1 119.5(4) . . ?
C44 C40 S1 120.3(4) . . ?
C40 C41 C42 119.0(5) . . ?
C40 C41 H41 120.5 . . ?
C42 C41 H41 120.5 . . ?
N4 C42 C41 122.5(5) . . ?
N4 C42 H42 118.7 . . ?
C41 C42 H42 118.7 . . ?
N4 C43 C44 123.3(5) . . ?
N4 C43 H43 118.4 . . ?
C44 C43 H43 118.4 . . ?
C43 C44 C40 117.7(5) . . ?
C43 C44 H44 121.1 . . ?
C40 C44 H44 121.1 . . ?

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

O8 Ni1 O1 C1 -64.1(5) 4 . . . ?
O5 Ni1 O1 C1 -174.3(13) . . . . ?
O9 Ni1 O1 C1 30.1(5) . . . . ?
N2 Ni1 O1 C1 119.6(5) 2_554 . . . ?
N1 Ni1 O1 C1 -152.0(5) . . . . ?
O7 Ni2 O2 C1 70.9(5) 4 . . . ?
O4 Ni2 O2 C1 -116.7(5) 2_554 . . . ?
N3 Ni2 O2 C1 156.7(5) . . . . ?
N4 Ni2 O2 C1 -172(3) 4_454 . . . ?
O9 Ni2 O2 C1 -26.2(5) . . . . ?
O8 Ni1 O5 C13 88.4(5) 4 . . . ?
O1 Ni1 O5 C13 -161.4(13) . . . . ?
O9 Ni1 O5 C13 -5.7(5) . . . . ?
N2 Ni1 O5 C13 -95.5(5) 2_554 . . . ?
N1 Ni1 O5 C13 176.2(5) . . . . ?
O8 Ni1 O9 Ni2 43.06(18) 4 . . . ?
O1 Ni1 O9 Ni2 -48.54(17) . . . . ?
O5 Ni1 O9 Ni2 133.98(17) . . . . ?
N2 Ni1 O9 Ni2 -136.09(17) 2_554 . . . ?
N1 Ni1 O9 Ni2 174(26) . . . . ?
O2 Ni2 O9 Ni1 46.43(18) . . . . ?
O7 Ni2 O9 Ni1 -46.52(17) 4 . . . ?
O4 Ni2 O9 Ni1 135.23(16) 2_554 . . . ?
N3 Ni2 O9 Ni1 173(2) . . . . ?
N4 Ni2 O9 Ni1 -135.37(17) 4_454 . . . ?
O8 Ni1 N1 C29 -59.4(4) 4 . . . ?
O1 Ni1 N1 C29 31.9(4) . . . . ?
O5 Ni1 N1 C29 -150.4(4) . . . . ?
O9 Ni1 N1 C29 170(3) . . . . ?
N2 Ni1 N1 C29 119.6(4) 2_554 . . . ?
O8 Ni1 N1 C25 126.7(4) 4 . . . ?
O1 Ni1 N1 C25 -141.9(4) . . . . ?
O5 Ni1 N1 C25 35.7(4) . . . . ?
O9 Ni1 N1 C25 -4(3) . . . . ?
N2 Ni1 N1 C25 -54.3(4) 2_554 . . . ?
O2 Ni2 N3 C35 -131.3(4) . . . . ?
O7 Ni2 N3 C35 -38.7(4) 4 . . . ?
O4 Ni2 N3 C35 139.8(4) 2_554 . . . ?
N4 Ni2 N3 C35 50.3(4) 4_454 . . . ?
O9 Ni2 N3 C35 102(2) . . . . ?
O2 Ni2 N3 C39 48.2(4) . . . . ?
O7 Ni2 N3 C39 140.8(4) 4 . . . ?
O4 Ni2 N3 C39 -40.6(4) 2_554 . . . ?
N4 Ni2 N3 C39 -130.1(4) 4_454 . . . ?
O9 Ni2 N3 C39 -78(2) . . . . ?
Ni2 O2 C1 O1 4.4(9) . . . . ?
Ni2 O2 C1 C2 -175.7(4) . . . . ?
Ni1 O1 C1 O2 -6.8(8) . . . . ?
Ni1 O1 C1 C2 173.4(3) . . . . ?
O2 C1 C2 C3 -176.9(5) . . . . ?
O1 C1 C2 C3 2.9(7) . . . . ?
O2 C1 C2 C7 4.1(8) . . . . ?
O1 C1 C2 C7 -176.0(6) . . . . ?
C7 C2 C3 C4 -1.9(9) . . . . ?
C1 C2 C3 C4 179.2(5) . . . . ?
C2 C3 C4 C5 0.2(9) . . . . ?
C2 C3 C4 C8 -179.0(5) . . . . ?
C3 C4 C5 C6 0.4(14) . . . . ?
C8 C4 C5 C6 179.6(10) . . . . ?
C4 C5 C6 C7 0.8(18) . . . . ?
C4 C5 C6 C9 173.3(10) . . . . ?
C3 C2 C7 C6 3.1(13) . . . . ?
C1 C2 C7 C6 -177.9(9) . . . . ?
C5 C6 C7 C2 -2.5(17) . . . . ?
C9 C6 C7 C2 -175.2(10) . . . . ?
Ni2 O4 C8 O3 -3.6(8) 2 . . . ?
Ni2 O4 C8 C4 176.5(3) 2 . . . ?
C5 C4 C8 O4 -2.2(9) . . . . ?
C3 C4 C8 O4 177.0(5) . . . . ?
C5 C4 C8 O3 177.8(7) . . . . ?
C3 C4 C8 O3 -3.0(8) . . . . ?
C5 C6 C9 C11' -15.7(18) . . . . ?
C7 C6 C9 C11' 156.6(15) . . . . ?
C5 C6 C9 C10 162.1(13) . . . . ?
C7 C6 C9 C10 -25.6(16) . . . . ?
C5 C6 C9 C10' -144.2(15) . . . . ?
C7 C6 C9 C10' 28.2(17) . . . . ?
C5 C6 C9 C12 41.2(17) . . . . ?
C7 C6 C9 C12 -146.5(12) . . . . ?
C5 C6 C9 C12' 100.3(15) . . . . ?
C7 C6 C9 C12' -87.4(15) . . . . ?
C5 C6 C9 C11 -76.9(16) . . . . ?
C7 C6 C9 C11 95.4(13) . . . . ?
Ni1 O5 C13 O6 5.2(8) . . . . ?
Ni1 O5 C13 C14 -176.3(3) . . . . ?
O6 C13 C14 C19 -176.7(6) . . . . ?
O5 C13 C14 C19 4.7(8) . . . . ?
O6 C13 C14 C15 1.4(8) . . . . ?
O5 C13 C14 C15 -177.2(5) . . . . ?
C19 C14 C15 C16 -2.4(9) . . . . ?
C13 C14 C15 C16 179.5(5) . . . . ?
C14 C15 C16 C17 1.0(9) . . . . ?
C14 C15 C16 C20 179.0(5) . . . . ?
C15 C16 C17 C18 0.2(11) . . . . ?
C20 C16 C17 C18 -177.9(7) . . . . ?
C16 C17 C18 C19 0.1(13) . . . . ?
C16 C17 C18 C21 175.6(6) . . . . ?
C15 C14 C19 C18 2.7(11) . . . . ?
C13 C14 C19 C18 -179.2(7) . . . . ?
C17 C18 C19 C14 -1.6(13) . . . . ?
C21 C18 C19 C14 -177.4(6) . . . . ?
Ni2 O7 C20 O8 18.1(7) 4_454 . . . ?
Ni2 O7 C20 C16 -159.9(3) 4_454 . . . ?
Ni1 O8 C20 O7 -15.1(8) 4_454 . . . ?
Ni1 O8 C20 C16 162.9(4) 4_454 . . . ?
C15 C16 C20 O7 -5.0(7) . . . . ?
C17 C16 C20 O7 173.1(5) . . . . ?
C15 C16 C20 O8 176.8(5) . . . . ?
C17 C16 C20 O8 -5.1(8) . . . . ?
C17 C18 C21 C24' -55.5(9) . . . . ?
C19 C18 C21 C24' 120.1(8) . . . . ?
C17 C18 C21 C23' 66.4(9) . . . . ?
C19 C18 C21 C23' -117.9(8) . . . . ?
C17 C18 C21 C24 5.6(10) . . . . ?
C19 C18 C21 C24 -178.7(7) . . . . ?
C17 C18 C21 C22' -175.1(8) . . . . ?
C19 C18 C21 C22' 0.6(9) . . . . ?
C17 C18 C21 C22 -116.0(8) . . . . ?
C19 C18 C21 C22 59.7(8) . . . . ?
C17 C18 C21 C23 126.1(8) . . . . ?
C19 C18 C21 C23 -58.2(8) . . . . ?
C29 N1 C25 C26 -3.7(8) . . . . ?
Ni1 N1 C25 C26 170.4(4) . . . . ?
N1 C25 C26 C27 2.3(8) . . . . ?
C25 C26 C27 C28 0.5(9) . . . . ?
C25 C26 C27 S2 176.2(4) . . . . ?
C30 S2 C27 C28 -50.9(6) . . . . ?
C30 S2 C27 C26 133.5(5) . . . . ?
C26 C27 C28 C29 -1.8(9) . . . . ?
S2 C27 C28 C29 -177.4(5) . . . . ?
C25 N1 C29 C28 2.3(8) . . . . ?
Ni1 N1 C29 C28 -171.7(5) . . . . ?
C27 C28 C29 N1 0.4(10) . . . . ?
C27 S2 C30 C31 -60.4(6) . . . . ?
C27 S2 C30 C34 121.3(5) . . . . ?
C34 C30 C31 C32 -0.4(10) . . . . ?
S2 C30 C31 C32 -178.7(5) . . . . ?
C33 N2 C32 C31 0.5(9) . . . . ?
Ni1 N2 C32 C31 179.9(5) 2 . . . ?
C30 C31 C32 N2 -0.3(10) . . . . ?
C32 N2 C33 C34 -0.1(9) . . . . ?
Ni1 N2 C33 C34 -179.4(5) 2 . . . ?
N2 C33 C34 C30 -0.6(10) . . . . ?
C31 C30 C34 C33 0.9(9) . . . . ?
S2 C30 C34 C33 179.2(5) . . . . ?
C39 N3 C35 C36 -0.1(7) . . . . ?
Ni2 N3 C35 C36 179.4(4) . . . . ?
N3 C35 C36 C37 -0.5(8) . . . . ?
C35 C36 C37 C38 1.0(7) . . . . ?
C35 C36 C37 S1 176.9(4) . . . . ?
C40 S1 C37 C36 38.5(5) . . . . ?
C40 S1 C37 C38 -145.6(4) . . . . ?
C36 C37 C38 C39 -1.0(7) . . . . ?
S1 C37 C38 C39 -177.0(4) . . . . ?
C35 N3 C39 C38 0.2(7) . . . . ?
Ni2 N3 C39 C38 -179.4(4) . . . . ?
C37 C38 C39 N3 0.4(8) . . . . ?
C37 S1 C40 C41 -135.2(5) . . . . ?
C37 S1 C40 C44 47.7(5) . . . . ?
C44 C40 C41 C42 -3.0(9) . . . . ?
S1 C40 C41 C42 179.9(5) . . . . ?
C43 N4 C42 C41 -0.8(8) . . . . ?
Ni2 N4 C42 C41 176.6(5) 4 . . . ?
C40 C41 C42 N4 1.9(9) . . . . ?
C42 N4 C43 C44 1.0(8) . . . . ?
Ni2 N4 C43 C44 -176.4(4) 4 . . . ?
N4 C43 C44 C40 -2.1(9) . . . . ?
C41 C40 C44 C43 3.1(8) . . . . ?
S1 C40 C44 C43 -179.8(4) . . . . ?

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

O9 H9A O6 0.97 1.78 2.658(5) 148.1 .
O9 H9B O3 0.97 1.74 2.624(5) 149.1 2_554

_diffrn_measured_fraction_theta_max 0.991

_diffrn_reflns_theta_full        25.50

_diffrn_measured_fraction_theta_full 0.991

_refine_diff_density_max         0.985

_refine_diff_density_min         -0.508

_refine_diff_density_rms         0.098


