# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Tatsuya Nabeshima'
_publ_contact_author_email       NABESIMA@CHEM.TSUKUBA.AC.JP

_publ_section_title              
;
Highly efficient regulation of cation recognition
and promotion of self-assembly by metalation of macrocyclic bis(N2O2)
ligand with nickel(II)
;
loop_
_publ_author_name
'Tatsuya Nabeshima'
'Shigehisa Akine'
'Fumihiko Utsuno'

# Attachment 'nabeshima_1.cif'

data_uts111
_database_code_depnum_ccdc_archive 'CCDC 743175'
#TrackingRef 'nabeshima_1.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            'H4L 2MeCN'
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H28 N4 O6, 2(C2 H3 N)'
_chemical_formula_sum            'C44 H34 N6 O6'
_chemical_formula_weight         742.77

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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   21.7674(9)
_cell_length_b                   8.3961(4)
_cell_length_c                   20.4083(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3729.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120
_cell_measurement_reflns_used    34359
_cell_measurement_theta_min      3.22
_cell_measurement_theta_max      27.46

_exptl_crystal_description       prismatic
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9649
_exptl_absorpt_correction_T_max  0.9911
_exptl_absorpt_process_details   'Rapid AUTO (Rigaku Corp.)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS Rapid'
_diffrn_measurement_method       IP
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            34359
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         27.46
_reflns_number_total             4248
_reflns_number_gt                3681
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rapid AUTO (Rigaku Corp.)'
_computing_cell_refinement       'Rapid AUTO (Rigaku Corp.)'
_computing_data_reduction        'Rapid AUTO (Rigaku Corp.)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  ORTEP-3

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+1.4171P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4248
_refine_ls_number_parameters     276
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1425
_refine_ls_wR_factor_gt          0.1376
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_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
C1 C 0.36920(6) 0.76979(18) 0.36908(8) 0.0333(3) Uani 1 1 d . . .
C2 C 0.34533(6) 0.70721(17) 0.31072(7) 0.0311(3) Uani 1 1 d . . .
C3 C 0.28402(6) 0.74408(17) 0.29334(7) 0.0308(3) Uani 1 1 d . . .
C4 C 0.24928(7) 0.84536(19) 0.33360(7) 0.0363(3) Uani 1 1 d . . .
H1 H 0.2080 0.8692 0.3222 0.044 Uiso 1 1 calc R . .
C5 C 0.27444(7) 0.9106(2) 0.38952(8) 0.0395(4) Uani 1 1 d . . .
H2 H 0.2509 0.9812 0.4159 0.047 Uiso 1 1 calc R . .
C6 C 0.33474(7) 0.8723(2) 0.40720(8) 0.0368(3) Uani 1 1 d . . .
H3 H 0.3521 0.9171 0.4457 0.044 Uiso 1 1 calc R . .
O1 O 0.38099(4) 0.61301(14) 0.27358(5) 0.0365(3) Uani 1 1 d . . .
H4 H 0.3617 0.5861 0.2397 0.055 Uiso 1 1 calc R . .
C7 C 0.25640(6) 0.67679(18) 0.23477(7) 0.0318(3) Uani 1 1 d . . .
H5 H 0.2152 0.7029 0.2239 0.038 Uiso 1 1 calc R . .
N1 N 0.28695(5) 0.58244(15) 0.19748(6) 0.0303(3) Uani 1 1 d . . .
C8 C 0.25917(6) 0.50876(17) 0.14258(7) 0.0298(3) Uani 1 1 d . . .
C9 C 0.19581(6) 0.48535(19) 0.13660(8) 0.0361(3) Uani 1 1 d . . .
H6 H 0.1689 0.5252 0.1693 0.043 Uiso 1 1 calc R . .
C10 C 0.17199(7) 0.4038(2) 0.08286(9) 0.0404(4) Uani 1 1 d . . .
H7 H 0.1289 0.3898 0.0787 0.048 Uiso 1 1 calc R . .
C11 C 0.21096(7) 0.3433(2) 0.03547(8) 0.0405(4) Uani 1 1 d . . .
H8 H 0.1945 0.2865 -0.0008 0.049 Uiso 1 1 calc R . .
C12 C 0.27382(7) 0.36506(19) 0.04075(8) 0.0363(3) Uani 1 1 d . . .
H9 H 0.3003 0.3237 0.0079 0.044 Uiso 1 1 calc R . .
C13 C 0.29854(6) 0.44734(18) 0.09397(7) 0.0304(3) Uani 1 1 d . . .
N2 N 0.36233(5) 0.47993(15) 0.09828(6) 0.0303(3) Uani 1 1 d . . .
C14 C 0.40168(6) 0.37426(18) 0.08143(7) 0.0316(3) Uani 1 1 d . . .
H10 H 0.3877 0.2715 0.0689 0.038 Uiso 1 1 calc R . .
C15 C 0.46725(6) 0.40759(18) 0.08099(7) 0.0313(3) Uani 1 1 d . . .
C16 C 0.48907(6) 0.56005(18) 0.09714(6) 0.0290(3) Uani 1 1 d . . .
C17 C 0.55293(6) 0.58698(18) 0.09800(7) 0.0310(3) Uani 1 1 d . . .
C18 C 0.59352(6) 0.4655(2) 0.08353(8) 0.0366(3) Uani 1 1 d . . .
H11 H 0.6365 0.4853 0.0840 0.044 Uiso 1 1 calc R . .
C19 C 0.57160(7) 0.3136(2) 0.06814(8) 0.0426(4) Uani 1 1 d . . .
H12 H 0.5997 0.2300 0.0588 0.051 Uiso 1 1 calc R . .
C20 C 0.50910(7) 0.2849(2) 0.06655(8) 0.0392(4) Uani 1 1 d . . .
H13 H 0.4943 0.1818 0.0557 0.047 Uiso 1 1 calc R . .
O2 O 0.45165(4) 0.68063(13) 0.11349(5) 0.0348(3) Uani 1 1 d . . .
H14 H 0.4150 0.6492 0.1125 0.052 Uiso 1 1 calc R . .
O3 O 0.56994(4) 0.74170(13) 0.11337(6) 0.0362(3) Uani 1 1 d . . .
N3 N 0.40271(14) 0.2191(4) 0.23758(19) 0.0541(8) Uani 0.50 1 d P A 1
C21 C 0.44576(14) 0.2961(4) 0.24265(16) 0.0376(7) Uani 0.50 1 d P A 1
C22 C 0.5000 0.3948(3) 0.2500 0.0367(5) Uani 1 2 d S . .
H15 H 0.4880 0.5073 0.2502 0.055 Uiso 0.50 1 calc PR A 1
H16 H 0.5282 0.3750 0.2134 0.055 Uiso 0.50 1 calc PR A 1
H17 H 0.5205 0.3688 0.2914 0.055 Uiso 0.50 1 calc PR A 1
N4 N 0.40811(19) 1.0835(5) 0.2527(3) 0.0873(15) Uani 0.50 1 d P B 2
C23 C 0.44887(18) 0.9960(5) 0.2518(2) 0.0559(10) Uani 0.50 1 d P B 2
C24 C 0.5000 0.8864(3) 0.2500 0.0505(6) Uani 1 2 d S . .
H18 H 0.4910 0.8001 0.2191 0.076 Uiso 0.50 1 calc PR B 2
H19 H 0.5066 0.8418 0.2938 0.076 Uiso 0.50 1 calc PR B 2
H20 H 0.5371 0.9429 0.2358 0.076 Uiso 0.50 1 calc PR B 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0226(6) 0.0372(7) 0.0401(8) -0.0014(6) 0.0004(6) 0.0027(6)
C2 0.0226(6) 0.0348(7) 0.0360(7) -0.0005(6) 0.0039(5) 0.0020(5)
C3 0.0247(6) 0.0349(7) 0.0329(7) 0.0046(6) 0.0024(5) 0.0027(5)
C4 0.0276(6) 0.0430(8) 0.0384(8) 0.0042(6) 0.0023(6) 0.0095(6)
C5 0.0344(8) 0.0438(9) 0.0402(8) -0.0032(7) 0.0052(6) 0.0111(7)
C6 0.0335(7) 0.0400(8) 0.0368(8) -0.0036(6) 0.0012(6) 0.0036(6)
O1 0.0233(5) 0.0479(6) 0.0384(6) -0.0110(5) -0.0004(4) 0.0050(4)
C7 0.0233(6) 0.0391(7) 0.0331(7) 0.0092(6) 0.0005(5) 0.0015(6)
N1 0.0234(5) 0.0375(6) 0.0298(6) 0.0046(5) 0.0007(4) -0.0023(5)
C8 0.0250(6) 0.0330(7) 0.0314(7) 0.0084(6) -0.0031(5) -0.0034(5)
C9 0.0251(7) 0.0411(8) 0.0422(8) 0.0121(6) -0.0014(6) -0.0046(6)
C10 0.0270(7) 0.0440(9) 0.0502(9) 0.0139(7) -0.0106(6) -0.0095(6)
C11 0.0366(8) 0.0430(9) 0.0418(8) 0.0063(7) -0.0143(6) -0.0086(7)
C12 0.0346(7) 0.0408(8) 0.0335(7) 0.0030(6) -0.0068(6) -0.0039(6)
C13 0.0252(6) 0.0354(7) 0.0306(7) 0.0063(6) -0.0043(5) -0.0040(5)
N2 0.0237(5) 0.0402(7) 0.0270(6) 0.0014(5) -0.0013(4) -0.0025(5)
C14 0.0295(7) 0.0374(7) 0.0279(7) -0.0015(6) -0.0039(5) -0.0027(6)
C15 0.0268(7) 0.0413(8) 0.0257(6) 0.0001(6) -0.0016(5) 0.0005(6)
C16 0.0241(6) 0.0382(7) 0.0246(6) 0.0035(5) -0.0010(5) 0.0017(5)
C17 0.0253(6) 0.0403(8) 0.0274(6) 0.0061(6) -0.0015(5) -0.0018(6)
C18 0.0235(6) 0.0508(9) 0.0354(7) 0.0003(7) 0.0005(6) 0.0023(6)
C19 0.0326(8) 0.0496(9) 0.0456(9) -0.0079(7) 0.0013(6) 0.0106(7)
C20 0.0357(8) 0.0412(8) 0.0406(8) -0.0088(7) -0.0010(6) 0.0027(7)
O2 0.0219(5) 0.0371(6) 0.0453(6) -0.0007(5) -0.0017(4) 0.0010(4)
O3 0.0229(5) 0.0385(6) 0.0470(6) 0.0066(5) -0.0042(4) -0.0018(4)
N3 0.0360(15) 0.0504(18) 0.076(2) -0.0019(16) -0.0038(15) -0.0029(14)
C21 0.0304(15) 0.0393(16) 0.0430(17) -0.0007(13) -0.0023(12) 0.0051(13)
C22 0.0335(10) 0.0380(11) 0.0387(11) 0.000 -0.0011(8) 0.000
N4 0.055(2) 0.057(2) 0.150(5) -0.002(3) -0.033(3) -0.0075(19)
C23 0.049(2) 0.0424(18) 0.076(3) 0.0026(19) -0.0225(19) -0.0111(17)
C24 0.0518(14) 0.0399(12) 0.0598(16) 0.000 -0.0061(12) 0.000

_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
C1 C6 1.381(2) . ?
C1 O3 1.3924(17) 4_655 ?
C1 C2 1.402(2) . ?
C2 O1 1.3425(17) . ?
C2 C3 1.4153(19) . ?
C3 C4 1.404(2) . ?
C3 C7 1.452(2) . ?
C4 C5 1.379(2) . ?
C4 H1 0.9500 . ?
C5 C6 1.399(2) . ?
C5 H2 0.9500 . ?
C6 H3 0.9500 . ?
O1 H4 0.8400 . ?
C7 N1 1.2841(19) . ?
C7 H5 0.9500 . ?
N1 C8 1.4155(18) . ?
C8 C9 1.3984(19) . ?
C8 C13 1.409(2) . ?
C9 C10 1.393(2) . ?
C9 H6 0.9500 . ?
C10 C11 1.383(3) . ?
C10 H7 0.9500 . ?
C11 C12 1.385(2) . ?
C11 H8 0.9500 . ?
C12 C13 1.395(2) . ?
C12 H9 0.9500 . ?
C13 N2 1.4180(17) . ?
N2 C14 1.2803(19) . ?
C14 C15 1.4545(19) . ?
C14 H10 0.9500 . ?
C15 C16 1.405(2) . ?
C15 C20 1.406(2) . ?
C16 O2 1.3415(17) . ?
C16 C17 1.4084(18) . ?
C17 C18 1.381(2) . ?
C17 O3 1.3867(19) . ?
C18 C19 1.398(2) . ?
C18 H11 0.9500 . ?
C19 C20 1.382(2) . ?
C19 H12 0.9500 . ?
C20 H13 0.9500 . ?
O2 H14 0.8400 . ?
O3 C1 1.3924(17) 4_655 ?
N3 C21 1.143(4) . ?
C21 C22 1.450(3) . ?
C22 H15 0.9800 . ?
C22 H16 0.9800 . ?
C22 H17 0.9800 . ?
N4 C23 1.152(5) . ?
C23 C24 1.445(5) . ?
C24 H18 0.9800 . ?
C24 H19 0.9800 . ?
C24 H20 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 O3 118.51(14) . 4_655 ?
C6 C1 C2 120.72(13) . . ?
O3 C1 C2 120.51(13) 4_655 . ?
O1 C2 C1 119.10(12) . . ?
O1 C2 C3 122.18(13) . . ?
C1 C2 C3 118.72(13) . . ?
C4 C3 C2 119.59(14) . . ?
C4 C3 C7 119.64(13) . . ?
C2 C3 C7 120.77(13) . . ?
C5 C4 C3 120.74(14) . . ?
C5 C4 H1 119.6 . . ?
C3 C4 H1 119.6 . . ?
C4 C5 C6 119.64(14) . . ?
C4 C5 H2 120.2 . . ?
C6 C5 H2 120.2 . . ?
C1 C6 C5 120.51(15) . . ?
C1 C6 H3 119.7 . . ?
C5 C6 H3 119.7 . . ?
C2 O1 H4 109.5 . . ?
N1 C7 C3 120.89(12) . . ?
N1 C7 H5 119.6 . . ?
C3 C7 H5 119.6 . . ?
C7 N1 C8 121.16(12) . . ?
C9 C8 C13 119.14(13) . . ?
C9 C8 N1 123.49(13) . . ?
C13 C8 N1 117.23(12) . . ?
C10 C9 C8 120.33(15) . . ?
C10 C9 H6 119.8 . . ?
C8 C9 H6 119.8 . . ?
C11 C10 C9 120.20(14) . . ?
C11 C10 H7 119.9 . . ?
C9 C10 H7 119.9 . . ?
C10 C11 C12 120.19(15) . . ?
C10 C11 H8 119.9 . . ?
C12 C11 H8 119.9 . . ?
C11 C12 C13 120.47(15) . . ?
C11 C12 H9 119.8 . . ?
C13 C12 H9 119.8 . . ?
C12 C13 C8 119.66(13) . . ?
C12 C13 N2 121.44(13) . . ?
C8 C13 N2 118.77(13) . . ?
C14 N2 C13 120.31(13) . . ?
N2 C14 C15 121.66(14) . . ?
N2 C14 H10 119.2 . . ?
C15 C14 H10 119.2 . . ?
C16 C15 C20 119.85(13) . . ?
C16 C15 C14 120.39(13) . . ?
C20 C15 C14 119.73(14) . . ?
O2 C16 C15 122.73(12) . . ?
O2 C16 C17 118.36(13) . . ?
C15 C16 C17 118.89(13) . . ?
C18 C17 O3 124.70(13) . . ?
C18 C17 C16 120.67(14) . . ?
O3 C17 C16 114.63(13) . . ?
C17 C18 C19 120.24(13) . . ?
C17 C18 H11 119.9 . . ?
C19 C18 H11 119.9 . . ?
C20 C19 C18 120.03(15) . . ?
C20 C19 H12 120.0 . . ?
C18 C19 H12 120.0 . . ?
C19 C20 C15 120.33(15) . . ?
C19 C20 H13 119.8 . . ?
C15 C20 H13 119.8 . . ?
C16 O2 H14 109.5 . . ?
C17 O3 C1 118.09(11) . 4_655 ?
N3 C21 C22 179.1(4) . . ?
N4 C23 C24 179.5(5) . . ?
C23 C24 H18 109.5 . . ?
C23 C24 H19 109.5 . . ?
H18 C24 H19 109.5 . . ?
C23 C24 H20 109.5 . . ?
H18 C24 H20 109.5 . . ?
H19 C24 H20 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 O1 177.37(14) . . . . ?
O3 C1 C2 O1 3.4(2) 4_655 . . . ?
C6 C1 C2 C3 -3.4(2) . . . . ?
O3 C1 C2 C3 -177.38(13) 4_655 . . . ?
O1 C2 C3 C4 -178.98(14) . . . . ?
C1 C2 C3 C4 1.8(2) . . . . ?
O1 C2 C3 C7 1.8(2) . . . . ?
C1 C2 C3 C7 -177.44(13) . . . . ?
C2 C3 C4 C5 0.7(2) . . . . ?
C7 C3 C4 C5 179.93(14) . . . . ?
C3 C4 C5 C6 -1.6(2) . . . . ?
O3 C1 C6 C5 176.61(14) 4_655 . . . ?
C2 C1 C6 C5 2.5(2) . . . . ?
C4 C5 C6 C1 0.0(3) . . . . ?
C4 C3 C7 N1 -179.24(14) . . . . ?
C2 C3 C7 N1 0.0(2) . . . . ?
C3 C7 N1 C8 176.07(12) . . . . ?
C7 N1 C8 C9 -22.8(2) . . . . ?
C7 N1 C8 C13 161.47(13) . . . . ?
C13 C8 C9 C10 -0.7(2) . . . . ?
N1 C8 C9 C10 -176.34(14) . . . . ?
C8 C9 C10 C11 1.0(2) . . . . ?
C9 C10 C11 C12 -0.8(2) . . . . ?
C10 C11 C12 C13 0.4(2) . . . . ?
C11 C12 C13 C8 -0.1(2) . . . . ?
C11 C12 C13 N2 -175.91(14) . . . . ?
C9 C8 C13 C12 0.2(2) . . . . ?
N1 C8 C13 C12 176.16(13) . . . . ?
C9 C8 C13 N2 176.19(13) . . . . ?
N1 C8 C13 N2 -7.90(19) . . . . ?
C12 C13 N2 C14 -40.8(2) . . . . ?
C8 C13 N2 C14 143.33(14) . . . . ?
C13 N2 C14 C15 175.72(12) . . . . ?
N2 C14 C15 C16 -2.2(2) . . . . ?
N2 C14 C15 C20 175.58(14) . . . . ?
C20 C15 C16 O2 -177.75(13) . . . . ?
C14 C15 C16 O2 0.0(2) . . . . ?
C20 C15 C16 C17 0.5(2) . . . . ?
C14 C15 C16 C17 178.25(12) . . . . ?
O2 C16 C17 C18 178.02(13) . . . . ?
C15 C16 C17 C18 -0.3(2) . . . . ?
O2 C16 C17 O3 -2.74(18) . . . . ?
C15 C16 C17 O3 178.94(12) . . . . ?
O3 C17 C18 C19 -179.51(14) . . . . ?
C16 C17 C18 C19 -0.3(2) . . . . ?
C17 C18 C19 C20 0.8(2) . . . . ?
C18 C19 C20 C15 -0.6(2) . . . . ?
C16 C15 C20 C19 0.0(2) . . . . ?
C14 C15 C20 C19 -177.81(15) . . . . ?
C18 C17 O3 C1 -16.2(2) . . . 4_655 ?
C16 C17 O3 C1 164.60(13) . . . 4_655 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.180
_refine_diff_density_min         -0.162
_refine_diff_density_rms         0.052

# Attachment 'nabeshima_2.cif'

data_uts118
_database_code_depnum_ccdc_archive 'CCDC 743176'
#TrackingRef 'nabeshima_2.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            (LNi2)_4DMSO
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H24 N4 Ni2 O6, 4(C2 H6 O S)'
_chemical_formula_sum            'C48 H48 N4 Ni2 O10 S4'
_chemical_formula_weight         1086.56

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.2439(8)
_cell_length_b                   11.7378(8)
_cell_length_c                   11.7488(9)
_cell_angle_alpha                63.3210(18)
_cell_angle_beta                 66.059(2)
_cell_angle_gamma                60.3036(16)
_cell_volume                     1169.48(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    120
_cell_measurement_reflns_used    11404
_cell_measurement_theta_min      3.26
_cell_measurement_theta_max      27.46

_exptl_crystal_description       prismatic
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             564
_exptl_absorpt_coefficient_mu    1.048
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7106
_exptl_absorpt_correction_T_max  0.9025
_exptl_absorpt_process_details   'Rapid AUTO (Rigaku Corp.)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS Rapid'
_diffrn_measurement_method       IP
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            11404
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.26
_diffrn_reflns_theta_max         27.46
_reflns_number_total             5298
_reflns_number_gt                4514
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Rapid AUTO (Rigaku Corp.)'
_computing_cell_refinement       'Rapid AUTO (Rigaku Corp.)'
_computing_data_reduction        'Rapid AUTO (Rigaku Corp.)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  ORTEP-3

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0744P)^2^+1.1497P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5298
_refine_ls_number_parameters     311
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0475
_refine_ls_wR_factor_ref         0.1345
_refine_ls_wR_factor_gt          0.1269
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_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 0.16181(3) 0.49074(3) 0.70479(3) 0.01790(12) Uani 1 1 d . . .
C1 C 0.3478(3) 0.7364(3) 0.6676(3) 0.0213(5) Uani 1 1 d . . .
C2 C 0.2466(3) 0.6764(3) 0.7109(3) 0.0187(5) Uani 1 1 d . . .
C3 C 0.1083(3) 0.7502(3) 0.7745(3) 0.0203(5) Uani 1 1 d . . .
C4 C 0.0731(3) 0.8792(3) 0.7854(3) 0.0237(6) Uani 1 1 d . . .
H1 H -0.0187 0.9247 0.8313 0.028 Uiso 1 1 calc R . .
C5 C 0.1692(3) 0.9386(3) 0.7308(3) 0.0256(6) Uani 1 1 d . . .
H2 H 0.1431 1.0279 0.7333 0.031 Uiso 1 1 calc R . .
C6 C 0.3074(3) 0.8666(3) 0.6707(3) 0.0233(5) Uani 1 1 d . . .
H3 H 0.3743 0.9086 0.6314 0.028 Uiso 1 1 calc R . .
O1 O 0.28403(18) 0.56301(19) 0.68849(18) 0.0200(4) Uani 1 1 d . . .
C7 C 0.0014(3) 0.6960(3) 0.8296(3) 0.0215(5) Uani 1 1 d . . .
H4 H -0.0854 0.7433 0.8801 0.026 Uiso 1 1 calc R . .
N1 N 0.0135(2) 0.5864(2) 0.8159(2) 0.0189(4) Uani 1 1 d . . .
C8 C -0.1001(3) 0.5403(3) 0.8757(3) 0.0206(5) Uani 1 1 d . . .
C9 C -0.2191(3) 0.5845(3) 0.9714(3) 0.0220(5) Uani 1 1 d . . .
H5 H -0.2301 0.6500 1.0050 0.026 Uiso 1 1 calc R . .
C10 C -0.3212(3) 0.5306(3) 1.0166(3) 0.0230(5) Uani 1 1 d . . .
H6 H -0.4036 0.5604 1.0811 0.028 Uiso 1 1 calc R . .
C11 C -0.3047(3) 0.4338(3) 0.9689(3) 0.0254(6) Uani 1 1 d . . .
H7 H -0.3758 0.3979 1.0016 0.030 Uiso 1 1 calc R . .
C12 C -0.1862(3) 0.3884(3) 0.8742(3) 0.0246(6) Uani 1 1 d . . .
H8 H -0.1750 0.3215 0.8422 0.029 Uiso 1 1 calc R . .
C13 C -0.0837(3) 0.4433(3) 0.8270(3) 0.0206(5) Uani 1 1 d . . .
N2 N 0.0406(2) 0.4147(2) 0.7260(2) 0.0206(5) Uani 1 1 d . . .
C14 C 0.0548(3) 0.3510(3) 0.6519(3) 0.0217(5) Uani 1 1 d . . .
H9 H -0.0181 0.3217 0.6709 0.026 Uiso 1 1 calc R . .
C15 C 0.1714(3) 0.3221(3) 0.5446(3) 0.0207(5) Uani 1 1 d . . .
C16 C 0.2912(3) 0.3501(3) 0.5173(3) 0.0201(5) Uani 1 1 d . . .
C17 C 0.4028(3) 0.3142(3) 0.4088(3) 0.0221(5) Uani 1 1 d . . .
C18 C 0.3883(3) 0.2685(3) 0.3278(3) 0.0229(5) Uani 1 1 d . . .
H10 H 0.4601 0.2553 0.2508 0.027 Uiso 1 1 calc R . .
C19 C 0.2696(3) 0.2411(3) 0.3570(3) 0.0229(5) Uani 1 1 d . . .
H11 H 0.2625 0.2063 0.3019 0.028 Uiso 1 1 calc R . .
C20 C 0.1640(3) 0.2646(3) 0.4652(3) 0.0235(5) Uani 1 1 d . . .
H12 H 0.0852 0.2424 0.4874 0.028 Uiso 1 1 calc R . .
O2 O 0.30466(19) 0.4043(2) 0.58465(19) 0.0219(4) Uani 1 1 d . . .
O3 O 0.5178(2) 0.3426(2) 0.3866(2) 0.0278(5) Uani 1 1 d . . .
S1 S 0.79738(7) 0.22851(7) 0.59828(7) 0.02502(17) Uani 1 1 d . . .
O4 O 0.8515(2) 0.2058(2) 0.7081(2) 0.0282(4) Uani 1 1 d . . .
C21 C 0.6114(3) 0.3232(3) 0.6381(3) 0.0299(6) Uani 1 1 d . . .
H13 H 0.5701 0.2741 0.7263 0.045 Uiso 1 1 calc R . .
H14 H 0.5691 0.3322 0.5745 0.045 Uiso 1 1 calc R . .
H15 H 0.5929 0.4152 0.6351 0.045 Uiso 1 1 calc R . .
C22 C 0.7961(3) 0.0654(3) 0.6266(3) 0.0336(7) Uani 1 1 d . . .
H16 H 0.8931 -0.0001 0.6063 0.050 Uiso 1 1 calc R . .
H17 H 0.7432 0.0778 0.5703 0.050 Uiso 1 1 calc R . .
H18 H 0.7514 0.0295 0.7188 0.050 Uiso 1 1 calc R . .
S2 S 0.28393(8) 0.06217(8) 0.93032(9) 0.0346(2) Uani 1 1 d . . .
O5 O 0.2977(3) 0.1065(2) 1.0245(3) 0.0424(6) Uani 1 1 d . . .
C23 C 0.4268(4) 0.0750(4) 0.7906(3) 0.0413(8) Uani 1 1 d . . .
H19 H 0.4129 0.1724 0.7444 0.062 Uiso 1 1 calc R . .
H20 H 0.4307 0.0343 0.7317 0.062 Uiso 1 1 calc R . .
H21 H 0.5153 0.0254 0.8189 0.062 Uiso 1 1 calc R . .
C24 C 0.3490(5) -0.1213(4) 0.9905(4) 0.0507(10) Uani 1 1 d . . .
H22 H 0.4465 -0.1578 0.9965 0.076 Uiso 1 1 calc R . .
H23 H 0.3459 -0.1563 0.9305 0.076 Uiso 1 1 calc R . .
H24 H 0.2905 -0.1509 1.0775 0.076 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.01484(18) 0.0204(2) 0.01991(19) -0.01198(14) 0.00111(13) -0.00682(13)
C1 0.0183(12) 0.0260(13) 0.0206(12) -0.0139(11) 0.0015(10) -0.0083(10)
C2 0.0186(12) 0.0227(13) 0.0162(11) -0.0100(10) -0.0011(9) -0.0077(10)
C3 0.0184(12) 0.0194(12) 0.0230(13) -0.0103(10) -0.0018(10) -0.0063(10)
C4 0.0180(12) 0.0235(13) 0.0299(14) -0.0154(12) -0.0019(11) -0.0050(10)
C5 0.0248(13) 0.0182(13) 0.0345(15) -0.0140(12) -0.0060(12) -0.0044(10)
C6 0.0221(12) 0.0254(14) 0.0270(14) -0.0135(11) -0.0012(11) -0.0112(11)
O1 0.0163(8) 0.0216(9) 0.0226(9) -0.0128(8) 0.0010(7) -0.0067(7)
C7 0.0180(12) 0.0221(13) 0.0226(13) -0.0122(11) -0.0010(10) -0.0048(10)
N1 0.0163(10) 0.0201(11) 0.0195(11) -0.0091(9) -0.0017(8) -0.0058(8)
C8 0.0192(12) 0.0208(13) 0.0197(12) -0.0070(10) -0.0036(10) -0.0064(10)
C9 0.0206(12) 0.0251(13) 0.0208(13) -0.0115(11) -0.0021(10) -0.0073(10)
C10 0.0184(12) 0.0252(14) 0.0206(13) -0.0104(11) 0.0017(10) -0.0070(10)
C11 0.0202(12) 0.0292(14) 0.0261(14) -0.0111(12) 0.0013(11) -0.0120(11)
C12 0.0215(12) 0.0292(14) 0.0263(14) -0.0152(12) 0.0017(11) -0.0119(11)
C13 0.0173(11) 0.0215(13) 0.0204(12) -0.0106(10) -0.0004(10) -0.0053(10)
N2 0.0145(10) 0.0232(11) 0.0216(11) -0.0112(9) 0.0010(8) -0.0058(8)
C14 0.0196(12) 0.0225(13) 0.0248(13) -0.0122(11) -0.0006(10) -0.0086(10)
C15 0.0189(12) 0.0228(13) 0.0222(13) -0.0111(11) -0.0031(10) -0.0071(10)
C16 0.0206(12) 0.0200(12) 0.0217(13) -0.0102(10) -0.0018(10) -0.0084(10)
C17 0.0169(12) 0.0250(13) 0.0273(14) -0.0143(11) -0.0007(10) -0.0081(10)
C18 0.0208(12) 0.0250(14) 0.0208(13) -0.0125(11) 0.0008(10) -0.0070(10)
C19 0.0239(13) 0.0258(14) 0.0233(13) -0.0138(11) -0.0053(11) -0.0074(11)
C20 0.0186(12) 0.0290(14) 0.0273(14) -0.0147(12) -0.0033(11) -0.0087(10)
O2 0.0184(9) 0.0269(10) 0.0250(10) -0.0157(8) 0.0011(7) -0.0100(7)
O3 0.0187(9) 0.0340(11) 0.0390(12) -0.0267(10) 0.0068(8) -0.0133(8)
S1 0.0216(3) 0.0288(4) 0.0237(3) -0.0091(3) -0.0020(3) -0.0108(3)
O4 0.0277(10) 0.0303(11) 0.0326(11) -0.0128(9) -0.0072(9) -0.0127(8)
C21 0.0240(13) 0.0292(15) 0.0340(16) -0.0100(13) -0.0045(12) -0.0102(11)
C22 0.0344(16) 0.0332(16) 0.0404(18) -0.0187(14) -0.0134(14) -0.0082(13)
S2 0.0267(4) 0.0330(4) 0.0441(5) -0.0200(4) 0.0003(3) -0.0113(3)
O5 0.0367(13) 0.0404(13) 0.0526(15) -0.0324(12) 0.0054(11) -0.0131(10)
C23 0.047(2) 0.0404(19) 0.0321(17) -0.0068(15) 0.0011(15) -0.0261(16)
C24 0.082(3) 0.039(2) 0.0304(18) -0.0153(16) 0.0081(18) -0.036(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2 1.8526(19) . ?
Ni1 N1 1.854(2) . ?
Ni1 O1 1.8547(19) . ?
Ni1 N2 1.856(2) . ?
C1 C6 1.376(4) . ?
C1 O3 1.382(3) 2_666 ?
C1 C2 1.432(4) . ?
C2 O1 1.299(3) . ?
C2 C3 1.425(3) . ?
C3 C4 1.415(4) . ?
C3 C7 1.424(4) . ?
C4 C5 1.359(4) . ?
C4 H1 0.9500 . ?
C5 C6 1.404(4) . ?
C5 H2 0.9500 . ?
C6 H3 0.9500 . ?
C7 N1 1.301(4) . ?
C7 H4 0.9500 . ?
N1 C8 1.425(3) . ?
C8 C9 1.392(4) . ?
C8 C13 1.396(4) . ?
C9 C10 1.388(4) . ?
C9 H5 0.9500 . ?
C10 C11 1.385(4) . ?
C10 H6 0.9500 . ?
C11 C12 1.387(4) . ?
C11 H7 0.9500 . ?
C12 C13 1.395(4) . ?
C12 H8 0.9500 . ?
C13 N2 1.422(3) . ?
N2 C14 1.303(4) . ?
C14 C15 1.423(4) . ?
C14 H9 0.9500 . ?
C15 C20 1.420(4) . ?
C15 C16 1.421(4) . ?
C16 O2 1.303(3) . ?
C16 C17 1.427(4) . ?
C17 C18 1.376(4) . ?
C17 O3 1.387(3) . ?
C18 C19 1.399(4) . ?
C18 H10 0.9500 . ?
C19 C20 1.367(4) . ?
C19 H11 0.9500 . ?
C20 H12 0.9500 . ?
O3 C1 1.382(3) 2_666 ?
S1 O4 1.508(2) . ?
S1 C21 1.788(3) . ?
S1 C22 1.796(3) . ?
C21 H13 0.9800 . ?
C21 H14 0.9800 . ?
C21 H15 0.9800 . ?
C22 H16 0.9800 . ?
C22 H17 0.9800 . ?
C22 H18 0.9800 . ?
S2 O5 1.502(3) . ?
S2 C24 1.779(4) . ?
S2 C23 1.782(4) . ?
C23 H19 0.9800 . ?
C23 H20 0.9800 . ?
C23 H21 0.9800 . ?
C24 H22 0.9800 . ?
C24 H23 0.9800 . ?
C24 H24 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 N1 176.19(9) . . ?
O2 Ni1 O1 86.01(8) . . ?
N1 Ni1 O1 94.47(9) . . ?
O2 Ni1 N2 94.44(9) . . ?
N1 Ni1 N2 85.20(10) . . ?
O1 Ni1 N2 178.27(9) . . ?
C6 C1 O3 124.8(2) . 2_666 ?
C6 C1 C2 121.1(2) . . ?
O3 C1 C2 113.8(2) 2_666 . ?
O1 C2 C3 124.7(2) . . ?
O1 C2 C1 119.5(2) . . ?
C3 C2 C1 115.8(2) . . ?
C4 C3 C7 118.0(2) . . ?
C4 C3 C2 121.1(2) . . ?
C7 C3 C2 120.9(2) . . ?
C5 C4 C3 120.7(2) . . ?
C5 C4 H1 119.6 . . ?
C3 C4 H1 119.6 . . ?
C4 C5 C6 119.3(3) . . ?
C4 C5 H2 120.3 . . ?
C6 C5 H2 120.3 . . ?
C1 C6 C5 121.2(3) . . ?
C1 C6 H3 119.4 . . ?
C5 C6 H3 119.4 . . ?
C2 O1 Ni1 125.40(16) . . ?
N1 C7 C3 124.9(2) . . ?
N1 C7 H4 117.5 . . ?
C3 C7 H4 117.5 . . ?
C7 N1 C8 120.5(2) . . ?
C7 N1 Ni1 125.36(19) . . ?
C8 N1 Ni1 113.70(17) . . ?
C9 C8 C13 120.7(3) . . ?
C9 C8 N1 126.3(2) . . ?
C13 C8 N1 113.0(2) . . ?
C10 C9 C8 118.5(3) . . ?
C10 C9 H5 120.7 . . ?
C8 C9 H5 120.7 . . ?
C11 C10 C9 120.9(2) . . ?
C11 C10 H6 119.6 . . ?
C9 C10 H6 119.6 . . ?
C10 C11 C12 121.1(3) . . ?
C10 C11 H7 119.5 . . ?
C12 C11 H7 119.5 . . ?
C11 C12 C13 118.4(3) . . ?
C11 C12 H8 120.8 . . ?
C13 C12 H8 120.8 . . ?
C12 C13 C8 120.4(2) . . ?
C12 C13 N2 126.4(2) . . ?
C8 C13 N2 113.1(2) . . ?
C14 N2 C13 119.8(2) . . ?
C14 N2 Ni1 126.29(19) . . ?
C13 N2 Ni1 113.63(18) . . ?
N2 C14 C15 124.8(2) . . ?
N2 C14 H9 117.6 . . ?
C15 C14 H9 117.6 . . ?
C20 C15 C16 121.0(2) . . ?
C20 C15 C14 117.8(2) . . ?
C16 C15 C14 121.3(2) . . ?
O2 C16 C15 124.4(2) . . ?
O2 C16 C17 119.4(2) . . ?
C15 C16 C17 116.2(2) . . ?
C18 C17 O3 124.2(2) . . ?
C18 C17 C16 121.4(2) . . ?
O3 C17 C16 114.1(2) . . ?
C17 C18 C19 121.0(3) . . ?
C17 C18 H10 119.5 . . ?
C19 C18 H10 119.5 . . ?
C20 C19 C18 119.5(3) . . ?
C20 C19 H11 120.2 . . ?
C18 C19 H11 120.2 . . ?
C19 C20 C15 120.4(3) . . ?
C19 C20 H12 119.8 . . ?
C15 C20 H12 119.8 . . ?
C16 O2 Ni1 126.14(17) . . ?
C1 O3 C17 121.0(2) 2_666 . ?
O4 S1 C21 106.08(14) . . ?
O4 S1 C22 105.37(14) . . ?
C21 S1 C22 98.73(15) . . ?
S1 C21 H13 109.5 . . ?
S1 C21 H14 109.5 . . ?
H13 C21 H14 109.5 . . ?
S1 C21 H15 109.5 . . ?
H13 C21 H15 109.5 . . ?
H14 C21 H15 109.5 . . ?
S1 C22 H16 109.5 . . ?
S1 C22 H17 109.5 . . ?
H16 C22 H17 109.5 . . ?
S1 C22 H18 109.5 . . ?
H16 C22 H18 109.5 . . ?
H17 C22 H18 109.5 . . ?
O5 S2 C24 105.92(18) . . ?
O5 S2 C23 106.35(17) . . ?
C24 S2 C23 96.52(18) . . ?
S2 C23 H19 109.5 . . ?
S2 C23 H20 109.5 . . ?
H19 C23 H20 109.5 . . ?
S2 C23 H21 109.5 . . ?
H19 C23 H21 109.5 . . ?
H20 C23 H21 109.5 . . ?
S2 C24 H22 109.5 . . ?
S2 C24 H23 109.5 . . ?
H22 C24 H23 109.5 . . ?
S2 C24 H24 109.5 . . ?
H22 C24 H24 109.5 . . ?
H23 C24 H24 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 O1 169.6(3) . . . . ?
O3 C1 C2 O1 -4.9(4) 2_666 . . . ?
C6 C1 C2 C3 -9.0(4) . . . . ?
O3 C1 C2 C3 176.4(2) 2_666 . . . ?
O1 C2 C3 C4 -174.6(3) . . . . ?
C1 C2 C3 C4 4.0(4) . . . . ?
O1 C2 C3 C7 5.7(4) . . . . ?
C1 C2 C3 C7 -175.8(2) . . . . ?
C7 C3 C4 C5 -177.7(3) . . . . ?
C2 C3 C4 C5 2.6(4) . . . . ?
C3 C4 C5 C6 -4.3(4) . . . . ?
O3 C1 C6 C5 -178.3(3) 2_666 . . . ?
C2 C1 C6 C5 7.8(4) . . . . ?
C4 C5 C6 C1 -0.9(5) . . . . ?
C3 C2 O1 Ni1 12.2(4) . . . . ?
C1 C2 O1 Ni1 -166.33(18) . . . . ?
O2 Ni1 O1 C2 155.0(2) . . . . ?
N1 Ni1 O1 C2 -21.2(2) . . . . ?
C4 C3 C7 N1 172.7(3) . . . . ?
C2 C3 C7 N1 -7.6(4) . . . . ?
C3 C7 N1 C8 179.8(2) . . . . ?
C3 C7 N1 Ni1 -8.6(4) . . . . ?
O1 Ni1 N1 C7 19.4(2) . . . . ?
N2 Ni1 N1 C7 -162.3(2) . . . . ?
O1 Ni1 N1 C8 -168.47(17) . . . . ?
N2 Ni1 N1 C8 9.82(18) . . . . ?
C7 N1 C8 C9 -13.3(4) . . . . ?
Ni1 N1 C8 C9 174.1(2) . . . . ?
C7 N1 C8 C13 165.6(2) . . . . ?
Ni1 N1 C8 C13 -6.9(3) . . . . ?
C13 C8 C9 C10 -0.4(4) . . . . ?
N1 C8 C9 C10 178.5(2) . . . . ?
C8 C9 C10 C11 0.8(4) . . . . ?
C9 C10 C11 C12 -0.3(4) . . . . ?
C10 C11 C12 C13 -0.5(4) . . . . ?
C11 C12 C13 C8 0.8(4) . . . . ?
C11 C12 C13 N2 -176.7(3) . . . . ?
C9 C8 C13 C12 -0.4(4) . . . . ?
N1 C8 C13 C12 -179.4(2) . . . . ?
C9 C8 C13 N2 177.4(2) . . . . ?
N1 C8 C13 N2 -1.6(3) . . . . ?
C12 C13 N2 C14 12.7(4) . . . . ?
C8 C13 N2 C14 -164.9(2) . . . . ?
C12 C13 N2 Ni1 -172.9(2) . . . . ?
C8 C13 N2 Ni1 9.5(3) . . . . ?
O2 Ni1 N2 C14 -13.0(2) . . . . ?
N1 Ni1 N2 C14 163.2(2) . . . . ?
O2 Ni1 N2 C13 173.07(18) . . . . ?
N1 Ni1 N2 C13 -10.73(18) . . . . ?
C13 N2 C14 C15 177.2(2) . . . . ?
Ni1 N2 C14 C15 3.6(4) . . . . ?
N2 C14 C15 C20 -173.6(3) . . . . ?
N2 C14 C15 C16 6.3(4) . . . . ?
C20 C15 C16 O2 179.1(3) . . . . ?
C14 C15 C16 O2 -0.8(4) . . . . ?
C20 C15 C16 C17 -1.4(4) . . . . ?
C14 C15 C16 C17 178.8(2) . . . . ?
O2 C16 C17 C18 -174.0(3) . . . . ?
C15 C16 C17 C18 6.4(4) . . . . ?
O2 C16 C17 O3 0.0(4) . . . . ?
C15 C16 C17 O3 -179.6(2) . . . . ?
O3 C17 C18 C19 179.6(2) . . . . ?
C16 C17 C18 C19 -7.1(4) . . . . ?
C17 C18 C19 C20 2.3(4) . . . . ?
C18 C19 C20 C15 2.7(4) . . . . ?
C16 C15 C20 C19 -3.1(4) . . . . ?
C14 C15 C20 C19 176.7(3) . . . . ?
C15 C16 O2 Ni1 -14.0(4) . . . . ?
C17 C16 O2 Ni1 166.47(19) . . . . ?
O1 Ni1 O2 C16 -163.6(2) . . . . ?
N2 Ni1 O2 C16 18.1(2) . . . . ?
C18 C17 O3 C1 -36.2(4) . . . 2_666 ?
C16 C17 O3 C1 150.0(3) . . . 2_666 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.229
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.107