# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Zhong-Min Su'
_publ_contact_author_email       ZMSU@NENU.EDU.CN

_publ_section_title              
;
Two eight-connected self-penetrating porous
metal-organic frameworks: configurational isomers caused by different
linking modes between terephthalic acid anions and binuclear nickel
building units
;
loop_
_publ_author_name
'Zhong-Min Su'
'Chun-Jie Jiang'
'Ya-Qian Lan'
'Kuizhan Shao'
;
Xin-long Wang
;
'Guang-Sheng Yang'
'Hong-Ying Zang'

# Attachment '1.cif'

data_mm2
_database_code_depnum_ccdc_archive 'CCDC 695643'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H72 N14 Ni2 O15'
_chemical_formula_weight         1322.72

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Fdd2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+1/4, -y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+1/4, -y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+3/4, -y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'

_cell_length_a                   37.129(7)
_cell_length_b                   14.135(4)
_cell_length_c                   26.074(3)
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_volume                     13684(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.52
_cell_measurement_theta_max      30.85

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5552
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8454
_exptl_absorpt_correction_T_max  0.9127
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_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  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16827
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.73
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6002
_reflns_number_gt                5127
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1997)'
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.1283P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    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   0.86(2)
_refine_ls_number_reflns         6002
_refine_ls_number_parameters     267
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0607
_refine_ls_wR_factor_ref         0.1759
_refine_ls_wR_factor_gt          0.1693
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_restrained_S_all      1.002
_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 0.269528(16) 0.13562(4) 0.25024(2) 0.02089(18) Uani 1 1 d . . .
O1W O 0.2500 0.2500 0.29271(18) 0.0212(10) Uani 1 2 d S . .
O4 O 0.45611(10) -0.0249(3) 0.44709(14) 0.0295(8) Uani 1 1 d . . .
O3 O 0.47073(10) 0.1257(2) 0.46409(15) 0.0300(9) Uani 1 1 d . . .
O1 O 0.31694(10) 0.1340(3) 0.29025(15) 0.0317(9) Uani 1 1 d . . .
C5 C 0.42021(14) 0.0951(4) 0.4123(2) 0.0316(12) Uani 1 1 d . . .
N4 N 0.46131(13) -0.2095(4) 0.0998(2) 0.0445(13) Uani 1 1 d . . .
O2 O 0.31332(12) 0.2626(3) 0.33885(19) 0.0558(12) Uani 1 1 d U . .
N2 N 0.32826(15) -0.0614(4) 0.1639(2) 0.0499(14) Uani 1 1 d . . .
N1 N 0.28904(12) 0.0286(3) 0.20500(19) 0.0337(11) Uani 1 1 d . . .
N3 N 0.50021(13) -0.2913(4) 0.05474(19) 0.0379(11) Uani 1 1 d . . .
C7 C 0.37265(16) 0.0628(4) 0.3517(2) 0.0390(14) Uani 1 1 d . . .
H7 H 0.3607 0.0203 0.3305 0.047 Uiso 1 1 calc R . .
C2 C 0.36106(14) 0.1557(4) 0.3541(2) 0.0322(12) Uani 1 1 d . . .
C4 C 0.40920(16) 0.1886(4) 0.4138(2) 0.0392(14) Uani 1 1 d . . .
H4 H 0.4225 0.2316 0.4332 0.047 Uiso 1 1 calc R . .
C6 C 0.40199(16) 0.0318(4) 0.3806(2) 0.0412(14) Uani 1 1 d . . .
H6 H 0.4094 -0.0310 0.3788 0.049 Uiso 1 1 calc R . .
C12 C 0.36283(18) -0.0992(5) 0.1478(3) 0.0525(18) Uani 1 1 d . . .
C8 C 0.45187(13) 0.0610(4) 0.44387(19) 0.0287(12) Uani 1 1 d . . .
C9 C 0.32298(17) 0.0069(5) 0.2002(3) 0.0461(15) Uani 1 1 d . . .
H9 H 0.3414 0.0346 0.2192 0.055 Uiso 1 1 calc R . .
C3 C 0.37936(16) 0.2200(4) 0.3878(3) 0.0484(17) Uani 1 1 d . . .
H3 H 0.3711 0.2816 0.3920 0.058 Uiso 1 1 calc R . .
C18 C 0.46568(14) -0.2740(4) 0.0634(2) 0.0377(14) Uani 1 1 d . . .
H18 H 0.4469 -0.3035 0.0461 0.045 Uiso 1 1 calc R . .
C1 C 0.32745(14) 0.1911(4) 0.3257(2) 0.0358(13) Uani 1 1 d . . .
C16 C 0.4249(2) -0.0824(6) 0.1382(3) 0.063(2) Uani 1 1 d U . .
H16 H 0.4456 -0.0472 0.1441 0.076 Uiso 1 1 calc R . .
C17 C 0.3920(2) -0.0454(6) 0.1512(3) 0.061(2) Uani 1 1 d U . .
H17 H 0.3902 0.0169 0.1623 0.074 Uiso 1 1 calc R . .
C15 C 0.42772(16) -0.1701(5) 0.1166(3) 0.0424(15) Uani 1 1 d . . .
C14 C 0.39598(19) -0.2264(5) 0.1131(4) 0.069(2) Uani 1 1 d . . .
H14 H 0.3970 -0.2879 0.1005 0.083 Uiso 1 1 calc R . .
C13 C 0.3638(2) -0.1876(6) 0.1290(3) 0.063(2) Uani 1 1 d U . .
H13 H 0.3426 -0.2227 0.1266 0.075 Uiso 1 1 calc R . .
C19 C 0.51783(19) -0.2378(6) 0.0888(3) 0.057(2) Uani 1 1 d U . .
H19 H 0.5428 -0.2337 0.0914 0.069 Uiso 1 1 calc R . .
C11 C 0.2945(2) -0.0843(6) 0.1451(3) 0.063(2) Uani 1 1 d U . .
H11 H 0.2889 -0.1292 0.1202 0.076 Uiso 1 1 calc R . .
C10 C 0.2717(2) -0.0283(6) 0.1703(3) 0.062(2) Uani 1 1 d U . .
H10 H 0.2470 -0.0279 0.1649 0.075 Uiso 1 1 calc R . .
C20 C 0.4942(2) -0.1903(6) 0.1190(3) 0.067(2) Uani 1 1 d U . .
H20 H 0.4996 -0.1523 0.1471 0.081 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 0.0127(3) 0.0274(3) 0.0226(3) 0.0007(3) -0.0001(2) 0.0006(3)
O1W 0.014(2) 0.024(2) 0.025(3) 0.000 0.000 0.0015(19)
O4 0.0246(19) 0.027(2) 0.037(2) 0.0040(16) -0.0129(16) 0.0029(15)
O3 0.0185(19) 0.032(2) 0.040(2) 0.0012(16) -0.0146(16) -0.0041(15)
O1 0.023(2) 0.041(2) 0.031(2) -0.0062(17) -0.0061(16) 0.0056(16)
C5 0.020(3) 0.044(3) 0.031(3) -0.001(2) -0.009(2) 0.003(2)
N4 0.031(3) 0.058(3) 0.044(3) -0.021(3) 0.007(2) -0.015(2)
O2 0.048(2) 0.050(2) 0.068(3) -0.013(2) -0.026(2) 0.015(2)
N2 0.043(3) 0.042(3) 0.066(4) -0.023(3) 0.013(3) 0.016(2)
N1 0.028(3) 0.031(2) 0.042(3) -0.005(2) 0.004(2) 0.004(2)
N3 0.031(3) 0.038(3) 0.045(3) -0.008(2) -0.001(2) 0.003(2)
C7 0.027(3) 0.040(3) 0.049(3) -0.012(3) -0.013(3) 0.002(3)
C2 0.019(3) 0.044(3) 0.034(3) -0.003(2) -0.014(2) 0.000(2)
C4 0.042(3) 0.038(3) 0.038(3) -0.007(3) -0.022(3) 0.002(3)
C6 0.035(3) 0.034(3) 0.054(4) -0.002(3) -0.017(3) 0.000(3)
C12 0.041(4) 0.056(4) 0.060(4) -0.025(4) 0.012(3) 0.013(3)
C8 0.013(2) 0.056(4) 0.017(2) -0.001(2) -0.0017(19) 0.004(2)
C9 0.033(3) 0.049(4) 0.056(4) -0.019(3) 0.002(3) -0.003(3)
C3 0.038(3) 0.029(3) 0.079(5) -0.008(3) -0.030(3) 0.010(3)
C18 0.019(3) 0.049(4) 0.046(3) -0.024(3) 0.006(2) 0.007(3)
C1 0.022(3) 0.041(3) 0.044(3) 0.005(3) -0.012(2) 0.012(3)
C16 0.057(4) 0.058(3) 0.075(4) -0.016(3) 0.007(3) 0.001(3)
C17 0.057(4) 0.057(4) 0.070(4) -0.017(3) 0.016(3) -0.002(3)
C15 0.030(3) 0.042(3) 0.055(4) -0.018(3) 0.001(3) 0.008(3)
C14 0.045(4) 0.043(4) 0.120(7) -0.030(4) 0.037(4) -0.001(3)
C13 0.055(4) 0.062(4) 0.072(4) -0.015(3) 0.008(3) 0.004(3)
C19 0.048(3) 0.059(4) 0.065(4) -0.026(3) 0.002(3) -0.004(3)
C11 0.053(3) 0.069(4) 0.069(4) -0.025(3) -0.007(3) 0.005(3)
C10 0.050(4) 0.069(4) 0.068(4) -0.019(3) -0.007(3) 0.003(3)
C20 0.051(3) 0.078(4) 0.073(4) -0.027(3) 0.000(3) 0.005(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.047(4) . ?
Ni1 O3 2.049(4) 12_454 ?
Ni1 N1 2.051(5) . ?
Ni1 N3 2.077(5) 16_445 ?
Ni1 O4 2.082(4) 11_554 ?
Ni1 O1W 2.090(3) . ?
O1W Ni1 2.090(3) 14 ?
O4 C8 1.228(7) . ?
O4 Ni1 2.082(3) 15_545 ?
O3 C8 1.267(7) . ?
O3 Ni1 2.049(4) 4 ?
O1 C1 1.287(7) . ?
C5 C4 1.384(8) . ?
C5 C6 1.393(8) . ?
C5 C8 1.514(7) . ?
N4 C18 1.327(7) . ?
N4 C20 1.349(9) . ?
N4 C15 1.434(7) . ?
O2 C1 1.190(7) . ?
N2 C9 1.366(8) . ?
N2 C11 1.385(9) . ?
N2 C12 1.452(8) . ?
N1 C9 1.303(8) . ?
N1 C10 1.371(9) . ?
N3 C18 1.325(7) . ?
N3 C19 1.337(9) . ?
N3 Ni1 2.077(5) 8_544 ?
C7 C2 1.383(8) . ?
C7 C6 1.396(8) . ?
C7 H7 0.9300 . ?
C2 C3 1.436(8) . ?
C2 C1 1.535(7) . ?
C4 C3 1.373(8) . ?
C4 H4 0.9300 . ?
C6 H6 0.9300 . ?
C12 C17 1.326(10) . ?
C12 C13 1.344(10) . ?
C9 H9 0.9300 . ?
C3 H3 0.9300 . ?
C18 H18 0.9300 . ?
C16 C15 1.365(10) . ?
C16 C17 1.372(10) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C15 C14 1.425(9) . ?
C14 C13 1.379(9) . ?
C14 H14 0.9300 . ?
C13 H13 0.9300 . ?
C19 C20 1.356(10) . ?
C19 H19 0.9300 . ?
C11 C10 1.331(11) . ?
C11 H11 0.9300 . ?
C10 H10 0.9300 . ?
C20 H20 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O3 173.98(16) . 12_454 ?
O1 Ni1 N1 88.92(17) . . ?
O3 Ni1 N1 89.44(17) 12_454 . ?
O1 Ni1 N3 86.62(18) . 16_445 ?
O3 Ni1 N3 87.66(18) 12_454 16_445 ?
N1 Ni1 N3 92.39(19) . 16_445 ?
O1 Ni1 O4 88.41(16) . 11_554 ?
O3 Ni1 O4 97.21(15) 12_454 11_554 ?
N1 Ni1 O4 84.94(17) . 11_554 ?
N3 Ni1 O4 174.40(18) 16_445 11_554 ?
O1 Ni1 O1W 92.11(13) . . ?
O3 Ni1 O1W 89.85(12) 12_454 . ?
N1 Ni1 O1W 176.68(18) . . ?
N3 Ni1 O1W 90.83(17) 16_445 . ?
O4 Ni1 O1W 91.93(14) 11_554 . ?
Ni1 O1W Ni1 116.0(2) . 14 ?
C8 O4 Ni1 134.6(3) . 15_545 ?
C8 O3 Ni1 128.6(3) . 4 ?
C1 O1 Ni1 128.3(3) . . ?
C4 C5 C6 119.2(5) . . ?
C4 C5 C8 121.1(5) . . ?
C6 C5 C8 119.6(5) . . ?
C18 N4 C20 107.1(5) . . ?
C18 N4 C15 126.3(5) . . ?
C20 N4 C15 126.6(5) . . ?
C9 N2 C11 106.3(5) . . ?
C9 N2 C12 125.9(6) . . ?
C11 N2 C12 127.7(6) . . ?
C9 N1 C10 104.6(5) . . ?
C9 N1 Ni1 124.8(4) . . ?
C10 N1 Ni1 130.3(4) . . ?
C18 N3 C19 104.9(5) . . ?
C18 N3 Ni1 124.7(4) . 8_544 ?
C19 N3 Ni1 130.4(5) . 8_544 ?
C2 C7 C6 121.2(5) . . ?
C2 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
C7 C2 C3 118.7(5) . . ?
C7 C2 C1 122.8(5) . . ?
C3 C2 C1 118.3(5) . . ?
C3 C4 C5 122.1(5) . . ?
C3 C4 H4 119.0 . . ?
C5 C4 H4 119.0 . . ?
C5 C6 C7 119.8(5) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C17 C12 C13 122.4(6) . . ?
C17 C12 N2 119.5(6) . . ?
C13 C12 N2 118.1(6) . . ?
O4 C8 O3 127.9(5) . . ?
O4 C8 C5 116.8(5) . . ?
O3 C8 C5 115.2(5) . . ?
N1 C9 N2 111.8(6) . . ?
N1 C9 H9 124.1 . . ?
N2 C9 H9 124.1 . . ?
C4 C3 C2 118.7(5) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
N3 C18 N4 111.5(5) . . ?
N3 C18 H18 124.3 . . ?
N4 C18 H18 124.3 . . ?
O2 C1 O1 127.3(5) . . ?
O2 C1 C2 119.8(5) . . ?
O1 C1 C2 112.9(5) . . ?
C15 C16 C17 121.1(7) . . ?
C15 C16 H16 119.4 . . ?
C17 C16 H16 119.4 . . ?
C12 C17 C16 119.5(7) . . ?
C12 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C16 C15 C14 118.1(6) . . ?
C16 C15 N4 123.0(6) . . ?
C14 C15 N4 118.9(5) . . ?
C13 C14 C15 118.4(7) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
C12 C13 C14 120.1(7) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
N3 C19 C20 110.5(7) . . ?
N3 C19 H19 124.8 . . ?
C20 C19 H19 124.8 . . ?
C10 C11 N2 105.1(7) . . ?
C10 C11 H11 127.4 . . ?
N2 C11 H11 127.4 . . ?
C11 C10 N1 112.1(7) . . ?
C11 C10 H10 123.9 . . ?
N1 C10 H10 123.9 . . ?
N4 C20 C19 105.7(7) . . ?
N4 C20 H20 127.2 . . ?
C19 C20 H20 127.2 . . ?

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
O1 Ni1 O1W Ni1 128.66(12) . . . 14 ?
O3 Ni1 O1W Ni1 -57.03(11) 12_454 . . 14 ?
N1 Ni1 O1W Ni1 21(2) . . . 14 ?
N3 Ni1 O1W Ni1 -144.69(14) 16_445 . . 14 ?
O4 Ni1 O1W Ni1 40.18(11) 11_554 . . 14 ?
O3 Ni1 O1 C1 -112.0(16) 12_454 . . . ?
N1 Ni1 O1 C1 173.7(5) . . . . ?
N3 Ni1 O1 C1 -93.8(5) 16_445 . . . ?
O4 Ni1 O1 C1 88.8(5) 11_554 . . . ?
O1W Ni1 O1 C1 -3.1(5) . . . . ?
O1 Ni1 N1 C9 -19.3(5) . . . . ?
O3 Ni1 N1 C9 166.4(5) 12_454 . . . ?
N3 Ni1 N1 C9 -105.9(6) 16_445 . . . ?
O4 Ni1 N1 C9 69.2(5) 11_554 . . . ?
O1W Ni1 N1 C9 89(3) . . . . ?
O1 Ni1 N1 C10 168.0(6) . . . . ?
O3 Ni1 N1 C10 -6.2(6) 12_454 . . . ?
N3 Ni1 N1 C10 81.4(6) 16_445 . . . ?
O4 Ni1 N1 C10 -103.5(6) 11_554 . . . ?
O1W Ni1 N1 C10 -84(3) . . . . ?
C6 C7 C2 C3 -1.3(9) . . . . ?
C6 C7 C2 C1 -175.8(6) . . . . ?
C6 C5 C4 C3 4.4(10) . . . . ?
C8 C5 C4 C3 -176.2(6) . . . . ?
C4 C5 C6 C7 -1.0(9) . . . . ?
C8 C5 C6 C7 179.5(5) . . . . ?
C2 C7 C6 C5 -0.4(10) . . . . ?
C9 N2 C12 C17 -27.9(12) . . . . ?
C11 N2 C12 C17 149.9(8) . . . . ?
C9 N2 C12 C13 153.4(8) . . . . ?
C11 N2 C12 C13 -28.8(12) . . . . ?
Ni1 O4 C8 O3 24.7(9) 15_545 . . . ?
Ni1 O4 C8 C5 -154.9(4) 15_545 . . . ?
Ni1 O3 C8 O4 10.5(8) 4 . . . ?
Ni1 O3 C8 C5 -169.9(3) 4 . . . ?
C4 C5 C8 O4 168.0(5) . . . . ?
C6 C5 C8 O4 -12.6(8) . . . . ?
C4 C5 C8 O3 -11.6(8) . . . . ?
C6 C5 C8 O3 167.8(5) . . . . ?
C10 N1 C9 N2 0.0(8) . . . . ?
Ni1 N1 C9 N2 -174.2(4) . . . . ?
C11 N2 C9 N1 -0.5(9) . . . . ?
C12 N2 C9 N1 177.7(6) . . . . ?
C5 C4 C3 C2 -6.1(10) . . . . ?
C7 C2 C3 C4 4.4(10) . . . . ?
C1 C2 C3 C4 179.2(6) . . . . ?
C19 N3 C18 N4 2.5(8) . . . . ?
Ni1 N3 C18 N4 -179.0(4) 8_544 . . . ?
C20 N4 C18 N3 -5.8(8) . . . . ?
C15 N4 C18 N3 176.1(6) . . . . ?
Ni1 O1 C1 O2 -8.6(9) . . . . ?
Ni1 O1 C1 C2 168.3(4) . . . . ?
C7 C2 C1 O2 160.6(6) . . . . ?
C3 C2 C1 O2 -14.0(9) . . . . ?
C7 C2 C1 O1 -16.6(8) . . . . ?
C3 C2 C1 O1 168.8(6) . . . . ?
C13 C12 C17 C16 -4.3(14) . . . . ?
N2 C12 C17 C16 177.1(7) . . . . ?
C15 C16 C17 C12 7.1(13) . . . . ?
C17 C16 C15 C14 -6.7(12) . . . . ?
C17 C16 C15 N4 176.4(7) . . . . ?
C18 N4 C15 C16 -153.7(7) . . . . ?
C20 N4 C15 C16 28.6(12) . . . . ?
C18 N4 C15 C14 29.4(11) . . . . ?
C20 N4 C15 C14 -148.3(8) . . . . ?
C16 C15 C14 C13 3.6(12) . . . . ?
N4 C15 C14 C13 -179.4(8) . . . . ?
C17 C12 C13 C14 1.3(14) . . . . ?
N2 C12 C13 C14 179.9(8) . . . . ?
C15 C14 C13 C12 -0.9(13) . . . . ?
C18 N3 C19 C20 1.7(9) . . . . ?
Ni1 N3 C19 C20 -176.6(5) 8_544 . . . ?
C9 N2 C11 C10 0.9(9) . . . . ?
C12 N2 C11 C10 -177.3(8) . . . . ?
N2 C11 C10 N1 -0.9(10) . . . . ?
C9 N1 C10 C11 0.6(9) . . . . ?
Ni1 N1 C10 C11 174.4(6) . . . . ?
C18 N4 C20 C19 6.5(9) . . . . ?
C15 N4 C20 C19 -175.4(7) . . . . ?
N3 C19 C20 N4 -5.2(10) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.087

# Attachment '2.cif'

data_mm
_database_code_depnum_ccdc_archive 'CCDC 695644'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H75 N13 Ni2 O14'
_chemical_formula_weight         1319.75

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'
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   C2/c

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

_cell_length_a                   14.248(4)
_cell_length_b                   26.912(9)
_cell_length_c                   18.125(3)
_cell_angle_alpha                90.000
_cell_angle_beta                 100.584(6)
_cell_angle_gamma                90.000
_cell_volume                     6832(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.52
_cell_measurement_theta_max      30.85

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2776
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8604
_exptl_absorpt_correction_T_max  0.9293
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_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  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17102
_diffrn_reflns_av_R_equivalents  0.0793
_diffrn_reflns_av_sigmaI/netI    0.1137
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         24.99
_reflns_number_total             6001
_reflns_number_gt                3368
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1997)'
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 1997)'

_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^)+(0.0088P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6001
_refine_ls_number_parameters     267
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.0669
_refine_ls_wR_factor_gt          0.0638
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_restrained_S_all      1.025
_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 0.37506(3) 0.393544(15) 0.22649(2) 0.02514(11) Uani 1 1 d . . .
O1 O 0.43684(14) 0.44513(7) 0.16794(11) 0.0329(6) Uani 1 1 d . . .
O4 O 0.45643(15) 0.30323(9) 0.12632(13) 0.0586(7) Uani 1 1 d U . .
O2 O 0.59141(13) 0.42819(7) 0.17003(10) 0.0320(6) Uani 1 1 d . . .
N2 N 0.13396(18) 0.47490(10) 0.12781(16) 0.0414(8) Uani 1 1 d . . .
O3 O 0.33157(13) 0.35427(8) 0.12549(11) 0.0344(6) Uani 1 1 d . . .
O1W O 0.5000 0.35102(9) 0.2500 0.0244(7) Uani 1 2 d S . .
C2 C 0.5066(2) 0.47510(11) 0.06890(16) 0.0262(8) Uani 1 1 d . . .
N1 N 0.25437(17) 0.43670(10) 0.19946(15) 0.0346(7) Uani 1 1 d . . .
N4 N 0.2573(2) 0.29085(11) 0.35931(18) 0.0515(9) Uani 1 1 d . . .
C3 C 0.4212(2) 0.49452(12) 0.03303(18) 0.0454(10) Uani 1 1 d . . .
H3 H 0.3670 0.4908 0.0544 0.055 Uiso 1 1 calc R . .
C6 C 0.3078(2) 0.28259(12) 0.04903(18) 0.0368(9) Uani 1 1 d . . .
C12 C 0.0660(2) 0.48794(13) 0.0630(2) 0.0402(10) Uani 1 1 d . . .
C18 C 0.2537(3) 0.26951(13) 0.4303(2) 0.0483(11) Uani 1 1 d . . .
C5 C 0.3700(2) 0.31633(13) 0.10398(18) 0.0360(9) Uani 1 1 d . . .
N3 N 0.30202(17) 0.34029(10) 0.27460(15) 0.0370(7) Uani 1 1 d . . .
C1 C 0.5124(2) 0.44697(11) 0.14164(17) 0.0250(8) Uani 1 1 d . . .
C8 C 0.1556(2) 0.26100(13) -0.02361(19) 0.0513(11) Uani 1 1 d . . .
H8 H 0.0914 0.2686 -0.0395 0.062 Uiso 1 1 calc R . .
C4 C 0.4147(2) 0.51978(13) -0.03520(18) 0.0442(10) Uani 1 1 d . . .
H4 H 0.3566 0.5333 -0.0581 0.053 Uiso 1 1 calc R . .
C9 C 0.2019(2) 0.43927(13) 0.13244(19) 0.0435(10) Uani 1 1 d . . .
H9 H 0.2102 0.4190 0.0926 0.052 Uiso 1 1 calc R . .
C13 C -0.0112(2) 0.51586(13) 0.0699(2) 0.0529(11) Uani 1 1 d U . .
H13 H -0.0197 0.5267 0.1170 0.064 Uiso 1 1 calc R . .
C7 C 0.2125(2) 0.29307(12) 0.02466(19) 0.0454(10) Uani 1 1 d . . .
H7 H 0.1864 0.3219 0.0408 0.055 Uiso 1 1 calc R . .
C15 C 0.3191(2) 0.32565(12) 0.34571(19) 0.0420(10) Uani 1 1 d . . .
H15 H 0.3682 0.3381 0.3819 0.050 Uiso 1 1 calc R . .
C19 C 0.1682(3) 0.25643(14) 0.4483(2) 0.0643(12) Uani 1 1 d . . .
H19 H 0.1122 0.2608 0.4135 0.077 Uiso 1 1 calc R . .
C20 C 0.1643(3) 0.23648(14) 0.5188(2) 0.0671(13) Uani 1 1 d . . .
H20 H 0.1060 0.2273 0.5308 0.081 Uiso 1 1 calc R . .
C14 C -0.0774(2) 0.52808(14) 0.0064(2) 0.0602(12) Uani 1 1 d U . .
H14 H -0.1301 0.5474 0.0110 0.072 Uiso 1 1 calc R . .
C11 C 0.1444(3) 0.49616(14) 0.1980(2) 0.0705(13) Uani 1 1 d U . .
H11 H 0.1078 0.5215 0.2131 0.085 Uiso 1 1 calc R . .
C16 C 0.2241(3) 0.31217(14) 0.2425(2) 0.0666(13) Uani 1 1 d U . .
H16 H 0.1949 0.3140 0.1923 0.080 Uiso 1 1 calc R . .
C10 C 0.2197(3) 0.47210(14) 0.2407(2) 0.0640(12) Uani 1 1 d U . .
H10 H 0.2438 0.4790 0.2909 0.077 Uiso 1 1 calc R . .
C17 C 0.1958(3) 0.28166(16) 0.2936(2) 0.0776(14) Uani 1 1 d U . .
H17 H 0.1453 0.2592 0.2857 0.093 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 0.0283(2) 0.0281(2) 0.0168(2) 0.0003(2) -0.00148(17) -0.0003(3)
O1 0.0328(13) 0.0382(15) 0.0296(14) 0.0129(11) 0.0106(12) 0.0039(12)
O4 0.0391(14) 0.0634(17) 0.0648(18) -0.0351(14) -0.0130(13) 0.0044(13)
O2 0.0325(13) 0.0407(15) 0.0203(13) 0.0088(11) -0.0017(11) 0.0032(11)
N2 0.0393(18) 0.050(2) 0.0301(19) -0.0041(16) -0.0072(15) 0.0194(16)
O3 0.0393(14) 0.0323(14) 0.0272(14) -0.0084(11) -0.0056(11) 0.0032(12)
O1W 0.0207(16) 0.0213(17) 0.0281(19) 0.000 -0.0035(14) 0.000
C2 0.0283(19) 0.029(2) 0.020(2) 0.0107(15) 0.0012(16) 0.0049(17)
N1 0.0328(17) 0.040(2) 0.0285(19) -0.0063(15) -0.0003(15) 0.0062(14)
N4 0.063(2) 0.051(2) 0.043(2) 0.0142(18) 0.0167(19) -0.0215(18)
C3 0.033(2) 0.066(3) 0.038(2) 0.024(2) 0.0098(19) 0.007(2)
C6 0.033(2) 0.037(2) 0.036(2) -0.0177(18) -0.0067(18) 0.0019(18)
C12 0.036(2) 0.046(2) 0.033(2) 0.0053(19) -0.0091(19) 0.0111(19)
C18 0.056(3) 0.047(3) 0.046(3) 0.011(2) 0.019(2) -0.003(2)
C5 0.036(2) 0.040(2) 0.027(2) -0.0115(18) -0.0045(18) -0.001(2)
N3 0.0343(17) 0.0431(19) 0.0319(19) 0.0034(15) 0.0017(15) -0.0036(15)
C1 0.034(2) 0.0202(19) 0.019(2) -0.0018(15) 0.0016(17) -0.0027(17)
C8 0.031(2) 0.057(3) 0.056(3) -0.025(2) -0.017(2) 0.012(2)
C4 0.0235(19) 0.074(3) 0.034(2) 0.023(2) 0.0023(18) 0.0080(19)
C9 0.046(2) 0.045(3) 0.034(2) -0.0079(19) -0.0086(19) 0.014(2)
C13 0.055(2) 0.064(2) 0.037(2) -0.003(2) 0.0010(19) 0.022(2)
C7 0.036(2) 0.045(2) 0.050(3) -0.029(2) -0.0072(19) 0.0069(19)
C15 0.045(2) 0.045(2) 0.035(2) 0.011(2) 0.006(2) -0.008(2)
C19 0.060(3) 0.073(3) 0.061(3) 0.028(2) 0.015(2) -0.014(2)
C20 0.062(3) 0.072(3) 0.074(3) 0.033(3) 0.030(3) -0.011(3)
C14 0.053(2) 0.072(3) 0.050(3) -0.003(2) -0.003(2) 0.033(2)
C11 0.072(3) 0.071(3) 0.061(3) -0.015(2) -0.008(2) 0.040(2)
C16 0.073(3) 0.075(3) 0.047(3) 0.000(2) -0.004(2) -0.033(2)
C10 0.066(3) 0.072(3) 0.047(3) -0.012(2) -0.007(2) 0.026(2)
C17 0.090(3) 0.082(3) 0.061(3) 0.010(2) 0.015(2) -0.042(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 O1 2.043(2) . ?
Ni1 N3 2.057(3) . ?
Ni1 N1 2.058(3) . ?
Ni1 O2 2.070(2) 2_655 ?
Ni1 O1W 2.0932(15) . ?
Ni1 O3 2.106(2) . ?
O1 C1 1.256(3) . ?
O4 C5 1.273(3) . ?
O2 C1 1.255(3) . ?
O2 Ni1 2.070(2) 2_655 ?
N2 C9 1.354(3) . ?
N2 C11 1.378(4) . ?
N2 C12 1.423(4) . ?
O3 C5 1.254(3) . ?
O1W Ni1 2.0932(15) 2_655 ?
C2 C3 1.374(4) . ?
C2 C4 1.378(4) 5_665 ?
C2 C1 1.509(4) . ?
N1 C9 1.306(3) . ?
N1 C10 1.359(4) . ?
N4 C15 1.338(3) . ?
N4 C17 1.365(4) . ?
N4 C18 1.419(4) . ?
C3 C4 1.399(4) . ?
C3 H3 0.9300 . ?
C6 C7 1.378(4) . ?
C6 C8 1.396(4) 7 ?
C6 C5 1.509(4) . ?
C12 C13 1.357(4) . ?
C12 C14 1.367(4) 5_565 ?
C18 C20 1.359(5) 7_556 ?
C18 C19 1.364(4) . ?
N3 C15 1.327(3) . ?
N3 C16 1.380(4) . ?
C8 C7 1.381(4) . ?
C8 C6 1.396(4) 7 ?
C8 H8 0.9300 . ?
C4 C2 1.378(4) 5_665 ?
C4 H4 0.9300 . ?
C9 H9 0.9300 . ?
C13 C14 1.388(4) . ?
C13 H13 0.9300 . ?
C7 H7 0.9300 . ?
C15 H15 0.9300 . ?
C19 C20 1.395(5) . ?
C19 H19 0.9300 . ?
C20 C18 1.359(5) 7_556 ?
C20 H20 0.9300 . ?
C14 C12 1.367(4) 5_565 ?
C14 H14 0.9300 . ?
C11 C10 1.366(4) . ?
C11 H11 0.9300 . ?
C16 C17 1.353(4) . ?
C16 H16 0.9300 . ?
C10 H10 0.9300 . ?
C17 H17 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 N3 173.61(10) . . ?
O1 Ni1 N1 85.05(9) . . ?
N3 Ni1 N1 91.63(10) . . ?
O1 Ni1 O2 96.60(8) . 2_655 ?
N3 Ni1 O2 88.87(10) . 2_655 ?
N1 Ni1 O2 90.30(9) . 2_655 ?
O1 Ni1 O1W 92.62(7) . . ?
N3 Ni1 O1W 90.60(9) . . ?
N1 Ni1 O1W 177.49(8) . . ?
O2 Ni1 O1W 90.90(6) 2_655 . ?
O1 Ni1 O3 88.60(8) . . ?
N3 Ni1 O3 85.86(10) . . ?
N1 Ni1 O3 88.67(9) . . ?
O2 Ni1 O3 174.60(8) 2_655 . ?
O1W Ni1 O3 90.34(7) . . ?
C1 O1 Ni1 134.9(2) . . ?
C1 O2 Ni1 126.4(2) . 2_655 ?
C9 N2 C11 106.4(3) . . ?
C9 N2 C12 126.6(3) . . ?
C11 N2 C12 127.0(3) . . ?
C5 O3 Ni1 127.1(2) . . ?
Ni1 O1W Ni1 113.72(12) 2_655 . ?
C3 C2 C4 118.3(3) . 5_665 ?
C3 C2 C1 120.4(3) . . ?
C4 C2 C1 121.3(3) 5_665 . ?
C9 N1 C10 105.7(3) . . ?
C9 N1 Ni1 124.2(2) . . ?
C10 N1 Ni1 129.6(2) . . ?
C15 N4 C17 107.7(3) . . ?
C15 N4 C18 125.8(3) . . ?
C17 N4 C18 126.4(3) . . ?
C2 C3 C4 120.8(3) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C7 C6 C8 118.2(3) . 7 ?
C7 C6 C5 120.9(3) . . ?
C8 C6 C5 120.9(3) 7 . ?
C13 C12 C14 119.7(3) . 5_565 ?
C13 C12 N2 120.0(3) . . ?
C14 C12 N2 120.3(3) 5_565 . ?
C20 C18 C19 120.1(4) 7_556 . ?
C20 C18 N4 119.6(4) 7_556 . ?
C19 C18 N4 120.3(4) . . ?
O3 C5 O4 125.4(3) . . ?
O3 C5 C6 117.2(3) . . ?
O4 C5 C6 117.4(3) . . ?
C15 N3 C16 103.6(3) . . ?
C15 N3 Ni1 127.0(2) . . ?
C16 N3 Ni1 129.3(3) . . ?
O2 C1 O1 126.5(3) . . ?
O2 C1 C2 117.5(3) . . ?
O1 C1 C2 116.0(3) . . ?
C7 C8 C6 121.5(3) . 7 ?
C7 C8 H8 119.2 . . ?
C6 C8 H8 119.2 7 . ?
C2 C4 C3 120.9(3) 5_665 . ?
C2 C4 H4 119.6 5_665 . ?
C3 C4 H4 119.6 . . ?
N1 C9 N2 112.1(3) . . ?
N1 C9 H9 124.0 . . ?
N2 C9 H9 124.0 . . ?
C12 C13 C14 119.5(3) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C6 C7 C8 120.3(3) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
N3 C15 N4 112.2(3) . . ?
N3 C15 H15 123.9 . . ?
N4 C15 H15 123.9 . . ?
C18 C19 C20 120.4(4) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C18 C20 C19 119.5(4) 7_556 . ?
C18 C20 H20 120.2 7_556 . ?
C19 C20 H20 120.2 . . ?
C12 C14 C13 120.7(3) 5_565 . ?
C12 C14 H14 119.6 5_565 . ?
C13 C14 H14 119.6 . . ?
C10 C11 N2 105.4(3) . . ?
C10 C11 H11 127.3 . . ?
N2 C11 H11 127.3 . . ?
C17 C16 N3 111.2(4) . . ?
C17 C16 H16 124.4 . . ?
N3 C16 H16 124.4 . . ?
N1 C10 C11 110.4(4) . . ?
N1 C10 H10 124.8 . . ?
C11 C10 H10 124.8 . . ?
C16 C17 N4 105.2(4) . . ?
C16 C17 H17 127.4 . . ?
N4 C17 H17 127.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Ni1 O1 C1 -107.1(8) . . . . ?
N1 Ni1 O1 C1 -166.0(3) . . . . ?
O2 Ni1 O1 C1 104.3(3) 2_655 . . . ?
O1W Ni1 O1 C1 13.1(3) . . . . ?
O3 Ni1 O1 C1 -77.2(3) . . . . ?
O1 Ni1 O3 C5 101.0(3) . . . . ?
N3 Ni1 O3 C5 -82.2(3) . . . . ?
N1 Ni1 O3 C5 -173.9(3) . . . . ?
O2 Ni1 O3 C5 -94.9(9) 2_655 . . . ?
O1W Ni1 O3 C5 8.4(3) . . . . ?
O1 Ni1 O1W Ni1 38.49(6) . . . 2_655 ?
N3 Ni1 O1W Ni1 -147.03(8) . . . 2_655 ?
N1 Ni1 O1W Ni1 60(2) . . . 2_655 ?
O2 Ni1 O1W Ni1 -58.15(6) 2_655 . . 2_655 ?
O3 Ni1 O1W Ni1 127.10(6) . . . 2_655 ?
O1 Ni1 N1 C9 72.9(3) . . . . ?
N3 Ni1 N1 C9 -101.7(3) . . . . ?
O2 Ni1 N1 C9 169.4(3) 2_655 . . . ?
O1W Ni1 N1 C9 51(2) . . . . ?
O3 Ni1 N1 C9 -15.9(3) . . . . ?
O1 Ni1 N1 C10 -97.4(3) . . . . ?
N3 Ni1 N1 C10 88.1(3) . . . . ?
O2 Ni1 N1 C10 -0.8(3) 2_655 . . . ?
O1W Ni1 N1 C10 -119(2) . . . . ?
O3 Ni1 N1 C10 173.9(3) . . . . ?
C4 C2 C3 C4 -1.3(6) 5_665 . . . ?
C1 C2 C3 C4 -178.7(3) . . . . ?
C9 N2 C12 C13 164.7(3) . . . . ?
C11 N2 C12 C13 -15.9(5) . . . . ?
C9 N2 C12 C14 -14.5(5) . . . 5_565 ?
C11 N2 C12 C14 165.0(4) . . . 5_565 ?
C15 N4 C18 C20 -32.7(6) . . . 7_556 ?
C17 N4 C18 C20 150.9(4) . . . 7_556 ?
C15 N4 C18 C19 145.3(4) . . . . ?
C17 N4 C18 C19 -31.0(6) . . . . ?
Ni1 O3 C5 O4 -22.8(5) . . . . ?
Ni1 O3 C5 C6 155.0(2) . . . . ?
C7 C6 C5 O3 -0.8(5) . . . . ?
C8 C6 C5 O3 -178.5(3) 7 . . . ?
C7 C6 C5 O4 177.2(3) . . . . ?
C8 C6 C5 O4 -0.5(5) 7 . . . ?
O1 Ni1 N3 C15 -176.8(7) . . . . ?
N1 Ni1 N3 C15 -118.2(3) . . . . ?
O2 Ni1 N3 C15 -28.0(3) 2_655 . . . ?
O1W Ni1 N3 C15 62.9(3) . . . . ?
O3 Ni1 N3 C15 153.2(3) . . . . ?
O1 Ni1 N3 C16 1.9(10) . . . . ?
N1 Ni1 N3 C16 60.5(3) . . . . ?
O2 Ni1 N3 C16 150.8(3) 2_655 . . . ?
O1W Ni1 N3 C16 -118.4(3) . . . . ?
O3 Ni1 N3 C16 -28.1(3) . . . . ?
Ni1 O2 C1 O1 -5.7(4) 2_655 . . . ?
Ni1 O2 C1 C2 173.79(18) 2_655 . . . ?
Ni1 O1 C1 O2 -34.9(5) . . . . ?
Ni1 O1 C1 C2 145.6(2) . . . . ?
C3 C2 C1 O2 176.9(3) . . . . ?
C4 C2 C1 O2 -0.4(4) 5_665 . . . ?
C3 C2 C1 O1 -3.6(4) . . . . ?
C4 C2 C1 O1 179.1(3) 5_665 . . . ?
C2 C3 C4 C2 1.4(6) . . . 5_665 ?
C10 N1 C9 N2 0.0(4) . . . . ?
Ni1 N1 C9 N2 -172.3(2) . . . . ?
C11 N2 C9 N1 -0.5(4) . . . . ?
C12 N2 C9 N1 179.0(3) . . . . ?
C14 C12 C13 C14 -0.4(6) 5_565 . . . ?
N2 C12 C13 C14 -179.6(3) . . . . ?
C8 C6 C7 C8 0.0(6) 7 . . . ?
C5 C6 C7 C8 -177.8(3) . . . . ?
C6 C8 C7 C6 0.0(6) 7 . . . ?
C16 N3 C15 N4 -0.1(4) . . . . ?
Ni1 N3 C15 N4 178.8(2) . . . . ?
C17 N4 C15 N3 0.2(4) . . . . ?
C18 N4 C15 N3 -176.7(3) . . . . ?
C20 C18 C19 C20 -0.5(7) 7_556 . . . ?
N4 C18 C19 C20 -178.5(3) . . . . ?
C18 C19 C20 C18 0.5(7) . . . 7_556 ?
C12 C13 C14 C12 0.4(6) . . . 5_565 ?
C9 N2 C11 C10 0.8(4) . . . . ?
C12 N2 C11 C10 -178.7(3) . . . . ?
C15 N3 C16 C17 0.1(4) . . . . ?
Ni1 N3 C16 C17 -178.9(3) . . . . ?
C9 N1 C10 C11 0.6(4) . . . . ?
Ni1 N1 C10 C11 172.2(2) . . . . ?
N2 C11 C10 N1 -0.8(4) . . . . ?
N3 C16 C17 N4 0.0(5) . . . . ?
C15 N4 C17 C16 -0.1(4) . . . . ?
C18 N4 C17 C16 176.7(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.053