# 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_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'Jian-Zhong Cui'
_publ_contact_author_email       CUIJIANZHONG@TJU.EDU.CN
loop_
_publ_author_name
'Jian-Zhong Cui'
'Peng Cheng'
'Hong-Ling Gao'
'Fan-Li Lu'
;
Ying-Ping Quan
;
'Wei Shi'
'Ai-Hong Yang'
'Li-Hua Zhao'

data_r71108e
_database_code_depnum_ccdc_archive 'CCDC 705859'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H14 N4 Ni O10'
_chemical_formula_weight         529.06

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   P2(1)/n

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

_cell_length_a                   8.0552(16)
_cell_length_b                   25.966(5)
_cell_length_c                   9.888(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.59(3)
_cell_angle_gamma                90.00
_cell_volume                     1971.5(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    4014
_cell_measurement_theta_min      2.161
_cell_measurement_theta_max      27.960

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1080
_exptl_absorpt_coefficient_mu    1.057
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9202
_exptl_absorpt_correction_T_max  0.9792
_exptl_absorpt_process_details   crystalclear

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  confocal
_diffrn_measurement_device_type  'rigaku saturn'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            12061
_diffrn_reflns_av_R_equivalents  0.0956
_diffrn_reflns_av_sigmaI/netI    0.0952
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.30
_diffrn_reflns_theta_max         25.02
_reflns_number_total             3489
_reflns_number_gt                2699
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       crystalclear
_computing_cell_refinement       crystalclear
_computing_data_reduction        crystalclear
_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)+(0.0479P)²+0.0000P] 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         3489
_refine_ls_number_parameters     317
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0614
_refine_ls_wR_factor_ref         0.1292
_refine_ls_wR_factor_gt          0.1173
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_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 0.53129(7) 0.37987(2) 0.81556(7) 0.0181(2) Uani 1 1 d . . .
O1 O 0.7299(4) 0.32460(11) 0.8668(3) 0.0216(7) Uani 1 1 d . . .
O2 O 0.7854(4) 0.24069(11) 0.8864(4) 0.0281(9) Uani 1 1 d . . .
O3 O 0.6283(4) 0.16012(12) 0.8184(4) 0.0383(10) Uani 1 1 d . . .
H3 H 0.6758 0.1885 0.8475 0.057 Uiso 1 1 calc R . .
O4 O 0.3667(4) 0.13224(11) 0.6988(4) 0.0270(8) Uani 1 1 d . . .
O5 O -0.1215(4) 0.21740(13) 0.5841(4) 0.0372(10) Uani 1 1 d . . .
O6 O -0.1587(4) 0.30084(13) 0.5772(4) 0.0406(11) Uani 1 1 d . . .
H6A H -0.1107 0.3304 0.5981 0.049 Uiso 1 1 d R . .
O7 O 0.0012(4) 0.38016(12) 0.6351(4) 0.0331(9) Uani 1 1 d . . .
O8 O 0.2738(4) 0.40462(11) 0.7435(3) 0.0196(7) Uani 1 1 d . . .
O9 O 0.5292(4) 0.37438(11) 1.0248(4) 0.0252(8) Uani 1 1 d . . .
H9A H 0.4552 0.3501 1.0133 0.030 Uiso 1 1 d R . .
H9B H 0.6331 0.3672 1.0748 0.030 Uiso 1 1 d R . .
N1 N 0.3982(4) 0.31282(13) 0.7605(4) 0.0191(9) Uani 1 1 d . . .
N2 N 0.2201(4) 0.22408(13) 0.6875(4) 0.0196(9) Uani 1 1 d . . .
N3 N 0.5648(4) 0.39295(13) 0.6203(4) 0.0199(9) Uani 1 1 d . . .
N4 N 0.6574(4) 0.44937(13) 0.8569(4) 0.0192(9) Uani 1 1 d . . .
C1 C 0.6844(5) 0.27878(18) 0.8491(5) 0.0210(11) Uani 1 1 d . . .
C2 C 0.4883(5) 0.26866(16) 0.7820(5) 0.0180(10) Uani 1 1 d . . .
C3 C 0.3934(5) 0.22251(16) 0.7415(5) 0.0189(10) Uani 1 1 d . . .
C4 C 0.4641(6) 0.16749(17) 0.7515(5) 0.0243(11) Uani 1 1 d . . .
C5 C 0.1617(6) 0.37125(17) 0.6953(6) 0.0250(11) Uani 1 1 d . . .
C6 C 0.2240(5) 0.31491(16) 0.7061(5) 0.0187(10) Uani 1 1 d . . .
C7 C 0.1337(5) 0.26823(16) 0.6688(5) 0.0182(10) Uani 1 1 d . . .
C8 C -0.0643(6) 0.26076(19) 0.6065(5) 0.0259(12) Uani 1 1 d . . .
C9 C 0.5203(5) 0.36437(17) 0.5044(5) 0.0203(10) Uani 1 1 d . . .
H9 H 0.4655 0.3322 0.5076 0.024 Uiso 1 1 calc R . .
C10 C 0.5492(6) 0.37873(17) 0.3782(5) 0.0256(11) Uani 1 1 d . . .
H10 H 0.5139 0.3569 0.2974 0.031 Uiso 1 1 calc R . .
C11 C 0.6293(6) 0.42470(16) 0.3720(5) 0.0239(11) Uani 1 1 d . . .
H11 H 0.6489 0.4353 0.2861 0.029 Uiso 1 1 calc R . .
C12 C 0.6824(5) 0.45610(17) 0.4925(5) 0.0220(11) Uani 1 1 d . . .
C13 C 0.7717(6) 0.50422(17) 0.4988(6) 0.0268(12) Uani 1 1 d . . .
H13 H 0.7986 0.5163 0.4171 0.032 Uiso 1 1 calc R . .
C14 C 0.8187(6) 0.53296(17) 0.6195(6) 0.0278(12) Uani 1 1 d . . .
H14 H 0.8772 0.5648 0.6206 0.033 Uiso 1 1 calc R . .
C15 C 0.7816(5) 0.51602(16) 0.7439(5) 0.0229(11) Uani 1 1 d . . .
C16 C 0.8222(6) 0.54498(17) 0.8700(6) 0.0286(12) Uani 1 1 d . . .
H16 H 0.8789 0.5773 0.8761 0.034 Uiso 1 1 calc R . .
C17 C 0.7784(6) 0.52572(17) 0.9847(6) 0.0307(13) Uani 1 1 d . . .
H17 H 0.8029 0.5450 1.0702 0.037 Uiso 1 1 calc R . .
C18 C 0.6976(6) 0.47761(16) 0.9741(5) 0.0248(11) Uani 1 1 d . . .
H18 H 0.6702 0.4645 1.0545 0.030 Uiso 1 1 calc R . .
C19 C 0.6964(5) 0.46860(16) 0.7422(5) 0.0183(10) Uani 1 1 d . . .
C20 C 0.6469(5) 0.43897(16) 0.6139(5) 0.0169(10) Uani 1 1 d . . .
O10 O 0.0961(4) 0.34271(13) 0.9476(4) 0.0417(10) Uani 1 1 d . . .
H10A H 0.1469 0.3172 0.9977 0.050 Uiso 1 1 d R . .
H10B H -0.0154 0.3423 0.9233 0.050 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 N1 2.031(3) . ?
Ni1 N4 2.051(3) . ?
Ni1 N3 2.057(4) . ?
Ni1 O9 2.079(3) . ?
Ni1 O8 2.081(3) . ?
Ni1 O1 2.094(3) . ?
O1 C1 1.241(5) . ?
O2 C1 1.263(5) . ?
O3 C4 1.301(5) . ?
O3 H3 0.8400 . ?
O4 C4 1.216(5) . ?
O5 C8 1.211(5) . ?
O6 C8 1.270(5) . ?
O6 H6A 0.8552 . ?
O7 C5 1.270(5) . ?
O8 C5 1.239(5) . ?
O9 H9A 0.8505 . ?
O9 H9B 0.8541 . ?
N1 C2 1.339(5) . ?
N1 C6 1.343(5) . ?
N2 C7 1.325(5) . ?
N2 C3 1.336(5) . ?
N3 C9 1.321(6) . ?
N3 C20 1.376(5) . ?
N4 C18 1.326(6) . ?
N4 C19 1.361(6) . ?
C1 C2 1.540(6) . ?
C2 C3 1.413(6) . ?
C3 C4 1.530(6) . ?
C5 C6 1.540(6) . ?
C6 C7 1.404(6) . ?
C7 C8 1.539(6) . ?
C9 C10 1.387(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.367(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.400(7) . ?
C11 H11 0.9500 . ?
C12 C20 1.389(7) . ?
C12 C13 1.434(6) . ?
C13 C14 1.360(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.421(7) . ?
C14 H14 0.9500 . ?
C15 C19 1.407(6) . ?
C15 C16 1.407(7) . ?
C16 C17 1.379(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.398(6) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.434(6) . ?
O10 H10A 0.8552 . ?
O10 H10B 0.8568 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N4 175.97(15) . . ?
N1 Ni1 N3 95.63(15) . . ?
N4 Ni1 N3 81.05(15) . . ?
N1 Ni1 O9 92.62(14) . . ?
N4 Ni1 O9 90.81(14) . . ?
N3 Ni1 O9 171.22(13) . . ?
N1 Ni1 O8 77.42(12) . . ?
N4 Ni1 O8 100.29(12) . . ?
N3 Ni1 O8 91.59(13) . . ?
O9 Ni1 O8 93.13(13) . . ?
N1 Ni1 O1 77.30(12) . . ?
N4 Ni1 O1 105.00(12) . . ?
N3 Ni1 O1 91.88(13) . . ?
O9 Ni1 O1 87.01(12) . . ?
O8 Ni1 O1 154.70(11) . . ?
C1 O1 Ni1 116.8(3) . . ?
C4 O3 H3 109.5 . . ?
C8 O6 H6A 118.9 . . ?
C5 O8 Ni1 116.8(3) . . ?
Ni1 O9 H9A 97.7 . . ?
Ni1 O9 H9B 106.8 . . ?
H9A O9 H9B 116.1 . . ?
C2 N1 C6 123.3(4) . . ?
C2 N1 Ni1 118.3(3) . . ?
C6 N1 Ni1 118.4(3) . . ?
C7 N2 C3 121.6(4) . . ?
C9 N3 C20 117.1(4) . . ?
C9 N3 Ni1 130.1(3) . . ?
C20 N3 Ni1 112.8(3) . . ?
C18 N4 C19 117.9(4) . . ?
C18 N4 Ni1 129.5(3) . . ?
C19 N4 Ni1 112.5(3) . . ?
O1 C1 O2 125.0(4) . . ?
O1 C1 C2 116.4(4) . . ?
O2 C1 C2 118.6(4) . . ?
N1 C2 C3 117.4(4) . . ?
N1 C2 C1 111.0(4) . . ?
C3 C2 C1 131.6(4) . . ?
N2 C3 C2 119.9(4) . . ?
N2 C3 C4 112.2(4) . . ?
C2 C3 C4 127.9(4) . . ?
O4 C4 O3 122.1(4) . . ?
O4 C4 C3 119.7(4) . . ?
O3 C4 C3 118.1(4) . . ?
O8 C5 O7 125.0(4) . . ?
O8 C5 C6 117.0(4) . . ?
O7 C5 C6 118.0(4) . . ?
N1 C6 C7 117.7(4) . . ?
N1 C6 C5 110.2(4) . . ?
C7 C6 C5 132.0(4) . . ?
N2 C7 C6 120.1(4) . . ?
N2 C7 C8 112.6(4) . . ?
C6 C7 C8 127.3(4) . . ?
O5 C8 O6 123.5(4) . . ?
O5 C8 C7 118.8(4) . . ?
O6 C8 C7 117.7(4) . . ?
N3 C9 C10 123.6(4) . . ?
N3 C9 H9 118.2 . . ?
C10 C9 H9 118.2 . . ?
C11 C10 C9 119.0(5) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C10 C11 C12 119.8(5) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C20 C12 C11 117.4(4) . . ?
C20 C12 C13 118.2(5) . . ?
C11 C12 C13 124.4(5) . . ?
C14 C13 C12 121.3(5) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C13 C14 C15 120.9(4) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 H14 119.5 . . ?
C19 C15 C16 117.4(5) . . ?
C19 C15 C14 119.3(4) . . ?
C16 C15 C14 123.3(4) . . ?
C17 C16 C15 119.1(4) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
C16 C17 C18 119.4(5) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
N4 C18 C17 123.1(5) . . ?
N4 C18 H18 118.5 . . ?
C17 C18 H18 118.5 . . ?
N4 C19 C15 123.1(4) . . ?
N4 C19 C20 117.9(4) . . ?
C15 C19 C20 119.0(4) . . ?
N3 C20 C12 123.0(4) . . ?
N3 C20 C19 115.7(4) . . ?
C12 C20 C19 121.2(4) . . ?
H10A O10 H10B 115.5 . . ?

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 O1 C1 -2.9(3) . . . . ?
N4 Ni1 O1 C1 -179.5(3) . . . . ?
N3 Ni1 O1 C1 -98.2(3) . . . . ?
O9 Ni1 O1 C1 90.5(3) . . . . ?
O8 Ni1 O1 C1 -0.5(5) . . . . ?
N1 Ni1 O8 C5 -3.5(3) . . . . ?
N4 Ni1 O8 C5 173.1(3) . . . . ?
N3 Ni1 O8 C5 91.9(4) . . . . ?
O9 Ni1 O8 C5 -95.5(3) . . . . ?
O1 Ni1 O8 C5 -5.9(5) . . . . ?
N4 Ni1 N1 C2 126.3(19) . . . . ?
N3 Ni1 N1 C2 91.6(4) . . . . ?
O9 Ni1 N1 C2 -85.4(3) . . . . ?
O8 Ni1 N1 C2 -178.0(4) . . . . ?
O1 Ni1 N1 C2 1.0(3) . . . . ?
N4 Ni1 N1 C6 -55(2) . . . . ?
N3 Ni1 N1 C6 -89.3(4) . . . . ?
O9 Ni1 N1 C6 93.7(4) . . . . ?
O8 Ni1 N1 C6 1.1(3) . . . . ?
O1 Ni1 N1 C6 -179.9(4) . . . . ?
N1 Ni1 N3 C9 -3.3(4) . . . . ?
N4 Ni1 N3 C9 179.0(4) . . . . ?
O9 Ni1 N3 C9 156.7(7) . . . . ?
O8 Ni1 N3 C9 -80.8(4) . . . . ?
O1 Ni1 N3 C9 74.1(4) . . . . ?
N1 Ni1 N3 C20 176.8(3) . . . . ?
N4 Ni1 N3 C20 -0.9(3) . . . . ?
O9 Ni1 N3 C20 -23.3(10) . . . . ?
O8 Ni1 N3 C20 99.2(3) . . . . ?
O1 Ni1 N3 C20 -105.8(3) . . . . ?
N1 Ni1 N4 C18 142.8(19) . . . . ?
N3 Ni1 N4 C18 177.7(4) . . . . ?
O9 Ni1 N4 C18 -5.6(4) . . . . ?
O8 Ni1 N4 C18 87.7(4) . . . . ?
O1 Ni1 N4 C18 -92.8(4) . . . . ?
N1 Ni1 N4 C19 -34(2) . . . . ?
N3 Ni1 N4 C19 0.6(3) . . . . ?
O9 Ni1 N4 C19 177.2(3) . . . . ?
O8 Ni1 N4 C19 -89.4(3) . . . . ?
O1 Ni1 N4 C19 90.1(3) . . . . ?
Ni1 O1 C1 O2 -173.3(4) . . . . ?
Ni1 O1 C1 C2 4.0(5) . . . . ?
C6 N1 C2 C3 1.6(7) . . . . ?
Ni1 N1 C2 C3 -179.3(3) . . . . ?
C6 N1 C2 C1 -178.4(4) . . . . ?
Ni1 N1 C2 C1 0.6(5) . . . . ?
O1 C1 C2 N1 -3.1(6) . . . . ?
O2 C1 C2 N1 174.4(4) . . . . ?
O1 C1 C2 C3 176.9(5) . . . . ?
O2 C1 C2 C3 -5.7(8) . . . . ?
C7 N2 C3 C2 0.9(7) . . . . ?
C7 N2 C3 C4 -179.3(4) . . . . ?
N1 C2 C3 N2 -1.6(7) . . . . ?
C1 C2 C3 N2 178.4(5) . . . . ?
N1 C2 C3 C4 178.6(5) . . . . ?
C1 C2 C3 C4 -1.3(8) . . . . ?
N2 C3 C4 O4 7.7(7) . . . . ?
C2 C3 C4 O4 -172.6(5) . . . . ?
N2 C3 C4 O3 -171.6(4) . . . . ?
C2 C3 C4 O3 8.1(8) . . . . ?
Ni1 O8 C5 O7 -173.1(4) . . . . ?
Ni1 O8 C5 C6 5.1(6) . . . . ?
C2 N1 C6 C7 -0.8(7) . . . . ?
Ni1 N1 C6 C7 -179.9(3) . . . . ?
C2 N1 C6 C5 180.0(4) . . . . ?
Ni1 N1 C6 C5 0.9(5) . . . . ?
O8 C5 C6 N1 -4.0(6) . . . . ?
O7 C5 C6 N1 174.3(4) . . . . ?
O8 C5 C6 C7 177.0(5) . . . . ?
O7 C5 C6 C7 -4.7(8) . . . . ?
C3 N2 C7 C6 -0.1(7) . . . . ?
C3 N2 C7 C8 -179.6(4) . . . . ?
N1 C6 C7 N2 0.0(7) . . . . ?
C5 C6 C7 N2 179.0(5) . . . . ?
N1 C6 C7 C8 179.4(5) . . . . ?
C5 C6 C7 C8 -1.6(8) . . . . ?
N2 C7 C8 O5 1.6(7) . . . . ?
C6 C7 C8 O5 -177.8(5) . . . . ?
N2 C7 C8 O6 -176.3(4) . . . . ?
C6 C7 C8 O6 4.3(8) . . . . ?
C20 N3 C9 C10 -1.1(6) . . . . ?
Ni1 N3 C9 C10 178.9(3) . . . . ?
N3 C9 C10 C11 0.6(7) . . . . ?
C9 C10 C11 C12 0.7(6) . . . . ?
C10 C11 C12 C20 -1.3(6) . . . . ?
C10 C11 C12 C13 178.1(4) . . . . ?
C20 C12 C13 C14 -0.9(6) . . . . ?
C11 C12 C13 C14 179.6(4) . . . . ?
C12 C13 C14 C15 0.4(7) . . . . ?
C13 C14 C15 C19 0.6(6) . . . . ?
C13 C14 C15 C16 -177.9(4) . . . . ?
C19 C15 C16 C17 0.4(6) . . . . ?
C14 C15 C16 C17 178.9(4) . . . . ?
C15 C16 C17 C18 1.1(7) . . . . ?
C19 N4 C18 C17 -0.3(6) . . . . ?
Ni1 N4 C18 C17 -177.3(3) . . . . ?
C16 C17 C18 N4 -1.2(7) . . . . ?
C18 N4 C19 C15 1.9(6) . . . . ?
Ni1 N4 C19 C15 179.4(3) . . . . ?
C18 N4 C19 C20 -177.6(4) . . . . ?
Ni1 N4 C19 C20 -0.1(5) . . . . ?
C16 C15 C19 N4 -2.0(6) . . . . ?
C14 C15 C19 N4 179.4(4) . . . . ?
C16 C15 C19 C20 177.6(4) . . . . ?
C14 C15 C19 C20 -1.0(6) . . . . ?
C9 N3 C20 C12 0.5(6) . . . . ?
Ni1 N3 C20 C12 -179.6(3) . . . . ?
C9 N3 C20 C19 -178.8(4) . . . . ?
Ni1 N3 C20 C19 1.1(4) . . . . ?
C11 C12 C20 N3 0.7(6) . . . . ?
C13 C12 C20 N3 -178.8(4) . . . . ?
C11 C12 C20 C19 180.0(4) . . . . ?
C13 C12 C20 C19 0.5(6) . . . . ?
N4 C19 C20 N3 -0.7(5) . . . . ?
C15 C19 C20 N3 179.8(3) . . . . ?
N4 C19 C20 C12 -180.0(4) . . . . ?
C15 C19 C20 C12 0.4(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.095

# Attachment 'complex 2.cif'

data_r071119e1
_database_code_depnum_ccdc_archive 'CCDC 709706'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H47 N8 Ni O18.50'
_chemical_formula_weight         1042.61

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           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   12.833(3)
_cell_length_b                   14.547(3)
_cell_length_c                   15.272(3)
_cell_angle_alpha                66.40(3)
_cell_angle_beta                 65.24(3)
_cell_angle_gamma                86.54(3)
_cell_volume                     2352.6(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1086
_exptl_absorpt_coefficient_mu    0.498
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.9707
_exptl_absorpt_correction_T_max  0.9901
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      113(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14308
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_sigmaI/netI    0.1398
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         25.02
_reflns_number_total             8230
_reflns_number_gt                4565
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0716P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8230
_refine_ls_number_parameters     680
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0663
_refine_ls_wR_factor_ref         0.1787
_refine_ls_wR_factor_gt          0.1670
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_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 0.55356(5) 0.69126(4) 0.66010(5) 0.02355(19) Uani 1 1 d . . .
O1 O 0.8443(3) 0.7101(2) -0.0352(3) 0.0422(9) Uani 1 1 d . . .
H1A H 0.7937 0.7446 -0.0125 0.063 Uiso 1 1 calc R . .
O2 O 0.8693(4) 0.6815(3) 0.1082(3) 0.0661(13) Uani 1 1 d . . .
O3 O 0.9391(3) 0.3087(3) 0.2611(3) 0.0567(11) Uani 1 1 d . . .
O4 O 0.8924(3) 0.2414(3) 0.1725(3) 0.0554(11) Uani 1 1 d . . .
O5 O 0.3101(3) 0.1905(3) 0.9773(3) 0.0543(11) Uani 1 1 d . . .
O6 O 0.2044(4) 0.0445(3) 1.1039(3) 0.0668(13) Uani 1 1 d . . .
O7 O 0.2902(4) 0.0117(3) 0.9024(4) 0.0634(12) Uani 1 1 d . . .
H7 H 0.2266 -0.0147 0.9141 0.095 Uiso 1 1 calc R . .
O8 O 0.3405(4) -0.1445(3) 0.9414(4) 0.0682(13) Uani 1 1 d . . .
N1 N 0.4365(3) 0.6274(3) 0.8209(3) 0.0280(9) Uani 1 1 d . . .
N2 N 0.6193(3) 0.5544(2) 0.7115(3) 0.0254(9) Uani 1 1 d . . .
N3 N 0.4474(3) 0.6294(3) 0.6189(3) 0.0279(9) Uani 1 1 d . . .
N4 N 0.6617(3) 0.7317(2) 0.4996(3) 0.0238(9) Uani 1 1 d . . .
N5 N 0.4802(3) 0.8270(3) 0.6372(3) 0.0238(9) Uani 1 1 d . . .
N6 N 0.6639(3) 0.7740(2) 0.6785(3) 0.0245(9) Uani 1 1 d . . .
N7 N 0.9222(3) 0.4929(3) 0.1002(3) 0.0313(10) Uani 1 1 d . . .
N8 N 0.4780(4) 0.0739(3) 1.0402(3) 0.0417(11) Uani 1 1 d . . .
C1 C 0.3458(4) 0.6625(4) 0.8747(4) 0.0335(12) Uani 1 1 d . . .
H1 H 0.3329 0.7295 0.8396 0.040 Uiso 1 1 calc R . .
C2 C 0.2687(4) 0.6073(4) 0.9790(4) 0.0412(13) Uani 1 1 d . . .
H2 H 0.2051 0.6365 1.0138 0.049 Uiso 1 1 calc R . .
C3 C 0.2847(4) 0.5110(4) 1.0313(4) 0.0443(14) Uani 1 1 d . . .
H3 H 0.2320 0.4719 1.1028 0.053 Uiso 1 1 calc R . .
C4 C 0.3809(4) 0.4695(4) 0.9779(4) 0.0358(12) Uani 1 1 d . . .
C5 C 0.4064(5) 0.3688(4) 1.0263(4) 0.0488(15) Uani 1 1 d . . .
H5 H 0.3561 0.3265 1.0975 0.059 Uiso 1 1 calc R . .
C6 C 0.4986(5) 0.3337(4) 0.9735(4) 0.0467(15) Uani 1 1 d . . .
H6 H 0.5136 0.2672 1.0078 0.056 Uiso 1 1 calc R . .
C7 C 0.5761(4) 0.3950(3) 0.8650(4) 0.0349(12) Uani 1 1 d . . .
C8 C 0.6765(4) 0.3636(4) 0.8041(4) 0.0405(13) Uani 1 1 d . . .
H8 H 0.6970 0.2986 0.8350 0.049 Uiso 1 1 calc R . .
C9 C 0.7433(4) 0.4258(3) 0.7021(4) 0.0350(12) Uani 1 1 d . . .
H9 H 0.8108 0.4048 0.6611 0.042 Uiso 1 1 calc R . .
C10 C 0.7121(4) 0.5210(3) 0.6576(4) 0.0301(11) Uani 1 1 d . . .
H10 H 0.7593 0.5637 0.5857 0.036 Uiso 1 1 calc R . .
C11 C 0.5523(4) 0.4928(3) 0.8146(4) 0.0274(11) Uani 1 1 d . . .
C12 C 0.4539(4) 0.5303(3) 0.8730(4) 0.0281(11) Uani 1 1 d . . .
C13 C 0.3405(4) 0.5788(3) 0.6789(4) 0.0331(12) Uani 1 1 d . . .
H13 H 0.3060 0.5642 0.7523 0.040 Uiso 1 1 calc R . .
C14 C 0.2776(4) 0.5465(4) 0.6387(4) 0.0397(13) Uani 1 1 d . . .
H14 H 0.2018 0.5111 0.6841 0.048 Uiso 1 1 calc R . .
C15 C 0.3254(4) 0.5660(4) 0.5342(5) 0.0456(14) Uani 1 1 d . . .
H15 H 0.2830 0.5442 0.5062 0.055 Uiso 1 1 calc R . .
C16 C 0.4394(4) 0.6192(4) 0.4663(4) 0.0329(12) Uani 1 1 d . . .
C17 C 0.4978(4) 0.6455(4) 0.3548(4) 0.0424(13) Uani 1 1 d . . .
H17 H 0.4593 0.6264 0.3222 0.051 Uiso 1 1 calc R . .
C18 C 0.6052(4) 0.6964(3) 0.2945(4) 0.0359(12) Uani 1 1 d . . .
H18 H 0.6413 0.7125 0.2208 0.043 Uiso 1 1 calc R . .
C19 C 0.6651(4) 0.7262(3) 0.3412(4) 0.0287(11) Uani 1 1 d . . .
C20 C 0.7790(4) 0.7791(3) 0.2825(4) 0.0317(12) Uani 1 1 d . . .
H20 H 0.8195 0.7960 0.2088 0.038 Uiso 1 1 calc R . .
C21 C 0.8290(4) 0.8053(3) 0.3333(4) 0.0312(11) Uani 1 1 d . . .
H21 H 0.9055 0.8398 0.2956 0.037 Uiso 1 1 calc R . .
C22 C 0.7678(4) 0.7812(3) 0.4408(4) 0.0292(11) Uani 1 1 d . . .
H22 H 0.8042 0.8015 0.4742 0.035 Uiso 1 1 calc R . .
C23 C 0.6108(4) 0.7037(3) 0.4499(4) 0.0247(11) Uani 1 1 d . . .
C24 C 0.4955(4) 0.6493(3) 0.5138(4) 0.0255(11) Uani 1 1 d . . .
C25 C 0.3884(4) 0.8521(3) 0.6174(4) 0.0295(11) Uani 1 1 d . . .
H25 H 0.3538 0.8074 0.6029 0.035 Uiso 1 1 calc R . .
C26 C 0.3404(4) 0.9410(4) 0.6169(4) 0.0341(12) Uani 1 1 d . . .
H26 H 0.2749 0.9561 0.6022 0.041 Uiso 1 1 calc R . .
C27 C 0.3889(4) 1.0058(4) 0.6380(4) 0.0364(13) Uani 1 1 d . . .
H27 H 0.3564 1.0659 0.6395 0.044 Uiso 1 1 calc R . .
C28 C 0.4875(4) 0.9832(3) 0.6577(4) 0.0303(11) Uani 1 1 d . . .
C29 C 0.5462(4) 1.0485(3) 0.6773(4) 0.0341(12) Uani 1 1 d . . .
H29 H 0.5169 1.1093 0.6799 0.041 Uiso 1 1 calc R . .
C30 C 0.6421(4) 1.0244(3) 0.6920(4) 0.0341(12) Uani 1 1 d . . .
H30 H 0.6811 1.0698 0.7024 0.041 Uiso 1 1 calc R . .
C31 C 0.6871(4) 0.9315(3) 0.6923(4) 0.0288(11) Uani 1 1 d . . .
C32 C 0.7871(4) 0.9037(4) 0.7057(4) 0.0357(12) Uani 1 1 d . . .
H32 H 0.8299 0.9474 0.7149 0.043 Uiso 1 1 calc R . .
C33 C 0.8235(4) 0.8125(4) 0.7056(4) 0.0359(12) Uani 1 1 d . . .
H33 H 0.8914 0.7927 0.7149 0.043 Uiso 1 1 calc R . .
C34 C 0.7595(4) 0.7498(3) 0.6918(4) 0.0279(11) Uani 1 1 d . . .
H34 H 0.7852 0.6872 0.6918 0.033 Uiso 1 1 calc R . .
C35 C 0.6285(4) 0.8646(3) 0.6770(3) 0.0240(10) Uani 1 1 d . . .
C36 C 0.5289(4) 0.8913(3) 0.6577(3) 0.0236(10) Uani 1 1 d . . .
C37 C 0.8836(4) 0.6639(4) 0.0329(4) 0.0371(13) Uani 1 1 d . . .
C38 C 0.9491(4) 0.5789(3) 0.0139(4) 0.0284(11) Uani 1 1 d . . .
C39 C 0.9727(4) 0.4130(3) 0.0864(4) 0.0311(12) Uani 1 1 d . . .
C40 C 0.9323(4) 0.3116(4) 0.1833(5) 0.0417(14) Uani 1 1 d . . .
C41 C 0.2952(5) 0.0971(4) 1.0329(5) 0.0463(15) Uani 1 1 d . . .
C42 C 0.4069(5) 0.0466(4) 1.0110(4) 0.0406(14) Uani 1 1 d . . .
C43 C 0.4283(5) -0.0261(4) 0.9698(4) 0.0424(14) Uani 1 1 d . . .
C44 C 0.3471(5) -0.0573(4) 0.9355(4) 0.0484(15) Uani 1 1 d . . .
O9 O 0.1448(6) 0.8187(5) 0.2109(6) 0.0329(18) Uani 0.50 1 d P A 1
O9' O 0.1982(8) 0.8557(6) 0.2186(7) 0.063(3) Uani 0.50 1 d P B 2
O10 O 0.0332(8) 0.6591(6) 0.2055(8) 0.040(2) Uani 0.50 1 d P C 1
O10' O -0.0064(8) 0.6155(7) 0.2117(8) 0.050(3) Uani 0.50 1 d P D 2
O11 O 1.0081(3) 0.6275(3) 0.5195(4) 0.0619(12) Uani 1 1 d . . .
H11A H 0.9808 0.6031 0.5962 0.13(3) Uiso 1 1 d R . .
H11B H 0.9718 0.6030 0.4864 0.15(4) Uiso 1 1 d R . .
O12 O 0.0831(3) 0.8292(3) 0.4145(3) 0.0577(11) Uani 1 1 d . . .
H12A H 0.0298 0.8642 0.4320 0.087 Uiso 1 1 d R . .
H12B H 0.0651 0.7644 0.4424 0.087 Uiso 1 1 d R . .
O13 O 0.1539(3) 0.8621(3) 0.5525(3) 0.0577(11) Uani 1 1 d . . .
H13A H 0.1796 0.9047 0.5623 0.086 Uiso 1 1 d R . .
H13B H 0.1478 0.8637 0.5008 0.086 Uiso 1 1 d R . .
O14 O 0.9062(3) 0.5599(3) 0.4281(3) 0.0569(11) Uani 1 1 d . . .
H14A H 0.9140 0.4960 0.4551 0.085 Uiso 1 1 d R . .
H14B H 0.9483 0.5876 0.3588 0.085 Uiso 1 1 d R . .
O15 O 0.9305(3) 0.5597(3) 0.7330(3) 0.0693(13) Uani 1 1 d . . .
H15A H 0.9704 0.5958 0.7431 0.104 Uiso 1 1 d R . .
H15B H 0.9540 0.5022 0.7414 0.104 Uiso 1 1 d R . .
O16 O 0.9800(3) 0.0646(3) 0.2026(3) 0.0660(12) Uani 1 1 d . . .
H16A H 0.9794 0.1256 0.2009 0.099 Uiso 1 1 d R . .
H16B H 0.9225 0.0526 0.1879 0.099 Uiso 1 1 d R . .
O17 O 0.9222(3) 0.9651(3) 0.4150(3) 0.0632(12) Uani 1 1 d . . .
H17A H 0.8808 0.9205 0.4166 0.095 Uiso 1 1 d R . .
H17B H 0.9574 1.0123 0.3509 0.095 Uiso 1 1 d R . .
O18 O 0.0828(8) 0.9635(7) 0.9390(7) 0.087(3) Uani 0.50 1 d P . .
O19 O 0.0903(9) 0.8032(8) 0.1281(9) 0.103(4) Uani 0.50 1 d P . .
O20 O 0.8575(10) 0.2011(9) 0.0419(10) 0.115(4) Uani 0.50 1 d P . .


_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 N6 2.084(4) . ?
Ni1 N4 2.092(4) . ?
Ni1 N3 2.093(4) . ?
Ni1 N2 2.096(3) . ?
Ni1 N1 2.099(4) . ?
Ni1 N5 2.099(3) . ?
O1 C37 1.276(6) . ?
O1 H1A 0.8400 . ?
O2 C37 1.215(6) . ?
O3 C40 1.211(7) . ?
O4 C40 1.265(6) . ?
O5 C41 1.254(6) . ?
O6 C41 1.226(7) . ?
O7 C44 1.269(6) . ?
O7 H7 0.8400 . ?
O8 C44 1.242(6) . ?
N1 C1 1.324(5) . ?
N1 C12 1.374(6) . ?
N2 C10 1.326(5) . ?
N2 C11 1.360(6) . ?
N3 C13 1.338(5) . ?
N3 C24 1.364(6) . ?
N4 C22 1.325(5) . ?
N4 C23 1.365(6) . ?
N5 C25 1.330(5) . ?
N5 C36 1.355(5) . ?
N6 C34 1.330(5) . ?
N6 C35 1.362(5) . ?
N7 C38 1.332(6) . ?
N7 C39 1.345(5) . ?
N8 C42 1.309(7) . ?
N8 C43 1.336(6) 2_657 ?
C1 C2 1.383(7) . ?
C1 H1 0.9500 . ?
C2 C3 1.360(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.420(7) . ?
C3 H3 0.9500 . ?
C4 C12 1.390(6) . ?
C4 C5 1.441(7) . ?
C5 C6 1.330(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.440(7) . ?
C6 H6 0.9500 . ?
C7 C11 1.406(6) . ?
C7 C8 1.414(7) . ?
C8 C9 1.352(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.396(6) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.433(6) . ?
C13 C14 1.394(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.357(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.428(7) . ?
C15 H15 0.9500 . ?
C16 C24 1.403(6) . ?
C16 C17 1.433(7) . ?
C17 C18 1.346(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.425(7) . ?
C18 H18 0.9500 . ?
C19 C23 1.405(6) . ?
C19 C20 1.421(6) . ?
C20 C21 1.357(7) . ?
C20 H20 0.9500 . ?
C21 C22 1.388(6) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C24 1.443(6) . ?
C25 C26 1.397(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.365(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.410(7) . ?
C27 H27 0.9500 . ?
C28 C36 1.407(6) . ?
C28 C29 1.436(7) . ?
C29 C30 1.343(7) . ?
C29 H29 0.9500 . ?
C30 C31 1.436(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.393(6) . ?
C31 C35 1.409(6) . ?
C32 C33 1.380(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.394(6) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C36 1.427(6) . ?
C37 C38 1.508(6) . ?
C38 C39 1.396(6) 2_765 ?
C39 C38 1.397(6) 2_765 ?
C39 C40 1.529(7) . ?
C41 C42 1.542(6) . ?
C42 C43 1.394(7) . ?
C43 N8 1.336(6) 2_657 ?
C43 C44 1.506(8) . ?
O9 O19 1.768(13) . ?
O11 H11A 0.9801 . ?
O11 H11B 0.9798 . ?
O12 H12A 0.8439 . ?
O12 H12B 0.8648 . ?
O13 H13A 0.8088 . ?
O13 H13B 0.8168 . ?
O14 H14A 0.8729 . ?
O14 H14B 0.8840 . ?
O15 H15A 0.8511 . ?
O15 H15B 0.8506 . ?
O16 H16A 0.8762 . ?
O16 H16B 0.9006 . ?
O17 H17A 0.8500 . ?
O17 H17B 0.8744 . ?

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
N6 Ni1 N4 93.53(14) . . ?
N6 Ni1 N3 170.56(14) . . ?
N4 Ni1 N3 79.93(15) . . ?
N6 Ni1 N2 94.88(14) . . ?
N4 Ni1 N2 94.34(14) . . ?
N3 Ni1 N2 92.41(14) . . ?
N6 Ni1 N1 95.06(14) . . ?
N4 Ni1 N1 170.06(13) . . ?
N3 Ni1 N1 92.10(15) . . ?
N2 Ni1 N1 79.96(14) . . ?
N6 Ni1 N5 79.73(14) . . ?
N4 Ni1 N5 95.39(14) . . ?
N3 Ni1 N5 94.02(14) . . ?
N2 Ni1 N5 169.14(15) . . ?
N1 Ni1 N5 91.07(14) . . ?
C37 O1 H1A 109.5 . . ?
C44 O7 H7 109.5 . . ?
C1 N1 C12 117.3(4) . . ?
C1 N1 Ni1 130.2(3) . . ?
C12 N1 Ni1 112.2(3) . . ?
C10 N2 C11 118.2(4) . . ?
C10 N2 Ni1 129.3(3) . . ?
C11 N2 Ni1 112.4(3) . . ?
C13 N3 C24 117.5(4) . . ?
C13 N3 Ni1 129.5(3) . . ?
C24 N3 Ni1 112.8(3) . . ?
C22 N4 C23 117.1(4) . . ?
C22 N4 Ni1 130.1(3) . . ?
C23 N4 Ni1 112.8(3) . . ?
C25 N5 C36 117.9(4) . . ?
C25 N5 Ni1 129.5(3) . . ?
C36 N5 Ni1 112.2(3) . . ?
C34 N6 C35 118.3(4) . . ?
C34 N6 Ni1 129.2(3) . . ?
C35 N6 Ni1 112.5(3) . . ?
C38 N7 C39 116.8(4) . . ?
C42 N8 C43 115.8(4) . 2_657 ?
N1 C1 C2 123.9(5) . . ?
N1 C1 H1 118.0 . . ?
C2 C1 H1 118.0 . . ?
C3 C2 C1 119.4(5) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 119.3(5) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C12 C4 C3 117.5(5) . . ?
C12 C4 C5 118.9(5) . . ?
C3 C4 C5 123.7(5) . . ?
C6 C5 C4 121.5(5) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C6 C7 120.9(5) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C11 C7 C8 116.7(5) . . ?
C11 C7 C6 119.1(4) . . ?
C8 C7 C6 124.2(5) . . ?
C9 C8 C7 120.2(4) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C10 119.3(5) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
N2 C10 C9 122.9(5) . . ?
N2 C10 H10 118.6 . . ?
C9 C10 H10 118.6 . . ?
N2 C11 C7 122.7(4) . . ?
N2 C11 C12 117.9(4) . . ?
C7 C11 C12 119.4(4) . . ?
N1 C12 C4 122.7(4) . . ?
N1 C12 C11 117.0(4) . . ?
C4 C12 C11 120.2(4) . . ?
N3 C13 C14 123.0(5) . . ?
N3 C13 H13 118.5 . . ?
C14 C13 H13 118.5 . . ?
C15 C14 C13 119.5(5) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C16 120.0(5) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C24 C16 C15 116.3(5) . . ?
C24 C16 C17 118.8(4) . . ?
C15 C16 C17 125.0(5) . . ?
C18 C17 C16 122.3(5) . . ?
C18 C17 H17 118.9 . . ?
C16 C17 H17 118.9 . . ?
C17 C18 C19 120.1(5) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C23 C19 C20 117.2(4) . . ?
C23 C19 C18 119.8(4) . . ?
C20 C19 C18 123.0(4) . . ?
C21 C20 C19 119.0(5) . . ?
C21 C20 H20 120.5 . . ?
C19 C20 H20 120.5 . . ?
C20 C21 C22 119.7(4) . . ?
C20 C21 H21 120.2 . . ?
C22 C21 H21 120.2 . . ?
N4 C22 C21 124.0(5) . . ?
N4 C22 H22 118.0 . . ?
C21 C22 H22 118.0 . . ?
N4 C23 C19 123.0(4) . . ?
N4 C23 C24 117.2(4) . . ?
C19 C23 C24 119.7(4) . . ?
N3 C24 C16 123.6(4) . . ?
N3 C24 C23 117.1(4) . . ?
C16 C24 C23 119.3(4) . . ?
N5 C25 C26 123.3(5) . . ?
N5 C25 H25 118.4 . . ?
C26 C25 H25 118.4 . . ?
C27 C26 C25 119.1(4) . . ?
C27 C26 H26 120.5 . . ?
C25 C26 H26 120.5 . . ?
C26 C27 C28 119.7(4) . . ?
C26 C27 H27 120.2 . . ?
C28 C27 H27 120.2 . . ?
C36 C28 C27 117.2(4) . . ?
C36 C28 C29 119.4(4) . . ?
C27 C28 C29 123.4(4) . . ?
C30 C29 C28 120.7(4) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C29 C30 C31 121.5(4) . . ?
C29 C30 H30 119.3 . . ?
C31 C30 H30 119.3 . . ?
C32 C31 C35 117.6(4) . . ?
C32 C31 C30 123.7(4) . . ?
C35 C31 C30 118.8(4) . . ?
C33 C32 C31 119.7(5) . . ?
C33 C32 H32 120.1 . . ?
C31 C32 H32 120.1 . . ?
C32 C33 C34 119.2(5) . . ?
C32 C33 H33 120.4 . . ?
C34 C33 H33 120.4 . . ?
N6 C34 C33 122.8(4) . . ?
N6 C34 H34 118.6 . . ?
C33 C34 H34 118.6 . . ?
N6 C35 C31 122.5(4) . . ?
N6 C35 C36 117.5(4) . . ?
C31 C35 C36 120.0(4) . . ?
N5 C36 C28 122.9(4) . . ?
N5 C36 C35 117.5(4) . . ?
C28 C36 C35 119.6(4) . . ?
O2 C37 O1 125.8(4) . . ?
O2 C37 C38 121.2(5) . . ?
O1 C37 C38 113.0(4) . . ?
N7 C38 C39 122.1(4) . 2_765 ?
N7 C38 C37 114.5(4) . . ?
C39 C38 C37 123.3(4) 2_765 . ?
N7 C39 C38 121.1(4) . 2_765 ?
N7 C39 C40 116.9(4) . . ?
C38 C39 C40 121.8(4) 2_765 . ?
O3 C40 O4 128.1(6) . . ?
O3 C40 C39 116.9(5) . . ?
O4 C40 C39 114.9(5) . . ?
O6 C41 O5 127.5(5) . . ?
O6 C41 C42 118.0(5) . . ?
O5 C41 C42 114.4(5) . . ?
N8 C42 C43 122.5(4) . . ?
N8 C42 C41 113.9(4) . . ?
C43 C42 C41 123.5(5) . . ?
N8 C43 C42 121.7(5) 2_657 . ?
N8 C43 C44 115.7(4) 2_657 . ?
C42 C43 C44 122.6(5) . . ?
O8 C44 O7 125.8(6) . . ?
O8 C44 C43 119.8(5) . . ?
O7 C44 C43 114.4(5) . . ?
H11A O11 H11B 123.8 . . ?
H12A O12 H12B 117.6 . . ?
H13A O13 H13B 131.8 . . ?
H14A O14 H14B 110.9 . . ?
H15A O15 H15B 110.9 . . ?
H16A O16 H16B 108.6 . . ?
H17A O17 H17B 110.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N6 Ni1 N1 C1 86.8(4) . . . . ?
N4 Ni1 N1 C1 -123.5(8) . . . . ?
N3 Ni1 N1 C1 -87.0(4) . . . . ?
N2 Ni1 N1 C1 -179.1(4) . . . . ?
N5 Ni1 N1 C1 7.1(4) . . . . ?
N6 Ni1 N1 C12 -99.8(3) . . . . ?
N4 Ni1 N1 C12 49.9(9) . . . . ?
N3 Ni1 N1 C12 86.4(3) . . . . ?
N2 Ni1 N1 C12 -5.7(3) . . . . ?
N5 Ni1 N1 C12 -179.6(3) . . . . ?
N6 Ni1 N2 C10 -82.9(4) . . . . ?
N4 Ni1 N2 C10 11.1(4) . . . . ?
N3 Ni1 N2 C10 91.2(4) . . . . ?
N1 Ni1 N2 C10 -177.1(4) . . . . ?
N5 Ni1 N2 C10 -142.5(6) . . . . ?
N6 Ni1 N2 C11 99.1(3) . . . . ?
N4 Ni1 N2 C11 -167.0(3) . . . . ?
N3 Ni1 N2 C11 -86.9(3) . . . . ?
N1 Ni1 N2 C11 4.8(3) . . . . ?
N5 Ni1 N2 C11 39.4(8) . . . . ?
N6 Ni1 N3 C13 -133.1(8) . . . . ?
N4 Ni1 N3 C13 -179.8(4) . . . . ?
N2 Ni1 N3 C13 86.3(4) . . . . ?
N1 Ni1 N3 C13 6.2(4) . . . . ?
N5 Ni1 N3 C13 -85.0(4) . . . . ?
N6 Ni1 N3 C24 43.6(9) . . . . ?
N4 Ni1 N3 C24 -3.1(3) . . . . ?
N2 Ni1 N3 C24 -97.0(3) . . . . ?
N1 Ni1 N3 C24 -177.1(3) . . . . ?
N5 Ni1 N3 C24 91.7(3) . . . . ?
N6 Ni1 N4 C22 7.6(4) . . . . ?
N3 Ni1 N4 C22 -179.2(4) . . . . ?
N2 Ni1 N4 C22 -87.6(4) . . . . ?
N1 Ni1 N4 C22 -142.1(7) . . . . ?
N5 Ni1 N4 C22 87.6(4) . . . . ?
N6 Ni1 N4 C23 -170.5(3) . . . . ?
N3 Ni1 N4 C23 2.7(3) . . . . ?
N2 Ni1 N4 C23 94.4(3) . . . . ?
N1 Ni1 N4 C23 39.8(9) . . . . ?
N5 Ni1 N4 C23 -90.5(3) . . . . ?
N6 Ni1 N5 C25 -179.5(4) . . . . ?
N4 Ni1 N5 C25 87.8(4) . . . . ?
N3 Ni1 N5 C25 7.6(4) . . . . ?
N2 Ni1 N5 C25 -118.6(7) . . . . ?
N1 Ni1 N5 C25 -84.6(4) . . . . ?
N6 Ni1 N5 C36 -7.4(3) . . . . ?
N4 Ni1 N5 C36 -100.0(3) . . . . ?
N3 Ni1 N5 C36 179.8(3) . . . . ?
N2 Ni1 N5 C36 53.6(8) . . . . ?
N1 Ni1 N5 C36 87.6(3) . . . . ?
N4 Ni1 N6 C34 -80.1(4) . . . . ?
N3 Ni1 N6 C34 -125.9(8) . . . . ?
N2 Ni1 N6 C34 14.6(4) . . . . ?
N1 Ni1 N6 C34 94.9(4) . . . . ?
N5 Ni1 N6 C34 -174.9(4) . . . . ?
N4 Ni1 N6 C35 100.6(3) . . . . ?
N3 Ni1 N6 C35 54.8(9) . . . . ?
N2 Ni1 N6 C35 -164.7(3) . . . . ?
N1 Ni1 N6 C35 -84.4(3) . . . . ?
N5 Ni1 N6 C35 5.8(3) . . . . ?
C12 N1 C1 C2 0.0(7) . . . . ?
Ni1 N1 C1 C2 173.1(4) . . . . ?
N1 C1 C2 C3 -0.2(8) . . . . ?
C1 C2 C3 C4 0.6(8) . . . . ?
C2 C3 C4 C12 -0.7(7) . . . . ?
C2 C3 C4 C5 179.3(5) . . . . ?
C12 C4 C5 C6 1.0(8) . . . . ?
C3 C4 C5 C6 -179.0(5) . . . . ?
C4 C5 C6 C7 -0.7(9) . . . . ?
C5 C6 C7 C11 -0.8(8) . . . . ?
C5 C6 C7 C8 179.2(5) . . . . ?
C11 C7 C8 C9 -1.1(7) . . . . ?
C6 C7 C8 C9 178.9(5) . . . . ?
C7 C8 C9 C10 -0.1(7) . . . . ?
C11 N2 C10 C9 0.2(7) . . . . ?
Ni1 N2 C10 C9 -177.8(3) . . . . ?
C8 C9 C10 N2 0.6(7) . . . . ?
C10 N2 C11 C7 -1.4(7) . . . . ?
Ni1 N2 C11 C7 176.9(4) . . . . ?
C10 N2 C11 C12 178.5(4) . . . . ?
Ni1 N2 C11 C12 -3.2(5) . . . . ?
C8 C7 C11 N2 1.9(7) . . . . ?
C6 C7 C11 N2 -178.1(4) . . . . ?
C8 C7 C11 C12 -178.1(4) . . . . ?
C6 C7 C11 C12 2.0(7) . . . . ?
C1 N1 C12 C4 -0.1(7) . . . . ?
Ni1 N1 C12 C4 -174.4(4) . . . . ?
C1 N1 C12 C11 -179.8(4) . . . . ?
Ni1 N1 C12 C11 5.8(5) . . . . ?
C3 C4 C12 N1 0.4(7) . . . . ?
C5 C4 C12 N1 -179.6(4) . . . . ?
C3 C4 C12 C11 -179.8(4) . . . . ?
C5 C4 C12 C11 0.2(7) . . . . ?
N2 C11 C12 N1 -1.8(6) . . . . ?
C7 C11 C12 N1 178.1(4) . . . . ?
N2 C11 C12 C4 178.4(4) . . . . ?
C7 C11 C12 C4 -1.7(7) . . . . ?
C24 N3 C13 C14 -0.1(6) . . . . ?
Ni1 N3 C13 C14 176.4(3) . . . . ?
N3 C13 C14 C15 0.4(7) . . . . ?
C13 C14 C15 C16 0.0(8) . . . . ?
C14 C15 C16 C24 -0.5(7) . . . . ?
C14 C15 C16 C17 -178.8(5) . . . . ?
C24 C16 C17 C18 1.3(7) . . . . ?
C15 C16 C17 C18 179.6(5) . . . . ?
C16 C17 C18 C19 -0.1(7) . . . . ?
C17 C18 C19 C23 -1.0(7) . . . . ?
C17 C18 C19 C20 179.4(4) . . . . ?
C23 C19 C20 C21 -0.1(6) . . . . ?
C18 C19 C20 C21 179.5(4) . . . . ?
C19 C20 C21 C22 -0.9(6) . . . . ?
C23 N4 C22 C21 -0.3(6) . . . . ?
Ni1 N4 C22 C21 -178.3(3) . . . . ?
C20 C21 C22 N4 1.2(7) . . . . ?
C22 N4 C23 C19 -0.8(6) . . . . ?
Ni1 N4 C23 C19 177.5(3) . . . . ?
C22 N4 C23 C24 179.7(3) . . . . ?
Ni1 N4 C23 C24 -1.9(4) . . . . ?
C20 C19 C23 N4 1.0(6) . . . . ?
C18 C19 C23 N4 -178.6(4) . . . . ?
C20 C19 C23 C24 -179.5(4) . . . . ?
C18 C19 C23 C24 0.9(6) . . . . ?
C13 N3 C24 C16 -0.4(6) . . . . ?
Ni1 N3 C24 C16 -177.6(3) . . . . ?
C13 N3 C24 C23 -179.9(4) . . . . ?
Ni1 N3 C24 C23 3.0(4) . . . . ?
C15 C16 C24 N3 0.8(7) . . . . ?
C17 C16 C24 N3 179.2(4) . . . . ?
C15 C16 C24 C23 -179.8(4) . . . . ?
C17 C16 C24 C23 -1.4(6) . . . . ?
N4 C23 C24 N3 -0.7(5) . . . . ?
C19 C23 C24 N3 179.8(4) . . . . ?
N4 C23 C24 C16 179.8(4) . . . . ?
C19 C23 C24 C16 0.3(6) . . . . ?
C36 N5 C25 C26 -0.1(7) . . . . ?
Ni1 N5 C25 C26 171.7(3) . . . . ?
N5 C25 C26 C27 -0.2(7) . . . . ?
C25 C26 C27 C28 1.3(7) . . . . ?
C26 C27 C28 C36 -2.1(7) . . . . ?
C26 C27 C28 C29 178.0(4) . . . . ?
C36 C28 C29 C30 2.3(7) . . . . ?
C27 C28 C29 C30 -177.8(5) . . . . ?
C28 C29 C30 C31 -2.2(7) . . . . ?
C29 C30 C31 C32 179.1(5) . . . . ?
C29 C30 C31 C35 -0.2(7) . . . . ?
C35 C31 C32 C33 -1.2(7) . . . . ?
C30 C31 C32 C33 179.6(4) . . . . ?
C31 C32 C33 C34 0.2(7) . . . . ?
C35 N6 C34 C33 0.9(7) . . . . ?
Ni1 N6 C34 C33 -178.4(3) . . . . ?
C32 C33 C34 N6 0.0(7) . . . . ?
C34 N6 C35 C31 -2.0(6) . . . . ?
Ni1 N6 C35 C31 177.4(3) . . . . ?
C34 N6 C35 C36 177.1(4) . . . . ?
Ni1 N6 C35 C36 -3.5(5) . . . . ?
C32 C31 C35 N6 2.1(7) . . . . ?
C30 C31 C35 N6 -178.6(4) . . . . ?
C32 C31 C35 C36 -176.9(4) . . . . ?
C30 C31 C35 C36 2.4(6) . . . . ?
C25 N5 C36 C28 -0.8(6) . . . . ?
Ni1 N5 C36 C28 -173.9(3) . . . . ?
C25 N5 C36 C35 -178.9(4) . . . . ?
Ni1 N5 C36 C35 7.9(5) . . . . ?
C27 C28 C36 N5 1.8(6) . . . . ?
C29 C28 C36 N5 -178.3(4) . . . . ?
C27 C28 C36 C35 179.9(4) . . . . ?
C29 C28 C36 C35 -0.1(6) . . . . ?
N6 C35 C36 N5 -3.1(6) . . . . ?
C31 C35 C36 N5 176.1(4) . . . . ?
N6 C35 C36 C28 178.7(4) . . . . ?
C31 C35 C36 C28 -2.2(6) . . . . ?
C39 N7 C38 C39 -1.0(8) . . . 2_765 ?
C39 N7 C38 C37 175.8(4) . . . . ?
O2 C37 C38 N7 43.8(7) . . . . ?
O1 C37 C38 N7 -134.2(5) . . . . ?
O2 C37 C38 C39 -139.4(6) . . . 2_765 ?
O1 C37 C38 C39 42.6(7) . . . 2_765 ?
C38 N7 C39 C38 1.0(8) . . . 2_765 ?
C38 N7 C39 C40 -173.7(4) . . . . ?
N7 C39 C40 O3 -56.1(6) . . . . ?
C38 C39 C40 O3 129.2(5) 2_765 . . . ?
N7 C39 C40 O4 121.8(5) . . . . ?
C38 C39 C40 O4 -52.8(7) 2_765 . . . ?
C43 N8 C42 C43 -1.5(8) 2_657 . . . ?
C43 N8 C42 C41 175.0(5) 2_657 . . . ?
O6 C41 C42 N8 -108.7(6) . . . . ?
O5 C41 C42 N8 68.1(6) . . . . ?
O6 C41 C42 C43 67.7(7) . . . . ?
O5 C41 C42 C43 -115.4(6) . . . . ?
N8 C42 C43 N8 1.6(9) . . . 2_657 ?
C41 C42 C43 N8 -174.6(5) . . . 2_657 ?
N8 C42 C43 C44 -179.6(5) . . . . ?
C41 C42 C43 C44 4.2(8) . . . . ?
N8 C43 C44 O8 28.7(7) 2_657 . . . ?
C42 C43 C44 O8 -150.2(5) . . . . ?
N8 C43 C44 O7 -151.4(5) 2_657 . . . ?
C42 C43 C44 O7 29.7(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.110


