# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2011


data_global

_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
#TrackingRef 'wj-702.cif'

_publ_contact_author_email       wangjjudy@163.com
_publ_contact_author_name        'Jiang Wang'
loop_
_publ_author_name
'Hong Liu'
'Jiang Wang'
'Shengbin Zhou'
'Daizong Lin'
'Xiao Ding'
'Hualiang Jiang'

data_wj_702
_database_code_depnum_ccdc_archive 'CCDC 796799'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H44 N4 Ni O5'
_chemical_formula_weight         791.56

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'
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)

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

_cell_length_a                   9.5816(5)
_cell_length_b                   12.4509(7)
_cell_length_c                   16.5961(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.6403(7)
_cell_angle_gamma                90.00
_cell_volume                     1915.62(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6996
_cell_measurement_theta_min      4.493
_cell_measurement_theta_max      54.568

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.071
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             832
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6189
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13805
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         25.99
_reflns_number_total             6977
_reflns_number_gt                6527
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.0399P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       ?
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.021(8)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         6977
_refine_ls_number_parameters     512
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.0760
_refine_ls_wR_factor_gt          0.0743
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.004
_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 0.20653(2) 0.823382(19) 0.801968(13) 0.03168(8) Uani 1 1 d . . .
O1 O 0.40909(16) 0.63829(13) 0.97839(9) 0.0423(3) Uani 1 1 d . . .
O2 O 0.33304(16) 0.77955(12) 0.90041(9) 0.0393(3) Uani 1 1 d . . .
O3 O -0.0586(2) 1.03155(16) 0.68227(15) 0.0768(6) Uani 1 1 d . . .
O4 O 0.2446(3) 0.55626(17) 0.55297(14) 0.0730(6) Uani 1 1 d . . .
O5 O 0.2981(2) 0.69806(18) 0.48843(14) 0.0705(6) Uani 1 1 d . . .
N1 N 0.16732(18) 0.68085(14) 0.78118(10) 0.0307(3) Uani 1 1 d . . .
N2 N 0.06880(18) 0.87350(15) 0.71201(11) 0.0373(4) Uani 1 1 d . . .
N3 N 0.27059(19) 0.96834(14) 0.82696(12) 0.0393(4) Uani 1 1 d . . .
N4 N 0.5108(2) 0.31356(18) 0.90342(11) 0.0464(4) Uani 1 1 d . . .
C1 C 0.3435(2) 0.67909(17) 0.91261(13) 0.0345(4) Uani 1 1 d . . .
C2 C 0.2710(2) 0.61208(17) 0.83855(12) 0.0312(4) Uani 1 1 d . . .
H2 H 0.2192 0.5529 0.8570 0.037 Uiso 1 1 calc R . .
C3 C 0.0598(2) 0.63836(17) 0.72781(13) 0.0327(4) Uani 1 1 d . . .
C4 C -0.0339(2) 0.69981(18) 0.66173(13) 0.0361(4) Uani 1 1 d . . .
C5 C -0.1320(2) 0.6430(2) 0.60012(15) 0.0485(5) Uani 1 1 d . . .
H5 H -0.1424 0.5696 0.6072 0.058 Uiso 1 1 calc R . .
C6 C -0.2131(3) 0.6905(2) 0.53013(17) 0.0585(7) Uani 1 1 d . . .
H6 H -0.2784 0.6503 0.4906 0.070 Uiso 1 1 calc R . .
C7 C -0.1974(3) 0.7975(2) 0.51853(16) 0.0546(7) Uani 1 1 d . . .
H7 H -0.2486 0.8301 0.4695 0.066 Uiso 1 1 calc R . .
C8 C -0.1078(2) 0.8565(2) 0.57798(15) 0.0471(5) Uani 1 1 d . . .
H8 H -0.1008 0.9299 0.5693 0.057 Uiso 1 1 calc R . .
C9 C -0.02443(19) 0.8117(2) 0.65249(12) 0.0359(4) Uani 1 1 d . . .
C10 C 0.0484(3) 0.9814(2) 0.71487(17) 0.0457(6) Uani 1 1 d . . .
C11 C 0.1789(3) 1.03978(19) 0.76247(15) 0.0455(5) Uani 1 1 d . . .
H11 H 0.1503 1.1035 0.7890 0.055 Uiso 1 1 calc R . .
C12 C 0.2705(3) 1.0726(3) 0.70469(18) 0.0657(8) Uani 1 1 d . . .
H12A H 0.2149 1.0711 0.6471 0.079 Uiso 1 1 calc R . .
H12B H 0.3096 1.1441 0.7179 0.079 Uiso 1 1 calc R . .
C13 C 0.3877(3) 0.9909(2) 0.72000(19) 0.0654(8) Uani 1 1 d . . .
H13A H 0.4726 1.0182 0.7051 0.078 Uiso 1 1 calc R . .
H13B H 0.3561 0.9255 0.6891 0.078 Uiso 1 1 calc R . .
C14 C 0.4165(3) 0.9724(2) 0.81246(18) 0.0536(6) Uani 1 1 d . . .
H14A H 0.4676 0.9054 0.8284 0.064 Uiso 1 1 calc R . .
H14B H 0.4725 1.0308 0.8434 0.064 Uiso 1 1 calc R . .
C15 C 0.2785(3) 1.0053(2) 0.91362(15) 0.0464(5) Uani 1 1 d . . .
H15A H 0.3406 0.9568 0.9524 0.056 Uiso 1 1 calc R . .
H15B H 0.3227 1.0759 0.9213 0.056 Uiso 1 1 calc R . .
C16 C 0.1376(3) 1.0110(2) 0.93412(14) 0.0465(5) Uani 1 1 d . . .
C17 C 0.0790(4) 0.9204(3) 0.95910(19) 0.0691(8) Uani 1 1 d . . .
H17 H 0.1268 0.8550 0.9623 0.083 Uiso 1 1 calc R . .
C18 C -0.0508(4) 0.9272(4) 0.9793(2) 0.0879(11) Uani 1 1 d . . .
H18 H -0.0912 0.8658 0.9961 0.105 Uiso 1 1 calc R . .
C19 C -0.1205(4) 1.0218(4) 0.9752(2) 0.0849(11) Uani 1 1 d . . .
H19 H -0.2095 1.0251 0.9879 0.102 Uiso 1 1 calc R . .
C20 C -0.0615(4) 1.1116(3) 0.9528(2) 0.0805(10) Uani 1 1 d . . .
H20 H -0.1090 1.1771 0.9508 0.097 Uiso 1 1 calc R . .
C21 C 0.0677(3) 1.1061(2) 0.93314(18) 0.0636(7) Uani 1 1 d . . .
H21 H 0.1090 1.1686 0.9188 0.076 Uiso 1 1 calc R . .
C22 C 0.0307(2) 0.52198(17) 0.73358(13) 0.0367(4) Uani 1 1 d . . .
C23 C -0.0551(3) 0.4906(2) 0.78359(17) 0.0528(6) Uani 1 1 d . . .
H23 H -0.0935 0.5414 0.8129 0.063 Uiso 1 1 calc R . .
C24 C -0.0845(3) 0.3833(3) 0.7904(2) 0.0678(8) Uani 1 1 d . . .
H24 H -0.1427 0.3617 0.8246 0.081 Uiso 1 1 calc R . .
C25 C -0.0294(3) 0.3094(2) 0.7478(2) 0.0652(7) Uani 1 1 d . . .
H25 H -0.0504 0.2371 0.7524 0.078 Uiso 1 1 calc R . .
C26 C 0.0560(3) 0.3394(2) 0.69849(19) 0.0594(7) Uani 1 1 d . . .
H26 H 0.0953 0.2877 0.6703 0.071 Uiso 1 1 calc R . .
C27 C 0.0851(3) 0.4460(2) 0.68981(16) 0.0473(5) Uani 1 1 d . . .
H27 H 0.1416 0.4667 0.6544 0.057 Uiso 1 1 calc R . .
C28 C 0.3813(2) 0.56529(15) 0.79313(11) 0.0308(4) Uani 1 1 d . . .
H28 H 0.3278 0.5544 0.7351 0.037 Uiso 1 1 calc R . .
C29 C 0.5018(2) 0.64121(17) 0.79093(13) 0.0370(4) Uani 1 1 d . . .
C30 C 0.4961(3) 0.7022(2) 0.72049(16) 0.0535(6) Uani 1 1 d . . .
H30 H 0.4160 0.6980 0.6753 0.064 Uiso 1 1 calc R . .
C31 C 0.6073(4) 0.7683(3) 0.7172(2) 0.0743(9) Uani 1 1 d . . .
H31 H 0.6038 0.8081 0.6693 0.089 Uiso 1 1 calc R . .
C32 C 0.7244(4) 0.7767(3) 0.7840(3) 0.0751(9) Uani 1 1 d . . .
H32 H 0.7988 0.8240 0.7824 0.090 Uiso 1 1 calc R . .
C33 C 0.7313(3) 0.7165(3) 0.8518(2) 0.0738(9) Uani 1 1 d . . .
H33 H 0.8120 0.7214 0.8967 0.089 Uiso 1 1 calc R . .
C34 C 0.6229(2) 0.6484(2) 0.85618(16) 0.0517(6) Uani 1 1 d . . .
H34 H 0.6305 0.6065 0.9035 0.062 Uiso 1 1 calc R . .
C35 C 0.4349(2) 0.45777(17) 0.82543(12) 0.0340(4) Uani 1 1 d . . .
C36 C 0.4467(2) 0.41157(18) 0.90043(14) 0.0420(5) Uani 1 1 d . . .
H36 H 0.4155 0.4423 0.9439 0.050 Uiso 1 1 calc R . .
C37 C 0.5422(2) 0.29601(16) 0.82911(14) 0.0397(5) Uani 1 1 d . . .
C38 C 0.4938(2) 0.38423(16) 0.77829(13) 0.0351(4) Uani 1 1 d . . .
C39 C 0.5086(3) 0.3839(2) 0.69634(15) 0.0501(6) Uani 1 1 d . . .
H39 H 0.4756 0.4413 0.6608 0.060 Uiso 1 1 calc R . .
C40 C 0.5720(3) 0.2982(2) 0.67022(18) 0.0600(7) Uani 1 1 d . . .
H40 H 0.5796 0.2961 0.6155 0.072 Uiso 1 1 calc R . .
C41 C 0.6257(3) 0.2137(2) 0.7230(2) 0.0579(7) Uani 1 1 d . . .
H41 H 0.6722 0.1575 0.7036 0.069 Uiso 1 1 calc R . .
C42 C 0.6121(2) 0.21101(19) 0.80303(18) 0.0499(6) Uani 1 1 d . . .
H42 H 0.6484 0.1541 0.8384 0.060 Uiso 1 1 calc R . .
C43 C 0.3106(3) 0.5959(2) 0.51028(17) 0.0556(6) Uani 1 1 d . . .
C44 C 0.4168(5) 0.5407(3) 0.4768(3) 0.0952(12) Uani 1 1 d . . .
H44A H 0.3773 0.4740 0.4521 0.143 Uiso 1 1 calc R . .
H44B H 0.5014 0.5267 0.5208 0.143 Uiso 1 1 calc R . .
H44C H 0.4421 0.5849 0.4352 0.143 Uiso 1 1 calc R . .
C45 C 0.1909(4) 0.7592(3) 0.5133(2) 0.0760(10) Uani 1 1 d . . .
H45A H 0.1969 0.7471 0.5718 0.091 Uiso 1 1 calc R . .
H45B H 0.0956 0.7378 0.4812 0.091 Uiso 1 1 calc R . .
C46 C 0.2157(5) 0.8730(3) 0.4987(3) 0.0847(11) Uani 1 1 d . . .
H46A H 0.2119 0.8838 0.4409 0.127 Uiso 1 1 calc R . .
H46B H 0.3088 0.8940 0.5320 0.127 Uiso 1 1 calc R . .
H46C H 0.1426 0.9157 0.5135 0.127 Uiso 1 1 calc R . .
H4 H 0.523(3) 0.266(3) 0.9479(19) 0.068(9) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.03565(12) 0.02178(12) 0.03583(12) -0.00256(11) 0.00574(8) -0.00106(11)
O1 0.0555(9) 0.0380(9) 0.0300(7) -0.0017(6) 0.0045(6) 0.0050(7)
O2 0.0480(8) 0.0265(7) 0.0385(8) -0.0045(6) 0.0019(6) -0.0006(6)
O3 0.0750(12) 0.0396(10) 0.0975(15) -0.0071(11) -0.0120(11) 0.0204(10)
O4 0.0982(15) 0.0584(13) 0.0734(13) 0.0064(10) 0.0420(12) -0.0145(11)
O5 0.0744(12) 0.0617(13) 0.0873(14) 0.0309(11) 0.0425(11) 0.0100(10)
N1 0.0352(8) 0.0228(9) 0.0340(8) -0.0004(7) 0.0086(7) 0.0002(7)
N2 0.0391(9) 0.0268(9) 0.0438(10) 0.0008(7) 0.0067(8) 0.0010(7)
N3 0.0416(10) 0.0265(10) 0.0473(10) -0.0065(8) 0.0068(8) -0.0029(7)
N4 0.0619(10) 0.0326(10) 0.0407(9) 0.0095(10) 0.0052(8) 0.0052(10)
C1 0.0376(10) 0.0320(12) 0.0353(11) -0.0029(9) 0.0119(8) 0.0007(8)
C2 0.0353(9) 0.0263(10) 0.0315(10) 0.0013(8) 0.0078(8) 0.0008(8)
C3 0.0339(10) 0.0263(11) 0.0378(11) -0.0042(8) 0.0091(8) -0.0019(8)
C4 0.0340(10) 0.0333(11) 0.0393(11) 0.0003(9) 0.0061(8) 0.0019(8)
C5 0.0466(12) 0.0383(13) 0.0527(13) -0.0022(10) -0.0021(10) -0.0019(10)
C6 0.0496(13) 0.0574(18) 0.0550(15) -0.0071(12) -0.0115(11) 0.0014(12)
C7 0.0519(12) 0.0523(19) 0.0508(13) 0.0048(11) -0.0032(10) 0.0095(11)
C8 0.0492(12) 0.0388(13) 0.0473(13) 0.0050(9) 0.0011(10) 0.0050(9)
C9 0.0340(8) 0.0314(11) 0.0420(10) -0.0001(10) 0.0088(7) 0.0019(9)
C10 0.0520(14) 0.0295(12) 0.0526(14) 0.0024(10) 0.0076(11) 0.0066(10)
C11 0.0617(14) 0.0242(11) 0.0474(13) -0.0005(9) 0.0077(11) 0.0011(10)
C12 0.084(2) 0.0490(16) 0.0648(18) 0.0078(13) 0.0201(15) -0.0188(14)
C13 0.0750(19) 0.0502(16) 0.081(2) -0.0058(14) 0.0377(16) -0.0180(14)
C14 0.0467(13) 0.0363(13) 0.0806(18) -0.0057(12) 0.0213(12) -0.0107(10)
C15 0.0506(13) 0.0342(13) 0.0477(13) -0.0117(10) 0.0002(10) -0.0001(10)
C16 0.0557(13) 0.0421(13) 0.0374(11) -0.0105(10) 0.0039(10) 0.0049(10)
C17 0.092(2) 0.0523(17) 0.0739(19) -0.0071(14) 0.0414(17) 0.0054(15)
C18 0.104(3) 0.088(3) 0.089(2) -0.017(2) 0.057(2) -0.014(2)
C19 0.078(2) 0.106(3) 0.076(2) -0.026(2) 0.0308(18) 0.006(2)
C20 0.079(2) 0.086(3) 0.077(2) -0.0127(19) 0.0188(17) 0.0323(19)
C21 0.0740(17) 0.0526(16) 0.0610(16) -0.0077(13) 0.0111(13) 0.0159(14)
C22 0.0339(9) 0.0277(11) 0.0438(11) -0.0001(8) 0.0014(8) -0.0049(8)
C23 0.0521(13) 0.0419(14) 0.0671(16) -0.0046(11) 0.0203(12) -0.0120(11)
C24 0.0680(17) 0.0530(18) 0.085(2) 0.0116(15) 0.0244(16) -0.0232(14)
C25 0.0603(14) 0.0312(15) 0.0946(19) 0.0121(15) 0.0021(14) -0.0096(12)
C26 0.0539(12) 0.0317(15) 0.0875(18) -0.0079(13) 0.0083(12) 0.0027(11)
C27 0.0480(12) 0.0335(12) 0.0592(14) -0.0086(11) 0.0112(11) -0.0058(10)
C28 0.0398(10) 0.0251(10) 0.0262(9) -0.0011(7) 0.0060(8) 0.0043(8)
C29 0.0450(11) 0.0297(11) 0.0399(11) -0.0020(8) 0.0175(9) 0.0051(8)
C30 0.0676(15) 0.0482(14) 0.0501(14) 0.0073(11) 0.0250(12) 0.0018(12)
C31 0.104(2) 0.0545(18) 0.083(2) 0.0100(16) 0.059(2) -0.0068(17)
C32 0.0699(19) 0.0594(19) 0.110(3) -0.0116(18) 0.049(2) -0.0170(14)
C33 0.0510(15) 0.076(2) 0.096(2) -0.0122(19) 0.0223(16) -0.0150(14)
C34 0.0451(12) 0.0528(15) 0.0558(14) -0.0001(11) 0.0104(10) -0.0073(11)
C35 0.0380(10) 0.0296(11) 0.0320(10) 0.0009(8) 0.0041(8) 0.0020(8)
C36 0.0526(12) 0.0366(12) 0.0349(11) 0.0013(9) 0.0077(10) 0.0040(9)
C37 0.0391(10) 0.0292(12) 0.0478(12) 0.0015(8) 0.0056(9) -0.0016(8)
C38 0.0373(10) 0.0277(11) 0.0386(11) 0.0003(8) 0.0068(9) 0.0015(8)
C39 0.0637(15) 0.0433(14) 0.0456(13) -0.0007(10) 0.0180(11) 0.0038(11)
C40 0.0722(15) 0.053(2) 0.0631(15) -0.0135(13) 0.0333(13) 0.0026(12)
C41 0.0532(14) 0.0369(13) 0.088(2) -0.0173(13) 0.0266(14) -0.0009(11)
C42 0.0409(12) 0.0236(11) 0.0815(18) -0.0009(11) 0.0087(11) -0.0005(9)
C43 0.0595(14) 0.0548(17) 0.0535(14) 0.0028(12) 0.0164(12) -0.0070(12)
C44 0.108(3) 0.071(2) 0.129(3) 0.019(2) 0.071(3) 0.014(2)
C45 0.0697(19) 0.074(2) 0.092(2) 0.0249(19) 0.0346(18) 0.0152(16)
C46 0.101(3) 0.070(2) 0.089(3) 0.0045(19) 0.036(2) 0.0116(19)

_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 1.8287(17) . ?
Ni1 N2 1.8341(18) . ?
Ni1 O2 1.8535(15) . ?
Ni1 N3 1.9177(18) . ?
O1 C1 1.224(3) . ?
O2 C1 1.267(3) . ?
O3 C10 1.206(3) . ?
O4 C43 1.171(3) . ?
O5 C43 1.320(4) . ?
O5 C45 1.421(4) . ?
N1 C3 1.290(3) . ?
N1 C2 1.466(3) . ?
N2 C10 1.360(3) . ?
N2 C9 1.386(3) . ?
N3 C14 1.478(3) . ?
N3 C15 1.494(3) . ?
N3 C11 1.494(3) . ?
N4 C37 1.359(3) . ?
N4 C36 1.361(3) . ?
N4 H4 0.93(3) . ?
C1 C2 1.503(3) . ?
C2 C28 1.558(3) . ?
C2 H2 0.9800 . ?
C3 C4 1.448(3) . ?
C3 C22 1.483(3) . ?
C4 C5 1.394(3) . ?
C4 C9 1.406(3) . ?
C5 C6 1.359(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.360(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.350(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.407(3) . ?
C8 H8 0.9300 . ?
C10 C11 1.489(4) . ?
C11 C12 1.511(4) . ?
C11 H11 0.9800 . ?
C12 C13 1.488(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.506(4) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.475(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C21 1.359(4) . ?
C16 C17 1.370(4) . ?
C17 C18 1.370(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.348(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.347(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.360(4) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.365(3) . ?
C22 C27 1.373(3) . ?
C23 C24 1.375(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.347(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.348(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.371(4) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C35 1.485(3) . ?
C28 C29 1.500(3) . ?
C28 H28 0.9800 . ?
C29 C34 1.375(3) . ?
C29 C30 1.384(3) . ?
C30 C31 1.358(4) . ?
C30 H30 0.9300 . ?
C31 C32 1.367(5) . ?
C31 H31 0.9300 . ?
C32 C33 1.339(5) . ?
C32 H32 0.9300 . ?
C33 C34 1.357(4) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 C36 1.350(3) . ?
C35 C38 1.411(3) . ?
C36 H36 0.9300 . ?
C37 C42 1.379(3) . ?
C37 C38 1.391(3) . ?
C38 C39 1.403(3) . ?
C39 C40 1.351(4) . ?
C39 H39 0.9300 . ?
C40 C41 1.382(4) . ?
C40 H40 0.9300 . ?
C41 C42 1.367(4) . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?
C43 C44 1.450(4) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 C46 1.467(5) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N2 96.05(8) . . ?
N1 Ni1 O2 86.44(7) . . ?
N2 Ni1 O2 173.42(8) . . ?
N1 Ni1 N3 173.42(8) . . ?
N2 Ni1 N3 88.91(8) . . ?
O2 Ni1 N3 89.09(7) . . ?
C1 O2 Ni1 116.05(14) . . ?
C43 O5 C45 117.3(2) . . ?
C3 N1 C2 119.93(18) . . ?
C3 N1 Ni1 128.14(15) . . ?
C2 N1 Ni1 111.79(14) . . ?
C10 N2 C9 120.1(2) . . ?
C10 N2 Ni1 112.82(16) . . ?
C9 N2 Ni1 126.35(15) . . ?
C14 N3 C15 109.05(19) . . ?
C14 N3 C11 105.76(19) . . ?
C15 N3 C11 112.56(18) . . ?
C14 N3 Ni1 105.16(14) . . ?
C15 N3 Ni1 115.72(15) . . ?
C11 N3 Ni1 107.90(14) . . ?
C37 N4 C36 108.21(18) . . ?
C37 N4 H4 127.1(19) . . ?
C36 N4 H4 124.5(19) . . ?
O1 C1 O2 123.7(2) . . ?
O1 C1 C2 121.74(19) . . ?
O2 C1 C2 114.58(18) . . ?
N1 C2 C1 107.72(17) . . ?
N1 C2 C28 109.59(16) . . ?
C1 C2 C28 111.94(16) . . ?
N1 C2 H2 109.2 . . ?
C1 C2 H2 109.2 . . ?
C28 C2 H2 109.2 . . ?
N1 C3 C4 122.54(19) . . ?
N1 C3 C22 119.10(19) . . ?
C4 C3 C22 118.35(18) . . ?
C5 C4 C9 118.2(2) . . ?
C5 C4 C3 117.5(2) . . ?
C9 C4 C3 124.14(19) . . ?
C6 C5 C4 122.6(2) . . ?
C6 C5 H5 118.7 . . ?
C4 C5 H5 118.7 . . ?
C5 C6 C7 119.2(2) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 H6 120.4 . . ?
C8 C7 C6 120.1(2) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C7 C8 C9 122.8(2) . . ?
C7 C8 H8 118.6 . . ?
C9 C8 H8 118.6 . . ?
N2 C9 C4 121.34(19) . . ?
N2 C9 C8 121.8(2) . . ?
C4 C9 C8 116.8(2) . . ?
O3 C10 N2 127.5(3) . . ?
O3 C10 C11 119.3(2) . . ?
N2 C10 C11 113.1(2) . . ?
C10 C11 N3 110.6(2) . . ?
C10 C11 C12 109.9(2) . . ?
N3 C11 C12 106.6(2) . . ?
C10 C11 H11 109.9 . . ?
N3 C11 H11 109.9 . . ?
C12 C11 H11 109.9 . . ?
C13 C12 C11 103.9(2) . . ?
C13 C12 H12A 111.0 . . ?
C11 C12 H12A 111.0 . . ?
C13 C12 H12B 111.0 . . ?
C11 C12 H12B 111.0 . . ?
H12A C12 H12B 109.0 . . ?
C12 C13 C14 102.4(2) . . ?
C12 C13 H13A 111.3 . . ?
C14 C13 H13A 111.3 . . ?
C12 C13 H13B 111.3 . . ?
C14 C13 H13B 111.3 . . ?
H13A C13 H13B 109.2 . . ?
N3 C14 C13 103.5(2) . . ?
N3 C14 H14A 111.1 . . ?
C13 C14 H14A 111.1 . . ?
N3 C14 H14B 111.1 . . ?
C13 C14 H14B 111.1 . . ?
H14A C14 H14B 109.0 . . ?
C16 C15 N3 114.23(19) . . ?
C16 C15 H15A 108.7 . . ?
N3 C15 H15A 108.7 . . ?
C16 C15 H15B 108.7 . . ?
N3 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
C21 C16 C17 118.9(3) . . ?
C21 C16 C15 121.1(3) . . ?
C17 C16 C15 120.0(2) . . ?
C18 C17 C16 119.4(3) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C19 C18 C17 120.7(4) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C20 C19 C18 120.2(3) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C19 C20 C21 119.7(3) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C16 C21 C20 121.1(3) . . ?
C16 C21 H21 119.4 . . ?
C20 C21 H21 119.4 . . ?
C23 C22 C27 119.4(2) . . ?
C23 C22 C3 118.1(2) . . ?
C27 C22 C3 122.4(2) . . ?
C22 C23 C24 119.7(3) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C25 C24 C23 120.3(3) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 120.5(3) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C25 C26 C27 120.2(3) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C26 C27 C22 119.8(2) . . ?
C26 C27 H27 120.1 . . ?
C22 C27 H27 120.1 . . ?
C35 C28 C29 112.25(17) . . ?
C35 C28 C2 112.20(16) . . ?
C29 C28 C2 113.36(16) . . ?
C35 C28 H28 106.1 . . ?
C29 C28 H28 106.1 . . ?
C2 C28 H28 106.1 . . ?
C34 C29 C30 118.3(2) . . ?
C34 C29 C28 121.55(19) . . ?
C30 C29 C28 120.1(2) . . ?
C31 C30 C29 120.2(3) . . ?
C31 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
C30 C31 C32 120.4(3) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C33 C32 C31 119.6(3) . . ?
C33 C32 H32 120.2 . . ?
C31 C32 H32 120.2 . . ?
C32 C33 C34 121.3(3) . . ?
C32 C33 H33 119.4 . . ?
C34 C33 H33 119.4 . . ?
C33 C34 C29 120.2(3) . . ?
C33 C34 H34 119.9 . . ?
C29 C34 H34 119.9 . . ?
C36 C35 C38 106.43(19) . . ?
C36 C35 C28 131.12(19) . . ?
C38 C35 C28 122.37(18) . . ?
C35 C36 N4 110.3(2) . . ?
C35 C36 H36 124.8 . . ?
N4 C36 H36 124.8 . . ?
N4 C37 C42 130.1(2) . . ?
N4 C37 C38 107.86(19) . . ?
C42 C37 C38 122.0(2) . . ?
C37 C38 C39 119.0(2) . . ?
C37 C38 C35 107.15(19) . . ?
C39 C38 C35 133.8(2) . . ?
C40 C39 C38 118.5(2) . . ?
C40 C39 H39 120.7 . . ?
C38 C39 H39 120.7 . . ?
C39 C40 C41 121.5(3) . . ?
C39 C40 H40 119.2 . . ?
C41 C40 H40 119.2 . . ?
C42 C41 C40 121.5(2) . . ?
C42 C41 H41 119.2 . . ?
C40 C41 H41 119.2 . . ?
C41 C42 C37 117.3(2) . . ?
C41 C42 H42 121.3 . . ?
C37 C42 H42 121.3 . . ?
O4 C43 O5 123.1(3) . . ?
O4 C43 C44 124.8(3) . . ?
O5 C43 C44 112.0(2) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O5 C45 C46 108.1(3) . . ?
O5 C45 H45A 110.1 . . ?
C46 C45 H45A 110.1 . . ?
O5 C45 H45B 110.1 . . ?
C46 C45 H45B 110.1 . . ?
H45A C45 H45B 108.4 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 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
N1 Ni1 O2 C1 1.09(15) . . . . ?
N2 Ni1 O2 C1 113.6(7) . . . . ?
N3 Ni1 O2 C1 -174.07(15) . . . . ?
N2 Ni1 N1 C3 -10.12(18) . . . . ?
O2 Ni1 N1 C3 163.77(18) . . . . ?
N3 Ni1 N1 C3 -148.9(6) . . . . ?
N2 Ni1 N1 C2 174.10(13) . . . . ?
O2 Ni1 N1 C2 -12.01(13) . . . . ?
N3 Ni1 N1 C2 35.4(8) . . . . ?
N1 Ni1 N2 C10 169.01(16) . . . . ?
O2 Ni1 N2 C10 57.0(7) . . . . ?
N3 Ni1 N2 C10 -15.33(17) . . . . ?
N1 Ni1 N2 C9 -1.00(17) . . . . ?
O2 Ni1 N2 C9 -113.0(7) . . . . ?
N3 Ni1 N2 C9 174.67(17) . . . . ?
N1 Ni1 N3 C14 26.1(8) . . . . ?
N2 Ni1 N3 C14 -112.94(16) . . . . ?
O2 Ni1 N3 C14 73.33(16) . . . . ?
N1 Ni1 N3 C15 -94.3(7) . . . . ?
N2 Ni1 N3 C15 126.67(16) . . . . ?
O2 Ni1 N3 C15 -47.06(16) . . . . ?
N1 Ni1 N3 C11 138.6(7) . . . . ?
N2 Ni1 N3 C11 -0.41(15) . . . . ?
O2 Ni1 N3 C11 -174.14(14) . . . . ?
Ni1 O2 C1 O1 -171.24(16) . . . . ?
Ni1 O2 C1 C2 10.1(2) . . . . ?
C3 N1 C2 C1 -157.23(18) . . . . ?
Ni1 N1 C2 C1 18.95(18) . . . . ?
C3 N1 C2 C28 80.8(2) . . . . ?
Ni1 N1 C2 C28 -103.06(16) . . . . ?
O1 C1 C2 N1 162.55(18) . . . . ?
O2 C1 C2 N1 -18.8(2) . . . . ?
O1 C1 C2 C28 -76.9(2) . . . . ?
O2 C1 C2 C28 101.8(2) . . . . ?
C2 N1 C3 C4 -170.71(17) . . . . ?
Ni1 N1 C3 C4 13.8(3) . . . . ?
C2 N1 C3 C22 8.9(3) . . . . ?
Ni1 N1 C3 C22 -166.61(14) . . . . ?
N1 C3 C4 C5 170.1(2) . . . . ?
C22 C3 C4 C5 -9.5(3) . . . . ?
N1 C3 C4 C9 -4.8(3) . . . . ?
C22 C3 C4 C9 175.59(19) . . . . ?
C9 C4 C5 C6 3.2(4) . . . . ?
C3 C4 C5 C6 -172.0(2) . . . . ?
C4 C5 C6 C7 0.9(4) . . . . ?
C5 C6 C7 C8 -3.3(4) . . . . ?
C6 C7 C8 C9 1.7(4) . . . . ?
C10 N2 C9 C4 -161.2(2) . . . . ?
Ni1 N2 C9 C4 8.1(3) . . . . ?
C10 N2 C9 C8 22.5(3) . . . . ?
Ni1 N2 C9 C8 -168.16(16) . . . . ?
C5 C4 C9 N2 178.83(19) . . . . ?
C3 C4 C9 N2 -6.3(3) . . . . ?
C5 C4 C9 C8 -4.7(3) . . . . ?
C3 C4 C9 C8 170.2(2) . . . . ?
C7 C8 C9 N2 178.9(2) . . . . ?
C7 C8 C9 C4 2.4(3) . . . . ?
C9 N2 C10 O3 16.1(4) . . . . ?
Ni1 N2 C10 O3 -154.7(3) . . . . ?
C9 N2 C10 C11 -161.88(19) . . . . ?
Ni1 N2 C10 C11 27.4(3) . . . . ?
O3 C10 C11 N3 154.5(3) . . . . ?
N2 C10 C11 N3 -27.4(3) . . . . ?
O3 C10 C11 C12 -88.1(3) . . . . ?
N2 C10 C11 C12 90.0(3) . . . . ?
C14 N3 C11 C10 126.6(2) . . . . ?
C15 N3 C11 C10 -114.4(2) . . . . ?
Ni1 N3 C11 C10 14.5(2) . . . . ?
C14 N3 C11 C12 7.2(3) . . . . ?
C15 N3 C11 C12 126.2(2) . . . . ?
Ni1 N3 C11 C12 -104.94(19) . . . . ?
C10 C11 C12 C13 -100.8(3) . . . . ?
N3 C11 C12 C13 19.1(3) . . . . ?
C11 C12 C13 C14 -37.4(3) . . . . ?
C15 N3 C14 C13 -151.7(2) . . . . ?
C11 N3 C14 C13 -30.4(2) . . . . ?
Ni1 N3 C14 C13 83.6(2) . . . . ?
C12 C13 C14 N3 42.3(2) . . . . ?
C14 N3 C15 C16 176.6(2) . . . . ?
C11 N3 C15 C16 59.5(3) . . . . ?
Ni1 N3 C15 C16 -65.2(2) . . . . ?
N3 C15 C16 C21 -100.4(3) . . . . ?
N3 C15 C16 C17 83.3(3) . . . . ?
C21 C16 C17 C18 2.5(4) . . . . ?
C15 C16 C17 C18 178.9(3) . . . . ?
C16 C17 C18 C19 -0.3(5) . . . . ?
C17 C18 C19 C20 -1.5(6) . . . . ?
C18 C19 C20 C21 1.0(5) . . . . ?
C17 C16 C21 C20 -3.0(4) . . . . ?
C15 C16 C21 C20 -179.4(3) . . . . ?
C19 C20 C21 C16 1.3(5) . . . . ?
N1 C3 C22 C23 87.8(3) . . . . ?
C4 C3 C22 C23 -92.6(3) . . . . ?
N1 C3 C22 C27 -93.1(3) . . . . ?
C4 C3 C22 C27 86.5(3) . . . . ?
C27 C22 C23 C24 0.8(4) . . . . ?
C3 C22 C23 C24 179.9(2) . . . . ?
C22 C23 C24 C25 -0.2(5) . . . . ?
C23 C24 C25 C26 0.5(5) . . . . ?
C24 C25 C26 C27 -1.4(4) . . . . ?
C25 C26 C27 C22 2.1(4) . . . . ?
C23 C22 C27 C26 -1.7(4) . . . . ?
C3 C22 C27 C26 179.2(2) . . . . ?
N1 C2 C28 C35 -149.37(17) . . . . ?
C1 C2 C28 C35 91.2(2) . . . . ?
N1 C2 C28 C29 82.2(2) . . . . ?
C1 C2 C28 C29 -37.3(2) . . . . ?
C35 C28 C29 C34 -43.7(3) . . . . ?
C2 C28 C29 C34 84.7(2) . . . . ?
C35 C28 C29 C30 133.0(2) . . . . ?
C2 C28 C29 C30 -98.6(2) . . . . ?
C34 C29 C30 C31 -0.9(4) . . . . ?
C28 C29 C30 C31 -177.8(2) . . . . ?
C29 C30 C31 C32 -1.2(4) . . . . ?
C30 C31 C32 C33 2.3(5) . . . . ?
C31 C32 C33 C34 -1.2(5) . . . . ?
C32 C33 C34 C29 -1.0(5) . . . . ?
C30 C29 C34 C33 2.0(4) . . . . ?
C28 C29 C34 C33 178.8(2) . . . . ?
C29 C28 C35 C36 103.0(3) . . . . ?
C2 C28 C35 C36 -26.0(3) . . . . ?
C29 C28 C35 C38 -73.2(2) . . . . ?
C2 C28 C35 C38 157.72(19) . . . . ?
C38 C35 C36 N4 0.5(3) . . . . ?
C28 C35 C36 N4 -176.2(2) . . . . ?
C37 N4 C36 C35 0.4(3) . . . . ?
C36 N4 C37 C42 177.1(2) . . . . ?
C36 N4 C37 C38 -1.2(2) . . . . ?
N4 C37 C38 C39 -177.5(2) . . . . ?
C42 C37 C38 C39 3.9(3) . . . . ?
N4 C37 C38 C35 1.5(2) . . . . ?
C42 C37 C38 C35 -177.0(2) . . . . ?
C36 C35 C38 C37 -1.3(2) . . . . ?
C28 C35 C38 C37 175.77(18) . . . . ?
C36 C35 C38 C39 177.6(3) . . . . ?
C28 C35 C38 C39 -5.3(4) . . . . ?
C37 C38 C39 C40 -1.2(4) . . . . ?
C35 C38 C39 C40 -180.0(2) . . . . ?
C38 C39 C40 C41 -2.0(4) . . . . ?
C39 C40 C41 C42 2.6(4) . . . . ?
C40 C41 C42 C37 0.1(4) . . . . ?
N4 C37 C42 C41 178.5(2) . . . . ?
C38 C37 C42 C41 -3.3(3) . . . . ?
C45 O5 C43 O4 -5.0(5) . . . . ?
C45 O5 C43 C44 176.3(3) . . . . ?
C43 O5 C45 C46 168.1(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4 H4 O1 0.93(3) 2.01(3) 2.905(3) 161(3) 2_647
N4 H4 O2 0.93(3) 2.55(3) 3.249(2) 132(3) 2_647

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.045