
#=============================================================================
data_Compound-1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H38 Co3 N2 O17'
_chemical_formula_sum            'C36 H38 Co3 N2 O17'
_chemical_formula_weight         947.47

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbcn
_symmetry_space_group_name_hall  '-P 2n 2ab'

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

_cell_length_a                   9.694(5)
_cell_length_b                   24.8060(10)
_cell_length_c                   15.8790(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3818(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4208
_cell_measurement_theta_min      3.2317
_cell_measurement_theta_max      29.0955

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1940
_exptl_absorpt_coefficient_mu    1.368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7348
_exptl_absorpt_correction_T_max  0.8211
_exptl_absorpt_process_details   
;
CrysAlis (Oxford Diffraction, 2006)
;
_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  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13088
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.24
_diffrn_reflns_theta_max         25.03
_reflns_number_total             3360
_reflns_number_gt                2897
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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.

For  o1w, o2w,  o3w and o3w' atoms, some anisotropic 
displacement ellipsoids were rather elongated which led us to use 
the ISOR restraints.
;

_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)+(0.0440P)²+4.5639P] 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         3360
_refine_ls_number_parameters     281
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0935
_refine_ls_wR_factor_gt          0.0879
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.077
_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
Co1 Co 0.33125(3) 0.303321(14) 0.50189(2) 0.02294(13) Uani 1 1 d . . .
Co2 Co 1.0000 0.68890(2) 0.7500 0.02657(15) Uani 1 2 d S . .
C1 C 0.2867(3) 0.35719(11) 0.63304(18) 0.0293(6) Uani 1 1 d . . .
C2 C 0.2393(3) 0.37691(12) 0.71764(17) 0.0318(6) Uani 1 1 d . . .
C3 C 0.1986(4) 0.33786(15) 0.7753(2) 0.0474(8) Uani 1 1 d . . .
H3 H 0.2083 0.3016 0.7619 0.057 Uiso 1 1 calc R . .
C4 C 0.1439(4) 0.35239(17) 0.8520(2) 0.0587(10) Uani 1 1 d . . .
H4 H 0.1162 0.3261 0.8901 0.070 Uiso 1 1 calc R . .
C5 C 0.1307(4) 0.40611(18) 0.8720(2) 0.0582(10) Uani 1 1 d . . .
H5 H 0.0922 0.4160 0.9233 0.070 Uiso 1 1 calc R . .
C6 C 0.1741(4) 0.44552(15) 0.8164(2) 0.0467(8) Uani 1 1 d . . .
H6 H 0.1662 0.4816 0.8313 0.056 Uiso 1 1 calc R . .
C7 C 0.2295(3) 0.43169(12) 0.73825(18) 0.0328(7) Uani 1 1 d . . .
C8 C 0.2859(3) 0.47474(12) 0.68266(18) 0.0315(6) Uani 1 1 d . . .
C9 C 0.2103(3) 0.52011(13) 0.6617(2) 0.0418(8) Uani 1 1 d . . .
H9 H 0.1202 0.5235 0.6810 0.050 Uiso 1 1 calc R . .
C10 C 0.2668(3) 0.56064(12) 0.6122(2) 0.0399(7) Uani 1 1 d . . .
H10 H 0.2137 0.5906 0.5982 0.048 Uiso 1 1 calc R . .
C11 C 0.4021(3) 0.55707(11) 0.58306(17) 0.0295(6) Uani 1 1 d . . .
C12 C 0.4774(3) 0.51139(11) 0.60439(18) 0.0294(6) Uani 1 1 d . . .
H12 H 0.5678 0.5080 0.5855 0.035 Uiso 1 1 calc R . .
C13 C 0.4208(3) 0.47083(11) 0.65316(17) 0.0297(6) Uani 1 1 d . . .
H13 H 0.4734 0.4406 0.6664 0.036 Uiso 1 1 calc R . .
C14 C 0.4686(3) 0.60057(11) 0.52994(18) 0.0295(6) Uani 1 1 d . . .
H14A H 0.5336 0.5837 0.4917 0.035 Uiso 1 1 calc R . .
H14B H 0.3976 0.6175 0.4960 0.035 Uiso 1 1 calc R . .
C15 C 0.4451(3) 0.68094(11) 0.61897(17) 0.0262(6) Uani 1 1 d . . .
H15A H 0.4887 0.6973 0.6677 0.031 Uiso 1 1 calc R . .
H15B H 0.3645 0.6613 0.6381 0.031 Uiso 1 1 calc R . .
C16 C 0.4014(3) 0.72478(10) 0.55725(17) 0.0248(6) Uani 1 1 d . . .
C17 C 0.6411(3) 0.62085(11) 0.63949(18) 0.0277(6) Uani 1 1 d . . .
H17A H 0.6826 0.5885 0.6165 0.033 Uiso 1 1 calc R . .
H17B H 0.5926 0.6111 0.6907 0.033 Uiso 1 1 calc R . .
C18 C 0.7524(3) 0.66148(12) 0.65955(17) 0.0278(6) Uani 1 1 d . . .
N1 N 0.5425(2) 0.64342(9) 0.57813(13) 0.0227(5) Uani 1 1 d . . .
O1 O 0.2245(2) 0.36994(9) 0.56642(12) 0.0367(5) Uani 1 1 d . . .
O2 O 0.3860(2) 0.32444(8) 0.62895(12) 0.0347(5) Uani 1 1 d . . .
O3 O 0.49169(19) 0.74238(8) 0.50829(12) 0.0303(5) Uani 1 1 d . . .
O4 O 0.27973(18) 0.74185(8) 0.56198(12) 0.0316(5) Uani 1 1 d . . .
O5 O 0.77224(19) 0.69995(8) 0.60892(12) 0.0311(5) Uani 1 1 d . . .
O6 O 0.8200(2) 0.65344(9) 0.72545(12) 0.0369(5) Uani 1 1 d . . .
O1W O 1.0000 0.76724(14) 0.7500 0.0461(9) Uani 1 2 d SU . .
H1A H 0.960(4) 0.7869(17) 0.782(2) 0.069 Uiso 1 1 d . . .
O2W O 1.0587(2) 0.68391(9) 0.62235(13) 0.0322(5) Uani 1 1 d U . .
H2A H 1.002(4) 0.7013(15) 0.594(2) 0.048 Uiso 1 1 d . . .
H2B H 1.127(4) 0.7035(15) 0.612(2) 0.048 Uiso 1 1 d . . .
O3W O 0.8656(8) 0.5355(3) 0.5237(4) 0.0594(16) Uani 0.50 1 d PU . .
O3W' O 0.9083(11) 0.5535(4) 0.5393(7) 0.105(4) Uani 0.50 1 d PU . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
Co1 O5 2.0271(19) 5_666 ?
Co1 O3 2.063(2) 5_666 ?
Co1 O4 2.0960(19) 7_655 ?
Co1 O2 2.1511(19) . ?
Co1 O1 2.203(2) . ?
Co1 N1 2.204(2) 5_666 ?
Co1 C1 2.512(3) . ?
Co2 O1W 1.943(3) . ?
Co2 O6 1.993(2) . ?
Co2 O6 1.993(2) 4_756 ?
Co2 O2W 2.109(2) . ?
Co2 O2W 2.109(2) 4_756 ?
C1 O1 1.258(3) . ?
C1 O2 1.262(4) . ?
C1 C2 1.502(4) . ?
C2 C3 1.390(4) . ?
C2 C7 1.401(4) . ?
C3 C4 1.377(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.376(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.382(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.395(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.489(4) . ?
C8 C9 1.384(4) . ?
C8 C13 1.393(4) . ?
C9 C10 1.389(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.394(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.390(4) . ?
C11 C14 1.514(4) . ?
C12 C13 1.383(4) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 N1 1.493(3) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N1 1.476(3) . ?
C15 C16 1.524(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 O3 1.249(3) . ?
C16 O4 1.256(3) . ?
C17 N1 1.475(3) . ?
C17 C18 1.510(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 O6 1.251(3) . ?
C18 O5 1.263(3) . ?
N1 Co1 2.204(2) 5_666 ?
O3 Co1 2.063(2) 5_666 ?
O4 Co1 2.0960(19) 7_665 ?
O5 Co1 2.0271(19) 5_666 ?
O1W H1A 0.80(4) . ?
O2W H2A 0.83(4) . ?
O2W H2B 0.84(4) . ?
O3W O3W' 0.656(10) . ?

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
O5 Co1 O3 108.77(8) 5_666 5_666 ?
O5 Co1 O4 96.43(8) 5_666 7_655 ?
O3 Co1 O4 93.61(8) 5_666 7_655 ?
O5 Co1 O2 161.10(8) 5_666 . ?
O3 Co1 O2 90.11(8) 5_666 . ?
O4 Co1 O2 82.93(8) 7_655 . ?
O5 Co1 O1 101.60(8) 5_666 . ?
O3 Co1 O1 147.09(8) 5_666 . ?
O4 Co1 O1 95.33(8) 7_655 . ?
O2 Co1 O1 59.80(8) . . ?
O5 Co1 N1 78.36(8) 5_666 5_666 ?
O3 Co1 N1 79.76(8) 5_666 5_666 ?
O4 Co1 N1 169.59(8) 7_655 5_666 ?
O2 Co1 N1 104.93(8) . 5_666 ?
O1 Co1 N1 94.56(8) . 5_666 ?
O5 Co1 C1 130.98(9) 5_666 . ?
O3 Co1 C1 120.03(9) 5_666 . ?
O4 Co1 C1 85.49(8) 7_655 . ?
O2 Co1 C1 30.15(9) . . ?
O1 Co1 C1 30.05(8) . . ?
N1 Co1 C1 104.75(8) 5_666 . ?
O1W Co2 O6 116.19(7) . . ?
O1W Co2 O6 116.19(7) . 4_756 ?
O6 Co2 O6 127.62(14) . 4_756 ?
O1W Co2 O2W 93.36(6) . . ?
O6 Co2 O2W 91.28(9) . . ?
O6 Co2 O2W 85.75(8) 4_756 . ?
O1W Co2 O2W 93.36(6) . 4_756 ?
O6 Co2 O2W 85.75(8) . 4_756 ?
O6 Co2 O2W 91.28(9) 4_756 4_756 ?
O2W Co2 O2W 173.28(12) . 4_756 ?
O1 C1 O2 119.0(3) . . ?
O1 C1 C2 121.6(3) . . ?
O2 C1 C2 119.3(3) . . ?
O1 C1 Co1 61.25(15) . . ?
O2 C1 Co1 58.90(14) . . ?
C2 C1 Co1 165.38(19) . . ?
C3 C2 C7 120.2(3) . . ?
C3 C2 C1 116.7(3) . . ?
C7 C2 C1 123.1(3) . . ?
C4 C3 C2 120.6(3) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C5 C4 C3 119.6(3) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 120.6(3) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C7 120.7(3) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C6 C7 C2 118.2(3) . . ?
C6 C7 C8 119.5(3) . . ?
C2 C7 C8 122.2(3) . . ?
C9 C8 C13 118.2(3) . . ?
C9 C8 C7 122.1(3) . . ?
C13 C8 C7 119.6(3) . . ?
C8 C9 C10 121.1(3) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C9 C10 C11 120.9(3) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 H10 119.6 . . ?
C12 C11 C10 117.7(3) . . ?
C12 C11 C14 119.6(3) . . ?
C10 C11 C14 122.7(3) . . ?
C13 C12 C11 121.4(3) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C12 C13 C8 120.7(3) . . ?
C12 C13 H13 119.7 . . ?
C8 C13 H13 119.7 . . ?
N1 C14 C11 115.2(2) . . ?
N1 C14 H14A 108.5 . . ?
C11 C14 H14A 108.5 . . ?
N1 C14 H14B 108.5 . . ?
C11 C14 H14B 108.5 . . ?
H14A C14 H14B 107.5 . . ?
N1 C15 C16 110.2(2) . . ?
N1 C15 H15A 109.6 . . ?
C16 C15 H15A 109.6 . . ?
N1 C15 H15B 109.6 . . ?
C16 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
O3 C16 O4 125.3(2) . . ?
O3 C16 C15 117.1(2) . . ?
O4 C16 C15 117.6(2) . . ?
N1 C17 C18 110.4(2) . . ?
N1 C17 H17A 109.6 . . ?
C18 C17 H17A 109.6 . . ?
N1 C17 H17B 109.6 . . ?
C18 C17 H17B 109.6 . . ?
H17A C17 H17B 108.1 . . ?
O6 C18 O5 125.0(3) . . ?
O6 C18 C17 116.4(2) . . ?
O5 C18 C17 118.6(2) . . ?
C17 N1 C15 111.3(2) . . ?
C17 N1 C14 112.3(2) . . ?
C15 N1 C14 111.6(2) . . ?
C17 N1 Co1 104.41(15) . 5_666 ?
C15 N1 Co1 103.33(15) . 5_666 ?
C14 N1 Co1 113.44(16) . 5_666 ?
C1 O1 Co1 88.70(17) . . ?
C1 O2 Co1 90.96(17) . . ?
C16 O3 Co1 116.07(17) . 5_666 ?
C16 O4 Co1 134.45(18) . 7_665 ?
C18 O5 Co1 116.55(17) . 5_666 ?
C18 O6 Co2 123.52(18) . . ?
Co2 O1W H1A 128(3) . . ?
Co2 O2W H2A 108(2) . . ?
Co2 O2W H2B 111(2) . . ?
H2A O2W H2B 97(3) . . ?

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
O5 Co1 C1 O1 -14.2(2) 5_666 . . . ?
O3 Co1 C1 O1 159.62(15) 5_666 . . . ?
O4 Co1 C1 O1 -108.81(17) 7_655 . . . ?
O2 Co1 C1 O1 167.5(3) . . . . ?
N1 Co1 C1 O1 73.07(17) 5_666 . . . ?
O5 Co1 C1 O2 178.29(14) 5_666 . . . ?
O3 Co1 C1 O2 -7.88(19) 5_666 . . . ?
O4 Co1 C1 O2 83.69(16) 7_655 . . . ?
O1 Co1 C1 O2 -167.5(3) . . . . ?
N1 Co1 C1 O2 -94.43(17) 5_666 . . . ?
O5 Co1 C1 C2 91.1(8) 5_666 . . . ?
O3 Co1 C1 C2 -95.1(8) 5_666 . . . ?
O4 Co1 C1 C2 -3.5(8) 7_655 . . . ?
O2 Co1 C1 C2 -87.2(8) . . . . ?
O1 Co1 C1 C2 105.3(9) . . . . ?
N1 Co1 C1 C2 178.4(8) 5_666 . . . ?
O1 C1 C2 C3 118.0(3) . . . . ?
O2 C1 C2 C3 -57.6(4) . . . . ?
Co1 C1 C2 C3 21.1(10) . . . . ?
O1 C1 C2 C7 -59.2(4) . . . . ?
O2 C1 C2 C7 125.2(3) . . . . ?
Co1 C1 C2 C7 -156.1(7) . . . . ?
C7 C2 C3 C4 2.2(5) . . . . ?
C1 C2 C3 C4 -175.1(3) . . . . ?
C2 C3 C4 C5 -0.5(6) . . . . ?
C3 C4 C5 C6 -1.2(6) . . . . ?
C4 C5 C6 C7 1.3(6) . . . . ?
C5 C6 C7 C2 0.3(5) . . . . ?
C5 C6 C7 C8 -175.0(3) . . . . ?
C3 C2 C7 C6 -2.0(5) . . . . ?
C1 C2 C7 C6 175.1(3) . . . . ?
C3 C2 C7 C8 173.2(3) . . . . ?
C1 C2 C7 C8 -9.7(5) . . . . ?
C6 C7 C8 C9 -52.2(4) . . . . ?
C2 C7 C8 C9 132.6(3) . . . . ?
C6 C7 C8 C13 125.1(3) . . . . ?
C2 C7 C8 C13 -50.0(4) . . . . ?
C13 C8 C9 C10 0.3(5) . . . . ?
C7 C8 C9 C10 177.7(3) . . . . ?
C8 C9 C10 C11 -0.8(5) . . . . ?
C9 C10 C11 C12 0.8(4) . . . . ?
C9 C10 C11 C14 -179.2(3) . . . . ?
C10 C11 C12 C13 -0.3(4) . . . . ?
C14 C11 C12 C13 179.7(3) . . . . ?
C11 C12 C13 C8 -0.2(4) . . . . ?
C9 C8 C13 C12 0.2(4) . . . . ?
C7 C8 C13 C12 -177.2(3) . . . . ?
C12 C11 C14 N1 -89.5(3) . . . . ?
C10 C11 C14 N1 90.5(3) . . . . ?
N1 C15 C16 O3 -38.0(3) . . . . ?
N1 C15 C16 O4 144.8(2) . . . . ?
N1 C17 C18 O6 161.8(2) . . . . ?
N1 C17 C18 O5 -19.4(4) . . . . ?
C18 C17 N1 C15 -77.9(3) . . . . ?
C18 C17 N1 C14 156.2(2) . . . . ?
C18 C17 N1 Co1 32.9(2) . . . 5_666 ?
C16 C15 N1 C17 149.1(2) . . . . ?
C16 C15 N1 C14 -84.6(3) . . . . ?
C16 C15 N1 Co1 37.6(2) . . . 5_666 ?
C11 C14 N1 C17 51.2(3) . . . . ?
C11 C14 N1 C15 -74.5(3) . . . . ?
C11 C14 N1 Co1 169.27(19) . . . 5_666 ?
O2 C1 O1 Co1 12.2(3) . . . . ?
C2 C1 O1 Co1 -163.4(2) . . . . ?
O5 Co1 O1 C1 169.10(16) 5_666 . . . ?
O3 Co1 O1 C1 -33.7(2) 5_666 . . . ?
O4 Co1 O1 C1 71.40(17) 7_655 . . . ?
O2 Co1 O1 C1 -7.22(15) . . . . ?
N1 Co1 O1 C1 -111.86(17) 5_666 . . . ?
O1 C1 O2 Co1 -12.5(3) . . . . ?
C2 C1 O2 Co1 163.2(2) . . . . ?
O5 Co1 O2 C1 -4.0(3) 5_666 . . . ?
O3 Co1 O2 C1 173.18(16) 5_666 . . . ?
O4 Co1 O2 C1 -93.19(17) 7_655 . . . ?
O1 Co1 O2 C1 7.20(15) . . . . ?
N1 Co1 O2 C1 93.76(17) 5_666 . . . ?
O4 C16 O3 Co1 -168.1(2) . . . 5_666 ?
C15 C16 O3 Co1 15.0(3) . . . 5_666 ?
O3 C16 O4 Co1 -1.9(4) . . . 7_665 ?
C15 C16 O4 Co1 174.93(18) . . . 7_665 ?
O6 C18 O5 Co1 170.5(2) . . . 5_666 ?
C17 C18 O5 Co1 -8.1(3) . . . 5_666 ?
O5 C18 O6 Co2 -15.2(4) . . . . ?
C17 C18 O6 Co2 163.46(19) . . . . ?
O1W Co2 O6 C18 57.4(2) . . . . ?
O6 Co2 O6 C18 -122.6(2) 4_756 . . . ?
O2W Co2 O6 C18 -37.0(2) . . . . ?
O2W Co2 O6 C18 149.1(2) 4_756 . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.064
#=========================END
data_Compound-2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H38 N2 O17 Zn3'
_chemical_formula_sum            'C36 H38 N2 O17 Zn3'
_chemical_formula_weight         966.79

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c n'
_symmetry_space_group_name_hall  '-P 2n 2ab'


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

_cell_length_a                   9.6780(4)
_cell_length_b                   24.8730(12)
_cell_length_c                   15.8270(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3809.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3644
_cell_measurement_theta_min      3.2289
_cell_measurement_theta_max      29.2293

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1976
_exptl_absorpt_coefficient_mu    1.954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6408
_exptl_absorpt_correction_T_max  0.7582
_exptl_absorpt_process_details   
;
CrysAlis (Oxford Diffraction, 2006)
;
_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  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13065
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.24
_diffrn_reflns_theta_max         25.02
_reflns_number_total             3355
_reflns_number_gt                2843
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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.

For o2w atom, some anisotropic displacement ellipsoids were rather 
elongated which led us to use the ISOR restraints.
;

_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)+(0.0367P)²+2.4206P] 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         3355
_refine_ls_number_parameters     272
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0317
_refine_ls_wR_factor_ref         0.0799
_refine_ls_wR_factor_gt          0.0753
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.082
_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
Zn1 Zn 0.83205(3) 0.196724(12) 0.003181(18) 0.02409(11) Uani 1 1 d . . .
Zn2 Zn 1.5000 -0.189928(17) 0.2500 0.02522(13) Uani 1 2 d S . .
C1 C 0.7823(3) 0.14125(11) 0.13336(18) 0.0313(7) Uani 1 1 d . . .
C2 C 0.7382(3) 0.12178(11) 0.21943(17) 0.0321(6) Uani 1 1 d . . .
C3 C 0.6981(4) 0.16035(13) 0.2778(2) 0.0460(8) Uani 1 1 d . . .
H3 H 0.7076 0.1966 0.2644 0.055 Uiso 1 1 calc R . .
C4 C 0.6444(4) 0.14618(16) 0.3551(2) 0.0553(10) Uani 1 1 d . . .
H4 H 0.6164 0.1725 0.3932 0.066 Uiso 1 1 calc R . .
C5 C 0.6326(4) 0.09247(16) 0.3752(2) 0.0557(10) Uani 1 1 d . . .
H5 H 0.5959 0.0824 0.4272 0.067 Uiso 1 1 calc R . .
C6 C 0.6747(3) 0.05360(14) 0.3188(2) 0.0448(8) Uani 1 1 d . . .
H6 H 0.6671 0.0175 0.3337 0.054 Uiso 1 1 calc R . .
C7 C 0.7282(3) 0.06717(11) 0.24039(18) 0.0326(7) Uani 1 1 d . . .
C8 C 0.7849(3) 0.02452(11) 0.18402(17) 0.0300(6) Uani 1 1 d . . .
C9 C 0.9193(3) 0.02841(11) 0.15333(17) 0.0287(6) Uani 1 1 d . . .
H9 H 0.9718 0.0587 0.1659 0.034 Uiso 1 1 calc R . .
C10 C 0.9760(3) -0.01175(10) 0.10474(18) 0.0282(6) Uani 1 1 d . . .
H10 H 1.0664 -0.0083 0.0857 0.034 Uiso 1 1 calc R . .
C11 C 0.9005(3) -0.05755(11) 0.08350(17) 0.0286(6) Uani 1 1 d . . .
C12 C 0.7657(3) -0.06121(11) 0.1135(2) 0.0382(7) Uani 1 1 d . . .
H12 H 0.7125 -0.0911 0.0998 0.046 Uiso 1 1 calc R . .
C13 C 0.7094(3) -0.02105(12) 0.1635(2) 0.0402(8) Uani 1 1 d . . .
H13 H 0.6195 -0.0247 0.1835 0.048 Uiso 1 1 calc R . .
C14 C 0.9664(3) -0.10060(11) 0.03020(18) 0.0297(6) Uani 1 1 d . . .
H14A H 0.8952 -0.1174 -0.0038 0.036 Uiso 1 1 calc R . .
H14B H 1.0314 -0.0837 -0.0081 0.036 Uiso 1 1 calc R . .
C15 C 0.9436(3) -0.18121(10) 0.11842(16) 0.0252(6) Uani 1 1 d . . .
H15A H 0.8628 -0.1617 0.1378 0.030 Uiso 1 1 calc R . .
H15B H 0.9872 -0.1977 0.1671 0.030 Uiso 1 1 calc R . .
C16 C 0.8996(3) -0.22483(10) 0.05606(16) 0.0241(6) Uani 1 1 d . . .
C17 C 1.1401(3) -0.12152(10) 0.13956(17) 0.0257(6) Uani 1 1 d . . .
H17A H 1.0921 -0.1124 0.1914 0.031 Uiso 1 1 calc R . .
H17B H 1.1804 -0.0888 0.1170 0.031 Uiso 1 1 calc R . .
C18 C 1.2536(3) -0.16140(11) 0.15868(16) 0.0259(6) Uani 1 1 d . . .
N1 N 1.0408(2) -0.14357(8) 0.07827(13) 0.0222(5) Uani 1 1 d . . .
O1 O 0.8822(2) 0.17378(8) 0.12861(12) 0.0395(5) Uani 1 1 d . . .
O2 O 0.7183(2) 0.12842(9) 0.06855(12) 0.0419(5) Uani 1 1 d . . .
O3 O 1.32111(19) -0.15324(8) 0.22471(12) 0.0343(5) Uani 1 1 d . . .
O4 O 1.2751(2) -0.19912(7) 0.10725(12) 0.0313(5) Uani 1 1 d . . .
O5 O 0.99042(19) -0.24297(7) 0.00742(12) 0.0297(4) Uani 1 1 d . . .
O6 O 0.77674(19) -0.24090(8) 0.05984(12) 0.0331(5) Uani 1 1 d . . .
O1W O 1.4409(2) -0.18384(9) 0.37687(13) 0.0336(5) Uani 1 1 d . . .
H1A H 1.371(4) -0.1998(14) 0.393(2) 0.050 Uiso 1 1 d . . .
H1B H 1.494(4) -0.1968(14) 0.404(2) 0.050 Uiso 1 1 d . . .
O2W O 1.5000 -0.26869(13) 0.2500 0.0511(10) Uani 1 2 d SU . .
H2A H 1.530(5) -0.2858(17) 0.217(3) 0.077 Uiso 1 1 d . . .
O3W O 0.6218(4) 0.04071(16) -0.0291(2) 0.1167(14) Uani 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
Zn1 O4 2.0330(18) 5_755 ?
Zn1 O5 2.0744(19) 5_755 ?
Zn1 O6 2.0785(18) 7_765 ?
Zn1 O1 2.122(2) . ?
Zn1 N1 2.219(2) 5_755 ?
Zn1 O2 2.274(2) . ?
Zn1 C1 2.526(3) . ?
Zn2 O2W 1.959(3) . ?
Zn2 O3 1.9976(18) 4_855 ?
Zn2 O3 1.9976(18) . ?
Zn2 O1W 2.093(2) . ?
Zn2 O1W 2.093(2) 4_855 ?
C1 O2 1.240(3) . ?
C1 O1 1.263(4) . ?
C1 C2 1.507(4) . ?
C2 C3 1.387(4) . ?
C2 C7 1.402(4) . ?
C3 C4 1.375(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.378(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.377(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.387(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.491(4) . ?
C8 C13 1.387(4) . ?
C8 C9 1.392(4) . ?
C9 C10 1.375(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.395(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.391(4) . ?
C11 C14 1.505(4) . ?
C12 C13 1.386(4) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 N1 1.496(3) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N1 1.471(3) . ?
C15 C16 1.528(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 O5 1.253(3) . ?
C16 O6 1.256(3) . ?
C17 N1 1.472(3) . ?
C17 C18 1.511(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 O3 1.249(3) . ?
C18 O4 1.259(3) . ?
N1 Zn1 2.219(2) 5_755 ?
O4 Zn1 2.0330(18) 5_755 ?
O5 Zn1 2.0744(19) 5_755 ?
O6 Zn1 2.0785(18) 7_755 ?
O1W H1A 0.83(4) . ?
O1W H1B 0.74(4) . ?
O2W H2A 0.73(4) . ?

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
O4 Zn1 O5 109.67(8) 5_755 5_755 ?
O4 Zn1 O6 95.21(7) 5_755 7_765 ?
O5 Zn1 O6 92.32(7) 5_755 7_765 ?
O4 Zn1 O1 158.26(8) 5_755 . ?
O5 Zn1 O1 92.02(8) 5_755 . ?
O6 Zn1 O1 85.01(8) 7_765 . ?
O4 Zn1 N1 78.50(7) 5_755 5_755 ?
O5 Zn1 N1 79.87(7) 5_755 5_755 ?
O6 Zn1 N1 167.51(8) 7_765 5_755 ?
O1 Zn1 N1 104.86(8) . 5_755 ?
O4 Zn1 O2 99.56(8) 5_755 . ?
O5 Zn1 O2 148.46(8) 5_755 . ?
O6 Zn1 O2 96.67(8) 7_765 . ?
O1 Zn1 O2 58.95(8) . . ?
N1 Zn1 O2 95.03(8) 5_755 . ?
O4 Zn1 C1 128.32(9) 5_755 . ?
O5 Zn1 C1 121.78(9) 5_755 . ?
O6 Zn1 C1 87.67(8) 7_765 . ?
O1 Zn1 C1 29.95(9) . . ?
N1 Zn1 C1 104.72(8) 5_755 . ?
O2 Zn1 C1 29.35(8) . . ?
O2W Zn2 O3 117.18(6) . 4_855 ?
O2W Zn2 O3 117.18(6) . . ?
O3 Zn2 O3 125.63(12) 4_855 . ?
O2W Zn2 O1W 94.15(6) . . ?
O3 Zn2 O1W 90.66(8) 4_855 . ?
O3 Zn2 O1W 85.55(8) . . ?
O2W Zn2 O1W 94.15(6) . 4_855 ?
O3 Zn2 O1W 85.55(8) 4_855 4_855 ?
O3 Zn2 O1W 90.66(8) . 4_855 ?
O1W Zn2 O1W 171.70(12) . 4_855 ?
O2 C1 O1 119.9(3) . . ?
O2 C1 C2 121.6(3) . . ?
O1 C1 C2 118.4(3) . . ?
O2 C1 Zn1 63.97(15) . . ?
O1 C1 Zn1 57.01(14) . . ?
C2 C1 Zn1 165.14(19) . . ?
C3 C2 C7 119.5(3) . . ?
C3 C2 C1 117.3(3) . . ?
C7 C2 C1 123.0(2) . . ?
C4 C3 C2 121.4(3) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 119.0(3) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C6 C5 C4 120.4(3) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C7 121.3(3) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C6 C7 C2 118.3(3) . . ?
C6 C7 C8 120.0(3) . . ?
C2 C7 C8 121.5(2) . . ?
C13 C8 C9 117.9(3) . . ?
C13 C8 C7 121.9(3) . . ?
C9 C8 C7 120.2(3) . . ?
C10 C9 C8 121.2(3) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C9 C10 C11 121.3(3) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C12 C11 C10 117.6(3) . . ?
C12 C11 C14 122.8(3) . . ?
C10 C11 C14 119.6(3) . . ?
C13 C12 C11 121.1(3) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C12 C13 C8 121.0(3) . . ?
C12 C13 H13 119.5 . . ?
C8 C13 H13 119.5 . . ?
N1 C14 C11 115.3(2) . . ?
N1 C14 H14A 108.4 . . ?
C11 C14 H14A 108.4 . . ?
N1 C14 H14B 108.4 . . ?
C11 C14 H14B 108.4 . . ?
H14A C14 H14B 107.5 . . ?
N1 C15 C16 110.6(2) . . ?
N1 C15 H15A 109.5 . . ?
C16 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
O5 C16 O6 125.4(2) . . ?
O5 C16 C15 117.2(2) . . ?
O6 C16 C15 117.3(2) . . ?
N1 C17 C18 111.2(2) . . ?
N1 C17 H17A 109.4 . . ?
C18 C17 H17A 109.4 . . ?
N1 C17 H17B 109.4 . . ?
C18 C17 H17B 109.4 . . ?
H17A C17 H17B 108.0 . . ?
O3 C18 O4 125.2(2) . . ?
O3 C18 C17 116.2(2) . . ?
O4 C18 C17 118.6(2) . . ?
C15 N1 C17 111.7(2) . . ?
C15 N1 C14 111.5(2) . . ?
C17 N1 C14 112.5(2) . . ?
C15 N1 Zn1 103.08(14) . 5_755 ?
C17 N1 Zn1 104.06(15) . 5_755 ?
C14 N1 Zn1 113.39(16) . 5_755 ?
C1 O1 Zn1 93.04(17) . . ?
C1 O2 Zn1 86.67(18) . . ?
C18 O3 Zn2 123.13(17) . . ?
C18 O4 Zn1 116.74(16) . 5_755 ?
C16 O5 Zn1 115.55(16) . 5_755 ?
C16 O6 Zn1 134.15(17) . 7_755 ?
Zn2 O1W H1A 119(3) . . ?
Zn2 O1W H1B 109(3) . . ?
H1A O1W H1B 101(4) . . ?
Zn2 O2W H2A 126(3) . . ?

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
O4 Zn1 C1 O2 13.2(2) 5_755 . . . ?
O5 Zn1 C1 O2 -160.68(15) 5_755 . . . ?
O6 Zn1 C1 O2 108.03(17) 7_765 . . . ?
O1 Zn1 C1 O2 -167.9(3) . . . . ?
N1 Zn1 C1 O2 -73.61(17) 5_755 . . . ?
O4 Zn1 C1 O1 -178.84(14) 5_755 . . . ?
O5 Zn1 C1 O1 7.24(19) 5_755 . . . ?
O6 Zn1 C1 O1 -84.05(16) 7_765 . . . ?
N1 Zn1 C1 O1 94.31(16) 5_755 . . . ?
O2 Zn1 C1 O1 167.9(3) . . . . ?
O4 Zn1 C1 C2 -102.3(9) 5_755 . . . ?
O5 Zn1 C1 C2 83.8(9) 5_755 . . . ?
O6 Zn1 C1 C2 -7.5(9) 7_765 . . . ?
O1 Zn1 C1 C2 76.6(8) . . . . ?
N1 Zn1 C1 C2 170.9(8) 5_755 . . . ?
O2 Zn1 C1 C2 -115.5(9) . . . . ?
O2 C1 C2 C3 -117.4(3) . . . . ?
O1 C1 C2 C3 58.6(4) . . . . ?
Zn1 C1 C2 C3 -9.5(10) . . . . ?
O2 C1 C2 C7 58.5(4) . . . . ?
O1 C1 C2 C7 -125.6(3) . . . . ?
Zn1 C1 C2 C7 166.3(7) . . . . ?
C7 C2 C3 C4 -2.0(5) . . . . ?
C1 C2 C3 C4 174.0(3) . . . . ?
C2 C3 C4 C5 1.1(6) . . . . ?
C3 C4 C5 C6 0.4(6) . . . . ?
C4 C5 C6 C7 -0.8(6) . . . . ?
C5 C6 C7 C2 -0.1(5) . . . . ?
C5 C6 C7 C8 174.3(3) . . . . ?
C3 C2 C7 C6 1.5(4) . . . . ?
C1 C2 C7 C6 -174.3(3) . . . . ?
C3 C2 C7 C8 -172.9(3) . . . . ?
C1 C2 C7 C8 11.4(4) . . . . ?
C6 C7 C8 C13 52.4(4) . . . . ?
C2 C7 C8 C13 -133.3(3) . . . . ?
C6 C7 C8 C9 -124.7(3) . . . . ?
C2 C7 C8 C9 49.5(4) . . . . ?
C13 C8 C9 C10 -0.5(4) . . . . ?
C7 C8 C9 C10 176.7(3) . . . . ?
C8 C9 C10 C11 0.8(4) . . . . ?
C9 C10 C11 C12 -0.2(4) . . . . ?
C9 C10 C11 C14 -179.9(2) . . . . ?
C10 C11 C12 C13 -0.8(4) . . . . ?
C14 C11 C12 C13 179.0(3) . . . . ?
C11 C12 C13 C8 1.1(5) . . . . ?
C9 C8 C13 C12 -0.4(4) . . . . ?
C7 C8 C13 C12 -177.6(3) . . . . ?
C12 C11 C14 N1 -89.9(3) . . . . ?
C10 C11 C14 N1 89.8(3) . . . . ?
N1 C15 C16 O5 39.2(3) . . . . ?
N1 C15 C16 O6 -143.3(2) . . . . ?
N1 C17 C18 O3 -161.6(2) . . . . ?
N1 C17 C18 O4 19.7(3) . . . . ?
C16 C15 N1 C17 -148.7(2) . . . . ?
C16 C15 N1 C14 84.5(3) . . . . ?
C16 C15 N1 Zn1 -37.5(2) . . . 5_755 ?
C18 C17 N1 C15 78.5(3) . . . . ?
C18 C17 N1 C14 -155.2(2) . . . . ?
C18 C17 N1 Zn1 -32.1(2) . . . 5_755 ?
C11 C14 N1 C15 75.0(3) . . . . ?
C11 C14 N1 C17 -51.4(3) . . . . ?
C11 C14 N1 Zn1 -169.15(18) . . . 5_755 ?
O2 C1 O1 Zn1 12.5(3) . . . . ?
C2 C1 O1 Zn1 -163.5(2) . . . . ?
O4 Zn1 O1 C1 2.5(3) 5_755 . . . ?
O5 Zn1 O1 C1 -173.84(16) 5_755 . . . ?
O6 Zn1 O1 C1 94.00(17) 7_765 . . . ?
N1 Zn1 O1 C1 -93.79(17) 5_755 . . . ?
O2 Zn1 O1 C1 -6.88(15) . . . . ?
O1 C1 O2 Zn1 -11.7(3) . . . . ?
C2 C1 O2 Zn1 164.2(2) . . . . ?
O4 Zn1 O2 C1 -169.50(16) 5_755 . . . ?
O5 Zn1 O2 C1 32.5(2) 5_755 . . . ?
O6 Zn1 O2 C1 -73.05(17) 7_765 . . . ?
O1 Zn1 O2 C1 7.00(16) . . . . ?
N1 Zn1 O2 C1 111.33(17) 5_755 . . . ?
O4 C18 O3 Zn2 12.5(4) . . . . ?
C17 C18 O3 Zn2 -166.01(18) . . . . ?
O2W Zn2 O3 C18 -56.4(2) . . . . ?
O3 Zn2 O3 C18 123.6(2) 4_855 . . . ?
O1W Zn2 O3 C18 -148.8(2) . . . . ?
O1W Zn2 O3 C18 38.6(2) 4_855 . . . ?
O3 C18 O4 Zn1 -171.5(2) . . . 5_755 ?
C17 C18 O4 Zn1 7.0(3) . . . 5_755 ?
O6 C16 O5 Zn1 166.4(2) . . . 5_755 ?
C15 C16 O5 Zn1 -16.4(3) . . . 5_755 ?
O5 C16 O6 Zn1 5.7(4) . . . 7_755 ?
C15 C16 O6 Zn1 -171.57(17) . . . 7_755 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.062
#=========================END
data_Compound-3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H52 Co3 N6 O16'
_chemical_formula_sum            'C56 H52 Co3 N6 O16'
_chemical_formula_weight         1241.83

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_space_group_name_hall  '-P 2ybc '

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

_cell_length_a                   13.4440(5)
_cell_length_b                   8.4060(4)
_cell_length_c                   23.7830(7)
_cell_angle_alpha                90
_cell_angle_beta                 93.752(3)
_cell_angle_gamma                90
_cell_volume                     2681.96(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2188
_cell_measurement_theta_min      2.9637
_cell_measurement_theta_max      29.2124

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1278
_exptl_absorpt_coefficient_mu    0.995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7962
_exptl_absorpt_correction_T_max  0.8651
_exptl_absorpt_process_details   
;
CrysAlis (Oxford Diffraction, 2006)
;
_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  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9407
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.97
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4695
_reflns_number_gt                3676
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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.
For c17 and c17'atoms, some anisotropic 
displacement ellipsoids were rather elongated which led us to use 
the ISOR restraints.

For C15 and N1 atoms, SIMU restraint was used to make them behave similar 
anisotropic displacement parameters.
;

_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)+(0.0487P)²+0.8045P] 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         4695
_refine_ls_number_parameters     389
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0441
_refine_ls_wR_factor_ref         0.1098
_refine_ls_wR_factor_gt          0.0996
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.051
_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
Co2 Co 0.5000 0.0000 0.5000 0.02592(17) Uani 1 2 d S . .
Co1 Co 0.23810(3) 0.27154(5) 0.354463(18) 0.03090(15) Uani 1 1 d . . .
C1 C 0.1723(3) 1.1270(4) 0.59589(15) 0.0450(9) Uani 1 1 d . . .
H1 H 0.2184 1.1251 0.5684 0.054 Uiso 1 1 calc R . .
C2 C 0.1686(3) 1.2583(4) 0.63072(18) 0.0544(11) Uani 1 1 d . . .
H2 H 0.2129 1.3422 0.6272 0.065 Uiso 1 1 calc R . .
C3 C 0.0991(3) 1.2642(5) 0.67066(17) 0.0553(11) Uani 1 1 d . . .
H3 H 0.0941 1.3539 0.6932 0.066 Uiso 1 1 calc R . .
C4 C 0.0373(3) 1.1370(4) 0.67702(14) 0.0430(9) Uani 1 1 d . . .
H4 H -0.0093 1.1413 0.7042 0.052 Uiso 1 1 calc R . .
C5 C 0.0424(2) 1.0016(4) 0.64386(13) 0.0324(7) Uani 1 1 d . . .
C6 C 0.1089(2) 0.9975(4) 0.60087(13) 0.0314(7) Uani 1 1 d . . .
C7 C -0.0260(2) 0.8649(4) 0.65626(13) 0.0324(7) Uani 1 1 d . . .
C8 C 0.1118(2) 0.8635(4) 0.55947(13) 0.0327(7) Uani 1 1 d . . .
C9 C 0.1148(2) 0.7050(4) 0.57578(14) 0.0370(8) Uani 1 1 d . . .
H9 H 0.1163 0.6788 0.6138 0.044 Uiso 1 1 calc R . .
C10 C 0.1155(2) 0.5858(4) 0.53588(15) 0.0382(8) Uani 1 1 d . . .
H10 H 0.1161 0.4803 0.5476 0.046 Uiso 1 1 calc R . .
C11 C 0.1153(2) 0.6190(4) 0.47884(14) 0.0382(8) Uani 1 1 d . . .
C12 C 0.1115(3) 0.7760(5) 0.46294(15) 0.0462(10) Uani 1 1 d . . .
H12 H 0.1095 0.8016 0.4248 0.055 Uiso 1 1 calc R . .
C13 C 0.1104(3) 0.8974(4) 0.50252(14) 0.0417(9) Uani 1 1 d . . .
H13 H 0.1088 1.0028 0.4906 0.050 Uiso 1 1 calc R . .
C14 C 0.1220(2) 0.4866(4) 0.43588(16) 0.0440(9) Uani 1 1 d . A .
H14A H 0.0907 0.3921 0.4500 0.053 Uiso 1 1 calc R . .
H14B H 0.0847 0.5179 0.4014 0.053 Uiso 1 1 calc R . .
C15 C 0.2723(3) 0.5879(5) 0.39960(18) 0.0582(11) Uani 1 1 d U A .
H15A H 0.2941 0.6574 0.4305 0.070 Uiso 1 1 calc R . .
H15B H 0.2229 0.6451 0.3759 0.070 Uiso 1 1 calc R . .
C16 C 0.3604(2) 0.5502(4) 0.36555(15) 0.0378(8) Uani 1 1 d . A .
C17 C 0.2911(9) 0.3937(12) 0.4707(3) 0.042(3) Uani 0.76(3) 1 d PU A 1
C17' C 0.251(2) 0.343(3) 0.4762(7) 0.027(6) Uani 0.24(3) 1 d PU A 2
C18 C 0.3337(2) 0.2264(4) 0.46416(14) 0.0305(7) Uani 1 1 d . . .
C19 C 0.5747(2) 0.2868(4) 0.43594(14) 0.0364(8) Uani 1 1 d . . .
H19 H 0.5599 0.3365 0.4693 0.044 Uiso 1 1 calc R . .
C20 C 0.6042(2) 0.3800(4) 0.39278(14) 0.0372(8) Uani 1 1 d . . .
H20 H 0.6080 0.4899 0.3970 0.045 Uiso 1 1 calc R . .
C21 C 0.6283(2) 0.3094(4) 0.34256(14) 0.0347(8) Uani 1 1 d . . .
C22 C 0.6218(3) 0.1452(4) 0.33945(15) 0.0454(9) Uani 1 1 d . . .
H22 H 0.6383 0.0923 0.3070 0.055 Uiso 1 1 calc R . .
C23 C 0.5907(3) 0.0603(4) 0.38485(15) 0.0428(9) Uani 1 1 d . . .
H23 H 0.5868 -0.0499 0.3819 0.051 Uiso 1 1 calc R . .
C24 C 0.6575(2) 0.4090(4) 0.29480(14) 0.0355(8) Uani 1 1 d . . .
C25 C 0.6102(3) 0.5513(5) 0.28265(16) 0.0469(9) Uani 1 1 d . . .
H25 H 0.5575 0.5834 0.3035 0.056 Uiso 1 1 calc R . .
C26 C 0.6405(3) 0.6464(5) 0.23982(15) 0.0475(10) Uani 1 1 d . . .
H26 H 0.6073 0.7420 0.2326 0.057 Uiso 1 1 calc R . .
C27 C 0.7594(3) 0.4669(4) 0.21881(16) 0.0457(9) Uani 1 1 d . . .
H27 H 0.8100 0.4354 0.1964 0.055 Uiso 1 1 calc R . .
C28 C 0.7338(3) 0.3659(4) 0.26110(16) 0.0484(10) Uani 1 1 d . . .
H28 H 0.7672 0.2699 0.2671 0.058 Uiso 1 1 calc R . .
N1 N 0.22549(18) 0.4461(3) 0.42247(11) 0.0295(6) Uani 1 1 d U . .
N2 N 0.56612(19) 0.1284(3) 0.43282(11) 0.0334(6) Uani 1 1 d . . .
N3 N 0.7158(2) 0.6073(3) 0.20805(11) 0.0378(7) Uani 1 1 d . . .
O1 O 0.00509(19) 0.7680(4) 0.69321(12) 0.0611(8) Uani 1 1 d . . .
O2 O -0.11053(16) 0.8610(3) 0.63014(9) 0.0374(5) Uani 1 1 d . . .
O3 O 0.42714(18) 0.6529(3) 0.36302(11) 0.0546(7) Uani 1 1 d . . .
O4 O 0.35696(18) 0.4199(3) 0.33951(11) 0.0525(7) Uani 1 1 d . . .
O5 O 0.39135(16) 0.1815(3) 0.50410(9) 0.0367(5) Uani 1 1 d . A .
O6 O 0.31554(17) 0.1525(3) 0.41846(10) 0.0412(6) Uani 1 1 d . A .
O1W O 0.1459(2) 0.4183(3) 0.29864(11) 0.0514(7) Uani 1 1 d . . .
H1A H 0.168(3) 0.434(6) 0.268(2) 0.077 Uiso 1 1 d . . .
H1B H 0.084(3) 0.356(6) 0.2992(18) 0.077 Uiso 1 1 d . . .
O2W O 0.41196(19) -0.1199(3) 0.43970(10) 0.0375(6) Uani 1 1 d . . .
H2A H 0.425(3) -0.189(5) 0.4196(17) 0.056 Uiso 1 1 d . . .
H2B H 0.372(3) -0.040(5) 0.4259(17) 0.056 Uiso 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
Co2 O2W 2.062(2) . ?
Co2 O2W 2.062(2) 3_656 ?
Co2 O5 2.119(2) . ?
Co2 O5 2.119(2) 3_656 ?
Co2 N2 2.166(2) 3_656 ?
Co2 N2 2.166(2) . ?
Co1 O6 2.048(2) . ?
Co1 O4 2.076(2) . ?
Co1 O2 2.097(2) 3_566 ?
Co1 O1W 2.146(3) . ?
Co1 N3 2.150(3) 2_645 ?
Co1 N1 2.199(2) . ?
C1 C2 1.383(5) . ?
C1 C6 1.392(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.377(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.369(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.389(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.402(4) . ?
C5 C7 1.513(5) . ?
C6 C8 1.498(4) . ?
C7 O1 1.250(4) . ?
C7 O2 1.260(4) . ?
C8 C13 1.383(5) . ?
C8 C9 1.388(5) . ?
C9 C10 1.380(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.385(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.373(5) . ?
C11 C14 1.517(5) . ?
C12 C13 1.389(5) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 N1 1.487(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N1 1.469(5) . ?
C15 C16 1.512(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 O3 1.249(4) . ?
C16 O4 1.258(4) . ?
C17 N1 1.468(6) . ?
C17 C18 1.530(7) . ?
C17' C18 1.520(16) . ?
C17' N1 1.562(18) . ?
C18 O5 1.245(4) . ?
C18 O6 1.262(4) . ?
C19 N2 1.339(4) . ?
C19 C20 1.370(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.391(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.385(5) . ?
C21 C24 1.485(4) . ?
C22 C23 1.381(5) . ?
C22 H22 0.9300 . ?
C23 N2 1.337(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.376(5) . ?
C24 C28 1.391(5) . ?
C25 C26 1.377(5) . ?
C25 H25 0.9300 . ?
C26 N3 1.344(4) . ?
C26 H26 0.9300 . ?
C27 N3 1.335(4) . ?
C27 C28 1.377(5) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
N3 Co1 2.150(3) 2_655 ?
O2 Co1 2.097(2) 3_566 ?
O1W H1A 0.82(5) . ?
O1W H1B 0.98(5) . ?
O2W H2A 0.78(4) . ?
O2W H2B 0.91(4) . ?

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
O2W Co2 O2W 180.000(1) . 3_656 ?
O2W Co2 O5 91.03(10) . . ?
O2W Co2 O5 88.97(10) 3_656 . ?
O2W Co2 O5 88.97(10) . 3_656 ?
O2W Co2 O5 91.03(10) 3_656 3_656 ?
O5 Co2 O5 180.00(11) . 3_656 ?
O2W Co2 N2 91.43(10) . 3_656 ?
O2W Co2 N2 88.57(10) 3_656 3_656 ?
O5 Co2 N2 90.42(9) . 3_656 ?
O5 Co2 N2 89.58(9) 3_656 3_656 ?
O2W Co2 N2 88.57(10) . . ?
O2W Co2 N2 91.43(10) 3_656 . ?
O5 Co2 N2 89.58(9) . . ?
O5 Co2 N2 90.42(9) 3_656 . ?
N2 Co2 N2 180.000(1) 3_656 . ?
O6 Co1 O4 93.51(11) . . ?
O6 Co1 O2 89.57(9) . 3_566 ?
O4 Co1 O2 175.15(10) . 3_566 ?
O6 Co1 O1W 170.25(10) . . ?
O4 Co1 O1W 88.21(12) . . ?
O2 Co1 O1W 88.13(10) 3_566 . ?
O6 Co1 N3 92.57(10) . 2_645 ?
O4 Co1 N3 90.43(10) . 2_645 ?
O2 Co1 N3 93.18(10) 3_566 2_645 ?
O1W Co1 N3 97.02(11) . 2_645 ?
O6 Co1 N1 80.75(9) . . ?
O4 Co1 N1 79.77(9) . . ?
O2 Co1 N1 97.05(9) 3_566 . ?
O1W Co1 N1 90.13(10) . . ?
N3 Co1 N1 167.71(10) 2_645 . ?
C2 C1 C6 121.8(4) . . ?
C2 C1 H1 119.1 . . ?
C6 C1 H1 119.1 . . ?
C3 C2 C1 119.6(3) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C4 C3 C2 119.5(3) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 121.6(3) . . ?
C3 C4 H4 119.2 . . ?
C5 C4 H4 119.2 . . ?
C4 C5 C6 119.5(3) . . ?
C4 C5 C7 117.3(3) . . ?
C6 C5 C7 123.2(3) . . ?
C1 C6 C5 117.8(3) . . ?
C1 C6 C8 119.3(3) . . ?
C5 C6 C8 122.9(3) . . ?
O1 C7 O2 125.4(3) . . ?
O1 C7 C5 116.9(3) . . ?
O2 C7 C5 117.6(3) . . ?
C13 C8 C9 118.0(3) . . ?
C13 C8 C6 119.3(3) . . ?
C9 C8 C6 122.7(3) . . ?
C10 C9 C8 120.4(3) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C11 121.9(3) . . ?
C9 C10 H10 119.1 . . ?
C11 C10 H10 119.1 . . ?
C12 C11 C10 117.5(3) . . ?
C12 C11 C14 121.5(3) . . ?
C10 C11 C14 121.0(3) . . ?
C11 C12 C13 121.4(3) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
C8 C13 C12 120.8(3) . . ?
C8 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
N1 C14 C11 114.2(3) . . ?
N1 C14 H14A 108.7 . . ?
C11 C14 H14A 108.7 . . ?
N1 C14 H14B 108.7 . . ?
C11 C14 H14B 108.7 . . ?
H14A C14 H14B 107.6 . . ?
N1 C15 C16 113.4(3) . . ?
N1 C15 H15A 108.9 . . ?
C16 C15 H15A 108.9 . . ?
N1 C15 H15B 108.9 . . ?
C16 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
O3 C16 O4 125.6(3) . . ?
O3 C16 C15 118.1(3) . . ?
O4 C16 C15 116.2(3) . . ?
N1 C17 C18 113.9(4) . . ?
C18 C17' N1 109.3(12) . . ?
O5 C18 O6 125.7(3) . . ?
O5 C18 C17' 118.5(7) . . ?
O6 C18 C17' 112.2(9) . . ?
O5 C18 C17 114.8(3) . . ?
O6 C18 C17 119.2(3) . . ?
C17' C18 C17 26.5(8) . . ?
N2 C19 C20 123.7(3) . . ?
N2 C19 H19 118.1 . . ?
C20 C19 H19 118.1 . . ?
C19 C20 C21 119.6(3) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C22 C21 C20 117.0(3) . . ?
C22 C21 C24 122.7(3) . . ?
C20 C21 C24 120.3(3) . . ?
C23 C22 C21 119.6(3) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
N2 C23 C22 123.4(3) . . ?
N2 C23 H23 118.3 . . ?
C22 C23 H23 118.3 . . ?
C25 C24 C28 117.0(3) . . ?
C25 C24 C21 120.6(3) . . ?
C28 C24 C21 122.4(3) . . ?
C24 C25 C26 120.3(3) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
N3 C26 C25 123.0(3) . . ?
N3 C26 H26 118.5 . . ?
C25 C26 H26 118.5 . . ?
N3 C27 C28 123.9(3) . . ?
N3 C27 H27 118.1 . . ?
C28 C27 H27 118.1 . . ?
C27 C28 C24 119.3(3) . . ?
C27 C28 H28 120.3 . . ?
C24 C28 H28 120.3 . . ?
C17 N1 C15 106.4(6) . . ?
C17 N1 C14 115.1(5) . . ?
C15 N1 C14 108.8(3) . . ?
C17 N1 C17' 26.5(7) . . ?
C15 N1 C17' 132.3(13) . . ?
C14 N1 C17' 96.5(9) . . ?
C17 N1 Co1 107.7(2) . . ?
C15 N1 Co1 102.34(19) . . ?
C14 N1 Co1 115.40(19) . . ?
C17' N1 Co1 102.0(7) . . ?
C23 N2 C19 116.6(3) . . ?
C23 N2 Co2 123.5(2) . . ?
C19 N2 Co2 119.5(2) . . ?
C27 N3 C26 116.5(3) . . ?
C27 N3 Co1 123.9(2) . 2_655 ?
C26 N3 Co1 119.6(2) . 2_655 ?
C7 O2 Co1 130.5(2) . 3_566 ?
C16 O4 Co1 116.3(2) . . ?
C18 O5 Co2 125.5(2) . . ?
C18 O6 Co1 117.4(2) . . ?
Co1 O1W H1A 115(3) . . ?
Co1 O1W H1B 98(3) . . ?
H1A O1W H1B 117(4) . . ?
Co2 O2W H2A 131(3) . . ?
Co2 O2W H2B 101(2) . . ?
H2A O2W H2B 118(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
C6 C1 C2 C3 -1.6(6) . . . . ?
C1 C2 C3 C4 2.8(6) . . . . ?
C2 C3 C4 C5 -0.4(6) . . . . ?
C3 C4 C5 C6 -3.3(5) . . . . ?
C3 C4 C5 C7 177.1(3) . . . . ?
C2 C1 C6 C5 -2.0(5) . . . . ?
C2 C1 C6 C8 176.0(3) . . . . ?
C4 C5 C6 C1 4.3(5) . . . . ?
C7 C5 C6 C1 -176.1(3) . . . . ?
C4 C5 C6 C8 -173.5(3) . . . . ?
C7 C5 C6 C8 6.0(5) . . . . ?
C4 C5 C7 O1 -86.7(4) . . . . ?
C6 C5 C7 O1 93.7(4) . . . . ?
C4 C5 C7 O2 90.9(4) . . . . ?
C6 C5 C7 O2 -88.7(4) . . . . ?
C1 C6 C8 C13 -47.3(4) . . . . ?
C5 C6 C8 C13 130.5(3) . . . . ?
C1 C6 C8 C9 133.3(3) . . . . ?
C5 C6 C8 C9 -48.9(4) . . . . ?
C13 C8 C9 C10 -0.6(5) . . . . ?
C6 C8 C9 C10 178.8(3) . . . . ?
C8 C9 C10 C11 1.3(5) . . . . ?
C9 C10 C11 C12 -1.8(5) . . . . ?
C9 C10 C11 C14 176.5(3) . . . . ?
C10 C11 C12 C13 1.7(5) . . . . ?
C14 C11 C12 C13 -176.7(3) . . . . ?
C9 C8 C13 C12 0.4(5) . . . . ?
C6 C8 C13 C12 -179.0(3) . . . . ?
C11 C12 C13 C8 -1.0(5) . . . . ?
C12 C11 C14 N1 87.5(4) . . . . ?
C10 C11 C14 N1 -90.8(4) . . . . ?
N1 C15 C16 O3 -152.5(3) . . . . ?
N1 C15 C16 O4 31.3(5) . . . . ?
N1 C17' C18 O5 151.4(11) . . . . ?
N1 C17' C18 O6 -49(2) . . . . ?
N1 C17' C18 C17 62.5(17) . . . . ?
N1 C17 C18 O5 178.4(7) . . . . ?
N1 C17 C18 O6 4.3(13) . . . . ?
N1 C17 C18 C17' -77.0(16) . . . . ?
N2 C19 C20 C21 -0.9(5) . . . . ?
C19 C20 C21 C22 -0.7(5) . . . . ?
C19 C20 C21 C24 178.2(3) . . . . ?
C20 C21 C22 C23 1.1(5) . . . . ?
C24 C21 C22 C23 -177.7(3) . . . . ?
C21 C22 C23 N2 -0.2(6) . . . . ?
C22 C21 C24 C25 139.9(4) . . . . ?
C20 C21 C24 C25 -39.0(5) . . . . ?
C22 C21 C24 C28 -41.3(5) . . . . ?
C20 C21 C24 C28 139.9(4) . . . . ?
C28 C24 C25 C26 -1.7(6) . . . . ?
C21 C24 C25 C26 177.2(3) . . . . ?
C24 C25 C26 N3 0.1(6) . . . . ?
N3 C27 C28 C24 0.8(6) . . . . ?
C25 C24 C28 C27 1.3(6) . . . . ?
C21 C24 C28 C27 -177.6(3) . . . . ?
C18 C17 N1 C15 -118.7(9) . . . . ?
C18 C17 N1 C14 120.7(7) . . . . ?
C18 C17 N1 C17' 71.9(16) . . . . ?
C18 C17 N1 Co1 -9.6(11) . . . . ?
C16 C15 N1 C17 76.3(4) . . . . ?
C16 C15 N1 C14 -159.1(3) . . . . ?
C16 C15 N1 C17' 82.6(9) . . . . ?
C16 C15 N1 Co1 -36.6(4) . . . . ?
C11 C14 N1 C17 59.4(6) . . . . ?
C11 C14 N1 C15 -59.9(4) . . . . ?
C11 C14 N1 C17' 79.1(11) . . . . ?
C11 C14 N1 Co1 -174.3(2) . . . . ?
C18 C17' N1 C17 -67.8(18) . . . . ?
C18 C17' N1 C15 -81.6(18) . . . . ?
C18 C17' N1 C14 155.5(17) . . . . ?
C18 C17' N1 Co1 38(2) . . . . ?
O6 Co1 N1 C17 9.1(7) . . . . ?
O4 Co1 N1 C17 -86.2(7) . . . . ?
O2 Co1 N1 C17 97.5(7) 3_566 . . . ?
O1W Co1 N1 C17 -174.4(7) . . . . ?
N3 Co1 N1 C17 -48.6(8) 2_645 . . . ?
O6 Co1 N1 C15 121.0(2) . . . . ?
O4 Co1 N1 C15 25.7(2) . . . . ?
O2 Co1 N1 C15 -150.6(2) 3_566 . . . ?
O1W Co1 N1 C15 -62.4(2) . . . . ?
N3 Co1 N1 C15 63.3(6) 2_645 . . . ?
O6 Co1 N1 C14 -121.0(2) . . . . ?
O4 Co1 N1 C14 143.7(2) . . . . ?
O2 Co1 N1 C14 -32.6(2) 3_566 . . . ?
O1W Co1 N1 C14 55.6(2) . . . . ?
N3 Co1 N1 C14 -178.7(4) 2_645 . . . ?
O6 Co1 N1 C17' -17.7(12) . . . . ?
O4 Co1 N1 C17' -113.0(12) . . . . ?
O2 Co1 N1 C17' 70.7(12) 3_566 . . . ?
O1W Co1 N1 C17' 158.8(12) . . . . ?
N3 Co1 N1 C17' -75.4(13) 2_645 . . . ?
C22 C23 N2 C19 -1.3(5) . . . . ?
C22 C23 N2 Co2 172.1(3) . . . . ?
C20 C19 N2 C23 1.9(5) . . . . ?
C20 C19 N2 Co2 -171.8(3) . . . . ?
O2W Co2 N2 C23 -41.3(3) . . . . ?
O2W Co2 N2 C23 138.7(3) 3_656 . . . ?
O5 Co2 N2 C23 -132.4(3) . . . . ?
O5 Co2 N2 C23 47.6(3) 3_656 . . . ?
N2 Co2 N2 C23 -79(100) 3_656 . . . ?
O2W Co2 N2 C19 131.9(2) . . . . ?
O2W Co2 N2 C19 -48.1(2) 3_656 . . . ?
O5 Co2 N2 C19 40.9(2) . . . . ?
O5 Co2 N2 C19 -139.1(2) 3_656 . . . ?
N2 Co2 N2 C19 95(100) 3_656 . . . ?
C28 C27 N3 C26 -2.4(6) . . . . ?
C28 C27 N3 Co1 175.9(3) . . . 2_655 ?
C25 C26 N3 C27 2.0(6) . . . . ?
C25 C26 N3 Co1 -176.5(3) . . . 2_655 ?
O1 C7 O2 Co1 12.3(5) . . . 3_566 ?
C5 C7 O2 Co1 -165.0(2) . . . 3_566 ?
O3 C16 O4 Co1 178.3(3) . . . . ?
C15 C16 O4 Co1 -5.8(5) . . . . ?
O6 Co1 O4 C16 -92.1(3) . . . . ?
O2 Co1 O4 C16 37.3(13) 3_566 . . . ?
O1W Co1 O4 C16 78.3(3) . . . . ?
N3 Co1 O4 C16 175.3(3) 2_645 . . . ?
N1 Co1 O4 C16 -12.1(3) . . . . ?
O6 C18 O5 Co2 15.4(5) . . . . ?
C17' C18 O5 Co2 172.3(15) . . . . ?
C17 C18 O5 Co2 -158.2(6) . . . . ?
O2W Co2 O5 C18 -31.7(3) . . . . ?
O2W Co2 O5 C18 148.3(3) 3_656 . . . ?
O5 Co2 O5 C18 120(100) 3_656 . . . ?
N2 Co2 O5 C18 -123.1(3) 3_656 . . . ?
N2 Co2 O5 C18 56.9(3) . . . . ?
O5 C18 O6 Co1 -169.0(2) . . . . ?
C17' C18 O6 Co1 32.9(13) . . . . ?
C17 C18 O6 Co1 4.4(7) . . . . ?
O4 Co1 O6 C18 71.3(2) . . . . ?
O2 Co1 O6 C18 -104.9(2) 3_566 . . . ?
O1W Co1 O6 C18 -28.6(7) . . . . ?
N3 Co1 O6 C18 161.9(2) 2_645 . . . ?
N1 Co1 O6 C18 -7.7(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.074
#=========================END
data_Compound-4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C78 H84 N14 Ni3 O18'
_chemical_formula_sum            'C78 H84 N14 Ni3 O18'
_chemical_formula_weight         1681.72

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_hall  '-P 1'

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

_cell_length_a                   9.6530(4)
_cell_length_b                   13.8230(5)
_cell_length_c                   15.2330(8)
_cell_angle_alpha                81.369(4)
_cell_angle_beta                 78.690(4)
_cell_angle_gamma                75.595(4)
_cell_volume                     1919.45(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3350
_cell_measurement_theta_min      2.7374
_cell_measurement_theta_max      29.1374

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             878
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8296
_exptl_absorpt_correction_T_max  0.8883
_exptl_absorpt_process_details   
;
CrysAlis (Oxford Diffraction, 2006)
;
_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  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11847
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0616
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.74
_diffrn_reflns_theta_max         25.02
_reflns_number_total             6781
_reflns_number_gt                4737
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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.

For  o2w, o2w', o3w and o3w' atoms, some anisotropic 
displacement ellipsoids were rather elongated which led us to use 
the ISOR restraints.
;

_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)+(0.0747P)²+1.3600P] 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         6781
_refine_ls_number_parameters     535
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0544
_refine_ls_wR_factor_ref         0.1519
_refine_ls_wR_factor_gt          0.1319
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.012
_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 0.60755(5) -0.24723(4) -0.32183(3) 0.03954(18) Uani 1 1 d . . .
Ni2 Ni 0.5000 -0.5000 0.0000 0.02820(19) Uani 1 2 d S . .
C1 C 1.4565(5) -0.7496(4) -0.4963(3) 0.0548(13) Uani 1 1 d . . .
C2 C 1.5382(5) -0.7107(4) -0.4392(3) 0.0557(13) Uani 1 1 d . . .
C3 C 1.6815(6) -0.7632(5) -0.4379(4) 0.081(2) Uani 1 1 d . . .
H3 H 1.7203 -0.8175 -0.4714 0.097 Uiso 1 1 calc R . .
C4 C 1.7664(6) -0.7351(6) -0.3873(4) 0.087(2) Uani 1 1 d . . .
H4 H 1.8628 -0.7689 -0.3886 0.104 Uiso 1 1 calc R . .
C5 C 1.7096(6) -0.6588(6) -0.3362(4) 0.0813(19) Uani 1 1 d . . .
H5 H 1.7653 -0.6423 -0.2998 0.098 Uiso 1 1 calc R . .
C6 C 1.5675(5) -0.6044(5) -0.3377(3) 0.0656(15) Uani 1 1 d . . .
H6 H 1.5299 -0.5509 -0.3031 0.079 Uiso 1 1 calc R . .
C7 C 1.4802(5) -0.6289(4) -0.3907(3) 0.0513(12) Uani 1 1 d . . .
C8 C 1.3313(4) -0.5664(4) -0.3917(3) 0.0447(11) Uani 1 1 d . . .
C9 C 1.3087(5) -0.4626(4) -0.3974(3) 0.0549(13) Uani 1 1 d . . .
H9 H 1.3866 -0.4336 -0.3994 0.066 Uiso 1 1 calc R . .
C10 C 1.1701(5) -0.4010(4) -0.4002(3) 0.0525(12) Uani 1 1 d . . .
H10 H 1.1574 -0.3316 -0.4049 0.063 Uiso 1 1 calc R . .
C11 C 1.0514(4) -0.4423(4) -0.3961(3) 0.0432(11) Uani 1 1 d . . .
C12 C 1.0742(4) -0.5451(4) -0.3900(3) 0.0449(11) Uani 1 1 d . . .
H12 H 0.9963 -0.5742 -0.3878 0.054 Uiso 1 1 calc R . .
C13 C 1.2120(5) -0.6064(4) -0.3869(3) 0.0484(11) Uani 1 1 d . . .
H13 H 1.2240 -0.6758 -0.3816 0.058 Uiso 1 1 calc R . .
C14 C 0.9022(4) -0.3741(4) -0.3999(3) 0.0495(12) Uani 1 1 d . . .
H14A H 0.9139 -0.3132 -0.4386 0.059 Uiso 1 1 calc R . .
H14B H 0.8474 -0.4074 -0.4279 0.059 Uiso 1 1 calc R . .
C15 C 0.8870(5) -0.2885(4) -0.2682(4) 0.0619(14) Uani 1 1 d . . .
H15A H 0.9380 -0.2472 -0.3141 0.074 Uiso 1 1 calc R . .
H15B H 0.9584 -0.3352 -0.2365 0.074 Uiso 1 1 calc R . .
C16 C 0.7835(6) -0.2220(4) -0.2027(3) 0.0588(13) Uani 1 1 d . . .
C17 C 0.7860(5) -0.4340(4) -0.2520(3) 0.0611(14) Uani 1 1 d . . .
H17A H 0.8530 -0.4515 -0.2092 0.073 Uiso 1 1 calc R . .
H17B H 0.8053 -0.4899 -0.2876 0.073 Uiso 1 1 calc R . .
C18 C 0.6320(4) -0.4211(3) -0.1999(3) 0.0348(9) Uani 1 1 d . . .
C19 C 0.3615(5) -0.0583(4) -0.3320(3) 0.0528(12) Uani 1 1 d . . .
H19 H 0.4263 -0.0174 -0.3551 0.063 Uiso 1 1 calc R . .
C20 C 0.2736(5) -0.1871(4) -0.2821(3) 0.0551(12) Uani 1 1 d . . .
H20 H 0.2662 -0.2532 -0.2640 0.066 Uiso 1 1 calc R . .
C21 C 0.1608(5) -0.1066(4) -0.2826(3) 0.0572(13) Uani 1 1 d . . .
H21 H 0.0631 -0.1068 -0.2644 0.069 Uiso 1 1 calc R . .
C22 C 0.1370(6) 0.0801(4) -0.3296(3) 0.0587(13) Uani 1 1 d . . .
H21A H 0.0416 0.0799 -0.3409 0.070 Uiso 1 1 calc R . .
H22B H 0.1866 0.1122 -0.3834 0.070 Uiso 1 1 calc R . .
C23 C 0.1185(5) 0.1428(3) -0.2533(3) 0.0471(11) Uani 1 1 d . . .
C24 C 0.2362(5) 0.1653(4) -0.2280(3) 0.0543(12) Uani 1 1 d . . .
H24 H 0.3297 0.1365 -0.2548 0.065 Uiso 1 1 calc R . .
C25 C 0.2160(5) 0.2301(4) -0.1632(3) 0.0526(12) Uani 1 1 d . . .
H25 H 0.2964 0.2438 -0.1467 0.063 Uiso 1 1 calc R . .
C26 C 0.0785(4) 0.2747(3) -0.1226(3) 0.0408(10) Uani 1 1 d . . .
C27 C -0.0383(5) 0.2508(4) -0.1467(3) 0.0491(11) Uani 1 1 d . . .
H27 H -0.1318 0.2796 -0.1201 0.059 Uiso 1 1 calc R . .
C28 C -0.0180(5) 0.1845(4) -0.2099(3) 0.0504(12) Uani 1 1 d . . .
H28 H -0.0982 0.1675 -0.2234 0.061 Uiso 1 1 calc R . .
C29 C 0.0521(5) 0.3447(4) -0.0513(3) 0.0499(12) Uani 1 1 d . . .
H29A H -0.0470 0.3840 -0.0466 0.060 Uiso 1 1 calc R . .
H29B H 0.0628 0.3052 0.0062 0.060 Uiso 1 1 calc R . .
C30 C 0.1754(5) 0.4767(4) -0.1461(3) 0.0466(11) Uani 1 1 d . . .
H30 H 0.1308 0.4863 -0.1965 0.056 Uiso 1 1 calc R . .
C31 C 0.2382(4) 0.4239(3) -0.0151(3) 0.0373(10) Uani 1 1 d . . .
H31 H 0.2426 0.3889 0.0418 0.045 Uiso 1 1 calc R . .
C32 C 0.2782(4) 0.5229(3) -0.1338(3) 0.0415(10) Uani 1 1 d . . .
H32 H 0.3163 0.5702 -0.1752 0.050 Uiso 1 1 calc R . .
C33 C 0.5678(4) -0.7008(3) -0.0829(3) 0.0398(10) Uani 1 1 d . . .
H33 H 0.5398 -0.6674 -0.1365 0.048 Uiso 1 1 calc R . .
C34 C 0.6091(5) -0.8008(4) -0.0654(3) 0.0489(11) Uani 1 1 d . . .
H34 H 0.6155 -0.8485 -0.1039 0.059 Uiso 1 1 calc R . .
C35 C 0.6161(4) -0.7291(3) 0.0502(3) 0.0411(10) Uani 1 1 d . . .
H35 H 0.6287 -0.7203 0.1072 0.049 Uiso 1 1 calc R . .
C36 C 0.6964(6) -0.9182(4) 0.0675(3) 0.0603(13) Uani 1 1 d . . .
H36A H 0.6398 -0.9646 0.0604 0.072 Uiso 1 1 calc R . .
H36B H 0.6844 -0.9118 0.1312 0.072 Uiso 1 1 calc R . .
C37 C 0.8544(5) -0.9607(3) 0.0330(3) 0.0512(12) Uani 1 1 d . . .
C38 C 0.9606(6) -0.9171(4) 0.0461(3) 0.0604(13) Uani 1 1 d . . .
H38 H 0.9349 -0.8607 0.0773 0.072 Uiso 1 1 calc R . .
C39 C 0.8939(6) -1.0443(4) -0.0137(3) 0.0578(13) Uani 1 1 d . . .
H39 H 0.8233 -1.0748 -0.0234 0.069 Uiso 1 1 calc R . .
N1 N 0.8155(3) -0.3455(3) -0.3119(2) 0.0392(8) Uani 1 1 d . . .
N2 N 0.4008(4) -0.1564(3) -0.3124(2) 0.0470(9) Uani 1 1 d . . .
N3 N 0.2178(4) -0.0248(3) -0.3149(2) 0.0477(9) Uani 1 1 d . . .
N4 N 0.1504(3) 0.4131(3) -0.0693(2) 0.0408(8) Uani 1 1 d . . .
N5 N 0.3169(3) 0.4885(3) -0.0505(2) 0.0343(8) Uani 1 1 d . . .
N6 N 0.5730(3) -0.6553(2) -0.0102(2) 0.0320(7) Uani 1 1 d . . .
N7 N 0.6399(4) -0.8186(3) 0.0198(2) 0.0438(9) Uani 1 1 d . . .
O1 O 1.4304(5) -0.8346(3) -0.4691(2) 0.0804(12) Uani 1 1 d . . .
O2 O 1.4262(3) -0.6963(2) -0.56745(19) 0.0487(8) Uani 1 1 d . . .
O3 O 0.6188(3) -0.4806(2) -0.13060(17) 0.0386(7) Uani 1 1 d . . .
O4 O 0.5340(3) -0.3572(2) -0.23269(18) 0.0415(7) Uani 1 1 d . . .
O5 O 0.6527(3) -0.1932(3) -0.2147(2) 0.0555(8) Uani 1 1 d . . .
O6 O 0.8349(5) -0.1948(4) -0.1438(3) 0.1017(16) Uani 1 1 d . . .
O1W O 0.7083(5) -0.1420(3) -0.4086(3) 0.0743(12) Uani 1 1 d D . .
H1A H 0.650(8) -0.085(6) -0.408(5) 0.111 Uiso 1 1 d . . .
H1B H 0.666(7) -0.148(6) -0.455(3) 0.111 Uiso 1 1 d D . .
O2W O 0.6488(13) 0.0392(10) -0.3505(8) 0.185(4) Uani 0.70 1 d PU . .
O2W' O 0.738(3) 0.021(2) -0.307(2) 0.199(11) Uani 0.30 1 d PU . .
O3W O 0.6425(19) -0.9924(14) -0.1927(13) 0.177(7) Uani 0.50 1 d PU . .
O3W' O 0.6180(13) -1.0168(10) -0.1413(9) 0.126(4) Uani 0.50 1 d PU . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O4 2.049(3) . ?
Ni1 O5 2.053(3) . ?
Ni1 N2 2.068(4) . ?
Ni1 O2 2.073(3) 2_744 ?
Ni1 O1W 2.105(4) . ?
Ni1 N1 2.144(3) . ?
Ni2 N6 2.105(3) 2_645 ?
Ni2 N6 2.105(3) . ?
Ni2 O3 2.108(3) . ?
Ni2 O3 2.108(3) 2_645 ?
Ni2 N5 2.110(3) 2_655 ?
Ni2 N5 2.110(3) 1_545 ?
C1 O1 1.254(6) . ?
C1 O2 1.258(5) . ?
C1 C2 1.512(7) . ?
C2 C7 1.383(7) . ?
C2 C3 1.395(7) . ?
C3 C4 1.383(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.346(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.393(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.402(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.483(6) . ?
C8 C13 1.382(6) . ?
C8 C9 1.389(7) . ?
C9 C10 1.400(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.389(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.374(6) . ?
C11 C14 1.519(6) . ?
C12 C13 1.393(6) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 N1 1.486(5) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N1 1.466(6) . ?
C15 C16 1.505(7) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 O6 1.250(6) . ?
C16 O5 1.267(6) . ?
C17 N1 1.466(6) . ?
C17 C18 1.524(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 O3 1.243(5) . ?
C18 O4 1.250(5) . ?
C19 N2 1.318(6) . ?
C19 N3 1.335(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.350(7) . ?
C20 N2 1.371(6) . ?
C20 H20 0.9300 . ?
C21 N3 1.364(6) . ?
C21 H21 0.9300 . ?
C22 N3 1.473(6) . ?
C22 C23 1.508(6) . ?
C22 H21A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C28 1.378(6) . ?
C23 C24 1.386(6) . ?
C24 C25 1.385(7) . ?
C24 H24 0.9300 . ?
C25 C26 1.382(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.378(6) . ?
C26 C29 1.505(6) . ?
C27 C28 1.380(6) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 N4 1.461(5) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C32 1.361(6) . ?
C30 N4 1.372(5) . ?
C30 H30 0.9300 . ?
C31 N5 1.303(5) . ?
C31 N4 1.341(5) . ?
C31 H31 0.9300 . ?
C32 N5 1.376(5) . ?
C32 H32 0.9300 . ?
C33 C34 1.340(6) . ?
C33 N6 1.368(5) . ?
C33 H33 0.9300 . ?
C34 N7 1.361(5) . ?
C34 H34 0.9300 . ?
C35 N6 1.311(5) . ?
C35 N7 1.337(5) . ?
C35 H35 0.9300 . ?
C36 N7 1.483(6) . ?
C36 C37 1.510(7) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 C38 1.371(7) . ?
C37 C39 1.381(7) . ?
C38 C39 1.391(7) 2_735 ?
C38 H38 0.9300 . ?
C39 C38 1.391(7) 2_735 ?
C39 H39 0.9300 . ?
N5 Ni2 2.110(3) 1_565 ?
O2 Ni1 2.073(3) 2_744 ?
O1W H1A 0.84(7) . ?
O1W H1B 0.906(10) . ?
O2W O2W' 1.14(3) . ?
O2W' O3W 1.81(3) 1_565 ?
O3W O3W' 0.819(19) . ?
O3W O2W' 1.81(3) 1_545 ?

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
O4 Ni1 O5 88.04(12) . . ?
O4 Ni1 N2 91.24(13) . . ?
O5 Ni1 N2 93.18(14) . . ?
O4 Ni1 O2 93.21(12) . 2_744 ?
O5 Ni1 O2 176.93(12) . 2_744 ?
N2 Ni1 O2 89.60(13) . 2_744 ?
O4 Ni1 O1W 172.93(13) . . ?
O5 Ni1 O1W 88.72(16) . . ?
N2 Ni1 O1W 95.22(16) . . ?
O2 Ni1 O1W 89.72(16) 2_744 . ?
O4 Ni1 N1 83.12(12) . . ?
O5 Ni1 N1 81.21(13) . . ?
N2 Ni1 N1 172.15(13) . . ?
O2 Ni1 N1 96.16(12) 2_744 . ?
O1W Ni1 N1 90.17(15) . . ?
N6 Ni2 N6 180.0 2_645 . ?
N6 Ni2 O3 93.90(11) 2_645 . ?
N6 Ni2 O3 86.10(11) . . ?
N6 Ni2 O3 86.10(11) 2_645 2_645 ?
N6 Ni2 O3 93.90(11) . 2_645 ?
O3 Ni2 O3 180.00(16) . 2_645 ?
N6 Ni2 N5 85.73(12) 2_645 2_655 ?
N6 Ni2 N5 94.27(12) . 2_655 ?
O3 Ni2 N5 87.80(11) . 2_655 ?
O3 Ni2 N5 92.20(11) 2_645 2_655 ?
N6 Ni2 N5 94.27(12) 2_645 1_545 ?
N6 Ni2 N5 85.73(12) . 1_545 ?
O3 Ni2 N5 92.20(11) . 1_545 ?
O3 Ni2 N5 87.80(11) 2_645 1_545 ?
N5 Ni2 N5 180.00(15) 2_655 1_545 ?
O1 C1 O2 126.3(5) . . ?
O1 C1 C2 116.0(4) . . ?
O2 C1 C2 117.6(5) . . ?
C7 C2 C3 120.2(5) . . ?
C7 C2 C1 124.4(4) . . ?
C3 C2 C1 115.4(5) . . ?
C4 C3 C2 120.6(6) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C5 C4 C3 120.1(5) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.1(6) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C7 121.1(6) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C2 C7 C6 117.8(4) . . ?
C2 C7 C8 123.5(4) . . ?
C6 C7 C8 118.6(5) . . ?
C13 C8 C9 117.7(4) . . ?
C13 C8 C7 123.1(5) . . ?
C9 C8 C7 119.2(4) . . ?
C8 C9 C10 120.9(4) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
C11 C10 C9 120.8(5) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C12 C11 C10 118.1(4) . . ?
C12 C11 C14 121.9(4) . . ?
C10 C11 C14 120.0(4) . . ?
C11 C12 C13 121.1(4) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
C8 C13 C12 121.4(5) . . ?
C8 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
N1 C14 C11 115.7(3) . . ?
N1 C14 H14A 108.4 . . ?
C11 C14 H14A 108.4 . . ?
N1 C14 H14B 108.4 . . ?
C11 C14 H14B 108.4 . . ?
H14A C14 H14B 107.4 . . ?
N1 C15 C16 113.4(4) . . ?
N1 C15 H15A 108.9 . . ?
C16 C15 H15A 108.9 . . ?
N1 C15 H15B 108.9 . . ?
C16 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
O6 C16 O5 124.9(5) . . ?
O6 C16 C15 117.5(5) . . ?
O5 C16 C15 117.5(4) . . ?
N1 C17 C18 114.8(4) . . ?
N1 C17 H17A 108.6 . . ?
C18 C17 H17A 108.6 . . ?
N1 C17 H17B 108.6 . . ?
C18 C17 H17B 108.6 . . ?
H17A C17 H17B 107.5 . . ?
O3 C18 O4 127.7(4) . . ?
O3 C18 C17 114.3(4) . . ?
O4 C18 C17 117.8(4) . . ?
N2 C19 N3 112.0(4) . . ?
N2 C19 H19 124.0 . . ?
N3 C19 H19 124.0 . . ?
C21 C20 N2 109.4(5) . . ?
C21 C20 H20 125.3 . . ?
N2 C20 H20 125.3 . . ?
C20 C21 N3 106.7(4) . . ?
C20 C21 H21 126.6 . . ?
N3 C21 H21 126.6 . . ?
N3 C22 C23 115.5(4) . . ?
N3 C22 H21A 108.4 . . ?
C23 C22 H21A 108.4 . . ?
N3 C22 H22B 108.4 . . ?
C23 C22 H22B 108.4 . . ?
H21A C22 H22B 107.5 . . ?
C28 C23 C24 117.7(4) . . ?
C28 C23 C22 120.6(4) . . ?
C24 C23 C22 121.6(4) . . ?
C25 C24 C23 120.7(4) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C26 C25 C24 121.1(4) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C27 C26 C25 118.1(4) . . ?
C27 C26 C29 119.2(4) . . ?
C25 C26 C29 122.7(4) . . ?
C26 C27 C28 120.8(4) . . ?
C26 C27 H27 119.6 . . ?
C28 C27 H27 119.6 . . ?
C23 C28 C27 121.5(4) . . ?
C23 C28 H28 119.2 . . ?
C27 C28 H28 119.2 . . ?
N4 C29 C26 113.4(3) . . ?
N4 C29 H29A 108.9 . . ?
C26 C29 H29A 108.9 . . ?
N4 C29 H29B 108.9 . . ?
C26 C29 H29B 108.9 . . ?
H29A C29 H29B 107.7 . . ?
C32 C30 N4 106.6(4) . . ?
C32 C30 H30 126.7 . . ?
N4 C30 H30 126.7 . . ?
N5 C31 N4 112.9(4) . . ?
N5 C31 H31 123.5 . . ?
N4 C31 H31 123.5 . . ?
C30 C32 N5 109.1(4) . . ?
C30 C32 H32 125.4 . . ?
N5 C32 H32 125.4 . . ?
C34 C33 N6 110.0(4) . . ?
C34 C33 H33 125.0 . . ?
N6 C33 H33 125.0 . . ?
C33 C34 N7 106.4(4) . . ?
C33 C34 H34 126.8 . . ?
N7 C34 H34 126.8 . . ?
N6 C35 N7 111.7(4) . . ?
N6 C35 H35 124.1 . . ?
N7 C35 H35 124.1 . . ?
N7 C36 C37 112.7(4) . . ?
N7 C36 H36A 109.1 . . ?
C37 C36 H36A 109.1 . . ?
N7 C36 H36B 109.1 . . ?
C37 C36 H36B 109.1 . . ?
H36A C36 H36B 107.8 . . ?
C38 C37 C39 118.8(5) . . ?
C38 C37 C36 121.2(5) . . ?
C39 C37 C36 120.0(5) . . ?
C37 C38 C39 121.3(5) . 2_735 ?
C37 C38 H38 119.4 . . ?
C39 C38 H38 119.4 2_735 . ?
C37 C39 C38 119.9(5) . 2_735 ?
C37 C39 H39 120.1 . . ?
C38 C39 H39 120.1 2_735 . ?
C15 N1 C17 110.3(4) . . ?
C15 N1 C14 111.6(3) . . ?
C17 N1 C14 111.2(4) . . ?
C15 N1 Ni1 103.6(3) . . ?
C17 N1 Ni1 105.7(2) . . ?
C14 N1 Ni1 114.0(2) . . ?
C19 N2 C20 105.2(4) . . ?
C19 N2 Ni1 128.7(3) . . ?
C20 N2 Ni1 126.2(3) . . ?
C19 N3 C21 106.7(4) . . ?
C19 N3 C22 126.4(4) . . ?
C21 N3 C22 126.9(4) . . ?
C31 N4 C30 106.0(3) . . ?
C31 N4 C29 126.8(4) . . ?
C30 N4 C29 127.2(4) . . ?
C31 N5 C32 105.3(3) . . ?
C31 N5 Ni2 123.3(3) . 1_565 ?
C32 N5 Ni2 129.3(3) . 1_565 ?
C35 N6 C33 105.1(3) . . ?
C35 N6 Ni2 130.2(3) . . ?
C33 N6 Ni2 124.3(3) . . ?
C35 N7 C34 106.8(4) . . ?
C35 N7 C36 126.8(4) . . ?
C34 N7 C36 126.3(4) . . ?
C1 O2 Ni1 123.9(3) . 2_744 ?
C18 O3 Ni2 144.5(3) . . ?
C18 O4 Ni1 113.9(2) . . ?
C16 O5 Ni1 114.7(3) . . ?
Ni1 O1W H1A 109(5) . . ?
Ni1 O1W H1B 92(5) . . ?
H1A O1W H1B 84(6) . . ?
O2W O2W' O3W 105(2) . 1_565 ?
O3W' O3W O2W' 161(3) . 1_545 ?

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 C1 C2 C7 -112.9(6) . . . . ?
O2 C1 C2 C7 69.7(6) . . . . ?
O1 C1 C2 C3 67.5(6) . . . . ?
O2 C1 C2 C3 -110.0(5) . . . . ?
C7 C2 C3 C4 1.0(9) . . . . ?
C1 C2 C3 C4 -179.4(5) . . . . ?
C2 C3 C4 C5 2.3(10) . . . . ?
C3 C4 C5 C6 -3.4(10) . . . . ?
C4 C5 C6 C7 1.3(9) . . . . ?
C3 C2 C7 C6 -3.0(7) . . . . ?
C1 C2 C7 C6 177.3(5) . . . . ?
C3 C2 C7 C8 177.1(5) . . . . ?
C1 C2 C7 C8 -2.5(8) . . . . ?
C5 C6 C7 C2 1.9(8) . . . . ?
C5 C6 C7 C8 -178.2(5) . . . . ?
C2 C7 C8 C13 43.0(7) . . . . ?
C6 C7 C8 C13 -136.8(5) . . . . ?
C2 C7 C8 C9 -137.2(5) . . . . ?
C6 C7 C8 C9 43.0(6) . . . . ?
C13 C8 C9 C10 -1.4(7) . . . . ?
C7 C8 C9 C10 178.8(4) . . . . ?
C8 C9 C10 C11 0.9(7) . . . . ?
C9 C10 C11 C12 -0.6(7) . . . . ?
C9 C10 C11 C14 -179.6(4) . . . . ?
C10 C11 C12 C13 0.7(6) . . . . ?
C14 C11 C12 C13 179.7(4) . . . . ?
C9 C8 C13 C12 1.5(6) . . . . ?
C7 C8 C13 C12 -178.6(4) . . . . ?
C11 C12 C13 C8 -1.2(6) . . . . ?
C12 C11 C14 N1 92.7(5) . . . . ?
C10 C11 C14 N1 -88.3(5) . . . . ?
N1 C15 C16 O6 159.0(5) . . . . ?
N1 C15 C16 O5 -25.0(7) . . . . ?
N1 C17 C18 O3 -158.3(4) . . . . ?
N1 C17 C18 O4 25.2(6) . . . . ?
N2 C20 C21 N3 1.0(6) . . . . ?
N3 C22 C23 C28 -119.0(5) . . . . ?
N3 C22 C23 C24 64.8(7) . . . . ?
C28 C23 C24 C25 -2.0(7) . . . . ?
C22 C23 C24 C25 174.3(5) . . . . ?
C23 C24 C25 C26 -0.6(8) . . . . ?
C24 C25 C26 C27 1.8(7) . . . . ?
C24 C25 C26 C29 179.4(5) . . . . ?
C25 C26 C27 C28 -0.3(7) . . . . ?
C29 C26 C27 C28 -178.0(4) . . . . ?
C24 C23 C28 C27 3.5(7) . . . . ?
C22 C23 C28 C27 -172.9(4) . . . . ?
C26 C27 C28 C23 -2.3(8) . . . . ?
C27 C26 C29 N4 -142.6(4) . . . . ?
C25 C26 C29 N4 39.8(6) . . . . ?
N4 C30 C32 N5 0.0(5) . . . . ?
N6 C33 C34 N7 0.4(5) . . . . ?
N7 C36 C37 C38 67.8(6) . . . . ?
N7 C36 C37 C39 -111.5(5) . . . . ?
C39 C37 C38 C39 -0.2(8) . . . 2_735 ?
C36 C37 C38 C39 -179.4(4) . . . 2_735 ?
C38 C37 C39 C38 0.2(8) . . . 2_735 ?
C36 C37 C39 C38 179.4(4) . . . 2_735 ?
C16 C15 N1 C17 -80.2(5) . . . . ?
C16 C15 N1 C14 155.6(4) . . . . ?
C16 C15 N1 Ni1 32.5(5) . . . . ?
C18 C17 N1 C15 98.1(5) . . . . ?
C18 C17 N1 C14 -137.6(4) . . . . ?
C18 C17 N1 Ni1 -13.4(5) . . . . ?
C11 C14 N1 C15 62.0(5) . . . . ?
C11 C14 N1 C17 -61.6(5) . . . . ?
C11 C14 N1 Ni1 179.0(3) . . . . ?
O4 Ni1 N1 C15 -113.8(3) . . . . ?
O5 Ni1 N1 C15 -24.7(3) . . . . ?
N2 Ni1 N1 C15 -69.4(11) . . . . ?
O2 Ni1 N1 C15 153.7(3) 2_744 . . . ?
O1W Ni1 N1 C15 64.0(3) . . . . ?
O4 Ni1 N1 C17 2.3(3) . . . . ?
O5 Ni1 N1 C17 91.4(3) . . . . ?
N2 Ni1 N1 C17 46.6(12) . . . . ?
O2 Ni1 N1 C17 -90.2(3) 2_744 . . . ?
O1W Ni1 N1 C17 -180.0(3) . . . . ?
O4 Ni1 N1 C14 124.7(3) . . . . ?
O5 Ni1 N1 C14 -146.2(3) . . . . ?
N2 Ni1 N1 C14 169.1(10) . . . . ?
O2 Ni1 N1 C14 32.2(3) 2_744 . . . ?
O1W Ni1 N1 C14 -57.5(3) . . . . ?
N3 C19 N2 C20 0.9(5) . . . . ?
N3 C19 N2 Ni1 -178.1(3) . . . . ?
C21 C20 N2 C19 -1.2(5) . . . . ?
C21 C20 N2 Ni1 177.9(3) . . . . ?
O4 Ni1 N2 C19 159.3(4) . . . . ?
O5 Ni1 N2 C19 71.2(4) . . . . ?
O2 Ni1 N2 C19 -107.5(4) 2_744 . . . ?
O1W Ni1 N2 C19 -17.8(4) . . . . ?
N1 Ni1 N2 C19 115.3(10) . . . . ?
O4 Ni1 N2 C20 -19.5(4) . . . . ?
O5 Ni1 N2 C20 -107.6(4) . . . . ?
O2 Ni1 N2 C20 73.7(4) 2_744 . . . ?
O1W Ni1 N2 C20 163.4(4) . . . . ?
N1 Ni1 N2 C20 -63.5(12) . . . . ?
N2 C19 N3 C21 -0.3(5) . . . . ?
N2 C19 N3 C22 -179.4(4) . . . . ?
C20 C21 N3 C19 -0.4(5) . . . . ?
C20 C21 N3 C22 178.7(4) . . . . ?
C23 C22 N3 C19 -86.4(6) . . . . ?
C23 C22 N3 C21 94.7(6) . . . . ?
N5 C31 N4 C30 0.0(5) . . . . ?
N5 C31 N4 C29 178.0(4) . . . . ?
C32 C30 N4 C31 0.0(5) . . . . ?
C32 C30 N4 C29 -178.0(4) . . . . ?
C26 C29 N4 C31 -123.7(4) . . . . ?
C26 C29 N4 C30 53.9(6) . . . . ?
N4 C31 N5 C32 0.1(5) . . . . ?
N4 C31 N5 Ni2 -165.0(3) . . . 1_565 ?
C30 C32 N5 C31 0.0(5) . . . . ?
C30 C32 N5 Ni2 163.8(3) . . . 1_565 ?
N7 C35 N6 C33 0.6(5) . . . . ?
N7 C35 N6 Ni2 173.6(3) . . . . ?
C34 C33 N6 C35 -0.6(5) . . . . ?
C34 C33 N6 Ni2 -174.1(3) . . . . ?
N6 Ni2 N6 C35 -157(100) 2_645 . . . ?
O3 Ni2 N6 C35 140.5(4) . . . . ?
O3 Ni2 N6 C35 -39.5(4) 2_645 . . . ?
N5 Ni2 N6 C35 53.0(4) 2_655 . . . ?
N5 Ni2 N6 C35 -127.0(4) 1_545 . . . ?
N6 Ni2 N6 C33 14(100) 2_645 . . . ?
O3 Ni2 N6 C33 -47.7(3) . . . . ?
O3 Ni2 N6 C33 132.3(3) 2_645 . . . ?
N5 Ni2 N6 C33 -135.2(3) 2_655 . . . ?
N5 Ni2 N6 C33 44.8(3) 1_545 . . . ?
N6 C35 N7 C34 -0.4(5) . . . . ?
N6 C35 N7 C36 176.7(4) . . . . ?
C33 C34 N7 C35 0.0(5) . . . . ?
C33 C34 N7 C36 -177.1(4) . . . . ?
C37 C36 N7 C35 -102.7(5) . . . . ?
C37 C36 N7 C34 73.8(6) . . . . ?
O1 C1 O2 Ni1 -22.4(7) . . . 2_744 ?
C2 C1 O2 Ni1 154.7(3) . . . 2_744 ?
O4 C18 O3 Ni2 -34.0(7) . . . . ?
C17 C18 O3 Ni2 149.9(4) . . . . ?
N6 Ni2 O3 C18 -21.5(5) 2_645 . . . ?
N6 Ni2 O3 C18 158.5(5) . . . . ?
O3 Ni2 O3 C18 63(100) 2_645 . . . ?
N5 Ni2 O3 C18 -107.1(5) 2_655 . . . ?
N5 Ni2 O3 C18 72.9(5) 1_545 . . . ?
O3 C18 O4 Ni1 161.5(3) . . . . ?
C17 C18 O4 Ni1 -22.5(5) . . . . ?
O5 Ni1 O4 C18 -70.1(3) . . . . ?
N2 Ni1 O4 C18 -163.2(3) . . . . ?
O2 Ni1 O4 C18 107.1(3) 2_744 . . . ?
O1W Ni1 O4 C18 -7.3(14) . . . . ?
N1 Ni1 O4 C18 11.3(3) . . . . ?
O6 C16 O5 Ni1 177.0(5) . . . . ?
C15 C16 O5 Ni1 1.3(6) . . . . ?
O4 Ni1 O5 C16 97.3(3) . . . . ?
N2 Ni1 O5 C16 -171.5(4) . . . . ?
O2 Ni1 O5 C16 -17(3) 2_744 . . . ?
O1W Ni1 O5 C16 -76.4(4) . . . . ?
N1 Ni1 O5 C16 14.0(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.073
#=========================END
data_Compound-5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H68 Co3 N14 O20'
_chemical_formula_sum            'C60 H68 Co3 N14 O20'
_chemical_formula_weight         1482.07

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_hall  '-P 1 '

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

_cell_length_a                   8.2990(4)
_cell_length_b                   12.7330(7)
_cell_length_c                   15.7170(7)
_cell_angle_alpha                76.610(4)
_cell_angle_beta                 84.891(4)
_cell_angle_gamma                86.738(4)
_cell_volume                     1608.14(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3753
_cell_measurement_theta_min      2.7956
_cell_measurement_theta_max      29.2293

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             767
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8218
_exptl_absorpt_correction_T_max  0.8830
_exptl_absorpt_process_details   
;
CrysAlis (Oxford Diffraction, 2006)
;
_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  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9827
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.80
_diffrn_reflns_theta_max         25.03
_reflns_number_total             5646
_reflns_number_gt                4490
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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.

For C17 and C17' atoms, some anisotropic displacement ellipsoids were 
rather elongated which led us to use the ISOR restraints.
;

_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)+(0.0391P)²+0.9260P] 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         5646
_refine_ls_number_parameters     473
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0417
_refine_ls_wR_factor_ref         0.1013
_refine_ls_wR_factor_gt          0.0918
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_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
Co1 Co 0.16075(4) 0.23540(3) 0.19599(2) 0.03676(13) Uani 1 1 d . . .
Co2 Co -0.5000 0.0000 0.5000 0.04552(17) Uani 1 2 d S . .
C1 C -0.3323(3) -0.3006(2) -0.01410(19) 0.0387(7) Uani 1 1 d . . .
C2 C -0.4858(3) -0.2919(2) 0.04356(18) 0.0376(7) Uani 1 1 d . . .
C3 C -0.6055(4) -0.3637(3) 0.0418(2) 0.0487(8) Uani 1 1 d . . .
H3 H -0.5853 -0.4151 0.0083 0.058 Uiso 1 1 calc R . .
C4 C -0.7529(4) -0.3602(3) 0.0888(2) 0.0570(9) Uani 1 1 d . . .
H4 H -0.8325 -0.4074 0.0857 0.068 Uiso 1 1 calc R . .
C5 C -0.7813(4) -0.2869(3) 0.1399(2) 0.0550(9) Uani 1 1 d . . .
H5 H -0.8802 -0.2849 0.1725 0.066 Uiso 1 1 calc R . .
C6 C -0.6640(3) -0.2158(3) 0.1436(2) 0.0459(8) Uani 1 1 d . . .
H6 H -0.6849 -0.1671 0.1795 0.055 Uiso 1 1 calc R . .
C7 C -0.5143(3) -0.2151(2) 0.09482(18) 0.0355(6) Uani 1 1 d . . .
C8 C -0.3941(3) -0.1343(2) 0.09908(17) 0.0356(6) Uani 1 1 d . . .
C9 C -0.2291(3) -0.1599(3) 0.1003(2) 0.0440(7) Uani 1 1 d . . .
H9 H -0.1917 -0.2303 0.1006 0.053 Uiso 1 1 calc R . .
C10 C -0.1203(4) -0.0826(3) 0.1012(2) 0.0490(8) Uani 1 1 d . . .
H10 H -0.0105 -0.1016 0.1006 0.059 Uiso 1 1 calc R . .
C11 C -0.1691(4) 0.0222(3) 0.10310(19) 0.0436(7) Uani 1 1 d . . .
C12 C -0.3338(4) 0.0476(3) 0.1023(2) 0.0475(8) Uani 1 1 d . . .
H12 H -0.3707 0.1178 0.1032 0.057 Uiso 1 1 calc R . .
C13 C -0.4440(4) -0.0287(3) 0.10041(19) 0.0435(7) Uani 1 1 d . . .
H13 H -0.5536 -0.0090 0.1000 0.052 Uiso 1 1 calc R . .
C14 C -0.0471(4) 0.1049(3) 0.1069(2) 0.0548(9) Uani 1 1 d . . .
H14A H 0.0545 0.0865 0.0772 0.066 Uiso 1 1 calc R . .
H14B H -0.0850 0.1749 0.0743 0.066 Uiso 1 1 calc R . .
C15 C -0.1623(4) 0.1563(4) 0.2386(2) 0.0690(11) Uani 1 1 d . . .
H15A H -0.2334 0.0969 0.2627 0.083 Uiso 1 1 calc R . .
H15B H -0.2190 0.2083 0.1950 0.083 Uiso 1 1 calc R . .
C16 C -0.1266(4) 0.2093(3) 0.31109(19) 0.0443(7) Uani 1 1 d . . .
C17 C 0.0839(15) 0.0083(11) 0.2151(9) 0.053(3) Uani 0.30 1 d PU . .
C17' C 0.0328(6) 0.0142(4) 0.2590(3) 0.0443(11) Uani 0.70 1 d PU . .
C18 C 0.2145(4) 0.0111(3) 0.27481(19) 0.0432(7) Uani 1 1 d . . .
C19 C 0.4739(4) 0.3604(3) 0.2060(2) 0.0508(8) Uani 1 1 d . . .
H19 H 0.5385 0.3191 0.1736 0.061 Uiso 1 1 calc R . .
C20 C 0.2727(4) 0.4197(3) 0.2710(2) 0.0501(8) Uani 1 1 d . . .
H20 H 0.1684 0.4314 0.2948 0.060 Uiso 1 1 calc R . .
C21 C 0.4073(5) 0.5630(3) 0.3215(2) 0.0642(10) Uani 1 1 d . . .
H21A H 0.3021 0.6002 0.3229 0.077 Uiso 1 1 calc R . .
H21B H 0.4838 0.6142 0.2874 0.077 Uiso 1 1 calc R . .
C22 C 0.4577(4) 0.5276(3) 0.4137(2) 0.0458(7) Uani 1 1 d . . .
C23 C 0.4834(4) 0.4211(3) 0.4557(2) 0.0580(9) Uani 1 1 d . . .
H23 H 0.4727 0.3670 0.4260 0.070 Uiso 1 1 calc R . .
C24 C 0.4749(4) 0.6061(3) 0.4586(2) 0.0537(8) Uani 1 1 d . . .
H24 H 0.4585 0.6784 0.4311 0.064 Uiso 1 1 calc R . .
C25 C -0.3251(5) -0.1349(3) 0.3655(2) 0.0617(9) Uani 1 1 d . . .
H25 H -0.4010 -0.1133 0.3242 0.074 Uiso 1 1 calc R . .
C26 C -0.2060(5) -0.1537(3) 0.4805(3) 0.0649(10) Uani 1 1 d . . .
H26 H -0.1783 -0.1496 0.5356 0.078 Uiso 1 1 calc R . .
C27 C 0.0314(4) -0.2690(3) 0.4440(3) 0.0737(11) Uani 1 1 d . . .
H27A H 0.0839 -0.2449 0.4884 0.088 Uiso 1 1 calc R . .
H27B H 0.1017 -0.2535 0.3902 0.088 Uiso 1 1 calc R . .
C28 C 0.0128(4) -0.3890(3) 0.4726(2) 0.0534(8) Uani 1 1 d . . .
C29 C 0.0646(4) -0.4433(3) 0.5524(3) 0.0579(9) Uani 1 1 d . . .
H29 H 0.1085 -0.4051 0.5880 0.069 Uiso 1 1 calc R . .
C30 C -0.0520(4) -0.4462(3) 0.4199(3) 0.0614(9) Uani 1 1 d . . .
H30 H -0.0871 -0.4103 0.3659 0.074 Uiso 1 1 calc R . .
N1 N -0.0153(3) 0.11492(19) 0.19543(15) 0.0377(6) Uani 1 1 d . . .
N2 N 0.3145(3) 0.3454(2) 0.22614(16) 0.0435(6) Uani 1 1 d . . .
N3 N 0.5303(3) 0.4377(3) 0.23554(18) 0.0566(7) Uani 1 1 d . . .
N4 N 0.3980(3) 0.4751(2) 0.27743(16) 0.0471(6) Uani 1 1 d . . .
N5 N -0.1216(4) -0.2074(2) 0.4291(2) 0.0608(8) Uani 1 1 d . . .
N6 N -0.1968(4) -0.1965(3) 0.3535(2) 0.0688(8) Uani 1 1 d . . .
N7 N -0.3371(3) -0.1056(2) 0.44306(19) 0.0608(8) Uani 1 1 d . . .
O1 O -0.2406(3) -0.38159(19) 0.00922(15) 0.0646(7) Uani 1 1 d . . .
O2 O -0.3106(2) -0.22870(16) -0.08282(12) 0.0415(5) Uani 1 1 d . . .
O3 O -0.2410(3) 0.2189(2) 0.36666(14) 0.0561(6) Uani 1 1 d . . .
O4 O 0.0105(2) 0.24500(19) 0.30839(14) 0.0544(6) Uani 1 1 d . . .
O5 O 0.2843(2) 0.09891(18) 0.26043(14) 0.0505(6) Uani 1 1 d . . .
O6 O 0.2706(3) -0.07861(19) 0.31287(14) 0.0568(6) Uani 1 1 d . . .
O1W O 0.0135(3) 0.3551(2) 0.12072(16) 0.0520(6) Uani 1 1 d . . .
H1A H -0.030(5) 0.412(3) 0.137(3) 0.078 Uiso 1 1 d . . .
H1B H 0.075(5) 0.373(3) 0.079(3) 0.078 Uiso 1 1 d . . .
O2W O -0.1463(3) -0.4763(2) 0.17584(19) 0.0657(7) Uani 1 1 d . . .
H2A H -0.185(5) -0.447(4) 0.128(3) 0.099 Uiso 1 1 d . . .
H2B H -0.237(5) -0.508(4) 0.202(3) 0.099 Uiso 1 1 d . . .
O3W O -0.5129(3) 0.1096(2) 0.38059(16) 0.0630(8) Uani 1 1 d . . .
H3A H -0.437(5) 0.142(4) 0.368(3) 0.095 Uiso 1 1 d . . .
H3B H -0.558(5) 0.102(4) 0.338(3) 0.095 Uiso 1 1 d . . .
O4W O -0.7048(3) -0.0746(2) 0.47792(17) 0.0689(8) Uani 1 1 d . . .
H4A H -0.697(5) -0.093(4) 0.422(3) 0.103 Uiso 1 1 d . . .
H4B H -0.720(6) -0.127(4) 0.514(3) 0.103 Uiso 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
Co1 O5 2.065(2) . ?
Co1 O4 2.093(2) . ?
Co1 O2 2.0934(19) 2 ?
Co1 O1W 2.104(2) . ?
Co1 N2 2.105(2) . ?
Co1 N1 2.180(2) . ?
Co2 O3W 2.070(2) 2_456 ?
Co2 O3W 2.070(2) . ?
Co2 O4W 2.087(2) 2_456 ?
Co2 O4W 2.087(2) . ?
Co2 N7 2.138(3) 2_456 ?
Co2 N7 2.138(3) . ?
C1 O1 1.250(4) . ?
C1 O2 1.250(3) . ?
C1 C2 1.510(4) . ?
C2 C3 1.394(4) . ?
C2 C7 1.403(4) . ?
C3 C4 1.375(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.364(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.381(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.400(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.489(4) . ?
C8 C13 1.389(4) . ?
C8 C9 1.390(4) . ?
C9 C10 1.377(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.378(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.387(4) . ?
C11 C14 1.516(4) . ?
C12 C13 1.378(4) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 N1 1.475(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N1 1.473(4) . ?
C15 C16 1.510(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 O4 1.243(3) . ?
C16 O3 1.252(3) . ?
C17 C17' 0.794(12) . ?
C17 C18 1.502(12) . ?
C17 N1 1.530(13) . ?
C17' N1 1.491(5) . ?
C17' C18 1.547(6) . ?
C18 O6 1.246(4) . ?
C18 O5 1.253(4) . ?
C19 N3 1.307(4) . ?
C19 N2 1.346(4) . ?
C19 H19 0.9300 . ?
C20 N4 1.313(4) . ?
C20 N2 1.320(4) . ?
C20 H20 0.9300 . ?
C21 N4 1.454(4) . ?
C21 C22 1.504(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C24 1.371(4) . ?
C22 C23 1.378(5) . ?
C23 C24 1.380(5) 2_666 ?
C23 H23 0.9300 . ?
C24 C23 1.380(5) 2_666 ?
C24 H24 0.9300 . ?
C25 N6 1.312(5) . ?
C25 N7 1.348(4) . ?
C25 H25 0.9300 . ?
C26 N5 1.309(5) . ?
C26 N7 1.333(4) . ?
C26 H26 0.9300 . ?
C27 N5 1.462(4) . ?
C27 C28 1.503(5) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.378(5) . ?
C28 C30 1.381(5) . ?
C29 C30 1.380(5) 2_546 ?
C29 H29 0.9300 . ?
C30 C29 1.380(5) 2_546 ?
C30 H30 0.9300 . ?
N3 N4 1.350(4) . ?
N5 N6 1.365(4) . ?
O2 Co1 2.0934(19) 2 ?
O1W H1A 0.87(4) . ?
O1W H1B 0.79(4) . ?
O2W H2A 0.84(5) . ?
O2W H2B 0.90(5) . ?
O3W H3A 0.76(5) . ?
O3W H3B 0.81(5) . ?
O4W H4A 0.95(5) . ?
O4W H4B 0.77(5) . ?

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
O5 Co1 O4 92.72(9) . . ?
O5 Co1 O2 88.14(8) . 2 ?
O4 Co1 O2 179.01(9) . 2 ?
O5 Co1 O1W 169.73(9) . . ?
O4 Co1 O1W 89.58(10) . . ?
O2 Co1 O1W 89.66(9) 2 . ?
O5 Co1 N2 95.20(9) . . ?
O4 Co1 N2 89.21(9) . . ?
O2 Co1 N2 90.24(9) 2 . ?
O1W Co1 N2 94.84(10) . . ?
O5 Co1 N1 80.72(8) . . ?
O4 Co1 N1 79.13(8) . . ?
O2 Co1 N1 101.49(8) 2 . ?
O1W Co1 N1 89.89(9) . . ?
N2 Co1 N1 167.39(9) . . ?
O3W Co2 O3W 180.00(9) 2_456 . ?
O3W Co2 O4W 90.44(10) 2_456 2_456 ?
O3W Co2 O4W 89.56(10) . 2_456 ?
O3W Co2 O4W 89.56(10) 2_456 . ?
O3W Co2 O4W 90.44(10) . . ?
O4W Co2 O4W 180.00(14) 2_456 . ?
O3W Co2 N7 91.92(12) 2_456 2_456 ?
O3W Co2 N7 88.08(12) . 2_456 ?
O4W Co2 N7 93.25(12) 2_456 2_456 ?
O4W Co2 N7 86.75(12) . 2_456 ?
O3W Co2 N7 88.08(12) 2_456 . ?
O3W Co2 N7 91.92(12) . . ?
O4W Co2 N7 86.75(12) 2_456 . ?
O4W Co2 N7 93.25(12) . . ?
N7 Co2 N7 180.00(14) 2_456 . ?
O1 C1 O2 125.4(3) . . ?
O1 C1 C2 117.0(3) . . ?
O2 C1 C2 117.5(3) . . ?
C3 C2 C7 119.8(3) . . ?
C3 C2 C1 116.2(3) . . ?
C7 C2 C1 123.9(2) . . ?
C4 C3 C2 121.3(3) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C5 C4 C3 119.5(3) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 120.3(3) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C7 121.7(3) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C6 C7 C2 117.3(3) . . ?
C6 C7 C8 119.5(3) . . ?
C2 C7 C8 123.2(2) . . ?
C13 C8 C9 117.3(3) . . ?
C13 C8 C7 120.5(2) . . ?
C9 C8 C7 122.2(3) . . ?
C10 C9 C8 120.9(3) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C11 122.1(3) . . ?
C9 C10 H10 119.0 . . ?
C11 C10 H10 119.0 . . ?
C10 C11 C12 117.0(3) . . ?
C10 C11 C14 121.0(3) . . ?
C12 C11 C14 122.0(3) . . ?
C13 C12 C11 121.5(3) . . ?
C13 C12 H12 119.2 . . ?
C11 C12 H12 119.2 . . ?
C12 C13 C8 121.2(3) . . ?
C12 C13 H13 119.4 . . ?
C8 C13 H13 119.4 . . ?
N1 C14 C11 115.9(2) . . ?
N1 C14 H14A 108.3 . . ?
C11 C14 H14A 108.3 . . ?
N1 C14 H14B 108.3 . . ?
C11 C14 H14B 108.3 . . ?
H14A C14 H14B 107.4 . . ?
N1 C15 C16 113.0(3) . . ?
N1 C15 H15A 109.0 . . ?
C16 C15 H15A 109.0 . . ?
N1 C15 H15B 109.0 . . ?
C16 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
O4 C16 O3 125.1(3) . . ?
O4 C16 C15 117.8(3) . . ?
O3 C16 C15 117.0(3) . . ?
C17' C17 C18 78.1(11) . . ?
C17' C17 N1 72.0(10) . . ?
C18 C17 N1 111.9(8) . . ?
C17 C17' N1 77.5(10) . . ?
C17 C17' C18 71.8(10) . . ?
N1 C17' C18 111.6(3) . . ?
O6 C18 O5 125.9(3) . . ?
O6 C18 C17 115.6(6) . . ?
O5 C18 C17 114.9(6) . . ?
O6 C18 C17' 115.1(3) . . ?
O5 C18 C17' 118.2(3) . . ?
C17 C18 C17' 30.1(5) . . ?
N3 C19 N2 114.5(3) . . ?
N3 C19 H19 122.8 . . ?
N2 C19 H19 122.8 . . ?
N4 C20 N2 111.0(3) . . ?
N4 C20 H20 124.5 . . ?
N2 C20 H20 124.5 . . ?
N4 C21 C22 114.2(3) . . ?
N4 C21 H21A 108.7 . . ?
C22 C21 H21A 108.7 . . ?
N4 C21 H21B 108.7 . . ?
C22 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
C24 C22 C23 118.6(3) . . ?
C24 C22 C21 117.7(3) . . ?
C23 C22 C21 123.6(3) . . ?
C22 C23 C24 120.7(3) . 2_666 ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 2_666 . ?
C22 C24 C23 120.6(3) . 2_666 ?
C22 C24 H24 119.7 . . ?
C23 C24 H24 119.7 2_666 . ?
N6 C25 N7 114.1(3) . . ?
N6 C25 H25 122.9 . . ?
N7 C25 H25 122.9 . . ?
N5 C26 N7 110.8(4) . . ?
N5 C26 H26 124.6 . . ?
N7 C26 H26 124.6 . . ?
N5 C27 C28 113.8(3) . . ?
N5 C27 H27A 108.8 . . ?
C28 C27 H27A 108.8 . . ?
N5 C27 H27B 108.8 . . ?
C28 C27 H27B 108.8 . . ?
H27A C27 H27B 107.7 . . ?
C29 C28 C30 119.4(3) . . ?
C29 C28 C27 119.1(3) . . ?
C30 C28 C27 121.5(4) . . ?
C28 C29 C30 120.7(3) . 2_546 ?
C28 C29 H29 119.7 . . ?
C30 C29 H29 119.7 2_546 . ?
C29 C30 C28 119.9(3) 2_546 . ?
C29 C30 H30 120.0 2_546 . ?
C28 C30 H30 120.0 . . ?
C15 N1 C14 110.0(2) . . ?
C15 N1 C17' 104.4(3) . . ?
C14 N1 C17' 117.2(3) . . ?
C15 N1 C17 133.4(6) . . ?
C14 N1 C17 93.6(5) . . ?
C17' N1 C17 30.4(5) . . ?
C15 N1 Co1 102.63(18) . . ?
C14 N1 Co1 113.94(18) . . ?
C17' N1 Co1 107.3(2) . . ?
C17 N1 Co1 103.4(5) . . ?
C20 N2 C19 102.3(3) . . ?
C20 N2 Co1 126.6(2) . . ?
C19 N2 Co1 131.1(2) . . ?
C19 N3 N4 103.0(2) . . ?
C20 N4 N3 109.2(3) . . ?
C20 N4 C21 129.4(3) . . ?
N3 N4 C21 121.3(3) . . ?
C26 N5 N6 109.3(3) . . ?
C26 N5 C27 128.4(4) . . ?
N6 N5 C27 122.3(3) . . ?
C25 N6 N5 103.1(3) . . ?
C26 N7 C25 102.8(3) . . ?
C26 N7 Co2 123.3(3) . . ?
C25 N7 Co2 133.7(3) . . ?
C1 O2 Co1 128.43(18) . 2 ?
C16 O4 Co1 114.87(18) . . ?
C18 O5 Co1 117.26(19) . . ?
Co1 O1W H1A 126(3) . . ?
Co1 O1W H1B 99(3) . . ?
H1A O1W H1B 110(4) . . ?
H2A O2W H2B 97(4) . . ?
Co2 O3W H3A 112(3) . . ?
Co2 O3W H3B 127(3) . . ?
H3A O3W H3B 113(4) . . ?
Co2 O4W H4A 113(3) . . ?
Co2 O4W H4B 111(4) . . ?
H4A O4W H4B 108(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
O1 C1 C2 C3 -71.5(4) . . . . ?
O2 C1 C2 C3 105.6(3) . . . . ?
O1 C1 C2 C7 110.6(3) . . . . ?
O2 C1 C2 C7 -72.2(4) . . . . ?
C7 C2 C3 C4 0.8(5) . . . . ?
C1 C2 C3 C4 -177.2(3) . . . . ?
C2 C3 C4 C5 -1.8(5) . . . . ?
C3 C4 C5 C6 0.9(5) . . . . ?
C4 C5 C6 C7 0.9(5) . . . . ?
C5 C6 C7 C2 -1.8(4) . . . . ?
C5 C6 C7 C8 178.1(3) . . . . ?
C3 C2 C7 C6 1.0(4) . . . . ?
C1 C2 C7 C6 178.8(3) . . . . ?
C3 C2 C7 C8 -178.9(3) . . . . ?
C1 C2 C7 C8 -1.1(4) . . . . ?
C6 C7 C8 C13 -40.0(4) . . . . ?
C2 C7 C8 C13 139.9(3) . . . . ?
C6 C7 C8 C9 141.1(3) . . . . ?
C2 C7 C8 C9 -39.0(4) . . . . ?
C13 C8 C9 C10 -1.1(4) . . . . ?
C7 C8 C9 C10 177.7(3) . . . . ?
C8 C9 C10 C11 1.6(5) . . . . ?
C9 C10 C11 C12 -1.2(5) . . . . ?
C9 C10 C11 C14 178.1(3) . . . . ?
C10 C11 C12 C13 0.4(4) . . . . ?
C14 C11 C12 C13 -178.9(3) . . . . ?
C11 C12 C13 C8 -0.1(5) . . . . ?
C9 C8 C13 C12 0.4(4) . . . . ?
C7 C8 C13 C12 -178.5(3) . . . . ?
C10 C11 C14 N1 -91.7(4) . . . . ?
C12 C11 C14 N1 87.6(4) . . . . ?
N1 C15 C16 O4 23.5(5) . . . . ?
N1 C15 C16 O3 -160.3(3) . . . . ?
C18 C17 C17' N1 118.0(5) . . . . ?
N1 C17 C17' C18 -118.0(5) . . . . ?
C17' C17 C18 O6 96.3(10) . . . . ?
N1 C17 C18 O6 161.2(6) . . . . ?
C17' C17 C18 O5 -103.8(11) . . . . ?
N1 C17 C18 O5 -38.9(10) . . . . ?
N1 C17 C18 C17' 64.9(10) . . . . ?
C17 C17' C18 O6 -98.3(11) . . . . ?
N1 C17' C18 O6 -166.3(3) . . . . ?
C17 C17' C18 O5 91.6(12) . . . . ?
N1 C17' C18 O5 23.6(5) . . . . ?
N1 C17' C18 C17 -68.0(11) . . . . ?
N4 C21 C22 C24 177.7(3) . . . . ?
N4 C21 C22 C23 -3.9(5) . . . . ?
C24 C22 C23 C24 0.3(6) . . . 2_666 ?
C21 C22 C23 C24 -178.1(3) . . . 2_666 ?
C23 C22 C24 C23 -0.3(6) . . . 2_666 ?
C21 C22 C24 C23 178.2(3) . . . 2_666 ?
N5 C27 C28 C29 -119.9(4) . . . . ?
N5 C27 C28 C30 61.4(5) . . . . ?
C30 C28 C29 C30 -0.1(6) . . . 2_546 ?
C27 C28 C29 C30 -178.8(3) . . . 2_546 ?
C29 C28 C30 C29 0.1(6) . . . 2_546 ?
C27 C28 C30 C29 178.8(3) . . . 2_546 ?
C16 C15 N1 C14 -157.5(3) . . . . ?
C16 C15 N1 C17' 75.9(4) . . . . ?
C16 C15 N1 C17 86.6(7) . . . . ?
C16 C15 N1 Co1 -35.9(3) . . . . ?
C11 C14 N1 C15 -65.3(4) . . . . ?
C11 C14 N1 C17' 53.7(4) . . . . ?
C11 C14 N1 C17 73.8(6) . . . . ?
C11 C14 N1 Co1 -179.9(2) . . . . ?
C17 C17' N1 C15 164.5(11) . . . . ?
C18 C17' N1 C15 -131.1(3) . . . . ?
C17 C17' N1 C14 42.6(11) . . . . ?
C18 C17' N1 C14 107.0(4) . . . . ?
C18 C17' N1 C17 64.4(10) . . . . ?
C17 C17' N1 Co1 -87.0(11) . . . . ?
C18 C17' N1 Co1 -22.6(4) . . . . ?
C17' C17 N1 C15 -20.9(14) . . . . ?
C18 C17 N1 C15 -89.5(9) . . . . ?
C17' C17 N1 C14 -142.9(10) . . . . ?
C18 C17 N1 C14 148.5(8) . . . . ?
C18 C17 N1 C17' -68.6(10) . . . . ?
C17' C17 N1 Co1 101.4(10) . . . . ?
C18 C17 N1 Co1 32.8(9) . . . . ?
O5 Co1 N1 C15 123.9(2) . . . . ?
O4 Co1 N1 C15 29.3(2) . . . . ?
O2 Co1 N1 C15 -150.0(2) 2 . . . ?
O1W Co1 N1 C15 -60.3(2) . . . . ?
N2 Co1 N1 C15 51.9(5) . . . . ?
O5 Co1 N1 C14 -117.3(2) . . . . ?
O4 Co1 N1 C14 148.1(2) . . . . ?
O2 Co1 N1 C14 -31.1(2) 2 . . . ?
O1W Co1 N1 C14 58.5(2) . . . . ?
N2 Co1 N1 C14 170.8(4) . . . . ?
O5 Co1 N1 C17' 14.2(3) . . . . ?
O4 Co1 N1 C17' -80.4(3) . . . . ?
O2 Co1 N1 C17' 100.4(3) 2 . . . ?
O1W Co1 N1 C17' -170.0(3) . . . . ?
N2 Co1 N1 C17' -57.8(5) . . . . ?
O5 Co1 N1 C17 -17.2(6) . . . . ?
O4 Co1 N1 C17 -111.8(6) . . . . ?
O2 Co1 N1 C17 69.0(6) 2 . . . ?
O1W Co1 N1 C17 158.7(6) . . . . ?
N2 Co1 N1 C17 -89.1(7) . . . . ?
N4 C20 N2 C19 -0.2(4) . . . . ?
N4 C20 N2 Co1 -179.6(2) . . . . ?
N3 C19 N2 C20 0.2(4) . . . . ?
N3 C19 N2 Co1 179.6(2) . . . . ?
O5 Co1 N2 C20 -119.7(3) . . . . ?
O4 Co1 N2 C20 -27.0(3) . . . . ?
O2 Co1 N2 C20 152.1(3) 2 . . . ?
O1W Co1 N2 C20 62.5(3) . . . . ?
N1 Co1 N2 C20 -49.3(6) . . . . ?
O5 Co1 N2 C19 61.0(3) . . . . ?
O4 Co1 N2 C19 153.7(3) . . . . ?
O2 Co1 N2 C19 -27.1(3) 2 . . . ?
O1W Co1 N2 C19 -116.8(3) . . . . ?
N1 Co1 N2 C19 131.5(4) . . . . ?
N2 C19 N3 N4 -0.1(4) . . . . ?
N2 C20 N4 N3 0.1(4) . . . . ?
N2 C20 N4 C21 -179.3(3) . . . . ?
C19 N3 N4 C20 0.0(4) . . . . ?
C19 N3 N4 C21 179.5(3) . . . . ?
C22 C21 N4 C20 94.3(4) . . . . ?
C22 C21 N4 N3 -85.0(4) . . . . ?
N7 C26 N5 N6 -0.1(4) . . . . ?
N7 C26 N5 C27 178.4(3) . . . . ?
C28 C27 N5 C26 101.5(4) . . . . ?
C28 C27 N5 N6 -80.2(5) . . . . ?
N7 C25 N6 N5 0.1(4) . . . . ?
C26 N5 N6 C25 0.0(4) . . . . ?
C27 N5 N6 C25 -178.6(3) . . . . ?
N5 C26 N7 C25 0.2(4) . . . . ?
N5 C26 N7 Co2 -175.4(2) . . . . ?
N6 C25 N7 C26 -0.1(4) . . . . ?
N6 C25 N7 Co2 174.7(2) . . . . ?
O3W Co2 N7 C26 -43.7(3) 2_456 . . . ?
O3W Co2 N7 C26 136.3(3) . . . . ?
O4W Co2 N7 C26 46.8(3) 2_456 . . . ?
O4W Co2 N7 C26 -133.2(3) . . . . ?
N7 Co2 N7 C26 -179(100) 2_456 . . . ?
O3W Co2 N7 C25 142.3(3) 2_456 . . . ?
O3W Co2 N7 C25 -37.7(3) . . . . ?
O4W Co2 N7 C25 -127.2(3) 2_456 . . . ?
O4W Co2 N7 C25 52.8(3) . . . . ?
N7 Co2 N7 C25 7(100) 2_456 . . . ?
O1 C1 O2 Co1 18.3(4) . . . 2 ?
C2 C1 O2 Co1 -158.64(19) . . . 2 ?
O3 C16 O4 Co1 -171.0(3) . . . . ?
C15 C16 O4 Co1 4.9(4) . . . . ?
O5 Co1 O4 C16 -100.4(2) . . . . ?
O2 Co1 O4 C16 109(5) 2 . . . ?
O1W Co1 O4 C16 69.6(2) . . . . ?
N2 Co1 O4 C16 164.5(2) . . . . ?
N1 Co1 O4 C16 -20.3(2) . . . . ?
O6 C18 O5 Co1 -179.8(2) . . . . ?
C17 C18 O5 Co1 22.7(7) . . . . ?
C17' C18 O5 Co1 -10.9(4) . . . . ?
O4 Co1 O5 C18 76.3(2) . . . . ?
O2 Co1 O5 C18 -104.1(2) 2 . . . ?
O1W Co1 O5 C18 -26.4(6) . . . . ?
N2 Co1 O5 C18 165.8(2) . . . . ?
N1 Co1 O5 C18 -2.2(2) . . . . ?

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
O2W H2A O1 0.84(5) 1.94(5) 2.778(4) 171(4) .
O3W H3A O3 0.76(5) 1.94(5) 2.684(3) 165(5) .
C23 H23 N4 0.93 2.53 2.869(4) 101.8 .
O1W H1A O2W 0.87(4) 1.86(4) 2.729(4) 173(4) 1_565
O1W H1B O1 0.79(4) 1.85(4) 2.628(3) 166(4) 2
O2W H2B N3 0.90(5) 2.07(5) 2.948(4) 166(4) 1_445
O3W H3B O5 0.81(5) 1.88(5) 2.670(3) 163(4) 1_455
O4W H4A O6 0.95(5) 1.73(5) 2.633(3) 157(4) 1_455
O4W H4B O3 0.77(5) 1.98(5) 2.714(3) 158(5) 2_456

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.053
#=========================END
data_Compound-6

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H68 N14 Ni3 O20'
_chemical_formula_sum            'C60 H68 N14 Ni3 O20'
_chemical_formula_weight         1481.41

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_hall  '-P 1'

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

_cell_length_a                   8.2860(9)
_cell_length_b                   12.6490(14)
_cell_length_c                   15.7450(15)
_cell_angle_alpha                76.209(9)
_cell_angle_beta                 84.840(9)
_cell_angle_gamma                86.847(9)
_cell_volume                     1595.2(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2914
_cell_measurement_theta_min      2.9212
_cell_measurement_theta_max      29.1348

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             770
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8017
_exptl_absorpt_correction_T_max  0.8690
_exptl_absorpt_process_details   
;
CrysAlis (Oxford Diffraction, 2006)
;
_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  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9792
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0588
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.93
_diffrn_reflns_theta_max         25.03
_reflns_number_total             5609
_reflns_number_gt                4172
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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.

For N1, C17 and C18 atoms, SIMU restraint was used to make them behave 
similar anisotropic displacement parameters.
;

_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)+(0.0273P)²+0.7299P] 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         5609
_refine_ls_number_parameters     473
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0476
_refine_ls_wR_factor_ref         0.0938
_refine_ls_wR_factor_gt          0.0828
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.027
_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 0.34017(5) 0.26343(3) 0.30287(3) 0.03633(14) Uani 1 1 d . . .
Ni2 Ni 1.0000 0.5000 0.0000 0.0474(2) Uani 1 2 d S . .
C1 C 0.8285(4) 0.7987(3) 0.5159(2) 0.0383(8) Uani 1 1 d . . .
C2 C 0.9819(4) 0.7905(2) 0.4580(2) 0.0355(8) Uani 1 1 d . . .
C3 C 1.1025(4) 0.8625(3) 0.4605(2) 0.0478(9) Uani 1 1 d . . .
H3 H 1.0826 0.9131 0.4948 0.057 Uiso 1 1 calc R . .
C4 C 1.2494(5) 0.8599(3) 0.4134(3) 0.0557(11) Uani 1 1 d . . .
H4 H 1.3289 0.9077 0.4166 0.067 Uiso 1 1 calc R . .
C5 C 1.2788(4) 0.7869(3) 0.3617(3) 0.0545(10) Uani 1 1 d . . .
H5 H 1.3781 0.7853 0.3293 0.065 Uiso 1 1 calc R . .
C6 C 1.1603(4) 0.7154(3) 0.3577(2) 0.0457(9) Uani 1 1 d . . .
H6 H 1.1810 0.6669 0.3216 0.055 Uiso 1 1 calc R . .
C7 C 1.0109(4) 0.7143(2) 0.4064(2) 0.0342(8) Uani 1 1 d . . .
C8 C 0.8911(4) 0.6326(2) 0.4019(2) 0.0355(8) Uani 1 1 d . . .
C9 C 0.7258(4) 0.6577(3) 0.4013(2) 0.0451(9) Uani 1 1 d . . .
H9 H 0.6879 0.7281 0.4019 0.054 Uiso 1 1 calc R . .
C10 C 0.6168(4) 0.5790(3) 0.4001(2) 0.0486(9) Uani 1 1 d . . .
H10 H 0.5066 0.5974 0.4009 0.058 Uiso 1 1 calc R . .
C11 C 0.6675(5) 0.4739(3) 0.3975(2) 0.0440(9) Uani 1 1 d . . .
C12 C 0.8306(5) 0.4492(3) 0.3975(2) 0.0479(10) Uani 1 1 d . . .
H12 H 0.8678 0.3790 0.3958 0.057 Uiso 1 1 calc R . .
C13 C 0.9414(4) 0.5263(3) 0.3998(2) 0.0426(8) Uani 1 1 d . . .
H13 H 1.0513 0.5068 0.4000 0.051 Uiso 1 1 calc R . .
C14 C 0.5440(5) 0.3899(3) 0.3938(2) 0.0568(11) Uani 1 1 d . A .
H14A H 0.5831 0.3189 0.4252 0.068 Uiso 1 1 calc R . .
H14B H 0.4431 0.4071 0.4248 0.068 Uiso 1 1 calc R . .
C15 C 0.6552(5) 0.3463(4) 0.2591(3) 0.0708(13) Uani 1 1 d . A .
H15A H 0.7180 0.2957 0.3011 0.085 Uiso 1 1 calc R . .
H15B H 0.7211 0.4088 0.2336 0.085 Uiso 1 1 calc R . .
C16 C 0.6206(5) 0.2920(3) 0.1874(2) 0.0459(9) Uani 1 1 d . A .
C17 C 0.407(3) 0.4874(13) 0.289(2) 0.050(5) Uani 0.32(3) 1 d PU A 1
H17A H 0.3547 0.4977 0.3443 0.060 Uiso 0.32(3) 1 calc PR A 1
H17B H 0.4770 0.5482 0.2648 0.060 Uiso 0.32(3) 1 calc PR A 1
C17' C 0.4570(13) 0.4843(6) 0.2438(9) 0.046(3) Uani 0.68(3) 1 d P A 2
H17C H 0.5228 0.4919 0.1887 0.055 Uiso 0.68(3) 1 calc PR A 2
H17D H 0.4760 0.5461 0.2676 0.055 Uiso 0.68(3) 1 calc PR A 2
C18 C 0.2794(4) 0.4866(3) 0.2263(2) 0.0434(9) Uani 1 1 d U . .
C19 C 0.0286(4) 0.1414(3) 0.2936(2) 0.0501(9) Uani 1 1 d . A .
H19 H -0.0354 0.1834 0.3256 0.060 Uiso 1 1 calc R . .
C20 C 0.2312(4) 0.0795(3) 0.2297(2) 0.0492(9) Uani 1 1 d . A .
H20 H 0.3357 0.0670 0.2064 0.059 Uiso 1 1 calc R . .
C21 C 0.0932(5) -0.0634(3) 0.1784(2) 0.0612(11) Uani 1 1 d . . .
H21A H 0.0164 -0.1151 0.2128 0.073 Uiso 1 1 calc R . .
H21B H 0.1984 -0.1009 0.1769 0.073 Uiso 1 1 calc R . .
C22 C 0.0424(4) -0.0271(3) 0.0863(2) 0.0455(9) Uani 1 1 d . . .
C23 C 0.0185(5) 0.0802(3) 0.0434(2) 0.0540(10) Uani 1 1 d . . .
H23 H 0.0312 0.1351 0.0722 0.065 Uiso 1 1 calc R . .
C24 C 0.0238(5) -0.1069(3) 0.0418(2) 0.0531(10) Uani 1 1 d . . .
H24 H 0.0403 -0.1797 0.0698 0.064 Uiso 1 1 calc R . .
C25 C 0.7089(6) 0.6517(3) 0.0187(3) 0.0658(12) Uani 1 1 d . . .
H25 H 0.6821 0.6488 -0.0368 0.079 Uiso 1 1 calc R . .
C26 C 0.8262(6) 0.6308(3) 0.1346(3) 0.0643(12) Uani 1 1 d . . .
H26 H 0.9016 0.6084 0.1761 0.077 Uiso 1 1 calc R . .
C27 C 0.4694(5) 0.7660(3) 0.0562(3) 0.0741(13) Uani 1 1 d . . .
H27A H 0.3998 0.7500 0.1102 0.089 Uiso 1 1 calc R . .
H27B H 0.4163 0.7416 0.0122 0.089 Uiso 1 1 calc R . .
C28 C 0.4871(4) 0.8881(3) 0.0267(3) 0.0546(10) Uani 1 1 d . . .
C29 C 0.5538(5) 0.9459(3) 0.0798(3) 0.0640(11) Uani 1 1 d . . .
H29 H 0.5897 0.9093 0.1337 0.077 Uiso 1 1 calc R . .
C30 C 0.4340(5) 0.9425(3) -0.0518(3) 0.0580(11) Uani 1 1 d . . .
H30 H 0.3890 0.9041 -0.0869 0.070 Uiso 1 1 calc R . .
N1 N 0.5095(3) 0.3825(2) 0.30589(17) 0.0361(7) Uani 1 1 d U . .
N2 N 0.1898(3) 0.1540(2) 0.27457(18) 0.0417(7) Uani 1 1 d . . .
N3 N -0.0299(4) 0.0646(3) 0.2631(2) 0.0537(8) Uani 1 1 d . . .
N4 N 0.1034(4) 0.0255(2) 0.22250(18) 0.0456(8) Uani 1 1 d . A .
N5 N 0.8398(4) 0.6029(2) 0.0562(2) 0.0588(9) Uani 1 1 d . . .
N6 N 0.6952(5) 0.6930(3) 0.1468(2) 0.0705(10) Uani 1 1 d . . .
N7 N 0.6226(4) 0.7043(2) 0.0706(3) 0.0620(9) Uani 1 1 d . . .
O1 O 0.7341(3) 0.8792(2) 0.49198(17) 0.0636(8) Uani 1 1 d . . .
O2 O 0.8089(3) 0.72704(16) 0.58605(14) 0.0387(5) Uani 1 1 d . . .
O3 O 0.2219(3) 0.57715(19) 0.18835(16) 0.0565(7) Uani 1 1 d . A .
O4 O 0.2136(3) 0.39660(18) 0.23674(15) 0.0486(6) Uani 1 1 d . A .
O5 O 0.4834(3) 0.2557(2) 0.19045(15) 0.0533(7) Uani 1 1 d . . .
O6 O 0.7344(3) 0.2832(2) 0.13122(16) 0.0590(7) Uani 1 1 d . . .
O1W O 1.2005(4) 0.5727(2) 0.02378(19) 0.0677(9) Uani 1 1 d . . .
H1A H 1.191(6) 0.595(4) 0.078(3) 0.101 Uiso 1 1 d . . .
H1B H 1.230(6) 0.622(4) -0.017(3) 0.101 Uiso 1 1 d . . .
O2W O 0.9884(3) 0.6124(2) -0.11682(18) 0.0663(9) Uani 1 1 d . . .
H2A H 1.061(6) 0.648(4) -0.130(3) 0.099 Uiso 1 1 d . . .
H2B H 0.947(6) 0.604(4) -0.164(3) 0.099 Uiso 1 1 d . . .
O3W O 0.4868(3) 0.1448(2) 0.37588(18) 0.0491(7) Uani 1 1 d . . .
H3A H 0.430(5) 0.124(3) 0.419(3) 0.074 Uiso 1 1 d . . .
H3B H 0.528(5) 0.088(3) 0.362(3) 0.074 Uiso 1 1 d . . .
O4W O 0.6473(3) -0.0259(2) 0.3231(2) 0.0628(8) Uani 1 1 d . . .
H4A H 0.733(6) -0.004(4) 0.298(3) 0.094 Uiso 1 1 d . . .
H4B H 0.679(6) -0.055(4) 0.372(3) 0.094 Uiso 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O4 2.047(2) . ?
Ni1 O5 2.060(2) . ?
Ni1 N2 2.062(3) . ?
Ni1 O3W 2.068(3) . ?
Ni1 O2 2.072(2) 2_666 ?
Ni1 N1 2.125(2) . ?
Ni2 O2W 2.045(2) 2_765 ?
Ni2 O2W 2.045(2) . ?
Ni2 O1W 2.047(2) . ?
Ni2 O1W 2.047(2) 2_765 ?
Ni2 N5 2.094(4) . ?
Ni2 N5 2.094(4) 2_765 ?
C1 O1 1.254(4) . ?
C1 O2 1.254(4) . ?
C1 C2 1.510(5) . ?
C2 C3 1.398(4) . ?
C2 C7 1.400(4) . ?
C3 C4 1.370(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.369(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.387(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.395(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.490(4) . ?
C8 C9 1.389(5) . ?
C8 C13 1.392(4) . ?
C9 C10 1.385(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.380(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.370(5) . ?
C11 C14 1.529(4) . ?
C12 C13 1.385(4) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 N1 1.465(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N1 1.466(5) . ?
C15 C16 1.510(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 O5 1.242(4) . ?
C16 O6 1.253(4) . ?
C17 C18 1.515(18) . ?
C17 N1 1.516(17) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17' N1 1.489(8) . ?
C17' C18 1.519(9) . ?
C17' H17C 0.9700 . ?
C17' H17D 0.9700 . ?
C18 O3 1.249(4) . ?
C18 O4 1.258(4) . ?
C19 N3 1.314(4) . ?
C19 N2 1.352(4) . ?
C19 H19 0.9300 . ?
C20 N4 1.319(4) . ?
C20 N2 1.320(4) . ?
C20 H20 0.9300 . ?
C21 N4 1.464(4) . ?
C21 C22 1.504(5) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.377(5) . ?
C22 C24 1.381(5) . ?
C23 C24 1.375(5) 2 ?
C23 H23 0.9300 . ?
C24 C23 1.375(5) 2 ?
C24 H24 0.9300 . ?
C25 N7 1.313(5) . ?
C25 N5 1.331(5) . ?
C25 H25 0.9300 . ?
C26 N6 1.332(5) . ?
C26 N5 1.356(5) . ?
C26 H26 0.9300 . ?
C27 N7 1.459(5) . ?
C27 C28 1.514(5) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C30 1.362(5) . ?
C28 C29 1.398(5) . ?
C29 C30 1.382(5) 2_675 ?
C29 H29 0.9300 . ?
C30 C29 1.382(5) 2_675 ?
C30 H30 0.9300 . ?
N3 N4 1.355(4) . ?
N6 N7 1.364(5) . ?
O2 Ni1 2.072(2) 2_666 ?
O1W H1A 0.96(5) . ?
O1W H1B 0.81(5) . ?
O2W H2A 0.75(5) . ?
O2W H2B 0.87(5) . ?
O3W H3A 0.78(4) . ?
O3W H3B 0.85(4) . ?
O4W H4A 0.81(5) . ?
O4W H4B 0.83(5) . ?

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
O4 Ni1 O5 91.12(10) . . ?
O4 Ni1 N2 93.71(10) . . ?
O5 Ni1 N2 88.55(10) . . ?
O4 Ni1 O3W 171.68(10) . . ?
O5 Ni1 O3W 90.20(11) . . ?
N2 Ni1 O3W 94.54(11) . . ?
O4 Ni1 O2 87.57(9) . 2_666 ?
O5 Ni1 O2 178.48(10) . 2_666 ?
N2 Ni1 O2 90.77(10) . 2_666 ?
O3W Ni1 O2 91.21(10) . 2_666 ?
O4 Ni1 N1 82.49(9) . . ?
O5 Ni1 N1 81.22(10) . . ?
N2 Ni1 N1 168.98(11) . . ?
O3W Ni1 N1 89.59(10) . . ?
O2 Ni1 N1 99.36(10) 2_666 . ?
O2W Ni2 O2W 180.00(17) 2_765 . ?
O2W Ni2 O1W 90.40(11) 2_765 . ?
O2W Ni2 O1W 89.60(11) . . ?
O2W Ni2 O1W 89.60(11) 2_765 2_765 ?
O2W Ni2 O1W 90.40(11) . 2_765 ?
O1W Ni2 O1W 180.0 . 2_765 ?
O2W Ni2 N5 92.42(14) 2_765 . ?
O2W Ni2 N5 87.58(14) . . ?
O1W Ni2 N5 93.04(13) . . ?
O1W Ni2 N5 86.96(13) 2_765 . ?
O2W Ni2 N5 87.58(14) 2_765 2_765 ?
O2W Ni2 N5 92.42(14) . 2_765 ?
O1W Ni2 N5 86.96(13) . 2_765 ?
O1W Ni2 N5 93.04(13) 2_765 2_765 ?
N5 Ni2 N5 180.00(17) . 2_765 ?
O1 C1 O2 125.1(3) . . ?
O1 C1 C2 117.4(3) . . ?
O2 C1 C2 117.4(3) . . ?
C3 C2 C7 119.6(3) . . ?
C3 C2 C1 115.9(3) . . ?
C7 C2 C1 124.5(3) . . ?
C4 C3 C2 121.2(4) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C5 C4 C3 119.8(3) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 119.9(4) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C5 C6 C7 121.7(4) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C6 C7 C2 117.7(3) . . ?
C6 C7 C8 119.1(3) . . ?
C2 C7 C8 123.1(3) . . ?
C9 C8 C13 117.2(3) . . ?
C9 C8 C7 122.1(3) . . ?
C13 C8 C7 120.7(3) . . ?
C10 C9 C8 120.8(3) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C11 C10 C9 121.7(3) . . ?
C11 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
C12 C11 C10 117.6(3) . . ?
C12 C11 C14 122.1(3) . . ?
C10 C11 C14 120.3(3) . . ?
C11 C12 C13 121.6(3) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.2 . . ?
C12 C13 C8 121.1(3) . . ?
C12 C13 H13 119.5 . . ?
C8 C13 H13 119.5 . . ?
N1 C14 C11 115.8(3) . . ?
N1 C14 H14A 108.3 . . ?
C11 C14 H14A 108.3 . . ?
N1 C14 H14B 108.3 . . ?
C11 C14 H14B 108.3 . . ?
H14A C14 H14B 107.4 . . ?
N1 C15 C16 114.0(3) . . ?
N1 C15 H15A 108.8 . . ?
C16 C15 H15A 108.8 . . ?
N1 C15 H15B 108.8 . . ?
C16 C15 H15B 108.8 . . ?
H15A C15 H15B 107.6 . . ?
O5 C16 O6 124.9(3) . . ?
O5 C16 C15 117.6(3) . . ?
O6 C16 C15 117.5(3) . . ?
C18 C17 N1 111.9(12) . . ?
C18 C17 H17A 109.2 . . ?
N1 C17 H17A 109.2 . . ?
C18 C17 H17B 109.2 . . ?
N1 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
N1 C17' C18 113.2(5) . . ?
N1 C17' H17C 108.9 . . ?
C18 C17' H17C 108.9 . . ?
N1 C17' H17D 108.9 . . ?
C18 C17' H17D 108.9 . . ?
H17C C17' H17D 107.8 . . ?
O3 C18 O4 125.7(3) . . ?
O3 C18 C17 116.6(7) . . ?
O4 C18 C17 114.6(8) . . ?
O3 C18 C17' 115.5(4) . . ?
O4 C18 C17' 117.5(4) . . ?
C17 C18 C17' 30.5(8) . . ?
N3 C19 N2 114.1(4) . . ?
N3 C19 H19 122.9 . . ?
N2 C19 H19 122.9 . . ?
N4 C20 N2 110.4(3) . . ?
N4 C20 H20 124.8 . . ?
N2 C20 H20 124.8 . . ?
N4 C21 C22 114.1(3) . . ?
N4 C21 H21A 108.7 . . ?
C22 C21 H21A 108.7 . . ?
N4 C21 H21B 108.7 . . ?
C22 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
C23 C22 C24 118.5(3) . . ?
C23 C22 C21 124.0(3) . . ?
C24 C22 C21 117.5(3) . . ?
C24 C23 C22 120.5(3) 2 . ?
C24 C23 H23 119.8 2 . ?
C22 C23 H23 119.8 . . ?
C23 C24 C22 121.0(3) 2 . ?
C23 C24 H24 119.5 2 . ?
C22 C24 H24 119.5 . . ?
N7 C25 N5 111.0(4) . . ?
N7 C25 H25 124.5 . . ?
N5 C25 H25 124.5 . . ?
N6 C26 N5 114.1(4) . . ?
N6 C26 H26 123.0 . . ?
N5 C26 H26 123.0 . . ?
N7 C27 C28 114.1(3) . . ?
N7 C27 H27A 108.7 . . ?
C28 C27 H27A 108.7 . . ?
N7 C27 H27B 108.7 . . ?
C28 C27 H27B 108.7 . . ?
H27A C27 H27B 107.6 . . ?
C30 C28 C29 119.7(3) . . ?
C30 C28 C27 119.3(4) . . ?
C29 C28 C27 121.0(4) . . ?
C30 C29 C28 119.7(4) 2_675 . ?
C30 C29 H29 120.2 2_675 . ?
C28 C29 H29 120.2 . . ?
C28 C30 C29 120.6(4) . 2_675 ?
C28 C30 H30 119.7 . . ?
C29 C30 H30 119.7 2_675 . ?
C14 N1 C15 110.5(3) . . ?
C14 N1 C17' 117.8(6) . . ?
C15 N1 C17' 103.1(6) . . ?
C14 N1 C17 93.8(11) . . ?
C15 N1 C17 132.5(13) . . ?
C17' N1 C17 30.8(8) . . ?
C14 N1 Ni1 114.96(18) . . ?
C15 N1 Ni1 102.55(19) . . ?
C17' N1 Ni1 106.2(3) . . ?
C17 N1 Ni1 102.8(7) . . ?
C20 N2 C19 103.0(3) . . ?
C20 N2 Ni1 126.7(2) . . ?
C19 N2 Ni1 130.3(3) . . ?
C19 N3 N4 102.7(3) . . ?
C20 N4 N3 109.8(3) . . ?
C20 N4 C21 129.0(4) . . ?
N3 N4 C21 121.2(3) . . ?
C25 N5 C26 102.6(4) . . ?
C25 N5 Ni2 123.3(3) . . ?
C26 N5 Ni2 133.9(3) . . ?
C26 N6 N7 102.3(4) . . ?
C25 N7 N6 110.0(4) . . ?
C25 N7 C27 128.9(4) . . ?
N6 N7 C27 121.2(4) . . ?
C1 O2 Ni1 127.7(2) . 2_666 ?
C18 O4 Ni1 115.7(2) . . ?
C16 O5 Ni1 113.8(2) . . ?
Ni2 O1W H1A 114(3) . . ?
Ni2 O1W H1B 113(3) . . ?
H1A O1W H1B 111(4) . . ?
Ni2 O2W H2A 115(4) . . ?
Ni2 O2W H2B 127(3) . . ?
H2A O2W H2B 109(5) . . ?
Ni1 O3W H3A 102(3) . . ?
Ni1 O3W H3B 127(3) . . ?
H3A O3W H3B 106(4) . . ?
H4A O4W H4B 100(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
O1 C1 C2 C3 73.8(4) . . . . ?
O2 C1 C2 C3 -103.2(3) . . . . ?
O1 C1 C2 C7 -108.7(4) . . . . ?
O2 C1 C2 C7 74.3(4) . . . . ?
C7 C2 C3 C4 -0.1(5) . . . . ?
C1 C2 C3 C4 177.4(3) . . . . ?
C2 C3 C4 C5 1.0(6) . . . . ?
C3 C4 C5 C6 -0.5(6) . . . . ?
C4 C5 C6 C7 -1.0(5) . . . . ?
C5 C6 C7 C2 1.9(5) . . . . ?
C5 C6 C7 C8 -177.6(3) . . . . ?
C3 C2 C7 C6 -1.3(4) . . . . ?
C1 C2 C7 C6 -178.6(3) . . . . ?
C3 C2 C7 C8 178.2(3) . . . . ?
C1 C2 C7 C8 0.8(5) . . . . ?
C6 C7 C8 C9 -141.8(3) . . . . ?
C2 C7 C8 C9 38.7(5) . . . . ?
C6 C7 C8 C13 39.5(4) . . . . ?
C2 C7 C8 C13 -140.0(3) . . . . ?
C13 C8 C9 C10 0.9(5) . . . . ?
C7 C8 C9 C10 -177.9(3) . . . . ?
C8 C9 C10 C11 -1.3(5) . . . . ?
C9 C10 C11 C12 0.8(5) . . . . ?
C9 C10 C11 C14 -178.5(3) . . . . ?
C10 C11 C12 C13 0.0(5) . . . . ?
C14 C11 C12 C13 179.3(3) . . . . ?
C11 C12 C13 C8 -0.3(5) . . . . ?
C9 C8 C13 C12 -0.1(5) . . . . ?
C7 C8 C13 C12 178.7(3) . . . . ?
C12 C11 C14 N1 -88.4(4) . . . . ?
C10 C11 C14 N1 90.8(4) . . . . ?
N1 C15 C16 O5 -19.9(5) . . . . ?
N1 C15 C16 O6 162.8(3) . . . . ?
N1 C17 C18 O3 -159.6(13) . . . . ?
N1 C17 C18 O4 39(2) . . . . ?
N1 C17 C18 C17' -63.9(18) . . . . ?
N1 C17' C18 O3 167.1(7) . . . . ?
N1 C17' C18 O4 -25.0(12) . . . . ?
N1 C17' C18 C17 67.4(14) . . . . ?
N4 C21 C22 C23 4.7(6) . . . . ?
N4 C21 C22 C24 -177.5(3) . . . . ?
C24 C22 C23 C24 0.4(6) . . . 2 ?
C21 C22 C23 C24 178.2(4) . . . 2 ?
C23 C22 C24 C23 -0.4(6) . . . 2 ?
C21 C22 C24 C23 -178.4(4) . . . 2 ?
N7 C27 C28 C30 120.1(4) . . . . ?
N7 C27 C28 C29 -61.2(6) . . . . ?
C30 C28 C29 C30 -0.4(7) . . . 2_675 ?
C27 C28 C29 C30 -179.0(4) . . . 2_675 ?
C29 C28 C30 C29 0.4(7) . . . 2_675 ?
C27 C28 C30 C29 179.0(4) . . . 2_675 ?
C11 C14 N1 C15 63.6(4) . . . . ?
C11 C14 N1 C17' -54.5(7) . . . . ?
C11 C14 N1 C17 -74.9(11) . . . . ?
C11 C14 N1 Ni1 179.1(3) . . . . ?
C16 C15 N1 C14 155.7(3) . . . . ?
C16 C15 N1 C17' -77.5(5) . . . . ?
C16 C15 N1 C17 -88.1(10) . . . . ?
C16 C15 N1 Ni1 32.7(4) . . . . ?
C18 C17' N1 C14 -108.9(8) . . . . ?
C18 C17' N1 C15 129.1(9) . . . . ?
C18 C17' N1 C17 -66.2(15) . . . . ?
C18 C17' N1 Ni1 21.6(11) . . . . ?
C18 C17 N1 C14 -151.6(19) . . . . ?
C18 C17 N1 C15 85.8(18) . . . . ?
C18 C17 N1 C17' 65.4(19) . . . . ?
C18 C17 N1 Ni1 -35(2) . . . . ?
O4 Ni1 N1 C14 120.2(3) . . . . ?
O5 Ni1 N1 C14 -147.5(3) . . . . ?
N2 Ni1 N1 C14 -169.5(5) . . . . ?
O3W Ni1 N1 C14 -57.3(3) . . . . ?
O2 Ni1 N1 C14 33.9(3) 2_666 . . . ?
O4 Ni1 N1 C15 -119.8(2) . . . . ?
O5 Ni1 N1 C15 -27.5(2) . . . . ?
N2 Ni1 N1 C15 -49.4(6) . . . . ?
O3W Ni1 N1 C15 62.7(2) . . . . ?
O2 Ni1 N1 C15 153.9(2) 2_666 . . . ?
O4 Ni1 N1 C17' -12.0(7) . . . . ?
O5 Ni1 N1 C17' 80.3(7) . . . . ?
N2 Ni1 N1 C17' 58.4(9) . . . . ?
O3W Ni1 N1 C17' 170.6(7) . . . . ?
O2 Ni1 N1 C17' -98.2(7) 2_666 . . . ?
O4 Ni1 N1 C17 19.7(13) . . . . ?
O5 Ni1 N1 C17 112.0(13) . . . . ?
N2 Ni1 N1 C17 90.1(15) . . . . ?
O3W Ni1 N1 C17 -157.7(13) . . . . ?
O2 Ni1 N1 C17 -66.6(13) 2_666 . . . ?
N4 C20 N2 C19 -0.2(4) . . . . ?
N4 C20 N2 Ni1 -178.5(2) . . . . ?
N3 C19 N2 C20 -0.2(4) . . . . ?
N3 C19 N2 Ni1 178.1(2) . . . . ?
O4 Ni1 N2 C20 118.6(3) . . . . ?
O5 Ni1 N2 C20 27.6(3) . . . . ?
O3W Ni1 N2 C20 -62.5(3) . . . . ?
O2 Ni1 N2 C20 -153.8(3) 2_666 . . . ?
N1 Ni1 N2 C20 49.3(7) . . . . ?
O4 Ni1 N2 C19 -59.2(3) . . . . ?
O5 Ni1 N2 C19 -150.2(3) . . . . ?
O3W Ni1 N2 C19 119.7(3) . . . . ?
O2 Ni1 N2 C19 28.4(3) 2_666 . . . ?
N1 Ni1 N2 C19 -128.6(5) . . . . ?
N2 C19 N3 N4 0.4(4) . . . . ?
N2 C20 N4 N3 0.5(4) . . . . ?
N2 C20 N4 C21 180.0(3) . . . . ?
C19 N3 N4 C20 -0.5(4) . . . . ?
C19 N3 N4 C21 179.9(3) . . . . ?
C22 C21 N4 C20 -95.8(5) . . . . ?
C22 C21 N4 N3 83.6(4) . . . . ?
N7 C25 N5 C26 -0.3(4) . . . . ?
N7 C25 N5 Ni2 174.9(2) . . . . ?
N6 C26 N5 C25 0.1(4) . . . . ?
N6 C26 N5 Ni2 -174.3(2) . . . . ?
O2W Ni2 N5 C25 -135.7(3) 2_765 . . . ?
O2W Ni2 N5 C25 44.3(3) . . . . ?
O1W Ni2 N5 C25 133.8(3) . . . . ?
O1W Ni2 N5 C25 -46.2(3) 2_765 . . . ?
N5 Ni2 N5 C25 -7(100) 2_765 . . . ?
O2W Ni2 N5 C26 37.8(3) 2_765 . . . ?
O2W Ni2 N5 C26 -142.2(3) . . . . ?
O1W Ni2 N5 C26 -52.7(3) . . . . ?
O1W Ni2 N5 C26 127.3(3) 2_765 . . . ?
N5 Ni2 N5 C26 167(100) 2_765 . . . ?
N5 C26 N6 N7 0.1(4) . . . . ?
N5 C25 N7 N6 0.4(4) . . . . ?
N5 C25 N7 C27 -178.4(3) . . . . ?
C26 N6 N7 C25 -0.2(4) . . . . ?
C26 N6 N7 C27 178.6(3) . . . . ?
C28 C27 N7 C25 -100.1(5) . . . . ?
C28 C27 N7 N6 81.2(5) . . . . ?
O1 C1 O2 Ni1 -17.9(5) . . . 2_666 ?
C2 C1 O2 Ni1 158.8(2) . . . 2_666 ?
O3 C18 O4 Ni1 -179.5(3) . . . . ?
C17 C18 O4 Ni1 -20.1(14) . . . . ?
C17' C18 O4 Ni1 13.8(8) . . . . ?
O5 Ni1 O4 C18 -81.6(2) . . . . ?
N2 Ni1 O4 C18 -170.2(2) . . . . ?
O3W Ni1 O4 C18 17.4(9) . . . . ?
O2 Ni1 O4 C18 99.1(2) 2_666 . . . ?
N1 Ni1 O4 C18 -0.6(2) . . . . ?
O6 C16 O5 Ni1 170.6(3) . . . . ?
C15 C16 O5 Ni1 -6.5(4) . . . . ?
O4 Ni1 O5 C16 102.5(3) . . . . ?
N2 Ni1 O5 C16 -163.8(3) . . . . ?
O3W Ni1 O5 C16 -69.2(3) . . . . ?
O2 Ni1 O5 C16 133(3) 2_666 . . . ?
N1 Ni1 O5 C16 20.3(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
O3W H3B O4W 0.85(4) 1.89(4) 2.732(4) 171(4) .
O1W H1A O3 0.96(5) 1.73(5) 2.627(4) 153(4) 1_655
O1W H1B O6 0.81(5) 1.92(5) 2.705(4) 163(5) 2_765
O2W H2B O4 0.87(5) 1.84(5) 2.659(3) 156(5) 2_665
O4W H4A N3 0.81(5) 2.16(5) 2.954(4) 165(5) 1_655
O4W H4B O1 0.83(5) 1.95(5) 2.785(4) 175(5) 1_545

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.056
#=========================END
data_Compound-7

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H68 N14 O20 Zn3'
_chemical_formula_sum            'C60 H68 N14 O20 Zn3'
_chemical_formula_weight         1501.39

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_hall  '-P 1 '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2610(5)
_cell_length_b                   12.7610(7)
_cell_length_c                   15.7500(11)
_cell_angle_alpha                76.617(5)
_cell_angle_beta                 85.085(5)
_cell_angle_gamma                86.823(5)
_cell_volume                     1608.23(17)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3718
_cell_measurement_theta_min      2.9631
_cell_measurement_theta_max      29.1728

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             776
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7542
_exptl_absorpt_correction_T_max  0.8410
_exptl_absorpt_process_details   
;
CrysAlis (Oxford Diffraction, 2006)
;
_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  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10068
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.97
_diffrn_reflns_theta_max         25.02
_reflns_number_total             5652
_reflns_number_gt                4427
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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.

For C17 and C17' atoms, some anisotropic displacement ellipsoids were 
rather elongated which led us to use the ISOR restraints.

;

_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)+(0.0392P)²+0.8042P] 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         5652
_refine_ls_number_parameters     472
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_ref         0.0972
_refine_ls_wR_factor_gt          0.0882
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.027
_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
Zn1 Zn -0.16399(4) 0.26509(3) 0.30641(2) 0.03611(12) Uani 1 1 d . . .
Zn2 Zn 0.5000 0.5000 0.0000 0.04514(17) Uani 1 2 d S . .
C1 C 0.3340(4) 0.8010(2) 0.5125(2) 0.0364(7) Uani 1 1 d . . .
C2 C 0.4875(4) 0.7932(2) 0.45491(19) 0.0347(7) Uani 1 1 d . . .
C3 C 0.6077(5) 0.8649(2) 0.4563(2) 0.0468(9) Uani 1 1 d . . .
H3 H 0.5875 0.9161 0.4898 0.056 Uiso 1 1 calc R . .
C4 C 0.7556(5) 0.8622(3) 0.4095(3) 0.0536(9) Uani 1 1 d . . .
H4 H 0.8349 0.9100 0.4122 0.064 Uiso 1 1 calc R . .
C5 C 0.7848(4) 0.7886(3) 0.3589(2) 0.0532(9) Uani 1 1 d . . .
H5 H 0.8843 0.7863 0.3268 0.064 Uiso 1 1 calc R . .
C6 C 0.6655(4) 0.7168(2) 0.3553(2) 0.0422(8) Uani 1 1 d . . .
H6 H 0.6863 0.6681 0.3196 0.051 Uiso 1 1 calc R . .
C7 C 0.5165(4) 0.7161(2) 0.40357(19) 0.0340(7) Uani 1 1 d . . .
C8 C 0.3959(4) 0.6357(2) 0.39981(19) 0.0339(7) Uani 1 1 d . . .
C9 C 0.4457(4) 0.5296(2) 0.3992(2) 0.0387(8) Uani 1 1 d . . .
H9 H 0.5557 0.5097 0.4003 0.046 Uiso 1 1 calc R . .
C10 C 0.3340(5) 0.4534(2) 0.3971(2) 0.0437(9) Uani 1 1 d . . .
H10 H 0.3710 0.3834 0.3963 0.052 Uiso 1 1 calc R . .
C11 C 0.1689(4) 0.4785(2) 0.3961(2) 0.0390(8) Uani 1 1 d . . .
C12 C 0.1196(4) 0.5836(3) 0.3977(2) 0.0459(8) Uani 1 1 d . . .
H12 H 0.0093 0.6027 0.3983 0.055 Uiso 1 1 calc R . .
C13 C 0.2299(4) 0.6609(2) 0.3986(2) 0.0408(8) Uani 1 1 d . . .
H13 H 0.1924 0.7311 0.3982 0.049 Uiso 1 1 calc R . .
C14 C 0.0461(5) 0.3967(3) 0.3923(2) 0.0483(9) Uani 1 1 d . . .
H14A H 0.0823 0.3271 0.4261 0.058 Uiso 1 1 calc R . .
H14B H -0.0564 0.4164 0.4204 0.058 Uiso 1 1 calc R . .
C15 C 0.1631(5) 0.3429(3) 0.2615(2) 0.0565(10) Uani 1 1 d . . .
H15A H 0.2190 0.2906 0.3052 0.068 Uiso 1 1 calc R . .
H15B H 0.2355 0.4016 0.2376 0.068 Uiso 1 1 calc R . .
C16 C 0.1262(4) 0.2898(2) 0.1883(2) 0.0404(8) Uani 1 1 d . . .
C17 C -0.0358(6) 0.4847(3) 0.2414(3) 0.0442(11) Uani 0.80 1 d PU . .
C17' C -0.082(3) 0.4971(15) 0.2854(14) 0.047(5) Uani 0.20 1 d PU . .
C18 C -0.2163(4) 0.4899(3) 0.2252(2) 0.0407(8) Uani 1 1 d . . .
C19 C -0.4731(4) 0.1389(3) 0.2941(2) 0.0481(9) Uani 1 1 d U . .
H19 H -0.5384 0.1789 0.3270 0.058 Uiso 1 1 calc R . .
C20 C -0.2695(4) 0.0829(3) 0.2275(2) 0.0463(8) Uani 1 1 d . . .
H20 H -0.1650 0.0731 0.2029 0.056 Uiso 1 1 calc R . .
C21 C -0.4028(5) -0.0615(3) 0.1774(2) 0.0590(11) Uani 1 1 d . . .
H21A H -0.4784 -0.1135 0.2115 0.071 Uiso 1 1 calc R . .
H21B H -0.2966 -0.0977 0.1756 0.071 Uiso 1 1 calc R . .
C22 C -0.4549(4) -0.0266(2) 0.0857(2) 0.0418(8) Uani 1 1 d . . .
C23 C -0.4823(5) 0.0795(3) 0.0435(2) 0.0519(9) Uani 1 1 d . . .
H23 H -0.4708 0.1339 0.0727 0.062 Uiso 1 1 calc R . .
C24 C -0.4736(5) -0.1060(3) 0.0416(2) 0.0484(9) Uani 1 1 d . . .
H24 H -0.4564 -0.1780 0.0693 0.058 Uiso 1 1 calc R . .
C25 C 0.2070(5) 0.6544(3) 0.0206(3) 0.0606(10) Uani 1 1 d . . .
H25 H 0.1792 0.6506 -0.0346 0.073 Uiso 1 1 calc R . .
C26 C 0.3276(5) 0.6356(3) 0.1353(3) 0.0582(10) Uani 1 1 d . . .
H26 H 0.4046 0.6147 0.1763 0.070 Uiso 1 1 calc R . .
C27 C -0.0321(5) 0.7685(3) 0.0568(3) 0.0672(12) Uani 1 1 d . . .
H27A H -0.1024 0.7533 0.1104 0.081 Uiso 1 1 calc R . .
H27B H -0.0848 0.7441 0.0125 0.081 Uiso 1 1 calc R . .
C28 C -0.0121(4) 0.8892(3) 0.0275(3) 0.0486(9) Uani 1 1 d . . .
C29 C 0.0542(5) 0.9467(3) 0.0799(3) 0.0573(10) Uani 1 1 d . . .
H29 H 0.0906 0.9110 0.1337 0.069 Uiso 1 1 calc R . .
C30 C -0.0660(4) 0.9426(3) -0.0520(3) 0.0531(9) Uani 1 1 d . . .
H30 H -0.1107 0.9041 -0.0872 0.064 Uiso 1 1 calc R . .
N1 N 0.0165(3) 0.38477(18) 0.30356(16) 0.0343(6) Uani 1 1 d . . .
N2 N -0.3137(3) 0.1556(2) 0.27325(17) 0.0399(6) Uani 1 1 d U . .
N3 N -0.5281(4) 0.0614(2) 0.26408(19) 0.0517(7) Uani 1 1 d . . .
N4 N -0.3946(4) 0.0264(2) 0.22199(17) 0.0424(7) Uani 1 1 d . . .
N5 N 0.3387(4) 0.6061(2) 0.0582(2) 0.0568(8) Uani 1 1 d . . .
N6 N 0.1971(4) 0.6971(2) 0.1473(2) 0.0630(9) Uani 1 1 d . . .
N7 N 0.1220(4) 0.7080(2) 0.0718(2) 0.0561(8) Uani 1 1 d . . .
O1 O 0.2404(3) 0.88159(19) 0.49019(16) 0.0600(7) Uani 1 1 d . . .
O2 O 0.3133(3) 0.72834(16) 0.58113(13) 0.0404(5) Uani 1 1 d . . .
O3 O -0.2708(3) 0.57955(18) 0.18644(15) 0.0538(6) Uani 1 1 d . . .
O4 O -0.2899(3) 0.40336(17) 0.24179(15) 0.0494(6) Uani 1 1 d . . .
O5 O -0.0122(3) 0.25659(19) 0.18990(15) 0.0541(6) Uani 1 1 d . . .
O6 O 0.2412(3) 0.28079(19) 0.13296(15) 0.0533(6) Uani 1 1 d . . .
O1W O -0.0107(3) 0.14672(19) 0.38125(18) 0.0491(6) Uani 1 1 d . . .
H1A H -0.065(5) 0.122(3) 0.429(3) 0.074 Uiso 1 1 d . . .
H1B H 0.035(5) 0.097(3) 0.364(3) 0.074 Uiso 1 1 d . . .
O2W O 0.5157(3) 0.3876(2) 0.11874(18) 0.0599(8) Uani 1 1 d . . .
H2A H 0.444(6) 0.352(4) 0.128(3) 0.090 Uiso 1 1 d . . .
H2B H 0.554(6) 0.397(4) 0.161(3) 0.090 Uiso 1 1 d . . .
O3W O 0.2903(4) 0.4276(2) -0.02158(19) 0.0610(8) Uani 1 1 d . . .
H3A H 0.264(6) 0.376(4) 0.018(3) 0.092 Uiso 1 1 d . . .
H3B H 0.353(6) 0.388(4) -0.048(3) 0.092 Uiso 1 1 d . . .
O4W O 0.1464(3) -0.0219(2) 0.32357(19) 0.0618(7) Uani 1 1 d D . .
H4A H 0.240(3) 0.005(3) 0.297(3) 0.093 Uiso 1 1 d D . .
H4B H 0.186(5) -0.052(3) 0.3750(16) 0.093 Uiso 1 1 d D . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
Zn1 O2 2.085(2) 2_566 ?
Zn1 O4 2.092(2) . ?
Zn1 N2 2.096(3) . ?
Zn1 O1W 2.120(2) . ?
Zn1 O5 2.153(2) . ?
Zn1 N1 2.183(2) . ?
Zn2 O2W 2.086(2) . ?
Zn2 O2W 2.086(2) 2_665 ?
Zn2 O3W 2.096(3) . ?
Zn2 O3W 2.096(3) 2_665 ?
Zn2 N5 2.148(3) . ?
Zn2 N5 2.148(3) 2_665 ?
C1 O1 1.253(4) . ?
C1 O2 1.257(4) . ?
C1 C2 1.507(4) . ?
C2 C3 1.392(4) . ?
C2 C7 1.410(4) . ?
C3 C4 1.375(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.365(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.396(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.390(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.484(4) . ?
C8 C13 1.392(4) . ?
C8 C9 1.396(4) . ?
C9 C10 1.385(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.384(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.386(4) . ?
C11 C14 1.509(4) . ?
C12 C13 1.382(4) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 N1 1.482(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N1 1.465(4) . ?
C15 C16 1.525(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 O5 1.238(4) . ?
C16 O6 1.252(4) . ?
C17 C17' 0.806(19) . ?
C17 N1 1.485(5) . ?
C17 C18 1.530(6) . ?
C17' C18 1.542(19) . ?
C17' N1 1.586(17) . ?
C18 O3 1.245(4) . ?
C18 O4 1.253(4) . ?
C19 N3 1.308(4) . ?
C19 N2 1.345(4) . ?
C19 H19 0.9300 . ?
C20 N4 1.313(4) . ?
C20 N2 1.319(4) . ?
C20 H20 0.9300 . ?
C21 N4 1.462(4) . ?
C21 C22 1.502(5) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C24 1.376(4) . ?
C22 C23 1.379(4) . ?
C23 C24 1.379(5) 2_455 ?
C23 H23 0.9300 . ?
C24 C23 1.379(5) 2_455 ?
C24 H24 0.9300 . ?
C25 N7 1.310(5) . ?
C25 N5 1.335(5) . ?
C25 H25 0.9300 . ?
C26 N6 1.324(5) . ?
C26 N5 1.347(5) . ?
C26 H26 0.9300 . ?
C27 N7 1.459(5) . ?
C27 C28 1.516(5) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C30 1.378(5) . ?
C28 C29 1.386(5) . ?
C29 C30 1.385(5) 2_575 ?
C29 H29 0.9300 . ?
C30 C29 1.385(5) 2_575 ?
C30 H30 0.9300 . ?
N3 N4 1.346(4) . ?
N6 N7 1.363(4) . ?
O2 Zn1 2.085(2) 2_566 ?
O1W H1A 0.85(4) . ?
O1W H1B 0.81(4) . ?
O2W H2A 0.75(5) . ?
O2W H2B 0.80(5) . ?
O3W H3A 0.82(5) . ?
O3W H3B 0.86(5) . ?
O4W H4A 0.895(10) . ?
O4W H4B 0.895(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Zn1 O4 87.95(9) 2_566 . ?
O2 Zn1 N2 91.86(10) 2_566 . ?
O4 Zn1 N2 95.46(9) . . ?
O2 Zn1 O1W 90.28(10) 2_566 . ?
O4 Zn1 O1W 168.68(9) . . ?
N2 Zn1 O1W 95.77(10) . . ?
O2 Zn1 O5 179.13(8) 2_566 . ?
O4 Zn1 O5 92.14(10) . . ?
N2 Zn1 O5 87.28(9) . . ?
O1W Zn1 O5 89.80(10) . . ?
O2 Zn1 N1 103.11(9) 2_566 . ?
O4 Zn1 N1 80.63(9) . . ?
N2 Zn1 N1 164.32(10) . . ?
O1W Zn1 N1 88.90(9) . . ?
O5 Zn1 N1 77.76(9) . . ?
O2W Zn2 O2W 180.00(17) . 2_665 ?
O2W Zn2 O3W 89.63(11) . . ?
O2W Zn2 O3W 90.37(11) 2_665 . ?
O2W Zn2 O3W 90.37(11) . 2_665 ?
O2W Zn2 O3W 89.63(11) 2_665 2_665 ?
O3W Zn2 O3W 180.00(13) . 2_665 ?
O2W Zn2 N5 92.65(13) . . ?
O2W Zn2 N5 87.35(13) 2_665 . ?
O3W Zn2 N5 86.39(12) . . ?
O3W Zn2 N5 93.61(12) 2_665 . ?
O2W Zn2 N5 87.35(13) . 2_665 ?
O2W Zn2 N5 92.65(13) 2_665 2_665 ?
O3W Zn2 N5 93.61(12) . 2_665 ?
O3W Zn2 N5 86.39(12) 2_665 2_665 ?
N5 Zn2 N5 180.00(15) . 2_665 ?
O1 C1 O2 125.1(3) . . ?
O1 C1 C2 117.5(3) . . ?
O2 C1 C2 117.3(3) . . ?
C3 C2 C7 119.5(3) . . ?
C3 C2 C1 116.6(3) . . ?
C7 C2 C1 123.9(3) . . ?
C4 C3 C2 121.8(3) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 120.1(3) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 121.8(3) . . ?
C7 C6 H6 119.1 . . ?
C5 C6 H6 119.1 . . ?
C6 C7 C2 117.5(3) . . ?
C6 C7 C8 119.7(3) . . ?
C2 C7 C8 122.8(3) . . ?
C13 C8 C9 117.1(3) . . ?
C13 C8 C7 122.4(3) . . ?
C9 C8 C7 120.5(3) . . ?
C10 C9 C8 121.0(3) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C11 C10 C9 121.8(3) . . ?
C11 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
C10 C11 C12 117.0(3) . . ?
C10 C11 C14 122.4(3) . . ?
C12 C11 C14 120.6(3) . . ?
C13 C12 C11 121.8(3) . . ?
C13 C12 H12 119.1 . . ?
C11 C12 H12 119.1 . . ?
C12 C13 C8 121.2(3) . . ?
C12 C13 H13 119.4 . . ?
C8 C13 H13 119.4 . . ?
N1 C14 C11 115.9(3) . . ?
N1 C14 H14A 108.3 . . ?
C11 C14 H14A 108.3 . . ?
N1 C14 H14B 108.3 . . ?
C11 C14 H14B 108.3 . . ?
H14A C14 H14B 107.4 . . ?
N1 C15 C16 112.8(3) . . ?
N1 C15 H15A 109.0 . . ?
C16 C15 H15A 109.0 . . ?
N1 C15 H15B 109.0 . . ?
C16 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
O5 C16 O6 125.6(3) . . ?
O5 C16 C15 117.7(3) . . ?
O6 C16 C15 116.6(3) . . ?
C17' C17 N1 81.9(14) . . ?
C17' C17 C18 75.6(15) . . ?
N1 C17 C18 113.8(3) . . ?
C17 C17' C18 73.9(15) . . ?
C17 C17' N1 67.9(12) . . ?
C18 C17' N1 107.6(12) . . ?
O3 C18 O4 125.8(3) . . ?
O3 C18 C17 115.4(3) . . ?
O4 C18 C17 118.1(3) . . ?
O3 C18 C17' 113.4(8) . . ?
O4 C18 C17' 116.5(8) . . ?
C17 C18 C17' 30.4(7) . . ?
N3 C19 N2 114.1(3) . . ?
N3 C19 H19 122.9 . . ?
N2 C19 H19 122.9 . . ?
N4 C20 N2 110.0(3) . . ?
N4 C20 H20 125.0 . . ?
N2 C20 H20 125.0 . . ?
N4 C21 C22 114.3(3) . . ?
N4 C21 H21A 108.7 . . ?
C22 C21 H21A 108.7 . . ?
N4 C21 H21B 108.7 . . ?
C22 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
C24 C22 C23 118.8(3) . . ?
C24 C22 C21 117.4(3) . . ?
C23 C22 C21 123.9(3) . . ?
C24 C23 C22 120.8(3) 2_455 . ?
C24 C23 H23 119.6 2_455 . ?
C22 C23 H23 119.6 . . ?
C22 C24 C23 120.4(3) . 2_455 ?
C22 C24 H24 119.8 . . ?
C23 C24 H24 119.8 2_455 . ?
N7 C25 N5 110.9(4) . . ?
N7 C25 H25 124.5 . . ?
N5 C25 H25 124.5 . . ?
N6 C26 N5 113.8(4) . . ?
N6 C26 H26 123.1 . . ?
N5 C26 H26 123.1 . . ?
N7 C27 C28 113.0(3) . . ?
N7 C27 H27A 109.0 . . ?
C28 C27 H27A 109.0 . . ?
N7 C27 H27B 109.0 . . ?
C28 C27 H27B 109.0 . . ?
H27A C27 H27B 107.8 . . ?
C30 C28 C29 119.7(3) . . ?
C30 C28 C27 118.7(3) . . ?
C29 C28 C27 121.6(3) . . ?
C30 C29 C28 119.9(3) 2_575 . ?
C30 C29 H29 120.1 2_575 . ?
C28 C29 H29 120.1 . . ?
C28 C30 C29 120.4(3) . 2_575 ?
C28 C30 H30 119.8 . . ?
C29 C30 H30 119.8 2_575 . ?
C15 N1 C14 110.9(3) . . ?
C15 N1 C17 106.2(3) . . ?
C14 N1 C17 115.9(3) . . ?
C15 N1 C17' 133.8(9) . . ?
C14 N1 C17' 90.4(7) . . ?
C17 N1 C17' 30.2(7) . . ?
C15 N1 Zn1 103.73(19) . . ?
C14 N1 Zn1 112.49(19) . . ?
C17 N1 Zn1 106.7(2) . . ?
C17' N1 Zn1 104.9(8) . . ?
C20 N2 C19 103.0(3) . . ?
C20 N2 Zn1 126.9(2) . . ?
C19 N2 Zn1 130.0(2) . . ?
C19 N3 N4 102.7(3) . . ?
C20 N4 N3 110.1(3) . . ?
C20 N4 C21 129.1(3) . . ?
N3 N4 C21 120.8(3) . . ?
C25 N5 C26 102.8(3) . . ?
C25 N5 Zn2 122.6(3) . . ?
C26 N5 Zn2 134.4(3) . . ?
C26 N6 N7 103.0(3) . . ?
C25 N7 N6 109.3(3) . . ?
C25 N7 C27 128.3(4) . . ?
N6 N7 C27 122.4(4) . . ?
C1 O2 Zn1 127.9(2) . 2_566 ?
C18 O4 Zn1 116.8(2) . . ?
C16 O5 Zn1 114.3(2) . . ?
Zn1 O1W H1A 106(3) . . ?
Zn1 O1W H1B 124(3) . . ?
H1A O1W H1B 109(4) . . ?
Zn2 O2W H2A 111(4) . . ?
Zn2 O2W H2B 126(3) . . ?
H2A O2W H2B 115(5) . . ?
Zn2 O3W H3A 113(3) . . ?
Zn2 O3W H3B 87(3) . . ?
H3A O3W H3B 92(5) . . ?
H4A O4W H4B 96(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
O1 C1 C2 C3 71.3(4) . . . . ?
O2 C1 C2 C3 -105.9(3) . . . . ?
O1 C1 C2 C7 -111.0(3) . . . . ?
O2 C1 C2 C7 71.8(4) . . . . ?
C7 C2 C3 C4 -0.7(5) . . . . ?
C1 C2 C3 C4 177.1(3) . . . . ?
C2 C3 C4 C5 1.2(5) . . . . ?
C3 C4 C5 C6 -0.2(5) . . . . ?
C4 C5 C6 C7 -1.3(5) . . . . ?
C5 C6 C7 C2 1.9(4) . . . . ?
C5 C6 C7 C8 -177.9(3) . . . . ?
C3 C2 C7 C6 -0.9(4) . . . . ?
C1 C2 C7 C6 -178.4(3) . . . . ?
C3 C2 C7 C8 178.9(3) . . . . ?
C1 C2 C7 C8 1.3(4) . . . . ?
C6 C7 C8 C13 -141.1(3) . . . . ?
C2 C7 C8 C13 39.1(4) . . . . ?
C6 C7 C8 C9 40.2(4) . . . . ?
C2 C7 C8 C9 -139.5(3) . . . . ?
C13 C8 C9 C10 0.3(4) . . . . ?
C7 C8 C9 C10 179.0(3) . . . . ?
C8 C9 C10 C11 -0.5(5) . . . . ?
C9 C10 C11 C12 -0.3(5) . . . . ?
C9 C10 C11 C14 179.0(3) . . . . ?
C10 C11 C12 C13 1.3(5) . . . . ?
C14 C11 C12 C13 -178.0(3) . . . . ?
C11 C12 C13 C8 -1.5(5) . . . . ?
C9 C8 C13 C12 0.7(5) . . . . ?
C7 C8 C13 C12 -178.0(3) . . . . ?
C10 C11 C14 N1 -86.1(4) . . . . ?
C12 C11 C14 N1 93.1(4) . . . . ?
N1 C15 C16 O5 -22.6(5) . . . . ?
N1 C15 C16 O6 159.6(3) . . . . ?
N1 C17 C17' C18 -117.2(5) . . . . ?
C18 C17 C17' N1 117.2(5) . . . . ?
C17' C17 C18 O3 93.3(16) . . . . ?
N1 C17 C18 O3 167.5(3) . . . . ?
C17' C17 C18 O4 -95.0(16) . . . . ?
N1 C17 C18 O4 -20.8(5) . . . . ?
N1 C17 C18 C17' 74.2(16) . . . . ?
C17 C17' C18 O3 -100.8(13) . . . . ?
N1 C17' C18 O3 -160.7(9) . . . . ?
C17 C17' C18 O4 101.1(15) . . . . ?
N1 C17' C18 O4 41.2(15) . . . . ?
N1 C17' C18 C17 -59.9(11) . . . . ?
N4 C21 C22 C24 -176.6(3) . . . . ?
N4 C21 C22 C23 4.3(6) . . . . ?
C24 C22 C23 C24 -0.5(6) . . . 2_455 ?
C21 C22 C23 C24 178.5(4) . . . 2_455 ?
C23 C22 C24 C23 0.5(6) . . . 2_455 ?
C21 C22 C24 C23 -178.6(4) . . . 2_455 ?
N7 C27 C28 C30 120.7(4) . . . . ?
N7 C27 C28 C29 -61.3(5) . . . . ?
C30 C28 C29 C30 -0.1(6) . . . 2_575 ?
C27 C28 C29 C30 -178.1(3) . . . 2_575 ?
C29 C28 C30 C29 0.1(6) . . . 2_575 ?
C27 C28 C30 C29 178.2(3) . . . 2_575 ?
C16 C15 N1 C14 158.3(3) . . . . ?
C16 C15 N1 C17 -75.0(4) . . . . ?
C16 C15 N1 C17' -89.7(11) . . . . ?
C16 C15 N1 Zn1 37.3(3) . . . . ?
C11 C14 N1 C15 64.7(4) . . . . ?
C11 C14 N1 C17 -56.5(4) . . . . ?
C11 C14 N1 C17' -73.3(9) . . . . ?
C11 C14 N1 Zn1 -179.7(2) . . . . ?
C17' C17 N1 C15 -158.7(17) . . . . ?
C18 C17 N1 C15 131.0(4) . . . . ?
C17' C17 N1 C14 -35.0(18) . . . . ?
C18 C17 N1 C14 -105.4(4) . . . . ?
C18 C17 N1 C17' -70.3(17) . . . . ?
C17' C17 N1 Zn1 91.1(17) . . . . ?
C18 C17 N1 Zn1 20.8(4) . . . . ?
C17 C17' N1 C15 29(2) . . . . ?
C18 C17' N1 C15 92.6(14) . . . . ?
C17 C17' N1 C14 148.9(15) . . . . ?
C18 C17' N1 C14 -147.4(12) . . . . ?
C18 C17' N1 C17 63.7(13) . . . . ?
C17 C17' N1 Zn1 -97.7(15) . . . . ?
C18 C17' N1 Zn1 -33.9(14) . . . . ?
O2 Zn1 N1 C15 149.3(2) 2_566 . . . ?
O4 Zn1 N1 C15 -125.1(2) . . . . ?
N2 Zn1 N1 C15 -48.4(4) . . . . ?
O1W Zn1 N1 C15 59.2(2) . . . . ?
O5 Zn1 N1 C15 -30.8(2) . . . . ?
O2 Zn1 N1 C14 29.4(2) 2_566 . . . ?
O4 Zn1 N1 C14 115.1(2) . . . . ?
N2 Zn1 N1 C14 -168.3(3) . . . . ?
O1W Zn1 N1 C14 -60.6(2) . . . . ?
O5 Zn1 N1 C14 -150.7(2) . . . . ?
O2 Zn1 N1 C17 -98.8(3) 2_566 . . . ?
O4 Zn1 N1 C17 -13.1(3) . . . . ?
N2 Zn1 N1 C17 63.5(5) . . . . ?
O1W Zn1 N1 C17 171.2(3) . . . . ?
O5 Zn1 N1 C17 81.1(3) . . . . ?
O2 Zn1 N1 C17' -67.4(8) 2_566 . . . ?
O4 Zn1 N1 C17' 18.3(8) . . . . ?
N2 Zn1 N1 C17' 94.9(9) . . . . ?
O1W Zn1 N1 C17' -157.4(8) . . . . ?
O5 Zn1 N1 C17' 112.5(8) . . . . ?
N4 C20 N2 C19 -0.2(4) . . . . ?
N4 C20 N2 Zn1 178.0(2) . . . . ?
N3 C19 N2 C20 -0.1(4) . . . . ?
N3 C19 N2 Zn1 -178.3(2) . . . . ?
O2 Zn1 N2 C20 -152.4(3) 2_566 . . . ?
O4 Zn1 N2 C20 119.5(3) . . . . ?
O1W Zn1 N2 C20 -61.9(3) . . . . ?
O5 Zn1 N2 C20 27.6(3) . . . . ?
N1 Zn1 N2 C20 44.8(5) . . . . ?
O2 Zn1 N2 C19 25.4(3) 2_566 . . . ?
O4 Zn1 N2 C19 -62.7(3) . . . . ?
O1W Zn1 N2 C19 115.9(3) . . . . ?
O5 Zn1 N2 C19 -154.6(3) . . . . ?
N1 Zn1 N2 C19 -137.4(4) . . . . ?
N2 C19 N3 N4 0.4(4) . . . . ?
N2 C20 N4 N3 0.5(4) . . . . ?
N2 C20 N4 C21 179.5(3) . . . . ?
C19 N3 N4 C20 -0.6(4) . . . . ?
C19 N3 N4 C21 -179.6(3) . . . . ?
C22 C21 N4 C20 -93.7(4) . . . . ?
C22 C21 N4 N3 85.1(4) . . . . ?
N7 C25 N5 C26 -0.7(4) . . . . ?
N7 C25 N5 Zn2 175.0(2) . . . . ?
N6 C26 N5 C25 0.9(4) . . . . ?
N6 C26 N5 Zn2 -174.0(3) . . . . ?
O2W Zn2 N5 C25 -136.1(3) . . . . ?
O2W Zn2 N5 C25 43.9(3) 2_665 . . . ?
O3W Zn2 N5 C25 -46.6(3) . . . . ?
O3W Zn2 N5 C25 133.4(3) 2_665 . . . ?
N5 Zn2 N5 C25 16(100) 2_665 . . . ?
O2W Zn2 N5 C26 38.0(4) . . . . ?
O2W Zn2 N5 C26 -142.0(4) 2_665 . . . ?
O3W Zn2 N5 C26 127.5(4) . . . . ?
O3W Zn2 N5 C26 -52.5(4) 2_665 . . . ?
N5 Zn2 N5 C26 -170(100) 2_665 . . . ?
N5 C26 N6 N7 -0.8(4) . . . . ?
N5 C25 N7 N6 0.2(4) . . . . ?
N5 C25 N7 C27 -177.8(3) . . . . ?
C26 N6 N7 C25 0.3(4) . . . . ?
C26 N6 N7 C27 178.5(3) . . . . ?
C28 C27 N7 C25 -101.4(5) . . . . ?
C28 C27 N7 N6 80.8(5) . . . . ?
O1 C1 O2 Zn1 -18.3(5) . . . 2_566 ?
C2 C1 O2 Zn1 158.6(2) . . . 2_566 ?
O3 C18 O4 Zn1 179.1(3) . . . . ?
C17 C18 O4 Zn1 8.5(4) . . . . ?
C17' C18 O4 Zn1 -25.8(9) . . . . ?
O2 Zn1 O4 C18 106.7(2) 2_566 . . . ?
N2 Zn1 O4 C18 -161.7(2) . . . . ?
O1W Zn1 O4 C18 25.5(6) . . . . ?
O5 Zn1 O4 C18 -74.2(2) . . . . ?
N1 Zn1 O4 C18 3.0(2) . . . . ?
O6 C16 O5 Zn1 170.8(3) . . . . ?
C15 C16 O5 Zn1 -6.9(4) . . . . ?
O2 Zn1 O5 C16 -162(6) 2_566 . . . ?
O4 Zn1 O5 C16 102.1(2) . . . . ?
N2 Zn1 O5 C16 -162.5(2) . . . . ?
O1W Zn1 O5 C16 -66.7(2) . . . . ?
N1 Zn1 O5 C16 22.2(2) . . . . ?

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
O1W H1B O4W 0.81(4) 1.93(4) 2.744(4) 179(4) .
O2W H2A O6 0.75(5) 1.94(5) 2.676(3) 168(5) .
O3W H3A O6 0.82(5) 1.94(5) 2.721(4) 161(5) .
O1W H1A O1 0.85(4) 1.83(5) 2.629(4) 155(4) 2_566
O2W H2B O4 0.80(5) 1.91(5) 2.670(3) 160(5) 1_655
O4W H4A N3 0.895(10) 2.065(15) 2.944(4) 167(4) 1_655

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.058
#=========================END
data_Compound-8

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C64 H72 Co3 N10 O20'
_chemical_formula_sum            'C64 H72 Co3 N10 O20'
_chemical_formula_weight         1478.11

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_hall  '-P 1'

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

_cell_length_a                   8.6280(4)
_cell_length_b                   11.7140(6)
_cell_length_c                   16.5560(8)
_cell_angle_alpha                78.743(4)
_cell_angle_beta                 80.461(4)
_cell_angle_gamma                84.379(4)
_cell_volume                     1614.68(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4185
_cell_measurement_theta_min      3.2138
_cell_measurement_theta_max      29.2207

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             767
_exptl_absorpt_coefficient_mu    0.846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8228
_exptl_absorpt_correction_T_max  0.8836
_exptl_absorpt_process_details   
;
CrysAlis (Oxford Diffraction, 2006)
;
_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  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9622
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         25.03
_reflns_number_total             5684
_reflns_number_gt                4708
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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.

For C17 and C17' atoms, some anisotropic displacement ellipsoids were 
rather elongated which led us to use the ISOR restraints.
;

_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)+(0.0482P)²+0.6550P] 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         5684
_refine_ls_number_parameters     472
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.1007
_refine_ls_wR_factor_gt          0.0931
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.030
_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
Co1 Co 0.5000 0.5000 0.0000 0.02985(14) Uani 1 2 d S . .
Co2 Co -0.17922(4) 0.27211(3) 0.28662(2) 0.03258(12) Uani 1 1 d . . .
C1 C 0.5996(3) 0.7240(3) 0.35687(18) 0.0426(7) Uani 1 1 d . . .
H1 H 0.6120 0.6784 0.3158 0.051 Uiso 1 1 calc R . .
C2 C 0.7156(3) 0.7976(3) 0.35739(19) 0.0496(8) Uani 1 1 d . . .
H2 H 0.8048 0.8007 0.3171 0.060 Uiso 1 1 calc R . .
C3 C 0.6989(4) 0.8657(3) 0.41723(19) 0.0496(8) Uani 1 1 d . . .
H3 H 0.7768 0.9149 0.4180 0.060 Uiso 1 1 calc R . .
C4 C 0.5656(3) 0.8606(2) 0.47637(18) 0.0443(7) Uani 1 1 d . . .
H4 H 0.5545 0.9071 0.5168 0.053 Uiso 1 1 calc R . .
C5 C 0.4475(3) 0.7876(2) 0.47707(16) 0.0348(6) Uani 1 1 d . . .
C6 C 0.4647(3) 0.7168(2) 0.41651(16) 0.0336(6) Uani 1 1 d . . .
C7 C 0.3099(3) 0.7847(3) 0.54723(18) 0.0414(7) Uani 1 1 d . . .
C8 C 0.3467(3) 0.6338(2) 0.41321(15) 0.0344(6) Uani 1 1 d . . .
C9 C 0.1865(3) 0.6675(2) 0.41356(16) 0.0366(6) Uani 1 1 d . . .
H9 H 0.1497 0.7432 0.4194 0.044 Uiso 1 1 calc R . .
C10 C 0.0821(3) 0.5896(2) 0.40530(16) 0.0390(6) Uani 1 1 d . . .
H10 H -0.0242 0.6133 0.4067 0.047 Uiso 1 1 calc R . .
C11 C 0.1339(3) 0.4755(2) 0.39490(16) 0.0403(7) Uani 1 1 d . . .
C12 C 0.2911(4) 0.4420(3) 0.39713(19) 0.0494(8) Uani 1 1 d . . .
H12 H 0.3272 0.3656 0.3930 0.059 Uiso 1 1 calc R . .
C13 C 0.3969(4) 0.5195(3) 0.40544(19) 0.0457(7) Uani 1 1 d . . .
H13 H 0.5026 0.4946 0.4058 0.055 Uiso 1 1 calc R . .
C14 C 0.0222(4) 0.3904(3) 0.38283(18) 0.0479(8) Uani 1 1 d . . .
H14A H 0.0665 0.3119 0.4006 0.057 Uiso 1 1 calc R . .
H14B H -0.0762 0.4007 0.4195 0.057 Uiso 1 1 calc R . .
C15 C -0.0999(4) 0.5124(3) 0.2713(2) 0.0541(8) Uani 1 1 d . . .
H15A H -0.0251 0.5721 0.2521 0.065 Uiso 1 1 calc R . .
H15B H -0.1702 0.5333 0.3191 0.065 Uiso 1 1 calc R . .
C16 C -0.1950(3) 0.5093(3) 0.20257(18) 0.0431(7) Uani 1 1 d . . .
C17 C 0.1218(5) 0.3882(4) 0.2319(3) 0.0457(10) Uani 0.80 1 d PU . .
C17' C 0.164(2) 0.3449(18) 0.2641(12) 0.052(5) Uani 0.20 1 d PU . .
C18 C 0.1303(3) 0.2745(2) 0.19809(17) 0.0388(6) Uani 1 1 d . . .
C19 C -0.2866(3) 0.0767(2) 0.21422(17) 0.0388(6) Uani 1 1 d . . .
H19 H -0.1871 0.0641 0.1844 0.047 Uiso 1 1 calc R . .
C20 C -0.4782(3) 0.1446(3) 0.29350(18) 0.0443(7) Uani 1 1 d . . .
H20 H -0.5374 0.1894 0.3297 0.053 Uiso 1 1 calc R . .
C21 C -0.5337(3) 0.0599(3) 0.26363(19) 0.0472(7) Uani 1 1 d . . .
H21 H -0.6358 0.0357 0.2754 0.057 Uiso 1 1 calc R . .
C22 C -0.4154(4) -0.0751(2) 0.16585(18) 0.0477(7) Uani 1 1 d . . .
H22A H -0.4897 -0.1303 0.1975 0.057 Uiso 1 1 calc R . .
H22B H -0.3122 -0.1164 0.1600 0.057 Uiso 1 1 calc R . .
C23 C -0.4610(3) -0.0331(2) 0.08050(16) 0.0342(6) Uani 1 1 d . . .
C24 C -0.4850(3) 0.0833(2) 0.04609(17) 0.0389(6) Uani 1 1 d . . .
H24 H -0.4752 0.1402 0.0766 0.047 Uiso 1 1 calc R . .
C25 C -0.4766(3) -0.1158(2) 0.03318(17) 0.0395(6) Uani 1 1 d . . .
H25 H -0.4609 -0.1946 0.0554 0.047 Uiso 1 1 calc R . .
C26 C 0.2365(3) 0.6732(2) 0.06485(18) 0.0426(7) Uani 1 1 d . . .
H26 H 0.1923 0.6811 0.0164 0.051 Uiso 1 1 calc R . .
C27 C 0.3866(3) 0.6183(3) 0.15834(17) 0.0431(7) Uani 1 1 d . . .
H27 H 0.4673 0.5805 0.1865 0.052 Uiso 1 1 calc R . .
C28 C 0.2739(4) 0.6953(3) 0.18748(19) 0.0475(7) Uani 1 1 d . . .
H28 H 0.2629 0.7197 0.2384 0.057 Uiso 1 1 calc R . .
C29 C 0.0333(4) 0.8052(3) 0.1362(2) 0.0541(8) Uani 1 1 d . . .
H29A H 0.0256 0.8366 0.1869 0.065 Uiso 1 1 calc R . .
H29B H -0.0553 0.7576 0.1424 0.065 Uiso 1 1 calc R . .
C30 C 0.0198(3) 0.9051(2) 0.0645(2) 0.0449(7) Uani 1 1 d . . .
C31 C 0.0874(4) 1.0094(3) 0.0609(2) 0.0517(8) Uani 1 1 d . . .
H31 H 0.1463 1.0164 0.1017 0.062 Uiso 1 1 calc R . .
C32 C -0.0678(4) 0.8979(3) 0.0026(2) 0.0512(8) Uani 1 1 d . . .
H32 H -0.1141 0.8289 0.0042 0.061 Uiso 1 1 calc R . .
N1 N -0.0139(2) 0.39951(19) 0.29727(13) 0.0335(5) Uani 1 1 d . . .
N2 N -0.3221(2) 0.15484(19) 0.26254(13) 0.0351(5) Uani 1 1 d . . .
N3 N -0.4111(3) 0.01716(19) 0.21301(13) 0.0357(5) Uani 1 1 d . . .
N4 N 0.1797(3) 0.73007(19) 0.12748(15) 0.0412(6) Uani 1 1 d . . .
N5 N 0.3630(3) 0.60455(18) 0.08037(14) 0.0362(5) Uani 1 1 d . . .
O1 O 0.3152(2) 0.70002(19) 0.60706(12) 0.0503(5) Uani 1 1 d . . .
O2 O 0.2050(3) 0.8640(2) 0.54595(17) 0.0692(7) Uani 1 1 d . . .
O3 O 0.2421(2) 0.26100(19) 0.14325(13) 0.0560(6) Uani 1 1 d . . .
O4 O 0.0190(2) 0.20709(18) 0.22454(14) 0.0557(6) Uani 1 1 d . . .
O5 O -0.2222(3) 0.60094(19) 0.15475(14) 0.0636(7) Uani 1 1 d . . .
O6 O -0.2468(2) 0.41203(17) 0.20238(12) 0.0482(5) Uani 1 1 d . . .
O1W O 0.0904(4) 0.9573(3) 0.2759(2) 0.0963(9) Uani 1 1 d D . .
H1A H 0.112(7) 0.960(4) 0.3282(14) 0.144 Uiso 1 1 d D . .
H1B H 0.080(7) 1.0335(15) 0.252(3) 0.144 Uiso 1 1 d D . .
O2W O 0.1302(4) 1.0448(5) 0.4132(2) 0.1307(14) Uani 1 1 d D . .
H2A H 0.130(7) 0.974(3) 0.449(4) 0.196 Uiso 1 1 d D . .
H2B H 0.031(3) 1.078(5) 0.426(4) 0.196 Uiso 1 1 d D . .
O3W O 0.5404(3) 0.36906(18) 0.10483(13) 0.0413(5) Uani 1 1 d . . .
H3A H 0.585(4) 0.381(3) 0.138(2) 0.062 Uiso 1 1 d . . .
H3B H 0.468(4) 0.338(3) 0.132(2) 0.062 Uiso 1 1 d . . .
O4W O 0.7058(3) 0.5773(2) 0.00647(14) 0.0472(5) Uani 1 1 d . . .
H4A H 0.732(5) 0.626(3) -0.027(2) 0.071 Uiso 1 1 d . . .
H4B H 0.726(4) 0.590(3) 0.049(2) 0.071 Uiso 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
Co1 O4W 2.098(2) . ?
Co1 O4W 2.098(2) 2_665 ?
Co1 N5 2.121(2) . ?
Co1 N5 2.121(2) 2_665 ?
Co1 O3W 2.1314(19) 2_665 ?
Co1 O3W 2.1314(19) . ?
Co2 O4 2.007(2) . ?
Co2 O1 2.012(2) 2_566 ?
Co2 O6 2.0399(19) . ?
Co2 N2 2.067(2) . ?
Co2 N1 2.2127(19) . ?
C1 C2 1.385(4) . ?
C1 C6 1.394(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.370(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.379(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.390(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.403(4) . ?
C5 C7 1.515(4) . ?
C6 C8 1.489(3) . ?
C7 O2 1.231(4) . ?
C7 O1 1.261(4) . ?
C8 C13 1.389(4) . ?
C8 C9 1.400(4) . ?
C9 C10 1.383(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.401(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.379(4) . ?
C11 C14 1.514(4) . ?
C12 C13 1.389(4) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 N1 1.482(3) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N1 1.475(4) . ?
C15 C16 1.517(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 O5 1.231(3) . ?
C16 O6 1.264(3) . ?
C17 C17' 0.773(17) . ?
C17 N1 1.472(4) . ?
C17 C18 1.533(5) . ?
C17' C18 1.569(19) . ?
C17' N1 1.653(18) . ?
C18 O3 1.231(3) . ?
C18 O4 1.270(3) . ?
C19 N2 1.312(3) . ?
C19 N3 1.342(3) . ?
C19 H19 0.9300 . ?
C20 C21 1.349(4) . ?
C20 N2 1.368(3) . ?
C20 H20 0.9300 . ?
C21 N3 1.356(4) . ?
C21 H21 0.9300 . ?
C22 N3 1.458(3) . ?
C22 C23 1.506(4) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.381(4) . ?
C23 C25 1.388(3) . ?
C24 C25 1.379(4) 2_455 ?
C24 H24 0.9300 . ?
C25 C24 1.379(4) 2_455 ?
C25 H25 0.9300 . ?
C26 N5 1.320(4) . ?
C26 N4 1.341(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.355(4) . ?
C27 N5 1.381(3) . ?
C27 H27 0.9300 . ?
C28 N4 1.363(4) . ?
C28 H28 0.9300 . ?
C29 N4 1.470(4) . ?
C29 C30 1.507(4) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C32 1.389(4) . ?
C30 C31 1.392(4) . ?
C31 C32 1.376(4) 2_575 ?
C31 H31 0.9300 . ?
C32 C31 1.376(4) 2_575 ?
C32 H32 0.9300 . ?
O1 Co2 2.012(2) 2_566 ?
O1W H1A 0.920(10) . ?
O1W H1B 0.907(10) . ?
O2W H2A 0.918(10) . ?
O2W H2B 0.912(10) . ?
O3W H3A 0.77(4) . ?
O3W H3B 0.79(3) . ?
O4W H4A 0.73(4) . ?
O4W H4B 0.80(4) . ?

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
O4W Co1 O4W 180.00(12) . 2_665 ?
O4W Co1 N5 91.39(9) . . ?
O4W Co1 N5 88.61(9) 2_665 . ?
O4W Co1 N5 88.61(9) . 2_665 ?
O4W Co1 N5 91.39(9) 2_665 2_665 ?
N5 Co1 N5 180.00(9) . 2_665 ?
O4W Co1 O3W 89.63(8) . 2_665 ?
O4W Co1 O3W 90.37(8) 2_665 2_665 ?
N5 Co1 O3W 89.90(8) . 2_665 ?
N5 Co1 O3W 90.10(8) 2_665 2_665 ?
O4W Co1 O3W 90.37(8) . . ?
O4W Co1 O3W 89.63(8) 2_665 . ?
N5 Co1 O3W 90.10(8) . . ?
N5 Co1 O3W 89.90(8) 2_665 . ?
O3W Co1 O3W 180.00(13) 2_665 . ?
O4 Co2 O1 151.57(10) . 2_566 ?
O4 Co2 O6 102.85(9) . . ?
O1 Co2 O6 102.21(9) 2_566 . ?
O4 Co2 N2 94.95(8) . . ?
O1 Co2 N2 95.03(8) 2_566 . ?
O6 Co2 N2 97.17(8) . . ?
O4 Co2 N1 80.32(8) . . ?
O1 Co2 N1 91.24(8) 2_566 . ?
O6 Co2 N1 79.58(7) . . ?
N2 Co2 N1 173.44(8) . . ?
C2 C1 C6 121.4(3) . . ?
C2 C1 H1 119.3 . . ?
C6 C1 H1 119.3 . . ?
C3 C2 C1 120.1(3) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 119.4(3) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C3 C4 C5 121.7(3) . . ?
C3 C4 H4 119.2 . . ?
C5 C4 H4 119.2 . . ?
C4 C5 C6 119.2(2) . . ?
C4 C5 C7 117.2(2) . . ?
C6 C5 C7 123.5(2) . . ?
C1 C6 C5 118.2(2) . . ?
C1 C6 C8 118.5(2) . . ?
C5 C6 C8 123.3(2) . . ?
O2 C7 O1 123.5(3) . . ?
O2 C7 C5 120.7(3) . . ?
O1 C7 C5 115.6(3) . . ?
C13 C8 C9 118.0(2) . . ?
C13 C8 C6 119.4(2) . . ?
C9 C8 C6 122.5(2) . . ?
C10 C9 C8 120.8(3) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C11 121.1(3) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C12 C11 C10 117.6(2) . . ?
C12 C11 C14 120.6(3) . . ?
C10 C11 C14 121.8(3) . . ?
C11 C12 C13 121.7(3) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.2 . . ?
C12 C13 C8 120.7(3) . . ?
C12 C13 H13 119.6 . . ?
C8 C13 H13 119.6 . . ?
N1 C14 C11 116.6(2) . . ?
N1 C14 H14A 108.1 . . ?
C11 C14 H14A 108.1 . . ?
N1 C14 H14B 108.1 . . ?
C11 C14 H14B 108.1 . . ?
H14A C14 H14B 107.3 . . ?
N1 C15 C16 112.4(2) . . ?
N1 C15 H15A 109.1 . . ?
C16 C15 H15A 109.1 . . ?
N1 C15 H15B 109.1 . . ?
C16 C15 H15B 109.1 . . ?
H15A C15 H15B 107.9 . . ?
O5 C16 O6 125.4(3) . . ?
O5 C16 C15 118.4(2) . . ?
O6 C16 C15 116.1(2) . . ?
C17' C17 N1 89.2(15) . . ?
C17' C17 C18 78.2(15) . . ?
N1 C17 C18 113.2(3) . . ?
C17 C17' C18 73.0(14) . . ?
C17 C17' N1 62.9(13) . . ?
C18 C17' N1 102.2(10) . . ?
O3 C18 O4 125.9(3) . . ?
O3 C18 C17 115.6(3) . . ?
O4 C18 C17 118.3(3) . . ?
O3 C18 C17' 115.1(7) . . ?
O4 C18 C17' 113.8(8) . . ?
C17 C18 C17' 28.8(6) . . ?
N2 C19 N3 111.8(2) . . ?
N2 C19 H19 124.1 . . ?
N3 C19 H19 124.1 . . ?
C21 C20 N2 109.9(3) . . ?
C21 C20 H20 125.1 . . ?
N2 C20 H20 125.1 . . ?
C20 C21 N3 106.4(2) . . ?
C20 C21 H21 126.8 . . ?
N3 C21 H21 126.8 . . ?
N3 C22 C23 114.4(2) . . ?
N3 C22 H22A 108.6 . . ?
C23 C22 H22A 108.6 . . ?
N3 C22 H22B 108.6 . . ?
C23 C22 H22B 108.6 . . ?
H22A C22 H22B 107.6 . . ?
C24 C23 C25 118.2(2) . . ?
C24 C23 C22 123.5(2) . . ?
C25 C23 C22 118.3(2) . . ?
C25 C24 C23 120.5(2) 2_455 . ?
C25 C24 H24 119.7 2_455 . ?
C23 C24 H24 119.7 . . ?
C24 C25 C23 121.3(3) 2_455 . ?
C24 C25 H25 119.4 2_455 . ?
C23 C25 H25 119.4 . . ?
N5 C26 N4 111.8(3) . . ?
N5 C26 H26 124.1 . . ?
N4 C26 H26 124.1 . . ?
C28 C27 N5 109.5(3) . . ?
C28 C27 H27 125.3 . . ?
N5 C27 H27 125.3 . . ?
C27 C28 N4 106.6(3) . . ?
C27 C28 H28 126.7 . . ?
N4 C28 H28 126.7 . . ?
N4 C29 C30 114.7(2) . . ?
N4 C29 H29A 108.6 . . ?
C30 C29 H29A 108.6 . . ?
N4 C29 H29B 108.6 . . ?
C30 C29 H29B 108.6 . . ?
H29A C29 H29B 107.6 . . ?
C32 C30 C31 118.2(3) . . ?
C32 C30 C29 120.8(3) . . ?
C31 C30 C29 120.8(3) . . ?
C32 C31 C30 120.4(3) 2_575 . ?
C32 C31 H31 119.8 2_575 . ?
C30 C31 H31 119.8 . . ?
C31 C32 C30 121.4(3) 2_575 . ?
C31 C32 H32 119.3 2_575 . ?
C30 C32 H32 119.3 . . ?
C17 N1 C15 107.0(3) . . ?
C17 N1 C14 116.3(3) . . ?
C15 N1 C14 110.2(2) . . ?
C17 N1 C17' 27.9(6) . . ?
C15 N1 C17' 132.1(8) . . ?
C14 N1 C17' 92.4(7) . . ?
C17 N1 Co2 105.93(18) . . ?
C15 N1 Co2 102.61(15) . . ?
C14 N1 Co2 113.70(15) . . ?
C17' N1 Co2 106.0(7) . . ?
C19 N2 C20 105.0(2) . . ?
C19 N2 Co2 128.72(18) . . ?
C20 N2 Co2 126.26(18) . . ?
C19 N3 C21 106.9(2) . . ?
C19 N3 C22 126.9(2) . . ?
C21 N3 C22 126.2(2) . . ?
C26 N4 C28 107.1(2) . . ?
C26 N4 C29 127.5(3) . . ?
C28 N4 C29 125.0(3) . . ?
C26 N5 C27 105.0(2) . . ?
C26 N5 Co1 126.50(19) . . ?
C27 N5 Co1 128.45(19) . . ?
C7 O1 Co2 113.80(19) . 2_566 ?
C18 O4 Co2 117.34(18) . . ?
C16 O6 Co2 117.63(17) . . ?
H1A O1W H1B 104.0(15) . . ?
H2A O2W H2B 103.8(15) . . ?
Co1 O3W H3A 121(3) . . ?
Co1 O3W H3B 119(3) . . ?
H3A O3W H3B 102(4) . . ?
Co1 O4W H4A 118(3) . . ?
Co1 O4W H4B 122(3) . . ?
H4A O4W H4B 108(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
C6 C1 C2 C3 -0.2(5) . . . . ?
C1 C2 C3 C4 -0.3(5) . . . . ?
C2 C3 C4 C5 0.2(5) . . . . ?
C3 C4 C5 C6 0.5(4) . . . . ?
C3 C4 C5 C7 177.2(3) . . . . ?
C2 C1 C6 C5 0.9(4) . . . . ?
C2 C1 C6 C8 -178.6(3) . . . . ?
C4 C5 C6 C1 -1.0(4) . . . . ?
C7 C5 C6 C1 -177.5(3) . . . . ?
C4 C5 C6 C8 178.5(2) . . . . ?
C7 C5 C6 C8 2.0(4) . . . . ?
C4 C5 C7 O2 77.6(3) . . . . ?
C6 C5 C7 O2 -105.9(3) . . . . ?
C4 C5 C7 O1 -99.2(3) . . . . ?
C6 C5 C7 O1 77.3(3) . . . . ?
C1 C6 C8 C13 48.5(4) . . . . ?
C5 C6 C8 C13 -131.0(3) . . . . ?
C1 C6 C8 C9 -128.3(3) . . . . ?
C5 C6 C8 C9 52.1(4) . . . . ?
C13 C8 C9 C10 -0.8(4) . . . . ?
C6 C8 C9 C10 176.0(2) . . . . ?
C8 C9 C10 C11 -1.1(4) . . . . ?
C9 C10 C11 C12 3.0(4) . . . . ?
C9 C10 C11 C14 -177.9(2) . . . . ?
C10 C11 C12 C13 -3.0(4) . . . . ?
C14 C11 C12 C13 177.9(3) . . . . ?
C11 C12 C13 C8 1.1(5) . . . . ?
C9 C8 C13 C12 0.9(4) . . . . ?
C6 C8 C13 C12 -176.1(3) . . . . ?
C12 C11 C14 N1 -98.6(3) . . . . ?
C10 C11 C14 N1 82.3(4) . . . . ?
N1 C15 C16 O5 -153.1(3) . . . . ?
N1 C15 C16 O6 30.5(4) . . . . ?
N1 C17 C17' C18 113.9(4) . . . . ?
C18 C17 C17' N1 -113.9(4) . . . . ?
C17' C17 C18 O3 -95.9(16) . . . . ?
N1 C17 C18 O3 -179.9(3) . . . . ?
C17' C17 C18 O4 88.3(16) . . . . ?
N1 C17 C18 O4 4.3(5) . . . . ?
N1 C17 C18 C17' -84.0(16) . . . . ?
C17 C17' C18 O3 98.1(14) . . . . ?
N1 C17' C18 O3 154.4(7) . . . . ?
C17 C17' C18 O4 -105.9(15) . . . . ?
N1 C17' C18 O4 -49.5(12) . . . . ?
N1 C17' C18 C17 56.4(11) . . . . ?
N2 C20 C21 N3 -0.4(3) . . . . ?
N3 C22 C23 C24 4.9(4) . . . . ?
N3 C22 C23 C25 -176.5(2) . . . . ?
C25 C23 C24 C25 0.0(4) . . . 2_455 ?
C22 C23 C24 C25 178.6(3) . . . 2_455 ?
C24 C23 C25 C24 0.0(4) . . . 2_455 ?
C22 C23 C25 C24 -178.7(3) . . . 2_455 ?
N5 C27 C28 N4 -0.1(3) . . . . ?
N4 C29 C30 C32 99.3(3) . . . . ?
N4 C29 C30 C31 -84.3(4) . . . . ?
C32 C30 C31 C32 -0.2(5) . . . 2_575 ?
C29 C30 C31 C32 -176.7(3) . . . 2_575 ?
C31 C30 C32 C31 0.2(5) . . . 2_575 ?
C29 C30 C32 C31 176.7(3) . . . 2_575 ?
C17' C17 N1 C15 156.9(16) . . . . ?
C18 C17 N1 C15 -126.3(3) . . . . ?
C17' C17 N1 C14 33.3(16) . . . . ?
C18 C17 N1 C14 110.0(3) . . . . ?
C18 C17 N1 C17' 76.8(16) . . . . ?
C17' C17 N1 Co2 -94.1(16) . . . . ?
C18 C17 N1 Co2 -17.4(4) . . . . ?
C16 C15 N1 C17 75.4(3) . . . . ?
C16 C15 N1 C14 -157.2(2) . . . . ?
C16 C15 N1 C17' 89.8(9) . . . . ?
C16 C15 N1 Co2 -35.8(3) . . . . ?
C11 C14 N1 C17 56.9(4) . . . . ?
C11 C14 N1 C15 -65.1(3) . . . . ?
C11 C14 N1 C17' 71.8(8) . . . . ?
C11 C14 N1 Co2 -179.6(2) . . . . ?
C18 C17' N1 C17 -63.5(12) . . . . ?
C17 C17' N1 C15 -30(2) . . . . ?
C18 C17' N1 C15 -93.8(12) . . . . ?
C17 C17' N1 C14 -150.5(14) . . . . ?
C18 C17' N1 C14 146.0(9) . . . . ?
C17 C17' N1 Co2 94.0(15) . . . . ?
C18 C17' N1 Co2 30.5(11) . . . . ?
O4 Co2 N1 C17 18.8(2) . . . . ?
O1 Co2 N1 C17 171.5(2) 2_566 . . . ?
O6 Co2 N1 C17 -86.3(2) . . . . ?
N2 Co2 N1 C17 -25.5(8) . . . . ?
O4 Co2 N1 C15 130.87(19) . . . . ?
O1 Co2 N1 C15 -76.42(19) 2_566 . . . ?
O6 Co2 N1 C15 25.76(18) . . . . ?
N2 Co2 N1 C15 86.6(8) . . . . ?
O4 Co2 N1 C14 -110.2(2) . . . . ?
O1 Co2 N1 C14 42.5(2) 2_566 . . . ?
O6 Co2 N1 C14 144.7(2) . . . . ?
N2 Co2 N1 C14 -154.5(7) . . . . ?
O4 Co2 N1 C17' -10.2(7) . . . . ?
O1 Co2 N1 C17' 142.5(7) 2_566 . . . ?
O6 Co2 N1 C17' -115.4(7) . . . . ?
N2 Co2 N1 C17' -54.5(10) . . . . ?
N3 C19 N2 C20 -0.3(3) . . . . ?
N3 C19 N2 Co2 -179.03(17) . . . . ?
C21 C20 N2 C19 0.4(3) . . . . ?
C21 C20 N2 Co2 179.2(2) . . . . ?
O4 Co2 N2 C19 -6.6(2) . . . . ?
O1 Co2 N2 C19 -160.0(2) 2_566 . . . ?
O6 Co2 N2 C19 97.0(2) . . . . ?
N1 Co2 N2 C19 37.1(9) . . . . ?
O4 Co2 N2 C20 174.8(2) . . . . ?
O1 Co2 N2 C20 21.5(2) 2_566 . . . ?
O6 Co2 N2 C20 -81.5(2) . . . . ?
N1 Co2 N2 C20 -141.5(7) . . . . ?
N2 C19 N3 C21 0.0(3) . . . . ?
N2 C19 N3 C22 179.4(2) . . . . ?
C20 C21 N3 C19 0.2(3) . . . . ?
C20 C21 N3 C22 -179.2(3) . . . . ?
C23 C22 N3 C19 -90.9(3) . . . . ?
C23 C22 N3 C21 88.4(3) . . . . ?
N5 C26 N4 C28 -0.7(3) . . . . ?
N5 C26 N4 C29 -173.9(2) . . . . ?
C27 C28 N4 C26 0.5(3) . . . . ?
C27 C28 N4 C29 173.9(2) . . . . ?
C30 C29 N4 C26 -56.1(4) . . . . ?
C30 C29 N4 C28 131.8(3) . . . . ?
N4 C26 N5 C27 0.6(3) . . . . ?
N4 C26 N5 Co1 -178.20(16) . . . . ?
C28 C27 N5 C26 -0.3(3) . . . . ?
C28 C27 N5 Co1 178.48(18) . . . . ?
O4W Co1 N5 C26 125.0(2) . . . . ?
O4W Co1 N5 C26 -55.0(2) 2_665 . . . ?
N5 Co1 N5 C26 0(100) 2_665 . . . ?
O3W Co1 N5 C26 35.4(2) 2_665 . . . ?
O3W Co1 N5 C26 -144.6(2) . . . . ?
O4W Co1 N5 C27 -53.5(2) . . . . ?
O4W Co1 N5 C27 126.5(2) 2_665 . . . ?
N5 Co1 N5 C27 -178(100) 2_665 . . . ?
O3W Co1 N5 C27 -143.1(2) 2_665 . . . ?
O3W Co1 N5 C27 36.9(2) . . . . ?
O2 C7 O1 Co2 -17.5(3) . . . 2_566 ?
C5 C7 O1 Co2 159.24(16) . . . 2_566 ?
O3 C18 O4 Co2 -161.3(2) . . . . ?
C17 C18 O4 Co2 13.9(4) . . . . ?
C17' C18 O4 Co2 45.7(8) . . . . ?
O1 Co2 O4 C18 -93.2(3) 2_566 . . . ?
O6 Co2 O4 C18 58.1(2) . . . . ?
N2 Co2 O4 C18 156.7(2) . . . . ?
N1 Co2 O4 C18 -18.7(2) . . . . ?
O5 C16 O6 Co2 178.5(3) . . . . ?
C15 C16 O6 Co2 -5.4(4) . . . . ?
O4 Co2 O6 C16 -89.8(2) . . . . ?
O1 Co2 O6 C16 76.7(2) 2_566 . . . ?
N2 Co2 O6 C16 173.4(2) . . . . ?
N1 Co2 O6 C16 -12.3(2) . . . . ?

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
O1W H1A O2W 0.920(10) 1.91(3) 2.752(6) 151(4) .
O2W H2A O2 0.918(10) 2.01(4) 2.849(5) 152(7) .
O3W H3B O3 0.79(3) 2.19(4) 2.900(3) 150(3) .
O1W H1B O4 0.907(10) 2.031(18) 2.918(4) 165(5) 1_565
O2W H2B O2 0.912(10) 2.091(14) 2.999(5) 173(6) 2_576
O3W H3A O6 0.77(4) 2.03(4) 2.778(3) 165(4) 1_655
O4W H4A O3 0.73(4) 2.11(4) 2.810(3) 161(4) 2_665
O4W H4B O5 0.80(4) 1.90(4) 2.701(3) 174(4) 1_655

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.053
#=========================END
data_Compound-9

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H72 Co3 N10 O20'
_chemical_formula_sum            'C56 H72 Co3 N10 O20'
_chemical_formula_weight         1382.03

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   10.1040(6)
_cell_length_b                   10.5370(8)
_cell_length_c                   15.1970(9)
_cell_angle_alpha                70.911(6)
_cell_angle_beta                 87.456(5)
_cell_angle_gamma                87.386(6)
_cell_volume                     1526.66(17)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3280
_cell_measurement_theta_min      3.4444
_cell_measurement_theta_max      29.2173

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             719
_exptl_absorpt_coefficient_mu    0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8084
_exptl_absorpt_correction_T_max  0.8783
_exptl_absorpt_process_details   
;
CrysAlis (Oxford Diffraction, 2006)
;
_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  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9255
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.45
_diffrn_reflns_theta_max         25.03
_reflns_number_total             5355
_reflns_number_gt                4499
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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)+(0.0345P)²+0.6215P] 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         5355
_refine_ls_number_parameters     434
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_ref         0.0844
_refine_ls_wR_factor_gt          0.0782
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.007
_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
Co1 Co 0.74487(3) 0.16257(3) 0.23332(2) 0.02607(11) Uani 1 1 d . . .
Co2 Co 0.5000 0.5000 -0.5000 0.02464(12) Uani 1 2 d S . .
C1 C 0.8392(2) 0.2400(3) 0.06221(18) 0.0347(6) Uani 1 1 d . . .
C2 C 0.9379(2) 0.2670(2) -0.01922(16) 0.0291(5) Uani 1 1 d . . .
C3 C 1.0435(3) 0.3466(3) -0.01848(19) 0.0398(6) Uani 1 1 d . . .
H3 H 1.0457 0.3876 0.0271 0.048 Uiso 1 1 calc R . .
C4 C 1.1450(3) 0.3653(3) -0.08487(19) 0.0424(7) Uani 1 1 d . . .
H4 H 1.2148 0.4198 -0.0847 0.051 Uiso 1 1 calc R . .
C5 C 1.1424(3) 0.3031(3) -0.15115(19) 0.0429(7) Uani 1 1 d . . .
H5 H 1.2111 0.3148 -0.1956 0.051 Uiso 1 1 calc R . .
C6 C 1.0387(2) 0.2234(3) -0.15238(18) 0.0379(6) Uani 1 1 d . . .
H6 H 1.0391 0.1810 -0.1973 0.046 Uiso 1 1 calc R . .
C7 C 0.9335(2) 0.2051(2) -0.08780(16) 0.0288(5) Uani 1 1 d . . .
C8 C 0.8178(2) 0.1264(3) -0.09477(15) 0.0286(5) Uani 1 1 d . . .
C9 C 0.6901(2) 0.1800(3) -0.09525(17) 0.0342(6) Uani 1 1 d . . .
H9 H 0.6768 0.2649 -0.0895 0.041 Uiso 1 1 calc R . .
C10 C 0.5819(2) 0.1098(3) -0.10417(17) 0.0351(6) Uani 1 1 d . . .
H10 H 0.4971 0.1477 -0.1036 0.042 Uiso 1 1 calc R . .
C11 C 0.5981(2) -0.0165(3) -0.11397(16) 0.0321(6) Uani 1 1 d . . .
C12 C 0.7262(2) -0.0710(3) -0.11240(18) 0.0378(6) Uani 1 1 d . . .
H12 H 0.7394 -0.1561 -0.1178 0.045 Uiso 1 1 calc R . .
C13 C 0.8348(2) -0.0009(3) -0.10298(17) 0.0354(6) Uani 1 1 d . . .
H13 H 0.9195 -0.0395 -0.1021 0.042 Uiso 1 1 calc R . .
C14 C 0.4799(2) -0.0922(3) -0.12632(17) 0.0340(6) Uani 1 1 d . . .
H14A H 0.5062 -0.1863 -0.1118 0.041 Uiso 1 1 calc R . .
H15B H 0.4106 -0.0861 -0.0815 0.041 Uiso 1 1 calc R . .
C15 C 0.5196(2) -0.0571(3) -0.29309(18) 0.0359(6) Uani 1 1 d . . .
H5A H 0.6084 -0.0490 -0.2741 0.043 Uiso 1 1 calc R . .
H5B H 0.5037 0.0160 -0.3504 0.043 Uiso 1 1 calc R . .
C16 C 0.5117(2) -0.1899(3) -0.31138(19) 0.0378(6) Uani 1 1 d . . .
C17 C 0.3667(2) 0.0929(3) -0.24482(18) 0.0342(6) Uani 1 1 d . . .
H17A H 0.4374 0.1565 -0.2638 0.041 Uiso 1 1 calc R . .
H17B H 0.3211 0.1049 -0.1904 0.041 Uiso 1 1 calc R . .
C18 C 0.2697(2) 0.1210(3) -0.32351(17) 0.0323(6) Uani 1 1 d . . .
C19 C 1.0240(2) 0.2526(3) 0.25854(19) 0.0407(7) Uani 1 1 d . . .
H19 H 1.0661 0.1929 0.2320 0.049 Uiso 1 1 calc R . .
C20 C 1.0865(2) 0.3357(3) 0.29395(19) 0.0426(7) Uani 1 1 d . . .
H20 H 1.1775 0.3431 0.2966 0.051 Uiso 1 1 calc R . .
C21 C 0.8734(2) 0.3634(2) 0.30807(16) 0.0268(5) Uani 1 1 d . . .
H21 H 0.7913 0.3957 0.3230 0.032 Uiso 1 1 calc R . .
C22 C 1.0086(3) 0.5049(3) 0.37232(18) 0.0390(6) Uani 1 1 d . . .
H22A H 0.9474 0.5809 0.3480 0.047 Uiso 1 1 calc R . .
H22B H 1.0979 0.5375 0.3585 0.047 Uiso 1 1 calc R . .
C23 C 0.9874(3) 0.4480(3) 0.47648(17) 0.0335(6) Uani 1 1 d . . .
H23A H 1.0467 0.3705 0.5009 0.040 Uiso 1 1 calc R . .
H23B H 0.8971 0.4184 0.4908 0.040 Uiso 1 1 calc R . .
C24 C 0.3079(2) 0.7117(2) -0.63617(16) 0.0296(5) Uani 1 1 d . . .
H24 H 0.3172 0.6703 -0.6817 0.036 Uiso 1 1 calc R . .
C25 C 0.3328(2) 0.7582(2) -0.51114(16) 0.0279(5) Uani 1 1 d . . .
H25 H 0.3619 0.7559 -0.4534 0.033 Uiso 1 1 calc R . .
C26 C 0.2276(2) 0.8194(3) -0.64104(16) 0.0308(6) Uani 1 1 d . . .
H26 H 0.1719 0.8646 -0.6893 0.037 Uiso 1 1 calc R . .
C27 C 0.1788(2) 0.9599(3) -0.53427(19) 0.0336(6) Uani 1 1 d . . .
H27A H 0.1922 1.0436 -0.5845 0.040 Uiso 1 1 calc R . .
H27B H 0.2204 0.9663 -0.4796 0.040 Uiso 1 1 calc R . .
C28 C 0.0317(2) 0.9421(2) -0.51358(18) 0.0311(5) Uani 1 1 d . . .
H28A H 0.0178 0.8586 -0.4632 0.037 Uiso 1 1 calc R . .
H28B H -0.0105 0.9365 -0.5682 0.037 Uiso 1 1 calc R . .
N1 N 0.42358(18) -0.0445(2) -0.22074(13) 0.0273(4) Uani 1 1 d . . .
N2 N 0.88949(18) 0.2702(2) 0.26786(13) 0.0272(4) Uani 1 1 d . . .
N3 N 0.98908(19) 0.4060(2) 0.32476(13) 0.0296(5) Uani 1 1 d . . .
N4 N 0.37406(17) 0.6722(2) -0.55374(13) 0.0274(4) Uani 1 1 d . . .
N5 N 0.24410(17) 0.84923(19) -0.56064(13) 0.0262(4) Uani 1 1 d . . .
O1 O 0.76093(18) 0.3302(2) 0.07029(15) 0.0525(5) Uani 1 1 d . . .
O2 O 0.84672(17) 0.1266(2) 0.12387(12) 0.0420(5) Uani 1 1 d . . .
O3 O 0.40482(16) -0.25398(19) -0.28552(13) 0.0404(5) Uani 1 1 d . . .
O4 O 0.60539(19) -0.2252(2) -0.35259(18) 0.0675(7) Uani 1 1 d . . .
O5 O 0.21602(17) 0.02016(18) -0.33245(12) 0.0397(4) Uani 1 1 d . . .
O6 O 0.24687(18) 0.23921(19) -0.37068(13) 0.0435(5) Uani 1 1 d . . .
O1W O 0.60907(19) 0.5483(2) -0.62904(13) 0.0365(4) Uani 1 1 d . . .
H1A H 0.571(3) 0.548(3) -0.675(2) 0.055 Uiso 1 1 d . . .
H1B H 0.649(3) 0.611(3) -0.637(2) 0.055 Uiso 1 1 d . . .
O2W O 0.36158(18) 0.3879(2) -0.54475(14) 0.0370(4) Uani 1 1 d . . .
H2A H 0.326(3) 0.344(3) -0.502(2) 0.056 Uiso 1 1 d . . .
H2B H 0.381(3) 0.342(3) -0.578(2) 0.056 Uiso 1 1 d . . .
O3W O 0.5337(13) 0.5270(18) -0.7958(11) 0.068(3) Uani 0.60 1 d P . .
O3W' O 0.493(2) 0.525(2) -0.7762(15) 0.079(5) Uani 0.40 1 d P . .
O4W O 0.3209(7) 0.4743(6) -0.9086(5) 0.146(2) Uani 0.65 1 d P . .
O4W' O 0.4489(10) 0.5351(11) -0.9647(6) 0.110(3) Uani 0.35 1 d P . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
Co1 O3 2.0261(17) 2_655 ?
Co1 O2 2.0480(18) . ?
Co1 O5 2.0541(18) 2_655 ?
Co1 N2 2.0746(17) . ?
Co1 N1 2.2046(18) 2_655 ?
Co2 N4 2.1189(19) . ?
Co2 N4 2.1189(19) 2_664 ?
Co2 O1W 2.1274(18) . ?
Co2 O1W 2.1274(18) 2_664 ?
Co2 O2W 2.1390(18) . ?
Co2 O2W 2.1390(18) 2_664 ?
C1 O1 1.242(3) . ?
C1 O2 1.256(3) . ?
C1 C2 1.514(3) . ?
C2 C3 1.389(3) . ?
C2 C7 1.401(3) . ?
C3 C4 1.380(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.372(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.376(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.391(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.491(3) . ?
C8 C9 1.384(3) . ?
C8 C13 1.390(4) . ?
C9 C10 1.384(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.388(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.390(4) . ?
C11 C14 1.518(3) . ?
C12 C13 1.388(3) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 N1 1.487(3) . ?
C14 H14A 0.9700 . ?
C14 H15B 0.9700 . ?
C15 N1 1.469(3) . ?
C15 C16 1.520(4) . ?
C15 H5A 0.9700 . ?
C15 H5B 0.9700 . ?
C16 O4 1.222(3) . ?
C16 O3 1.277(3) . ?
C17 N1 1.468(3) . ?
C17 C18 1.525(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 O6 1.234(3) . ?
C18 O5 1.263(3) . ?
C19 C20 1.358(4) . ?
C19 N2 1.371(3) . ?
C19 H19 0.9300 . ?
C20 N3 1.362(3) . ?
C20 H20 0.9300 . ?
C21 N2 1.317(3) . ?
C21 N3 1.334(3) . ?
C21 H21 0.9300 . ?
C22 N3 1.473(3) . ?
C22 C23 1.507(4) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C23 1.526(5) 2_766 ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C26 1.348(3) . ?
C24 N4 1.377(3) . ?
C24 H24 0.9300 . ?
C25 N4 1.319(3) . ?
C25 N5 1.341(3) . ?
C25 H25 0.9300 . ?
C26 N5 1.376(3) . ?
C26 H26 0.9300 . ?
C27 N5 1.472(3) . ?
C27 C28 1.513(3) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C28 1.518(5) 2_574 ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
N1 Co1 2.2046(18) 2_655 ?
O3 Co1 2.0261(17) 2_655 ?
O5 Co1 2.0541(18) 2_655 ?
O1W H1A 0.81(3) . ?
O1W H1B 0.76(3) . ?
O2W H2A 0.74(3) . ?
O2W H2B 0.82(3) . ?
O4W O4W' 1.559(11) . ?
O4W' O4W' 1.765(16) 2_663 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Co1 O2 151.43(8) 2_655 . ?
O3 Co1 O5 107.03(8) 2_655 2_655 ?
O2 Co1 O5 97.73(8) . 2_655 ?
O3 Co1 N2 93.27(7) 2_655 . ?
O2 Co1 N2 97.26(7) . . ?
O5 Co1 N2 97.93(7) 2_655 . ?
O3 Co1 N1 79.62(7) 2_655 2_655 ?
O2 Co1 N1 92.20(7) . 2_655 ?
O5 Co1 N1 77.85(7) 2_655 2_655 ?
N2 Co1 N1 170.11(7) . 2_655 ?
N4 Co2 N4 180.00(11) . 2_664 ?
N4 Co2 O1W 90.57(7) . . ?
N4 Co2 O1W 89.43(7) 2_664 . ?
N4 Co2 O1W 89.43(7) . 2_664 ?
N4 Co2 O1W 90.57(7) 2_664 2_664 ?
O1W Co2 O1W 180.00(10) . 2_664 ?
N4 Co2 O2W 88.16(7) . . ?
N4 Co2 O2W 91.84(7) 2_664 . ?
O1W Co2 O2W 92.11(8) . . ?
O1W Co2 O2W 87.89(8) 2_664 . ?
N4 Co2 O2W 91.84(7) . 2_664 ?
N4 Co2 O2W 88.16(7) 2_664 2_664 ?
O1W Co2 O2W 87.89(8) . 2_664 ?
O1W Co2 O2W 92.11(8) 2_664 2_664 ?
O2W Co2 O2W 180.0 . 2_664 ?
O1 C1 O2 121.9(2) . . ?
O1 C1 C2 120.8(3) . . ?
O2 C1 C2 117.2(2) . . ?
C3 C2 C7 120.1(2) . . ?
C3 C2 C1 116.6(2) . . ?
C7 C2 C1 122.9(2) . . ?
C4 C3 C2 120.5(2) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C5 C4 C3 119.6(2) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 120.5(2) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C7 121.3(2) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C6 C7 C2 118.0(2) . . ?
C6 C7 C8 120.2(2) . . ?
C2 C7 C8 121.8(2) . . ?
C9 C8 C13 118.1(2) . . ?
C9 C8 C7 120.5(2) . . ?
C13 C8 C7 121.3(2) . . ?
C10 C9 C8 121.3(2) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C9 C10 C11 120.9(2) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C10 C11 C12 117.8(2) . . ?
C10 C11 C14 121.1(2) . . ?
C12 C11 C14 121.2(2) . . ?
C13 C12 C11 121.3(2) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C12 C13 C8 120.5(2) . . ?
C12 C13 H13 119.7 . . ?
C8 C13 H13 119.7 . . ?
N1 C14 C11 115.31(19) . . ?
N1 C14 H14A 108.4 . . ?
C11 C14 H14A 108.4 . . ?
N1 C14 H15B 108.4 . . ?
C11 C14 H15B 108.4 . . ?
H14A C14 H15B 107.5 . . ?
N1 C15 C16 112.6(2) . . ?
N1 C15 H5A 109.1 . . ?
C16 C15 H5A 109.1 . . ?
N1 C15 H5B 109.1 . . ?
C16 C15 H5B 109.1 . . ?
H5A C15 H5B 107.8 . . ?
O4 C16 O3 124.8(2) . . ?
O4 C16 C15 118.0(2) . . ?
O3 C16 C15 117.2(2) . . ?
N1 C17 C18 110.98(19) . . ?
N1 C17 H17A 109.4 . . ?
C18 C17 H17A 109.4 . . ?
N1 C17 H17B 109.4 . . ?
C18 C17 H17B 109.4 . . ?
H17A C17 H17B 108.0 . . ?
O6 C18 O5 125.7(2) . . ?
O6 C18 C17 117.9(2) . . ?
O5 C18 C17 116.4(2) . . ?
C20 C19 N2 109.6(2) . . ?
C20 C19 H19 125.2 . . ?
N2 C19 H19 125.2 . . ?
C19 C20 N3 106.2(2) . . ?
C19 C20 H20 126.9 . . ?
N3 C20 H20 126.9 . . ?
N2 C21 N3 111.9(2) . . ?
N2 C21 H21 124.0 . . ?
N3 C21 H21 124.0 . . ?
N3 C22 C23 113.0(2) . . ?
N3 C22 H22A 109.0 . . ?
C23 C22 H22A 109.0 . . ?
N3 C22 H22B 109.0 . . ?
C23 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
C22 C23 C23 111.4(3) . 2_766 ?
C22 C23 H23A 109.3 . . ?
C23 C23 H23A 109.3 2_766 . ?
C22 C23 H23B 109.3 . . ?
C23 C23 H23B 109.3 2_766 . ?
H23A C23 H23B 108.0 . . ?
C26 C24 N4 109.8(2) . . ?
C26 C24 H24 125.1 . . ?
N4 C24 H24 125.1 . . ?
N4 C25 N5 112.2(2) . . ?
N4 C25 H25 123.9 . . ?
N5 C25 H25 123.9 . . ?
C24 C26 N5 106.6(2) . . ?
C24 C26 H26 126.7 . . ?
N5 C26 H26 126.7 . . ?
N5 C27 C28 113.13(19) . . ?
N5 C27 H27A 109.0 . . ?
C28 C27 H27A 109.0 . . ?
N5 C27 H27B 109.0 . . ?
C28 C27 H27B 109.0 . . ?
H27A C27 H27B 107.8 . . ?
C27 C28 C28 111.5(2) . 2_574 ?
C27 C28 H28A 109.3 . . ?
C28 C28 H28A 109.3 2_574 . ?
C27 C28 H28B 109.3 . . ?
C28 C28 H28B 109.3 2_574 . ?
H28A C28 H28B 108.0 . . ?
C15 N1 C17 110.99(19) . . ?
C15 N1 C14 112.40(19) . . ?
C17 N1 C14 112.52(19) . . ?
C15 N1 Co1 104.13(13) . 2_655 ?
C17 N1 Co1 103.26(13) . 2_655 ?
C14 N1 Co1 112.90(14) . 2_655 ?
C21 N2 C19 105.13(19) . . ?
C21 N2 Co1 128.09(15) . . ?
C19 N2 Co1 126.66(17) . . ?
C21 N3 C20 107.1(2) . . ?
C21 N3 C22 126.6(2) . . ?
C20 N3 C22 126.1(2) . . ?
C25 N4 C24 104.97(19) . . ?
C25 N4 Co2 126.94(16) . . ?
C24 N4 Co2 127.84(16) . . ?
C25 N5 C26 106.4(2) . . ?
C25 N5 C27 126.6(2) . . ?
C26 N5 C27 127.0(2) . . ?
C1 O2 Co1 101.52(16) . . ?
C16 O3 Co1 117.08(16) . 2_655 ?
C18 O5 Co1 117.03(15) . 2_655 ?
Co2 O1W H1A 118(2) . . ?
Co2 O1W H1B 111(2) . . ?
H1A O1W H1B 113(3) . . ?
Co2 O2W H2A 108(3) . . ?
Co2 O2W H2B 124(2) . . ?
H2A O2W H2B 107(3) . . ?
O4W O4W' O4W' 126.7(12) . 2_663 ?

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
O1W H1A O3W 0.81(3) 1.98(4) 2.759(17) 162(3) .
O2W H2A O6 0.74(3) 2.09(3) 2.824(3) 169(3) .
O1W H1B O6 0.76(3) 1.98(3) 2.724(3) 168(3) 2_664
O2W H2B O4 0.82(3) 1.86(3) 2.671(3) 169(3) 2_654

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.052
#=========================END
data_Compound-10

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H21 N Ni O9'
_chemical_formula_sum            'C18 H21 N Ni O9'
_chemical_formula_weight         454.07

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   'P 1 21/c 1'

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

_cell_length_a                   16.7460(8)
_cell_length_b                   7.0190(3)
_cell_length_c                   18.0500(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.184(6)
_cell_angle_gamma                90.00
_cell_volume                     1903.88(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3213
_cell_measurement_theta_min      2.8962
_cell_measurement_theta_max      29.1378

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             944
_exptl_absorpt_coefficient_mu    1.072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7830
_exptl_absorpt_correction_T_max  0.8557
_exptl_absorpt_process_details   
;
CrysAlis (Oxford Diffraction, 2006)
;
_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  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6811
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         25.02
_reflns_number_total             3341
_reflns_number_gt                3064
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 > 2σ(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)+(0.0293P)²+0.8629P] 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         3341
_refine_ls_number_parameters     284
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0237
_refine_ls_wR_factor_ref         0.0615
_refine_ls_wR_factor_gt          0.0596
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_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 0.428424(13) 0.22240(3) 0.335827(12) 0.01673(8) Uani 1 1 d . . .
C1 C 0.82783(12) -0.0814(3) 0.59774(12) 0.0319(4) Uani 1 1 d . . .
C2 C 0.92332(12) -0.0258(3) 0.62973(11) 0.0266(4) Uani 1 1 d . . .
C3 C 0.98235(13) -0.1316(3) 0.69643(12) 0.0352(5) Uani 1 1 d . . .
H3 H 0.9604 -0.2212 0.7208 0.042 Uiso 1 1 calc R . .
C4 C 1.07319(13) -0.1058(3) 0.72719(12) 0.0351(5) Uani 1 1 d . . .
H4 H 1.1122 -0.1783 0.7716 0.042 Uiso 1 1 calc R . .
C5 C 1.10521(12) 0.0274(3) 0.69170(12) 0.0330(4) Uani 1 1 d . . .
H5 H 1.1663 0.0437 0.7112 0.040 Uiso 1 1 calc R . .
C6 C 1.04724(12) 0.1375(3) 0.62716(12) 0.0294(4) Uani 1 1 d . . .
H6 H 1.0702 0.2295 0.6048 0.035 Uiso 1 1 calc R . .
C7 C 0.95504(12) 0.1152(2) 0.59434(11) 0.0239(4) Uani 1 1 d . . .
C8 C 0.89701(12) 0.2440(2) 0.52656(11) 0.0234(4) Uani 1 1 d . . .
C9 C 0.91762(12) 0.2831(3) 0.46129(11) 0.0264(4) Uani 1 1 d . . .
H9 H 0.9680 0.2288 0.4607 0.032 Uiso 1 1 calc R . .
C10 C 0.86421(12) 0.4016(3) 0.39744(11) 0.0260(4) Uani 1 1 d . . .
H10 H 0.8789 0.4237 0.3541 0.031 Uiso 1 1 calc R . .
C11 C 0.78924(11) 0.4883(2) 0.39634(10) 0.0221(4) Uani 1 1 d . . .
C12 C 0.77053(12) 0.4545(3) 0.46323(11) 0.0259(4) Uani 1 1 d . . .
H12 H 0.7220 0.5143 0.4653 0.031 Uiso 1 1 calc R . .
C13 C 0.82286(12) 0.3338(3) 0.52641(11) 0.0273(4) Uani 1 1 d . . .
H13 H 0.8083 0.3120 0.5698 0.033 Uiso 1 1 calc R . .
C14 C 0.73262(11) 0.6165(2) 0.32540(10) 0.0229(4) Uani 1 1 d . . .
H14A H 0.7181 0.7296 0.3478 0.028 Uiso 1 1 calc R . .
H14B H 0.7679 0.6568 0.2977 0.028 Uiso 1 1 calc R . .
C15 C 0.66447(12) 0.3608(2) 0.22267(11) 0.0247(4) Uani 1 1 d . . .
H15A H 0.6413 0.2500 0.2388 0.030 Uiso 1 1 calc R . .
H15B H 0.7282 0.3439 0.2438 0.030 Uiso 1 1 calc R . .
C16 C 0.62371(11) 0.3683(2) 0.12921(11) 0.0225(4) Uani 1 1 d . . .
C17 C 0.58690(11) 0.4871(3) 0.29986(10) 0.0213(4) Uani 1 1 d . . .
H17A H 0.5951 0.5807 0.3422 0.026 Uiso 1 1 calc R . .
H17B H 0.6020 0.3631 0.3261 0.026 Uiso 1 1 calc R . .
C18 C 0.49031(11) 0.4867(2) 0.23653(10) 0.0184(3) Uani 1 1 d . . .
N1 N 0.64783(9) 0.53170(19) 0.26239(8) 0.0176(3) Uani 1 1 d . . .
O1 O 0.79561(10) -0.1255(3) 0.64384(10) 0.0534(4) Uani 1 1 d . . .
O2 O 0.78395(10) -0.0854(2) 0.51719(9) 0.0407(4) Uani 1 1 d . . .
O3 O 0.63054(11) 0.22178(18) 0.09345(8) 0.0418(4) Uani 1 1 d . . .
O4 O 0.58678(8) 0.51958(16) 0.09274(7) 0.0233(3) Uani 1 1 d . . .
O5 O 0.47120(7) 0.56640(17) 0.16805(7) 0.0224(3) Uani 1 1 d . . .
O6 O 0.43246(8) 0.41646(17) 0.25414(7) 0.0249(3) Uani 1 1 d . . .
H2 H 0.729(2) -0.115(4) 0.5021(18) 0.075(9) Uiso 1 1 d . . .
O1W O 0.51897(10) 0.3730(2) 0.43682(9) 0.0305(3) Uani 1 1 d . . .
H1A H 0.5534(16) 0.323(4) 0.4820(16) 0.046 Uiso 1 1 d . . .
H1B H 0.5248(17) 0.469(4) 0.4402(16) 0.046 Uiso 1 1 d . . .
O2W O 0.32344(9) 0.37202(19) 0.33659(8) 0.0254(3) Uani 1 1 d . . .
H2A H 0.3362(15) 0.474(3) 0.3609(14) 0.038 Uiso 1 1 d . . .
H2B H 0.2944(15) 0.319(3) 0.3536(14) 0.038 Uiso 1 1 d . . .
O3W O 0.61351(10) -0.1764(2) 0.46391(9) 0.0401(4) Uani 1 1 d . . .
H3A H 0.5942(18) -0.103(4) 0.4268(17) 0.060 Uiso 1 1 d . . .
H3B H 0.6025(17) -0.131(4) 0.5005(17) 0.060 Uiso 1 1 d . . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O4 2.0109(11) 2_645 ?
Ni1 O6 2.0302(12) . ?
Ni1 O5 2.0330(11) 2_645 ?
Ni1 O2W 2.0531(12) . ?
Ni1 O1W 2.0736(14) . ?
Ni1 N1 2.1371(14) 2_645 ?
C1 O1 1.215(2) . ?
C1 O2 1.308(2) . ?
C1 C2 1.493(3) . ?
C2 C3 1.389(3) . ?
C2 C7 1.403(3) . ?
C3 C4 1.382(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.370(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.378(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.397(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.486(2) . ?
C8 C13 1.391(3) . ?
C8 C9 1.393(3) . ?
C9 C10 1.382(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.387(2) . ?
C10 H10 0.9300 . ?
C11 C12 1.395(2) . ?
C11 C14 1.509(2) . ?
C12 C13 1.380(3) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 N1 1.496(2) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N1 1.485(2) . ?
C15 C16 1.516(2) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 O3 1.246(2) . ?
C16 O4 1.259(2) . ?
C17 N1 1.4851(19) . ?
C17 C18 1.514(2) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 O6 1.2467(19) . ?
C18 O5 1.2627(19) . ?
N1 Ni1 2.1371(14) 2_655 ?
O2 H2 0.86(3) . ?
O4 Ni1 2.0109(11) 2_655 ?
O5 Ni1 2.0330(11) 2_655 ?
O1W H1A 0.84(3) . ?
O1W H1B 0.68(3) . ?
O2W H2A 0.82(2) . ?
O2W H2B 0.78(2) . ?
O3W H3A 0.79(3) . ?
O3W H3B 0.82(3) . ?

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
O4 Ni1 O6 174.18(5) 2_645 . ?
O4 Ni1 O5 88.93(5) 2_645 2_645 ?
O6 Ni1 O5 92.49(5) . 2_645 ?
O4 Ni1 O2W 90.38(5) 2_645 . ?
O6 Ni1 O2W 87.98(5) . . ?
O5 Ni1 O2W 177.67(5) 2_645 . ?
O4 Ni1 O1W 92.72(5) 2_645 . ?
O6 Ni1 O1W 92.91(5) . . ?
O5 Ni1 O1W 90.56(5) 2_645 . ?
O2W Ni1 O1W 91.69(6) . . ?
O4 Ni1 N1 83.69(5) 2_645 2_645 ?
O6 Ni1 N1 90.97(5) . 2_645 ?
O5 Ni1 N1 80.48(5) 2_645 2_645 ?
O2W Ni1 N1 97.24(5) . 2_645 ?
O1W Ni1 N1 170.39(6) . 2_645 ?
O1 C1 O2 123.65(18) . . ?
O1 C1 C2 121.70(18) . . ?
O2 C1 C2 114.59(16) . . ?
C3 C2 C7 120.28(17) . . ?
C3 C2 C1 115.26(16) . . ?
C7 C2 C1 124.37(17) . . ?
C4 C3 C2 120.97(18) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C5 C4 C3 119.36(18) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 120.21(18) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C7 122.01(17) . . ?
C5 C6 H6 119.0 . . ?
C7 C6 H6 119.0 . . ?
C6 C7 C2 117.11(16) . . ?
C6 C7 C8 118.66(16) . . ?
C2 C7 C8 124.21(16) . . ?
C13 C8 C9 117.57(16) . . ?
C13 C8 C7 122.40(16) . . ?
C9 C8 C7 120.00(16) . . ?
C10 C9 C8 120.87(17) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C11 121.63(16) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 H10 119.2 . . ?
C10 C11 C12 117.40(16) . . ?
C10 C11 C14 119.97(15) . . ?
C12 C11 C14 122.62(15) . . ?
C13 C12 C11 121.10(16) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C12 C13 C8 121.36(16) . . ?
C12 C13 H13 119.3 . . ?
C8 C13 H13 119.3 . . ?
N1 C14 C11 115.99(13) . . ?
N1 C14 H14A 108.3 . . ?
C11 C14 H14A 108.3 . . ?
N1 C14 H14B 108.3 . . ?
C11 C14 H14B 108.3 . . ?
H14A C14 H14B 107.4 . . ?
N1 C15 C16 114.90(14) . . ?
N1 C15 H15A 108.5 . . ?
C16 C15 H15A 108.5 . . ?
N1 C15 H15B 108.5 . . ?
C16 C15 H15B 108.5 . . ?
H15A C15 H15B 107.5 . . ?
O3 C16 O4 124.16(16) . . ?
O3 C16 C15 116.67(15) . . ?
O4 C16 C15 119.15(15) . . ?
N1 C17 C18 112.11(13) . . ?
N1 C17 H17A 109.2 . . ?
C18 C17 H17A 109.2 . . ?
N1 C17 H17B 109.2 . . ?
C18 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
O6 C18 O5 122.34(15) . . ?
O6 C18 C17 120.00(14) . . ?
O5 C18 C17 117.59(13) . . ?
C17 N1 C15 111.26(13) . . ?
C17 N1 C14 110.48(13) . . ?
C15 N1 C14 111.77(13) . . ?
C17 N1 Ni1 103.34(9) . 2_655 ?
C15 N1 Ni1 106.02(10) . 2_655 ?
C14 N1 Ni1 113.62(10) . 2_655 ?
C1 O2 H2 110.9(19) . . ?
C16 O4 Ni1 115.71(10) . 2_655 ?
C18 O5 Ni1 114.59(10) . 2_655 ?
C18 O6 Ni1 136.81(11) . . ?
Ni1 O1W H1A 124.3(17) . . ?
Ni1 O1W H1B 127(2) . . ?
H1A O1W H1B 109(3) . . ?
Ni1 O2W H2A 115.5(15) . . ?
Ni1 O2W H2B 116.3(17) . . ?
H2A O2W H2B 106(2) . . ?
H3A O3W H3B 106(3) . . ?

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 C1 C2 C3 39.6(3) . . . . ?
O2 C1 C2 C3 -137.90(19) . . . . ?
O1 C1 C2 C7 -143.8(2) . . . . ?
O2 C1 C2 C7 38.7(3) . . . . ?
C7 C2 C3 C4 -2.5(3) . . . . ?
C1 C2 C3 C4 174.24(19) . . . . ?
C2 C3 C4 C5 0.6(3) . . . . ?
C3 C4 C5 C6 1.4(3) . . . . ?
C4 C5 C6 C7 -1.6(3) . . . . ?
C5 C6 C7 C2 -0.3(3) . . . . ?
C5 C6 C7 C8 178.00(17) . . . . ?
C3 C2 C7 C6 2.3(3) . . . . ?
C1 C2 C7 C6 -174.14(17) . . . . ?
C3 C2 C7 C8 -175.87(18) . . . . ?
C1 C2 C7 C8 7.7(3) . . . . ?
C6 C7 C8 C13 -133.63(19) . . . . ?
C2 C7 C8 C13 44.5(3) . . . . ?
C6 C7 C8 C9 44.4(2) . . . . ?
C2 C7 C8 C9 -137.48(19) . . . . ?
C13 C8 C9 C10 -2.3(3) . . . . ?
C7 C8 C9 C10 179.61(17) . . . . ?
C8 C9 C10 C11 1.1(3) . . . . ?
C9 C10 C11 C12 1.2(3) . . . . ?
C9 C10 C11 C14 -179.91(16) . . . . ?
C10 C11 C12 C13 -2.3(3) . . . . ?
C14 C11 C12 C13 178.86(17) . . . . ?
C11 C12 C13 C8 1.1(3) . . . . ?
C9 C8 C13 C12 1.2(3) . . . . ?
C7 C8 C13 C12 179.26(17) . . . . ?
C10 C11 C14 N1 102.36(18) . . . . ?
C12 C11 C14 N1 -78.9(2) . . . . ?
N1 C15 C16 O3 -174.75(16) . . . . ?
N1 C15 C16 O4 6.3(2) . . . . ?
N1 C17 C18 O6 166.00(14) . . . . ?
N1 C17 C18 O5 -17.0(2) . . . . ?
C18 C17 N1 C15 -80.86(17) . . . . ?
C18 C17 N1 C14 154.38(14) . . . . ?
C18 C17 N1 Ni1 32.50(15) . . . 2_655 ?
C16 C15 N1 C17 110.71(16) . . . . ?
C16 C15 N1 C14 -125.26(16) . . . . ?
C16 C15 N1 Ni1 -0.96(17) . . . 2_655 ?
C11 C14 N1 C17 64.34(18) . . . . ?
C11 C14 N1 C15 -60.13(18) . . . . ?
C11 C14 N1 Ni1 179.94(11) . . . 2_655 ?
O3 C16 O4 Ni1 172.66(15) . . . 2_655 ?
C15 C16 O4 Ni1 -8.5(2) . . . 2_655 ?
O6 C18 O5 Ni1 166.32(12) . . . 2_655 ?
C17 C18 O5 Ni1 -10.64(18) . . . 2_655 ?
O5 C18 O6 Ni1 159.87(12) . . . . ?
C17 C18 O6 Ni1 -23.2(2) . . . . ?
O4 Ni1 O6 C18 -136.8(4) 2_645 . . . ?
O5 Ni1 O6 C18 -32.81(16) 2_645 . . . ?
O2W Ni1 O6 C18 149.47(17) . . . . ?
O1W Ni1 O6 C18 57.88(17) . . . . ?
N1 Ni1 O6 C18 -113.32(16) 2_645 . . . ?

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
O2 H2 O3W 0.86(3) 1.80(3) 2.656(2) 177(3) .
O1W H1A O3 0.84(3) 1.88(3) 2.695(2) 165(2) 4_566
O2W H2B O1 0.78(2) 2.04(2) 2.778(2) 158(2) 3_656
O3W H3A O5 0.79(3) 1.97(3) 2.758(2) 172(3) 2_645
O3W H3B O4 0.82(3) 1.96(3) 2.7817(19) 175(3) 4_566

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.047
#=========================END
