# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
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#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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data_lyp-1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C70 H54 Co3 N12 O16'
_chemical_formula_weight         1496.04

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   p-1

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

_cell_length_a                   10.193(4)
_cell_length_b                   13.722(5)
_cell_length_c                   14.606(6)
_cell_angle_alpha                107.685(6)
_cell_angle_beta                 102.170(7)
_cell_angle_gamma                111.188(6)
_cell_volume                     1692.5(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             767
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.7942
_exptl_absorpt_correction_T_max  0.8428
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8518
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.57
_diffrn_reflns_theta_max         25.10
_reflns_number_total             5909
_reflns_number_gt                4343
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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 > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2500P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5909
_refine_ls_number_parameters     457
_refine_ls_number_restraints     312
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0731
_refine_ls_wR_factor_ref         0.3114
_refine_ls_wR_factor_gt          0.2094
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.003

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 0.0000 0.0000 0.5000 0.0277(4) Uani 1 2 d SU . .
Co2 Co 0.23876(8) 1.09423(6) 1.08206(6) 0.0182(3) Uani 1 1 d U . .
C1 C -0.2486(9) 0.3477(6) 0.4943(7) 0.052(2) Uani 1 1 d U . .
H1A H -0.3334 0.3230 0.4375 0.063 Uiso 1 1 calc R . .
C2 C -0.1689(8) 0.4606(6) 0.5595(6) 0.0442(19) Uani 1 1 d U . .
H2A H -0.2030 0.5120 0.5489 0.053 Uiso 1 1 calc R . .
C3 C -0.0364(7) 0.5013(5) 0.6425(5) 0.0294(15) Uani 1 1 d U . .
C4 C 0.0102(7) 0.4233(5) 0.6588(5) 0.0269(14) Uani 1 1 d U . .
H4A H 0.0987 0.4501 0.7135 0.032 Uiso 1 1 calc R . .
C5 C -0.0715(7) 0.3041(5) 0.5955(5) 0.0284(15) Uani 1 1 d U . .
C6 C -0.2030(8) 0.2669(5) 0.5124(6) 0.0430(19) Uani 1 1 d U . .
H6A H -0.2604 0.1890 0.4691 0.052 Uiso 1 1 calc R . .
C7 C 0.2168(6) 0.6737(5) 0.7422(5) 0.0226(13) Uani 1 1 d U . .
H7A H 0.2606 0.6290 0.7141 0.027 Uiso 1 1 calc R . .
C8 C 0.3068(6) 0.7853(5) 0.8115(4) 0.0176(12) Uani 1 1 d U . .
C9 C 0.2457(6) 0.8565(5) 0.8506(5) 0.0196(12) Uani 1 1 d U . .
H9A H 0.3079 0.9326 0.8973 0.024 Uiso 1 1 calc R . .
C10 C 0.0869(6) 0.8113(4) 0.8181(5) 0.0177(12) Uani 1 1 d U . .
C11 C -0.0022(6) 0.6964(5) 0.7477(5) 0.0215(13) Uani 1 1 d U . .
H11A H -0.1065 0.6677 0.7241 0.026 Uiso 1 1 calc R . .
C12 C 0.0570(6) 0.6248(5) 0.7121(5) 0.0223(13) Uani 1 1 d U . .
C13 C 0.4784(6) 0.8325(5) 0.8465(5) 0.0211(13) Uani 1 1 d U . .
C14 C -0.0126(7) 0.2228(5) 0.6110(6) 0.0277(15) Uani 1 1 d U . .
C15 C 0.2217(10) 0.6410(6) 1.1633(7) 0.047(2) Uani 1 1 d U . .
H15A H 0.2214 0.6795 1.2277 0.056 Uiso 1 1 calc R . .
C16 C 0.2422(10) 0.5416(6) 1.1422(6) 0.045(2) Uani 1 1 d U . .
H16A H 0.2471 0.5098 1.1900 0.054 Uiso 1 1 calc R . .
C17 C 0.2549(7) 0.4927(5) 1.0500(5) 0.0284(14) Uani 1 1 d U . .
C18 C 0.2332(10) 0.5313(6) 0.9732(6) 0.046(2) Uani 1 1 d U . .
H18A H 0.2337 0.4928 0.9088 0.055 Uiso 1 1 calc R . .
C19 C 0.2107(11) 0.6285(7) 0.9945(7) 0.051(2) Uani 1 1 d U . .
H19A H 0.2015 0.6581 0.9454 0.061 Uiso 1 1 calc R . .
C20 C 0.2019(8) 0.6814(5) 1.0882(5) 0.0314(15) Uani 1 1 d U . .
C21 C 0.0212(6) 0.8883(4) 0.8655(5) 0.0197(13) Uani 1 1 d U . .
C22 C 0.0768(8) 0.8001(5) 1.1519(6) 0.0332(16) Uani 1 1 d U . .
H22A H 0.0154 0.7519 1.1748 0.040 Uiso 1 1 calc R . .
C23 C 0.2427(8) 0.8724(5) 1.0884(6) 0.0341(16) Uani 1 1 d U . .
H23A H 0.3174 0.8823 1.0599 0.041 Uiso 1 1 calc R . .
C24 C 0.0847(8) 0.9001(5) 1.1557(6) 0.0318(15) Uani 1 1 d U . .
H24A H 0.0283 0.9335 1.1820 0.038 Uiso 1 1 calc R . .
C25 C 0.2406(7) 1.3175(5) 1.0732(5) 0.0287(14) Uani 1 1 d U . .
H25A H 0.1904 1.3219 1.1194 0.034 Uiso 1 1 calc R . .
C26 C 0.3478(9) 1.2595(6) 0.9742(6) 0.0401(18) Uani 1 1 d U . .
H26A H 0.3861 1.2149 0.9384 0.048 Uiso 1 1 calc R . .
C27 C 0.3487(9) 1.3579(6) 0.9652(7) 0.0441(19) Uani 1 1 d U . .
H27A H 0.3878 1.3925 0.9248 0.053 Uiso 1 1 calc R . .
C28 C -0.4507(8) -0.4123(5) 0.5980(6) 0.0320(16) Uani 1 1 d U . .
H28 H -0.4192 -0.3546 0.6631 0.038 Uiso 1 1 calc R . .
C29 C -0.4675(8) -0.4713(5) 0.4234(6) 0.0348(17) Uani 1 1 d U . .
H29 H -0.4455 -0.4507 0.3714 0.042 Uiso 1 1 calc R . .
C30 C -0.4198(7) -0.3878(5) 0.5202(5) 0.0249(14) Uani 1 1 d U . .
C31 C -0.2414(8) -0.0805(6) 0.5953(6) 0.0420(19) Uani 1 1 d U . .
H31A H -0.2241 -0.0051 0.6283 0.050 Uiso 1 1 calc R . .
C32 C -0.3342(8) -0.1712(5) 0.6064(6) 0.0363(18) Uani 1 1 d U . .
H32A H -0.3885 -0.1697 0.6501 0.044 Uiso 1 1 calc R . .
C33 C -0.2370(9) -0.2299(6) 0.4937(7) 0.045(2) Uani 1 1 d U . .
H33A H -0.2153 -0.2765 0.4444 0.055 Uiso 1 1 calc R . .
C34 C 0.2261(14) 0.0301(9) 0.7108(9) 0.079(3) Uani 1 1 d U . .
H34A H 0.2270 0.0481 0.7806 0.095 Uiso 1 1 calc R . .
H34B H 0.1848 -0.0525 0.6744 0.095 Uiso 1 1 calc R . .
C35 C 0.3769(16) 0.0875(15) 0.7118(13) 0.141(6) Uani 1 1 d U . .
H35A H 0.4406 0.0616 0.7450 0.211 Uiso 1 1 calc R . .
H35B H 0.4165 0.1691 0.7487 0.211 Uiso 1 1 calc R . .
H35C H 0.3737 0.0699 0.6423 0.211 Uiso 1 1 calc R . .
N1 N 0.2837(6) 1.2383(4) 1.0421(4) 0.0266(12) Uani 1 1 d U . .
N2 N 0.2786(7) 1.3918(4) 1.0295(5) 0.0330(14) Uani 1 1 d U . .
N3 N 0.1769(6) 0.7818(4) 1.1076(5) 0.0325(13) Uani 1 1 d U . .
N4 N 0.1888(6) 0.9473(4) 1.1149(4) 0.0298(12) Uani 1 1 d U . .
N5 N -0.1772(7) -0.1162(4) 0.5284(5) 0.0358(14) Uani 1 1 d U . .
N6 N -0.3331(6) -0.2682(4) 0.5394(5) 0.0310(13) Uani 1 1 d U . .
O1 O 0.1082(4) 0.9896(3) 0.9300(3) 0.0243(10) Uani 1 1 d U . .
O2 O -0.1219(4) 0.8427(3) 0.8371(3) 0.0252(10) Uani 1 1 d U . .
O3 O 0.5380(5) 0.7937(4) 0.7855(4) 0.0293(11) Uani 1 1 d U . .
O4 O 0.5571(4) 0.9086(3) 0.9364(4) 0.0294(11) Uani 1 1 d U . .
O5 O 0.1000(6) 0.2604(4) 0.6912(4) 0.0395(12) Uani 1 1 d U . .
O6 O -0.0764(5) 0.1238(4) 0.5416(4) 0.0388(12) Uani 1 1 d U . .
O7 O 0.1367(7) 0.0731(5) 0.6578(4) 0.0532(15) Uani 1 1 d U . .
O8 O 0.401(3) 0.4559(18) 0.7777(18) 0.306(11) Uani 1 1 d U . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O6 2.096(5) 2_556 ?
Co1 O6 2.096(5) . ?
Co1 O7 2.119(6) 2_556 ?
Co1 O7 2.119(6) . ?
Co1 N5 2.148(5) 2_556 ?
Co1 N5 2.148(5) . ?
Co2 O1 2.049(4) . ?
Co2 O2 2.069(4) 2_577 ?
Co2 N4 2.123(5) . ?
Co2 N1 2.148(5) . ?
Co2 O4 2.166(4) 2_677 ?
Co2 O3 2.256(5) 2_677 ?
C1 C2 1.355(10) . ?
C1 C6 1.419(11) . ?
C1 H1A 0.9300 . ?
C2 C3 1.399(10) . ?
C2 H2A 0.9300 . ?
C3 C4 1.380(9) . ?
C3 C12 1.479(8) . ?
C4 C5 1.412(8) . ?
C4 H4A 0.9300 . ?
C5 C6 1.404(10) . ?
C5 C14 1.496(9) . ?
C6 H6A 0.9300 . ?
C7 C8 1.365(8) . ?
C7 C12 1.424(8) . ?
C7 H7A 0.9300 . ?
C8 C9 1.385(8) . ?
C8 C13 1.531(7) . ?
C9 C10 1.414(7) . ?
C9 H9A 0.9300 . ?
C10 C11 1.398(8) . ?
C10 C21 1.519(7) . ?
C11 C12 1.360(8) . ?
C11 H11A 0.9300 . ?
C13 O4 1.256(8) . ?
C13 O3 1.273(7) . ?
C14 O6 1.242(8) . ?
C14 O5 1.262(9) . ?
C15 C20 1.382(10) . ?
C15 C16 1.407(9) . ?
C15 H15A 0.9300 . ?
C16 C17 1.366(10) . ?
C16 H16A 0.9300 . ?
C17 C18 1.389(10) . ?
C17 N2 1.445(7) 1_545 ?
C18 C19 1.389(10) . ?
C18 H18A 0.9300 . ?
C19 C20 1.379(11) . ?
C19 H19A 0.9300 . ?
C20 N3 1.445(8) . ?
C21 O1 1.252(7) . ?
C21 O2 1.272(7) . ?
C22 C24 1.328(9) . ?
C22 N3 1.375(8) . ?
C22 H22A 0.9300 . ?
C23 N4 1.328(8) . ?
C23 N3 1.328(8) . ?
C23 H23A 0.9300 . ?
C24 N4 1.379(8) . ?
C24 H24A 0.9300 . ?
C25 N1 1.307(8) . ?
C25 N2 1.345(8) . ?
C25 H25A 0.9300 . ?
C26 N1 1.344(9) . ?
C26 C27 1.394(9) . ?
C26 H26A 0.9300 . ?
C27 N2 1.366(9) . ?
C27 H27A 0.9300 . ?
C28 C30 1.345(9) . ?
C28 C29 1.403(8) 2_446 ?
C28 H28 0.9300 . ?
C29 C30 1.368(10) . ?
C29 C28 1.403(8) 2_446 ?
C29 H29 0.9300 . ?
C30 N6 1.456(7) . ?
C31 C32 1.344(8) . ?
C31 N5 1.353(9) . ?
C31 H31A 0.9300 . ?
C32 N6 1.398(8) . ?
C32 H32A 0.9300 . ?
C33 N5 1.329(8) . ?
C33 N6 1.341(8) . ?
C33 H33A 0.9300 . ?
C34 C35 1.446(17) . ?
C34 O7 1.465(12) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
N2 C17 1.445(7) 1_565 ?
O2 Co2 2.069(4) 2_577 ?
O3 Co2 2.256(5) 2_677 ?
O4 Co2 2.166(4) 2_677 ?

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
O6 Co1 O6 180.0(3) 2_556 . ?
O6 Co1 O7 86.5(2) 2_556 2_556 ?
O6 Co1 O7 93.5(2) . 2_556 ?
O6 Co1 O7 93.5(2) 2_556 . ?
O6 Co1 O7 86.5(2) . . ?
O7 Co1 O7 180.000(1) 2_556 . ?
O6 Co1 N5 90.1(2) 2_556 2_556 ?
O6 Co1 N5 89.9(2) . 2_556 ?
O7 Co1 N5 89.4(2) 2_556 2_556 ?
O7 Co1 N5 90.6(2) . 2_556 ?
O6 Co1 N5 89.9(2) 2_556 . ?
O6 Co1 N5 90.1(2) . . ?
O7 Co1 N5 90.6(2) 2_556 . ?
O7 Co1 N5 89.4(2) . . ?
N5 Co1 N5 180.000(1) 2_556 . ?
O1 Co2 O2 112.31(17) . 2_577 ?
O1 Co2 N4 89.8(2) . . ?
O2 Co2 N4 95.7(2) 2_577 . ?
O1 Co2 N1 87.83(19) . . ?
O2 Co2 N1 85.24(19) 2_577 . ?
N4 Co2 N1 177.6(2) . . ?
O1 Co2 O4 93.84(17) . 2_677 ?
O2 Co2 O4 153.19(18) 2_577 2_677 ?
N4 Co2 O4 90.01(19) . 2_677 ?
N1 Co2 O4 90.12(18) . 2_677 ?
O1 Co2 O3 153.04(16) . 2_677 ?
O2 Co2 O3 93.52(16) 2_577 2_677 ?
N4 Co2 O3 95.42(19) . 2_677 ?
N1 Co2 O3 86.72(19) . 2_677 ?
O4 Co2 O3 59.81(16) 2_677 2_677 ?
C2 C1 C6 120.1(7) . . ?
C2 C1 H1A 119.9 . . ?
C6 C1 H1A 119.9 . . ?
C1 C2 C3 121.4(7) . . ?
C1 C2 H2A 119.3 . . ?
C3 C2 H2A 119.3 . . ?
C4 C3 C2 118.5(6) . . ?
C4 C3 C12 118.8(6) . . ?
C2 C3 C12 122.7(6) . . ?
C3 C4 C5 122.4(6) . . ?
C3 C4 H4A 118.8 . . ?
C5 C4 H4A 118.8 . . ?
C6 C5 C4 117.3(6) . . ?
C6 C5 C14 121.5(6) . . ?
C4 C5 C14 121.0(6) . . ?
C5 C6 C1 120.2(6) . . ?
C5 C6 H6A 119.9 . . ?
C1 C6 H6A 119.9 . . ?
C8 C7 C12 120.9(5) . . ?
C8 C7 H7A 119.5 . . ?
C12 C7 H7A 119.5 . . ?
C7 C8 C9 121.2(5) . . ?
C7 C8 C13 119.3(5) . . ?
C9 C8 C13 119.5(5) . . ?
C8 C9 C10 118.8(5) . . ?
C8 C9 H9A 120.6 . . ?
C10 C9 H9A 120.6 . . ?
C11 C10 C9 118.6(5) . . ?
C11 C10 C21 122.9(5) . . ?
C9 C10 C21 118.4(5) . . ?
C12 C11 C10 122.9(5) . . ?
C12 C11 H11A 118.5 . . ?
C10 C11 H11A 118.5 . . ?
C11 C12 C7 117.2(5) . . ?
C11 C12 C3 123.3(5) . . ?
C7 C12 C3 119.4(5) . . ?
O4 C13 O3 121.5(5) . . ?
O4 C13 C8 118.3(5) . . ?
O3 C13 C8 120.2(5) . . ?
O6 C14 O5 125.1(6) . . ?
O6 C14 C5 116.8(7) . . ?
O5 C14 C5 118.1(6) . . ?
C20 C15 C16 120.0(7) . . ?
C20 C15 H15A 120.0 . . ?
C16 C15 H15A 120.0 . . ?
C17 C16 C15 118.5(7) . . ?
C17 C16 H16A 120.8 . . ?
C15 C16 H16A 120.8 . . ?
C16 C17 C18 122.0(6) . . ?
C16 C17 N2 118.3(6) . 1_545 ?
C18 C17 N2 119.5(6) . 1_545 ?
C19 C18 C17 118.6(7) . . ?
C19 C18 H18A 120.7 . . ?
C17 C18 H18A 120.7 . . ?
C20 C19 C18 120.3(7) . . ?
C20 C19 H19A 119.8 . . ?
C18 C19 H19A 119.8 . . ?
C19 C20 C15 120.3(6) . . ?
C19 C20 N3 119.0(6) . . ?
C15 C20 N3 120.7(6) . . ?
O1 C21 O2 124.4(5) . . ?
O1 C21 C10 119.4(5) . . ?
O2 C21 C10 116.2(5) . . ?
C24 C22 N3 106.7(5) . . ?
C24 C22 H22A 126.7 . . ?
N3 C22 H22A 126.7 . . ?
N4 C23 N3 111.7(6) . . ?
N4 C23 H23A 124.1 . . ?
N3 C23 H23A 124.1 . . ?
C22 C24 N4 110.2(6) . . ?
C22 C24 H24A 124.9 . . ?
N4 C24 H24A 124.9 . . ?
N1 C25 N2 111.1(6) . . ?
N1 C25 H25A 124.4 . . ?
N2 C25 H25A 124.4 . . ?
N1 C26 C27 110.2(6) . . ?
N1 C26 H26A 124.9 . . ?
C27 C26 H26A 124.9 . . ?
N2 C27 C26 103.9(6) . . ?
N2 C27 H27A 128.1 . . ?
C26 C27 H27A 128.1 . . ?
C30 C28 C29 117.1(6) . 2_446 ?
C30 C28 H28 121.5 . . ?
C29 C28 H28 121.4 2_446 . ?
C30 C29 C28 120.6(6) . 2_446 ?
C30 C29 H29 119.7 . . ?
C28 C29 H29 119.7 2_446 . ?
C28 C30 C29 122.3(5) . . ?
C28 C30 N6 119.0(6) . . ?
C29 C30 N6 118.7(5) . . ?
C32 C31 N5 109.4(6) . . ?
C32 C31 H31A 125.3 . . ?
N5 C31 H31A 125.3 . . ?
C31 C32 N6 106.6(6) . . ?
C31 C32 H32A 126.7 . . ?
N6 C32 H32A 126.7 . . ?
N5 C33 N6 110.6(6) . . ?
N5 C33 H33A 124.7 . . ?
N6 C33 H33A 124.7 . . ?
C35 C34 O7 105.9(10) . . ?
C35 C34 H34A 110.6 . . ?
O7 C34 H34A 110.6 . . ?
C35 C34 H34B 110.6 . . ?
O7 C34 H34B 110.6 . . ?
H34A C34 H34B 108.7 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C25 N1 C26 106.5(5) . . ?
C25 N1 Co2 125.7(4) . . ?
C26 N1 Co2 127.6(4) . . ?
C25 N2 C27 108.3(5) . . ?
C25 N2 C17 125.9(6) . 1_565 ?
C27 N2 C17 125.7(5) . 1_565 ?
C23 N3 C22 106.9(5) . . ?
C23 N3 C20 128.6(6) . . ?
C22 N3 C20 124.5(5) . . ?
C23 N4 C24 104.5(5) . . ?
C23 N4 Co2 125.4(4) . . ?
C24 N4 Co2 129.7(4) . . ?
C33 N5 C31 107.1(5) . . ?
C33 N5 Co1 129.6(5) . . ?
C31 N5 Co1 123.2(4) . . ?
C33 N6 C32 106.2(5) . . ?
C33 N6 C30 126.0(5) . . ?
C32 N6 C30 127.8(5) . . ?
C21 O1 Co2 145.3(4) . . ?
C21 O2 Co2 124.4(4) . 2_577 ?
C13 O3 Co2 87.0(4) . 2_677 ?
C13 O4 Co2 91.5(3) . 2_677 ?
C14 O6 Co1 131.1(5) . . ?
C34 O7 Co1 128.6(6) . . ?

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 3.4(13) . . . . ?
C1 C2 C3 C4 -1.8(11) . . . . ?
C1 C2 C3 C12 177.0(7) . . . . ?
C2 C3 C4 C5 -0.6(10) . . . . ?
C12 C3 C4 C5 -179.4(6) . . . . ?
C3 C4 C5 C6 1.2(10) . . . . ?
C3 C4 C5 C14 175.9(6) . . . . ?
C4 C5 C6 C1 0.4(10) . . . . ?
C14 C5 C6 C1 -174.3(7) . . . . ?
C2 C1 C6 C5 -2.7(12) . . . . ?
C12 C7 C8 C9 -3.7(9) . . . . ?
C12 C7 C8 C13 176.4(5) . . . . ?
C7 C8 C9 C10 0.6(9) . . . . ?
C13 C8 C9 C10 -179.5(5) . . . . ?
C8 C9 C10 C11 0.0(9) . . . . ?
C8 C9 C10 C21 176.9(5) . . . . ?
C9 C10 C11 C12 2.7(9) . . . . ?
C21 C10 C11 C12 -174.1(6) . . . . ?
C10 C11 C12 C7 -5.6(9) . . . . ?
C10 C11 C12 C3 176.2(6) . . . . ?
C8 C7 C12 C11 6.0(9) . . . . ?
C8 C7 C12 C3 -175.7(6) . . . . ?
C4 C3 C12 C11 -139.5(6) . . . . ?
C2 C3 C12 C11 41.7(10) . . . . ?
C4 C3 C12 C7 42.3(9) . . . . ?
C2 C3 C12 C7 -136.5(7) . . . . ?
C7 C8 C13 O4 -148.4(6) . . . . ?
C9 C8 C13 O4 31.8(8) . . . . ?
C7 C8 C13 O3 30.8(8) . . . . ?
C9 C8 C13 O3 -149.1(6) . . . . ?
C6 C5 C14 O6 7.1(9) . . . . ?
C4 C5 C14 O6 -167.4(6) . . . . ?
C6 C5 C14 O5 -175.2(6) . . . . ?
C4 C5 C14 O5 10.4(9) . . . . ?
C20 C15 C16 C17 5.5(13) . . . . ?
C15 C16 C17 C18 -6.5(12) . . . . ?
C15 C16 C17 N2 178.9(7) . . . 1_545 ?
C16 C17 C18 C19 5.6(12) . . . . ?
N2 C17 C18 C19 -180.0(7) 1_545 . . . ?
C17 C18 C19 C20 -3.5(13) . . . . ?
C18 C19 C20 C15 2.7(13) . . . . ?
C18 C19 C20 N3 -179.4(7) . . . . ?
C16 C15 C20 C19 -3.7(13) . . . . ?
C16 C15 C20 N3 178.4(7) . . . . ?
C11 C10 C21 O1 178.3(6) . . . . ?
C9 C10 C21 O1 1.5(8) . . . . ?
C11 C10 C21 O2 -0.5(9) . . . . ?
C9 C10 C21 O2 -177.3(5) . . . . ?
N3 C22 C24 N4 -0.2(9) . . . . ?
N1 C26 C27 N2 -1.4(9) . . . . ?
C29 C28 C30 C29 1.3(12) 2_446 . . . ?
C29 C28 C30 N6 -179.0(6) 2_446 . . . ?
C28 C29 C30 C28 -1.3(12) 2_446 . . . ?
C28 C29 C30 N6 179.0(6) 2_446 . . . ?
N5 C31 C32 N6 -3.0(9) . . . . ?
N2 C25 N1 C26 -1.6(8) . . . . ?
N2 C25 N1 Co2 -176.2(4) . . . . ?
C27 C26 N1 C25 1.9(9) . . . . ?
C27 C26 N1 Co2 176.3(5) . . . . ?
O1 Co2 N1 C25 114.3(6) . . . . ?
O2 Co2 N1 C25 1.7(5) 2_577 . . . ?
N4 Co2 N1 C25 115(5) . . . . ?
O4 Co2 N1 C25 -151.8(6) 2_677 . . . ?
O3 Co2 N1 C25 -92.1(6) 2_677 . . . ?
O1 Co2 N1 C26 -59.1(6) . . . . ?
O2 Co2 N1 C26 -171.7(6) 2_577 . . . ?
N4 Co2 N1 C26 -58(5) . . . . ?
O4 Co2 N1 C26 34.8(6) 2_677 . . . ?
O3 Co2 N1 C26 94.5(6) 2_677 . . . ?
N1 C25 N2 C27 0.8(9) . . . . ?
N1 C25 N2 C17 -176.9(6) . . . 1_565 ?
C26 C27 N2 C25 0.3(9) . . . . ?
C26 C27 N2 C17 178.0(7) . . . 1_565 ?
N4 C23 N3 C22 -1.7(9) . . . . ?
N4 C23 N3 C20 178.8(7) . . . . ?
C24 C22 N3 C23 1.1(8) . . . . ?
C24 C22 N3 C20 -179.3(7) . . . . ?
C19 C20 N3 C23 -45.1(11) . . . . ?
C15 C20 N3 C23 132.9(8) . . . . ?
C19 C20 N3 C22 135.5(8) . . . . ?
C15 C20 N3 C22 -46.6(11) . . . . ?
N3 C23 N4 C24 1.5(8) . . . . ?
N3 C23 N4 Co2 -171.9(5) . . . . ?
C22 C24 N4 C23 -0.7(8) . . . . ?
C22 C24 N4 Co2 172.3(5) . . . . ?
O1 Co2 N4 C23 72.3(6) . . . . ?
O2 Co2 N4 C23 -175.3(6) 2_577 . . . ?
N1 Co2 N4 C23 72(5) . . . . ?
O4 Co2 N4 C23 -21.6(6) 2_677 . . . ?
O3 Co2 N4 C23 -81.2(6) 2_677 . . . ?
O1 Co2 N4 C24 -99.4(6) . . . . ?
O2 Co2 N4 C24 13.0(6) 2_577 . . . ?
N1 Co2 N4 C24 -100(5) . . . . ?
O4 Co2 N4 C24 166.7(6) 2_677 . . . ?
O3 Co2 N4 C24 107.1(6) 2_677 . . . ?
N6 C33 N5 C31 -2.7(10) . . . . ?
N6 C33 N5 Co1 172.7(5) . . . . ?
C32 C31 N5 C33 3.5(10) . . . . ?
C32 C31 N5 Co1 -172.2(5) . . . . ?
O6 Co1 N5 C33 -21.1(8) 2_556 . . . ?
O6 Co1 N5 C33 158.9(8) . . . . ?
O7 Co1 N5 C33 65.4(8) 2_556 . . . ?
O7 Co1 N5 C33 -114.6(8) . . . . ?
N5 Co1 N5 C33 0(100) 2_556 . . . ?
O6 Co1 N5 C31 153.6(6) 2_556 . . . ?
O6 Co1 N5 C31 -26.4(6) . . . . ?
O7 Co1 N5 C31 -119.9(6) 2_556 . . . ?
O7 Co1 N5 C31 60.1(6) . . . . ?
N5 Co1 N5 C31 0(100) 2_556 . . . ?
N5 C33 N6 C32 0.8(10) . . . . ?
N5 C33 N6 C30 179.7(7) . . . . ?
C31 C32 N6 C33 1.4(9) . . . . ?
C31 C32 N6 C30 -177.5(7) . . . . ?
C28 C30 N6 C33 147.8(8) . . . . ?
C29 C30 N6 C33 -32.5(11) . . . . ?
C28 C30 N6 C32 -33.5(10) . . . . ?
C29 C30 N6 C32 146.2(8) . . . . ?
O2 C21 O1 Co2 94.2(8) . . . . ?
C10 C21 O1 Co2 -84.5(8) . . . . ?
O2 Co2 O1 C21 -91.7(6) 2_577 . . . ?
N4 Co2 O1 C21 4.4(7) . . . . ?
N1 Co2 O1 C21 -175.6(7) . . . . ?
O4 Co2 O1 C21 94.4(7) 2_677 . . . ?
O3 Co2 O1 C21 106.0(7) 2_677 . . . ?
O1 C21 O2 Co2 -18.4(8) . . . 2_577 ?
C10 C21 O2 Co2 160.3(4) . . . 2_577 ?
O4 C13 O3 Co2 3.9(6) . . . 2_677 ?
C8 C13 O3 Co2 -175.2(5) . . . 2_677 ?
O3 C13 O4 Co2 -4.1(6) . . . 2_677 ?
C8 C13 O4 Co2 175.1(4) . . . 2_677 ?
O5 C14 O6 Co1 -21.4(9) . . . . ?
C5 C14 O6 Co1 156.3(4) . . . . ?
O6 Co1 O6 C14 17(100) 2_556 . . . ?
O7 Co1 O6 C14 -149.5(6) 2_556 . . . ?
O7 Co1 O6 C14 30.5(6) . . . . ?
N5 Co1 O6 C14 -60.0(6) 2_556 . . . ?
N5 Co1 O6 C14 120.0(6) . . . . ?
C35 C34 O7 Co1 94.5(10) . . . . ?
O6 Co1 O7 C34 -9.2(8) 2_556 . . . ?
O6 Co1 O7 C34 170.8(8) . . . . ?
O7 Co1 O7 C34 0(100) 2_556 . . . ?
N5 Co1 O7 C34 -99.4(8) 2_556 . . . ?
N5 Co1 O7 C34 80.6(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         1.095
_refine_diff_density_min         -1.796
_refine_diff_density_rms         0.297
_database_code_depnum_ccdc_archive 'CCDC 991512'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_added_by_encifer


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H50 Mn3 N8 O20'
_chemical_formula_weight         1295.84

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.1250(8)
_cell_length_b                   10.7664(9)
_cell_length_c                   13.2928(12)
_cell_angle_alpha                86.5210(10)
_cell_angle_beta                 73.151(2)
_cell_angle_gamma                85.3170(10)
_cell_volume                     1381.2(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1408
_cell_measurement_theta_min      2.437
_cell_measurement_theta_max      22.696

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             665
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8037
_exptl_absorpt_correction_T_max  0.8383
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7599
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         26.24
_reflns_number_total             5398
_reflns_number_gt                3781
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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 > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0940P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5398
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_ref         0.1705
_refine_ls_wR_factor_gt          0.1315
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_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
Mn1 Mn -0.13841(6) 0.59120(5) 0.30786(5) 0.02791(19) Uani 1 1 d . . .
Mn2 Mn 0.0000 1.0000 0.0000 0.0315(2) Uani 1 2 d S . .
C1 C 0.1205(4) 1.2501(4) 0.0723(3) 0.0300(9) Uani 1 1 d . . .
C2 C 0.1999(4) 1.2260(3) 0.1522(3) 0.0277(8) Uani 1 1 d . . .
C3 C 0.2538(4) 1.3219(4) 0.1908(3) 0.0355(10) Uani 1 1 d . . .
H3 H 0.2349 1.4046 0.1722 0.043 Uiso 1 1 calc R . .
C4 C 0.3357(5) 1.2922(4) 0.2568(3) 0.0403(10) Uani 1 1 d . . .
H4 H 0.3718 1.3561 0.2824 0.048 Uiso 1 1 calc R . .
C5 C 0.3653(4) 1.1705(4) 0.2857(3) 0.0366(10) Uani 1 1 d . . .
H5 H 0.4228 1.1527 0.3288 0.044 Uiso 1 1 calc R . .
C6 C 0.3089(4) 1.0745(4) 0.2501(3) 0.0304(9) Uani 1 1 d . . .
C7 C 0.2254(4) 1.1043(3) 0.1843(3) 0.0268(8) Uani 1 1 d . . .
H7 H 0.1858 1.0407 0.1612 0.032 Uiso 1 1 calc R . .
C8 C 0.3339(4) 0.9402(4) 0.2777(3) 0.0290(9) Uani 1 1 d . . .
C9 C 0.4622(4) 0.8869(4) 0.2824(3) 0.0305(9) Uani 1 1 d . . .
H9 H 0.5360 0.9369 0.2726 0.037 Uiso 1 1 calc R . .
C10 C 0.4801(4) 0.7582(4) 0.3021(3) 0.0314(9) Uani 1 1 d . . .
C11 C 0.6205(4) 0.6998(4) 0.2997(3) 0.0354(10) Uani 1 1 d . . .
C12 C 0.3701(4) 0.6829(4) 0.3190(3) 0.0315(9) Uani 1 1 d . . .
H12 H 0.3824 0.5976 0.3325 0.038 Uiso 1 1 calc R . .
C13 C 0.2415(4) 0.7360(4) 0.3157(3) 0.0302(9) Uani 1 1 d . . .
C14 C 0.1199(4) 0.6576(4) 0.3299(3) 0.0307(9) Uani 1 1 d . . .
C15 C 0.2253(4) 0.8619(4) 0.2940(3) 0.0292(9) Uani 1 1 d . . .
H15 H 0.1395 0.8960 0.2900 0.035 Uiso 1 1 calc R . .
C16 C -0.1722(5) 0.3047(4) 0.2686(4) 0.0406(11) Uani 1 1 d . . .
H16 H -0.2144 0.3268 0.2160 0.049 Uiso 1 1 calc R . .
C17 C -0.1482(5) 0.1885(4) 0.3020(4) 0.0422(11) Uani 1 1 d . . .
H17 H -0.1692 0.1158 0.2772 0.051 Uiso 1 1 calc R . .
C18 C -0.0732(4) 0.3179(3) 0.3892(3) 0.0354(10) Uani 1 1 d . . .
H18 H -0.0326 0.3491 0.4360 0.043 Uiso 1 1 calc R . .
C19 C -0.4256(4) 1.1549(4) 0.0338(4) 0.0406(11) Uani 1 1 d . . .
H19 H -0.5191 1.1451 0.0442 0.049 Uiso 1 1 calc R . .
C20 C -0.3274(4) 1.0644(4) 0.0380(3) 0.0358(10) Uani 1 1 d . . .
H20 H -0.3429 0.9805 0.0528 0.043 Uiso 1 1 calc R . .
C21 C -0.2256(4) 1.2346(4) 0.0012(3) 0.0371(10) Uani 1 1 d . . .
H21 H -0.1582 1.2922 -0.0148 0.045 Uiso 1 1 calc R . .
C22 C -0.4285(4) 1.3860(4) 0.0036(3) 0.0323(9) Uani 1 1 d . . .
C23 C -0.5288(4) 1.3987(4) -0.0489(3) 0.0376(10) Uani 1 1 d . . .
H23 H -0.5481 1.3310 -0.0812 0.045 Uiso 1 1 calc R . .
C24 C -0.3991(4) 1.4850(4) 0.0527(3) 0.0375(10) Uani 1 1 d . . .
H24 H -0.3319 1.4748 0.0882 0.045 Uiso 1 1 calc R . .
C25 C -0.0413(4) 0.0960(3) 0.4411(3) 0.0323(9) Uani 1 1 d . . .
C26 C -0.1062(4) -0.0151(4) 0.4564(3) 0.0361(10) Uani 1 1 d . . .
H26 H -0.1773 -0.0245 0.4268 0.043 Uiso 1 1 calc R . .
C27 C 0.06450(8) 0.11152(7) 0.48419(7) 0.0357(10) Uani 1 1 d . . .
H27 H 0.1074 0.1863 0.4733 0.043 Uiso 1 1 calc R . .
N1 N -0.12557(8) 0.38720(7) 0.32318(7) 0.0344(8) Uani 1 1 d R . .
N2 N -0.08601(8) 0.19707(7) 0.38036(7) 0.0338(8) Uani 1 1 d R . .
N3 N -0.20048(8) 1.11385(7) 0.01711(7) 0.0373(8) Uani 1 1 d R . .
N4 N -0.36070(8) 1.26439(7) 0.01111(7) 0.0314(8) Uani 1 1 d R . .
O1 O 0.09533(8) 1.36148(7) 0.04575(7) 0.0453(8) Uani 1 1 d R . .
O2 O 0.08750(8) 1.15768(7) 0.03482(7) 0.0442(8) Uani 1 1 d R . .
O3 O 0.72158(8) 0.76600(7) 0.28249(7) 0.0500(9) Uani 1 1 d R . .
O4 O 0.63660(8) 0.58449(7) 0.31350(7) 0.0475(8) Uani 1 1 d R . .
O5 O 0.11590(8) 0.55269(7) 0.37449(7) 0.0413(7) Uani 1 1 d R . .
O6 O 0.02340(8) 0.70710(7) 0.29301(7) 0.0419(8) Uani 1 1 d R . .
O7 O -0.21517(8) 0.60355(7) 0.48418(7) 0.0451(8) Uani 1 1 d R . .
O8 O -0.05873(8) 0.56274(7) 0.13873(7) 0.0603(10) Uani 1 1 d R . .
O9 O -0.06918(8) 0.91766(7) 0.17134(7) 0.0401(7) Uani 1 1 d R . .
O10 O 0.50215(8) 0.37797(7) 0.43053(7) 0.0706(11) Uani 1 1 d R . .
H10A H 0.5490 0.4414 0.4201 0.106 Uiso 1 1 d R . .
H10B H 0.5315 0.3354 0.4775 0.106 Uiso 1 1 d R . .
H9B H -0.1459 0.8797 0.1895 0.106 Uiso 1 1 d R . .
H9A H -0.0170 0.8570 0.1902 0.106 Uiso 1 1 d R . .
H7A H -0.3011 0.6082 0.5125 0.106 Uiso 1 1 d R . .
H7B H -0.1804 0.5721 0.5311 0.106 Uiso 1 1 d R . .
H8A H -0.0189 0.4914 0.1233 0.106 Uiso 1 1 d R . .
H8B H -0.0774 0.5896 0.0831 0.106 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O6 2.0967 . ?
Mn1 O8 2.1888(11) . ?
Mn1 N1 2.1902 . ?
Mn1 O7 2.2539(11) . ?
Mn1 O4 2.2643 1_455 ?
Mn1 O3 2.3301 1_455 ?
Mn2 O2 2.1118 2_575 ?
Mn2 O2 2.1118 . ?
Mn2 N3 2.2438 . ?
Mn2 N3 2.2438 2_575 ?
Mn2 O9 2.3228 2_575 ?
Mn2 O9 2.3228 . ?
C1 O2 1.250(4) . ?
C1 O1 1.256(4) . ?
C1 C2 1.507(5) . ?
C2 C7 1.380(5) . ?
C2 C3 1.394(6) . ?
C3 C4 1.379(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.377(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.390(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.391(5) . ?
C6 C8 1.489(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.394(5) . ?
C8 C15 1.398(5) . ?
C9 C10 1.401(5) . ?
C9 H9 0.9300 . ?
C10 C12 1.389(5) . ?
C10 C11 1.499(5) . ?
C11 O4 1.249(4) . ?
C11 O3 1.253(4) . ?
C12 C13 1.391(5) . ?
C12 H12 0.9300 . ?
C13 C15 1.375(5) . ?
C13 C14 1.510(5) . ?
C14 O5 1.241(4) . ?
C14 O6 1.280(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.329(6) . ?
C16 N1 1.372(4) . ?
C16 H16 0.9300 . ?
C17 N2 1.376(4) . ?
C17 H17 0.9300 . ?
C18 N1 1.317(4) . ?
C18 N2 1.333(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.344(5) . ?
C19 N4 1.371(4) . ?
C19 H19 0.9300 . ?
C20 N3 1.378(4) . ?
C20 H20 0.9300 . ?
C21 N3 1.320(4) . ?
C21 N4 1.350(4) . ?
C21 H21 0.9300 . ?
C22 C24 1.378(6) . ?
C22 C23 1.383(5) . ?
C22 N4 1.439(4) . ?
C23 C24 1.402(5) 2_485 ?
C23 H23 0.9300 . ?
C24 C23 1.402(5) 2_485 ?
C24 H24 0.9300 . ?
C25 C27 1.378(4) . ?
C25 C26 1.388(5) . ?
C25 N2 1.437(4) . ?
C26 C27 1.379(4) 2_556 ?
C26 H26 0.9300 . ?
C27 C26 1.379(4) 2_556 ?
C27 H27 0.9300 . ?
O3 Mn1 2.3301 1_655 ?
O4 Mn1 2.2643 1_655 ?
O7 H7A 0.8407 . ?
O7 H7B 0.8429 . ?
O8 H8A 0.8459 . ?
O8 H8B 0.8446 . ?
O9 H9B 0.8718 . ?
O9 H9A 0.8770 . ?
O10 H10A 0.8453 . ?
O10 H10B 0.8596 . ?

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
O6 Mn1 O8 88.2 . . ?
O6 Mn1 N1 126.3 . . ?
O8 Mn1 N1 84.8 . . ?
O6 Mn1 O7 93.6 . . ?
O8 Mn1 O7 175.2 . . ?
N1 Mn1 O7 90.5 . . ?
O6 Mn1 O4 145.4 . 1_455 ?
O8 Mn1 O4 94.9 . 1_455 ?
N1 Mn1 O4 88.3 . 1_455 ?
O7 Mn1 O4 86.2 . 1_455 ?
O6 Mn1 O3 89.1 . 1_455 ?
O8 Mn1 O3 92.3 . 1_455 ?
N1 Mn1 O3 144.2 . 1_455 ?
O7 Mn1 O3 92.1 . 1_455 ?
O4 Mn1 O3 56.3 1_455 1_455 ?
O2 Mn2 O2 180.0 2_575 . ?
O2 Mn2 N3 90.5 2_575 . ?
O2 Mn2 N3 89.5 . . ?
O2 Mn2 N3 89.5 2_575 2_575 ?
O2 Mn2 N3 90.5 . 2_575 ?
N3 Mn2 N3 180.0 . 2_575 ?
O2 Mn2 O9 96.2 2_575 2_575 ?
O2 Mn2 O9 83.8 . 2_575 ?
N3 Mn2 O9 86.7 . 2_575 ?
N3 Mn2 O9 93.3 2_575 2_575 ?
O2 Mn2 O9 83.8 2_575 . ?
O2 Mn2 O9 96.2 . . ?
N3 Mn2 O9 93.3 . . ?
N3 Mn2 O9 86.7 2_575 . ?
O9 Mn2 O9 180.0 2_575 . ?
O2 C1 O1 124.4(3) . . ?
O2 C1 C2 117.6(3) . . ?
O1 C1 C2 117.9(3) . . ?
C7 C2 C3 119.2(3) . . ?
C7 C2 C1 118.6(3) . . ?
C3 C2 C1 122.1(3) . . ?
C4 C3 C2 119.0(4) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C5 C4 C3 121.8(4) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
C4 C5 C6 119.6(4) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C7 C6 C5 118.7(3) . . ?
C7 C6 C8 117.7(3) . . ?
C5 C6 C8 123.6(3) . . ?
C2 C7 C6 121.6(4) . . ?
C2 C7 H7 119.2 . . ?
C6 C7 H7 119.2 . . ?
C9 C8 C15 118.1(3) . . ?
C9 C8 C6 123.3(3) . . ?
C15 C8 C6 118.5(3) . . ?
C8 C9 C10 120.0(4) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C12 C10 C9 120.6(3) . . ?
C12 C10 C11 119.4(4) . . ?
C9 C10 C11 120.0(4) . . ?
O4 C11 O3 120.1(3) . . ?
O4 C11 C10 119.6(3) . . ?
O3 C11 C10 120.3(3) . . ?
C10 C12 C13 119.5(4) . . ?
C10 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
C15 C13 C12 119.7(4) . . ?
C15 C13 C14 118.7(3) . . ?
C12 C13 C14 121.5(4) . . ?
O5 C14 O6 123.4(3) . . ?
O5 C14 C13 121.3(3) . . ?
O6 C14 C13 115.3(3) . . ?
C13 C15 C8 122.1(3) . . ?
C13 C15 H15 118.9 . . ?
C8 C15 H15 118.9 . . ?
C17 C16 N1 110.0(4) . . ?
C17 C16 H16 125.0 . . ?
N1 C16 H16 125.0 . . ?
C16 C17 N2 106.4(3) . . ?
C16 C17 H17 126.8 . . ?
N2 C17 H17 126.8 . . ?
N1 C18 N2 111.2(3) . . ?
N1 C18 H18 124.4 . . ?
N2 C18 H18 124.4 . . ?
C20 C19 N4 106.5(3) . . ?
C20 C19 H19 126.8 . . ?
N4 C19 H19 126.8 . . ?
C19 C20 N3 110.3(3) . . ?
C19 C20 H20 124.8 . . ?
N3 C20 H20 124.8 . . ?
N3 C21 N4 111.9(3) . . ?
N3 C21 H21 124.0 . . ?
N4 C21 H21 124.0 . . ?
C24 C22 C23 121.2(4) . . ?
C24 C22 N4 120.5(3) . . ?
C23 C22 N4 118.2(3) . . ?
C22 C23 C24 119.2(4) . 2_485 ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 2_485 . ?
C22 C24 C23 119.6(4) . 2_485 ?
C22 C24 H24 120.2 . . ?
C23 C24 H24 120.2 2_485 . ?
C27 C25 C26 121.0(3) . . ?
C27 C25 N2 119.4(3) . . ?
C26 C25 N2 119.5(3) . . ?
C27 C26 C25 119.6(4) 2_556 . ?
C27 C26 H26 120.2 2_556 . ?
C25 C26 H26 120.2 . . ?
C25 C27 C26 119.4(2) . 2_556 ?
C25 C27 H27 120.3 . . ?
C26 C27 H27 120.3 2_556 . ?
C18 N1 C16 105.4(3) . . ?
C18 N1 Mn1 126.67(19) . . ?
C16 N1 Mn1 127.93(18) . . ?
C18 N2 C17 107.0(3) . . ?
C18 N2 C25 125.9(2) . . ?
C17 N2 C25 127.1(2) . . ?
C21 N3 C20 104.7(2) . . ?
C21 N3 Mn2 130.66(18) . . ?
C20 N3 Mn2 124.35(17) . . ?
C21 N4 C19 106.5(2) . . ?
C21 N4 C22 128.3(2) . . ?
C19 N4 C22 125.2(2) . . ?
C1 O2 Mn2 168.56(18) . . ?
C11 O3 Mn1 90.09(19) . 1_655 ?
C11 O4 Mn1 93.28(19) . 1_655 ?
C14 O6 Mn1 113.88(18) . . ?
Mn1 O7 H7A 117.9 . . ?
Mn1 O7 H7B 130.1 . . ?
H7A O7 H7B 105.4 . . ?
Mn1 O8 H8A 114.2 . . ?
Mn1 O8 H8B 137.9 . . ?
H8A O8 H8B 103.7 . . ?
Mn2 O9 H9B 116.5 . . ?
Mn2 O9 H9A 118.5 . . ?
H9B O9 H9A 97.1 . . ?
H10A O10 H10B 102.4 . . ?

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
O2 C1 C2 C7 -3.6(5) . . . . ?
O1 C1 C2 C7 178.4(3) . . . . ?
O2 C1 C2 C3 173.3(3) . . . . ?
O1 C1 C2 C3 -4.7(6) . . . . ?
C7 C2 C3 C4 2.5(6) . . . . ?
C1 C2 C3 C4 -174.4(4) . . . . ?
C2 C3 C4 C5 -0.1(7) . . . . ?
C3 C4 C5 C6 -1.7(7) . . . . ?
C4 C5 C6 C7 1.1(6) . . . . ?
C4 C5 C6 C8 -179.5(4) . . . . ?
C3 C2 C7 C6 -3.1(6) . . . . ?
C1 C2 C7 C6 173.9(4) . . . . ?
C5 C6 C7 C2 1.2(6) . . . . ?
C8 C6 C7 C2 -178.1(3) . . . . ?
C7 C6 C8 C9 139.0(4) . . . . ?
C5 C6 C8 C9 -40.3(6) . . . . ?
C7 C6 C8 C15 -37.4(5) . . . . ?
C5 C6 C8 C15 143.3(4) . . . . ?
C15 C8 C9 C10 0.6(6) . . . . ?
C6 C8 C9 C10 -175.8(4) . . . . ?
C8 C9 C10 C12 -1.3(6) . . . . ?
C8 C9 C10 C11 175.7(4) . . . . ?
C12 C10 C11 O4 -0.3(6) . . . . ?
C9 C10 C11 O4 -177.4(4) . . . . ?
C12 C10 C11 O3 178.6(4) . . . . ?
C9 C10 C11 O3 1.6(6) . . . . ?
C9 C10 C12 C13 0.4(6) . . . . ?
C11 C10 C12 C13 -176.6(4) . . . . ?
C10 C12 C13 C15 1.1(6) . . . . ?
C10 C12 C13 C14 177.8(4) . . . . ?
C15 C13 C14 O5 -161.7(3) . . . . ?
C12 C13 C14 O5 21.5(6) . . . . ?
C15 C13 C14 O6 18.2(5) . . . . ?
C12 C13 C14 O6 -158.6(3) . . . . ?
C12 C13 C15 C8 -1.8(6) . . . . ?
C14 C13 C15 C8 -178.6(4) . . . . ?
C9 C8 C15 C13 0.9(6) . . . . ?
C6 C8 C15 C13 177.5(4) . . . . ?
N1 C16 C17 N2 0.6(5) . . . . ?
N4 C19 C20 N3 -0.7(4) . . . . ?
C24 C22 C23 C24 0.5(7) . . . 2_485 ?
N4 C22 C23 C24 176.9(3) . . . 2_485 ?
C23 C22 C24 C23 -0.5(7) . . . 2_485 ?
N4 C22 C24 C23 -176.9(3) . . . 2_485 ?
C27 C25 C26 C27 0.1(6) . . . 2_556 ?
N2 C25 C26 C27 -179.2(3) . . . 2_556 ?
C26 C25 C27 C26 -0.1(6) . . . 2_556 ?
N2 C25 C27 C26 179.2(3) . . . 2_556 ?
N2 C18 N1 C16 -0.9(4) . . . . ?
N2 C18 N1 Mn1 177.86(13) . . . . ?
C17 C16 N1 C18 0.2(4) . . . . ?
C17 C16 N1 Mn1 -178.6(3) . . . . ?
O6 Mn1 N1 C18 49.7(3) . . . . ?
O8 Mn1 N1 C18 133.6(2) . . . . ?
O7 Mn1 N1 C18 -45.2(2) . . . . ?
O4 Mn1 N1 C18 -131.3(2) 1_455 . . . ?
O3 Mn1 N1 C18 -139.5(2) 1_455 . . . ?
O6 Mn1 N1 C16 -131.8(3) . . . . ?
O8 Mn1 N1 C16 -47.9(3) . . . . ?
O7 Mn1 N1 C16 133.3(3) . . . . ?
O4 Mn1 N1 C16 47.2(3) 1_455 . . . ?
O3 Mn1 N1 C16 39.0(3) 1_455 . . . ?
N1 C18 N2 C17 1.3(4) . . . . ?
N1 C18 N2 C25 -179.4(2) . . . . ?
C16 C17 N2 C18 -1.1(5) . . . . ?
C16 C17 N2 C25 179.6(3) . . . . ?
C27 C25 N2 C18 -25.3(5) . . . . ?
C26 C25 N2 C18 154.0(4) . . . . ?
C27 C25 N2 C17 153.9(3) . . . . ?
C26 C25 N2 C17 -26.8(5) . . . . ?
N4 C21 N3 C20 0.2(4) . . . . ?
N4 C21 N3 Mn2 174.23(12) . . . . ?
C19 C20 N3 C21 0.3(4) . . . . ?
C19 C20 N3 Mn2 -174.2(3) . . . . ?
O2 Mn2 N3 C21 -151.3(3) 2_575 . . . ?
O2 Mn2 N3 C21 28.7(3) . . . . ?
N3 Mn2 N3 C21 0(100) 2_575 . . . ?
O9 Mn2 N3 C21 -55.1(3) 2_575 . . . ?
O9 Mn2 N3 C21 124.9(3) . . . . ?
O2 Mn2 N3 C20 21.8(2) 2_575 . . . ?
O2 Mn2 N3 C20 -158.2(2) . . . . ?
N3 Mn2 N3 C20 0(100) 2_575 . . . ?
O9 Mn2 N3 C20 118.0(2) 2_575 . . . ?
O9 Mn2 N3 C20 -62.0(2) . . . . ?
N3 C21 N4 C19 -0.6(4) . . . . ?
N3 C21 N4 C22 177.4(3) . . . . ?
C20 C19 N4 C21 0.8(4) . . . . ?
C20 C19 N4 C22 -177.3(3) . . . . ?
C24 C22 N4 C21 -44.3(5) . . . . ?
C23 C22 N4 C21 139.3(4) . . . . ?
C24 C22 N4 C19 133.4(4) . . . . ?
C23 C22 N4 C19 -43.1(5) . . . . ?
O1 C1 O2 Mn2 -103.3(9) . . . . ?
C2 C1 O2 Mn2 78.8(10) . . . . ?
O2 Mn2 O2 C1 0.0(3) 2_575 . . . ?
N3 Mn2 O2 C1 59.8(9) . . . . ?
N3 Mn2 O2 C1 -120.2(9) 2_575 . . . ?
O9 Mn2 O2 C1 146.5(9) 2_575 . . . ?
O9 Mn2 O2 C1 -33.5(9) . . . . ?
O4 C11 O3 Mn1 -4.6(4) . . . 1_655 ?
C10 C11 O3 Mn1 176.5(3) . . . 1_655 ?
O3 C11 O4 Mn1 4.7(4) . . . 1_655 ?
C10 C11 O4 Mn1 -176.4(3) . . . 1_655 ?
O5 C14 O6 Mn1 -3.0(4) . . . . ?
C13 C14 O6 Mn1 177.1(2) . . . . ?
O8 Mn1 O6 C14 -105.9(2) . . . . ?
N1 Mn1 O6 C14 -23.7(2) . . . . ?
O7 Mn1 O6 C14 69.6(2) . . . . ?
O4 Mn1 O6 C14 158.1(2) 1_455 . . . ?
O3 Mn1 O6 C14 161.7(2) 1_455 . . . ?

_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_theta_full        26.24
_diffrn_measured_fraction_theta_full 0.967
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.093
_database_code_depnum_ccdc_archive 'CCDC 991513'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_added_by_encifer


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H24 N4 Ni O9'
_chemical_formula_weight         607.21

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   11.6286(16)
_cell_length_b                   13.6585(18)
_cell_length_c                   15.944(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2532.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1256
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7884
_exptl_absorpt_correction_T_max  0.8253
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13850
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_sigmaI/netI    0.1045
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         26.27
_reflns_number_total             5094
_reflns_number_gt                3546
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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 > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0520P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_number_reflns         5094
_refine_ls_number_parameters     374
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0533
_refine_ls_wR_factor_ref         0.1340
_refine_ls_wR_factor_gt          0.1086
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_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 0.80588(6) 0.65022(5) 1.04409(4) 0.03382(19) Uani 1 1 d . . .
C1 C 0.5945(4) 0.5212(4) 1.0480(4) 0.0333(12) Uani 1 1 d . . .
C2 C 0.5295(4) 0.4446(4) 1.0979(3) 0.0302(12) Uani 1 1 d . . .
C3 C 0.5791(4) 0.4025(4) 1.1686(3) 0.0310(12) Uani 1 1 d . . .
H3 H 0.6533 0.4199 1.1845 0.037 Uiso 1 1 calc R . .
C4 C 0.5175(4) 0.3343(4) 1.2156(3) 0.0308(12) Uani 1 1 d . . .
C5 C 0.4045(4) 0.3125(4) 1.1932(3) 0.0301(12) Uani 1 1 d . . .
H5 H 0.3622 0.2697 1.2265 0.036 Uiso 1 1 calc R . .
C6 C 0.3536(4) 0.3527(4) 1.1225(3) 0.0316(12) Uani 1 1 d . . .
C7 C 0.4176(5) 0.4187(4) 1.0756(3) 0.0347(13) Uani 1 1 d . . .
H7 H 0.3850 0.4465 1.0279 0.042 Uiso 1 1 calc R . .
C8 C 0.5715(5) 0.2884(4) 1.2922(3) 0.0350(13) Uani 1 1 d . . .
C9 C 0.2332(4) 0.3305(4) 1.1010(3) 0.0331(13) Uani 1 1 d . . .
C10 C 0.1479(4) 0.3278(4) 1.1633(3) 0.0346(13) Uani 1 1 d . . .
H10 H 0.1685 0.3376 1.2190 0.042 Uiso 1 1 calc R . .
C11 C 0.0328(4) 0.3109(4) 1.1430(3) 0.0341(13) Uani 1 1 d . . .
C12 C 0.0024(5) 0.2952(4) 1.0606(4) 0.0424(15) Uani 1 1 d . . .
H12 H -0.0744 0.2855 1.0467 0.051 Uiso 1 1 calc R . .
C13 C 0.0853(5) 0.2939(4) 0.9981(4) 0.0446(15) Uani 1 1 d . . .
H13 H 0.0647 0.2808 0.9429 0.054 Uiso 1 1 calc R . .
C14 C 0.1998(5) 0.3124(4) 1.0187(3) 0.0378(13) Uani 1 1 d . . .
H14 H 0.2550 0.3127 0.9765 0.045 Uiso 1 1 calc R . .
C15 C -0.0528(5) 0.3105(4) 1.2132(4) 0.0391(14) Uani 1 1 d . . .
C16 C 0.8439(5) 0.4823(4) 0.9161(4) 0.0481(16) Uani 1 1 d . . .
H16 H 0.7678 0.4616 0.9190 0.058 Uiso 1 1 calc R . .
C17 C 0.9252(5) 0.4441(5) 0.8639(4) 0.0484(16) Uani 1 1 d . . .
H17 H 0.9152 0.3942 0.8249 0.058 Uiso 1 1 calc R . .
C18 C 0.9985(4) 0.5606(4) 0.9409(3) 0.0358(13) Uani 1 1 d . . .
H18 H 1.0509 0.6047 0.9635 0.043 Uiso 1 1 calc R . .
C19 C 1.1359(5) 0.4812(4) 0.8430(4) 0.0363(13) Uani 1 1 d . . .
C20 C 1.1452(5) 0.4415(4) 0.7630(4) 0.0386(14) Uani 1 1 d . . .
H20 H 1.0793 0.4267 0.7325 0.046 Uiso 1 1 calc R . .
C21 C 1.2523(5) 0.4239(4) 0.7289(4) 0.0427(15) Uani 1 1 d . . .
H21 H 1.2585 0.3948 0.6764 0.051 Uiso 1 1 calc R . .
C22 C 1.3505(4) 0.4496(4) 0.7727(3) 0.0343(13) Uani 1 1 d . . .
C23 C 1.3420(5) 0.4913(4) 0.8516(4) 0.0410(15) Uani 1 1 d . . .
H23 H 1.4078 0.5095 0.8810 0.049 Uiso 1 1 calc R . .
C24 C 1.2341(5) 0.5055(4) 0.8859(4) 0.0407(15) Uani 1 1 d . . .
H24 H 1.2280 0.5321 0.9394 0.049 Uiso 1 1 calc R . .
C25 C 1.4871(5) 0.3976(5) 0.6605(3) 0.0454(16) Uani 1 1 d . . .
H25 H 1.4319 0.3816 0.6206 0.054 Uiso 1 1 calc R . .
C26 C 1.6477(5) 0.4198(4) 0.7225(4) 0.0443(15) Uani 1 1 d . . .
H26 H 1.7263 0.4215 0.7332 0.053 Uiso 1 1 calc R . .
C27 C 1.5663(5) 0.4458(5) 0.7771(4) 0.0479(16) Uani 1 1 d . . .
H27 H 1.5776 0.4693 0.8312 0.057 Uiso 1 1 calc R . .
N1 N 0.8911(4) 0.5560(3) 0.9641(3) 0.0354(10) Uani 1 1 d . . .
N2 N 1.0261(4) 0.4950(3) 0.8808(3) 0.0353(11) Uani 1 1 d . . .
N3 N 1.4626(4) 0.4311(3) 0.7380(3) 0.0364(11) Uani 1 1 d . . .
N4 N 1.5993(4) 0.3901(3) 0.6481(3) 0.0395(12) Uani 1 1 d . . .
O1 O 0.6875(3) 0.5492(3) 1.0797(2) 0.0410(9) Uani 1 1 d . . .
O2 O 0.5543(3) 0.5498(3) 0.9787(2) 0.0492(11) Uani 1 1 d . . .
O3 O -0.1587(3) 0.2966(4) 1.1846(3) 0.0569(12) Uani 1 1 d . . .
H3A H -0.2052 0.3118 1.2210 0.085 Uiso 1 1 calc R . .
O4 O -0.0281(3) 0.3216(3) 1.2861(3) 0.0525(12) Uani 1 1 d . . .
O5 O 0.5086(3) 0.2424(3) 1.3430(2) 0.0415(10) Uani 1 1 d . . .
O6 O 0.6787(3) 0.2989(3) 1.3020(2) 0.0402(9) Uani 1 1 d . . .
O7 O 0.7197(3) 0.7533(3) 1.1194(2) 0.0494(11) Uani 1 1 d . . .
H7A H 0.7563 0.7624 1.1626 0.074 Uiso 1 1 calc R . .
H7B H 0.6501 0.7471 1.1348 0.074 Uiso 1 1 d R . .
O8 O 0.7015(3) 0.7001(3) 0.9477(2) 0.0448(9) Uani 1 1 d . . .
H8A H 0.6524 0.6587 0.9371 0.067 Uiso 1 1 calc R . .
H8B H 0.7388 0.6995 0.9018 0.067 Uiso 1 1 d R . .
O9 O 0.9205(4) 0.7629(3) 1.0103(3) 0.0572(13) Uani 1 1 d . . .
H9A H 0.9354 0.7588 0.9602 0.086 Uiso 1 1 calc R . .
H9B H 0.9622 0.8139 1.0152 0.086 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.030(4) . ?
Ni1 N4 2.066(5) 2_765 ?
Ni1 N1 2.065(4) . ?
Ni1 O8 2.074(4) . ?
Ni1 O7 2.104(4) . ?
Ni1 O9 2.106(4) . ?
C1 O1 1.253(6) . ?
C1 O2 1.262(6) . ?
C1 C2 1.516(7) . ?
C2 C3 1.390(7) . ?
C2 C7 1.394(7) . ?
C3 C4 1.394(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.394(7) . ?
C4 C8 1.510(7) . ?
C5 C6 1.386(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.388(7) . ?
C6 C9 1.473(6) . ?
C7 H7 0.9300 . ?
C8 O5 1.259(6) . ?
C8 O6 1.264(6) . ?
C9 C14 1.390(7) . ?
C9 C10 1.404(7) . ?
C10 C11 1.396(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.378(7) . ?
C11 C15 1.498(7) . ?
C12 C13 1.385(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.395(8) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 O4 1.207(6) . ?
C15 O3 1.326(7) . ?
C16 C17 1.364(8) . ?
C16 N1 1.379(7) . ?
C16 H16 0.9300 . ?
C17 N2 1.391(7) . ?
C17 H17 0.9300 . ?
C18 N1 1.304(6) . ?
C18 N2 1.351(6) . ?
C18 H18 0.9300 . ?
C19 C24 1.373(7) . ?
C19 C20 1.389(8) . ?
C19 N2 1.424(7) . ?
C20 C21 1.380(7) . ?
C20 H20 0.9300 . ?
C21 C22 1.384(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.385(8) . ?
C22 N3 1.439(7) . ?
C23 C24 1.382(8) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 N4 1.323(7) . ?
C25 N3 1.347(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.335(8) . ?
C26 N4 1.374(7) . ?
C26 H26 0.9300 . ?
C27 N3 1.372(7) . ?
C27 H27 0.9300 . ?
N4 Ni1 2.066(5) 2_764 ?
O3 H3A 0.8200 . ?
O7 H7A 0.8200 . ?
O7 H7B 0.8506 . ?
O8 H8A 0.8200 . ?
O8 H8B 0.8500 . ?
O9 H9A 0.8200 . ?
O9 H9B 0.8529 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 N4 87.49(16) . 2_765 ?
O1 Ni1 N1 94.28(17) . . ?
N4 Ni1 N1 94.20(18) 2_765 . ?
O1 Ni1 O8 91.94(15) . . ?
N4 Ni1 O8 174.21(17) 2_765 . ?
N1 Ni1 O8 91.59(16) . . ?
O1 Ni1 O7 88.42(15) . . ?
N4 Ni1 O7 88.58(17) 2_765 . ?
N1 Ni1 O7 176.20(17) . . ?
O8 Ni1 O7 85.65(15) . . ?
O1 Ni1 O9 175.86(17) . . ?
N4 Ni1 O9 93.55(18) 2_765 . ?
N1 Ni1 O9 89.64(17) . . ?
O8 Ni1 O9 86.62(17) . . ?
O7 Ni1 O9 87.60(16) . . ?
O1 C1 O2 125.3(5) . . ?
O1 C1 C2 115.4(5) . . ?
O2 C1 C2 119.2(5) . . ?
C3 C2 C7 119.3(5) . . ?
C3 C2 C1 120.2(5) . . ?
C7 C2 C1 120.4(5) . . ?
C2 C3 C4 120.0(5) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 119.3(5) . . ?
C5 C4 C8 120.7(5) . . ?
C3 C4 C8 120.0(5) . . ?
C4 C5 C6 121.7(5) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C7 C6 C5 117.8(5) . . ?
C7 C6 C9 121.1(5) . . ?
C5 C6 C9 120.9(5) . . ?
C6 C7 C2 121.8(5) . . ?
C6 C7 H7 119.1 . . ?
C2 C7 H7 119.1 . . ?
O5 C8 O6 123.4(5) . . ?
O5 C8 C4 119.1(5) . . ?
O6 C8 C4 117.6(5) . . ?
C14 C9 C10 117.7(5) . . ?
C14 C9 C6 121.5(5) . . ?
C10 C9 C6 120.8(4) . . ?
C11 C10 C9 121.2(5) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C12 C11 C10 119.5(5) . . ?
C12 C11 C15 122.8(5) . . ?
C10 C11 C15 117.7(5) . . ?
C13 C12 C11 120.6(5) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C14 119.5(5) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
C9 C14 C13 121.4(5) . . ?
C9 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
O4 C15 O3 124.8(5) . . ?
O4 C15 C11 124.1(5) . . ?
O3 C15 C11 111.2(5) . . ?
C17 C16 N1 110.0(5) . . ?
C17 C16 H16 125.0 . . ?
N1 C16 H16 125.0 . . ?
C16 C17 N2 106.0(5) . . ?
C16 C17 H17 127.0 . . ?
N2 C17 H17 127.0 . . ?
N1 C18 N2 113.4(5) . . ?
N1 C18 H18 123.3 . . ?
N2 C18 H18 123.3 . . ?
C24 C19 C20 119.1(5) . . ?
C24 C19 N2 120.2(5) . . ?
C20 C19 N2 120.7(5) . . ?
C21 C20 C19 120.0(5) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C22 120.1(5) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C23 C22 C21 120.3(5) . . ?
C23 C22 N3 119.1(5) . . ?
C21 C22 N3 120.6(5) . . ?
C24 C23 C22 118.8(5) . . ?
C24 C23 H23 120.6 . . ?
C22 C23 H23 120.6 . . ?
C19 C24 C23 121.6(5) . . ?
C19 C24 H24 119.2 . . ?
C23 C24 H24 119.2 . . ?
N4 C25 N3 111.9(5) . . ?
N4 C25 H25 124.1 . . ?
N3 C25 H25 124.1 . . ?
C27 C26 N4 110.6(5) . . ?
C27 C26 H26 124.7 . . ?
N4 C26 H26 124.7 . . ?
C26 C27 N3 106.7(5) . . ?
C26 C27 H27 126.7 . . ?
N3 C27 H27 126.7 . . ?
C18 N1 C16 105.0(5) . . ?
C18 N1 Ni1 127.2(4) . . ?
C16 N1 Ni1 127.3(4) . . ?
C18 N2 C17 105.6(5) . . ?
C18 N2 C19 127.0(5) . . ?
C17 N2 C19 127.5(5) . . ?
C25 N3 C27 106.3(5) . . ?
C25 N3 C22 127.2(5) . . ?
C27 N3 C22 126.5(5) . . ?
C25 N4 C26 104.6(5) . . ?
C25 N4 Ni1 131.9(4) . 2_764 ?
C26 N4 Ni1 123.5(4) . 2_764 ?
C1 O1 Ni1 132.8(4) . . ?
C15 O3 H3A 109.5 . . ?
Ni1 O7 H7A 109.5 . . ?
Ni1 O7 H7B 123.5 . . ?
H7A O7 H7B 105.4 . . ?
Ni1 O8 H8A 109.5 . . ?
Ni1 O8 H8B 109.6 . . ?
H8A O8 H8B 99.9 . . ?
Ni1 O9 H9A 109.5 . . ?
Ni1 O9 H9B 159.1 . . ?
H9A O9 H9B 91.4 . . ?

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 -6.7(7) . . . . ?
O2 C1 C2 C3 171.5(5) . . . . ?
O1 C1 C2 C7 170.4(5) . . . . ?
O2 C1 C2 C7 -11.3(8) . . . . ?
C7 C2 C3 C4 0.8(8) . . . . ?
C1 C2 C3 C4 178.0(5) . . . . ?
C2 C3 C4 C5 -2.9(8) . . . . ?
C2 C3 C4 C8 179.8(5) . . . . ?
C3 C4 C5 C6 3.6(8) . . . . ?
C8 C4 C5 C6 -179.1(5) . . . . ?
C4 C5 C6 C7 -2.1(8) . . . . ?
C4 C5 C6 C9 -178.5(5) . . . . ?
C5 C6 C7 C2 -0.1(8) . . . . ?
C9 C6 C7 C2 176.3(5) . . . . ?
C3 C2 C7 C6 0.7(8) . . . . ?
C1 C2 C7 C6 -176.5(5) . . . . ?
C5 C4 C8 O5 -11.2(8) . . . . ?
C3 C4 C8 O5 166.1(5) . . . . ?
C5 C4 C8 O6 169.2(5) . . . . ?
C3 C4 C8 O6 -13.5(7) . . . . ?
C7 C6 C9 C14 45.3(8) . . . . ?
C5 C6 C9 C14 -138.4(5) . . . . ?
C7 C6 C9 C10 -134.2(6) . . . . ?
C5 C6 C9 C10 42.1(8) . . . . ?
C14 C9 C10 C11 -2.1(8) . . . . ?
C6 C9 C10 C11 177.4(5) . . . . ?
C9 C10 C11 C12 0.8(8) . . . . ?
C9 C10 C11 C15 -179.2(5) . . . . ?
C10 C11 C12 C13 1.5(9) . . . . ?
C15 C11 C12 C13 -178.5(5) . . . . ?
C11 C12 C13 C14 -2.5(9) . . . . ?
C10 C9 C14 C13 1.1(8) . . . . ?
C6 C9 C14 C13 -178.3(6) . . . . ?
C12 C13 C14 C9 1.1(9) . . . . ?
C12 C11 C15 O4 178.1(6) . . . . ?
C10 C11 C15 O4 -1.9(9) . . . . ?
C12 C11 C15 O3 -2.0(8) . . . . ?
C10 C11 C15 O3 178.0(5) . . . . ?
N1 C16 C17 N2 0.7(7) . . . . ?
C24 C19 C20 C21 2.1(9) . . . . ?
N2 C19 C20 C21 -176.7(5) . . . . ?
C19 C20 C21 C22 -2.7(10) . . . . ?
C20 C21 C22 C23 1.2(9) . . . . ?
C20 C21 C22 N3 179.7(5) . . . . ?
C21 C22 C23 C24 0.9(9) . . . . ?
N3 C22 C23 C24 -177.6(5) . . . . ?
C20 C19 C24 C23 0.0(10) . . . . ?
N2 C19 C24 C23 178.8(5) . . . . ?
C22 C23 C24 C19 -1.5(10) . . . . ?
N4 C26 C27 N3 1.1(7) . . . . ?
N2 C18 N1 C16 0.0(6) . . . . ?
N2 C18 N1 Ni1 -173.0(3) . . . . ?
C17 C16 N1 C18 -0.4(7) . . . . ?
C17 C16 N1 Ni1 172.6(4) . . . . ?
O1 Ni1 N1 C18 -154.4(5) . . . . ?
N4 Ni1 N1 C18 -66.6(5) 2_765 . . . ?
O8 Ni1 N1 C18 113.5(5) . . . . ?
O7 Ni1 N1 C18 70(3) . . . . ?
O9 Ni1 N1 C18 26.9(5) . . . . ?
O1 Ni1 N1 C16 34.1(5) . . . . ?
N4 Ni1 N1 C16 121.9(5) 2_765 . . . ?
O8 Ni1 N1 C16 -58.0(5) . . . . ?
O7 Ni1 N1 C16 -101(3) . . . . ?
O9 Ni1 N1 C16 -144.6(5) . . . . ?
N1 C18 N2 C17 0.5(6) . . . . ?
N1 C18 N2 C19 -179.5(5) . . . . ?
C16 C17 N2 C18 -0.7(7) . . . . ?
C16 C17 N2 C19 179.3(5) . . . . ?
C24 C19 N2 C18 26.5(9) . . . . ?
C20 C19 N2 C18 -154.8(5) . . . . ?
C24 C19 N2 C17 -153.5(6) . . . . ?
C20 C19 N2 C17 25.2(9) . . . . ?
N4 C25 N3 C27 0.0(7) . . . . ?
N4 C25 N3 C22 179.1(5) . . . . ?
C26 C27 N3 C25 -0.6(7) . . . . ?
C26 C27 N3 C22 -179.8(5) . . . . ?
C23 C22 N3 C25 -175.1(6) . . . . ?
C21 C22 N3 C25 6.4(9) . . . . ?
C23 C22 N3 C27 3.9(8) . . . . ?
C21 C22 N3 C27 -174.6(6) . . . . ?
N3 C25 N4 C26 0.6(7) . . . . ?
N3 C25 N4 Ni1 -177.2(4) . . . 2_764 ?
C27 C26 N4 C25 -1.1(7) . . . . ?
C27 C26 N4 Ni1 177.0(4) . . . 2_764 ?
O2 C1 O1 Ni1 3.9(9) . . . . ?
C2 C1 O1 Ni1 -178.0(3) . . . . ?
N4 Ni1 O1 C1 -178.1(5) 2_765 . . . ?
N1 Ni1 O1 C1 -84.1(5) . . . . ?
O8 Ni1 O1 C1 7.6(5) . . . . ?
O7 Ni1 O1 C1 93.2(5) . . . . ?
O9 Ni1 O1 C1 77(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.27
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.096
_database_code_depnum_ccdc_archive 'CCDC 991514'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_added_by_encifer

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C78 H74 N16 Ni3 O34'
_chemical_formula_weight         1955.66

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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                   13.683(2)
_cell_length_b                   23.839(4)
_cell_length_c                   14.576(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.745(4)
_cell_angle_gamma                90.00
_cell_volume                     4685.8(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2020
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8206
_exptl_absorpt_correction_T_max  0.8527
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23742
_diffrn_reflns_av_R_equivalents  0.1409
_diffrn_reflns_av_sigmaI/netI    0.1812
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.51
_diffrn_reflns_theta_max         25.10
_reflns_number_total             8350
_reflns_number_gt                3836
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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 > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0200P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8350
_refine_ls_number_parameters     597
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1828
_refine_ls_R_factor_gt           0.0890
_refine_ls_wR_factor_ref         0.2808
_refine_ls_wR_factor_gt          0.2193
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_restrained_S_all      1.153
_refine_ls_shift/su_max          0.002
_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 0.0000 0.5000 1.0000 0.0300(4) Uani 1 2 d S . .
Ni2 Ni -0.01770(7) 0.74490(5) 0.21803(8) 0.0292(3) Uani 1 1 d . . .
C1 C 0.0850(6) 0.6256(4) 0.2421(6) 0.041(2) Uani 1 1 d . . .
H1 H 0.1014 0.6247 0.1827 0.049 Uiso 1 1 calc R . .
C2 C 0.1092(7) 0.5856(4) 0.3071(7) 0.046(3) Uani 1 1 d . . .
H2 H 0.1452 0.5531 0.3016 0.055 Uiso 1 1 calc R . .
C3 C 0.0243(6) 0.6524(4) 0.3608(6) 0.035(2) Uani 1 1 d . . .
H3 H -0.0086 0.6729 0.4005 0.042 Uiso 1 1 calc R . .
C4 C 0.0766(7) 0.5762(4) 0.4731(6) 0.039(2) Uani 1 1 d . . .
C5 C 0.1661(7) 0.5547(4) 0.5160(7) 0.044(3) Uani 1 1 d . . .
H5 H 0.2206 0.5548 0.4857 0.053 Uiso 1 1 calc R . .
C6 C 0.1735(6) 0.5335(4) 0.6036(7) 0.044(3) Uani 1 1 d . . .
H6 H 0.2337 0.5186 0.6328 0.053 Uiso 1 1 calc R . .
C7 C 0.0929(7) 0.5335(4) 0.6501(7) 0.036(2) Uani 1 1 d . . .
C8 C 0.0033(7) 0.5531(4) 0.6060(6) 0.037(2) Uani 1 1 d . . .
H8 H -0.0515 0.5520 0.6359 0.045 Uiso 1 1 calc R . .
C9 C -0.0054(6) 0.5746(4) 0.5164(6) 0.036(2) Uani 1 1 d . . .
H9 H -0.0662 0.5879 0.4858 0.043 Uiso 1 1 calc R . .
C10 C 0.1805(8) 0.4851(5) 0.7927(8) 0.069(4) Uani 1 1 d . . .
H10 H 0.2355 0.4718 0.7696 0.082 Uiso 1 1 calc R . .
C11 C 0.1629(8) 0.4793(5) 0.8809(7) 0.059(3) Uani 1 1 d . . .
H11 H 0.2056 0.4623 0.9293 0.070 Uiso 1 1 calc R . .
C12 C 0.0401(7) 0.5231(4) 0.8046(7) 0.039(2) Uani 1 1 d . . .
H12 H -0.0198 0.5421 0.7891 0.047 Uiso 1 1 calc R . .
C13 C 0.1570(7) 0.8288(5) 0.2411(9) 0.064(3) Uani 1 1 d . . .
H13 H 0.1159 0.8585 0.2506 0.077 Uiso 1 1 calc R . .
C14 C 0.2536(7) 0.8335(4) 0.2402(9) 0.066(4) Uani 1 1 d . . .
H14 H 0.2915 0.8661 0.2492 0.079 Uiso 1 1 calc R . .
C15 C 0.2068(6) 0.7479(4) 0.2173(7) 0.038(2) Uani 1 1 d . . .
H15 H 0.2084 0.7094 0.2075 0.046 Uiso 1 1 calc R . .
C16 C 0.3830(6) 0.7650(4) 0.2159(7) 0.038(2) Uani 1 1 d . . .
C17 C 0.4115(6) 0.7096(4) 0.2286(7) 0.048(3) Uani 1 1 d . . .
H17 H 0.3658 0.6829 0.2408 0.057 Uiso 1 1 calc R . .
C18 C 0.5070(6) 0.6935(4) 0.2232(7) 0.044(3) Uani 1 1 d . . .
H18 H 0.5256 0.6560 0.2314 0.053 Uiso 1 1 calc R . .
C19 C 0.5749(6) 0.7330(4) 0.2056(6) 0.037(2) Uani 1 1 d . . .
C20 C 0.5468(6) 0.7878(4) 0.1935(7) 0.044(3) Uani 1 1 d . . .
H20 H 0.5932 0.8144 0.1823 0.052 Uiso 1 1 calc R . .
C21 C 0.4515(6) 0.8046(4) 0.1975(7) 0.042(2) Uani 1 1 d . . .
H21 H 0.4332 0.8420 0.1879 0.051 Uiso 1 1 calc R . .
C22 C 0.7048(6) 0.6627(4) 0.1793(7) 0.046(3) Uani 1 1 d . . .
H22 H 0.6650 0.6311 0.1657 0.056 Uiso 1 1 calc R . .
C23 C 0.8048(7) 0.6659(4) 0.1826(7) 0.050(3) Uani 1 1 d . . .
H23 H 0.8451 0.6364 0.1703 0.060 Uiso 1 1 calc R . .
C24 C 0.7573(6) 0.7488(4) 0.2161(6) 0.040(2) Uani 1 1 d . . .
H24 H 0.7571 0.7867 0.2312 0.048 Uiso 1 1 calc R . .
C25 C 0.2945(6) 0.7006(4) 0.4572(7) 0.046(3) Uani 1 1 d . . .
H25 H 0.2719 0.6638 0.4491 0.055 Uiso 1 1 calc R . .
C26 C 0.3926(6) 0.7124(4) 0.4527(7) 0.042(3) Uani 1 1 d . . .
H26 H 0.4353 0.6835 0.4426 0.050 Uiso 1 1 calc R . .
C27 C 0.4280(6) 0.7674(4) 0.4633(6) 0.032(2) Uani 1 1 d . . .
C28 C 0.3615(6) 0.8073(4) 0.4810(6) 0.038(2) Uani 1 1 d . . .
H28 H 0.3837 0.8441 0.4893 0.046 Uiso 1 1 calc R . .
C29 C 0.2656(6) 0.7966(3) 0.4873(6) 0.032(2) Uani 1 1 d . . .
C30 C 0.2301(6) 0.7418(4) 0.4734(7) 0.042(2) Uani 1 1 d . . .
H30 H 0.1640 0.7335 0.4752 0.050 Uiso 1 1 calc R . .
C31 C 0.1948(7) 0.8422(4) 0.5057(7) 0.039(2) Uani 1 1 d . . .
C32 C 0.6058(6) 0.7398(4) 0.4615(6) 0.037(2) Uani 1 1 d . . .
H32 H 0.5900 0.7030 0.4741 0.045 Uiso 1 1 calc R . .
C33 C 0.7018(6) 0.7526(4) 0.4505(6) 0.030(2) Uani 1 1 d . . .
C34 C 0.7257(6) 0.8077(4) 0.4318(6) 0.032(2) Uani 1 1 d . . .
H34 H 0.7901 0.8164 0.4241 0.038 Uiso 1 1 calc R . .
C35 C 0.6557(6) 0.8492(4) 0.4246(6) 0.035(2) Uani 1 1 d . . .
C36 C 0.5585(6) 0.8357(4) 0.4354(7) 0.039(2) Uani 1 1 d . . .
H36 H 0.5108 0.8639 0.4299 0.046 Uiso 1 1 calc R . .
C37 C 0.5317(6) 0.7812(4) 0.4540(6) 0.032(2) Uani 1 1 d . . .
C38 C 0.7799(7) 0.7070(4) 0.4627(7) 0.042(2) Uani 1 1 d . . .
C39 C 0.6826(7) 0.9099(4) 0.4063(7) 0.044(3) Uani 1 1 d . . .
N1 N 0.0694(5) 0.6027(3) 0.3838(5) 0.0367(19) Uani 1 1 d . . .
N2 N 0.0322(5) 0.6683(3) 0.2760(5) 0.0337(18) Uani 1 1 d . . .
N3 N 0.1035(5) 0.5139(3) 0.7445(5) 0.0382(19) Uani 1 1 d . . .
N4 N 0.0727(5) 0.5021(3) 0.8878(5) 0.0384(19) Uani 1 1 d . . .
N5 N 0.1264(5) 0.7753(3) 0.2263(5) 0.0365(19) Uani 1 1 d . . .
N6 N 0.2862(5) 0.7808(3) 0.2237(5) 0.0374(19) Uani 1 1 d . . .
N7 N 0.8374(5) 0.7194(3) 0.2070(5) 0.0346(18) Uani 1 1 d . . .
N8 N 0.6753(5) 0.7152(3) 0.1999(5) 0.0379(19) Uani 1 1 d . . .
O1 O -0.0221(4) 0.7117(3) 0.0855(4) 0.0446(17) Uani 1 1 d . . .
H1A H 0.0346 0.7072 0.0756 0.067 Uiso 1 1 calc R . .
O2 O -0.0671(5) 0.8218(2) 0.1553(4) 0.0416(16) Uani 1 1 d . . .
H2A H -0.0861 0.8422 0.1940 0.062 Uiso 1 1 calc R . .
O3 O -0.0315(4) 0.7828(3) 0.3452(4) 0.0374(15) Uani 1 1 d . . .
H3A H 0.0202 0.7991 0.3663 0.056 Uiso 1 1 calc R . .
O4 O 0.1309(4) 0.5204(2) 1.0887(4) 0.0366(15) Uani 1 1 d . . .
H4A H 0.1676 0.4930 1.0956 0.055 Uiso 1 1 calc R . .
H4B H 0.1408 0.5369 1.0381 0.055 Uiso 1 1 d R . .
O5 O 0.0348(4) 0.4158(2) 1.0185(5) 0.0479(18) Uani 1 1 d . . .
H5A H 0.0117 0.4037 1.0630 0.072 Uiso 1 1 calc R . .
H5B H 0.0954 0.4170 1.0441 0.072 Uiso 1 1 d R . .
O6 O 0.1033(4) 0.8342(2) 0.4827(4) 0.0411(17) Uani 1 1 d . . .
O7 O 0.2300(5) 0.8853(3) 0.5440(6) 0.067(2) Uani 1 1 d . . .
O8 O 0.7566(5) 0.6577(3) 0.4746(7) 0.095(3) Uani 1 1 d . . .
O9 O 0.8702(4) 0.7219(3) 0.4618(4) 0.0403(16) Uani 1 1 d . . .
O10 O 0.7704(4) 0.9196(3) 0.3967(5) 0.0495(19) Uani 1 1 d . . .
O11 O 0.6178(5) 0.9454(3) 0.4031(7) 0.088(3) Uani 1 1 d . . .
O1W O 0.6156(6) 0.0564(3) 0.3542(8) 0.112(4) Uani 1 1 d . . .
O2W O 0.3972(16) 0.5668(8) 0.3483(19) 0.340(13) Uani 1 1 d . . .
O3W O 0.6115(12) 0.5802(6) 0.4274(16) 0.288(11) Uani 1 1 d . . .
O4W O 0.8092(6) 0.8993(4) 0.2228(7) 0.103(3) Uani 1 1 d . . .
O5W O 0.4289(10) 0.9464(5) 0.2786(18) 0.324(14) Uani 1 1 d . . .
O6W O 0.5776(6) 0.9525(4) 0.6012(9) 0.133(4) Uani 1 1 d . . .
H1B H -0.0540 0.7249 0.0377 0.199 Uiso 1 1 d R . .
H2B H -0.0718 0.8437 0.1041 0.199 Uiso 1 1 d R . .
H3B H -0.0559 0.8205 0.3086 0.199 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N4 2.053(7) . ?
Ni1 N4 2.053(7) 3_567 ?
Ni1 O5 2.069(6) . ?
Ni1 O5 2.069(6) 3_567 ?
Ni1 O4 2.082(5) . ?
Ni1 O4 2.082(5) 3_567 ?
Ni2 N7 2.054(7) 1_455 ?
Ni2 O1 2.079(6) . ?
Ni2 N2 2.079(7) . ?
Ni2 N5 2.084(7) . ?
Ni2 O3 2.100(6) . ?
Ni2 O2 2.109(6) . ?
C1 C2 1.345(12) . ?
C1 N2 1.387(10) . ?
C1 H1 0.9300 . ?
C2 N1 1.385(11) . ?
C2 H2 0.9300 . ?
C3 N2 1.315(10) . ?
C3 N1 1.350(10) . ?
C3 H3 0.9300 . ?
C4 C9 1.377(11) . ?
C4 C5 1.376(12) . ?
C4 N1 1.436(11) . ?
C5 C6 1.360(12) . ?
C5 H5 0.9300 . ?
C6 C7 1.389(12) . ?
C6 H6 0.9300 . ?
C7 C8 1.366(12) . ?
C7 N3 1.437(11) . ?
C8 C9 1.390(12) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 N3 1.350(11) . ?
C10 C11 1.355(13) . ?
C10 H10 0.9300 . ?
C11 N4 1.368(11) . ?
C11 H11 0.9300 . ?
C12 N4 1.317(11) . ?
C12 N3 1.352(11) . ?
C12 H12 0.9300 . ?
C13 C14 1.329(12) . ?
C13 N5 1.348(12) . ?
C13 H13 0.9300 . ?
C14 N6 1.368(12) . ?
C14 H14 0.9300 . ?
C15 N5 1.304(10) . ?
C15 N6 1.331(10) . ?
C15 H15 0.9300 . ?
C16 C17 1.382(12) . ?
C16 C21 1.388(11) . ?
C16 N6 1.400(10) . ?
C17 C18 1.377(12) . ?
C17 H17 0.9300 . ?
C18 C19 1.378(12) . ?
C18 H18 0.9300 . ?
C19 C20 1.365(12) . ?
C19 N8 1.453(10) . ?
C20 C21 1.374(12) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.362(12) . ?
C22 N8 1.366(11) . ?
C22 H22 0.9300 . ?
C23 N7 1.376(11) . ?
C23 H23 0.9300 . ?
C24 N7 1.326(11) . ?
C24 N8 1.366(10) . ?
C24 H24 0.9300 . ?
C25 C30 1.366(12) . ?
C25 C26 1.384(12) . ?
C25 H25 0.9300 . ?
C26 C27 1.397(11) . ?
C26 H26 0.9300 . ?
C27 C28 1.371(11) . ?
C27 C37 1.485(11) . ?
C28 C29 1.355(11) . ?
C28 H28 0.9300 . ?
C29 C30 1.398(11) . ?
C29 C31 1.509(12) . ?
C30 H30 0.9300 . ?
C31 O7 1.228(10) . ?
C31 O6 1.255(9) . ?
C32 C33 1.383(11) . ?
C32 C37 1.405(11) . ?
C32 H32 0.9300 . ?
C33 C34 1.390(11) . ?
C33 C38 1.515(12) . ?
C34 C35 1.369(11) . ?
C34 H34 0.9300 . ?
C35 C36 1.403(11) . ?
C35 C39 1.528(12) . ?
C36 C37 1.391(11) . ?
C36 H36 0.9300 . ?
C38 O8 1.238(11) . ?
C38 O9 1.287(10) . ?
C39 O11 1.220(11) . ?
C39 O10 1.255(10) . ?
N7 Ni2 2.054(7) 1_655 ?
O1 H1A 0.8200 . ?
O1 H1B 0.8190 . ?
O2 H2A 0.8200 . ?
O2 H2B 0.9039 . ?
O3 H3A 0.8200 . ?
O3 H3B 1.0681 . ?
O4 H4A 0.8200 . ?
O4 H4B 0.8662 . ?
O5 H5A 0.8200 . ?
O5 H5B 0.8501 . ?

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
N4 Ni1 N4 179.997(2) . 3_567 ?
N4 Ni1 O5 89.8(3) . . ?
N4 Ni1 O5 90.2(3) 3_567 . ?
N4 Ni1 O5 90.2(3) . 3_567 ?
N4 Ni1 O5 89.8(3) 3_567 3_567 ?
O5 Ni1 O5 179.999(2) . 3_567 ?
N4 Ni1 O4 90.4(3) . . ?
N4 Ni1 O4 89.6(3) 3_567 . ?
O5 Ni1 O4 89.5(2) . . ?
O5 Ni1 O4 90.5(2) 3_567 . ?
N4 Ni1 O4 89.6(3) . 3_567 ?
N4 Ni1 O4 90.4(3) 3_567 3_567 ?
O5 Ni1 O4 90.5(2) . 3_567 ?
O5 Ni1 O4 89.5(2) 3_567 3_567 ?
O4 Ni1 O4 179.999(1) . 3_567 ?
N7 Ni2 O1 86.5(3) 1_455 . ?
N7 Ni2 N2 91.0(3) 1_455 . ?
O1 Ni2 N2 90.0(3) . . ?
N7 Ni2 N5 176.7(3) 1_455 . ?
O1 Ni2 N5 93.7(3) . . ?
N2 Ni2 N5 92.2(3) . . ?
N7 Ni2 O3 88.1(3) 1_455 . ?
O1 Ni2 O3 172.5(2) . . ?
N2 Ni2 O3 95.3(3) . . ?
N5 Ni2 O3 91.4(3) . . ?
N7 Ni2 O2 89.4(3) 1_455 . ?
O1 Ni2 O2 88.3(2) . . ?
N2 Ni2 O2 178.2(3) . . ?
N5 Ni2 O2 87.4(3) . . ?
O3 Ni2 O2 86.5(2) . . ?
C2 C1 N2 110.4(8) . . ?
C2 C1 H1 124.8 . . ?
N2 C1 H1 124.8 . . ?
C1 C2 N1 106.1(8) . . ?
C1 C2 H2 127.0 . . ?
N1 C2 H2 127.0 . . ?
N2 C3 N1 112.3(8) . . ?
N2 C3 H3 123.9 . . ?
N1 C3 H3 123.9 . . ?
C9 C4 C5 120.9(8) . . ?
C9 C4 N1 119.4(9) . . ?
C5 C4 N1 119.7(8) . . ?
C6 C5 C4 119.0(9) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C5 C6 C7 121.2(9) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C8 C7 C6 119.6(9) . . ?
C8 C7 N3 119.9(8) . . ?
C6 C7 N3 120.5(8) . . ?
C7 C8 C9 119.7(8) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C4 C9 C8 119.5(9) . . ?
C4 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
N3 C10 C11 107.3(9) . . ?
N3 C10 H10 126.4 . . ?
C11 C10 H10 126.4 . . ?
C10 C11 N4 109.7(9) . . ?
C10 C11 H11 125.2 . . ?
N4 C11 H11 125.2 . . ?
N4 C12 N3 112.4(8) . . ?
N4 C12 H12 123.8 . . ?
N3 C12 H12 123.8 . . ?
C14 C13 N5 111.2(9) . . ?
C14 C13 H13 124.4 . . ?
N5 C13 H13 124.4 . . ?
C13 C14 N6 106.1(9) . . ?
C13 C14 H14 126.9 . . ?
N6 C14 H14 126.9 . . ?
N5 C15 N6 113.0(8) . . ?
N5 C15 H15 123.5 . . ?
N6 C15 H15 123.5 . . ?
C17 C16 C21 119.4(8) . . ?
C17 C16 N6 119.7(8) . . ?
C21 C16 N6 120.9(9) . . ?
C18 C17 C16 120.5(8) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C19 119.8(9) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C20 C19 C18 119.7(8) . . ?
C20 C19 N8 121.3(8) . . ?
C18 C19 N8 119.0(9) . . ?
C19 C20 C21 121.4(8) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C20 C21 C16 119.2(9) . . ?
C20 C21 H21 120.4 . . ?
C16 C21 H21 120.4 . . ?
C23 C22 N8 105.8(8) . . ?
C23 C22 H22 127.1 . . ?
N8 C22 H22 127.1 . . ?
C22 C23 N7 110.0(8) . . ?
C22 C23 H23 125.0 . . ?
N7 C23 H23 125.0 . . ?
N7 C24 N8 110.0(8) . . ?
N7 C24 H24 125.0 . . ?
N8 C24 H24 125.0 . . ?
C30 C25 C26 121.4(9) . . ?
C30 C25 H25 119.3 . . ?
C26 C25 H25 119.3 . . ?
C25 C26 C27 120.4(8) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C28 C27 C26 116.3(8) . . ?
C28 C27 C37 122.6(8) . . ?
C26 C27 C37 121.1(8) . . ?
C29 C28 C27 124.3(8) . . ?
C29 C28 H28 117.8 . . ?
C27 C28 H28 117.8 . . ?
C28 C29 C30 118.9(8) . . ?
C28 C29 C31 122.3(8) . . ?
C30 C29 C31 118.7(7) . . ?
C25 C30 C29 118.6(8) . . ?
C25 C30 H30 120.7 . . ?
C29 C30 H30 120.7 . . ?
O7 C31 O6 123.0(9) . . ?
O7 C31 C29 118.0(8) . . ?
O6 C31 C29 119.0(8) . . ?
C33 C32 C37 121.6(8) . . ?
C33 C32 H32 119.2 . . ?
C37 C32 H32 119.2 . . ?
C32 C33 C34 119.3(8) . . ?
C32 C33 C38 119.5(8) . . ?
C34 C33 C38 121.1(8) . . ?
C35 C34 C33 120.9(8) . . ?
C35 C34 H34 119.6 . . ?
C33 C34 H34 119.6 . . ?
C34 C35 C36 119.3(8) . . ?
C34 C35 C39 120.9(8) . . ?
C36 C35 C39 119.8(8) . . ?
C37 C36 C35 121.5(8) . . ?
C37 C36 H36 119.3 . . ?
C35 C36 H36 119.3 . . ?
C36 C37 C32 117.4(8) . . ?
C36 C37 C27 120.8(8) . . ?
C32 C37 C27 121.8(8) . . ?
O8 C38 O9 122.3(8) . . ?
O8 C38 C33 120.3(8) . . ?
O9 C38 C33 117.4(9) . . ?
O11 C39 O10 124.9(9) . . ?
O11 C39 C35 117.9(8) . . ?
O10 C39 C35 117.2(8) . . ?
C3 N1 C2 106.4(8) . . ?
C3 N1 C4 124.7(8) . . ?
C2 N1 C4 128.8(8) . . ?
C3 N2 C1 104.8(7) . . ?
C3 N2 Ni2 124.2(6) . . ?
C1 N2 Ni2 130.9(6) . . ?
C10 N3 C12 106.0(8) . . ?
C10 N3 C7 127.4(8) . . ?
C12 N3 C7 126.6(8) . . ?
C12 N4 C11 104.6(8) . . ?
C12 N4 Ni1 127.4(6) . . ?
C11 N4 Ni1 127.8(6) . . ?
C15 N5 C13 104.2(8) . . ?
C15 N5 Ni2 128.7(6) . . ?
C13 N5 Ni2 127.1(6) . . ?
C15 N6 C14 105.5(7) . . ?
C15 N6 C16 127.5(8) . . ?
C14 N6 C16 127.0(8) . . ?
C24 N7 C23 106.1(7) . . ?
C24 N7 Ni2 129.7(6) . 1_655 ?
C23 N7 Ni2 124.1(6) . 1_655 ?
C22 N8 C24 108.1(7) . . ?
C22 N8 C19 126.8(7) . . ?
C24 N8 C19 125.2(8) . . ?
Ni2 O1 H1A 109.5 . . ?
Ni2 O1 H1B 124.9 . . ?
H1A O1 H1B 106.5 . . ?
Ni2 O2 H2A 109.5 . . ?
Ni2 O2 H2B 146.4 . . ?
H2A O2 H2B 103.8 . . ?
Ni2 O3 H3A 109.5 . . ?
Ni2 O3 H3B 89.3 . . ?
H3A O3 H3B 88.1 . . ?
Ni1 O4 H4A 109.5 . . ?
Ni1 O4 H4B 79.6 . . ?
H4A O4 H4B 106.6 . . ?
Ni1 O5 H5A 109.5 . . ?
Ni1 O5 H5B 102.2 . . ?
H5A O5 H5B 98.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C1 C2 N1 1.0(11) . . . . ?
C9 C4 C5 C6 -2.1(15) . . . . ?
N1 C4 C5 C6 175.2(8) . . . . ?
C4 C5 C6 C7 -0.5(15) . . . . ?
C5 C6 C7 C8 2.7(15) . . . . ?
C5 C6 C7 N3 -176.3(9) . . . . ?
C6 C7 C8 C9 -2.3(14) . . . . ?
N3 C7 C8 C9 176.7(8) . . . . ?
C5 C4 C9 C8 2.5(14) . . . . ?
N1 C4 C9 C8 -174.8(8) . . . . ?
C7 C8 C9 C4 -0.3(13) . . . . ?
N3 C10 C11 N4 2.6(14) . . . . ?
N5 C13 C14 N6 0.4(14) . . . . ?
C21 C16 C17 C18 0.1(15) . . . . ?
N6 C16 C17 C18 -178.6(9) . . . . ?
C16 C17 C18 C19 0.4(16) . . . . ?
C17 C18 C19 C20 -0.2(15) . . . . ?
C17 C18 C19 N8 -179.8(9) . . . . ?
C18 C19 C20 C21 -0.6(15) . . . . ?
N8 C19 C20 C21 179.0(9) . . . . ?
C19 C20 C21 C16 1.2(15) . . . . ?
C17 C16 C21 C20 -0.9(15) . . . . ?
N6 C16 C21 C20 177.8(9) . . . . ?
N8 C22 C23 N7 1.3(12) . . . . ?
C30 C25 C26 C27 -1.0(16) . . . . ?
C25 C26 C27 C28 2.1(14) . . . . ?
C25 C26 C27 C37 -176.9(9) . . . . ?
C26 C27 C28 C29 -1.0(15) . . . . ?
C37 C27 C28 C29 178.0(9) . . . . ?
C27 C28 C29 C30 -1.1(15) . . . . ?
C27 C28 C29 C31 -179.2(9) . . . . ?
C26 C25 C30 C29 -1.2(16) . . . . ?
C28 C29 C30 C25 2.2(15) . . . . ?
C31 C29 C30 C25 -179.6(9) . . . . ?
C28 C29 C31 O7 -22.9(14) . . . . ?
C30 C29 C31 O7 159.0(9) . . . . ?
C28 C29 C31 O6 158.0(9) . . . . ?
C30 C29 C31 O6 -20.0(13) . . . . ?
C37 C32 C33 C34 0.1(14) . . . . ?
C37 C32 C33 C38 177.9(8) . . . . ?
C32 C33 C34 C35 0.3(13) . . . . ?
C38 C33 C34 C35 -177.4(8) . . . . ?
C33 C34 C35 C36 -0.6(13) . . . . ?
C33 C34 C35 C39 178.5(8) . . . . ?
C34 C35 C36 C37 0.5(14) . . . . ?
C39 C35 C36 C37 -178.7(8) . . . . ?
C35 C36 C37 C32 -0.1(14) . . . . ?
C35 C36 C37 C27 -178.8(9) . . . . ?
C33 C32 C37 C36 -0.2(13) . . . . ?
C33 C32 C37 C27 178.4(8) . . . . ?
C28 C27 C37 C36 -19.3(14) . . . . ?
C26 C27 C37 C36 159.7(9) . . . . ?
C28 C27 C37 C32 162.1(9) . . . . ?
C26 C27 C37 C32 -18.9(14) . . . . ?
C32 C33 C38 O8 5.9(15) . . . . ?
C34 C33 C38 O8 -176.4(10) . . . . ?
C32 C33 C38 O9 -172.7(8) . . . . ?
C34 C33 C38 O9 5.1(13) . . . . ?
C34 C35 C39 O11 -178.0(10) . . . . ?
C36 C35 C39 O11 1.1(15) . . . . ?
C34 C35 C39 O10 1.2(14) . . . . ?
C36 C35 C39 O10 -179.6(9) . . . . ?
N2 C3 N1 C2 -0.1(10) . . . . ?
N2 C3 N1 C4 177.2(8) . . . . ?
C1 C2 N1 C3 -0.6(10) . . . . ?
C1 C2 N1 C4 -177.7(9) . . . . ?
C9 C4 N1 C3 43.9(13) . . . . ?
C5 C4 N1 C3 -133.4(9) . . . . ?
C9 C4 N1 C2 -139.4(9) . . . . ?
C5 C4 N1 C2 43.2(13) . . . . ?
N1 C3 N2 C1 0.7(10) . . . . ?
N1 C3 N2 Ni2 -175.2(5) . . . . ?
C2 C1 N2 C3 -1.1(10) . . . . ?
C2 C1 N2 Ni2 174.4(6) . . . . ?
N7 Ni2 N2 C3 -72.1(7) 1_455 . . . ?
O1 Ni2 N2 C3 -158.6(7) . . . . ?
N5 Ni2 N2 C3 107.7(7) . . . . ?
O3 Ni2 N2 C3 16.1(7) . . . . ?
O2 Ni2 N2 C3 -176(100) . . . . ?
N7 Ni2 N2 C1 113.1(8) 1_455 . . . ?
O1 Ni2 N2 C1 26.7(8) . . . . ?
N5 Ni2 N2 C1 -67.0(8) . . . . ?
O3 Ni2 N2 C1 -158.7(7) . . . . ?
O2 Ni2 N2 C1 9(9) . . . . ?
C11 C10 N3 C12 -1.8(13) . . . . ?
C11 C10 N3 C7 175.3(9) . . . . ?
N4 C12 N3 C10 0.4(11) . . . . ?
N4 C12 N3 C7 -176.7(8) . . . . ?
C8 C7 N3 C10 168.2(10) . . . . ?
C6 C7 N3 C10 -12.8(15) . . . . ?
C8 C7 N3 C12 -15.3(13) . . . . ?
C6 C7 N3 C12 163.7(9) . . . . ?
N3 C12 N4 C11 1.2(11) . . . . ?
N3 C12 N4 Ni1 -175.3(6) . . . . ?
C10 C11 N4 C12 -2.3(13) . . . . ?
C10 C11 N4 Ni1 174.1(8) . . . . ?
N4 Ni1 N4 C12 -36(5) 3_567 . . . ?
O5 Ni1 N4 C12 131.3(8) . . . . ?
O5 Ni1 N4 C12 -48.7(8) 3_567 . . . ?
O4 Ni1 N4 C12 -139.2(8) . . . . ?
O4 Ni1 N4 C12 40.8(8) 3_567 . . . ?
N4 Ni1 N4 C11 149(5) 3_567 . . . ?
O5 Ni1 N4 C11 -44.3(9) . . . . ?
O5 Ni1 N4 C11 135.7(9) 3_567 . . . ?
O4 Ni1 N4 C11 45.2(9) . . . . ?
O4 Ni1 N4 C11 -134.8(9) 3_567 . . . ?
N6 C15 N5 C13 -1.2(12) . . . . ?
N6 C15 N5 Ni2 177.9(6) . . . . ?
C14 C13 N5 C15 0.5(13) . . . . ?
C14 C13 N5 Ni2 -178.6(8) . . . . ?
N7 Ni2 N5 C15 -150(5) 1_455 . . . ?
O1 Ni2 N5 C15 -56.3(8) . . . . ?
N2 Ni2 N5 C15 33.8(9) . . . . ?
O3 Ni2 N5 C15 129.1(8) . . . . ?
O2 Ni2 N5 C15 -144.5(8) . . . . ?
N7 Ni2 N5 C13 29(6) 1_455 . . . ?
O1 Ni2 N5 C13 122.6(9) . . . . ?
N2 Ni2 N5 C13 -147.3(9) . . . . ?
O3 Ni2 N5 C13 -52.0(9) . . . . ?
O2 Ni2 N5 C13 34.4(9) . . . . ?
N5 C15 N6 C14 1.4(12) . . . . ?
N5 C15 N6 C16 -179.0(9) . . . . ?
C13 C14 N6 C15 -1.1(12) . . . . ?
C13 C14 N6 C16 179.4(10) . . . . ?
C17 C16 N6 C15 -19.9(15) . . . . ?
C21 C16 N6 C15 161.4(9) . . . . ?
C17 C16 N6 C14 159.5(10) . . . . ?
C21 C16 N6 C14 -19.2(16) . . . . ?
N8 C24 N7 C23 1.2(11) . . . . ?
N8 C24 N7 Ni2 178.0(6) . . . 1_655 ?
C22 C23 N7 C24 -1.6(11) . . . . ?
C22 C23 N7 Ni2 -178.6(7) . . . 1_655 ?
C23 C22 N8 C24 -0.5(11) . . . . ?
C23 C22 N8 C19 -179.6(9) . . . . ?
N7 C24 N8 C22 -0.4(11) . . . . ?
N7 C24 N8 C19 178.7(8) . . . . ?
C20 C19 N8 C22 -156.1(10) . . . . ?
C18 C19 N8 C22 23.5(14) . . . . ?
C20 C19 N8 C24 25.0(14) . . . . ?
C18 C19 N8 C24 -155.4(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.746
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.199
_database_code_depnum_ccdc_archive 'CCDC 991515'
