#######################################################################
#
#                 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_z

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C78 H58 N16 Ni3 O14, C12 H10 N4, 4(H2 O)'
_chemical_formula_sum            'C90 H76 N20 Ni3 O18'
_chemical_formula_weight         1901.84

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'
N N 0.0061 0.0033 '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'
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
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   13.4907(14)
_cell_length_b                   13.5050(14)
_cell_length_c                   13.7924(14)
_cell_angle_alpha                102.084(2)
_cell_angle_beta                 97.561(2)
_cell_angle_gamma                116.001(2)
_cell_volume                     2136.0(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4423
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      28.40

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             984
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8089
_exptl_absorpt_correction_T_max  0.8910
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11030
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7472
_reflns_number_gt                6106
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0800P)²+2.7102P] 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         7472
_refine_ls_number_parameters     646
_refine_ls_number_restraints     146
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1381
_refine_ls_wR_factor_gt          0.1283
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_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 0.28079(2) 0.02117(2) 0.07508(2) 0.02053(8) Uani 1 1 d . . .
Ni2 Ni 1.0000 0.5000 0.5000 0.02025(10) Uani 1 2 d S . .
O1 O 0.82867(14) 0.36418(15) 0.47858(14) 0.0311(5) Uani 1 1 d . . .
O2 O 0.82169(15) 0.27292(17) 0.59713(15) 0.0406(5) Uani 1 1 d . . .
O3 O 0.29755(14) 0.01616(14) 0.22720(13) 0.0271(4) Uani 1 1 d . . .
O4 O 0.44774(15) 0.13220(15) 0.18552(13) 0.0315(5) Uani 1 1 d . . .
O5 O 0.14215(16) -0.0038(2) 0.84549(16) 0.0544(6) Uani 1 1 d . . .
O6 O 0.31346(15) 0.05570(15) 0.94540(13) 0.0309(4) Uani 1 1 d . . .
O7 O 0.10918(14) -0.09686(15) 0.00396(14) 0.0317(5) Uani 1 1 d . . .
H7A H 0.0612(3) -0.1048(6) 0.0354(3) 0.080 Uiso 1 1 d D . .
H7B H 0.1057(12) -0.072(2) -0.0441(8) 0.080 Uiso 1 1 d D . .
N1 N 0.96384(18) 0.44145(17) 0.33786(15) 0.0276(5) Uani 1 1 d . . .
N2 N 0.95865(19) 0.42913(17) 0.17511(15) 0.0288(5) Uani 1 1 d . . .
N3 N 0.93056(18) 0.61148(18) 0.49898(17) 0.0297(5) Uani 1 1 d . . .
N4 N 0.92314(18) 0.77245(18) 0.50719(19) 0.0346(6) Uani 1 1 d . . .
N5 N 0.23829(19) 0.15004(18) 0.11479(17) 0.0325(5) Uani 1 1 d . . .
N6 N 0.2299(2) 0.3103(2) 0.1214(2) 0.0445(6) Uani 1 1 d . . .
N7 N 0.32009(17) -0.11123(17) 0.03874(16) 0.0267(5) Uani 1 1 d . . .
N8 N 0.31992(18) -0.27478(18) 0.03636(18) 0.0323(5) Uani 1 1 d . . .
C1 C 0.7773(2) 0.2927(2) 0.52347(19) 0.0260(6) Uani 1 1 d . . .
C2 C 0.6482(2) 0.2234(2) 0.48698(19) 0.0249(6) Uani 1 1 d . . .
C3 C 0.5878(2) 0.1951(2) 0.38674(19) 0.0255(6) Uani 1 1 d . . .
H3 H 0.6260 0.2211 0.3383 0.031 Uiso 1 1 calc R . .
C4 C 0.4703(2) 0.1279(2) 0.35966(18) 0.0245(6) Uani 1 1 d . . .
C5 C 0.4131(2) 0.0930(2) 0.43306(19) 0.0282(6) Uani 1 1 d . . .
H5 H 0.3340 0.0487 0.4138 0.034 Uiso 1 1 calc R . .
C6 C 0.4709(2) 0.1226(2) 0.53435(19) 0.0267(6) Uani 1 1 d . . .
C7 C 0.5886(2) 0.1855(2) 0.55822(19) 0.0275(6) Uani 1 1 d . . .
H7 H 0.6296 0.2032 0.6248 0.033 Uiso 1 1 calc R . .
C8 C 0.4025(2) 0.0907(2) 0.25118(19) 0.0247(6) Uani 1 1 d . . .
C9 C 0.4106(2) 0.0924(2) 0.61515(19) 0.0291(6) Uani 1 1 d . . .
C10 C 0.3011(4) 0.0787(5) 0.6061(4) 0.0390(11) Uani 0.60 1 d PU . .
H10A H 0.2620 0.0834 0.5452 0.047 Uiso 0.60 1 d PR . .
C10A C 0.2924(7) 0.0276(8) 0.5956(6) 0.0419(16) Uani 0.40 1 d PU . .
H10B H 0.2474 -0.0036 0.5260 0.050 Uiso 0.40 1 d PR . .
C11 C 0.2489(4) 0.0592(5) 0.6857(4) 0.0397(12) Uani 0.60 1 d PU . .
H11A H 0.1741 0.0518 0.6795 0.048 Uiso 0.60 1 d PR . .
C11A C 0.2374(7) 0.0074(8) 0.6733(6) 0.0431(16) Uani 0.40 1 d PU . .
H11B H 0.1558 -0.0354 0.6583 0.052 Uiso 0.40 1 d PR . .
C12 C 0.3021(2) 0.0507(2) 0.77380(19) 0.0302(6) Uani 1 1 d . . .
C13 C 0.4157(4) 0.0663(4) 0.7817(4) 0.0235(10) Uani 0.60 1 d PU . .
H13A H 0.4570 0.0677 0.8446 0.028 Uiso 0.60 1 d PR . .
C13A C 0.4132(7) 0.0963(7) 0.7945(7) 0.0327(16) Uani 0.40 1 d PU . .
H13B H 0.4545 0.1327 0.8653 0.039 Uiso 0.40 1 d PR . .
C14 C 0.4668(4) 0.0855(4) 0.7028(4) 0.0233(10) Uani 0.60 1 d PU . .
H14A H 0.5435 0.0979 0.7107 0.028 Uiso 0.60 1 d PR . .
C14A C 0.4690(7) 0.1171(7) 0.7178(6) 0.0326(16) Uani 0.40 1 d PU . .
H14B H 0.5508 0.1572 0.7367 0.039 Uiso 0.40 1 d PR . .
C15 C 0.2467(2) 0.0325(2) 0.8613(2) 0.0297(6) Uani 1 1 d . . .
C16 C 0.1690(3) 0.1598(3) 0.1750(3) 0.0500(8) Uani 1 1 d . . .
H16 H 0.1310 0.1062 0.2078 0.060 Uiso 1 1 calc R . .
C17 C 0.1628(3) 0.2583(3) 0.1809(3) 0.0518(8) Uani 1 1 d . . .
H17 H 0.1216 0.2848 0.2175 0.062 Uiso 1 1 calc R . .
C18 C 0.2720(3) 0.2408(2) 0.0825(2) 0.0422(7) Uani 1 1 d . . .
H18 H 0.3193 0.2559 0.0381 0.051 Uiso 1 1 calc R . .
C19 C 0.2515(3) 0.4161(2) 0.1009(2) 0.0457(8) Uani 1 1 d . . .
C20 C 0.2533(3) 0.5046(2) 0.1735(2) 0.0437(8) Uani 1 1 d . . .
H20 H 0.2398 0.4956 0.2364 0.052 Uiso 1 1 calc R . .
C21 C 0.2753(3) 0.6070(2) 0.1525(2) 0.0420(8) Uani 1 1 d . . .
H21 H 0.2755 0.6666 0.2007 0.050 Uiso 1 1 calc R . .
C22 C 0.2685(3) 0.4281(3) 0.0078(3) 0.0616(10) Uani 1 1 d . . .
H22 H 0.2641 0.3668 -0.0417 0.074 Uiso 1 1 calc R . .
C23 C 0.3770(2) -0.1338(2) -0.0317(2) 0.0307(6) Uani 1 1 d . . .
H23 H 0.4097 -0.0872 -0.0718 0.037 Uiso 1 1 calc R . .
C24 C 0.3779(2) -0.2333(2) -0.0337(2) 0.0344(7) Uani 1 1 d . . .
H24 H 0.4111 -0.2674 -0.0743 0.041 Uiso 1 1 calc R . .
C25 C 0.2874(2) -0.1976(2) 0.0782(2) 0.0289(6) Uani 1 1 d . . .
H25 H 0.2471 -0.2046 0.1284 0.035 Uiso 1 1 calc R . .
C26 C 0.2969(2) -0.3796(2) 0.0597(2) 0.0390(7) Uani 1 1 d . . .
C27 C 0.2921(3) -0.4701(3) -0.0134(3) 0.0581(9) Uani 1 1 d . . .
H27 H 0.3047 -0.4621 -0.0767 0.070 Uiso 1 1 calc R . .
C28 C 0.8367(3) 0.6046(3) 0.5317(3) 0.0550(9) Uani 1 1 d . . .
H28 H 0.7844 0.5413 0.5475 0.066 Uiso 1 1 calc R . .
C29 C 0.8312(3) 0.7029(3) 0.5377(3) 0.0612(10) Uani 1 1 d . . .
H29 H 0.7762 0.7201 0.5583 0.073 Uiso 1 1 calc R . .
C30 C 0.9807(2) 0.7137(2) 0.4867(2) 0.0325(6) Uani 1 1 d . . .
H30 H 1.0482 0.7426 0.4662 0.039 Uiso 1 1 calc R . .
C31 C 0.9601(2) 0.8878(2) 0.5026(2) 0.0326(7) Uani 1 1 d . . .
C32 C 0.9468(2) 0.9657(2) 0.5749(2) 0.0369(7) Uani 1 1 d . . .
H32 H 0.9110 0.9425 0.6255 0.044 Uiso 1 1 calc R . .
C33 C 1.0134(2) 0.9220(2) 0.4279(2) 0.0375(7) Uani 1 1 d . . .
H33 H 1.0226 0.8695 0.3795 0.045 Uiso 1 1 calc R . .
C34 C 0.9098(2) 0.3269(2) 0.2800(2) 0.0361(7) Uani 1 1 d . . .
H34 H 0.8799 0.2647 0.3062 0.043 Uiso 1 1 calc R . .
C35 C 0.9065(2) 0.3178(2) 0.1806(2) 0.0356(7) Uani 1 1 d . . .
H35 H 0.8753 0.2500 0.1264 0.043 Uiso 1 1 calc R . .
C36 C 0.9918(2) 0.4996(2) 0.27253(19) 0.0300(6) Uani 1 1 d . . .
H36 H 1.0299 0.5798 0.2905 0.036 Uiso 1 1 calc R . .
C37 C 0.9792(2) 0.4649(2) 0.08580(19) 0.0293(6) Uani 1 1 d . . .
C38 C 0.9915(2) 0.5710(2) 0.0823(2) 0.0334(7) Uani 1 1 d . . .
H38 H 0.9857 0.6189 0.1378 0.040 Uiso 1 1 calc R . .
C39 C 0.9875(2) 0.3937(2) 0.0034(2) 0.0318(7) Uani 1 1 d . . .
H39 H 0.9790 0.3221 0.0055 0.038 Uiso 1 1 calc R . .
N9 N 0.5313(5) 0.5130(4) 0.3129(7) 0.1806(8) Uani 1 1 d U . .
N10 N 0.5533(5) 0.5683(5) 0.1682(8) 0.1938(10) Uani 1 1 d U . .
C40 C 0.5172(6) 0.4217(6) 0.2207(9) 0.1857(10) Uani 1 1 d U . .
H40 H 0.5008 0.3475 0.2214 0.223 Uiso 1 1 calc R . .
C41 C 0.5297(6) 0.4550(6) 0.1424(9) 0.1894(11) Uani 1 1 d U . .
H41 H 0.5240 0.4107 0.0784 0.227 Uiso 1 1 calc R . .
C42 C 0.5529(6) 0.6066(6) 0.2713(9) 0.1874(10) Uani 1 1 d U . .
H42 H 0.5646 0.6794 0.3058 0.225 Uiso 1 1 calc R . .
C43 C 0.5158(2) 0.50883(17) 0.4032(4) 0.1748(9) Uani 1 1 d DU . .
C44 C 0.5284(3) 0.4260(2) 0.44056(17) 0.1752(10) Uani 1 1 d DU . .
H44 H 0.5519 0.3784 0.4030 0.210 Uiso 1 1 calc R . .
C45 C 0.5056(4) 0.4144(4) 0.5341(2) 0.1758(12) Uani 1 1 d DU . .
H45 H 0.5050 0.3527 0.5545 0.211 Uiso 1 1 calc R . .
O1W O 0.04034(10) 0.13964(13) 0.87503(11) 0.0694(8) Uani 1 1 d D . .
H1WA H 0.07634(11) 0.10478(15) 0.8634(3) 0.080 Uiso 1 1 d D . .
H1WB H 0.0157(3) 0.1543(3) 0.8254(2) 0.080 Uiso 1 1 d D . .
O2W O 0.13234(13) 0.82992(9) 0.26267(13) 0.0531(6) Uani 1 1 d D . .
H2WA H 0.1537(4) 0.80364(14) 0.3045(2) 0.080 Uiso 1 1 d D . .
H2WB H 0.1771(4) 0.89704(16) 0.2679(3) 0.080 Uiso 1 1 d D . .


_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 O6 1.9968(18) 1_554 ?
Ni1 N5 2.053(2) . ?
Ni1 N7 2.063(2) . ?
Ni1 O7 2.0917(16) . ?
Ni1 O3 2.0990(17) . ?
Ni1 O4 2.1957(17) . ?
Ni1 C8 2.474(2) . ?
Ni2 N3 2.094(2) 2_766 ?
Ni2 N3 2.094(2) . ?
Ni2 N1 2.121(2) . ?
Ni2 N1 2.121(2) 2_766 ?
Ni2 O1 2.1611(16) 2_766 ?
Ni2 O1 2.1611(16) . ?
O1 C1 1.254(3) . ?
O2 C1 1.248(3) . ?
O3 C8 1.271(3) . ?
O4 C8 1.251(3) . ?
O5 C15 1.243(3) . ?
O6 C15 1.257(3) . ?
O6 Ni1 1.9968(18) 1_556 ?
O7 H7A 0.807(5) . ?
O7 H7B 0.809(14) . ?
N1 C36 1.303(3) . ?
N1 C34 1.380(3) . ?
N2 C36 1.358(3) . ?
N2 C35 1.377(3) . ?
N2 C37 1.431(3) . ?
N3 C30 1.304(3) . ?
N3 C28 1.372(4) . ?
N4 C30 1.348(4) . ?
N4 C29 1.370(4) . ?
N4 C31 1.432(3) . ?
N5 C18 1.304(4) . ?
N5 C16 1.359(4) . ?
N6 C18 1.351(4) . ?
N6 C17 1.365(4) . ?
N6 C19 1.427(4) . ?
N7 C25 1.314(3) . ?
N7 C23 1.379(4) . ?
N8 C25 1.352(4) . ?
N8 C24 1.379(4) . ?
N8 C26 1.427(4) . ?
C1 C2 1.518(3) . ?
C2 C3 1.390(3) . ?
C2 C7 1.390(4) . ?
C3 C4 1.385(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.389(4) . ?
C4 C8 1.500(3) . ?
C5 C6 1.388(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.384(3) . ?
C6 C9 1.485(4) . ?
C7 H7 0.9300 . ?
C9 C14 1.383(6) . ?
C9 C10 1.392(6) . ?
C10 C11 1.390(8) . ?
C11 C12 1.380(6) . ?
C12 C13 1.438(6) . ?
C12 C15 1.509(4) . ?
C13 C14 1.373(7) . ?
C16 C17 1.356(5) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C22 1.364(5) . ?
C19 C20 1.378(4) . ?
C20 C21 1.383(4) . ?
C20 H20 0.9300 . ?
C21 C26 1.380(5) 1_565 ?
C21 H21 0.9300 . ?
C22 C27 1.374(5) 1_565 ?
C22 H22 0.9300 . ?
C23 C24 1.344(4) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C21 1.380(5) 1_545 ?
C26 C27 1.383(4) . ?
C27 C22 1.374(5) 1_545 ?
C27 H27 0.9300 . ?
C28 C29 1.349(5) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 C33 1.376(4) . ?
C31 C32 1.381(4) . ?
C32 C33 1.381(4) 2_776 ?
C32 H32 0.9300 . ?
C33 C32 1.381(4) 2_776 ?
C33 H33 0.9300 . ?
C34 C35 1.345(4) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 C39 1.378(4) . ?
C37 C38 1.381(4) . ?
C38 C39 1.383(4) 2_765 ?
C38 H38 0.9300 . ?
C39 C38 1.383(4) 2_765 ?
C39 H39 0.9300 . ?
N9 C43 1.298(10) . ?
N9 C42 1.427(11) . ?
N9 C40 1.499(11) . ?
N10 C41 1.372(9) . ?
N10 C42 1.410(13) . ?
C40 C41 1.257(14) . ?
C40 H40 0.9300 . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?
C43 C45 1.364(6) 2_666 ?
C43 C44 1.3897(10) . ?
C44 C45 1.3895(10) . ?
C44 H44 0.9300 . ?
C45 C43 1.364(6) 2_666 ?
C45 H45 0.9300 . ?
O1W H1WA 0.8201(10) . ?
O1W H1WB 0.8198(10) . ?
O2W H2WA 0.8200(10) . ?
O2W H2WB 0.8202(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
O6 Ni1 N5 92.91(9) 1_554 . ?
O6 Ni1 N7 89.07(9) 1_554 . ?
N5 Ni1 N7 177.87(9) . . ?
O6 Ni1 O7 92.98(7) 1_554 . ?
N5 Ni1 O7 89.80(8) . . ?
N7 Ni1 O7 89.32(8) . . ?
O6 Ni1 O3 163.39(7) 1_554 . ?
N5 Ni1 O3 88.70(8) . . ?
N7 Ni1 O3 89.61(8) . . ?
O7 Ni1 O3 103.56(7) . . ?
O6 Ni1 O4 102.22(7) 1_554 . ?
N5 Ni1 O4 89.53(8) . . ?
N7 Ni1 O4 90.80(8) . . ?
O7 Ni1 O4 164.80(7) . . ?
O3 Ni1 O4 61.24(6) . . ?
O6 Ni1 C8 132.53(8) 1_554 . ?
N5 Ni1 C8 89.13(9) . . ?
N7 Ni1 C8 90.10(8) . . ?
O7 Ni1 C8 134.48(8) . . ?
O3 Ni1 C8 30.91(7) . . ?
O4 Ni1 C8 30.32(7) . . ?
N3 Ni2 N3 180.000(1) 2_766 . ?
N3 Ni2 N1 86.40(9) 2_766 . ?
N3 Ni2 N1 93.60(9) . . ?
N3 Ni2 N1 93.60(9) 2_766 2_766 ?
N3 Ni2 N1 86.40(9) . 2_766 ?
N1 Ni2 N1 180.000(1) . 2_766 ?
N3 Ni2 O1 87.12(8) 2_766 2_766 ?
N3 Ni2 O1 92.88(8) . 2_766 ?
N1 Ni2 O1 95.49(7) . 2_766 ?
N1 Ni2 O1 84.51(7) 2_766 2_766 ?
N3 Ni2 O1 92.88(8) 2_766 . ?
N3 Ni2 O1 87.12(8) . . ?
N1 Ni2 O1 84.51(7) . . ?
N1 Ni2 O1 95.49(7) 2_766 . ?
O1 Ni2 O1 180.00(10) 2_766 . ?
C1 O1 Ni2 137.37(17) . . ?
C8 O3 Ni1 91.07(15) . . ?
C8 O4 Ni1 87.25(13) . . ?
C15 O6 Ni1 130.40(17) . 1_556 ?
Ni1 O7 H7A 120.4(3) . . ?
Ni1 O7 H7B 95.8(10) . . ?
H7A O7 H7B 117.3(15) . . ?
C36 N1 C34 105.2(2) . . ?
C36 N1 Ni2 130.11(16) . . ?
C34 N1 Ni2 124.49(18) . . ?
C36 N2 C35 106.4(2) . . ?
C36 N2 C37 126.2(2) . . ?
C35 N2 C37 127.3(2) . . ?
C30 N3 C28 105.2(2) . . ?
C30 N3 Ni2 126.00(19) . . ?
C28 N3 Ni2 127.5(2) . . ?
C30 N4 C29 106.5(2) . . ?
C30 N4 C31 124.1(2) . . ?
C29 N4 C31 129.3(3) . . ?
C18 N5 C16 105.1(3) . . ?
C18 N5 Ni1 125.3(2) . . ?
C16 N5 Ni1 129.6(2) . . ?
C18 N6 C17 106.9(3) . . ?
C18 N6 C19 125.3(3) . . ?
C17 N6 C19 127.8(3) . . ?
C25 N7 C23 105.7(2) . . ?
C25 N7 Ni1 124.04(19) . . ?
C23 N7 Ni1 130.13(19) . . ?
C25 N8 C24 106.8(2) . . ?
C25 N8 C26 126.3(3) . . ?
C24 N8 C26 126.9(2) . . ?
O2 C1 O1 126.4(2) . . ?
O2 C1 C2 115.6(2) . . ?
O1 C1 C2 118.0(2) . . ?
C3 C2 C7 119.0(2) . . ?
C3 C2 C1 123.5(2) . . ?
C7 C2 C1 117.5(2) . . ?
C4 C3 C2 119.4(2) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 120.2(2) . . ?
C3 C4 C8 121.0(2) . . ?
C5 C4 C8 118.8(2) . . ?
C4 C5 C6 121.6(2) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C7 C6 C5 116.9(2) . . ?
C7 C6 C9 120.8(2) . . ?
C5 C6 C9 122.3(2) . . ?
C6 C7 C2 122.8(2) . . ?
C6 C7 H7 118.6 . . ?
C2 C7 H7 118.6 . . ?
O4 C8 O3 120.4(2) . . ?
O4 C8 C4 121.0(2) . . ?
O3 C8 C4 118.5(2) . . ?
O4 C8 Ni1 62.43(12) . . ?
O3 C8 Ni1 58.02(12) . . ?
C4 C8 Ni1 176.56(18) . . ?
C14 C9 C10 120.0(4) . . ?
C14 C9 C6 119.6(3) . . ?
C10 C9 C6 120.3(3) . . ?
C11 C10 C9 119.8(4) . . ?
C12 C11 C10 121.7(5) . . ?
C11 C12 C15 121.7(3) . . ?
O5 C15 O6 125.9(3) . . ?
O5 C15 C12 119.1(2) . . ?
O6 C15 C12 115.0(2) . . ?
N5 C16 C17 110.9(3) . . ?
N5 C16 H16 124.6 . . ?
C17 C16 H16 124.6 . . ?
C16 C17 N6 105.2(3) . . ?
C16 C17 H17 127.4 . . ?
N6 C17 H17 127.4 . . ?
N5 C18 N6 111.8(3) . . ?
N5 C18 H18 124.1 . . ?
N6 C18 H18 124.1 . . ?
C22 C19 C20 120.3(3) . . ?
C22 C19 N6 119.1(3) . . ?
C20 C19 N6 120.5(3) . . ?
C19 C20 C21 119.6(3) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C26 C21 C20 119.9(3) 1_565 . ?
C26 C21 H21 120.1 1_565 . ?
C20 C21 H21 120.1 . . ?
C19 C22 C27 120.6(3) . 1_565 ?
C19 C22 H22 119.7 . . ?
C27 C22 H22 119.7 1_565 . ?
C24 C23 N7 109.9(3) . . ?
C24 C23 H23 125.1 . . ?
N7 C23 H23 125.1 . . ?
C23 C24 N8 106.3(3) . . ?
C23 C24 H24 126.8 . . ?
N8 C24 H24 126.8 . . ?
N7 C25 N8 111.3(2) . . ?
N7 C25 H25 124.4 . . ?
N8 C25 H25 124.4 . . ?
C21 C26 C27 119.8(3) 1_545 . ?
C21 C26 N8 120.9(3) 1_545 . ?
C27 C26 N8 119.3(3) . . ?
C22 C27 C26 119.7(3) 1_545 . ?
C22 C27 H27 120.1 1_545 . ?
C26 C27 H27 120.2 . . ?
C29 C28 N3 110.1(3) . . ?
C29 C28 H28 125.0 . . ?
N3 C28 H28 125.0 . . ?
C28 C29 N4 106.1(3) . . ?
C28 C29 H29 127.0 . . ?
N4 C29 H29 126.9 . . ?
N3 C30 N4 112.1(2) . . ?
N3 C30 H30 124.0 . . ?
N4 C30 H30 123.9 . . ?
C33 C31 C32 120.2(3) . . ?
C33 C31 N4 119.4(3) . . ?
C32 C31 N4 120.4(3) . . ?
C33 C32 C31 119.9(3) 2_776 . ?
C33 C32 H32 120.0 2_776 . ?
C31 C32 H32 120.0 . . ?
C31 C33 C32 119.9(3) . 2_776 ?
C31 C33 H33 120.1 . . ?
C32 C33 H33 120.1 2_776 . ?
C35 C34 N1 110.4(2) . . ?
C35 C34 H34 124.8 . . ?
N1 C34 H34 124.8 . . ?
C34 C35 N2 106.0(2) . . ?
C34 C35 H35 127.0 . . ?
N2 C35 H35 127.0 . . ?
N1 C36 N2 111.9(2) . . ?
N1 C36 H36 124.0 . . ?
N2 C36 H36 124.0 . . ?
C39 C37 C38 119.9(3) . . ?
C39 C37 N2 120.0(2) . . ?
C38 C37 N2 120.1(2) . . ?
C37 C38 C39 120.3(3) . 2_765 ?
C37 C38 H38 119.9 . . ?
C39 C38 H38 119.9 2_765 . ?
C37 C39 C38 119.8(3) . 2_765 ?
C37 C39 H39 120.1 . . ?
C38 C39 H39 120.1 2_765 . ?
C43 N9 C42 127.3(6) . . ?
C43 N9 C40 131.5(6) . . ?
C42 N9 C40 100.8(8) . . ?
C41 N10 C42 110.4(9) . . ?
C41 C40 N9 113.7(8) . . ?
C41 C40 H40 123.2 . . ?
N9 C40 H40 123.2 . . ?
C40 C41 N10 107.9(10) . . ?
C40 C41 H41 126.0 . . ?
N10 C41 H41 126.0 . . ?
N10 C42 N9 107.2(7) . . ?
N10 C42 H42 126.4 . . ?
N9 C42 H42 126.4 . . ?
N9 C43 C45 123.5(4) . 2_666 ?
N9 C43 C44 118.3(4) . . ?
C45 C43 C44 118.0(4) 2_666 . ?
C45 C44 C43 119.9(4) . . ?
C45 C44 H44 120.1 . . ?
C43 C44 H44 120.1 . . ?
C43 C45 C44 121.6(4) 2_666 . ?
C43 C45 H45 119.2 2_666 . ?
C44 C45 H45 119.2 . . ?
H1WA O1W H1WB 114.6(2) . . ?
H2WA O2W H2WB 114.6(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         0.847
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.076
_database_code_depnum_ccdc_archive 'CCDC 977304'
#######################################################################
#
#                 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_z

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H22 Co2 N4 O7, H2 O'
_chemical_formula_sum            'C29 H24 Co2 N4 O8'
_chemical_formula_weight         674.38

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   P2(1)/n
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   12.337(2)
_cell_length_b                   11.051(2)
_cell_length_c                   21.819(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.761(4)
_cell_angle_gamma                90.00
_cell_volume                     2922.3(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1666
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      22.16


_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1376
_exptl_absorpt_coefficient_mu    1.192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6736
_exptl_absorpt_correction_T_max  0.9212
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14729
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0788
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5133
_reflns_number_gt                3497
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0430P)²+1.8129P] 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         5133
_refine_ls_number_parameters     397
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1138
_refine_ls_wR_factor_gt          0.0971
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.011
_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
C1 C 0.9452(4) 0.6971(4) 0.44041(18) 0.0210(10) Uani 1 1 d . . .
C2 C 0.9699(3) 0.5827(4) 0.40903(18) 0.0197(9) Uani 1 1 d . . .
C3 C 1.0364(3) 0.5881(4) 0.36409(19) 0.0238(10) Uani 1 1 d . . .
H3 H 1.0618 0.6629 0.3533 0.029 Uiso 1 1 calc R . .
C4 C 1.0657(3) 0.4846(4) 0.33487(19) 0.0234(10) Uani 1 1 d . . .
C5 C 1.0340(3) 0.3734(4) 0.35520(18) 0.0227(10) Uani 1 1 d . . .
H5 H 1.0583 0.3028 0.3389 0.027 Uiso 1 1 calc R . .
C6 C 0.9666(3) 0.3655(3) 0.39938(17) 0.0174(9) Uani 1 1 d . . .
C7 C 0.9315(3) 0.4704(4) 0.42489(18) 0.0197(9) Uani 1 1 d . . .
H7 H 0.8825 0.4657 0.4524 0.024 Uiso 1 1 calc R . .
C8 C 0.9324(4) 0.2433(4) 0.41864(18) 0.0208(10) Uani 1 1 d . . .
C9 C 1.1294(4) 0.4959(4) 0.2839(2) 0.0248(10) Uani 1 1 d . . .
C10 C 1.1075(4) 0.5900(4) 0.2410(2) 0.0320(11) Uani 1 1 d . . .
H10 H 1.0532 0.6461 0.2452 0.038 Uiso 1 1 calc R . .
C11 C 1.1638(4) 0.6028(4) 0.1924(2) 0.0292(11) Uani 1 1 d . . .
H11 H 1.1465 0.6662 0.1643 0.035 Uiso 1 1 calc R . .
C12 C 1.2455(3) 0.5217(4) 0.18535(18) 0.0224(10) Uani 1 1 d . . .
C13 C 1.2685(4) 0.4265(4) 0.2278(2) 0.0335(12) Uani 1 1 d . . .
H13 H 1.3230 0.3706 0.2235 0.040 Uiso 1 1 calc R . .
C14 C 1.2115(4) 0.4145(4) 0.2761(2) 0.0316(11) Uani 1 1 d . . .
H14 H 1.2282 0.3506 0.3039 0.038 Uiso 1 1 calc R . .
C15 C 1.3051(3) 0.5344(4) 0.1318(2) 0.0243(10) Uani 1 1 d . . .
C16 C 0.6240(4) 0.7440(5) 0.4300(2) 0.0430(14) Uani 1 1 d . . .
H16 H 0.6608 0.6719 0.4257 0.052 Uiso 1 1 calc R . .
C17 C 0.4976(5) 0.8797(7) 0.4204(4) 0.086(2) Uani 1 1 d . . .
H17 H 0.4313 0.9211 0.4091 0.103 Uiso 1 1 calc R . .
C18 C 0.5897(5) 0.9213(6) 0.4569(3) 0.069(2) Uani 1 1 d . . .
H18 H 0.5978 0.9977 0.4750 0.083 Uiso 1 1 calc R . .
C19 C 0.4426(5) 0.6853(6) 0.3616(3) 0.078(2) Uani 1 1 d . . .
H19A H 0.4398 0.7089 0.3185 0.093 Uiso 1 1 calc R . .
H19B H 0.3691 0.6942 0.3709 0.093 Uiso 1 1 calc R . .
C20 C 0.4778(5) 0.5551(7) 0.3700(3) 0.0669(11) Uani 1 1 d U . .
C21 C 0.4393(6) 0.4811(7) 0.4118(3) 0.0737(11) Uani 1 1 d U . .
H21 H 0.3872 0.5099 0.4341 0.088 Uiso 1 1 calc R . .
C22 C 0.4776(5) 0.3649(7) 0.4207(3) 0.0759(12) Uani 1 1 d U . .
H22 H 0.4519 0.3162 0.4497 0.091 Uiso 1 1 calc R . .
C23 C 0.5534(5) 0.3178(7) 0.3877(3) 0.0717(11) Uani 1 1 d U . .
H23 H 0.5782 0.2386 0.3941 0.086 Uiso 1 1 calc R . .
C24 C 0.5916(5) 0.3917(7) 0.3447(3) 0.0652(11) Uani 1 1 d U . .
C25 C 0.5535(5) 0.5090(6) 0.3365(3) 0.0635(11) Uani 1 1 d U . .
H25 H 0.5792 0.5584 0.3077 0.076 Uiso 1 1 calc R . .
C26 C 0.6785(5) 0.3407(6) 0.3123(2) 0.0634(18) Uani 1 1 d . . .
H26A H 0.7500 0.3507 0.3391 0.076 Uiso 1 1 calc R . .
H26B H 0.6656 0.2546 0.3061 0.076 Uiso 1 1 calc R . .
C27 C 0.7293(5) 0.4899(6) 0.1737(3) 0.0648(19) Uani 1 1 d . . .
H27 H 0.7710 0.5319 0.1493 0.078 Uiso 1 1 calc R . .
C28 C 0.7654(5) 0.4555(6) 0.2334(3) 0.076(2) Uani 1 1 d . . .
H28 H 0.8350 0.4697 0.2572 0.091 Uiso 1 1 calc R . .
C29 C 0.5981(4) 0.3973(5) 0.2026(2) 0.0422(13) Uani 1 1 d . . .
H29 H 0.5300 0.3613 0.2027 0.051 Uiso 1 1 calc R . .
Co1 Co 0.99409(5) 0.97392(5) 0.42856(3) 0.01918(16) Uani 1 1 d . . .
Co2 Co 0.82556(5) 0.84153(5) 0.51605(3) 0.02218(17) Uani 1 1 d . . .
N1 N 0.6688(3) 0.8353(4) 0.46343(18) 0.0343(10) Uani 1 1 d . . .
N2 N 0.5195(3) 0.7654(5) 0.4028(2) 0.0515(13) Uani 1 1 d . . .
N3 N 0.6817(3) 0.3968(4) 0.25176(18) 0.0444(11) Uani 1 1 d . . .
N4 N 0.6235(3) 0.4543(3) 0.15456(17) 0.0309(9) Uani 1 1 d . . .
O1 O 1.0040(2) 0.7870(3) 0.43382(13) 0.0276(7) Uani 1 1 d . . .
O2 O 0.8684(2) 0.6955(2) 0.47174(13) 0.0262(7) Uani 1 1 d . . .
O3 O 0.8381(2) 0.2265(3) 0.42918(13) 0.0295(7) Uani 1 1 d . . .
O4 O 1.0067(2) 0.1606(2) 0.42177(12) 0.0218(7) Uani 1 1 d . . .
O5 O 1.3797(2) 0.4611(3) 0.12653(13) 0.0271(7) Uani 1 1 d . . .
O6 O 1.2726(2) 0.6216(3) 0.09485(14) 0.0339(8) Uani 1 1 d . . .
O7 O 0.8861(2) 0.9938(2) 0.49005(13) 0.0210(7) Uani 1 1 d D . .
H7A H 0.844(4) 1.050(3) 0.478(3) 0.080 Uiso 1 1 d D . .
O1W O 0.7617(4) 0.7339(6) 0.9589(3) 0.1011(18) Uani 1 1 d D . .
H1WA H 0.753(4) 0.801(3) 0.974(3) 0.080 Uiso 1 1 d D . .
H1WB H 0.705(2) 0.703(4) 0.940(3) 0.080 Uiso 1 1 d D . .


_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
C1 O1 1.255(5) . ?
C1 O2 1.268(5) . ?
C1 C2 1.496(6) . ?
C2 C3 1.392(6) . ?
C2 C7 1.395(5) . ?
C3 C4 1.390(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.387(5) . ?
C4 C9 1.482(6) . ?
C5 C6 1.388(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.390(5) . ?
C6 C8 1.498(5) . ?
C7 H7 0.9300 . ?
C8 O3 1.241(5) . ?
C8 O4 1.288(5) . ?
C9 C14 1.388(6) . ?
C9 C10 1.392(6) . ?
C10 C11 1.378(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.379(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.395(6) . ?
C12 C15 1.499(5) . ?
C13 C14 1.377(6) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 O5 1.247(5) . ?
C15 O6 1.273(5) . ?
C16 N1 1.306(6) . ?
C16 N2 1.336(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.341(8) . ?
C17 N2 1.360(8) . ?
C17 H17 0.9300 . ?
C18 N1 1.350(6) . ?
C18 H18 0.9300 . ?
C19 N2 1.475(7) . ?
C19 C20 1.505(9) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.375(8) . ?
C20 C25 1.386(8) . ?
C21 C22 1.369(9) . ?
C21 H21 0.9300 . ?
C22 C23 1.385(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.390(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.379(9) . ?
C24 C26 1.499(8) . ?
C25 H25 0.9300 . ?
C26 N3 1.466(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.350(8) . ?
C27 N4 1.353(6) . ?
C27 H27 0.9300 . ?
C28 N3 1.343(7) . ?
C28 H28 0.9300 . ?
C29 N4 1.311(6) . ?
C29 N3 1.342(6) . ?
C29 H29 0.9300 . ?
Co1 O1 2.071(3) . ?
Co1 O7 2.071(3) . ?
Co1 O4 2.076(3) 1_565 ?
Co1 N4 2.111(4) 2_655 ?
Co1 O7 2.118(3) 3_776 ?
Co1 O5 2.142(3) 2_755 ?
Co2 O7 1.968(3) . ?
Co2 O6 1.992(3) 4_576 ?
Co2 O2 2.002(3) . ?
Co2 N1 2.057(4) . ?
Co2 O4 2.253(3) 3_766 ?
N4 Co1 2.111(4) 2_645 ?
O4 Co1 2.076(3) 1_545 ?
O4 Co2 2.253(3) 3_766 ?
O5 Co1 2.142(3) 2_745 ?
O6 Co2 1.992(3) 4_675 ?
O7 Co1 2.118(3) 3_776 ?
O7 H7A 0.8200(11) . ?
O1W H1WA 0.8201(11) . ?
O1W H1WB 0.8200(11) . ?

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 C1 O2 125.4(4) . . ?
O1 C1 C2 116.4(4) . . ?
O2 C1 C2 118.1(4) . . ?
C3 C2 C7 119.0(4) . . ?
C3 C2 C1 118.9(4) . . ?
C7 C2 C1 122.0(4) . . ?
C4 C3 C2 121.7(4) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C5 C4 C3 117.9(4) . . ?
C5 C4 C9 122.4(4) . . ?
C3 C4 C9 119.6(4) . . ?
C6 C5 C4 121.3(4) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C6 C7 119.8(4) . . ?
C5 C6 C8 119.3(4) . . ?
C7 C6 C8 120.9(4) . . ?
C6 C7 C2 119.8(4) . . ?
C6 C7 H7 120.1 . . ?
C2 C7 H7 120.1 . . ?
O3 C8 O4 124.5(4) . . ?
O3 C8 C6 120.7(4) . . ?
O4 C8 C6 114.8(4) . . ?
C14 C9 C10 117.1(4) . . ?
C14 C9 C4 122.6(4) . . ?
C10 C9 C4 120.3(4) . . ?
C11 C10 C9 122.1(4) . . ?
C11 C10 H10 119.0 . . ?
C9 C10 H10 119.0 . . ?
C10 C11 C12 120.2(4) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C13 118.5(4) . . ?
C11 C12 C15 120.1(4) . . ?
C13 C12 C15 121.3(4) . . ?
C14 C13 C12 120.7(4) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C13 C14 C9 121.3(4) . . ?
C13 C14 H14 119.3 . . ?
C9 C14 H14 119.3 . . ?
O5 C15 O6 125.8(4) . . ?
O5 C15 C12 119.2(4) . . ?
O6 C15 C12 115.0(4) . . ?
N1 C16 N2 112.5(5) . . ?
N1 C16 H16 123.7 . . ?
N2 C16 H16 123.7 . . ?
C18 C17 N2 107.1(5) . . ?
C18 C17 H17 126.4 . . ?
N2 C17 H17 126.4 . . ?
C17 C18 N1 109.7(6) . . ?
C17 C18 H18 125.1 . . ?
N1 C18 H18 125.1 . . ?
N2 C19 C20 111.2(5) . . ?
N2 C19 H19A 109.4 . . ?
C20 C19 H19A 109.4 . . ?
N2 C19 H19B 109.4 . . ?
C20 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
C21 C20 C25 118.9(7) . . ?
C21 C20 C19 121.4(7) . . ?
C25 C20 C19 119.7(6) . . ?
C22 C21 C20 119.9(7) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C21 C22 C23 121.8(7) . . ?
C21 C22 H22 119.1 . . ?
C23 C22 H22 119.1 . . ?
C22 C23 C24 118.6(7) . . ?
C22 C23 H23 120.7 . . ?
C24 C23 H23 120.7 . . ?
C25 C24 C23 119.3(7) . . ?
C25 C24 C26 123.2(6) . . ?
C23 C24 C26 117.4(7) . . ?
C24 C25 C20 121.6(6) . . ?
C24 C25 H25 119.2 . . ?
C20 C25 H25 119.2 . . ?
N3 C26 C24 114.1(5) . . ?
N3 C26 H26A 108.7 . . ?
C24 C26 H26A 108.7 . . ?
N3 C26 H26B 108.7 . . ?
C24 C26 H26B 108.7 . . ?
H26A C26 H26B 107.6 . . ?
C28 C27 N4 110.0(5) . . ?
C28 C27 H27 125.0 . . ?
N4 C27 H27 125.0 . . ?
N3 C28 C27 106.9(5) . . ?
N3 C28 H28 126.6 . . ?
C27 C28 H28 126.6 . . ?
N4 C29 N3 112.2(5) . . ?
N4 C29 H29 123.9 . . ?
N3 C29 H29 123.9 . . ?
O1 Co1 O7 96.23(11) . . ?
O1 Co1 O4 172.09(11) . 1_565 ?
O7 Co1 O4 90.37(11) . 1_565 ?
O1 Co1 N4 88.24(13) . 2_655 ?
O7 Co1 N4 98.37(13) . 2_655 ?
O4 Co1 N4 95.13(13) 1_565 2_655 ?
O1 Co1 O7 95.54(11) . 3_776 ?
O7 Co1 O7 82.60(12) . 3_776 ?
O4 Co1 O7 80.95(10) 1_565 3_776 ?
N4 Co1 O7 175.98(13) 2_655 3_776 ?
O1 Co1 O5 85.61(11) . 2_755 ?
O7 Co1 O5 173.36(11) . 2_755 ?
O4 Co1 O5 87.35(11) 1_565 2_755 ?
N4 Co1 O5 88.05(13) 2_655 2_755 ?
O7 Co1 O5 90.88(11) 3_776 2_755 ?
O7 Co2 O6 106.12(12) . 4_576 ?
O7 Co2 O2 113.68(12) . . ?
O6 Co2 O2 137.73(13) 4_576 . ?
O7 Co2 N1 103.62(14) . . ?
O6 Co2 N1 93.59(14) 4_576 . ?
O2 Co2 N1 90.51(14) . . ?
O7 Co2 O4 80.02(11) . 3_766 ?
O6 Co2 O4 83.97(11) 4_576 3_766 ?
O2 Co2 O4 89.26(11) . 3_766 ?
N1 Co2 O4 176.10(13) . 3_766 ?
C16 N1 C18 105.2(4) . . ?
C16 N1 Co2 126.4(3) . . ?
C18 N1 Co2 128.4(4) . . ?
C16 N2 C17 105.4(5) . . ?
C16 N2 C19 128.5(5) . . ?
C17 N2 C19 126.1(5) . . ?
C29 N3 C28 106.2(4) . . ?
C29 N3 C26 125.1(5) . . ?
C28 N3 C26 128.7(5) . . ?
C29 N4 C27 104.7(4) . . ?
C29 N4 Co1 120.6(3) . 2_645 ?
C27 N4 Co1 134.7(4) . 2_645 ?
C1 O1 Co1 140.1(3) . . ?
C1 O2 Co2 122.7(3) . . ?
C8 O4 Co1 130.3(3) . 1_545 ?
C8 O4 Co2 127.2(3) . 3_766 ?
Co1 O4 Co2 91.12(10) 1_545 3_766 ?
C15 O5 Co1 129.4(3) . 2_745 ?
C15 O6 Co2 125.8(3) . 4_675 ?
Co2 O7 Co1 114.88(13) . . ?
Co2 O7 Co1 98.35(12) . 3_776 ?
Co1 O7 Co1 97.40(11) . 3_776 ?
Co2 O7 H7A 119(4) . . ?
Co1 O7 H7A 109(4) . . ?
Co1 O7 H7A 116(4) 3_776 . ?
H1WA O1W H1WB 114.6(2) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.090
_database_code_depnum_ccdc_archive 'CCDC 977305'
#######################################################################
#
#                 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_z

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H24 N4 O7 Zn'
_chemical_formula_weight         605.89

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

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

_cell_length_a                   8.9151(10)
_cell_length_b                   12.3303(13)
_cell_length_c                   13.3052(14)
_cell_angle_alpha                108.564(2)
_cell_angle_beta                 107.760(2)
_cell_angle_gamma                99.002(2)
_cell_volume                     1267.3(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2587
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      27.22

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             624
_exptl_absorpt_coefficient_mu    1.028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8866
_exptl_absorpt_correction_T_max  0.9223
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6388
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0633
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4428
_reflns_number_gt                3522
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

The H atoms on water molecule are very difficult to determined by X-ray 
diffraction, no suitable hydrogen bonds were found for water molecules, 
so we did not add H atoms on this water molecules


;

_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)+(0.0850P)²+0.1325P] 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         4428
_refine_ls_number_parameters     371
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0450
_refine_ls_wR_factor_ref         0.1378
_refine_ls_wR_factor_gt          0.1228
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.006
_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
C1 C 0.0098(4) 0.7226(3) 0.5094(3) 0.0283(9) Uani 1 1 d . . .
C2 C 0.0370(4) 0.7706(3) 0.4234(3) 0.0253(8) Uani 1 1 d . . .
C3 C 0.1523(4) 0.8806(3) 0.4653(3) 0.0241(8) Uani 1 1 d . . .
H3 H 0.2073 0.9211 0.5441 0.029 Uiso 1 1 calc R . .
C4 C 0.1875(4) 0.9318(3) 0.3927(3) 0.0236(8) Uani 1 1 d . . .
C5 C 0.1058(4) 0.8686(3) 0.2740(3) 0.0285(9) Uani 1 1 d . . .
H5 H 0.1305 0.8990 0.2236 0.034 Uiso 1 1 calc R . .
C6 C -0.0134(4) 0.7592(3) 0.2318(3) 0.0277(8) Uani 1 1 d . . .
C7 C -0.0489(4) 0.7104(3) 0.3057(3) 0.0252(8) Uani 1 1 d . . .
H7 H -0.1292 0.6383 0.2768 0.030 Uiso 1 1 calc R . .
C8 C -0.1026(5) 0.6978(3) 0.1043(3) 0.0282(8) Uani 1 1 d . . .
C9 C 0.3074(4) 1.0516(3) 0.4421(3) 0.0249(8) Uani 1 1 d . . .
C10 C 0.3134(5) 1.1388(3) 0.5402(3) 0.0313(9) Uani 1 1 d . . .
H10 H 0.2437 1.1215 0.5761 0.038 Uiso 1 1 calc R . .
C11 C 0.4222(5) 1.2522(3) 0.5862(3) 0.0325(9) Uani 1 1 d . . .
H11 H 0.4251 1.3093 0.6528 0.039 Uiso 1 1 calc R . .
C12 C 0.5251(4) 1.2807(3) 0.5342(3) 0.0251(8) Uani 1 1 d . . .
C13 C 0.5191(4) 1.1935(3) 0.4340(3) 0.0262(8) Uani 1 1 d . . .
H13 H 0.5860 1.2119 0.3967 0.031 Uiso 1 1 calc R . .
C14 C 0.4144(4) 1.0805(3) 0.3906(3) 0.0264(8) Uani 1 1 d . . .
H14 H 0.4150 1.0224 0.3259 0.032 Uiso 1 1 calc R . .
C15 C 0.6378(4) 1.4046(3) 0.5819(3) 0.0271(8) Uani 1 1 d . . .
C16 C 0.2117(4) 0.6039(3) 0.7293(3) 0.0278(7) Uani 1 1 d U . .
H16 H 0.2413 0.5927 0.6663 0.033 Uiso 1 1 calc R . .
C17 C 0.3157(4) 0.6307(3) 0.8314(3) 0.0225(6) Uani 1 1 d U . .
H17 H 0.4284 0.6415 0.8553 0.027 Uiso 1 1 calc R . .
C18 C 0.0675(5) 0.6171(3) 0.8294(3) 0.0284(8) Uani 1 1 d . . .
H18 H -0.0190 0.6180 0.8545 0.034 Uiso 1 1 calc R . .
C19 C 0.2975(5) 0.6797(3) 1.0219(3) 0.0361(10) Uani 1 1 d . . .
H19A H 0.3703 0.6326 1.0421 0.043 Uiso 1 1 calc R . .
H19B H 0.2116 0.6679 1.0511 0.043 Uiso 1 1 calc R . .
C20 C 0.3928(5) 0.8101(3) 1.0759(3) 0.0313(9) Uani 1 1 d . . .
C21 C 0.5565(5) 0.8448(4) 1.1487(3) 0.0353(10) Uani 1 1 d . . .
H21 H 0.6058 0.7879 1.1645 0.042 Uiso 1 1 calc R . .
C22 C 0.6472(5) 0.9637(4) 1.1981(3) 0.0400(9) Uani 1 1 d U . .
H22 H 0.7561 0.9867 1.2479 0.048 Uiso 1 1 calc R . .
C23 C 0.5733(5) 1.0485(4) 1.1725(3) 0.0408(9) Uani 1 1 d U . .
H23 H 0.6346 1.1280 1.2039 0.049 Uiso 1 1 calc R . .
C24 C 0.4087(5) 1.0155(3) 1.1001(3) 0.0327(9) Uani 1 1 d . . .
C25 C 0.3195(5) 0.8964(3) 1.0524(3) 0.0311(9) Uani 1 1 d . . .
H25 H 0.2096 0.8736 1.0043 0.037 Uiso 1 1 calc R . .
C26 C 0.3287(6) 1.1086(4) 1.0760(4) 0.0409(11) Uani 1 1 d . . .
H26A H 0.4108 1.1741 1.0813 0.049 Uiso 1 1 calc R . .
H26B H 0.2466 1.0741 0.9987 0.049 Uiso 1 1 calc R . .
C27 C 0.1182(4) 1.0836(3) 1.1560(3) 0.0267(8) Uani 1 1 d U . .
H27 H 0.0623 1.0047 1.1071 0.032 Uiso 1 1 calc R . .
C28 C 0.0870(5) 1.1526(4) 1.2401(4) 0.0405(10) Uani 1 1 d . . .
H28 H 0.0016 1.1273 1.2610 0.049 Uiso 1 1 calc R . .
C29 C 0.2923(5) 1.2613(3) 1.2390(3) 0.0326(9) Uani 1 1 d . . .
H29 H 0.3797 1.3249 1.2554 0.039 Uiso 1 1 calc R . .
N1 N 0.0541(4) 0.5937(3) 0.7227(2) 0.0269(7) Uani 1 1 d . . .
N2 N 0.2235(4) 0.6393(3) 0.8954(3) 0.0268(6) Uani 1 1 d U . .
N3 N 0.2508(4) 1.1542(3) 1.1572(3) 0.0321(8) Uani 1 1 d U . .
N4 N 0.1904(4) 1.2644(3) 1.2938(3) 0.0281(7) Uani 1 1 d . . .
O1 O -0.1086(3) 0.6280(2) 0.4711(2) 0.0332(6) Uani 1 1 d . . .
O2 O 0.0995(3) 0.7760(2) 0.6116(2) 0.0368(7) Uani 1 1 d . . .
O3 O -0.2335(4) 0.6102(3) 0.0740(2) 0.0463(8) Uani 1 1 d . . .
H3A H -0.2546 0.5625 0.0090 0.070 Uiso 1 1 calc R . .
O4 O -0.0626(4) 0.7268(3) 0.0369(3) 0.0580(9) Uani 1 1 d . . .
O5 O 0.6962(3) 1.4358(2) 0.5144(2) 0.0334(6) Uani 1 1 d . . .
O6 O 0.6718(4) 1.4729(2) 0.6819(2) 0.0417(7) Uani 1 1 d . . .
O1W O 0.5753(3) 0.5075(3) 0.8584(2) 0.0407(7) Uani 1 1 d . . .
Zn1 Zn -0.14677(5) 0.59521(3) 0.59764(3) 0.02468(17) Uani 1 1 d . . .


_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
C1 O2 1.235(4) . ?
C1 O1 1.282(4) . ?
C1 C2 1.508(5) . ?
C2 C3 1.393(5) . ?
C2 C7 1.393(5) . ?
C3 C4 1.393(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.403(5) . ?
C4 C9 1.488(5) . ?
C5 C6 1.403(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.391(5) . ?
C6 C8 1.502(5) . ?
C7 H7 0.9300 . ?
C8 O4 1.192(5) . ?
C8 O3 1.316(4) . ?
C9 C10 1.382(5) . ?
C9 C14 1.398(5) . ?
C10 C11 1.393(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.373(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.400(5) . ?
C12 C15 1.503(5) . ?
C13 C14 1.377(5) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 O6 1.237(4) . ?
C15 O5 1.291(4) . ?
C16 C17 1.290(5) . ?
C16 N1 1.364(5) . ?
C16 H16 0.9300 . ?
C17 N2 1.345(5) . ?
C17 H17 0.9300 . ?
C18 N1 1.318(5) . ?
C18 N2 1.328(5) . ?
C18 H18 0.9300 . ?
C19 N2 1.484(5) . ?
C19 C20 1.513(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.389(6) . ?
C20 C25 1.401(5) . ?
C21 C22 1.388(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.396(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.396(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.388(5) . ?
C24 C26 1.510(6) . ?
C25 H25 0.9300 . ?
C26 N3 1.469(5) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.308(6) . ?
C27 N3 1.346(5) . ?
C27 H27 0.9300 . ?
C28 N4 1.354(5) . ?
C28 H28 0.9300 . ?
C29 N3 1.323(5) . ?
C29 N4 1.326(5) . ?
C29 H29 0.9300 . ?
N1 Zn1 2.046(3) . ?
N4 Zn1 2.048(3) 2_577 ?
O1 Zn1 1.963(3) . ?
O3 H3A 0.8200 . ?
O5 Zn1 1.964(2) 1_665 ?
Zn1 O5 1.964(2) 1_445 ?
Zn1 N4 2.048(3) 2_577 ?

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 C1 O1 123.6(3) . . ?
O2 C1 C2 119.2(3) . . ?
O1 C1 C2 117.2(3) . . ?
C3 C2 C7 119.5(3) . . ?
C3 C2 C1 117.7(3) . . ?
C7 C2 C1 122.8(3) . . ?
C2 C3 C4 122.0(3) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
C3 C4 C5 118.3(3) . . ?
C3 C4 C9 119.8(3) . . ?
C5 C4 C9 121.9(3) . . ?
C6 C5 C4 119.7(3) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C7 C6 C5 121.1(3) . . ?
C7 C6 C8 121.3(3) . . ?
C5 C6 C8 117.6(3) . . ?
C6 C7 C2 119.3(3) . . ?
C6 C7 H7 120.3 . . ?
C2 C7 H7 120.3 . . ?
O4 C8 O3 123.0(4) . . ?
O4 C8 C6 123.9(3) . . ?
O3 C8 C6 113.1(3) . . ?
C10 C9 C14 118.0(3) . . ?
C10 C9 C4 120.3(3) . . ?
C14 C9 C4 121.8(3) . . ?
C9 C10 C11 121.1(3) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C12 C11 C10 120.7(4) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 118.8(3) . . ?
C11 C12 C15 120.4(3) . . ?
C13 C12 C15 120.8(3) . . ?
C14 C13 C12 120.3(3) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C9 121.2(3) . . ?
C13 C14 H14 119.4 . . ?
C9 C14 H14 119.4 . . ?
O6 C15 O5 122.2(3) . . ?
O6 C15 C12 120.6(3) . . ?
O5 C15 C12 117.2(3) . . ?
C17 C16 N1 113.6(3) . . ?
C17 C16 H16 123.2 . . ?
N1 C16 H16 123.2 . . ?
C16 C17 N2 104.0(3) . . ?
C16 C17 H17 128.0 . . ?
N2 C17 H17 128.0 . . ?
N1 C18 N2 109.6(3) . . ?
N1 C18 H18 125.2 . . ?
N2 C18 H18 125.2 . . ?
N2 C19 C20 110.4(3) . . ?
N2 C19 H19A 109.6 . . ?
C20 C19 H19A 109.6 . . ?
N2 C19 H19B 109.6 . . ?
C20 C19 H19B 109.6 . . ?
H19A C19 H19B 108.1 . . ?
C21 C20 C25 119.3(4) . . ?
C21 C20 C19 119.5(4) . . ?
C25 C20 C19 121.1(3) . . ?
C22 C21 C20 120.6(4) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C23 119.4(4) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
C24 C23 C22 120.8(4) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C25 C24 C23 119.0(4) . . ?
C25 C24 C26 120.7(4) . . ?
C23 C24 C26 120.3(4) . . ?
C24 C25 C20 120.8(4) . . ?
C24 C25 H25 119.6 . . ?
C20 C25 H25 119.6 . . ?
N3 C26 C24 111.5(3) . . ?
N3 C26 H26A 109.3 . . ?
C24 C26 H26A 109.3 . . ?
N3 C26 H26B 109.3 . . ?
C24 C26 H26B 109.3 . . ?
H26A C26 H26B 108.0 . . ?
C28 C27 N3 103.3(3) . . ?
C28 C27 H27 128.3 . . ?
N3 C27 H27 128.3 . . ?
C27 C28 N4 113.8(4) . . ?
C27 C28 H28 123.1 . . ?
N4 C28 H28 123.1 . . ?
N3 C29 N4 109.7(3) . . ?
N3 C29 H29 125.1 . . ?
N4 C29 H29 125.1 . . ?
C18 N1 C16 103.2(3) . . ?
C18 N1 Zn1 124.0(3) . . ?
C16 N1 Zn1 130.2(3) . . ?
C18 N2 C17 109.6(3) . . ?
C18 N2 C19 128.3(3) . . ?
C17 N2 C19 121.9(3) . . ?
C29 N3 C27 110.0(3) . . ?
C29 N3 C26 129.3(4) . . ?
C27 N3 C26 120.7(3) . . ?
C29 N4 C28 103.2(3) . . ?
C29 N4 Zn1 131.2(3) . 2_577 ?
C28 N4 Zn1 123.9(3) . 2_577 ?
C1 O1 Zn1 110.8(2) . . ?
C8 O3 H3A 109.5 . . ?
C15 O5 Zn1 110.3(2) . 1_665 ?
O1 Zn1 O5 100.89(11) . 1_445 ?
O1 Zn1 N1 116.45(12) . . ?
O5 Zn1 N1 110.61(12) 1_445 . ?
O1 Zn1 N4 112.49(12) . 2_577 ?
O5 Zn1 N4 123.15(12) 1_445 2_577 ?
N1 Zn1 N4 94.28(12) . 2_577 ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.084
_database_code_depnum_ccdc_archive 'CCDC 977306'
#######################################################################
#
#                 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_z

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C67 H49 Co2 N8 O14'
_chemical_formula_weight         1308.00

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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)

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

_cell_length_a                   11.7332(4)
_cell_length_b                   15.2259(6)
_cell_length_c                   16.1433(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.4970(10)
_cell_angle_gamma                90.00
_cell_volume                     2815.65(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5191
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      26.61

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1346
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7525
_exptl_absorpt_correction_T_max  0.8946
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14627
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9085
_reflns_number_gt                8188
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0730P)²+1.5972P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(17)
_refine_ls_number_reflns         9085
_refine_ls_number_parameters     888
_refine_ls_number_restraints     159
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0452
_refine_ls_wR_factor_ref         0.1237
_refine_ls_wR_factor_gt          0.1183
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.004
_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 0.89440(4) 0.84340(3) 0.97782(3) 0.02513(11) Uani 1 1 d . . .
Co2 Co 1.12642(3) 1.03672(3) 1.01265(3) 0.02538(11) Uani 1 1 d . . .
O1 O 0.81867(19) 0.72554(15) 0.98670(16) 0.0286(6) Uani 1 1 d . . .
O2 O 0.71581(18) 0.60445(14) 0.98194(15) 0.0270(6) Uani 1 1 d . . .
O3 O 0.5237(3) 0.96732(18) 1.07737(17) 0.0497(8) Uani 1 1 d . . .
O4 O 0.4217(2) 1.00927(16) 0.95005(16) 0.0391(7) Uani 1 1 d . . .
H4 H 0.3876 1.0425 0.9765 0.059 Uiso 1 1 calc R . .
O5 O 0.0320(3) 0.5313(2) 0.59118(18) 0.0561(8) Uani 1 1 d . . .
O6 O -0.0275(2) 0.6695(2) 0.56427(18) 0.0613(10) Uani 1 1 d . . .
H6 H -0.0733 0.6470 0.5243 0.092 Uiso 1 1 calc R . .
O7 O 0.95643(18) 1.03222(18) 1.02446(14) 0.0313(6) Uani 1 1 d . . .
O8 O 0.7983(2) 0.95432(16) 0.96898(16) 0.0346(7) Uani 1 1 d . . .
O9 O 0.94155(18) 1.35041(18) 1.03639(15) 0.0335(6) Uani 1 1 d . . .
O10 O 0.7803(2) 1.42229(16) 0.97953(17) 0.0353(7) Uani 1 1 d . . .
O11 O 0.1610(3) 1.2721(2) 0.5902(2) 0.0715(11) Uani 1 1 d . . .
O12 O 0.1817(3) 1.1307(2) 0.56268(18) 0.0540(9) Uani 1 1 d . . .
N1 N 0.8513(2) 0.8313(2) 0.84368(18) 0.0368(8) Uani 1 1 d . . .
N2 N 0.7488(3) 0.8149(2) 0.7144(2) 0.0444(10) Uani 1 1 d . . .
N3 N 0.0509(3) 0.8307(3) 0.24062(19) 0.0434(9) Uani 1 1 d . . .
N4 N -0.0575(3) 0.8420(3) 0.11089(18) 0.0401(8) Uani 1 1 d . . .
N5 N 1.1685(2) 1.0470(2) 1.14466(18) 0.0380(8) Uani 1 1 d . . .
N6 N 1.2767(3) 1.0533(3) 1.27459(19) 0.0454(10) Uani 1 1 d . . .
N7 N 1.9686(3) 1.0657(2) 1.75375(19) 0.0406(9) Uani 1 1 d . . .
N8 N 2.0766(3) 1.0555(2) 1.88273(19) 0.0376(9) Uani 1 1 d . . .
C1 C 0.7229(3) 0.6879(2) 0.97569(17) 0.0208(7) Uani 1 1 d . . .
C2 C 0.6116(3) 0.7374(2) 0.9533(2) 0.0238(8) Uani 1 1 d . . .
C3 C 0.5165(3) 0.7022(2) 0.89428(19) 0.0260(8) Uani 1 1 d . . .
H3 H 0.5213 0.6454 0.8742 0.031 Uiso 1 1 calc R . .
C4 C 0.4152(3) 0.7512(2) 0.8655(2) 0.0274(8) Uani 1 1 d . . .
C5 C 0.4095(3) 0.8344(2) 0.8987(2) 0.0289(8) Uani 1 1 d . . .
H5 H 0.3434 0.8684 0.8791 0.035 Uiso 1 1 calc R . .
C6 C 0.4996(3) 0.8685(2) 0.9603(2) 0.0276(8) Uani 1 1 d . . .
C7 C 0.6014(3) 0.8197(2) 0.9877(2) 0.0254(8) Uani 1 1 d . . .
H7 H 0.6622 0.8423 1.0289 0.031 Uiso 1 1 calc R . .
C8 C 0.4851(3) 0.9531(2) 1.0030(3) 0.0331(9) Uani 1 1 d . . .
C9 C 0.3165(3) 0.7143(2) 0.8008(2) 0.0308(9) Uani 1 1 d . . .
C10 C 0.2919(3) 0.6262(3) 0.7957(2) 0.0378(10) Uani 1 1 d . . .
H10 H 0.3362 0.5881 0.8348 0.045 Uiso 1 1 calc R . .
C11 C 0.2015(3) 0.5929(3) 0.7330(2) 0.0403(10) Uani 1 1 d . . .
H11 H 0.1864 0.5329 0.7309 0.048 Uiso 1 1 calc R . .
C12 C 0.1350(3) 0.6473(3) 0.6746(2) 0.0314(9) Uani 1 1 d . . .
C13 C 0.1559(3) 0.7362(3) 0.6796(2) 0.0380(10) Uani 1 1 d . . .
H13 H 0.1091 0.7741 0.6416 0.046 Uiso 1 1 calc R . .
C14 C 0.2473(3) 0.7696(3) 0.7418(2) 0.0360(10) Uani 1 1 d . . .
H14 H 0.2622 0.8296 0.7438 0.043 Uiso 1 1 calc R . .
C15 C 0.0399(3) 0.6100(3) 0.6050(2) 0.0402(10) Uani 1 1 d . . .
C16 C 0.8502(3) 1.0270(2) 0.9914(2) 0.0241(7) Uani 1 1 d . . .
C17 C 0.7813(3) 1.1094(2) 0.9716(2) 0.0249(8) Uani 1 1 d . . .
C18 C 0.6712(3) 1.1084(2) 0.9157(2) 0.0259(8) Uani 1 1 d . . .
H18 H 0.6363 1.0549 0.8975 0.031 Uiso 1 1 calc R . .
C19 C 0.6137(2) 1.1868(3) 0.88721(18) 0.0239(7) Uani 1 1 d . . .
C20 C 0.6669(3) 1.2649(2) 0.9190(2) 0.0257(8) Uani 1 1 d . . .
H20 H 0.6287 1.3177 0.9026 0.031 Uiso 1 1 calc R . .
C21 C 0.7754(3) 1.2669(2) 0.9746(2) 0.0231(8) Uani 1 1 d . . .
C22 C 0.8328(3) 1.1891(3) 1.00048(19) 0.0256(7) Uani 1 1 d . . .
H22 H 0.9058 1.1900 1.0372 0.031 Uiso 1 1 calc R . .
C23 C 0.8360(3) 1.3527(2) 0.9990(2) 0.0252(8) Uani 1 1 d . . .
C24 C 0.5037(3) 1.1865(3) 0.82041(18) 0.0270(8) Uani 1 1 d . . .
C25 C 0.4398(3) 1.2648(3) 0.7983(2) 0.0399(10) Uani 1 1 d . . .
H25 H 0.4614 1.3153 0.8301 0.048 Uiso 1 1 calc R . .
C26 C 0.3466(3) 1.2673(3) 0.7305(2) 0.0421(11) Uani 1 1 d . . .
H26 H 0.3070 1.3201 0.7168 0.051 Uiso 1 1 calc R . .
C27 C 0.3096(3) 1.1937(3) 0.6820(2) 0.0337(8) Uani 1 1 d . . .
C28 C 0.3695(3) 1.1163(3) 0.7039(2) 0.0388(10) Uani 1 1 d . . .
H28 H 0.3459 1.0656 0.6729 0.047 Uiso 1 1 calc R . .
C29 C 0.4661(3) 1.1137(3) 0.7729(2) 0.0352(10) Uani 1 1 d . . .
H29 H 0.5055 1.0608 0.7866 0.042 Uiso 1 1 calc R . .
C30 C 0.2089(3) 1.2005(3) 0.6059(2) 0.0396(10) Uani 1 1 d . . .
C31 C 0.9250(4) 0.8215(4) 0.7899(3) 0.0689(18) Uani 1 1 d . . .
H31 H 1.0061 0.8208 0.8057 0.083 Uiso 1 1 calc R . .
C32 C 0.8622(4) 0.8130(5) 0.7103(3) 0.083(2) Uani 1 1 d . . .
H32 H 0.8914 0.8069 0.6614 0.099 Uiso 1 1 calc R . .
C33 C 0.7455(3) 0.8274(3) 0.7951(2) 0.0421(11) Uani 1 1 d . . .
H33 H 0.6771 0.8328 0.8150 0.051 Uiso 1 1 calc R . .
C34 C 0.6486(4) 0.8099(3) 0.6443(2) 0.0481(12) Uani 1 1 d . . .
C35 C 0.5383(4) 0.7989(6) 0.6587(3) 0.105(3) Uani 1 1 d . . .
H35 H 0.5278 0.7902 0.7136 0.125 Uiso 1 1 calc R . .
C36 C 0.4433(4) 0.8009(6) 0.5916(3) 0.104(3) Uani 1 1 d . . .
H36 H 0.3688 0.7979 0.6026 0.124 Uiso 1 1 calc R . .
C37 C 0.4545(4) 0.8072(3) 0.5099(2) 0.0464(12) Uani 1 1 d . . .
C38 C 0.5656(4) 0.8126(4) 0.4965(3) 0.075(2) Uani 1 1 d . . .
H38 H 0.5757 0.8154 0.4410 0.090 Uiso 1 1 calc R . .
C39 C 0.6625(4) 0.8140(4) 0.5617(3) 0.0685(18) Uani 1 1 d . . .
H39 H 0.7367 0.8178 0.5503 0.082 Uiso 1 1 calc R . .
C40 C 0.3499(4) 0.8103(3) 0.4380(2) 0.0495(13) Uani 1 1 d . . .
C41 C 0.1381(8) 0.8094(8) 0.3889(5) 0.0587(12) Uani 0.50 1 d PU . .
H41A H 0.0612 0.8024 0.3995 0.070 Uiso 0.50 1 d PR . .
C41A C 0.1515(8) 0.8614(8) 0.3864(5) 0.0567(12) Uani 0.50 1 d PU . .
H41B H 0.0817 0.8890 0.3956 0.068 Uiso 0.50 1 d PR . .
C42 C 0.2377(8) 0.8005(8) 0.4539(6) 0.0591(12) Uani 0.50 1 d PU . .
H42A H 0.2292 0.7873 0.5104 0.071 Uiso 0.50 1 d PR . .
C42A C 0.2489(8) 0.8568(8) 0.4509(5) 0.0558(12) Uani 0.50 1 d PU . .
H42B H 0.2495 0.8848 0.5042 0.067 Uiso 0.50 1 d PR . .
C43 C 0.1525(3) 0.8221(3) 0.3077(2) 0.0405(11) Uani 1 1 d . . .
C44 C 0.2565(4) 0.8018(5) 0.2932(3) 0.085(2) Uani 1 1 d . . .
H44 H 0.2630 0.7928 0.2374 0.102 Uiso 1 1 calc R . .
C45 C 0.3559(4) 0.7935(5) 0.3574(3) 0.090(2) Uani 1 1 d . . .
H45 H 0.4262 0.7765 0.3447 0.108 Uiso 1 1 calc R . .
C46 C -0.1129(7) 0.8878(8) 0.1674(5) 0.0570(14) Uani 0.50 1 d PU . .
H46 H -0.1841 0.9204 0.1503 0.068 Uiso 0.50 1 d PR . .
C46A C -0.1369(6) 0.8106(8) 0.1660(6) 0.0666(15) Uani 0.50 1 d PDU . .
H46A H -0.2176 0.7936 0.1520 0.080 Uiso 0.50 1 d PR . .
C47 C -0.0566(8) 0.8787(8) 0.2477(5) 0.0582(14) Uani 0.50 1 d PU . .
H47A H -0.0791 0.8973 0.2987 0.070 Uiso 0.50 1 d PR . .
C47A C -0.0564(9) 0.8102(9) 0.2440(6) 0.0649(15) Uani 0.50 1 d PU . .
H47B H -0.0839 0.7952 0.2940 0.078 Uiso 0.50 1 d PR . .
C48 C 0.0483(4) 0.8306(4) 0.1580(3) 0.0621(15) Uani 1 1 d D . .
H48 H 0.1144 0.8233 0.1357 0.075 Uiso 1 1 calc R . .
C49 C 1.1010(4) 1.0655(6) 1.2001(3) 0.101(3) Uani 1 1 d . . .
H49 H 1.0204 1.0722 1.1856 0.121 Uiso 1 1 calc R . .
C50 C 1.1652(4) 1.0729(6) 1.2782(3) 0.121(4) Uani 1 1 d . . .
H50 H 1.1386 1.0886 1.3264 0.145 Uiso 1 1 calc R . .
C51 C 1.2739(3) 1.0407(3) 1.1931(2) 0.0412(10) Uani 1 1 d . . .
H51 H 1.3400 1.0285 1.1721 0.049 Uiso 1 1 calc R . .
C52 C 1.3774(3) 1.0542(3) 1.3439(2) 0.0447(12) Uani 1 1 d . . .
C53 C 1.3627(4) 1.0661(4) 1.4235(3) 0.0654(18) Uani 1 1 d . . .
H53 H 1.2882 1.0732 1.4337 0.079 Uiso 1 1 calc R . .
C54 C 1.4590(4) 1.0676(4) 1.4896(3) 0.0685(18) Uani 1 1 d . . .
H54 H 1.4470 1.0755 1.5442 0.082 Uiso 1 1 calc R . .
C55 C 1.5691(4) 1.0583(3) 1.4801(2) 0.0501(13) Uani 1 1 d . . .
C56 C 1.5833(4) 1.0442(6) 1.3980(3) 0.102(3) Uani 1 1 d . . .
H56 H 1.6583 1.0392 1.3883 0.123 Uiso 1 1 calc R . .
C57 C 1.4872(4) 1.0374(6) 1.3292(3) 0.100(3) Uani 1 1 d . . .
H57 H 1.4972 1.0222 1.2754 0.120 Uiso 1 1 calc R . .
C59A C 1.7858(8) 1.0630(9) 1.5382(6) 0.0738(12) Uani 0.50 1 d PU . .
H59A H 1.7963 1.0538 1.4815 0.089 Uiso 0.50 1 d PR . .
C60A C 1.8860(8) 1.0701(9) 1.6065(5) 0.0719(12) Uani 0.50 1 d PU . .
H60A H 1.9632 1.0722 1.5958 0.086 Uiso 0.50 1 d PR . .
C62A C 1.7627(9) 1.0574(10) 1.7012(6) 0.0850(12) Uani 0.50 1 d PU . .
H62A H 1.7546 1.0496 1.7586 0.102 Uiso 0.50 1 d PR . .
C63 C 1.6676(2) 1.0241(2) 1.62766(15) 0.0925(13) Uani 0.50 1 d PU . .
H63A H 1.5967 0.9963 1.6344 0.111 Uiso 0.50 1 d PR . .
C58 C 1.6739(2) 1.0617(2) 1.55033(15) 0.0484(13) Uani 1 1 d R . .
C59 C 1.7764(2) 1.1020(2) 1.54055(15) 0.0719(13) Uani 0.50 1 d PRU . .
H59B H 1.7808 1.1280 1.4871 0.086 Uiso 0.50 1 d PR . .
C60 C 1.8726(2) 1.1048(2) 1.60812(15) 0.0712(13) Uani 0.50 1 d PRU . .
H60B H 1.9435 1.1326 1.6013 0.085 Uiso 0.50 1 d PR . .
C61 C 1.8663(2) 1.0672(2) 1.68544(15) 0.0385(10) Uani 1 1 d R . .
C62 C 1.7637(2) 1.0268(2) 1.69523(15) 0.0852(13) Uani 0.50 1 d PRU . .
H62B H 1.7594 1.0008 1.7486 0.102 Uiso 0.50 1 d PR . .
C63A C 1.6667(5) 1.0549(6) 1.6354(4) 0.0969(12) Uani 1 1 d U . .
H63B H 1.5905 1.0506 1.6478 0.116 Uiso 1 1 d R . .
C64 C 2.1461(5) 1.0370(6) 1.8277(4) 0.0945(13) Uani 1 1 d U . .
H64 H 2.2274 1.0224 1.8447 0.113 Uiso 1 1 d R . .
C64A C 2.1325(7) 1.1219(9) 1.8327(7) 0.0901(16) Uani 0.50 1 d PDU . .
H64A H 2.2021 1.1559 1.8522 0.108 Uiso 0.50 1 d PR . .
C65 C 2.0853(8) 1.0433(10) 1.7445(6) 0.0779(15) Uani 0.50 1 d PU . .
H65 H 2.1128 1.0349 1.6932 0.094 Uiso 0.50 1 d PR . .
C65A C 2.0613(9) 1.1145(10) 1.7523(7) 0.0843(16) Uani 0.50 1 d PU . .
H65A H 2.0769 1.1442 1.7034 0.101 Uiso 0.50 1 d PR . .
C66 C 1.9734(3) 1.0565(3) 1.8341(2) 0.0501(13) Uani 1 1 d D . .
H66 H 1.9064 1.0510 1.8557 0.060 Uiso 1 1 calc R . .
O2W O 0.1838(6) 0.9502(4) 0.6108(5) 0.187(3) Uani 1 1 d . . .
H2WA H 0.1875 1.0036 0.5982 0.224 Uiso 1 1 d R . .
H2WB H 0.1200 0.9281 0.5876 0.224 Uiso 1 1 d R . .
O1W O 0.0304(4) 0.3835(3) 0.4703(3) 0.0958(15) Uani 1 1 d . . .
H1WA H 0.0438 0.4344 0.4920 0.115 Uiso 1 1 d R . .
H1WB H 0.0772 0.3473 0.5002 0.115 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
Co1 O9 1.990(2) 2_747 ?
Co1 O8 2.018(2) . ?
Co1 O1 2.021(2) . ?
Co1 N4 2.100(3) 1_656 ?
Co1 N1 2.123(3) . ?
Co2 O7 2.045(2) . ?
Co2 O10 2.047(2) 2_747 ?
Co2 N8 2.072(3) 1_454 ?
Co2 N5 2.087(3) . ?
Co2 O2 2.104(2) 2_757 ?
O1 C1 1.239(4) . ?
O2 C1 1.279(4) . ?
O2 Co2 2.104(2) 2_747 ?
O3 C8 1.207(5) . ?
O4 C8 1.320(4) . ?
O4 H4 0.8200 . ?
O5 C15 1.218(5) . ?
O6 C15 1.287(5) . ?
O6 H6 0.8200 . ?
O7 C16 1.248(4) . ?
O8 C16 1.277(4) . ?
O9 C23 1.255(4) . ?
O9 Co1 1.990(2) 2_757 ?
O10 C23 1.249(4) . ?
O10 Co2 2.047(2) 2_757 ?
O11 C30 1.227(6) . ?
O12 C30 1.274(5) . ?
N1 C33 1.318(5) . ?
N1 C31 1.360(6) . ?
N2 C33 1.326(5) . ?
N2 C32 1.346(6) . ?
N2 C34 1.447(5) . ?
N3 C47A 1.310(11) . ?
N3 C48 1.327(5) . ?
N3 C43 1.432(5) . ?
N3 C47 1.483(10) . ?
N4 C48 1.320(5) . ?
N4 C46 1.413(10) . ?
N4 C46A 1.499(9) . ?
N4 Co1 2.100(3) 1_454 ?
N5 C51 1.316(4) . ?
N5 C49 1.347(6) . ?
N6 C51 1.323(5) . ?
N6 C50 1.355(6) . ?
N6 C52 1.441(4) . ?
N7 C66 1.294(5) . ?
N7 C65A 1.322(13) . ?
N7 C61 1.444(4) . ?
N7 C65 1.450(11) . ?
N8 C66 1.293(5) . ?
N8 C64 1.359(7) . ?
N8 C64A 1.528(11) . ?
N8 Co2 2.072(3) 1_656 ?
C1 C2 1.484(4) . ?
C2 C7 1.386(5) . ?
C2 C3 1.407(4) . ?
C3 C4 1.395(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.383(5) . ?
C4 C9 1.492(4) . ?
C5 C6 1.386(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.395(5) . ?
C6 C8 1.488(5) . ?
C7 H7 0.9300 . ?
C9 C10 1.370(5) . ?
C9 C14 1.393(5) . ?
C10 C11 1.393(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.366(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.376(5) . ?
C12 C15 1.512(5) . ?
C13 C14 1.396(5) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C16 C17 1.490(5) . ?
C17 C22 1.390(5) . ?
C17 C18 1.406(4) . ?
C18 C19 1.400(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.390(5) . ?
C19 C24 1.492(4) . ?
C20 C21 1.390(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.382(5) . ?
C21 C23 1.499(5) . ?
C22 H22 0.9300 . ?
C24 C29 1.366(5) . ?
C24 C25 1.411(5) . ?
C25 C26 1.370(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.382(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.378(6) . ?
C27 C30 1.513(4) . ?
C28 C29 1.407(5) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C31 C32 1.343(6) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 C35 1.374(6) . ?
C34 C39 1.380(6) . ?
C35 C36 1.377(6) . ?
C35 H35 0.9300 . ?
C36 C37 1.356(6) . ?
C36 H36 0.9300 . ?
C37 C38 1.369(6) . ?
C37 C40 1.497(5) . ?
C38 C39 1.372(6) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C40 C45 1.341(6) . ?
C40 C42 1.403(11) . ?
C41 C43 1.371(10) . ?
C41 C42 1.398(12) . ?
C44 H44 0.9300 . ?
C45 H45 0.9300 . ?
C46 H46 0.9600 . ?
C48 H48 0.9300 . ?
C49 C50 1.325(6) . ?
C49 H49 0.9300 . ?
C50 H50 0.9300 . ?
C51 H51 0.9300 . ?
C52 C53 1.345(6) . ?
C52 C57 1.384(6) . ?
C53 C54 1.377(6) . ?
C53 H53 0.9300 . ?
C54 C55 1.341(6) . ?
C54 H54 0.9300 . ?
C55 C56 1.387(6) . ?
C55 C58 1.483(4) . ?
C56 C57 1.404(6) . ?
C56 H56 0.9300 . ?
C57 H57 0.9300 . ?
C63 C62 1.3902 . ?
C58 C59 1.3899 . ?
C59 C60 1.3902 . ?
C60 C61 1.3898 . ?
C61 C62 1.3902 . ?
C64 C65 1.381(11) . ?
C64 H64 0.9600 . ?
C65 H65 0.9599 . ?
C66 H66 0.9300 . ?
O2W H2WA 0.8410 . ?
O2W H2WB 0.8325 . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8498 . ?

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
O9 Co1 O8 119.09(11) 2_747 . ?
O9 Co1 O1 120.45(11) 2_747 . ?
O8 Co1 O1 120.04(10) . . ?
O9 Co1 N4 93.78(11) 2_747 1_656 ?
O8 Co1 N4 95.91(13) . 1_656 ?
O1 Co1 N4 86.76(12) . 1_656 ?
O9 Co1 N1 84.83(10) 2_747 . ?
O8 Co1 N1 89.68(12) . . ?
O1 Co1 N1 89.08(12) . . ?
N4 Co1 N1 174.19(15) 1_656 . ?
O7 Co2 O10 119.00(11) . 2_747 ?
O7 Co2 N8 91.83(11) . 1_454 ?
O10 Co2 N8 102.11(12) 2_747 1_454 ?
O7 Co2 N5 85.82(10) . . ?
O10 Co2 N5 89.75(12) 2_747 . ?
N8 Co2 N5 167.47(14) 1_454 . ?
O7 Co2 O2 151.57(10) . 2_757 ?
O10 Co2 O2 87.76(9) 2_747 2_757 ?
N8 Co2 O2 91.55(11) 1_454 2_757 ?
N5 Co2 O2 84.81(11) . 2_757 ?
C1 O1 Co1 143.1(2) . . ?
C1 O2 Co2 114.7(2) . 2_747 ?
C8 O4 H4 109.5 . . ?
C15 O6 H6 109.5 . . ?
C16 O7 Co2 150.0(2) . . ?
C16 O8 Co1 118.7(2) . . ?
C23 O9 Co1 145.5(2) . 2_757 ?
C23 O10 Co2 117.6(2) . 2_757 ?
C33 N1 C31 105.2(3) . . ?
C33 N1 Co1 126.6(3) . . ?
C31 N1 Co1 128.1(2) . . ?
C33 N2 C32 107.0(3) . . ?
C33 N2 C34 125.8(3) . . ?
C32 N2 C34 127.2(3) . . ?
C48 N3 C43 126.4(3) . . ?
C48 N3 C47 104.1(4) . . ?
C43 N3 C47 124.7(4) . . ?
C48 N4 C46 101.5(4) . . ?
C48 N4 C46A 104.1(4) . . ?
C46 N4 C46A 48.9(6) . . ?
C48 N4 Co1 127.0(3) . 1_454 ?
C46 N4 Co1 126.6(4) . 1_454 ?
C51 N5 C49 103.4(3) . . ?
C51 N5 Co2 125.8(3) . . ?
C49 N5 Co2 130.7(3) . . ?
C51 N6 C50 105.0(3) . . ?
C51 N6 C52 127.8(3) . . ?
C50 N6 C52 127.0(4) . . ?
C66 N7 C61 128.0(3) . . ?
C66 N7 C65 103.9(5) . . ?
C61 N7 C65 125.0(5) . . ?
C66 N8 C64 102.8(4) . . ?
C66 N8 Co2 129.6(3) . 1_656 ?
C64 N8 Co2 123.8(3) . 1_656 ?
O1 C1 O2 121.4(3) . . ?
O1 C1 C2 121.5(3) . . ?
O2 C1 C2 117.1(3) . . ?
C7 C2 C3 119.4(3) . . ?
C7 C2 C1 120.6(3) . . ?
C3 C2 C1 119.9(3) . . ?
C4 C3 C2 121.1(3) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C5 C4 C3 118.0(3) . . ?
C5 C4 C9 121.4(3) . . ?
C3 C4 C9 120.6(3) . . ?
C4 C5 C6 121.9(3) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C5 C6 C7 119.7(3) . . ?
C5 C6 C8 120.8(3) . . ?
C7 C6 C8 119.3(3) . . ?
C2 C7 C6 119.8(3) . . ?
C2 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
O3 C8 O4 124.4(3) . . ?
O3 C8 C6 124.1(3) . . ?
O4 C8 C6 111.4(3) . . ?
C10 C9 C14 117.8(3) . . ?
C10 C9 C4 122.2(3) . . ?
C14 C9 C4 120.0(3) . . ?
C9 C10 C11 121.2(3) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C12 C11 C10 120.8(4) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 119.2(3) . . ?
C11 C12 C15 120.3(4) . . ?
C13 C12 C15 120.4(3) . . ?
C12 C13 C14 120.0(4) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C9 C14 C13 121.0(4) . . ?
C9 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
O5 C15 O6 125.9(3) . . ?
O5 C15 C12 121.3(4) . . ?
O6 C15 C12 112.8(4) . . ?
O7 C16 O8 123.2(3) . . ?
O7 C16 C17 118.9(3) . . ?
O8 C16 C17 117.8(3) . . ?
C22 C17 C18 119.8(3) . . ?
C22 C17 C16 119.1(3) . . ?
C18 C17 C16 120.6(3) . . ?
C19 C18 C17 120.8(3) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C20 C19 C18 117.6(3) . . ?
C20 C19 C24 121.3(3) . . ?
C18 C19 C24 121.0(3) . . ?
C21 C20 C19 122.2(3) . . ?
C21 C20 H20 118.9 . . ?
C19 C20 H20 118.9 . . ?
C22 C21 C20 119.7(3) . . ?
C22 C21 C23 119.7(3) . . ?
C20 C21 C23 120.3(3) . . ?
C21 C22 C17 119.9(3) . . ?
C21 C22 H22 120.1 . . ?
C17 C22 H22 120.1 . . ?
O10 C23 O9 123.6(3) . . ?
O10 C23 C21 118.7(3) . . ?
O9 C23 C21 117.7(3) . . ?
C29 C24 C25 117.0(3) . . ?
C29 C24 C19 122.1(3) . . ?
C25 C24 C19 120.6(3) . . ?
C26 C25 C24 121.0(4) . . ?
C26 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
C25 C26 C27 121.8(4) . . ?
C25 C26 H26 119.1 . . ?
C27 C26 H26 119.1 . . ?
C28 C27 C26 117.9(3) . . ?
C28 C27 C30 122.1(4) . . ?
C26 C27 C30 119.9(4) . . ?
C27 C28 C29 120.4(4) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 H28 119.8 . . ?
C24 C29 C28 121.8(3) . . ?
C24 C29 H29 119.1 . . ?
C28 C29 H29 119.1 . . ?
O11 C30 O12 125.4(3) . . ?
O11 C30 C27 118.0(4) . . ?
O12 C30 C27 116.6(4) . . ?
C32 C31 N1 109.2(4) . . ?
C32 C31 H31 125.4 . . ?
N1 C31 H31 125.4 . . ?
C31 C32 N2 107.1(4) . . ?
C31 C32 H32 126.5 . . ?
N2 C32 H32 126.5 . . ?
N1 C33 N2 111.5(3) . . ?
N1 C33 H33 124.2 . . ?
N2 C33 H33 124.2 . . ?
C35 C34 C39 118.8(4) . . ?
C35 C34 N2 120.7(4) . . ?
C39 C34 N2 120.5(4) . . ?
C34 C35 C36 119.7(4) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C37 C36 C35 122.3(5) . . ?
C37 C36 H36 118.9 . . ?
C35 C36 H36 118.9 . . ?
C36 C37 C38 117.0(4) . . ?
C36 C37 C40 121.4(4) . . ?
C38 C37 C40 121.6(4) . . ?
C37 C38 C39 122.6(4) . . ?
C37 C38 H38 118.7 . . ?
C39 C38 H38 118.7 . . ?
C38 C39 C34 119.3(4) . . ?
C38 C39 H39 120.4 . . ?
C34 C39 H39 120.4 . . ?
C45 C40 C42 113.9(5) . . ?
C45 C40 C37 122.7(4) . . ?
C42 C40 C37 119.9(5) . . ?
C43 C41 C42 118.4(8) . . ?
N4 C48 N3 113.2(4) . . ?
N4 C48 H48 123.4 . . ?
N3 C48 H48 123.4 . . ?
C50 C49 N5 110.8(4) . . ?
C50 C49 H49 124.6 . . ?
N5 C49 H49 124.6 . . ?
C49 C50 N6 107.2(4) . . ?
C49 C50 H50 126.4 . . ?
N6 C50 H50 126.4 . . ?
N5 C51 N6 113.4(3) . . ?
N5 C51 H51 123.3 . . ?
N6 C51 H51 123.3 . . ?
C53 C52 C57 120.4(4) . . ?
C53 C52 N6 119.3(4) . . ?
C57 C52 N6 120.2(3) . . ?
C52 C53 C54 119.3(4) . . ?
C52 C53 H53 120.3 . . ?
C54 C53 H53 120.3 . . ?
C55 C54 C53 123.9(4) . . ?
C55 C54 H54 118.0 . . ?
C53 C54 H54 118.0 . . ?
C54 C55 C56 116.4(4) . . ?
C54 C55 C58 124.7(4) . . ?
C56 C55 C58 119.0(4) . . ?
C55 C56 C57 121.6(4) . . ?
C55 C56 H56 119.2 . . ?
C57 C56 H56 119.2 . . ?
C52 C57 C56 118.0(4) . . ?
C52 C57 H57 121.0 . . ?
C56 C57 H57 121.0 . . ?
C59 C58 C55 121.6(2) . . ?
C63 C58 C55 118.4(2) . . ?
C60 C61 N7 119.69(17) . . ?
C62 C61 N7 120.21(17) . . ?
C63 C62 C61 120.0 . . ?
N7 C65 H65 128.4 . . ?
N8 C66 N7 116.2(4) . . ?
N8 C66 H66 121.9 . . ?
N7 C66 H66 121.9 . . ?
H2WA O2W H2WB 111.7 . . ?
H1WA O1W H1WB 108.6 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.065
_database_code_depnum_ccdc_archive 'CCDC 977307'
#######################################################################
#
#                 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_z

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C120 H88 Mn5 N20 O22 S2'
_chemical_formula_weight         2500.92

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'
S S 0.1246 0.1234 '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                   12.150(3)
_cell_length_b                   13.422(3)
_cell_length_c                   17.825(4)
_cell_angle_alpha                77.205(4)
_cell_angle_beta                 70.985(4)
_cell_angle_gamma                83.344(4)
_cell_volume                     2676.8(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2984
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      26.49

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1281
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7532
_exptl_absorpt_correction_T_max  0.8283
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13563
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0720
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9187
_reflns_number_gt                5349
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1504P)²+3.1548P] 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         9187
_refine_ls_number_parameters     802
_refine_ls_number_restraints     115
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_gt           0.0690
_refine_ls_wR_factor_ref         0.1581
_refine_ls_wR_factor_gt          0.1102
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.005
_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
Mn1 Mn 0.5000 0.5000 0.5000 0.0682(2) Uani 1 2 d S . .
Mn2 Mn 0.07540(4) 0.75462(3) 0.75000(2) 0.05560(12) Uani 1 1 d . . .
Mn3 Mn 0.37884(5) 0.76159(3) 0.58420(2) 0.06627(15) Uani 1 1 d . . .
S1 S 0.24937(8) 0.57571(5) 0.64670(4) 0.0626(2) Uani 1 1 d . . .
O1 O 0.29925(19) 0.90307(13) 0.62130(10) 0.0638(6) Uani 1 1 d . . .
O1W O -0.0239(2) 0.61867(15) 0.76480(12) 0.0948(8) Uani 1 1 d . . .
H1WA H -0.0826 0.6280 0.8020 0.114 Uiso 1 1 d R . .
H1WB H -0.0364 0.6100 0.7242 0.114 Uiso 1 1 d R . .
O2 O 0.16358(18) 0.88524(14) 0.74319(10) 0.0732(6) Uani 1 1 d . . .
O3 O 0.4470(2) 1.24809(15) 0.49506(10) 0.0830(7) Uani 1 1 d . . .
O4 O 0.4210(2) 1.36332(14) 0.57295(11) 0.0920(8) Uani 1 1 d . . .
O5 O 0.08252(18) 1.19807(14) 1.15867(9) 0.0586(6) Uani 1 1 d . . .
O6 O 0.16973(16) 1.34538(14) 1.09916(10) 0.0558(6) Uani 1 1 d . . .
O7 O 0.2672(2) 0.50250(14) 0.71484(10) 0.0686(7) Uani 1 1 d . . .
O8 O 0.1565(2) 0.54934(16) 0.62086(12) 0.0913(8) Uani 1 1 d . . .
O9 O 0.22146(19) 0.68103(13) 0.66734(10) 0.0627(6) Uani 1 1 d . . .
O10 O 0.3619(2) 0.59232(13) 0.57837(10) 0.0726(7) Uani 1 1 d . . .
N1 N 0.13849(19) 0.68276(16) 0.85963(12) 0.0514(7) Uani 1 1 d . . .
N2 N 0.11341(17) 0.66355(15) 0.98920(11) 0.0411(6) Uani 1 1 d . . .
N3 N -0.0237(2) 0.8211(2) 1.53124(13) 0.07941(19) Uani 1 1 d U . .
N4 N 0.0088(2) 0.8201(2) 1.64560(13) 0.07818(19) Uani 1 1 d U . .
N5 N 0.4718(3) 0.75263(18) 0.67417(12) 0.0705(9) Uani 1 1 d . . .
N6 N 0.5123(2) 0.78194(17) 0.77962(11) 0.0556(7) Uani 1 1 d . . .
N7 N 0.3658(3) 0.88052(18) 1.33889(12) 0.0778(10) Uani 1 1 d . . .
N8 N 0.3393(3) 0.83815(19) 1.47014(13) 0.0946(12) Uani 1 1 d . . .
N9 N 0.3986(3) 0.51474(18) 0.41176(12) 0.0723(9) Uani 1 1 d . . .
N10 N 0.3796(2) 0.51529(18) 0.29255(12) 0.0597(8) Uani 1 1 d . . .
C1 C 0.1473(2) 0.5815(2) 0.89045(14) 0.0481(8) Uani 1 1 d . . .
H1 H 0.1621 0.5296 0.8609 0.058 Uiso 1 1 calc R . .
C2 C 0.1310(2) 0.5672(2) 0.97107(14) 0.0476(8) Uani 1 1 d . . .
H2 H 0.1315 0.5052 1.0067 0.057 Uiso 1 1 calc R . .
C3 C 0.1187(2) 0.7301(2) 0.91951(13) 0.0486(8) Uani 1 1 d . . .
H3 H 0.1094 0.8007 0.9147 0.058 Uiso 1 1 calc R . .
C4 C 0.0890(2) 0.68764(19) 1.06780(13) 0.0423(7) Uani 1 1 d . . .
C5 C 0.0264(2) 0.62234(19) 1.13528(13) 0.0452(7) Uani 1 1 d . . .
H5 H 0.0004 0.5625 1.1300 0.054 Uiso 1 1 calc R . .
C6 C 0.0021(2) 0.6454(2) 1.21108(14) 0.0531(8) Uani 1 1 d . . .
H6 H -0.0411 0.6012 1.2565 0.064 Uiso 1 1 calc R . .
C7 C 0.0414(2) 0.7338(2) 1.22040(14) 0.0474(8) Uani 1 1 d . . .
C8 C 0.1028(3) 0.7978(2) 1.15209(16) 0.0646(9) Uani 1 1 d . . .
H8 H 0.1289 0.8579 1.1568 0.078 Uiso 1 1 calc R . .
C9 C 0.1272(3) 0.7752(2) 1.07578(15) 0.0674(9) Uani 1 1 d . . .
H9 H 0.1694 0.8197 1.0302 0.081 Uiso 1 1 calc R . .
C11 C -0.0042(4) 0.6777(3) 1.37478(19) 0.0905(2) Uani 0.50 1 d PDU . .
H11A H -0.0192 0.6092 1.3743 0.109 Uiso 0.50 1 d PR . .
C11A C -0.10167(15) 0.75323(14) 1.44044(9) 0.0904(2) Uani 0.50 1 d PGDU . .
H11B H -0.1734 0.7370 1.4830 0.108 Uiso 0.50 1 d PR . .
C12A C -0.08577(18) 0.73286(18) 1.36437(10) 0.0903(2) Uani 0.50 1 d PGDU . .
H12A H -0.1470 0.7040 1.3542 0.108 Uiso 0.50 1 d PR . .
C10 C 0.0188(2) 0.7543(2) 1.30301(10) 0.0567(9) Uani 1 1 d G . .
C14A C 0.10740(18) 0.7960(3) 1.31772(13) 0.0622(2) Uani 0.50 1 d PGU . .
H14A H 0.1796 0.8108 1.2753 0.075 Uiso 0.50 1 d PR . .
C15A C 0.09150(19) 0.8164(3) 1.39379(14) 0.0622(2) Uani 0.50 1 d PGU . .
H15A H 0.1527 0.8453 1.4040 0.075 Uiso 0.50 1 d PR . .
C13 C -0.01303(18) 0.79502(19) 1.45515(11) 0.0789(12) Uani 1 1 d GD . .
C12 C -0.0166(4) 0.6991(3) 1.4482(2) 0.0907(2) Uani 0.50 1 d PDU . .
H12B H -0.0334 0.6427 1.4934 0.109 Uiso 0.50 1 d PR . .
C14 C 0.0020(5) 0.8932(5) 1.3830(3) 0.0621(2) Uani 0.50 1 d PU . .
H14B H 0.0003 0.9618 1.3912 0.074 Uiso 0.50 1 d PR . .
C15 C 0.0178(5) 0.8681(5) 1.3074(3) 0.0621(2) Uani 0.50 1 d PU . .
H15B H 0.0270 0.9204 1.2596 0.075 Uiso 0.50 1 d PR . .
C16 C -0.1312(3) 0.8346(4) 1.5880(2) 0.0791(2) Uani 0.50 1 d PDU . .
H16 H -0.2061 0.8425 1.5795 0.095 Uiso 0.50 1 d PR . .
C17 C -0.1089(3) 0.8355(4) 1.6613(2) 0.0787(2) Uani 0.50 1 d PRDU . .
H17 H -0.1651 0.8460 1.7115 0.094 Uiso 0.50 1 d PR . .
C16A C -0.0638(6) 0.9378(6) 1.5465(3) 0.0793(2) Uani 0.50 1 d PU . .
H16A H -0.0881 0.9965 1.5127 0.095 Uiso 0.50 1 d PR . .
C17A C -0.0505(6) 0.9271(6) 1.6238(3) 0.0788(2) Uani 0.50 1 d PU . .
H17A H -0.0747 0.9774 1.6575 0.095 Uiso 0.50 1 d PR . .
C18 C 0.0427(2) 0.7851(3) 1.57788(15) 0.0788(2) Uani 1 1 d DU . .
H18 H 0.1066 0.7398 1.5643 0.095 Uiso 1 1 calc R . .
C19 C 0.4286(3) 0.7778(2) 0.74646(14) 0.0642(10) Uani 1 1 d . . .
H19 H 0.3497 0.7910 0.7713 0.077 Uiso 1 1 calc R . .
C20 C 0.5896(4) 0.7398(2) 0.66301(16) 0.0826(13) Uani 1 1 d . . .
H20 H 0.6441 0.7217 0.6171 0.099 Uiso 1 1 calc R . .
C21 C 0.6162(3) 0.7563(2) 0.72576(16) 0.0688(11) Uani 1 1 d . . .
H21 H 0.6899 0.7515 0.7320 0.083 Uiso 1 1 calc R . .
C22 C 0.4936(2) 0.8059(2) 0.85743(14) 0.0474(8) Uani 1 1 d . . .
C23 C 0.5623(2) 0.7545(2) 0.90367(15) 0.0509(9) Uani 1 1 d . . .
H23 H 0.6218 0.7080 0.8838 0.061 Uiso 1 1 calc R . .
C24 C 0.5401(2) 0.7742(2) 0.97963(15) 0.0542(8) Uani 1 1 d . . .
H24 H 0.5865 0.7403 1.0107 0.065 Uiso 1 1 calc R . .
C25 C 0.4514(2) 0.8424(2) 1.01252(13) 0.0447(7) Uani 1 1 d . . .
C26 C 0.3894(2) 0.8972(2) 0.96234(14) 0.0492(8) Uani 1 1 d . . .
H26 H 0.3335 0.9473 0.9806 0.059 Uiso 1 1 calc R . .
C27 C 0.4096(2) 0.8785(2) 0.88505(14) 0.0534(9) Uani 1 1 d . . .
H27 H 0.3665 0.9149 0.8524 0.064 Uiso 1 1 calc R . .
C28 C 0.4264(2) 0.8540(2) 1.09719(13) 0.0468(8) Uani 1 1 d . . .
C29 C 0.4562(3) 0.7763(2) 1.15205(16) 0.0721(11) Uani 1 1 d . . .
H29 H 0.4889 0.7151 1.1362 0.086 Uiso 1 1 calc R . .
C30 C 0.4385(3) 0.7867(2) 1.23096(16) 0.0835(12) Uani 1 1 d . . .
H30 H 0.4647 0.7345 1.2660 0.100 Uiso 1 1 calc R . .
C31 C 0.3846(3) 0.8707(2) 1.25730(15) 0.0675(10) Uani 1 1 d . . .
C32 C 0.3507(3) 0.9522(2) 1.20369(14) 0.0573(9) Uani 1 1 d . . .
H32 H 0.3148 1.0116 1.2211 0.069 Uiso 1 1 calc R . .
C33 C 0.3716(2) 0.9427(2) 1.12447(14) 0.0534(9) Uani 1 1 d . . .
H33 H 0.3488 0.9962 1.0887 0.064 Uiso 1 1 calc R . .
C34 C 0.3619(4) 0.9688(2) 1.36553(17) 0.0904(14) Uani 1 1 d . . .
H34 H 0.3693 1.0348 1.3347 0.108 Uiso 1 1 calc R . .
C35 C 0.3452(4) 0.9410(2) 1.44563(18) 0.1002(15) Uani 1 1 d . . .
H35 H 0.3386 0.9863 1.4797 0.120 Uiso 1 1 calc R . .
C36 C 0.3534(4) 0.8035(3) 1.40398(17) 0.1009(15) Uani 1 1 d . . .
H36 H 0.3548 0.7346 1.4022 0.121 Uiso 1 1 calc R . .
C37 C 0.2839(4) 0.5155(3) 0.41834(18) 0.0931(15) Uani 1 1 d . . .
H37 H 0.2228 0.5155 0.4661 0.112 Uiso 1 1 calc R . .
C38 C 0.2714(4) 0.5165(3) 0.34620(19) 0.0908(15) Uani 1 1 d . . .
H38 H 0.2015 0.5177 0.3352 0.109 Uiso 1 1 calc R . .
C39 C 0.4552(3) 0.5140(2) 0.33447(14) 0.0620(9) Uani 1 1 d . . .
H39 H 0.5359 0.5128 0.3120 0.074 Uiso 1 1 calc R . .
C40 C 0.4149(2) 0.5101(2) 0.20904(14) 0.0504(8) Uani 1 1 d . . .
C41 C 0.5265(2) 0.4812(2) 0.16902(15) 0.0556(9) Uani 1 1 d . . .
H41 H 0.5813 0.4634 0.1966 0.067 Uiso 1 1 calc R . .
C42 C 0.5582(2) 0.4783(2) 0.08755(14) 0.0530(8) Uani 1 1 d . . .
H42 H 0.6347 0.4588 0.0614 0.064 Uiso 1 1 calc R . .
C43 C 0.4818(2) 0.5028(2) 0.04430(13) 0.0445(8) Uani 1 1 d . . .
C44 C 0.3706(3) 0.5303(3) 0.08511(16) 0.0804(12) Uani 1 1 d . . .
H44 H 0.3164 0.5477 0.0570 0.096 Uiso 1 1 calc R . .
C45 C 0.3348(3) 0.5334(3) 0.16685(16) 0.0799(12) Uani 1 1 d . . .
H45 H 0.2576 0.5509 0.1931 0.096 Uiso 1 1 calc R . .
C46 C 0.2403(2) 0.93426(18) 0.68454(13) 0.0483(8) Uani 1 1 d . . .
C47 C 0.2635(2) 1.03778(17) 0.69267(12) 0.0350(6) Uani 1 1 d . . .
C48 C 0.2247(2) 1.06519(17) 0.76865(12) 0.0390(7) Uani 1 1 d . . .
H48 H 0.1817 1.0197 0.8131 0.047 Uiso 1 1 calc R . .
C49 C 0.2493(2) 1.15929(17) 0.77920(12) 0.0384(7) Uani 1 1 d . . .
C50 C 0.3046(3) 1.22816(18) 0.71058(13) 0.0534(8) Uani 1 1 d . . .
H50 H 0.3171 1.2931 0.7155 0.064 Uiso 1 1 calc R . .
C51 C 0.3419(3) 1.20275(18) 0.63421(13) 0.0495(8) Uani 1 1 d . . .
C52 C 0.3251(2) 1.10596(17) 0.62589(13) 0.0396(7) Uani 1 1 d . . .
H52 H 0.3550 1.0870 0.5757 0.048 Uiso 1 1 calc R . .
C53 C 0.4078(3) 1.2778(2) 0.56227(14) 0.0712(10) Uani 1 1 d . . .
C54 C 0.2178(2) 1.18342(17) 0.86155(12) 0.0377(7) Uani 1 1 d . . .
C55 C 0.1700(3) 1.11331(19) 0.93113(14) 0.0533(9) Uani 1 1 d . . .
H55 H 0.1543 1.0489 0.9270 0.064 Uiso 1 1 calc R . .
C56 C 0.1448(3) 1.1367(2) 1.00772(14) 0.0544(9) Uani 1 1 d . . .
H56 H 0.1116 1.0881 1.0535 0.065 Uiso 1 1 calc R . .
C57 C 0.1682(2) 1.23056(19) 1.01666(13) 0.0425(7) Uani 1 1 d . . .
C58 C 0.2158(2) 1.30191(18) 0.94666(13) 0.0436(7) Uani 1 1 d . . .
H58 H 0.2325 1.3658 0.9512 0.052 Uiso 1 1 calc R . .
C59 C 0.2390(2) 1.28033(17) 0.87084(13) 0.0415(7) Uani 1 1 d . . .
H59 H 0.2689 1.3303 0.8252 0.050 Uiso 1 1 calc R . .
C60 C 0.1369(2) 1.26057(19) 1.09849(13) 0.0441(7) Uani 1 1 d . . .


_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 O4 2.1251(18) 2_676 ?
Mn1 O4 2.1251(18) 1_545 ?
Mn1 O10 2.2490(19) 2_666 ?
Mn1 O10 2.2490(19) . ?
Mn1 N9 2.258(3) 2_666 ?
Mn1 N9 2.258(3) . ?
Mn2 O2 2.120(2) . ?
Mn2 O9 2.1977(18) . ?
Mn2 O5 2.2079(18) 2_577 ?
Mn2 O1W 2.223(2) . ?
Mn2 N4 2.232(3) 1_554 ?
Mn2 N1 2.304(2) . ?
Mn3 O3 2.135(2) 2_676 ?
Mn3 O1 2.1661(18) . ?
Mn3 N5 2.220(3) . ?
Mn3 O9 2.2236(19) . ?
Mn3 N8 2.240(3) 1_554 ?
Mn3 O10 2.3326(19) . ?
S1 O7 1.443(2) . ?
S1 O8 1.454(3) . ?
S1 O10 1.506(2) . ?
S1 O9 1.5120(19) . ?
O1 C46 1.254(3) . ?
O1W H1WA 0.8200 . ?
O1W H1WB 0.8201 . ?
O2 C46 1.264(3) . ?
O3 C53 1.271(3) . ?
O3 Mn3 2.135(2) 2_676 ?
O4 C53 1.241(4) . ?
O4 Mn1 2.1251(18) 1_565 ?
O5 C60 1.248(3) . ?
O5 Mn2 2.2079(18) 2_577 ?
O6 C60 1.253(3) . ?
N1 C3 1.303(3) . ?
N1 C1 1.355(3) . ?
N2 C3 1.347(3) . ?
N2 C2 1.377(3) . ?
N2 C4 1.436(3) . ?
N3 C18 1.320(4) . ?
N3 C16 1.389(4) . ?
N3 C13 1.437(3) . ?
N3 C16A 1.641(8) . ?
N4 C18 1.315(4) . ?
N4 C17 1.365(4) . ?
N4 C17A 1.558(8) . ?
N4 Mn2 2.232(3) 1_556 ?
N5 C19 1.327(3) . ?
N5 C20 1.375(5) . ?
N6 C19 1.344(4) . ?
N6 C21 1.375(4) . ?
N6 C22 1.433(3) . ?
N7 C36 1.352(4) . ?
N7 C34 1.362(4) . ?
N7 C31 1.430(4) . ?
N8 C36 1.315(4) . ?
N8 C35 1.355(4) . ?
N8 Mn3 2.240(3) 1_556 ?
N9 C39 1.326(3) . ?
N9 C37 1.358(5) . ?
N10 C38 1.351(4) . ?
N10 C39 1.357(4) . ?
N10 C40 1.424(3) . ?
C1 C2 1.357(4) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C9 1.364(4) . ?
C4 C5 1.373(3) . ?
C5 C6 1.383(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.390(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.367(3) . ?
C7 C10 1.489(3) . ?
C8 C9 1.389(4) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C11 C12 1.358(5) . ?
C11 C10 1.422(4) . ?
C10 C15 1.545(7) . ?
C13 C12 1.328(4) . ?
C13 C14 1.606(6) . ?
C14 C15 1.409(8) . ?
C16 C17 1.4200 . ?
C16 H16 0.9600 . ?
C17 H17 0.9601 . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.329(5) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C27 1.374(4) . ?
C22 C23 1.384(4) . ?
C23 C24 1.371(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.393(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.389(4) . ?
C25 C28 1.479(3) . ?
C26 C27 1.393(4) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.366(4) . ?
C28 C33 1.399(4) . ?
C29 C30 1.389(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.336(4) . ?
C30 H30 0.9300 . ?
C31 C32 1.402(4) . ?
C32 C33 1.383(4) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 C35 1.346(4) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 C38 1.340(5) . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C40 C41 1.367(4) . ?
C40 C45 1.383(5) . ?
C41 C42 1.384(4) . ?
C41 H41 0.9300 . ?
C42 C43 1.360(4) . ?
C42 H42 0.9300 . ?
C43 C44 1.362(4) . ?
C43 C43 1.512(5) 2_665 ?
C44 C45 1.387(4) . ?
C44 H44 0.9300 . ?
C45 H45 0.9300 . ?
C46 C47 1.496(3) . ?
C47 C52 1.382(3) . ?
C47 C48 1.399(3) . ?
C48 C49 1.396(3) . ?
C48 H48 0.9300 . ?
C49 C50 1.382(3) . ?
C49 C54 1.490(3) . ?
C50 C51 1.394(3) . ?
C50 H50 0.9300 . ?
C51 C52 1.385(4) . ?
C51 C53 1.498(3) . ?
C52 H52 0.9300 . ?
C54 C55 1.379(3) . ?
C54 C59 1.409(4) . ?
C55 C56 1.397(4) . ?
C55 H55 0.9300 . ?
C56 C57 1.376(4) . ?
C56 H56 0.9300 . ?
C57 C58 1.392(3) . ?
C57 C60 1.516(3) . ?
C58 C59 1.377(3) . ?
C58 H58 0.9300 . ?
C59 H59 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Mn1 O4 180.000(1) 2_676 1_545 ?
O4 Mn1 O10 89.83(7) 2_676 2_666 ?
O4 Mn1 O10 90.17(7) 1_545 2_666 ?
O4 Mn1 O10 90.17(7) 2_676 . ?
O4 Mn1 O10 89.83(7) 1_545 . ?
O10 Mn1 O10 180.000(1) 2_666 . ?
O4 Mn1 N9 93.82(9) 2_676 2_666 ?
O4 Mn1 N9 86.18(9) 1_545 2_666 ?
O10 Mn1 N9 91.95(9) 2_666 2_666 ?
O10 Mn1 N9 88.05(9) . 2_666 ?
O4 Mn1 N9 86.18(9) 2_676 . ?
O4 Mn1 N9 93.82(9) 1_545 . ?
O10 Mn1 N9 88.05(9) 2_666 . ?
O10 Mn1 N9 91.95(9) . . ?
N9 Mn1 N9 180.000(1) 2_666 . ?
O2 Mn2 O9 96.70(8) . . ?
O2 Mn2 O5 92.35(7) . 2_577 ?
O9 Mn2 O5 170.18(7) . 2_577 ?
O2 Mn2 O1W 176.46(7) . . ?
O9 Mn2 O1W 86.42(8) . . ?
O5 Mn2 O1W 84.43(8) 2_577 . ?
O2 Mn2 N4 96.32(10) . 1_554 ?
O9 Mn2 N4 88.32(9) . 1_554 ?
O5 Mn2 N4 94.48(8) 2_577 1_554 ?
O1W Mn2 N4 85.42(10) . 1_554 ?
O2 Mn2 N1 85.71(8) . . ?
O9 Mn2 N1 92.30(8) . . ?
O5 Mn2 N1 84.57(7) 2_577 . ?
O1W Mn2 N1 92.51(9) . . ?
N4 Mn2 N1 177.80(9) 1_554 . ?
O3 Mn3 O1 122.12(8) 2_676 . ?
O3 Mn3 N5 81.87(9) 2_676 . ?
O1 Mn3 N5 85.27(9) . . ?
O3 Mn3 O9 148.26(7) 2_676 . ?
O1 Mn3 O9 89.26(7) . . ?
N5 Mn3 O9 97.51(8) . . ?
O3 Mn3 N8 83.53(10) 2_676 1_554 ?
O1 Mn3 N8 81.91(9) . 1_554 ?
N5 Mn3 N8 151.42(11) . 1_554 ?
O9 Mn3 N8 107.71(11) . 1_554 ?
O3 Mn3 O10 87.81(8) 2_676 . ?
O1 Mn3 O10 149.71(8) . . ?
N5 Mn3 O10 105.34(9) . . ?
O9 Mn3 O10 61.57(7) . . ?
N8 Mn3 O10 98.49(9) 1_554 . ?
O7 S1 O8 112.71(13) . . ?
O7 S1 O10 110.82(13) . . ?
O8 S1 O10 112.31(13) . . ?
O7 S1 O9 110.10(11) . . ?
O8 S1 O9 108.99(13) . . ?
O10 S1 O9 101.30(10) . . ?
C46 O1 Mn3 139.14(15) . . ?
Mn2 O1W H1WA 101.4 . . ?
Mn2 O1W H1WB 116.4 . . ?
H1WA O1W H1WB 114.6 . . ?
C46 O2 Mn2 130.09(17) . . ?
C53 O3 Mn3 130.5(2) . 2_676 ?
C53 O4 Mn1 136.51(16) . 1_565 ?
C60 O5 Mn2 121.64(16) . 2_577 ?
S1 O9 Mn2 135.66(11) . . ?
S1 O9 Mn3 100.67(9) . . ?
Mn2 O9 Mn3 123.66(8) . . ?
S1 O10 Mn1 138.66(11) . . ?
S1 O10 Mn3 96.26(9) . . ?
Mn1 O10 Mn3 124.50(9) . . ?
C3 N1 C1 106.7(2) . . ?
C3 N1 Mn2 120.72(17) . . ?
C1 N1 Mn2 125.97(19) . . ?
C3 N2 C2 106.5(2) . . ?
C3 N2 C4 126.9(2) . . ?
C2 N2 C4 126.52(19) . . ?
C18 N3 C16 101.7(2) . . ?
C18 N3 C13 126.8(3) . . ?
C16 N3 C13 122.2(3) . . ?
C18 N4 C17 103.6(3) . . ?
C18 N4 Mn2 123.3(2) . 1_556 ?
C17 N4 Mn2 117.7(2) . 1_556 ?
C17A N4 Mn2 129.9(3) . 1_556 ?
C19 N5 C20 103.6(3) . . ?
C19 N5 Mn3 126.9(2) . . ?
C20 N5 Mn3 128.38(18) . . ?
C19 N6 C21 106.8(2) . . ?
C19 N6 C22 125.5(2) . . ?
C21 N6 C22 127.7(3) . . ?
C36 N7 C34 106.6(3) . . ?
C36 N7 C31 126.6(3) . . ?
C34 N7 C31 126.7(2) . . ?
C36 N8 C35 104.9(2) . . ?
C36 N8 Mn3 130.1(2) . 1_556 ?
C35 N8 Mn3 119.7(3) . 1_556 ?
C39 N9 C37 105.1(3) . . ?
C39 N9 Mn1 119.6(2) . . ?
C37 N9 Mn1 134.99(18) . . ?
C38 N10 C39 106.6(3) . . ?
C38 N10 C40 129.6(3) . . ?
C39 N10 C40 123.7(2) . . ?
N1 C1 C2 109.6(2) . . ?
N1 C1 H1 125.2 . . ?
C2 C1 H1 125.2 . . ?
C1 C2 N2 105.9(2) . . ?
C1 C2 H2 127.1 . . ?
N2 C2 H2 127.1 . . ?
N1 C3 N2 111.3(2) . . ?
N1 C3 H3 124.3 . . ?
N2 C3 H3 124.3 . . ?
C9 C4 C5 119.8(2) . . ?
C9 C4 N2 120.4(2) . . ?
C5 C4 N2 119.8(2) . . ?
C4 C5 C6 120.0(3) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C7 120.9(2) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C8 C7 C6 117.7(2) . . ?
C8 C7 C10 122.5(3) . . ?
C6 C7 C10 119.7(2) . . ?
C7 C8 C9 121.6(3) . . ?
C7 C8 H8 119.2 . . ?
C9 C8 H8 119.2 . . ?
C4 C9 C8 119.9(2) . . ?
C4 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C12A C11 C12 94.8(3) . . ?
C12A C11 C10 63.2(2) . . ?
C12 C11 C10 122.2(3) . . ?
C11 C10 C7 124.4(3) . . ?
C11 C10 C15 120.4(3) . . ?
C7 C10 C15 115.1(3) . . ?
C12 C13 N3 121.8(3) . . ?
C12 C13 C14 125.5(3) . . ?
N3 C13 C14 112.7(3) . . ?
C13 C12 C11 119.9(3) . . ?
C15 C14 C13 113.1(5) . . ?
N3 C16 C17 106.6(2) . . ?
N3 C16 H16 126.9 . . ?
C17 C16 H16 126.5 . . ?
N4 C17 C16 106.13(19) . . ?
N4 C17 H17 126.9 . . ?
C16 C17 H17 126.9 . . ?
N4 C18 N3 112.9(3) . . ?
N4 C18 H18 123.6 . . ?
N3 C18 H18 123.6 . . ?
N5 C19 N6 112.0(3) . . ?
N5 C19 H19 124.0 . . ?
N6 C19 H19 124.0 . . ?
C21 C20 N5 111.9(3) . . ?
C21 C20 H20 124.1 . . ?
N5 C20 H20 124.1 . . ?
C20 C21 N6 105.7(3) . . ?
C20 C21 H21 127.1 . . ?
N6 C21 H21 127.1 . . ?
C27 C22 C23 121.0(2) . . ?
C27 C22 N6 120.6(2) . . ?
C23 C22 N6 118.4(2) . . ?
C24 C23 C22 118.1(2) . . ?
C24 C23 H23 121.0 . . ?
C22 C23 H23 121.0 . . ?
C23 C24 C25 123.2(3) . . ?
C23 C24 H24 118.4 . . ?
C25 C24 H24 118.4 . . ?
C26 C25 C24 116.8(2) . . ?
C26 C25 C28 122.8(2) . . ?
C24 C25 C28 120.4(2) . . ?
C25 C26 C27 121.0(2) . . ?
C25 C26 H26 119.5 . . ?
C27 C26 H26 119.5 . . ?
C22 C27 C26 119.5(3) . . ?
C22 C27 H27 120.2 . . ?
C26 C27 H27 120.2 . . ?
C29 C28 C33 117.6(2) . . ?
C29 C28 C25 120.1(2) . . ?
C33 C28 C25 122.3(2) . . ?
C28 C29 C30 121.3(3) . . ?
C28 C29 H29 119.3 . . ?
C30 C29 H29 119.3 . . ?
C31 C30 C29 120.9(3) . . ?
C31 C30 H30 119.5 . . ?
C29 C30 H30 119.5 . . ?
C30 C31 C32 119.9(3) . . ?
C30 C31 N7 120.6(3) . . ?
C32 C31 N7 119.5(3) . . ?
C33 C32 C31 119.0(3) . . ?
C33 C32 H32 120.5 . . ?
C31 C32 H32 120.5 . . ?
C32 C33 C28 121.2(2) . . ?
C32 C33 H33 119.4 . . ?
C28 C33 H33 119.4 . . ?
C35 C34 N7 105.9(3) . . ?
C35 C34 H34 127.1 . . ?
N7 C34 H34 127.1 . . ?
C34 C35 N8 111.0(3) . . ?
C34 C35 H35 124.5 . . ?
N8 C35 H35 124.5 . . ?
N8 C36 N7 111.5(3) . . ?
N8 C36 H36 124.2 . . ?
N7 C36 H36 124.2 . . ?
C38 C37 N9 110.4(3) . . ?
C38 C37 H37 124.8 . . ?
N9 C37 H37 124.8 . . ?
C37 C38 N10 107.0(4) . . ?
C37 C38 H38 126.5 . . ?
N10 C38 H38 126.5 . . ?
N9 C39 N10 110.9(3) . . ?
N9 C39 H39 124.6 . . ?
N10 C39 H39 124.6 . . ?
C41 C40 C45 118.5(2) . . ?
C41 C40 N10 121.7(3) . . ?
C45 C40 N10 119.8(2) . . ?
C40 C41 C42 120.1(3) . . ?
C40 C41 H41 119.9 . . ?
C42 C41 H41 119.9 . . ?
C43 C42 C41 122.5(2) . . ?
C43 C42 H42 118.7 . . ?
C41 C42 H42 118.7 . . ?
C42 C43 C44 116.8(2) . . ?
C42 C43 C43 121.4(3) . 2_665 ?
C44 C43 C43 121.8(3) . 2_665 ?
C43 C44 C45 122.6(3) . . ?
C43 C44 H44 118.7 . . ?
C45 C44 H44 118.7 . . ?
C40 C45 C44 119.4(3) . . ?
C40 C45 H45 120.3 . . ?
C44 C45 H45 120.3 . . ?
O1 C46 O2 125.8(2) . . ?
O1 C46 C47 117.7(2) . . ?
O2 C46 C47 116.5(2) . . ?
C52 C47 C48 119.6(2) . . ?
C52 C47 C46 120.5(2) . . ?
C48 C47 C46 119.86(18) . . ?
C49 C48 C47 121.49(19) . . ?
C49 C48 H48 119.3 . . ?
C47 C48 H48 119.3 . . ?
C50 C49 C48 117.4(2) . . ?
C50 C49 C54 121.7(2) . . ?
C48 C49 C54 120.92(18) . . ?
C49 C50 C51 121.7(2) . . ?
C49 C50 H50 119.2 . . ?
C51 C50 H50 119.2 . . ?
C52 C51 C50 119.9(2) . . ?
C52 C51 C53 120.2(2) . . ?
C50 C51 C53 119.7(2) . . ?
C47 C52 C51 119.6(2) . . ?
C47 C52 H52 120.2 . . ?
C51 C52 H52 120.2 . . ?
O4 C53 O3 125.1(2) . . ?
O4 C53 C51 117.7(2) . . ?
O3 C53 C51 117.2(2) . . ?
C55 C54 C59 117.2(2) . . ?
C55 C54 C49 122.7(2) . . ?
C59 C54 C49 120.14(18) . . ?
C54 C55 C56 121.5(2) . . ?
C54 C55 H55 119.2 . . ?
C56 C55 H55 119.2 . . ?
C57 C56 C55 121.1(2) . . ?
C57 C56 H56 119.4 . . ?
C55 C56 H56 119.4 . . ?
C56 C57 C58 117.6(2) . . ?
C56 C57 C60 122.7(2) . . ?
C58 C57 C60 119.6(2) . . ?
C59 C58 C57 121.7(2) . . ?
C59 C58 H58 119.1 . . ?
C57 C58 H58 119.1 . . ?
C58 C59 C54 120.76(19) . . ?
C58 C59 H59 119.6 . . ?
C54 C59 H59 119.6 . . ?
O5 C60 O6 126.3(2) . . ?
O5 C60 C57 117.1(2) . . ?
O6 C60 C57 116.57(19) . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         1.457
_refine_diff_density_min         -1.098
_refine_diff_density_rms         0.104
_database_code_depnum_ccdc_archive 'CCDC 977308'
