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

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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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
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# 
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#  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.
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data_z



_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

 ?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            
'C32 H24 Mn N2 O10'

_chemical_formula_weight         651.47



loop_

_atom_type_symbol

_atom_type_description

_atom_type_scat_dispersion_real

_atom_type_scat_dispersion_imag

_atom_type_scat_source










C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



_symmetry_cell_setting           Triclinic

_symmetry_space_group_name_H-M   P-1



loop_

_symmetry_equiv_pos_as_xyz


'x, y, z'
'-x, -y, -z'



_cell_length_a                   10.454(5)

_cell_length_b                   10.739(5)

_cell_length_c                   13.686(7)

_cell_angle_alpha                99.384(6)

_cell_angle_beta                 99.642(6)

_cell_angle_gamma                94.786(6)

_cell_volume                     1484.8(12)

_cell_formula_units_Z            2

_cell_measurement_temperature    296(2)

_cell_measurement_reflns_used    3678

_cell_measurement_theta_min      1.9

_cell_measurement_theta_max      27.5



_exptl_crystal_description       prism

_exptl_crystal_colour            pink

_exptl_crystal_size_max          0.25

_exptl_crystal_size_mid          0.24

_exptl_crystal_size_min          0.22

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.457

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             670

_exptl_absorpt_coefficient_mu    0.507

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.8836

_exptl_absorpt_correction_T_max  0.8966

_exptl_absorpt_process_details   SADABS



_exptl_special_details           
;

 ?

;



_diffrn_ambient_temperature      296(2)

_diffrn_radiation_wavelength     0.71073

_diffrn_radiation_type           MoK\a

_diffrn_radiation_source         'fine-focus sealed tube'

_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker P4'

_diffrn_measurement_method       'ω scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            15990

_diffrn_reflns_av_R_equivalents  0.0500

_diffrn_reflns_av_unetI/netI     0.0516

_diffrn_reflns_limit_h_min       -13

_diffrn_reflns_limit_h_max       13

_diffrn_reflns_limit_k_min       -13

_diffrn_reflns_limit_k_max       13

_diffrn_reflns_limit_l_min       -17

_diffrn_reflns_limit_l_max       17

_diffrn_reflns_theta_min         1.53

_diffrn_reflns_theta_max         27.52

_reflns_number_total             6797

_reflns_number_gt                5414

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'Bruker XSCANS'

_computing_cell_refinement       'Bruker XSCANS'

_computing_data_reduction        'Bruker SHELXTL'

_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)+(0.0709P)²+0.1715P] 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         6797

_refine_ls_number_parameters     418

_refine_ls_number_restraints     8

_refine_ls_R_factor_all          0.0637

_refine_ls_R_factor_gt           0.0473

_refine_ls_wR_factor_ref         0.1435

_refine_ls_wR_factor_gt          0.1263

_refine_ls_goodness_of_fit_ref   1.080

_refine_ls_restrained_S_all      1.085

_refine_ls_shift/su_max          0.000

_refine_ls_shift/su_mean         0.000



loop_

_atom_site_label

_atom_site_type_symbol

_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z

_atom_site_U_iso_or_equiv

_atom_site_adp_type

_atom_site_occupancy

_atom_site_symmetry_multiplicity

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_assembly

_atom_site_disorder_group





































































Mn1 Mn 0.53783(3) 0.43247(3) 0.17973(2) 0.03639(12) Uani 1 1 d . . .
O1 O 0.4500(2) 0.26850(16) 0.07628(14) 0.0561(5) Uani 1 1 d . . .
O2 O 0.45597(19) 0.20250(16) -0.08319(14) 0.0537(5) Uani 1 1 d . . .
O3 O 0.3146(2) 0.0607(2) -0.22084(14) 0.0657(6) Uani 1 1 d D . .
H3A H 0.367(3) 0.111(3) -0.170(2) 0.099 Uiso 1 1 d D . .
O4 O 0.14825(18) -0.08480(18) -0.24399(12) 0.0494(4) Uani 1 1 d . . .
O5 O -0.30238(15) -0.51582(16) 0.11180(13) 0.0446(4) Uani 1 1 d . . .
O6 O -0.13476(17) -0.59041(18) 0.19846(16) 0.0578(5) Uani 1 1 d . . .
O7 O 0.13658(19) -0.0852(2) 0.56616(13) 0.0593(5) Uani 1 1 d D . .
H7A H 0.139(4) -0.095(3) 0.6268(16) 0.089 Uiso 1 1 d D . .
O8 O 0.3321(2) -0.1559(2) 0.58378(13) 0.0612(5) Uani 1 1 d . . .
O9 O 0.42520(16) 0.55557(16) 0.09159(13) 0.0418(4) Uani 1 1 d D . .
H9A H 0.461(3) 0.6285(18) 0.095(2) 0.063 Uiso 1 1 d D . .
H9B H 0.379(3) 0.528(2) 0.0328(15) 0.063 Uiso 1 1 d D . .
O10 O 0.66060(19) 0.3167(2) 0.26704(18) 0.0740(7) Uani 1 1 d D . .
H10B H 0.6594 0.2578 0.3063 0.111 Uiso 1 1 d RD . .
H10A H 0.7385 0.3417 0.2524 0.111 Uiso 1 1 d RD . .
N1 N 0.3771(2) 0.42305(19) 0.27431(15) 0.0448(5) Uani 1 1 d . . .
N2 N 0.5887(2) 0.5976(2) 0.31285(17) 0.0534(5) Uani 1 1 d . . .
C1 C 0.4220(2) 0.1875(2) -0.00158(18) 0.0372(5) Uani 1 1 d . . .
C2 C 0.3384(2) 0.06685(18) 0.00500(16) 0.0312(4) Uani 1 1 d . . .
C3 C 0.2552(2) -0.01686(19) -0.07517(15) 0.0312(4) Uani 1 1 d . . .
C4 C 0.2369(2) -0.0137(2) -0.18635(16) 0.0380(5) Uani 1 1 d . . .
C5 C 0.1758(2) -0.11520(19) -0.05195(15) 0.0324(4) Uani 1 1 d . . .
H5 H 0.1215 -0.1710 -0.1045 0.039 Uiso 1 1 calc R . .
C6 C 0.1744(2) -0.13331(19) 0.04592(15) 0.0306(4) Uani 1 1 d . . .
C7 C 0.2577(2) -0.05128(19) 0.12543(15) 0.0312(4) Uani 1 1 d . . .
C8 C 0.3393(2) 0.0452(2) 0.10263(16) 0.0333(4) Uani 1 1 d . . .
H8 H 0.3971 0.0976 0.1552 0.040 Uiso 1 1 calc R . .
C9 C 0.0844(2) -0.23879(19) 0.06409(15) 0.0313(4) Uani 1 1 d . . .
C10 C -0.0490(2) -0.2468(2) 0.02812(18) 0.0398(5) Uani 1 1 d . . .
H10 H -0.0811 -0.1901 -0.0120 0.048 Uiso 1 1 calc R . .
C11 C -0.1348(2) -0.3384(2) 0.05140(18) 0.0416(5) Uani 1 1 d . . .
H11 H -0.2240 -0.3415 0.0281 0.050 Uiso 1 1 calc R . .
C12 C -0.0883(2) -0.4256(2) 0.10936(16) 0.0339(4) Uani 1 1 d . . .
C13 C 0.0452(2) -0.4217(2) 0.14083(18) 0.0387(5) Uani 1 1 d . . .
H13 H 0.0778 -0.4817 0.1772 0.046 Uiso 1 1 calc R . .
C14 C 0.1307(2) -0.3291(2) 0.11857(17) 0.0370(5) Uani 1 1 d . . .
H14 H 0.2201 -0.3275 0.1404 0.044 Uiso 1 1 calc R . .
C15 C -0.1802(2) -0.5190(2) 0.14192(18) 0.0385(5) Uani 1 1 d . . .
C16 C 0.2563(2) -0.0603(2) 0.23285(15) 0.0322(4) Uani 1 1 d . . .
C17 C 0.1404(2) -0.0538(2) 0.26983(16) 0.0411(5) Uani 1 1 d . . .
H17 H 0.0652 -0.0395 0.2282 0.049 Uiso 1 1 calc R . .
C18 C 0.1359(2) -0.0684(2) 0.36801(16) 0.0415(5) Uani 1 1 d . . .
H18 H 0.0581 -0.0631 0.3921 0.050 Uiso 1 1 calc R . .
C19 C 0.2468(2) -0.0909(2) 0.43012(15) 0.0370(5) Uani 1 1 d . . .
C20 C 0.3634(2) -0.0926(2) 0.39467(16) 0.0409(5) Uani 1 1 d . . .
H20 H 0.4390 -0.1050 0.4368 0.049 Uiso 1 1 calc R . .
C21 C 0.3685(2) -0.0759(2) 0.29726(17) 0.0403(5) Uani 1 1 d . . .
H21 H 0.4478 -0.0751 0.2749 0.048 Uiso 1 1 calc R . .
C22 C 0.2438(3) -0.1142(2) 0.53438(16) 0.0413(5) Uani 1 1 d . . .
C23 C 0.2668(3) 0.3428(3) 0.2472(2) 0.0540(6) Uani 1 1 d . . .
H23 H 0.2604 0.2779 0.1920 0.065 Uiso 1 1 calc R . .
C24 C 0.1623(3) 0.3510(3) 0.2963(3) 0.0660(8) Uani 1 1 d . . .
H24 H 0.0882 0.2922 0.2761 0.079 Uiso 1 1 calc R . .
C25 C 0.1714(4) 0.4486(4) 0.3760(3) 0.0812(11) Uani 1 1 d . . .
H25 H 0.1017 0.4582 0.4098 0.097 Uiso 1 1 calc R . .
C26 C 0.2828(4) 0.5321(3) 0.4060(3) 0.0727(9) Uani 1 1 d . . .
H26 H 0.2895 0.5981 0.4604 0.087 Uiso 1 1 calc R . .
C27 C 0.3861(3) 0.5171(2) 0.35405(19) 0.0503(6) Uani 1 1 d . . .
C28 C 0.5112(3) 0.6017(2) 0.38237(19) 0.0524(7) Uani 1 1 d . . .
C29 C 0.5478(4) 0.6814(3) 0.4757(2) 0.0664(9) Uani 1 1 d . . .
H29 H 0.4943 0.6814 0.5236 0.080 Uiso 1 1 calc R . .
C30 C 0.6627(4) 0.7598(3) 0.4968(3) 0.0783(11) Uani 1 1 d . . .
H30 H 0.6879 0.8136 0.5588 0.094 Uiso 1 1 calc R . .
C31 C 0.7402(4) 0.7578(3) 0.4250(3) 0.0828(11) Uani 1 1 d . . .
H31 H 0.8182 0.8111 0.4371 0.099 Uiso 1 1 calc R . .
C32 C 0.6998(4) 0.6744(3) 0.3338(3) 0.0702(9) Uani 1 1 d . . .
H32 H 0.7528 0.6724 0.2855 0.084 Uiso 1 1 calc R . .






_geom_special_details            
;

 All esds (except the esd in the dihedral angle between two l.s. planes)

 are estimated using the full covariance matrix.  The cell esds are taken

 into account individually in the estimation of esds in distances, angles

 and torsion angles; correlations between esds in cell parameters are only

 used when they are defined by crystal symmetry.  An approximate (isotropic)

 treatment of cell esds is used for estimating esds involving l.s. planes.

;



loop_

_geom_bond_atom_site_label_1

_geom_bond_atom_site_label_2

_geom_bond_distance

_geom_bond_site_symmetry_2

_geom_bond_publ_flag












































































Mn1 O1 2.1047(18) . ?
Mn1 O5 2.1206(17) 1_665 ?
Mn1 O10 2.204(2) . ?
Mn1 O9 2.2120(17) . ?
Mn1 N2 2.283(2) . ?
Mn1 N1 2.292(2) . ?
O1 C1 1.236(3) . ?
O2 C1 1.258(3) . ?
O3 C4 1.290(3) . ?
O3 H3A 0.881(18) . ?
O4 C4 1.227(3) . ?
O5 C15 1.280(3) . ?
O5 Mn1 2.1206(17) 1_445 ?
O6 C15 1.242(3) . ?
O7 C22 1.311(3) . ?
O7 H7A 0.851(18) . ?
O8 C22 1.212(3) . ?
O9 H9A 0.833(16) . ?
O9 H9B 0.860(16) . ?
O10 H10B 0.8950 . ?
O10 H10A 0.9003 . ?
N1 C23 1.341(3) . ?
N1 C27 1.346(3) . ?
N2 C32 1.328(4) . ?
N2 C28 1.347(4) . ?
C1 C2 1.525(3) . ?
C2 C8 1.392(3) . ?
C2 C3 1.413(3) . ?
C3 C5 1.399(3) . ?
C3 C4 1.508(3) . ?
C5 C6 1.387(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.400(3) . ?
C6 C9 1.491(3) . ?
C7 C8 1.395(3) . ?
C7 C16 1.492(3) . ?
C8 H8 0.9300 . ?
C9 C14 1.387(3) . ?
C9 C10 1.389(3) . ?
C10 C11 1.387(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.390(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.384(3) . ?
C12 C15 1.502(3) . ?
C13 C14 1.387(3) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C16 C21 1.385(3) . ?
C16 C17 1.391(3) . ?
C17 C18 1.386(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.382(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.386(3) . ?
C19 C22 1.493(3) . ?
C20 C21 1.383(3) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C23 C24 1.376(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.368(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.369(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.395(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.484(4) . ?
C28 C29 1.392(4) . ?
C29 C30 1.367(5) . ?
C29 H29 0.9300 . ?
C30 C31 1.373(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.390(4) . ?
C31 H31 0.9300 . ?
C32 H32 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































































































































O1 Mn1 O5 100.22(8) . 1_665 ?
O1 Mn1 O10 90.52(9) . . ?
O5 Mn1 O10 89.69(7) 1_665 . ?
O1 Mn1 O9 91.43(8) . . ?
O5 Mn1 O9 87.28(7) 1_665 . ?
O10 Mn1 O9 176.64(7) . . ?
O1 Mn1 N2 164.85(8) . . ?
O5 Mn1 N2 94.92(8) 1_665 . ?
O10 Mn1 N2 89.49(10) . . ?
O9 Mn1 N2 89.33(8) . . ?
O1 Mn1 N1 92.59(8) . . ?
O5 Mn1 N1 166.77(7) 1_665 . ?
O10 Mn1 N1 93.49(8) . . ?
O9 Mn1 N1 89.15(7) . . ?
N2 Mn1 N1 72.29(9) . . ?
C1 O1 Mn1 160.95(16) . . ?
C4 O3 H3A 109(3) . . ?
C15 O5 Mn1 129.27(15) . 1_445 ?
C22 O7 H7A 111(2) . . ?
Mn1 O9 H9A 116(2) . . ?
Mn1 O9 H9B 123.0(19) . . ?
H9A O9 H9B 111(2) . . ?
Mn1 O10 H10B 144.1 . . ?
Mn1 O10 H10A 99.1 . . ?
H10B O10 H10A 116.8 . . ?
C23 N1 C27 118.1(2) . . ?
C23 N1 Mn1 124.40(18) . . ?
C27 N1 Mn1 116.73(18) . . ?
C32 N2 C28 118.6(3) . . ?
C32 N2 Mn1 123.8(2) . . ?
C28 N2 Mn1 116.51(18) . . ?
O1 C1 O2 123.3(2) . . ?
O1 C1 C2 116.1(2) . . ?
O2 C1 C2 120.6(2) . . ?
C8 C2 C3 118.25(18) . . ?
C8 C2 C1 114.45(18) . . ?
C3 C2 C1 127.11(19) . . ?
C5 C3 C2 118.23(18) . . ?
C5 C3 C4 113.47(18) . . ?
C2 C3 C4 128.28(18) . . ?
O4 C4 O3 120.3(2) . . ?
O4 C4 C3 118.97(19) . . ?
O3 C4 C3 120.7(2) . . ?
C6 C5 C3 123.00(19) . . ?
C6 C5 H5 118.5 . . ?
C3 C5 H5 118.5 . . ?
C5 C6 C7 118.87(18) . . ?
C5 C6 C9 119.50(18) . . ?
C7 C6 C9 121.64(18) . . ?
C8 C7 C6 118.41(18) . . ?
C8 C7 C16 119.62(18) . . ?
C6 C7 C16 121.89(18) . . ?
C2 C8 C7 123.17(19) . . ?
C2 C8 H8 118.4 . . ?
C7 C8 H8 118.4 . . ?
C14 C9 C10 118.58(19) . . ?
C14 C9 C6 121.24(19) . . ?
C10 C9 C6 120.17(19) . . ?
C11 C10 C9 120.7(2) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C10 C11 C12 120.5(2) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C13 C12 C11 118.82(19) . . ?
C13 C12 C15 119.95(19) . . ?
C11 C12 C15 121.2(2) . . ?
C12 C13 C14 120.6(2) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C9 C14 C13 120.7(2) . . ?
C9 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
O6 C15 O5 124.2(2) . . ?
O6 C15 C12 119.1(2) . . ?
O5 C15 C12 116.71(19) . . ?
C21 C16 C17 118.8(2) . . ?
C21 C16 C7 121.21(19) . . ?
C17 C16 C7 120.00(19) . . ?
C18 C17 C16 120.7(2) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C19 C18 C17 120.1(2) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C18 C19 C20 119.2(2) . . ?
C18 C19 C22 121.5(2) . . ?
C20 C19 C22 119.2(2) . . ?
C21 C20 C19 120.7(2) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C20 C21 C16 120.3(2) . . ?
C20 C21 H21 119.8 . . ?
C16 C21 H21 119.8 . . ?
O8 C22 O7 124.0(2) . . ?
O8 C22 C19 122.8(2) . . ?
O7 C22 C19 113.2(2) . . ?
N1 C23 C24 123.8(3) . . ?
N1 C23 H23 118.1 . . ?
C24 C23 H23 118.1 . . ?
C25 C24 C23 117.7(3) . . ?
C25 C24 H24 121.2 . . ?
C23 C24 H24 121.2 . . ?
C24 C25 C26 120.1(3) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C25 C26 C27 119.3(3) . . ?
C25 C26 H26 120.3 . . ?
C27 C26 H26 120.3 . . ?
N1 C27 C26 121.0(3) . . ?
N1 C27 C28 116.0(2) . . ?
C26 C27 C28 123.0(3) . . ?
N2 C28 C29 121.2(3) . . ?
N2 C28 C27 116.6(2) . . ?
C29 C28 C27 122.3(3) . . ?
C30 C29 C28 119.7(3) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C29 C30 C31 119.1(3) . . ?
C29 C30 H30 120.5 . . ?
C31 C30 H30 120.5 . . ?
C30 C31 C32 118.6(4) . . ?
C30 C31 H31 120.7 . . ?
C32 C31 H31 120.7 . . ?
N2 C32 C31 122.8(3) . . ?
N2 C32 H32 118.6 . . ?
C31 C32 H32 118.6 . . ?



loop_

_geom_torsion_atom_site_label_1

_geom_torsion_atom_site_label_2

_geom_torsion_atom_site_label_3

_geom_torsion_atom_site_label_4

_geom_torsion

_geom_torsion_site_symmetry_1

_geom_torsion_site_symmetry_2

_geom_torsion_site_symmetry_3

_geom_torsion_site_symmetry_4

_geom_torsion_publ_flag



















































































































O5 Mn1 O1 C1 -15.9(6) 1_665 . . . ?
O10 Mn1 O1 C1 -105.7(6) . . . . ?
O9 Mn1 O1 C1 71.6(6) . . . . ?
N2 Mn1 O1 C1 164.3(5) . . . . ?
N1 Mn1 O1 C1 160.8(6) . . . . ?
O1 Mn1 N1 C23 -8.2(2) . . . . ?
O5 Mn1 N1 C23 157.5(3) 1_665 . . . ?
O10 Mn1 N1 C23 -98.9(2) . . . . ?
O9 Mn1 N1 C23 83.2(2) . . . . ?
N2 Mn1 N1 C23 172.8(2) . . . . ?
O1 Mn1 N1 C27 -177.62(17) . . . . ?
O5 Mn1 N1 C27 -11.9(4) 1_665 . . . ?
O10 Mn1 N1 C27 91.70(18) . . . . ?
O9 Mn1 N1 C27 -86.22(18) . . . . ?
N2 Mn1 N1 C27 3.35(17) . . . . ?
O1 Mn1 N2 C32 170.0(3) . . . . ?
O5 Mn1 N2 C32 -9.8(2) 1_665 . . . ?
O10 Mn1 N2 C32 79.8(2) . . . . ?
O9 Mn1 N2 C32 -97.0(2) . . . . ?
N1 Mn1 N2 C32 173.7(3) . . . . ?
O1 Mn1 N2 C28 1.9(4) . . . . ?
O5 Mn1 N2 C28 -177.86(19) 1_665 . . . ?
O10 Mn1 N2 C28 -88.2(2) . . . . ?
O9 Mn1 N2 C28 94.93(19) . . . . ?
N1 Mn1 N2 C28 5.61(18) . . . . ?
Mn1 O1 C1 O2 -11.0(7) . . . . ?
Mn1 O1 C1 C2 170.9(5) . . . . ?
O1 C1 C2 C8 -19.6(3) . . . . ?
O2 C1 C2 C8 162.2(2) . . . . ?
O1 C1 C2 C3 155.3(2) . . . . ?
O2 C1 C2 C3 -22.9(3) . . . . ?
C8 C2 C3 C5 1.5(3) . . . . ?
C1 C2 C3 C5 -173.2(2) . . . . ?
C8 C2 C3 C4 -180.0(2) . . . . ?
C1 C2 C3 C4 5.3(3) . . . . ?
C5 C3 C4 O4 7.6(3) . . . . ?
C2 C3 C4 O4 -170.9(2) . . . . ?
C5 C3 C4 O3 -171.0(2) . . . . ?
C2 C3 C4 O3 10.5(4) . . . . ?
C2 C3 C5 C6 0.6(3) . . . . ?
C4 C3 C5 C6 -178.12(19) . . . . ?
C3 C5 C6 C7 -1.3(3) . . . . ?
C3 C5 C6 C9 178.57(19) . . . . ?
C5 C6 C7 C8 -0.2(3) . . . . ?
C9 C6 C7 C8 179.95(19) . . . . ?
C5 C6 C7 C16 176.48(19) . . . . ?
C9 C6 C7 C16 -3.3(3) . . . . ?
C3 C2 C8 C7 -3.1(3) . . . . ?
C1 C2 C8 C7 172.24(19) . . . . ?
C6 C7 C8 C2 2.5(3) . . . . ?
C16 C7 C8 C2 -174.32(19) . . . . ?
C5 C6 C9 C14 125.1(2) . . . . ?
C7 C6 C9 C14 -55.0(3) . . . . ?
C5 C6 C9 C10 -56.2(3) . . . . ?
C7 C6 C9 C10 123.6(2) . . . . ?
C14 C9 C10 C11 3.9(3) . . . . ?
C6 C9 C10 C11 -174.8(2) . . . . ?
C9 C10 C11 C12 -1.4(4) . . . . ?
C10 C11 C12 C13 -1.9(4) . . . . ?
C10 C11 C12 C15 175.3(2) . . . . ?
C11 C12 C13 C14 2.7(3) . . . . ?
C15 C12 C13 C14 -174.5(2) . . . . ?
C10 C9 C14 C13 -3.1(3) . . . . ?
C6 C9 C14 C13 175.6(2) . . . . ?
C12 C13 C14 C9 -0.2(4) . . . . ?
Mn1 O5 C15 O6 24.8(4) 1_445 . . . ?
Mn1 O5 C15 C12 -152.41(15) 1_445 . . . ?
C13 C12 C15 O6 1.2(3) . . . . ?
C11 C12 C15 O6 -175.9(2) . . . . ?
C13 C12 C15 O5 178.6(2) . . . . ?
C11 C12 C15 O5 1.5(3) . . . . ?
C8 C7 C16 C21 -59.2(3) . . . . ?
C6 C7 C16 C21 124.1(2) . . . . ?
C8 C7 C16 C17 121.2(2) . . . . ?
C6 C7 C16 C17 -55.5(3) . . . . ?
C21 C16 C17 C18 -2.9(4) . . . . ?
C7 C16 C17 C18 176.7(2) . . . . ?
C16 C17 C18 C19 -0.6(4) . . . . ?
C17 C18 C19 C20 3.1(4) . . . . ?
C17 C18 C19 C22 -176.6(2) . . . . ?
C18 C19 C20 C21 -2.0(4) . . . . ?
C22 C19 C20 C21 177.7(2) . . . . ?
C19 C20 C21 C16 -1.6(4) . . . . ?
C17 C16 C21 C20 4.0(4) . . . . ?
C7 C16 C21 C20 -175.6(2) . . . . ?
C18 C19 C22 O8 166.6(3) . . . . ?
C20 C19 C22 O8 -13.1(4) . . . . ?
C18 C19 C22 O7 -13.3(3) . . . . ?
C20 C19 C22 O7 167.0(2) . . . . ?
C27 N1 C23 C24 -0.2(4) . . . . ?
Mn1 N1 C23 C24 -169.5(2) . . . . ?
N1 C23 C24 C25 1.5(4) . . . . ?
C23 C24 C25 C26 -1.6(5) . . . . ?
C24 C25 C26 C27 0.5(5) . . . . ?
C23 N1 C27 C26 -1.1(4) . . . . ?
Mn1 N1 C27 C26 169.1(2) . . . . ?
C23 N1 C27 C28 178.8(2) . . . . ?
Mn1 N1 C27 C28 -11.1(3) . . . . ?
C25 C26 C27 N1 0.9(4) . . . . ?
C25 C26 C27 C28 -178.9(3) . . . . ?
C32 N2 C28 C29 -2.1(4) . . . . ?
Mn1 N2 C28 C29 166.61(19) . . . . ?
C32 N2 C28 C27 178.1(2) . . . . ?
Mn1 N2 C28 C27 -13.2(3) . . . . ?
N1 C27 C28 N2 16.3(3) . . . . ?
C26 C27 C28 N2 -163.9(3) . . . . ?
N1 C27 C28 C29 -163.6(2) . . . . ?
C26 C27 C28 C29 16.3(4) . . . . ?
N2 C28 C29 C30 1.8(4) . . . . ?
C27 C28 C29 C30 -178.3(3) . . . . ?
C28 C29 C30 C31 -0.2(5) . . . . ?
C29 C30 C31 C32 -1.0(5) . . . . ?
C28 N2 C32 C31 0.8(5) . . . . ?
Mn1 N2 C32 C31 -167.0(3) . . . . ?
C30 C31 C32 N2 0.7(5) . . . . ?



loop_

_geom_hbond_atom_site_label_D

_geom_hbond_atom_site_label_H

_geom_hbond_atom_site_label_A

_geom_hbond_distance_DH

_geom_hbond_distance_HA

_geom_hbond_distance_DA

_geom_hbond_angle_DHA

_geom_hbond_site_symmetry_A






O3 H3A O2 0.881(18) 1.530(19) 2.410(3) 177(4) .
O7 H7A O4 0.851(18) 1.74(2) 2.580(3) 169(4) 1_556
O9 H9A O2 0.833(16) 1.985(18) 2.813(3) 173(3) 2_665
O9 H9B O5 0.860(16) 1.98(2) 2.811(3) 161(3) 2
O10 H10B O8 0.89 1.99 2.876(3) 168.6 2_656
O10 H10A O6 0.90 1.78 2.660(3) 164.3 1_665



_diffrn_measured_fraction_theta_max 0.995

_diffrn_reflns_theta_full        27.52

_diffrn_measured_fraction_theta_full 0.995

_refine_diff_density_max         0.340

_refine_diff_density_min         -0.442

_refine_diff_density_rms         0.086

_database_code_depnum_ccdc_archive 'CCDC 1010213'
#######################################################################
#
#                 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            'C26 H23 Co N3 O10.50'

_chemical_formula_weight         604.40



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   C2/c



loop_

_symmetry_equiv_pos_as_xyz








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



_cell_length_a                   28.966(4)

_cell_length_b                   7.6922(7)

_cell_length_c                   24.702(3)

_cell_angle_alpha                90.00

_cell_angle_beta                 107.507(6)

_cell_angle_gamma                90.00

_cell_volume                     5249.0(11)

_cell_formula_units_Z            8

_cell_measurement_temperature    296(2)

_cell_measurement_reflns_used    5469

_cell_measurement_theta_min      1.9

_cell_measurement_theta_max      27.5



_exptl_crystal_description       Prism

_exptl_crystal_colour            Colorless

_exptl_crystal_size_max          0.21

_exptl_crystal_size_mid          0.19

_exptl_crystal_size_min          0.16

_exptl_crystal_density_meas      NONE

_exptl_crystal_density_diffrn    1.530

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             2488

_exptl_absorpt_coefficient_mu    0.720

_exptl_absorpt_correction_type   MULTI-SCAN

_exptl_absorpt_correction_T_min  0.8635

_exptl_absorpt_correction_T_max  0.8935

_exptl_absorpt_process_details   SADABS



_exptl_special_details           
;

 ?

;



_diffrn_ambient_temperature      296(2)

_diffrn_radiation_wavelength     0.71073

_diffrn_radiation_type           MoK\a

_diffrn_radiation_source         'fine-focus sealed tube'

_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker P4'

_diffrn_measurement_method       'ω scans'

_diffrn_detector_area_resol_mean NONE

_diffrn_standards_number         NONE

_diffrn_standards_interval_count NONE

_diffrn_standards_interval_time  NONE

_diffrn_standards_decay_%        NONE

_diffrn_reflns_number            23051

_diffrn_reflns_av_R_equivalents  0.0854

_diffrn_reflns_av_sigmaI/netI    0.0718

_diffrn_reflns_limit_h_min       -34

_diffrn_reflns_limit_h_max       34

_diffrn_reflns_limit_k_min       -9

_diffrn_reflns_limit_k_max       9

_diffrn_reflns_limit_l_min       -29

_diffrn_reflns_limit_l_max       29

_diffrn_reflns_theta_min         1.73

_diffrn_reflns_theta_max         25.50

_reflns_number_total             4879

_reflns_number_gt                3796

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'Bruker XSCANS'

_computing_cell_refinement       'Bruker XSCANS'

_computing_data_reduction        'Bruker SHELXTL'

_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)+(0.0865P)²+0.2679P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct

_atom_sites_solution_secondary   difmap

_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    CONSTR

_refine_ls_extinction_method     none

_refine_ls_extinction_coef       ?

_refine_ls_number_reflns         4879

_refine_ls_number_parameters     370

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0769

_refine_ls_R_factor_gt           0.0543

_refine_ls_wR_factor_ref         0.1623

_refine_ls_wR_factor_gt          0.1416

_refine_ls_goodness_of_fit_ref   1.074

_refine_ls_restrained_S_all      1.074

_refine_ls_shift/su_max          0.000

_refine_ls_shift/su_mean         0.000



loop_

_atom_site_label

_atom_site_type_symbol

_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z

_atom_site_U_iso_or_equiv

_atom_site_adp_type

_atom_site_occupancy

_atom_site_symmetry_multiplicity

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_assembly

_atom_site_disorder_group

































































Co1 Co 0.220678(17) 0.65636(6) 0.66876(2) 0.02872(18) Uani 1 1 d . . .
O1 O 0.16763(9) 0.5689(3) 0.59820(11) 0.0340(6) Uani 1 1 d . . .
O2 O 0.16921(10) 0.2846(3) 0.61625(13) 0.0452(8) Uani 1 1 d . . .
O3 O -0.11355(9) -0.0533(3) 0.36883(13) 0.0446(8) Uani 1 1 d . . .
H3A H -0.1343 -0.1159 0.3779 0.067 Uiso 1 1 d R . .
O4 O -0.17724(9) 0.1124(3) 0.32605(14) 0.0417(7) Uani 1 1 d . . .
O5 O -0.19104(9) 0.4545(3) 0.27346(11) 0.0349(6) Uani 1 1 d . . .
O6 O -0.15879(10) 0.3535(4) 0.20916(12) 0.0457(8) Uani 1 1 d . . .
O7 O 0.09443(12) 1.1594(4) 0.31283(15) 0.0540(9) Uani 1 1 d . . .
H7A H 0.1151 1.2225 0.3039 0.081 Uiso 1 1 d R . .
O8 O 0.14068(12) 0.9488(5) 0.2946(2) 0.0757(12) Uani 1 1 d . . .
O9 O 0.27631(11) 0.7275(4) 0.74251(15) 0.0626(10) Uani 1 1 d . . .
H9A H 0.3000 0.6627 0.7422 0.094 Uiso 1 1 d R . .
H9B H 0.2867 0.8294 0.7527 0.094 Uiso 1 1 d R . .
O10 O 0.26181(10) 0.4288(3) 0.66676(13) 0.0461(8) Uani 1 1 d . . .
H10A H 0.2920 0.4455 0.6817 0.069 Uiso 1 1 d R . .
H10B H 0.2439 0.3393 0.6629 0.069 Uiso 1 1 d R . .
O11 O 0.3434(2) 0.6325(8) 0.4906(3) 0.0615(19) Uani 0.50 1 d P . .
H11A H 0.3313 0.7001 0.5100 0.092 Uiso 0.50 1 d PR . .
H11B H 0.3425 0.6843 0.4599 0.092 Uiso 0.50 1 d PR . .
N1 N 0.25333(12) 0.7982(4) 0.61780(15) 0.0395(8) Uani 1 1 d . . .
N2 N 0.28505(12) 1.0055(4) 0.58028(14) 0.0419(9) Uani 1 1 d . . .
N3 N 0.29756(18) 0.8568(6) 0.5597(2) 0.0656(12) Uani 1 1 d . . .
C1 C 0.15107(13) 0.4166(5) 0.58677(16) 0.0317(8) Uani 1 1 d . . .
C2 C 0.10841(13) 0.3976(5) 0.53503(16) 0.0307(8) Uani 1 1 d . . .
C3 C 0.08044(13) 0.5418(5) 0.51220(16) 0.0330(9) Uani 1 1 d . . .
H3 H 0.0888 0.6499 0.5292 0.040 Uiso 1 1 calc R . .
C4 C 0.04055(13) 0.5280(5) 0.46497(16) 0.0326(9) Uani 1 1 d . . .
H4 H 0.0220 0.6262 0.4510 0.039 Uiso 1 1 calc R . .
C5 C 0.02751(12) 0.3676(5) 0.43765(15) 0.0281(8) Uani 1 1 d . . .
C6 C 0.05568(14) 0.2217(5) 0.45984(16) 0.0345(9) Uani 1 1 d . . .
H6 H 0.0477 0.1144 0.4422 0.041 Uiso 1 1 calc R . .
C7 C 0.09526(14) 0.2357(5) 0.50780(16) 0.0352(9) Uani 1 1 d . . .
H7 H 0.1134 0.1373 0.5223 0.042 Uiso 1 1 calc R . .
C8 C -0.01695(13) 0.3566(5) 0.38785(15) 0.0284(8) Uani 1 1 d . . .
C9 C -0.05133(12) 0.2263(5) 0.38471(15) 0.0283(8) Uani 1 1 d . . .
H9 H -0.0435 0.1349 0.4105 0.034 Uiso 1 1 calc R . .
C10 C -0.09695(12) 0.2284(4) 0.34433(15) 0.0270(8) Uani 1 1 d . . .
C11 C -0.13312(13) 0.0900(5) 0.34541(16) 0.0297(8) Uani 1 1 d . . .
C12 C -0.10864(12) 0.3638(4) 0.30485(15) 0.0260(8) Uani 1 1 d . . .
C13 C -0.15663(13) 0.3871(4) 0.25899(16) 0.0291(8) Uani 1 1 d . . .
C14 C -0.07373(13) 0.4888(5) 0.30549(16) 0.0313(8) Uani 1 1 d . . .
H14 H -0.0811 0.5759 0.2781 0.038 Uiso 1 1 calc R . .
C15 C -0.02829(13) 0.4882(5) 0.34550(16) 0.0303(8) Uani 1 1 d . . .
C16 C 0.00727(13) 0.6217(5) 0.33991(16) 0.0298(8) Uani 1 1 d . . .
C17 C 0.05342(14) 0.5718(5) 0.33924(16) 0.0333(9) Uani 1 1 d . . .
H17 H 0.0629 0.4561 0.3452 0.040 Uiso 1 1 calc R . .
C18 C 0.08509(14) 0.6947(5) 0.32978(17) 0.0360(9) Uani 1 1 d . . .
H18 H 0.1156 0.6606 0.3286 0.043 Uiso 1 1 calc R . .
C19 C 0.07161(14) 0.8686(5) 0.32199(17) 0.0355(9) Uani 1 1 d . . .
C20 C 0.02651(14) 0.9195(5) 0.32412(17) 0.0369(9) Uani 1 1 d . . .
H20 H 0.0178 1.0362 0.3198 0.044 Uiso 1 1 calc R . .
C21 C -0.00606(14) 0.7971(5) 0.33277(17) 0.0351(9) Uani 1 1 d . . .
H21 H -0.0365 0.8318 0.3338 0.042 Uiso 1 1 calc R . .
C22 C 0.10578(14) 0.9950(6) 0.30905(19) 0.0429(10) Uani 1 1 d . . .
C23 C 0.25895(16) 0.9692(6) 0.61494(19) 0.0447(10) Uani 1 1 d . . .
H23 H 0.2465 1.0514 0.6343 0.054 Uiso 1 1 calc R . .
C24 C 0.2773(2) 0.7361(6) 0.5824(2) 0.0598(13) Uani 1 1 d . . .
H24 H 0.2792 0.6183 0.5749 0.072 Uiso 1 1 calc R . .
C25 C 0.30218(18) 1.1741(6) 0.5661(2) 0.0528(12) Uani 1 1 d . . .
H25A H 0.3367 1.1669 0.5715 0.063 Uiso 1 1 calc R . .
H25B H 0.2970 1.2615 0.5920 0.063 Uiso 1 1 calc R . .
C26 C 0.27685(16) 1.2311(6) 0.5056(2) 0.0495(11) Uani 1 1 d . . .
H26A H 0.2804 1.1405 0.4798 0.059 Uiso 1 1 calc R . .
H26B H 0.2926 1.3348 0.4974 0.059 Uiso 1 1 calc 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 O5 2.059(3) 5_566 ?
Co1 O1 2.059(2) . ?
Co1 N1 2.094(3) . ?
Co1 O9 2.109(3) . ?
Co1 O10 2.127(3) . ?
Co1 O4 2.205(3) 5_566 ?
O1 C1 1.265(4) . ?
O2 C1 1.268(4) . ?
O3 C11 1.294(4) . ?
O3 H3A 0.8500 . ?
O4 C11 1.235(4) . ?
O4 Co1 2.205(3) 5_566 ?
O5 C13 1.267(4) . ?
O5 Co1 2.059(3) 5_566 ?
O6 C13 1.241(5) . ?
O7 C22 1.317(5) . ?
O7 H7A 0.8500 . ?
O8 C22 1.222(5) . ?
O9 H9A 0.8499 . ?
O9 H9B 0.8500 . ?
O10 H10A 0.8499 . ?
O10 H10B 0.8500 . ?
O11 H11A 0.8500 . ?
O11 H11B 0.8500 . ?
N1 C23 1.330(5) . ?
N1 C24 1.356(6) . ?
N2 C23 1.331(5) . ?
N2 N3 1.345(5) . ?
N2 C25 1.468(5) . ?
N3 C24 1.311(6) . ?
C1 C2 1.494(5) . ?
C2 C3 1.389(5) . ?
C2 C7 1.412(5) . ?
C3 C4 1.377(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.403(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.399(5) . ?
C5 C8 1.492(5) . ?
C6 C7 1.383(5) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.398(5) . ?
C8 C15 1.421(5) . ?
C9 C10 1.396(5) . ?
C9 H9 0.9300 . ?
C10 C12 1.397(5) . ?
C10 C11 1.500(5) . ?
C12 C14 1.392(5) . ?
C12 C13 1.517(5) . ?
C14 C15 1.388(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.490(5) . ?
C16 C17 1.396(5) . ?
C16 C21 1.399(5) . ?
C17 C18 1.385(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.391(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.380(5) . ?
C19 C22 1.489(5) . ?
C20 C21 1.395(5) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C26 1.518(6) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C26 1.524(9) 7_576 ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?



loop_

_geom_angle_atom_site_label_1

_geom_angle_atom_site_label_2

_geom_angle_atom_site_label_3

_geom_angle

_geom_angle_site_symmetry_1

_geom_angle_site_symmetry_3

_geom_angle_publ_flag






















































































































O5 Co1 O1 95.21(11) 5_566 . ?
O5 Co1 N1 172.07(13) 5_566 . ?
O1 Co1 N1 91.05(12) . . ?
O5 Co1 O9 83.01(13) 5_566 . ?
O1 Co1 O9 175.98(11) . . ?
N1 Co1 O9 91.04(14) . . ?
O5 Co1 O10 91.62(11) 5_566 . ?
O1 Co1 O10 89.55(11) . . ?
N1 Co1 O10 93.30(12) . . ?
O9 Co1 O10 86.90(12) . . ?
O5 Co1 O4 85.97(11) 5_566 5_566 ?
O1 Co1 O4 91.10(11) . 5_566 ?
N1 Co1 O4 89.05(12) . 5_566 ?
O9 Co1 O4 92.38(12) . 5_566 ?
O10 Co1 O4 177.56(11) . 5_566 ?
C1 O1 Co1 128.9(2) . . ?
C11 O3 H3A 110.6 . . ?
C11 O4 Co1 129.2(2) . 5_566 ?
C13 O5 Co1 123.6(2) . 5_566 ?
C22 O7 H7A 108.7 . . ?
Co1 O9 H9A 104.4 . . ?
Co1 O9 H9B 127.3 . . ?
H9A O9 H9B 109.1 . . ?
Co1 O10 H10A 112.0 . . ?
Co1 O10 H10B 109.9 . . ?
H10A O10 H10B 133.3 . . ?
H11A O11 H11B 107.9 . . ?
C23 N1 C24 102.7(4) . . ?
C23 N1 Co1 129.2(3) . . ?
C24 N1 Co1 128.0(3) . . ?
C23 N2 N3 109.5(3) . . ?
C23 N2 C25 129.6(4) . . ?
N3 N2 C25 120.8(4) . . ?
C24 N3 N2 103.6(4) . . ?
O1 C1 O2 123.3(3) . . ?
O1 C1 C2 116.2(3) . . ?
O2 C1 C2 120.4(3) . . ?
C3 C2 C7 118.0(3) . . ?
C3 C2 C1 120.0(3) . . ?
C7 C2 C1 121.9(3) . . ?
C4 C3 C2 121.4(4) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 120.7(3) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C6 C5 C4 118.4(3) . . ?
C6 C5 C8 122.3(3) . . ?
C4 C5 C8 119.1(3) . . ?
C7 C6 C5 120.6(3) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C2 120.8(3) . . ?
C6 C7 H7 119.6 . . ?
C2 C7 H7 119.6 . . ?
C9 C8 C15 117.8(3) . . ?
C9 C8 C5 120.7(3) . . ?
C15 C8 C5 121.2(3) . . ?
C10 C9 C8 122.5(3) . . ?
C10 C9 H9 118.8 . . ?
C8 C9 H9 118.8 . . ?
C9 C10 C12 119.1(3) . . ?
C9 C10 C11 119.7(3) . . ?
C12 C10 C11 121.2(3) . . ?
O4 C11 O3 123.7(3) . . ?
O4 C11 C10 122.8(3) . . ?
O3 C11 C10 113.5(3) . . ?
C14 C12 C10 119.0(3) . . ?
C14 C12 C13 115.2(3) . . ?
C10 C12 C13 125.8(3) . . ?
O6 C13 O5 123.8(3) . . ?
O6 C13 C12 118.5(3) . . ?
O5 C13 C12 117.4(3) . . ?
C15 C14 C12 122.4(3) . . ?
C15 C14 H14 118.8 . . ?
C12 C14 H14 118.8 . . ?
C14 C15 C8 119.1(3) . . ?
C14 C15 C16 117.7(3) . . ?
C8 C15 C16 123.1(3) . . ?
C17 C16 C21 119.5(3) . . ?
C17 C16 C15 120.1(3) . . ?
C21 C16 C15 120.3(3) . . ?
C18 C17 C16 120.0(4) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 120.5(4) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C20 C19 C18 119.8(4) . . ?
C20 C19 C22 121.4(4) . . ?
C18 C19 C22 118.7(4) . . ?
C19 C20 C21 120.4(4) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
C20 C21 C16 119.8(4) . . ?
C20 C21 H21 120.1 . . ?
C16 C21 H21 120.1 . . ?
O8 C22 O7 123.1(4) . . ?
O8 C22 C19 122.3(4) . . ?
O7 C22 C19 114.6(4) . . ?
N1 C23 N2 110.2(4) . . ?
N1 C23 H23 124.9 . . ?
N2 C23 H23 124.9 . . ?
N3 C24 N1 114.1(4) . . ?
N3 C24 H24 123.0 . . ?
N1 C24 H24 123.0 . . ?
N2 C25 C26 113.1(4) . . ?
N2 C25 H25A 109.0 . . ?
C26 C25 H25A 109.0 . . ?
N2 C25 H25B 109.0 . . ?
C26 C25 H25B 109.0 . . ?
H25A C25 H25B 107.8 . . ?
C25 C26 C26 113.4(5) . 7_576 ?
C25 C26 H26A 108.9 . . ?
C26 C26 H26A 108.9 7_576 . ?
C25 C26 H26B 108.9 . . ?
C26 C26 H26B 108.9 7_576 . ?
H26A C26 H26B 107.7 . . ?



loop_

_geom_torsion_atom_site_label_1

_geom_torsion_atom_site_label_2

_geom_torsion_atom_site_label_3

_geom_torsion_atom_site_label_4

_geom_torsion

_geom_torsion_site_symmetry_1

_geom_torsion_site_symmetry_2

_geom_torsion_site_symmetry_3

_geom_torsion_site_symmetry_4

_geom_torsion_publ_flag





























































































O5 Co1 O1 C1 -50.3(3) 5_566 . . . ?
N1 Co1 O1 C1 134.6(3) . . . . ?
O9 Co1 O1 C1 13.3(19) . . . . ?
O10 Co1 O1 C1 41.3(3) . . . . ?
O4 Co1 O1 C1 -136.4(3) 5_566 . . . ?
O5 Co1 N1 C23 -26.2(11) 5_566 . . . ?
O1 Co1 N1 C23 115.9(4) . . . . ?
O9 Co1 N1 C23 -67.5(4) . . . . ?
O10 Co1 N1 C23 -154.5(4) . . . . ?
O4 Co1 N1 C23 24.8(4) 5_566 . . . ?
O5 Co1 N1 C24 148.4(8) 5_566 . . . ?
O1 Co1 N1 C24 -69.5(4) . . . . ?
O9 Co1 N1 C24 107.0(4) . . . . ?
O10 Co1 N1 C24 20.1(4) . . . . ?
O4 Co1 N1 C24 -160.6(4) 5_566 . . . ?
C23 N2 N3 C24 1.2(5) . . . . ?
C25 N2 N3 C24 178.1(4) . . . . ?
Co1 O1 C1 O2 -7.8(6) . . . . ?
Co1 O1 C1 C2 173.1(2) . . . . ?
O1 C1 C2 C3 -19.0(5) . . . . ?
O2 C1 C2 C3 161.9(4) . . . . ?
O1 C1 C2 C7 160.8(4) . . . . ?
O2 C1 C2 C7 -18.3(6) . . . . ?
C7 C2 C3 C4 1.0(6) . . . . ?
C1 C2 C3 C4 -179.2(3) . . . . ?
C2 C3 C4 C5 -1.4(6) . . . . ?
C3 C4 C5 C6 0.6(6) . . . . ?
C3 C4 C5 C8 177.8(3) . . . . ?
C4 C5 C6 C7 0.4(6) . . . . ?
C8 C5 C6 C7 -176.7(4) . . . . ?
C5 C6 C7 C2 -0.7(6) . . . . ?
C3 C2 C7 C6 0.0(6) . . . . ?
C1 C2 C7 C6 -179.8(4) . . . . ?
C6 C5 C8 C9 46.1(5) . . . . ?
C4 C5 C8 C9 -131.0(4) . . . . ?
C6 C5 C8 C15 -140.9(4) . . . . ?
C4 C5 C8 C15 42.0(5) . . . . ?
C15 C8 C9 C10 -4.5(5) . . . . ?
C5 C8 C9 C10 168.7(3) . . . . ?
C8 C9 C10 C12 1.1(5) . . . . ?
C8 C9 C10 C11 -176.5(3) . . . . ?
Co1 O4 C11 O3 139.7(3) 5_566 . . . ?
Co1 O4 C11 C10 -39.8(5) 5_566 . . . ?
C9 C10 C11 O4 154.2(4) . . . . ?
C12 C10 C11 O4 -23.4(6) . . . . ?
C9 C10 C11 O3 -25.4(5) . . . . ?
C12 C10 C11 O3 157.1(3) . . . . ?
C9 C10 C12 C14 2.6(5) . . . . ?
C11 C10 C12 C14 -179.8(3) . . . . ?
C9 C10 C12 C13 -179.0(3) . . . . ?
C11 C10 C12 C13 -1.4(6) . . . . ?
Co1 O5 C13 O6 123.9(3) 5_566 . . . ?
Co1 O5 C13 C12 -62.5(4) 5_566 . . . ?
C14 C12 C13 O6 73.3(4) . . . . ?
C10 C12 C13 O6 -105.2(4) . . . . ?
C14 C12 C13 O5 -100.7(4) . . . . ?
C10 C12 C13 O5 80.8(5) . . . . ?
C10 C12 C14 C15 -2.8(6) . . . . ?
C13 C12 C14 C15 178.6(3) . . . . ?
C12 C14 C15 C8 -0.7(6) . . . . ?
C12 C14 C15 C16 176.2(3) . . . . ?
C9 C8 C15 C14 4.3(5) . . . . ?
C5 C8 C15 C14 -168.9(3) . . . . ?
C9 C8 C15 C16 -172.5(3) . . . . ?
C5 C8 C15 C16 14.3(6) . . . . ?
C14 C15 C16 C17 -127.4(4) . . . . ?
C8 C15 C16 C17 49.4(5) . . . . ?
C14 C15 C16 C21 49.7(5) . . . . ?
C8 C15 C16 C21 -133.5(4) . . . . ?
C21 C16 C17 C18 -2.0(6) . . . . ?
C15 C16 C17 C18 175.1(3) . . . . ?
C16 C17 C18 C19 1.2(6) . . . . ?
C17 C18 C19 C20 0.5(6) . . . . ?
C17 C18 C19 C22 -177.0(4) . . . . ?
C18 C19 C20 C21 -1.4(6) . . . . ?
C22 C19 C20 C21 175.9(4) . . . . ?
C19 C20 C21 C16 0.7(6) . . . . ?
C17 C16 C21 C20 1.1(6) . . . . ?
C15 C16 C21 C20 -176.1(4) . . . . ?
C20 C19 C22 O8 -163.4(5) . . . . ?
C18 C19 C22 O8 14.0(7) . . . . ?
C20 C19 C22 O7 14.7(6) . . . . ?
C18 C19 C22 O7 -167.9(4) . . . . ?
C24 N1 C23 N2 -0.5(5) . . . . ?
Co1 N1 C23 N2 175.1(3) . . . . ?
N3 N2 C23 N1 -0.4(5) . . . . ?
C25 N2 C23 N1 -177.0(4) . . . . ?
N2 N3 C24 N1 -1.7(6) . . . . ?
C23 N1 C24 N3 1.4(6) . . . . ?
Co1 N1 C24 N3 -174.3(3) . . . . ?
C23 N2 C25 C26 -110.2(5) . . . . ?
N3 N2 C25 C26 73.7(6) . . . . ?
N2 C25 C26 C26 66.0(7) . . . 7_576 ?



_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        25.50

_diffrn_measured_fraction_theta_full 0.999

_refine_diff_density_max         0.551

_refine_diff_density_min         -0.599

_refine_diff_density_rms         0.099

_database_code_depnum_ccdc_archive 'CCDC 1010214'
#######################################################################
#
#                 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            
'C27 H23 Co N2 O10'

_chemical_formula_weight         594.40



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   C2/c



loop_

_symmetry_equiv_pos_as_xyz








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



_cell_length_a                   28.550(2)

_cell_length_b                   7.7222(7)

_cell_length_c                   24.645(2)

_cell_angle_alpha                90.00

_cell_angle_beta                 106.196(19)

_cell_angle_gamma                90.00

_cell_volume                     5217.8(7)

_cell_formula_units_Z            8

_cell_measurement_temperature    296(2)

_cell_measurement_reflns_used    6236

_cell_measurement_theta_min      2.6

_cell_measurement_theta_max      27.5



_exptl_crystal_description       Prism

_exptl_crystal_colour            Colorless

_exptl_crystal_size_max          0.21

_exptl_crystal_size_mid          0.20

_exptl_crystal_size_min          0.18

_exptl_crystal_density_meas      NONE

_exptl_crystal_density_diffrn    1.513

_exptl_crystal_density_method    NONE

_exptl_crystal_F_000             2448

_exptl_absorpt_coefficient_mu    0.720

_exptl_absorpt_correction_type   MULTI-SCAN

_exptl_absorpt_correction_T_min  0.8634

_exptl_absorpt_correction_T_max  0.8813

_exptl_absorpt_process_details   SADABS



_exptl_special_details           
;

 ?

;



_diffrn_ambient_temperature      296(2)

_diffrn_radiation_wavelength     0.71073

_diffrn_radiation_type           MoK\a

_diffrn_radiation_source         'fine-focus sealed tube'

_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker P4'

_diffrn_measurement_method       'ω scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            22653

_diffrn_reflns_av_R_equivalents  0.0873

_diffrn_reflns_av_sigmaI/netI    0.0678

_diffrn_reflns_limit_h_min       -34

_diffrn_reflns_limit_h_max       34

_diffrn_reflns_limit_k_min       -9

_diffrn_reflns_limit_k_max       9

_diffrn_reflns_limit_l_min       -29

_diffrn_reflns_limit_l_max       29

_diffrn_reflns_theta_min         2.57

_diffrn_reflns_theta_max         25.50

_reflns_number_total             4849

_reflns_number_gt                4024

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'Bruker XSCANS'

_computing_cell_refinement       'Bruker XSCANS'

_computing_data_reduction        'Bruker SHELXTL'

_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)+(0.0401P)²+4.9602P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct

_atom_sites_solution_secondary   difmap

_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    CONSTR

_refine_ls_extinction_method     none

_refine_ls_extinction_coef       ?

_refine_ls_number_reflns         4849

_refine_ls_number_parameters     363

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0578

_refine_ls_R_factor_gt           0.0443

_refine_ls_wR_factor_ref         0.1106

_refine_ls_wR_factor_gt          0.1014

_refine_ls_goodness_of_fit_ref   1.076

_refine_ls_restrained_S_all      1.076

_refine_ls_shift/su_max          0.002

_refine_ls_shift/su_mean         0.000



loop_

_atom_site_label

_atom_site_type_symbol

_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z

_atom_site_U_iso_or_equiv

_atom_site_adp_type

_atom_site_occupancy

_atom_site_symmetry_multiplicity

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_assembly

_atom_site_disorder_group































































Co1 Co 0.223812(13) 0.35221(5) 0.662454(15) 0.02505(12) Uani 1 1 d . . .
O1 O 0.16937(7) 0.4394(2) 0.59403(8) 0.0309(5) Uani 1 1 d . . .
O2 O 0.17015(7) 0.7234(2) 0.61127(9) 0.0362(5) Uani 1 1 d . . .
O3 O 0.13830(8) 0.0406(3) 0.28359(12) 0.0543(7) Uani 1 1 d . . .
O4 O 0.09616(9) -0.1652(3) 0.31243(12) 0.0500(6) Uani 1 1 d . . .
H4A H 0.1150 -0.2280 0.3018 0.075 Uiso 1 1 calc R . .
O5 O -0.16031(7) 0.6408(3) 0.21281(9) 0.0406(5) Uani 1 1 d . . .
O6 O -0.19299(7) 0.5400(3) 0.27833(8) 0.0327(5) Uani 1 1 d . . .
O7 O -0.17903(6) 0.8770(2) 0.33338(9) 0.0327(5) Uani 1 1 d . . .
O8 O -0.11441(7) 1.0455(3) 0.36984(10) 0.0431(6) Uani 1 1 d . . .
H8A H -0.1352 1.1094 0.3763 0.065 Uiso 1 1 calc R . .
O9 O 0.26117(7) 0.5918(3) 0.66057(9) 0.0372(5) Uani 1 1 d . . .
H9A H 0.2384 0.6662 0.6516 0.056 Uiso 1 1 d R . .
H9B H 0.2818 0.6339 0.6893 0.056 Uiso 1 1 d R . .
O10 O 0.27950(7) 0.2747(3) 0.73273(9) 0.0436(6) Uani 1 1 d . . .
H10B H 0.2834 0.1664 0.7382 0.065 Uiso 1 1 d R . .
H10A H 0.3052 0.3351 0.7370 0.065 Uiso 1 1 d R . .
N1 N 0.25821(9) 0.2230(3) 0.60972(11) 0.0340(6) Uani 1 1 d . . .
N2 N 0.29091(9) 0.0096(3) 0.57283(11) 0.0370(6) Uani 1 1 d . . .
C1 C 0.15211(10) 0.5901(3) 0.58308(11) 0.0267(6) Uani 1 1 d . . .
C2 C 0.10846(10) 0.6073(3) 0.53251(11) 0.0263(6) Uani 1 1 d . . .
C3 C 0.08248(10) 0.4598(4) 0.51000(11) 0.0287(6) Uani 1 1 d . . .
H3 H 0.0924 0.3526 0.5264 0.034 Uiso 1 1 calc R . .
C4 C 0.04188(10) 0.4699(4) 0.46345(12) 0.0300(6) Uani 1 1 d . . .
H4 H 0.0243 0.3700 0.4499 0.036 Uiso 1 1 calc R . .
C5 C 0.02708(9) 0.6286(3) 0.43668(11) 0.0252(6) Uani 1 1 d . . .
C6 C 0.05368(10) 0.7766(4) 0.45876(12) 0.0321(6) Uani 1 1 d . . .
H6 H 0.0447 0.8830 0.4413 0.039 Uiso 1 1 calc R . .
C7 C 0.09358(10) 0.7671(4) 0.50667(12) 0.0321(7) Uani 1 1 d . . .
H7 H 0.1104 0.8674 0.5215 0.039 Uiso 1 1 calc R . .
C8 C -0.01762(9) 0.6350(3) 0.38803(11) 0.0254(6) Uani 1 1 d . . .
C9 C -0.02858(9) 0.5039(4) 0.34620(11) 0.0268(6) Uani 1 1 d . . .
C10 C 0.00716(10) 0.3704(4) 0.33954(11) 0.0275(6) Uani 1 1 d . . .
C11 C 0.05339(10) 0.4193(4) 0.33612(12) 0.0305(6) Uani 1 1 d . . .
H11 H 0.0629 0.5348 0.3410 0.037 Uiso 1 1 calc R . .
C12 C 0.08509(10) 0.2972(4) 0.32555(12) 0.0312(6) Uani 1 1 d . . .
H12 H 0.1156 0.3314 0.3229 0.037 Uiso 1 1 calc R . .
C13 C 0.07175(10) 0.1239(4) 0.31881(12) 0.0293(6) Uani 1 1 d . . .
C14 C 0.02611(10) 0.0732(4) 0.32336(12) 0.0334(7) Uani 1 1 d . . .
H14 H 0.0172 -0.0431 0.3199 0.040 Uiso 1 1 calc R . .
C15 C -0.00612(10) 0.1961(4) 0.33311(13) 0.0325(7) Uani 1 1 d . . .
H15 H -0.0368 0.1621 0.3354 0.039 Uiso 1 1 calc R . .
C16 C 0.10518(10) -0.0023(4) 0.30324(13) 0.0350(7) Uani 1 1 d . . .
C17 C -0.07458(10) 0.5036(4) 0.30719(12) 0.0293(6) Uani 1 1 d . . .
H17 H -0.0820 0.4165 0.2801 0.035 Uiso 1 1 calc R . .
C18 C -0.10975(9) 0.6279(3) 0.30714(11) 0.0248(6) Uani 1 1 d . . .
C19 C -0.09819(9) 0.7639(3) 0.34618(11) 0.0246(6) Uani 1 1 d . . .
C20 C -0.05214(9) 0.7657(4) 0.38550(11) 0.0261(6) Uani 1 1 d . . .
H20 H -0.0442 0.8572 0.4109 0.031 Uiso 1 1 calc R . .
C21 C -0.15816(10) 0.6065(3) 0.26285(12) 0.0251(6) Uani 1 1 d . . .
C22 C -0.13463(10) 0.8991(3) 0.34886(12) 0.0268(6) Uani 1 1 d . . .
C23 C 0.26241(12) 0.0532(4) 0.60576(14) 0.0392(7) Uani 1 1 d . . .
H23 H 0.2474 -0.0266 0.6237 0.047 Uiso 1 1 calc R . .
C24 C 0.28615(13) 0.2905(4) 0.57782(15) 0.0484(9) Uani 1 1 d . . .
H24 H 0.2906 0.4080 0.5727 0.058 Uiso 1 1 calc R . .
C25 C 0.30631(14) 0.1607(4) 0.55488(16) 0.0528(9) Uani 1 1 d . . .
H25 H 0.3267 0.1723 0.5315 0.063 Uiso 1 1 calc R . .
C26 C 0.30498(13) -0.1676(4) 0.56116(15) 0.0466(8) Uani 1 1 d . . .
H26A H 0.2993 -0.2456 0.5895 0.056 Uiso 1 1 calc R . .
H26B H 0.3396 -0.1696 0.5642 0.056 Uiso 1 1 calc R . .
C27 C 0.27681(12) -0.2328(4) 0.50270(14) 0.0453(8) Uani 1 1 d . . .
H27A H 0.2792 -0.1476 0.4747 0.054 Uiso 1 1 calc R . .
H27B H 0.2918 -0.3389 0.4947 0.054 Uiso 1 1 calc 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 O1 2.0615(19) . ?
Co1 O6 2.0768(19) 5_566 ?
Co1 O10 2.086(2) . ?
Co1 N1 2.088(2) . ?
Co1 O9 2.143(2) . ?
Co1 O7 2.2025(19) 5_566 ?
O1 C1 1.263(3) . ?
O2 C1 1.268(3) . ?
O3 C16 1.222(4) . ?
O4 C16 1.316(4) . ?
O4 H4A 0.8200 . ?
O5 C21 1.246(3) . ?
O6 C21 1.269(3) . ?
O6 Co1 2.0768(19) 5_566 ?
O7 C22 1.230(3) . ?
O7 Co1 2.2025(19) 5_566 ?
O8 C22 1.308(3) . ?
O8 H8A 0.8200 . ?
O9 H9A 0.8501 . ?
O9 H9B 0.8499 . ?
O10 H10B 0.8499 . ?
O10 H10A 0.8499 . ?
N1 C23 1.323(4) . ?
N1 C24 1.370(4) . ?
N2 C23 1.343(4) . ?
N2 C25 1.363(4) . ?
N2 C26 1.477(4) . ?
C1 C2 1.502(4) . ?
C2 C3 1.388(4) . ?
C2 C7 1.399(4) . ?
C3 C4 1.387(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.400(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.396(4) . ?
C5 C8 1.488(4) . ?
C6 C7 1.395(4) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C20 1.399(4) . ?
C8 C9 1.416(4) . ?
C9 C17 1.395(4) . ?
C9 C10 1.491(4) . ?
C10 C15 1.395(4) . ?
C10 C11 1.398(4) . ?
C11 C12 1.381(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.389(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.395(4) . ?
C13 C16 1.487(4) . ?
C14 C15 1.389(4) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C17 C18 1.389(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.400(4) . ?
C18 C21 1.512(4) . ?
C19 C20 1.399(4) . ?
C19 C22 1.488(4) . ?
C20 H20 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.356(5) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C27 1.526(5) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C27 1.522(6) 7_546 ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?



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 Co1 O6 94.21(8) . 5_566 ?
O1 Co1 O10 177.62(8) . . ?
O6 Co1 O10 84.60(8) 5_566 . ?
O1 Co1 N1 91.43(9) . . ?
O6 Co1 N1 173.61(9) 5_566 . ?
O10 Co1 N1 89.88(9) . . ?
O1 Co1 O9 88.09(8) . . ?
O6 Co1 O9 88.86(8) 5_566 . ?
O10 Co1 O9 89.83(8) . . ?
N1 Co1 O9 94.35(9) . . ?
O1 Co1 O7 89.17(7) . 5_566 ?
O6 Co1 O7 85.65(8) 5_566 5_566 ?
O10 Co1 O7 92.79(8) . 5_566 ?
N1 Co1 O7 91.43(9) . 5_566 ?
O9 Co1 O7 173.66(7) . 5_566 ?
C1 O1 Co1 129.48(17) . . ?
C16 O4 H4A 109.5 . . ?
C21 O6 Co1 124.77(17) . 5_566 ?
C22 O7 Co1 131.21(18) . 5_566 ?
C22 O8 H8A 109.5 . . ?
Co1 O9 H9A 103.9 . . ?
Co1 O9 H9B 123.0 . . ?
H9A O9 H9B 105.1 . . ?
Co1 O10 H10B 116.8 . . ?
Co1 O10 H10A 112.2 . . ?
H10B O10 H10A 116.7 . . ?
C23 N1 C24 104.8(3) . . ?
C23 N1 Co1 126.0(2) . . ?
C24 N1 Co1 128.7(2) . . ?
C23 N2 C25 106.6(3) . . ?
C23 N2 C26 126.4(3) . . ?
C25 N2 C26 126.9(3) . . ?
O1 C1 O2 123.8(2) . . ?
O1 C1 C2 116.3(2) . . ?
O2 C1 C2 119.9(2) . . ?
C3 C2 C7 118.8(2) . . ?
C3 C2 C1 119.1(2) . . ?
C7 C2 C1 122.1(2) . . ?
C4 C3 C2 121.0(3) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 120.7(3) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C6 C5 C4 118.2(2) . . ?
C6 C5 C8 122.5(2) . . ?
C4 C5 C8 119.1(2) . . ?
C7 C6 C5 120.9(3) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C6 C7 C2 120.3(3) . . ?
C6 C7 H7 119.9 . . ?
C2 C7 H7 119.9 . . ?
C20 C8 C9 118.2(2) . . ?
C20 C8 C5 119.7(2) . . ?
C9 C8 C5 121.9(2) . . ?
C17 C9 C8 118.5(2) . . ?
C17 C9 C10 117.7(2) . . ?
C8 C9 C10 123.7(2) . . ?
C15 C10 C11 119.0(3) . . ?
C15 C10 C9 120.4(2) . . ?
C11 C10 C9 120.4(2) . . ?
C12 C11 C10 120.4(3) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 120.6(3) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C14 119.5(3) . . ?
C12 C13 C16 119.2(3) . . ?
C14 C13 C16 121.2(3) . . ?
C15 C14 C13 120.1(3) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C10 120.5(3) . . ?
C14 C15 H15 119.8 . . ?
C10 C15 H15 119.8 . . ?
O3 C16 O4 122.5(3) . . ?
O3 C16 C13 123.2(3) . . ?
O4 C16 C13 114.3(3) . . ?
C18 C17 C9 122.8(3) . . ?
C18 C17 H17 118.6 . . ?
C9 C17 H17 118.6 . . ?
C17 C18 C19 119.1(2) . . ?
C17 C18 C21 116.1(2) . . ?
C19 C18 C21 124.8(2) . . ?
C20 C19 C18 118.6(2) . . ?
C20 C19 C22 119.7(2) . . ?
C18 C19 C22 121.5(2) . . ?
C19 C20 C8 122.5(2) . . ?
C19 C20 H20 118.7 . . ?
C8 C20 H20 118.7 . . ?
O5 C21 O6 123.9(2) . . ?
O5 C21 C18 118.3(2) . . ?
O6 C21 C18 117.5(2) . . ?
O7 C22 O8 123.1(2) . . ?
O7 C22 C19 124.2(2) . . ?
O8 C22 C19 112.8(2) . . ?
N1 C23 N2 112.1(3) . . ?
N1 C23 H23 124.0 . . ?
N2 C23 H23 124.0 . . ?
C25 C24 N1 109.9(3) . . ?
C25 C24 H24 125.0 . . ?
N1 C24 H24 125.0 . . ?
C24 C25 N2 106.5(3) . . ?
C24 C25 H25 126.7 . . ?
N2 C25 H25 126.7 . . ?
N2 C26 C27 112.9(3) . . ?
N2 C26 H26A 109.0 . . ?
C27 C26 H26A 109.0 . . ?
N2 C26 H26B 109.0 . . ?
C27 C26 H26B 109.0 . . ?
H26A C26 H26B 107.8 . . ?
C27 C27 C26 113.1(3) 7_546 . ?
C27 C27 H27A 109.0 7_546 . ?
C26 C27 H27A 109.0 . . ?
C27 C27 H27B 109.0 7_546 . ?
C26 C27 H27B 109.0 . . ?
H27A C27 H27B 107.8 . . ?



loop_

_geom_torsion_atom_site_label_1

_geom_torsion_atom_site_label_2

_geom_torsion_atom_site_label_3

_geom_torsion_atom_site_label_4

_geom_torsion

_geom_torsion_site_symmetry_1

_geom_torsion_site_symmetry_2

_geom_torsion_site_symmetry_3

_geom_torsion_site_symmetry_4

_geom_torsion_publ_flag





























































































O6 Co1 O1 C1 51.2(2) 5_566 . . . ?
O10 Co1 O1 C1 -9(2) . . . . ?
N1 Co1 O1 C1 -131.8(2) . . . . ?
O9 Co1 O1 C1 -37.5(2) . . . . ?
O7 Co1 O1 C1 136.8(2) 5_566 . . . ?
O1 Co1 N1 C23 -112.7(3) . . . . ?
O6 Co1 N1 C23 39.2(9) 5_566 . . . ?
O10 Co1 N1 C23 69.3(3) . . . . ?
O9 Co1 N1 C23 159.1(3) . . . . ?
O7 Co1 N1 C23 -23.5(3) 5_566 . . . ?
O1 Co1 N1 C24 76.5(3) . . . . ?
O6 Co1 N1 C24 -131.6(7) 5_566 . . . ?
O10 Co1 N1 C24 -101.5(3) . . . . ?
O9 Co1 N1 C24 -11.7(3) . . . . ?
O7 Co1 N1 C24 165.7(3) 5_566 . . . ?
Co1 O1 C1 O2 8.2(4) . . . . ?
Co1 O1 C1 C2 -173.41(17) . . . . ?
O1 C1 C2 C3 16.1(4) . . . . ?
O2 C1 C2 C3 -165.4(3) . . . . ?
O1 C1 C2 C7 -162.7(3) . . . . ?
O2 C1 C2 C7 15.7(4) . . . . ?
C7 C2 C3 C4 -1.3(4) . . . . ?
C1 C2 C3 C4 179.8(2) . . . . ?
C2 C3 C4 C5 2.3(4) . . . . ?
C3 C4 C5 C6 -1.3(4) . . . . ?
C3 C4 C5 C8 -178.0(2) . . . . ?
C4 C5 C6 C7 -0.8(4) . . . . ?
C8 C5 C6 C7 175.8(3) . . . . ?
C5 C6 C7 C2 1.8(5) . . . . ?
C3 C2 C7 C6 -0.7(4) . . . . ?
C1 C2 C7 C6 178.1(3) . . . . ?
C6 C5 C8 C20 -42.6(4) . . . . ?
C4 C5 C8 C20 134.0(3) . . . . ?
C6 C5 C8 C9 142.9(3) . . . . ?
C4 C5 C8 C9 -40.5(4) . . . . ?
C20 C8 C9 C17 -4.8(4) . . . . ?
C5 C8 C9 C17 169.8(3) . . . . ?
C20 C8 C9 C10 172.0(3) . . . . ?
C5 C8 C9 C10 -13.4(4) . . . . ?
C17 C9 C10 C15 -50.2(4) . . . . ?
C8 C9 C10 C15 133.0(3) . . . . ?
C17 C9 C10 C11 125.8(3) . . . . ?
C8 C9 C10 C11 -51.0(4) . . . . ?
C15 C10 C11 C12 1.1(4) . . . . ?
C9 C10 C11 C12 -174.9(3) . . . . ?
C10 C11 C12 C13 -0.7(4) . . . . ?
C11 C12 C13 C14 -0.7(4) . . . . ?
C11 C12 C13 C16 175.5(3) . . . . ?
C12 C13 C14 C15 1.7(4) . . . . ?
C16 C13 C14 C15 -174.4(3) . . . . ?
C13 C14 C15 C10 -1.3(5) . . . . ?
C11 C10 C15 C14 -0.1(4) . . . . ?
C9 C10 C15 C14 175.9(3) . . . . ?
C12 C13 C16 O3 -17.2(5) . . . . ?
C14 C13 C16 O3 158.9(3) . . . . ?
C12 C13 C16 O4 162.8(3) . . . . ?
C14 C13 C16 O4 -21.1(4) . . . . ?
C8 C9 C17 C18 1.0(4) . . . . ?
C10 C9 C17 C18 -176.0(3) . . . . ?
C9 C17 C18 C19 2.8(4) . . . . ?
C9 C17 C18 C21 -178.6(3) . . . . ?
C17 C18 C19 C20 -2.6(4) . . . . ?
C21 C18 C19 C20 178.9(3) . . . . ?
C17 C18 C19 C22 -178.9(3) . . . . ?
C21 C18 C19 C22 2.6(4) . . . . ?
C18 C19 C20 C8 -1.3(4) . . . . ?
C22 C19 C20 C8 175.0(3) . . . . ?
C9 C8 C20 C19 5.1(4) . . . . ?
C5 C8 C20 C19 -169.6(3) . . . . ?
Co1 O6 C21 O5 -123.8(2) 5_566 . . . ?
Co1 O6 C21 C18 62.7(3) 5_566 . . . ?
C17 C18 C21 O5 -73.5(3) . . . . ?
C19 C18 C21 O5 105.0(3) . . . . ?
C17 C18 C21 O6 100.4(3) . . . . ?
C19 C18 C21 O6 -81.1(3) . . . . ?
Co1 O7 C22 O8 -144.6(2) 5_566 . . . ?
Co1 O7 C22 C19 35.0(4) 5_566 . . . ?
C20 C19 C22 O7 -150.6(3) . . . . ?
C18 C19 C22 O7 25.6(4) . . . . ?
C20 C19 C22 O8 29.1(4) . . . . ?
C18 C19 C22 O8 -154.7(3) . . . . ?
C24 N1 C23 N2 -0.6(4) . . . . ?
Co1 N1 C23 N2 -173.3(2) . . . . ?
C25 N2 C23 N1 0.5(4) . . . . ?
C26 N2 C23 N1 177.3(3) . . . . ?
C23 N1 C24 C25 0.5(4) . . . . ?
Co1 N1 C24 C25 172.9(2) . . . . ?
N1 C24 C25 N2 -0.2(4) . . . . ?
C23 N2 C25 C24 -0.2(4) . . . . ?
C26 N2 C25 C24 -177.0(3) . . . . ?
C23 N2 C26 C27 103.5(4) . . . . ?
C25 N2 C26 C27 -80.3(4) . . . . ?
N2 C26 C27 C27 -69.6(5) . . . 7_546 ?



loop_

_geom_hbond_atom_site_label_D

_geom_hbond_atom_site_label_H

_geom_hbond_atom_site_label_A

_geom_hbond_distance_DH

_geom_hbond_distance_HA

_geom_hbond_distance_DA

_geom_hbond_angle_DHA

_geom_hbond_site_symmetry_A







O10 H10A O3 0.85 2.06 2.869(3) 158.8 7_556
O10 H10B O6 0.85 1.90 2.701(3) 157.2 8_556
O9 H9B O3 0.85 2.57 2.996(3) 112.0 7_556
O9 H9B O5 0.85 2.36 3.056(3) 139.6 8_566
O9 H9A O2 0.85 1.97 2.739(3) 149.2 .
O8 H8A O2 0.82 1.71 2.519(3) 167.9 5_576
O4 H4A O5 0.82 1.76 2.573(3) 173.0 2_545



_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        25.50

_diffrn_measured_fraction_theta_full 0.999

_refine_diff_density_max         0.284

_refine_diff_density_min         -0.468

_refine_diff_density_rms         0.060

_database_code_depnum_ccdc_archive 'CCDC 1010215'
#######################################################################
#
#                 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            'C22 H20 Co2 O13'

_chemical_formula_weight         610.24



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'
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)/c



loop_

_symmetry_equiv_pos_as_xyz




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



_cell_length_a                   14.444(8)

_cell_length_b                   6.526(4)

_cell_length_c                   23.959(13)

_cell_angle_alpha                90.00

_cell_angle_beta                 97.852(7)

_cell_angle_gamma                90.00

_cell_volume                     2237(2)

_cell_formula_units_Z            4

_cell_measurement_temperature    296(2)

_cell_measurement_reflns_used    5479

_cell_measurement_theta_min      2.1

_cell_measurement_theta_max      27.5


_exptl_crystal_description       Prism

_exptl_crystal_colour            Colorless

_exptl_crystal_size_max          0.19

_exptl_crystal_size_mid          0.17

_exptl_crystal_size_min          0.16

_exptl_crystal_density_meas      none

_exptl_crystal_density_diffrn    1.812

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             1240

_exptl_absorpt_coefficient_mu    1.557

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.7563

_exptl_absorpt_correction_T_max  0.7888

_exptl_absorpt_process_details   sadabs



_exptl_special_details           
;

 ?

;



_diffrn_ambient_temperature      296(2)

_diffrn_radiation_wavelength     0.71073

_diffrn_radiation_type           MoK\a

_diffrn_radiation_source         'fine-focus sealed tube'

_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker P4'

_diffrn_measurement_method       'ω scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            23097

_diffrn_reflns_av_R_equivalents  0.0675

_diffrn_reflns_av_sigmaI/netI    0.0503

_diffrn_reflns_limit_h_min       -18

_diffrn_reflns_limit_h_max       18

_diffrn_reflns_limit_k_min       -8

_diffrn_reflns_limit_k_max       8

_diffrn_reflns_limit_l_min       -31

_diffrn_reflns_limit_l_max       31

_diffrn_reflns_theta_min         2.85

_diffrn_reflns_theta_max         27.56

_reflns_number_total             5179

_reflns_number_gt                4285

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'Bruker XSCANS'

_computing_cell_refinement       'Bruker XSCANS'

_computing_data_reduction        'Bruker SHELXTL'

_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)+(0.0517P)²+1.0439P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct

_atom_sites_solution_secondary   difmap

_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    constr

_refine_ls_extinction_method     none

_refine_ls_extinction_coef       ?

_refine_ls_number_reflns         5179

_refine_ls_number_parameters     337

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0497

_refine_ls_R_factor_gt           0.0387

_refine_ls_wR_factor_ref         0.1080

_refine_ls_wR_factor_gt          0.1011

_refine_ls_goodness_of_fit_ref   1.030

_refine_ls_restrained_S_all      1.030

_refine_ls_shift/su_max          0.001

_refine_ls_shift/su_mean         0.000



loop_

_atom_site_label

_atom_site_type_symbol

_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z

_atom_site_U_iso_or_equiv

_atom_site_adp_type

_atom_site_occupancy

_atom_site_symmetry_multiplicity

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_assembly

_atom_site_disorder_group


























































Co1 Co 1.0000 -0.5000 0.5000 0.02212(13) Uani 1 2 d S . .
Co2 Co 0.5000 0.0000 0.5000 0.01569(12) Uani 1 2 d S . .
Co3 Co 0.39620(2) 0.49977(4) 0.475038(13) 0.01757(10) Uani 1 1 d . . .
O1 O 0.83652(16) -0.5734(3) 0.39062(8) 0.0396(5) Uani 1 1 d . . .
O2 O 0.87466(14) -0.3619(3) 0.46279(7) 0.0346(5) Uani 1 1 d . . .
O3 O 0.65134(12) -0.3758(2) 0.45327(7) 0.0253(4) Uani 1 1 d . . .
O4 O 0.62894(13) -0.0436(2) 0.47086(7) 0.0249(4) Uani 1 1 d . . .
O5 O 0.91373(17) -0.2384(3) 0.12186(9) 0.0480(6) Uani 1 1 d . . .
H5D H 0.9250 -0.2935 0.0928 0.072 Uiso 1 1 calc R . .
O6 O 0.94104(15) 0.0489(3) 0.07520(8) 0.0375(5) Uani 1 1 d . . .
O7 O 0.58430(14) 0.1274(3) 0.10215(7) 0.0291(4) Uani 1 1 d . . .
O8 O 0.56897(14) 0.4616(3) 0.08283(7) 0.0281(4) Uani 1 1 d . . .
O9 O 0.95103(14) -0.7791(3) 0.46730(8) 0.0344(4) Uani 1 1 d . . .
H9B H 0.9217 -0.8728 0.4822 0.052 Uiso 1 1 d R . .
H9A H 0.9069 -0.7419 0.4422 0.052 Uiso 1 1 d R . .
O10 O 0.51142(11) 0.3058(2) 0.47661(6) 0.0175(3) Uani 1 1 d . . .
H10D H 0.5290 0.3058 0.4385 0.026 Uiso 1 1 d R . .
O11 O 0.31000(13) 0.2869(3) 0.42131(8) 0.0335(4) Uani 1 1 d . . .
H11A H 0.3403 0.1779 0.4167 0.050 Uiso 1 1 d R . .
H11B H 0.2973 0.3450 0.3894 0.050 Uiso 1 1 d R . .
O12 O 0.27959(13) 0.7020(3) 0.48113(10) 0.0417(5) Uani 1 1 d . . .
H12B H 0.2997 0.7975 0.5037 0.063 Uiso 1 1 d R . .
H12A H 0.2457 0.6351 0.5011 0.063 Uiso 1 1 d R . .
O13 O 0.85991(16) 0.5465(3) 0.02995(9) 0.0439(5) Uani 1 1 d . . .
H13B H 0.8051 0.5188 0.0367 0.066 Uiso 1 1 d R . .
H13A H 0.8650 0.6240 0.0020 0.066 Uiso 1 1 d R . .
C1 C 0.83438(16) -0.4040(4) 0.41331(10) 0.0217(5) Uani 1 1 d . . .
C2 C 0.78599(16) -0.2294(3) 0.37955(9) 0.0190(4) Uani 1 1 d . . .
C3 C 0.70777(16) -0.1271(3) 0.39403(9) 0.0187(4) Uani 1 1 d . . .
C4 C 0.65958(15) -0.1885(3) 0.44324(9) 0.0182(4) Uani 1 1 d . . .
C5 C 0.66859(16) 0.0324(3) 0.35996(10) 0.0193(5) Uani 1 1 d . . .
H5 H 0.6157 0.0980 0.3694 0.023 Uiso 1 1 calc R . .
C6 C 0.70576(16) 0.0967(3) 0.31255(9) 0.0192(5) Uani 1 1 d . . .
C7 C 0.78860(17) 0.0040(3) 0.30051(10) 0.0205(5) Uani 1 1 d . . .
C8 C 0.82571(16) -0.1613(4) 0.33310(10) 0.0223(5) Uani 1 1 d . . .
H8 H 0.8783 -0.2277 0.3236 0.027 Uiso 1 1 calc R . .
C9 C 0.83983(17) 0.0929(4) 0.25594(10) 0.0226(5) Uani 1 1 d . . .
C10 C 0.85843(18) -0.0195(4) 0.20960(11) 0.0242(5) Uani 1 1 d . . .
H10 H 0.8423 -0.1574 0.2065 0.029 Uiso 1 1 calc R . .
C11 C 0.90148(17) 0.0751(4) 0.16757(10) 0.0243(5) Uani 1 1 d . . .
C12 C 0.92063(18) -0.0398(4) 0.11702(11) 0.0278(5) Uani 1 1 d . . .
C13 C 0.92647(18) 0.2803(4) 0.17222(11) 0.0283(5) Uani 1 1 d . . .
H13 H 0.9529 0.3440 0.1435 0.034 Uiso 1 1 calc R . .
C14 C 0.91202(19) 0.3896(4) 0.21959(11) 0.0311(6) Uani 1 1 d . . .
H14 H 0.9314 0.5252 0.2237 0.037 Uiso 1 1 calc R . .
C15 C 0.86845(18) 0.2965(4) 0.26109(11) 0.0284(5) Uani 1 1 d . . .
H15 H 0.8582 0.3711 0.2927 0.034 Uiso 1 1 calc R . .
C16 C 0.65770(16) 0.2546(3) 0.27403(9) 0.0195(5) Uani 1 1 d . . .
C17 C 0.63914(16) 0.2135(3) 0.21644(9) 0.0205(5) Uani 1 1 d . . .
H17 H 0.6529 0.0847 0.2032 0.025 Uiso 1 1 calc R . .
C18 C 0.60043(16) 0.3614(3) 0.17841(9) 0.0199(4) Uani 1 1 d . . .
C19 C 0.58310(16) 0.3117(3) 0.11645(9) 0.0200(5) Uani 1 1 d . . .
C20 C 0.57899(18) 0.5548(4) 0.19873(10) 0.0242(5) Uani 1 1 d . . .
H20 H 0.5553 0.6568 0.1737 0.029 Uiso 1 1 calc R . .
C21 C 0.59295(18) 0.5939(4) 0.25597(10) 0.0266(5) Uani 1 1 d . . .
H21 H 0.5762 0.7205 0.2693 0.032 Uiso 1 1 calc R . .
C22 C 0.63194(17) 0.4452(4) 0.29379(10) 0.0243(5) Uani 1 1 d . . .
H22 H 0.6409 0.4726 0.3322 0.029 Uiso 1 1 calc 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 2.069(2) 3_746 ?
Co1 O9 2.069(2) . ?
Co1 O2 2.108(2) 3_746 ?
Co1 O2 2.108(2) . ?
Co1 O6 2.120(2) 2_745 ?
Co1 O6 2.120(2) 4_556 ?
Co2 O10 2.0853(18) . ?
Co2 O10 2.0853(18) 3_656 ?
Co2 O4 2.0958(19) . ?
Co2 O4 2.0958(19) 3_656 ?
Co2 O8 2.110(2) 2_645 ?
Co2 O8 2.110(2) 4_566 ?
Co3 O10 2.0761(17) 3_666 ?
Co3 O7 2.0821(19) 2_655 ?
Co3 O10 2.0873(18) . ?
Co3 O3 2.0974(18) 3_656 ?
Co3 O12 2.160(2) . ?
Co3 O11 2.1678(19) . ?
O1 C1 1.234(3) . ?
O2 C1 1.277(3) . ?
O3 C4 1.255(3) . ?
O3 Co3 2.0974(18) 3_656 ?
O4 C4 1.268(3) . ?
O5 C12 1.307(3) . ?
O5 H5D 0.8200 . ?
O6 C12 1.227(3) . ?
O6 Co1 2.120(2) 2_755 ?
O7 C19 1.251(3) . ?
O7 Co3 2.0821(19) 2_645 ?
O8 C19 1.266(3) . ?
O8 Co2 2.110(2) 2_655 ?
O9 H9B 0.8500 . ?
O9 H9A 0.8499 . ?
O10 Co3 2.0761(17) 3_666 ?
O10 H10D 0.9800 . ?
O11 H11A 0.8500 . ?
O11 H11B 0.8502 . ?
O12 H12B 0.8499 . ?
O12 H12A 0.8500 . ?
O13 H13B 0.8499 . ?
O13 H13A 0.8501 . ?
C1 C2 1.512(3) . ?
C2 C8 1.393(3) . ?
C2 C3 1.396(3) . ?
C3 C5 1.395(3) . ?
C3 C4 1.503(3) . ?
C5 C6 1.386(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.405(3) . ?
C6 C16 1.490(3) . ?
C7 C8 1.395(3) . ?
C7 C9 1.497(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.387(3) . ?
C9 C15 1.392(4) . ?
C10 C11 1.397(3) . ?
C10 H10 0.9300 . ?
C11 C13 1.387(4) . ?
C11 C12 1.482(4) . ?
C13 C14 1.380(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.387(4) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.395(3) . ?
C16 C22 1.399(3) . ?
C17 C18 1.391(3) . ?
C17 H17 0.9300 . ?
C18 C20 1.402(3) . ?
C18 C19 1.506(3) . ?
C20 C21 1.382(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.393(3) . ?
C21 H21 0.9300 . ?
C22 H22 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






































































































































O9 Co1 O9 180.00(5) 3_746 . ?
O9 Co1 O2 89.24(8) 3_746 3_746 ?
O9 Co1 O2 90.76(8) . 3_746 ?
O9 Co1 O2 90.76(8) 3_746 . ?
O9 Co1 O2 89.24(8) . . ?
O2 Co1 O2 180.00(9) 3_746 . ?
O9 Co1 O6 91.89(8) 3_746 2_745 ?
O9 Co1 O6 88.11(8) . 2_745 ?
O2 Co1 O6 90.13(9) 3_746 2_745 ?
O2 Co1 O6 89.87(9) . 2_745 ?
O9 Co1 O6 88.11(8) 3_746 4_556 ?
O9 Co1 O6 91.89(8) . 4_556 ?
O2 Co1 O6 89.87(9) 3_746 4_556 ?
O2 Co1 O6 90.13(9) . 4_556 ?
O6 Co1 O6 180.000(1) 2_745 4_556 ?
O10 Co2 O10 180.00(2) . 3_656 ?
O10 Co2 O4 86.21(6) . . ?
O10 Co2 O4 93.79(6) 3_656 . ?
O10 Co2 O4 93.79(6) . 3_656 ?
O10 Co2 O4 86.21(6) 3_656 3_656 ?
O4 Co2 O4 180.00(9) . 3_656 ?
O10 Co2 O8 84.58(6) . 2_645 ?
O10 Co2 O8 95.42(6) 3_656 2_645 ?
O4 Co2 O8 89.85(8) . 2_645 ?
O4 Co2 O8 90.15(8) 3_656 2_645 ?
O10 Co2 O8 95.42(6) . 4_566 ?
O10 Co2 O8 84.58(6) 3_656 4_566 ?
O4 Co2 O8 90.15(8) . 4_566 ?
O4 Co2 O8 89.85(8) 3_656 4_566 ?
O8 Co2 O8 180.0 2_645 4_566 ?
O10 Co3 O7 95.53(7) 3_666 2_655 ?
O10 Co3 O10 84.87(7) 3_666 . ?
O7 Co3 O10 93.12(7) 2_655 . ?
O10 Co3 O3 92.08(7) 3_666 3_656 ?
O7 Co3 O3 168.77(7) 2_655 3_656 ?
O10 Co3 O3 95.78(7) . 3_656 ?
O10 Co3 O12 92.09(8) 3_666 . ?
O7 Co3 O12 90.97(8) 2_655 . ?
O10 Co3 O12 175.12(7) . . ?
O3 Co3 O12 80.49(8) 3_656 . ?
O10 Co3 O11 175.04(7) 3_666 . ?
O7 Co3 O11 82.26(8) 2_655 . ?
O10 Co3 O11 90.80(7) . . ?
O3 Co3 O11 90.76(8) 3_656 . ?
O12 Co3 O11 92.39(9) . . ?
C1 O2 Co1 123.83(16) . . ?
C4 O3 Co3 125.66(15) . 3_656 ?
C4 O4 Co2 131.65(15) . . ?
C12 O5 H5D 109.5 . . ?
C12 O6 Co1 142.4(2) . 2_755 ?
C19 O7 Co3 129.52(15) . 2_645 ?
C19 O8 Co2 134.79(16) . 2_655 ?
Co1 O9 H9B 129.6 . . ?
Co1 O9 H9A 101.6 . . ?
H9B O9 H9A 97.8 . . ?
Co3 O10 Co2 120.23(8) 3_666 . ?
Co3 O10 Co3 95.13(7) 3_666 . ?
Co2 O10 Co3 119.55(8) . . ?
Co3 O10 H10D 106.9 3_666 . ?
Co2 O10 H10D 106.9 . . ?
Co3 O10 H10D 106.9 . . ?
Co3 O11 H11A 110.5 . . ?
Co3 O11 H11B 106.5 . . ?
H11A O11 H11B 107.9 . . ?
Co3 O12 H12B 106.8 . . ?
Co3 O12 H12A 103.8 . . ?
H12B O12 H12A 101.1 . . ?
H13B O13 H13A 117.4 . . ?
O1 C1 O2 124.5(2) . . ?
O1 C1 C2 118.5(2) . . ?
O2 C1 C2 117.0(2) . . ?
C8 C2 C3 118.8(2) . . ?
C8 C2 C1 117.2(2) . . ?
C3 C2 C1 123.9(2) . . ?
C5 C3 C2 119.3(2) . . ?
C5 C3 C4 117.6(2) . . ?
C2 C3 C4 123.0(2) . . ?
O3 C4 O4 125.3(2) . . ?
O3 C4 C3 118.42(19) . . ?
O4 C4 C3 116.29(19) . . ?
C6 C5 C3 122.3(2) . . ?
C6 C5 H5 118.9 . . ?
C3 C5 H5 118.9 . . ?
C5 C6 C7 118.3(2) . . ?
C5 C6 C16 121.1(2) . . ?
C7 C6 C16 120.5(2) . . ?
C8 C7 C6 119.4(2) . . ?
C8 C7 C9 120.6(2) . . ?
C6 C7 C9 119.8(2) . . ?
C2 C8 C7 121.7(2) . . ?
C2 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C10 C9 C15 119.2(2) . . ?
C10 C9 C7 122.3(2) . . ?
C15 C9 C7 118.4(2) . . ?
C9 C10 C11 119.8(2) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C13 C11 C10 120.3(2) . . ?
C13 C11 C12 118.6(2) . . ?
C10 C11 C12 121.1(2) . . ?
O6 C12 O5 124.8(3) . . ?
O6 C12 C11 121.4(3) . . ?
O5 C12 C11 113.8(2) . . ?
C14 C13 C11 119.9(2) . . ?
C14 C13 H13 120.1 . . ?
C11 C13 H13 120.1 . . ?
C13 C14 C15 119.8(2) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C14 C15 C9 120.8(2) . . ?
C14 C15 H15 119.6 . . ?
C9 C15 H15 119.6 . . ?
C17 C16 C22 118.8(2) . . ?
C17 C16 C6 119.3(2) . . ?
C22 C16 C6 121.9(2) . . ?
C18 C17 C16 121.4(2) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C17 C18 C20 119.0(2) . . ?
C17 C18 C19 119.6(2) . . ?
C20 C18 C19 121.4(2) . . ?
O7 C19 O8 125.1(2) . . ?
O7 C19 C18 118.0(2) . . ?
O8 C19 C18 116.8(2) . . ?
C21 C20 C18 120.1(2) . . ?
C21 C20 H20 120.0 . . ?
C18 C20 H20 120.0 . . ?
C20 C21 C22 120.5(2) . . ?
C20 C21 H21 119.7 . . ?
C22 C21 H21 119.7 . . ?
C21 C22 C16 120.1(2) . . ?
C21 C22 H22 119.9 . . ?
C16 C22 H22 119.9 . . ?



loop_

_geom_torsion_atom_site_label_1

_geom_torsion_atom_site_label_2

_geom_torsion_atom_site_label_3

_geom_torsion_atom_site_label_4

_geom_torsion

_geom_torsion_site_symmetry_1

_geom_torsion_site_symmetry_2

_geom_torsion_site_symmetry_3

_geom_torsion_site_symmetry_4

_geom_torsion_publ_flag






































































































O9 Co1 O2 C1 138.5(2) 3_746 . . . ?
O9 Co1 O2 C1 -41.5(2) . . . . ?
O2 Co1 O2 C1 -74(100) 3_746 . . . ?
O6 Co1 O2 C1 46.6(2) 2_745 . . . ?
O6 Co1 O2 C1 -133.4(2) 4_556 . . . ?
O10 Co2 O4 C4 -140.0(2) . . . . ?
O10 Co2 O4 C4 40.0(2) 3_656 . . . ?
O4 Co2 O4 C4 -43(100) 3_656 . . . ?
O8 Co2 O4 C4 -55.4(2) 2_645 . . . ?
O8 Co2 O4 C4 124.6(2) 4_566 . . . ?
O10 Co2 O10 Co3 143(100) 3_656 . . 3_666 ?
O4 Co2 O10 Co3 -74.50(9) . . . 3_666 ?
O4 Co2 O10 Co3 105.50(9) 3_656 . . 3_666 ?
O8 Co2 O10 Co3 -164.71(9) 2_645 . . 3_666 ?
O8 Co2 O10 Co3 15.29(9) 4_566 . . 3_666 ?
O10 Co2 O10 Co3 27(100) 3_656 . . . ?
O4 Co2 O10 Co3 168.81(9) . . . . ?
O4 Co2 O10 Co3 -11.19(9) 3_656 . . . ?
O8 Co2 O10 Co3 78.60(9) 2_645 . . . ?
O8 Co2 O10 Co3 -101.40(9) 4_566 . . . ?
O10 Co3 O10 Co3 0.0 3_666 . . 3_666 ?
O7 Co3 O10 Co3 95.28(7) 2_655 . . 3_666 ?
O3 Co3 O10 Co3 -91.58(7) 3_656 . . 3_666 ?
O12 Co3 O10 Co3 -51.6(8) . . . 3_666 ?
O11 Co3 O10 Co3 177.58(7) . . . 3_666 ?
O10 Co3 O10 Co2 129.19(11) 3_666 . . . ?
O7 Co3 O10 Co2 -135.53(8) 2_655 . . . ?
O3 Co3 O10 Co2 37.61(9) 3_656 . . . ?
O12 Co3 O10 Co2 77.5(8) . . . . ?
O11 Co3 O10 Co2 -53.24(9) . . . . ?
Co1 O2 C1 O1 31.6(4) . . . . ?
Co1 O2 C1 C2 -144.59(17) . . . . ?
O1 C1 C2 C8 -65.7(3) . . . . ?
O2 C1 C2 C8 110.7(3) . . . . ?
O1 C1 C2 C3 117.9(3) . . . . ?
O2 C1 C2 C3 -65.7(3) . . . . ?
C8 C2 C3 C5 3.5(3) . . . . ?
C1 C2 C3 C5 179.9(2) . . . . ?
C8 C2 C3 C4 179.9(2) . . . . ?
C1 C2 C3 C4 -3.8(4) . . . . ?
Co3 O3 C4 O4 -10.0(3) 3_656 . . . ?
Co3 O3 C4 C3 171.24(15) 3_656 . . . ?
Co2 O4 C4 O3 -45.6(3) . . . . ?
Co2 O4 C4 C3 133.21(18) . . . . ?
C5 C3 C4 O3 137.8(2) . . . . ?
C2 C3 C4 O3 -38.6(3) . . . . ?
C5 C3 C4 O4 -41.0(3) . . . . ?
C2 C3 C4 O4 142.5(2) . . . . ?
C2 C3 C5 C6 -1.4(4) . . . . ?
C4 C3 C5 C6 -177.9(2) . . . . ?
C3 C5 C6 C7 -3.4(3) . . . . ?
C3 C5 C6 C16 174.4(2) . . . . ?
C5 C6 C7 C8 6.0(3) . . . . ?
C16 C6 C7 C8 -171.9(2) . . . . ?
C5 C6 C7 C9 -169.4(2) . . . . ?
C16 C6 C7 C9 12.7(3) . . . . ?
C3 C2 C8 C7 -0.9(4) . . . . ?
C1 C2 C8 C7 -177.5(2) . . . . ?
C6 C7 C8 C2 -4.0(4) . . . . ?
C9 C7 C8 C2 171.4(2) . . . . ?
C8 C7 C9 C10 62.6(3) . . . . ?
C6 C7 C9 C10 -122.1(3) . . . . ?
C8 C7 C9 C15 -118.3(3) . . . . ?
C6 C7 C9 C15 57.0(3) . . . . ?
C15 C9 C10 C11 -3.0(4) . . . . ?
C7 C9 C10 C11 176.1(2) . . . . ?
C9 C10 C11 C13 0.6(4) . . . . ?
C9 C10 C11 C12 -178.8(2) . . . . ?
Co1 O6 C12 O5 -16.4(5) 2_755 . . . ?
Co1 O6 C12 C11 163.5(2) 2_755 . . . ?
C13 C11 C12 O6 -13.9(4) . . . . ?
C10 C11 C12 O6 165.5(3) . . . . ?
C13 C11 C12 O5 166.0(2) . . . . ?
C10 C11 C12 O5 -14.6(4) . . . . ?
C10 C11 C13 C14 2.5(4) . . . . ?
C12 C11 C13 C14 -178.1(2) . . . . ?
C11 C13 C14 C15 -3.1(4) . . . . ?
C13 C14 C15 C9 0.7(4) . . . . ?
C10 C9 C15 C14 2.4(4) . . . . ?
C7 C9 C15 C14 -176.8(2) . . . . ?
C5 C6 C16 C17 -127.6(2) . . . . ?
C7 C6 C16 C17 50.2(3) . . . . ?
C5 C6 C16 C22 53.5(3) . . . . ?
C7 C6 C16 C22 -128.7(3) . . . . ?
C22 C16 C17 C18 3.5(4) . . . . ?
C6 C16 C17 C18 -175.4(2) . . . . ?
C16 C17 C18 C20 -0.6(4) . . . . ?
C16 C17 C18 C19 178.9(2) . . . . ?
Co3 O7 C19 O8 20.0(4) 2_645 . . . ?
Co3 O7 C19 C18 -159.48(16) 2_645 . . . ?
Co2 O8 C19 O7 24.9(4) 2_655 . . . ?
Co2 O8 C19 C18 -155.57(17) 2_655 . . . ?
C17 C18 C19 O7 15.7(3) . . . . ?
C20 C18 C19 O7 -164.8(2) . . . . ?
C17 C18 C19 O8 -163.9(2) . . . . ?
C20 C18 C19 O8 15.6(3) . . . . ?
C17 C18 C20 C21 -2.5(4) . . . . ?
C19 C18 C20 C21 178.0(2) . . . . ?
C18 C20 C21 C22 2.7(4) . . . . ?
C20 C21 C22 C16 0.3(4) . . . . ?
C17 C16 C22 C21 -3.3(4) . . . . ?
C6 C16 C22 C21 175.6(2) . . . . ?



_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        27.56

_diffrn_measured_fraction_theta_full 0.998

_refine_diff_density_max         0.660

_refine_diff_density_min         -0.576

_refine_diff_density_rms         0.078

_database_code_depnum_ccdc_archive 'CCDC 1010216'
#######################################################################
#
#                 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            
'C32 H25 N3 Ni2 O11'

_chemical_formula_weight         744.97



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           Monoclinic

_symmetry_space_group_name_H-M   P21/c



loop_

_symmetry_equiv_pos_as_xyz




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



_cell_length_a                   15.896(7)

_cell_length_b                   7.823(3)

_cell_length_c                   23.210(10)

_cell_angle_alpha                90.00

_cell_angle_beta                 92.895(7)

_cell_angle_gamma                90.00

_cell_volume                     2883(2)

_cell_formula_units_Z            4

_cell_measurement_temperature    296(2)

_cell_measurement_reflns_used    8039

_cell_measurement_theta_min      2.1

_cell_measurement_theta_max      27.5



_exptl_crystal_description       prism

_exptl_crystal_colour            green

_exptl_crystal_size_max          0.21

_exptl_crystal_size_mid          0.19

_exptl_crystal_size_min          0.16

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.717

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             1528

_exptl_absorpt_coefficient_mu    1.379

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.7605

_exptl_absorpt_correction_T_max  0.8095

_exptl_absorpt_process_details   SADABS



_exptl_special_details           
;

 ?

;



_diffrn_ambient_temperature      296(2)

_diffrn_radiation_wavelength     0.71073

_diffrn_radiation_type           MoK\a

_diffrn_radiation_source         'fine-focus sealed tube'

_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker P4'

_diffrn_measurement_method       'ω scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            29630

_diffrn_reflns_av_R_equivalents  0.0722

_diffrn_reflns_av_unetI/netI     0.0449

_diffrn_reflns_limit_h_min       -20

_diffrn_reflns_limit_h_max       20

_diffrn_reflns_limit_k_min       -10

_diffrn_reflns_limit_k_max       10

_diffrn_reflns_limit_l_min       -30

_diffrn_reflns_limit_l_max       30

_diffrn_reflns_theta_min         1.76

_diffrn_reflns_theta_max         27.55

_reflns_number_total             6618

_reflns_number_gt                5898

_reflns_threshold_expression     >2sigma(I)



_computing_data_collection       'Bruker XSCANS'

_computing_cell_refinement       'Bruker XSCANS'

_computing_data_reduction        'Bruker SHELXTL'

_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)+(0.0725P)²+2.9964P] 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         6618

_refine_ls_number_parameters     442

_refine_ls_number_restraints     9

_refine_ls_R_factor_all          0.0504

_refine_ls_R_factor_gt           0.0446

_refine_ls_wR_factor_ref         0.1325

_refine_ls_wR_factor_gt          0.1273

_refine_ls_goodness_of_fit_ref   1.066

_refine_ls_restrained_S_all      1.073

_refine_ls_shift/su_max          0.000

_refine_ls_shift/su_mean         0.000



loop_

_atom_site_label

_atom_site_type_symbol

_atom_site_fract_x

_atom_site_fract_y

_atom_site_fract_z

_atom_site_U_iso_or_equiv

_atom_site_adp_type

_atom_site_occupancy

_atom_site_symmetry_multiplicity

_atom_site_calc_flag

_atom_site_refinement_flags

_atom_site_disorder_assembly

_atom_site_disorder_group










































































Ni1 Ni 0.5000 1.0000 0.5000 0.01605(12) Uani 1 2 d S . .
Ni2 Ni 0.25010(2) 0.56884(5) 0.466433(14) 0.02128(11) Uani 1 1 d . . .
Ni3 Ni 0.0000 1.0000 0.5000 0.01632(12) Uani 1 2 d S . .
O1 O 0.40383(12) 0.9933(3) 0.43835(9) 0.0247(4) Uani 1 1 d . . .
O2 O 0.33747(13) 0.7576(3) 0.46241(9) 0.0300(5) Uani 1 1 d . . .
O3 O 0.15448(12) 0.7430(3) 0.45830(8) 0.0258(4) Uani 1 1 d . . .
O4 O 0.10595(13) 1.0112(3) 0.45034(9) 0.0251(4) Uani 1 1 d . . .
O5 O 0.08661(14) 1.4756(3) 0.13568(9) 0.0278(4) Uani 1 1 d . . .
O6 O 0.05166(13) 1.3214(3) 0.05651(8) 0.0264(4) Uani 1 1 d . . .
O7 O 0.25004(13) 0.9038(3) 0.05534(9) 0.0286(4) Uani 1 1 d . . .
O8 O 0.35053(13) 1.0555(3) 0.01877(8) 0.0274(4) Uani 1 1 d . . .
O9 O 0.49269(12) 1.2681(3) 0.49129(9) 0.0270(4) Uani 1 1 d D . .
H9A H 0.5378 1.3109 0.5023 0.040 Uiso 1 1 calc RD . .
H9B H 0.4506(7) 1.318(4) 0.5048(15) 0.040 Uiso 1 1 d D . .
O10 O 0.16146(17) 0.3664(3) 0.47545(11) 0.0415(6) Uani 1 1 d D . .
H10A H 0.1462 0.3645 0.5087 0.062 Uiso 1 1 d RD . .
H10C H 0.155(3) 0.272(3) 0.4580(10) 0.062 Uiso 1 1 d D . .
O11 O -0.04912(13) 1.2001(3) 0.45293(8) 0.0257(4) Uani 1 1 d D . .
H11A H -0.0667 1.1657 0.4212 0.038 Uiso 1 1 d RD . .
H11C H -0.0974 1.2298 0.4690 0.038 Uiso 1 1 d RD . .
N1 N 0.26051(16) 0.5049(3) 0.38084(10) 0.0252(5) Uani 1 1 d . . .
N2 N 0.24655(16) 0.5347(3) 0.19975(10) 0.0270(5) Uani 1 1 d . . .
H2A H 0.1955 0.5491 0.1865 0.032 Uiso 1 1 calc R . .
N3 N 0.41721(15) 0.5138(3) 0.06723(10) 0.0212(5) Uani 1 1 d . . .
C1 C 0.34650(16) 0.8869(4) 0.43072(11) 0.0197(5) Uani 1 1 d . . .
C2 C 0.28660(15) 0.9211(3) 0.37952(10) 0.0178(5) Uani 1 1 d . . .
C3 C 0.19852(16) 0.9214(3) 0.38128(11) 0.0180(5) Uani 1 1 d . . .
C4 C 0.15090(16) 0.8885(3) 0.43475(11) 0.0191(5) Uani 1 1 d . . .
C5 C 0.15069(16) 0.9573(4) 0.33097(11) 0.0209(5) Uani 1 1 d . . .
H5A H 0.0923 0.9594 0.3323 0.025 Uiso 1 1 calc R . .
C6 C 0.18677(16) 0.9905(3) 0.27844(11) 0.0194(5) Uani 1 1 d . . .
C7 C 0.27607(17) 0.9970(3) 0.27668(11) 0.0180(5) Uani 1 1 d . . .
C8 C 0.32243(16) 0.9623(4) 0.32798(11) 0.0208(5) Uani 1 1 d . . .
H8A H 0.3809 0.9672 0.3276 0.025 Uiso 1 1 calc R . .
C9 C 0.12801(16) 1.0119(3) 0.22700(11) 0.0197(5) Uani 1 1 d . . .
C10 C 0.07322(18) 0.8799(4) 0.21101(12) 0.0255(6) Uani 1 1 d . . .
H10B H 0.0707 0.7833 0.2342 0.031 Uiso 1 1 calc R . .
C11 C 0.02207(19) 0.8905(4) 0.16080(13) 0.0273(6) Uani 1 1 d . . .
H11B H -0.0134 0.8003 0.1500 0.033 Uiso 1 1 calc R . .
C12 C 0.02418(18) 1.0367(4) 0.12670(12) 0.0253(6) Uani 1 1 d . . .
H12A H -0.0077 1.0420 0.0920 0.030 Uiso 1 1 calc R . .
C13 C 0.07399(16) 1.1743(4) 0.14451(11) 0.0203(5) Uani 1 1 d . . .
C14 C 0.12588(16) 1.1614(3) 0.19460(11) 0.0208(5) Uani 1 1 d . . .
H14A H 0.1594 1.2536 0.2064 0.025 Uiso 1 1 calc R . .
C15 C 0.07086(16) 1.3375(4) 0.11005(11) 0.0211(5) Uani 1 1 d . . .
C16 C 0.32444(17) 1.0395(4) 0.22495(11) 0.0196(5) Uani 1 1 d . . .
C17 C 0.29973(18) 0.9899(3) 0.16876(11) 0.0202(5) Uani 1 1 d . . .
H17A H 0.2506 0.9268 0.1622 0.024 Uiso 1 1 calc R . .
C18 C 0.34781(17) 1.0338(4) 0.12234(11) 0.0213(5) Uani 1 1 d . . .
C19 C 0.42410(17) 1.1200(4) 0.13173(12) 0.0258(6) Uani 1 1 d . . .
H19A H 0.4572 1.1453 0.1010 0.031 Uiso 1 1 calc R . .
C20 C 0.45012(18) 1.1676(4) 0.18749(12) 0.0285(6) Uani 1 1 d . . .
H20A H 0.5009 1.2248 0.1942 0.034 Uiso 1 1 calc R . .
C21 C 0.40038(18) 1.1297(4) 0.23307(11) 0.0248(6) Uani 1 1 d . . .
H21A H 0.4178 1.1650 0.2700 0.030 Uiso 1 1 calc R . .
C22 C 0.31524(18) 0.9936(4) 0.06255(12) 0.0226(5) Uani 1 1 d . . .
C23 C 0.18823(19) 0.5054(4) 0.34900(13) 0.0268(6) Uani 1 1 d . . .
H23A H 0.1383 0.5002 0.3681 0.032 Uiso 1 1 calc R . .
C24 C 0.18269(18) 0.5132(4) 0.28968(12) 0.0258(6) Uani 1 1 d . . .
H24A H 0.1302 0.5135 0.2700 0.031 Uiso 1 1 calc R . .
C25 C 0.25598(18) 0.5205(4) 0.25908(12) 0.0231(5) Uani 1 1 d . . .
C26 C 0.33236(19) 0.5089(4) 0.29180(13) 0.0272(6) Uani 1 1 d . . .
H26A H 0.3832 0.5060 0.2737 0.033 Uiso 1 1 calc R . .
C27 C 0.33119(19) 0.5020(4) 0.35102(13) 0.0292(6) Uani 1 1 d . . .
H27A H 0.3826 0.4949 0.3719 0.035 Uiso 1 1 calc R . .
C28 C 0.30654(18) 0.5295(4) 0.15783(12) 0.0235(5) Uani 1 1 d . . .
C29 C 0.28263(18) 0.4564(4) 0.10464(13) 0.0276(6) Uani 1 1 d . . .
H29A H 0.2288 0.4115 0.0984 0.033 Uiso 1 1 calc R . .
C30 C 0.33838(18) 0.4509(4) 0.06165(12) 0.0250(6) Uani 1 1 d . . .
H30A H 0.3209 0.4011 0.0267 0.030 Uiso 1 1 calc R . .
C31 C 0.43911(17) 0.5902(4) 0.11775(12) 0.0244(6) Uani 1 1 d . . .
H31A H 0.4924 0.6391 0.1221 0.029 Uiso 1 1 calc R . .
C32 C 0.38698(18) 0.6002(4) 0.16349(12) 0.0265(6) Uani 1 1 d . . .
H32A H 0.4054 0.6534 0.1977 0.032 Uiso 1 1 calc R . .






_geom_special_details            
;

 All esds (except the esd in the dihedral angle between two l.s. planes)

 are estimated using the full covariance matrix.  The cell esds are taken

 into account individually in the estimation of esds in distances, angles

 and torsion angles; correlations between esds in cell parameters are only

 used when they are defined by crystal symmetry.  An approximate (isotropic)

 treatment of cell esds is used for estimating esds involving l.s. planes.

;



loop_

_geom_bond_atom_site_label_1

_geom_bond_atom_site_label_2

_geom_bond_distance

_geom_bond_site_symmetry_2

_geom_bond_publ_flag































































































Ni1 O1 2.041(2) 3_676 ?
Ni1 O1 2.041(2) . ?
Ni1 N3 2.094(2) 4_576 ?
Ni1 N3 2.094(2) 2_655 ?
Ni1 O9 2.110(2) 3_676 ?
Ni1 O9 2.110(2) . ?
Ni2 O2 2.032(2) . ?
Ni2 O3 2.043(2) . ?
Ni2 N1 2.063(2) . ?
Ni2 O7 2.075(2) 4_576 ?
Ni2 O10 2.137(2) . ?
Ni2 O8 2.185(2) 4_576 ?
Ni2 C22 2.460(3) 4_576 ?
Ni3 O11 2.041(2) 3_576 ?
Ni3 O11 2.041(2) . ?
Ni3 O6 2.059(2) 4_586 ?
Ni3 O6 2.059(2) 2_545 ?
Ni3 O4 2.090(2) 3_576 ?
Ni3 O4 2.090(2) . ?
O1 C1 1.241(3) . ?
O2 C1 1.263(3) . ?
O3 C4 1.263(3) . ?
O4 C4 1.260(3) . ?
O5 C15 1.252(4) . ?
O6 C15 1.271(3) . ?
O6 Ni3 2.059(2) 2 ?
O7 C22 1.256(4) . ?
O7 Ni2 2.075(2) 4_575 ?
O8 C22 1.280(3) . ?
O8 Ni2 2.185(2) 4_575 ?
O9 H9A 0.8200 . ?
O9 H9B 0.847(10) . ?
O10 H10A 0.8200 . ?
O10 H10C 0.844(10) . ?
O11 H11A 0.8201 . ?
O11 H11C 0.9010 . ?
N1 C23 1.334(4) . ?
N1 C27 1.349(4) . ?
N2 C25 1.382(4) . ?
N2 C28 1.397(4) . ?
N2 H2A 0.8600 . ?
N3 C31 1.346(4) . ?
N3 C30 1.346(4) . ?
N3 Ni1 2.094(2) 2_645 ?
C1 C2 1.509(3) . ?
C2 C8 1.389(4) . ?
C2 C3 1.403(3) . ?
C3 C5 1.389(4) . ?
C3 C4 1.508(3) . ?
C5 C6 1.398(4) . ?
C5 H5A 0.9300 . ?
C6 C7 1.423(4) . ?
C6 C9 1.488(4) . ?
C7 C8 1.395(4) . ?
C7 C16 1.495(4) . ?
C8 H8A 0.9300 . ?
C9 C10 1.389(4) . ?
C9 C14 1.390(4) . ?
C10 C11 1.389(4) . ?
C10 H10B 0.9300 . ?
C11 C12 1.392(4) . ?
C11 H11B 0.9300 . ?
C12 C13 1.387(4) . ?
C12 H12A 0.9300 . ?
C13 C14 1.395(4) . ?
C13 C15 1.506(4) . ?
C14 H14A 0.9300 . ?
C16 C21 1.403(4) . ?
C16 C17 1.398(4) . ?
C17 C18 1.395(4) . ?
C17 H17A 0.9300 . ?
C18 C19 1.395(4) . ?
C18 C22 1.490(4) . ?
C19 C20 1.389(4) . ?
C19 H19A 0.9300 . ?
C20 C21 1.384(4) . ?
C20 H20A 0.9300 . ?
C21 H21A 0.9300 . ?
C22 Ni2 2.460(3) 4_575 ?
C23 C24 1.376(4) . ?
C23 H23A 0.9300 . ?
C24 C25 1.396(4) . ?
C24 H24A 0.9300 . ?
C25 C26 1.402(4) . ?
C26 C27 1.377(4) . ?
C26 H26A 0.9300 . ?
C27 H27A 0.9300 . ?
C28 C32 1.393(4) . ?
C28 C29 1.396(4) . ?
C29 C30 1.368(4) . ?
C29 H29A 0.9300 . ?
C30 H30A 0.9300 . ?
C31 C32 1.381(4) . ?
C31 H31A 0.9300 . ?
C32 H32A 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















































































































































































O1 Ni1 O1 180.0 3_676 . ?
O1 Ni1 N3 87.46(9) 3_676 4_576 ?
O1 Ni1 N3 92.54(9) . 4_576 ?
O1 Ni1 N3 92.54(10) 3_676 2_655 ?
O1 Ni1 N3 87.46(9) . 2_655 ?
N3 Ni1 N3 180.000(1) 4_576 2_655 ?
O1 Ni1 O9 85.56(8) 3_676 3_676 ?
O1 Ni1 O9 94.44(8) . 3_676 ?
N3 Ni1 O9 84.90(8) 4_576 3_676 ?
N3 Ni1 O9 95.10(8) 2_655 3_676 ?
O1 Ni1 O9 94.44(8) 3_676 . ?
O1 Ni1 O9 85.56(8) . . ?
N3 Ni1 O9 95.10(8) 4_576 . ?
N3 Ni1 O9 84.90(8) 2_655 . ?
O9 Ni1 O9 180.000(1) 3_676 . ?
O2 Ni2 O3 91.04(10) . . ?
O2 Ni2 N1 92.51(9) . . ?
O3 Ni2 N1 99.69(9) . . ?
O2 Ni2 O7 90.31(9) . 4_576 ?
O3 Ni2 O7 89.16(8) . 4_576 ?
N1 Ni2 O7 170.66(9) . 4_576 ?
O2 Ni2 O10 176.68(9) . . ?
O3 Ni2 O10 90.70(10) . . ?
N1 Ni2 O10 89.99(10) . . ?
O7 Ni2 O10 86.89(9) 4_576 . ?
O2 Ni2 O8 82.36(9) . 4_576 ?
O3 Ni2 O8 150.18(8) . 4_576 ?
N1 Ni2 O8 109.60(9) . 4_576 ?
O7 Ni2 O8 61.97(8) 4_576 4_576 ?
O10 Ni2 O8 94.73(10) . 4_576 ?
O2 Ni2 C22 85.90(9) . 4_576 ?
O3 Ni2 C22 119.55(9) . 4_576 ?
N1 Ni2 C22 140.74(10) . 4_576 ?
O7 Ni2 C22 30.68(9) 4_576 4_576 ?
O10 Ni2 C22 90.78(10) . 4_576 ?
O8 Ni2 C22 31.29(8) 4_576 4_576 ?
O11 Ni3 O11 180.00(9) 3_576 . ?
O11 Ni3 O6 92.86(9) 3_576 4_586 ?
O11 Ni3 O6 87.14(9) . 4_586 ?
O11 Ni3 O6 87.14(9) 3_576 2_545 ?
O11 Ni3 O6 92.86(9) . 2_545 ?
O6 Ni3 O6 180.0 4_586 2_545 ?
O11 Ni3 O4 88.27(8) 3_576 3_576 ?
O11 Ni3 O4 91.73(8) . 3_576 ?
O6 Ni3 O4 89.06(9) 4_586 3_576 ?
O6 Ni3 O4 90.94(9) 2_545 3_576 ?
O11 Ni3 O4 91.73(8) 3_576 . ?
O11 Ni3 O4 88.27(8) . . ?
O6 Ni3 O4 90.94(9) 4_586 . ?
O6 Ni3 O4 89.06(9) 2_545 . ?
O4 Ni3 O4 180.00(9) 3_576 . ?
C1 O1 Ni1 129.50(18) . . ?
C1 O2 Ni2 134.95(18) . . ?
C4 O3 Ni2 131.17(18) . . ?
C4 O4 Ni3 127.65(18) . . ?
C15 O6 Ni3 128.61(18) . 2 ?
C22 O7 Ni2 91.88(16) . 4_575 ?
C22 O8 Ni2 86.31(17) . 4_575 ?
Ni1 O9 H9A 109.5 . . ?
Ni1 O9 H9B 117(2) . . ?
H9A O9 H9B 113.0 . . ?
Ni2 O10 H10A 109.5 . . ?
Ni2 O10 H10C 131(2) . . ?
H10A O10 H10C 113.8 . . ?
Ni3 O11 H11A 109.5 . . ?
Ni3 O11 H11C 106.7 . . ?
H11A O11 H11C 101.4 . . ?
C23 N1 C27 115.6(3) . . ?
C23 N1 Ni2 115.08(19) . . ?
C27 N1 Ni2 127.4(2) . . ?
C25 N2 C28 130.4(3) . . ?
C25 N2 H2A 114.8 . . ?
C28 N2 H2A 114.8 . . ?
C31 N3 C30 116.4(2) . . ?
C31 N3 Ni1 121.81(19) . 2_645 ?
C30 N3 Ni1 121.77(19) . 2_645 ?
O1 C1 O2 124.0(2) . . ?
O1 C1 C2 115.0(2) . . ?
O2 C1 C2 121.0(2) . . ?
C8 C2 C3 118.6(2) . . ?
C8 C2 C1 116.7(2) . . ?
C3 C2 C1 124.7(2) . . ?
C5 C3 C2 118.7(2) . . ?
C5 C3 C4 116.7(2) . . ?
C2 C3 C4 124.5(2) . . ?
O4 C4 O3 125.2(2) . . ?
O4 C4 C3 115.0(2) . . ?
O3 C4 C3 119.8(2) . . ?
C3 C5 C6 122.6(2) . . ?
C3 C5 H5A 118.7 . . ?
C6 C5 H5A 118.7 . . ?
C5 C6 C7 119.1(2) . . ?
C5 C6 C9 116.9(2) . . ?
C7 C6 C9 124.0(2) . . ?
C8 C7 C6 117.0(2) . . ?
C8 C7 C16 117.2(2) . . ?
C6 C7 C16 125.8(2) . . ?
C2 C8 C7 124.0(2) . . ?
C2 C8 H8A 118.0 . . ?
C7 C8 H8A 118.0 . . ?
C10 C9 C14 118.9(2) . . ?
C10 C9 C6 119.4(2) . . ?
C14 C9 C6 121.8(2) . . ?
C9 C10 C11 120.8(3) . . ?
C9 C10 H10B 119.6 . . ?
C11 C10 H10B 119.6 . . ?
C10 C11 C12 119.7(3) . . ?
C10 C11 H11B 120.1 . . ?
C12 C11 H11B 120.1 . . ?
C13 C12 C11 119.9(3) . . ?
C13 C12 H12A 120.1 . . ?
C11 C12 H12A 120.1 . . ?
C12 C13 C14 119.8(2) . . ?
C12 C13 C15 119.8(2) . . ?
C14 C13 C15 120.4(2) . . ?
C9 C14 C13 120.6(3) . . ?
C9 C14 H14A 119.7 . . ?
C13 C14 H14A 119.7 . . ?
O5 C15 O6 125.6(2) . . ?
O5 C15 C13 118.6(2) . . ?
O6 C15 C13 115.8(2) . . ?
C21 C16 C17 117.7(2) . . ?
C21 C16 C7 118.6(2) . . ?
C17 C16 C7 123.8(2) . . ?
C18 C17 C16 120.9(3) . . ?
C18 C17 H17A 119.6 . . ?
C16 C17 H17A 119.6 . . ?
C17 C18 C19 120.3(2) . . ?
C17 C18 C22 119.3(2) . . ?
C19 C18 C22 120.4(2) . . ?
C20 C19 C18 119.4(2) . . ?
C20 C19 H19A 120.3 . . ?
C18 C19 H19A 120.3 . . ?
C21 C20 C19 120.0(3) . . ?
C21 C20 H20A 120.0 . . ?
C19 C20 H20A 120.0 . . ?
C20 C21 C16 121.7(3) . . ?
C20 C21 H21A 119.1 . . ?
C16 C21 H21A 119.1 . . ?
O7 C22 O8 119.8(3) . . ?
O7 C22 C18 119.2(2) . . ?
O8 C22 C18 120.9(3) . . ?
O7 C22 Ni2 57.44(14) . 4_575 ?
O8 C22 Ni2 62.41(15) . 4_575 ?
C18 C22 Ni2 175.4(2) . 4_575 ?
N1 C23 C24 124.3(3) . . ?
N1 C23 H23A 117.8 . . ?
C24 C23 H23A 117.8 . . ?
C23 C24 C25 119.9(3) . . ?
C23 C24 H24A 120.1 . . ?
C25 C24 H24A 120.1 . . ?
N2 C25 C24 117.3(3) . . ?
N2 C25 C26 126.3(3) . . ?
C24 C25 C26 116.4(3) . . ?
C27 C26 C25 119.2(3) . . ?
C27 C26 H26A 120.4 . . ?
C25 C26 H26A 120.4 . . ?
N1 C27 C26 124.4(3) . . ?
N1 C27 H27A 117.8 . . ?
C26 C27 H27A 117.8 . . ?
C32 C28 N2 125.3(3) . . ?
C32 C28 C29 117.0(3) . . ?
N2 C28 C29 117.6(3) . . ?
C30 C29 C28 120.0(3) . . ?
C30 C29 H29A 120.0 . . ?
C28 C29 H29A 120.0 . . ?
N3 C30 C29 123.5(3) . . ?
N3 C30 H30A 118.2 . . ?
C29 C30 H30A 118.2 . . ?
N3 C31 C32 123.7(3) . . ?
N3 C31 H31A 118.1 . . ?
C32 C31 H31A 118.1 . . ?
C31 C32 C28 119.2(3) . . ?
C31 C32 H32A 120.4 . . ?
C28 C32 H32A 120.4 . . ?



loop_

_geom_torsion_atom_site_label_1

_geom_torsion_atom_site_label_2

_geom_torsion_atom_site_label_3

_geom_torsion_atom_site_label_4

_geom_torsion

_geom_torsion_site_symmetry_1

_geom_torsion_site_symmetry_2

_geom_torsion_site_symmetry_3

_geom_torsion_site_symmetry_4

_geom_torsion_publ_flag






































































































































O1 Ni1 O1 C1 -37(100) 3_676 . . . ?
N3 Ni1 O1 C1 -55.1(2) 4_576 . . . ?
N3 Ni1 O1 C1 124.9(2) 2_655 . . . ?
O9 Ni1 O1 C1 30.0(2) 3_676 . . . ?
O9 Ni1 O1 C1 -150.0(2) . . . . ?
O3 Ni2 O2 C1 -45.6(3) . . . . ?
N1 Ni2 O2 C1 54.1(3) . . . . ?
O7 Ni2 O2 C1 -134.8(3) 4_576 . . . ?
O10 Ni2 O2 C1 -167.3(16) . . . . ?
O8 Ni2 O2 C1 163.6(3) 4_576 . . . ?
C22 Ni2 O2 C1 -165.2(3) 4_576 . . . ?
O2 Ni2 O3 C4 27.0(2) . . . . ?
N1 Ni2 O3 C4 -65.8(2) . . . . ?
O7 Ni2 O3 C4 117.3(2) 4_576 . . . ?
O10 Ni2 O3 C4 -155.9(2) . . . . ?
O8 Ni2 O3 C4 103.3(3) 4_576 . . . ?
C22 Ni2 O3 C4 112.8(2) 4_576 . . . ?
O11 Ni3 O4 C4 34.1(2) 3_576 . . . ?
O11 Ni3 O4 C4 -145.9(2) . . . . ?
O6 Ni3 O4 C4 127.0(2) 4_586 . . . ?
O6 Ni3 O4 C4 -53.0(2) 2_545 . . . ?
O4 Ni3 O4 C4 -95(3) 3_576 . . . ?
O2 Ni2 N1 C23 -125.5(2) . . . . ?
O3 Ni2 N1 C23 -34.0(2) . . . . ?
O7 Ni2 N1 C23 127.1(6) 4_576 . . . ?
O10 Ni2 N1 C23 56.7(2) . . . . ?
O8 Ni2 N1 C23 151.8(2) 4_576 . . . ?
C22 Ni2 N1 C23 148.0(2) 4_576 . . . ?
O2 Ni2 N1 C27 37.9(3) . . . . ?
O3 Ni2 N1 C27 129.3(3) . . . . ?
O7 Ni2 N1 C27 -69.5(7) 4_576 . . . ?
O10 Ni2 N1 C27 -139.9(3) . . . . ?
O8 Ni2 N1 C27 -44.9(3) 4_576 . . . ?
C22 Ni2 N1 C27 -48.7(3) 4_576 . . . ?
Ni1 O1 C1 O2 0.7(4) . . . . ?
Ni1 O1 C1 C2 -178.84(17) . . . . ?
Ni2 O2 C1 O1 175.5(2) . . . . ?
Ni2 O2 C1 C2 -5.0(4) . . . . ?
O1 C1 C2 C8 46.8(4) . . . . ?
O2 C1 C2 C8 -132.7(3) . . . . ?
O1 C1 C2 C3 -130.2(3) . . . . ?
O2 C1 C2 C3 50.2(4) . . . . ?
C8 C2 C3 C5 2.1(4) . . . . ?
C1 C2 C3 C5 179.1(3) . . . . ?
C8 C2 C3 C4 -176.6(3) . . . . ?
C1 C2 C3 C4 0.4(4) . . . . ?
Ni3 O4 C4 O3 -20.0(4) . . . . ?
Ni3 O4 C4 C3 155.88(18) . . . . ?
Ni2 O3 C4 O4 -149.9(2) . . . . ?
Ni2 O3 C4 C3 34.4(4) . . . . ?
C5 C3 C4 O4 -60.7(3) . . . . ?
C2 C3 C4 O4 118.1(3) . . . . ?
C5 C3 C4 O3 115.5(3) . . . . ?
C2 C3 C4 O3 -65.8(4) . . . . ?
C2 C3 C5 C6 1.1(4) . . . . ?
C4 C3 C5 C6 179.9(3) . . . . ?
C3 C5 C6 C7 -3.5(4) . . . . ?
C3 C5 C6 C9 174.8(3) . . . . ?
C5 C6 C7 C8 2.5(4) . . . . ?
C9 C6 C7 C8 -175.6(3) . . . . ?
C5 C6 C7 C16 -176.7(3) . . . . ?
C9 C6 C7 C16 5.2(4) . . . . ?
C3 C2 C8 C7 -3.0(4) . . . . ?
C1 C2 C8 C7 179.8(3) . . . . ?
C6 C7 C8 C2 0.6(4) . . . . ?
C16 C7 C8 C2 179.9(3) . . . . ?
C5 C6 C9 C10 -58.5(4) . . . . ?
C7 C6 C9 C10 119.6(3) . . . . ?
C5 C6 C9 C14 121.0(3) . . . . ?
C7 C6 C9 C14 -60.9(4) . . . . ?
C14 C9 C10 C11 5.4(4) . . . . ?
C6 C9 C10 C11 -175.1(3) . . . . ?
C9 C10 C11 C12 -1.5(5) . . . . ?
C10 C11 C12 C13 -3.3(4) . . . . ?
C11 C12 C13 C14 4.2(4) . . . . ?
C11 C12 C13 C15 -175.1(3) . . . . ?
C10 C9 C14 C13 -4.5(4) . . . . ?
C6 C9 C14 C13 176.0(2) . . . . ?
C12 C13 C14 C9 -0.2(4) . . . . ?
C15 C13 C14 C9 179.0(2) . . . . ?
Ni3 O6 C15 O5 -23.5(4) 2 . . . ?
Ni3 O6 C15 C13 156.17(18) 2 . . . ?
C12 C13 C15 O5 151.7(3) . . . . ?
C14 C13 C15 O5 -27.6(4) . . . . ?
C12 C13 C15 O6 -28.0(4) . . . . ?
C14 C13 C15 O6 152.7(3) . . . . ?
C8 C7 C16 C21 -33.7(4) . . . . ?
C6 C7 C16 C21 145.5(3) . . . . ?
C8 C7 C16 C17 144.2(3) . . . . ?
C6 C7 C16 C17 -36.5(4) . . . . ?
C21 C16 C17 C18 -2.0(4) . . . . ?
C7 C16 C17 C18 -180.0(3) . . . . ?
C16 C17 C18 C19 3.6(4) . . . . ?
C16 C17 C18 C22 -174.1(3) . . . . ?
C17 C18 C19 C20 -2.5(4) . . . . ?
C22 C18 C19 C20 175.1(3) . . . . ?
C18 C19 C20 C21 -0.1(5) . . . . ?
C19 C20 C21 C16 1.7(5) . . . . ?
C17 C16 C21 C20 -0.7(4) . . . . ?
C7 C16 C21 C20 177.4(3) . . . . ?
Ni2 O7 C22 O8 -0.4(3) 4_575 . . . ?
Ni2 O7 C22 C18 176.4(2) 4_575 . . . ?
Ni2 O8 C22 O7 0.4(3) 4_575 . . . ?
Ni2 O8 C22 C18 -176.4(2) 4_575 . . . ?
C17 C18 C22 O7 -8.1(4) . . . . ?
C19 C18 C22 O7 174.2(3) . . . . ?
C17 C18 C22 O8 168.7(3) . . . . ?
C19 C18 C22 O8 -9.0(4) . . . . ?
C17 C18 C22 Ni2 33(3) . . . 4_575 ?
C19 C18 C22 Ni2 -144(2) . . . 4_575 ?
C27 N1 C23 C24 -3.9(5) . . . . ?
Ni2 N1 C23 C24 161.4(2) . . . . ?
N1 C23 C24 C25 0.2(5) . . . . ?
C28 N2 C25 C24 -173.6(3) . . . . ?
C28 N2 C25 C26 4.9(5) . . . . ?
C23 C24 C25 N2 -177.6(3) . . . . ?
C23 C24 C25 C26 3.7(4) . . . . ?
N2 C25 C26 C27 177.5(3) . . . . ?
C24 C25 C26 C27 -4.0(4) . . . . ?
C23 N1 C27 C26 3.6(5) . . . . ?
Ni2 N1 C27 C26 -159.6(2) . . . . ?
C25 C26 C27 N1 0.3(5) . . . . ?
C25 N2 C28 C32 -38.0(5) . . . . ?
C25 N2 C28 C29 146.0(3) . . . . ?
C32 C28 C29 C30 2.4(5) . . . . ?
N2 C28 C29 C30 178.7(3) . . . . ?
C31 N3 C30 C29 -2.3(4) . . . . ?
Ni1 N3 C30 C29 179.6(2) 2_645 . . . ?
C28 C29 C30 N3 -0.3(5) . . . . ?
C30 N3 C31 C32 2.8(4) . . . . ?
Ni1 N3 C31 C32 -179.1(2) 2_645 . . . ?
N3 C31 C32 C28 -0.7(5) . . . . ?
N2 C28 C32 C31 -178.0(3) . . . . ?
C29 C28 C32 C31 -1.9(4) . . . . ?



_diffrn_measured_fraction_theta_max 0.996

_diffrn_reflns_theta_full        27.55

_diffrn_measured_fraction_theta_full 0.996

_refine_diff_density_max         1.143

_refine_diff_density_min         -1.120

_refine_diff_density_rms         0.132

_database_code_depnum_ccdc_archive 'CCDC 958450'
