# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Euan K Brechin'
_publ_contact_author_email       EBRECHIN@STAFFMAIL.ED.AC.UK

_publ_section_title              
;
Splitting the cube: A tetranuclear cobalt(II)
cubane cluster and its dimer of dimers
;
loop_
_publ_author_name
'Euan K Brechin'
'Ross Inglis'
'Athanasios D. Katsenis'
'Vadim G. Kessler'
;
G.Papaefstathiou
;
'Alexandra M Z Slawin'

# Attachment 'tdk281.cif'

data_tdk281
_database_code_depnum_ccdc_archive 'CCDC 727655'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H72 Co4 N12 O12,(N O3)4,(C H4 O)2'
_chemical_formula_sum            'C74 H80 Co4 N16 O26'
_chemical_formula_weight         1845.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   13.463(3)
_cell_length_b                   14.090(3)
_cell_length_c                   21.268(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.875(9)
_cell_angle_gamma                90.00
_cell_volume                     4025.1(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4370
_cell_measurement_theta_min      21.3646
_cell_measurement_theta_max      68.6039

_exptl_crystal_description       Prism
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.1200
_exptl_crystal_size_mid          0.1200
_exptl_crystal_size_min          0.1200
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1904
_exptl_absorpt_coefficient_mu    7.104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4808
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  confocal
_diffrn_measurement_device_type  CCD
_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            53265
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.77
_diffrn_reflns_theta_max         67.95
_reflns_number_total             6967
_reflns_number_gt                6320
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Corp., 2004)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2004)'
_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)+(0.0537P)²+4.6710P] 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         6967
_refine_ls_number_parameters     550
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0459
_refine_ls_wR_factor_ref         0.1145
_refine_ls_wR_factor_gt          0.1099
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.39013(3) 0.21945(3) 0.17644(2) 0.02178(13) Uani 1 1 d . . .
Co2 Co 0.61553(3) 0.23081(3) 0.212960(19) 0.02072(13) Uani 1 1 d . . .
O1 O 0.52628(14) 0.15822(12) 0.15100(8) 0.0221(4) Uani 1 1 d . . .
C1 C 0.5258(2) 0.06106(18) 0.15562(13) 0.0232(6) Uani 1 1 d . . .
C2 C 0.4221(2) 0.02518(19) 0.13100(12) 0.0243(6) Uani 1 1 d . . .
N3 N 0.34814(18) 0.08942(16) 0.13208(10) 0.0255(5) Uani 1 1 d . . .
C4 C 0.2563(2) 0.0647(2) 0.10882(13) 0.0301(7) Uani 1 1 d . . .
H4A H 0.2044 0.1104 0.1092 0.036 Uiso 1 1 calc R . .
C5 C 0.2344(2) -0.0242(2) 0.08445(14) 0.0335(7) Uani 1 1 d . . .
H5A H 0.1690 -0.0392 0.0679 0.040 Uiso 1 1 calc R . .
C6 C 0.3096(2) -0.0911(2) 0.08459(14) 0.0339(7) Uani 1 1 d . . .
H6A H 0.2962 -0.1533 0.0690 0.041 Uiso 1 1 calc R . .
C7 C 0.4046(2) -0.0665(2) 0.10773(14) 0.0312(7) Uani 1 1 d . . .
H7A H 0.4573 -0.1113 0.1078 0.037 Uiso 1 1 calc R . .
C8 C 0.5550(2) 0.02769(19) 0.22331(13) 0.0243(6) Uani 1 1 d . . .
N9 N 0.59228(17) 0.09552(16) 0.26241(10) 0.0247(5) Uani 1 1 d . . .
C10 C 0.6194(2) 0.0711(2) 0.32216(13) 0.0307(7) Uani 1 1 d . . .
H10A H 0.6449 0.1191 0.3502 0.037 Uiso 1 1 calc R . .
C11 C 0.6120(2) -0.0205(2) 0.34483(15) 0.0348(7) Uani 1 1 d . . .
H11A H 0.6310 -0.0349 0.3876 0.042 Uiso 1 1 calc R . .
C12 C 0.5764(2) -0.0905(2) 0.30377(15) 0.0374(8) Uani 1 1 d . . .
H12A H 0.5716 -0.1543 0.3177 0.045 Uiso 1 1 calc R . .
C13 C 0.5476(2) -0.0665(2) 0.24201(14) 0.0302(7) Uani 1 1 d . . .
H13A H 0.5233 -0.1136 0.2129 0.036 Uiso 1 1 calc R . .
O14 O 0.60080(15) 0.01740(13) 0.12104(9) 0.0285(5) Uani 1 1 d . . .
C14 C 0.6018(2) 0.0460(2) 0.05683(14) 0.0341(7) Uani 1 1 d . . .
H14A H 0.5515 0.0953 0.0480 0.051 Uiso 1 1 calc R . .
H14B H 0.5870 -0.0088 0.0294 0.051 Uiso 1 1 calc R . .
H14C H 0.6677 0.0711 0.0490 0.051 Uiso 1 1 calc R . .
O15 O 0.24406(16) 0.27617(16) 0.18265(10) 0.0379(5) Uani 1 1 d . . .
C15 C 0.1800(3) 0.2771(3) 0.2332(2) 0.0618(12) Uani 1 1 d . . .
H15A H 0.1571 0.2124 0.2410 0.093 Uiso 1 1 calc R . .
H15B H 0.1224 0.3178 0.2221 0.093 Uiso 1 1 calc R . .
H15C H 0.2162 0.3018 0.2712 0.093 Uiso 1 1 calc R . .
O21 O 0.47975(14) 0.30512(13) 0.23081(8) 0.0222(4) Uani 1 1 d . . .
N21 N 0.37953(18) 0.16102(17) 0.27026(11) 0.0263(5) Uani 1 1 d . . .
C21 C 0.4659(2) 0.3097(2) 0.29415(12) 0.0251(6) Uani 1 1 d . . .
C22 C 0.4132(2) 0.2201(2) 0.31626(13) 0.0263(6) Uani 1 1 d . . .
C24 C 0.3352(2) 0.0797(2) 0.28629(15) 0.0329(7) Uani 1 1 d . . .
H24A H 0.3125 0.0371 0.2537 0.040 Uiso 1 1 calc R . .
C25 C 0.3215(3) 0.0555(3) 0.34759(16) 0.0429(8) Uani 1 1 d . . .
H25A H 0.2912 -0.0031 0.3573 0.052 Uiso 1 1 calc R . .
C26 C 0.3523(3) 0.1178(3) 0.39454(16) 0.0476(9) Uani 1 1 d . . .
H26A H 0.3415 0.1034 0.4372 0.057 Uiso 1 1 calc R . .
C27 C 0.3992(3) 0.2017(2) 0.37961(14) 0.0362(7) Uani 1 1 d . . .
H27A H 0.4212 0.2454 0.4116 0.043 Uiso 1 1 calc R . .
C28 C 0.5676(2) 0.3250(2) 0.33065(13) 0.0265(6) Uani 1 1 d . . .
N29 N 0.64735(18) 0.29684(16) 0.30024(10) 0.0247(5) Uani 1 1 d . . .
C30 C 0.7390(2) 0.3074(2) 0.32904(14) 0.0285(6) Uani 1 1 d . . .
H30A H 0.7951 0.2873 0.3077 0.034 Uiso 1 1 calc R . .
C31 C 0.7541(3) 0.3462(2) 0.38812(14) 0.0348(7) Uani 1 1 d . . .
H31A H 0.8195 0.3531 0.4072 0.042 Uiso 1 1 calc R . .
C32 C 0.6728(3) 0.3751(2) 0.41935(15) 0.0418(8) Uani 1 1 d . . .
H32A H 0.6815 0.4017 0.4604 0.050 Uiso 1 1 calc R . .
C33 C 0.5785(3) 0.3649(2) 0.39020(14) 0.0363(8) Uani 1 1 d . . .
H33A H 0.5218 0.3852 0.4108 0.044 Uiso 1 1 calc R . .
O34 O 0.39956(15) 0.38437(14) 0.30952(9) 0.0300(5) Uani 1 1 d . . .
C34 C 0.4281(3) 0.4769(2) 0.28939(15) 0.0372(8) Uani 1 1 d . . .
H34A H 0.4829 0.5007 0.3177 0.056 Uiso 1 1 calc R . .
H34B H 0.3712 0.5201 0.2903 0.056 Uiso 1 1 calc R . .
H34C H 0.4497 0.4733 0.2464 0.056 Uiso 1 1 calc R . .
O35 O 0.76050(16) 0.18604(14) 0.19352(9) 0.0321(5) Uani 1 1 d . . .
C35 C 0.8157(3) 0.1073(3) 0.21991(17) 0.0453(9) Uani 1 1 d . . .
H35A H 0.7988 0.0975 0.2636 0.068 Uiso 1 1 calc R . .
H35B H 0.8871 0.1202 0.2191 0.068 Uiso 1 1 calc R . .
H35C H 0.7990 0.0501 0.1952 0.068 Uiso 1 1 calc R . .
C41 C 0.3736(2) 0.44362(19) -0.00316(12) 0.0227(6) Uani 1 1 d . . .
C42 C 0.3790(2) 0.3463(2) -0.01518(14) 0.0325(7) Uani 1 1 d . . .
H42A H 0.3773 0.3237 -0.0573 0.039 Uiso 1 1 calc R . .
C43 C 0.3869(3) 0.2829(2) 0.03461(14) 0.0317(7) Uani 1 1 d . . .
H43A H 0.3909 0.2171 0.0253 0.038 Uiso 1 1 calc R . .
N44 N 0.38917(18) 0.30908(16) 0.09510(11) 0.0242(5) Uani 1 1 d . . .
C45 C 0.3860(2) 0.4028(2) 0.10661(13) 0.0271(6) Uani 1 1 d . . .
H45A H 0.3895 0.4232 0.1493 0.033 Uiso 1 1 calc R . .
C46 C 0.3779(2) 0.47089(19) 0.05996(13) 0.0247(6) Uani 1 1 d . . .
H46A H 0.3753 0.5362 0.0708 0.030 Uiso 1 1 calc R . .
C51 C 0.6344(2) 0.48408(18) 0.05415(13) 0.0223(6) Uani 1 1 d . . .
C52 C 0.6482(3) 0.3881(2) 0.04013(14) 0.0328(7) Uani 1 1 d . . .
H52A H 0.6571 0.3690 -0.0020 0.039 Uiso 1 1 calc R . .
C53 C 0.6488(3) 0.3214(2) 0.08757(14) 0.0324(7) Uani 1 1 d . . .
H53A H 0.6572 0.2566 0.0768 0.039 Uiso 1 1 calc R . .
N54 N 0.63825(18) 0.34322(15) 0.14795(10) 0.0239(5) Uani 1 1 d . . .
C55 C 0.6282(2) 0.43513(19) 0.16192(13) 0.0238(6) Uani 1 1 d . . .
H55A H 0.6219 0.4522 0.2047 0.029 Uiso 1 1 calc R . .
C56 C 0.6266(2) 0.50648(19) 0.11742(13) 0.0245(6) Uani 1 1 d . . .
H56A H 0.6203 0.5708 0.1299 0.029 Uiso 1 1 calc R . .
N61 N 0.4616(2) 0.68644(18) 0.14426(12) 0.0353(6) Uani 1 1 d . . .
O61 O 0.4419(2) 0.61953(18) 0.17920(12) 0.0571(7) Uani 1 1 d . . .
O62 O 0.4059(2) 0.70421(17) 0.09704(13) 0.0629(8) Uani 1 1 d . . .
O63 O 0.5385(2) 0.73497(17) 0.15508(13) 0.0522(7) Uani 1 1 d . . .
N64 N 0.5974(2) 0.6775(2) 0.43734(14) 0.0475(8) Uani 1 1 d . . .
O64 O 0.6830(3) 0.6521(4) 0.4327(2) 0.1193(16) Uani 1 1 d . . .
O65 O 0.5607(4) 0.7169(3) 0.39187(17) 0.138(2) Uani 1 1 d . . .
O66 O 0.5513(3) 0.6641(3) 0.48260(16) 0.1060(14) Uani 1 1 d . . .
O67 O 0.3760(2) 0.7931(3) 0.42143(17) 0.0820(11) Uani 1 1 d D . .
H67O H 0.435(4) 0.753(5) 0.420(4) 0.16(3) Uiso 1 1 d D . .
C67 C 0.3904(4) 0.8560(4) 0.4710(2) 0.0729(13) Uani 1 1 d . . .
H67A H 0.3951 0.8209 0.5108 0.109 Uiso 1 1 calc R . .
H67B H 0.3342 0.9003 0.4706 0.109 Uiso 1 1 calc R . .
H67C H 0.4521 0.8916 0.4666 0.109 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 O21 2.0153(19) . ?
Co1 N3 2.120(2) . ?
Co1 O1 2.1286(19) . ?
Co1 O15 2.135(2) . ?
Co1 N44 2.141(2) . ?
Co1 N21 2.172(2) . ?
Co2 O1 2.0031(19) . ?
Co2 N29 2.095(2) . ?
Co2 O35 2.118(2) . ?
Co2 N54 2.138(2) . ?
Co2 O21 2.1624(19) . ?
Co2 N9 2.210(2) . ?
O1 C1 1.373(3) . ?
C1 O14 1.428(3) . ?
C1 C8 1.540(4) . ?
C1 C2 1.542(4) . ?
C2 N3 1.347(4) . ?
C2 C7 1.397(4) . ?
N3 C4 1.347(4) . ?
C4 C5 1.380(4) . ?
C4 H4A 0.9500 . ?
C5 C6 1.384(5) . ?
C5 H5A 0.9500 . ?
C6 C7 1.383(4) . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9500 . ?
C8 N9 1.342(4) . ?
C8 C13 1.391(4) . ?
N9 C10 1.343(4) . ?
C10 C11 1.384(4) . ?
C10 H10A 0.9500 . ?
C11 C12 1.382(5) . ?
C11 H11A 0.9500 . ?
C12 C13 1.386(4) . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
O14 C14 1.425(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
O15 C15 1.423(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
O21 C21 1.374(3) . ?
N21 C22 1.340(4) . ?
N21 C24 1.347(4) . ?
C21 O34 1.433(3) . ?
C21 C22 1.537(4) . ?
C21 C28 1.543(4) . ?
C22 C27 1.397(4) . ?
C24 C25 1.372(4) . ?
C24 H24A 0.9500 . ?
C25 C26 1.372(5) . ?
C25 H25A 0.9500 . ?
C26 C27 1.387(5) . ?
C26 H26A 0.9500 . ?
C27 H27A 0.9500 . ?
C28 N29 1.349(4) . ?
C28 C33 1.385(4) . ?
N29 C30 1.348(4) . ?
C30 C31 1.373(4) . ?
C30 H30A 0.9500 . ?
C31 C32 1.380(5) . ?
C31 H31A 0.9500 . ?
C32 C33 1.381(5) . ?
C32 H32A 0.9500 . ?
C33 H33A 0.9500 . ?
O34 C34 1.433(4) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
O35 C35 1.429(4) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C41 C46 1.394(4) . ?
C41 C42 1.398(4) . ?
C41 C51 1.487(4) 3_665 ?
C42 C43 1.384(4) . ?
C42 H42A 0.9500 . ?
C43 N44 1.337(4) . ?
C43 H43A 0.9500 . ?
N44 C45 1.344(4) . ?
C45 C46 1.380(4) . ?
C45 H45A 0.9500 . ?
C46 H46A 0.9500 . ?
C51 C56 1.393(4) . ?
C51 C52 1.399(4) . ?
C51 C41 1.487(4) 3_665 ?
C52 C53 1.379(4) . ?
C52 H52A 0.9500 . ?
C53 N54 1.337(4) . ?
C53 H53A 0.9500 . ?
N54 C55 1.338(3) . ?
C55 C56 1.380(4) . ?
C55 H55A 0.9500 . ?
C56 H56A 0.9500 . ?
N61 O62 1.238(4) . ?
N61 O61 1.240(3) . ?
N61 O63 1.249(4) . ?
N64 O65 1.192(4) . ?
N64 O66 1.195(4) . ?
N64 O64 1.217(4) . ?
O67 C67 1.381(5) . ?
O67 H67O 0.97(2) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?

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
O21 Co1 N3 154.73(9) . . ?
O21 Co1 O1 84.04(7) . . ?
N3 Co1 O1 75.22(8) . . ?
O21 Co1 O15 104.98(8) . . ?
N3 Co1 O15 97.59(9) . . ?
O1 Co1 O15 168.53(8) . . ?
O21 Co1 N44 94.64(8) . . ?
N3 Co1 N44 99.40(9) . . ?
O1 Co1 N44 89.54(8) . . ?
O15 Co1 N44 82.76(9) . . ?
O21 Co1 N21 76.93(8) . . ?
N3 Co1 N21 92.82(9) . . ?
O1 Co1 N21 101.01(8) . . ?
O15 Co1 N21 88.11(9) . . ?
N44 Co1 N21 165.59(9) . . ?
O1 Co2 N29 152.55(9) . . ?
O1 Co2 O35 103.84(8) . . ?
N29 Co2 O35 99.75(9) . . ?
O1 Co2 N54 93.36(8) . . ?
N29 Co2 N54 102.38(9) . . ?
O35 Co2 N54 85.44(9) . . ?
O1 Co2 O21 83.46(7) . . ?
N29 Co2 O21 75.76(8) . . ?
O35 Co2 O21 168.37(8) . . ?
N54 Co2 O21 85.09(8) . . ?
O1 Co2 N9 76.97(8) . . ?
N29 Co2 N9 89.34(9) . . ?
O35 Co2 N9 89.88(8) . . ?
N54 Co2 N9 167.95(9) . . ?
O21 Co2 N9 100.69(8) . . ?
C1 O1 Co2 117.89(16) . . ?
C1 O1 Co1 112.19(16) . . ?
Co2 O1 Co1 96.57(8) . . ?
O1 C1 O14 112.7(2) . . ?
O1 C1 C8 111.7(2) . . ?
O14 C1 C8 101.8(2) . . ?
O1 C1 C2 108.1(2) . . ?
O14 C1 C2 109.8(2) . . ?
C8 C1 C2 112.7(2) . . ?
N3 C2 C7 121.3(3) . . ?
N3 C2 C1 115.3(2) . . ?
C7 C2 C1 123.4(3) . . ?
C2 N3 C4 118.8(2) . . ?
C2 N3 Co1 114.39(18) . . ?
C4 N3 Co1 126.7(2) . . ?
N3 C4 C5 122.7(3) . . ?
N3 C4 H4A 118.7 . . ?
C5 C4 H4A 118.7 . . ?
C4 C5 C6 118.7(3) . . ?
C4 C5 H5A 120.6 . . ?
C6 C5 H5A 120.6 . . ?
C7 C6 C5 119.2(3) . . ?
C7 C6 H6A 120.4 . . ?
C5 C6 H6A 120.4 . . ?
C6 C7 C2 119.2(3) . . ?
C6 C7 H7A 120.4 . . ?
C2 C7 H7A 120.4 . . ?
N9 C8 C13 122.2(3) . . ?
N9 C8 C1 115.0(2) . . ?
C13 C8 C1 122.7(3) . . ?
C10 N9 C8 118.1(2) . . ?
C10 N9 Co2 129.3(2) . . ?
C8 N9 Co2 112.25(17) . . ?
N9 C10 C11 123.2(3) . . ?
N9 C10 H10A 118.4 . . ?
C11 C10 H10A 118.4 . . ?
C12 C11 C10 118.4(3) . . ?
C12 C11 H11A 120.8 . . ?
C10 C11 H11A 120.8 . . ?
C11 C12 C13 119.2(3) . . ?
C11 C12 H12A 120.4 . . ?
C13 C12 H12A 120.4 . . ?
C12 C13 C8 118.9(3) . . ?
C12 C13 H13A 120.6 . . ?
C8 C13 H13A 120.6 . . ?
C14 O14 C1 115.2(2) . . ?
O14 C14 H14A 109.5 . . ?
O14 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O14 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C15 O15 Co1 131.2(2) . . ?
O15 C15 H15A 109.5 . . ?
O15 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O15 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 O21 Co1 118.36(17) . . ?
C21 O21 Co2 111.52(16) . . ?
Co1 O21 Co2 95.15(7) . . ?
C22 N21 C24 118.6(2) . . ?
C22 N21 Co1 113.28(18) . . ?
C24 N21 Co1 127.8(2) . . ?
O21 C21 O34 112.7(2) . . ?
O21 C21 C22 111.0(2) . . ?
O34 C21 C22 103.0(2) . . ?
O21 C21 C28 109.0(2) . . ?
O34 C21 C28 109.2(2) . . ?
C22 C21 C28 111.9(2) . . ?
N21 C22 C27 121.8(3) . . ?
N21 C22 C21 115.3(2) . . ?
C27 C22 C21 122.9(3) . . ?
N21 C24 C25 122.8(3) . . ?
N21 C24 H24A 118.6 . . ?
C25 C24 H24A 118.6 . . ?
C24 C25 C26 118.7(3) . . ?
C24 C25 H25A 120.7 . . ?
C26 C25 H25A 120.7 . . ?
C25 C26 C27 119.9(3) . . ?
C25 C26 H26A 120.1 . . ?
C27 C26 H26A 120.1 . . ?
C26 C27 C22 118.2(3) . . ?
C26 C27 H27A 120.9 . . ?
C22 C27 H27A 120.9 . . ?
N29 C28 C33 121.3(3) . . ?
N29 C28 C21 115.2(2) . . ?
C33 C28 C21 123.5(3) . . ?
C30 N29 C28 118.9(2) . . ?
C30 N29 Co2 125.3(2) . . ?
C28 N29 Co2 115.70(19) . . ?
N29 C30 C31 122.3(3) . . ?
N29 C30 H30A 118.9 . . ?
C31 C30 H30A 118.9 . . ?
C30 C31 C32 119.0(3) . . ?
C30 C31 H31A 120.5 . . ?
C32 C31 H31A 120.5 . . ?
C31 C32 C33 119.2(3) . . ?
C31 C32 H32A 120.4 . . ?
C33 C32 H32A 120.4 . . ?
C32 C33 C28 119.4(3) . . ?
C32 C33 H33A 120.3 . . ?
C28 C33 H33A 120.3 . . ?
C21 O34 C34 114.6(2) . . ?
O34 C34 H34A 109.5 . . ?
O34 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
O34 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C35 O35 Co2 128.0(2) . . ?
O35 C35 H35A 109.5 . . ?
O35 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
O35 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C46 C41 C42 116.6(2) . . ?
C46 C41 C51 120.7(2) . 3_665 ?
C42 C41 C51 122.7(2) . 3_665 ?
C43 C42 C41 119.7(3) . . ?
C43 C42 H42A 120.2 . . ?
C41 C42 H42A 120.2 . . ?
N44 C43 C42 123.6(3) . . ?
N44 C43 H43A 118.2 . . ?
C42 C43 H43A 118.2 . . ?
C43 N44 C45 116.6(2) . . ?
C43 N44 Co1 127.82(19) . . ?
C45 N44 Co1 115.51(18) . . ?
N44 C45 C46 123.7(3) . . ?
N44 C45 H45A 118.2 . . ?
C46 C45 H45A 118.2 . . ?
C45 C46 C41 119.8(3) . . ?
C45 C46 H46A 120.1 . . ?
C41 C46 H46A 120.1 . . ?
C56 C51 C52 116.4(2) . . ?
C56 C51 C41 122.9(2) . 3_665 ?
C52 C51 C41 120.7(2) . 3_665 ?
C53 C52 C51 119.8(3) . . ?
C53 C52 H52A 120.1 . . ?
C51 C52 H52A 120.1 . . ?
N54 C53 C52 123.4(3) . . ?
N54 C53 H53A 118.3 . . ?
C52 C53 H53A 118.3 . . ?
C53 N54 C55 117.0(2) . . ?
C53 N54 Co2 118.69(18) . . ?
C55 N54 Co2 123.55(18) . . ?
N54 C55 C56 123.4(3) . . ?
N54 C55 H55A 118.3 . . ?
C56 C55 H55A 118.3 . . ?
C55 C56 C51 119.9(3) . . ?
C55 C56 H56A 120.0 . . ?
C51 C56 H56A 120.0 . . ?
O62 N61 O61 119.8(3) . . ?
O62 N61 O63 119.2(3) . . ?
O61 N61 O63 120.9(3) . . ?
O65 N64 O66 121.2(4) . . ?
O65 N64 O64 114.4(4) . . ?
O66 N64 O64 124.4(4) . . ?
C67 O67 H67O 108(5) . . ?
O67 C67 H67A 109.5 . . ?
O67 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
O67 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N29 Co2 O1 C1 -85.2(3) . . . . ?
O35 Co2 O1 C1 63.27(19) . . . . ?
N54 Co2 O1 C1 149.39(18) . . . . ?
O21 Co2 O1 C1 -125.94(18) . . . . ?
N9 Co2 O1 C1 -23.34(18) . . . . ?
N29 Co2 O1 Co1 34.2(2) . . . . ?
O35 Co2 O1 Co1 -177.32(7) . . . . ?
N54 Co2 O1 Co1 -91.19(8) . . . . ?
O21 Co2 O1 Co1 -6.53(7) . . . . ?
N9 Co2 O1 Co1 96.07(9) . . . . ?
O21 Co1 O1 C1 130.75(17) . . . . ?
N3 Co1 O1 C1 -34.68(17) . . . . ?
O15 Co1 O1 C1 -86.8(4) . . . . ?
N44 Co1 O1 C1 -134.53(17) . . . . ?
N21 Co1 O1 C1 55.35(18) . . . . ?
O21 Co1 O1 Co2 7.00(7) . . . . ?
N3 Co1 O1 Co2 -158.43(9) . . . . ?
O15 Co1 O1 Co2 149.4(4) . . . . ?
N44 Co1 O1 Co2 101.72(9) . . . . ?
N21 Co1 O1 Co2 -68.40(9) . . . . ?
Co2 O1 C1 O14 -87.5(2) . . . . ?
Co1 O1 C1 O14 161.64(16) . . . . ?
Co2 O1 C1 C8 26.4(3) . . . . ?
Co1 O1 C1 C8 -84.5(2) . . . . ?
Co2 O1 C1 C2 150.91(16) . . . . ?
Co1 O1 C1 C2 40.1(2) . . . . ?
O1 C1 C2 N3 -22.4(3) . . . . ?
O14 C1 C2 N3 -145.7(2) . . . . ?
C8 C1 C2 N3 101.6(3) . . . . ?
O1 C1 C2 C7 156.3(2) . . . . ?
O14 C1 C2 C7 33.0(3) . . . . ?
C8 C1 C2 C7 -79.8(3) . . . . ?
C7 C2 N3 C4 -1.5(4) . . . . ?
C1 C2 N3 C4 177.2(2) . . . . ?
C7 C2 N3 Co1 175.1(2) . . . . ?
C1 C2 N3 Co1 -6.2(3) . . . . ?
O21 Co1 N3 C2 -14.8(3) . . . . ?
O1 Co1 N3 C2 21.09(17) . . . . ?
O15 Co1 N3 C2 -168.03(18) . . . . ?
N44 Co1 N3 C2 108.10(19) . . . . ?
N21 Co1 N3 C2 -79.56(19) . . . . ?
O21 Co1 N3 C4 161.6(2) . . . . ?
O1 Co1 N3 C4 -162.6(2) . . . . ?
O15 Co1 N3 C4 8.3(2) . . . . ?
N44 Co1 N3 C4 -75.6(2) . . . . ?
N21 Co1 N3 C4 96.8(2) . . . . ?
C2 N3 C4 C5 0.7(4) . . . . ?
Co1 N3 C4 C5 -175.5(2) . . . . ?
N3 C4 C5 C6 0.8(4) . . . . ?
C4 C5 C6 C7 -1.4(4) . . . . ?
C5 C6 C7 C2 0.6(4) . . . . ?
N3 C2 C7 C6 0.9(4) . . . . ?
C1 C2 C7 C6 -177.7(3) . . . . ?
O1 C1 C8 N9 -11.3(3) . . . . ?
O14 C1 C8 N9 109.2(3) . . . . ?
C2 C1 C8 N9 -133.2(2) . . . . ?
O1 C1 C8 C13 171.4(3) . . . . ?
O14 C1 C8 C13 -68.1(3) . . . . ?
C2 C1 C8 C13 49.5(4) . . . . ?
C13 C8 N9 C10 -2.6(4) . . . . ?
C1 C8 N9 C10 -179.9(2) . . . . ?
C13 C8 N9 Co2 170.6(2) . . . . ?
C1 C8 N9 Co2 -6.6(3) . . . . ?
O1 Co2 N9 C10 -172.1(3) . . . . ?
N29 Co2 N9 C10 -16.1(3) . . . . ?
O35 Co2 N9 C10 83.7(3) . . . . ?
N54 Co2 N9 C10 150.7(4) . . . . ?
O21 Co2 N9 C10 -91.5(3) . . . . ?
O1 Co2 N9 C8 15.57(19) . . . . ?
N29 Co2 N9 C8 171.6(2) . . . . ?
O35 Co2 N9 C8 -88.7(2) . . . . ?
N54 Co2 N9 C8 -21.7(5) . . . . ?
O21 Co2 N9 C8 96.20(19) . . . . ?
C8 N9 C10 C11 0.9(4) . . . . ?
Co2 N9 C10 C11 -171.0(2) . . . . ?
N9 C10 C11 C12 1.0(5) . . . . ?
C10 C11 C12 C13 -1.2(5) . . . . ?
C11 C12 C13 C8 -0.4(5) . . . . ?
N9 C8 C13 C12 2.4(5) . . . . ?
C1 C8 C13 C12 179.5(3) . . . . ?
O1 C1 O14 C14 -52.0(3) . . . . ?
C8 C1 O14 C14 -171.7(2) . . . . ?
C2 C1 O14 C14 68.7(3) . . . . ?
O21 Co1 O15 C15 -70.8(3) . . . . ?
N3 Co1 O15 C15 97.7(3) . . . . ?
O1 Co1 O15 C15 148.1(4) . . . . ?
N44 Co1 O15 C15 -163.7(3) . . . . ?
N21 Co1 O15 C15 5.1(3) . . . . ?
N3 Co1 O21 C21 -89.6(3) . . . . ?
O1 Co1 O21 C21 -124.32(18) . . . . ?
O15 Co1 O21 C21 62.90(19) . . . . ?
N44 Co1 O21 C21 146.63(19) . . . . ?
N21 Co1 O21 C21 -21.53(18) . . . . ?
N3 Co1 O21 Co2 28.2(2) . . . . ?
O1 Co1 O21 Co2 -6.47(7) . . . . ?
O15 Co1 O21 Co2 -179.25(7) . . . . ?
N44 Co1 O21 Co2 -95.52(8) . . . . ?
N21 Co1 O21 Co2 96.32(8) . . . . ?
O1 Co2 O21 C21 130.12(17) . . . . ?
N29 Co2 O21 C21 -31.80(17) . . . . ?
O35 Co2 O21 C21 -100.3(4) . . . . ?
N54 Co2 O21 C21 -135.92(18) . . . . ?
N9 Co2 O21 C21 54.76(18) . . . . ?
O1 Co2 O21 Co1 6.88(7) . . . . ?
N29 Co2 O21 Co1 -155.05(9) . . . . ?
O35 Co2 O21 Co1 136.4(3) . . . . ?
N54 Co2 O21 Co1 100.84(8) . . . . ?
N9 Co2 O21 Co1 -68.49(9) . . . . ?
O21 Co1 N21 C22 15.7(2) . . . . ?
N3 Co1 N21 C22 172.3(2) . . . . ?
O1 Co1 N21 C22 96.8(2) . . . . ?
O15 Co1 N21 C22 -90.2(2) . . . . ?
N44 Co1 N21 C22 -39.6(5) . . . . ?
O21 Co1 N21 C24 -171.6(3) . . . . ?
N3 Co1 N21 C24 -15.0(3) . . . . ?
O1 Co1 N21 C24 -90.4(3) . . . . ?
O15 Co1 N21 C24 82.6(3) . . . . ?
N44 Co1 N21 C24 133.1(4) . . . . ?
Co1 O21 C21 O34 -92.1(2) . . . . ?
Co2 O21 C21 O34 159.12(17) . . . . ?
Co1 O21 C21 C22 22.9(3) . . . . ?
Co2 O21 C21 C22 -85.9(2) . . . . ?
Co1 O21 C21 C28 146.58(17) . . . . ?
Co2 O21 C21 C28 37.8(2) . . . . ?
C24 N21 C22 C27 -3.2(4) . . . . ?
Co1 N21 C22 C27 170.3(2) . . . . ?
C24 N21 C22 C21 178.0(3) . . . . ?
Co1 N21 C22 C21 -8.5(3) . . . . ?
O21 C21 C22 N21 -8.0(4) . . . . ?
O34 C21 C22 N21 112.8(3) . . . . ?
C28 C21 C22 N21 -130.0(3) . . . . ?
O21 C21 C22 C27 173.1(3) . . . . ?
O34 C21 C22 C27 -66.0(4) . . . . ?
C28 C21 C22 C27 51.1(4) . . . . ?
C22 N21 C24 C25 1.2(5) . . . . ?
Co1 N21 C24 C25 -171.2(3) . . . . ?
N21 C24 C25 C26 1.4(5) . . . . ?
C24 C25 C26 C27 -2.1(6) . . . . ?
C25 C26 C27 C22 0.3(6) . . . . ?
N21 C22 C27 C26 2.4(5) . . . . ?
C21 C22 C27 C26 -178.8(3) . . . . ?
O21 C21 C28 N29 -23.2(3) . . . . ?
O34 C21 C28 N29 -146.6(2) . . . . ?
C22 C21 C28 N29 100.0(3) . . . . ?
O21 C21 C28 C33 156.6(3) . . . . ?
O34 C21 C28 C33 33.1(4) . . . . ?
C22 C21 C28 C33 -80.3(3) . . . . ?
C33 C28 N29 C30 0.6(4) . . . . ?
C21 C28 N29 C30 -179.7(2) . . . . ?
C33 C28 N29 Co2 176.5(2) . . . . ?
C21 C28 N29 Co2 -3.7(3) . . . . ?
O1 Co2 N29 C30 152.1(2) . . . . ?
O35 Co2 N29 C30 3.1(2) . . . . ?
N54 Co2 N29 C30 -84.4(2) . . . . ?
O21 Co2 N29 C30 -166.0(2) . . . . ?
N9 Co2 N29 C30 92.8(2) . . . . ?
O1 Co2 N29 C28 -23.6(3) . . . . ?
O35 Co2 N29 C28 -172.61(18) . . . . ?
N54 Co2 N29 C28 99.97(19) . . . . ?
O21 Co2 N29 C28 18.37(18) . . . . ?
N9 Co2 N29 C28 -82.84(19) . . . . ?
C28 N29 C30 C31 -0.3(4) . . . . ?
Co2 N29 C30 C31 -175.9(2) . . . . ?
N29 C30 C31 C32 0.3(5) . . . . ?
C30 C31 C32 C33 -0.5(5) . . . . ?
C31 C32 C33 C28 0.7(5) . . . . ?
N29 C28 C33 C32 -0.8(5) . . . . ?
C21 C28 C33 C32 179.5(3) . . . . ?
O21 C21 O34 C34 -56.1(3) . . . . ?
C22 C21 O34 C34 -175.7(2) . . . . ?
C28 C21 O34 C34 65.2(3) . . . . ?
O1 Co2 O35 C35 -89.1(3) . . . . ?
N29 Co2 O35 C35 76.8(3) . . . . ?
N54 Co2 O35 C35 178.6(3) . . . . ?
O21 Co2 O35 C35 143.0(4) . . . . ?
N9 Co2 O35 C35 -12.5(3) . . . . ?
C46 C41 C42 C43 0.8(4) . . . . ?
C51 C41 C42 C43 179.6(3) 3_665 . . . ?
C41 C42 C43 N44 0.4(5) . . . . ?
C42 C43 N44 C45 -1.7(5) . . . . ?
C42 C43 N44 Co1 175.0(2) . . . . ?
O21 Co1 N44 C43 144.6(3) . . . . ?
N3 Co1 N44 C43 -14.3(3) . . . . ?
O1 Co1 N44 C43 60.6(3) . . . . ?
O15 Co1 N44 C43 -110.9(3) . . . . ?
N21 Co1 N44 C43 -162.0(3) . . . . ?
O21 Co1 N44 C45 -38.7(2) . . . . ?
N3 Co1 N44 C45 162.4(2) . . . . ?
O1 Co1 N44 C45 -122.6(2) . . . . ?
O15 Co1 N44 C45 65.9(2) . . . . ?
N21 Co1 N44 C45 14.8(5) . . . . ?
C43 N44 C45 C46 1.8(4) . . . . ?
Co1 N44 C45 C46 -175.3(2) . . . . ?
N44 C45 C46 C41 -0.6(5) . . . . ?
C42 C41 C46 C45 -0.7(4) . . . . ?
C51 C41 C46 C45 -179.5(3) 3_665 . . . ?
C56 C51 C52 C53 3.0(5) . . . . ?
C41 C51 C52 C53 -175.7(3) 3_665 . . . ?
C51 C52 C53 N54 -1.1(5) . . . . ?
C52 C53 N54 C55 -1.0(5) . . . . ?
C52 C53 N54 Co2 169.5(3) . . . . ?
O1 Co2 N54 C53 -39.1(2) . . . . ?
N29 Co2 N54 C53 163.5(2) . . . . ?
O35 Co2 N54 C53 64.5(2) . . . . ?
O21 Co2 N54 C53 -122.3(2) . . . . ?
N9 Co2 N54 C53 -3.0(6) . . . . ?
O1 Co2 N54 C55 130.7(2) . . . . ?
N29 Co2 N54 C55 -26.6(2) . . . . ?
O35 Co2 N54 C55 -125.6(2) . . . . ?
O21 Co2 N54 C55 47.6(2) . . . . ?
N9 Co2 N54 C55 166.9(4) . . . . ?
C53 N54 C55 C56 1.1(4) . . . . ?
Co2 N54 C55 C56 -168.9(2) . . . . ?
N54 C55 C56 C51 0.9(4) . . . . ?
C52 C51 C56 C55 -2.9(4) . . . . ?
C41 C51 C56 C55 175.8(3) 3_665 . . . ?

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
O67 H67O O65 0.97(2) 1.91(4) 2.818(6) 155(7) .

_diffrn_measured_fraction_theta_max 0.951
_diffrn_reflns_theta_full        67.00
_diffrn_measured_fraction_theta_full 0.955
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.064

# Attachment 'tdk408.cif'

data_tdk408
_database_code_depnum_ccdc_archive 'CCDC 727656'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H38 Co4 N12 O21'
_chemical_formula_weight         1306.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   20.4504(18)
_cell_length_b                   12.7826(11)
_cell_length_c                   20.0563(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.455(2)
_cell_angle_gamma                90.00
_cell_volume                     5053.3(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    8669
_cell_measurement_theta_min      1.03
_cell_measurement_theta_max      28.36

_exptl_crystal_description       block
_exptl_crystal_colour            Purple
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2648
_exptl_absorpt_coefficient_mu    1.384
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.6074
_exptl_absorpt_correction_T_max  0.8193
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(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 SMART CCD 1k'
_diffrn_measurement_method       'Bruker SMART'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29350
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.03
_diffrn_reflns_theta_max         28.36
_reflns_number_total             11941
_reflns_number_gt                9163
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINTPLUS'
_computing_data_reduction        'Bruker SAINTPLUS'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL 5.31'
_computing_publication_material  'Bruker SHELXTL 5.31'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0401P)²+18.7219P] 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       none
_refine_ls_number_reflns         11941
_refine_ls_number_parameters     731
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0554
_refine_ls_wR_factor_ref         0.1369
_refine_ls_wR_factor_gt          0.1232
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_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 0.15474(3) 0.42237(4) 0.21580(3) 0.02556(12) Uani 1 1 d . . .
Co2 Co 0.27083(3) 0.60182(4) 0.27447(3) 0.02583(12) Uani 1 1 d . . .
Co3 Co 0.30942(3) 0.35986(4) 0.26380(3) 0.02576(12) Uani 1 1 d . . .
Co4 Co 0.25488(3) 0.49881(4) 0.12646(3) 0.02615(12) Uani 1 1 d . . .
C1 C 0.0997(2) 0.2346(4) 0.2837(3) 0.0406(10) Uani 1 1 d . . .
H1 H 0.0731 0.2207 0.2392 0.049 Uiso 1 1 calc R . .
C2 C 0.0918(3) 0.1730(4) 0.3373(3) 0.0489(12) Uani 1 1 d . . .
H2 H 0.0609 0.1180 0.3292 0.059 Uiso 1 1 calc R . .
C3 C 0.1304(3) 0.1948(4) 0.4026(3) 0.0514(13) Uani 1 1 d . . .
H3 H 0.1246 0.1565 0.4401 0.062 Uiso 1 1 calc R . .
C4 C 0.1779(2) 0.2734(4) 0.4128(2) 0.0434(11) Uani 1 1 d . . .
H4 H 0.2060 0.2869 0.4567 0.052 Uiso 1 1 calc R . .
C5 C 0.1830(2) 0.3320(3) 0.3566(2) 0.0316(8) Uani 1 1 d . . .
C6 C 0.2315(2) 0.4263(3) 0.36484(19) 0.0305(8) Uani 1 1 d . . .
C7 C 0.3038(2) 0.3993(3) 0.4073(2) 0.0351(9) Uani 1 1 d . . .
C8 C 0.3258(3) 0.4133(4) 0.4783(2) 0.0512(12) Uani 1 1 d . . .
H8 H 0.2961 0.4376 0.5028 0.061 Uiso 1 1 calc R . .
C9 C 0.3927(3) 0.3903(5) 0.5123(3) 0.0664(17) Uani 1 1 d . . .
H9 H 0.4083 0.3981 0.5600 0.080 Uiso 1 1 calc R . .
C10 C 0.4357(3) 0.3557(5) 0.4745(3) 0.0672(17) Uani 1 1 d . . .
H10 H 0.4808 0.3407 0.4964 0.081 Uiso 1 1 calc R . .
C11 C 0.4111(2) 0.3437(4) 0.4041(3) 0.0493(12) Uani 1 1 d . . .
H11 H 0.4400 0.3197 0.3787 0.059 Uiso 1 1 calc R . .
C12 C 0.0334(2) 0.3333(4) 0.1021(2) 0.0444(11) Uani 1 1 d . . .
H12 H 0.0072 0.3808 0.1189 0.053 Uiso 1 1 calc R . .
C13 C 0.0019(3) 0.2688(5) 0.0482(3) 0.0564(14) Uani 1 1 d . . .
H13 H -0.0448 0.2722 0.0294 0.068 Uiso 1 1 calc R . .
C14 C 0.0396(3) 0.2002(5) 0.0228(3) 0.0567(14) Uani 1 1 d . . .
H14 H 0.0190 0.1556 -0.0133 0.068 Uiso 1 1 calc R . .
C15 C 0.1089(3) 0.1973(4) 0.0511(2) 0.0454(11) Uani 1 1 d . . .
H15 H 0.1357 0.1516 0.0337 0.054 Uiso 1 1 calc R . .
C16 C 0.1383(2) 0.2637(3) 0.1063(2) 0.0311(8) Uani 1 1 d . . .
C17 C 0.21328(19) 0.2608(3) 0.14375(19) 0.0273(8) Uani 1 1 d . . .
C18 C 0.2251(2) 0.1772(3) 0.2023(2) 0.0290(8) Uani 1 1 d . . .
C19 C 0.1943(2) 0.0806(3) 0.1922(3) 0.0428(10) Uani 1 1 d . . .
H19 H 0.1663 0.0621 0.1492 0.051 Uiso 1 1 calc R . .
C20 C 0.2057(3) 0.0119(4) 0.2472(3) 0.0493(12) Uani 1 1 d . . .
H20 H 0.1842 -0.0529 0.2420 0.059 Uiso 1 1 calc R . .
C21 C 0.2484(3) 0.0392(4) 0.3090(3) 0.0471(12) Uani 1 1 d . . .
H21 H 0.2569 -0.0069 0.3463 0.057 Uiso 1 1 calc R . .
C22 C 0.2789(2) 0.1363(3) 0.3157(2) 0.0393(10) Uani 1 1 d . . .
H22 H 0.3087 0.1547 0.3578 0.047 Uiso 1 1 calc R . .
C23 C 0.1815(2) 0.7571(3) 0.3260(2) 0.0362(9) Uani 1 1 d . . .
H23 H 0.2159 0.7545 0.3670 0.043 Uiso 1 1 calc R . .
C24 C 0.1238(2) 0.8134(4) 0.3246(2) 0.0428(11) Uani 1 1 d . . .
H24 H 0.1187 0.8466 0.3642 0.051 Uiso 1 1 calc R . .
C25 C 0.0738(2) 0.8192(4) 0.2635(3) 0.0430(10) Uani 1 1 d . . .
H25 H 0.0344 0.8570 0.2612 0.052 Uiso 1 1 calc R . .
C26 C 0.0822(2) 0.7689(3) 0.2055(2) 0.0359(9) Uani 1 1 d . . .
H26 H 0.0493 0.7736 0.1635 0.043 Uiso 1 1 calc R . .
C27 C 0.14107(19) 0.7111(3) 0.21113(19) 0.0264(7) Uani 1 1 d . . .
C28 C 0.15291(18) 0.6476(3) 0.15145(18) 0.0248(7) Uani 1 1 d . . .
C29 C 0.1901(2) 0.7094(3) 0.10718(19) 0.0293(8) Uani 1 1 d . . .
C30 C 0.1683(2) 0.8090(3) 0.0825(2) 0.0396(10) Uani 1 1 d . . .
H30 H 0.1324 0.8414 0.0947 0.048 Uiso 1 1 calc R . .
C31 C 0.2015(3) 0.8585(4) 0.0396(3) 0.0500(12) Uani 1 1 d . . .
H31 H 0.1876 0.9244 0.0217 0.060 Uiso 1 1 calc R . .
C32 C 0.2549(3) 0.8093(4) 0.0236(3) 0.0487(12) Uani 1 1 d . . .
H32 H 0.2782 0.8418 -0.0046 0.058 Uiso 1 1 calc R . .
C33 C 0.2734(2) 0.7112(4) 0.0500(2) 0.0399(10) Uani 1 1 d . . .
H33 H 0.3096 0.6781 0.0388 0.048 Uiso 1 1 calc R . .
C34 C 0.3278(2) 0.8154(3) 0.2368(3) 0.0444(11) Uani 1 1 d . . .
H34 H 0.2930 0.8459 0.2520 0.053 Uiso 1 1 calc R . .
C35 C 0.3713(3) 0.8788(4) 0.2147(3) 0.0552(14) Uani 1 1 d . . .
H35 H 0.3664 0.9511 0.2151 0.066 Uiso 1 1 calc R . .
C36 C 0.4221(3) 0.8349(4) 0.1920(3) 0.0609(15) Uani 1 1 d . . .
H36 H 0.4518 0.8770 0.1760 0.073 Uiso 1 1 calc R . .
C37 C 0.4291(2) 0.7268(4) 0.1928(3) 0.0491(12) Uani 1 1 d . . .
H37 H 0.4640 0.6950 0.1785 0.059 Uiso 1 1 calc R . .
C38 C 0.3825(2) 0.6678(3) 0.2158(2) 0.0319(8) Uani 1 1 d . . .
C39 C 0.38840(19) 0.5468(3) 0.2217(2) 0.0302(8) Uani 1 1 d . . .
C40 C 0.4032(2) 0.4975(3) 0.1578(2) 0.0348(9) Uani 1 1 d . . .
C41 C 0.4685(2) 0.4743(4) 0.1543(3) 0.0503(12) Uani 1 1 d . . .
H41 H 0.5060 0.4886 0.1911 0.060 Uiso 1 1 calc R . .
C42 C 0.4758(3) 0.4292(5) 0.0941(4) 0.0721(19) Uani 1 1 d . . .
H42 H 0.5188 0.4127 0.0898 0.086 Uiso 1 1 calc R . .
C43 C 0.4198(3) 0.4089(5) 0.0407(3) 0.0702(17) Uani 1 1 d . . .
H43 H 0.4248 0.3784 0.0002 0.084 Uiso 1 1 calc R . .
C44 C 0.3567(3) 0.4334(4) 0.0468(3) 0.0514(12) Uani 1 1 d . . .
H44 H 0.3188 0.4199 0.0103 0.062 Uiso 1 1 calc R . .
N1 N 0.14424(17) 0.3138(3) 0.29315(17) 0.0314(7) Uani 1 1 d . . .
N2 N 0.34588(18) 0.3660(3) 0.37105(18) 0.0364(8) Uani 1 1 d . . .
N3 N 0.10094(17) 0.3302(3) 0.13155(17) 0.0327(7) Uani 1 1 d . . .
N4 N 0.26679(17) 0.2054(2) 0.26299(17) 0.0300(7) Uani 1 1 d . . .
N5 N 0.19028(16) 0.7059(2) 0.27053(16) 0.0274(7) Uani 1 1 d . . .
N6 N 0.24132(17) 0.6609(3) 0.09131(16) 0.0304(7) Uani 1 1 d . . .
N7 N 0.33319(17) 0.7098(3) 0.23755(18) 0.0314(7) Uani 1 1 d . . .
N8 N 0.34863(19) 0.4772(3) 0.10581(19) 0.0367(8) Uani 1 1 d . . .
N10 N 0.3787(3) 0.6850(4) 0.3977(2) 0.0645(13) Uani 1 1 d . . .
N20 N 0.3947(2) 0.1948(3) 0.2290(2) 0.0478(10) Uani 1 1 d . . .
N30 N 0.1665(2) 0.5185(3) -0.01471(19) 0.0475(10) Uani 1 1 d . . .
O1 O 0.23463(12) 0.45616(19) 0.30060(12) 0.0216(5) Uani 1 1 d . . .
O2 O 0.20823(17) 0.5071(3) 0.40018(16) 0.0442(8) Uani 1 1 d . . .
H2A H 0.1677 0.5168 0.3825 0.066 Uiso 1 1 calc R . .
O3 O 0.23386(12) 0.3545(2) 0.17422(12) 0.0223(5) Uani 1 1 d . . .
O4 O 0.24873(16) 0.2323(2) 0.09538(15) 0.0391(7) Uani 1 1 d . . .
H4A H 0.2896 0.2378 0.1131 0.059 Uiso 1 1 calc R . .
O5 O 0.19060(11) 0.56041(17) 0.17715(11) 0.0167(4) Uani 1 1 d . . .
O6 O 0.08726(13) 0.6184(2) 0.10973(14) 0.0319(6) Uani 1 1 d . . .
H6 H 0.0913 0.5766 0.0801 0.048 Uiso 1 1 calc R . .
O7 O 0.32854(12) 0.50897(17) 0.22831(12) 0.0205(5) Uani 1 1 d . . .
O8 O 0.44203(15) 0.5202(3) 0.27944(17) 0.0424(7) Uani 1 1 d . . .
H8A H 0.4358 0.5476 0.3142 0.064 Uiso 1 1 calc R . .
O9 O 0.06435(16) 0.4973(3) 0.2218(2) 0.0498(8) Uani 1 1 d . . .
O11 O 0.32564(19) 0.6334(3) 0.37516(17) 0.0614(11) Uani 1 1 d . . .
O12 O 0.4319(2) 0.6607(5) 0.3846(2) 0.0920(17) Uani 1 1 d . . .
O13 O 0.3766(4) 0.7589(7) 0.4336(5) 0.196(5) Uani 1 1 d . . .
O21 O 0.38639(19) 0.2934(3) 0.2299(2) 0.0587(10) Uani 1 1 d . . .
O22 O 0.3761(3) 0.1473(4) 0.1736(3) 0.0790(13) Uani 1 1 d . . .
O23 O 0.4175(2) 0.1494(3) 0.2842(3) 0.0742(13) Uani 1 1 d . . .
O31 O 0.1847(2) 0.4568(3) 0.03764(16) 0.0605(11) Uani 1 1 d . . .
O32 O 0.1118(2) 0.5601(4) -0.0254(2) 0.0777(13) Uani 1 1 d . . .
O33 O 0.2066(2) 0.5334(4) -0.0497(2) 0.0709(12) Uani 1 1 d . . .
N40 N 0.0277(6) 0.5199(8) 0.3720(5) 0.052(2) Uiso 0.530(9) 1 d P A 1
O41 O 0.0760(4) 0.5544(7) 0.3440(5) 0.075(3) Uiso 0.530(9) 1 d P A 1
O42 O 0.0600(8) 0.5052(12) 0.4352(9) 0.142(5) Uiso 0.530(9) 1 d P A 1
O43 O -0.0290(13) 0.5356(19) 0.3335(13) 0.195(9) Uiso 0.530(9) 1 d P A 1
N40A N -0.0055(9) 0.4955(12) 0.3613(8) 0.077(4) Uiso 0.470(9) 1 d P A 2
O41A O -0.0356(5) 0.4818(8) 0.3936(5) 0.073(3) Uiso 0.470(9) 1 d P A 2
O43A O 0.0033(9) 0.5631(13) 0.3103(9) 0.127(6) Uiso 0.470(9) 1 d P A 2
O42A O 0.0635(8) 0.4629(13) 0.3813(8) 0.122(5) Uiso 0.470(9) 1 d P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.066(2) . ?
Co1 N3 2.113(3) . ?
Co1 O9 2.114(3) . ?
Co1 N1 2.134(3) . ?
Co1 O5 2.134(2) . ?
Co1 O3 2.188(2) . ?
Co2 O7 2.059(2) . ?
Co2 O11 2.071(3) . ?
Co2 N5 2.103(3) . ?
Co2 O1 2.121(2) . ?
Co2 N7 2.141(3) . ?
Co2 O5 2.253(2) . ?
Co3 O3 2.035(2) . ?
Co3 O21 2.057(3) . ?
Co3 N2 2.082(3) . ?
Co3 O7 2.107(2) . ?
Co3 N4 2.157(3) . ?
Co3 O1 2.236(2) . ?
Co4 O5 2.023(2) . ?
Co4 O31 2.039(3) . ?
Co4 N8 2.085(4) . ?
Co4 O3 2.174(2) . ?
Co4 N6 2.182(3) . ?
Co4 O7 2.195(2) . ?
C1 N1 1.342(5) . ?
C1 C2 1.376(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.366(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.375(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.379(6) . ?
C4 H4 0.9300 . ?
C5 N1 1.329(5) . ?
C5 C6 1.542(6) . ?
C6 O1 1.361(4) . ?
C6 O2 1.407(5) . ?
C6 C7 1.535(6) . ?
C7 N2 1.336(6) . ?
C7 C8 1.387(6) . ?
C8 C9 1.387(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.377(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.375(7) . ?
C10 H10 0.9300 . ?
C11 N2 1.352(6) . ?
C11 H11 0.9300 . ?
C12 N3 1.350(5) . ?
C12 C13 1.376(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.352(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.379(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.397(6) . ?
C15 H15 0.9300 . ?
C16 N3 1.330(5) . ?
C16 C17 1.518(5) . ?
C17 O3 1.360(4) . ?
C17 O4 1.405(5) . ?
C17 C18 1.558(5) . ?
C18 N4 1.336(5) . ?
C18 C19 1.376(6) . ?
C19 C20 1.381(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.357(7) . ?
C20 H20 0.9300 . ?
C21 C22 1.380(7) . ?
C21 H21 0.9300 . ?
C22 N4 1.349(5) . ?
C22 H22 0.9300 . ?
C23 N5 1.342(5) . ?
C23 C24 1.377(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.373(7) . ?
C24 H24 0.9300 . ?
C25 C26 1.379(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.391(6) . ?
C26 H26 0.9300 . ?
C27 N5 1.341(5) . ?
C27 C28 1.519(5) . ?
C28 O5 1.374(4) . ?
C28 O6 1.429(4) . ?
C28 C29 1.534(5) . ?
C29 N6 1.326(5) . ?
C29 C30 1.396(6) . ?
C30 C31 1.383(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.370(7) . ?
C31 H31 0.9300 . ?
C32 C33 1.374(6) . ?
C32 H32 0.9300 . ?
C33 N6 1.349(5) . ?
C33 H33 0.9300 . ?
C34 N7 1.354(5) . ?
C34 C35 1.363(7) . ?
C34 H34 0.9300 . ?
C35 C36 1.361(8) . ?
C35 H35 0.9300 . ?
C36 C37 1.390(7) . ?
C36 H36 0.9300 . ?
C37 C38 1.386(6) . ?
C37 H37 0.9300 . ?
C38 N7 1.317(5) . ?
C38 C39 1.553(5) . ?
C39 O7 1.355(4) . ?
C39 O8 1.408(5) . ?
C39 C40 1.530(6) . ?
C40 N8 1.333(6) . ?
C40 C41 1.388(6) . ?
C41 C42 1.382(8) . ?
C41 H41 0.9300 . ?
C42 C43 1.368(9) . ?
C42 H42 0.9300 . ?
C43 C44 1.367(8) . ?
C43 H43 0.9300 . ?
C44 N8 1.358(6) . ?
C44 H44 0.9300 . ?
N10 O13 1.196(7) . ?
N10 O12 1.227(6) . ?
N10 O11 1.247(5) . ?
N20 O23 1.226(6) . ?
N20 O22 1.234(6) . ?
N20 O21 1.273(5) . ?
N30 O32 1.206(6) . ?
N30 O33 1.227(6) . ?
N30 O31 1.286(5) . ?
O2 H2A 0.8200 . ?
O4 H4A 0.8200 . ?
O6 H6 0.8200 . ?
O8 H8A 0.8200 . ?
N40 O43 1.23(3) . ?
N40 O42 1.277(17) . ?
N40 O41 1.335(13) . ?
N40A O41A 1.022(16) . ?
N40A O43A 1.39(3) . ?
N40A O42A 1.42(2) . ?

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 N3 154.70(12) . . ?
O1 Co1 O9 111.71(13) . . ?
N3 Co1 O9 91.24(14) . . ?
O1 Co1 N1 75.41(12) . . ?
N3 Co1 N1 94.99(13) . . ?
O9 Co1 N1 89.66(13) . . ?
O1 Co1 O5 81.56(9) . . ?
N3 Co1 O5 109.07(11) . . ?
O9 Co1 O5 92.09(11) . . ?
N1 Co1 O5 155.82(11) . . ?
O1 Co1 O3 83.90(9) . . ?
N3 Co1 O3 75.78(11) . . ?
O9 Co1 O3 161.53(12) . . ?
N1 Co1 O3 104.31(11) . . ?
O5 Co1 O3 80.14(9) . . ?
O7 Co2 O11 108.93(14) . . ?
O7 Co2 N5 152.25(11) . . ?
O11 Co2 N5 97.37(15) . . ?
O7 Co2 O1 83.38(9) . . ?
O11 Co2 O1 93.66(12) . . ?
N5 Co2 O1 104.09(11) . . ?
O7 Co2 N7 75.56(11) . . ?
O11 Co2 N7 89.66(14) . . ?
N5 Co2 N7 96.41(13) . . ?
O1 Co2 N7 158.60(11) . . ?
O7 Co2 O5 81.22(9) . . ?
O11 Co2 O5 166.02(12) . . ?
N5 Co2 O5 74.56(10) . . ?
O1 Co2 O5 77.66(8) . . ?
N7 Co2 O5 102.43(11) . . ?
O3 Co3 O21 99.35(14) . . ?
O3 Co3 N2 153.15(12) . . ?
O21 Co3 N2 105.18(16) . . ?
O3 Co3 O7 84.13(10) . . ?
O21 Co3 O7 91.98(11) . . ?
N2 Co3 O7 105.52(12) . . ?
O3 Co3 N4 75.65(11) . . ?
O21 Co3 N4 87.88(13) . . ?
N2 Co3 N4 94.29(14) . . ?
O7 Co3 N4 159.48(11) . . ?
O3 Co3 O1 83.38(9) . . ?
O21 Co3 O1 170.82(12) . . ?
N2 Co3 O1 74.13(12) . . ?
O7 Co3 O1 79.54(9) . . ?
N4 Co3 O1 101.29(11) . . ?
O5 Co4 O31 98.14(14) . . ?
O5 Co4 N8 155.01(12) . . ?
O31 Co4 N8 105.16(16) . . ?
O5 Co4 O3 82.96(9) . . ?
O31 Co4 O3 89.18(11) . . ?
N8 Co4 O3 105.99(12) . . ?
O5 Co4 N6 75.48(11) . . ?
O31 Co4 N6 88.21(13) . . ?
N8 Co4 N6 96.09(13) . . ?
O3 Co4 N6 157.68(11) . . ?
O5 Co4 O7 83.46(9) . . ?
O31 Co4 O7 167.71(11) . . ?
N8 Co4 O7 75.72(12) . . ?
O3 Co4 O7 78.89(9) . . ?
N6 Co4 O7 103.95(11) . . ?
N1 C1 C2 122.6(5) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C3 C2 C1 118.3(5) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C2 C3 C4 119.8(4) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 118.7(4) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 122.1(4) . . ?
N1 C5 C6 116.2(3) . . ?
C4 C5 C6 121.6(4) . . ?
O1 C6 O2 112.2(3) . . ?
O1 C6 C7 107.9(3) . . ?
O2 C6 C7 106.9(3) . . ?
O1 C6 C5 108.0(3) . . ?
O2 C6 C5 109.4(3) . . ?
C7 C6 C5 112.4(3) . . ?
N2 C7 C8 121.4(4) . . ?
N2 C7 C6 115.7(3) . . ?
C8 C7 C6 122.8(4) . . ?
C7 C8 C9 118.9(5) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 H8 120.5 . . ?
C10 C9 C8 119.3(5) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
C11 C10 C9 119.2(5) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
N2 C11 C10 121.5(5) . . ?
N2 C11 H11 119.2 . . ?
C10 C11 H11 119.2 . . ?
N3 C12 C13 122.3(5) . . ?
N3 C12 H12 118.8 . . ?
C13 C12 H12 118.8 . . ?
C14 C13 C12 119.4(5) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 119.2(5) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C14 C15 C16 119.2(5) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
N3 C16 C15 121.4(4) . . ?
N3 C16 C17 115.7(3) . . ?
C15 C16 C17 122.8(4) . . ?
O3 C17 O4 112.5(3) . . ?
O3 C17 C16 110.6(3) . . ?
O4 C17 C16 107.7(3) . . ?
O3 C17 C18 107.3(3) . . ?
O4 C17 C18 109.8(3) . . ?
C16 C17 C18 108.8(3) . . ?
N4 C18 C19 122.1(4) . . ?
N4 C18 C17 115.8(3) . . ?
C19 C18 C17 122.1(4) . . ?
C18 C19 C20 118.7(4) . . ?
C18 C19 H19 120.7 . . ?
C20 C19 H19 120.7 . . ?
C21 C20 C19 119.8(4) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C20 C21 C22 118.9(4) . . ?
C20 C21 H21 120.5 . . ?
C22 C21 H21 120.5 . . ?
N4 C22 C21 121.9(4) . . ?
N4 C22 H22 119.0 . . ?
C21 C22 H22 119.0 . . ?
N5 C23 C24 122.7(4) . . ?
N5 C23 H23 118.6 . . ?
C24 C23 H23 118.6 . . ?
C25 C24 C23 118.5(4) . . ?
C25 C24 H24 120.8 . . ?
C23 C24 H24 120.8 . . ?
C24 C25 C26 119.8(4) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C25 C26 C27 118.6(4) . . ?
C25 C26 H26 120.7 . . ?
C27 C26 H26 120.7 . . ?
N5 C27 C26 121.8(4) . . ?
N5 C27 C28 115.7(3) . . ?
C26 C27 C28 122.4(3) . . ?
O5 C28 O6 110.7(3) . . ?
O5 C28 C27 109.2(3) . . ?
O6 C28 C27 106.2(3) . . ?
O5 C28 C29 108.6(3) . . ?
O6 C28 C29 109.2(3) . . ?
C27 C28 C29 112.9(3) . . ?
N6 C29 C30 122.6(4) . . ?
N6 C29 C28 116.3(3) . . ?
C30 C29 C28 121.0(4) . . ?
C31 C30 C29 118.3(4) . . ?
C31 C30 H30 120.8 . . ?
C29 C30 H30 120.8 . . ?
C32 C31 C30 119.3(4) . . ?
C32 C31 H31 120.3 . . ?
C30 C31 H31 120.3 . . ?
C31 C32 C33 118.9(4) . . ?
C31 C32 H32 120.5 . . ?
C33 C32 H32 120.5 . . ?
N6 C33 C32 122.8(5) . . ?
N6 C33 H33 118.6 . . ?
C32 C33 H33 118.6 . . ?
N7 C34 C35 122.5(5) . . ?
N7 C34 H34 118.7 . . ?
C35 C34 H34 118.7 . . ?
C36 C35 C34 119.1(5) . . ?
C36 C35 H35 120.4 . . ?
C34 C35 H35 120.4 . . ?
C35 C36 C37 119.5(5) . . ?
C35 C36 H36 120.3 . . ?
C37 C36 H36 120.3 . . ?
C38 C37 C36 117.8(5) . . ?
C38 C37 H37 121.1 . . ?
C36 C37 H37 121.1 . . ?
N7 C38 C37 122.9(4) . . ?
N7 C38 C39 115.5(3) . . ?
C37 C38 C39 121.4(4) . . ?
O7 C39 O8 111.1(3) . . ?
O7 C39 C40 108.7(3) . . ?
O8 C39 C40 107.8(3) . . ?
O7 C39 C38 108.0(3) . . ?
O8 C39 C38 109.3(3) . . ?
C40 C39 C38 112.0(3) . . ?
N8 C40 C41 122.4(4) . . ?
N8 C40 C39 115.1(3) . . ?
C41 C40 C39 122.5(4) . . ?
C42 C41 C40 117.5(5) . . ?
C42 C41 H41 121.2 . . ?
C40 C41 H41 121.2 . . ?
C43 C42 C41 120.1(5) . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C44 C43 C42 120.0(5) . . ?
C44 C43 H43 120.0 . . ?
C42 C43 H43 120.0 . . ?
N8 C44 C43 120.7(5) . . ?
N8 C44 H44 119.7 . . ?
C43 C44 H44 119.7 . . ?
C5 N1 C1 118.5(4) . . ?
C5 N1 Co1 115.7(3) . . ?
C1 N1 Co1 125.7(3) . . ?
C7 N2 C11 119.6(4) . . ?
C7 N2 Co3 118.0(3) . . ?
C11 N2 Co3 122.3(3) . . ?
C16 N3 C12 118.5(4) . . ?
C16 N3 Co1 115.6(3) . . ?
C12 N3 Co1 125.9(3) . . ?
C18 N4 C22 118.5(4) . . ?
C18 N4 Co3 114.3(2) . . ?
C22 N4 Co3 127.2(3) . . ?
C27 N5 C23 118.5(3) . . ?
C27 N5 Co2 117.4(2) . . ?
C23 N5 Co2 123.6(3) . . ?
C29 N6 C33 117.9(4) . . ?
C29 N6 Co4 114.0(3) . . ?
C33 N6 Co4 127.6(3) . . ?
C38 N7 C34 118.1(4) . . ?
C38 N7 Co2 115.6(3) . . ?
C34 N7 Co2 126.3(3) . . ?
C40 N8 C44 119.4(4) . . ?
C40 N8 Co4 116.2(3) . . ?
C44 N8 Co4 124.0(3) . . ?
O13 N10 O12 120.4(6) . . ?
O13 N10 O11 118.0(6) . . ?
O12 N10 O11 121.6(5) . . ?
O23 N20 O22 122.1(5) . . ?
O23 N20 O21 118.4(5) . . ?
O22 N20 O21 119.4(5) . . ?
O32 N30 O33 124.0(5) . . ?
O32 N30 O31 118.0(5) . . ?
O33 N30 O31 118.0(5) . . ?
C6 O1 Co1 119.6(2) . . ?
C6 O1 Co2 126.0(2) . . ?
Co1 O1 Co2 103.39(10) . . ?
C6 O1 Co3 111.5(2) . . ?
Co1 O1 Co3 94.22(9) . . ?
Co2 O1 Co3 95.00(10) . . ?
C6 O2 H2A 109.5 . . ?
C17 O3 Co3 119.9(2) . . ?
C17 O3 Co4 128.6(2) . . ?
Co3 O3 Co4 99.65(10) . . ?
C17 O3 Co1 110.4(2) . . ?
Co3 O3 Co1 96.60(10) . . ?
Co4 O3 Co1 94.86(10) . . ?
C17 O4 H4A 109.5 . . ?
C28 O5 Co4 120.1(2) . . ?
C28 O5 Co1 126.4(2) . . ?
Co4 O5 Co1 101.13(9) . . ?
C28 O5 Co2 109.91(19) . . ?
Co4 O5 Co2 96.09(9) . . ?
Co1 O5 Co2 96.95(9) . . ?
C28 O6 H6 109.5 . . ?
C39 O7 Co2 118.6(2) . . ?
C39 O7 Co3 127.6(2) . . ?
Co2 O7 Co3 100.91(10) . . ?
C39 O7 Co4 110.1(2) . . ?
Co2 O7 Co4 96.84(10) . . ?
Co3 O7 Co4 96.76(10) . . ?
C39 O8 H8A 109.5 . . ?
N10 O11 Co2 130.5(4) . . ?
N20 O21 Co3 122.0(3) . . ?
N30 O31 Co4 122.3(3) . . ?
O43 N40 O42 143.3(17) . . ?
O43 N40 O41 111.2(15) . . ?
O42 N40 O41 102.8(11) . . ?
O41A N40A O43A 142.6(18) . . ?
O41A N40A O42A 119.4(17) . . ?
O43A N40A O42A 94.3(15) . . ?

_diffrn_measured_fraction_theta_max 0.946
_diffrn_reflns_theta_full        28.36
_diffrn_measured_fraction_theta_full 0.946
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.100


