data_global

_journal_coden_Cambridge         222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Philip Gale'
'Gareth W Bates'
'Mark E Light'
'Mark Ogden'
'Colin N. Warriner'

_publ_contact_author_name        'Philip Gale'
_publ_contact_author_email       PHILIP.GALE@SOTON.AC.UK

_publ_section_title              
;
Structural diversity in the first metal complexes of
2,5-dicarboxamidopyrroles and
2,5-dicarbothioamidopyrroles
;

# Attachment '0925_1251_1397_0393_0637_1194_0773.cif'

data_2005sot0925
_database_code_depnum_ccdc_archive 'CCDC 678031'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C63 H48 Co K3 N14 O25'
_chemical_formula_weight         1577.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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/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                   14.6300(16)
_cell_length_b                   29.024(3)
_cell_length_c                   15.4370(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.507(2)
_cell_angle_gamma                90.00
_cell_volume                     6524.6(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5503
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      22.80

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3232
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9572
_exptl_absorpt_correction_T_max  0.9945
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
;
absolute Tmin and Tmax unknown, but SADABS gives ratio as 0.592
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.6814
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD diffractometer'
_diffrn_measurement_method       'fine-slice \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        5
_diffrn_reflns_number            48591
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_av_sigmaI/netI    0.0783
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.92
_diffrn_reflns_theta_max         25.03
_reflns_number_total             11503
_reflns_number_gt                7382
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin, et al., 1993)'
_computing_publication_material  'WINGX (Farrugia, 1998)'

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

Most of the CheckCIF alerts are due to the disorder in one of the solvent
molecules or coordination radius used by the program for K.

The crystals were weakly diffracting and have a low completeness to theta
max
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1644P)^2^+24.3354P] where P=(Fo^2^+2Fc^2^)/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         11503
_refine_ls_number_parameters     945
_refine_ls_number_restraints     64
_refine_ls_R_factor_all          0.1330
_refine_ls_R_factor_gt           0.0866
_refine_ls_wR_factor_ref         0.2854
_refine_ls_wR_factor_gt          0.2436
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.001

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 0.64923(2) 0.126977(12) 0.10027(2) 0.02376(9) Uani 1 1 d . . .
N1 N 0.46654(16) 0.03004(8) -0.16751(14) 0.0308(6) Uani 1 1 d . . .
N2 N 0.23149(15) 0.13052(8) -0.06394(15) 0.0324(6) Uani 1 1 d . . .
N3 N 0.52397(15) 0.10266(8) 0.11388(13) 0.0265(6) Uani 1 1 d . . .
N4 N 0.64559(15) 0.12919(7) 0.21768(13) 0.0241(6) Uani 1 1 d . . .
N5 N 0.77696(15) 0.14939(8) 0.14037(13) 0.0257(6) Uani 1 1 d . . .
N6 N 0.90314(15) 0.16651(8) -0.13676(14) 0.0298(6) Uani 1 1 d . . .
N7 N 1.07786(17) 0.08238(9) 0.09900(17) 0.0407(7) Uani 1 1 d . . .
O1 O 0.53265(14) 0.00465(7) -0.14790(12) 0.0362(6) Uani 1 1 d . . .
O2 O 0.42893(14) 0.03378(8) -0.24148(12) 0.0399(6) Uani 1 1 d . . .
O3 O 0.21410(14) 0.16135(7) -0.01352(14) 0.0404(6) Uani 1 1 d . . .
O4 O 0.17834(13) 0.11821(7) -0.12583(13) 0.0378(6) Uani 1 1 d . . .
O5 O 0.41463(12) 0.09728(7) 0.21271(12) 0.0316(5) Uani 1 1 d . . .
O6 O 0.87146(13) 0.16519(7) 0.26659(12) 0.0344(5) Uani 1 1 d . . .
O7 O 0.83566(14) 0.19042(7) -0.16062(12) 0.0373(6) Uani 1 1 d . . .
O8 O 0.96197(14) 0.15660(7) -0.18519(12) 0.0402(6) Uani 1 1 d . . .
O9 O 1.13722(14) 0.07515(8) 0.05067(15) 0.0515(7) Uani 1 1 d . . .
O10 O 1.08112(17) 0.06795(10) 0.17374(15) 0.0658(8) Uani 1 1 d . . .
C1 C 0.48601(18) 0.06249(9) -0.02056(16) 0.0283(7) Uani 1 1 d . . .
H1 H 0.5392 0.0450 -0.0100 0.034 Uiso 1 1 calc R . .
C2 C 0.43129(18) 0.05834(9) -0.09822(16) 0.0257(7) Uani 1 1 d . . .
C3 C 0.34731(18) 0.07952(10) -0.11490(16) 0.0286(7) Uani 1 1 d . . .
H3 H 0.3108 0.0754 -0.1670 0.034 Uiso 1 1 calc R . .
C4 C 0.32104(18) 0.10706(9) -0.04969(17) 0.0281(7) Uani 1 1 d . . .
C5 C 0.37536(18) 0.11594(9) 0.02770(17) 0.0270(7) Uani 1 1 d . . .
H5 H 0.3556 0.1362 0.0687 0.032 Uiso 1 1 calc R . .
C6 C 0.45969(18) 0.09377(9) 0.04228(16) 0.0256(7) Uani 1 1 d . . .
C7 C 0.49543(18) 0.10501(9) 0.19478(16) 0.0268(7) Uani 1 1 d . . .
C8 C 0.57187(18) 0.11825(9) 0.25894(16) 0.0266(7) Uani 1 1 d . . .
C9 C 0.59244(18) 0.12761(9) 0.34908(17) 0.0266(7) Uani 1 1 d . . .
C10 C 0.68330(18) 0.14625(10) 0.35770(16) 0.0275(7) Uani 1 1 d . . .
C11 C 0.71307(17) 0.14652(9) 0.27334(16) 0.0253(7) Uani 1 1 d . . .
C12 C 0.79515(18) 0.15463(9) 0.22821(17) 0.0273(7) Uani 1 1 d . . .
C13 C 0.85143(18) 0.14279(9) 0.09036(16) 0.0277(7) Uani 1 1 d . . .
C14 C 0.84490(18) 0.15923(10) 0.00526(17) 0.0282(7) Uani 1 1 d . . .
H14 H 0.7944 0.1767 -0.0161 0.034 Uiso 1 1 calc R . .
C15 C 0.91372(18) 0.14955(10) -0.04722(16) 0.0288(7) Uani 1 1 d . . .
C16 C 0.99197(19) 0.12498(10) -0.01936(19) 0.0330(8) Uani 1 1 d . . .
H16 H 1.0383 0.1193 -0.0552 0.040 Uiso 1 1 calc R . .
C17 C 0.99637(19) 0.10963(10) 0.06461(18) 0.0308(7) Uani 1 1 d . . .
C18 C 0.92858(19) 0.11732(9) 0.11992(17) 0.0287(7) Uani 1 1 d . . .
H18 H 0.9347 0.1055 0.1762 0.034 Uiso 1 1 calc R . .
C19 C 0.53351(18) 0.11699(9) 0.41816(16) 0.0260(7) Uani 1 1 d . . .
C20 C 0.48212(19) 0.07668(10) 0.41660(17) 0.0314(8) Uani 1 1 d . . .
H20 H 0.4850 0.0563 0.3705 0.038 Uiso 1 1 calc R . .
C21 C 0.4273(2) 0.06610(10) 0.48104(17) 0.0347(8) Uani 1 1 d . . .
H21 H 0.3937 0.0389 0.4783 0.042 Uiso 1 1 calc R . .
C22 C 0.42200(19) 0.09662(11) 0.55165(17) 0.0340(8) Uani 1 1 d . . .
H22 H 0.3851 0.0896 0.5957 0.041 Uiso 1 1 calc R . .
C23 C 0.47204(19) 0.13679(10) 0.55438(16) 0.0306(7) Uani 1 1 d . . .
H23 H 0.4691 0.1572 0.6005 0.037 Uiso 1 1 calc R . .
C24 C 0.52705(18) 0.14706(10) 0.48843(16) 0.0276(7) Uani 1 1 d . . .
H24 H 0.5603 0.1744 0.4909 0.033 Uiso 1 1 calc R . .
C25 C 0.73979(17) 0.16231(9) 0.43663(16) 0.0264(7) Uani 1 1 d . . .
C26 C 0.75714(19) 0.13408(10) 0.50907(18) 0.0329(8) Uani 1 1 d . . .
H26 H 0.7310 0.1049 0.5089 0.039 Uiso 1 1 calc R . .
C27 C 0.8127(2) 0.14876(12) 0.58145(19) 0.0400(9) Uani 1 1 d . . .
H27 H 0.8235 0.1293 0.6293 0.048 Uiso 1 1 calc R . .
C28 C 0.8521(2) 0.19173(13) 0.58334(19) 0.0474(10) Uani 1 1 d . . .
H28 H 0.8891 0.2017 0.6321 0.057 Uiso 1 1 calc R . .
C29 C 0.8358(2) 0.22014(13) 0.5108(2) 0.0510(10) Uani 1 1 d . . .
H29 H 0.8626 0.2492 0.5112 0.061 Uiso 1 1 calc R . .
C30 C 0.7807(2) 0.20598(11) 0.43881(18) 0.0377(8) Uani 1 1 d . . .
H30 H 0.7705 0.2255 0.3911 0.045 Uiso 1 1 calc R . .
N8 N 0.74074(17) -0.00112(9) 0.36369(15) 0.0377(7) Uani 1 1 d . . .
N9 N 0.96756(16) -0.03275(8) 0.15948(16) 0.0335(7) Uani 1 1 d . . .
N10 N 0.70474(15) 0.06589(8) 0.07284(13) 0.0264(6) Uani 1 1 d . . .
N11 N 0.64532(14) 0.12990(8) -0.01821(13) 0.0245(6) Uani 1 1 d . . .
N12 N 0.59960(15) 0.19053(8) 0.07480(13) 0.0263(6) Uani 1 1 d . . .
N13 N 0.76840(18) 0.30918(10) 0.24600(18) 0.0466(8) Uani 1 1 d . . .
N14 N 0.49320(17) 0.23901(8) 0.34684(15) 0.0366(7) Uani 1 1 d . . .
O11 O 0.68123(15) 0.02389(8) 0.38478(12) 0.0436(6) Uani 1 1 d . . .
O12 O 0.77590(17) -0.03163(9) 0.41154(14) 0.0596(8) Uani 1 1 d . . .
O13 O 1.00447(14) -0.05992(8) 0.21382(14) 0.0463(6) Uani 1 1 d . . .
O14 O 1.00013(15) -0.02338(9) 0.09125(14) 0.0513(7) Uani 1 1 d . . .
O15 O 0.73959(13) 0.02105(6) -0.04493(11) 0.0304(5) Uani 1 1 d . . .
O16 O 0.58314(13) 0.24544(7) -0.03469(12) 0.0325(5) Uani 1 1 d . . .
O17 O 0.79510(17) 0.32764(9) 0.18266(18) 0.0635(8) Uani 1 1 d . . .
O18 O 0.80494(15) 0.31215(9) 0.32002(16) 0.0578(7) Uani 1 1 d . . .
O19 O 0.42191(14) 0.21740(8) 0.32646(14) 0.0435(6) Uani 1 1 d . . .
O20 O 0.51308(16) 0.25579(7) 0.41898(12) 0.0430(6) Uani 1 1 d . . .
C31 C 0.72447(19) 0.03166(9) 0.21730(16) 0.0282(7) Uani 1 1 d . . .
H31 H 0.6716 0.0465 0.2317 0.034 Uiso 1 1 calc R . .
C32 C 0.7733(2) 0.00464(10) 0.27702(17) 0.0319(8) Uani 1 1 d . . .
C33 C 0.8521(2) -0.01925(10) 0.26091(18) 0.0345(8) Uani 1 1 d . . .
H33 H 0.8829 -0.0388 0.3017 0.041 Uiso 1 1 calc R . .
C34 C 0.88133(18) -0.01173(10) 0.17921(17) 0.0299(7) Uani 1 1 d . . .
C35 C 0.83510(18) 0.01510(9) 0.11596(17) 0.0283(7) Uani 1 1 d . . .
H35 H 0.8576 0.0185 0.0620 0.034 Uiso 1 1 calc R . .
C36 C 0.75368(18) 0.03734(9) 0.13358(17) 0.0275(7) Uani 1 1 d . . .
C37 C 0.71156(17) 0.05701(9) -0.01485(16) 0.0252(7) Uani 1 1 d . . .
C38 C 0.67633(17) 0.09662(9) -0.06799(16) 0.0245(7) Uani 1 1 d . . .
C39 C 0.66356(18) 0.11106(10) -0.15572(16) 0.0267(7) Uani 1 1 d . . .
C40 C 0.62234(18) 0.15540(9) -0.15421(16) 0.0266(7) Uani 1 1 d . . .
C41 C 0.61345(18) 0.16574(9) -0.06577(16) 0.0267(7) Uani 1 1 d . . .
C42 C 0.59531(18) 0.20445(9) -0.00935(16) 0.0269(7) Uani 1 1 d . . .
C43 C 0.60453(18) 0.22276(9) 0.14208(17) 0.0266(7) Uani 1 1 d . . .
C44 C 0.67699(19) 0.25380(10) 0.15339(17) 0.0316(8) Uani 1 1 d . . .
H44 H 0.7173 0.2576 0.1109 0.038 Uiso 1 1 calc R . .
C45 C 0.6874(2) 0.27931(10) 0.2311(2) 0.0360(8) Uani 1 1 d . . .
C46 C 0.6309(2) 0.27518(10) 0.29681(19) 0.0355(8) Uani 1 1 d . . .
H46 H 0.6411 0.2914 0.3488 0.043 Uiso 1 1 calc R . .
C47 C 0.55806(19) 0.24536(10) 0.28023(17) 0.0318(7) Uani 1 1 d . . .
C48 C 0.54163(18) 0.21990(9) 0.20419(17) 0.0280(7) Uani 1 1 d . . .
H48 H 0.4898 0.2013 0.1949 0.034 Uiso 1 1 calc R . .
C49 C 0.68687(18) 0.08344(9) -0.23164(16) 0.0264(7) Uani 1 1 d . . .
C50 C 0.77439(18) 0.06473(10) -0.23254(17) 0.0293(7) Uani 1 1 d . . .
H50 H 0.8190 0.0708 -0.1870 0.035 Uiso 1 1 calc R . .
C51 C 0.7951(2) 0.03723(10) -0.30059(18) 0.0338(8) Uani 1 1 d . . .
H51 H 0.8533 0.0242 -0.3000 0.041 Uiso 1 1 calc R . .
C52 C 0.7296(2) 0.02866(10) -0.37057(18) 0.0364(8) Uani 1 1 d . . .
H52 H 0.7438 0.0100 -0.4164 0.044 Uiso 1 1 calc R . .
C53 C 0.6438(2) 0.04812(10) -0.37080(17) 0.0335(8) Uani 1 1 d . . .
H53 H 0.6000 0.0431 -0.4176 0.040 Uiso 1 1 calc R . .
C54 C 0.6223(2) 0.07528(10) -0.30143(16) 0.0312(7) Uani 1 1 d . . .
H54 H 0.5640 0.0881 -0.3019 0.037 Uiso 1 1 calc R . .
C55 C 0.59481(19) 0.18704(9) -0.22754(16) 0.0282(7) Uani 1 1 d . . .
C56 C 0.6520(2) 0.19521(10) -0.29377(17) 0.0329(8) Uani 1 1 d . . .
H56 H 0.7071 0.1793 -0.2939 0.039 Uiso 1 1 calc R . .
C57 C 0.6271(2) 0.22675(10) -0.35904(17) 0.0380(8) Uani 1 1 d . . .
H57 H 0.6655 0.2317 -0.4028 0.046 Uiso 1 1 calc R . .
C58 C 0.5462(2) 0.25086(10) -0.35977(18) 0.0415(9) Uani 1 1 d . . .
H58 H 0.5300 0.2720 -0.4039 0.050 Uiso 1 1 calc R . .
C59 C 0.4892(2) 0.24377(11) -0.29511(18) 0.0392(8) Uani 1 1 d . . .
H59 H 0.4347 0.2603 -0.2954 0.047 Uiso 1 1 calc R . .
C60 C 0.5131(2) 0.21172(10) -0.22888(17) 0.0317(8) Uani 1 1 d . . .
H60 H 0.4741 0.2069 -0.1856 0.038 Uiso 1 1 calc R . .
C61 C 1.0280(3) 0.09665(14) 0.5621(3) 0.0935(6) Uani 1 1 d DU . .
H61A H 1.0599 0.0679 0.5705 0.140 Uiso 1 1 calc R . .
H61B H 1.0307 0.1069 0.5033 0.140 Uiso 1 1 calc R . .
H61C H 0.9650 0.0926 0.5731 0.140 Uiso 1 1 calc R . .
O21 O 1.0703(2) 0.13042(11) 0.6210(2) 0.0935(6) Uani 1 1 d DU . .
H21A H 1.0702 0.1211 0.6711 0.140 Uiso 1 1 calc R . .
C62A C 0.2009(5) 0.10137(16) 0.4485(7) 0.0935(6) Uani 0.50 1 d PDU A 1
H62A H 0.1778 0.0903 0.5008 0.140 Uiso 0.50 1 calc PR A 1
H62B H 0.2453 0.0799 0.4302 0.140 Uiso 0.50 1 calc PR A 1
H62C H 0.1512 0.1043 0.4036 0.140 Uiso 0.50 1 calc PR A 1
O22A O 0.2422(4) 0.14394(15) 0.4641(4) 0.0935(6) Uani 0.50 1 d PDU A 1
H22A H 0.2209 0.1563 0.5055 0.140 Uiso 0.50 1 calc PR A 1
O22B O 0.0630(5) 0.16144(13) 0.4935(4) 0.0935(6) Uani 0.50 1 d PDU B 2
H22B H 0.0109 0.1721 0.4904 0.140 Uiso 0.50 1 calc PR B 2
C62B C 0.0585(8) 0.11301(15) 0.4710(6) 0.0935(6) Uani 0.50 1 d PD B 2
H62D H 0.0768 0.1089 0.4134 0.140 Uiso 0.50 1 calc PR B 2
H62E H -0.0032 0.1021 0.4729 0.140 Uiso 0.50 1 calc PR B 2
H62F H 0.0990 0.0959 0.5118 0.140 Uiso 0.50 1 calc PR B 2
C63 C 0.2694(3) 0.11559(15) 0.2940(3) 0.0935(6) Uani 1 1 d DU . .
H63A H 0.2259 0.1004 0.3270 0.140 Uiso 1 1 calc R . .
H63B H 0.3055 0.0930 0.2672 0.140 Uiso 1 1 calc R . .
H63C H 0.2372 0.1343 0.2497 0.140 Uiso 1 1 calc R . .
O23 O 0.3262(2) 0.14305(11) 0.3484(2) 0.0935(6) Uani 1 1 d DU . .
H23A H 0.3070 0.1439 0.3966 0.140 Uiso 1 1 calc R . .
O24 O 0.8367(3) 0.27178(10) 0.0109(2) 0.1251(11) Uani 1 1 d DU . .
H99 H 0.8516(8) 0.24787(12) 0.0397(5) 0.120 Uiso 1 1 d D . .
H98 H 0.8745(4) 0.29358(14) 0.0226(10) 0.120 Uiso 1 1 d D . .
O25 O 0.6069(2) 0.33460(13) 0.7885(2) 0.1251(11) Uani 1 1 d DU . .
H96 H 0.5502(2) 0.3319(4) 0.7892(6) 0.120 Uiso 1 1 d D . .
H97 H 0.6311(3) 0.3164(2) 0.7558(4) 0.120 Uiso 1 1 d D . .
K1 K 0.72766(8) 0.26911(4) 0.86352(8) 0.0897(4) Uani 1 1 d . . .
K2 K 0.28796(4) 0.03455(2) 0.17467(4) 0.03421(17) Uani 1 1 d . . .
K3 K 0.98649(7) 0.18696(3) 0.39724(7) 0.0747(3) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.02538(16) 0.02817(17) 0.01801(15) -0.00040(14) 0.00361(13) 0.00075(15)
N1 0.0361(12) 0.0343(12) 0.0223(10) -0.0062(9) 0.0042(9) -0.0086(10)
N2 0.0259(11) 0.0415(13) 0.0303(11) 0.0043(10) 0.0058(9) 0.0008(10)
N3 0.0296(11) 0.0310(11) 0.0190(10) -0.0012(9) 0.0025(9) 0.0010(10)
N4 0.0284(10) 0.0234(10) 0.0209(10) -0.0018(9) 0.0041(9) 0.0002(9)
N5 0.0280(10) 0.0306(11) 0.0193(10) 0.0008(9) 0.0065(9) 0.0012(9)
N6 0.0299(11) 0.0362(12) 0.0246(10) 0.0012(10) 0.0086(9) -0.0083(10)
N7 0.0371(13) 0.0385(13) 0.0472(14) 0.0041(12) 0.0070(11) 0.0106(11)
O1 0.0392(10) 0.0399(11) 0.0299(9) -0.0020(9) 0.0052(8) 0.0079(9)
O2 0.0403(11) 0.0551(13) 0.0240(9) -0.0045(9) 0.0014(8) -0.0060(10)
O3 0.0363(10) 0.0415(11) 0.0437(11) -0.0006(10) 0.0043(9) 0.0088(9)
O4 0.0263(9) 0.0512(12) 0.0352(10) 0.0030(9) -0.0006(8) 0.0011(9)
O5 0.0271(9) 0.0397(10) 0.0283(9) -0.0012(8) 0.0034(8) -0.0021(8)
O6 0.0297(9) 0.0484(11) 0.0257(9) -0.0039(9) 0.0062(8) -0.0063(9)
O7 0.0367(10) 0.0456(11) 0.0301(10) 0.0080(9) 0.0053(8) -0.0031(9)
O8 0.0437(11) 0.0514(12) 0.0277(9) -0.0049(9) 0.0150(8) -0.0064(10)
O9 0.0374(10) 0.0597(13) 0.0610(13) 0.0184(11) 0.0229(10) 0.0196(10)
O10 0.0588(13) 0.1010(18) 0.0376(12) 0.0167(13) 0.0053(11) 0.0389(13)
C1 0.0296(13) 0.0325(14) 0.0230(12) 0.0036(11) 0.0034(11) -0.0060(12)
C2 0.0310(13) 0.0275(13) 0.0194(11) -0.0023(10) 0.0065(10) -0.0042(11)
C3 0.0267(13) 0.0361(14) 0.0221(12) 0.0031(11) -0.0015(11) -0.0014(12)
C4 0.0294(13) 0.0287(13) 0.0267(12) 0.0074(11) 0.0048(11) 0.0040(11)
C5 0.0312(13) 0.0256(13) 0.0255(12) 0.0010(11) 0.0089(11) -0.0032(11)
C6 0.0282(12) 0.0303(13) 0.0190(11) 0.0024(10) 0.0057(10) -0.0065(11)
C7 0.0313(13) 0.0271(13) 0.0225(12) 0.0005(11) 0.0048(11) 0.0005(11)
C8 0.0289(12) 0.0279(13) 0.0241(12) 0.0007(11) 0.0081(10) 0.0024(11)
C9 0.0291(13) 0.0272(13) 0.0233(12) -0.0017(11) 0.0022(11) 0.0070(11)
C10 0.0292(13) 0.0326(14) 0.0215(12) 0.0034(11) 0.0058(10) 0.0015(12)
C11 0.0245(12) 0.0288(13) 0.0226(12) -0.0001(11) 0.0027(10) -0.0005(11)
C12 0.0276(13) 0.0308(13) 0.0231(12) 0.0012(11) 0.0001(11) 0.0017(11)
C13 0.0312(13) 0.0293(13) 0.0242(12) -0.0017(11) 0.0100(11) -0.0035(11)
C14 0.0243(12) 0.0343(14) 0.0264(13) -0.0031(11) 0.0040(11) -0.0021(11)
C15 0.0327(13) 0.0361(14) 0.0180(11) -0.0037(11) 0.0044(11) -0.0038(12)
C16 0.0273(13) 0.0355(15) 0.0378(14) -0.0039(12) 0.0111(11) -0.0007(12)
C17 0.0277(13) 0.0327(14) 0.0321(14) 0.0006(12) 0.0036(11) 0.0032(12)
C18 0.0328(13) 0.0328(14) 0.0205(12) -0.0023(11) 0.0028(11) -0.0031(12)
C19 0.0274(12) 0.0325(13) 0.0180(11) 0.0014(11) 0.0012(10) 0.0032(11)
C20 0.0372(14) 0.0368(15) 0.0199(12) -0.0019(11) 0.0016(11) -0.0010(13)
C21 0.0408(15) 0.0361(15) 0.0279(13) -0.0017(12) 0.0068(12) -0.0084(13)
C22 0.0280(13) 0.0533(17) 0.0215(12) 0.0007(13) 0.0060(11) -0.0033(13)
C23 0.0373(14) 0.0416(15) 0.0143(11) -0.0027(11) 0.0093(10) -0.0016(13)
C24 0.0283(13) 0.0312(13) 0.0228(12) -0.0026(11) 0.0003(11) 0.0010(11)
C25 0.0244(12) 0.0367(14) 0.0188(11) -0.0015(11) 0.0061(10) -0.0005(11)
C26 0.0317(14) 0.0386(15) 0.0286(13) -0.0019(12) 0.0041(12) 0.0018(12)
C27 0.0338(15) 0.0614(19) 0.0247(13) 0.0016(14) 0.0025(12) 0.0000(15)
C28 0.0399(16) 0.074(2) 0.0269(14) -0.0114(15) -0.0022(13) -0.0099(16)
C29 0.061(2) 0.0551(19) 0.0362(16) -0.0027(15) -0.0003(15) -0.0218(17)
C30 0.0402(15) 0.0482(17) 0.0241(13) -0.0006(13) 0.0006(12) -0.0165(14)
N8 0.0341(12) 0.0513(15) 0.0275(11) 0.0056(11) 0.0015(10) -0.0003(12)
N9 0.0280(11) 0.0318(12) 0.0397(13) -0.0053(11) -0.0013(10) 0.0021(10)
N10 0.0291(11) 0.0302(11) 0.0198(10) 0.0018(9) 0.0023(9) 0.0019(10)
N11 0.0239(10) 0.0316(11) 0.0184(9) 0.0037(9) 0.0035(8) 0.0005(9)
N12 0.0274(11) 0.0290(11) 0.0224(10) -0.0010(9) 0.0021(9) 0.0027(9)
N13 0.0395(14) 0.0463(15) 0.0557(15) -0.0154(13) 0.0132(12) -0.0024(12)
N14 0.0499(13) 0.0341(12) 0.0286(11) -0.0001(10) 0.0184(10) 0.0113(11)
O11 0.0512(12) 0.0540(12) 0.0267(10) 0.0039(9) 0.0097(9) 0.0110(11)
O12 0.0599(14) 0.0795(16) 0.0410(11) 0.0300(11) 0.0130(11) 0.0234(13)
O13 0.0367(11) 0.0518(13) 0.0496(12) 0.0126(11) -0.0008(10) 0.0115(10)
O14 0.0469(12) 0.0671(14) 0.0422(11) 0.0084(11) 0.0160(10) 0.0197(11)
O15 0.0359(10) 0.0304(9) 0.0245(9) -0.0016(8) 0.0014(8) 0.0043(8)
O16 0.0389(10) 0.0329(10) 0.0258(9) 0.0008(8) 0.0037(8) 0.0058(9)
O17 0.0597(14) 0.0604(15) 0.0718(16) -0.0068(13) 0.0127(13) -0.0268(12)
O18 0.0389(12) 0.0745(15) 0.0602(13) -0.0360(12) 0.0058(11) -0.0067(11)
O19 0.0442(11) 0.0463(12) 0.0434(11) -0.0021(10) 0.0210(9) -0.0032(10)
O20 0.0662(13) 0.0397(11) 0.0238(9) -0.0037(9) 0.0079(9) 0.0130(10)
C31 0.0297(13) 0.0317(14) 0.0233(12) -0.0010(11) 0.0021(11) 0.0015(12)
C32 0.0364(14) 0.0347(14) 0.0246(13) 0.0050(12) 0.0029(11) 0.0000(13)
C33 0.0368(15) 0.0415(16) 0.0244(13) 0.0038(12) -0.0011(12) 0.0045(13)
C34 0.0266(13) 0.0331(14) 0.0304(13) -0.0033(12) 0.0054(11) 0.0041(11)
C35 0.0274(13) 0.0301(14) 0.0271(13) -0.0032(11) 0.0011(11) 0.0009(11)
C36 0.0305(13) 0.0265(13) 0.0254(12) -0.0039(11) 0.0014(11) -0.0027(11)
C37 0.0212(11) 0.0312(13) 0.0234(12) 0.0010(11) 0.0035(10) -0.0034(11)
C38 0.0235(12) 0.0296(13) 0.0206(11) -0.0012(10) 0.0033(10) 0.0006(11)
C39 0.0250(12) 0.0350(14) 0.0202(12) -0.0024(11) 0.0025(10) 0.0015(11)
C40 0.0260(12) 0.0332(14) 0.0205(12) 0.0041(11) 0.0025(10) 0.0043(11)
C41 0.0286(13) 0.0319(14) 0.0194(11) 0.0027(11) 0.0020(10) 0.0012(11)
C42 0.0271(12) 0.0309(14) 0.0234(12) 0.0029(11) 0.0060(10) 0.0026(11)
C43 0.0270(12) 0.0267(13) 0.0265(12) 0.0026(11) 0.0049(10) 0.0072(11)
C44 0.0305(13) 0.0371(15) 0.0281(13) -0.0012(12) 0.0079(11) 0.0041(12)
C45 0.0329(14) 0.0305(14) 0.0446(16) -0.0088(13) 0.0040(13) -0.0017(12)
C46 0.0384(15) 0.0373(15) 0.0310(14) -0.0074(12) 0.0050(12) 0.0040(13)
C47 0.0325(13) 0.0399(15) 0.0235(12) 0.0054(12) 0.0047(11) 0.0068(12)
C48 0.0272(13) 0.0314(14) 0.0258(12) -0.0020(11) 0.0041(11) 0.0026(11)
C49 0.0327(13) 0.0311(13) 0.0164(11) 0.0026(10) 0.0070(10) -0.0003(12)
C50 0.0287(13) 0.0352(14) 0.0246(12) -0.0053(11) 0.0047(11) -0.0031(12)
C51 0.0305(14) 0.0399(15) 0.0308(14) -0.0016(12) 0.0025(12) 0.0024(13)
C52 0.0504(17) 0.0346(15) 0.0252(13) -0.0059(12) 0.0088(12) -0.0033(14)
C53 0.0380(15) 0.0407(16) 0.0218(12) -0.0019(12) 0.0022(11) 0.0020(13)
C54 0.0368(14) 0.0359(15) 0.0208(12) 0.0025(11) 0.0025(11) -0.0003(12)
C55 0.0367(14) 0.0303(13) 0.0178(11) -0.0017(11) 0.0038(11) -0.0005(12)
C56 0.0375(15) 0.0344(15) 0.0266(13) 0.0009(12) 0.0020(12) 0.0022(13)
C57 0.0588(18) 0.0378(15) 0.0181(12) 0.0005(12) 0.0070(13) -0.0093(14)
C58 0.067(2) 0.0316(15) 0.0245(13) 0.0042(12) -0.0041(14) 0.0113(15)
C59 0.0519(17) 0.0378(15) 0.0263(14) -0.0029(12) -0.0051(13) 0.0153(14)
C60 0.0382(15) 0.0350(14) 0.0215(12) 0.0017(11) 0.0013(11) 0.0050(13)
C61 0.0966(10) 0.0931(10) 0.0924(10) -0.0085(8) 0.0165(8) 0.0080(9)
O21 0.0966(10) 0.0931(10) 0.0924(10) -0.0085(8) 0.0165(8) 0.0080(9)
C62A 0.0966(10) 0.0931(10) 0.0924(10) -0.0085(8) 0.0165(8) 0.0080(9)
O22A 0.0966(10) 0.0931(10) 0.0924(10) -0.0085(8) 0.0165(8) 0.0080(9)
O22B 0.0966(10) 0.0931(10) 0.0924(10) -0.0085(8) 0.0165(8) 0.0080(9)
C62B 0.0966(10) 0.0931(10) 0.0924(10) -0.0085(8) 0.0165(8) 0.0080(9)
C63 0.0966(10) 0.0931(10) 0.0924(10) -0.0085(8) 0.0165(8) 0.0080(9)
O23 0.0966(10) 0.0931(10) 0.0924(10) -0.0085(8) 0.0165(8) 0.0080(9)
O24 0.146(2) 0.1165(18) 0.1115(18) 0.0006(15) 0.0072(16) -0.0392(16)
O25 0.146(2) 0.1165(18) 0.1115(18) 0.0006(15) 0.0072(16) -0.0392(16)
K1 0.0850(6) 0.0757(6) 0.1153(8) -0.0022(6) 0.0446(5) -0.0128(5)
K2 0.0349(3) 0.0360(3) 0.0320(3) -0.0071(3) 0.0045(3) -0.0029(3)
K3 0.0706(5) 0.0587(5) 0.0884(6) -0.0012(5) -0.0259(5) -0.0092(4)

_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 N4 1.819(2) . ?
Co1 N11 1.826(2) . ?
Co1 N3 1.994(2) . ?
Co1 N12 2.007(2) . ?
Co1 N10 2.012(2) . ?
Co1 N5 2.019(2) . ?
N1 O2 1.224(3) . ?
N1 O1 1.230(3) . ?
N1 C2 1.480(3) . ?
N2 O4 1.226(3) . ?
N2 O3 1.228(3) . ?
N2 C4 1.474(3) . ?
N3 C7 1.356(3) . ?
N3 C6 1.405(3) . ?
N4 C8 1.342(3) . ?
N4 C11 1.343(3) . ?
N5 C12 1.365(3) . ?
N5 C13 1.407(3) . ?
N6 O8 1.227(3) . ?
N6 O7 1.234(3) . ?
N6 C15 1.461(3) . ?
N7 O9 1.216(3) . ?
N7 O10 1.224(3) . ?
N7 C17 1.486(4) . ?
O1 K2 2.926(2) 3_655 ?
O5 C7 1.260(3) . ?
O5 K2 2.624(2) . ?
O6 C12 1.251(3) . ?
O6 K3 2.578(2) . ?
O7 K1 2.822(2) 1_554 ?
O9 K2 3.018(2) 1_655 ?
O10 K2 3.176(3) 1_655 ?
C1 C2 1.381(3) . ?
C1 C6 1.409(4) . ?
C2 C3 1.376(4) . ?
C3 C4 1.369(4) . ?
C4 C5 1.394(4) . ?
C5 C6 1.391(4) . ?
C7 C8 1.472(4) . ?
C8 C9 1.421(4) . ?
C9 C10 1.429(4) . ?
C9 C19 1.467(4) . ?
C10 C11 1.412(4) . ?
C10 C25 1.480(3) . ?
C11 C12 1.464(4) . ?
C13 C18 1.389(4) . ?
C13 C14 1.392(4) . ?
C14 C15 1.380(4) . ?
C15 C16 1.382(4) . ?
C16 C17 1.366(4) . ?
C17 C18 1.387(4) . ?
C19 C20 1.390(4) . ?
C19 C24 1.403(4) . ?
C20 C21 1.371(4) . ?
C21 C22 1.413(4) . ?
C22 C23 1.375(4) . ?
C23 C24 1.389(4) . ?
C25 C26 1.390(4) . ?
C25 C30 1.401(4) . ?
C26 C27 1.384(4) . ?
C27 C28 1.373(5) . ?
C28 C29 1.392(5) . ?
C29 C30 1.372(4) . ?
C29 K3 3.100(4) . ?
C30 K3 3.186(3) . ?
N8 O11 1.202(3) . ?
N8 O12 1.234(3) . ?
N8 C32 1.472(4) . ?
N9 O14 1.228(3) . ?
N9 O13 1.237(3) . ?
N9 C34 1.459(4) . ?
N10 C37 1.391(3) . ?
N10 C36 1.396(3) . ?
N11 C41 1.331(3) . ?
N11 C38 1.340(3) . ?
N12 C42 1.356(3) . ?
N12 C43 1.394(3) . ?
N13 O17 1.212(4) . ?
N13 O18 1.217(4) . ?
N13 C45 1.468(4) . ?
N14 O20 1.225(3) . ?
N14 O19 1.232(3) . ?
N14 C47 1.476(4) . ?
O15 C37 1.229(3) . ?
O15 K2 2.5737(19) 3_655 ?
O16 C42 1.260(3) . ?
O16 K3 2.582(2) 4_565 ?
O16 K1 2.837(2) 1_554 ?
O19 K1 2.978(2) 4_565 ?
C31 C32 1.359(4) . ?
C31 C36 1.409(4) . ?
C32 C33 1.389(4) . ?
C33 C34 1.387(4) . ?
C34 C35 1.375(4) . ?
C35 C36 1.404(4) . ?
C37 C38 1.476(4) . ?
C38 C39 1.413(3) . ?
C39 C40 1.423(4) . ?
C39 C49 1.486(4) . ?
C40 C41 1.416(4) . ?
C40 C55 1.483(4) . ?
C41 C42 1.461(4) . ?
C42 K1 3.443(3) 1_554 ?
C43 C44 1.389(4) . ?
C43 C48 1.394(4) . ?
C44 C45 1.406(4) . ?
C45 C46 1.374(4) . ?
C46 C47 1.377(4) . ?
C47 C48 1.388(4) . ?
C49 C54 1.383(4) . ?
C49 C50 1.392(4) . ?
C50 C51 1.376(4) . ?
C50 K2 3.176(3) 3_655 ?
C51 C52 1.396(4) . ?
C51 K2 3.170(3) 3_655 ?
C52 C53 1.377(4) . ?
C53 C54 1.390(4) . ?
C55 C60 1.393(4) . ?
C55 C56 1.402(4) . ?
C55 K1 3.302(3) 1_554 ?
C56 C57 1.384(4) . ?
C56 K1 3.348(3) 1_554 ?
C57 C58 1.374(5) . ?
C58 C59 1.376(5) . ?
C59 C60 1.401(4) . ?
C61 O21 1.436(5) . ?
C62A O22A 1.386(6) . ?
O22B C62B 1.448(6) . ?
C63 O23 1.378(5) . ?
O24 K1 2.652(4) 1_554 ?
O25 K3 2.622(4) 4_566 ?
O25 K1 2.772(4) . ?
K1 O24 2.652(4) 1_556 ?
K1 O7 2.822(2) 1_556 ?
K1 O16 2.837(2) 1_556 ?
K1 O23 2.949(4) 4_666 ?
K1 O22A 2.960(5) 4_666 ?
K1 O19 2.978(2) 4_666 ?
K1 C55 3.302(3) 1_556 ?
K1 C56 3.348(3) 1_556 ?
K1 C42 3.443(3) 1_556 ?
K1 K3 3.8338(15) 4_566 ?
K2 O15 2.5737(19) 3_655 ?
K2 O1 2.926(2) 3_655 ?
K2 O9 3.018(2) 1_455 ?
K2 C51 3.170(3) 3_655 ?
K2 O10 3.176(3) 1_455 ?
K2 C50 3.176(3) 3_655 ?
K3 O22B 1.920(6) 1_655 ?
K3 O16 2.582(2) 4_666 ?
K3 C62B 2.605(7) 1_655 ?
K3 O25 2.622(4) 4_665 ?
K3 K1 3.8338(16) 4_665 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Co1 N11 174.18(10) . . ?
N4 Co1 N3 78.02(9) . . ?
N11 Co1 N3 100.44(9) . . ?
N4 Co1 N12 96.78(9) . . ?
N11 Co1 N12 77.60(9) . . ?
N3 Co1 N12 91.55(9) . . ?
N4 Co1 N10 106.97(9) . . ?
N11 Co1 N10 78.73(9) . . ?
N3 Co1 N10 95.96(9) . . ?
N12 Co1 N10 156.09(9) . . ?
N4 Co1 N5 78.34(9) . . ?
N11 Co1 N5 103.37(9) . . ?
N3 Co1 N5 156.19(8) . . ?
N12 Co1 N5 94.06(9) . . ?
N10 Co1 N5 88.16(9) . . ?
O2 N1 O1 123.7(2) . . ?
O2 N1 C2 117.9(2) . . ?
O1 N1 C2 118.3(2) . . ?
O4 N2 O3 123.5(2) . . ?
O4 N2 C4 118.0(2) . . ?
O3 N2 C4 118.5(2) . . ?
C7 N3 C6 119.5(2) . . ?
C7 N3 Co1 116.53(17) . . ?
C6 N3 Co1 122.34(17) . . ?
C8 N4 C11 111.1(2) . . ?
C8 N4 Co1 124.47(17) . . ?
C11 N4 Co1 124.10(18) . . ?
C12 N5 C13 118.2(2) . . ?
C12 N5 Co1 115.28(17) . . ?
C13 N5 Co1 122.03(16) . . ?
O8 N6 O7 122.5(2) . . ?
O8 N6 C15 118.7(2) . . ?
O7 N6 C15 118.7(2) . . ?
O9 N7 O10 123.6(3) . . ?
O9 N7 C17 117.9(2) . . ?
O10 N7 C17 118.5(3) . . ?
N1 O1 K2 153.21(17) . 3_655 ?
C7 O5 K2 137.04(17) . . ?
C12 O6 K3 156.42(18) . . ?
N6 O7 K1 149.08(16) . 1_554 ?
N7 O9 K2 101.52(17) . 1_655 ?
N7 O10 K2 93.42(17) . 1_655 ?
C2 C1 C6 118.7(2) . . ?
C3 C2 C1 123.8(2) . . ?
C3 C2 N1 118.6(2) . . ?
C1 C2 N1 117.5(2) . . ?
C4 C3 C2 115.6(2) . . ?
C3 C4 C5 124.1(2) . . ?
C3 C4 N2 117.9(2) . . ?
C5 C4 N2 117.9(2) . . ?
C6 C5 C4 118.5(2) . . ?
C5 C6 N3 124.0(2) . . ?
C5 C6 C1 118.9(2) . . ?
N3 C6 C1 117.0(2) . . ?
O5 C7 N3 124.9(2) . . ?
O5 C7 C8 124.5(2) . . ?
N3 C7 C8 110.6(2) . . ?
N4 C8 C9 108.4(2) . . ?
N4 C8 C7 109.6(2) . . ?
C9 C8 C7 141.7(3) . . ?
C8 C9 C10 105.7(2) . . ?
C8 C9 C19 126.0(2) . . ?
C10 C9 C19 128.2(2) . . ?
C11 C10 C9 106.4(2) . . ?
C11 C10 C25 124.0(2) . . ?
C9 C10 C25 129.5(2) . . ?
N4 C11 C10 108.4(2) . . ?
N4 C11 C12 110.0(2) . . ?
C10 C11 C12 141.2(2) . . ?
O6 C12 N5 125.3(2) . . ?
O6 C12 C11 123.3(2) . . ?
N5 C12 C11 111.4(2) . . ?
C18 C13 C14 118.2(2) . . ?
C18 C13 N5 122.7(2) . . ?
C14 C13 N5 119.0(2) . . ?
C15 C14 C13 119.7(2) . . ?
C14 C15 C16 123.5(2) . . ?
C14 C15 N6 118.0(2) . . ?
C16 C15 N6 118.5(2) . . ?
C17 C16 C15 115.2(3) . . ?
C16 C17 C18 124.1(3) . . ?
C16 C17 N7 118.4(3) . . ?
C18 C17 N7 117.5(2) . . ?
C17 C18 C13 119.3(2) . . ?
C20 C19 C24 117.4(2) . . ?
C20 C19 C9 121.3(2) . . ?
C24 C19 C9 121.3(2) . . ?
C21 C20 C19 121.9(3) . . ?
C20 C21 C22 119.9(3) . . ?
C23 C22 C21 119.1(3) . . ?
C22 C23 C24 120.2(3) . . ?
C23 C24 C19 121.3(3) . . ?
C26 C25 C30 118.0(2) . . ?
C26 C25 C10 121.4(2) . . ?
C30 C25 C10 120.5(2) . . ?
C27 C26 C25 121.0(3) . . ?
C28 C27 C26 120.6(3) . . ?
C27 C28 C29 118.8(3) . . ?
C30 C29 C28 121.1(3) . . ?
C30 C29 K3 80.9(2) . . ?
C28 C29 K3 101.2(2) . . ?
C29 C30 C25 120.4(3) . . ?
C29 C30 K3 73.9(2) . . ?
C25 C30 K3 104.37(19) . . ?
O11 N8 O12 122.8(2) . . ?
O11 N8 C32 118.9(2) . . ?
O12 N8 C32 118.3(2) . . ?
O14 N9 O13 122.9(2) . . ?
O14 N9 C34 120.1(2) . . ?
O13 N9 C34 117.0(2) . . ?
C37 N10 C36 117.6(2) . . ?
C37 N10 Co1 115.87(17) . . ?
C36 N10 Co1 124.96(17) . . ?
C41 N11 C38 111.5(2) . . ?
C41 N11 Co1 124.34(18) . . ?
C38 N11 Co1 124.12(17) . . ?
C42 N12 C43 120.5(2) . . ?
C42 N12 Co1 116.36(17) . . ?
C43 N12 Co1 118.60(16) . . ?
O17 N13 O18 125.4(3) . . ?
O17 N13 C45 116.9(3) . . ?
O18 N13 C45 117.6(3) . . ?
O20 N14 O19 123.8(2) . . ?
O20 N14 C47 118.1(2) . . ?
O19 N14 C47 118.1(2) . . ?
C37 O15 K2 142.54(16) . 3_655 ?
C42 O16 K3 154.10(17) . 4_565 ?
C42 O16 K1 108.06(16) . 1_554 ?
K3 O16 K1 89.93(7) 4_565 1_554 ?
N14 O19 K1 133.17(18) . 4_565 ?
C32 C31 C36 120.2(3) . . ?
C31 C32 C33 123.9(3) . . ?
C31 C32 N8 119.2(3) . . ?
C33 C32 N8 116.9(2) . . ?
C34 C33 C32 114.7(3) . . ?
C35 C34 C33 124.1(3) . . ?
C35 C34 N9 117.7(2) . . ?
C33 C34 N9 118.2(2) . . ?
C34 C35 C36 119.4(3) . . ?
N10 C36 C35 122.2(2) . . ?
N10 C36 C31 120.3(2) . . ?
C35 C36 C31 117.5(2) . . ?
O15 C37 N10 125.7(2) . . ?
O15 C37 C38 124.3(2) . . ?
N10 C37 C38 110.0(2) . . ?
N11 C38 C39 108.4(2) . . ?
N11 C38 C37 111.2(2) . . ?
C39 C38 C37 140.4(2) . . ?
C38 C39 C40 105.7(2) . . ?
C38 C39 C49 125.2(2) . . ?
C40 C39 C49 129.1(2) . . ?
C41 C40 C39 106.6(2) . . ?
C41 C40 C55 124.2(2) . . ?
C39 C40 C55 129.2(2) . . ?
N11 C41 C40 107.8(2) . . ?
N11 C41 C42 110.2(2) . . ?
C40 C41 C42 140.9(2) . . ?
O16 C42 N12 124.8(2) . . ?
O16 C42 C41 124.7(2) . . ?
N12 C42 C41 110.3(2) . . ?
O16 C42 K1 51.58(14) . 1_554 ?
N12 C42 K1 137.03(17) . 1_554 ?
C41 C42 K1 86.28(15) . 1_554 ?
C44 C43 C48 119.9(2) . . ?
C44 C43 N12 120.9(2) . . ?
C48 C43 N12 118.8(2) . . ?
C43 C44 C45 117.9(3) . . ?
C46 C45 C44 124.1(3) . . ?
C46 C45 N13 118.0(3) . . ?
C44 C45 N13 117.7(3) . . ?
C45 C46 C47 115.3(3) . . ?
C46 C47 C48 124.0(3) . . ?
C46 C47 N14 119.1(2) . . ?
C48 C47 N14 116.9(2) . . ?
C47 C48 C43 118.5(2) . . ?
C54 C49 C50 119.0(2) . . ?
C54 C49 C39 121.0(2) . . ?
C50 C49 C39 119.9(2) . . ?
C51 C50 C49 120.3(2) . . ?
C51 C50 K2 77.23(17) . 3_655 ?
C49 C50 K2 93.55(17) . 3_655 ?
C50 C51 C52 120.6(3) . . ?
C50 C51 K2 77.73(17) . 3_655 ?
C52 C51 K2 94.72(18) . 3_655 ?
C53 C52 C51 119.2(3) . . ?
C52 C53 C54 120.3(3) . . ?
C49 C54 C53 120.6(3) . . ?
C60 C55 C56 118.3(2) . . ?
C60 C55 C40 120.0(2) . . ?
C56 C55 C40 121.6(2) . . ?
C60 C55 K1 96.02(17) . 1_554 ?
C56 C55 K1 79.66(16) . 1_554 ?
C40 C55 K1 90.92(15) . 1_554 ?
C57 C56 C55 120.6(3) . . ?
C57 C56 K1 98.61(18) . 1_554 ?
C55 C56 K1 76.01(15) . 1_554 ?
C58 C57 C56 120.6(3) . . ?
C57 C58 C59 120.0(3) . . ?
C58 C59 C60 120.2(3) . . ?
C55 C60 C59 120.4(3) . . ?
K3 O25 K1 90.54(12) 4_566 . ?
O24 K1 O25 130.18(11) 1_556 . ?
O24 K1 O7 80.71(9) 1_556 1_556 ?
O25 K1 O7 147.40(10) . 1_556 ?
O24 K1 O16 87.18(10) 1_556 1_556 ?
O25 K1 O16 85.31(9) . 1_556 ?
O7 K1 O16 109.49(7) 1_556 1_556 ?
O24 K1 O23 77.54(10) 1_556 4_666 ?
O25 K1 O23 70.78(10) . 4_666 ?
O7 K1 O23 113.90(9) 1_556 4_666 ?
O16 K1 O23 130.46(9) 1_556 4_666 ?
O24 K1 O22A 61.18(13) 1_556 4_666 ?
O25 K1 O22A 69.21(14) . 4_666 ?
O7 K1 O22A 138.27(13) 1_556 4_666 ?
O16 K1 O22A 86.32(14) 1_556 4_666 ?
O23 K1 O22A 45.03(14) 4_666 4_666 ?
O24 K1 O19 69.78(10) 1_556 4_666 ?
O25 K1 O19 114.29(9) . 4_666 ?
O7 K1 O19 61.60(6) 1_556 4_666 ?
O16 K1 O19 156.04(7) 1_556 4_666 ?
O23 K1 O19 52.31(8) 4_666 4_666 ?
O22A K1 O19 88.10(13) 4_666 4_666 ?
O24 K1 C55 131.87(9) 1_556 1_556 ?
O25 K1 C55 89.51(9) . 1_556 ?
O7 K1 C55 70.98(7) 1_556 1_556 ?
O16 K1 C55 67.77(6) 1_556 1_556 ?
O23 K1 C55 149.57(9) 4_666 1_556 ?
O22A K1 C55 148.00(13) 4_666 1_556 ?
O19 K1 C55 123.14(7) 4_666 1_556 ?
O24 K1 C56 140.44(9) 1_556 1_556 ?
O25 K1 C56 89.04(9) . 1_556 ?
O7 K1 C56 62.37(7) 1_556 1_556 ?
O16 K1 C56 91.97(7) 1_556 1_556 ?
O23 K1 C56 128.81(9) 4_666 1_556 ?
O22A K1 C56 158.26(13) 4_666 1_556 ?
O19 K1 C56 101.55(7) 4_666 1_556 ?
C55 K1 C56 24.33(7) 1_556 1_556 ?
O24 K1 C42 81.48(9) 1_556 1_556 ?
O25 K1 C42 103.95(9) . 1_556 ?
O7 K1 C42 89.24(7) 1_556 1_556 ?
O16 K1 C42 20.36(6) 1_556 1_556 ?
O23 K1 C42 145.30(9) 4_666 1_556 ?
O22A K1 C42 100.47(14) 4_666 1_556 ?
O19 K1 C42 141.30(7) 4_666 1_556 ?
C55 K1 C42 60.61(7) 1_556 1_556 ?
C56 K1 C42 84.22(7) 1_556 1_556 ?
O24 K1 K3 111.07(9) 1_556 4_566 ?
O25 K1 K3 43.16(8) . 4_566 ?
O7 K1 K3 145.21(6) 1_556 4_566 ?
O16 K1 K3 42.34(4) 1_556 4_566 ?
O23 K1 K3 100.74(7) 4_666 4_566 ?
O22A K1 K3 70.48(12) 4_666 4_566 ?
O19 K1 K3 152.87(6) 4_666 4_566 ?
C55 K1 K3 77.64(6) 1_556 4_566 ?
C56 K1 K3 93.83(6) 1_556 4_566 ?
C42 K1 K3 61.88(5) 1_556 4_566 ?
O15 K2 O5 131.59(6) 3_655 . ?
O15 K2 O1 73.85(6) 3_655 3_655 ?
O5 K2 O1 71.19(6) . 3_655 ?
O15 K2 O9 72.60(6) 3_655 1_455 ?
O5 K2 O9 109.18(6) . 1_455 ?
O1 K2 O9 132.30(6) 3_655 1_455 ?
O15 K2 C51 91.40(7) 3_655 3_655 ?
O5 K2 C51 128.53(7) . 3_655 ?
O1 K2 C51 103.47(7) 3_655 3_655 ?
O9 K2 C51 110.22(7) 1_455 3_655 ?
O15 K2 O10 96.31(6) 3_655 1_455 ?
O5 K2 O10 116.19(7) . 1_455 ?
O1 K2 O10 170.09(6) 3_655 1_455 ?
O9 K2 O10 40.54(6) 1_455 1_455 ?
C51 K2 O10 77.42(7) 3_655 1_455 ?
O15 K2 C50 67.80(6) 3_655 3_655 ?
O5 K2 C50 141.46(7) . 3_655 ?
O1 K2 C50 88.43(7) 3_655 3_655 ?
O9 K2 C50 108.69(7) 1_455 3_655 ?
C51 K2 C50 25.05(7) 3_655 3_655 ?
O10 K2 C50 88.79(7) 1_455 3_655 ?
O22B K3 O6 142.99(14) 1_655 . ?
O22B K3 O16 73.90(14) 1_655 4_666 ?
O6 K3 O16 142.69(7) . 4_666 ?
O22B K3 C62B 33.1(2) 1_655 1_655 ?
O6 K3 C62B 110.26(19) . 1_655 ?
O16 K3 C62B 105.4(2) 4_666 1_655 ?
O22B K3 O25 91.5(2) 1_655 4_665 ?
O6 K3 O25 82.48(9) . 4_665 ?
O16 K3 O25 93.81(9) 4_666 4_665 ?
C62B K3 O25 79.3(3) 1_655 4_665 ?
O22B K3 C29 94.3(2) 1_655 . ?
O6 K3 C29 94.14(8) . . ?
O16 K3 C29 85.72(8) 4_666 . ?
C62B K3 C29 106.8(2) 1_655 . ?
O25 K3 C29 173.80(11) 4_665 . ?
O22B K3 C30 113.7(2) 1_655 . ?
O6 K3 C30 69.00(7) . . ?
O16 K3 C30 106.11(8) 4_666 . ?
C62B K3 C30 113.9(3) 1_655 . ?
O25 K3 C30 151.15(9) 4_665 . ?
C29 K3 C30 25.16(8) . . ?
O22B K3 K1 76.0(2) 1_655 4_665 ?
O6 K3 K1 121.02(6) . 4_665 ?
O16 K3 K1 47.73(5) 4_666 4_665 ?
C62B K3 K1 89.7(2) 1_655 4_665 ?
O25 K3 K1 46.30(8) 4_665 4_665 ?
C29 K3 K1 133.43(7) . 4_665 ?
C30 K3 K1 150.40(7) . 4_665 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.899
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.138

#===END

data_2005sot1251
_database_code_depnum_ccdc_archive 'CCDC 678032'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H58 K4 N14 Ni O27'
_chemical_formula_weight         1694.37

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   P4(2)/n
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -z-1/2'

_cell_length_a                   15.6020(10)
_cell_length_b                   15.6020(10)
_cell_length_c                   15.9970(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3894.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    4267
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       Block
_exptl_crystal_colour            'Dark Orange'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1744
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8879
_exptl_absorpt_correction_T_max  0.9837
_exptl_absorpt_process_details   
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;

_exptl_special_details           
;
SADABS was used to perform the Absorption correction
Parameter refinement on 8931 reflections reduced R(int) from 0.1110 to 0.0688
Ratio of minimum to maximum apparent transmission: 0.596858
The given Tmin and Tmax were generated using the SHELX SIZE command
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans to fill the asymmetric unit'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16842
_diffrn_reflns_av_R_equivalents  0.0995
_diffrn_reflns_av_sigmaI/netI    0.1133
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         27.46
_reflns_number_total             4460
_reflns_number_gt                2732
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin, et al., 1993)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1126P)^2^+6.6118P] where P=(Fo^2^+2Fc^2^)/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         4460
_refine_ls_number_parameters     276
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.1374
_refine_ls_R_factor_gt           0.0797
_refine_ls_wR_factor_ref         0.2307
_refine_ls_wR_factor_gt          0.2010
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.001

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 0.2500 0.2500 0.7500 0.01651(10) Uani 1 4 d S . .
K1 K 0.31066(3) 0.52143(3) 1.03425(3) 0.02782(12) Uani 1 1 d . . .
N1 N 0.41968(11) 0.42546(11) 0.50691(10) 0.0302(5) Uani 1 1 d . . .
N2 N 0.37539(11) 0.66213(11) 0.70316(10) 0.0307(5) Uani 1 1 d . . .
N3 N 0.33353(9) 0.36099(9) 0.78887(9) 0.0169(4) Uani 1 1 d . . .
N4 N 0.2500 0.2500 0.87104(12) 0.0178(5) Uani 1 2 d S . .
O1 O 0.44825(10) 0.35244(9) 0.50079(9) 0.0365(4) Uani 1 1 d . . .
O2 O 0.40944(12) 0.47441(11) 0.44729(9) 0.0443(5) Uani 1 1 d . . .
O3 O 0.38859(12) 0.71207(10) 0.64545(10) 0.0498(5) Uani 1 1 d . . .
O4 O 0.36132(13) 0.68531(10) 0.77436(10) 0.0502(5) Uani 1 1 d . . .
O5 O 0.37844(8) 0.43282(8) 0.90941(7) 0.0229(4) Uani 1 1 d . . .
C1 C 0.38256(12) 0.39794(12) 0.65253(11) 0.0227(5) Uani 1 1 d . . .
H1 H 0.3867 0.3398 0.6404 0.027 Uiso 1 1 calc R . .
C2 C 0.39858(13) 0.45694(13) 0.59149(12) 0.0254(5) Uani 1 1 d . . .
C3 C 0.39605(13) 0.54519(13) 0.60393(12) 0.0268(5) Uani 1 1 d . . .
H3 H 0.4056 0.5845 0.5612 0.032 Uiso 1 1 calc R . .
C4 C 0.37802(12) 0.56951(12) 0.68543(11) 0.0233(5) Uani 1 1 d . . .
C5 C 0.36024(12) 0.51264(12) 0.74946(12) 0.0213(5) Uani 1 1 d . . .
H5 H 0.3486 0.5331 0.8029 0.026 Uiso 1 1 calc R . .
C6 C 0.35970(11) 0.42442(12) 0.73410(10) 0.0184(5) Uani 1 1 d . . .
C7 C 0.34061(11) 0.37188(11) 0.87193(10) 0.0177(5) Uani 1 1 d . . .
C8 C 0.29608(11) 0.30317(11) 0.91916(10) 0.0166(4) Uani 1 1 d . . .
C9 C 0.28049(11) 0.28403(12) 1.00429(11) 0.0183(5) Uani 1 1 d . . .
C10 C 0.31876(13) 0.32747(12) 1.07786(10) 0.0207(5) Uani 1 1 d . . .
C11 C 0.26815(13) 0.35583(13) 1.14468(11) 0.0255(5) Uani 1 1 d . . .
H11 H 0.2096 0.3448 1.1443 0.031 Uiso 1 1 calc R . .
C12 C 0.30390(15) 0.40014(13) 1.21155(12) 0.0313(6) Uani 1 1 d . . .
H12 H 0.2694 0.4181 1.2556 0.038 Uiso 1 1 calc R . .
C13 C 0.39059(16) 0.41746(14) 1.21263(12) 0.0354(6) Uani 1 1 d . . .
H13 H 0.4144 0.4480 1.2568 0.042 Uiso 1 1 calc R . .
C14 C 0.44262(15) 0.38897(14) 1.14701(12) 0.0338(6) Uani 1 1 d . . .
H14 H 0.5012 0.4000 1.1478 0.041 Uiso 1 1 calc R . .
C15 C 0.40650(13) 0.34391(12) 1.08033(12) 0.0245(5) Uani 1 1 d . . .
H15 H 0.4414 0.3247 1.0371 0.029 Uiso 1 1 calc R . .
O6A O 0.1986(6) 0.6343(6) 0.9494(3) 0.0426(8) Uani 0.15 1 d PDU A 1
H6A H 0.2430 0.6624 0.9486 0.064 Uiso 0.15 1 calc PR A 1
C16A C 0.1755(8) 0.6107(8) 0.8652(3) 0.0426(8) Uani 0.15 1 d PDU A 1
H16A H 0.1910 0.6560 0.8276 0.064 Uiso 0.15 1 calc PR A 1
H16B H 0.1148 0.6010 0.8622 0.064 Uiso 0.15 1 calc PR A 1
H16C H 0.2053 0.5592 0.8498 0.064 Uiso 0.15 1 calc PR A 1
O6B O 0.2331(2) 0.6437(3) 0.9406(2) 0.0426(8) Uani 0.35 1 d PDU B 2
H6B H 0.2506 0.5978 0.9589 0.064 Uiso 0.35 1 calc PRD B 2
C16B C 0.1731(3) 0.6283(4) 0.8752(3) 0.0426(8) Uani 0.35 1 d PDU B 2
H16D H 0.1281 0.6701 0.8779 0.064 Uiso 0.35 1 calc PR B 2
H16E H 0.1492 0.5720 0.8813 0.064 Uiso 0.35 1 calc PR B 2
H16F H 0.2016 0.6325 0.8221 0.064 Uiso 0.35 1 calc PR B 2
O7 O 0.45025(11) 0.60469(11) 1.08310(12) 0.0550(5) Uani 1 1 d U . .
H7 H 0.4991 0.5857 1.0797 0.083 Uiso 1 1 calc R . .
C17 C 0.44276(16) 0.65377(18) 1.15481(18) 0.0550(5) Uani 1 1 d U . .
H17A H 0.4575 0.6196 1.2026 0.083 Uiso 1 1 calc R . .
H17B H 0.3848 0.6737 1.1602 0.083 Uiso 1 1 calc R . .
H17C H 0.4808 0.7020 1.1513 0.083 Uiso 1 1 calc R . .
O8 O 0.366435(3) 0.713333(3) 0.968361(5) 0.0553(18) Uani 0.25 1 d PDU . .
H99 H 0.319860(3) 0.704008(4) 0.943640(5) 0.050 Uiso 0.25 1 d PD . .
H98 H 0.368789(6) 0.762369(3) 0.989921(5) 0.050 Uiso 0.25 1 d PD . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.01800(13) 0.01800(13) 0.01354(19) 0.000 0.000 0.000
K1 0.0266(2) 0.0298(2) 0.0270(2) -0.00553(18) 0.00221(18) -0.00046(18)
N1 0.0383(10) 0.0288(9) 0.0234(8) -0.0009(7) 0.0087(7) -0.0078(8)
N2 0.0370(10) 0.0238(9) 0.0312(9) 0.0020(7) 0.0054(7) -0.0038(8)
N3 0.0157(7) 0.0184(7) 0.0165(7) 0.0014(6) 0.0011(6) -0.0040(6)
N4 0.0225(11) 0.0156(10) 0.0154(9) 0.000 0.000 -0.0026(9)
O1 0.0509(9) 0.0270(8) 0.0318(7) -0.0052(6) 0.0153(7) -0.0076(7)
O2 0.0684(11) 0.0435(9) 0.0211(7) 0.0044(7) 0.0081(7) -0.0037(8)
O3 0.0824(12) 0.0233(8) 0.0435(8) 0.0111(7) 0.0221(8) -0.0037(8)
O4 0.0882(12) 0.0206(8) 0.0418(8) -0.0051(7) 0.0198(8) -0.0049(8)
O5 0.0265(7) 0.0218(6) 0.0204(6) -0.0031(5) -0.0012(5) -0.0077(5)
C1 0.0243(9) 0.0218(9) 0.0221(9) 0.0001(8) -0.0004(8) -0.0039(8)
C2 0.0275(10) 0.0262(10) 0.0224(9) 0.0005(8) 0.0046(8) -0.0058(8)
C3 0.0323(10) 0.0263(10) 0.0218(9) 0.0034(8) 0.0022(8) -0.0056(9)
C4 0.0249(10) 0.0209(9) 0.0242(9) 0.0018(8) -0.0028(8) -0.0020(8)
C5 0.0207(9) 0.0217(9) 0.0214(8) -0.0037(7) 0.0024(7) -0.0057(7)
C6 0.0149(8) 0.0220(9) 0.0183(8) 0.0007(7) -0.0017(7) -0.0018(7)
C7 0.0146(8) 0.0203(9) 0.0181(8) 0.0014(7) 0.0003(7) 0.0014(7)
C8 0.0155(8) 0.0183(9) 0.0159(8) -0.0016(7) -0.0008(7) 0.0000(7)
C9 0.0164(9) 0.0227(9) 0.0158(8) 0.0008(7) 0.0005(7) -0.0007(7)
C10 0.0302(10) 0.0175(9) 0.0144(8) 0.0022(7) -0.0001(7) -0.0005(8)
C11 0.0280(10) 0.0277(10) 0.0207(9) 0.0025(8) -0.0017(8) -0.0071(8)
C12 0.0461(12) 0.0303(11) 0.0175(9) -0.0051(8) -0.0021(9) -0.0057(10)
C13 0.0569(14) 0.0275(11) 0.0218(9) -0.0052(8) -0.0132(9) -0.0092(10)
C14 0.0366(11) 0.0392(12) 0.0256(10) 0.0020(9) -0.0078(9) -0.0103(10)
C15 0.0261(10) 0.0267(10) 0.0206(9) 0.0017(8) -0.0020(8) -0.0051(8)
O6A 0.0508(16) 0.0441(14) 0.0331(12) 0.0177(11) 0.0013(12) 0.0114(13)
C16A 0.0508(16) 0.0441(14) 0.0331(12) 0.0177(11) 0.0013(12) 0.0114(13)
O6B 0.0508(16) 0.0441(14) 0.0331(12) 0.0177(11) 0.0013(12) 0.0114(13)
C16B 0.0508(16) 0.0441(14) 0.0331(12) 0.0177(11) 0.0013(12) 0.0114(13)
O7 0.0344(7) 0.0542(9) 0.0765(9) -0.0173(7) -0.0070(7) -0.0001(7)
C17 0.0344(7) 0.0542(9) 0.0765(9) -0.0173(7) -0.0070(7) -0.0001(7)
O8 0.058(3) 0.062(3) 0.046(3) 0.001(3) -0.007(3) 0.022(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N4 1.9363(19) 7_567 ?
Ni1 N4 1.9363(19) . ?
Ni1 N3 2.2547(15) . ?
Ni1 N3 2.2547(15) 7_567 ?
Ni1 N3 2.2547(15) 2 ?
Ni1 N3 2.2547(14) 8_657 ?
K1 O5 2.6492(13) . ?
K1 O3 2.7389(17) 4_465 ?
K1 O1 2.8448(15) 8_657 ?
K1 C10 3.1081(19) . ?
K1 C11 3.199(2) . ?
K1 C15 3.233(2) . ?
K1 C12 3.411(2) . ?
K1 C14 3.430(2) . ?
K1 C13 3.511(2) . ?
K1 C7 3.5220(18) . ?
N1 O1 1.227(2) . ?
N1 O2 1.232(2) . ?
N1 C2 1.476(2) . ?
N2 O4 1.215(2) . ?
N2 O3 1.226(2) . ?
N2 C4 1.473(3) . ?
N3 C7 1.344(2) . ?
N3 C6 1.383(2) . ?
N4 C8 1.341(2) . ?
N4 C8 1.341(2) 2 ?
O1 K1 2.8448(15) 7_567 ?
O3 K1 2.7389(17) 3_654 ?
O5 C7 1.269(2) . ?
C1 C2 1.365(3) . ?
C1 C6 1.414(2) . ?
C2 C3 1.392(3) . ?
C3 C4 1.387(3) . ?
C4 C5 1.383(3) . ?
C5 C6 1.398(3) . ?
C7 C8 1.484(2) . ?
C8 C9 1.415(2) . ?
C9 C9 1.426(4) 2 ?
C9 C10 1.484(2) . ?
C10 C15 1.393(3) . ?
C10 C11 1.401(3) . ?
C11 C12 1.390(3) . ?
C12 C13 1.379(3) . ?
C13 C14 1.400(3) . ?
C14 C15 1.396(3) . ?
O6A C16A 1.442(7) . ?
O6B C16B 1.425(5) . ?
O7 C17 1.384(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Ni1 N4 180.0 7_567 . ?
N4 Ni1 N3 106.01(4) 7_567 . ?
N4 Ni1 N3 73.99(4) . . ?
N4 Ni1 N3 73.99(4) 7_567 7_567 ?
N4 Ni1 N3 106.01(4) . 7_567 ?
N3 Ni1 N3 94.361(19) . 7_567 ?
N4 Ni1 N3 106.01(4) 7_567 2 ?
N4 Ni1 N3 73.99(4) . 2 ?
N3 Ni1 N3 147.99(7) . 2 ?
N3 Ni1 N3 94.361(19) 7_567 2 ?
N4 Ni1 N3 73.99(4) 7_567 8_657 ?
N4 Ni1 N3 106.01(4) . 8_657 ?
N3 Ni1 N3 94.361(19) . 8_657 ?
N3 Ni1 N3 147.99(7) 7_567 8_657 ?
N3 Ni1 N3 94.361(19) 2 8_657 ?
O5 K1 O3 168.91(5) . 4_465 ?
O5 K1 O1 89.95(4) . 8_657 ?
O3 K1 O1 80.29(5) 4_465 8_657 ?
O5 K1 C10 69.20(4) . . ?
O3 K1 C10 112.09(5) 4_465 . ?
O1 K1 C10 71.93(5) 8_657 . ?
O5 K1 C11 94.45(5) . . ?
O3 K1 C11 86.50(5) 4_465 . ?
O1 K1 C11 66.38(5) 8_657 . ?
C10 K1 C11 25.61(5) . . ?
O5 K1 C15 62.62(4) . . ?
O3 K1 C15 123.42(5) 4_465 . ?
O1 K1 C15 96.59(5) 8_657 . ?
C10 K1 C15 25.29(5) . . ?
C11 K1 C15 43.79(5) . . ?
O5 K1 C12 110.46(5) . . ?
O3 K1 C12 74.15(5) 4_465 . ?
O1 K1 C12 85.04(5) 8_657 . ?
C10 K1 C12 43.49(5) . . ?
C11 K1 C12 24.01(5) . . ?
C15 K1 C12 49.41(5) . . ?
O5 K1 C14 80.93(5) . . ?
O3 K1 C14 107.72(5) 4_465 . ?
O1 K1 C14 113.50(5) 8_657 . ?
C10 K1 C14 43.19(5) . . ?
C11 K1 C14 49.27(5) . . ?
C15 K1 C14 23.96(5) . . ?
C12 K1 C14 41.15(5) . . ?
O5 K1 C13 103.28(5) . . ?
O3 K1 C13 84.75(5) 4_465 . ?
O1 K1 C13 107.00(5) 8_657 . ?
C10 K1 C13 49.71(5) . . ?
C11 K1 C13 41.57(5) . . ?
C15 K1 C13 41.80(5) . . ?
C12 K1 C13 22.93(5) . . ?
C14 K1 C13 23.23(5) . . ?
O5 K1 C7 17.36(4) . . ?
O3 K1 C7 153.24(5) 4_465 . ?
O1 K1 C7 73.00(4) 8_657 . ?
C10 K1 C7 61.00(4) . . ?
C11 K1 C7 84.24(5) . . ?
C15 K1 C7 62.56(4) . . ?
C12 K1 C7 104.45(5) . . ?
C14 K1 C7 84.77(5) . . ?
C13 K1 C7 104.24(5) . . ?
O1 N1 O2 124.10(17) . . ?
O1 N1 C2 117.57(16) . . ?
O2 N1 C2 118.31(17) . . ?
O4 N2 O3 123.19(17) . . ?
O4 N2 C4 118.52(16) . . ?
O3 N2 C4 118.29(16) . . ?
C7 N3 C6 120.75(15) . . ?
C7 N3 Ni1 114.66(11) . . ?
C6 N3 Ni1 123.05(11) . . ?
C8 N4 C8 109.9(2) . 2 ?
C8 N4 Ni1 125.04(10) . . ?
C8 N4 Ni1 125.04(10) 2 . ?
N1 O1 K1 172.67(12) . 7_567 ?
N2 O3 K1 158.83(15) . 3_654 ?
C7 O5 K1 124.14(11) . . ?
C2 C1 C6 120.61(18) . . ?
C1 C2 C3 124.03(18) . . ?
C1 C2 N1 118.17(17) . . ?
C3 C2 N1 117.80(17) . . ?
C4 C3 C2 114.26(17) . . ?
C5 C4 C3 124.15(18) . . ?
C5 C4 N2 118.75(16) . . ?
C3 C4 N2 117.07(16) . . ?
C4 C5 C6 120.17(17) . . ?
N3 C6 C5 126.50(16) . . ?
N3 C6 C1 116.73(16) . . ?
C5 C6 C1 116.62(16) . . ?
O5 C7 N3 126.85(16) . . ?
O5 C7 C8 121.21(15) . . ?
N3 C7 C8 111.93(15) . . ?
N3 C7 K1 143.29(12) . . ?
C8 C7 K1 92.35(10) . . ?
N4 C8 C9 109.25(16) . . ?
N4 C8 C7 113.93(15) . . ?
C9 C8 C7 136.28(16) . . ?
C8 C9 C9 105.77(10) . 2 ?
C8 C9 C10 126.71(16) . . ?
C9 C9 C10 127.50(10) 2 . ?
C15 C10 C11 118.30(17) . . ?
C15 C10 C9 120.13(16) . . ?
C11 C10 C9 121.53(17) . . ?
C15 C10 K1 82.36(11) . . ?
C11 C10 K1 80.84(11) . . ?
C9 C10 K1 104.50(11) . . ?
C12 C11 C10 121.21(19) . . ?
C12 C11 K1 86.57(12) . . ?
C10 C11 K1 73.56(11) . . ?
C13 C12 C11 120.02(19) . . ?
C13 C12 K1 82.61(12) . . ?
C11 C12 K1 69.42(11) . . ?
C12 C13 C14 119.82(19) . . ?
C12 C13 K1 74.46(12) . . ?
C14 C13 K1 75.12(12) . . ?
C15 C14 C13 119.9(2) . . ?
C15 C14 K1 70.08(12) . . ?
C13 C14 K1 81.65(13) . . ?
C10 C15 C14 120.73(18) . . ?
C10 C15 K1 72.35(11) . . ?
C14 C15 K1 85.96(13) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.270
_refine_diff_density_min         -1.258
_refine_diff_density_rms         0.110

#===END

data_2005sot1397
_database_code_depnum_ccdc_archive 'CCDC 678033'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H60 Co N6 S4'
_chemical_formula_weight         956.23

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   11.820(5)
_cell_length_b                   12.819(5)
_cell_length_c                   17.669(5)
_cell_angle_alpha                111.096(5)
_cell_angle_beta                 100.723(5)
_cell_angle_gamma                92.892(5)
_cell_volume                     2434.0(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    10866
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       Block
_exptl_crystal_colour            'Dark Red'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1010
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9568
_exptl_absorpt_correction_T_max  0.9832
_exptl_absorpt_process_details   
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;

_exptl_special_details           
;
SADABS was used to perform the Absorption correction
Parameter refinement on 20498 reflections reduced R(int) from 0.1058 to 0.0595
Ratio of minimum to maximum apparent transmission: 0.780533
The given Tmin and Tmax were generated using the SHELX SIZE command
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans to fill the asymmetric unit'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39694
_diffrn_reflns_av_R_equivalents  0.0905
_diffrn_reflns_av_sigmaI/netI    0.1182
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         27.48
_reflns_number_total             11133
_reflns_number_gt                6353
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin, et al., 1993)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0907P)^2^+2.3798P] where P=(Fo^2^+2Fc^2^)/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         11133
_refine_ls_number_parameters     541
_refine_ls_number_restraints     570
_refine_ls_R_factor_all          0.1479
_refine_ls_R_factor_gt           0.0774
_refine_ls_wR_factor_ref         0.2146
_refine_ls_wR_factor_gt          0.1858
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.002

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
C1A C 0.238(2) -0.412(2) 0.6097(17) 0.117(4) Uani 0.35 1 d PU A 1
H1A1 H 0.2805 -0.4768 0.5899 0.176 Uiso 0.35 1 calc PR A 1
H1A2 H 0.1798 -0.4098 0.5631 0.176 Uiso 0.35 1 calc PR A 1
H1A3 H 0.1995 -0.4191 0.6524 0.176 Uiso 0.35 1 calc PR A 1
C2A C 0.3240(6) -0.3023(7) 0.6470(5) 0.0816(19) Uani 0.35 1 d PU A 1
H2A1 H 0.3448 -0.2840 0.6010 0.098 Uiso 0.35 1 calc PR A 1
H2A2 H 0.2850 -0.2399 0.6789 0.098 Uiso 0.35 1 calc PR A 1
C1B C 0.2375(11) -0.2485(13) 0.6976(9) 0.117(4) Uani 0.65 1 d PU A 2
H1B1 H 0.1956 -0.3054 0.7107 0.176 Uiso 0.65 1 calc PR A 2
H1B2 H 0.1822 -0.2173 0.6655 0.176 Uiso 0.65 1 calc PR A 2
H1B3 H 0.2787 -0.1879 0.7493 0.176 Uiso 0.65 1 calc PR A 2
C2B C 0.3240(6) -0.3023(7) 0.6470(5) 0.0816(19) Uani 0.65 1 d PU A 2
H2B1 H 0.2897 -0.3790 0.6073 0.098 Uiso 0.65 1 calc PR A 2
H2B2 H 0.3425 -0.2572 0.6146 0.098 Uiso 0.65 1 calc PR A 2
C3 C 0.4320(5) -0.3091(5) 0.7023(4) 0.0634(16) Uani 1 1 d U . .
H3A H 0.4729 -0.3690 0.6694 0.076 Uiso 1 1 calc R A 1
H3B H 0.4107 -0.3318 0.7462 0.076 Uiso 1 1 calc R A 1
C4 C 0.5153(5) -0.1998(5) 0.7434(3) 0.0535(14) Uani 1 1 d U A .
H4A H 0.4746 -0.1383 0.7747 0.064 Uiso 1 1 calc R . .
H4B H 0.5811 -0.2089 0.7833 0.064 Uiso 1 1 calc R . .
C5 C 0.6278(4) -0.0757(4) 0.7009(3) 0.0309(10) Uani 1 1 d U A .
C6 C 0.6683(4) -0.0466(4) 0.6377(3) 0.0304(10) Uani 1 1 d U A .
C7 C 0.6503(4) -0.0945(4) 0.5496(3) 0.0302(10) Uani 1 1 d U . .
C8 C 0.7183(4) -0.0243(4) 0.5267(2) 0.0277(10) Uani 1 1 d U D .
C9 C 0.7773(4) 0.0650(4) 0.6018(2) 0.0271(10) Uani 1 1 d U . .
C10 C 0.8569(4) 0.1663(4) 0.6244(3) 0.0288(10) Uani 1 1 d U A .
C11 C 0.9715(5) 0.2979(5) 0.5886(3) 0.0426(12) Uani 1 1 d U . .
H11A H 1.0426 0.2971 0.6281 0.051 Uiso 1 1 calc R B 3
H11B H 0.9348 0.3648 0.6165 0.051 Uiso 1 1 calc R B 3
C12A C 1.0041(5) 0.3070(6) 0.5130(3) 0.0597(14) Uani 0.60 1 d PU C 3
H12A H 0.9322 0.3160 0.4782 0.072 Uiso 0.60 1 calc PR C 3
H12B H 1.0563 0.3787 0.5323 0.072 Uiso 0.60 1 calc PR C 3
C13A C 1.0537(9) 0.2293(9) 0.4630(6) 0.0517(17) Uani 0.60 1 d PU C 3
H13A H 0.9993 0.1584 0.4382 0.062 Uiso 0.60 1 calc PR C 3
H13B H 1.1235 0.2154 0.4970 0.062 Uiso 0.60 1 calc PR C 3
C14A C 1.0899(11) 0.2551(10) 0.3928(6) 0.071(2) Uani 0.60 1 d PU C 3
H14A H 1.0207 0.2601 0.3546 0.106 Uiso 0.60 1 calc PR C 3
H14B H 1.1314 0.1947 0.3627 0.106 Uiso 0.60 1 calc PR C 3
H14C H 1.1409 0.3269 0.4159 0.106 Uiso 0.60 1 calc PR C 3
C12B C 1.0041(5) 0.3070(6) 0.5130(3) 0.0597(14) Uani 0.40 1 d PU C 4
H12C H 1.0326 0.2354 0.4835 0.072 Uiso 0.40 1 calc PR C 4
H12D H 0.9317 0.3110 0.4761 0.072 Uiso 0.40 1 calc PR C 4
C13B C 1.0877(12) 0.3967(13) 0.5204(8) 0.0517(17) Uani 0.40 1 d PU C 4
H13C H 1.1547 0.4026 0.5654 0.062 Uiso 0.40 1 calc PR C 4
H13D H 1.0526 0.4676 0.5392 0.062 Uiso 0.40 1 calc PR C 4
C14B C 1.1355(16) 0.3917(15) 0.4443(9) 0.071(2) Uani 0.40 1 d PU C 4
H14D H 1.1950 0.3405 0.4370 0.106 Uiso 0.40 1 calc PR C 4
H14E H 1.1700 0.4673 0.4527 0.106 Uiso 0.40 1 calc PR C 4
H14F H 1.0723 0.3643 0.3946 0.106 Uiso 0.40 1 calc PR C 4
C15A C 0.5762(4) -0.1996(3) 0.4873(2) 0.0325(12) Uani 0.75 1 d PGU D 4
C16A C 0.4591(4) -0.2194(4) 0.4863(3) 0.0358(14) Uani 0.75 1 d PGU D 4
H16A H 0.4245 -0.1651 0.5246 0.043 Uiso 0.75 1 calc PR D 4
C17A C 0.3927(3) -0.3187(4) 0.4293(3) 0.0396(13) Uani 0.75 1 d PGU D 4
H17A H 0.3127 -0.3322 0.4286 0.048 Uiso 0.75 1 calc PR D 4
C18A C 0.4433(3) -0.3982(3) 0.3733(3) 0.0443(15) Uani 0.75 1 d PGU D 4
H18A H 0.3979 -0.4660 0.3343 0.053 Uiso 0.75 1 calc PR D 4
C19A C 0.5604(3) -0.3784(3) 0.3743(2) 0.0475(16) Uani 0.75 1 d PGU D 4
H19A H 0.5950 -0.4327 0.3360 0.057 Uiso 0.75 1 calc PR D 4
C20A C 0.6268(3) -0.2791(3) 0.4313(3) 0.0385(13) Uani 0.75 1 d PGU D 4
H20A H 0.7068 -0.2656 0.4319 0.046 Uiso 0.75 1 calc PR D 4
C15B C 0.5721(12) -0.2069(9) 0.5061(9) 0.0325(12) Uani 0.25 1 d PGU D 5
C16B C 0.4635(13) -0.2074(10) 0.4592(9) 0.0358(14) Uani 0.25 1 d PGU D 5
H16B H 0.4418 -0.1399 0.4533 0.043 Uiso 0.25 1 calc PR D 5
C17B C 0.3869(10) -0.3066(13) 0.4209(9) 0.0396(13) Uani 0.25 1 d PGU D 5
H17B H 0.3127 -0.3069 0.3888 0.048 Uiso 0.25 1 calc PR D 5
C18B C 0.4188(10) -0.4053(11) 0.4296(9) 0.0443(15) Uani 0.25 1 d PGU D 5
H18B H 0.3664 -0.4731 0.4034 0.053 Uiso 0.25 1 calc PR D 5
C19B C 0.5273(11) -0.4048(9) 0.4765(8) 0.0475(16) Uani 0.25 1 d PGU D 5
H19B H 0.5491 -0.4722 0.4824 0.057 Uiso 0.25 1 calc PR D 5
C20B C 0.6039(9) -0.3056(11) 0.5147(8) 0.0385(13) Uani 0.25 1 d PGU D 5
H20B H 0.6781 -0.3052 0.5468 0.046 Uiso 0.25 1 calc PR D 5
C21 C 0.7278(2) -0.0382(3) 0.44041(13) 0.0286(10) Uani 1 1 d GU . .
C22 C 0.62833(18) -0.0461(3) 0.38150(16) 0.0329(11) Uani 1 1 d GU D .
H22 H 0.5545 -0.0456 0.3955 0.039 Uiso 1 1 calc R . .
C23 C 0.6369(2) -0.0549(3) 0.30208(15) 0.0400(12) Uani 1 1 d GU D .
H23 H 0.5689 -0.0604 0.2618 0.048 Uiso 1 1 calc R . .
C24 C 0.7449(3) -0.0558(3) 0.28157(14) 0.0426(12) Uani 1 1 d GU D .
H24 H 0.7507 -0.0618 0.2273 0.051 Uiso 1 1 calc R . .
C25 C 0.8443(2) -0.0478(3) 0.34048(18) 0.0408(12) Uani 1 1 d GU D .
H25 H 0.9182 -0.0484 0.3265 0.049 Uiso 1 1 calc R . .
C26 C 0.83581(19) -0.0390(3) 0.41990(16) 0.0368(11) Uani 1 1 d GU D .
H26 H 0.9038 -0.0336 0.4602 0.044 Uiso 1 1 calc R . .
C27 C 1.3629(8) -0.1183(8) 0.9104(6) 0.117(3) Uani 1 1 d U . .
H27A H 1.3238 -0.1084 0.8599 0.176 Uiso 1 1 calc R . .
H27B H 1.3955 -0.1900 0.8952 0.176 Uiso 1 1 calc R . .
H27C H 1.4255 -0.0561 0.9418 0.176 Uiso 1 1 calc R . .
C28 C 1.2801(5) -0.1192(5) 0.9612(4) 0.0576(15) Uani 1 1 d U . .
H28A H 1.3198 -0.1323 1.0109 0.069 Uiso 1 1 calc R . .
H28B H 1.2180 -0.1830 0.9291 0.069 Uiso 1 1 calc R . .
C29 C 1.2244(5) -0.0105(5) 0.9896(3) 0.0473(13) Uani 1 1 d U . .
H29A H 1.1687 -0.0183 1.0233 0.057 Uiso 1 1 calc R . .
H29B H 1.2856 0.0524 1.0258 0.057 Uiso 1 1 calc R . .
C30 C 1.1618(4) 0.0187(4) 0.9188(3) 0.0367(11) Uani 1 1 d U . .
H30A H 1.2187 0.0381 0.8898 0.044 Uiso 1 1 calc R . .
H30B H 1.1073 -0.0473 0.8784 0.044 Uiso 1 1 calc R . .
C31 C 1.0046(4) 0.1308(4) 0.9063(2) 0.0272(10) Uani 1 1 d U A .
C32 C 0.9422(4) 0.2230(4) 0.9432(3) 0.0266(10) Uani 1 1 d U . .
C33 C 0.9525(4) 0.3099(4) 1.0228(2) 0.0263(9) Uani 1 1 d U . .
C34 C 0.8663(4) 0.3779(4) 1.0145(2) 0.0264(10) Uani 1 1 d U . .
C35 C 0.8037(4) 0.3302(4) 0.9305(3) 0.0280(10) Uani 1 1 d U . .
C36 C 0.7051(4) 0.3540(4) 0.8810(3) 0.0293(10) Uani 1 1 d U A .
C37 C 0.5632(6) 0.4860(6) 0.8674(4) 0.0703(19) Uani 1 1 d U . .
H37A H 0.4864 0.4536 0.8693 0.084 Uiso 1 1 calc R . .
H37B H 0.5686 0.4631 0.8085 0.084 Uiso 1 1 calc R . .
C38 C 0.5783(8) 0.6192(8) 0.9107(5) 0.107(2) Uani 1 1 d U . .
H38A H 0.6608 0.6489 0.9202 0.129 Uiso 1 1 calc R . .
H38B H 0.5318 0.6501 0.8730 0.129 Uiso 1 1 calc R . .
C39 C 0.5422(9) 0.6574(9) 0.9899(6) 0.133(3) Uani 1 1 d U . .
H39A H 0.4576 0.6332 0.9771 0.160 Uiso 1 1 calc R . .
H39B H 0.5797 0.6141 1.0218 0.160 Uiso 1 1 calc R . .
C40 C 0.5607(8) 0.7703(8) 1.0443(5) 0.106(3) Uani 1 1 d U . .
H40A H 0.6430 0.7992 1.0564 0.159 Uiso 1 1 calc R . .
H40B H 0.5380 0.7761 1.0962 0.159 Uiso 1 1 calc R . .
H40C H 0.5139 0.8147 1.0186 0.159 Uiso 1 1 calc R . .
C41 C 1.0403(2) 0.3284(2) 1.10114(14) 0.0251(9) Uani 1 1 d GU . .
C42 C 1.0638(3) 0.23871(17) 1.12565(16) 0.0325(11) Uani 1 1 d GU . .
H42 H 1.0254 0.1650 1.0922 0.039 Uiso 1 1 calc R . .
C43 C 1.1437(3) 0.2568(2) 1.19906(18) 0.0372(11) Uani 1 1 d GU . .
H43 H 1.1598 0.1956 1.2158 0.045 Uiso 1 1 calc R . .
C44 C 1.1999(2) 0.3646(2) 1.24795(15) 0.0384(12) Uani 1 1 d GU . .
H44 H 1.2545 0.3770 1.2981 0.046 Uiso 1 1 calc R . .
C45 C 1.1764(3) 0.45430(19) 1.22344(16) 0.0388(12) Uani 1 1 d GU . .
H45 H 1.2148 0.5280 1.2569 0.047 Uiso 1 1 calc R . .
C46 C 1.0965(3) 0.43617(19) 1.15003(17) 0.0306(10) Uani 1 1 d GU . .
H46 H 1.0804 0.4975 1.1333 0.037 Uiso 1 1 calc R . .
C47 C 0.8374(3) 0.4748(2) 1.08340(15) 0.0293(10) Uani 1 1 d GU . .
C48 C 0.7980(3) 0.45375(19) 1.14655(18) 0.0374(11) Uani 1 1 d GU . .
H48 H 0.7931 0.3797 1.1468 0.045 Uiso 1 1 calc R . .
C49 C 0.7659(3) 0.5410(3) 1.20928(16) 0.0446(13) Uani 1 1 d GU . .
H49 H 0.7390 0.5266 1.2524 0.054 Uiso 1 1 calc R . .
C50 C 0.7731(3) 0.6494(2) 1.20887(16) 0.0398(12) Uani 1 1 d GU . .
H50 H 0.7512 0.7091 1.2517 0.048 Uiso 1 1 calc R . .
C51 C 0.8125(3) 0.67045(19) 1.14572(18) 0.0391(12) Uani 1 1 d GU . .
H51 H 0.8175 0.7445 1.1454 0.047 Uiso 1 1 calc R . .
C52 C 0.8447(3) 0.5832(2) 1.08299(15) 0.0317(10) Uani 1 1 d GU . .
H52 H 0.8716 0.5976 1.0398 0.038 Uiso 1 1 calc R . .
N1 N 0.5592(4) -0.1699(4) 0.6807(3) 0.0417(10) Uani 1 1 d U . .
H1 H 0.5392 -0.2161 0.6283 0.050 Uiso 1 1 calc R A .
N2 N 0.7441(3) 0.0487(3) 0.6674(2) 0.0277(8) Uani 1 1 d U A .
N3 N 0.8921(3) 0.1968(3) 0.5680(2) 0.0323(9) Uani 1 1 d U A .
H3 H 0.8662 0.1537 0.5153 0.039 Uiso 1 1 calc R . .
N4 N 1.0983(3) 0.1134(3) 0.9500(2) 0.0332(9) Uani 1 1 d U . .
H4 H 1.1244 0.1619 1.0013 0.040 Uiso 1 1 calc R . .
N5 N 0.8502(3) 0.2363(3) 0.8896(2) 0.0255(8) Uani 1 1 d U . .
N6 N 0.6564(4) 0.4453(4) 0.9130(2) 0.0418(10) Uani 1 1 d U . .
H6 H 0.6819 0.4856 0.9663 0.050 Uiso 1 1 calc R . .
S1 S 0.67563(10) 0.01834(10) 0.80200(7) 0.0328(3) Uani 1 1 d . . .
S2 S 0.90317(10) 0.24506(10) 0.72823(6) 0.0294(3) Uani 1 1 d . . .
S3 S 0.94947(10) 0.04870(10) 0.80233(6) 0.0302(3) Uani 1 1 d . . .
S4 S 0.65674(10) 0.26131(10) 0.78089(7) 0.0318(3) Uani 1 1 d . . .
Co1 Co 0.79667(5) 0.14278(5) 0.77842(3) 0.02668(18) Uani 1 1 d . A .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1A 0.080(6) 0.123(8) 0.120(7) 0.030(6) -0.008(6) -0.014(6)
C2A 0.057(3) 0.092(4) 0.085(4) 0.028(3) 0.009(3) -0.019(3)
C1B 0.080(6) 0.123(8) 0.120(7) 0.030(6) -0.008(6) -0.014(6)
C2B 0.057(3) 0.092(4) 0.085(4) 0.028(3) 0.009(3) -0.019(3)
C3 0.057(3) 0.062(3) 0.071(3) 0.027(3) 0.013(3) -0.007(3)
C4 0.058(3) 0.048(3) 0.053(3) 0.022(3) 0.009(3) -0.010(3)
C5 0.026(2) 0.032(2) 0.034(2) 0.012(2) 0.0051(19) 0.003(2)
C6 0.025(2) 0.029(2) 0.030(2) 0.0057(19) 0.0022(18) -0.0004(19)
C7 0.022(2) 0.032(2) 0.027(2) 0.0017(18) 0.0009(17) 0.0032(18)
C8 0.023(2) 0.031(2) 0.0207(19) 0.0023(17) 0.0013(17) 0.0019(18)
C9 0.026(2) 0.030(2) 0.023(2) 0.0058(18) 0.0051(17) 0.0033(18)
C10 0.027(2) 0.029(2) 0.024(2) 0.0043(18) 0.0016(18) 0.0021(19)
C11 0.044(3) 0.048(3) 0.035(2) 0.016(2) 0.010(2) -0.006(2)
C12A 0.060(3) 0.070(3) 0.046(3) 0.023(2) 0.007(2) -0.011(3)
C13A 0.051(4) 0.061(4) 0.047(3) 0.025(3) 0.012(3) 0.000(3)
C14A 0.081(6) 0.081(6) 0.055(5) 0.027(4) 0.028(4) 0.007(5)
C12B 0.060(3) 0.070(3) 0.046(3) 0.023(2) 0.007(2) -0.011(3)
C13B 0.051(4) 0.061(4) 0.047(3) 0.025(3) 0.012(3) 0.000(3)
C14B 0.081(6) 0.081(6) 0.055(5) 0.027(4) 0.028(4) 0.007(5)
C15A 0.027(2) 0.030(2) 0.032(2) 0.0047(19) 0.003(2) 0.0001(18)
C16A 0.027(2) 0.033(2) 0.037(3) 0.003(2) 0.006(2) -0.001(2)
C17A 0.028(2) 0.038(3) 0.041(2) 0.007(2) -0.001(2) -0.006(2)
C18A 0.036(3) 0.037(3) 0.045(3) 0.005(2) -0.004(3) -0.006(2)
C19A 0.039(3) 0.037(3) 0.049(3) -0.004(3) 0.009(3) 0.002(3)
C20A 0.029(3) 0.033(3) 0.039(3) 0.000(2) 0.003(2) 0.000(2)
C15B 0.027(2) 0.030(2) 0.032(2) 0.0047(19) 0.003(2) 0.0001(18)
C16B 0.027(2) 0.033(2) 0.037(3) 0.003(2) 0.006(2) -0.001(2)
C17B 0.028(2) 0.038(3) 0.041(2) 0.007(2) -0.001(2) -0.006(2)
C18B 0.036(3) 0.037(3) 0.045(3) 0.005(2) -0.004(3) -0.006(2)
C19B 0.039(3) 0.037(3) 0.049(3) -0.004(3) 0.009(3) 0.002(3)
C20B 0.029(3) 0.033(3) 0.039(3) 0.000(2) 0.003(2) 0.000(2)
C21 0.027(2) 0.026(2) 0.022(2) -0.0011(17) 0.0020(18) 0.0008(18)
C22 0.034(2) 0.034(2) 0.026(2) 0.0075(19) 0.0019(19) 0.006(2)
C23 0.043(3) 0.044(3) 0.028(2) 0.009(2) 0.002(2) 0.010(2)
C24 0.057(3) 0.042(3) 0.029(2) 0.011(2) 0.014(2) 0.009(2)
C25 0.043(3) 0.038(3) 0.035(2) 0.002(2) 0.019(2) 0.004(2)
C26 0.029(2) 0.037(3) 0.033(2) 0.002(2) 0.003(2) 0.003(2)
C27 0.129(7) 0.141(7) 0.158(8) 0.104(6) 0.095(6) 0.086(6)
C28 0.059(4) 0.069(4) 0.059(3) 0.034(3) 0.022(3) 0.026(3)
C29 0.056(3) 0.053(3) 0.042(3) 0.024(2) 0.016(2) 0.030(3)
C30 0.037(3) 0.044(3) 0.033(2) 0.016(2) 0.011(2) 0.013(2)
C31 0.031(2) 0.027(2) 0.022(2) 0.0084(18) 0.0050(18) 0.0000(19)
C32 0.028(2) 0.027(2) 0.024(2) 0.0089(17) 0.0040(18) 0.0000(18)
C33 0.027(2) 0.029(2) 0.0221(19) 0.0080(17) 0.0067(17) -0.0005(19)
C34 0.028(2) 0.028(2) 0.0195(19) 0.0063(17) 0.0027(17) -0.0019(19)
C35 0.029(2) 0.029(2) 0.026(2) 0.0107(18) 0.0058(18) 0.0044(19)
C36 0.028(2) 0.033(2) 0.025(2) 0.0076(19) 0.0061(18) 0.007(2)
C37 0.064(4) 0.088(4) 0.041(3) 0.007(3) -0.005(3) 0.044(3)
C38 0.100(4) 0.135(5) 0.106(5) 0.060(4) 0.024(4) 0.071(4)
C39 0.117(6) 0.154(7) 0.096(6) 0.019(5) -0.015(5) 0.078(6)
C40 0.095(6) 0.100(6) 0.104(6) 0.025(5) -0.004(5) 0.032(5)
C41 0.024(2) 0.027(2) 0.024(2) 0.0076(17) 0.0077(17) 0.0004(18)
C42 0.037(3) 0.029(2) 0.028(2) 0.0099(19) 0.003(2) -0.001(2)
C43 0.044(3) 0.036(3) 0.031(2) 0.017(2) -0.001(2) 0.000(2)
C44 0.037(3) 0.044(3) 0.031(2) 0.016(2) -0.003(2) -0.004(2)
C45 0.036(3) 0.035(3) 0.036(2) 0.011(2) -0.007(2) -0.005(2)
C46 0.028(2) 0.030(2) 0.034(2) 0.0147(19) 0.0019(19) 0.0006(19)
C47 0.024(2) 0.031(2) 0.026(2) 0.0043(18) 0.0017(18) 0.0033(19)
C48 0.043(3) 0.035(3) 0.036(2) 0.011(2) 0.016(2) 0.008(2)
C49 0.056(3) 0.043(3) 0.037(3) 0.011(2) 0.023(2) 0.011(3)
C50 0.033(3) 0.041(3) 0.037(2) 0.002(2) 0.012(2) 0.010(2)
C51 0.035(3) 0.034(3) 0.041(3) 0.008(2) 0.004(2) 0.004(2)
C52 0.030(2) 0.033(2) 0.028(2) 0.0083(19) 0.0055(19) 0.001(2)
N1 0.041(2) 0.043(2) 0.036(2) 0.0133(19) 0.0050(19) -0.007(2)
N2 0.0226(18) 0.029(2) 0.0234(18) 0.0041(15) -0.0015(15) -0.0011(16)
N3 0.034(2) 0.032(2) 0.0258(19) 0.0073(16) 0.0031(16) -0.0055(17)
N4 0.033(2) 0.037(2) 0.0229(18) 0.0050(17) 0.0030(16) 0.0064(18)
N5 0.0263(19) 0.0275(19) 0.0209(17) 0.0075(15) 0.0050(15) 0.0014(16)
N6 0.041(2) 0.046(2) 0.027(2) 0.0043(18) -0.0027(18) 0.019(2)
S1 0.0318(6) 0.0365(7) 0.0283(6) 0.0110(5) 0.0062(5) 0.0003(5)
S2 0.0302(6) 0.0292(6) 0.0222(5) 0.0044(5) 0.0026(5) -0.0019(5)
S3 0.0317(6) 0.0296(6) 0.0245(6) 0.0052(5) 0.0051(5) 0.0035(5)
S4 0.0291(6) 0.0362(7) 0.0244(6) 0.0077(5) 0.0001(5) 0.0029(5)
Co1 0.0260(3) 0.0283(3) 0.0207(3) 0.0050(3) 0.0024(2) 0.0007(3)

_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
C1A C2A 1.54(2) . ?
C2A C3 1.483(9) . ?
C3 C4 1.525(8) . ?
C4 N1 1.464(7) . ?
C5 N1 1.314(6) . ?
C5 C6 1.447(6) . ?
C5 S1 1.723(5) . ?
C6 N2 1.351(5) . ?
C6 C7 1.422(6) . ?
C7 C8 1.389(6) . ?
C7 C15A 1.500(5) . ?
C7 C15B 1.525(10) . ?
C8 C9 1.428(6) . ?
C8 C21 1.496(5) . ?
C9 N2 1.370(5) . ?
C9 C10 1.447(6) . ?
C10 N3 1.317(6) . ?
C10 S2 1.710(4) . ?
C11 N3 1.451(6) . ?
C11 C12A 1.499(7) . ?
C12A C13A 1.317(11) . ?
C13A C14A 1.520(13) . ?
C13B C14B 1.535(19) . ?
C15A C16A 1.3900 . ?
C15A C20A 1.3900 . ?
C16A C17A 1.3900 . ?
C17A C18A 1.3900 . ?
C18A C19A 1.3900 . ?
C19A C20A 1.3900 . ?
C15B C16B 1.3900 . ?
C15B C20B 1.3900 . ?
C16B C17B 1.3900 . ?
C17B C18B 1.3900 . ?
C18B C19B 1.3900 . ?
C19B C20B 1.3900 . ?
C21 C22 1.3900 . ?
C21 C26 1.3900 . ?
C22 C23 1.3900 . ?
C23 C24 1.3900 . ?
C24 C25 1.3900 . ?
C25 C26 1.3900 . ?
C27 C28 1.448(9) . ?
C28 C29 1.529(8) . ?
C29 C30 1.508(7) . ?
C30 N4 1.451(6) . ?
C31 N4 1.305(6) . ?
C31 C32 1.442(6) . ?
C31 S3 1.732(4) . ?
C32 N5 1.364(5) . ?
C32 C33 1.424(6) . ?
C33 C34 1.395(6) . ?
C33 C41 1.501(5) . ?
C34 C35 1.421(6) . ?
C34 C47 1.500(5) . ?
C35 N5 1.364(6) . ?
C35 C36 1.437(6) . ?
C36 N6 1.316(6) . ?
C36 S4 1.707(4) . ?
C37 N6 1.471(7) . ?
C37 C38 1.585(11) . ?
C38 C39 1.460(12) . ?
C39 C40 1.398(12) . ?
C41 C42 1.3900 . ?
C41 C46 1.3900 . ?
C42 C43 1.3900 . ?
C43 C44 1.3900 . ?
C44 C45 1.3900 . ?
C45 C46 1.3900 . ?
C47 C48 1.3900 . ?
C47 C52 1.3900 . ?
C48 C49 1.3900 . ?
C49 C50 1.3900 . ?
C50 C51 1.3900 . ?
C51 C52 1.3900 . ?
N2 Co1 1.860(3) . ?
N5 Co1 1.860(3) . ?
S1 Co1 2.2879(14) . ?
S2 Co1 2.2751(14) . ?
S3 Co1 2.2798(15) . ?
S4 Co1 2.2976(15) . ?

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
C3 C2A C1A 113.6(12) . . ?
C2A C3 C4 114.5(6) . . ?
N1 C4 C3 110.4(5) . . ?
N1 C5 C6 120.6(4) . . ?
N1 C5 S1 122.9(4) . . ?
C6 C5 S1 116.5(3) . . ?
N2 C6 C7 109.3(4) . . ?
N2 C6 C5 114.6(4) . . ?
C7 C6 C5 136.1(4) . . ?
C8 C7 C6 106.9(4) . . ?
C8 C7 C15A 122.4(4) . . ?
C6 C7 C15A 130.7(4) . . ?
C8 C7 C15B 136.7(7) . . ?
C6 C7 C15B 116.2(7) . . ?
C15A C7 C15B 14.6(6) . . ?
C7 C8 C9 106.6(4) . . ?
C7 C8 C21 127.1(4) . . ?
C9 C8 C21 126.3(4) . . ?
N2 C9 C8 108.6(4) . . ?
N2 C9 C10 114.7(4) . . ?
C8 C9 C10 136.7(4) . . ?
N3 C10 C9 121.9(4) . . ?
N3 C10 S2 121.4(3) . . ?
C9 C10 S2 116.7(3) . . ?
N3 C11 C12A 111.9(4) . . ?
C13A C12A C11 122.9(7) . . ?
C12A C13A C14A 116.6(9) . . ?
C16A C15A C20A 120.0 . . ?
C16A C15A C7 120.9(3) . . ?
C20A C15A C7 119.0(3) . . ?
C15A C16A C17A 120.0 . . ?
C16A C17A C18A 120.0 . . ?
C17A C18A C19A 120.0 . . ?
C20A C19A C18A 120.0 . . ?
C19A C20A C15A 120.0 . . ?
C16B C15B C20B 120.0 . . ?
C16B C15B C7 117.6(9) . . ?
C20B C15B C7 122.4(9) . . ?
C17B C16B C15B 120.0 . . ?
C16B C17B C18B 120.0 . . ?
C19B C18B C17B 120.0 . . ?
C20B C19B C18B 120.0 . . ?
C19B C20B C15B 120.0 . . ?
C22 C21 C26 120.0 . . ?
C22 C21 C8 119.6(2) . . ?
C26 C21 C8 120.3(2) . . ?
C23 C22 C21 120.0 . . ?
C24 C23 C22 120.0 . . ?
C23 C24 C25 120.0 . . ?
C26 C25 C24 120.0 . . ?
C25 C26 C21 120.0 . . ?
C27 C28 C29 114.1(6) . . ?
C30 C29 C28 113.5(4) . . ?
N4 C30 C29 110.1(4) . . ?
N4 C31 C32 120.5(4) . . ?
N4 C31 S3 123.2(4) . . ?
C32 C31 S3 116.3(3) . . ?
N5 C32 C33 108.5(4) . . ?
N5 C32 C31 114.7(4) . . ?
C33 C32 C31 136.8(4) . . ?
C34 C33 C32 107.0(4) . . ?
C34 C33 C41 125.6(4) . . ?
C32 C33 C41 127.5(4) . . ?
C33 C34 C35 106.8(4) . . ?
C33 C34 C47 126.2(3) . . ?
C35 C34 C47 126.7(4) . . ?
N5 C35 C34 108.8(4) . . ?
N5 C35 C36 114.8(4) . . ?
C34 C35 C36 136.4(4) . . ?
N6 C36 C35 120.1(4) . . ?
N6 C36 S4 122.4(3) . . ?
C35 C36 S4 117.5(3) . . ?
N6 C37 C38 107.5(5) . . ?
C39 C38 C37 112.4(8) . . ?
C40 C39 C38 122.9(11) . . ?
C42 C41 C46 120.0 . . ?
C42 C41 C33 120.3(2) . . ?
C46 C41 C33 119.6(2) . . ?
C41 C42 C43 120.0 . . ?
C42 C43 C44 120.0 . . ?
C43 C44 C45 120.0 . . ?
C46 C45 C44 120.0 . . ?
C45 C46 C41 120.0 . . ?
C48 C47 C52 120.0 . . ?
C48 C47 C34 118.7(2) . . ?
C52 C47 C34 121.2(2) . . ?
C47 C48 C49 120.0 . . ?
C50 C49 C48 120.0 . . ?
C49 C50 C51 120.0 . . ?
C52 C51 C50 120.0 . . ?
C51 C52 C47 120.0 . . ?
C5 N1 C4 121.5(4) . . ?
C6 N2 C9 108.6(3) . . ?
C6 N2 Co1 126.3(3) . . ?
C9 N2 Co1 125.0(3) . . ?
C10 N3 C11 123.3(4) . . ?
C31 N4 C30 123.7(4) . . ?
C35 N5 C32 108.9(3) . . ?
C35 N5 Co1 125.2(3) . . ?
C32 N5 Co1 125.9(3) . . ?
C36 N6 C37 125.8(4) . . ?
C5 S1 Co1 98.44(16) . . ?
C10 S2 Co1 98.83(16) . . ?
C31 S3 Co1 98.69(16) . . ?
C36 S4 Co1 98.02(16) . . ?
N2 Co1 N5 179.57(17) . . ?
N2 Co1 S2 84.68(12) . . ?
N5 Co1 S2 95.30(11) . . ?
N2 Co1 S3 95.19(12) . . ?
N5 Co1 S3 84.38(12) . . ?
S2 Co1 S3 91.22(6) . . ?
N2 Co1 S1 84.09(12) . . ?
N5 Co1 S1 95.94(11) . . ?
S2 Co1 S1 168.75(5) . . ?
S3 Co1 S1 90.33(6) . . ?
N2 Co1 S4 96.07(12) . . ?
N5 Co1 S4 84.36(12) . . ?
S2 Co1 S4 89.28(6) . . ?
S3 Co1 S4 168.73(5) . . ?
S1 Co1 S4 91.37(6) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.618
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.095

#===END

data_2006sot0393
_database_code_depnum_ccdc_archive 'CCDC 678034'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H44 Cl4 Co2 N6 S4'
_chemical_formula_weight         1236.91

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.9056(12)
_cell_length_b                   15.0017(17)
_cell_length_c                   20.544(2)
_cell_angle_alpha                70.153(6)
_cell_angle_beta                 77.191(6)
_cell_angle_gamma                89.844(6)
_cell_volume                     3073.0(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    11088
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      26.02

_exptl_crystal_description       Fragment
_exptl_crystal_colour            'Dark Red'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_exptl_absorpt_coefficient_mu    0.891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9262
_exptl_absorpt_correction_T_max  0.9824
_exptl_absorpt_process_details   
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;

_exptl_special_details           
;
SADABS was used to perform the Absorption correction
Parameter refinement on 18027 reflections reduced R(int) from 0.1560 to 0.0635
Ratio of minimum to maximum apparent transmission: 0.509085
The given Tmin and Tmax were generated using the SHELX SIZE command
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans to fill the asymmetric unit'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            48354
_diffrn_reflns_av_R_equivalents  0.1411
_diffrn_reflns_av_sigmaI/netI    0.1148
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         25.03
_reflns_number_total             10811
_reflns_number_gt                6150
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin, et al., 1993)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The crystals looked like they had lost solvent or degraded in some other
way

Highest peak 3.11 at 0.5852 0.4709 0.2510 [ 0.05 A from CL1 ]
Deepest hole -3.78 at 0.5558 0.4636 0.4218 [ 0.09 A from CL4 ]
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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         10811
_refine_ls_number_parameters     571
_refine_ls_number_restraints     454
_refine_ls_R_factor_all          0.2665
_refine_ls_R_factor_gt           0.1962
_refine_ls_wR_factor_ref         0.5137
_refine_ls_wR_factor_gt          0.4795
_refine_ls_goodness_of_fit_ref   1.680
_refine_ls_restrained_S_all      1.674
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.003

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.75407(17) 0.04116(13) 0.21382(9) 0.0471(6) Uani 1 1 d . . .
S1 S 0.9567(3) 0.1041(3) 0.19134(18) 0.0551(10) Uani 1 1 d . . .
S2 S 0.5469(3) -0.0105(3) 0.25564(18) 0.0530(9) Uani 1 1 d . . .
S3 S 0.8060(3) -0.1016(3) 0.28081(18) 0.0524(9) Uani 1 1 d . . .
S4 S 0.7082(4) 0.1714(3) 0.1298(2) 0.0633(11) Uani 1 1 d U . .
N1 N 1.0241(10) 0.2095(9) 0.2634(6) 0.056(3) Uani 1 1 d U . .
H1 H 0.9940 0.2343 0.2963 0.067 Uiso 1 1 calc R . .
N2 N 0.7253(10) 0.0981(8) 0.2846(5) 0.050(3) Uani 1 1 d U . .
N3 N 0.3917(10) 0.0360(8) 0.3611(5) 0.048(2) Uani 1 1 d U . .
H3 H 0.3802 0.0702 0.3890 0.058 Uiso 1 1 calc R . .
N4 N 0.8652(13) -0.2436(9) 0.2335(6) 0.063(3) Uani 1 1 d U . .
H4 H 0.8781 -0.2677 0.1992 0.075 Uiso 1 1 calc R . .
N5 N 0.7782(11) -0.0141(9) 0.1443(6) 0.058(3) Uani 1 1 d U . .
N6 N 0.7026(13) 0.1763(10) -0.0002(7) 0.076(3) Uani 1 1 d U . .
H6 H 0.7180 0.1440 -0.0294 0.091 Uiso 1 1 calc R . .
C1 C 1.2235(10) 0.2023(9) 0.1822(7) 0.094(4) Uani 1 1 d GU . .
H1A H 1.1841 0.1619 0.1647 0.112 Uiso 1 1 calc R . .
C2 C 1.3521(10) 0.2287(10) 0.1569(7) 0.103(4) Uani 1 1 d GU . .
H2 H 1.4005 0.2062 0.1220 0.124 Uiso 1 1 calc R . .
C3 C 1.4097(7) 0.2879(10) 0.1826(7) 0.097(4) Uani 1 1 d GU . .
H3A H 1.4975 0.3060 0.1652 0.117 Uiso 1 1 calc R . .
C4 C 1.3387(10) 0.3208(9) 0.2337(7) 0.085(4) Uani 1 1 d GU . .
H4A H 1.3781 0.3613 0.2512 0.102 Uiso 1 1 calc R . .
C5 C 1.2102(9) 0.2944(8) 0.2590(6) 0.076(4) Uani 1 1 d GU . .
H5 H 1.1617 0.3169 0.2940 0.091 Uiso 1 1 calc R . .
C6 C 1.1526(7) 0.2352(9) 0.2333(6) 0.068(3) Uani 1 1 d GU . .
C7 C 0.9369(13) 0.1570(10) 0.2543(7) 0.051(3) Uani 1 1 d U . .
C8 C 0.8111(13) 0.1468(10) 0.2976(7) 0.051(3) Uani 1 1 d U . .
C9 C 0.7508(11) 0.1820(9) 0.3504(6) 0.041(2) Uani 1 1 d U . .
C10 C 0.6219(12) 0.1515(9) 0.3706(6) 0.045(3) Uani 1 1 d U . .
C11 C 0.6089(12) 0.0964(10) 0.3259(7) 0.048(3) Uani 1 1 d U . .
C12 C 0.5083(12) 0.0414(10) 0.3196(7) 0.051(3) Uani 1 1 d U . .
C13 C 0.2868(7) -0.0207(7) 0.3629(5) 0.059(3) Uani 1 1 d GU . .
C14 C 0.2949(7) -0.1119(7) 0.3600(5) 0.062(3) Uani 1 1 d GU . .
H14 H 0.3745 -0.1378 0.3544 0.074 Uiso 1 1 calc R . .
C15 C 0.1866(9) -0.1650(6) 0.3654(5) 0.069(3) Uani 1 1 d GU . .
H15 H 0.1922 -0.2273 0.3635 0.082 Uiso 1 1 calc R . .
C16 C 0.0702(7) -0.1271(7) 0.3736(6) 0.073(4) Uani 1 1 d GU . .
H16 H -0.0039 -0.1634 0.3773 0.088 Uiso 1 1 calc R . .
C17 C 0.0620(7) -0.0359(8) 0.3764(6) 0.079(4) Uani 1 1 d GU . .
H17 H -0.0176 -0.0100 0.3820 0.094 Uiso 1 1 calc R . .
C18 C 0.1703(9) 0.0173(6) 0.3711(6) 0.073(4) Uani 1 1 d GU . .
H18 H 0.1648 0.0796 0.3730 0.088 Uiso 1 1 calc R . .
C19 C 0.8150(8) 0.2463(6) 0.3774(5) 0.049(3) Uani 1 1 d GU . .
C20 C 0.8844(9) 0.2097(5) 0.4284(5) 0.056(3) Uani 1 1 d GU . .
H20 H 0.8841 0.1429 0.4508 0.068 Uiso 1 1 calc R . .
C21 C 0.9540(8) 0.2710(7) 0.4469(4) 0.063(3) Uani 1 1 d GU . .
H21 H 1.0014 0.2460 0.4818 0.076 Uiso 1 1 calc R . .
C22 C 0.9544(9) 0.3687(6) 0.4142(5) 0.060(3) Uani 1 1 d GU . .
H22 H 1.0020 0.4106 0.4268 0.072 Uiso 1 1 calc R . .
C23 C 0.8851(9) 0.4053(5) 0.3631(5) 0.065(3) Uani 1 1 d GU . .
H23 H 0.8853 0.4721 0.3408 0.078 Uiso 1 1 calc R . .
C24 C 0.8154(8) 0.3440(6) 0.3447(4) 0.052(3) Uani 1 1 d GU . .
H24 H 0.7681 0.3690 0.3098 0.063 Uiso 1 1 calc R . .
C25 C 0.5219(9) 0.1703(8) 0.4231(4) 0.057(3) Uani 1 1 d GU . .
C26 C 0.5178(9) 0.1296(9) 0.4953(5) 0.092(4) Uani 1 1 d GU . .
H26 H 0.5834 0.0923 0.5106 0.110 Uiso 1 1 calc R . .
C27 C 0.4176(11) 0.1434(9) 0.5452(4) 0.096(4) Uani 1 1 d GU . .
H27 H 0.4148 0.1156 0.5945 0.115 Uiso 1 1 calc R . .
C28 C 0.3216(10) 0.1980(9) 0.5228(4) 0.081(4) Uani 1 1 d GU . .
H28 H 0.2531 0.2075 0.5569 0.097 Uiso 1 1 calc R . .
C29 C 0.3257(9) 0.2387(9) 0.4506(5) 0.086(4) Uani 1 1 d GU . .
H29 H 0.2600 0.2760 0.4353 0.103 Uiso 1 1 calc R . .
C30 C 0.4258(10) 0.2248(8) 0.4007(4) 0.078(4) Uani 1 1 d GU . .
H30 H 0.4286 0.2526 0.3514 0.093 Uiso 1 1 calc R . .
C31 C 0.7779(10) -0.3295(8) 0.3596(6) 0.079(4) Uani 1 1 d GU . .
H31 H 0.6972 -0.3128 0.3512 0.095 Uiso 1 1 calc R . .
C32 C 0.7896(11) -0.3806(8) 0.4281(5) 0.088(4) Uani 1 1 d GU . .
H32 H 0.7170 -0.3989 0.4665 0.105 Uiso 1 1 calc R . .
C33 C 0.9076(13) -0.4050(8) 0.4403(5) 0.092(4) Uani 1 1 d GU . .
H33 H 0.9157 -0.4400 0.4872 0.110 Uiso 1 1 calc R . .
C34 C 1.0139(10) -0.3783(8) 0.3841(7) 0.088(4) Uani 1 1 d GU . .
H34 H 1.0945 -0.3949 0.3925 0.106 Uiso 1 1 calc R . .
C35 C 1.0021(10) -0.3271(8) 0.3156(6) 0.086(4) Uani 1 1 d GU . .
H35 H 1.0747 -0.3089 0.2772 0.103 Uiso 1 1 calc R . .
C36 C 0.8841(12) -0.3028(7) 0.3033(5) 0.074(3) Uani 1 1 d GU . .
C37 C 0.8308(13) -0.1587(10) 0.2197(7) 0.052(3) Uani 1 1 d U . .
C38 C 0.8063(14) -0.1047(11) 0.1499(7) 0.056(3) Uani 1 1 d U . .
C39 C 0.8111(14) -0.1199(11) 0.0853(7) 0.060(3) Uani 1 1 d U . .
C40 C 0.7792(13) -0.0338(12) 0.0402(7) 0.058(3) Uani 1 1 d U . .
C41 C 0.7604(13) 0.0321(11) 0.0760(7) 0.057(3) Uani 1 1 d U . .
C42 C 0.7250(15) 0.1276(12) 0.0643(8) 0.064(3) Uani 1 1 d U . .
C43 C 0.6626(15) 0.2619(9) -0.0302(7) 0.102(4) Uani 1 1 d GU . .
C44 C 0.6662(16) 0.3360(11) -0.0043(7) 0.117(5) Uani 1 1 d GU . .
H44 H 0.7010 0.3281 0.0356 0.140 Uiso 1 1 calc R . .
C45 C 0.6188(19) 0.4217(10) -0.0368(9) 0.137(6) Uani 1 1 d GU . .
H45 H 0.6212 0.4724 -0.0191 0.164 Uiso 1 1 calc R . .
C46 C 0.5679(18) 0.4333(10) -0.0952(9) 0.141(6) Uani 1 1 d GU . .
H46 H 0.5355 0.4919 -0.1174 0.170 Uiso 1 1 calc R . .
C47 C 0.5643(18) 0.3592(12) -0.1211(7) 0.139(6) Uani 1 1 d GU . .
H47 H 0.5295 0.3672 -0.1611 0.166 Uiso 1 1 calc R . .
C48 C 0.6117(17) 0.2735(10) -0.0886(8) 0.119(5) Uani 1 1 d GU . .
H48 H 0.6093 0.2229 -0.1064 0.143 Uiso 1 1 calc R . .
C49 C 0.8365(13) -0.2073(8) 0.0690(6) 0.083(4) Uani 1 1 d GU . .
C50 C 0.7643(13) -0.2917(10) 0.1111(6) 0.101(4) Uani 1 1 d GU . .
H50 H 0.7029 -0.2943 0.1526 0.122 Uiso 1 1 calc R . .
C51 C 0.7820(15) -0.3725(8) 0.0925(7) 0.118(5) Uani 1 1 d GU . .
H51 H 0.7327 -0.4302 0.1213 0.141 Uiso 1 1 calc R . .
C52 C 0.8719(15) -0.3688(8) 0.0317(8) 0.120(5) Uani 1 1 d GU . .
H52 H 0.8840 -0.4240 0.0190 0.144 Uiso 1 1 calc R . .
C53 C 0.9441(13) -0.2844(10) -0.0104(7) 0.110(5) Uani 1 1 d GU . .
H53 H 1.0056 -0.2819 -0.0519 0.132 Uiso 1 1 calc R . .
C54 C 0.9264(13) -0.2036(8) 0.0082(7) 0.099(4) Uani 1 1 d GU . .
H54 H 0.9757 -0.1459 -0.0206 0.118 Uiso 1 1 calc R . .
C55 C 0.7637(9) -0.0133(9) -0.0331(4) 0.067(3) Uani 1 1 d GU . .
C56 C 0.6522(9) -0.0485(9) -0.0410(4) 0.084(4) Uani 1 1 d GU . .
H56 H 0.5928 -0.0892 -0.0004 0.101 Uiso 1 1 calc R . .
C57 C 0.6275(9) -0.0243(10) -0.1081(5) 0.091(4) Uani 1 1 d GU . .
H57 H 0.5513 -0.0484 -0.1135 0.109 Uiso 1 1 calc R . .
C58 C 0.7143(10) 0.0351(10) -0.1675(4) 0.088(4) Uani 1 1 d GU . .
H58 H 0.6974 0.0517 -0.2134 0.106 Uiso 1 1 calc R . .
C59 C 0.8258(9) 0.0704(9) -0.1596(4) 0.081(4) Uani 1 1 d GU . .
H59 H 0.8851 0.1111 -0.2002 0.098 Uiso 1 1 calc R . .
C60 C 0.8504(8) 0.0462(9) -0.0925(5) 0.073(3) Uani 1 1 d GU . .
H60 H 0.9266 0.0703 -0.0871 0.088 Uiso 1 1 calc R . .
Co2 Co 0.4715(2) -0.4643(2) 0.32672(13) 0.0907(10) Uani 1 1 d D . .
Cl1 Cl 0.5808(6) -0.5299(5) 0.2506(3) 0.1331(13) Uani 1 1 d D . .
Cl2 Cl 0.2683(6) -0.5188(6) 0.3630(4) 0.1331(13) Uani 1 1 d D . .
Cl3 Cl 0.4980(6) -0.3035(5) 0.2917(4) 0.1331(13) Uani 1 1 d D . .
Cl4 Cl 0.5486(6) -0.5349(6) 0.4209(3) 0.1331(13) Uani 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0444(11) 0.0604(12) 0.0319(9) -0.0154(8) -0.0004(7) -0.0058(9)
S1 0.045(2) 0.072(2) 0.0430(19) -0.0242(17) 0.0066(15) -0.0079(17)
S2 0.047(2) 0.072(2) 0.0402(18) -0.0223(17) -0.0072(15) -0.0032(18)
S3 0.051(2) 0.063(2) 0.0409(18) -0.0197(16) -0.0039(15) -0.0047(17)
S4 0.060(2) 0.072(3) 0.050(2) -0.0145(18) -0.0068(18) 0.001(2)
N1 0.041(5) 0.072(6) 0.058(5) -0.028(5) -0.008(4) 0.000(5)
N2 0.037(5) 0.064(5) 0.035(5) -0.006(4) 0.005(4) -0.007(4)
N3 0.043(5) 0.057(5) 0.035(5) -0.004(4) -0.008(4) -0.009(4)
N4 0.080(6) 0.057(6) 0.052(5) -0.028(5) -0.004(5) 0.003(5)
N5 0.050(5) 0.074(6) 0.036(5) -0.009(5) 0.003(4) -0.009(5)
N6 0.080(7) 0.086(7) 0.051(6) -0.011(5) -0.017(5) 0.002(6)
C1 0.057(7) 0.111(8) 0.101(8) -0.042(7) 0.013(6) -0.023(7)
C2 0.061(7) 0.120(9) 0.112(8) -0.044(7) 0.016(7) -0.025(7)
C3 0.060(7) 0.105(9) 0.106(8) -0.031(7) 0.012(7) -0.019(7)
C4 0.056(7) 0.095(8) 0.085(8) -0.019(7) 0.003(6) -0.020(6)
C5 0.054(6) 0.083(8) 0.076(7) -0.022(6) 0.004(6) -0.012(6)
C6 0.045(5) 0.085(7) 0.072(6) -0.032(5) 0.002(5) -0.004(5)
C7 0.040(5) 0.058(6) 0.054(6) -0.018(5) -0.009(5) 0.001(5)
C8 0.043(5) 0.059(5) 0.045(5) -0.015(4) -0.004(4) -0.008(5)
C9 0.036(5) 0.050(5) 0.038(5) -0.019(4) -0.002(4) 0.001(4)
C10 0.042(5) 0.055(5) 0.032(4) -0.008(4) -0.007(4) 0.005(4)
C11 0.038(5) 0.058(5) 0.036(5) -0.007(4) -0.003(4) 0.004(4)
C12 0.039(5) 0.062(6) 0.041(5) -0.005(5) -0.008(5) -0.004(5)
C13 0.052(5) 0.071(6) 0.038(5) 0.000(5) -0.008(5) -0.005(5)
C14 0.058(6) 0.079(7) 0.038(5) -0.007(5) -0.009(5) -0.010(6)
C15 0.066(6) 0.083(7) 0.046(6) -0.009(6) -0.013(6) -0.017(6)
C16 0.060(6) 0.080(7) 0.060(6) 0.002(6) -0.016(6) -0.009(6)
C17 0.055(6) 0.084(7) 0.071(7) 0.007(7) -0.015(6) 0.003(6)
C18 0.055(6) 0.076(7) 0.060(6) 0.007(6) -0.008(6) 0.001(6)
C19 0.040(5) 0.057(5) 0.045(5) -0.014(4) -0.006(4) 0.003(5)
C20 0.048(6) 0.071(6) 0.049(6) -0.021(5) -0.009(5) 0.003(5)
C21 0.057(6) 0.084(7) 0.050(6) -0.028(6) -0.011(5) 0.001(6)
C22 0.058(6) 0.079(7) 0.056(6) -0.039(5) -0.013(5) -0.002(6)
C23 0.059(6) 0.071(7) 0.063(6) -0.027(6) -0.006(5) 0.000(6)
C24 0.047(6) 0.061(6) 0.050(6) -0.023(5) -0.007(5) -0.002(5)
C25 0.059(6) 0.066(6) 0.039(5) -0.013(5) -0.003(5) 0.017(5)
C26 0.085(7) 0.098(8) 0.054(6) 0.006(6) 0.008(6) 0.035(7)
C27 0.088(8) 0.100(8) 0.057(7) 0.002(6) 0.019(6) 0.041(7)
C28 0.079(7) 0.086(8) 0.052(6) -0.010(6) 0.013(6) 0.033(6)
C29 0.078(7) 0.092(8) 0.057(6) -0.002(6) 0.006(6) 0.035(6)
C30 0.078(7) 0.084(7) 0.048(6) -0.005(6) 0.004(6) 0.028(6)
C31 0.113(8) 0.060(7) 0.062(7) -0.010(6) -0.032(6) 0.003(7)
C32 0.127(9) 0.061(7) 0.075(7) -0.015(6) -0.037(7) 0.003(7)
C33 0.132(9) 0.060(7) 0.089(8) -0.021(6) -0.044(7) -0.006(7)
C34 0.122(9) 0.052(7) 0.093(8) -0.016(6) -0.046(7) -0.006(7)
C35 0.112(8) 0.060(7) 0.086(7) -0.016(6) -0.039(7) -0.006(7)
C36 0.099(7) 0.058(6) 0.069(6) -0.022(5) -0.030(6) 0.001(6)
C37 0.054(6) 0.057(6) 0.043(5) -0.022(5) 0.001(5) -0.003(5)
C38 0.051(5) 0.065(6) 0.045(5) -0.018(5) 0.002(5) -0.009(5)
C39 0.059(6) 0.075(6) 0.041(5) -0.021(5) 0.002(5) -0.019(5)
C40 0.048(5) 0.086(6) 0.036(5) -0.021(5) -0.003(4) -0.022(5)
C41 0.046(5) 0.075(6) 0.041(5) -0.014(5) -0.003(4) -0.009(5)
C42 0.056(5) 0.077(6) 0.050(5) -0.011(5) -0.010(5) -0.001(5)
C43 0.119(8) 0.104(8) 0.067(7) -0.002(6) -0.031(6) 0.011(7)
C44 0.146(10) 0.111(9) 0.075(8) -0.004(7) -0.033(8) 0.021(9)
C45 0.167(11) 0.122(10) 0.095(9) -0.004(8) -0.031(9) 0.020(9)
C46 0.168(11) 0.125(10) 0.098(9) 0.006(9) -0.037(9) 0.022(10)
C47 0.161(11) 0.127(10) 0.093(9) 0.007(8) -0.034(9) 0.016(10)
C48 0.139(10) 0.117(9) 0.077(8) 0.002(8) -0.033(8) 0.012(9)
C49 0.087(7) 0.090(7) 0.060(6) -0.027(6) 0.006(6) -0.020(6)
C50 0.108(8) 0.104(8) 0.074(8) -0.031(7) 0.018(7) -0.028(8)
C51 0.124(9) 0.109(9) 0.092(8) -0.032(8) 0.026(8) -0.022(8)
C52 0.126(10) 0.112(9) 0.097(9) -0.038(8) 0.025(8) -0.018(8)
C53 0.113(9) 0.106(9) 0.094(8) -0.040(7) 0.020(8) -0.014(8)
C54 0.096(8) 0.099(8) 0.083(8) -0.031(7) 0.013(7) -0.013(7)
C55 0.053(5) 0.106(7) 0.035(5) -0.024(5) 0.003(5) -0.026(5)
C56 0.066(7) 0.127(8) 0.048(6) -0.021(6) -0.005(6) -0.036(7)
C57 0.071(7) 0.139(9) 0.051(6) -0.023(7) -0.005(6) -0.039(7)
C58 0.068(7) 0.135(9) 0.048(6) -0.025(7) 0.002(6) -0.026(7)
C59 0.058(7) 0.129(9) 0.041(6) -0.021(6) 0.008(6) -0.026(7)
C60 0.048(6) 0.121(8) 0.040(5) -0.024(6) 0.004(5) -0.028(6)
Co2 0.0702(16) 0.133(2) 0.0568(14) -0.0202(15) -0.0114(12) 0.0126(16)
Cl1 0.107(2) 0.166(3) 0.104(2) -0.027(2) -0.0096(18) 0.004(2)
Cl2 0.107(2) 0.166(3) 0.104(2) -0.027(2) -0.0096(18) 0.004(2)
Cl3 0.107(2) 0.166(3) 0.104(2) -0.027(2) -0.0096(18) 0.004(2)
Cl4 0.107(2) 0.166(3) 0.104(2) -0.027(2) -0.0096(18) 0.004(2)

_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 N5 1.852(12) . ?
Co1 N2 1.892(12) . ?
Co1 S4 2.266(4) . ?
Co1 S3 2.267(4) . ?
Co1 S2 2.267(4) . ?
Co1 S1 2.291(4) . ?
S1 C7 1.710(15) . ?
S2 C12 1.720(15) . ?
S3 C37 1.720(14) . ?
S4 C42 1.664(17) . ?
N1 C7 1.319(18) . ?
N1 C6 1.397(13) . ?
N2 C8 1.315(18) . ?
N2 C11 1.356(16) . ?
N3 C12 1.351(16) . ?
N3 C13 1.414(13) . ?
N4 C37 1.282(18) . ?
N4 C36 1.468(15) . ?
N5 C38 1.365(19) . ?
N5 C41 1.396(18) . ?
N6 C43 1.342(17) . ?
N6 C42 1.354(19) . ?
C1 C2 1.3900 . ?
C1 C6 1.3900 . ?
C2 C3 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C7 C8 1.437(19) . ?
C8 C9 1.399(18) . ?
C9 C10 1.404(18) . ?
C9 C19 1.505(14) . ?
C10 C25 1.455(14) . ?
C10 C11 1.456(19) . ?
C11 C12 1.43(2) . ?
C13 C14 1.3900 . ?
C13 C18 1.3900 . ?
C14 C15 1.3900 . ?
C15 C16 1.3900 . ?
C16 C17 1.3900 . ?
C17 C18 1.3900 . ?
C19 C20 1.3900 . ?
C19 C24 1.3900 . ?
C20 C21 1.3900 . ?
C21 C22 1.3900 . ?
C22 C23 1.3900 . ?
C23 C24 1.3900 . ?
C25 C26 1.3900 . ?
C25 C30 1.3900 . ?
C26 C27 1.3900 . ?
C27 C28 1.3900 . ?
C28 C29 1.3900 . ?
C29 C30 1.3900 . ?
C31 C32 1.3900 . ?
C31 C36 1.3900 . ?
C32 C33 1.3900 . ?
C33 C34 1.3900 . ?
C34 C35 1.3900 . ?
C35 C36 1.3900 . ?
C37 C38 1.47(2) . ?
C38 C39 1.41(2) . ?
C39 C40 1.41(2) . ?
C39 C49 1.471(19) . ?
C40 C41 1.41(2) . ?
C40 C55 1.481(15) . ?
C41 C42 1.44(2) . ?
C43 C44 1.3900 . ?
C43 C48 1.3900 . ?
C44 C45 1.3900 . ?
C45 C46 1.3900 . ?
C46 C47 1.3900 . ?
C47 C48 1.3900 . ?
C49 C50 1.3900 . ?
C49 C54 1.3900 . ?
C50 C51 1.3900 . ?
C51 C52 1.3900 . ?
C52 C53 1.3900 . ?
C53 C54 1.3900 . ?
C55 C56 1.3900 . ?
C55 C60 1.3900 . ?
C56 C57 1.3900 . ?
C57 C58 1.3900 . ?
C58 C59 1.3900 . ?
C59 C60 1.3900 . ?
Co2 Cl4 2.214(6) . ?
Co2 Cl2 2.235(6) . ?
Co2 Cl1 2.247(6) . ?
Co2 Cl3 2.270(7) . ?

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
N5 Co1 N2 178.6(5) . . ?
N5 Co1 S4 85.7(4) . . ?
N2 Co1 S4 93.5(4) . . ?
N5 Co1 S3 83.0(4) . . ?
N2 Co1 S3 97.7(3) . . ?
S4 Co1 S3 168.79(16) . . ?
N5 Co1 S2 93.7(4) . . ?
N2 Co1 S2 85.1(3) . . ?
S4 Co1 S2 90.94(15) . . ?
S3 Co1 S2 89.93(14) . . ?
N5 Co1 S1 98.1(4) . . ?
N2 Co1 S1 83.1(3) . . ?
S4 Co1 S1 91.18(16) . . ?
S3 Co1 S1 90.27(15) . . ?
S2 Co1 S1 168.05(15) . . ?
C7 S1 Co1 99.2(5) . . ?
C12 S2 Co1 99.1(5) . . ?
C37 S3 Co1 100.3(5) . . ?
C42 S4 Co1 98.0(6) . . ?
C7 N1 C6 135.4(12) . . ?
C8 N2 C11 112.2(12) . . ?
C8 N2 Co1 125.4(9) . . ?
C11 N2 Co1 122.3(10) . . ?
C12 N3 C13 124.5(12) . . ?
C37 N4 C36 123.5(12) . . ?
C38 N5 C41 107.9(12) . . ?
C38 N5 Co1 128.6(10) . . ?
C41 N5 Co1 123.3(11) . . ?
C43 N6 C42 135.2(16) . . ?
C2 C1 C6 120.0 . . ?
C3 C2 C1 120.0 . . ?
C4 C3 C2 120.0 . . ?
C3 C4 C5 120.0 . . ?
C6 C5 C4 120.0 . . ?
C5 C6 C1 120.0 . . ?
C5 C6 N1 116.3(9) . . ?
C1 C6 N1 123.6(9) . . ?
N1 C7 C8 118.5(13) . . ?
N1 C7 S1 125.9(11) . . ?
C8 C7 S1 115.5(11) . . ?
N2 C8 C9 107.8(12) . . ?
N2 C8 C7 116.8(13) . . ?
C9 C8 C7 135.3(14) . . ?
C8 C9 C10 109.0(12) . . ?
C8 C9 C19 124.4(11) . . ?
C10 C9 C19 126.6(10) . . ?
C9 C10 C25 129.1(12) . . ?
C9 C10 C11 104.1(10) . . ?
C25 C10 C11 126.8(12) . . ?
N2 C11 C12 117.7(13) . . ?
N2 C11 C10 106.9(12) . . ?
C12 C11 C10 135.3(12) . . ?
N3 C12 C11 119.4(13) . . ?
N3 C12 S2 125.0(11) . . ?
C11 C12 S2 115.6(10) . . ?
C14 C13 C18 120.0 . . ?
C14 C13 N3 123.3(8) . . ?
C18 C13 N3 116.6(8) . . ?
C13 C14 C15 120.0 . . ?
C14 C15 C16 120.0 . . ?
C17 C16 C15 120.0 . . ?
C16 C17 C18 120.0 . . ?
C17 C18 C13 120.0 . . ?
C20 C19 C24 120.0 . . ?
C20 C19 C9 121.1(7) . . ?
C24 C19 C9 118.6(7) . . ?
C21 C20 C19 120.0 . . ?
C20 C21 C22 120.0 . . ?
C21 C22 C23 120.0 . . ?
C24 C23 C22 120.0 . . ?
C23 C24 C19 120.0 . . ?
C26 C25 C30 120.0 . . ?
C26 C25 C10 120.6(7) . . ?
C30 C25 C10 119.3(7) . . ?
C25 C26 C27 120.0 . . ?
C28 C27 C26 120.0 . . ?
C29 C28 C27 120.0 . . ?
C28 C29 C30 120.0 . . ?
C29 C30 C25 120.0 . . ?
C32 C31 C36 120.0 . . ?
C31 C32 C33 120.0 . . ?
C32 C33 C34 120.0 . . ?
C35 C34 C33 120.0 . . ?
C36 C35 C34 120.0 . . ?
C35 C36 C31 120.0 . . ?
C35 C36 N4 123.1(9) . . ?
C31 C36 N4 116.7(9) . . ?
N4 C37 C38 121.1(13) . . ?
N4 C37 S3 123.3(11) . . ?
C38 C37 S3 115.6(11) . . ?
N5 C38 C39 110.9(13) . . ?
N5 C38 C37 112.2(12) . . ?
C39 C38 C37 136.8(15) . . ?
C40 C39 C38 104.6(14) . . ?
C40 C39 C49 126.9(13) . . ?
C38 C39 C49 128.5(14) . . ?
C39 C40 C41 109.5(12) . . ?
C39 C40 C55 126.8(14) . . ?
C41 C40 C55 123.6(14) . . ?
N5 C41 C40 107.0(13) . . ?
N5 C41 C42 113.3(13) . . ?
C40 C41 C42 139.7(14) . . ?
N6 C42 C41 116.8(15) . . ?
N6 C42 S4 123.5(13) . . ?
C41 C42 S4 119.7(11) . . ?
N6 C43 C44 123.3(12) . . ?
N6 C43 C48 116.6(12) . . ?
C44 C43 C48 120.0 . . ?
C45 C44 C43 120.0 . . ?
C44 C45 C46 120.0 . . ?
C47 C46 C45 120.0 . . ?
C46 C47 C48 120.0 . . ?
C47 C48 C43 120.0 . . ?
C50 C49 C54 120.0 . . ?
C50 C49 C39 120.1(9) . . ?
C54 C49 C39 119.7(9) . . ?
C49 C50 C51 120.0 . . ?
C52 C51 C50 120.0 . . ?
C51 C52 C53 120.0 . . ?
C54 C53 C52 120.0 . . ?
C53 C54 C49 120.0 . . ?
C56 C55 C60 120.0 . . ?
C56 C55 C40 117.5(8) . . ?
C60 C55 C40 122.2(8) . . ?
C55 C56 C57 120.0 . . ?
C56 C57 C58 120.0 . . ?
C59 C58 C57 120.0 . . ?
C60 C59 C58 120.0 . . ?
C59 C60 C55 120.0 . . ?
Cl4 Co2 Cl2 103.7(3) . . ?
Cl4 Co2 Cl1 99.9(3) . . ?
Cl2 Co2 Cl1 111.6(3) . . ?
Cl4 Co2 Cl3 111.8(3) . . ?
Cl2 Co2 Cl3 112.6(3) . . ?
Cl1 Co2 Cl3 115.9(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         3.109
_refine_diff_density_min         -3.782
_refine_diff_density_rms         0.206

#===END

data_2006sot0637
_database_code_depnum_ccdc_archive 'CCDC 678035'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H25 N5 O2'
_chemical_formula_weight         487.55

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'

_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                   9.6907(3)
_cell_length_b                   10.9090(3)
_cell_length_c                   12.3922(3)
_cell_angle_alpha                87.119(2)
_cell_angle_beta                 67.8340(10)
_cell_angle_gamma                77.531(2)
_cell_volume                     1183.91(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5246
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             512
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9725
_exptl_absorpt_correction_T_max  0.9930
_exptl_absorpt_process_details   
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;

_exptl_special_details           
;
SADABS was used to perform the Absorption correction
Parameter refinement on 16868 reflections reduced R(int) from 0.1459 to 0.0432
Ratio of minimum to maximum apparent transmission: 0.803112
The given Tmin and Tmax were generated using the SHELX SIZE command
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans to fill the asymmetric unit'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22295
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.28
_diffrn_reflns_theta_max         27.48
_reflns_number_total             5409
_reflns_number_gt                4353
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin, et al., 1993)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0355P)^2^+0.7319P] where P=(Fo^2^+2Fc^2^)/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         5409
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0483
_refine_ls_wR_factor_ref         0.1129
_refine_ls_wR_factor_gt          0.1059
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.22601(19) -0.27712(16) 0.01333(15) 0.0283(4) Uani 1 1 d . . .
H1 H 0.2650 -0.3275 0.0645 0.034 Uiso 1 1 calc R . .
C2 C 0.15354(19) -0.33037(16) -0.04336(15) 0.0284(4) Uani 1 1 d . . .
H2 H 0.1439 -0.4154 -0.0320 0.034 Uiso 1 1 calc R . .
C3 C 0.09534(18) -0.25658(16) -0.11724(15) 0.0264(4) Uani 1 1 d . . .
H3 H 0.0443 -0.2899 -0.1572 0.032 Uiso 1 1 calc R . .
C4 C 0.11283(17) -0.13390(16) -0.13165(14) 0.0232(3) Uani 1 1 d . . .
H4 H 0.0730 -0.0812 -0.1811 0.028 Uiso 1 1 calc R . .
C5 C 0.18958(17) -0.08844(15) -0.07269(13) 0.0199(3) Uani 1 1 d . . .
C6 C 0.21935(18) 0.04248(15) -0.09226(13) 0.0218(3) Uani 1 1 d . . .
H6A H 0.3009 0.0450 -0.1697 0.026 Uiso 1 1 calc R . .
H6B H 0.1259 0.1019 -0.0913 0.026 Uiso 1 1 calc R . .
C7 C 0.28535(17) 0.19751(15) 0.00393(13) 0.0193(3) Uani 1 1 d . . .
C8 C 0.32655(17) 0.22744(14) 0.10116(13) 0.0181(3) Uani 1 1 d . . .
C9 C 0.31931(16) 0.17049(14) 0.20562(13) 0.0178(3) Uani 1 1 d . . .
C10 C 0.37816(16) 0.24357(14) 0.26304(13) 0.0171(3) Uani 1 1 d . . .
C11 C 0.41640(16) 0.34414(14) 0.19182(13) 0.0173(3) Uani 1 1 d . . .
C12 C 0.47478(16) 0.45646(14) 0.20114(13) 0.0172(3) Uani 1 1 d . . .
C13 C 0.57370(18) 0.57253(14) 0.31039(14) 0.0208(3) Uani 1 1 d . . .
H13A H 0.4999 0.6236 0.3802 0.025 Uiso 1 1 calc R . .
H13B H 0.5888 0.6268 0.2422 0.025 Uiso 1 1 calc R . .
C14 C 0.72394(18) 0.52722(14) 0.32547(13) 0.0200(3) Uani 1 1 d . . .
C15 C 0.85742(18) 0.55820(15) 0.24800(14) 0.0235(3) Uani 1 1 d . . .
H15 H 0.8572 0.6071 0.1824 0.028 Uiso 1 1 calc R . .
C16 C 0.99089(19) 0.51658(16) 0.26797(16) 0.0291(4) Uani 1 1 d . . .
H16 H 1.0838 0.5362 0.2161 0.035 Uiso 1 1 calc R . .
C17 C 0.9869(2) 0.44625(17) 0.36417(17) 0.0341(4) Uani 1 1 d . . .
H17 H 1.0762 0.4173 0.3809 0.041 Uiso 1 1 calc R . .
C18 C 0.8494(2) 0.4193(2) 0.43542(18) 0.0413(5) Uani 1 1 d . . .
H18 H 0.8472 0.3700 0.5013 0.050 Uiso 1 1 calc R . .
C19 C 0.25696(17) 0.05670(14) 0.25017(13) 0.0171(3) Uani 1 1 d . . .
C20 C 0.34727(18) -0.06340(15) 0.22027(14) 0.0214(3) Uani 1 1 d . . .
H20 H 0.4527 -0.0733 0.1737 0.026 Uiso 1 1 calc R . .
C21 C 0.28642(19) -0.16921(15) 0.25707(15) 0.0255(4) Uani 1 1 d . . .
H21 H 0.3496 -0.2507 0.2353 0.031 Uiso 1 1 calc R . .
C22 C 0.1331(2) -0.15535(16) 0.32571(15) 0.0259(4) Uani 1 1 d . . .
H22 H 0.0907 -0.2275 0.3507 0.031 Uiso 1 1 calc R . .
C23 C 0.04124(19) -0.03647(16) 0.35800(14) 0.0255(4) Uani 1 1 d . . .
H23 H -0.0637 -0.0271 0.4058 0.031 Uiso 1 1 calc R . .
C24 C 0.10291(17) 0.06909(15) 0.32035(13) 0.0209(3) Uani 1 1 d . . .
H24 H 0.0396 0.1505 0.3426 0.025 Uiso 1 1 calc R . .
C25 C 0.39715(17) 0.21259(13) 0.37558(13) 0.0170(3) Uani 1 1 d . . .
C26 C 0.27202(17) 0.20468(14) 0.47776(13) 0.0195(3) Uani 1 1 d . . .
H26 H 0.1725 0.2209 0.4761 0.023 Uiso 1 1 calc R . .
C27 C 0.29217(19) 0.17334(15) 0.58135(14) 0.0234(3) Uani 1 1 d . . .
H27 H 0.2063 0.1686 0.6502 0.028 Uiso 1 1 calc R . .
C28 C 0.43659(19) 0.14886(15) 0.58533(14) 0.0235(3) Uani 1 1 d . . .
H28 H 0.4499 0.1270 0.6565 0.028 Uiso 1 1 calc R . .
C29 C 0.56109(19) 0.15651(14) 0.48498(14) 0.0227(3) Uani 1 1 d . . .
H29 H 0.6603 0.1406 0.4873 0.027 Uiso 1 1 calc R . .
C30 C 0.54164(17) 0.18730(14) 0.38105(13) 0.0193(3) Uani 1 1 d . . .
H30 H 0.6282 0.1912 0.3124 0.023 Uiso 1 1 calc R . .
N1 N 0.24422(15) -0.15778(13) -0.00018(12) 0.0248(3) Uani 1 1 d . . .
N2 N 0.26486(15) 0.08033(12) -0.00261(11) 0.0206(3) Uani 1 1 d . . .
H92 H 0.2794 0.0256 0.0487 0.025 Uiso 1 1 calc R . .
N3 N 0.38356(14) 0.33281(12) 0.09572(11) 0.0177(3) Uani 1 1 d . . .
H93 H 0.3971 0.3856 0.0384 0.021 Uiso 1 1 calc R . .
N4 N 0.51141(15) 0.46763(12) 0.29349(11) 0.0202(3) Uani 1 1 d . . .
H94 H 0.4975 0.4095 0.3461 0.024 Uiso 1 1 calc R . .
N5 N 0.71877(17) 0.45767(15) 0.41816(13) 0.0329(4) Uani 1 1 d . . .
O1 O 0.27199(14) 0.27640(11) -0.06798(10) 0.0288(3) Uani 1 1 d . . .
O2 O 0.48604(13) 0.53534(10) 0.12491(10) 0.0241(3) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0285(9) 0.0275(9) 0.0291(9) 0.0031(7) -0.0109(7) -0.0069(7)
C2 0.0267(9) 0.0242(8) 0.0322(9) -0.0028(7) -0.0065(7) -0.0083(7)
C3 0.0209(8) 0.0313(9) 0.0270(9) -0.0083(7) -0.0063(7) -0.0082(7)
C4 0.0197(8) 0.0316(9) 0.0189(8) -0.0017(7) -0.0065(6) -0.0073(7)
C5 0.0155(7) 0.0269(8) 0.0156(7) -0.0022(6) -0.0028(6) -0.0058(6)
C6 0.0242(8) 0.0296(8) 0.0164(7) 0.0031(6) -0.0093(6) -0.0130(7)
C7 0.0171(7) 0.0264(8) 0.0172(7) 0.0057(6) -0.0071(6) -0.0101(6)
C8 0.0181(7) 0.0205(7) 0.0176(7) 0.0039(6) -0.0070(6) -0.0083(6)
C9 0.0161(7) 0.0213(7) 0.0170(7) 0.0029(6) -0.0060(6) -0.0067(6)
C10 0.0150(7) 0.0201(7) 0.0163(7) 0.0021(6) -0.0046(6) -0.0066(6)
C11 0.0158(7) 0.0205(7) 0.0162(7) 0.0017(6) -0.0064(6) -0.0045(6)
C12 0.0154(7) 0.0187(7) 0.0166(7) 0.0012(6) -0.0048(6) -0.0041(6)
C13 0.0245(8) 0.0177(7) 0.0240(8) 0.0014(6) -0.0119(7) -0.0073(6)
C14 0.0252(8) 0.0171(7) 0.0208(8) 0.0011(6) -0.0114(6) -0.0058(6)
C15 0.0271(8) 0.0217(8) 0.0233(8) 0.0035(6) -0.0108(7) -0.0062(7)
C16 0.0234(8) 0.0283(9) 0.0345(10) 0.0001(7) -0.0099(7) -0.0052(7)
C17 0.0301(9) 0.0339(10) 0.0433(11) 0.0035(8) -0.0229(9) -0.0007(8)
C18 0.0412(11) 0.0493(12) 0.0400(11) 0.0221(10) -0.0252(9) -0.0095(9)
C19 0.0193(7) 0.0211(7) 0.0147(7) 0.0033(6) -0.0091(6) -0.0076(6)
C20 0.0195(7) 0.0241(8) 0.0230(8) 0.0025(6) -0.0106(6) -0.0052(6)
C21 0.0314(9) 0.0192(8) 0.0313(9) 0.0040(7) -0.0185(7) -0.0044(7)
C22 0.0337(9) 0.0252(8) 0.0275(9) 0.0098(7) -0.0169(7) -0.0165(7)
C23 0.0228(8) 0.0316(9) 0.0241(8) 0.0048(7) -0.0067(7) -0.0144(7)
C24 0.0202(7) 0.0219(8) 0.0211(8) -0.0005(6) -0.0071(6) -0.0066(6)
C25 0.0213(7) 0.0146(7) 0.0169(7) 0.0015(6) -0.0082(6) -0.0058(6)
C26 0.0188(7) 0.0212(8) 0.0205(8) 0.0021(6) -0.0077(6) -0.0083(6)
C27 0.0288(8) 0.0247(8) 0.0182(8) 0.0039(6) -0.0068(7) -0.0135(7)
C28 0.0358(9) 0.0205(8) 0.0214(8) 0.0059(6) -0.0158(7) -0.0123(7)
C29 0.0258(8) 0.0183(8) 0.0289(9) 0.0011(6) -0.0164(7) -0.0038(6)
C30 0.0191(7) 0.0193(7) 0.0190(7) 0.0007(6) -0.0061(6) -0.0049(6)
N1 0.0234(7) 0.0291(7) 0.0245(7) 0.0022(6) -0.0102(6) -0.0090(6)
N2 0.0255(7) 0.0253(7) 0.0169(6) 0.0055(5) -0.0116(5) -0.0115(6)
N3 0.0202(6) 0.0200(6) 0.0168(6) 0.0059(5) -0.0088(5) -0.0098(5)
N4 0.0272(7) 0.0202(6) 0.0185(6) 0.0062(5) -0.0116(6) -0.0118(5)
N5 0.0313(8) 0.0388(9) 0.0327(8) 0.0167(7) -0.0162(7) -0.0117(7)
O1 0.0383(7) 0.0334(7) 0.0278(6) 0.0146(5) -0.0216(6) -0.0206(5)
O2 0.0351(6) 0.0211(6) 0.0219(6) 0.0072(5) -0.0150(5) -0.0119(5)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.345(2) . ?
C1 C2 1.383(2) . ?
C2 C3 1.387(3) . ?
C3 C4 1.379(2) . ?
C4 C5 1.392(2) . ?
C5 N1 1.333(2) . ?
C5 C6 1.507(2) . ?
C6 N2 1.4470(19) . ?
C7 O1 1.2302(18) . ?
C7 N2 1.346(2) . ?
C7 C8 1.475(2) . ?
C8 N3 1.3672(18) . ?
C8 C9 1.391(2) . ?
C9 C10 1.424(2) . ?
C9 C19 1.488(2) . ?
C10 C11 1.397(2) . ?
C10 C25 1.488(2) . ?
C11 N3 1.3611(19) . ?
C11 C12 1.483(2) . ?
C12 O2 1.2352(18) . ?
C12 N4 1.3379(19) . ?
C13 N4 1.4614(18) . ?
C13 C14 1.511(2) . ?
C14 N5 1.335(2) . ?
C14 C15 1.389(2) . ?
C15 C16 1.385(2) . ?
C16 C17 1.377(3) . ?
C17 C18 1.378(3) . ?
C18 N5 1.338(2) . ?
C19 C20 1.389(2) . ?
C19 C24 1.396(2) . ?
C20 C21 1.388(2) . ?
C21 C22 1.385(2) . ?
C22 C23 1.385(2) . ?
C23 C24 1.391(2) . ?
C25 C30 1.394(2) . ?
C25 C26 1.399(2) . ?
C26 C27 1.385(2) . ?
C27 C28 1.386(2) . ?
C28 C29 1.382(2) . ?
C29 C30 1.385(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
N1 C1 C2 123.45(16) . . ?
C1 C2 C3 118.34(16) . . ?
C4 C3 C2 118.82(15) . . ?
C3 C4 C5 119.08(15) . . ?
N1 C5 C4 122.71(15) . . ?
N1 C5 C6 116.80(13) . . ?
C4 C5 C6 120.45(14) . . ?
N2 C6 C5 110.52(13) . . ?
O1 C7 N2 122.06(14) . . ?
O1 C7 C8 121.01(14) . . ?
N2 C7 C8 116.94(13) . . ?
N3 C8 C9 107.86(13) . . ?
N3 C8 C7 118.49(13) . . ?
C9 C8 C7 133.65(14) . . ?
C8 C9 C10 107.22(13) . . ?
C8 C9 C19 126.12(13) . . ?
C10 C9 C19 126.63(13) . . ?
C11 C10 C9 106.66(13) . . ?
C11 C10 C25 128.43(13) . . ?
C9 C10 C25 124.89(13) . . ?
N3 C11 C10 108.13(13) . . ?
N3 C11 C12 116.82(13) . . ?
C10 C11 C12 134.98(14) . . ?
O2 C12 N4 123.18(14) . . ?
O2 C12 C11 119.11(13) . . ?
N4 C12 C11 117.70(13) . . ?
N4 C13 C14 111.54(12) . . ?
N5 C14 C15 122.81(15) . . ?
N5 C14 C13 115.71(14) . . ?
C15 C14 C13 121.47(14) . . ?
C16 C15 C14 118.86(15) . . ?
C17 C16 C15 119.00(16) . . ?
C16 C17 C18 117.94(16) . . ?
N5 C18 C17 124.44(17) . . ?
C20 C19 C24 118.40(14) . . ?
C20 C19 C9 121.60(13) . . ?
C24 C19 C9 119.96(13) . . ?
C21 C20 C19 121.27(15) . . ?
C22 C21 C20 119.63(15) . . ?
C21 C22 C23 120.12(15) . . ?
C22 C23 C24 119.91(15) . . ?
C23 C24 C19 120.67(15) . . ?
C30 C25 C26 118.22(14) . . ?
C30 C25 C10 120.52(13) . . ?
C26 C25 C10 121.24(13) . . ?
C27 C26 C25 120.47(14) . . ?
C26 C27 C28 120.57(15) . . ?
C29 C28 C27 119.49(15) . . ?
C28 C29 C30 120.17(15) . . ?
C29 C30 C25 121.08(14) . . ?
C5 N1 C1 117.58(14) . . ?
C7 N2 C6 121.39(13) . . ?
C11 N3 C8 110.10(12) . . ?
C12 N4 C13 122.58(13) . . ?
C14 N5 C18 116.95(15) . . ?

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
N3 H93 O2 0.88 2.15 2.9872(16) 157.8 2_665

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.048

#===END

data_2006sot1194
_database_code_depnum_ccdc_archive 'CCDC 678036'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H44 Cl4 Co N6 O6'
_chemical_formula_weight         761.42

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'
Cl Cl 0.1484 0.1585 '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   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                   15.3090(6)
_cell_length_b                   21.0300(14)
_cell_length_c                   13.4079(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 124.112(3)
_cell_angle_gamma                90.00
_cell_volume                     3573.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    3678
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      27.48

_exptl_crystal_description       Block
_exptl_crystal_colour            Pink
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1588
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6727
_exptl_absorpt_correction_T_max  0.8521
_exptl_absorpt_process_details   
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;

_exptl_special_details           
;
SADABS was used to perform the Absorption correction
Parameter refinement on 15295 reflections reduced R(int) from 0.0614 to 0.0433
Ratio of minimum to maximum apparent transmission: 0.829478
The given Tmin and Tmax were generated using the SHELX SIZE command
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans to fill the asymmetric unit'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24246
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.19
_diffrn_reflns_theta_max         27.48
_reflns_number_total             4072
_reflns_number_gt                3005
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin, et al., 1993)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0420P)^2^+3.1184P] where P=(Fo^2^+2Fc^2^)/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         4072
_refine_ls_number_parameters     212
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0385
_refine_ls_wR_factor_ref         0.0909
_refine_ls_wR_factor_gt          0.0805
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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
C1 C -0.1137(2) 0.20667(19) 0.0696(3) 0.0577(10) Uani 1 1 d . . .
H1A H -0.1538 0.1894 -0.0124 0.086 Uiso 1 1 calc R . .
H1B H -0.1537 0.2413 0.0750 0.086 Uiso 1 1 calc R . .
H1C H -0.1015 0.1730 0.1267 0.086 Uiso 1 1 calc R . .
C2 C -0.00862(18) 0.23181(14) 0.0999(2) 0.0354(6) Uani 1 1 d . . .
H2A H 0.0311 0.2496 0.1825 0.042 Uiso 1 1 calc R . .
H2B H -0.0216 0.2668 0.0438 0.042 Uiso 1 1 calc R . .
C3 C 0.05912(16) 0.18056(12) 0.0923(2) 0.0254(5) Uani 1 1 d . . .
H3A H 0.0683 0.1440 0.1438 0.031 Uiso 1 1 calc R . .
H3B H 0.0228 0.1652 0.0082 0.031 Uiso 1 1 calc R . .
C4 C 0.16668(16) 0.20737(11) 0.13317(19) 0.0212(5) Uani 1 1 d . . .
H4A H 0.1567 0.2504 0.0983 0.025 Uiso 1 1 calc R . .
H4B H 0.2092 0.2120 0.2219 0.025 Uiso 1 1 calc R . .
C5 C 0.20937(15) 0.17430(10) -0.00862(18) 0.0164(4) Uani 1 1 d . . .
C10 C 0.54817(15) 0.08965(10) 0.09671(18) 0.0169(4) Uani 1 1 d . . .
C11 C 0.71566(16) 0.05644(12) 0.12607(19) 0.0248(5) Uani 1 1 d . . .
H11A H 0.7310 0.0226 0.1851 0.030 Uiso 1 1 calc R . .
H11B H 0.7550 0.0951 0.1710 0.030 Uiso 1 1 calc R . .
C12 C 0.75048(16) 0.03529(11) 0.04574(19) 0.0226(5) Uani 1 1 d . . .
H12A H 0.7360 0.0697 -0.0121 0.027 Uiso 1 1 calc R . .
H12B H 0.7089 -0.0024 -0.0010 0.027 Uiso 1 1 calc R . .
C13 C 0.86761(17) 0.01881(13) 0.1176(2) 0.0293(6) Uani 1 1 d . . .
H13A H 0.9090 0.0561 0.1665 0.035 Uiso 1 1 calc R . .
H13B H 0.8816 -0.0165 0.1735 0.035 Uiso 1 1 calc R . .
C14 C 0.9038(2) -0.00037(14) 0.0374(2) 0.0382(7) Uani 1 1 d . . .
H14A H 0.8623 -0.0369 -0.0122 0.057 Uiso 1 1 calc R . .
H14B H 0.9786 -0.0120 0.0874 0.057 Uiso 1 1 calc R . .
H14C H 0.8939 0.0353 -0.0150 0.057 Uiso 1 1 calc R . .
N1 N 0.22606(13) 0.16895(9) 0.09993(15) 0.0178(4) Uani 1 1 d . . .
H1 H 0.2736 0.1419 0.1523 0.021 Uiso 1 1 calc R . .
N3 N 0.60209(13) 0.06993(10) 0.05228(16) 0.0240(4) Uani 1 1 d . . .
H3 H 0.5677 0.0646 -0.0261 0.029 Uiso 1 1 calc R . .
O1 O 0.13456(10) 0.20612(7) -0.09104(12) 0.0207(3) Uani 1 1 d . . .
O2 O 0.59168(10) 0.09561(7) 0.20863(12) 0.0179(3) Uani 1 1 d . . .
O3 O 0.44266(12) 0.22805(8) 0.30328(14) 0.0205(3) Uani 1 1 d . . .
H98 H 0.502(2) 0.2499(14) 0.355(2) 0.041 Uiso 1 1 d . . .
H99 H 0.405(2) 0.2524(14) 0.238(3) 0.041 Uiso 1 1 d . . .
C6 C 0.28587(15) 0.14286(10) -0.02669(17) 0.0150(4) Uani 1 1 d . . .
C7 C 0.27031(15) 0.12475(10) -0.13610(18) 0.0183(5) Uani 1 1 d . . .
C8 C 0.36583(16) 0.10183(11) -0.11021(18) 0.0189(5) Uani 1 1 d . . .
C9 C 0.43671(15) 0.10582(10) 0.01505(17) 0.0168(4) Uani 1 1 d . . .
N2 N 0.38768(12) 0.13101(8) 0.06520(14) 0.0153(4) Uani 1 1 d . . .
Cl1 Cl 0.15577(4) 0.12719(3) -0.27848(4) 0.02749(15) Uani 1 1 d . . .
Cl2 Cl 0.38946(4) 0.07455(3) -0.21398(5) 0.02913(16) Uani 1 1 d . . .
Co1 Co 0.5000 0.149895(19) 0.2500 0.01458(12) Uani 1 2 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0262(14) 0.099(3) 0.0488(18) -0.0184(18) 0.0218(14) 0.0013(15)
C2 0.0290(13) 0.0516(18) 0.0306(13) 0.0024(12) 0.0198(12) 0.0079(12)
C3 0.0189(11) 0.0354(15) 0.0229(11) 0.0031(10) 0.0122(10) 0.0014(10)
C4 0.0208(11) 0.0243(13) 0.0189(11) -0.0021(9) 0.0114(9) 0.0000(9)
C5 0.0142(10) 0.0152(11) 0.0155(10) -0.0024(8) 0.0058(9) -0.0029(8)
C10 0.0160(10) 0.0168(12) 0.0175(10) -0.0023(8) 0.0091(9) -0.0016(8)
C11 0.0149(10) 0.0358(15) 0.0217(11) -0.0024(10) 0.0092(9) 0.0034(9)
C12 0.0184(11) 0.0273(13) 0.0220(11) 0.0001(9) 0.0113(10) 0.0028(9)
C13 0.0226(12) 0.0388(16) 0.0310(13) 0.0058(11) 0.0178(11) 0.0064(10)
C14 0.0319(13) 0.0509(19) 0.0453(16) 0.0090(13) 0.0299(13) 0.0121(12)
N1 0.0131(8) 0.0226(10) 0.0150(8) 0.0018(7) 0.0062(7) 0.0037(7)
N3 0.0158(9) 0.0377(12) 0.0161(9) -0.0051(8) 0.0074(8) 0.0024(8)
O1 0.0160(7) 0.0229(9) 0.0177(7) 0.0039(6) 0.0060(6) 0.0051(6)
O2 0.0154(7) 0.0206(8) 0.0147(7) -0.0018(6) 0.0066(6) 0.0019(6)
O3 0.0182(8) 0.0207(9) 0.0188(8) 0.0005(6) 0.0082(7) -0.0001(6)
C6 0.0118(9) 0.0160(11) 0.0134(9) 0.0007(8) 0.0047(8) 0.0000(8)
C7 0.0155(10) 0.0191(12) 0.0125(9) 0.0009(8) 0.0031(9) 0.0020(8)
C8 0.0211(11) 0.0206(12) 0.0148(10) -0.0018(8) 0.0100(9) 0.0010(9)
C9 0.0179(10) 0.0174(11) 0.0149(10) -0.0006(8) 0.0091(9) 0.0006(8)
N2 0.0149(8) 0.0159(9) 0.0149(8) -0.0010(7) 0.0081(7) -0.0005(7)
Cl1 0.0230(3) 0.0324(3) 0.0129(3) -0.0024(2) 0.0014(2) 0.0071(2)
Cl2 0.0291(3) 0.0416(4) 0.0165(3) -0.0042(2) 0.0126(2) 0.0066(3)
Co1 0.01199(19) 0.0182(2) 0.01128(19) 0.000 0.00514(16) 0.000

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.516(4) . ?
C2 C3 1.538(3) . ?
C3 C4 1.522(3) . ?
C4 N1 1.460(3) . ?
C5 O1 1.249(2) . ?
C5 N1 1.334(3) . ?
C5 C6 1.478(3) . ?
C10 O2 1.261(2) . ?
C10 N3 1.326(3) . ?
C10 C9 1.460(3) . ?
C11 N3 1.467(3) . ?
C11 C12 1.512(3) . ?
C12 C13 1.525(3) . ?
C13 C14 1.515(3) . ?
O2 Co1 2.1104(14) . ?
O3 Co1 2.1646(16) . ?
C6 N2 1.362(2) . ?
C6 C7 1.401(3) . ?
C7 C8 1.386(3) . ?
C7 Cl1 1.7225(19) . ?
C8 C9 1.400(3) . ?
C8 Cl2 1.721(2) . ?
C9 N2 1.365(3) . ?
N2 Co1 2.1155(16) . ?
Co1 O2 2.1104(14) 2_655 ?
Co1 N2 2.1155(16) 2_655 ?
Co1 O3 2.1646(16) 2_655 ?

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
C1 C2 C3 113.0(2) . . ?
C4 C3 C2 110.5(2) . . ?
N1 C4 C3 114.70(18) . . ?
O1 C5 N1 121.99(19) . . ?
O1 C5 C6 120.80(18) . . ?
N1 C5 C6 117.16(18) . . ?
O2 C10 N3 121.27(18) . . ?
O2 C10 C9 118.98(18) . . ?
N3 C10 C9 119.74(18) . . ?
N3 C11 C12 109.53(17) . . ?
C11 C12 C13 112.10(18) . . ?
C14 C13 C12 112.4(2) . . ?
C5 N1 C4 121.03(18) . . ?
C10 N3 C11 123.92(18) . . ?
C10 O2 Co1 112.41(12) . . ?
N2 C6 C7 109.51(18) . . ?
N2 C6 C5 122.91(18) . . ?
C7 C6 C5 127.46(18) . . ?
C8 C7 C6 107.24(17) . . ?
C8 C7 Cl1 124.27(16) . . ?
C6 C7 Cl1 128.48(16) . . ?
C7 C8 C9 106.18(18) . . ?
C7 C8 Cl2 125.74(15) . . ?
C9 C8 Cl2 128.08(16) . . ?
N2 C9 C8 110.10(17) . . ?
N2 C9 C10 117.09(17) . . ?
C8 C9 C10 132.79(19) . . ?
C6 N2 C9 106.97(16) . . ?
C6 N2 Co1 142.30(14) . . ?
C9 N2 Co1 109.85(12) . . ?
O2 Co1 O2 114.51(8) 2_655 . ?
O2 Co1 N2 89.01(6) 2_655 . ?
O2 Co1 N2 79.29(6) . . ?
O2 Co1 N2 79.29(6) 2_655 2_655 ?
O2 Co1 N2 89.01(6) . 2_655 ?
N2 Co1 N2 158.36(10) . 2_655 ?
O2 Co1 O3 82.61(6) 2_655 . ?
O2 Co1 O3 161.81(6) . . ?
N2 Co1 O3 108.39(6) . . ?
N2 Co1 O3 88.26(6) 2_655 . ?
O2 Co1 O3 161.81(6) 2_655 2_655 ?
O2 Co1 O3 82.61(6) . 2_655 ?
N2 Co1 O3 88.26(6) . 2_655 ?
N2 Co1 O3 108.39(6) 2_655 2_655 ?
O3 Co1 O3 81.20(8) . 2_655 ?

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
N1 H1 O2 0.88 2.09 2.953(2) 167.1 2_655
N3 H3 Cl2 0.88 2.47 3.2119(18) 141.7 .
O3 H98 O1 0.90(3) 1.97(3) 2.808(2) 156(2) 8_556
O3 H99 O1 0.89(3) 1.92(3) 2.764(2) 158(2) 7
O3 H99 Cl1 0.89(3) 2.85(3) 3.3297(17) 115(2) 7

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.079

#===END

data_2007sot0773
_database_code_depnum_ccdc_archive 'CCDC 678037'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C62 H48 Co2 N10 O6'
_chemical_formula_weight         1146.96

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   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                   13.8197(5)
_cell_length_b                   24.1188(10)
_cell_length_c                   19.9231(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.468(2)
_cell_angle_gamma                90.00
_cell_volume                     6334.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    125639
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       Plate
_exptl_crystal_colour            'Pale Brown'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2368
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8931
_exptl_absorpt_correction_T_max  0.9885
_exptl_absorpt_process_details   
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;

_exptl_special_details           
;
SADABS was used to perform the Absorption correction
Parameter refinement on 25421 reflections reduced R(int) from 0.1221 to 0.0693
Ratio of minimum to maximum apparent transmission: 0.805162
The given Tmin and Tmax were generated using the SHELX SIZE command

The methoxy group is disordered over two possible sites (70:30) in the
molecule.
The modelling of this is somewhat hampered by one of the potential
sites being on the edge of a channel which is most likely filled with
disordered solvent.
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans to fill the asymmetric unit'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34159
_diffrn_reflns_av_R_equivalents  0.0851
_diffrn_reflns_av_sigmaI/netI    0.0687
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.97
_diffrn_reflns_theta_max         25.03
_reflns_number_total             5610
_reflns_number_gt                3807
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin, et al., 1993)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1549P)^2^+57.7576P] where P=(Fo^2^+2Fc^2^)/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         5610
_refine_ls_number_parameters     364
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1544
_refine_ls_R_factor_gt           0.1147
_refine_ls_wR_factor_ref         0.3124
_refine_ls_wR_factor_gt          0.2865
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.010
_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
C12 C 0.5751(6) 0.0929(4) 0.1878(4) 0.0497(19) Uani 1 1 d . A .
C14 C 0.7046(6) 0.1015(4) 0.3766(4) 0.0491(19) Uani 1 1 d . . .
C15 C 0.7516(7) 0.0747(4) 0.4406(4) 0.065(2) Uani 1 1 d . A .
H15 H 0.7570 0.0354 0.4430 0.078 Uiso 1 1 calc R . .
C16 C 0.7896(7) 0.1067(5) 0.4998(4) 0.068(3) Uani 1 1 d . . .
H16 H 0.8229 0.0899 0.5438 0.082 Uiso 1 1 calc R A .
C17 C 0.7789(6) 0.1628(5) 0.4946(4) 0.067(3) Uani 1 1 d . A .
H17 H 0.8034 0.1850 0.5356 0.080 Uiso 1 1 calc R . .
C18 C 0.7323(5) 0.1881(4) 0.4298(4) 0.056(2) Uani 1 1 d . . .
H18 H 0.7268 0.2273 0.4265 0.067 Uiso 1 1 calc R A .
N4 N 0.6121(4) 0.1071(3) 0.2565(3) 0.0477(16) Uani 1 1 d . . .
N5 N 0.6949(4) 0.1561(3) 0.3716(3) 0.0478(16) Uani 1 1 d . . .
O2 O 0.5777(5) 0.0459(3) 0.1628(3) 0.0662(16) Uani 1 1 d . . .
C6A C 0.3194(6) 0.2952(4) 0.2226(4) 0.054(2) Uani 0.697(7) 1 d P A 1
H6A H 0.3579 0.3257 0.2531 0.065 Uiso 0.697(7) 1 calc PR A 1
O3A O 0.2424(5) 0.3162(3) 0.1612(4) 0.0496(14) Uani 0.697(7) 1 d PD A 1
C31A C 0.2249(8) 0.3743(4) 0.1646(5) 0.0496(14) Uani 0.697(7) 1 d PD A 1
H31A H 0.2012 0.3822 0.2053 0.074 Uiso 0.697(7) 1 calc PR A 1
H31B H 0.1735 0.3862 0.1215 0.074 Uiso 0.697(7) 1 calc PR A 1
H31C H 0.2883 0.3945 0.1695 0.074 Uiso 0.697(7) 1 calc PR A 1
C6B C 0.3194(6) 0.2952(4) 0.2226(4) 0.054(2) Uani 0.303(7) 1 d P A 2
H6B1 H 0.2701 0.3134 0.1819 0.065 Uiso 0.303(7) 1 calc PR A 2
H6B2 H 0.3593 0.3242 0.2542 0.065 Uiso 0.303(7) 1 calc PR A 2
C13A C 0.6648(6) 0.0683(5) 0.3093(4) 0.074(3) Uani 0.303(7) 1 d PD A 3
H13A H 0.6204 0.0369 0.3145 0.089 Uiso 0.303(7) 1 calc PR A 3
O3B O 0.7558(12) 0.0491(6) 0.2929(8) 0.0496(14) Uani 0.303(7) 1 d PD A 3
C31B C 0.7591(16) -0.0097(7) 0.2777(12) 0.0496(14) Uani 0.303(7) 1 d PD A 3
H31D H 0.8134 -0.0275 0.3148 0.074 Uiso 0.303(7) 1 calc PR A 3
H31E H 0.7721 -0.0145 0.2323 0.074 Uiso 0.303(7) 1 calc PR A 3
H31F H 0.6939 -0.0268 0.2757 0.074 Uiso 0.303(7) 1 calc PR A 3
C13B C 0.6648(6) 0.0683(5) 0.3093(4) 0.074(3) Uani 0.697(7) 1 d P A 4
H13B H 0.7215 0.0509 0.2962 0.089 Uiso 0.697(7) 1 calc PR A 4
H13C H 0.6182 0.0388 0.3152 0.089 Uiso 0.697(7) 1 calc PR A 4
C1 C 0.2255(6) 0.1692(4) 0.2864(4) 0.063(2) Uani 1 1 d . . .
H1 H 0.2339 0.1302 0.2836 0.076 Uiso 1 1 calc R . .
C2 C 0.1579(6) 0.1900(5) 0.3201(5) 0.072(3) Uani 1 1 d . . .
H2 H 0.1185 0.1651 0.3382 0.087 Uiso 1 1 calc R . .
C3 C 0.1483(7) 0.2462(5) 0.3272(5) 0.079(3) Uani 1 1 d . . .
H3 H 0.1055 0.2609 0.3523 0.094 Uiso 1 1 calc R . .
C4 C 0.2024(7) 0.2799(4) 0.2971(5) 0.067(2) Uani 1 1 d . A .
H4 H 0.1966 0.3190 0.3007 0.080 Uiso 1 1 calc R . .
C5 C 0.2660(6) 0.2583(4) 0.2611(4) 0.057(2) Uani 1 1 d . . .
C7 C 0.4474(6) 0.2796(4) 0.1649(4) 0.0489(19) Uani 1 1 d . A .
C8 C 0.5007(5) 0.2332(3) 0.1429(3) 0.0443(18) Uani 1 1 d . . .
C9 C 0.5206(5) 0.2206(3) 0.0812(4) 0.0444(18) Uani 1 1 d . . .
C10 C 0.5428(5) 0.1620(4) 0.0827(3) 0.051(2) Uani 1 1 d . A .
C11 C 0.5359(5) 0.1427(3) 0.1463(4) 0.0447(18) Uani 1 1 d . . .
C19 C 0.5107(5) 0.2577(4) 0.0209(4) 0.0495(19) Uani 1 1 d . . .
C20 C 0.5485(6) 0.3112(4) 0.0316(4) 0.059(2) Uani 1 1 d . . .
H20 H 0.5853 0.3230 0.0777 0.071 Uiso 1 1 calc R . .
C21 C 0.5332(7) 0.3479(5) -0.0243(5) 0.071(3) Uani 1 1 d . . .
H21 H 0.5603 0.3844 -0.0165 0.086 Uiso 1 1 calc R . .
C22 C 0.4780(7) 0.3312(5) -0.0919(5) 0.069(3) Uani 1 1 d . . .
H22 H 0.4654 0.3565 -0.1302 0.083 Uiso 1 1 calc R . .
C23 C 0.4429(6) 0.2789(5) -0.1026(4) 0.069(3) Uani 1 1 d . . .
H23 H 0.4073 0.2673 -0.1490 0.082 Uiso 1 1 calc R . .
C24 C 0.4572(5) 0.2418(4) -0.0482(4) 0.053(2) Uani 1 1 d . . .
H24 H 0.4308 0.2053 -0.0572 0.063 Uiso 1 1 calc R . .
C25 C 0.5722(6) 0.1309(4) 0.0280(3) 0.0498(19) Uani 1 1 d . . .
C26 C 0.6514(6) 0.1508(4) 0.0046(4) 0.058(2) Uani 1 1 d . A .
H26 H 0.6872 0.1831 0.0255 0.069 Uiso 1 1 calc R . .
C27 C 0.6783(7) 0.1241(5) -0.0483(4) 0.070(3) Uani 1 1 d . . .
H27 H 0.7323 0.1377 -0.0639 0.084 Uiso 1 1 calc R A .
C28 C 0.6250(8) 0.0768(5) -0.0787(5) 0.076(3) Uani 1 1 d . A .
H28 H 0.6434 0.0579 -0.1148 0.092 Uiso 1 1 calc R . .
C30 C 0.5204(7) 0.0849(4) -0.0027(4) 0.062(2) Uani 1 1 d . A .
H30 H 0.4662 0.0713 0.0129 0.074 Uiso 1 1 calc R . .
C39 C 0.5456(8) 0.0574(4) -0.0567(4) 0.074(3) Uani 1 1 d . . .
H39 H 0.5086 0.0255 -0.0781 0.089 Uiso 1 1 calc R A .
N1 N 0.2788(5) 0.2036(3) 0.2576(3) 0.0503(16) Uani 1 1 d . A .
N2 N 0.3848(4) 0.2583(3) 0.1996(3) 0.0513(17) Uani 1 1 d . . .
N3 N 0.5097(4) 0.1854(3) 0.1848(3) 0.0403(14) Uani 1 1 d . . .
O1 O 0.4544(4) 0.3284(3) 0.1502(3) 0.0581(15) Uani 1 1 d . . .
Co1 Co 0.38901(7) 0.18274(5) 0.22006(5) 0.0449(4) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C12 0.047(4) 0.064(5) 0.039(4) -0.011(4) 0.013(3) -0.007(4)
C14 0.042(4) 0.068(6) 0.037(4) 0.003(4) 0.010(3) 0.002(4)
C15 0.064(5) 0.075(6) 0.050(5) 0.003(5) 0.008(4) -0.002(5)
C16 0.059(5) 0.092(8) 0.042(5) 0.012(5) -0.001(4) 0.008(5)
C17 0.047(5) 0.117(9) 0.031(4) -0.006(5) 0.003(3) -0.003(5)
C18 0.034(4) 0.096(7) 0.037(4) -0.001(4) 0.009(3) -0.010(4)
N4 0.035(3) 0.080(5) 0.030(3) -0.002(3) 0.013(2) -0.003(3)
N5 0.036(3) 0.076(5) 0.030(3) 0.001(3) 0.009(2) -0.009(3)
O2 0.077(4) 0.074(4) 0.041(3) -0.008(3) 0.008(3) -0.002(3)
C6A 0.044(4) 0.081(6) 0.040(4) 0.000(4) 0.014(3) 0.007(4)
O3A 0.043(3) 0.065(3) 0.038(3) 0.010(3) 0.007(2) 0.022(3)
C31A 0.043(3) 0.065(3) 0.038(3) 0.010(3) 0.007(2) 0.022(3)
C6B 0.044(4) 0.081(6) 0.040(4) 0.000(4) 0.014(3) 0.007(4)
C13A 0.042(4) 0.145(10) 0.029(4) 0.010(5) 0.002(3) -0.002(5)
O3B 0.043(3) 0.065(3) 0.038(3) 0.010(3) 0.007(2) 0.022(3)
C31B 0.043(3) 0.065(3) 0.038(3) 0.010(3) 0.007(2) 0.022(3)
C13B 0.042(4) 0.145(10) 0.029(4) 0.010(5) 0.002(3) -0.002(5)
C1 0.047(4) 0.100(7) 0.043(4) 0.014(5) 0.012(4) 0.000(4)
C2 0.048(5) 0.122(9) 0.058(5) 0.010(6) 0.032(4) 0.005(5)
C3 0.066(6) 0.113(9) 0.073(6) -0.005(6) 0.045(5) 0.009(6)
C4 0.068(5) 0.087(7) 0.058(5) 0.004(5) 0.035(5) 0.013(5)
C5 0.046(4) 0.088(7) 0.038(4) 0.002(4) 0.014(3) 0.017(4)
C7 0.053(4) 0.057(5) 0.032(4) -0.005(4) 0.005(3) -0.001(4)
C8 0.037(4) 0.066(5) 0.029(3) -0.002(3) 0.009(3) -0.001(3)
C9 0.036(4) 0.066(5) 0.032(4) -0.006(3) 0.011(3) -0.007(3)
C10 0.036(4) 0.092(6) 0.023(3) -0.008(4) 0.007(3) -0.009(4)
C11 0.032(3) 0.069(5) 0.033(4) -0.003(4) 0.009(3) -0.003(3)
C19 0.038(4) 0.075(6) 0.039(4) 0.005(4) 0.017(3) 0.005(4)
C20 0.055(5) 0.080(6) 0.049(5) 0.015(4) 0.025(4) 0.008(5)
C21 0.062(5) 0.091(7) 0.075(6) 0.022(6) 0.042(5) 0.004(5)
C22 0.050(5) 0.118(9) 0.045(5) 0.029(5) 0.023(4) 0.020(5)
C23 0.045(5) 0.125(9) 0.042(5) 0.017(5) 0.020(4) 0.014(5)
C24 0.039(4) 0.092(6) 0.032(4) 0.003(4) 0.019(3) 0.008(4)
C25 0.045(4) 0.079(6) 0.025(3) -0.005(4) 0.010(3) -0.003(4)
C26 0.054(5) 0.088(6) 0.035(4) 0.000(4) 0.020(4) -0.002(4)
C27 0.071(6) 0.102(8) 0.047(5) 0.001(5) 0.034(4) 0.015(6)
C28 0.089(7) 0.096(8) 0.050(5) 0.003(5) 0.029(5) 0.025(6)
C30 0.067(5) 0.084(6) 0.031(4) 0.003(4) 0.009(4) -0.007(5)
C39 0.095(7) 0.083(7) 0.041(5) -0.009(5) 0.016(5) -0.006(6)
N1 0.041(3) 0.081(5) 0.030(3) 0.005(3) 0.011(3) 0.004(3)
N2 0.036(3) 0.093(5) 0.027(3) -0.001(3) 0.014(3) 0.004(3)
N3 0.035(3) 0.058(4) 0.032(3) -0.004(3) 0.016(2) -0.002(3)
O1 0.058(3) 0.074(4) 0.042(3) -0.002(3) 0.014(3) -0.003(3)
Co1 0.0363(5) 0.0719(8) 0.0276(5) 0.0013(5) 0.0112(4) 0.0018(5)

_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
C12 O2 1.244(10) . ?
C12 N4 1.352(9) . ?
C12 C11 1.466(11) . ?
C14 N5 1.323(10) . ?
C14 C15 1.403(11) . ?
C14 C13A 1.516(12) . ?
C15 C16 1.375(13) . ?
C16 C17 1.361(14) . ?
C17 C18 1.398(12) . ?
C18 N5 1.360(10) . ?
N4 C13A 1.433(11) . ?
N4 Co1 1.884(7) 2_655 ?
N5 Co1 1.955(6) 2_655 ?
C6A N2 1.438(10) . ?
C6A O3A 1.450(10) . ?
C6A C5 1.506(12) . ?
O3A C31A 1.427(8) . ?
C13A O3B 1.466(17) . ?
O3B C31B 1.454(10) . ?
C1 N1 1.345(11) . ?
C1 C2 1.397(12) . ?
C2 C3 1.374(15) . ?
C3 C4 1.360(14) . ?
C4 C5 1.392(11) . ?
C5 N1 1.337(11) . ?
C7 O1 1.224(10) . ?
C7 N2 1.359(10) . ?
C7 C8 1.477(11) . ?
C8 C9 1.372(10) . ?
C8 N3 1.407(10) . ?
C9 C10 1.442(12) . ?
C9 C19 1.473(11) . ?
C10 C11 1.379(10) . ?
C10 C25 1.479(10) . ?
C11 N3 1.397(9) . ?
C19 C20 1.385(12) . ?
C19 C24 1.405(11) . ?
C20 C21 1.388(12) . ?
C21 C22 1.394(14) . ?
C22 C23 1.344(14) . ?
C23 C24 1.374(12) . ?
C25 C30 1.362(12) . ?
C25 C26 1.397(11) . ?
C26 C27 1.378(12) . ?
C27 C28 1.392(14) . ?
C28 C39 1.380(14) . ?
C30 C39 1.395(13) . ?
N1 Co1 1.953(6) . ?
N2 Co1 1.865(8) . ?
N3 Co1 1.990(6) 2_655 ?
N3 Co1 1.996(5) . ?
Co1 N4 1.884(7) 2_655 ?
Co1 N5 1.955(6) 2_655 ?
Co1 N3 1.990(6) 2_655 ?
Co1 Co1 2.9387(18) 2_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C12 N4 126.1(8) . . ?
O2 C12 C11 124.7(7) . . ?
N4 C12 C11 109.1(7) . . ?
N5 C14 C15 122.4(8) . . ?
N5 C14 C13A 117.2(7) . . ?
C15 C14 C13A 120.4(8) . . ?
C16 C15 C14 118.3(9) . . ?
C17 C16 C15 119.2(8) . . ?
C16 C17 C18 120.9(9) . . ?
N5 C18 C17 119.5(9) . . ?
C12 N4 C13A 122.1(7) . . ?
C12 N4 Co1 117.9(6) . 2_655 ?
C13A N4 Co1 119.3(5) . 2_655 ?
C14 N5 C18 119.8(7) . . ?
C14 N5 Co1 114.6(5) . 2_655 ?
C18 N5 Co1 125.2(6) . 2_655 ?
N2 C6A O3A 108.7(6) . . ?
N2 C6A C5 104.4(7) . . ?
O3A C6A C5 106.8(6) . . ?
C31A O3A C6A 113.2(7) . . ?
N4 C13A O3B 108.9(8) . . ?
N4 C13A C14 105.9(8) . . ?
O3B C13A C14 104.8(8) . . ?
C31B O3B C13A 116.0(12) . . ?
N1 C1 C2 120.9(10) . . ?
C3 C2 C1 120.2(9) . . ?
C4 C3 C2 117.5(9) . . ?
C3 C4 C5 121.2(10) . . ?
N1 C5 C4 120.7(8) . . ?
N1 C5 C6A 117.7(7) . . ?
C4 C5 C6A 121.6(9) . . ?
O1 C7 N2 126.4(8) . . ?
O1 C7 C8 125.2(7) . . ?
N2 C7 C8 108.3(7) . . ?
C9 C8 N3 110.1(7) . . ?
C9 C8 C7 133.3(7) . . ?
N3 C8 C7 114.1(6) . . ?
C8 C9 C10 107.3(7) . . ?
C8 C9 C19 127.0(7) . . ?
C10 C9 C19 125.5(6) . . ?
C11 C10 C9 106.2(7) . . ?
C11 C10 C25 127.9(8) . . ?
C9 C10 C25 125.8(7) . . ?
C10 C11 N3 110.8(7) . . ?
C10 C11 C12 132.9(7) . . ?
N3 C11 C12 114.0(6) . . ?
C20 C19 C24 118.0(8) . . ?
C20 C19 C9 120.2(7) . . ?
C24 C19 C9 121.7(8) . . ?
C19 C20 C21 120.7(9) . . ?
C20 C21 C22 119.9(10) . . ?
C23 C22 C21 119.4(9) . . ?
C22 C23 C24 121.8(9) . . ?
C23 C24 C19 120.2(9) . . ?
C30 C25 C26 119.3(7) . . ?
C30 C25 C10 121.4(7) . . ?
C26 C25 C10 119.2(7) . . ?
C27 C26 C25 120.8(9) . . ?
C26 C27 C28 119.1(9) . . ?
C39 C28 C27 120.5(9) . . ?
C25 C30 C39 120.9(9) . . ?
C28 C39 C30 119.3(10) . . ?
C5 N1 C1 119.2(7) . . ?
C5 N1 Co1 113.9(5) . . ?
C1 N1 Co1 126.4(7) . . ?
C7 N2 C6A 119.0(7) . . ?
C7 N2 Co1 119.9(5) . . ?
C6A N2 Co1 121.1(5) . . ?
C11 N3 C8 105.7(5) . . ?
C11 N3 Co1 106.0(4) . 2_655 ?
C8 N3 Co1 120.2(4) . 2_655 ?
C11 N3 Co1 123.5(5) . . ?
C8 N3 Co1 107.5(4) . . ?
Co1 N3 Co1 95.0(2) 2_655 . ?
N2 Co1 N4 176.8(2) . 2_655 ?
N2 Co1 N1 81.7(3) . . ?
N4 Co1 N1 95.1(3) 2_655 . ?
N2 Co1 N5 98.4(3) . 2_655 ?
N4 Co1 N5 82.3(3) 2_655 2_655 ?
N1 Co1 N5 97.5(2) . 2_655 ?
N2 Co1 N3 98.3(3) . 2_655 ?
N4 Co1 N3 81.4(2) 2_655 2_655 ?
N1 Co1 N3 91.9(2) . 2_655 ?
N5 Co1 N3 161.9(3) 2_655 2_655 ?
N2 Co1 N3 82.3(2) . . ?
N4 Co1 N3 100.9(2) 2_655 . ?
N1 Co1 N3 163.1(3) . . ?
N5 Co1 N3 90.3(2) 2_655 . ?
N3 Co1 N3 84.9(2) 2_655 . ?
N2 Co1 Co1 92.80(18) . 2_655 ?
N4 Co1 Co1 89.10(17) 2_655 2_655 ?
N1 Co1 Co1 133.10(18) . 2_655 ?
N5 Co1 Co1 129.29(18) 2_655 2_655 ?
N3 Co1 Co1 42.58(15) 2_655 2_655 ?
N3 Co1 Co1 42.43(16) . 2_655 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.661
_refine_diff_density_min         -0.968
_refine_diff_density_rms         0.113

#===END