# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Hong-Cai Zhou' loop_ _publ_author_name J.Park J.-R.Li E.C.Sanudo D.Yuan H.-C.Zhou data_PCN-121 _database_code_depnum_ccdc_archive 'CCDC 813603' #TrackingRef '4307_web_deposit_cif_file_0_JinheePark_1297901619.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H26 Co3 N2 O12' _chemical_formula_sum 'C30 H26 Co3 N2 O12' _chemical_formula_weight 783.32 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 hexagonal _symmetry_space_group_name_H-M P61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/6' '-y, x-y, z+1/3' '-x, -y, z+1/2' '-x+y, -x, z+2/3' 'y, -x+y, z+5/6' _cell_length_a 24.65(2) _cell_length_b 24.65(2) _cell_length_c 19.730(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10384(16) _cell_formula_units_Z 6 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9113 _cell_measurement_theta_min 2.2705 _cell_measurement_theta_max 27.6885 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.752 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2382 _exptl_absorpt_coefficient_mu 0.741 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7560 _exptl_absorpt_correction_T_max 0.8083 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 125711 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 28.02 _reflns_number_total 16690 _reflns_number_gt 15571 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0291P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(5) _refine_ls_number_reflns 16690 _refine_ls_number_parameters 427 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0229 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0500 _refine_ls_wR_factor_gt 0.0495 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.039 0.717 0.021 6708 1437 ' ' _platon_squeeze_details ; ; 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 0.196352(7) 0.160060(7) 0.945292(8) 0.01582(3) Uani 1 1 d . . . Co2 Co 0.213978(7) 0.109322(7) 0.788563(8) 0.01688(4) Uani 1 1 d . . . Co3 Co 0.332072(7) 0.243428(7) 0.885045(8) 0.01869(4) Uani 1 1 d . . . O1 O 0.25434(3) 0.15796(3) 0.87331(3) 0.00763(13) Uani 1 1 d . . . H1A H 0.2561 0.1273 0.8908 0.011 Uiso 1 1 d R . . O2 O 0.38360(4) 0.20919(4) 0.83305(5) 0.0343(2) Uani 1 1 d . . . H2E H 0.3672 0.1818 0.8019 0.051 Uiso 1 1 d R . . H2F H 0.4177 0.2110 0.8446 0.051 Uiso 1 1 d R . . O3 O 0.13724(4) 0.12136(4) 0.78994(4) 0.02380(18) Uani 1 1 d . . . O4 O 0.13493(4) 0.17355(4) 0.88108(4) 0.01857(17) Uani 1 1 d . . . O5 O 0.13760(4) 0.16536(4) 1.01670(4) 0.01794(16) Uani 1 1 d . . . O6 O 0.07167(4) 0.13825(4) 1.10415(4) 0.02200(18) Uani 1 1 d . . . O7 O 0.29355(4) 0.09825(4) 0.77971(5) 0.02475(18) Uani 1 1 d . . . O8 O 0.25721(4) -0.00366(4) 0.76763(4) 0.02098(18) Uani 1 1 d . . . O9 O 0.34860(4) 0.21496(4) 0.97573(5) 0.0265(2) Uani 1 1 d . . . O10 O 0.25208(4) 0.15289(4) 1.01775(4) 0.02319(19) Uani 1 1 d . . . O11 O 0.27315(4) -0.04269(4) 1.62857(4) 0.0263(2) Uani 1 1 d . . . O12 O 0.18849(4) -0.07423(4) 1.56234(4) 0.0273(2) Uani 1 1 d . . . N1 N 0.38367(6) 0.07673(8) 1.28852(7) 0.0533(4) Uani 1 1 d . . . N2 N 0.66987(5) 0.08257(5) 1.23747(6) 0.0267(2) Uani 1 1 d . . . C1 C 0.11323(6) 0.14592(6) 0.82482(7) 0.0239(3) Uani 1 1 d . . . C2 C 0.05293(8) 0.14034(10) 0.80018(9) 0.0514(5) Uani 1 1 d . . . H2A H 0.0178 0.0994 0.8133 0.077 Uiso 1 1 calc R . . H2B H 0.0542 0.1444 0.7507 0.077 Uiso 1 1 calc R . . H2C H 0.0475 0.1736 0.8205 0.077 Uiso 1 1 calc R . . C3 C 0.11060(6) 0.13266(6) 1.06917(6) 0.0195(2) Uani 1 1 d . . . C4 C 0.12492(9) 0.08253(8) 1.09147(8) 0.0446(4) Uani 1 1 d . . . H4A H 0.0927 0.0418 1.0739 0.067 Uiso 1 1 calc R . . H4B H 0.1254 0.0811 1.1411 0.067 Uiso 1 1 calc R . . H4C H 0.1660 0.0922 1.0738 0.067 Uiso 1 1 calc R . . C5 C 0.30056(6) 0.05248(6) 0.76758(6) 0.0246(3) Uani 1 1 d . . . C6 C 0.36605(7) 0.06553(8) 0.75052(10) 0.0453(4) Uani 1 1 d . . . H6A H 0.3952 0.1108 0.7513 0.068 Uiso 1 1 calc R . . H6B H 0.3660 0.0491 0.7053 0.068 Uiso 1 1 calc R . . H6C H 0.3793 0.0451 0.7840 0.068 Uiso 1 1 calc R . . C7 C 0.31011(6) 0.17704(6) 1.01866(6) 0.0234(3) Uani 1 1 d . . . C8 C 0.33866(7) 0.15984(7) 1.07620(7) 0.0316(3) Uani 1 1 d . . . C9 C 0.40239(8) 0.18689(10) 1.08228(9) 0.0575(5) Uani 1 1 d . . . H9 H 0.4290 0.2184 1.0511 0.069 Uiso 1 1 calc R . . C10 C 0.42804(8) 0.16886(12) 1.13297(10) 0.0781(8) Uani 1 1 d . . . H10 H 0.4723 0.1886 1.1370 0.094 Uiso 1 1 calc R . . C11 C 0.39041(7) 0.12219(10) 1.17844(9) 0.0517(5) Uani 1 1 d . . . C12 C 0.32646(7) 0.09637(10) 1.17402(9) 0.0497(5) Uani 1 1 d . . . H12 H 0.2998 0.0656 1.2059 0.060 Uiso 1 1 calc R . . C13 C 0.30116(7) 0.11536(8) 1.12304(8) 0.0410(4) Uani 1 1 d . . . H13 H 0.2570 0.0973 1.1203 0.049 Uiso 1 1 calc R . . C14 C 0.41748(8) 0.10040(11) 1.23219(9) 0.0573(6) Uani 1 1 d . . . C15 C 0.47450(8) 0.10263(10) 1.22197(9) 0.0568(6) Uani 1 1 d . . . H15 H 0.4974 0.1195 1.1813 0.068 Uiso 1 1 calc R . . C16 C 0.49740(8) 0.07980(10) 1.27211(8) 0.0510(5) Uani 1 1 d . . . C17 C 0.46365(7) 0.05677(9) 1.33095(8) 0.0464(4) Uani 1 1 d . . . H17 H 0.4793 0.0428 1.3669 0.056 Uiso 1 1 calc R . . C18 C 0.40541(7) 0.05419(10) 1.33707(8) 0.0502(5) Uani 1 1 d . . . C19 C 0.36571(7) 0.02809(9) 1.39802(8) 0.0421(4) Uani 1 1 d . . . C20 C 0.39094(7) 0.03222(9) 1.46234(8) 0.0449(4) Uani 1 1 d . . . H20 H 0.4351 0.0523 1.4677 0.054 Uiso 1 1 calc R . . C21 C 0.35306(7) 0.00779(8) 1.51788(7) 0.0389(4) Uani 1 1 d . . . H21 H 0.3711 0.0107 1.5612 0.047 Uiso 1 1 calc R . . C22 C 0.28779(6) -0.02155(7) 1.51115(7) 0.0298(3) Uani 1 1 d . . . C23 C 0.26252(7) -0.02538(9) 1.44734(8) 0.0442(4) Uani 1 1 d . . . H23 H 0.2183 -0.0454 1.4422 0.053 Uiso 1 1 calc R . . C24 C 0.30062(7) -0.00048(10) 1.39103(8) 0.0490(5) Uani 1 1 d . . . H24 H 0.2826 -0.0028 1.3478 0.059 Uiso 1 1 calc R . . C25 C 0.24618(6) -0.04766(6) 1.57306(6) 0.0232(3) Uani 1 1 d . . . C26 C 0.55697(7) 0.08046(9) 1.26055(8) 0.0413(4) Uani 1 1 d . . . C27 C 0.57841(8) 0.08116(11) 1.19544(8) 0.0545(5) Uani 1 1 d . . . H27 H 0.5545 0.0807 1.1575 0.065 Uiso 1 1 calc R . . C28 C 0.63536(7) 0.08259(9) 1.18572(8) 0.0431(4) Uani 1 1 d . . . H28 H 0.6498 0.0836 1.1408 0.052 Uiso 1 1 calc R . . C29 C 0.64897(7) 0.08136(8) 1.30014(7) 0.0361(3) Uani 1 1 d . . . H29 H 0.6736 0.0816 1.3372 0.043 Uiso 1 1 calc R . . C30 C 0.59352(7) 0.07983(9) 1.31373(7) 0.0415(4) Uani 1 1 d . . . H30 H 0.5803 0.0784 1.3593 0.050 Uiso 1 1 calc R . . 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 0.01668(7) 0.01641(7) 0.01474(7) 0.00140(6) -0.00019(6) 0.00856(6) Co2 0.01841(8) 0.01512(7) 0.01493(7) 0.00114(6) 0.00079(6) 0.00676(6) Co3 0.01676(8) 0.01819(8) 0.01561(8) 0.00194(6) -0.00078(6) 0.00460(6) O1 0.0074(3) 0.0055(3) 0.0073(3) 0.0018(3) 0.0013(3) 0.0013(3) O2 0.0221(5) 0.0342(5) 0.0417(6) -0.0104(5) 0.0009(4) 0.0104(4) O3 0.0288(5) 0.0274(4) 0.0199(4) -0.0034(4) -0.0043(4) 0.0176(4) O4 0.0208(4) 0.0205(4) 0.0152(4) 0.0010(3) -0.0011(3) 0.0108(3) O5 0.0190(4) 0.0185(4) 0.0174(4) 0.0024(3) 0.0008(3) 0.0102(3) O6 0.0228(4) 0.0240(4) 0.0231(5) 0.0068(3) 0.0053(3) 0.0145(4) O7 0.0174(4) 0.0221(4) 0.0302(5) -0.0036(4) 0.0029(4) 0.0064(3) O8 0.0194(4) 0.0219(4) 0.0219(4) 0.0005(3) 0.0026(3) 0.0105(4) O9 0.0217(4) 0.0316(5) 0.0236(5) 0.0082(4) -0.0014(4) 0.0114(4) O10 0.0220(4) 0.0305(5) 0.0201(4) 0.0060(4) -0.0004(4) 0.0154(4) O11 0.0195(4) 0.0392(5) 0.0176(4) 0.0063(4) 0.0027(4) 0.0127(4) O12 0.0196(4) 0.0393(5) 0.0205(5) 0.0049(4) 0.0048(4) 0.0129(4) N1 0.0387(7) 0.1091(12) 0.0318(7) 0.0364(8) 0.0159(6) 0.0518(8) N2 0.0237(5) 0.0382(6) 0.0240(6) 0.0029(5) 0.0016(4) 0.0198(5) C1 0.0252(6) 0.0256(6) 0.0243(7) -0.0007(5) -0.0033(5) 0.0153(5) C2 0.0511(10) 0.0925(14) 0.0342(9) -0.0280(9) -0.0238(8) 0.0536(10) C3 0.0217(6) 0.0200(6) 0.0186(6) 0.0010(5) -0.0002(5) 0.0119(5) C4 0.0715(11) 0.0556(10) 0.0352(8) 0.0279(7) 0.0290(8) 0.0531(10) C5 0.0189(6) 0.0263(6) 0.0252(7) -0.0010(5) 0.0039(5) 0.0087(5) C6 0.0202(7) 0.0363(8) 0.0741(12) -0.0086(8) 0.0086(7) 0.0102(6) C7 0.0238(6) 0.0301(7) 0.0195(6) 0.0032(5) -0.0003(5) 0.0159(6) C8 0.0285(7) 0.0490(9) 0.0247(7) 0.0118(6) 0.0018(6) 0.0248(7) C9 0.0311(8) 0.0922(15) 0.0469(10) 0.0380(10) 0.0085(7) 0.0291(9) C10 0.0269(8) 0.138(2) 0.0661(13) 0.0664(14) 0.0130(8) 0.0391(11) C11 0.0306(8) 0.0956(14) 0.0377(9) 0.0347(9) 0.0112(7) 0.0382(9) C12 0.0314(8) 0.0912(14) 0.0360(9) 0.0363(9) 0.0143(7) 0.0377(9) C13 0.0283(7) 0.0729(11) 0.0319(8) 0.0228(8) 0.0078(6) 0.0328(8) C14 0.0378(9) 0.1098(16) 0.0396(10) 0.0436(10) 0.0181(7) 0.0484(11) C15 0.0366(9) 0.1129(16) 0.0383(9) 0.0444(10) 0.0194(7) 0.0506(10) C16 0.0372(8) 0.1000(14) 0.0342(9) 0.0326(9) 0.0139(7) 0.0481(10) C17 0.0367(8) 0.0919(13) 0.0292(8) 0.0271(8) 0.0102(6) 0.0461(9) C18 0.0332(8) 0.0982(14) 0.0336(9) 0.0313(9) 0.0129(7) 0.0437(9) C19 0.0289(7) 0.0778(12) 0.0293(8) 0.0269(8) 0.0120(6) 0.0339(8) C20 0.0232(7) 0.0782(12) 0.0308(8) 0.0201(8) 0.0067(6) 0.0235(8) C21 0.0287(7) 0.0656(11) 0.0217(7) 0.0134(7) 0.0054(6) 0.0229(7) C22 0.0222(6) 0.0465(8) 0.0237(7) 0.0116(6) 0.0080(5) 0.0195(6) C23 0.0235(7) 0.0787(12) 0.0315(8) 0.0169(8) 0.0104(6) 0.0263(8) C24 0.0323(8) 0.0984(14) 0.0219(7) 0.0200(8) 0.0080(6) 0.0368(9) C25 0.0222(6) 0.0284(7) 0.0200(6) 0.0057(5) 0.0069(5) 0.0134(5) C26 0.0314(8) 0.0761(12) 0.0291(8) 0.0250(8) 0.0111(6) 0.0365(8) C27 0.0434(9) 0.1165(17) 0.0246(8) 0.0181(9) 0.0040(7) 0.0557(11) C28 0.0325(8) 0.0843(13) 0.0220(7) 0.0077(8) 0.0035(6) 0.0363(9) C29 0.0358(8) 0.0609(10) 0.0247(7) 0.0059(7) -0.0006(6) 0.0340(8) C30 0.0351(8) 0.0833(12) 0.0202(7) 0.0132(7) 0.0088(6) 0.0401(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O6 2.0211(19) 6_554 ? Co1 O1 2.0341(15) . ? Co1 O10 2.0506(15) . ? Co1 O5 2.0710(15) . ? Co1 O8 2.122(2) 2 ? Co1 O4 2.1241(16) . ? Co2 O1 2.0075(16) . ? Co2 O3 2.0564(19) . ? Co2 O12 2.0708(16) 2_554 ? Co2 O4 2.1059(16) 6_554 ? Co2 O7 2.119(2) . ? Co2 O5 2.1307(16) 6_554 ? Co3 O1 2.0316(18) . ? Co3 O11 2.0322(18) 2_554 ? Co3 O9 2.0359(18) . ? Co3 N2 2.101(2) 5_664 ? Co3 O2 2.1096(17) . ? Co3 O8 2.1763(17) 2 ? O1 H1A 0.8502 . ? O2 H2E 0.8500 . ? O2 H2F 0.8513 . ? O3 C1 1.2447(17) . ? O4 C1 1.2718(18) . ? O4 Co2 2.1058(16) 2 ? O5 C3 1.2760(17) . ? O5 Co2 2.1306(16) 2 ? O6 C3 1.2444(17) . ? O6 Co1 2.0211(19) 2 ? O7 C5 1.2470(18) . ? O8 C5 1.2564(19) . ? O8 Co1 2.122(2) 6_554 ? O8 Co3 2.1765(17) 6_554 ? O9 C7 1.2668(17) . ? O10 C7 1.2450(18) . ? O11 C25 1.2550(18) . ? O11 Co3 2.0323(18) 6 ? O12 C25 1.2510(18) . ? O12 Co2 2.0708(16) 6 ? N1 C14 1.336(2) . ? N1 C18 1.346(2) . ? N2 C28 1.329(2) . ? N2 C29 1.334(2) . ? N2 Co3 2.101(2) 3_655 ? C1 C2 1.504(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.510(2) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.518(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.504(2) . ? C8 C9 1.371(2) . ? C8 C13 1.378(2) . ? C9 C10 1.371(2) . ? C9 H9 0.9500 . ? C10 C11 1.386(3) . ? C10 H10 0.9500 . ? C11 C12 1.376(2) . ? C11 C14 1.489(2) . ? C12 C13 1.383(2) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.394(2) . ? C15 C16 1.390(2) . ? C15 H15 0.9500 . ? C16 C17 1.375(2) . ? C16 C26 1.478(2) . ? C17 C18 1.410(2) . ? C17 H17 0.9500 . ? C18 C19 1.479(2) . ? C19 C20 1.394(2) . ? C19 C24 1.400(2) . ? C20 C21 1.369(2) . ? C20 H20 0.9500 . ? C21 C22 1.402(2) . ? C21 H21 0.9500 . ? C22 C23 1.387(2) . ? C22 C25 1.516(2) . ? C23 C24 1.384(2) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C26 C27 1.386(3) . ? C26 C30 1.388(2) . ? C27 C28 1.400(2) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.375(2) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Co1 O1 91.38(3) 6_554 . ? O6 Co1 O10 94.49(4) 6_554 . ? O1 Co1 O10 88.57(3) . . ? O6 Co1 O5 90.26(3) 6_554 . ? O1 Co1 O5 177.69(3) . . ? O10 Co1 O5 92.92(8) . . ? O6 Co1 O8 169.40(4) 6_554 2 ? O1 Co1 O8 79.49(3) . 2 ? O10 Co1 O8 90.70(4) . 2 ? O5 Co1 O8 98.72(3) . 2 ? O6 Co1 O4 88.78(3) 6_554 . ? O1 Co1 O4 98.77(3) . . ? O10 Co1 O4 171.90(3) . . ? O5 Co1 O4 79.63(8) . . ? O8 Co1 O4 87.31(3) 2 . ? O1 Co2 O3 96.88(3) . . ? O1 Co2 O12 91.66(7) . 2_554 ? O3 Co2 O12 90.78(4) . 2_554 ? O1 Co2 O4 163.96(3) . 6_554 ? O3 Co2 O4 92.28(3) . 6_554 ? O12 Co2 O4 101.39(8) 2_554 6_554 ? O1 Co2 O7 86.06(3) . . ? O3 Co2 O7 175.96(4) . . ? O12 Co2 O7 86.35(4) 2_554 . ? O4 Co2 O7 85.51(3) 6_554 . ? O1 Co2 O5 88.08(7) . 6_554 ? O3 Co2 O5 90.27(3) . 6_554 ? O12 Co2 O5 178.95(4) 2_554 6_554 ? O4 Co2 O5 78.71(8) 6_554 6_554 ? O7 Co2 O5 92.61(3) . 6_554 ? O1 Co3 O11 91.20(3) . 2_554 ? O1 Co3 O9 89.44(4) . . ? O11 Co3 O9 179.08(4) 2_554 . ? O1 Co3 N2 176.06(4) . 5_664 ? O11 Co3 N2 92.65(4) 2_554 5_664 ? O9 Co3 N2 86.71(5) . 5_664 ? O1 Co3 O2 88.51(3) . . ? O11 Co3 O2 89.24(7) 2_554 . ? O9 Co3 O2 91.44(7) . . ? N2 Co3 O2 92.38(4) 5_664 . ? O1 Co3 O8 78.27(3) . 2 ? O11 Co3 O8 90.77(7) 2_554 2 ? O9 Co3 O8 88.71(7) . 2 ? N2 Co3 O8 100.83(4) 5_664 2 ? O2 Co3 O8 166.78(3) . 2 ? Co2 O1 Co3 130.03(4) . . ? Co2 O1 Co1 116.87(6) . . ? Co3 O1 Co1 101.80(4) . . ? Co2 O1 H1A 92.2 . . ? Co3 O1 H1A 115.7 . . ? Co1 O1 H1A 95.0 . . ? Co3 O2 H2E 121.7 . . ? Co3 O2 H2F 128.7 . . ? H2E O2 H2F 107.6 . . ? C1 O3 Co2 140.64(9) . . ? C1 O4 Co2 134.90(9) . 2 ? C1 O4 Co1 125.36(8) . . ? Co2 O4 Co1 96.25(8) 2 . ? C3 O5 Co1 132.25(8) . . ? C3 O5 Co2 126.30(8) . 2 ? Co1 O5 Co2 97.10(7) . 2 ? C3 O6 Co1 138.65(8) . 2 ? C5 O7 Co2 133.50(8) . . ? C5 O8 Co1 126.49(8) . 6_554 ? C5 O8 Co3 134.22(8) . 6_554 ? Co1 O8 Co3 94.44(3) 6_554 6_554 ? C7 O9 Co3 129.56(9) . . ? C7 O10 Co1 128.91(9) . . ? C25 O11 Co3 132.90(9) . 6 ? C25 O12 Co2 135.45(9) . 6 ? C14 N1 C18 118.84(13) . . ? C28 N2 C29 118.15(13) . . ? C28 N2 Co3 119.40(10) . 3_655 ? C29 N2 Co3 122.38(9) . 3_655 ? O3 C1 O4 124.60(12) . . ? O3 C1 C2 117.75(13) . . ? O4 C1 C2 117.59(12) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O6 C3 O5 124.57(11) . . ? O6 C3 C4 115.97(12) . . ? O5 C3 C4 119.46(11) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O7 C5 O8 124.77(11) . . ? O7 C5 C6 117.68(12) . . ? O8 C5 C6 117.54(12) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O10 C7 O9 126.93(12) . . ? O10 C7 C8 117.64(11) . . ? O9 C7 C8 115.43(12) . . ? C9 C8 C13 118.56(13) . . ? C9 C8 C7 120.86(13) . . ? C13 C8 C7 120.57(13) . . ? C10 C9 C8 120.56(16) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 121.03(16) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C12 C11 C10 118.64(14) . . ? C12 C11 C14 119.63(15) . . ? C10 C11 C14 121.72(15) . . ? C11 C12 C13 119.71(15) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C8 C13 C12 121.39(14) . . ? C8 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? N1 C14 C15 122.30(14) . . ? N1 C14 C11 117.13(14) . . ? C15 C14 C11 120.52(14) . . ? C16 C15 C14 119.14(15) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C17 C16 C15 118.93(14) . . ? C17 C16 C26 121.85(13) . . ? C15 C16 C26 119.22(14) . . ? C16 C17 C18 118.90(13) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? N1 C18 C17 121.80(14) . . ? N1 C18 C19 116.41(14) . . ? C17 C18 C19 121.77(13) . . ? C20 C19 C24 118.91(13) . . ? C20 C19 C18 122.29(15) . . ? C24 C19 C18 118.78(14) . . ? C21 C20 C19 121.03(15) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 120.37(14) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C23 C22 C21 118.79(13) . . ? C23 C22 C25 121.14(13) . . ? C21 C22 C25 120.07(13) . . ? C24 C23 C22 121.08(14) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C19 119.80(14) . . ? C23 C24 H24 120.1 . . ? C19 C24 H24 120.1 . . ? O12 C25 O11 127.35(11) . . ? O12 C25 C22 115.91(12) . . ? O11 C25 C22 116.66(12) . . ? C27 C26 C30 117.07(14) . . ? C27 C26 C16 120.91(13) . . ? C30 C26 C16 122.01(14) . . ? C26 C27 C28 119.92(14) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? N2 C28 C27 121.93(14) . . ? N2 C28 H28 119.0 . . ? C27 C28 H28 119.0 . . ? N2 C29 C30 123.29(13) . . ? N2 C29 H29 118.4 . . ? C30 C29 H29 118.4 . . ? C29 C30 C26 119.62(14) . . ? C29 C30 H30 120.2 . . ? C26 C30 H30 120.2 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.239 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.033 data_PCN-122 _database_code_depnum_ccdc_archive 'CCDC 813719' #TrackingRef '4320_web_deposit_cif_file_0_JinheePark_1297970601.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H15 Co N2 O4.50' _chemical_formula_sum 'C24 H15 Co N2 O4.50' _chemical_formula_weight 462.31 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 tetragonal _symmetry_space_group_name_H-M I41cd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x+1/2, z+1/4' '-x, -y, z' 'y, -x+1/2, z+1/4' '-x, y, z+1/2' 'x, -y, z+1/2' '-y+1/2, -x, z+1/4' 'y+1/2, x, z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1, z+3/4' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1, z+3/4' '-x+1/2, y+1/2, z+1' 'x+1/2, -y+1/2, z+1' '-y+1, -x+1/2, z+3/4' 'y+1, x+1/2, z+3/4' _cell_length_a 23.394(4) _cell_length_b 23.394(4) _cell_length_c 49.524(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 27103(9) _cell_formula_units_Z 16 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9519 _cell_measurement_theta_min 2.3045 _cell_measurement_theta_max 18.4055 _exptl_crystal_description sheet _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3776 _exptl_absorpt_coefficient_mu 0.265 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9490 _exptl_absorpt_correction_T_max 0.9740 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 152492 _diffrn_reflns_av_R_equivalents 0.1264 _diffrn_reflns_av_sigmaI/netI 0.0869 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -64 _diffrn_reflns_limit_l_max 64 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.70 _reflns_number_total 15720 _reflns_number_gt 9307 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0381P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.063(9) _refine_ls_number_reflns 15720 _refine_ls_number_parameters 285 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0894 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 0.842 _refine_ls_restrained_S_all 0.842 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.015 -0.005 -0.017 20886 4104 ' ' _platon_squeeze_details ; ; 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 0.957157(12) 0.439570(11) 0.918162(6) 0.04362(8) Uani 1 1 d . . . O1 O 0.94029(6) 0.11201(6) 0.69630(3) 0.0511(4) Uani 1 1 d . . . O2 O 0.88039(6) 0.04030(6) 0.70180(3) 0.0575(4) Uani 1 1 d . . . O3 O 0.57468(5) -0.00181(6) 0.89275(3) 0.0453(3) Uani 1 1 d . . . O4 O 0.53330(6) 0.08241(6) 0.90232(3) 0.0539(4) Uani 1 1 d . . . O5 O 1.0000 0.5000 0.94395(4) 0.0560(6) Uani 1 2 d S . . H5A H 1.0214 0.4805 0.9543 0.084 Uiso 1 1 d R . . N1 N 0.91643(8) 0.37785(7) 0.89332(4) 0.0527(5) Uani 1 1 d . . . N2 N 0.78127(8) 0.15494(8) 0.82209(4) 0.0752(6) Uani 1 1 d . . . C1 C 0.94791(11) 0.33607(13) 0.88004(5) 0.0899(9) Uani 1 1 d . . . H1 H 0.9885 0.3370 0.8810 0.108 Uiso 1 1 calc R . . C2 C 0.92322(13) 0.29577(13) 0.86628(7) 0.1147(13) Uani 1 1 d . . . H2 H 0.9460 0.2672 0.8579 0.138 Uiso 1 1 calc R . . C3 C 0.86217(11) 0.29368(10) 0.86348(4) 0.0639(7) Uani 1 1 d . . . C4 C 0.83245(11) 0.33440(11) 0.87661(6) 0.0863(9) Uani 1 1 d . . . H4 H 0.7919 0.3357 0.8755 0.104 Uiso 1 1 calc R . . C5 C 0.86214(10) 0.37464(10) 0.89193(5) 0.0701(7) Uani 1 1 d . . . H5 H 0.8404 0.4015 0.9020 0.084 Uiso 1 1 calc R . . C6 C 0.82828(11) 0.18124(10) 0.81158(5) 0.0746(8) Uani 1 1 d . . . C7 C 0.85441(10) 0.22425(10) 0.82490(5) 0.0717(7) Uani 1 1 d . . . H7 H 0.8884 0.2404 0.8177 0.086 Uiso 1 1 calc R . . C8 C 0.83260(10) 0.24477(10) 0.84852(5) 0.0659(7) Uani 1 1 d . . . C9 C 0.78520(10) 0.22127(11) 0.85830(5) 0.0751(8) Uani 1 1 d . . . H9 H 0.7679 0.2367 0.8740 0.090 Uiso 1 1 calc R . . C10 C 0.76131(10) 0.17538(10) 0.84596(5) 0.0700(7) Uani 1 1 d . . . C11 C 0.84834(10) 0.15703(11) 0.78579(5) 0.0715(7) Uani 1 1 d . . . C12 C 0.88806(11) 0.18375(10) 0.77004(5) 0.0781(8) Uani 1 1 d . . . H12 H 0.9040 0.2191 0.7758 0.094 Uiso 1 1 calc R . . C13 C 0.90528(11) 0.16015(11) 0.74600(5) 0.0734(8) Uani 1 1 d . . . H13 H 0.9336 0.1792 0.7357 0.088 Uiso 1 1 calc R . . C14 C 0.88330(9) 0.11090(10) 0.73663(4) 0.0557(6) Uani 1 1 d . . . C15 C 0.84359(11) 0.08375(12) 0.75142(5) 0.0839(9) Uani 1 1 d . . . H15 H 0.8259 0.0504 0.7443 0.101 Uiso 1 1 calc R . . C16 C 0.82788(12) 0.10316(12) 0.77663(6) 0.1086(12) Uani 1 1 d . . . H16 H 0.8036 0.0808 0.7878 0.130 Uiso 1 1 calc R . . C17 C 0.90209(10) 0.08737(11) 0.71039(5) 0.0588(6) Uani 1 1 d . . . C18 C 0.66038(10) 0.05502(10) 0.86358(4) 0.0655(7) Uani 1 1 d . . . H18 H 0.6571 0.0151 0.8604 0.079 Uiso 1 1 calc R . . C19 C 0.70489(10) 0.08546(10) 0.85245(5) 0.0737(8) Uani 1 1 d . . . H19 H 0.7317 0.0665 0.8412 0.088 Uiso 1 1 calc R . . C20 C 0.71135(9) 0.14406(10) 0.85753(5) 0.0621(6) Uani 1 1 d . . . C21 C 0.67230(9) 0.17072(9) 0.87373(5) 0.0648(7) Uani 1 1 d . . . H21 H 0.6766 0.2105 0.8771 0.078 Uiso 1 1 calc R . . C22 C 0.62885(10) 0.14335(9) 0.88485(5) 0.0584(6) Uani 1 1 d . . . H22 H 0.6035 0.1636 0.8964 0.070 Uiso 1 1 calc R . . C23 C 0.61918(9) 0.08377(9) 0.87989(4) 0.0510(6) Uani 1 1 d . . . C24 C 0.57290(8) 0.05249(10) 0.89265(4) 0.0445(5) 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 0.04669(16) 0.04454(15) 0.03963(13) 0.00092(15) 0.00818(14) 0.00131(13) O1 0.0444(9) 0.0631(10) 0.0460(9) -0.0088(7) 0.0066(7) -0.0067(8) O2 0.0594(10) 0.0553(10) 0.0576(10) -0.0175(8) 0.0076(8) -0.0053(8) O3 0.0542(9) 0.0410(9) 0.0408(8) -0.0016(7) 0.0043(7) 0.0045(7) O4 0.0523(9) 0.0513(9) 0.0580(10) 0.0027(7) 0.0186(8) 0.0050(7) O5 0.0613(14) 0.0496(13) 0.0573(13) 0.000 0.000 0.0023(11) N1 0.0509(12) 0.0511(11) 0.0562(12) -0.0092(9) 0.0181(9) -0.0057(9) N2 0.0783(15) 0.0737(14) 0.0737(14) -0.0286(11) 0.0371(12) -0.0279(12) C1 0.0717(19) 0.106(2) 0.092(2) -0.0582(18) 0.0189(16) -0.0167(17) C2 0.090(2) 0.098(2) 0.156(3) -0.081(2) 0.073(2) -0.0318(18) C3 0.0711(17) 0.0746(17) 0.0461(14) -0.0141(12) 0.0276(12) -0.0169(14) C4 0.0689(17) 0.0725(18) 0.117(2) -0.0440(17) 0.0320(17) -0.0054(15) C5 0.0471(15) 0.0712(17) 0.092(2) -0.0375(15) 0.0225(14) -0.0112(13) C6 0.0820(18) 0.0689(17) 0.0730(17) -0.0289(14) 0.0393(15) -0.0275(15) C7 0.0707(16) 0.0719(17) 0.0724(17) -0.0321(14) 0.0357(13) -0.0281(13) C8 0.0770(17) 0.0740(17) 0.0467(14) -0.0225(12) 0.0229(13) -0.0207(14) C9 0.0810(18) 0.0846(18) 0.0597(16) -0.0385(14) 0.0442(14) -0.0452(15) C10 0.0732(17) 0.0787(18) 0.0582(16) -0.0198(14) 0.0316(13) -0.0136(14) C11 0.0729(17) 0.0859(19) 0.0556(15) -0.0275(14) 0.0224(13) -0.0209(15) C12 0.0887(19) 0.0708(17) 0.0746(18) -0.0347(14) 0.0417(15) -0.0326(15) C13 0.0909(19) 0.0756(18) 0.0537(16) -0.0180(14) 0.0333(14) -0.0296(15) C14 0.0627(15) 0.0645(16) 0.0398(13) -0.0204(11) 0.0241(12) -0.0196(12) C15 0.091(2) 0.095(2) 0.0656(18) -0.0447(15) 0.0387(15) -0.0338(16) C16 0.104(2) 0.104(2) 0.118(3) -0.059(2) 0.0641(19) -0.0602(19) C17 0.0522(15) 0.0632(17) 0.0609(16) -0.0218(13) -0.0026(13) -0.0086(13) C18 0.0813(17) 0.0568(15) 0.0584(15) -0.0249(12) 0.0209(13) -0.0040(13) C19 0.0678(17) 0.0653(17) 0.0879(19) -0.0282(14) 0.0424(15) -0.0180(13) C20 0.0550(15) 0.0673(17) 0.0638(16) -0.0195(13) 0.0199(12) -0.0274(12) C21 0.0651(15) 0.0490(14) 0.0802(17) -0.0338(13) 0.0309(14) -0.0237(12) C22 0.0717(16) 0.0447(14) 0.0590(15) -0.0094(11) 0.0268(13) -0.0030(12) C23 0.0582(15) 0.0532(14) 0.0415(12) -0.0001(11) 0.0206(11) 0.0019(11) C24 0.0393(13) 0.0609(16) 0.0333(11) -0.0028(11) -0.0004(9) 0.0010(11) _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 O3 2.0048(14) 13_654 ? Co1 O4 2.0131(14) 14_554 ? Co1 N1 2.1229(18) . ? Co1 O1 2.1357(14) 2_645 ? Co1 O5 2.1526(13) . ? Co1 O2 2.1668(15) 2_645 ? Co1 C17 2.496(2) 2_645 ? O1 C17 1.272(3) . ? O1 Co1 2.1358(14) 12_554 ? O2 C17 1.285(2) . ? O2 Co1 2.1669(15) 12_554 ? O3 C24 1.271(2) . ? O3 Co1 2.0048(14) 13_644 ? O4 C24 1.256(2) . ? O4 Co1 2.0130(14) 14_454 ? O5 Co1 2.1527(13) 3_765 ? O5 H5A 0.8494 . ? N1 C5 1.274(3) . ? N1 C1 1.389(3) . ? N2 C10 1.358(3) . ? N2 C6 1.364(3) . ? C1 C2 1.299(3) . ? C1 H1 0.9500 . ? C2 C3 1.436(3) . ? C2 H2 0.9500 . ? C3 C4 1.347(3) . ? C3 C8 1.529(3) . ? C4 C5 1.394(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.350(3) . ? C6 C11 1.474(3) . ? C7 C8 1.364(3) . ? C7 H7 0.9500 . ? C8 C9 1.329(3) . ? C9 C10 1.356(3) . ? C9 H9 0.9500 . ? C10 C20 1.494(3) . ? C11 C12 1.365(3) . ? C11 C16 1.422(3) . ? C12 C13 1.373(3) . ? C12 H12 0.9500 . ? C13 C14 1.344(3) . ? C13 H13 0.9500 . ? C14 C15 1.343(3) . ? C14 C17 1.478(3) . ? C15 C16 1.379(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 Co1 2.495(2) 12_554 ? C18 C19 1.377(3) . ? C18 C23 1.426(3) . ? C18 H18 0.9500 . ? C19 C20 1.402(3) . ? C19 H19 0.9500 . ? C20 C21 1.367(3) . ? C21 C22 1.321(3) . ? C21 H21 0.9500 . ? C22 C23 1.433(3) . ? C22 H22 0.9500 . ? C23 C24 1.451(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 O3 Co1 O4 104.99(6) 13_654 14_554 ? O3 Co1 N1 86.26(6) 13_654 . ? O4 Co1 N1 89.86(6) 14_554 . ? O3 Co1 O1 97.06(6) 13_654 2_645 ? O4 Co1 O1 157.93(6) 14_554 2_645 ? N1 Co1 O1 92.49(6) . 2_645 ? O3 Co1 O5 95.52(5) 13_654 . ? O4 Co1 O5 89.25(5) 14_554 . ? N1 Co1 O5 178.17(6) . . ? O1 Co1 O5 87.73(5) 2_645 . ? O3 Co1 O2 158.42(6) 13_654 2_645 ? O4 Co1 O2 96.44(6) 14_554 2_645 ? N1 Co1 O2 91.33(7) . 2_645 ? O1 Co1 O2 61.59(6) 2_645 2_645 ? O5 Co1 O2 87.18(6) . 2_645 ? O3 Co1 C17 127.70(7) 13_654 2_645 ? O4 Co1 C17 127.31(7) 14_554 2_645 ? N1 Co1 C17 93.40(8) . 2_645 ? O1 Co1 C17 30.64(6) 2_645 2_645 ? O5 Co1 C17 85.87(7) . 2_645 ? O2 Co1 C17 30.99(6) 2_645 2_645 ? C17 O1 Co1 90.51(13) . 12_554 ? C17 O2 Co1 88.77(13) . 12_554 ? C24 O3 Co1 132.37(13) . 13_644 ? C24 O4 Co1 131.23(13) . 14_454 ? Co1 O5 Co1 107.22(9) . 3_765 ? Co1 O5 H5A 106.3 . . ? Co1 O5 H5A 115.8 3_765 . ? C5 N1 C1 117.5(2) . . ? C5 N1 Co1 121.25(15) . . ? C1 N1 Co1 120.99(16) . . ? C10 N2 C6 116.78(19) . . ? C2 C1 N1 121.6(3) . . ? C2 C1 H1 119.2 . . ? N1 C1 H1 119.2 . . ? C1 C2 C3 121.2(2) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C4 C3 C2 116.3(2) . . ? C4 C3 C8 122.0(2) . . ? C2 C3 C8 121.5(2) . . ? C3 C4 C5 118.9(2) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 124.5(2) . . ? N1 C5 H5 117.8 . . ? C4 C5 H5 117.8 . . ? C7 C6 N2 121.0(2) . . ? C7 C6 C11 124.5(2) . . ? N2 C6 C11 114.5(2) . . ? C6 C7 C8 120.8(2) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C9 C8 C7 118.6(2) . . ? C9 C8 C3 120.7(2) . . ? C7 C8 C3 120.7(2) . . ? C8 C9 C10 120.5(2) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C9 C10 N2 122.0(2) . . ? C9 C10 C20 122.6(2) . . ? N2 C10 C20 115.5(2) . . ? C12 C11 C16 116.9(2) . . ? C12 C11 C6 122.4(2) . . ? C16 C11 C6 120.6(2) . . ? C11 C12 C13 120.7(2) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C14 C13 C12 122.1(2) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C15 C14 C13 118.8(2) . . ? C15 C14 C17 120.6(2) . . ? C13 C14 C17 120.6(2) . . ? C14 C15 C16 121.5(2) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C15 C16 C11 119.4(2) . . ? C15 C16 H16 120.3 . . ? C11 C16 H16 120.3 . . ? O1 C17 O2 119.0(2) . . ? O1 C17 C14 121.5(2) . . ? O2 C17 C14 119.5(2) . . ? O1 C17 Co1 58.85(11) . 12_554 ? O2 C17 Co1 60.24(11) . 12_554 ? C14 C17 Co1 175.33(18) . 12_554 ? C19 C18 C23 119.6(2) . . ? C19 C18 H18 120.2 . . ? C23 C18 H18 120.2 . . ? C18 C19 C20 121.0(2) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C21 C20 C19 118.7(2) . . ? C21 C20 C10 121.6(2) . . ? C19 C20 C10 119.7(2) . . ? C22 C21 C20 122.5(2) . . ? C22 C21 H21 118.7 . . ? C20 C21 H21 118.7 . . ? C21 C22 C23 121.4(2) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C18 C23 C22 116.7(2) . . ? C18 C23 C24 120.9(2) . . ? C22 C23 C24 122.23(19) . . ? O4 C24 O3 125.41(18) . . ? O4 C24 C23 115.81(19) . . ? O3 C24 C23 118.76(19) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.70 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.438 _refine_diff_density_min -0.173 _refine_diff_density_rms 0.025