Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_contact_author 'Dra. Miren Karmele Urtiaga' _publ_contact_author_address ; Dra. Miren Karmele Urtiaga Dpto. de Mineralog\'ia y Petrolog\'ia Universidad del Pa\'is Vasco Apartado 644 48080 Bilbao Spain ; _publ_contact_author_phone '34 4 6012555' _publ_contact_author_fax '34 4 4648500' _publ_contact_author_email nppurgrm@lg.ehu.es _publ_requested_journal 'J.Chem.Soc.Dalton Trans.' loop_ _publ_author_name _publ_author_address 'Hernandez, M.L.' ; Dpto. Qu\'imica Inorg\'anica Facultad de Ciencias Universidad del Pa\'is Vasco/E.H.U. P.O. Box 644 48080 Bilbao Spain ; 'Urtiaga, M.K.' ; Dpto. de Mineralog\'ia y Petrolog\'ia Facultad de Ciencias Universidad del Pa\'is Vasco/E.H.U. P.O. Box 644 48080 Bilbao Spain ; 'Barandika, M.G.' ; Dpto. Qu\'imica Inorg\'anica Facultad de Farmacia Universidad del Pa\'is Vasco/E.H.U. P.O. Box 450 01080 Vitoria Spain ; 'Cortes, R.' ; Dpto. Qu\'imica Inorg\'anica Facultad de Farmacia Universidad del Pa\'is Vasco/E.H.U. P.O. Box 450 01080 Vitoria Spain ; 'Lezama, L.' ; Dpto. Qu\'imica Inorg\'anica Facultad de Ciencias Universidad del Pa\'is Vasco/E.H.U. P.O. Box 644 48080 Bilbao Spain ; 'Arriortua, M.I.' ; Dpto. de Mineralog\'ia y Petrolog\'ia Facultad de Ciencias Universidad del Pa\'is Vasco/E.H.U. P.O. Box 644 48080 Bilbao Spain ; 'Rojo, T.' ; Dpto. Qu\'imica Inorg\'anica Facultad de Ciencias Universidad del Pa\'is Vasco/E.H.U. P.O. Box 644 48080 Bilbao Spain data_conco _database_code_CSD 158590 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H36 Co N8 O2' _chemical_formula_weight 695.68 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 19.869(2) _cell_length_b 9.639(2) _cell_length_c 18.821(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.72(2) _cell_angle_gamma 90.00 _cell_volume 3586.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1452 _exptl_absorpt_coefficient_mu 0.523 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _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 10494 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 30.03 _reflns_number_total 5252 _reflns_number_gt 3227 _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^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5252 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1258 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.2020 _refine_ls_wR_factor_gt 0.1458 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 0.30913(6) 0.2500 0.0422(2) Uani 1 2 d S . . N3 N 0.04173(15) 0.3060(3) 0.15379(15) 0.0558(7) Uani 1 1 d . . . C13 C 0.07505(15) 0.2933(3) 0.10712(16) 0.0415(6) Uani 1 1 d . . . O1 O 0.10817(13) 0.2797(3) 0.05777(14) 0.0651(7) Uani 1 1 d . . . N1 N -0.07366(14) 0.1492(3) 0.21200(14) 0.0472(6) Uani 1 1 d . . . C1 C -0.11244(18) 0.1612(4) 0.14926(18) 0.0500(8) Uani 1 1 d . . . C2 C -0.16573(18) 0.0740(4) 0.12911(18) 0.0528(8) Uani 1 1 d . . . C3 C -0.18106(15) -0.0344(3) 0.17282(18) 0.0463(7) Uani 1 1 d . . . C4 C -0.1399(2) -0.0495(4) 0.23632(19) 0.0548(8) Uani 1 1 d . . . C5 C -0.0886(2) 0.0420(4) 0.25329(19) 0.0559(9) Uani 1 1 d . . . C6 C -0.23933(17) -0.1311(4) 0.1520(2) 0.0577(9) Uani 1 1 d . . . C7 C -0.21967(19) -0.2506(4) 0.1037(2) 0.0578(9) Uani 1 1 d . . . C8 C -0.0580(2) -0.4485(4) 0.1539(2) 0.0670(11) Uani 1 1 d . . . C9 C -0.1045(2) -0.3582(4) 0.1198(2) 0.0641(10) Uani 1 1 d . . . C10 C -0.16788(17) -0.3476(3) 0.14078(18) 0.0484(7) Uani 1 1 d . . . C11 C -0.18107(19) -0.4289(5) 0.1978(2) 0.0714(12) Uani 1 1 d . . . C12 C -0.1322(2) -0.5161(4) 0.2295(2) 0.0672(11) Uani 1 1 d . . . N2 N -0.07137(14) -0.5287(3) 0.20789(15) 0.0490(6) Uani 1 1 d . . . N4 N 0.17809(19) 0.6929(4) 0.0591(2) 0.0822(11) Uani 1 1 d . . . C14 C 0.1833(2) 0.8279(5) 0.0696(3) 0.0777(13) Uani 1 1 d . . . C15 C 0.1298(2) 0.9194(5) 0.0625(2) 0.0627(10) Uani 1 1 d . . . C16 C 0.06505(17) 0.8701(4) 0.04478(17) 0.0473(7) Uani 1 1 d . . . C17 C 0.0592(2) 0.7289(4) 0.0330(2) 0.0580(9) Uani 1 1 d . . . C18 C 0.1156(3) 0.6464(5) 0.0409(3) 0.0756(12) Uani 1 1 d . . . C19 C 0.00430(18) 0.9659(4) 0.03661(19) 0.0508(8) Uani 1 1 d . . . H1 H -0.0978(17) 0.229(4) 0.1224(19) 0.048(9) Uiso 1 1 d . . . H2 H -0.1923(18) 0.089(4) 0.0865(19) 0.051(9) Uiso 1 1 d . . . H4 H -0.1482(18) -0.126(4) 0.2680(19) 0.057(10) Uiso 1 1 d . . . H5 H -0.0583(18) 0.029(4) 0.2986(18) 0.053(9) Uiso 1 1 d . . . H6A H -0.259(2) -0.182(5) 0.193(3) 0.086(15) Uiso 1 1 d . . . H6B H -0.2755(19) -0.078(4) 0.1246(19) 0.060(10) Uiso 1 1 d . . . H7A H -0.261(2) -0.298(4) 0.087(2) 0.061(11) Uiso 1 1 d . . . H7B H -0.2015(19) -0.202(4) 0.057(2) 0.064(11) Uiso 1 1 d . . . H8 H -0.010(2) -0.452(4) 0.141(2) 0.069(12) Uiso 1 1 d . . . H9 H -0.090(2) -0.306(5) 0.085(3) 0.090(16) Uiso 1 1 d . . . H11 H -0.225(2) -0.425(4) 0.212(2) 0.067(11) Uiso 1 1 d . . . H12 H -0.140(2) -0.567(5) 0.270(2) 0.084(14) Uiso 1 1 d . . . H14 H 0.227(3) 0.871(5) 0.078(2) 0.090(15) Uiso 1 1 d . . . H15 H 0.137(2) 1.010(5) 0.069(2) 0.089(15) Uiso 1 1 d . . . H17 H 0.020(2) 0.696(5) 0.016(3) 0.086(15) Uiso 1 1 d . . . H18 H 0.112(2) 0.557(6) 0.031(3) 0.094(16) Uiso 1 1 d . . . H19A H -0.038(2) 0.911(5) 0.042(2) 0.075(12) Uiso 1 1 d . . . H19B H 0.010(2) 1.039(5) 0.074(2) 0.075(13) Uiso 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 0.0454(3) 0.0374(3) 0.0442(3) 0.000 0.0062(2) 0.000 N3 0.0613(17) 0.0545(17) 0.0524(15) -0.0008(13) 0.0104(13) 0.0047(14) C13 0.0433(15) 0.0341(14) 0.0461(16) -0.0001(12) -0.0007(13) -0.0010(12) O1 0.0616(15) 0.0731(18) 0.0634(15) -0.0082(13) 0.0202(13) -0.0050(13) N1 0.0490(15) 0.0430(13) 0.0484(14) 0.0010(11) -0.0010(12) -0.0023(11) C1 0.0564(19) 0.0468(18) 0.0460(17) 0.0061(14) 0.0018(14) 0.0006(14) C2 0.0537(19) 0.0539(19) 0.0480(17) -0.0015(15) -0.0093(15) 0.0062(15) C3 0.0365(15) 0.0458(16) 0.0560(18) -0.0061(14) 0.0013(13) 0.0059(12) C4 0.066(2) 0.0438(17) 0.0526(19) 0.0063(15) -0.0034(16) -0.0085(15) C5 0.067(2) 0.0475(18) 0.0496(18) 0.0095(15) -0.0127(16) -0.0070(16) C6 0.0366(16) 0.054(2) 0.080(3) -0.0032(18) -0.0076(16) 0.0065(15) C7 0.0477(19) 0.0493(18) 0.071(2) -0.0044(18) -0.0206(17) 0.0003(15) C8 0.062(2) 0.061(2) 0.084(3) 0.024(2) 0.034(2) 0.0183(18) C9 0.075(3) 0.055(2) 0.066(2) 0.0218(18) 0.026(2) 0.0165(18) C10 0.0500(18) 0.0386(15) 0.0544(18) -0.0043(13) -0.0051(14) -0.0052(13) C11 0.0385(18) 0.080(3) 0.098(3) 0.028(2) 0.0229(19) 0.0041(18) C12 0.054(2) 0.072(2) 0.079(3) 0.032(2) 0.0255(19) 0.0094(18) N2 0.0483(15) 0.0413(14) 0.0586(16) 0.0076(12) 0.0122(12) 0.0027(11) N4 0.063(2) 0.073(2) 0.107(3) 0.008(2) -0.005(2) 0.0239(19) C14 0.048(2) 0.077(3) 0.105(3) -0.002(3) -0.010(2) 0.007(2) C15 0.055(2) 0.056(2) 0.074(2) -0.0080(19) -0.0076(18) 0.0027(17) C16 0.0473(17) 0.0484(17) 0.0452(16) 0.0043(13) -0.0002(13) 0.0096(14) C17 0.052(2) 0.0496(19) 0.071(2) 0.0071(17) -0.0010(18) 0.0004(15) C18 0.077(3) 0.046(2) 0.102(3) 0.006(2) -0.001(2) 0.014(2) C19 0.0469(18) 0.0482(18) 0.0570(19) 0.0021(15) 0.0032(15) 0.0066(14) _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 N3 2.066(3) 2 ? Co1 N3 2.066(3) . ? Co1 N1 2.196(3) . ? Co1 N1 2.196(3) 2 ? Co1 N2 2.204(3) 2_565 ? Co1 N2 2.204(3) 1_565 ? N3 C13 1.158(4) . ? C13 O1 1.198(4) . ? N1 C5 1.343(4) . ? N1 C1 1.349(4) . ? C1 C2 1.375(5) . ? C1 H1 0.90(4) . ? C2 C3 1.383(5) . ? C2 H2 0.93(4) . ? C3 C4 1.387(5) . ? C3 C6 1.507(5) . ? C4 C5 1.362(5) . ? C4 H4 0.97(4) . ? C5 H5 1.00(4) . ? C6 C7 1.542(5) . ? C6 H6A 1.02(5) . ? C6 H6B 0.99(4) . ? C7 C10 1.509(5) . ? C7 H7A 0.97(4) . ? C7 H7B 1.09(4) . ? C8 N2 1.325(4) . ? C8 C9 1.380(5) . ? C8 H8 1.01(4) . ? C9 C10 1.362(5) . ? C9 H9 0.89(5) . ? C10 C11 1.375(5) . ? C11 C12 1.374(5) . ? C11 H11 0.94(4) . ? C12 N2 1.319(5) . ? C12 H12 0.93(5) . ? N2 Co1 2.204(3) 1_545 ? N4 C14 1.319(6) . ? N4 C18 1.332(6) . ? C14 C15 1.377(6) . ? C14 H14 0.95(5) . ? C15 C16 1.382(5) . ? C15 H15 0.89(5) . ? C16 C17 1.382(5) . ? C16 C19 1.516(5) . ? C17 C18 1.370(6) . ? C17 H17 0.86(5) . ? C18 H18 0.89(5) . ? C19 C19 1.521(7) 5_575 ? C19 H19A 1.01(4) . ? C19 H19B 1.00(4) . ? 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 N3 Co1 N3 178.31(17) 2 . ? N3 Co1 N1 87.84(11) 2 . ? N3 Co1 N1 90.97(11) . . ? N3 Co1 N1 90.97(11) 2 2 ? N3 Co1 N1 87.84(11) . 2 ? N1 Co1 N1 90.82(14) . 2 ? N3 Co1 N2 89.73(11) 2 2_565 ? N3 Co1 N2 91.46(11) . 2_565 ? N1 Co1 N2 177.51(11) . 2_565 ? N1 Co1 N2 89.82(10) 2 2_565 ? N3 Co1 N2 91.46(11) 2 1_565 ? N3 Co1 N2 89.73(11) . 1_565 ? N1 Co1 N2 89.81(10) . 1_565 ? N1 Co1 N2 177.50(11) 2 1_565 ? N2 Co1 N2 89.65(15) 2_565 1_565 ? C13 N3 Co1 167.5(3) . . ? N3 C13 O1 178.5(4) . . ? C5 N1 C1 115.6(3) . . ? C5 N1 Co1 122.0(2) . . ? C1 N1 Co1 121.9(2) . . ? N1 C1 C2 123.1(3) . . ? N1 C1 H1 112(2) . . ? C2 C1 H1 125(2) . . ? C1 C2 C3 120.5(3) . . ? C1 C2 H2 120(2) . . ? C3 C2 H2 120(2) . . ? C2 C3 C4 116.5(3) . . ? C2 C3 C6 121.5(3) . . ? C4 C3 C6 122.0(3) . . ? C5 C4 C3 119.8(3) . . ? C5 C4 H4 121(2) . . ? C3 C4 H4 119(2) . . ? N1 C5 C4 124.5(3) . . ? N1 C5 H5 116(2) . . ? C4 C5 H5 119(2) . . ? C3 C6 C7 112.5(3) . . ? C3 C6 H6A 116(3) . . ? C7 C6 H6A 103(3) . . ? C3 C6 H6B 108(2) . . ? C7 C6 H6B 107(2) . . ? H6A C6 H6B 109(3) . . ? C10 C7 C6 113.0(3) . . ? C10 C7 H7A 112(2) . . ? C6 C7 H7A 107(2) . . ? C10 C7 H7B 112(2) . . ? C6 C7 H7B 106(2) . . ? H7A C7 H7B 106(3) . . ? N2 C8 C9 123.2(4) . . ? N2 C8 H8 115(2) . . ? C9 C8 H8 121(2) . . ? C10 C9 C8 120.5(3) . . ? C10 C9 H9 123(3) . . ? C8 C9 H9 117(3) . . ? C9 C10 C11 116.0(3) . . ? C9 C10 C7 121.4(3) . . ? C11 C10 C7 122.7(3) . . ? C12 C11 C10 120.4(3) . . ? C12 C11 H11 122(2) . . ? C10 C11 H11 117(2) . . ? N2 C12 C11 123.5(4) . . ? N2 C12 H12 116(3) . . ? C11 C12 H12 121(3) . . ? C12 N2 C8 116.3(3) . . ? C12 N2 Co1 122.1(2) . 1_545 ? C8 N2 Co1 121.2(2) . 1_545 ? C14 N4 C18 115.3(4) . . ? N4 C14 C15 124.7(4) . . ? N4 C14 H14 120(3) . . ? C15 C14 H14 115(3) . . ? C14 C15 C16 119.6(4) . . ? C14 C15 H15 120(3) . . ? C16 C15 H15 121(3) . . ? C15 C16 C17 116.0(3) . . ? C15 C16 C19 121.9(3) . . ? C17 C16 C19 122.0(3) . . ? C18 C17 C16 119.9(4) . . ? C18 C17 H17 122(3) . . ? C16 C17 H17 118(3) . . ? N4 C18 C17 124.4(4) . . ? N4 C18 H18 116(3) . . ? C17 C18 H18 120(3) . . ? C16 C19 C19 111.8(4) . 5_575 ? C16 C19 H19A 109(2) . . ? C19 C19 H19A 107(2) 5_575 . ? C16 C19 H19B 109(2) . . ? C19 C19 H19B 109(2) 5_575 . ? H19A C19 H19B 109(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.357 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.054