Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'J.Chem.Soc.,Dalton Trans.' loop_ _publ_author_name 'Champeil, Elise' 'Draper, Sylvia M.' _publ_contact_author_name 'Dr Sylvia M Draper' _publ_contact_author_address ; Dr Sylvia M Draper Chemistry Department University of Dublin Trinity College Dublin 2 REPUBLIC OF IRELAND ; _publ_contact_author_email ? data_elise1 _database_code_CSD 151896 _audit_creation_method SHELXL _chemical_formula_sum 'C42 H32 Cl2 Co2 Fe O5 P2' _chemical_formula_weight 923.23 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' 'Cl' 'Cl' 0.1484 0.1585 '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 10.597(9) _cell_length_b 11.004(5) _cell_length_c 18.059(8) _cell_angle_alpha 74.86(4) _cell_angle_beta 88.66(5) _cell_angle_gamma 71.27(5) _cell_volume 1920.9(20) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 16 _cell_measurement_theta_max 18 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.596 _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.494 _exptl_absorpt_correction_type psiscan _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 6438 _diffrn_reflns_av_R_equivalents 0.0159 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 24.97 _reflns_number_total 6206 _reflns_number_observed 4904 _reflns_observed_criterion >2sigma(I) _computing_data_collection cad4 _computing_cell_refinement celdim _computing_data_reduction wingx _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ortex _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0676P)^2^+1.6698P] 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 varied _refine_ls_extinction_method none _refine_ls_number_reflns 6206 _refine_ls_number_parameters 494 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_obs 0.0373 _refine_ls_wR_factor_all 0.1079 _refine_ls_wR_factor_obs 0.0974 _refine_ls_goodness_of_fit_all 1.014 _refine_ls_goodness_of_fit_obs 1.040 _refine_ls_restrained_S_all 1.014 _refine_ls_restrained_S_obs 1.040 _refine_ls_shift/esd_max 0.148 _refine_ls_shift/esd_mean 0.006 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co2 Co 0.25483(4) 0.09314(4) 0.71833(3) 0.02547(13) Uani 1 d . . Co1 Co 0.33764(4) 0.08834(4) 0.84755(3) 0.02574(13) Uani 1 d . . Fe Fe 0.66156(4) 0.12240(5) 0.57427(3) 0.03073(15) Uani 1 d . . P2 P 0.46728(8) -0.09489(8) 0.82157(5) 0.0269(2) Uani 1 d . . P1 P 0.16609(8) 0.24465(8) 0.77794(5) 0.0251(2) Uani 1 d . . O13 O 0.4700(2) 0.2666(2) 0.76221(15) 0.0343(6) Uani 1 d . . O43 O 0.1317(3) 0.2323(3) 0.5651(2) 0.0557(8) Uani 1 d . . O42 O 0.0980(3) -0.0866(3) 0.7675(2) 0.0567(8) Uani 1 d . . O40 O 0.1676(3) -0.0377(3) 0.9509(2) 0.0688(10) Uani 1 d . . O41 O 0.4677(3) 0.1682(3) 0.9578(2) 0.0602(9) Uani 1 d . . C12 C 0.4493(3) -0.0264(3) 0.7198(2) 0.0269(7) Uani 1 d . . H12 H 0.4761(32) -0.0779(32) 0.6866(20) 0.018(8) Uiso 1 d . . C11 C 0.4463(3) 0.1086(3) 0.6983(2) 0.0264(7) Uani 1 d . . C10 C 0.4802(3) 0.1721(3) 0.6214(2) 0.0283(8) Uani 1 d . . C9 C 0.5256(3) 0.2852(3) 0.5993(2) 0.0340(8) Uani 1 d . . H9 H 0.5403(3) 0.3339(3) 0.6320(2) 0.056(5) Uiso 1 calc R . C8 C 0.5444(3) 0.3109(4) 0.5192(2) 0.0411(10) Uani 1 d . . H8 H 0.5740(3) 0.3794(4) 0.4898(2) 0.056(5) Uiso 1 calc R . C7 C 0.5112(4) 0.2164(4) 0.4915(2) 0.0442(10) Uani 1 d . . H7 H 0.5145(4) 0.2112(4) 0.4403(2) 0.056(5) Uiso 1 calc R . C6 C 0.4715(3) 0.1297(4) 0.5541(2) 0.0364(9) Uani 1 d . . H6 H 0.4445(3) 0.0574(4) 0.5514(2) 0.056(5) Uiso 1 calc R . C1 C 0.7816(4) -0.0637(4) 0.5747(3) 0.0508(11) Uani 1 d . . H1 H 0.7548(4) -0.1295(4) 0.5617(3) 0.056(5) Uiso 1 calc R . C5 C 0.7832(4) -0.0447(4) 0.6478(3) 0.0499(11) Uani 1 d . . H5 H 0.7575(4) -0.0944(4) 0.6927(3) 0.056(5) Uiso 1 calc R . C4 C 0.8305(4) 0.0629(5) 0.6417(4) 0.070(2) Uani 1 d . . H4 H 0.8421(4) 0.0987(5) 0.6820(4) 0.056(5) Uiso 1 calc R . C3 C 0.8576(4) 0.1077(5) 0.5641(4) 0.070(2) Uani 1 d . . H3 H 0.8912(4) 0.1780(5) 0.5435(4) 0.056(5) Uiso 1 calc R . C2 C 0.8256(4) 0.0293(5) 0.5245(3) 0.0602(13) Uani 1 d . . H2 H 0.8328(4) 0.0379(5) 0.4715(3) 0.072 Uiso 1 calc R . C13 C 0.4363(3) 0.1709(3) 0.7629(2) 0.0267(7) Uani 1 d . . C43 C 0.1836(3) 0.1757(4) 0.6242(2) 0.0346(8) Uani 1 d . . C42 C 0.1622(3) -0.0201(3) 0.7485(2) 0.0342(8) Uani 1 d . . C40 C 0.2341(4) 0.0097(4) 0.9119(2) 0.0381(9) Uani 1 d . . C41 C 0.4154(4) 0.1376(4) 0.9154(2) 0.0361(9) Uani 1 d . . C14 C 0.1502(3) 0.4189(3) 0.7336(2) 0.0286(8) Uani 1 d . . C15 C 0.2055(3) 0.4562(4) 0.6641(2) 0.0350(8) Uani 1 d . . H15 H 0.2572(3) 0.3905(4) 0.6412(2) 0.049(3) Uiso 1 calc R . C16 C 0.1848(4) 0.5896(4) 0.6284(2) 0.0428(9) Uani 1 d . . H16 H 0.2232(4) 0.6139(4) 0.5817(2) 0.049(3) Uiso 1 calc R . C17 C 0.1082(4) 0.6867(4) 0.6612(3) 0.0454(10) Uani 1 d . . H17 H 0.0927(4) 0.7771(4) 0.6363(3) 0.049(3) Uiso 1 calc R . C18 C 0.0546(4) 0.6512(4) 0.7302(3) 0.0423(10) Uani 1 d . . H18 H 0.0039(4) 0.7173(4) 0.7530(3) 0.049(3) Uiso 1 calc R . C19 C 0.0752(3) 0.5183(3) 0.7662(2) 0.0341(8) Uani 1 d . . H19 H 0.0380(3) 0.4949(3) 0.8134(2) 0.049(3) Uiso 1 calc R . C20 C 0.0020(3) 0.2607(3) 0.8161(2) 0.0295(8) Uani 1 d . . C21 C -0.0230(4) 0.2720(4) 0.8900(2) 0.0402(9) Uani 1 d . . H21 H 0.0466(4) 0.2686(4) 0.9226(2) 0.049(3) Uiso 1 calc R . C22 C -0.1506(4) 0.2885(4) 0.9164(3) 0.0517(11) Uani 1 d . . H22 H -0.1670(4) 0.2969(4) 0.9665(3) 0.049(3) Uiso 1 calc R . C23 C -0.2519(4) 0.2924(5) 0.8691(3) 0.0565(13) Uani 1 d . . H23 H -0.3379(4) 0.3033(5) 0.8868(3) 0.049(3) Uiso 1 calc R . C24 C -0.2276(4) 0.2805(4) 0.7963(3) 0.0542(12) Uani 1 d . . H24 H -0.2975(4) 0.2837(4) 0.7640(3) 0.049(3) Uiso 1 calc R . C25 C -0.1009(3) 0.2639(4) 0.7693(2) 0.0394(9) Uani 1 d . . H25 H -0.0853(3) 0.2548(4) 0.7193(2) 0.049(3) Uiso 1 calc R . C32 C 0.4217(3) -0.2463(3) 0.8417(2) 0.0303(8) Uani 1 d . . C33 C 0.3975(4) -0.3041(4) 0.9159(2) 0.0414(9) Uani 1 d . . H33 H 0.4016(4) -0.2636(4) 0.9552(2) 0.049(3) Uiso 1 calc R . C34 C 0.3674(4) -0.4212(4) 0.9325(3) 0.0498(11) Uani 1 d . . H34 H 0.3498(4) -0.4594(4) 0.9830(3) 0.049(3) Uiso 1 calc R . C35 C 0.3629(4) -0.4824(4) 0.8754(3) 0.0542(12) Uani 1 d . . H35 H 0.3426(4) -0.5622(4) 0.8868(3) 0.049(3) Uiso 1 calc R . C36 C 0.3880(4) -0.4263(4) 0.8025(3) 0.0535(12) Uani 1 d . . H36 H 0.3857(4) -0.4683(4) 0.7636(3) 0.049(3) Uiso 1 calc R . C37 C 0.4170(4) -0.3077(4) 0.7845(2) 0.0404(9) Uani 1 d . . H37 H 0.4333(4) -0.2694(4) 0.7338(2) 0.049(3) Uiso 1 calc R . C26 C 0.6435(3) -0.1588(4) 0.8560(2) 0.0321(8) Uani 1 d . . C27 C 0.7153(4) -0.2933(4) 0.8767(2) 0.0426(9) Uani 1 d . . H27 H 0.6739(4) -0.3556(4) 0.8731(2) 0.049(3) Uiso 1 calc R . C28 C 0.8492(4) -0.3364(5) 0.9028(3) 0.0560(12) Uani 1 d . . H28 H 0.8976(4) -0.4280(5) 0.9174(3) 0.049(3) Uiso 1 calc R . C29 C 0.9104(4) -0.2464(5) 0.9073(3) 0.0562(12) Uani 1 d . . H29 H 1.0008(4) -0.2763(5) 0.9249(3) 0.049(3) Uiso 1 calc R . C30 C 0.8406(4) -0.1126(5) 0.8861(3) 0.0530(11) Uani 1 d . . H30 H 0.8834(4) -0.0510(5) 0.8889(3) 0.049(3) Uiso 1 calc R . C31 C 0.7072(4) -0.0683(4) 0.8606(2) 0.0432(10) Uani 1 d . . H31 H 0.6596(4) 0.0234(4) 0.8464(2) 0.049(3) Uiso 1 calc R . Cl1 Cl 0.28480(14) 0.38195(14) 0.31853(8) 0.0761(4) Uani 1 d . . Cl2 Cl 0.2141(2) 0.5399(2) 0.42729(11) 0.1026(6) Uani 1 d . . C44 C 0.1765(6) 0.4262(6) 0.3886(4) 0.074(2) Uani 1 d . . H44A H 0.0846(6) 0.4648(6) 0.3657(4) 0.178(27) Uiso 1 calc R . H44B H 0.1821(6) 0.3460(6) 0.4298(4) 0.178(27) Uiso 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 Co2 0.0172(2) 0.0303(2) 0.0334(3) -0.0127(2) 0.0011(2) -0.0103(2) Co1 0.0193(2) 0.0290(2) 0.0313(3) -0.0108(2) 0.0011(2) -0.0089(2) Fe 0.0170(2) 0.0338(3) 0.0420(3) -0.0127(2) 0.0051(2) -0.0074(2) P2 0.0196(4) 0.0274(4) 0.0359(6) -0.0108(4) 0.0002(4) -0.0085(3) P1 0.0166(4) 0.0288(4) 0.0333(5) -0.0117(4) 0.0030(3) -0.0092(3) O13 0.0283(12) 0.0380(13) 0.046(2) -0.0172(12) 0.0046(11) -0.0186(11) O43 0.042(2) 0.077(2) 0.043(2) -0.010(2) -0.0107(15) -0.016(2) O42 0.038(2) 0.051(2) 0.090(2) -0.016(2) 0.005(2) -0.0289(14) O40 0.058(2) 0.059(2) 0.078(2) -0.001(2) 0.033(2) -0.021(2) O41 0.077(2) 0.066(2) 0.052(2) -0.023(2) -0.013(2) -0.036(2) C12 0.019(2) 0.033(2) 0.032(2) -0.016(2) 0.0037(14) -0.0083(13) C11 0.0140(14) 0.033(2) 0.035(2) -0.0124(15) 0.0031(13) -0.0080(13) C10 0.0154(15) 0.034(2) 0.036(2) -0.012(2) 0.0034(13) -0.0077(13) C9 0.026(2) 0.027(2) 0.046(3) -0.010(2) 0.009(2) -0.0055(14) C8 0.026(2) 0.034(2) 0.052(3) 0.000(2) 0.009(2) -0.0040(15) C7 0.029(2) 0.061(3) 0.034(2) -0.006(2) 0.003(2) -0.008(2) C6 0.023(2) 0.047(2) 0.038(2) -0.010(2) -0.001(2) -0.011(2) C1 0.037(2) 0.037(2) 0.073(4) -0.022(2) 0.004(2) 0.000(2) C5 0.024(2) 0.052(2) 0.055(3) -0.002(2) -0.001(2) 0.003(2) C4 0.030(2) 0.082(4) 0.100(5) -0.055(3) -0.027(3) 0.007(2) C3 0.021(2) 0.054(3) 0.129(5) -0.014(3) 0.012(3) -0.015(2) C2 0.037(2) 0.065(3) 0.066(3) -0.019(3) 0.023(2) 0.000(2) C13 0.0139(14) 0.028(2) 0.038(2) -0.0087(14) -0.0007(13) -0.0067(12) C43 0.020(2) 0.046(2) 0.042(3) -0.018(2) 0.003(2) -0.013(2) C42 0.023(2) 0.036(2) 0.046(2) -0.016(2) -0.002(2) -0.0086(15) C40 0.033(2) 0.035(2) 0.043(2) -0.009(2) 0.005(2) -0.008(2) C41 0.038(2) 0.036(2) 0.035(2) -0.008(2) 0.000(2) -0.015(2) C14 0.018(2) 0.033(2) 0.038(2) -0.0110(15) 0.0006(14) -0.0104(13) C15 0.026(2) 0.037(2) 0.043(2) -0.013(2) 0.008(2) -0.0114(15) C16 0.041(2) 0.042(2) 0.046(3) -0.006(2) 0.007(2) -0.018(2) C17 0.044(2) 0.030(2) 0.061(3) -0.005(2) 0.002(2) -0.015(2) C18 0.034(2) 0.035(2) 0.061(3) -0.018(2) 0.010(2) -0.011(2) C19 0.029(2) 0.036(2) 0.042(2) -0.017(2) 0.008(2) -0.0127(15) C20 0.018(2) 0.030(2) 0.041(2) -0.0080(15) 0.0038(14) -0.0093(13) C21 0.028(2) 0.047(2) 0.048(3) -0.016(2) 0.010(2) -0.013(2) C22 0.041(2) 0.059(3) 0.052(3) -0.013(2) 0.024(2) -0.015(2) C23 0.022(2) 0.065(3) 0.077(4) -0.009(2) 0.018(2) -0.015(2) C24 0.023(2) 0.065(3) 0.075(4) -0.011(2) -0.003(2) -0.022(2) C25 0.025(2) 0.050(2) 0.048(3) -0.015(2) 0.002(2) -0.016(2) C32 0.019(2) 0.027(2) 0.043(2) -0.007(2) -0.0015(14) -0.0073(13) C33 0.038(2) 0.037(2) 0.049(3) -0.011(2) 0.004(2) -0.013(2) C34 0.044(2) 0.040(2) 0.060(3) 0.001(2) 0.004(2) -0.018(2) C35 0.042(2) 0.034(2) 0.086(4) -0.006(2) -0.006(2) -0.020(2) C36 0.053(3) 0.035(2) 0.078(4) -0.022(2) -0.012(2) -0.016(2) C37 0.040(2) 0.038(2) 0.046(3) -0.015(2) -0.003(2) -0.014(2) C26 0.021(2) 0.042(2) 0.033(2) -0.013(2) 0.0025(14) -0.0088(15) C27 0.031(2) 0.041(2) 0.052(3) -0.014(2) 0.003(2) -0.005(2) C28 0.029(2) 0.061(3) 0.063(3) -0.018(2) -0.003(2) 0.006(2) C29 0.020(2) 0.087(4) 0.056(3) -0.025(2) -0.005(2) -0.005(2) C30 0.027(2) 0.074(3) 0.068(3) -0.031(2) -0.002(2) -0.020(2) C31 0.027(2) 0.049(2) 0.056(3) -0.018(2) -0.005(2) -0.011(2) Cl1 0.0708(8) 0.0751(9) 0.0711(9) -0.0172(7) 0.0060(7) -0.0105(7) Cl2 0.1173(14) 0.0900(11) 0.0991(13) -0.0458(9) -0.0354(10) -0.0126(10) C44 0.075(4) 0.072(3) 0.089(4) -0.037(3) 0.021(3) -0.031(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 Co2 C43 1.759(4) . ? Co2 C42 1.795(4) . ? Co2 C12 2.054(4) . ? Co2 C11 2.105(3) . ? Co2 P1 2.1694(15) . ? Co2 Co1 2.4940(14) . ? Co2 P2 2.831(3) . ? Co1 C41 1.776(4) . ? Co1 C40 1.824(4) . ? Co1 C13 2.016(4) . ? Co1 P1 2.194(2) . ? Co1 P2 2.204(2) . ? Fe C4 2.013(5) . ? Fe C7 2.022(4) . ? Fe C5 2.022(4) . ? Fe C6 2.028(4) . ? Fe C1 2.033(4) . ? Fe C2 2.036(4) . ? Fe C3 2.039(4) . ? Fe C8 2.040(4) . ? Fe C10 2.051(4) . ? Fe C9 2.055(4) . ? P2 C12 1.784(4) . ? P2 C32 1.826(3) . ? P2 C26 1.831(4) . ? P1 C20 1.828(4) . ? P1 C14 1.829(4) . ? O13 C13 1.213(4) . ? O43 C43 1.136(5) . ? O42 C42 1.136(4) . ? O40 C40 1.133(5) . ? O41 C41 1.133(5) . ? C12 C11 1.424(5) . ? C12 H12 0.91(3) . ? C11 C10 1.475(5) . ? C11 C13 1.486(5) . ? C10 C6 1.426(5) . ? C10 C9 1.434(5) . ? C9 C8 1.421(6) . ? C9 H9 0.94 . ? C8 C7 1.403(6) . ? C8 H8 0.94 . ? C7 C6 1.427(5) . ? C7 H7 0.94 . ? C6 H6 0.94 . ? C1 C2 1.374(7) . ? C1 C5 1.390(7) . ? C1 H1 0.94 . ? C5 C4 1.407(7) . ? C5 H5 0.94 . ? C4 C3 1.414(8) . ? C4 H4 0.94 . ? C3 C2 1.376(7) . ? C3 H3 0.94 . ? C2 H2 0.94 . ? C14 C19 1.389(5) . ? C14 C15 1.392(5) . ? C15 C16 1.388(5) . ? C15 H15 0.94 . ? C16 C17 1.379(6) . ? C16 H16 0.94 . ? C17 C18 1.372(6) . ? C17 H17 0.94 . ? C18 C19 1.384(5) . ? C18 H18 0.94 . ? C19 H19 0.94 . ? C20 C25 1.381(5) . ? C20 C21 1.383(6) . ? C21 C22 1.395(5) . ? C21 H21 0.94 . ? C22 C23 1.370(7) . ? C22 H22 0.94 . ? C23 C24 1.365(7) . ? C23 H23 0.94 . ? C24 C25 1.390(5) . ? C24 H24 0.94 . ? C25 H25 0.94 . ? C32 C33 1.381(5) . ? C32 C37 1.383(5) . ? C33 C34 1.383(5) . ? C33 H33 0.94 . ? C34 C35 1.380(7) . ? C34 H34 0.94 . ? C35 C36 1.360(7) . ? C35 H35 0.94 . ? C36 C37 1.391(5) . ? C36 H36 0.94 . ? C37 H37 0.94 . ? C26 C27 1.382(5) . ? C26 C31 1.390(5) . ? C27 C28 1.393(6) . ? C27 H27 0.94 . ? C28 C29 1.366(7) . ? C28 H28 0.94 . ? C29 C30 1.371(7) . ? C29 H29 0.94 . ? C30 C31 1.385(5) . ? C30 H30 0.94 . ? C31 H31 0.94 . ? Cl1 C44 1.746(6) . ? Cl2 C44 1.733(6) . ? C44 H44A 0.98 . ? C44 H44B 0.98 . ? 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 C43 Co2 C42 100.8(2) . . ? C43 Co2 C12 112.2(2) . . ? C42 Co2 C12 104.9(2) . . ? C43 Co2 C11 96.9(2) . . ? C42 Co2 C11 144.90(14) . . ? C12 Co2 C11 40.02(13) . . ? C43 Co2 P1 101.31(13) . . ? C42 Co2 P1 102.86(13) . . ? C12 Co2 P1 130.77(11) . . ? C11 Co2 P1 103.05(10) . . ? C43 Co2 Co1 152.86(12) . . ? C42 Co2 Co1 98.58(13) . . ? C12 Co2 Co1 80.53(12) . . ? C11 Co2 Co1 77.34(11) . . ? P1 Co2 Co1 55.60(5) . . ? C43 Co2 P2 150.86(12) . . ? C42 Co2 P2 87.52(13) . . ? C12 Co2 P2 38.91(11) . . ? C11 Co2 P2 63.46(11) . . ? P1 Co2 P2 103.98(6) . . ? Co1 Co2 P2 48.39(4) . . ? C41 Co1 C40 98.7(2) . . ? C41 Co1 C13 90.3(2) . . ? C40 Co1 C13 170.9(2) . . ? C41 Co1 P1 115.40(13) . . ? C40 Co1 P1 93.82(13) . . ? C13 Co1 P1 81.15(11) . . ? C41 Co1 P2 112.69(13) . . ? C40 Co1 P2 96.23(13) . . ? C13 Co1 P2 81.21(11) . . ? P1 Co1 P2 128.49(6) . . ? C41 Co1 Co2 156.93(12) . . ? C40 Co1 Co2 102.58(14) . . ? C13 Co1 Co2 68.29(10) . . ? P1 Co1 Co2 54.68(5) . . ? P2 Co1 Co2 73.82(6) . . ? C4 Fe C7 165.8(2) . . ? C4 Fe C5 40.8(2) . . ? C7 Fe C5 151.4(2) . . ? C4 Fe C6 152.5(2) . . ? C7 Fe C6 41.3(2) . . ? C5 Fe C6 117.2(2) . . ? C4 Fe C1 67.5(2) . . ? C7 Fe C1 118.0(2) . . ? C5 Fe C1 40.1(2) . . ? C6 Fe C1 106.8(2) . . ? C4 Fe C2 67.4(2) . . ? C7 Fe C2 107.8(2) . . ? C5 Fe C2 67.4(2) . . ? C6 Fe C2 126.3(2) . . ? C1 Fe C2 39.5(2) . . ? C4 Fe C3 40.9(2) . . ? C7 Fe C3 127.0(2) . . ? C5 Fe C3 68.2(2) . . ? C6 Fe C3 163.8(2) . . ? C1 Fe C3 66.8(2) . . ? C2 Fe C3 39.5(2) . . ? C4 Fe C8 129.0(2) . . ? C7 Fe C8 40.4(2) . . ? C5 Fe C8 166.8(2) . . ? C6 Fe C8 68.8(2) . . ? C1 Fe C8 152.1(2) . . ? C2 Fe C8 119.7(2) . . ? C3 Fe C8 109.5(2) . . ? C4 Fe C10 119.5(2) . . ? C7 Fe C10 68.9(2) . . ? C5 Fe C10 107.5(2) . . ? C6 Fe C10 40.9(2) . . ? C1 Fe C10 126.9(2) . . ? C2 Fe C10 163.8(2) . . ? C3 Fe C10 154.8(2) . . ? C8 Fe C10 68.76(15) . . ? C4 Fe C9 109.8(2) . . ? C7 Fe C9 68.3(2) . . ? C5 Fe C9 128.5(2) . . ? C6 Fe C9 68.7(2) . . ? C1 Fe C9 165.5(2) . . ? C2 Fe C9 154.1(2) . . ? C3 Fe C9 121.2(2) . . ? C8 Fe C9 40.6(2) . . ? C10 Fe C9 40.87(14) . . ? C12 P2 C32 107.1(2) . . ? C12 P2 C26 110.7(2) . . ? C32 P2 C26 102.5(2) . . ? C12 P2 Co1 95.20(13) . . ? C32 P2 Co1 121.99(12) . . ? C26 P2 Co1 118.59(13) . . ? C12 P2 Co2 46.31(11) . . ? C32 P2 Co2 102.80(12) . . ? C26 P2 Co2 150.36(13) . . ? Co1 P2 Co2 57.79(5) . . ? C20 P1 C14 101.4(2) . . ? C20 P1 Co2 119.92(12) . . ? C14 P1 Co2 120.74(13) . . ? C20 P1 Co1 116.80(13) . . ? C14 P1 Co1 127.62(11) . . ? Co2 P1 Co1 69.72(5) . . ? C11 C12 P2 112.0(3) . . ? C11 C12 Co2 71.9(2) . . ? P2 C12 Co2 94.8(2) . . ? C11 C12 H12 120.3(21) . . ? P2 C12 H12 122.3(21) . . ? Co2 C12 H12 122.2(20) . . ? C12 C11 C10 122.2(3) . . ? C12 C11 C13 115.0(3) . . ? C10 C11 C13 121.5(3) . . ? C12 C11 Co2 68.1(2) . . ? C10 C11 Co2 121.6(2) . . ? C13 C11 Co2 89.3(2) . . ? C6 C10 C9 107.3(3) . . ? C6 C10 C11 124.6(3) . . ? C9 C10 C11 128.1(3) . . ? C6 C10 Fe 68.7(2) . . ? C9 C10 Fe 69.7(2) . . ? C11 C10 Fe 127.2(2) . . ? C8 C9 C10 108.0(3) . . ? C8 C9 Fe 69.1(2) . . ? C10 C9 Fe 69.4(2) . . ? C8 C9 H9 126.0(2) . . ? C10 C9 H9 126.0(2) . . ? Fe C9 H9 127.08(12) . . ? C7 C8 C9 108.3(3) . . ? C7 C8 Fe 69.1(2) . . ? C9 C8 Fe 70.3(2) . . ? C7 C8 H8 125.9(2) . . ? C9 C8 H8 125.8(2) . . ? Fe C8 H8 126.32(11) . . ? C8 C7 C6 108.6(4) . . ? C8 C7 Fe 70.5(2) . . ? C6 C7 Fe 69.6(2) . . ? C8 C7 H7 125.7(2) . . ? C6 C7 H7 125.7(2) . . ? Fe C7 H7 125.82(13) . . ? C10 C6 C7 107.8(3) . . ? C10 C6 Fe 70.4(2) . . ? C7 C6 Fe 69.2(2) . . ? C10 C6 H6 126.1(2) . . ? C7 C6 H6 126.1(2) . . ? Fe C6 H6 125.90(12) . . ? C2 C1 C5 109.0(4) . . ? C2 C1 Fe 70.4(2) . . ? C5 C1 Fe 69.5(2) . . ? C2 C1 H1 125.5(3) . . ? C5 C1 H1 125.5(3) . . ? Fe C1 H1 126.14(14) . . ? C1 C5 C4 106.9(5) . . ? C1 C5 Fe 70.4(2) . . ? C4 C5 Fe 69.2(3) . . ? C1 C5 H5 126.5(3) . . ? C4 C5 H5 126.5(3) . . ? Fe C5 H5 125.45(13) . . ? C5 C4 C3 107.7(4) . . ? C5 C4 Fe 70.0(2) . . ? C3 C4 Fe 70.6(3) . . ? C5 C4 H4 126.2(3) . . ? C3 C4 H4 126.2(3) . . ? Fe C4 H4 124.93(15) . . ? C2 C3 C4 107.3(4) . . ? C2 C3 Fe 70.1(2) . . ? C4 C3 Fe 68.6(2) . . ? C2 C3 H3 126.4(3) . . ? C4 C3 H3 126.4(3) . . ? Fe C3 H3 126.46(15) . . ? C1 C2 C3 109.1(5) . . ? C1 C2 Fe 70.1(2) . . ? C3 C2 Fe 70.4(3) . . ? C1 C2 H2 125.4(3) . . ? C3 C2 H2 125.4(3) . . ? Fe C2 H2 125.7(2) . . ? O13 C13 C11 125.2(3) . . ? O13 C13 Co1 124.1(3) . . ? C11 C13 Co1 110.3(2) . . ? O43 C43 Co2 176.4(3) . . ? O42 C42 Co2 176.6(3) . . ? O40 C40 Co1 178.6(4) . . ? O41 C41 Co1 178.4(4) . . ? C19 C14 C15 118.4(3) . . ? C19 C14 P1 120.5(3) . . ? C15 C14 P1 121.0(3) . . ? C16 C15 C14 120.4(3) . . ? C16 C15 H15 119.8(2) . . ? C14 C15 H15 119.8(2) . . ? C17 C16 C15 120.2(4) . . ? C17 C16 H16 119.9(2) . . ? C15 C16 H16 119.9(2) . . ? C18 C17 C16 120.0(4) . . ? C18 C17 H17 120.0(2) . . ? C16 C17 H17 120.0(2) . . ? C17 C18 C19 120.1(4) . . ? C17 C18 H18 120.0(2) . . ? C19 C18 H18 119.9(2) . . ? C18 C19 C14 120.9(4) . . ? C18 C19 H19 119.5(2) . . ? C14 C19 H19 119.5(2) . . ? C25 C20 C21 118.9(3) . . ? C25 C20 P1 119.0(3) . . ? C21 C20 P1 122.1(3) . . ? C20 C21 C22 120.6(4) . . ? C20 C21 H21 119.7(2) . . ? C22 C21 H21 119.7(3) . . ? C23 C22 C21 119.8(4) . . ? C23 C22 H22 120.1(3) . . ? C21 C22 H22 120.1(3) . . ? C24 C23 C22 119.9(4) . . ? C24 C23 H23 120.1(2) . . ? C22 C23 H23 120.1(3) . . ? C23 C24 C25 120.9(4) . . ? C23 C24 H24 119.6(2) . . ? C25 C24 H24 119.6(3) . . ? C20 C25 C24 119.9(4) . . ? C20 C25 H25 120.0(2) . . ? C24 C25 H25 120.0(3) . . ? C33 C32 C37 119.4(3) . . ? C33 C32 P2 119.6(3) . . ? C37 C32 P2 121.0(3) . . ? C32 C33 C34 120.2(4) . . ? C32 C33 H33 119.9(2) . . ? C34 C33 H33 119.9(3) . . ? C35 C34 C33 120.4(4) . . ? C35 C34 H34 119.8(2) . . ? C33 C34 H34 119.8(3) . . ? C36 C35 C34 119.5(4) . . ? C36 C35 H35 120.3(2) . . ? C34 C35 H35 120.3(3) . . ? C35 C36 C37 121.0(4) . . ? C35 C36 H36 119.5(2) . . ? C37 C36 H36 119.5(3) . . ? C32 C37 C36 119.6(4) . . ? C32 C37 H37 120.2(2) . . ? C36 C37 H37 120.2(3) . . ? C27 C26 C31 119.1(3) . . ? C27 C26 P2 122.3(3) . . ? C31 C26 P2 118.6(3) . . ? C26 C27 C28 119.9(4) . . ? C26 C27 H27 120.0(2) . . ? C28 C27 H27 120.0(3) . . ? C29 C28 C27 120.4(4) . . ? C29 C28 H28 119.8(3) . . ? C27 C28 H28 119.8(3) . . ? C28 C29 C30 120.3(4) . . ? C28 C29 H29 119.9(3) . . ? C30 C29 H29 119.9(2) . . ? C29 C30 C31 120.0(4) . . ? C29 C30 H30 120.0(2) . . ? C31 C30 H30 120.0(3) . . ? C30 C31 C26 120.3(4) . . ? C30 C31 H31 119.8(3) . . ? C26 C31 H31 119.8(2) . . ? Cl2 C44 Cl1 112.0(3) . . ? Cl2 C44 H44A 109.2(2) . . ? Cl1 C44 H44A 109.2(2) . . ? Cl2 C44 H44B 109.2(2) . . ? Cl1 C44 H44B 109.2(2) . . ? H44A C44 H44B 107.9 . . ? _refine_diff_density_max 0.710 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.082 #===END data_ec2 _database_code_CSD 151897 _audit_creation_method SHELXL _chemical_formula_sum 'C18 H9 Co2 Fe O6' _chemical_formula_weight 494.96 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' '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' 'Fe' 'Fe' 0.3463 0.8444 '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 9.064(9) _cell_length_b 9.311(4) _cell_length_c 11.823(16) _cell_angle_alpha 81.84(12) _cell_angle_beta 88.05(17) _cell_angle_gamma 65.13(7) _cell_volume 895.7(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14 _cell_measurement_theta_max 18 _exptl_crystal_description prisms _exptl_crystal_colour dark red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.835 _exptl_crystal_F_000 490 _exptl_absorpt_coefficient_mu 2.661 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 3289 _diffrn_reflns_av_R_equivalents 0.1057 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 24.96 _diffrn_standards_number 6 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% <0.1 _reflns_number_total 3081 _reflns_number_observed 2125 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ortex _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1419P)^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 fixed _refine_ls_extinction_method none _refine_ls_number_reflns 3081 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1398 _refine_ls_R_factor_obs 0.0987 _refine_ls_wR_factor_all 0.2455 _refine_ls_wR_factor_obs 0.2230 _refine_ls_goodness_of_fit_all 1.253 _refine_ls_goodness_of_fit_obs 1.391 _refine_ls_restrained_S_all 1.253 _refine_ls_restrained_S_obs 1.391 _refine_ls_shift/esd_max 0.043 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co2 Co 0.4585(2) 0.79119(15) 0.14123(11) 0.0451(4) Uani 1 d . . Co1 Co 0.72769(14) 0.72834(14) 0.05601(11) 0.0433(4) Uani 1 d . . Fe Fe 0.7959(2) 0.8968(2) 0.37454(12) 0.0483(5) Uani 1 d . . C1 C 1.0103(18) 0.7028(18) 0.3684(12) 0.093(5) Uani 1 d . . H1 H 1.0719(18) 0.6782(18) 0.3036(12) 0.111 Uiso 1 calc R . C2 C 1.0229(16) 0.7962(17) 0.4466(14) 0.084(4) Uani 1 d . . H2 H 1.0943(16) 0.8448(17) 0.4428(14) 0.101 Uiso 1 calc R . C3 C 0.9148(18) 0.8037(14) 0.5279(11) 0.074(4) Uani 1 d . . H3 H 0.8986(18) 0.8592(14) 0.5900(11) 0.089 Uiso 1 calc R . C4 C 0.8311(16) 0.7167(15) 0.5056(12) 0.084(4) Uani 1 d . . H4 H 0.7501(16) 0.7024(15) 0.5495(12) 0.101 Uiso 1 calc R . C5 C 0.8915(21) 0.6535(14) 0.4035(14) 0.091(5) Uani 1 d . . H5 H 0.8572(21) 0.5903(14) 0.3669(14) 0.110 Uiso 1 calc R . C6 C 0.7531(12) 1.0467(11) 0.2237(8) 0.047(2) Uani 1 d . . H6 H 0.8266(12) 1.0362(11) 0.1652(8) 0.056 Uiso 1 calc R . C7 C 0.7365(14) 1.1325(12) 0.3165(9) 0.058(3) Uani 1 d . . H7 H 0.7963(14) 1.1894(12) 0.3289(9) 0.069 Uiso 1 calc R . C8 C 0.6146(14) 1.1171(12) 0.3865(9) 0.060(3) Uani 1 d . . H8 H 0.5795(14) 1.1612(12) 0.4536(9) 0.072 Uiso 1 calc R . C9 C 0.5550(12) 1.0221(11) 0.3362(8) 0.050(2) Uani 1 d . . H9 H 0.4736(12) 0.9925(11) 0.3653(8) 0.060 Uiso 1 calc R . C10 C 0.6387(11) 0.9797(10) 0.2351(7) 0.043(2) Uani 1 d . . C11 C 0.6018(10) 0.8969(10) 0.1509(7) 0.039(2) Uani 1 d . . C12 C 0.5385(10) 0.9346(10) 0.0459(7) 0.036(2) Uani 1 d . . C30 C 0.8992(13) 0.7772(13) 0.0406(10) 0.060(3) Uani 1 d . . C31 C 0.7101(13) 0.6707(12) -0.0851(10) 0.057(3) Uani 1 d . . C32 C 0.8251(13) 0.5351(13) 0.1417(10) 0.059(3) Uani 1 d . . C34 C 0.3861(12) 0.7036(11) 0.0387(9) 0.051(2) Uani 1 d . . C33 C 0.2690(14) 0.9360(13) 0.1834(9) 0.057(3) Uani 1 d . . C35 C 0.5133(14) 0.6458(15) 0.2719(11) 0.071(3) Uani 1 d . . O30 O 1.0061(10) 0.8110(12) 0.0347(9) 0.096(3) Uani 1 d . . O31 O 0.7036(13) 0.6391(12) -0.1700(8) 0.092(3) Uani 1 d . . O32 O 0.8904(11) 0.4122(9) 0.1945(8) 0.086(3) Uani 1 d . . 034 O 0.3484(9) 0.6501(9) -0.0269(8) 0.073(2) Uani 1 d . . O33 O 0.1519(10) 1.0287(11) 0.2124(8) 0.084(3) Uani 1 d . . O35 O 0.5409(15) 0.5624(14) 0.3541(10) 0.127(4) Uani 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 Co2 0.0447(8) 0.0423(7) 0.0504(8) -0.0008(5) -0.0025(6) -0.0217(6) Co1 0.0388(7) 0.0389(7) 0.0484(8) -0.0063(5) -0.0039(5) -0.0123(5) Fe 0.0542(9) 0.0430(8) 0.0422(8) -0.0010(6) -0.0159(6) -0.0155(6) C1 0.083(10) 0.086(10) 0.061(8) -0.019(7) -0.020(7) 0.015(8) C2 0.059(8) 0.080(9) 0.099(11) 0.015(8) -0.037(8) -0.022(7) C3 0.094(10) 0.061(7) 0.057(7) -0.006(6) -0.033(7) -0.020(7) C4 0.072(8) 0.066(8) 0.075(9) 0.038(7) -0.011(7) -0.006(7) C5 0.119(12) 0.040(6) 0.104(12) 0.009(7) -0.061(10) -0.024(7) C6 0.050(5) 0.052(6) 0.045(5) 0.002(4) -0.011(4) -0.028(5) C7 0.072(7) 0.045(6) 0.057(6) 0.002(5) -0.023(6) -0.025(5) C8 0.084(8) 0.047(6) 0.038(5) -0.007(4) -0.013(5) -0.016(6) C9 0.052(6) 0.047(5) 0.046(6) 0.000(4) 0.000(4) -0.017(5) C10 0.044(5) 0.038(5) 0.038(5) 0.002(4) -0.014(4) -0.011(4) C11 0.035(4) 0.034(4) 0.043(5) -0.003(4) -0.005(4) -0.012(4) C12 0.030(4) 0.035(4) 0.042(5) -0.003(4) 0.000(4) -0.013(4) C30 0.045(6) 0.058(6) 0.071(7) -0.021(5) 0.000(5) -0.011(5) C31 0.053(6) 0.047(6) 0.064(7) -0.011(5) -0.008(5) -0.013(5) C32 0.056(6) 0.046(6) 0.069(7) -0.008(5) -0.009(5) -0.015(5) C34 0.048(6) 0.036(5) 0.069(7) 0.000(5) -0.002(5) -0.019(4) C33 0.060(7) 0.068(7) 0.057(7) -0.012(5) 0.011(5) -0.039(6) C35 0.056(7) 0.068(7) 0.079(9) 0.015(6) -0.008(6) -0.023(6) O30 0.057(5) 0.114(8) 0.140(9) -0.044(7) 0.019(5) -0.051(6) O31 0.116(8) 0.096(7) 0.058(5) -0.029(5) -0.007(5) -0.033(6) O32 0.097(7) 0.049(5) 0.089(6) 0.009(4) -0.020(5) -0.013(5) 034 0.065(5) 0.060(5) 0.101(6) -0.024(4) -0.019(4) -0.029(4) O33 0.058(5) 0.091(6) 0.094(7) -0.028(5) 0.020(5) -0.019(5) O35 0.136(10) 0.125(9) 0.100(8) 0.052(7) -0.008(7) -0.057(8) _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 Co2 C33 1.789(12) . ? Co2 C34 1.831(11) . ? Co2 C35 1.832(12) . ? Co2 C11 1.946(9) . ? Co2 C12 1.977(9) . ? Co2 Co1 2.471(4) . ? Co1 C30 1.791(12) . ? Co1 C32 1.803(11) . ? Co1 C31 1.855(12) . ? Co1 C12 1.955(8) . ? Co1 C11 1.983(9) . ? Fe C3 2.025(12) . ? Fe C2 2.027(12) . ? Fe C9 2.027(10) . ? Fe C1 2.030(12) . ? Fe C5 2.037(12) . ? Fe C8 2.039(11) . ? Fe C4 2.039(12) . ? Fe C6 2.041(10) . ? Fe C7 2.044(10) . ? Fe C10 2.053(9) . ? C1 C5 1.37(2) . ? C1 C2 1.39(2) . ? C2 C3 1.34(2) . ? C3 C4 1.37(2) . ? C4 C5 1.41(2) . ? C6 C10 1.411(13) . ? C6 C7 1.415(14) . ? C7 C8 1.40(2) . ? C8 C9 1.415(14) . ? C9 C10 1.407(13) . ? C10 C11 1.468(12) . ? C11 C12 1.322(12) . ? C12 C12 1.45(2) 2_675 ? C30 O30 1.135(13) . ? C31 O31 1.096(12) . ? C32 O32 1.141(13) . ? C34 034 1.113(12) . ? C33 O33 1.130(12) . ? C35 O35 1.118(14) . ? 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 C33 Co2 C34 100.4(5) . . ? C33 Co2 C35 99.3(5) . . ? C34 Co2 C35 105.4(5) . . ? C33 Co2 C11 101.8(4) . . ? C34 Co2 C11 140.6(4) . . ? C35 Co2 C11 102.6(5) . . ? C33 Co2 C12 99.8(4) . . ? C34 Co2 C12 104.8(4) . . ? C35 Co2 C12 140.4(5) . . ? C11 Co2 C12 39.4(3) . . ? C33 Co2 Co1 149.5(3) . . ? C34 Co2 Co1 95.6(3) . . ? C35 Co2 Co1 101.3(4) . . ? C11 Co2 Co1 51.7(3) . . ? C12 Co2 Co1 50.7(2) . . ? C30 Co1 C32 98.5(5) . . ? C30 Co1 C31 103.1(5) . . ? C32 Co1 C31 101.2(5) . . ? C30 Co1 C12 104.8(4) . . ? C32 Co1 C12 143.6(5) . . ? C31 Co1 C12 100.3(4) . . ? C30 Co1 C11 95.8(4) . . ? C32 Co1 C11 111.6(4) . . ? C31 Co1 C11 139.1(4) . . ? C12 Co1 C11 39.2(3) . . ? C30 Co1 Co2 146.1(3) . . ? C32 Co1 Co2 94.5(4) . . ? C31 Co1 Co2 104.9(4) . . ? C12 Co1 Co2 51.5(3) . . ? C11 Co1 Co2 50.4(3) . . ? C3 Fe C2 38.5(6) . . ? C3 Fe C9 130.3(5) . . ? C2 Fe C9 166.5(6) . . ? C3 Fe C1 66.1(6) . . ? C2 Fe C1 40.2(6) . . ? C9 Fe C1 151.8(6) . . ? C3 Fe C5 66.9(5) . . ? C2 Fe C5 66.8(6) . . ? C9 Fe C5 119.3(6) . . ? C1 Fe C5 39.3(6) . . ? C3 Fe C8 109.1(5) . . ? C2 Fe C8 128.4(6) . . ? C9 Fe C8 40.7(4) . . ? C1 Fe C8 166.7(6) . . ? C5 Fe C8 152.1(7) . . ? C3 Fe C4 39.5(6) . . ? C2 Fe C4 66.0(6) . . ? C9 Fe C4 110.0(5) . . ? C1 Fe C4 66.6(6) . . ? C5 Fe C4 40.5(6) . . ? C8 Fe C4 118.4(5) . . ? C3 Fe C6 150.6(5) . . ? C2 Fe C6 118.8(6) . . ? C9 Fe C6 67.8(4) . . ? C1 Fe C6 109.5(6) . . ? C5 Fe C6 129.5(6) . . ? C8 Fe C6 68.1(4) . . ? C4 Fe C6 168.2(6) . . ? C3 Fe C7 118.0(5) . . ? C2 Fe C7 108.9(5) . . ? C9 Fe C7 67.7(4) . . ? C1 Fe C7 129.7(7) . . ? C5 Fe C7 167.1(7) . . ? C8 Fe C7 40.1(5) . . ? C4 Fe C7 150.5(6) . . ? C6 Fe C7 40.5(4) . . ? C3 Fe C10 168.2(5) . . ? C2 Fe C10 152.0(6) . . ? C9 Fe C10 40.3(4) . . ? C1 Fe C10 119.0(5) . . ? C5 Fe C10 109.6(5) . . ? C8 Fe C10 68.3(4) . . ? C4 Fe C10 130.6(5) . . ? C6 Fe C10 40.3(4) . . ? C7 Fe C10 67.9(4) . . ? C5 C1 C2 108.2(13) . . ? C5 C1 Fe 70.6(8) . . ? C2 C1 Fe 69.8(7) . . ? C3 C2 C1 108.2(13) . . ? C3 C2 Fe 70.7(7) . . ? C1 C2 Fe 70.0(7) . . ? C2 C3 C4 109.6(13) . . ? C2 C3 Fe 70.8(7) . . ? C4 C3 Fe 70.8(7) . . ? C3 C4 C5 107.0(14) . . ? C3 C4 Fe 69.7(7) . . ? C5 C4 Fe 69.7(7) . . ? C1 C5 C4 106.9(13) . . ? C1 C5 Fe 70.0(7) . . ? C4 C5 Fe 69.8(7) . . ? C10 C6 C7 108.2(9) . . ? C10 C6 Fe 70.3(5) . . ? C7 C6 Fe 69.9(6) . . ? C8 C7 C6 108.3(9) . . ? C8 C7 Fe 69.7(6) . . ? C6 C7 Fe 69.6(6) . . ? C7 C8 C9 107.3(9) . . ? C7 C8 Fe 70.1(6) . . ? C9 C8 Fe 69.2(6) . . ? C10 C9 C8 109.0(9) . . ? C10 C9 Fe 70.8(6) . . ? C8 C9 Fe 70.1(6) . . ? C9 C10 C6 107.2(8) . . ? C9 C10 C11 126.3(9) . . ? C6 C10 C11 126.2(8) . . ? C9 C10 Fe 68.8(5) . . ? C6 C10 Fe 69.4(5) . . ? C11 C10 Fe 131.9(6) . . ? C12 C11 C10 136.7(8) . . ? C12 C11 Co2 71.6(5) . . ? C10 C11 Co2 136.3(7) . . ? C12 C11 Co1 69.2(5) . . ? C10 C11 Co1 136.6(6) . . ? Co2 C11 Co1 78.0(3) . . ? C11 C12 C12 144.3(11) . 2_675 ? C11 C12 Co1 71.5(5) . . ? C12 C12 Co1 134.0(9) 2_675 . ? C11 C12 Co2 69.0(5) . . ? C12 C12 Co2 132.0(8) 2_675 . ? Co1 C12 Co2 77.9(3) . . ? O30 C30 Co1 177.3(10) . . ? O31 C31 Co1 177.4(11) . . ? O32 C32 Co1 178.2(11) . . ? 034 C34 Co2 176.5(10) . . ? O33 C33 Co2 177.9(10) . . ? O35 C35 Co2 176.6(13) . . ? _refine_diff_density_max 3.254 _refine_diff_density_min -1.451 _refine_diff_density_rms 0.549 #===END data_ec3s _database_code_CSD 151898 _audit_creation_method SHELXL _chemical_formula_sum 'C30 H18 Co2 Fe2 O6' _chemical_formula_weight 704.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M p212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.6378(7) _cell_length_b 11.5265(7) _cell_length_c 22.328(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2737.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _exptl_crystal_description prism _exptl_crystal_colour dark red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.708 _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 2.272 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 2176 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 24.96 _diffrn_standards_number 6 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% <0.1 _reflns_number_total 2176 _reflns_number_observed 1860 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ortex _refine_special_details ; Refinement on F^2^ for ALL reflections except for 12 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+8.1523P] 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 fixed _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.14(7) _refine_ls_number_reflns 2164 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_obs 0.0467 _refine_ls_wR_factor_all 0.1872 _refine_ls_wR_factor_obs 0.1292 _refine_ls_goodness_of_fit_all 1.216 _refine_ls_goodness_of_fit_obs 1.214 _refine_ls_restrained_S_all 1.612 _refine_ls_restrained_S_obs 1.214 _refine_ls_shift/esd_max -0.051 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co2 Co 0.0854(2) 0.61918(15) 0.61645(7) 0.0385(5) Uani 1 d . . Co1 Co 0.0196(2) 0.66443(13) 0.51283(7) 0.0366(5) Uani 1 d . . Fe2 Fe -0.1175(2) 0.27562(15) 0.58725(8) 0.0399(5) Uani 1 d . . Fe1 Fe -0.4021(2) 0.6941(2) 0.75611(8) 0.0458(6) Uani 1 d . . O31 O 0.0458(14) 0.9178(10) 0.5171(6) 0.090(4) Uani 1 d . . O32 O -0.1755(12) 0.6309(11) 0.4228(5) 0.076(4) Uani 1 d . . O30 O 0.2433(12) 0.5889(12) 0.4457(5) 0.081(4) Uani 1 d . . O34 O 0.0897(16) 0.8569(10) 0.6655(6) 0.107(5) Uani 1 d . . O35 O 0.0405(13) 0.4965(10) 0.7283(4) 0.080(4) Uani 1 d . . O33 O 0.3412(13) 0.5414(11) 0.5852(5) 0.072(3) Uani 1 d . . C11 C -0.0104(13) 0.5251(9) 0.5614(5) 0.030(3) Uani 1 d . . C12 C -0.0821(13) 0.6123(10) 0.5805(5) 0.036(3) Uani 1 d . . C13 C -0.2025(14) 0.6355(11) 0.6051(5) 0.042(4) Uani 1 d . . C14 C -0.2977(14) 0.6559(12) 0.6319(5) 0.044(3) Uani 1 d . . C15 C -0.4081(13) 0.6687(14) 0.6660(5) 0.051(4) Uani 1 d . . C10 C -0.0168(13) 0.4012(10) 0.5452(5) 0.036(3) Uani 1 d . . C16 C -0.4672(15) 0.7752(15) 0.6814(6) 0.059(4) Uani 1 d . . H16 H -0.4433(15) 0.8484(15) 0.6680(6) 0.071 Uiso 1 calc R . C17 C -0.5686(15) 0.7510(17) 0.7203(6) 0.064(5) Uani 1 d . . H17 H -0.6235(15) 0.8055(17) 0.7363(6) 0.077 Uiso 1 calc R . C18 C -0.5727(17) 0.6269(22) 0.7312(8) 0.092(7) Uani 1 d . . H18 H -0.6291(17) 0.5877(22) 0.7557(8) 0.111 Uiso 1 calc R . C19 C -0.4764(16) 0.5785(14) 0.6980(6) 0.061(4) Uani 1 d . . H19 H -0.4579(16) 0.4997(14) 0.6963(6) 0.074 Uiso 1 calc R . C20 C -0.2205(17) 0.7204(34) 0.7776(8) 0.121(12) Uani 1 d . . H20 H -0.1555(17) 0.7280(34) 0.7500(8) 0.145 Uiso 1 calc R . C21 C -0.2913(21) 0.8051(18) 0.8007(9) 0.082(6) Uani 1 d . . H21 H -0.2809(21) 0.8832(18) 0.7916(9) 0.098 Uiso 1 calc R . C22 C -0.3777(19) 0.7657(19) 0.8380(8) 0.075(5) Uani 1 d . . H22 H -0.4365(19) 0.8112(19) 0.8580(8) 0.090 Uiso 1 calc R . C23 C -0.3676(26) 0.6478(26) 0.8426(8) 0.108(8) Uani 1 d . . H23 H -0.4176(26) 0.5998(26) 0.8661(8) 0.130 Uiso 1 calc R . C24 C -0.2679(27) 0.6117(19) 0.8053(11) 0.102(8) Uani 1 d . . H24 H -0.2384(27) 0.5366(19) 0.7995(11) 0.122 Uiso 1 calc R . C6 C -0.1012(16) 0.3489(11) 0.5054(5) 0.051(4) Uani 1 d . . H6 H -0.1646(16) 0.3869(11) 0.4844(5) 0.062 Uiso 1 calc R . C7 C -0.0742(20) 0.2286(13) 0.5021(6) 0.070(5) Uani 1 d . . H7 H -0.1166(20) 0.1745(13) 0.4786(6) 0.084 Uiso 1 calc R . C8 C 0.0279(18) 0.2050(12) 0.5404(8) 0.069(5) Uani 1 d . . H8 H 0.0639(18) 0.1328(12) 0.5477(8) 0.083 Uiso 1 calc R . C9 C 0.0654(13) 0.3131(10) 0.5659(6) 0.044(4) Uani 1 d . . H9 H 0.1327(13) 0.3240(10) 0.5919(6) 0.053 Uiso 1 calc R . C5 C -0.2028(15) 0.3424(16) 0.6614(6) 0.062(5) Uani 1 d . . H5 H -0.1902(15) 0.4167(16) 0.6765(6) 0.074 Uiso 1 calc R . C1 C -0.2917(16) 0.3117(14) 0.6187(7) 0.065(4) Uani 1 d . . H1 H -0.3495(16) 0.3613(14) 0.6009(7) 0.078 Uiso 1 calc R . C2 C -0.2789(16) 0.1932(15) 0.6073(7) 0.064(5) Uani 1 d . . H2 H -0.3273(16) 0.1507(15) 0.5804(7) 0.077 Uiso 1 calc R . C3 C -0.1836(18) 0.1493(15) 0.6421(7) 0.070(5) Uani 1 d . . H3 H -0.1551(18) 0.0730(15) 0.6425(7) 0.084 Uiso 1 calc R . C4 C -0.1356(16) 0.2438(16) 0.6780(6) 0.066(5) Uani 1 d . . H4 H -0.0722(16) 0.2396(16) 0.7066(6) 0.079 Uiso 1 calc R . C31 C 0.0337(13) 0.8197(10) 0.5142(6) 0.044(3) Uani 1 d . . C32 C -0.0982(16) 0.6478(12) 0.4565(6) 0.051(4) Uani 1 d . . C30 C 0.1605(15) 0.6180(12) 0.4711(5) 0.045(4) Uani 1 d . . C34 C 0.0899(18) 0.7639(12) 0.6469(6) 0.062(4) Uani 1 d . . C35 C 0.0611(14) 0.5435(12) 0.6839(6) 0.048(4) Uani 1 d . . C33 C 0.2476(19) 0.5740(14) 0.5980(6) 0.053(4) Uani 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 Co2 0.0328(12) 0.0404(9) 0.0423(9) -0.0058(7) 0.0007(8) -0.0024(9) Co1 0.0339(12) 0.0333(8) 0.0428(9) 0.0041(7) 0.0053(8) 0.0017(8) Fe2 0.0396(14) 0.0363(9) 0.0439(9) 0.0005(8) 0.0058(9) -0.0077(10) Fe1 0.0311(14) 0.0660(13) 0.0405(10) -0.0064(8) -0.0025(8) 0.0053(11) O31 0.112(12) 0.049(7) 0.109(10) 0.010(6) -0.019(9) -0.011(7) O32 0.057(9) 0.094(9) 0.076(8) 0.000(7) -0.026(7) -0.005(7) O30 0.062(9) 0.099(9) 0.084(8) 0.003(7) 0.034(7) 0.025(8) O34 0.148(14) 0.067(7) 0.106(9) -0.043(7) 0.038(10) -0.029(9) O35 0.095(10) 0.092(8) 0.052(6) 0.014(6) 0.006(6) 0.000(8) O33 0.048(9) 0.094(9) 0.074(7) -0.002(7) 0.000(7) 0.017(7) C11 0.024(8) 0.030(6) 0.037(6) -0.002(4) 0.006(5) -0.004(6) C12 0.035(9) 0.038(6) 0.034(6) -0.009(5) 0.002(6) -0.001(7) C13 0.049(11) 0.050(8) 0.025(6) -0.005(5) -0.005(6) 0.005(7) C14 0.044(11) 0.056(8) 0.033(7) -0.001(6) 0.002(7) 0.007(8) C15 0.026(9) 0.088(10) 0.039(7) -0.010(7) -0.006(6) 0.011(9) C10 0.041(9) 0.045(7) 0.023(6) -0.008(5) 0.010(5) -0.006(7) C16 0.047(11) 0.085(10) 0.045(8) -0.002(7) -0.005(7) 0.034(9) C17 0.034(11) 0.100(14) 0.059(9) -0.018(9) -0.006(7) 0.026(10) C18 0.034(12) 0.173(23) 0.070(11) -0.050(13) 0.007(9) -0.012(14) C19 0.060(12) 0.073(10) 0.052(9) -0.013(7) 0.010(8) -0.010(9) C20 0.021(12) 0.276(38) 0.066(12) -0.038(20) -0.022(9) 0.017(19) C21 0.061(15) 0.087(13) 0.097(14) -0.005(11) -0.022(12) -0.025(12) C22 0.061(15) 0.099(14) 0.065(10) -0.017(10) -0.015(10) 0.023(12) C23 0.128(23) 0.151(23) 0.046(10) 0.020(13) -0.026(12) -0.020(20) C24 0.134(23) 0.075(13) 0.096(16) -0.016(12) -0.059(16) 0.047(15) C6 0.064(11) 0.047(7) 0.042(7) 0.002(6) 0.000(7) -0.020(8) C7 0.106(16) 0.056(9) 0.047(8) -0.009(7) 0.018(9) -0.033(11) C8 0.075(14) 0.035(7) 0.096(13) -0.017(8) 0.038(11) 0.005(8) C9 0.027(10) 0.031(7) 0.074(9) 0.005(6) 0.020(7) 0.007(6) C5 0.050(12) 0.085(12) 0.049(9) -0.019(8) 0.023(8) -0.014(10) C1 0.054(12) 0.062(10) 0.079(10) -0.010(9) 0.020(9) 0.004(9) C2 0.048(11) 0.078(11) 0.066(10) 0.000(8) 0.004(8) -0.031(9) C3 0.085(15) 0.056(10) 0.068(10) 0.019(8) 0.023(10) 0.001(10) C4 0.059(13) 0.095(13) 0.043(8) 0.009(8) 0.010(7) -0.007(11) C31 0.042(10) 0.025(7) 0.066(8) -0.003(6) -0.006(7) 0.006(6) C32 0.042(11) 0.053(8) 0.058(8) 0.013(7) 0.007(8) 0.003(8) C30 0.051(12) 0.042(7) 0.041(7) 0.000(6) 0.002(7) -0.011(7) C34 0.073(12) 0.052(8) 0.060(8) -0.017(7) 0.018(8) -0.011(9) C35 0.026(10) 0.058(9) 0.061(9) -0.003(7) -0.008(7) 0.000(7) C33 0.062(14) 0.061(9) 0.035(8) -0.013(6) -0.002(7) 0.003(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 Co2 C35 1.759(15) . ? Co2 C34 1.802(14) . ? Co2 C33 1.85(2) . ? Co2 C11 1.930(12) . ? Co2 C12 1.955(13) . ? Co2 Co1 2.473(2) . ? Co1 C32 1.79(2) . ? Co1 C31 1.796(12) . ? Co1 C30 1.85(2) . ? Co1 C12 1.954(12) . ? Co1 C11 1.964(11) . ? Fe2 C2 2.01(2) . ? Fe2 C6 2.022(12) . ? Fe2 C1 2.02(2) . ? Fe2 C3 2.028(15) . ? Fe2 C7 2.031(14) . ? Fe2 C10 2.031(12) . ? Fe2 C8 2.037(15) . ? Fe2 C5 2.039(14) . ? Fe2 C9 2.049(14) . ? Fe2 C4 2.069(14) . ? Fe1 C21 2.00(2) . ? Fe1 C20 2.01(2) . ? Fe1 C19 2.021(15) . ? Fe1 C22 2.02(2) . ? Fe1 C15 2.033(12) . ? Fe1 C16 2.035(14) . ? Fe1 C23 2.04(2) . ? Fe1 C24 2.04(2) . ? Fe1 C18 2.05(2) . ? Fe1 C17 2.05(2) . ? O31 C31 1.14(2) . ? O32 C32 1.13(2) . ? O30 C30 1.10(2) . ? O34 C34 1.15(2) . ? O35 C35 1.15(2) . ? O33 C33 1.10(2) . ? C11 C12 1.33(2) . ? C11 C10 1.48(2) . ? C12 C13 1.42(2) . ? C13 C14 1.20(2) . ? C14 C15 1.41(2) . ? C15 C16 1.42(2) . ? C15 C19 1.45(2) . ? C10 C6 1.40(2) . ? C10 C9 1.42(2) . ? C16 C17 1.41(2) . ? C17 C18 1.45(3) . ? C18 C19 1.38(2) . ? C20 C21 1.34(3) . ? C20 C24 1.49(3) . ? C21 C22 1.32(3) . ? C22 C23 1.37(3) . ? C23 C24 1.41(3) . ? C6 C7 1.42(2) . ? C7 C8 1.41(3) . ? C8 C9 1.43(2) . ? C5 C1 1.39(2) . ? C5 C4 1.39(2) . ? C1 C2 1.40(2) . ? C2 C3 1.37(2) . ? C3 C4 1.45(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 C35 Co2 C34 98.0(7) . . ? C35 Co2 C33 100.9(6) . . ? C34 Co2 C33 108.6(8) . . ? C35 Co2 C11 100.9(6) . . ? C34 Co2 C11 140.8(7) . . ? C33 Co2 C11 101.1(6) . . ? C35 Co2 C12 101.4(6) . . ? C34 Co2 C12 102.5(7) . . ? C33 Co2 C12 138.4(5) . . ? C11 Co2 C12 40.1(5) . . ? C35 Co2 Co1 149.8(5) . . ? C34 Co2 Co1 99.5(5) . . ? C33 Co2 Co1 96.6(4) . . ? C11 Co2 Co1 51.2(3) . . ? C12 Co2 Co1 50.7(3) . . ? C32 Co1 C31 100.2(6) . . ? C32 Co1 C30 100.6(6) . . ? C31 Co1 C30 103.3(6) . . ? C32 Co1 C12 97.1(6) . . ? C31 Co1 C12 109.8(6) . . ? C30 Co1 C12 138.8(6) . . ? C32 Co1 C11 100.8(6) . . ? C31 Co1 C11 145.0(6) . . ? C30 Co1 C11 100.0(6) . . ? C12 Co1 C11 39.7(5) . . ? C32 Co1 Co2 146.6(4) . . ? C31 Co1 Co2 99.8(5) . . ? C30 Co1 Co2 100.5(4) . . ? C12 Co1 Co2 50.8(4) . . ? C11 Co1 Co2 50.0(3) . . ? C2 Fe2 C6 118.2(7) . . ? C2 Fe2 C1 40.4(7) . . ? C6 Fe2 C1 107.9(7) . . ? C2 Fe2 C3 39.8(7) . . ? C6 Fe2 C3 151.2(7) . . ? C1 Fe2 C3 67.7(7) . . ? C2 Fe2 C7 106.0(7) . . ? C6 Fe2 C7 41.0(6) . . ? C1 Fe2 C7 126.0(8) . . ? C3 Fe2 C7 116.9(7) . . ? C2 Fe2 C10 152.8(7) . . ? C6 Fe2 C10 40.4(5) . . ? C1 Fe2 C10 119.8(6) . . ? C3 Fe2 C10 166.8(7) . . ? C7 Fe2 C10 68.7(5) . . ? C2 Fe2 C8 125.0(7) . . ? C6 Fe2 C8 68.7(7) . . ? C1 Fe2 C8 162.8(7) . . ? C3 Fe2 C8 106.6(7) . . ? C7 Fe2 C8 40.5(7) . . ? C10 Fe2 C8 69.3(5) . . ? C2 Fe2 C5 67.5(6) . . ? C6 Fe2 C5 128.0(7) . . ? C1 Fe2 C5 40.0(6) . . ? C3 Fe2 C5 68.0(7) . . ? C7 Fe2 C5 164.3(8) . . ? C10 Fe2 C5 110.0(6) . . ? C8 Fe2 C5 154.9(8) . . ? C2 Fe2 C9 164.0(6) . . ? C6 Fe2 C9 67.7(6) . . ? C1 Fe2 C9 155.0(6) . . ? C3 Fe2 C9 128.4(7) . . ? C7 Fe2 C9 67.8(7) . . ? C10 Fe2 C9 40.7(5) . . ? C8 Fe2 C9 40.9(6) . . ? C5 Fe2 C9 122.1(6) . . ? C2 Fe2 C4 67.6(7) . . ? C6 Fe2 C4 165.5(6) . . ? C1 Fe2 C4 67.1(7) . . ? C3 Fe2 C4 41.3(6) . . ? C7 Fe2 C4 153.1(7) . . ? C10 Fe2 C4 128.9(6) . . ? C8 Fe2 C4 120.2(8) . . ? C5 Fe2 C4 39.6(6) . . ? C9 Fe2 C4 110.7(6) . . ? C21 Fe1 C20 38.9(9) . . ? C21 Fe1 C19 165.9(9) . . ? C20 Fe1 C19 128.9(10) . . ? C21 Fe1 C22 38.3(8) . . ? C20 Fe1 C22 66.5(8) . . ? C19 Fe1 C22 154.1(8) . . ? C21 Fe1 C15 127.0(8) . . ? C20 Fe1 C15 106.7(7) . . ? C19 Fe1 C15 42.1(6) . . ? C22 Fe1 C15 163.1(8) . . ? C21 Fe1 C16 108.3(8) . . ? C20 Fe1 C16 116.9(10) . . ? C19 Fe1 C16 69.1(7) . . ? C22 Fe1 C16 126.7(8) . . ? C15 Fe1 C16 40.9(5) . . ? C21 Fe1 C23 65.8(9) . . ? C20 Fe1 C23 69.0(10) . . ? C19 Fe1 C23 120.4(9) . . ? C22 Fe1 C23 39.4(8) . . ? C15 Fe1 C23 154.9(10) . . ? C16 Fe1 C23 163.6(10) . . ? C21 Fe1 C24 67.5(8) . . ? C20 Fe1 C24 43.1(10) . . ? C19 Fe1 C24 108.3(8) . . ? C22 Fe1 C24 67.2(8) . . ? C15 Fe1 C24 119.2(8) . . ? C16 Fe1 C24 153.6(10) . . ? C23 Fe1 C24 40.5(9) . . ? C21 Fe1 C18 153.7(9) . . ? C20 Fe1 C18 166.2(13) . . ? C19 Fe1 C18 39.7(6) . . ? C22 Fe1 C18 120.9(8) . . ? C15 Fe1 C18 69.5(6) . . ? C16 Fe1 C18 69.5(8) . . ? C23 Fe1 C18 108.5(10) . . ? C24 Fe1 C18 126.2(11) . . ? C21 Fe1 C17 119.8(8) . . ? C20 Fe1 C17 150.8(12) . . ? C19 Fe1 C17 67.8(7) . . ? C22 Fe1 C17 109.4(7) . . ? C15 Fe1 C17 68.5(6) . . ? C16 Fe1 C17 40.5(6) . . ? C23 Fe1 C17 127.5(10) . . ? C24 Fe1 C17 164.7(11) . . ? C18 Fe1 C17 41.4(7) . . ? C12 C11 C10 141.5(13) . . ? C12 C11 Co2 71.0(7) . . ? C10 C11 Co2 136.4(10) . . ? C12 C11 Co1 69.7(7) . . ? C10 C11 Co1 131.6(8) . . ? Co2 C11 Co1 78.8(4) . . ? C11 C12 C13 141.6(12) . . ? C11 C12 Co1 70.5(7) . . ? C13 C12 Co1 137.8(10) . . ? C11 C12 Co2 68.9(8) . . ? C13 C12 Co2 131.0(8) . . ? Co1 C12 Co2 78.5(5) . . ? C14 C13 C12 172.6(13) . . ? C13 C14 C15 174.3(16) . . ? C14 C15 C16 126.1(15) . . ? C14 C15 C19 127.4(14) . . ? C16 C15 C19 106.1(12) . . ? C14 C15 Fe1 121.6(9) . . ? C16 C15 Fe1 69.6(7) . . ? C19 C15 Fe1 68.5(7) . . ? C6 C10 C9 107.1(11) . . ? C6 C10 C11 127.1(13) . . ? C9 C10 C11 125.8(12) . . ? C6 C10 Fe2 69.5(7) . . ? C9 C10 Fe2 70.4(7) . . ? C11 C10 Fe2 126.9(8) . . ? C17 C16 C15 108.3(15) . . ? C17 C16 Fe1 70.4(8) . . ? C15 C16 Fe1 69.5(8) . . ? C16 C17 C18 108.7(15) . . ? C16 C17 Fe1 69.2(8) . . ? C18 C17 Fe1 69.2(10) . . ? C19 C18 C17 106.6(18) . . ? C19 C18 Fe1 69.0(10) . . ? C17 C18 Fe1 69.3(11) . . ? C18 C19 C15 110.2(17) . . ? C18 C19 Fe1 71.3(10) . . ? C15 C19 Fe1 69.4(8) . . ? C21 C20 C24 105.2(18) . . ? C21 C20 Fe1 70.2(10) . . ? C24 C20 Fe1 69.3(12) . . ? C22 C21 C20 112.6(22) . . ? C22 C21 Fe1 71.6(11) . . ? C20 C21 Fe1 70.9(12) . . ? C21 C22 C23 109.5(21) . . ? C21 C22 Fe1 70.1(11) . . ? C23 C22 Fe1 70.9(11) . . ? C22 C23 C24 107.9(22) . . ? C22 C23 Fe1 69.8(12) . . ? C24 C23 Fe1 69.7(10) . . ? C23 C24 C20 104.6(19) . . ? C23 C24 Fe1 69.7(12) . . ? C20 C24 Fe1 67.6(10) . . ? C10 C6 C7 108.9(15) . . ? C10 C6 Fe2 70.2(7) . . ? C7 C6 Fe2 69.8(8) . . ? C8 C7 C6 108.3(14) . . ? C8 C7 Fe2 70.0(8) . . ? C6 C7 Fe2 69.2(8) . . ? C7 C8 C9 106.8(14) . . ? C7 C8 Fe2 69.5(9) . . ? C9 C8 Fe2 70.0(8) . . ? C10 C9 C8 108.8(14) . . ? C10 C9 Fe2 69.0(7) . . ? C8 C9 Fe2 69.1(9) . . ? C1 C5 C4 108.9(15) . . ? C1 C5 Fe2 69.4(8) . . ? C4 C5 Fe2 71.3(9) . . ? C5 C1 C2 108.0(17) . . ? C5 C1 Fe2 70.6(9) . . ? C2 C1 Fe2 69.3(10) . . ? C3 C2 C1 109.2(16) . . ? C3 C2 Fe2 70.7(9) . . ? C1 C2 Fe2 70.2(10) . . ? C2 C3 C4 107.3(15) . . ? C2 C3 Fe2 69.5(9) . . ? C4 C3 Fe2 70.9(9) . . ? C5 C4 C3 106.6(14) . . ? C5 C4 Fe2 69.1(8) . . ? C3 C4 Fe2 67.8(8) . . ? O31 C31 Co1 177.2(13) . . ? O32 C32 Co1 175.4(13) . . ? O30 C30 Co1 178.7(14) . . ? O34 C34 Co2 178.0(19) . . ? O35 C35 Co2 177.1(14) . . ? O33 C33 Co2 175.6(15) . . ? _refine_diff_density_max 0.647 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.134 #===END data_syl _database_code_CSD 151899 _audit_creation_method SHELXL chemical_formula_sum 'C22 H15 Co Fe Mo O5' _chemical_formula_weight 570.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' 'Mo' 'Mo' -1.6832 0.6857 '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 8.2046(8) _cell_length_b 8.7356(7) _cell_length_c 14.869(2) _cell_angle_alpha 78.365(7) _cell_angle_beta 87.176(8) _cell_angle_gamma 78.197(7) _cell_volume 1021.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14 _cell_measurement_theta_max 18 _exptl_crystal_description prism _exptl_crystal_colour dark red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.853 _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 2.139 _exptl_absorpt_correction_type psiscan _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 CAD4 _diffrn_measurement_method CAD4 _diffrn_standards_number 6 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% <0.1 _diffrn_reflns_number 3738 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 24.97 _reflns_number_total 3482 _reflns_number_observed 2710 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ortex _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 rotational disorder of the unbound Cp ring (C1-C5) was modelled as two Cp rings with refined occupancies of 0.55827 and 0.44173. The carbon atoms were held isotopic. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+1.0971P] 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 fixed _refine_ls_extinction_method none _refine_ls_number_reflns 3479 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_obs 0.0313 _refine_ls_wR_factor_all 0.0726 _refine_ls_wR_factor_obs 0.0624 _refine_ls_goodness_of_fit_all 1.044 _refine_ls_goodness_of_fit_obs 1.056 _refine_ls_restrained_S_all 1.076 _refine_ls_restrained_S_obs 1.056 _refine_ls_shift/esd_max -0.070 _refine_ls_shift/esd_mean 0.014 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo Mo 0.25704(4) 0.96689(4) 0.73299(2) 0.02876(11) Uani 1 d . . Co Co 0.21482(7) 0.75422(7) 0.88598(4) 0.0314(2) Uani 1 d . . Fe Fe 0.71650(8) 0.55200(7) 0.69647(4) 0.0333(2) Uani 1 d . . O1 O 0.4496(5) 0.8313(4) 1.0044(2) 0.0643(10) Uani 1 d . . O2 O -0.1183(5) 0.9179(5) 0.9337(3) 0.0737(12) Uani 1 d . . O3 O 0.2048(5) 0.4213(4) 0.9633(3) 0.0656(11) Uani 1 d . . O4 O 0.2666(6) 0.9079(5) 0.5321(3) 0.0812(14) Uani 1 d . . O5 O -0.1254(4) 1.0089(5) 0.7036(3) 0.0761(12) Uani 1 d . . C1A C 0.5986(6) 0.5888(10) 0.5732(5) 0.037(2) Uiso 0.558(10) d PG 1 H1AA H 0.4798(6) 0.5935(10) 0.5649(5) 0.045 Uiso 0.558(10) calc PR 1 C2A C 0.6736(10) 0.7201(5) 0.5772(5) 0.039(2) Uiso 0.558(10) d PG 1 H2AA H 0.6156(17) 0.8312(6) 0.5722(8) 0.046 Uiso 0.558(10) calc PR 1 C3A C 0.8471(9) 0.6618(11) 0.5904(5) 0.053(3) Uiso 0.558(10) d PG 1 H3AA H 0.9300(14) 0.7257(18) 0.5959(8) 0.064 Uiso 0.558(10) calc PR 1 C4A C 0.8794(8) 0.4944(11) 0.5946(5) 0.060(3) Uiso 0.558(10) d PG 1 H4AA H 0.9886(11) 0.4227(17) 0.6032(8) 0.072 Uiso 0.558(10) calc PR 1 C5A C 0.7258(12) 0.4493(6) 0.5841(6) 0.062(3) Uiso 0.558(10) d PG 1 H5AA H 0.7103(20) 0.3410(7) 0.5841(9) 0.074 Uiso 0.558(10) calc PR 1 C1B C 0.6267(10) 0.6537(14) 0.5703(7) 0.060(4) Uiso 0.442(10) d PG 2 H1BA H 0.5172(10) 0.7229(14) 0.5563(7) 0.072 Uiso 0.442(10) calc PR 2 C2B C 0.7759(17) 0.7047(7) 0.5834(7) 0.059(4) Uiso 0.442(10) d PG 2 H2BA H 0.7872(27) 0.8150(9) 0.5809(10) 0.071 Uiso 0.442(10) calc PR 2 C3B C 0.9062(8) 0.5679(13) 0.5998(6) 0.035(3) Uiso 0.442(10) d PG 2 H3BA H 1.0226(10) 0.5669(23) 0.6125(9) 0.042 Uiso 0.442(10) calc PR 2 C4B C 0.8376(12) 0.4324(7) 0.5969(6) 0.034(3) Uiso 0.442(10) d PG 2 H4BA H 0.8981(21) 0.3214(9) 0.6075(9) 0.041 Uiso 0.442(10) calc PR 2 C5B C 0.6648(11) 0.4855(14) 0.5786(7) 0.062(4) Uiso 0.442(10) d PG 2 H5BA H 0.5858(18) 0.4178(21) 0.5727(11) 0.074 Uiso 0.442(10) calc PR 2 C6 C 0.7011(5) 0.6589(6) 0.8069(3) 0.0381(10) Uani 1 d . . H6 H 0.7200(5) 0.7604(6) 0.8065(3) 0.046 Uiso 1 calc R . C7 C 0.8229(6) 0.5169(6) 0.8211(3) 0.0478(12) Uani 1 d . . H7 H 0.9354(6) 0.5087(6) 0.8318(3) 0.057 Uiso 1 calc R . C8 C 0.7450(6) 0.3907(6) 0.8163(3) 0.0497(13) Uani 1 d . . H8 H 0.7965(6) 0.2839(6) 0.8233(3) 0.060 Uiso 1 calc R . C9 C 0.5751(6) 0.4536(5) 0.7992(3) 0.0421(11) Uani 1 d . . H9 H 0.4953(6) 0.3949(5) 0.7927(3) 0.051 Uiso 1 calc R . C1O C 0.5448(5) 0.6216(5) 0.7933(3) 0.0283(9) Uani 1 d . . C11 C 0.3819(5) 0.7263(5) 0.7828(3) 0.0276(9) Uani 1 d . . C12 C 0.2274(5) 0.7208(5) 0.7598(3) 0.0324(10) Uani 1 d . . H12 H 0.1699(61) 0.6626(58) 0.7291(33) 0.060(15) Uiso 1 d . . C13 C 0.3030(6) 1.2192(5) 0.6695(3) 0.0431(11) Uani 1 d . . H13 H 0.2664(6) 1.2677(5) 0.6104(3) 0.052 Uiso 1 calc R . C14 C 0.4592(6) 1.1198(5) 0.6934(4) 0.0466(12) Uani 1 d . . H14 H 0.5438(6) 1.0906(5) 0.6525(4) 0.056 Uiso 1 calc R . C15 C 0.4655(6) 1.0725(5) 0.7890(3) 0.0432(11) Uani 1 d . . H15 H 0.5548(6) 1.0070(5) 0.8227(3) 0.052 Uiso 1 calc R . C16 C 0.3130(6) 1.1415(5) 0.8251(3) 0.0399(11) Uani 1 d . . H16 H 0.2837(6) 1.1296(5) 0.8870(3) 0.048 Uiso 1 calc R . C17 C 0.2127(6) 1.2315(5) 0.7515(3) 0.0420(11) Uani 1 d . . H17 H 0.1051(6) 1.2893(5) 0.7562(3) 0.050 Uiso 1 calc R . C18 C 0.3552(6) 0.8029(5) 0.9600(3) 0.0415(11) Uani 1 d . . C19 C 0.0098(6) 0.8520(6) 0.9154(3) 0.0445(11) Uani 1 d . . C20 C 0.2099(6) 0.5502(6) 0.9361(3) 0.0413(11) Uani 1 d . . C21 C 0.2669(6) 0.9274(6) 0.6053(3) 0.0472(12) Uani 1 d . . C22 C 0.0130(6) 0.9927(6) 0.7161(3) 0.0467(12) Uani 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 Mo 0.0279(2) 0.0291(2) 0.0298(2) -0.00529(15) -0.00022(15) -0.00729(15) Co 0.0308(3) 0.0341(3) 0.0309(3) -0.0072(2) 0.0044(2) -0.0104(3) Fe 0.0363(4) 0.0402(4) 0.0249(3) -0.0094(3) 0.0045(3) -0.0092(3) O1 0.072(3) 0.073(3) 0.055(2) -0.011(2) -0.022(2) -0.028(2) O2 0.048(2) 0.077(3) 0.094(3) -0.032(2) 0.019(2) -0.001(2) O3 0.098(3) 0.037(2) 0.062(2) -0.001(2) 0.005(2) -0.024(2) O4 0.132(4) 0.071(3) 0.036(2) -0.017(2) -0.014(2) -0.001(3) O5 0.036(2) 0.082(3) 0.107(3) -0.004(2) -0.021(2) -0.012(2) C6 0.039(3) 0.048(3) 0.031(2) -0.018(2) -0.002(2) -0.009(2) C7 0.038(3) 0.068(3) 0.035(3) -0.017(2) -0.003(2) 0.002(2) C8 0.055(3) 0.039(3) 0.044(3) 0.001(2) 0.014(2) 0.005(2) C9 0.048(3) 0.029(2) 0.049(3) -0.006(2) 0.016(2) -0.012(2) C1O 0.032(2) 0.033(2) 0.022(2) -0.007(2) 0.004(2) -0.008(2) C11 0.034(2) 0.028(2) 0.022(2) -0.006(2) 0.004(2) -0.009(2) C12 0.037(2) 0.032(2) 0.031(2) -0.005(2) -0.002(2) -0.013(2) C13 0.053(3) 0.031(3) 0.043(3) -0.001(2) 0.004(2) -0.011(2) C14 0.039(3) 0.038(3) 0.069(4) -0.017(2) 0.020(2) -0.019(2) C15 0.042(3) 0.032(2) 0.060(3) -0.012(2) -0.011(2) -0.012(2) C16 0.052(3) 0.033(2) 0.040(3) -0.013(2) 0.005(2) -0.016(2) C17 0.039(3) 0.032(2) 0.054(3) -0.011(2) 0.003(2) -0.002(2) C18 0.050(3) 0.043(3) 0.033(3) -0.007(2) 0.005(2) -0.015(2) C19 0.044(3) 0.044(3) 0.049(3) -0.013(2) 0.008(2) -0.015(2) C20 0.046(3) 0.045(3) 0.034(3) -0.011(2) 0.008(2) -0.011(2) C21 0.059(3) 0.037(3) 0.042(3) -0.004(2) -0.004(2) -0.006(2) C22 0.037(3) 0.046(3) 0.057(3) -0.004(2) -0.009(2) -0.009(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 Mo C22 1.991(5) . ? Mo C21 1.993(5) . ? Mo C11 2.140(4) . ? Mo C12 2.167(4) . ? Mo C13 2.315(4) . ? Mo C14 2.318(4) . ? Mo C17 2.335(4) . ? Mo C15 2.359(4) . ? Mo C16 2.368(4) . ? Mo Co 2.6883(7) . ? Co C20 1.795(5) . ? Co C18 1.799(5) . ? Co C19 1.800(5) . ? Co C12 1.951(4) . ? Co C11 2.025(4) . ? Fe C1B 2.013(9) . ? Fe C8 2.027(5) . ? Fe C7 2.027(5) . ? Fe C9 2.030(4) . ? Fe C2B 2.031(9) . ? Fe C6 2.033(4) . ? Fe C4A 2.041(7) . ? Fe C5A 2.042(7) . ? Fe C5B 2.043(9) . ? Fe C3A 2.049(7) . ? Fe C1A 2.051(6) . ? Fe C2A 2.056(6) . ? O1 C18 1.136(5) . ? O2 C19 1.139(5) . ? O3 C20 1.126(5) . ? O4 C21 1.135(6) . ? O5 C22 1.135(5) . ? C1A C5A 1.42 . ? C1A C2A 1.42 . ? C2A C3A 1.42 . ? C3A C4A 1.42 . ? C4A C5A 1.42 . ? C1B C2B 1.42 . ? C1B C5B 1.42 . ? C2B C3B 1.42 . ? C3B C4B 1.42 . ? C4B C5B 1.42 . ? C6 C7 1.411(6) . ? C6 C1O 1.419(6) . ? C7 C8 1.398(7) . ? C8 C9 1.405(7) . ? C9 C1O 1.422(6) . ? C1O C11 1.452(5) . ? C11 C12 1.342(6) . ? C13 C17 1.407(6) . ? C13 C14 1.410(6) . ? C14 C15 1.398(7) . ? C15 C16 1.404(6) . ? C16 C17 1.404(6) . ? 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 C22 Mo C21 82.8(2) . . ? C22 Mo C11 114.2(2) . . ? C21 Mo C11 90.6(2) . . ? C22 Mo C12 78.5(2) . . ? C21 Mo C12 79.8(2) . . ? C11 Mo C12 36.30(15) . . ? C22 Mo C13 102.2(2) . . ? C21 Mo C13 86.8(2) . . ? C11 Mo C13 142.9(2) . . ? C12 Mo C13 166.4(2) . . ? C22 Mo C14 137.4(2) . . ? C21 Mo C14 89.1(2) . . ? C11 Mo C14 107.6(2) . . ? C12 Mo C14 141.0(2) . . ? C13 Mo C14 35.4(2) . . ? C22 Mo C17 88.9(2) . . ? C21 Mo C17 117.6(2) . . ? C11 Mo C17 146.2(2) . . ? C12 Mo C17 157.3(2) . . ? C13 Mo C17 35.2(2) . . ? C14 Mo C17 58.4(2) . . ? C22 Mo C15 144.8(2) . . ? C21 Mo C15 121.2(2) . . ? C11 Mo C15 92.5(2) . . ? C12 Mo C15 127.7(2) . . ? C13 Mo C15 58.4(2) . . ? C14 Mo C15 34.8(2) . . ? C17 Mo C15 57.9(2) . . ? C22 Mo C16 110.9(2) . . ? C21 Mo C16 144.0(2) . . ? C11 Mo C16 111.6(2) . . ? C12 Mo C16 134.6(2) . . ? C13 Mo C16 58.2(2) . . ? C14 Mo C16 57.8(2) . . ? C17 Mo C16 34.7(2) . . ? C15 Mo C16 34.6(2) . . ? C22 Mo Co 85.43(14) . . ? C21 Mo Co 125.61(14) . . ? C11 Mo Co 47.94(10) . . ? C12 Mo Co 45.84(11) . . ? C13 Mo Co 147.52(12) . . ? C14 Mo Co 131.02(13) . . ? C17 Mo Co 115.01(12) . . ? C15 Mo Co 97.60(12) . . ? C16 Mo Co 89.50(11) . . ? C20 Co C18 102.5(2) . . ? C20 Co C19 101.0(2) . . ? C18 Co C19 105.7(2) . . ? C20 Co C12 94.6(2) . . ? C18 Co C12 134.5(2) . . ? C19 Co C12 112.0(2) . . ? C20 Co C11 101.0(2) . . ? C18 Co C11 95.5(2) . . ? C19 Co C11 145.1(2) . . ? C12 Co C11 39.4(2) . . ? C20 Co Mo 146.99(14) . . ? C18 Co Mo 98.80(14) . . ? C19 Co Mo 97.1(2) . . ? C12 Co Mo 52.83(12) . . ? C11 Co Mo 51.70(11) . . ? C1B Fe C8 156.7(4) . . ? C1B Fe C7 162.3(4) . . ? C8 Fe C7 40.3(2) . . ? C1B Fe C9 122.7(3) . . ? C8 Fe C9 40.5(2) . . ? C7 Fe C9 68.0(2) . . ? C1B Fe C2B 41.1(2) . . ? C8 Fe C2B 159.6(4) . . ? C7 Fe C2B 124.2(4) . . ? C9 Fe C2B 158.9(4) . . ? C1B Fe C6 126.4(3) . . ? C8 Fe C6 68.1(2) . . ? C7 Fe C6 40.7(2) . . ? C9 Fe C6 67.9(2) . . ? C2B Fe C6 109.0(2) . . ? C8 Fe C4A 114.8(2) . . ? C7 Fe C4A 114.2(2) . . ? C9 Fe C4A 141.7(3) . . ? C6 Fe C4A 140.3(3) . . ? C8 Fe C5A 113.1(2) . . ? C7 Fe C5A 141.0(3) . . ? C9 Fe C5A 112.1(2) . . ? C6 Fe C5A 178.3(3) . . ? C4A Fe C5A 40.71(13) . . ? C1B Fe C5B 41.0(2) . . ? C8 Fe C5B 120.1(3) . . ? C7 Fe C5B 154.5(4) . . ? C9 Fe C5B 108.0(3) . . ? C2B Fe C5B 68.7(2) . . ? C6 Fe C5B 163.3(3) . . ? C8 Fe C3A 142.7(3) . . ? C7 Fe C3A 114.0(2) . . ? C9 Fe C3A 176.6(3) . . ? C6 Fe C3A 111.6(2) . . ? C4A Fe C3A 40.63(12) . . ? C5A Fe C3A 68.3(2) . . ? C8 Fe C1A 138.6(3) . . ? C7 Fe C1A 177.4(2) . . ? C9 Fe C1A 109.8(2) . . ? C6 Fe C1A 137.7(3) . . ? C4A Fe C1A 68.3(2) . . ? C5A Fe C1A 40.60(12) . . ? C3A Fe C1A 68.16(14) . . ? C8 Fe C2A 176.7(3) . . ? C7 Fe C2A 140.4(3) . . ? C9 Fe C2A 136.2(3) . . ? C6 Fe C2A 110.6(2) . . ? C4A Fe C2A 68.2(2) . . ? C5A Fe C2A 68.22(15) . . ? C3A Fe C2A 40.47(11) . . ? C1A Fe C2A 40.46(11) . . ? C5A C1A C2A 108.0 . . ? C5A C1A Fe 69.3(3) . . ? C2A C1A Fe 70.0(3) . . ? C3A C2A C1A 108.0 . . ? C3A C2A Fe 69.5(2) . . ? C1A C2A Fe 69.6(3) . . ? C2A C3A C4A 108.0 . . ? C2A C3A Fe 70.0(2) . . ? C4A C3A Fe 69.4(3) . . ? C5A C4A C3A 108.0 . . ? C5A C4A Fe 69.7(3) . . ? C3A C4A Fe 70.0(3) . . ? C4A C5A C1A 108.0 . . ? C4A C5A Fe 69.6(3) . . ? C1A C5A Fe 70.1(2) . . ? C2B C1B C5B 108.0 . . ? C2B C1B Fe 70.1(3) . . ? C5B C1B Fe 70.7(3) . . ? C1B C2B C3B 108.0 . . ? C1B C2B Fe 68.7(3) . . ? C3B C2B Fe 71.3(3) . . ? C4B C3B C2B 108.0 . . ? C4B C3B Fe 70.3(3) . . ? C2B C3B Fe 68.2(3) . . ? C3B C4B C5B 108.0 . . ? C3B C4B Fe 69.7(3) . . ? C5B C4B Fe 68.5(3) . . ? C4B C5B C1B 108.0 . . ? C4B C5B Fe 71.2(3) . . ? C1B C5B Fe 68.3(3) . . ? C7 C6 C1O 108.9(4) . . ? C7 C6 Fe 69.5(3) . . ? C1O C6 Fe 70.6(2) . . ? C8 C7 C6 108.0(4) . . ? C8 C7 Fe 69.8(3) . . ? C6 C7 Fe 69.9(3) . . ? C7 C8 C9 108.0(4) . . ? C7 C8 Fe 69.9(3) . . ? C9 C8 Fe 69.9(3) . . ? C8 C9 C1O 109.1(4) . . ? C8 C9 Fe 69.6(3) . . ? C1O C9 Fe 70.6(2) . . ? C6 C1O C9 106.0(4) . . ? C6 C1O C11 128.8(4) . . ? C9 C1O C11 125.1(4) . . ? C6 C1O Fe 68.8(2) . . ? C9 C1O Fe 68.6(2) . . ? C11 C1O Fe 130.7(3) . . ? C12 C11 C1O 138.0(4) . . ? C12 C11 Co 67.3(2) . . ? C1O C11 Co 124.8(3) . . ? C12 C11 Mo 72.9(2) . . ? C1O C11 Mo 143.4(3) . . ? Co C11 Mo 80.35(14) . . ? C11 C12 Co 73.3(3) . . ? C11 C12 Mo 70.8(2) . . ? Co C12 Mo 81.3(2) . . ? C17 C13 C14 107.3(4) . . ? C17 C13 Mo 73.2(2) . . ? C14 C13 Mo 72.4(2) . . ? C15 C14 C13 108.5(4) . . ? C15 C14 Mo 74.2(2) . . ? C13 C14 Mo 72.1(2) . . ? C14 C15 C16 107.9(4) . . ? C14 C15 Mo 71.0(2) . . ? C16 C15 Mo 73.1(3) . . ? C17 C16 C15 108.0(4) . . ? C17 C16 Mo 71.4(3) . . ? C15 C16 Mo 72.4(2) . . ? C16 C17 C13 108.2(4) . . ? C16 C17 Mo 73.9(2) . . ? C13 C17 Mo 71.6(3) . . ? O1 C18 Co 177.0(4) . . ? O2 C19 Co 178.0(4) . . ? O3 C20 Co 176.5(4) . . ? O4 C21 Mo 177.4(5) . . ? O5 C22 Mo 177.8(5) . . ? _refine_diff_density_max 0.668 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.082 #===END data_ec5s _database_code_CSD 151900 _chemical_formula_sum 'C38 H18 Co4 Fe O12' _chemical_formula_weight 958.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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 10.914(3) _cell_length_b 12.113(2) _cell_length_c 14.919(2) _cell_angle_alpha 93.710(11) _cell_angle_beta 107.050(15) _cell_angle_gamma 96.54(2) _cell_volume 1863.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 16 _cell_measurement_theta_max 18 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.708 _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 2.186 _exptl_absorpt_correction_type psi scan _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 6494 _diffrn_reflns_av_R_equivalents 0.0129 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.08 _diffrn_standards_number 6 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% <0.1 _reflns_number_total 6148 _reflns_number_observed 4729 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ortex _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+0.1715P] 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 fixed _refine_ls_extinction_method none _refine_ls_number_reflns 6148 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_obs 0.0297 _refine_ls_wR_factor_all 0.0731 _refine_ls_wR_factor_obs 0.0650 _refine_ls_goodness_of_fit_all 1.073 _refine_ls_goodness_of_fit_obs 1.103 _refine_ls_restrained_S_all 1.073 _refine_ls_restrained_S_obs 1.103 _refine_ls_shift/esd_max 0.154 _refine_ls_shift/esd_mean 0.018 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.31706(4) 0.66203(3) 0.01966(3) 0.03533(11) Uani 1 d . . Co2 Co 0.44011(4) 0.70497(4) 0.37973(3) 0.04539(12) Uani 1 d . . Co3 Co 0.13819(4) 0.83568(4) -0.28178(3) 0.04578(12) Uani 1 d . . Co1 Co 0.44035(4) 0.87881(3) 0.30209(3) 0.04193(12) Uani 1 d . . Co4 Co 0.05120(4) 0.63667(3) -0.29307(3) 0.04375(12) Uani 1 d . . C1 C 0.2039(3) 0.6943(3) 0.1028(2) 0.0410(7) Uani 1 d . . H1 H 0.1739(3) 0.7619(3) 0.1111(2) 0.049 Uiso 1 calc R . C2 C 0.1409(3) 0.6054(3) 0.0315(2) 0.0490(8) Uani 1 d . . H2 H 0.0623(3) 0.6050(3) -0.0149(2) 0.059 Uiso 1 calc R . C3 C 0.2165(3) 0.5190(3) 0.0427(2) 0.0534(9) Uani 1 d . . H3 H 0.1965(3) 0.4508(3) 0.0056(2) 0.064 Uiso 1 calc R . C4 C 0.3291(3) 0.5531(2) 0.1204(2) 0.0445(7) Uani 1 d . . H4 H 0.3968(3) 0.5119(2) 0.1423(2) 0.053 Uiso 1 calc R . C5 C 0.3204(3) 0.6618(2) 0.1592(2) 0.0369(7) Uani 1 d . . C6 C 0.4098(3) 0.7250(2) 0.2434(2) 0.0362(7) Uani 1 d . . C7 C 0.5346(3) 0.7517(2) 0.2927(2) 0.0375(7) Uani 1 d . . C8 C 0.6631(3) 0.7448(2) 0.2856(2) 0.0388(7) Uani 1 d . . C9 C 0.7729(3) 0.8018(3) 0.3526(2) 0.0539(9) Uani 1 d . . H9 H 0.7649(3) 0.8429(3) 0.4049(2) 0.065 Uiso 1 calc R . C10 C 0.8919(3) 0.7978(3) 0.3421(3) 0.0640(10) Uani 1 d . . H10 H 0.9648(3) 0.8357(3) 0.3876(3) 0.077 Uiso 1 calc R . C11 C 0.9052(3) 0.7382(3) 0.2647(3) 0.0611(10) Uani 1 d . . H11 H 0.9868(3) 0.7371(3) 0.2573(3) 0.073 Uiso 1 calc R . C12 C 0.7984(3) 0.6805(3) 0.1987(3) 0.0581(9) Uani 1 d . . H12 H 0.8073(3) 0.6394(3) 0.1467(3) 0.070 Uiso 1 calc R . C13 C 0.6787(3) 0.6835(3) 0.2092(2) 0.0478(8) Uani 1 d . . H13 H 0.6065(3) 0.6437(3) 0.1643(2) 0.057 Uiso 1 calc R . C14 C 0.3585(3) 0.6322(3) -0.1048(2) 0.0430(7) Uani 1 d . . H14 H 0.3351(3) 0.5658(3) -0.1446(2) 0.052 Uiso 1 calc R . C15 C 0.4736(3) 0.6607(3) -0.0286(2) 0.0484(8) Uani 1 d . . H15 H 0.5388(3) 0.6163(3) -0.0092(2) 0.058 Uiso 1 calc R . C16 C 0.4720(3) 0.7683(3) 0.0130(2) 0.0447(8) Uani 1 d . . H16 H 0.5368(3) 0.8075(3) 0.0639(2) 0.054 Uiso 1 calc R . C17 C 0.3559(3) 0.8063(3) -0.0357(2) 0.0398(7) Uani 1 d . . H17 H 0.3299(3) 0.8741(3) -0.0219(2) 0.048 Uiso 1 calc R . C18 C 0.2852(3) 0.7219(2) -0.1103(2) 0.0372(7) Uani 1 d . . C19 C 0.1660(3) 0.7316(2) -0.1827(2) 0.0377(7) Uani 1 d . . C20 C 0.0470(3) 0.7595(2) -0.2027(2) 0.0389(7) Uani 1 d . . C21 C -0.0480(3) 0.7878(3) -0.1574(2) 0.0439(7) Uani 1 d . . C22 C -0.1784(4) 0.7642(4) -0.2019(3) 0.0765(12) Uani 1 d . . H22 H -0.2082(4) 0.7320(4) -0.2640(3) 0.092 Uiso 1 calc R . C23 C -0.2656(4) 0.7878(4) -0.1557(4) 0.094(2) Uani 1 d . . H23 H -0.3538(4) 0.7715(4) -0.1870(4) 0.113 Uiso 1 calc R . C24 C -0.2253(4) 0.8342(4) -0.0651(4) 0.0847(13) Uani 1 d . . H24 H -0.2854(4) 0.8493(4) -0.0345(4) 0.102 Uiso 1 calc R . C25 C -0.0966(4) 0.8588(4) -0.0192(3) 0.0774(12) Uani 1 d . . H25 H -0.0683(4) 0.8911(4) 0.0429(3) 0.093 Uiso 1 calc R . C26 C -0.0088(3) 0.8357(3) -0.0646(2) 0.0584(9) Uani 1 d . . H26 H 0.0792(3) 0.8526(3) -0.0326(2) 0.070 Uiso 1 calc R . C27 C 0.2823(4) 0.9122(3) 0.2991(3) 0.0658(10) Uani 1 d . . C28 C 0.5531(3) 0.9673(3) 0.4015(2) 0.0547(9) Uani 1 d . . C29 C 0.4620(3) 0.9551(3) 0.2079(2) 0.0511(8) Uani 1 d . . C30 C 0.2847(4) 0.6971(4) 0.4005(3) 0.0679(11) Uani 1 d . . C31 C 0.5504(4) 0.7547(3) 0.4967(2) 0.0605(9) Uani 1 d . . C32 C 0.4559(5) 0.5596(4) 0.3743(3) 0.0770(12) Uani 1 d . . C33 C 0.0136(4) 0.8845(3) -0.3748(3) 0.0689(11) Uani 1 d . . C34 C 0.2740(5) 0.8130(3) -0.3225(3) 0.0710(11) Uani 1 d . . C35 C 0.1981(3) 0.9639(3) -0.2070(2) 0.0528(8) Uani 1 d . . C36 C -0.0897(4) 0.6341(3) -0.3949(3) 0.0740(12) Uani 1 d . . C37 C 0.1632(4) 0.5690(3) -0.3400(3) 0.0640(10) Uani 1 d . . C38 C -0.0108(3) 0.5272(3) -0.2378(3) 0.0546(9) Uani 1 d . . O1 O 0.1833(3) 0.9309(3) 0.2950(3) 0.1107(12) Uani 1 d . . O2 O 0.6272(3) 1.0190(2) 0.4631(2) 0.0798(8) Uani 1 d . . O3 O 0.4754(3) 1.0033(2) 0.1481(2) 0.0750(8) Uani 1 d . . O4 O 0.1904(3) 0.6914(4) 0.4156(3) 0.1187(14) Uani 1 d . . O5 O 0.6174(3) 0.7877(3) 0.5686(2) 0.0946(10) Uani 1 d . . O6 O 0.4654(4) 0.4684(3) 0.3680(3) 0.1309(15) Uani 1 d . . O7 O -0.0641(4) 0.9168(3) -0.4296(2) 0.1093(12) Uani 1 d . . O8 O 0.3616(4) 0.7920(3) -0.3422(3) 0.1134(13) Uani 1 d . . O9 O 0.2341(3) 1.0411(2) -0.1558(2) 0.0765(8) Uani 1 d . . O10 O -0.1783(4) 0.6322(3) -0.4562(2) 0.1257(14) Uani 1 d . . O11 O 0.2344(4) 0.5280(3) -0.3660(3) 0.1063(12) Uani 1 d . . O12 O -0.0505(3) 0.4620(2) -0.2000(2) 0.0948(10) Uani 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 Fe 0.0326(2) 0.0398(2) 0.0297(2) 0.0002(2) 0.0071(2) -0.0027(2) Co2 0.0454(3) 0.0548(3) 0.0319(2) 0.0063(2) 0.0070(2) 0.0016(2) Co3 0.0583(3) 0.0431(2) 0.0323(2) 0.0030(2) 0.0112(2) -0.0008(2) Co1 0.0416(2) 0.0413(2) 0.0391(2) -0.0024(2) 0.0089(2) 0.0029(2) Co4 0.0504(3) 0.0426(2) 0.0320(2) -0.0036(2) 0.0074(2) -0.0013(2) C1 0.033(2) 0.054(2) 0.036(2) 0.0052(14) 0.0133(13) 0.0006(14) C2 0.034(2) 0.066(2) 0.038(2) 0.001(2) 0.0066(14) -0.013(2) C3 0.064(2) 0.048(2) 0.040(2) -0.0036(15) 0.015(2) -0.019(2) C4 0.052(2) 0.038(2) 0.040(2) 0.0045(13) 0.0118(15) -0.0018(14) C5 0.035(2) 0.043(2) 0.0297(15) 0.0040(12) 0.0076(12) -0.0010(13) C6 0.038(2) 0.037(2) 0.0311(15) 0.0059(12) 0.0078(13) 0.0029(13) C7 0.041(2) 0.039(2) 0.0297(15) 0.0006(12) 0.0076(13) 0.0040(13) C8 0.037(2) 0.039(2) 0.036(2) 0.0052(13) 0.0046(13) 0.0048(13) C9 0.044(2) 0.063(2) 0.047(2) -0.010(2) 0.005(2) 0.005(2) C10 0.043(2) 0.065(2) 0.071(3) -0.011(2) 0.004(2) 0.001(2) C11 0.040(2) 0.063(2) 0.080(3) 0.001(2) 0.016(2) 0.011(2) C12 0.055(2) 0.063(2) 0.056(2) -0.008(2) 0.015(2) 0.018(2) C13 0.042(2) 0.049(2) 0.044(2) -0.0041(14) 0.0022(14) 0.0089(15) C14 0.042(2) 0.050(2) 0.036(2) -0.0042(14) 0.0133(14) 0.0060(14) C15 0.036(2) 0.064(2) 0.046(2) 0.005(2) 0.0134(15) 0.0107(15) C16 0.035(2) 0.055(2) 0.040(2) 0.0052(14) 0.0090(14) -0.0082(14) C17 0.041(2) 0.042(2) 0.035(2) 0.0041(13) 0.0121(13) -0.0017(13) C18 0.037(2) 0.043(2) 0.0306(15) 0.0007(12) 0.0114(12) -0.0020(13) C19 0.045(2) 0.037(2) 0.0283(15) -0.0004(12) 0.0101(13) -0.0036(13) C20 0.044(2) 0.040(2) 0.0282(15) 0.0015(12) 0.0060(13) 0.0005(13) C21 0.045(2) 0.044(2) 0.043(2) 0.0040(14) 0.0120(15) 0.0085(14) C22 0.047(2) 0.104(3) 0.066(3) -0.019(2) 0.005(2) 0.009(2) C23 0.042(2) 0.127(4) 0.107(4) -0.015(3) 0.018(2) 0.014(2) C24 0.069(3) 0.099(4) 0.101(4) 0.000(3) 0.046(3) 0.024(3) C25 0.082(3) 0.097(3) 0.062(3) -0.007(2) 0.035(2) 0.025(2) C26 0.051(2) 0.075(3) 0.047(2) -0.004(2) 0.014(2) 0.013(2) C27 0.057(2) 0.060(2) 0.081(3) -0.003(2) 0.026(2) 0.004(2) C28 0.060(2) 0.052(2) 0.049(2) -0.001(2) 0.016(2) 0.001(2) C29 0.054(2) 0.044(2) 0.050(2) -0.003(2) 0.009(2) 0.008(2) C30 0.053(2) 0.101(3) 0.046(2) 0.017(2) 0.009(2) 0.004(2) C31 0.058(2) 0.075(3) 0.044(2) 0.015(2) 0.008(2) 0.008(2) C32 0.104(3) 0.067(3) 0.064(3) 0.022(2) 0.030(2) 0.009(2) C33 0.093(3) 0.055(2) 0.042(2) 0.003(2) 0.001(2) -0.001(2) C34 0.098(3) 0.054(2) 0.070(3) 0.003(2) 0.046(2) -0.008(2) C35 0.064(2) 0.049(2) 0.043(2) 0.011(2) 0.012(2) 0.007(2) C36 0.083(3) 0.065(3) 0.050(2) -0.010(2) -0.011(2) 0.004(2) C37 0.085(3) 0.053(2) 0.055(2) -0.008(2) 0.031(2) -0.001(2) C38 0.058(2) 0.047(2) 0.061(2) -0.005(2) 0.027(2) 0.000(2) O1 0.061(2) 0.109(3) 0.172(4) 0.004(2) 0.049(2) 0.023(2) O2 0.087(2) 0.075(2) 0.057(2) -0.0164(14) 0.0049(15) -0.017(2) O3 0.100(2) 0.064(2) 0.066(2) 0.0193(14) 0.029(2) 0.0124(15) O4 0.055(2) 0.205(4) 0.105(3) 0.044(3) 0.032(2) 0.017(2) O5 0.086(2) 0.124(3) 0.046(2) 0.003(2) -0.017(2) 0.004(2) O6 0.200(4) 0.062(2) 0.151(4) 0.032(2) 0.076(3) 0.029(2) O7 0.131(3) 0.089(2) 0.068(2) 0.012(2) -0.034(2) 0.020(2) O8 0.125(3) 0.093(2) 0.158(4) 0.009(2) 0.102(3) 0.004(2) O9 0.100(2) 0.049(2) 0.066(2) -0.0086(14) 0.011(2) -0.0043(14) O10 0.123(3) 0.127(3) 0.077(2) -0.019(2) -0.045(2) 0.025(2) O11 0.134(3) 0.092(2) 0.121(3) -0.013(2) 0.083(3) 0.023(2) O12 0.129(3) 0.064(2) 0.116(3) 0.008(2) 0.083(2) -0.007(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 Fe C2 2.028(3) . ? Fe C17 2.034(3) . ? Fe C16 2.036(3) . ? Fe C15 2.040(3) . ? Fe C1 2.040(3) . ? Fe C3 2.047(3) . ? Fe C4 2.049(3) . ? Fe C14 2.056(3) . ? Fe C18 2.061(3) . ? Fe C5 2.072(3) . ? Co2 C32 1.788(5) . ? Co2 C30 1.805(4) . ? Co2 C31 1.824(4) . ? Co2 C7 1.953(3) . ? Co2 C6 1.997(3) . ? Co2 Co1 2.4681(7) . ? Co3 C35 1.789(4) . ? Co3 C34 1.800(5) . ? Co3 C33 1.819(4) . ? Co3 C20 1.964(3) . ? Co3 C19 1.982(3) . ? Co3 Co4 2.4644(7) . ? Co1 C29 1.789(4) . ? Co1 C27 1.805(4) . ? Co1 C28 1.813(4) . ? Co1 C6 1.955(3) . ? Co1 C7 1.966(3) . ? Co4 C38 1.778(4) . ? Co4 C36 1.813(4) . ? Co4 C37 1.820(4) . ? Co4 C19 1.954(3) . ? Co4 C20 1.956(3) . ? C1 C5 1.417(4) . ? C1 C2 1.421(4) . ? C2 C3 1.394(5) . ? C3 C4 1.419(4) . ? C4 C5 1.429(4) . ? C5 C6 1.450(4) . ? C6 C7 1.335(4) . ? C7 C8 1.449(4) . ? C8 C13 1.383(4) . ? C8 C9 1.390(4) . ? C9 C10 1.358(5) . ? C10 C11 1.375(5) . ? C11 C12 1.367(5) . ? C12 C13 1.365(4) . ? C14 C18 1.414(4) . ? C14 C15 1.416(4) . ? C15 C16 1.410(4) . ? C16 C17 1.408(4) . ? C17 C18 1.431(4) . ? C18 C19 1.450(4) . ? C19 C20 1.332(4) . ? C20 C21 1.453(4) . ? C21 C22 1.371(5) . ? C21 C26 1.388(4) . ? C22 C23 1.372(5) . ? C23 C24 1.353(6) . ? C24 C25 1.358(6) . ? C25 C26 1.369(5) . ? C27 O1 1.114(4) . ? C28 O2 1.125(4) . ? C29 O3 1.132(4) . ? C30 O4 1.112(4) . ? C31 O5 1.123(4) . ? C32 O6 1.122(5) . ? C33 O7 1.119(4) . ? C34 O8 1.129(5) . ? C35 O9 1.123(4) . ? C36 O10 1.115(4) . ? C37 O11 1.113(5) . ? C38 O12 1.119(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 C2 Fe C17 123.67(14) . . ? C2 Fe C16 160.85(14) . . ? C17 Fe C16 40.47(12) . . ? C2 Fe C15 156.60(13) . . ? C17 Fe C15 68.28(13) . . ? C16 Fe C15 40.47(13) . . ? C2 Fe C1 40.87(12) . . ? C17 Fe C1 106.98(12) . . ? C16 Fe C1 124.56(13) . . ? C15 Fe C1 161.59(12) . . ? C2 Fe C3 40.01(14) . . ? C17 Fe C3 160.05(13) . . ? C16 Fe C3 158.13(14) . . ? C15 Fe C3 122.51(15) . . ? C1 Fe C3 68.01(14) . . ? C2 Fe C4 67.94(13) . . ? C17 Fe C4 157.45(12) . . ? C16 Fe C4 122.90(13) . . ? C15 Fe C4 109.05(13) . . ? C1 Fe C4 68.09(13) . . ? C3 Fe C4 40.54(12) . . ? C2 Fe C14 120.90(12) . . ? C17 Fe C14 68.21(12) . . ? C16 Fe C14 67.91(12) . . ? C15 Fe C14 40.44(12) . . ? C1 Fe C14 156.12(12) . . ? C3 Fe C14 108.09(13) . . ? C4 Fe C14 125.27(13) . . ? C2 Fe C18 106.79(12) . . ? C17 Fe C18 40.88(11) . . ? C16 Fe C18 68.08(11) . . ? C15 Fe C18 67.99(12) . . ? C1 Fe C18 120.88(12) . . ? C3 Fe C18 123.69(12) . . ? C4 Fe C18 160.77(12) . . ? C14 Fe C18 40.18(12) . . ? C2 Fe C5 68.12(12) . . ? C17 Fe C5 121.50(12) . . ? C16 Fe C5 108.79(12) . . ? C15 Fe C5 125.73(12) . . ? C1 Fe C5 40.31(11) . . ? C3 Fe C5 68.04(12) . . ? C4 Fe C5 40.57(12) . . ? C14 Fe C5 162.19(12) . . ? C18 Fe C5 156.57(12) . . ? C32 Co2 C30 99.1(2) . . ? C32 Co2 C31 101.0(2) . . ? C30 Co2 C31 101.8(2) . . ? C32 Co2 C7 99.5(2) . . ? C30 Co2 C7 143.76(15) . . ? C31 Co2 C7 104.87(14) . . ? C32 Co2 C6 98.5(2) . . ? C30 Co2 C6 106.88(14) . . ? C31 Co2 C6 142.06(14) . . ? C7 Co2 C6 39.48(11) . . ? C32 Co2 Co1 147.42(13) . . ? C30 Co2 Co1 100.12(13) . . ? C31 Co2 Co1 100.56(12) . . ? C7 Co2 Co1 51.19(9) . . ? C6 Co2 Co1 50.60(8) . . ? C35 Co3 C34 101.9(2) . . ? C35 Co3 C33 99.1(2) . . ? C34 Co3 C33 109.9(2) . . ? C35 Co3 C20 97.78(14) . . ? C34 Co3 C20 135.5(2) . . ? C33 Co3 C20 105.8(2) . . ? C35 Co3 C19 98.29(13) . . ? C34 Co3 C19 97.9(2) . . ? C33 Co3 C19 143.1(2) . . ? C20 Co3 C19 39.46(12) . . ? C35 Co3 Co4 146.38(11) . . ? C34 Co3 Co4 95.94(12) . . ? C33 Co3 Co4 101.24(12) . . ? C20 Co3 Co4 50.91(8) . . ? C19 Co3 Co4 50.73(8) . . ? C29 Co1 C27 98.4(2) . . ? C29 Co1 C28 99.74(15) . . ? C27 Co1 C28 105.5(2) . . ? C29 Co1 C6 101.20(13) . . ? C27 Co1 C6 105.09(15) . . ? C28 Co1 C6 139.67(14) . . ? C29 Co1 C7 102.29(13) . . ? C27 Co1 C7 142.07(15) . . ? C28 Co1 C7 101.98(14) . . ? C6 Co1 C7 39.81(11) . . ? C29 Co1 Co2 150.97(10) . . ? C27 Co1 Co2 99.86(13) . . ? C28 Co1 Co2 96.95(11) . . ? C6 Co1 Co2 52.13(8) . . ? C7 Co1 Co2 50.74(8) . . ? C38 Co4 C36 98.3(2) . . ? C38 Co4 C37 101.5(2) . . ? C36 Co4 C37 103.7(2) . . ? C38 Co4 C19 100.51(14) . . ? C36 Co4 C19 143.3(2) . . ? C37 Co4 C19 103.01(15) . . ? C38 Co4 C20 96.72(14) . . ? C36 Co4 C20 106.9(2) . . ? C37 Co4 C20 141.47(15) . . ? C19 Co4 C20 39.83(12) . . ? C38 Co4 Co3 147.16(11) . . ? C36 Co4 Co3 98.10(13) . . ? C37 Co4 Co3 101.93(12) . . ? C19 Co4 Co3 51.75(8) . . ? C20 Co4 Co3 51.18(9) . . ? C5 C1 C2 108.1(3) . . ? C5 C1 Fe 71.0(2) . . ? C2 C1 Fe 69.1(2) . . ? C3 C2 C1 108.6(3) . . ? C3 C2 Fe 70.7(2) . . ? C1 C2 Fe 70.0(2) . . ? C2 C3 C4 108.2(3) . . ? C2 C3 Fe 69.3(2) . . ? C4 C3 Fe 69.8(2) . . ? C3 C4 C5 108.1(3) . . ? C3 C4 Fe 69.7(2) . . ? C5 C4 Fe 70.6(2) . . ? C1 C5 C4 107.1(3) . . ? C1 C5 C6 126.1(3) . . ? C4 C5 C6 126.7(3) . . ? C1 C5 Fe 68.6(2) . . ? C4 C5 Fe 68.8(2) . . ? C6 C5 Fe 130.1(2) . . ? C7 C6 C5 144.2(3) . . ? C7 C6 Co1 70.5(2) . . ? C5 C6 Co1 136.2(2) . . ? C7 C6 Co2 68.5(2) . . ? C5 C6 Co2 131.1(2) . . ? Co1 C6 Co2 77.27(10) . . ? C6 C7 C8 141.4(3) . . ? C6 C7 Co2 72.1(2) . . ? C8 C7 Co2 135.5(2) . . ? C6 C7 Co1 69.7(2) . . ? C8 C7 Co1 132.4(2) . . ? Co2 C7 Co1 78.07(11) . . ? C13 C8 C9 118.3(3) . . ? C13 C8 C7 120.1(3) . . ? C9 C8 C7 121.6(3) . . ? C10 C9 C8 120.4(3) . . ? C9 C10 C11 120.5(3) . . ? C12 C11 C10 119.9(3) . . ? C13 C12 C11 119.9(3) . . ? C12 C13 C8 121.0(3) . . ? C18 C14 C15 108.2(3) . . ? C18 C14 Fe 70.1(2) . . ? C15 C14 Fe 69.2(2) . . ? C16 C15 C14 108.0(3) . . ? C16 C15 Fe 69.6(2) . . ? C14 C15 Fe 70.4(2) . . ? C17 C16 C15 108.5(3) . . ? C17 C16 Fe 69.7(2) . . ? C15 C16 Fe 69.9(2) . . ? C16 C17 C18 107.8(3) . . ? C16 C17 Fe 69.8(2) . . ? C18 C17 Fe 70.6(2) . . ? C14 C18 C17 107.5(3) . . ? C14 C18 C19 126.5(3) . . ? C17 C18 C19 125.8(3) . . ? C14 C18 Fe 69.7(2) . . ? C17 C18 Fe 68.6(2) . . ? C19 C18 Fe 131.0(2) . . ? C20 C19 C18 146.9(3) . . ? C20 C19 Co4 70.2(2) . . ? C18 C19 Co4 135.7(2) . . ? C20 C19 Co3 69.5(2) . . ? C18 C19 Co3 128.0(2) . . ? Co4 C19 Co3 77.51(10) . . ? C19 C20 C21 141.3(3) . . ? C19 C20 Co4 70.0(2) . . ? C21 C20 Co4 133.9(2) . . ? C19 C20 Co3 71.0(2) . . ? C21 C20 Co3 134.9(2) . . ? Co4 C20 Co3 77.92(11) . . ? C22 C21 C26 117.4(3) . . ? C22 C21 C20 122.1(3) . . ? C26 C21 C20 120.5(3) . . ? C21 C22 C23 120.6(4) . . ? C24 C23 C22 121.1(4) . . ? C23 C24 C25 119.7(4) . . ? C24 C25 C26 119.8(4) . . ? C25 C26 C21 121.5(4) . . ? O1 C27 Co1 178.1(4) . . ? O2 C28 Co1 176.8(3) . . ? O3 C29 Co1 179.8(4) . . ? O4 C30 Co2 178.1(4) . . ? O5 C31 Co2 178.4(4) . . ? O6 C32 Co2 177.8(4) . . ? O7 C33 Co3 177.5(4) . . ? O8 C34 Co3 173.7(4) . . ? O9 C35 Co3 175.8(3) . . ? O10 C36 Co4 178.3(5) . . ? O11 C37 Co4 177.8(4) . . ? O12 C38 Co4 176.7(3) . . ? _refine_diff_density_max 0.354 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.079 #===END