# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Manabendra Ray' _publ_contact_author_email MANABRAY@IITG.ERNET.IN _publ_section_title ; Bowl shaped chiral cavity in bis-copper(II) complexes of ferrocenyl-methyl-L-tyrosine and its interaction with achiral guests ; loop_ _publ_author_name 'Manabendra Ray' 'Subash Chandra Sahoo' # Attachment 'StructuresCIF.cif' data_1_[Cu(S-fTyr)2(MeCN)2]2MeCN _database_code_depnum_ccdc_archive 'CCDC 708590' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C44 H46 Cu Fe2 N4 O6, 2(C2 H3 N)' _chemical_formula_sum 'C48 H52 Cu Fe2 N6 O6' #Hydrogen atoms attached to one acetonitrile in 1 #could not be located or fixed. Thus the calculated #and reported formula differ. _chemical_compound_source synthesized _exptl_crystal_recrystallization_method 'methanol, diethylether' _chemical_melting_point ? _exptl_crystal_description rod _exptl_crystal_colour green _diffrn_ambient_temperature 296(2) _chemical_formula_weight 983.18 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 43 21 2' _symmetry_int_tables_number 96 _chemical_absolute_configuration syn _symmetry_space_group_name_Hall 'P 4nw 2abw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 10.73030(10) _cell_length_b 10.73030(10) _cell_length_c 41.1772(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4741.12(10) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9502 _cell_measurement_theta_min 3.80 _cell_measurement_theta_max 23.98 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 1.101 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53882 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.01 _reflns_number_total 5162 _reflns_number_gt 4148 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics wingx _computing_publication_material wingx _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^ > 2\s(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^)+(0.0367P)^2^+0.4464P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.019(14) _refine_ls_number_reflns 5162 _refine_ls_number_parameters 291 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.64274(3) 0.64274(3) 0.0000 0.04455(12) Uani 1 2 d S . . Fe1 Fe 0.64017(4) 0.49589(3) 0.142393(8) 0.04146(10) Uani 1 1 d . . . C3 C 0.5168(3) 0.6332(3) 0.15516(6) 0.0500(6) Uani 1 1 d . . . H2 H 0.4589 0.6306 0.1720 0.060 Uiso 1 1 calc R . . C4 C 0.6409(3) 0.6772(2) 0.15751(7) 0.0528(7) Uani 1 1 d . . . H1 H 0.6790 0.7080 0.1761 0.063 Uiso 1 1 calc R . . C2 C 0.4961(3) 0.5941(2) 0.12288(6) 0.0451(6) Uani 1 1 d . . . H3 H 0.4223 0.5612 0.1147 0.054 Uiso 1 1 calc R . . C1 C 0.6081(2) 0.6135(2) 0.10489(6) 0.0419(6) Uani 1 1 d . . . C5 C 0.6967(3) 0.6661(2) 0.12649(6) 0.0470(7) Uani 1 1 d . . . H5 H 0.7777 0.6892 0.1212 0.056 Uiso 1 1 calc R . . C8 C 0.6089(3) 0.3419(3) 0.17041(9) 0.0663(9) Uani 1 1 d . . . H7 H 0.5455 0.3327 0.1856 0.080 Uiso 1 1 calc R . . C9 C 0.7286(3) 0.3884(3) 0.17650(8) 0.0650(9) Uani 1 1 d . . . H6 H 0.7583 0.4156 0.1965 0.078 Uiso 1 1 calc R . . C7 C 0.6017(4) 0.3115(3) 0.13705(10) 0.0758(11) Uani 1 1 d . . . H8 H 0.5328 0.2787 0.1263 0.091 Uiso 1 1 calc R . . C6 C 0.7191(4) 0.3402(3) 0.12287(8) 0.0683(10) Uani 1 1 d . . . H9 H 0.7410 0.3299 0.1012 0.082 Uiso 1 1 calc R . . C10 C 0.7957(3) 0.3870(3) 0.14756(8) 0.0644(9) Uani 1 1 d . . . H10 H 0.8778 0.4129 0.1450 0.077 Uiso 1 1 calc R . . C11 C 0.6275(3) 0.5824(3) 0.06979(6) 0.0472(7) Uani 1 1 d . . . H11A H 0.7117 0.5509 0.0671 0.057 Uiso 1 1 calc R . . H11B H 0.5707 0.5158 0.0639 0.057 Uiso 1 1 calc R . . N1 N 0.60902(19) 0.68755(19) 0.04674(5) 0.0392(5) Uani 1 1 d . . . H01 H 0.6654 0.7473 0.0522 0.047 Uiso 1 1 calc R . . C12 C 0.4837(2) 0.7467(2) 0.04864(6) 0.0388(6) Uani 1 1 d . . . H12 H 0.4258 0.6838 0.0571 0.047 Uiso 1 1 calc R . . C15 C 0.5718(2) 0.9595(2) 0.06405(6) 0.0395(6) Uani 1 1 d . . . C14 C 0.4774(2) 0.8590(3) 0.07149(6) 0.0420(6) Uani 1 1 d . . . H14A H 0.3946 0.8948 0.0703 0.050 Uiso 1 1 calc R . . H14B H 0.4902 0.8303 0.0936 0.050 Uiso 1 1 calc R . . C16 C 0.5615(3) 1.0368(3) 0.03708(7) 0.0508(7) Uani 1 1 d . . . H15 H 0.4947 1.0263 0.0230 0.061 Uiso 1 1 calc R . . C17 C 0.6482(3) 1.1289(3) 0.03079(6) 0.0520(7) Uani 1 1 d . . . H16 H 0.6391 1.1794 0.0126 0.062 Uiso 1 1 calc R . . C18 C 0.7478(2) 1.1464(3) 0.05122(6) 0.0460(6) Uani 1 1 d . . . C19 C 0.7598(3) 1.0715(2) 0.07840(7) 0.0508(7) Uani 1 1 d . . . H18 H 0.8263 1.0830 0.0926 0.061 Uiso 1 1 calc R . . C20 C 0.6722(3) 0.9792(2) 0.08444(6) 0.0459(7) Uani 1 1 d . . . H19 H 0.6813 0.9293 0.1027 0.055 Uiso 1 1 calc R . . O3 O 0.8365(2) 1.2361(2) 0.04670(5) 0.0645(6) Uani 1 1 d . . . H1A H 0.8305 1.2646 0.0283 0.097 Uiso 1 1 calc R . . O1 O 0.76042(18) 0.51098(18) 0.00932(4) 0.0522(5) Uani 1 1 d . . . O2 O 0.33546(17) 0.83156(19) 0.01198(5) 0.0570(5) Uani 1 1 d . . . C13 C 0.4387(3) 0.7824(3) 0.01456(7) 0.0434(6) Uani 1 1 d . . . N2 N 0.4757(3) 0.4757(3) 0.0000 0.0890(14) Uani 1 2 d SDU . . C22 C 0.4052(5) 0.4052(5) 0.0000 0.125(3) Uani 1 2 d SDU . . C21 C 0.3066(5) 0.3066(5) 0.0000 0.209(5) Uani 1 2 d SDU . . C24 C 0.8925(4) 0.8925(4) 0.0000 0.0925(18) Uani 1 2 d SU . . C23 C 0.9869(4) 0.9869(4) 0.0000 0.140(3) Uani 1 2 d SU . . H24A H 0.9485 1.0676 -0.0013 0.209 Uiso 0.50 1 calc PR . . H24B H 1.0407 0.9753 -0.0184 0.209 Uiso 0.50 1 calc PR . . H24C H 1.0348 0.9812 0.0196 0.209 Uiso 0.50 1 calc PR . . N3 N 0.8182(3) 0.8182(3) 0.0000 0.124(2) Uani 1 2 d SU . . N4 N 0.2417(5) 0.5049(5) 0.06072(19) 0.197(3) Uani 1 1 d U . . C25 C 0.0074(5) 0.5032(5) 0.06679(12) 0.1320(17) Uani 1 1 d U . . H25A H -0.0249 0.4257 0.0588 0.198 Uiso 1 1 calc R . . H25B H -0.0284 0.5709 0.0547 0.198 Uiso 1 1 calc R . . H25C H -0.0135 0.5118 0.0893 0.198 Uiso 1 1 calc R . . C26 C 0.1377(6) 0.5048(4) 0.06317(13) 0.1133(16) Uani 1 1 d U . . 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 Cu1 0.04919(17) 0.04919(17) 0.0353(2) 0.00107(14) -0.00107(14) 0.0133(2) Fe1 0.0457(2) 0.0369(2) 0.04177(19) 0.00338(17) -0.00247(18) 0.00071(18) C3 0.0549(18) 0.0484(16) 0.0467(14) 0.0041(13) 0.0071(13) 0.0117(14) C4 0.0684(19) 0.0424(16) 0.0475(15) -0.0040(12) -0.0077(15) 0.0025(15) C2 0.0417(14) 0.0450(14) 0.0485(15) 0.0080(11) -0.0035(13) -0.0024(13) C1 0.0449(16) 0.0401(15) 0.0408(13) 0.0048(11) -0.0012(12) 0.0019(11) C5 0.0452(15) 0.0386(15) 0.0573(17) 0.0083(13) -0.0044(13) -0.0032(12) C8 0.072(2) 0.0482(18) 0.079(2) 0.0239(17) 0.0109(17) 0.0029(16) C9 0.072(2) 0.061(2) 0.062(2) 0.0129(16) -0.0124(17) 0.0117(17) C7 0.083(3) 0.0375(17) 0.107(3) 0.0056(18) -0.030(2) -0.0078(16) C6 0.094(3) 0.0415(18) 0.069(2) -0.0072(16) 0.0095(19) 0.0073(18) C10 0.0582(19) 0.0469(18) 0.088(2) 0.0050(17) 0.0003(18) 0.0097(15) C11 0.0548(17) 0.0448(15) 0.0421(14) 0.0053(11) 0.0011(13) 0.0093(14) N1 0.0369(12) 0.0416(12) 0.0390(11) 0.0024(9) -0.0006(9) 0.0024(9) C12 0.0328(13) 0.0398(14) 0.0439(13) 0.0023(11) 0.0017(11) -0.0003(11) C15 0.0412(15) 0.0395(15) 0.0380(13) -0.0005(11) 0.0011(11) 0.0029(12) C14 0.0386(14) 0.0448(15) 0.0424(13) 0.0020(12) 0.0072(11) 0.0008(13) C16 0.0534(18) 0.0533(18) 0.0456(15) 0.0057(13) -0.0111(13) -0.0060(14) C17 0.0598(17) 0.0501(16) 0.0462(15) 0.0147(13) -0.0124(14) -0.0050(16) C18 0.0477(15) 0.0340(14) 0.0562(16) 0.0059(13) -0.0083(12) -0.0009(13) C19 0.0597(19) 0.0372(15) 0.0555(17) 0.0054(13) -0.0196(14) -0.0019(13) C20 0.0593(18) 0.0373(15) 0.0411(14) 0.0061(11) -0.0049(12) 0.0034(12) O3 0.0693(14) 0.0511(12) 0.0731(14) 0.0242(10) -0.0223(11) -0.0200(11) O1 0.0572(12) 0.0571(12) 0.0422(10) 0.0032(9) -0.0012(9) 0.0173(10) O2 0.0414(11) 0.0683(14) 0.0614(12) -0.0075(10) -0.0104(9) 0.0132(10) C13 0.0417(15) 0.0420(15) 0.0465(16) -0.0029(12) -0.0053(13) -0.0006(12) N2 0.089(2) 0.089(2) 0.090(3) -0.001(2) 0.001(2) -0.030(3) C22 0.119(3) 0.119(3) 0.136(6) 0.003(4) -0.003(4) -0.019(4) C21 0.175(6) 0.175(6) 0.277(12) -0.045(7) 0.045(7) -0.091(7) C24 0.085(2) 0.085(2) 0.107(4) -0.029(3) 0.029(3) -0.019(3) C23 0.142(4) 0.142(4) 0.136(6) -0.064(5) 0.064(5) -0.085(5) N3 0.095(2) 0.095(2) 0.181(6) -0.041(3) 0.041(3) -0.031(3) N4 0.097(3) 0.137(4) 0.356(9) 0.002(5) 0.009(5) -0.022(4) C25 0.097(3) 0.125(4) 0.174(5) -0.001(4) -0.005(4) -0.019(4) C26 0.098(3) 0.076(3) 0.167(5) 0.001(3) -0.005(4) -0.016(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.9342(18) . ? Cu1 O1 1.9342(18) 7 ? Cu1 N1 2.017(2) 7 ? Cu1 N1 2.017(2) . ? Fe1 C1 2.024(2) . ? Fe1 C5 2.032(2) . ? Fe1 C7 2.033(3) . ? Fe1 C2 2.036(3) . ? Fe1 C6 2.038(3) . ? Fe1 C8 2.042(3) . ? Fe1 C4 2.043(3) . ? Fe1 C10 2.048(3) . ? Fe1 C3 2.050(3) . ? Fe1 C9 2.050(3) . ? C3 C2 1.412(4) . ? C3 C4 1.416(4) . ? C3 H2 0.9300 . ? C4 C5 1.416(4) . ? C4 H1 0.9300 . ? C2 C1 1.427(4) . ? C2 H3 0.9300 . ? C1 C5 1.419(4) . ? C1 C11 1.498(3) . ? C5 H5 0.9300 . ? C8 C9 1.400(5) . ? C8 C7 1.414(5) . ? C8 H7 0.9300 . ? C9 C10 1.392(4) . ? C9 H6 0.9300 . ? C7 C6 1.422(5) . ? C7 H8 0.9300 . ? C6 C10 1.400(5) . ? C6 H9 0.9300 . ? C10 H10 0.9300 . ? C11 N1 1.488(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? N1 C12 1.490(3) . ? N1 H01 0.9100 . ? C12 C14 1.530(3) . ? C12 C13 1.532(3) . ? C12 H12 0.9800 . ? C15 C20 1.382(4) . ? C15 C16 1.390(4) . ? C15 C14 1.511(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C16 C17 1.382(4) . ? C16 H15 0.9300 . ? C17 C18 1.373(4) . ? C17 H16 0.9300 . ? C18 O3 1.367(3) . ? C18 C19 1.384(3) . ? C19 C20 1.387(4) . ? C19 H18 0.9300 . ? C20 H19 0.9300 . ? O3 H1A 0.8200 . ? O1 C13 1.275(3) 7 ? O2 C13 1.231(3) . ? C13 O1 1.275(3) 7 ? N2 C22 1.069(7) . ? C22 C21 1.496(10) . ? C24 N3 1.127(6) . ? C24 C23 1.433(8) . ? C23 H24A 0.9600 . ? C23 H24B 0.9600 . ? C23 H24C 0.9600 . ? N4 C26 1.121(6) . ? C25 C26 1.406(7) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O1 173.67(13) . 7 ? O1 Cu1 N1 84.41(7) . 7 ? O1 Cu1 N1 95.85(7) 7 7 ? O1 Cu1 N1 95.85(7) . . ? O1 Cu1 N1 84.41(7) 7 . ? N1 Cu1 N1 175.21(13) 7 . ? C1 Fe1 C5 40.94(10) . . ? C1 Fe1 C7 119.34(13) . . ? C5 Fe1 C7 154.16(15) . . ? C1 Fe1 C2 41.14(10) . . ? C5 Fe1 C2 68.56(11) . . ? C7 Fe1 C2 107.87(13) . . ? C1 Fe1 C6 106.31(12) . . ? C5 Fe1 C6 119.01(13) . . ? C7 Fe1 C6 40.90(14) . . ? C2 Fe1 C6 125.72(12) . . ? C1 Fe1 C8 155.15(13) . . ? C5 Fe1 C8 163.24(14) . . ? C7 Fe1 C8 40.60(14) . . ? C2 Fe1 C8 121.13(12) . . ? C6 Fe1 C8 68.17(14) . . ? C1 Fe1 C4 68.84(11) . . ? C5 Fe1 C4 40.66(11) . . ? C7 Fe1 C4 163.86(15) . . ? C2 Fe1 C4 68.29(11) . . ? C6 Fe1 C4 154.06(15) . . ? C8 Fe1 C4 126.78(14) . . ? C1 Fe1 C10 125.00(12) . . ? C5 Fe1 C10 107.62(12) . . ? C7 Fe1 C10 67.75(14) . . ? C2 Fe1 C10 162.69(12) . . ? C6 Fe1 C10 40.08(13) . . ? C8 Fe1 C10 67.27(13) . . ? C4 Fe1 C10 120.58(13) . . ? C1 Fe1 C3 68.74(10) . . ? C5 Fe1 C3 68.26(11) . . ? C7 Fe1 C3 126.61(15) . . ? C2 Fe1 C3 40.43(10) . . ? C6 Fe1 C3 163.51(14) . . ? C8 Fe1 C3 109.31(13) . . ? C4 Fe1 C3 40.48(12) . . ? C10 Fe1 C3 155.48(12) . . ? C1 Fe1 C9 162.22(13) . . ? C5 Fe1 C9 126.01(13) . . ? C7 Fe1 C9 67.71(14) . . ? C2 Fe1 C9 155.91(13) . . ? C6 Fe1 C9 67.48(14) . . ? C8 Fe1 C9 40.01(14) . . ? C4 Fe1 C9 108.98(13) . . ? C10 Fe1 C9 39.73(13) . . ? C3 Fe1 C9 121.85(12) . . ? C2 C3 C4 108.1(2) . . ? C2 C3 Fe1 69.25(16) . . ? C4 C3 Fe1 69.49(16) . . ? C2 C3 H2 125.9 . . ? C4 C3 H2 125.9 . . ? Fe1 C3 H2 126.9 . . ? C3 C4 C5 108.0(2) . . ? C3 C4 Fe1 70.03(16) . . ? C5 C4 Fe1 69.28(15) . . ? C3 C4 H1 126.0 . . ? C5 C4 H1 126.0 . . ? Fe1 C4 H1 126.2 . . ? C3 C2 C1 108.2(2) . . ? C3 C2 Fe1 70.32(16) . . ? C1 C2 Fe1 68.99(15) . . ? C3 C2 H3 125.9 . . ? C1 C2 H3 125.9 . . ? Fe1 C2 H3 126.4 . . ? C5 C1 C2 107.3(2) . . ? C5 C1 C11 126.9(2) . . ? C2 C1 C11 125.8(2) . . ? C5 C1 Fe1 69.85(14) . . ? C2 C1 Fe1 69.87(14) . . ? C11 C1 Fe1 124.96(18) . . ? C4 C5 C1 108.4(2) . . ? C4 C5 Fe1 70.05(15) . . ? C1 C5 Fe1 69.21(14) . . ? C4 C5 H5 125.8 . . ? C1 C5 H5 125.8 . . ? Fe1 C5 H5 126.5 . . ? C9 C8 C7 107.9(3) . . ? C9 C8 Fe1 70.29(17) . . ? C7 C8 Fe1 69.33(17) . . ? C9 C8 H7 126.1 . . ? C7 C8 H7 126.1 . . ? Fe1 C8 H7 125.9 . . ? C10 C9 C8 108.5(3) . . ? C10 C9 Fe1 70.05(18) . . ? C8 C9 Fe1 69.70(17) . . ? C10 C9 H6 125.8 . . ? C8 C9 H6 125.8 . . ? Fe1 C9 H6 126.1 . . ? C8 C7 C6 107.5(3) . . ? C8 C7 Fe1 70.07(18) . . ? C6 C7 Fe1 69.75(18) . . ? C8 C7 H8 126.3 . . ? C6 C7 H8 126.3 . . ? Fe1 C7 H8 125.5 . . ? C10 C6 C7 107.4(3) . . ? C10 C6 Fe1 70.34(17) . . ? C7 C6 Fe1 69.35(18) . . ? C10 C6 H9 126.3 . . ? C7 C6 H9 126.3 . . ? Fe1 C6 H9 125.6 . . ? C9 C10 C6 108.8(3) . . ? C9 C10 Fe1 70.22(18) . . ? C6 C10 Fe1 69.58(18) . . ? C9 C10 H10 125.6 . . ? C6 C10 H10 125.6 . . ? Fe1 C10 H10 126.2 . . ? N1 C11 C1 115.3(2) . . ? N1 C11 H11A 108.5 . . ? C1 C11 H11A 108.5 . . ? N1 C11 H11B 108.5 . . ? C1 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? C11 N1 C12 114.24(19) . . ? C11 N1 Cu1 113.82(15) . . ? C12 N1 Cu1 108.28(14) . . ? C11 N1 H01 106.7 . . ? C12 N1 H01 106.7 . . ? Cu1 N1 H01 106.7 . . ? N1 C12 C14 114.0(2) . . ? N1 C12 C13 110.05(19) . . ? C14 C12 C13 110.7(2) . . ? N1 C12 H12 107.3 . . ? C14 C12 H12 107.3 . . ? C13 C12 H12 107.3 . . ? C20 C15 C16 117.1(2) . . ? C20 C15 C14 120.6(2) . . ? C16 C15 C14 122.3(2) . . ? C15 C14 C12 114.1(2) . . ? C15 C14 H14A 108.7 . . ? C12 C14 H14A 108.7 . . ? C15 C14 H14B 108.7 . . ? C12 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C17 C16 C15 121.5(3) . . ? C17 C16 H15 119.2 . . ? C15 C16 H15 119.2 . . ? C18 C17 C16 120.5(2) . . ? C18 C17 H16 119.8 . . ? C16 C17 H16 119.8 . . ? O3 C18 C17 123.7(2) . . ? O3 C18 C19 117.0(2) . . ? C17 C18 C19 119.2(3) . . ? C18 C19 C20 119.8(3) . . ? C18 C19 H18 120.1 . . ? C20 C19 H18 120.1 . . ? C15 C20 C19 121.9(2) . . ? C15 C20 H19 119.1 . . ? C19 C20 H19 119.1 . . ? C18 O3 H1A 109.5 . . ? C13 O1 Cu1 114.36(16) 7 . ? O2 C13 O1 124.1(3) . 7 ? O2 C13 C12 118.0(2) . . ? O1 C13 C12 118.0(2) 7 . ? N2 C22 C21 180.000(1) . . ? N3 C24 C23 180.0(6) . . ? C24 C23 H24A 109.5 . . ? C24 C23 H24B 109.5 . . ? H24A C23 H24B 109.5 . . ? C24 C23 H24C 109.5 . . ? H24A C23 H24C 109.5 . . ? H24B C23 H24C 109.5 . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N4 C26 C25 178.9(8) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.01 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.182 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.041 data_2_[Cu(S-fTyr)2(Pyz)] _database_code_depnum_ccdc_archive 'CCDC 708591' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H44 Cu Fe2 N4 O6' _chemical_formula_sum 'C44 H44 Cu Fe2 N4 O6' _chemical_formula_weight 900.07 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' _chemical_absolute_configuration syn _symmetry_space_group_name_Hall 'P 2 2ab' _symmetry_int_tables_number 18 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 10.97160(10) _cell_length_b 11.74050(10) _cell_length_c 15.2578(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1965.39(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9625 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 27.91 _exptl_crystal_description rod _exptl_crystal_colour black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 930 _exptl_absorpt_coefficient_mu 1.320 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16568 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.28 _reflns_number_total 4515 _reflns_number_gt 4121 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of 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^)+(0.0400P)^2^+1.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.014(15) _refine_ls_number_reflns 4515 _refine_ls_number_parameters 264 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0822 _refine_ls_wR_factor_gt 0.0809 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.0000 0.0000 0.79665(3) 0.03346(11) Uani 1 2 d S . . Fe1 Fe 0.67789(4) 0.33643(3) 0.59787(2) 0.03470(10) Uani 1 1 d . . . C1 C 0.5231(3) 0.2407(3) 0.5822(2) 0.0618(10) Uani 1 1 d . . . H1 H 0.4733 0.2078 0.6291 0.074 Uiso 1 1 calc R . . C4 C 0.6691(4) 0.2634(3) 0.4770(2) 0.0592(9) Uani 1 1 d . . . H4 H 0.7386 0.2485 0.4383 0.071 Uiso 1 1 calc R . . C3 C 0.5987(3) 0.3652(3) 0.4789(2) 0.0546(9) Uani 1 1 d . . . H3 H 0.6101 0.4324 0.4416 0.065 Uiso 1 1 calc R . . C2 C 0.5079(3) 0.3502(3) 0.5434(2) 0.0561(8) Uani 1 1 d . . . H2 H 0.4458 0.4064 0.5597 0.067 Uiso 1 1 calc R . . C5 C 0.6231(4) 0.1885(3) 0.5404(2) 0.0620(10) Uani 1 1 d . . . H5 H 0.6551 0.1125 0.5535 0.074 Uiso 1 1 calc R . . C7 C 0.7882(3) 0.4715(3) 0.6300(2) 0.0482(8) Uani 1 1 d . . . H7 H 0.8014 0.5398 0.5944 0.058 Uiso 1 1 calc R . . C6 C 0.8557(3) 0.3689(2) 0.62480(18) 0.0407(7) Uani 1 1 d . . . H6 H 0.9246 0.3546 0.5854 0.049 Uiso 1 1 calc R . . C9 C 0.7076(2) 0.3462(3) 0.72931(16) 0.0374(6) Uani 1 1 d . . . H9 H 0.6555 0.3130 0.7748 0.045 Uiso 1 1 calc R . . C8 C 0.6963(3) 0.4572(2) 0.69441(18) 0.0440(7) Uani 1 1 d . . . H8 H 0.6350 0.5139 0.7112 0.053 Uiso 1 1 calc R . . C10 C 0.8062(2) 0.2899(2) 0.68640(16) 0.0333(5) Uani 1 1 d . . . C11 C 0.8492(3) 0.1715(2) 0.70359(19) 0.0388(5) Uani 1 1 d . . . H11A H 0.8809 0.1398 0.6495 0.047 Uiso 1 1 calc R . . H11B H 0.7799 0.1254 0.7211 0.047 Uiso 1 1 calc R . . C12 C 0.9450(2) -0.2348(2) 0.75582(17) 0.0320(5) Uani 1 1 d . . . H12 H 0.9450 -0.2519 0.6929 0.038 Uiso 1 1 calc R . . C13 C 0.9482(3) -0.3496(2) 0.80354(18) 0.0364(5) Uani 1 1 d . . . H13A H 0.8724 -0.3895 0.7924 0.044 Uiso 1 1 calc R . . H13B H 1.0138 -0.3952 0.7793 0.044 Uiso 1 1 calc R . . C14 C 0.9663(2) -0.3402(2) 0.90139(17) 0.0349(5) Uani 1 1 d . . . C15 C 1.0755(3) -0.3671(2) 0.9409(2) 0.0396(6) Uani 1 1 d . . . H15 H 1.1409 -0.3889 0.9060 0.047 Uiso 1 1 calc R . . C16 C 1.0912(3) -0.3627(2) 1.0309(2) 0.0419(7) Uani 1 1 d . . . H16 H 1.1656 -0.3829 1.0556 0.050 Uiso 1 1 calc R . . C19 C 0.8700(3) -0.3059(3) 0.9570(2) 0.0468(7) Uani 1 1 d . . . H19 H 0.7950 -0.2866 0.9328 0.056 Uiso 1 1 calc R . . C17 C 0.9954(3) -0.3280(3) 1.08426(18) 0.0457(6) Uani 1 1 d . . . C18 C 0.8857(3) -0.3008(3) 1.0458(2) 0.0527(8) Uani 1 1 d . . . H18 H 0.8208 -0.2785 1.0811 0.063 Uiso 1 1 calc R . . N1 N 0.9455(2) 0.1627(2) 0.77278(14) 0.0300(4) Uani 1 1 d . . . N2 N 1.0000 0.0000 0.9484(2) 0.0518(9) Uani 1 2 d S . . O2 O 0.73012(19) -0.2180(2) 0.76783(16) 0.0509(6) Uani 1 1 d . . . O1 O 0.83758(18) -0.06201(15) 0.79244(15) 0.0446(5) Uani 1 1 d . . . C20 C 0.8280(3) -0.1669(2) 0.77413(15) 0.0358(5) Uani 1 1 d . . . N3 N 1.0000 0.0000 1.1326(3) 0.0778(13) Uani 1 2 d S . . C25 C 1.0949(4) -0.0276(4) 0.9958(3) 0.0675(11) Uani 1 1 d . . . H25 H 1.1664 -0.0465 0.9666 0.081 Uiso 1 1 calc R . . C24 C 1.0960(4) -0.0304(4) 1.0851(3) 0.0775(13) Uani 1 1 d . . . H24 H 1.1664 -0.0543 1.1137 0.093 Uiso 1 1 calc R . . O3 O 1.0047(3) -0.3224(3) 1.17320(14) 0.0676(7) Uani 1 1 d . . . H6A H 1.0729 -0.3432 1.1883 0.101 Uiso 1 1 calc R . . H5X H 0.918(3) 0.184(3) 0.815(2) 0.032(8) 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 Cu1 0.0299(2) 0.0274(2) 0.0431(2) 0.000 0.000 0.00393(18) Fe1 0.0374(2) 0.03867(19) 0.02803(16) -0.00333(15) -0.00725(15) 0.00790(16) C1 0.056(2) 0.072(2) 0.057(2) -0.0067(17) -0.0182(17) -0.0145(17) C4 0.059(2) 0.077(2) 0.0415(17) -0.0239(16) -0.0151(16) 0.0189(19) C3 0.056(2) 0.072(2) 0.0354(15) -0.0047(14) -0.0179(14) 0.0142(16) C2 0.0441(18) 0.074(2) 0.0506(17) -0.0144(15) -0.0177(16) 0.0141(18) C5 0.076(3) 0.050(2) 0.060(2) -0.0162(16) -0.0285(19) 0.0087(17) C7 0.059(2) 0.0421(18) 0.0434(15) 0.0108(12) -0.0148(14) -0.0044(13) C6 0.0398(17) 0.0489(16) 0.0334(13) 0.0062(11) -0.0034(12) -0.0009(12) C9 0.0377(15) 0.0460(15) 0.0284(12) 0.0003(11) -0.0024(10) 0.0016(12) C8 0.0553(19) 0.0422(14) 0.0345(13) -0.0069(11) -0.0116(14) 0.0134(12) C10 0.0320(14) 0.0383(13) 0.0295(12) 0.0007(9) -0.0074(11) 0.0024(10) C11 0.0384(15) 0.0358(12) 0.0423(13) -0.0020(11) -0.0128(12) 0.0012(11) C12 0.0326(13) 0.0334(13) 0.0300(12) -0.0035(10) 0.0017(10) 0.0009(10) C13 0.0398(14) 0.0294(13) 0.0398(13) -0.0041(11) 0.0057(12) -0.0044(10) C14 0.0377(15) 0.0274(11) 0.0396(13) 0.0022(11) 0.0059(11) -0.0038(10) C15 0.0338(16) 0.0357(15) 0.0491(16) -0.0028(11) 0.0078(12) 0.0006(10) C16 0.0340(16) 0.0445(17) 0.0470(16) -0.0039(12) -0.0025(12) 0.0008(11) C19 0.0379(17) 0.060(2) 0.0424(15) 0.0004(13) 0.0023(13) 0.0087(13) C17 0.0379(15) 0.0569(16) 0.0423(14) -0.0015(13) -0.0003(14) 0.0007(15) C18 0.0406(18) 0.075(2) 0.0420(16) -0.0046(14) 0.0073(14) 0.0093(15) N1 0.0306(11) 0.0287(10) 0.0308(11) -0.0003(9) -0.0025(9) 0.0021(9) N2 0.047(2) 0.070(2) 0.0382(18) 0.000 0.000 0.005(2) O2 0.0326(11) 0.0563(13) 0.0637(15) -0.0087(11) 0.0029(10) -0.0084(9) O1 0.0319(10) 0.0357(10) 0.0661(13) 0.0001(9) 0.0030(10) 0.0032(8) C20 0.0333(14) 0.0413(13) 0.0328(12) 0.0018(11) 0.0017(11) 0.0006(13) N3 0.076(3) 0.094(3) 0.063(3) 0.000 0.000 0.006(3) C25 0.057(2) 0.085(3) 0.061(2) -0.0033(19) 0.0018(18) 0.0053(19) C24 0.064(3) 0.114(4) 0.054(2) -0.005(2) -0.005(2) 0.014(2) O3 0.0452(13) 0.114(2) 0.0433(11) -0.0088(13) -0.0014(11) 0.0109(16) _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 Cu1 O1 1.926(2) . ? Cu1 O1 1.926(2) 2_755 ? Cu1 N1 2.035(2) 2_755 ? Cu1 N1 2.035(2) . ? Cu1 N2 2.316(4) . ? Fe1 C10 2.026(2) . ? Fe1 C6 2.030(3) . ? Fe1 C9 2.035(2) . ? Fe1 C5 2.036(3) . ? Fe1 C4 2.036(3) . ? Fe1 C3 2.041(3) . ? Fe1 C2 2.048(3) . ? Fe1 C1 2.050(4) . ? Fe1 C7 2.054(3) . ? Fe1 C8 2.054(3) . ? C1 C5 1.409(6) . ? C1 C2 1.425(5) . ? C1 H1 0.9800 . ? C4 C5 1.402(6) . ? C4 C3 1.424(5) . ? C4 H4 0.9800 . ? C3 C2 1.412(5) . ? C3 H3 0.9800 . ? C2 H2 0.9800 . ? C5 H5 0.9800 . ? C7 C6 1.416(4) . ? C7 C8 1.417(5) . ? C7 H7 0.9800 . ? C6 C10 1.428(4) . ? C6 H6 0.9800 . ? C9 C8 1.413(4) . ? C9 C10 1.427(4) . ? C9 H9 0.9800 . ? C8 H8 0.9800 . ? C10 C11 1.492(4) . ? C11 N1 1.498(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N1 1.492(3) 2_755 ? C12 C13 1.532(4) . ? C12 C20 1.537(4) . ? C12 H12 0.9800 . ? C13 C14 1.510(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.379(4) . ? C14 C19 1.413(4) . ? C15 C16 1.385(4) . ? C15 H15 0.9300 . ? C16 C17 1.390(4) . ? C16 H16 0.9300 . ? C19 C18 1.368(4) . ? C19 H19 0.9300 . ? C17 O3 1.362(3) . ? C17 C18 1.377(5) . ? C18 H18 0.9300 . ? N1 C12 1.492(3) 2_755 ? N1 H5X 0.76(3) . ? N2 C25 1.308(4) 2_755 ? N2 C25 1.308(4) . ? O2 C20 1.234(3) . ? O1 C20 1.267(3) . ? N3 C24 1.327(5) . ? N3 C24 1.327(5) 2_755 ? C25 C24 1.363(6) . ? C25 H25 0.9300 . ? C24 H24 0.9300 . ? O3 H6A 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O1 176.18(14) . 2_755 ? O1 Cu1 N1 84.88(9) . 2_755 ? O1 Cu1 N1 94.43(8) 2_755 2_755 ? O1 Cu1 N1 94.43(8) . . ? O1 Cu1 N1 84.88(9) 2_755 . ? N1 Cu1 N1 159.38(13) 2_755 . ? O1 Cu1 N2 91.91(7) . . ? O1 Cu1 N2 91.91(7) 2_755 . ? N1 Cu1 N2 100.31(6) 2_755 . ? N1 Cu1 N2 100.31(6) . . ? C10 Fe1 C6 41.22(11) . . ? C10 Fe1 C9 41.15(11) . . ? C6 Fe1 C9 68.66(11) . . ? C10 Fe1 C5 105.22(13) . . ? C6 Fe1 C5 122.10(15) . . ? C9 Fe1 C5 121.31(14) . . ? C10 Fe1 C4 121.55(13) . . ? C6 Fe1 C4 107.94(14) . . ? C9 Fe1 C4 157.51(13) . . ? C5 Fe1 C4 40.27(16) . . ? C10 Fe1 C3 158.99(13) . . ? C6 Fe1 C3 123.93(14) . . ? C9 Fe1 C3 159.30(13) . . ? C5 Fe1 C3 68.44(15) . . ? C4 Fe1 C3 40.87(14) . . ? C10 Fe1 C2 157.60(13) . . ? C6 Fe1 C2 160.46(14) . . ? C9 Fe1 C2 122.74(13) . . ? C5 Fe1 C2 67.91(15) . . ? C4 Fe1 C2 67.84(14) . . ? C3 Fe1 C2 40.40(14) . . ? C10 Fe1 C1 120.38(14) . . ? C6 Fe1 C1 157.32(14) . . ? C9 Fe1 C1 106.17(14) . . ? C5 Fe1 C1 40.33(16) . . ? C4 Fe1 C1 67.93(16) . . ? C3 Fe1 C1 68.55(16) . . ? C2 Fe1 C1 40.69(15) . . ? C10 Fe1 C7 68.86(11) . . ? C6 Fe1 C7 40.56(12) . . ? C9 Fe1 C7 68.09(12) . . ? C5 Fe1 C7 159.26(16) . . ? C4 Fe1 C7 124.70(16) . . ? C3 Fe1 C7 109.60(14) . . ? C2 Fe1 C7 124.91(14) . . ? C1 Fe1 C7 159.87(15) . . ? C10 Fe1 C8 68.87(11) . . ? C6 Fe1 C8 68.32(12) . . ? C9 Fe1 C8 40.42(12) . . ? C5 Fe1 C8 157.87(16) . . ? C4 Fe1 C8 160.86(15) . . ? C3 Fe1 C8 124.43(13) . . ? C2 Fe1 C8 109.01(13) . . ? C1 Fe1 C8 122.92(15) . . ? C7 Fe1 C8 40.37(13) . . ? C5 C1 C2 107.2(4) . . ? C5 C1 Fe1 69.3(2) . . ? C2 C1 Fe1 69.6(2) . . ? C5 C1 H1 126.4 . . ? C2 C1 H1 126.4 . . ? Fe1 C1 H1 126.4 . . ? C5 C4 C3 108.5(3) . . ? C5 C4 Fe1 69.85(18) . . ? C3 C4 Fe1 69.74(17) . . ? C5 C4 H4 125.8 . . ? C3 C4 H4 125.8 . . ? Fe1 C4 H4 125.8 . . ? C2 C3 C4 107.0(3) . . ? C2 C3 Fe1 70.08(18) . . ? C4 C3 Fe1 69.38(17) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? Fe1 C3 H3 126.5 . . ? C3 C2 C1 108.6(3) . . ? C3 C2 Fe1 69.52(19) . . ? C1 C2 Fe1 69.72(19) . . ? C3 C2 H2 125.7 . . ? C1 C2 H2 125.7 . . ? Fe1 C2 H2 125.7 . . ? C4 C5 C1 108.7(3) . . ? C4 C5 Fe1 69.89(19) . . ? C1 C5 Fe1 70.4(2) . . ? C4 C5 H5 125.7 . . ? C1 C5 H5 125.7 . . ? Fe1 C5 H5 125.7 . . ? C6 C7 C8 108.1(3) . . ? C6 C7 Fe1 68.83(17) . . ? C8 C7 Fe1 69.84(17) . . ? C6 C7 H7 125.9 . . ? C8 C7 H7 125.9 . . ? Fe1 C7 H7 125.9 . . ? C7 C6 C10 108.4(3) . . ? C7 C6 Fe1 70.61(18) . . ? C10 C6 Fe1 69.24(16) . . ? C7 C6 H6 125.8 . . ? C10 C6 H6 125.8 . . ? Fe1 C6 H6 125.8 . . ? C8 C9 C10 108.7(2) . . ? C8 C9 Fe1 70.53(15) . . ? C10 C9 Fe1 69.10(14) . . ? C8 C9 H9 125.7 . . ? C10 C9 H9 125.7 . . ? Fe1 C9 H9 125.7 . . ? C9 C8 C7 107.9(2) . . ? C9 C8 Fe1 69.05(15) . . ? C7 C8 Fe1 69.79(17) . . ? C9 C8 H8 126.0 . . ? C7 C8 H8 126.0 . . ? Fe1 C8 H8 126.0 . . ? C9 C10 C6 106.8(2) . . ? C9 C10 C11 126.2(3) . . ? C6 C10 C11 127.0(3) . . ? C9 C10 Fe1 69.75(14) . . ? C6 C10 Fe1 69.54(15) . . ? C11 C10 Fe1 126.02(18) . . ? C10 C11 N1 114.2(2) . . ? C10 C11 H11A 108.7 . . ? N1 C11 H11A 108.7 . . ? C10 C11 H11B 108.7 . . ? N1 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? N1 C12 C13 113.4(2) 2_755 . ? N1 C12 C20 110.3(2) 2_755 . ? C13 C12 C20 112.9(2) . . ? N1 C12 H12 106.6 2_755 . ? C13 C12 H12 106.6 . . ? C20 C12 H12 106.6 . . ? C14 C13 C12 114.1(2) . . ? C14 C13 H13A 108.7 . . ? C12 C13 H13A 108.7 . . ? C14 C13 H13B 108.7 . . ? C12 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C15 C14 C19 116.9(3) . . ? C15 C14 C13 122.0(2) . . ? C19 C14 C13 121.1(3) . . ? C14 C15 C16 122.2(3) . . ? C14 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? C15 C16 C17 119.8(3) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C19 C14 120.9(3) . . ? C18 C19 H19 119.6 . . ? C14 C19 H19 119.6 . . ? O3 C17 C18 118.6(3) . . ? O3 C17 C16 122.7(3) . . ? C18 C17 C16 118.7(3) . . ? C19 C18 C17 121.4(3) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C12 N1 C11 114.0(2) 2_755 . ? C12 N1 Cu1 109.10(15) 2_755 . ? C11 N1 Cu1 113.43(17) . . ? C12 N1 H5X 106(2) 2_755 . ? C11 N1 H5X 107(2) . . ? Cu1 N1 H5X 106(2) . . ? C25 N2 C25 112.9(4) 2_755 . ? C25 N2 Cu1 123.6(2) 2_755 . ? C25 N2 Cu1 123.6(2) . . ? C20 O1 Cu1 116.86(18) . . ? O2 C20 O1 124.3(3) . . ? O2 C20 C12 117.3(2) . . ? O1 C20 C12 118.4(2) . . ? C24 N3 C24 113.9(5) . 2_755 ? N2 C25 C24 124.5(4) . . ? N2 C25 H25 117.8 . . ? C24 C25 H25 117.8 . . ? N3 C24 C25 122.1(4) . . ? N3 C24 H24 118.9 . . ? C25 C24 H24 118.9 . . ? C17 O3 H6A 109.5 . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.836 _refine_diff_density_min -0.386 _refine_diff_density_rms 0.061 _chemical_compound_source synthesized _exptl_crystal_recrystallization_method 'methanol,slow evaporation' data_3_[Cu(S-fTyr)2(pyridine)] _database_code_depnum_ccdc_archive 'CCDC 708592' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H45 Cu Fe2 N3 O6' _chemical_formula_sum 'C45 H45 Cu Fe2 N3 O6' _chemical_formula_weight 899.112 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' _symmetry_space_group_name_Hall 'P 2 2ab' _chemical_absolute_configuration syn _symmetry_int_tables_number 18 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 11.0240(2) _cell_length_b 11.7776(2) _cell_length_c 15.3338(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1990.88(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9019 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 27.57 _exptl_crystal_description rod _exptl_crystal_colour black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.5 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 930.0 _exptl_absorpt_coefficient_mu 1.310 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29385 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 35.21 _reflns_number_total 7965 _reflns_number_gt 6099 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of 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^)+(0.0500P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.017(10) _refine_ls_number_reflns 7965 _refine_ls_number_parameters 264 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0922 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.0000 1.0000 0.79700(2) 0.03493(7) Uani 1 2 d S . . Fe1 Fe 0.31471(3) 0.66136(2) 0.596441(16) 0.03796(7) Uani 1 1 d . . . C4 C 0.3715(3) 0.8087(2) 0.54131(18) 0.0677(7) Uani 1 1 d . . . H4 H 0.3408 0.8803 0.5543 0.081 Uiso 1 1 calc R . . C1 C 0.3972(2) 0.6331(2) 0.47885(15) 0.0601(6) Uani 1 1 d . . . H1 H 0.3865 0.5695 0.4438 0.072 Uiso 1 1 calc R . . C3 C 0.4703(3) 0.7566(3) 0.5834(2) 0.0689(7) Uani 1 1 d . . . H3 H 0.5168 0.7872 0.6283 0.083 Uiso 1 1 calc R . . C2 C 0.4855(2) 0.6476(2) 0.54396(16) 0.0622(6) Uani 1 1 d . . . H2 H 0.5445 0.5946 0.5590 0.075 Uiso 1 1 calc R . . C5 C 0.3265(3) 0.7357(2) 0.47682(16) 0.0646(7) Uani 1 1 d . . . H5 H 0.2623 0.7509 0.4393 0.077 Uiso 1 1 calc R . . C8 C 0.18772(17) 0.70849(13) 0.68459(11) 0.0345(3) Uani 1 1 d . . . C11 C 0.14838(17) 0.82826(14) 0.70373(13) 0.0400(4) Uani 1 1 d . . . H11A H 0.2186 0.8719 0.7218 0.048 Uiso 1 1 calc R . . H11B H 0.1174 0.8621 0.6505 0.048 Uiso 1 1 calc R . . C9 C 0.28376(18) 0.64892(16) 0.72693(12) 0.0396(4) Uani 1 1 d . . . H9 H 0.3333 0.6772 0.7710 0.048 Uiso 1 1 calc R . . C6 C 0.1986(2) 0.52959(16) 0.62541(15) 0.0519(5) Uani 1 1 d . . . H6 H 0.1825 0.4662 0.5912 0.062 Uiso 1 1 calc R . . C7 C 0.1355(2) 0.63385(17) 0.62188(13) 0.0441(4) Uani 1 1 d . . . H7 H 0.0711 0.6508 0.5850 0.053 Uiso 1 1 calc R . . C10 C 0.2903(2) 0.53758(15) 0.68945(13) 0.0475(5) Uani 1 1 d . . . H10 H 0.3451 0.4808 0.7046 0.057 Uiso 1 1 calc R . . N1 N 0.05319(13) 0.83670(12) 0.77288(9) 0.0313(3) Uani 1 1 d . . . C14 C -0.17235(16) 0.83336(15) 0.77351(11) 0.0362(3) Uani 1 1 d . . . C12 C -0.05615(16) 0.76600(14) 0.75640(12) 0.0334(3) Uani 1 1 d . . . H12 H -0.0558 0.7481 0.6940 0.040 Uiso 1 1 calc R . . C13 C -0.05359(18) 0.65152(13) 0.80486(12) 0.0387(3) Uani 1 1 d . . . H13A H -0.1293 0.6121 0.7941 0.046 Uiso 1 1 calc R . . H13B H 0.0113 0.6055 0.7810 0.046 Uiso 1 1 calc R . . O1 O -0.16242(12) 0.93886(10) 0.78985(11) 0.0456(3) Uani 1 1 d . . . O2 O -0.27017(13) 0.78340(13) 0.76773(11) 0.0513(4) Uani 1 1 d . . . C15 C -0.03552(15) 0.66193(13) 0.90228(12) 0.0359(3) Uani 1 1 d . . . C16 C -0.1303(2) 0.69929(18) 0.95719(14) 0.0466(4) Uani 1 1 d . . . H16 H -0.2046 0.7192 0.9329 0.056 Uiso 1 1 calc R . . C18 C -0.0060(2) 0.67774(18) 1.08401(13) 0.0475(4) Uani 1 1 d . . . C17 C -0.1145(2) 0.7067(2) 1.04548(15) 0.0541(5) Uani 1 1 d . . . H17 H -0.1783 0.7318 1.0802 0.065 Uiso 1 1 calc R . . C19 C 0.07226(18) 0.63253(16) 0.94195(14) 0.0414(4) Uani 1 1 d . . . H19 H 0.1363 0.6074 0.9075 0.050 Uiso 1 1 calc R . . C20 C 0.08844(19) 0.63916(17) 1.03140(14) 0.0445(4) Uani 1 1 d . . . H20 H 0.1620 0.6180 1.0562 0.053 Uiso 1 1 calc R . . O3 O 0.00396(19) 0.6863(2) 1.17235(11) 0.0725(5) Uani 1 1 d . . . H3A H 0.0735 0.6706 1.1871 0.109 Uiso 1 1 calc R . . N2 N 0.0000 1.0000 0.94393(16) 0.0468(5) Uani 1 2 d S . . C24 C 0.0982(2) 0.9744(2) 0.98971(18) 0.0589(6) Uani 1 1 d . . . H24 H 0.1687 0.9568 0.9593 0.071 Uiso 1 1 calc R . . C29 C 0.0000 1.0000 1.1244(3) 0.0697(9) Uani 1 2 d S . . H29 H 0.0000 1.0000 1.1850 0.084 Uiso 1 2 calc SR . . C30 C 0.1026(3) 0.9722(3) 1.07965(17) 0.0666(7) Uani 1 1 d . . . H30 H 0.1735 0.9524 1.1088 0.080 Uiso 1 1 calc R . . H5X H 0.077(2) 0.8170(19) 0.8159(16) 0.037(6) 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 Cu1 0.03102(14) 0.02694(11) 0.04684(17) 0.000 0.000 0.00373(10) Fe1 0.04347(15) 0.03887(12) 0.03155(11) 0.00432(9) 0.00913(10) 0.00957(10) C4 0.0858(19) 0.0535(12) 0.0639(15) 0.0181(11) 0.0328(14) 0.0086(12) C1 0.0606(15) 0.0776(15) 0.0420(12) 0.0044(10) 0.0195(10) 0.0173(12) C3 0.0680(17) 0.0713(15) 0.0675(16) 0.0073(12) 0.0205(13) -0.0139(12) C2 0.0522(14) 0.0743(14) 0.0600(13) 0.0144(11) 0.0209(12) 0.0125(12) C5 0.0688(16) 0.0786(15) 0.0463(12) 0.0259(11) 0.0179(12) 0.0175(13) C8 0.0377(9) 0.0338(7) 0.0321(8) -0.0013(5) 0.0070(7) 0.0032(6) C11 0.0401(9) 0.0330(7) 0.0468(9) 0.0015(7) 0.0147(8) 0.0031(6) C9 0.0450(10) 0.0433(8) 0.0305(8) 0.0005(6) 0.0032(7) 0.0050(7) C6 0.0702(15) 0.0395(9) 0.0460(10) -0.0129(7) 0.0135(11) -0.0047(9) C7 0.0453(11) 0.0523(10) 0.0346(9) -0.0064(7) 0.0014(8) 0.0002(8) C10 0.0679(14) 0.0363(8) 0.0383(10) 0.0066(7) 0.0101(9) 0.0138(8) N1 0.0331(7) 0.0275(6) 0.0333(7) -0.0003(5) 0.0034(5) 0.0021(5) C14 0.0317(8) 0.0413(8) 0.0356(8) 0.0006(6) 0.0001(6) -0.0008(7) C12 0.0352(9) 0.0333(7) 0.0316(8) -0.0043(6) 0.0029(7) -0.0007(6) C13 0.0460(9) 0.0266(6) 0.0435(9) -0.0032(6) 0.0061(8) -0.0042(6) O1 0.0323(6) 0.0352(6) 0.0692(9) 0.0000(6) 0.0023(7) 0.0036(5) O2 0.0352(7) 0.0527(8) 0.0659(10) -0.0085(7) 0.0035(7) -0.0074(6) C15 0.0382(9) 0.0272(6) 0.0421(8) 0.0012(7) 0.0065(7) -0.0040(5) C16 0.0361(10) 0.0591(11) 0.0446(10) -0.0013(8) 0.0021(8) 0.0063(8) C18 0.0394(9) 0.0605(10) 0.0424(10) -0.0021(8) 0.0006(9) -0.0003(9) C17 0.0406(11) 0.0759(15) 0.0458(12) -0.0037(10) 0.0084(9) 0.0062(10) C19 0.0360(9) 0.0367(8) 0.0514(11) -0.0029(7) 0.0067(8) 0.0010(6) C20 0.0360(10) 0.0478(10) 0.0498(11) -0.0030(8) -0.0034(8) 0.0016(7) O3 0.0462(9) 0.1269(16) 0.0444(8) -0.0084(9) -0.0014(8) 0.0065(11) N2 0.0482(13) 0.0526(11) 0.0396(12) 0.000 0.000 0.0030(12) C24 0.0478(13) 0.0698(16) 0.0590(14) -0.0016(10) 0.0017(11) 0.0066(10) C29 0.067(2) 0.092(3) 0.0497(19) 0.000 0.000 -0.012(2) C30 0.0555(14) 0.090(2) 0.0545(15) -0.0010(12) -0.0110(11) 0.0012(12) _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 Cu1 O1 1.9329(14) 2_575 ? Cu1 O1 1.9330(14) . ? Cu1 N1 2.0443(14) 2_575 ? Cu1 N1 2.0444(14) . ? Cu1 N2 2.253(2) . ? Fe1 C8 2.0236(16) . ? Fe1 C4 2.029(2) . ? Fe1 C9 2.0351(17) . ? Fe1 C5 2.037(2) . ? Fe1 C7 2.039(2) . ? Fe1 C1 2.047(2) . ? Fe1 C2 2.054(2) . ? Fe1 C10 2.0571(18) . ? Fe1 C3 2.059(3) . ? Fe1 C6 2.060(2) . ? C4 C5 1.401(4) . ? C4 C3 1.407(4) . ? C4 H4 0.9300 . ? C1 C2 1.405(4) . ? C1 C5 1.438(3) . ? C1 H1 0.9300 . ? C3 C2 1.430(4) . ? C3 H3 0.9300 . ? C2 H2 0.9300 . ? C5 H5 0.9300 . ? C8 C7 1.424(3) . ? C8 C9 1.426(3) . ? C8 C11 1.505(2) . ? C11 N1 1.495(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C9 C10 1.434(3) . ? C9 H9 0.9300 . ? C6 C10 1.412(4) . ? C6 C7 1.412(3) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C10 H10 0.9300 . ? N1 C12 1.487(2) . ? N1 H5X 0.75(2) . ? C14 O2 1.232(2) . ? C14 O1 1.272(2) . ? C14 C12 1.529(2) . ? C12 C13 1.540(2) . ? C12 H12 0.9800 . ? C13 C15 1.512(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C15 C19 1.379(3) . ? C15 C16 1.412(3) . ? C16 C17 1.368(3) . ? C16 H16 0.9300 . ? C18 O3 1.363(3) . ? C18 C17 1.377(3) . ? C18 C20 1.393(3) . ? C17 H17 0.9300 . ? C19 C20 1.385(3) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? O3 H3A 0.8200 . ? N2 C24 1.325(3) 2_575 ? N2 C24 1.325(3) . ? C24 C30 1.380(4) . ? C24 H24 0.9300 . ? C29 C30 1.363(3) . ? C29 C30 1.363(3) 2_575 ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O1 173.50(10) 2_575 . ? O1 Cu1 N1 84.55(6) 2_575 2_575 ? O1 Cu1 N1 94.27(6) . 2_575 ? O1 Cu1 N1 94.27(6) 2_575 . ? O1 Cu1 N1 84.55(6) . . ? N1 Cu1 N1 159.16(8) 2_575 . ? O1 Cu1 N2 93.25(5) 2_575 . ? O1 Cu1 N2 93.25(5) . . ? N1 Cu1 N2 100.42(4) 2_575 . ? N1 Cu1 N2 100.42(4) . . ? C8 Fe1 C4 104.90(9) . . ? C8 Fe1 C9 41.15(7) . . ? C4 Fe1 C9 121.53(10) . . ? C8 Fe1 C5 121.87(9) . . ? C4 Fe1 C5 40.31(12) . . ? C9 Fe1 C5 158.00(9) . . ? C8 Fe1 C7 41.04(7) . . ? C4 Fe1 C7 120.95(11) . . ? C9 Fe1 C7 68.78(8) . . ? C5 Fe1 C7 107.61(11) . . ? C8 Fe1 C1 160.12(9) . . ? C4 Fe1 C1 68.58(11) . . ? C9 Fe1 C1 158.28(9) . . ? C5 Fe1 C1 41.23(10) . . ? C7 Fe1 C1 124.97(10) . . ? C8 Fe1 C2 156.57(10) . . ? C4 Fe1 C2 67.78(11) . . ? C9 Fe1 C2 122.22(10) . . ? C5 Fe1 C2 67.82(11) . . ? C7 Fe1 C2 161.85(10) . . ? C1 Fe1 C2 40.07(11) . . ? C8 Fe1 C10 68.95(7) . . ? C4 Fe1 C10 159.26(12) . . ? C9 Fe1 C10 41.01(8) . . ? C5 Fe1 C10 159.62(11) . . ? C7 Fe1 C10 68.18(9) . . ? C1 Fe1 C10 123.62(9) . . ? C2 Fe1 C10 109.59(9) . . ? C8 Fe1 C3 119.45(10) . . ? C4 Fe1 C3 40.26(13) . . ? C9 Fe1 C3 105.92(11) . . ? C5 Fe1 C3 67.98(13) . . ? C7 Fe1 C3 155.77(10) . . ? C1 Fe1 C3 68.47(12) . . ? C2 Fe1 C3 40.68(12) . . ? C10 Fe1 C3 124.21(11) . . ? C8 Fe1 C6 68.46(7) . . ? C4 Fe1 C6 157.77(12) . . ? C9 Fe1 C6 68.26(9) . . ? C5 Fe1 C6 123.91(12) . . ? C7 Fe1 C6 40.31(9) . . ? C1 Fe1 C6 110.10(10) . . ? C2 Fe1 C6 126.46(10) . . ? C10 Fe1 C6 40.13(10) . . ? C3 Fe1 C6 161.58(11) . . ? C5 C4 C3 109.3(2) . . ? C5 C4 Fe1 70.13(14) . . ? C3 C4 Fe1 71.03(14) . . ? C5 C4 H4 125.4 . . ? C3 C4 H4 125.4 . . ? Fe1 C4 H4 125.1 . . ? C2 C1 C5 106.8(2) . . ? C2 C1 Fe1 70.25(13) . . ? C5 C1 Fe1 69.01(12) . . ? C2 C1 H1 126.6 . . ? C5 C1 H1 126.6 . . ? Fe1 C1 H1 125.7 . . ? C4 C3 C2 106.8(3) . . ? C4 C3 Fe1 68.72(16) . . ? C2 C3 Fe1 69.47(16) . . ? C4 C3 H3 126.6 . . ? C2 C3 H3 126.6 . . ? Fe1 C3 H3 126.7 . . ? C1 C2 C3 109.1(2) . . ? C1 C2 Fe1 69.68(14) . . ? C3 C2 Fe1 69.85(14) . . ? C1 C2 H2 125.4 . . ? C3 C2 H2 125.4 . . ? Fe1 C2 H2 126.6 . . ? C4 C5 C1 108.0(2) . . ? C4 C5 Fe1 69.56(13) . . ? C1 C5 Fe1 69.76(12) . . ? C4 C5 H5 126.0 . . ? C1 C5 H5 126.0 . . ? Fe1 C5 H5 126.2 . . ? C7 C8 C9 107.68(15) . . ? C7 C8 C11 126.43(18) . . ? C9 C8 C11 125.89(17) . . ? C7 C8 Fe1 70.07(11) . . ? C9 C8 Fe1 69.86(10) . . ? C11 C8 Fe1 125.93(12) . . ? N1 C11 C8 113.76(14) . . ? N1 C11 H11A 108.8 . . ? C8 C11 H11A 108.8 . . ? N1 C11 H11B 108.8 . . ? C8 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C8 C9 C10 107.75(17) . . ? C8 C9 Fe1 68.99(10) . . ? C10 C9 Fe1 70.32(10) . . ? C8 C9 H9 126.1 . . ? C10 C9 H9 126.1 . . ? Fe1 C9 H9 126.1 . . ? C10 C6 C7 108.74(17) . . ? C10 C6 Fe1 69.83(12) . . ? C7 C6 Fe1 69.06(12) . . ? C10 C6 H6 125.6 . . ? C7 C6 H6 125.6 . . ? Fe1 C6 H6 127.1 . . ? C6 C7 C8 108.16(19) . . ? C6 C7 Fe1 70.63(13) . . ? C8 C7 Fe1 68.89(11) . . ? C6 C7 H7 125.9 . . ? C8 C7 H7 125.9 . . ? Fe1 C7 H7 126.1 . . ? C6 C10 C9 107.67(17) . . ? C6 C10 Fe1 70.04(12) . . ? C9 C10 Fe1 68.67(10) . . ? C6 C10 H10 126.2 . . ? C9 C10 H10 126.2 . . ? Fe1 C10 H10 126.7 . . ? C12 N1 C11 114.28(14) . . ? C12 N1 Cu1 108.97(10) . . ? C11 N1 Cu1 113.08(10) . . ? C12 N1 H5X 105.2(18) . . ? C11 N1 H5X 111.0(18) . . ? Cu1 N1 H5X 103.5(17) . . ? O2 C14 O1 123.78(17) . . ? O2 C14 C12 118.24(16) . . ? O1 C14 C12 117.92(15) . . ? N1 C12 C14 111.06(13) . . ? N1 C12 C13 113.17(15) . . ? C14 C12 C13 112.75(14) . . ? N1 C12 H12 106.4 . . ? C14 C12 H12 106.4 . . ? C13 C12 H12 106.4 . . ? C15 C13 C12 114.09(13) . . ? C15 C13 H13A 108.7 . . ? C12 C13 H13A 108.7 . . ? C15 C13 H13B 108.7 . . ? C12 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C14 O1 Cu1 117.04(12) . . ? C19 C15 C16 116.91(18) . . ? C19 C15 C13 121.94(16) . . ? C16 C15 C13 121.13(17) . . ? C17 C16 C15 121.1(2) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? O3 C18 C17 118.6(2) . . ? O3 C18 C20 122.6(2) . . ? C17 C18 C20 118.79(19) . . ? C16 C17 C18 121.3(2) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C15 C19 C20 122.24(18) . . ? C15 C19 H19 118.9 . . ? C20 C19 H19 118.9 . . ? C19 C20 C18 119.69(19) . . ? C19 C20 H20 120.2 . . ? C18 C20 H20 120.2 . . ? C18 O3 H3A 109.5 . . ? C24 N2 C24 116.0(3) 2_575 . ? C24 N2 Cu1 121.99(14) 2_575 . ? C24 N2 Cu1 121.99(14) . . ? N2 C24 C30 124.2(2) . . ? N2 C24 H24 117.9 . . ? C30 C24 H24 117.9 . . ? C30 C29 C30 119.6(4) . 2_575 ? C30 C29 H29 120.2 . . ? C30 C29 H29 120.2 2_575 . ? C29 C30 C24 118.0(3) . . ? C29 C30 H30 121.0 . . ? C24 C30 H30 121.0 . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 35.21 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 1.183 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.072 _chemical_compound_source synthesized _exptl_crystal_recrystallization_method 'methanol, slow evaporation' data_4_[Cu(S-fTyr)2(4,4'bpy)]H2O _database_code_depnum_ccdc_archive 'CCDC 708593' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C50 H48 Cu Fe2 N4 O6, H2 O' _chemical_formula_sum 'C50 H50 Cu Fe2 N4 O7' _chemical_compound_source synthesized _exptl_crystal_recrystallization_method 'methanol, slow evaporation' _chemical_melting_point ? _exptl_crystal_description rod _exptl_crystal_colour green _diffrn_ambient_temperature 296(2) _chemical_formula_weight 994.189 #H's on the water molecule could not be located #or fixed but included in the formula 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_int_tables_number 4 _chemical_absolute_configuration syn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.3132(4) _cell_length_b 10.4178(3) _cell_length_c 17.2315(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.306(2) _cell_angle_gamma 90.00 _cell_volume 2187.21(11) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5518 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 20.07 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1026 _exptl_absorpt_coefficient_mu 1.195 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25354 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0851 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 28.31 _reflns_number_total 9323 _reflns_number_gt 5756 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of 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^)+(0.0000P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(7) _refine_ls_number_reflns 9323 _refine_ls_number_parameters 587 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0526 _refine_ls_wR_factor_gt 0.0485 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.016 _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 Cu1 Cu 0.76530(3) 0.47554(3) 0.17634(2) 0.03429(11) Uani 1 1 d . . . Fe2 Fe 0.86576(4) 0.25461(4) 0.45007(2) 0.03536(13) Uani 1 1 d . . . Fe1 Fe 0.52734(4) 0.79321(4) 0.38633(3) 0.04306(14) Uani 1 1 d . . . C2 C 0.5944(4) 0.9702(5) 0.3874(2) 0.0733(12) Uani 1 1 d . . . H2 H 0.5824 1.0334 0.3449 0.088 Uiso 1 1 calc R . . C4 C 0.5781(3) 0.8575(4) 0.4974(2) 0.0639(12) Uani 1 1 d . . . H4 H 0.5509 0.8266 0.5447 0.077 Uiso 1 1 calc R . . C3 C 0.5326(3) 0.9584(4) 0.4498(2) 0.0673(11) Uani 1 1 d . . . H3 H 0.4696 1.0113 0.4584 0.081 Uiso 1 1 calc R . . C1 C 0.6772(4) 0.8759(5) 0.3975(3) 0.0785(15) Uani 1 1 d . . . H1 H 0.7329 0.8618 0.3631 0.094 Uiso 1 1 calc R . . C5 C 0.6668(4) 0.8064(4) 0.4661(3) 0.0742(12) Uani 1 1 d . . . H5 H 0.7132 0.7347 0.4878 0.089 Uiso 1 1 calc R . . C8 C 0.4926(3) 0.6049(3) 0.36653(19) 0.0409(9) Uani 1 1 d . . . H8 H 0.5292 0.5329 0.3962 0.049 Uiso 1 1 calc R . . C7 C 0.5264(3) 0.6627(3) 0.29965(17) 0.0313(8) Uani 1 1 d . . . C6 C 0.4514(3) 0.7611(3) 0.27544(17) 0.0438(9) Uani 1 1 d . . . H6 H 0.4535 0.8179 0.2303 0.053 Uiso 1 1 calc R . . C9 C 0.3980(3) 0.6675(4) 0.3833(2) 0.0543(10) Uani 1 1 d . . . H9 H 0.3577 0.6479 0.4269 0.065 Uiso 1 1 calc R . . C10 C 0.3725(3) 0.7648(4) 0.3275(2) 0.0552(10) Uani 1 1 d . . . H10 H 0.3109 0.8250 0.3251 0.066 Uiso 1 1 calc R . . C13 C 0.9294(3) 0.0751(3) 0.4554(2) 0.0569(11) Uani 1 1 d . . . H13 H 0.9200 0.0122 0.4127 0.068 Uiso 1 1 calc R . . C12 C 1.0136(3) 0.1646(4) 0.4691(2) 0.0556(11) Uani 1 1 d . . . H12 H 1.0742 0.1754 0.4385 0.067 Uiso 1 1 calc R . . C15 C 0.9012(3) 0.1876(4) 0.56269(19) 0.0521(10) Uani 1 1 d . . . H15 H 0.8691 0.2180 0.6082 0.063 Uiso 1 1 calc R . . C11 C 0.9965(3) 0.2360(3) 0.5364(2) 0.0596(12) Uani 1 1 d . . . H11 H 1.0429 0.3059 0.5606 0.072 Uiso 1 1 calc R . . C14 C 0.8613(3) 0.0886(3) 0.5122(2) 0.0511(10) Uani 1 1 d . . . H14 H 0.7955 0.0373 0.5160 0.061 Uiso 1 1 calc R . . C19 C 0.7766(3) 0.4199(3) 0.4466(2) 0.0536(11) Uani 1 1 d . . . H19 H 0.7654 0.4728 0.4917 0.064 Uiso 1 1 calc R . . C17 C 0.8510(2) 0.3354(3) 0.34118(17) 0.0313(8) Uani 1 1 d . . . C16 C 0.7547(2) 0.2649(3) 0.35073(17) 0.0423(9) Uani 1 1 d . . . H16 H 0.7248 0.1919 0.3186 0.051 Uiso 1 1 calc R . . C18 C 0.8642(3) 0.4326(3) 0.40074(17) 0.0422(9) Uani 1 1 d . . . H18 H 0.9238 0.4957 0.4093 0.051 Uiso 1 1 calc R . . C20 C 0.7098(3) 0.3180(4) 0.4153(2) 0.0519(11) Uani 1 1 d . . . H20 H 0.6439 0.2872 0.4353 0.062 Uiso 1 1 calc R . . C22 C 0.9221(2) 0.3057(3) 0.27947(16) 0.0375(8) Uani 1 1 d . . . H22A H 0.9971 0.2939 0.3045 0.045 Uiso 1 1 calc R . . H22B H 0.8977 0.2258 0.2538 0.045 Uiso 1 1 calc R . . C21 C 0.6282(2) 0.6287(3) 0.26594(17) 0.0390(8) Uani 1 1 d . . . H21A H 0.6576 0.7066 0.2463 0.047 Uiso 1 1 calc R . . H21B H 0.6822 0.5966 0.3080 0.047 Uiso 1 1 calc R . . C23 C 0.6048(3) 0.2959(3) 0.19034(16) 0.0324(8) Uani 1 1 d . . . C24 C 0.5492(2) 0.4168(3) 0.21613(16) 0.0282(7) Uani 1 1 d . . . H24 H 0.5518 0.4104 0.2731 0.034 Uiso 1 1 calc R . . C25 C 0.4271(2) 0.4257(3) 0.18134(16) 0.0339(8) Uani 1 1 d . . . H25A H 0.3896 0.3496 0.1962 0.041 Uiso 1 1 calc R . . H25B H 0.3950 0.4994 0.2038 0.041 Uiso 1 1 calc R . . C28 C 0.3875(2) 0.3416(3) -0.03635(19) 0.0406(9) Uani 1 1 d . . . H28 H 0.3825 0.2682 -0.0674 0.049 Uiso 1 1 calc R . . C26 C 0.4080(2) 0.4379(3) 0.09239(17) 0.0303(8) Uani 1 1 d . . . C27 C 0.3998(2) 0.3307(3) 0.04486(19) 0.0396(9) Uani 1 1 d . . . H27 H 0.4026 0.2496 0.0676 0.048 Uiso 1 1 calc R . . C29 C 0.3993(2) 0.5575(3) 0.05608(19) 0.0375(8) Uani 1 1 d . . . H29 H 0.4016 0.6311 0.0869 0.045 Uiso 1 1 calc R . . C30 C 0.3873(2) 0.5697(3) -0.02399(19) 0.0397(9) Uani 1 1 d . . . H30 H 0.3824 0.6510 -0.0466 0.048 Uiso 1 1 calc R . . C32 C 0.6666(3) 0.4696(3) -0.08508(18) 0.0445(8) Uani 1 1 d . . . H32 H 0.6068 0.4376 -0.1187 0.053 Uiso 1 1 calc R . . C33 C 0.8319(3) 0.5673(3) 0.01915(19) 0.0498(10) Uani 1 1 d . . . H33 H 0.8875 0.6047 0.0542 0.060 Uiso 1 1 calc R . . C31 C 0.6722(3) 0.4584(3) -0.00425(19) 0.0408(8) Uani 1 1 d . . . H31 H 0.6154 0.4148 0.0146 0.049 Uiso 1 1 calc R . . C35 C 0.7532(3) 0.5304(3) -0.11447(18) 0.0362(8) Uani 1 1 d . . . C34 C 0.8368(3) 0.5798(3) -0.0613(2) 0.0462(9) Uani 1 1 d . . . H34 H 0.8960 0.6209 -0.0785 0.055 Uiso 1 1 calc R . . C38 C 0.8526(3) 0.5126(4) -0.2313(2) 0.0573(11) Uani 1 1 d . . . H38 H 0.9130 0.4784 -0.1993 0.069 Uiso 1 1 calc R . . C37 C 0.6733(3) 0.5965(3) -0.2503(2) 0.0459(9) Uani 1 1 d . . . H37 H 0.6073 0.6167 -0.2328 0.055 Uiso 1 1 calc R . . C36 C 0.7595(3) 0.5452(3) -0.19944(18) 0.0394(8) Uani 1 1 d . . . C39 C 0.8566(3) 0.5299(4) -0.3089(2) 0.0683(13) Uani 1 1 d . . . H39 H 0.9190 0.5025 -0.3288 0.082 Uiso 1 1 calc R . . C40 C 0.6866(3) 0.6170(4) -0.3271(2) 0.0595(11) Uani 1 1 d . . . H40 H 0.6294 0.6566 -0.3595 0.071 Uiso 1 1 calc R . . C41 C 0.9317(3) 0.6481(3) 0.22811(18) 0.0357(8) Uani 1 1 d . . . C42 C 0.9913(2) 0.5204(3) 0.24622(17) 0.0371(9) Uani 1 1 d . . . H42 H 1.0043 0.5139 0.3035 0.045 Uiso 1 1 calc R . . C46 C 1.1065(2) 0.4807(4) -0.0007(2) 0.0528(9) Uani 1 1 d . . . H46 H 1.1055 0.4152 -0.0374 0.063 Uiso 1 1 calc R . . C45 C 1.1115(3) 0.7023(3) 0.0317(2) 0.0512(10) Uani 1 1 d . . . H45 H 1.1136 0.7878 0.0166 0.061 Uiso 1 1 calc R . . C47 C 1.1070(3) 0.6067(4) -0.0242(2) 0.0477(10) Uani 1 1 d . . . C44 C 1.1129(3) 0.6720(3) 0.1101(2) 0.0500(10) Uani 1 1 d . . . H44 H 1.1172 0.7379 0.1469 0.060 Uiso 1 1 calc R . . C43 C 1.1080(2) 0.5471(3) 0.13511(19) 0.0424(9) Uani 1 1 d . . . C48 C 0.3825(2) 0.4625(3) -0.07091(17) 0.0337(7) Uani 1 1 d . . . C49 C 1.1057(2) 0.5163(3) 0.22008(18) 0.0479(9) Uani 1 1 d . . . H49A H 1.1530 0.5767 0.2518 0.058 Uiso 1 1 calc R . . H49B H 1.1363 0.4313 0.2307 0.058 Uiso 1 1 calc R . . N1 N 0.6146(2) 0.5317(2) 0.20150(16) 0.0325(7) Uani 1 1 d . . . N1A N 0.9193(2) 0.4097(3) 0.21873(16) 0.0336(7) Uani 1 1 d . . . N2 N 0.7521(2) 0.5050(2) 0.04830(13) 0.0350(7) Uani 1 1 d . . . N3 N 0.7755(3) 0.5844(3) -0.35875(18) 0.0654(10) Uani 1 1 d . . . O1 O 0.69617(16) 0.30842(18) 0.16480(11) 0.0339(5) Uani 1 1 d . . . O2 O 0.55780(16) 0.1913(2) 0.19643(11) 0.0378(6) Uani 1 1 d . . . O1A O 0.83189(18) 0.64149(18) 0.19538(12) 0.0406(6) Uani 1 1 d . . . O2A O 0.98121(17) 0.7479(2) 0.24766(12) 0.0511(6) Uani 1 1 d . . . O3 O 0.37211(18) 0.4677(2) -0.15115(11) 0.0446(6) Uani 1 1 d . . . H8A H 0.3907 0.5390 -0.1647 0.067 Uiso 1 1 calc R . . O3A O 1.0997(2) 0.6434(2) -0.10112(13) 0.0605(7) Uani 1 1 d . . . H10P H 1.1100 0.5809 -0.1281 0.091 Uiso 1 1 calc R . . C50 C 1.1074(2) 0.4510(3) 0.0786(2) 0.0494(10) Uani 1 1 d . . . H50 H 1.1076 0.3654 0.0939 0.059 Uiso 1 1 calc R . . O4 O 0.14113(17) 0.4650(2) 0.79147(12) 0.0618(6) Uani 1 1 d . . . H4A H 0.587(2) 0.564(2) 0.1650(13) 0.000(8) Uiso 1 1 d . . . H5A H 0.938(2) 0.376(3) 0.1810(16) 0.041(11) 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 Cu1 0.0329(2) 0.0334(2) 0.0366(2) -0.0027(2) 0.00533(18) -0.0038(2) Fe2 0.0405(3) 0.0345(3) 0.0299(3) 0.0056(2) 0.0014(2) 0.0029(2) Fe1 0.0498(3) 0.0391(3) 0.0421(3) -0.0085(2) 0.0130(3) -0.0005(3) C2 0.112(4) 0.054(3) 0.054(3) -0.014(3) 0.013(3) -0.037(3) C4 0.083(3) 0.062(3) 0.044(3) -0.008(2) 0.000(2) 0.011(2) C3 0.093(3) 0.054(3) 0.051(2) -0.019(2) -0.002(2) 0.011(3) C1 0.053(3) 0.101(4) 0.086(4) -0.055(3) 0.021(3) -0.037(3) C5 0.067(3) 0.071(3) 0.077(3) -0.033(3) -0.014(3) 0.006(3) C8 0.043(2) 0.038(2) 0.043(2) 0.0013(17) 0.0124(19) 0.0006(18) C7 0.038(2) 0.0275(19) 0.0304(19) -0.0019(15) 0.0102(17) 0.0007(16) C6 0.054(2) 0.034(2) 0.043(2) 0.0036(17) 0.0061(18) 0.0033(19) C9 0.048(3) 0.059(3) 0.062(3) -0.005(2) 0.030(2) -0.004(2) C10 0.040(2) 0.050(3) 0.075(3) -0.017(2) 0.007(2) 0.010(2) C13 0.077(3) 0.036(2) 0.055(3) 0.0007(19) -0.004(2) 0.017(2) C12 0.040(3) 0.066(3) 0.063(3) 0.024(2) 0.017(2) 0.017(2) C15 0.060(3) 0.069(3) 0.027(2) 0.0069(19) 0.004(2) 0.020(2) C11 0.060(3) 0.044(3) 0.063(3) 0.007(2) -0.033(2) -0.011(2) C14 0.050(3) 0.047(3) 0.053(3) 0.021(2) -0.003(2) -0.005(2) C19 0.069(3) 0.055(3) 0.041(2) 0.0094(19) 0.018(2) 0.025(2) C17 0.037(2) 0.0246(18) 0.0303(19) 0.0051(14) -0.0006(17) 0.0000(15) C16 0.043(2) 0.052(2) 0.0277(18) 0.0161(18) -0.0076(17) -0.0028(19) C18 0.057(2) 0.035(2) 0.035(2) 0.0033(16) 0.0055(19) 0.0060(17) C20 0.034(2) 0.075(3) 0.046(2) 0.030(2) 0.006(2) 0.007(2) C22 0.048(2) 0.0328(19) 0.0311(18) -0.0018(15) 0.0036(16) 0.0034(17) C21 0.045(2) 0.040(2) 0.033(2) -0.0086(16) 0.0078(18) -0.0056(16) C23 0.035(2) 0.037(2) 0.0229(18) 0.0001(16) -0.0041(16) -0.0012(19) C24 0.034(2) 0.0256(18) 0.0257(18) 0.0018(13) 0.0079(16) -0.0054(15) C25 0.027(2) 0.0332(19) 0.042(2) 0.0016(15) 0.0088(17) 0.0002(15) C28 0.047(2) 0.031(2) 0.041(2) -0.0072(16) -0.0010(19) -0.0060(16) C26 0.0233(19) 0.033(2) 0.034(2) 0.0011(15) -0.0005(15) -0.0037(14) C27 0.040(2) 0.025(2) 0.051(2) 0.0069(16) -0.0010(18) -0.0044(16) C29 0.040(2) 0.025(2) 0.046(2) -0.0073(16) 0.0036(18) 0.0029(15) C30 0.045(2) 0.0261(19) 0.048(2) 0.0051(17) 0.0052(19) 0.0014(16) C32 0.044(2) 0.052(2) 0.036(2) -0.0056(19) 0.0022(17) -0.002(2) C33 0.049(3) 0.053(2) 0.044(2) 0.0000(19) -0.004(2) -0.0099(19) C31 0.040(2) 0.045(2) 0.040(2) -0.0017(18) 0.0149(17) -0.0101(18) C35 0.038(2) 0.037(2) 0.033(2) 0.0047(16) 0.0049(18) 0.0045(16) C34 0.044(2) 0.054(2) 0.041(2) 0.0119(19) 0.008(2) -0.0095(19) C38 0.042(3) 0.084(3) 0.048(2) 0.016(2) 0.014(2) 0.011(2) C37 0.044(3) 0.051(2) 0.043(2) -0.0013(18) 0.009(2) 0.0090(19) C36 0.044(2) 0.041(2) 0.034(2) 0.0033(16) 0.0087(19) 0.0024(17) C39 0.068(3) 0.089(4) 0.053(3) 0.011(2) 0.026(3) 0.004(3) C40 0.064(3) 0.070(3) 0.042(3) 0.010(2) 0.001(2) 0.004(2) C41 0.039(3) 0.043(2) 0.027(2) -0.0059(17) 0.0124(18) -0.0076(19) C42 0.034(2) 0.046(2) 0.0302(19) 0.0042(15) 0.0018(17) -0.0072(18) C46 0.055(2) 0.048(2) 0.059(3) -0.009(2) 0.020(2) 0.002(2) C45 0.056(3) 0.040(2) 0.062(3) 0.004(2) 0.022(2) -0.0093(19) C47 0.043(2) 0.049(3) 0.056(3) 0.003(2) 0.022(2) -0.0033(19) C44 0.054(3) 0.043(2) 0.056(3) -0.0042(19) 0.018(2) -0.0117(19) C43 0.029(2) 0.046(2) 0.054(2) 0.0027(19) 0.0119(18) -0.0018(17) C48 0.0296(19) 0.036(2) 0.0336(19) -0.0022(17) -0.0015(15) -0.0062(16) C49 0.038(2) 0.057(3) 0.050(2) 0.0087(17) 0.0082(18) -0.0042(18) N1 0.042(2) 0.0318(17) 0.0225(17) 0.0018(13) 0.0021(15) -0.0017(14) N1A 0.037(2) 0.0397(19) 0.0253(17) -0.0004(14) 0.0074(15) -0.0036(14) N2 0.0309(17) 0.0376(18) 0.0373(17) 0.0031(13) 0.0074(14) -0.0092(13) N3 0.081(3) 0.076(3) 0.044(2) 0.0065(18) 0.024(2) 0.004(2) O1 0.0316(13) 0.0310(13) 0.0400(13) -0.0029(10) 0.0087(11) -0.0054(11) O2 0.0384(15) 0.0287(13) 0.0464(14) 0.0003(11) 0.0063(11) -0.0056(11) O1A 0.0341(15) 0.0320(14) 0.0547(16) -0.0021(11) 0.0030(13) -0.0053(12) O2A 0.0507(16) 0.0432(15) 0.0581(15) -0.0107(13) 0.0038(12) -0.0200(13) O3 0.0581(16) 0.0375(14) 0.0362(13) 0.0013(12) -0.0001(11) -0.0064(13) O3A 0.0748(19) 0.0590(17) 0.0525(17) 0.0022(13) 0.0252(15) -0.0061(15) C50 0.047(2) 0.034(2) 0.070(3) 0.006(2) 0.021(2) 0.0025(17) O4 0.0608(16) 0.0587(16) 0.0647(15) -0.0027(14) 0.0051(12) 0.0069(15) _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 Cu1 O1A 1.921(2) . ? Cu1 O1 1.936(2) . ? Cu1 N1A 2.049(3) . ? Cu1 N1 2.051(3) . ? Cu1 N2 2.210(2) . ? Fe2 C13 2.024(3) . ? Fe2 C12 2.032(4) . ? Fe2 C16 2.034(3) . ? Fe2 C11 2.038(3) . ? Fe2 C19 2.038(3) . ? Fe2 C20 2.038(3) . ? Fe2 C18 2.038(3) . ? Fe2 C14 2.039(3) . ? Fe2 C17 2.041(3) . ? Fe2 C15 2.049(3) . ? Fe1 C7 2.019(3) . ? Fe1 C2 2.020(4) . ? Fe1 C1 2.021(4) . ? Fe1 C8 2.027(3) . ? Fe1 C6 2.030(3) . ? Fe1 C3 2.035(4) . ? Fe1 C4 2.038(3) . ? Fe1 C5 2.043(4) . ? Fe1 C10 2.048(3) . ? Fe1 C9 2.057(3) . ? C2 C1 1.409(5) . ? C2 C3 1.410(4) . ? C2 H2 0.9800 . ? C4 C5 1.391(5) . ? C4 C3 1.400(4) . ? C4 H4 0.9800 . ? C3 H3 0.9800 . ? C1 C5 1.410(5) . ? C1 H1 0.9800 . ? C5 H5 0.9800 . ? C8 C9 1.401(4) . ? C8 C7 1.415(4) . ? C8 H8 0.9800 . ? C7 C6 1.402(4) . ? C7 C21 1.498(4) . ? C6 C10 1.415(4) . ? C6 H6 0.9800 . ? C9 C10 1.401(5) . ? C9 H9 0.9800 . ? C10 H10 0.9800 . ? C13 C14 1.385(4) . ? C13 C12 1.389(5) . ? C13 H13 0.9800 . ? C12 C11 1.419(4) . ? C12 H12 0.9800 . ? C15 C14 1.392(4) . ? C15 C11 1.411(4) . ? C15 H15 0.9800 . ? C11 H11 0.9800 . ? C14 H14 0.9800 . ? C19 C20 1.402(4) . ? C19 C18 1.433(4) . ? C19 H19 0.9800 . ? C17 C16 1.425(4) . ? C17 C18 1.434(4) . ? C17 C22 1.503(4) . ? C16 C20 1.424(4) . ? C16 H16 0.9800 . ? C18 H18 0.9800 . ? C20 H20 0.9800 . ? C22 N1A 1.503(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C21 N1 1.493(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C23 O2 1.246(3) . ? C23 O1 1.272(3) . ? C23 C24 1.530(4) . ? C24 N1 1.485(3) . ? C24 C25 1.538(4) . ? C24 H24 0.9800 . ? C25 C26 1.522(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C28 C27 1.390(4) . ? C28 C48 1.391(4) . ? C28 H28 0.9300 . ? C26 C27 1.379(4) . ? C26 C29 1.392(4) . ? C27 H27 0.9300 . ? C29 C30 1.372(4) . ? C29 H29 0.9300 . ? C30 C48 1.375(4) . ? C30 H30 0.9300 . ? C32 C31 1.390(4) . ? C32 C35 1.397(4) . ? C32 H32 0.9300 . ? C33 N2 1.335(3) . ? C33 C34 1.403(4) . ? C33 H33 0.9300 . ? C31 N2 1.329(3) . ? C31 H31 0.9300 . ? C35 C34 1.375(4) . ? C35 C36 1.485(4) . ? C34 H34 0.9300 . ? C38 C39 1.357(4) . ? C38 C36 1.383(4) . ? C38 H38 0.9300 . ? C37 C40 1.374(4) . ? C37 C36 1.383(4) . ? C37 H37 0.9300 . ? C39 N3 1.345(4) . ? C39 H39 0.9300 . ? C40 N3 1.335(4) . ? C40 H40 0.9300 . ? C41 O2A 1.228(3) . ? C41 O1A 1.278(3) . ? C41 C42 1.529(4) . ? C42 N1A 1.490(4) . ? C42 C49 1.541(4) . ? C42 H42 0.9800 . ? C46 C47 1.375(5) . ? C46 C50 1.399(4) . ? C46 H46 0.9300 . ? C45 C47 1.381(4) . ? C45 C44 1.385(4) . ? C45 H45 0.9300 . ? C47 O3A 1.369(4) . ? C44 C43 1.374(4) . ? C44 H44 0.9300 . ? C43 C50 1.396(4) . ? C43 C49 1.503(4) . ? C48 O3 1.371(3) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? N1 H4A 0.75(2) . ? N1A H5A 0.80(3) . ? O3 H8A 0.8200 . ? O3A H10P 0.8200 . ? C50 H50 0.9300 . ? 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 O1A Cu1 O1 175.93(9) . . ? O1A Cu1 N1A 83.70(10) . . ? O1 Cu1 N1A 96.09(10) . . ? O1A Cu1 N1 94.82(10) . . ? O1 Cu1 N1 83.13(9) . . ? N1A Cu1 N1 147.03(11) . . ? O1A Cu1 N2 90.78(9) . . ? O1 Cu1 N2 93.12(9) . . ? N1A Cu1 N2 109.46(10) . . ? N1 Cu1 N2 103.49(10) . . ? C13 Fe2 C12 40.05(14) . . ? C13 Fe2 C16 107.22(15) . . ? C12 Fe2 C16 129.65(16) . . ? C13 Fe2 C11 67.60(15) . . ? C12 Fe2 C11 40.81(13) . . ? C16 Fe2 C11 169.75(17) . . ? C13 Fe2 C19 170.03(18) . . ? C12 Fe2 C19 149.41(17) . . ? C16 Fe2 C19 68.69(14) . . ? C11 Fe2 C19 117.87(16) . . ? C13 Fe2 C20 130.93(18) . . ? C12 Fe2 C20 168.98(18) . . ? C16 Fe2 C20 40.94(12) . . ? C11 Fe2 C20 149.04(18) . . ? C19 Fe2 C20 40.24(13) . . ? C13 Fe2 C18 147.06(15) . . ? C12 Fe2 C18 116.16(15) . . ? C16 Fe2 C18 68.68(13) . . ? C11 Fe2 C18 110.47(14) . . ? C19 Fe2 C18 41.15(12) . . ? C20 Fe2 C18 68.34(14) . . ? C13 Fe2 C14 39.86(13) . . ? C12 Fe2 C14 67.39(14) . . ? C16 Fe2 C14 114.90(14) . . ? C11 Fe2 C14 67.31(14) . . ? C19 Fe2 C14 132.57(15) . . ? C20 Fe2 C14 109.49(15) . . ? C18 Fe2 C14 172.32(15) . . ? C13 Fe2 C17 113.92(14) . . ? C12 Fe2 C17 107.30(13) . . ? C16 Fe2 C17 40.94(10) . . ? C11 Fe2 C17 131.80(15) . . ? C19 Fe2 C17 69.42(12) . . ? C20 Fe2 C17 68.95(12) . . ? C18 Fe2 C17 41.16(10) . . ? C14 Fe2 C17 145.83(14) . . ? C13 Fe2 C15 67.31(14) . . ? C12 Fe2 C15 68.09(14) . . ? C16 Fe2 C15 147.20(15) . . ? C11 Fe2 C15 40.39(12) . . ? C19 Fe2 C15 110.83(14) . . ? C20 Fe2 C15 116.86(14) . . ? C18 Fe2 C15 133.83(15) . . ? C14 Fe2 C15 39.82(13) . . ? C17 Fe2 C15 171.82(15) . . ? C7 Fe1 C2 125.48(15) . . ? C7 Fe1 C1 105.38(15) . . ? C2 Fe1 C1 40.81(15) . . ? C7 Fe1 C8 40.96(11) . . ? C2 Fe1 C8 164.10(18) . . ? C1 Fe1 C8 126.63(18) . . ? C7 Fe1 C6 40.52(11) . . ? C2 Fe1 C6 106.92(14) . . ? C1 Fe1 C6 116.73(17) . . ? C8 Fe1 C6 67.96(13) . . ? C7 Fe1 C3 164.49(15) . . ? C2 Fe1 C3 40.69(13) . . ? C1 Fe1 C3 68.33(16) . . ? C8 Fe1 C3 153.99(15) . . ? C6 Fe1 C3 128.29(15) . . ? C7 Fe1 C4 152.15(15) . . ? C2 Fe1 C4 67.79(15) . . ? C1 Fe1 C4 67.60(16) . . ? C8 Fe1 C4 120.32(14) . . ? C6 Fe1 C4 167.10(15) . . ? C3 Fe1 C4 40.19(12) . . ? C7 Fe1 C5 117.25(15) . . ? C2 Fe1 C5 68.29(18) . . ? C1 Fe1 C5 40.58(15) . . ? C8 Fe1 C5 108.35(16) . . ? C6 Fe1 C5 150.75(17) . . ? C3 Fe1 C5 67.87(16) . . ? C4 Fe1 C5 39.86(13) . . ? C7 Fe1 C10 68.34(13) . . ? C2 Fe1 C10 119.13(18) . . ? C1 Fe1 C10 151.8(2) . . ? C8 Fe1 C10 67.53(14) . . ? C6 Fe1 C10 40.62(11) . . ? C3 Fe1 C10 110.07(15) . . ? C4 Fe1 C10 130.49(16) . . ? C5 Fe1 C10 167.07(18) . . ? C7 Fe1 C9 68.31(12) . . ? C2 Fe1 C9 153.60(19) . . ? C1 Fe1 C9 165.3(2) . . ? C8 Fe1 C9 40.12(12) . . ? C6 Fe1 C9 67.75(13) . . ? C3 Fe1 C9 121.10(15) . . ? C4 Fe1 C9 111.38(15) . . ? C5 Fe1 C9 129.21(18) . . ? C10 Fe1 C9 39.90(13) . . ? C1 C2 C3 107.8(4) . . ? C1 C2 Fe1 69.6(3) . . ? C3 C2 Fe1 70.2(2) . . ? C1 C2 H2 126.1 . . ? C3 C2 H2 126.1 . . ? Fe1 C2 H2 126.1 . . ? C5 C4 C3 109.3(4) . . ? C5 C4 Fe1 70.3(2) . . ? C3 C4 Fe1 69.8(2) . . ? C5 C4 H4 125.3 . . ? C3 C4 H4 125.3 . . ? Fe1 C4 H4 125.3 . . ? C4 C3 C2 107.3(4) . . ? C4 C3 Fe1 70.0(2) . . ? C2 C3 Fe1 69.1(2) . . ? C4 C3 H3 126.3 . . ? C2 C3 H3 126.3 . . ? Fe1 C3 H3 126.3 . . ? C2 C1 C5 108.0(4) . . ? C2 C1 Fe1 69.5(2) . . ? C5 C1 Fe1 70.6(2) . . ? C2 C1 H1 126.0 . . ? C5 C1 H1 126.0 . . ? Fe1 C1 H1 126.0 . . ? C4 C5 C1 107.5(4) . . ? C4 C5 Fe1 69.9(2) . . ? C1 C5 Fe1 68.9(2) . . ? C4 C5 H5 126.3 . . ? C1 C5 H5 126.3 . . ? Fe1 C5 H5 126.3 . . ? C9 C8 C7 108.7(3) . . ? C9 C8 Fe1 71.1(2) . . ? C7 C8 Fe1 69.20(17) . . ? C9 C8 H8 125.7 . . ? C7 C8 H8 125.7 . . ? Fe1 C8 H8 125.7 . . ? C6 C7 C8 107.2(3) . . ? C6 C7 C21 127.5(3) . . ? C8 C7 C21 125.2(3) . . ? C6 C7 Fe1 70.18(17) . . ? C8 C7 Fe1 69.84(17) . . ? C21 C7 Fe1 122.0(2) . . ? C7 C6 C10 108.3(3) . . ? C7 C6 Fe1 69.30(17) . . ? C10 C6 Fe1 70.37(18) . . ? C7 C6 H6 125.8 . . ? C10 C6 H6 125.8 . . ? Fe1 C6 H6 125.8 . . ? C10 C9 C8 107.9(3) . . ? C10 C9 Fe1 69.7(2) . . ? C8 C9 Fe1 68.79(18) . . ? C10 C9 H9 126.1 . . ? C8 C9 H9 126.1 . . ? Fe1 C9 H9 126.1 . . ? C9 C10 C6 108.0(3) . . ? C9 C10 Fe1 70.4(2) . . ? C6 C10 Fe1 69.01(18) . . ? C9 C10 H10 126.0 . . ? C6 C10 H10 126.0 . . ? Fe1 C10 H10 126.0 . . ? C14 C13 C12 109.0(3) . . ? C14 C13 Fe2 70.7(2) . . ? C12 C13 Fe2 70.3(2) . . ? C14 C13 H13 125.5 . . ? C12 C13 H13 125.5 . . ? Fe2 C13 H13 125.5 . . ? C13 C12 C11 107.2(3) . . ? C13 C12 Fe2 69.7(2) . . ? C11 C12 Fe2 69.8(2) . . ? C13 C12 H12 126.4 . . ? C11 C12 H12 126.4 . . ? Fe2 C12 H12 126.4 . . ? C14 C15 C11 107.4(3) . . ? C14 C15 Fe2 69.71(18) . . ? C11 C15 Fe2 69.37(19) . . ? C14 C15 H15 126.3 . . ? C11 C15 H15 126.3 . . ? Fe2 C15 H15 126.3 . . ? C15 C11 C12 107.7(3) . . ? C15 C11 Fe2 70.24(19) . . ? C12 C11 Fe2 69.38(19) . . ? C15 C11 H11 126.2 . . ? C12 C11 H11 126.2 . . ? Fe2 C11 H11 126.2 . . ? C13 C14 C15 108.7(3) . . ? C13 C14 Fe2 69.48(19) . . ? C15 C14 Fe2 70.5(2) . . ? C13 C14 H14 125.6 . . ? C15 C14 H14 125.6 . . ? Fe2 C14 H14 125.6 . . ? C20 C19 C18 107.8(3) . . ? C20 C19 Fe2 69.9(2) . . ? C18 C19 Fe2 69.45(17) . . ? C20 C19 H19 126.1 . . ? C18 C19 H19 126.1 . . ? Fe2 C19 H19 126.1 . . ? C16 C17 C18 107.0(3) . . ? C16 C17 C22 123.7(3) . . ? C18 C17 C22 129.3(3) . . ? C16 C17 Fe2 69.27(15) . . ? C18 C17 Fe2 69.34(16) . . ? C22 C17 Fe2 125.6(2) . . ? C20 C16 C17 108.3(3) . . ? C20 C16 Fe2 69.69(18) . . ? C17 C16 Fe2 69.79(16) . . ? C20 C16 H16 125.9 . . ? C17 C16 H16 125.9 . . ? Fe2 C16 H16 125.9 . . ? C19 C18 C17 108.2(3) . . ? C19 C18 Fe2 69.40(17) . . ? C17 C18 Fe2 69.50(16) . . ? C19 C18 H18 125.9 . . ? C17 C18 H18 125.9 . . ? Fe2 C18 H18 125.9 . . ? C19 C20 C16 108.8(3) . . ? C19 C20 Fe2 69.9(2) . . ? C16 C20 Fe2 69.37(18) . . ? C19 C20 H20 125.6 . . ? C16 C20 H20 125.6 . . ? Fe2 C20 H20 125.6 . . ? N1A C22 C17 112.8(2) . . ? N1A C22 H22A 109.0 . . ? C17 C22 H22A 109.0 . . ? N1A C22 H22B 109.0 . . ? C17 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? N1 C21 C7 116.0(2) . . ? N1 C21 H21A 108.3 . . ? C7 C21 H21A 108.3 . . ? N1 C21 H21B 108.3 . . ? C7 C21 H21B 108.3 . . ? H21A C21 H21B 107.4 . . ? O2 C23 O1 124.3(3) . . ? O2 C23 C24 117.5(3) . . ? O1 C23 C24 118.2(3) . . ? N1 C24 C23 109.7(2) . . ? N1 C24 C25 114.1(2) . . ? C23 C24 C25 113.0(2) . . ? N1 C24 H24 106.5 . . ? C23 C24 H24 106.5 . . ? C25 C24 H24 106.5 . . ? C26 C25 C24 113.4(2) . . ? C26 C25 H25A 108.9 . . ? C24 C25 H25A 108.9 . . ? C26 C25 H25B 108.9 . . ? C24 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? C27 C28 C48 119.7(3) . . ? C27 C28 H28 120.1 . . ? C48 C28 H28 120.1 . . ? C27 C26 C29 117.6(3) . . ? C27 C26 C25 121.2(3) . . ? C29 C26 C25 121.2(3) . . ? C26 C27 C28 121.3(3) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? C30 C29 C26 121.7(3) . . ? C30 C29 H29 119.2 . . ? C26 C29 H29 119.2 . . ? C29 C30 C48 120.3(3) . . ? C29 C30 H30 119.8 . . ? C48 C30 H30 119.8 . . ? C31 C32 C35 118.2(3) . . ? C31 C32 H32 120.9 . . ? C35 C32 H32 120.9 . . ? N2 C33 C34 123.8(3) . . ? N2 C33 H33 118.1 . . ? C34 C33 H33 118.1 . . ? N2 C31 C32 125.2(3) . . ? N2 C31 H31 117.4 . . ? C32 C31 H31 117.4 . . ? C34 C35 C32 117.7(3) . . ? C34 C35 C36 118.5(3) . . ? C32 C35 C36 123.8(3) . . ? C35 C34 C33 119.3(3) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? C39 C38 C36 120.6(3) . . ? C39 C38 H38 119.7 . . ? C36 C38 H38 119.7 . . ? C40 C37 C36 118.9(3) . . ? C40 C37 H37 120.6 . . ? C36 C37 H37 120.6 . . ? C37 C36 C38 116.6(3) . . ? C37 C36 C35 121.4(3) . . ? C38 C36 C35 122.0(3) . . ? N3 C39 C38 123.8(4) . . ? N3 C39 H39 118.1 . . ? C38 C39 H39 118.1 . . ? N3 C40 C37 125.0(4) . . ? N3 C40 H40 117.5 . . ? C37 C40 H40 117.5 . . ? O2A C41 O1A 125.0(3) . . ? O2A C41 C42 118.5(3) . . ? O1A C41 C42 116.5(3) . . ? N1A C42 C41 111.2(3) . . ? N1A C42 C49 114.4(3) . . ? C41 C42 C49 113.3(3) . . ? N1A C42 H42 105.7 . . ? C41 C42 H42 105.7 . . ? C49 C42 H42 105.7 . . ? C47 C46 C50 120.0(4) . . ? C47 C46 H46 120.0 . . ? C50 C46 H46 120.0 . . ? C47 C45 C44 120.7(3) . . ? C47 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? O3A C47 C46 123.3(3) . . ? O3A C47 C45 117.7(3) . . ? C46 C47 C45 118.9(3) . . ? C43 C44 C45 121.7(3) . . ? C43 C44 H44 119.1 . . ? C45 C44 H44 119.1 . . ? C44 C43 C50 117.2(3) . . ? C44 C43 C49 120.9(3) . . ? C50 C43 C49 121.9(3) . . ? O3 C48 C30 123.4(3) . . ? O3 C48 C28 117.4(3) . . ? C30 C48 C28 119.2(3) . . ? C43 C49 C42 115.2(3) . . ? C43 C49 H49A 108.5 . . ? C42 C49 H49A 108.5 . . ? C43 C49 H49B 108.5 . . ? C42 C49 H49B 108.5 . . ? H49A C49 H49B 107.5 . . ? C24 N1 C21 115.1(2) . . ? C24 N1 Cu1 109.60(18) . . ? C21 N1 Cu1 110.05(19) . . ? C24 N1 H4A 108(2) . . ? C21 N1 H4A 108.2(19) . . ? Cu1 N1 H4A 105.4(19) . . ? C42 N1A C22 112.6(2) . . ? C42 N1A Cu1 109.39(19) . . ? C22 N1A Cu1 114.61(19) . . ? C42 N1A H5A 112(2) . . ? C22 N1A H5A 105(2) . . ? Cu1 N1A H5A 102(2) . . ? C31 N2 C33 115.7(3) . . ? C31 N2 Cu1 124.7(2) . . ? C33 N2 Cu1 119.4(2) . . ? C40 N3 C39 115.0(3) . . ? C23 O1 Cu1 117.0(2) . . ? C41 O1A Cu1 118.9(2) . . ? C48 O3 H8A 109.5 . . ? C47 O3A H10P 109.5 . . ? C43 C50 C46 121.4(3) . . ? C43 C50 H50 119.3 . . ? C46 C50 H50 119.3 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.439 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.063 data_5_[Cu(S-fTyr)2(H2O)]MeOH,H2O _database_code_depnum_ccdc_archive 'CCDC 708594' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C40 H42 Cu Fe2 N2 O7, C H4 O, H2 O ' _chemical_formula_sum 'C41 H48 Cu Fe2 N2 O9' #one H on the water molecule could not be located #or fixed but included in the formula _chemical_compound_source synthesized _exptl_crystal_recrystallization_method methanol _chemical_melting_point ? _exptl_crystal_description rod _exptl_crystal_colour green _diffrn_ambient_temperature 296(2) _chemical_formula_weight 887.05 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_int_tables_number 4 _chemical_absolute_configuration syn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.2115(3) _cell_length_b 11.5925(3) _cell_length_c 13.9124(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.0720(10) _cell_angle_gamma 90.00 _cell_volume 2001.33(8) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9745 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 26.71 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 1.298 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.634 _exptl_absorpt_correction_T_max 0.723 _exptl_absorpt_process_details multi-scan _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23979 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.29 _reflns_number_total 9596 _reflns_number_gt 8387 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics wingx _computing_publication_material wingx _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^ > 2\s(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^)+(0.0284P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(6) _refine_ls_number_reflns 9596 _refine_ls_number_parameters 516 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0569 _refine_ls_wR_factor_gt 0.0553 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.002 _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 Cu1 Cu 0.112136(16) 0.780269(17) 0.682851(14) 0.03312(5) Uani 1 1 d . . . Fe1 Fe 0.48024(2) 0.74111(2) 0.60490(2) 0.04539(8) Uani 1 1 d . . . Fe2 Fe 0.34033(2) 1.11004(2) 0.89943(2) 0.04560(8) Uani 1 1 d . . . C4 C 0.48002(16) 0.90762(18) 0.65358(16) 0.0476(5) Uani 1 1 d . . . H1 H 0.5313 0.9679 0.6517 0.057 Uiso 1 1 calc R . . C1 C 0.33275(13) 0.78619(17) 0.60555(12) 0.0338(3) Uani 1 1 d . . . C3 C 0.49169(16) 0.83134(19) 0.73525(15) 0.0460(4) Uani 1 1 d . . . H2 H 0.5525 0.8291 0.8000 0.055 Uiso 1 1 calc R . . C2 C 0.40125(14) 0.75672(15) 0.70686(13) 0.0378(4) Uani 1 1 d . . . H55 H 0.3885 0.6944 0.7489 0.045 Uiso 1 1 calc R . . C5 C 0.38276(16) 0.88101(17) 0.57375(15) 0.0433(4) Uani 1 1 d . . . H110 H 0.3547 0.9206 0.5076 0.052 Uiso 1 1 calc R . . C21 C 0.22796(16) 0.98593(17) 0.84184(14) 0.0410(4) Uani 1 1 d . . . C22 C 0.27985(19) 1.0120(2) 0.77077(16) 0.0532(5) Uani 1 1 d . . . H108 H 0.3208 0.9577 0.7443 0.064 Uiso 1 1 calc R . . C25 C 0.17858(16) 1.08940(19) 0.85798(17) 0.0511(5) Uani 1 1 d . . . H8 H 0.1362 1.0982 0.9032 0.061 Uiso 1 1 calc R . . C24 C 0.20183(19) 1.1776(2) 0.7993(2) 0.0630(6) Uani 1 1 d . . . H9 H 0.1787 1.2583 0.7966 0.076 Uiso 1 1 calc R . . C7 C 0.5055(4) 0.6971(5) 0.4738(3) 0.1277(17) Uani 1 1 d . . . H10 H 0.4772 0.7350 0.4069 0.153 Uiso 1 1 calc R . . C10 C 0.5270(3) 0.5748(3) 0.6046(4) 0.1089(13) Uani 1 1 d . . . H12 H 0.5148 0.5143 0.6486 0.131 Uiso 1 1 calc R . . C8 C 0.6064(3) 0.7186(4) 0.5547(4) 0.1109(14) Uani 1 1 d . . . H11 H 0.6599 0.7770 0.5544 0.133 Uiso 1 1 calc R . . C16 C 0.08647(16) 0.71522(19) 0.28442(14) 0.0460(5) Uani 1 1 d . . . H17 H 0.0366 0.6676 0.2985 0.055 Uiso 1 1 calc R . . C18 C 0.22297(18) 0.7411(2) 0.20876(15) 0.0557(5) Uani 1 1 d . . . C15 C 0.09583(16) 0.82867(18) 0.31610(13) 0.0426(4) Uani 1 1 d . . . C17 C 0.14985(17) 0.6709(2) 0.23209(15) 0.0516(5) Uani 1 1 d . . . H18 H 0.1433 0.5938 0.2125 0.062 Uiso 1 1 calc R . . C20 C 0.16906(19) 0.8981(2) 0.29190(16) 0.0537(5) Uani 1 1 d . . . H15 H 0.1764 0.9750 0.3120 0.064 Uiso 1 1 calc R . . C19 C 0.2311(2) 0.8547(2) 0.23844(18) 0.0616(6) Uani 1 1 d . . . H14 H 0.2792 0.9029 0.2222 0.074 Uiso 1 1 calc R . . C36 C -0.14006(15) 0.7840(2) 0.80317(13) 0.0483(4) Uani 1 1 d . . . H53 H -0.1503 0.7636 0.7358 0.058 Uiso 1 1 calc R . . C35 C -0.05912(15) 0.73072(17) 0.88219(14) 0.0398(4) Uani 1 1 d . . . C39 C -0.11094(17) 0.84712(18) 1.00198(14) 0.0449(4) Uani 1 1 d . . . H51 H -0.1004 0.8686 1.0691 0.054 Uiso 1 1 calc R . . C40 C -0.04603(16) 0.76312(18) 0.98135(14) 0.0462(5) Uani 1 1 d . . . H19 H 0.0073 0.7280 1.0354 0.055 Uiso 1 1 calc R . . C37 C -0.20582(16) 0.8671(2) 0.82266(15) 0.0487(5) Uani 1 1 d . . . H54 H -0.2599 0.9016 0.7687 0.058 Uiso 1 1 calc R . . C11 C 0.23410(13) 0.72307(15) 0.54247(12) 0.0340(3) Uani 1 1 d . . . H24A H 0.2394 0.6437 0.5659 0.041 Uiso 1 1 calc R . . H24B H 0.2317 0.7221 0.4720 0.041 Uiso 1 1 calc R . . C12 C 0.10105(13) 0.88767(14) 0.49466(12) 0.0324(3) Uani 1 1 d . . . H26 H 0.1683 0.9269 0.4995 0.039 Uiso 1 1 calc R . . C13 C 0.04392(14) 0.96204(15) 0.55218(13) 0.0352(4) Uani 1 1 d . . . C14 C 0.03334(16) 0.87695(19) 0.38016(14) 0.0447(4) Uani 1 1 d . . . H25A H -0.0280 0.8273 0.3729 0.054 Uiso 1 1 calc R . . H25B H 0.0058 0.9525 0.3541 0.054 Uiso 1 1 calc R . . C33 C 0.18321(14) 0.60576(16) 0.82443(13) 0.0352(4) Uani 1 1 d . . . C32 C 0.12699(15) 0.68920(15) 0.87555(13) 0.0359(4) Uani 1 1 d . . . H29 H 0.1676 0.6926 0.9491 0.043 Uiso 1 1 calc R . . C34 C 0.01316(16) 0.64305(16) 0.85853(16) 0.0445(4) Uani 1 1 d . . . H28A H -0.0192 0.6188 0.7878 0.053 Uiso 1 1 calc R . . H28B H 0.0185 0.5758 0.9015 0.053 Uiso 1 1 calc R . . O1A O 0.18100(11) 0.63291(11) 0.73501(9) 0.0400(3) Uani 1 1 d . . . O2A O 0.22233(13) 0.51483(13) 0.86718(11) 0.0508(4) Uani 1 1 d . . . O1 O 0.04057(10) 0.92467(11) 0.63658(9) 0.0396(3) Uani 1 1 d . . . O2 O 0.00447(14) 1.05511(12) 0.51428(12) 0.0555(4) Uani 1 1 d . . . N1 N 0.13027(10) 0.77343(13) 0.54566(9) 0.0306(3) Uani 1 1 d . . . H1A H 0.0780 0.7244 0.5079 0.037 Uiso 1 1 calc R . . N1A N 0.12598(12) 0.80460(12) 0.83014(10) 0.0336(3) Uani 1 1 d . . . C28 C 0.4192(3) 1.2392(3) 0.9937(2) 0.0869(9) Uani 1 1 d . . . H32 H 0.3953 1.3196 0.9905 0.104 Uiso 1 1 calc R . . C31 C 0.22536(17) 0.87145(17) 0.88898(15) 0.0467(5) Uani 1 1 d . . . H35A H 0.2274 0.8822 0.9588 0.056 Uiso 1 1 calc R . . H35B H 0.2887 0.8277 0.8912 0.056 Uiso 1 1 calc R . . C38 C -0.19112(15) 0.89839(17) 0.92185(14) 0.0411(4) Uani 1 1 d . . . O3A O -0.25675(12) 0.98336(14) 0.93707(11) 0.0529(4) Uani 1 1 d . . . H109 H -0.2495 0.9864 0.9980 0.079 Uiso 1 1 calc R . . O3 O 0.28787(17) 0.70325(19) 0.15677(16) 0.0803(6) Uani 1 1 d . . . H107 H 0.2909 0.6326 0.1588 0.120 Uiso 1 1 calc R . . C23 C 0.2630(2) 1.1303(2) 0.74538(18) 0.0635(6) Uani 1 1 d . . . H37 H 0.2911 1.1723 0.6988 0.076 Uiso 1 1 calc R . . C29 C 0.4858(2) 1.1920(3) 0.9415(3) 0.0891(10) Uani 1 1 d . . . H38 H 0.5160 1.2336 0.8963 0.107 Uiso 1 1 calc R . . C26 C 0.4448(3) 1.0485(3) 1.0331(3) 0.1066(14) Uani 1 1 d . . . H40 H 0.4419 0.9724 1.0628 0.128 Uiso 1 1 calc R . . C30 C 0.4992(3) 1.0760(3) 0.9669(4) 0.1022(12) Uani 1 1 d . . . H39 H 0.5389 1.0242 0.9431 0.123 Uiso 1 1 calc . . . C27 C 0.3938(3) 1.1504(3) 1.0500(2) 0.0990(11) Uani 1 1 d . . . H41 H 0.3496 1.1577 1.0937 0.119 Uiso 1 1 calc R . . C9 C 0.6146(2) 0.6425(4) 0.6302(4) 0.1021(12) Uani 1 1 d . . . H43 H 0.6751 0.6384 0.6951 0.123 Uiso 1 1 calc R . . C6 C 0.4575(3) 0.6023(4) 0.5124(4) 0.1190(18) Uani 1 1 d . . . H42 H 0.3887 0.5641 0.4764 0.143 Uiso 1 1 calc R . . O4 O 0.93208(15) 0.69482(17) 0.60960(13) 0.0595(4) Uani 1 1 d . . . O6 O 0.80093(18) 0.8973(3) 0.5427(3) 0.1222(10) Uani 1 1 d . . . O5 O 0.7364(3) 0.9328(3) 0.3380(2) 0.1288(10) Uani 1 1 d . . . H6A H 0.7698 0.9776 0.3143 0.193 Uiso 1 1 calc R . . C41 C 0.6425(4) 0.9148(3) 0.2715(4) 0.1088(12) Uani 1 1 d . . . H61 H 0.6085 0.8523 0.2939 0.163 Uiso 1 1 calc R . . H62 H 0.6494 0.8954 0.2069 0.163 Uiso 1 1 calc R . . H63 H 0.5995 0.9832 0.2639 0.163 Uiso 1 1 calc R . . H1W H 0.873(2) 0.737(2) 0.559(2) 0.071(8) Uiso 1 1 d . . . H2W H 0.7939(14) 0.8983(16) 0.4644(15) 0.027(4) Uiso 1 1 d . . . H172 H 0.0640(17) 0.845(2) 0.8299(15) 0.044(6) Uiso 1 1 d . . . H173 H 0.941(3) 0.649(3) 0.574(3) 0.103(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 Cu1 0.04069(11) 0.02927(10) 0.03234(9) 0.00353(8) 0.01630(8) 0.00237(9) Fe1 0.03441(14) 0.05107(17) 0.05472(16) -0.00485(12) 0.02049(11) 0.00235(12) Fe2 0.04004(15) 0.03460(14) 0.05701(17) -0.01223(12) 0.01004(12) -0.00194(12) C4 0.0431(11) 0.0436(11) 0.0579(12) 0.0011(9) 0.0198(9) -0.0081(9) C1 0.0336(8) 0.0361(8) 0.0342(8) 0.0013(7) 0.0151(6) 0.0054(8) C3 0.0436(11) 0.0502(11) 0.0409(10) -0.0012(8) 0.0104(8) 0.0000(9) C2 0.0369(9) 0.0375(11) 0.0396(9) 0.0056(7) 0.0142(7) 0.0035(7) C5 0.0427(11) 0.0454(11) 0.0429(10) 0.0100(8) 0.0161(8) 0.0005(9) C21 0.0404(10) 0.0377(10) 0.0433(10) -0.0102(8) 0.0125(8) -0.0078(8) C22 0.0623(14) 0.0507(12) 0.0519(12) -0.0170(9) 0.0266(10) -0.0146(10) C25 0.0388(11) 0.0468(12) 0.0669(13) -0.0093(9) 0.0170(9) 0.0001(9) C24 0.0528(13) 0.0428(12) 0.0800(16) 0.0035(11) 0.0054(11) 0.0014(10) C7 0.142(4) 0.183(5) 0.081(2) -0.018(3) 0.068(3) 0.063(4) C10 0.094(3) 0.0567(18) 0.196(5) -0.031(2) 0.076(3) 0.0110(19) C8 0.084(2) 0.112(3) 0.176(4) -0.044(3) 0.096(3) -0.016(2) C16 0.0413(10) 0.0591(13) 0.0350(9) 0.0003(8) 0.0097(7) -0.0044(9) C18 0.0589(12) 0.0698(14) 0.0422(10) -0.0073(10) 0.0222(9) -0.0028(11) C15 0.0424(10) 0.0532(11) 0.0286(9) 0.0055(8) 0.0075(7) 0.0028(9) C17 0.0544(13) 0.0581(13) 0.0387(10) -0.0099(9) 0.0112(9) -0.0006(10) C20 0.0697(14) 0.0498(12) 0.0448(11) 0.0020(9) 0.0238(10) -0.0019(11) C19 0.0737(16) 0.0641(15) 0.0575(13) -0.0024(11) 0.0361(12) -0.0119(12) C36 0.0449(10) 0.0654(12) 0.0381(9) -0.0139(10) 0.0189(7) -0.0013(11) C35 0.0408(9) 0.0391(9) 0.0473(10) -0.0033(8) 0.0253(8) -0.0053(8) C39 0.0563(12) 0.0490(11) 0.0339(9) -0.0022(8) 0.0212(8) 0.0011(9) C40 0.0519(11) 0.0505(12) 0.0395(9) 0.0071(8) 0.0197(8) 0.0050(9) C37 0.0390(10) 0.0668(14) 0.0394(10) -0.0043(9) 0.0122(8) 0.0054(10) C11 0.0358(9) 0.0337(9) 0.0351(8) -0.0016(7) 0.0153(6) 0.0058(7) C12 0.0306(8) 0.0324(9) 0.0340(8) 0.0051(6) 0.0107(6) 0.0036(7) C13 0.0344(9) 0.0325(9) 0.0395(9) 0.0042(7) 0.0137(7) 0.0027(8) C14 0.0425(11) 0.0520(12) 0.0368(9) 0.0069(8) 0.0099(7) 0.0108(9) C33 0.0363(9) 0.0331(9) 0.0396(9) 0.0049(7) 0.0173(7) -0.0001(8) C32 0.0454(10) 0.0335(9) 0.0338(9) 0.0023(7) 0.0200(7) 0.0021(8) C34 0.0502(11) 0.0373(10) 0.0568(11) -0.0014(8) 0.0322(9) -0.0027(8) O1A 0.0524(8) 0.0363(7) 0.0381(7) 0.0067(5) 0.0243(6) 0.0091(6) O2A 0.0679(10) 0.0439(8) 0.0517(8) 0.0173(6) 0.0349(7) 0.0168(7) O1 0.0488(8) 0.0348(7) 0.0387(7) 0.0027(5) 0.0195(5) 0.0056(6) O2 0.0709(9) 0.0426(8) 0.0630(9) 0.0200(7) 0.0358(8) 0.0254(8) N1 0.0286(6) 0.0299(7) 0.0343(6) 0.0003(6) 0.0122(5) -0.0015(6) N1A 0.0394(8) 0.0296(8) 0.0340(7) 0.0000(5) 0.0155(6) 0.0008(6) C28 0.089(2) 0.0600(16) 0.090(2) -0.0275(15) 0.0020(16) -0.0216(15) C31 0.0485(11) 0.0390(10) 0.0464(10) -0.0045(8) 0.0084(8) -0.0048(9) C38 0.0397(10) 0.0455(11) 0.0445(10) -0.0072(8) 0.0227(8) -0.0024(8) O3A 0.0578(9) 0.0600(9) 0.0482(8) -0.0034(7) 0.0277(7) 0.0127(7) O3 0.0886(13) 0.0906(13) 0.0830(12) -0.0244(11) 0.0568(11) -0.0126(11) C23 0.0725(16) 0.0582(15) 0.0561(13) 0.0047(10) 0.0172(11) -0.0201(12) C29 0.0489(15) 0.078(2) 0.126(3) -0.0189(18) 0.0124(15) -0.0189(14) C26 0.094(3) 0.075(2) 0.100(3) 0.0091(19) -0.033(2) -0.0105(19) C30 0.0466(16) 0.088(2) 0.146(3) -0.015(2) -0.0008(18) 0.0087(15) C27 0.115(3) 0.099(3) 0.0620(17) -0.0318(17) 0.0042(17) -0.032(2) C9 0.0517(18) 0.088(2) 0.166(4) -0.028(2) 0.037(2) 0.0249(17) C6 0.064(2) 0.145(4) 0.158(4) -0.105(3) 0.052(2) -0.013(2) O4 0.0671(11) 0.0605(10) 0.0572(9) -0.0118(8) 0.0293(8) -0.0054(8) O6 0.0678(14) 0.140(2) 0.150(2) 0.0585(19) 0.0251(14) -0.0028(14) O5 0.174(3) 0.106(2) 0.117(2) 0.0184(16) 0.062(2) -0.037(2) C41 0.145(4) 0.068(2) 0.127(3) 0.001(2) 0.064(3) 0.015(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.9217(12) . ? Cu1 O1A 1.9544(12) . ? Cu1 N1 2.0051(13) . ? Cu1 N1A 2.0137(14) . ? Fe1 C6 2.018(3) . ? Fe1 C1 2.0204(16) . ? Fe1 C5 2.023(2) . ? Fe1 C10 2.025(3) . ? Fe1 C7 2.029(3) . ? Fe1 C8 2.033(3) . ? Fe1 C2 2.0371(18) . ? Fe1 C9 2.038(3) . ? Fe1 C4 2.046(2) . ? Fe1 C3 2.054(2) . ? Fe2 C30 2.022(3) . ? Fe2 C27 2.023(3) . ? Fe2 C21 2.0247(19) . ? Fe2 C28 2.027(3) . ? Fe2 C25 2.028(2) . ? Fe2 C26 2.028(3) . ? Fe2 C22 2.038(2) . ? Fe2 C24 2.038(2) . ? Fe2 C29 2.041(3) . ? Fe2 C23 2.047(2) . ? C4 C3 1.406(3) . ? C4 C5 1.414(3) . ? C4 H1 0.9800 . ? C1 C5 1.429(3) . ? C1 C2 1.431(2) . ? C1 C11 1.490(2) . ? C3 C2 1.417(3) . ? C3 H2 0.9800 . ? C2 H55 0.9800 . ? C5 H110 0.9800 . ? C21 C22 1.416(3) . ? C21 C25 1.420(3) . ? C21 C31 1.486(3) . ? C22 C23 1.416(3) . ? C22 H108 0.9800 . ? C25 C24 1.407(3) . ? C25 H8 0.9800 . ? C24 C23 1.390(4) . ? C24 H9 0.9800 . ? C7 C8 1.441(6) . ? C7 C6 1.461(7) . ? C7 H10 0.9800 . ? C10 C6 1.335(6) . ? C10 C9 1.341(5) . ? C10 H12 0.9800 . ? C8 C9 1.347(6) . ? C8 H11 0.9800 . ? C16 C15 1.379(3) . ? C16 C17 1.383(3) . ? C16 H17 0.9300 . ? C18 O3 1.370(3) . ? C18 C19 1.373(3) . ? C18 C17 1.384(3) . ? C15 C20 1.386(3) . ? C15 C14 1.515(3) . ? C17 H18 0.9300 . ? C20 C19 1.377(3) . ? C20 H15 0.9300 . ? C19 H14 0.9300 . ? C36 C37 1.384(3) . ? C36 C35 1.388(3) . ? C36 H53 0.9300 . ? C35 C40 1.382(3) . ? C35 C34 1.506(3) . ? C39 C38 1.381(3) . ? C39 C40 1.391(3) . ? C39 H51 0.9300 . ? C40 H19 0.9300 . ? C37 C38 1.375(3) . ? C37 H54 0.9300 . ? C11 N1 1.505(2) . ? C11 H24A 0.9700 . ? C11 H24B 0.9700 . ? C12 N1 1.489(2) . ? C12 C13 1.539(2) . ? C12 C14 1.541(2) . ? C12 H26 0.9800 . ? C13 O2 1.235(2) . ? C13 O1 1.266(2) . ? C14 H25A 0.9700 . ? C14 H25B 0.9700 . ? C33 O2A 1.233(2) . ? C33 O1A 1.274(2) . ? C33 C32 1.535(2) . ? C32 N1A 1.477(2) . ? C32 C34 1.536(3) . ? C32 H29 0.9800 . ? C34 H28A 0.9700 . ? C34 H28B 0.9700 . ? N1 H1A 0.9100 . ? N1A C31 1.502(2) . ? N1A H172 0.94(2) . ? C28 C27 1.403(5) . ? C28 C29 1.427(5) . ? C28 H32 0.9800 . ? C31 H35A 0.9700 . ? C31 H35B 0.9700 . ? C38 O3A 1.376(2) . ? O3A H109 0.8200 . ? O3 H107 0.8200 . ? C23 H37 0.9800 . ? C29 C30 1.387(5) . ? C29 H38 0.9800 . ? C26 C30 1.385(6) . ? C26 C27 1.420(5) . ? C26 H40 0.9800 . ? C30 H39 0.9300 . ? C27 H41 0.9800 . ? C9 H43 0.9800 . ? C6 H42 0.9800 . ? O4 H1W 0.98(3) . ? O4 H173 0.77(4) . ? O6 H2W 1.061(18) . ? O5 C41 1.285(5) . ? O5 H6A 0.8200 . ? C41 H61 0.9600 . ? C41 H62 0.9600 . ? C41 H63 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O1A 177.03(5) . . ? O1 Cu1 N1 85.49(6) . . ? O1A Cu1 N1 97.26(5) . . ? O1 Cu1 N1A 94.66(6) . . ? O1A Cu1 N1A 82.90(5) . . ? N1 Cu1 N1A 167.27(6) . . ? C6 Fe1 C1 106.03(11) . . ? C6 Fe1 C5 123.93(16) . . ? C1 Fe1 C5 41.38(8) . . ? C6 Fe1 C10 38.56(19) . . ? C1 Fe1 C10 122.81(13) . . ? C5 Fe1 C10 159.23(15) . . ? C6 Fe1 C7 42.32(19) . . ? C1 Fe1 C7 121.72(15) . . ? C5 Fe1 C7 107.36(15) . . ? C10 Fe1 C7 67.3(2) . . ? C6 Fe1 C8 68.84(15) . . ? C1 Fe1 C8 160.13(18) . . ? C5 Fe1 C8 124.48(17) . . ? C10 Fe1 C8 65.80(18) . . ? C7 Fe1 C8 41.55(18) . . ? C6 Fe1 C2 120.99(15) . . ? C1 Fe1 C2 41.29(6) . . ? C5 Fe1 C2 68.74(7) . . ? C10 Fe1 C2 108.40(14) . . ? C7 Fe1 C2 158.44(19) . . ? C8 Fe1 C2 157.95(17) . . ? C6 Fe1 C9 65.99(16) . . ? C1 Fe1 C9 158.21(16) . . ? C5 Fe1 C9 159.95(15) . . ? C10 Fe1 C9 38.54(15) . . ? C7 Fe1 C9 67.16(18) . . ? C8 Fe1 C9 38.65(17) . . ? C2 Fe1 C9 123.60(16) . . ? C6 Fe1 C4 161.2(2) . . ? C1 Fe1 C4 69.12(8) . . ? C5 Fe1 C4 40.67(8) . . ? C10 Fe1 C4 159.06(16) . . ? C7 Fe1 C4 123.67(19) . . ? C8 Fe1 C4 109.23(14) . . ? C2 Fe1 C4 68.07(8) . . ? C9 Fe1 C4 124.90(12) . . ? C6 Fe1 C3 156.80(19) . . ? C1 Fe1 C3 69.09(7) . . ? C5 Fe1 C3 68.25(8) . . ? C10 Fe1 C3 123.83(17) . . ? C7 Fe1 C3 159.5(2) . . ? C8 Fe1 C3 123.24(14) . . ? C2 Fe1 C3 40.53(8) . . ? C9 Fe1 C3 109.71(14) . . ? C4 Fe1 C3 40.11(8) . . ? C30 Fe2 C27 68.06(18) . . ? C30 Fe2 C21 123.24(12) . . ? C27 Fe2 C21 121.48(13) . . ? C30 Fe2 C28 67.83(14) . . ? C27 Fe2 C28 40.52(14) . . ? C21 Fe2 C28 157.69(13) . . ? C30 Fe2 C25 159.00(16) . . ? C27 Fe2 C25 106.33(14) . . ? C21 Fe2 C25 41.02(8) . . ? C28 Fe2 C25 121.92(12) . . ? C30 Fe2 C26 40.01(17) . . ? C27 Fe2 C26 41.03(16) . . ? C21 Fe2 C26 106.78(12) . . ? C28 Fe2 C26 68.26(14) . . ? C25 Fe2 C26 122.58(16) . . ? C30 Fe2 C22 109.30(14) . . ? C27 Fe2 C22 158.60(13) . . ? C21 Fe2 C22 40.78(8) . . ? C28 Fe2 C22 160.02(13) . . ? C25 Fe2 C22 68.11(9) . . ? C26 Fe2 C22 123.19(13) . . ? C30 Fe2 C24 159.68(17) . . ? C27 Fe2 C24 122.10(15) . . ? C21 Fe2 C24 68.80(9) . . ? C28 Fe2 C24 107.45(12) . . ? C25 Fe2 C24 40.50(10) . . ? C26 Fe2 C24 158.62(18) . . ? C22 Fe2 C24 67.96(10) . . ? C30 Fe2 C29 39.91(15) . . ? C27 Fe2 C29 68.61(16) . . ? C21 Fe2 C29 159.18(12) . . ? C28 Fe2 C29 41.07(14) . . ? C25 Fe2 C29 158.92(12) . . ? C26 Fe2 C29 67.87(16) . . ? C22 Fe2 C29 123.96(13) . . ? C24 Fe2 C29 123.58(13) . . ? C30 Fe2 C23 125.05(17) . . ? C27 Fe2 C23 158.32(14) . . ? C21 Fe2 C23 68.45(9) . . ? C28 Fe2 C23 123.61(12) . . ? C25 Fe2 C23 67.49(10) . . ? C26 Fe2 C23 159.86(16) . . ? C22 Fe2 C23 40.55(10) . . ? C24 Fe2 C23 39.79(11) . . ? C29 Fe2 C23 109.23(13) . . ? C3 C4 C5 108.39(17) . . ? C3 C4 Fe1 70.24(12) . . ? C5 C4 Fe1 68.80(12) . . ? C3 C4 H1 125.8 . . ? C5 C4 H1 125.8 . . ? Fe1 C4 H1 125.8 . . ? C5 C1 C2 106.59(15) . . ? C5 C1 C11 126.84(15) . . ? C2 C1 C11 126.35(16) . . ? C5 C1 Fe1 69.42(10) . . ? C2 C1 Fe1 69.98(9) . . ? C11 C1 Fe1 121.36(12) . . ? C4 C3 C2 108.10(16) . . ? C4 C3 Fe1 69.65(12) . . ? C2 C3 Fe1 69.11(11) . . ? C4 C3 H2 125.9 . . ? C2 C3 H2 125.9 . . ? Fe1 C3 H2 125.9 . . ? C3 C2 C1 108.45(16) . . ? C3 C2 Fe1 70.36(11) . . ? C1 C2 Fe1 68.73(9) . . ? C3 C2 H55 125.8 . . ? C1 C2 H55 125.8 . . ? Fe1 C2 H55 125.8 . . ? C4 C5 C1 108.46(16) . . ? C4 C5 Fe1 70.53(12) . . ? C1 C5 Fe1 69.20(10) . . ? C4 C5 H110 125.8 . . ? C1 C5 H110 125.8 . . ? Fe1 C5 H110 125.8 . . ? C22 C21 C25 106.82(19) . . ? C22 C21 C31 126.06(19) . . ? C25 C21 C31 127.1(2) . . ? C22 C21 Fe2 70.11(11) . . ? C25 C21 Fe2 69.60(11) . . ? C31 C21 Fe2 125.79(13) . . ? C23 C22 C21 108.0(2) . . ? C23 C22 Fe2 70.06(13) . . ? C21 C22 Fe2 69.11(11) . . ? C23 C22 H108 126.0 . . ? C21 C22 H108 126.0 . . ? Fe2 C22 H108 126.0 . . ? C24 C25 C21 108.6(2) . . ? C24 C25 Fe2 70.16(13) . . ? C21 C25 Fe2 69.39(12) . . ? C24 C25 H8 125.7 . . ? C21 C25 H8 125.7 . . ? Fe2 C25 H8 125.7 . . ? C23 C24 C25 108.0(2) . . ? C23 C24 Fe2 70.44(14) . . ? C25 C24 Fe2 69.35(13) . . ? C23 C24 H9 126.0 . . ? C25 C24 H9 126.0 . . ? Fe2 C24 H9 126.0 . . ? C8 C7 C6 104.2(4) . . ? C8 C7 Fe1 69.36(18) . . ? C6 C7 Fe1 68.43(17) . . ? C8 C7 H10 127.9 . . ? C6 C7 H10 127.9 . . ? Fe1 C7 H10 127.9 . . ? C6 C10 C9 111.3(4) . . ? C6 C10 Fe1 70.4(2) . . ? C9 C10 Fe1 71.26(19) . . ? C6 C10 H12 124.4 . . ? C9 C10 H12 124.4 . . ? Fe1 C10 H12 124.4 . . ? C9 C8 C7 107.5(4) . . ? C9 C8 Fe1 70.90(18) . . ? C7 C8 Fe1 69.09(18) . . ? C9 C8 H11 126.2 . . ? C7 C8 H11 126.2 . . ? Fe1 C8 H11 126.2 . . ? C15 C16 C17 121.2(2) . . ? C15 C16 H17 119.4 . . ? C17 C16 H17 119.4 . . ? O3 C18 C19 117.9(2) . . ? O3 C18 C17 123.3(2) . . ? C19 C18 C17 118.8(2) . . ? C16 C15 C20 118.0(2) . . ? C16 C15 C14 122.22(19) . . ? C20 C15 C14 119.70(19) . . ? C16 C17 C18 120.1(2) . . ? C16 C17 H18 119.9 . . ? C18 C17 H18 119.9 . . ? C19 C20 C15 120.9(2) . . ? C19 C20 H15 119.5 . . ? C15 C20 H15 119.5 . . ? C18 C19 C20 120.9(2) . . ? C18 C19 H14 119.6 . . ? C20 C19 H14 119.6 . . ? C37 C36 C35 121.28(17) . . ? C37 C36 H53 119.4 . . ? C35 C36 H53 119.4 . . ? C40 C35 C36 117.90(18) . . ? C40 C35 C34 122.01(18) . . ? C36 C35 C34 120.07(17) . . ? C38 C39 C40 119.41(17) . . ? C38 C39 H51 120.3 . . ? C40 C39 H51 120.3 . . ? C35 C40 C39 121.43(18) . . ? C35 C40 H19 119.3 . . ? C39 C40 H19 119.3 . . ? C38 C37 C36 119.89(18) . . ? C38 C37 H54 120.1 . . ? C36 C37 H54 120.1 . . ? C1 C11 N1 114.46(14) . . ? C1 C11 H24A 108.6 . . ? N1 C11 H24A 108.6 . . ? C1 C11 H24B 108.6 . . ? N1 C11 H24B 108.6 . . ? H24A C11 H24B 107.6 . . ? N1 C12 C13 110.10(13) . . ? N1 C12 C14 112.60(14) . . ? C13 C12 C14 111.62(14) . . ? N1 C12 H26 107.4 . . ? C13 C12 H26 107.4 . . ? C14 C12 H26 107.4 . . ? O2 C13 O1 123.42(17) . . ? O2 C13 C12 118.55(16) . . ? O1 C13 C12 118.03(15) . . ? C15 C14 C12 113.43(15) . . ? C15 C14 H25A 108.9 . . ? C12 C14 H25A 108.9 . . ? C15 C14 H25B 108.9 . . ? C12 C14 H25B 108.9 . . ? H25A C14 H25B 107.7 . . ? O2A C33 O1A 123.19(17) . . ? O2A C33 C32 120.31(15) . . ? O1A C33 C32 116.38(15) . . ? N1A C32 C33 107.90(13) . . ? N1A C32 C34 112.63(15) . . ? C33 C32 C34 108.24(15) . . ? N1A C32 H29 109.3 . . ? C33 C32 H29 109.3 . . ? C34 C32 H29 109.3 . . ? C35 C34 C32 113.07(15) . . ? C35 C34 H28A 109.0 . . ? C32 C34 H28A 109.0 . . ? C35 C34 H28B 109.0 . . ? C32 C34 H28B 109.0 . . ? H28A C34 H28B 107.8 . . ? C33 O1A Cu1 115.48(11) . . ? C13 O1 Cu1 116.03(11) . . ? C12 N1 C11 114.87(13) . . ? C12 N1 Cu1 108.80(10) . . ? C11 N1 Cu1 116.82(9) . . ? C12 N1 H1A 105.0 . . ? C11 N1 H1A 105.0 . . ? Cu1 N1 H1A 105.0 . . ? C32 N1A C31 110.86(14) . . ? C32 N1A Cu1 107.01(10) . . ? C31 N1A Cu1 112.58(12) . . ? C32 N1A H172 109.1(14) . . ? C31 N1A H172 110.2(13) . . ? Cu1 N1A H172 106.9(12) . . ? C27 C28 C29 108.1(3) . . ? C27 C28 Fe2 69.58(15) . . ? C29 C28 Fe2 69.99(16) . . ? C27 C28 H32 126.0 . . ? C29 C28 H32 126.0 . . ? Fe2 C28 H32 126.0 . . ? C21 C31 N1A 111.62(15) . . ? C21 C31 H35A 109.3 . . ? N1A C31 H35A 109.3 . . ? C21 C31 H35B 109.3 . . ? N1A C31 H35B 109.3 . . ? H35A C31 H35B 108.0 . . ? C37 C38 O3A 117.66(18) . . ? C37 C38 C39 120.10(18) . . ? O3A C38 C39 122.22(16) . . ? C38 O3A H109 109.5 . . ? C18 O3 H107 109.5 . . ? C24 C23 C22 108.6(2) . . ? C24 C23 Fe2 69.77(14) . . ? C22 C23 Fe2 69.39(13) . . ? C24 C23 H37 125.7 . . ? C22 C23 H37 125.7 . . ? Fe2 C23 H37 125.7 . . ? C30 C29 C28 106.8(4) . . ? C30 C29 Fe2 69.32(18) . . ? C28 C29 Fe2 68.94(16) . . ? C30 C29 H38 126.6 . . ? C28 C29 H38 126.6 . . ? Fe2 C29 H38 126.6 . . ? C30 C26 C27 107.6(3) . . ? C30 C26 Fe2 69.8(2) . . ? C27 C26 Fe2 69.30(18) . . ? C30 C26 H40 126.2 . . ? C27 C26 H40 126.2 . . ? Fe2 C26 H40 126.2 . . ? C26 C30 C29 110.0(4) . . ? C26 C30 Fe2 70.2(2) . . ? C29 C30 Fe2 70.77(18) . . ? C26 C30 H39 125.0 . . ? C29 C30 H39 125.0 . . ? Fe2 C30 H39 125.6 . . ? C28 C27 C26 107.4(4) . . ? C28 C27 Fe2 69.90(17) . . ? C26 C27 Fe2 69.66(18) . . ? C28 C27 H41 126.3 . . ? C26 C27 H41 126.3 . . ? Fe2 C27 H41 126.3 . . ? C10 C9 C8 110.1(4) . . ? C10 C9 Fe1 70.20(18) . . ? C8 C9 Fe1 70.45(19) . . ? C10 C9 H43 124.9 . . ? C8 C9 H43 124.9 . . ? Fe1 C9 H43 124.9 . . ? C10 C6 C7 106.8(3) . . ? C10 C6 Fe1 71.02(19) . . ? C7 C6 Fe1 69.3(2) . . ? C10 C6 H42 126.6 . . ? C7 C6 H42 126.6 . . ? Fe1 C6 H42 126.6 . . ? H1W O4 H173 98(3) . . ? C41 O5 H6A 109.5 . . ? O5 C41 H61 109.5 . . ? O5 C41 H62 109.5 . . ? H61 C41 H62 109.5 . . ? O5 C41 H63 109.5 . . ? H61 C41 H63 109.5 . . ? H62 C41 H63 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.254 _refine_diff_density_min -0.234 _refine_diff_density_rms 0.042