Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Acade Rita Delgado' _publ_contact_author_address ; Chemistry Division Universidade Nova de Lisboa, ITQB Apartado 127 Oeiras 2781-901 PORTUGAL ; _publ_contact_author_email DELGADO@ITQB.UNL.PT _publ_section_title ; Bis[1,1'-N,N'-(2-picolyl) aminomethyl]ferrocene as a Redox Sensor for Transition Metal Ions ; loop_ _publ_author_name 'Rita Delgado' 'Helena M. Carapuca' 'Xiuling Cui' 'Michael Drew' 'Vitor Felix' data_[{CuL1(NO3)(H2O)}2](NO3)2.3.96H2O_1 _database_code_depnum_ccdc_archive 'CCDC 230139' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[{CuL1(NO3)(H2O)}2](NO3)2.3.96H2O' _chemical_formula_sum 'C48 H56.96 Cu2 Fe2 N12 O17.94' _chemical_formula_weight 1327.79 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 11.852(13) _cell_length_b 17.28(2) _cell_length_c 27.41(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.320(10) _cell_angle_gamma 90.00 _cell_volume 5541(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2730 _exptl_absorpt_coefficient_mu 1.353 _exptl_absorpt_correction_type 'Empirical, DIFABS, N.Walker and D.Stuart, Acta Cryst. 1983' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MAR research image plate system' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12594 _diffrn_reflns_av_R_equivalents 0.1811 _diffrn_reflns_av_sigmaI/netI 0.2908 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.86 _reflns_number_total 4388 _reflns_number_gt 2118 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'W. Kabsch, J. Appl. Crystallogr. 21,916,1983' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0908P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4388 _refine_ls_number_parameters 360 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1982 _refine_ls_R_factor_gt 0.0991 _refine_ls_wR_factor_ref 0.2165 _refine_ls_wR_factor_gt 0.1846 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu -0.26800(10) 0.06230(9) 0.12070(5) 0.0320(4) Uani 1 d . . . Fe Fe -0.22003(12) 0.18747(9) 0.33604(6) 0.0259(5) Uani 1 d . . . C11 C -0.3651(8) 0.1802(7) 0.2856(4) 0.035(3) Uani 1 d . . . H11 H -0.3944 0.2188 0.2635 0.042 Uiso 1 calc R . . C12 C -0.3936(10) 0.1705(8) 0.3333(5) 0.044(4) Uani 1 d . . . H12 H -0.4445 0.2003 0.3478 0.053 Uiso 1 calc R . . C13 C -0.3308(9) 0.1075(8) 0.3544(5) 0.043(4) Uani 1 d . . . H13 H -0.3309 0.0889 0.3862 0.052 Uiso 1 calc R . . C14 C -0.2677(10) 0.0768(7) 0.3204(5) 0.045(3) Uani 1 d . . . H14 H -0.2212 0.0333 0.3256 0.054 Uiso 1 calc R . . C15 C -0.2852(9) 0.1226(7) 0.2758(4) 0.029(3) Uani 1 d . . . C16 C -0.2316(8) 0.1106(7) 0.2299(4) 0.033(3) Uani 1 d . . . H16A H -0.1717 0.0720 0.2365 0.040 Uiso 1 calc R . . H16B H -0.1972 0.1586 0.2214 0.040 Uiso 1 calc R . . N17 N -0.3201(7) 0.0844(5) 0.1869(3) 0.025(2) Uani 1 d . . . H17 H -0.3724 0.1232 0.1811 0.030 Uiso 1 calc R . . C18 C -0.3826(8) 0.0157(6) 0.1994(4) 0.029(3) Uani 1 d . . . H18A H -0.3288 -0.0211 0.2168 0.035 Uiso 1 calc R . . H18B H -0.4352 0.0307 0.2214 0.035 Uiso 1 calc R . . N21 N -0.4078(7) -0.0069(6) 0.1122(3) 0.031(2) Uani 1 d . . . C22 C -0.4467(8) -0.0214(6) 0.1553(4) 0.027(3) Uani 1 d . . . C23 C -0.5416(9) -0.0677(7) 0.1541(4) 0.036(3) Uani 1 d . . . H23 H -0.5695 -0.0769 0.1834 0.043 Uiso 1 calc R . . C24 C -0.5963(10) -0.1007(8) 0.1113(5) 0.045(3) Uani 1 d . . . H24 H -0.6588 -0.1332 0.1115 0.054 Uiso 1 calc R . . C25 C -0.5573(9) -0.0849(7) 0.0690(5) 0.044(4) Uani 1 d . . . H25 H -0.5938 -0.1064 0.0395 0.053 Uiso 1 calc R . . C26 C -0.4629(9) -0.0369(7) 0.0687(5) 0.048(4) Uani 1 d . . . H26 H -0.4376 -0.0254 0.0391 0.058 Uiso 1 calc R . . N41 N 0.2163(7) 0.0456(6) 0.4452(3) 0.035(3) Uani 1 d . . . C42 C 0.2148(9) -0.0209(9) 0.4707(5) 0.048(4) Uani 1 d U . . H42 H 0.2427 -0.0651 0.4574 0.058 Uiso 1 calc R . . C43 C 0.1745(11) -0.0280(9) 0.5154(5) 0.060(4) Uani 1 d . . . H43 H 0.1755 -0.0748 0.5322 0.072 Uiso 1 calc R . . C44 C 0.1318(10) 0.0413(10) 0.5335(5) 0.061(4) Uani 1 d . . . H44 H 0.1037 0.0406 0.5632 0.073 Uiso 1 calc R . . C45 C 0.1312(9) 0.1095(9) 0.5076(5) 0.052(4) Uani 1 d . . . H45 H 0.1028 0.1548 0.5193 0.062 Uiso 1 calc R . . C46 C 0.1741(11) 0.1086(9) 0.4635(5) 0.052(4) Uani 1 d . . . C38 C 0.1754(8) 0.1780(8) 0.4323(4) 0.044(4) Uani 1 d . . . H38A H 0.2474 0.2051 0.4413 0.053 Uiso 1 calc R . . H38B H 0.1142 0.2127 0.4377 0.053 Uiso 1 calc R . . N37 N 0.1600(6) 0.1548(5) 0.3783(3) 0.032(2) Uani 1 d . . . H37 H 0.1829 0.1939 0.3599 0.039 Uiso 1 calc R . . C36 C 0.0366(8) 0.1329(7) 0.3587(4) 0.032(3) Uani 1 d . . . H36A H 0.0324 0.1142 0.3251 0.038 Uiso 1 calc R . . H36B H 0.0150 0.0905 0.3785 0.038 Uiso 1 calc R . . C35 C -0.0495(7) 0.1973(6) 0.3588(4) 0.024(3) Uani 1 d . . . C31 C -0.1097(8) 0.2163(7) 0.3989(5) 0.037(3) Uani 1 d . . . H41 H -0.1043 0.1919 0.4295 0.044 Uiso 1 calc R . . C32 C -0.1781(11) 0.2798(8) 0.3816(5) 0.049(4) Uani 1 d U . . H32 H -0.2259 0.3056 0.3999 0.059 Uiso 1 calc R . . C33 C -0.1656(10) 0.2990(7) 0.3342(6) 0.058(4) Uani 1 d . . . H33 H -0.2040 0.3388 0.3156 0.070 Uiso 1 calc R . . C34 C -0.0860(9) 0.2490(7) 0.3184(4) 0.037(3) Uani 1 d . . . H34 H -0.0616 0.2492 0.2878 0.045 Uiso 1 calc R . . N401 N 0.2094(13) -0.1790(16) 0.1936(8) 0.134(10) Uani 1 d . . . O402 O 0.1903(18) -0.1179(9) 0.2134(7) 0.169(10) Uani 1 d . . . O403 O 0.3021(14) -0.2039(9) 0.1945(6) 0.145(6) Uani 1 d . . . O404 O 0.1337(15) -0.2218(12) 0.1739(8) 0.251(15) Uani 1 d . . . N201 N -0.4831(17) 0.1679(15) 0.0483(7) 0.115(4) Uiso 0.465(11) d PD A 1 O202 O -0.580(2) 0.1355(16) 0.0367(10) 0.115(4) Uiso 0.465(11) d PD A 1 O203 O -0.4312(18) 0.1638(16) 0.0927(7) 0.115(4) Uiso 0.465(11) d PD A 1 O204 O -0.452(2) 0.2191(15) 0.0197(8) 0.115(4) Uiso 0.465(11) d PD A 1 N301 N -0.5452(15) 0.1956(10) 0.0368(10) 0.115(4) Uiso 0.535(11) d PD A 2 O302 O -0.5913(17) 0.2621(10) 0.0350(8) 0.115(4) Uiso 0.535(11) d PD A 2 O303 O -0.6042(19) 0.1373(11) 0.0201(10) 0.115(4) Uiso 0.535(11) d PD A 2 O304 O -0.4454(14) 0.1859(13) 0.0609(9) 0.115(4) Uiso 0.535(11) d PD A 2 O600 O -0.6760(18) 0.2977(13) 0.0163(9) 0.087(8) Uiso 0.465(11) d P A 3 O100 O -0.1468(6) -0.0362(4) 0.1570(3) 0.044(2) Uani 1 d . B 3 O400 O -0.0271(8) -0.1352(6) 0.1054(4) 0.078(3) Uani 1 d . C 3 O500 O 0.0000 -0.0646(9) 0.2500 0.088(5) Uani 1 d S D 3 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 Cu 0.0291(7) 0.0427(10) 0.0245(8) -0.0001(8) 0.0047(5) -0.0111(7) Fe 0.0244(8) 0.0244(10) 0.0282(10) -0.0097(9) 0.0025(6) -0.0016(7) C11 0.028(6) 0.032(8) 0.040(8) -0.006(7) -0.006(5) 0.000(5) C12 0.035(7) 0.046(10) 0.050(9) -0.013(7) 0.001(6) -0.006(6) C13 0.029(7) 0.067(10) 0.040(8) -0.032(8) 0.025(6) -0.022(6) C14 0.066(9) 0.027(9) 0.038(8) -0.010(7) -0.002(6) -0.014(6) C15 0.035(7) 0.026(8) 0.026(7) -0.007(6) 0.005(5) -0.017(5) C16 0.026(6) 0.036(9) 0.039(7) 0.000(6) 0.011(5) -0.012(5) N17 0.035(5) 0.029(6) 0.011(5) 0.004(4) 0.002(4) -0.002(4) C18 0.034(6) 0.031(8) 0.024(7) 0.001(6) 0.008(5) 0.001(5) N21 0.021(5) 0.046(7) 0.024(6) 0.004(5) -0.004(4) -0.004(4) C22 0.024(6) 0.028(8) 0.030(7) 0.007(6) 0.011(5) 0.009(5) C23 0.042(7) 0.025(8) 0.041(8) -0.006(7) 0.008(6) -0.010(6) C24 0.041(8) 0.044(9) 0.053(9) -0.003(8) 0.011(6) -0.007(6) C25 0.027(7) 0.045(10) 0.054(9) -0.017(7) -0.011(6) 0.003(6) C26 0.034(7) 0.063(11) 0.046(9) 0.013(7) 0.003(6) -0.008(6) N41 0.024(5) 0.053(8) 0.029(6) 0.002(6) 0.005(4) 0.007(5) C42 0.044(8) 0.074(12) 0.028(8) 0.010(8) 0.010(6) -0.002(7) C43 0.063(10) 0.067(12) 0.046(10) 0.019(9) -0.007(7) 0.002(8) C44 0.046(8) 0.088(14) 0.049(10) 0.017(10) 0.009(7) 0.017(8) C45 0.022(7) 0.075(12) 0.055(10) -0.013(9) 0.000(6) 0.008(7) C46 0.059(9) 0.065(11) 0.028(8) -0.018(8) -0.006(6) 0.023(8) C38 0.014(6) 0.063(10) 0.050(9) -0.037(8) -0.013(5) 0.016(6) N37 0.025(5) 0.040(7) 0.025(6) -0.003(5) -0.014(4) -0.001(4) C36 0.034(6) 0.036(8) 0.027(7) -0.016(6) 0.013(5) -0.011(5) C35 0.013(5) 0.021(7) 0.037(7) -0.011(6) 0.007(4) -0.005(4) C31 0.020(6) 0.035(8) 0.055(9) -0.024(7) 0.008(5) 0.004(5) C32 0.057(7) 0.045(7) 0.049(7) -0.033(6) 0.014(6) -0.008(6) C33 0.029(7) 0.029(9) 0.113(14) -0.007(9) 0.000(7) 0.011(6) C34 0.040(7) 0.051(10) 0.016(7) -0.006(6) -0.011(5) -0.018(6) N401 0.045(11) 0.21(3) 0.15(2) 0.116(19) 0.022(10) 0.035(14) O402 0.27(2) 0.074(11) 0.182(18) 0.007(12) 0.090(16) 0.065(13) O403 0.166(15) 0.112(13) 0.174(16) 0.054(11) 0.078(13) -0.011(11) O404 0.139(15) 0.21(2) 0.34(3) 0.110(19) -0.157(17) -0.084(15) O100 0.048(5) 0.042(6) 0.038(5) 0.004(4) -0.005(4) 0.003(4) O400 0.074(7) 0.072(8) 0.094(8) -0.005(7) 0.032(6) 0.003(6) O500 0.124(12) 0.079(12) 0.060(10) 0.000 0.008(9) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N41 2.021(9) 6_556 ? Cu N21 2.027(9) . ? Cu N17 2.044(8) . ? Cu N37 2.046(9) 6_556 ? Cu O100 2.343(8) . ? Fe C14 2.020(12) . ? Fe C35 2.024(9) . ? Fe C13 2.025(12) . ? Fe C11 2.029(10) . ? Fe C34 2.034(11) . ? Fe C33 2.035(13) . ? Fe C32 2.037(12) . ? Fe C15 2.041(11) . ? Fe C31 2.049(12) . ? Fe C12 2.068(11) . ? C11 C12 1.415(16) . ? C11 C15 1.428(15) . ? C12 C13 1.390(17) . ? C13 C14 1.391(15) . ? C14 C15 1.442(15) . ? C15 C16 1.512(14) . ? C16 N17 1.515(13) . ? N17 C18 1.470(12) . ? C18 C22 1.468(15) . ? N21 C22 1.358(13) . ? N21 C26 1.366(14) . ? C22 C23 1.376(14) . ? C23 C24 1.370(16) . ? C24 C25 1.345(16) . ? C25 C26 1.394(15) . ? N41 C46 1.330(15) . ? N41 C42 1.345(15) . ? N41 Cu 2.021(9) 6_556 ? C42 C43 1.392(17) . ? C43 C44 1.421(18) . ? C44 C45 1.375(18) . ? C45 C46 1.384(17) . ? C46 C38 1.476(18) . ? C38 N37 1.516(13) . ? N37 C36 1.521(12) . ? N37 Cu 2.046(9) 6_556 ? C36 C35 1.510(14) . ? C35 C34 1.433(15) . ? C35 C31 1.444(14) . ? C31 C32 1.401(17) . ? C32 C33 1.371(18) . ? C33 C34 1.400(16) . ? N401 O403 1.177(18) . ? N401 O404 1.22(3) . ? N401 O402 1.22(3) . ? N201 O202 1.272(5) . ? N201 O204 1.272(5) . ? N201 O203 1.274(5) . ? N301 O304 1.268(5) . ? N301 O302 1.270(5) . ? N301 O303 1.271(5) . ? 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 N41 Cu N21 100.0(4) 6_556 . ? N41 Cu N17 177.4(4) 6_556 . ? N21 Cu N17 81.6(3) . . ? N41 Cu N37 81.0(4) 6_556 6_556 ? N21 Cu N37 164.0(3) . 6_556 ? N17 Cu N37 96.9(4) . 6_556 ? N41 Cu O100 91.3(3) 6_556 . ? N21 Cu O100 93.1(3) . . ? N17 Cu O100 90.7(3) . . ? N37 Cu O100 102.9(3) 6_556 . ? C14 Fe C35 112.1(5) . . ? C14 Fe C13 40.2(4) . . ? C35 Fe C13 129.5(5) . . ? C14 Fe C11 67.6(5) . . ? C35 Fe C11 155.4(4) . . ? C13 Fe C11 67.4(5) . . ? C14 Fe C34 130.3(5) . . ? C35 Fe C34 41.4(4) . . ? C13 Fe C34 168.1(5) . . ? C11 Fe C34 118.6(5) . . ? C14 Fe C33 165.9(6) . . ? C35 Fe C33 67.9(5) . . ? C13 Fe C33 150.8(5) . . ? C11 Fe C33 106.2(5) . . ? C34 Fe C33 40.2(5) . . ? C14 Fe C32 154.6(6) . . ? C35 Fe C32 67.2(5) . . ? C13 Fe C32 119.1(5) . . ? C11 Fe C32 124.2(5) . . ? C34 Fe C32 67.3(5) . . ? C33 Fe C32 39.4(5) . . ? C14 Fe C15 41.6(4) . . ? C35 Fe C15 121.6(4) . . ? C13 Fe C15 69.5(4) . . ? C11 Fe C15 41.1(4) . . ? C34 Fe C15 107.6(4) . . ? C33 Fe C15 125.4(6) . . ? C32 Fe C15 161.6(5) . . ? C14 Fe C31 121.8(5) . . ? C35 Fe C31 41.5(4) . . ? C13 Fe C31 107.9(5) . . ? C11 Fe C31 160.7(4) . . ? C34 Fe C31 69.9(4) . . ? C33 Fe C31 68.2(5) . . ? C32 Fe C31 40.1(5) . . ? C15 Fe C31 157.0(5) . . ? C14 Fe C12 67.4(5) . . ? C35 Fe C12 164.0(5) . . ? C13 Fe C12 39.7(5) . . ? C11 Fe C12 40.4(4) . . ? C34 Fe C12 151.3(5) . . ? C33 Fe C12 116.8(5) . . ? C32 Fe C12 106.0(5) . . ? C15 Fe C12 69.4(5) . . ? C31 Fe C12 124.1(5) . . ? C12 C11 C15 110.8(11) . . ? C12 C11 Fe 71.3(6) . . ? C15 C11 Fe 69.9(6) . . ? C13 C12 C11 106.6(11) . . ? C13 C12 Fe 68.5(7) . . ? C11 C12 Fe 68.3(6) . . ? C12 C13 C14 109.3(12) . . ? C12 C13 Fe 71.8(8) . . ? C14 C13 Fe 69.7(7) . . ? C13 C14 C15 109.9(12) . . ? C13 C14 Fe 70.1(7) . . ? C15 C14 Fe 70.0(7) . . ? C11 C15 C14 103.4(10) . . ? C11 C15 C16 129.2(11) . . ? C14 C15 C16 127.4(11) . . ? C11 C15 Fe 69.0(6) . . ? C14 C15 Fe 68.4(6) . . ? C16 C15 Fe 126.4(7) . . ? C15 C16 N17 111.0(8) . . ? C18 N17 C16 111.7(8) . . ? C18 N17 Cu 107.0(6) . . ? C16 N17 Cu 118.5(6) . . ? C22 C18 N17 111.9(9) . . ? C22 N21 C26 120.5(10) . . ? C22 N21 Cu 113.3(7) . . ? C26 N21 Cu 126.2(8) . . ? N21 C22 C23 118.6(10) . . ? N21 C22 C18 115.6(9) . . ? C23 C22 C18 125.8(10) . . ? C24 C23 C22 122.3(11) . . ? C25 C24 C23 118.3(12) . . ? C24 C25 C26 120.9(12) . . ? N21 C26 C25 119.4(12) . . ? C46 N41 C42 117.8(11) . . ? C46 N41 Cu 114.0(9) . 6_556 ? C42 N41 Cu 128.1(9) . 6_556 ? N41 C42 C43 124.6(13) . . ? C42 C43 C44 115.1(14) . . ? C45 C44 C43 121.0(14) . . ? C44 C45 C46 117.9(14) . . ? N41 C46 C45 123.5(14) . . ? N41 C46 C38 114.0(11) . . ? C45 C46 C38 122.4(13) . . ? C46 C38 N37 109.9(10) . . ? C38 N37 C36 111.5(8) . . ? C38 N37 Cu 102.6(6) . 6_556 ? C36 N37 Cu 111.9(7) . 6_556 ? C35 C36 N37 115.3(8) . . ? C34 C35 C31 108.8(10) . . ? C34 C35 C36 125.3(10) . . ? C31 C35 C36 125.9(10) . . ? C34 C35 Fe 69.7(6) . . ? C31 C35 Fe 70.2(6) . . ? C36 C35 Fe 125.4(7) . . ? C32 C31 C35 104.4(11) . . ? C32 C31 Fe 69.5(7) . . ? C35 C31 Fe 68.3(6) . . ? C33 C32 C31 111.5(12) . . ? C33 C32 Fe 70.3(8) . . ? C31 C32 Fe 70.4(7) . . ? C32 C33 C34 109.0(12) . . ? C32 C33 Fe 70.4(8) . . ? C34 C33 Fe 69.8(7) . . ? C33 C34 C35 106.3(11) . . ? C33 C34 Fe 69.9(7) . . ? C35 C34 Fe 68.9(6) . . ? O403 N401 O404 114(3) . . ? O403 N401 O402 123(3) . . ? O404 N401 O402 123(2) . . ? O202 N201 O204 119.4(6) . . ? O202 N201 O203 119.3(7) . . ? O204 N201 O203 119.0(6) . . ? O304 N301 O302 120.0(6) . . ? O304 N301 O303 119.7(6) . . ? O302 N301 O303 119.7(6) . . ? _diffrn_measured_fraction_theta_max 0.409 _diffrn_reflns_theta_full 25.86 _diffrn_measured_fraction_theta_full 0.409 _refine_diff_density_max 0.644 _refine_diff_density_min -0.735 _refine_diff_density_rms 0.141