# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1786 # CIF FOR C30 H42 Cu2 Fe N13 O6.5 (complex 2) # Manuscript ref. 9/08485A data_MG716 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H42 Cu2 Fe N13 O6.50' _chemical_formula_weight 871.70 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.592(6) _cell_length_b 12.226(6) _cell_length_c 14.737(5) _cell_angle_alpha 102.78(4) _cell_angle_beta 101.86(4) _cell_angle_gamma 109.95(5) _cell_volume 1822.4(14) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 898 _exptl_absorpt_coefficient_mu 1.612 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5656 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.1141 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5412 _reflns_number_gt 3699 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+3.0593P] 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 5412 _refine_ls_number_parameters 476 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1129 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1434 _refine_ls_wR_factor_gt 0.1296 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 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 Fe1 Fe 0.5000 0.0000 0.5000 0.0205(3) Uani 1 d S . . Fe2 Fe 0.0000 0.0000 0.0000 0.0213(4) Uani 1 d S . . Cu1 Cu 0.41588(9) -0.02308(10) 0.15513(7) 0.0334(3) Uani 1 d . . . Cu2 Cu 0.06627(9) 0.23281(8) 0.32963(7) 0.0244(2) Uani 1 d . . . O1 O -0.1993(6) 0.7108(5) 0.4109(5) 0.0546(18) Uani 1 d . . . O2 O 0.0372(6) 0.6208(6) 0.2183(5) 0.0592(19) Uani 1 d . . . O3 O -0.1932(7) 0.6601(6) 0.2081(5) 0.068(2) Uani 1 d . . . O4 O 0.1142(9) 0.4298(7) 0.1386(6) 0.097(3) Uani 1 d . . . O5A O 0.0361(10) 0.6826(10) 0.0484(8) 0.081(4) Uiso 0.747(18) d P . . O5B O 0.056(3) 0.587(3) 0.036(2) 0.066(12) Uiso 0.253(18) d P . . O6A O 0.3223(14) 0.3881(17) 0.1059(17) 0.086(8) Uiso 0.61(5) d P . . O6B O 0.337(3) 0.421(3) 0.065(3) 0.098(13) Uiso 0.39(5) d P . . O7A O 0.5652(18) 0.5221(19) 0.0303(15) 0.124(7) Uiso 0.50 d P . . N1 N 0.5004(6) 0.0649(6) 0.3113(5) 0.0283(15) Uani 1 d . . . N2 N 0.3397(6) 0.1477(6) 0.5491(5) 0.0311(15) Uani 1 d . . . N3 N 0.2482(7) -0.2265(7) 0.3772(5) 0.0418(18) Uani 1 d . . . N4 N 0.2562(6) 0.0005(6) 0.1094(5) 0.0342(16) Uani 1 d . . . N5 N 0.0191(6) 0.1987(6) 0.1759(5) 0.0302(15) Uani 1 d . . . N6 N 0.1506(7) 0.1901(7) -0.0836(5) 0.0416(18) Uani 1 d . . . N7 N 0.5255(6) 0.1276(7) 0.1299(5) 0.0370(17) Uani 1 d . . . N8 N 0.5602(7) -0.0732(7) 0.1299(5) 0.0389(18) Uani 1 d . . . N9 N 0.3142(7) -0.1832(6) 0.1713(5) 0.0410(18) Uani 1 d . . . H9A H 0.2999 -0.1650 0.2294 0.049 Uiso 1 d R . . H9B H 0.2368 -0.2155 0.1253 0.049 Uiso 1 d R . . N10 N -0.0376(6) 0.3321(6) 0.3587(4) 0.0259(15) Uani 1 d . . . N11 N -0.0761(6) 0.1081(5) 0.3576(4) 0.0263(15) Uani 1 d . . . N12 N 0.1688(6) 0.1322(5) 0.3302(4) 0.0252(14) Uani 1 d . . . N13 N 0.2505(6) 0.3727(5) 0.3610(4) 0.0245(14) Uani 1 d . . . C1 C 0.5032(6) 0.0429(6) 0.3846(5) 0.0209(16) Uani 1 d . . . C2 C 0.3991(7) 0.0916(6) 0.5300(5) 0.0234(17) Uani 1 d . . . C3 C 0.3431(8) -0.1418(7) 0.4252(5) 0.0262(17) Uani 1 d . . . C4 C 0.1578(7) -0.0007(7) 0.0687(5) 0.0260(17) Uani 1 d . . . C5 C 0.0131(7) 0.1244(7) 0.1092(5) 0.0258(17) Uani 1 d . . . C6 C 0.0945(8) 0.1194(8) -0.0519(5) 0.0290(19) Uani 1 d . . . C7 C 0.5099(9) 0.2309(9) 0.1387(6) 0.043(2) Uani 1 d . . . H7 H 0.4325 0.2318 0.1463 0.052 Uiso 1 d R . . C8 C 0.6013(10) 0.3379(9) 0.1375(7) 0.055(3) Uani 1 d . . . H8 H 0.5869 0.4092 0.1444 0.066 Uiso 1 d R . . C9 C 0.7179(10) 0.3343(11) 0.1252(7) 0.063(3) Uani 1 d . . . H9 H 0.7828 0.4039 0.1241 0.076 Uiso 1 d R . . C10 C 0.7339(9) 0.2235(10) 0.1146(7) 0.054(3) Uani 1 d . . . H10 H 0.8088 0.2183 0.1047 0.065 Uiso 1 d R . . C11 C 0.6382(8) 0.1239(9) 0.1191(6) 0.041(2) Uani 1 d . . . C12 C 0.6511(8) 0.0107(9) 0.1188(6) 0.041(2) Uani 1 d . . . H12 H 0.7243 -0.0003 0.1106 0.050 Uiso 1 d R . . C13 C 0.5693(10) -0.1887(9) 0.1341(8) 0.061(3) Uani 1 d . . . H13A H 0.5418 -0.2433 0.0677 0.074 Uiso 1 d R . . H13B H 0.6591 -0.1719 0.1630 0.074 Uiso 1 d R . . C14 C 0.4957(13) -0.2510(12) 0.1875(10) 0.090(4) Uani 1 d . . . H14A H 0.5361 -0.2018 0.2558 0.108 Uiso 1 d R . . H14B H 0.5067 -0.3272 0.1811 0.108 Uiso 1 d R . . C15 C 0.3592(10) -0.2816(10) 0.1673(9) 0.069(3) Uani 1 d . . . H15A H 0.3305 -0.3221 0.2132 0.083 Uiso 1 d R . . H15B H 0.3160 -0.3413 0.1025 0.083 Uiso 1 d R . . C16 C -0.0250(8) 0.4384(8) 0.3483(6) 0.034(2) Uani 1 d . . . H16 H 0.0353 0.4741 0.3189 0.041 Uiso 1 d R . . C17 C -0.0972(8) 0.5004(7) 0.3786(6) 0.0327(19) Uani 1 d . . . H17 H -0.0830 0.5776 0.3724 0.039 Uiso 1 d R . . C18 C -0.1896(8) 0.4462(8) 0.4179(6) 0.034(2) Uani 1 d . . . H18 H -0.2383 0.4867 0.4400 0.041 Uiso 1 d R . . C19 C -0.2099(8) 0.3310(7) 0.4245(6) 0.0333(19) Uani 1 d . . . H19 H -0.2743 0.2917 0.4492 0.040 Uiso 1 d R . . C20 C -0.1336(7) 0.2743(7) 0.3939(5) 0.0249(17) Uani 1 d . . . C21 C -0.1506(7) 0.1500(7) 0.3913(5) 0.0262(17) Uani 1 d . . . H21 H -0.2136 0.1029 0.4134 0.031 Uiso 1 d R . . C22 C -0.0951(7) -0.0193(7) 0.3442(6) 0.0302(18) Uani 1 d . . . H22A H -0.1369 -0.0664 0.2755 0.036 Uiso 1 d R . . H22B H -0.1518 -0.0530 0.3803 0.036 Uiso 1 d R . . C23 C 0.0311(7) -0.0325(7) 0.3785(5) 0.0288(18) Uani 1 d . . . H23A H 0.0760 0.0195 0.4458 0.035 Uiso 1 d R . . H23B H 0.0125 -0.1167 0.3766 0.035 Uiso 1 d R . . C24 C 0.1186(7) 0.0022(7) 0.3160(6) 0.0288(18) Uani 1 d . . . H24A H 0.1897 -0.0219 0.3327 0.035 Uiso 1 d R . . H24B H 0.0704 -0.0421 0.2476 0.035 Uiso 1 d R . . C25 C 0.2885(7) 0.1903(7) 0.3411(5) 0.0293(18) Uani 1 d . . . H25 H 0.3436 0.1501 0.3402 0.035 Uiso 1 d R . . C26 C 0.3351(7) 0.3213(7) 0.3550(5) 0.0298(18) Uani 1 d . . . C27 C 0.4614(8) 0.3876(8) 0.3617(6) 0.043(2) Uani 1 d . . . H27 H 0.5178 0.3491 0.3583 0.051 Uiso 1 d R . . C28 C 0.5033(8) 0.5106(8) 0.3732(7) 0.046(2) Uani 1 d . . . H28 H 0.5871 0.5566 0.3759 0.055 Uiso 1 d R . . C29 C 0.4169(8) 0.5634(8) 0.3808(6) 0.041(2) Uani 1 d . . . H29 H 0.4422 0.6469 0.3898 0.049 Uiso 1 d R . . C30 C 0.2932(8) 0.4925(7) 0.3749(6) 0.0332(19) Uani 1 d . . . H30 H 0.2365 0.5302 0.3809 0.040 Uiso 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0260(8) 0.0240(8) 0.0165(8) 0.0061(7) 0.0083(6) 0.0153(7) Fe2 0.0207(8) 0.0253(8) 0.0204(8) 0.0039(7) 0.0078(6) 0.0133(7) Cu1 0.0299(6) 0.0524(7) 0.0269(6) 0.0131(5) 0.0119(5) 0.0250(5) Cu2 0.0264(5) 0.0234(5) 0.0284(5) 0.0084(4) 0.0140(4) 0.0127(4) O1 0.045(4) 0.032(3) 0.107(6) 0.028(4) 0.044(4) 0.025(3) O2 0.058(4) 0.053(4) 0.048(4) 0.014(3) 0.006(3) 0.008(4) O3 0.079(5) 0.048(4) 0.089(6) 0.029(4) 0.045(4) 0.025(4) O4 0.127(8) 0.060(5) 0.092(6) 0.016(5) 0.031(6) 0.031(5) N1 0.029(4) 0.032(4) 0.028(4) 0.013(3) 0.011(3) 0.014(3) N2 0.033(4) 0.033(4) 0.033(4) 0.009(3) 0.011(3) 0.021(3) N3 0.033(4) 0.040(4) 0.043(4) 0.009(4) 0.011(4) 0.006(4) N4 0.034(4) 0.046(4) 0.028(4) 0.012(3) 0.011(3) 0.021(3) N5 0.034(4) 0.034(4) 0.028(4) 0.010(3) 0.011(3) 0.019(3) N6 0.054(5) 0.041(4) 0.039(4) 0.014(4) 0.026(4) 0.022(4) N7 0.037(4) 0.061(5) 0.027(4) 0.021(4) 0.014(3) 0.028(4) N8 0.029(4) 0.056(5) 0.034(4) 0.006(4) 0.010(3) 0.026(4) N9 0.041(4) 0.052(5) 0.035(4) 0.014(4) 0.011(3) 0.025(4) N10 0.032(4) 0.027(4) 0.026(3) 0.008(3) 0.017(3) 0.017(3) N11 0.026(3) 0.029(4) 0.023(3) 0.006(3) 0.009(3) 0.011(3) N12 0.027(4) 0.024(3) 0.023(3) 0.007(3) 0.008(3) 0.009(3) N13 0.027(3) 0.022(3) 0.024(3) 0.006(3) 0.009(3) 0.010(3) C1 0.019(4) 0.020(4) 0.022(4) 0.000(3) 0.004(3) 0.011(3) C2 0.033(4) 0.019(4) 0.017(4) 0.008(3) 0.004(3) 0.009(4) C3 0.039(5) 0.030(5) 0.029(4) 0.016(4) 0.020(4) 0.027(4) C4 0.027(4) 0.032(4) 0.022(4) 0.004(3) 0.017(4) 0.014(4) C5 0.023(4) 0.034(5) 0.023(4) 0.007(4) 0.007(3) 0.015(4) C6 0.032(5) 0.042(5) 0.025(4) 0.012(4) 0.016(4) 0.024(4) C7 0.047(6) 0.063(7) 0.038(5) 0.026(5) 0.023(4) 0.034(5) C8 0.071(7) 0.057(7) 0.048(6) 0.022(5) 0.024(5) 0.032(6) C9 0.045(6) 0.075(8) 0.045(6) 0.016(6) 0.008(5) 0.001(6) C10 0.034(5) 0.080(8) 0.062(7) 0.029(6) 0.025(5) 0.029(6) C11 0.030(5) 0.068(7) 0.026(5) 0.012(4) 0.014(4) 0.021(5) C12 0.025(5) 0.068(7) 0.031(5) 0.009(5) 0.005(4) 0.025(5) C13 0.051(6) 0.063(7) 0.069(7) 0.001(6) 0.013(6) 0.038(6) C14 0.122(11) 0.107(10) 0.131(12) 0.084(10) 0.089(10) 0.093(10) C15 0.062(7) 0.063(7) 0.096(9) 0.032(7) 0.037(7) 0.028(6) C16 0.044(5) 0.040(5) 0.035(5) 0.014(4) 0.026(4) 0.026(4) C17 0.044(5) 0.022(4) 0.034(5) 0.007(4) 0.009(4) 0.017(4) C18 0.038(5) 0.047(5) 0.028(4) 0.012(4) 0.014(4) 0.026(4) C19 0.037(5) 0.035(5) 0.033(5) 0.008(4) 0.019(4) 0.018(4) C20 0.025(4) 0.024(4) 0.018(4) 0.000(3) 0.002(3) 0.009(3) C21 0.028(4) 0.033(4) 0.021(4) 0.011(3) 0.011(3) 0.014(4) C22 0.036(5) 0.023(4) 0.036(5) 0.010(4) 0.016(4) 0.014(4) C23 0.038(5) 0.026(4) 0.029(4) 0.014(4) 0.011(4) 0.016(4) C24 0.029(4) 0.029(4) 0.031(4) 0.011(4) 0.005(4) 0.016(4) C25 0.036(5) 0.037(5) 0.022(4) 0.006(4) 0.011(4) 0.023(4) C26 0.036(5) 0.028(4) 0.025(4) 0.008(4) 0.006(4) 0.015(4) C27 0.025(5) 0.046(6) 0.060(6) 0.016(5) 0.018(4) 0.016(4) C28 0.030(5) 0.041(6) 0.055(6) 0.014(5) 0.014(4) 0.001(4) C29 0.047(5) 0.029(5) 0.041(5) 0.016(4) 0.013(4) 0.006(4) C30 0.033(5) 0.031(5) 0.034(5) 0.007(4) 0.013(4) 0.011(4) _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 Fe1 C1 1.892(8) 2_656 ? Fe1 C1 1.892(8) . ? Fe1 C2 1.925(8) . ? Fe1 C2 1.925(8) 2_656 ? Fe1 C3 1.925(9) . ? Fe1 C3 1.925(9) 2_656 ? Fe2 C5 1.893(7) . ? Fe2 C5 1.893(7) 2 ? Fe2 C4 1.904(8) . ? Fe2 C4 1.904(8) 2 ? Fe2 C6 1.913(8) 2 ? Fe2 C6 1.913(8) . ? Cu1 N4 1.975(7) . ? Cu1 N9 2.007(7) . ? Cu1 N7 2.011(7) . ? Cu1 N8 2.041(6) . ? Cu1 N1 2.162(6) . ? Cu2 N12 1.981(6) . ? Cu2 N11 2.015(6) . ? Cu2 N10 2.021(6) . ? Cu2 N13 2.110(6) . ? Cu2 N5 2.127(6) . ? O5A O5B 1.25(3) . ? O6A O6B 0.81(3) . ? O7A O7A 1.43(4) 2_665 ? N1 C1 1.165(9) . ? N2 C2 1.158(9) . ? N3 C3 1.167(9) . ? N4 C4 1.167(9) . ? N5 C5 1.153(9) . ? N6 C6 1.145(9) . ? N7 C7 1.318(10) . ? N7 C11 1.362(10) . ? N8 C12 1.264(10) . ? N8 C13 1.465(12) . ? N9 C15 1.461(12) . ? N9 H9A 0.8999 . ? N9 H9B 0.9000 . ? N10 C16 1.305(9) . ? N10 C20 1.368(9) . ? N11 C21 1.273(9) . ? N11 C22 1.458(9) . ? N12 C25 1.280(9) . ? N12 C24 1.443(9) . ? N13 C30 1.328(9) . ? N13 C26 1.340(9) . ? C7 C8 1.381(12) . ? C7 H7 0.9300 . ? C8 C9 1.413(13) . ? C8 H8 0.9301 . ? C9 C10 1.408(14) . ? C9 H9 0.9300 . ? C10 C11 1.365(12) . ? C10 H10 0.9300 . ? C11 C12 1.440(12) . ? C12 H12 0.9300 . ? C13 C14 1.423(14) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.443(14) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9699 . ? C16 C17 1.383(10) . ? C16 H16 0.9300 . ? C17 C18 1.364(11) . ? C17 H17 0.9300 . ? C18 C19 1.376(11) . ? C18 H18 0.9300 . ? C19 C20 1.382(10) . ? C19 H19 0.9301 . ? C20 C21 1.455(10) . ? C21 H21 0.9299 . ? C22 C23 1.521(10) . ? C22 H22A 0.9701 . ? C22 H22B 0.9700 . ? C23 C24 1.524(10) . ? C23 H23A 0.9700 . ? C23 H23B 0.9701 . ? C24 H24A 0.9700 . ? C24 H24B 0.9699 . ? C25 C26 1.456(10) . ? C25 H25 0.9300 . ? C26 C27 1.381(11) . ? C27 C28 1.371(12) . ? C27 H27 0.9300 . ? C28 C29 1.373(12) . ? C28 H28 0.9300 . ? C29 C30 1.372(11) . ? C29 H29 0.9299 . ? 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 C1 Fe1 C1 180.0 2_656 . ? C1 Fe1 C2 89.1(3) 2_656 . ? C1 Fe1 C2 90.9(3) . . ? C1 Fe1 C2 90.9(3) 2_656 2_656 ? C1 Fe1 C2 89.1(3) . 2_656 ? C2 Fe1 C2 180.000(2) . 2_656 ? C1 Fe1 C3 91.5(3) 2_656 . ? C1 Fe1 C3 88.5(3) . . ? C2 Fe1 C3 89.3(3) . . ? C2 Fe1 C3 90.7(3) 2_656 . ? C1 Fe1 C3 88.5(3) 2_656 2_656 ? C1 Fe1 C3 91.5(3) . 2_656 ? C2 Fe1 C3 90.7(3) . 2_656 ? C2 Fe1 C3 89.3(3) 2_656 2_656 ? C3 Fe1 C3 180.0 . 2_656 ? C5 Fe2 C5 180.0 . 2 ? C5 Fe2 C4 90.4(3) . . ? C5 Fe2 C4 89.6(3) 2 . ? C5 Fe2 C4 89.6(3) . 2 ? C5 Fe2 C4 90.4(3) 2 2 ? C4 Fe2 C4 180.0 . 2 ? C5 Fe2 C6 88.6(3) . 2 ? C5 Fe2 C6 91.4(3) 2 2 ? C4 Fe2 C6 90.6(3) . 2 ? C4 Fe2 C6 89.4(3) 2 2 ? C5 Fe2 C6 91.4(3) . . ? C5 Fe2 C6 88.6(3) 2 . ? C4 Fe2 C6 89.4(3) . . ? C4 Fe2 C6 90.6(3) 2 . ? C6 Fe2 C6 180.0 2 . ? N4 Cu1 N9 90.6(3) . . ? N4 Cu1 N7 92.9(3) . . ? N9 Cu1 N7 173.9(3) . . ? N4 Cu1 N8 151.8(3) . . ? N9 Cu1 N8 94.1(3) . . ? N7 Cu1 N8 80.5(3) . . ? N4 Cu1 N1 109.8(2) . . ? N9 Cu1 N1 92.3(3) . . ? N7 Cu1 N1 91.2(3) . . ? N8 Cu1 N1 97.8(3) . . ? N12 Cu2 N11 92.0(2) . . ? N12 Cu2 N10 167.3(2) . . ? N11 Cu2 N10 80.8(2) . . ? N12 Cu2 N13 81.1(2) . . ? N11 Cu2 N13 156.3(2) . . ? N10 Cu2 N13 101.3(2) . . ? N12 Cu2 N5 93.8(2) . . ? N11 Cu2 N5 108.6(2) . . ? N10 Cu2 N5 98.4(2) . . ? N13 Cu2 N5 94.6(2) . . ? C1 N1 Cu1 140.8(6) . . ? C4 N4 Cu1 169.0(6) . . ? C5 N5 Cu2 136.4(6) . . ? C7 N7 C11 119.1(8) . . ? C7 N7 Cu1 127.6(6) . . ? C11 N7 Cu1 112.2(6) . . ? C12 N8 C13 120.9(8) . . ? C12 N8 Cu1 113.5(6) . . ? C13 N8 Cu1 125.3(6) . . ? C15 N9 Cu1 122.8(6) . . ? C15 N9 H9A 106.6 . . ? Cu1 N9 H9A 106.6 . . ? C15 N9 H9B 106.6 . . ? Cu1 N9 H9B 106.6 . . ? H9A N9 H9B 106.6 . . ? C16 N10 C20 118.6(6) . . ? C16 N10 Cu2 129.5(5) . . ? C20 N10 Cu2 111.9(5) . . ? C21 N11 C22 120.7(6) . . ? C21 N11 Cu2 114.2(5) . . ? C22 N11 Cu2 125.2(5) . . ? C25 N12 C24 119.5(6) . . ? C25 N12 Cu2 115.0(5) . . ? C24 N12 Cu2 125.5(5) . . ? C30 N13 C26 117.2(6) . . ? C30 N13 Cu2 133.7(5) . . ? C26 N13 Cu2 108.7(5) . . ? N1 C1 Fe1 177.1(6) . . ? N2 C2 Fe1 179.1(6) . . ? N3 C3 Fe1 177.8(7) . . ? N4 C4 Fe2 178.2(7) . . ? N5 C5 Fe2 178.7(7) . . ? N6 C6 Fe2 179.5(8) . . ? N7 C7 C8 124.1(9) . . ? N7 C7 H7 117.9 . . ? C8 C7 H7 117.9 . . ? C7 C8 C9 117.0(10) . . ? C7 C8 H8 121.5 . . ? C9 C8 H8 121.5 . . ? C10 C9 C8 118.9(10) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C11 C10 C9 119.2(9) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? N7 C11 C10 121.6(9) . . ? N7 C11 C12 115.2(8) . . ? C10 C11 C12 123.1(8) . . ? N8 C12 C11 118.1(8) . . ? N8 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? C14 C13 N8 115.5(8) . . ? C14 C13 H13A 108.4 . . ? N8 C13 H13A 108.4 . . ? C14 C13 H13B 108.4 . . ? N8 C13 H13B 108.4 . . ? H13A C13 H13B 107.5 . . ? C13 C14 C15 122.4(11) . . ? C13 C14 H14A 106.7 . . ? C15 C14 H14A 106.7 . . ? C13 C14 H14B 106.7 . . ? C15 C14 H14B 106.7 . . ? H14A C14 H14B 106.6 . . ? C14 C15 N9 118.7(9) . . ? C14 C15 H15A 107.7 . . ? N9 C15 H15A 107.7 . . ? C14 C15 H15B 107.6 . . ? N9 C15 H15B 107.6 . . ? H15A C15 H15B 107.1 . . ? N10 C16 C17 123.1(7) . . ? N10 C16 H16 118.4 . . ? C17 C16 H16 118.5 . . ? C18 C17 C16 118.7(7) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C17 C18 C19 119.3(7) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.3 . . ? C18 C19 C20 119.2(7) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? N10 C20 C19 120.8(7) . . ? N10 C20 C21 114.6(6) . . ? C19 C20 C21 124.6(7) . . ? N11 C21 C20 117.6(7) . . ? N11 C21 H21 121.2 . . ? C20 C21 H21 121.2 . . ? N11 C22 C23 112.4(6) . . ? N11 C22 H22A 109.1 . . ? C23 C22 H22A 109.1 . . ? N11 C22 H22B 109.1 . . ? C23 C22 H22B 109.1 . . ? H22A C22 H22B 107.9 . . ? C22 C23 C24 112.4(6) . . ? C22 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? C22 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? N12 C24 C23 111.6(6) . . ? N12 C24 H24A 109.3 . . ? C23 C24 H24A 109.3 . . ? N12 C24 H24B 109.3 . . ? C23 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? N12 C25 C26 117.7(7) . . ? N12 C25 H25 121.1 . . ? C26 C25 H25 121.2 . . ? N13 C26 C27 122.6(7) . . ? N13 C26 C25 117.0(7) . . ? C27 C26 C25 120.4(7) . . ? C28 C27 C26 119.6(8) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 117.7(8) . . ? C27 C28 H28 121.2 . . ? C29 C28 H28 121.2 . . ? C30 C29 C28 119.7(8) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? N13 C30 C29 123.2(8) . . ? N13 C30 H30 118.4 . . ? C29 C30 H30 118.4 . . ? _diffrn_measured_fraction_theta_max 0.841 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.841 _refine_diff_density_max 0.543 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.107 # END OF CIF data_global _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? #ActaC _publ_contact_author #ActaC ; Prof. Enrique Colacio Departamento de Qu\'imica Inorg\'anica Facultad de Ciencias Universidad de Granada E-18071 Granada Spain ; _publ_contact_letter #ActaC ; Please consider this CIF submission as crystallographic information for compound 1 of manuscript ref. 9/08485A. ; _publ_contact_author_phone '+34 58 243236' #ActaC _publ_contact_author_fax '+34 58 243322' #ActaC _publ_contact_author_email 'ecolacio@ugr.es' #ActaC loop_ _publ_author_name #ActaC _publ_author_address #ActaC 'Colacio, E.' ; Departamento de Qu\'imica Inorg\'anica Facultad de Ciencias Universidad de Granada E-18071 Granada Spain ; 'Dominguez-Vera, J.-M.' ; Departamento de Qu\'imica Inorg\'anica Facultad de Ciencias Universidad de Granada E-18071 Granada Spain ; 'Ghazi, M,' ; Departamento de Qu\'imica Inorg\'anica Facultad de Ciencias Universidad de Granada E-18071 Granada Spain ; 'Kivek\"as, R.' ; Laboratory of Inorganic Chemistry Department of Chemistry P.O.Box 55 FIN-00014 University of Helsinki Finland ; 'Moreno, J.-M.' ; Departamento de Qu\'imica Inorg\'anica Facultad de Ciencias Universidad de Granada E-18071 Granada Spain ; 'Pajunen, A.' ; Laboratory of Inorganic Chemistry Department of Chemistry P.O.Box 55 FIN-00014 University of Helsinki Finland ; _publ_section_title #ActaC ; ? ; _publ_section_abstract #ActaC ; ? ; _publ_section_comment #ActaC ; ? ; _publ_section_experimental #ActaC ; ? ; _publ_section_references #ActaC ; ? ; _publ_section_figure_captions #ActaC ; ? ; _publ_section_acknowledgements #ActaC ; ? ; #============================================================================== # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? data_compound1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C16 H24 Cu Fe N10, 4(H2 O), K' _chemical_formula_sum 'C16 H32 Cu Fe K N10 O4' _chemical_formula_weight 587.01 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' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' 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' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 14.405(3) _cell_length_b 12.284(3) _cell_length_c 9.836(2) _cell_angle_alpha 90.00 _cell_angle_beta 131.59(3) _cell_angle_gamma 90.00 _cell_volume 1301.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 12.5 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 1.575 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_process_details ? _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 'Siemens STADI4' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 4 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% 2.6 _diffrn_reflns_number 1156 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0575 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1156 _reflns_number_gt 842 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Electron density synthesis with coefficients Fo-Fc Highest peak 0.90 at 0.4497 0.0000 0.4170 [ 0.64 A from CU ] Deepest hole -1.53 at 0.0000 0.0381 0.0000 [ 0.47 A from FE ] ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1601P)^2^+4.7622P] 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_number_reflns 1156 _refine_ls_number_parameters 91 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1071 _refine_ls_R_factor_gt 0.0819 _refine_ls_wR_factor_ref 0.2595 _refine_ls_wR_factor_gt 0.2355 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.140 _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 0.0000 0.5000 0.5000 0.0311(4) Uani 1 d S . . Fe Fe 0.5000 0.5000 1.0000 0.0468(6) Uani 1 d S . . K K 0.3280(8) 0.5000 0.4101(12) 0.115(3) Uani 0.50 d SP . . O O 0.1852(5) 0.3231(6) 0.3532(9) 0.083(2) Uani 1 d . . . N1 N 0.2236(7) 0.5000 0.6527(12) 0.061(3) Uani 1 d S . . N2 N 0.5674(7) 0.5000 0.7610(11) 0.072(3) Uani 1 d SD . . N3 N 0.5000 0.7450(9) 1.0000 0.106(5) Uani 1 d SD . . N4 N -0.0283(4) 0.6196(5) 0.3363(7) 0.0467(15) Uani 1 d . . . H4 H 0.0435 0.6274 0.3583 0.056 Uiso 1 calc R . . C1 C 0.3249(9) 0.5000 0.7785(14) 0.049(3) Uani 1 d S . . C2 C 0.5447(6) 0.5000 0.8532(10) 0.036(2) Uani 1 d SD . . C3 C 0.5000 0.6543(8) 1.0000 0.044(2) Uani 1 d SD . . C4 C -0.0467(7) 0.7223(7) 0.3975(9) 0.076(3) Uani 1 d D . . H4A H -0.1303 0.7252 0.3525 0.091 Uiso 1 calc R . . H4B H -0.0341 0.7851 0.3517 0.091 Uiso 1 calc R . . C5 C -0.1301(7) 0.6022(8) 0.1357(10) 0.077(3) Uani 1 d D . . H5A H -0.2092 0.5970 0.1053 0.092 Uiso 1 calc R . . H5B H -0.1337 0.6634 0.0702 0.092 Uiso 1 calc R . . C6 C -0.1061(12) 0.5000 0.0816(16) 0.109(7) Uani 1 d SD . . H6A H -0.1577 0.5000 -0.0494 0.130 Uiso 1 calc SR . . H6B H -0.0202 0.5000 0.1355 0.130 Uiso 1 calc SR . . 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 0.0459(6) 0.0229(7) 0.0299(6) 0.000 0.0275(5) 0.000 Fe 0.0336(8) 0.0622(14) 0.0395(9) 0.000 0.0221(7) 0.000 K 0.127(4) 0.128(7) 0.133(5) 0.000 0.104(4) 0.000 O 0.060(2) 0.100(5) 0.097(4) 0.027(4) 0.055(3) 0.017(3) N1 0.034(4) 0.080(7) 0.045(5) 0.000 0.016(3) 0.000 N2 0.063(4) 0.096(9) 0.069(5) 0.000 0.049(4) 0.000 N3 0.077(6) 0.163(16) 0.074(7) 0.000 0.048(5) 0.000 N4 0.0283(19) 0.060(4) 0.048(3) 0.026(3) 0.0240(19) 0.013(2) C1 0.040(4) 0.057(7) 0.049(5) 0.000 0.029(4) 0.000 C2 0.022(3) 0.057(6) 0.026(3) 0.000 0.014(3) 0.000 C3 0.037(4) 0.047(6) 0.037(4) 0.000 0.021(3) 0.000 C4 0.071(4) 0.049(5) 0.129(6) 0.040(4) 0.075(4) 0.020(4) C5 0.045(3) 0.129(9) 0.046(3) 0.042(5) 0.026(3) 0.020(5) C6 0.067(6) 0.23(2) 0.038(5) 0.000 0.038(5) 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 N4 2.012(6) 6_565 ? Cu N4 2.012(6) 2_556 ? Cu N4 2.012(6) 5_566 ? Cu N4 2.012(6) . ? Cu N1 2.492(9) 5_566 ? Cu N1 2.492(9) . ? Fe C3 1.895(10) 5_667 ? Fe C3 1.895(10) . ? Fe C2 1.933(8) 5_667 ? Fe C2 1.933(8) . ? Fe C1 1.952(9) . ? Fe C1 1.952(9) 5_667 ? K O 2.782(9) . ? K O 2.782(9) 6_565 ? K N2 2.829(12) . ? N1 C1 1.124(12) . ? N2 C2 1.151(8) . ? N3 C3 1.115(9) . ? N4 C4 1.495(11) . ? N4 C5 1.499(9) . ? N4 H4 0.9100 . ? C4 C4 1.508(14) 2_556 ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.491(11) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C5 1.491(11) 6_565 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? 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 N4 Cu N4 180.000(1) 6_565 2_556 ? N4 Cu N4 86.2(4) 6_565 5_566 ? N4 Cu N4 93.8(4) 2_556 5_566 ? N4 Cu N4 93.8(4) 6_565 . ? N4 Cu N4 86.2(4) 2_556 . ? N4 Cu N4 180.0 5_566 . ? N4 Cu N1 91.4(2) 6_565 5_566 ? N4 Cu N1 88.6(2) 2_556 5_566 ? N4 Cu N1 88.6(2) 5_566 5_566 ? N4 Cu N1 91.4(2) . 5_566 ? N4 Cu N1 88.6(2) 6_565 . ? N4 Cu N1 91.4(2) 2_556 . ? N4 Cu N1 91.4(2) 5_566 . ? N4 Cu N1 88.6(2) . . ? N1 Cu N1 180.0 5_566 . ? C3 Fe C3 180.000(2) 5_667 . ? C3 Fe C2 90.000(4) 5_667 5_667 ? C3 Fe C2 90.000(2) . 5_667 ? C3 Fe C2 90.000(1) 5_667 . ? C3 Fe C2 90.000(4) . . ? C2 Fe C2 180.000(2) 5_667 . ? C3 Fe C1 90.000(7) 5_667 . ? C3 Fe C1 90.000(1) . . ? C2 Fe C1 90.5(4) 5_667 . ? C2 Fe C1 89.5(4) . . ? C3 Fe C1 90.000(2) 5_667 5_667 ? C3 Fe C1 90.000(7) . 5_667 ? C2 Fe C1 89.5(4) 5_667 5_667 ? C2 Fe C1 90.5(4) . 5_667 ? C1 Fe C1 180.000(1) . 5_667 ? O K O 102.8(4) . 6_565 ? O K N2 112.7(3) . . ? O K N2 112.7(3) 6_565 . ? C1 N1 Cu 151.4(9) . . ? C2 N2 K 102.0(6) . . ? C4 N4 C5 111.8(6) . . ? C4 N4 Cu 106.8(5) . . ? C5 N4 Cu 116.8(5) . . ? C4 N4 H4 107.0 . . ? C5 N4 H4 107.0 . . ? Cu N4 H4 107.0 . . ? N1 C1 Fe 178.8(11) . . ? N2 C2 Fe 177.8(7) . . ? N3 C3 Fe 180.000(3) . . ? N4 C4 C4 107.4(4) . 2_556 ? N4 C4 H4A 110.2 . . ? C4 C4 H4A 110.2 2_556 . ? N4 C4 H4B 110.2 . . ? C4 C4 H4B 110.2 2_556 . ? H4A C4 H4B 108.5 . . ? C6 C5 N4 109.5(7) . . ? C6 C5 H5A 109.8 . . ? N4 C5 H5A 109.8 . . ? C6 C5 H5B 109.8 . . ? N4 C5 H5B 109.8 . . ? H5A C5 H5B 108.2 . . ? C5 C6 C5 114.7(11) 6_565 . ? C5 C6 H6A 108.6 6_565 . ? C5 C6 H6A 108.6 . . ? C5 C6 H6B 108.6 6_565 . ? C5 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.478 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.478 _refine_diff_density_max 0.905 _refine_diff_density_min -1.532 _refine_diff_density_rms 0.172 #===END