# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1541 data_global # Paper ref: B000408L #SUBMISSION DETAILS _pulic_contact_author ; Dr G\'abor Speier Department of Organic Chemistry University of Veszpr\'em Wartha V. u. 1 H-8201 Veszpr\'em Hungary ; _publ_contact_author_email speier@almos.vein.hu _publ_contact_author_fax '36(88)427492' _publ_contact_author_phone '36(88)422022' _publ_requested_journal 'Chem. Comm.' #=========================================================== #TITLE AND AUTHOR LIST _publ_section_title ;Preparation and Characterization of Homoleptic and Ethoxy-bridged Nitronato Iron(III) Complexes ; loop_ _publ_author_name _publ_author_address 'Kovacs, Tibor' ;Department of Organic Chemistry University of Veszpr\'em 8201 Veszpr\'em Hungary ; 'Speier, Gabor' ;Department of Organic Chemistry University of Veszpr\'em 8201 Veszpr\'em Hungary Research Group for Petrochemistry of the Hungarian Academy of Sciences 8201 Veszpr\'em Hungary ; 'Reglier, Marius' ;Chimie, Biologie et Radicaux Libres, UMR CNRS 6517 Universites d'Aix-Marseille 1 et 3 Facult des Sciences et Techniques de Saint Jerme, case 432 avenue Escadrille Normandie-Niemen 13397 Marseille Cedex 20, France ; 'Giorgi, Michel' ;Chimie, Biologie et Radicaux Libres, UMR CNRS 6517 Universites d'Aix-Marseille 1 et 3 Facult des Sciences et Techniques de Saint Jerme, case 432 avenue Escadrille Normandie-Niemen 13397 Marseille Cedex 20, France ; 'Vertes, Attila' Hungarian Academy of Sciences at Eotvos University Research Goup for Nuclear Methods in Stuctural Chemistry 1518 Budapest Hungary ; 'Vanko, Gyorgy' Hungarian Academy of Sciences at Eotvos University Research Goup for Nuclear Methods in Stuctural Chemistry 1518 Budapest Hungary ; #===================================================== data_kt7 _publ_section_abstract ; We present the crystal and molecular structure of Compound kt7 ; _publ_section_comment ; The study of the titled structure was undertaken to establish its three dimensional structure. Geometries are tabulated below. All Diagrams and calculations were performed using maXus (MacScience, Japan). ; _chemical_compound_source 'Local laboratory' _exptl_crystal_description 'prism' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _chemical_formula_sum 'C9 H18 Fe1 O6 N3' _chemical_formula_weight 320.10 _cell_length_a 12.395(1) _cell_length_b 9.226(1) _cell_length_c 13.343(1) _cell_angle_alpha 90.000(1) _cell_angle_beta 109.082(1) _cell_angle_gamma 90.000(1) _cell_volume 1442.0(4) _cell_measurement_reflns_used ? _cell_measurement_theta_min '1' _cell_measurement_theta_max '25' _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.47 _exptl_crystal_density_meas 1.25 _exptl_absorpt_coefficient_mu 10.698 _cell_measurement_temperature '298' _exptl_absorpt_correction_type 'none' _diffrn_reflns_number 3070 _reflns_number_total 2889 _reflns_number_observed 2153 _reflns_observed_criterion 'refl_observed_if_I_>_3.00_sigma(I)' _diffrn_reflns_theta_max 25.41 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.032 _refine_ls_wR_factor_obs 0.033 _refine_ls_hydrogen_treatment 'noref' _refine_ls_number_reflns 2153 _refine_ls_number_parameters 226 _refine_ls_goodness_of_fit_obs 0.850 _refine_ls_weighting_scheme 'Unit' _refine_ls_shift/esd_max 0.3806 _refine_ls_shift/esd_mean 0.0188 _refine_diff_density_min -0.27 _refine_diff_density_max 0.19 _refine_ls_extinction_method 'None' _atom_type_scat_source 'D.Waasmaier&A.Kirfel,Acta Cryst.1995,A51, 416-431' _computing_data_reduction 'maXus' _computing_molecular_graphics 'maXus' _computing_publication_material 'maXus' _computing_structure_refinement 'maXus' _computing_structure_solution 'maXus' _diffrn_measurement_device 'KappaCCD' _computing_data_collection 'KappaCCD' _diffrn_radiation_type 'xray' _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_radiation_wavelength 0.71073 _diffrn_orient_matrix_type 'X=UH' _diffrn_orient_matrix_UB_11 0.01000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.01000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.01000 loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z -X+0.5,+Y+0.5,-Z+0.5 +X+0.5,-Y+0.5,+Z+0.5 _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_cell_setting 'Monoclinic' #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Fe1 0.26710(3) 0.23860(4) 0.01170(3) 0.0375(2) 1.00 Uij O2 0.3090(2) 0.3591(2) -0.0966(2) 0.046(1) 1.00 Uij O3 0.3013(2) 0.1504(2) 0.1579(2) 0.046(1) 1.00 Uij O4 0.0975(2) 0.2589(2) -0.0181(2) 0.046(1) 1.00 Uij O5 0.3044(2) 0.4468(2) 0.0552(2) 0.046(1) 1.00 Uij O6 0.1731(2) 0.0827(2) -0.0836(2) 0.046(1) 1.00 Uij O7 0.4146(2) 0.1269(2) 0.0618(2) 0.050(1) 1.00 Uij N8 0.3980(2) 0.0905(3) 0.1528(2) 0.043(1) 1.00 Uij N9 0.3243(2) 0.4781(3) -0.0357(2) 0.037(1) 1.00 Uij N10 0.0754(2) 0.1385(3) -0.0773(2) 0.041(1) 1.00 Uij C11 0.3533(2) 0.6033(3) -0.0602(2) 0.042(1) 1.00 Uij C12 0.3683(4) 0.7236(4) 0.0163(3) 0.072(2) 1.00 Uij C13 -0.1251(3) 0.1565(4) -0.1051(3) 0.061(2) 1.00 Uij C14 0.4654(3) 0.0099(3) 0.2260(3) 0.053(2) 1.00 Uij C15 -0.0249(3) 0.0842(3) -0.1204(2) 0.046(2) 1.00 Uij C16 -0.0372(4) -0.0509(5) -0.1833(3) 0.065(2) 1.00 Uij C17 0.5720(3) -0.0437(5) 0.2112(4) 0.074(2) 1.00 Uij C18 0.3746(3) 0.6225(5) -0.1629(3) 0.059(2) 1.00 Uij C19 0.4345(5) -0.0244(4) 0.3221(3) 0.073(2) 1.00 Uij H13A -0.100(3) 0.238(5) -0.053(3) 0.05000 1.00 Uiso H13B -0.168(3) 0.090(5) -0.086(3) 0.05000 1.00 Uiso H16A 0.038(4) -0.095(5) -0.181(3) 0.05000 1.00 Uiso H13C -0.169(3) 0.198(4) -0.173(3) 0.05000 1.00 Uiso H18A 0.454(4) 0.647(4) -0.146(3) 0.05000 1.00 Uiso H18B 0.350(3) 0.545(5) -0.207(3) 0.05000 1.00 Uiso H12A 0.348(3) 0.703(4) 0.078(3) 0.05000 1.00 Uiso H18C 0.325(3) 0.696(5) -0.201(3) 0.05000 1.00 Uiso H16B -0.087(3) -0.027(4) -0.260(3) 0.05000 1.00 Uiso H19A 0.496(3) 0.021(4) 0.384(3) 0.05000 1.00 Uiso H19B 0.355(4) 0.017(5) 0.315(3) 0.05000 1.00 Uiso H12B 0.437(3) 0.775(4) 0.027(3) 0.05000 1.00 Uiso H17A 0.589(3) -0.135(5) 0.232(3) 0.05000 1.00 Uiso H16C -0.083(3) -0.117(5) -0.166(3) 0.05000 1.00 Uiso H17B 0.579(4) -0.022(5) 0.144(3) 0.05000 1.00 Uiso H17C 0.645(3) 0.012(4) 0.262(3) 0.05000 1.00 Uiso H12C 0.331(4) 0.793(5) -0.016(3) 0.05000 1.00 Uiso H19C 0.438(4) -0.112(5) 0.334(3) 0.05000 1.00 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe1 0.0362(2) 0.0383(2) 0.0322(2) -.0058(2) 0.0065(2) 0.0003(2) O2 0.058(1) 0.038(1) 0.037(1) -.0085(9) 0.0165(9) -.0066(9) O3 0.048(1) 0.047(1) 0.037(1) -.002(1) 0.0091(9) 0.0027(9) O4 0.038(1) 0.038(1) 0.051(1) -.0040(9) 0.0057(9) -.005(1) O5 0.055(1) 0.045(1) 0.032(1) -.013(1) 0.0178(9) -.0039(9) O6 0.045(1) 0.046(1) 0.041(1) -.009(1) 0.0141(9) -.0067(9) O7 0.038(1) 0.053(1) 0.051(1) -.002(1) 0.011(1) 0.009(1) N8 0.039(1) 0.038(1) 0.043(1) -.008(1) 0.000(1) 0.000(1) N9 0.034(1) 0.040(1) 0.033(1) -.005(1) 0.009(1) -.002(1) N10 0.042(1) 0.041(1) 0.032(1) -.008(1) 0.005(1) 0.003(1) C11 0.039(2) 0.040(2) 0.043(2) -.008(1) 0.013(1) 0.001(1) C12 0.090(3) 0.047(2) 0.074(3) -.025(2) 0.042(2) -.015(2) C13 0.040(2) 0.060(2) 0.072(3) -.009(2) 0.004(2) 0.021(2) C14 0.056(2) 0.032(2) 0.056(2) -.007(1) -.009(2) 0.001(1) C15 0.046(2) 0.050(2) 0.034(1) -.016(1) 0.002(1) 0.009(1) C16 0.071(3) 0.064(2) 0.050(2) -.032(2) 0.015(2) -.009(2) C17 0.054(2) 0.052(2) 0.095(3) 0.006(2) -.010(2) 0.005(2) C18 0.064(2) 0.061(2) 0.046(2) -.021(2) 0.022(2) 0.000(2) C19 0.108(3) 0.041(2) 0.050(2) 0.000(2) 0.000(2) 0.010(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O2 2.021(2) . . ? Fe1 O3 2.026(2) . . ? Fe1 O4 2.016(2) . . ? Fe1 O5 2.016(2) . . ? Fe1 O6 2.019(3) . . ? Fe1 O7 2.013(2) . . ? O2 N9 1.342(3) . . ? O3 N8 1.342(4) . . ? O4 N10 1.338(4) . . ? O5 N9 1.346(3) . . ? O6 N10 1.344(4) . . ? O7 N8 1.339(4) . . ? N8 C14 1.293(5) . . ? N9 C11 1.283(4) . . ? N10 C15 1.288(4) . . ? C11 C12 1.478(6) . . ? C11 C18 1.488(5) . . ? C13 C15 1.482(5) . . ? C14 C17 1.483(6) . . ? C14 C19 1.487(6) . . ? C15 C16 1.482(6) . . ? C11 H18A 1.99(5) . . ? C11 H18B 2.02(5) . . ? C11 H12A 2.08(5) . . ? C11 H18C 1.99(5) . . ? C11 H12B 2.04(5) . . ? C11 H12C 1.89(5) . . ? C14 H19A 2.02(5) . . ? C14 H19B 2.09(5) . . ? C14 H17A 2.01(5) . . ? C14 H17B 2.06(5) . . ? C14 H19C 1.94(5) . . ? C15 H13A 2.06(5) . . ? C15 H13B 1.97(4) . . ? C15 H16A 2.10(5) . . ? C15 H13C 1.99(4) . . ? C15 H16B 2.05(5) . . ? C15 H16C 2.01(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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Fe1 O3 152.5(1) . . . ? O2 Fe1 O4 107.6(1) . . . ? O2 Fe1 O5 66.0(1) . . . ? O2 Fe1 O6 99.9(1) . . . ? O2 Fe1 O7 95.8(1) . . . ? O3 Fe1 O4 95.9(1) . . . ? O3 Fe1 O5 98.6(1) . . . ? O3 Fe1 O6 102.5(1) . . . ? O3 Fe1 O7 66.0(1) . . . ? O4 Fe1 O5 95.4(1) . . . ? O4 Fe1 O6 65.9(1) . . . ? O4 Fe1 O7 152.6(1) . . . ? O5 Fe1 O6 153.0(1) . . . ? O5 Fe1 O7 107.1(1) . . . ? O6 Fe1 O7 96.8(1) . . . ? Fe1 O2 N9 92.0(2) . . . ? Fe1 O3 N8 91.5(2) . . . ? Fe1 O4 N10 92.2(2) . . . ? Fe1 O5 N9 92.1(2) . . . ? Fe1 O6 N10 91.9(2) . . . ? Fe1 O7 N8 92.1(2) . . . ? O3 N8 O7 110.3(3) . . . ? O3 N8 C14 124.5(3) . . . ? O7 N8 C14 125.2(3) . . . ? O2 N9 O5 109.8(2) . . . ? O2 N9 C11 125.3(3) . . . ? O5 N9 C11 124.9(3) . . . ? O4 N10 O6 109.9(2) . . . ? O4 N10 C15 124.6(3) . . . ? O6 N10 C15 125.5(3) . . . ? N9 C11 C12 118.8(3) . . . ? N9 C11 C18 119.4(3) . . . ? C12 C11 C18 121.8(4) . . . ? N8 C14 C17 118.4(4) . . . ? N8 C14 C19 119.3(4) . . . ? C17 C14 C19 122.4(4) . . . ? N10 C15 C13 119.6(3) . . . ? N10 C15 C16 119.0(3) . . . ? C13 C15 C16 121.4(4) . . . ? N9 C11 H18A 127.6(12) . . . ? N9 C11 H18B 95.2(13) . . . ? N9 C11 H12A 94.6(12) . . . ? N9 C11 H18C 130.6(13) . . . ? N9 C11 H12B 133.6(12) . . . ? N9 C11 H12C 132.1(14) . . . ? C12 C11 H18A 106.5(12) . . . ? C12 C11 H18B 145.8(13) . . . ? C12 C11 H12A 24.4(12) . . . ? C12 C11 H18C 105.8(13) . . . ? C12 C11 H12B 25.5(12) . . . ? C12 C11 H12C 24.3(14) . . . ? C18 C11 H18A 27.5(12) . . . ? C18 C11 H18B 24.6(13) . . . ? C18 C11 H12A 146.0(12) . . . ? C18 C11 H18C 26.9(12) . . . ? C18 C11 H12B 102.6(12) . . . ? C18 C11 H12C 105.4(14) . . . ? H18A C11 H18B 46.5(17) . . . ? H18A C11 H12A 128.9(16) . . . ? H18A C11 H18C 47.1(17) . . . ? H18A C11 H12B 82.5(17) . . . ? H18A C11 H12C 100.0(18) . . . ? H18B C11 H12A 168.7(17) . . . ? H18B C11 H18C 41.9(18) . . . ? H18B C11 H12B 126.9(17) . . . ? H18B C11 H12C 126.2(19) . . . ? H12A C11 H18C 126.8(17) . . . ? H12A C11 H12B 46.5(16) . . . ? H12A C11 H12C 42.6(18) . . . ? H18C C11 H12B 95.8(17) . . . ? H18C C11 H12C 84.3(18) . . . ? H12B C11 H12C 37.1(18) . . . ? N8 C14 H19A 128.0(12) . . . ? N8 C14 H19B 91.6(12) . . . ? N8 C14 H17A 135.0(12) . . . ? N8 C14 H17B 93.8(13) . . . ? N8 C14 H19C 131.9(13) . . . ? C17 C14 H19A 106.4(12) . . . ? C17 C14 H19B 150.0(12) . . . ? C17 C14 H17A 23.9(13) . . . ? C17 C14 H17B 24.6(13) . . . ? C17 C14 H19C 106.4(13) . . . ? C19 C14 H19A 28.9(12) . . . ? C19 C14 H19B 27.7(12) . . . ? C19 C14 H17A 103.3(13) . . . ? C19 C14 H17B 146.9(13) . . . ? C19 C14 H19C 23.3(13) . . . ? H19A C14 H19B 48.8(17) . . . ? H19A C14 H17A 96.2(17) . . . ? H19A C14 H17B 129.0(17) . . . ? H19A C14 H19C 43.4(18) . . . ? H19B C14 H17A 129.0(17) . . . ? H19B C14 H17B 173.2(17) . . . ? H19B C14 H19C 44.9(17) . . . ? H17A C14 H17B 44.5(17) . . . ? H17A C14 H19C 84.1(18) . . . ? H17B C14 H19C 128.5(18) . . . ? N10 C15 H13A 92.7(12) . . . ? N10 C15 H13B 133.9(13) . . . ? N10 C15 H16A 93.1(12) . . . ? N10 C15 H13C 125.2(12) . . . ? N10 C15 H16B 128.4(12) . . . ? N10 C15 H16C 133.7(12) . . . ? C13 C15 H13A 27.0(12) . . . ? C13 C15 H13B 25.5(13) . . . ? C13 C15 H16A 147.2(12) . . . ? C13 C15 H13C 27.8(13) . . . ? C13 C15 H16B 105.7(12) . . . ? C13 C15 H16C 102.9(12) . . . ? C16 C15 H13A 148.1(12) . . . ? C16 C15 H13B 102.8(13) . . . ? C16 C15 H16A 26.0(12) . . . ? C16 C15 H13C 109.2(13) . . . ? C16 C15 H16B 28.8(12) . . . ? C16 C15 H16C 25.0(12) . . . ? H13A C15 H13B 46.2(17) . . . ? H13A C15 H16A 171.3(17) . . . ? H13A C15 H13C 46.2(17) . . . ? H13A C15 H16B 130.8(16) . . . ? H13A C15 H16C 126.7(17) . . . ? H13B C15 H16A 125.8(18) . . . ? H13B C15 H13C 45.4(17) . . . ? H13B C15 H16B 97.5(16) . . . ? H13B C15 H16C 80.5(17) . . . ? H16A C15 H13C 133.0(17) . . . ? H16A C15 H16B 47.9(16) . . . ? H16A C15 H16C 45.3(17) . . . ? H13C C15 H16B 85.2(17) . . . ? H13C C15 H16C 100.9(17) . . . ? H16B C15 H16C 43.5(16) . . . ? #=======END data_kt10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H34 Fe2 N4 O10' _chemical_formula_weight 554.16 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' 'Fe' 'Fe' 0.3463 0.8444 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1033(4) _cell_length_b 10.3819(4) _cell_length_c 13.8442(4) _cell_angle_alpha 111.605(2) _cell_angle_beta 95.663(2) _cell_angle_gamma 99.772(1) _cell_volume 1295.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 197(2) _cell_measurement_reflns_used 4865 _cell_measurement_theta_min 3 _cell_measurement_theta_max 26.37 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 1.15 _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 197(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'Phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4865 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4865 _reflns_number_gt 4324 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD' _computing_cell_refinement 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'maxus(Mackay et al., 1999)' _computing_publication_material 'maxus(Mackay et al., 1999)' _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^)+(0.0340P)^2^+2.5600P] 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 4865 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.909 _refine_diff_density_max 0.740 _refine_diff_density_min -0.768 _refine_diff_density_rms 0.067 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 Fe1 Fe 0.38198(4) 0.50852(4) 0.56228(3) 0.02639(12) Uani 1 1 d . . . O1 O 0.4841(2) 0.37223(19) 0.48221(15) 0.0287(4) Uani 1 1 d . . . O2 O 0.4532(2) 0.5001(2) 0.70151(16) 0.0335(5) Uani 1 1 d . . . O3 O 0.3634(2) 0.6755(2) 0.69359(16) 0.0323(4) Uani 1 1 d . . . O4 O 0.2049(2) 0.3631(2) 0.54064(17) 0.0349(5) Uani 1 1 d . . . O5 O 0.2273(2) 0.5061(2) 0.45677(18) 0.0355(5) Uani 1 1 d . . . N1 N 0.4169(2) 0.6203(2) 0.75754(19) 0.0290(5) Uani 1 1 d . . . N2 N 0.1452(2) 0.3969(3) 0.4656(2) 0.0302(5) Uani 1 1 d . . . C1 C 0.4802(3) 0.2315(3) 0.4756(3) 0.0376(7) Uani 1 1 d . . . H1A H 0.3901 0.1903 0.4807 0.068 Uiso 1 1 d R . . H1B H 0.5022 0.1758 0.4092 0.068 Uiso 1 1 d R . . C2 C 0.5779(4) 0.2268(4) 0.5622(3) 0.0513(9) Uani 1 1 d . . . H2A H 0.5719 0.1303 0.5551 0.084 Uiso 1 1 d R . . H2B H 0.5568 0.2813 0.6293 0.084 Uiso 1 1 d R . . H2C H 0.6689 0.2668 0.5577 0.084 Uiso 1 1 d R . . C3 C 0.4319(3) 0.6745(3) 0.8592(2) 0.0329(6) Uani 1 1 d . . . C4 C 0.4928(4) 0.5991(4) 0.9185(3) 0.0465(8) Uani 1 1 d . . . H4A H 0.5145 0.5154 0.8697 0.077 Uiso 1 1 d R . . H4B H 0.4290 0.5726 0.9586 0.077 Uiso 1 1 d R . . H4C H 0.5743 0.6607 0.9654 0.077 Uiso 1 1 d R . . C5 C 0.3876(4) 0.8082(4) 0.9130(3) 0.0477(9) Uani 1 1 d . . . H5A H 0.3503 0.8394 0.8610 0.074 Uiso 1 1 d R . . H5B H 0.4636 0.8799 0.9596 0.074 Uiso 1 1 d R . . H5C H 0.3183 0.7918 0.9529 0.074 Uiso 1 1 d R . . C6 C 0.0270(3) 0.3321(3) 0.4083(3) 0.0377(7) Uani 1 1 d . . . C7 C -0.0229(4) 0.3769(5) 0.3240(3) 0.0523(9) Uani 1 1 d . . . H7A H 0.0429 0.4561 0.3256 0.080 Uiso 1 1 d R . . H7B H -0.1082 0.4046 0.3356 0.080 Uiso 1 1 d R . . H7C H -0.0363 0.2997 0.2565 0.080 Uiso 1 1 d R . . C8 C -0.0519(4) 0.2115(4) 0.4261(4) 0.0590(11) Uani 1 1 d . . . H8A H -0.0648 0.2447 0.5044 0.16(3) Uiso 1 1 d R . . H8B H -0.1428 0.1847 0.3913 0.11(2) Uiso 1 1 d R . . H8C H 0.0010 0.1258 0.4163 0.17(3) Uiso 1 1 d R . . Fe2 Fe 0.94037(4) 0.87850(4) 0.03140(3) 0.02852(12) Uani 1 1 d . . . O6 O 1.0920(2) 1.0456(2) 0.07683(17) 0.0347(5) Uani 1 1 d . . . O7 O 1.0648(2) 0.7417(2) -0.01756(18) 0.0360(5) Uani 1 1 d . . . O8 O 0.8416(2) 0.6719(2) -0.05715(18) 0.0373(5) Uani 1 1 d . . . O9 O 0.9339(2) 0.8707(2) 0.17694(18) 0.0397(5) Uani 1 1 d . . . O10 O 0.7691(2) 0.9215(2) 0.09162(18) 0.0405(5) Uani 1 1 d . . . N3 N 0.9593(3) 0.6310(3) -0.0697(2) 0.0338(6) Uani 1 1 d . . . N4 N 0.8071(3) 0.8903(3) 0.1742(2) 0.0361(6) Uani 1 1 d . . . C9 C 1.2379(7) 1.0582(6) 0.1375(5) 0.098(2) Uani 1 1 d . . . H9A H 1.2383 0.9707 0.1459 0.133 Uiso 1 1 d R . . H9B H 1.3052 1.0760 0.0982 0.133 Uiso 1 1 d R . . C10 C 1.2289(10) 1.1577(10) 0.2175(8) 0.163(4) Uani 1 1 d . . . H10A H 1.3092 1.1837 0.2681 0.226 Uiso 1 1 d R . . H10B H 1.1502 1.1316 0.2472 0.226 Uiso 1 1 d R . . H10C H 1.2170 1.2369 0.1995 0.226 Uiso 1 1 d R . . C11 C 0.9709(4) 0.5037(3) -0.1243(3) 0.0409(8) Uani 1 1 d . . . C12 C 1.1101(4) 0.4755(4) -0.1319(3) 0.0538(10) Uani 1 1 d . . . H12A H 1.1757 0.5613 -0.0903 0.088 Uiso 1 1 d R . . H12B H 1.1216 0.4440 -0.2041 0.088 Uiso 1 1 d R . . H12C H 1.1200 0.4034 -0.1058 0.088 Uiso 1 1 d R . . C13 C 0.8452(5) 0.3917(4) -0.1794(4) 0.0620(11) Uani 1 1 d . . . H13A H 0.7662 0.4319 -0.1641 0.086 Uiso 1 1 d R . . H13B H 0.8419 0.3154 -0.1557 0.086 Uiso 1 1 d R . . H13C H 0.8435 0.3560 -0.2541 0.086 Uiso 1 1 d R . . C14 C 0.7287(4) 0.8787(3) 0.2409(3) 0.0451(8) Uani 1 1 d . . . C15 C 0.7801(5) 0.8407(4) 0.3286(3) 0.0600(11) Uani 1 1 d . . . H15A H 0.8706 0.8284 0.3240 0.091 Uiso 1 1 d R . . H15B H 0.7220 0.7539 0.3238 0.091 Uiso 1 1 d R . . H15C H 0.7784 0.9155 0.3949 0.091 Uiso 1 1 d R . . C16 C 0.5897(5) 0.9047(5) 0.2274(4) 0.0662(12) Uani 1 1 d . . . H16A H 0.5745 0.9275 0.1664 0.101 Uiso 1 1 d R . . H16B H 0.5785 0.9826 0.2887 0.101 Uiso 1 1 d R . . H16C H 0.5222 0.8210 0.2176 0.101 Uiso 1 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 0.0259(2) 0.0290(2) 0.0244(2) 0.01083(16) 0.00524(17) 0.00489(15) O1 0.0309(10) 0.0251(10) 0.0286(11) 0.0095(8) 0.0067(9) 0.0041(8) O2 0.0414(12) 0.0347(11) 0.0258(11) 0.0086(8) 0.0081(9) 0.0183(9) O3 0.0369(11) 0.0336(11) 0.0300(11) 0.0139(9) 0.0082(9) 0.0127(9) O4 0.0316(11) 0.0398(11) 0.0383(12) 0.0234(9) 0.0050(10) 0.0030(9) O5 0.0293(10) 0.0403(12) 0.0401(12) 0.0230(10) 0.0033(10) 0.0007(9) N1 0.0289(12) 0.0295(12) 0.0285(13) 0.0102(10) 0.0069(11) 0.0081(9) N2 0.0271(12) 0.0337(13) 0.0307(13) 0.0147(10) 0.0066(11) 0.0036(10) C1 0.0469(18) 0.0236(14) 0.0416(18) 0.0119(12) 0.0115(15) 0.0056(12) C2 0.056(2) 0.0441(19) 0.062(2) 0.0307(18) 0.0084(19) 0.0107(16) C3 0.0327(15) 0.0352(15) 0.0271(15) 0.0090(12) 0.0073(13) 0.0046(12) C4 0.054(2) 0.058(2) 0.0308(18) 0.0177(15) 0.0078(16) 0.0173(17) C5 0.063(2) 0.0381(18) 0.0356(18) 0.0047(14) 0.0152(17) 0.0135(16) C6 0.0271(14) 0.0440(17) 0.0355(17) 0.0104(13) 0.0060(13) 0.0030(13) C7 0.0334(17) 0.080(3) 0.041(2) 0.0220(18) 0.0009(16) 0.0123(17) C8 0.041(2) 0.055(2) 0.069(3) 0.021(2) 0.005(2) -0.0101(17) Fe2 0.0326(2) 0.0258(2) 0.0318(2) 0.01664(17) 0.00614(18) 0.00608(16) O6 0.0347(11) 0.0345(11) 0.0347(12) 0.0200(9) -0.0057(10) -0.0010(9) O7 0.0329(11) 0.0283(10) 0.0468(13) 0.0155(9) 0.0058(10) 0.0056(8) O8 0.0342(11) 0.0300(11) 0.0472(13) 0.0163(9) 0.0032(10) 0.0056(9) O9 0.0477(13) 0.0403(12) 0.0374(13) 0.0237(10) 0.0063(11) 0.0076(10) O10 0.0501(13) 0.0465(13) 0.0403(13) 0.0274(10) 0.0177(11) 0.0211(11) N3 0.0377(14) 0.0278(12) 0.0386(15) 0.0171(11) 0.0057(12) 0.0057(10) N4 0.0512(16) 0.0277(12) 0.0340(14) 0.0162(10) 0.0124(13) 0.0087(11) C9 0.137(5) 0.062(3) 0.084(4) 0.016(3) 0.059(4) 0.002(3) C10 0.233(10) 0.184(8) 0.200(9) 0.143(8) 0.160(9) 0.156(8) C11 0.056(2) 0.0279(15) 0.0428(19) 0.0173(13) 0.0104(16) 0.0103(14) C12 0.071(3) 0.0370(18) 0.068(3) 0.0269(17) 0.029(2) 0.0263(18) C13 0.075(3) 0.0331(18) 0.062(3) 0.0090(17) 0.002(2) -0.0012(18) C14 0.067(2) 0.0339(16) 0.0388(18) 0.0168(14) 0.0231(18) 0.0089(15) C15 0.097(3) 0.048(2) 0.043(2) 0.0261(17) 0.026(2) 0.011(2) C16 0.076(3) 0.078(3) 0.064(3) 0.036(2) 0.043(2) 0.031(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.9650(19) . ? Fe1 O1 1.9749(19) 2_666 ? Fe1 O5 2.021(2) . ? Fe1 O2 2.028(2) . ? Fe1 O3 2.050(2) . ? Fe1 O4 2.053(2) . ? O1 C1 1.423(3) . ? O1 Fe1 1.9749(19) 2_666 ? O2 N1 1.339(3) . ? O3 N1 1.337(3) . ? O4 N2 1.335(3) . ? O5 N2 1.338(3) . ? N1 C3 1.290(4) . ? N2 C6 1.286(4) . ? C1 C2 1.497(5) . ? C1 H1A 0.9588 . ? C1 H1B 0.9598 . ? C2 H2A 0.9606 . ? C2 H2B 0.9599 . ? C2 H2C 0.9604 . ? C3 C5 1.482(4) . ? C3 C4 1.485(5) . ? C4 H4A 0.9598 . ? C4 H4B 0.9603 . ? C4 H4C 0.9584 . ? C5 H5A 0.9617 . ? C5 H5B 0.9563 . ? C5 H5C 0.9641 . ? C6 C8 1.481(5) . ? C6 C7 1.481(5) . ? C7 H7A 0.9574 . ? C7 H7B 0.9636 . ? C7 H7C 0.9595 . ? C8 H8A 1.0387 . ? C8 H8B 0.9382 . ? C8 H8C 1.0874 . ? Fe2 O6 1.958(2) 2_775 ? Fe2 O6 1.964(2) . ? Fe2 O7 2.030(2) . ? Fe2 O10 2.040(2) . ? Fe2 O8 2.048(2) . ? Fe2 O9 2.053(2) . ? O6 C9 1.583(8) . ? O6 Fe2 1.958(2) 2_775 ? O7 N3 1.341(3) . ? O8 N3 1.335(3) . ? O9 N4 1.331(4) . ? O10 N4 1.337(3) . ? N3 C11 1.290(4) . ? N4 C14 1.299(4) . ? C9 C10 1.228(9) . ? C9 H9A 0.9580 . ? C9 H9B 0.9470 . ? C10 H10A 0.9466 . ? C10 H10B 0.9737 . ? C10 H10C 0.9650 . ? C11 C13 1.484(5) . ? C11 C12 1.491(5) . ? C12 H12A 0.9544 . ? C12 H12B 0.9564 . ? C12 H12C 0.9583 . ? C13 H13A 0.9682 . ? C13 H13B 0.9596 . ? C13 H13C 0.9587 . ? C14 C16 1.481(6) . ? C14 C15 1.482(5) . ? C15 H15A 0.9495 . ? C15 H15B 0.9642 . ? C15 H15C 0.9636 . ? C16 H16A 0.9627 . ? C16 H16B 0.9652 . ? C16 H16C 0.9656 . ? 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 Fe1 O1 77.65(8) . 2_666 ? O1 Fe1 O5 106.41(9) . . ? O1 Fe1 O5 92.19(8) 2_666 . ? O1 Fe1 O2 93.35(8) . . ? O1 Fe1 O2 113.01(9) 2_666 . ? O5 Fe1 O2 151.01(9) . . ? O1 Fe1 O3 152.15(9) . . ? O1 Fe1 O3 93.91(8) 2_666 . ? O5 Fe1 O3 100.33(9) . . ? O2 Fe1 O3 65.28(8) . . ? O1 Fe1 O4 96.84(8) . . ? O1 Fe1 O4 154.44(9) 2_666 . ? O5 Fe1 O4 65.13(8) . . ? O2 Fe1 O4 92.08(9) . . ? O3 Fe1 O4 101.37(9) . . ? C1 O1 Fe1 128.35(18) . . ? C1 O1 Fe1 128.29(18) . 2_666 ? Fe1 O1 Fe1 102.35(8) . 2_666 ? N1 O2 Fe1 92.51(15) . . ? N1 O3 Fe1 91.57(14) . . ? N2 O4 Fe1 91.52(14) . . ? N2 O5 Fe1 92.80(15) . . ? C3 N1 O3 125.2(2) . . ? C3 N1 O2 124.3(2) . . ? O3 N1 O2 110.6(2) . . ? C6 N2 O4 125.1(3) . . ? C6 N2 O5 124.7(3) . . ? O4 N2 O5 110.3(2) . . ? O1 C1 C2 112.8(3) . . ? O1 C1 H1A 108.9 . . ? C2 C1 H1A 107.8 . . ? O1 C1 H1B 109.5 . . ? C2 C1 H1B 108.4 . . ? H1A C1 H1B 109.5 . . ? C1 C2 H2A 110.2 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.6 . . ? C1 C2 H2C 108.8 . . ? H2A C2 H2C 109.3 . . ? H2B C2 H2C 109.4 . . ? N1 C3 C5 119.6(3) . . ? N1 C3 C4 118.3(3) . . ? C5 C3 C4 122.0(3) . . ? C3 C4 H4A 109.3 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.3 . . ? H4A C4 H4C 109.6 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.2 . . ? C3 C5 H5B 110.0 . . ? H5A C5 H5B 109.6 . . ? C3 C5 H5C 109.7 . . ? H5A C5 H5C 109.0 . . ? H5B C5 H5C 109.4 . . ? N2 C6 C8 118.7(3) . . ? N2 C6 C7 118.9(3) . . ? C8 C6 C7 122.3(3) . . ? C6 C7 H7A 109.2 . . ? C6 C7 H7B 109.6 . . ? H7A C7 H7B 109.3 . . ? C6 C7 H7C 109.8 . . ? H7A C7 H7C 109.7 . . ? H7B C7 H7C 109.3 . . ? C6 C8 H8A 109.6 . . ? C6 C8 H8B 111.8 . . ? H8A C8 H8B 101.0 . . ? C6 C8 H8C 113.5 . . ? H8A C8 H8C 103.4 . . ? H8B C8 H8C 116.2 . . ? O6 Fe2 O6 77.43(10) 2_775 . ? O6 Fe2 O7 107.33(9) 2_775 . ? O6 Fe2 O7 92.58(9) . . ? O6 Fe2 O10 94.31(9) 2_775 . ? O6 Fe2 O10 113.74(10) . . ? O7 Fe2 O10 149.22(9) . . ? O6 Fe2 O8 97.55(9) 2_775 . ? O6 Fe2 O8 154.90(9) . . ? O7 Fe2 O8 65.13(8) . . ? O10 Fe2 O8 91.02(9) . . ? O6 Fe2 O9 154.62(9) 2_775 . ? O6 Fe2 O9 97.15(9) . . ? O7 Fe2 O9 97.60(9) . . ? O10 Fe2 O9 64.85(9) . . ? O8 Fe2 O9 97.15(9) . . ? C9 O6 Fe2 124.5(2) . 2_775 ? C9 O6 Fe2 124.5(2) . . ? Fe2 O6 Fe2 102.58(10) 2_775 . ? N3 O7 Fe2 92.62(15) . . ? N3 O8 Fe2 92.03(15) . . ? N4 O9 Fe2 91.61(16) . . ? N4 O10 Fe2 92.01(16) . . ? C11 N3 O8 125.3(3) . . ? C11 N3 O7 124.5(3) . . ? O8 N3 O7 110.2(2) . . ? C14 N4 O9 125.3(3) . . ? C14 N4 O10 124.0(3) . . ? O9 N4 O10 110.7(2) . . ? C10 C9 O6 94.4(7) . . ? C10 C9 H9A 115.0 . . ? O6 C9 H9A 108.1 . . ? C10 C9 H9B 117.5 . . ? O6 C9 H9B 109.5 . . ? H9A C9 H9B 110.7 . . ? C9 C10 H10A 109.3 . . ? C9 C10 H10B 110.9 . . ? H10A C10 H10B 109.3 . . ? C9 C10 H10C 109.1 . . ? H10A C10 H10C 110.3 . . ? H10B C10 H10C 107.9 . . ? N3 C11 C13 118.8(3) . . ? N3 C11 C12 118.8(3) . . ? C13 C11 C12 122.4(3) . . ? C11 C12 H12A 108.6 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 110.2 . . ? C11 C12 H12C 109.0 . . ? H12A C12 H12C 110.0 . . ? H12B C12 H12C 109.8 . . ? C11 C13 H13A 109.2 . . ? C11 C13 H13B 110.2 . . ? H13A C13 H13B 108.9 . . ? C11 C13 H13C 109.8 . . ? H13A C13 H13C 109.0 . . ? H13B C13 H13C 109.6 . . ? N4 C14 C16 118.8(3) . . ? N4 C14 C15 119.6(4) . . ? C16 C14 C15 121.6(3) . . ? C14 C15 H15A 109.2 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.9 . . ? C14 C15 H15C 109.2 . . ? H15A C15 H15C 110.2 . . ? H15B C15 H15C 108.8 . . ? C14 C16 H16A 109.7 . . ? C14 C16 H16B 110.6 . . ? H16A C16 H16B 108.9 . . ? C14 C16 H16C 110.2 . . ? H16A C16 H16C 108.8 . . ? H16B C16 H16C 108.5 . . ? _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (1999). maXus Computer Program for the Solution and Refinement of Crystal Structures. Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Otwinowski, Z. and Minor, W, (1997). In Methods in Enzymology, 276, edited by C.W. Carter, Jr. & R.M. Sweet pp. 307-326, New York:Academic Press. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. ; #=======END