Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Paul-L Fabre' 'Bruno Donnadieu' 'Anne-M Galibert' 'Brigitte Soula' _publ_contact_author_name 'Prof Paul-L Fabre' _publ_contact_author_address ; Laboratoire de Chimie Inorganique Universite Paul Sabatier 118 route de Narbonne Toulouse Cedex 04 31062 FRANCE ; _publ_contact_author_email FABRE@CHIMIE.UPS-TLSE.FR _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Diversity of the co-ordination modes of croconate violet. Crystal structures, spectroscopic characterizations and redox studies of mono-, di- and polynuclear iron(II) complexes ; #============================================================================== _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. and Camalli, M. (1994)., SIR92 program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. 27, 435. DIFABS - N. Walker and D. Stuart, Acta Crystallogr., Sect A 1983, 39, 158-166. Farrugia, L. J., ORTEP3 for Windows, J. Appl. Crystallogr. 1997, 30, 565. Sheldrick, G. M. (1997). SHELXL97. Program for the refinement of Crystal Structures. University of Göttingen, Germany. Stoe, IPDS Manual. Version 2.75. Stoe & Cie, Darmstadt,1996, Germany. Stoe, X-RED, Data Reduction for STADI4 and IPDS, Revision 1.08. Stoe & Cie, Darmstadt, 1996, Germany. WINGX L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838 ; #**************************************************************************** data_(1) _database_code_CSD 203378 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H8 Fe K2 N8 O10' _chemical_formula_weight 678.41 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 9.3903(9) _cell_length_b 6.9968(5) _cell_length_c 19.461(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.818(12) _cell_angle_gamma 90.00 _cell_volume 1277.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 26.05 _exptl_crystal_description plate _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.764 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.991 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.33 _exptl_absorpt_correction_T_max 0.76 _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS). The crystal-to-detector distance was 70 mm. 154 frames (5 min per frame) were obtained with 0 < \f < 200.2\% and with the crystals rotated through 1.3\% in \f. Coverage of the unique set was over 98.4% complete to at least 26.09\%. Crystal decay was monitored by measuring 200 reflexions per frame. ; _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 'Stoe IPDS' _diffrn_measurement_method \f _diffrn_standards_number 200 _diffrn_standards_interval_time 'every frame' _diffrn_standards_decay_% <0.1 _diffrn_reflns_number 9671 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 26.09 _reflns_number_total 2509 _reflns_number_gt 2193 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software (Stoe, 1996)' _computing_data_reduction 'XRED (Stoe, 1.08, 1996)' _computing_cell_refinement 'Stoe IPDS software (Stoe, 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _computing_corr_abs DIFABS _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^)+(0.0550P)^2^+0.3080P] 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 SHELXL _refine_ls_extinction_coef 0.0005(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2509 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 0.7500 0.32276(6) 0.2500 0.01936(15) Uani 1 2 d S . . K1 K 0.92409(4) 0.26946(7) 0.44530(2) 0.02454(15) Uani 1 1 d . . . O1 O 0.17289(13) 0.3641(2) 0.51517(7) 0.0244(3) Uani 1 1 d . . . O2 O 0.31149(15) 0.1967(2) 0.63794(7) 0.0254(3) Uani 1 1 d . . . O3 O 0.64956(14) 0.2272(2) 0.46739(7) 0.0243(3) Uani 1 1 d . . . N1 N 0.57283(17) 0.3335(3) 0.31182(9) 0.0255(4) Uani 1 1 d . . . O1W O 0.65313(16) 0.1021(2) 0.18628(7) 0.0260(3) Uani 1 1 d . . . O2W O 0.85021(17) 0.5221(2) 0.31552(8) 0.0324(4) Uani 1 1 d . . . N2 N 0.13801(18) 0.4704(3) 0.34547(10) 0.0380(5) Uani 1 1 d . . . N3 N 0.57242(19) 0.0736(3) 0.74270(9) 0.0377(5) Uani 1 1 d . . . N4 N 0.87583(18) 0.0454(3) 0.57933(9) 0.0300(4) Uani 1 1 d . . . C1 C 0.48758(19) 0.3443(3) 0.35173(9) 0.0206(4) Uani 1 1 d . . . C2 C 0.37859(18) 0.3573(3) 0.39888(9) 0.0186(4) Uani 1 1 d . . . C3 C 0.24399(19) 0.4199(3) 0.37064(10) 0.0238(4) Uani 1 1 d . . . C4 C 0.40141(18) 0.3058(2) 0.46726(9) 0.0175(4) Uani 1 1 d . . . C5 C 0.29814(19) 0.3083(3) 0.51981(10) 0.0188(4) Uani 1 1 d . . . C6 C 0.37002(19) 0.2279(3) 0.58275(10) 0.0189(4) Uani 1 1 d . . . C7 C 0.51797(19) 0.1933(3) 0.56941(10) 0.0182(4) Uani 1 1 d . . . C8 C 0.62315(18) 0.1302(3) 0.61569(9) 0.0196(4) Uani 1 1 d . . . C9 C 0.59524(19) 0.0995(3) 0.68618(10) 0.0252(4) Uani 1 1 d . . . C10 C 0.76390(19) 0.0866(3) 0.59525(9) 0.0217(4) Uani 1 1 d . . . C11 C 0.53684(18) 0.2402(3) 0.49748(9) 0.0181(4) Uani 1 1 d . . . H11 H 0.704(4) 0.013(5) 0.1710(16) 0.060(9) Uiso 1 1 d . . . H12 H 0.586(4) 0.047(5) 0.2002(16) 0.053(9) Uiso 1 1 d . . . H21 H 0.931(3) 0.534(4) 0.3184(14) 0.043(8) Uiso 1 1 d . . . H22 H 0.809(4) 0.612(6) 0.3376(17) 0.064(10) 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 Fe1 0.0134(2) 0.0290(2) 0.0161(2) 0.000 0.00477(13) 0.000 K1 0.0139(2) 0.0333(3) 0.0268(3) -0.00292(17) 0.00408(16) 0.00135(15) O1 0.0116(6) 0.0347(8) 0.0274(7) -0.0039(6) 0.0047(5) 0.0026(5) O2 0.0224(7) 0.0308(8) 0.0240(7) 0.0022(6) 0.0122(6) 0.0019(6) O3 0.0127(6) 0.0356(8) 0.0251(7) 0.0022(6) 0.0068(5) 0.0036(5) N1 0.0163(8) 0.0395(10) 0.0213(8) 0.0023(7) 0.0060(6) 0.0007(7) O1W 0.0213(7) 0.0314(8) 0.0259(7) -0.0035(6) 0.0080(6) -0.0029(6) O2W 0.0147(7) 0.0407(9) 0.0420(9) -0.0180(7) 0.0029(6) 0.0025(6) N2 0.0206(9) 0.0525(12) 0.0406(11) 0.0042(9) -0.0006(7) 0.0050(8) N3 0.0288(9) 0.0596(13) 0.0249(9) 0.0056(9) 0.0048(7) -0.0058(9) N4 0.0212(8) 0.0395(10) 0.0296(9) 0.0015(8) 0.0041(6) 0.0072(7) C1 0.0162(9) 0.0255(10) 0.0203(9) 0.0008(7) 0.0018(7) 0.0000(7) C2 0.0117(8) 0.0233(9) 0.0211(9) -0.0007(7) 0.0047(6) -0.0014(7) C3 0.0187(9) 0.0302(10) 0.0230(9) 0.0003(8) 0.0052(7) 0.0011(8) C4 0.0123(8) 0.0180(9) 0.0227(9) -0.0031(7) 0.0057(7) -0.0005(6) C5 0.0137(8) 0.0202(9) 0.0229(9) -0.0044(7) 0.0041(7) -0.0025(7) C6 0.0157(9) 0.0192(9) 0.0222(9) -0.0031(7) 0.0056(7) 0.0001(7) C7 0.0149(8) 0.0181(8) 0.0220(9) -0.0025(7) 0.0059(7) -0.0011(6) C8 0.0163(8) 0.0223(9) 0.0207(9) -0.0001(7) 0.0055(7) -0.0011(7) C9 0.0182(8) 0.0309(10) 0.0264(10) 0.0028(8) 0.0019(7) -0.0014(8) C10 0.0206(9) 0.0239(10) 0.0205(9) 0.0023(7) 0.0003(7) -0.0001(7) C11 0.0135(8) 0.0194(9) 0.0216(9) -0.0017(7) 0.0038(7) -0.0008(7) _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 O2W 2.0828(16) 2_655 ? Fe1 O2W 2.0828(16) . ? Fe1 N1 2.1018(16) . ? Fe1 N1 2.1018(16) 2_655 ? Fe1 O1W 2.1537(15) . ? Fe1 O1W 2.1537(15) 2_655 ? K1 O3 2.6508(14) . ? K1 O1 2.7264(14) 1_655 ? K1 O1 2.8398(15) 3_666 ? K1 O1W 2.8761(16) 2_655 ? K1 N4 2.9497(18) 3_756 ? K1 N4 3.0959(18) . ? K1 O2W 3.1323(18) . ? K1 N2 3.189(2) 1_655 ? K1 K1 4.0835(9) 3_766 ? K1 K1 4.5262(9) 3_756 ? K1 H21 3.09(3) . ? O1 C5 1.238(2) . ? O1 K1 2.7264(14) 1_455 ? O1 K1 2.8398(15) 3_666 ? O2 C6 1.250(2) . ? O3 C11 1.238(2) . ? N1 C1 1.145(2) . ? O1W K1 2.8761(16) 2_655 ? O1W H11 0.85(4) . ? O1W H12 0.80(3) . ? O2W H21 0.76(3) . ? O2W H22 0.86(4) . ? N2 C3 1.143(3) . ? N2 K1 3.189(2) 1_455 ? N3 C9 1.145(3) . ? N4 C10 1.147(3) . ? N4 K1 2.9497(18) 3_756 ? C1 C2 1.411(2) . ? C2 C4 1.385(3) . ? C2 C3 1.422(3) . ? C4 C5 1.444(2) . ? C4 C11 1.449(2) . ? C5 C6 1.480(3) . ? C6 C7 1.446(2) . ? C7 C8 1.376(3) . ? C7 C11 1.457(3) . ? C8 C9 1.426(3) . ? C8 C10 1.432(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2W Fe1 O2W 95.94(10) 2_655 . ? O2W Fe1 N1 88.86(6) 2_655 . ? O2W Fe1 N1 88.41(7) . . ? O2W Fe1 N1 88.41(7) 2_655 2_655 ? O2W Fe1 N1 88.86(6) . 2_655 ? N1 Fe1 N1 175.92(10) . 2_655 ? O2W Fe1 O1W 87.83(7) 2_655 . ? O2W Fe1 O1W 176.23(6) . . ? N1 Fe1 O1W 91.79(6) . . ? N1 Fe1 O1W 91.13(6) 2_655 . ? O2W Fe1 O1W 176.23(6) 2_655 2_655 ? O2W Fe1 O1W 87.83(7) . 2_655 ? N1 Fe1 O1W 91.13(6) . 2_655 ? N1 Fe1 O1W 91.79(6) 2_655 2_655 ? O1W Fe1 O1W 88.39(8) . 2_655 ? O3 K1 O1 139.69(4) . 1_655 ? O3 K1 O1 74.30(4) . 3_666 ? O1 K1 O1 85.64(4) 1_655 3_666 ? O3 K1 O1W 83.94(4) . 2_655 ? O1 K1 O1W 135.66(4) 1_655 2_655 ? O1 K1 O1W 122.60(4) 3_666 2_655 ? O3 K1 N4 125.13(5) . 3_756 ? O1 K1 N4 74.06(5) 1_655 3_756 ? O1 K1 N4 159.00(5) 3_666 3_756 ? O1W K1 N4 71.69(5) 2_655 3_756 ? O3 K1 N4 67.86(4) . . ? O1 K1 N4 81.96(5) 1_655 . ? O1 K1 N4 99.60(5) 3_666 . ? O1W K1 N4 120.20(5) 2_655 . ? N4 K1 N4 83.08(5) 3_756 . ? O3 K1 O2W 90.86(4) . . ? O1 K1 O2W 114.55(5) 1_655 . ? O1 K1 O2W 69.38(4) 3_666 . ? O1W K1 O2W 58.38(4) 2_655 . ? N4 K1 O2W 114.08(5) 3_756 . ? N4 K1 O2W 158.34(4) . . ? O3 K1 N2 142.62(5) . 1_655 ? O1 K1 N2 69.31(5) 1_655 1_655 ? O1 K1 N2 89.26(5) 3_666 1_655 ? O1W K1 N2 77.05(5) 2_655 1_655 ? N4 K1 N2 78.75(5) 3_756 1_655 ? N4 K1 N2 149.23(5) . 1_655 ? O2W K1 N2 51.77(4) . 1_655 ? O3 K1 K1 108.72(4) . 3_766 ? O1 K1 K1 43.90(3) 1_655 3_766 ? O1 K1 K1 41.74(3) 3_666 3_766 ? O1W K1 K1 148.45(4) 2_655 3_766 ? N4 K1 K1 117.77(4) 3_756 3_766 ? N4 K1 K1 91.29(4) . 3_766 ? O2W K1 K1 91.86(3) . 3_766 ? N2 K1 K1 75.83(4) 1_655 3_766 ? O3 K1 K1 96.73(4) . 3_756 ? O1 K1 K1 74.06(3) 1_655 3_756 ? O1 K1 K1 136.26(3) 3_666 3_756 ? O1W K1 K1 98.01(4) 2_655 3_756 ? N4 K1 K1 42.77(4) 3_756 3_756 ? N4 K1 K1 40.31(3) . 3_756 ? O2W K1 K1 154.36(3) . 3_756 ? N2 K1 K1 117.42(4) 1_655 3_756 ? K1 K1 K1 108.61(2) 3_766 3_756 ? O3 K1 H21 104.8(6) . . ? O1 K1 H21 101.6(6) 1_655 . ? O1 K1 H21 72.3(6) 3_666 . ? O1W K1 H21 63.0(5) 2_655 . ? N4 K1 H21 106.2(6) 3_756 . ? N4 K1 H21 170.7(6) . . ? O2W K1 H21 14.1(6) . . ? N2 K1 H21 37.8(6) 1_655 . ? K1 K1 H21 85.6(6) 3_766 . ? K1 K1 H21 148.9(6) 3_756 . ? C5 O1 K1 138.36(12) . 1_455 ? C5 O1 K1 125.52(12) . 3_666 ? K1 O1 K1 94.36(4) 1_455 3_666 ? C11 O3 K1 158.35(13) . . ? C1 N1 Fe1 171.94(16) . . ? Fe1 O1W K1 107.55(6) . 2_655 ? Fe1 O1W H11 120(2) . . ? K1 O1W H11 96(2) 2_655 . ? Fe1 O1W H12 118(2) . . ? K1 O1W H12 109(2) 2_655 . ? H11 O1W H12 104(3) . . ? Fe1 O2W K1 101.03(6) . . ? Fe1 O2W H21 122(2) . . ? K1 O2W H21 80(2) . . ? Fe1 O2W H22 126(2) . . ? K1 O2W H22 95(2) . . ? H21 O2W H22 111(3) . . ? C3 N2 K1 99.43(15) . 1_455 ? C10 N4 K1 146.22(16) . 3_756 ? C10 N4 K1 105.90(14) . . ? K1 N4 K1 96.92(5) 3_756 . ? N1 C1 C2 177.9(2) . . ? C4 C2 C1 121.68(16) . . ? C4 C2 C3 122.95(16) . . ? C1 C2 C3 115.32(16) . . ? N2 C3 C2 177.3(2) . . ? C2 C4 C5 126.86(16) . . ? C2 C4 C11 124.30(15) . . ? C5 C4 C11 108.84(16) . . ? O1 C5 C4 128.38(18) . . ? O1 C5 C6 124.96(17) . . ? C4 C5 C6 106.66(15) . . ? O2 C6 C7 126.31(18) . . ? O2 C6 C5 125.15(17) . . ? C7 C6 C5 108.54(15) . . ? C8 C7 C6 126.94(17) . . ? C8 C7 C11 125.71(16) . . ? C6 C7 C11 107.34(16) . . ? C7 C8 C9 121.21(16) . . ? C7 C8 C10 121.95(16) . . ? C9 C8 C10 116.82(16) . . ? N3 C9 C8 179.5(2) . . ? N4 C10 C8 177.7(2) . . ? O3 C11 C4 125.80(17) . . ? O3 C11 C7 125.81(17) . . ? C4 C11 C7 108.39(14) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.09 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.336 _refine_diff_density_min -0.811 _refine_diff_density_rms 0.070 #====END data_(2) _database_code_CSD 203379 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H14 Fe N6 O6' _chemical_formula_weight 502.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 10.540(7) _cell_length_b 10.754(8) _cell_length_c 10.977(9) _cell_angle_alpha 84.22(9) _cell_angle_beta 63.69(8) _cell_angle_gamma 67.82(8) _cell_volume 1029.4(13) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 26.0 _exptl_crystal_description plate _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 0.787 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.38 _exptl_absorpt_correction_T_max 0.86 _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS). The crystal-to-detector distance was 70 mm. 250 frames (5 min per frame) were obtained with 0 < \f < 250.\% and with the crystals rotated through 1.0\% in \f. Coverage of the unique set was over 94.7% complete to at least 23.25\%. Crystal decay was monitored by measuring 200 reflexions per frame. ; _diffrn_ambient_temperature 160(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 'Stoe IPDS' _diffrn_measurement_method \f _diffrn_standards_number 200 _diffrn_standards_interval_time 'every frame' _diffrn_standards_decay_% <0.1 _diffrn_reflns_number 7381 _diffrn_reflns_av_R_equivalents 0.1007 _diffrn_reflns_av_sigmaI/netI 0.0767 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 23.25 _reflns_number_total 2793 _reflns_number_gt 2389 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software (Stoe, 1996)' _computing_data_reduction 'XRED (Stoe, 1.08, 1996)' _computing_cell_refinement 'Stoe IPDS software (Stoe, 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _computing_corr_abs DIFABS _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^)+(0.1454P)^2^+0.1559P] 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 2793 _refine_ls_number_parameters 337 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0681 _refine_ls_wR_factor_ref 0.1878 _refine_ls_wR_factor_gt 0.1784 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.005 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.91800(7) 0.29938(5) 0.82861(6) 0.0320(3) Uani 1 1 d . . . O1W O 0.7399(4) 0.4084(3) 1.0121(3) 0.0346(8) Uani 1 1 d D . . H1W H 0.707(6) 0.482(3) 1.018(5) 0.043(11) Uiso 1 1 d D . . H2W H 0.682(6) 0.379(5) 1.043(5) 0.043(11) Uiso 1 1 d D . . O2W O 1.1085(4) 0.1938(3) 0.6374(4) 0.0400(8) Uani 1 1 d D . . H3W H 1.182(5) 0.184(5) 0.642(6) 0.047(11) Uiso 1 1 d D . . H4W H 1.131(7) 0.133(4) 0.591(5) 0.047(11) Uiso 1 1 d D . . O1 O 0.6500(4) 0.0531(3) 0.7590(3) 0.0372(8) Uani 1 1 d . . . O2 O 0.4868(4) -0.3114(3) 0.9149(3) 0.0398(8) Uani 1 1 d . . . O3 O 0.7013(4) -0.3247(3) 1.0176(3) 0.0369(8) Uani 1 1 d . . . N1 N 0.7845(4) 0.4011(3) 0.7214(4) 0.0341(9) Uani 1 1 d . . . N2 N 0.9850(5) 0.4674(3) 0.7601(4) 0.0338(9) Uani 1 1 d . . . N3 N 0.8573(5) 0.1291(4) 0.8657(4) 0.0370(9) Uani 1 1 d . . . N4 N 0.9360(5) -0.2149(3) 1.0764(4) 0.0353(9) Uani 1 1 d . . . N5 N 0.4201(5) 0.1466(4) 0.6113(4) 0.0454(10) Uani 1 1 d . . . N6 N 0.2671(6) -0.1697(5) 0.7369(6) 0.0615(14) Uani 1 1 d . . . C1 C 0.6794(6) 0.3679(5) 0.7130(5) 0.0405(11) Uani 1 1 d . . . H1 H 0.6643 0.2890 0.7527 0.049 Uiso 1 1 calc R . . C2 C 0.5908(6) 0.4428(5) 0.6491(5) 0.0459(12) Uani 1 1 d . . . H2 H 0.5146 0.4175 0.6470 0.055 Uiso 1 1 calc R . . C3 C 0.6162(6) 0.5557(5) 0.5884(5) 0.0488(13) Uani 1 1 d . . . H3 H 0.5584 0.6084 0.5423 0.059 Uiso 1 1 calc R . . C4 C 0.7256(6) 0.5913(4) 0.5949(4) 0.0394(11) Uani 1 1 d . . . H4 H 0.7445 0.6682 0.5529 0.047 Uiso 1 1 calc R . . C5 C 0.8084(6) 0.5132(4) 0.6637(4) 0.0344(10) Uani 1 1 d . . . C6 C 0.9210(5) 0.5497(4) 0.6840(4) 0.0341(10) Uani 1 1 d . . . C7 C 0.9573(6) 0.6613(4) 0.6331(4) 0.0381(11) Uani 1 1 d . . . H7 H 0.9139 0.7170 0.5778 0.046 Uiso 1 1 calc R . . C8 C 1.0577(6) 0.6910(4) 0.6637(5) 0.0403(11) Uani 1 1 d . . . H8 H 1.0812 0.7687 0.6317 0.048 Uiso 1 1 calc R . . C9 C 1.1231(6) 0.6073(4) 0.7407(5) 0.0407(11) Uani 1 1 d . . . H9 H 1.1932 0.6249 0.7619 0.049 Uiso 1 1 calc R . . C10 C 1.0831(6) 0.4965(4) 0.7860(5) 0.0374(11) Uani 1 1 d . . . H10 H 1.1284 0.4379 0.8386 0.045 Uiso 1 1 calc R . . C11 C 0.8303(5) 0.0339(4) 0.8912(4) 0.0314(10) Uani 1 1 d . . . C12 C 0.7983(5) -0.0848(4) 0.9343(4) 0.0296(10) Uani 1 1 d . . . C13 C 0.8729(5) -0.1609(4) 1.0128(4) 0.0315(10) Uani 1 1 d . . . C14 C 0.7009(5) -0.1201(4) 0.9054(4) 0.0304(10) Uani 1 1 d . . . C15 C 0.6300(5) -0.0469(4) 0.8197(4) 0.0328(10) Uani 1 1 d . . . C16 C 0.5331(5) -0.1116(4) 0.8151(4) 0.0308(10) Uani 1 1 d . . . C17 C 0.5490(5) -0.2297(4) 0.8958(4) 0.0317(10) Uani 1 1 d . . . C18 C 0.6576(5) -0.2348(4) 0.9491(4) 0.0311(10) Uani 1 1 d . . . C19 C 0.4472(5) -0.0666(4) 0.7444(5) 0.0337(10) Uani 1 1 d . . . C20 C 0.4388(6) 0.0527(5) 0.6715(5) 0.0377(11) Uani 1 1 d . . . C21 C 0.3484(6) -0.1283(4) 0.7440(5) 0.0426(12) Uani 1 1 d . . . O1S1 O 1.0969(11) 0.9947(8) 0.5043(9) 0.048(2) Uani 0.50 1 d P . . O1S2 O 1.1757(13) 0.9602(8) 0.5150(8) 0.0399(17) Uani 0.50 1 d P . . H1S H 1.197(10) 0.963(7) 0.436(8) 0.074(16) Uiso 1 1 d . . . H1S2 H 1.212(17) 0.892(14) 0.546(14) 0.074(16) Uiso 0.50 1 d P . . H1S1 H 1.0000 1.0000 0.5000 0.074(16) Uiso 1 2 d S . . 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 0.0335(5) 0.0268(4) 0.0434(5) 0.0090(3) -0.0221(4) -0.0145(3) O1W 0.035(2) 0.0261(15) 0.0460(19) 0.0048(13) -0.0177(16) -0.0152(13) O2W 0.037(2) 0.0378(17) 0.0447(18) 0.0036(13) -0.0206(16) -0.0098(15) O1 0.043(2) 0.0305(15) 0.0491(17) 0.0119(13) -0.0264(16) -0.0190(13) O2 0.037(2) 0.0364(16) 0.0529(19) 0.0062(13) -0.0214(16) -0.0191(14) O3 0.041(2) 0.0282(14) 0.0505(18) 0.0102(13) -0.0267(16) -0.0161(13) N1 0.034(2) 0.0269(17) 0.040(2) 0.0034(14) -0.0178(18) -0.0096(15) N2 0.037(2) 0.0279(17) 0.0372(19) 0.0034(14) -0.0178(17) -0.0106(16) N3 0.041(3) 0.031(2) 0.051(2) 0.0100(16) -0.028(2) -0.0177(17) N4 0.036(2) 0.0305(17) 0.049(2) 0.0082(16) -0.025(2) -0.0160(16) N5 0.045(3) 0.041(2) 0.060(2) 0.0126(19) -0.031(2) -0.0173(18) N6 0.071(4) 0.056(3) 0.100(4) 0.025(2) -0.066(3) -0.037(2) C1 0.039(3) 0.039(2) 0.051(3) 0.0051(19) -0.024(2) -0.018(2) C2 0.039(3) 0.051(3) 0.053(3) 0.003(2) -0.027(3) -0.015(2) C3 0.048(3) 0.048(3) 0.050(3) 0.003(2) -0.030(3) -0.007(2) C4 0.043(3) 0.030(2) 0.039(2) 0.0020(17) -0.021(2) -0.0048(19) C5 0.032(3) 0.030(2) 0.035(2) 0.0000(17) -0.012(2) -0.0086(18) C6 0.035(3) 0.0242(19) 0.038(2) 0.0000(16) -0.013(2) -0.0084(18) C7 0.039(3) 0.029(2) 0.038(2) 0.0039(17) -0.012(2) -0.0107(19) C8 0.044(3) 0.028(2) 0.044(2) 0.0008(18) -0.011(2) -0.017(2) C9 0.040(3) 0.035(2) 0.047(3) 0.0017(19) -0.015(2) -0.018(2) C10 0.039(3) 0.031(2) 0.046(2) 0.0024(18) -0.020(2) -0.0144(19) C11 0.031(3) 0.028(2) 0.041(2) 0.0040(17) -0.023(2) -0.0089(18) C12 0.031(3) 0.0220(19) 0.037(2) 0.0035(16) -0.019(2) -0.0072(17) C13 0.028(3) 0.0265(19) 0.042(2) 0.0015(18) -0.015(2) -0.0117(17) C14 0.030(3) 0.0237(19) 0.038(2) -0.0005(16) -0.016(2) -0.0074(17) C15 0.033(3) 0.027(2) 0.035(2) -0.0014(17) -0.015(2) -0.0069(18) C16 0.026(2) 0.029(2) 0.035(2) -0.0022(16) -0.0107(19) -0.0103(17) C17 0.025(3) 0.028(2) 0.041(2) -0.0016(17) -0.012(2) -0.0099(18) C18 0.026(3) 0.028(2) 0.035(2) -0.0008(17) -0.0098(19) -0.0081(17) C19 0.033(3) 0.029(2) 0.045(2) 0.0030(17) -0.022(2) -0.0131(18) C20 0.029(3) 0.039(3) 0.047(3) -0.001(2) -0.019(2) -0.012(2) C21 0.049(3) 0.033(2) 0.059(3) 0.010(2) -0.036(3) -0.015(2) O1S1 0.033(5) 0.054(5) 0.059(5) -0.001(4) -0.020(5) -0.017(4) O1S2 0.045(6) 0.039(4) 0.043(4) 0.009(3) -0.023(4) -0.020(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 O1W 2.102(5) . ? Fe1 N3 2.105(4) . ? Fe1 N4 2.111(4) 2_757 ? Fe1 N2 2.133(4) . ? Fe1 N1 2.146(4) . ? Fe1 O2W 2.179(5) . ? O1W H1W 0.73(3) . ? O1W H2W 0.73(3) . ? O2W H3W 0.77(3) . ? O2W H4W 0.77(3) . ? O1 C15 1.244(5) . ? O2 C17 1.233(6) . ? O3 C18 1.240(5) . ? N1 C1 1.327(7) . ? N1 C5 1.361(6) . ? N2 C10 1.331(6) . ? N2 C6 1.355(6) . ? N3 C11 1.140(6) . ? N4 C13 1.142(6) . ? N4 Fe1 2.111(4) 2_757 ? N5 C20 1.151(6) . ? N6 C21 1.137(7) . ? C1 C2 1.383(7) . ? C1 H1 0.9500 . ? C2 C3 1.383(8) . ? C2 H2 0.9500 . ? C3 C4 1.376(8) . ? C3 H3 0.9500 . ? C4 C5 1.393(7) . ? C4 H4 0.9500 . ? C5 C6 1.489(7) . ? C6 C7 1.386(7) . ? C7 C8 1.387(8) . ? C7 H7 0.9500 . ? C8 C9 1.376(7) . ? C8 H8 0.9500 . ? C9 C10 1.385(7) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.425(7) . ? C12 C14 1.381(7) . ? C12 C13 1.415(6) . ? C14 C18 1.440(6) . ? C14 C15 1.446(6) . ? C15 C16 1.456(7) . ? C16 C19 1.369(7) . ? C16 C17 1.473(6) . ? C17 C18 1.481(6) . ? C19 C21 1.432(7) . ? C19 C20 1.437(7) . ? O1S1 O1S2 0.829(9) . ? O1S1 H1S 0.94(8) . ? O1S1 H1S1 1.023(11) . ? O1S2 H1S 0.80(8) . ? O1S2 H1S2 0.81(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Fe1 N3 94.47(17) . . ? O1W Fe1 N4 91.08(16) . 2_757 ? N3 Fe1 N4 89.86(16) . 2_757 ? O1W Fe1 N2 92.00(16) . . ? N3 Fe1 N2 171.30(14) . . ? N4 Fe1 N2 95.83(16) 2_757 . ? O1W Fe1 N1 90.49(16) . . ? N3 Fe1 N1 96.78(16) . . ? N4 Fe1 N1 173.03(15) 2_757 . ? N2 Fe1 N1 77.33(16) . . ? O1W Fe1 O2W 176.97(12) . . ? N3 Fe1 O2W 88.44(17) . . ? N4 Fe1 O2W 88.07(16) 2_757 . ? N2 Fe1 O2W 85.19(16) . . ? N1 Fe1 O2W 90.01(16) . . ? Fe1 O1W H1W 121(4) . . ? Fe1 O1W H2W 112(4) . . ? H1W O1W H2W 112(6) . . ? Fe1 O2W H3W 107(4) . . ? Fe1 O2W H4W 137(5) . . ? H3W O2W H4W 104(6) . . ? C1 N1 C5 119.0(4) . . ? C1 N1 Fe1 126.1(3) . . ? C5 N1 Fe1 114.8(3) . . ? C10 N2 C6 118.5(4) . . ? C10 N2 Fe1 125.4(3) . . ? C6 N2 Fe1 116.1(3) . . ? C11 N3 Fe1 175.1(3) . . ? C13 N4 Fe1 169.5(4) . 2_757 ? N1 C1 C2 123.1(5) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 118.1(5) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? C4 C3 C2 119.7(4) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 119.2(4) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 120.7(5) . . ? N1 C5 C6 116.4(4) . . ? C4 C5 C6 122.8(4) . . ? N2 C6 C7 121.0(5) . . ? N2 C6 C5 115.3(4) . . ? C7 C6 C5 123.7(4) . . ? C6 C7 C8 119.4(4) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C9 C8 C7 119.6(4) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 117.6(5) . . ? C8 C9 H9 121.2 . . ? C10 C9 H9 121.2 . . ? N2 C10 C9 123.8(4) . . ? N2 C10 H10 118.1 . . ? C9 C10 H10 118.1 . . ? N3 C11 C12 174.6(4) . . ? C14 C12 C13 123.4(4) . . ? C14 C12 C11 123.2(4) . . ? C13 C12 C11 113.4(4) . . ? N4 C13 C12 175.2(5) . . ? C12 C14 C18 126.9(4) . . ? C12 C14 C15 123.9(4) . . ? C18 C14 C15 109.1(4) . . ? O1 C15 C14 125.8(4) . . ? O1 C15 C16 125.9(4) . . ? C14 C15 C16 108.3(4) . . ? C19 C16 C15 123.6(4) . . ? C19 C16 C17 128.7(4) . . ? C15 C16 C17 107.7(4) . . ? O2 C17 C16 127.4(4) . . ? O2 C17 C18 125.6(4) . . ? C16 C17 C18 107.1(4) . . ? O3 C18 C14 128.1(4) . . ? O3 C18 C17 124.2(4) . . ? C14 C18 C17 107.7(3) . . ? C16 C19 C21 123.2(4) . . ? C16 C19 C20 123.3(4) . . ? C21 C19 C20 113.4(4) . . ? N5 C20 C19 172.8(5) . . ? N6 C21 C19 174.5(5) . . ? O1S2 O1S1 H1S 53(5) . . ? O1S2 O1S1 H1S1 157.4(13) . . ? H1S O1S1 H1S1 128(6) . . ? O1S1 O1S2 H1S 70(6) . . ? O1S1 O1S2 H1S2 134(10) . . ? H1S O1S2 H1S2 122(10) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.654 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.121 #====END data_(3) _database_code_CSD 203380 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H8 Fe N4 O7' _chemical_formula_weight 364.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 6.9599(8) _cell_length_b 10.9174(11) _cell_length_c 11.2349(12) _cell_angle_alpha 108.533(13) _cell_angle_beta 101.440(13) _cell_angle_gamma 106.686(12) _cell_volume 734.85(14) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 26.05 _exptl_crystal_description parallelepiped _exptl_crystal_colour black _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.37 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 1.069 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.38 _exptl_absorpt_correction_T_max 0.79 _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS). The crystal-to-detector distance was 70 mm. 192 frames (4 min per frame) were obtained with 0 < \f < 249.6\% and with the crystals rotated through 1.3\% in \f. Coverage of the unique set was over 92.4% complete to at least 26.05\%. Crystal decay was monitored by measuring 200 reflexions per frame. ; _diffrn_ambient_temperature 180(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 'Stoe IPDS' _diffrn_measurement_method \f _diffrn_standards_number 200 _diffrn_standards_interval_time 'every frame' _diffrn_standards_decay_% <0.1 _diffrn_reflns_number 7260 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 26.05 _reflns_number_total 2682 _reflns_number_gt 2396 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software (Stoe, 1996)' _computing_data_reduction 'XRED (Stoe, 1.08, 1996)' _computing_cell_refinement 'Stoe IPDS software (Stoe, 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _computing_corr_abs DIFABS _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^)+(0.0584P)^2^+0.0335P] 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 2682 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0813 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Fe1 Fe 0.78089(3) 1.08003(2) 0.27970(2) 0.01701(11) Uani 1 1 d . . . O1 O 0.73646(18) 0.91473(13) 0.35718(12) 0.0191(3) Uani 1 1 d . . . O2 O 0.51369(19) 0.90889(13) 0.11912(13) 0.0222(3) Uani 1 1 d . . . O3 O 0.2911(2) 0.44514(13) 0.08591(14) 0.0264(3) Uani 1 1 d . . . N1 N 0.9462(2) 0.78317(16) 0.55566(16) 0.0216(4) Uani 1 1 d . . . N2 N 0.4871(3) 0.37138(18) 0.34777(17) 0.0278(4) Uani 1 1 d . . . N3 N 0.2075(2) 0.77549(17) -0.19167(16) 0.0231(4) Uani 1 1 d . . . N4 N -0.0171(2) 0.35538(17) -0.22127(17) 0.0256(4) Uani 1 1 d . . . C1 C 0.6054(2) 0.80225(18) 0.26475(17) 0.0155(4) Uani 1 1 d . . . C2 C 0.4899(2) 0.80124(18) 0.13975(17) 0.0169(4) Uani 1 1 d . . . C3 C 0.3542(2) 0.65837(18) 0.05484(17) 0.0164(4) Uani 1 1 d . . . C4 C 0.3826(2) 0.57248(18) 0.12819(17) 0.0172(4) Uani 1 1 d . . . C5 C 0.5409(2) 0.66357(18) 0.25840(17) 0.0156(4) Uani 1 1 d . . . C6 C 0.6174(2) 0.62038(18) 0.35489(17) 0.0166(4) Uani 1 1 d . . . C7 C 0.7970(3) 0.71287(19) 0.46691(18) 0.0176(4) Uani 1 1 d . . . C8 C 0.5386(3) 0.48069(19) 0.34564(17) 0.0186(4) Uani 1 1 d . . . C9 C 0.2246(2) 0.61119(18) -0.07338(17) 0.0168(4) Uani 1 1 d . . . C10 C 0.2162(2) 0.70359(19) -0.13677(18) 0.0181(4) Uani 1 1 d . . . C11 C 0.0921(2) 0.46720(19) -0.15162(17) 0.0180(4) Uani 1 1 d . . . O1W O 0.5798(2) 1.14280(17) 0.37749(15) 0.0253(3) Uani 1 1 d . . . H11W H 0.546(4) 1.201(3) 0.368(3) 0.029(7) Uiso 1 1 d . . . H12W H 0.482(5) 1.086(3) 0.377(3) 0.057(10) Uiso 1 1 d . . . O2W O 0.9842(2) 1.00792(16) 0.19005(16) 0.0241(3) Uani 1 1 d . . . H21W H 0.937(4) 0.954(3) 0.123(3) 0.032(7) Uiso 1 1 d . . . H22W H 1.063(5) 0.990(3) 0.237(3) 0.056(9) Uiso 1 1 d . . . O3W O 0.7722(2) 1.05536(16) 0.63080(15) 0.0243(3) Uani 1 1 d . . . H31W H 0.815(4) 1.139(3) 0.653(3) 0.045(8) Uiso 1 1 d . . . H32W H 0.773(5) 1.020(4) 0.550(4) 0.073(11) Uiso 1 1 d . . . O4W O 0.1790(4) -0.8294(2) 0.05401(19) 0.0488(5) Uani 1 1 d . . . H41W H 0.216(5) -0.748(4) 0.074(4) 0.063(10) Uiso 1 1 d . . . H42W H 0.156(8) -0.840(6) 0.119(6) 0.13(2) 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 Fe1 0.01670(15) 0.01421(16) 0.01558(16) 0.00488(12) 0.00114(10) 0.00342(11) O1 0.0186(6) 0.0152(6) 0.0162(6) 0.0030(5) 0.0009(5) 0.0029(5) O2 0.0224(6) 0.0161(6) 0.0204(6) 0.0070(6) -0.0017(5) 0.0026(5) O3 0.0303(7) 0.0144(6) 0.0230(7) 0.0053(6) -0.0032(5) 0.0031(5) N1 0.0223(8) 0.0175(8) 0.0195(8) 0.0068(7) 0.0005(6) 0.0045(6) N2 0.0324(9) 0.0205(9) 0.0270(9) 0.0090(8) 0.0064(7) 0.0079(7) N3 0.0232(8) 0.0192(8) 0.0188(8) 0.0052(7) -0.0001(6) 0.0042(6) N4 0.0243(8) 0.0207(8) 0.0230(8) 0.0027(7) 0.0054(6) 0.0044(6) C1 0.0139(7) 0.0165(8) 0.0159(8) 0.0066(7) 0.0047(6) 0.0051(6) C2 0.0149(7) 0.0159(8) 0.0171(8) 0.0057(7) 0.0035(6) 0.0038(6) C3 0.0132(7) 0.0160(8) 0.0185(8) 0.0056(7) 0.0048(6) 0.0050(6) C4 0.0156(7) 0.0163(8) 0.0173(8) 0.0050(7) 0.0035(6) 0.0059(6) C5 0.0140(7) 0.0162(8) 0.0158(8) 0.0047(7) 0.0052(6) 0.0059(6) C6 0.0151(8) 0.0158(8) 0.0155(8) 0.0040(7) 0.0032(6) 0.0045(6) C7 0.0194(8) 0.0173(8) 0.0187(9) 0.0087(8) 0.0069(7) 0.0084(7) C8 0.0175(8) 0.0198(9) 0.0147(8) 0.0044(7) 0.0016(6) 0.0072(7) C9 0.0141(7) 0.0171(8) 0.0171(8) 0.0056(7) 0.0040(6) 0.0049(6) C10 0.0141(7) 0.0175(9) 0.0155(8) 0.0024(8) 0.0011(6) 0.0033(6) C11 0.0163(8) 0.0216(10) 0.0156(8) 0.0069(8) 0.0047(7) 0.0074(7) O1W 0.0255(7) 0.0188(7) 0.0355(8) 0.0134(7) 0.0117(6) 0.0096(6) O2W 0.0265(7) 0.0234(7) 0.0186(7) 0.0050(7) 0.0047(6) 0.0094(6) O3W 0.0254(7) 0.0208(8) 0.0235(8) 0.0070(6) 0.0075(6) 0.0064(6) O4W 0.0838(14) 0.0189(8) 0.0298(9) 0.0034(8) 0.0214(9) 0.0047(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1W 2.0781(15) . ? Fe1 O2W 2.0826(15) . ? Fe1 N3 2.1030(19) 2_675 ? Fe1 N1 2.1167(16) 2_776 ? Fe1 O2 2.1760(13) . ? Fe1 O1 2.2125(14) . ? O1 C1 1.260(2) . ? O2 C2 1.241(2) . ? O3 C4 1.231(2) . ? N1 C7 1.143(2) . ? N1 Fe1 2.1167(16) 2_776 ? N2 C8 1.153(3) . ? N3 C10 1.149(3) . ? N3 Fe1 2.1030(19) 2_675 ? N4 C11 1.142(2) . ? C1 C5 1.424(3) . ? C1 C2 1.468(2) . ? C2 C3 1.444(2) . ? C3 C9 1.378(2) . ? C3 C4 1.460(3) . ? C4 C5 1.466(2) . ? C5 C6 1.386(3) . ? C6 C7 1.418(2) . ? C6 C8 1.426(3) . ? C9 C10 1.415(3) . ? C9 C11 1.436(2) . ? O1W H11W 0.76(3) . ? O1W H12W 0.77(3) . ? O2W H21W 0.73(3) . ? O2W H22W 0.80(4) . ? O3W H31W 0.80(3) . ? O3W H32W 0.87(4) . ? O4W H41W 0.79(4) . ? O4W H42W 0.81(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Fe1 O2W 175.63(7) . . ? O1W Fe1 N3 91.68(7) . 2_675 ? O2W Fe1 N3 92.66(6) . 2_675 ? O1W Fe1 N1 92.62(6) . 2_776 ? O2W Fe1 N1 86.46(6) . 2_776 ? N3 Fe1 N1 94.25(6) 2_675 2_776 ? O1W Fe1 O2 91.20(6) . . ? O2W Fe1 O2 88.99(6) . . ? N3 Fe1 O2 95.59(6) 2_675 . ? N1 Fe1 O2 169.33(6) 2_776 . ? O1W Fe1 O1 87.04(6) . . ? O2W Fe1 O1 88.71(6) . . ? N3 Fe1 O1 174.16(5) 2_675 . ? N1 Fe1 O1 91.50(6) 2_776 . ? O2 Fe1 O1 78.75(5) . . ? C1 O1 Fe1 107.75(11) . . ? C2 O2 Fe1 108.56(11) . . ? C7 N1 Fe1 177.80(15) . 2_776 ? C10 N3 Fe1 174.73(14) . 2_675 ? O1 C1 C5 130.05(16) . . ? O1 C1 C2 120.80(16) . . ? C5 C1 C2 109.15(14) . . ? O2 C2 C3 129.78(16) . . ? O2 C2 C1 122.70(15) . . ? C3 C2 C1 107.51(16) . . ? C9 C3 C2 126.17(18) . . ? C9 C3 C4 126.14(16) . . ? C2 C3 C4 107.68(15) . . ? O3 C4 C3 125.33(16) . . ? O3 C4 C5 126.45(17) . . ? C3 C4 C5 108.22(15) . . ? C6 C5 C1 126.84(15) . . ? C6 C5 C4 125.70(16) . . ? C1 C5 C4 107.42(15) . . ? C5 C6 C7 120.85(16) . . ? C5 C6 C8 124.24(15) . . ? C7 C6 C8 114.67(16) . . ? N1 C7 C6 176.88(19) . . ? N2 C8 C6 174.51(18) . . ? C3 C9 C10 121.29(16) . . ? C3 C9 C11 123.07(18) . . ? C10 C9 C11 115.64(15) . . ? N3 C10 C9 178.05(18) . . ? N4 C11 C9 175.1(2) . . ? Fe1 O1W H11W 119(2) . . ? Fe1 O1W H12W 118(2) . . ? H11W O1W H12W 108(3) . . ? Fe1 O2W H21W 117(2) . . ? Fe1 O2W H22W 112(2) . . ? H21W O2W H22W 112(3) . . ? H31W O3W H32W 107(3) . . ? H41W O4W H42W 104(5) . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.519 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.070 #====END