data_global _publ_contact_author ; Hideo Nagashima Institute for Advanced Material Study Kyushu University, Kasuga, Fukuoka 816-8580, Japan' ; _publ_section_title ; Thermally Reversible Photochemical Haptotropic Rearrangement of Diiron Carbonyl Complexes Bearing a Bridging Acenaphthylene or Aceanthrylene Ligand ; _publ_author_name ; S. Niibayashi, K. Matsubara, Masa-aki Haga, and H. Nagashima ; data_1-A _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H8 Fe2 O5' _chemical_formula_weight 403.94 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' '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 'Orthorhombic' _symmetry_space_group_name_H-M 'C 2 2 21 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' '-x, y, -z+1/2' '-x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z+1/2' '-x+1/2, -y+1/2, z+1/2' _cell_length_a 12.7813(10) _cell_length_b 13.8254(8) _cell_length_c 16.7924(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2967.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15786 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description 'Block' _exptl_crystal_colour 'Red' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.808 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 1.980 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.436 _exptl_absorpt_correction_T_max 0.673 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method 'oscillation' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 1807 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.47 _reflns_number_total 1807 _reflns_number_gt 1614 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction ; teXsan for Windows version 1.06 (MSC, 1997-1999) ; _computing_structure_solution ; DIRDIF94 PATTY (Beurskens, 1994) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP III (Farrujia, 1998)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.43(3) _refine_ls_number_reflns 1807 _refine_ls_number_parameters 249 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.048 _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 0.32202(5) 0.25884(4) 0.05198(3) 0.02435(15) Uani 1 1 d . . . Fe2 Fe 0.22009(5) 0.21894(5) 0.19381(3) 0.02412(16) Uani 1 1 d . . . O1 O 0.2463(4) 0.1061(3) -0.0522(2) 0.0538(12) Uani 1 1 d . . . O2 O 0.2007(4) 0.4007(3) -0.0382(3) 0.0552(12) Uani 1 1 d . . . O3 O 0.1140(3) 0.0688(3) 0.1010(2) 0.0391(8) Uani 1 1 d . . . O4 O 0.0994(3) 0.3873(3) 0.1408(3) 0.0490(11) Uani 1 1 d . . . O5 O 0.0844(3) 0.1892(4) 0.3322(2) 0.0544(12) Uani 1 1 d . . . C1 C 0.4796(4) 0.2325(5) 0.0250(3) 0.0440(13) Uani 1 1 d . . . C2 C 0.4645(4) 0.3332(4) 0.0400(4) 0.0462(14) Uani 1 1 d . . . C3 C 0.3953(5) 0.4232(4) 0.1704(5) 0.0558(19) Uani 1 1 d . . . C4 C 0.3498(5) 0.4030(5) 0.2411(5) 0.062(2) Uani 1 1 d . . . C5 C 0.3300(4) 0.3053(5) 0.2683(3) 0.0463(14) Uani 1 1 d . . . C6 C 0.3517(4) 0.1266(4) 0.2395(3) 0.0375(12) Uani 1 1 d . . . C7 C 0.3966(4) 0.0559(4) 0.1861(4) 0.0412(12) Uani 1 1 d . . . C8 C 0.4453(4) 0.0793(4) 0.1168(3) 0.0402(13) Uani 1 1 d . . . C9 C 0.4517(3) 0.1800(4) 0.0958(3) 0.0316(10) Uani 1 1 d . . . C10 C 0.4275(4) 0.3446(4) 0.1207(4) 0.0411(13) Uani 1 1 d . . . C11 C 0.4207(3) 0.2492(4) 0.1526(3) 0.0276(9) Uani 1 1 d . . . C12 C 0.3748(3) 0.2270(4) 0.2271(3) 0.0328(10) Uani 1 1 d . . . C13 C 0.2727(4) 0.1640(4) -0.0088(3) 0.0330(10) Uani 1 1 d . . . C14 C 0.2455(4) 0.3455(4) 0.0011(3) 0.0346(11) Uani 1 1 d . . . C15 C 0.1590(4) 0.1285(4) 0.1340(3) 0.0288(10) Uani 1 1 d . . . C16 C 0.1510(4) 0.3213(4) 0.1577(3) 0.0326(10) Uani 1 1 d . . . C17 C 0.1395(4) 0.1990(4) 0.2786(3) 0.0360(11) Uani 1 1 d . . . H1 H 0.497(6) 0.205(4) -0.024(4) 0.057(19) Uiso 1 1 d . . . H2 H 0.475(4) 0.388(4) 0.001(4) 0.038(15) Uiso 1 1 d . . . H3 H 0.405(6) 0.489(6) 0.145(4) 0.06(2) Uiso 1 1 d . . . H4 H 0.325(6) 0.468(6) 0.272(5) 0.09(3) Uiso 1 1 d . . . H5 H 0.310(6) 0.294(5) 0.329(4) 0.07(2) Uiso 1 1 d . . . H6 H 0.338(6) 0.099(6) 0.288(5) 0.09(3) Uiso 1 1 d . . . H7 H 0.393(5) -0.018(5) 0.200(4) 0.058(19) Uiso 1 1 d . . . H8 H 0.471(5) 0.019(5) 0.074(4) 0.06(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 0.0230(3) 0.0310(3) 0.0190(3) 0.0019(2) 0.0007(2) 0.0028(2) Fe2 0.0170(2) 0.0381(4) 0.0173(3) -0.0012(3) -0.0011(2) 0.0030(2) O1 0.089(4) 0.044(2) 0.0288(18) -0.0081(18) -0.013(2) -0.002(2) O2 0.064(3) 0.040(2) 0.061(3) 0.017(2) -0.021(2) 0.0061(18) O3 0.044(2) 0.0308(16) 0.043(2) 0.0033(17) -0.0080(19) -0.0040(15) O4 0.051(2) 0.0422(19) 0.054(3) -0.0077(19) -0.009(2) 0.0207(19) O5 0.041(2) 0.092(3) 0.0301(19) 0.003(2) 0.0106(17) 0.003(2) C1 0.022(2) 0.080(4) 0.030(2) 0.007(3) 0.0103(19) 0.007(2) C2 0.024(2) 0.057(3) 0.057(4) 0.019(3) 0.011(2) -0.004(2) C3 0.036(3) 0.038(3) 0.094(6) -0.021(3) -0.010(3) -0.011(2) C4 0.040(3) 0.071(4) 0.074(5) -0.048(4) -0.013(3) 0.002(3) C5 0.030(2) 0.076(4) 0.033(3) -0.026(3) -0.009(2) 0.004(3) C6 0.024(2) 0.061(3) 0.028(3) 0.012(2) -0.005(2) 0.006(2) C7 0.035(2) 0.048(3) 0.040(3) 0.009(2) -0.013(2) 0.015(2) C8 0.032(3) 0.050(3) 0.039(3) -0.002(3) -0.006(2) 0.021(2) C9 0.023(2) 0.048(3) 0.025(2) -0.003(2) 0.0014(18) 0.0104(18) C10 0.021(2) 0.043(3) 0.059(4) -0.003(3) -0.004(2) -0.010(2) C11 0.0130(17) 0.042(2) 0.028(2) -0.0047(19) -0.0035(15) 0.0033(17) C12 0.0158(17) 0.063(3) 0.0189(18) -0.004(2) -0.0080(16) 0.003(2) C13 0.041(2) 0.035(2) 0.022(2) 0.0045(19) 0.001(2) 0.006(2) C14 0.033(2) 0.038(3) 0.033(3) 0.000(2) -0.002(2) 0.0024(18) C15 0.026(2) 0.036(2) 0.024(2) 0.0060(18) -0.0018(18) 0.0083(19) C16 0.028(2) 0.039(2) 0.030(2) -0.011(2) -0.0029(19) 0.0014(19) C17 0.026(2) 0.053(3) 0.029(2) 0.002(2) -0.001(2) 0.003(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 C14 1.768(5) . ? Fe1 C13 1.776(5) . ? Fe1 C1 2.097(5) . ? Fe1 C2 2.101(5) . ? Fe1 C11 2.112(4) . ? Fe1 C9 2.116(5) . ? Fe1 C10 2.134(5) . ? Fe1 Fe2 2.7702(9) . ? Fe2 C16 1.775(5) . ? Fe2 C17 1.779(5) . ? Fe2 C15 1.784(5) . ? Fe2 C12 2.058(4) . ? Fe2 C5 2.227(5) . ? Fe2 C6 2.247(5) . ? O1 C13 1.134(6) . ? O2 C14 1.159(7) . ? O3 C15 1.148(6) . ? O4 C16 1.161(6) . ? O5 C17 1.151(6) . ? C1 C2 1.427(9) . ? C1 C9 1.439(7) . ? C2 C10 1.443(9) . ? C3 C4 1.350(11) . ? C3 C10 1.432(9) . ? C4 C5 1.449(10) . ? C5 C12 1.407(7) . ? C6 C12 1.434(8) . ? C6 C7 1.445(8) . ? C7 C8 1.360(8) . ? C8 C9 1.438(8) . ? C9 C11 1.407(7) . ? C10 C11 1.426(8) . ? C11 C12 1.416(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 C14 Fe1 C13 91.5(2) . . ? C14 Fe1 C1 123.0(2) . . ? C13 Fe1 C1 95.1(2) . . ? C14 Fe1 C2 95.8(2) . . ? C13 Fe1 C2 127.9(2) . . ? C1 Fe1 C2 39.8(2) . . ? C14 Fe1 C11 139.5(2) . . ? C13 Fe1 C11 128.6(2) . . ? C1 Fe1 C11 65.69(18) . . ? C2 Fe1 C11 65.8(2) . . ? C14 Fe1 C9 162.0(2) . . ? C13 Fe1 C9 95.6(2) . . ? C1 Fe1 C9 39.94(19) . . ? C2 Fe1 C9 66.8(2) . . ? C11 Fe1 C9 38.87(18) . . ? C14 Fe1 C10 103.6(2) . . ? C13 Fe1 C10 160.8(2) . . ? C1 Fe1 C10 66.8(2) . . ? C2 Fe1 C10 39.8(2) . . ? C11 Fe1 C10 39.2(2) . . ? C9 Fe1 C10 66.6(2) . . ? C14 Fe1 Fe2 106.89(18) . . ? C13 Fe1 Fe2 100.36(16) . . ? C1 Fe1 Fe2 127.10(15) . . ? C2 Fe1 Fe2 125.96(19) . . ? C11 Fe1 Fe2 65.21(12) . . ? C9 Fe1 Fe2 88.09(13) . . ? C10 Fe1 Fe2 86.73(17) . . ? C16 Fe2 C17 96.2(2) . . ? C16 Fe2 C15 98.6(2) . . ? C17 Fe2 C15 95.1(2) . . ? C16 Fe2 C12 121.9(2) . . ? C17 Fe2 C12 110.4(2) . . ? C15 Fe2 C12 127.7(2) . . ? C16 Fe2 C5 94.5(2) . . ? C17 Fe2 C5 90.0(2) . . ? C15 Fe2 C5 165.4(2) . . ? C12 Fe2 C5 38.1(2) . . ? C16 Fe2 C6 160.4(2) . . ? C17 Fe2 C6 94.2(2) . . ? C15 Fe2 C6 97.0(2) . . ? C12 Fe2 C6 38.6(2) . . ? C5 Fe2 C6 68.9(2) . . ? C16 Fe2 Fe1 77.39(16) . . ? C17 Fe2 Fe1 172.45(16) . . ? C15 Fe2 Fe1 82.03(16) . . ? C12 Fe2 Fe1 76.75(12) . . ? C5 Fe2 Fe1 94.56(16) . . ? C6 Fe2 Fe1 93.12(14) . . ? C2 C1 C9 108.2(5) . . ? C2 C1 Fe1 70.3(3) . . ? C9 C1 Fe1 70.8(3) . . ? C1 C2 C10 108.5(5) . . ? C1 C2 Fe1 70.0(3) . . ? C10 C2 Fe1 71.3(3) . . ? C4 C3 C10 118.6(6) . . ? C3 C4 C5 123.1(6) . . ? C12 C5 C4 119.4(5) . . ? C12 C5 Fe2 64.4(3) . . ? C4 C5 Fe2 115.7(4) . . ? C12 C6 C7 118.9(5) . . ? C12 C6 Fe2 63.6(3) . . ? C7 C6 Fe2 118.0(4) . . ? C8 C7 C6 123.5(5) . . ? C7 C8 C9 117.8(5) . . ? C11 C9 C8 118.5(5) . . ? C11 C9 C1 106.7(5) . . ? C8 C9 C1 134.8(5) . . ? C11 C9 Fe1 70.4(3) . . ? C8 C9 Fe1 122.6(4) . . ? C1 C9 Fe1 69.3(3) . . ? C11 C10 C3 117.7(6) . . ? C11 C10 C2 105.8(5) . . ? C3 C10 C2 136.4(6) . . ? C11 C10 Fe1 69.6(3) . . ? C3 C10 Fe1 123.8(4) . . ? C2 C10 Fe1 68.9(3) . . ? C9 C11 C12 124.6(5) . . ? C9 C11 C10 110.9(5) . . ? C12 C11 C10 123.9(5) . . ? C9 C11 Fe1 70.7(3) . . ? C12 C11 Fe1 118.2(3) . . ? C10 C11 Fe1 71.2(3) . . ? C5 C12 C11 115.9(5) . . ? C5 C12 C6 126.1(5) . . ? C11 C12 C6 115.0(5) . . ? C5 C12 Fe2 77.5(3) . . ? C11 C12 Fe2 99.8(3) . . ? C6 C12 Fe2 77.8(3) . . ? O1 C13 Fe1 174.6(5) . . ? O2 C14 Fe1 173.9(5) . . ? O3 C15 Fe2 174.0(5) . . ? O4 C16 Fe2 173.1(5) . . ? O5 C17 Fe2 176.9(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 Fe1 Fe2 C16 -10.6(2) . . . . ? C13 Fe1 Fe2 C16 -105.4(2) . . . . ? C1 Fe1 Fe2 C16 150.0(3) . . . . ? C2 Fe1 Fe2 C16 100.0(3) . . . . ? C11 Fe1 Fe2 C16 126.7(2) . . . . ? C9 Fe1 Fe2 C16 159.2(2) . . . . ? C10 Fe1 Fe2 C16 92.6(2) . . . . ? C14 Fe1 Fe2 C17 22.3(14) . . . . ? C13 Fe1 Fe2 C17 -72.4(14) . . . . ? C1 Fe1 Fe2 C17 -177.0(14) . . . . ? C2 Fe1 Fe2 C17 133.0(14) . . . . ? C11 Fe1 Fe2 C17 159.6(14) . . . . ? C9 Fe1 Fe2 C17 -167.8(14) . . . . ? C10 Fe1 Fe2 C17 125.5(14) . . . . ? C14 Fe1 Fe2 C15 90.1(2) . . . . ? C13 Fe1 Fe2 C15 -4.7(2) . . . . ? C1 Fe1 Fe2 C15 -109.3(3) . . . . ? C2 Fe1 Fe2 C15 -159.3(2) . . . . ? C11 Fe1 Fe2 C15 -132.6(2) . . . . ? C9 Fe1 Fe2 C15 -100.06(19) . . . . ? C10 Fe1 Fe2 C15 -166.7(2) . . . . ? C14 Fe1 Fe2 C12 -138.1(2) . . . . ? C13 Fe1 Fe2 C12 127.1(2) . . . . ? C1 Fe1 Fe2 C12 22.6(3) . . . . ? C2 Fe1 Fe2 C12 -27.5(3) . . . . ? C11 Fe1 Fe2 C12 -0.8(2) . . . . ? C9 Fe1 Fe2 C12 31.8(2) . . . . ? C10 Fe1 Fe2 C12 -34.9(2) . . . . ? C14 Fe1 Fe2 C5 -104.2(2) . . . . ? C13 Fe1 Fe2 C5 161.0(2) . . . . ? C1 Fe1 Fe2 C5 56.5(3) . . . . ? C2 Fe1 Fe2 C5 6.4(3) . . . . ? C11 Fe1 Fe2 C5 33.1(2) . . . . ? C9 Fe1 Fe2 C5 65.7(2) . . . . ? C10 Fe1 Fe2 C5 -1.0(2) . . . . ? C14 Fe1 Fe2 C6 -173.3(2) . . . . ? C13 Fe1 Fe2 C6 91.9(2) . . . . ? C1 Fe1 Fe2 C6 -12.6(3) . . . . ? C2 Fe1 Fe2 C6 -62.7(3) . . . . ? C11 Fe1 Fe2 C6 -36.0(2) . . . . ? C9 Fe1 Fe2 C6 -3.4(2) . . . . ? C10 Fe1 Fe2 C6 -70.1(2) . . . . ? C14 Fe1 C1 C2 53.8(4) . . . . ? C13 Fe1 C1 C2 148.9(4) . . . . ? C11 Fe1 C1 C2 -80.7(4) . . . . ? C9 Fe1 C1 C2 -118.4(5) . . . . ? C10 Fe1 C1 C2 -37.7(4) . . . . ? Fe2 Fe1 C1 C2 -104.0(3) . . . . ? C14 Fe1 C1 C9 172.2(3) . . . . ? C13 Fe1 C1 C9 -92.7(3) . . . . ? C2 Fe1 C1 C9 118.4(5) . . . . ? C11 Fe1 C1 C9 37.7(3) . . . . ? C10 Fe1 C1 C9 80.7(3) . . . . ? Fe2 Fe1 C1 C9 14.4(4) . . . . ? C9 C1 C2 C10 0.3(6) . . . . ? Fe1 C1 C2 C10 61.2(4) . . . . ? C9 C1 C2 Fe1 -60.9(4) . . . . ? C14 Fe1 C2 C1 -137.2(4) . . . . ? C13 Fe1 C2 C1 -40.7(4) . . . . ? C11 Fe1 C2 C1 80.5(3) . . . . ? C9 Fe1 C2 C1 37.9(3) . . . . ? C10 Fe1 C2 C1 118.7(5) . . . . ? Fe2 Fe1 C2 C1 107.1(3) . . . . ? C14 Fe1 C2 C10 104.2(4) . . . . ? C13 Fe1 C2 C10 -159.3(3) . . . . ? C1 Fe1 C2 C10 -118.7(5) . . . . ? C11 Fe1 C2 C10 -38.2(3) . . . . ? C9 Fe1 C2 C10 -80.8(3) . . . . ? Fe2 Fe1 C2 C10 -11.6(4) . . . . ? C10 C3 C4 C5 -1.4(10) . . . . ? C3 C4 C5 C12 11.2(9) . . . . ? C3 C4 C5 Fe2 -62.6(7) . . . . ? C16 Fe2 C5 C12 -139.3(3) . . . . ? C17 Fe2 C5 C12 124.4(3) . . . . ? C15 Fe2 C5 C12 14.1(10) . . . . ? C6 Fe2 C5 C12 29.9(3) . . . . ? Fe1 Fe2 C5 C12 -61.6(3) . . . . ? C16 Fe2 C5 C4 -27.4(5) . . . . ? C17 Fe2 C5 C4 -123.6(5) . . . . ? C15 Fe2 C5 C4 126.1(9) . . . . ? C12 Fe2 C5 C4 112.0(6) . . . . ? C6 Fe2 C5 C4 141.9(5) . . . . ? Fe1 Fe2 C5 C4 50.3(4) . . . . ? C16 Fe2 C6 C12 4.1(8) . . . . ? C17 Fe2 C6 C12 -117.9(3) . . . . ? C15 Fe2 C6 C12 146.5(3) . . . . ? C5 Fe2 C6 C12 -29.6(3) . . . . ? Fe1 Fe2 C6 C12 64.1(3) . . . . ? C16 Fe2 C6 C7 -106.2(7) . . . . ? C17 Fe2 C6 C7 131.8(5) . . . . ? C15 Fe2 C6 C7 36.2(5) . . . . ? C12 Fe2 C6 C7 -110.3(5) . . . . ? C5 Fe2 C6 C7 -139.8(5) . . . . ? Fe1 Fe2 C6 C7 -46.1(4) . . . . ? C12 C6 C7 C8 -11.5(8) . . . . ? Fe2 C6 C7 C8 62.1(7) . . . . ? C6 C7 C8 C9 -0.2(8) . . . . ? C7 C8 C9 C11 8.6(7) . . . . ? C7 C8 C9 C1 -167.9(5) . . . . ? C7 C8 C9 Fe1 -75.3(6) . . . . ? C2 C1 C9 C11 -0.3(6) . . . . ? Fe1 C1 C9 C11 -60.8(3) . . . . ? C2 C1 C9 C8 176.5(6) . . . . ? Fe1 C1 C9 C8 115.9(6) . . . . ? C2 C1 C9 Fe1 60.6(4) . . . . ? C14 Fe1 C9 C11 95.8(7) . . . . ? C13 Fe1 C9 C11 -151.4(3) . . . . ? C1 Fe1 C9 C11 117.4(4) . . . . ? C2 Fe1 C9 C11 79.7(3) . . . . ? C10 Fe1 C9 C11 36.1(3) . . . . ? Fe2 Fe1 C9 C11 -51.2(3) . . . . ? C14 Fe1 C9 C8 -152.3(7) . . . . ? C13 Fe1 C9 C8 -39.5(4) . . . . ? C1 Fe1 C9 C8 -130.8(6) . . . . ? C2 Fe1 C9 C8 -168.5(5) . . . . ? C11 Fe1 C9 C8 111.9(5) . . . . ? C10 Fe1 C9 C8 148.0(4) . . . . ? Fe2 Fe1 C9 C8 60.7(4) . . . . ? C14 Fe1 C9 C1 -21.6(8) . . . . ? C13 Fe1 C9 C1 91.2(4) . . . . ? C2 Fe1 C9 C1 -37.7(4) . . . . ? C11 Fe1 C9 C1 -117.4(4) . . . . ? C10 Fe1 C9 C1 -81.3(4) . . . . ? Fe2 Fe1 C9 C1 -168.5(3) . . . . ? C4 C3 C10 C11 -7.1(8) . . . . ? C4 C3 C10 C2 170.1(7) . . . . ? C4 C3 C10 Fe1 75.9(8) . . . . ? C1 C2 C10 C11 -0.3(6) . . . . ? Fe1 C2 C10 C11 60.1(3) . . . . ? C1 C2 C10 C3 -177.6(6) . . . . ? Fe1 C2 C10 C3 -117.3(7) . . . . ? C1 C2 C10 Fe1 -60.4(4) . . . . ? C14 Fe1 C10 C11 160.2(3) . . . . ? C13 Fe1 C10 C11 -59.0(8) . . . . ? C1 Fe1 C10 C11 -79.4(3) . . . . ? C2 Fe1 C10 C11 -117.1(4) . . . . ? C9 Fe1 C10 C11 -35.8(3) . . . . ? Fe2 Fe1 C10 C11 53.6(3) . . . . ? C14 Fe1 C10 C3 49.8(6) . . . . ? C13 Fe1 C10 C3 -169.4(6) . . . . ? C1 Fe1 C10 C3 170.2(6) . . . . ? C2 Fe1 C10 C3 132.5(7) . . . . ? C11 Fe1 C10 C3 -110.4(7) . . . . ? C9 Fe1 C10 C3 -146.2(6) . . . . ? Fe2 Fe1 C10 C3 -56.8(6) . . . . ? C14 Fe1 C10 C2 -82.8(4) . . . . ? C13 Fe1 C10 C2 58.0(8) . . . . ? C1 Fe1 C10 C2 37.6(3) . . . . ? C11 Fe1 C10 C2 117.1(4) . . . . ? C9 Fe1 C10 C2 81.3(3) . . . . ? Fe2 Fe1 C10 C2 170.6(3) . . . . ? C8 C9 C11 C12 -5.7(7) . . . . ? C1 C9 C11 C12 171.7(4) . . . . ? Fe1 C9 C11 C12 111.6(4) . . . . ? C8 C9 C11 C10 -177.3(4) . . . . ? C1 C9 C11 C10 0.1(5) . . . . ? Fe1 C9 C11 C10 -60.0(3) . . . . ? C8 C9 C11 Fe1 -117.3(4) . . . . ? C1 C9 C11 Fe1 60.1(3) . . . . ? C3 C10 C11 C9 178.1(5) . . . . ? C2 C10 C11 C9 0.1(6) . . . . ? Fe1 C10 C11 C9 59.8(3) . . . . ? C3 C10 C11 C12 6.4(7) . . . . ? C2 C10 C11 C12 -171.6(4) . . . . ? Fe1 C10 C11 C12 -111.9(4) . . . . ? C3 C10 C11 Fe1 118.3(5) . . . . ? C2 C10 C11 Fe1 -59.7(4) . . . . ? C14 Fe1 C11 C9 -151.8(3) . . . . ? C13 Fe1 C11 C9 37.6(4) . . . . ? C1 Fe1 C11 C9 -38.7(3) . . . . ? C2 Fe1 C11 C9 -82.5(3) . . . . ? C10 Fe1 C11 C9 -121.2(4) . . . . ? Fe2 Fe1 C11 C9 121.0(3) . . . . ? C14 Fe1 C11 C12 88.5(5) . . . . ? C13 Fe1 C11 C12 -82.1(5) . . . . ? C1 Fe1 C11 C12 -158.4(5) . . . . ? C2 Fe1 C11 C12 157.8(5) . . . . ? C9 Fe1 C11 C12 -119.7(5) . . . . ? C10 Fe1 C11 C12 119.1(5) . . . . ? Fe2 Fe1 C11 C12 1.3(4) . . . . ? C14 Fe1 C11 C10 -30.5(5) . . . . ? C13 Fe1 C11 C10 158.8(3) . . . . ? C1 Fe1 C11 C10 82.5(3) . . . . ? C2 Fe1 C11 C10 38.7(3) . . . . ? C9 Fe1 C11 C10 121.2(4) . . . . ? Fe2 Fe1 C11 C10 -117.8(3) . . . . ? C4 C5 C12 C11 -11.4(7) . . . . ? Fe2 C5 C12 C11 94.9(3) . . . . ? C4 C5 C12 C6 -171.0(5) . . . . ? Fe2 C5 C12 C6 -64.6(4) . . . . ? C4 C5 C12 Fe2 -106.3(5) . . . . ? C9 C11 C12 C5 -167.5(4) . . . . ? C10 C11 C12 C5 3.0(6) . . . . ? Fe1 C11 C12 C5 -82.4(5) . . . . ? C9 C11 C12 C6 -5.7(6) . . . . ? C10 C11 C12 C6 164.9(4) . . . . ? Fe1 C11 C12 C6 79.5(5) . . . . ? C9 C11 C12 Fe2 -86.7(5) . . . . ? C10 C11 C12 Fe2 83.8(5) . . . . ? Fe1 C11 C12 Fe2 -1.6(4) . . . . ? C7 C6 C12 C5 173.5(5) . . . . ? Fe2 C6 C12 C5 64.5(4) . . . . ? C7 C6 C12 C11 13.8(6) . . . . ? Fe2 C6 C12 C11 -95.2(3) . . . . ? C7 C6 C12 Fe2 109.0(5) . . . . ? C16 Fe2 C12 C5 49.9(4) . . . . ? C17 Fe2 C12 C5 -61.6(4) . . . . ? C15 Fe2 C12 C5 -175.5(3) . . . . ? C6 Fe2 C12 C5 -131.7(5) . . . . ? Fe1 Fe2 C12 C5 115.7(3) . . . . ? C16 Fe2 C12 C11 -64.7(4) . . . . ? C17 Fe2 C12 C11 -176.2(4) . . . . ? C15 Fe2 C12 C11 69.9(4) . . . . ? C5 Fe2 C12 C11 -114.6(5) . . . . ? C6 Fe2 C12 C11 113.7(5) . . . . ? Fe1 Fe2 C12 C11 1.1(3) . . . . ? C16 Fe2 C12 C6 -178.4(3) . . . . ? C17 Fe2 C12 C6 70.1(3) . . . . ? C15 Fe2 C12 C6 -43.8(4) . . . . ? C5 Fe2 C12 C6 131.7(5) . . . . ? Fe1 Fe2 C12 C6 -112.6(3) . . . . ? C14 Fe1 C13 O1 76(5) . . . . ? C1 Fe1 C13 O1 -48(5) . . . . ? C2 Fe1 C13 O1 -23(5) . . . . ? C11 Fe1 C13 O1 -110(5) . . . . ? C9 Fe1 C13 O1 -88(5) . . . . ? C10 Fe1 C13 O1 -66(5) . . . . ? Fe2 Fe1 C13 O1 -177(5) . . . . ? C13 Fe1 C14 O2 -66(5) . . . . ? C1 Fe1 C14 O2 31(5) . . . . ? C2 Fe1 C14 O2 62(5) . . . . ? C11 Fe1 C14 O2 121(4) . . . . ? C9 Fe1 C14 O2 47(5) . . . . ? C10 Fe1 C14 O2 102(5) . . . . ? Fe2 Fe1 C14 O2 -168(5) . . . . ? C16 Fe2 C15 O3 -96(4) . . . . ? C17 Fe2 C15 O3 1(4) . . . . ? C12 Fe2 C15 O3 122(4) . . . . ? C5 Fe2 C15 O3 111(4) . . . . ? C6 Fe2 C15 O3 96(4) . . . . ? Fe1 Fe2 C15 O3 -172(4) . . . . ? C17 Fe2 C16 O4 2(4) . . . . ? C15 Fe2 C16 O4 98(4) . . . . ? C12 Fe2 C16 O4 -117(4) . . . . ? C5 Fe2 C16 O4 -89(4) . . . . ? C6 Fe2 C16 O4 -120(3) . . . . ? Fe1 Fe2 C16 O4 177(4) . . . . ? C16 Fe2 C17 O5 6(10) . . . . ? C15 Fe2 C17 O5 -93(10) . . . . ? C12 Fe2 C17 O5 133(10) . . . . ? C5 Fe2 C17 O5 101(10) . . . . ? C6 Fe2 C17 O5 169(10) . . . . ? Fe1 Fe2 C17 O5 -26(11) . . . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.538 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.209 #===END data_1-B _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H8 Fe2 O5' _chemical_formula_weight 403.94 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' '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 7.9815(17) _cell_length_b 12.8740(18) _cell_length_c 7.8145(15) _cell_angle_alpha 100.420(9) _cell_angle_beta 111.648(9) _cell_angle_gamma 88.591(12) _cell_volume 733.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5285 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.4 _exptl_crystal_description 'Block' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.830 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 2.003 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.338 _exptl_absorpt_correction_T_max 0.606 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method 'oscillation' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3061 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3061 _reflns_number_gt 2505 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction ; teXsan for Windows version 1.06 (MSC, 1997-1999) ; _computing_structure_solution ; DIRDIF94 PATTY (Beurskens, 1994) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP III (Farrujia, 1998)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twic e 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^)+(0.0572P)^2^+3.1861P] 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 0.070(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3061 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1543 _refine_ls_wR_factor_gt 0.1350 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.36240(9) 0.33333(6) 1.19247(10) 0.0301(3) Uani 1 1 d . . . Fe2 Fe 0.14334(9) 0.21882(6) 0.84202(10) 0.0274(2) Uani 1 1 d . . . O1 O 0.7495(6) 0.3569(6) 1.2796(8) 0.0780(19) Uani 1 1 d . . . O2 O 0.2976(9) 0.5392(4) 1.0856(8) 0.0728(16) Uani 1 1 d . . . O3 O 0.5161(5) 0.2403(4) 0.8730(6) 0.0457(10) Uani 1 1 d . . . O4 O -0.0058(8) 0.4100(4) 0.7006(8) 0.0649(14) Uani 1 1 d . . . O5 O 0.0604(6) 0.1093(3) 0.4579(6) 0.0461(10) Uani 1 1 d . . . C1 C 0.3415(8) 0.3420(5) 1.4552(8) 0.0374(12) Uani 1 1 d . . . C2 C 0.1673(8) 0.3479(5) 1.3173(8) 0.0365(12) Uani 1 1 d . . . C3 C -0.0209(6) 0.2135(5) 1.0062(8) 0.0337(11) Uani 1 1 d . . . C4 C -0.0062(7) 0.1144(5) 0.9053(8) 0.0361(12) Uani 1 1 d . . . C5 C 0.1671(7) 0.0703(5) 0.9440(8) 0.0352(11) Uani 1 1 d . . . C6 C 0.4582(8) 0.0407(5) 1.2163(8) 0.0381(12) Uani 1 1 d . . . C7 C 0.5864(8) 0.0875(5) 1.3961(8) 0.0415(13) Uani 1 1 d . . . C8 C 0.5704(7) 0.1852(6) 1.4916(8) 0.0419(14) Uani 1 1 d . . . C9 C 0.4100(7) 0.2399(4) 1.4126(7) 0.0323(11) Uani 1 1 d . . . C10 C 0.1270(7) 0.2531(4) 1.1786(7) 0.0298(10) Uani 1 1 d . . . C11 C 0.2808(6) 0.1892(4) 1.2401(7) 0.0276(10) Uani 1 1 d . . . C12 C 0.3048(7) 0.0938(4) 1.1326(7) 0.0303(10) Uani 1 1 d . . . C13 C 0.5982(8) 0.3459(6) 1.2404(8) 0.0469(15) Uani 1 1 d . . . C14 C 0.3233(9) 0.4579(5) 1.1241(9) 0.0453(14) Uani 1 1 d . . . C15 C 0.3817(7) 0.2436(4) 0.8963(8) 0.0331(11) Uani 1 1 d . . . C16 C 0.0516(8) 0.3363(5) 0.7589(8) 0.0386(12) Uani 1 1 d . . . C17 C 0.0905(7) 0.1528(4) 0.6102(8) 0.0334(11) Uani 1 1 d . . . H1 H 0.3997 0.3951 1.5620 0.037 Uiso 1 1 d . . . H2 H 0.0902 0.4062 1.3187 0.036 Uiso 1 1 d . . . H3 H 0.1804 0.0069 0.8675 0.039 Uiso 1 1 d . . . H4 H -0.1114 0.0745 0.8066 0.037 Uiso 1 1 d . . . H5 H -0.1348 0.2457 0.9732 0.036 Uiso 1 1 d . . . H6 H 0.4728 -0.0298 1.1504 0.041 Uiso 1 1 d . . . H7 H 0.6844 0.0451 1.4525 0.044 Uiso 1 1 d . . . H8 H 0.6655 0.2159 1.6068 0.042 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 0.0245(4) 0.0341(4) 0.0319(4) 0.0034(3) 0.0114(3) -0.0051(3) Fe2 0.0205(4) 0.0316(4) 0.0290(4) 0.0058(3) 0.0078(3) -0.0009(3) O1 0.028(2) 0.147(6) 0.056(3) 0.012(3) 0.013(2) -0.023(3) O2 0.106(5) 0.036(3) 0.078(4) 0.018(3) 0.031(3) -0.010(3) O3 0.034(2) 0.062(3) 0.043(2) -0.004(2) 0.0209(18) -0.0103(19) O4 0.079(4) 0.051(3) 0.064(3) 0.022(2) 0.021(3) 0.025(3) O5 0.056(3) 0.046(2) 0.036(2) 0.0025(18) 0.018(2) -0.011(2) C1 0.040(3) 0.038(3) 0.037(3) 0.000(2) 0.020(2) -0.003(2) C2 0.035(3) 0.040(3) 0.043(3) 0.008(2) 0.024(2) 0.006(2) C3 0.017(2) 0.047(3) 0.041(3) 0.014(2) 0.011(2) 0.001(2) C4 0.024(2) 0.044(3) 0.039(3) 0.012(2) 0.008(2) -0.008(2) C5 0.034(3) 0.039(3) 0.032(3) 0.000(2) 0.014(2) -0.006(2) C6 0.037(3) 0.045(3) 0.039(3) 0.010(2) 0.021(2) 0.012(2) C7 0.031(3) 0.058(4) 0.039(3) 0.018(3) 0.013(2) 0.012(3) C8 0.025(3) 0.066(4) 0.032(3) 0.014(3) 0.006(2) 0.003(2) C9 0.028(2) 0.043(3) 0.027(2) 0.006(2) 0.012(2) -0.004(2) C10 0.023(2) 0.038(3) 0.035(3) 0.010(2) 0.018(2) 0.0032(19) C11 0.022(2) 0.035(3) 0.027(2) 0.007(2) 0.0098(18) 0.0032(18) C12 0.029(2) 0.033(3) 0.031(3) 0.009(2) 0.012(2) -0.0008(19) C13 0.038(3) 0.068(4) 0.034(3) 0.003(3) 0.016(2) -0.012(3) C14 0.058(4) 0.032(3) 0.048(3) 0.004(3) 0.022(3) -0.014(3) C15 0.027(2) 0.039(3) 0.033(3) 0.006(2) 0.011(2) -0.002(2) C16 0.040(3) 0.038(3) 0.040(3) 0.008(2) 0.016(2) 0.005(2) C17 0.030(3) 0.035(3) 0.035(3) 0.008(2) 0.010(2) -0.007(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 C14 1.765(6) . ? Fe1 C13 1.783(6) . ? Fe1 C1 2.104(6) . ? Fe1 C2 2.110(5) . ? Fe1 C11 2.119(5) . ? Fe1 C10 2.124(5) . ? Fe1 C9 2.190(5) . ? Fe1 C15 2.450(6) . ? Fe1 Fe2 2.8042(11) . ? Fe2 C17 1.755(6) . ? Fe2 C16 1.787(6) . ? Fe2 C15 1.813(5) . ? Fe2 C4 2.057(5) . ? Fe2 C3 2.156(5) . ? Fe2 C5 2.179(6) . ? O1 C13 1.137(7) . ? O2 C14 1.135(8) . ? O3 C15 1.151(6) . ? O4 C16 1.139(7) . ? O5 C17 1.159(7) . ? C2 C1 1.421(8) . ? C2 C10 1.432(8) . ? C1 C9 1.442(8) . ? C8 C7 1.371(9) . ? C8 C9 1.431(8) . ? C7 C6 1.431(9) . ? C6 C12 1.387(7) . ? C5 C4 1.429(8) . ? C5 C12 1.460(7) . ? C4 C3 1.400(8) . ? C3 C10 1.441(7) . ? C10 C11 1.439(7) . ? C9 C11 1.413(7) . ? C11 C12 1.409(7) . ? 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 C14 Fe1 C13 92.4(3) . . ? C14 Fe1 C1 109.7(3) . . ? C13 Fe1 C1 105.3(3) . . ? C14 Fe1 C2 93.9(3) . . ? C13 Fe1 C2 143.8(3) . . ? C1 Fe1 C2 39.4(2) . . ? C14 Fe1 C11 153.7(3) . . ? C13 Fe1 C11 113.8(3) . . ? C1 Fe1 C11 65.2(2) . . ? C2 Fe1 C11 65.4(2) . . ? C14 Fe1 C10 114.1(3) . . ? C13 Fe1 C10 153.5(3) . . ? C1 Fe1 C10 66.6(2) . . ? C2 Fe1 C10 39.5(2) . . ? C11 Fe1 C10 39.66(18) . . ? C14 Fe1 C9 148.2(3) . . ? C13 Fe1 C9 91.5(3) . . ? C1 Fe1 C9 39.2(2) . . ? C2 Fe1 C9 65.5(2) . . ? C11 Fe1 C9 38.23(19) . . ? C10 Fe1 C9 65.98(19) . . ? C14 Fe1 C15 94.3(2) . . ? C13 Fe1 C15 77.9(2) . . ? C1 Fe1 C15 155.4(2) . . ? C2 Fe1 C15 136.9(2) . . ? C11 Fe1 C15 90.91(19) . . ? C10 Fe1 C15 99.37(19) . . ? C9 Fe1 C15 117.4(2) . . ? C14 Fe1 Fe2 94.9(2) . . ? C13 Fe1 Fe2 117.5(2) . . ? C1 Fe1 Fe2 129.31(16) . . ? C2 Fe1 Fe2 97.45(17) . . ? C11 Fe1 Fe2 73.18(14) . . ? C10 Fe1 Fe2 62.95(14) . . ? C9 Fe1 Fe2 111.08(15) . . ? C15 Fe1 Fe2 39.65(12) . . ? C17 Fe2 C16 89.9(3) . . ? C17 Fe2 C15 96.8(2) . . ? C16 Fe2 C15 101.2(3) . . ? C17 Fe2 C4 94.7(2) . . ? C16 Fe2 C4 122.0(3) . . ? C15 Fe2 C4 135.2(2) . . ? C17 Fe2 C3 125.3(2) . . ? C16 Fe2 C3 95.2(2) . . ? C15 Fe2 C3 134.7(2) . . ? C4 Fe2 C3 38.7(2) . . ? C17 Fe2 C5 92.0(2) . . ? C16 Fe2 C5 161.3(2) . . ? C15 Fe2 C5 97.1(2) . . ? C4 Fe2 C5 39.3(2) . . ? C3 Fe2 C5 68.6(2) . . ? C17 Fe2 Fe1 156.27(17) . . ? C16 Fe2 Fe1 92.37(19) . . ? C15 Fe2 Fe1 59.58(17) . . ? C4 Fe2 Fe1 104.00(16) . . ? C3 Fe2 Fe1 77.98(15) . . ? C5 Fe2 Fe1 93.30(15) . . ? C1 C2 C10 108.8(5) . . ? C1 C2 Fe1 70.1(3) . . ? C10 C2 Fe1 70.8(3) . . ? C2 C1 C9 108.8(5) . . ? C2 C1 Fe1 70.5(3) . . ? C9 C1 Fe1 73.6(3) . . ? C7 C8 C9 117.8(5) . . ? C8 C7 C6 123.8(5) . . ? C12 C6 C7 119.6(5) . . ? C4 C5 C12 120.2(5) . . ? C4 C5 Fe2 65.7(3) . . ? C12 C5 Fe2 104.5(4) . . ? C3 C4 C5 119.4(5) . . ? C3 C4 Fe2 74.4(3) . . ? C5 C4 Fe2 75.0(3) . . ? C4 C3 C10 117.8(5) . . ? C4 C3 Fe2 66.8(3) . . ? C10 C3 Fe2 92.2(3) . . ? C2 C10 C11 105.5(5) . . ? C2 C10 C3 135.5(5) . . ? C11 C10 C3 119.0(5) . . ? C2 C10 Fe1 69.7(3) . . ? C11 C10 Fe1 70.0(3) . . ? C3 C10 Fe1 123.8(4) . . ? C11 C9 C8 117.2(5) . . ? C11 C9 C1 105.8(5) . . ? C8 C9 C1 136.9(5) . . ? C11 C9 Fe1 68.2(3) . . ? C8 C9 Fe1 125.2(4) . . ? C1 C9 Fe1 67.2(3) . . ? C12 C11 C9 125.0(5) . . ? C12 C11 C10 123.8(5) . . ? C9 C11 C10 110.9(5) . . ? C12 C11 Fe1 118.5(4) . . ? C9 C11 Fe1 73.6(3) . . ? C10 C11 Fe1 70.3(3) . . ? C6 C12 C11 116.1(5) . . ? C6 C12 C5 130.3(5) . . ? C11 C12 C5 113.5(5) . . ? O1 C13 Fe1 176.5(6) . . ? O2 C14 Fe1 177.8(6) . . ? O3 C15 Fe2 157.7(5) . . ? O3 C15 Fe1 121.6(4) . . ? Fe2 C15 Fe1 80.8(2) . . ? O4 C16 Fe2 177.7(6) . . ? O5 C17 Fe2 178.2(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 Fe1 Fe2 C17 84.5(5) . . . . ? C13 Fe1 Fe2 C17 -10.8(5) . . . . ? C1 Fe1 Fe2 C17 -155.0(5) . . . . ? C2 Fe1 Fe2 C17 179.1(5) . . . . ? C11 Fe1 Fe2 C17 -119.4(5) . . . . ? C10 Fe1 Fe2 C17 -160.9(5) . . . . ? C9 Fe1 Fe2 C17 -114.3(5) . . . . ? C15 Fe1 Fe2 C17 -6.4(5) . . . . ? C14 Fe1 Fe2 C16 -10.7(3) . . . . ? C13 Fe1 Fe2 C16 -106.0(3) . . . . ? C1 Fe1 Fe2 C16 109.8(3) . . . . ? C2 Fe1 Fe2 C16 83.9(2) . . . . ? C11 Fe1 Fe2 C16 145.4(2) . . . . ? C10 Fe1 Fe2 C16 103.9(2) . . . . ? C9 Fe1 Fe2 C16 150.5(2) . . . . ? C15 Fe1 Fe2 C16 -101.6(3) . . . . ? C14 Fe1 Fe2 C15 90.9(3) . . . . ? C13 Fe1 Fe2 C15 -4.4(3) . . . . ? C1 Fe1 Fe2 C15 -148.6(3) . . . . ? C2 Fe1 Fe2 C15 -174.5(3) . . . . ? C11 Fe1 Fe2 C15 -113.0(2) . . . . ? C10 Fe1 Fe2 C15 -154.5(3) . . . . ? C9 Fe1 Fe2 C15 -107.9(3) . . . . ? C14 Fe1 Fe2 C4 -134.5(3) . . . . ? C13 Fe1 Fe2 C4 130.2(3) . . . . ? C1 Fe1 Fe2 C4 -14.0(3) . . . . ? C2 Fe1 Fe2 C4 -39.9(2) . . . . ? C11 Fe1 Fe2 C4 21.6(2) . . . . ? C10 Fe1 Fe2 C4 -19.9(2) . . . . ? C9 Fe1 Fe2 C4 26.7(2) . . . . ? C15 Fe1 Fe2 C4 134.6(3) . . . . ? C14 Fe1 Fe2 C3 -105.5(3) . . . . ? C13 Fe1 Fe2 C3 159.1(3) . . . . ? C1 Fe1 Fe2 C3 15.0(3) . . . . ? C2 Fe1 Fe2 C3 -10.9(2) . . . . ? C11 Fe1 Fe2 C3 50.5(2) . . . . ? C10 Fe1 Fe2 C3 9.0(2) . . . . ? C9 Fe1 Fe2 C3 55.7(2) . . . . ? C15 Fe1 Fe2 C3 163.5(3) . . . . ? C14 Fe1 Fe2 C5 -172.8(3) . . . . ? C13 Fe1 Fe2 C5 91.8(3) . . . . ? C1 Fe1 Fe2 C5 -52.3(3) . . . . ? C2 Fe1 Fe2 C5 -78.2(2) . . . . ? C11 Fe1 Fe2 C5 -16.7(2) . . . . ? C10 Fe1 Fe2 C5 -58.3(2) . . . . ? C9 Fe1 Fe2 C5 -11.6(2) . . . . ? C15 Fe1 Fe2 C5 96.3(3) . . . . ? C14 Fe1 C2 C1 -116.7(4) . . . . ? C13 Fe1 C2 C1 -17.1(6) . . . . ? C11 Fe1 C2 C1 80.3(3) . . . . ? C10 Fe1 C2 C1 119.4(5) . . . . ? C9 Fe1 C2 C1 38.1(3) . . . . ? C15 Fe1 C2 C1 142.7(3) . . . . ? Fe2 Fe1 C2 C1 147.9(3) . . . . ? C14 Fe1 C2 C10 124.0(4) . . . . ? C13 Fe1 C2 C10 -136.5(5) . . . . ? C1 Fe1 C2 C10 -119.4(5) . . . . ? C11 Fe1 C2 C10 -39.1(3) . . . . ? C9 Fe1 C2 C10 -81.3(3) . . . . ? C15 Fe1 C2 C10 23.3(5) . . . . ? Fe2 Fe1 C2 C10 28.5(3) . . . . ? C10 C2 C1 C9 -3.8(6) . . . . ? Fe1 C2 C1 C9 -64.2(4) . . . . ? C10 C2 C1 Fe1 60.4(4) . . . . ? C14 Fe1 C1 C2 71.3(4) . . . . ? C13 Fe1 C1 C2 169.6(4) . . . . ? C11 Fe1 C1 C2 -80.8(3) . . . . ? C10 Fe1 C1 C2 -37.2(3) . . . . ? C9 Fe1 C1 C2 -117.4(5) . . . . ? C15 Fe1 C1 C2 -95.9(6) . . . . ? Fe2 Fe1 C1 C2 -43.0(4) . . . . ? C14 Fe1 C1 C9 -171.4(3) . . . . ? C13 Fe1 C1 C9 -73.0(4) . . . . ? C2 Fe1 C1 C9 117.4(5) . . . . ? C11 Fe1 C1 C9 36.6(3) . . . . ? C10 Fe1 C1 C9 80.2(3) . . . . ? C15 Fe1 C1 C9 21.4(7) . . . . ? Fe2 Fe1 C1 C9 74.4(3) . . . . ? C9 C8 C7 C6 4.6(9) . . . . ? C8 C7 C6 C12 -2.1(9) . . . . ? C17 Fe2 C5 C4 -94.9(4) . . . . ? C16 Fe2 C5 C4 0.8(9) . . . . ? C15 Fe2 C5 C4 167.9(3) . . . . ? C3 Fe2 C5 C4 32.5(3) . . . . ? Fe1 Fe2 C5 C4 108.2(3) . . . . ? C17 Fe2 C5 C12 148.1(4) . . . . ? C16 Fe2 C5 C12 -116.2(7) . . . . ? C15 Fe2 C5 C12 51.0(4) . . . . ? C4 Fe2 C5 C12 -117.0(5) . . . . ? C3 Fe2 C5 C12 -84.5(4) . . . . ? Fe1 Fe2 C5 C12 -8.8(3) . . . . ? C12 C5 C4 C3 31.2(8) . . . . ? Fe2 C5 C4 C3 -62.0(5) . . . . ? C12 C5 C4 Fe2 93.1(5) . . . . ? C17 Fe2 C4 C3 -145.5(3) . . . . ? C16 Fe2 C4 C3 -52.7(4) . . . . ? C15 Fe2 C4 C3 109.9(4) . . . . ? C5 Fe2 C4 C3 127.0(5) . . . . ? Fe1 Fe2 C4 C3 49.2(3) . . . . ? C17 Fe2 C4 C5 87.5(3) . . . . ? C16 Fe2 C4 C5 -179.7(3) . . . . ? C15 Fe2 C4 C5 -17.1(5) . . . . ? C3 Fe2 C4 C5 -127.0(5) . . . . ? Fe1 Fe2 C4 C5 -77.8(3) . . . . ? C5 C4 C3 C10 -17.4(8) . . . . ? Fe2 C4 C3 C10 -79.7(4) . . . . ? C5 C4 C3 Fe2 62.2(5) . . . . ? C17 Fe2 C3 C4 43.7(4) . . . . ? C16 Fe2 C3 C4 137.3(3) . . . . ? C15 Fe2 C3 C4 -111.2(4) . . . . ? C5 Fe2 C3 C4 -32.9(3) . . . . ? Fe1 Fe2 C3 C4 -131.3(3) . . . . ? C17 Fe2 C3 C10 163.2(3) . . . . ? C16 Fe2 C3 C10 -103.2(4) . . . . ? C15 Fe2 C3 C10 8.2(5) . . . . ? C4 Fe2 C3 C10 119.5(5) . . . . ? C5 Fe2 C3 C10 86.5(3) . . . . ? Fe1 Fe2 C3 C10 -11.9(3) . . . . ? C1 C2 C10 C11 1.3(6) . . . . ? Fe1 C2 C10 C11 61.3(3) . . . . ? C1 C2 C10 C3 -178.0(5) . . . . ? Fe1 C2 C10 C3 -118.0(6) . . . . ? C1 C2 C10 Fe1 -59.9(4) . . . . ? C4 C3 C10 C2 178.4(6) . . . . ? Fe2 C3 C10 C2 113.6(6) . . . . ? C4 C3 C10 C11 -0.8(7) . . . . ? Fe2 C3 C10 C11 -65.6(5) . . . . ? C4 C3 C10 Fe1 83.5(6) . . . . ? Fe2 C3 C10 Fe1 18.7(4) . . . . ? C14 Fe1 C10 C2 -65.0(4) . . . . ? C13 Fe1 C10 C2 114.2(6) . . . . ? C1 Fe1 C10 C2 37.1(3) . . . . ? C11 Fe1 C10 C2 115.9(4) . . . . ? C9 Fe1 C10 C2 80.0(3) . . . . ? C15 Fe1 C10 C2 -164.1(3) . . . . ? Fe2 Fe1 C10 C2 -147.9(3) . . . . ? C14 Fe1 C10 C11 179.1(3) . . . . ? C13 Fe1 C10 C11 -1.7(7) . . . . ? C1 Fe1 C10 C11 -78.9(3) . . . . ? C2 Fe1 C10 C11 -115.9(4) . . . . ? C9 Fe1 C10 C11 -35.9(3) . . . . ? C15 Fe1 C10 C11 80.0(3) . . . . ? Fe2 Fe1 C10 C11 96.1(3) . . . . ? C14 Fe1 C10 C3 66.9(5) . . . . ? C13 Fe1 C10 C3 -113.9(6) . . . . ? C1 Fe1 C10 C3 169.0(5) . . . . ? C2 Fe1 C10 C3 131.9(6) . . . . ? C11 Fe1 C10 C3 -112.2(6) . . . . ? C9 Fe1 C10 C3 -148.1(5) . . . . ? C15 Fe1 C10 C3 -32.2(5) . . . . ? Fe2 Fe1 C10 C3 -16.0(4) . . . . ? C7 C8 C9 C11 -0.8(8) . . . . ? C7 C8 C9 C1 -175.6(6) . . . . ? C7 C8 C9 Fe1 -82.2(7) . . . . ? C2 C1 C9 C11 4.7(6) . . . . ? Fe1 C1 C9 C11 -57.5(3) . . . . ? C2 C1 C9 C8 179.9(6) . . . . ? Fe1 C1 C9 C8 117.8(7) . . . . ? C2 C1 C9 Fe1 62.2(4) . . . . ? C14 Fe1 C9 C11 134.6(5) . . . . ? C13 Fe1 C9 C11 -128.2(4) . . . . ? C1 Fe1 C9 C11 119.1(4) . . . . ? C2 Fe1 C9 C11 80.8(3) . . . . ? C10 Fe1 C9 C11 37.2(3) . . . . ? C15 Fe1 C9 C11 -51.1(3) . . . . ? Fe2 Fe1 C9 C11 -7.9(3) . . . . ? C14 Fe1 C9 C8 -116.8(6) . . . . ? C13 Fe1 C9 C8 -19.6(5) . . . . ? C1 Fe1 C9 C8 -132.3(6) . . . . ? C2 Fe1 C9 C8 -170.6(6) . . . . ? C11 Fe1 C9 C8 108.6(6) . . . . ? C10 Fe1 C9 C8 145.8(6) . . . . ? C15 Fe1 C9 C8 57.6(5) . . . . ? Fe2 Fe1 C9 C8 100.7(5) . . . . ? C14 Fe1 C9 C1 15.5(6) . . . . ? C13 Fe1 C9 C1 112.7(4) . . . . ? C2 Fe1 C9 C1 -38.3(3) . . . . ? C11 Fe1 C9 C1 -119.1(4) . . . . ? C10 Fe1 C9 C1 -81.8(3) . . . . ? C15 Fe1 C9 C1 -170.1(3) . . . . ? Fe2 Fe1 C9 C1 -127.0(3) . . . . ? C8 C9 C11 C12 -5.8(8) . . . . ? C1 C9 C11 C12 170.5(5) . . . . ? Fe1 C9 C11 C12 113.7(5) . . . . ? C8 C9 C11 C10 179.7(5) . . . . ? C1 C9 C11 C10 -3.9(6) . . . . ? Fe1 C9 C11 C10 -60.8(4) . . . . ? C8 C9 C11 Fe1 -119.5(5) . . . . ? C1 C9 C11 Fe1 56.8(4) . . . . ? C2 C10 C11 C12 -172.8(5) . . . . ? C3 C10 C11 C12 6.6(7) . . . . ? Fe1 C10 C11 C12 -111.8(5) . . . . ? C2 C10 C11 C9 1.7(6) . . . . ? C3 C10 C11 C9 -178.9(4) . . . . ? Fe1 C10 C11 C9 62.7(4) . . . . ? C2 C10 C11 Fe1 -61.1(3) . . . . ? C3 C10 C11 Fe1 118.4(4) . . . . ? C14 Fe1 C11 C12 116.6(6) . . . . ? C13 Fe1 C11 C12 -62.3(5) . . . . ? C1 Fe1 C11 C12 -158.8(5) . . . . ? C2 Fe1 C11 C12 157.6(5) . . . . ? C10 Fe1 C11 C12 118.6(5) . . . . ? C9 Fe1 C11 C12 -121.4(5) . . . . ? C15 Fe1 C11 C12 14.9(4) . . . . ? Fe2 Fe1 C11 C12 50.9(4) . . . . ? C14 Fe1 C11 C9 -122.0(6) . . . . ? C13 Fe1 C11 C9 59.1(4) . . . . ? C1 Fe1 C11 C9 -37.5(3) . . . . ? C2 Fe1 C11 C9 -81.0(3) . . . . ? C10 Fe1 C11 C9 -120.1(4) . . . . ? C15 Fe1 C11 C9 136.3(3) . . . . ? Fe2 Fe1 C11 C9 172.3(3) . . . . ? C14 Fe1 C11 C10 -1.9(7) . . . . ? C13 Fe1 C11 C10 179.2(3) . . . . ? C1 Fe1 C11 C10 82.6(3) . . . . ? C2 Fe1 C11 C10 39.0(3) . . . . ? C9 Fe1 C11 C10 120.1(4) . . . . ? C15 Fe1 C11 C10 -103.7(3) . . . . ? Fe2 Fe1 C11 C10 -67.7(3) . . . . ? C7 C6 C12 C11 -4.2(8) . . . . ? C7 C6 C12 C5 171.5(5) . . . . ? C9 C11 C12 C6 8.3(8) . . . . ? C10 C11 C12 C6 -178.0(5) . . . . ? Fe1 C11 C12 C6 97.6(5) . . . . ? C9 C11 C12 C5 -168.1(5) . . . . ? C10 C11 C12 C5 5.7(7) . . . . ? Fe1 C11 C12 C5 -78.8(5) . . . . ? C4 C5 C12 C6 160.1(6) . . . . ? Fe2 C5 C12 C6 -129.8(5) . . . . ? C4 C5 C12 C11 -24.2(7) . . . . ? Fe2 C5 C12 C11 45.9(5) . . . . ? C14 Fe1 C13 O1 82(12) . . . . ? C1 Fe1 C13 O1 -29(12) . . . . ? C2 Fe1 C13 O1 -18(12) . . . . ? C11 Fe1 C13 O1 -98(12) . . . . ? C10 Fe1 C13 O1 -97(12) . . . . ? C9 Fe1 C13 O1 -66(12) . . . . ? C15 Fe1 C13 O1 176(100) . . . . ? Fe2 Fe1 C13 O1 179(100) . . . . ? C13 Fe1 C14 O2 -105(17) . . . . ? C1 Fe1 C14 O2 2(17) . . . . ? C2 Fe1 C14 O2 39(17) . . . . ? C11 Fe1 C14 O2 76(17) . . . . ? C10 Fe1 C14 O2 75(17) . . . . ? C9 Fe1 C14 O2 -8(17) . . . . ? C15 Fe1 C14 O2 177(100) . . . . ? Fe2 Fe1 C14 O2 137(17) . . . . ? C17 Fe2 C15 O3 -3.7(14) . . . . ? C16 Fe2 C15 O3 -95.0(14) . . . . ? C4 Fe2 C15 O3 100.0(13) . . . . ? C3 Fe2 C15 O3 155.9(12) . . . . ? C5 Fe2 C15 O3 89.2(14) . . . . ? Fe1 Fe2 C15 O3 178.9(14) . . . . ? C17 Fe2 C15 Fe1 177.4(2) . . . . ? C16 Fe2 C15 Fe1 86.1(2) . . . . ? C4 Fe2 C15 Fe1 -78.8(3) . . . . ? C3 Fe2 C15 Fe1 -22.9(4) . . . . ? C5 Fe2 C15 Fe1 -89.68(18) . . . . ? C14 Fe1 C15 O3 88.1(6) . . . . ? C13 Fe1 C15 O3 -3.5(5) . . . . ? C1 Fe1 C15 O3 -104.0(7) . . . . ? C2 Fe1 C15 O3 -171.4(5) . . . . ? C11 Fe1 C15 O3 -117.7(5) . . . . ? C10 Fe1 C15 O3 -156.6(5) . . . . ? C9 Fe1 C15 O3 -88.9(5) . . . . ? Fe2 Fe1 C15 O3 -179.5(6) . . . . ? C14 Fe1 C15 Fe2 -92.4(3) . . . . ? C13 Fe1 C15 Fe2 176.0(3) . . . . ? C1 Fe1 C15 Fe2 75.5(5) . . . . ? C2 Fe1 C15 Fe2 8.1(4) . . . . ? C11 Fe1 C15 Fe2 61.8(2) . . . . ? C10 Fe1 C15 Fe2 22.9(2) . . . . ? C9 Fe1 C15 Fe2 90.6(2) . . . . ? C17 Fe2 C16 O4 -24(15) . . . . ? C15 Fe2 C16 O4 73(15) . . . . ? C4 Fe2 C16 O4 -120(15) . . . . ? C3 Fe2 C16 O4 -150(15) . . . . ? C5 Fe2 C16 O4 -120(15) . . . . ? Fe1 Fe2 C16 O4 132(15) . . . . ? C16 Fe2 C17 O5 107(16) . . . . ? C15 Fe2 C17 O5 6(16) . . . . ? C4 Fe2 C17 O5 -131(16) . . . . ? C3 Fe2 C17 O5 -157(16) . . . . ? C5 Fe2 C17 O5 -92(16) . . . . ? Fe1 Fe2 C17 O5 11(16) . . . . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.520 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.133 #===END data_2-B _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H10 Fe2 O5, C3 H3' _chemical_formula_sum 'C24 H13 Fe2 O5' _chemical_formula_weight 493.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 'monoclinic' _symmetry_space_group_name_H-M 'P21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.7522(19) _cell_length_b 11.951(2) _cell_length_c 13.4917(16) _cell_angle_alpha 90.00 _cell_angle_beta 103.053(10) _cell_angle_gamma 90.00 _cell_volume 2003.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.6 _cell_measurement_theta_max 15.0 _exptl_crystal_description 'Platelet' _exptl_crystal_colour 'Red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 1.483 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.524 _exptl_absorpt_correction_T_max 0.744 _exptl_absorpt_process_details ; North, Phillips & Mathews, 1968 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.90 _diffrn_reflns_number 4810 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0835 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4608 _reflns_number_gt 2702 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DSC/AFC Diffractometer Control' _computing_cell_refinement 'DSC/AFC Diffractometer Control' _computing_data_reduction ; teXsan for Wi ndows version 1.06 (MSC, 1997-1999) ; _computing_structure_solution ; DIRDIF94 PATTY (Beurskens, 1994) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP III (Farrujia, 1998)' _computing_publication_material 'SHELXL-97/2 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4608 _refine_ls_number_parameters 332 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1147 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1336 _refine_ls_wR_factor_gt 0.1109 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.003 _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 0.49853(4) 0.16149(5) 0.77441(4) 0.02985(15) Uani 1 1 d . . . Fe2 Fe 0.59008(4) -0.03755(5) 0.72019(4) 0.03298(16) Uani 1 1 d . . . O1 O 0.3021(2) 0.1900(3) 0.6184(2) 0.0516(8) Uani 1 1 d . . . O2 O 0.6071(3) 0.3372(3) 0.6876(3) 0.0687(11) Uani 1 1 d . . . O3 O 0.3977(3) -0.0181(3) 0.5552(2) 0.0511(8) Uani 1 1 d . . . O4 O 0.7467(3) 0.1157(3) 0.6660(3) 0.0727(12) Uani 1 1 d . . . O5 O 0.6662(3) -0.2237(3) 0.6162(3) 0.0683(10) Uani 1 1 d . . . C1 C 0.4913(3) 0.2225(4) 0.9192(3) 0.0381(9) Uani 1 1 d . . . C2 C 0.5960(3) 0.1795(4) 0.9208(3) 0.0401(10) Uani 1 1 d . . . C3 C 0.6594(4) -0.0233(4) 0.8803(3) 0.0443(11) Uani 1 1 d . . . C4 C 0.6171(4) -0.1283(4) 0.8527(3) 0.0468(11) Uani 1 1 d . . . C5 C 0.5035(4) -0.1411(4) 0.8107(3) 0.0396(9) Uani 1 1 d . . . C6 C 0.3187(4) -0.0745(4) 0.8280(3) 0.0389(9) Uani 1 1 d . . . C7 C 0.2554(3) 0.0159(3) 0.8563(3) 0.0354(9) Uani 1 1 d . . . C8 C 0.2997(3) 0.1226(3) 0.8862(3) 0.0315(8) Uani 1 1 d . . . C9 C 0.4150(3) 0.1340(3) 0.8943(3) 0.0309(8) Uani 1 1 d . . . C10 C 0.5865(3) 0.0638(4) 0.8959(3) 0.0349(9) Uani 1 1 d . . . C11 C 0.4731(3) 0.0395(3) 0.8775(3) 0.0290(7) Uani 1 1 d . . . C12 C 0.4260(3) -0.0646(3) 0.8392(3) 0.0325(8) Uani 1 1 d . . . C13 C 0.3804(3) 0.1772(3) 0.6788(3) 0.0364(9) Uani 1 1 d . . . C14 C 0.5655(3) 0.2662(4) 0.7205(3) 0.0430(10) Uani 1 1 d . . . C15 C 0.4709(3) -0.0166(3) 0.6222(3) 0.0368(9) Uani 1 1 d . . . C16 C 0.6838(4) 0.0587(4) 0.6868(3) 0.0487(11) Uani 1 1 d . . . C17 C 0.6389(3) -0.1505(4) 0.6586(3) 0.0442(10) Uani 1 1 d . . . C18 C 0.1463(4) -0.0011(4) 0.8546(3) 0.0479(11) Uani 1 1 d . . . C19 C 0.0844(4) 0.0815(5) 0.8839(4) 0.0553(12) Uani 1 1 d . . . C20 C 0.1290(4) 0.1867(5) 0.9129(4) 0.0496(12) Uani 1 1 d . . . C21 C 0.2354(3) 0.2066(4) 0.9135(3) 0.0400(9) Uani 1 1 d . . . C22 C -0.0284(4) 0.0289(4) 0.5893(4) 0.0445(10) Uani 1 1 d . . . C23 C 0.0771(4) 0.0353(4) 0.5830(4) 0.0478(11) Uani 1 1 d . . . C24 C 0.1058(4) 0.0073(4) 0.4931(4) 0.0449(10) Uani 1 1 d . . . H1 H 0.473(3) 0.286(4) 0.930(3) 0.028(10) Uiso 1 1 d . . . H2 H 0.655(3) 0.220(3) 0.935(3) 0.024(9) Uiso 1 1 d . . . H3 H 0.727(4) -0.013(4) 0.898(4) 0.056(15) Uiso 1 1 d . . . H4 H 0.660(4) -0.191(4) 0.852(4) 0.057(14) Uiso 1 1 d . . . H5 H 0.483(3) -0.205(4) 0.788(3) 0.032(11) Uiso 1 1 d . . . H6 H 0.290(3) -0.133(4) 0.807(3) 0.032(11) Uiso 1 1 d . . . H7 H 0.109(3) -0.066(4) 0.824(3) 0.046(13) Uiso 1 1 d . . . H8 H 0.010(4) 0.072(5) 0.879(4) 0.069(16) Uiso 1 1 d . . . H9 H 0.090(3) 0.240(3) 0.939(3) 0.030(10) Uiso 1 1 d . . . H10 H 0.266(3) 0.267(4) 0.937(3) 0.035(12) Uiso 1 1 d . . . H11 H -0.048(3) 0.043(3) 0.643(3) 0.025(10) Uiso 1 1 d . . . H12 H 0.126(4) 0.062(5) 0.633(4) 0.070(17) Uiso 1 1 d . . . H13 H 0.171(4) 0.006(5) 0.491(4) 0.066(17) 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 0.0298(3) 0.0313(3) 0.0285(3) 0.0005(2) 0.0067(2) -0.0016(2) Fe2 0.0320(3) 0.0396(3) 0.0279(3) -0.0005(2) 0.0080(2) 0.0053(2) O1 0.0423(17) 0.054(2) 0.0501(18) -0.0046(15) -0.0064(15) 0.0055(15) O2 0.055(2) 0.065(2) 0.089(3) 0.029(2) 0.022(2) -0.0109(19) O3 0.0456(18) 0.063(2) 0.0410(17) -0.0076(15) 0.0019(14) 0.0118(16) O4 0.067(2) 0.071(3) 0.093(3) -0.024(2) 0.048(2) -0.028(2) O5 0.069(2) 0.073(3) 0.066(2) -0.018(2) 0.0234(19) 0.019(2) C1 0.045(2) 0.038(2) 0.033(2) -0.0106(17) 0.0112(17) -0.0050(19) C2 0.034(2) 0.052(3) 0.032(2) -0.0080(18) 0.0020(16) -0.0130(19) C3 0.033(2) 0.071(3) 0.0257(19) 0.002(2) 0.0003(16) 0.016(2) C4 0.059(3) 0.050(3) 0.033(2) 0.0074(19) 0.012(2) 0.022(2) C5 0.057(3) 0.027(2) 0.037(2) 0.0003(17) 0.0138(19) 0.0055(19) C6 0.052(3) 0.033(2) 0.036(2) -0.0024(18) 0.0174(18) -0.012(2) C7 0.036(2) 0.043(2) 0.0290(18) 0.0014(16) 0.0113(16) -0.0029(17) C8 0.036(2) 0.037(2) 0.0232(16) 0.0037(15) 0.0093(14) 0.0019(16) C9 0.0347(19) 0.036(2) 0.0232(16) -0.0006(15) 0.0081(14) 0.0012(16) C10 0.0332(19) 0.050(2) 0.0200(16) -0.0002(15) 0.0021(14) 0.0005(18) C11 0.0309(18) 0.0335(19) 0.0225(16) 0.0012(14) 0.0061(14) 0.0013(16) C12 0.044(2) 0.0298(19) 0.0249(17) 0.0027(14) 0.0105(16) -0.0035(17) C13 0.039(2) 0.034(2) 0.038(2) -0.0024(17) 0.0131(18) -0.0028(17) C14 0.033(2) 0.051(3) 0.045(2) 0.009(2) 0.0080(18) -0.0005(19) C15 0.039(2) 0.039(2) 0.035(2) 0.0007(17) 0.0143(17) 0.0061(18) C16 0.047(3) 0.062(3) 0.040(2) -0.010(2) 0.016(2) -0.005(2) C17 0.040(2) 0.055(3) 0.039(2) -0.003(2) 0.0116(18) 0.009(2) C18 0.038(2) 0.058(3) 0.047(2) 0.003(2) 0.0067(19) -0.011(2) C19 0.030(2) 0.077(4) 0.060(3) 0.009(3) 0.012(2) 0.002(2) C20 0.039(2) 0.065(3) 0.048(3) 0.010(2) 0.016(2) 0.017(2) C21 0.039(2) 0.044(2) 0.037(2) 0.0029(19) 0.0093(18) 0.008(2) C22 0.050(3) 0.043(3) 0.043(2) 0.001(2) 0.016(2) 0.002(2) C23 0.040(2) 0.053(3) 0.046(2) 0.004(2) -0.0021(19) -0.006(2) C24 0.032(2) 0.049(3) 0.054(3) 0.012(2) 0.010(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are esti mated 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 C13 1.758(4) . ? Fe1 C14 1.762(4) . ? Fe1 C11 2.090(4) . ? Fe1 C2 2.094(4) . ? Fe1 C1 2.107(4) . ? Fe1 C10 2.116(4) . ? Fe1 C9 2.153(3) . ? Fe1 Fe2 2.8182(8) . ? Fe2 C17 1.771(5) . ? Fe2 C16 1.788(5) . ? Fe2 C15 1.792(4) . ? Fe2 C4 2.052(4) . ? Fe2 C3 2.149(4) . ? Fe2 C5 2.203(4) . ? O1 C13 1.148(5) . ? O2 C14 1.143(5) . ? O3 C15 1.144(5) . ? O4 C16 1.135(5) . ? O5 C17 1.142(5) . ? C1 C9 1.424(5) . ? C1 C2 1.427(6) . ? C2 C10 1.421(6) . ? C3 C4 1.383(7) . ? C3 C10 1.443(6) . ? C4 C5 1.440(7) . ? C5 C12 1.460(5) . ? C6 C12 1.348(6) . ? C6 C7 1.450(6) . ? C7 C18 1.401(5) . ? C7 C8 1.416(6) . ? C8 C21 1.397(6) . ? C8 C9 1.456(5) . ? C9 C11 1.397(5) . ? C10 C11 1.440(5) . ? C11 C12 1.427(5) . ? C18 C19 1.377(7) . ? C19 C20 1.399(7) . ? C20 C21 1.376(6) . ? C22 C23 1.370(6) . ? C22 C24 1.379(6) 3_556 ? C23 C24 1.383(7) . ? C24 C22 1.379(6) 3_556 ? 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 C13 Fe1 C14 92.07(18) . . ? C13 Fe1 C11 109.07(16) . . ? C14 Fe1 C11 158.83(17) . . ? C13 Fe1 C2 155.39(18) . . ? C14 Fe1 C2 94.40(19) . . ? C11 Fe1 C2 65.93(16) . . ? C13 Fe1 C1 115.72(18) . . ? C14 Fe1 C1 105.31(19) . . ? C11 Fe1 C1 65.07(16) . . ? C2 Fe1 C1 39.71(16) . . ? C13 Fe1 C10 147.53(17) . . ? C14 Fe1 C10 119.35(17) . . ? C11 Fe1 C10 40.04(14) . . ? C2 Fe1 C10 39.46(16) . . ? C1 Fe1 C10 66.37(17) . . ? C13 Fe1 C9 94.63(16) . . ? C14 Fe1 C9 141.86(18) . . ? C11 Fe1 C9 38.40(14) . . ? C2 Fe1 C9 66.16(16) . . ? C1 Fe1 C9 39.05(15) . . ? C10 Fe1 C9 66.38(14) . . ? C13 Fe1 Fe2 103.65(13) . . ? C14 Fe1 Fe2 102.97(15) . . ? C11 Fe1 Fe2 73.72(10) . . ? C2 Fe1 Fe2 97.99(13) . . ? C1 Fe1 Fe2 129.81(13) . . ? C10 Fe1 Fe2 63.72(11) . . ? C9 Fe1 Fe2 111.74(10) . . ? C17 Fe2 C16 92.7(2) . . ? C17 Fe2 C15 95.15(19) . . ? C16 Fe2 C15 103.2(2) . . ? C17 Fe2 C4 89.91(19) . . ? C16 Fe2 C4 124.7(2) . . ? C15 Fe2 C4 131.59(19) . . ? C17 Fe2 C3 115.07(19) . . ? C16 Fe2 C3 93.2(2) . . ? C15 Fe2 C3 144.95(17) . . ? C4 Fe2 C3 38.36(19) . . ? C17 Fe2 C5 96.06(19) . . ? C16 Fe2 C5 161.52(19) . . ? C15 Fe2 C5 92.27(18) . . ? C4 Fe2 C5 39.35(18) . . ? C3 Fe2 C5 68.34(19) . . ? C17 Fe2 Fe1 167.33(15) . . ? C16 Fe2 Fe1 82.05(15) . . ? C15 Fe2 Fe1 75.04(13) . . ? C4 Fe2 Fe1 102.58(13) . . ? C3 Fe2 Fe1 76.87(12) . . ? C5 Fe2 Fe1 92.37(11) . . ? C9 C1 C2 108.8(4) . . ? C9 C1 Fe1 72.3(2) . . ? C2 C1 Fe1 69.7(2) . . ? C10 C2 C1 108.5(4) . . ? C10 C2 Fe1 71.1(2) . . ? C1 C2 Fe1 70.6(2) . . ? C4 C3 C10 117.9(4) . . ? C4 C3 Fe2 67.0(2) . . ? C10 C3 Fe2 94.1(2) . . ? C3 C4 C5 120.0(4) . . ? C3 C4 Fe2 74.6(3) . . ? C5 C4 Fe2 76.0(2) . . ? C4 C5 C12 120.7(4) . . ? C4 C5 Fe2 64.7(2) . . ? C12 C5 Fe2 104.4(3) . . ? C12 C6 C7 121.1(4) . . ? C18 C7 C8 117.8(4) . . ? C18 C7 C6 119.8(4) . . ? C8 C7 C6 122.4(3) . . ? C21 C8 C7 120.1(4) . . ? C21 C8 C9 123.7(4) . . ? C7 C8 C9 115.9(3) . . ? C11 C9 C1 106.3(3) . . ? C11 C9 C8 118.4(3) . . ? C1 C9 C8 135.4(4) . . ? C11 C9 Fe1 68.3(2) . . ? C1 C9 Fe1 68.7(2) . . ? C8 C9 Fe1 128.3(2) . . ? C2 C10 C11 105.4(3) . . ? C2 C10 C3 135.5(4) . . ? C11 C10 C3 119.0(4) . . ? C2 C10 Fe1 69.4(2) . . ? C11 C10 Fe1 69.0(2) . . ? C3 C10 Fe1 122.1(3) . . ? C9 C11 C12 124.7(3) . . ? C9 C11 C10 110.9(3) . . ? C12 C11 C10 124.2(3) . . ? C9 C11 Fe1 73.3(2) . . ? C12 C11 Fe1 118.9(2) . . ? C10 C11 Fe1 70.9(2) . . ? C6 C12 C11 116.8(4) . . ? C6 C12 C5 130.3(4) . . ? C11 C12 C5 112.8(3) . . ? O1 C13 Fe1 177.7(4) . . ? O2 C14 Fe1 177.3(4) . . ? O3 C15 Fe2 170.3(4) . . ? O4 C16 Fe2 176.7(5) . . ? O5 C17 Fe2 177.1(4) . . ? C19 C18 C7 121.6(5) . . ? C18 C19 C20 120.1(4) . . ? C21 C20 C19 119.7(5) . . ? C20 C21 C8 120.7(5) . . ? C23 C22 C24 120.1(4) . 3_556 ? C22 C23 C24 119.9(4) . . ? C22 C24 C23 120.0(4) 3_556 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 Fe1 Fe2 C17 41.6(7) . . . . ? C14 Fe1 Fe2 C17 -53.8(7) . . . . ? C11 Fe1 Fe2 C17 147.8(7) . . . . ? C2 Fe1 Fe2 C17 -150.2(7) . . . . ? C1 Fe1 Fe2 C17 -176.8(7) . . . . ? C10 Fe1 Fe2 C17 -170.4(7) . . . . ? C9 Fe1 Fe2 C17 142.3(7) . . . . ? C13 Fe1 Fe2 C16 107.5(2) . . . . ? C14 Fe1 Fe2 C16 12.1(2) . . . . ? C11 Fe1 Fe2 C16 -146.27(18) . . . . ? C2 Fe1 Fe2 C16 -84.32(19) . . . . ? C1 Fe1 Fe2 C16 -110.9(2) . . . . ? C10 Fe1 Fe2 C16 -104.46(19) . . . . ? C9 Fe1 Fe2 C16 -151.77(18) . . . . ? C13 Fe1 Fe2 C15 1.53(18) . . . . ? C14 Fe1 Fe2 C15 -93.87(19) . . . . ? C11 Fe1 Fe2 C15 107.75(17) . . . . ? C2 Fe1 Fe2 C15 169.71(18) . . . . ? C1 Fe1 Fe2 C15 143.1(2) . . . . ? C10 Fe1 Fe2 C15 149.57(18) . . . . ? C9 Fe1 Fe2 C15 102.26(17) . . . . ? C13 Fe1 Fe2 C4 -128.6(2) . . . . ? C14 Fe1 Fe2 C4 136.0(2) . . . . ? C11 Fe1 Fe2 C4 -22.37(18) . . . . ? C2 Fe1 Fe2 C4 39.6(2) . . . . ? C1 Fe1 Fe2 C4 13.0(2) . . . . ? C10 Fe1 Fe2 C4 19.4(2) . . . . ? C9 Fe1 Fe2 C4 -27.86(19) . . . . ? C13 Fe1 Fe2 C3 -157.30(19) . . . . ? C14 Fe1 Fe2 C3 107.3(2) . . . . ? C11 Fe1 Fe2 C3 -51.08(17) . . . . ? C2 Fe1 Fe2 C3 10.88(18) . . . . ? C1 Fe1 Fe2 C3 -15.7(2) . . . . ? C10 Fe1 Fe2 C3 -9.26(18) . . . . ? C9 Fe1 Fe2 C3 -56.57(18) . . . . ? C13 Fe1 Fe2 C5 -90.19(18) . . . . ? C14 Fe1 Fe2 C5 174.41(19) . . . . ? C11 Fe1 Fe2 C5 16.03(16) . . . . ? C2 Fe1 Fe2 C5 77.99(17) . . . . ? C1 Fe1 Fe2 C5 51.4(2) . . . . ? C10 Fe1 Fe2 C5 57.85(17) . . . . ? C9 Fe1 Fe2 C5 10.54(16) . . . . ? C13 Fe1 C1 C9 63.1(3) . . . . ? C14 Fe1 C1 C9 163.1(2) . . . . ? C11 Fe1 C1 C9 -37.0(2) . . . . ? C2 Fe1 C1 C9 -118.7(4) . . . . ? C10 Fe1 C1 C9 -81.1(3) . . . . ? Fe2 Fe1 C1 C9 -74.8(3) . . . . ? C13 Fe1 C1 C2 -178.2(3) . . . . ? C14 Fe1 C1 C2 -78.2(3) . . . . ? C11 Fe1 C1 C2 81.7(3) . . . . ? C10 Fe1 C1 C2 37.6(3) . . . . ? C9 Fe1 C1 C2 118.7(4) . . . . ? Fe2 Fe1 C1 C2 43.9(3) . . . . ? C9 C1 C2 C10 0.6(5) . . . . ? Fe1 C1 C2 C10 -61.3(3) . . . . ? C9 C1 C2 Fe1 62.0(3) . . . . ? C13 Fe1 C2 C10 122.4(4) . . . . ? C14 Fe1 C2 C10 -132.8(3) . . . . ? C11 Fe1 C2 C10 39.0(2) . . . . ? C1 Fe1 C2 C10 118.4(4) . . . . ? C9 Fe1 C2 C10 81.2(2) . . . . ? Fe2 Fe1 C2 C10 -29.1(2) . . . . ? C13 Fe1 C2 C1 4.0(6) . . . . ? C14 Fe1 C2 C1 108.8(3) . . . . ? C11 Fe1 C2 C1 -79.4(3) . . . . ? C10 Fe1 C2 C1 -118.4(4) . . . . ? C9 Fe1 C2 C1 -37.2(2) . . . . ? Fe2 Fe1 C2 C1 -147.5(2) . . . . ? C17 Fe2 C3 C4 -53.6(3) . . . . ? C16 Fe2 C3 C4 -148.0(3) . . . . ? C15 Fe2 C3 C4 93.5(4) . . . . ? C5 Fe2 C3 C4 33.0(3) . . . . ? Fe1 Fe2 C3 C4 130.9(3) . . . . ? C17 Fe2 C3 C10 -172.3(3) . . . . ? C16 Fe2 C3 C10 93.3(3) . . . . ? C15 Fe2 C3 C10 -25.2(5) . . . . ? C4 Fe2 C3 C10 -118.7(4) . . . . ? C5 Fe2 C3 C10 -85.7(3) . . . . ? Fe1 Fe2 C3 C10 12.2(2) . . . . ? C10 C3 C4 C5 18.8(6) . . . . ? Fe2 C3 C4 C5 -63.3(4) . . . . ? C10 C3 C4 Fe2 82.1(3) . . . . ? C17 Fe2 C4 C3 133.2(3) . . . . ? C16 Fe2 C4 C3 40.1(4) . . . . ? C15 Fe2 C4 C3 -130.0(3) . . . . ? C5 Fe2 C4 C3 -127.1(4) . . . . ? Fe1 Fe2 C4 C3 -48.9(3) . . . . ? C17 Fe2 C4 C5 -99.7(3) . . . . ? C16 Fe2 C4 C5 167.1(3) . . . . ? C15 Fe2 C4 C5 -2.9(4) . . . . ? C3 Fe2 C4 C5 127.1(4) . . . . ? Fe1 Fe2 C4 C5 78.2(2) . . . . ? C3 C4 C5 C12 -29.5(6) . . . . ? Fe2 C4 C5 C12 -92.2(4) . . . . ? C3 C4 C5 Fe2 62.6(4) . . . . ? C17 Fe2 C5 C4 82.4(3) . . . . ? C16 Fe2 C5 C4 -35.3(7) . . . . ? C15 Fe2 C5 C4 177.8(3) . . . . ? C3 Fe2 C5 C4 -32.2(3) . . . . ? Fe1 Fe2 C5 C4 -107.1(2) . . . . ? C17 Fe2 C5 C12 -160.1(3) . . . . ? C16 Fe2 C5 C12 82.2(7) . . . . ? C15 Fe2 C5 C12 -64.6(3) . . . . ? C4 Fe2 C5 C12 117.5(4) . . . . ? C3 Fe2 C5 C12 85.3(3) . . . . ? Fe1 Fe2 C5 C12 10.5(3) . . . . ? C12 C6 C7 C18 -172.9(4) . . . . ? C12 C6 C7 C8 7.2(6) . . . . ? C18 C7 C8 C21 0.5(6) . . . . ? C6 C7 C8 C21 -179.6(4) . . . . ? C18 C7 C8 C9 175.5(3) . . . . ? C6 C7 C8 C9 -4.5(5) . . . . ? C2 C1 C9 C11 -2.1(4) . . . . ? Fe1 C1 C9 C11 58.3(2) . . . . ? C2 C1 C9 C8 176.1(4) . . . . ? Fe1 C1 C9 C8 -123.5(4) . . . . ? C2 C1 C9 Fe1 -60.3(3) . . . . ? C21 C8 C9 C11 171.7(3) . . . . ? C7 C8 C9 C11 -3.1(5) . . . . ? C21 C8 C9 C1 -6.4(7) . . . . ? C7 C8 C9 C1 178.8(4) . . . . ? C21 C8 C9 Fe1 -104.5(4) . . . . ? C7 C8 C9 Fe1 80.7(4) . . . . ? C13 Fe1 C9 C11 115.2(2) . . . . ? C14 Fe1 C9 C11 -145.5(3) . . . . ? C2 Fe1 C9 C11 -80.8(2) . . . . ? C1 Fe1 C9 C11 -118.6(3) . . . . ? C10 Fe1 C9 C11 -37.5(2) . . . . ? Fe2 Fe1 C9 C11 8.5(2) . . . . ? C13 Fe1 C9 C1 -126.3(3) . . . . ? C14 Fe1 C9 C1 -27.0(4) . . . . ? C11 Fe1 C9 C1 118.6(3) . . . . ? C2 Fe1 C9 C1 37.8(3) . . . . ? C10 Fe1 C9 C1 81.1(3) . . . . ? Fe2 Fe1 C9 C1 127.1(2) . . . . ? C13 Fe1 C9 C8 5.4(4) . . . . ? C14 Fe1 C9 C8 104.7(4) . . . . ? C11 Fe1 C9 C8 -109.7(4) . . . . ? C2 Fe1 C9 C8 169.5(4) . . . . ? C1 Fe1 C9 C8 131.7(5) . . . . ? C10 Fe1 C9 C8 -147.2(4) . . . . ? Fe2 Fe1 C9 C8 -101.2(3) . . . . ? C1 C2 C10 C11 1.1(4) . . . . ? Fe1 C2 C10 C11 -60.0(2) . . . . ? C1 C2 C10 C3 176.4(4) . . . . ? Fe1 C2 C10 C3 115.4(5) . . . . ? C1 C2 C10 Fe1 61.0(3) . . . . ? C4 C3 C10 C2 -177.8(4) . . . . ? Fe2 C3 C10 C2 -111.7(5) . . . . ? C4 C3 C10 C11 -2.8(5) . . . . ? Fe2 C3 C10 C11 63.3(4) . . . . ? C4 C3 C10 Fe1 -85.1(5) . . . . ? Fe2 C3 C10 Fe1 -19.0(4) . . . . ? C13 Fe1 C10 C2 -139.1(3) . . . . ? C14 Fe1 C10 C2 57.0(3) . . . . ? C11 Fe1 C10 C2 -116.6(3) . . . . ? C1 Fe1 C10 C2 -37.8(2) . . . . ? C9 Fe1 C10 C2 -80.6(3) . . . . ? Fe2 Fe1 C10 C2 147.6(3) . . . . ? C13 Fe1 C10 C11 -22.5(4) . . . . ? C14 Fe1 C10 C11 173.6(2) . . . . ? C2 Fe1 C10 C11 116.6(3) . . . . ? C1 Fe1 C10 C11 78.8(2) . . . . ? C9 Fe1 C10 C11 36.0(2) . . . . ? Fe2 Fe1 C10 C11 -95.8(2) . . . . ? C13 Fe1 C10 C3 89.4(5) . . . . ? C14 Fe1 C10 C3 -74.5(4) . . . . ? C11 Fe1 C10 C3 111.8(4) . . . . ? C2 Fe1 C10 C3 -131.6(5) . . . . ? C1 Fe1 C10 C3 -169.4(4) . . . . ? C9 Fe1 C10 C3 147.8(4) . . . . ? Fe2 Fe1 C10 C3 16.0(3) . . . . ? C1 C9 C11 C12 -172.4(3) . . . . ? C8 C9 C11 C12 9.0(5) . . . . ? Fe1 C9 C11 C12 -113.9(3) . . . . ? C1 C9 C11 C10 2.8(4) . . . . ? C8 C9 C11 C10 -175.8(3) . . . . ? Fe1 C9 C11 C10 61.3(3) . . . . ? C1 C9 C11 Fe1 -58.5(3) . . . . ? C8 C9 C11 Fe1 122.9(3) . . . . ? C2 C10 C11 C9 -2.4(4) . . . . ? C3 C10 C11 C9 -178.7(3) . . . . ? Fe1 C10 C11 C9 -62.7(3) . . . . ? C2 C10 C11 C12 172.8(3) . . . . ? C3 C10 C11 C12 -3.5(5) . . . . ? Fe1 C10 C11 C12 112.5(3) . . . . ? C2 C10 C11 Fe1 60.3(3) . . . . ? C3 C10 C11 Fe1 -116.0(3) . . . . ? C13 Fe1 C11 C9 -72.6(2) . . . . ? C14 Fe1 C11 C9 104.4(5) . . . . ? C2 Fe1 C11 C9 81.4(2) . . . . ? C1 Fe1 C11 C9 37.6(2) . . . . ? C10 Fe1 C11 C9 119.9(3) . . . . ? Fe2 Fe1 C11 C9 -171.8(2) . . . . ? C13 Fe1 C11 C12 48.2(3) . . . . ? C14 Fe1 C11 C12 -134.8(5) . . . . ? C2 Fe1 C11 C12 -157.8(3) . . . . ? C1 Fe1 C11 C12 158.4(3) . . . . ? C10 Fe1 C11 C12 -119.3(4) . . . . ? C9 Fe1 C11 C12 120.8(4) . . . . ? Fe2 Fe1 C11 C12 -51.0(3) . . . . ? C13 Fe1 C11 C10 167.5(2) . . . . ? C14 Fe1 C11 C10 -15.5(6) . . . . ? C2 Fe1 C11 C10 -38.5(2) . . . . ? C1 Fe1 C11 C10 -82.3(2) . . . . ? C9 Fe1 C11 C10 -119.9(3) . . . . ? Fe2 Fe1 C11 C10 68.3(2) . . . . ? C7 C6 C12 C11 -1.6(6) . . . . ? C7 C6 C12 C5 -176.1(4) . . . . ? C9 C11 C12 C6 -6.6(5) . . . . ? C10 C11 C12 C6 178.9(4) . . . . ? Fe1 C11 C12 C6 -95.5(4) . . . . ? C9 C11 C12 C5 168.9(3) . . . . ? C10 C11 C12 C5 -5.7(5) . . . . ? Fe1 C11 C12 C5 79.9(4) . . . . ? C4 C5 C12 C6 -163.7(4) . . . . ? Fe2 C5 C12 C6 127.5(4) . . . . ? C4 C5 C12 C11 21.7(5) . . . . ? Fe2 C5 C12 C11 -47.1(4) . . . . ? C14 Fe1 C13 O1 -92(10) . . . . ? C11 Fe1 C13 O1 87(10) . . . . ? C2 Fe1 C13 O1 13(10) . . . . ? C1 Fe1 C13 O1 16(10) . . . . ? C10 Fe1 C13 O1 102(10) . . . . ? C9 Fe1 C13 O1 51(10) . . . . ? Fe2 Fe1 C13 O1 164(9) . . . . ? C13 Fe1 C14 O2 84(9) . . . . ? C11 Fe1 C14 O2 -93(9) . . . . ? C2 Fe1 C14 O2 -72(9) . . . . ? C1 Fe1 C14 O2 -33(9) . . . . ? C10 Fe1 C14 O2 -104(9) . . . . ? C9 Fe1 C14 O2 -16(9) . . . . ? Fe2 Fe1 C14 O2 -171(9) . . . . ? C17 Fe2 C15 O3 17(2) . . . . ? C16 Fe2 C15 O3 111(2) . . . . ? C4 Fe2 C15 O3 -77(2) . . . . ? C3 Fe2 C15 O3 -133(2) . . . . ? C5 Fe2 C15 O3 -79(2) . . . . ? Fe1 Fe2 C15 O3 -171(2) . . . . ? C17 Fe2 C16 O4 -34(7) . . . . ? C15 Fe2 C16 O4 -129(7) . . . . ? C4 Fe2 C16 O4 58(7) . . . . ? C3 Fe2 C16 O4 82(7) . . . . ? C5 Fe2 C16 O4 85(7) . . . . ? Fe1 Fe2 C16 O4 158(7) . . . . ? C16 Fe2 C17 O5 -119(9) . . . . ? C15 Fe2 C17 O5 -16(9) . . . . ? C4 Fe2 C17 O5 116(9) . . . . ? C3 Fe2 C17 O5 146(9) . . . . ? C5 Fe2 C17 O5 77(9) . . . . ? Fe1 Fe2 C17 O5 -54(9) . . . . ? C8 C7 C18 C19 -2.0(6) . . . . ? C6 C7 C18 C19 178.0(4) . . . . ? C7 C18 C19 C20 2.3(7) . . . . ? C18 C19 C20 C21 -1.1(7) . . . . ? C19 C20 C21 C8 -0.5(7) . . . . ? C7 C8 C21 C20 0.7(6) . . . . ? C9 C8 C21 C20 -173.9(4) . . . . ? C24 C22 C23 C24 1.2(8) 3_556 . . . ? C22 C23 C24 C22 -1.2(8) . . . 3_556 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.827 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.094 #===END