#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/4/4060233.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4060233 _journal_name_full 'Organometallics' _journal_year 2004 _chemical_formula_sum 'C17 H8 Fe2 O5' _chemical_formula_weight 403.94 _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 _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) 'MSC/AFC Diffractometer Control' ; teXsan for Windows version 1.06 (MSC, 1997-1999) ; ; DIRDIF94 PATTY (Beurskens, 1994) ; _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)