#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/4/4060234.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_4060234 _journal_name_full 'Organometallics' _journal_year 2004 _chemical_formula_moiety 'C21 H10 Fe2 O5, C3 H3' _chemical_formula_sum 'C24 H13 Fe2 O5' _chemical_formula_weight 493.05 _symmetry_cell_setting 'monoclinic' _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_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 ; _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) _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) _cod_database_code 4060234