#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/32/2203254.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2203254 loop_ _publ_author_name 'Koikawa, Masayuki' 'Iwashita, Kumiko' 'Tokii, Tadashi' _publ_section_title ; Dichlorobis[N-(2-oxymethylphenyl)salicylideneiminato]diiron(III) ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m239 _journal_page_last m241 _journal_paper_doi 10.1107/S1600536804001709 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Fe2 (C28 H22 N2 O4) Cl2 ]' _chemical_formula_moiety '[Fe2 (C28 H22 N2 O4) Cl2 ]' _chemical_formula_sum 'C28 H22 Cl2 Fe2 N2 O4' _chemical_formula_weight 633.09 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _cell_angle_alpha 90 _cell_angle_beta 106.110(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.182(2) _cell_length_b 12.131(2) _cell_length_c 11.300(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 296.1 _cell_measurement_theta_max 12.4 _cell_measurement_theta_min 10.1 _cell_volume 1340.9(4) _computing_cell_refinement 'MSC/AFC Diffractometer Control ' _computing_data_collection 'MSC/AFC Diffractometer Control (Molecular Structure Corporation, 1991)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material CrystalStructure _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _diffrn_measured_fraction_theta_full 0.9988 _diffrn_measured_fraction_theta_max 0.9988 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 3405 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_standards_decay_% 1.2 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.317 _exptl_absorpt_correction_T_max 0.768 _exptl_absorpt_correction_T_min 0.724 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour 'dark brown' _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 644.00 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 1.02 _refine_diff_density_min -1.65 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.00 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 183 _refine_ls_number_reflns 3079 _refine_ls_R_factor_gt 0.040 _refine_ls_shift/su_max <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = (1/[\s(Fo^2^) + 0.0006Fo^2^])/(4Fo^2^)' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.123 _reflns_number_gt 1809 _reflns_number_total 3081 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ya6192.cif _cod_data_source_block I _cod_database_code 2203254 _cod_database_fobs_code 2203254 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Fe1 0.61814(5) 0.08380(4) 0.55417(4) 0.03230(10) Uani d . 1.00 Fe Cl1 0.55060(10) 0.24033(9) 0.62070(10) 0.0565(3) Uani d . 1.00 Cl O1 0.5356(3) -0.0526(2) 0.5934(2) 0.0400(7) Uani d . 1.00 O O2 0.7415(3) 0.1125(3) 0.4634(2) 0.0473(8) Uani d . 1.00 O N1 0.7818(3) 0.0481(2) 0.7076(3) 0.0316(7) Uani d . 1.00 N C1 0.5874(4) -0.1264(3) 0.6939(3) 0.0410(10) Uani d . 1.00 C C2 0.6494(4) -0.0640(3) 0.8113(3) 0.0362(9) Uani d . 1.00 C C3 0.6136(4) -0.0896(4) 0.9181(3) 0.0450(10) Uani d . 1.00 C C4 0.6745(5) -0.0384(4) 1.0280(4) 0.0540(10) Uani d . 1.00 C C5 0.7722(5) 0.0409(4) 1.0341(4) 0.0510(10) Uani d . 1.00 C C6 0.8099(4) 0.0692(3) 0.9291(3) 0.0440(10) Uani d . 1.00 C C7 0.7500(4) 0.0165(3) 0.8185(3) 0.0338(9) Uani d . 1.00 C C8 0.9091(4) 0.0673(3) 0.7120(4) 0.0390(10) Uani d . 1.00 C C9 0.9594(4) 0.1078(3) 0.6153(4) 0.0400(10) Uani d . 1.00 C C10 1.1003(4) 0.1287(4) 0.6401(5) 0.0570(10) Uani d . 1.00 C C11 1.1561(5) 0.1701(4) 0.5539(5) 0.065(2) Uani d . 1.00 C C12 1.0731(5) 0.1924(4) 0.4372(5) 0.0550(10) Uani d . 1.00 C C13 0.9348(4) 0.1731(4) 0.4070(4) 0.0500(10) Uani d . 1.00 C C14 0.8749(4) 0.1310(3) 0.4952(4) 0.0420(10) Uani d . 1.00 C H1 0.5148 -0.1710 0.7044 0.047 Uiso c R 1.00 H H2 0.6554 -0.1720 0.6762 0.047 Uiso c R 1.00 H H3 0.5454 -0.1438 0.9150 0.053 Uiso c R 1.00 H H4 0.6490 -0.0580 1.1000 0.065 Uiso c R 1.00 H H5 0.8140 0.0765 1.1101 0.057 Uiso c R 1.00 H H6 0.8768 0.1248 0.9331 0.049 Uiso c R 1.00 H H7 0.9751 0.0525 0.7882 0.044 Uiso c R 1.00 H H8 1.1582 0.1133 0.7201 0.066 Uiso c R 1.00 H H9 1.2516 0.1836 0.5734 0.081 Uiso c R 1.00 H H10 1.1123 0.2216 0.3768 0.072 Uiso c R 1.00 H H11 0.8797 0.1882 0.3259 0.063 Uiso c R 1.00 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe1 0.0268(2) 0.0341(3) 0.0318(3) -0.0050(2) 0.0012(2) 0.0005(3) Cl1 0.0540(6) 0.0481(6) 0.0592(7) 0.0133(5) 0.0024(5) -0.0072(5) O1 0.0370(10) 0.0410(10) 0.0330(10) -0.0130(10) -0.0050(10) 0.0050(10) O2 0.0350(10) 0.068(2) 0.0380(10) -0.0070(10) 0.0090(10) 0.0000(10) N1 0.0270(10) 0.032(2) 0.0320(10) -0.0030(10) 0.0020(10) 0.0030(10) C1 0.045(2) 0.036(2) 0.036(2) -0.007(2) 0.001(2) 0.009(2) C2 0.034(2) 0.037(2) 0.033(2) 0.004(2) 0.0010(10) 0.0060(10) C3 0.039(2) 0.050(2) 0.044(2) -0.003(2) 0.009(2) 0.014(2) C4 0.062(3) 0.066(3) 0.035(2) 0.008(2) 0.014(2) 0.007(2) C5 0.064(3) 0.047(2) 0.032(2) 0.005(2) -0.001(2) -0.006(2) C6 0.047(2) 0.037(2) 0.039(2) 0.000(2) -0.005(2) -0.001(2) C7 0.032(2) 0.032(2) 0.033(2) 0.0040(10) 0.0000(10) 0.0030(10) C8 0.029(2) 0.037(2) 0.045(2) 0.001(2) 0.000(2) 0.006(2) C9 0.030(2) 0.037(2) 0.053(2) -0.002(2) 0.011(2) 0.001(2) C10 0.033(2) 0.058(3) 0.073(3) -0.002(2) 0.006(2) 0.011(2) C11 0.035(2) 0.062(3) 0.105(4) -0.007(2) 0.033(3) 0.007(3) C12 0.056(3) 0.055(3) 0.068(3) -0.010(2) 0.039(2) -0.004(2) C13 0.056(3) 0.056(3) 0.047(2) -0.010(2) 0.025(2) -0.009(2) C14 0.039(2) 0.041(2) 0.048(2) -0.004(2) 0.017(2) -0.011(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.346 0.844 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 Fe1 O1 . 116.90(9) yes Cl1 Fe1 O2 . 110.30(10) yes Cl1 Fe1 N1 . 98.46(9) yes Cl1 Fe1 O1 2_656 101.64(3) yes O1 Fe1 O2 . 132.80(10) yes O1 Fe1 N1 . 86.00(10) yes O1 Fe1 O1 2_656 74.99(7) yes O2 Fe1 N1 . 89.50(10) yes O2 Fe1 O1 2_656 93.90(8) yes N1 Fe1 O1 2_656 157.00(8) yes C1 O1 Fe1 . 128.5(2) yes C1 O1 Fe1 2_656 125.5(2) yes Fe1 O1 Fe1 2_656 105.00(10) yes C14 O2 Fe1 . 132.8(3) yes C7 N1 C8 . 118.6(3) yes C7 N1 Fe1 . 117.3(2) yes C8 N1 Fe1 . 123.4(3) yes C2 C1 O1 . 110.9(3) yes C3 C2 C7 . 118.0(3) yes C3 C2 C1 . 120.4(3) yes C7 C2 C1 . 121.5(4) yes C4 C3 C2 . 121.6(4) yes C5 C4 C3 . 120.1(4) yes C6 C5 C4 . 120.0(4) yes C7 C6 C5 . 120.0(4) yes N1 C7 C2 . 118.4(3) yes N1 C7 C6 . 121.1(3) yes C2 C7 C6 . 120.4(4) yes C9 C8 N1 . 126.9(3) yes C10 C9 C14 . 118.0(4) yes C10 C9 C8 . 118.4(4) yes C14 C9 C8 . 123.6(3) yes C11 C10 C9 . 122.1(4) yes C12 C11 C10 . 119.5(4) yes C13 C12 C11 . 121.2(5) yes C14 C13 C12 . 120.3(4) yes O2 C14 C9 . 122.0(4) yes O2 C14 C13 . 119.0(3) yes C9 C14 C13 . 118.9(4) yes C2 C1 H1 . 109.1 no C2 C1 H2 . 109.1 no H1 C1 H2 . 109.5 no H1 C1 O1 . 109.1 no H2 C1 O1 . 109.1 no C4 C3 H3 . 119.2 no H3 C3 C2 . 119.2 no C5 C4 H4 . 120.0 no H4 C4 C3 . 119.9 no C6 C5 H5 . 120.0 no H5 C5 C4 . 120.0 no C7 C6 H6 . 120.0 no H6 C6 C5 . 120.0 no C9 C8 H7 . 116.6 no H7 C8 N1 . 116.6 no C11 C10 H8 . 118.9 no H8 C10 C9 . 118.9 no C12 C11 H9 . 120.3 no H9 C11 C10 . 120.3 no C13 C12 H10 . 119.4 no H10 C12 C11 . 119.4 no C14 C13 H11 . 119.9 no H11 C13 C12 . 119.9 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 Cl1 . 2.2200(10) yes Fe1 O1 . 1.962(3) yes Fe1 O1 2_656 1.981(2) yes Fe1 O2 . 1.862(3) yes Fe1 N1 . 2.090(2) yes O1 C1 . 1.428(4) yes O2 C14 . 1.324(5) yes N1 C7 . 1.431(5) yes N1 C8 . 1.303(5) yes C1 C2 . 1.506(5) yes C2 C3 . 1.388(6) yes C2 C7 . 1.401(5) yes C3 C4 . 1.373(6) yes C4 C5 . 1.372(7) yes C5 C6 . 1.387(6) yes C6 C7 . 1.386(5) yes C8 C9 . 1.418(6) yes C9 C10 . 1.406(6) yes C9 C14 . 1.419(5) yes C10 C11 . 1.354(8) yes C11 C12 . 1.381(7) yes C12 C13 . 1.374(6) yes C13 C14 . 1.402(7) yes Fe1 Fe1 2_656 3.1282(7) yes C1 H1 . 0.950 no C1 H2 . 0.950 no C3 H3 . 0.950 no C4 H4 . 0.950 no C5 H5 . 0.950 no C6 H6 . 0.950 no C8 H7 . 0.950 no C10 H8 . 0.950 no C11 H9 . 0.950 no C12 H10 . 0.950 no C13 H11 . 0.950 no