#------------------------------------------------------------------------------ #$Date: 2025-08-19 07:12:48 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301798 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/03/2010338.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_2010338 loop_ _publ_author_name 'Ramm, Matthias' 'Baumann, Hendrik' 'Kirschke, Klaus' _publ_section_title ; 8-Chloro-3,6-dioxaoctyl (E,E)-2-chloro-3-(3,5-dichloro-2-hydroxyphenylazo)-2-butenoate ; _journal_issue 12 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 2072 _journal_page_last 2074 _journal_paper_doi 10.1107/S0108270194000879 _journal_volume 50 _journal_year 1994 _chemical_formula_moiety 'C16 H18 Cl4 N2 O5' _chemical_formula_sum 'C16 H18 Cl4 N2 O5' _chemical_formula_weight 460.14 _chemical_melting_point 344.6(5) _chemical_name_systematic ; 8-Chloro-3,6-dioxaoctyl-(E,E)-3-(3,5-dichloro-2-hydroxyphenylazo)-2-chloro- 2-but-enoat ; _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' _atom_type_scat_source IntTabIV _audit_creation_method 'PLATON TABLE ACC option' _cell_angle_alpha 90 _cell_angle_beta 98.641(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.1189(4) _cell_length_b 25.685(3) _cell_length_c 11.1476(9) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 40 _cell_measurement_theta_min 36 _cell_volume 2015.2(3) _computing_cell_refinement 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'MolEN PROCESS (Fair, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _computing_structure_refinement 'MolEN LSFM (Fair, 1990)' _computing_structure_solution ; MULTAN11/82 (Main, Fiske, Hull, Lessinger, Germain, Declercq & Woolfson, 1982) ; _diffrn_ambient_temperature 293 _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI 0.07 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 4068 _diffrn_reflns_reduction_process ; ? ; _diffrn_reflns_theta_max 75 _diffrn_reflns_theta_min 1.5 _diffrn_standards_decay_% -2.4 _diffrn_standards_interval_time 60 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 5.731 _exptl_absorpt_correction_T_max 1.498 _exptl_absorpt_correction_T_min 0.745 _exptl_absorpt_correction_type refdelf _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.517 _exptl_crystal_description plate _exptl_crystal_F_000 944 _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.27 _refine_diff_density_max 0.342 _refine_diff_density_min -0.358 _refine_ls_abs_structure_details ; ? ; _refine_ls_extinction_coef 1.0166E-6 _refine_ls_extinction_method 'B-C Type 1, isotropic' _refine_ls_goodness_of_fit_obs 2.459 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 2758 _refine_ls_R_factor_obs 0.045 _refine_ls_shift/esd_max 0.02 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/\s(F)^2^' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.071 _reflns_number_observed 2758 _reflns_number_total 3986 _reflns_observed_criterion refl_observed_if_F_>_3.0_sigma(F) _cod_data_source_file se1046.cif _cod_data_source_block baum _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_chemical_melting_point' value '71 -72_C' was changed to '344.6(5)' - it was converted from degrees Celsius(C) to Kelvins(K), the average value was taken and precision was estimated. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana The following automatic conversions were performed: '_chemical_melting_point' value '71 -72_C' was changed to '344.6(5)' - it was converted from degrees Celsius(C) to Kelvins(K), the average value was taken and precision was estimated. '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/\s(F)^2^' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/\s(F)^2^'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2010338 loop_ _symmetry_equiv_pos_as_xyz X,Y,Z 1/2+X,1/2-Y,1/2+Z -X,-Y,-Z 1/2-X,1/2+Y,1/2-Z 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 Cl1 0.1224(9) 0.0820(6) 0.0387(3) -0.0090(4) 0.0063(5) 0.0121(6) Cl2 0.1258(9) 0.0572(4) 0.0842(5) -0.0050(4) 0.0437(5) -0.0051(6) Cl3 0.0653(6) 0.0942(6) 0.0416(3) 0.0081(4) 0.0075(4) -0.0165(5) Cl4 0.0715(7) 0.0761(5) 0.0836(6) 0.0083(5) -0.0097(5) -0.0088(5) O1 0.0827(18) 0.0574(12) 0.0429(10) -0.0086(9) 0.0065(11) 0.0081(12) O2 0.133(3) 0.0711(15) 0.0492(11) -0.0046(11) 0.0296(14) -0.0156(16) O3 0.0555(15) 0.0639(13) 0.0520(11) 0.0028(10) 0.0050(11) -0.0017(12) O4 0.0517(15) 0.0694(13) 0.0683(14) -0.0015(12) -0.0036(12) -0.0012(13) O5 0.0569(16) 0.0715(14) 0.0734(15) -0.0019(12) -0.0050(13) 0.0006(13) N1 0.0413(15) 0.0658(15) 0.0438(12) -0.0067(12) 0.0065(11) -0.0026(13) N2 0.0364(15) 0.0641(14) 0.0418(11) -0.0030(11) 0.0044(11) -0.0004(13) C1 0.0355(17) 0.0642(17) 0.0406(13) -0.0070(13) 0.0057(12) 0.0000(15) C2 0.0381(18) 0.0587(16) 0.0419(13) -0.0062(13) 0.0005(13) 0.0066(15) C3 0.051(2) 0.0653(17) 0.0404(13) -0.0057(14) -0.0028(14) 0.0089(17) C4 0.053(2) 0.0651(18) 0.0452(14) 0.0005(14) 0.0052(15) 0.0071(17) C5 0.055(2) 0.0565(16) 0.0587(16) -0.0061(15) 0.0139(15) 0.0035(17) C6 0.051(2) 0.0629(18) 0.0485(15) -0.0114(14) 0.0109(15) -0.0015(17) C7 0.0368(18) 0.078(2) 0.0352(12) -0.0048(13) 0.0054(12) -0.0101(16) C8 0.071(2) 0.085(2) 0.0460(14) -0.0160(16) 0.0179(15) -0.017(2) C9 0.0347(18) 0.075(2) 0.0381(13) 0.0023(13) 0.0023(13) -0.0069(16) C10 0.0359(18) 0.0697(19) 0.0460(14) 0.0027(15) 0.0019(13) -0.0014(16) C11 0.056(2) 0.0621(19) 0.0629(18) 0.0000(16) 0.0112(17) 0.0115(18) C12 0.054(2) 0.0575(17) 0.0603(17) -0.0063(16) 0.0077(16) 0.0058(17) C13 0.057(2) 0.075(2) 0.071(2) -0.0098(19) -0.004(2) -0.006(2) C14 0.052(2) 0.092(3) 0.068(2) -0.001(2) -0.0038(19) -0.004(2) C15 0.067(3) 0.063(2) 0.077(2) -0.0052(18) -0.001(2) -0.001(2) C16 0.072(3) 0.079(2) 0.070(2) -0.0025(19) 0.001(2) 0.018(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_thermal_displace_type Cl1 0.27730(19) 0.02987(4) 0.06612(7) 0.0816(4) Uani Cl2 0.27354(19) 0.20683(4) 0.32066(9) 0.0862(4) Uani Cl3 0.22017(14) -0.12438(4) 0.77274(7) 0.0671(3) Uani Cl4 -0.94626(16) -0.17921(4) 0.02035(10) 0.0793(3) Uani O1 0.2722(4) -0.02052(9) 0.29773(19) 0.0613(8) Uani O2 0.2695(5) -0.11181(11) 0.4347(2) 0.0828(12) Uani O3 0.1964(3) -0.17503(9) 0.5537(2) 0.0575(8) Uani O4 -0.1038(3) -0.19167(10) 0.3518(2) 0.0644(8) Uani O5 -0.5642(4) -0.16776(10) 0.1887(2) 0.0688(9) Uani N1 0.2556(4) 0.03340(11) 0.5294(2) 0.0503(8) Uani N2 0.2508(4) -0.01559(10) 0.5260(2) 0.0476(8) Uani C1 0.2648(5) 0.05756(13) 0.4170(3) 0.0468(9) Uani C2 0.2705(5) 0.03084(12) 0.3071(3) 0.0468(9) Uani C3 0.2774(5) 0.06122(13) 0.2034(3) 0.0532(10) Uani C4 0.2799(5) 0.11463(13) 0.2072(3) 0.0547(10) Uani C5 0.2742(5) 0.13962(13) 0.3167(3) 0.0562(10) Uani C6 0.2645(5) 0.11164(13) 0.4210(3) 0.0538(10) Uani C7 0.2414(5) -0.03989(14) 0.6390(3) 0.0500(10) Uani C8 0.2355(6) -0.00657(15) 0.7479(3) 0.0664(11) Uani C9 0.2349(5) -0.09207(14) 0.6383(3) 0.0496(10) Uani C10 0.2361(5) -0.12654(14) 0.5301(3) 0.0510(10) Uani C11 0.1946(5) -0.21376(14) 0.4582(3) 0.0601(11) Uani C12 -0.0026(5) -0.23223(13) 0.4179(3) 0.0574(10) Uani C13 -0.2902(6) -0.20558(15) 0.2979(4) 0.0691(12) Uani C14 -0.3685(6) -0.15970(17) 0.2271(4) 0.0720(14) Uani C15 -0.6513(6) -0.12308(15) 0.1284(4) 0.0702(14) Uani C16 -0.8574(6) -0.12765(16) 0.1198(4) 0.0747(14) Uani H1 0.256(7) -0.037(2) 0.399(4) 0.29(4) Uiso H4 0.279(5) 0.1339(12) 0.130(3) 0.120(19) Uiso H6 0.256(5) 0.1292(13) 0.490(3) 0.15(2) Uiso H81 0.182(6) -0.0257(16) 0.804(4) 0.22(3) Uiso H82 0.127(5) 0.0158(14) 0.725(3) 0.16(2) Uiso H83 0.351(5) 0.0133(14) 0.763(3) 0.16(2) Uiso H111 0.240(5) -0.2033(13) 0.390(3) 0.13(2) Uiso H112 0.273(5) -0.2381(14) 0.487(3) 0.15(2) Uiso H121 -0.058(5) -0.2408(12) 0.487(3) 0.119(19) Uiso H122 -0.010(4) -0.2609(12) 0.363(3) 0.103(18) Uiso H131 -0.341(6) -0.2150(16) 0.374(4) 0.21(3) Uiso H132 -0.296(5) -0.2344(13) 0.259(3) 0.14(2) Uiso H141 -0.342(8) -0.156(2) 0.150(5) 0.30(4) Uiso H142 -0.359(6) -0.1309(16) 0.285(4) 0.20(3) Uiso H151 -0.604(5) -0.1211(14) 0.057(3) 0.16(2) Uiso H152 -0.601(5) -0.0910(13) 0.187(3) 0.15(2) Uiso H161 -0.934(6) -0.1010(16) 0.080(4) 0.20(3) Uiso H162 -0.904(5) -0.1400(15) 0.195(3) 0.17(2) Uiso loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 17 5 2 17 3 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C10 O3 C11 118.7(3) yes C12 O4 C13 114.1(3) yes C14 O5 C15 111.4(3) yes N2 N1 C1 114.7(2) yes N1 N2 C7 114.7(2) yes N1 C1 C2 124.7(3) yes N1 C1 C6 114.3(3) yes C2 C1 C6 121.0(3) yes O1 C2 C1 123.7(3) yes O1 C2 C3 119.2(3) yes C1 C2 C3 117.0(3) yes Cl1 C3 C2 118.4(3) yes Cl1 C3 C4 119.4(3) yes C2 C3 C4 122.2(3) yes C3 C4 C5 119.2(3) yes Cl2 C5 C4 119.1(3) yes Cl2 C5 C6 120.0(3) yes C4 C5 C6 120.9(3) yes C1 C6 C5 119.6(3) yes N2 C7 C8 118.8(3) yes N2 C7 C9 116.2(3) yes C8 C7 C9 125.0(3) yes Cl3 C9 C7 118.7(3) yes Cl3 C9 C10 115.0(3) yes C7 C9 C10 126.2(3) yes O2 C10 O3 124.1(3) yes O2 C10 C9 124.0(3) yes O3 C10 C9 111.8(3) yes O3 C11 C12 110.1(3) yes O4 C12 C11 107.9(3) yes O4 C13 C14 106.2(3) yes O5 C14 C13 108.7(3) yes O5 C15 C16 109.2(3) yes Cl4 C16 C15 111.1(3) yes C2 O1 H1 106(2) no C3 C4 H4 118.3(18) no C5 C4 H4 122.4(18) no C1 C6 H6 122(2) no C5 C6 H6 119(2) no C7 C8 H81 108(3) no C7 C8 H82 104(2) no C7 C8 H83 109(2) no H81 C8 H82 96(3) no H81 C8 H83 126(3) no H82 C8 H83 111(3) no O3 C11 H111 116(2) no O3 C11 H112 107(2) no C12 C11 H111 106(2) no C12 C11 H112 114(2) no H111 C11 H112 103(3) no O4 C12 H121 111(2) no O4 C12 H122 105.1(19) no C11 C12 H121 109(2) no C11 C12 H122 113.5(18) no H121 C12 H122 111(3) no O4 C13 H131 98(3) no O4 C13 H132 114(2) no C14 C13 H131 119(2) no C14 C13 H132 116(2) no H131 C13 H132 103(3) no O5 C14 H141 94(4) no O5 C14 H142 106(3) no C13 C14 H141 118(3) no C13 C14 H142 106(3) no H141 C14 H142 123(4) no O5 C15 H151 105(2) no O5 C15 H152 104.4(18) no C16 C15 H151 117(2) no C16 C15 H152 109.9(19) no H151 C15 H152 111(3) no Cl4 C16 H161 97(3) no Cl4 C16 H162 99(2) no C15 C16 H161 118(3) no C15 C16 H162 115(2) no H161 C16 H162 113(3) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cl1 C3 . . 1.729(3) yes Cl2 C5 . . 1.727(3) yes Cl3 C9 . . 1.730(4) yes Cl4 C16 . . 1.781(4) yes O1 C2 . . 1.324(4) yes O2 C10 . . 1.186(4) yes O3 C10 . . 1.312(4) yes O3 C11 . . 1.456(4) yes O4 C12 . . 1.410(4) yes O4 C13 . . 1.418(5) yes O5 C14 . . 1.410(5) yes O5 C15 . . 1.424(5) yes N1 N2 . . 1.259(4) yes N1 C1 . . 1.409(4) yes N2 C7 . . 1.416(4) yes C1 C2 . . 1.410(5) yes C1 C6 . . 1.390(5) yes C2 C3 . . 1.402(5) yes C3 C4 . . 1.373(5) yes C4 C5 . . 1.385(5) yes C5 C6 . . 1.377(5) yes C7 C8 . . 1.491(5) yes C7 C9 . . 1.341(5) yes C9 C10 . . 1.497(5) yes C11 C12 . . 1.486(5) yes C13 C14 . . 1.480(6) yes C15 C16 . . 1.461(6) yes O1 H1 . . 1.23(5) no C4 H4 . . 0.99(3) no C6 H6 . . 0.90(3) no C8 H81 . . 0.92(4) no C8 H82 . . 0.97(4) no C8 H83 . . 0.96(4) no C11 H111 . . 0.91(3) no C11 H112 . . 0.87(4) no C12 H121 . . 0.94(3) no C12 H122 . . 0.95(3) no C13 H131 . . 1.00(4) no C13 H132 . . 0.86(3) no C14 H141 . . 0.91(6) no C14 H142 . . 0.98(4) no C15 H151 . . 0.91(3) no C15 H152 . . 1.08(3) no C16 H161 . . 0.94(4) no C16 H162 . . 1.00(3) no 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_publ_flag C10 O3 C11 C12 -111.3(3) no C11 O3 C10 C9 -179.1(3) no C11 O3 C10 O2 0.7(5) no C13 O4 C12 C11 174.4(3) no C12 O4 C13 C14 -176.6(3) no C15 O5 C14 C13 175.2(3) no C14 O5 C15 C16 -164.9(3) no N2 N1 C1 C6 178.2(3) no N2 N1 C1 C2 -0.6(5) no C1 N1 N2 C7 -180.0(6) no N1 N2 C7 C9 179.6(3) no N1 N2 C7 C8 0.8(5) no N1 C1 C2 C3 179.3(3) no C6 C1 C2 C3 0.5(5) no N1 C1 C6 C5 179.6(3) no C2 C1 C6 C5 -1.5(5) no N1 C1 C2 O1 -1.6(6) no C6 C1 C2 O1 179.6(3) no O1 C2 C3 C4 -178.7(3) no O1 C2 C3 Cl1 2.8(5) no C1 C2 C3 Cl1 -178.1(3) no C1 C2 C3 C4 0.4(5) no C2 C3 C4 C5 -0.4(6) no Cl1 C3 C4 C5 178.1(3) no C3 C4 C5 C6 -0.5(5) no C3 C4 C5 Cl2 -179.0(3) no Cl2 C5 C6 C1 179.9(3) no C4 C5 C6 C1 1.5(5) no C8 C7 C9 C10 178.5(4) no N2 C7 C9 C10 -0.2(5) no C8 C7 C9 Cl3 -0.5(5) no N2 C7 C9 Cl3 -179.2(2) no Cl3 C9 C10 O2 -170.0(3) no C7 C9 C10 O3 -169.3(3) no Cl3 C9 C10 O3 9.8(4) no C7 C9 C10 O2 11.0(6) no O3 C11 C12 O4 71.7(3) no O4 C13 C14 O5 -169.9(3) no O5 C15 C16 Cl4 -67.7(4) no loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139057451