#------------------------------------------------------------------------------ #$Date: 2025-08-19 11:43:10 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301803 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/49/2204940.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_2204940 loop_ _publ_author_name 'Dege, Necmi' '\"Ozdemir, Nam\?ik' '\,Cetin, Ahmet' 'Cans\?iz, Ahmet' '\,Sekerci, Memet' 'Din\,cer, Muharrem' _publ_section_title ; 4-Ethyl-5-(2-hydroxyphenyl)-2H-1,2,4-triazole-3(4H)-thione ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o17 _journal_page_last o19 _journal_paper_doi 10.1107/S1600536804031137 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac 'C10 H11 N3 O S' _chemical_formula_moiety 'C10 H11 N3 O S' _chemical_formula_sum 'C10 H11 N3 O S' _chemical_formula_weight 221.28 _chemical_name_systematic ; 4-Ethyl-5-(2-hydroxyphenyl)-2H-1,2,4-triazole-3(4H)-thione ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 102.266(6) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.7879(8) _cell_length_b 7.9071(5) _cell_length_c 13.8045(10) _cell_measurement_reflns_used 12416 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.37 _cell_measurement_theta_min 2.13 _cell_volume 1043.99(13) _computing_cell_refinement X-AREA _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-RED (Stoe & Cie, 2002)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999) and PLATON (Spek, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 6.67 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'STOE IPDS-II' _diffrn_measurement_method 'w scans' _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_source 'sealed X-ray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 9857 _diffrn_reflns_theta_full 29.25 _diffrn_reflns_theta_max 29.25 _diffrn_reflns_theta_min 2.13 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.286 _exptl_absorpt_correction_T_max 0.9354 _exptl_absorpt_correction_T_min 0.8688 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(X-RED; Stoe & Cie, 2002)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 464 _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.49 _exptl_crystal_size_min 0.40 _refine_diff_density_max 0.308 _refine_diff_density_min -0.258 _refine_ls_extinction_coef 0.043(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 181 _refine_ls_number_reflns 2825 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.009 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0305 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.2483P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0836 _refine_ls_wR_factor_ref 0.0863 _reflns_number_gt 2440 _reflns_number_total 2825 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ob6445.cif _cod_data_source_block III _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: '_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 ; _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2204940 _cod_database_fobs_code 2204940 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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_occupancy _atom_site_type_symbol S1 1.06463(3) 0.25539(4) 0.45325(2) 0.02626(11) Uani d 1 S O1 0.49766(9) 0.31314(13) 0.22506(6) 0.0273(2) Uani d 1 O H1 0.424(2) 0.372(2) 0.2147(13) 0.043(5) Uiso d 1 H N1 0.74356(9) 0.01738(12) 0.29738(6) 0.01858(19) Uani d 1 N N2 0.85055(9) 0.04088(12) 0.37852(7) 0.01856(19) Uani d 1 N H2 0.8695(18) -0.037(2) 0.4270(13) 0.040(4) Uiso d 1 H N3 0.85843(9) 0.25331(11) 0.28499(7) 0.01731(18) Uani d 1 N C1 0.75026(10) 0.14977(13) 0.24182(7) 0.01641(19) Uani d 1 C C2 0.92342(11) 0.18245(13) 0.37324(7) 0.0182(2) Uani d 1 C C3 0.65877(11) 0.18360(13) 0.14442(7) 0.0170(2) Uani d 1 C C4 0.53203(11) 0.26801(14) 0.13856(7) 0.0188(2) Uani d 1 C C5 0.44767(12) 0.30188(16) 0.04614(8) 0.0230(2) Uani d 1 C H5 0.3597(17) 0.364(2) 0.0420(12) 0.032(4) Uiso d 1 H C6 0.49001(13) 0.25253(15) -0.03933(8) 0.0244(2) Uani d 1 C H6 0.4297(18) 0.274(2) -0.1018(13) 0.033(4) Uiso d 1 H C7 0.61616(13) 0.16998(16) -0.03379(8) 0.0258(2) Uani d 1 C H7 0.6460(18) 0.136(2) -0.0926(13) 0.037(4) Uiso d 1 H C8 0.70067(12) 0.13553(15) 0.05792(8) 0.0222(2) Uani d 1 C H8 0.7916(16) 0.077(2) 0.0649(11) 0.025(4) Uiso d 1 H C9 0.89554(12) 0.41659(14) 0.24674(8) 0.0219(2) Uani d 1 C H9A 0.8723(15) 0.4106(19) 0.1741(11) 0.026(4) Uiso d 1 H H9B 0.9990(17) 0.432(2) 0.2687(12) 0.032(4) Uiso d 1 H C10 0.81831(16) 0.56160(16) 0.28239(11) 0.0320(3) Uani d 1 C H10A 0.720(2) 0.540(2) 0.2648(13) 0.043(5) Uiso d 1 H H10B 0.8433(18) 0.669(2) 0.2539(13) 0.039(4) Uiso d 1 H H10C 0.840(2) 0.565(3) 0.3547(15) 0.051(5) Uiso d 1 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 S1 0.02542(17) 0.02366(16) 0.02394(16) -0.00738(10) -0.00773(11) 0.00530(10) O1 0.0229(4) 0.0430(5) 0.0154(3) 0.0135(4) 0.0028(3) -0.0016(3) N1 0.0156(4) 0.0209(4) 0.0177(4) -0.0011(3) 0.0001(3) 0.0021(3) N2 0.0162(4) 0.0199(4) 0.0175(4) -0.0018(3) -0.0012(3) 0.0036(3) N3 0.0168(4) 0.0175(4) 0.0167(4) -0.0008(3) 0.0014(3) 0.0025(3) C1 0.0143(4) 0.0181(4) 0.0169(4) 0.0011(3) 0.0034(3) 0.0000(3) C2 0.0178(5) 0.0184(5) 0.0176(4) 0.0002(4) 0.0021(4) 0.0016(4) C3 0.0164(5) 0.0185(4) 0.0153(4) 0.0004(4) 0.0013(3) 0.0007(3) C4 0.0180(5) 0.0224(5) 0.0157(4) 0.0013(4) 0.0028(4) -0.0006(4) C5 0.0193(5) 0.0300(6) 0.0180(5) 0.0054(4) 0.0001(4) 0.0003(4) C6 0.0263(6) 0.0293(6) 0.0154(4) 0.0025(4) -0.0006(4) 0.0014(4) C7 0.0301(6) 0.0313(6) 0.0167(5) 0.0030(5) 0.0066(4) -0.0016(4) C8 0.0216(5) 0.0258(5) 0.0198(5) 0.0044(4) 0.0057(4) -0.0001(4) C9 0.0231(5) 0.0200(5) 0.0219(5) -0.0033(4) 0.0028(4) 0.0053(4) C10 0.0392(7) 0.0199(5) 0.0371(7) 0.0015(5) 0.0083(6) 0.0027(5) 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 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 _geom_angle_publ_flag C4 O1 H1 111.1(12) ? C1 N1 N2 104.20(9) yes C2 N2 N1 113.06(9) yes C2 N2 H2 125.9(11) ? N1 N2 H2 121.0(11) ? C2 N3 C1 108.20(8) yes C2 N3 C9 125.17(9) ? C1 N3 C9 126.57(9) no N1 C1 N3 110.71(9) yes N1 C1 C3 125.75(9) no N3 C1 C3 123.51(9) no N2 C2 N3 103.81(9) yes N2 C2 S1 128.77(8) no N3 C2 S1 127.40(8) ? C8 C3 C4 120.00(9) ? C8 C3 C1 119.97(9) no C4 C3 C1 120.01(9) ? O1 C4 C5 123.19(10) ? O1 C4 C3 117.31(9) no C5 C4 C3 119.50(9) ? C6 C5 C4 119.98(10) ? C6 C5 H5 120.5(9) ? C4 C5 H5 119.5(9) ? C7 C6 C5 120.66(10) ? C7 C6 H6 120.6(10) ? C5 C6 H6 118.7(10) ? C8 C7 C6 119.73(10) ? C8 C7 H7 119.3(10) ? C6 C7 H7 121.0(10) ? C7 C8 C3 120.13(10) ? C7 C8 H8 122.1(9) ? C3 C8 H8 117.8(9) ? N3 C9 C10 111.75(9) ? N3 C9 H9A 107.7(9) ? C10 C9 H9A 110.2(9) ? N3 C9 H9B 107.8(10) ? C10 C9 H9B 110.9(9) ? H9A C9 H9B 108.3(12) ? C9 C10 H10A 109.1(11) ? C9 C10 H10B 109.7(10) ? H10A C10 H10B 111.9(15) ? C9 C10 H10C 109.9(12) ? H10A C10 H10C 104.9(15) ? H10B C10 H10C 111.2(16) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag S1 C2 1.6776(11) ? O1 C4 1.3554(12) ? O1 H1 0.850(19) ? N1 C1 1.3076(13) yes N1 N2 1.3737(13) yes N2 C2 1.3376(14) yes N2 H2 0.901(18) ? N3 C2 1.3688(13) yes N3 C1 1.3705(13) yes N3 C9 1.4694(13) yes C1 C3 1.4731(14) ? C3 C8 1.3951(14) ? C3 C4 1.3958(14) ? C4 C5 1.3906(15) ? C5 C6 1.3869(15) ? C5 H5 0.982(16) ? C6 C7 1.3843(17) ? C6 H6 0.951(18) ? C7 C8 1.3843(16) ? C7 H7 0.958(16) ? C8 H8 0.990(15) ? C9 C10 1.5121(17) no C9 H9A 0.981(15) ? C9 H9B 1.001(17) ? C10 H10A 0.957(19) ? C10 H10B 0.985(18) ? C10 H10C 0.98(2) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C9 H9B S1 . 1.00(2) 2.86(2) 3.2383(12) 104.0(10) O1 H1 N1 2_655 0.85(2) 1.98(2) 2.8227(12) 175(2) N2 H2 S1 3_756 0.90(2) 2.38(2) 3.2789(10) 174(2) C9 H9B Cg1 2_755 1.00(2) 2.76(2) 3.4652(13) 128.0(10) 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 C1 N1 N2 C2 -0.93(12) ? N2 N1 C1 N3 0.71(11) ? N2 N1 C1 C3 178.77(9) ? C2 N3 C1 N1 -0.30(12) ? C9 N3 C1 N1 -177.53(9) ? C2 N3 C1 C3 -178.41(9) ? C9 N3 C1 C3 4.36(15) ? N1 N2 C2 N3 0.74(11) ? N1 N2 C2 S1 -177.51(8) no C1 N3 C2 N2 -0.27(11) ? C9 N3 C2 N2 177.01(9) ? C1 N3 C2 S1 178.01(8) no C9 N3 C2 S1 -4.71(15) ? N1 C1 C3 C8 -94.29(13) ? N3 C1 C3 C8 83.54(13) yes N1 C1 C3 C4 87.54(13) ? N3 C1 C3 C4 -94.64(12) ? C8 C3 C4 O1 -179.29(10) no C1 C3 C4 O1 -1.12(15) ? C8 C3 C4 C5 0.70(16) ? C1 C3 C4 C5 178.87(10) ? O1 C4 C5 C6 179.70(11) no C3 C4 C5 C6 -0.29(18) ? C4 C5 C6 C7 -0.22(19) ? C5 C6 C7 C8 0.32(19) ? C6 C7 C8 C3 0.09(18) ? C4 C3 C8 C7 -0.60(17) ? C1 C3 C8 C7 -178.78(10) ? C2 N3 C9 C10 -88.28(13) ? C1 N3 C9 C10 88.49(13) yes loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 14184186 2 PubChem 719792