#------------------------------------------------------------------------------ #$Date: 2025-08-19 07:12:48 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301798 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/04/2010447.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_2010447 loop_ _publ_author_name 'Kokila, M.K.' Puttaraja 'Kulkarni, M.V.' 'Thampi, S.' _publ_section_title ; 3,4,5-Trimethoxybenzaldehyde Thiosemicarbazone Monohydrate ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 330 _journal_page_last 333 _journal_paper_doi 10.1107/S0108270193014015 _journal_volume 51 _journal_year 1995 _chemical_formula_moiety 'C11 H15 N3 O3 S1,H2 O1' _chemical_formula_sum 'C11 H17 N3 O4 S' _chemical_formula_weight 287.33 _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_type_scat_source IntTabIV _cell_angle_alpha 73.29(2) _cell_angle_beta 70.89(2) _cell_angle_gamma 70.49(2) _cell_formula_units_Z 2 _cell_length_a 7.4280(10) _cell_length_b 9.6520(10) _cell_length_c 11.102(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 300 _cell_measurement_theta_max 25 _cell_measurement_theta_min 0 _cell_volume 694.6(2) _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_reflns_av_R_equivalents 0.000(11) _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 2767 _diffrn_reflns_theta_max 65 _diffrn_standards_decay_% none _diffrn_standards_interval_count 50 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.17 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_meas 1.359 _exptl_crystal_description needle _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.25 _refine_diff_density_max 0.28 _refine_diff_density_min -0.20 _refine_ls_extinction_coef 0.85(2) _refine_ls_extinction_method secondary _refine_ls_goodness_of_fit_obs 1.92 _refine_ls_hydrogen_treatment refU _refine_ls_number_parameters 240 _refine_ls_R_factor_obs 0.036 _refine_ls_shift/esd_max 0.159 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/\s^2^(F)' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.039 _reflns_number_observed 2398 _reflns_number_total 2528 _reflns_observed_criterion I>=2.5\s(I) _cod_data_source_file cr1072.cif _cod_data_source_block cr1072_structure_1_of_1 _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value '1/\s^2^(F)' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/\s^2^(F)'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_formula_sum 'C11 H17 N3 O4 S1' _cod_database_code 2010447 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,-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 S 0.0445(3) 0.0310(3) 0.0266(3) -0.0137(2) 0.0063(2) -0.0018(2) O(W) 0.0522(11) 0.0554(11) 0.0429(10) -0.0027(8) -0.0001(9) -0.0125(8) O(1) 0.0507(9) 0.0324(8) 0.0347(8) -0.0191(7) -0.0002(7) -0.0039(6) O(2) 0.0566(10) 0.0398(9) 0.0269(7) -0.0132(7) 0.0037(7) -0.0116(6) O(3) 0.0426(9) 0.0423(9) 0.0270(7) -0.0126(7) 0.0059(6) 0.0013(6) N(1) 0.0388(10) 0.0334(9) 0.0247(8) -0.0132(7) 0.0013(7) -0.0020(7) N(2) 0.0431(10) 0.0285(9) 0.0264(8) -0.0112(8) 0.0048(7) -0.0036(7) N(3) 0.0564(13) 0.0302(10) 0.0453(11) -0.0147(9) 0.0158(10) -0.0090(8) C(1) 0.0317(10) 0.0314(10) 0.0261(9) -0.0085(8) -0.0033(8) -0.0031(8) C(2) 0.0393(11) 0.0297(11) 0.0280(10) -0.0107(9) -0.0033(8) -0.0041(8) C(3) 0.0356(11) 0.0350(11) 0.0236(9) -0.0064(8) -0.0019(8) -0.0064(8) C(4) 0.0330(11) 0.0348(11) 0.0235(9) -0.0095(8) 0.0002(8) -0.0011(8) C(5) 0.0324(10) 0.0289(10) 0.0310(10) -0.0088(8) -0.0053(8) -0.0026(8) C(6) 0.0358(11) 0.0314(10) 0.0250(9) -0.0090(8) -0.0018(8) -0.0055(8) C(7) 0.0372(11) 0.0321(11) 0.0265(10) -0.0109(9) -0.0016(8) -0.0046(8) C(8) 0.0405(12) 0.0324(11) 0.0262(9) -0.0128(9) -0.0036(8) -0.0046(8) C(9) 0.0547(16) 0.0457(14) 0.0429(14) -0.0126(12) -0.0051(12) -0.0186(11) C(10) 0.075(2) 0.0601(18) 0.0311(13) -0.0097(15) -0.0041(13) 0.0099(12) C(11) 0.0541(15) 0.0376(13) 0.0477(14) -0.0165(11) -0.0039(12) -0.0141(11) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z S .28610(10) .20320(10) .07250(10) O(W) .1342(3) .65140(10) .0194 O(1) .7992(2) 1.0191(2) -.5415(2) O(2) .9153(2) .5923(2) -.70170(10) O(3) .9685(2) .8582(2) -.7312(3) N(1) .5518(3) .4656(2) -.2180(2) N(2) .4337(3) .4147(2) -.1003(2) N(3) .6005(3) .1768(2) -.1294(2) C(1) .6442(3) .6724(2) -.3755(2) C(2) .7278(3) .5934(2) -.4767(2) C(3) .8300(3) .6583(2) -.5956(2) C(4) .8541(3) .8014(2) -.6149(2) C(5) .7683(3) .8808(2) -.5141(2) C(6) .6630(3) .8167(2) -.3956(2) C(7) .5376(3) .6062(2) -.2484(2) C(8) .4505(3) .2667(2) -.0607(2) C(9) .8925(4) .4471(3) -.6876(3) C(10) .8611(5) .9752(4) -.8148(3) C(11) .7267(4) 1.0985(3) -.4373(3) H(2) .711(3) .494(3) -.460(2) H(6) .613(4) .865(3) -.325(3) H(7) .454(4) .671(3) -.189(3) H(N2) .335(4) .475(3) -.055(3) H(N3A) .699(4) .218(3) -.199(3) H(N3B) .609(5) .082(4) -.099(3) H(9A) .940(4) .375(3) -.612(3) H(9B) .747(4) .449(3) -.661(3) H(9C) .950(5) .425(3) -.780(3) H(10A) .790(6) .925(4) -.842(4) H(10B) .781(6) 1.054(4) -.770(4) H(10C) .956(5) 1.012(4) -.888(3) H(11A) .575(4) 1.118(3) -.400(3) H(11B) .783(4) 1.038(3) -.359(3) H(11C) .780(4) 1.192(3) -.475(3) H(OWA) .250(6) .667(4) -.033(4) H(OWB) .081(6) .692(4) .083(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 C(5) O(1) C(11) 117.0(2) yes C(4) O(3) C(10) 115.0(2) yes N(1) N(2) C(8) 119.0(2) yes C(2) C(1) C(7) 121.0(2) yes C(1) C(2) C(3) 119.7(2) yes O(2) C(3) C(4) 114.8(2) yes O(3) C(4) C(3) 119.0(2) yes C(3) C(4) C(5) 119.6(2) yes O(1) C(5) C(6) 124.6(2) yes C(1) C(6) C(5) 120.5(2) yes S C(8) N(2) 120.0(2) yes N(2) C(8) N(3) 117.0(2) yes C(3) O(2) C(9) 117.0(2) yes N(2) N(1) C(7) 116.6(2) yes C(2) C(1) C(6) 119.9(2) yes C(6) C(1) C(7) 119.1(2) yes O(2) C(3) C(2) 124.7(2) yes C(2) C(3) C(4) 120.5(2) yes O(3) C(4) C(5) 121.3(2) yes O(1) C(5) C(4) 115.6(2) yes C(4) C(5) C(6) 120.0(2) yes N(1) C(7) C(1) 120.6(2) yes S C(8) N(3) 123.1(2) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag S C(8) 1.688(2) yes C(2) C(3) 1.378(3) yes O(1) C(5) 1.361(2) yes O(1) C(11) 1.429(3) yes O(2) C(3) 1.367(2) yes O(2) C(9) 1.426(3) yes O(3) C(10) 1.434(3) yes N(1) C(7) 1.277(3) yes N(3) C(8) 1.325(3) yes C(1) C(2) 1.396(3) yes C(1) C(6) 1.392(3) yes C(3) C(4) 1.398(3) yes C(4) C(5) 1.396(3) yes C(5) C(6) 1.380(3) yes O(3) C(4) 1.370(2) yes N(1) N(2) 1.374(2) yes N(2) C(8) 1.343(3) yes C(1) C(7) 1.454(3) yes loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139057489