#------------------------------------------------------------------------------ #$Date: 2025-08-19 07:12:48 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301798 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/15/2011504.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_2011504 loop_ _publ_author_name 'Wu, De-Hong' 'He, Cheng' 'Duan, Chun-Ying' 'You, Xiao-Zeng' _publ_section_title ; Terephthalaldehyde bis(thiosemicarbazone) bis(dimethylformamide) solvate ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1336 _journal_page_last 1337 _journal_paper_doi 10.1107/S0108270100009914 _journal_volume 56 _journal_year 2000 _chemical_formula_analytical 'C10 H12 N6 S2, 2C3 H7 N O' _chemical_formula_iupac 'C10 H12 N6 S2, 2C3 H7 N O' _chemical_formula_moiety 'C10 H12 N6 S2, 2C3 H7 N O' _chemical_formula_sum 'C16 H26 N8 O2 S2' _chemical_formula_weight 426.56 _chemical_name_systematic ; Terephthaldehyde Thiosemicarbazone Bis-N,N-Dimethylformamide ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 94.753(19) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 28.227(6) _cell_length_b 5.991(3) _cell_length_c 12.873(3) _cell_measurement_reflns_used 32 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 11.74 _cell_measurement_theta_min 5.18 _cell_volume 2169.4(13) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Siemens, 1994)' _computing_data_reduction 'SHELXTL (Siemens, 1995)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution SHELXTL _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .997 _diffrn_measured_fraction_theta_max .997 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .028 _diffrn_reflns_av_sigmaI/netI .0307 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 2412 _diffrn_reflns_theta_full 25.01 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_min 2.90 _diffrn_standards_decay_% 9.1 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu .274 _exptl_absorpt_correction_T_max .938 _exptl_absorpt_correction_T_min .817 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 904 _exptl_crystal_size_max .50 _exptl_crystal_size_mid .40 _exptl_crystal_size_min .40 _refine_diff_density_max .175 _refine_diff_density_min -.191 _refine_ls_extinction_coef .0036(6) _refine_ls_extinction_method SHELXTL _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 130 _refine_ls_number_reflns 1902 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.027 _refine_ls_R_factor_all .048 _refine_ls_R_factor_gt .038 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0519P)^2^+1.5245P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .110 _reflns_number_gt 1578 _reflns_number_total 1902 _reflns_threshold_expression I>2\s(I) _cod_data_source_file fr1278.cif _cod_data_source_block I _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_cell_volume 2169.2(14) _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2011504 _cod_database_fobs_code 2011504 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' '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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol S1 .35205(2) .36673(11) .07922(4) .0621(2) Uani d . 1 . . S N2 .40444(6) .5453(3) .23451(12) .0485(4) Uani d . 1 . . N H2A .3976 .4289 .2695 .058 Uiso calc R 1 . . H N3 .43213(6) .7111(3) .28144(12) .0446(4) Uani d . 1 . . N C1 .38788(7) .5650(3) .13336(14) .0439(5) Uani d . 1 . . C C2 .44279(7) .6859(3) .37899(15) .0437(5) Uani d . 1 . . C H2B .4318 .5605 .4122 .052 Uiso calc R 1 . . H C3 .47171(6) .8491(3) .43953(14) .0399(4) Uani d . 1 . . C C4 .48568(7) .8044(3) .54390(15) .0439(5) Uani d . 1 . . C H4A .4758 .6731 .5740 .053 Uiso calc R 1 . . H C5 .51387(7) .9517(4) .60303(14) .0439(5) Uani d . 1 . . C H5A .5233 .9176 .6721 .053 Uiso calc R 1 . . H O1 .36653(6) .2122(3) .36084(11) .0607(4) Uani d . 1 . . O N1 .40164(7) .7407(3) .08186(13) .0557(5) Uani d . 1 . . N H1A .4204 .8372 .1128 .067 Uiso calc R 1 . . H H1B .3918 .7586 .0174 .067 Uiso calc R 1 . . H C6 .34432(8) .0553(4) .31922(16) .0515(5) Uani d . 1 . . C H6A .3553 -.0029 .2587 .062 Uiso calc R 1 . . H C7 .28523(10) -.2362(5) .3057(2) .0790(8) Uani d . 1 . . C H7A .3002 -.2703 .2433 .118 Uiso calc R 1 . . H H7B .2519 -.2121 .2888 .118 Uiso calc R 1 . . H H7C .2896 -.3586 .3537 .118 Uiso calc R 1 . . H C8 .28567(9) .0517(5) .44367(18) .0655(7) Uani d . 1 . . C H8A .2972 .2005 .4571 .098 Uiso calc R 1 . . H H8B .2945 -.0411 .5030 .098 Uiso calc R 1 . . H H8C .2517 .0545 .4311 .098 Uiso calc R 1 . . H N4 .30630(6) -.0372(3) .35294(14) .0504(4) Uani d . 1 . . N 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 .0673(4) .0664(4) .0499(3) -.0247(3) -.0115(3) -.0082(3) N2 .0561(10) .0481(10) .0396(9) -.0160(8) -.0065(7) -.0019(7) N3 .0439(9) .0478(10) .0408(9) -.0097(8) -.0036(7) -.0069(7) C1 .0415(10) .0498(12) .0398(10) -.0024(9) -.0006(8) -.0065(9) C2 .0450(10) .0447(11) .0405(10) -.0057(9) -.0019(8) -.0027(8) C3 .0365(9) .0453(11) .0374(9) -.0027(8) .0000(7) -.0054(8) C4 .0465(11) .0442(11) .0402(10) -.0070(9) -.0006(8) .0014(8) C5 .0441(10) .0535(12) .0328(9) -.0031(9) -.0042(8) -.0004(8) O1 .0712(10) .0615(10) .0481(8) -.0182(8) -.0019(7) -.0005(7) N1 .0665(12) .0577(12) .0410(9) -.0169(9) -.0069(8) -.0004(8) C6 .0566(12) .0524(12) .0445(11) .0028(11) -.0016(9) -.0007(10) C7 .0757(18) .0635(17) .095(2) -.0135(14) -.0060(15) -.0126(14) C8 .0620(14) .0714(16) .0639(14) .0086(13) .0101(11) .0034(12) N4 .0514(10) .0440(10) .0549(10) .0012(8) -.0007(8) -.0011(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 N2 N3 . . 119.96(17) yes C1 N2 H2A . . 120.0 . N3 N2 H2A . . 120.0 ? C2 N3 N2 . . 115.25(17) yes N1 C1 N2 . . 117.45(18) yes N1 C1 S1 . . 123.34(15) yes N2 C1 S1 . . 119.20(16) yes N3 C2 C3 . . 121.53(19) yes N3 C2 H2B . . 119.2 ? C3 C2 H2B . . 119.2 ? C5 C3 C4 5_676 . 118.44(18) ? C5 C3 C2 5_676 . 122.35(17) ? C4 C3 C2 . . 119.21(18) yes C5 C4 C3 . . 120.99(19) yes C5 C4 H4A . . 119.5 ? C3 C4 H4A . . 119.5 ? C4 C5 C3 . 5_676 120.56(18) ? C4 C5 H5A . . 119.7 ? C3 C5 H5A 5_676 . 119.7 ? C1 N1 H1A . . 120.0 ? C1 N1 H1B . . 120.0 ? H1A N1 H1B . . 120.0 ? O1 C6 N4 . . 125.5(2) ? O1 C6 H6A . . 117.3 ? N4 C6 H6A . . 117.3 ? N4 C7 H7A . . 109.5 ? N4 C7 H7B . . 109.5 ? H7A C7 H7B . . 109.5 ? N4 C7 H7C . . 109.5 ? H7A C7 H7C . . 109.5 ? H7B C7 H7C . . 109.5 ? N4 C8 H8A . . 109.5 ? N4 C8 H8B . . 109.5 ? H8A C8 H8B . . 109.5 ? N4 C8 H8C . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? C6 N4 C7 . . 121.9(2) ? C6 N4 C8 . . 120.4(2) ? C7 N4 C8 . . 117.6(2) ? 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 S1 C1 . 1.674(2) yes N2 C1 . 1.352(2) yes N2 N3 . 1.373(2) yes N2 H2A . .8600 ? N3 C2 . 1.276(2) yes C1 N1 . 1.319(3) yes C2 C3 . 1.457(3) yes C2 H2B . .9300 ? C3 C5 5_676 1.388(3) ? C3 C4 . 1.394(3) yes C4 C5 . 1.375(3) yes C4 H4A . .9300 ? C5 C3 5_676 1.388(3) ? C5 H5A . .9300 ? O1 C6 . 1.228(3) ? N1 H1A . .8600 ? N1 H1B . .8600 ? C6 N4 . 1.313(3) ? C6 H6A . .9300 ? C7 N4 . 1.444(3) ? C7 H7A . .9600 ? C7 H7B . .9600 ? C7 H7C . .9600 ? C8 N4 . 1.449(3) ? C8 H8A . .9600 ? C8 H8B . .9600 ? C8 H8C . .9600 ? loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139057992