#------------------------------------------------------------------------------ #$Date: 2025-08-18 23:52:38 +0100 (Mon, 18 Aug 2025) $ #$Revision: 301791 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/74/2007457.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_2007457 loop_ _publ_author_name 'Karczmarzyk, Zbigniew' 'Malinka, Wies\/law' _publ_section_title 4,6-Dimethyl-2-(4-phenylpiperazin-1-ylmethyl)isothiazolo[5,4-b]pyridin-3(2H)-one _journal_issue 7 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 992 _journal_page_last 994 _journal_paper_doi 10.1107/S0108270198001474 _journal_volume 54 _journal_year 1998 _chemical_formula_moiety 'C19 H22 N4 O S' _chemical_formula_sum 'C19 H22 N4 O S' _chemical_formula_weight 354.47 _chemical_name_systematic ;4,6-Dimethyl-2-(4-phenylpiperazin-1-ylmethyl)isothiazolo[5,4-b]pyridin-3-(2H)- one ; _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' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 93.010(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 17.4350(10) _cell_length_b 10.9260(10) _cell_length_c 9.089(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 50 _cell_measurement_theta_min 10 _cell_volume 1729.0(4) _computing_cell_refinement 'Kuma KM-4 software' _computing_data_collection 'Kuma KM-4 software' _computing_data_reduction 'Kuma KM-4 software' _computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 1989)' _computing_publication_material SHELXL93 _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Kuma KM-4 four-circle diffractometer' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI 0.026 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 3866 _diffrn_reflns_theta_max 80.34 _diffrn_reflns_theta_min 2.54 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 100 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 1.779 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_meas ? _exptl_crystal_description prism _exptl_crystal_F_000 752 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.298 _refine_diff_density_min -0.482 _refine_ls_extinction_coef 0.0020(4) _refine_ls_extinction_method SHELXL93 _refine_ls_goodness_of_fit_all 1.085 _refine_ls_goodness_of_fit_obs 1.148 _refine_ls_hydrogen_treatment isotropic _refine_ls_matrix_type full _refine_ls_number_parameters 315 _refine_ls_number_reflns 3402 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.085 _refine_ls_restrained_S_obs 1.148 _refine_ls_R_factor_all 0.057 _refine_ls_R_factor_obs .041 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0875P)^2^+0.1604P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.129 _refine_ls_wR_factor_obs .119 _reflns_number_observed 2653 _reflns_number_total 3402 _reflns_observed_criterion I>2sigma(I) _cod_data_source_file na1333.cif _cod_data_source_block na1333 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0875P)^2^+0.1604P] where P=(Fo^2^+2Fc^2^)/3' 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^(Fo^2^)+(0.0875P)^2^+0.1604P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2007457 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_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 .0414(3) .0458(3) .0520(3) .0004(2) .0178(2) .0011(2) N2 .0398(7) .0410(8) .0562(10) .0004(6) .0133(7) .0000(7) N7 .0410(8) .0434(8) .0517(10) -.0018(6) .0110(7) .0041(7) N21 .0345(7) .0406(7) .0443(9) .0014(6) .0024(6) -.0061(6) N24 .0395(7) .0415(7) .0383(8) .0025(6) .0036(6) -.0046(6) O3 .0478(7) .0458(8) .0807(11) -.0044(6) .0244(7) .0070(7) C3 .0338(8) .0440(9) .0469(11) -.0005(7) .0067(7) .0017(8) C4 .0306(7) .0480(10) .0436(10) -.0001(7) .0066(7) .0023(7) C5 .0397(9) .0450(10) .0525(12) .0039(7) .0105(8) -.0012(8) C6 .0403(9) .0434(10) .0536(12) .0007(7) .0082(8) .0030(8) C8 .0320(8) .0442(9) .0430(10) .0004(7) .0073(7) .0031(8) C9 .0305(7) .0416(9) .0407(9) -.0008(6) .0034(6) .0033(7) C10 .0393(9) .0536(11) .0572(12) -.0005(8) .0179(8) .0030(10) C11 .0646(14) .0446(11) .083(2) .0000(10) .0259(13) .0054(11) C12 .0365(9) .0425(9) .0607(12) -.0019(7) .0059(8) -.0067(9) C22 .0429(9) .0407(9) .0500(11) .0013(7) -.0015(8) -.0098(8) C23 .0437(9) .0453(10) .0435(11) .0042(8) .0014(7) -.0103(8) C25 .0402(9) .0485(10) .0437(11) -.0025(7) .0048(7) -.0102(8) C26 .0404(9) .0530(10) .0402(10) -.0014(8) .0042(7) -.0072(8) C31 .0413(9) .0373(8) .0441(10) .0080(7) .0050(7) .0036(7) C32 .0493(11) .0593(12) .0445(11) .0125(9) .0056(8) -.0029(9) C33 .0535(12) .078(2) .0455(12) .0221(11) .0114(9) .0027(11) C34 .0464(11) .0686(14) .0629(14) .0123(10) .0175(10) .0170(11) C35 .0445(10) .0507(11) .071(2) .0014(9) .0090(10) .0078(10) C36 .0451(10) .0467(10) .0555(13) .0007(8) .0099(8) -.0034(9) 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 _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol S1 .27543(3) .12451(4) .09510(6) .0459(2) Uani d . 1 . S N2 .32263(9) .24065(15) .0123(2) .0453(4) Uani d . 1 . N N7 .32269(9) -.10061(15) .0245(2) .0451(4) Uani d . 1 . N N21 .22108(8) .36590(14) .0828(2) .0398(3) Uani d . 1 . N N24 .06281(9) .41125(15) .1192(2) .0397(3) Uani d . 1 . N O3 .42384(8) .28497(14) -.1283(2) .0574(4) Uani d . 1 . O C3 .38311(10) .2093(2) -.0705(2) .0414(4) Uani d . 1 . C C4 .43663(10) .0000(2) -.1535(2) .0405(4) Uani d . 1 . C C5 .42647(11) -.1247(2) -.1373(2) .0455(4) Uani d . 1 . C C6 .36999(11) -.1719(2) -.0489(2) .0456(4) Uani d . 1 . C C8 .33351(10) .0196(2) .0093(2) .0396(4) Uani d . 1 . C C9 .38789(9) .0752(2) -.0754(2) .0376(4) Uani d . 1 . C C10 .49572(12) .0498(2) -.2513(3) .0495(5) Uani d . 1 . C C11 .3590(2) -.3074(2) -.0340(4) .0632(7) Uani d . 1 . C C12 .30004(11) .3671(2) .0405(3) .0465(4) Uani d . 1 . C C22 .19908(11) .4746(2) .1632(3) .0447(4) Uani d . 1 . C C23 .12146(11) .4554(2) .2266(2) .0442(4) Uani d . 1 . C C25 .08815(11) .3204(2) .0140(2) .0440(4) Uani d . 1 . C C26 .16585(11) .3518(2) -.0427(2) .0445(4) Uani d . 1 . C C31 -.01017(11) .3923(2) .1731(2) .0408(4) Uani d . 1 . C C32 -.03407(12) .4553(2) .2970(2) .0509(5) Uani d . 1 . C C33 -.10678(13) .4362(2) .3485(3) .0585(6) Uani d . 1 . C C34 -.15754(13) .3552(2) .2802(3) .0588(6) Uani d . 1 . C C35 -.13474(12) .2934(2) .1569(3) .0553(5) Uani d . 1 . C C36 -.06277(11) .3107(2) .1044(3) .0488(5) Uani d . 1 . C H51 .4551(14) -.179(2) -.179(3) .053(7) Uiso d . 1 . H H101 .5271(18) .113(3) -.200(4) .077(9) Uiso d . 1 . H H102 .472(2) .100(3) -.337(4) .096(11) Uiso d . 1 . H H103 .528(2) -.017(4) -.280(4) .107(12) Uiso d . 1 . H H111 .405(2) -.349(3) -.004(4) .095(11) Uiso d . 1 . H H112 .3302(18) -.324(3) .039(4) .075(9) Uiso d . 1 . H H113 .340(3) -.338(4) -.140(5) .126(14) Uiso d . 1 . H H121 .3327(16) .401(3) .125(3) .063(7) Uiso d . 1 . H H122 .3095(13) .418(2) -.057(3) .050(6) Uiso d . 1 . H H221 .1976(15) .549(3) .108(3) .073(8) Uiso d . 1 . H H222 .2379(14) .491(2) .238(3) .057(7) Uiso d . 1 . H H231 .1058(15) .538(2) .266(3) .066(7) Uiso d . 1 . H H232 .1252(17) .390(3) .308(4) .071(8) Uiso d . 1 . H H251 .0908(12) .241(2) .057(2) .039(5) Uiso d . 1 . H H252 .0487(14) .309(2) -.072(3) .058(7) Uiso d . 1 . H H261 .1834(14) .280(2) -.100(3) .055(6) Uiso d . 1 . H H262 .1608(14) .433(2) -.111(3) .055(6) Uiso d . 1 . H H321 .0012(15) .519(2) .350(3) .057(7) Uiso d . 1 . H H331 -.123(2) .494(4) .447(4) .109(11) Uiso d . 1 . H H341 -.2052(19) .343(3) .321(4) .087(10) Uiso d . 1 . H H351 -.1686(15) .231(3) .110(3) .060(7) Uiso d . 1 . H H361 -.0507(14) .265(2) .025(3) .054(7) Uiso d . 1 . H loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 N2 S1 C8 89.23(8) yes C3 N2 C12 123.6(2) yes C3 N2 S1 117.30(13) yes C12 N2 S1 118.93(13) yes C8 N7 C6 115.3(2) yes C12 N21 C22 113.86(15) ? C12 N21 C26 113.0(2) ? C22 N21 C26 107.33(15) ? C31 N24 C23 115.6(2) ? C31 N24 C25 116.0(2) ? C23 N24 C25 115.90(14) ? O3 C3 N2 123.1(2) yes O3 C3 C9 128.7(2) yes N2 C3 C9 108.2(2) yes C5 C4 C9 116.0(2) yes C5 C4 C10 121.2(2) yes C9 C4 C10 122.8(2) yes C4 C5 C6 121.5(2) yes N7 C6 C5 122.8(2) yes N7 C6 C11 116.4(2) yes C5 C6 C11 120.8(2) yes N7 C8 C9 126.2(2) yes N7 C8 S1 120.85(13) yes C9 C8 S1 112.92(14) yes C8 C9 C4 118.2(2) yes C8 C9 C3 112.2(2) yes C4 C9 C3 129.6(2) yes N21 C12 N2 107.82(15) ? N21 C22 C23 110.0(2) ? N24 C23 C22 113.6(2) ? N24 C25 C26 112.1(2) ? N21 C26 C25 108.8(2) ? C36 C31 C32 117.1(2) ? C36 C31 N24 121.5(2) ? C32 C31 N24 121.4(2) ? C33 C32 C31 120.8(2) ? C34 C33 C32 121.4(2) ? C33 C34 C35 118.3(2) ? C36 C35 C34 121.2(2) ? C35 C36 C31 121.3(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 N2 . 1.709(2) yes S1 C8 . 1.741(2) yes N2 C3 . 1.371(2) yes N2 C12 . 1.463(2) ? N7 C8 . 1.335(2) yes N7 C6 . 1.338(3) yes N21 C12 . 1.449(2) ? N21 C22 . 1.457(2) ? N21 C26 . 1.462(2) ? N24 C31 . 1.403(2) ? N24 C23 . 1.458(2) ? N24 C25 . 1.463(2) ? O3 C3 . 1.226(2) yes C3 C9 . 1.468(3) yes C4 C5 . 1.382(3) yes C4 C9 . 1.402(2) yes C4 C10 . 1.498(2) yes C5 C6 . 1.401(3) yes C6 C11 . 1.499(3) yes C8 C9 . 1.392(2) yes C22 C23 . 1.513(3) ? C25 C26 . 1.514(3) ? C31 C36 . 1.402(3) ? C31 C32 . 1.402(3) ? C32 C33 . 1.390(3) ? C33 C34 . 1.376(4) ? C34 C35 . 1.385(4) ? C35 C36 . 1.378(3) ? 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 C10 H103 O3 2_644 0.96(4) 2.48(4) 3.420(3) 164(3) C34 H341 N7 2_555 0.94(4) 2.62(4) 3.495(3) 156(3) 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 C8 S1 N2 C3 -3.7(2) C8 S1 N2 C12 -179.9(2) C12 N2 C3 O3 0.1(3) S1 N2 C3 O3 -175.9(2) C12 N2 C3 C9 -179.6(2) S1 N2 C3 C9 4.5(2) C9 C4 C5 C6 0.7(3) C10 C4 C5 C6 -178.4(2) C8 N7 C6 C5 -0.8(3) C8 N7 C6 C11 -179.9(2) C4 C5 C6 N7 0.1(3) C4 C5 C6 C11 179.2(2) C6 N7 C8 C9 0.7(3) C6 N7 C8 S1 178.8(2) N2 S1 C8 N7 -176.6(2) N2 S1 C8 C9 1.73(15) N7 C8 C9 C4 0.1(3) S1 C8 C9 C4 -178.15(14) N7 C8 C9 C3 178.7(2) S1 C8 C9 C3 0.4(2) C5 C4 C9 C8 -0.8(3) C10 C4 C9 C8 178.3(2) C5 C4 C9 C3 -179.0(2) C10 C4 C9 C3 0.0(3) O3 C3 C9 C8 177.4(2) N2 C3 C9 C8 -2.9(2) O3 C3 C9 C4 -4.2(4) N2 C3 C9 C4 175.4(2) C22 N21 C12 N2 159.4(2) C26 N21 C12 N2 -77.9(2) C3 N2 C12 N21 159.6(2) S1 N2 C12 N21 -24.5(2) C12 N21 C22 C23 -169.6(2) C26 N21 C22 C23 64.6(2) C31 N24 C23 C22 -179.9(2) C25 N24 C23 C22 39.4(2) N21 C22 C23 N24 -50.4(2) C31 N24 C25 C26 177.5(2) C23 N24 C25 C26 -42.0(2) C12 N21 C26 C25 166.2(2) C22 N21 C26 C25 -67.4(2) N24 C25 C26 N21 55.7(2) C23 N24 C31 C36 -155.9(2) C25 N24 C31 C36 -15.2(3) C23 N24 C31 C32 24.9(3) C25 N24 C31 C32 165.5(2) C36 C31 C32 C33 0.3(3) N24 C31 C32 C33 179.5(2) C31 C32 C33 C34 0.1(3) C32 C33 C34 C35 -0.7(3) C33 C34 C35 C36 0.9(4) C34 C35 C36 C31 -0.6(4) C32 C31 C36 C35 0.0(3) N24 C31 C36 C35 -179.3(2) loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 353892 2 PubChem 399235