#------------------------------------------------------------------------------ #$Date: 2025-08-18 23:52:38 +0100 (Mon, 18 Aug 2025) $ #$Revision: 301791 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/72/2007258.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_2007258 loop_ _publ_author_name 'Hasegawa, Kazuhiro' 'Ishikawa, Kohki' 'Kawaoka, Rie' 'Sano, Chiaki' 'Iitani, Kinzo' 'Komatsu, Hiroshi' 'Nagashima, Nobuya' _publ_section_title ; Complexes Between L-Leucine and its Precipitants ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 637 _journal_page_last 641 _journal_paper_doi 10.1107/S0108270197018106 _journal_volume 54 _journal_year 1998 _chemical_formula_iupac 'C6 H14 N1 O2 1+, C7 H7 O3 S1 1-, H2 O1' _chemical_formula_moiety 'C13 H21 N O5 S, H2 O' _chemical_formula_sum 'C13 H23 N O6 S' _chemical_formula_weight 321.39 _chemical_name_systematic ; L-leucine 4-methylbenzenesulfonate monohydrate ; _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_type_scat_source IntTabIV _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.866(2) _cell_length_b 28.201(9) _cell_length_c 6.250(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 298 _cell_measurement_theta_max 40 _cell_measurement_theta_min 30 _cell_volume 1738.9(9) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988) ; _computing_data_reduction 'MSC/AFC Diffractometer Control Software' _computing_publication_material 'PLUTO (Motherwell & Clegg, 1978) and ORTEPII (Johnson, 1976)' _computing_structure_refinement 'ALLS (Lapp & Jacobson, 1979)' _computing_structure_solution 'MITHRIL (Gilmore, 1984)' _diffrn_measurement_device 'Rigaku AFC-5S' _diffrn_measurement_method \w/2\q _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2115 _diffrn_reflns_theta_max 80 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.875 _exptl_absorpt_correction_T_max 0.693 _exptl_absorpt_correction_T_min 0.575 _exptl_absorpt_correction_type 'empirical via \y scans (North et al., 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.228 _exptl_crystal_description plate _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.23 _refine_diff_density_min -0.35 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 2.86 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 189 _refine_ls_number_reflns 1806 _refine_ls_R_factor_obs .047 _refine_ls_shift/esd_max 0.04 _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 .055 _reflns_number_observed 1806 _reflns_number_total 2115 _reflns_observed_criterion I>3\s(I) _cod_data_source_file oa1024.cif _cod_data_source_block Leu_p-TS _cod_depositor_comments ; Updating space group information and adding the symmetry operation list. Antanas Vaitkus, 2018-06-18 Adding the _atom_site_type_symbol data item to prevent confusion between hydrogen and holmium. Andrius Merkys 2013-10-15 The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'w = 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_cell_volume 1739.0(10) _cod_database_code 2007258 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x+1/2,-y,z+1/2 3 x+1/2,-y+1/2,-z 4 -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 S .0498(5) .0446(5) .0714(7) -.0032(5) -.0094(6) -.0081(6) O1 .0310(10) .070(2) .071(2) .0000(10) -.008(2) -.008(2) O2 .141(4) .076(2) .182(5) .041(2) -.114(4) -.057(3) O3 .072(2) .048(2) .055(2) .0110(10) .002(2) .0030(10) O4 .155(4) .066(2) .059(2) .005(3) -.049(3) -.015(2) O5 .052(2) .077(2) .209(5) -.020(2) .027(3) -.041(3) O6 .061(2) .075(2) .049(2) -.010(2) -.006(2) .003(2) N .0330(10) .058(2) .045(2) -.0080(10) -.004(2) .006(2) C1 .030(2) .055(2) .043(2) .005(2) .001(2) .006(2) C2 .048(2) .048(2) .056(3) .001(2) -.017(2) .000(2) C3 .041(2) .071(2) .053(2) .004(2) .000(2) .016(2) C4 .060(3) .064(3) .084(4) .002(2) -.019(3) .020(3) C5 .145(6) .124(5) .150(7) .044(5) .044(6) .088(5) C6 .122(5) .108(4) .135(6) .060(4) .052(5) .029(5) C7 .038(2) .044(2) .053(2) .002(2) -.008(2) -.004(2) C8 .074(3) .063(3) .057(3) -.002(3) .000(3) -.005(2) C9 .090(4) .072(3) .065(3) .008(3) -.001(3) -.024(3) C10 .073(3) .058(3) .097(4) -.004(3) -.014(4) -.016(3) C11 .086(4) .065(3) .095(4) -.023(3) .019(4) .007(3) C12 .075(3) .059(3) .065(3) -.009(2) .011(3) -.004(2) C13 .148(6) .075(4) .183(8) -.029(4) -.002(7) -.045(5) loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z S S .19781(9) .15745(3) .9470(2) O O1 .4126(2) .23165(8) .3495(4) O O2 .5072(4) .16590(10) .2325(6) O O3 .0961(2) .18872(7) .8584(4) O O4 .1973(3) .15754(9) 1.1782(4) O O5 .3296(2) .16735(9) .8577(7) O O6 .4199(2) .26616(8) -.1562(4) N N .6319(2) .26295(9) .5349(4) C C1 .6387(3) .21380(10) .4563(6) C C2 .5059(3) .20450(10) .3421(6) C C3 .6652(3) .17980(10) .6422(6) C C4 .7021(4) .12940(10) .5887(7) C C5 .7147(6) .1006(2) .7921(9) C C6 .8318(5) .1259(2) .4626(9) C C7 .1540(3) .09960(10) .8659(6) C C8 .1883(4) .08360(10) .6664(6) C C9 .1493(4) .03850(10) .6073(7) C C10 .0761(4) .00980(10) .7361(8) C C11 .0417(4) .02670(10) .9336(8) C C12 .0805(4) .07170(10) .9992(6) C C13 .0364(6) -.03990(10) .6686(9) H H1 .7106 .2112 .3558 H HN1 .7147 .2707 .6041 H HN2 .6183 .2838 .4172 H HO2 .4447 .1599 .2026 H HN3 .5591 .2660 .6326 H H4 .6309 .1160 .5044 H H8 .2373 .1032 .5710 H H9 .1766 .0270 .4714 H H11 -.0101 .0073 1.0273 H H12 .0567 .0829 1.1369 H H31 .7378 .1924 .7239 H H32 .5856 .1787 .7273 H H51 .6334 .1022 .8715 H H52 .7372 .0690 .7604 H H53 .7868 .1142 .8785 H HO61 .3934 .2348 -.1274 H H61 .8521 .0938 .4329 H HO62 .4471 .2757 -.0437 H H62 .8242 .1432 .3330 H H63 .9044 .1393 .5456 H H131 -.0162 -.0544 .7763 H H132 -.0148 -.0383 .5389 H H133 .1161 -.0582 .6433 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O3 S O4 112.3(2) O3 S O5 111.1(2) O3 S C7 106.5(2) O4 S O5 112.9(3) O4 S C7 106.8(2) O5 S C7 106.8(2) N C1 C2 106.3(3) N C1 C3 110.2(3) C2 C1 C3 113.4(3) O1 C2 O2 124.6(4) O1 C2 C1 122.4(4) O2 C2 C1 113.0(4) C1 C3 C4 117.7(4) C3 C4 C5 110.0(5) C3 C4 C6 112.7(4) C5 C4 C6 109.6(5) S C7 C8 120.4(3) S C7 C12 119.4(3) C8 C7 C12 120.1(4) C7 C8 C9 118.5(5) C8 C9 C10 122.8(5) C9 C10 C11 117.6(5) C9 C10 C13 121.7(6) C11 C10 C13 120.7(6) C10 C11 C12 121.2(5) C7 C12 C11 119.8(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag S O3 1.447(3) yes S O4 1.445(3) yes S O5 1.442(3) yes S C7 1.763(4) yes O1 C2 1.200(4) yes O2 C2 1.285(5) yes N C1 1.472(4) yes C1 C2 1.515(5) yes C1 C3 1.529(5) yes C3 C4 1.504(6) yes C4 C5 1.512(8) yes C4 C6 1.506(7) yes C7 C8 1.370(6) yes C7 C12 1.355(6) yes C8 C9 1.379(6) yes C9 C10 1.350(7) yes C10 C11 1.367(7) yes C10 C13 1.516(6) yes C11 C12 1.386(6) yes 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 S C7 C8 C9 -178.5(4) ? S C7 C12 C11 177.8(4) ? O1 C2 C1 N -9.2(6) yes O1 C2 C1 C3 112.0(5) yes O2 C2 C1 N 168.3(4) yes O2 C2 C1 C3 -70.5(5) yes O3 S C7 C8 81.7(4) ? O3 S C7 C12 -95.4(4) ? O4 S C7 C8 -158.2(4) ? O4 S C7 C12 24.8(4) ? O5 S C7 C8 -37.1(4) ? O5 S C7 C12 145.8(4) ? N C1 C3 C4 -168.4(3) yes C1 C3 C4 C5 -176.0(5) yes C1 C3 C4 C6 61.3(6) yes C2 C1 C3 C4 72.6(5) yes C7 C8 C9 C10 1.5(8) ? C7 C12 C11 C10 0.0(8) ? C8 C7 C12 C11 0.7(7) ? C8 C9 C10 C11 -0.8(9) ? C8 C9 C10 C13 -178.9(5) ? C9 C8 C7 C12 -1.4(7) ? C9 C10 C11 C12 0.0(9) ? C12 C11 C10 C13 178.2(5) ? loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 129865871