#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/02/2200281.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_2200281 loop_ _publ_author_name 'Troup, Susan D.' 'Ward, Mark F.' 'Jaspars, Marcel' 'Harrison, William T. A.' _publ_section_title ; S-Benzyl-L-cysteine ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o535 _journal_page_last o537 _journal_paper_doi 10.1107/S1600536801008340 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac 'C10 H13 N O2 S' _chemical_formula_moiety 'C10 H13 N O2 S' _chemical_formula_sum 'C10 H13 N O2 S' _chemical_formula_weight 211.28 _chemical_melting_point 481 _chemical_name_systematic S-benzyl-L-cysteine _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 94.8950(9) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.4224(2) _cell_length_b 5.09470(10) _cell_length_c 21.5510(7) _cell_measurement_reflns_used 18971 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 2.91 _cell_volume 1030.77(4) _computing_cell_refinement 'KappaCCD Software' _computing_data_collection 'KappaCCD Software (Nonius, 1999)' _computing_data_reduction 'KappaCCD Software' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .994 _diffrn_measured_fraction_theta_max .994 _diffrn_measurement_device_type 'Enraf-Nonius KappaCCD' _diffrn_measurement_method 'combination of \w and \f scans' _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 .1588 _diffrn_reflns_av_sigmaI/netI .1380 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 12824 _diffrn_reflns_theta_full 27.51 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_min 3.00 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu .287 _exptl_absorpt_correction_T_max .989 _exptl_absorpt_correction_T_min .987 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SORTAV; Enraf-Nonius, 1999)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_description rod _exptl_crystal_F_000 448 _exptl_crystal_size_max .10 _exptl_crystal_size_mid .05 _exptl_crystal_size_min .04 _refine_diff_density_max .418 _refine_diff_density_min -.536 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -.19(10) _refine_ls_extinction_coef .011(4) _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref .994 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 254 _refine_ls_number_reflns 4668 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all .994 _refine_ls_R_factor_all .095 _refine_ls_R_factor_gt .062 _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^)+(0.0732P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .160 _reflns_number_gt 3425 _reflns_number_total 4668 _reflns_threshold_expression I>2\s(I) _cod_data_source_file bt6050.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 2200281 _cod_database_fobs_code 2200281 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' 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 .46331(10) 1.11851(18) .21713(4) .0267(3) Uani d . 1 . . S O1 .1623(2) .8349(5) .04598(11) .0207(6) Uani d . 1 . . O O2 .2276(3) .4435(5) .08454(12) .0240(6) Uani d . 1 . . O N1 .4283(3) 1.0318(5) .07619(12) .0172(6) Uani d . 1 . . N H1A .3756 1.1752 .0825 .021 Uiso calc R 1 . . H H1B .4202 .9908 .0354 .021 Uiso calc R 1 . . H H1C .5202 1.0645 .0887 .021 Uiso calc R 1 . . H C1 .2457(4) .6805(7) .07759(15) .0168(8) Uani d . 1 . . C C2 .3768(4) .8085(7) .11256(15) .0174(8) Uani d . 1 . . C H21 .4528 .6779 .1195 .021 Uiso calc R 1 . . H C3 .3335(4) .9074(8) .17537(15) .0205(8) Uani d . 1 . . C H31 .3167 .7570 .2013 .025 Uiso calc R 1 . . H H32 .2444 1.0025 .1684 .025 Uiso calc R 1 . . H C4 .6018(4) .8877(9) .24731(16) .0284(9) Uani d . 1 . . C H41 .5912 .7247 .2241 .034 Uiso calc R 1 . . H H42 .6946 .9602 .2408 .034 Uiso calc R 1 . . H C5 .5953(4) .8308(8) .31577(17) .0265(9) Uani d . 1 . . C C6 .6746(5) .9809(11) .35949(19) .0433(11) Uani d . 1 . . C H61 .7327 1.1148 .3468 .052 Uiso calc R 1 . . H C7 .6668(6) .9295(11) .4233(2) .0534(14) Uani d . 1 . . C H71 .7204 1.0298 .4527 .064 Uiso calc R 1 . . H C8 .5814(5) .7341(10) .4423(2) .0458(12) Uani d . 1 . . C H81 .5771 .7017 .4846 .055 Uiso calc R 1 . . H C9 .5016(5) .5851(10) .39901(19) .0450(11) Uani d . 1 . . C H91 .4424 .4532 .4118 .054 Uiso calc R 1 . . H C10 .5103(5) .6335(9) .33596(19) .0398(10) Uani d . 1 . . C H101 .4575 .5306 .3068 .048 Uiso calc R 1 . . H S2 -.08617(12) .37634(18) .21438(4) .0309(3) Uani d . 1 . . S O3 -.3769(2) .5097(5) .05489(11) .0196(5) Uani d . 1 . . O O4 -.2800(2) .1397(5) .09592(11) .0204(5) Uani d . 1 . . O N2 -.1222(3) .7327(6) .04447(13) .0171(6) Uani d . 1 . . N H2A -.1790 .8639 .0554 .021 Uiso calc R 1 . . H H2B -.1514 .6775 .0058 .021 Uiso calc R 1 . . H H2C -.0319 .7907 .0452 .021 Uiso calc R 1 . . H C11 -.2744(3) .3746(7) .07859(15) .0168(7) Uani d . 1 . . C C12 -.1296(4) .5098(7) .08928(15) .0175(7) Uani d . 1 . . C H121 -.0546 .3829 .0821 .021 Uiso calc R 1 . . H C13 -.1006(4) .6252(8) .15456(15) .0219(7) Uani d . 1 . . C H131 -.1770 .7448 .1625 .026 Uiso calc R 1 . . H H132 -.0127 .7253 .1565 .026 Uiso calc R 1 . . H C14 -.0065(5) .5798(9) .27778(16) .0354(10) Uani d . 1 . . C H141 .0712 .6818 .2634 .042 Uiso calc R 1 . . H H142 -.0771 .7005 .2914 .042 Uiso calc R 1 . . H C15 .0484(4) .4066(8) .33126(17) .0271(9) Uani d . 1 . . C C16 .1598(4) .2400(10) .3240(2) .0394(11) Uani d . 1 . . C H161 .2009 .2355 .2863 .047 Uiso calc R 1 . . H C17 .2123(5) .0764(11) .3729(2) .0503(13) Uani d . 1 . . C H171 .2875 -.0374 .3677 .060 Uiso calc R 1 . . H C18 .1520(5) .0858(11) .4282(2) .0476(13) Uani d . 1 . . C H181 .1865 -.0224 .4608 .057 Uiso calc R 1 . . H C19 .0422(6) .2517(10) .43601(19) .0459(12) Uani d . 1 . . C H191 .0024 .2568 .4740 .055 Uiso calc R 1 . . H C20 -.0112(5) .4134(9) .38788(19) .0366(10) Uani d . 1 . . C H201 -.0867 .5261 .3935 .044 Uiso calc R 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 .0342(5) .0315(5) .0134(5) -.0019(5) -.0045(4) -.0061(4) O1 .0178(12) .0269(13) .0165(13) -.0021(11) -.0040(10) .0047(11) O2 .0238(14) .0217(13) .0259(15) -.0008(11) -.0019(11) .0004(11) N1 .0185(14) .0240(16) .0085(14) -.0041(13) -.0017(11) -.0034(12) C1 .0179(17) .0223(19) .0107(17) .0007(14) .0039(13) -.0025(14) C2 .0211(17) .0197(18) .0109(17) .0000(14) -.0016(14) .0001(13) C3 .0182(17) .031(2) .0126(17) .0004(17) .0007(13) -.0023(16) C4 .0258(19) .043(2) .0153(18) .0034(19) -.0034(14) -.0037(19) C5 .029(2) .035(2) .0149(19) .0086(18) -.0031(15) -.0063(17) C6 .043(3) .058(3) .026(2) -.006(2) -.0104(19) -.005(2) C7 .071(3) .067(4) .018(2) -.004(3) -.017(2) -.012(2) C8 .067(3) .050(3) .020(2) .018(3) -.002(2) -.001(2) C9 .070(3) .041(3) .024(2) .001(3) .003(2) .004(2) C10 .059(3) .037(2) .022(2) -.001(2) -.0042(19) -.005(2) S2 .0453(6) .0316(5) .0138(5) -.0124(5) -.0096(4) .0055(4) O3 .0158(12) .0295(13) .0132(12) .0004(11) -.0002(9) .0004(11) O4 .0230(13) .0199(12) .0181(13) -.0023(11) .0002(10) -.0002(11) N2 .0153(14) .0229(14) .0127(15) -.0026(13) -.0007(11) -.0004(12) C11 .0163(17) .0243(18) .0100(16) -.0012(16) .0025(13) -.0029(16) C12 .0208(18) .0190(16) .0125(17) .0000(15) -.0007(14) .0020(14) C13 .0313(19) .0227(16) .0108(17) -.0074(19) -.0035(14) .0017(17) C14 .050(2) .041(2) .014(2) -.006(2) -.0077(18) -.0020(19) C15 .035(2) .030(2) .0150(18) -.0072(18) -.0062(15) -.0006(17) C16 .035(2) .057(3) .026(2) -.005(2) -.0008(19) -.005(2) C17 .043(3) .060(3) .045(3) .013(3) -.013(2) .001(3) C18 .061(3) .053(3) .025(2) -.002(3) -.017(2) .010(2) C19 .070(3) .053(3) .015(2) -.009(3) .005(2) .003(2) C20 .045(2) .044(3) .021(2) .003(2) .0019(18) -.007(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 C3 S1 C4 103.04(18) yes C2 N1 H1A 109.5 ? C2 N1 H1B 109.5 ? H1A N1 H1B 109.5 ? C2 N1 H1C 109.5 ? H1A N1 H1C 109.5 ? H1B N1 H1C 109.5 ? O2 C1 O1 126.0(3) yes O2 C1 C2 118.1(3) yes O1 C1 C2 115.8(3) yes N1 C2 C3 109.8(3) yes N1 C2 C1 110.6(3) yes C3 C2 C1 108.1(3) yes N1 C2 H21 109.5 ? C3 C2 H21 109.5 ? C1 C2 H21 109.5 ? C2 C3 S1 114.6(2) yes C2 C3 H31 108.6 ? S1 C3 H31 108.6 ? C2 C3 H32 108.6 ? S1 C3 H32 108.6 ? H31 C3 H32 107.6 ? C5 C4 S1 112.5(3) yes C5 C4 H41 109.1 ? S1 C4 H41 109.1 ? C5 C4 H42 109.1 ? S1 C4 H42 109.1 ? H41 C4 H42 107.8 ? C10 C5 C6 118.9(4) ? C10 C5 C4 121.4(4) ? C6 C5 C4 119.7(4) ? C5 C6 C7 119.5(5) ? C5 C6 H61 120.2 ? C7 C6 H61 120.2 ? C8 C7 C6 120.7(5) ? C8 C7 H71 119.7 ? C6 C7 H71 119.7 ? C7 C8 C9 120.1(4) ? C7 C8 H81 120.0 ? C9 C8 H81 120.0 ? C8 C9 C10 119.4(5) ? C8 C9 H91 120.3 ? C10 C9 H91 120.3 ? C5 C10 C9 121.5(4) ? C5 C10 H101 119.3 ? C9 C10 H101 119.3 ? C13 S2 C14 97.86(17) yes C12 N2 H2A 109.5 ? C12 N2 H2B 109.5 ? H2A N2 H2B 109.5 ? C12 N2 H2C 109.5 ? H2A N2 H2C 109.5 ? H2B N2 H2C 109.5 ? O4 C11 O3 126.3(3) yes O4 C11 C12 116.4(3) yes O3 C11 C12 117.3(3) yes N2 C12 C13 106.7(3) yes N2 C12 C11 109.6(3) yes C13 C12 C11 113.6(3) yes N2 C12 H121 109.0 ? C13 C12 H121 109.0 ? C11 C12 H121 109.0 ? C12 C13 S2 112.6(3) yes C12 C13 H131 109.1 ? S2 C13 H131 109.1 ? C12 C13 H132 109.1 ? S2 C13 H132 109.1 ? H131 C13 H132 107.8 ? C15 C14 S2 109.4(3) yes C15 C14 H141 109.8 ? S2 C14 H141 109.8 ? C15 C14 H142 109.8 ? S2 C14 H142 109.8 ? H141 C14 H142 108.2 ? C16 C15 C20 119.2(4) ? C16 C15 C14 119.5(4) ? C20 C15 C14 121.3(4) ? C15 C16 C17 120.6(4) ? C15 C16 H161 119.7 ? C17 C16 H161 119.7 ? C18 C17 C16 119.3(5) ? C18 C17 H171 120.3 ? C16 C17 H171 120.3 ? C19 C18 C17 120.6(4) ? C19 C18 H181 119.7 ? C17 C18 H181 119.7 ? C18 C19 C20 120.6(4) ? C18 C19 H191 119.7 ? C20 C19 H191 119.7 ? C19 C20 C15 119.7(4) ? C19 C20 H201 120.1 ? C15 C20 H201 120.1 ? 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 C3 . 1.810(3) yes S1 C4 . 1.834(4) yes O1 C1 . 1.268(4) yes O2 C1 . 1.230(4) yes N1 C2 . 1.486(4) yes N1 H1A . .9000 ? N1 H1B . .9000 ? N1 H1C . .9000 ? C1 C2 . 1.536(4) yes C2 C3 . 1.532(5) yes C2 H21 . .9800 ? C3 H31 . .9700 ? C3 H32 . .9700 ? C4 C5 . 1.510(5) yes C4 H41 . .9700 ? C4 H42 . .9700 ? C5 C10 . 1.379(6) ? C5 C6 . 1.382(6) ? C6 C7 . 1.407(6) ? C6 H61 . .9300 ? C7 C8 . 1.365(7) ? C7 H71 . .9300 ? C8 C9 . 1.375(6) ? C8 H81 . .9300 ? C9 C10 . 1.390(6) ? C9 H91 . .9300 ? C10 H101 . .9300 ? S2 C13 . 1.805(4) yes S2 C14 . 1.825(4) yes O3 C11 . 1.258(4) yes O4 C11 . 1.256(4) yes N2 C12 . 1.496(4) yes N2 H2A . .9000 ? N2 H2B . .9000 ? N2 H2C . .9000 ? C11 C12 . 1.528(5) yes C12 C13 . 1.528(5) yes C12 H121 . .9800 ? C13 H131 . .9700 ? C13 H132 . .9700 ? C14 C15 . 1.508(5) yes C14 H141 . .9700 ? C14 H142 . .9700 ? C15 C16 . 1.369(6) ? C15 C20 . 1.386(6) ? C16 C17 . 1.399(6) ? C16 H161 . .9300 ? C17 C18 . 1.365(7) ? C17 H171 . .9300 ? C18 C19 . 1.358(7) ? C18 H181 . .9300 ? C19 C20 . 1.385(6) ? C19 H191 . .9300 ? C20 H201 . .9300 ? 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 _geom_hbond_publ_flag N1 H1A O2 1_565 .90 1.96 2.841(4) 166.9 yes N1 H1C O4 1_665 .90 1.91 2.800(3) 167.3 yes N1 H1B O3 2 .90 1.96 2.827(3) 162.3 yes N2 H2A O4 1_565 .90 1.95 2.832(4) 168.1 yes N2 H2C O1 . .90 1.84 2.729(4) 167.8 yes N2 H2B O1 2_545 .90 2.07 2.815(4) 139.5 yes N2 H2B O2 2 .90 2.43 3.066(4) 127.8 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 C1 C2 C3 S1 -168.9(2) yes C2 C3 S1 C4 -75.2(3) ? C3 S1 C4 C5 -103.1(3) yes N1 C2 C3 S1 -48.2(3) yes O1 C1 C2 C3 85.7(3) ? O2 C1 C2 C3 -91.3(4) ? C11 C12 C13 S2 65.5(3) yes C12 C13 S2 C14 165.5(3) ? C13 S2 C14 C15 -167.3(3) yes N2 C12 C13 S2 -173.7(2) yes O3 C11 C12 C13 93.6(4) ? O4 C11 C12 C13 -84.7(4) ?