#------------------------------------------------------------------------------ #$Date: 2011-09-17 21:27:16 +0100 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2200444.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2200444 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2001 _journal_volume 57 _journal_page_first o772 _journal_page_last o774 _publ_section_title ; Bis(DL-phenylalaninium) sulfate monohydrate ; _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' loop_ _publ_author_name 'Srinivasan, N.' 'Sridhar, B.' 'Rajaram, R. K.' _chemical_name_common 'Bis(DL-phenylalaninium)sulfate monohydrate' _chemical_formula_moiety '2C9 H12 N O2 1+, O4 S 2-, H2 O' _chemical_formula_sum 'C18 H26 N2 O9 S' _chemical_formula_iupac '2C9 H12 N O2 1+, O4 S 2-, H2 O' _chemical_formula_weight 446.47 _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.560(2) _cell_length_b 6.6000(12) _cell_length_c 22.115(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.70(2) _cell_angle_gamma 90.00 _cell_volume 2124.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_meas 1.39 _diffrn_ambient_temperature 293(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 S .27906(4) .20427(9) -.10666(3) .02978(17) Uani d . 1 . . S O1 .32429(11) .2919(3) -.05195(7) .0369(4) Uani d . 1 . . O O2 .19967(12) .0864(3) -.08762(9) .0530(6) Uani d . 1 . . O O3 .34514(12) .0639(3) -.13478(8) .0468(5) Uani d . 1 . . O O4 .25546(17) .3665(3) -.14796(10) .0673(7) Uani d . 1 . . O OW .57935(17) .4282(4) .18734(12) .0684(7) Uani d D 1 . . O H1 .628(2) .513(6) .1784(18) .101(14) Uiso d D 1 . . H H2 .539(2) .445(6) .1566(13) .081(12) Uiso d D 1 . . H O1A .50678(12) .3299(3) .04872(8) .0447(5) Uani d . 1 . . O O1B .49823(11) .1962(3) -.04434(8) .0433(5) Uani d . 1 . . O H1B .4439 .2278 -.0425 .065 Uiso calc R 1 . . H C11 .54087(16) .2536(3) .00510(11) .0318(5) Uani d . 1 . . C C12 .64337(15) .2134(4) .00081(10) .0317(5) Uani d . 1 . . C H12 .6529 .0672 -.0037 .038 Uiso calc R 1 . . H N11 .68793(14) .2804(3) .05773(9) .0344(5) Uani d . 1 . . N H11A .7481 .2577 .0559 .052 Uiso calc R 1 . . H H11B .6647 .2116 .0886 .052 Uiso calc R 1 . . H H11C .6779 .4122 .0630 .052 Uiso calc R 1 . . H C13 .68506(17) .3202(4) -.05313(12) .0404(6) Uani d . 1 . . C H13A .6562 .2692 -.0898 .048 Uiso calc R 1 . . H H13B .6715 .4638 -.0505 .048 Uiso calc R 1 . . H C14 .78803(17) .2929(4) -.05764(11) .0380(6) Uani d . 1 . . C C15 .8272(2) .1050(5) -.06414(16) .0612(9) Uani d . 1 . . C H15 .7900 -.0095 -.0660 .073 Uiso calc R 1 . . H C16 .9219(2) .0849(6) -.06797(17) .0706(10) Uani d . 1 . . C H16 .9478 -.0431 -.0719 .085 Uiso calc R 1 . . H C17 .9768(2) .2511(6) -.06595(14) .0621(10) Uani d . 1 . . C H17 1.0402 .2369 -.0686 .075 Uiso calc R 1 . . H C18 .9391(2) .4382(6) -.06004(13) .0557(9) Uani d . 1 . . C H18 .9767 .5521 -.0593 .067 Uiso calc R 1 . . H C19 .84491(19) .4598(5) -.05507(12) .0451(7) Uani d . 1 . . C H19 .8198 .5881 -.0500 .054 Uiso calc R 1 . . H O2A -.19852(14) .2220(3) .20968(9) .0572(6) Uani d . 1 . . O O2B -.10045(13) .1978(4) .13422(10) .0584(6) Uani d . 1 . . O H2B -.1328 .1015 .1242 .088 Uiso calc R 1 . . H C21 -.13276(16) .2795(4) .18392(11) .0352(6) Uani d . 1 . . C C22 -.07529(15) .4580(4) .20500(11) .0323(5) Uani d . 1 . . C H22 -.0597 .5423 .1701 .039 Uiso calc R 1 . . H N21 -.13195(13) .5768(3) .24707(9) .0334(5) Uani d . 1 . . N H21A -.1001 .6834 .2603 .050 Uiso calc R 1 . . H H21B -.1474 .4995 .2783 .050 Uiso calc R 1 . . H H21C -.1826 .6192 .2280 .050 Uiso calc R 1 . . H C23 .01357(16) .3814(4) .23563(14) .0441(7) Uani d . 1 . . C H23A -.0024 .2894 .2680 .053 Uiso calc R 1 . . H H23B .0487 .3056 .2063 .053 Uiso calc R 1 . . H C24 .07292(15) .5482(4) .26114(12) .0366(6) Uani d . 1 . . C C25 .11920(18) .6813(5) .22420(12) .0465(7) Uani d . 1 . . C H25 .1133 .6686 .1824 .056 Uiso calc R 1 . . H C26 .1739(2) .8323(5) .24803(14) .0577(8) Uani d . 1 . . C H26 .2040 .9218 .2225 .069 Uiso calc R 1 . . H C27 .1840(2) .8505(6) .31019(15) .0611(9) Uani d . 1 . . C H27 .2219 .9502 .3266 .073 Uiso calc R 1 . . H C28 .1380(2) .7217(5) .34712(13) .0555(8) Uani d . 1 . . C H28 .1438 .7355 .3888 .067 Uiso calc R 1 . . H C29 .08293(18) .5708(5) .32339(13) .0463(7) Uani d . 1 . . C H29 .0522 .4834 .3492 .056 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 S .0282(3) .0276(3) .0333(3) -.0037(3) -.0074(2) -.0020(3) O1 .0336(9) .0384(10) .0387(10) -.0027(8) -.0090(7) -.0088(8) O2 .0362(10) .0633(14) .0597(13) -.0206(10) .0064(9) -.0188(11) O3 .0380(10) .0588(13) .0439(11) .0020(9) .0019(8) -.0149(9) O4 .0854(16) .0513(13) .0644(14) .0018(12) -.0350(12) .0122(11) OW .0604(15) .0556(15) .0889(19) -.0116(12) -.0160(13) .0189(13) O1A .0376(10) .0548(12) .0418(11) .0040(9) .0065(8) .0005(9) O1B .0291(9) .0482(11) .0523(11) .0011(9) -.0069(8) -.0123(9) C11 .0314(12) .0225(12) .0415(14) -.0014(10) .0002(11) .0022(11) C12 .0298(12) .0311(12) .0340(12) -.0016(11) -.0032(9) -.0026(10) N11 .0346(11) .0331(11) .0353(11) -.0014(9) -.0041(9) -.0002(9) C13 .0345(13) .0487(17) .0379(14) .0009(12) .0001(11) .0058(12) C14 .0337(13) .0482(16) .0322(13) .0026(13) .0024(10) .0021(12) C15 .0512(18) .0501(19) .083(2) -.0004(16) .0156(16) .0005(17) C16 .054(2) .068(2) .090(3) .0240(19) .0210(18) .014(2) C17 .0317(15) .104(3) .0508(18) .0092(18) .0026(13) .0097(19) C18 .0393(16) .085(3) .0431(17) -.0165(16) -.0020(12) -.0015(16) C19 .0449(15) .0493(17) .0412(15) -.0031(13) .0005(12) -.0034(13) O2A .0453(11) .0670(14) .0597(12) -.0273(11) .0167(10) -.0143(11) O2B .0465(12) .0628(14) .0664(14) -.0218(10) .0188(10) -.0313(11) C21 .0258(12) .0417(14) .0381(13) -.0018(11) -.0002(10) -.0030(12) C22 .0242(11) .0385(14) .0342(13) -.0021(10) .0015(9) -.0029(11) N21 .0280(10) .0395(12) .0325(11) .0024(9) -.0003(8) -.0006(9) C23 .0266(13) .0415(15) .0641(18) .0007(11) -.0047(12) -.0060(14) C24 .0205(11) .0451(15) .0441(15) .0028(11) -.0005(10) -.0046(12) C25 .0371(14) .066(2) .0359(14) -.0110(14) .0009(11) -.0085(14) C26 .0496(17) .068(2) .0553(19) -.0253(16) .0070(14) -.0048(16) C27 .0469(17) .075(2) .061(2) -.0210(17) .0007(15) -.0251(18) C28 .0464(16) .080(2) .0401(15) -.0041(16) -.0038(13) -.0153(16) C29 .0351(14) .0601(19) .0436(15) -.0010(13) .0005(11) .0047(14) 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 S O4 . 1.446(2) ? S O2 . 1.4597(19) ? S O3 . 1.4782(19) ? S O1 . 1.4876(17) ? OW H1 . .92(2) ? OW H2 . .90(2) ? O1A C11 . 1.201(3) yes O1B C11 . 1.307(3) yes O1B H1B . .82 ? C11 C12 . 1.520(3) ? C12 N11 . 1.477(3) ? C12 C13 . 1.519(3) ? C12 H12 . .98 ? N11 H11A . .89 ? N11 H11B . .89 ? N11 H11C . .89 ? C13 C14 . 1.515(3) ? C13 H13A . .97 ? C13 H13B . .97 ? C14 C15 . 1.373(4) ? C14 C19 . 1.379(4) ? C15 C16 . 1.389(4) ? C15 H15 . .93 ? C16 C17 . 1.358(5) ? C16 H16 . .93 ? C17 C18 . 1.358(5) ? C17 H17 . .93 ? C18 C19 . 1.385(4) ? C18 H18 . .93 ? C19 H19 . .93 ? O2A C21 . 1.183(3) yes O2B C21 . 1.316(3) yes O2B H2B . .82 ? C21 C22 . 1.516(3) ? C22 N21 . 1.476(3) ? C22 C23 . 1.538(3) ? C22 H22 . .98 ? N21 H21A . .89 ? N21 H21B . .89 ? N21 H21C . .89 ? C23 C24 . 1.505(4) ? C23 H23A . .97 ? C23 H23B . .97 ? C24 C25 . 1.381(4) ? C24 C29 . 1.391(4) ? C25 C26 . 1.377(4) ? C25 H25 . .93 ? C26 C27 . 1.386(4) ? C26 H26 . .93 ? C27 C28 . 1.361(5) ? C27 H27 . .93 ? C28 C29 . 1.378(4) ? C28 H28 . .93 ? C29 H29 . .93 ? _cod_database_code 2200444