#------------------------------------------------------------------------------ #$Date: 2011-09-17 21:27:16 +0100 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2200323.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_2200323 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2001 _journal_volume 57 _journal_page_first o466 _journal_page_last o468 _publ_section_title ; L-Valine L-valinium perchlorate monohydrate ; _space_group_IT_number 4 _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _[local]_cod_cif_authors_sg_H-M 'P 21' loop_ _publ_author_name 'S. Pandiarajan' 'B. Sridhar' 'R. K. Rajaram' _chemical_name_common 'L-Valine L-Valinium Perchlorate' _chemical_formula_moiety 'C5 H11 N O2 +, Cl O4 -, C5 H12 N O2, H2 O' _chemical_formula_sum 'C10 H25 Cl N2 O9' _chemical_formula_iupac 'C5 H11 N O2 +, Cl O4 -, C5 H12 N O2, H2 O' _chemical_formula_weight 352.77 _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.235(3) _cell_length_b 5.8312(14) _cell_length_c 13.0948(19) _cell_angle_alpha 90.00 _cell_angle_beta 91.282(16) _cell_angle_gamma 90.00 _cell_volume 857.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_meas 1.369 _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 Cl1 .32517(7) .02913(19) .09205(6) .0528(3) Uani d . 1 . . Cl O1 .2394(3) -.0572(11) .0241(3) .1091(18) Uani d . 1 A . O O3 .2751(5) .0918(11) .1838(3) .1308(19) Uani d . 1 A . O O2 .3962(13) .197(4) .0469(13) .112(6) Uani d P .65(5) A 1 O O4 .4124(9) -.132(3) .133(2) .124(6) Uani d P .65(5) A 1 O O2' .368(5) .231(7) .055(3) .178(16) Uani d P .35(5) A 2 O O4' .4038(19) -.147(4) .084(3) .112(7) Uani d P .35(5) A 2 O O1A .4708(3) .4853(5) .3769(2) .0628(8) Uani d . 1 . . O O1B .3434(3) .3121(4) .4765(2) .0605(8) Uani d . 1 . . O C11 .3832(3) .4873(6) .4311(2) .0385(8) Uani d . 1 . . C C12 .3191(3) .7135(6) .4498(3) .0335(7) Uani d . 1 . . C H12 .3297 .7530 .5222 .040 Uiso calc R 1 . . H N11 .3775(2) .8941(5) .3884(2) .0380(6) Uani d . 1 . . N H11A .3410 1.0276 .3980 .057 Uiso calc R 1 . . H H11B .3728 .8567 .3225 .057 Uiso calc R 1 . . H H11C .4536 .9061 .4079 .057 Uiso calc R 1 . . H C13 .1852(3) .6948(7) .4259(3) .0516(9) Uani d . 1 . . C H13 .1543 .5767 .4715 .062 Uiso calc R 1 . . H C14 .1204(4) .9175(10) .4518(5) .0815(16) Uani d . 1 . . C H14A .1406 .9619 .5206 .122 Uiso calc R 1 . . H H14B .0359 .8940 .4454 .122 Uiso calc R 1 . . H H14C .1439 1.0362 .4056 .122 Uiso calc R 1 . . H C15 .1584(4) .6139(10) .3180(4) .0811(15) Uani d . 1 . . C H15A .0738 .6049 .3069 .122 Uiso calc R 1 . . H H15B .1930 .4651 .3082 .122 Uiso calc R 1 . . H H15C .1914 .7202 .2704 .122 Uiso calc R 1 . . H O2A .3947(2) .5095(6) .69524(19) .0576(7) Uani d . 1 . . O O2B .2391(3) .2967(6) .6483(2) .0647(8) Uani d . 1 . . O H2B .2688 .3051 .5918 .097 Uiso calc R 1 . . H C21 .3045(3) .4107(7) .7145(3) .0437(8) Uani d . 1 . . C C22 .2528(3) .4105(7) .8206(3) .0421(8) Uani d . 1 . . C H22 .2531 .2517 .8452 .050 Uiso calc R 1 . . H N21 .3369(2) .5432(7) .88663(19) .0498(7) Uani d . 1 . . N H21A .3103 .5470 .9501 .075 Uiso calc R 1 . . H H21B .3428 .6856 .8628 .075 Uiso calc R 1 . . H H21C .4082 .4766 .8866 .075 Uiso calc R 1 . . H C23 .1250(3) .4973(9) .8235(3) .0602(10) Uani d . 1 . . C H23 .0779 .4046 .7749 .072 Uiso calc R 1 . . H C24 .0737(4) .4601(13) .9282(5) .097(2) Uani d . 1 . . C H24A .0825 .3019 .9472 .145 Uiso calc R 1 . . H H24B -.0092 .5001 .9265 .145 Uiso calc R 1 . . H H24C .1153 .5548 .9772 .145 Uiso calc R 1 . . H C25 .1139(5) .7465(11) .7894(5) .0901(17) Uani d . 1 . . C H25A .0322 .7935 .7922 .135 Uiso calc R 1 . . H H25B .1410 .7612 .7207 .135 Uiso calc R 1 . . H H25C .1616 .8418 .8340 .135 Uiso calc R 1 . . H OW1 .5770(3) .4660(5) .1852(2) .0578(8) Uani d . 1 . . O HW1 .519(4) .503(12) .153(4) .083(17) Uiso d . 1 . . H HW2 .543(4) .449(10) .245(4) .068(14) Uiso d . 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 Cl1 .0524(5) .0638(6) .0419(4) -.0023(5) -.0037(3) .0025(5) O1 .0665(18) .177(5) .083(2) -.021(3) -.0084(16) -.043(3) O3 .189(4) .139(5) .066(2) .002(4) .039(2) -.020(3) O2 .102(7) .150(14) .084(7) -.070(7) -.020(5) .042(7) O4 .080(4) .120(8) .170(13) -.019(6) -.060(6) .065(8) O2' .29(4) .113(17) .13(2) -.04(2) -.08(2) .096(17) O4' .095(10) .111(11) .127(17) .067(11) -.059(10) -.042(12) O1A .0708(16) .0456(17) .0731(17) .0148(14) .0253(14) -.0042(14) O1B .107(2) .0256(13) .0498(15) .0036(15) .0198(15) .0005(12) C11 .0523(17) .0316(18) .0315(14) .0059(15) -.0015(13) -.0056(14) C12 .0405(16) .0248(15) .0353(16) .0001(14) .0034(13) -.0006(13) N11 .0407(13) .0269(13) .0466(15) -.0021(12) .0059(11) -.0032(11) C13 .0384(17) .0375(19) .079(3) -.0039(16) .0071(17) .0009(18) C14 .046(2) .068(3) .131(4) .016(2) .009(2) -.015(3) C15 .070(3) .075(3) .097(3) -.010(3) -.032(2) -.015(3) O2A .0586(14) .0598(16) .0550(13) -.0118(16) .0198(11) -.0046(15) O2B .0749(18) .071(2) .0489(14) -.0180(17) .0104(12) -.0075(16) C21 .0466(17) .0368(17) .0480(18) .0015(16) .0106(15) .0026(16) C22 .0404(16) .0381(17) .0481(18) .0022(16) .0085(13) .0084(16) N21 .0476(14) .060(2) .0420(13) .0017(17) .0038(11) .0070(16) C23 .0392(16) .067(3) .075(2) .004(2) .0068(15) -.007(3) C24 .063(3) .105(5) .125(4) -.003(3) .053(3) -.006(4) C25 .075(3) .079(4) .116(4) .038(3) -.015(3) .008(3) OW1 .0605(16) .058(2) .0550(15) -.0017(14) .0053(13) .0006(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 Cl1 O4' . 1.360(17) ? Cl1 O2' . 1.37(3) ? Cl1 O3 . 1.387(4) ? Cl1 O1 . 1.391(4) ? Cl1 O2 . 1.402(12) ? Cl1 O4 . 1.456(11) ? O1A C11 . 1.225(4) yes O1B C11 . 1.268(4) yes C11 C12 . 1.525(5) ? C12 N11 . 1.486(4) ? C12 C13 . 1.534(5) ? C12 H12 . .9800 ? N11 H11A . .8900 ? N11 H11B . .8900 ? N11 H11C . .8900 ? C13 C15 . 1.513(6) ? C13 C14 . 1.531(6) ? C13 H13 . .9800 ? C14 H14A . .9600 ? C14 H14B . .9600 ? C14 H14C . .9600 ? C15 H15A . .9600 ? C15 H15B . .9600 ? C15 H15C . .9600 ? O2A C21 . 1.197(4) yes O2B C21 . 1.305(5) yes O2B H2B . .8200 ? C21 C22 . 1.519(5) ? C22 N21 . 1.485(5) ? C22 C23 . 1.523(5) ? C22 H22 . .9800 ? N21 H21A . .8900 ? N21 H21B . .8900 ? N21 H21C . .8900 ? C23 C24 . 1.515(7) ? C23 C25 . 1.524(8) ? C23 H23 . .9800 ? C24 H24A . .9600 ? C24 H24B . .9600 ? C24 H24C . .9600 ? C25 H25A . .9600 ? C25 H25B . .9600 ? C25 H25C . .9600 ? OW1 HW1 . .80(5) ? OW1 HW2 . .89(5) ? _cod_database_code 2200323