#------------------------------------------------------------------------------ #$Date: 2016-02-19 22:18:51 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176760 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/13/2011355.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_2011355 loop_ _publ_author_name 'Okabe, Nobuo' 'Eguchi, Yoko' 'Miura, Junko' 'Akiko, Shimosaki' _publ_section_title ; L-Kynureninium sulfate dihydrate ; _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first e416 _journal_page_last e417 _journal_paper_doi 10.1107/S0108270100011100 _journal_volume 56 _journal_year 2000 _chemical_formula_iupac 'C10 H14 N2 O3 2+, S O4 2-, 2H2 O' _chemical_formula_sum 'C10 H18 N2 O9 S' _chemical_formula_weight 342.32 _chemical_name_systematic ; L-Kynulenine sulfate dihydrate ; _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_type_scat_source 'International Tables for X-ray Crystallography Vol.IV' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.353(5) _cell_length_b 22.134(5) _cell_length_c 5.897(7) _cell_measurement_reflns_used 25 _cell_measurement_temperature 296 _cell_measurement_theta_max 14.5 _cell_measurement_theta_min 10.3 _cell_volume 1481.8(19) _computing_cell_refinement ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1999a) ; _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1999a) ; _computing_data_reduction ' TEXSAN PROCESS (Molecular Structure Corporation, 1999b)' _computing_publication_material TEXSAN _computing_structure_refinement ' TEXSAN LS' _computing_structure_solution ; SIR88 (Burla et al., 1989) and DIRDIF (Beurskens et al., 1994) ; _diffrn_measured_fraction_theta_full 1.0412 _diffrn_measured_fraction_theta_max 1.0412 _diffrn_measurement_device 'Rigaku AFC-5R' _diffrn_measurement_method \w-2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71069 _diffrn_reflns_av_R_equivalents .058 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 4128 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.5 _diffrn_standards_decay_% .12 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu .267 _exptl_absorpt_correction_T_max .998 _exptl_absorpt_correction_T_min .972 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour 'light yellow' _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_meas ? _exptl_crystal_description needle _exptl_crystal_size_max .50 _exptl_crystal_size_mid .10 _exptl_crystal_size_min .05 _refine_diff_density_max .81 _refine_diff_density_min -.90 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 200 _refine_ls_number_reflns 2071 _refine_ls_R_factor_gt .0565 _refine_ls_shift/su_max .0044 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.06100(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .1629 _reflns_number_gt 1088 _reflns_number_total 2072 _reflns_threshold_expression F^2^>2\s(F^2^) _cod_data_source_file qa0372.cif _cod_data_source_block I _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 ; _cod_original_cell_volume 1481.0(10) _cod_database_code 2011355 _cod_database_fobs_code 2011355 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+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 S .11570(10) .10868(7) .0645(3) .0328(4) Uani d . 1.00 . . S O1 .3674(4) .0657(2) .4722(7) .0440(10) Uani d . 1.00 . . O O2 .5063(4) .2318(2) .9046(9) .0530(10) Uani d . 1.00 . . O O3 .3324(4) .2748(2) .8345(9) .0530(10) Uani d . 1.00 . . O O4 .1080(4) .1037(2) .3108(7) .0420(10) Uani d . 1.00 . . O O5 .1170(5) .1721(2) -.0005(8) .0570(10) Uani d . 1.00 . . O O6 .0108(4) .0798(2) -.0396(9) .059(2) Uani d . 1.00 . . O O7 .2182(4) .0787(2) -.0293(9) .053(2) Uani d . 1.00 . . O O8 .7406(5) .2143(2) .6611(9) .065(2) Uani d . 1.00 . . O O9 .9181(8) .1402(5) .5880(10) .168(4) Uani d . 1.00 . . O N1 .3908(5) -.0003(2) .0929(8) .0290(10) Uani d . 1.00 . . N N2 .2493(4) .1814(2) .6008(9) .0300(10) Uani d . 1.00 . . N C1 .5284(5) .0801(2) .2230(10) .0290(10) Uani d . 1.00 . . C C2 .5027(5) .0335(2) .0710(10) .0280(10) Uani d . 1.00 . . C C3 .5777(6) .0176(3) -.0980(10) .039(2) Uani d . 1.00 . . C C4 .6861(6) .0476(3) -.1180(10) .046(2) Uani d . 1.00 . . C C5 .7152(5) .0921(3) .0310(10) .045(2) Uani d . 1.00 . . C C6 .6368(5) .1092(3) .1960(10) .037(2) Uani d . 1.00 . . C C7 .4444(5) .0992(3) .4060(10) .0310(10) Uani d . 1.00 . . C C8 .4585(6) .1615(3) .5030(10) .036(2) Uani d . 1.00 . . C C9 .3688(5) .1759(2) .6883(10) .0270(10) Uani d . 1.00 . . C C10 .4004(6) .2341(3) .8165(10) .0320(10) Uani d . 1.00 . . C H1 .5594 -.0150 -.1918 .0440 Uiso calc . 1.00 . . H H2 .7419 .0347 -.2218 .0591 Uiso calc . 1.00 . . H H3 .7892 .1112 .0127 .0633 Uiso calc . 1.00 . . H H4 .6569 .1415 .2949 .0373 Uiso calc . 1.00 . . H H5 .5359 .1668 .5558 .0397 Uiso calc . 1.00 . . H H6 .4464 .1894 .3760 .0397 Uiso calc . 1.00 . . H H7 .3703 .1434 .7935 .0280 Uiso calc . 1.00 . . H H8 .5064 .2873 .8871 .0610 Uiso calc . 1.00 . . H H9 .1954 .1671 .7149 .0327 Uiso calc . 1.00 . . H H10 .2327 .2230 .5731 .0327 Uiso calc . 1.00 . . H H11 .2405 .1588 .4685 .0327 Uiso calc . 1.00 . . H H12 .3892 -.0197 .2445 .0415 Uiso calc . 1.00 . . H H13 .3264 .0253 .0833 .0415 Uiso calc . 1.00 . . H H14 .3874 -.0317 -.0147 .0415 Uiso calc . 1.00 . . H H15 .6970 .2428 .7383 .0610 Uiso calc . 1.00 . . H H16 .8016 .2228 .7087 .0610 Uiso calc . 1.00 . . H H17 .9535 .1831 .5596 .0610 Uiso calc . 1.00 . . H H18 .9376 .1241 .7491 .0610 Uiso calc . 1.00 . . 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 .0401(9) .0300(7) .0283(7) .0087(8) .0104(8) .0074(7) O1 .046(3) .036(2) .048(3) -.013(2) .018(3) -.012(2) O2 .049(2) .038(2) .072(4) .006(2) -.016(3) -.013(3) O3 .052(3) .040(3) .068(3) .009(2) -.014(3) -.023(3) O4 .052(3) .042(2) .0310(10) -.014(3) .010(3) .003(2) O5 .075(3) .030(2) .065(3) .017(3) .041(3) .011(2) O6 .056(3) .077(4) .045(3) -.015(3) -.011(3) -.007(3) O7 .054(3) .044(3) .060(4) .031(2) .028(3) .015(3) O8 .068(4) .059(3) .069(4) .017(3) .009(3) .012(3) O9 .173(9) .250(10) .076(5) .159(8) .029(6) .063(7) N1 .033(2) .025(2) .029(2) -.001(2) .001(3) -.006(2) N2 .033(2) .023(2) .034(3) -.008(2) .016(2) -.007(2) C1 .030(3) .027(3) .031(3) .000(2) -.002(2) -.002(2) C2 .030(3) .026(3) .029(3) -.001(2) -.003(3) .004(2) C3 .041(3) .041(4) .036(4) -.002(3) .006(3) -.014(3) C4 .038(3) .053(5) .048(5) .001(3) .022(3) -.008(3) C5 .025(3) .052(4) .057(5) -.006(3) .012(3) -.006(3) C6 .033(3) .034(3) .042(3) -.006(3) .002(3) -.005(3) C7 .033(3) .028(3) .032(3) .004(2) -.001(2) -.004(2) C8 .033(3) .032(3) .043(4) -.004(3) .015(3) -.016(3) C9 .037(3) .018(2) .027(3) -.001(3) .008(2) .006(2) C10 .046(3) .029(3) .022(3) -.009(2) .007(3) -.004(2) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O4 S O5 1_555 1_555 109.8(3) yes O4 S O6 1_555 1_555 109.3(3) yes O4 S O7 1_555 1_555 113.1(3) yes O5 S O6 1_555 1_555 108.3(4) yes O5 S O7 1_555 1_555 109.4(3) yes O6 S O7 1_555 1_555 106.8(3) yes C2 C1 C6 1_555 1_555 116.8(6) yes C2 C1 C7 1_555 1_555 122.3(6) yes C6 C1 C7 1_555 1_555 120.9(6) yes N1 C2 C1 1_555 1_555 119.8(6) yes N1 C2 C3 1_555 1_555 118.2(5) yes C1 C2 C3 1_555 1_555 122.0(6) yes C2 C3 C4 1_555 1_555 119.5(6) yes C3 C4 C5 1_555 1_555 119.9(6) yes C4 C5 C6 1_555 1_555 120.1(6) yes C1 C6 C5 1_555 1_555 121.7(7) yes O1 C7 C1 1_555 1_555 121.3(5) yes O1 C7 C8 1_555 1_555 121.1(6) yes C1 C7 C8 1_555 1_555 117.6(5) yes C7 C8 C9 1_555 1_555 113.1(5) yes N2 C9 C8 1_555 1_555 112.6(5) yes N2 C9 C10 1_555 1_555 108.8(5) yes C8 C9 C10 1_555 1_555 111.9(5) yes O2 C10 O3 1_555 1_555 126.1(6) yes O2 C10 C9 1_555 1_555 112.2(6) yes O3 C10 C9 1_555 1_555 121.7(6) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S O4 . . 1.461(4) yes S O5 . . 1.455(5) yes S O6 . . 1.486(5) yes S O7 . . 1.447(5) yes O1 C7 . . 1.212(8) yes O2 C10 . . 1.309(8) yes O3 C10 . . 1.189(8) yes N1 C2 . . 1.480(8) yes N2 C9 . . 1.458(8) yes C1 C2 . . 1.398(8) yes C1 C6 . . 1.397(9) yes C1 C7 . . 1.500(9) yes C2 C3 . . 1.357(9) yes C3 C4 . . 1.405(10) yes C4 C5 . . 1.360(10) yes C5 C6 . . 1.374(9) yes C7 C8 . . 1.503(9) yes C8 C9 . . 1.527(9) yes C9 C10 . . 1.537(9) yes 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 H12 O1 1_555 .991 2.334 2.688(7) 99.928 no N2 H11 O1 1_555 .929 2.514 2.992(7) 112.188 no N2 H10 O3 1_555 .949 2.225 2.655(7) 106.467 no N1 H13 O7 1_555 .929 1.826 2.723(7) 161.424 no N1 H12 O6 2_555 .991 2.162 3.004(8) 141.845 no N1 H12 O7 2_555 .991 2.234 3.086(7) 143.381 no N1 H14 O4 2_554 .939 1.893 2.822(6) 169.482 no N2 H11 O4 1_555 .929 2.150 2.906(7) 137.703 no N2 H9 O5 1_556 .964 1.903 2.799(8) 153.490 no N2 H9 O7 1_556 .964 2.488 3.178(8) 128.416 no N1 H13 O1 2_554 .929 3.055 3.345(7) 100.033 no 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O1 C7 C1 C2 1_555 1_555 1_555 1_555 21.2(10) yes O1 C7 C1 C6 1_555 1_555 1_555 1_555 -159.6(7) yes O1 C7 C8 C9 1_555 1_555 1_555 1_555 .7(9) yes O2 C10 C9 N2 1_555 1_555 1_555 1_555 178.6(5) yes O2 C10 C9 C8 1_555 1_555 1_555 1_555 -56.5(7) yes O3 C10 C9 N2 1_555 1_555 1_555 1_555 .4(8) yes O3 C10 C9 C8 1_555 1_555 1_555 1_555 125.3(7) yes N1 C2 C1 C6 1_555 1_555 1_555 1_555 178.6(5) yes N1 C2 C1 C7 1_555 1_555 1_555 1_555 -2.2(9) yes N1 C2 C3 C4 1_555 1_555 1_555 1_555 -177.9(6) yes N2 C9 C8 C7 1_555 1_555 1_555 1_555 -68.7(7) yes C1 C2 C3 C4 1_555 1_555 1_555 1_555 1.0(10) yes C1 C6 C5 C4 1_555 1_555 1_555 1_555 2.0(10) yes C1 C7 C8 C9 1_555 1_555 1_555 1_555 -179.6(5) yes C2 C1 C6 C5 1_555 1_555 1_555 1_555 -1.0(10) yes C2 C1 C7 C8 1_555 1_555 1_555 1_555 -158.4(6) yes C2 C3 C4 C5 1_555 1_555 1_555 1_555 .0(10) yes C3 C2 C1 C6 1_555 1_555 1_555 1_555 -1.1(9) yes C3 C2 C1 C7 1_555 1_555 1_555 1_555 178.1(6) yes C3 C4 C5 C6 1_555 1_555 1_555 1_555 -1.0(10) yes C5 C6 C1 C7 1_555 1_555 1_555 1_555 179.7(6) yes C6 C1 C7 C8 1_555 1_555 1_555 1_555 20.8(9) yes C7 C8 C9 C10 1_555 1_555 1_555 1_555 168.4(5) yes