#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2011355.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
;
 <small>L</small>-Kynureninium sulfate dihydrate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              e416
_journal_page_last               e417
_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      'not measured'
_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^)
_[local]_cod_data_source_file    qa0372.cif
_[local]_cod_data_source_block   I
_cod_original_cell_volume        1481.0(10)
_cod_database_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_occupancy
_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_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