#------------------------------------------------------------------------------
#$Date: 2019-07-03 21:47:50 +0300 (Wed, 03 Jul 2019) $
#$Revision: 216712 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/16/2021697.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_2021697
loop_
_publ_author_name
'Pogoda, Dorota'
'Janczak, Jan'
'Pawlak, Sylwia'
'Zaworotko, Michael'
'Videnova-Adrabinska, Veneta'
_publ_section_title
;
Tautomeric polymorphism of the neuroactive inhibitor kynurenic acid
;
_journal_coeditor_code UK3175
_journal_issue 6
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 793
_journal_page_last 805
_journal_paper_doi 10.1107/S2053229619005990
_journal_volume 75
_journal_year 2019
_chemical_absolute_configuration rm
_chemical_formula_iupac 'C10 H7 N O3, C2 H6 O S'
_chemical_formula_moiety 'C10 H7 N O3, C2 H6 O S'
_chemical_formula_sum 'C12 H13 N O4 S'
_chemical_formula_weight 267.29
_chemical_name_common
;
Kynurenic acid dimethyl sulfoxide monosolvate
;
_chemical_name_systematic
;
4-Hydroxyquinoline-2-carboxylic acid dimethyl sulfoxide monosolvate
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_symmetry_space_group_name_Hall 'P 2ac 2ab'
_symmetry_space_group_name_H-M 'P 21 21 21'
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2014/7
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 4.9552(3)
_cell_length_b 10.8444(6)
_cell_length_c 22.7982(11)
_cell_measurement_reflns_used 4335
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 28.6480
_cell_measurement_theta_min 4.0170
_cell_volume 1225.09(12)
_computing_cell_refinement
;
CrysAlis RED (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis CCD (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis RED (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2005)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 10.6249
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type 'Kuma KM-4 with CCD detector'
_diffrn_measurement_method \w-scan
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0426
_diffrn_reflns_av_unetI/netI 0.0385
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_number 14513
_diffrn_reflns_theta_full 27.500
_diffrn_reflns_theta_max 29.534
_diffrn_reflns_theta_min 2.592
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.270
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.92317
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.449
_exptl_crystal_description parallelepiped
_exptl_crystal_F_000 560
_exptl_crystal_size_max 0.410
_exptl_crystal_size_mid 0.210
_exptl_crystal_size_min 0.120
_refine_diff_density_max 0.280
_refine_diff_density_min -0.253
_refine_ls_abs_structure_details
;
Flack x determined using 999 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.11(4)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.000
_refine_ls_hydrogen_treatment refxyz
_refine_ls_matrix_type full
_refine_ls_number_parameters 202
_refine_ls_number_reflns 3044
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.000
_refine_ls_R_factor_all 0.0430
_refine_ls_R_factor_gt 0.0360
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+0.2943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0808
_refine_ls_wR_factor_ref 0.0849
_reflns_number_gt 2756
_reflns_number_total 3044
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file uk3175sup1.cif
_cod_data_source_block kyn_100
_cod_database_code 2021697
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.897
_shelx_estimated_absorpt_t_max 0.968
_shelx_hkl_file
;
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0 0 -5 188.990 157.098 1
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0 0 5 62.4265 155.747 4
0 0 -6 119685. 3422.04 1
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0 0 0 0.00 0.00 0
TITL KYN_100 in P2(1)2(1)2(1)
REM P2(1)2(1)2(1) (#19 in standard setting)
CELL 0.71073 4.955216 10.844422 22.798191 90.0000 90.0000 90.0000
ZERR 6.00 0.000283 0.000638 0.001148 0.0000 0.0000 0.0000
LATT -1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H N O S
UNIT 48.00 48.00 6.00 6.00 6.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 80286
_shelx_res_file
;
kyn_100.res created by SHELXL-2014/7
TITL kyn_100_a.res in P2(1)2(1)2(1)
CELL 0.71073 4.955216 10.844422 22.798191 90 90 90
ZERR 4 0.000283 0.000638 0.001148 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H N O S
UNIT 48 52 4 16 4
temp -173
L.S. 6
PLAN 20
BOND $H
HTAB 2
HTAB N1 O4
EQIV $1 -X, Y-0.5, -Z+1.5
HTAB O2 O3_$1
list 4
fmap 2
acta 55
size 0.41 0.21 0.12
WGHT 0.046100 0.294300
FVAR 6.25988
N1 3 0.423988 0.570919 0.643643 11.00000 0.01272 0.01127 =
0.01612 -0.00210 0.00063 -0.00037
H1N 2 0.400477 0.497150 0.627978 11.00000 -1.20000
C1 1 0.255051 0.607844 0.686930 11.00000 0.00903 0.01601 =
0.01472 0.00245 -0.00223 0.00044
C2 1 0.262620 0.724306 0.709335 11.00000 0.01142 0.01526 =
0.01588 0.00185 -0.00035 0.00094
H2 2 0.135600 0.745059 0.737864 11.00000 -1.20000
C3 1 0.448760 0.813127 0.687332 11.00000 0.01156 0.01200 =
0.01920 -0.00105 -0.00179 0.00217
C4 1 0.629330 0.771749 0.641205 11.00000 0.00853 0.01573 =
0.01424 0.00133 -0.00092 0.00140
C5 1 0.611250 0.649977 0.620135 11.00000 0.01035 0.01391 =
0.01433 0.00274 -0.00106 0.00095
C6 1 0.821082 0.851940 0.615979 11.00000 0.01230 0.01497 =
0.01839 0.00050 -0.00218 0.00155
H6 2 0.832934 0.931026 0.631383 11.00000 -1.20000
C7 1 0.987544 0.811218 0.571767 11.00000 0.01259 0.02191 =
0.01773 0.00365 0.00074 -0.00249
H7 2 1.122061 0.867374 0.554121 11.00000 -1.20000
C8 1 0.970710 0.689033 0.551681 11.00000 0.01369 0.02355 =
0.01359 -0.00115 0.00328 0.00116
H8 2 1.089668 0.662112 0.520820 11.00000 -1.20000
C9 1 0.786226 0.608449 0.575440 11.00000 0.01498 0.01456 =
0.01766 -0.00226 -0.00026 0.00077
H9 2 0.775843 0.521353 0.562969 11.00000 -1.20000
C10 1 0.059445 0.511154 0.707660 11.00000 0.01291 0.01504 =
0.01619 0.00149 0.00105 0.00015
O1 4 0.052270 0.409614 0.685668 11.00000 0.01859 0.01508 =
0.02584 -0.00154 0.00459 -0.00262
O2 4 -0.096725 0.551729 0.749775 11.00000 0.01638 0.01421 =
0.02622 -0.00018 0.00823 -0.00150
H2O 2 -0.213157 0.491587 0.762329 11.00000 -1.50000
O3 4 0.461516 0.923300 0.706062 11.00000 0.01549 0.01230 =
0.02988 -0.00512 0.00657 -0.00024
S1 5 0.319482 0.241499 0.591545 11.00000 0.01852 0.01551 =
0.02248 -0.00096 -0.00118 -0.00321
O4 4 0.411460 0.365111 0.568371 11.00000 0.03283 0.01424 =
0.02057 0.00003 -0.00001 -0.00212
C11 1 0.522698 0.212544 0.654371 11.00000 0.02390 0.02193 =
0.02383 0.00232 0.00019 -0.00041
H11A 2 0.706427 0.226072 0.645250 11.00000 -1.50000
H11B 2 0.491174 0.127583 0.665878 11.00000 -1.50000
H11C 2 0.464652 0.266383 0.683832 11.00000 -1.50000
C12 1 0.466240 0.129632 0.543486 11.00000 0.04908 0.01744 =
0.02853 -0.00421 0.00263 -0.00083
H12A 2 0.374367 0.140223 0.504617 11.00000 -1.50000
H12B 2 0.434516 0.049434 0.559749 11.00000 -1.50000
H12C 2 0.657162 0.144047 0.541160 11.00000 -1.50000
HKLF 4
REM kyn_100_a.res in P2(1)2(1)2(1)
REM R1 = 0.0360 for 2756 Fo > 4sig(Fo) and 0.0430 for all 3044 data
REM 202 parameters refined using 0 restraints
END
WGHT 0.0379 0.2972
REM Instructions for potential hydrogen bonds
HTAB N1 S1
HTAB N1 O4
HTAB C9 O4
HTAB O2 O3_$1
EQIV $2 x, y-1, z
HTAB C11 O3_$2
HTAB C11 O1
REM Highest difference peak 0.280, deepest hole -0.253, 1-sigma level 0.054
Q1 1 0.8405 0.8411 0.5775 11.00000 0.05 0.28
Q2 1 0.3208 0.2412 0.6314 11.00000 0.05 0.27
Q3 1 0.1799 0.5590 0.7038 11.00000 0.05 0.27
Q4 1 0.3809 0.7563 0.7050 11.00000 0.05 0.26
Q5 1 0.9560 0.6387 0.5742 11.00000 0.05 0.25
Q6 1 0.3291 0.1981 0.5584 11.00000 0.05 0.25
Q7 1 0.6748 0.8173 0.6205 11.00000 0.05 0.24
Q8 1 0.2202 0.6893 0.6738 11.00000 0.05 0.24
Q9 1 0.6657 0.6991 0.6442 11.00000 0.05 0.23
Q10 1 0.9305 0.7530 0.5578 11.00000 0.05 0.23
Q11 1 0.3104 0.7629 0.6938 11.00000 0.05 0.22
Q12 1 0.8057 0.6564 0.5507 11.00000 0.05 0.21
Q13 1 0.9787 0.8259 0.6074 11.00000 0.05 0.21
Q14 1 0.0603 0.4191 0.7217 11.00000 0.05 0.20
Q15 1 0.2685 0.5976 0.6643 11.00000 0.05 0.20
Q16 1 0.3526 0.2926 0.5609 11.00000 0.05 0.20
Q17 1 0.2654 0.6614 0.7121 11.00000 0.05 0.20
Q18 1 1.0111 0.7381 0.5765 11.00000 0.05 0.19
Q19 1 0.4007 0.5960 0.6807 11.00000 0.05 0.19
Q20 1 0.7554 0.7969 0.6361 11.00000 0.05 0.19
;
_shelx_res_checksum 6156
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_type_symbol
_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
N N1 0.4240(4) 0.57092(18) 0.64364(8) 0.0134(4) Uani d 1
H H1N 0.400(6) 0.497(3) 0.6280(11) 0.016 Uiso d 1
C C1 0.2551(4) 0.6078(2) 0.68693(9) 0.0133(5) Uani d 1
C C2 0.2626(4) 0.7243(2) 0.70933(10) 0.0142(5) Uani d 1
H H2 0.136(6) 0.745(2) 0.7379(11) 0.017 Uiso d 1
C C3 0.4488(5) 0.8131(2) 0.68733(10) 0.0143(4) Uani d 1
C C4 0.6293(4) 0.7717(2) 0.64121(9) 0.0128(4) Uani d 1
C C5 0.6112(4) 0.6500(2) 0.62013(10) 0.0129(5) Uani d 1
C C6 0.8211(5) 0.8519(2) 0.61598(10) 0.0152(4) Uani d 1
H H6 0.833(6) 0.931(3) 0.6314(11) 0.018 Uiso d 1
C C7 0.9875(5) 0.8112(2) 0.57177(10) 0.0174(5) Uani d 1
H H7 1.122(6) 0.867(2) 0.5541(11) 0.021 Uiso d 1
C C8 0.9707(5) 0.6890(2) 0.55168(10) 0.0169(5) Uani d 1
H H8 1.090(6) 0.662(3) 0.5208(12) 0.020 Uiso d 1
C C9 0.7862(5) 0.6084(2) 0.57544(9) 0.0157(5) Uani d 1
H H9 0.776(6) 0.521(3) 0.5630(12) 0.019 Uiso d 1
C C10 0.0594(5) 0.5112(2) 0.70766(10) 0.0147(5) Uani d 1
O O1 0.0523(3) 0.40961(15) 0.68567(7) 0.0198(4) Uani d 1
O O2 -0.0967(3) 0.55173(16) 0.74977(7) 0.0189(4) Uani d 1
H H2O -0.213(7) 0.492(3) 0.7623(13) 0.028 Uiso d 1
O O3 0.4615(3) 0.92330(15) 0.70606(8) 0.0192(4) Uani d 1
S S1 0.31948(12) 0.24150(5) 0.59155(3) 0.01884(15) Uani d 1
O O4 0.4115(4) 0.36511(15) 0.56837(7) 0.0225(4) Uani d 1
C C11 0.5227(6) 0.2125(3) 0.65437(12) 0.0232(5) Uani d 1
H H11A 0.706(7) 0.226(3) 0.6453(14) 0.035 Uiso d 1
H H11B 0.491(7) 0.128(3) 0.6659(13) 0.035 Uiso d 1
H H11C 0.465(6) 0.266(3) 0.6838(13) 0.035 Uiso d 1
C C12 0.4662(8) 0.1296(3) 0.54349(13) 0.0317(6) Uani d 1
H H12A 0.374(7) 0.140(3) 0.5046(15) 0.048 Uiso d 1
H H12B 0.435(8) 0.049(3) 0.5597(15) 0.048 Uiso d 1
H H12C 0.657(8) 0.144(3) 0.5412(15) 0.048 Uiso d 1
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
N1 0.0127(9) 0.0113(9) 0.0161(9) -0.0004(7) 0.0006(8) -0.0021(8)
C1 0.0090(10) 0.0160(11) 0.0147(10) 0.0004(8) -0.0022(8) 0.0025(9)
C2 0.0114(10) 0.0153(11) 0.0159(10) 0.0009(8) -0.0004(8) 0.0019(9)
C3 0.0116(10) 0.0120(11) 0.0192(11) 0.0022(9) -0.0018(9) -0.0010(9)
C4 0.0085(9) 0.0157(11) 0.0142(10) 0.0014(8) -0.0009(8) 0.0013(8)
C5 0.0104(10) 0.0139(11) 0.0143(10) 0.0010(8) -0.0011(8) 0.0027(8)
C6 0.0123(10) 0.0150(11) 0.0184(11) 0.0016(10) -0.0022(9) 0.0005(9)
C7 0.0126(10) 0.0219(13) 0.0177(11) -0.0025(9) 0.0007(9) 0.0037(9)
C8 0.0137(10) 0.0236(13) 0.0136(11) 0.0012(10) 0.0033(9) -0.0012(9)
C9 0.0150(10) 0.0146(11) 0.0177(11) 0.0008(9) -0.0003(9) -0.0023(8)
C10 0.0129(10) 0.0150(11) 0.0162(10) 0.0002(9) 0.0011(9) 0.0015(9)
O1 0.0186(8) 0.0151(9) 0.0258(8) -0.0026(7) 0.0046(7) -0.0015(7)
O2 0.0164(8) 0.0142(9) 0.0262(9) -0.0015(7) 0.0082(7) -0.0002(7)
O3 0.0155(8) 0.0123(8) 0.0299(9) -0.0002(7) 0.0066(7) -0.0051(7)
S1 0.0185(3) 0.0155(3) 0.0225(3) -0.0032(2) -0.0012(2) -0.0010(2)
O4 0.0328(10) 0.0142(9) 0.0206(8) -0.0021(7) 0.0000(8) 0.0000(7)
C11 0.0239(13) 0.0219(14) 0.0238(12) -0.0004(11) 0.0002(11) 0.0023(10)
C12 0.0491(19) 0.0174(14) 0.0285(14) -0.0008(13) 0.0026(14) -0.0042(11)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
C1 N1 C5 121.2(2)
C1 N1 H1N 118.7(18)
C5 N1 H1N 119.8(17)
N1 C1 C2 122.0(2)
N1 C1 C10 114.9(2)
C2 C1 C10 123.1(2)
C1 C2 C3 120.8(2)
C1 C2 H2 117.8(17)
C3 C2 H2 121.3(17)
O3 C3 C2 123.3(2)
O3 C3 C4 120.2(2)
C2 C3 C4 116.4(2)
C5 C4 C6 118.8(2)
C5 C4 C3 119.9(2)
C6 C4 C3 121.3(2)
N1 C5 C4 119.7(2)
N1 C5 C9 119.9(2)
C4 C5 C9 120.4(2)
C7 C6 C4 120.3(2)
C7 C6 H6 122.4(18)
C4 C6 H6 117.2(17)
C6 C7 C8 120.4(2)
C6 C7 H7 120.3(16)
C8 C7 H7 119.2(16)
C9 C8 C7 120.7(2)
C9 C8 H8 120.1(17)
C7 C8 H8 119.2(17)
C8 C9 C5 119.3(2)
C8 C9 H9 121.9(17)
C5 C9 H9 118.7(17)
O1 C10 O2 126.3(2)
O1 C10 C1 121.5(2)
O2 C10 C1 112.15(19)
C10 O2 H2O 111.2(19)
O4 S1 C11 105.51(12)
O4 S1 C12 105.35(14)
C11 S1 C12 98.24(15)
S1 C11 H11A 109.9(19)
S1 C11 H11B 107.1(18)
H11A C11 H11B 111(3)
S1 C11 H11C 107.1(19)
H11A C11 H11C 111(3)
H11B C11 H11C 110(3)
S1 C12 H12A 106(2)
S1 C12 H12B 108(2)
H12A C12 H12B 112(3)
S1 C12 H12C 109(2)
H12A C12 H12C 112(3)
H12B C12 H12C 109(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N1 C1 1.355(3)
N1 C5 1.372(3)
N1 H1N 0.88(3)
C1 C2 1.363(3)
C1 C10 1.504(3)
C2 C3 1.425(3)
C2 H2 0.93(3)
C3 O3 1.270(3)
C3 C4 1.452(3)
C4 C5 1.408(3)
C4 C6 1.411(3)
C5 C9 1.412(3)
C6 C7 1.375(3)
C6 H6 0.93(3)
C7 C8 1.404(3)
C7 H7 0.99(3)
C8 C9 1.376(3)
C8 H8 0.96(3)
C9 H9 0.99(3)
C10 O1 1.210(3)
C10 O2 1.309(3)
O2 H2O 0.92(3)
S1 O4 1.5112(18)
S1 C11 1.779(3)
S1 C12 1.789(3)
C11 H11A 0.95(3)
C11 H11B 0.97(3)
C11 H11C 0.94(3)
C12 H12A 1.00(3)
C12 H12B 0.96(4)
C12 H12C 0.96(4)
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
N1 H1N O4 . 0.88(3) 1.97(3) 2.816(3) 159(2)
O2 H2O O3 3_546 0.92(3) 1.61(3) 2.494(2) 162(3)
_cod_database_fobs_code 2021697