#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176760 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/93/2019374.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_2019374 loop_ _publ_author_name 'H\"utzler, Wilhelm Maximilian' 'Egert, Ernst' _publ_section_title ; N---H···S and N---H···O hydrogen bonds: `pure' and `mixed' R^2^~2~(8) patterns in the crystal structures of eight 2-thiouracil derivatives ; _journal_coeditor_code EG3147 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 241 _journal_page_last 249 _journal_paper_doi 10.1107/S2053229614001387 _journal_volume 70 _journal_year 2014 _chemical_formula_iupac 'C5 H6 N2 O2 S, C4 H9 N O' _chemical_formula_moiety 'C5 H6 N2 O2 S, C4 H9 N O' _chemical_formula_sum 'C9 H15 N3 O3 S' _chemical_formula_weight 245.30 _chemical_name_systematic ; 5-Methoxy-2-thiouracil--dimethylacetamide (1/1) ; _space_group_IT_number 11 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yb' _symmetry_space_group_name_H-M 'P 1 21/m 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90.00 _cell_angle_beta 97.170(15) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.225(3) _cell_length_b 6.4726(8) _cell_length_c 13.867(3) _cell_measurement_reflns_used 6964 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 26.27 _cell_measurement_theta_min 3.27 _cell_volume 1177.7(4) _computing_cell_refinement 'X-AREA (Stoe & Cie, 2001)' _computing_data_collection 'X-AREA (Stoe & Cie, 2001)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2001)' _computing_molecular_graphics ; Mercury (Macrae et al., 2008) and XP in SHELXTL-Plus (Sheldrick, 2008) ; _computing_publication_material 'publCIF (Westrip, 2010)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measurement_device_type 'Stoe IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_radiation_monochromator 'Genix 3D multilayer optics' _diffrn_radiation_source 'Genix 3D I\mS microfocus X-ray source' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1157 _diffrn_reflns_av_sigmaI/netI 0.0840 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 9319 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 3.27 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.272 _exptl_absorpt_correction_T_max 0.9681 _exptl_absorpt_correction_T_min 0.9228 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(X-AREA; Stoe & Cie, 2001)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 520 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.495 _refine_diff_density_min -0.421 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 227 _refine_ls_number_reflns 2470 _refine_ls_number_restraints 260 _refine_ls_restrained_S_all 1.166 _refine_ls_R_factor_all 0.1152 _refine_ls_R_factor_gt 0.0766 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0805P)^2^+1.0888P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1736 _refine_ls_wR_factor_ref 0.1901 _reflns_number_gt 1767 _reflns_number_total 2470 _reflns_threshold_expression I>2\s(I) _iucr_refine_instructions_details ; TITL IIa in P21/m CELL 0.71073 13.225 6.4726 13.867 90.000 97.170 90.000 ZERR 4 0.003 0.0008 0.003 0.000 0.015 0.000 LATT 1 SYMM - X , 0.5 + Y , - Z SFAC C H N O S UNIT 36 60 12 12 4 SIZE 0.30 0.18 0.12 REM farblose Nadel ACTA 50 L.S. 10 BOND $H CONF FMAP 2 PLAN 10 TEMP -100 OMIT -6 1 2 OMIT -6 0 3 OMIT 6 0 1 SIMU C1X > N3Y' DELU C1X > N3Y' HTAB N1A O21X HTAB N3A S21B HTAB N1B O21Y HTAB N3B S21A DFIX 0.88 0.02 N1A H1A N3A H3A N1B H1B N3B H3B DFIX 1.52 0.01 C1X C2X C31X C2X' C1Y C2Y C31Y C2Y' DFIX 1.25 0.01 C2X O21X C2X' O21X C2Y O21Y C2Y' O21Y DFIX 1.30 0.01 C2X N3X C2X' N3X' C2Y N3Y C2Y' N3Y' DFIX 1.47 0.01 N3X C31X N3X C32X N3X' C1X N3X' C32X DFIX 1.47 0.01 N3Y C31Y N3Y C32Y N3Y' C1Y N3Y' C32Y DFIX 2.42 0.02 O21X C1X O21X C31X O21Y C1Y O21Y C31Y DFIX 2.23 0.02 O21X N3X O21X N3X' O21Y N3Y O21Y N3Y' DFIX 2.41 0.02 C1X N3X C31X N3X' C1Y N3Y C31Y N3Y' DFIX 2.41 0.02 C2X C31X C2X' C1X C2Y C31Y C2Y' C1Y DFIX 2.43 0.02 C2X C32X C2X' C32X C2Y C32Y C2Y' C32Y DFIX 2.52 0.02 C31X C32X C1X C32X C31Y C32Y C1Y C32Y WGHT 0.080500 1.088800 FVAR 0.19017 0.66838 0.75931 N1A 3 0.457470 0.250000 0.465662 10.50000 0.01771 0.04185 = 0.02332 0.00000 0.00265 0.00000 H1A 2 0.521076 0.250000 0.457031 10.50000 -1.20000 C2A 1 0.383704 0.250000 0.390179 10.50000 0.02373 0.02604 = 0.02249 0.00000 0.00048 0.00000 S21A 5 0.408628 0.250000 0.274306 10.50000 0.02321 0.04538 = 0.02322 0.00000 0.00207 0.00000 N3A 3 0.286962 0.250000 0.415071 10.50000 0.01553 0.02886 = 0.02383 0.00000 -0.00144 0.00000 H3A 2 0.237775 0.250000 0.366978 10.50000 -1.20000 C4A 1 0.258213 0.250000 0.507891 10.50000 0.02270 0.02293 = 0.02918 0.00000 0.00655 0.00000 O41A 4 0.168334 0.250000 0.520278 10.50000 0.01875 0.04732 = 0.03489 0.00000 0.00348 0.00000 C5A 1 0.344259 0.250000 0.584654 10.50000 0.02580 0.02892 = 0.01973 0.00000 0.00113 0.00000 O51A 4 0.316294 0.250000 0.675364 10.50000 0.02412 0.04938 = 0.02326 0.00000 0.00375 0.00000 C52A 1 0.399553 0.250000 0.752542 10.50000 0.03057 0.05174 = 0.02123 0.00000 -0.00332 0.00000 AFIX 33 H5AA 2 0.372762 0.250000 0.815322 10.50000 -1.50000 H5AB 2 0.441347 0.373624 0.747478 10.50000 -1.50000 H5AC 2 0.441347 0.126376 0.747478 10.50000 -1.50000 AFIX 0 C6A 1 0.438840 0.250000 0.561624 10.50000 0.02606 0.03041 = 0.02645 0.00000 -0.00240 0.00000 AFIX 43 H6A 2 0.494619 0.250000 0.611939 10.50000 -1.20000 AFIX 0 N1B 3 0.033997 0.250000 0.050655 10.50000 0.01642 0.03326 = 0.03219 0.00000 0.00478 0.00000 H1B 2 -0.032817 0.250000 0.054692 10.50000 -1.20000 C2B 1 0.105615 0.250000 0.127421 10.50000 0.02199 0.02035 = 0.02993 0.00000 -0.00166 0.00000 S21B 5 0.077677 0.250000 0.243162 10.50000 0.02300 0.04387 = 0.02768 0.00000 0.00137 0.00000 N3B 3 0.203209 0.250000 0.105976 10.50000 0.02277 0.03089 = 0.02666 0.00000 -0.00112 0.00000 H3B 2 0.251849 0.250000 0.154738 10.50000 -1.20000 C4B 1 0.234389 0.250000 0.013451 10.50000 0.02283 0.02601 = 0.02947 0.00000 0.00169 0.00000 O41B 4 0.324210 0.250000 0.003761 10.50000 0.02062 0.04244 = 0.04060 0.00000 0.00053 0.00000 C5B 1 0.150889 0.250000 -0.064628 10.50000 0.02516 0.02514 = 0.02822 0.00000 0.00257 0.00000 O51B 4 0.182046 0.250000 -0.153428 10.50000 0.02249 0.04219 = 0.02169 0.00000 0.00188 0.00000 C52B 1 0.102918 0.250000 -0.234042 10.50000 0.02916 0.04600 = 0.02742 0.00000 -0.00160 0.00000 AFIX 33 H5BA 2 0.133398 0.250000 -0.294932 10.50000 -1.50000 H5BB 2 0.060617 0.373624 -0.231167 10.50000 -1.50000 H5BC 2 0.060616 0.126376 -0.231167 10.50000 -1.50000 AFIX 0 C6B 1 0.054806 0.250000 -0.044133 10.50000 0.01993 0.03222 = 0.02764 0.00000 -0.00374 0.00000 AFIX 43 H6B 2 0.000203 0.250000 -0.095620 10.50000 -1.20000 AFIX 0 C1X 1 0.772604 0.250000 0.669950 10.50000 0.08796 0.03618 = 0.03444 0.00000 0.01152 0.00000 AFIX 33 PART 1 H1XA 2 0.846837 0.250000 0.686557 20.50000 -1.50000 H1XB 2 0.743988 0.126376 0.697067 20.50000 -1.50000 H1XC 2 0.743988 0.373624 0.697067 20.50000 -1.50000 PART 2 H1XD 2 0.826834 0.250000 0.725000 -20.50000 -1.50000 H1XE 2 0.730324 0.126380 0.672910 -20.50000 -1.50000 H1XF 2 0.730324 0.373620 0.672910 -20.50000 -1.50000 AFIX 0 PART 0 O21X 4 0.658190 0.250000 0.515175 10.50000 0.02168 0.05214 = 0.06095 0.00000 -0.01007 0.00000 C31X 1 0.802279 0.250000 0.406357 10.50000 0.15989 0.05039 = 0.02974 0.00000 0.02024 0.00000 AFIX 33 PART 1 H3XA 2 0.865190 0.250000 0.375759 20.50000 -1.50000 H3XB 2 0.762333 0.373624 0.386236 20.50000 -1.50000 H3XC 2 0.762333 0.126376 0.386236 20.50000 -1.50000 PART 2 H3XD 2 0.876329 0.250000 0.424397 -20.50000 -1.50000 H3XE 2 0.782198 0.373620 0.367857 -20.50000 -1.50000 H3XF 2 0.782198 0.126380 0.367857 -20.50000 -1.50000 AFIX 0 PART 0 C32X 1 0.929023 0.250000 0.565021 10.50000 0.02484 0.06984 = 0.06234 0.00000 -0.00231 0.00000 AFIX 33 PART 1 H4XA 2 0.978819 0.250000 0.518277 20.50000 -1.50000 H4XB 2 0.938664 0.126376 0.605937 20.50000 -1.50000 H4XC 2 0.938664 0.373624 0.605938 20.50000 -1.50000 PART 2 H4XD 2 0.969673 0.250000 0.629151 -20.50000 -1.50000 H4XE 2 0.945013 0.373620 0.529031 -20.50000 -1.50000 H4XF 2 0.945013 0.126380 0.529031 -20.50000 -1.50000 AFIX 0 PART 0 C1Y 1 -0.241593 0.250000 0.166323 10.50000 0.05916 0.03196 = 0.03519 0.00000 -0.00226 0.00000 AFIX 33 PART 1 H1YA 2 -0.311314 0.250000 0.183362 30.50000 -1.50000 H1YB 2 -0.205730 0.373624 0.193247 30.50000 -1.50000 H1YC 2 -0.205730 0.126376 0.193246 30.50000 -1.50000 PART 2 H1YD 2 -0.280683 0.250000 0.221893 -30.50000 -1.50000 H1YE 2 -0.198563 0.373620 0.168813 -30.50000 -1.50000 H1YF 2 -0.198563 0.126380 0.168813 -30.50000 -1.50000 AFIX 0 PART 0 O21Y 4 -0.169634 0.250000 0.010750 10.50000 0.01991 0.05848 = 0.05460 0.00000 0.00603 0.00000 C31Y 1 -0.344625 0.250000 -0.098192 10.50000 0.04628 0.05671 = 0.03542 0.00000 -0.01469 0.00000 AFIX 33 PART 1 H3YA 2 -0.416700 0.250000 -0.125295 30.50000 -1.50000 H3YB 2 -0.311372 0.126376 -0.120209 30.50000 -1.50000 H3YC 2 -0.311372 0.373624 -0.120209 30.50000 -1.50000 PART 2 H3YD 2 -0.413885 0.250000 -0.080002 -30.50000 -1.50000 H3YE 2 -0.334705 0.126380 -0.136722 -30.50000 -1.50000 H3YF 2 -0.334705 0.373620 -0.136722 -30.50000 -1.50000 AFIX 0 PART 0 C32Y 1 -0.426560 0.250000 0.060059 10.50000 0.02755 0.07000 = 0.06719 0.00000 0.01604 0.00000 AFIX 33 PART 1 H4YA 2 -0.488024 0.250000 0.012594 30.50000 -1.50000 H4YB 2 -0.426073 0.373624 0.100916 30.50000 -1.50000 H4YC 2 -0.426073 0.126376 0.100916 30.50000 -1.50000 PART 2 H4YD 2 -0.451670 0.250000 0.123629 -30.50000 -1.50000 H4YE 2 -0.451340 0.126380 0.023719 -30.50000 -1.50000 H4YF 2 -0.451340 0.373620 0.023719 -30.50000 -1.50000 AFIX 0 PART 1 C2X 1 0.746019 0.250000 0.559184 20.50000 0.02055 0.02207 = 0.04385 0.00000 -0.00359 0.00000 N3X 3 0.828007 0.250000 0.513706 20.50000 0.02522 0.03942 = 0.03599 0.00000 -0.00327 0.00000 PART 2 C2X' 1 0.748847 0.250000 0.499341 -20.50000 0.02996 0.02173 = 0.03547 0.00000 -0.00480 0.00000 N3X' 3 0.818888 0.250000 0.576939 -20.50000 0.03087 0.02959 = 0.02765 0.00000 -0.00619 0.00000 PART 1 C2Y 1 -0.244679 0.250000 0.057248 30.50000 0.02475 0.02889 = 0.03223 0.00000 -0.00197 0.00000 N3Y 3 -0.336242 0.250000 0.008918 30.50000 0.01837 0.03767 = 0.04487 0.00000 0.00320 0.00000 PART 2 C2Y' 1 -0.267036 0.250000 -0.005787 -30.50000 0.02234 0.03578 = 0.03370 0.00000 0.00097 0.00000 N3Y' 3 -0.313326 0.250000 0.073871 -30.50000 0.02529 0.04054 = 0.03695 0.00000 0.00568 0.00000 PART 0 HKLF 4 REM mh15_2 in P21/m REM R1 = 0.0766 for 1767 Fo > 4sig(Fo) and 0.1152 for all 2470 data REM 227 parameters refined using 260 restraints END ; _cod_data_source_file eg3147sup1.cif _cod_data_source_block IIa _cod_original_sg_symbol_H-M 'P 21/m' _cod_database_code 2019374 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -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_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_disorder_assembly _atom_site_disorder_group N N1A 0.4575(3) 0.2500 0.4657(3) 0.0276(12) Uani d SD 1 2 . . H H1A 0.521(2) 0.2500 0.457(4) 0.033 Uiso d SD 1 2 . . C C2A 0.3837(4) 0.2500 0.3902(4) 0.0243(12) Uani d S 1 2 . . S S21A 0.40863(10) 0.2500 0.27431(9) 0.0307(4) Uani d S 1 2 . . N N3A 0.2870(3) 0.2500 0.4151(3) 0.0231(10) Uani d SD 1 2 . . H H3A 0.238(3) 0.2500 0.367(3) 0.028 Uiso d SD 1 2 . . C C4A 0.2582(4) 0.2500 0.5079(4) 0.0247(12) Uani d S 1 2 . . O O41A 0.1683(3) 0.2500 0.5203(3) 0.0336(11) Uani d S 1 2 . . C C5A 0.3443(4) 0.2500 0.5847(3) 0.0250(12) Uani d S 1 2 . . O O51A 0.3163(3) 0.2500 0.6754(3) 0.0322(10) Uani d S 1 2 . . C C52A 0.3996(5) 0.2500 0.7525(4) 0.0351(15) Uani d S 1 2 . . H H5AA 0.3728 0.2500 0.8153 0.053 Uiso calc SR 1 2 . . H H5AB 0.4413 0.3736 0.7475 0.053 Uiso calc PR 0.50 1 . . H H5AC 0.4413 0.1264 0.7475 0.053 Uiso calc PR 0.50 1 . . C C6A 0.4388(4) 0.2500 0.5616(4) 0.0281(13) Uani d S 1 2 . . H H6A 0.4946 0.2500 0.6119 0.034 Uiso calc SR 1 2 . . N N1B 0.0340(3) 0.2500 0.0507(3) 0.0271(11) Uani d SD 1 2 . . H H1B -0.0328(19) 0.2500 0.055(4) 0.033 Uiso d SD 1 2 . . C C2B 0.1056(4) 0.2500 0.1274(4) 0.0245(12) Uani d S 1 2 . . S S21B 0.07768(11) 0.2500 0.24316(10) 0.0317(4) Uani d S 1 2 . . N N3B 0.2032(4) 0.2500 0.1060(3) 0.0271(11) Uani d SD 1 2 . . H H3B 0.252(3) 0.2500 0.155(3) 0.033 Uiso d SD 1 2 . . C C4B 0.2344(4) 0.2500 0.0135(4) 0.0262(13) Uani d S 1 2 . . O O41B 0.3242(3) 0.2500 0.0038(3) 0.0348(11) Uani d S 1 2 . . C C5B 0.1509(4) 0.2500 -0.0646(4) 0.0262(12) Uani d S 1 2 . . O O51B 0.1820(3) 0.2500 -0.1534(2) 0.0289(10) Uani d S 1 2 . . C C52B 0.1029(5) 0.2500 -0.2340(4) 0.0346(15) Uani d S 1 2 . . H H5BA 0.1334 0.2500 -0.2949 0.052 Uiso calc SR 1 2 . . H H5BB 0.0606 0.3736 -0.2312 0.052 Uiso calc PR 0.50 1 . . H H5BC 0.0606 0.1264 -0.2312 0.052 Uiso calc PR 0.50 1 . . C C6B 0.0548(4) 0.2500 -0.0441(4) 0.0272(13) Uani d S 1 2 . . H H6B 0.0002 0.2500 -0.0956 0.033 Uiso calc SR 1 2 . . C C1X 0.7726(6) 0.2500 0.6700(4) 0.0525(19) Uani d SDU 1 2 . . H H1XA 0.8468 0.2500 0.6866 0.079 Uiso calc SPR 0.668(12) 2 A 1 H H1XB 0.7440 0.1264 0.6971 0.079 Uiso calc PR 0.334(6) 1 A 1 H H1XC 0.7440 0.3736 0.6971 0.079 Uiso calc PR 0.334(6) 1 A 1 H H1XD 0.8268 0.2500 0.7250 0.079 Uiso d SPR 0.332(12) 2 A 2 H H1XE 0.7303 0.1264 0.6729 0.079 Uiso d PR 0.166(6) 1 A 2 H H1XF 0.7303 0.3736 0.6729 0.079 Uiso d PR 0.166(6) 1 A 2 O O21X 0.6582(3) 0.2500 0.5152(3) 0.0462(13) Uani d SDU 1 2 . . C C31X 0.8023(8) 0.2500 0.4064(4) 0.079(3) Uani d SDU 1 2 . . H H3XA 0.8652 0.2500 0.3758 0.119 Uiso calc SPR 0.668(12) 2 A 1 H H3XB 0.7623 0.3736 0.3862 0.119 Uiso calc PR 0.334(6) 1 A 1 H H3XC 0.7623 0.1264 0.3862 0.119 Uiso calc PR 0.334(6) 1 A 1 H H3XD 0.8763 0.2500 0.4244 0.119 Uiso d SPR 0.332(12) 2 A 2 H H3XE 0.7822 0.3736 0.3679 0.119 Uiso d PR 0.166(6) 1 A 2 H H3XF 0.7822 0.1264 0.3679 0.119 Uiso d PR 0.166(6) 1 A 2 C C32X 0.9290(4) 0.2500 0.5650(5) 0.053(2) Uani d SDU 1 2 . . H H4XA 0.9788 0.2500 0.5183 0.079 Uiso calc SPR 0.668(12) 2 A 1 H H4XB 0.9387 0.1264 0.6059 0.079 Uiso calc PR 0.334(6) 1 A 1 H H4XC 0.9387 0.3736 0.6059 0.079 Uiso calc PR 0.334(6) 1 A 1 H H4XD 0.9697 0.2500 0.6292 0.079 Uiso d SPR 0.332(12) 2 A 2 H H4XE 0.9450 0.3736 0.5290 0.079 Uiso d PR 0.166(6) 1 A 2 H H4XF 0.9450 0.1264 0.5290 0.079 Uiso d PR 0.166(6) 1 A 2 C C1Y -0.2416(5) 0.2500 0.1663(4) 0.0428(16) Uani d SDU 1 2 . . H H1YA -0.3113 0.2500 0.1834 0.064 Uiso calc SPR 0.759(11) 2 B 1 H H1YB -0.2057 0.3736 0.1932 0.064 Uiso calc PR 0.380(6) 1 B 1 H H1YC -0.2057 0.1264 0.1932 0.064 Uiso calc PR 0.380(6) 1 B 1 H H1YD -0.2807 0.2500 0.2219 0.064 Uiso d SPR 0.241(11) 2 B 2 H H1YE -0.1986 0.3736 0.1688 0.064 Uiso d PR 0.120(6) 1 B 2 H H1YF -0.1986 0.1264 0.1688 0.064 Uiso d PR 0.120(6) 1 B 2 O O21Y -0.1696(3) 0.2500 0.0108(3) 0.0442(13) Uani d SDU 1 2 . . C C31Y -0.3446(5) 0.2500 -0.0982(4) 0.0478(18) Uani d SDU 1 2 . . H H3YA -0.4167 0.2500 -0.1253 0.072 Uiso calc SPR 0.759(11) 2 B 1 H H3YB -0.3114 0.1264 -0.1202 0.072 Uiso calc PR 0.380(6) 1 B 1 H H3YC -0.3114 0.3736 -0.1202 0.072 Uiso calc PR 0.380(6) 1 B 1 H H3YD -0.4139 0.2500 -0.0800 0.072 Uiso d SPR 0.241(11) 2 B 2 H H3YE -0.3347 0.1264 -0.1367 0.072 Uiso d PR 0.120(6) 1 B 2 H H3YF -0.3347 0.3736 -0.1367 0.072 Uiso d PR 0.120(6) 1 B 2 C C32Y -0.4266(4) 0.2500 0.0601(5) 0.054(2) Uani d SDU 1 2 . . H H4YA -0.4880 0.2500 0.0126 0.081 Uiso calc SPR 0.759(11) 2 B 1 H H4YB -0.4261 0.3736 0.1009 0.081 Uiso calc PR 0.380(6) 1 B 1 H H4YC -0.4261 0.1264 0.1009 0.081 Uiso calc PR 0.380(6) 1 B 1 H H4YD -0.4517 0.2500 0.1236 0.081 Uiso d SPR 0.241(11) 2 B 2 H H4YE -0.4513 0.1264 0.0237 0.081 Uiso d PR 0.120(6) 1 B 2 H H4YF -0.4513 0.3736 0.0237 0.081 Uiso d PR 0.120(6) 1 B 2 C C2X 0.7460(5) 0.2500 0.5592(5) 0.029(2) Uani d SPDU 0.668(12) 2 A 1 N N3X 0.8280(5) 0.2500 0.5137(5) 0.034(2) Uani d SPDU 0.668(12) 2 A 1 C C2X' 0.7488(6) 0.2500 0.4993(7) 0.030(4) Uani d SPDU 0.332(12) 2 A 2 N N3X' 0.8189(6) 0.2500 0.5769(6) 0.030(4) Uani d SPDU 0.332(12) 2 A 2 C C2Y -0.2447(5) 0.2500 0.0572(4) 0.0291(19) Uani d SPDU 0.759(11) 2 B 1 N N3Y -0.3362(4) 0.2500 0.0089(4) 0.0337(19) Uani d SPDU 0.759(11) 2 B 1 C C2Y' -0.2670(7) 0.2500 -0.0058(7) 0.031(5) Uani d SPDU 0.241(11) 2 B 2 N N3Y' -0.3133(7) 0.2500 0.0739(7) 0.034(5) Uani d SPDU 0.241(11) 2 B 2 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 N1A 0.018(2) 0.042(4) 0.023(2) 0.000 0.0026(18) 0.000 C2A 0.024(3) 0.026(3) 0.022(2) 0.000 0.000(2) 0.000 S21A 0.0232(7) 0.0454(11) 0.0232(6) 0.000 0.0021(5) 0.000 N3A 0.016(2) 0.029(3) 0.024(2) 0.000 -0.0014(16) 0.000 C4A 0.023(3) 0.023(3) 0.029(3) 0.000 0.007(2) 0.000 O41A 0.019(2) 0.047(3) 0.035(2) 0.000 0.0035(16) 0.000 C5A 0.026(3) 0.029(4) 0.020(2) 0.000 0.001(2) 0.000 O51A 0.024(2) 0.049(3) 0.0233(17) 0.000 0.0038(15) 0.000 C52A 0.031(3) 0.052(5) 0.021(2) 0.000 -0.003(2) 0.000 C6A 0.026(3) 0.030(4) 0.026(3) 0.000 -0.002(2) 0.000 N1B 0.016(2) 0.033(3) 0.032(2) 0.000 0.0048(19) 0.000 C2B 0.022(3) 0.020(3) 0.030(3) 0.000 -0.002(2) 0.000 S21B 0.0230(7) 0.0439(11) 0.0277(7) 0.000 0.0014(5) 0.000 N3B 0.023(2) 0.031(3) 0.027(2) 0.000 -0.0011(18) 0.000 C4B 0.023(3) 0.026(4) 0.029(3) 0.000 0.002(2) 0.000 O41B 0.021(2) 0.042(3) 0.041(2) 0.000 0.0005(17) 0.000 C5B 0.025(3) 0.025(3) 0.028(3) 0.000 0.003(2) 0.000 O51B 0.0225(19) 0.042(3) 0.0217(17) 0.000 0.0019(14) 0.000 C52B 0.029(3) 0.046(5) 0.027(3) 0.000 -0.002(2) 0.000 C6B 0.020(3) 0.032(4) 0.028(3) 0.000 -0.004(2) 0.000 C1X 0.088(6) 0.036(4) 0.034(3) 0.000 0.012(3) 0.000 O21X 0.022(2) 0.052(4) 0.061(3) 0.000 -0.0101(19) 0.000 C31X 0.160(9) 0.050(6) 0.030(3) 0.000 0.020(4) 0.000 C32X 0.025(3) 0.070(6) 0.062(4) 0.000 -0.002(3) 0.000 C1Y 0.059(4) 0.032(4) 0.035(3) 0.000 -0.002(3) 0.000 O21Y 0.020(2) 0.058(4) 0.055(3) 0.000 0.0060(18) 0.000 C31Y 0.046(4) 0.057(5) 0.035(3) 0.000 -0.015(3) 0.000 C32Y 0.028(3) 0.070(6) 0.067(4) 0.000 0.016(3) 0.000 C2X 0.021(4) 0.022(5) 0.044(5) 0.000 -0.004(4) 0.000 N3X 0.025(4) 0.039(5) 0.036(4) 0.000 -0.003(3) 0.000 C2X' 0.030(6) 0.022(10) 0.035(6) 0.000 -0.005(6) 0.000 N3X' 0.031(6) 0.030(9) 0.028(6) 0.000 -0.006(5) 0.000 C2Y 0.025(4) 0.029(5) 0.032(4) 0.000 -0.002(3) 0.000 N3Y 0.018(3) 0.038(5) 0.045(4) 0.000 0.003(3) 0.000 C2Y' 0.022(7) 0.036(13) 0.034(7) 0.000 0.001(6) 0.000 N3Y' 0.025(7) 0.041(12) 0.037(7) 0.000 0.006(6) 0.000 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 C2A N1A C6A 123.5(5) C2A N1A H1A 121(4) C6A N1A H1A 115(4) N1A C2A N3A 114.6(4) N1A C2A S21A 122.5(4) N3A C2A S21A 122.9(4) C2A N3A C4A 127.5(5) C2A N3A H3A 116(4) C4A N3A H3A 116(4) O41A C4A N3A 121.0(5) O41A C4A C5A 125.6(5) N3A C4A C5A 113.5(4) C6A C5A O51A 126.7(5) C6A C5A C4A 119.8(5) O51A C5A C4A 113.5(4) C5A O51A C52A 114.8(4) O51A C52A H5AA 109.5 O51A C52A H5AB 109.5 H5AA C52A H5AB 109.5 O51A C52A H5AC 109.5 H5AA C52A H5AC 109.5 H5AB C52A H5AC 109.5 C5A C6A N1A 121.1(5) C5A C6A H6A 119.4 N1A C6A H6A 119.4 C2B N1B C6B 123.8(5) C2B N1B H1B 124(4) C6B N1B H1B 112(4) N1B C2B N3B 115.1(4) N1B C2B S21B 122.7(4) N3B C2B S21B 122.2(4) C2B N3B C4B 126.7(5) C2B N3B H3B 117(4) C4B N3B H3B 116(4) O41B C4B N3B 120.5(5) O41B C4B C5B 125.7(5) N3B C4B C5B 113.7(5) C6B C5B O51B 127.0(5) C6B C5B C4B 119.9(5) O51B C5B C4B 113.1(5) C5B O51B C52B 115.9(4) O51B C52B H5BA 109.5 O51B C52B H5BB 109.5 H5BA C52B H5BB 109.5 O51B C52B H5BC 109.5 H5BA C52B H5BC 109.5 H5BB C52B H5BC 109.5 C5B C6B N1B 120.8(5) C5B C6B H6B 119.6 N1B C6B H6B 119.6 C2X C1X H1XA 109.5 C2X C1X H1XB 109.5 H1XA C1X H1XB 109.5 C2X C1X H1XC 109.5 H1XA C1X H1XC 109.5 H1XB C1X H1XC 109.5 N3X' C1X H1XD 109.5 N3X' C1X H1XE 109.5 H1XD C1X H1XE 109.5 N3X' C1X H1XF 109.5 H1XD C1X H1XF 109.5 H1XE C1X H1XF 109.5 N3X C31X H3XA 109.5 N3X C31X H3XB 109.5 H3XA C31X H3XB 109.5 N3X C31X H3XC 109.5 H3XA C31X H3XC 109.5 H3XB C31X H3XC 109.5 C2X' C31X H3XD 109.5 C2X' C31X H3XE 109.5 H3XD C31X H3XE 109.5 C2X' C31X H3XF 109.5 H3XD C31X H3XF 109.5 H3XE C31X H3XF 109.5 N3X C32X H4XA 109.5 N3X C32X H4XB 109.5 H4XA C32X H4XB 109.5 N3X C32X H4XC 109.5 H4XA C32X H4XC 109.5 H4XB C32X H4XC 109.5 N3X' C32X H4XD 109.5 N3X' C32X H4XE 109.5 H4XD C32X H4XE 109.5 N3X' C32X H4XF 109.5 H4XD C32X H4XF 109.5 H4XE C32X H4XF 109.5 C2Y C1Y H1YA 109.5 C2Y C1Y H1YB 109.5 H1YA C1Y H1YB 109.5 C2Y C1Y H1YC 109.5 H1YA C1Y H1YC 109.5 H1YB C1Y H1YC 109.5 N3Y' C1Y H1YD 109.5 N3Y' C1Y H1YE 109.5 H1YD C1Y H1YE 109.5 N3Y' C1Y H1YF 109.5 H1YD C1Y H1YF 109.5 H1YE C1Y H1YF 109.5 N3Y C31Y H3YA 109.5 N3Y C31Y H3YB 109.5 H3YA C31Y H3YB 109.5 N3Y C31Y H3YC 109.5 H3YA C31Y H3YC 109.5 H3YB C31Y H3YC 109.5 C2Y' C31Y H3YD 109.5 C2Y' C31Y H3YE 109.5 H3YD C31Y H3YE 109.5 C2Y' C31Y H3YF 109.5 H3YD C31Y H3YF 109.5 H3YE C31Y H3YF 109.5 N3Y C32Y H4YA 109.5 N3Y C32Y H4YB 109.5 H4YA C32Y H4YB 109.5 N3Y C32Y H4YC 109.5 H4YA C32Y H4YC 109.5 H4YB C32Y H4YC 109.5 N3Y' C32Y H4YD 109.5 N3Y' C32Y H4YE 109.5 H4YD C32Y H4YE 109.5 N3Y' C32Y H4YF 109.5 H4YD C32Y H4YF 109.5 H4YE C32Y H4YF 109.5 O21X C2X N3X 122.6(6) O21X C2X C1X 125.1(6) N3X C2X C1X 112.3(6) C2X N3X C32X 122.2(6) C2X N3X C31X 112.3(6) C32X N3X C31X 125.5(6) O21X C2X' N3X' 116.5(8) O21X C2X' C31X 134.2(9) N3X' C2X' C31X 109.3(7) C2X' N3X' C32X 120.2(7) C2X' N3X' C1X 112.3(7) C32X N3X' C1X 127.5(7) O21Y C2Y N3Y 118.7(5) O21Y C2Y C1Y 126.4(5) N3Y C2Y C1Y 114.9(5) C2Y N3Y C32Y 120.7(6) C2Y N3Y C31Y 117.6(5) C32Y N3Y C31Y 121.6(5) O21Y C2Y' N3Y' 114.1(8) O21Y C2Y' C31Y 134.5(9) N3Y' C2Y' C31Y 111.3(7) C2Y' N3Y' C32Y 117.0(7) C2Y' N3Y' C1Y 113.8(7) C32Y N3Y' C1Y 129.1(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1A C2A 1.339(7) N1A C6A 1.383(7) N1A H1A 0.86(2) C2A N3A 1.366(7) C2A S21A 1.680(5) N3A C4A 1.387(6) N3A H3A 0.87(2) C4A O41A 1.222(6) C4A C5A 1.458(8) C5A C6A 1.329(8) C5A O51A 1.355(6) O51A C52A 1.437(7) C52A H5AA 0.9800 C52A H5AB 0.9800 C52A H5AC 0.9800 C6A H6A 0.9500 N1B C2B 1.334(7) N1B C6B 1.376(7) N1B H1B 0.89(2) C2B N3B 1.360(7) C2B S21B 1.691(5) N3B C4B 1.396(7) N3B H3B 0.87(2) C4B O41B 1.212(6) C4B C5B 1.447(8) C5B C6B 1.336(7) C5B O51B 1.346(6) O51B C52B 1.433(7) C52B H5BA 0.9800 C52B H5BB 0.9800 C52B H5BC 0.9800 C6B H6B 0.9500 C1X N3X' 1.495(8) C1X C2X 1.532(7) C1X H1XA 0.9800 C1X H1XB 0.9800 C1X H1XC 0.9800 C1X H1XD 0.9800 C1X H1XE 0.9799 C1X H1XF 0.9799 O21X C2X 1.243(7) O21X C2X' 1.246(8) C31X N3X 1.485(7) C31X C2X' 1.546(8) C31X H3XA 0.9800 C31X H3XB 0.9800 C31X H3XC 0.9800 C31X H3XD 0.9800 C31X H3XE 0.9800 C31X H3XF 0.9800 C32X N3X 1.433(7) C32X N3X' 1.486(8) C32X H4XA 0.9800 C32X H4XB 0.9800 C32X H4XC 0.9800 C32X H4XD 0.9801 C32X H4XE 0.9800 C32X H4XF 0.9800 C1Y N3Y' 1.497(9) C1Y C2Y 1.508(7) C1Y H1YA 0.9800 C1Y H1YB 0.9800 C1Y H1YC 0.9800 C1Y H1YD 0.9801 C1Y H1YE 0.9800 C1Y H1YF 0.9800 O21Y C2Y 1.249(6) O21Y C2Y' 1.280(8) C31Y N3Y 1.476(7) C31Y C2Y' 1.538(8) C31Y H3YA 0.9800 C31Y H3YB 0.9800 C31Y H3YC 0.9800 C31Y H3YD 0.9799 C31Y H3YE 0.9800 C31Y H3YF 0.9800 C32Y N3Y 1.463(6) C32Y N3Y' 1.486(8) C32Y H4YA 0.9800 C32Y H4YB 0.9800 C32Y H4YC 0.9800 C32Y H4YD 0.9800 C32Y H4YE 0.9800 C32Y H4YF 0.9800 C2X N3X 1.321(7) C2X' N3X' 1.329(9) C2Y N3Y 1.309(7) C2Y' N3Y' 1.328(9) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N1A H1A O21X 0.86(2) 1.89(4) 2.658(6) 147(6) N3A H3A S21B 0.87(2) 2.55(2) 3.420(5) 172(5) N1B H1B O21Y 0.89(2) 1.84(3) 2.681(6) 157(6) N3B H3B S21A 0.87(2) 2.49(2) 3.354(5) 171(5) 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 C6A N1A C2A N3A 0.0000(10) C6A N1A C2A S21A 180.0 N1A C2A N3A C4A 0.0000(10) S21A C2A N3A C4A 180.0 C2A N3A C4A O41A 180.0 C2A N3A C4A C5A 0.0000(10) O41A C4A C5A C6A 180.0000(10) N3A C4A C5A C6A 0.0000(10) O41A C4A C5A O51A 0.0000(10) N3A C4A C5A O51A 180.0 C6A C5A O51A C52A 0.000(2) C4A C5A O51A C52A 180.0000(10) O51A C5A C6A N1A 180.0000(10) C4A C5A C6A N1A 0.000(2) C2A N1A C6A C5A 0.0000(10) C6B N1B C2B N3B 0.0 C6B N1B C2B S21B 180.0 N1B C2B N3B C4B 0.0 S21B C2B N3B C4B 180.0 C2B N3B C4B O41B 180.0 C2B N3B C4B C5B 0.0 O41B C4B C5B C6B 180.0 N3B C4B C5B C6B 0.0 O41B C4B C5B O51B 0.0 N3B C4B C5B O51B 180.0 C6B C5B O51B C52B 0.0 C4B C5B O51B C52B 180.0 O51B C5B C6B N1B 180.0 C4B C5B C6B N1B 0.0 C2B N1B C6B C5B 0.0 C2X' O21X C2X N3X 0.000(2) C2X' O21X C2X C1X 180.000(2) N3X' C1X C2X O21X 180.000(3) N3X' C1X C2X N3X 0.000(2) O21X C2X N3X C32X 180.000(2) C1X C2X N3X C32X 0.000(2) O21X C2X N3X C31X 0.000(2) C1X C2X N3X C31X 180.0000(10) N3X' C32X N3X C2X 0.000(2) N3X' C32X N3X C31X 180.000(2) C2X' C31X N3X C2X 0.000(2) C2X' C31X N3X C32X 180.000(2) C2X O21X C2X' N3X' 0.000(3) C2X O21X C2X' C31X 180.000(4) N3X C31X C2X' O21X 180.000(3) N3X C31X C2X' N3X' 0.000(3) O21X C2X' N3X' C32X 180.000(2) C31X C2X' N3X' C32X 0.0000(10) O21X C2X' N3X' C1X 0.000(2) C31X C2X' N3X' C1X 180.0000(10) N3X C32X N3X' C2X' 0.000(2) N3X C32X N3X' C1X 180.000(3) C2X C1X N3X' C2X' 0.000(3) C2X C1X N3X' C32X 180.000(3) C2Y' O21Y C2Y N3Y 0.0 C2Y' O21Y C2Y C1Y 180.0 N3Y' C1Y C2Y O21Y 180.0 N3Y' C1Y C2Y N3Y 0.0 O21Y C2Y N3Y C32Y 180.0 C1Y C2Y N3Y C32Y 0.0 O21Y C2Y N3Y C31Y 0.0 C1Y C2Y N3Y C31Y 180.0 N3Y' C32Y N3Y C2Y 0.0 N3Y' C32Y N3Y C31Y 180.0 C2Y' C31Y N3Y C2Y 0.0 C2Y' C31Y N3Y C32Y 180.0 C2Y O21Y C2Y' N3Y' 0.0 C2Y O21Y C2Y' C31Y 180.0 N3Y C31Y C2Y' O21Y 180.0 N3Y C31Y C2Y' N3Y' 0.0 O21Y C2Y' N3Y' C32Y 180.0 C31Y C2Y' N3Y' C32Y 0.0 O21Y C2Y' N3Y' C1Y 0.0 C31Y C2Y' N3Y' C1Y 180.0 N3Y C32Y N3Y' C2Y' 0.0 N3Y C32Y N3Y' C1Y 180.0 C2Y C1Y N3Y' C2Y' 0.0 C2Y C1Y N3Y' C32Y 180.0