#------------------------------------------------------------------------------ #$Date: 2024-07-05 20:58:57 +0300 (Fri, 05 Jul 2024) $ #$Revision: 293266 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/98/7159895.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_7159895 loop_ _publ_author_name 'Gerasimova, Tatiana P.' 'Zagidullin, Almaz A.' 'Nikolaeva, Anastasiia N.' 'Fayzullin, Robert R.' 'Saitova, Aliya M.' 'Miluykov, Vasili A.' 'Grimme, Stefan' 'Katsyuba, Sergey A.' _publ_section_title ; Structural flexibility of favipiravir and its structural analogues in solutions: experimental and computational insight. ; _journal_issue 18 _journal_name_full 'Organic & biomolecular chemistry' _journal_page_first 3668 _journal_page_last 3683 _journal_paper_doi 10.1039/d4ob00404c _journal_volume 22 _journal_year 2024 _chemical_formula_moiety 'C8 H10 K N5 O5' _chemical_formula_sum 'C8 H10 K N5 O5' _chemical_formula_weight 295.31 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2024-02-18 deposited with the CCDC. 2024-04-09 downloaded from the CCDC. ; _cell_angle_alpha 86.9918(11) _cell_angle_beta 85.9992(11) _cell_angle_gamma 68.7003(10) _cell_formula_units_Z 2 _cell_length_a 8.1404(3) _cell_length_b 8.4811(4) _cell_length_c 9.2843(4) _cell_measurement_reflns_used 31722 _cell_measurement_temperature 162(2) _cell_measurement_theta_max 37.66 _cell_measurement_theta_min 2.20 _cell_volume 595.49(4) _computing_cell_refinement 'APEX4 v2021.10-0 (Bruker AXS)' _computing_data_collection 'APEX4 v2021.10-0 (Bruker AXS)' _computing_data_reduction 'APEX4 v2021.10-0 (Bruker AXS)' _computing_molecular_graphics ; WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012); PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009) ; _computing_publication_material ; WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012); PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009) ; _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT-2018/2 (Sheldrick, 2015)' _diffrn_ambient_temperature 162(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.891 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_unetI/netI 0.0228 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.891 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 70459 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.891 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 37.780 _diffrn_reflns_theta_min 2.200 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 0.473 _exptl_absorpt_correction_T_max 0.8806 _exptl_absorpt_correction_T_min 0.7348 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; SADABS-2016/2 (Stalke et al., 2015) Equivalent reflections defined by point group -1 for scaling and error model Mean and maximum errors in direction cosine check function = 0.001 0.003 Restraint esd for equal adjacent scale factors = 0.0090 Maximum odd and even orders for spherical harmonics = 1 4 wR2(int) = 0.1614 (selected reflections only, before parameter refinement) wR2(int) = 0.0532 (selected reflections only, after parameter refinement) 70839 total and 5676 unique reflections assuming Friedel's law plus 2776 total and 1529 unique reflections in fast scans Reflections rejected for which |I-|/su > 3.00 where: su^2 = sigma(I)^2 + ( 0.04000 )^2 (sigma(I) from SAINT) 70457 total and 5676 unique reflections left after |I-|/su test plus 2692 total and 1520 unique reflections in fast scans su^2 = [K*sigma(I)]^2 + [g]^2 where sigma(I) is from SAINT Error model 5: refine all K and overall g Run 2theta R(int) Incid. factors Diffr. factors K g I/s(lim) Total I>2sig(I) 1 21.9 0.0409 0.152 - 0.377 0.991 - 1.040 0.918 0.0262 38.2 4169 3080 2 21.9 0.0348 0.078 - 0.221 0.987 - 1.039 0.911 0.0262 38.2 4140 3301 3 21.9 0.0344 0.103 - 0.142 0.987 - 1.025 0.921 0.0262 38.2 4073 3292 4 21.9 0.0415 0.119 - 0.350 0.987 - 1.035 0.889 0.0262 38.2 4140 3165 5 21.9 0.0404 0.144 - 0.280 0.991 - 1.036 0.943 0.0262 38.2 4164 3145 6 21.9 0.0405 0.099 - 0.336 0.987 - 1.037 0.934 0.0262 38.2 4206 3166 7 21.9 0.0435 0.142 - 0.384 0.987 - 1.038 0.960 0.0262 38.2 4201 3119 8 21.9 0.0359 0.128 - 0.189 0.987 - 1.027 0.933 0.0262 38.2 4114 3234 9 21.9 0.0418 0.148 - 0.349 0.987 - 1.029 0.908 0.0262 38.2 4170 3144 10 21.9 0.0324 0.082 - 0.146 0.987 - 1.035 0.933 0.0262 38.2 4115 3409 11 21.9 0.0424 0.127 - 0.366 0.987 - 1.031 0.923 0.0262 38.2 4135 3117 12 21.9 0.0384 0.102 - 0.313 0.988 - 1.040 0.959 0.0262 38.2 6218 4971 13 21.9 0.0411 0.120 - 0.312 0.987 - 1.040 1.022 0.0262 38.2 6873 5368 14 -21.9 0.0371 0.081 - 0.275 0.987 - 1.040 0.933 0.0262 38.2 4081 3189 15 34.9 0.0288 0.141 - 0.311 0.994 - 1.040 0.891 0.0262 38.2 4493 3782 16 0.0 0.0351 0.189 - 0.268 0.991 - 1.040 1.061 0.0262 38.2 1761 1492 17 0.0 0.0320 0.154 - 0.256 0.987 - 1.026 1.014 0.0262 38.2 1404 1216 18f 0.0 0.0980 1.137 - 2.997 0.989 - 1.034 1.084 0.0262 38.2 2692 1689 2 Overloads replaced by fast scan measurements 70459 Corrected reflections written to file hkl Estimated minimum and maximum transmission: 0.7348 0.8806 The ratio of these values is more reliable than their absolute values! Additional spherical absorption correction applied with mu*r = 0.0800 3lambda correction factor = 0.00150 ; _exptl_crystal_colour 'light yellow' _exptl_crystal_density_diffrn 1.647 _exptl_crystal_description plate _exptl_crystal_F_000 304 _exptl_crystal_size_max 0.591 _exptl_crystal_size_mid 0.346 _exptl_crystal_size_min 0.130 _refine_diff_density_max 0.474 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.059 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 182 _refine_ls_number_reflns 5678 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0315 _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^)+(0.0356P)^2^+0.1456P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.0808 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4715 _reflns_number_total 5678 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ob00404c2.cif _cod_data_source_block zagid009 _cod_depositor_comments 'Adding full bibliography for 7159893--7159895.cif.' _cod_database_code 7159895 _shelx_shelxl_version_number 2018/3 _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 0.767 _shelx_estimated_absorpt_t_max 0.941 _shelx_res_file ; TITL zagid009 in P-1 shelx.res created by SHELXL-2018/3 at 10:52:49 on 18-Feb-2024 CELL 0.71073 8.14040 8.48110 9.28430 86.9918 85.9992 68.7003 ZERR 2.00 0.00030 0.00040 0.00040 0.0011 0.0011 0.0010 LATT 1 SFAC C H K N O UNIT 16 20 2 10 10 MERG 2 FREE K1 C1 MORE -1 HTAB N1 O3 EQIV $1 -x, -y+2, -z+2 HTAB N1 O2_$1 FMAP 2 PLAN 18 SIZE 0.130 0.346 0.591 ACTA BOND $H CONF LIST 4 L.S. 20 TEMP -111.15 WGHT 0.035600 0.145600 FVAR 0.83449 K1 3 0.015039 0.740574 0.922947 11.00000 0.01535 0.02150 = 0.02307 -0.00135 -0.00079 -0.00555 O1 5 0.207211 0.931920 1.009072 11.00000 0.01742 0.02293 = 0.03637 -0.01054 -0.00432 -0.00072 O2 5 -0.223627 0.828446 0.697403 11.00000 0.04455 0.02884 = 0.02203 -0.00241 -0.00264 -0.00569 O3 5 0.750144 0.641476 1.039773 11.00000 0.01665 0.02733 = 0.02383 -0.00122 -0.00390 -0.00814 O51 5 0.202596 0.585190 0.650398 11.00000 0.02081 0.02971 = 0.03306 -0.00632 -0.00777 -0.00519 O52 5 0.434946 0.375290 0.579209 11.00000 0.03164 0.02526 = 0.02591 -0.01001 0.00004 -0.00819 N1 4 0.448777 0.885978 1.135315 11.00000 0.02138 0.02352 = 0.02259 -0.00497 -0.00264 -0.00617 N2 4 0.381218 0.672493 0.837309 11.00000 0.01581 0.01620 = 0.01747 -0.00003 -0.00091 -0.00521 N3 4 0.743995 0.488949 0.848108 11.00000 0.01523 0.02134 = 0.02308 -0.00150 0.00061 -0.00341 N4 4 -0.178152 0.871024 0.456922 11.00000 0.03186 0.02322 = 0.02135 -0.00351 -0.00138 -0.00406 N5 4 0.361246 0.500112 0.653936 11.00000 0.02159 0.01986 = 0.01850 -0.00122 -0.00183 -0.00716 C1 1 0.365045 0.853858 1.028881 11.00000 0.01753 0.01610 = 0.02029 -0.00101 -0.00035 -0.00570 C2 1 0.473010 0.710924 0.932278 11.00000 0.01436 0.01576 = 0.01744 0.00010 -0.00062 -0.00512 C3 1 0.661472 0.615483 0.944376 11.00000 0.01435 0.01816 = 0.01851 0.00186 -0.00026 -0.00583 C4 1 0.647861 0.456507 0.753291 11.00000 0.01795 0.01943 = 0.02038 -0.00228 0.00130 -0.00370 AFIX 43 H4 2 0.703109 0.370028 0.685766 11.00000 -1.20000 AFIX 0 C5 1 0.467360 0.546419 0.750326 11.00000 0.01701 0.01713 = 0.01703 -0.00065 -0.00114 -0.00555 C6 1 -0.173777 0.775655 0.574687 11.00000 0.02507 0.01936 = 0.02553 -0.00311 -0.00521 -0.00333 AFIX 43 H6 2 -0.128457 0.656450 0.563998 11.00000 -1.20000 AFIX 0 C7 1 -0.250667 1.053794 0.463718 11.00000 0.10962 0.02295 = 0.04198 0.00440 0.01013 -0.00194 AFIX 137 H7A 2 -0.360997 1.097873 0.413456 11.00000 -1.50000 H7B 2 -0.165872 1.100737 0.417364 11.00000 -1.50000 H7C 2 -0.274224 1.086505 0.564935 11.00000 -1.50000 AFIX 0 C8 1 -0.111676 0.799534 0.316764 11.00000 0.03595 0.05273 = 0.02428 -0.01199 0.00172 -0.01368 AFIX 137 H8A 2 -0.011893 0.832368 0.281875 11.00000 -1.50000 H8B 2 -0.205599 0.842055 0.248437 11.00000 -1.50000 H8C 2 -0.072578 0.675830 0.325194 11.00000 -1.50000 AFIX 0 H1A 2 0.559334 0.829819 1.141916 11.00000 0.03817 H1B 2 0.389014 0.965734 1.192259 11.00000 0.03534 HKLF 4 REM zagid009 in P-1 REM wR2 = 0.0808, GooF = S = 1.045, Restrained GooF = 1.045 for all data REM R1 = 0.0315 for 4715 Fo > 4sig(Fo) and 0.0446 for all 5678 data REM 182 parameters refined using 0 restraints END WGHT 0.0356 0.1456 REM Highest difference peak 0.474, deepest hole -0.305, 1-sigma level 0.059 Q1 1 0.5541 0.4968 0.7523 11.00000 0.05 0.47 Q2 1 0.4245 0.7823 0.9774 11.00000 0.05 0.40 Q3 1 0.5697 0.6643 0.9370 11.00000 0.05 0.37 Q4 1 0.4269 0.6976 0.8819 11.00000 0.05 0.35 Q5 1 0.4165 0.5201 0.7068 11.00000 0.05 0.31 Q6 1 0.4272 0.6070 0.7963 11.00000 0.05 0.31 Q7 1 0.4185 0.8641 1.0833 11.00000 0.05 0.29 Q8 1 -0.1663 0.8350 0.5231 11.00000 0.05 0.29 Q9 1 0.6912 0.4711 0.8018 11.00000 0.05 0.28 Q10 1 0.6957 0.5544 0.8824 11.00000 0.05 0.26 Q11 1 -0.1721 0.8354 0.4054 11.00000 0.05 0.24 Q12 1 0.2919 0.6715 0.8462 11.00000 0.05 0.23 Q13 1 -0.3614 1.0948 0.5239 11.00000 0.05 0.23 Q14 1 -0.1789 0.8717 0.6821 11.00000 0.05 0.23 Q15 1 -0.3018 0.8416 0.6796 11.00000 0.05 0.23 Q16 1 0.2813 0.8842 1.0276 11.00000 0.05 0.23 Q17 1 0.7030 0.6196 1.0023 11.00000 0.05 0.23 Q18 1 0.8249 0.4546 0.8536 11.00000 0.05 0.22 ; _shelx_res_checksum 19385 _shelx_hkl_file ; -1 0 0 265.012 6.69401 10 -1 0 0 263.369 6.74705 8 -1 0 0 252.190 7.04586 1 -1 0 0 247.269 7.05607 7 -1 0 0 253.829 7.03802 9 -1 0 0 253.452 6.91932 5 -1 0 0 239.297 6.90269 6 -1 0 0 246.703 6.94724 4 -1 0 0 251.710 6.96716 11 -1 0 0 243.165 7.03283 11 -1 0 0 254.801 7.10673 17 -1 0 0 237.247 6.95859 12 -1 0 0 257.711 6.81060 14 -1 0 0 248.984 6.75756 2 -1 0 0 244.566 6.97680 13 -1 0 0 234.191 6.69063 15 1 0 0 246.552 7.08205 13 1 0 0 238.856 6.94354 12 1 0 0 249.779 6.92367 6 1 0 0 250.029 7.00880 13 1 0 0 256.432 7.03604 9 1 0 0 267.671 6.68545 10 1 0 0 265.257 6.94179 12 1 0 0 248.928 7.05735 1 1 0 0 248.020 6.69635 15 1 0 0 247.989 6.95873 4 1 0 0 254.827 6.98645 11 1 0 0 250.581 7.06545 7 1 0 0 258.711 7.06173 11 1 0 0 250.976 6.81160 14 1 0 0 245.956 6.74612 2 1 0 0 258.003 6.93101 5 1 0 0 253.879 6.75419 8 -2 0 0 357.082 9.95737 4 -2 0 0 361.579 10.2574 17 -2 0 0 354.064 10.0302 12 -2 0 0 346.038 9.85662 6 -2 0 0 354.239 9.97087 11 -2 0 0 350.452 10.1226 1 -2 0 0 356.685 10.1430 11 -2 0 0 361.391 9.52799 8 -2 0 0 352.497 9.43462 10 -2 0 0 349.147 9.57792 2 -2 0 0 349.555 10.0853 9 -2 0 0 355.414 9.86762 5 -2 0 0 341.232 9.66210 14 -2 0 0 344.895 9.98930 13 -2 0 0 358.737 10.1679 7 2 0 0 339.674 10.0582 13 2 0 0 339.060 9.65414 14 2 0 0 344.525 9.99151 4 2 0 0 357.325 10.0218 11 2 0 0 347.084 9.43820 15 2 0 0 357.288 10.1984 7 2 0 0 339.696 9.52677 2 2 0 0 347.219 9.93739 12 2 0 0 365.602 10.2537 17 2 0 0 346.522 10.1780 1 2 0 0 363.290 9.78948 12 2 0 0 354.536 10.0977 9 2 0 0 338.215 9.99710 13 2 0 0 358.314 9.89999 5 2 0 0 355.383 10.1361 11 2 0 0 332.693 9.87883 6 2 0 0 358.302 9.38916 10 2 0 0 354.748 9.55067 8 -3 0 0 1.30076 0.52187 7 -3 0 0 1.14354 0.37776 14 -3 0 0 1.78826 0.44047 12 -3 0 0 1.96138 0.60466 13 -3 0 0 1.59126 0.57963 11 -3 0 0 0.40608 0.47087 1 -3 0 0 1.10781 0.48417 5 -3 0 0 1.41865 0.27286 10 -3 0 0 0.99783 0.41684 4 -3 0 0 1.41362 0.53917 12 -3 0 0 0.58103 0.44964 9 -3 0 0 2.67227 0.52957 6 -3 0 0 0.74721 0.43577 17 -3 0 0 1.04165 0.30819 8 3 0 0 1.74219 0.61016 1 3 0 0 1.55895 0.56492 7 3 0 0 1.14010 0.26235 15 3 0 0 1.24800 0.53434 12 3 0 0 1.78753 0.45168 14 3 0 0 1.87997 0.58572 9 3 0 0 1.38682 0.52555 4 3 0 0 0.78091 0.41826 11 3 0 0 0.87991 0.46207 17 3 0 0 2.04463 0.56550 13 3 0 0 1.31383 0.31522 2 3 0 0 1.66488 0.67747 7 3 0 0 0.97605 0.45556 6 3 0 0 1.85917 0.36619 8 3 0 0 1.25205 0.22187 10 3 0 0 0.38639 0.37697 12 -4 0 0 520.446 14.7961 12 -4 0 0 520.942 15.5040 9 -4 0 0 519.598 14.9895 5 -4 0 0 547.040 15.1392 6 -4 0 0 529.699 14.1302 10 -4 0 0 525.114 14.2516 8 -4 0 0 515.449 15.1570 4 -4 0 0 505.741 14.4887 2 -4 0 0 520.832 15.4073 12 -4 0 0 515.946 15.7339 17 -4 0 0 466.069 14.5813 14 4 0 0 534.785 15.7858 7 4 0 0 520.652 15.2893 13 4 0 0 522.561 14.3976 2 4 0 0 518.866 15.4185 11 4 0 0 508.032 15.6389 1 4 0 0 522.672 14.8458 12 4 0 0 534.396 15.1682 5 4 0 0 524.178 14.0322 10 4 0 0 517.696 14.7062 14 4 0 0 536.230 14.3552 8 4 0 0 536.371 15.7044 17 4 0 0 520.716 15.5379 13 4 0 0 521.581 14.1728 15 -5 0 0 1131.51 30.9859 12 -5 0 0 1111.30 29.9552 10 -5 0 0 1135.40 32.2292 17 -5 0 0 1123.33 31.3431 6 -5 0 0 1107.14 30.1437 8 -5 0 0 1122.87 31.4735 4 -5 0 0 1123.31 31.7940 12 -5 0 0 1152.67 31.9233 9 -5 0 0 1124.62 30.6104 2 5 0 0 1140.54 32.0612 13 5 0 0 1127.28 32.3084 7 5 0 0 1104.86 30.0794 15 5 0 0 1124.86 30.9508 12 5 0 0 1113.51 32.0499 17 5 0 0 1076.43 30.8416 14 5 0 0 1116.37 31.5851 13 5 0 0 1116.96 30.2329 8 5 0 0 1131.07 32.1597 1 5 0 0 1142.12 31.3469 5 5 0 0 1127.13 29.8972 10 5 0 0 1128.75 31.8617 11 -6 0 0 110.643 5.85781 12 -6 0 0 103.055 5.30813 17 -6 0 0 108.569 4.13702 2 -6 0 0 103.775 3.59279 8 -6 0 0 106.201 4.77587 6 -6 0 0 105.651 3.32100 10 -6 0 0 107.404 5.20369 9 -6 0 0 108.689 4.54899 12 -6 0 0 105.347 3.27332 10 -6 0 0 104.606 4.88283 4 6 0 0 106.439 4.44807 14 6 0 0 107.449 5.41721 17 6 0 0 112.813 4.85686 5 6 0 0 107.750 5.39566 1 6 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53.5511 13 0 2 -2 1978.87 51.9447 6 0 2 -2 1920.54 53.2377 12 0 2 -2 1955.14 53.7008 13 0 2 -2 1944.33 52.6657 5 0 2 -2 2009.82 53.8787 7 0 2 -2 1954.93 53.6887 16 0 2 -2 1974.81 51.9888 6 0 2 -2 1958.93 52.3700 4 0 2 -2 2001.07 53.8200 11 0 -2 2 1972.46 53.3649 1 0 -2 2 1988.05 52.0436 6 0 -2 2 1854.60 53.7285 7 0 -2 2 1928.53 53.0508 12 0 -2 2 1889.22 53.5501 13 0 -2 2 1939.95 52.5556 4 0 -2 2 1934.67 53.1878 9 0 -2 2 1909.51 53.5811 16 -1 2 -2 1455.23 39.7887 7 -1 2 -2 1422.41 38.3810 8 -1 2 -2 1377.29 39.7800 1 -1 2 -2 1403.48 38.6619 12 -1 2 -2 1398.66 39.5930 13 -1 2 -2 1437.59 37.5930 10 -1 2 -2 1463.33 39.1146 9 -1 2 -2 1432.84 37.2859 2 -1 2 -2 1411.23 39.7566 16 -1 2 -2 1447.51 38.8996 5 -1 2 -2 1468.20 39.7278 11 -1 2 -2 1399.85 39.3415 13 -1 2 -2 1447.28 37.8515 6 -1 2 -2 1354.90 39.1170 12 -1 2 -2 1390.18 38.3256 4 1 -2 2 1415.82 38.7984 4 1 -2 2 1451.87 39.4755 16 1 -2 2 1394.98 39.8715 11 1 -2 2 1460.38 38.6891 5 1 -2 2 1423.65 38.3490 6 1 -2 2 1400.69 37.4084 2 1 -2 2 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5 3 4 13 0.05553 2.14439 10 3 4 13 -8.2109 3.73629 3 3 4 13 3.43051 2.93237 2 -4 -4 -13 65.4467 8.62004 1 -4 -4 -13 75.3014 4.38804 15 -4 -4 -13 90.8447 8.81634 14 -4 -4 -13 75.3028 7.70360 7 4 4 13 84.7768 6.42658 2 4 4 13 65.7960 5.22316 10 -5 -4 -13 4.14588 5.36257 1 -5 -4 -13 5.42632 5.06522 14 -5 -4 -13 -0.9915 3.95862 7 5 4 13 10.8206 5.07418 14 5 4 13 1.56296 3.27282 2 5 4 13 2.98411 2.79571 10 5 4 13 3.25221 4.02899 7 5 4 13 4.34754 5.40100 1 -6 -4 -13 10.5239 4.56585 7 6 4 13 9.00052 3.89132 2 6 4 13 9.70272 4.30293 7 6 4 13 9.53185 1.74648 15 7 4 13 8.73087 1.56118 15 8 4 13 2.96909 1.30138 15 4 -5 -13 12.9189 2.87483 15 3 -5 -13 4.45488 1.85957 15 2 -5 -13 18.1603 2.76501 15 -2 5 13 8.09352 5.40609 6 1 -5 -13 12.3937 2.26174 15 -1 5 13 9.05424 3.92912 6 0 -5 -13 14.1688 2.29567 15 0 -5 -13 21.6866 8.31804 1 0 5 13 13.6656 4.15928 6 -1 -5 -13 14.8286 2.28548 15 -1 -5 -13 12.8383 7.09692 1 1 5 13 21.9849 4.66917 6 -2 -5 -13 -0.7652 6.83289 1 -2 -5 -13 3.38903 5.30779 14 -2 -5 -13 4.23441 1.41868 15 -3 -5 -13 1.98639 1.25368 15 -3 -5 -13 2.23246 4.84920 14 -3 -5 -13 11.7766 6.74705 1 3 5 13 0.83073 3.51419 2 -4 -5 -13 9.63064 5.34200 14 -4 -5 -13 3.40995 5.33420 1 -4 -5 -13 8.09305 1.65151 15 4 5 13 7.83989 3.96557 2 -5 -5 -13 10.1823 5.78908 14 -5 -5 -13 16.9321 6.02135 1 5 5 13 10.2981 5.75019 1 5 5 13 11.4342 5.77334 14 5 5 13 10.9201 5.33700 2 -6 -5 -13 4.53676 7.27945 1 -6 -5 -13 8.70019 5.58008 14 6 5 13 4.59790 1.51297 15 6 5 13 4.16446 5.90831 1 6 5 13 1.06048 5.50489 14 7 5 13 9.95290 1.74427 15 8 5 13 -0.1511 0.99985 15 3 -6 -13 13.3986 2.66417 15 2 -6 -13 16.7699 2.76266 15 1 -6 -13 24.2745 3.22877 15 0 -6 -13 2.53373 1.31232 15 0 6 13 2.90264 4.34103 6 -1 -6 -13 1.17135 7.50327 1 -1 -6 -13 1.67303 1.15365 15 1 6 13 1.59430 4.25188 6 -2 -6 -13 9.48159 7.05450 1 -2 -6 -13 10.9308 2.02577 15 -3 -6 -13 101.064 5.31742 15 -3 -6 -13 84.0589 11.2704 1 3 6 13 80.3758 9.33705 6 -4 -6 -13 26.6946 2.67394 15 -4 -6 -13 29.7070 6.97634 1 -5 -6 -13 6.39704 1.60769 15 -5 -6 -13 11.7862 6.45860 1 5 6 13 3.47860 6.18912 1 7 6 13 1.14024 1.13223 15 8 6 13 20.2323 2.19092 15 2 -7 -13 3.82167 2.52890 15 1 -7 -13 3.23980 1.87030 15 0 -7 -13 11.5578 2.54517 15 -1 -7 -13 -1.5095 1.22811 15 -2 -7 -13 5.20292 1.73745 15 -3 -7 -13 8.14919 1.89819 15 3 7 13 7.87527 6.41863 6 -4 -7 -13 1.94409 1.17350 15 4 7 13 -0.0870 6.50031 6 -5 -7 -13 3.50980 1.40900 15 7 7 13 -2.3464 1.10656 15 8 7 13 2.44521 1.25700 15 0 -8 -13 1.65010 1.67777 15 -1 -8 -13 -0.4717 1.46037 15 -2 -8 -13 7.41624 2.10298 15 -3 -8 -13 11.5372 2.20478 15 -4 -8 -13 45.3196 3.63590 15 -5 -8 -13 8.12906 1.90587 15 7 8 13 33.7006 2.89935 15 -3 -9 -13 21.5973 2.87560 15 -4 -9 -13 58.9048 4.75564 15 -2 -6 14 11.6251 2.89381 15 -1 -6 14 2.70604 1.17258 15 0 -6 14 12.1371 1.73520 15 -4 -5 14 1.61449 1.25252 15 -3 -5 14 8.33337 1.71660 15 -2 -5 14 2.16828 1.25214 15 -1 -5 14 0.57445 1.04181 15 0 -5 14 3.11305 1.37635 15 1 -5 14 12.7746 2.03741 15 2 -5 14 1.77065 0.98104 15 -3 -4 14 30.0074 2.85637 15 -2 -4 14 6.35831 1.46923 15 -1 -4 14 29.3162 2.64633 15 0 -4 14 38.3303 2.96818 15 1 -4 14 1.83311 1.02979 15 3 -4 14 5.91375 1.30381 15 5 3 -14 1.45910 1.32041 15 4 3 -14 23.3214 2.53532 15 3 3 -14 27.5107 2.70421 15 -1 -3 14 22.5518 2.56221 15 0 -3 14 1.26535 0.99517 15 1 -3 14 0.41226 1.02372 15 2 -3 14 2.88058 1.15386 15 3 -3 14 0.01179 0.93424 15 4 -3 14 5.37042 1.37066 15 5 2 -14 8.73628 1.99723 15 4 2 -14 9.01052 1.73958 15 3 2 -14 20.2574 11.5285 11 2 2 -14 33.5288 8.10507 11 2 2 -14 41.5301 3.31141 15 1 2 -14 0.19165 5.76391 11 -1 -2 14 -0.7884 2.17436 2 0 2 -14 13.7575 6.07783 11 0 -2 14 12.6072 2.53051 2 1 -2 14 11.1755 1.93160 15 2 -2 14 22.5702 2.27122 15 3 -2 14 21.7610 2.23155 15 4 -2 14 3.52809 1.75328 15 5 -2 14 3.97035 1.20117 15 4 1 -14 14.5779 2.45647 15 3 1 -14 2.85333 1.43311 15 2 1 -14 19.7180 7.19941 14 2 1 -14 30.1434 2.85012 15 1 1 -14 -0.2596 0.88164 15 -1 -1 14 -0.9315 2.29004 2 0 1 -14 1.84699 1.06732 15 0 1 -14 2.54875 5.44992 11 0 -1 14 1.69111 2.07641 2 -1 1 -14 -1.1054 4.53101 11 1 -1 14 1.22955 3.63400 2 -2 1 -14 0.90305 4.34932 11 2 -1 14 1.97299 1.03614 15 3 -1 14 -0.4260 0.88423 15 4 -1 14 1.55324 1.07381 15 6 -1 14 4.49811 1.26105 15 5 0 -14 16.7757 2.75771 15 4 0 -14 10.5873 2.23704 15 3 0 -14 1.87926 1.33695 15 2 0 -14 21.4107 2.79145 15 2 0 -14 2.99216 6.37816 14 1 0 -14 13.7598 2.23373 15 1 0 -14 18.4225 6.31593 14 0 0 -14 10.8892 5.06893 11 0 0 -14 9.96569 1.98667 15 0 0 -14 15.8921 5.95051 14 0 0 -14 4.03610 10.3132 7 0 0 14 8.47592 2.39613 2 -1 0 -14 1.71359 1.05033 15 -1 0 -14 -2.3554 4.00780 11 -1 0 -14 1.31402 9.31871 7 1 0 14 2.91124 2.22442 2 2 0 14 13.4526 2.98540 2 -3 0 -14 15.7874 4.61613 11 3 0 14 14.4463 2.10538 15 4 0 14 32.5970 2.77412 15 5 0 14 7.19657 1.48999 15 6 0 14 3.43582 1.23555 15 5 -1 -14 47.7373 4.21361 15 4 -1 -14 -1.3561 1.75912 15 3 -1 -14 5.15292 1.73023 15 2 -1 -14 9.55192 1.91041 15 1 -1 -14 12.3572 2.16720 15 1 -1 -14 19.8306 6.76986 14 1 -1 -14 2.37967 7.55391 7 0 -1 -14 7.34963 1.73006 15 0 -1 -14 1.51010 6.51840 7 0 -1 -14 19.0711 9.84829 14 0 1 14 5.94129 2.68266 2 -1 -1 -14 3.22712 5.71862 7 -1 -1 -14 0.96833 5.52529 14 1 1 14 -1.7727 2.26303 2 -2 -1 -14 -1.2097 5.72356 7 -2 -1 -14 1.56368 3.78974 11 -2 -1 -14 1.44126 1.08160 15 2 1 14 0.04465 2.18474 2 -3 -1 -14 5.58943 5.86497 11 -4 -1 -14 0.32284 3.91090 11 4 1 14 2.09405 1.16031 15 5 1 14 1.87592 1.18889 15 7 1 14 1.69832 1.08289 15 4 -2 -14 5.29206 1.85022 15 3 -2 -14 10.7198 2.15607 15 2 -2 -14 12.4131 10.0270 7 2 -2 -14 19.9462 2.78809 15 1 -2 -14 1.01465 1.15266 15 1 -2 -14 -1.5405 7.06581 7 0 -2 -14 7.65484 1.84521 15 0 -2 -14 10.2326 6.12266 14 0 -2 -14 1.72699 6.53736 7 -1 -2 -14 8.72111 6.53475 7 -1 -2 -14 11.7712 2.03068 15 -1 -2 -14 9.59780 6.07932 14 1 2 14 9.00762 3.15055 2 -2 -2 -14 21.4099 6.24335 14 -2 -2 -14 18.4469 6.48446 7 -2 -2 -14 22.1561 2.52683 15 2 2 14 18.3263 3.25118 2 -3 -2 -14 -0.4499 4.81908 7 3 2 14 -0.4327 2.54335 2 4 2 14 39.1778 3.92328 13 4 2 14 60.2336 3.83512 15 4 2 14 50.1774 4.74723 2 -5 -2 -14 0.50023 4.97596 11 5 2 14 -1.1231 0.90261 15 6 2 14 85.7139 4.59942 15 7 2 14 0.87767 1.00476 15 4 -3 -14 0.48963 1.61630 15 3 -3 -14 18.0673 3.35826 15 2 -3 -14 8.97442 2.01163 15 1 -3 -14 0.88916 1.16421 15 0 -3 -14 15.8831 13.6723 7 0 -3 -14 22.2803 2.93687 15 -1 -3 -14 26.9752 3.20631 15 -1 -3 -14 22.0106 6.86410 14 -2 -3 -14 7.18349 5.93679 14 -2 -3 -14 6.24865 6.63978 7 -3 -3 -14 15.8954 6.02258 14 -3 -3 -14 6.08313 5.36004 7 -3 -3 -14 1.64079 1.11484 15 3 3 14 1.84525 4.27492 2 -4 -3 -14 5.42218 5.22723 7 4 3 14 2.25151 3.35451 2 5 3 14 2.43430 1.22509 15 5 3 14 2.06608 4.13532 2 6 3 14 77.0981 4.42680 15 7 3 14 15.3933 2.05078 15 3 -4 -14 1.97401 1.44900 15 1 -4 -14 22.1293 3.18173 15 0 -4 -14 7.51685 1.78283 15 -1 -4 -14 24.9966 3.14285 15 -2 -4 -14 -0.2829 1.03382 15 -3 -4 -14 10.4621 8.75114 14 -4 -4 -14 9.85513 6.46340 14 -4 -4 -14 10.9104 1.95401 15 4 4 14 11.1688 8.57488 14 6 4 14 10.6708 1.72550 15 7 4 14 8.62173 2.01720 15 2 -5 -14 3.83958 1.93011 15 1 -5 -14 4.36468 1.96514 15 0 -5 -14 -0.3924 1.29102 15 -1 -5 -14 9.33300 2.06502 15 -2 -5 -14 25.9488 2.85316 15 -3 -5 -14 6.10609 1.67413 15 -4 -5 -14 1.78943 1.24883 15 6 5 14 0.71442 1.20948 15 7 5 14 3.09837 1.48756 15 1 -6 -14 -2.2448 1.52993 15 0 -6 -14 17.0584 2.76773 15 -2 -6 -14 2.52532 1.56056 15 -3 -6 -14 2.27580 1.24992 15 -4 -6 -14 4.78151 1.58466 15 -5 -6 -14 37.5909 3.22573 15 -1 -7 -14 4.95117 2.04108 15 -2 -7 -14 25.8433 3.27274 15 -3 -7 -14 -0.1221 1.29626 15 -4 -7 -14 16.8667 3.49020 15 -5 -7 -14 2.69343 1.50688 15 -2 -4 15 6.71124 1.69588 15 -1 -4 15 0.41898 1.14738 15 0 -4 15 8.56818 1.72721 15 1 -4 15 -0.1144 1.05539 15 -2 -3 15 19.4168 2.59620 15 -1 -3 15 6.20997 1.53090 15 0 -3 15 8.79928 1.83301 15 1 -3 15 1.78352 1.20806 15 2 -3 15 4.11819 1.33091 15 3 2 -15 2.10393 1.31464 15 1 -2 15 -0.4516 1.92020 15 2 -2 15 5.43526 1.48826 15 3 -2 15 4.14958 1.34013 15 3 1 -15 -0.1932 1.30618 15 1 1 -15 40.8076 3.65043 15 1 -1 15 2.65456 1.41029 15 3 -1 15 -1.4745 0.98573 15 4 -1 15 14.9800 2.29048 15 3 0 -15 3.78598 1.56490 15 2 0 -15 34.5419 5.66361 15 1 0 -15 1.02067 1.37819 15 0 0 -15 0.55860 1.17098 15 2 0 15 -1.7685 1.15309 15 3 0 15 3.93343 1.96440 15 4 0 15 24.2095 2.64136 15 5 0 15 4.07319 1.29525 15 3 -1 -15 -0.6151 1.32198 15 2 -1 -15 24.2789 3.25294 15 0 -1 -15 8.54882 1.82006 15 -1 -1 -15 37.9941 3.29991 15 4 1 15 6.08230 1.52464 15 5 1 15 25.5894 2.61871 15 2 -2 -15 6.06783 2.08860 15 1 -2 -15 4.49336 1.70224 15 0 -2 -15 0.59914 1.75269 15 -1 -2 -15 -0.4632 1.21259 15 -2 -2 -15 32.4644 3.09718 15 4 2 15 4.49809 1.72976 15 5 2 15 6.55224 1.68083 15 2 -3 -15 3.24561 1.75488 15 1 -3 -15 0.21169 1.48386 15 0 -3 -15 23.2981 3.21269 15 5 3 15 7.51566 1.73429 15 1 -4 -15 2.81274 1.60032 15 0 -4 -15 4.56910 1.69081 15 -1 -4 -15 0.66330 1.35522 15 -2 -4 -15 -0.8187 1.15165 15 -3 -4 -15 9.43170 1.96482 15 5 4 15 4.08154 1.51388 15 -1 -5 -15 1.59277 1.47239 15 -2 -5 -15 11.8907 2.21785 15 -3 -5 -15 0.54932 1.30441 15 -4 -5 -15 12.5763 2.25224 15 0 0 0 0.00 0.00 0 _chemical_formula_moiety 'C8 H10 K N5 O5' _exptl_crystal_description plate _exptl_crystal_colour 'light yellow' _cell_measurement_reflns_used 31722 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 37.66 _exptl_absorpt_correction_T_min 0.7348 _exptl_absorpt_correction_T_max 0.8806 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ) SADABS-2016/2 (Stalke et al., 2015) Equivalent reflections defined by point group -1 for scaling and error model Mean and maximum errors in direction cosine check function = 0.001 0.003 Restraint esd for equal adjacent scale factors = 0.0090 Maximum odd and even orders for spherical harmonics = 1 4 wR2(int) = 0.1614 (selected reflections only, before parameter refinement) wR2(int) = 0.0532 (selected reflections only, after parameter refinement) 70839 total and 5676 unique reflections assuming Friedel's law plus 2776 total and 1529 unique reflections in fast scans Reflections rejected for which |I-|/su > 3.00 where: su^2 = sigma(I)^2 + ( 0.04000 )^2 (sigma(I) from SAINT) 70457 total and 5676 unique reflections left after |I-|/su test plus 2692 total and 1520 unique reflections in fast scans su^2 = [K*sigma(I)]^2 + [g]^2 where sigma(I) is from SAINT Error model 5: refine all K and overall g Run 2theta R(int) Incid. factors Diffr. factors K g I/s(lim) Total I>2sig(I) 1 21.9 0.0409 0.152 - 0.377 0.991 - 1.040 0.918 0.0262 38.2 4169 3080 2 21.9 0.0348 0.078 - 0.221 0.987 - 1.039 0.911 0.0262 38.2 4140 3301 3 21.9 0.0344 0.103 - 0.142 0.987 - 1.025 0.921 0.0262 38.2 4073 3292 4 21.9 0.0415 0.119 - 0.350 0.987 - 1.035 0.889 0.0262 38.2 4140 3165 5 21.9 0.0404 0.144 - 0.280 0.991 - 1.036 0.943 0.0262 38.2 4164 3145 6 21.9 0.0405 0.099 - 0.336 0.987 - 1.037 0.934 0.0262 38.2 4206 3166 7 21.9 0.0435 0.142 - 0.384 0.987 - 1.038 0.960 0.0262 38.2 4201 3119 8 21.9 0.0359 0.128 - 0.189 0.987 - 1.027 0.933 0.0262 38.2 4114 3234 9 21.9 0.0418 0.148 - 0.349 0.987 - 1.029 0.908 0.0262 38.2 4170 3144 10 21.9 0.0324 0.082 - 0.146 0.987 - 1.035 0.933 0.0262 38.2 4115 3409 11 21.9 0.0424 0.127 - 0.366 0.987 - 1.031 0.923 0.0262 38.2 4135 3117 12 21.9 0.0384 0.102 - 0.313 0.988 - 1.040 0.959 0.0262 38.2 6218 4971 13 21.9 0.0411 0.120 - 0.312 0.987 - 1.040 1.022 0.0262 38.2 6873 5368 14 -21.9 0.0371 0.081 - 0.275 0.987 - 1.040 0.933 0.0262 38.2 4081 3189 15 34.9 0.0288 0.141 - 0.311 0.994 - 1.040 0.891 0.0262 38.2 4493 3782 16 0.0 0.0351 0.189 - 0.268 0.991 - 1.040 1.061 0.0262 38.2 1761 1492 17 0.0 0.0320 0.154 - 0.256 0.987 - 1.026 1.014 0.0262 38.2 1404 1216 18f 0.0 0.0980 1.137 - 2.997 0.989 - 1.034 1.084 0.0262 38.2 2692 1689 2 Overloads replaced by fast scan measurements 70459 Corrected reflections written to file hkl Estimated minimum and maximum transmission: 0.7348 0.8806 The ratio of these values is more reliable than their absolute values! Additional spherical absorption correction applied with mu*r = 0.0800 3lambda correction factor = 0.00150 ) loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -4.00 -1.00 1.00 0.1040 -4.00 1.00 0.00 0.0650 -4.00 0.00 -1.00 0.0610 -3.00 3.00 -2.00 0.1240 -3.00 2.00 -1.00 0.1050 -3.00 0.00 1.00 0.0700 -3.00 -1.00 0.00 0.1060 -3.00 -1.00 4.00 0.1650 -2.00 -3.00 0.00 0.2190 -2.00 3.00 -2.00 0.1450 -2.00 1.00 -1.00 0.0890 -2.00 -1.00 0.00 0.1270 -1.00 0.00 -1.00 0.1090 -1.00 3.00 4.00 0.2350 0.00 0.00 -1.00 0.1460 1.00 0.00 3.00 0.1540 1.00 -3.00 0.00 0.1650 1.00 4.00 -3.00 0.1940 2.00 -1.00 0.00 0.0650 4.00 -1.00 4.00 0.1080 4.00 -1.00 -4.00 0.0880 4.00 1.00 -2.00 0.0880 4.00 -3.00 0.00 0.0860 4.00 0.00 -1.00 0.0430 4.00 1.00 -1.00 0.0790 4.00 2.00 -1.00 0.1180 4.00 -1.00 2.00 0.0780 4.00 -1.00 0.00 0.0410 4.00 0.00 1.00 0.0600 _chemical_absolute_configuration . _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed tube' _diffrn_source_type MoK\a _diffrn_measurement_device 'four-circle diffractometer' _diffrn_radiation_monochromator graphite _diffrn_detector 'CCD plate' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w and \f scans' _computing_data_collection 'APEX4 v2021.10-0 (Bruker AXS)' _computing_cell_refinement 'APEX4 v2021.10-0 (Bruker AXS)' _computing_data_reduction 'APEX4 v2021.10-0 (Bruker AXS)' _computing_structure_solution 'SHELXT-2018/2 (Sheldrick, 2015)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015)' _computing_molecular_graphics ) WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012); PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009) ) _computing_publication_material ) WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012); PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009) ) _refine_special_details ) Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ) CELL 0.71073 8.14040 8.48110 9.28430 86.9918 85.9992 68.7003 ZERR 2.00 0.00030 0.00040 0.00040 0.0011 0.0011 0.0010 LATT 1 ; _shelx_hkl_checksum 74909 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.01504(2) 0.74057(2) 0.92295(2) 0.02027(5) Uani 1 1 d . . . . . O1 O 0.20721(8) 0.93192(8) 1.00907(8) 0.02690(14) Uani 1 1 d . . . . . O2 O -0.22363(11) 0.82845(10) 0.69740(8) 0.03382(16) Uani 1 1 d . . . . . O3 O 0.75014(8) 0.64148(8) 1.03977(7) 0.02239(12) Uani 1 1 d . . . . . O51 O 0.20260(9) 0.58519(9) 0.65040(8) 0.02844(14) Uani 1 1 d . . . . . O52 O 0.43495(10) 0.37529(9) 0.57921(8) 0.02792(14) Uani 1 1 d . . . . . N1 N 0.44878(10) 0.88598(10) 1.13532(8) 0.02281(14) Uani 1 1 d . . . . . N2 N 0.38122(9) 0.67249(8) 0.83731(7) 0.01667(12) Uani 1 1 d . . . . . N3 N 0.74400(9) 0.48895(9) 0.84811(8) 0.02083(13) Uani 1 1 d . . . . . N4 N -0.17815(11) 0.87102(10) 0.45692(9) 0.02701(16) Uani 1 1 d . . . . . N5 N 0.36125(10) 0.50011(9) 0.65394(8) 0.02001(13) Uani 1 1 d . . . . . C1 C 0.36504(10) 0.85386(10) 1.02888(9) 0.01809(13) Uani 1 1 d . . . . . C2 C 0.47301(10) 0.71092(9) 0.93228(8) 0.01597(12) Uani 1 1 d . . . . . C3 C 0.66147(10) 0.61548(10) 0.94438(8) 0.01714(13) Uani 1 1 d . . . . . C4 C 0.64786(11) 0.45651(10) 0.75329(9) 0.02016(14) Uani 1 1 d . . . . . H4 H 0.703109 0.370028 0.685766 0.024 Uiso 1 1 calc R U . . . C5 C 0.46736(10) 0.54642(10) 0.75033(8) 0.01721(13) Uani 1 1 d . . . . . C6 C -0.17378(12) 0.77565(11) 0.57469(10) 0.02434(16) Uani 1 1 d . . . . . H6 H -0.128457 0.656450 0.563998 0.029 Uiso 1 1 calc R U . . . C7 C -0.2507(3) 1.05379(16) 0.46372(16) 0.0652(5) Uani 1 1 d . . . . . H7A H -0.360997 1.097873 0.413456 0.098 Uiso 1 1 calc R U . . . H7B H -0.165872 1.100737 0.417364 0.098 Uiso 1 1 calc R U . . . H7C H -0.274224 1.086505 0.564935 0.098 Uiso 1 1 calc R U . . . C8 C -0.11168(16) 0.79953(17) 0.31676(11) 0.0381(2) Uani 1 1 d . . . . . H8A H -0.011893 0.832368 0.281875 0.057 Uiso 1 1 calc R U . . . H8B H -0.205599 0.842055 0.248437 0.057 Uiso 1 1 calc R U . . . H8C H -0.072578 0.675830 0.325194 0.057 Uiso 1 1 calc R U . . . H1A H 0.559(2) 0.8298(19) 1.1419(16) 0.038(4) Uiso 1 1 d . . . . . H1B H 0.3890(19) 0.9657(19) 1.1923(15) 0.035(4) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.01535(7) 0.02150(8) 0.02307(8) -0.00135(6) -0.00079(5) -0.00555(6) O1 0.0174(3) 0.0229(3) 0.0364(4) -0.0105(3) -0.0043(2) -0.0007(2) O2 0.0446(4) 0.0288(3) 0.0220(3) -0.0024(3) -0.0026(3) -0.0057(3) O3 0.0166(3) 0.0273(3) 0.0238(3) -0.0012(2) -0.0039(2) -0.0081(2) O51 0.0208(3) 0.0297(3) 0.0331(3) -0.0063(3) -0.0078(2) -0.0052(2) O52 0.0316(3) 0.0253(3) 0.0259(3) -0.0100(2) 0.0000(2) -0.0082(3) N1 0.0214(3) 0.0235(3) 0.0226(3) -0.0050(3) -0.0026(2) -0.0062(3) N2 0.0158(3) 0.0162(3) 0.0175(3) 0.0000(2) -0.0009(2) -0.0052(2) N3 0.0152(3) 0.0213(3) 0.0231(3) -0.0015(2) 0.0006(2) -0.0034(2) N4 0.0319(4) 0.0232(3) 0.0213(3) -0.0035(3) -0.0014(3) -0.0041(3) N5 0.0216(3) 0.0199(3) 0.0185(3) -0.0012(2) -0.0018(2) -0.0072(2) C1 0.0175(3) 0.0161(3) 0.0203(3) -0.0010(2) -0.0004(2) -0.0057(2) C2 0.0144(3) 0.0158(3) 0.0174(3) 0.0001(2) -0.0006(2) -0.0051(2) C3 0.0143(3) 0.0182(3) 0.0185(3) 0.0019(2) -0.0003(2) -0.0058(2) C4 0.0179(3) 0.0194(3) 0.0204(3) -0.0023(3) 0.0013(3) -0.0037(3) C5 0.0170(3) 0.0171(3) 0.0170(3) -0.0006(2) -0.0011(2) -0.0056(2) C6 0.0251(4) 0.0194(3) 0.0255(4) -0.0031(3) -0.0052(3) -0.0033(3) C7 0.1096(14) 0.0229(5) 0.0420(7) 0.0044(5) 0.0101(8) -0.0019(7) C8 0.0360(5) 0.0527(7) 0.0243(4) -0.0120(4) 0.0017(4) -0.0137(5) 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' K K 0.2009 0.2494 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 K1 O1 86.02(2) 1_455 2_577 ? O3 K1 O1 136.67(2) 1_455 . ? O1 K1 O1 68.76(2) 2_577 . ? O3 K1 O2 78.04(2) 1_455 . ? O1 K1 O2 77.51(2) 2_577 . ? O1 K1 O2 126.22(2) . . ? O3 K1 N2 151.62(2) 1_455 . ? O1 K1 N2 119.98(2) 2_577 . ? O1 K1 N2 56.162(19) . . ? O2 K1 N2 116.36(2) . . ? O3 K1 O51 118.25(2) 1_455 . ? O1 K1 O51 132.97(2) 2_577 . ? O1 K1 O51 104.48(2) . . ? O2 K1 O51 70.18(2) . . ? N2 K1 O51 53.478(19) . . ? O3 K1 N3 88.22(2) 1_455 2_667 ? O1 K1 N3 119.94(2) 2_577 2_667 ? O1 K1 N3 75.97(2) . 2_667 ? O2 K1 N3 157.25(2) . 2_667 ? N2 K1 N3 69.541(19) . 2_667 ? O51 K1 N3 101.61(2) . 2_667 ? O3 K1 O3 84.442(19) 1_455 2_667 ? O1 K1 O3 160.49(2) 2_577 2_667 ? O1 K1 O3 107.728(18) . 2_667 ? O2 K1 O3 116.85(2) . 2_667 ? N2 K1 O3 67.300(18) . 2_667 ? O51 K1 O3 66.439(19) . 2_667 ? N3 K1 O3 42.843(18) 2_667 2_667 ? O3 K1 C3 20.048(18) 1_455 1_455 ? O1 K1 C3 89.87(2) 2_577 1_455 ? O1 K1 C3 153.37(2) . 1_455 ? O2 K1 C3 59.71(2) . 1_455 ? N2 K1 C3 149.27(2) . 1_455 ? O51 K1 C3 101.73(2) . 1_455 ? N3 K1 C3 103.31(2) 2_667 1_455 ? O3 K1 C3 86.979(18) 2_667 1_455 ? O3 K1 C3 92.781(19) 1_455 2_667 ? O1 K1 C3 143.32(2) 2_577 2_667 ? O1 K1 C3 88.22(2) . 2_667 ? O2 K1 C3 138.05(2) . 2_667 ? N2 K1 C3 59.832(19) . 2_667 ? O51 K1 C3 79.122(19) . 2_667 ? N3 K1 C3 23.532(19) 2_667 2_667 ? O3 K1 C3 21.356(17) 2_667 2_667 ? C3 K1 C3 101.323(17) 1_455 2_667 ? O3 K1 K1 45.745(14) 1_455 2_567 ? O1 K1 K1 129.401(18) 2_577 2_567 ? O1 K1 K1 132.536(17) . 2_567 ? O2 K1 K1 101.240(18) . 2_567 ? N2 K1 K1 105.959(15) . 2_567 ? O51 K1 K1 90.552(16) . 2_567 ? N3 K1 K1 56.825(15) 2_667 2_567 ? O3 K1 K1 38.697(12) 2_667 2_567 ? C3 K1 K1 51.096(13) 1_455 2_567 ? C3 K1 K1 50.228(14) 2_667 2_567 ? O3 K1 K1 113.607(15) 1_455 2_577 ? O1 K1 K1 34.525(14) 2_577 2_577 ? O1 K1 K1 34.236(13) . 2_577 ? O2 K1 K1 103.224(17) . 2_577 ? N2 K1 K1 87.882(15) . 2_577 ? O51 K1 K1 124.297(16) . 2_577 ? N3 K1 K1 98.852(16) 2_667 2_577 ? O3 K1 K1 138.947(13) 2_667 2_577 ? C3 K1 K1 122.832(15) 1_455 2_577 ? C3 K1 K1 117.725(15) 2_667 2_577 ? K1 K1 K1 142.581(9) 2_567 2_577 ? C1 O1 K1 131.46(6) . 2_577 ? C1 O1 K1 116.45(5) . . ? K1 O1 K1 111.24(2) 2_577 . ? C6 O2 K1 120.73(6) . . ? C3 O3 K1 111.93(5) . 1_655 ? C3 O3 K1 93.87(5) . 2_667 ? K1 O3 K1 95.558(19) 1_655 2_667 ? N5 O51 K1 117.53(5) . . ? C1 N1 H1A 119.2(10) . . ? C1 N1 H1B 117.6(10) . . ? H1A N1 H1B 123.2(13) . . ? C2 N2 C5 117.47(7) . . ? C2 N2 K1 115.46(5) . . ? C5 N2 K1 119.95(5) . . ? C4 N3 C3 118.41(7) . . ? C4 N3 K1 131.35(6) . 2_667 ? C3 N3 K1 92.91(5) . 2_667 ? C6 N4 C7 120.54(9) . . ? C6 N4 C8 122.27(9) . . ? C7 N4 C8 117.19(10) . . ? O51 N5 O52 122.94(7) . . ? O51 N5 C5 119.20(7) . . ? O52 N5 C5 117.86(7) . . ? O1 C1 N1 123.44(8) . . ? O1 C1 C2 120.30(7) . . ? N1 C1 C2 116.25(7) . . ? N2 C2 C3 121.54(7) . . ? N2 C2 C1 114.27(7) . . ? C3 C2 C1 124.13(7) . . ? O3 C3 N3 118.84(7) . . ? O3 C3 C2 123.12(7) . . ? N3 C3 C2 118.02(7) . . ? O3 C3 K1 48.02(4) . 1_655 ? N3 C3 K1 91.44(5) . 1_655 ? C2 C3 K1 131.56(5) . 1_655 ? O3 C3 K1 64.78(4) . 2_667 ? N3 C3 K1 63.55(4) . 2_667 ? C2 C3 K1 147.63(5) . 2_667 ? K1 C3 K1 78.677(17) 1_655 2_667 ? N3 C4 C5 121.26(7) . . ? N3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? N2 C5 C4 123.21(7) . . ? N2 C5 N5 116.14(7) . . ? C4 C5 N5 120.59(7) . . ? O2 C6 N4 125.42(9) . . ? O2 C6 H6 117.3 . . ? N4 C6 H6 117.3 . . ? N4 C7 H7A 109.5 . . ? N4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N4 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O3 2.7253(7) 1_455 ? K1 O1 2.7858(7) 2_577 ? K1 O1 2.8063(7) . ? K1 O2 2.8402(8) . ? K1 N2 2.8841(7) . ? K1 O51 2.9698(8) . ? K1 N3 3.0869(7) 2_667 ? K1 O3 3.1221(7) 2_667 ? K1 C3 3.4008(8) 1_455 ? K1 C3 3.4433(8) 2_667 ? K1 K1 4.3385(4) 2_567 ? K1 K1 4.6152(4) 2_577 ? O1 C1 1.2350(10) . ? O2 C6 1.2330(11) . ? O3 C3 1.2567(10) . ? O51 N5 1.2313(10) . ? O52 N5 1.2327(9) . ? N1 C1 1.3313(11) . ? N1 H1A 0.857(15) . ? N1 H1B 0.858(15) . ? N2 C2 1.3195(10) . ? N2 C5 1.3244(10) . ? N3 C4 1.3195(11) . ? N3 C3 1.3766(11) . ? N4 C6 1.3201(12) . ? N4 C7 1.4476(15) . ? N4 C8 1.4491(13) . ? N5 C5 1.4465(10) . ? C1 C2 1.5088(11) . ? C2 C3 1.4607(10) . ? C4 C5 1.3895(11) . ? C4 H4 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? 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 _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N1 H1A O3 0.857(15) 2.004(15) 2.7016(10) 138.0(13) . yes N1 H1B O2 0.858(15) 2.049(15) 2.9000(11) 171.5(14) 2_577 yes 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag K1 O51 N5 O52 146.85(7) . . . . ? K1 O51 N5 C5 -32.69(9) . . . . ? K1 O1 C1 N1 26.97(13) 2_577 . . . ? K1 O1 C1 N1 -141.34(7) . . . . ? K1 O1 C1 C2 -154.50(6) 2_577 . . . ? K1 O1 C1 C2 37.19(10) . . . . ? C5 N2 C2 C3 -1.70(11) . . . . ? K1 N2 C2 C3 148.84(6) . . . . ? C5 N2 C2 C1 -179.06(7) . . . . ? K1 N2 C2 C1 -28.51(8) . . . . ? O1 C1 C2 N2 -4.91(11) . . . . ? N1 C1 C2 N2 173.72(7) . . . . ? O1 C1 C2 C3 177.82(8) . . . . ? N1 C1 C2 C3 -3.55(12) . . . . ? K1 O3 C3 N3 62.81(8) 1_655 . . . ? K1 O3 C3 N3 -34.77(7) 2_667 . . . ? K1 O3 C3 C2 -118.58(7) 1_655 . . . ? K1 O3 C3 C2 143.84(7) 2_667 . . . ? K1 O3 C3 K1 -97.58(3) 2_667 . . 1_655 ? K1 O3 C3 K1 97.58(3) 1_655 . . 2_667 ? C4 N3 C3 O3 176.41(8) . . . . ? K1 N3 C3 O3 35.18(8) 2_667 . . . ? C4 N3 C3 C2 -2.27(11) . . . . ? K1 N3 C3 C2 -143.50(6) 2_667 . . . ? C4 N3 C3 K1 -142.18(7) . . . 1_655 ? K1 N3 C3 K1 76.59(2) 2_667 . . 1_655 ? C4 N3 C3 K1 141.22(8) . . . 2_667 ? N2 C2 C3 O3 -175.15(7) . . . . ? C1 C2 C3 O3 1.93(12) . . . . ? N2 C2 C3 N3 3.47(11) . . . . ? C1 C2 C3 N3 -179.45(7) . . . . ? N2 C2 C3 K1 124.11(7) . . . 1_655 ? C1 C2 C3 K1 -58.80(10) . . . 1_655 ? N2 C2 C3 K1 -80.62(12) . . . 2_667 ? C1 C2 C3 K1 96.46(11) . . . 2_667 ? C3 N3 C4 C5 -0.40(12) . . . . ? K1 N3 C4 C5 123.18(7) 2_667 . . . ? C2 N2 C5 C4 -1.14(12) . . . . ? K1 N2 C5 C4 -150.31(6) . . . . ? C2 N2 C5 N5 176.10(7) . . . . ? K1 N2 C5 N5 26.93(9) . . . . ? N3 C4 C5 N2 2.32(13) . . . . ? N3 C4 C5 N5 -174.81(8) . . . . ? O51 N5 C5 N2 4.88(11) . . . . ? O52 N5 C5 N2 -174.68(7) . . . . ? O51 N5 C5 C4 -177.80(8) . . . . ? O52 N5 C5 C4 2.64(12) . . . . ? K1 O2 C6 N4 -119.48(9) . . . . ? C7 N4 C6 O2 -2.02(19) . . . . ? C8 N4 C6 O2 177.92(10) . . . . ?