#------------------------------------------------------------------------------ #$Date: 2013-10-25 10:29:26 +0300 (Fri, 25 Oct 2013) $ #$Revision: 89416 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/91/2019147.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_2019147 loop_ _publ_author_name 'Rychkov, Denis' 'Boldyreva, Elena V.' 'Tumanov, Nikolay A.' _publ_section_title ; A new structure of a serotonin salt: comparison and conformational analysis of all known serotonin complexes ; _journal_coeditor_code YF3040 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1055 _journal_page_last 1061 _journal_paper_doi 10.1107/S0108270113019823 _journal_volume 69 _journal_year 2013 _chemical_formula_iupac 'C10 H13 N2 O + , C6 H9 O4 -' _chemical_formula_moiety 'C10 H13 N2 O +, C6 H9 O4 -' _chemical_formula_sum 'C16 H22 N2 O5' _chemical_formula_weight 322.36 _chemical_name_common 'Serotonin adipate' _chemical_name_systematic ; 2-(5-Hydroxy-1H-indol-3-yl)ethanaminium 3-carboxypropanoate ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 113.202(6) _cell_angle_beta 101.233(4) _cell_angle_gamma 98.045(4) _cell_formula_units_Z 2 _cell_length_a 7.1582(3) _cell_length_b 10.5984(7) _cell_length_c 12.1715(7) _cell_measurement_reflns_used 2039 _cell_measurement_temperature 298 _cell_measurement_theta_max 26.3219 _cell_measurement_theta_min 1.8894 _cell_volume 808.05(9) _computing_cell_refinement 'CrysAlis PRO (Oxford Diffraction, 2008)' _computing_data_collection 'CrysAlis PRO (Oxford Diffraction, 2008)' _computing_data_reduction 'CrysAlis PRO (Oxford Diffraction, 2008)' _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009), Mercury (Macrae et al., 2008), PLATON (Spek, 2009) and CrystalExplorer (McKinnon et al., 1998; Spackman & McKinnon, 2002) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009), enCIFer (Allen et al., 2004) and publCIF (Westrip, 2010) ; _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 298 _diffrn_detector_area_resol_mean 10.3457 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Oxford Gemini Ultra R' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 10092 _diffrn_reflns_theta_full 26.38 _diffrn_reflns_theta_max 26.38 _diffrn_reflns_theta_min 1.89 _exptl_absorpt_coefficient_mu 0.099 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.99359 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(CrysAlis PRO; Oxford Diffraction, 2008)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 344 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.160 _refine_diff_density_min -0.197 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 296 _refine_ls_number_reflns 3286 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.995 _refine_ls_R_factor_all 0.1080 _refine_ls_R_factor_gt 0.0514 _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^)+(0.0429P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0968 _refine_ls_wR_factor_ref 0.1205 _reflns_number_gt 1849 _reflns_number_total 3286 _reflns_threshold_expression I>2\s(I) _iucr_refine_instructions_details ; TITL AdiSer_str_0.8a in P-1 #2 CELL 0.71073 7.158165 10.598371 12.171485 113.2021 101.233 98.0454 ZERR 2 0.000293 0.000665 0.000706 0.0057 0.0041 0.0042 LATT 1 SFAC C H N O UNIT 32 44 4 10 EQIV $1 +X,1+Y,+Z EQIV $2 -X,-Y,1-Z EQIV $3 +X,-1+Y,+Z EQIV $4 +X,+Y,1+Z L.S. 10 0 0 511 PLAN 20 TEMP 24.85 HTAB O1 O4_$1 HTAB N1 O3_$2 HTAB N1 O5_$3 HTAB O5 O2_$4 fmap 2 acta REM D:/02-Denis/OLEX2_Structure/AdiSer_str_0.8a.hkl WGHT 0.042900 FVAR 2.16557 N1 3 0.246796 -0.130525 0.798672 11.00000 0.06989 0.03819 = 0.05612 0.02244 0.02418 0.01985 N2 3 0.258062 0.076404 0.424983 11.00000 0.06950 0.05949 = 0.04221 0.02126 0.01881 0.01338 O1 4 0.234598 0.812136 0.166694 11.00000 0.08244 0.03789 = 0.06198 0.02961 0.03367 0.02448 O2 4 0.304967 0.654192 0.007953 11.00000 0.11895 0.05111 = 0.06526 0.03400 0.05265 0.03329 O3 4 0.119585 0.089109 0.180573 11.00000 0.07021 0.04489 = 0.05706 0.02936 0.03274 0.02167 O4 4 0.323486 -0.010228 0.079003 11.00000 0.06430 0.04261 = 0.07172 0.03519 0.03361 0.02509 O5 4 0.244754 0.595387 0.769511 11.00000 0.11392 0.04941 = 0.05893 0.02928 0.02897 0.02870 C1 1 0.259154 0.686279 0.104845 11.00000 0.04726 0.03496 = 0.04687 0.01985 0.01680 0.01261 C2 1 0.230718 0.586797 0.162728 11.00000 0.05284 0.03773 = 0.05108 0.02419 0.01826 0.01542 C3 1 0.251492 0.440432 0.085233 11.00000 0.05439 0.03452 = 0.05033 0.02295 0.01604 0.01259 C4 1 0.229009 0.339497 0.144199 11.00000 0.05901 0.03591 = 0.05515 0.02639 0.02183 0.01569 C5 1 0.249762 0.194010 0.061639 11.00000 0.05990 0.03537 = 0.04748 0.02254 0.01991 0.01368 C6 1 0.228768 0.084940 0.111760 11.00000 0.04513 0.03130 = 0.04226 0.01858 0.01031 0.00668 C7 1 0.261772 -0.101719 0.690504 11.00000 0.05652 0.04754 = 0.05023 0.02501 0.02066 0.01539 C8 1 0.253284 0.049150 0.718835 11.00000 0.05710 0.04125 = 0.04701 0.01992 0.01524 0.01093 C9 1 0.257780 0.085693 0.612898 11.00000 0.04477 0.04403 = 0.04500 0.02199 0.01471 0.01252 C10 1 0.255229 0.222000 0.617305 11.00000 0.04346 0.04719 = 0.04227 0.02319 0.01308 0.00993 C11 1 0.250788 0.351090 0.710749 11.00000 0.05416 0.04664 = 0.04255 0.02352 0.01803 0.01481 C12 1 0.247581 0.464253 0.682852 11.00000 0.06349 0.04418 = 0.05021 0.02131 0.01510 0.01366 C13 1 0.248233 0.453679 0.564578 11.00000 0.08405 0.05577 = 0.05649 0.03584 0.01743 0.01518 C14 1 0.253366 0.328963 0.472363 11.00000 0.08039 0.06421 = 0.04598 0.03280 0.01684 0.01014 C15 1 0.254724 0.213121 0.498524 11.00000 0.05059 0.04934 = 0.04226 0.02027 0.01302 0.01033 C16 1 0.257170 -0.000042 0.494308 11.00000 0.05826 0.04744 = 0.04940 0.01797 0.01613 0.01174 H1 2 0.261194 0.878707 0.124488 11.00000 0.07979 H1A 2 0.123438 -0.117177 0.821332 11.00000 0.09401 H1B 2 0.249257 -0.232011 0.774966 11.00000 0.06963 H1C 2 0.337250 -0.072451 0.870843 11.00000 0.09874 H2 2 0.236397 0.039784 0.342463 11.00000 0.10094 H2A 2 0.324535 0.631307 0.245156 11.00000 0.05027 H2B 2 0.100918 0.584354 0.180808 11.00000 0.07067 H3A 2 0.156277 0.399801 0.003055 11.00000 0.05116 H3B 2 0.375302 0.448016 0.068890 11.00000 0.05961 H4A 2 0.101333 0.331797 0.161831 11.00000 0.06004 H4B 2 0.328069 0.379803 0.225479 11.00000 0.07020 H5 2 0.254370 0.598039 0.840669 11.00000 0.08817 H5A 2 0.143380 0.154358 -0.020510 11.00000 0.05866 H5B 2 0.370289 0.203601 0.043811 11.00000 0.06720 H7A 2 0.145202 -0.172222 0.618187 11.00000 0.05415 H7B 2 0.382000 -0.123069 0.674930 11.00000 0.05623 H8A 2 0.128528 0.064231 0.747629 11.00000 0.06852 H8B 2 0.358619 0.111786 0.791163 11.00000 0.05612 H11 2 0.250489 0.359811 0.794491 11.00000 0.05103 H13 2 0.237581 0.539523 0.548100 11.00000 0.06687 H14 2 0.248725 0.320807 0.394845 11.00000 0.06180 H16 2 0.252350 -0.103780 0.453426 11.00000 0.06940 HKLF 4 REM AdiSer_str_0.8a in P-1 #2 REM R1 = 0.0514 for 1849 Fo > 4sig(Fo) and 0.1080 for all 3286 data REM 296 parameters refined using 0 restraints END WGHT 0.0434 0.0000 REM Highest difference peak 0.160, deepest hole -0.197, 1-sigma level 0.044 Q1 1 0.0803 0.5379 0.3808 11.00000 0.05 0.16 Q2 1 0.4424 0.1442 0.7975 11.00000 0.05 0.16 Q3 1 0.0568 0.4133 0.6286 11.00000 0.05 0.16 Q4 1 0.1637 0.6381 0.0036 11.00000 0.05 0.15 Q5 1 0.0275 0.4868 0.2604 11.00000 0.05 0.15 Q6 1 0.4995 0.2372 0.0681 11.00000 0.05 0.15 Q7 1 0.0663 0.2553 0.7592 11.00000 0.05 0.14 Q8 1 0.4501 0.4183 0.0248 11.00000 0.05 0.13 Q9 1 0.0913 0.3432 -0.1016 11.00000 0.05 0.13 Q10 1 0.0779 -0.0014 0.1800 11.00000 0.05 0.13 Q11 1 0.3956 0.8403 0.0602 11.00000 0.05 0.13 Q12 1 0.4187 0.2518 0.3283 11.00000 0.05 0.13 Q13 1 0.0068 0.5428 0.1246 11.00000 0.05 0.13 Q14 1 0.4707 -0.2172 0.6359 11.00000 0.05 0.13 Q15 1 0.4753 0.3241 0.1796 11.00000 0.05 0.13 Q16 1 0.0000 0.5000 0.5000 10.50000 0.05 0.13 Q17 1 0.3646 0.5550 0.5593 11.00000 0.05 0.12 Q18 1 0.0956 0.3156 0.3533 11.00000 0.05 0.12 Q19 1 0.6107 0.1868 0.0397 11.00000 0.05 0.12 Q20 1 0.0640 0.1971 0.2614 11.00000 0.05 0.12 ; _[local]_cod_data_source_file yf3040.cif _[local]_cod_data_source_block I _cod_original_cell_volume 808.04(8) _cod_database_code 2019147 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -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 _atom_site_symmetry_multiplicity N N1 0.2468(4) -0.1305(3) 0.7987(2) 0.0523(6) Uani d 1 1 N N2 0.2581(3) 0.0764(2) 0.4250(2) 0.0570(6) Uani d 1 1 O O1 0.2346(2) 0.81214(18) 0.16669(15) 0.0549(5) Uani d 1 1 O O2 0.3050(3) 0.65419(18) 0.00795(17) 0.0699(5) Uani d 1 1 O O3 0.1196(2) 0.08911(16) 0.18057(15) 0.0518(4) Uani d 1 1 O O4 0.3235(2) -0.01023(16) 0.07900(15) 0.0524(4) Uani d 1 1 O O5 0.2448(3) 0.5954(2) 0.7695(2) 0.0704(6) Uani d 1 1 C C1 0.2592(3) 0.6863(2) 0.1048(2) 0.0414(5) Uani d 1 1 C C2 0.2307(4) 0.5868(2) 0.1627(2) 0.0445(6) Uani d 1 1 C C3 0.2515(4) 0.4404(2) 0.0852(2) 0.0444(6) Uani d 1 1 C C4 0.2290(4) 0.3395(2) 0.1442(2) 0.0464(6) Uani d 1 1 C C5 0.2498(4) 0.1940(2) 0.0616(2) 0.0450(6) Uani d 1 1 C C6 0.2288(3) 0.0849(2) 0.1118(2) 0.0392(5) Uani d 1 1 C C7 0.2618(4) -0.1017(3) 0.6905(2) 0.0489(6) Uani d 1 1 C C8 0.2533(4) 0.0492(3) 0.7188(2) 0.0481(6) Uani d 1 1 C C9 0.2578(3) 0.0857(2) 0.6129(2) 0.0431(6) Uani d 1 1 C C10 0.2552(3) 0.2220(2) 0.6173(2) 0.0429(6) Uani d 1 1 C C11 0.2508(3) 0.3511(3) 0.7107(2) 0.0454(6) Uani d 1 1 C C12 0.2476(3) 0.4643(3) 0.6829(2) 0.0523(6) Uani d 1 1 C C13 0.2482(4) 0.4537(3) 0.5646(3) 0.0621(7) Uani d 1 1 C C14 0.2534(4) 0.3290(3) 0.4724(3) 0.0614(7) Uani d 1 1 C C15 0.2547(3) 0.2131(3) 0.4985(2) 0.0474(6) Uani d 1 1 C C16 0.2572(3) 0.0000(3) 0.4943(2) 0.0526(6) Uani d 1 1 H H1 0.261(3) 0.879(3) 0.124(2) 0.080(8) Uiso d 1 1 H H1A 0.123(4) -0.117(3) 0.821(3) 0.094(10) Uiso d 1 1 H H1B 0.249(3) -0.232(3) 0.775(2) 0.070(8) Uiso d 1 1 H H1C 0.337(4) -0.072(3) 0.871(3) 0.099(11) Uiso d 1 1 H H2 0.236(4) 0.040(3) 0.342(3) 0.101(11) Uiso d 1 1 H H2A 0.325(3) 0.631(2) 0.245(2) 0.050(6) Uiso d 1 1 H H2B 0.101(3) 0.584(2) 0.181(2) 0.071(8) Uiso d 1 1 H H3A 0.156(3) 0.400(2) 0.003(2) 0.051(6) Uiso d 1 1 H H3B 0.375(3) 0.448(2) 0.069(2) 0.060(7) Uiso d 1 1 H H4A 0.101(3) 0.332(2) 0.162(2) 0.060(7) Uiso d 1 1 H H4B 0.328(3) 0.380(2) 0.225(2) 0.070(8) Uiso d 1 1 H H5 0.254(4) 0.598(3) 0.841(3) 0.088(11) Uiso d 1 1 H H5A 0.143(3) 0.154(2) -0.021(2) 0.059(7) Uiso d 1 1 H H5B 0.370(3) 0.204(2) 0.044(2) 0.067(8) Uiso d 1 1 H H7A 0.145(3) -0.172(2) 0.618(2) 0.054(6) Uiso d 1 1 H H7B 0.382(3) -0.123(2) 0.675(2) 0.056(7) Uiso d 1 1 H H8A 0.129(3) 0.064(2) 0.748(2) 0.069(7) Uiso d 1 1 H H8B 0.359(3) 0.112(2) 0.791(2) 0.056(7) Uiso d 1 1 H H11 0.250(3) 0.360(2) 0.794(2) 0.051(6) Uiso d 1 1 H H14 0.249(3) 0.321(2) 0.395(2) 0.062(7) Uiso d 1 1 H H13 0.238(3) 0.540(3) 0.548(2) 0.067(7) Uiso d 1 1 H H16 0.252(3) -0.104(3) 0.453(2) 0.069(8) Uiso d 1 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 0.0699(16) 0.0382(14) 0.0561(15) 0.0199(11) 0.0242(13) 0.0224(12) N2 0.0695(13) 0.0595(16) 0.0422(13) 0.0134(10) 0.0188(11) 0.0213(12) O1 0.0824(11) 0.0379(11) 0.0620(11) 0.0245(8) 0.0337(9) 0.0296(9) O2 0.1189(14) 0.0511(12) 0.0653(12) 0.0333(10) 0.0526(11) 0.0340(10) O3 0.0702(10) 0.0449(10) 0.0571(10) 0.0217(8) 0.0327(9) 0.0294(8) O4 0.0643(9) 0.0426(10) 0.0717(11) 0.0251(8) 0.0336(8) 0.0352(9) O5 0.1139(15) 0.0494(13) 0.0589(13) 0.0287(10) 0.0290(11) 0.0293(11) C1 0.0473(12) 0.0350(14) 0.0469(14) 0.0126(10) 0.0168(11) 0.0198(12) C2 0.0528(15) 0.0377(14) 0.0511(15) 0.0154(11) 0.0183(13) 0.0242(12) C3 0.0544(15) 0.0345(14) 0.0503(15) 0.0126(11) 0.0160(13) 0.0229(12) C4 0.0590(16) 0.0359(14) 0.0552(16) 0.0157(11) 0.0218(14) 0.0264(12) C5 0.0599(16) 0.0354(14) 0.0475(15) 0.0137(11) 0.0199(14) 0.0225(12) C6 0.0451(12) 0.0313(13) 0.0423(13) 0.0067(10) 0.0103(11) 0.0186(11) C7 0.0565(16) 0.0475(16) 0.0502(15) 0.0154(12) 0.0207(13) 0.0250(13) C8 0.0571(16) 0.0412(15) 0.0470(15) 0.0109(12) 0.0152(13) 0.0199(12) C9 0.0448(12) 0.0440(15) 0.0450(14) 0.0125(10) 0.0147(10) 0.0220(12) C10 0.0435(12) 0.0472(15) 0.0423(13) 0.0099(10) 0.0131(10) 0.0232(12) C11 0.0542(14) 0.0466(16) 0.0425(14) 0.0148(10) 0.0180(11) 0.0235(13) C12 0.0635(15) 0.0442(17) 0.0502(15) 0.0137(11) 0.0151(12) 0.0213(13) C13 0.0840(18) 0.0558(19) 0.0565(17) 0.0152(14) 0.0174(14) 0.0358(16) C14 0.0804(18) 0.064(2) 0.0460(16) 0.0101(13) 0.0168(14) 0.0328(16) C15 0.0506(13) 0.0493(16) 0.0423(14) 0.0103(10) 0.0130(11) 0.0203(13) C16 0.0583(15) 0.0474(18) 0.0494(16) 0.0117(11) 0.0161(12) 0.0180(14) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N1 C7 C8 110.1(2) N1 C7 H7A 105.7(12) N1 C7 H7B 105.1(13) N2 C15 C10 107.3(2) N2 C15 C14 130.9(2) N2 C16 H16 119.2(15) O1 C1 C2 115.3(2) O2 C1 O1 121.8(2) O2 C1 C2 122.9(2) O3 C6 O4 122.7(2) O3 C6 C5 120.0(2) O4 C6 C5 117.3(2) O5 C12 C13 116.0(2) C1 O1 H1 112.4(14) C1 C2 C3 113.5(2) C1 C2 H2A 106.7(12) C1 C2 H2B 108.4(13) C2 C3 C4 114.2(2) C2 C3 H3A 109.8(12) C2 C3 H3B 108.9(14) C3 C2 H2A 112.2(12) C3 C2 H2B 111.8(14) C3 C4 C5 111.8(2) C3 C4 H4A 109.7(13) C3 C4 H4B 108.9(14) C4 C3 H3A 109.5(12) C4 C3 H3B 109.4(14) C4 C5 H5A 108.4(12) C4 C5 H5B 108.8(15) C5 C4 H4A 110.0(13) C5 C4 H4B 110.4(13) C6 C5 C4 116.0(2) C6 C5 H5A 106.4(12) C6 C5 H5B 109.5(15) C7 N1 H1A 112.9(16) C7 N1 H1B 107.4(14) C7 N1 H1C 115(2) C7 C8 H8A 106.9(13) C7 C8 H8B 108.9(13) C8 C7 H7A 111.4(11) C8 C7 H7B 113.9(13) C9 C8 C7 113.9(2) C9 C8 H8A 111.8(13) C9 C8 H8B 110.9(14) C9 C16 N2 109.9(2) C9 C16 H16 130.8(15) C10 C9 C8 124.5(2) C10 C11 H11 120.5(12) C11 C10 C15 119.0(2) C11 C10 C9 133.4(2) C11 C12 O5 122.2(2) C11 C12 C13 121.8(2) C12 O5 H5 112(2) C12 C11 C10 118.4(2) C12 C11 H11 121.1(12) C12 C13 H13 118.1(14) C13 C14 C15 118.3(3) C13 C14 H14 120.9(15) C14 C15 C10 121.8(2) C14 C13 C12 120.7(3) C14 C13 H13 121.1(14) C15 N2 C16 108.7(2) C15 N2 H2 124(2) C15 C10 C9 107.5(2) C15 C14 H14 120.7(16) C16 N2 H2 126(2) C16 C9 C10 106.5(2) C16 C9 C8 128.9(2) H1A N1 H1B 108(2) H1A N1 H1C 102(3) H1B N1 H1C 112(2) H2A C2 H2B 103.7(19) H3A C3 H3B 104.6(19) H4A C4 H4B 106(2) H5A C5 H5B 107(2) H7A C7 H7B 110.1(18) H8A C8 H8B 103.9(19) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C7 1.483(3) N1 H1A 0.99(3) N1 H1B 1.00(3) N1 H1C 0.90(3) N2 C16 1.381(3) N2 H2 0.89(3) O1 H1 1.04(3) O3 C6 1.245(2) O4 C6 1.271(2) O5 H5 0.84(3) O5 C12 1.380(3) C1 O1 1.305(3) C1 O2 1.217(3) C1 C2 1.493(3) C2 C3 1.511(3) C2 H2A 0.98(2) C2 H2B 1.00(2) C3 H3A 0.98(2) C3 H3B 0.94(2) C4 C3 1.512(3) C4 C5 1.520(3) C4 H4A 0.98(2) C4 H4B 0.99(2) C5 H5A 1.02(2) C5 H5B 0.93(2) C6 C5 1.508(3) C7 H7A 1.02(2) C7 H7B 0.95(2) C8 C7 1.510(3) C8 C9 1.490(3) C8 H8A 1.03(2) C8 H8B 0.96(2) C9 C16 1.368(3) C10 C9 1.427(3) C10 C11 1.402(3) C11 C12 1.371(3) C11 H11 0.99(2) C12 C13 1.400(3) C13 C14 1.367(4) C13 H13 1.02(2) C14 H14 0.91(2) C15 N2 1.377(3) C15 C10 1.411(3) C15 C14 1.385(3) C16 H16 1.00(3) 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 O1 H1 O4 1_565 1.04(3) 1.53(3) 2.569(2) 172(2) N1 H1A O3 2_556 0.99(3) 1.80(3) 2.762(3) 163(2) N1 H1B O5 1_545 1.00(3) 1.80(3) 2.782(3) 166(2) O5 H5 O2 1_556 0.84(3) 1.82(3) 2.647(3) 164(3) _cod_database_fobs_code 2019147