#------------------------------------------------------------------------------ #$Date: 2018-02-08 09:56:03 +0200 (Thu, 08 Feb 2018) $ #$Revision: 206297 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/23/2242374.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_2242374 loop_ _publ_author_name 'Naziri, Mir Abolfazl' '\,Sahin, Ertan' 'H\"okelek, Tuncer' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of (E)-4-{[2-(4-hydroxybenzoyl)hydrazin-1-ylidene]methyl}pyridin-1-ium nitrate ; _journal_coeditor_code SU5422 _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 323 _journal_page_last 327 _journal_paper_doi 10.1107/S2056989018002141 _journal_volume 74 _journal_year 2018 _chemical_formula_iupac 'C13 H12 N3 O2 +, N O3 -' _chemical_formula_moiety 'C13 H12 N3 O2 +, N O3 -' _chemical_formula_sum 'C13 H12 N4 O5' _chemical_formula_weight 304.27 _chemical_name_systematic ; (E)-4-{[2-(4-Hydroxybenzoyl)hydrazin-1-ylidene]methyl}pyridin-1-ium nitrate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 95.902(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.335(3) _cell_length_b 13.929(5) _cell_length_c 12.184(4) _cell_measurement_reflns_used 9700 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 3.12 _cell_volume 1407.0(9) _computing_cell_refinement ; SAINT (Bruker, 2012) ; _computing_data_collection ; APEX2 (Bruker, 2012) ; _computing_data_reduction ; SAINT (Bruker, 2012) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae et al., 2008) ; _computing_publication_material ; WinGX (Farrugia, 2012) and PLATON (Spek, 2015) ; _computing_structure_refinement ; SHELXL97 (Sheldrick, 2008) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 44410 _diffrn_reflns_theta_full 28.38 _diffrn_reflns_theta_max 28.38 _diffrn_reflns_theta_min 2.86 _exptl_absorpt_coefficient_mu 0.113 _exptl_absorpt_correction_T_max 0.976 _exptl_absorpt_correction_T_min 0.945 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2012) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 632 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.749 _refine_diff_density_min -0.253 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 211 _refine_ls_number_reflns 3499 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.038 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0486 _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^)+(0.0782P)^2^+0.4149P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1285 _refine_ls_wR_factor_ref 0.1485 _reflns_number_gt 2508 _reflns_number_total 3499 _reflns_threshold_expression I>2\s(I) _iucr_refine_instructions_details ; TITL ertan78_0m_a.res in P2(1)/n CELL 0.71073 8.3355 13.9294 12.1838 90.000 95.902 90.000 ZERR 4.00 0.0025 0.0046 0.0040 0.000 0.010 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 52 48 16 20 MERG 2 OMIT -4.00 180.00 FMAP 2 PLAN 20 ACTA BOND $H CONF LIST 4 L.S. 10 WGHT 0.078200 0.414900 FVAR 0.67590 O2 4 0.823280 0.322877 0.592838 11.00000 0.07972 0.04573 = 0.04513 0.00579 0.03448 0.01200 O1 4 1.156867 0.080551 0.241273 11.00000 0.08050 0.04118 = 0.05799 -0.01315 0.03949 -0.00544 N2 3 0.740514 0.498811 0.518834 11.00000 0.03849 0.03739 = 0.03603 -0.00475 0.01065 0.00263 O3 4 0.331560 0.992981 0.576669 11.00000 0.08838 0.05616 = 0.04519 0.00669 0.02640 0.00926 O4 4 0.373848 0.955696 0.748187 11.00000 0.08374 0.05660 = 0.04005 -0.00063 0.01563 0.01419 N1 3 0.815687 0.434070 0.457376 11.00000 0.04958 0.03869 = 0.03156 -0.00114 0.01448 0.00661 N4 3 0.308325 1.009150 0.672528 11.00000 0.05015 0.03591 = 0.04733 -0.00561 0.01419 -0.00169 N3 3 0.501220 0.801767 0.643408 11.00000 0.04456 0.03301 = 0.04662 -0.00129 0.01322 0.00257 O5 4 0.222049 1.075561 0.698409 11.00000 0.07234 0.05934 = 0.08754 -0.02596 0.00900 0.02168 C9 1 0.628010 0.654467 0.532498 11.00000 0.03459 0.03635 = 0.03338 -0.00090 0.00455 0.00041 C5 1 0.937161 0.279901 0.428999 11.00000 0.03274 0.03694 = 0.03148 -0.00268 0.00800 -0.00046 C7 1 0.855000 0.346128 0.500248 11.00000 0.03593 0.03680 = 0.03429 -0.00179 0.01036 -0.00113 C10 1 0.563307 0.637412 0.631679 11.00000 0.04209 0.03138 = 0.04117 0.00222 0.01129 -0.00283 AFIX 43 H10 2 0.562944 0.575785 0.661017 11.00000 -1.20000 AFIX 0 C6 1 1.008829 0.309700 0.336445 11.00000 0.03550 0.03745 = 0.03395 0.00343 0.00851 0.00177 AFIX 43 H6 2 1.007267 0.374406 0.317557 11.00000 -1.20000 AFIX 0 C8 1 0.703027 0.578934 0.472335 11.00000 0.04965 0.04368 = 0.03326 -0.00046 0.01103 0.00579 AFIX 43 H8 2 0.723628 0.589260 0.399686 11.00000 -1.20000 AFIX 0 C2 1 1.086457 0.148034 0.300314 11.00000 0.04163 0.03979 = 0.03644 -0.00964 0.01343 -0.00501 C1 1 1.082092 0.244597 0.272402 11.00000 0.03790 0.04411 = 0.02959 -0.00012 0.01026 -0.00163 AFIX 43 H1 2 1.128609 0.265466 0.210444 11.00000 -1.20000 AFIX 0 C13 1 0.625654 0.747908 0.491474 11.00000 0.04489 0.04251 = 0.03416 0.00700 0.00956 0.00302 AFIX 43 H13 2 0.667274 0.760958 0.425108 11.00000 -1.20000 AFIX 0 C11 1 0.500365 0.712640 0.685211 11.00000 0.04343 0.03733 = 0.04224 0.00057 0.01537 -0.00298 AFIX 43 H11 2 0.456486 0.701944 0.751299 11.00000 -1.20000 AFIX 0 C4 1 0.943868 0.182655 0.456707 11.00000 0.04998 0.03891 = 0.03728 -0.00044 0.01976 -0.00593 AFIX 43 H4 2 0.897997 0.161649 0.518866 11.00000 -1.20000 AFIX 0 C3 1 1.017342 0.117427 0.393414 11.00000 0.05858 0.03293 = 0.04785 -0.00227 0.02361 -0.00511 AFIX 43 H3 2 1.020803 0.052846 0.412879 11.00000 -1.20000 AFIX 0 C12 1 0.562038 0.820240 0.549034 11.00000 0.05215 0.03500 = 0.04637 0.00881 0.01057 0.00418 AFIX 43 H12 2 0.561279 0.882712 0.522056 11.00000 -1.20000 AFIX 0 H1B 2 0.830412 0.451249 0.392752 11.00000 0.05496 H3A 2 0.456009 0.854836 0.681095 11.00000 0.06900 H1A 2 1.207217 0.110861 0.182699 11.00000 0.08045 HKLF 4 REM ertan78_0m_a.res in P2(1)/n REM R1 = 0.0486 for 2508 Fo > 4sig(Fo) and 0.0738 for all 3499 data REM 211 parameters refined using 0 restraints END WGHT 0.0778 0.4156 REM Highest difference peak 0.749, deepest hole -0.253, 1-sigma level 0.051 Q1 1 1.1969 0.4266 0.1434 11.00000 0.05 0.75 Q2 1 0.4295 1.0211 0.6128 11.00000 0.05 0.21 Q3 1 0.9079 0.3135 0.4625 11.00000 0.05 0.20 Q4 1 0.6031 0.6978 0.5020 11.00000 0.05 0.18 Q5 1 1.0098 0.1375 0.3353 11.00000 0.05 0.18 Q6 1 0.9423 0.2419 0.4426 11.00000 0.05 0.17 Q7 1 0.5912 0.6458 0.5796 11.00000 0.05 0.17 Q8 1 0.9507 0.2937 0.3790 11.00000 0.05 0.16 Q9 1 0.7738 0.6194 0.3868 11.00000 0.05 0.16 Q10 1 0.3218 0.9033 0.7306 11.00000 0.05 0.15 Q11 1 1.0903 0.2799 0.3185 11.00000 0.05 0.14 Q12 1 1.0668 0.4155 0.3370 11.00000 0.05 0.14 Q13 1 0.8299 0.1604 0.5024 11.00000 0.05 0.13 Q14 1 0.6512 0.6174 0.5044 11.00000 0.05 0.13 Q15 1 0.5517 0.6742 0.6593 11.00000 0.05 0.13 Q16 1 0.4996 0.6716 0.6393 11.00000 0.05 0.12 Q17 1 0.7659 0.3216 0.5409 11.00000 0.05 0.12 Q18 1 1.0505 0.1956 0.2733 11.00000 0.05 0.12 Q19 1 0.7249 0.7814 0.4359 11.00000 0.05 0.12 Q20 1 0.7433 0.6514 0.3397 11.00000 0.05 0.12 ; _cod_data_source_file su5422sup1.cif _cod_data_source_block I _cod_original_cell_volume 1407.1(8) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2242374 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 O O1 1.15687(19) 0.08055(9) 0.24127(12) 0.0576(4) Uani d . 1 1 H H1A 1.207(3) 0.1109(18) 0.183(2) 0.080(8) Uiso d . 1 1 O O2 0.82328(18) 0.32288(9) 0.59284(11) 0.0549(4) Uani d . 1 1 O O3 0.3316(2) 0.99298(10) 0.57667(11) 0.0619(4) Uani d . 1 1 O O4 0.37385(19) 0.95570(10) 0.74819(11) 0.0595(4) Uani d . 1 1 O O5 0.22205(19) 1.07556(11) 0.69841(15) 0.0730(5) Uani d . 1 1 N N1 0.81569(17) 0.43407(10) 0.45738(12) 0.0392(3) Uani d . 1 1 H H1B 0.830(3) 0.4512(15) 0.3928(19) 0.055(6) Uiso d . 1 1 N N2 0.74051(16) 0.49881(10) 0.51883(11) 0.0368(3) Uani d . 1 1 N N3 0.50122(17) 0.80177(10) 0.64341(12) 0.0408(3) Uani d . 1 1 H H3A 0.456(3) 0.8548(17) 0.6811(19) 0.069(7) Uiso d . 1 1 N N4 0.30832(18) 1.00915(10) 0.67253(13) 0.0438(4) Uani d . 1 1 C C1 1.08209(19) 0.24460(12) 0.27240(13) 0.0367(4) Uani d . 1 1 H H1 1.1286 0.2655 0.2104 0.044 Uiso calc R 1 1 C C2 1.0865(2) 0.14803(12) 0.30031(14) 0.0386(4) Uani d . 1 1 C C3 1.0173(2) 0.11743(13) 0.39341(15) 0.0452(4) Uani d . 1 1 H H3 1.0208 0.0528 0.4129 0.054 Uiso calc R 1 1 C C4 0.9439(2) 0.18265(12) 0.45671(14) 0.0410(4) Uani d . 1 1 H H4 0.8980 0.1616 0.5189 0.049 Uiso calc R 1 1 C C5 0.93716(18) 0.27990(11) 0.42900(13) 0.0334(3) Uani d . 1 1 C C6 1.00883(18) 0.30970(12) 0.33645(13) 0.0353(4) Uani d . 1 1 H H6 1.0073 0.3744 0.3176 0.042 Uiso calc R 1 1 C C7 0.85500(18) 0.34613(11) 0.50025(13) 0.0352(3) Uani d . 1 1 C C8 0.7030(2) 0.57893(12) 0.47233(14) 0.0417(4) Uani d . 1 1 H H8 0.7236 0.5893 0.3997 0.050 Uiso calc R 1 1 C C9 0.62801(18) 0.65447(11) 0.53250(13) 0.0347(3) Uani d . 1 1 C C10 0.56331(19) 0.63741(12) 0.63168(14) 0.0377(4) Uani d . 1 1 H H10 0.5629 0.5758 0.6610 0.045 Uiso calc R 1 1 C C11 0.5004(2) 0.71264(12) 0.68521(15) 0.0402(4) Uani d . 1 1 H H11 0.4565 0.7019 0.7513 0.048 Uiso calc R 1 1 C C12 0.5620(2) 0.82024(12) 0.54903(15) 0.0441(4) Uani d . 1 1 H H12 0.5613 0.8827 0.5221 0.053 Uiso calc R 1 1 C C13 0.6257(2) 0.74791(12) 0.49147(14) 0.0401(4) Uani d . 1 1 H H13 0.6673 0.7610 0.4251 0.048 Uiso calc R 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 O1 0.0805(10) 0.0412(7) 0.0580(9) -0.0054(6) 0.0395(8) -0.0132(6) O2 0.0797(10) 0.0457(7) 0.0451(7) 0.0120(6) 0.0345(7) 0.0058(6) O3 0.0884(11) 0.0562(9) 0.0452(8) 0.0093(7) 0.0264(7) 0.0067(6) O4 0.0837(10) 0.0566(8) 0.0401(7) 0.0142(7) 0.0156(7) -0.0006(6) O5 0.0723(10) 0.0593(9) 0.0875(12) 0.0217(8) 0.0090(9) -0.0260(8) N1 0.0496(8) 0.0387(8) 0.0316(7) 0.0066(6) 0.0145(6) -0.0011(6) N2 0.0385(7) 0.0374(7) 0.0360(7) 0.0026(5) 0.0107(6) -0.0047(6) N3 0.0446(8) 0.0330(7) 0.0466(8) 0.0026(6) 0.0132(6) -0.0013(6) N4 0.0502(8) 0.0359(7) 0.0473(9) -0.0017(6) 0.0142(7) -0.0056(6) C1 0.0379(8) 0.0441(9) 0.0296(8) -0.0016(7) 0.0103(6) -0.0001(7) C2 0.0416(8) 0.0398(9) 0.0364(8) -0.0050(7) 0.0134(7) -0.0096(7) C3 0.0586(11) 0.0329(9) 0.0479(10) -0.0051(7) 0.0236(8) -0.0023(7) C4 0.0500(9) 0.0389(9) 0.0373(9) -0.0059(7) 0.0198(7) -0.0004(7) C5 0.0327(7) 0.0369(8) 0.0315(8) -0.0005(6) 0.0080(6) -0.0027(6) C6 0.0355(8) 0.0375(8) 0.0340(8) 0.0018(6) 0.0085(6) 0.0034(6) C7 0.0359(8) 0.0368(8) 0.0343(8) -0.0011(6) 0.0104(6) -0.0018(6) C8 0.0496(9) 0.0437(9) 0.0333(8) 0.0058(8) 0.0110(7) -0.0005(7) C9 0.0346(8) 0.0363(8) 0.0334(8) 0.0004(6) 0.0046(6) -0.0009(6) C10 0.0421(8) 0.0314(8) 0.0412(9) -0.0028(6) 0.0113(7) 0.0022(7) C11 0.0434(9) 0.0373(9) 0.0422(9) -0.0030(7) 0.0154(7) 0.0006(7) C12 0.0522(10) 0.0350(9) 0.0464(10) 0.0042(7) 0.0106(8) 0.0088(7) C13 0.0449(9) 0.0425(9) 0.0342(8) 0.0030(7) 0.0096(7) 0.0070(7) 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 C2 O1 H1A 109.6(15) N2 N1 H1B 116.3(15) C7 N1 N2 119.41(14) C7 N1 H1B 124.2(15) C8 N2 N1 116.08(14) C11 N3 H3A 120.6(14) C12 N3 C11 121.66(15) C12 N3 H3A 117.7(14) O3 N4 O4 119.23(15) O3 N4 O5 122.40(17) O5 N4 O4 118.37(16) C2 C1 H1 120.0 C6 C1 C2 120.06(14) C6 C1 H1 120.0 O1 C2 C1 123.03(15) O1 C2 C3 117.33(16) C1 C2 C3 119.64(15) C2 C3 H3 120.0 C4 C3 C2 120.02(16) C4 C3 H3 120.0 C3 C4 C5 120.96(15) C3 C4 H4 119.5 C5 C4 H4 119.5 C4 C5 C7 118.16(14) C6 C5 C4 118.38(14) C6 C5 C7 123.46(15) C1 C6 C5 120.92(15) C1 C6 H6 119.5 C5 C6 H6 119.5 O2 C7 N1 121.65(15) O2 C7 C5 122.00(15) N1 C7 C5 116.35(14) N2 C8 C9 120.38(15) N2 C8 H8 119.8 C9 C8 H8 119.8 C10 C9 C8 122.46(15) C10 C9 C13 118.54(14) C13 C9 C8 118.96(15) C9 C10 H10 120.5 C11 C10 C9 119.00(15) C11 C10 H10 120.5 N3 C11 C10 120.71(16) N3 C11 H11 119.6 C10 C11 H11 119.6 N3 C12 C13 120.30(16) N3 C12 H12 119.9 C13 C12 H12 119.9 C9 C13 H13 120.1 C12 C13 C9 119.79(15) C12 C13 H13 120.1 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C2 1.354(2) O1 H1A 0.96(3) O2 C7 1.228(2) O3 N4 1.224(2) O4 N4 1.264(2) N1 C7 1.359(2) N1 H1B 0.84(2) N2 N1 1.3649(19) N2 C8 1.276(2) N3 C11 1.342(2) N3 C12 1.329(2) N3 H3A 0.97(2) N4 O5 1.2325(19) C1 H1 0.9300 C2 C1 1.387(2) C2 C3 1.391(2) C3 H3 0.9300 C4 C3 1.376(2) C4 H4 0.9300 C5 C4 1.396(2) C5 C6 1.393(2) C5 C7 1.482(2) C6 C1 1.379(2) C6 H6 0.9300 C8 H8 0.9300 C9 C8 1.459(2) C9 C10 1.393(2) C9 C13 1.394(2) C10 C11 1.367(2) C10 H10 0.9300 C11 H11 0.9300 C12 H12 0.9300 C13 C12 1.366(2) C13 H13 0.9300 loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 _geom_contact_publ_flag O1 H10 2.48 4_665 yes O2 H1 2.58 4_566 yes O2 H1A 1.79(2) 4_566 yes O2 H4 2.52 . yes O3 H3A 2.48(2) . yes O3 H12 2.59 . yes O4 H3A 1.80(2) . yes N1 H6 2.59 . yes N2 H1A 2.56(2) 4_566 yes N2 H10 2.62 . yes N4 H3A 2.47(2) . yes C6 H1B 2.61(2) . yes C7 H1A 2.72(2) 4_566 yes H1 H1A 2.28 . yes H1B O4 2.25(2) 4_675 yes H1B O5 2.47(2) 4_675 yes H1B N4 2.73(2) 4_675 yes H6 O4 2.71 4_675 yes H6 O5 2.75 4_675 yes H6 N4 2.81 4_675 yes H6 H1B 2.11 . yes H8 O4 2.42 4_675 yes H8 H1B 2.12 . yes H8 H13 2.46 . yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1A O2 4_665 0.96(2) 1.79(2) 2.742(2) 170(2) yes N1 H1B O4 4_675 0.84(2) 2.25(2) 3.057(2) 161(2) yes N1 H1B O5 4_675 0.84(2) 2.47(2) 3.174(3) 141(2) yes N3 H3A O4 . 0.97(2) 1.80(2) 2.763(2) 178(2) yes C1 H1 O2 4_665 0.93 2.58 3.258(2) 130 yes C8 H8 O4 4_675 0.93 2.42 3.243(2) 148 yes C10 H10 O1 4_566 0.93 2.48 3.375(2) 162 yes C11 H11 O5 2_546 0.93 2.42 3.104(3) 130 yes C12 H12 O3 3_676 0.93 2.34 3.191(2) 152 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 N2 N1 C7 O2 0.7(2) N2 N1 C7 C5 -179.66(13) C8 N2 N1 C7 -178.09(15) N1 N2 C8 C9 -177.58(14) C12 N3 C11 C10 0.3(3) C11 N3 C12 C13 0.1(3) O1 C2 C1 C6 -179.76(15) C3 C2 C1 C6 -0.3(3) O1 C2 C3 C4 -179.94(17) C1 C2 C3 C4 0.6(3) C5 C4 C3 C2 0.0(3) C6 C5 C4 C3 -0.9(3) C7 C5 C4 C3 179.50(16) C4 C5 C6 C1 1.2(2) C7 C5 C6 C1 -179.26(15) C4 C5 C7 O2 15.3(2) C4 C5 C7 N1 -164.34(15) C6 C5 C7 O2 -164.23(16) C6 C5 C7 N1 16.1(2) C5 C6 C1 C2 -0.6(2) C10 C9 C8 N2 -13.9(3) C13 C9 C8 N2 163.87(16) C8 C9 C10 C11 177.61(16) C13 C9 C10 C11 -0.1(2) C8 C9 C13 C12 -177.27(16) C10 C9 C13 C12 0.6(2) C9 C10 C11 N3 -0.3(3) C9 C13 C12 N3 -0.6(3) _cod_database_fobs_code 2242374