#------------------------------------------------------------------------------ #$Date: 2025-05-03 21:21:32 +0200 (Sat, 03 May 2025) $ #$Revision: 299526 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/34/2023446.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_2023446 loop_ _publ_author_name 'Shikhaliyev, Namiq Q.' 'Babazade, Aliyar A.' 'Atakishiyeva, Gulnar T.' 'Shikhaliyeva, Irada M.' 'Maharramov, Abel M.' 'Khrustalev, Victor N.' 'Atioğlu, Zeliha' 'Akkurt, Mehmet' 'Bhattarai, Ajaya' _publ_section_title ; Crystal structures and Hirshfeld surface analyses of methyl (2Z)-(4-bromo-phen-yl)[2-(4-methyl-phen-yl)hydrazinyl-idene]acetate, methyl (2Z)-(4-bromophen-yl)[2-(3,5-di-methyl-phen-yl)hydrazinyl-idene]acetate, methyl (2Z)-[2-(4-meth-oxy-phen-yl)hydrazinyl-idene](3-nitro-phen-yl)acetate, methyl (2E)-(4-chlorophen-yl)(2-phenyl-hydrazinyl-idene)acetate and methyl (2Z)-[2-(4-bromo-phen-yl)hydrazinylidene](4-chloro-phen-yl)acetate. ; _journal_coeditor_code WM5749 _journal_issue 'Pt 4' _journal_name_full 'Acta crystallographica. Section E, Crystallographic communications' _journal_page_first 314 _journal_page_last 323 _journal_paper_doi 10.1107/S2056989025002051 _journal_volume 81 _journal_year 2025 _chemical_formula_iupac 'C16 H15 N3 O5' _chemical_formula_moiety 'C16 H15 N3 O5' _chemical_formula_sum 'C16 H15 N3 O5' _chemical_formula_weight 329.31 _chemical_name_systematic ; Methyl (Z)-2-[2-(4-methoxyphenyl)hydrazin-1-ylidene]-2-(3-nitrophenyl)acetate ; _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary difmap _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 96.156(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 18.8022(5) _cell_length_b 21.9649(6) _cell_length_c 7.43092(15) _cell_measurement_reflns_used 4042 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 78.232 _cell_measurement_theta_min 4.026 _cell_volume 3051.19(13) _computing_cell_refinement ; CrysAlisPro (Rigaku OD, 2021) ; _computing_data_collection ; CrysAlisPro (Rigaku OD, 2021) ; _computing_data_reduction ; CrysAlisPro (Rigaku OD, 2021) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Rigaku XtaLAB Synergy-S, HyPix-6000HE area-detector' _diffrn_measurement_method '\f and \w' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0724 _diffrn_reflns_av_unetI/netI 0.0440 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_number 21181 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 80.023 _diffrn_reflns_theta_min 3.104 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.914 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.322 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2021). ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.434 _exptl_crystal_description 'prismatic needle' _exptl_crystal_F_000 1376 _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.271 _refine_diff_density_min -0.252 _refine_ls_extinction_coef 0.00022(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 223 _refine_ls_number_reflns 3303 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.066 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0461 _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^)+(0.0486P)^2^+2.64P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1093 _refine_ls_wR_factor_ref 0.1260 _reflns_number_gt 2634 _reflns_number_total 3303 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5749.cif _cod_data_source_block 3 _cod_depositor_comments 'Adding full bibliography for 2023444--2023448.cif.' _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2023446 _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 0.777 _shelx_estimated_absorpt_t_max 0.922 _shelx_hkl_file ; 0 0 1 0.03 0.09 0 0 1 0.10 0.17 0 0 1 -0.10 0.20 0 0 2 265.23 11.33 0 0 3 -0.32 0.45 0 0 3 -0.31 0.44 0 0 3 0.34 0.49 0 0 4 0.44 0.88 0 0 4 0.99 0.86 0 0 4 -0.98 1.84 0 0 4 0.90 1.20 0 0 4 -0.90 1.43 0 0 4 0.45 1.11 0 0 5 0.58 0.58 0 0 5 -0.59 0.84 0 0 5 -0.67 0.67 0 0 5 -0.59 0.84 0 0 5 0.60 1.04 0 0 5 0.66 0.93 0 0 6 165.44 12.76 0 0 6 159.76 12.33 0 0 6 177.00 13.49 0 0 6 161.15 12.72 0 0 6 151.12 12.76 0 0 6 175.91 12.41 0 0 6 171.51 12.17 0 0 6 155.72 12.22 0 0 6 181.78 13.42 0 0 6 143.22 12.30 0 0 6 165.16 13.13 0 0 6 165.14 12.49 0 0 6 149.25 12.59 0 0 7 0.70 0.70 0 0 7 -0.71 1.75 0 0 7 0.76 0.76 0 0 7 -0.71 0.71 0 0 7 -0.81 1.14 0 0 7 0.59 0.83 0 0 7 -0.81 0.82 0 0 7 -0.74 1.06 0 0 7 -0.60 0.85 0 0 7 -0.72 1.02 0 0 7 0.83 1.18 0 0 7 0.77 0.77 0 0 7 -0.71 1.00 0 0 7 0.64 1.58 0 0 8 0.52 1.27 0 0 8 5.42 2.10 0 0 8 1.59 1.51 0 0 8 3.86 1.84 0 0 8 6.70 2.07 0 0 8 5.36 1.99 0 0 8 3.64 1.65 0 0 8 1.55 1.16 0 2 0 19.27 1.22 0 -2 1 667.95 23.76 0 2 1 674.43 23.75 0 2 1 683.20 23.80 0 -2 1 696.50 23.85 0 2 1 689.57 23.67 0 -2 1 698.27 23.92 0 2 1 696.86 23.89 0 2 -1 706.23 23.20 0 -2 2 468.82 18.19 0 2 2 464.95 18.17 0 -2 2 469.87 18.40 0 2 2 467.75 18.39 0 2 2 470.07 17.09 0 2 2 471.04 18.15 0 -2 2 494.49 18.31 0 -2 3 176.52 9.70 0 2 3 184.38 9.78 0 2 3 198.66 10.27 0 -2 3 179.61 9.99 0 2 3 175.20 7.87 0 -2 3 185.14 9.74 0 2 3 180.35 9.65 0 -2 4 19.30 3.26 0 2 4 16.34 3.07 0 2 4 13.97 2.72 0 -2 4 15.74 2.82 0 -2 4 13.43 2.71 0 2 4 13.90 2.79 0 -2 4 13.90 2.79 0 2 4 19.21 3.18 0 2 4 18.18 3.28 0 -2 4 18.53 3.29 0 2 -4 16.89 2.36 0 2 4 15.60 2.95 0 -2 4 17.41 3.05 0 -2 5 52.98 6.06 0 2 5 61.14 6.52 0 -2 5 65.29 6.74 0 2 5 64.79 6.72 0 -2 5 64.31 6.97 0 2 5 64.15 7.05 0 -2 5 61.99 6.69 0 2 5 53.69 6.33 0 2 5 63.42 6.99 0 -2 5 67.37 7.24 0 -2 6 5.87 2.18 0 -2 6 5.51 2.62 0 -2 6 4.92 2.24 0 -2 6 4.46 2.12 0 2 6 1.41 1.23 0 2 6 4.53 2.28 0 -2 6 10.43 3.05 0 -2 6 7.11 2.37 0 2 6 5.56 2.21 0 2 6 5.50 2.37 0 -2 6 4.68 2.08 0 2 6 4.04 1.99 0 -2 6 7.22 2.55 0 2 6 6.62 2.45 0 -2 6 4.25 2.02 0 2 6 5.31 2.16 0 2 6 1.63 1.64 0 2 6 7.28 2.57 0 -2 6 4.04 2.15 0 -2 6 5.89 2.28 0 -2 6 4.95 2.02 0 2 6 2.40 1.61 0 -2 6 10.39 3.11 0 2 6 4.93 1.83 0 -2 6 2.90 1.64 0 -2 6 9.31 2.79 0 2 6 5.01 2.16 0 -2 7 29.83 4.92 0 2 7 25.79 4.59 0 -2 7 26.21 4.71 0 2 7 22.96 4.57 0 2 7 30.90 5.33 0 -2 7 28.72 4.76 0 2 7 22.28 4.52 0 2 7 21.86 4.25 0 -2 7 26.84 4.95 0 -2 7 21.04 4.35 0 2 7 24.55 4.68 0 -2 7 23.93 4.46 0 -2 7 24.40 4.74 0 -2 7 21.87 4.18 0 2 7 21.49 4.69 0 2 7 24.38 4.87 0 -2 7 24.80 4.29 0 -2 7 18.03 3.98 0 -2 7 25.51 4.55 0 2 7 24.85 4.51 0 -2 7 23.90 4.65 0 2 7 26.81 5.02 0 2 7 21.37 4.39 0 -2 7 26.27 4.39 0 2 8 -0.56 0.57 0 -2 8 -0.56 1.11 0 2 8 -0.51 0.89 0 2 8 -0.57 0.99 0 -2 8 -0.51 0.89 0 -2 8 -0.57 0.81 0 2 8 -0.52 0.74 0 2 8 0.57 0.81 0 2 8 -0.58 1.01 0 2 8 0.50 1.33 0 2 8 1.00 1.01 0 -2 8 0.50 1.01 0 4 0 2148.62 71.15 0 -4 1 1121.65 39.25 0 4 1 1236.00 39.38 0 4 1 1187.67 39.34 0 -4 1 1144.92 39.31 0 4 1 1205.60 40.22 0 4 1 1156.67 39.40 0 -4 1 1124.73 39.38 0 4 -1 1205.60 39.14 0 -4 2 311.91 12.81 0 4 2 325.69 12.85 0 -4 2 299.97 12.75 0 4 2 302.93 12.76 0 4 2 311.80 12.69 0 -4 2 284.36 12.81 0 4 2 329.13 13.13 0 4 -2 308.82 11.56 0 4 3 452.85 18.97 0 -4 3 463.68 19.07 0 -4 3 459.41 19.14 0 4 3 446.89 19.03 0 4 3 462.84 18.07 0 4 -3 441.56 16.99 0 4 3 463.11 19.54 0 -4 3 448.88 19.35 0 -4 4 5.71 1.82 0 4 4 4.82 1.76 0 -4 4 2.64 1.26 0 4 4 4.84 1.72 0 4 4 4.92 1.64 0 -4 4 3.45 1.41 0 4 4 5.26 1.71 0 -4 4 4.40 1.54 0 4 4 6.00 1.83 0 -4 4 6.02 1.79 0 4 4 2.94 1.48 0 -4 4 3.39 1.46 0 4 5 9.21 2.65 0 -4 5 5.92 2.21 0 4 5 8.66 2.47 0 -4 5 8.64 2.40 0 -4 5 8.31 2.50 0 4 5 9.70 2.77 0 4 6 2.03 1.67 0 -4 6 -0.73 0.74 0 -4 6 5.40 2.04 0 -4 6 1.36 1.81 0 4 6 6.13 2.43 0 4 6 1.34 1.16 0 -4 6 1.33 1.16 0 4 6 2.75 1.83 0 -4 6 3.44 2.07 0 -4 6 6.43 2.42 0 4 6 6.24 2.41 0 4 6 1.57 1.58 0 4 6 4.01 1.97 0 -4 6 4.66 2.21 0 4 6 4.09 2.01 0 -4 6 3.77 1.78 0 4 6 1.57 1.11 0 -4 6 5.50 2.23 0 -4 6 4.17 1.85 0 -4 6 2.28 1.28 0 -4 6 3.05 1.50 0 -4 6 0.59 1.45 0 -4 6 4.65 2.06 0 4 6 2.32 1.55 0 -4 6 2.44 1.37 0 4 7 -0.70 1.73 0 4 7 0.64 1.11 0 -4 7 -0.63 1.10 0 4 7 -0.81 1.15 0 -4 7 -0.56 0.79 0 4 7 0.75 1.06 0 4 7 0.75 0.75 0 -4 7 0.74 1.05 0 -4 7 -0.66 0.93 0 -4 7 -0.75 1.06 0 4 7 -0.66 0.93 0 -4 7 -0.55 0.96 0 4 7 0.85 1.20 0 -4 7 -0.65 0.92 0 -4 7 0.71 1.00 0 -4 7 -0.67 0.95 0 4 7 -0.65 0.65 0 4 7 -0.74 1.05 0 -4 7 -0.53 0.76 0 -4 7 -0.74 1.05 0 -4 7 -0.54 0.54 0 4 7 -0.87 1.24 0 4 8 1.14 1.15 0 -4 8 1.04 1.04 0 4 8 1.84 1.37 0 4 8 -0.51 0.51 0 4 8 1.13 0.98 0 4 8 0.46 0.65 0 -4 8 1.99 1.12 0 4 8 1.72 1.41 0 6 0 296.74 12.25 0 -6 1 32.59 1.93 0 6 1 28.14 1.85 0 -6 1 30.48 1.89 0 6 1 32.01 1.96 0 -6 1 28.18 1.93 0 6 -1 31.28 2.31 0 -6 2 32.71 2.75 0 6 2 31.80 2.75 0 -6 2 33.60 2.80 0 6 2 29.91 2.67 0 6 -2 29.70 2.36 0 6 2 37.40 3.43 0 -6 2 31.49 2.83 0 6 2 34.21 2.94 0 6 -2 30.33 2.23 0 -6 3 4.43 1.27 0 6 3 4.38 1.29 0 -6 3 4.82 1.39 0 6 3 5.08 1.48 0 6 3 6.26 1.52 0 6 3 5.01 1.39 0 -6 3 6.39 1.56 0 6 -3 4.33 0.86 0 -6 3 5.17 0.89 0 -6 4 8.08 2.29 0 6 4 8.44 2.23 0 -6 4 11.50 2.44 0 6 4 7.19 2.15 0 6 4 9.07 2.26 0 -6 4 12.47 2.49 0 -6 4 14.22 2.71 0 6 4 13.03 2.68 0 -6 4 13.59 2.78 0 6 4 14.00 2.76 0 6 4 10.27 2.04 0 6 4 8.05 2.15 0 -6 4 14.90 2.79 0 6 5 38.28 5.40 0 6 5 36.86 5.20 0 -6 5 41.53 5.53 0 -6 5 30.88 4.83 0 -6 6 33.22 5.01 0 -6 6 27.92 4.73 0 6 6 23.20 4.28 0 -6 6 26.07 4.44 0 -6 6 38.91 5.27 0 6 6 32.13 4.86 0 6 6 28.08 5.14 0 -6 6 32.55 4.97 0 -6 6 33.81 5.92 0 6 6 21.63 4.10 0 6 6 22.96 4.95 0 -6 6 28.17 4.97 0 6 6 36.37 5.96 0 -6 6 28.07 5.04 0 -6 6 27.72 4.42 0 6 6 31.63 5.51 0 -6 6 36.92 4.94 0 -6 6 34.26 4.49 0 6 6 24.58 4.58 0 -6 6 37.21 5.61 0 -6 6 23.28 4.43 0 6 6 32.51 5.47 0 6 6 25.06 4.72 0 6 6 52.44 9.18 0 6 6 32.34 6.08 0 -6 7 11.84 2.90 0 6 7 6.54 2.19 0 6 7 5.10 1.98 0 6 7 8.00 2.52 0 6 7 10.96 3.25 0 6 7 10.20 2.96 0 6 7 7.58 2.65 0 6 7 5.91 2.30 0 -6 7 6.67 2.33 0 -6 7 9.46 2.97 0 6 7 7.53 2.26 0 -6 7 7.48 2.32 0 -6 7 4.41 2.10 0 6 8 22.54 3.99 0 6 8 23.00 3.75 0 6 8 28.89 4.32 0 -6 8 23.13 3.84 0 6 9 5.41 1.24 0 8 0 71.06 4.98 0 8 -1 7.82 1.49 0 8 -1 6.71 1.21 0 8 2 64.16 4.07 0 -8 2 59.89 4.04 0 8 -2 64.58 3.88 0 8 -2 60.48 4.25 0 8 2 71.51 5.56 0 8 3 0.41 0.41 0 -8 3 0.32 0.45 0 -8 3 0.56 0.75 0 -8 4 15.71 2.88 0 8 4 13.68 2.70 0 -8 4 12.10 2.53 0 8 4 12.42 2.51 0 -8 4 8.76 2.36 0 8 4 8.38 2.17 0 8 5 24.18 6.56 0 -8 5 9.49 2.60 0 8 5 14.96 3.73 0 -8 5 11.45 2.86 0 8 5 11.32 3.27 0 -8 5 11.15 3.32 0 -8 5 13.25 3.52 0 -8 5 13.02 2.79 0 8 5 9.88 3.46 0 8 5 10.04 2.61 0 8 5 9.07 2.96 0 -8 5 13.17 3.03 0 -8 5 12.57 3.49 0 -8 6 1.66 1.11 0 8 6 1.66 1.24 0 8 6 1.09 0.94 0 8 6 1.45 1.26 0 -8 6 1.63 1.22 0 8 6 1.68 1.88 0 -8 6 1.29 1.30 0 8 6 0.66 1.14 0 8 6 1.92 1.29 0 -8 6 0.65 1.31 0 -8 6 3.11 1.53 0 -8 6 2.55 1.91 0 8 6 1.57 1.57 0 8 6 1.07 1.07 0 8 6 2.86 1.91 0 8 6 0.83 0.83 0 8 6 1.12 0.97 0 -8 6 1.13 1.27 0 -8 7 10.05 2.47 0 8 7 9.62 2.44 0 -8 7 7.96 2.23 0 8 7 6.58 2.08 0 8 7 9.55 2.60 0 8 7 16.14 3.79 0 8 7 13.78 3.43 0 -8 7 13.22 3.76 0 8 7 12.66 4.48 0 -8 7 5.53 2.40 0 8 7 7.68 2.69 0 8 7 11.30 3.02 0 -8 7 11.66 2.75 0 8 7 12.15 3.50 0 8 7 12.43 2.78 0 8 8 -0.46 1.31 0 -8 8 0.49 0.99 0 8 8 1.51 1.24 0 8 8 3.93 1.86 0 8 8 3.88 1.46 0 8 9 18.74 1.95 0 10 0 8.64 1.86 0 10 1 2.31 1.03 0 10 -1 5.77 1.44 0 10 -2 22.46 2.79 0 10 2 24.66 3.56 0 10 3 1.03 0.89 0 -10 3 0.82 0.48 0 -10 4 28.88 4.66 0 10 4 28.61 4.45 0 10 5 15.96 5.32 0 10 5 7.64 2.83 0 -10 5 7.05 2.36 0 10 5 5.05 2.24 0 -10 5 5.24 2.33 0 -10 5 7.00 2.40 0 10 5 5.43 2.68 0 10 5 7.43 2.59 0 -10 5 2.65 1.78 0 10 6 26.95 3.89 0 10 6 28.52 3.88 0 10 6 37.06 5.30 0 10 6 32.72 5.68 0 10 6 22.52 4.70 0 10 6 35.17 6.69 0 10 6 34.95 8.24 0 -10 6 23.63 4.84 0 -10 6 22.29 5.00 0 -10 6 35.71 4.70 0 10 6 27.77 5.05 0 10 6 47.64 7.47 0 10 7 2.81 2.45 0 10 7 1.57 1.58 0 10 7 4.86 1.97 0 10 7 5.66 2.19 0 10 7 4.47 2.12 0 -10 8 0.43 0.74 0 10 8 0.61 1.06 0 10 8 -0.72 1.02 0 10 8 -0.41 0.72 0 10 8 -0.46 0.65 0 12 0 1249.35 46.94 0 12 1 257.73 14.09 0 12 -1 242.54 13.08 0 12 -2 166.02 9.83 0 12 2 167.82 11.27 0 12 3 0.63 0.63 0 -12 4 44.35 6.22 0 12 4 43.21 5.92 0 -12 4 32.64 5.58 0 12 4 38.83 5.91 0 -12 4 40.78 6.03 0 12 4 46.52 6.53 0 12 5 1.38 1.38 0 12 5 -1.16 1.17 0 12 5 3.48 3.03 0 -12 5 0.89 1.27 0 12 5 1.68 1.47 0 -12 5 0.85 1.21 0 -12 5 1.60 1.39 0 12 6 0.84 1.46 0 12 6 0.81 1.41 0 12 6 1.69 2.41 0 12 6 1.08 1.88 0 -12 6 -0.86 1.22 0 12 6 -1.04 1.48 0 12 6 0.67 0.95 0 -12 6 -0.88 1.26 0 -12 7 1.92 1.29 0 12 7 2.64 2.30 0 12 7 3.92 1.97 0 12 7 0.61 0.62 0 12 7 5.01 1.89 0 12 7 1.98 1.31 0 12 8 -0.44 0.88 0 12 8 0.32 0.46 0 14 0 9.48 2.46 0 14 1 88.39 8.13 0 14 -1 95.50 7.95 0 14 2 0.67 0.95 0 14 -2 -0.49 0.69 0 14 3 236.85 15.68 0 14 4 108.84 10.29 0 14 4 71.33 8.23 0 14 4 83.38 9.22 0 -14 4 89.96 9.51 0 14 4 92.76 9.42 0 -14 4 87.03 9.34 0 -14 4 76.41 8.68 0 14 5 94.16 11.50 0 14 5 100.70 8.57 0 14 5 91.98 9.53 0 14 5 86.04 9.71 0 -14 5 100.24 9.90 0 14 5 98.76 14.31 0 -14 5 98.85 10.45 0 -14 5 94.70 9.76 0 -14 5 100.29 10.18 0 14 6 18.93 5.74 0 14 6 19.24 4.57 0 14 6 16.21 3.66 0 14 6 17.30 3.24 0 -14 6 20.91 4.22 0 14 7 1.02 1.78 0 14 7 -0.48 0.68 0 -14 7 0.50 0.50 0 14 7 1.95 1.09 0 14 7 -0.32 0.73 0 14 8 3.41 1.10 0 14 8 2.62 0.73 0 16 0 97.07 9.02 0 16 1 0.73 1.03 0 16 -1 2.55 1.43 0 -16 -2 21.74 4.46 0 -16 2 11.39 3.08 0 16 2 27.78 5.10 0 16 2 17.14 3.87 0 16 2 17.36 3.92 0 -16 -3 4.03 1.98 0 16 3 0.76 1.08 0 -16 3 0.70 0.70 0 -16 3 -0.71 1.00 0 -16 3 0.86 0.86 0 16 3 0.85 0.85 0 16 3 2.60 1.74 0 -16 3 1.71 1.49 0 -16 -4 121.50 10.89 0 16 4 105.90 10.53 0 16 4 119.20 10.32 0 16 4 106.08 10.69 0 -16 4 109.43 10.41 0 -16 4 126.60 11.65 0 -16 4 140.76 11.49 0 16 4 125.65 11.65 0 -16 4 130.48 11.74 0 -16 5 12.49 3.36 0 16 5 14.56 4.33 0 16 5 14.85 3.42 0 16 5 14.55 3.92 0 -16 5 15.28 3.84 0 16 5 15.82 5.74 0 -16 5 13.39 3.37 0 16 6 13.61 4.50 0 16 6 13.73 3.62 0 16 6 16.80 3.85 0 16 6 9.27 2.48 0 16 6 11.66 2.94 0 16 6 14.70 3.07 0 -16 6 11.75 2.86 0 -16 7 2.58 1.22 0 -16 7 3.03 1.17 0 16 7 0.84 0.63 0 16 7 2.55 1.01 0 18 0 17.98 4.05 0 18 0 16.26 4.08 0 -18 0 24.11 4.74 0 -18 0 18.81 4.34 0 18 0 21.21 4.35 0 18 0 16.65 4.08 0 18 -1 19.19 4.13 0 18 1 17.13 4.19 0 -18 -1 14.04 3.78 0 -18 1 22.41 4.43 0 -18 1 21.45 4.57 0 18 1 19.09 4.21 0 18 -1 13.91 3.50 0 18 -1 19.26 4.03 0 18 2 4.28 2.11 0 18 2 0.93 1.86 0 18 -2 1.44 1.26 0 -18 2 0.93 1.61 0 -18 -2 1.77 1.26 0 -18 2 2.32 1.55 0 -18 2 3.50 1.86 0 -18 -2 5.94 2.41 0 18 3 123.31 10.50 0 -18 -3 125.48 11.34 0 -18 -3 126.83 11.45 0 18 3 107.09 11.05 0 18 3 103.36 10.74 0 -18 3 118.77 11.29 0 -18 4 44.11 6.52 0 18 4 33.90 5.72 0 -18 -4 49.99 6.39 0 -18 -4 47.62 6.49 0 -18 4 36.43 5.28 0 -18 4 41.49 6.37 0 18 4 50.07 6.56 0 -18 5 1.43 1.62 0 -18 5 8.23 2.49 0 -18 5 5.12 1.81 0 18 5 5.91 2.40 0 -18 -5 5.68 1.80 0 18 5 1.28 1.82 0 18 5 5.35 2.13 0 18 5 5.33 1.76 0 18 6 112.32 7.24 0 -18 6 104.86 7.46 0 -18 6 100.68 8.13 0 18 6 91.93 10.05 0 -18 7 1.20 0.48 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0.98 -22 4 3 0.68 0.84 -22 -4 3 1.38 0.92 -22 4 2 3.25 1.42 -22 -4 2 2.88 1.31 -22 4 2 5.29 1.59 -22 -4 2 6.58 1.85 -22 4 2 4.30 1.50 -22 -4 2 4.49 1.48 22 -4 -2 3.79 1.30 22 4 -2 2.79 1.11 -22 4 2 4.17 1.57 -22 -4 2 2.14 1.22 -22 -4 2 2.08 1.03 -22 4 2 5.78 1.66 -22 4 2 1.29 0.97 22 4 -2 4.51 1.44 22 -4 -2 3.77 1.25 22 4 -1 10.07 2.14 22 -4 -1 7.28 1.82 -22 4 1 7.97 1.99 -22 -4 1 2.55 1.30 -22 4 1 5.46 1.75 -22 -4 1 6.81 2.06 -22 4 1 7.34 1.90 -22 -4 1 11.06 2.44 -22 4 1 9.76 2.24 -22 -4 1 5.92 1.76 -22 4 1 7.92 2.10 -22 -4 1 3.86 1.38 -22 4 1 5.10 1.61 22 -4 -1 10.01 2.13 22 4 -1 7.04 1.81 -22 -4 0 11.54 2.31 -22 4 0 7.87 1.96 -22 4 0 9.18 2.21 -22 4 0 7.99 2.06 22 -4 0 8.55 2.05 22 4 0 8.32 2.01 -22 4 0 6.20 1.73 -22 -4 0 10.61 2.18 22 4 0 9.05 2.11 22 -4 0 9.70 2.08 -22 4 0 8.81 2.03 -22 -4 0 13.16 2.49 -22 4 -1 1.97 0.99 -22 -4 -1 2.73 1.19 22 -4 1 3.66 0.99 -22 4 -1 4.83 1.43 22 -4 1 3.42 1.24 22 4 1 2.46 1.06 -22 4 -1 3.04 1.27 22 4 2 5.24 1.22 22 -4 2 7.15 1.43 -22 -4 -2 5.34 1.27 -22 4 -2 6.25 1.33 22 4 2 5.06 1.22 -22 -6 4 4.99 1.07 -22 -6 3 -0.24 0.48 -22 -6 3 0.25 0.44 22 6 -3 0.40 0.41 -22 -6 3 0.71 0.58 22 6 -3 0.30 0.68 -22 -6 2 2.54 1.06 -22 6 2 1.81 0.97 -22 -6 2 2.67 1.07 22 6 -2 3.60 1.18 -22 -6 2 4.44 1.36 22 6 -2 2.74 1.18 -22 -6 1 27.48 3.33 -22 -6 1 32.36 3.73 22 6 -1 22.91 2.99 -22 6 1 30.94 3.90 22 6 -1 26.88 3.60 -22 6 1 21.83 3.18 -22 -6 1 33.16 3.62 -22 6 0 17.97 2.96 -22 6 0 18.60 2.93 22 6 0 16.09 2.47 -22 -6 -1 0.51 0.44 22 6 1 0.65 0.49 -22 6 -1 0.31 0.62 22 6 1 1.00 0.61 -22 6 -1 0.99 0.66 22 6 2 0.36 0.40 -22 -8 3 12.60 1.73 22 8 -3 14.80 1.94 22 8 -2 25.65 3.15 -22 8 1 37.83 3.84 -22 -8 1 26.36 2.45 -22 -8 1 20.33 2.26 22 8 -1 34.12 3.69 -22 -8 1 26.84 2.45 -22 8 0 0.33 0.33 -22 8 0 0.32 0.45 -22 8 -1 0.98 0.61 -22 8 -1 1.28 0.63 -22 -8 -1 1.00 0.62 22 10 -2 16.35 2.08 -22 10 1 0.44 0.49 22 10 -1 -0.24 0.34 -22 10 0 0.42 0.42 -23 -1 3 0.77 0.63 -23 1 3 1.16 0.58 -23 -1 3 0.51 0.51 23 1 -3 0.43 0.44 23 1 -3 0.25 0.35 -23 1 3 0.79 0.59 -23 -1 3 0.27 0.46 -23 -1 2 0.65 0.66 23 1 -2 1.15 0.76 -23 -1 2 3.27 1.18 -23 -1 2 1.36 0.84 -23 -1 1 2.40 1.14 -23 -1 1 0.69 0.69 23 1 -1 1.61 0.86 -23 -1 1 1.07 0.88 23 1 0 0.32 0.55 -23 -1 0 0.33 0.57 -23 1 0 0.64 0.78 23 1 1 5.43 1.30 23 1 1 2.52 0.95 -23 1 -1 4.80 1.22 -23 1 -1 4.03 1.11 -23 -1 -1 3.07 1.03 -23 3 3 2.51 0.83 -23 -3 3 4.92 1.15 -23 3 3 4.06 1.02 -23 3 3 6.30 1.23 -23 -3 3 7.58 1.36 23 3 -3 7.16 1.35 23 -3 -3 5.67 1.08 23 3 -3 2.57 0.82 -23 3 3 7.55 1.35 -23 -3 3 8.03 1.42 -23 3 2 35.37 3.57 -23 -3 2 41.29 3.90 -23 3 2 32.08 3.53 -23 -3 2 46.93 4.21 -23 3 2 37.74 3.67 -23 -3 2 41.10 3.87 23 -3 -2 40.27 3.62 23 3 -2 45.19 3.83 -23 3 1 3.65 1.19 -23 -3 1 6.81 1.59 23 -3 -1 4.84 1.29 23 3 -1 7.26 1.58 -23 -3 1 4.32 1.29 -23 3 1 3.93 1.22 -23 3 1 4.38 1.32 23 3 -1 3.69 1.16 -23 3 1 4.06 1.26 -23 -3 1 4.20 1.31 -23 -3 0 -0.30 0.59 -23 3 0 0.28 0.40 -23 3 0 -0.30 0.42 23 -3 0 -0.27 1.07 23 3 0 -1.41 1.30 -23 3 0 -0.27 1.03 -23 3 0 -0.30 0.42 23 -3 1 5.57 1.19 23 3 1 6.48 1.32 -23 3 -1 5.53 1.16 -23 -3 -1 6.60 1.31 -23 3 -1 6.92 1.40 23 3 1 7.17 1.28 23 -3 1 7.27 1.38 -23 5 3 0.18 0.31 -23 -5 2 6.05 1.23 -23 -5 2 7.22 1.32 23 5 -2 3.84 0.97 -23 -5 2 4.10 1.03 -23 -5 1 -0.23 0.40 -23 -5 1 -0.23 0.40 -23 -5 1 -0.24 0.42 23 5 -1 -0.27 0.47 23 5 -1 0.22 0.31 23 5 0 1.19 0.63 -23 -5 0 0.60 0.45 -23 -5 0 0.81 0.54 -23 -5 0 0.86 0.61 -23 5 0 2.27 0.91 -23 5 0 2.11 0.84 -23 5 -1 1.08 0.51 23 7 -2 20.29 2.22 23 7 -1 0.20 0.41 -23 7 1 0.64 0.48 -23 7 0 0.18 0.25 -23 7 0 0.20 0.28 0 0 0 0.00 0.00 TITL 24VKh_R081_gaus in C2/c REM C2/c (#15 in standard setting) CELL 1.54184 18.802233 21.964929 7.430919 90.0000 96.1561 90.0000 ZERR 8.00 0.000474 0.000616 0.000153 0.0000 0.0023 0.0000 LATT 7 SYMM -x, y,-z+1/2 SFAC C H N O UNIT 128.00 120.00 24.00 40.00 REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0 TEMP -173 SIZE 0.09 0.10 0.29 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 38364 _shelx_res_file ; TITL (3) in C2/c CELL 1.54184 18.8022 21.9649 7.43092 90.0000 96.156 90.0000 ZERR 8.00 0.0005 0.0006 0.00015 0.0000 0.002 0.0000 LATT 7 SYMM -X, +Y, 0.5-Z SFAC C H N O UNIT 128 120 24 40 TEMP -173.0 SIZE 0.09 0.10 0.29 L.S. 12 BOND $H ACTA CONF HTAB N2 O1 WGHT 0.048600 2.640000 EXTI 0.000217 FVAR 0.19101 O1 4 0.616960 0.619435 0.382951 11.00000 0.02971 0.02394 = 0.02766 -0.00019 0.00433 -0.00029 O2 4 0.683701 0.704459 0.371264 11.00000 0.01914 0.02620 = 0.03570 0.00095 0.00565 0.00053 O3 4 0.637578 0.865429 -0.028054 11.00000 0.03956 0.03294 = 0.01964 -0.00127 0.00875 -0.00220 O4 4 0.592729 0.951444 0.048567 11.00000 0.03101 0.02459 = 0.03054 0.00854 0.00243 -0.00095 O5 4 0.243121 0.553646 0.766394 11.00000 0.02210 0.02496 = 0.02783 0.00034 0.00708 -0.00202 N1 3 0.506395 0.698268 0.500097 11.00000 0.02306 0.02399 = 0.01888 0.00339 0.00015 -0.00252 N2 3 0.493234 0.639458 0.515245 11.00000 0.02422 0.02331 = 0.02562 0.00282 0.00409 -0.00260 H2 2 0.524637 0.613301 0.487862 11.00000 -1.20000 N3 3 0.609484 0.898183 0.079225 11.00000 0.02294 0.02584 = 0.02006 0.00282 0.00152 -0.00387 C1 1 0.566609 0.716597 0.442526 11.00000 0.02117 0.02488 = 0.01653 0.00259 0.00046 -0.00103 C2 1 0.623025 0.674544 0.394943 11.00000 0.02262 0.02546 = 0.01761 0.00153 0.00128 -0.00237 C3 1 0.743751 0.667345 0.332418 11.00000 0.02312 0.03216 = 0.04047 -0.00017 0.00587 0.00448 AFIX 137 H3A 2 0.731299 0.645038 0.219204 11.00000 -1.50000 H3B 2 0.755439 0.638355 0.431429 11.00000 -1.50000 H3C 2 0.785196 0.693498 0.320302 11.00000 -1.50000 AFIX 0 C4 1 0.575189 0.783404 0.428926 11.00000 0.01690 0.02360 = 0.01823 0.00214 -0.00050 -0.00118 C5 1 0.593111 0.809072 0.267229 11.00000 0.01886 0.02563 = 0.01604 -0.00141 0.00184 -0.00019 AFIX 43 H5 2 0.603816 0.784000 0.169503 11.00000 -1.20000 AFIX 0 C6 1 0.594827 0.871672 0.253461 11.00000 0.01841 0.02453 = 0.01679 0.00232 0.00119 -0.00235 C7 1 0.581086 0.910570 0.392228 11.00000 0.02083 0.02135 = 0.02522 -0.00218 0.00203 -0.00101 AFIX 43 H7 2 0.581852 0.953497 0.376954 11.00000 -1.20000 AFIX 0 C8 1 0.566152 0.884698 0.554456 11.00000 0.02142 0.02995 = 0.01990 -0.00336 0.00354 0.00079 AFIX 43 H8 2 0.558154 0.910046 0.653901 11.00000 -1.20000 AFIX 0 C9 1 0.562881 0.821740 0.571626 11.00000 0.01887 0.03027 = 0.01780 0.00242 0.00316 -0.00044 AFIX 43 H9 2 0.552046 0.804558 0.682798 11.00000 -1.20000 AFIX 0 C10 1 0.429436 0.619272 0.579572 11.00000 0.02375 0.02666 = 0.01776 0.00111 0.00054 -0.00453 C11 1 0.421162 0.557012 0.600322 11.00000 0.02263 0.02414 = 0.02556 0.00001 0.00458 0.00038 AFIX 43 H11 2 0.457914 0.530230 0.571189 11.00000 -1.20000 AFIX 0 C12 1 0.359649 0.533084 0.663374 11.00000 0.02471 0.02173 = 0.02354 0.00054 0.00293 -0.00186 AFIX 43 H12 2 0.354547 0.490386 0.677808 11.00000 -1.20000 AFIX 0 C13 1 0.306013 0.572563 0.704709 11.00000 0.02191 0.02609 = 0.01682 0.00054 0.00179 -0.00380 C14 1 0.313906 0.635143 0.683473 11.00000 0.02403 0.02526 = 0.02058 -0.00151 0.00186 0.00074 AFIX 43 H14 2 0.277007 0.661923 0.711690 11.00000 -1.20000 AFIX 0 C15 1 0.375401 0.658649 0.621284 11.00000 0.02674 0.02295 = 0.02165 0.00140 0.00056 -0.00161 AFIX 43 H15 2 0.380594 0.701356 0.607260 11.00000 -1.20000 AFIX 0 C16 1 0.230325 0.489378 0.763547 11.00000 0.02551 0.02619 = 0.02477 0.00335 0.00396 -0.00405 AFIX 137 H16A 2 0.230200 0.474174 0.639526 11.00000 -1.50000 H16B 2 0.183875 0.481055 0.806915 11.00000 -1.50000 H16C 2 0.268140 0.468916 0.842250 11.00000 -1.50000 AFIX 0 HKLF 4 REM (3) in C2/c REM R1 = 0.0461 for 2634 Fo > 4sig(Fo) and 0.0595 for all 3303 data REM 223 parameters refined using 0 restraints END WGHT 0.0486 2.6381 REM Highest difference peak 0.271, deepest hole -0.252, 1-sigma level 0.057 Q1 1 0.5978 0.8401 0.2663 11.00000 0.05 0.27 Q2 1 0.4747 0.7226 0.5443 11.00000 0.05 0.26 Q3 1 0.4217 0.5914 0.5593 11.00000 0.05 0.25 Q4 1 0.3111 0.6074 0.6753 11.00000 0.05 0.25 Q5 1 0.5711 0.7532 0.4378 11.00000 0.05 0.24 Q6 1 0.4152 0.6337 0.6358 11.00000 0.05 0.24 Q7 1 0.5502 0.8042 0.4809 11.00000 0.05 0.22 Q8 1 0.2612 0.4522 0.8366 11.00000 0.05 0.21 Q9 1 0.5797 0.7977 0.3605 11.00000 0.05 0.20 Q10 1 0.5754 0.8932 0.3044 11.00000 0.05 0.20 Q11 1 0.7223 0.5939 0.3089 11.00000 0.05 0.20 Q12 1 0.6014 0.5682 0.4371 11.00000 0.05 0.20 Q13 1 0.7406 0.6295 0.2630 11.00000 0.05 0.19 Q14 1 0.3377 0.5507 0.7051 11.00000 0.05 0.19 Q15 1 0.5557 0.8935 0.4639 11.00000 0.05 0.18 Q16 1 0.2998 0.7297 0.4050 11.00000 0.05 0.18 Q17 1 0.5692 0.8587 0.5748 11.00000 0.05 0.18 Q18 1 0.5923 0.7931 0.5107 11.00000 0.05 0.18 Q19 1 0.6223 0.8306 0.0210 11.00000 0.05 0.18 Q20 1 0.2651 0.7100 0.7655 11.00000 0.05 0.18 ; _shelx_res_checksum 79511 _shelxl_version_number .2013 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.61696(7) 0.61943(6) 0.38295(16) 0.0270(3) Uani d 1 . . O O2 0.68370(6) 0.70446(6) 0.37126(17) 0.0268(3) Uani d 1 . . O O3 0.63758(7) 0.86543(6) -0.02805(16) 0.0303(3) Uani d 1 . . O O4 0.59273(7) 0.95144(6) 0.04857(17) 0.0288(3) Uani d 1 . . O O5 0.24312(6) 0.55365(6) 0.76639(16) 0.0246(3) Uani d 1 . . N N1 0.50639(8) 0.69827(7) 0.50010(18) 0.0221(3) Uani d 1 . . N N2 0.49323(8) 0.63946(7) 0.5152(2) 0.0243(3) Uani d 1 . . H H2 0.5246(12) 0.6133(11) 0.488(3) 0.029 Uiso d 1 . . N N3 0.60948(8) 0.89818(7) 0.07922(18) 0.0230(3) Uani d 1 . . C C1 0.56661(9) 0.71660(8) 0.4425(2) 0.0210(3) Uani d 1 . . C C2 0.62303(9) 0.67454(8) 0.3949(2) 0.0220(4) Uani d 1 . . C C3 0.74375(10) 0.66734(9) 0.3324(3) 0.0317(4) Uani d 1 . . H H3A 0.7313 0.6450 0.2192 0.048 Uiso calc 1 . . H H3B 0.7554 0.6384 0.4314 0.048 Uiso calc 1 . . H H3C 0.7852 0.6935 0.3203 0.048 Uiso calc 1 . . C C4 0.57519(8) 0.78340(8) 0.4289(2) 0.0197(3) Uani d 1 . . C C5 0.59311(8) 0.80907(8) 0.2672(2) 0.0202(3) Uani d 1 . . H H5 0.6038 0.7840 0.1695 0.024 Uiso calc 1 . . C C6 0.59483(9) 0.87167(8) 0.2535(2) 0.0200(3) Uani d 1 . . C C7 0.58109(9) 0.91057(8) 0.3922(2) 0.0225(3) Uani d 1 . . H H7 0.5819 0.9535 0.3770 0.027 Uiso calc 1 . . C C8 0.56615(9) 0.88470(9) 0.5545(2) 0.0237(4) Uani d 1 . . H H8 0.5582 0.9100 0.6539 0.028 Uiso calc 1 . . C C9 0.56288(9) 0.82174(8) 0.5716(2) 0.0222(4) Uani d 1 . . H H9 0.5520 0.8046 0.6828 0.027 Uiso calc 1 . . C C10 0.42944(9) 0.61927(8) 0.5796(2) 0.0228(4) Uani d 1 . . C C11 0.42116(9) 0.55701(8) 0.6003(2) 0.0240(4) Uani d 1 . . H H11 0.4579 0.5302 0.5712 0.029 Uiso calc 1 . . C C12 0.35965(9) 0.53308(8) 0.6634(2) 0.0233(4) Uani d 1 . . H H12 0.3545 0.4904 0.6778 0.028 Uiso calc 1 . . C C13 0.30601(9) 0.57256(8) 0.7047(2) 0.0216(4) Uani d 1 . . C C14 0.31391(9) 0.63514(8) 0.6835(2) 0.0233(4) Uani d 1 . . H H14 0.2770 0.6619 0.7117 0.028 Uiso calc 1 . . C C15 0.37540(9) 0.65865(8) 0.6213(2) 0.0239(4) Uani d 1 . . H H15 0.3806 0.7014 0.6073 0.029 Uiso calc 1 . . C C16 0.23032(9) 0.48938(8) 0.7635(2) 0.0254(4) Uani d 1 . . H H16A 0.2302 0.4742 0.6395 0.038 Uiso calc 1 . . H H16B 0.1839 0.4811 0.8069 0.038 Uiso calc 1 . . H H16C 0.2681 0.4689 0.8423 0.038 Uiso calc 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 0.0297(7) 0.0239(7) 0.0277(6) -0.0003(5) 0.0043(5) -0.0002(5) O2 0.0191(6) 0.0262(7) 0.0357(7) 0.0005(5) 0.0057(5) 0.0010(5) O3 0.0396(7) 0.0329(7) 0.0196(6) -0.0022(6) 0.0088(5) -0.0013(5) O4 0.0310(7) 0.0246(7) 0.0305(6) -0.0009(6) 0.0024(5) 0.0085(5) O5 0.0221(6) 0.0250(6) 0.0278(6) -0.0020(5) 0.0071(5) 0.0003(5) N1 0.0231(7) 0.0240(7) 0.0189(6) -0.0025(6) 0.0002(5) 0.0034(6) N2 0.0242(7) 0.0233(8) 0.0256(7) -0.0026(6) 0.0041(6) 0.0028(6) N3 0.0229(7) 0.0258(8) 0.0201(7) -0.0039(6) 0.0015(5) 0.0028(6) C1 0.0212(7) 0.0249(9) 0.0165(7) -0.0010(7) 0.0005(6) 0.0026(6) C2 0.0226(8) 0.0255(9) 0.0176(7) -0.0024(7) 0.0013(6) 0.0015(6) C3 0.0231(9) 0.0322(10) 0.0405(10) 0.0045(8) 0.0059(8) -0.0002(8) C4 0.0169(7) 0.0236(9) 0.0182(7) -0.0012(6) -0.0005(6) 0.0021(6) C5 0.0189(7) 0.0256(9) 0.0160(7) -0.0002(7) 0.0018(6) -0.0014(6) C6 0.0184(7) 0.0245(9) 0.0168(7) -0.0023(6) 0.0012(6) 0.0023(6) C7 0.0208(7) 0.0213(8) 0.0252(8) -0.0010(7) 0.0020(6) -0.0022(7) C8 0.0214(8) 0.0299(9) 0.0199(8) 0.0008(7) 0.0035(6) -0.0034(7) C9 0.0189(7) 0.0303(9) 0.0178(7) -0.0004(7) 0.0032(6) 0.0024(7) C10 0.0238(8) 0.0267(9) 0.0178(7) -0.0045(7) 0.0005(6) 0.0011(7) C11 0.0226(8) 0.0241(9) 0.0256(8) 0.0004(7) 0.0046(6) 0.0000(7) C12 0.0247(8) 0.0217(9) 0.0235(8) -0.0019(7) 0.0029(6) 0.0005(7) C13 0.0219(8) 0.0261(9) 0.0168(7) -0.0038(7) 0.0018(6) 0.0005(6) C14 0.0240(8) 0.0253(9) 0.0206(8) 0.0007(7) 0.0019(6) -0.0015(7) C15 0.0267(8) 0.0229(9) 0.0216(8) -0.0016(7) 0.0006(6) 0.0014(7) C16 0.0255(8) 0.0262(9) 0.0248(8) -0.0041(7) 0.0040(7) 0.0034(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.1485 -1 0 -2 0.1392 1 1 -2 0.1371 -2 -1 0 0.0456 2 1 0 0.0513 -1 -2 0 0.0456 1 2 0 0.0475 0 -1 0 0.0420 0 1 0 0.0439 -1 2 0 0.0478 -1 1 2 0.1334 1 -1 -2 0.1430 0 1 -2 0.1376 1 -1 0 0.0573 -1 1 0 0.0439 2 -1 0 0.0533 -2 1 0 0.0401 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 O2 C3 . . 116.24(15) ? C13 O5 C16 . . 116.19(13) ? C1 N1 N2 . . 120.14(15) ? N1 N2 C10 . . 120.66(15) ? N1 N2 H2 . . 119.4(15) ? C10 N2 H2 . . 119.9(15) ? O4 N3 O3 . . 123.74(14) ? O4 N3 C6 . . 118.16(14) ? O3 N3 C6 . . 118.10(14) ? N1 C1 C2 . . 123.46(16) ? N1 C1 C4 . . 115.42(15) ? C2 C1 C4 . . 121.12(14) ? O1 C2 O2 . . 123.38(16) ? O1 C2 C1 . . 125.07(15) ? O2 C2 C1 . . 111.52(15) ? O2 C3 H3A . . 109.5 ? O2 C3 H3B . . 109.5 ? H3A C3 H3B . . 109.5 ? O2 C3 H3C . . 109.5 ? H3A C3 H3C . . 109.5 ? H3B C3 H3C . . 109.5 ? C9 C4 C5 . . 118.99(16) ? C9 C4 C1 . . 121.26(14) ? C5 C4 C1 . . 119.69(15) ? C6 C5 C4 . . 118.33(15) ? C6 C5 H5 . . 120.8 ? C4 C5 H5 . . 120.8 ? C5 C6 C7 . . 123.51(15) ? C5 C6 N3 . . 117.87(14) ? C7 C6 N3 . . 118.58(15) ? C6 C7 C8 . . 117.73(16) ? C6 C7 H7 . . 121.1 ? C8 C7 H7 . . 121.1 ? C7 C8 C9 . . 120.11(15) ? C7 C8 H8 . . 119.9 ? C9 C8 H8 . . 119.9 ? C8 C9 C4 . . 121.25(15) ? C8 C9 H9 . . 119.4 ? C4 C9 H9 . . 119.4 ? C11 C10 C15 . . 119.60(16) ? C11 C10 N2 . . 117.23(16) ? C15 C10 N2 . . 123.17(17) ? C10 C11 C12 . . 121.02(16) ? C10 C11 H11 . . 119.5 ? C12 C11 H11 . . 119.5 ? C13 C12 C11 . . 119.10(16) ? C13 C12 H12 . . 120.5 ? C11 C12 H12 . . 120.5 ? O5 C13 C12 . . 123.69(16) ? O5 C13 C14 . . 116.16(15) ? C12 C13 C14 . . 120.14(15) ? C15 C14 C13 . . 120.44(16) ? C15 C14 H14 . . 119.8 ? C13 C14 H14 . . 119.8 ? C14 C15 C10 . . 119.70(17) ? C14 C15 H15 . . 120.1 ? C10 C15 H15 . . 120.1 ? O5 C16 H16A . . 109.5 ? O5 C16 H16B . . 109.5 ? H16A C16 H16B . . 109.5 ? O5 C16 H16C . . 109.5 ? H16A C16 H16C . . 109.5 ? H16B C16 H16C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C2 . 1.218(2) ? O2 C2 . 1.344(2) ? O2 C3 . 1.447(2) ? O3 N3 . 1.2339(19) ? O4 N3 . 1.227(2) ? O5 C13 . 1.3774(19) ? O5 C16 . 1.432(2) ? N1 C1 . 1.316(2) ? N1 N2 . 1.322(2) ? N2 C10 . 1.410(2) ? N2 H2 . 0.86(2) ? N3 C6 . 1.472(2) ? C1 C2 . 1.478(2) ? C1 C4 . 1.481(2) ? C3 H3A . 0.9800 ? C3 H3B . 0.9800 ? C3 H3C . 0.9800 ? C4 C9 . 1.393(2) ? C4 C5 . 1.401(2) ? C5 C6 . 1.379(2) ? C5 H5 . 0.9500 ? C6 C7 . 1.385(2) ? C7 C8 . 1.388(2) ? C7 H7 . 0.9500 ? C8 C9 . 1.391(3) ? C8 H8 . 0.9500 ? C9 H9 . 0.9500 ? C10 C11 . 1.387(2) ? C10 C15 . 1.394(3) ? C11 C12 . 1.396(2) ? C11 H11 . 0.9500 ? C12 C13 . 1.389(2) ? C12 H12 . 0.9500 ? C13 C14 . 1.393(2) ? C14 C15 . 1.390(2) ? C14 H14 . 0.9500 ? C15 H15 . 0.9500 ? C16 H16A . 0.9800 ? C16 H16B . 0.9800 ? C16 H16C . 0.9800 ? 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 N2 H2 O1 . 0.86(2) 1.98(2) 2.657(2) 134(2) yes C7 H7 O4 6_576 0.95 2.44 3.245(2) 142 yes C12 H12 O1 5_666 0.95 2.52 3.401(2) 154 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C1 N1 N2 C10 . . . . 178.96(15) ? N2 N1 C1 C2 . . . . -1.1(2) ? N2 N1 C1 C4 . . . . 179.31(14) ? C3 O2 C2 O1 . . . . -0.9(2) ? C3 O2 C2 C1 . . . . 177.22(14) ? N1 C1 C2 O1 . . . . 9.1(3) ? C4 C1 C2 O1 . . . . -171.35(15) ? N1 C1 C2 O2 . . . . -169.00(15) ? C4 C1 C2 O2 . . . . 10.5(2) ? N1 C1 C4 C9 . . . . 49.2(2) ? C2 C1 C4 C9 . . . . -130.37(17) ? N1 C1 C4 C5 . . . . -128.10(16) ? C2 C1 C4 C5 . . . . 52.3(2) ? C9 C4 C5 C6 . . . . -2.7(2) ? C1 C4 C5 C6 . . . . 174.63(14) ? C4 C5 C6 C7 . . . . 1.3(2) ? C4 C5 C6 N3 . . . . -176.41(14) ? O4 N3 C6 C5 . . . . 160.87(15) ? O3 N3 C6 C5 . . . . -18.7(2) ? O4 N3 C6 C7 . . . . -16.9(2) ? O3 N3 C6 C7 . . . . 163.47(15) ? C5 C6 C7 C8 . . . . 1.2(3) ? N3 C6 C7 C8 . . . . 178.90(14) ? C6 C7 C8 C9 . . . . -2.2(2) ? C7 C8 C9 C4 . . . . 0.8(2) ? C5 C4 C9 C8 . . . . 1.8(2) ? C1 C4 C9 C8 . . . . -175.54(15) ? N1 N2 C10 C11 . . . . -176.81(14) ? N1 N2 C10 C15 . . . . 3.5(2) ? C15 C10 C11 C12 . . . . -0.4(3) ? N2 C10 C11 C12 . . . . 179.97(15) ? C10 C11 C12 C13 . . . . 0.3(3) ? C16 O5 C13 C12 . . . . -8.3(2) ? C16 O5 C13 C14 . . . . 171.31(14) ? C11 C12 C13 O5 . . . . 179.49(15) ? C11 C12 C13 C14 . . . . -0.1(2) ? O5 C13 C14 C15 . . . . -179.76(14) ? C12 C13 C14 C15 . . . . -0.1(2) ? C13 C14 C15 C10 . . . . 0.1(2) ? C11 C10 C15 C14 . . . . 0.1(2) ? N2 C10 C15 C14 . . . . 179.77(15) ?