#------------------------------------------------------------------------------ #$Date: 2022-06-08 03:18:06 +0100 (Wed, 08 Jun 2022) $ #$Revision: 275903 $ #$URL: svn://www.crystallography.net/cod/cif/2/24/41/2244109.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_2244109 loop_ _publ_author_name 'Naghiyev, Farid N.' 'Khrustalev, Victor N.' 'Safronenko, Marina G.' 'Akkurt, Mehmet' 'Khalilov, Ali N.' 'Bhattarai, Ajaya' 'Mamedov, \.Ibrahim G.' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of 2,2'-(phenylazanediyl)bis(1-phenylethan-1-one) ; _journal_coeditor_code TX2050 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first ; ; _journal_paper_doi 10.1107/S2056989022005382 _journal_volume 78 _journal_year 2022 _chemical_formula_iupac 'C22 H19 N O2' _chemical_formula_moiety 'C22 H19 N O2' _chemical_formula_sum 'C22 H19 N O2' _chemical_formula_weight 329.38 _chemical_name_systematic ; 2,2'-(Phenylazanediyl)bis(1-phenylethan-1-one) ; _space_group_crystal_system orthorhombic _space_group_IT_number 60 _space_group_name_Hall '-P 2n 2ab' _space_group_name_H-M_alt 'P b c n' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 20.8269(2) _cell_length_b 9.09843(10) _cell_length_c 9.01580(10) _cell_measurement_reflns_used 14002 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 78.99 _cell_measurement_theta_min 4.25 _cell_volume 1708.42(3) _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 ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014/5 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\f and \w' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_unetI/netI 0.0158 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 21247 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 79.366 _diffrn_reflns_theta_min 4.246 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.649 _exptl_absorpt_correction_T_max 0.939 _exptl_absorpt_correction_T_min 0.906 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2021) ; _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 1.281 _exptl_crystal_description prism _exptl_crystal_F_000 696 _exptl_crystal_size_max 0.090 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.285 _refine_diff_density_min -0.232 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 115 _refine_ls_number_reflns 1834 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.089 _refine_ls_R_factor_all 0.0517 _refine_ls_R_factor_gt 0.0505 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0811P)^2^+0.6375P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1407 _refine_ls_wR_factor_ref 0.1418 _reflns_number_gt 1746 _reflns_number_total 1834 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file tx2050sup1.cif _cod_data_source_block I _cod_database_code 2244109 _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 0.944 _shelx_estimated_absorpt_t_max 0.968 _shelx_hkl_file ; 0 0 1 0.06 0.28 0 0 2 9999.00 250.65 0 0 3 0.18 0.60 0 0 4 407.87 10.90 0 0 5 0.20 0.80 0 0 5 0.14 0.36 0 0 6 1981.52 48.35 0 0 6 1865.39 47.43 0 0 7 -0.01 0.53 0 0 7 0.26 0.41 0 0 7 -0.16 0.45 0 0 7 -0.18 0.50 0 0 7 0.17 0.84 0 0 7 0.17 0.52 0 0 8 194.90 5.13 0 0 8 196.86 5.11 0 0 8 179.09 5.07 0 0 8 195.21 5.12 0 0 8 191.71 5.15 0 0 9 0.09 0.58 0 0 9 -0.12 0.53 0 0 9 0.20 0.47 0 0 9 0.55 0.62 0 0 9 -0.10 0.43 0 0 10 1135.19 29.19 0 0 10 1175.86 29.15 0 -1 1 1.01 0.37 0 -1 1 -0.08 0.32 0 1 1 0.44 0.30 0 -1 2 2.36 0.72 0 1 2 2.67 0.67 0 1 3 19.49 1.03 0 -1 3 18.33 1.06 0 -1 4 0.84 0.75 0 1 4 0.51 0.71 0 -1 4 0.47 0.87 0 -1 5 0.08 0.80 0 1 5 0.55 0.77 0 1 5 0.16 0.36 0 -1 5 0.45 0.36 0 1 6 -0.09 0.40 0 -1 6 0.11 0.41 0 -1 6 0.06 0.40 0 -1 6 -0.55 0.82 0 1 6 0.28 0.78 0 1 6 -0.06 0.46 0 -1 6 0.18 0.41 0 -1 7 -0.03 0.43 0 1 7 0.19 0.41 0 -1 7 0.03 0.45 0 1 7 -0.08 0.56 0 -1 7 0.42 0.52 0 -1 7 -0.08 0.41 0 1 7 0.05 0.80 0 -1 7 -0.17 0.80 0 -1 7 0.10 0.52 0 1 7 0.45 0.54 0 -1 7 0.02 0.39 0 -1 7 -0.14 0.49 0 -1 8 1.17 0.48 0 1 8 0.76 0.64 0 -1 8 0.77 0.65 0 1 8 1.50 0.52 0 -1 8 1.60 0.55 0 1 8 1.71 0.62 0 -1 8 1.77 0.64 0 -1 8 0.90 0.59 0 1 8 0.98 0.59 0 -1 9 13.27 0.77 0 1 9 15.12 0.86 0 -1 9 14.78 0.87 0 1 9 17.24 0.78 0 1 9 16.54 0.85 0 -1 9 16.50 0.88 0 -1 9 14.53 0.79 0 1 9 13.15 0.84 0 -1 9 11.40 0.71 0 -1 10 -0.21 0.42 0 -1 10 0.18 0.40 0 1 10 0.19 0.29 0 1 10 0.58 0.46 0 -1 10 -0.08 0.51 0 1 10 -0.01 0.48 0 1 10 -0.01 0.42 0 -1 11 -0.09 0.21 0 1 11 -0.06 0.25 0 -1 11 0.00 0.25 0 -2 1 2716.21 70.12 0 2 1 2786.75 70.12 0 -2 1 2956.83 70.23 0 -2 2 46.69 1.54 0 2 2 47.72 1.52 0 -2 2 47.51 1.66 0 -2 3 394.65 10.71 0 2 3 414.85 10.57 0 -2 3 401.96 10.58 0 -2 3 396.34 10.77 0 2 4 5.69 0.77 0 -2 4 3.96 0.77 0 -2 4 4.97 1.01 0 2 4 4.28 0.36 0 -2 5 626.90 15.90 0 2 5 591.57 14.89 0 -2 5 570.82 14.89 0 -2 5 589.00 15.58 0 2 5 612.43 15.56 0 -2 6 154.11 4.40 0 2 6 174.34 4.48 0 -2 6 155.26 4.39 0 -2 6 154.12 4.34 0 2 6 172.08 4.42 0 -2 6 156.99 4.36 0 2 6 169.42 4.37 0 -2 6 164.12 4.38 0 2 6 179.05 5.15 0 2 6 167.03 4.37 0 -2 6 173.70 5.19 0 -2 6 164.73 4.37 0 2 6 177.53 4.38 0 -2 7 14.44 0.85 0 -2 7 15.42 0.77 0 -2 7 15.96 0.74 0 -2 7 15.58 0.80 0 2 7 17.11 0.89 0 -2 7 15.23 0.78 0 2 7 15.50 0.74 0 2 7 14.59 0.71 0 -2 7 15.78 0.82 0 2 7 16.19 1.28 0 -2 7 17.08 0.84 0 2 7 16.82 0.82 0 -2 7 14.26 1.30 0 -2 7 16.55 0.82 0 -2 7 15.53 0.76 0 2 7 17.54 0.75 0 2 7 19.00 0.78 0 -2 8 12.13 0.70 0 -2 8 12.21 0.67 0 -2 8 11.73 0.78 0 2 8 13.56 0.66 0 2 8 11.50 0.80 0 2 8 10.08 0.56 0 2 8 11.99 0.79 0 -2 8 10.58 0.66 0 -2 8 11.58 0.78 0 2 8 11.85 0.77 0 -2 8 10.05 0.75 0 -2 8 10.51 0.66 0 -2 9 39.50 1.33 0 2 9 41.64 1.44 0 -2 9 42.94 1.39 0 -2 9 41.71 1.35 0 2 9 42.79 1.44 0 -2 9 43.85 1.42 0 -2 9 43.50 1.36 0 2 10 22.59 0.80 0 -2 10 20.12 0.76 0 -2 10 20.80 0.78 0 2 10 21.14 0.85 0 -2 10 21.38 0.85 0 2 10 22.30 0.83 0 -2 10 21.82 0.79 0 -2 11 89.10 2.25 0 2 11 93.32 2.26 0 -3 0 0.04 0.48 0 -3 1 0.28 0.60 0 -3 1 0.08 0.51 0 -3 2 0.88 0.74 0 -3 2 0.56 0.37 0 -3 2 1.80 0.72 0 3 2 0.65 0.35 0 -3 3 8.88 0.72 0 3 3 9.49 0.71 0 -3 3 11.37 1.06 0 -3 4 0.10 0.92 0 3 4 0.42 0.26 0 -3 4 0.48 0.27 0 -3 4 -0.17 0.97 0 3 4 0.11 0.57 0 -3 4 0.06 0.57 0 -3 5 -0.18 1.02 0 -3 5 -0.22 0.62 0 3 5 0.04 0.61 0 3 5 0.10 0.33 0 -3 5 0.21 0.33 0 -3 6 0.09 0.58 0 -3 6 0.05 0.46 0 -3 6 0.18 0.48 0 -3 6 -0.14 0.47 0 -3 6 0.33 0.52 0 -3 6 -0.14 0.43 0 3 6 0.21 0.41 0 3 6 0.28 0.33 0 -3 6 0.54 0.34 0 -3 6 -0.09 0.38 0 3 6 0.06 0.47 0 -3 6 0.02 0.57 0 -3 6 0.15 0.36 0 3 6 0.02 0.43 0 -3 6 0.03 0.43 0 3 6 0.34 0.57 0 -3 6 0.28 0.50 0 3 6 0.82 0.66 0 -3 6 0.45 0.70 0 3 7 0.45 0.38 0 -3 7 0.14 0.39 0 -3 7 0.34 0.44 0 -3 7 0.03 0.69 0 3 7 0.16 0.62 0 -3 7 -0.17 0.57 0 -3 7 0.01 0.50 0 3 7 0.11 0.40 0 3 7 0.01 0.44 0 -3 7 -0.27 0.53 0 3 7 0.16 0.51 0 -3 7 0.93 0.77 0 -3 7 0.25 0.54 0 3 8 0.66 0.57 0 -3 8 0.31 0.56 0 -3 8 1.20 0.57 0 -3 8 0.33 0.38 0 -3 8 0.70 0.55 0 -3 -8 0.51 0.39 0 -3 8 -0.01 0.43 0 -3 8 0.19 0.47 0 -3 8 0.31 0.74 0 -3 8 0.33 0.60 0 3 8 0.69 0.41 0 -3 8 0.71 0.43 0 3 8 0.70 0.43 0 -3 8 0.79 0.63 0 3 8 0.56 0.64 0 -3 9 4.38 0.68 0 -3 9 4.27 0.51 0 3 9 4.21 0.64 0 -3 9 4.28 0.46 0 3 9 4.14 0.59 0 -3 9 4.84 0.58 0 -3 9 4.27 0.63 0 -3 10 -0.06 0.46 0 3 10 0.10 0.36 0 3 10 -0.07 0.33 0 -3 10 -0.20 0.36 0 -3 10 -0.15 0.40 0 -3 10 0.51 0.50 0 3 10 0.27 0.41 0 3 11 0.05 0.13 0 -4 0 121.45 3.75 0 -4 0 134.91 3.71 0 -4 1 3274.09 82.37 0 -4 1 3255.80 82.21 0 -4 2 7.91 0.98 0 -4 2 8.01 0.90 0 -4 3 29.30 1.68 0 -4 3 27.15 1.52 0 -4 4 159.74 5.06 0 4 4 165.50 4.58 0 -4 4 154.54 4.56 0 -4 5 124.58 3.46 0 -4 5 130.82 4.42 0 -4 5 122.78 3.40 0 -4 5 122.11 3.29 0 -4 5 132.25 3.47 0 -4 5 123.02 3.35 0 -4 5 122.39 3.30 0 4 5 132.43 3.48 0 -4 5 122.15 3.40 0 -4 5 126.39 3.43 0 -4 5 122.67 3.32 0 -4 5 143.15 4.71 0 -4 5 120.76 3.35 0 -4 5 122.81 3.42 0 4 5 124.95 3.42 0 4 5 127.85 3.30 0 -4 5 121.04 3.29 0 -4 6 0.07 0.36 0 -4 6 0.05 0.55 0 -4 6 -0.28 0.47 0 -4 6 0.73 0.49 0 -4 6 0.52 0.61 0 -4 6 0.17 0.75 0 -4 6 -0.33 0.57 0 -4 6 -0.25 0.50 0 -4 6 -0.05 0.53 0 -4 6 -0.08 0.53 0 -4 6 0.49 0.34 0 4 6 0.38 0.54 0 -4 6 0.54 0.41 0 -4 6 0.43 0.41 0 -4 6 -0.20 0.76 0 -4 6 -0.20 0.58 0 4 6 0.49 0.44 0 -4 6 0.42 0.44 0 4 6 0.70 0.43 0 -4 7 6.49 0.57 0 4 7 6.80 0.56 0 -4 7 7.41 0.60 0 -4 7 6.34 0.72 0 -4 7 6.33 0.71 0 -4 7 6.71 0.93 0 -4 7 5.69 0.62 0 -4 7 4.98 0.63 0 -4 -7 6.32 0.56 0 -4 7 6.63 0.55 0 4 7 7.51 0.70 0 -4 7 6.24 0.89 0 4 7 6.00 0.60 0 4 7 6.33 0.54 0 -4 7 6.66 0.47 0 -4 7 6.60 0.63 0 -4 7 7.25 0.73 0 4 7 6.86 0.45 0 -4 7 5.69 0.45 0 4 7 7.30 0.79 0 -4 8 59.15 1.72 0 -4 8 58.22 1.81 0 -4 8 52.37 1.82 0 -4 8 54.90 1.64 0 4 8 58.22 1.85 0 4 8 54.07 1.69 0 4 8 52.20 1.66 0 -4 8 50.90 1.67 0 -4 8 56.22 1.64 0 -4 -8 55.91 1.64 0 -4 8 60.76 1.76 0 -4 9 113.66 3.00 0 4 9 109.26 3.09 0 4 9 116.27 3.08 0 -4 9 113.77 2.97 0 -4 9 111.29 3.06 0 -4 -9 104.57 2.91 0 4 10 23.63 0.72 0 4 10 23.79 0.76 0 -4 10 24.22 0.82 0 -4 10 21.68 0.75 0 4 10 24.56 0.75 0 -5 0 0.23 0.70 0 -5 0 0.11 0.72 0 -5 1 0.65 0.79 0 -5 -1 0.24 0.83 0 -5 1 -0.74 0.74 0 -5 2 0.78 0.88 0 -5 2 0.85 0.85 0 -5 3 24.06 1.66 0 -5 3 20.86 1.50 0 -5 4 -0.32 0.61 0 -5 4 0.50 1.06 0 -5 4 -0.19 0.49 0 -5 4 -0.84 1.06 0 -5 4 0.11 0.45 0 -5 -4 0.25 0.39 0 5 4 0.13 0.50 0 -5 4 -0.19 0.74 0 5 4 0.25 0.44 0 -5 4 -0.09 0.36 0 -5 4 0.23 0.46 0 -5 4 -0.14 0.57 0 -5 4 0.16 0.55 0 -5 4 0.01 0.44 0 -5 5 -0.02 0.55 0 -5 5 0.63 1.09 0 -5 5 0.25 0.58 0 -5 5 0.28 0.45 0 -5 5 -0.29 0.55 0 -5 -5 -0.20 0.47 0 -5 5 -0.20 0.45 0 -5 5 0.49 0.42 0 -5 5 -0.11 0.66 0 -5 5 0.19 0.51 0 -5 5 0.02 0.53 0 -5 5 0.41 0.62 0 -5 6 0.49 0.78 0 -5 6 0.07 0.91 0 -5 6 0.77 0.56 0 -5 6 0.57 0.65 0 -5 6 0.44 0.52 0 -5 6 0.80 0.64 0 -5 -6 0.35 0.50 0 -5 6 0.39 0.49 0 5 6 -0.39 0.59 0 -5 6 0.74 0.97 0 -5 6 0.54 0.45 0 5 6 0.37 0.53 0 -5 6 -0.28 0.72 0 -5 6 1.00 0.66 0 -5 6 0.71 0.57 0 -5 7 0.04 0.79 0 -5 7 -0.55 0.98 0 -5 7 0.15 0.52 0 -5 7 -0.33 0.60 0 -5 -7 0.08 0.47 0 -5 7 0.19 0.49 0 5 7 -0.29 0.59 0 -5 7 0.11 0.96 0 5 7 0.33 0.51 0 -5 7 0.48 0.54 0 -5 7 0.59 0.63 0 -5 7 0.17 0.62 0 5 7 -0.26 0.68 0 -5 7 -0.63 0.72 0 -5 7 -0.67 0.64 0 -5 8 1.36 0.64 0 -5 8 1.73 0.60 0 -5 8 0.80 0.51 0 -5 8 -0.25 0.91 0 5 8 1.18 0.66 0 -5 8 1.03 0.74 0 -5 -8 0.98 0.44 0 5 8 1.41 0.49 0 5 8 1.53 0.47 0 -5 8 1.24 0.77 0 5 9 0.46 0.48 0 -5 9 1.25 0.63 0 -5 9 0.82 0.61 0 5 9 1.63 0.43 0 -5 9 1.35 0.48 0 -5 -9 1.68 0.30 0 5 10 -0.15 0.21 0 5 10 -0.11 0.15 0 -6 0 3619.35 88.04 0 -6 0 3337.87 88.10 0 -6 -1 101.78 3.20 0 -6 1 95.51 3.23 0 -6 -1 82.17 3.02 0 -6 1 88.07 3.30 0 -6 -2 1.10 0.37 0 -6 -2 0.46 0.92 0 -6 2 -0.15 0.89 0 -6 2 0.54 0.78 0 -6 -2 0.57 0.62 0 -6 2 -0.18 0.94 0 -6 2 0.21 0.42 0 -6 2 0.77 0.43 0 -6 2 -0.08 0.47 0 -6 2 0.31 0.47 0 -6 3 8.08 0.62 0 -6 -3 8.60 0.57 0 -6 3 8.10 0.63 0 -6 3 8.69 1.26 0 -6 3 8.10 0.66 0 -6 -3 7.83 0.55 0 -6 3 8.17 0.96 0 -6 3 7.51 0.57 0 -6 3 7.75 0.87 0 6 3 8.65 0.61 0 -6 3 7.16 1.30 0 -6 3 8.10 0.77 0 -6 3 8.29 0.60 0 -6 3 7.49 0.48 0 -6 3 7.60 0.61 0 -6 4 543.03 14.24 0 -6 4 571.67 15.53 0 -6 4 576.11 14.32 0 -6 4 572.89 14.28 0 -6 4 605.12 15.86 0 -6 4 544.60 14.14 0 6 4 563.60 14.33 0 -6 4 584.92 14.28 0 -6 4 533.22 14.25 0 6 4 570.68 14.30 0 -6 4 537.02 14.28 0 -6 4 551.28 14.18 0 -6 4 562.83 14.33 0 -6 5 655.59 16.65 0 -6 5 659.55 18.32 0 -6 5 665.99 16.85 0 -6 5 675.93 16.79 0 -6 5 662.46 16.82 0 -6 5 642.87 18.08 0 -6 5 651.03 16.79 0 -6 -5 663.46 16.71 0 6 5 667.47 16.83 0 -6 5 645.09 16.64 0 -6 5 614.43 16.72 0 -6 5 655.67 16.79 0 -6 5 645.70 16.66 0 -6 5 662.82 16.80 0 -6 5 684.53 16.72 0 -6 6 1187.09 30.08 0 -6 6 1174.12 29.95 0 -6 6 1264.55 30.15 0 -6 6 1191.27 30.14 0 -6 -6 1207.69 30.01 0 -6 6 1199.72 29.94 0 -6 6 1133.22 30.00 0 -6 6 1198.59 30.09 0 6 6 1133.37 30.06 0 -6 6 1196.00 30.10 0 -6 6 1167.89 29.95 0 -6 6 1229.24 30.02 0 -6 7 12.71 0.87 0 -6 7 11.06 0.80 0 -6 7 12.16 0.96 0 -6 -7 12.50 0.70 0 6 7 13.03 0.91 0 -6 7 12.22 0.73 0 6 7 11.45 0.71 0 -6 7 12.21 0.71 0 -6 7 11.67 1.16 0 6 7 12.43 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2 4.86 0.47 -23 3 2 5.39 0.48 23 3 2 4.00 0.40 -23 -3 2 4.24 0.45 23 -3 -2 5.13 0.58 23 -3 2 5.75 0.56 23 -3 2 3.88 0.61 -23 3 2 3.14 0.37 -23 3 -2 3.64 0.35 23 3 -2 4.50 0.43 23 3 2 4.06 0.44 -23 -3 -3 0.49 0.31 -23 3 -3 0.71 0.29 23 -3 3 0.14 0.42 23 -3 -3 0.53 0.47 23 3 3 0.67 0.32 -23 -3 3 0.74 0.36 -23 -3 -3 0.39 0.39 23 -3 3 0.83 0.45 -23 -3 3 0.72 0.36 23 3 -3 0.90 0.33 -23 -3 4 7.00 0.40 23 -3 4 5.98 0.38 23 -3 -4 6.80 0.45 23 -3 4 7.54 0.43 -23 -3 4 7.96 0.40 -23 -3 -4 8.33 0.41 23 -4 0 -0.13 0.48 23 -4 0 0.74 0.54 -23 -4 0 0.21 0.44 -23 4 0 -0.02 0.45 -23 -4 -1 -0.18 0.35 23 -4 1 -0.29 0.44 -23 -4 1 0.13 0.29 -23 -4 -1 -0.14 0.41 -23 -4 1 0.38 0.41 -23 4 -1 0.19 0.42 -23 4 1 0.22 0.40 -23 -4 -2 17.42 0.64 -23 -4 2 15.68 0.63 -23 4 -2 18.88 0.63 -23 4 2 16.70 0.62 23 -4 2 16.12 0.72 -23 -4 -2 17.67 0.64 23 -4 2 16.44 0.73 -23 -4 2 15.57 0.59 23 -4 3 7.18 0.47 -23 -4 3 8.27 0.41 23 4 3 7.52 0.44 23 -4 3 7.18 0.47 -23 -4 -4 0.25 0.19 23 -4 4 0.03 0.21 -23 -4 4 0.64 0.20 23 -5 0 0.76 0.32 23 -5 0 1.07 0.35 -23 -5 0 1.62 0.35 -23 5 0 1.43 0.34 23 -5 1 2.61 0.36 23 -5 -1 2.20 0.34 -23 -5 1 2.85 0.34 -23 5 -1 3.08 0.34 -23 5 1 2.98 0.33 -23 -5 -1 3.01 0.34 23 -5 2 30.92 0.89 -23 -5 2 27.27 0.86 23 -5 -2 29.78 0.87 23 5 2 28.90 0.88 -23 -5 -2 29.78 0.85 -23 5 -2 27.65 0.82 24 0 0 114.60 3.01 -24 0 0 109.77 2.95 -24 0 0 117.81 3.00 -24 0 -1 0.31 0.38 24 0 1 -0.14 0.53 24 0 -1 -0.24 0.56 -24 0 -1 0.10 0.46 -24 0 1 -0.11 0.47 24 0 1 0.21 0.50 24 0 1 0.04 0.33 24 0 -1 -0.29 0.36 -24 0 1 0.07 0.37 24 0 2 90.68 2.29 24 0 -2 88.93 2.30 -24 0 -2 86.73 2.24 -24 0 2 83.25 2.23 24 0 2 86.15 2.29 -24 0 2 77.79 2.22 -24 0 -2 83.52 2.23 24 0 -2 74.23 2.16 -24 0 -3 -0.18 0.31 24 0 -3 -0.23 0.52 -24 0 3 -0.20 0.42 -24 0 -3 -0.18 0.29 24 0 3 -0.10 0.42 24 0 -3 0.03 0.28 24 0 3 0.18 0.41 -24 0 3 0.16 0.31 24 0 4 12.28 0.53 24 0 -4 12.80 0.59 24 0 4 12.08 0.53 -24 0 -4 11.05 0.45 -24 -1 0 -0.21 0.47 -24 1 0 0.40 0.49 24 1 0 0.18 0.52 24 -1 0 0.34 0.52 24 -1 0 -0.01 0.41 -24 1 0 -0.05 0.36 -24 -1 0 0.43 0.36 -24 1 -1 19.20 0.78 -24 1 1 17.93 0.77 -24 -1 -1 18.67 0.76 -24 -1 1 17.55 0.76 -24 1 1 13.60 0.67 -24 -1 1 16.45 0.69 -24 1 -1 16.89 0.69 -24 -1 -1 15.70 0.69 24 -1 1 16.61 0.72 24 -1 -1 16.29 0.74 24 1 1 17.88 0.80 24 -1 1 18.30 0.80 24 1 -1 17.82 0.81 24 -1 -1 17.86 0.82 24 1 1 15.69 0.76 -24 1 -2 56.65 1.55 -24 1 2 53.86 1.54 -24 -1 -2 53.93 1.54 -24 -1 2 52.74 1.53 -24 1 2 47.82 1.52 -24 -1 2 47.72 1.53 -24 1 -2 51.73 1.52 -24 -1 -2 53.93 1.53 24 -1 2 50.59 1.58 -24 -1 2 49.40 1.57 24 -1 -2 49.16 1.53 24 -1 2 50.11 1.51 24 1 2 55.02 1.58 24 -1 2 54.87 1.59 24 1 2 56.32 1.59 24 1 -2 53.55 1.60 24 -1 -2 54.53 1.59 24 1 3 89.86 2.42 -24 -1 3 78.12 2.38 -24 1 3 75.82 2.36 24 -1 3 78.30 2.33 24 -1 -3 98.54 2.38 24 1 -3 107.21 2.44 24 -1 -3 95.18 2.42 24 -1 3 95.95 2.43 24 1 3 99.91 2.43 -24 -1 3 90.65 2.42 -24 1 3 86.69 2.37 -24 1 -3 96.79 2.38 -24 -1 3 90.97 2.39 -24 -1 -3 84.89 2.37 24 -1 3 66.45 2.31 -24 -1 -3 96.88 2.39 -24 -1 -3 89.54 2.33 -24 1 -3 86.54 2.32 -24 -1 4 0.67 0.31 -24 1 4 0.49 0.27 -24 -1 -4 1.19 0.26 -24 1 -4 0.68 0.21 24 -1 4 1.22 0.30 24 1 4 0.61 0.31 24 -1 -4 1.20 0.26 24 1 -4 0.70 0.38 24 -1 -4 0.54 0.35 24 -2 0 11.00 0.63 -24 2 0 8.41 0.50 -24 -2 0 8.99 0.51 24 2 0 11.10 0.62 24 -2 0 10.38 0.61 -24 -2 0 8.72 0.49 -24 -2 0 10.26 0.52 -24 2 0 13.37 0.66 -24 -2 0 11.01 0.62 24 2 0 9.88 0.53 24 2 1 12.84 0.63 24 2 -1 13.94 0.59 24 -2 1 15.05 0.69 -24 -2 -1 14.63 0.64 -24 -2 1 15.24 0.54 -24 -2 -1 14.38 0.68 -24 -2 1 16.72 0.69 -24 2 -1 16.15 0.70 -24 2 1 17.47 0.70 -24 2 1 14.40 0.59 -24 -2 1 13.61 0.60 -24 2 -1 11.27 0.58 -24 -2 -1 11.50 0.58 -24 -2 1 14.89 0.64 24 -2 1 14.38 0.71 24 -2 -1 17.59 0.71 24 -2 1 14.24 0.68 24 2 1 13.21 0.67 24 2 -1 16.21 0.71 24 -2 -1 16.66 0.68 -24 -2 2 15.91 0.57 24 2 -2 13.99 0.66 24 -2 -2 14.53 0.63 24 -2 2 15.12 0.63 24 2 2 13.94 0.64 -24 2 -2 16.35 0.63 -24 -2 -2 14.91 0.62 -24 -2 2 15.94 0.62 -24 2 2 15.97 0.62 -24 2 2 13.64 0.57 -24 -2 2 13.02 0.57 -24 2 -2 11.25 0.56 -24 -2 -2 11.29 0.56 -24 -2 2 13.70 0.63 24 -2 -2 14.71 0.67 24 -2 2 13.07 0.64 24 -2 2 13.19 0.70 24 2 2 13.47 0.61 24 -2 2 14.28 0.67 24 2 -2 12.70 0.52 24 2 3 84.93 2.34 24 -2 3 89.12 2.37 -24 -2 -3 98.21 2.36 -24 2 -3 75.82 2.27 -24 -2 -3 79.06 2.28 -24 -2 3 91.42 2.37 24 -2 3 72.76 2.33 24 2 -3 97.43 2.35 24 2 3 91.34 2.35 -24 -2 3 97.83 2.33 24 -2 3 91.98 2.35 24 -2 -3 96.47 2.38 -24 -2 4 36.95 0.93 24 -2 -4 34.81 0.94 -24 -2 4 33.71 0.95 -24 -2 -4 34.25 0.92 24 3 0 0.17 0.31 -24 -3 0 -0.10 0.40 -24 3 0 0.04 0.43 24 -3 0 0.54 0.43 24 -3 1 2.78 0.45 24 -3 -1 3.32 0.46 -24 -3 1 1.44 0.26 -24 -3 -1 2.58 0.37 24 3 -1 2.47 0.33 24 -3 1 2.64 0.53 -24 -3 -1 2.53 0.42 -24 -3 1 3.00 0.40 -24 3 -1 3.21 0.42 -24 3 1 2.83 0.42 24 3 1 2.37 0.33 -24 -3 -2 1.94 0.34 -24 3 -2 2.30 0.34 -24 3 2 1.51 0.33 24 -3 2 1.20 0.39 24 -3 -2 1.63 0.40 24 3 2 1.39 0.27 -24 -3 2 1.24 0.28 -24 -3 -2 1.85 0.35 24 -3 2 1.91 0.42 24 3 -2 1.31 0.27 -24 -3 2 1.88 0.29 24 3 3 20.48 0.71 -24 -3 3 18.81 0.68 24 -3 3 17.58 0.72 -24 -3 3 25.26 0.70 -24 -3 -3 25.44 0.73 24 -3 3 24.40 0.75 24 -3 -3 26.78 0.76 24 -4 0 -0.11 0.34 24 -4 0 0.28 0.37 -24 -4 0 -0.09 0.33 -24 4 0 0.06 0.34 24 -4 1 133.42 3.48 24 -4 -1 140.81 3.48 -24 -4 -1 139.47 3.47 -24 -4 1 139.94 3.46 -24 4 -1 147.26 3.47 -24 4 1 144.44 3.46 -24 4 -2 19.21 0.59 -24 -4 -2 20.49 0.62 24 -4 2 21.36 0.68 25 0 0 -0.15 0.42 -25 0 0 0.17 0.30 25 0 0 -0.50 0.44 -25 0 0 0.26 0.38 25 0 1 0.07 0.38 -25 0 -1 -0.33 0.37 -25 0 1 0.15 0.36 -25 0 -1 0.20 0.29 -25 0 1 -0.05 0.31 25 0 1 -0.58 0.42 25 0 -1 -0.02 0.46 25 0 2 19.48 0.62 -25 0 -2 16.23 0.54 25 0 2 18.62 0.64 25 0 3 -0.11 0.29 25 0 -3 0.35 0.34 25 0 3 0.37 0.30 -25 0 3 0.11 0.28 -25 0 -3 -0.07 0.25 25 1 0 46.99 1.41 -25 1 0 57.97 1.46 -25 -1 0 54.46 1.44 -25 1 0 44.27 1.37 -25 -1 0 45.56 1.38 25 -1 0 44.84 1.36 -25 -1 0 41.39 1.35 25 1 0 53.31 1.45 25 -1 0 52.59 1.44 25 -1 1 0.81 0.39 25 1 1 0.64 0.39 25 1 -1 1.37 0.44 25 -1 -1 1.54 0.44 -25 -1 -1 1.31 0.36 -25 -1 1 1.35 0.36 -25 1 -1 1.43 0.38 -25 1 1 1.34 0.37 -25 -1 1 1.24 0.35 25 1 1 1.08 0.35 25 1 -1 1.18 0.34 25 -1 1 0.90 0.29 25 -1 -1 1.40 0.33 25 -1 2 1.64 0.35 25 1 2 1.72 0.35 -25 -1 2 1.67 0.24 25 1 2 1.50 0.35 25 -1 -2 1.89 0.29 25 1 -2 1.50 0.40 25 -1 -2 1.50 0.41 -25 -1 -2 1.55 0.31 -25 1 -2 1.75 0.31 -25 -1 2 1.49 0.34 25 -1 2 0.92 0.29 -25 -1 3 1.86 0.22 25 1 -3 2.09 0.32 25 -1 -3 2.04 0.31 -25 -1 -3 2.61 0.28 25 1 3 2.20 0.28 25 -1 3 1.91 0.29 25 -1 3 2.13 0.29 25 1 3 1.83 0.28 -25 -1 3 1.74 0.28 25 2 0 -0.01 0.24 25 -2 0 0.01 0.33 25 -2 0 0.12 0.34 -25 -2 0 0.11 0.34 -25 2 0 0.18 0.37 25 2 0 0.37 0.35 25 2 1 1.56 0.34 25 2 -1 1.83 0.34 -25 -2 1 0.97 0.24 -25 -2 -1 2.16 0.31 25 2 1 1.18 0.27 25 -2 1 1.86 0.34 25 -2 1 1.76 0.34 25 -2 -1 2.13 0.36 25 -2 1 1.12 0.42 -25 -2 -1 1.77 0.35 -25 -2 1 1.50 0.34 -25 2 -1 2.27 0.36 -25 2 1 2.09 0.35 25 2 2 0.43 0.26 -25 -2 2 0.36 0.24 25 2 2 0.49 0.22 25 -2 2 0.26 0.28 25 -2 2 0.24 0.25 25 -2 -2 0.48 0.29 -25 -2 -2 0.57 0.26 -25 2 -2 0.34 0.25 25 2 -2 -0.15 0.28 25 -2 2 0.26 0.28 -25 -2 3 0.00 0.18 -25 2 3 0.19 0.19 -25 -2 -3 0.21 0.21 -25 -3 0 31.83 0.89 -25 3 0 32.47 0.89 -25 -3 -1 31.55 0.91 -25 -3 1 32.26 0.91 -25 3 -1 33.10 0.91 -25 3 1 34.77 0.91 25 -3 1 29.80 0.92 25 -3 -1 28.02 0.92 -25 -3 -2 36.34 0.85 25 -3 2 24.91 0.84 25 -3 2 33.18 0.86 25 -3 -2 36.85 0.88 26 0 0 73.43 1.84 26 0 0 73.92 1.85 26 0 1 -0.11 0.25 26 0 -1 0.04 0.25 -26 0 -1 0.03 0.25 -26 0 1 -0.27 0.25 -26 0 1 0.07 0.24 26 0 1 -0.12 0.28 26 0 -1 0.15 0.28 26 0 2 60.82 1.62 -26 0 -2 63.36 1.60 26 0 -2 65.05 1.62 26 1 0 0.04 0.21 26 -1 0 0.08 0.27 -26 -1 0 0.16 0.27 -26 1 0 0.06 0.27 26 -1 0 0.17 0.27 26 1 0 0.03 0.27 26 -1 0 0.23 0.29 -26 -1 -1 8.27 0.36 -26 -1 1 8.31 0.36 -26 1 -1 8.41 0.36 -26 1 1 8.59 0.36 -26 -1 -1 7.50 0.34 26 1 -1 7.60 0.38 26 -1 -1 7.09 0.37 26 -1 1 6.21 0.36 26 1 1 6.47 0.37 26 1 1 5.61 0.33 26 -1 -1 7.60 0.39 -26 1 2 6.11 0.31 26 -1 -2 6.76 0.31 -26 1 -2 6.97 0.29 -26 2 0 58.85 1.28 -26 -2 0 57.90 1.28 26 -2 -1 4.26 0.29 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 29273 _shelx_res_file ; TITL T-251 in Pbcn shelx.res created by SHELXL-2018/3 at 17:24:00 on 14-May-2022 CELL 1.54184 20.8269 9.09843 9.01580 90.000 90.000 90.000 ZERR 4.00 0.0002 0.00010 0.00009 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, 0.5-Y, 0.5+Z SYMM -X, +Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O UNIT 88 76 4 8 TEMP -173.0 SIZE 0.05 0.06 0.09 OMIT 8 1 3 OMIT 1 5 6 OMIT 25 0 2 OMIT 4 5 3 OMIT 2 7 3 OMIT 1 2 3 OMIT 1 1 6 OMIT 7 3 0 OMIT 14 3 9 OMIT 5 3 0 OMIT 4 5 8 OMIT 0 4 0 OMIT 21 0 2 OMIT 7 4 8 OMIT 9 10 3 OMIT 2 4 0 OMIT 23 2 2 OMIT 2 8 5 L.S. 12 BOND $H ACTA CONF WGHT 0.081100 0.637500 FVAR 0.73219 O1 4 0.382037 0.427869 0.146219 11.00000 0.03358 0.03995 = 0.03023 0.00713 -0.00240 -0.00322 N1 3 0.500000 0.503561 0.250000 10.50000 0.02601 0.02256 = 0.03384 0.00000 0.00683 0.00000 C1 1 0.500000 0.655521 0.250000 10.50000 0.02851 0.02391 = 0.02498 0.00000 -0.00426 0.00000 C2 1 0.545846 0.735401 0.168247 11.00000 0.03778 0.02808 = 0.02775 0.00138 -0.00055 -0.00374 AFIX 43 H2 2 0.577660 0.684521 0.112882 11.00000 -1.20000 AFIX 0 C3 1 0.544880 0.888240 0.167981 11.00000 0.06318 0.02860 = 0.03784 0.00471 0.00282 -0.01022 AFIX 43 H3 2 0.575533 0.940593 0.110555 11.00000 -1.20000 AFIX 0 C4 1 0.500000 0.965076 0.250000 10.50000 0.09081 0.02277 = 0.04753 0.00000 0.00328 0.00000 AFIX 43 H4 2 0.499999 1.069489 0.250000 10.50000 -1.20000 AFIX 0 C5 1 0.458041 0.418526 0.343838 11.00000 0.02512 0.02409 = 0.02770 0.00072 0.00201 -0.00044 AFIX 23 H5A 2 0.447899 0.476190 0.433961 11.00000 -1.20000 H5B 2 0.480651 0.328071 0.375413 11.00000 -1.20000 AFIX 0 C6 1 0.395561 0.376099 0.266634 11.00000 0.02657 0.02469 = 0.02723 -0.00191 0.00271 0.00284 C7 1 0.352476 0.268778 0.342300 11.00000 0.02538 0.02356 = 0.02775 -0.00279 0.00351 0.00139 C8 1 0.365411 0.214545 0.484026 11.00000 0.02916 0.03265 = 0.02925 -0.00088 0.00089 -0.00361 AFIX 43 H8 2 0.402012 0.248116 0.537005 11.00000 -1.20000 AFIX 0 C9 1 0.324613 0.111347 0.547374 11.00000 0.03775 0.04066 = 0.03029 0.00405 0.00397 -0.00644 AFIX 43 H9 2 0.333629 0.073789 0.643461 11.00000 -1.20000 AFIX 0 C10 1 0.270803 0.062840 0.471163 11.00000 0.03520 0.03666 = 0.03664 -0.00186 0.00864 -0.00918 AFIX 43 H10 2 0.243425 -0.008843 0.514406 11.00000 -1.20000 AFIX 0 C11 1 0.256965 0.119048 0.331716 11.00000 0.03047 0.03821 = 0.03718 -0.00634 0.00142 -0.00863 AFIX 43 H11 2 0.219476 0.087802 0.280639 11.00000 -1.20000 AFIX 0 C12 1 0.297751 0.220635 0.266958 11.00000 0.03161 0.03279 = 0.03037 -0.00191 -0.00090 -0.00245 AFIX 43 H12 2 0.288486 0.257788 0.170838 11.00000 -1.20000 AFIX 0 HKLF 4 REM T-251 in Pbcn REM wR2 = 0.1418, GooF = S = 1.089, Restrained GooF = 1.089 for all data REM R1 = 0.0505 for 1746 Fo > 4sig(Fo) and 0.0517 for all 1834 data REM 115 parameters refined using 0 restraints END WGHT 0.0811 0.6375 REM Highest difference peak 0.285, deepest hole -0.232, 1-sigma level 0.055 Q1 1 0.6254 0.7806 0.1611 11.00000 0.05 0.29 Q2 1 0.3855 0.4153 0.5099 11.00000 0.05 0.23 Q3 1 0.3566 0.2155 0.1698 11.00000 0.05 0.23 Q4 1 0.2779 -0.0865 0.3389 11.00000 0.05 0.22 Q5 1 0.4313 0.3962 0.3104 11.00000 0.05 0.21 Q6 1 0.4863 0.5761 0.2279 11.00000 0.05 0.20 Q7 1 0.4741 1.1006 0.2021 11.00000 0.05 0.19 Q8 1 0.2579 0.0729 0.1687 11.00000 0.05 0.19 Q9 1 0.6474 0.7395 0.0187 11.00000 0.05 0.19 Q10 1 0.3331 0.2381 0.3034 11.00000 0.05 0.18 Q11 1 0.5424 0.8226 0.1713 11.00000 0.05 0.18 Q12 1 0.5241 0.2798 0.3251 11.00000 0.05 0.18 Q13 1 0.2622 -0.1182 0.4867 11.00000 0.05 0.17 Q14 1 0.3920 0.3766 0.4099 11.00000 0.05 0.17 Q15 1 0.5888 0.6004 0.1610 11.00000 0.05 0.17 Q16 1 0.5411 0.6850 0.2427 11.00000 0.05 0.16 Q17 1 0.4572 0.1164 0.4927 11.00000 0.05 0.16 Q18 1 0.5071 0.9352 0.1824 11.00000 0.05 0.16 Q19 1 0.4939 0.5038 0.4223 11.00000 0.05 0.16 Q20 1 0.3257 0.1219 0.7690 11.00000 0.05 0.15 ; _shelx_res_checksum 81441 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.38204(5) 0.42787(12) 0.14622(11) 0.0346(3) Uani d 1 . . N N1 0.500000 0.50356(17) 0.250000 0.0275(4) Uani d 1 . . C C1 0.500000 0.65552(19) 0.250000 0.0258(4) Uani d 1 . . C C2 0.54585(7) 0.73540(15) 0.16825(14) 0.0312(3) Uani d 1 . . H H2 0.577660 0.684521 0.112882 0.037 Uiso calc 1 . . C C3 0.54488(9) 0.88824(18) 0.16798(17) 0.0432(4) Uani d 1 . . H H3 0.575533 0.940593 0.110555 0.052 Uiso calc 1 . . C C4 0.500000 0.9651(2) 0.250000 0.0537(7) Uani d 1 . . H H4 0.499999 1.069489 0.250000 0.064 Uiso calc 1 . . C C5 0.45804(6) 0.41853(14) 0.34384(14) 0.0256(3) Uani d 1 . . H H5A 0.447899 0.476190 0.433961 0.031 Uiso calc 1 . . H H5B 0.480651 0.328071 0.375413 0.031 Uiso calc 1 . . C C6 0.39556(6) 0.37610(14) 0.26663(14) 0.0262(3) Uani d 1 . . C C7 0.35248(6) 0.26878(14) 0.34230(13) 0.0256(3) Uani d 1 . . C C8 0.36541(6) 0.21454(15) 0.48403(15) 0.0304(3) Uani d 1 . . H H8 0.402012 0.248116 0.537005 0.036 Uiso calc 1 . . C C9 0.32461(7) 0.11135(17) 0.54737(16) 0.0362(4) Uani d 1 . . H H9 0.333629 0.073789 0.643461 0.043 Uiso calc 1 . . C C10 0.27080(7) 0.06284(17) 0.47116(17) 0.0362(4) Uani d 1 . . H H10 0.243425 -0.008843 0.514406 0.043 Uiso calc 1 . . C C11 0.25697(7) 0.11905(17) 0.33172(16) 0.0353(4) Uani d 1 . . H H11 0.219476 0.087802 0.280639 0.042 Uiso calc 1 . . C C12 0.29775(7) 0.22064(15) 0.26696(16) 0.0316(3) Uani d 1 . . H H12 0.288486 0.257788 0.170838 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 0.0336(5) 0.0400(6) 0.0302(5) -0.0032(4) -0.0024(4) 0.0071(4) N1 0.0260(7) 0.0226(7) 0.0338(8) 0.000 0.0068(6) 0.000 C1 0.0285(8) 0.0239(8) 0.0250(8) 0.000 -0.0043(6) 0.000 C2 0.0378(8) 0.0281(7) 0.0277(7) -0.0037(5) -0.0006(5) 0.0014(5) C3 0.0632(11) 0.0286(7) 0.0378(8) -0.0102(7) 0.0028(7) 0.0047(6) C4 0.091(2) 0.0228(10) 0.0475(13) 0.000 0.0033(12) 0.000 C5 0.0251(6) 0.0241(6) 0.0277(6) -0.0004(4) 0.0020(4) 0.0007(4) C6 0.0266(6) 0.0247(6) 0.0272(6) 0.0028(5) 0.0027(5) -0.0019(5) C7 0.0254(6) 0.0236(6) 0.0277(6) 0.0014(5) 0.0035(4) -0.0028(4) C8 0.0292(6) 0.0326(7) 0.0292(6) -0.0036(5) 0.0009(5) -0.0009(5) C9 0.0377(7) 0.0407(8) 0.0303(7) -0.0064(6) 0.0040(6) 0.0041(6) C10 0.0352(7) 0.0367(7) 0.0366(7) -0.0092(6) 0.0086(6) -0.0019(6) C11 0.0305(7) 0.0382(8) 0.0372(8) -0.0086(6) 0.0014(5) -0.0063(6) C12 0.0316(7) 0.0328(7) 0.0304(7) -0.0024(5) -0.0009(5) -0.0019(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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_ _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 C1 N1 C5 . . 122.46(7) ? C1 N1 C5 . 3_655 122.46(7) ? C5 N1 C5 . 3_655 115.08(14) ? N1 C1 C2 . 3_655 121.07(9) ? N1 C1 C2 . . 121.07(9) ? C2 C1 C2 3_655 . 117.86(17) ? C3 C2 C1 . . 120.47(14) ? C3 C2 H2 . . 119.8 ? C1 C2 H2 . . 119.8 ? C4 C3 C2 . . 120.98(15) ? C4 C3 H3 . . 119.5 ? C2 C3 H3 . . 119.5 ? C3 C4 C3 3_655 . 119.2(2) ? C3 C4 H4 3_655 . 120.4 ? C3 C4 H4 . . 120.4 ? N1 C5 C6 . . 112.65(9) ? N1 C5 H5A . . 109.1 ? C6 C5 H5A . . 109.1 ? N1 C5 H5B . . 109.1 ? C6 C5 H5B . . 109.1 ? H5A C5 H5B . . 107.8 ? O1 C6 C7 . . 121.50(12) ? O1 C6 C5 . . 120.45(11) ? C7 C6 C5 . . 118.05(11) ? C8 C7 C12 . . 119.44(12) ? C8 C7 C6 . . 122.28(12) ? C12 C7 C6 . . 118.27(12) ? C9 C8 C7 . . 119.81(13) ? C9 C8 H8 . . 120.1 ? C7 C8 H8 . . 120.1 ? C10 C9 C8 . . 120.38(13) ? C10 C9 H9 . . 119.8 ? C8 C9 H9 . . 119.8 ? C9 C10 C11 . . 119.97(13) ? C9 C10 H10 . . 120.0 ? C11 C10 H10 . . 120.0 ? C12 C11 C10 . . 120.05(13) ? C12 C11 H11 . . 120.0 ? C10 C11 H11 . . 120.0 ? C11 C12 C7 . . 120.32(13) ? C11 C12 H12 . . 119.8 ? C7 C12 H12 . . 119.8 ? 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 C6 . 1.2165(16) ? N1 C1 . 1.383(2) ? N1 C5 . 1.4415(14) ? N1 C5 3_655 1.4416(14) ? C1 C2 3_655 1.4082(16) ? C1 C2 . 1.4082(16) ? C2 C3 . 1.391(2) ? C2 H2 . 0.9500 ? C3 C4 . 1.382(2) ? C3 H3 . 0.9500 ? C4 H4 . 0.9500 ? C5 C6 . 1.5254(17) ? C5 H5A . 0.9900 ? C5 H5B . 0.9900 ? C6 C7 . 1.4913(18) ? C7 C8 . 1.3960(19) ? C7 C12 . 1.3973(19) ? C8 C9 . 1.3892(19) ? C8 H8 . 0.9500 ? C9 C10 . 1.387(2) ? C9 H9 . 0.9500 ? C10 C11 . 1.388(2) ? C10 H10 . 0.9500 ? C11 C12 . 1.384(2) ? C11 H11 . 0.9500 ? C12 H12 . 0.9500 ? 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 C5 H5A O1 7_566 0.99 2.51 3.4483(16) 158 C8 H8 Cg1 5_666 0.95 2.85 3.6963(14) 148 C8 H8 Cg1 8_565 0.95 2.85 3.6963(14) 148 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 C5 N1 C1 C2 . . . 3_655 -6.40(9) ? C5 N1 C1 C2 3_655 . . 3_655 173.60(9) ? C5 N1 C1 C2 . . . . 173.59(9) ? C5 N1 C1 C2 3_655 . . . -6.41(9) ? N1 C1 C2 C3 . . . . 179.32(10) ? C2 C1 C2 C3 3_655 . . . -0.68(10) ? C1 C2 C3 C4 . . . . 1.4(2) ? C2 C3 C4 C3 . . . 3_655 -0.69(11) ? C1 N1 C5 C6 . . . . 93.41(9) ? C5 N1 C5 C6 3_655 . . . -86.59(9) ? N1 C5 C6 O1 . . . . -8.70(17) ? N1 C5 C6 C7 . . . . 170.61(11) ? O1 C6 C7 C8 . . . . -176.33(12) ? C5 C6 C7 C8 . . . . 4.37(18) ? O1 C6 C7 C12 . . . . 4.30(19) ? C5 C6 C7 C12 . . . . -175.00(11) ? C12 C7 C8 C9 . . . . 1.3(2) ? C6 C7 C8 C9 . . . . -178.06(12) ? C7 C8 C9 C10 . . . . -0.6(2) ? C8 C9 C10 C11 . . . . -0.9(2) ? C9 C10 C11 C12 . . . . 1.7(2) ? C10 C11 C12 C7 . . . . -1.0(2) ? C8 C7 C12 C11 . . . . -0.6(2) ? C6 C7 C12 C11 . . . . 178.84(12) ? _cod_database_fobs_code 2244109