#------------------------------------------------------------------------------ #$Date: 2020-04-18 05:14:00 +0300 (Sat, 18 Apr 2020) $ #$Revision: 250923 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/78/1557817.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_1557817 loop_ _publ_author_name 'Chadeayne, Andrew R.' 'Pham, Duyen N. K.' 'Golen, James A.' 'Manke, David R.' _publ_section_title ; 5-MeO-DALT: the freebase of N,N-diallyl-5-methoxytryptamine ; _journal_coeditor_code BX4017 _journal_issue 4 _journal_name_full IUCrData _journal_paper_doi 10.1107/S2414314620004988 _journal_volume 5 _journal_year 2020 _chemical_formula_iupac 'C17 H22 N2 O' _chemical_formula_moiety 'C17 H22 N2 O' _chemical_formula_sum 'C17 H22 N2 O' _chemical_formula_weight 270.36 _chemical_name_common ; N,N-Diallyl-5-methoxytryptamine ; _chemical_name_systematic N-[2-(5-Methoxy-1H-indol-3-yl)ethyl]-N-(prop-2-en-1-yl)prop-2-en-1-amine _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_method ; Olex2 1.3 (compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032) ; _cell_angle_alpha 90 _cell_angle_beta 91.626(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.1444(6) _cell_length_b 12.8514(13) _cell_length_c 19.3315(19) _cell_measurement_reflns_used 7918 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 24.47 _cell_measurement_theta_min 3.17 _cell_volume 1525.9(3) _computing_cell_refinement ; SAINT (Bruker, 2018) ; _computing_data_collection ; APEX3 (Bruker, 2018) ; _computing_data_reduction ; SAINT (Bruker, 2018) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 296.15 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Bruker D8 Venture CMOS' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_unetI/netI 0.0226 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 45375 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.462 _diffrn_reflns_theta_min 3.170 _diffrn_source_current 30.0 _diffrn_source_power 1.5 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.6939 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2018) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.177 _exptl_crystal_description PLATE _exptl_crystal_F_000 584 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.154 _refine_diff_density_min -0.128 _refine_ls_extinction_coef 0.036(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2018 (Sheldrick, 2015b) ; _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 186 _refine_ls_number_reflns 2810 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0408 _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^)+(0.0421P)^2^+0.3975P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0941 _refine_ls_wR_factor_ref 0.1057 _reflns_number_gt 2145 _reflns_number_total 2810 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file bx4017sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1557817 _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 0.978 _shelx_estimated_absorpt_t_max 0.998 _shelx_hkl_file ; 1 0 0 -0.40 3.40 1 0 0 3.50 4.00 1 0 0 7.90 5.10 -1 0 0 -5.80 3.10 1 0 0 -0.80 3.00 -1 0 0 3.50 4.40 -1 0 0 4.00 6.30 -2 0 0 3305.57 81.39 -2 0 0 3405.06 82.19 -2 0 0 3364.76 83.39 -2 0 0 3327.47 83.49 2 0 0 3358.56 83.49 -2 0 0 3275.47 86.89 2 0 0 3509.75 87.49 2 0 0 3455.35 83.39 2 0 0 3299.37 81.99 -2 0 0 3373.46 86.79 -3 0 0 9.70 6.30 -3 0 0 2.00 7.80 -3 0 0 -0.60 11.50 -3 0 0 -4.90 7.50 -3 0 0 -1.80 11.30 -3 0 0 -3.20 5.30 3 0 0 1.60 10.90 3 0 0 -14.30 7.10 3 0 0 -0.50 7.20 3 0 0 -0.90 6.20 -4 0 0 759.12 35.20 -4 0 0 793.52 34.70 4 0 0 755.32 25.20 4 0 0 774.32 28.30 4 0 0 757.32 27.40 4 0 0 761.52 35.00 -4 0 0 737.73 23.60 -4 0 0 758.52 25.60 -4 0 0 762.92 28.30 -4 0 0 744.43 28.00 5 0 0 -10.00 16.20 5 0 0 2.70 9.70 5 0 0 5.10 6.40 -5 0 0 8.10 15.30 -5 0 0 -7.00 9.90 -5 0 0 -2.40 9.90 -5 0 0 -0.10 5.90 5 0 0 1.70 7.80 -5 0 0 6.50 15.00 -6 0 0 143.39 23.70 -6 0 0 137.49 8.80 -6 0 0 168.08 24.60 -6 0 0 119.39 15.80 6 0 0 119.29 22.60 -6 0 0 133.99 17.10 6 0 0 156.38 16.40 7 0 0 5.20 6.60 -7 0 0 -25.60 17.90 -7 0 0 22.70 20.90 -7 0 0 12.10 12.10 7 0 0 -8.60 29.20 -7 0 0 -7.50 11.10 7 0 0 13.60 10.40 -1 -1 0 -3.20 4.70 -1 -1 0 6.80 6.70 -1 -1 0 12.70 3.90 1 -1 0 2.70 3.00 1 -1 0 6.30 5.30 1 -1 0 6.10 7.20 1 -1 0 -3.70 5.30 -1 -1 0 5.30 3.80 1 -1 0 4.50 6.10 -1 -1 0 7.30 3.10 -1 1 0 6.90 3.10 1 1 0 -2.00 4.60 1 1 0 5.40 5.70 -1 1 0 7.10 6.10 1 1 0 7.60 3.20 -1 1 0 11.20 7.70 -1 1 0 8.60 5.80 -1 1 0 3.20 6.20 -1 1 0 10.60 6.30 -2 -1 0 234.88 9.90 2 -1 0 228.68 17.70 -2 -1 0 258.67 16.70 -2 -1 0 216.78 11.90 2 -1 0 233.18 14.80 2 -1 0 246.08 13.70 2 -1 0 244.48 9.10 -2 -1 0 251.57 16.30 -2 -1 0 249.58 12.00 2 -1 0 248.48 14.40 2 1 0 250.07 9.90 2 1 0 248.18 11.80 -2 1 0 253.77 14.00 -2 1 0 243.08 9.20 -2 1 0 267.27 19.30 -2 1 0 229.48 14.80 2 1 0 220.98 16.00 -2 1 0 241.08 14.70 -3 -1 0 76.39 7.00 3 -1 0 82.19 10.10 3 -1 0 101.99 16.20 -3 -1 0 90.49 9.50 3 -1 0 100.19 11.50 3 -1 0 115.09 11.60 -3 -1 0 96.59 14.00 -3 -1 0 103.39 13.90 -3 -1 0 85.29 9.50 3 1 0 85.79 8.50 3 1 0 83.69 8.70 -3 1 0 92.19 14.70 -3 1 0 75.49 10.80 -3 1 0 91.39 7.30 3 1 0 96.49 13.70 -3 1 0 77.79 9.60 3 1 0 107.89 10.10 -4 -1 0 618.24 24.00 4 -1 0 622.34 32.40 -4 -1 0 661.53 31.50 -4 -1 0 644.84 30.70 4 -1 0 635.84 25.80 -4 -1 0 615.04 22.60 4 -1 0 609.64 23.50 -4 -1 0 603.14 20.30 4 -1 0 601.34 25.90 -4 -1 0 597.94 23.60 4 1 0 653.73 20.20 4 1 0 626.94 30.60 -4 1 0 571.44 30.70 -4 1 0 592.04 29.70 -4 1 0 597.44 26.00 -4 1 0 581.24 18.30 4 1 0 626.04 23.90 -4 1 0 606.24 32.70 4 1 0 571.44 22.70 -5 -1 0 279.67 19.40 5 -1 0 290.07 17.40 5 -1 0 284.37 26.00 -5 -1 0 311.67 26.60 -5 -1 0 318.57 19.40 5 -1 0 304.17 24.80 -5 -1 0 301.97 16.50 -5 -1 0 279.57 27.30 5 -1 0 311.17 20.10 5 1 0 295.77 26.90 -5 1 0 282.37 26.50 -5 1 0 274.47 21.80 5 1 0 310.27 17.80 5 1 0 298.97 19.00 -5 1 0 298.67 10.60 -5 1 0 299.77 21.60 -5 1 0 351.06 30.70 -6 -1 0 40.30 8.50 -6 -1 0 49.20 19.60 -6 -1 0 25.80 11.60 6 -1 0 27.20 12.00 -6 -1 0 42.80 19.10 6 -1 0 28.90 12.40 -6 -1 0 27.50 12.20 6 -1 0 59.89 20.40 -6 1 0 51.39 14.50 -6 1 0 24.20 18.30 -6 1 0 57.89 20.20 6 1 0 5.70 6.40 6 1 0 32.10 10.10 6 1 0 55.69 18.90 -6 1 0 43.00 14.00 7 -1 0 4.50 11.50 7 -1 0 13.00 18.90 -7 -1 0 -6.00 4.20 -7 -1 0 -3.00 18.40 7 -1 0 6.90 7.20 -7 -1 0 -4.30 10.80 -7 -1 0 18.90 11.80 -7 -1 0 15.50 18.80 -7 -1 0 -2.80 4.30 7 -1 0 -4.80 4.20 -7 1 0 -25.90 16.30 -7 1 0 -10.30 18.10 -7 1 0 -12.00 11.80 7 1 0 18.40 6.00 7 1 0 -12.80 16.20 -7 1 0 -21.40 12.30 -7 1 0 14.90 18.50 0 -2 0 2609.14 64.39 0 -2 0 2658.83 65.09 0 -2 0 2598.54 64.49 0 -2 0 2610.74 63.79 0 -2 0 2549.65 62.79 0 2 0 2636.04 62.89 0 2 0 2727.33 64.59 1 -2 0 4544.15 110.09 1 -2 0 4700.63 112.59 -1 -2 0 4675.23 112.69 -1 -2 0 4576.04 111.59 1 -2 0 4630.14 112.39 1 -2 0 4449.06 112.19 -1 -2 0 4523.65 109.49 1 -2 0 4642.74 112.39 -1 -2 0 4646.64 109.49 -1 -2 0 4458.95 109.39 1 -2 0 4405.06 112.99 -1 2 0 4825.72 113.59 -1 2 0 4540.55 112.29 1 2 0 4659.73 109.49 1 2 0 4736.23 109.49 1 2 0 4594.24 111.49 -1 2 0 4527.55 112.19 -1 2 0 4632.94 112.69 -1 2 0 4642.04 112.59 -2 -2 0 74.19 7.10 2 -2 0 67.29 10.30 -2 -2 0 63.19 6.70 -2 -2 0 71.19 8.90 -2 -2 0 70.39 10.70 -2 -2 0 65.19 6.80 2 -2 0 61.99 10.30 2 -2 0 70.19 10.70 2 -2 0 65.09 12.60 2 -2 0 70.49 6.90 -2 2 0 58.39 10.90 -2 2 0 53.69 12.90 -2 2 0 60.59 10.80 2 2 0 68.99 10.40 2 2 0 63.49 6.60 2 2 0 65.99 10.50 -2 2 0 70.49 10.30 -2 2 0 74.49 11.30 -2 2 0 67.29 7.00 3 -2 0 72.99 11.80 -3 -2 0 82.19 12.50 -3 -2 0 56.29 7.90 3 -2 0 81.79 11.20 -3 -2 0 69.79 7.30 -3 -2 0 72.99 13.10 3 -2 0 60.59 10.80 -3 -2 0 67.29 8.10 3 -2 0 80.79 16.30 -3 2 0 83.29 12.20 -3 2 0 71.69 13.00 -3 2 0 73.89 6.60 3 2 0 70.69 12.00 -3 2 0 62.89 14.60 3 2 0 64.69 7.50 -3 2 0 64.89 11.70 4 -2 0 291.27 24.70 4 -2 0 313.47 18.70 -4 -2 0 303.17 16.30 -4 -2 0 286.87 11.80 4 -2 0 300.37 19.80 -4 -2 0 317.57 22.80 4 -2 0 265.67 19.10 -4 -2 0 300.17 23.70 -4 -2 0 290.77 16.00 -4 2 0 287.87 26.40 -4 2 0 265.57 20.50 -4 2 0 286.57 9.70 4 2 0 281.37 22.60 4 2 0 289.37 14.90 4 2 0 291.17 16.00 -4 2 0 328.97 19.50 -5 -2 0 411.36 29.40 5 -2 0 363.86 22.80 5 -2 0 383.56 21.00 5 -2 0 383.96 30.30 -5 -2 0 366.66 20.50 5 -2 0 382.06 23.10 -5 -2 0 421.46 29.10 -5 -2 0 387.56 20.50 -5 -2 0 414.06 20.60 5 2 0 391.76 18.80 -5 2 0 387.86 32.20 -5 2 0 431.16 43.80 5 2 0 344.77 19.60 5 2 0 333.67 27.80 -5 2 0 370.96 24.80 -5 2 0 421.06 29.90 -5 2 0 414.96 25.30 -6 -2 0 139.39 14.90 6 -2 0 107.69 15.70 -6 -2 0 114.89 12.90 -6 -2 0 121.29 21.10 -6 -2 0 127.19 21.90 6 -2 0 69.99 14.80 -6 -2 0 137.09 14.60 -6 2 0 141.19 18.50 6 2 0 158.38 22.40 6 2 0 143.39 14.10 -6 2 0 127.89 22.20 -6 2 0 155.58 18.90 -6 2 0 176.28 26.20 7 -2 0 32.20 14.30 -7 -2 0 29.10 11.30 -7 -2 0 21.70 20.10 -7 -2 0 6.70 18.00 -7 -2 0 36.40 9.10 7 -2 0 3.70 8.70 7 -2 0 0.40 18.80 -7 -2 0 27.10 11.10 7 2 0 6.80 7.60 -7 2 0 28.40 15.40 7 2 0 53.19 18.10 -7 2 0 48.20 22.60 -7 2 0 32.70 15.20 -7 2 0 25.20 19.80 -7 2 0 22.70 20.10 0 -3 0 4.00 5.20 0 -3 0 -8.90 9.10 0 -3 0 -9.10 7.40 0 -3 0 5.60 8.10 0 -3 0 -2.00 5.90 0 -3 0 2.50 8.60 0 3 0 6.00 7.70 0 3 0 -1.90 5.50 0 3 0 -2.00 4.60 0 3 0 -3.80 7.30 0 3 0 -0.80 7.90 2 -3 0 1864.11 46.70 2 -3 0 1774.62 51.09 -2 -3 0 1833.62 46.40 2 -3 0 1868.11 54.59 -2 -3 0 1769.32 46.40 -2 -3 0 1772.52 52.09 2 -3 0 1838.72 51.59 2 -3 0 1791.42 51.39 -2 -3 0 1793.62 57.09 -2 -3 0 1726.93 47.90 -2 3 0 1758.62 55.79 2 3 0 1791.42 46.40 2 3 0 1836.92 48.20 2 3 0 1796.82 50.79 -2 3 0 1851.11 51.99 -2 3 0 1804.82 51.49 -2 3 0 1786.02 53.69 -2 3 0 1783.52 51.79 -3 -3 0 8.90 4.50 3 -3 0 26.70 13.40 3 -3 0 6.60 9.80 -3 -3 0 16.30 6.20 3 -3 0 20.90 10.50 3 -3 0 10.70 12.40 3 -3 0 4.30 4.50 -3 -3 0 17.10 10.50 -3 -3 0 35.10 10.20 -3 -3 0 8.70 6.10 -3 3 0 -15.00 10.40 -3 3 0 17.70 10.30 -3 3 0 19.40 10.90 3 3 0 -5.80 9.70 3 3 0 3.00 9.20 -3 3 0 4.20 12.50 3 3 0 20.30 6.30 -3 3 0 7.60 10.20 -4 -3 0 150.18 17.90 -4 -3 0 133.99 15.60 -4 -3 0 172.48 12.80 4 -3 0 175.98 17.60 -4 -3 0 142.39 8.00 -4 -3 0 148.99 12.30 4 -3 0 186.58 21.10 4 -3 0 172.48 17.00 4 -3 0 163.88 16.70 -4 3 0 158.88 20.50 4 3 0 155.18 12.20 -4 3 0 171.18 17.20 -4 3 0 154.28 16.00 4 3 0 138.29 15.60 4 3 0 149.19 11.30 -4 3 0 183.08 17.50 -4 3 0 149.49 18.10 -5 -3 0 514.55 32.80 5 -3 0 537.85 26.50 -5 -3 0 508.25 22.30 -5 -3 0 515.45 25.50 -5 -3 0 514.35 22.20 -5 -3 0 498.75 30.60 5 -3 0 513.25 27.70 5 -3 0 527.35 27.60 5 -3 0 563.74 35.90 5 3 0 538.25 30.50 5 3 0 503.65 21.60 -5 3 0 536.45 29.20 -5 3 0 511.65 32.40 -5 3 0 546.55 46.90 -5 3 0 508.25 47.20 -5 3 0 574.34 30.10 -6 -3 0 15.90 9.10 -6 -3 0 0.00 8.50 6 -3 0 25.80 30.80 -6 -3 0 27.50 18.20 -6 -3 0 1.30 15.70 6 -3 0 -9.70 11.30 6 -3 0 -6.70 6.70 -6 -3 0 -5.10 10.10 6 3 0 -1.20 13.10 -6 3 0 13.90 17.20 -6 3 0 -9.40 17.40 6 3 0 4.30 7.50 -6 3 0 -24.90 12.50 -6 3 0 -8.00 16.60 6 3 0 10.50 7.60 7 -3 0 -2.80 6.00 -7 -3 0 12.00 9.80 -7 -3 0 22.50 10.40 7 -3 0 10.80 8.30 -7 -3 0 14.00 10.30 -7 -3 0 11.60 18.40 7 -3 0 47.60 21.00 7 -3 0 40.10 14.30 -7 -3 0 15.60 9.90 -7 -3 0 26.90 18.60 -7 3 0 24.60 21.70 7 3 0 -6.20 13.50 7 3 0 16.00 6.20 -7 3 0 6.60 15.50 -7 3 0 21.00 15.00 1 -4 0 0.60 9.30 1 -4 0 1.70 9.80 1 -4 0 12.30 10.30 1 -4 0 1.60 9.10 -1 -4 0 5.50 7.20 1 -4 0 5.00 9.90 -1 -4 0 -2.50 6.40 -1 -4 0 6.10 7.50 1 4 0 0.20 6.50 -1 4 0 2.40 9.30 1 4 0 -13.40 9.10 -1 4 0 -0.70 9.30 -1 4 0 2.60 8.70 1 4 0 13.60 6.60 -1 4 0 -2.20 9.80 1 4 0 14.60 7.50 2 -4 0 722.83 23.40 -2 -4 0 676.63 28.30 2 -4 0 701.33 27.60 -2 -4 0 617.84 21.10 2 -4 0 674.73 27.80 -2 -4 0 676.43 26.50 2 -4 0 727.63 27.90 2 -4 0 710.23 29.00 -2 -4 0 670.33 28.20 -2 -4 0 615.94 21.50 2 -4 0 704.53 29.40 -2 4 0 703.03 27.70 2 4 0 665.03 21.40 2 4 0 641.34 21.60 -2 4 0 680.03 27.30 -2 4 0 763.22 29.80 2 4 0 642.24 21.70 2 4 0 644.14 26.40 -2 4 0 757.12 30.80 -2 4 0 737.43 28.40 3 -4 0 327.47 24.00 -3 -4 0 283.87 19.90 -3 -4 0 311.07 14.40 3 -4 0 308.07 13.60 -3 -4 0 351.66 22.40 -3 -4 0 289.87 12.90 -3 -4 0 317.97 14.30 3 -4 0 311.97 20.30 3 -4 0 318.77 20.70 -3 -4 0 288.47 16.90 3 -4 0 347.37 22.30 -3 4 0 310.67 20.80 3 4 0 311.17 17.40 -3 4 0 338.77 22.30 -3 4 0 333.97 22.10 -3 4 0 310.87 21.40 -3 4 0 354.66 25.40 3 4 0 285.57 14.00 3 4 0 349.27 20.90 -4 -4 0 516.45 25.20 -4 -4 0 490.75 19.50 -4 -4 0 461.75 19.10 4 -4 0 452.25 29.10 -4 -4 0 477.65 27.80 4 -4 0 467.65 26.50 4 -4 0 513.25 26.10 -4 -4 0 474.95 15.10 4 -4 0 495.05 27.30 4 -4 0 495.45 15.50 -4 4 0 463.65 27.20 4 4 0 482.35 24.40 -4 4 0 483.15 32.60 -4 4 0 473.25 27.40 -4 4 0 499.05 26.70 -5 -4 0 36.70 8.90 5 -4 0 48.80 14.10 5 -4 0 12.50 14.20 5 -4 0 74.89 14.40 5 -4 0 42.60 13.70 -5 -4 0 51.69 16.60 -5 -4 0 40.90 9.30 -5 -4 0 49.20 14.00 -5 4 0 62.09 17.50 5 4 0 51.19 13.40 5 4 0 48.90 8.50 -5 4 0 86.99 21.50 -5 4 0 48.60 16.00 -6 -4 0 -8.10 8.10 -6 -4 0 10.60 14.10 -6 -4 0 -13.00 10.80 -6 -4 0 4.50 16.00 -6 -4 0 -6.10 11.70 6 -4 0 -6.10 8.10 6 -4 0 35.50 25.10 6 -4 0 -13.10 17.90 6 -4 0 5.70 13.20 -6 4 0 9.10 17.10 -6 4 0 -13.70 16.20 6 4 0 4.80 12.20 -6 4 0 4.40 15.20 6 4 0 10.80 6.60 -6 4 0 -13.30 13.50 -6 4 0 4.30 18.60 -7 -4 0 21.10 17.30 -7 -4 0 4.70 8.60 7 -4 0 -7.80 7.00 7 -4 0 -9.80 23.70 7 -4 0 13.60 14.00 -7 -4 0 11.10 18.70 -7 -4 0 21.10 9.50 7 -4 0 11.40 9.40 -7 -4 0 15.30 11.50 -7 4 0 -1.00 15.40 -7 4 0 -17.40 17.90 -7 4 0 30.30 36.30 -7 4 0 20.40 15.40 7 4 0 6.70 3.90 7 4 0 1.00 4.40 0 -5 0 -15.50 9.40 0 -5 0 1.00 10.20 0 -5 0 24.90 9.80 0 -5 0 -0.90 9.40 0 -5 0 4.60 7.50 0 -5 0 -5.10 5.30 0 5 0 9.10 9.20 0 5 0 0.50 9.00 0 5 0 2.50 5.30 0 5 0 16.30 9.80 0 5 0 1.70 6.50 1 -5 0 1219.08 37.80 1 -5 0 1098.49 36.00 1 -5 0 1121.69 38.40 -1 -5 0 1087.99 34.30 -1 -5 0 1102.39 34.00 -1 -5 0 1100.99 37.50 -1 -5 0 1155.68 34.20 1 -5 0 1188.08 37.90 1 -5 0 1191.58 37.30 -1 5 0 1178.08 37.70 -1 5 0 1141.59 37.20 -1 5 0 1110.79 36.90 -1 5 0 1126.99 36.10 1 5 0 1126.79 37.50 1 5 0 1116.99 33.60 1 5 0 1116.69 34.70 1 5 0 1023.00 33.50 2 -5 0 677.93 29.70 -2 -5 0 663.73 29.40 -2 -5 0 611.34 19.70 2 -5 0 738.43 29.20 -2 -5 0 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24.60 -1 5 21 87.79 20.40 1 5 -21 35.40 15.50 -1 5 21 54.79 21.70 -1 5 21 44.60 20.30 0 -5 21 -21.20 17.60 0 -5 21 0.60 15.30 0 -5 -21 -11.70 18.60 0 -5 -21 16.10 18.50 0 -5 -21 1.10 18.60 0 -5 -21 4.90 5.20 0 -5 21 -7.40 19.50 0 -5 21 7.60 19.90 0 -5 21 -10.90 19.50 0 5 -21 29.70 20.30 0 5 -21 5.40 15.20 0 5 21 -16.60 18.00 0 5 21 -1.30 16.20 0 5 -21 -1.30 5.50 0 5 21 42.50 20.90 0 5 21 20.70 18.10 0 5 -21 4.50 12.90 -1 -5 -21 16.70 16.20 -1 -5 -21 -2.40 18.30 -1 -5 -21 10.60 20.80 1 -5 21 22.20 25.80 1 -5 21 5.00 18.50 1 -5 21 -11.50 20.20 1 -5 21 5.50 19.50 -1 -5 -21 -1.60 9.70 1 -5 21 6.40 17.30 -1 -5 -21 -6.10 18.10 -1 5 -21 16.70 19.50 1 5 21 4.50 18.40 -1 5 -21 25.50 17.90 1 5 21 -11.60 17.30 1 5 21 9.80 18.50 -1 5 -21 -17.60 15.60 -1 5 -21 -0.40 7.30 1 5 21 6.90 20.30 2 5 21 18.50 19.30 1 -6 -21 27.80 19.20 -1 -6 21 10.90 23.50 -1 -6 21 -26.40 21.00 1 -6 -21 -12.10 16.30 1 -6 -21 33.40 21.70 -1 -6 21 8.00 14.90 1 -6 -21 -1.90 4.30 -1 -6 21 -1.90 18.20 -1 -6 21 15.40 16.50 1 6 -21 28.70 14.30 1 6 -21 -1.20 4.80 1 6 -21 -7.00 6.00 -1 6 21 23.40 19.40 -1 6 21 -20.50 15.20 -1 6 21 1.30 20.70 1 6 -21 -1.10 17.00 -1 6 21 11.60 19.80 0 -6 21 34.60 20.50 0 -6 -21 10.30 19.40 0 -6 -21 39.20 20.70 0 -6 21 40.80 17.00 0 -6 -21 12.70 6.80 0 -6 -21 14.50 27.50 0 -6 -21 48.30 21.10 0 -6 21 61.19 22.30 0 6 -21 11.40 9.50 0 6 21 28.80 17.50 0 6 -21 11.60 11.90 0 6 -21 64.19 17.70 0 6 21 25.10 21.00 0 6 21 63.39 22.90 1 -6 21 22.30 18.90 1 -6 21 6.00 18.80 -1 -6 -21 36.30 19.40 -1 -6 -21 41.50 19.00 -1 -6 -21 12.70 10.80 1 -6 21 17.50 21.00 1 -6 21 -24.80 19.50 -1 -6 -21 38.30 18.00 1 -6 21 11.10 23.90 1 6 21 28.20 18.80 -1 6 -21 -2.70 8.00 1 6 21 41.20 19.70 -1 6 -21 -3.90 15.30 1 6 21 -3.10 19.70 1 6 21 24.30 18.80 2 0 -22 7.80 9.10 -2 0 22 39.40 20.90 2 0 -22 57.29 15.70 -2 0 22 50.09 14.40 2 0 -22 85.59 22.60 -2 0 22 56.19 16.20 -2 0 22 47.50 19.00 -1 0 22 2.00 11.90 -1 0 22 19.70 20.70 -1 0 22 -20.40 19.50 -1 0 22 25.10 25.40 1 0 -22 -22.50 14.10 1 0 -22 30.10 22.90 -1 0 22 -6.60 13.80 0 0 -22 11.60 18.90 0 0 -22 -9.30 3.30 0 0 22 3.60 18.50 0 0 22 17.20 19.40 0 0 22 5.80 19.60 0 0 22 43.10 19.70 0 0 -22 0.70 3.80 0 0 22 7.90 12.10 0 0 -22 -6.00 16.00 0 0 22 5.20 17.00 0 0 -22 -9.90 26.00 1 0 22 -9.30 18.00 -1 0 -22 -11.60 16.80 1 0 22 -1.70 12.40 -1 0 -22 -3.00 16.30 1 0 22 25.40 19.10 -1 0 -22 7.90 14.80 1 0 22 -20.00 19.20 1 0 22 -8.40 19.60 -1 0 -22 -11.80 18.60 -1 0 -22 -7.30 5.40 1 0 22 8.00 17.10 2 0 22 -1.00 21.40 -2 0 -22 -23.40 17.70 2 0 22 8.20 23.80 2 0 22 -23.90 16.00 -2 0 -22 -2.50 14.00 2 0 22 37.60 37.30 2 0 22 -10.20 13.40 -2 0 -22 2.20 7.30 2 -1 -22 39.50 18.00 2 -1 -22 23.80 15.60 -2 -1 22 26.20 14.80 -2 -1 22 35.90 17.00 -2 -1 22 5.80 19.80 2 -1 -22 1.50 10.70 -2 1 22 13.80 15.10 2 1 -22 15.40 8.80 2 1 -22 36.20 15.90 -2 1 22 0.30 13.60 -2 1 22 27.80 21.10 -2 1 22 43.40 18.50 -1 -1 22 5.20 19.60 -1 -1 22 19.50 11.90 -1 -1 22 -5.80 19.90 1 -1 -22 34.40 23.60 -1 -1 22 -18.60 14.00 1 -1 -22 25.80 15.60 -1 -1 22 39.20 17.70 1 -1 -22 6.80 15.20 1 1 -22 13.50 17.20 -1 1 22 2.10 16.50 1 1 -22 -0.70 11.80 -1 1 22 -2.40 13.10 -1 1 22 -23.90 18.30 -1 1 22 6.60 15.70 -1 1 22 44.70 21.20 1 1 -22 8.20 15.00 0 -1 -22 6.10 17.20 0 -1 -22 -2.50 3.60 0 -1 22 25.20 16.70 0 -1 -22 0.90 15.80 0 -1 22 25.90 19.30 0 -1 22 6.40 18.60 0 -1 22 13.00 20.50 0 -1 -22 -0.20 3.70 0 -1 22 3.70 17.80 0 -1 -22 22.70 18.70 0 -1 22 -11.80 14.20 0 1 22 6.70 20.60 0 1 -22 -3.60 17.60 0 1 -22 5.10 17.30 0 1 22 16.90 19.90 0 1 22 6.90 18.70 0 1 -22 7.40 15.90 0 1 22 41.20 18.40 0 1 22 1.40 13.40 0 1 -22 0.50 3.80 -1 -1 -22 6.30 5.90 -1 -1 -22 -19.80 16.10 -1 -1 -22 20.00 18.90 -1 -1 -22 28.10 15.10 1 -1 22 4.60 12.30 -1 -1 -22 4.30 20.00 1 -1 22 19.80 19.20 1 -1 22 -2.70 17.70 1 -1 22 -6.40 16.40 1 -1 22 8.10 21.90 1 -1 22 -25.80 16.50 1 1 22 33.60 22.30 -1 1 -22 -3.50 17.30 1 1 22 -1.90 13.90 -1 1 -22 0.00 17.60 1 1 22 10.20 16.80 1 1 22 23.80 20.30 1 1 22 -10.00 17.40 1 1 22 -7.30 18.10 -1 1 -22 9.40 11.10 -1 1 -22 -4.30 5.50 -1 1 -22 -5.20 17.80 2 -1 22 29.40 18.20 2 -1 22 -22.60 19.60 2 -1 22 -14.50 20.80 2 -1 22 14.30 13.50 -2 -1 -22 -15.00 6.30 -2 -1 -22 5.60 14.60 2 -1 22 -6.70 18.10 -2 -1 -22 2.90 19.50 -2 1 -22 54.69 21.00 2 1 22 7.70 17.70 2 1 22 27.90 33.00 2 1 22 -12.50 20.60 -2 1 -22 2.00 7.60 2 1 22 16.50 20.80 2 1 22 -6.30 13.30 -2 1 -22 31.20 13.90 2 1 22 12.20 32.10 -2 -2 22 38.40 16.00 2 -2 -22 35.70 17.00 -2 -2 22 44.60 15.80 2 -2 -22 38.40 16.30 -2 -2 22 -9.70 34.50 2 -2 -22 29.40 14.50 -2 -2 22 51.69 21.60 -2 -2 22 25.10 11.00 2 2 -22 48.10 15.70 -2 2 22 16.60 16.50 2 2 -22 71.39 20.60 -2 2 22 27.80 14.90 2 2 -22 8.40 6.80 -2 2 22 22.50 20.20 -2 2 22 8.10 40.20 1 -2 -22 12.60 16.80 1 -2 -22 13.90 15.80 -1 -2 22 -15.60 18.60 -1 -2 22 22.00 20.90 -1 -2 22 8.40 16.60 -1 -2 22 17.80 15.20 1 -2 -22 -20.80 19.80 -1 -2 22 -6.70 9.60 -1 2 22 13.50 18.00 1 2 -22 -22.20 9.70 1 2 -22 14.80 17.20 -1 2 22 9.90 20.10 -1 2 22 5.90 13.40 -1 2 22 -3.70 15.60 1 2 -22 6.40 15.20 -1 2 22 14.60 20.40 0 -2 22 0.20 18.90 0 -2 22 -17.30 14.90 0 -2 22 21.20 19.40 0 -2 -22 15.30 16.50 0 -2 -22 -38.00 16.40 0 -2 22 -2.60 17.10 0 -2 22 33.80 20.50 0 -2 -22 20.00 18.30 0 -2 -22 2.30 4.20 0 -2 22 15.10 10.50 0 2 22 9.10 20.30 0 2 22 15.10 19.50 0 2 -22 -3.30 3.80 0 2 -22 -6.60 15.30 0 2 -22 3.90 15.10 0 2 22 32.50 17.90 0 2 22 17.90 14.40 0 2 22 -0.10 19.30 0 2 -22 26.10 19.80 -1 -2 -22 2.60 7.90 1 -2 22 26.80 20.00 -1 -2 -22 18.60 18.30 -1 -2 -22 -6.40 19.10 -1 -2 -22 1.50 5.90 1 -2 22 18.20 22.30 -1 -2 -22 -5.80 17.70 1 -2 22 -16.80 10.10 1 -2 22 41.20 19.50 1 -2 22 -14.80 17.60 1 -2 22 -27.50 17.60 -1 -2 -22 -8.90 14.00 -1 2 -22 -6.50 17.40 1 2 22 9.50 21.30 1 2 22 4.10 17.50 1 2 22 2.70 20.40 1 2 22 -0.90 14.20 1 2 22 1.60 18.90 -1 2 -22 -5.10 16.70 -1 2 -22 1.10 18.60 1 2 22 27.20 19.40 -1 2 -22 -7.40 5.00 2 -2 22 -6.20 21.60 2 -2 22 0.00 17.00 -2 -2 -22 27.50 20.80 -2 -2 -22 7.70 14.50 2 -2 22 24.70 13.40 2 -2 22 46.10 20.40 2 -2 22 -8.10 19.10 -2 -2 -22 10.80 8.30 2 2 22 13.50 29.60 -2 2 -22 4.60 8.00 -2 2 -22 42.10 20.70 2 2 22 -10.30 18.40 -2 2 -22 2.60 10.50 2 2 22 -5.70 15.20 2 2 22 3.80 21.10 2 2 22 22.70 17.40 2 2 22 5.80 27.90 -2 -3 22 4.80 7.90 2 -3 -22 21.90 14.00 -2 -3 22 35.60 22.30 2 -3 -22 -32.50 22.10 -2 -3 22 -3.50 13.30 -2 -3 22 -7.40 14.00 2 -3 -22 -14.10 13.30 -2 -3 22 27.70 21.10 -2 3 22 -9.90 18.80 2 3 -22 8.60 13.80 -2 3 22 14.00 18.20 2 3 -22 1.90 6.40 -2 3 22 -11.80 26.60 2 3 -22 7.00 17.70 -2 3 22 20.20 23.40 -2 3 22 -8.00 14.00 -1 -3 22 4.60 8.40 -1 -3 22 -4.30 19.50 -1 -3 22 4.30 14.80 -1 -3 22 -15.20 20.80 -1 -3 22 -14.10 16.10 1 -3 -22 5.80 16.50 1 -3 -22 -5.10 16.00 1 -3 -22 14.10 18.20 1 3 -22 -4.60 8.30 -1 3 22 30.30 15.40 1 3 -22 0.50 1.80 -1 3 22 15.10 20.80 1 3 -22 -0.40 17.20 -1 3 22 9.60 19.60 -1 3 22 30.60 20.20 -1 3 22 -12.50 17.20 1 3 -22 -17.40 12.90 0 -3 22 8.60 9.30 0 -3 -22 7.80 18.20 0 -3 22 11.50 20.40 0 -3 -22 5.90 4.10 0 -3 22 13.80 18.20 0 -3 -22 26.80 17.70 0 -3 -22 -8.80 17.40 0 -3 -22 7.10 4.40 0 -3 22 10.90 21.40 0 -3 22 -13.60 17.60 0 -3 22 -11.30 15.50 0 3 -22 6.80 5.00 0 3 -22 1.20 13.60 0 3 22 13.10 19.20 0 3 22 -6.10 20.10 0 3 22 -1.30 17.80 0 3 -22 32.80 19.80 0 3 22 -26.00 17.20 0 3 -22 27.20 16.80 0 3 22 4.60 14.60 1 -3 22 -2.10 18.10 -1 -3 -22 25.70 21.60 1 -3 22 0.80 20.70 -1 -3 -22 16.20 19.70 -1 -3 -22 -10.60 5.30 -1 -3 -22 2.50 22.10 -1 -3 -22 1.50 15.40 1 -3 22 0.20 17.70 -1 -3 -22 16.90 8.90 1 -3 22 12.40 10.80 1 3 22 9.90 19.50 -1 3 -22 8.00 30.00 1 3 22 9.20 16.00 -1 3 -22 2.20 20.60 1 3 22 48.20 21.80 1 3 22 8.50 19.30 1 3 22 -14.10 29.70 -1 3 -22 26.50 18.50 -1 -4 22 20.60 7.00 1 -4 -22 4.40 18.60 -1 -4 22 32.10 16.80 -1 -4 22 25.70 28.50 1 -4 -22 7.90 17.80 1 -4 -22 -1.20 20.50 -1 -4 22 -22.70 17.90 -1 -4 22 5.70 20.40 -1 4 22 -26.80 16.90 1 4 -22 -2.20 7.70 1 4 -22 19.00 16.00 1 4 -22 5.70 17.50 -1 4 22 31.90 22.60 -1 4 22 16.20 16.70 1 4 -22 -0.90 3.40 -1 4 22 25.70 20.80 0 -4 22 11.10 21.10 0 -4 -22 0.70 4.00 0 -4 -22 -23.20 16.00 0 -4 22 29.90 30.00 0 -4 22 19.00 7.40 0 -4 22 -2.50 15.40 0 -4 -22 8.70 19.30 0 -4 22 20.20 22.00 0 4 22 25.30 32.70 0 4 -22 2.10 12.90 0 4 22 20.50 16.70 0 4 22 31.30 21.00 0 4 -22 -0.70 5.40 0 4 -22 15.10 15.80 0 4 22 39.40 21.00 0 4 -22 30.80 21.80 -1 -4 -22 -3.10 7.50 1 -4 22 -4.20 17.60 1 -4 22 1.70 20.80 -1 -4 -22 -11.30 18.50 1 -4 22 -2.20 19.00 -1 -4 -22 0.40 15.90 -1 4 -22 -0.50 6.60 1 4 22 -4.80 17.20 1 4 22 21.90 34.30 -1 4 -22 7.50 17.70 1 4 22 9.80 21.20 1 4 22 -32.10 17.40 -1 -5 22 4.90 18.60 0 -5 22 -17.80 20.00 0 -5 22 -16.50 19.50 0 -5 -22 4.50 4.60 0 5 22 8.50 19.20 0 5 -22 27.10 14.20 0 5 -22 4.30 5.90 0 5 22 -11.90 19.10 0 5 -22 17.40 25.40 0 5 22 7.20 16.30 -1 0 23 -5.10 26.00 1 0 -23 17.20 18.60 1 0 -23 -23.20 18.80 -1 0 23 26.40 21.60 1 0 -23 33.60 15.40 -1 0 23 6.80 17.60 -1 0 23 19.60 12.80 0 0 -23 1.30 3.80 0 0 -23 14.40 18.30 0 0 23 -30.50 16.50 0 0 23 -11.20 11.80 0 0 23 -25.90 23.40 0 0 -23 -12.90 17.80 0 0 23 -3.70 19.40 0 0 23 -10.40 17.20 0 0 -23 1.60 3.90 1 -1 -23 67.59 20.10 -1 -1 23 109.39 18.30 -1 -1 23 60.29 27.80 -1 -1 23 83.79 22.10 -1 -1 23 66.79 23.80 -1 -1 23 117.79 37.00 1 -1 -23 117.39 26.00 -1 1 23 54.49 23.30 1 1 -23 83.59 21.50 -1 1 23 89.69 17.00 -1 1 23 72.29 23.30 -1 1 23 91.79 23.10 0 -1 -23 -2.90 16.80 0 -1 23 -1.80 17.90 0 -1 23 14.30 12.10 0 -1 23 9.40 20.90 0 -1 23 32.90 38.80 0 -1 -23 -6.20 17.80 0 -1 23 3.30 20.30 0 1 23 6.20 14.20 0 1 23 26.70 19.80 0 1 23 -41.40 23.00 0 1 23 16.80 20.00 0 1 -23 18.80 16.40 0 1 23 -23.30 15.90 0 1 -23 28.30 25.50 0 -2 23 21.20 11.60 0 -2 23 34.80 18.60 0 -2 -23 -3.20 17.20 0 -2 -23 9.00 4.90 0 -2 23 46.50 20.40 0 -2 23 15.60 28.30 0 -2 -23 29.40 22.50 0 2 23 15.90 19.40 0 2 23 48.60 16.20 0 2 23 25.30 18.40 0 2 -23 7.60 4.30 0 2 23 38.60 21.40 0 2 -23 14.70 23.70 0 2 23 21.00 35.00 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 16467 _shelx_res_file ; TITL UMD1957E_a.res in P2(1)/n umd1957e_a.res created by SHELXL-2018/3 at 13:58:39 on 18-Mar-2020 REM Old TITL UMD1957E in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.171, Rweak 0.012, Alpha 0.030, Orientation as input REM Formula found by SHELXT: C16 N3 O REM COLORLESS CELL 0.71073 6.1444 12.8514 19.3315 90 91.626 90 ZERR 4 0.0006 0.0013 0.0019 0 0.003 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O UNIT 68 88 8 4 EQIV $1 0.5-X,-0.5+Y,0.5-Z DFIX 0.86 0.005 N1 H1 L.S. 10 PLAN 2 SIZE 0.03 0.1 0.3 TEMP 23 HTAB N1 N2_$1 CONF BOND $H LIST 6 HTAB 2 MORE -1 fmap 2 acta OMIT 3 2 16 OMIT 0 1 2 REM REM REM WGHT 0.042100 0.397500 EXTI 0.035662 FVAR 1.32386 O1 4 0.404701 0.314523 0.550902 11.00000 0.07428 0.07889 = 0.04889 -0.00736 -0.00492 0.00103 N1 3 0.048069 0.156466 0.309522 11.00000 0.04628 0.03882 = 0.05580 -0.00106 -0.00070 -0.00554 N2 3 0.717263 0.467402 0.224289 11.00000 0.03551 0.03526 = 0.04369 -0.00238 0.00043 -0.00107 C1 1 0.198825 0.188546 0.263176 11.00000 0.05377 0.03666 = 0.04747 -0.00162 0.00264 0.00075 AFIX 43 H1A 2 0.192685 0.173076 0.216165 11.00000 -1.20000 AFIX 0 C2 1 0.112024 0.192413 0.373884 11.00000 0.04181 0.03210 = 0.05105 0.00274 0.00006 0.00353 C3 1 0.019582 0.179297 0.438230 11.00000 0.04700 0.04447 = 0.05999 0.00840 0.00770 -0.00003 AFIX 43 H3 2 -0.109406 0.142352 0.442694 11.00000 -1.20000 AFIX 0 C4 1 0.124287 0.222424 0.494733 11.00000 0.05840 0.05615 = 0.04812 0.00890 0.00865 0.00972 AFIX 43 H4 2 0.064549 0.214786 0.538107 11.00000 -1.20000 AFIX 0 C5 1 0.319434 0.277834 0.488769 11.00000 0.05271 0.04722 = 0.04697 -0.00046 -0.00312 0.00949 C6 1 0.411532 0.292880 0.425533 11.00000 0.04320 0.03800 = 0.05424 -0.00099 -0.00077 0.00285 AFIX 43 H6 2 0.539720 0.330673 0.421748 11.00000 -1.20000 AFIX 0 C7 1 0.306251 0.249445 0.366677 11.00000 0.03941 0.02995 = 0.04824 0.00169 0.00110 0.00454 C8 1 0.359040 0.246115 0.294972 11.00000 0.04298 0.02843 = 0.05047 0.00013 0.00364 0.00372 C9 1 0.551784 0.294698 0.262051 11.00000 0.04698 0.03688 = 0.05862 0.00106 0.01130 0.00283 AFIX 23 H9A 2 0.572877 0.262073 0.217492 11.00000 -1.20000 H9B 2 0.680614 0.281261 0.290827 11.00000 -1.20000 AFIX 0 C10 1 0.527985 0.412156 0.251648 11.00000 0.03421 0.03641 = 0.04593 -0.00001 0.00011 0.00102 AFIX 23 H10A 2 0.404340 0.424296 0.220377 11.00000 -1.20000 H10B 2 0.493855 0.443084 0.295809 11.00000 -1.20000 AFIX 0 C11 1 0.907841 0.466787 0.272230 11.00000 0.03588 0.04369 = 0.05369 -0.00432 -0.00226 -0.00127 AFIX 23 H11A 2 1.029007 0.500425 0.250178 11.00000 -1.20000 H11B 2 0.949342 0.395345 0.281998 11.00000 -1.20000 AFIX 0 C12 1 0.864688 0.520925 0.338445 11.00000 0.04815 0.04013 = 0.05515 -0.00540 -0.00540 -0.00329 AFIX 43 H12 2 0.791552 0.584226 0.335903 11.00000 -1.20000 AFIX 0 C13 1 0.921464 0.486499 0.399762 11.00000 0.07017 0.06768 = 0.05594 -0.00510 -0.01221 0.00606 AFIX 93 H13A 2 0.994865 0.423490 0.404413 11.00000 -1.20000 H13B 2 0.888570 0.524946 0.438859 11.00000 -1.20000 AFIX 0 C14 1 0.773237 0.427456 0.155925 11.00000 0.04899 0.04818 = 0.04646 -0.00480 0.00349 -0.00832 AFIX 23 H14A 2 0.643138 0.426748 0.126309 11.00000 -1.20000 H14B 2 0.823752 0.356257 0.160826 11.00000 -1.20000 AFIX 0 C15 1 0.944443 0.490121 0.121919 11.00000 0.05774 0.05405 = 0.05046 -0.00025 0.00426 -0.01331 AFIX 43 H15 2 0.939074 0.562062 0.126783 11.00000 -1.20000 AFIX 0 C16 1 1.099829 0.451473 0.086146 11.00000 0.07705 0.08713 = 0.07685 -0.01933 0.02751 -0.03146 AFIX 93 H16A 2 1.110188 0.379848 0.080213 11.00000 -1.20000 H16B 2 1.201163 0.495318 0.066365 11.00000 -1.20000 AFIX 0 C17 1 0.604253 0.369141 0.549804 11.00000 0.07533 0.08925 = 0.06385 -0.01251 -0.01558 -0.00170 AFIX 137 H17A 2 0.641883 0.393335 0.595580 11.00000 -1.50000 H17B 2 0.589963 0.427531 0.519037 11.00000 -1.50000 H17C 2 0.716441 0.323651 0.534050 11.00000 -1.50000 AFIX 0 H1 2 -0.052509 0.111423 0.300065 11.00000 -1.20000 HKLF 4 REM UMD1957E_a.res in P2(1)/n REM wR2 = 0.1057, GooF = S = 1.050, Restrained GooF = 1.050 for all data REM R1 = 0.0408 for 2145 Fo > 4sig(Fo) and 0.0598 for all 2810 data REM 186 parameters refined using 1 restraints END WGHT 0.0421 0.3975 REM Instructions for potential hydrogen bonds HTAB N1 N2_$1 REM Highest difference peak 0.154, deepest hole -0.128, 1-sigma level 0.029 Q1 1 0.3207 0.2722 0.3330 11.00000 0.05 0.14 Q2 1 0.2210 0.2220 0.3768 11.00000 0.05 0.14 ; _shelx_res_checksum 90255 loop_ _space_group_symop_operation_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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.4047(2) 0.31452(11) 0.55090(6) 0.0675(4) Uani d 1 . . N N1 0.0481(2) 0.15647(10) 0.30952(7) 0.0470(4) Uani d 1 . . N N2 0.71726(19) 0.46740(9) 0.22429(6) 0.0382(3) Uani d 1 . . C C1 0.1988(3) 0.18855(12) 0.26318(9) 0.0459(4) Uani d 1 . . H H1A 0.192685 0.173076 0.216165 0.055 Uiso calc 1 . . C C2 0.1120(2) 0.19241(11) 0.37388(8) 0.0417(4) Uani d 1 . . C C3 0.0196(3) 0.17930(13) 0.43823(9) 0.0504(4) Uani d 1 . . H H3 -0.109406 0.142352 0.442694 0.060 Uiso calc 1 . . C C4 0.1243(3) 0.22242(14) 0.49473(9) 0.0541(5) Uani d 1 . . H H4 0.064549 0.214786 0.538107 0.065 Uiso calc 1 . . C C5 0.3194(3) 0.27783(13) 0.48877(9) 0.0491(4) Uani d 1 . . C C6 0.4115(3) 0.29288(12) 0.42553(8) 0.0452(4) Uani d 1 . . H H6 0.539720 0.330673 0.421748 0.054 Uiso calc 1 . . C C7 0.3063(2) 0.24944(11) 0.36668(8) 0.0392(4) Uani d 1 . . C C8 0.3590(2) 0.24612(11) 0.29497(8) 0.0406(4) Uani d 1 . . C C9 0.5518(3) 0.29470(12) 0.26205(9) 0.0473(4) Uani d 1 . . H H9A 0.572877 0.262073 0.217492 0.057 Uiso calc 1 . . H H9B 0.680614 0.281261 0.290827 0.057 Uiso calc 1 . . C C10 0.5280(2) 0.41216(11) 0.25165(8) 0.0389(4) Uani d 1 . . H H10A 0.404340 0.424296 0.220377 0.047 Uiso calc 1 . . H H10B 0.493855 0.443084 0.295809 0.047 Uiso calc 1 . . C C11 0.9078(2) 0.46679(13) 0.27223(8) 0.0445(4) Uani d 1 . . H H11A 1.029007 0.500425 0.250178 0.053 Uiso calc 1 . . H H11B 0.949342 0.395345 0.281998 0.053 Uiso calc 1 . . C C12 0.8647(3) 0.52092(13) 0.33844(9) 0.0479(4) Uani d 1 . . H H12 0.791552 0.584226 0.335903 0.058 Uiso calc 1 . . C C13 0.9215(3) 0.48650(16) 0.39976(10) 0.0649(5) Uani d 1 . . H H13A 0.994865 0.423490 0.404413 0.078 Uiso calc 1 . . H H13B 0.888570 0.524946 0.438859 0.078 Uiso calc 1 . . C C14 0.7732(3) 0.42746(13) 0.15593(8) 0.0478(4) Uani d 1 . . H H14A 0.643138 0.426748 0.126309 0.057 Uiso calc 1 . . H H14B 0.823752 0.356257 0.160826 0.057 Uiso calc 1 . . C C15 0.9444(3) 0.49012(14) 0.12192(9) 0.0540(5) Uani d 1 . . H H15 0.939074 0.562062 0.126783 0.065 Uiso calc 1 . . C C16 1.0998(4) 0.45147(19) 0.08615(11) 0.0799(7) Uani d 1 . . H H16A 1.110188 0.379848 0.080213 0.096 Uiso calc 1 . . H H16B 1.201163 0.495318 0.066365 0.096 Uiso calc 1 . . C C17 0.6043(4) 0.36914(19) 0.54980(11) 0.0765(6) Uani d 1 . . H H17A 0.641883 0.393335 0.595580 0.115 Uiso calc 1 . . H H17B 0.589963 0.427531 0.519037 0.115 Uiso calc 1 . . H H17C 0.716441 0.323651 0.534050 0.115 Uiso calc 1 . . H H1 -0.053(3) 0.1114(13) 0.3001(11) 0.092 Uiso d 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 0.0743(9) 0.0789(9) 0.0489(8) 0.0010(7) -0.0049(6) -0.0074(6) N1 0.0463(8) 0.0388(8) 0.0558(9) -0.0055(6) -0.0007(6) -0.0011(6) N2 0.0355(6) 0.0353(7) 0.0437(7) -0.0011(5) 0.0004(5) -0.0024(5) C1 0.0538(9) 0.0367(8) 0.0475(9) 0.0008(7) 0.0026(7) -0.0016(7) C2 0.0418(8) 0.0321(8) 0.0511(9) 0.0035(6) 0.0001(7) 0.0027(7) C3 0.0470(9) 0.0445(9) 0.0600(11) 0.0000(7) 0.0077(8) 0.0084(8) C4 0.0584(11) 0.0562(10) 0.0481(10) 0.0097(8) 0.0087(8) 0.0089(8) C5 0.0527(10) 0.0472(9) 0.0470(10) 0.0095(8) -0.0031(8) -0.0005(7) C6 0.0432(8) 0.0380(8) 0.0542(10) 0.0029(7) -0.0008(7) -0.0010(7) C7 0.0394(8) 0.0299(7) 0.0482(9) 0.0045(6) 0.0011(7) 0.0017(6) C8 0.0430(8) 0.0284(7) 0.0505(9) 0.0037(6) 0.0036(7) 0.0001(6) C9 0.0470(9) 0.0369(9) 0.0586(10) 0.0028(7) 0.0113(8) 0.0011(7) C10 0.0342(8) 0.0364(8) 0.0459(9) 0.0010(6) 0.0001(6) 0.0000(6) C11 0.0359(8) 0.0437(9) 0.0537(10) -0.0013(7) -0.0023(7) -0.0043(7) C12 0.0481(9) 0.0401(9) 0.0552(10) -0.0033(7) -0.0054(8) -0.0054(7) C13 0.0702(13) 0.0677(12) 0.0559(11) 0.0061(10) -0.0122(9) -0.0051(9) C14 0.0490(9) 0.0482(9) 0.0465(9) -0.0083(7) 0.0035(7) -0.0048(7) C15 0.0577(11) 0.0540(10) 0.0505(10) -0.0133(8) 0.0043(8) -0.0003(8) C16 0.0770(14) 0.0871(15) 0.0769(14) -0.0315(12) 0.0275(12) -0.0193(12) C17 0.0753(14) 0.0892(16) 0.0639(13) -0.0017(12) -0.0156(10) -0.0125(11) 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C5 O1 C17 . . 117.69(15) ? C1 N1 C2 . . 108.04(13) ? C1 N1 H1 . . 123.8(15) ? C2 N1 H1 . . 127.0(15) ? C11 N2 C10 . . 113.15(12) ? C14 N2 C10 . . 111.23(12) ? C14 N2 C11 . . 111.24(12) ? N1 C1 H1A . . 124.4 ? C8 C1 N1 . . 111.17(14) ? C8 C1 H1A . . 124.4 ? N1 C2 C3 . . 130.91(15) ? N1 C2 C7 . . 107.83(14) ? C3 C2 C7 . . 121.25(15) ? C2 C3 H3 . . 121.0 ? C4 C3 C2 . . 118.00(16) ? C4 C3 H3 . . 121.0 ? C3 C4 H4 . . 119.2 ? C3 C4 C5 . . 121.57(16) ? C5 C4 H4 . . 119.2 ? O1 C5 C4 . . 113.98(15) ? C6 C5 O1 . . 124.76(16) ? C6 C5 C4 . . 121.26(16) ? C5 C6 H6 . . 120.9 ? C5 C6 C7 . . 118.12(15) ? C7 C6 H6 . . 120.9 ? C2 C7 C8 . . 107.18(13) ? C6 C7 C2 . . 119.78(14) ? C6 C7 C8 . . 133.00(14) ? C1 C8 C7 . . 105.77(13) ? C1 C8 C9 . . 127.18(15) ? C7 C8 C9 . . 127.04(14) ? C8 C9 H9A . . 108.9 ? C8 C9 H9B . . 108.9 ? C8 C9 C10 . . 113.19(13) ? H9A C9 H9B . . 107.8 ? C10 C9 H9A . . 108.9 ? C10 C9 H9B . . 108.9 ? N2 C10 C9 . . 116.70(12) ? N2 C10 H10A . . 108.1 ? N2 C10 H10B . . 108.1 ? C9 C10 H10A . . 108.1 ? C9 C10 H10B . . 108.1 ? H10A C10 H10B . . 107.3 ? N2 C11 H11A . . 109.1 ? N2 C11 H11B . . 109.1 ? N2 C11 C12 . . 112.40(13) ? H11A C11 H11B . . 107.9 ? C12 C11 H11A . . 109.1 ? C12 C11 H11B . . 109.1 ? C11 C12 H12 . . 117.5 ? C13 C12 C11 . . 125.04(17) ? C13 C12 H12 . . 117.5 ? C12 C13 H13A . . 120.0 ? C12 C13 H13B . . 120.0 ? H13A C13 H13B . . 120.0 ? N2 C14 H14A . . 108.9 ? N2 C14 H14B . . 108.9 ? N2 C14 C15 . . 113.21(13) ? H14A C14 H14B . . 107.7 ? C15 C14 H14A . . 108.9 ? C15 C14 H14B . . 108.9 ? C14 C15 H15 . . 117.7 ? C16 C15 C14 . . 124.64(18) ? C16 C15 H15 . . 117.7 ? C15 C16 H16A . . 120.0 ? C15 C16 H16B . . 120.0 ? H16A C16 H16B . . 120.0 ? O1 C17 H17A . . 109.5 ? O1 C17 H17B . . 109.5 ? O1 C17 H17C . . 109.5 ? H17A C17 H17B . . 109.5 ? H17A C17 H17C . . 109.5 ? H17B C17 H17C . . 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 C5 . 1.380(2) ? O1 C17 . 1.414(2) ? N1 C1 . 1.370(2) ? N1 C2 . 1.374(2) ? N1 H1 . 0.863(5) ? N2 C10 . 1.4735(18) ? N2 C11 . 1.4726(19) ? N2 C14 . 1.4677(19) ? C1 H1A . 0.9300 ? C1 C8 . 1.364(2) ? C2 C3 . 1.392(2) ? C2 C7 . 1.411(2) ? C3 H3 . 0.9300 ? C3 C4 . 1.369(2) ? C4 H4 . 0.9300 ? C4 C5 . 1.402(2) ? C5 C6 . 1.375(2) ? C6 H6 . 0.9300 ? C6 C7 . 1.408(2) ? C7 C8 . 1.433(2) ? C8 C9 . 1.497(2) ? C9 H9A . 0.9700 ? C9 H9B . 0.9700 ? C9 C10 . 1.529(2) ? C10 H10A . 0.9700 ? C10 H10B . 0.9700 ? C11 H11A . 0.9700 ? C11 H11B . 0.9700 ? C11 C12 . 1.487(2) ? C12 H12 . 0.9300 ? C12 C13 . 1.303(2) ? C13 H13A . 0.9300 ? C13 H13B . 0.9300 ? C14 H14A . 0.9700 ? C14 H14B . 0.9700 ? C14 C15 . 1.492(2) ? C15 H15 . 0.9300 ? C15 C16 . 1.294(3) ? C16 H16A . 0.9300 ? C16 H16B . 0.9300 ? C17 H17A . 0.9600 ? C17 H17B . 0.9600 ? C17 H17C . 0.9600 ? 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 N1 H1 N2 2_545 0.863(5) 2.155(9) 2.9880(18) 162(2) 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 O1 C5 C6 C7 . . . . 179.25(14) ? N1 C1 C8 C7 . . . . 0.67(17) ? N1 C1 C8 C9 . . . . 179.97(14) ? N1 C2 C3 C4 . . . . 178.16(16) ? N1 C2 C7 C6 . . . . -178.18(13) ? N1 C2 C7 C8 . . . . -0.40(16) ? N2 C11 C12 C13 . . . . 135.82(18) ? N2 C14 C15 C16 . . . . 140.91(19) ? C1 N1 C2 C3 . . . . -178.24(16) ? C1 N1 C2 C7 . . . . 0.80(17) ? C1 C8 C9 C10 . . . . 103.67(18) ? C2 N1 C1 C8 . . . . -0.94(18) ? C2 C3 C4 C5 . . . . -0.3(2) ? C2 C7 C8 C1 . . . . -0.16(16) ? C2 C7 C8 C9 . . . . -179.46(14) ? C3 C2 C7 C6 . . . . 1.0(2) ? C3 C2 C7 C8 . . . . 178.75(14) ? C3 C4 C5 O1 . . . . -178.99(15) ? C3 C4 C5 C6 . . . . 1.3(3) ? C4 C5 C6 C7 . . . . -1.1(2) ? C5 C6 C7 C2 . . . . 0.0(2) ? C5 C6 C7 C8 . . . . -177.13(15) ? C6 C7 C8 C1 . . . . 177.21(16) ? C6 C7 C8 C9 . . . . -2.1(3) ? C7 C2 C3 C4 . . . . -0.8(2) ? C7 C8 C9 C10 . . . . -77.2(2) ? C8 C9 C10 N2 . . . . 175.60(13) ? C10 N2 C11 C12 . . . . -62.30(17) ? C10 N2 C14 C15 . . . . 172.28(13) ? C11 N2 C10 C9 . . . . -65.85(17) ? C11 N2 C14 C15 . . . . -60.60(18) ? C14 N2 C10 C9 . . . . 60.23(18) ? C14 N2 C11 C12 . . . . 171.63(13) ? C17 O1 C5 C4 . . . . 178.50(16) ? C17 O1 C5 C6 . . . . -1.8(2) ? _cod_database_fobs_code 1557817