#------------------------------------------------------------------------------ #$Date: 2023-08-16 04:47:53 +0300 (Wed, 16 Aug 2023) $ #$Revision: 285783 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/28/2022836.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_2022836 loop_ _publ_author_name 'Decato, Daniel' 'Jahnke, Michael' 'Berryman, Orion' _publ_section_title ; Conformational polymorphism of 3-(azidomethyl)benzoic acid ; _journal_coeditor_code EQ3010 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C Structural Chemistry' _journal_paper_doi 10.1107/S2053229623006824 _journal_volume 79 _journal_year 2023 _chemical_formula_iupac 'C8 H7 N3 O2' _chemical_formula_moiety 'C8 H7 N3 O2' _chemical_formula_sum 'C8 H7 N3 O2' _chemical_formula_weight 177.17 _chemical_name_systematic ; 3-(Azidomethyl)benzoic acid ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_method ;FinalCif V117 by Daniel Kratzert, Freiburg 2023, https://dkratzert.de/finalcif.html ; _cell_angle_alpha 66.828(2) _cell_angle_beta 82.168(3) _cell_angle_gamma 82.245(2) _cell_formula_units_Z 2 _cell_length_a 3.8029(2) _cell_length_b 9.9199(5) _cell_length_c 11.5709(6) _cell_measurement_reflns_used 4919 _cell_measurement_temperature 100 _cell_measurement_theta_max 24.989 _cell_measurement_theta_min 3.468 _cell_volume 395.96(4) _computing_cell_refinement ; SAINT (Bruker, 2016) ; _computing_data_collection ; APEX4 (Bruker, 2021) ; _computing_data_reduction ; SAINT (Bruker, 2016) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2018 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100 _diffrn_detector 'Bruker Photon II' _diffrn_detector_area_resol_mean 7.39 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device 'Fixed Chi Three-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE DUO' _diffrn_measurement_method '\w and \f scans' _diffrn_measurement_specimen_support 'MiTeGen micromount' _diffrn_radiation_monochromator 'TRIUMPH graphite' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_unetI/netI 0.0215 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 10604 _diffrn_reflns_theta_full 25.078 _diffrn_reflns_theta_max 25.078 _diffrn_reflns_theta_min 2.330 _diffrn_source 'sealed tube' _diffrn_source_current 30.0 _diffrn_source_power 1.35 _diffrn_source_voltage 45.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.111 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.6922 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.486 _exptl_crystal_description plate _exptl_crystal_F_000 184 _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.282 _refine_diff_density_min -0.221 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 122 _refine_ls_number_reflns 1405 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.051 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0357 _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^)+(0.0480P)^2^+0.1860P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0898 _refine_ls_wR_factor_ref 0.0960 _reflns_number_gt 1196 _reflns_number_total 1405 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file eq3010sup1.cif _cod_data_source_block C _cod_database_code 2022836 _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 0.966 _shelx_estimated_absorpt_t_max 0.999 _shelx_hkl_file ; -1 0 0 9999.00 309.37 -2 0 0 270.97 13.00 -2 0 0 224.58 16.90 -2 0 0 252.47 16.60 -2 0 0 265.17 13.10 2 0 0 248.88 16.00 2 0 0 236.68 12.60 2 0 0 253.47 13.20 2 0 0 257.27 15.50 2 0 0 226.48 14.90 -3 0 0 578.14 23.30 -3 0 0 553.94 23.50 -3 0 0 559.24 27.90 -3 0 0 568.64 26.50 3 0 0 611.54 26.60 3 0 0 534.35 26.40 3 0 0 597.64 23.80 3 0 0 588.54 23.60 3 0 0 565.44 26.70 -4 0 0 134.99 17.20 -4 0 0 103.29 13.40 -4 0 0 111.29 14.80 -4 0 0 127.59 19.70 4 0 0 136.19 15.90 4 0 0 142.79 19.10 4 0 0 110.59 15.80 4 0 0 129.99 14.60 4 -1 0 97.49 16.00 4 -1 0 79.69 15.20 4 -1 0 101.79 12.90 4 -1 0 107.49 14.00 -4 1 0 82.89 15.80 -4 1 0 129.39 18.30 3 -1 0 -2.10 9.70 3 -1 0 10.50 6.30 3 -1 0 3.50 10.40 3 -1 0 9.30 9.60 3 -1 0 11.10 6.70 -3 1 0 -3.60 6.30 -3 1 0 10.70 5.30 -3 1 0 13.40 8.80 -3 1 0 5.80 11.50 -3 1 0 -4.00 10.70 2 -1 0 599.44 25.00 2 -1 0 577.54 23.60 2 -1 0 629.64 21.50 2 -1 0 573.84 24.30 2 -1 0 603.04 21.50 -2 1 0 633.64 21.90 -2 1 0 579.94 23.10 -2 1 0 595.14 25.10 -2 1 0 599.44 25.50 1 -1 0 1525.35 46.10 1 -1 0 1480.85 47.80 1 -1 0 1435.86 46.50 1 -1 0 1522.95 46.10 1 -1 0 1415.36 47.20 1 -1 0 1422.66 48.00 -1 1 0 1484.75 46.20 -1 1 0 1446.26 46.40 -1 1 0 1423.36 48.60 -1 1 0 1535.15 46.30 -1 1 0 1487.95 48.20 -1 1 0 1402.16 47.00 -1 -1 0 3821.02 119.09 -1 -1 0 3825.72 118.69 -1 -1 0 3775.82 118.59 -1 -1 0 3509.75 118.19 -1 -1 0 3588.64 118.29 -1 -1 0 3865.91 118.59 1 1 0 3720.73 118.39 1 1 0 3854.11 119.09 1 1 0 3920.91 118.59 1 1 0 3914.01 118.69 1 1 0 3836.32 118.49 -2 -1 0 290.07 14.20 -2 -1 0 285.37 16.90 -2 -1 0 290.67 17.50 -2 -1 0 279.27 14.90 2 1 0 256.07 14.50 2 1 0 252.37 15.50 2 1 0 256.17 15.80 2 1 0 267.17 17.00 -3 -1 0 376.96 18.50 -3 -1 0 433.66 22.50 -3 -1 0 384.96 19.50 -3 -1 0 395.16 23.40 -3 -1 0 442.96 25.00 3 1 0 391.96 18.90 3 1 0 363.86 21.40 3 1 0 439.26 23.00 3 1 0 365.76 21.70 3 1 0 354.96 19.20 -4 -1 0 21.30 11.50 -4 -1 0 6.90 16.50 -4 -1 0 24.70 14.70 -4 -1 0 9.50 8.10 4 1 0 15.50 13.20 4 1 0 11.80 10.80 4 1 0 -17.50 11.80 4 1 0 25.90 14.30 4 -2 0 8.30 6.50 4 -2 0 -12.60 12.10 4 -2 0 -2.30 6.80 4 -2 0 -27.90 12.50 -4 2 0 -8.50 13.40 -4 2 0 13.10 15.50 -4 2 0 20.50 8.10 -4 2 0 11.80 14.40 3 -2 0 239.28 18.30 3 -2 0 223.08 11.60 3 -2 0 213.18 18.00 3 -2 0 228.88 12.10 -3 2 0 221.08 18.00 -3 2 0 197.08 21.50 -3 2 0 236.48 12.70 -3 2 0 253.77 12.80 -3 2 0 258.67 19.50 2 -2 0 23.10 8.50 2 -2 0 36.30 3.90 2 -2 0 26.10 3.80 2 -2 0 37.00 8.10 -2 2 0 46.60 8.90 -2 2 0 28.10 4.80 -2 2 0 32.20 4.70 -2 2 0 29.20 8.60 1 -2 0 211.08 11.90 1 -2 0 226.48 11.80 1 -2 0 216.48 11.70 -1 2 0 206.98 10.80 -1 2 0 220.68 13.40 -1 2 0 226.98 12.30 -1 2 0 212.58 12.30 0 -2 0 630.64 22.40 0 -2 0 643.54 23.00 0 -2 0 661.23 21.50 0 -2 0 671.83 21.50 0 2 0 627.14 21.50 0 2 0 629.54 22.50 0 2 0 624.34 21.50 0 2 0 631.74 22.10 0 2 0 631.34 21.30 -1 -2 0 163.48 9.40 -1 -2 0 142.89 13.20 -1 -2 0 169.08 10.50 -1 -2 0 178.28 13.80 -1 -2 0 147.49 14.00 -1 -2 0 168.98 10.70 1 2 0 178.38 11.20 1 2 0 177.38 11.30 1 2 0 170.58 13.00 1 2 0 175.98 12.50 1 2 0 175.28 11.60 1 2 0 177.18 9.00 -2 -2 0 251.67 14.50 -2 -2 0 256.57 15.10 -2 -2 0 244.38 16.00 -2 -2 0 244.78 17.30 2 2 0 253.97 14.60 2 2 0 263.07 14.70 2 2 0 280.77 15.70 2 2 0 252.27 16.80 2 2 0 249.28 16.60 -3 -2 0 247.58 21.10 -3 -2 0 216.88 16.60 -3 -2 0 246.38 20.00 -3 -2 0 183.88 16.70 3 2 0 215.58 16.80 3 2 0 223.58 19.40 3 2 0 253.37 16.60 3 2 0 191.38 21.00 3 2 0 201.38 17.40 -4 -2 0 109.29 14.30 -4 -2 0 114.39 19.00 -4 -2 0 85.79 16.90 -4 -2 0 108.79 15.00 4 2 0 100.09 16.60 4 2 0 94.19 12.90 4 2 0 99.99 15.80 4 2 0 96.99 15.10 4 -3 0 6.10 14.50 4 -3 0 6.90 12.60 -4 3 0 11.70 12.50 -4 3 0 31.40 13.70 -4 3 0 8.40 6.50 -4 3 0 23.80 17.00 3 -3 0 140.09 18.50 3 -3 0 145.29 16.70 -3 3 0 185.28 18.90 -3 3 0 169.98 10.40 -3 3 0 196.08 20.30 -3 3 0 163.58 17.70 -3 3 0 174.28 10.30 2 -3 0 2508.95 83.89 2 -3 0 2559.24 82.09 2 -3 0 2449.55 82.99 -2 3 0 2716.73 80.39 -2 3 0 2570.64 84.49 -2 3 0 2516.75 84.49 -2 3 0 2661.03 80.29 1 -3 0 17.10 6.90 1 -3 0 28.10 7.50 1 -3 0 7.90 7.10 -1 3 0 12.90 7.00 -1 3 0 8.20 6.90 0 -3 0 590.44 22.00 0 -3 0 568.84 22.30 0 -3 0 608.44 20.40 0 -3 0 579.54 20.50 0 3 0 573.24 20.00 0 3 0 559.94 20.20 0 3 0 568.24 20.50 0 3 0 570.54 22.00 -1 -3 0 7814.42 232.88 -1 -3 0 7712.33 232.58 -1 -3 0 7050.19 231.28 -1 -3 0 6786.92 232.38 -1 -3 0 7699.53 231.18 -1 -3 0 7767.72 230.78 1 3 0 7784.12 231.38 1 3 0 7104.49 231.88 1 3 0 6743.73 232.18 1 3 0 7619.84 232.58 1 3 0 7713.73 232.58 1 3 0 7671.23 232.38 -2 -3 0 19.40 8.10 -2 -3 0 19.90 7.70 -2 -3 0 3.90 7.50 -2 -3 0 27.40 10.20 2 3 0 18.50 8.10 2 3 0 20.10 6.60 2 3 0 23.30 9.60 2 3 0 17.30 7.60 2 3 0 0.00 8.60 -3 -3 0 18.60 12.40 -3 -3 0 16.10 8.90 -3 -3 0 7.80 11.80 -3 -3 0 9.60 10.40 -3 -3 0 33.30 11.50 3 3 0 23.70 8.60 3 3 0 11.30 8.30 3 3 0 1.10 9.60 3 3 0 20.40 11.10 -4 -3 0 21.10 15.00 -4 -3 0 8.70 16.10 -4 -3 0 14.90 9.00 -4 -3 0 39.40 12.60 4 3 0 27.80 16.10 4 3 0 24.90 11.40 4 3 0 22.90 12.90 4 -4 0 7.00 14.50 4 -4 0 28.10 13.40 -4 4 0 22.30 16.00 -4 4 0 45.70 13.80 -4 4 0 8.90 14.10 -4 4 0 30.30 5.80 3 -4 0 24.20 11.90 -3 4 0 27.70 11.20 -3 4 0 28.60 11.90 -3 4 0 19.10 4.00 2 -4 0 90.39 9.60 2 -4 0 103.99 13.40 2 -4 0 118.79 13.50 -2 4 0 94.99 13.20 -2 4 0 110.99 11.80 -2 4 0 102.79 12.80 1 -4 0 93.59 9.60 1 -4 0 84.19 9.70 1 -4 0 92.39 9.60 -1 4 0 84.99 10.60 -1 4 0 97.09 11.40 0 -4 0 4671.73 147.29 0 -4 0 4579.44 146.29 0 -4 0 4665.43 147.19 0 -4 0 4623.44 147.29 0 4 0 4986.80 146.69 0 4 0 4701.83 147.29 0 4 0 4620.94 146.39 0 4 0 4658.63 146.49 -1 -4 0 1097.19 37.90 -1 -4 0 1043.80 35.30 -1 -4 0 1023.30 36.20 -1 -4 0 981.10 36.20 1 4 0 1032.50 34.30 1 4 0 1045.20 36.70 1 4 0 1034.50 36.30 1 4 0 931.71 35.60 1 4 0 1060.79 36.90 -2 -4 0 725.63 28.90 -2 -4 0 718.83 28.30 -2 -4 0 702.63 29.60 -2 -4 0 694.53 26.40 -2 -4 0 689.83 24.60 -2 -4 0 620.24 27.20 2 4 0 690.13 28.10 2 4 0 635.14 27.30 2 4 0 689.53 26.60 2 4 0 727.23 29.30 2 4 0 692.03 29.50 -3 -4 0 41.80 13.70 -3 -4 0 27.60 10.80 -3 -4 0 44.40 10.50 -3 -4 0 40.90 12.40 -3 -4 0 52.79 10.80 3 4 0 52.79 12.40 3 4 0 36.80 11.20 3 4 0 30.60 9.80 3 4 0 32.50 13.60 3 4 0 44.00 10.00 -4 -4 0 28.50 17.20 -4 -4 0 66.39 18.20 4 4 0 76.59 14.80 4 4 0 49.99 14.30 4 4 0 71.49 13.40 4 4 0 56.29 16.90 3 -5 0 419.56 24.90 3 -5 0 457.45 25.80 -3 5 0 448.76 27.10 -3 5 0 453.55 24.20 -3 5 0 439.16 25.00 2 -5 0 2.00 9.60 2 -5 0 11.30 9.40 2 -5 0 0.10 9.40 -2 5 0 3.10 8.00 -2 5 0 3.30 8.30 -2 5 0 7.50 8.50 -2 5 0 -8.70 8.60 1 -5 0 88.29 10.00 -1 5 0 80.89 8.90 -1 5 0 73.99 10.20 -1 5 0 84.99 9.90 -1 5 0 74.79 5.60 -1 5 0 69.89 5.50 0 -5 0 133.69 9.50 0 -5 0 105.49 13.30 0 -5 0 127.39 12.60 0 -5 0 121.09 9.60 0 5 0 125.89 13.00 0 5 0 131.29 10.60 0 5 0 117.49 9.00 0 5 0 119.19 9.70 -1 -5 0 461.45 22.80 -1 -5 0 441.36 19.80 -1 -5 0 452.65 19.70 -1 -5 0 442.36 20.50 1 5 0 477.05 20.50 1 5 0 443.96 21.40 1 5 0 454.75 17.70 1 5 0 442.36 21.20 1 5 0 438.86 19.80 -2 -5 0 658.73 24.60 -2 -5 0 641.64 27.80 -2 -5 0 679.33 24.90 -2 -5 0 656.73 28.00 -2 -5 0 681.83 29.90 -2 -5 0 647.54 25.00 2 5 0 664.53 25.30 2 5 0 599.44 26.90 2 5 0 619.44 29.30 2 5 0 676.53 29.30 -3 -5 0 203.08 18.00 -3 -5 0 245.28 19.40 -3 -5 0 237.68 18.80 -3 -5 0 216.58 20.60 3 5 0 269.17 18.70 3 5 0 262.37 24.10 3 5 0 244.78 19.10 3 5 0 263.87 16.90 3 5 0 236.78 20.60 -4 -5 0 46.00 17.50 -4 -5 0 34.10 17.00 -4 -5 0 39.40 11.70 4 5 0 29.90 13.50 4 5 0 44.80 17.40 4 5 0 31.80 11.30 4 5 0 28.20 15.50 3 -6 0 73.99 13.70 3 -6 0 54.09 14.60 -3 6 0 68.39 14.30 -3 6 0 41.00 12.10 -3 6 0 59.59 12.10 -3 6 0 47.60 11.50 2 -6 0 7.00 10.20 2 -6 0 9.00 9.90 -2 6 0 1.60 8.50 -2 6 0 0.20 9.60 -2 6 0 7.50 8.60 -2 6 0 3.40 11.20 1 -6 0 921.61 35.30 -1 6 0 950.90 30.70 -1 6 0 936.91 30.60 -1 6 0 928.61 35.10 -1 6 0 906.71 33.10 0 -6 0 277.97 17.10 0 -6 0 279.27 13.90 0 -6 0 276.07 18.10 0 6 0 285.07 14.20 0 6 0 282.57 17.40 0 6 0 276.57 17.60 0 6 0 280.17 13.50 0 6 0 277.17 14.60 -1 -6 0 342.57 17.90 -1 -6 0 310.47 19.30 -1 -6 0 280.97 16.40 -1 -6 0 299.07 17.20 1 6 0 330.77 19.00 1 6 0 311.97 16.80 1 6 0 285.77 18.80 1 6 0 321.57 14.20 1 6 0 334.67 17.60 -2 -6 0 9.30 7.50 -2 -6 0 3.90 9.10 -2 -6 0 13.10 7.00 -2 -6 0 2.80 12.50 -2 -6 0 8.10 9.40 -2 -6 0 8.30 9.00 2 6 0 4.30 9.50 2 6 0 4.80 7.60 2 6 0 -0.40 10.90 2 6 0 -9.20 11.80 2 6 0 -3.40 8.70 -3 -6 0 1823.72 68.69 -3 -6 0 1887.61 66.99 -3 -6 0 1809.72 66.99 -3 -6 0 1864.21 63.39 -3 -6 0 1930.11 64.09 3 6 0 1871.71 66.79 3 6 0 1844.22 67.69 3 6 0 1860.01 66.59 3 6 0 1901.31 64.39 3 -7 0 731.13 34.80 3 -7 0 714.13 33.50 -3 7 0 698.13 31.30 -3 7 0 733.03 33.90 -3 7 0 716.33 33.30 -3 7 0 659.23 32.50 2 -7 0 387.06 23.40 -2 7 0 378.66 23.20 -2 7 0 385.06 23.10 -2 7 0 360.16 21.90 -2 7 0 367.16 21.20 1 -7 0 109.19 13.50 -1 7 0 135.09 13.30 -1 7 0 115.39 11.40 -1 7 0 130.29 8.30 -1 7 0 126.39 8.60 -1 7 0 112.99 16.40 0 -7 0 218.08 18.80 0 -7 0 216.38 13.10 0 -7 0 235.88 17.60 0 7 0 216.08 12.30 0 7 0 229.48 14.50 0 7 0 226.08 17.70 0 7 0 236.28 13.30 -1 -7 0 33.90 13.40 -1 -7 0 36.40 13.00 -1 -7 0 61.29 9.50 1 7 0 26.40 11.90 1 7 0 44.90 7.10 1 7 0 25.60 10.90 1 7 0 44.30 8.10 -2 -7 0 49.80 11.20 -2 -7 0 46.50 10.80 -2 -7 0 19.40 13.90 -2 -7 0 50.29 10.90 2 7 0 48.80 14.60 2 7 0 26.70 12.90 2 7 0 45.10 8.90 2 7 0 40.30 9.90 2 7 0 42.70 10.40 -3 -7 0 1032.00 42.90 -3 -7 0 1050.49 45.50 -3 -7 0 1102.19 48.00 -3 -7 0 944.91 42.70 3 7 0 1024.50 42.40 3 7 0 978.50 45.60 3 7 0 1000.20 43.30 3 7 0 1012.10 42.50 3 7 0 1091.39 39.60 2 -8 0 37.10 13.20 -2 8 0 51.69 13.20 -2 8 0 49.10 11.70 -2 8 0 63.89 11.00 -2 8 0 56.39 11.80 1 -8 0 567.34 29.70 -1 8 0 609.34 25.60 -1 8 0 604.14 22.30 -1 8 0 619.64 22.40 -1 8 0 606.64 24.00 -1 8 0 616.24 24.90 -1 8 0 611.24 28.30 0 -8 0 478.75 25.00 0 -8 0 441.66 19.90 0 -8 0 459.05 25.70 0 -8 0 442.86 19.80 0 8 0 435.76 20.60 0 8 0 468.25 25.60 0 8 0 463.95 25.10 0 8 0 445.56 20.00 -1 -8 0 6.40 11.40 -1 -8 0 1.20 8.60 -1 -8 0 -5.90 4.60 -1 -8 0 -0.90 13.60 1 8 0 9.20 11.50 1 8 0 -0.20 7.80 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554.34 27.00 0 -2 -12 516.05 30.20 0 -2 -12 534.75 31.30 0 -2 -12 567.04 29.10 0 -2 -12 528.95 32.80 0 -2 -12 582.74 29.10 0 2 12 564.34 31.10 0 2 12 543.85 29.20 0 2 12 594.64 32.40 0 2 12 539.75 28.90 0 2 12 503.25 36.00 -1 -2 -12 2.30 12.00 -1 -2 -12 -3.60 9.80 -1 -2 -12 -2.60 14.20 -1 -2 -12 14.80 14.40 1 2 12 -9.20 19.40 1 2 12 5.20 16.90 -2 -2 -12 49.70 11.50 -2 -2 -12 38.80 16.60 -2 -2 -12 24.50 16.00 -2 -2 -12 51.69 14.40 2 2 12 57.59 14.40 2 2 12 34.80 19.00 2 2 12 12.60 17.90 1 -3 -12 158.78 19.10 1 -3 -12 137.09 16.30 1 -3 -12 116.89 15.90 1 -3 -12 106.19 17.00 -1 3 12 109.19 15.00 -1 3 12 147.29 19.10 -1 3 12 160.58 27.10 -1 3 12 169.18 22.50 0 -3 -12 413.36 27.00 0 -3 -12 408.56 26.90 0 -3 -12 397.76 25.10 0 -3 -12 439.36 24.80 0 -3 -12 402.06 25.20 0 3 12 422.26 23.90 0 3 12 383.86 29.90 0 3 12 452.05 27.80 0 3 12 435.46 33.80 0 3 12 403.36 25.80 -1 -3 -12 1468.25 57.59 -1 -3 -12 1603.84 58.69 -1 -3 -12 1705.63 60.79 -1 -3 -12 1670.13 60.79 -1 -3 -12 1651.93 60.29 1 3 12 1617.64 60.99 1 3 12 1713.43 61.99 1 3 12 1680.83 64.39 -2 -3 -12 300.77 26.00 -2 -3 -12 313.07 24.20 -2 -3 -12 270.47 25.70 2 3 12 306.77 28.20 2 3 12 287.67 24.10 2 3 12 330.17 33.00 1 -4 -12 106.99 19.40 1 -4 -12 195.38 20.10 1 -4 -12 158.38 18.00 1 -4 -12 178.38 23.20 -1 4 12 128.89 24.80 -1 4 12 150.08 22.30 0 -4 -12 91.29 14.60 0 -4 -12 163.98 20.90 0 -4 -12 136.29 14.70 0 -4 -12 134.89 16.30 0 -4 -12 149.19 14.80 0 -4 -12 138.39 18.70 0 4 12 172.18 22.00 0 4 12 106.99 14.80 0 4 12 123.49 23.60 0 4 12 119.39 22.30 -1 -4 -12 89.69 15.70 -1 -4 -12 123.99 15.10 -1 -4 -12 97.79 13.70 -1 -4 -12 138.49 18.80 -1 -4 -12 163.18 14.50 1 4 12 134.39 21.80 1 4 12 135.99 21.50 1 4 12 172.08 20.00 1 4 12 119.19 16.60 -2 -4 -12 47.30 12.90 -2 -4 -12 21.70 12.50 -2 -4 -12 6.90 13.70 -2 -4 -12 14.00 17.00 2 4 12 24.30 19.10 2 4 12 38.10 13.90 2 4 12 1.10 19.00 1 -5 -12 186.58 23.20 1 -5 -12 181.98 22.10 1 -5 -12 161.48 19.60 1 -5 -12 194.68 20.70 -1 5 12 123.19 22.90 -1 5 12 180.18 19.30 -1 5 12 177.98 27.40 0 -5 -12 99.29 13.50 0 -5 -12 102.69 15.10 0 -5 -12 81.99 13.60 0 -5 -12 92.99 15.00 0 5 12 112.69 21.80 0 5 12 88.59 23.00 0 5 12 70.59 13.10 0 5 12 80.29 14.80 -1 -5 -12 -23.70 11.70 -1 -5 -12 3.20 8.80 -1 -5 -12 5.40 10.70 -1 -5 -12 25.90 11.70 -1 -5 -12 -17.60 12.60 -1 -5 -12 -1.30 9.60 -1 -5 -12 29.40 11.20 1 5 12 24.40 13.90 1 5 12 23.40 11.60 1 5 12 -2.50 18.60 1 5 12 -11.80 18.50 -2 -5 -12 141.49 17.00 -2 -5 -12 170.38 18.50 -2 -5 -12 180.48 18.10 -2 -5 -12 162.08 18.20 2 5 12 157.78 22.00 2 5 12 110.89 23.10 1 -6 -12 96.49 16.30 1 -6 -12 108.39 13.70 1 -6 -12 114.89 17.30 -1 6 12 104.29 13.70 -1 6 12 90.99 23.20 -1 6 12 67.79 25.50 0 -6 -12 328.97 24.70 0 -6 -12 271.97 23.60 0 -6 -12 295.47 21.60 0 6 12 272.97 22.60 0 6 12 305.87 34.20 0 6 12 326.47 32.50 -1 -6 -12 7.90 13.30 -1 -6 -12 32.60 11.80 -1 -6 -12 37.90 13.30 -1 -6 -12 -0.10 13.90 1 6 12 25.70 20.00 1 6 12 19.60 14.20 1 6 12 1.80 10.80 1 6 12 13.20 17.30 -2 -6 -12 34.80 15.10 -2 -6 -12 50.49 12.70 -2 -6 -12 31.00 14.80 2 6 12 38.50 15.20 2 6 12 3.20 19.10 2 6 12 -0.60 18.30 1 -7 -12 8.00 15.40 1 -7 -12 13.70 11.20 1 -7 -12 31.30 15.30 1 -7 -12 34.40 14.70 -1 7 12 33.40 22.60 -1 7 12 30.00 9.80 -1 7 12 -11.30 21.90 0 -7 -12 206.88 22.00 0 -7 -12 221.48 22.10 0 -7 -12 224.28 23.00 0 7 12 141.89 23.90 0 7 12 184.88 26.00 -1 -7 -12 385.96 27.20 -1 -7 -12 438.66 24.70 -1 -7 -12 473.45 28.20 1 7 12 452.85 33.50 1 7 12 407.76 25.00 1 7 12 416.16 34.10 -2 -7 -12 19.20 12.50 -2 -7 -12 32.00 14.30 2 7 12 55.09 20.70 2 7 12 51.09 15.60 2 7 12 48.40 17.30 0 -8 -12 249.97 25.00 0 -8 -12 286.27 21.90 0 -8 -12 272.57 27.00 0 8 12 279.27 33.60 0 8 12 183.28 27.40 0 8 12 236.98 19.20 -1 -8 -12 134.49 17.40 1 8 12 92.99 23.50 1 8 12 113.69 20.00 -2 -8 -12 -15.70 13.50 -2 -8 -12 9.10 17.40 2 8 12 5.90 16.80 2 8 12 7.50 20.50 0 -9 -12 -18.70 15.50 0 -9 -12 -10.60 10.50 0 -9 -12 -1.00 13.60 0 -9 -12 -10.40 12.90 0 9 12 23.40 24.80 0 9 12 -4.20 9.00 0 9 12 0.00 20.20 -1 -9 -12 306.67 25.00 -1 -9 -12 277.97 21.90 1 9 12 239.08 31.80 1 9 12 276.47 28.80 1 9 12 270.17 23.10 0 -1 -13 39.90 14.60 0 -1 -13 8.50 13.70 0 -1 -13 12.10 11.00 0 -1 -13 2.10 16.00 0 1 13 18.50 17.30 0 1 13 5.40 15.50 0 1 13 -1.10 20.10 0 1 13 35.90 15.50 -1 -1 -13 36.80 17.50 0 -2 -13 92.29 18.20 0 -2 -13 98.69 13.40 0 2 13 85.69 22.60 0 2 13 112.49 21.70 0 2 13 88.09 17.30 0 2 13 102.29 17.10 -1 -2 -13 560.04 36.10 -1 -2 -13 639.14 34.60 1 2 13 616.94 38.50 1 2 13 605.54 33.10 1 2 13 641.34 33.70 0 -3 -13 89.69 14.00 0 -3 -13 76.19 14.90 0 -3 -13 76.89 13.70 0 -3 -13 103.09 17.20 0 3 13 102.89 20.50 0 3 13 85.39 15.30 0 3 13 80.99 22.80 0 3 13 60.09 17.20 -1 -3 -13 541.55 29.30 -1 -3 -13 494.25 32.20 -1 -3 -13 612.54 33.10 -1 -3 -13 587.84 29.00 1 3 13 585.54 32.80 1 3 13 562.54 32.90 1 3 13 553.64 36.90 0 -4 -13 45.50 14.50 0 -4 -13 11.30 14.20 0 -4 -13 -7.80 14.10 0 -4 -13 38.10 13.20 0 4 13 42.50 21.70 0 4 13 -4.80 11.50 0 4 13 11.20 20.70 -1 -4 -13 50.59 20.50 -1 -4 -13 33.30 15.40 1 4 13 45.40 15.30 1 4 13 59.29 20.60 1 4 13 19.30 19.20 -2 -4 -13 337.47 27.10 -2 -4 -13 281.37 28.30 -2 -4 -13 374.66 25.30 -2 -4 -13 358.86 23.90 2 4 13 343.67 31.70 2 4 13 314.17 31.60 2 4 13 307.27 25.70 0 -5 -13 46.50 12.80 0 -5 -13 28.70 12.00 0 -5 -13 34.40 16.00 0 -5 -13 45.50 13.40 0 5 13 45.30 23.40 0 5 13 -4.30 22.80 -1 -5 -13 -1.60 14.10 -1 -5 -13 8.70 14.00 -1 -5 -13 17.10 11.10 -1 -5 -13 -2.30 11.60 1 5 13 37.50 21.20 1 5 13 44.90 15.50 1 5 13 9.50 19.30 -2 -5 -13 -11.10 14.20 -2 -5 -13 19.80 15.80 2 5 13 8.50 17.90 2 5 13 46.00 20.50 2 5 13 -13.90 13.60 0 -6 -13 73.39 15.90 0 -6 -13 90.29 15.90 0 -6 -13 59.09 14.30 0 -6 -13 83.49 13.70 0 6 13 86.09 25.50 0 6 13 90.99 22.90 -1 -6 -13 100.29 16.80 -1 -6 -13 98.39 12.80 -1 -6 -13 60.79 14.40 -1 -6 -13 83.39 14.30 1 6 13 67.19 20.20 1 6 13 80.49 22.10 0 -7 -13 23.10 15.70 0 -7 -13 26.00 13.10 0 -7 -13 48.70 15.40 0 -7 -13 12.60 11.40 0 7 13 42.60 14.00 0 7 13 18.00 23.60 0 7 13 18.60 20.90 -1 -7 -13 34.30 15.50 -1 -7 -13 2.00 12.10 -1 -7 -13 16.10 11.80 -1 -7 -13 0.60 11.30 1 7 13 23.90 13.90 1 7 13 16.30 18.70 1 7 13 14.80 22.10 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 69851 _shelx_res_file ; TITL umt_dd8_bp_a.res in P-1 umt_dd8_bp.res created by SHELXL-2018/3 at 20:01:00 on 31-Jul-2023 REM Old TITL UMT_DD8_BP in P-1 REM SHELXT solution in P-1: R1 0.115, Rweak 0.005, Alpha 0.025 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C10 N O2 CELL 0.71073 3.8029 9.9199 11.5709 66.828 82.168 82.245 ZERR 2 0.0002 0.0005 0.0006 0.002 0.003 0.002 LATT 1 SFAC C H N O UNIT 16 14 6 4 EQIV $1 -X,2-Y,1-Z L.S. 10 PLAN 1 SIZE 0.01 0.12 0.31 TEMP -173.15 CONF HTAB O2 O1_$1 BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.048000 0.186000 FVAR 2.20401 O1 4 0.032575 0.838270 0.490823 11.00000 0.02328 0.01678 = 0.01932 -0.00878 0.00299 -0.00118 O2 4 0.290419 1.037894 0.354579 11.00000 0.02989 0.01495 = 0.02375 -0.01045 0.00678 -0.00298 H2 2 0.186132 1.077752 0.410222 11.00000 0.05374 N1 3 0.335941 0.400723 0.212566 11.00000 0.02332 0.02374 = 0.03574 -0.01982 -0.00499 0.00190 N2 3 0.562510 0.334941 0.161592 11.00000 0.02555 0.02068 = 0.02140 -0.00843 -0.00045 -0.00725 N3 3 0.744260 0.274906 0.107687 11.00000 0.03394 0.04108 = 0.03248 -0.02502 0.00852 -0.00961 C1 1 0.388802 0.822688 0.309908 11.00000 0.01368 0.01820 = 0.01836 -0.00925 -0.00396 0.00149 C2 1 0.351063 0.673374 0.347075 11.00000 0.01225 0.02069 = 0.01692 -0.00846 -0.00114 0.00063 AFIX 43 H2A 2 0.223831 0.622462 0.425784 11.00000 -1.20000 AFIX 0 C3 1 0.497040 0.597996 0.270545 11.00000 0.01231 0.01905 = 0.02206 -0.01074 -0.00476 0.00195 C4 1 0.681147 0.675467 0.154898 11.00000 0.01442 0.02462 = 0.02040 -0.01358 -0.00123 0.00126 AFIX 43 H4 2 0.783049 0.625313 0.101590 11.00000 -1.20000 AFIX 0 C5 1 0.717152 0.823383 0.117010 11.00000 0.01693 0.02332 = 0.01789 -0.00890 0.00124 -0.00099 AFIX 43 H5 2 0.841506 0.874346 0.037700 11.00000 -1.20000 AFIX 0 C6 1 0.573009 0.898573 0.193890 11.00000 0.01704 0.01820 = 0.02044 -0.00807 -0.00283 0.00022 AFIX 43 H6 2 0.599376 1.000494 0.167874 11.00000 -1.20000 AFIX 0 C7 1 0.221961 0.899694 0.393148 11.00000 0.01488 0.01680 = 0.01784 -0.00742 -0.00311 0.00111 C8 1 0.460603 0.436093 0.312714 11.00000 0.01865 0.02086 = 0.02205 -0.01110 0.00114 -0.00202 AFIX 23 H8A 2 0.694016 0.380445 0.335739 11.00000 -1.20000 H8B 2 0.289201 0.404683 0.388834 11.00000 -1.20000 AFIX 0 HKLF 4 REM umt_dd8_bp_a.res in P-1 REM wR2 = 0.0960, GooF = S = 1.051, Restrained GooF = 1.051 for all data REM R1 = 0.0357 for 1196 Fo > 4sig(Fo) and 0.0455 for all 1405 data REM 122 parameters refined using 0 restraints END WGHT 0.0480 0.1860 REM Highest difference peak 0.282, deepest hole -0.221, 1-sigma level 0.046 Q1 1 1.0602 0.2445 0.0584 11.00000 0.05 0.28 ; _shelx_res_checksum 66856 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.0326(3) 0.83827(12) 0.49082(10) 0.0198(3) Uani d 1 . . O O2 0.2904(3) 1.03789(12) 0.35458(11) 0.0227(3) Uani d 1 . . H H2 0.186(6) 1.078(3) 0.410(2) 0.054(7) Uiso d 1 . . N N1 0.3359(4) 0.40072(15) 0.21257(14) 0.0251(4) Uani d 1 . . N N2 0.5625(4) 0.33494(15) 0.16159(13) 0.0221(3) Uani d 1 . . N N3 0.7443(4) 0.27491(18) 0.10769(15) 0.0329(4) Uani d 1 . . C C1 0.3888(4) 0.82269(17) 0.30991(14) 0.0161(3) Uani d 1 . . C C2 0.3511(4) 0.67337(17) 0.34707(14) 0.0164(3) Uani d 1 . . H H2A 0.223831 0.622462 0.425784 0.020 Uiso calc 1 . . C C3 0.4970(4) 0.59800(17) 0.27054(14) 0.0169(3) Uani d 1 . . C C4 0.6811(4) 0.67547(18) 0.15490(15) 0.0186(4) Uani d 1 . . H H4 0.783049 0.625313 0.101590 0.022 Uiso calc 1 . . C C5 0.7172(4) 0.82338(18) 0.11701(15) 0.0194(4) Uani d 1 . . H H5 0.841506 0.874346 0.037700 0.023 Uiso calc 1 . . C C6 0.5730(4) 0.89857(18) 0.19389(15) 0.0184(4) Uani d 1 . . H H6 0.599376 1.000494 0.167874 0.022 Uiso calc 1 . . C C7 0.2220(4) 0.89969(17) 0.39315(14) 0.0163(3) Uani d 1 . . C C8 0.4606(4) 0.43609(17) 0.31271(15) 0.0199(4) Uani d 1 . . H H8A 0.694016 0.380445 0.335739 0.024 Uiso calc 1 . . H H8B 0.289201 0.404683 0.388834 0.024 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 0.0233(6) 0.0168(6) 0.0193(6) -0.0012(4) 0.0030(5) -0.0088(5) O2 0.0299(6) 0.0149(6) 0.0238(6) -0.0030(5) 0.0068(5) -0.0104(5) N1 0.0233(7) 0.0237(8) 0.0357(8) 0.0019(6) -0.0050(6) -0.0198(7) N2 0.0256(7) 0.0207(7) 0.0214(7) -0.0072(6) -0.0005(6) -0.0084(6) N3 0.0339(9) 0.0411(10) 0.0325(8) -0.0096(7) 0.0085(7) -0.0250(8) C1 0.0137(7) 0.0182(8) 0.0184(8) 0.0015(6) -0.0040(6) -0.0092(6) C2 0.0122(7) 0.0207(8) 0.0169(8) 0.0006(6) -0.0011(6) -0.0085(6) C3 0.0123(7) 0.0190(8) 0.0221(8) 0.0019(6) -0.0048(6) -0.0107(6) C4 0.0144(7) 0.0246(9) 0.0204(8) 0.0013(6) -0.0012(6) -0.0136(7) C5 0.0169(7) 0.0233(9) 0.0179(8) -0.0010(6) 0.0012(6) -0.0089(7) C6 0.0170(7) 0.0182(8) 0.0204(8) 0.0002(6) -0.0028(6) -0.0081(7) C7 0.0149(7) 0.0168(8) 0.0178(8) 0.0011(6) -0.0031(6) -0.0074(6) C8 0.0187(8) 0.0209(9) 0.0220(8) -0.0020(6) 0.0011(6) -0.0111(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C7 O2 H2 . . 110.5(15) ? N2 N1 C8 . . 115.34(13) ? N3 N2 N1 . . 173.10(16) ? C2 C1 C6 . . 119.94(14) ? C2 C1 C7 . . 119.07(13) ? C6 C1 C7 . . 120.97(13) ? C1 C2 H2A . . 119.6 ? C3 C2 C1 . . 120.81(14) ? C3 C2 H2A . . 119.6 ? C2 C3 C4 . . 118.53(14) ? C2 C3 C8 . . 120.37(14) ? C4 C3 C8 . . 121.10(14) ? C3 C4 H4 . . 119.5 ? C5 C4 C3 . . 121.01(14) ? C5 C4 H4 . . 119.5 ? C4 C5 H5 . . 119.8 ? C4 C5 C6 . . 120.46(14) ? C6 C5 H5 . . 119.8 ? C1 C6 H6 . . 120.4 ? C5 C6 C1 . . 119.25(15) ? C5 C6 H6 . . 120.4 ? O1 C7 O2 . . 122.90(14) ? O1 C7 C1 . . 122.22(13) ? O2 C7 C1 . . 114.88(13) ? N1 C8 C3 . . 111.77(13) ? N1 C8 H8A . . 109.3 ? N1 C8 H8B . . 109.3 ? C3 C8 H8A . . 109.3 ? C3 C8 H8B . . 109.3 ? H8A C8 H8B . . 107.9 ? 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 C7 . 1.2337(18) ? O2 H2 . 0.90(3) ? O2 C7 . 1.3151(19) ? N1 N2 . 1.2364(19) ? N1 C8 . 1.485(2) ? N2 N3 . 1.1337(19) ? C1 C2 . 1.392(2) ? C1 C6 . 1.397(2) ? C1 C7 . 1.482(2) ? C2 H2A . 0.9500 ? C2 C3 . 1.388(2) ? C3 C4 . 1.397(2) ? C3 C8 . 1.504(2) ? C4 H4 . 0.9500 ? C4 C5 . 1.377(2) ? C5 H5 . 0.9500 ? C5 C6 . 1.388(2) ? C6 H6 . 0.9500 ? C8 H8A . 0.9900 ? C8 H8B . 0.9900 ? 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 O2 H2 O1 2_576 0.90(3) 1.73(3) 2.6346(15) 176(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 N2 N1 C8 C3 . . . . 108.18(15) ? C1 C2 C3 C4 . . . . -0.4(2) ? C1 C2 C3 C8 . . . . 178.84(13) ? C2 C1 C6 C5 . . . . -0.1(2) ? C2 C1 C7 O1 . . . . -4.4(2) ? C2 C1 C7 O2 . . . . 175.81(13) ? C2 C3 C4 C5 . . . . -0.2(2) ? C2 C3 C8 N1 . . . . 131.44(14) ? C3 C4 C5 C6 . . . . 0.6(2) ? C4 C3 C8 N1 . . . . -49.36(18) ? C4 C5 C6 C1 . . . . -0.4(2) ? C6 C1 C2 C3 . . . . 0.5(2) ? C6 C1 C7 O1 . . . . 173.70(14) ? C6 C1 C7 O2 . . . . -6.1(2) ? C7 C1 C2 C3 . . . . 178.66(13) ? C7 C1 C6 C5 . . . . -178.22(13) ? C8 C3 C4 C5 . . . . -179.37(14) ? _cod_database_fobs_code 2022836