#------------------------------------------------------------------------------ #$Date: 2023-08-16 04:47:53 +0300 (Wed, 16 Aug 2023) $ #$Revision: 285783 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/28/2022835.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_2022835 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 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 _atom_sites_solution_primary direct _audit_creation_method ;FinalCif V117 by Daniel Kratzert, Freiburg 2023, https://dkratzert.de/finalcif.html ; _cell_angle_alpha 90 _cell_angle_beta 93.099(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 3.7712(3) _cell_length_b 6.1229(5) _cell_length_c 34.868(3) _cell_measurement_reflns_used 5546 _cell_measurement_temperature 100 _cell_measurement_theta_max 26.195 _cell_measurement_theta_min 3.378 _cell_volume 803.95(11) _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) and SHELXS (Sheldrick, 2008) ; _diffrn_ambient_temperature 100 _diffrn_detector 'Bruker Photon II' _diffrn_detector_area_resol_mean 7.39 _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.964 _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 0.0363 _diffrn_reflns_av_unetI/netI 0.0372 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_number 10613 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.374 _diffrn_reflns_theta_min 2.925 _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 0.110 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6824 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.464 _exptl_crystal_description plate _exptl_crystal_F_000 368 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.254 _refine_diff_density_min -0.233 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 123 _refine_ls_number_reflns 1656 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.132 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0434 _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^)+(0.0299P)^2^+0.3387P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0803 _refine_ls_wR_factor_ref 0.0851 _reflns_number_gt 1411 _reflns_number_total 1656 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file eq3010sup1.cif _cod_data_source_block B _cod_original_cell_volume 803.96(11) _cod_database_code 2022835 _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 0.970 _shelx_estimated_absorpt_t_max 0.998 _shelx_hkl_file ; 1 0 0 52.94 1.47 1 0 0 48.76 1.77 1 0 0 50.39 1.61 -1 0 0 51.09 1.64 1 0 0 49.53 1.62 -1 0 0 49.47 1.65 -1 0 0 50.94 1.46 -1 0 0 52.00 1.72 -2 0 0 21.15 1.46 -2 0 0 22.73 1.27 -2 0 0 20.91 1.32 -2 0 0 21.81 0.97 2 0 0 22.40 1.06 2 0 0 22.84 1.30 2 0 0 22.69 1.46 2 0 0 22.75 1.25 3 0 0 4.35 0.89 -3 0 0 5.16 1.05 -3 0 0 4.11 0.97 -3 0 0 4.44 0.87 3 0 0 2.87 0.67 3 0 0 5.54 1.31 4 0 0 36.58 2.73 0 -1 0 -0.21 0.26 0 -1 0 0.28 0.45 0 -1 0 0.45 0.32 0 -1 0 0.86 0.41 0 1 0 -0.22 0.30 0 1 0 0.17 0.48 0 1 0 0.62 0.45 1 -1 0 865.58 21.06 -1 -1 0 865.40 21.07 -1 -1 0 855.95 20.88 1 -1 0 813.78 20.92 1 -1 0 836.88 21.03 -1 -1 0 874.14 20.94 -1 -1 0 839.17 21.04 1 -1 0 834.96 20.95 -1 1 0 859.44 20.97 -1 1 0 818.38 20.92 1 1 0 836.31 20.88 -1 1 0 855.67 21.04 1 1 0 866.29 21.08 -1 1 0 859.33 21.07 1 1 0 848.51 21.04 1 1 0 844.93 20.92 -2 -1 0 253.78 6.83 2 -1 0 252.02 6.62 2 -1 0 265.74 6.93 -2 -1 0 258.31 6.60 2 -1 0 250.50 6.65 2 -1 0 255.59 6.80 2 -1 0 257.73 6.57 -2 -1 0 251.53 6.86 -2 -1 0 258.52 6.54 -2 1 0 255.59 6.67 2 1 0 250.03 6.78 2 1 0 257.29 6.54 -2 1 0 259.87 6.77 -2 1 0 254.57 6.84 2 1 0 261.31 6.89 2 1 0 254.16 6.59 -3 -1 0 32.02 1.90 -3 -1 0 27.15 1.23 -3 -1 0 28.80 1.48 3 -1 0 30.13 1.26 3 -1 0 27.76 2.12 3 -1 0 30.54 1.60 3 1 0 29.15 2.12 -3 1 0 32.36 1.73 3 1 0 30.20 1.64 3 1 0 29.94 1.40 -3 1 0 25.60 1.84 -3 1 0 31.81 1.65 4 -1 0 -0.22 1.62 4 1 0 1.77 1.61 0 -2 0 43.57 1.58 0 -2 0 42.06 1.50 0 -2 0 40.87 1.25 0 -2 0 41.71 1.32 0 -2 0 40.20 1.53 0 2 0 39.34 1.21 0 2 0 41.51 1.54 0 2 0 40.02 1.30 1 -2 0 46.23 1.65 1 -2 0 49.02 1.72 -1 -2 0 47.45 1.60 -1 -2 0 43.00 1.92 1 -2 0 46.65 1.81 -1 -2 0 47.74 1.76 1 2 0 45.07 1.65 -1 2 0 47.25 1.65 1 2 0 47.57 1.78 1 2 0 49.86 1.61 -2 -2 0 194.10 5.34 2 -2 0 193.29 5.12 -2 -2 0 192.93 4.93 2 -2 0 195.46 5.50 2 -2 0 185.48 5.03 2 -2 0 190.67 5.17 -2 -2 0 191.49 5.09 2 -2 0 191.50 5.29 -2 -2 0 197.53 5.38 -2 2 0 193.40 5.14 -2 2 0 189.26 5.36 2 2 0 200.52 5.41 -2 2 0 189.42 5.03 2 2 0 191.18 5.04 2 2 0 185.18 5.28 -2 2 0 191.32 5.29 3 -2 0 17.91 2.01 -3 -2 0 17.13 1.83 -3 -2 0 15.73 1.13 3 -2 0 17.78 1.15 3 -2 0 19.80 1.34 -3 2 0 14.58 1.59 3 2 0 18.81 1.89 -3 2 0 19.27 1.37 3 2 0 17.63 1.10 4 -2 0 0.74 1.78 4 2 0 2.80 1.51 0 -3 0 0.37 0.61 0 -3 0 0.05 0.67 0 -3 0 0.08 0.42 0 -3 0 0.67 0.77 0 -3 0 -0.58 0.47 0 3 0 -0.35 0.49 0 3 0 -0.04 0.36 0 3 0 1.10 0.68 1 -3 0 105.43 3.20 -1 -3 0 106.10 3.14 -1 -3 0 102.65 2.99 1 -3 0 102.16 3.04 1 -3 0 99.31 3.03 -1 -3 0 103.18 3.02 1 3 0 100.30 2.98 1 3 0 104.63 3.14 -1 3 0 101.50 3.09 -1 3 0 102.24 3.04 1 3 0 99.95 2.96 -1 3 0 101.94 3.03 -2 -3 0 9.01 1.14 -2 -3 0 9.36 1.36 2 -3 0 8.51 1.07 2 -3 0 8.86 1.21 -2 -3 0 8.77 1.18 2 -3 0 12.30 1.30 2 3 0 8.67 1.10 -2 3 0 8.26 1.05 2 3 0 8.59 1.07 -2 3 0 8.10 1.17 -2 3 0 9.41 1.21 3 -3 0 35.67 1.69 3 -3 0 38.96 2.06 3 3 0 40.98 2.29 3 3 0 37.32 1.53 4 -3 0 10.60 1.98 4 3 0 12.94 2.05 0 -4 0 70.01 2.44 0 -4 0 71.54 2.14 0 -4 0 75.34 2.51 0 -4 0 68.80 2.40 0 4 0 71.64 2.12 0 4 0 70.85 2.38 1 -4 0 33.62 1.60 1 -4 0 35.38 1.55 -1 -4 0 31.08 1.64 -1 -4 0 32.70 1.56 1 -4 0 33.27 1.85 -1 4 0 32.99 1.52 -1 4 0 32.24 1.59 1 4 0 33.60 1.72 1 4 0 33.66 1.54 -1 4 0 32.73 1.57 1 4 0 34.38 1.42 -2 -4 0 4.53 1.05 2 -4 0 5.30 0.92 -2 -4 0 5.61 0.96 2 -4 0 5.04 1.29 -2 -4 0 4.61 1.13 2 4 0 5.67 1.03 -2 4 0 3.60 0.92 2 4 0 6.91 1.16 -2 4 0 7.13 1.00 2 4 0 5.25 0.89 3 -4 0 10.60 1.74 3 4 0 11.12 1.51 4 -4 0 4.39 2.07 4 4 0 4.81 1.68 0 -5 0 1.42 1.00 0 -5 0 -0.45 0.80 0 -5 0 0.03 0.71 0 -5 0 -0.09 0.61 0 5 0 -0.32 0.75 1 -5 0 2.25 1.09 -1 -5 0 3.06 1.02 -1 -5 0 2.85 0.92 1 -5 0 3.57 0.85 1 -5 0 3.45 0.84 -1 -5 0 5.30 0.92 1 5 0 1.28 1.05 -1 5 0 5.77 1.01 1 5 0 4.24 0.73 1 5 0 3.35 0.92 2 5 0 4.14 0.91 2 5 0 4.00 1.30 3 -5 0 -0.39 1.57 3 5 0 2.51 1.52 -3 5 0 2.52 1.11 0 -6 0 2.43 1.28 0 6 0 3.05 0.97 1 -6 0 10.20 1.53 -1 -6 0 9.58 1.41 1 6 0 10.58 1.41 -1 6 0 11.05 1.44 2 -6 0 7.72 1.68 2 6 0 12.74 1.81 2 6 0 9.03 1.16 0 -7 0 1.16 1.45 1 -7 0 4.48 1.57 -1 -7 0 5.64 1.59 4 0 -1 0.17 1.70 -3 0 1 9.14 1.21 3 0 -1 7.02 1.29 3 0 -1 10.05 1.08 -3 0 1 9.92 1.20 3 0 -1 9.37 0.78 -3 0 1 10.91 1.18 2 0 -1 0.90 0.56 2 0 -1 1.25 0.71 2 0 -1 -0.37 0.95 -2 0 1 1.56 0.86 -2 0 1 1.32 0.73 -2 0 1 1.73 0.73 2 0 -1 0.91 0.44 2 0 -1 1.07 0.70 1 0 -1 41.88 1.62 -1 0 1 39.72 1.57 1 0 -1 38.63 1.44 1 0 -1 40.41 1.38 -1 0 1 40.02 1.51 1 0 -1 43.59 1.21 -1 0 1 41.82 1.40 -1 0 1 41.41 1.20 -1 0 -1 784.16 19.47 1 0 1 779.38 19.39 1 0 1 820.42 19.36 -1 0 -1 773.30 19.39 1 0 1 764.71 19.42 -1 0 -1 802.22 19.35 -1 0 -1 766.44 19.42 2 0 1 0.11 0.68 -2 0 -1 0.02 0.76 2 0 1 0.06 0.68 2 0 1 -0.73 0.64 2 0 1 0.98 0.99 -2 0 -1 0.61 0.53 -2 0 -1 0.33 0.80 -2 0 -1 0.54 0.69 -3 0 -1 0.54 0.75 3 0 1 0.81 0.85 -3 0 -1 -0.74 0.78 -3 0 -1 0.83 0.99 3 0 1 0.17 0.58 3 0 1 -0.08 1.20 4 0 1 -2.15 1.45 4 -1 -1 2.20 1.64 4 1 -1 1.31 1.47 3 -1 -1 22.59 1.11 -3 -1 1 23.99 1.39 3 -1 -1 23.21 1.44 -3 -1 1 22.14 1.05 -3 -1 1 20.72 1.77 -3 -1 1 17.71 1.62 3 -1 -1 22.62 1.93 3 1 -1 22.92 1.15 3 1 -1 23.73 1.96 -3 1 1 23.42 1.61 -3 1 1 18.27 1.71 3 1 -1 22.46 1.48 -3 1 1 20.47 1.49 2 -1 -1 9.86 1.00 -2 -1 1 9.65 0.74 2 -1 -1 9.10 1.20 -2 -1 1 10.35 0.99 -2 -1 1 9.51 1.28 2 -1 -1 12.16 0.92 2 -1 -1 9.28 0.80 2 -1 -1 9.35 1.11 -2 -1 1 12.49 1.35 -2 1 1 10.54 1.28 2 1 -1 9.65 1.07 2 1 -1 9.64 0.82 2 1 -1 9.64 1.36 -2 1 1 10.82 1.19 2 1 -1 10.60 0.93 -2 1 1 11.18 0.99 -1 -1 1 834.79 20.55 1 -1 -1 844.32 20.55 -1 -1 1 817.32 20.37 1 -1 -1 826.68 20.43 1 -1 -1 805.71 20.51 1 -1 -1 792.79 20.40 -1 -1 1 822.28 20.53 -1 -1 1 862.77 20.40 -1 1 1 840.67 20.43 1 1 -1 827.08 20.39 1 1 -1 841.02 20.55 -1 1 1 827.45 20.52 -1 1 1 814.27 20.40 1 1 -1 818.67 20.51 -1 1 1 831.12 20.53 0 -1 -1 5.24 0.61 0 -1 1 4.92 0.54 0 -1 1 4.23 0.41 0 -1 1 3.91 0.44 0 -1 1 4.95 0.51 0 -1 -1 4.45 0.45 0 -1 -1 4.64 0.53 0 -1 -1 5.04 0.46 0 1 -1 4.78 0.63 0 1 -1 4.20 0.48 0 1 1 4.89 0.51 0 1 -1 4.52 0.49 0 1 1 4.81 0.48 0 1 1 4.00 0.58 -1 -1 -1 197.19 5.15 -1 -1 -1 195.53 4.92 1 -1 1 191.24 4.98 1 -1 1 196.24 5.11 -1 -1 -1 195.68 5.14 -1 -1 -1 200.76 5.02 1 -1 1 195.69 5.02 1 -1 1 199.71 5.16 -1 1 -1 191.60 4.98 1 1 1 198.85 5.01 1 1 1 193.53 5.10 1 1 1 194.36 5.14 -1 1 -1 192.11 5.11 -1 1 -1 196.90 5.04 1 1 1 192.12 4.92 -1 1 -1 195.85 5.13 2 -1 1 50.67 2.15 2 -1 1 47.40 1.59 2 -1 1 47.24 1.69 -2 -1 -1 47.83 1.65 2 -1 1 49.63 1.83 -2 -1 -1 43.40 1.55 -2 -1 -1 46.97 2.02 -2 -1 -1 43.56 1.99 2 -1 1 48.97 1.68 -2 1 -1 50.30 1.86 -2 1 -1 50.88 1.99 2 1 1 46.75 1.84 2 1 1 46.55 1.63 2 1 1 46.13 1.95 -2 1 -1 48.94 1.77 2 1 1 45.60 1.59 3 -1 1 10.32 1.22 3 -1 1 9.85 0.93 -3 -1 -1 8.98 1.25 -3 -1 -1 8.42 1.12 3 -1 1 8.80 1.52 -3 1 -1 10.28 1.37 3 1 1 8.23 1.10 3 1 1 8.57 1.40 3 1 1 8.64 1.19 -3 1 -1 5.98 1.13 4 -1 1 -1.91 1.59 4 1 1 2.37 1.67 4 -2 -1 4.15 1.72 4 2 -1 3.14 1.60 3 -2 -1 70.48 2.41 3 -2 -1 70.19 2.28 -3 -2 1 71.27 2.26 -3 -2 1 72.76 2.88 3 -2 -1 65.77 3.11 -3 2 1 70.41 2.44 3 2 -1 67.20 2.91 3 2 -1 70.11 2.16 2 -2 -1 55.43 2.29 -2 -2 1 60.16 2.22 -2 -2 1 62.34 1.77 2 -2 -1 57.25 1.89 2 -2 -1 54.92 2.17 2 -2 -1 57.74 1.95 -2 -2 1 61.34 2.28 -2 -2 1 61.38 1.92 2 2 -1 60.56 2.12 -2 2 1 60.05 2.17 2 2 -1 59.68 2.28 -2 2 1 55.84 1.84 -2 2 1 59.77 1.95 -2 2 1 53.42 2.19 2 2 -1 59.63 1.84 -1 -2 1 40.54 1.87 -1 -2 1 47.59 1.56 1 -2 -1 47.29 1.71 1 -2 -1 46.77 1.79 1 -2 -1 45.07 1.62 -1 -2 1 46.42 1.76 1 2 -1 47.18 1.77 1 2 -1 46.55 1.68 -1 2 1 46.38 1.63 1 2 -1 49.14 1.57 0 -2 1 19.74 0.81 0 -2 1 20.70 1.18 0 -2 1 21.68 1.11 0 -2 1 19.75 0.88 0 -2 -1 21.35 1.07 0 -2 -1 20.06 1.13 0 -2 -1 19.67 0.90 0 -2 -1 19.39 0.82 0 -2 -1 19.42 1.07 0 -2 1 18.88 1.18 0 2 -1 18.42 1.15 0 2 -1 19.61 0.76 0 2 1 20.06 0.77 0 2 1 19.57 1.17 0 2 1 20.01 0.85 0 2 -1 19.54 0.88 1 -2 1 80.70 2.41 -1 -2 -1 82.55 2.39 1 -2 1 81.00 2.55 -1 -2 -1 79.08 2.70 1 -2 1 85.58 2.49 -1 -2 -1 79.82 2.46 1 2 1 76.26 2.38 1 2 1 81.97 2.47 1 2 1 78.66 2.33 -1 2 -1 71.11 3.19 -1 2 -1 81.42 2.42 -1 2 -1 82.73 2.70 -2 -2 -1 107.20 3.34 -2 -2 -1 108.62 3.35 2 -2 1 105.84 3.43 2 -2 1 108.30 3.11 2 -2 1 104.17 2.96 -2 -2 -1 104.67 2.83 2 -2 1 106.68 3.19 2 -2 1 107.83 3.05 -2 -2 -1 99.12 3.05 2 2 1 102.81 3.29 -2 2 -1 110.34 3.26 2 2 1 103.22 3.21 -2 2 -1 104.89 3.29 2 2 1 103.72 2.99 -2 2 -1 104.02 2.95 3 -2 1 15.09 1.22 3 -2 1 15.13 2.08 -3 -2 -1 14.85 1.77 3 -2 1 11.66 1.10 3 -2 1 13.13 1.39 3 2 1 14.84 1.06 -3 2 -1 14.99 1.31 3 2 1 12.55 1.53 4 -2 1 4.57 1.82 4 2 1 6.75 1.84 4 -3 -1 34.29 3.12 4 3 -1 32.63 2.71 3 -3 -1 23.30 1.35 3 -3 -1 22.50 1.65 3 3 -1 20.15 1.86 3 3 -1 17.44 1.91 -2 -3 1 8.41 1.19 2 -3 -1 9.55 1.06 2 -3 -1 11.82 1.21 -2 -3 1 10.05 1.18 -2 -3 1 10.59 1.09 2 -3 -1 8.98 1.27 2 3 -1 8.64 0.98 -2 3 1 8.46 1.00 2 3 -1 10.90 1.11 -2 3 1 11.63 1.08 -2 3 1 9.90 1.18 2 3 -1 10.79 1.38 1 -3 -1 88.80 2.74 -1 -3 1 92.90 2.77 -1 -3 1 93.36 2.72 1 -3 -1 88.72 2.74 -1 -3 1 88.43 2.83 1 -3 -1 89.97 2.90 -1 3 1 89.73 2.75 1 3 -1 93.16 2.87 1 3 -1 88.99 2.66 1 3 -1 90.94 2.70 -1 3 1 89.82 2.81 -1 3 1 89.88 2.74 0 -3 1 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1.52 2 -2 34 3.24 1.52 -2 -2 -34 6.26 1.41 -2 2 -34 4.51 1.53 2 2 34 4.48 1.75 -2 3 34 7.69 1.64 -1 -3 34 3.98 1.66 1 -3 -34 3.75 1.33 0 -3 34 8.35 1.20 0 -3 -34 6.06 1.42 0 3 -34 7.00 1.46 0 3 34 7.68 1.43 1 -3 34 -0.27 1.16 -1 -3 -34 0.97 1.31 1 3 34 0.59 1.43 -1 3 -34 -0.77 1.33 2 -3 34 3.20 1.44 2 3 34 2.26 1.64 -1 -4 34 6.00 1.59 1 -4 -34 4.03 1.58 -1 4 34 3.92 1.29 0 -4 34 8.70 1.54 0 -4 34 5.28 1.10 0 -4 -34 6.73 1.56 1 -4 34 4.57 1.43 -2 0 35 2.84 1.56 1 0 -35 1.85 1.39 -1 0 35 0.76 1.14 0 0 -35 3.84 1.31 1 0 35 1.13 1.45 -1 0 -35 0.71 1.21 2 0 35 1.21 1.65 -2 0 -35 -0.16 1.31 -2 -1 35 5.44 1.64 -2 1 35 7.81 1.77 -1 -1 35 4.78 1.17 1 -1 -35 4.80 1.46 -1 1 35 4.50 1.32 0 -1 -35 7.17 1.50 0 1 -35 8.90 1.46 0 1 35 8.56 1.53 -1 -1 -35 1.59 1.29 1 -1 35 3.23 1.42 1 1 35 3.29 1.62 -1 1 -35 2.23 1.30 2 -1 35 1.83 1.54 -2 -1 -35 0.99 1.32 2 1 35 -0.15 1.50 -2 1 -35 3.22 1.46 -2 2 35 1.43 1.37 -2 2 35 -0.74 1.60 1 -2 -35 5.85 1.49 -1 -2 35 5.25 1.66 0 -2 35 10.91 1.45 0 -2 -35 16.44 1.83 0 2 35 14.57 1.80 0 2 -35 12.70 1.68 1 -2 35 4.15 1.38 -1 -2 -35 3.59 1.37 -1 2 -35 5.98 1.50 1 2 35 3.86 1.58 -2 2 -35 -1.58 1.39 -2 3 35 8.37 1.66 -1 -3 35 1.41 1.62 1 -3 -35 2.14 1.31 0 -3 35 6.74 1.20 0 -3 -35 10.14 1.45 0 3 35 7.99 1.52 0 3 -35 9.95 1.56 -1 -3 -35 3.37 1.41 1 -3 35 2.97 1.26 -1 3 -35 1.55 1.34 1 3 35 1.27 1.48 -1 -4 35 7.42 1.67 -1 4 35 4.63 1.39 -1 4 35 2.39 1.28 0 -4 35 11.15 1.59 0 -4 -35 12.80 1.79 0 -4 35 12.43 1.46 -1 -4 -35 1.11 1.26 1 4 35 4.44 1.53 -2 0 36 10.97 1.82 -1 0 36 4.23 1.24 1 0 -36 0.39 1.28 0 0 -36 18.65 2.07 0 0 36 17.32 1.84 1 0 36 -0.24 1.48 -1 0 -36 1.62 1.28 2 0 36 7.96 1.88 -2 1 36 1.46 1.70 1 -1 -36 2.57 1.46 -1 -1 36 4.16 1.22 1 1 -36 3.90 1.36 -1 1 36 2.39 1.21 0 -1 36 -1.79 1.13 0 -1 -36 -0.61 1.21 0 1 -36 0.09 1.24 0 1 36 -1.67 1.29 1 -1 36 10.04 1.55 -1 -1 -36 11.39 1.59 -1 1 -36 10.14 1.65 -2 -1 -36 -0.64 1.37 -2 1 -36 3.80 1.48 -2 -2 36 9.87 2.00 -2 2 36 7.04 1.77 -2 2 36 4.57 1.45 -1 -2 36 9.13 1.75 1 -2 -36 5.25 1.51 -1 2 36 6.89 1.31 0 -2 -36 0.62 1.34 0 -2 36 1.72 1.17 0 2 -36 0.56 1.30 0 2 36 1.15 1.31 1 -2 36 0.87 1.22 -1 -2 -36 2.59 1.31 1 2 36 1.06 1.51 -1 2 -36 -1.87 1.32 2 -2 36 -0.61 1.46 -2 -2 -36 0.59 1.26 2 2 36 -0.49 1.69 -2 2 -36 0.64 1.52 -2 3 36 5.12 1.62 -1 -3 36 4.18 1.71 1 -3 -36 2.10 1.34 0 -3 -36 -0.11 1.30 0 -3 36 1.68 1.06 0 3 -36 2.83 1.42 0 3 36 -1.83 1.19 -1 -3 -36 4.80 1.41 1 -3 36 3.96 1.28 1 3 36 3.32 1.54 -1 3 -36 1.05 1.40 -1 -4 36 1.84 1.55 -1 4 36 4.50 1.37 -1 4 36 3.97 1.28 0 -4 36 1.57 1.00 0 -4 36 4.55 1.41 0 -4 -36 0.93 1.37 -2 0 37 -2.34 1.53 -1 0 37 3.04 1.23 1 0 -37 0.78 1.44 0 0 -37 1.42 1.32 0 0 37 0.14 1.31 1 0 37 1.01 1.52 -1 0 -37 3.80 1.44 -2 0 -37 0.75 1.85 -2 -1 37 1.46 1.60 -2 1 37 2.41 1.75 1 -1 -37 9.19 1.55 1 1 -37 11.48 1.62 -1 1 37 10.21 1.50 0 -1 -37 3.56 1.47 0 -1 37 2.33 1.25 0 1 -37 4.29 1.42 0 1 37 2.30 1.41 -1 -1 -37 3.73 1.43 1 -1 37 3.75 1.48 1 1 37 3.23 1.61 -1 1 -37 3.28 1.50 -2 -1 -37 1.80 1.34 2 -1 37 -1.84 1.57 -2 1 -37 4.02 1.53 2 1 37 -1.25 1.63 -2 2 37 0.55 1.67 1 -2 -37 2.12 1.44 -1 -2 37 0.45 1.56 -1 2 37 1.53 1.23 0 -2 37 2.12 1.15 0 -2 -37 1.24 1.30 0 2 -37 -0.56 1.45 0 2 37 0.99 1.36 -1 -2 -37 0.95 1.28 1 -2 37 1.09 1.28 1 2 37 0.03 1.51 1 -3 -37 2.41 1.40 -1 -3 37 2.29 1.56 0 -3 -37 22.98 2.14 0 -3 37 21.68 1.74 0 3 -37 24.63 2.21 0 3 37 24.81 2.01 -1 -3 -37 0.29 1.26 1 -3 37 0.49 1.19 -1 3 -37 0.32 1.48 0 -4 37 -0.48 0.92 0 -4 -37 1.65 1.52 -2 0 38 4.44 1.75 1 0 -38 2.20 1.41 0 0 -38 0.17 1.31 0 0 38 4.46 1.49 -1 0 -38 0.69 1.39 1 0 38 0.55 1.57 2 0 38 30.24 2.65 -2 0 -38 32.23 2.44 -2 1 38 -1.27 1.72 1 -1 -38 3.03 1.52 1 1 -38 1.96 1.53 0 -1 -38 12.90 1.66 0 -1 38 10.76 1.48 0 1 38 11.10 1.68 0 1 -38 10.97 1.64 1 -1 38 10.79 1.68 -1 -1 -38 12.96 1.72 1 1 38 8.87 1.86 -1 1 -38 12.78 1.70 -2 -2 38 0.55 1.88 -2 2 38 -1.14 1.66 1 -2 -38 -0.01 1.32 -1 -2 38 3.47 1.82 -1 2 38 1.63 1.24 0 -2 -38 1.01 1.31 0 -2 38 1.35 1.17 0 2 38 1.81 1.37 0 2 -38 2.21 1.56 -1 -2 -38 7.54 1.51 1 -2 38 6.45 1.48 -1 2 -38 3.85 1.60 1 2 38 6.09 1.77 -1 -3 38 3.01 1.62 1 -3 -38 -0.09 1.38 0 -3 -38 9.14 1.57 0 -3 38 8.30 1.29 0 3 38 9.20 1.70 0 3 -38 10.17 1.71 -1 3 -38 6.54 1.67 1 3 38 5.05 1.78 1 0 -39 -0.60 1.38 0 0 39 0.32 1.33 0 0 -39 0.29 1.36 -1 0 -39 1.15 1.43 1 0 39 0.59 1.58 -2 -1 39 0.90 2.14 1 -1 -39 11.62 1.81 1 1 -39 12.28 1.77 0 -1 39 -0.85 1.20 0 -1 -39 2.22 1.41 0 1 -39 -0.23 1.48 0 1 39 1.05 1.42 1 -1 39 1.69 1.50 -1 -1 -39 0.88 1.40 1 1 39 3.18 1.77 -1 1 -39 3.04 1.58 -1 -2 39 7.36 1.98 1 -2 -39 5.43 1.51 0 -2 39 -0.08 1.19 0 -2 -39 -0.07 1.40 0 2 39 1.86 1.41 0 2 -39 1.58 1.58 1 -2 39 9.00 1.57 1 -3 -39 4.74 1.59 0 -3 39 6.18 1.24 0 3 -39 10.89 1.74 0 3 39 8.08 1.56 -2 0 40 35.06 2.64 1 0 -40 1.64 1.59 0 0 40 11.89 1.73 0 0 -40 12.14 1.83 -1 0 -40 2.86 1.44 1 0 40 4.53 1.72 -2 -1 40 2.12 1.88 -2 1 40 1.87 1.91 1 -1 -40 2.41 1.45 1 1 -40 3.51 1.69 0 -1 40 3.76 1.41 0 1 -40 7.47 1.70 0 1 40 4.89 1.54 1 -1 40 1.76 1.56 1 1 40 5.95 1.76 -1 1 -40 5.49 1.66 1 -2 -40 5.13 1.45 0 -2 -40 2.71 1.44 0 -2 40 2.79 1.27 0 2 40 3.10 1.46 0 2 -40 5.99 1.72 -1 -2 -40 11.64 1.70 -1 2 -40 13.70 1.99 0 -3 40 8.15 1.31 0 3 -40 7.33 1.68 1 0 -41 1.10 1.73 0 0 41 3.23 1.45 0 0 -41 1.17 1.44 0 -1 -41 1.71 1.48 0 -1 41 2.56 1.41 0 1 41 1.06 1.48 0 1 -41 4.14 1.67 -1 -1 -41 9.18 1.66 0 -2 41 4.26 1.32 0 2 -41 2.95 1.58 0 2 41 1.17 1.41 0 0 42 41.82 2.55 1 0 42 -0.30 1.68 1 1 -42 6.11 1.86 0 -1 42 3.37 1.44 0 1 42 -2.65 1.37 1 0 -43 1.64 1.70 0 0 43 5.50 1.56 0 0 -43 4.77 1.76 0 -1 43 2.94 1.48 0 -1 -43 -0.05 1.49 0 1 43 2.24 1.52 0 1 -43 3.33 1.62 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 29068 _shelx_res_file ; TITL UMT_DD2_BP in P21/n #14 umt_dd2_bp.res created by SHELXL-2018/3 at 22:18:34 on 31-Jul-2023 CELL 0.71073 3.7712 6.1229 34.8683 90 93.0992 90 ZERR 4 0.0003 0.0005 0.0029 0 0.0029 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O UNIT 32 28 12 8 EQIV $1 2-X,1-Y,-Z L.S. 10 PLAN 1 SIZE 0.28 0.06 0.02 TEMP -173.15 CONF HTAB O2 O1_$1 BOND MORE -1 BOND $H fmap 2 53 acta TWIN -1 0 0 0 -1 0 1 0 1 2 REM REM REM WGHT 0.029900 0.338700 BASF 0.54707 FVAR 0.36406 O1 4 1.062295 0.496145 0.047463 11.00000 0.02691 0.01964 = 0.01767 -0.00123 0.00051 -0.00678 O2 4 0.772453 0.251849 0.009562 11.00000 0.03360 0.02569 = 0.01325 0.00021 -0.00306 -0.01014 H1 2 0.832403 0.347207 -0.008127 11.00000 0.07189 N1 3 0.785350 0.434015 0.190500 11.00000 0.03064 0.02141 = 0.02167 -0.00467 -0.00810 0.00264 N2 3 0.969165 0.555241 0.211767 11.00000 0.03181 0.02399 = 0.01340 0.00179 -0.00185 0.00750 N3 3 1.108150 0.685689 0.229966 11.00000 0.05093 0.02624 = 0.02986 -0.01172 -0.01121 0.00415 C1 1 0.806478 0.185250 0.076353 11.00000 0.01333 0.01796 = 0.01666 0.00046 -0.00060 0.00267 C2 1 0.893001 0.259981 0.113379 11.00000 0.01563 0.01339 = 0.01913 -0.00221 -0.00111 -0.00037 AFIX 43 H2 2 1.002494 0.398639 0.117123 11.00000 -1.20000 AFIX 0 C3 1 0.819351 0.131930 0.144873 11.00000 0.01235 0.01744 = 0.01676 -0.00061 -0.00196 0.00335 C4 1 0.658442 -0.070343 0.139018 11.00000 0.01464 0.01820 = 0.02077 0.00428 0.00233 0.00192 AFIX 43 H4 2 0.604339 -0.157416 0.160482 11.00000 -1.20000 AFIX 0 C5 1 0.575786 -0.146603 0.102023 11.00000 0.01642 0.01384 = 0.02699 -0.00203 -0.00313 -0.00162 AFIX 43 H5 2 0.469034 -0.286048 0.098269 11.00000 -1.20000 AFIX 0 C6 1 0.649514 -0.018753 0.070711 11.00000 0.01476 0.01946 = 0.01741 -0.00273 -0.00071 0.00189 AFIX 43 H6 2 0.593077 -0.070155 0.045407 11.00000 -1.20000 AFIX 0 C7 1 0.891904 0.324877 0.043130 11.00000 0.01645 0.01793 = 0.01510 -0.00329 0.00083 0.00472 C8 1 0.924202 0.209395 0.185079 11.00000 0.02180 0.01708 = 0.01891 0.00088 -0.00149 0.00149 AFIX 23 H8A 2 0.825573 0.109447 0.204114 11.00000 -1.20000 H8B 2 1.186115 0.209188 0.189068 11.00000 -1.20000 AFIX 0 HKLF 4 REM UMT_DD2_BP in P21/n #14 REM wR2 = 0.0851, GooF = S = 1.132, Restrained GooF = 1.132 for all data REM R1 = 0.0434 for 1411 Fo > 4sig(Fo) and 0.0595 for all 1656 data REM 123 parameters refined using 0 restraints END WGHT 0.0299 0.3397 REM Highest difference peak 0.254, deepest hole -0.233, 1-sigma level 0.059 Q1 1 0.5305 0.1985 0.1603 11.00000 0.05 0.25 ; _shelx_res_checksum 47469 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 1.0623(4) 0.4961(2) 0.04746(4) 0.0214(4) Uani d 1 . . O O2 0.7725(4) 0.2518(3) 0.00956(4) 0.0243(4) Uani d 1 . . H H1 0.832(9) 0.347(5) -0.0081(9) 0.072(11) Uiso d 1 . . N N1 0.7854(5) 0.4340(3) 0.19050(5) 0.0249(5) Uani d 1 . . N N2 0.9692(6) 0.5552(3) 0.21177(5) 0.0232(5) Uani d 1 . . N N3 1.1081(7) 0.6857(3) 0.22997(6) 0.0362(6) Uani d 1 . . C C1 0.8065(6) 0.1853(3) 0.07635(6) 0.0160(5) Uani d 1 . . C C2 0.8930(5) 0.2600(3) 0.11338(5) 0.0161(5) Uani d 1 . . H H2 1.002494 0.398639 0.117123 0.019 Uiso calc 1 . . C C3 0.8194(6) 0.1319(3) 0.14487(6) 0.0156(5) Uani d 1 . . C C4 0.6584(6) -0.0703(3) 0.13902(6) 0.0178(5) Uani d 1 . . H H4 0.604339 -0.157416 0.160482 0.021 Uiso calc 1 . . C C5 0.5758(6) -0.1466(3) 0.10202(6) 0.0192(5) Uani d 1 . . H H5 0.469034 -0.286048 0.098269 0.023 Uiso calc 1 . . C C6 0.6495(6) -0.0188(3) 0.07071(6) 0.0173(5) Uani d 1 . . H H6 0.593077 -0.070155 0.045407 0.021 Uiso calc 1 . . C C7 0.8919(6) 0.3249(3) 0.04313(6) 0.0165(5) Uani d 1 . . C C8 0.9242(6) 0.2094(3) 0.18508(6) 0.0194(5) Uani d 1 . . H H8A 0.825573 0.109447 0.204114 0.023 Uiso calc 1 . . H H8B 1.186115 0.209188 0.189068 0.023 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 0.0269(9) 0.0196(8) 0.0177(7) -0.0068(8) 0.0005(7) -0.0012(6) O2 0.0336(10) 0.0257(9) 0.0132(8) -0.0101(9) -0.0031(7) 0.0002(7) N1 0.0306(13) 0.0214(10) 0.0217(9) 0.0026(10) -0.0081(9) -0.0047(8) N2 0.0318(12) 0.0240(10) 0.0134(9) 0.0075(10) -0.0018(9) 0.0018(9) N3 0.0509(15) 0.0262(11) 0.0299(11) 0.0041(12) -0.0112(11) -0.0117(10) C1 0.0133(11) 0.0180(11) 0.0167(10) 0.0027(10) -0.0006(10) 0.0005(8) C2 0.0156(12) 0.0134(11) 0.0191(11) -0.0004(10) -0.0011(9) -0.0022(8) C3 0.0123(12) 0.0174(11) 0.0168(11) 0.0034(10) -0.0020(9) -0.0006(8) C4 0.0146(12) 0.0182(11) 0.0208(11) 0.0019(10) 0.0023(9) 0.0043(9) C5 0.0164(12) 0.0138(11) 0.0270(12) -0.0016(11) -0.0031(10) -0.0020(9) C6 0.0148(12) 0.0195(11) 0.0174(10) 0.0019(10) -0.0007(9) -0.0027(9) C7 0.0165(12) 0.0179(11) 0.0151(10) 0.0047(11) 0.0008(9) -0.0033(8) C8 0.0218(13) 0.0171(11) 0.0189(11) 0.0015(11) -0.0015(9) 0.0009(8) 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 H1 . . 108.0(19) ? N2 N1 C8 . . 116.23(18) ? N3 N2 N1 . . 171.5(2) ? C2 C1 C7 . . 118.89(19) ? C6 C1 C2 . . 120.19(19) ? C6 C1 C7 . . 120.91(18) ? C1 C2 H2 . . 120.0 ? C3 C2 C1 . . 120.05(19) ? C3 C2 H2 . . 120.0 ? C2 C3 C8 . . 120.15(18) ? C4 C3 C2 . . 119.42(18) ? C4 C3 C8 . . 120.40(18) ? C3 C4 H4 . . 119.7 ? C3 C4 C5 . . 120.64(19) ? C5 C4 H4 . . 119.7 ? C4 C5 H5 . . 120.1 ? C6 C5 C4 . . 119.8(2) ? C6 C5 H5 . . 120.1 ? C1 C6 H6 . . 120.1 ? C5 C6 C1 . . 119.89(19) ? C5 C6 H6 . . 120.1 ? O1 C7 O2 . . 123.42(18) ? O1 C7 C1 . . 121.70(18) ? O2 C7 C1 . . 114.88(19) ? N1 C8 C3 . . 109.37(17) ? N1 C8 H8A . . 109.8 ? N1 C8 H8B . . 109.8 ? C3 C8 H8A . . 109.8 ? C3 C8 H8B . . 109.8 ? H8A C8 H8B . . 108.2 ? 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 . 1.235(3) ? O2 H1 . 0.89(3) ? O2 C7 . 1.310(2) ? N1 N2 . 1.235(3) ? N1 C8 . 1.487(3) ? N2 N3 . 1.131(3) ? C1 C2 . 1.392(3) ? C1 C6 . 1.392(3) ? C1 C7 . 1.489(3) ? C2 H2 . 0.9500 ? C2 C3 . 1.390(3) ? C3 C4 . 1.389(3) ? C3 C8 . 1.512(3) ? C4 H4 . 0.9500 ? C4 C5 . 1.391(3) ? C5 H5 . 0.9500 ? C5 C6 . 1.384(3) ? 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 H1 O1 3_765 0.89(3) 1.74(3) 2.619(2) 172(3) 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 . . . . -146.9(2) ? C1 C2 C3 C4 . . . . -0.1(3) ? C1 C2 C3 C8 . . . . 177.95(19) ? C2 C1 C6 C5 . . . . 0.7(3) ? C2 C1 C7 O1 . . . . 5.9(3) ? C2 C1 C7 O2 . . . . -173.96(19) ? C2 C3 C4 C5 . . . . 1.0(3) ? C2 C3 C8 N1 . . . . 52.1(3) ? C3 C4 C5 C6 . . . . -0.9(3) ? C4 C3 C8 N1 . . . . -129.8(2) ? C4 C5 C6 C1 . . . . 0.1(3) ? C6 C1 C2 C3 . . . . -0.7(3) ? C6 C1 C7 O1 . . . . -172.7(2) ? C6 C1 C7 O2 . . . . 7.4(3) ? C7 C1 C2 C3 . . . . -179.4(2) ? C7 C1 C6 C5 . . . . 179.4(2) ? C8 C3 C4 C5 . . . . -177.1(2) ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.4529(16) 2 0.5471(16)