#------------------------------------------------------------------------------ #$Date: 2022-01-28 04:36:10 +0200 (Fri, 28 Jan 2022) $ #$Revision: 272309 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/25/2022529.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_2022529 loop_ _publ_author_name 'Jiang, Tan-Lin' 'Li, Wei-Zhou' 'Gao, Qi-Feng' 'Tan, Deng-Feng' 'Pang, Jin-Ying' 'Zhang, Shu-Hua' _publ_section_title ; Syntheses, crystal structures and Hirshfeld surface analysis of (Z)-3-[(3-acetyl-2-hydroxyphenyl)amino]-2-bromoprop-2-enal and a novel Zn^II^ complex ; _journal_coeditor_code LF3125 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229622000924 _journal_volume 78 _journal_year 2022 _chemical_formula_iupac 'C11 H10 Br N O3' _chemical_formula_moiety 'C11 H10 Br N O3' _chemical_formula_sum 'C11 H10 Br N O3' _chemical_formula_weight 284.11 _chemical_melting_point 403.35 _chemical_name_systematic ; (Z)-3-[(3-Acetyl-2-hydroxyphenyl)amino]-2-bromoprop-2-enal ; _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 geom _audit_creation_method SHELXL-2014 _cell_angle_alpha 85.770(2) _cell_angle_beta 86.907(2) _cell_angle_gamma 63.586(2) _cell_formula_units_Z 4 _cell_length_a 9.8671(7) _cell_length_b 10.6765(8) _cell_length_c 11.8719(8) _cell_measurement_reflns_used 8447 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 25.97 _cell_measurement_theta_min 3.01 _cell_volume 1116.73(14) _computing_cell_refinement ; SAINT (Bruker, 2016) ; _computing_data_collection ; APEX2 (Bruker, 2016) ; _computing_data_reduction ; SAINT (Bruker, 2016) ; _computing_publication_material ; SHELXL2014 (Sheldrick, 2015) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015) ; _computing_structure_solution ; olex2.solve (Bourhis et al., 2015) and OLEX2 (Dolomanov et al., 2009) ; _diffrn_ambient_temperature 273(2) _diffrn_detector_area_resol_mean 16.0233 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_unetI/netI 0.0270 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 19863 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.094 _diffrn_reflns_theta_min 3.443 _exptl_absorpt_coefficient_mu 3.671 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.5334 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2016) ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.690 _exptl_crystal_description irregular _exptl_crystal_F_000 568 _exptl_crystal_size_max 0.248 _exptl_crystal_size_mid 0.151 _exptl_crystal_size_min 0.081 _refine_diff_density_max 0.376 _refine_diff_density_min -0.412 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 292 _refine_ls_number_reflns 3956 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.998 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0310 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+0.7701P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.0737 _reflns_number_gt 3058 _reflns_number_total 3956 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file lf3125sup1.cif _cod_data_source_block Sm _cod_database_code 2022529 _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 0.463 _shelx_estimated_absorpt_t_max 0.755 _shelx_hkl_file ; -2 0 0 490.85 14.00 -2 0 0 461.05 13.20 -2 0 0 489.45 14.00 2 0 0 490.95 14.10 2 0 0 500.25 14.10 2 0 0 483.45 14.00 2 0 0 478.35 13.30 2 0 0 512.95 14.00 -3 0 0 1456.95 41.50 -3 0 0 1483.85 40.50 -3 0 0 1574.94 41.60 3 0 0 1535.85 41.70 3 0 0 1618.44 41.90 3 0 0 1530.45 41.80 3 0 0 1621.94 41.70 3 0 0 1494.55 40.70 -4 0 0 9.60 2.20 -4 0 0 9.00 3.10 -4 0 0 10.40 3.50 4 0 0 11.20 3.80 4 0 0 11.70 2.50 4 0 0 8.10 3.10 4 0 0 9.60 3.70 4 0 0 7.80 3.30 -5 0 0 50.39 5.10 -5 0 0 50.49 4.60 -5 0 0 37.30 5.10 5 0 0 45.60 5.70 5 0 0 36.70 5.50 5 0 0 50.99 6.20 5 0 0 49.30 5.20 5 0 0 51.49 6.10 -6 0 0 775.92 25.20 -6 0 0 758.62 24.60 6 0 0 792.72 25.50 6 0 0 777.72 25.90 6 0 0 790.52 22.90 6 0 0 802.02 22.30 6 0 0 819.12 26.00 6 0 0 775.02 24.90 -7 0 0 4.40 6.00 -7 0 0 -6.60 5.10 7 0 0 2.50 5.70 7 0 0 0.10 6.50 7 0 0 2.70 7.10 7 0 0 -0.30 4.70 7 0 0 2.80 3.80 -8 0 0 1.60 7.80 -8 0 0 -5.70 6.40 8 0 0 3.90 4.30 8 0 0 16.60 4.80 8 0 0 -3.70 8.20 8 0 0 9.30 9.20 -9 0 0 117.39 13.10 9 0 0 112.19 14.50 9 0 0 124.09 13.60 -10 0 0 10.20 11.00 10 0 0 -8.20 12.60 10 0 0 19.60 12.90 -11 0 0 20.40 15.00 11 0 0 -16.50 15.90 11 0 0 -4.50 15.80 11 -1 0 45.10 18.20 11 -1 0 8.80 16.40 -11 1 0 12.60 16.40 10 -1 0 26.90 15.00 10 -1 0 18.90 15.10 -10 1 0 -1.10 12.80 9 -1 0 8.60 12.10 9 -1 0 -0.40 5.60 9 -1 0 -6.70 11.90 -9 1 0 -0.50 10.50 8 -1 0 -2.60 5.90 8 -1 0 -15.00 9.30 8 -1 0 -0.20 6.60 8 -1 0 -2.40 10.20 -8 1 0 1.30 8.00 7 -1 0 271.97 17.10 7 -1 0 280.87 12.40 7 -1 0 295.37 17.90 7 -1 0 251.37 13.00 -7 1 0 281.87 15.70 6 -1 0 -2.60 4.40 6 -1 0 3.20 6.00 6 -1 0 0.60 5.40 6 -1 0 -5.50 4.50 6 -1 0 1.80 4.80 6 -1 0 -1.40 6.00 -6 1 0 3.20 4.50 -6 1 0 2.10 5.20 5 -1 0 298.57 13.40 5 -1 0 299.77 13.10 5 -1 0 305.07 11.50 5 -1 0 292.97 12.10 5 -1 0 303.77 13.30 -5 1 0 299.77 12.60 -5 1 0 287.07 11.90 4 -1 0 3430.26 89.29 4 -1 0 3478.75 89.59 4 -1 0 3381.86 88.39 4 -1 0 3364.86 89.49 4 -1 0 3331.17 89.09 -4 1 0 3276.87 88.09 -4 1 0 3313.57 88.79 -4 1 0 3266.27 89.09 3 -1 0 463.85 14.40 3 -1 0 371.46 13.90 3 -1 0 461.25 13.60 3 -1 0 452.35 13.90 3 -1 0 459.75 14.40 -3 1 0 464.45 13.70 -3 1 0 444.46 14.00 -3 1 0 447.46 13.40 2 -1 0 429.46 12.60 2 -1 0 428.86 12.60 2 -1 0 436.86 13.00 2 -1 0 434.26 12.50 2 -1 0 394.86 13.00 2 -1 0 435.36 12.60 -2 1 0 414.56 12.40 -2 1 0 423.86 12.60 1 -1 0 3593.04 90.79 1 -1 0 3596.44 90.69 1 -1 0 3534.05 90.89 1 -1 0 3652.13 90.89 -1 1 0 3334.97 90.69 -1 1 0 3507.15 90.69 -1 1 0 3449.46 90.79 -1 1 0 3308.07 90.79 2 1 0 9055.19 234.08 -3 -1 0 1270.57 36.20 -3 -1 0 1403.76 36.10 3 1 0 1304.07 35.90 3 1 0 1284.27 36.20 3 1 0 1329.47 36.10 3 1 0 1346.07 35.90 -4 -1 0 1.50 2.90 -4 -1 0 4.00 3.10 4 1 0 -1.40 2.80 4 1 0 3.00 3.10 4 1 0 2.70 3.30 4 1 0 5.40 2.80 -5 -1 0 1410.26 40.40 5 1 0 1431.36 40.80 5 1 0 1375.76 37.80 5 1 0 1471.05 40.50 5 1 0 1469.75 40.40 5 1 0 1433.76 40.50 -6 -1 0 0.30 4.80 -6 -1 0 -6.60 4.20 6 1 0 0.60 5.20 6 1 0 -1.20 4.70 6 1 0 -0.30 4.30 6 1 0 3.30 5.10 -7 -1 0 9.70 5.70 -7 -1 0 16.90 6.80 7 1 0 -5.30 6.20 7 1 0 11.40 6.70 7 1 0 -4.70 6.60 7 1 0 8.80 5.20 -8 -1 0 369.46 19.00 -8 -1 0 311.87 16.40 8 1 0 382.46 20.20 8 1 0 376.26 19.90 -9 -1 0 8.00 8.20 9 1 0 19.20 11.00 9 1 0 18.50 9.80 -10 -1 0 -5.70 11.20 10 1 0 -5.90 11.50 10 1 0 8.00 12.80 -11 -1 0 36.70 14.40 11 1 0 14.30 15.70 11 1 0 20.20 15.40 10 -2 0 12.20 15.60 10 -2 0 19.50 17.60 -10 2 0 -15.00 13.90 9 -2 0 8.80 13.00 9 -2 0 7.20 6.70 9 -2 0 3.00 12.80 -9 2 0 12.30 11.10 8 -2 0 55.39 11.90 8 -2 0 47.90 12.00 8 -2 0 70.09 8.40 8 -2 0 65.19 8.50 -8 2 0 51.59 10.20 7 -2 0 -1.90 6.60 7 -2 0 -3.20 5.90 7 -2 0 8.70 8.90 7 -2 0 -0.30 6.40 7 -2 0 10.20 8.20 -7 2 0 -1.50 7.60 6 -2 0 121.79 13.00 6 -2 0 130.09 10.30 6 -2 0 117.69 10.60 6 -2 0 131.79 10.40 6 -2 0 120.09 13.40 6 -2 0 107.09 10.10 -6 2 0 143.39 12.00 5 -2 0 294.57 12.80 5 -2 0 321.17 12.80 5 -2 0 300.47 13.90 5 -2 0 295.87 12.80 5 -2 0 338.17 14.80 5 -2 0 313.67 14.20 -5 2 0 307.37 13.60 4 -2 0 1519.45 42.10 4 -2 0 1554.04 42.60 4 -2 0 1491.55 41.80 4 -2 0 1509.15 42.50 4 -2 0 1484.25 41.70 4 -2 0 1523.95 41.60 -4 2 0 1410.56 41.90 3 -2 0 46.00 4.70 3 -2 0 39.10 4.50 3 -2 0 38.00 4.20 3 -2 0 52.49 5.70 3 -2 0 32.10 3.80 3 -2 0 50.79 4.60 -3 2 0 38.10 4.10 -3 2 0 39.90 4.30 2 -2 0 1097.69 30.10 2 -2 0 1087.49 30.40 2 -2 0 1105.49 30.30 2 -2 0 1112.19 30.20 2 -2 0 1086.69 29.90 -2 2 0 1083.99 30.30 1 -2 0 4735.83 121.19 1 -2 0 4747.52 121.59 1 -2 0 4755.02 121.09 1 -2 0 4566.04 121.19 1 -2 0 4680.33 121.09 -1 2 0 4608.74 120.99 -1 2 0 4625.74 121.09 -1 2 0 4582.24 121.49 0 -2 0 354.26 10.20 0 -2 0 350.96 10.30 0 -2 0 338.17 9.70 0 -2 0 344.37 10.50 0 2 0 350.46 9.60 0 2 0 353.26 10.20 0 2 0 342.37 10.40 0 2 0 350.06 10.20 -1 -2 0 4285.87 104.59 -1 -2 0 3717.63 104.89 -1 -2 0 4182.28 104.49 -1 -2 0 4229.98 104.49 1 2 0 4202.78 104.99 1 2 0 3512.45 104.39 -2 -2 0 51.89 2.90 -2 -2 0 53.49 4.60 -2 -2 0 59.69 3.00 -2 -2 0 65.49 4.00 2 2 0 59.79 4.00 2 2 0 61.59 2.90 2 2 0 58.59 4.80 2 2 0 57.49 2.80 -3 -2 0 1220.28 33.90 -3 -2 0 1218.68 32.30 3 2 0 1221.48 32.20 3 2 0 1214.08 33.10 3 2 0 1216.38 33.80 3 2 0 1221.08 33.20 3 2 0 1268.57 33.80 -4 -2 0 1239.68 35.70 -4 -2 0 1285.77 35.50 4 2 0 1241.08 35.60 4 2 0 1249.97 34.90 4 2 0 1257.97 34.90 4 2 0 1301.87 35.50 -5 -2 0 290.77 16.20 -5 -2 0 284.07 11.90 5 2 0 302.07 11.70 5 2 0 267.67 11.40 5 2 0 300.17 11.40 5 2 0 281.97 12.30 -6 -2 0 47.20 6.20 -6 -2 0 55.99 6.60 6 2 0 51.29 6.00 6 2 0 53.29 6.50 6 2 0 64.79 7.70 6 2 0 53.59 6.30 -7 -2 0 157.58 11.90 -7 -2 0 155.78 11.80 7 2 0 168.28 11.00 7 2 0 162.18 12.30 7 2 0 178.98 11.00 7 2 0 166.08 14.10 -8 -2 0 58.29 8.00 -8 -2 0 74.89 9.60 8 2 0 63.09 9.20 8 2 0 53.59 9.40 -9 -2 0 -1.00 9.00 9 2 0 0.20 9.60 9 2 0 -6.60 8.50 -10 -2 0 28.20 12.10 10 2 0 19.80 12.70 10 2 0 42.20 12.30 -11 -2 0 29.60 14.70 11 2 0 8.80 15.10 11 2 0 13.20 14.20 -12 -2 0 -15.90 16.10 12 2 0 -14.90 16.80 12 2 0 15.80 15.30 10 -3 0 3.00 17.20 10 -3 0 -17.10 16.10 9 -3 0 20.90 15.90 9 -3 0 -0.30 14.60 -9 3 0 -3.10 12.60 8 -3 0 19.80 12.10 8 -3 0 12.30 11.60 8 -3 0 20.00 9.20 -8 3 0 8.10 10.60 7 -3 0 20.50 8.30 7 -3 0 45.30 10.10 7 -3 0 32.40 8.80 7 -3 0 29.80 10.40 -7 3 0 35.40 9.70 6 -3 0 178.28 13.30 6 -3 0 151.08 11.70 6 -3 0 191.48 15.90 6 -3 0 185.18 13.10 6 -3 0 193.28 14.60 -6 3 0 171.38 14.30 5 -3 0 6.70 4.90 5 -3 0 7.90 5.90 5 -3 0 0.40 5.80 5 -3 0 8.00 5.90 5 -3 0 7.80 4.80 5 -3 0 12.10 6.20 5 -3 0 3.90 5.60 -5 3 0 0.30 5.40 4 -3 0 397.76 14.50 4 -3 0 382.76 14.50 4 -3 0 409.96 15.10 4 -3 0 403.96 15.40 4 -3 0 393.26 15.10 4 -3 0 386.16 15.50 4 -3 0 388.86 15.10 -4 3 0 382.76 14.90 3 -3 0 1014.40 30.40 3 -3 0 1026.50 29.90 3 -3 0 1022.20 29.90 3 -3 0 988.00 31.40 3 -3 0 1070.49 29.70 3 -3 0 1013.00 29.60 3 -3 0 1024.10 29.80 2 -3 0 134.89 7.60 2 -3 0 116.79 6.90 2 -3 0 126.39 6.70 2 -3 0 127.89 6.80 2 -3 0 120.49 6.90 2 -3 0 121.29 6.90 -2 3 0 126.69 7.20 -2 3 0 122.69 6.70 1 -3 0 9.20 3.10 1 -3 0 8.20 2.40 1 -3 0 4.30 2.50 1 -3 0 6.20 2.50 1 -3 0 7.70 2.40 -1 3 0 6.10 2.10 -1 3 0 1.90 2.40 -1 3 0 3.70 2.80 0 -3 0 1114.09 29.80 0 -3 0 1142.89 30.60 0 -3 0 1117.09 31.10 0 -3 0 1116.69 30.80 0 3 0 1106.09 30.50 0 3 0 1130.29 30.60 0 3 0 1117.39 29.60 -1 -3 0 316.77 10.10 -1 -3 0 318.87 10.30 -1 -3 0 318.17 10.90 -1 -3 0 318.07 10.40 1 3 0 325.17 10.70 1 3 0 307.87 10.10 -2 -3 0 2846.62 75.49 -2 -3 0 2855.41 74.59 -2 -3 0 2828.62 75.49 -2 -3 0 2849.91 76.49 -2 -3 0 2948.00 75.89 2 3 0 2918.61 75.89 2 3 0 2856.01 74.59 2 3 0 2916.61 76.79 -3 -3 0 27.30 3.30 -3 -3 0 27.90 3.80 -3 -3 0 32.90 3.60 3 3 0 36.30 4.20 3 3 0 28.70 3.60 3 3 0 25.80 3.00 3 3 0 31.90 3.40 -4 -3 0 2248.77 60.99 -4 -3 0 2284.37 58.99 -4 -3 0 2240.38 60.99 4 3 0 2225.68 59.79 4 3 0 2259.17 60.99 4 3 0 2207.58 58.69 4 3 0 2245.78 60.79 -5 -3 0 16.60 4.50 -5 -3 0 15.50 4.40 -5 -3 0 23.50 2.70 5 3 0 18.80 2.00 5 3 0 15.00 3.80 5 3 0 21.40 4.10 5 3 0 17.80 4.30 5 3 0 22.70 4.80 -6 -3 0 527.05 19.20 -6 -3 0 523.15 18.90 6 3 0 529.35 19.30 6 3 0 543.55 18.40 6 3 0 498.25 18.00 6 3 0 528.95 17.80 -7 -3 0 273.47 14.50 -7 -3 0 248.28 14.20 7 3 0 284.37 15.40 7 3 0 273.37 12.90 7 3 0 235.98 12.50 7 3 0 253.07 13.30 -8 -3 0 9.50 7.20 -8 -3 0 13.00 6.70 8 3 0 1.50 7.00 8 3 0 -3.40 7.70 -9 -3 0 14.20 8.70 9 3 0 12.00 9.90 9 3 0 21.70 9.10 -10 -3 0 95.39 13.20 10 3 0 136.79 14.90 10 3 0 90.69 13.80 -11 -3 0 11.70 13.00 11 3 0 0.00 14.40 11 3 0 3.10 13.10 -12 -3 0 19.20 16.50 12 3 0 -2.50 15.60 12 3 0 -2.20 17.30 9 -4 0 2.90 16.40 9 -4 0 0.60 15.10 9 -4 0 -9.80 16.70 8 -4 0 21.60 13.70 8 -4 0 33.40 12.80 8 -4 0 31.00 13.90 8 -4 0 21.40 11.30 7 -4 0 41.20 10.50 7 -4 0 34.20 10.90 7 -4 0 14.50 11.30 7 -4 0 32.30 11.00 7 -4 0 27.30 11.50 6 -4 0 3.80 8.30 6 -4 0 4.20 8.40 6 -4 0 5.30 8.60 6 -4 0 21.30 9.40 6 -4 0 8.50 9.50 5 -4 0 47.10 6.50 5 -4 0 51.39 8.30 5 -4 0 58.29 8.40 5 -4 0 37.30 9.10 5 -4 0 66.29 8.80 5 -4 0 48.30 6.70 5 -4 0 49.20 8.20 5 -4 0 50.09 8.70 4 -4 0 255.07 13.80 4 -4 0 227.88 11.80 4 -4 0 243.98 13.60 4 -4 0 229.28 11.70 4 -4 0 249.58 13.50 4 -4 0 217.58 12.70 4 -4 0 234.78 12.90 4 -4 0 240.28 13.10 3 -4 0 17.30 5.60 3 -4 0 25.00 5.20 3 -4 0 18.70 4.80 3 -4 0 22.80 5.60 3 -4 0 23.40 5.10 3 -4 0 31.10 5.30 3 -4 0 24.50 4.70 3 -4 0 25.60 5.50 2 -4 0 82.59 7.00 2 -4 0 79.89 6.70 2 -4 0 88.69 6.80 2 -4 0 80.09 7.60 2 -4 0 88.29 8.20 2 -4 0 81.39 8.00 2 -4 0 84.69 6.70 -2 4 0 76.59 6.80 1 -4 0 10.60 3.90 1 -4 0 9.60 3.00 1 -4 0 11.20 3.70 1 -4 0 8.10 3.20 1 -4 0 10.40 3.70 -1 4 0 10.40 3.30 0 -4 0 493.85 15.30 0 -4 0 500.45 16.10 0 -4 0 475.15 16.10 0 -4 0 500.95 15.90 0 -4 0 487.25 14.30 0 4 0 506.25 15.50 0 4 0 491.65 14.00 0 4 0 511.75 15.50 -1 -4 0 1306.67 36.40 -1 -4 0 1312.77 36.50 -1 -4 0 1293.87 36.00 -1 -4 0 1352.06 36.90 1 4 0 1280.17 36.00 1 4 0 1317.67 36.30 -2 -4 0 624.84 18.00 -2 -4 0 605.64 18.10 -2 -4 0 592.54 19.20 -2 -4 0 581.44 18.00 2 4 0 583.64 18.00 2 4 0 597.14 19.00 -3 -4 0 799.02 22.70 -3 -4 0 783.22 24.30 -3 -4 0 791.82 23.40 -3 -4 0 788.32 22.60 3 4 0 819.82 24.60 3 4 0 773.82 23.40 3 4 0 781.12 21.50 -4 -4 0 83.29 6.90 -4 -4 0 75.49 7.60 -4 -4 0 80.39 5.40 -4 -4 0 73.19 5.10 4 4 0 72.39 7.50 4 4 0 78.49 5.10 4 4 0 78.99 4.90 4 4 0 86.49 7.60 -5 -4 0 44.50 4.40 -5 -4 0 46.20 4.80 -5 -4 0 33.50 5.20 -5 -4 0 24.30 5.00 5 4 0 41.00 4.10 5 4 0 31.00 5.00 5 4 0 37.40 5.60 5 4 0 47.30 4.70 -6 -4 0 1341.37 39.50 -6 -4 0 1306.97 35.90 -6 -4 0 1307.77 35.40 -6 -4 0 1335.97 39.40 6 4 0 1333.07 39.20 6 4 0 1322.17 39.10 6 4 0 1322.67 37.50 6 4 0 1331.57 37.90 -7 -4 0 -17.10 5.40 -7 -4 0 1.60 6.00 7 4 0 6.10 4.90 7 4 0 -5.70 5.30 7 4 0 -1.30 4.60 7 4 0 5.30 6.70 -8 -4 0 12.80 6.80 -8 -4 0 11.60 7.90 8 4 0 23.50 7.20 8 4 0 6.10 6.70 8 4 0 34.10 8.80 -9 -4 0 132.49 13.00 9 4 0 142.89 13.20 9 4 0 146.19 16.80 -10 -4 0 20.10 11.40 10 4 0 19.80 12.20 10 4 0 24.20 11.10 -11 -4 0 32.50 13.70 11 4 0 58.09 13.40 11 4 0 26.80 14.50 -12 -4 0 17.10 16.50 12 4 0 -2.90 14.70 12 4 0 11.00 16.80 8 -5 0 4.60 12.30 8 -5 0 -1.90 15.00 8 -5 0 -12.70 14.50 8 -5 0 -4.00 15.60 7 -5 0 14.60 13.60 7 -5 0 6.40 12.30 7 -5 0 20.40 12.20 7 -5 0 2.20 11.90 6 -5 0 22.00 10.50 6 -5 0 15.70 10.50 6 -5 0 33.90 11.50 6 -5 0 15.70 10.70 5 -5 0 -2.40 9.00 5 -5 0 -15.40 7.40 5 -5 0 8.60 8.80 5 -5 0 -1.30 8.10 4 -5 0 36.30 8.00 4 -5 0 33.80 7.30 4 -5 0 21.90 7.40 4 -5 0 32.20 8.20 4 -5 0 25.40 6.70 4 -5 0 18.90 6.20 4 -5 0 16.60 5.70 4 -5 0 37.80 7.20 3 -5 0 113.49 11.50 3 -5 0 128.49 11.80 3 -5 0 136.69 9.80 3 -5 0 117.59 12.20 3 -5 0 134.19 10.50 3 -5 0 131.49 9.90 3 -5 0 121.39 9.80 2 -5 0 135.19 10.00 2 -5 0 118.19 8.70 2 -5 0 127.29 10.30 2 -5 0 126.69 8.60 2 -5 0 121.49 8.50 2 -5 0 125.19 8.60 2 -5 0 118.69 10.80 -2 5 0 129.39 8.90 1 -5 0 391.96 15.70 1 -5 0 394.46 15.20 1 -5 0 327.67 13.10 1 -5 0 422.86 15.10 1 -5 0 395.26 13.90 1 -5 0 418.46 13.20 -1 5 0 409.16 14.30 0 -5 0 449.46 16.40 0 -5 0 462.25 16.20 0 -5 0 439.56 13.80 0 -5 0 447.36 15.10 0 -5 0 456.05 16.30 0 5 0 475.65 16.40 0 5 0 447.56 15.30 -1 -5 0 1423.16 40.10 -1 -5 0 1449.76 39.60 -1 -5 0 1449.06 40.70 -1 -5 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15.20 1 -1 14 2.20 12.80 -2 1 -14 14.40 17.90 2 -1 14 -0.10 13.80 2 -1 14 15.10 15.40 -3 1 -14 10.20 18.40 3 -1 14 3.50 16.30 3 -1 14 39.20 14.50 -4 1 -14 25.90 19.60 4 -1 14 12.90 17.60 4 -1 14 18.40 14.70 4 0 -14 99.19 17.20 4 0 -14 101.09 18.70 -4 0 14 68.49 17.90 3 0 -14 4.50 15.30 3 0 -14 18.60 16.10 -3 0 14 44.50 16.30 2 0 -14 5.40 15.10 2 0 -14 9.70 14.80 -2 0 14 30.00 15.20 1 0 -14 53.29 16.40 1 0 -14 55.69 14.10 -1 0 14 72.59 15.90 0 0 -14 -9.00 10.50 0 0 -14 -10.20 15.20 0 0 14 13.70 11.50 0 0 14 3.30 13.90 -1 0 -14 31.10 16.40 1 0 14 -10.80 12.40 1 0 14 0.00 14.70 -2 0 -14 127.09 20.30 2 0 14 81.99 16.60 2 0 14 80.29 14.40 -3 0 -14 -1.50 17.40 3 0 14 -9.10 12.50 3 0 14 16.00 15.70 -4 0 -14 9.70 19.50 4 0 14 -5.30 13.30 4 0 14 -1.80 16.90 -5 0 -14 4.40 20.20 5 0 14 -13.50 13.60 5 0 14 -14.30 16.30 4 -1 -14 -13.70 17.10 4 -1 -14 -22.10 15.90 -4 1 14 4.80 15.90 3 -1 -14 11.20 16.10 3 -1 -14 31.30 17.10 -3 1 14 37.40 17.10 2 -1 -14 48.60 16.40 2 -1 -14 69.29 17.20 -2 1 14 42.70 16.50 1 -1 -14 16.70 13.40 1 -1 -14 30.20 16.60 -1 1 14 13.50 14.80 0 -1 -14 18.20 13.00 0 -1 -14 47.60 16.90 0 1 14 38.90 15.70 -1 -1 -14 16.90 11.30 -1 -1 -14 50.29 16.90 1 1 14 18.50 14.60 1 1 14 14.20 12.90 -2 -1 -14 59.09 17.40 2 1 14 32.30 15.70 2 1 14 48.20 12.10 -3 -1 -14 20.40 17.80 3 1 14 13.80 16.60 3 1 14 1.80 11.30 -4 -1 -14 32.10 18.10 4 1 14 -15.90 16.70 4 1 14 -12.50 12.30 -5 -1 -14 17.80 19.00 5 1 14 16.00 13.80 5 1 14 -4.10 17.60 3 -2 -14 10.20 16.90 3 -2 -14 11.80 16.10 -3 2 14 60.49 16.80 2 -2 -14 81.49 17.60 2 -2 -14 87.79 17.20 -2 2 14 73.49 19.10 1 -2 -14 70.59 16.40 1 -2 -14 43.60 17.00 -1 2 14 63.89 16.30 0 -2 -14 7.40 13.00 0 -2 -14 23.40 16.10 0 2 14 -10.50 14.70 -1 -2 -14 182.18 20.50 -1 -2 -14 188.88 20.70 1 2 14 162.68 18.90 -2 -2 -14 33.50 16.80 2 2 14 55.99 16.80 -3 -2 -14 20.40 16.90 3 2 14 14.40 10.30 3 2 14 -11.20 14.90 -4 -2 -14 89.89 19.10 4 2 14 51.49 12.00 4 2 14 65.79 18.90 -5 -2 -14 10.40 19.20 5 2 14 3.80 17.20 5 2 14 -13.90 11.90 3 -3 -14 63.19 17.50 3 -3 -14 57.79 18.10 -3 3 14 35.80 17.60 2 -3 -14 24.20 16.70 2 -3 -14 31.80 16.70 -2 3 14 32.10 18.10 1 -3 -14 16.90 16.10 1 -3 -14 17.40 14.90 -1 3 14 4.60 16.90 0 -3 -14 89.19 15.30 0 -3 -14 69.69 17.10 0 3 14 98.19 17.90 -1 -3 -14 3.50 12.80 -1 -3 -14 -14.80 15.30 1 3 14 -13.40 13.90 -2 -3 -14 11.70 10.70 -2 -3 -14 -15.50 16.20 2 3 14 18.30 14.80 -3 -3 -14 192.58 21.70 3 3 14 173.08 20.20 -4 -3 -14 24.40 17.60 4 3 14 38.90 18.40 -5 -3 -14 27.70 19.90 5 3 14 5.10 9.90 5 3 14 5.80 16.60 -6 -3 -14 41.70 20.20 6 3 14 31.70 12.40 6 3 14 -13.20 17.00 2 -4 -14 7.40 17.20 2 -4 -14 -11.90 16.00 -2 4 14 -18.70 16.40 1 -4 -14 172.28 21.30 1 -4 -14 162.48 19.20 -1 4 14 200.38 22.00 0 -4 -14 93.39 16.50 0 -4 -14 77.99 18.90 0 4 14 102.59 17.70 -1 -4 -14 138.59 16.40 -1 -4 -14 102.59 18.20 1 4 14 108.39 18.60 -2 -4 -14 293.07 31.30 -2 -4 -14 274.77 23.30 2 4 14 254.67 29.60 -3 -4 -14 -10.80 16.80 3 4 14 11.20 16.50 -4 -4 -14 -24.80 17.30 4 4 14 9.10 16.60 -5 -4 -14 60.09 19.10 5 4 14 77.19 18.80 -6 -4 -14 38.80 21.10 6 4 14 29.70 17.90 1 -5 -14 1.30 16.30 1 -5 -14 8.40 17.70 -1 5 14 12.70 17.40 0 -5 -14 33.60 18.80 0 -5 -14 26.70 15.60 0 5 14 21.70 18.20 -1 -5 -14 155.68 20.60 -1 -5 -14 141.69 17.50 1 5 14 169.18 22.70 -2 -5 -14 22.00 13.80 -2 -5 -14 -1.20 16.60 2 5 14 21.70 18.30 -3 -5 -14 77.19 19.30 -3 -5 -14 89.69 12.90 3 5 14 90.89 19.70 -4 -5 -14 216.98 23.90 4 5 14 206.38 22.50 -5 -5 -14 22.80 17.80 5 5 14 32.30 17.20 -1 -6 -14 11.90 15.90 -1 -6 -14 22.60 19.20 1 6 14 9.90 17.40 -2 -6 -14 21.60 14.60 -2 -6 -14 6.30 17.70 2 6 14 4.20 18.30 -3 -6 -14 55.99 17.80 -3 -6 -14 74.89 14.00 3 6 14 85.29 19.20 -4 -6 -14 -5.20 17.60 4 6 14 1.40 17.70 -5 -6 -14 53.79 19.40 5 6 14 32.30 17.70 1 2 -15 27.70 19.40 -1 -2 15 45.70 16.90 0 2 -15 19.70 18.40 0 -2 15 -11.80 15.40 0 -2 15 41.10 17.10 2 1 -15 29.40 14.90 2 1 -15 22.20 18.00 -2 -1 15 35.60 18.00 1 1 -15 15.50 18.30 -1 -1 15 16.60 17.20 0 1 -15 -20.90 16.70 0 -1 15 11.40 16.30 -1 1 -15 3.10 17.10 1 -1 15 40.70 17.80 1 -1 15 20.60 14.60 -2 1 -15 -18.50 18.70 2 -1 15 11.80 16.60 2 -1 15 -11.90 13.70 2 0 -15 21.90 18.20 2 0 -15 6.60 14.60 -2 0 15 -1.40 16.90 1 0 -15 2.30 18.30 -1 0 15 -5.10 16.50 0 0 -15 -0.30 17.70 0 0 15 4.70 15.90 -1 0 -15 69.29 19.60 1 0 15 82.79 18.10 -2 0 -15 24.70 18.10 2 0 15 19.10 17.70 2 -1 -15 23.70 16.50 2 -1 -15 32.30 18.60 -2 1 15 18.90 16.50 1 -1 -15 -21.40 17.10 1 -1 -15 38.80 14.10 -1 1 15 22.10 15.50 0 -1 -15 81.59 19.20 0 1 15 124.89 19.50 -1 -1 -15 2.60 17.80 1 1 15 9.70 17.30 -2 -1 -15 26.60 18.50 2 1 15 30.90 17.60 -3 -1 -15 94.79 20.80 3 1 15 113.79 19.10 1 -2 -15 81.59 17.20 1 -2 -15 81.29 20.30 -1 2 15 104.09 19.60 0 -2 -15 21.60 18.30 0 -2 -15 20.90 14.20 0 2 15 22.80 16.70 -1 -2 -15 40.30 18.80 1 2 15 19.10 16.70 -2 -2 -15 20.60 18.50 2 2 15 52.19 17.70 -3 -2 -15 -18.30 17.50 3 2 15 28.20 16.90 0 -3 -15 16.10 15.30 0 -3 -15 11.20 18.10 0 3 15 -2.80 16.60 -1 -3 -15 154.68 22.10 1 3 15 114.79 19.80 -2 -3 -15 26.90 18.20 2 3 15 53.89 18.00 -3 -3 -15 44.50 19.00 3 3 15 91.39 18.90 -1 -4 -15 -15.50 16.40 -1 -4 -15 28.90 14.10 1 4 15 17.20 17.30 -2 -4 -15 5.60 17.00 2 4 15 -6.70 16.00 -3 -4 -15 36.00 18.80 3 4 15 70.79 19.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 79219 _shelx_res_file ; TITL sm_a.res in P-1 REM Old TITL sm_a.res in P-1 REM SHELXT solution in P-1: R1 0.206, Rweak 0.013, Alpha 0.061 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C22 Br2 N2 O6 CELL 0.71073 9.8671 10.6765 11.8719 85.77 86.907 63.586 ZERR 4 0.0007 0.0008 0.0008 0.002 0.002 0.002 LATT 1 SFAC C H Br N O UNIT 44 40 4 4 12 L.S. 30 0 0 PLAN 1 SIZE 0.081 0.151 0.248 TEMP 0 CONF BOND $H list 4 htab fmap 2 53 acta OMIT -3 50.2 OMIT -1 0 1 REM REM REM WGHT 0.031300 0.770100 FVAR 0.74921 BR1 3 0.166650 0.621566 0.726527 11.00000 0.07558 0.06343 = 0.04906 -0.01078 0.00968 -0.04348 O1 5 0.287488 0.794909 0.564568 11.00000 0.12161 0.07720 = 0.04533 -0.01585 0.02802 -0.05915 N1 4 0.158746 0.760227 0.951378 11.00000 0.05907 0.04937 = 0.03628 -0.00156 0.00279 -0.03046 AFIX 43 H1 2 0.135007 0.693346 0.942214 11.00000 -1.20000 AFIX 0 C1 1 0.284932 0.817413 0.663873 11.00000 0.07281 0.05183 = 0.05187 -0.01124 0.01658 -0.03426 AFIX 43 H1A 2 0.321672 0.880087 0.681085 11.00000 -1.20000 AFIX 0 BR2 3 0.487518 0.938225 0.376722 11.00000 0.10835 0.06531 = 0.04541 -0.02145 0.01018 -0.05595 O2 5 0.024233 0.658593 1.101695 11.00000 0.08623 0.06861 = 0.04998 -0.00309 0.00163 -0.05508 AFIX 147 H2 2 -0.013123 0.629193 1.154214 11.00000 -1.50000 AFIX 0 N2 4 0.437754 0.675219 0.326474 11.00000 0.05863 0.03953 = 0.03751 -0.00779 0.00385 -0.02710 AFIX 43 H2A 2 0.415876 0.719634 0.387530 11.00000 -1.20000 AFIX 0 C2 1 0.231535 0.757679 0.756174 11.00000 0.04678 0.03981 = 0.04409 -0.00491 0.00633 -0.01995 O3 5 -0.075343 0.645911 1.302536 11.00000 0.09572 0.09260 = 0.06424 0.00872 0.00184 -0.06847 C3 1 0.216740 0.803151 0.861455 11.00000 0.04673 0.04460 = 0.04563 -0.00248 0.00061 -0.02162 AFIX 43 H3 2 0.249991 0.870330 0.872024 11.00000 -1.20000 AFIX 0 O4 5 0.652102 0.961867 0.148992 11.00000 0.12279 0.09297 = 0.07889 -0.02712 0.03037 -0.08682 C4 1 0.132193 0.812713 1.059804 11.00000 0.04283 0.04378 = 0.03733 0.00255 -0.00329 -0.01981 O5 5 0.444613 0.533140 0.130482 11.00000 0.08259 0.05684 = 0.03309 -0.00793 0.01129 -0.04976 AFIX 147 H5A 2 0.440200 0.484832 0.081542 11.00000 -1.50000 AFIX 0 C5 1 0.171094 0.913588 1.091130 11.00000 0.05025 0.05117 = 0.04536 0.00038 0.00306 -0.02976 AFIX 43 H5 2 0.217089 0.952527 1.038741 11.00000 -1.20000 AFIX 0 O6 5 0.382174 0.357559 0.044441 11.00000 0.14377 0.10670 = 0.04102 -0.02646 0.02968 -0.10130 C6 1 0.141938 0.957492 1.200689 11.00000 0.05864 0.05479 = 0.05307 -0.00623 0.00003 -0.03523 AFIX 43 H6 2 0.168261 1.026101 1.221088 11.00000 -1.20000 AFIX 0 C7 1 0.074872 0.901045 1.279170 11.00000 0.05020 0.05932 = 0.04150 -0.00613 0.00005 -0.02582 AFIX 43 H7 2 0.057585 0.930429 1.352636 11.00000 -1.20000 AFIX 0 C8 1 0.060853 0.756705 1.138434 11.00000 0.04586 0.04397 = 0.04343 0.00194 -0.00423 -0.02360 C9 1 0.032146 0.799312 1.249470 11.00000 0.04311 0.05213 = 0.04046 0.00340 -0.00285 -0.02349 C10 1 -0.039388 0.735883 1.331504 11.00000 0.05585 0.07662 = 0.04886 0.00717 -0.00249 -0.03661 C11 1 -0.068066 0.779400 1.450889 11.00000 0.09802 0.12326 = 0.04759 0.00077 0.01611 -0.07049 AFIX 137 H11A 2 -0.148023 0.872983 1.453022 11.00000 -1.50000 H11B 2 0.022373 0.776461 1.479792 11.00000 -1.50000 H11C 2 -0.096937 0.716658 1.496402 11.00000 -1.50000 AFIX 0 C12 1 0.615794 0.865461 0.158484 11.00000 0.09143 0.07290 = 0.05530 -0.03053 0.02513 -0.05897 AFIX 43 H12 2 0.641346 0.808936 0.097300 11.00000 -1.20000 AFIX 0 C13 1 0.541132 0.829428 0.249089 11.00000 0.06088 0.04897 = 0.04036 -0.01765 0.00782 -0.03412 C14 1 0.507278 0.719466 0.245894 11.00000 0.05011 0.04328 = 0.04324 -0.01226 0.00432 -0.02535 AFIX 43 H14 2 0.535811 0.670163 0.180448 11.00000 -1.20000 AFIX 0 C15 1 0.394606 0.565942 0.326418 11.00000 0.04112 0.03446 = 0.03696 -0.00312 0.00066 -0.01849 C16 1 0.395041 0.497759 0.230250 11.00000 0.04627 0.03928 = 0.03000 -0.00048 0.00386 -0.02337 C17 1 0.343966 0.528506 0.428009 11.00000 0.06016 0.05369 = 0.03265 -0.00963 0.00368 -0.02965 AFIX 43 H17 2 0.343545 0.573568 0.492237 11.00000 -1.20000 AFIX 0 C18 1 0.293959 0.426239 0.437108 11.00000 0.07806 0.06791 = 0.03460 -0.00333 0.01003 -0.04710 AFIX 43 H18 2 0.261954 0.401893 0.506797 11.00000 -1.20000 AFIX 0 C19 1 0.291844 0.360901 0.342701 11.00000 0.07039 0.05681 = 0.04477 -0.00596 0.01263 -0.04369 AFIX 43 H19 2 0.257271 0.292566 0.348438 11.00000 -1.20000 AFIX 0 C20 1 0.341009 0.395736 0.237948 11.00000 0.04983 0.04401 = 0.03730 -0.00479 0.00739 -0.02912 C21 1 0.332114 0.332031 0.135218 11.00000 0.07536 0.06158 = 0.04467 -0.01296 0.01208 -0.04788 C22 1 0.260446 0.233545 0.140218 11.00000 0.11639 0.10075 = 0.05538 -0.02163 0.01743 -0.08767 AFIX 33 H22A 2 0.226746 0.223776 0.216288 11.00000 -1.50000 H22B 2 0.175538 0.270258 0.091156 11.00000 -1.50000 H22C 2 0.333258 0.143669 0.116403 11.00000 -1.50000 AFIX 0 HKLF 4 REM sm_a.res in P-1 REM R1 = 0.0310 for 3058 Fo > 4sig(Fo) and 0.0471 for all 3956 data REM 292 parameters refined using 0 restraints END WGHT 0.0359 0.5750 REM Instructions for potential hydrogen bonds HTAB N1 Br1 HTAB O2 O3 HTAB N2 O1 HTAB N2 Br2 EQIV $1 -x+1, -y+2, -z+1 HTAB C3 O4_$1 HTAB O5 O6 EQIV $2 -x+1, -y+1, -z HTAB C12 O6_$2 HTAB C14 O5 HTAB C17 O1 REM Highest difference peak 0.376, deepest hole -0.412, 1-sigma level 0.051 Q1 1 0.1053 0.7077 0.7047 11.00000 0.05 0.38 ; _shelx_res_checksum 88014 _shelxl_version_number 2.014 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 Br Br1 0.16665(4) 0.62157(4) 0.72653(3) 0.05801(12) Uani d 1 . . O O1 0.2875(3) 0.7949(3) 0.56457(19) 0.0763(7) Uani d 1 . . N N1 0.1587(3) 0.7602(3) 0.95138(18) 0.0461(6) Uani d 1 . . H H1 0.1350 0.6933 0.9422 0.055 Uiso calc 1 . . C C1 0.2849(4) 0.8174(3) 0.6639(3) 0.0566(8) Uani d 1 . . H H1A 0.3217 0.8801 0.6811 0.068 Uiso calc 1 . . Br Br2 0.48752(5) 0.93823(4) 0.37672(3) 0.06600(13) Uani d 1 . . O O2 0.0242(3) 0.6586(2) 1.10169(18) 0.0607(6) Uani d 1 . . H H2 -0.0131 0.6292 1.1542 0.091 Uiso calc 1 . . N N2 0.4378(3) 0.6752(2) 0.32647(19) 0.0431(6) Uani d 1 . . H H2A 0.4159 0.7196 0.3875 0.052 Uiso calc 1 . . C C2 0.2315(3) 0.7577(3) 0.7562(2) 0.0434(7) Uani d 1 . . O O3 -0.0753(3) 0.6459(3) 1.3025(2) 0.0751(7) Uani d 1 . . C C3 0.2167(3) 0.8032(3) 0.8615(2) 0.0452(7) Uani d 1 . . H H3 0.2500 0.8703 0.8720 0.054 Uiso calc 1 . . O O4 0.6521(3) 0.9619(3) 0.1490(2) 0.0838(8) Uani d 1 . . C C4 0.1322(3) 0.8127(3) 1.0598(2) 0.0412(7) Uani d 1 . . O O5 0.4446(3) 0.5331(2) 0.13048(15) 0.0507(5) Uani d 1 . . H H5A 0.4402 0.4848 0.0815 0.076 Uiso calc 1 . . C C5 0.1711(3) 0.9136(3) 1.0911(2) 0.0466(7) Uani d 1 . . H H5 0.2171 0.9525 1.0387 0.056 Uiso calc 1 . . O O6 0.3822(3) 0.3576(3) 0.04444(18) 0.0802(8) Uani d 1 . . C C6 0.1419(3) 0.9575(3) 1.2007(3) 0.0516(8) Uani d 1 . . H H6 0.1683 1.0261 1.2211 0.062 Uiso calc 1 . . C C7 0.0749(3) 0.9010(3) 1.2792(3) 0.0496(7) Uani d 1 . . H H7 0.0576 0.9304 1.3526 0.060 Uiso calc 1 . . C C8 0.0609(3) 0.7567(3) 1.1384(2) 0.0432(7) Uani d 1 . . C C9 0.0321(3) 0.7993(3) 1.2495(2) 0.0446(7) Uani d 1 . . C C10 -0.0394(4) 0.7359(4) 1.3315(3) 0.0583(8) Uani d 1 . . C C11 -0.0681(5) 0.7794(5) 1.4509(3) 0.0827(12) Uani d 1 . . H H11A -0.1480 0.8730 1.4530 0.124 Uiso calc 1 . . H H11B 0.0224 0.7765 1.4798 0.124 Uiso calc 1 . . H H11C -0.0969 0.7167 1.4964 0.124 Uiso calc 1 . . C C12 0.6158(4) 0.8655(4) 0.1585(3) 0.0644(10) Uani d 1 . . H H12 0.6413 0.8089 0.0973 0.077 Uiso calc 1 . . C C13 0.5411(3) 0.8294(3) 0.2491(2) 0.0460(7) Uani d 1 . . C C14 0.5073(3) 0.7195(3) 0.2459(2) 0.0435(7) Uani d 1 . . H H14 0.5358 0.6702 0.1804 0.052 Uiso calc 1 . . C C15 0.3946(3) 0.5659(3) 0.3264(2) 0.0369(6) Uani d 1 . . C C16 0.3950(3) 0.4978(3) 0.2302(2) 0.0371(6) Uani d 1 . . C C17 0.3440(3) 0.5285(3) 0.4280(2) 0.0470(7) Uani d 1 . . H H17 0.3435 0.5736 0.4922 0.056 Uiso calc 1 . . C C18 0.2940(4) 0.4262(3) 0.4371(2) 0.0551(8) Uani d 1 . . H H18 0.2620 0.4019 0.5068 0.066 Uiso calc 1 . . C C19 0.2918(4) 0.3609(3) 0.3427(2) 0.0520(8) Uani d 1 . . H H19 0.2573 0.2926 0.3484 0.062 Uiso calc 1 . . C C20 0.3410(3) 0.3957(3) 0.2379(2) 0.0408(6) Uani d 1 . . C C21 0.3321(4) 0.3320(3) 0.1352(3) 0.0540(8) Uani d 1 . . C C22 0.2604(5) 0.2335(4) 0.1402(3) 0.0760(11) Uani d 1 . . H H22A 0.2267 0.2238 0.2163 0.114 Uiso calc 1 . . H H22B 0.1755 0.2703 0.0912 0.114 Uiso calc 1 . . H H22C 0.3333 0.1437 0.1164 0.114 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 Br1 0.0756(2) 0.0634(2) 0.0491(2) -0.04348(18) 0.00968(16) -0.01078(15) O1 0.122(2) 0.0772(17) 0.0453(14) -0.0591(16) 0.0280(14) -0.0159(12) N1 0.0591(16) 0.0494(14) 0.0363(13) -0.0305(13) 0.0028(11) -0.0016(11) C1 0.073(2) 0.0518(19) 0.052(2) -0.0343(17) 0.0166(16) -0.0112(15) Br2 0.1083(3) 0.0653(2) 0.0454(2) -0.0560(2) 0.01018(18) -0.02145(16) O2 0.0862(17) 0.0686(15) 0.0500(13) -0.0551(13) 0.0016(12) -0.0031(11) N2 0.0586(15) 0.0395(13) 0.0375(13) -0.0271(12) 0.0038(11) -0.0078(10) C2 0.0468(17) 0.0398(16) 0.0441(17) -0.0200(13) 0.0063(13) -0.0049(13) O3 0.0957(19) 0.0926(19) 0.0642(15) -0.0685(16) 0.0018(13) 0.0087(13) C3 0.0467(17) 0.0446(17) 0.0456(17) -0.0216(14) 0.0006(14) -0.0025(13) O4 0.123(2) 0.0930(19) 0.0789(17) -0.0868(18) 0.0304(15) -0.0271(14) C4 0.0428(16) 0.0438(16) 0.0373(16) -0.0198(13) -0.0033(13) 0.0026(13) O5 0.0826(15) 0.0568(13) 0.0331(11) -0.0498(12) 0.0113(10) -0.0079(9) C5 0.0503(18) 0.0512(18) 0.0454(17) -0.0298(15) 0.0031(14) 0.0004(14) O6 0.144(2) 0.107(2) 0.0410(13) -0.1013(19) 0.0297(14) -0.0265(13) C6 0.059(2) 0.0548(19) 0.0531(19) -0.0352(16) 0.0000(15) -0.0062(15) C7 0.0502(18) 0.0593(19) 0.0415(16) -0.0258(16) 0.0001(14) -0.0061(14) C8 0.0459(17) 0.0440(17) 0.0434(17) -0.0236(14) -0.0042(13) 0.0019(13) C9 0.0431(17) 0.0521(18) 0.0405(16) -0.0235(14) -0.0029(13) 0.0034(13) C10 0.056(2) 0.077(2) 0.0489(19) -0.0366(18) -0.0025(15) 0.0072(17) C11 0.098(3) 0.123(3) 0.048(2) -0.070(3) 0.016(2) 0.001(2) C12 0.091(3) 0.073(2) 0.055(2) -0.059(2) 0.0251(18) -0.0305(18) C13 0.0609(19) 0.0490(17) 0.0404(16) -0.0341(15) 0.0078(14) -0.0176(13) C14 0.0501(17) 0.0433(16) 0.0432(16) -0.0253(14) 0.0043(13) -0.0123(13) C15 0.0411(16) 0.0345(14) 0.0370(15) -0.0185(12) 0.0007(12) -0.0031(12) C16 0.0463(16) 0.0393(15) 0.0300(14) -0.0234(13) 0.0039(12) -0.0005(11) C17 0.0602(19) 0.0537(18) 0.0326(15) -0.0297(15) 0.0037(14) -0.0096(13) C18 0.078(2) 0.068(2) 0.0346(16) -0.0471(19) 0.0100(15) -0.0033(15) C19 0.070(2) 0.0568(19) 0.0448(17) -0.0437(17) 0.0126(15) -0.0060(15) C20 0.0498(17) 0.0440(16) 0.0373(15) -0.0291(14) 0.0074(13) -0.0048(12) C21 0.075(2) 0.062(2) 0.0447(17) -0.0479(18) 0.0121(16) -0.0130(15) C22 0.116(3) 0.101(3) 0.055(2) -0.088(3) 0.017(2) -0.022(2) 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' Br Br -0.2901 2.4595 '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 C3 N1 C4 . . 126.9(2) ? C3 N1 H1 . . 116.6 ? C4 N1 H1 . . 116.6 ? O1 C1 C2 . . 126.6(3) ? O1 C1 H1A . . 116.7 ? C2 C1 H1A . . 116.7 ? C8 O2 H2 . . 109.5 ? C14 N2 C15 . . 129.3(2) ? C14 N2 H2A . . 115.3 ? C15 N2 H2A . . 115.3 ? C3 C2 C1 . . 121.4(3) ? C3 C2 Br1 . . 120.1(2) ? C1 C2 Br1 . . 118.3(2) ? N1 C3 C2 . . 125.7(3) ? N1 C3 H3 . . 117.1 ? C2 C3 H3 . . 117.1 ? C5 C4 C8 . . 119.5(3) ? C5 C4 N1 . . 124.4(3) ? C8 C4 N1 . . 116.2(2) ? C16 O5 H5A . . 109.5 ? C4 C5 C6 . . 120.2(3) ? C4 C5 H5 . . 119.9 ? C6 C5 H5 . . 119.9 ? C7 C6 C5 . . 120.8(3) ? C7 C6 H6 . . 119.6 ? C5 C6 H6 . . 119.6 ? C6 C7 C9 . . 120.4(3) ? C6 C7 H7 . . 119.8 ? C9 C7 H7 . . 119.8 ? O2 C8 C4 . . 116.5(3) ? O2 C8 C9 . . 122.7(3) ? C4 C8 C9 . . 120.8(3) ? C8 C9 C7 . . 118.3(3) ? C8 C9 C10 . . 119.7(3) ? C7 C9 C10 . . 121.9(3) ? O3 C10 C9 . . 120.3(3) ? O3 C10 C11 . . 119.8(3) ? C9 C10 C11 . . 120.0(3) ? C10 C11 H11A . . 109.5 ? C10 C11 H11B . . 109.5 ? H11A C11 H11B . . 109.5 ? C10 C11 H11C . . 109.5 ? H11A C11 H11C . . 109.5 ? H11B C11 H11C . . 109.5 ? O4 C12 C13 . . 128.6(3) ? O4 C12 H12 . . 115.7 ? C13 C12 H12 . . 115.7 ? C14 C13 C12 . . 121.4(3) ? C14 C13 Br2 . . 120.5(2) ? C12 C13 Br2 . . 118.1(2) ? N2 C14 C13 . . 126.7(3) ? N2 C14 H14 . . 116.6 ? C13 C14 H14 . . 116.6 ? C17 C15 C16 . . 118.7(2) ? C17 C15 N2 . . 117.0(2) ? C16 C15 N2 . . 124.3(2) ? O5 C16 C15 . . 119.3(2) ? O5 C16 C20 . . 120.9(2) ? C15 C16 C20 . . 119.8(2) ? C18 C17 C15 . . 122.0(3) ? C18 C17 H17 . . 119.0 ? C15 C17 H17 . . 119.0 ? C19 C18 C17 . . 119.4(3) ? C19 C18 H18 . . 120.3 ? C17 C18 H18 . . 120.3 ? C18 C19 C20 . . 120.7(3) ? C18 C19 H19 . . 119.6 ? C20 C19 H19 . . 119.6 ? C19 C20 C16 . . 119.3(3) ? C19 C20 C21 . . 121.3(3) ? C16 C20 C21 . . 119.3(2) ? O6 C21 C20 . . 121.2(3) ? O6 C21 C22 . . 118.9(3) ? C20 C21 C22 . . 119.9(3) ? C21 C22 H22A . . 109.5 ? C21 C22 H22B . . 109.5 ? H22A C22 H22B . . 109.5 ? C21 C22 H22C . . 109.5 ? H22A C22 H22C . . 109.5 ? H22B C22 H22C . . 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 Br1 C2 . 1.890(3) ? O1 C1 . 1.217(4) ? N1 C3 . 1.331(3) ? N1 C4 . 1.407(3) ? N1 H1 . 0.8600 ? C1 C2 . 1.421(4) ? C1 H1A . 0.9300 ? Br2 C13 . 1.885(3) ? O2 C8 . 1.356(3) ? O2 H2 . 0.8200 ? N2 C14 . 1.327(3) ? N2 C15 . 1.409(3) ? N2 H2A . 0.8600 ? C2 C3 . 1.351(4) ? O3 C10 . 1.238(4) ? C3 H3 . 0.9300 ? O4 C12 . 1.228(4) ? C4 C5 . 1.374(4) ? C4 C8 . 1.395(4) ? O5 C16 . 1.349(3) ? O5 H5A . 0.8200 ? C5 C6 . 1.387(4) ? C5 H5 . 0.9300 ? O6 C21 . 1.224(3) ? C6 C7 . 1.369(4) ? C6 H6 . 0.9300 ? C7 C9 . 1.401(4) ? C7 H7 . 0.9300 ? C8 C9 . 1.399(4) ? C9 C10 . 1.469(4) ? C10 C11 . 1.497(5) ? C11 H11A . 0.9600 ? C11 H11B . 0.9600 ? C11 H11C . 0.9600 ? C12 C13 . 1.398(4) ? C12 H12 . 0.9300 ? C13 C14 . 1.359(4) ? C14 H14 . 0.9300 ? C15 C17 . 1.380(4) ? C15 C16 . 1.397(4) ? C16 C20 . 1.406(4) ? C17 C18 . 1.380(4) ? C17 H17 . 0.9300 ? C18 C19 . 1.369(4) ? C18 H18 . 0.9300 ? C19 C20 . 1.396(4) ? C19 H19 . 0.9300 ? C20 C21 . 1.465(4) ? C21 C22 . 1.502(4) ? C22 H22A . 0.9600 ? C22 H22B . 0.9600 ? C22 H22C . 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 Br1 . 0.86 2.69 3.127(2) 113.0 yes O2 H2 O3 . 0.82 1.83 2.547(3) 145.6 yes N2 H2A O1 . 0.86 2.39 3.196(3) 155.8 yes N2 H2A Br2 . 0.86 2.72 3.160(2) 113.6 yes C3 H3 O4 2_676 0.93 2.38 3.288(4) 166.0 yes O5 H5A O6 . 0.82 1.78 2.513(3) 147.6 yes C12 H12 O6 2_665 0.93 2.63 3.503(4) 157.5 yes C14 H14 O5 . 0.93 2.16 2.794(3) 124.6 yes C17 H17 O1 . 0.93 2.39 3.194(4) 144.6 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 C1 C2 C3 . . . . -171.7(3) ? O1 C1 C2 Br1 . . . . 3.6(5) ? C4 N1 C3 C2 . . . . -175.1(3) ? C1 C2 C3 N1 . . . . 175.4(3) ? Br1 C2 C3 N1 . . . . 0.1(4) ? C3 N1 C4 C5 . . . . -3.9(5) ? C3 N1 C4 C8 . . . . 175.9(3) ? C8 C4 C5 C6 . . . . 1.1(4) ? N1 C4 C5 C6 . . . . -179.2(3) ? C4 C5 C6 C7 . . . . 0.3(5) ? C5 C6 C7 C9 . . . . -1.1(5) ? C5 C4 C8 O2 . . . . 179.4(3) ? N1 C4 C8 O2 . . . . -0.3(4) ? C5 C4 C8 C9 . . . . -1.7(4) ? N1 C4 C8 C9 . . . . 178.6(3) ? O2 C8 C9 C7 . . . . 179.8(3) ? C4 C8 C9 C7 . . . . 0.9(4) ? O2 C8 C9 C10 . . . . 0.5(4) ? C4 C8 C9 C10 . . . . -178.3(3) ? C6 C7 C9 C8 . . . . 0.5(4) ? C6 C7 C9 C10 . . . . 179.7(3) ? C8 C9 C10 O3 . . . . -0.6(5) ? C7 C9 C10 O3 . . . . -179.8(3) ? C8 C9 C10 C11 . . . . 179.0(3) ? C7 C9 C10 C11 . . . . -0.2(5) ? O4 C12 C13 C14 . . . . 179.2(4) ? O4 C12 C13 Br2 . . . . -0.6(6) ? C15 N2 C14 C13 . . . . 177.3(3) ? C12 C13 C14 N2 . . . . 179.7(3) ? Br2 C13 C14 N2 . . . . -0.5(4) ? C14 N2 C15 C17 . . . . 170.5(3) ? C14 N2 C15 C16 . . . . -11.8(5) ? C17 C15 C16 O5 . . . . -179.8(3) ? N2 C15 C16 O5 . . . . 2.5(4) ? C17 C15 C16 C20 . . . . 1.5(4) ? N2 C15 C16 C20 . . . . -176.1(3) ? C16 C15 C17 C18 . . . . 0.0(4) ? N2 C15 C17 C18 . . . . 177.8(3) ? C15 C17 C18 C19 . . . . -1.1(5) ? C17 C18 C19 C20 . . . . 0.6(5) ? C18 C19 C20 C16 . . . . 0.9(5) ? C18 C19 C20 C21 . . . . -176.8(3) ? O5 C16 C20 C19 . . . . 179.5(3) ? C15 C16 C20 C19 . . . . -2.0(4) ? O5 C16 C20 C21 . . . . -2.8(4) ? C15 C16 C20 C21 . . . . 175.8(3) ? C19 C20 C21 O6 . . . . -176.3(3) ? C16 C20 C21 O6 . . . . 6.0(5) ? C19 C20 C21 C22 . . . . 3.7(5) ? C16 C20 C21 C22 . . . . -174.0(3) ? _cod_database_fobs_code 2022529