#------------------------------------------------------------------------------ #$Date: 2024-08-07 01:03:54 +0300 (Wed, 07 Aug 2024) $ #$Revision: 293987 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023153.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_2023153 loop_ _publ_author_name 'Kumagai, Hitoshi' 'Kawata, Satoshi' 'Ogihara, Nobuhiro' _publ_section_title ; Crystal structures of 1,1'-bis-(carb-oxy-meth-yl)-4,4'-bipyridinium derivatives. ; _journal_coeditor_code JP2007 _journal_issue 'Pt 7' _journal_name_full 'Acta crystallographica. Section E, Crystallographic communications' _journal_page_first 695 _journal_page_last 698 _journal_paper_doi 10.1107/S2056989024005127 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac 'C14 H20 N2 O8' _chemical_formula_moiety 'C14 H20 N2 O8' _chemical_formula_sum 'C14 H20 N2 O8' _chemical_formula_weight 344.32 _chemical_name_systematic ; 1,1'-Bis(carboxylatomethyl)-4,4'-bipyridine-1,1'-diium ; _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 geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.0000 _cell_angle_beta 99.4832(14) _cell_angle_gamma 90.0000 _cell_formula_units_Z 2 _cell_length_a 6.2521(2) _cell_length_b 11.4122(4) _cell_length_c 11.1413(4) _cell_measurement_reflns_used 7055 _cell_measurement_temperature 296 _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 3.31 _cell_volume 784.07(5) _computing_cell_refinement ; RAPID-AUTO (Rigaku, 1995) ; _computing_data_collection ; RAPID-AUTO (Rigaku, 1995) ; _computing_data_reduction ; RAPID-AUTO (Rigaku, 1995) ; _computing_molecular_graphics ; CrystalStructure 4.3 (Rigaku, 2019) ; _computing_publication_material ; CrystalStructure 4.3 (Rigaku, 2019) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015) ; _computing_structure_solution ; Superflip (Palatinus & Chapuis, 2007) ; _diffrn_ambient_temperature 296 _diffrn_detector_area_resol_mean 10.000 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_unetI/netI 0.0231 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 7476 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.482 _diffrn_reflns_theta_min 3.512 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.120 _exptl_absorpt_correction_T_max 0.951 _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (ABSCOR; Rigaku, 1995) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 364.00 _exptl_crystal_size_max 0.480 _exptl_crystal_size_mid 0.460 _exptl_crystal_size_min 0.420 _refine_diff_density_max 0.40 _refine_diff_density_min -0.28 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_hydrogen_treatment mixed _refine_ls_number_parameters 125 _refine_ls_number_reflns 1793 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0479 _refine_ls_shift/su_max 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0813P)^2^+0.1761P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1211 _refine_ls_wR_factor_ref 0.1227 _reflns_number_gt 1678 _reflns_number_total 1793 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file jp2007.cif _cod_data_source_block bcbpy _cod_depositor_comments 'Adding full bibliography for 2023152--2023153.cif.' _cod_database_code 2023153 _shelx_hkl_file ; -1 0 0 1.99 0.31 1 0 0 1.80 0.27 1 0 -1 227.43 3.66 -1 0 1 223.62 4.20 1 0 -1 214.67 3.60 0 -2 0 1101.25 24.57 0 2 0 1005.05 22.41 0 0 2 1990.37 51.95 0 0 -2 1996.31 53.77 0 0 -2 1957.97 51.35 0 0 2 1969.59 52.02 -1 -1 0 1034.70 23.08 1 1 0 1022.10 22.73 1 1 -1 1744.33 44.60 1 -1 -1 1711.90 43.00 1 -1 -1 1709.26 43.13 -1 -1 1 1772.35 45.48 -1 1 1 1710.62 43.10 -1 1 1 1715.94 43.52 0 2 -1 4081.40 137.45 0 -2 -1 4295.11 138.84 0 2 1 4315.35 139.45 0 -2 1 4093.89 135.60 -1 0 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555.93 12.59 -2 8 2 300.63 5.93 -2 -8 2 307.88 7.42 2 8 -2 297.05 6.53 4 5 0 596.21 14.44 -4 -5 0 547.94 14.07 -4 5 0 592.22 12.01 -4 5 0 597.85 14.90 3 7 0 908.99 22.97 -3 7 0 888.32 21.40 -3 -7 0 907.55 22.44 -2 -8 -1 467.31 10.47 -2 8 -1 448.58 10.04 2 8 1 435.48 9.30 2 -8 1 453.61 9.86 4 4 2 40.46 1.26 4 4 2 39.18 0.93 -4 -4 -2 47.89 1.44 -4 4 -2 39.90 1.67 -3 7 2 65.19 2.01 -3 7 2 70.25 1.66 3 7 -2 70.01 2.95 -3 -7 2 98.52 4.25 3 5 4 511.53 11.15 -3 -5 -4 499.05 11.44 -3 5 -4 528.37 12.25 -2 6 6 56.17 0.92 -2 6 6 58.47 1.77 -2 6 6 56.42 0.94 -2 -6 6 62.54 2.36 2 6 -6 59.12 2.15 0 -9 0 0.32 0.51 0 9 0 -0.01 0.96 -3 0 -6 -0.02 0.34 -3 0 -6 3.66 0.59 -4 3 -3 73.69 3.30 4 3 3 72.99 1.36 -4 3 -3 72.12 0.98 -4 -3 -3 74.26 1.88 0 -8 4 146.31 3.71 0 8 4 148.93 2.33 0 -8 -4 147.73 2.52 0 8 4 147.08 3.56 0 8 -4 145.48 3.85 1 -2 8 179.00 3.82 -1 2 -8 187.15 4.07 -1 -2 -8 182.39 5.04 -1 2 -8 198.92 5.08 -1 -2 -8 186.43 4.28 1 2 8 188.34 5.24 -2 -3 8 303.78 8.38 2 3 -8 300.72 6.73 2 -3 -8 302.90 6.76 -2 3 8 324.09 5.77 -2 3 8 301.32 6.74 2 -3 -8 316.32 5.55 2 3 -8 319.21 8.46 -4 5 3 251.71 5.92 4 5 -3 259.95 5.76 -4 5 3 251.25 5.73 -4 5 3 249.16 4.61 -4 -5 3 255.02 5.96 -3 -1 -6 18.01 0.90 -3 1 -6 17.23 0.63 3 1 6 18.26 0.71 -3 -1 -6 16.99 0.76 -3 -1 -6 16.82 1.07 -3 1 -6 17.28 1.79 -1 6 -6 912.78 22.99 1 -6 6 945.56 25.01 -1 -6 -6 1012.55 21.24 1 6 6 871.98 23.28 -1 -6 -6 941.60 19.56 0 9 1 237.49 4.86 0 -9 1 236.24 5.17 0 9 -1 242.04 5.37 0 -9 -1 235.48 5.51 -1 8 4 251.33 4.67 1 8 -4 239.48 5.80 -1 8 4 244.07 5.47 -1 -8 4 241.15 5.89 -4 0 -4 323.20 6.87 -4 0 -4 322.29 7.07 -3 6 -3 363.20 8.36 3 6 3 354.30 7.57 3 -6 3 369.97 8.19 -3 -6 -3 358.46 7.41 3 6 3 347.29 7.75 4 -2 -6 2441.69 71.50 -4 2 6 2399.99 70.89 -4 -2 6 2416.46 72.31 4 2 -6 2402.82 71.01 4 -2 -6 2327.22 68.65 4 2 -6 2327.90 69.65 -1 7 -5 3.37 1.00 -1 -7 -5 1.15 0.37 1 -7 5 2.18 0.86 1 7 5 2.26 0.75 2 -5 -7 2.09 0.71 -2 -5 7 1.56 1.72 2 5 -7 0.21 0.89 -2 5 7 0.00 1.23 -2 5 7 1.65 0.20 -3 -7 -1 348.70 7.85 3 7 1 358.96 7.51 -3 7 -1 357.81 7.98 2 6 5 431.01 9.65 -2 6 -5 438.49 10.37 -2 -6 -5 473.18 9.13 2 -6 5 446.59 10.08 4 1 4 101.41 1.68 -4 -1 -4 97.04 2.42 -4 -1 -4 92.09 3.04 -4 1 -4 98.90 2.61 -4 1 -4 95.86 2.33 -3 5 6 7.32 0.73 -3 5 6 6.44 0.36 -3 5 6 7.34 0.60 3 5 -6 6.02 1.01 -3 -5 6 9.14 1.21 3 4 5 1694.48 46.11 -3 4 -5 1727.25 46.62 -3 4 -5 1673.60 46.82 -3 -4 -5 1711.19 46.20 -2 7 5 234.40 5.16 -2 -7 5 242.34 6.22 2 7 -5 219.11 7.07 -2 7 5 242.57 4.07 -2 7 5 240.96 4.21 1 -4 -8 246.31 5.60 -1 4 8 250.25 5.70 1 4 -8 243.29 5.90 -1 -4 8 246.76 5.71 1 4 -8 253.41 5.70 -4 -5 -1 87.93 2.31 4 5 1 92.06 2.20 -4 5 -1 91.53 2.54 -5 0 1 183.88 5.28 -5 0 2 0.09 1.07 5 0 -2 0.24 0.16 5 0 -2 0.53 0.58 -2 -8 3 669.15 16.09 2 8 -3 640.69 15.16 -2 8 3 634.77 14.64 -2 8 3 672.10 15.05 -3 7 3 54.17 1.19 -3 -7 3 55.57 2.25 -3 7 3 54.45 1.31 3 7 -3 58.58 1.90 -3 7 3 54.82 1.39 -3 -6 5 607.95 14.60 -3 6 5 634.62 13.09 -3 6 5 594.59 13.34 3 6 -5 601.37 14.22 -3 6 5 617.29 13.36 2 3 7 122.95 2.75 2 -3 7 121.40 2.87 -2 -3 -7 124.12 2.19 -2 -3 -7 120.47 2.24 -2 -3 -7 121.31 2.69 -2 3 -7 121.01 2.56 -2 3 -7 122.10 3.20 1 9 0 106.85 2.48 -1 -9 0 120.64 2.88 1 -9 0 107.43 2.45 -1 9 0 111.60 3.66 -5 -1 1 23.11 2.09 5 1 -1 25.06 0.43 5 1 -1 23.65 1.22 -5 1 1 23.16 1.23 2 8 2 24.08 1.23 -2 -8 -2 20.40 1.13 -2 8 -2 24.45 1.43 -5 1 2 20.70 1.82 -5 -1 2 17.06 1.94 5 1 -2 17.72 0.37 5 1 -2 19.31 1.11 3 0 -8 0.19 0.59 3 0 -8 0.28 0.41 -3 0 8 0.59 0.51 -1 -9 1 61.21 2.04 1 -9 -1 63.84 2.09 -1 9 1 63.94 1.67 1 9 -1 62.20 1.88 2 -7 4 1567.24 42.64 2 7 4 1523.05 43.39 -2 7 -4 1542.77 42.71 2 7 4 1571.14 41.23 -2 -7 -4 1642.53 43.52 0 -4 -8 326.90 7.35 0 4 -8 335.33 7.51 0 4 -8 302.78 9.66 0 4 8 330.24 9.00 0 -4 8 322.11 7.32 3 2 6 897.16 21.35 -3 -2 -6 948.98 22.36 -3 -2 -6 921.52 21.88 -3 2 -6 940.55 21.53 -3 2 -6 916.51 22.52 1 0 -9 49.64 1.30 -1 0 9 48.60 1.28 1 0 -9 49.70 1.85 -4 4 5 83.60 1.76 4 4 -5 85.69 2.42 -4 4 5 81.47 2.34 -4 -4 5 84.57 2.63 2 5 6 177.52 4.84 -2 5 -6 173.67 4.41 2 -5 6 173.17 4.05 -2 -5 -6 176.80 3.36 -2 -5 -6 170.42 2.91 0 9 -2 4.83 0.98 0 9 2 4.53 0.89 0 -9 2 8.90 0.93 0 -9 -2 5.80 0.49 -5 0 0 0.77 0.68 3 -1 -8 113.53 2.80 3 1 -8 118.21 2.84 -3 1 8 119.10 3.19 3 -1 -8 117.32 2.83 -3 -1 8 115.36 3.77 3 1 -8 116.26 2.60 1 -5 7 549.85 12.78 1 5 7 543.87 14.11 -1 -5 -7 601.70 11.28 -1 -5 -7 626.54 11.65 -1 5 -7 535.77 13.00 5 0 -3 3.55 1.34 -5 0 3 4.22 1.45 5 0 -3 4.38 0.26 1 1 -9 1645.56 44.34 -1 -1 9 1699.47 45.35 1 1 -9 1636.70 44.90 1 -1 -9 1666.07 43.57 1 -1 -9 1648.77 45.42 -1 1 9 1676.82 44.54 -1 -9 -1 3.04 0.63 1 9 1 2.05 0.51 1 -9 1 1.93 0.66 -1 9 -1 1.63 0.78 -4 2 -4 100.02 3.90 -4 -2 -4 100.49 2.37 4 2 4 102.26 1.80 -4 2 -4 102.59 1.69 -3 4 7 2013.88 54.55 -3 4 7 1898.43 55.64 3 4 -7 1918.90 55.02 3 -4 -7 1932.76 54.94 -3 -4 7 1993.71 57.23 -1 3 -8 46.46 1.54 -1 3 -8 48.39 2.09 1 3 8 47.06 2.57 -1 -3 -8 46.00 1.62 -1 -3 -8 48.63 1.35 -1 -3 -8 47.36 1.05 1 -3 8 48.20 1.57 -5 -1 0 11.64 1.06 -5 1 0 13.52 1.00 -5 1 3 272.99 7.09 5 -1 -3 284.71 5.10 -5 -1 3 270.66 6.12 5 1 -3 266.15 7.02 5 1 -3 281.46 4.96 -4 5 4 1059.31 25.39 -4 -5 4 1091.43 27.88 4 5 -4 1080.86 27.49 -4 5 4 1101.28 26.87 -4 5 4 1069.15 26.16 1 -8 4 126.96 3.34 1 8 4 127.11 2.33 1 8 4 131.43 3.33 -1 -8 -4 130.78 2.23 -1 8 -4 127.01 3.58 0 0 -9 0.21 0.69 0 0 9 0.12 0.39 0 0 -9 0.91 0.89 4 -3 -6 214.59 4.27 4 3 -6 226.27 5.12 -4 -3 6 231.94 5.46 -4 3 6 235.82 4.82 4 -3 -6 241.01 5.61 -4 3 6 221.44 4.50 1 7 -6 320.94 7.73 -1 7 6 318.43 8.52 -1 -7 6 327.95 7.76 -1 -9 2 45.30 1.83 1 9 -2 41.48 1.67 1 -9 -2 43.22 1.49 -1 9 2 42.12 1.68 5 2 -1 76.32 2.13 -5 -2 1 79.16 3.28 -5 2 1 73.34 2.06 5 2 -2 47.09 2.52 -5 2 2 47.41 1.57 -5 -2 2 46.40 1.75 0 7 -6 973.79 24.86 0 7 6 992.28 24.93 0 -7 6 1014.17 25.49 1 6 -7 107.27 3.28 -1 6 7 112.90 2.99 -1 -6 7 107.57 3.22 3 7 2 62.59 1.52 -3 -7 -2 63.73 1.73 -3 7 -2 63.76 2.21 -4 4 -3 234.71 4.04 4 4 3 234.92 4.92 -4 4 -3 233.44 6.95 -4 -4 -3 229.46 4.92 0 -1 -9 1534.13 39.64 0 1 -9 1548.84 41.95 0 1 -9 1548.26 41.21 0 1 9 1442.61 39.75 0 -1 -9 1553.02 44.10 0 -1 9 1613.30 43.59 0 1 9 1515.24 39.66 2 -4 -8 88.52 2.46 2 4 -8 86.87 3.71 -2 4 8 88.08 2.49 -2 -4 8 89.70 2.70 -2 4 8 88.52 1.52 3 -2 -8 6.01 0.84 -3 -2 8 6.97 0.94 -3 2 8 5.80 0.54 3 2 -8 5.52 0.86 -3 2 8 6.63 0.90 3 2 -8 5.79 0.78 3 -2 -8 6.07 0.43 0 6 -7 40.22 2.04 0 6 7 44.59 1.77 0 -6 7 41.28 1.89 1 -2 -9 14.54 0.44 1 2 -9 13.73 2.05 -1 2 9 13.86 0.72 -1 2 9 19.78 2.27 -1 -2 9 13.79 0.97 1 2 -9 13.48 1.02 1 -2 -9 14.68 1.21 -4 -5 -2 902.37 22.00 4 5 2 886.29 21.41 -4 5 -2 908.99 22.61 -4 6 1 60.32 1.14 4 6 -1 65.40 1.89 -4 -6 1 62.19 2.05 -4 6 1 63.97 1.81 -4 6 1 62.57 1.61 -3 -7 4 196.73 5.07 -3 7 4 192.80 4.08 -3 7 4 194.36 3.98 -3 7 4 194.84 3.69 3 7 -4 196.38 4.70 -5 -2 0 26.42 1.37 -5 2 0 27.29 1.28 5 2 0 27.70 1.28 2 0 -9 0.09 0.37 2 0 -9 -0.13 1.14 -2 0 9 0.34 0.44 -5 -2 3 265.86 6.13 5 2 -3 281.18 5.13 -5 2 3 263.67 5.78 5 2 -3 264.78 5.92 -5 0 -1 1985.05 57.25 2 8 -4 121.44 3.32 -2 8 4 123.37 3.94 -2 8 4 123.81 2.20 -2 -8 4 124.52 3.64 4 0 -7 -0.17 0.85 -4 0 7 0.26 0.57 4 0 -7 0.55 0.81 -1 -9 -2 639.12 13.87 1 -9 2 647.92 16.20 1 9 2 625.02 13.42 -1 9 -2 612.22 14.48 -4 -6 2 59.19 2.11 -4 6 2 58.86 2.30 4 6 -2 59.84 1.89 -4 6 2 56.76 1.46 -4 6 2 56.27 1.49 -3 3 -6 15.43 0.96 -3 -3 -6 13.83 1.04 -3 -3 -6 13.07 1.11 3 3 6 13.48 0.73 -3 3 -6 12.69 1.18 5 0 -4 0.09 0.44 5 0 -4 1.82 0.61 -5 0 4 -0.08 1.18 2 1 -9 81.21 3.50 2 1 -9 83.55 1.98 -2 1 9 86.82 2.38 -2 -1 9 84.66 2.13 2 -1 -9 83.32 2.43 2 -1 -9 84.87 2.10 0 9 3 76.22 1.44 0 9 -3 75.13 3.67 0 -9 3 75.21 2.36 0 -9 -3 75.20 1.39 4 6 0 59.49 1.73 -4 -6 0 58.65 1.92 -4 6 0 58.07 1.06 -4 6 0 58.51 2.84 -5 1 -1 7.76 0.92 -5 -1 -1 8.81 0.97 4 -1 -7 456.39 9.77 -4 -1 7 456.55 11.71 -4 1 7 464.01 10.11 4 -1 -7 460.96 10.00 4 1 -7 455.58 11.15 4 1 -7 459.53 10.02 0 -8 5 32.80 1.74 0 8 5 34.78 2.53 0 8 -5 31.95 1.82 -4 -3 -4 56.06 1.57 -4 3 -4 55.45 2.01 -4 3 -4 55.50 0.87 4 3 4 56.67 1.16 2 -8 3 1477.28 39.65 -2 -8 -3 1527.46 40.89 2 8 3 1453.32 37.49 -2 8 -3 1458.32 42.22 5 -1 -4 21.58 0.57 5 -1 -4 21.84 1.09 -5 -1 4 23.20 1.30 5 1 -4 20.52 1.17 5 1 -4 23.11 0.63 -5 1 4 22.41 1.17 -1 -8 5 105.43 3.21 1 8 -5 103.67 3.21 -1 8 5 106.13 1.47 -1 8 5 112.14 1.59 -1 8 5 109.41 2.89 0 2 9 2452.14 70.00 0 2 -9 2313.00 69.14 0 2 -9 2263.50 67.33 0 -2 -9 2289.70 68.68 0 -2 9 2355.02 69.34 0 -2 -9 2334.53 66.29 0 2 9 2290.92 68.99 -2 -4 -7 18.03 0.84 -2 4 -7 18.01 0.86 -2 -4 -7 17.97 0.51 -2 4 -7 17.39 1.39 2 4 7 17.40 1.63 2 -4 7 16.14 1.91 -3 6 -4 30.86 1.74 3 6 4 29.52 0.86 -3 -6 -4 29.32 1.48 3 6 4 30.63 1.80 3 -6 4 29.71 1.55 -1 9 3 35.95 0.88 1 9 -3 36.51 1.66 -1 -9 3 35.90 2.90 1 -9 -3 35.69 0.79 -3 5 -5 80.90 2.69 3 5 5 82.80 2.73 3 -5 5 83.27 2.49 -3 -5 -5 81.36 1.72 -1 5 8 1269.36 33.50 1 -5 -8 1293.01 33.84 1 5 -8 1251.59 33.33 -1 -5 8 1300.54 34.07 -5 3 1 31.79 1.30 5 3 -1 32.05 2.20 -5 -3 1 32.73 2.43 -5 3 2 210.31 4.60 -5 -3 2 211.01 4.94 5 3 -2 210.76 4.74 -2 0 -8 148.34 3.15 -2 0 -8 135.30 3.03 -4 6 3 65.08 1.53 -4 6 3 60.37 1.57 4 6 -3 62.68 2.04 -4 6 3 62.64 1.74 -4 -6 3 63.49 2.34 1 -4 8 7.76 1.00 1 4 8 7.54 0.98 -1 -4 -8 8.61 0.97 -1 -4 -8 7.55 0.35 -1 4 -8 8.45 1.21 -1 4 -8 7.56 0.87 3 3 -8 20.88 2.02 3 3 -8 21.99 1.25 3 -3 -8 23.25 2.02 -3 3 8 22.45 1.26 3 -3 -8 21.48 0.89 -3 -3 8 20.44 2.40 -3 3 8 22.25 0.72 2 2 -9 322.38 7.99 -2 2 9 328.66 7.57 2 2 -9 314.70 7.14 -2 2 9 328.68 6.15 2 -2 -9 319.68 7.28 2 -2 -9 327.46 6.47 -2 -2 9 326.73 7.24 2 6 -7 310.67 7.44 -2 6 7 316.72 7.15 -2 -6 7 328.37 7.86 -2 -1 -8 98.30 2.85 -2 1 -8 96.75 2.23 2 1 8 102.87 2.44 -2 1 -8 98.59 2.47 -2 -1 -8 97.98 3.08 5 2 1 345.90 5.75 -5 2 -1 304.12 7.07 -5 2 -1 297.02 6.71 -5 -2 -1 306.00 6.96 4 2 -7 110.28 3.54 -4 2 7 117.99 3.27 4 -2 -7 110.04 2.30 -4 -2 7 112.63 3.05 4 -2 -7 109.44 3.34 4 2 -7 111.33 3.77 2 7 -6 307.33 7.51 -2 -7 6 312.78 7.79 -2 7 6 365.97 6.26 -2 7 6 310.67 7.11 -2 7 6 353.29 5.95 -3 8 1 545.42 12.12 3 8 -1 539.45 12.41 -3 -8 1 560.43 13.26 0 5 8 3327.77 111.56 0 5 -8 3123.59 102.48 0 -5 8 3310.09 107.62 -1 3 9 97.36 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69.57 2.78 -6 -4 -6 67.27 2.25 -6 -4 -6 65.21 2.18 -6 4 -6 68.37 3.14 -4 6 -9 1.00 1.24 -4 -6 -9 0.46 0.35 -4 -6 -9 0.29 0.58 4 6 9 0.30 0.60 -4 6 -9 0.52 0.39 -6 9 2 0.72 0.86 -6 -9 2 0.96 2.48 -6 9 2 1.53 0.69 6 9 -2 1.25 1.67 3 10 -9 99.14 3.74 -3 -10 9 101.87 4.39 1 -14 1 -0.16 0.61 1 14 1 0.10 0.47 -1 -14 -1 0.14 0.48 -1 14 -1 0.38 0.71 -4 8 10 7.93 1.19 -4 -8 10 6.79 1.87 4 8 -10 5.34 1.45 7 0 -8 0.68 1.30 -7 0 8 -0.06 0.86 7 0 -8 0.38 0.37 -6 5 9 217.54 5.60 -6 -5 9 237.29 6.88 6 5 -9 235.70 6.77 6 5 -9 234.45 6.30 -5 0 -9 48.57 2.08 -5 0 -9 49.43 1.76 6 9 -1 30.13 1.73 -6 9 1 28.37 2.31 -6 -9 1 31.60 2.22 -6 9 1 28.16 1.76 -2 -12 7 2.07 1.53 2 12 -7 2.13 1.38 -3 11 -6 9.49 1.82 3 11 6 10.44 1.38 3 -11 6 9.85 2.68 6 3 -10 1.20 1.26 6 -3 -10 1.94 0.66 -6 -3 10 1.61 1.14 -6 3 10 0.49 1.06 6 3 -10 1.33 0.93 -3 -12 6 1.25 1.89 3 12 -6 8.05 1.48 1 6 12 3.72 1.22 1 -6 12 0.32 1.89 -1 6 -12 0.22 1.79 -1 6 -12 5.38 1.61 7 1 -8 21.29 1.52 -7 1 8 19.29 2.42 7 1 -8 19.85 1.25 7 -1 -8 20.13 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8 11 8.85 2.52 3 8 -11 8.77 1.64 -3 -8 11 12.87 1.89 -2 5 13 104.61 3.82 2 5 -13 102.06 5.52 2 -5 -13 100.66 3.68 2 5 -13 101.09 3.26 -2 -5 13 99.06 3.20 -5 11 1 264.34 6.21 -5 11 1 257.56 6.48 -5 -11 1 274.52 10.64 5 11 -1 263.08 8.02 5 11 -2 18.37 1.48 -5 11 2 20.08 1.67 -5 -11 2 25.16 2.43 -5 11 2 17.96 1.28 4 -5 -12 14.16 1.45 -4 -5 12 14.33 1.68 4 5 -12 13.18 2.41 4 5 -12 12.87 1.59 1 12 7 126.43 4.22 -1 12 -7 112.51 6.42 1 -12 7 119.83 4.11 6 7 4 4.30 0.50 -6 7 -4 3.83 1.31 -6 7 -4 3.58 1.56 -6 -7 -4 3.45 1.56 5 10 3 217.95 5.90 -5 10 -3 206.19 6.16 5 10 3 204.14 6.11 -5 -10 -3 207.99 5.42 -1 8 -11 11.03 2.31 1 -8 11 13.65 1.62 1 8 11 11.80 2.80 -1 8 -11 14.16 2.09 1 10 -10 143.43 5.21 -1 10 10 162.54 5.16 -1 -10 10 150.53 5.13 -5 5 -8 3.93 1.46 -5 -5 -8 4.38 0.64 -5 -5 -8 3.98 1.07 5 5 8 3.71 0.56 -1 14 -2 0.62 1.42 1 -14 2 -0.19 0.69 -1 -14 -2 0.13 0.71 1 14 2 0.21 0.40 2 -13 4 66.71 2.63 -2 13 -4 61.40 2.79 2 13 4 66.12 2.88 -7 -5 6 57.87 3.00 -7 5 6 56.04 1.97 7 5 -6 57.04 1.49 -7 5 6 54.86 1.88 7 5 -6 59.37 2.65 -4 1 13 2.63 0.60 4 1 -13 3.51 0.64 4 -1 -13 2.07 0.47 -4 -1 13 3.01 1.38 -6 6 -5 36.64 2.24 -6 -6 -5 35.14 1.61 -6 6 -5 35.52 4.27 -7 -2 8 43.16 2.37 -7 2 8 41.56 1.82 7 -2 -8 45.06 1.58 7 2 -8 45.56 2.10 7 2 -8 42.97 1.24 -5 -10 6 3.07 1.75 -5 10 6 1.61 0.47 -5 10 6 1.48 0.68 5 10 -6 0.92 1.20 -5 -2 -9 210.37 4.92 -5 2 -9 213.06 5.32 -5 2 -9 208.54 7.52 -5 -2 -9 207.73 5.07 -7 -4 7 10.19 3.11 7 4 -7 10.11 1.15 -7 4 7 10.08 1.04 7 4 -7 10.81 1.51 3 11 -8 90.52 3.62 -3 -11 8 100.27 6.68 0 -14 3 108.16 3.34 0 14 -3 102.76 3.40 -4 12 4 335.49 7.03 -4 -12 4 345.09 10.14 4 12 -4 324.19 8.49 -4 12 4 328.29 7.93 1 0 -14 0.16 1.22 1 0 -14 2.23 0.45 -1 0 14 0.28 0.70 -7 -5 -2 10.94 1.42 -7 5 -2 9.15 2.56 -7 5 -2 9.53 1.71 -1 11 9 34.63 2.36 -1 -11 9 32.26 4.31 1 11 -9 30.13 2.58 5 -5 -11 20.51 1.37 5 5 -11 19.34 1.57 5 5 -11 20.08 1.54 -5 -5 11 21.05 1.98 -6 9 4 18.24 1.03 -6 9 4 19.01 1.17 -6 -9 4 26.33 4.30 6 9 -4 19.52 2.94 -4 9 -7 0.52 1.94 4 9 7 0.34 1.05 -4 9 -7 -0.04 0.38 -4 7 11 9.04 1.33 4 7 -11 9.79 1.57 4 7 -11 11.29 1.42 -4 -7 11 10.17 1.87 -5 11 0 11.11 1.34 -5 -11 0 10.63 1.72 5 11 0 10.02 1.10 3 -7 10 38.67 2.30 3 7 10 37.46 1.83 -3 7 -10 36.17 2.83 -3 7 -10 37.89 1.45 -6 2 -7 5.63 2.50 -6 2 -7 6.98 1.21 -6 -2 -7 6.24 1.09 -6 -2 -7 5.63 1.02 -7 2 -4 0.22 1.10 -7 -2 -4 0.18 0.92 -7 -2 -4 0.56 0.92 -7 2 -4 -0.02 1.68 -7 4 -3 131.30 4.52 -7 -4 -3 129.02 3.99 -7 4 -3 133.49 4.14 -5 11 3 87.89 2.87 -5 11 3 83.54 2.38 5 11 -3 84.93 2.96 -5 -11 3 88.51 4.21 5 2 -12 20.69 1.25 5 2 -12 18.66 1.64 5 -2 -12 19.36 1.29 -5 2 12 21.09 1.61 -5 -2 12 23.11 1.58 5 -2 -12 19.40 1.53 -1 -1 14 176.21 3.73 1 1 -14 181.22 4.64 1 1 -14 177.87 5.26 1 -1 -14 179.19 5.33 2 -7 11 92.73 3.28 -2 7 -11 93.59 2.79 -2 7 -11 95.61 6.73 2 7 11 95.11 3.27 -3 5 -11 0.60 1.27 -3 5 -11 -0.04 0.98 3 5 11 0.24 0.74 1 14 -3 85.16 3.01 -1 -14 3 83.30 4.50 0 5 13 87.43 5.16 0 -5 -13 86.72 3.27 0 5 -13 79.31 3.26 0 -5 13 80.26 3.91 0 5 -13 84.94 3.17 2 0 -14 1.89 0.46 -2 0 14 1.71 0.46 -5 -8 -6 26.17 1.12 5 8 6 26.84 1.18 -5 8 -6 25.80 2.38 -1 -13 6 2.28 2.45 1 13 -6 2.63 1.39 -1 13 6 3.32 1.31 0 13 -6 3.55 1.51 0 -13 6 4.60 1.41 0 13 6 4.41 1.45 0 -10 10 358.05 9.85 0 10 -10 324.50 9.66 0 10 10 366.22 9.96 3 -13 2 80.34 2.75 3 13 2 83.35 2.09 -3 13 -2 79.00 2.98 -3 -13 -2 81.88 2.40 -1 -9 11 9.59 1.77 1 9 -11 10.16 1.93 -1 9 11 11.04 1.75 4 8 8 45.83 1.73 -4 8 -8 44.31 1.78 -4 8 -8 44.97 4.64 -4 -2 13 188.00 6.03 4 2 -13 189.15 5.25 4 2 -13 187.13 4.46 4 -2 -13 190.18 5.30 4 12 2 0.41 0.78 -4 -12 -2 -0.71 0.83 -4 12 -2 0.02 0.91 2 1 -14 0.63 0.79 2 1 -14 -0.13 1.07 -2 -1 14 0.44 0.83 0 11 9 0.16 1.01 0 -11 9 0.28 1.06 0 11 -9 -0.50 1.19 -6 -8 -3 115.80 3.36 -6 8 -3 121.14 3.89 -6 8 -3 117.63 4.24 6 8 3 115.16 2.55 -5 -8 9 106.88 4.49 5 8 -9 93.50 5.38 -5 8 9 105.04 2.89 -7 6 5 2.16 0.76 -7 -6 5 1.82 2.39 7 6 -5 1.29 1.13 7 6 -5 0.16 0.46 -7 6 5 1.62 1.27 4 10 6 13.78 1.23 -4 10 -6 10.93 1.97 -2 -10 10 85.31 3.85 2 10 -10 86.18 5.75 -3 0 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9 -11 78.28 3.10 0 -9 11 89.07 5.30 -6 3 -7 101.14 3.79 -6 3 -7 103.68 3.34 -6 -3 -7 99.56 2.92 -6 -3 -7 96.50 2.86 -7 3 -4 203.14 6.26 -7 3 -4 205.69 5.84 -7 -3 -4 199.97 5.55 -7 -3 -4 197.30 5.54 5 3 -12 56.09 2.34 5 -3 -12 59.51 1.39 5 -3 -12 57.00 2.27 -5 -3 12 56.32 3.86 -5 3 12 57.18 2.08 5 3 -12 56.03 2.09 6 0 -11 0.08 0.61 6 0 -11 0.38 0.68 -6 0 11 0.21 0.76 2 -14 1 5.86 0.94 -2 -14 -1 6.56 0.84 2 14 1 6.35 0.74 -2 14 -1 4.69 1.06 -6 9 5 47.00 1.50 -6 9 5 48.53 2.38 -6 9 5 47.28 1.22 6 9 -5 49.10 2.57 -6 -9 5 48.93 3.21 -7 7 2 24.22 1.69 -7 -7 2 21.88 2.21 7 7 -2 24.65 3.07 -7 7 2 22.92 1.50 3 7 -12 100.08 5.25 -3 -7 12 95.51 3.73 -3 7 12 100.90 3.62 3 7 -12 92.65 3.65 0 -1 14 55.49 1.52 0 -1 -14 57.80 2.63 0 1 -14 53.23 1.65 -2 0 -13 -1.60 1.44 -2 0 -13 -0.41 0.70 -6 6 9 25.39 0.96 6 6 -9 25.66 3.23 6 6 -9 26.08 1.44 -6 6 9 23.86 0.90 -6 -6 9 29.67 4.09 2 10 9 88.50 3.27 2 -10 9 81.07 3.47 -2 10 -9 76.68 3.79 -3 -2 -12 0.52 0.40 -3 2 -12 1.23 0.99 -3 2 -12 0.98 0.64 -3 -2 -12 0.33 0.71 -3 -2 -12 0.09 1.02 4 5 10 0.19 0.57 -4 5 -10 0.19 0.40 -4 5 -10 0.31 1.12 -6 -1 11 276.64 7.05 6 -1 -11 269.36 6.47 6 -1 -11 282.06 6.40 6 1 -11 283.91 6.82 6 1 -11 271.12 6.58 -6 1 11 281.47 6.65 0 12 8 96.89 3.72 0 -12 8 92.06 3.76 0 12 -8 86.51 3.89 4 12 -5 51.70 2.53 -4 -12 5 54.75 3.40 4 3 -13 159.62 4.81 4 3 -13 164.89 5.39 -4 -3 13 164.16 4.38 4 -3 -13 161.61 4.73 -4 0 -11 0.16 0.47 -4 0 -11 -0.59 0.52 -4 0 -11 -1.81 1.29 7 7 -3 307.12 8.28 -7 7 3 295.82 8.74 -7 7 3 293.43 7.50 -7 -7 3 299.78 8.71 0 14 4 157.33 5.07 0 14 -4 142.25 4.45 0 -14 4 153.96 4.53 -8 0 2 0.70 1.15 3 -5 -13 32.15 2.14 -3 -5 13 33.12 3.20 3 5 -13 29.95 3.66 3 5 -13 31.52 1.81 -3 5 13 31.32 2.15 -2 -1 -13 12.75 2.12 -2 -1 -13 8.01 0.85 -2 1 -13 7.89 1.15 -2 1 -13 8.12 1.11 -1 6 13 1.05 1.20 -1 -6 13 0.04 0.95 1 6 -13 0.84 1.85 1 6 -13 1.02 1.12 7 7 -1 46.50 2.25 -7 -7 1 43.35 2.46 -7 7 1 42.40 1.95 -7 7 1 42.79 2.19 -6 8 7 150.64 3.33 -6 -8 7 161.06 5.60 -6 8 7 155.22 3.37 6 8 -7 149.61 6.67 -6 8 7 151.38 3.36 -8 0 3 0.67 1.99 2 11 8 12.28 1.63 2 -11 8 11.59 1.79 -2 11 -8 11.92 2.04 -2 -13 6 54.39 2.99 2 13 -6 55.41 2.87 -4 7 -9 47.11 1.33 -4 7 -9 43.29 4.67 4 7 9 45.40 2.55 1 14 -4 23.10 3.08 -1 -14 4 23.05 3.16 -4 -1 -11 1.47 0.71 -4 1 -11 0.92 0.50 -4 1 -11 0.84 0.91 -4 1 -11 0.01 0.63 -4 -1 -11 0.53 0.53 -8 1 2 52.66 2.64 -8 -1 2 50.82 4.31 -3 -12 7 26.08 4.36 3 12 -7 23.00 3.43 7 5 -7 17.21 1.72 -7 5 7 14.43 1.12 7 5 -7 16.46 1.38 -7 -5 7 16.67 2.09 -8 -1 3 4.46 1.47 -8 1 3 4.42 1.37 1 3 -14 45.42 2.59 -1 -3 14 40.40 1.59 1 -3 -14 42.22 4.31 1 3 -14 40.07 2.57 3 -10 8 82.79 5.21 -3 10 -8 74.78 5.94 3 10 8 87.32 4.42 1 -13 6 35.48 3.78 -1 13 -6 35.98 2.46 1 13 6 40.69 2.48 1 8 -12 27.92 3.60 -1 8 12 27.95 2.22 -1 -8 12 24.88 2.09 1 8 -12 25.94 2.30 -8 0 1 -1.24 2.25 -2 9 -10 53.52 3.23 2 -9 10 55.85 2.81 2 9 10 59.72 4.05 -2 9 -10 57.61 2.18 -3 13 -3 430.42 11.56 -3 -13 -3 453.97 10.37 3 -13 3 458.90 11.87 3 13 3 464.45 11.13 7 0 -9 9.82 0.69 -7 0 9 6.89 1.28 7 0 -9 6.87 1.09 -1 7 -12 0.13 1.25 -1 7 -12 0.19 0.85 1 7 12 0.40 1.03 1 -7 12 0.11 1.63 0 -2 -14 131.34 4.19 0 2 -14 132.47 4.14 0 -2 14 127.91 3.02 0 2 -14 128.69 3.29 4 11 5 166.40 4.53 -4 11 -5 159.18 5.41 -2 -6 13 -0.01 1.01 2 6 -13 0.39 1.18 2 6 -13 1.28 1.04 -2 6 13 1.06 1.22 5 10 4 74.40 2.27 -5 -10 -4 74.39 3.38 -5 10 -4 73.90 3.43 -2 -14 3 10.30 1.49 -2 14 3 8.77 0.68 2 14 -3 10.96 2.28 -3 0 14 0.18 0.43 3 0 -14 0.29 0.39 4 6 -12 15.02 2.73 4 6 -12 12.18 1.35 -4 6 12 14.46 1.53 -4 -6 12 0.04 3.04 -7 -5 -3 136.64 4.16 -7 5 -3 142.39 4.47 -7 5 -3 144.09 4.93 -5 -6 -8 0.15 1.00 -5 -6 -8 4.80 0.60 5 6 8 4.43 0.61 -5 6 -8 4.76 1.56 -6 2 11 28.49 1.36 6 -2 -11 30.17 1.18 6 -2 -11 29.86 1.42 6 2 -11 30.18 1.62 6 2 -11 30.19 1.52 -6 -2 11 30.17 1.91 -2 13 -5 1.71 2.41 2 -13 5 2.62 1.23 2 13 5 3.31 1.32 -7 -6 6 55.83 3.10 7 6 -6 56.20 2.68 -7 6 6 52.15 2.71 -7 6 6 49.44 1.79 7 6 -6 55.52 1.58 4 12 3 55.44 1.54 4 12 3 54.28 2.34 -4 12 -3 52.38 2.70 -4 -12 -3 55.74 2.09 -8 0 4 201.50 5.88 -8 1 1 133.41 4.45 -8 -1 1 132.55 4.55 6 9 2 100.67 3.10 -6 9 -2 103.16 3.35 -6 9 -2 100.81 3.73 -6 -9 -2 99.20 3.18 6 9 2 101.09 2.90 7 -1 -9 3.37 0.53 -7 1 9 2.77 1.69 7 1 -9 3.48 1.69 7 1 -9 1.22 0.97 -7 -1 9 3.68 2.04 7 -1 -9 2.66 0.85 -3 9 -9 147.66 3.67 3 -9 9 145.22 4.70 -3 9 -9 134.36 5.03 3 9 9 146.35 4.24 5 10 -7 88.93 3.46 -5 10 7 89.38 2.44 -5 -10 7 94.81 4.46 -7 7 4 -0.14 0.73 -7 -7 4 1.22 2.18 7 7 -4 0.04 1.78 -7 7 4 0.59 1.16 2 -3 -14 7.09 1.57 -2 -3 14 7.54 0.96 2 3 -14 7.76 0.94 -2 2 -13 90.85 2.80 -2 -2 -13 90.87 2.89 -2 2 -13 83.82 2.95 -2 14 -2 21.78 1.59 2 14 2 22.24 0.94 2 -14 2 22.11 1.44 -2 -14 -2 21.13 1.60 2 12 -8 22.83 2.21 -2 -12 8 23.38 2.43 3 1 -14 22.70 1.98 3 1 -14 22.94 1.01 -3 -1 14 22.04 1.69 7 7 0 153.74 4.40 -7 7 0 146.89 4.19 -7 7 0 147.15 4.64 -7 -7 0 145.82 4.61 -7 0 -5 444.40 12.00 -7 0 -5 417.91 12.98 -7 6 -2 33.59 2.41 -7 6 -2 33.13 2.08 -7 -6 -2 31.71 1.95 -4 -2 -11 15.08 1.06 -4 -2 -11 15.95 0.83 -4 2 -11 15.43 1.60 -4 2 -11 16.07 0.86 -8 1 4 4.20 2.32 -8 -1 4 4.10 1.46 -5 11 -2 131.45 6.12 5 11 2 138.38 3.41 -5 -11 -2 132.13 3.93 5 6 -11 8.45 1.38 -5 6 11 7.35 1.14 5 6 -11 8.61 1.33 -5 -6 11 8.13 1.74 3 13 -5 479.87 12.89 -3 -13 5 478.11 16.50 -8 -2 2 54.05 2.82 -8 2 2 52.19 2.64 7 4 -8 124.75 3.99 7 4 -8 120.78 2.79 -7 -4 8 121.09 4.38 -7 4 8 116.45 4.18 -5 -4 -9 -0.03 1.09 -5 4 -9 2.42 2.35 5 4 9 2.91 0.54 -5 -4 -9 2.67 0.60 1 -11 9 2.24 2.55 -1 11 -9 1.82 2.86 1 11 9 3.60 1.40 1 -10 10 7.62 1.63 -1 10 -10 6.39 1.88 1 10 10 7.04 1.57 -8 2 3 81.19 4.83 -8 -2 3 81.99 3.49 -5 11 5 212.90 4.49 -5 11 5 209.73 4.58 -5 -11 5 223.28 7.42 5 11 -5 212.30 6.05 -2 -8 12 298.40 8.31 2 8 -12 305.86 8.53 2 8 -12 323.78 8.87 -2 8 12 314.23 8.74 -3 3 -12 149.18 3.71 -3 3 -12 142.72 4.53 -7 1 -5 48.88 4.27 -7 1 -5 48.20 2.40 -7 -1 -5 47.42 3.89 -7 -1 -5 47.47 2.37 -3 11 -7 13.28 3.61 3 11 7 15.49 1.56 3 -11 7 14.27 3.09 -6 5 10 111.67 2.55 6 5 -10 114.60 3.68 6 5 -10 112.76 3.17 -6 -5 10 117.00 4.25 -3 6 -11 59.35 1.86 -3 6 -11 59.85 3.24 3 6 11 63.79 2.35 6 7 5 107.18 2.88 -6 7 -5 110.04 4.33 -6 7 -5 118.44 4.01 -6 -7 -5 108.55 4.09 0 -6 13 75.47 2.77 0 6 -13 75.15 3.24 0 6 -13 77.12 3.03 0 6 13 76.17 3.26 -4 9 10 4.79 1.13 -4 -9 10 4.80 1.83 4 9 -10 3.81 1.43 -6 -4 -7 19.60 1.25 -6 4 -7 19.33 2.06 -6 -4 -7 18.03 1.24 -7 4 -4 2.23 1.51 -1 5 -13 1.39 2.05 1 5 13 0.12 1.95 -5 -4 12 107.35 3.69 5 4 -12 109.34 4.81 5 -4 -12 101.79 3.19 -8 2 1 10.19 1.64 -7 2 9 26.92 1.50 7 2 -9 29.50 1.76 4 10 -9 7.97 1.63 3 2 -14 2.26 1.15 ; _shelx_hkl_checksum 23640 _shelx_res_file ; TITL 160728kmgh-5 shelxl.res created by SHELXL-2018/3 at 17:24:12 on 18-Jan-2024 CELL 0.71075 6.25212 11.41220 11.14130 90.00000 99.48320 90.00000 ZERR 2 0.00024 0.00044 0.00039 0.00000 0.00140 0.00000 LATT 1 SYMM .50-X, .50+Y, .50-Z SFAC C H N O UNIT 28 40 4 16 L.S. 10 FMAP 2 PLAN 185 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP 23.0 ACTA SIZE 0.480 0.460 0.420 WGHT 0.081300 0.176100 FVAR 1.42723 O1 4 0.516132 0.685083 0.030406 11.00000 0.02413 0.03372 = 0.01898 0.00342 0.00712 -0.00429 O2 4 0.485703 0.708875 0.226992 11.00000 0.02275 0.02640 = 0.01926 -0.00101 0.00374 -0.00356 O3 4 0.806837 0.879022 0.299099 11.00000 0.02655 0.02824 = 0.02587 0.00551 0.00330 -0.00596 O4 4 0.414171 0.747974 0.467451 11.00000 0.02098 0.03801 = 0.02413 -0.00648 0.00413 -0.00005 N1 3 0.178380 0.542783 0.220705 11.00000 0.01854 0.01852 = 0.01624 0.00003 0.00449 -0.00249 C7 1 0.288702 0.469293 0.303540 11.00000 0.02063 0.02039 = 0.02211 0.00229 0.00671 0.00283 AFIX 43 H7 2 0.411238 0.430906 0.286205 11.00000 -1.20000 AFIX 0 C6 1 0.221084 0.450721 0.413633 11.00000 0.02146 0.01978 = 0.02092 0.00395 0.00590 0.00318 AFIX 43 H6 2 0.297168 0.399296 0.469856 11.00000 -1.20000 AFIX 0 C5 1 0.038386 0.508992 0.441027 11.00000 0.01732 0.01547 = 0.01712 -0.00045 0.00371 -0.00229 C4 1 -0.071031 0.584730 0.353177 11.00000 0.01805 0.02122 = 0.01933 0.00133 0.00452 0.00156 AFIX 43 H4 2 -0.193261 0.624817 0.368421 11.00000 -1.20000 AFIX 0 C3 1 0.001730 0.600212 0.243904 11.00000 0.01907 0.02190 = 0.01858 0.00247 0.00289 0.00163 AFIX 43 H3 2 -0.071887 0.650736 0.185822 11.00000 -1.20000 AFIX 0 C2 1 0.261948 0.566484 0.106753 11.00000 0.02144 0.02302 = 0.01506 -0.00031 0.00576 -0.00175 AFIX 23 H2A 2 0.143316 0.591106 0.044479 11.00000 -1.20000 H2B 2 0.322475 0.495057 0.079110 11.00000 -1.20000 AFIX 0 C1 1 0.437895 0.662595 0.124605 11.00000 0.01619 0.02087 = 0.01823 0.00265 0.00354 0.00128 H9 2 0.708985 0.829087 0.270024 11.00000 0.04076 H8 2 0.860319 0.853784 0.369286 11.00000 0.04916 H10 2 0.400135 0.736475 0.387330 11.00000 0.04062 H11 2 0.284756 0.755070 0.482022 11.00000 0.04275 HKLF 4 REM 160728kmgh-5 REM wR2 = 0.1227, GooF = S = 1.110, Restrained GooF = 1.110 for all data REM R1 = 0.0479 for 1678 Fo > 4sig(Fo) and 0.0494 for all 1793 data REM 125 parameters refined using 0 restraints END WGHT 0.0813 0.1761 REM Instructions for potential hydrogen bonds EQIV $2 -x+3/2, y-1/2, -z+1/2 HTAB C7 O3_$2 EQIV $3 -x+1, -y+1, -z+1 HTAB C6 O4_$3 EQIV $4 x-1, y, z HTAB C4 O2_$4 EQIV $5 x-1/2, -y+3/2, z-1/2 HTAB C2 O4_$5 HTAB O3 O2 EQIV $6 x+1/2, -y+3/2, z+1/2 HTAB O3 O1_$6 HTAB O4 O2 EQIV $7 x-1/2, -y+3/2, z+1/2 HTAB O4 O1_$7 REM Highest difference peak 0.401, deepest hole -0.276, 1-sigma level 0.082 Q1 1 0.3481 0.6167 0.1205 11.00000 0.05 0.36 Q2 1 0.1460 0.4905 0.4374 11.00000 0.05 0.35 Q3 1 -0.0225 0.5928 0.3009 11.00000 0.05 0.33 Q4 1 -0.0047 0.5540 0.4056 11.00000 0.05 0.31 Q5 1 0.0000 0.5000 0.5000 10.50000 0.05 0.31 Q6 1 -0.0348 0.5355 0.3847 11.00000 0.05 0.31 Q7 1 0.2472 0.4646 0.3588 11.00000 0.05 0.28 Q8 1 0.2198 0.5516 0.1803 11.00000 0.05 0.28 Q9 1 0.2337 0.5107 0.2520 11.00000 0.05 0.25 Q10 1 0.5173 0.7025 0.5308 11.00000 0.05 0.24 Q11 1 -0.0643 0.6457 0.1543 11.00000 0.05 0.21 Q12 1 0.0016 0.6180 -0.0727 11.00000 0.05 0.19 Q13 1 0.0828 0.6437 0.0228 11.00000 0.05 0.19 Q14 1 0.7268 0.7590 0.4384 11.00000 0.05 0.18 Q15 1 -0.2098 0.6150 0.2871 11.00000 0.05 0.17 Q16 1 0.5110 0.8829 0.2768 11.00000 0.05 0.17 Q17 1 0.7173 0.8611 0.3918 11.00000 0.05 0.16 Q18 1 0.4818 0.6495 0.2789 11.00000 0.05 0.16 Q19 1 0.8353 0.8816 0.2283 11.00000 0.05 0.15 Q20 1 0.5103 0.4025 0.5614 11.00000 0.05 0.14 Q21 1 0.5756 0.3913 0.4358 11.00000 0.05 0.14 Q22 1 0.5338 0.5899 0.2320 11.00000 0.05 0.13 Q23 1 -0.2830 0.6408 0.3883 11.00000 0.05 0.13 Q24 1 -0.1019 0.4852 0.1375 11.00000 0.05 0.13 Q25 1 1.0342 0.8033 0.2938 11.00000 0.05 0.13 Q26 1 0.2856 0.7587 0.5889 11.00000 0.05 0.13 Q27 1 0.1447 0.4392 0.0100 11.00000 0.05 0.13 Q28 1 0.5000 0.5000 0.5000 10.50000 0.05 0.12 Q29 1 0.4957 0.5750 0.3365 11.00000 0.05 0.12 Q30 1 0.5806 0.6607 0.3824 11.00000 0.05 0.12 Q31 1 0.0266 0.7579 0.1307 11.00000 0.05 0.12 Q32 1 0.2305 0.8549 0.4167 11.00000 0.05 0.12 Q33 1 -0.0478 0.5068 0.0820 11.00000 0.05 0.12 Q34 1 0.7282 0.8169 0.1966 11.00000 0.05 0.12 Q35 1 0.5716 0.5021 0.3807 11.00000 0.05 0.11 Q36 1 0.8734 0.7934 0.1966 11.00000 0.05 0.11 Q37 1 0.6808 0.9639 0.2258 11.00000 0.05 0.11 Q38 1 0.7508 0.7209 0.3017 11.00000 0.05 0.11 Q39 1 -0.2467 0.4740 0.3860 11.00000 0.05 0.10 Q40 1 0.6667 0.5992 0.1375 11.00000 0.05 0.10 Q41 1 0.5117 0.7350 0.3324 11.00000 0.05 0.10 Q42 1 -0.1507 0.6827 0.3658 11.00000 0.05 0.10 Q43 1 0.2131 0.7266 0.1406 11.00000 0.05 0.10 Q44 1 0.5148 0.8086 0.0354 11.00000 0.05 0.10 Q45 1 -0.1788 0.6005 0.0431 11.00000 0.05 0.10 Q46 1 0.3469 0.4373 0.4880 11.00000 0.05 0.09 Q47 1 0.4935 0.4808 0.2645 11.00000 0.05 0.09 Q48 1 -0.0954 0.5996 0.0452 11.00000 0.05 0.09 Q49 1 -0.0709 0.4124 0.3517 11.00000 0.05 0.09 Q50 1 0.2860 0.6556 0.6007 11.00000 0.05 0.09 Q51 1 0.6942 0.6603 0.2382 11.00000 0.05 0.09 Q52 1 0.3236 0.6452 0.5850 11.00000 0.05 0.09 Q53 1 -0.0835 0.4491 0.3215 11.00000 0.05 0.08 Q54 1 -0.1568 0.4256 0.4364 11.00000 0.05 0.08 Q55 1 0.7735 1.0213 0.2913 11.00000 0.05 0.08 Q56 1 0.9006 0.9998 0.3527 11.00000 0.05 0.08 Q57 1 -0.2269 0.5278 0.1076 11.00000 0.05 0.08 Q58 1 0.2767 0.5056 0.5270 11.00000 0.05 0.08 Q59 1 0.1688 0.5375 0.0326 11.00000 0.05 0.08 Q60 1 -0.0615 0.7443 0.2824 11.00000 0.05 0.08 Q61 1 0.4844 0.3393 0.3187 11.00000 0.05 0.08 Q62 1 1.0269 0.8016 0.4113 11.00000 0.05 0.07 Q63 1 0.3305 0.8405 0.2852 11.00000 0.05 0.06 Q64 1 0.0000 0.5000 0.0000 10.50000 0.05 0.06 Q65 1 0.3118 0.3345 0.3002 11.00000 0.05 0.05 Q66 1 0.3100 0.4386 -0.0332 11.00000 0.05 0.05 Q67 1 0.2766 0.4979 -0.0459 11.00000 0.05 0.04 Q68 1 0.5065 0.3953 0.2731 11.00000 0.05 0.04 Q69 1 0.0642 0.5885 0.1300 11.00000 0.05 0.03 Q70 1 0.4265 0.5209 0.0976 11.00000 0.05 0.03 Q71 1 0.2932 0.6228 0.3575 11.00000 0.05 0.02 Q72 1 0.1775 0.6823 0.2377 11.00000 0.05 0.02 Q73 1 1.0679 0.8743 0.4131 11.00000 0.05 0.01 ; _shelx_res_checksum 37491 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 -1/2+X,-1/2-Y,-1/2+Z loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.51613(14) 0.68508(8) 0.03041(7) 0.0252(2) Uani d 1 . . O O2 0.48570(13) 0.70887(7) 0.22699(7) 0.0228(2) Uani d 1 . . O O3 0.80684(15) 0.87902(8) 0.29910(8) 0.0270(2) Uani d 1 . . O O4 0.41417(14) 0.74797(8) 0.46745(8) 0.0277(2) Uani d 1 . . N N1 0.17838(14) 0.54278(8) 0.22070(8) 0.0176(2) Uani d 1 . . C C7 0.28870(17) 0.46929(10) 0.30354(10) 0.0207(3) Uani d 1 . . H H7 0.411238 0.430906 0.286205 0.025 Uiso calc 1 . . C C6 0.22108(18) 0.45072(9) 0.41363(10) 0.0204(3) Uani d 1 . . H H6 0.297168 0.399296 0.469856 0.025 Uiso calc 1 . . C C5 0.03839(16) 0.50899(9) 0.44103(9) 0.0165(3) Uani d 1 . . C C4 -0.07103(17) 0.58473(10) 0.35318(9) 0.0194(3) Uani d 1 . . H H4 -0.193261 0.624817 0.368421 0.023 Uiso calc 1 . . C C3 0.00173(17) 0.60021(10) 0.24390(10) 0.0199(3) Uani d 1 . . H H3 -0.071887 0.650736 0.185822 0.024 Uiso calc 1 . . C C2 0.26195(17) 0.56648(10) 0.10675(9) 0.0195(3) Uani d 1 . . H H2A 0.143316 0.591106 0.044479 0.023 Uiso calc 1 . . H H2B 0.322475 0.495057 0.079110 0.023 Uiso calc 1 . . C C1 0.43789(17) 0.66260(9) 0.12460(9) 0.0183(2) Uani d 1 . . H H9 0.709(3) 0.8291(18) 0.2700(17) 0.041(5) Uiso d 1 . . H H8 0.860(3) 0.8538(18) 0.369(2) 0.049(5) Uiso d 1 . . H H10 0.400(3) 0.7365(16) 0.387(2) 0.041(5) Uiso d 1 . . H H11 0.285(3) 0.7551(15) 0.4820(18) 0.043(5) Uiso d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0241(4) 0.0337(5) 0.0190(4) -0.0043(3) 0.0071(3) 0.0034(3) O2 0.0228(4) 0.0264(4) 0.0193(4) -0.0036(3) 0.0037(3) -0.0010(3) O3 0.0265(5) 0.0282(5) 0.0259(5) -0.0060(3) 0.0033(3) 0.0055(3) O4 0.0210(5) 0.0380(5) 0.0241(5) 0.0000(3) 0.0041(3) -0.0065(4) N1 0.0185(5) 0.0185(4) 0.0162(4) -0.0025(3) 0.0045(3) 0.0000(3) C7 0.0206(5) 0.0204(5) 0.0221(5) 0.0028(4) 0.0067(4) 0.0023(4) C6 0.0215(5) 0.0198(5) 0.0209(5) 0.0032(4) 0.0059(4) 0.0039(4) C5 0.0173(5) 0.0155(5) 0.0171(5) -0.0023(4) 0.0037(4) -0.0004(4) C4 0.0180(5) 0.0212(5) 0.0193(5) 0.0016(4) 0.0045(4) 0.0013(4) C3 0.0191(5) 0.0219(5) 0.0186(5) 0.0016(4) 0.0029(4) 0.0025(4) C2 0.0214(5) 0.0230(5) 0.0151(5) -0.0017(4) 0.0058(4) -0.0003(4) C1 0.0162(5) 0.0209(5) 0.0182(5) 0.0013(4) 0.0035(4) 0.0026(4) 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 for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (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 H9 O3 H8 . . 105.7(19) ? H10 O4 H11 . . 105.3(18) ? C3 N1 C7 . . 120.97(9) ? C3 N1 C2 . . 119.62(9) ? C7 N1 C2 . . 119.27(9) ? N1 C7 C6 . . 120.47(10) ? N1 C7 H7 . . 119.8 ? C6 C7 H7 . . 119.8 ? C7 C6 C5 . . 120.17(10) ? C7 C6 H6 . . 119.9 ? C5 C6 H6 . . 119.9 ? C4 C5 C6 . . 117.68(9) ? C4 C5 C5 . 3_566 120.85(11) ? C6 C5 C5 . 3_566 121.47(12) ? C3 C4 C5 . . 120.19(10) ? C3 C4 H4 . . 119.9 ? C5 C4 H4 . . 119.9 ? N1 C3 C4 . . 120.51(10) ? N1 C3 H3 . . 119.7 ? C4 C3 H3 . . 119.7 ? N1 C2 C1 . . 111.44(8) ? N1 C2 H2A . . 109.3 ? C1 C2 H2A . . 109.3 ? N1 C2 H2B . . 109.3 ? C1 C2 H2B . . 109.3 ? H2A C2 H2B . . 108.0 ? O2 C1 O1 . . 127.60(10) ? O2 C1 C2 . . 118.49(9) ? O1 C1 C2 . . 113.91(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 C1 . 1.2553(13) ? O2 C1 . 1.2479(14) ? O3 H9 . 0.86(2) ? O3 H8 . 0.85(2) ? O4 H10 . 0.89(2) ? O4 H11 . 0.85(2) ? N1 C3 . 1.3454(14) ? N1 C7 . 1.3495(15) ? N1 C2 . 1.4753(13) ? C7 C6 . 1.3780(14) ? C7 H7 . 0.9300 ? C6 C5 . 1.3982(14) ? C6 H6 . 0.9300 ? C5 C4 . 1.3973(15) ? C5 C5 3_566 1.4856(19) ? C4 C3 . 1.3794(14) ? C4 H4 . 0.9300 ? C3 H3 . 0.9300 ? C2 C1 . 1.5429(15) ? C2 H2A . 0.9700 ? C2 H2B . 0.9700 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _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 O3 H9 O2 . . . 0.859(19) 1.96(2) 2.8135(12) 172.1(19) yes O3 H8 O1 . . 4_676 0.85(2) 1.95(2) 2.7888(11) 171(2) yes O4 H10 O2 . . . 0.89(2) 1.97(2) 2.8233(12) 158.9(18) yes O4 H11 O1 . . 4_576 0.85(2) 1.97(2) 2.8007(13) 164.1(17) 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 C3 N1 C7 C6 . . . . 0.60(17) ? C2 N1 C7 C6 . . . . 176.33(10) ? N1 C7 C6 C5 . . . . -0.68(17) ? C7 C6 C5 C4 . . . . 0.41(16) ? C7 C6 C5 C5 . . . 3_566 -179.89(11) ? C6 C5 C4 C3 . . . . -0.07(16) ? C5 C5 C4 C3 3_566 . . . -179.76(11) ? C7 N1 C3 C4 . . . . -0.25(16) ? C2 N1 C3 C4 . . . . -175.96(10) ? C5 C4 C3 N1 . . . . -0.02(17) ? C3 N1 C2 C1 . . . . 92.74(11) ? C7 N1 C2 C1 . . . . -83.05(12) ? N1 C2 C1 O2 . . . . -1.12(14) ? N1 C2 C1 O1 . . . . 179.23(9) ?