#------------------------------------------------------------------------------ #$Date: 2023-12-07 12:49:16 +0100 (Thu, 07 Dec 2023) $ #$Revision: 288134 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/29/2022916.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_2022916 loop_ _publ_author_name 'Chidambaranathan, B.' 'Sivaraj, S.' 'Vijayamathubalan, P.' 'Selvakumar, S.' _publ_section_title ; Synthesis, crystal structure and Hirshfeld surface analysis of di-acetato-bis-[4-(2-amino-eth-yl)morpholine]cadmium tetra-hydrate. ; _journal_coeditor_code JQ2030 _journal_issue 'Pt 11' _journal_name_full 'Acta crystallographica. Section E, Crystallographic communications' _journal_page_first 1049 _journal_page_last 1054 _journal_paper_doi 10.1107/S2056989023008782 _journal_volume 79 _journal_year 2023 _chemical_formula_iupac '[Cd (C2 H3 O2)2 (C6 H14 N2 O)2], 4H2 O' _chemical_formula_moiety 'C16 H34 Cd N4 O6, 4(H2 O)' _chemical_formula_sum 'C16 H42 Cd N4 O10' _chemical_formula_weight 562.93 _chemical_name_systematic ; Diacetatobis[4-(2-aminoethyl)morpholine]cadmium tetrahydrate ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2019/3 _cell_angle_alpha 66.004(2) _cell_angle_beta 73.603(2) _cell_angle_gamma 70.161(2) _cell_formula_units_Z 1 _cell_length_a 8.8639(4) _cell_length_b 9.1035(5) _cell_length_c 9.2106(5) _cell_measurement_reflns_used 8460 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 27.72 _cell_measurement_theta_min 2.46 _cell_volume 629.63(6) _computing_cell_refinement ; APEX2 and SAINT (Bruker, 2004) ; _computing_data_collection ; APEX2 (Bruker, 2004) ; _computing_data_reduction ; SAINT and XPREP (Bruker, 2004) ; _computing_molecular_graphics 'Mercury (Macrae et al., 2020)' _computing_publication_material ; SHELXL2019/2 (Sheldrick, 2015b) ; _computing_structure_refinement ; SHELXL2019/2 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2018/2 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 296(2) _diffrn_detector_area_resol_mean 8.333 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker APEXII' _diffrn_measurement_method '\w and \f scan' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_unetI/netI 0.0356 _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 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 19482 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.996 _diffrn_reflns_theta_min 2.455 _exptl_absorpt_coefficient_mu 0.920 _exptl_absorpt_correction_T_max 0.7459 _exptl_absorpt_correction_T_min 0.6029 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.485 _exptl_crystal_description BLOCK _exptl_crystal_F_000 294 _exptl_crystal_size_max 0.420 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.200 _refine_diff_density_max 0.354 _refine_diff_density_min -0.413 _refine_ls_extinction_coef 0.070(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2019/2 (Sheldrick 2015b) ; _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 209 _refine_ls_number_reflns 3034 _refine_ls_number_restraints 156 _refine_ls_restrained_S_all 1.007 _refine_ls_R_factor_all 0.0225 _refine_ls_R_factor_gt 0.0223 _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^)+(0.0252P)^2^+0.0883P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.0556 _reflns_number_gt 3024 _reflns_number_total 3034 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jq2030sup1.cif _cod_data_source_block I _cod_depositor_comments 'Adding full bibliography for 2022916.cif.' _cod_database_code 2022916 _cod_database_fobs_code 2022916 _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 0.699 _shelx_estimated_absorpt_t_max 0.837 _shelx_hkl_file ; 1 0 0 1576.04 96.79 1 0 0 1213.78 100.39 1 0 0 1506.35 102.19 -2 0 0 1906.91 151.88 -2 0 0 2139.79 143.89 -2 0 0 2072.59 155.78 -2 0 0 1956.40 177.48 -2 0 0 2325.27 148.89 -2 0 0 1959.70 148.89 2 0 0 2254.47 143.79 2 0 0 2151.38 143.69 2 0 0 2029.80 151.88 2 0 0 2114.09 160.88 2 0 0 2203.88 155.98 2 0 0 2176.08 149.19 2 0 0 2274.17 149.29 -3 0 0 321.77 23.70 -3 0 0 330.87 27.20 -3 0 0 319.47 23.50 -3 0 0 342.07 23.70 -3 0 0 352.86 29.10 -3 0 0 329.27 27.60 3 0 0 328.87 23.30 3 0 0 314.67 24.30 3 0 0 331.77 23.20 3 0 0 339.57 24.40 -4 0 0 269.87 24.00 -4 0 0 256.77 23.50 -4 0 0 278.77 23.60 -4 0 0 251.67 19.10 4 0 0 252.57 18.50 4 0 0 264.87 19.90 4 0 0 256.27 19.70 -5 0 0 745.63 63.09 -5 0 0 728.93 54.99 -5 0 0 858.21 55.09 5 0 0 825.22 54.29 5 0 0 796.82 57.29 5 0 0 746.83 60.79 5 0 0 799.22 57.19 -6 0 0 867.11 57.79 -6 0 0 815.52 57.79 -6 0 0 836.72 67.89 6 0 0 752.72 69.09 6 0 0 831.72 60.09 6 0 0 858.91 56.49 6 0 0 836.52 60.29 6 0 0 772.82 64.09 -7 0 0 349.96 27.00 -7 0 0 404.76 27.20 -7 0 0 336.27 34.90 7 0 0 369.66 28.70 7 0 0 329.67 35.30 7 0 0 410.46 32.40 -8 0 0 179.68 23.70 -8 0 0 158.68 12.70 8 0 0 165.28 17.20 8 0 0 153.28 14.10 8 0 0 167.48 22.90 -9 0 0 350.86 37.40 9 0 0 390.26 38.70 9 0 0 362.76 32.60 9 0 0 349.47 28.20 -10 0 0 8.50 8.10 10 0 0 8.40 8.70 11 0 0 166.78 27.40 11 -1 0 152.18 26.60 10 -1 0 55.39 16.00 -10 1 0 68.89 16.90 9 -1 0 63.79 15.20 9 -1 0 71.39 9.80 -9 1 0 61.29 8.10 -9 1 0 70.99 15.80 8 -1 0 270.97 24.30 8 -1 0 324.57 26.90 8 -1 0 308.47 32.50 -8 1 0 213.88 30.40 -8 1 0 312.97 23.40 7 -1 0 439.76 32.80 7 -1 0 313.77 36.30 7 -1 0 365.06 30.30 -7 1 0 356.16 35.70 -7 1 0 390.06 29.20 6 -1 0 83.29 10.00 6 -1 0 72.29 7.30 6 -1 0 74.89 9.30 6 -1 0 81.79 9.30 6 -1 0 45.90 11.10 -6 1 0 74.99 13.10 -6 1 0 73.99 6.50 -6 1 0 76.09 9.50 -6 1 0 79.39 8.60 -6 1 0 79.29 9.00 5 -1 0 585.24 45.10 5 -1 0 509.25 49.50 5 -1 0 591.44 43.40 5 -1 0 566.54 41.20 5 -1 0 531.85 43.30 -5 1 0 579.64 48.20 -5 1 0 651.43 51.99 -5 1 0 566.84 41.90 -5 1 0 592.84 41.70 4 -1 0 631.24 46.00 4 -1 0 624.04 47.20 4 -1 0 625.04 43.80 4 -1 0 681.83 46.00 4 -1 0 569.64 51.79 -4 1 0 677.13 44.30 -4 1 0 554.44 44.00 -4 1 0 636.64 49.99 -4 1 0 556.84 45.00 3 -1 0 1225.18 90.99 3 -1 0 1182.98 96.99 3 -1 0 1192.08 84.99 3 -1 0 1287.67 88.59 3 -1 0 1223.88 88.49 -3 1 0 1249.07 87.99 -3 1 0 1215.98 85.39 -3 1 0 1090.99 92.69 -3 1 0 1313.37 85.39 -3 1 0 1308.97 88.29 2 -1 0 8137.29 593.34 2 -1 0 8993.80 628.54 2 -1 0 7641.64 615.54 2 -1 0 8472.15 636.04 2 -1 0 8174.28 621.14 2 -1 0 9429.56 593.44 2 -1 0 8494.45 665.43 2 -1 0 9608.24 615.94 -2 1 0 8888.41 593.64 -2 1 0 9410.06 615.64 -2 1 0 8193.58 636.74 -2 1 0 9955.00 593.74 -2 1 0 8452.05 615.64 -2 1 0 9035.30 636.14 1 -1 0 1015.90 78.29 1 -1 0 947.11 72.29 1 -1 0 947.91 73.09 1 -1 0 1054.39 77.29 1 -1 0 972.60 69.69 1 -1 0 1041.90 74.19 1 -1 0 1080.99 69.79 1 -1 0 1165.78 72.69 -1 1 0 1049.49 77.29 -1 1 0 1019.50 74.09 -1 1 0 979.70 72.39 -1 1 0 1106.69 69.89 -1 1 0 880.71 73.09 -1 1 0 1027.60 69.89 -1 1 0 998.20 74.69 -1 1 0 977.10 72.19 -1 1 0 1001.10 78.19 0 -1 0 2375.66 183.58 0 -1 0 2627.64 202.48 0 -1 0 2655.43 194.48 0 -1 0 2864.21 183.78 0 -1 0 2632.24 205.38 0 -1 0 3072.49 190.78 0 -1 0 2942.21 190.68 0 1 0 2381.76 205.18 0 1 0 2998.20 183.88 0 1 0 2502.35 202.48 0 1 0 2662.63 190.68 0 1 0 2780.52 190.58 0 1 0 2783.62 194.58 0 1 0 2665.13 196.88 -1 -1 0 3326.27 219.08 -1 -1 0 2658.13 211.08 -1 -1 0 3362.96 211.28 -1 -1 0 3535.55 233.48 1 1 0 3287.17 233.38 1 1 0 2880.51 226.58 1 1 0 3338.47 211.18 1 1 0 3096.69 211.18 1 1 0 2664.93 226.18 1 1 0 3067.99 219.08 -2 -1 0 1034.50 71.19 -2 -1 0 1034.50 78.39 -2 -1 0 978.30 80.99 -2 -1 0 986.90 76.09 2 1 0 1086.49 73.79 2 1 0 1184.88 81.39 2 1 0 1008.60 73.79 2 1 0 1106.19 78.19 -3 -1 0 338.47 26.10 -3 -1 0 307.67 26.40 -3 -1 0 301.97 27.20 3 1 0 312.77 26.00 -4 -1 0 2130.09 164.28 -4 -1 0 2118.19 168.38 4 1 0 2262.67 158.68 4 1 0 2466.25 158.78 -5 -1 0 351.46 29.10 -5 -1 0 362.06 29.80 5 1 0 288.27 22.40 5 1 0 311.47 22.60 -6 -1 0 294.47 30.40 -6 -1 0 354.86 32.40 6 1 0 345.07 24.70 6 1 0 333.77 24.50 -7 -1 0 562.24 48.70 7 1 0 478.05 48.20 7 1 0 576.04 39.80 -8 -1 0 180.48 25.20 8 1 0 219.88 21.60 8 1 0 238.48 24.90 8 1 0 205.58 16.10 -9 -1 0 529.85 52.59 9 1 0 588.54 48.50 9 1 0 585.74 53.49 10 1 0 115.39 16.50 10 1 0 119.89 20.00 11 1 0 67.89 16.60 10 -2 0 197.88 31.50 10 -2 0 214.98 20.90 -10 2 0 197.38 29.40 9 -2 0 59.29 9.90 9 -2 0 54.39 15.20 -9 2 0 66.89 16.20 -9 2 0 52.49 8.90 8 -2 0 159.98 24.50 8 -2 0 179.68 17.40 -8 2 0 158.78 15.80 -8 2 0 153.88 22.70 7 -2 0 370.16 30.20 7 -2 0 396.76 30.20 7 -2 0 330.47 36.30 -7 2 0 326.77 34.00 -7 2 0 313.97 28.20 6 -2 0 690.23 47.20 6 -2 0 611.14 49.50 6 -2 0 592.14 56.99 6 -2 0 631.64 49.90 -6 2 0 619.24 47.90 -6 2 0 724.53 47.80 -6 2 0 619.94 47.70 -6 2 0 621.64 54.19 5 -2 0 769.02 52.69 5 -2 0 674.33 53.19 5 -2 0 728.13 50.59 5 -2 0 714.73 52.79 5 -2 0 614.64 59.39 5 -2 0 613.04 52.49 -5 2 0 682.83 51.09 -5 2 0 709.43 51.99 -5 2 0 669.43 56.69 -5 2 0 732.93 50.89 4 -2 0 1805.62 130.29 4 -2 0 1626.74 141.89 4 -2 0 1679.33 132.79 4 -2 0 1973.00 131.39 4 -2 0 1767.12 124.99 4 -2 0 1945.81 130.39 -4 2 0 1590.84 125.19 -4 2 0 1874.91 129.79 -4 2 0 1834.82 135.99 -4 2 0 1943.21 125.59 3 -2 0 3205.28 220.78 3 -2 0 2731.63 235.78 3 -2 0 2897.21 223.48 3 -2 0 2904.11 217.78 3 -2 0 3039.10 209.68 3 -2 0 3200.88 217.88 -3 2 0 3001.80 217.48 -3 2 0 2895.91 209.88 -3 2 0 2982.40 225.48 -3 2 0 3520.75 224.08 -3 2 0 3294.57 210.08 2 -2 0 729.03 67.59 2 -2 0 808.62 63.19 2 -2 0 812.12 62.59 2 -2 0 836.42 60.19 2 -2 0 992.50 63.19 2 -2 0 906.21 62.39 -2 2 0 905.71 63.39 -2 2 0 745.53 60.29 -2 2 0 933.51 60.59 -2 2 0 839.62 64.49 -2 2 0 819.02 62.09 -2 2 0 894.41 62.69 1 -2 0 900.91 66.29 1 -2 0 930.41 68.99 1 -2 0 1003.60 69.19 1 -2 0 901.41 66.19 1 -2 0 983.10 73.99 1 -2 0 1074.69 69.29 1 -2 0 974.30 70.19 1 -2 0 903.71 74.09 -1 2 0 927.41 73.99 -1 2 0 909.61 68.79 -1 2 0 993.00 70.09 -1 2 0 875.11 73.49 -1 2 0 860.61 68.99 -1 2 0 971.20 66.59 -1 2 0 1047.60 66.69 -1 2 0 917.21 68.59 0 -2 0 1005.90 67.39 0 -2 0 768.22 60.49 0 -2 0 802.32 67.29 0 -2 0 901.51 60.69 0 -2 0 881.91 63.09 0 -2 0 840.92 62.89 0 2 0 867.01 63.69 0 2 0 828.22 62.89 0 2 0 971.50 60.99 0 2 0 805.52 60.59 0 2 0 777.02 66.89 0 2 0 962.80 63.19 0 2 0 899.11 64.69 0 2 0 868.71 67.29 -1 -2 0 796.52 53.89 -1 -2 0 851.11 59.79 -1 -2 0 768.42 53.89 -1 -2 0 664.73 59.29 -1 -2 0 791.62 56.59 -1 -2 0 716.63 55.69 1 2 0 833.72 55.99 1 2 0 765.82 59.59 1 2 0 796.92 56.59 1 2 0 628.64 55.59 1 2 0 771.12 59.49 1 2 0 800.02 53.89 1 2 0 849.22 53.89 -2 -2 0 2623.14 183.28 -2 -2 0 2890.91 203.28 -2 -2 0 2479.35 189.78 -2 -2 0 2658.23 183.28 -2 -2 0 2693.63 189.88 2 2 0 2746.43 197.08 2 2 0 2704.53 183.18 2 2 0 2884.11 183.18 2 2 0 2859.11 190.28 2 2 0 2773.32 196.28 2 2 0 2404.56 202.88 2 2 0 2615.34 190.08 -3 -2 0 931.61 64.09 -3 -2 0 1036.40 65.69 -3 -2 0 939.61 69.19 -3 -2 0 904.51 65.59 -3 -2 0 884.91 73.79 3 2 0 925.71 63.79 3 2 0 972.10 63.79 3 2 0 808.72 72.59 3 2 0 925.71 70.69 3 2 0 947.71 66.39 -4 -2 0 16.40 5.20 -4 -2 0 31.40 2.80 -4 -2 0 33.00 2.90 -4 -2 0 31.90 6.00 -4 -2 0 26.40 6.20 4 2 0 30.50 3.00 4 2 0 32.50 3.10 -5 -2 0 363.86 30.50 -5 -2 0 374.36 29.30 -5 -2 0 291.87 30.30 5 2 0 338.87 25.30 5 2 0 309.27 23.30 5 2 0 321.27 28.50 -6 -2 0 607.74 50.39 -6 -2 0 592.94 51.99 -6 -2 0 573.54 48.60 -7 -2 0 367.66 34.50 -7 -2 0 378.56 35.60 -8 -2 0 380.76 37.50 9 2 0 188.88 22.90 9 2 0 198.28 25.00 10 2 0 224.48 24.20 10 2 0 233.28 29.50 11 2 0 109.49 19.90 10 -3 0 79.89 14.20 10 -3 0 98.59 21.90 -10 3 0 97.99 13.20 -10 3 0 106.29 20.70 9 -3 0 30.00 13.70 9 -3 0 48.60 9.90 -9 3 0 44.60 13.60 -9 3 0 35.60 8.40 8 -3 0 154.78 24.60 8 -3 0 140.69 17.60 -8 3 0 153.58 17.10 -8 3 0 119.79 20.30 7 -3 0 197.78 26.60 7 -3 0 144.19 19.20 -7 3 0 190.88 18.40 -7 3 0 230.98 26.10 6 -3 0 1191.08 96.89 6 -3 0 1381.76 109.49 6 -3 0 1350.36 92.89 6 -3 0 1311.17 97.79 -6 3 0 1361.06 96.09 -6 3 0 1256.67 102.39 -6 3 0 1271.37 93.79 5 -3 0 1623.94 114.89 5 -3 0 1730.23 119.39 5 -3 0 1703.93 121.39 5 -3 0 1557.24 131.49 5 -3 0 1637.84 120.09 -5 3 0 1497.15 115.29 -5 3 0 1592.54 124.99 -5 3 0 1669.73 119.19 4 -3 0 951.90 74.59 4 -3 0 918.41 71.09 4 -3 0 899.61 81.59 4 -3 0 1055.49 73.29 4 -3 0 926.21 74.39 -4 3 0 1008.90 77.49 -4 3 0 1102.79 75.09 -4 3 0 948.31 71.89 -4 3 0 1093.69 74.49 3 -3 0 246.28 26.40 3 -3 0 285.17 23.30 3 -3 0 289.67 24.80 3 -3 0 296.67 22.50 3 -3 0 269.97 23.30 -3 3 0 268.17 23.70 -3 3 0 317.07 23.40 -3 3 0 297.37 25.30 -3 3 0 294.17 24.50 2 -3 0 55.49 7.60 2 -3 0 83.69 9.20 2 -3 0 46.20 6.30 2 -3 0 51.69 8.20 2 -3 0 58.59 5.70 -2 3 0 47.00 6.80 -2 3 0 49.40 8.60 -2 3 0 51.59 5.80 -2 3 0 54.09 5.50 -2 3 0 45.30 7.50 -2 3 0 55.49 8.00 1 -3 0 1082.59 86.99 1 -3 0 1201.68 81.39 1 -3 0 1071.09 81.19 1 -3 0 1101.89 82.49 1 -3 0 1134.69 78.29 -1 3 0 1082.39 81.09 -1 3 0 1138.89 81.49 -1 3 0 1061.69 78.29 -1 3 0 1144.89 82.39 -1 3 0 1014.30 86.39 0 -3 0 788.72 55.79 0 -3 0 704.53 55.09 0 -3 0 735.73 58.89 0 -3 0 736.13 53.19 0 -3 0 730.53 53.29 0 3 0 812.62 56.49 0 3 0 709.93 58.89 0 3 0 766.32 55.09 0 3 0 733.73 58.49 0 3 0 722.93 55.39 0 3 0 677.73 55.09 0 3 0 757.32 53.59 -1 -3 0 3847.11 248.38 -1 -3 0 3442.26 257.07 -1 -3 0 3701.93 263.77 -1 -3 0 3920.81 248.18 1 3 0 3227.68 257.17 1 3 0 3370.46 273.27 1 3 0 3725.63 262.97 1 3 0 3553.04 263.97 1 3 0 3653.83 276.47 1 3 0 4028.80 257.47 1 3 0 3528.85 247.88 -2 -3 0 225.98 15.90 -2 -3 0 181.98 15.70 -2 -3 0 199.48 15.40 -2 -3 0 173.98 15.50 2 3 0 183.08 16.10 2 3 0 189.28 15.30 2 3 0 201.78 16.10 2 3 0 212.08 16.50 2 3 0 168.28 17.30 2 3 0 192.78 15.40 -3 -3 0 1218.28 79.89 -3 -3 0 1082.79 82.09 -3 -3 0 1141.09 79.79 3 3 0 1297.97 82.89 3 3 0 1157.98 82.79 3 3 0 1064.99 84.99 3 3 0 1115.19 79.39 3 3 0 1133.79 89.39 -4 -3 0 443.26 41.90 -4 -3 0 500.05 35.10 -4 -3 0 457.45 38.60 -4 -3 0 457.65 34.90 -4 -3 0 555.94 35.30 4 3 0 491.95 36.40 4 3 0 488.15 36.20 4 3 0 489.55 34.50 4 3 0 447.76 41.00 4 3 0 518.85 38.90 -5 -3 0 406.36 42.00 -5 -3 0 469.35 33.90 -5 -3 0 486.65 34.00 -5 -3 0 512.05 39.80 5 3 0 528.55 35.50 5 3 0 431.36 41.30 5 3 0 494.35 35.50 5 3 0 505.75 39.80 -6 -3 0 941.91 85.19 -6 -3 0 963.40 79.79 6 3 0 1106.09 74.09 6 3 0 1068.79 73.89 -7 -3 0 614.64 54.49 -7 -3 0 725.93 59.69 -8 -3 0 249.18 25.10 -8 -3 0 189.08 26.80 9 3 0 80.19 14.40 10 3 0 137.69 20.50 10 3 0 128.59 20.40 11 3 0 49.99 12.50 11 3 0 32.50 10.40 11 3 0 32.60 10.30 9 -4 0 99.79 22.50 9 -4 0 75.49 14.20 -9 4 0 111.69 20.20 -9 4 0 90.39 14.20 8 -4 0 154.28 26.70 8 -4 0 153.58 20.30 -8 4 0 152.38 19.00 -8 4 0 205.28 26.00 7 -4 0 123.99 21.70 7 -4 0 108.79 16.20 -7 4 0 115.59 15.80 -7 4 0 117.19 18.60 6 -4 0 267.47 25.70 6 -4 0 225.48 30.60 6 -4 0 272.27 22.80 -6 4 0 265.07 24.60 -6 4 0 246.68 26.70 5 -4 0 226.68 20.00 5 -4 0 244.88 26.20 5 -4 0 238.38 21.00 5 -4 0 218.98 22.40 -5 4 0 207.98 22.70 -5 4 0 224.78 21.40 -5 4 0 217.98 21.50 4 -4 0 742.93 64.49 4 -4 0 769.72 70.19 4 -4 0 848.12 61.89 4 -4 0 939.61 62.09 4 -4 0 808.62 63.39 -4 4 0 878.61 64.29 -4 4 0 794.42 62.29 -4 4 0 811.12 65.89 3 -4 0 382.26 28.50 3 -4 0 296.77 29.40 3 -4 0 341.37 28.50 3 -4 0 383.66 27.30 3 -4 0 327.97 32.20 -3 4 0 313.77 29.10 -3 4 0 359.96 29.80 -3 4 0 318.97 28.60 -3 4 0 339.47 26.70 2 -4 0 373.76 30.30 2 -4 0 455.45 30.00 2 -4 0 328.87 33.10 2 -4 0 370.66 31.70 2 -4 0 344.77 30.30 -2 4 0 335.97 30.90 -2 4 0 371.46 30.60 -2 4 0 373.66 29.10 -2 4 0 402.36 30.90 -2 4 0 373.66 34.20 1 -4 0 890.81 70.39 1 -4 0 1019.60 75.09 1 -4 0 922.51 67.49 -1 4 0 982.90 70.99 -1 4 0 990.90 69.49 -1 4 0 782.52 66.99 -1 4 0 896.61 74.69 0 -4 0 282.07 26.90 0 -4 0 339.17 25.80 0 -4 0 307.67 26.20 0 -4 0 377.36 25.80 0 4 0 321.07 25.70 0 4 0 265.47 25.70 0 4 0 290.37 25.20 0 4 0 301.77 28.00 -1 -4 0 326.07 22.80 -1 -4 0 279.47 24.10 -1 -4 0 261.27 23.50 -1 -4 0 289.27 24.50 1 4 0 261.87 24.40 1 4 0 269.87 25.90 1 4 0 291.37 23.50 1 4 0 328.67 25.10 1 4 0 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7.20 4 8 11 29.10 12.00 4 8 11 47.70 10.60 4 8 11 29.30 11.60 4 8 11 24.50 10.00 -5 -8 -11 37.80 11.90 -5 -8 -11 37.60 12.10 5 8 11 13.50 9.20 5 8 11 11.60 8.90 5 8 11 23.60 8.70 5 8 11 28.80 11.30 -6 -8 -11 34.90 11.50 6 8 11 24.50 12.40 6 8 11 44.50 13.30 6 8 11 39.10 11.50 -7 -8 -11 44.80 12.20 7 8 11 47.50 13.00 7 8 11 49.10 14.40 7 8 11 43.20 13.60 -8 -8 -11 52.79 12.60 8 8 11 24.20 10.80 8 8 11 43.80 13.90 8 8 11 55.69 15.50 -1 -9 -11 26.30 11.90 -1 -9 -11 30.20 13.20 -1 -9 -11 32.80 13.00 1 9 11 34.90 13.60 1 9 11 26.00 12.70 1 9 11 21.40 9.60 -2 -9 -11 81.79 18.30 -2 -9 -11 132.89 22.00 2 9 11 74.19 18.90 2 9 11 121.59 21.50 2 9 11 153.28 23.50 -3 -9 -11 66.19 16.30 -3 -9 -11 32.60 12.70 3 9 11 36.80 13.60 3 9 11 52.59 15.50 3 9 11 44.20 13.90 -4 -9 -11 62.49 16.10 -4 -9 -11 48.30 13.40 4 9 11 77.79 16.80 4 9 11 56.79 16.20 4 9 11 69.69 16.30 -5 -9 -11 46.10 12.70 -5 -9 -11 58.99 15.10 5 9 11 60.99 12.90 5 9 11 55.49 14.20 5 9 11 40.20 14.50 5 9 11 70.19 15.10 -6 -9 -11 29.30 11.80 6 9 11 37.30 12.90 6 9 11 57.39 15.90 6 9 11 64.09 14.20 -7 -9 -11 49.60 13.30 7 9 11 56.19 15.80 7 9 11 51.49 14.10 7 9 11 36.20 11.80 -3 -10 -11 116.79 21.40 -3 -10 -11 120.79 21.00 3 10 11 95.69 19.40 3 10 11 66.99 18.20 3 10 11 86.69 19.30 -4 -10 -11 53.19 14.60 -4 -10 -11 69.69 17.30 4 10 11 31.60 13.00 4 10 11 51.59 16.90 4 10 11 60.19 14.90 -5 -10 -11 58.69 16.10 5 10 11 72.29 18.60 5 10 11 57.69 15.50 -6 -10 -11 52.39 15.20 6 10 11 133.09 20.10 6 10 11 69.89 17.80 6 10 11 84.39 18.00 -2 -1 -12 27.30 11.80 -2 -1 -12 25.30 11.20 -2 -1 -12 30.20 12.40 -2 -1 -12 47.60 19.80 2 1 12 45.50 14.70 2 1 12 63.69 17.30 2 1 12 18.10 10.00 -3 -1 -12 40.20 18.60 -3 -1 -12 41.00 12.80 -3 -1 -12 39.40 13.10 -3 -1 -12 21.60 11.30 3 1 12 49.30 15.80 3 1 12 31.60 13.00 3 1 12 27.70 12.70 0 -2 -12 31.30 13.40 0 -2 -12 46.00 14.70 0 -2 -12 46.60 14.00 0 -2 -12 25.00 16.30 0 2 12 64.89 16.10 0 2 12 72.49 14.90 -1 -2 -12 45.20 14.40 -1 -2 -12 10.50 9.70 -1 -2 -12 39.00 13.20 -1 -2 -12 28.50 15.30 1 2 12 29.10 12.00 1 2 12 46.30 14.30 1 2 12 36.70 11.40 -2 -2 -12 49.20 13.90 -2 -2 -12 42.10 14.00 -2 -2 -12 37.30 12.90 -2 -2 -12 54.19 19.30 2 2 12 56.69 13.80 2 2 12 71.79 16.20 2 2 12 37.70 14.80 -3 -2 -12 35.30 12.70 -3 -2 -12 48.80 13.00 -3 -2 -12 78.79 21.80 -3 -2 -12 68.89 17.10 3 2 12 75.89 17.70 3 2 12 47.50 14.90 3 2 12 69.69 16.10 -4 -2 -12 47.00 12.80 -4 -2 -12 81.39 17.50 -4 -2 -12 33.20 16.70 -4 -2 -12 43.30 14.10 4 2 12 46.30 16.30 4 2 12 67.09 16.60 4 2 12 75.49 16.70 -5 -2 -12 36.40 13.70 -5 -2 -12 56.49 14.10 -5 -2 -12 21.90 14.30 -5 -2 -12 52.29 14.10 5 2 12 34.00 19.60 5 2 12 62.09 16.90 5 2 12 59.09 15.30 0 -3 -12 6.00 12.60 0 -3 -12 0.90 8.00 0 -3 -12 20.60 10.90 0 -3 -12 23.50 10.20 0 3 12 18.60 9.30 0 3 12 31.00 12.50 0 3 12 22.80 10.70 -1 -3 -12 37.60 12.80 -1 -3 -12 59.09 20.80 -1 -3 -12 40.20 14.00 -1 -3 -12 56.79 15.50 1 3 12 44.80 12.80 1 3 12 57.69 15.20 1 3 12 61.39 15.80 -2 -3 -12 63.39 15.90 -2 -3 -12 69.99 16.60 -2 -3 -12 60.09 20.60 -2 -3 -12 92.49 17.10 2 3 12 51.89 14.80 2 3 12 87.99 17.50 2 3 12 52.79 14.30 -3 -3 -12 37.90 16.90 -3 -3 -12 50.39 14.10 -3 -3 -12 25.20 11.10 -3 -3 -12 42.60 12.90 3 3 12 66.29 15.20 3 3 12 39.10 13.00 3 3 12 47.20 15.00 -4 -3 -12 28.00 11.80 -4 -3 -12 25.30 10.00 -4 -3 -12 5.20 11.60 -4 -3 -12 20.00 9.60 4 3 12 28.70 12.50 4 3 12 16.00 10.90 4 3 12 34.30 11.80 -5 -3 -12 34.90 16.70 -5 -3 -12 38.30 13.10 -5 -3 -12 66.59 15.60 -5 -3 -12 50.79 12.60 5 3 12 42.50 13.10 5 3 12 41.40 14.40 5 3 12 29.10 13.40 -6 -3 -12 30.60 12.30 -6 -3 -12 4.50 9.20 6 3 12 17.90 10.10 6 3 12 11.00 10.60 0 -4 -12 42.30 12.60 0 -4 -12 48.40 19.10 0 -4 -12 56.19 14.90 0 -4 -12 51.79 14.30 0 4 12 35.40 12.50 0 4 12 59.79 14.20 -1 -4 -12 80.49 18.70 -1 -4 -12 21.40 11.00 -1 -4 -12 14.60 15.70 -1 -4 -12 63.59 15.90 1 4 12 48.40 14.30 1 4 12 32.50 11.80 1 4 12 73.09 15.90 -2 -4 -12 40.60 17.80 -2 -4 -12 38.30 12.60 -2 -4 -12 13.70 10.10 -2 -4 -12 34.10 11.80 2 4 12 31.20 11.70 2 4 12 24.70 11.50 2 4 12 45.40 13.40 -3 -4 -12 32.70 12.20 -3 -4 -12 27.00 11.70 -3 -4 -12 46.20 18.70 -3 -4 -12 62.89 15.30 3 4 12 45.60 13.30 3 4 12 50.59 14.40 3 4 12 43.50 14.00 -4 -4 -12 22.50 10.70 -4 -4 -12 25.90 11.00 -4 -4 -12 37.70 11.00 -4 -4 -12 50.39 17.00 4 4 12 40.90 13.70 4 4 12 27.50 12.40 4 4 12 15.50 9.50 -5 -4 -12 63.99 14.90 -5 -4 -12 41.00 12.60 -5 -4 -12 76.49 15.80 -5 -4 -12 32.90 14.20 5 4 12 61.99 15.40 5 4 12 33.10 13.40 5 4 12 58.39 14.80 -6 -4 -12 42.80 15.90 -6 -4 -12 44.40 13.40 6 4 12 59.99 15.80 6 4 12 49.90 15.40 0 -5 -12 6.90 8.70 0 -5 -12 18.60 10.80 0 -5 -12 31.80 12.10 0 -5 -12 1.40 12.00 0 5 12 16.40 8.50 0 5 12 8.70 9.00 -1 -5 -12 70.49 15.60 -1 -5 -12 44.90 14.50 -1 -5 -12 73.39 16.40 -1 -5 -12 46.40 20.20 1 5 12 53.69 15.10 1 5 12 46.70 13.10 -2 -5 -12 63.99 15.10 -2 -5 -12 70.79 15.60 -2 -5 -12 48.60 14.00 -2 -5 -12 76.79 23.00 2 5 12 41.50 12.20 2 5 12 64.89 16.00 2 5 12 75.49 16.20 -3 -5 -12 98.29 18.80 -3 -5 -12 81.49 17.60 -3 -5 -12 100.29 25.30 -3 -5 -12 89.99 18.20 3 5 12 116.09 20.10 3 5 12 125.69 21.00 3 5 12 119.49 19.90 -4 -5 -12 67.79 16.80 -4 -5 -12 115.29 19.60 -4 -5 -12 89.89 22.90 -4 -5 -12 92.19 17.60 4 5 12 96.89 18.90 4 5 12 104.29 19.60 4 5 12 107.29 18.60 -5 -5 -12 47.30 13.50 -5 -5 -12 62.49 14.90 -5 -5 -12 58.29 17.40 -5 -5 -12 12.30 9.70 5 5 12 19.80 10.90 5 5 12 41.00 13.40 5 5 12 22.50 11.10 -6 -5 -12 70.69 15.00 -6 -5 -12 53.79 16.00 6 5 12 54.59 14.40 6 5 12 55.69 14.90 -7 -5 -12 23.20 10.30 -7 -5 -12 43.70 14.00 7 5 12 30.60 11.60 7 5 12 40.20 13.60 0 -6 -12 49.30 14.70 0 -6 -12 12.30 8.70 0 -6 -12 12.10 15.10 0 -6 -12 3.40 8.10 0 6 12 38.40 14.30 0 6 12 12.30 8.90 -1 -6 -12 33.20 11.90 -1 -6 -12 35.20 19.10 -1 -6 -12 69.19 15.80 -1 -6 -12 52.19 15.20 1 6 12 72.79 15.30 1 6 12 40.10 14.20 -2 -6 -12 121.09 19.50 -2 -6 -12 117.79 19.30 -2 -6 -12 37.70 18.50 -2 -6 -12 87.89 18.10 2 6 12 76.89 17.30 2 6 12 104.19 18.70 -3 -6 -12 151.68 21.90 -3 -6 -12 82.99 24.60 -3 -6 -12 146.79 22.70 -3 -6 -12 94.59 18.40 3 6 12 121.29 20.10 3 6 12 137.29 21.80 3 6 12 135.89 21.80 -4 -6 -12 146.99 22.00 -4 -6 -12 83.79 17.90 -4 -6 -12 99.09 24.70 -4 -6 -12 106.99 18.70 4 6 12 117.99 19.90 4 6 12 93.19 17.80 4 6 12 104.89 20.10 4 6 12 107.29 19.40 -5 -6 -12 77.09 15.30 -5 -6 -12 72.69 14.70 -5 -6 -12 76.09 16.10 -5 -6 -12 74.39 20.30 5 6 12 40.50 13.20 5 6 12 53.79 14.50 5 6 12 30.10 12.30 5 6 12 72.79 15.90 -6 -6 -12 20.10 11.80 -6 -6 -12 23.40 12.00 6 6 12 46.70 13.90 6 6 12 36.40 12.60 6 6 12 20.30 11.00 -7 -6 -12 36.80 11.50 -7 -6 -12 47.00 15.60 7 6 12 51.59 14.30 7 6 12 44.50 13.30 7 6 12 67.19 16.10 -1 -7 -12 49.50 14.00 -1 -7 -12 46.00 13.00 -1 -7 -12 50.99 13.80 1 7 12 68.69 16.90 1 7 12 48.20 13.70 -2 -7 -12 24.40 9.00 -2 -7 -12 13.30 10.70 -2 -7 -12 34.00 12.20 2 7 12 14.50 10.00 2 7 12 12.40 9.90 -3 -7 -12 28.10 9.30 -3 -7 -12 32.00 12.10 -3 -7 -12 22.20 11.00 3 7 12 14.30 9.60 3 7 12 32.50 13.10 3 7 12 37.50 13.10 -4 -7 -12 42.90 12.20 -4 -7 -12 52.89 14.20 -4 -7 -12 58.69 12.70 4 7 12 44.70 12.50 4 7 12 57.89 14.90 4 7 12 31.30 13.10 4 7 12 63.79 16.50 -5 -7 -12 74.19 14.30 -5 -7 -12 61.09 15.00 -5 -7 -12 48.10 13.30 5 7 12 53.19 14.30 5 7 12 49.00 15.00 5 7 12 66.59 16.00 5 7 12 42.00 13.10 -6 -7 -12 16.10 10.50 6 7 12 23.40 10.70 6 7 12 30.80 12.80 6 7 12 30.00 11.00 -7 -7 -12 15.10 8.40 7 7 12 13.50 9.90 7 7 12 13.00 10.60 7 7 12 17.10 10.90 -2 -8 -12 33.60 13.50 -2 -8 -12 43.80 13.70 -2 -8 -12 55.49 12.80 2 8 12 63.39 15.80 2 8 12 62.49 16.40 2 8 12 31.90 13.70 -3 -8 -12 19.80 10.60 -3 -8 -12 -1.80 8.70 -3 -8 -12 23.80 8.10 3 8 12 20.80 12.60 3 8 12 2.70 7.70 3 8 12 21.40 12.00 -4 -8 -12 34.10 13.30 -4 -8 -12 42.60 13.30 4 8 12 45.40 13.40 4 8 12 30.70 13.80 4 8 12 29.60 11.20 -5 -8 -12 29.80 11.30 -5 -8 -12 43.40 12.70 5 8 12 28.10 11.10 5 8 12 22.80 11.50 5 8 12 48.20 12.70 5 8 12 33.60 12.30 -6 -8 -12 50.19 14.80 6 8 12 23.60 10.80 6 8 12 49.80 13.00 6 8 12 35.40 14.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 66066 _shelx_res_file ; TITL shelxt_a.res in P-1 I.res created by SHELXL-2019/3 at 01:24:12 on 26-Sep-2023 CELL 0.71073 8.8639 9.1035 9.2106 66.004 73.603 70.161 ZERR 1.00 0.0004 0.0005 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H N O CD UNIT 16 42 4 10 1 LIST 4 MERG 2 OMIT -3.00 56.00 OMIT 1 0 0 SADI 0.02 N2 H1 N2 H2 DFIX 0.84 0.02 O4 H3 O4 H4 o4 h4' O5 H5 O5 H6 O5 H6' o5B h5 o5B h6 o5B h6' SADI 0.02 H3 H4 H3 H4' H5 H6 H5 H6' SADI 0.02 C7 C8 C7B C8B SADI 0.02 C7 O1 C7B O1B SADI 0.02 C7 O2 C7B O2B SADI 0.02 O1 O2 O1B O2B SADI 0.02 O2 C8 O2B C8B SADI 0.02 O1 C8 O1B C8B SIMU 0.02 0.04 C7 > O2B FLAT o1 o2 c7 c8 FLAT o1b o2b c7b c8b RIGU C7 > O2B EQIV $1 -x+1, -y, -z+1 HTAB C4 O2B_$1 HTAB C5 O1B HTAB N2 O4_$1 HTAB N2 O1 HTAB N2 O1B HTAB O4 O2 HTAB O4 O2B EQIV $2 -x+1, -y, -z HTAB O4 O4_$2 HTAB O5 O1 HTAB O5B O1B EQIV $3 -x+2, -y+1, -z HTAB O5 O5_$3 EQIV $4 -x+1, -y+1, -z HTAB O5 O4_$4 HTAB O5B O4_$4 FMAP 2 PLAN 20 SIZE 0.200 0.250 0.420 ACTA BOND BOND $H CONF L.S. 50 TEMP 23.00 BIND 3 4 BIND 3 1 BIND 2 4 WGHT 0.025200 0.088300 EXTI 0.069977 FVAR 1.11580 0.74856 CD1 5 0.500000 0.000000 0.500000 10.50000 0.02855 0.02433 = 0.03058 -0.00839 -0.00444 -0.00663 C1 1 0.159745 0.317330 0.399249 11.00000 0.03559 0.03303 = 0.04869 -0.00998 -0.01586 0.00147 AFIX 23 H1A 2 0.234102 0.335992 0.297375 11.00000 -1.20000 H1B 2 0.092779 0.424930 0.404315 11.00000 -1.20000 AFIX 0 C2 1 0.052677 0.217121 0.405128 11.00000 0.03685 0.05213 = 0.07147 -0.02052 -0.02572 -0.00203 AFIX 23 H2A 2 -0.011008 0.279160 0.318855 11.00000 -1.20000 H2B 2 0.120004 0.114484 0.388209 11.00000 -1.20000 AFIX 0 C3 1 0.040481 0.087710 0.680693 11.00000 0.03346 0.04983 = 0.06647 -0.01668 0.00223 -0.01428 AFIX 23 H3A 2 0.110930 -0.013930 0.663716 11.00000 -1.20000 H3B 2 -0.031524 0.057256 0.783056 11.00000 -1.20000 AFIX 0 C4 1 0.142810 0.187704 0.686915 11.00000 0.03365 0.03713 = 0.04562 -0.01589 0.00114 -0.00561 AFIX 23 H4A 2 0.072480 0.287436 0.707912 11.00000 -1.20000 H4B 2 0.204906 0.122555 0.774156 11.00000 -1.20000 AFIX 0 C5 1 0.335701 0.353559 0.530380 11.00000 0.03913 0.02414 = 0.04873 -0.01231 -0.00697 -0.00702 AFIX 23 H5A 2 0.254126 0.441193 0.564346 11.00000 -1.20000 H5B 2 0.386251 0.404292 0.420633 11.00000 -1.20000 AFIX 0 C6 1 0.462867 0.274134 0.637551 11.00000 0.03831 0.03578 = 0.04523 -0.02028 -0.00642 -0.01196 AFIX 23 H6A 2 0.504495 0.359169 0.639032 11.00000 -1.20000 H6B 2 0.414465 0.218855 0.746809 11.00000 -1.20000 AFIX 0 N1 3 0.254769 0.234130 0.533076 11.00000 0.02665 0.02598 = 0.03752 -0.00942 -0.00572 -0.00522 N2 3 0.596860 0.152872 0.579077 11.00000 0.02859 0.04096 = 0.04705 -0.01785 -0.00730 -0.01053 H1 2 0.657411 0.101064 0.649048 11.00000 -1.20000 H2 2 0.654321 0.202470 0.495017 11.00000 -1.20000 PART 1 10.5 C7 1 0.634356 0.266417 0.151684 10.50000 0.04877 0.03438 = 0.03825 -0.00227 -0.00612 -0.00588 C8 1 0.666987 0.321098 -0.030128 10.50000 0.08375 0.06905 = 0.03314 0.00516 0.00449 -0.02195 AFIX 137 H8A 2 0.565533 0.368190 -0.069697 10.50000 -1.50000 H8B 2 0.727822 0.226857 -0.062787 10.50000 -1.50000 H8C 2 0.728342 0.402997 -0.073442 10.50000 -1.50000 AFIX 0 O1 4 0.695640 0.317922 0.222753 10.50000 0.05047 0.04333 = 0.04548 -0.00544 -0.00139 -0.01731 O2 4 0.538780 0.170775 0.222823 10.50000 0.04418 0.04510 = 0.03183 0.00235 -0.00726 -0.01411 PART 2 10.5 C7B 1 0.641610 0.268158 0.163533 10.50000 0.04247 0.04204 = 0.02759 -0.00174 0.00873 -0.00533 C8B 1 0.706840 0.297279 -0.014835 10.50000 0.10637 0.07944 = 0.04141 -0.01865 0.01971 -0.04015 AFIX 137 H8B1 2 0.647320 0.403671 -0.077770 10.50000 -1.50000 H8B2 2 0.694369 0.211533 -0.042399 10.50000 -1.50000 H8B3 2 0.819967 0.295000 -0.036825 10.50000 -1.50000 AFIX 0 O1B 4 0.666420 0.351042 0.228393 10.50000 0.06251 0.04124 = 0.04919 -0.01411 0.01291 -0.01773 O2B 4 0.565911 0.154221 0.233079 10.50000 0.04110 0.03977 = 0.02981 -0.00205 -0.00986 -0.00578 PART 0 O3 4 -0.053465 0.179295 0.554926 11.00000 0.02777 0.06369 = 0.09335 -0.02493 -0.01513 -0.00774 O4 4 0.363871 0.101916 0.078094 11.00000 0.08287 0.05613 = 0.05290 -0.01678 -0.02366 -0.00546 H3 2 0.423847 0.132894 0.109059 11.00000 -1.50000 part 3 H4 2 0.301508 0.190028 0.034353 10.50000 -1.50000 part 4 H4' 2 0.430540 0.029536 0.043549 10.50000 -1.50000 part 0 part 3 21.0 eadp o5 o5B O5 4 0.847420 0.583301 0.076054 21.00000 0.05596 0.05283 = 0.06477 -0.02083 -0.00289 -0.01721 part 0 H5 2 0.795700 0.510191 0.114593 11.00000 -1.50000 PART 3 H6 2 0.938848 0.529299 0.048530 10.50000 -1.50000 PART 4 H6' 2 0.777936 0.665352 0.032147 10.50000 -1.50000 part 4 -21.0 O5B 4 0.841934 0.572105 0.034125 -21.00000 0.05596 0.05283 = 0.06477 -0.02083 -0.00289 -0.01721 HKLF 4 REM shelxt_a.res in P-1 REM wR2 = 0.0556, GooF = S = 1.028, Restrained GooF = 1.007 for all data REM R1 = 0.0223 for 3024 Fo > 4sig(Fo) and 0.0225 for all 3034 data REM 209 parameters refined using 156 restraints END WGHT 0.0235 0.0647 REM Highest difference peak 0.354, deepest hole -0.413, 1-sigma level 0.055 Q1 1 0.4943 0.0895 0.4154 11.00000 0.05 0.35 Q2 1 0.5415 0.0993 0.3563 11.00000 0.05 0.30 Q3 1 0.3746 0.1203 0.5126 11.00000 0.05 0.29 Q4 1 0.2978 0.1341 0.5355 11.00000 0.05 0.28 Q5 1 0.2703 -0.0198 0.5485 11.00000 0.05 0.25 Q6 1 0.4775 0.0560 0.5521 11.00000 0.05 0.25 Q7 1 0.3998 0.2986 0.5893 11.00000 0.05 0.23 Q8 1 0.4531 -0.0025 0.3759 11.00000 0.05 0.22 Q9 1 0.6324 0.3312 0.0567 11.00000 0.05 0.22 Q10 1 0.2099 0.2715 0.4721 11.00000 0.05 0.21 Q11 1 0.0994 0.1344 0.6750 11.00000 0.05 0.19 Q12 1 0.2008 0.2141 0.6102 11.00000 0.05 0.19 Q13 1 0.3056 0.2840 0.5287 11.00000 0.05 0.19 Q14 1 0.7518 0.2234 0.2711 11.00000 0.05 0.19 Q15 1 0.4632 0.3063 0.6991 11.00000 0.05 0.19 Q16 1 0.4534 0.2141 0.1578 11.00000 0.05 0.18 Q17 1 -0.0675 0.1375 0.6541 11.00000 0.05 0.18 Q18 1 0.8553 0.2177 -0.0237 11.00000 0.05 0.18 Q19 1 0.8288 0.3430 -0.0395 11.00000 0.05 0.18 Q20 1 0.0336 0.1508 0.4794 11.00000 0.05 0.16 ; _shelx_res_checksum 38445 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 Cd Cd1 0.500000 0.000000 0.500000 0.02834(8) Uani d 1 . . C C1 0.1597(2) 0.3173(2) 0.3992(2) 0.0414(4) Uani d 1 . . H H1A 0.234102 0.335992 0.297375 0.050 Uiso calc 1 . . H H1B 0.092779 0.424930 0.404315 0.050 Uiso calc 1 . . C C2 0.0527(3) 0.2171(3) 0.4051(3) 0.0526(5) Uani d 1 . . H H2A -0.011008 0.279160 0.318855 0.063 Uiso calc 1 . . H H2B 0.120004 0.114484 0.388209 0.063 Uiso calc 1 . . C C3 0.0405(3) 0.0877(3) 0.6807(3) 0.0525(5) Uani d 1 . . H H3A 0.110930 -0.013930 0.663716 0.063 Uiso calc 1 . . H H3B -0.031524 0.057256 0.783056 0.063 Uiso calc 1 . . C C4 0.1428(2) 0.1877(2) 0.6869(2) 0.0410(4) Uani d 1 . . H H4A 0.072480 0.287436 0.707912 0.049 Uiso calc 1 . . H H4B 0.204906 0.122555 0.774156 0.049 Uiso calc 1 . . C C5 0.3357(2) 0.3536(2) 0.5304(2) 0.0378(4) Uani d 1 . . H H5A 0.254126 0.441193 0.564346 0.045 Uiso calc 1 . . H H5B 0.386251 0.404292 0.420633 0.045 Uiso calc 1 . . C C6 0.4629(2) 0.2741(2) 0.6376(2) 0.0371(4) Uani d 1 . . H H6A 0.504495 0.359169 0.639032 0.044 Uiso calc 1 . . H H6B 0.414465 0.218855 0.746809 0.044 Uiso calc 1 . . N N1 0.25477(17) 0.23413(17) 0.53308(17) 0.0309(3) Uani d 1 . . N N2 0.59686(19) 0.1529(2) 0.5791(2) 0.0373(3) Uani d 1 . . H H1 0.657(3) 0.101(3) 0.649(3) 0.045 Uiso d 1 . . H H2 0.654(3) 0.202(3) 0.495(2) 0.045 Uiso d 1 . . C C7 0.6344(19) 0.2664(19) 0.1517(17) 0.046(2) Uani d 0.5 A 1 C C8 0.667(2) 0.321(2) -0.0301(15) 0.072(3) Uani d 0.5 A 1 H H8A 0.565533 0.368190 -0.069697 0.108 Uiso calc 0.5 A 1 H H8B 0.727822 0.226857 -0.062787 0.108 Uiso calc 0.5 A 1 H H8C 0.728342 0.402997 -0.073442 0.108 Uiso calc 0.5 A 1 O O1 0.6956(18) 0.3179(17) 0.2228(18) 0.0498(19) Uani d 0.5 A 1 O O2 0.539(2) 0.171(2) 0.223(2) 0.045(3) Uani d 0.5 A 1 C C7B 0.6416(18) 0.2682(19) 0.1635(16) 0.046(2) Uani d 0.5 A 2 C C8B 0.707(2) 0.297(2) -0.0148(15) 0.079(4) Uani d 0.5 A 2 H H8B1 0.647320 0.403671 -0.077770 0.119 Uiso calc 0.5 A 2 H H8B2 0.694369 0.211533 -0.042399 0.119 Uiso calc 0.5 A 2 H H8B3 0.819967 0.295000 -0.036825 0.119 Uiso calc 0.5 A 2 O O1B 0.6664(19) 0.3510(17) 0.228(2) 0.055(3) Uani d 0.5 A 2 O O2B 0.566(2) 0.154(2) 0.233(2) 0.0407(19) Uani d 0.5 A 2 O O3 -0.05347(18) 0.1793(2) 0.5549(2) 0.0623(4) Uani d 1 . . O O4 0.3639(3) 0.1019(2) 0.0781(2) 0.0653(5) Uani d 1 . . H H3 0.424(4) 0.133(4) 0.109(4) 0.098 Uiso d 1 . . H H4 0.302(6) 0.190(4) 0.034(8) 0.098 Uiso d 0.5 B 3 H H4' 0.431(5) 0.030(7) 0.044(8) 0.098 Uiso d 0.5 C 4 O O5 0.8474(6) 0.5833(6) 0.0761(12) 0.0584(13) Uani d 0.75(3) D 3 H H5 0.796(3) 0.510(3) 0.115(3) 0.088 Uiso d 1 . . H H6 0.939(2) 0.529(6) 0.049(6) 0.088 Uiso d 0.5 E 3 H H6' 0.778(5) 0.665(3) 0.032(6) 0.088 Uiso d 0.5 F 4 O O5B 0.842(2) 0.572(2) 0.034(2) 0.0584(13) Uani d 0.25(3) D 4 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 Cd1 0.02855(11) 0.02433(10) 0.03058(10) -0.00663(6) -0.00444(6) -0.00839(6) C1 0.0356(9) 0.0330(9) 0.0487(10) 0.0015(7) -0.0159(8) -0.0100(8) C2 0.0369(11) 0.0521(12) 0.0715(14) -0.0020(9) -0.0257(10) -0.0205(11) C3 0.0335(10) 0.0498(12) 0.0665(14) -0.0143(9) 0.0022(9) -0.0167(10) C4 0.0337(9) 0.0371(9) 0.0456(10) -0.0056(7) 0.0011(7) -0.0159(8) C5 0.0391(10) 0.0241(8) 0.0487(10) -0.0070(7) -0.0070(8) -0.0123(7) C6 0.0383(9) 0.0358(9) 0.0452(9) -0.0120(7) -0.0064(7) -0.0203(8) N1 0.0266(7) 0.0260(6) 0.0375(7) -0.0052(5) -0.0057(5) -0.0094(5) N2 0.0286(8) 0.0410(8) 0.0470(9) -0.0105(6) -0.0073(6) -0.0179(7) C7 0.049(5) 0.034(4) 0.038(4) -0.006(3) -0.006(3) -0.002(3) C8 0.084(7) 0.069(5) 0.033(3) -0.022(5) 0.004(3) 0.005(3) O1 0.050(4) 0.043(5) 0.045(3) -0.017(4) -0.001(3) -0.005(3) O2 0.044(5) 0.045(4) 0.032(3) -0.014(4) -0.007(3) 0.002(2) C7B 0.042(4) 0.042(4) 0.028(3) -0.005(3) 0.009(3) -0.002(3) C8B 0.106(10) 0.079(8) 0.041(4) -0.040(8) 0.020(5) -0.019(5) O1B 0.063(6) 0.041(5) 0.049(3) -0.018(4) 0.013(3) -0.014(3) O2B 0.041(4) 0.040(3) 0.030(3) -0.006(3) -0.010(3) -0.002(2) O3 0.0278(7) 0.0637(10) 0.0934(13) -0.0077(7) -0.0151(8) -0.0249(9) O4 0.0829(13) 0.0561(10) 0.0529(9) -0.0055(9) -0.0237(9) -0.0168(8) O5 0.0560(11) 0.0528(12) 0.065(3) -0.0172(9) -0.0029(15) -0.0208(15) O5B 0.0560(11) 0.0528(12) 0.065(3) -0.0172(9) -0.0029(15) -0.0208(15) 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' Cd Cd -0.8075 1.2024 '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 N2 Cd1 N2 . 2_656 180.0 ? N2 Cd1 O2B . 2_656 88.9(4) ? N2 Cd1 O2B 2_656 2_656 91.1(4) ? N2 Cd1 O2B . . 91.1(4) ? N2 Cd1 O2B 2_656 . 88.9(4) ? O2B Cd1 O2B 2_656 . 180.0 ? N2 Cd1 O2 . 2_656 86.6(4) ? N2 Cd1 O2 2_656 2_656 93.4(4) ? O2B Cd1 O2 2_656 2_656 5.9(8) ? O2B Cd1 O2 . 2_656 174.1(8) ? N2 Cd1 O2 . . 93.4(4) ? N2 Cd1 O2 2_656 . 86.6(4) ? O2 Cd1 O2 2_656 . 180.0 ? N2 Cd1 N1 . . 76.46(5) ? N2 Cd1 N1 2_656 . 103.54(5) ? O2B Cd1 N1 2_656 . 89.6(5) ? O2B Cd1 N1 . . 90.4(5) ? O2 Cd1 N1 2_656 . 94.4(5) ? O2 Cd1 N1 . . 85.6(5) ? N2 Cd1 N1 . 2_656 103.54(5) ? N2 Cd1 N1 2_656 2_656 76.46(5) ? O2 Cd1 N1 2_656 2_656 85.6(5) ? O2 Cd1 N1 . 2_656 94.4(5) ? N1 Cd1 N1 . 2_656 180.0 ? N1 C1 C2 . . 112.45(16) ? N1 C1 H1A . . 109.1 ? C2 C1 H1A . . 109.1 ? N1 C1 H1B . . 109.1 ? C2 C1 H1B . . 109.1 ? H1A C1 H1B . . 107.8 ? O3 C2 C1 . . 111.52(19) ? O3 C2 H2A . . 109.3 ? C1 C2 H2A . . 109.3 ? O3 C2 H2B . . 109.3 ? C1 C2 H2B . . 109.3 ? H2A C2 H2B . . 108.0 ? O3 C3 C4 . . 111.37(18) ? O3 C3 H3A . . 109.4 ? C4 C3 H3A . . 109.4 ? O3 C3 H3B . . 109.4 ? C4 C3 H3B . . 109.4 ? H3A C3 H3B . . 108.0 ? N1 C4 C3 . . 110.44(16) ? N1 C4 H4A . . 109.6 ? C3 C4 H4A . . 109.6 ? N1 C4 H4B . . 109.6 ? C3 C4 H4B . . 109.6 ? H4A C4 H4B . . 108.1 ? N1 C5 C6 . . 113.08(14) ? N1 C5 H5A . . 109.0 ? C6 C5 H5A . . 109.0 ? N1 C5 H5B . . 109.0 ? C6 C5 H5B . . 109.0 ? H5A C5 H5B . . 107.8 ? N2 C6 C5 . . 110.33(14) ? N2 C6 H6A . . 109.6 ? C5 C6 H6A . . 109.6 ? N2 C6 H6B . . 109.6 ? C5 C6 H6B . . 109.6 ? H6A C6 H6B . . 108.1 ? C4 N1 C5 . . 110.11(14) ? C4 N1 C1 . . 108.91(14) ? C5 N1 C1 . . 107.85(14) ? C4 N1 Cd1 . . 113.82(10) ? C5 N1 Cd1 . . 100.13(10) ? C1 N1 Cd1 . . 115.51(11) ? C6 N2 Cd1 . . 110.81(11) ? C6 N2 H1 . . 107.4(16) ? Cd1 N2 H1 . . 117.5(16) ? C6 N2 H2 . . 110.1(16) ? Cd1 N2 H2 . . 104.7(15) ? H1 N2 H2 . . 106(2) ? O1 C7 O2 . . 124.2(10) ? O1 C7 C8 . . 120.4(9) ? O2 C7 C8 . . 115.3(9) ? C7 C8 H8A . . 109.5 ? C7 C8 H8B . . 109.5 ? H8A C8 H8B . . 109.5 ? C7 C8 H8C . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? C7 O2 Cd1 . . 128.0(11) ? O1B C7B O2B . . 126.0(10) ? O1B C7B C8B . . 119.6(9) ? O2B C7B C8B . . 114.4(9) ? C7B C8B H8B1 . . 109.5 ? C7B C8B H8B2 . . 109.5 ? H8B1 C8B H8B2 . . 109.5 ? C7B C8B H8B3 . . 109.5 ? H8B1 C8B H8B3 . . 109.5 ? H8B2 C8B H8B3 . . 109.5 ? C7B O2B Cd1 . . 132.3(10) ? C2 O3 C3 . . 109.06(16) ? H3 O4 H4 . . 103(3) ? H3 O4 H4' . . 102(3) ? H4 O4 H4' . . 132(7) ? H5 O5 H6 . . 101(3) ? H5 O5 H6' . . 101(3) ? H6 O5 H6' . . 137(5) ? H5 O5B H6 . . 101(3) ? H5 O5B H6' . . 100(3) ? H6 O5B H6' . . 132(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 Cd1 N2 . 2.2788(15) ? Cd1 N2 2_656 2.2788(15) ? Cd1 O2B 2_656 2.301(16) ? Cd1 O2B . 2.301(16) ? Cd1 O2 2_656 2.386(16) ? Cd1 O2 . 2.386(16) ? Cd1 N1 . 2.5239(13) ? Cd1 N1 2_656 2.5239(13) ? C1 N1 . 1.482(2) ? C1 C2 . 1.501(3) ? C1 H1A . 0.9700 ? C1 H1B . 0.9700 ? C2 O3 . 1.417(3) ? C2 H2A . 0.9700 ? C2 H2B . 0.9700 ? C3 O3 . 1.421(3) ? C3 C4 . 1.512(3) ? C3 H3A . 0.9700 ? C3 H3B . 0.9700 ? C4 N1 . 1.475(2) ? C4 H4A . 0.9700 ? C4 H4B . 0.9700 ? C5 N1 . 1.481(2) ? C5 C6 . 1.504(3) ? C5 H5A . 0.9700 ? C5 H5B . 0.9700 ? C6 N2 . 1.467(2) ? C6 H6A . 0.9700 ? C6 H6B . 0.9700 ? N2 H1 . 0.838(18) ? N2 H2 . 0.844(18) ? C7 O1 . 1.252(9) ? C7 O2 . 1.276(9) ? C7 C8 . 1.511(10) ? C8 H8A . 0.9600 ? C8 H8B . 0.9600 ? C8 H8C . 0.9600 ? C7B O1B . 1.236(10) ? C7B O2B . 1.275(9) ? C7B C8B . 1.522(9) ? C8B H8B1 . 0.9600 ? C8B H8B2 . 0.9600 ? C8B H8B3 . 0.9600 ? O4 H3 . 0.834(17) ? O4 H4 . 0.820(19) ? O4 H4' . 0.827(19) ? O5 H5 . 0.838(16) ? O5 H6 . 0.823(18) ? O5 H6' . 0.827(19) ? O5B H5 . 0.825(17) ? O5B H6 . 0.838(19) ? O5B H6' . 0.842(19) ? 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 C4 H4B O2B 2_656 0.97 2.66 3.264(19) 120.9 yes C5 H5B O1B . 0.97 2.63 3.425(16) 139.0 yes N2 H1 O4 2_656 0.838(18) 2.44(2) 3.096(3) 136(2) yes N2 H2 O1 . 0.844(18) 2.26(2) 3.009(16) 147(2) yes N2 H2 O1B . 0.844(18) 2.26(3) 2.993(17) 145(2) yes O4 H3 O2 . 0.834(17) 1.84(3) 2.661(17) 167(4) yes O4 H3 O2B . 0.834(17) 2.02(3) 2.837(17) 165(3) yes O4 H4 O5 2_665 0.82(5) 2.06(5) 2.879(7) 178(7) yes O4 H4 O5B 2_665 0.82(5) 2.05(5) 2.847(18) 165(5) yes O4 H4' O4 2_655 0.827(19) 2.11(3) 2.917(4) 164(6) yes O5 H5 O1 . 0.838(16) 1.99(2) 2.828(16) 173(3) yes O5B H5 O1B . 0.825(17) 1.93(2) 2.70(2) 155(3) yes O5 H6 O5 2_765 0.823(18) 2.09(3) 2.895(13) 166(5) yes O5 H6 O5B 2_765 0.82(4) 1.93(5) 2.75(2) 173(5) yes O5 H6' O4 2_665 0.827(19) 2.065(17) 2.878(5) 168(5) yes O5B H6' O4 2_665 0.842(19) 2.065(17) 2.846(17) 154(5) 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 N1 C1 C2 O3 . . . . 56.0(2) ? O3 C3 C4 N1 . . . . -59.6(2) ? N1 C5 C6 N2 . . . . 64.5(2) ? C3 C4 N1 C5 . . . . 171.13(15) ? C3 C4 N1 C1 . . . . 53.06(19) ? C3 C4 N1 Cd1 . . . . -77.39(17) ? C6 C5 N1 C4 . . . . 73.18(18) ? C6 C5 N1 C1 . . . . -168.10(15) ? C6 C5 N1 Cd1 . . . . -46.96(16) ? C2 C1 N1 C4 . . . . -52.0(2) ? C2 C1 N1 C5 . . . . -171.48(16) ? C2 C1 N1 Cd1 . . . . 77.53(18) ? C5 C6 N2 Cd1 . . . . -41.77(17) ? O1 C7 O2 Cd1 . . . . -18(2) ? C8 C7 O2 Cd1 . . . . 163.7(13) ? O1B C7B O2B Cd1 . . . . -18(2) ? C8B C7B O2B Cd1 . . . . 160.8(14) ? C1 C2 O3 C3 . . . . -59.3(2) ? C4 C3 O3 C2 . . . . 61.5(2) ?