#------------------------------------------------------------------------------ #$Date: 2024-09-25 04:05:43 +0200 (Wed, 25 Sep 2024) $ #$Revision: 294881 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/32/2023255.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_2023255 loop_ _publ_author_name 'Vinodh, Mickey' 'Al-Azemi, Talal F.' _publ_section_title ; Crystal structure and supramolecular features of a host--guest inclusion complex based on A1/A2-hetero-difunctionalized pillar[5]arene ; _journal_coeditor_code JQ2036 _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989024009216 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac 'C47 H53.18 Br0.82 O10, C6 H8 N2' _chemical_formula_moiety 'C47 H53.18 Br0.82 O10, C6 H8 N2' _chemical_formula_sum 'C53 H61.18 Br0.82 N2 O10' _chemical_formula_weight 951.38 _chemical_name_systematic ; A1/A2-Bromobutoxy--hydroxy difunctionalized pillar[5]arene-- hexanedinitrile (1/1) ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2019/3 _cell_angle_alpha 90 _cell_angle_beta 92.659(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.9686(12) _cell_length_b 21.180(2) _cell_length_c 20.107(2) _cell_measurement_reflns_used 22410 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 24.95 _cell_measurement_theta_min 3.04 _cell_volume 5091.5(9) _computing_cell_refinement ; CrystalClear 2.1 (Rigaku, 2016) ; _computing_data_collection ; CrystalClear 2.1 (Rigaku, 2016) ; _computing_data_reduction ; CrystalClear 2.1 (Rigaku, 2016) ; _computing_molecular_graphics ; Mercury (Macrae et al., 2020) ; _computing_structure_refinement ; SHELXL2019/2 (Sheldrick, 2015) ; _computing_structure_solution ; CrystalStructure 4.2 (Rigaku, 2017) ; _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 10.000 _diffrn_measured_fraction_theta_full 0.997 _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 0.0525 _diffrn_reflns_av_unetI/netI 0.0479 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 46597 _diffrn_reflns_theta_full 24.969 _diffrn_reflns_theta_max 24.969 _diffrn_reflns_theta_min 3.059 _exptl_absorpt_coefficient_mu 0.720 _exptl_absorpt_correction_T_max 0.853 _exptl_absorpt_correction_T_min 0.403 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (ABSCOR; Higashi, 1995) ; _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.241 _exptl_crystal_description Block _exptl_crystal_F_000 2007 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.180 _refine_diff_density_max 0.393 _refine_diff_density_min -0.233 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 797 _refine_ls_number_reflns 8895 _refine_ls_number_restraints 1090 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0951 _refine_ls_R_factor_gt 0.0541 _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^)+(0.0926P)^2^+0.6834P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1479 _refine_ls_wR_factor_ref 0.1702 _reflns_number_gt 5350 _reflns_number_total 8895 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jq2036.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2023255 _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 0.869 _shelx_estimated_absorpt_t_max 0.881 _shelx_hkl_file ; 0 0 3 5.97 2.03 0 0 -3 4.37 2.12 0 0 4 8247.27 290.64 0 0 -4 8377.92 292.80 0 0 5 9.35 3.76 0 0 -5 9.72 5.93 0 0 6 6318.05 206.29 0 0 -6 6554.02 211.14 0 0 7 14.39 5.22 0 0 -7 5.92 5.22 0 0 8 9.44 9.45 0 0 -8 -5.51 9.86 0 0 9 3.58 6.51 0 0 -9 2.04 6.78 0 0 10 1255.37 30.24 0 0 -10 1343.73 31.67 0 0 11 18.08 13.53 0 0 -11 5.62 13.94 0 0 12 406.08 16.17 0 0 -12 441.39 16.93 0 0 13 1.50 10.34 0 0 -13 -3.13 10.17 0 0 14 80.64 11.87 0 0 -14 78.02 18.99 0 0 15 7.65 11.12 0 0 -15 7.68 11.87 0 0 16 67.44 13.99 0 0 -16 83.81 13.83 0 0 17 14.41 13.38 0 0 -17 -11.17 13.94 0 0 18 57.85 15.02 0 0 -18 35.29 15.52 0 0 19 -7.06 14.53 0 0 -19 -6.93 15.21 0 0 20 21.25 15.68 0 0 -20 27.13 16.84 0 0 21 5.89 15.20 0 0 -21 -7.46 16.61 0 0 22 -25.01 25.79 0 0 -22 4.48 29.57 0 0 23 -2.29 16.59 0 0 -23 -9.69 18.98 0 1 -3 3100.88 62.54 0 1 3 3244.67 61.60 0 -1 3 3277.77 66.08 0 -1 -3 3283.34 61.89 0 1 -4 214.10 5.26 0 1 4 220.08 4.42 0 -1 4 217.69 5.34 0 -1 -4 221.32 4.41 0 1 -5 8904.56 348.34 0 1 5 8427.69 325.27 0 -1 5 8679.48 343.74 0 -1 -5 8723.97 321.70 0 1 -6 6048.03 198.69 0 1 6 5708.84 174.07 0 -1 6 5828.21 182.94 0 -1 -6 5986.90 179.78 0 1 -7 566.46 13.61 0 1 7 577.79 12.21 0 -1 7 558.73 13.42 0 -1 -7 581.46 12.08 0 1 -8 218.43 9.24 0 1 8 217.69 8.13 0 -1 8 213.78 9.28 0 -1 -8 228.65 8.14 0 1 -9 149.31 9.44 0 1 9 122.54 12.03 0 -1 9 142.49 13.81 0 -1 -9 147.16 8.29 0 1 -10 1358.58 32.61 0 1 10 1250.61 29.36 0 -1 10 1268.67 31.56 0 -1 -10 1302.74 30.41 0 1 -11 33.94 9.38 0 1 11 30.06 8.20 0 -1 11 23.94 14.58 0 -1 -11 19.14 8.73 0 1 -12 12.51 10.53 0 1 12 11.63 8.69 0 -1 12 8.97 9.68 0 -1 -12 18.98 9.23 0 1 -13 618.12 22.23 0 1 13 626.71 28.24 0 -1 13 617.67 21.95 0 -1 -13 662.27 30.01 0 1 -14 50.84 12.45 0 1 14 62.50 11.31 0 -1 14 55.41 12.16 0 -1 -14 32.39 11.26 0 1 -15 7.62 20.88 0 1 15 26.59 11.47 0 -1 15 12.84 12.59 0 -1 -15 26.74 11.77 0 1 -16 3.98 13.58 0 1 16 -5.12 11.64 0 -1 16 4.14 21.13 0 -1 -16 11.40 12.32 0 1 -17 -2.11 14.79 0 1 17 53.34 21.02 0 -1 17 -9.51 14.42 0 -1 -17 36.32 13.71 0 1 -18 155.37 28.41 0 1 18 144.64 15.67 0 -1 18 125.45 17.38 0 -1 -18 115.62 25.90 0 1 -19 15.62 15.86 0 1 19 6.26 13.83 0 -1 19 -14.10 15.35 0 -1 -19 11.20 13.66 0 1 -20 28.30 17.88 0 1 20 47.06 23.80 0 -1 20 17.05 16.15 0 -1 -20 49.00 15.85 0 1 21 7.08 15.06 0 1 -21 4.44 28.64 0 -1 21 3.26 15.88 0 -1 -21 -10.66 16.07 0 1 -22 9.38 19.95 0 1 22 19.96 15.90 0 -1 22 35.22 17.27 0 -1 -22 17.38 17.44 0 1 -23 -15.28 20.02 0 1 23 33.86 25.40 0 -1 23 1.15 17.22 0 -1 -23 31.24 29.10 0 2 -312203.52 570.02 0 2 312484.13 557.88 0 -2 312705.27 609.73 0 -2 -312593.82 563.36 0 2 -413474.29 699.00 0 2 413258.14 649.06 0 -2 413674.99 699.89 0 -2 -413949.02 686.09 0 2 -529432.09 2730.89 0 2 528453.90 2617.46 0 -2 529259.28 2729.29 0 -2 -530116.22 2760.46 0 2 -6 48.81 5.93 0 2 6 47.27 4.28 0 -2 6 53.77 5.99 0 -2 -6 48.50 4.18 0 2 -7 1466.62 30.66 0 2 7 1368.07 25.70 0 -2 7 1388.58 29.86 0 -2 -7 1464.11 26.66 0 2 -8 1202.75 27.30 0 2 8 1191.78 28.76 0 -2 8 1203.17 27.38 0 -2 -8 1265.25 24.51 0 2 -9 5751.98 193.67 0 2 9 5344.00 173.21 0 -2 9 5522.91 188.30 0 2 -10 602.52 18.57 0 2 10 555.56 15.03 0 -2 10 583.50 18.40 0 -2 -10 597.25 15.54 0 2 -11 13.84 10.10 0 2 11 -2.80 12.00 0 -2 11 14.53 15.81 0 -2 -11 -1.83 7.72 0 2 -12 1228.59 35.17 0 2 12 1171.89 38.78 0 -2 12 1190.84 34.55 0 -2 -12 1216.41 31.33 0 2 -13 51.49 11.75 0 2 13 33.85 9.56 0 -2 13 28.52 12.20 0 -2 -13 39.79 9.78 0 2 -14 139.07 14.43 0 2 14 117.46 11.97 0 -2 14 131.47 14.12 0 -2 -14 130.82 12.57 0 2 -15 56.57 14.27 0 2 15 42.98 11.28 0 -2 15 37.64 14.37 0 -2 -15 52.65 11.50 0 2 -16 149.46 16.98 0 2 16 120.31 13.57 0 -2 16 138.98 16.78 0 -2 -16 138.72 14.49 0 2 -17 570.39 39.93 0 2 17 524.04 33.16 0 -2 17 525.10 27.02 0 -2 -17 552.77 34.47 0 2 -18 21.34 16.18 0 2 18 6.55 13.17 0 -2 18 65.37 25.73 0 -2 -18 25.64 13.98 0 2 -19 0.18 19.85 0 2 19 6.96 13.59 0 -2 19 11.77 16.08 0 -2 -19 20.62 22.56 0 2 -20 -37.69 28.31 0 2 20 17.61 22.24 0 -2 20 -0.38 16.74 0 -2 -20 9.79 14.92 0 2 -21 -12.33 18.53 0 2 21 -0.84 14.67 0 -2 21 -13.96 16.81 0 -2 -21 30.67 15.30 0 2 -22 5.10 19.94 0 2 22 9.33 14.85 0 -2 22 19.02 17.74 0 -2 -22 -5.82 16.25 0 2 -23 18.89 33.54 0 2 23 -4.78 24.75 0 -2 23 3.82 28.95 0 -2 -23 10.31 17.84 0 3 1 3124.15 57.57 0 3 -1 3044.84 58.92 0 3 1 3027.62 58.55 0 3 -1 2998.59 57.30 0 -3 -1 2891.96 56.57 0 -3 1 3040.86 59.50 0 -3 -1 3272.77 63.88 0 -3 1 3131.48 60.65 0 3 2 161.46 3.01 0 3 -2 151.56 3.87 0 3 -2 156.66 4.32 0 -3 -2 155.64 3.05 0 -3 2 164.66 4.28 0 -3 -2 158.58 4.46 0 -3 2 158.19 5.97 0 3 -3 7801.39 268.62 0 -3 -3 7493.74 249.89 0 -3 3 7920.65 277.30 0 -3 -3 7947.65 253.83 0 3 -4 8027.41 293.55 0 3 4 7925.06 271.10 0 -3 4 8122.76 311.76 0 -3 -4 8318.24 279.78 0 3 -518343.21 1205.93 0 3 517514.21 1088.39 0 -3 518438.14 1226.74 0 -3 -517747.17 1110.13 0 3 -6 1625.97 34.29 0 3 6 1627.89 28.81 0 -3 6 1591.60 34.44 0 -3 -6 1673.12 32.94 0 3 -7 1820.12 40.15 0 3 7 1745.79 33.53 0 -3 7 1769.51 40.45 0 -3 -7 1844.71 34.77 0 3 -8 607.36 16.58 0 3 8 580.00 12.65 0 -3 8 586.15 16.85 0 -3 -8 600.41 12.90 0 3 -9 7454.12 298.24 0 3 9 7140.30 284.60 0 -3 9 7132.74 311.18 0 -3 -9 7632.26 281.43 0 3 -10 393.22 16.25 0 3 10 385.09 11.79 0 -3 10 378.96 16.25 0 -3 -10 365.96 11.88 0 3 -11 235.16 14.22 0 3 11 219.51 10.40 0 -3 11 217.53 21.37 0 -3 -11 221.76 10.58 0 3 -12 251.16 15.71 0 3 12 240.42 11.63 0 -3 12 259.80 15.21 0 -3 -12 262.29 11.97 0 3 -13 11.88 12.24 0 3 13 20.09 9.07 0 -3 13 12.97 18.90 0 -3 -13 7.98 9.20 0 3 -14 15.14 21.33 0 3 14 -4.61 9.62 0 -3 14 5.72 12.51 0 -3 -14 15.35 15.53 0 3 -15 1439.04 47.40 0 3 15 1290.54 38.07 0 -3 15 1269.35 59.67 0 -3 -15 1357.04 39.20 0 3 -16 478.14 25.18 0 3 16 451.89 28.55 0 -3 16 459.96 24.69 0 -3 -16 482.94 29.40 0 3 -17 71.85 16.91 0 3 17 44.33 12.27 0 -3 17 24.30 17.12 0 -3 -17 46.85 12.82 0 3 -18 104.36 18.77 0 3 18 73.68 13.99 0 -3 18 65.67 18.86 0 -3 -18 88.37 22.66 0 3 -19 345.26 38.70 0 3 19 289.18 19.03 0 -3 19 295.23 24.01 0 -3 -19 301.35 19.61 0 3 -20 130.43 22.63 0 3 20 144.25 24.85 0 -3 20 127.27 20.02 0 -3 -20 149.39 25.58 0 3 -21 19.93 19.81 0 3 21 7.50 13.68 0 -3 21 -7.94 18.35 0 -3 -21 19.75 14.70 0 3 -22 72.21 35.57 0 3 22 67.78 15.79 0 -3 22 70.63 31.22 0 -3 -22 46.63 26.51 0 3 -23 52.33 22.18 0 3 23 21.57 15.27 0 -3 23 17.28 18.36 0 -3 -23 19.97 16.78 0 4 0 2063.80 35.16 0 4 0 2002.05 34.92 0 -4 0 2114.07 36.29 0 -4 0 2149.11 37.74 0 4 1 240.27 4.44 0 4 -1 234.09 4.96 0 4 1 238.77 5.37 0 4 -1 225.61 4.99 0 -4 -1 238.58 4.51 0 -4 1 231.41 5.26 0 -4 -1 246.25 5.53 0 -4 1 237.83 5.43 0 4 2 541.84 7.71 0 4 -2 507.25 8.67 0 4 2 525.56 9.21 0 -4 2 539.58 12.06 0 -4 -2 529.75 8.01 0 -4 -2 545.61 10.02 0 -4 2 518.53 9.52 0 4 315335.92 803.97 0 4 -315651.74 853.53 0 4 -314467.84 787.66 0 -4 -313702.89 745.55 0 -4 -315948.12 872.30 0 -4 314406.23 793.95 0 4 -4 487.99 10.74 0 -4 -4 501.33 8.01 0 -4 4 501.18 15.20 0 -4 -4 496.56 7.43 0 4 -5 190.02 7.81 0 -4 -5 163.32 6.84 0 -4 5 183.20 8.02 0 -4 -5 175.52 6.54 0 4 -6 1398.37 30.54 0 4 6 1469.39 28.56 0 -4 6 1469.84 39.19 0 -4 -6 1448.82 24.76 0 4 -7 230.73 10.49 0 4 7 236.48 6.66 0 -4 7 233.39 10.50 0 -4 -7 235.93 6.64 0 4 -8 3264.14 90.08 0 4 8 3186.60 76.55 0 -4 8 3141.57 88.68 0 -4 -8 3358.37 86.84 0 4 -910154.69 487.62 0 4 9 9812.21 456.79 0 -4 9 9550.10 467.03 0 -4 -910110.26 448.30 0 4 -10 1392.13 38.21 0 4 10 1323.02 29.44 0 -4 10 1345.87 37.89 0 -4 -10 1351.15 29.39 0 4 -11 3760.54 121.17 0 4 11 3660.61 104.35 0 -4 11 3679.68 120.24 0 -4 -11 3750.86 105.12 0 4 -12 303.36 17.70 0 4 12 291.18 11.95 0 -4 12 301.45 16.76 0 -4 -12 319.02 17.88 0 4 -13 397.08 20.31 0 4 13 370.05 20.62 0 -4 13 379.27 19.55 0 -4 -13 377.40 14.32 0 4 -14 170.32 17.03 0 4 14 124.29 17.06 0 -4 14 121.16 16.10 0 -4 -14 144.17 11.63 0 4 -15 82.02 16.56 0 4 15 63.02 11.28 0 -4 15 63.29 15.38 0 -4 -15 79.36 17.52 0 4 -16 833.46 34.37 0 4 16 744.70 25.45 0 -4 16 715.27 32.14 0 -4 -16 779.39 25.51 0 4 -17 64.16 29.50 0 4 17 77.53 12.92 0 -4 17 80.82 18.24 0 -4 -17 88.09 20.11 0 4 -18 691.26 34.78 0 4 18 644.96 25.27 0 -4 18 615.18 33.55 0 -4 -18 657.24 25.87 0 4 -19 -39.43 19.35 0 4 19 -12.16 12.40 0 -4 19 11.66 18.04 0 -4 -19 6.01 13.62 0 4 -20 7.17 20.10 0 4 20 8.93 20.57 0 -4 20 37.06 18.47 0 -4 -20 15.30 13.35 0 4 -21 19.91 33.46 0 4 21 0.35 12.95 0 -4 21 23.07 30.56 0 -4 -21 4.47 14.08 0 4 -22 5.93 21.48 0 4 22 -0.93 13.44 0 -4 22 -7.93 18.96 0 -4 -22 7.63 14.90 0 4 -23 -8.23 23.01 0 4 23 14.14 13.71 0 -4 23 -18.36 30.25 0 -4 -23 -26.32 17.58 0 5 0 5.22 3.25 0 5 0 1.25 3.55 0 -5 0 -0.35 3.32 0 -5 0 4.81 3.92 0 5 1 333.08 6.31 0 5 -1 341.22 7.22 0 5 1 363.79 7.68 0 5 -1 324.77 7.14 0 -5 -1 334.05 6.40 0 -5 1 322.50 7.38 0 -5 -1 338.29 7.94 0 -5 1 328.09 7.60 0 5 2 803.25 12.40 0 5 -2 777.94 16.99 0 5 2 813.09 14.72 0 5 -2 803.68 14.72 0 -5 -2 802.63 12.60 0 -5 2 808.02 14.90 0 -5 2 775.02 14.46 0 5 3 2.74 2.96 0 5 -3 10.55 4.46 0 5 -3 6.72 5.04 0 -5 -3 7.02 2.92 0 -5 3 4.05 4.88 0 -5 -3 5.68 5.41 0 -5 3 4.25 5.02 0 5 -4 2177.87 45.95 0 5 -4 1988.99 40.82 0 -5 -4 2088.43 38.21 0 -5 -4 2226.23 53.95 0 -5 4 1986.82 43.10 0 5 -5 4415.86 126.58 0 5 -5 4399.18 124.74 0 -5 -5 4828.46 124.95 0 -5 -5 4799.22 120.16 0 -5 5 4534.44 134.46 0 5 -6 956.38 22.20 0 -5 -6 983.10 17.17 0 -5 6 964.02 22.84 0 -5 -6 954.72 16.08 0 5 -7 0.49 7.92 0 -5 -7 7.19 4.51 0 -5 7 -1.79 8.12 0 -5 -7 8.29 4.32 0 5 -8 1994.00 52.05 0 5 8 2095.10 43.02 0 -5 8 1989.33 52.99 0 -5 -8 2064.03 41.86 0 5 -9 1549.82 53.02 0 5 9 1501.60 31.10 0 -5 9 1453.43 41.39 0 -5 -9 1521.13 31.27 0 5 -10 61.10 11.56 0 5 10 62.48 6.96 0 -5 10 71.38 11.78 0 -5 -10 72.45 10.81 0 5 -11 141.56 14.30 0 5 11 132.96 8.67 0 -5 11 147.32 13.68 0 -5 -11 120.58 12.64 0 5 -12 295.87 17.87 0 5 12 282.26 16.97 0 -5 12 269.81 17.34 0 -5 -12 285.95 16.82 0 5 -13 39.10 22.69 0 5 13 37.57 8.59 0 -5 13 33.35 14.08 0 -5 -13 23.71 8.33 0 5 -14 1437.05 64.49 0 5 14 1301.74 35.15 0 -5 14 1293.09 46.43 0 -5 -14 1360.63 36.28 0 5 -15 437.96 24.61 0 5 15 380.53 16.03 0 -5 15 368.61 23.72 0 -5 -15 410.24 17.11 0 5 -16 152.00 20.82 0 5 16 153.00 12.89 0 -5 16 140.66 19.45 0 -5 -16 148.16 20.07 0 5 -17 85.31 19.89 0 5 17 59.61 12.34 0 -5 17 39.98 18.77 0 -5 -17 75.55 12.18 0 5 -18 58.71 19.81 0 5 18 30.72 11.97 0 -5 18 28.82 18.74 0 -5 -18 45.01 12.85 0 5 -19 55.45 21.74 0 5 19 63.80 12.51 0 -5 19 50.97 19.66 0 -5 -19 64.66 14.17 0 5 -20 46.12 21.01 0 5 20 11.74 19.33 0 -5 20 -0.13 30.24 0 -5 -20 10.61 12.94 0 5 -21 7.63 21.66 0 5 21 2.23 12.80 0 -5 21 2.44 19.83 0 -5 -21 -2.56 13.47 0 5 -22 3.31 22.74 0 5 22 16.17 13.37 0 -5 22 17.84 32.51 0 -5 -22 16.85 15.59 0 5 -23 4.56 23.97 0 5 23 9.97 12.97 0 -5 23 10.17 19.72 0 -5 -23 -15.01 25.94 0 6 0 7024.17 233.76 0 6 0 6671.31 223.82 0 -6 0 6831.33 229.69 0 -6 0 7316.00 259.23 0 6 1 305.97 6.83 0 6 -1 294.84 7.45 0 6 1 304.03 7.84 0 6 -1 291.62 7.67 0 -6 -1 287.94 6.86 0 -6 1 302.37 11.01 0 -6 -1 304.99 8.74 0 -6 1 305.93 8.56 0 6 2 2285.57 44.33 0 6 -2 2372.80 49.57 0 6 2 2291.03 54.18 0 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13 4 0 22.70 18.22 -13 4 0 -1.22 6.50 13 -4 0 36.51 25.03 13 -4 0 27.79 20.38 13 4 1 29.91 18.12 13 4 1 -8.03 16.92 -13 4 -1 6.49 7.47 13 -4 1 35.98 23.92 13 -4 1 -8.59 31.96 13 4 2 15.15 16.53 13 4 2 -28.58 15.83 -13 4 -2 10.73 8.06 13 -4 2 -9.00 23.64 13 -4 2 -15.40 18.98 13 4 3 5.18 15.42 13 4 3 9.86 15.13 -13 4 -3 -8.78 8.82 13 -4 3 -11.92 22.82 13 -4 3 -5.24 19.96 13 4 4 -0.20 13.24 13 4 4 -4.10 23.78 -13 4 -4 2.41 9.52 13 -4 4 1.44 21.98 13 -4 4 -14.39 18.40 13 4 5 128.24 15.37 13 4 5 140.23 16.88 -13 4 -5 131.29 13.20 13 -4 5 141.27 25.46 13 -4 5 125.78 21.54 13 4 6 1.65 17.55 13 4 6 -1.24 12.91 -13 4 -6 2.77 11.63 13 -4 6 15.62 21.27 13 -4 6 -16.86 28.25 13 4 7 24.56 12.49 13 4 7 -11.12 11.78 -13 4 -7 18.84 13.20 13 -4 7 13.08 21.41 13 -4 7 9.87 17.84 13 5 -9 -29.74 27.51 13 5 -9 -18.49 19.05 13 -5 -9 -34.54 30.12 13 -5 -9 20.03 24.93 13 5 -8 -6.32 25.91 13 5 -8 -10.55 29.70 13 -5 -8 -12.40 32.70 13 -5 -8 -25.78 30.16 13 5 -7 7.20 25.36 13 5 -7 6.44 24.15 13 -5 -7 18.27 31.74 13 5 -6 -0.64 23.69 13 5 -6 -26.65 22.82 13 -5 -6 -10.32 27.40 13 5 -5 28.07 34.12 13 5 -5 8.09 35.50 13 -5 -5 -26.73 28.50 13 5 -4 7.89 21.24 13 5 -4 -3.19 21.31 13 -5 -4 -3.37 24.71 13 5 -3 -3.73 20.87 13 5 -3 -8.07 19.16 13 -5 -3 -8.76 26.45 13 -5 -3 17.70 22.61 13 5 -2 18.50 19.17 13 5 -2 -20.13 19.28 13 -5 -2 -32.10 43.80 13 -5 -2 29.14 22.13 13 5 -1 46.66 20.08 13 5 -1 32.09 32.51 13 -5 -1 78.84 28.18 13 -5 -1 57.00 22.65 13 5 0 24.36 18.41 13 5 0 20.61 18.06 -13 5 0 12.16 12.24 13 -5 0 20.71 26.81 13 -5 0 10.09 21.34 13 5 1 73.69 19.25 13 5 1 80.30 18.32 -13 5 -1 60.54 9.49 13 -5 1 74.15 27.26 13 -5 1 38.04 22.60 13 5 2 12.35 24.98 13 5 2 22.57 15.53 -13 5 -2 -10.43 14.86 13 -5 2 17.57 24.75 13 -5 2 30.27 32.74 13 5 3 34.54 13.65 13 5 3 3.05 14.68 -13 5 -3 8.57 9.93 13 -5 3 5.24 23.12 13 -5 3 15.98 19.09 13 5 4 -15.29 12.46 13 5 4 34.79 22.75 -13 5 -4 8.22 10.72 13 -5 4 -30.30 36.21 13 -5 4 23.14 19.12 13 5 5 35.77 12.17 13 5 5 19.19 21.62 -13 5 -5 18.91 12.38 13 -5 5 54.04 22.72 13 -5 5 45.64 19.18 13 5 6 18.10 12.30 13 5 6 -3.81 12.04 -13 5 -6 -7.10 12.79 13 -5 6 31.42 21.59 13 -5 6 13.14 18.94 13 5 7 2.72 10.46 13 5 7 7.49 10.57 -13 5 -7 3.97 13.85 13 -5 7 11.70 20.72 13 -5 7 -12.66 18.07 13 6 -8 36.86 25.46 13 6 -8 -36.39 17.91 13 -6 -8 5.84 31.70 13 -6 -8 9.94 10.37 13 6 -7 2.99 24.23 13 6 -7 2.75 24.41 13 -6 -7 -8.83 28.02 13 -6 -7 -2.61 10.39 13 6 -6 11.88 22.81 13 6 -6 87.44 38.14 13 -6 -6 4.85 32.17 13 6 -5 33.68 23.45 13 6 -5 31.15 22.79 13 -6 -5 32.99 28.39 13 6 -4 22.22 22.60 13 6 -4 26.98 21.44 13 -6 -4 51.06 29.75 13 6 -3 41.33 21.43 13 6 -3 61.97 21.39 13 -6 -3 81.13 31.86 13 -6 -3 104.93 26.47 13 6 -2 21.42 19.27 13 6 -2 40.52 19.27 -13 6 2 3.34 8.04 13 -6 -2 6.88 27.80 13 -6 -2 10.35 22.11 13 6 -1 -5.69 18.52 13 6 -1 -34.11 29.58 -13 6 1 -0.65 13.21 13 -6 -1 23.74 44.01 13 -6 -1 18.77 22.00 13 6 0 51.06 27.92 13 6 0 31.30 18.21 -13 6 0 22.71 9.63 13 -6 0 43.10 27.43 13 -6 0 46.90 23.91 13 6 1 -3.78 16.49 13 6 1 30.56 16.04 -13 6 -1 1.90 9.58 13 -6 1 10.14 26.37 13 -6 1 -15.66 33.87 13 6 2 40.62 14.84 13 6 2 60.74 16.99 -13 6 -2 54.15 18.26 13 -6 2 65.92 27.79 13 -6 2 69.20 22.44 13 6 3 21.08 20.82 13 6 3 35.11 14.86 -13 6 -3 23.64 18.04 13 -6 3 8.54 26.13 13 -6 3 10.83 20.62 13 6 4 36.12 18.82 13 6 4 37.92 14.31 -13 6 -4 44.17 12.78 13 -6 4 46.59 24.78 13 -6 4 38.17 20.76 13 6 5 25.65 12.24 13 6 5 12.48 11.90 -13 6 -5 -8.15 12.84 13 -6 5 -17.96 36.16 13 -6 5 -5.08 19.64 13 6 6 25.93 11.57 -13 6 -6 50.52 22.59 13 6 6 43.50 17.61 13 -6 6 21.65 22.93 13 7 -8 17.72 18.70 13 -7 -8 -0.81 24.41 13 7 -7 23.84 22.29 13 7 -7 40.43 39.41 13 -7 -7 -34.12 29.33 13 -7 -7 13.59 13.31 13 7 -6 10.95 21.56 13 7 -6 24.00 23.35 13 -7 -6 28.01 29.03 13 -7 -6 10.84 13.95 13 7 -5 1.09 21.88 13 7 -5 4.03 21.09 13 -7 -5 -3.29 31.28 13 7 -4 7.22 21.09 13 7 -4 26.95 21.15 13 -7 -4 7.01 30.88 13 -7 -4 7.98 26.09 13 7 -3 10.81 19.09 13 7 -3 -7.66 19.13 13 -7 -3 0.32 29.62 13 -7 -3 -19.54 25.86 13 7 -2 20.19 31.31 13 7 -2 40.89 31.20 -13 7 2 41.71 15.77 13 -7 -2 28.59 30.81 13 -7 -2 32.93 25.85 13 7 -1 3.08 17.48 13 7 -1 -2.25 17.82 -13 7 1 1.97 9.66 13 -7 -1 -23.39 28.55 13 -7 -1 -11.67 23.71 13 7 0 15.02 16.83 13 7 0 21.08 16.70 -13 7 0 -0.15 10.19 13 -7 0 -9.77 28.98 13 -7 0 18.39 26.10 13 7 1 -6.33 15.06 13 7 1 -16.21 16.07 -13 7 -1 6.71 10.91 13 -7 1 11.55 28.14 13 -7 1 -15.64 21.95 13 7 2 -21.68 13.13 13 7 2 -2.10 14.73 -13 7 -2 1.24 18.64 13 -7 2 25.73 26.51 13 -7 2 9.50 21.27 13 7 3 -0.89 11.71 13 7 3 7.15 13.36 -13 7 -3 11.62 19.24 13 -7 3 -18.23 25.78 13 -7 3 -13.75 20.67 13 7 4 -14.45 16.78 13 7 4 7.11 12.06 -13 7 -4 10.32 20.93 13 -7 4 1.39 26.18 13 -7 4 17.52 20.48 13 7 5 -5.61 11.22 -13 7 -5 -27.30 21.89 13 7 5 -6.78 10.63 13 -7 5 21.69 24.23 13 8 -6 11.37 21.81 13 8 -6 75.39 24.36 13 -8 -6 42.76 30.90 13 -8 -6 16.84 24.92 13 -8 -6 46.91 16.43 13 8 -5 8.13 34.46 13 8 -5 11.09 21.96 13 -8 -5 23.30 33.15 13 -8 -5 19.76 28.67 13 8 -4 53.91 21.42 13 8 -4 48.05 20.91 13 -8 -4 77.54 33.12 13 -8 -4 53.73 29.35 13 8 -3 2.73 30.56 13 8 -3 -35.09 32.13 -13 8 3 -3.49 10.21 13 -8 -3 -50.25 30.95 13 -8 -3 -37.19 42.87 13 8 -2 27.51 18.34 13 8 -2 22.08 29.81 -13 8 2 7.33 10.99 13 -8 -2 3.14 30.72 13 -8 -2 13.31 25.96 13 8 -1 8.53 17.54 13 8 -1 27.90 16.99 -13 8 1 1.79 11.19 13 -8 -1 -10.77 30.12 13 -8 -1 -3.07 41.23 13 8 0 13.73 16.18 13 8 0 3.61 15.95 -13 8 0 11.38 11.81 13 -8 0 7.75 29.81 13 -8 0 33.60 25.16 13 8 1 -12.26 13.50 13 8 1 2.62 15.41 -13 8 -1 -8.66 19.48 13 -8 1 11.92 28.57 13 -8 1 -29.17 16.74 13 8 2 7.27 12.36 13 8 2 8.38 13.97 -13 8 -2 0.57 21.74 13 -8 2 -9.71 28.09 13 -8 2 29.88 16.26 13 8 3 6.72 11.02 13 8 3 10.27 12.15 -13 8 -3 15.16 21.77 13 -8 3 34.88 27.80 13 -8 3 -2.93 15.89 13 8 4 -7.19 11.38 -13 8 -4 -11.58 22.86 13 8 4 -2.46 10.69 13 -8 4 26.93 26.85 13 9 -5 -2.15 20.13 13 9 -5 -9.72 21.91 13 -9 -5 28.06 30.70 13 -9 -5 -6.71 28.66 13 -9 -5 -31.67 14.69 13 9 -4 11.56 32.50 13 9 -4 -4.57 33.94 13 -9 -4 -5.10 32.99 13 -9 -4 18.92 46.01 13 9 -3 42.89 19.40 13 9 -3 -14.94 31.33 -13 9 3 11.99 11.70 13 -9 -3 -19.41 32.64 13 -9 -3 40.16 28.14 13 9 -2 18.50 17.71 13 9 -2 12.47 17.64 -13 9 2 -2.99 12.06 13 -9 -2 -26.73 31.16 13 -9 -2 -33.25 26.95 13 9 -1 1.59 26.39 13 9 -1 8.84 16.68 -13 9 1 15.62 12.56 13 -9 -1 -8.24 30.93 13 -9 -1 2.27 25.87 13 9 0 10.35 22.57 13 9 0 14.95 16.16 -13 9 0 -7.66 20.59 13 -9 0 -9.21 29.75 13 -9 0 -6.73 25.37 13 9 1 -0.45 19.90 13 9 1 3.04 14.41 -13 9 -1 -0.36 22.15 13 -9 1 29.89 29.86 13 -9 1 -29.63 23.86 13 9 2 13.33 17.62 13 9 2 8.97 20.17 -13 9 -2 -25.63 22.72 13 -9 2 5.27 29.62 13 -9 2 -2.22 16.66 13 9 3 7.58 11.88 -13 9 -3 7.35 14.64 13 9 3 -19.12 17.78 13 -9 3 5.96 29.28 13 10 -2 -8.33 27.59 13 10 -2 -16.45 17.47 13 -10 -2 -27.94 52.58 13 -10 -2 12.36 27.88 13 10 -1 -4.47 14.81 13 10 -1 6.56 16.73 -13 10 1 -6.65 21.83 13 -10 -1 26.23 32.26 13 -10 -1 40.70 26.90 13 10 0 -4.43 13.84 13 10 0 -24.42 24.15 13 -10 0 20.14 48.99 13 -10 0 -57.08 43.43 14 0 -5 -63.31 32.05 14 0 -4 40.26 27.91 14 0 -4 31.42 17.94 14 0 -3 4.85 25.60 14 0 -3 -4.01 22.68 14 0 -2 5.25 23.75 14 0 -1 13.56 38.14 14 0 -1 34.12 22.35 14 0 0 -24.52 23.75 14 0 0 -53.15 21.92 14 0 1 20.13 21.80 14 0 1 -2.74 32.31 14 0 2 56.88 22.04 14 0 2 -1.68 20.54 14 0 3 13.38 19.41 14 1 -5 -11.35 17.90 14 -1 -5 -0.31 18.26 14 1 -4 61.39 44.16 14 1 -4 48.24 18.01 14 -1 -4 71.50 29.49 14 -1 -4 63.38 19.08 14 1 -3 -12.87 24.06 14 1 -3 32.30 38.29 14 -1 -3 2.87 26.63 14 -1 -3 23.13 16.98 14 1 -2 54.31 36.86 14 1 -2 12.72 21.62 14 -1 -2 15.19 25.35 14 -1 -2 8.90 26.17 14 1 -1 6.38 22.96 14 1 -1 28.56 21.19 14 -1 -1 15.40 24.22 14 1 0 -25.32 22.57 14 1 0 14.61 32.28 14 -1 0 -1.01 36.11 14 -1 0 -0.67 21.05 14 1 1 13.84 22.03 14 1 1 16.45 20.82 14 -1 1 28.12 22.84 14 -1 1 11.62 20.89 14 1 2 49.56 35.18 14 1 2 78.95 21.62 14 -1 2 56.47 23.55 14 -1 2 108.36 33.95 14 2 -4 20.22 23.61 14 2 -4 1.03 42.22 14 -2 -4 7.19 28.27 14 -2 -4 -17.59 17.60 14 2 -3 -20.64 23.46 14 2 -3 -9.68 22.84 14 -2 -3 15.24 27.89 14 -2 -3 29.71 17.62 14 2 -2 0.61 21.84 14 2 -2 46.65 22.25 14 -2 -2 4.06 26.95 14 -2 -2 20.45 16.51 14 2 -1 35.82 21.66 14 2 -1 7.93 34.33 14 -2 -1 55.36 25.85 14 -2 -1 25.28 23.53 14 2 0 -18.14 34.45 14 2 0 4.04 20.61 14 -2 0 15.15 24.09 14 -2 0 56.46 35.17 14 2 1 -16.30 21.38 14 2 1 16.56 19.53 14 -2 1 -13.18 22.43 14 -2 1 3.67 21.11 14 2 2 7.25 19.43 14 2 2 -13.74 19.10 14 -2 2 -23.79 21.84 14 -2 2 18.13 20.02 14 3 -4 33.73 24.19 14 3 -3 43.25 22.62 14 3 -3 15.71 22.72 14 -3 -3 23.66 47.75 14 -3 -3 1.30 25.08 14 3 -2 24.71 22.45 14 3 -2 16.81 35.26 14 -3 -2 -5.28 28.53 14 -3 -2 33.43 17.12 14 3 -1 14.48 35.09 14 3 -1 0.76 19.98 14 -3 -1 16.60 26.54 14 -3 -1 30.47 26.37 14 3 0 18.78 21.26 14 3 0 9.04 19.24 14 -3 0 -1.31 25.11 14 -3 0 6.61 22.10 14 3 1 41.03 21.21 14 3 1 43.84 19.90 14 -3 1 45.22 25.39 14 -3 1 43.52 22.39 14 4 -2 -26.93 32.88 14 4 -2 1.62 20.32 14 -4 -2 -38.30 45.74 14 -4 -2 13.82 17.16 14 4 -1 2.34 21.30 14 4 -1 22.34 20.56 14 -4 -1 -2.69 28.56 14 -4 -1 -6.08 16.48 14 4 0 -0.14 20.49 14 4 0 27.83 19.55 14 -4 0 37.87 26.49 ; _shelx_hkl_checksum 32965 _shelx_res_file ; TITL User-defined I.res created by SHELXL-2019/3 at 20:36:44 on 25-Aug-2024 CELL 0.71075 11.9686 21.1795 20.1074 90.0000 92.6589 90.0000 ZERR 4 0.0012 0.0022 0.0021 0.0000 0.0065 0.0000 LATT 1 SYMM .50-X, .50+Y, .50-Z SFAC C H O BR N UNIT 212 244.739 40 3.2614 8 L.S. 30 FMAP 2 PLAN 20 WPDB -2 EQIV $1 -x+3/2, y-1/2, -z+3/2 HTAB C37A O6_$1 EQIV $2 -x+1, -y+1, -z+2 HTAB O2 N2_$2 HTAB O2 N2B_$2 HTAB C20 O4 HTAB C27 O6 HTAB C40 N1 BOND $H CONF LIST 4 TEMP -123.1 ACTA SIZE 0.200 0.200 0.180 SADI 0.02 C39A BR1A C39B BR1B C39c BR1c DFIX 1.54 0.01 C36B C37B C37B C38B C38B C39B DFIX 1.54 0.01 C36A C37A C37A C38A C38A C39A DFIX 1.54 0.01 C36c C37c C37c C38c C38c C39c DFIX 1.54 0.01 C49 C50 C50 C51 C51 C52 RIGU 0.01 O1A > Br1c SIMU 0.01 0.02 3 O1A > Br1c RIGU n1 > n2b SIMU 0.01 n1 > n2b dfix 1.15 0.01 c53 n2 c53b n2b n1 c48 n1b c48b dfix 2.65 0.01 c52 n2 c52b n2b n1 c49 n1b c49b dfix 1.47 0.01 c53 c52 c53b c52b c49 c48 c49b c48b sadi 0.01 c1 o1a c1 o1b c3 o1a c3 o1b c1 o1c c3 o1c sadi 0.01 c2 o1a c2 o1b c2 o1c simu 0.01 $Br rigu 0.003 $Br sadi 0.01 c36a c37a c37a c38a c38a c39a c36b c37b c37b c38b c38b c39b sadi 0.01 c36a c38a c37a c39a c36b c38b c37b c39b sump 1 0.000001 1 2 1 3 1 4 sump 0 0.000001 -1 2 1 6 1 7 bind 1 4 WGHT 0.092600 0.683400 FVAR 0.84236 0.79742 0.06533 0.13724 0.62500 0.61278 0.18464 FVAR 0.92356 PART 1 O1A 3 0.628978 0.166578 0.999438 21.00000 0.08643 0.07042 = 0.08152 -0.00699 -0.01668 0.01610 C36A 1 0.639860 0.123952 0.945678 21.00000 0.10888 0.07605 = 0.09061 -0.00881 -0.01377 0.02405 AFIX 23 H36A 2 0.650499 0.147636 0.903999 21.00000 -1.20000 H36B 2 0.571359 0.097991 0.939611 21.00000 -1.20000 AFIX 0 C37A 1 0.740881 0.081589 0.961513 21.00000 0.10595 0.08173 = 0.09491 -0.01681 -0.00768 0.01661 AFIX 23 H37A 2 0.764911 0.062328 0.919651 21.00000 -1.20000 H37B 2 0.803342 0.107934 0.979815 21.00000 -1.20000 AFIX 0 C38A 1 0.718560 0.030496 1.009770 21.00000 0.10914 0.07520 = 0.09559 -0.01536 -0.02631 0.02204 AFIX 23 H38A 2 0.655068 0.004602 0.992045 21.00000 -1.20000 H38B 2 0.696536 0.049642 1.052126 21.00000 -1.20000 AFIX 0 C39A 1 0.819369 -0.012047 1.023548 21.00000 0.12341 0.08182 = 0.10363 -0.01069 -0.02358 0.02481 part 4 AFIX 33 H39C 2 0.800416 -0.044823 1.055529 71.00000 -1.50000 H39D 2 0.840585 -0.031888 0.981949 71.00000 -1.50000 H39E 2 0.882060 0.013160 1.042042 71.00000 -1.50000 AFIX 23 PART 1 H39A 2 0.882816 0.013282 1.042305 61.00000 -1.20000 H39B 2 0.842215 -0.031297 0.981418 61.00000 -1.20000 AFIX 0 BR1A 4 0.782378 -0.078479 1.086385 61.00000 0.16592 0.06874 = 0.15765 0.02046 -0.00894 0.01275 part 0 same c2 o1a > br1a C2 1 0.550166 0.213900 0.993766 11.00000 0.05990 0.06444 = 0.06678 0.00724 -0.00010 0.00598 PART 2 O1B 3 0.623742 0.163973 0.998601 31.00000 0.09741 0.07620 = 0.08792 -0.00680 -0.01327 0.01849 C36B 1 0.578699 0.105770 1.019482 31.00000 0.10193 0.07712 = 0.09103 -0.00866 -0.01535 0.01737 AFIX 23 H36C 2 0.524773 0.089375 0.984859 31.00000 -1.20000 H36D 2 0.538763 0.111889 1.061026 31.00000 -1.20000 AFIX 0 C37B 1 0.674366 0.058854 1.031344 31.00000 0.10883 0.07909 = 0.09503 -0.00939 -0.01945 0.01978 AFIX 23 H37C 2 0.693953 0.040168 0.988283 31.00000 -1.20000 H37D 2 0.740998 0.081463 1.050136 31.00000 -1.20000 AFIX 0 C38B 1 0.643428 0.006394 1.078679 31.00000 0.11587 0.08325 = 0.10045 -0.00934 -0.02066 0.01905 AFIX 23 H38C 2 0.569503 -0.011058 1.064222 31.00000 -1.20000 H38D 2 0.637271 0.024094 1.123931 31.00000 -1.20000 AFIX 0 C39B 1 0.729736 -0.046585 1.081035 31.00000 0.12011 0.08305 = 0.10365 -0.00794 -0.02351 0.02445 AFIX 23 H39F 2 0.695006 -0.082283 1.055912 31.00000 -1.20000 H39G 2 0.737403 -0.060307 1.128092 31.00000 -1.20000 AFIX 0 BR1B 4 0.875093 -0.039230 1.051840 31.00000 0.16964 0.13737 = 0.16010 0.01050 -0.04279 0.05207 PART 3 same o1a > br1a O1C 3 0.609579 0.159338 1.008773 41.00000 0.09857 0.07760 = 0.08901 -0.00365 -0.01380 0.02028 C36C 1 0.568174 0.100401 0.985034 41.00000 0.10163 0.07861 = 0.09056 -0.00632 -0.01435 0.01720 AFIX 23 H36G 2 0.557441 0.101303 0.935927 41.00000 -1.20000 H36H 2 0.495352 0.090996 1.004264 41.00000 -1.20000 AFIX 0 C37C 1 0.655202 0.049667 1.006426 41.00000 0.11022 0.08001 = 0.09642 -0.00875 -0.01895 0.02027 AFIX 23 H37E 2 0.705832 0.044146 0.969300 41.00000 -1.20000 H37F 2 0.700855 0.066859 1.044556 41.00000 -1.20000 AFIX 0 C38C 1 0.615245 -0.015509 1.026175 41.00000 0.11663 0.08606 = 0.10148 -0.01051 -0.01986 0.01894 AFIX 23 H38E 2 0.557749 -0.028763 0.992022 41.00000 -1.20000 H38F 2 0.576759 -0.010603 1.068400 41.00000 -1.20000 AFIX 0 C39C 1 0.698213 -0.071079 1.035874 41.00000 0.12304 0.08505 = 0.10273 -0.00900 -0.02319 0.01676 AFIX 23 H39H 2 0.719706 -0.084975 0.991229 41.00000 -1.20000 H39I 2 0.657568 -0.106576 1.055778 41.00000 -1.20000 AFIX 0 BR1C 4 0.822441 -0.058592 1.085005 41.00000 0.14752 0.11303 = 0.10230 0.01310 -0.05286 0.02212 PART 0 O2 3 0.324304 0.361744 0.979087 11.00000 0.06903 0.09269 = 0.10386 -0.01638 -0.01028 0.02291 H2 2 0.345396 0.392204 1.007204 11.00000 -1.50000 O3 3 0.363030 0.181970 0.793077 11.00000 0.10916 0.06111 = 0.08507 0.00077 0.00723 -0.00043 O4 3 0.319803 0.436753 0.738849 11.00000 0.07004 0.06909 = 0.12619 0.01984 0.02007 0.00584 O5 3 0.588729 0.290244 0.595193 11.00000 0.09071 0.09463 = 0.09680 -0.02546 0.00016 -0.00271 O6 3 0.682254 0.527037 0.698922 11.00000 0.08845 0.08318 = 0.10606 -0.00362 -0.00656 -0.02380 O7 3 0.963149 0.341232 0.700076 11.00000 0.09546 0.14130 = 0.07099 -0.02352 0.00088 0.02041 O8 3 0.925761 0.515945 0.901553 11.00000 0.10185 0.07255 = 0.07275 -0.00142 -0.01763 0.00027 O9 3 0.990314 0.270267 0.929136 11.00000 0.07327 0.06964 = 0.08967 -0.00746 0.02112 0.00296 O10 3 0.713112 0.403227 1.091008 11.00000 0.07738 0.08235 = 0.09485 -0.02176 0.02368 -0.00064 C1 1 0.569170 0.266874 1.033942 11.00000 0.05515 0.06936 = 0.04938 0.00513 0.00756 -0.00757 C3 1 0.457412 0.210917 0.949225 11.00000 0.06430 0.06507 = 0.06293 0.00008 0.00075 -0.00466 AFIX 43 H3 2 0.446014 0.174378 0.922357 11.00000 -1.20000 AFIX 0 C4 1 0.380900 0.260749 0.943410 11.00000 0.04537 0.07147 = 0.05809 0.00806 0.00771 -0.00336 C5 1 0.399394 0.312853 0.984179 11.00000 0.05081 0.07287 = 0.06651 0.00115 0.00691 0.00392 C6 1 0.492076 0.315222 1.029122 11.00000 0.05728 0.07183 = 0.06097 -0.00582 0.00694 0.00021 AFIX 43 H6 2 0.502177 0.351119 1.057085 11.00000 -1.20000 AFIX 0 C7 1 0.282655 0.257965 0.893233 11.00000 0.04964 0.07740 = 0.07042 0.00437 0.00527 -0.00313 AFIX 23 H7A 2 0.219818 0.282628 0.910294 11.00000 -1.20000 H7B 2 0.257697 0.213594 0.888113 11.00000 -1.20000 AFIX 0 C8 1 0.311395 0.283798 0.825410 11.00000 0.03995 0.07143 = 0.06240 0.00016 -0.00339 -0.00434 C9 1 0.353613 0.244938 0.776498 11.00000 0.06161 0.05803 = 0.06630 -0.00011 -0.00732 -0.00664 C10 1 0.383320 0.269661 0.715892 11.00000 0.06184 0.06999 = 0.06237 -0.00938 -0.00544 -0.00608 AFIX 43 H10 2 0.412121 0.242392 0.683312 11.00000 -1.20000 AFIX 0 C11 1 0.371590 0.333747 0.702091 11.00000 0.04854 0.06968 = 0.06007 0.00159 -0.00633 -0.01107 C12 1 0.328868 0.372220 0.750585 11.00000 0.04505 0.06156 = 0.07905 0.00532 0.00077 -0.00237 C13 1 0.299481 0.347322 0.810744 11.00000 0.04719 0.06859 = 0.07241 -0.00252 0.00383 0.00049 AFIX 43 H13 2 0.270159 0.374657 0.843089 11.00000 -1.20000 AFIX 0 C14 1 0.407107 0.360406 0.636375 11.00000 0.06463 0.08614 = 0.06172 0.00317 -0.00782 -0.01322 AFIX 23 H14A 2 0.355321 0.394869 0.622366 11.00000 -1.20000 H14B 2 0.400995 0.326889 0.602080 11.00000 -1.20000 AFIX 0 C15 1 0.526026 0.385774 0.639981 11.00000 0.06436 0.08013 = 0.04830 0.00782 -0.00148 -0.01020 C16 1 0.615233 0.349164 0.620352 11.00000 0.07122 0.08560 = 0.05426 -0.00269 -0.00175 -0.00776 C17 1 0.724192 0.373201 0.626852 11.00000 0.06656 0.10976 = 0.05034 0.00233 0.00325 0.00195 AFIX 43 H17 2 0.784561 0.348427 0.612307 11.00000 -1.20000 AFIX 0 C18 1 0.745818 0.431996 0.653879 11.00000 0.06546 0.09790 = 0.04853 0.01075 -0.00212 -0.01829 C19 1 0.656406 0.468546 0.672962 11.00000 0.07225 0.08054 = 0.05677 0.01036 -0.00403 -0.01625 C20 1 0.548263 0.445369 0.665531 11.00000 0.06358 0.07586 = 0.06405 0.00577 0.00002 -0.00556 AFIX 43 H20 2 0.487826 0.471059 0.678307 11.00000 -1.20000 AFIX 0 C21 1 0.866255 0.455340 0.664082 11.00000 0.06474 0.12984 = 0.05975 0.01351 -0.00097 -0.02226 AFIX 23 H21A 2 0.914090 0.433802 0.632229 11.00000 -1.20000 H21B 2 0.869131 0.501278 0.655220 11.00000 -1.20000 AFIX 0 C22 1 0.910423 0.442286 0.734599 11.00000 0.04913 0.10798 = 0.05840 0.01021 0.00365 -0.01665 C23 1 0.957641 0.383866 0.751176 11.00000 0.05475 0.11135 = 0.05803 -0.01279 0.00936 -0.01066 C24 1 0.996830 0.371754 0.816226 11.00000 0.05185 0.09474 = 0.06340 0.00111 0.00403 -0.00094 AFIX 43 H24 2 1.031625 0.332414 0.826518 11.00000 -1.20000 AFIX 0 C25 1 0.985971 0.416018 0.866126 11.00000 0.04644 0.07988 = 0.05826 0.00177 0.00318 -0.01397 C26 1 0.937345 0.474220 0.850167 11.00000 0.05564 0.07281 = 0.06627 0.00733 -0.00192 -0.01396 C27 1 0.902089 0.486977 0.784021 11.00000 0.06185 0.08451 = 0.06818 0.01465 -0.00917 -0.02003 AFIX 43 H27 2 0.871791 0.527304 0.773017 11.00000 -1.20000 AFIX 0 C28 1 1.024865 0.400752 0.937192 11.00000 0.05081 0.07185 = 0.06143 0.00319 -0.00468 -0.00660 AFIX 23 H28A 2 1.045515 0.440415 0.960741 11.00000 -1.20000 H28B 2 1.092461 0.373846 0.936705 11.00000 -1.20000 AFIX 0 C29 1 0.935267 0.366856 0.974840 11.00000 0.04820 0.06641 = 0.05206 0.00318 -0.00625 -0.00359 C30 1 0.919107 0.302099 0.969537 11.00000 0.04993 0.06993 = 0.05204 -0.00189 0.00299 0.00492 C31 1 0.835424 0.272431 1.003602 11.00000 0.05934 0.05897 = 0.05506 0.00474 -0.00489 0.00044 AFIX 43 H31 2 0.825188 0.228128 0.999134 11.00000 -1.20000 AFIX 0 C32 1 0.766349 0.306700 1.044194 11.00000 0.05063 0.07358 = 0.04426 0.00299 -0.00251 0.00045 C33 1 0.783290 0.371156 1.050128 11.00000 0.05422 0.06984 = 0.05865 -0.00591 0.00106 0.00358 C34 1 0.866123 0.400599 1.015500 11.00000 0.05570 0.06580 = 0.06146 -0.00586 -0.00117 -0.00200 AFIX 43 H34 2 0.875820 0.444963 1.019692 11.00000 -1.20000 AFIX 0 C35 1 0.673635 0.272792 1.079208 11.00000 0.05695 0.08203 = 0.05245 0.00701 0.00085 -0.00439 AFIX 23 H35A 2 0.699691 0.230184 1.092965 11.00000 -1.20000 H35B 2 0.655725 0.296497 1.119790 11.00000 -1.20000 AFIX 0 C40 1 0.403722 0.139950 0.744814 11.00000 0.16616 0.06339 = 0.12256 -0.01624 0.01970 0.00136 AFIX 137 H40A 2 0.410223 0.097424 0.763809 11.00000 -1.50000 H40B 2 0.477344 0.154233 0.731587 11.00000 -1.50000 H40C 2 0.351694 0.139182 0.705724 11.00000 -1.50000 AFIX 0 sadi 0.01 o4 c41 o4 c41a sadi c12 c41 c12 c41a eadp C41 C41a part 1 81.0 C41 1 0.211658 0.460224 0.728970 81.00000 0.08346 0.09147 = 0.13325 0.02613 0.02604 0.02987 AFIX 137 H41A 2 0.170966 0.434965 0.694951 81.00000 -1.50000 H41B 2 0.214907 0.504254 0.714200 81.00000 -1.50000 H41C 2 0.172973 0.457976 0.770806 81.00000 -1.50000 AFIX 0 part 2 -81.0 C41A 1 0.277877 0.474802 0.787656 -81.00000 0.08346 0.09147 = 0.13325 0.02613 0.02604 0.02987 AFIX 137 H41D 2 0.220495 0.451679 0.810934 -81.00000 -1.50000 H41E 2 0.244799 0.512832 0.767147 -81.00000 -1.50000 H41F 2 0.338605 0.486876 0.819496 -81.00000 -1.50000 AFIX 0 part 0 C42 1 0.675564 0.252466 0.572022 11.00000 0.11900 0.11025 = 0.12181 -0.03482 -0.00925 0.02796 AFIX 137 H42A 2 0.728380 0.242243 0.609163 11.00000 -1.50000 H42B 2 0.714638 0.275492 0.537782 11.00000 -1.50000 H42C 2 0.644114 0.213369 0.552992 11.00000 -1.50000 AFIX 0 C43 1 0.593782 0.566292 0.718847 11.00000 0.11911 0.08030 = 0.18070 -0.01823 -0.00675 -0.00347 AFIX 137 H43A 2 0.624596 0.606040 0.736633 11.00000 -1.50000 H43B 2 0.552693 0.544818 0.753306 11.00000 -1.50000 H43C 2 0.542938 0.575135 0.680366 11.00000 -1.50000 AFIX 0 C44 1 1.007263 0.280902 0.715123 11.00000 0.11182 0.16598 = 0.09380 -0.05483 0.00176 0.03752 AFIX 137 H44A 2 0.999801 0.254001 0.675511 11.00000 -1.50000 H44B 2 0.966173 0.261987 0.751158 11.00000 -1.50000 H44C 2 1.086475 0.284786 0.729159 11.00000 -1.50000 AFIX 0 C45 1 0.875323 0.575122 0.887391 11.00000 0.11131 0.07924 = 0.09484 0.00752 -0.01790 0.00900 AFIX 137 H45A 2 0.801195 0.568578 0.865718 11.00000 -1.50000 H45B 2 0.922067 0.599197 0.857699 11.00000 -1.50000 H45C 2 0.867760 0.598595 0.928942 11.00000 -1.50000 AFIX 0 C46 1 0.978527 0.204652 0.922818 11.00000 0.08696 0.08207 = 0.12355 -0.02162 0.02507 0.00668 AFIX 137 H46A 2 0.902734 0.194691 0.905415 11.00000 -1.50000 H46B 2 0.991513 0.184781 0.966509 11.00000 -1.50000 H46C 2 1.033093 0.188620 0.892113 11.00000 -1.50000 AFIX 0 C47 1 0.731686 0.468067 1.101703 11.00000 0.11446 0.08386 = 0.13361 -0.03111 0.02836 0.00456 AFIX 137 H47A 2 0.720997 0.490778 1.059422 11.00000 -1.50000 H47B 2 0.808300 0.474616 1.119713 11.00000 -1.50000 H47C 2 0.678705 0.483998 1.133428 11.00000 -1.50000 AFIX 0 part 1 51.0 same n2 < n1 N1 5 0.688415 0.182572 0.768128 51.00000 0.16829 0.12280 = 0.16891 -0.02185 0.01636 0.02767 C48 1 0.703547 0.235997 0.777649 51.00000 0.12223 0.12039 = 0.13383 -0.01506 -0.00060 0.01366 C49 1 0.716573 0.302796 0.796004 51.00000 0.12143 0.12221 = 0.11874 0.00128 0.02408 -0.00925 AFIX 23 H49A 2 0.713396 0.328781 0.755032 51.00000 -1.20000 H49B 2 0.791025 0.309049 0.818579 51.00000 -1.20000 AFIX 0 C50 1 0.629253 0.324713 0.840435 51.00000 0.09871 0.10635 = 0.11200 -0.00820 0.01275 -0.00855 AFIX 23 H50A 2 0.633032 0.300413 0.882539 51.00000 -1.20000 H50B 2 0.554041 0.318957 0.818674 51.00000 -1.20000 AFIX 0 C51 1 0.652091 0.396282 0.854597 51.00000 0.09890 0.10914 = 0.11052 -0.01173 0.01066 -0.00891 AFIX 23 H51A 2 0.727090 0.401772 0.876720 51.00000 -1.20000 H51B 2 0.649674 0.420260 0.812291 51.00000 -1.20000 AFIX 0 C52 1 0.565220 0.419817 0.898118 51.00000 0.12555 0.10980 = 0.13746 -0.01246 0.02880 -0.01510 AFIX 23 H52A 2 0.491540 0.418426 0.873661 51.00000 -1.20000 H52B 2 0.561603 0.391966 0.937502 51.00000 -1.20000 AFIX 0 C53 1 0.588636 0.484786 0.920205 51.00000 0.12022 0.10748 = 0.13343 -0.02607 0.01121 -0.00979 N2 5 0.610327 0.537205 0.932678 51.00000 0.12791 0.10563 = 0.17093 -0.03035 0.01702 -0.00510 part 2 -51.0 same 0.01 0.02 n1 > n2 N1B 5 0.710454 0.192164 0.741567 -51.00000 0.15450 0.13503 = 0.13453 -0.02166 0.01733 0.02298 C48B 1 0.702142 0.227809 0.784956 -51.00000 0.12563 0.11969 = 0.13262 -0.01450 0.00052 0.00782 C49B 1 0.709588 0.280396 0.832810 -51.00000 0.12228 0.12455 = 0.12559 -0.00563 -0.00281 0.00396 AFIX 23 H49C 2 0.690537 0.264687 0.877251 -51.00000 -1.20000 H49D 2 0.787609 0.296010 0.836214 -51.00000 -1.20000 AFIX 0 C50B 1 0.635228 0.332685 0.813948 -51.00000 0.10320 0.10771 = 0.11571 -0.00877 0.00811 -0.00544 AFIX 23 H50C 2 0.556833 0.317813 0.809341 -51.00000 -1.20000 H50D 2 0.656074 0.350849 0.770884 -51.00000 -1.20000 AFIX 0 C51B 1 0.648058 0.383681 0.870600 -51.00000 0.10211 0.10837 = 0.11930 -0.01203 0.01464 -0.00886 AFIX 23 H51C 2 0.636013 0.364028 0.914362 -51.00000 -1.20000 H51D 2 0.724370 0.401802 0.871721 -51.00000 -1.20000 AFIX 0 C52B 1 0.565519 0.433213 0.857175 -51.00000 0.12013 0.11454 = 0.12108 -0.01500 0.00322 -0.00433 AFIX 23 H52C 2 0.489617 0.416165 0.863136 -51.00000 -1.20000 H52D 2 0.569423 0.447405 0.810428 -51.00000 -1.20000 AFIX 0 C53B 1 0.585502 0.487550 0.902291 -51.00000 0.11989 0.10874 = 0.13656 -0.02947 0.00834 -0.00942 N2B 5 0.595092 0.525410 0.944229 -51.00000 0.12753 0.10561 = 0.14155 -0.02822 0.00419 -0.01114 REM REM /Volumes/Data3/Dropbox/editor/2024/Acta/jq2036/revised manuscript/I.hkl REM HKLF 4 REM User-defined REM wR2 = 0.1702, GooF = S = 1.017, Restrained GooF = 1.035 for all data REM R1 = 0.0541 for 5350 Fo > 4sig(Fo) and 0.0951 for all 8895 data REM 797 parameters refined using 1090 restraints END WGHT 0.0926 0.6832 REM Highest difference peak 0.393, deepest hole -0.233, 1-sigma level 0.036 Q1 1 0.7399 -0.0850 1.0363 11.00000 0.05 0.39 Q2 1 0.8225 -0.0673 1.0364 11.00000 0.05 0.27 Q3 1 0.9286 -0.0230 1.0159 11.00000 0.05 0.27 Q4 1 1.0000 0.0000 1.0000 10.50000 0.05 0.22 Q5 1 0.6896 -0.0665 1.0855 11.00000 0.05 0.19 Q6 1 0.6276 0.4505 0.8419 11.00000 0.05 0.18 Q7 1 0.8789 -0.0393 1.0921 11.00000 0.05 0.16 Q8 1 0.6584 0.4258 0.9038 11.00000 0.05 0.15 Q9 1 0.8015 0.0491 0.9875 11.00000 0.05 0.15 Q10 1 0.6481 0.2975 0.7764 11.00000 0.05 0.15 Q11 1 0.3718 0.6318 0.7489 11.00000 0.05 0.15 Q12 1 0.6137 0.0335 1.0425 11.00000 0.05 0.14 Q13 1 0.7113 -0.0358 1.0190 11.00000 0.05 0.14 Q14 1 0.7751 -0.0327 1.0712 11.00000 0.05 0.14 Q15 1 0.6318 0.0524 1.0556 11.00000 0.05 0.13 Q16 1 0.6372 0.2700 0.8442 11.00000 0.05 0.13 Q17 1 0.6054 0.3241 0.7547 11.00000 0.05 0.13 Q18 1 0.8177 0.1991 0.9754 11.00000 0.05 0.13 Q19 1 0.7537 0.2470 0.6025 11.00000 0.05 0.13 Q20 1 0.8057 0.2241 0.9842 11.00000 0.05 0.12 ; _shelx_res_checksum 52664 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1A 0.6290(3) 0.16658(14) 0.9994(3) 0.0801(12) Uani d 0.7974(18) A 1 C C36A 0.6399(4) 0.12395(19) 0.9457(2) 0.0924(11) Uani d 0.7974(18) A 1 H H36A 0.650499 0.147636 0.903999 0.111 Uiso calc 0.7974(18) A 1 H H36B 0.571359 0.097991 0.939611 0.111 Uiso calc 0.7974(18) A 1 C C37A 0.7409(3) 0.08159(17) 0.9615(2) 0.0946(11) Uani d 0.7974(18) A 1 H H37A 0.764911 0.062328 0.919651 0.113 Uiso calc 0.7974(18) A 1 H H37B 0.803342 0.107934 0.979815 0.113 Uiso calc 0.7974(18) A 1 C C38A 0.7186(4) 0.03050(17) 1.0098(2) 0.0943(11) Uani d 0.7974(18) A 1 H H38A 0.655068 0.004602 0.992045 0.113 Uiso calc 0.7974(18) A 1 H H38B 0.696536 0.049642 1.052126 0.113 Uiso calc 0.7974(18) A 1 C C39A 0.8194(4) -0.0120(2) 1.0235(3) 0.1039(12) Uani d 0.7974(18) A 1 H H39C 0.800416 -0.044823 1.055529 0.156 Uiso calc 0.185(2) B 4 H H39D 0.840585 -0.031888 0.981949 0.156 Uiso calc 0.185(2) B 4 H H39E 0.882060 0.013160 1.042042 0.156 Uiso calc 0.185(2) B 4 H H39A 0.882816 0.013282 1.042305 0.125 Uiso calc 0.613(2) C 1 H H39B 0.842215 -0.031297 0.981418 0.125 Uiso calc 0.613(2) C 1 Br Br1A 0.78238(16) -0.07848(6) 1.08639(10) 0.1313(6) Uani d 0.613(2) A 1 C C2 0.5502(2) 0.21390(12) 0.99377(14) 0.0638(6) Uani d 1 . . O O1B 0.624(2) 0.1640(10) 0.9986(19) 0.088(2) Uani d 0.0653(18) A 2 C C36B 0.579(3) 0.1058(15) 1.019(3) 0.0906(19) Uani d 0.0653(18) A 2 H H36C 0.524773 0.089375 0.984859 0.109 Uiso calc 0.0653(18) A 2 H H36D 0.538763 0.111889 1.061026 0.109 Uiso calc 0.0653(18) A 2 C C37B 0.674(3) 0.0589(15) 1.031(2) 0.0951(18) Uani d 0.0653(18) A 2 H H37C 0.693953 0.040168 0.988283 0.114 Uiso calc 0.0653(18) A 2 H H37D 0.740998 0.081463 1.050136 0.114 Uiso calc 0.0653(18) A 2 C C38B 0.643(3) 0.0064(16) 1.079(2) 0.101(2) Uani d 0.0653(18) A 2 H H38C 0.569503 -0.011058 1.064222 0.121 Uiso calc 0.0653(18) A 2 H H38D 0.637271 0.024094 1.123931 0.121 Uiso calc 0.0653(18) A 2 C C39B 0.730(3) -0.0466(16) 1.081(3) 0.103(2) Uani d 0.0653(18) A 2 H H39F 0.695006 -0.082283 1.055912 0.124 Uiso calc 0.0653(18) A 2 H H39G 0.737403 -0.060307 1.128092 0.124 Uiso calc 0.0653(18) A 2 Br Br1B 0.8751(12) -0.0392(6) 1.0518(8) 0.157(4) Uani d 0.0653(18) A 2 O O1C 0.610(2) 0.1593(6) 1.0088(14) 0.089(2) Uani d 0.137(2) A 3 C C36C 0.5682(19) 0.1004(7) 0.9850(14) 0.0909(18) Uani d 0.137(2) A 3 H H36G 0.557441 0.101303 0.935927 0.109 Uiso calc 0.137(2) A 3 H H36H 0.495352 0.090996 1.004264 0.109 Uiso calc 0.137(2) A 3 C C37C 0.6552(18) 0.0497(8) 1.0064(14) 0.0963(18) Uani d 0.137(2) A 3 H H37E 0.705832 0.044146 0.969300 0.116 Uiso calc 0.137(2) A 3 H H37F 0.700855 0.066859 1.044556 0.116 Uiso calc 0.137(2) A 3 C C38C 0.6152(16) -0.0155(8) 1.0262(14) 0.102(2) Uani d 0.137(2) A 3 H H38E 0.557749 -0.028763 0.992022 0.123 Uiso calc 0.137(2) A 3 H H38F 0.576759 -0.010603 1.068400 0.123 Uiso calc 0.137(2) A 3 C C39C 0.6982(17) -0.0711(9) 1.0359(14) 0.104(2) Uani d 0.137(2) A 3 H H39H 0.719706 -0.084975 0.991229 0.125 Uiso calc 0.137(2) A 3 H H39I 0.657568 -0.106576 1.055778 0.125 Uiso calc 0.137(2) A 3 Br Br1C 0.8224(7) -0.0586(4) 1.0850(4) 0.123(2) Uani d 0.137(2) A 3 O O2 0.32430(17) 0.36174(11) 0.97909(12) 0.0890(7) Uani d 1 . . H H2 0.345(3) 0.392(2) 1.007(2) 0.133 Uiso d 1 . . O O3 0.36303(18) 0.18197(9) 0.79308(11) 0.0850(6) Uani d 1 . . O O4 0.31980(16) 0.43675(9) 0.73885(12) 0.0880(6) Uani d 1 . . O O5 0.58873(18) 0.29024(11) 0.59519(12) 0.0942(7) Uani d 1 . . O O6 0.68225(18) 0.52704(10) 0.69892(12) 0.0929(7) Uani d 1 . . O O7 0.96315(19) 0.34123(13) 0.70008(11) 0.1027(7) Uani d 1 . . O O8 0.92576(17) 0.51595(9) 0.90155(10) 0.0831(6) Uani d 1 . . O O9 0.99031(15) 0.27027(9) 0.92914(10) 0.0770(5) Uani d 1 . . O O10 0.71311(16) 0.40323(10) 1.09101(11) 0.0843(6) Uani d 1 . . C C1 0.5692(2) 0.26687(12) 1.03394(12) 0.0578(6) Uani d 1 . . C C3 0.4574(2) 0.21092(12) 0.94922(13) 0.0642(7) Uani d 1 . . H H3 0.446014 0.174378 0.922357 0.077 Uiso calc 1 . . C C4 0.38090(19) 0.26075(12) 0.94341(12) 0.0581(6) Uani d 1 . . C C5 0.3994(2) 0.31285(13) 0.98418(14) 0.0633(7) Uani d 1 . . C C6 0.4921(2) 0.31522(13) 1.02912(13) 0.0632(7) Uani d 1 . . H H6 0.502177 0.351119 1.057085 0.076 Uiso calc 1 . . C C7 0.2827(2) 0.25796(14) 0.89323(13) 0.0657(7) Uani d 1 . . H H7A 0.219818 0.282628 0.910294 0.079 Uiso calc 1 . . H H7B 0.257697 0.213594 0.888113 0.079 Uiso calc 1 . . C C8 0.31140(18) 0.28380(12) 0.82541(13) 0.0581(6) Uani d 1 . . C C9 0.3536(2) 0.24494(12) 0.77650(14) 0.0623(7) Uani d 1 . . C C10 0.3833(2) 0.26966(13) 0.71589(14) 0.0650(7) Uani d 1 . . H H10 0.412121 0.242392 0.683312 0.078 Uiso calc 1 . . C C11 0.37159(19) 0.33375(13) 0.70209(13) 0.0597(7) Uani d 1 . . C C12 0.32887(19) 0.37222(12) 0.75059(14) 0.0620(7) Uani d 1 . . C C13 0.29948(19) 0.34732(12) 0.81074(14) 0.0627(7) Uani d 1 . . H H13 0.270159 0.374657 0.843089 0.075 Uiso calc 1 . . C C14 0.4071(2) 0.36041(14) 0.63637(13) 0.0712(7) Uani d 1 . . H H14A 0.355321 0.394869 0.622366 0.085 Uiso calc 1 . . H H14B 0.400995 0.326889 0.602080 0.085 Uiso calc 1 . . C C15 0.5260(2) 0.38577(13) 0.63998(13) 0.0644(7) Uani d 1 . . C C16 0.6152(2) 0.34916(14) 0.62035(13) 0.0705(7) Uani d 1 . . C C17 0.7242(2) 0.37320(16) 0.62685(13) 0.0755(8) Uani d 1 . . H H17 0.784561 0.348427 0.612307 0.091 Uiso calc 1 . . C C18 0.7458(2) 0.43200(15) 0.65388(13) 0.0708(8) Uani d 1 . . C C19 0.6564(2) 0.46855(14) 0.67296(14) 0.0701(7) Uani d 1 . . C C20 0.5483(2) 0.44537(13) 0.66553(14) 0.0679(7) Uani d 1 . . H H20 0.487826 0.471059 0.678307 0.082 Uiso calc 1 . . C C21 0.8663(2) 0.45534(18) 0.66408(14) 0.0849(9) Uani d 1 . . H H21A 0.914090 0.433802 0.632229 0.102 Uiso calc 1 . . H H21B 0.869131 0.501278 0.655220 0.102 Uiso calc 1 . . C C22 0.9104(2) 0.44229(16) 0.73460(14) 0.0718(8) Uani d 1 . . C C23 0.9576(2) 0.38387(16) 0.75118(14) 0.0745(8) Uani d 1 . . C C24 0.9968(2) 0.37175(15) 0.81623(14) 0.0700(7) Uani d 1 . . H H24 1.031625 0.332414 0.826518 0.084 Uiso calc 1 . . C C25 0.9860(2) 0.41602(13) 0.86613(13) 0.0615(7) Uani d 1 . . C C26 0.9373(2) 0.47422(13) 0.85017(14) 0.0651(7) Uani d 1 . . C C27 0.9021(2) 0.48698(15) 0.78402(14) 0.0719(8) Uani d 1 . . H H27 0.871791 0.527304 0.773017 0.086 Uiso calc 1 . . C C28 1.0249(2) 0.40075(13) 0.93719(13) 0.0616(7) Uani d 1 . . H H28A 1.045515 0.440415 0.960741 0.074 Uiso calc 1 . . H H28B 1.092461 0.373846 0.936705 0.074 Uiso calc 1 . . C C29 0.93527(19) 0.36686(12) 0.97484(12) 0.0558(6) Uani d 1 . . C C30 0.91911(19) 0.30210(12) 0.96954(12) 0.0573(6) Uani d 1 . . C C31 0.8354(2) 0.27243(12) 1.00360(12) 0.0580(6) Uani d 1 . . H H31 0.825188 0.228128 0.999134 0.070 Uiso calc 1 . . C C32 0.76635(19) 0.30670(12) 1.04419(12) 0.0563(6) Uani d 1 . . C C33 0.7833(2) 0.37116(13) 1.05013(13) 0.0610(6) Uani d 1 . . C C34 0.8661(2) 0.40060(13) 1.01550(13) 0.0611(6) Uani d 1 . . H H34 0.875820 0.444963 1.019692 0.073 Uiso calc 1 . . C C35 0.6736(2) 0.27279(13) 1.07921(13) 0.0639(7) Uani d 1 . . H H35A 0.699691 0.230184 1.092965 0.077 Uiso calc 1 . . H H35B 0.655725 0.296497 1.119790 0.077 Uiso calc 1 . . C C40 0.4037(4) 0.13995(15) 0.7448(2) 0.1170(13) Uani d 1 . . H H40A 0.410223 0.097424 0.763809 0.175 Uiso calc 1 . . H H40B 0.477344 0.154233 0.731587 0.175 Uiso calc 1 . . H H40C 0.351694 0.139182 0.705724 0.175 Uiso calc 1 . . C C41 0.2117(3) 0.46022(18) 0.7290(2) 0.1021(14) Uani d 0.924(6) D 1 H H41A 0.170966 0.434965 0.694951 0.153 Uiso calc 0.924(6) D 1 H H41B 0.214907 0.504254 0.714200 0.153 Uiso calc 0.924(6) D 1 H H41C 0.172973 0.457976 0.770806 0.153 Uiso calc 0.924(6) D 1 C C41A 0.278(4) 0.4748(12) 0.7877(15) 0.1021(14) Uani d 0.076(6) D 2 H H41D 0.220495 0.451679 0.810934 0.153 Uiso calc 0.076(6) D 2 H H41E 0.244799 0.512832 0.767147 0.153 Uiso calc 0.076(6) D 2 H H41F 0.338605 0.486876 0.819496 0.153 Uiso calc 0.076(6) D 2 C C42 0.6756(3) 0.25247(19) 0.5720(2) 0.1175(13) Uani d 1 . . H H42A 0.728380 0.242243 0.609163 0.176 Uiso calc 1 . . H H42B 0.714638 0.275492 0.537782 0.176 Uiso calc 1 . . H H42C 0.644114 0.213369 0.552992 0.176 Uiso calc 1 . . C C43 0.5938(4) 0.56629(17) 0.7188(3) 0.1271(15) Uani d 1 . . H H43A 0.624596 0.606040 0.736633 0.191 Uiso calc 1 . . H H43B 0.552693 0.544818 0.753306 0.191 Uiso calc 1 . . H H43C 0.542938 0.575135 0.680366 0.191 Uiso calc 1 . . C C44 1.0073(3) 0.2809(2) 0.7151(2) 0.1240(15) Uani d 1 . . H H44A 0.999801 0.254001 0.675511 0.186 Uiso calc 1 . . H H44B 0.966173 0.261987 0.751158 0.186 Uiso calc 1 . . H H44C 1.086475 0.284786 0.729159 0.186 Uiso calc 1 . . C C45 0.8753(3) 0.57512(15) 0.88739(18) 0.0958(10) Uani d 1 . . H H45A 0.801195 0.568578 0.865718 0.144 Uiso calc 1 . . H H45B 0.922067 0.599197 0.857699 0.144 Uiso calc 1 . . H H45C 0.867760 0.598595 0.928942 0.144 Uiso calc 1 . . C C46 0.9785(3) 0.20465(15) 0.9228(2) 0.0969(10) Uani d 1 . . H H46A 0.902734 0.194691 0.905415 0.145 Uiso calc 1 . . H H46B 0.991513 0.184781 0.966509 0.145 Uiso calc 1 . . H H46C 1.033093 0.188620 0.892113 0.145 Uiso calc 1 . . C C47 0.7317(3) 0.46807(16) 1.1017(2) 0.1099(12) Uani d 1 . . H H47A 0.720997 0.490778 1.059422 0.165 Uiso calc 1 . . H H47B 0.808300 0.474616 1.119713 0.165 Uiso calc 1 . . H H47C 0.678705 0.483998 1.133428 0.165 Uiso calc 1 . . N N1 0.6884(13) 0.1826(4) 0.7681(6) 0.153(4) Uani d 0.625(8) E 1 C C48 0.7035(17) 0.2360(4) 0.7776(7) 0.126(2) Uani d 0.625(8) E 1 C C49 0.7166(6) 0.3028(3) 0.7960(5) 0.120(2) Uani d 0.625(8) E 1 H H49A 0.713396 0.328781 0.755032 0.144 Uiso calc 0.625(8) E 1 H H49B 0.791025 0.309049 0.818579 0.144 Uiso calc 0.625(8) E 1 C C50 0.6293(7) 0.3247(3) 0.8404(5) 0.105(2) Uani d 0.625(8) E 1 H H50A 0.633032 0.300413 0.882539 0.127 Uiso calc 0.625(8) E 1 H H50B 0.554041 0.318957 0.818674 0.127 Uiso calc 0.625(8) E 1 C C51 0.6521(7) 0.3963(3) 0.8546(5) 0.106(2) Uani d 0.625(8) E 1 H H51A 0.727090 0.401772 0.876720 0.127 Uiso calc 0.625(8) E 1 H H51B 0.649674 0.420260 0.812291 0.127 Uiso calc 0.625(8) E 1 C C52 0.5652(7) 0.4198(3) 0.8981(5) 0.124(2) Uani d 0.625(8) E 1 H H52A 0.491540 0.418426 0.873661 0.148 Uiso calc 0.625(8) E 1 H H52B 0.561603 0.391966 0.937502 0.148 Uiso calc 0.625(8) E 1 C C53 0.5886(14) 0.4848(4) 0.9202(6) 0.120(2) Uani d 0.625(8) E 1 N N2 0.610(2) 0.5372(5) 0.9327(8) 0.135(4) Uani d 0.625(8) E 1 N N1B 0.710(2) 0.1922(8) 0.7416(8) 0.141(5) Uani d 0.375(8) E 2 C C48B 0.702(3) 0.2278(8) 0.7850(11) 0.126(3) Uani d 0.375(8) E 2 C C49B 0.7096(12) 0.2804(6) 0.8328(8) 0.124(2) Uani d 0.375(8) E 2 H H49C 0.690537 0.264687 0.877251 0.149 Uiso calc 0.375(8) E 2 H H49D 0.787609 0.296010 0.836214 0.149 Uiso calc 0.375(8) E 2 C C50B 0.6352(14) 0.3327(6) 0.8139(7) 0.109(3) Uani d 0.375(8) E 2 H H50C 0.556833 0.317813 0.809341 0.131 Uiso calc 0.375(8) E 2 H H50D 0.656074 0.350849 0.770884 0.131 Uiso calc 0.375(8) E 2 C C51B 0.6481(14) 0.3837(6) 0.8706(8) 0.110(3) Uani d 0.375(8) E 2 H H51C 0.636013 0.364028 0.914362 0.132 Uiso calc 0.375(8) E 2 H H51D 0.724370 0.401802 0.871721 0.132 Uiso calc 0.375(8) E 2 C C52B 0.5655(11) 0.4332(5) 0.8572(8) 0.119(2) Uani d 0.375(8) E 2 H H52C 0.489617 0.416165 0.863136 0.142 Uiso calc 0.375(8) E 2 H H52D 0.569423 0.447405 0.810428 0.142 Uiso calc 0.375(8) E 2 C C53B 0.586(2) 0.4876(7) 0.9023(10) 0.122(3) Uani d 0.375(8) E 2 N N2B 0.595(4) 0.5254(10) 0.9442(11) 0.125(5) Uani d 0.375(8) E 2 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 O1A 0.0864(19) 0.0704(15) 0.0815(19) 0.0161(14) -0.0167(17) -0.0070(14) C36A 0.109(2) 0.076(2) 0.091(2) 0.0240(19) -0.014(2) -0.0088(19) C37A 0.106(2) 0.082(2) 0.095(2) 0.0166(19) -0.008(2) -0.0168(19) C38A 0.109(2) 0.075(2) 0.096(2) 0.0220(19) -0.026(2) -0.0154(19) C39A 0.123(3) 0.082(2) 0.104(3) 0.025(2) -0.024(2) -0.011(2) Br1A 0.1659(13) 0.0687(6) 0.1577(10) 0.0128(6) -0.0089(9) 0.0205(5) C2 0.0599(14) 0.0644(15) 0.0668(16) 0.0060(12) -0.0001(13) 0.0072(13) O1B 0.097(4) 0.076(4) 0.088(4) 0.018(4) -0.013(4) -0.007(4) C36B 0.102(3) 0.077(3) 0.091(3) 0.017(3) -0.015(3) -0.009(3) C37B 0.109(3) 0.079(3) 0.095(3) 0.020(3) -0.019(3) -0.009(3) C38B 0.116(4) 0.083(4) 0.100(4) 0.019(4) -0.021(4) -0.009(4) C39B 0.120(4) 0.083(4) 0.104(4) 0.024(4) -0.024(4) -0.008(4) Br1B 0.170(7) 0.137(6) 0.160(7) 0.052(5) -0.043(6) 0.011(6) O1C 0.099(4) 0.078(3) 0.089(4) 0.020(3) -0.014(4) -0.004(3) C36C 0.102(3) 0.079(3) 0.091(3) 0.017(3) -0.014(3) -0.006(3) C37C 0.110(3) 0.080(3) 0.096(3) 0.020(3) -0.019(3) -0.009(3) C38C 0.117(4) 0.086(3) 0.101(4) 0.019(3) -0.020(4) -0.011(3) C39C 0.123(4) 0.085(4) 0.103(4) 0.017(4) -0.023(4) -0.009(4) Br1C 0.148(5) 0.113(5) 0.102(3) 0.022(3) -0.053(3) 0.013(3) O2 0.0690(12) 0.0927(15) 0.1039(17) 0.0229(11) -0.0103(11) -0.0164(12) O3 0.1092(15) 0.0611(12) 0.0851(14) -0.0004(10) 0.0072(12) 0.0008(10) O4 0.0700(12) 0.0691(13) 0.1262(19) 0.0058(10) 0.0201(12) 0.0198(12) O5 0.0907(15) 0.0946(15) 0.0968(16) -0.0027(12) 0.0002(12) -0.0255(13) O6 0.0884(14) 0.0832(15) 0.1061(17) -0.0238(12) -0.0066(12) -0.0036(12) O7 0.0955(16) 0.141(2) 0.0710(14) 0.0204(15) 0.0009(12) -0.0235(14) O8 0.1018(15) 0.0726(12) 0.0727(13) 0.0003(11) -0.0176(11) -0.0014(10) O9 0.0733(12) 0.0696(12) 0.0897(14) 0.0030(9) 0.0211(10) -0.0075(10) O10 0.0774(12) 0.0824(14) 0.0948(15) -0.0006(10) 0.0237(11) -0.0218(11) C1 0.0551(14) 0.0694(16) 0.0494(14) -0.0076(12) 0.0076(11) 0.0051(12) C3 0.0643(15) 0.0651(16) 0.0629(16) -0.0047(13) 0.0007(13) 0.0001(13) C4 0.0454(13) 0.0715(16) 0.0581(15) -0.0034(12) 0.0077(11) 0.0081(13) C5 0.0508(14) 0.0729(17) 0.0665(17) 0.0039(13) 0.0069(12) 0.0012(14) C6 0.0573(15) 0.0718(17) 0.0610(16) 0.0002(13) 0.0069(12) -0.0058(13) C7 0.0496(14) 0.0774(17) 0.0704(18) -0.0031(12) 0.0053(12) 0.0044(14) C8 0.0400(12) 0.0714(17) 0.0624(16) -0.0043(11) -0.0034(11) 0.0002(14) C9 0.0616(15) 0.0580(16) 0.0663(17) -0.0066(12) -0.0073(13) -0.0001(13) C10 0.0618(15) 0.0700(17) 0.0624(17) -0.0061(13) -0.0054(13) -0.0094(14) C11 0.0485(13) 0.0697(17) 0.0601(16) -0.0111(12) -0.0063(12) 0.0016(13) C12 0.0450(13) 0.0616(16) 0.0791(19) -0.0024(11) 0.0008(13) 0.0053(14) C13 0.0472(13) 0.0686(17) 0.0724(18) 0.0005(12) 0.0038(12) -0.0025(14) C14 0.0646(16) 0.0861(19) 0.0617(17) -0.0132(14) -0.0078(13) 0.0032(15) C15 0.0644(16) 0.0801(18) 0.0483(15) -0.0102(14) -0.0015(12) 0.0078(13) C16 0.0712(18) 0.086(2) 0.0543(16) -0.0078(15) -0.0018(13) -0.0027(14) C17 0.0666(17) 0.110(2) 0.0503(16) 0.0020(17) 0.0033(13) 0.0023(16) C18 0.0655(17) 0.098(2) 0.0485(15) -0.0183(16) -0.0021(13) 0.0108(15) C19 0.0722(18) 0.0805(19) 0.0568(16) -0.0163(15) -0.0040(14) 0.0104(14) C20 0.0636(16) 0.0759(18) 0.0640(17) -0.0056(14) 0.0000(13) 0.0058(14) C21 0.0647(17) 0.130(3) 0.0598(17) -0.0223(17) -0.0010(13) 0.0135(18) C22 0.0491(14) 0.108(2) 0.0584(17) -0.0166(15) 0.0036(12) 0.0102(17) C23 0.0547(15) 0.111(2) 0.0580(18) -0.0107(16) 0.0094(13) -0.0128(17) C24 0.0519(14) 0.095(2) 0.0634(17) -0.0009(14) 0.0040(13) 0.0011(16) C25 0.0464(13) 0.0799(18) 0.0583(16) -0.0140(13) 0.0032(11) 0.0018(14) C26 0.0556(14) 0.0728(18) 0.0663(18) -0.0140(13) -0.0019(13) 0.0073(15) C27 0.0619(16) 0.0845(19) 0.0682(19) -0.0200(14) -0.0092(14) 0.0146(16) C28 0.0508(13) 0.0718(16) 0.0614(16) -0.0066(12) -0.0047(12) 0.0032(13) C29 0.0482(13) 0.0664(16) 0.0521(14) -0.0036(11) -0.0063(11) 0.0032(12) C30 0.0499(13) 0.0699(16) 0.0520(14) 0.0049(12) 0.0030(11) -0.0019(12) C31 0.0593(14) 0.0590(14) 0.0551(15) 0.0004(12) -0.0049(12) 0.0047(12) C32 0.0506(13) 0.0736(17) 0.0443(13) 0.0004(12) -0.0025(11) 0.0030(12) C33 0.0542(14) 0.0698(17) 0.0587(16) 0.0036(13) 0.0011(12) -0.0059(13) C34 0.0557(14) 0.0658(15) 0.0615(16) -0.0020(13) -0.0012(13) -0.0059(13) C35 0.0570(14) 0.0820(18) 0.0525(15) -0.0044(13) 0.0008(12) 0.0070(13) C40 0.166(4) 0.063(2) 0.123(3) 0.001(2) 0.020(3) -0.016(2) C41 0.083(2) 0.091(3) 0.133(4) 0.030(2) 0.026(2) 0.026(2) C41A 0.083(2) 0.091(3) 0.133(4) 0.030(2) 0.026(2) 0.026(2) C42 0.119(3) 0.110(3) 0.122(3) 0.028(2) -0.009(2) -0.035(2) C43 0.119(3) 0.080(2) 0.181(4) -0.003(2) -0.007(3) -0.018(3) C44 0.112(3) 0.166(4) 0.094(3) 0.038(3) 0.002(2) -0.055(3) C45 0.111(3) 0.079(2) 0.095(2) 0.0090(18) -0.018(2) 0.0075(18) C46 0.087(2) 0.082(2) 0.124(3) 0.0067(17) 0.025(2) -0.022(2) C47 0.114(3) 0.084(2) 0.134(3) 0.005(2) 0.028(2) -0.031(2) N1 0.168(7) 0.123(5) 0.169(8) 0.028(5) 0.016(7) -0.022(6) C48 0.122(4) 0.120(4) 0.134(5) 0.014(4) -0.001(4) -0.015(4) C49 0.121(4) 0.122(4) 0.119(4) -0.009(3) 0.024(3) 0.001(3) C50 0.099(3) 0.106(3) 0.112(4) -0.009(3) 0.013(3) -0.008(3) C51 0.099(3) 0.109(4) 0.111(4) -0.009(3) 0.011(3) -0.012(3) C52 0.126(4) 0.110(3) 0.137(5) -0.015(3) 0.029(4) -0.012(4) C53 0.120(4) 0.107(4) 0.133(6) -0.010(4) 0.011(5) -0.026(4) N2 0.128(8) 0.106(5) 0.171(7) -0.005(5) 0.017(6) -0.030(6) N1B 0.155(9) 0.135(8) 0.135(9) 0.023(7) 0.017(8) -0.022(6) C48B 0.126(5) 0.120(5) 0.133(5) 0.008(5) 0.001(5) -0.015(5) C49B 0.122(4) 0.125(5) 0.126(5) 0.004(4) -0.003(5) -0.006(4) C50B 0.103(4) 0.108(4) 0.116(5) -0.005(4) 0.008(5) -0.009(4) C51B 0.102(4) 0.108(4) 0.119(5) -0.009(4) 0.015(4) -0.012(4) C52B 0.120(4) 0.115(4) 0.121(5) -0.004(4) 0.003(5) -0.015(4) C53B 0.120(5) 0.109(5) 0.137(6) -0.009(5) 0.008(6) -0.029(4) N2B 0.128(10) 0.106(8) 0.142(8) -0.011(8) 0.004(8) -0.028(6) 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' O O 0.0106 0.0060 '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' 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 C2 O1A C36A . . 119.1(3) ? O1A C36A C37A . . 108.3(3) ? O1A C36A H36A . . 110.0 ? C37A C36A H36A . . 110.0 ? O1A C36A H36B . . 110.0 ? C37A C36A H36B . . 110.0 ? H36A C36A H36B . . 108.4 ? C38A C37A C36A . . 113.5(4) ? C38A C37A H37A . . 108.9 ? C36A C37A H37A . . 108.9 ? C38A C37A H37B . . 108.9 ? C36A C37A H37B . . 108.9 ? H37A C37A H37B . . 107.7 ? C37A C38A C39A . . 112.7(4) ? C37A C38A H38A . . 109.1 ? C39A C38A H38A . . 109.1 ? C37A C38A H38B . . 109.1 ? C39A C38A H38B . . 109.1 ? H38A C38A H38B . . 107.8 ? C38A C39A Br1A . . 110.0(3) ? C38A C39A H39C . . 109.5 ? Br1A C39A H39C . . 0.9 ? C38A C39A H39D . . 109.5 ? Br1A C39A H39D . . 108.6 ? H39C C39A H39D . . 109.5 ? C38A C39A H39E . . 109.5 ? Br1A C39A H39E . . 109.8 ? H39C C39A H39E . . 109.5 ? H39D C39A H39E . . 109.5 ? C38A C39A H39A . . 109.7 ? Br1A C39A H39A . . 109.7 ? H39C C39A H39A . . 109.3 ? H39D C39A H39A . . 109.4 ? H39E C39A H39A . . 0.2 ? C38A C39A H39B . . 109.7 ? Br1A C39A H39B . . 109.7 ? H39C C39A H39B . . 110.6 ? H39D C39A H39B . . 1.4 ? H39E C39A H39B . . 108.2 ? H39A C39A H39B . . 108.2 ? O1B C2 C1 . . 119.4(5) ? O1A C2 C1 . . 116.4(2) ? O1C C2 C1 . . 118.5(5) ? O1B C2 C3 . . 119.9(5) ? O1A C2 C3 . . 122.8(3) ? O1C C2 C3 . . 119.2(5) ? C1 C2 C3 . . 120.8(2) ? C2 O1B C36B . . 116(3) ? O1B C36B C37B . . 108.6(17) ? O1B C36B H36C . . 110.0 ? C37B C36B H36C . . 110.0 ? O1B C36B H36D . . 110.0 ? C37B C36B H36D . . 110.0 ? H36C C36B H36D . . 108.3 ? C38B C37B C36B . . 111.8(8) ? C38B C37B H37C . . 109.3 ? C36B C37B H37C . . 109.3 ? C38B C37B H37D . . 109.3 ? C36B C37B H37D . . 109.3 ? H37C C37B H37D . . 107.9 ? C37B C38B C39B . . 111.9(8) ? C37B C38B H38C . . 109.2 ? C39B C38B H38C . . 109.2 ? C37B C38B H38D . . 109.2 ? C39B C38B H38D . . 109.2 ? H38C C38B H38D . . 107.9 ? C38B C39B Br1B . . 124.6(15) ? C38B C39B H39F . . 106.2 ? Br1B C39B H39F . . 106.2 ? C38B C39B H39G . . 106.2 ? Br1B C39B H39G . . 106.2 ? H39F C39B H39G . . 106.4 ? C2 O1C C36C . . 119.6(10) ? O1C C36C C37C . . 107.4(13) ? O1C C36C H36G . . 110.2 ? C37C C36C H36G . . 110.2 ? O1C C36C H36H . . 110.2 ? C37C C36C H36H . . 110.2 ? H36G C36C H36H . . 108.5 ? C38C C37C C36C . . 119.3(15) ? C38C C37C H37E . . 107.5 ? C36C C37C H37E . . 107.5 ? C38C C37C H37F . . 107.5 ? C36C C37C H37F . . 107.5 ? H37E C37C H37F . . 107.0 ? C37C C38C C39C . . 121.1(15) ? C37C C38C H38E . . 107.1 ? C39C C38C H38E . . 107.1 ? C37C C38C H38F . . 107.1 ? C39C C38C H38F . . 107.1 ? H38E C38C H38F . . 106.8 ? C38C C39C Br1C . . 118.4(14) ? C38C C39C H39H . . 107.7 ? Br1C C39C H39H . . 107.7 ? C38C C39C H39I . . 107.7 ? Br1C C39C H39I . . 107.7 ? H39H C39C H39I . . 107.1 ? C5 O2 H2 . . 110(3) ? C9 O3 C40 . . 117.9(3) ? C41A O4 C12 . . 118.7(13) ? C12 O4 C41 . . 116.1(2) ? C16 O5 C42 . . 118.4(3) ? C19 O6 C43 . . 118.5(2) ? C23 O7 C44 . . 117.8(3) ? C26 O8 C45 . . 118.5(2) ? C30 O9 C46 . . 118.4(2) ? C33 O10 C47 . . 118.4(2) ? C6 C1 C2 . . 117.8(2) ? C6 C1 C35 . . 120.7(2) ? C2 C1 C35 . . 121.4(2) ? C2 C3 C4 . . 121.2(2) ? C2 C3 H3 . . 119.4 ? C4 C3 H3 . . 119.4 ? C5 C4 C3 . . 117.7(2) ? C5 C4 C7 . . 121.5(2) ? C3 C4 C7 . . 120.8(2) ? O2 C5 C4 . . 118.1(2) ? O2 C5 C6 . . 121.2(2) ? C4 C5 C6 . . 120.7(2) ? C1 C6 C5 . . 121.8(2) ? C1 C6 H6 . . 119.1 ? C5 C6 H6 . . 119.1 ? C4 C7 C8 . . 112.4(2) ? C4 C7 H7A . . 109.1 ? C8 C7 H7A . . 109.1 ? C4 C7 H7B . . 109.1 ? C8 C7 H7B . . 109.1 ? H7A C7 H7B . . 107.8 ? C13 C8 C9 . . 117.4(2) ? C13 C8 C7 . . 121.0(2) ? C9 C8 C7 . . 121.6(2) ? O3 C9 C10 . . 123.8(2) ? O3 C9 C8 . . 115.4(2) ? C10 C9 C8 . . 120.8(2) ? C9 C10 C11 . . 121.0(3) ? C9 C10 H10 . . 119.5 ? C11 C10 H10 . . 119.5 ? C12 C11 C10 . . 118.0(2) ? C12 C11 C14 . . 121.4(2) ? C10 C11 C14 . . 120.5(3) ? C13 C12 C11 . . 120.6(2) ? C13 C12 O4 . . 120.2(3) ? C11 C12 O4 . . 119.1(2) ? C12 C13 C8 . . 122.0(3) ? C12 C13 H13 . . 119.0 ? C8 C13 H13 . . 119.0 ? C11 C14 C15 . . 113.0(2) ? C11 C14 H14A . . 109.0 ? C15 C14 H14A . . 109.0 ? C11 C14 H14B . . 109.0 ? C15 C14 H14B . . 109.0 ? H14A C14 H14B . . 107.8 ? C20 C15 C16 . . 118.5(2) ? C20 C15 C14 . . 120.2(3) ? C16 C15 C14 . . 121.2(3) ? O5 C16 C15 . . 116.2(2) ? O5 C16 C17 . . 124.1(3) ? C15 C16 C17 . . 119.6(3) ? C18 C17 C16 . . 121.5(3) ? C18 C17 H17 . . 119.3 ? C16 C17 H17 . . 119.3 ? C17 C18 C19 . . 118.6(3) ? C17 C18 C21 . . 120.2(3) ? C19 C18 C21 . . 121.1(3) ? O6 C19 C20 . . 123.6(3) ? O6 C19 C18 . . 116.4(2) ? C20 C19 C18 . . 120.0(3) ? C15 C20 C19 . . 121.7(3) ? C15 C20 H20 . . 119.1 ? C19 C20 H20 . . 119.1 ? C22 C21 C18 . . 110.6(2) ? C22 C21 H21A . . 109.5 ? C18 C21 H21A . . 109.5 ? C22 C21 H21B . . 109.5 ? C18 C21 H21B . . 109.5 ? H21A C21 H21B . . 108.1 ? C27 C22 C23 . . 118.6(3) ? C27 C22 C21 . . 121.0(3) ? C23 C22 C21 . . 120.4(3) ? O7 C23 C24 . . 123.8(3) ? O7 C23 C22 . . 116.0(3) ? C24 C23 C22 . . 120.2(3) ? C25 C24 C23 . . 121.2(3) ? C25 C24 H24 . . 119.4 ? C23 C24 H24 . . 119.4 ? C24 C25 C26 . . 119.0(2) ? C24 C25 C28 . . 120.2(2) ? C26 C25 C28 . . 120.8(2) ? O8 C26 C25 . . 116.9(2) ? O8 C26 C27 . . 123.6(3) ? C25 C26 C27 . . 119.5(3) ? C22 C27 C26 . . 121.5(3) ? C22 C27 H27 . . 119.3 ? C26 C27 H27 . . 119.3 ? C25 C28 C29 . . 112.13(19) ? C25 C28 H28A . . 109.2 ? C29 C28 H28A . . 109.2 ? C25 C28 H28B . . 109.2 ? C29 C28 H28B . . 109.2 ? H28A C28 H28B . . 107.9 ? C34 C29 C30 . . 118.0(2) ? C34 C29 C28 . . 120.2(2) ? C30 C29 C28 . . 121.8(2) ? O9 C30 C29 . . 116.1(2) ? O9 C30 C31 . . 123.2(2) ? C29 C30 C31 . . 120.7(2) ? C30 C31 C32 . . 121.0(2) ? C30 C31 H31 . . 119.5 ? C32 C31 H31 . . 119.5 ? C33 C32 C31 . . 118.4(2) ? C33 C32 C35 . . 122.2(2) ? C31 C32 C35 . . 119.4(2) ? O10 C33 C32 . . 116.5(2) ? O10 C33 C34 . . 123.2(2) ? C32 C33 C34 . . 120.4(2) ? C33 C34 C29 . . 121.6(2) ? C33 C34 H34 . . 119.2 ? C29 C34 H34 . . 119.2 ? C1 C35 C32 . . 111.1(2) ? C1 C35 H35A . . 109.4 ? C32 C35 H35A . . 109.4 ? C1 C35 H35B . . 109.4 ? C32 C35 H35B . . 109.4 ? H35A C35 H35B . . 108.0 ? O3 C40 H40A . . 109.5 ? O3 C40 H40B . . 109.5 ? H40A C40 H40B . . 109.5 ? O3 C40 H40C . . 109.5 ? H40A C40 H40C . . 109.5 ? H40B C40 H40C . . 109.5 ? O4 C41 H41A . . 109.5 ? O4 C41 H41B . . 109.5 ? H41A C41 H41B . . 109.5 ? O4 C41 H41C . . 109.5 ? H41A C41 H41C . . 109.5 ? H41B C41 H41C . . 109.5 ? O4 C41A H41D . . 109.5 ? O4 C41A H41E . . 109.5 ? H41D C41A H41E . . 109.5 ? O4 C41A H41F . . 109.5 ? H41D C41A H41F . . 109.5 ? H41E C41A H41F . . 109.5 ? O5 C42 H42A . . 109.5 ? O5 C42 H42B . . 109.5 ? H42A C42 H42B . . 109.5 ? O5 C42 H42C . . 109.5 ? H42A C42 H42C . . 109.5 ? H42B C42 H42C . . 109.5 ? O6 C43 H43A . . 109.5 ? O6 C43 H43B . . 109.5 ? H43A C43 H43B . . 109.5 ? O6 C43 H43C . . 109.5 ? H43A C43 H43C . . 109.5 ? H43B C43 H43C . . 109.5 ? O7 C44 H44A . . 109.5 ? O7 C44 H44B . . 109.5 ? H44A C44 H44B . . 109.5 ? O7 C44 H44C . . 109.5 ? H44A C44 H44C . . 109.5 ? H44B C44 H44C . . 109.5 ? O8 C45 H45A . . 109.5 ? O8 C45 H45B . . 109.5 ? H45A C45 H45B . . 109.5 ? O8 C45 H45C . . 109.5 ? H45A C45 H45C . . 109.5 ? H45B C45 H45C . . 109.5 ? O9 C46 H46A . . 109.5 ? O9 C46 H46B . . 109.5 ? H46A C46 H46B . . 109.5 ? O9 C46 H46C . . 109.5 ? H46A C46 H46C . . 109.5 ? H46B C46 H46C . . 109.5 ? O10 C47 H47A . . 109.5 ? O10 C47 H47B . . 109.5 ? H47A C47 H47B . . 109.5 ? O10 C47 H47C . . 109.5 ? H47A C47 H47C . . 109.5 ? H47B C47 H47C . . 109.5 ? N1 C48 C49 . . 174.1(15) ? C48 C49 C50 . . 112.6(7) ? C48 C49 H49A . . 109.1 ? C50 C49 H49A . . 109.1 ? C48 C49 H49B . . 109.1 ? C50 C49 H49B . . 109.1 ? H49A C49 H49B . . 107.8 ? C49 C50 C51 . . 106.9(6) ? C49 C50 H50A . . 110.3 ? C51 C50 H50A . . 110.3 ? C49 C50 H50B . . 110.3 ? C51 C50 H50B . . 110.3 ? H50A C50 H50B . . 108.6 ? C52 C51 C50 . . 108.3(6) ? C52 C51 H51A . . 110.0 ? C50 C51 H51A . . 110.0 ? C52 C51 H51B . . 110.0 ? C50 C51 H51B . . 110.0 ? H51A C51 H51B . . 108.4 ? C53 C52 C51 . . 111.5(7) ? C53 C52 H52A . . 109.3 ? C51 C52 H52A . . 109.3 ? C53 C52 H52B . . 109.3 ? C51 C52 H52B . . 109.3 ? H52A C52 H52B . . 108.0 ? N2 C53 C52 . . 174.5(14) ? N1B C48B C49B . . 168(3) ? C50B C49B C48B . . 112.7(12) ? C50B C49B H49C . . 109.0 ? C48B C49B H49C . . 109.0 ? C50B C49B H49D . . 109.0 ? C48B C49B H49D . . 109.0 ? H49C C49B H49D . . 107.8 ? C49B C50B C51B . . 107.2(9) ? C49B C50B H50C . . 110.3 ? C51B C50B H50C . . 110.3 ? C49B C50B H50D . . 110.3 ? C51B C50B H50D . . 110.3 ? H50C C50B H50D . . 108.5 ? C52B C51B C50B . . 108.5(10) ? C52B C51B H51C . . 110.0 ? C50B C51B H51C . . 110.0 ? C52B C51B H51D . . 110.0 ? C50B C51B H51D . . 110.0 ? H51C C51B H51D . . 108.4 ? C51B C52B C53B . . 111.0(10) ? C51B C52B H52C . . 109.4 ? C53B C52B H52C . . 109.4 ? C51B C52B H52D . . 109.4 ? C53B C52B H52D . . 109.4 ? H52C C52B H52D . . 108.0 ? N2B C53B C52B . . 171(2) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1A C2 . 1.377(3) ? O1A C36A . 1.419(5) ? C36A C37A . 1.527(4) ? C36A H36A . 0.9900 ? C36A H36B . 0.9900 ? C37A C38A . 1.486(4) ? C37A H37A . 0.9900 ? C37A H37B . 0.9900 ? C38A C39A . 1.521(4) ? C38A H38A . 0.9900 ? C38A H38B . 0.9900 ? C39A Br1A . 1.956(5) ? C39A H39C . 0.9800 ? C39A H39D . 0.9800 ? C39A H39E . 0.9800 ? C39A H39A . 0.9900 ? C39A H39B . 0.9900 ? C2 O1B . 1.377(6) ? C2 O1C . 1.383(7) ? C2 C1 . 1.395(4) ? C2 C3 . 1.395(3) ? O1B C36B . 1.42(2) ? C36B C37B . 1.526(6) ? C36B H36C . 0.9900 ? C36B H36D . 0.9900 ? C37B C38B . 1.520(6) ? C37B H37C . 0.9900 ? C37B H37D . 0.9900 ? C38B C39B . 1.524(6) ? C38B H38C . 0.9900 ? C38B H38D . 0.9900 ? C39B Br1B . 1.868(18) ? C39B H39F . 0.9900 ? C39B H39G . 0.9900 ? O1C C36C . 1.418(17) ? C36C C37C . 1.544(9) ? C36C H36G . 0.9900 ? C36C H36H . 0.9900 ? C37C C38C . 1.520(9) ? C37C H37E . 0.9900 ? C37C H37F . 0.9900 ? C38C C39C . 1.546(9) ? C38C H38E . 0.9900 ? C38C H38F . 0.9900 ? C39C Br1C . 1.766(16) ? C39C H39H . 0.9900 ? C39C H39I . 0.9900 ? O2 C5 . 1.372(3) ? O2 H2 . 0.89(4) ? O3 C9 . 1.378(3) ? O3 C40 . 1.419(4) ? O4 C41A . 1.382(10) ? O4 C12 . 1.390(3) ? O4 C41 . 1.392(4) ? O5 C16 . 1.378(3) ? O5 C42 . 1.408(4) ? O6 C19 . 1.374(3) ? O6 C43 . 1.419(4) ? O7 C23 . 1.372(3) ? O7 C44 . 1.410(5) ? O8 C26 . 1.372(3) ? O8 C45 . 1.414(3) ? O9 C30 . 1.380(3) ? O9 C46 . 1.402(3) ? O10 C33 . 1.381(3) ? O10 C47 . 1.406(4) ? C1 C6 . 1.379(3) ? C1 C35 . 1.517(3) ? C3 C4 . 1.399(3) ? C3 H3 . 0.9500 ? C4 C5 . 1.386(4) ? C4 C7 . 1.515(3) ? C5 C6 . 1.399(4) ? C6 H6 . 0.9500 ? C7 C8 . 1.523(4) ? C7 H7A . 0.9900 ? C7 H7B . 0.9900 ? C8 C13 . 1.383(3) ? C8 C9 . 1.395(4) ? C9 C10 . 1.388(4) ? C10 C11 . 1.391(4) ? C10 H10 . 0.9500 ? C11 C12 . 1.387(4) ? C11 C14 . 1.516(4) ? C12 C13 . 1.380(4) ? C13 H13 . 0.9500 ? C14 C15 . 1.520(4) ? C14 H14A . 0.9900 ? C14 H14B . 0.9900 ? C15 C20 . 1.384(4) ? C15 C16 . 1.391(4) ? C16 C17 . 1.400(4) ? C17 C18 . 1.378(4) ? C17 H17 . 0.9500 ? C18 C19 . 1.389(4) ? C18 C21 . 1.529(4) ? C19 C20 . 1.386(4) ? C20 H20 . 0.9500 ? C21 C22 . 1.516(4) ? C21 H21A . 0.9900 ? C21 H21B . 0.9900 ? C22 C27 . 1.379(4) ? C22 C23 . 1.394(4) ? C23 C24 . 1.393(4) ? C24 C25 . 1.384(4) ? C24 H24 . 0.9500 ? C25 C26 . 1.394(4) ? C25 C28 . 1.517(4) ? C26 C27 . 1.403(4) ? C27 H27 . 0.9500 ? C28 C29 . 1.521(3) ? C28 H28A . 0.9900 ? C28 H28B . 0.9900 ? C29 C34 . 1.388(3) ? C29 C30 . 1.389(3) ? C30 C31 . 1.390(3) ? C31 C32 . 1.393(3) ? C31 H31 . 0.9500 ? C32 C33 . 1.384(4) ? C32 C35 . 1.522(3) ? C33 C34 . 1.386(4) ? C34 H34 . 0.9500 ? C35 H35A . 0.9900 ? C35 H35B . 0.9900 ? C40 H40A . 0.9800 ? C40 H40B . 0.9800 ? C40 H40C . 0.9800 ? C41 H41A . 0.9800 ? C41 H41B . 0.9800 ? C41 H41C . 0.9800 ? C41A H41D . 0.9800 ? C41A H41E . 0.9800 ? C41A H41F . 0.9800 ? C42 H42A . 0.9800 ? C42 H42B . 0.9800 ? C42 H42C . 0.9800 ? C43 H43A . 0.9800 ? C43 H43B . 0.9800 ? C43 H43C . 0.9800 ? C44 H44A . 0.9800 ? C44 H44B . 0.9800 ? C44 H44C . 0.9800 ? C45 H45A . 0.9800 ? C45 H45B . 0.9800 ? C45 H45C . 0.9800 ? C46 H46A . 0.9800 ? C46 H46B . 0.9800 ? C46 H46C . 0.9800 ? C47 H47A . 0.9800 ? C47 H47B . 0.9800 ? C47 H47C . 0.9800 ? N1 C48 . 1.160(6) ? C48 C49 . 1.469(6) ? C49 C50 . 1.481(6) ? C49 H49A . 0.9900 ? C49 H49B . 0.9900 ? C50 C51 . 1.564(6) ? C50 H50A . 0.9900 ? C50 H50B . 0.9900 ? C51 C52 . 1.476(6) ? C51 H51A . 0.9900 ? C51 H51B . 0.9900 ? C52 C53 . 1.469(5) ? C52 H52A . 0.9900 ? C52 H52B . 0.9900 ? C53 N2 . 1.165(6) ? N1B C48B . 1.161(7) ? C48B C49B . 1.472(6) ? C49B C50B . 1.460(9) ? C49B H49C . 0.9900 ? C49B H49D . 0.9900 ? C50B C51B . 1.572(10) ? C50B H50C . 0.9900 ? C50B H50D . 0.9900 ? C51B C52B . 1.458(10) ? C51B H51C . 0.9900 ? C51B H51D . 0.9900 ? C52B C53B . 1.478(6) ? C52B H52C . 0.9900 ? C52B H52D . 0.9900 ? C53B N2B . 1.165(7) ? 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 C37A H37A O6 2_646 0.99 2.60 3.587(5) 171.5 yes O2 H2 N2 3_667 0.89(4) 1.98(4) 2.866(10) 178(4) yes O2 H2 N2B 3_667 0.89(4) 2.11(4) 2.980(14) 168(4) yes C20 H20 O4 . 0.95 2.51 3.171(3) 127.1 yes C27 H27 O6 . 0.95 2.66 3.186(3) 115.8 yes C40 H40B N1 . 0.98 2.67 3.535(16) 147.9 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 C2 O1A C36A C37A . . . . 173.6(4) ? O1A C36A C37A C38A . . . . 77.7(5) ? C36A C37A C38A C39A . . . . 178.6(3) ? C37A C38A C39A Br1A . . . . -179.2(3) ? C36A O1A C2 C1 . . . . -156.6(4) ? C36A O1A C2 C3 . . . . 21.6(7) ? C1 C2 O1B C36B . . . . 118(3) ? C3 C2 O1B C36B . . . . -62(4) ? C2 O1B C36B C37B . . . . -172(3) ? O1B C36B C37B C38B . . . . 157(4) ? C36B C37B C38B C39B . . . . 170(4) ? C37B C38B C39B Br1B . . . . 18(7) ? C1 C2 O1C C36C . . . . 159(2) ? C3 C2 O1C C36C . . . . -7(4) ? C2 O1C C36C C37C . . . . 177(3) ? O1C C36C C37C C38C . . . . 144(3) ? C36C C37C C38C C39C . . . . 169(2) ? C37C C38C C39C Br1C . . . . 48(3) ? O1B C2 C1 C6 . . . . -178(2) ? O1A C2 C1 C6 . . . . 179.6(4) ? O1C C2 C1 C6 . . . . -164.5(19) ? C3 C2 C1 C6 . . . . 1.4(4) ? O1B C2 C1 C35 . . . . 5(2) ? O1A C2 C1 C35 . . . . 2.4(5) ? O1C C2 C1 C35 . . . . 18.3(19) ? C3 C2 C1 C35 . . . . -175.8(2) ? O1B C2 C3 C4 . . . . 180(2) ? O1A C2 C3 C4 . . . . -178.0(4) ? O1C C2 C3 C4 . . . . 165.9(19) ? C1 C2 C3 C4 . . . . 0.1(4) ? C2 C3 C4 C5 . . . . -1.0(4) ? C2 C3 C4 C7 . . . . 177.9(2) ? C3 C4 C5 O2 . . . . -179.6(2) ? C7 C4 C5 O2 . . . . 1.6(4) ? C3 C4 C5 C6 . . . . 0.4(4) ? C7 C4 C5 C6 . . . . -178.5(2) ? C2 C1 C6 C5 . . . . -2.0(4) ? C35 C1 C6 C5 . . . . 175.2(2) ? O2 C5 C6 C1 . . . . -178.9(2) ? C4 C5 C6 C1 . . . . 1.1(4) ? C5 C4 C7 C8 . . . . 90.5(3) ? C3 C4 C7 C8 . . . . -88.3(3) ? C4 C7 C8 C13 . . . . -88.3(3) ? C4 C7 C8 C9 . . . . 89.8(3) ? C40 O3 C9 C10 . . . . -1.1(4) ? C40 O3 C9 C8 . . . . 178.9(3) ? C13 C8 C9 O3 . . . . -179.4(2) ? C7 C8 C9 O3 . . . . 2.4(3) ? C13 C8 C9 C10 . . . . 0.6(3) ? C7 C8 C9 C10 . . . . -177.6(2) ? O3 C9 C10 C11 . . . . 179.9(2) ? C8 C9 C10 C11 . . . . -0.2(4) ? C9 C10 C11 C12 . . . . -0.3(4) ? C9 C10 C11 C14 . . . . 178.4(2) ? C10 C11 C12 C13 . . . . 0.3(3) ? C14 C11 C12 C13 . . . . -178.4(2) ? C10 C11 C12 O4 . . . . 177.9(2) ? C14 C11 C12 O4 . . . . -0.8(3) ? C41A O4 C12 C13 . . . . -2(2) ? C41 O4 C12 C13 . . . . -72.5(4) ? C41A O4 C12 C11 . . . . -180(2) ? C41 O4 C12 C11 . . . . 109.8(3) ? C11 C12 C13 C8 . . . . 0.2(4) ? O4 C12 C13 C8 . . . . -177.4(2) ? C9 C8 C13 C12 . . . . -0.7(3) ? C7 C8 C13 C12 . . . . 177.6(2) ? C12 C11 C14 C15 . . . . 84.9(3) ? C10 C11 C14 C15 . . . . -93.7(3) ? C11 C14 C15 C20 . . . . -81.1(3) ? C11 C14 C15 C16 . . . . 96.4(3) ? C42 O5 C16 C15 . . . . 177.3(3) ? C42 O5 C16 C17 . . . . -2.6(4) ? C20 C15 C16 O5 . . . . -179.9(2) ? C14 C15 C16 O5 . . . . 2.6(4) ? C20 C15 C16 C17 . . . . 0.0(4) ? C14 C15 C16 C17 . . . . -177.5(2) ? O5 C16 C17 C18 . . . . -178.4(3) ? C15 C16 C17 C18 . . . . 1.6(4) ? C16 C17 C18 C19 . . . . -2.0(4) ? C16 C17 C18 C21 . . . . 176.4(3) ? C43 O6 C19 C20 . . . . -0.5(4) ? C43 O6 C19 C18 . . . . 179.7(3) ? C17 C18 C19 O6 . . . . -179.3(2) ? C21 C18 C19 O6 . . . . 2.3(4) ? C17 C18 C19 C20 . . . . 0.9(4) ? C21 C18 C19 C20 . . . . -177.5(2) ? C16 C15 C20 C19 . . . . -1.2(4) ? C14 C15 C20 C19 . . . . 176.4(2) ? O6 C19 C20 C15 . . . . -179.1(2) ? C18 C19 C20 C15 . . . . 0.7(4) ? C17 C18 C21 C22 . . . . -95.5(3) ? C19 C18 C21 C22 . . . . 82.9(4) ? C18 C21 C22 C27 . . . . -92.7(3) ? C18 C21 C22 C23 . . . . 85.5(3) ? C44 O7 C23 C24 . . . . 2.5(4) ? C44 O7 C23 C22 . . . . -178.1(3) ? C27 C22 C23 O7 . . . . 179.7(2) ? C21 C22 C23 O7 . . . . 1.4(4) ? C27 C22 C23 C24 . . . . -1.0(4) ? C21 C22 C23 C24 . . . . -179.2(2) ? O7 C23 C24 C25 . . . . -178.1(2) ? C22 C23 C24 C25 . . . . 2.6(4) ? C23 C24 C25 C26 . . . . -1.6(4) ? C23 C24 C25 C28 . . . . 177.4(2) ? C45 O8 C26 C25 . . . . -179.1(2) ? C45 O8 C26 C27 . . . . 0.1(4) ? C24 C25 C26 O8 . . . . 178.4(2) ? C28 C25 C26 O8 . . . . -0.7(3) ? C24 C25 C26 C27 . . . . -0.9(4) ? C28 C25 C26 C27 . . . . -179.9(2) ? C23 C22 C27 C26 . . . . -1.6(4) ? C21 C22 C27 C26 . . . . 176.6(2) ? O8 C26 C27 C22 . . . . -176.7(2) ? C25 C26 C27 C22 . . . . 2.5(4) ? C24 C25 C28 C29 . . . . -86.0(3) ? C26 C25 C28 C29 . . . . 93.1(3) ? C25 C28 C29 C34 . . . . -96.5(3) ? C25 C28 C29 C30 . . . . 83.0(3) ? C46 O9 C30 C29 . . . . 179.1(3) ? C46 O9 C30 C31 . . . . -0.8(4) ? C34 C29 C30 O9 . . . . -179.4(2) ? C28 C29 C30 O9 . . . . 1.1(3) ? C34 C29 C30 C31 . . . . 0.6(3) ? C28 C29 C30 C31 . . . . -178.9(2) ? O9 C30 C31 C32 . . . . 179.5(2) ? C29 C30 C31 C32 . . . . -0.5(4) ? C30 C31 C32 C33 . . . . -0.3(3) ? C30 C31 C32 C35 . . . . 178.4(2) ? C47 O10 C33 C32 . . . . 176.2(3) ? C47 O10 C33 C34 . . . . -4.6(4) ? C31 C32 C33 O10 . . . . -179.8(2) ? C35 C32 C33 O10 . . . . 1.5(3) ? C31 C32 C33 C34 . . . . 1.0(4) ? C35 C32 C33 C34 . . . . -177.7(2) ? O10 C33 C34 C29 . . . . 180.0(2) ? C32 C33 C34 C29 . . . . -0.9(4) ? C30 C29 C34 C33 . . . . 0.1(4) ? C28 C29 C34 C33 . . . . 179.6(2) ? C6 C1 C35 C32 . . . . -85.2(3) ? C2 C1 C35 C32 . . . . 91.9(3) ? C33 C32 C35 C1 . . . . 94.0(3) ? C31 C32 C35 C1 . . . . -84.6(3) ? C48 C49 C50 C51 . . . . -178.9(10) ? C49 C50 C51 C52 . . . . 179.2(8) ? C50 C51 C52 C53 . . . . 173.2(9) ? N1B C48B C49B C50B . . . . 88(16) ? C48B C49B C50B C51B . . . . 177.6(17) ? C49B C50B C51B C52B . . . . -173.5(14) ? C50B C51B C52B C53B . . . . -170.6(16) ?