#------------------------------------------------------------------------------ #$Date: 2024-10-25 05:04:23 +0300 (Fri, 25 Oct 2024) $ #$Revision: 295627 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/29/1572955.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1572955 loop_ _publ_author_name 'Vinodh, Mickey' 'Alipour, Fatemeh H.' 'Al-Azemi, Talal F.' _journal_coeditor_code BT4156 _journal_paper_doi 10.1107/S2414314624010289 _journal_year 2024 _chemical_absolute_configuration unk _chemical_formula_iupac 'C70 H70 N4 O12' _chemical_formula_moiety 'C70 H70 N4 O12' _chemical_formula_sum 'C70 H70 N4 O12' _chemical_formula_weight 1159.30 _chemical_name_common ; meso-5,15-Bis[3-(isopropylidenegalactopyranoxy)phenyl]-\ 10,20-bis(4-methylphenyl)porphyrin ; _chemical_name_systematic meso-5,15-Bis{4-[{4,4,11,11-tetramethyl-3,5,7,10,12-pentaoxatricyclo[7.3.0.0^2,6^]dodecan-8-yl)methoxy]phenyl}-10,20-bis(4-methylphenyl)porphyrin _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2019/3 _cell_angle_alpha 90 _cell_angle_beta 99.376(7) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 16.565(2) _cell_length_b 9.7051(13) _cell_length_c 19.708(3) _cell_measurement_reflns_used 7206 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 25.27 _cell_measurement_theta_min 3.08 _cell_volume 3126.0(7) _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 ; SHELXL2019/3 (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 0.995 _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 0.1440 _diffrn_reflns_av_unetI/netI 0.2047 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 25359 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.339 _diffrn_reflns_theta_min 3.082 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_T_max 0.997 _exptl_absorpt_correction_T_min 0.438 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (ABSCOR; Higashi, 1995) ; _exptl_crystal_colour Purple _exptl_crystal_density_diffrn 1.232 _exptl_crystal_description Platelet _exptl_crystal_F_000 1228 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_min 0.040 _refine_diff_density_max 0.214 _refine_diff_density_min -0.203 _refine_ls_abs_structure_details ; Flack x determined using 1142 quotients [(I^+^)-(I^-^)]/[(I^+^)+(I^-^)] (Parsons et al., 2013) ; _refine_ls_abs_structure_Flack -1.0(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 785 _refine_ls_number_reflns 11348 _refine_ls_number_restraints 168 _refine_ls_restrained_S_all 0.942 _refine_ls_R_factor_all 0.2350 _refine_ls_R_factor_gt 0.0823 _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^)+(0.0622P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1390 _refine_ls_wR_factor_ref 0.1860 _reflns_number_gt 4159 _reflns_number_total 11348 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file bt4156.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 1572955 _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 0.987 _shelx_estimated_absorpt_t_max 0.997 _shelx_hkl_file ; 0 0 3 -8.53 16.96 0 0 3 -6.78 51.11 0 0 -3 1.17 29.58 0 0 450119.70 1268.60 0 0 449005.22 1537.49 0 0 -449263.35 1538.70 0 0 5 2.12 23.97 0 0 5 6.23 44.22 0 0 -5 -29.29 67.36 0 0 6 9709.50 168.36 0 0 6 9810.63 299.86 0 0 -6 9684.58 296.94 0 0 7 -5.55 26.06 0 0 7 -0.44 77.19 0 0 -7 -26.94 72.44 0 0 8 6383.60 117.88 0 0 8 6675.84 232.37 0 0 -8 6432.74 229.24 0 0 9 4.83 26.22 0 0 9 59.91 84.25 0 0 -9 50.21 76.90 0 0 10 568.05 70.22 0 0 10 669.71 33.94 0 0 -10 551.77 103.00 0 0 11 -40.37 86.87 0 0 11 -6.01 26.20 0 0 11 -52.30 42.74 0 0 -11 -27.04 51.82 0 0 12 -2.40 97.00 0 0 12 63.77 45.87 0 0 12 125.59 29.00 0 0 13 -2.36 28.84 0 0 13 11.04 44.86 0 0 13 63.16 95.20 0 0 14 189.05 34.48 0 0 14 166.43 52.06 0 0 15 2.92 47.25 0 0 15 176.37 101.19 0 0 15 21.65 33.28 0 0 16 975.14 143.91 0 0 16 882.95 67.00 0 0 16 699.18 49.71 0 0 17 -199.54 127.73 0 0 17 69.34 35.37 0 0 17 80.31 50.13 0 0 18 635.90 55.19 0 0 18 488.13 66.30 0 0 18 466.60 165.57 0 0 19 -11.68 135.33 0 0 19 -1.32 30.67 0 0 19 75.84 44.31 0 0 20 8.31 29.52 0 0 20 229.22 149.17 0 0 21 200.07 169.82 0 0 22 -67.83 168.98 0 0 23 103.73 177.12 0 1 -3 114.83 64.89 0 1 -3 125.12 32.02 0 1 3 161.12 40.38 0 -1 3 134.82 24.82 0 -1 3 85.11 38.98 0 -1 -3 132.85 46.33 0 1 -4 2628.25 63.74 0 1 4 2507.45 72.15 0 1 -4 2626.07 129.73 0 -1 4 2620.98 135.59 0 -1 -4 2559.24 90.02 0 -1 4 2507.28 64.46 0 1 5 1097.77 68.80 0 1 -5 1100.05 42.72 0 1 -5 1167.35 110.62 0 -1 5 985.50 112.95 0 -1 5 1039.39 41.76 0 1 6 -21.48 35.47 0 1 -6 -48.68 82.77 0 1 6 33.63 65.38 0 1 -6 -1.80 25.68 0 -1 6 2.46 51.34 0 -1 6 -1.47 22.80 0 1 7 419.66 80.86 0 1 7 411.52 46.50 0 1 -7 419.48 99.52 0 1 -7 396.60 31.32 0 -1 7 309.09 99.46 0 -1 7 359.44 25.75 0 1 8 251.13 45.76 0 1 -8 267.87 27.76 0 1 8 262.74 83.28 0 1 -8 330.05 93.69 0 -1 8 223.33 95.13 0 -1 8 259.85 24.32 0 1 9 162.72 75.49 0 1 9 127.48 26.49 0 1 -9 146.39 32.19 0 1 9 117.34 42.06 0 1 -9 169.29 91.98 0 -1 9 133.43 22.54 0 -1 9 231.50 90.67 0 1 10 1586.24 81.61 0 1 10 1568.46 117.81 0 1 -10 1399.86 130.07 0 1 10 1310.59 43.59 0 1 -10 1388.61 41.86 0 -1 10 1375.01 41.70 0 -1 10 1308.85 130.50 0 1 11 235.81 35.14 0 1 11 276.65 44.88 0 1 11 179.43 90.15 0 1 -11 206.60 102.64 0 -1 11 189.03 25.08 0 -1 11 170.83 102.82 0 1 12 102.04 26.85 0 1 12 157.92 54.79 0 1 12 200.14 91.99 0 1 -12 62.73 103.30 0 -1 12 144.69 25.04 0 -1 12 239.39 97.70 0 1 13 101.46 41.28 0 1 13 170.63 35.26 0 1 -13 185.78 70.74 0 1 13 38.17 95.47 0 -1 13 222.13 107.47 0 -1 13 85.91 26.38 0 1 14 110.63 38.27 0 1 14 124.01 99.73 0 1 14 78.46 58.85 0 1 -14 173.05 111.82 0 -1 14 103.07 108.34 0 -1 14 87.47 33.81 0 1 -15 64.57 121.13 0 1 15 73.68 57.98 0 1 15 139.69 110.82 0 1 15 141.93 38.61 0 -1 15 98.72 43.08 0 -1 15 48.40 29.45 0 -1 15 224.98 118.39 0 1 16 274.89 71.09 0 1 16 250.80 45.14 0 1 16 204.11 130.42 0 1 -16 376.09 144.46 0 -1 16 315.59 33.94 0 -1 16 211.46 46.34 0 -1 16 435.40 134.01 0 1 17 605.11 78.78 0 1 17 553.81 146.79 0 1 17 392.91 48.03 0 -1 17 522.52 152.92 0 1 18 488.38 151.42 0 1 18 561.52 80.29 0 1 18 416.33 49.73 0 -1 18 438.80 105.49 0 1 19 45.90 41.52 0 1 19 53.39 64.98 0 1 19 1.35 133.50 0 -1 19 281.22 146.49 0 1 20 45.82 38.04 0 1 20 94.22 137.12 0 1 20 -6.41 57.76 0 1 21 86.68 149.05 0 1 21 3.00 31.94 0 1 21 -24.89 46.98 0 -1 21 130.04 154.23 0 1 22 -56.48 153.78 0 -1 22 67.67 163.70 0 1 23 121.52 175.99 0 -1 23 131.69 184.89 0 2 020792.45 507.60 0 -2 020580.27 459.41 0 2 112063.36 251.72 0 2 -112436.77 285.27 0 -2 112069.44 284.43 0 -2 -111731.12 299.11 0 2 2 2281.45 106.71 0 2 -2 2237.04 84.54 0 -2 2 2188.37 86.43 0 -2 -2 2136.95 109.82 0 2 3 6418.23 189.04 0 2 -3 6509.05 148.97 0 2 -3 6451.04 220.69 0 -2 -3 6339.95 191.94 0 -2 3 6374.69 150.41 0 2 410980.03 290.08 0 2 -411502.94 285.76 0 2 -411357.73 259.81 0 -2 411499.89 360.09 0 -2 -411038.70 302.78 0 -2 411187.26 266.14 0 2 5 53.40 56.55 0 2 -5 43.13 33.34 0 2 -5 27.48 53.08 0 -2 -5 157.44 64.11 0 -2 5 -25.70 87.15 0 -2 5 20.55 47.91 0 2 -6 567.35 37.44 0 2 6 585.22 64.18 0 2 -6 580.75 109.59 0 -2 6 562.21 53.07 0 -2 6 544.63 107.91 0 -2 -6 524.05 70.81 0 2 -7 306.95 29.19 0 2 7 326.37 54.20 0 2 -7 240.11 62.48 0 -2 7 274.64 43.21 0 -2 -7 299.04 87.52 0 -2 7 290.94 102.60 0 2 -8 2650.58 71.74 0 2 -8 2413.86 162.83 0 2 8 2704.53 93.39 0 -2 8 2757.36 115.52 0 -2 8 2614.86 65.04 0 2 9 1595.81 74.22 0 2 -9 1780.25 141.44 0 2 -9 1602.66 54.53 0 -2 9 1497.24 134.62 0 -2 9 1591.06 59.13 0 2 10 1208.16 106.11 0 2 -10 1301.69 40.38 0 2 10 1413.71 66.57 0 2 -10 1530.07 140.96 0 -2 10 1444.25 133.33 0 -2 10 1229.04 54.90 0 2 11 38.07 40.20 0 2 -11 -35.88 97.71 0 2 11 -56.29 74.70 0 2 -11 5.12 29.73 0 -2 11 31.14 32.87 0 -2 11 -54.81 93.30 0 2 12 311.00 48.69 0 2 12 330.78 94.47 0 2 -12 324.76 34.11 0 2 -12 305.71 76.89 0 -2 12 243.20 38.87 0 -2 12 254.09 111.35 0 2 13 7.37 31.64 0 2 13 -110.87 87.66 0 2 13 6.61 56.68 0 2 -13 64.04 107.54 0 2 -13 20.83 28.15 0 -2 13 33.94 105.25 0 -2 13 31.70 40.93 0 2 -14 195.07 31.66 0 2 14 219.75 51.52 0 2 14 346.65 105.72 0 2 14 198.48 46.54 0 2 -14 366.69 130.86 0 -2 14 199.41 40.02 0 -2 14 287.86 122.83 0 2 15 -38.41 105.55 0 2 15 101.38 45.22 0 2 -15 144.63 89.10 0 2 15 76.12 67.65 0 -2 15 98.87 38.05 0 -2 15 88.26 121.37 0 2 16 153.34 69.89 0 2 16 143.44 113.60 0 2 -16 271.24 138.88 0 2 16 156.59 38.50 0 -2 16 163.26 136.04 0 -2 16 81.36 38.74 0 2 17 361.66 127.84 0 2 17 192.91 58.52 0 2 17 176.22 51.22 0 2 -17 445.51 157.24 0 -2 17 134.96 143.54 0 -2 17 154.43 37.34 0 2 18 77.16 39.62 0 2 18 98.98 130.34 0 2 -18 310.57 158.70 0 2 18 239.79 62.57 0 -2 18 79.30 38.35 0 -2 18 53.72 150.42 0 -2 18 88.03 34.53 0 2 19 -46.92 73.96 0 2 -19 170.91 161.39 0 2 19 -27.41 125.73 0 2 19 2.07 46.89 0 -2 19 4.07 94.45 0 2 20 -50.59 74.86 0 2 20 19.19 142.11 0 2 20 -15.33 46.65 0 2 -20 -93.93 111.58 0 -2 20 45.90 156.34 0 2 21 12.91 51.69 0 2 21 -0.34 33.29 0 2 21 -103.04 146.55 0 -2 21 -94.35 162.61 0 2 22 469.47 175.37 0 -2 22 220.62 201.47 0 3 0 -21.91 65.32 0 -3 0 -10.22 69.01 0 3 1 128.90 72.78 0 3 -1 -34.53 63.44 0 -3 1 160.20 65.95 0 -3 -1 57.50 45.60 0 3 2 529.03 85.07 0 3 -2 504.16 70.05 0 -3 2 532.33 75.29 0 -3 -2 580.82 85.57 0 3 3 7526.71 228.85 0 3 -3 7475.30 195.14 0 -3 3 7348.92 206.17 0 -3 -3 7144.74 230.63 0 3 4 2901.02 130.40 0 3 -4 2897.53 160.71 0 3 -4 2891.26 100.14 0 -3 4 2682.96 104.55 0 -3 -4 2741.41 132.96 0 3 5 326.99 71.87 0 3 -5 217.74 45.69 0 3 -5 205.16 99.82 0 -3 -5 211.23 50.25 0 -3 5 260.66 50.97 0 3 6 1419.61 99.44 0 3 -6 1440.21 62.63 0 3 -6 1306.87 88.81 0 -3 -6 1295.49 107.04 0 -3 6 1436.94 69.60 0 3 -7 4895.34 116.55 0 3 7 5195.17 171.78 0 3 -7 4575.93 225.98 0 -3 7 4946.83 150.86 0 -3 7 5047.31 169.91 0 -3 -7 4735.56 180.89 0 3 -8 8008.63 191.39 0 3 8 7737.65 233.30 0 3 -8 7662.20 317.83 0 -3 8 7785.66 189.78 0 -3 -8 7714.97 256.91 0 -3 8 8097.06 306.38 0 3 9 307.21 67.66 0 3 -9 362.74 46.23 0 3 -9 266.07 71.15 0 -3 9 369.65 41.86 0 -3 -9 203.61 77.19 0 -3 9 447.63 105.59 0 3 -10 295.15 34.28 0 3 -10 209.64 76.45 0 3 10 165.84 63.70 0 -3 10 326.18 109.64 0 -3 10 378.57 52.66 0 3 -11 620.35 38.82 0 3 11 739.34 73.36 0 3 -11 543.86 88.01 0 -3 11 507.22 58.57 0 -3 11 721.10 84.37 0 3 12 440.51 96.96 0 3 12 441.35 70.35 0 3 -12 380.97 46.97 0 3 -12 296.29 135.35 0 -3 12 420.56 125.38 0 -3 12 443.97 43.59 0 3 13 578.13 113.91 0 3 13 928.93 96.42 0 3 -13 548.18 51.79 0 3 -13 569.28 154.34 0 -3 13 576.58 61.58 0 -3 13 576.37 138.00 0 3 14 108.60 60.41 0 3 14 37.75 94.67 0 3 -14 40.28 123.50 0 3 -14 -20.75 38.02 0 -3 14 4.14 115.59 0 -3 14 -22.15 45.06 0 3 15 413.71 123.57 0 3 -15 373.17 163.04 0 3 15 633.04 72.67 0 3 -15 450.45 46.30 0 -3 15 350.20 61.39 0 -3 15 531.15 152.06 0 3 16 141.02 113.83 0 3 16 101.97 43.80 0 3 -16 274.42 96.94 0 3 16 137.51 65.05 0 3 -16 71.18 36.67 0 -3 16 287.01 142.08 0 -3 16 91.82 50.63 0 3 -17 56.61 25.36 0 3 17 9.40 83.66 0 3 17 35.86 55.54 0 3 17 -15.33 119.40 0 3 -17 34.43 152.24 0 -3 17 118.59 48.15 0 -3 17 187.44 145.70 0 3 18 128.05 74.30 0 3 18 246.11 126.15 0 3 -18 19.52 171.61 0 3 18 1.27 44.58 0 -3 18 8.09 156.64 0 -3 18 98.25 43.99 0 3 19 208.90 60.19 0 3 19 120.15 146.67 0 3 19 240.12 105.76 0 3 -19 331.26 120.70 0 -3 19 110.54 45.22 0 -3 19 97.08 172.55 0 3 20 -15.65 90.97 0 3 -20 -35.57 170.60 0 3 20 -99.45 142.49 0 3 20 3.17 42.14 0 -3 20 100.14 158.28 0 3 21 50.06 58.08 0 3 21 48.49 93.09 0 3 21 -85.13 151.48 0 3 -21 127.73 185.18 0 -3 21 27.32 114.62 0 3 22 -36.16 168.24 0 3 -22 209.02 218.18 0 -3 22 349.33 196.43 0 4 0 3087.22 140.55 0 -4 0 3052.30 145.29 0 4 -1 917.65 89.09 0 4 1 996.58 91.03 0 -4 -1 1006.97 98.92 0 -4 1 863.89 97.95 0 4 2 1290.81 101.49 0 4 -2 1403.75 93.65 0 -4 2 1256.69 65.60 0 -4 -2 1153.12 110.55 0 4 3 129.67 48.64 0 4 -3 192.72 61.74 0 -4 3 133.40 66.47 0 -4 -3 188.75 81.05 0 4 -4 1379.21 84.43 0 4 4 1517.11 108.59 0 4 -4 1599.99 141.19 0 -4 4 1549.95 94.49 0 -4 -4 1550.09 118.15 0 4 5 2030.27 83.46 0 4 -5 2082.99 89.40 0 4 -5 1866.26 105.55 0 -4 5 1848.14 98.42 0 -4 -5 1999.68 126.60 0 4 6 225.18 73.20 0 4 -6 140.13 47.95 0 4 -6 110.60 100.41 0 -4 -6 217.83 83.58 0 -4 6 123.51 57.52 0 4 -7 2.61 44.12 0 4 7 29.86 67.31 0 4 -7 102.64 93.31 0 -4 7 18.61 50.22 0 -4 -7 34.00 79.48 0 4 8 3360.74 150.07 0 4 -8 3375.85 125.53 0 4 -8 3211.09 144.48 0 -4 -8 3166.76 161.16 0 -4 8 3140.23 115.21 0 4 9 -7.78 66.77 0 4 -9 -4.11 105.50 0 4 -9 24.75 49.65 0 -4 -9 60.03 77.34 0 -4 9 14.96 62.58 0 4 10 176.82 69.73 0 4 -10 84.73 39.18 0 4 -10 205.08 118.18 0 -4 -10 123.33 85.14 0 -4 10 97.42 64.47 0 -4 10 -34.48 71.28 0 4 -11 505.08 48.62 0 4 11 471.53 84.37 0 4 -11 479.47 136.83 0 -4 11 420.38 75.55 0 -4 -11 377.26 97.44 0 -4 11 437.00 87.63 0 4 -12 262.29 42.54 0 4 12 230.83 76.58 0 4 -12 83.33 134.73 0 -4 12 121.49 69.12 0 -4 12 174.16 82.38 0 4 13 624.24 90.27 0 4 -13 562.01 155.99 0 4 -13 582.37 50.66 0 -4 13 405.78 148.16 0 -4 13 469.84 78.63 0 4 14 186.15 77.08 0 4 14 246.21 106.44 0 4 -14 181.56 54.95 0 4 -14 293.85 97.19 0 -4 14 120.58 138.34 0 -4 14 109.91 55.26 0 4 15 182.86 98.95 0 4 -15 99.39 156.46 0 4 15 12.17 108.51 0 4 -15 133.35 53.86 0 -4 15 98.13 69.18 0 -4 15 105.86 133.27 0 4 16 -53.38 77.85 0 4 16 -18.03 112.37 0 4 -16 56.22 50.95 0 4 -16 126.84 155.50 0 -4 16 124.12 65.92 0 -4 16 60.45 139.37 0 4 -17 50.68 35.41 0 4 17 94.93 123.43 0 4 17 82.28 104.10 0 4 17 63.76 33.24 0 4 -17 9.04 169.64 0 -4 17 128.74 149.13 0 -4 17 100.06 64.46 0 4 18 112.22 49.41 0 4 18 46.52 90.36 0 4 18 21.21 123.29 0 4 -18 12.17 39.47 0 4 -18 126.00 111.55 0 -4 18 -30.60 62.05 0 -4 18 55.68 152.48 0 4 19 104.53 113.51 0 4 19 55.92 135.67 0 4 -19 21.69 24.85 0 4 19 -39.73 64.45 0 4 -19 35.77 187.83 0 -4 19 -46.66 170.67 0 -4 19 -0.55 62.84 0 4 20 324.60 143.59 0 4 20 40.29 50.97 0 4 20 11.59 88.34 0 4 -20 -122.01 194.48 0 -4 20 -157.54 179.61 0 4 21 60.68 50.19 0 4 21 31.81 92.69 0 4 21 -10.50 155.47 0 4 -21 223.59 136.92 0 -4 21 -103.15 193.82 0 5 0 3.26 42.33 0 -5 0 64.96 74.94 0 5 1 111.94 74.67 0 5 -1 249.54 71.56 0 -5 1 135.48 80.08 0 -5 -1 88.48 53.82 0 5 2 951.10 101.32 0 5 -2 1179.46 92.61 0 -5 2 968.15 68.87 0 -5 -2 965.35 111.89 0 5 3 563.92 58.62 0 5 -3 620.67 77.56 0 -5 3 548.39 90.03 0 -5 -3 599.38 100.73 0 5 -4 1839.52 115.82 0 5 4 1858.61 124.43 0 5 -4 2070.04 101.28 0 -5 4 1869.83 80.59 0 -5 -4 1849.53 133.39 0 5 5 193.22 80.54 0 5 -5 154.64 59.46 0 5 -5 156.64 65.69 0 -5 5 117.60 69.12 0 -5 -5 86.52 56.74 0 5 -6 32.05 105.80 0 5 6 3.95 75.82 0 5 -6 52.86 53.61 0 -5 6 43.66 64.96 0 -5 -6 123.11 57.62 0 5 7 209.62 81.89 0 5 -7 158.28 56.32 0 5 -7 308.10 115.45 0 -5 7 117.76 66.47 0 -5 -7 225.48 95.50 0 5 8 808.32 99.19 0 5 -8 744.65 70.84 0 5 -8 734.85 94.74 0 -5 -8 967.12 117.72 0 -5 8 789.59 83.67 0 5 9 -7.30 79.38 0 5 -9 8.21 50.29 0 5 -9 -41.00 77.79 0 -5 9 -54.37 59.29 0 -5 -9 -10.96 90.25 0 5 -10 30.93 143.92 0 5 10 440.19 92.76 0 5 -10 339.27 59.39 0 -5 -10 421.90 113.05 0 -5 10 437.99 73.50 0 5 11 -5.51 85.23 0 5 -11 6.49 136.20 0 5 -11 162.17 49.61 0 -5 -11 111.10 105.64 0 -5 11 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-1 77.68 114.92 -19 3 1 -169.88 103.16 -19 -3 1 49.30 126.60 -19 3 0 3.29 102.59 ; _shelx_hkl_checksum 99788 _shelx_res_file ; TITL User-defined shelxl.res created by SHELXL-2019/3 at 07:42:53 on 02-Oct-2024 CELL 0.71075 16.56490 9.70512 19.70800 90.000 99.376 90.000 ZERR 2 0.00230 0.00134 0.00250 0.000 0.007 0.000 LATT -1 SYMM -X, .50+Y, -Z SFAC C H N O UNIT 140 140 8 24 SHEL 99999.000000 0.000000 L.S. 10 FMAP 2 PLAN -107 WPDB -2 HTAB BOND $H CONF LIST 4 MERG 2 TEMP -123.0 ACTA SIZE 0.150 0.070 0.040 DELU 0.01 C27 > C32 C57 SIMU 0.01 C27 > C32 C57 DELU 0.01 C39 > C44 C70 SIMU 0.01 C39 > C44 C70 DFIX 1.40 0.01 C39 C40 C40 C41 C41 C42 C42 C43 C43 C44 C39 C44 DFIX 1.40 0.01 C27 C28 C28 C29 C29 C30 C30 C31 C31 C32 C32 C27 DELU 0.01 C54 O5 C55 C56 O6 SIMU 0.01 C54 O5 C55 C56 O6 DELU 0.01 C1 C20 SIMU 0.01 C1 C20 WGHT 0.062200 FVAR 1.22079 O1 4 0.628001 0.252213 0.100906 11.00000 0.03933 0.05547 = 0.06480 0.00376 -0.00730 -0.00743 O2 4 0.452567 0.069154 0.017678 11.00000 0.06139 0.04787 = 0.06788 0.00478 -0.01720 -0.01124 O3 4 0.407399 0.090518 -0.099320 11.00000 0.09415 0.05986 = 0.05978 -0.00087 -0.01083 0.00205 O4 4 0.381011 0.313935 -0.076996 11.00000 0.07152 0.04968 = 0.05510 0.00036 -0.00547 0.00307 O5 4 0.320092 0.232027 0.085937 11.00000 0.05756 0.11280 = 0.09300 0.03542 0.02673 0.01314 O6 4 0.450111 0.235346 0.142941 11.00000 0.07359 0.12178 = 0.05860 0.01686 0.01962 0.01140 O7 4 1.365261 1.307448 0.398087 11.00000 0.04103 0.04733 = 0.07374 0.00885 -0.00975 -0.00308 O8 4 1.531257 1.110218 0.486692 11.00000 0.05367 0.03578 = 0.07396 0.00505 -0.00916 -0.00237 O9 4 1.583461 1.142560 0.601851 11.00000 0.08797 0.05358 = 0.06366 0.00291 -0.00122 -0.00764 O10 4 1.618309 1.358997 0.571858 11.00000 0.06533 0.05053 = 0.06074 -0.00418 0.00323 0.00371 O11 4 1.543847 1.240222 0.357406 11.00000 0.05954 0.08995 = 0.06376 -0.01181 0.00488 -0.00638 O12 4 1.674163 1.256648 0.410173 11.00000 0.05182 0.09023 = 0.09077 -0.00331 0.01674 0.00084 N1 3 0.928206 0.679812 0.159155 11.00000 0.04513 0.06338 = 0.04293 -0.00716 -0.00278 -0.00469 AFIX 43 H1 2 0.954839 0.711788 0.198271 11.00000 -1.20000 AFIX 0 N2 3 0.976119 0.574904 0.297193 11.00000 0.03712 0.06410 = 0.05423 -0.01336 -0.00039 -0.00194 N3 3 1.075632 0.816943 0.343747 11.00000 0.04074 0.06071 = 0.04278 -0.00682 0.00103 0.00345 AFIX 43 H3 2 1.047742 0.788022 0.304487 11.00000 -1.20000 AFIX 0 N4 3 1.028252 0.922893 0.205249 11.00000 0.04097 0.05433 = 0.05759 0.00305 0.00956 -0.00215 C1 1 0.918446 0.749921 0.097375 11.00000 0.03751 0.07118 = 0.04153 -0.00063 0.00140 -0.00450 C2 1 0.870221 0.664417 0.048961 11.00000 0.03953 0.07340 = 0.05730 0.00655 0.00083 -0.01267 AFIX 43 H2 2 0.851864 0.686988 0.002081 11.00000 -1.20000 AFIX 0 C3 1 0.854387 0.546544 0.079421 11.00000 0.04674 0.06915 = 0.05060 -0.01064 -0.00464 -0.00499 AFIX 43 H3A 2 0.824321 0.470900 0.057576 11.00000 -1.20000 AFIX 0 C4 1 0.890737 0.553640 0.151195 11.00000 0.04128 0.07335 = 0.04399 -0.00677 -0.00345 0.00721 C5 1 0.883811 0.457363 0.202751 11.00000 0.03162 0.05682 = 0.06226 -0.00807 0.00274 -0.00023 C6 1 0.920591 0.471361 0.272661 11.00000 0.02633 0.07897 = 0.05126 0.00594 -0.00304 0.00225 C7 1 0.902845 0.382318 0.326051 11.00000 0.05365 0.06871 = 0.05455 -0.00496 0.00107 -0.01433 AFIX 43 H7 2 0.865585 0.307189 0.321197 11.00000 -1.20000 AFIX 0 C8 1 0.949565 0.426057 0.384913 11.00000 0.06773 0.06386 = 0.05875 0.00450 0.01008 -0.00374 AFIX 43 H8 2 0.952624 0.386823 0.429422 11.00000 -1.20000 AFIX 0 C9 1 0.993342 0.543377 0.366356 11.00000 0.04370 0.06056 = 0.04943 0.00159 0.00553 -0.00303 C10 1 1.049992 0.617005 0.414461 11.00000 0.04769 0.06382 = 0.05383 0.00046 -0.00402 0.00461 C11 1 1.084442 0.742239 0.403959 11.00000 0.04976 0.06560 = 0.04487 -0.00204 0.00100 0.00968 C12 1 1.134611 0.827537 0.454278 11.00000 0.04034 0.08507 = 0.04788 -0.01766 -0.00061 -0.00297 AFIX 43 H12 2 1.153168 0.803771 0.500976 11.00000 -1.20000 AFIX 0 C13 1 1.150698 0.947195 0.423543 11.00000 0.04481 0.08319 = 0.05140 -0.00450 -0.00294 -0.01463 AFIX 43 H13 2 1.180582 1.022649 0.445768 11.00000 -1.20000 AFIX 0 C14 1 1.115281 0.941656 0.351889 11.00000 0.03253 0.06555 = 0.05966 -0.00782 0.00361 -0.00383 C15 1 1.119560 1.036957 0.301247 11.00000 0.03297 0.06787 = 0.04583 -0.00389 -0.00455 -0.00199 C16 1 1.081648 1.022578 0.231564 11.00000 0.04322 0.04698 = 0.05837 0.00186 0.01327 0.00181 C17 1 1.097571 1.115598 0.176987 11.00000 0.05183 0.05521 = 0.06763 -0.00704 0.00797 -0.00303 AFIX 43 H17 2 1.133870 1.192042 0.181368 11.00000 -1.20000 AFIX 0 C18 1 1.049848 1.070309 0.118789 11.00000 0.05214 0.07414 = 0.06198 0.00251 -0.00030 -0.01022 AFIX 43 H18 2 1.045910 1.110858 0.074498 11.00000 -1.20000 AFIX 0 C19 1 1.006969 0.952358 0.135387 11.00000 0.04880 0.05270 = 0.05257 0.00053 0.00693 0.00619 C20 1 0.953193 0.875680 0.088532 11.00000 0.04186 0.07232 = 0.04083 0.00220 0.01086 0.00660 C21 1 0.833899 0.331214 0.183981 11.00000 0.03993 0.05908 = 0.04634 -0.00984 0.00108 0.00284 C22 1 0.752270 0.341328 0.152512 11.00000 0.04336 0.03921 = 0.05707 0.00343 -0.00109 0.00063 AFIX 43 H22 2 0.727941 0.429648 0.144192 11.00000 -1.20000 AFIX 0 C23 1 0.706489 0.224951 0.133349 11.00000 0.03974 0.06004 = 0.05452 0.00164 -0.00525 0.00621 C24 1 0.738923 0.097461 0.146363 11.00000 0.04302 0.05812 = 0.05476 -0.00659 -0.00390 -0.01080 AFIX 43 H24 2 0.706349 0.017820 0.134432 11.00000 -1.20000 AFIX 0 C25 1 0.820397 0.084206 0.177370 11.00000 0.05646 0.05200 = 0.05313 -0.01278 -0.00101 0.01374 AFIX 43 H25 2 0.844028 -0.004627 0.185696 11.00000 -1.20000 AFIX 0 C26 1 0.865617 0.198074 0.195532 11.00000 0.05520 0.06887 = 0.05296 -0.00663 0.00372 0.00833 AFIX 43 H26 2 0.920947 0.187429 0.216917 11.00000 -1.20000 AFIX 0 C27 1 1.074535 0.549715 0.483330 11.00000 0.05470 0.08247 = 0.05406 -0.00270 -0.00061 0.00463 C28 1 1.045949 0.589348 0.541807 11.00000 0.06680 0.07431 = 0.06083 -0.00196 0.00990 -0.01479 AFIX 43 H28 2 1.007720 0.662807 0.539723 11.00000 -1.20000 AFIX 0 C29 1 1.072432 0.522785 0.604768 11.00000 0.07179 0.08634 = 0.05637 -0.00486 0.00906 -0.02722 AFIX 43 H29 2 1.053241 0.554033 0.644960 11.00000 -1.20000 AFIX 0 C30 1 1.125181 0.414144 0.609242 11.00000 0.07413 0.09430 = 0.05533 0.00818 -0.00029 -0.01415 C31 1 1.154262 0.373258 0.551376 11.00000 0.11673 0.13666 = 0.07461 0.02347 0.00682 0.04969 AFIX 43 H31 2 1.192796 0.300186 0.553893 11.00000 -1.20000 AFIX 0 C32 1 1.127441 0.438737 0.488366 11.00000 0.09961 0.13497 = 0.05965 0.01208 0.00514 0.04642 AFIX 43 H32 2 1.146059 0.406078 0.448177 11.00000 -1.20000 AFIX 0 C33 1 1.164315 1.169762 0.318417 11.00000 0.03486 0.07105 = 0.05795 -0.00599 0.00491 -0.00131 C34 1 1.246003 1.169132 0.350425 11.00000 0.04757 0.05513 = 0.06081 0.00336 0.00340 0.00178 AFIX 43 H34 2 1.273934 1.084639 0.361723 11.00000 -1.20000 AFIX 0 C35 1 1.285434 1.293354 0.365351 11.00000 0.04262 0.06273 = 0.04954 0.00461 0.00179 -0.00567 C36 1 1.247987 1.417105 0.347221 11.00000 0.04915 0.06297 = 0.05852 0.00515 -0.00030 0.00075 AFIX 43 H36 2 1.277357 1.501065 0.355812 11.00000 -1.20000 AFIX 0 C37 1 1.166593 1.417729 0.316159 11.00000 0.04972 0.06303 = 0.06998 0.00578 0.00142 0.00945 AFIX 43 H37 2 1.139301 1.502405 0.303901 11.00000 -1.20000 AFIX 0 C38 1 1.124961 1.292464 0.303008 11.00000 0.03952 0.06788 = 0.05550 -0.00976 0.00746 0.00704 AFIX 43 H38 2 1.068714 1.292745 0.283148 11.00000 -1.20000 AFIX 0 C39 1 0.926259 0.943230 0.019535 11.00000 0.05653 0.08327 = 0.04778 0.00489 0.00685 -0.00104 C40 1 0.875894 1.057934 0.014735 11.00000 0.10820 0.13556 = 0.05033 0.01379 0.00937 0.04217 AFIX 43 H40 2 0.859411 1.091771 0.055595 11.00000 -1.20000 AFIX 0 C41 1 0.848103 1.126358 -0.046776 11.00000 0.12770 0.14011 = 0.05825 0.01640 -0.00022 0.04251 AFIX 43 H41 2 0.814105 1.205354 -0.047514 11.00000 -1.20000 AFIX 0 C42 1 0.870642 1.077768 -0.106058 11.00000 0.08623 0.10153 = 0.04139 -0.00205 -0.00273 -0.01560 C43 1 0.926047 0.973533 -0.101534 11.00000 0.07423 0.10233 = 0.04487 -0.00442 0.01450 -0.02092 AFIX 43 H43 2 0.946518 0.945562 -0.141692 11.00000 -1.20000 AFIX 0 C44 1 0.953469 0.906965 -0.039853 11.00000 0.06010 0.08014 = 0.05122 -0.00046 0.01440 -0.01074 AFIX 43 H44 2 0.992116 0.834364 -0.038827 11.00000 -1.20000 AFIX 0 C45 1 0.578123 0.133625 0.079501 11.00000 0.04810 0.06465 = 0.06425 -0.00742 0.00247 -0.00178 AFIX 23 H45A 2 0.565493 0.082156 0.119858 11.00000 -1.20000 H45B 2 0.606285 0.071094 0.051268 11.00000 -1.20000 AFIX 0 C46 1 0.501177 0.191055 0.037786 11.00000 0.04407 0.04970 = 0.06284 0.01034 -0.00095 -0.00777 AFIX 13 H46 2 0.514950 0.237211 -0.004232 11.00000 -1.20000 AFIX 0 C47 1 0.383626 0.094253 -0.033112 11.00000 0.04829 0.05927 = 0.07912 0.00634 -0.01896 -0.01069 AFIX 13 H47 2 0.341382 0.021761 -0.030353 11.00000 -1.20000 AFIX 0 C48 1 0.346514 0.234130 -0.027125 11.00000 0.04136 0.06713 = 0.07539 0.01922 -0.00387 0.00142 AFIX 13 H48 2 0.285845 0.228251 -0.041341 11.00000 -1.20000 AFIX 0 C49 1 0.392744 0.223299 -0.130606 11.00000 0.10158 0.06347 = 0.03982 0.00290 -0.00818 -0.00728 C50 1 0.469131 0.267363 -0.157443 11.00000 0.14726 0.09058 = 0.05338 0.00285 0.03617 0.01246 AFIX 137 H50A 2 0.479188 0.204350 -0.194016 11.00000 -1.20000 H50B 2 0.515870 0.265140 -0.119912 11.00000 -1.20000 H50C 2 0.461893 0.361185 -0.175812 11.00000 -1.20000 AFIX 0 C51 1 0.316855 0.219783 -0.186158 11.00000 0.14411 0.09952 = 0.07140 0.00216 -0.05439 0.00519 AFIX 137 H51A 2 0.268674 0.198315 -0.165108 11.00000 -1.20000 H51B 2 0.323673 0.148938 -0.220204 11.00000 -1.20000 H51C 2 0.309512 0.309840 -0.208816 11.00000 -1.20000 AFIX 0 C52 1 0.365646 0.305105 0.041971 11.00000 0.04663 0.08323 = 0.06191 0.00283 0.00883 -0.00637 AFIX 13 H52 2 0.348897 0.404161 0.038176 11.00000 -1.20000 AFIX 0 C53 1 0.455057 0.291018 0.076372 11.00000 0.03551 0.08156 = 0.04490 0.00131 0.00562 -0.00159 AFIX 13 H53 2 0.482634 0.382993 0.080629 11.00000 -1.20000 AFIX 0 C54 1 0.366844 0.236576 0.153632 11.00000 0.08133 0.12189 = 0.07895 0.02899 0.02838 0.01518 C55 1 0.351090 0.111844 0.191760 11.00000 0.09812 0.13933 = 0.12302 0.05945 0.05062 0.03400 AFIX 137 H55A 2 0.363465 0.030114 0.166114 11.00000 -1.20000 H55B 2 0.293452 0.109818 0.197542 11.00000 -1.20000 H55C 2 0.385852 0.112468 0.237035 11.00000 -1.20000 AFIX 0 C56 1 0.352061 0.371608 0.189791 11.00000 0.14140 0.14874 = 0.09308 0.01803 0.04054 0.06419 AFIX 137 H56A 2 0.296732 0.371387 0.201381 11.00000 -1.20000 H56B 2 0.357796 0.449309 0.159176 11.00000 -1.20000 H56C 2 0.392188 0.380598 0.231969 11.00000 -1.20000 AFIX 0 C57 1 1.154705 0.344014 0.677330 11.00000 0.10742 0.11503 = 0.06778 0.02554 -0.02135 -0.03798 AFIX 137 H57A 2 1.210454 0.374699 0.695308 11.00000 -1.20000 H57B 2 1.154416 0.243935 0.670676 11.00000 -1.20000 H57C 2 1.118369 0.367984 0.710108 11.00000 -1.20000 AFIX 0 C58 1 1.407910 1.183821 0.422416 11.00000 0.05380 0.04843 = 0.07611 0.01182 0.00231 -0.00133 AFIX 23 H58A 2 1.416401 1.123981 0.383511 11.00000 -1.20000 H58B 2 1.377085 1.131685 0.452991 11.00000 -1.20000 AFIX 0 C59 1 1.489617 1.234233 0.461857 11.00000 0.05184 0.04098 = 0.06643 0.01018 0.00295 -0.00942 AFIX 13 H59 2 1.479168 1.290577 0.502015 11.00000 -1.20000 AFIX 0 C60 1 1.603743 1.131119 0.534644 11.00000 0.04779 0.05875 = 0.06563 -0.00175 -0.00942 0.00076 AFIX 13 H60 2 1.641813 1.051695 0.532919 11.00000 -1.20000 AFIX 0 C61 1 1.648100 1.266168 0.524902 11.00000 0.04669 0.05054 = 0.07149 -0.00209 -0.00343 -0.00537 AFIX 13 H61 2 1.708568 1.253709 0.537920 11.00000 -1.20000 AFIX 0 C62 1 1.601205 1.277534 0.629727 11.00000 0.09074 0.06491 = 0.06086 0.00795 -0.00325 0.00952 C63 1 1.528700 1.334753 0.653722 11.00000 0.11964 0.09495 = 0.05551 -0.00464 0.01846 0.00458 AFIX 137 H63A 2 1.514538 1.277231 0.690929 11.00000 -1.20000 H63B 2 1.482699 1.336476 0.615538 11.00000 -1.20000 H63C 2 1.540511 1.428708 0.670703 11.00000 -1.20000 AFIX 0 C64 1 1.676464 1.274462 0.684699 11.00000 0.13673 0.05749 = 0.07417 -0.00416 -0.03793 0.00211 AFIX 137 H64A 2 1.692052 1.368875 0.698831 11.00000 -1.20000 H64B 2 1.721544 1.230188 0.666383 11.00000 -1.20000 H64C 2 1.664547 1.222335 0.724492 11.00000 -1.20000 AFIX 0 C65 1 1.538495 1.316798 0.420118 11.00000 0.05286 0.06158 = 0.05127 0.00227 -0.00107 -0.00516 AFIX 13 H65 2 1.512922 1.409154 0.409102 11.00000 -1.20000 AFIX 0 C66 1 1.628130 1.331894 0.454286 11.00000 0.04423 0.05441 = 0.07161 -0.00245 0.00693 -0.00008 AFIX 13 H66 2 1.644508 1.431172 0.456519 11.00000 -1.20000 AFIX 0 C67 1 1.624661 1.250855 0.343457 11.00000 0.06910 0.09261 = 0.08765 -0.01782 0.02191 0.00151 C68 1 1.647025 1.119792 0.309853 11.00000 0.15704 0.09559 = 0.12654 -0.03749 0.07894 0.00373 AFIX 137 H68A 2 1.614297 1.111910 0.263887 11.00000 -1.20000 H68B 2 1.636055 1.040584 0.337821 11.00000 -1.20000 H68C 2 1.705259 1.121701 0.306012 11.00000 -1.20000 AFIX 0 C69 1 1.633539 1.380330 0.302516 11.00000 0.11301 0.12694 = 0.10019 0.02575 0.04788 0.00644 AFIX 137 H69A 2 1.596684 1.375469 0.258318 11.00000 -1.20000 H69B 2 1.690162 1.388572 0.294416 11.00000 -1.20000 H69C 2 1.619521 1.460792 0.328301 11.00000 -1.20000 AFIX 0 C70 1 0.840729 1.155652 -0.173780 11.00000 0.12166 0.11966 = 0.05643 0.02056 -0.00816 -0.03049 AFIX 137 H70A 2 0.796702 1.103204 -0.201547 11.00000 -1.20000 H70B 2 0.886274 1.166548 -0.199439 11.00000 -1.20000 H70C 2 0.820220 1.246651 -0.163348 11.00000 -1.20000 AFIX 0 HKLF 4 REM User-defined REM wR2 = 0.1860, GooF = S = 0.930, Restrained GooF = 0.942 for all data REM R1 = 0.0823 for 4159 Fo > 4sig(Fo) and 0.2350 for all 11348 data REM 785 parameters refined using 168 restraints END WGHT 0.0622 0.0000 REM Instructions for potential hydrogen bonds HTAB N1 N2 HTAB N1 N4 HTAB N3 N2 HTAB N3 N4 EQIV $1 -x+1, y-1/2, -z HTAB C24 O4_$1 HTAB C45 O4_$1 REM Highest difference peak 0.214, deepest hole -0.203, 1-sigma level 0.043 Q1 1 1.1680 0.5380 0.4837 11.00000 0.05 0.21 Q2 1 1.2006 0.4638 0.5504 11.00000 0.05 0.20 Q3 1 0.8388 0.8852 0.0659 11.00000 0.05 0.19 Q4 1 1.4293 1.1734 0.3619 11.00000 0.05 0.18 Q5 1 0.8449 0.9528 0.0140 11.00000 0.05 0.18 Q6 1 1.2466 1.0012 0.4153 11.00000 0.05 0.18 Q7 1 1.1553 0.6029 0.4283 11.00000 0.05 0.17 Q8 1 1.4651 1.2181 0.5482 11.00000 0.05 0.17 Q9 1 1.1579 0.9362 0.5213 11.00000 0.05 0.16 Q10 1 0.4040 -0.0779 -0.0445 11.00000 0.05 0.16 Q11 1 0.7515 0.4755 0.0854 11.00000 0.05 0.15 Q12 1 1.7515 1.3843 0.4298 11.00000 0.05 0.15 Q13 1 1.7149 1.4594 0.4674 11.00000 0.05 0.15 Q14 1 0.7640 0.2193 0.2293 11.00000 0.05 0.15 Q15 1 1.3619 1.2019 0.3289 11.00000 0.05 0.15 Q16 1 1.0699 0.5507 0.2681 11.00000 0.05 0.15 Q17 1 0.7140 0.3561 0.0607 11.00000 0.05 0.15 Q18 1 0.5517 0.2962 0.1246 11.00000 0.05 0.15 Q19 1 0.9704 0.5221 0.5858 11.00000 0.05 0.15 Q20 1 0.9355 0.9171 -0.0038 11.00000 0.05 0.14 Q21 1 0.4955 0.0632 0.2223 11.00000 0.05 0.14 Q22 1 0.9910 1.0853 -0.0673 11.00000 0.05 0.14 Q23 1 1.1650 1.2855 0.2375 11.00000 0.05 0.14 Q24 1 0.8000 0.9232 -0.0905 11.00000 0.05 0.14 Q25 1 1.3099 1.1776 0.5744 11.00000 0.05 0.14 Q26 1 1.2314 0.9596 0.3697 11.00000 0.05 0.14 Q27 1 0.8030 1.0253 -0.0511 11.00000 0.05 0.14 Q28 1 1.0661 0.8065 0.2256 11.00000 0.05 0.14 Q29 1 1.1107 0.7391 0.3380 11.00000 0.05 0.14 Q30 1 1.3941 1.1179 0.5587 11.00000 0.05 0.14 Q31 1 1.0463 0.9249 0.0625 11.00000 0.05 0.14 Q32 1 0.3085 0.4210 -0.0570 11.00000 0.05 0.14 Q33 1 0.6726 0.0921 0.0586 11.00000 0.05 0.14 Q34 1 0.4915 0.2989 -0.0313 11.00000 0.05 0.13 Q35 1 1.0894 0.7362 0.5399 11.00000 0.05 0.13 Q36 1 0.3744 -0.1022 -0.0024 11.00000 0.05 0.13 Q37 1 1.0894 0.6213 0.3282 11.00000 0.05 0.13 Q38 1 0.3944 0.4347 -0.1857 11.00000 0.05 0.13 Q39 1 1.1476 1.1114 0.0948 11.00000 0.05 0.13 Q40 1 0.3626 -0.2382 0.0374 11.00000 0.05 0.13 Q41 1 0.7211 0.4886 0.1628 11.00000 0.05 0.13 Q42 1 0.4452 0.4426 -0.0417 11.00000 0.05 0.13 Q43 1 0.7260 0.4496 0.1656 11.00000 0.05 0.13 Q44 1 0.7991 0.6552 0.0814 11.00000 0.05 0.13 Q45 1 1.3540 1.4490 0.3265 11.00000 0.05 0.13 Q46 1 1.3631 1.1222 0.5018 11.00000 0.05 0.13 Q47 1 1.2732 1.0847 0.3376 11.00000 0.05 0.13 Q48 1 0.3224 0.4398 -0.1198 11.00000 0.05 0.13 Q49 1 0.5757 0.3915 0.1206 11.00000 0.05 0.13 Q50 1 1.4963 1.4406 0.4708 11.00000 0.05 0.13 Q51 1 1.3860 1.2632 0.3198 11.00000 0.05 0.13 Q52 1 1.2660 1.5486 0.3938 11.00000 0.05 0.13 Q53 1 1.1483 0.9536 0.2852 11.00000 0.05 0.13 Q54 1 0.8490 0.5357 0.2223 11.00000 0.05 0.13 Q55 1 0.8329 0.2155 0.2648 11.00000 0.05 0.13 Q56 1 0.9189 0.7622 -0.0356 11.00000 0.05 0.13 Q57 1 0.3543 0.5370 0.0743 11.00000 0.05 0.13 Q58 1 0.8559 0.3672 0.1282 11.00000 0.05 0.13 Q59 1 1.0336 0.4337 0.6742 11.00000 0.05 0.13 Q60 1 1.4919 1.3460 0.3223 11.00000 0.05 0.13 Q61 1 1.2484 0.4473 0.5003 11.00000 0.05 0.13 Q62 1 1.1288 0.8892 0.1845 11.00000 0.05 0.13 Q63 1 0.4158 0.8491 0.1682 11.00000 0.05 0.13 Q64 1 1.0617 0.5604 0.4983 11.00000 0.05 0.13 Q65 1 1.4500 1.0929 0.5133 11.00000 0.05 0.12 Q66 1 0.4936 0.0919 -0.0584 11.00000 0.05 0.12 Q67 1 0.6259 0.3367 0.1774 11.00000 0.05 0.12 Q68 1 0.6588 0.4344 0.1111 11.00000 0.05 0.12 Q69 1 1.0879 1.0496 0.0397 11.00000 0.05 0.12 Q70 1 0.9551 0.3367 0.4734 11.00000 0.05 0.12 Q71 1 1.1861 1.0574 0.3978 11.00000 0.05 0.12 Q72 1 1.1043 0.7277 0.5520 11.00000 0.05 0.12 Q73 1 0.9260 0.3998 0.1081 11.00000 0.05 0.12 Q74 1 0.6338 0.0638 0.1650 11.00000 0.05 0.12 Q75 1 1.0326 0.7186 0.4231 11.00000 0.05 0.12 Q76 1 0.9484 0.7939 0.0871 11.00000 0.05 0.12 Q77 1 0.3196 -0.1496 0.0772 11.00000 0.05 0.12 Q78 1 1.6335 1.0855 0.4576 11.00000 0.05 0.12 Q79 1 0.9380 0.7224 0.2790 11.00000 0.05 0.12 Q80 1 1.5460 1.2943 0.5402 11.00000 0.05 0.12 Q81 1 1.7740 1.2265 0.4497 11.00000 0.05 0.12 Q82 1 0.4985 0.4043 -0.0619 11.00000 0.05 0.12 Q83 1 0.9223 0.8434 0.2206 11.00000 0.05 0.12 Q84 1 1.1052 0.6208 0.5293 11.00000 0.05 0.12 Q85 1 0.8718 0.6246 0.3214 11.00000 0.05 0.12 Q86 1 0.9072 0.8790 0.1697 11.00000 0.05 0.12 Q87 1 1.3874 0.9898 0.3509 11.00000 0.05 0.12 Q88 1 1.5504 1.0201 0.4036 11.00000 0.05 0.12 Q89 1 0.3979 0.6651 0.1482 11.00000 0.05 0.12 Q90 1 1.0641 0.6827 0.2663 11.00000 0.05 0.12 Q91 1 1.5060 1.4268 0.2768 11.00000 0.05 0.12 Q92 1 1.4796 1.2779 0.2712 11.00000 0.05 0.12 Q93 1 0.9641 0.5500 0.4493 11.00000 0.05 0.12 Q94 1 1.4029 1.2970 0.5893 11.00000 0.05 0.12 Q95 1 0.8943 0.9919 0.1172 11.00000 0.05 0.12 Q96 1 0.3882 -0.1372 0.0837 11.00000 0.05 0.12 Q97 1 0.8447 0.3358 0.0720 11.00000 0.05 0.12 Q98 1 0.7722 0.5452 0.1296 11.00000 0.05 0.12 Q99 1 0.8547 0.5273 0.3928 11.00000 0.05 0.12 Q100 1 1.0624 0.9031 -0.0536 11.00000 0.05 0.12 Q101 1 1.1683 0.6134 0.5357 11.00000 0.05 0.12 Q102 1 1.2905 1.5193 0.3368 11.00000 0.05 0.12 Q103 1 1.2619 1.2168 0.3833 11.00000 0.05 0.12 Q104 1 0.9718 1.0110 -0.1328 11.00000 0.05 0.12 Q105 1 1.1709 0.7517 0.3117 11.00000 0.05 0.12 Q106 1 0.7119 0.0212 0.1567 11.00000 0.05 0.12 Q107 1 1.2428 0.3027 0.6778 11.00000 0.05 0.12 ; _shelx_res_checksum 97393 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.6280(4) 0.2522(7) 0.1009(4) 0.055(2) Uani d 1 . . O O2 0.4526(4) 0.0692(7) 0.0177(3) 0.0621(19) Uani d 1 . . O O3 0.4074(4) 0.0905(8) -0.0993(4) 0.074(2) Uani d 1 . . O O4 0.3810(4) 0.3139(7) -0.0770(3) 0.0605(19) Uani d 1 . . O O5 0.3201(5) 0.2320(9) 0.0859(5) 0.086(3) Uani d 1 . . O O6 0.4501(5) 0.2353(9) 0.1429(4) 0.084(3) Uani d 1 . . O O7 1.3653(4) 1.3074(7) 0.3981(4) 0.0562(19) Uani d 1 . . O O8 1.5313(3) 1.1102(6) 0.4867(3) 0.0567(18) Uani d 1 . . O O9 1.5835(4) 1.1426(8) 0.6019(3) 0.070(2) Uani d 1 . . O O10 1.6183(4) 1.3590(7) 0.5719(3) 0.060(2) Uani d 1 . . O O11 1.5438(5) 1.2402(8) 0.3574(4) 0.072(2) Uani d 1 . . O O12 1.6742(5) 1.2566(8) 0.4102(5) 0.077(3) Uani d 1 . . N N1 0.9282(5) 0.6798(10) 0.1592(4) 0.052(2) Uani d 1 . . H H1 0.954839 0.711788 0.198271 0.062 Uiso calc 1 . . N N2 0.9761(5) 0.5749(9) 0.2972(4) 0.053(2) Uani d 1 . . N N3 1.0756(5) 0.8169(10) 0.3437(4) 0.049(2) Uani d 1 . . H H3 1.047742 0.788022 0.304487 0.058 Uiso calc 1 . . N N4 1.0283(5) 0.9229(9) 0.2052(4) 0.051(2) Uani d 1 . . C C1 0.9184(6) 0.7499(13) 0.0974(6) 0.051(3) Uani d 1 . . C C2 0.8702(6) 0.6644(13) 0.0490(5) 0.058(3) Uani d 1 . . H H2 0.851864 0.686988 0.002081 0.069 Uiso calc 1 . . C C3 0.8544(6) 0.5465(13) 0.0794(5) 0.057(3) Uani d 1 . . H H3A 0.824321 0.470900 0.057576 0.068 Uiso calc 1 . . C C4 0.8907(6) 0.5536(13) 0.1512(5) 0.054(3) Uani d 1 . . C C5 0.8838(6) 0.4574(12) 0.2028(6) 0.051(3) Uani d 1 . . C C6 0.9206(6) 0.4714(12) 0.2727(6) 0.053(3) Uani d 1 . . C C7 0.9028(6) 0.3823(12) 0.3261(5) 0.060(3) Uani d 1 . . H H7 0.865585 0.307189 0.321197 0.072 Uiso calc 1 . . C C8 0.9496(7) 0.4261(12) 0.3849(6) 0.063(3) Uani d 1 . . H H8 0.952624 0.386823 0.429422 0.076 Uiso calc 1 . . C C9 0.9933(6) 0.5434(12) 0.3664(5) 0.051(3) Uani d 1 . . C C10 1.0500(6) 0.6170(13) 0.4145(5) 0.056(3) Uani d 1 . . C C11 1.0844(7) 0.7422(13) 0.4040(6) 0.054(3) Uani d 1 . . C C12 1.1346(6) 0.8275(14) 0.4543(5) 0.059(3) Uani d 1 . . H H12 1.153168 0.803771 0.500976 0.070 Uiso calc 1 . . C C13 1.1507(6) 0.9472(14) 0.4235(5) 0.061(3) Uani d 1 . . H H13 1.180582 1.022649 0.445768 0.073 Uiso calc 1 . . C C14 1.1153(6) 0.9417(13) 0.3519(6) 0.053(3) Uani d 1 . . C C15 1.1196(6) 1.0370(12) 0.3012(5) 0.050(3) Uani d 1 . . C C16 1.0816(7) 1.0226(11) 0.2316(6) 0.049(3) Uani d 1 . . C C17 1.0976(6) 1.1156(12) 0.1770(5) 0.058(3) Uani d 1 . . H H17 1.133870 1.192042 0.181368 0.070 Uiso calc 1 . . C C18 1.0498(6) 1.0703(13) 0.1188(6) 0.064(3) Uani d 1 . . H H18 1.045910 1.110858 0.074498 0.077 Uiso calc 1 . . C C19 1.0070(6) 0.9524(12) 0.1354(5) 0.052(3) Uani d 1 . . C C20 0.9532(6) 0.8757(12) 0.0885(5) 0.051(3) Uani d 1 . . C C21 0.8339(6) 0.3312(13) 0.1840(5) 0.049(3) Uani d 1 . . C C22 0.7523(6) 0.3413(12) 0.1525(5) 0.048(3) Uani d 1 . . H H22 0.727941 0.429648 0.144192 0.057 Uiso calc 1 . . C C23 0.7065(7) 0.2250(13) 0.1333(6) 0.053(3) Uani d 1 . . C C24 0.7389(6) 0.0975(13) 0.1464(5) 0.053(3) Uani d 1 . . H H24 0.706349 0.017820 0.134432 0.064 Uiso calc 1 . . C C25 0.8204(6) 0.0842(12) 0.1774(5) 0.055(3) Uani d 1 . . H H25 0.844028 -0.004627 0.185696 0.066 Uiso calc 1 . . C C26 0.8656(8) 0.1981(14) 0.1955(6) 0.060(3) Uani d 1 . . H H26 0.920947 0.187429 0.216917 0.071 Uiso calc 1 . . C C27 1.0745(6) 0.5497(12) 0.4833(5) 0.065(3) Uani d 1 . . C C28 1.0459(6) 0.5893(12) 0.5418(5) 0.067(3) Uani d 1 . . H H28 1.007720 0.662807 0.539723 0.081 Uiso calc 1 . . C C29 1.0724(7) 0.5228(12) 0.6048(6) 0.072(3) Uani d 1 . . H H29 1.053241 0.554033 0.644960 0.086 Uiso calc 1 . . C C30 1.1252(7) 0.4141(13) 0.6092(6) 0.076(3) Uani d 1 . . C C31 1.1543(9) 0.3733(16) 0.5514(6) 0.110(4) Uani d 1 . . H H31 1.192796 0.300186 0.553893 0.132 Uiso calc 1 . . C C32 1.1274(8) 0.4387(14) 0.4884(6) 0.099(4) Uani d 1 . . H H32 1.146059 0.406078 0.448177 0.119 Uiso calc 1 . . C C33 1.1643(6) 1.1698(14) 0.3184(5) 0.055(3) Uani d 1 . . C C34 1.2460(6) 1.1691(13) 0.3504(5) 0.055(3) Uani d 1 . . H H34 1.273934 1.084639 0.361723 0.066 Uiso calc 1 . . C C35 1.2854(7) 1.2934(13) 0.3654(6) 0.052(3) Uani d 1 . . C C36 1.2480(7) 1.4171(14) 0.3472(5) 0.058(3) Uani d 1 . . H H36 1.277357 1.501065 0.355812 0.069 Uiso calc 1 . . C C37 1.1666(7) 1.4177(14) 0.3162(5) 0.062(3) Uani d 1 . . H H37 1.139301 1.502405 0.303901 0.074 Uiso calc 1 . . C C38 1.1250(7) 1.2925(13) 0.3030(6) 0.054(3) Uani d 1 . . H H38 1.068714 1.292745 0.283148 0.065 Uiso calc 1 . . C C39 0.9263(6) 0.9432(12) 0.0195(5) 0.063(3) Uani d 1 . . C C40 0.8759(8) 1.0579(14) 0.0147(6) 0.098(4) Uani d 1 . . H H40 0.859411 1.091771 0.055595 0.118 Uiso calc 1 . . C C41 0.8481(9) 1.1264(16) -0.0468(5) 0.110(4) Uani d 1 . . H H41 0.814105 1.205354 -0.047514 0.132 Uiso calc 1 . . C C42 0.8706(8) 1.0778(13) -0.1061(5) 0.078(3) Uani d 1 . . C C43 0.9260(7) 0.9735(12) -0.1015(5) 0.073(3) Uani d 1 . . H H43 0.946518 0.945562 -0.141692 0.088 Uiso calc 1 . . C C44 0.9535(6) 0.9070(12) -0.0399(5) 0.063(3) Uani d 1 . . H H44 0.992116 0.834364 -0.038827 0.076 Uiso calc 1 . . C C45 0.5781(6) 0.1336(11) 0.0795(5) 0.060(3) Uani d 1 . . H H45A 0.565493 0.082156 0.119858 0.072 Uiso calc 1 . . H H45B 0.606285 0.071094 0.051268 0.072 Uiso calc 1 . . C C46 0.5012(6) 0.1911(11) 0.0378(5) 0.053(3) Uani d 1 . . H H46 0.514950 0.237211 -0.004232 0.064 Uiso calc 1 . . C C47 0.3836(6) 0.0943(12) -0.0331(5) 0.065(3) Uani d 1 . . H H47 0.341382 0.021761 -0.030353 0.079 Uiso calc 1 . . C C48 0.3465(7) 0.2341(13) -0.0271(7) 0.063(4) Uani d 1 . . H H48 0.285845 0.228251 -0.041341 0.075 Uiso calc 1 . . C C49 0.3927(9) 0.2233(13) -0.1306(6) 0.070(4) Uani d 1 . . C C50 0.4691(9) 0.2674(12) -0.1574(6) 0.095(5) Uani d 1 . . H H50A 0.479188 0.204350 -0.194016 0.114 Uiso calc 1 . . H H50B 0.515870 0.265140 -0.119912 0.114 Uiso calc 1 . . H H50C 0.461893 0.361185 -0.175812 0.114 Uiso calc 1 . . C C51 0.3169(9) 0.2198(14) -0.1862(7) 0.113(6) Uani d 1 . . H H51A 0.268674 0.198315 -0.165108 0.136 Uiso calc 1 . . H H51B 0.323673 0.148938 -0.220204 0.136 Uiso calc 1 . . H H51C 0.309512 0.309840 -0.208816 0.136 Uiso calc 1 . . C C52 0.3656(6) 0.3051(12) 0.0420(5) 0.064(3) Uani d 1 . . H H52 0.348897 0.404161 0.038176 0.077 Uiso calc 1 . . C C53 0.4551(5) 0.2910(11) 0.0764(4) 0.054(3) Uani d 1 . . H H53 0.482634 0.382993 0.080629 0.065 Uiso calc 1 . . C C54 0.3668(10) 0.2366(17) 0.1536(8) 0.092(4) Uani d 1 . . C C55 0.3511(8) 0.1118(16) 0.1918(6) 0.117(5) Uani d 1 . . H H55A 0.363465 0.030114 0.166114 0.140 Uiso calc 1 . . H H55B 0.293452 0.109818 0.197542 0.140 Uiso calc 1 . . H H55C 0.385852 0.112468 0.237035 0.140 Uiso calc 1 . . C C56 0.3521(9) 0.3716(16) 0.1898(6) 0.125(5) Uani d 1 . . H H56A 0.296732 0.371387 0.201381 0.150 Uiso calc 1 . . H H56B 0.357796 0.449309 0.159176 0.150 Uiso calc 1 . . H H56C 0.392188 0.380598 0.231969 0.150 Uiso calc 1 . . C C57 1.1547(8) 0.3440(15) 0.6773(6) 0.101(5) Uani d 1 . . H H57A 1.210454 0.374699 0.695308 0.121 Uiso calc 1 . . H H57B 1.154416 0.243935 0.670676 0.121 Uiso calc 1 . . H H57C 1.118369 0.367984 0.710108 0.121 Uiso calc 1 . . C C58 1.4079(6) 1.1838(11) 0.4224(5) 0.060(3) Uani d 1 . . H H58A 1.416401 1.123981 0.383511 0.072 Uiso calc 1 . . H H58B 1.377085 1.131685 0.452991 0.072 Uiso calc 1 . . C C59 1.4896(6) 1.2342(10) 0.4619(6) 0.054(3) Uani d 1 . . H H59 1.479168 1.290577 0.502015 0.065 Uiso calc 1 . . C C60 1.6037(6) 1.1311(11) 0.5346(5) 0.059(3) Uani d 1 . . H H60 1.641813 1.051695 0.532919 0.071 Uiso calc 1 . . C C61 1.6481(7) 1.2662(11) 0.5249(6) 0.058(4) Uani d 1 . . H H61 1.708568 1.253709 0.537920 0.069 Uiso calc 1 . . C C62 1.6012(9) 1.2775(13) 0.6297(7) 0.074(4) Uani d 1 . . C C63 1.5287(8) 1.3348(14) 0.6537(5) 0.090(4) Uani d 1 . . H H63A 1.514538 1.277231 0.690929 0.107 Uiso calc 1 . . H H63B 1.482699 1.336476 0.615538 0.107 Uiso calc 1 . . H H63C 1.540511 1.428708 0.670703 0.107 Uiso calc 1 . . C C64 1.6765(9) 1.2745(12) 0.6847(7) 0.096(5) Uani d 1 . . H H64A 1.692052 1.368875 0.698831 0.115 Uiso calc 1 . . H H64B 1.721544 1.230188 0.666383 0.115 Uiso calc 1 . . H H64C 1.664547 1.222335 0.724492 0.115 Uiso calc 1 . . C C65 1.5385(6) 1.3168(12) 0.4201(5) 0.056(3) Uani d 1 . . H H65 1.512922 1.409154 0.409102 0.068 Uiso calc 1 . . C C66 1.6281(5) 1.3319(11) 0.4543(5) 0.057(3) Uani d 1 . . H H66 1.644508 1.431172 0.456519 0.068 Uiso calc 1 . . C C67 1.6247(9) 1.2509(15) 0.3435(8) 0.082(4) Uani d 1 . . C C68 1.6470(9) 1.1198(14) 0.3099(6) 0.120(5) Uani d 1 . . H H68A 1.614297 1.111910 0.263887 0.144 Uiso calc 1 . . H H68B 1.636055 1.040584 0.337821 0.144 Uiso calc 1 . . H H68C 1.705259 1.121701 0.306012 0.144 Uiso calc 1 . . C C69 1.6335(9) 1.3803(16) 0.3025(6) 0.110(5) Uani d 1 . . H H69A 1.596684 1.375469 0.258318 0.132 Uiso calc 1 . . H H69B 1.690162 1.388572 0.294416 0.132 Uiso calc 1 . . H H69C 1.619521 1.460792 0.328301 0.132 Uiso calc 1 . . C C70 0.8407(8) 1.1557(16) -0.1738(5) 0.102(4) Uani d 1 . . H H70A 0.796702 1.103204 -0.201547 0.122 Uiso calc 1 . . H H70B 0.886274 1.166548 -0.199439 0.122 Uiso calc 1 . . H H70C 0.820220 1.246651 -0.163348 0.122 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.039(4) 0.055(5) 0.065(5) -0.007(4) -0.007(4) 0.004(4) O2 0.061(4) 0.048(5) 0.068(4) -0.011(4) -0.017(3) 0.005(3) O3 0.094(5) 0.060(6) 0.060(5) 0.002(4) -0.011(4) -0.001(4) O4 0.072(5) 0.050(5) 0.055(5) 0.003(4) -0.005(4) 0.000(4) O5 0.058(5) 0.113(7) 0.093(6) 0.013(5) 0.027(5) 0.035(5) O6 0.074(5) 0.122(7) 0.059(6) 0.011(5) 0.020(4) 0.017(4) O7 0.041(4) 0.047(4) 0.074(5) -0.003(4) -0.010(3) 0.009(4) O8 0.054(4) 0.036(4) 0.074(4) -0.002(3) -0.009(3) 0.005(3) O9 0.088(5) 0.054(6) 0.064(5) -0.008(4) -0.001(4) 0.003(4) O10 0.065(5) 0.051(5) 0.061(5) 0.004(4) 0.003(4) -0.004(4) O11 0.060(5) 0.090(6) 0.064(6) -0.006(4) 0.005(4) -0.012(4) O12 0.052(5) 0.090(7) 0.091(7) 0.001(4) 0.017(5) -0.003(5) N1 0.045(5) 0.063(7) 0.043(6) -0.005(5) -0.003(4) -0.007(5) N2 0.037(5) 0.064(7) 0.054(6) -0.002(5) 0.000(4) -0.013(5) N3 0.041(5) 0.061(6) 0.043(6) 0.003(5) 0.001(4) -0.007(5) N4 0.041(5) 0.054(6) 0.058(6) -0.002(5) 0.010(4) 0.003(5) C1 0.038(6) 0.071(7) 0.042(7) -0.005(5) 0.001(5) -0.001(6) C2 0.040(6) 0.073(9) 0.057(7) -0.013(7) 0.001(6) 0.007(7) C3 0.047(7) 0.069(9) 0.051(7) -0.005(6) -0.005(6) -0.011(7) C4 0.041(7) 0.073(10) 0.044(7) 0.007(7) -0.003(6) -0.007(6) C5 0.032(6) 0.057(8) 0.062(8) 0.000(6) 0.003(6) -0.008(7) C6 0.026(6) 0.079(9) 0.051(7) 0.002(6) -0.003(5) 0.006(7) C7 0.054(7) 0.069(9) 0.055(7) -0.014(6) 0.001(6) -0.005(6) C8 0.068(8) 0.064(9) 0.059(7) -0.004(7) 0.010(6) 0.005(7) C9 0.044(7) 0.061(9) 0.049(7) -0.003(6) 0.006(6) 0.002(6) C10 0.048(6) 0.064(9) 0.054(7) 0.005(6) -0.004(5) 0.000(7) C11 0.050(8) 0.066(8) 0.045(8) 0.010(6) 0.001(6) -0.002(7) C12 0.040(6) 0.085(10) 0.048(7) -0.003(7) -0.001(5) -0.018(8) C13 0.045(7) 0.083(10) 0.051(7) -0.015(7) -0.003(6) -0.004(7) C14 0.033(6) 0.066(9) 0.060(8) -0.004(6) 0.004(6) -0.008(7) C15 0.033(6) 0.068(8) 0.046(7) -0.002(6) -0.005(5) -0.004(6) C16 0.043(7) 0.047(7) 0.058(7) 0.002(6) 0.013(6) 0.002(6) C17 0.052(7) 0.055(8) 0.068(8) -0.003(6) 0.008(6) -0.007(7) C18 0.052(7) 0.074(10) 0.062(8) -0.010(7) 0.000(6) 0.003(7) C19 0.049(7) 0.053(8) 0.053(7) 0.006(7) 0.007(6) 0.001(6) C20 0.042(6) 0.072(8) 0.041(6) 0.007(6) 0.011(5) 0.002(6) C21 0.040(6) 0.059(9) 0.046(7) 0.003(7) 0.001(5) -0.010(6) C22 0.043(7) 0.039(7) 0.057(7) 0.001(6) -0.001(5) 0.003(6) C23 0.040(7) 0.060(9) 0.055(8) 0.006(6) -0.005(6) 0.002(6) C24 0.043(6) 0.058(8) 0.055(7) -0.011(6) -0.004(5) -0.007(6) C25 0.056(7) 0.052(8) 0.053(7) 0.014(6) -0.001(6) -0.013(6) C26 0.055(8) 0.069(9) 0.053(8) 0.008(8) 0.004(6) -0.007(7) C27 0.055(6) 0.082(7) 0.054(5) 0.005(5) -0.001(5) -0.003(6) C28 0.067(6) 0.074(7) 0.061(6) -0.015(6) 0.010(5) -0.002(5) C29 0.072(7) 0.086(8) 0.056(5) -0.027(5) 0.009(5) -0.005(6) C30 0.074(7) 0.094(8) 0.055(5) -0.014(6) 0.000(5) 0.008(6) C31 0.117(8) 0.137(9) 0.075(6) 0.050(7) 0.007(6) 0.023(7) C32 0.100(8) 0.135(9) 0.060(6) 0.046(7) 0.005(6) 0.012(7) C33 0.035(7) 0.071(9) 0.058(7) -0.001(7) 0.005(6) -0.006(7) C34 0.048(7) 0.055(8) 0.061(7) 0.002(7) 0.003(6) 0.003(6) C35 0.043(7) 0.063(9) 0.050(7) -0.006(7) 0.002(6) 0.005(6) C36 0.049(7) 0.063(9) 0.059(7) 0.001(6) 0.000(5) 0.005(6) C37 0.050(7) 0.063(9) 0.070(8) 0.009(6) 0.001(6) 0.006(7) C38 0.040(7) 0.068(9) 0.055(7) 0.007(7) 0.007(6) -0.010(7) C39 0.057(6) 0.083(7) 0.048(5) -0.001(5) 0.007(5) 0.005(6) C40 0.108(8) 0.136(9) 0.050(5) 0.042(7) 0.009(6) 0.014(6) C41 0.128(8) 0.140(9) 0.058(6) 0.043(7) 0.000(7) 0.016(6) C42 0.086(7) 0.102(8) 0.041(5) -0.016(6) -0.003(5) -0.002(5) C43 0.074(7) 0.102(8) 0.045(5) -0.021(6) 0.015(5) -0.004(6) C44 0.060(6) 0.080(7) 0.051(5) -0.011(5) 0.014(5) 0.000(5) C45 0.048(6) 0.065(8) 0.064(6) -0.002(6) 0.002(5) -0.007(6) C46 0.044(6) 0.050(7) 0.063(7) -0.008(6) -0.001(6) 0.010(6) C47 0.048(6) 0.059(9) 0.079(8) -0.011(6) -0.019(6) 0.006(7) C48 0.041(7) 0.067(9) 0.075(10) 0.001(6) -0.004(7) 0.019(7) C49 0.102(11) 0.063(10) 0.040(8) -0.007(8) -0.008(8) 0.003(6) C50 0.147(13) 0.091(11) 0.053(8) 0.012(9) 0.036(8) 0.003(6) C51 0.144(14) 0.100(13) 0.071(10) 0.005(10) -0.054(10) 0.002(8) C52 0.047(6) 0.083(9) 0.062(7) -0.006(6) 0.009(5) 0.003(7) C53 0.036(5) 0.082(9) 0.045(6) -0.002(6) 0.006(5) 0.001(6) C54 0.081(7) 0.122(8) 0.079(7) 0.015(7) 0.028(6) 0.029(6) C55 0.098(9) 0.139(11) 0.123(10) 0.034(9) 0.051(8) 0.059(9) C56 0.141(12) 0.149(11) 0.093(9) 0.064(11) 0.041(8) 0.018(8) C57 0.107(10) 0.115(11) 0.068(7) -0.038(9) -0.021(7) 0.026(8) C58 0.054(7) 0.048(7) 0.076(8) -0.001(6) 0.002(6) 0.012(6) C59 0.052(7) 0.041(7) 0.066(7) -0.009(6) 0.003(6) 0.010(6) C60 0.048(6) 0.059(8) 0.066(7) 0.001(6) -0.009(6) -0.002(6) C61 0.047(8) 0.051(9) 0.071(10) -0.005(6) -0.003(7) -0.002(7) C62 0.091(11) 0.065(11) 0.061(9) 0.010(8) -0.003(8) 0.008(7) C63 0.120(11) 0.095(10) 0.056(7) 0.005(10) 0.018(7) -0.005(7) C64 0.137(13) 0.057(10) 0.074(10) 0.002(8) -0.038(10) -0.004(7) C65 0.053(6) 0.062(8) 0.051(6) -0.005(6) -0.001(5) 0.002(6) C66 0.044(6) 0.054(7) 0.072(7) 0.000(6) 0.007(5) -0.002(6) C67 0.069(9) 0.093(11) 0.088(11) 0.002(8) 0.022(8) -0.018(8) C68 0.157(14) 0.096(12) 0.127(12) 0.004(11) 0.079(11) -0.037(10) C69 0.113(11) 0.127(14) 0.100(10) 0.006(10) 0.048(8) 0.026(10) C70 0.122(10) 0.120(11) 0.056(7) -0.030(9) -0.008(7) 0.021(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C23 O1 C45 . . 115.8(8) ? C47 O2 C46 . . 113.7(7) ? C47 O3 C49 . . 108.6(9) ? C49 O4 C48 . . 107.1(9) ? C52 O5 C54 . . 107.0(9) ? C54 O6 C53 . . 109.4(9) ? C35 O7 C58 . . 117.1(8) ? C60 O8 C59 . . 114.6(7) ? C60 O9 C62 . . 111.3(9) ? C61 O10 C62 . . 107.2(8) ? C67 O11 C65 . . 108.5(8) ? C67 O12 C66 . . 107.0(8) ? C4 N1 C1 . . 110.7(9) ? C4 N1 H1 . . 124.6 ? C1 N1 H1 . . 124.6 ? C9 N2 C6 . . 101.6(9) ? C14 N3 C11 . . 112.4(9) ? C14 N3 H3 . . 123.8 ? C11 N3 H3 . . 123.8 ? C16 N4 C19 . . 106.0(9) ? C20 C1 N1 . . 124.0(10) ? C20 C1 C2 . . 129.8(11) ? N1 C1 C2 . . 106.2(10) ? C3 C2 C1 . . 109.3(10) ? C3 C2 H2 . . 125.4 ? C1 C2 H2 . . 125.4 ? C2 C3 C4 . . 108.5(10) ? C2 C3 H3A . . 125.7 ? C4 C3 H3A . . 125.7 ? N1 C4 C5 . . 127.1(10) ? N1 C4 C3 . . 105.3(10) ? C5 C4 C3 . . 127.5(11) ? C4 C5 C6 . . 124.6(10) ? C4 C5 C21 . . 118.5(10) ? C6 C5 C21 . . 116.9(11) ? N2 C6 C5 . . 124.1(11) ? N2 C6 C7 . . 112.6(9) ? C5 C6 C7 . . 123.4(11) ? C8 C7 C6 . . 106.5(10) ? C8 C7 H7 . . 126.8 ? C6 C7 H7 . . 126.8 ? C7 C8 C9 . . 105.9(9) ? C7 C8 H8 . . 127.1 ? C9 C8 H8 . . 127.1 ? N2 C9 C10 . . 123.9(11) ? N2 C9 C8 . . 113.4(9) ? C10 C9 C8 . . 122.7(10) ? C11 C10 C9 . . 126.4(10) ? C11 C10 C27 . . 117.6(10) ? C9 C10 C27 . . 116.0(11) ? C10 C11 N3 . . 127.4(10) ? C10 C11 C12 . . 127.6(11) ? N3 C11 C12 . . 104.9(11) ? C13 C12 C11 . . 108.5(10) ? C13 C12 H12 . . 125.8 ? C11 C12 H12 . . 125.8 ? C12 C13 C14 . . 109.1(11) ? C12 C13 H13 . . 125.4 ? C14 C13 H13 . . 125.4 ? C15 C14 N3 . . 126.1(10) ? C15 C14 C13 . . 128.9(11) ? N3 C14 C13 . . 105.0(11) ? C14 C15 C16 . . 124.8(11) ? C14 C15 C33 . . 119.9(9) ? C16 C15 C33 . . 115.3(11) ? N4 C16 C15 . . 126.7(10) ? N4 C16 C17 . . 110.1(9) ? C15 C16 C17 . . 123.1(10) ? C18 C17 C16 . . 105.8(10) ? C18 C17 H17 . . 127.1 ? C16 C17 H17 . . 127.1 ? C17 C18 C19 . . 108.2(10) ? C17 C18 H18 . . 125.9 ? C19 C18 H18 . . 125.9 ? C20 C19 N4 . . 125.3(11) ? C20 C19 C18 . . 124.9(10) ? N4 C19 C18 . . 109.8(9) ? C1 C20 C19 . . 128.9(10) ? C1 C20 C39 . . 115.6(10) ? C19 C20 C39 . . 115.4(10) ? C22 C21 C26 . . 116.6(11) ? C22 C21 C5 . . 120.7(11) ? C26 C21 C5 . . 122.7(9) ? C23 C22 C21 . . 120.9(11) ? C23 C22 H22 . . 119.5 ? C21 C22 H22 . . 119.5 ? C24 C23 O1 . . 125.3(10) ? C24 C23 C22 . . 120.8(10) ? O1 C23 C22 . . 113.9(10) ? C23 C24 C25 . . 119.5(11) ? C23 C24 H24 . . 120.2 ? C25 C24 H24 . . 120.2 ? C26 C25 C24 . . 119.8(11) ? C26 C25 H25 . . 120.1 ? C24 C25 H25 . . 120.1 ? C25 C26 C21 . . 122.4(11) ? C25 C26 H26 . . 118.8 ? C21 C26 H26 . . 118.8 ? C28 C27 C32 . . 117.4(11) ? C28 C27 C10 . . 123.9(10) ? C32 C27 C10 . . 118.6(9) ? C27 C28 C29 . . 120.9(11) ? C27 C28 H28 . . 119.6 ? C29 C28 H28 . . 119.6 ? C30 C29 C28 . . 121.2(11) ? C30 C29 H29 . . 119.4 ? C28 C29 H29 . . 119.4 ? C29 C30 C31 . . 118.7(12) ? C29 C30 C57 . . 121.1(11) ? C31 C30 C57 . . 120.2(12) ? C30 C31 C32 . . 120.2(12) ? C30 C31 H31 . . 119.9 ? C32 C31 H31 . . 119.9 ? C27 C32 C31 . . 121.5(11) ? C27 C32 H32 . . 119.2 ? C31 C32 H32 . . 119.2 ? C38 C33 C34 . . 119.7(12) ? C38 C33 C15 . . 119.9(10) ? C34 C33 C15 . . 120.4(12) ? C35 C34 C33 . . 118.9(12) ? C35 C34 H34 . . 120.6 ? C33 C34 H34 . . 120.6 ? C36 C35 C34 . . 122.1(11) ? C36 C35 O7 . . 113.1(10) ? C34 C35 O7 . . 124.8(11) ? C35 C36 C37 . . 119.0(12) ? C35 C36 H36 . . 120.5 ? C37 C36 H36 . . 120.5 ? C36 C37 C38 . . 119.5(12) ? C36 C37 H37 . . 120.3 ? C38 C37 H37 . . 120.3 ? C33 C38 C37 . . 120.8(11) ? C33 C38 H38 . . 119.6 ? C37 C38 H38 . . 119.6 ? C44 C39 C40 . . 115.3(11) ? C44 C39 C20 . . 124.7(10) ? C40 C39 C20 . . 119.8(9) ? C39 C40 C41 . . 123.5(11) ? C39 C40 H40 . . 118.2 ? C41 C40 H40 . . 118.2 ? C42 C41 C40 . . 118.8(12) ? C42 C41 H41 . . 120.6 ? C40 C41 H41 . . 120.6 ? C43 C42 C41 . . 118.4(12) ? C43 C42 C70 . . 122.6(11) ? C41 C42 C70 . . 118.4(12) ? C42 C43 C44 . . 121.7(11) ? C42 C43 H43 . . 119.1 ? C44 C43 H43 . . 119.1 ? C39 C44 C43 . . 121.6(11) ? C39 C44 H44 . . 119.2 ? C43 C44 H44 . . 119.2 ? O1 C45 C46 . . 105.0(8) ? O1 C45 H45A . . 110.8 ? C46 C45 H45A . . 110.8 ? O1 C45 H45B . . 110.8 ? C46 C45 H45B . . 110.8 ? H45A C45 H45B . . 108.8 ? O2 C46 C45 . . 103.3(8) ? O2 C46 C53 . . 110.9(8) ? C45 C46 C53 . . 114.5(8) ? O2 C46 H46 . . 109.3 ? C45 C46 H46 . . 109.3 ? C53 C46 H46 . . 109.3 ? O2 C47 O3 . . 109.4(8) ? O2 C47 C48 . . 113.2(9) ? O3 C47 C48 . . 105.8(9) ? O2 C47 H47 . . 109.4 ? O3 C47 H47 . . 109.4 ? C48 C47 H47 . . 109.4 ? O4 C48 C47 . . 102.7(10) ? O4 C48 C52 . . 108.7(9) ? C47 C48 C52 . . 117.0(10) ? O4 C48 H48 . . 109.4 ? C47 C48 H48 . . 109.4 ? C52 C48 H48 . . 109.4 ? O4 C49 O3 . . 105.8(9) ? O4 C49 C50 . . 108.1(10) ? O3 C49 C50 . . 108.2(11) ? O4 C49 C51 . . 110.7(12) ? O3 C49 C51 . . 110.5(10) ? C50 C49 C51 . . 113.2(12) ? C49 C50 H50A . . 109.5 ? C49 C50 H50B . . 109.5 ? H50A C50 H50B . . 109.5 ? C49 C50 H50C . . 109.5 ? H50A C50 H50C . . 109.5 ? H50B C50 H50C . . 109.5 ? C49 C51 H51A . . 109.5 ? C49 C51 H51B . . 109.5 ? H51A C51 H51B . . 109.5 ? C49 C51 H51C . . 109.5 ? H51A C51 H51C . . 109.5 ? H51B C51 H51C . . 109.5 ? O5 C52 C48 . . 105.4(9) ? O5 C52 C53 . . 104.8(8) ? C48 C52 C53 . . 113.8(9) ? O5 C52 H52 . . 110.8 ? C48 C52 H52 . . 110.8 ? C53 C52 H52 . . 110.8 ? O6 C53 C46 . . 109.1(9) ? O6 C53 C52 . . 104.1(8) ? C46 C53 C52 . . 111.4(8) ? O6 C53 H53 . . 110.7 ? C46 C53 H53 . . 110.7 ? C52 C53 H53 . . 110.7 ? O6 C54 O5 . . 104.6(10) ? O6 C54 C55 . . 108.9(12) ? O5 C54 C55 . . 109.7(13) ? O6 C54 C56 . . 107.9(13) ? O5 C54 C56 . . 110.9(12) ? C55 C54 C56 . . 114.3(12) ? C54 C55 H55A . . 109.5 ? C54 C55 H55B . . 109.5 ? H55A C55 H55B . . 109.5 ? C54 C55 H55C . . 109.5 ? H55A C55 H55C . . 109.5 ? H55B C55 H55C . . 109.5 ? C54 C56 H56A . . 109.5 ? C54 C56 H56B . . 109.5 ? H56A C56 H56B . . 109.5 ? C54 C56 H56C . . 109.5 ? H56A C56 H56C . . 109.5 ? H56B C56 H56C . . 109.5 ? C30 C57 H57A . . 109.5 ? C30 C57 H57B . . 109.5 ? H57A C57 H57B . . 109.5 ? C30 C57 H57C . . 109.5 ? H57A C57 H57C . . 109.5 ? H57B C57 H57C . . 109.5 ? O7 C58 C59 . . 104.4(8) ? O7 C58 H58A . . 110.9 ? C59 C58 H58A . . 110.9 ? O7 C58 H58B . . 110.9 ? C59 C58 H58B . . 110.9 ? H58A C58 H58B . . 108.9 ? O8 C59 C65 . . 111.6(9) ? O8 C59 C58 . . 104.0(7) ? C65 C59 C58 . . 114.2(8) ? O8 C59 H59 . . 108.9 ? C65 C59 H59 . . 108.9 ? C58 C59 H59 . . 108.9 ? O8 C60 O9 . . 109.2(8) ? O8 C60 C61 . . 114.3(8) ? O9 C60 C61 . . 103.9(9) ? O8 C60 H60 . . 109.7 ? O9 C60 H60 . . 109.7 ? C61 C60 H60 . . 109.7 ? O10 C61 C66 . . 106.3(9) ? O10 C61 C60 . . 103.5(9) ? C66 C61 C60 . . 116.0(9) ? O10 C61 H61 . . 110.2 ? C66 C61 H61 . . 110.2 ? C60 C61 H61 . . 110.2 ? O9 C62 O10 . . 104.5(10) ? O9 C62 C63 . . 110.0(12) ? O10 C62 C63 . . 108.7(10) ? O9 C62 C64 . . 110.5(10) ? O10 C62 C64 . . 109.2(12) ? C63 C62 C64 . . 113.5(12) ? C62 C63 H63A . . 109.5 ? C62 C63 H63B . . 109.5 ? H63A C63 H63B . . 109.5 ? C62 C63 H63C . . 109.5 ? H63A C63 H63C . . 109.5 ? H63B C63 H63C . . 109.5 ? C62 C64 H64A . . 109.5 ? C62 C64 H64B . . 109.5 ? H64A C64 H64B . . 109.5 ? C62 C64 H64C . . 109.5 ? H64A C64 H64C . . 109.5 ? H64B C64 H64C . . 109.5 ? O11 C65 C59 . . 108.0(9) ? O11 C65 C66 . . 103.5(8) ? C59 C65 C66 . . 112.7(8) ? O11 C65 H65 . . 110.8 ? C59 C65 H65 . . 110.8 ? C66 C65 H65 . . 110.8 ? O12 C66 C61 . . 106.4(9) ? O12 C66 C65 . . 104.8(8) ? C61 C66 C65 . . 114.4(9) ? O12 C66 H66 . . 110.3 ? C61 C66 H66 . . 110.3 ? C65 C66 H66 . . 110.3 ? O11 C67 O12 . . 104.1(10) ? O11 C67 C68 . . 109.4(12) ? O12 C67 C68 . . 106.9(12) ? O11 C67 C69 . . 110.0(12) ? O12 C67 C69 . . 111.5(12) ? C68 C67 C69 . . 114.5(12) ? C67 C68 H68A . . 109.5 ? C67 C68 H68B . . 109.5 ? H68A C68 H68B . . 109.5 ? C67 C68 H68C . . 109.5 ? H68A C68 H68C . . 109.5 ? H68B C68 H68C . . 109.5 ? C67 C69 H69A . . 109.5 ? C67 C69 H69B . . 109.5 ? H69A C69 H69B . . 109.5 ? C67 C69 H69C . . 109.5 ? H69A C69 H69C . . 109.5 ? H69B C69 H69C . . 109.5 ? C42 C70 H70A . . 109.5 ? C42 C70 H70B . . 109.5 ? H70A C70 H70B . . 109.5 ? C42 C70 H70C . . 109.5 ? H70A C70 H70C . . 109.5 ? H70B C70 H70C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C23 . 1.378(12) ? O1 C45 . 1.439(11) ? O2 C47 . 1.412(10) ? O2 C46 . 1.450(11) ? O3 C47 . 1.424(11) ? O3 C49 . 1.432(13) ? O4 C49 . 1.412(14) ? O4 C48 . 1.441(13) ? O5 C52 . 1.427(12) ? O5 C54 . 1.430(15) ? O6 C54 . 1.429(15) ? O6 C53 . 1.433(11) ? O7 C35 . 1.380(12) ? O7 C58 . 1.435(11) ? O8 C60 . 1.416(9) ? O8 C59 . 1.433(11) ? O9 C60 . 1.423(11) ? O9 C62 . 1.432(14) ? O10 C61 . 1.435(13) ? O10 C62 . 1.453(14) ? O11 C67 . 1.414(15) ? O11 C65 . 1.457(12) ? O12 C67 . 1.433(15) ? O12 C66 . 1.444(11) ? N1 C4 . 1.370(14) ? N1 C1 . 1.381(13) ? N1 H1 . 0.8800 ? N2 C9 . 1.381(11) ? N2 C6 . 1.395(13) ? N3 C14 . 1.374(14) ? N3 C11 . 1.378(13) ? N3 H3 . 0.8800 ? N4 C16 . 1.356(13) ? N4 C19 . 1.394(12) ? C1 C20 . 1.373(14) ? C1 C2 . 1.410(14) ? C2 C3 . 1.338(14) ? C2 H2 . 0.9500 ? C3 C4 . 1.446(13) ? C3 H3A . 0.9500 ? C4 C5 . 1.399(14) ? C5 C6 . 1.419(13) ? C5 C21 . 1.490(15) ? C6 C7 . 1.429(13) ? C7 C8 . 1.354(13) ? C7 H7 . 0.9500 ? C8 C9 . 1.429(14) ? C8 H8 . 0.9500 ? C9 C10 . 1.414(14) ? C10 C11 . 1.373(14) ? C10 C27 . 1.501(14) ? C11 C12 . 1.446(14) ? C12 C13 . 1.356(15) ? C12 H12 . 0.9500 ? C13 C14 . 1.439(13) ? C13 H13 . 0.9500 ? C14 C15 . 1.371(14) ? C15 C16 . 1.421(13) ? C15 C33 . 1.498(16) ? C16 C17 . 1.461(13) ? C17 C18 . 1.356(13) ? C17 H17 . 0.9500 ? C18 C19 . 1.413(14) ? C18 H18 . 0.9500 ? C19 C20 . 1.390(14) ? C20 C39 . 1.510(13) ? C21 C22 . 1.396(13) ? C21 C26 . 1.399(16) ? C22 C23 . 1.378(14) ? C22 H22 . 0.9500 ? C23 C24 . 1.357(14) ? C24 C25 . 1.394(13) ? C24 H24 . 0.9500 ? C25 C26 . 1.350(15) ? C25 H25 . 0.9500 ? C26 H26 . 0.9500 ? C27 C28 . 1.370(10) ? C27 C32 . 1.382(10) ? C28 C29 . 1.404(10) ? C28 H28 . 0.9500 ? C29 C30 . 1.363(11) ? C29 H29 . 0.9500 ? C30 C31 . 1.367(10) ? C30 C57 . 1.513(15) ? C31 C32 . 1.401(10) ? C31 H31 . 0.9500 ? C32 H32 . 0.9500 ? C33 C38 . 1.368(15) ? C33 C34 . 1.397(13) ? C34 C35 . 1.380(15) ? C34 H34 . 0.9500 ? C35 C36 . 1.372(15) ? C36 C37 . 1.387(14) ? C36 H36 . 0.9500 ? C37 C38 . 1.401(16) ? C37 H37 . 0.9500 ? C38 H38 . 0.9500 ? C39 C44 . 1.367(9) ? C39 C40 . 1.385(10) ? C40 C41 . 1.393(10) ? C40 H40 . 0.9500 ? C41 C42 . 1.367(10) ? C41 H41 . 0.9500 ? C42 C43 . 1.359(11) ? C42 C70 . 1.544(15) ? C43 C44 . 1.386(10) ? C43 H43 . 0.9500 ? C44 H44 . 0.9500 ? C45 C46 . 1.507(12) ? C45 H45A . 0.9900 ? C45 H45B . 0.9900 ? C46 C53 . 1.514(14) ? C46 H46 . 1.0000 ? C47 C48 . 1.503(15) ? C47 H47 . 1.0000 ? C48 C52 . 1.513(15) ? C48 H48 . 1.0000 ? C49 C50 . 1.511(17) ? C49 C51 . 1.527(16) ? C50 H50A . 0.9800 ? C50 H50B . 0.9800 ? C50 H50C . 0.9800 ? C51 H51A . 0.9800 ? C51 H51B . 0.9800 ? C51 H51C . 0.9800 ? C52 C53 . 1.531(12) ? C52 H52 . 1.0000 ? C53 H53 . 1.0000 ? C54 C55 . 1.470(17) ? C54 C56 . 1.530(18) ? C55 H55A . 0.9800 ? C55 H55B . 0.9800 ? C55 H55C . 0.9800 ? C56 H56A . 0.9800 ? C56 H56B . 0.9800 ? C56 H56C . 0.9800 ? C57 H57A . 0.9800 ? C57 H57B . 0.9800 ? C57 H57C . 0.9800 ? C58 C59 . 1.527(12) ? C58 H58A . 0.9900 ? C58 H58B . 0.9900 ? C59 C65 . 1.480(13) ? C59 H59 . 1.0000 ? C60 C61 . 1.530(14) ? C60 H60 . 1.0000 ? C61 C66 . 1.518(14) ? C61 H61 . 1.0000 ? C62 C63 . 1.470(16) ? C62 C64 . 1.513(16) ? C63 H63A . 0.9800 ? C63 H63B . 0.9800 ? C63 H63C . 0.9800 ? C64 H64A . 0.9800 ? C64 H64B . 0.9800 ? C64 H64C . 0.9800 ? C65 C66 . 1.534(12) ? C65 H65 . 1.0000 ? C66 H66 . 1.0000 ? C67 C68 . 1.508(16) ? C67 C69 . 1.513(17) ? C68 H68A . 0.9800 ? C68 H68B . 0.9800 ? C68 H68C . 0.9800 ? C69 H69A . 0.9800 ? C69 H69B . 0.9800 ? C69 H69C . 0.9800 ? C70 H70A . 0.9800 ? C70 H70B . 0.9800 ? C70 H70C . 0.9800 ? 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 C45 H45B O4 2_645 0.99 2.55 3.180(10) 121 C24 H24 O4 2_645 0.95 2.60 3.540(10) 169 C48 H48 \p1 2_645 1.00 3.18 4.120 165 C53 H53 O3 2_655 1.00 2.70 3.670(10) 165 C40 H40 \p3 1_565 0.95 2.89 3.828 171 C32 H32 \p4 1_545 0.95 2.83 3.782 176 C58 H58B O10 2_846 0.99 2.70 3.190(10) 110 C61 H61 \p2 2_856 1.00 3.20 4.117 153 C36 H36 O9 2_856 0.95 2.70 3.560(10) 152 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 C4 N1 C1 C20 . . . . -176.2(10) ? C4 N1 C1 C2 . . . . 1.8(12) ? C20 C1 C2 C3 . . . . 175.6(11) ? N1 C1 C2 C3 . . . . -2.3(12) ? C1 C2 C3 C4 . . . . 1.8(13) ? C1 N1 C4 C5 . . . . -176.2(10) ? C1 N1 C4 C3 . . . . -0.8(11) ? C2 C3 C4 N1 . . . . -0.7(12) ? C2 C3 C4 C5 . . . . 174.8(11) ? N1 C4 C5 C6 . . . . -4.9(17) ? C3 C4 C5 C6 . . . . -179.4(11) ? N1 C4 C5 C21 . . . . 174.5(10) ? C3 C4 C5 C21 . . . . 0.1(16) ? C9 N2 C6 C5 . . . . -179.8(10) ? C9 N2 C6 C7 . . . . 1.8(11) ? C4 C5 C6 N2 . . . . -7.9(17) ? C21 C5 C6 N2 . . . . 172.7(10) ? C4 C5 C6 C7 . . . . 170.4(10) ? C21 C5 C6 C7 . . . . -9.0(15) ? N2 C6 C7 C8 . . . . -2.2(12) ? C5 C6 C7 C8 . . . . 179.4(11) ? C6 C7 C8 C9 . . . . 1.5(12) ? C6 N2 C9 C10 . . . . 177.7(10) ? C6 N2 C9 C8 . . . . -0.9(11) ? C7 C8 C9 N2 . . . . -0.4(13) ? C7 C8 C9 C10 . . . . -179.0(10) ? N2 C9 C10 C11 . . . . 12.8(17) ? C8 C9 C10 C11 . . . . -168.7(11) ? N2 C9 C10 C27 . . . . -166.8(9) ? C8 C9 C10 C27 . . . . 11.7(15) ? C9 C10 C11 N3 . . . . -4.9(19) ? C27 C10 C11 N3 . . . . 174.8(10) ? C9 C10 C11 C12 . . . . 171.9(11) ? C27 C10 C11 C12 . . . . -8.5(17) ? C14 N3 C11 C10 . . . . 177.0(11) ? C14 N3 C11 C12 . . . . -0.4(11) ? C10 C11 C12 C13 . . . . -175.4(11) ? N3 C11 C12 C13 . . . . 2.0(12) ? C11 C12 C13 C14 . . . . -2.7(13) ? C11 N3 C14 C15 . . . . 178.2(10) ? C11 N3 C14 C13 . . . . -1.2(11) ? C12 C13 C14 C15 . . . . -176.9(11) ? C12 C13 C14 N3 . . . . 2.4(12) ? N3 C14 C15 C16 . . . . 1.3(17) ? C13 C14 C15 C16 . . . . -179.4(11) ? N3 C14 C15 C33 . . . . 179.1(10) ? C13 C14 C15 C33 . . . . -1.6(17) ? C19 N4 C16 C15 . . . . 179.2(10) ? C19 N4 C16 C17 . . . . -2.2(11) ? C14 C15 C16 N4 . . . . 8.2(17) ? C33 C15 C16 N4 . . . . -169.7(10) ? C14 C15 C16 C17 . . . . -170.4(10) ? C33 C15 C16 C17 . . . . 11.8(15) ? N4 C16 C17 C18 . . . . 2.1(12) ? C15 C16 C17 C18 . . . . -179.1(10) ? C16 C17 C18 C19 . . . . -1.2(12) ? C16 N4 C19 C20 . . . . 180.0(10) ? C16 N4 C19 C18 . . . . 1.4(12) ? C17 C18 C19 C20 . . . . -178.7(10) ? C17 C18 C19 N4 . . . . -0.1(13) ? N1 C1 C20 C19 . . . . 4.4(18) ? C2 C1 C20 C19 . . . . -173.1(11) ? N1 C1 C20 C39 . . . . -172.4(9) ? C2 C1 C20 C39 . . . . 10.1(17) ? N4 C19 C20 C1 . . . . -9.0(18) ? C18 C19 C20 C1 . . . . 169.4(11) ? N4 C19 C20 C39 . . . . 167.8(9) ? C18 C19 C20 C39 . . . . -13.9(15) ? C4 C5 C21 C22 . . . . -55.8(14) ? C6 C5 C21 C22 . . . . 123.6(11) ? C4 C5 C21 C26 . . . . 123.1(11) ? C6 C5 C21 C26 . . . . -57.4(14) ? C26 C21 C22 C23 . . . . -0.8(16) ? C5 C21 C22 C23 . . . . 178.2(10) ? C45 O1 C23 C24 . . . . -0.3(17) ? C45 O1 C23 C22 . . . . 179.6(9) ? C21 C22 C23 C24 . . . . 1.9(18) ? C21 C22 C23 O1 . . . . -177.9(10) ? O1 C23 C24 C25 . . . . 177.6(10) ? C22 C23 C24 C25 . . . . -2.2(18) ? C23 C24 C25 C26 . . . . 1.5(17) ? C24 C25 C26 C21 . . . . -0.4(18) ? C22 C21 C26 C25 . . . . 0.1(17) ? C5 C21 C26 C25 . . . . -178.9(11) ? C11 C10 C27 C28 . . . . 76.5(15) ? C9 C10 C27 C28 . . . . -103.8(13) ? C11 C10 C27 C32 . . . . -105.2(14) ? C9 C10 C27 C32 . . . . 74.4(14) ? C32 C27 C28 C29 . . . . 2.6(17) ? C10 C27 C28 C29 . . . . -179.1(10) ? C27 C28 C29 C30 . . . . -2.1(18) ? C28 C29 C30 C31 . . . . 2.1(19) ? C28 C29 C30 C57 . . . . 179.0(11) ? C29 C30 C31 C32 . . . . -3(2) ? C57 C30 C31 C32 . . . . -179.5(13) ? C28 C27 C32 C31 . . . . -3(2) ? C10 C27 C32 C31 . . . . 178.5(13) ? C30 C31 C32 C27 . . . . 3(2) ? C14 C15 C33 C38 . . . . -124.1(12) ? C16 C15 C33 C38 . . . . 53.9(14) ? C14 C15 C33 C34 . . . . 55.6(15) ? C16 C15 C33 C34 . . . . -126.4(11) ? C38 C33 C34 C35 . . . . -0.5(17) ? C15 C33 C34 C35 . . . . 179.8(10) ? C33 C34 C35 C36 . . . . -2.7(18) ? C33 C34 C35 O7 . . . . 178.6(11) ? C58 O7 C35 C36 . . . . 176.6(10) ? C58 O7 C35 C34 . . . . -4.6(16) ? C34 C35 C36 C37 . . . . 3.5(18) ? O7 C35 C36 C37 . . . . -177.7(10) ? C35 C36 C37 C38 . . . . -1.0(18) ? C34 C33 C38 C37 . . . . 2.8(18) ? C15 C33 C38 C37 . . . . -177.5(11) ? C36 C37 C38 C33 . . . . -2.1(18) ? C1 C20 C39 C44 . . . . -77.4(14) ? C19 C20 C39 C44 . . . . 105.4(13) ? C1 C20 C39 C40 . . . . 108.5(13) ? C19 C20 C39 C40 . . . . -68.7(14) ? C44 C39 C40 C41 . . . . 5(2) ? C20 C39 C40 C41 . . . . -179.9(13) ? C39 C40 C41 C42 . . . . 1(2) ? C40 C41 C42 C43 . . . . -7(2) ? C40 C41 C42 C70 . . . . -179.0(13) ? C41 C42 C43 C44 . . . . 7(2) ? C70 C42 C43 C44 . . . . 178.5(11) ? C40 C39 C44 C43 . . . . -5.6(17) ? C20 C39 C44 C43 . . . . 180.0(11) ? C42 C43 C44 C39 . . . . -0.2(18) ? C23 O1 C45 C46 . . . . -172.6(9) ? C47 O2 C46 C45 . . . . -168.4(8) ? C47 O2 C46 C53 . . . . 68.5(11) ? O1 C45 C46 O2 . . . . -179.6(8) ? O1 C45 C46 C53 . . . . -58.9(11) ? C46 O2 C47 O3 . . . . 84.2(11) ? C46 O2 C47 C48 . . . . -33.6(13) ? C49 O3 C47 O2 . . . . -117.7(10) ? C49 O3 C47 C48 . . . . 4.6(11) ? C49 O4 C48 C47 . . . . 31.7(11) ? C49 O4 C48 C52 . . . . 156.2(9) ? O2 C47 C48 O4 . . . . 98.0(10) ? O3 C47 C48 O4 . . . . -21.9(10) ? O2 C47 C48 C52 . . . . -20.9(14) ? O3 C47 C48 C52 . . . . -140.8(9) ? C48 O4 C49 O3 . . . . -29.6(12) ? C48 O4 C49 C50 . . . . -145.4(9) ? C48 O4 C49 C51 . . . . 90.1(11) ? C47 O3 C49 O4 . . . . 15.0(12) ? C47 O3 C49 C50 . . . . 130.7(9) ? C47 O3 C49 C51 . . . . -104.9(12) ? C54 O5 C52 C48 . . . . 147.6(10) ? C54 O5 C52 C53 . . . . 27.2(12) ? O4 C48 C52 O5 . . . . 171.9(8) ? C47 C48 C52 O5 . . . . -72.5(12) ? O4 C48 C52 C53 . . . . -73.8(12) ? C47 C48 C52 C53 . . . . 41.8(14) ? C54 O6 C53 C46 . . . . -128.0(11) ? C54 O6 C53 C52 . . . . -9.0(13) ? O2 C46 C53 O6 . . . . 71.1(10) ? C45 C46 C53 O6 . . . . -45.3(12) ? O2 C46 C53 C52 . . . . -43.3(11) ? C45 C46 C53 C52 . . . . -159.7(9) ? O5 C52 C53 O6 . . . . -11.1(11) ? C48 C52 C53 O6 . . . . -125.8(10) ? O5 C52 C53 C46 . . . . 106.3(10) ? C48 C52 C53 C46 . . . . -8.4(13) ? C53 O6 C54 O5 . . . . 25.7(14) ? C53 O6 C54 C55 . . . . 142.9(11) ? C53 O6 C54 C56 . . . . -92.5(12) ? C52 O5 C54 O6 . . . . -32.9(14) ? C52 O5 C54 C55 . . . . -149.6(11) ? C52 O5 C54 C56 . . . . 83.2(13) ? C35 O7 C58 C59 . . . . -174.4(9) ? C60 O8 C59 C65 . . . . 66.2(11) ? C60 O8 C59 C58 . . . . -170.2(8) ? O7 C58 C59 O8 . . . . 179.3(8) ? O7 C58 C59 C65 . . . . -58.9(12) ? C59 O8 C60 O9 . . . . 86.1(10) ? C59 O8 C60 C61 . . . . -29.8(12) ? C62 O9 C60 O8 . . . . -114.6(10) ? C62 O9 C60 C61 . . . . 7.8(11) ? C62 O10 C61 C66 . . . . 154.0(9) ? C62 O10 C61 C60 . . . . 31.4(10) ? O8 C60 C61 O10 . . . . 95.2(10) ? O9 C60 C61 O10 . . . . -23.7(10) ? O8 C60 C61 C66 . . . . -20.8(14) ? O9 C60 C61 C66 . . . . -139.8(9) ? C60 O9 C62 O10 . . . . 11.0(12) ? C60 O9 C62 C63 . . . . 127.6(9) ? C60 O9 C62 C64 . . . . -106.4(12) ? C61 O10 C62 O9 . . . . -26.9(12) ? C61 O10 C62 C63 . . . . -144.3(10) ? C61 O10 C62 C64 . . . . 91.4(11) ? C67 O11 C65 C59 . . . . -138.0(10) ? C67 O11 C65 C66 . . . . -18.4(12) ? O8 C59 C65 O11 . . . . 67.0(10) ? C58 C59 C65 O11 . . . . -50.6(12) ? O8 C59 C65 C66 . . . . -46.6(12) ? C58 C59 C65 C66 . . . . -164.2(9) ? C67 O12 C66 C61 . . . . 144.7(9) ? C67 O12 C66 C65 . . . . 23.2(11) ? O10 C61 C66 O12 . . . . 166.9(8) ? C60 C61 C66 O12 . . . . -78.7(11) ? O10 C61 C66 C65 . . . . -77.9(11) ? C60 C61 C66 C65 . . . . 36.5(14) ? O11 C65 C66 O12 . . . . -3.2(10) ? C59 C65 C66 O12 . . . . 113.3(10) ? O11 C65 C66 C61 . . . . -119.3(9) ? C59 C65 C66 C61 . . . . -2.8(14) ? C65 O11 C67 O12 . . . . 33.1(12) ? C65 O11 C67 C68 . . . . 147.0(11) ? C65 O11 C67 C69 . . . . -86.4(12) ? C66 O12 C67 O11 . . . . -34.9(12) ? C66 O12 C67 C68 . . . . -150.6(10) ? C66 O12 C67 C69 . . . . 83.6(12) ?