#------------------------------------------------------------------------------ #$Date: 2023-03-14 03:15:44 +0000 (Tue, 14 Mar 2023) $ #$Revision: 281865 $ #$URL: svn://www.crystallography.net/cod/cif/2/24/42/2244234.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_2244234 loop_ _publ_author_name 'Okmanov, Rasul Ya.' 'Olimova, Manzura I.' 'Karabaeva, Surayyo B.' 'Sapaev, Frunza A.' 'Abdireymov, Kudaybergen B.' _publ_section_title ; Syntheses, crystal structures and Hirshfeld surface analyses of N-arylsulfonyl derivatives of cytisine ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first ; ; _journal_paper_doi 10.1107/S2056989023001950 _journal_volume 79 _journal_year 2023 _chemical_absolute_configuration rm _chemical_formula_iupac 'C17 H17 N3 O5 S' _chemical_formula_moiety 'C17 H17 N3 O5 S' _chemical_formula_sum 'C17 H17 N3 O5 S' _chemical_formula_weight 375.39 _chemical_name_common ; (7R,9R)-N-[(3-nitrophenyl)sulfonyl]cytisine ; _chemical_name_systematic (1R,5R)-3-((3-nitrophenyl)sulfonyl)-1,2,3,4,5,6-hexahydro-8H-1,5-methanopyrido[1,2-a][1,5]diazocin-8-one _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-2018/3 _cell_angle_alpha 90 _cell_angle_beta 94.03(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 11.040(2) _cell_length_b 6.2621(13) _cell_length_c 12.424(3) _cell_measurement_reflns_used 5501 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 71.3670 _cell_measurement_theta_min 4.0060 _cell_volume 856.8(3) _computing_cell_refinement ; CrysAlis PRO (Rigaku OD, 2021) ; _computing_data_collection ; CrysAlis PRO (Rigaku OD, 2021) ; _computing_data_reduction ; CrysAlis PRO (Rigaku OD, 2021) ; _computing_molecular_graphics ; XP in SHELXTL (Sheldrick, 2008) and Mercury (Macrae et al., 2020) ; _computing_publication_material ; SHELXTL (Sheldrick, 2015), PLATON (Spek, 2020) and publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS7 (Sheldrick, 2008) ; _diffrn_ambient_temperature 296(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Single source at home/near, HyPix3000' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_unetI/netI 0.0216 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 7776 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 71.460 _diffrn_reflns_theta_min 3.566 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 1.995 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.63895 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.455 _exptl_crystal_description prizmatic _exptl_crystal_F_000 392 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.471 _refine_diff_density_min -0.224 _refine_ls_abs_structure_details ; Flack x determined using 579 quotients [(I^+^)-(I^-^)]/[(I^+^)+(I^-^)] (Parsons et al., 2013) ; _refine_ls_abs_structure_Flack 0.017(16) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 235 _refine_ls_number_reflns 2446 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0394 _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^)+(0.0754P)^2^+0.1248P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1120 _refine_ls_wR_factor_ref 0.1136 _reflns_number_gt 2363 _reflns_number_total 2446 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5674sup1.cif _cod_data_source_block III _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 2244234 _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_hkl_file ; 0 -2 -5 543.498 83.5783 3 0 -2 -6 10519.7 432.335 3 0 -2 -7 3922.30 274.475 3 0 -2 8 1287.73 147.531 57 0 -2 -8 1352.78 179.378 3 0 -2 -9 290.232 101.523 3 0 -2 9 565.064 108.855 57 0 -2 10 19039.4 692.139 57 0 -2 11 7471.09 407.530 57 0 -2 -11 7570.83 393.637 22 0 -2 -12 1094.37 147.823 22 0 -2 12 1408.97 168.578 57 0 -2 13 1716.89 169.781 57 0 -2 -13 1092.64 134.700 22 0 -2 14 630.425 89.6433 57 0 -1 1 816086. 14712.6 1 0 -1 2 6402.92 199.972 1 0 -1 -2 6972.88 169.093 30 0 -1 -3 78548.8 1515.21 30 0 -1 3 79981.8 1568.91 1 0 -1 4 919.156 87.1208 1 0 -1 -6 54257.1 1276.01 3 0 -1 -7 16671.6 589.396 3 0 -1 8 16242.7 564.751 57 0 -1 -8 16631.2 635.259 3 0 -1 -9 8849.98 416.183 53 0 -1 9 9597.39 435.999 57 0 -1 -9 8314.14 464.108 3 0 -1 10 89.0068 57.0917 57 0 -1 -10 80.8842 59.1536 22 0 -1 -10 86.7041 58.3288 53 0 -1 -10-22.4750 88.2734 3 0 -1 11 3826.47 295.336 57 0 -1 -11 3524.33 277.064 53 0 -1 -11 3771.23 280.199 22 0 -1 -12 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506.932 57 -3 3 9 9928.45 462.336 15 3 3 -9 9806.35 469.898 21 -3 3 9 9545.70 493.343 43 3 3 -9 9107.52 469.051 20 3 3 -8 1132.94 160.000 21 -3 3 8 1283.78 159.524 15 -3 3 8 1537.21 217.753 27 -3 3 8 1334.47 181.939 57 3 3 -8 1124.17 151.691 8 -3 3 8 1149.37 171.873 43 3 3 -8 1049.03 154.961 20 3 3 -8 1199.44 206.660 62 3 3 -7 1261.51 199.096 62 3 3 -7 1277.02 155.143 8 -3 3 7 971.595 151.318 57 -3 3 7 1019.38 134.796 15 -3 3 7 856.663 167.624 27 3 3 -7 1171.36 154.879 21 -3 3 7 960.345 152.229 43 3 3 -7 1194.64 153.327 20 3 3 -6 5607.44 323.268 21 -3 3 6 5964.15 358.374 57 3 3 -6 6571.97 323.368 8 -3 3 6 6192.78 319.928 15 3 3 -6 5875.47 404.148 62 -3 3 6 4743.46 315.992 43 -3 3 6 5683.16 385.488 27 -3 3 5 98.7361 66.4233 27 3 3 -5 63.4201 52.5211 62 -3 3 5 59.9745 38.4794 15 3 3 -5 55.4176 46.6081 21 3 3 -5 11.5019 53.4599 8 3 3 -5 49.6413 37.7697 47 -3 3 5 106.035 53.2222 43 -3 3 5 80.3959 48.9274 57 3 3 -4 11386.3 521.911 62 -3 3 4 12497.4 532.106 27 3 3 -3 2646.67 206.401 4 -3 3 3 2723.80 205.001 6 -3 3 3 2742.94 210.808 7 3 3 -3 2699.83 224.027 62 -3 3 3 2689.62 210.680 18 3 3 -2 22266.7 691.287 4 3 3 -2 20276.6 690.578 41 -3 3 2 21055.3 681.333 7 -3 3 2 21718.3 692.951 18 3 3 -1 25407.7 761.694 4 3 3 -1 25752.2 788.736 41 -3 3 1 24482.2 756.371 7 -3 3 1 25400.9 766.410 18 -3 3 0 2824.82 208.572 32 3 3 0 2559.81 201.797 4 3 3 0 2474.11 203.617 42 -3 3 0 2920.77 214.389 7 3 3 0 2462.36 207.461 41 -3 3 0 2615.90 205.694 18 -3 3 -1 4426.81 271.875 32 3 3 1 4225.95 264.305 4 3 3 1 4781.84 277.604 42 -3 3 -1 4645.36 275.649 7 3 3 1 4498.59 280.790 41 -3 3 -1 4343.47 271.518 18 -3 3 -2 3404.01 243.357 32 3 3 2 3178.78 227.722 4 -3 3 -2 3166.83 227.488 7 -3 3 -2 3440.80 236.210 18 3 3 2 3238.89 236.785 5 3 3 3 10450.3 466.814 5 3 3 3 9632.53 420.441 4 -3 3 -3 9510.18 440.594 32 -3 3 -3 10057.3 430.701 18 3 3 4 4354.61 305.974 5 -3 3 -4 4029.11 286.660 32 -3 3 -4 3569.05 225.975 16 3 3 4 4082.96 264.108 10 3 3 5 1607.08 168.590 10 3 3 5 1610.46 198.233 5 -3 3 -5 1634.71 201.700 63 3 3 5 1594.85 166.893 51 3 3 5 1412.54 149.681 14 -3 3 -5 1530.59 161.803 47 -3 3 -5 1643.73 163.278 20 3 3 5 1326.53 166.980 58 -3 3 -5 1228.22 150.955 46 -3 3 -5 1515.39 150.102 16 3 3 6 45.5613 51.6554 5 3 3 6 29.1552 33.0554 14 -3 3 -6 24.3127 55.1293 63 -3 3 -6 16.3298 37.0284 49 -3 3 -6-15.8843 36.0182 46 -3 3 -6 75.9793 55.5598 20 3 3 6 37.5997 46.6978 39 3 3 6-18.7700 38.0684 58 3 3 6 64.9346 54.5980 10 3 3 7 1876.63 229.984 5 -3 3 -7 1686.04 172.175 16 -3 3 -7 1624.73 228.312 63 3 3 7 1847.11 212.475 39 3 3 7 1719.81 179.287 14 3 3 7 1585.84 197.422 58 3 3 7 1568.15 184.825 51 -3 3 -7 1518.37 177.618 49 -3 3 -7 1404.87 166.569 20 3 3 8 997.997 157.238 58 -3 3 -8 785.018 124.996 16 -3 3 -8 1027.00 152.671 49 3 3 8 1101.94 162.042 51 3 3 8 1001.92 142.968 14 -3 3 -8 715.902 125.741 20 3 3 8 1043.70 167.822 39 3 3 9 6549.43 370.169 14 3 3 9 6649.30 401.090 58 -3 3 -9 6192.80 342.449 16 3 3 9 6301.46 414.411 39 3 3 10 1907.62 194.262 14 3 3 10 1517.64 202.664 39 3 3 11 3063.50 232.490 14 3 3 11 3108.95 265.327 39 3 3 12 1274.27 133.143 14 3 3 12 1254.75 151.136 39 3 3 13 106.054 37.6754 14 3 3 13 72.1050 40.4947 39 3 3 13 129.035 48.5978 43 3 4 -12 2310.88 169.120 20 -3 4 12 2407.04 178.658 43 -3 4 11 657.943 114.104 43 3 4 -11 676.699 107.325 20 3 4 -10 3232.11 259.436 12 -3 4 10 3751.71 281.587 43 3 4 -10 3161.84 250.494 20 3 4 -9 2861.30 257.831 12 -3 4 9 3139.95 273.029 43 3 4 -9 2999.66 250.215 20 3 4 -8 3579.41 264.874 8 3 4 -8 3149.01 280.700 12 -3 4 8 3448.20 289.136 43 3 4 -8 3291.70 269.143 20 3 4 -7 6352.36 350.188 8 3 4 -7 5903.39 340.780 47 3 4 -7 4940.08 353.246 12 -3 4 7 5480.25 331.458 15 -3 4 7 5635.13 373.611 43 -3 4 6 18572.3 656.666 15 3 4 -6 20152.1 681.224 8 3 4 -6 18733.3 735.588 12 3 4 -6 19653.5 713.904 21 3 4 -6 21796.1 709.909 47 -3 4 6 19315.2 734.226 43 -3 4 6 19975.3 739.154 39 3 4 -5 23891.0 728.966 8 3 4 -5 22292.4 728.775 47 3 4 -5 20832.4 732.458 21 -3 4 5 20792.3 754.578 43 3 4 -5 22012.4 862.573 42 3 4 -5 21024.1 765.112 12 3 4 -4 2211.57 215.836 12 3 4 -4 2154.20 194.414 8 3 4 -4 2005.63 189.788 47 -3 4 4 2519.55 198.534 13 3 4 -4 2241.90 202.982 21 -3 4 4 1957.70 184.640 11 -3 4 4 2102.07 207.619 43 3 4 -4 2295.56 252.677 42 -3 4 3 24774.1 810.590 34 3 4 -3 23948.9 803.742 60 3 4 -3 25192.5 751.786 8 -3 4 3 25158.9 738.762 13 3 4 -3 26080.0 780.571 47 3 4 -3 25067.9 809.312 12 -3 4 3 25391.7 853.112 7 -3 4 3 27243.9 777.413 11 3 4 -3 25011.9 904.115 42 -3 4 2 11669.9 442.647 13 -3 4 2 11261.8 501.067 34 3 4 -2 11868.8 496.034 9 -3 4 2 12254.3 545.571 7 3 4 -2 11527.2 456.800 8 3 4 -2 11949.1 515.369 60 3 4 -2 12572.9 505.951 12 3 4 -2 12132.4 471.125 47 -3 4 2 11126.4 470.688 44 -3 4 2 12338.0 472.581 11 3 4 -2 11744.9 565.831 42 3 4 -2 11687.0 511.061 40 -3 4 2 11438.3 487.668 38 3 4 -1 26144.0 772.051 8 3 4 -1 26556.5 827.721 9 -3 4 1 26999.7 758.164 13 -3 4 1 27824.4 862.849 34 3 4 -1 27023.7 857.196 40 3 4 -1 25841.9 789.849 52 3 4 -1 26026.7 794.201 48 3 4 -1 27738.5 786.985 47 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-3 4 -3 33257.9 975.112 49 -3 4 -3 33389.0 990.270 47 -3 4 -3 35600.1 1004.01 46 3 4 3 34288.5 1097.20 6 3 4 3 35165.5 958.041 36 3 4 4 7474.24 384.785 51 -3 4 -4 7223.06 398.028 46 -3 4 -4 6695.98 378.080 49 -3 4 -4 7406.92 394.203 47 3 4 4 8331.01 390.314 14 -3 4 -4 7057.23 360.239 16 3 4 4 6849.57 444.158 6 -3 4 -5 14010.0 566.012 47 -3 4 -5 12095.9 502.083 16 3 4 5 12621.8 514.895 14 3 4 5 12436.2 532.385 51 -3 4 -5 12430.8 545.550 49 -3 4 -5 12280.9 545.015 46 3 4 6 5481.46 327.799 14 3 4 6 4531.72 316.361 51 -3 4 -6 4741.08 328.692 49 -3 4 -6 4369.88 313.451 46 3 4 6 5034.38 355.991 39 -3 4 -6 4529.54 297.538 16 -3 4 -6 4695.92 317.321 47 -3 4 -7 347.241 94.9485 16 3 4 7 224.271 82.1656 14 3 4 7 172.708 80.3472 51 -3 4 -7 469.023 113.922 49 -3 4 -7 325.096 95.0973 46 3 4 7 112.003 68.2802 39 -3 4 -8 2662.32 245.202 49 3 4 8 3083.15 271.683 59 3 4 8 2650.65 232.966 14 3 4 8 2410.65 250.876 39 -3 4 -8 3136.09 245.476 16 3 4 9 262.416 83.0621 59 -3 4 -9 356.914 89.4125 16 3 4 9 292.867 85.9351 14 -3 4 -9 416.290 99.6749 49 3 4 9 356.279 104.281 39 3 4 10 2005.96 193.580 59 3 4 10 2344.56 199.170 14 -3 4 -10 1941.69 174.222 16 3 4 10 2173.49 219.254 39 -3 4 -11 256.490 59.5372 16 3 4 11 331.841 74.4230 14 3 4 11 189.379 63.0059 43 3 4 11 202.944 62.5127 39 3 4 12 540.476 83.1033 43 3 4 12 380.683 70.8393 39 3 5 -11 2472.27 146.544 16 -3 5 11 2194.34 152.080 44 3 5 -10 1077.33 116.016 48 3 5 -10 1111.97 125.395 12 -3 5 10 1220.49 137.727 43 3 5 -9 653.463 114.912 12 -3 5 9 681.429 118.131 43 -3 5 8 493.107 110.410 43 3 5 -8 449.116 104.989 12 3 5 -7 1899.31 190.454 47 3 5 -7 1364.70 184.298 12 -3 5 7 1675.70 200.874 43 3 5 -7 2088.10 198.806 8 3 5 -6 8837.94 422.459 8 3 5 -6 8103.36 455.590 12 3 5 -6 9054.16 431.851 47 -3 5 6 7902.57 430.644 43 -3 5 6 7647.79 427.732 38 -3 5 6 6984.67 395.152 36 3 5 -5 10228.7 459.313 8 3 5 -5 8406.87 467.532 12 3 5 -5 9398.28 450.588 47 -3 5 5 9984.09 444.945 11 -3 5 5 9970.03 491.366 38 -3 5 5 8566.00 455.075 36 -3 5 4 16002.7 646.336 44 3 5 -4 17142.3 631.422 8 -3 5 4 18701.3 638.327 13 3 5 -4 16996.0 659.263 48 3 5 -4 17211.9 688.946 12 3 5 -4 18492.6 657.359 47 -3 5 4 17795.1 637.269 11 -3 5 4 16374.5 669.781 38 -3 5 4 17283.2 674.685 36 3 5 -3 5539.30 350.070 9 3 5 -3 5301.04 359.915 60 -3 5 3 6217.07 335.334 13 3 5 -3 5368.16 340.462 48 3 5 -3 5650.66 359.488 12 3 5 -3 5357.25 327.010 47 3 5 -3 5849.09 339.334 8 -3 5 3 5394.88 329.255 11 3 5 -3 4967.29 346.121 40 -3 5 3 5139.43 349.658 38 -3 5 3 4725.00 328.783 36 3 5 -2 18504.1 697.459 9 3 5 -2 17705.4 670.732 48 3 5 -2 18316.5 723.785 60 3 5 -2 19392.2 703.114 12 3 5 -2 18252.5 654.267 8 3 5 -2 18005.9 647.778 47 -3 5 2 20079.8 681.105 11 3 5 -2 16714.0 773.300 42 3 5 -2 18738.0 731.064 40 -3 5 2 17890.4 698.141 38 -3 5 2 18638.5 638.328 13 -3 5 2 17714.9 682.657 36 -3 5 1 45263.8 1300.14 34 3 5 -1 43721.3 1205.77 48 3 5 -1 46123.2 1300.15 60 3 5 -1 43741.5 1182.66 8 3 5 -1 44121.9 1242.37 9 -3 5 1 45921.4 1372.24 7 -3 5 1 45185.7 1162.60 13 -3 5 1 48134.1 1218.76 11 3 5 -1 42732.2 1351.20 42 3 5 -1 43713.7 1281.31 40 -3 5 1 47099.5 1271.81 38 -3 5 1 41319.3 1205.89 36 -3 5 0 21976.1 810.925 34 -3 5 0 20178.8 675.205 13 3 5 0 20494.5 718.003 48 3 5 0 20194.7 703.034 8 -3 5 0 22186.6 853.256 7 -3 5 0 22108.8 731.112 11 3 5 0 20072.4 828.444 42 3 5 0 20884.2 787.068 40 -3 5 0 20578.3 751.391 38 3 5 0 21497.3 762.016 9 3 5 0 20816.0 780.302 60 3 5 1 35748.2 1061.78 9 3 5 1 36634.5 1103.01 60 -3 5 -1 34804.5 966.581 13 3 5 1 32719.8 1009.77 11 -3 5 -1 34267.1 1036.21 47 -3 5 -1 38209.1 1187.91 7 3 5 1 36323.0 1103.58 40 3 5 2 24167.3 838.246 60 3 5 2 24631.8 818.771 9 -3 5 -2 23686.0 813.306 47 -3 5 -2 23539.9 804.104 46 3 5 2 21290.1 774.149 11 3 5 2 24587.3 846.989 40 3 5 3 164.970 81.0504 59 -3 5 -3 174.005 78.4870 47 3 5 3 94.5155 63.6551 11 3 5 4 8935.86 490.897 59 -3 5 -4 10542.1 455.834 16 -3 5 -4 9733.70 480.069 49 -3 5 -4 10272.0 496.414 47 -3 5 -4 9767.41 490.406 46 3 5 4 9365.76 475.955 11 -3 5 -5 10350.0 469.026 16 3 5 5 11198.8 552.067 59 3 5 5 10995.6 511.693 11 -3 5 -5 11409.8 524.354 47 -3 5 -5 11122.0 521.933 49 -3 5 -5 12038.9 549.167 46 3 5 6 1079.61 166.663 59 -3 5 -6 1411.69 175.492 47 3 5 6 1196.38 162.012 51 -3 5 -6 1638.91 196.050 49 3 5 6 1294.52 172.313 11 -3 5 -6 1607.89 174.600 16 -3 5 -7 6721.65 352.867 16 3 5 7 6225.20 386.538 59 -3 5 -7 6810.84 365.377 47 3 5 7 6561.38 360.731 11 3 5 7 6678.52 397.232 39 3 5 8 1047.28 149.424 59 -3 5 -8 1097.28 137.443 16 3 5 8 1201.91 160.866 39 3 5 9 626.634 106.735 59 -3 5 -9 627.629 97.4841 16 3 5 9 652.082 111.474 39 -3 5 -10 69.1300 36.1582 16 3 5 10 143.701 53.0931 43 3 5 10 92.9810 45.6696 39 3 5 10 51.6465 37.7937 59 3 6 -9 44.9482 28.4355 48 3 6 -8 1881.58 152.761 48 -3 6 8 1955.57 151.580 44 -3 6 8 2193.96 162.558 38 3 6 -7 2147.94 172.839 8 3 6 -7 1887.63 177.101 12 3 6 -7 2108.93 175.858 48 -3 6 7 1896.12 171.462 38 3 6 -6 1508.00 156.636 8 3 6 -6 1372.75 160.477 12 3 6 -6 1199.64 144.213 48 -3 6 6 1502.22 168.570 38 -3 6 6 1656.63 162.633 36 3 6 -5 764.552 125.536 48 3 6 -5 1014.23 135.216 47 3 6 -5 736.130 128.497 12 3 6 -5 838.317 131.637 8 -3 6 5 880.251 135.614 38 -3 6 5 947.865 133.960 36 3 6 -4 700.099 124.260 8 3 6 -4 654.442 120.172 48 -3 6 4 516.098 118.878 38 3 6 -4 570.889 116.389 12 3 6 -4 730.510 118.614 47 -3 6 4 616.226 116.988 36 3 6 -3 433.374 102.919 48 -3 6 3 325.246 84.9625 13 -3 6 3 133.764 63.6113 37 3 6 -3 377.007 86.6302 47 3 6 -3 212.152 85.6837 8 -3 6 3 278.844 96.2329 38 -3 6 3 214.891 83.3454 36 3 6 -2 2741.75 231.480 48 3 6 -2 2993.92 234.484 8 -3 6 2 3189.11 231.630 13 -3 6 2 2759.91 252.136 38 -3 6 2 2289.11 223.236 37 -3 6 2 2698.14 237.434 36 3 6 -1 1927.37 218.083 60 3 6 -1 1618.63 182.167 8 3 6 -1 1882.54 190.481 48 -3 6 1 1930.20 184.966 13 -3 6 1 2152.70 226.318 38 -3 6 1 2175.30 216.458 37 -3 6 1 1411.62 172.649 36 3 6 0 6318.43 398.085 60 3 6 0 6525.57 355.877 8 -3 6 0 5814.31 321.059 13 -3 6 0 5601.67 354.904 37 3 6 1 2432.39 217.753 8 -3 6 -1 2240.84 217.245 37 -3 6 -1 2521.15 205.442 13 -3 6 -2 289.833 86.5473 47 3 6 2 253.846 80.5539 8 -3 6 -2 201.581 68.2701 13 3 6 2 217.591 84.9713 11 -3 6 -2 239.720 77.7679 37 3 6 3 200.650 79.8712 8 -3 6 -3 170.848 67.1748 47 3 6 3 166.385 75.5228 11 3 6 4 3537.92 249.617 8 -3 6 -4 3835.14 271.353 47 3 6 4 3277.77 250.824 11 -3 6 -5 242.017 73.7448 47 3 6 5 354.229 86.1353 11 -3 6 -6 1762.57 155.174 16 -3 6 -6 2270.14 188.172 47 3 6 6 1757.11 165.963 11 -3 6 -7 479.225 78.0779 16 -3 6 -7 343.713 72.5981 47 3 6 7 373.385 78.3236 11 -3 6 -8 324.465 58.8993 16 3 6 8 308.868 62.7884 8 3 7 -5 2000.58 136.456 8 -3 7 5 1925.09 136.862 36 -3 7 4 275.754 60.4478 36 3 7 -4 302.393 67.2773 8 3 7 -4 305.297 58.5716 13 3 7 -3 732.380 96.9108 8 -3 7 3 819.158 103.245 36 -3 7 2 335.016 72.0960 36 3 7 -2 335.256 75.7141 8 -3 7 2 303.461 68.6296 37 3 7 -1 833.566 108.898 8 -3 7 1 636.475 99.7878 37 -3 7 0 408.823 76.2529 13 3 7 0 367.756 78.5377 8 -3 7 0 425.144 82.0211 37 -3 7 -1 885.166 101.601 13 3 7 1 847.235 108.926 8 -3 7 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3250.79 268.266 43 4 3 -10 3270.24 269.449 20 -4 3 9 3966.08 315.473 57 -4 3 9 4438.73 298.627 15 4 3 -9 4259.67 305.553 21 -4 3 9 4525.76 328.558 43 4 3 -9 4295.00 308.695 20 -4 3 8 12041.4 561.604 57 -4 3 8 11544.8 505.536 15 4 3 -8 12806.0 548.873 21 -4 3 8 11781.6 552.906 43 4 3 -8 11437.2 517.395 20 4 3 -7 2026.39 253.698 62 -4 3 7 1629.10 177.234 15 -4 3 7 2024.96 214.914 57 4 3 -7 1756.61 193.372 21 -4 3 7 2140.96 218.465 43 4 3 -6 10114.1 553.170 62 -4 3 6 9670.27 431.159 15 -4 3 6 9767.71 480.088 57 4 3 -6 10310.9 464.833 21 4 3 -6 11289.7 453.256 47 -4 3 6 10119.6 483.344 43 4 3 -5 438.690 107.126 62 4 3 -5 694.590 107.109 47 4 3 -5 612.429 107.559 21 -4 3 5 455.661 103.527 43 4 3 -4 2292.66 184.203 47 4 3 -4 2064.32 180.428 21 -4 3 4 2260.31 200.770 45 -4 3 4 1606.30 171.857 43 4 3 -3 7079.47 379.413 4 4 3 -3 8273.77 419.119 41 -4 3 3 8478.10 414.430 18 4 3 -2 25704.1 801.173 4 -4 3 2 24414.9 815.340 50 4 3 -2 24084.1 806.615 41 -4 3 2 26308.2 820.997 18 4 3 -1 3958.19 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145.967 10 -4 3 -6 980.225 171.010 63 4 3 6 832.006 141.856 58 -4 3 -6 660.905 112.892 16 4 3 6 857.609 157.850 5 4 3 6 986.054 136.118 14 4 3 6 852.784 136.371 51 -4 3 -6 683.383 118.437 46 4 3 7 3358.57 318.764 5 4 3 7 3081.90 242.380 14 4 3 7 3572.35 294.091 58 -4 3 -7 3138.11 236.771 16 4 3 7 3016.99 256.731 51 -4 3 -7 2592.53 238.931 49 4 3 7 3338.69 288.886 39 4 3 7 3482.72 271.255 10 4 3 8 2584.30 254.089 58 4 3 8 2508.79 221.984 14 -4 3 -8 2510.89 214.465 16 4 3 8 2334.44 232.288 51 -4 3 -8 2318.41 224.483 49 4 3 8 2802.45 271.297 39 4 3 9 937.833 157.424 58 4 3 9 802.399 133.215 14 4 3 9 746.963 145.131 39 4 3 10 737.770 119.329 14 4 3 10 664.907 123.422 58 4 3 10 631.669 129.616 39 4 3 11 1482.83 152.739 14 4 3 11 1210.92 160.698 39 4 3 12 497.982 92.5014 39 -4 4 12 337.325 63.9181 44 4 4 -12 313.122 61.3846 20 4 4 -11 442.619 88.8830 12 -4 4 11 490.387 95.0051 43 4 4 -11 364.498 79.2577 20 4 4 -10 1111.73 153.936 12 -4 4 10 1068.61 148.965 45 -4 4 10 1019.78 153.380 43 4 4 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376.866 42 4 4 0 6651.86 384.820 40 -4 4 0 6692.31 356.340 38 -4 4 -1 11905.4 539.813 34 -4 4 -1 13020.1 481.936 16 -4 4 -1 11865.9 563.188 32 4 4 1 13019.4 515.549 52 4 4 1 13216.3 515.052 48 -4 4 -1 11408.4 504.660 47 -4 4 -1 12175.0 574.514 7 4 4 1 12012.6 538.623 40 -4 4 -2 18998.4 713.129 34 4 4 2 20663.7 690.458 52 -4 4 -2 18705.9 757.777 32 -4 4 -2 20943.8 723.752 47 -4 4 -2 19814.9 701.273 46 -4 4 -2 19621.6 753.114 7 4 4 2 21541.8 744.015 40 -4 4 -2 20838.5 662.755 16 4 4 2 19728.5 695.170 9 -4 4 -3 3797.33 255.521 16 -4 4 -3 3920.91 326.498 32 4 4 3 3652.07 265.579 51 -4 4 -3 3759.14 282.057 47 -4 4 -3 3939.62 287.763 46 -4 4 -4 1778.96 178.350 16 4 4 4 1990.14 199.090 51 -4 4 -4 1969.08 206.356 49 -4 4 -4 1823.70 202.547 47 -4 4 -4 1839.58 201.583 46 4 4 4 1930.64 217.559 58 4 4 5 4307.97 304.437 51 4 4 5 4031.24 323.843 58 -4 4 -5 4347.68 289.781 16 -4 4 -5 4599.26 322.360 49 -4 4 -5 4218.03 304.510 47 -4 4 -5 4155.74 308.518 46 4 4 5 4506.62 294.443 14 -4 4 -6 3572.84 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2 -8 3494.01 256.682 56 -9 2 8 3371.02 237.558 15 9 2 -8 3221.21 248.262 21 -9 2 7 1876.05 198.209 35 9 2 -7 1887.68 199.228 56 -9 2 6 3065.52 269.898 35 9 2 -6 3977.56 292.784 56 -9 2 5 3561.42 302.903 35 9 2 -5 4128.41 302.174 56 -9 2 4 1033.34 166.077 35 9 2 -4 759.871 135.745 56 -9 2 3 1482.61 202.492 35 -9 2 3 1477.82 187.231 17 -9 2 3 1528.30 202.272 61 -9 2 2 10673.6 531.954 35 -9 2 2 10598.5 541.132 61 -9 2 1 2584.41 255.475 35 -9 2 1 2749.02 259.510 17 -9 2 1 3124.92 293.930 61 -9 2 0 8575.38 473.959 17 -9 2 0 9413.93 518.526 61 -9 2 -1 7468.21 431.479 17 -9 2 -1 7464.89 451.937 61 -9 2 -1 6640.07 401.377 54 -9 2 -2 7602.84 432.590 17 -9 2 -2 7051.21 434.262 61 -9 2 -2 7433.19 430.114 54 9 2 2 7595.79 419.307 10 -9 2 -3 6207.14 390.483 54 9 2 3 5401.53 361.613 10 -9 2 -4 14049.0 616.916 54 -9 2 -4 14775.6 577.741 23 9 2 4 14080.4 611.260 10 9 2 5 4601.45 327.054 58 -9 2 -5 4268.49 319.178 54 -9 2 -5 4338.90 291.319 23 9 2 5 4509.32 324.422 10 9 2 6 5229.47 349.233 58 -9 2 -6 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1 0 4379.06 322.595 54 -10 1 -1 3330.34 307.617 61 -10 1 -1 2960.14 267.122 54 -10 1 -2 8239.06 478.185 61 -10 1 -2 8147.33 454.127 54 -10 1 -3 385.102 107.022 54 -10 1 -4 5691.74 367.949 54 10 1 5 195.580 84.5875 10 10 1 5 140.814 69.1541 58 -10 1 -5 53.9600 48.2922 54 10 1 6 958.470 137.470 58 -10 1 -6 779.887 124.089 54 10 1 6 1193.29 152.873 10 10 1 7 507.843 96.4091 10 10 1 7 516.501 101.441 58 -10 1 -7 527.426 95.0018 54 10 1 8 640.750 94.5398 10 10 1 8 752.040 108.077 58 10 1 9 372.730 67.4771 58 10 2 -10 1947.63 137.650 21 -10 2 9 2423.08 161.720 15 10 2 -9 2254.36 170.498 21 10 2 -8 402.737 85.5647 56 -10 2 8 356.810 74.3602 15 10 2 -8 227.685 66.8901 21 -10 2 7 4652.03 293.659 35 10 2 -7 4674.52 289.316 56 10 2 -7 4155.03 268.578 21 -10 2 6 783.915 133.506 35 -10 2 5 527.733 117.641 35 -10 2 4 6430.35 394.389 35 -10 2 4 5557.76 359.413 61 -10 2 3 13047.7 596.242 35 -10 2 3 12651.7 562.982 17 -10 2 3 14287.3 616.952 61 -10 2 2 879.544 153.593 35 -10 2 2 638.750 139.988 61 -10 2 2 537.519 123.370 17 -10 2 1 8686.02 469.398 35 -10 2 1 8298.15 459.582 17 -10 2 1 9723.85 516.766 61 -10 2 0 2977.31 266.461 17 -10 2 0 2600.64 263.227 61 -10 2 -1 699.771 135.156 17 -10 2 -1 791.335 150.132 61 -10 2 -1 764.262 136.290 54 -10 2 -2 620.823 122.764 17 -10 2 -2 578.239 127.968 61 -10 2 -2 928.827 154.990 54 -10 2 -3 4566.99 322.745 54 10 2 3 4448.19 311.614 10 10 2 4 53.9520 60.5046 10 -10 2 -4 146.532 80.9766 54 -10 2 -5 1182.59 156.979 54 10 2 5 1531.23 175.042 10 10 2 6 305.370 83.5646 10 10 2 6 301.382 78.1161 58 -10 2 -6 326.405 86.6065 54 10 2 7 229.592 69.7250 10 10 2 7 132.257 52.0382 58 -10 2 -7 195.031 61.8840 54 10 2 8 114.074 45.2850 10 10 2 8 180.477 54.9516 58 -10 3 9 2615.68 147.408 15 10 3 -9 2397.64 147.666 21 -10 3 8 2091.20 150.987 15 10 3 -8 2303.77 162.721 21 -10 3 7 149.166 53.1045 15 10 3 -7 429.276 77.4498 21 -10 3 6 756.741 107.744 15 -10 3 4 221.393 73.3760 34 -10 3 3 736.384 134.802 34 -10 3 3 866.272 131.301 17 10 3 -3 803.897 142.036 40 -10 3 2 3706.78 278.459 17 10 3 -2 4167.59 314.394 40 -10 3 1 1246.57 167.404 17 10 3 -1 1252.90 184.747 40 -10 3 0 2764.92 241.114 17 10 3 0 2290.74 238.551 40 -10 3 -1 2881.07 260.267 34 -10 3 -1 2654.71 233.534 17 10 3 1 2798.08 258.952 40 -10 3 -2 399.824 97.8341 34 -10 3 -2 486.182 102.929 17 10 3 2 430.827 104.335 40 10 3 3 563.281 107.399 10 -10 3 -3 458.598 95.3013 54 10 3 4 590.974 108.616 10 -10 3 -4 557.568 104.162 54 10 3 4 828.967 123.825 51 -10 3 -4 452.054 91.7465 47 10 3 5 228.333 70.9260 10 -10 3 -5 109.618 58.9884 54 10 3 5 75.3533 45.9661 51 -10 3 -6 73.4287 42.5725 46 10 3 6 85.8943 46.5793 10 -10 3 -7 262.769 55.9047 49 -10 4 7 326.532 53.0704 15 -10 4 6 856.721 90.8906 15 -10 4 3 4090.66 267.827 34 10 4 -3 4534.36 284.124 40 -10 4 2 472.430 97.3184 34 10 4 -2 243.745 77.5185 40 -10 4 1 3162.74 245.529 34 -10 4 1 2984.82 220.006 47 10 4 -1 3310.32 256.779 40 -10 4 0 1115.23 148.089 34 -10 4 0 1341.00 151.796 47 10 4 0 1057.33 148.873 40 -10 4 -1 1986.49 189.638 34 -10 4 -1 1732.58 173.901 47 10 4 1 1973.31 192.572 40 10 4 2 204.273 67.3229 9 10 4 2 175.727 68.5871 51 -10 4 -2 164.836 60.7732 47 -10 4 -2 145.493 53.7141 46 10 4 2 85.5431 50.1508 40 10 4 3 1659.13 158.657 51 -10 4 -3 1580.18 154.470 47 -10 4 -3 1770.79 161.745 46 10 4 4 228.331 63.4959 51 -10 4 -4 298.704 65.9552 49 -10 4 -4 288.757 64.3160 47 -10 4 -4 199.928 56.4938 46 10 4 5 422.429 71.4770 51 -10 4 -5 327.900 62.9768 49 -10 4 -5 383.674 62.8313 47 -10 4 -5 320.566 63.3236 46 10 5 -3 632.490 81.5523 60 -10 5 2 1968.57 149.812 34 10 5 -2 1700.71 133.817 9 10 5 -2 1771.52 141.557 60 10 5 -2 1736.57 139.684 40 -10 5 1 762.891 96.8675 34 10 5 -1 877.028 101.416 9 10 5 -1 817.971 99.0757 60 10 5 -1 692.094 93.7258 40 -10 5 0 407.907 71.2423 34 10 5 0 319.678 63.9116 60 10 5 0 275.830 60.1151 9 10 5 0 277.338 62.9782 40 10 5 1 691.119 82.7594 9 10 5 1 630.044 82.4973 60 10 5 1 613.147 76.1466 51 -10 5 -1 727.088 82.7515 47 10 5 1 665.470 86.8504 40 -11 -4 5 1050.11 101.651 54 -11 -4 4 1610.28 135.020 54 11 -4 -4 1648.20 118.474 19 -11 -4 3-10.0950 32.3722 54 11 -4 -3-7.55399 28.6620 19 11 -4 -2 685.641 82.0351 19 11 -4 -1 2884.10 167.695 19 11 -4 0 757.094 84.7642 19 -11 -3 7 533.115 75.3100 54 11 -3 -7 593.229 70.4477 19 -11 -3 6 941.880 111.004 54 11 -3 -6 898.539 98.2609 19 -11 -3 5 860.897 115.982 54 11 -3 -5 837.308 100.381 19 -11 -3 4 286.736 78.4196 54 11 -3 -4 179.903 54.8546 19 -11 -3 3 1831.54 180.604 54 -11 -3 3 2233.44 194.822 25 11 -3 -3 2054.63 167.126 19 -11 -3 2 703.487 118.467 54 -11 -3 2 1011.87 138.075 25 11 -3 -2 778.921 106.251 19 -11 -3 1 418.386 94.9980 54 -11 -3 1 465.175 100.621 25 11 -3 -1 509.458 85.5556 19 -11 -3 0 2828.19 219.904 54 -11 -3 0 3041.53 243.149 25 -11 -3 -1 2526.15 221.301 25 -11 -3 -2 31.2056 52.4788 25 -11 -3 -3 1223.85 147.899 25 -11 -3 -4 889.765 121.934 25 -11 -3 -5 144.125 56.2713 25 11 -2 -8 2084.35 144.490 19 -11 -2 7 1027.24 113.280 24 11 -2 -7 1070.06 114.339 19 -11 -2 6 677.679 109.169 54 -11 -2 6 618.621 99.1587 24 11 -2 -6 754.410 104.740 19 -11 -2 5 825.461 124.873 54 11 -2 -5 682.768 103.557 19 -11 -2 4 2587.57 222.697 54 11 -2 -4 2131.16 181.649 19 -11 -2 3 68.5345 65.0627 54 -11 -2 3 166.775 79.7668 25 11 -2 -3 217.837 67.5704 19 -11 -2 2 4926.36 319.196 54 -11 -2 2 4992.90 334.466 25 -11 -2 1 3662.87 276.764 54 -11 -2 1 3465.37 284.098 25 -11 -2 0 367.412 98.9949 54 -11 -2 0 356.564 100.647 25 -11 -2 -1 2198.48 209.979 54 -11 -2 -1 2137.55 224.596 25 -11 -2 -2 1921.53 194.188 54 -11 -2 -2 2675.87 245.481 25 -11 -2 -3 2413.48 225.704 25 -11 -2 -4 2064.59 199.395 25 11 -2 5 2390.88 185.342 58 -11 -2 -5 2438.21 201.272 25 11 -2 6 1977.21 156.210 58 -11 -2 -6 1979.49 165.436 25 11 -2 7 203.928 48.3710 58 -11 -1 9 5039.38 225.829 24 -11 -1 8 1006.39 112.205 24 11 -1 -8 1036.38 114.635 19 -11 -1 7 1914.68 170.633 24 11 -1 -7 2031.97 167.872 19 -11 -1 6 4875.25 297.867 24 11 -1 -6 5220.65 285.067 19 11 -1 -5 360.269 85.8202 19 -11 -1 4 3522.27 266.026 54 11 -1 -4 3586.49 241.046 19 -11 -1 3 5296.56 339.714 54 -11 -1 3 5847.73 370.806 25 11 -1 -3 5281.45 294.708 19 -11 -1 2 301.351 95.6792 54 -11 -1 2 373.071 117.170 25 -11 -1 1 1492.84 188.501 54 -11 -1 1 1862.51 216.365 25 -11 -1 0 1411.48 186.071 54 -11 -1 0 1270.17 182.001 25 -11 -1 -1 1025.61 152.847 54 -11 -1 -1 1523.18 192.232 25 -11 -1 -2 943.402 145.456 54 -11 -1 -2 1010.65 158.637 25 -11 -1 -3 2359.22 215.849 54 -11 -1 -3 2380.19 227.400 25 11 -1 4 5555.85 309.439 58 -11 -1 -4 5347.27 311.111 54 -11 -1 -4 5249.80 323.855 25 11 -1 5 1716.82 167.921 58 11 -1 6 2423.81 188.696 58 11 -1 7 1774.73 148.976 58 11 -1 7 2137.84 153.444 10 -11 0 9 598.356 80.1668 24 -11 0 8 1381.00 136.418 24 -11 0 7 4214.09 253.972 24 11 0 -7 3750.52 239.145 19 -11 0 6 187.715 69.2755 35 -11 0 6 102.089 57.3463 24 11 0 -6 211.827 75.9960 19 -11 0 5 16349.7 649.964 35 11 0 -5 14647.8 538.715 19 -11 0 4 4753.29 340.394 61 11 0 -4 5373.53 298.122 19 -11 0 3 595.844 132.824 61 -11 0 2 10656.0 560.843 61 -11 0 2 11584.8 524.695 54 -11 0 2 12271.2 550.376 25 -11 0 1 4914.51 338.732 54 -11 0 1 5469.16 359.471 25 -11 0 0 699.552 132.781 54 -11 0 -1 1775.73 222.908 61 -11 0 -1 2063.89 219.654 54 -11 0 -2 62.8164 70.4270 61 -11 0 -2 37.4251 53.6774 54 -11 0 -3 1113.62 154.450 54 -11 0 -4 48.3545 56.6262 54 11 0 5 2749.61 213.103 58 -11 0 -5 2426.30 201.929 54 11 0 6-12.5137 35.8922 10 11 0 6-12.7505 36.5713 58 11 0 7 50.2982 35.3599 10 11 0 7 97.7419 41.2256 58 11 0 8 990.620 99.5824 58 -11 1 9 4730.87 212.248 24 11 1 -9 4501.03 222.897 21 -11 1 8 1082.79 111.894 24 11 1 -8 869.211 107.620 21 -11 1 7 2299.60 191.115 35 -11 1 7 1955.03 161.822 24 -11 1 6 5034.61 311.492 35 -11 1 5 361.870 97.3894 35 11 1 -5 487.109 93.7647 19 -11 1 4 3194.79 273.731 35 -11 1 4 3046.28 257.068 61 -11 1 3 5274.84 358.951 35 -11 1 3 5886.51 375.292 61 -11 1 2 405.478 109.122 35 -11 1 2 580.561 132.906 61 -11 1 1 1806.90 208.026 35 -11 1 1 2143.29 235.477 61 -11 1 0 1864.41 223.211 61 -11 1 0 1458.19 182.832 54 -11 1 -1 1325.24 184.889 61 -11 1 -1 1209.29 166.020 54 -11 1 -2 1120.95 161.743 61 -11 1 -2 1128.20 156.181 17 -11 1 -2 1206.05 162.859 54 -11 1 -3 2075.98 208.911 54 11 1 3 2085.69 198.472 10 -11 1 -4 5641.67 335.419 54 11 1 4 5768.93 327.917 10 -11 1 -5 1713.14 173.046 54 11 1 5 1599.11 165.669 10 11 1 6 2377.51 183.133 58 -11 1 -6 2344.40 184.139 54 11 1 6 2440.04 192.683 10 11 1 7 1845.98 147.779 58 -11 1 -7 1753.06 138.872 54 11 1 7 1784.71 146.642 10 -11 2 8 2235.44 145.211 15 11 2 -8 2107.70 148.197 21 -11 2 7 1021.16 110.907 15 11 2 -7 1026.29 112.346 21 -11 2 6 675.047 109.283 35 -11 2 5 860.950 127.215 35 -11 2 4 1550.79 182.038 35 -11 2 3 71.3268 57.2094 35 -11 2 3 127.294 60.3998 17 -11 2 3 106.241 67.2079 61 -11 2 2 4876.93 322.293 35 -11 2 2 4544.11 305.852 17 -11 2 2 4698.33 326.186 61 -11 2 1 3280.55 260.699 17 -11 2 1 3160.72 272.393 61 -11 2 0 351.157 94.4333 17 -11 2 0 368.204 100.411 61 -11 2 -1 1966.95 197.599 17 -11 2 -1 2092.04 212.887 61 -11 2 -1 1903.79 191.998 54 -11 2 -2 1919.95 186.481 17 -11 2 -2 1704.73 180.842 54 -11 2 -3 2226.21 205.748 54 11 2 3 2475.47 206.700 10 -11 2 -4 1841.43 180.576 54 11 2 4 1983.65 182.299 10 -11 2 -5 2657.21 200.794 54 11 2 5 2945.27 209.899 10 -11 2 -6 1891.11 155.730 54 11 2 6 1658.60 146.906 10 11 2 7 295.752 58.1287 10 -11 3 7 301.925 54.8197 15 -11 3 6 795.833 92.6888 15 -11 3 4 232.272 65.5594 34 -11 3 3 1977.73 186.200 34 -11 3 3 1785.84 164.841 17 11 3 -3 1728.27 175.341 40 -11 3 2 828.825 127.930 34 -11 3 2 651.962 106.064 17 11 3 -2 725.962 123.110 40 -11 3 1 509.431 105.939 34 -11 3 1 662.071 109.746 17 11 3 -1 634.338 118.979 40 -11 3 0 2789.62 230.766 34 -11 3 0 2716.53 217.680 17 11 3 0 2683.97 231.887 40 -11 3 -1 1907.56 186.283 34 -11 3 -1 2250.85 189.769 17 11 3 1 2140.39 201.589 40 -11 3 -2 48.5952 36.9802 17 11 3 2 113.124 51.7160 40 11 3 3 1091.10 124.813 51 -11 3 -3 1239.56 133.783 47 11 3 4 922.499 106.283 51 -11 3 -4 824.155 100.677 47 11 3 4 1006.89 111.228 10 -11 3 -5 205.870 50.1054 46 -11 4 3 9.80327 29.8257 34 11 4 -3 10.0309 30.5180 60 11 4 -3 26.7029 31.2696 9 11 4 -3 48.8967 32.8925 40 -11 4 2 723.471 99.0071 34 11 4 -2 733.468 96.9734 9 11 4 -2 688.237 98.3265 40 -11 4 1 2626.69 191.291 34 11 4 -1 2643.83 184.013 9 11 4 -1 2673.64 196.016 40 -11 4 0 827.507 107.753 34 11 4 0 662.644 94.7901 9 -11 4 0 695.778 92.5216 47 11 4 0 713.849 99.2211 40 -11 4 -1 2121.19 161.676 34 11 4 1 1663.46 146.499 60 11 4 1 2315.12 162.529 9 11 4 1 1994.87 153.142 51 -11 4 -1 1978.61 152.990 47 -11 4 -1 2046.37 147.951 46 11 4 1 2203.44 167.976 40 11 4 2 2900.73 177.656 51 -11 4 -2 2784.32 176.214 47 -11 4 -2 2887.93 173.363 46 11 4 3 223.912 49.0064 51 -11 4 -3 161.994 45.7306 47 -11 4 -3 170.588 43.9027 46 -12 -3 4 133.443 47.8150 54 12 -3 -4 170.695 44.4190 19 -12 -3 3 4960.17 249.517 54 12 -3 -3 5204.31 222.554 19 -12 -3 2 154.412 58.2421 54 12 -3 -2 252.894 51.9464 19 -12 -3 1 5042.48 253.875 54 -12 -3 1 4765.06 252.397 25 -12 -3 0 1564.00 144.902 25 -12 -3 -1 128.842 49.9474 25 -12 -3 -2 1320.95 127.337 25 -12 -2 6 2004.75 138.215 24 12 -2 -6 1967.22 136.740 19 -12 -2 5 872.606 105.108 54 -12 -2 5 823.493 100.743 24 12 -2 -5 942.839 101.248 19 -12 -2 4 5422.33 281.541 54 12 -2 -4 5537.91 255.357 19 -12 -2 3 51.4526 47.0307 54 12 -2 -3-9.33147 31.3843 19 -12 -2 2 6997.13 348.370 54 -12 -2 2 7963.97 377.344 25 -12 -2 1 899.739 123.798 54 -12 -2 1 785.896 124.006 25 -12 -2 0 159.838 63.4255 54 -12 -2 0 177.254 63.6214 25 -12 -2 -1 1591.18 154.147 54 -12 -2 -1 1642.43 168.276 25 -12 -2 -2 449.385 81.1319 54 -12 -2 -2 694.734 107.965 25 -12 -2 -3 1667.07 155.298 25 -12 -2 -4 1700.35 146.534 25 -12 -1 7 2736.15 166.565 24 12 -1 -7 2590.09 160.025 19 -12 -1 6 1258.47 132.843 35 -12 -1 6 1141.61 119.032 24 12 -1 -6 1059.67 110.877 19 -12 -1 5 814.354 117.937 35 -12 -1 5 503.069 87.0860 24 12 -1 -5 636.032 90.2639 19 -12 -1 4 424.477 87.8184 54 12 -1 -4 410.197 76.7816 19 -12 -1 3 4329.58 297.989 61 -12 -1 3 4134.79 265.148 54 -12 -1 2 616.872 109.738 54 -12 -1 2 907.141 139.028 25 -12 -1 1 1032.71 141.041 54 -12 -1 1 1047.26 145.857 25 -12 -1 0 2373.12 209.841 54 -12 -1 0 2421.94 217.155 25 -12 -1 -1 276.071 84.0802 61 -12 -1 -1 353.611 84.6850 54 -12 -1 -1 262.959 80.1573 25 -12 -1 -2 636.368 117.795 61 -12 -1 -2 631.599 111.682 25 -12 -1 -3 486.853 87.7101 54 12 -1 5 162.366 48.4895 10 -12 0 7 25.5532 28.6508 24 -12 0 6 12.1205 36.8724 35 -12 0 6-10.2029 32.7177 24 12 0 -6-9.53822 34.8738 19 -12 0 5 776.253 118.217 35 -12 0 5 649.762 98.5678 24 12 0 -5 730.238 97.8644 19 -12 0 4 128.091 60.7709 35 -12 0 4 59.4075 49.9746 61 -12 0 3 118.577 66.5532 35 -12 0 3 84.8105 64.3838 61 -12 0 2 1815.77 196.810 35 -12 0 2 2412.57 228.380 61 -12 0 2 1952.08 186.772 54 -12 0 1 545.621 111.722 35 -12 0 1 713.148 136.322 61 -12 0 1 560.365 108.734 54 -12 0 0 2286.35 225.320 61 -12 0 0 2030.28 197.280 54 -12 0 -1 1553.56 183.092 61 -12 0 -1 1480.07 165.468 54 -12 0 -2 2212.44 202.513 61 -12 0 -2 2805.80 218.325 54 12 0 3 11.8953 38.1483 10 -12 0 -3 53.2601 44.7846 54 -12 0 -4 1821.86 159.888 54 12 0 4 1858.71 159.041 10 -12 0 -5 797.264 98.0405 54 12 0 5 959.195 107.119 10 12 0 6 140.590 43.4545 10 -12 1 7 2342.16 160.425 35 12 1 -7 2787.40 161.751 21 -12 1 6 942.979 114.143 35 -12 1 5 601.703 102.937 35 -12 1 4 604.601 108.377 35 -12 1 3 3784.97 264.616 35 -12 1 3 3680.18 249.107 17 -12 1 3 4080.88 274.332 61 -12 1 2 758.705 123.418 35 -12 1 2 767.515 128.495 61 -12 1 2 797.696 122.889 17 -12 1 1 1081.81 150.759 61 -12 1 1 854.395 129.108 17 -12 1 0 2114.28 196.683 17 -12 1 0 1976.47 201.478 61 -12 1 0 1887.56 181.296 54 -12 1 -1 285.008 82.0549 61 -12 1 -1 316.670 88.9555 17 -12 1 -1 316.727 81.4686 54 -12 1 -2 688.198 104.888 17 -12 1 -2 573.504 104.930 61 -12 1 -2 775.670 117.296 54 12 1 3 623.315 96.1069 10 -12 1 -3 614.679 103.669 54 -12 1 -4 900.134 114.890 54 12 1 4 1070.32 117.570 10 12 1 5 148.165 47.9419 10 -12 1 -5 119.814 45.8481 54 -12 2 6 1982.90 134.715 15 -12 2 4 4693.30 267.064 35 -12 2 4 4738.40 260.444 34 -12 2 3 38.7834 41.4764 35 -12 2 3 138.315 52.2875 17 12 2 -3 64.7331 43.5621 40 -12 2 2 6315.40 323.015 35 -12 2 2 6723.84 327.125 17 -12 2 1 849.655 118.799 17 -12 2 0 167.474 61.3240 17 12 2 0 114.588 54.4031 40 -12 2 -1 1815.66 162.405 17 12 2 1 1621.26 163.300 40 -12 2 -2 461.469 78.1803 17 -12 2 -2 626.156 94.1248 54 -12 2 -3 1470.86 138.421 54 -12 2 -4 1398.79 125.928 54 12 2 4 1250.82 114.311 10 -12 3 4 210.509 43.3969 15 -12 3 3 4770.78 237.888 34 12 3 -3 4767.89 238.628 40 -12 3 2 266.798 62.3364 34 12 3 -2 245.683 60.4847 40 -12 3 1 4467.06 247.322 34 12 3 -1 4681.85 254.739 40 -12 3 0 1041.51 117.525 34 12 3 0 1250.80 128.966 40 -12 3 -1 48.3306 36.7027 34 -12 3 -1 66.6191 39.8161 47 12 3 1 150.667 48.8689 40 12 3 2 843.580 90.6043 51 -12 3 -2 1069.67 105.841 47 -12 3 -3 1302.96 107.092 46 -13 -2 2 2854.45 175.810 35 -13 -2 2 2657.52 173.392 61 -13 -2 2 2845.29 169.306 54 -13 -2 1 1021.57 110.959 61 -13 -2 1 863.028 93.6761 54 -13 -2 0 553.426 81.3327 61 -13 -2 0 644.314 79.5124 54 -13 -2 0 838.280 95.7591 25 -13 -1 4 1289.55 120.151 35 -13 -1 4 1406.20 114.769 24 -13 -1 3 3681.43 215.053 35 -13 -1 3 3599.07 211.725 61 -13 -1 3 3608.95 200.112 54 -13 -1 2 2865.05 191.322 35 -13 -1 2 3056.14 204.354 61 -13 -1 2 2667.55 178.227 54 -13 -1 1-11.7551 33.7163 61 -13 -1 1-10.1566 35.6786 54 -13 -1 0 657.953 99.0221 61 -13 -1 0 684.010 93.7082 54 -13 -1 -1 607.110 87.8937 61 -13 -1 -1 747.110 95.6966 54 -13 -1 -2 468.433 71.4654 54 -13 0 5 76.7192 35.6673 35 -13 0 4 2250.57 163.089 35 -13 0 3 2571.48 181.936 35 -13 0 3 2354.52 165.262 17 -13 0 3 2275.19 170.350 61 -13 0 2 406.069 76.8476 35 -13 0 2 293.503 70.6754 61 -13 0 2 295.534 67.9461 17 -13 0 1 121.207 56.3669 61 -13 0 1 120.369 49.6726 17 -13 0 1 123.120 46.5801 54 -13 0 0 828.723 105.154 17 -13 0 0 1020.52 121.219 61 -13 0 0 885.928 107.964 54 -13 0 -1 3542.52 206.321 17 -13 0 -1 3844.73 222.699 61 -13 0 -1 3573.59 210.706 54 -13 0 -2 18.4259 30.9871 54 -13 0 -3 1087.48 102.324 54 -13 1 4 1095.36 108.364 35 -13 1 3 3428.57 201.414 35 -13 1 3 3602.39 194.680 17 -13 1 2 2621.93 175.685 17 -13 1 2 2923.52 193.768 61 -13 1 1 89.1964 40.2090 17 -13 1 1 22.0045 31.5680 61 -13 1 0 635.075 88.0653 17 -13 1 0 681.194 96.0480 61 -13 1 -1 510.187 74.9412 17 -13 1 -1 486.889 74.0218 54 -13 1 -2 613.247 80.0396 54 -13 2 2 2591.63 161.755 34 -13 2 2 2589.93 152.254 17 13 2 -2 2254.07 152.221 40 -13 2 1 1246.45 115.083 34 -13 2 1 1089.66 100.863 17 13 2 -1 1064.73 106.279 40 -13 2 0 509.233 74.8903 34 -13 2 0 581.484 73.5211 17 13 2 0 499.586 72.4674 40 0 0 0 0.00 0.00 0 TITL exp_692_R81 in P2(1) REM P2(1) (#4 in standard setting) CELL 1.54184 11.040406 6.262138 12.424001 90.0000 94.0350 90.0000 ZERR 4.00 0.000169 0.000086 0.000222 0.0000 0.0015 0.0000 LATT -1 SYMM -x, y+1/2,-z SFAC C H N O UNIT 44.00 40.00 4.00 4.00 TREF HKLF 4 END ; _shelx_hkl_checksum 39136 _shelx_res_file ; TITL 81 in P2(1) III.res created by SHELXL-2018/3 at 15:58:24 on 16-Dec-2022 CELL 1.54184 11.0404 6.2621 12.4240 90.000 94.035 90.000 ZERR 2.00 0.0022 0.0013 0.0025 0.000 0.030 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O S UNIT 34 34 6 10 2 ACTA CONF TEMP 23 L.S. 4 BOND $H EQIV $1 -1+x, +y+1, +z EQIV $2 1+x, +y, +z EQIV $3 -x, -0.5+y, 2-z EQIV $4 +x, 1+y, +z RTAB C4O1 C4' H4'A RTAB C4O1 H4'A O1_$1 RTAB C4O1 C4' O1_$1 RTAB C4O1 C4' H4'A O1_$1 RTAB C10O C10 H10A RTAB C10O H10A O5_$2 RTAB C10O C10 O5_$2 RTAB C10O C10 H10A O5_$2 RTAB C11O C11 H11A RTAB C11O H11A O5_$3 RTAB C11O C11 O5_$3 RTAB C11O C11 H11A O5_$3 RTAB C13O C13 H13A RTAB C13O H13A O3_$4 RTAB C13O C13 O3_$4 RTAB C13O C13 H13A O3_$4 FMAP 2 PLAN 20 WGHT 0.075400 0.124800 FVAR 9.63827 S1 5 0.154185 0.106574 0.659112 11.00000 0.04948 0.04148 = 0.06082 -0.01116 0.00939 0.00459 O1 4 0.672838 -0.137788 0.775567 11.00000 0.06483 0.06346 = 0.10518 0.01167 0.00837 0.02335 O2 4 0.153548 0.161967 0.547903 11.00000 0.06884 0.08959 = 0.05080 -0.01784 0.00789 -0.00149 O3 4 0.153563 -0.112558 0.691376 11.00000 0.07251 0.03607 = 0.12104 -0.01428 0.01511 0.00358 O4 4 -0.106246 0.011377 0.988814 11.00000 0.10868 0.20490 = 0.12040 0.08539 0.03757 0.00644 O5 4 -0.227762 0.280524 0.993601 11.00000 0.12307 0.18583 = 0.11950 -0.02873 0.07097 -0.01607 N1 3 0.558882 0.162895 0.746205 11.00000 0.04050 0.04017 = 0.05327 -0.00294 0.00379 0.00248 N12 3 0.274962 0.215266 0.719846 11.00000 0.04368 0.03758 = 0.04583 0.00138 0.00793 0.00575 N3 3 -0.149335 0.177790 0.953692 11.00000 0.06019 0.14818 = 0.06930 0.00897 0.02439 -0.01272 C2 1 0.647437 0.017602 0.715653 11.00000 0.04436 0.04993 = 0.07245 -0.01100 0.00216 0.00579 C3 1 0.701870 0.064791 0.619068 11.00000 0.04942 0.06941 = 0.07442 -0.02151 0.01435 0.00396 AFIX 43 H3A 2 0.759057 -0.028879 0.594281 11.00000 -1.20000 AFIX 0 C4 1 0.672563 0.243979 0.561542 11.00000 0.06023 0.07230 = 0.06091 -0.01690 0.01942 -0.01179 AFIX 43 H4A 2 0.710971 0.272896 0.498892 11.00000 -1.20000 AFIX 0 C5 1 0.584328 0.386716 0.595994 11.00000 0.06123 0.05606 = 0.04953 -0.00026 0.00947 -0.00819 AFIX 43 H5A 2 0.564335 0.509117 0.556234 11.00000 -1.20000 AFIX 0 C6 1 0.528977 0.344005 0.687459 11.00000 0.04364 0.03945 = 0.04771 -0.00480 0.00233 -0.00419 C7 1 0.434585 0.490535 0.727456 11.00000 0.05701 0.03184 = 0.05951 -0.00023 0.00885 0.00194 AFIX 13 H7A 2 0.451784 0.635774 0.703421 11.00000 -1.20000 AFIX 0 C8 1 0.440069 0.489883 0.849949 11.00000 0.06307 0.05449 = 0.05697 -0.01778 0.00838 0.00111 AFIX 23 H8A 2 0.520190 0.532007 0.879470 11.00000 -1.20000 H8B 2 0.380876 0.588526 0.875750 11.00000 -1.20000 AFIX 0 C9 1 0.412021 0.263795 0.883440 11.00000 0.05463 0.06227 = 0.04149 -0.00163 0.00686 0.00248 AFIX 13 H9A 2 0.413307 0.261073 0.962380 11.00000 -1.20000 AFIX 0 C10 1 0.509426 0.112682 0.850136 11.00000 0.04908 0.05879 = 0.05387 0.01384 0.00392 0.00305 AFIX 23 H10A 2 0.575597 0.113061 0.905801 11.00000 -1.20000 H10B 2 0.476096 -0.030658 0.846320 11.00000 -1.20000 AFIX 0 C11 1 0.285021 0.197702 0.839379 11.00000 0.04999 0.05816 = 0.04737 0.00525 0.01200 0.00801 AFIX 23 H11A 2 0.269259 0.051691 0.860401 11.00000 -1.20000 H11B 2 0.225028 0.289081 0.869484 11.00000 -1.20000 AFIX 0 C13 1 0.306432 0.430032 0.682692 11.00000 0.05053 0.04003 = 0.05783 0.00960 0.00394 0.00856 AFIX 23 H13A 2 0.248524 0.533033 0.706739 11.00000 -1.20000 H13B 2 0.302369 0.432878 0.604459 11.00000 -1.20000 AFIX 0 C1' 1 0.029326 0.231409 0.714917 11.00000 0.03796 0.04222 = 0.05424 -0.00159 0.00184 0.00205 C2' 1 -0.014334 0.146689 0.807050 11.00000 0.03937 0.05465 = 0.06132 0.00876 0.00563 -0.00447 AFIX 43 H2'A 2 0.014481 0.017681 0.835735 11.00000 -1.20000 AFIX 0 C3' 1 -0.103083 0.262351 0.855021 11.00000 0.04257 0.08259 = 0.05721 -0.00527 0.00723 -0.01076 C4' 1 -0.147872 0.451973 0.813621 11.00000 0.04462 0.07565 = 0.08852 -0.02448 0.01158 0.00526 AFIX 43 H4'A 2 -0.207272 0.525883 0.847895 11.00000 -1.20000 AFIX 0 C5' 1 -0.104023 0.531046 0.721207 11.00000 0.05248 0.05633 = 0.09989 0.00397 0.00412 0.01519 AFIX 43 H5'A 2 -0.135141 0.657808 0.691690 11.00000 -1.20000 AFIX 0 C6' 1 -0.013819 0.423705 0.671506 11.00000 0.04898 0.05053 = 0.06819 0.00663 0.00577 0.00587 AFIX 43 H6'A 2 0.017549 0.479393 0.609888 11.00000 -1.20000 AFIX 0 HKLF 4 REM 81 in P2(1) REM wR2 = 0.1136, GooF = S = 1.043, Restrained GooF = 1.043 for all data REM R1 = 0.0394 for 2363 Fo > 4sig(Fo) and 0.0404 for all 2446 data REM 235 parameters refined using 1 restraints END WGHT 0.0754 0.1248 REM Highest difference peak 0.471, deepest hole -0.224, 1-sigma level 0.044 Q1 1 0.6123 0.1270 0.9194 11.00000 0.05 0.47 Q2 1 0.1390 -0.1356 0.7587 11.00000 0.05 0.22 Q3 1 0.1460 0.0111 0.7028 11.00000 0.05 0.21 Q4 1 0.2996 0.7701 0.6606 11.00000 0.05 0.14 Q5 1 0.5986 0.4611 0.9266 11.00000 0.05 0.13 Q6 1 0.4041 0.2828 1.0828 11.00000 0.05 0.13 Q7 1 0.5933 0.6141 0.9333 11.00000 0.05 0.11 Q8 1 -0.2844 0.6601 0.6610 11.00000 0.05 0.11 Q9 1 0.6587 0.5060 0.4105 11.00000 0.05 0.11 Q10 1 -0.1390 0.1183 1.0565 11.00000 0.05 0.10 Q11 1 -0.0343 0.5050 0.7165 11.00000 0.05 0.10 Q12 1 0.2580 0.3709 0.7330 11.00000 0.05 0.10 Q13 1 0.1952 0.3614 0.5521 11.00000 0.05 0.10 Q14 1 0.6773 0.0975 0.6757 11.00000 0.05 0.10 Q15 1 0.3056 0.6136 0.8164 11.00000 0.05 0.10 Q16 1 0.7925 0.3992 0.5618 11.00000 0.05 0.10 Q17 1 -0.2973 0.5606 0.7325 11.00000 0.05 0.10 Q18 1 0.8319 0.1583 0.4400 11.00000 0.05 0.10 Q19 1 0.7826 -0.1485 0.8318 11.00000 0.05 0.10 Q20 1 0.6210 0.6175 0.8845 11.00000 0.05 0.10 ; _shelx_res_checksum 24817 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 S S1 0.15419(6) 0.10657(14) 0.65911(6) 0.0503(2) Uani d 1 . . O O1 0.6728(3) -0.1378(5) 0.7756(3) 0.0777(8) Uani d 1 . . O O2 0.1535(2) 0.1620(5) 0.54790(18) 0.0696(9) Uani d 1 . . O O3 0.1536(3) -0.1126(4) 0.6914(3) 0.0761(8) Uani d 1 . . O O4 -0.1062(4) 0.0114(12) 0.9888(4) 0.143(2) Uani d 1 . . O O5 -0.2278(4) 0.2805(12) 0.9936(3) 0.140(2) Uani d 1 . . N N1 0.5589(2) 0.1629(4) 0.7462(2) 0.0446(6) Uani d 1 . . N N12 0.2750(2) 0.2153(4) 0.71985(18) 0.0421(5) Uani d 1 . . N N3 -0.1493(3) 0.1778(10) 0.9537(3) 0.0916(16) Uani d 1 . . C C2 0.6474(3) 0.0176(6) 0.7157(3) 0.0557(8) Uani d 1 . . C C3 0.7019(3) 0.0648(7) 0.6191(3) 0.0639(11) Uani d 1 . . H H3A 0.759057 -0.028879 0.594281 0.077 Uiso calc 1 . . C C4 0.6726(3) 0.2440(8) 0.5615(3) 0.0638(10) Uani d 1 . . H H4A 0.710971 0.272896 0.498892 0.077 Uiso calc 1 . . C C5 0.5843(3) 0.3867(6) 0.5960(3) 0.0553(8) Uani d 1 . . H H5A 0.564335 0.509117 0.556234 0.066 Uiso calc 1 . . C C6 0.5290(3) 0.3440(5) 0.6875(2) 0.0436(6) Uani d 1 . . C C7 0.4346(3) 0.4905(5) 0.7275(3) 0.0492(7) Uani d 1 . . H H7A 0.451784 0.635774 0.703421 0.059 Uiso calc 1 . . C C8 0.4401(3) 0.4899(7) 0.8499(3) 0.0580(9) Uani d 1 . . H H8A 0.520190 0.532007 0.879470 0.070 Uiso calc 1 . . H H8B 0.380876 0.588526 0.875750 0.070 Uiso calc 1 . . C C9 0.4120(3) 0.2638(7) 0.8834(2) 0.0526(8) Uani d 1 . . H H9A 0.413307 0.261073 0.962380 0.063 Uiso calc 1 . . C C10 0.5094(3) 0.1127(8) 0.8501(2) 0.0539(7) Uani d 1 . . H H10A 0.575597 0.113061 0.905801 0.065 Uiso calc 1 . . H H10B 0.476096 -0.030658 0.846320 0.065 Uiso calc 1 . . C C11 0.2850(3) 0.1977(6) 0.8394(2) 0.0514(8) Uani d 1 . . H H11A 0.269259 0.051691 0.860401 0.062 Uiso calc 1 . . H H11B 0.225028 0.289081 0.869484 0.062 Uiso calc 1 . . C C13 0.3064(3) 0.4300(6) 0.6827(3) 0.0495(7) Uani d 1 . . H H13A 0.248524 0.533033 0.706739 0.059 Uiso calc 1 . . H H13B 0.302369 0.432878 0.604459 0.059 Uiso calc 1 . . C C1' 0.0293(3) 0.2314(5) 0.7149(2) 0.0449(6) Uani d 1 . . C C2' -0.0143(3) 0.1467(6) 0.8071(2) 0.0517(8) Uani d 1 . . H H2'A 0.014481 0.017681 0.835735 0.062 Uiso calc 1 . . C C3' -0.1031(3) 0.2624(8) 0.8550(3) 0.0606(10) Uani d 1 . . C C4' -0.1479(3) 0.4520(8) 0.8136(4) 0.0693(11) Uani d 1 . . H H4'A -0.207272 0.525883 0.847895 0.083 Uiso calc 1 . . C C5' -0.1040(3) 0.5310(7) 0.7212(4) 0.0696(10) Uani d 1 . . H H5'A -0.135141 0.657808 0.691690 0.084 Uiso calc 1 . . C C6' -0.0138(3) 0.4237(6) 0.6715(3) 0.0558(8) Uani d 1 . . H H6'A 0.017549 0.479393 0.609888 0.067 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 S1 0.0495(4) 0.0415(4) 0.0608(4) 0.0046(3) 0.0094(3) -0.0112(4) O1 0.0648(16) 0.0635(19) 0.105(2) 0.0234(14) 0.0084(14) 0.0117(17) O2 0.0688(14) 0.090(3) 0.0508(11) -0.0015(14) 0.0079(10) -0.0178(13) O3 0.0725(17) 0.0361(14) 0.121(2) 0.0036(12) 0.0151(16) -0.0143(15) O4 0.109(3) 0.205(6) 0.120(3) 0.006(4) 0.038(2) 0.085(4) O5 0.123(3) 0.186(6) 0.120(3) -0.016(4) 0.071(3) -0.029(4) N1 0.0405(11) 0.0402(15) 0.0533(12) 0.0025(10) 0.0038(9) -0.0029(11) N12 0.0437(12) 0.0376(14) 0.0458(11) 0.0058(11) 0.0079(9) 0.0014(10) N3 0.060(2) 0.148(5) 0.069(2) -0.013(2) 0.0244(16) 0.009(3) C2 0.0444(15) 0.0499(19) 0.072(2) 0.0058(15) 0.0022(14) -0.0110(18) C3 0.0494(16) 0.069(3) 0.074(2) 0.0040(17) 0.0143(15) -0.022(2) C4 0.060(2) 0.072(3) 0.0609(18) -0.0118(19) 0.0194(16) -0.0169(19) C5 0.0612(19) 0.056(2) 0.0495(16) -0.0082(16) 0.0095(13) -0.0003(15) C6 0.0436(14) 0.0395(16) 0.0477(14) -0.0042(12) 0.0023(11) -0.0048(13) C7 0.0570(16) 0.0318(16) 0.0595(17) 0.0019(13) 0.0089(13) -0.0002(13) C8 0.0631(18) 0.054(2) 0.0570(17) 0.0011(17) 0.0084(14) -0.0178(16) C9 0.0546(17) 0.062(2) 0.0415(13) 0.0025(16) 0.0069(12) -0.0016(15) C10 0.0491(14) 0.0588(19) 0.0539(15) 0.0031(18) 0.0039(12) 0.0138(18) C11 0.0500(15) 0.058(2) 0.0474(14) 0.0080(15) 0.0120(12) 0.0053(15) C13 0.0505(16) 0.0400(17) 0.0578(16) 0.0086(14) 0.0039(13) 0.0096(15) C1' 0.0380(13) 0.0422(17) 0.0542(15) 0.0021(12) 0.0018(11) -0.0016(14) C2' 0.0394(13) 0.055(2) 0.0613(16) -0.0045(14) 0.0056(12) 0.0088(16) C3' 0.0426(15) 0.083(3) 0.0572(17) -0.0108(17) 0.0072(13) -0.0053(19) C4' 0.0446(16) 0.076(3) 0.089(3) 0.0053(18) 0.0116(16) -0.024(2) C5' 0.0525(17) 0.056(2) 0.100(3) 0.0152(17) 0.0041(18) 0.004(2) C6' 0.0490(16) 0.051(2) 0.0682(19) 0.0059(15) 0.0058(14) 0.0066(17) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 O2 S1 O3 . . 120.4(2) ? O2 S1 N12 . . 107.14(14) ? O3 S1 N12 . . 106.87(16) ? O2 S1 C1' . . 108.78(16) ? O3 S1 C1' . . 107.17(17) ? N12 S1 C1' . . 105.56(13) ? C6 N1 C2 . . 122.4(3) ? C6 N1 C10 . . 123.5(3) ? C2 N1 C10 . . 114.0(3) ? C13 N12 C11 . . 112.2(3) ? C13 N12 S1 . . 116.0(2) ? C11 N12 S1 . . 115.6(2) ? O5 N3 O4 . . 125.6(5) ? O5 N3 C3' . . 116.9(6) ? O4 N3 C3' . . 117.5(4) ? O1 C2 N1 . . 118.4(3) ? O1 C2 C3 . . 125.5(3) ? N1 C2 C3 . . 116.1(3) ? C4 C3 C2 . . 121.4(3) ? C4 C3 H3A . . 119.3 ? C2 C3 H3A . . 119.3 ? C3 C4 C5 . . 120.5(3) ? C3 C4 H4A . . 119.7 ? C5 C4 H4A . . 119.7 ? C6 C5 C4 . . 119.4(4) ? C6 C5 H5A . . 120.3 ? C4 C5 H5A . . 120.3 ? C5 C6 N1 . . 120.1(3) ? C5 C6 C7 . . 121.5(3) ? N1 C6 C7 . . 118.4(3) ? C6 C7 C8 . . 110.5(3) ? C6 C7 C13 . . 112.0(3) ? C8 C7 C13 . . 109.5(3) ? C6 C7 H7A . . 108.2 ? C8 C7 H7A . . 108.2 ? C13 C7 H7A . . 108.2 ? C9 C8 C7 . . 106.5(3) ? C9 C8 H8A . . 110.4 ? C7 C8 H8A . . 110.4 ? C9 C8 H8B . . 110.4 ? C7 C8 H8B . . 110.4 ? H8A C8 H8B . . 108.6 ? C10 C9 C8 . . 110.3(3) ? C10 C9 C11 . . 112.7(3) ? C8 C9 C11 . . 110.8(3) ? C10 C9 H9A . . 107.6 ? C8 C9 H9A . . 107.6 ? C11 C9 H9A . . 107.6 ? N1 C10 C9 . . 114.9(3) ? N1 C10 H10A . . 108.5 ? C9 C10 H10A . . 108.5 ? N1 C10 H10B . . 108.5 ? C9 C10 H10B . . 108.5 ? H10A C10 H10B . . 107.5 ? N12 C11 C9 . . 109.9(2) ? N12 C11 H11A . . 109.7 ? C9 C11 H11A . . 109.7 ? N12 C11 H11B . . 109.7 ? C9 C11 H11B . . 109.7 ? H11A C11 H11B . . 108.2 ? N12 C13 C7 . . 110.2(2) ? N12 C13 H13A . . 109.6 ? C7 C13 H13A . . 109.6 ? N12 C13 H13B . . 109.6 ? C7 C13 H13B . . 109.6 ? H13A C13 H13B . . 108.1 ? C2' C1' C6' . . 121.7(3) ? C2' C1' S1 . . 118.9(3) ? C6' C1' S1 . . 119.1(2) ? C1' C2' C3' . . 117.0(3) ? C1' C2' H2'A . . 121.5 ? C3' C2' H2'A . . 121.5 ? C4' C3' C2' . . 122.5(3) ? C4' C3' N3 . . 119.4(4) ? C2' C3' N3 . . 118.1(4) ? C5' C4' C3' . . 119.2(3) ? C5' C4' H4'A . . 120.4 ? C3' C4' H4'A . . 120.4 ? C4' C5' C6' . . 120.5(4) ? C4' C5' H5'A . . 119.8 ? C6' C5' H5'A . . 119.8 ? C5' C6' C1' . . 119.1(3) ? C5' C6' H6'A . . 120.5 ? C1' C6' H6'A . . 120.5 ? 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 S1 O2 . 1.424(3) ? S1 O3 . 1.430(3) ? S1 N12 . 1.634(3) ? S1 C1' . 1.768(3) ? O1 C2 . 1.245(5) ? O4 N3 . 1.214(8) ? O5 N3 . 1.212(7) ? N1 C6 . 1.376(4) ? N1 C2 . 1.407(4) ? N1 C10 . 1.471(4) ? N12 C13 . 1.471(4) ? N12 C11 . 1.485(4) ? N3 C3' . 1.460(5) ? C2 C3 . 1.411(5) ? C3 C4 . 1.357(6) ? C3 H3A . 0.9300 ? C4 C5 . 1.411(6) ? C4 H4A . 0.9300 ? C5 C6 . 1.354(4) ? C5 H5A . 0.9300 ? C6 C7 . 1.499(4) ? C7 C8 . 1.519(4) ? C7 C13 . 1.531(5) ? C7 H7A . 0.9800 ? C8 C9 . 1.514(6) ? C8 H8A . 0.9700 ? C8 H8B . 0.9700 ? C9 C10 . 1.512(5) ? C9 C11 . 1.526(5) ? C9 H9A . 0.9800 ? C10 H10A . 0.9700 ? C10 H10B . 0.9700 ? C11 H11A . 0.9700 ? C11 H11B . 0.9700 ? C13 H13A . 0.9700 ? C13 H13B . 0.9700 ? C1' C2' . 1.379(4) ? C1' C6' . 1.390(5) ? C2' C3' . 1.386(5) ? C2' H2'A . 0.9300 ? C3' C4' . 1.372(7) ? C4' C5' . 1.370(6) ? C4' H4'A . 0.9300 ? C5' C6' . 1.383(5) ? C5' H5'A . 0.9300 ? C6' H6'A . 0.9300 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C4' H4'A O1 1_465 0.93 2.613 3.257(5) 127 y C10 H10A O5 1_655 0.97 2.583 3.460(6) 151 y C11 H11A O5 2_547 0.97 2.549 3.428(7) 150 y C13 H13A O3 1_565 0.97 2.456 3.330(4) 150 y 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 O2 S1 N12 C13 . . . . 38.6(2) ? O3 S1 N12 C13 . . . . 168.9(2) ? C1' S1 N12 C13 . . . . -77.3(2) ? O2 S1 N12 C11 . . . . 173.1(2) ? O3 S1 N12 C11 . . . . -56.6(3) ? C1' S1 N12 C11 . . . . 57.3(3) y C6 N1 C2 O1 . . . . 177.1(3) ? C10 N1 C2 O1 . . . . 1.8(5) ? C6 N1 C2 C3 . . . . -1.8(4) ? C10 N1 C2 C3 . . . . -177.0(3) ? O1 C2 C3 C4 . . . . -176.7(4) ? N1 C2 C3 C4 . . . . 2.0(5) ? C2 C3 C4 C5 . . . . -1.3(6) ? C3 C4 C5 C6 . . . . 0.2(5) ? C4 C5 C6 N1 . . . . 0.1(5) ? C4 C5 C6 C7 . . . . -180.0(3) ? C2 N1 C6 C5 . . . . 0.8(4) ? C10 N1 C6 C5 . . . . 175.6(3) ? C2 N1 C6 C7 . . . . -179.2(3) ? C10 N1 C6 C7 . . . . -4.4(4) ? C5 C6 C7 C8 . . . . -147.0(3) ? N1 C6 C7 C8 . . . . 33.0(4) ? C5 C6 C7 C13 . . . . 90.6(4) ? N1 C6 C7 C13 . . . . -89.4(3) ? C6 C7 C8 C9 . . . . -62.1(3) ? C13 C7 C8 C9 . . . . 61.7(4) ? C7 C8 C9 C10 . . . . 64.2(3) ? C7 C8 C9 C11 . . . . -61.3(3) ? C6 N1 C10 C9 . . . . 6.1(5) ? C2 N1 C10 C9 . . . . -178.7(3) ? C8 C9 C10 N1 . . . . -36.5(4) ? C11 C9 C10 N1 . . . . 87.9(4) ? C13 N12 C11 C9 . . . . -55.3(4) ? S1 N12 C11 C9 . . . . 168.5(2) ? C10 C9 C11 N12 . . . . -65.9(4) ? C8 C9 C11 N12 . . . . 58.2(4) ? C11 N12 C13 C7 . . . . 56.7(3) ? S1 N12 C13 C7 . . . . -167.3(2) ? C6 C7 C13 N12 . . . . 62.7(3) ? C8 C7 C13 N12 . . . . -60.3(4) ? O2 S1 C1' C2' . . . . 157.4(3) ? O3 S1 C1' C2' . . . . 25.8(3) ? N12 S1 C1' C2' . . . . -87.9(3) y O2 S1 C1' C6' . . . . -29.2(3) ? O3 S1 C1' C6' . . . . -160.8(3) ? N12 S1 C1' C6' . . . . 85.5(3) ? C6' C1' C2' C3' . . . . -0.3(5) ? S1 C1' C2' C3' . . . . 173.0(2) ? C1' C2' C3' C4' . . . . 0.7(5) ? C1' C2' C3' N3 . . . . -179.0(3) ? O5 N3 C3' C4' . . . . 1.1(6) ? O4 N3 C3' C4' . . . . -178.9(5) ? O5 N3 C3' C2' . . . . -179.3(4) ? O4 N3 C3' C2' . . . . 0.8(6) ? C2' C3' C4' C5' . . . . 0.2(6) ? N3 C3' C4' C5' . . . . 179.8(4) ? C3' C4' C5' C6' . . . . -1.4(6) ? C4' C5' C6' C1' . . . . 1.8(6) ? C2' C1' C6' C5' . . . . -0.9(5) ? S1 C1' C6' C5' . . . . -174.1(3) ? _cod_database_fobs_code 2244234