#------------------------------------------------------------------------------ #$Date: 2021-09-08 05:05:53 +0300 (Wed, 08 Sep 2021) $ #$Revision: 269046 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/39/2243909.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_2243909 loop_ _publ_author_name 'Turgunov, Kambarali' 'Ziyadullaev, Mirjalol' 'Khoshimov, Farkhod' 'Karimov, Rikhsiboy' 'Elmuradov, Burkhon' _publ_section_title ; Crystal structures of 6-nitroquinazolin-4(3H)-one, 6-aminoquinazolin-4(3H)-one and 4-aminoquinazoline hemihydrochloride dihydrate ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first ; ; _journal_paper_doi 10.1107/S2056989021008823 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac 'C8 H5 N3 O3' _chemical_formula_moiety 'C8 H5 N3 O3' _chemical_formula_sum 'C8 H5 N3 O3' _chemical_formula_weight 191.15 _chemical_melting_point 560(2) _chemical_name_systematic ; 6-Nitroquinazolin-4(3H)-one ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 105.654(12) _cell_angle_beta 98.560(13) _cell_angle_gamma 90.784(13) _cell_formula_units_Z 2 _cell_length_a 5.5587(9) _cell_length_b 8.6673(13) _cell_length_c 8.7649(12) _cell_measurement_reflns_used 950 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 74.4730 _cell_measurement_theta_min 5.2610 _cell_volume 401.45(11) _computing_cell_refinement ; CrysAlisPro (Rigaku OD, 2018) ; _computing_data_collection ; CrysAlisPro (Rigaku OD, 2018) ; _computing_data_reduction ; CrysAlisPro (Rigaku OD, 2018) ; _computing_molecular_graphics ; XP in SHELXTL (Sheldrick, 2008) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2014/7 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2018/2 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.2576 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.960 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku Xcalibur, Ruby' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_unetI/netI 0.0458 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 2652 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.251 _diffrn_reflns_theta_min 5.308 _diffrn_source 'Enhance (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.073 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.74240 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2018) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.581 _exptl_crystal_description prism _exptl_crystal_F_000 196 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _refine_diff_density_max 0.181 _refine_diff_density_min -0.173 _refine_ls_extinction_coef 0.012(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2014/7 (Sheldrick, 2015b) ; _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 132 _refine_ls_number_reflns 1598 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0469 _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^)+(0.0615P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1250 _refine_ls_wR_factor_ref 0.1453 _reflns_number_gt 1124 _reflns_number_total 1598 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file dj2030sup1.cif _cod_data_source_block I _cod_database_code 2243909 _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 ; -1 1 0 859713. 8365.54 1 1 -1 0 865048. 8292.51 22 2 -2 0 8195.31 1205.96 22 3 -3 0 14659.0 2074.38 22 -4 4 0 394.697 256.181 4 -4 4 0 287.902 210.016 6 4 -4 0 114.079 238.730 22 -5 5 0 901.600 333.445 4 -6 5 0 17.1361 93.5731 4 -5 4 0 271.356 196.200 4 -4 3 0 1652.64 467.152 5 4 -3 0 1377.09 405.587 13 4 -3 0 2400.00 934.107 22 3 -2 0 2887.13 864.228 22 -2 1 0 73538.1 3192.13 1 -1 0 0 558646. 5451.67 1 0 -1 0 33038.0 1157.73 20 0 1 0 32871.3 977.804 3 0 -1 0 32666.4 1079.86 22 1 -2 0 95979.3 3268.51 22 2 -3 0 69163.7 3827.95 22 3 -4 0-112.080 206.219 22 -4 5 0 26671.6 1962.32 4 -4 5 0 28037.7 1925.89 6 -5 6 0 16979.1 1311.34 4 -5 6 0 16465.7 1081.28 6 -6 4 0 41.1034 88.8648 4 -5 3 0 97.5650 139.336 5 5 -3 0 72.9171 144.785 13 -4 2 0 39693.3 2106.83 5 4 -2 0 38858.9 3753.61 22 3 -1 0 13668.0 1797.28 22 -3 1 0 13705.6 1725.58 1 -2 0 0 125859. 3830.71 1 -1 -1 0 207586. 3350.72 1 0 -2 0 402292. 5473.04 22 0 -2 0 399127. 5716.94 20 0 2 0 398144. 4812.63 3 1 -3 0 81675.1 2098.23 21 -1 3 0 79994.0 2223.70 3 1 -3 0 76435.9 3346.85 22 2 -4 0 2771.08 844.113 22 -3 5 0 8637.04 1056.75 6 3 -5 0 9001.66 1840.61 22 -3 5 0 9574.55 1137.29 4 -4 6 0 40402.4 2272.29 6 -4 6 0 40195.9 2345.46 4 -5 7 0-66.8469 90.4370 11 6 -3 0 1106.87 287.341 13 -6 3 0 1087.19 336.514 4 -5 2 0 262.141 168.816 5 5 -2 0 174.366 169.056 13 4 -1 0 273.691 315.109 22 -3 0 0 747.952 382.246 1 -2 -1 0 402718. 6570.94 1 -1 -2 0 132141. 3771.03 20 0 3 0 137629. 3508.24 3 0 -3 0 137395. 4252.69 20 1 -4 0 753.910 407.827 22 2 -5 0 10154.2 1741.58 22 -3 6 0 761.638 344.447 4 -3 6 0 584.932 312.859 6 -4 7 0 270.008 191.381 11 -4 7 0 81.3766 123.903 6 6 -2 0 158.667 146.427 13 -5 1 0-20.5496 95.0560 5 4 0 0 8054.63 1612.38 22 -3 -1 0-65.2871 115.085 1 -2 -2 0 199916. 4718.99 1 1 3 0 18625.2 1667.03 3 -1 -3 0 17630.5 1648.86 20 0 4 0 516.785 238.340 3 0 -4 0 784.611 413.285 20 1 -5 0 4565.03 1059.01 20 -2 6 0 8067.12 1039.29 6 2 -6 0 8750.53 1709.51 20 -2 6 0 8463.24 1025.05 11 2 -6 0 6849.43 1565.91 22 -2 6 0 8106.84 1040.08 4 -3 7 0 337.309 230.802 6 -3 7 0 117.146 145.982 11 -4 8 0 545.377 219.450 6 -4 8 0 613.057 236.241 11 6 -1 0 919.070 289.205 13 -6 1 0 592.280 259.941 5 5 0 0 3072.12 643.907 12 -5 0 0 3665.28 657.484 5 4 1 0-3.04438 350.221 3 4 1 0-73.9733 115.320 12 3 2 0 229271. 8364.05 3 2 3 0 413932. 10049.1 3 -2 -3 0 433148. 7510.89 1 -1 -4 0 1889.27 664.805 20 1 4 0 2830.43 739.339 3 0 5 0 43240.6 2610.09 3 0 -5 0 36281.4 3026.35 20 1 -6 0 220.837 283.572 20 -2 7 0 1722.01 513.055 6 -2 7 0 1657.60 475.627 11 -3 8 0 1734.59 464.541 6 -3 8 0 1716.93 434.683 11 6 0 0 578.046 291.640 13 -6 0 0 424.000 174.027 5 5 1 0 180.349 206.847 12 5 1 0 206.051 192.293 9 4 2 0 3500.50 665.597 12 4 2 0 3762.92 749.087 8 4 2 0 3142.35 1197.88 3 3 3 0 21560.4 2781.89 3 2 4 0 47167.2 3498.19 3 -1 -5 0 4182.28 1094.77 20 1 5 0 5398.66 1088.16 3 0 -6 0-185.043 266.206 20 -1 7 0 9909.79 1146.83 11 -1 7 0 8245.33 1072.15 6 1 -7 0 10003.6 1981.93 20 -2 8 0 11109.0 1180.95 11 -2 8 0 11567.6 1236.66 15 -2 8 0 10508.7 1133.40 10 -2 8 0 10951.2 1183.22 6 -3 9 0 535.751 188.565 10 -6 -1 0 9833.67 857.321 5 6 1 0 10178.8 1065.97 13 5 2 0-1.25013 91.6943 12 4 3 0 354.338 425.869 3 4 3 0 153.031 166.825 12 4 3 0-123.676 238.689 8 3 4 0 4410.99 1319.06 3 3 4 0 5217.85 842.706 14 2 5 0 2705.77 838.404 3 1 6 0 3312.30 633.367 10 -1 -6 0 2177.40 860.482 20 1 6 0 2566.45 583.007 14 0 7 0 1920.20 478.271 6 0 7 0 1810.29 500.614 14 0 -7 0 1446.20 747.506 20 0 7 0 1643.20 446.627 10 -1 8 0 5635.01 865.195 10 -1 8 0 5103.97 827.434 6 -2 9 0 3012.39 540.593 15 -2 9 0 3004.21 539.341 10 6 2 0 79.8083 103.600 9 6 2 0-63.9880 119.344 13 5 3 0 659.715 317.633 8 5 3 0 78.4322 127.210 12 4 4 0 3284.16 730.204 8 4 4 0 3394.26 640.796 12 3 5 0 129.899 180.540 14 3 5 0 928.219 604.571 3 2 6 0 19352.1 1664.43 14 2 6 0 19318.5 2557.05 3 1 7 0 32588.1 2243.19 14 0 8 0 19137.8 1599.24 10 -1 9 0 653.848 268.083 10 -1 9 0 1288.53 369.785 15 6 3 0 1233.46 314.806 13 6 3 0 1472.88 363.846 9 5 4 0 2011.96 440.967 12 5 4 0 2048.78 529.209 8 4 5 0 1631.63 527.838 8 3 6 0 1142.30 424.094 14 2 7 0 2557.40 650.489 14 1 8 0 2479.75 624.631 14 0 9 0 333.990 162.774 15 -1 10 0 118.558 112.057 15 6 4 0 918.230 182.398 13 6 4 0 938.894 255.499 9 5 5 0 6563.36 858.796 8 4 6 0 5160.37 847.835 8 3 7 0 5034.85 842.065 14 2 8 0 6309.09 835.174 15 2 8 0 5830.15 903.249 14 1 9 0 358.020 203.310 14 1 9 0 170.622 133.890 15 0 10 0 4142.33 561.666 15 5 6 0 31.5470 70.1800 19 4 7 0 437.337 215.279 8 3 8 0 1457.40 402.304 8 2 9 0 11589.0 1043.14 8 1 10 0 3901.78 459.764 15 4 8 0 84.1014 88.4148 8 3 9 0 97.2264 124.998 8 2 9 1 4008.70 563.058 8 3 8 1 548.061 237.923 8 4 7 1 1649.41 384.979 8 0 10 1 2491.13 374.923 15 1 9 1 3090.09 526.357 14 1 9 1 3061.43 542.496 15 2 8 1 4676.48 692.878 15 2 8 1 5208.55 800.823 14 3 7 1 2580.70 588.123 14 4 6 1 612.387 289.005 8 5 5 1 96.6863 112.777 8 -1 10 1 1724.56 314.183 15 0 9 1 1374.74 389.317 15 1 8 1 5268.31 859.494 14 2 7 1 332.877 284.771 14 3 6 1 15068.6 1504.34 14 4 5 1 1698.70 429.366 12 4 5 1 1856.32 477.318 8 5 4 1 191.586 150.079 12 5 4 1 352.094 219.085 8 6 3 1 70.1317 119.207 13 -1 9 1 1731.55 410.737 10 -1 9 1 1998.07 470.727 15 0 8 1-318.611 226.420 14 0 8 1 71.8162 128.698 10 1 7 1 38857.1 2406.85 14 2 6 1 275846. 6378.48 14 3 5 1 13855.1 1453.66 14 4 4 1 3486.73 739.117 8 4 4 1 3800.21 700.015 12 5 3 1 599.570 317.301 12 5 3 1 411.481 237.789 8 -6 -2 -1-75.2016 59.4406 5 -2 9 1 313.483 185.838 15 -2 9 1 396.985 212.504 10 -1 8 1 3476.64 689.813 10 0 7 1 67.5407 283.610 14 0 7 1-25.8043 105.246 10 -1 -6 -1 38654.6 3731.13 20 1 6 1 38573.9 2209.26 10 1 6 1 37529.3 2247.64 14 2 5 1 11441.2 1233.80 14 2 5 1 10513.5 1821.16 3 3 4 1 2207.73 950.249 3 3 4 1 2207.48 564.674 14 4 3 1 5221.05 1476.20 3 4 3 1 5532.36 877.481 12 4 3 1 5391.36 892.711 8 5 2 1 1604.37 460.460 12 -6 -1 -1 13236.5 999.514 5 -3 9 1 1914.05 346.375 10 -2 8 1 17371.6 1485.48 6 -2 8 1 16919.6 1423.64 10 -2 8 1 17115.4 1467.31 11 -1 7 1 1646.91 486.528 11 -1 7 1 2497.36 578.658 6 -1 7 1 1669.46 493.310 10 0 6 1 33167.6 2041.43 10 0 -6 -1 31997.7 3349.70 20 0 6 1 33330.5 2082.60 14 0 6 1 34907.1 2011.88 6 -1 -5 -1 6980.70 1472.49 20 1 5 1 7002.99 1274.36 3 2 4 1 37208.0 3299.45 3 -2 -4 -1 36837.2 2949.97 1 3 3 1 9854.20 1894.97 3 4 2 1 499.085 271.068 12 4 2 1 1314.47 758.632 3 4 2 1 620.491 202.274 8 5 1 1 6638.92 948.557 9 5 1 1 5644.87 887.147 12 6 0 1 13527.4 1180.56 13 -6 0 -1 13340.0 1058.49 5 -3 8 1 264.245 139.337 11 -3 8 1 765.962 270.944 6 -2 7 1-182.599 155.488 6 -2 7 1 49.5454 93.0257 11 1 -6 -1-793.021 518.810 20 -1 6 1-34.8622 106.296 6 -1 6 1-486.815 255.778 11 0 -5 -1 118575. 5894.06 20 1 4 1 6698.05 1144.37 3 -1 -4 -1 5017.64 1100.35 20 -2 -3 -1 963.029 468.312 1 -3 -2 -1 7572.24 1308.45 1 4 1 1 546.247 276.542 12 5 0 1 36.5699 168.079 12 6 -1 1 162.407 205.926 13 -6 1 -1 222.312 121.312 5 -4 8 1 1260.53 296.342 10 -4 8 1 1311.04 304.764 11 -3 7 1 1041.12 386.317 11 -3 7 1 576.158 281.967 6 2 -6 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806.841 4 3 -5 -1 4798.99 1349.14 22 -3 5 1 4721.87 764.381 6 2 -4 -1 14966.9 1999.33 22 1 -3 -1 92316.2 2670.39 21 1 -3 -1 88665.3 3766.69 22 0 -2 -1 60565.1 1913.56 2 0 -2 -1 60556.4 2536.51 20 -1 -1 -1 64512.7 2479.62 1 -2 0 -1 27334.3 2010.60 1 -3 1 -1 35396.7 2910.78 1 -4 2 -1 27749.0 1807.23 5 4 -2 1 25836.3 3080.23 22 4 -2 1 30381.1 1870.22 12 5 -3 1 3736.39 705.097 13 -5 3 -1 2987.61 640.557 5 -6 4 -1 161.833 137.819 4 -5 6 1 6626.39 790.294 11 -4 5 1 68542.9 3117.35 4 -4 5 1 71717.2 3003.91 6 3 -4 -1 515.872 414.302 22 2 -3 -1 357.226 242.253 21 2 -3 -1 733.857 436.321 22 1 -2 -1 2813.26 477.667 21 1 -2 -1 2400.97 543.871 22 0 -1 -1 114647. 2409.42 2 0 -1 -1 114910. 2611.31 20 -1 0 -1 100371. 2854.00 1 -2 1 -1 37744.7 2447.57 1 3 -2 1 35702.8 3091.27 22 -3 2 -1 39331.7 3222.09 1 -4 3 -1 7676.19 967.091 5 4 -3 1 7875.17 1773.65 22 -5 4 -1 4189.25 746.333 4 -6 5 -1 85.1418 86.1160 4 -5 5 1 3594.99 647.286 4 -4 4 1 129.214 155.001 4 4 -4 -1 471.593 436.510 22 -4 4 1 154.512 159.031 6 3 -3 -1 6384.43 1381.66 22 2 -2 -1 51460.9 3052.43 22 1 -1 -1 90722.1 2749.75 22 0 0 -1 8526.41 405.307 20 0 0 -1 8158.47 532.123 3 -1 1 -1 44887.2 2023.42 1 -2 2 -1 21225.9 1972.97 1 3 -3 1 13342.5 1985.21 22 -4 4 -1 2134.83 532.775 5 -4 4 -1 2039.60 518.643 6 4 -4 1 2331.83 944.098 22 -5 5 -1 825.809 315.577 4 -6 5 1 268.575 139.531 11 -5 4 1 199.017 198.993 4 5 -4 -1 8.04293 181.136 13 4 -3 -1 22333.9 2897.31 22 4 -3 -1 22493.9 1686.53 13 3 -2 -1 34907.3 3003.88 22 2 -1 -1 65684.3 3067.69 22 1 0 -1 49760.2 1620.20 22 1 0 -1 49083.8 1536.64 3 0 1 -1 42078.9 1277.49 1 0 1 -1 43702.2 1448.25 3 -1 2 -1 91248.4 2793.27 3 1 -2 1 88210.1 3071.97 22 -1 2 -1 93128.5 3344.18 1 2 -3 1 5681.46 1078.99 22 3 -4 1 258.010 307.672 22 -4 5 -1 2182.88 570.850 4 -4 5 -1 1448.43 479.783 6 -5 6 -1 25426.5 1381.08 6 -5 6 -1 25771.4 1590.15 4 -6 4 1 2807.64 485.167 4 5 -3 -1 27.4103 93.9125 13 -5 3 1-70.9543 142.912 4 4 -2 -1 25678.0 2989.25 22 4 -2 -1 27016.8 1854.54 13 -4 2 1 26837.5 1743.43 5 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323.086 8 4 4 -2 268.777 334.243 3 3 5 -2 4763.66 852.590 8 3 5 -2 5645.62 1503.16 3 2 6 -2-865.311 546.671 3 2 6 -2 80.7025 137.555 14 1 7 -2 42163.8 2560.26 15 1 7 -2 44594.8 3816.48 3 0 8 -2 36378.4 2444.21 15 0 8 -2 36960.3 2114.59 10 -1 9 -2 7890.99 911.077 6 -1 9 -2 7713.80 996.024 15 -2 10 -2 433.751 152.254 15 6 3 -2 87.4996 118.666 9 6 3 -2 127.842 116.996 13 5 4 -2 3282.68 598.415 13 5 4 -2 3357.27 708.783 9 4 5 -2 3829.59 795.752 8 3 6 -2 179.906 188.357 8 2 7 -2 879.842 367.683 14 2 7 -2 907.947 307.548 15 1 8 -2 1402.85 508.447 15 0 9 -2 878.139 375.323 15 -1 10 -2 149.180 86.1887 15 6 4 -2 173.297 116.922 9 5 5 -2 4308.65 754.295 9 5 5 -2 5055.18 735.265 19 4 6 -2 12119.4 1352.49 8 3 7 -2 7996.38 1094.14 8 2 8 -2 6871.20 940.387 15 2 8 -2 7495.76 1025.03 8 1 9 -2 5626.86 913.071 15 0 10 -2 306.099 213.634 15 6 5 -2 59.0855 86.0830 9 5 6 -2 183.798 80.3006 19 5 6 -2 250.256 189.598 9 4 7 -2 29.8379 113.333 8 3 8 -2 714.969 284.997 8 2 9 -2 2070.09 457.569 8 2 9 -2 2375.15 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788.269 20 -1 5 3 1552.12 431.344 11 0 -4 -3 304.423 297.465 20 -1 -3 -3 37537.7 3287.69 1 -2 -2 -3 1415.71 581.869 1 -3 -1 -3 3840.01 1121.26 1 -3 -1 -3 3602.97 638.451 18 -4 0 -3-796.561 560.580 1 4 0 3 168.002 147.267 12 5 -1 3 238.593 192.131 12 -6 2 -3 117.041 104.301 5 -4 7 3 8.38853 125.649 11 -3 6 3 8210.45 1059.99 11 -2 5 3 30323.4 1987.34 11 -2 5 3 26968.3 1858.05 14 2 -5 -3 27616.0 3181.32 20 -2 5 3 24771.7 1797.31 6 1 -4 -3 10704.3 1741.09 20 0 -3 -3 311861. 7349.64 2 0 -3 -3 301445. 8233.37 20 -1 -2 -3 235544. 7322.84 1 -2 -1 -3 10436.2 1603.03 1 -3 0 -3 4082.58 1148.12 1 -4 1 -3 956.428 622.234 1 4 -1 3 699.429 267.568 12 5 -2 3 231.118 178.655 12 -5 2 -3-31.0782 142.938 5 -6 3 -3 197.886 124.314 4 -4 6 3 1425.26 393.612 11 -3 5 3 925.614 328.441 6 -3 5 3 1447.68 457.765 11 2 -4 -3 5756.89 1298.42 20 1 -3 -3 15251.6 1616.34 2 1 -3 -3 15204.2 1806.41 20 0 -2 -3 70259.6 3347.24 2 0 -2 -3 74601.5 3455.22 20 -1 -1 -3 50294.6 3022.43 1 -2 0 -3 4779.73 1059.32 1 -3 1 -3 1029.39 442.488 1 -4 2 -3 7547.94 976.964 6 4 -2 3 6721.72 924.639 12 4 -2 3 6132.82 1616.77 22 -4 2 -3 7535.34 1749.62 1 -5 3 -3 3364.07 633.852 5 -6 4 -3 181.056 112.393 4 -5 6 3-12.0695 116.715 11 -4 5 3 15581.3 1414.58 11 -3 4 3 104327. 3559.70 6 3 -4 -3 105650. 3584.45 13 -3 4 3 100965. 3711.52 4 3 -4 -3 99621.0 5959.29 20 2 -3 -3 1241.23 510.786 21 2 -3 -3 1321.59 559.340 20 1 -2 -3 5320.84 902.691 20 0 -1 -3 1205.52 398.599 2 0 -1 -3 1663.91 427.084 20 -1 0 -3 19966.7 1790.71 1 -2 1 -3 46928.3 3328.49 1 -3 2 -3 4082.49 1200.81 1 -4 3 -3 9990.96 1171.27 6 -4 3 -3 9644.05 1106.99 5 -5 4 -3 1253.88 382.782 4 -5 4 -3 1099.52 358.423 5 -5 5 3 6440.92 762.265 11 -4 4 3 5146.37 852.024 4 4 -4 -3 4430.97 739.828 13 3 -3 -3 199.835 294.155 22 3 -3 -3-285.601 307.354 21 2 -2 -3 9299.00 1391.77 21 2 -2 -3 8317.99 1351.27 22 1 -1 -3 56300.1 2379.39 20 1 -1 -3 54523.3 2826.10 21 0 0 -3 42674.5 2369.27 2 0 0 -3 42300.2 2273.55 1 -1 1 -3 80275.8 3587.70 1 -2 2 -3 35426.2 2977.05 1 3 -3 3 1439.80 626.669 22 -3 3 -3 1403.41 708.894 1 -4 4 -3 1474.97 455.193 6 -4 4 -3 1121.87 441.243 5 -5 5 -3 142.840 159.361 4 -5 5 -3 454.315 227.472 6 5 -4 -3 689.883 269.334 13 -5 4 3 942.216 328.198 4 -4 3 3 557.795 284.275 4 4 -3 -3 1057.94 338.152 16 4 -3 -3 1058.51 409.057 13 4 -3 -3 1809.75 833.154 22 3 -2 -3 45747.8 3625.35 21 3 -2 -3 46918.0 3584.66 22 2 -1 -3 70453.3 3791.71 21 2 -1 -3 70354.9 3424.72 22 1 0 -3 26951.9 1546.36 3 1 0 -3 29962.8 1238.13 20 1 0 -3 26968.3 1923.65 21 0 1 -3 7926.88 979.252 3 0 1 -3 8891.20 1034.63 2 0 1 -3 8736.35 946.806 1 -1 2 -3 2256.73 652.647 1 -2 3 -3 17531.2 2172.16 1 -3 4 -3 2446.74 517.111 5 -3 4 -3 1819.76 518.012 6 3 -4 3 1176.72 644.085 22 -4 5 -3 279.576 218.041 6 -4 5 -3 257.370 183.758 4 -5 6 -3 1562.72 326.623 4 -5 6 -3 1050.18 285.107 6 -6 4 3-5.46436 59.7714 11 5 -3 -3 8633.48 948.087 16 5 -3 -3 8707.95 1036.92 13 -5 3 3 10247.4 1111.41 4 4 -2 -3 341.524 216.391 16 4 -2 -3-78.5941 178.753 13 4 -2 -3 403.443 324.692 22 4 -2 -3 444.421 428.449 21 -4 2 3-156.160 151.670 4 3 -1 -3 97810.4 4689.06 22 3 -1 -3 89233.1 4986.77 21 2 0 -3 385508. 6211.20 3 2 0 -3 384478. 6822.63 22 2 0 -3 368112. 8310.58 21 1 1 -3 113841. 3745.07 3 1 1 -3 112324. 3901.49 21 1 1 -3 114160. 2571.04 1 0 2 -3 47022.7 2269.07 2 0 2 -3 45963.6 2211.48 1 0 2 -3 45191.8 2513.00 3 0 -2 3 43054.8 1084.57 20 -1 3 -3 36448.8 2629.43 3 -1 3 -3 37378.3 2660.81 1 -2 4 -3 484.572 400.910 1 2 -4 3 197.319 237.982 22 -3 5 -3 8553.36 1113.62 6 3 -5 3 9046.53 1805.58 22 -3 5 -3 10831.4 1118.52 5 -3 5 -3 7870.80 999.468 4 -4 6 -3-197.062 165.161 4 -4 6 -3 256.636 247.860 6 6 -3 -3 240.461 128.735 13 -5 2 3 1640.43 479.814 4 5 -2 -3 1932.09 479.638 16 5 -2 -3 1766.46 496.327 13 4 -1 -3 500.991 266.762 13 4 -1 -3 752.026 532.980 21 4 -1 -3 393.675 263.772 9 3 0 -3 10524.7 1671.20 21 3 0 -3 12247.5 1494.20 22 2 1 -3 18271.3 1158.28 22 2 1 -3 17403.8 1573.08 3 2 1 -3 16810.2 1738.12 21 1 2 -3 33725.5 2045.73 21 1 2 -3 33133.0 2157.95 3 1 2 -3 29560.0 790.155 1 0 3 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1482.20 9 4 1 -3 10578.9 1878.01 21 4 1 -3 10293.8 1153.60 13 4 1 -3 10810.4 1203.95 9 3 2 -3 19474.8 2163.57 3 3 2 -3 18934.6 2176.18 21 2 3 -3 1765.09 557.133 21 2 3 -3 958.046 501.143 3 1 4 -3 134847. 5344.73 3 0 5 -3 6946.76 1287.99 3 0 -5 3 8311.57 1205.86 20 -1 6 -3-56.9235 124.931 3 1 -6 3 986.813 437.513 20 -2 7 -3 6656.23 972.570 15 -2 7 -3 6084.31 938.544 6 -3 8 -3 72.0767 136.653 6 6 0 -3 703.467 290.680 13 5 1 -3 2533.49 613.408 9 5 1 -3 2826.54 636.840 13 4 2 -3 129528. 6293.92 3 4 2 -3 120916. 3879.37 13 4 2 -3 112898. 6343.72 21 4 2 -3 119462. 4085.90 9 3 3 -3 7430.15 1453.63 3 3 3 -3 10844.5 1688.59 21 2 4 -3 911.151 530.950 3 1 5 -3 15960.5 2016.63 3 -1 -5 3 18157.8 1799.18 20 0 6 -3 14821.7 2069.10 3 -1 7 -3 2562.24 557.617 7 -1 7 -3 1811.31 540.641 15 -1 7 -3 886.960 354.303 6 -2 8 -3 1878.09 495.717 15 -2 8 -3 1433.20 428.378 6 -3 9 -3 1609.17 371.419 6 6 1 -3 253.631 162.445 13 5 2 -3 126898. 4167.41 13 5 2 -3 123865. 4290.73 9 4 3 -3 102055. 5995.72 3 4 3 -3 99958.5 3502.67 13 4 3 -3 107923. 6272.97 21 4 3 -3 101321. 3619.46 19 4 3 -3 99214.1 3884.24 8 3 4 -3 1425.99 693.508 3 2 5 -3 27357.5 2945.61 3 1 6 -3-163.028 248.092 3 0 7 -3 15191.7 1414.01 7 0 7 -3 15075.5 1489.62 15 -1 8 -3 11331.9 1315.42 15 -1 8 -3 12612.9 1282.63 6 -2 9 -3 23.3330 94.1480 15 -2 9 -3-63.7976 108.815 6 6 2 -3 5.14077 125.139 9 6 2 -3 74.7656 93.9779 13 5 3 -3 333.639 267.035 9 5 3 -3 458.470 248.503 13 4 4 -3 602.636 290.705 8 4 4 -3 1387.75 500.415 19 4 4 -3 1470.45 779.341 3 3 5 -3 11387.9 1299.19 8 3 5 -3 11205.1 2054.48 3 2 6 -3 24271.4 1795.97 8 2 6 -3 24272.9 2945.06 3 2 6 -3 26105.3 1832.44 15 1 7 -3 20909.9 1765.63 15 1 7 -3 24694.9 2956.69 3 0 8 -3 155069. 4974.60 15 -1 9 -3 4791.55 789.680 15 -1 9 -3 5494.12 748.692 6 -2 10 -3-153.161 97.3181 6 6 3 -3 355.718 250.717 9 6 3 -3 334.605 160.580 13 5 4 -3 3187.16 594.295 19 5 4 -3 2521.11 598.976 9 4 5 -3 130.406 170.807 8 3 6 -3 7.00577 172.987 8 2 7 -3 1589.10 496.917 8 2 7 -3 1831.28 549.234 15 1 8 -3 28285.2 2144.63 15 0 9 -3 90.7589 263.128 15 -1 10 -3 1655.05 386.159 15 6 4 -3 1160.65 325.800 9 5 5 -3 3577.00 606.939 19 5 5 -3 3267.07 667.268 9 4 6 -3 2331.75 597.665 8 4 6 -3 2403.28 573.695 19 3 7 -3 780.942 337.430 8 2 8 -3 1561.49 450.553 15 1 9 -3 1676.87 528.681 15 0 10 -3 2776.04 552.363 15 6 5 -3 2281.42 373.151 9 5 6 -3 52.2581 173.048 19 5 6 -3-23.0481 81.8565 9 4 7 -3 131.088 183.028 8 4 7 -3 146.697 89.3103 19 4 7 -3 64.0514 121.473 9 3 8 -3 867.309 299.290 8 3 8 -3 406.302 220.427 19 2 9 -3 2716.98 523.361 15 2 9 -3 2455.69 515.141 19 1 10 -3 179.383 139.277 15 5 7 -3 451.943 168.017 19 5 7 -3 382.941 162.797 9 4 8 -3 356.102 204.742 19 3 9 -3 110.949 120.809 19 1 8 4 32.0854 74.9835 14 2 7 4 134.559 157.819 14 3 6 4 310.276 171.983 8 3 6 4 252.639 160.399 14 4 5 4 1406.62 300.364 12 0 8 4 999.386 293.568 14 1 7 4 702.109 294.793 14 2 6 4 7148.36 957.211 14 3 5 4 606.892 294.389 14 3 5 4 1070.25 393.326 12 -3 -5 -4 746.236 296.146 18 4 4 4 188.569 178.481 12 5 3 4 175.524 142.866 12 -1 8 4 3642.61 514.537 14 0 7 4 5975.85 844.842 14 -1 -6 -4 1859.43 432.002 18 1 6 4 1988.87 539.832 14 -2 -5 -4-101.231 169.707 18 2 5 4 196.461 209.282 14 3 4 4-373.523 238.700 14 -3 -4 -4 16.3079 87.0027 18 4 3 4 662.919 293.330 12 5 2 4 329.632 170.323 12 -2 8 4-92.6142 101.261 10 -1 7 4 3762.87 661.001 14 -1 7 4 4120.99 661.915 10 0 6 4 22290.5 1652.94 10 0 6 4 19970.6 1691.24 14 1 5 4 4644.94 826.173 14 -2 -4 -4 395.231 240.574 18 2 4 4 127.115 219.932 14 -3 -3 -4 883.726 359.989 18 4 2 4 162.837 172.636 12 5 1 4 1002.18 359.657 12 -2 7 4 113.155 125.769 14 -2 7 4 233.811 189.539 10 -1 6 4 3657.44 722.845 14 -1 6 4 4229.26 747.303 10 0 5 4 1899.25 531.635 14 0 5 4 2220.04 509.664 10 0 -5 -4 2124.33 940.584 1 -1 -4 -4 558.040 478.157 1 1 4 4 1200.27 404.798 14 2 3 4 6029.95 858.921 14 -2 -3 -4 4710.12 1315.18 1 -2 -3 -4 5601.86 846.195 18 -3 -2 -4 1681.98 810.649 1 -3 -2 -4 316.758 183.700 18 4 1 4 20637.1 1703.90 12 5 0 4 3980.99 663.436 12 -6 1 -4 134.143 73.9712 5 -3 7 4 9118.28 886.253 10 -2 6 4 693.969 295.152 14 -1 5 4 5031.23 835.112 14 1 -5 -4 7324.80 1648.37 20 -1 5 4 5289.97 836.036 10 0 4 4 6761.80 926.865 14 0 -4 -4 6523.34 1446.31 20 -1 -3 -4 356.758 349.751 1 -2 -2 -4 206.208 163.208 18 -2 -2 -4 40.0876 144.345 1 -3 -1 -4 1085.67 644.017 1 -3 -1 -4 474.250 261.351 18 4 0 4 3964.30 742.854 12 -5 1 -4 252.915 188.829 5 5 -1 4 217.853 165.866 12 -4 7 4 4619.53 487.560 10 -3 6 4 7321.22 867.694 14 -3 6 4 5885.16 839.042 11 2 -5 -4 3160.08 628.433 17 -2 5 4 2398.21 567.283 14 -2 5 4 2184.03 550.142 11 1 -4 -4 1710.41 448.447 17 -1 4 4 656.012 292.062 14 -1 4 4 1661.74 434.965 11 1 -4 -4 1503.64 690.360 20 0 -3 -4 4521.26 1030.25 2 0 -3 -4 5041.94 1112.53 20 -1 -2 -4 13263.9 1909.63 1 -2 -1 -4 7807.19 1504.88 1 -3 0 -4 1264.96 681.305 1 -3 0 -4 1558.80 445.952 18 4 -1 4 4048.11 744.789 12 -5 2 -4 92.7267 92.5224 5 5 -2 4 405.037 211.842 12 -4 6 4 1060.76 303.628 11 -3 5 4 639.791 286.078 14 -3 5 4 734.521 328.020 11 2 -4 -4 151593. 4401.72 17 -2 4 4 150120. 4240.42 11 2 -4 -4 160854. 7198.51 20 1 -3 -4 3657.23 932.552 2 1 -3 -4 2982.01 873.665 20 0 -2 -4 1407.23 607.112 2 0 -2 -4 2533.42 666.793 20 -1 -1 -4 6137.69 1225.28 1 -2 0 -4 35729.4 3170.29 1 -3 1 -4 7150.89 956.162 6 -3 1 -4 5514.18 1417.15 1 -3 1 -4 5837.45 853.166 18 -4 2 -4 748.338 319.524 6 4 -2 4 1138.27 388.487 12 -5 3 -4 790.776 278.397 5 -4 5 4 215.750 242.310 11 -3 4 4 182574. 4875.39 11 3 -4 -4 183273. 5028.25 17 2 -3 -4 110117. 5336.93 20 1 -2 -4 5119.66 1064.61 2 1 -2 -4 6011.45 1052.54 20 0 -1 -4 48345.4 3285.07 1 0 -1 -4 47911.3 3113.22 2 -1 0 -4 3293.56 890.182 1 -2 1 -4 23339.1 2599.55 1 -3 2 -4 15728.6 1459.99 6 -3 2 -4 14839.9 2381.19 1 -4 3 -4 734.024 300.731 6 -4 3 -4 631.600 299.094 5 -5 4 -4 135.520 109.304 4 -5 4 -4 428.384 194.935 6 -5 4 -4 182.456 135.501 5 -5 5 4 33.7648 89.0784 11 4 -4 -4 818.930 324.226 17 -4 4 4 867.340 386.769 11 3 -3 -4 1789.85 471.724 16 3 -3 -4 1431.43 665.636 21 3 -3 -4 1439.06 458.168 13 2 -2 -4 1075.24 524.557 21 2 -2 -4 636.833 359.865 20 1 -1 -4 74644.7 2933.20 20 0 0 -4 14806.2 1709.04 2 0 0 -4 14321.0 1572.00 1 -1 1 -4 274117. 7550.31 1 -2 2 -4 851566. 15881.2 1 -3 3 -4 15534.4 1494.71 6 -3 3 -4 14640.9 2420.82 1 -4 4 -4 31.9785 111.005 6 -4 4 -4 120.088 140.041 5 -5 5 -4 193.696 125.655 4 -5 5 -4-12.4532 75.7618 6 5 -4 -4 508.345 215.766 17 -5 4 4 283.260 212.033 11 4 -3 -4-152.578 157.623 16 4 -3 -4-200.412 183.847 13 -4 3 4 12.2652 87.2887 4 3 -2 -4 7624.89 955.775 16 3 -2 -4 8623.46 1035.35 13 3 -2 -4 8318.60 1597.14 21 2 -1 -4 10942.6 1604.94 21 1 0 -4 177.295 197.673 1 1 0 -4 25.5608 148.901 21 0 1 -4 25168.7 2128.14 2 0 1 -4 26882.3 1986.76 1 -1 2 -4 155439. 5754.78 1 -2 3 -4 465.325 287.660 1 -3 4 -4 3709.68 1223.09 1 -3 4 -4 3979.25 784.585 6 3 -4 4 4157.87 1252.42 22 -3 4 -4 3833.79 667.511 5 -4 5 -4 938.461 339.340 4 -4 5 -4 798.839 334.784 6 -5 6 -4 434.092 161.329 6 5 -3 -4 5787.08 816.360 13 4 -2 -4 380.070 177.391 16 4 -2 -4 843.263 354.892 13 3 -1 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437.410 17 1 -3 -5 1331.53 632.344 2 1 -3 -5 1470.77 432.642 19 0 -2 -5-115.956 215.611 1 0 -2 -5 275.673 293.499 2 -1 -1 -5 21388.7 2571.41 1 -2 0 -5 10751.1 1927.13 1 -2 0 -5 10743.6 1131.98 18 -3 1 -5 467.969 579.602 1 -3 1 -5-472.585 276.811 6 -3 1 -5 251.296 193.223 18 -4 2 -5-82.7418 137.799 6 -5 3 -5 1024.12 284.156 5 -4 5 5 216.479 143.337 14 3 -4 -5 18790.4 1602.27 17 2 -3 -5 67522.6 3029.83 17 2 -3 -5 73530.8 4921.05 2 1 -2 -5 2392.31 860.830 2 0 -1 -5 3399.29 958.983 2 0 -1 -5 4854.73 1155.82 1 -1 0 -5 1784.76 669.080 1 -2 1 -5 210.394 286.017 1 -3 2 -5 12072.2 1334.10 6 -3 2 -5 13349.6 2342.83 1 -4 3 -5 482.738 283.066 6 -4 3 -5 402.711 223.932 5 -5 4 -5 1864.17 335.041 6 4 -4 -5 9056.76 1031.50 17 3 -3 -5 3157.64 670.525 17 2 -2 -5 1484.00 433.872 17 1 -1 -5 8439.88 1502.55 1 1 -1 -5 7332.86 1414.93 2 0 0 -5 9738.48 1605.27 2 0 0 -5 9376.91 1487.80 1 -1 1 -5 2712.63 860.569 1 -2 2 -5 31700.8 3303.26 1 -3 3 -5 9311.50 1181.54 6 -3 3 -5 10139.1 2074.27 1 -4 4 -5-184.648 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-1 -9-2.92587 96.5056 18 -2 0 -9 855.661 271.677 6 -2 3 9 368.785 151.512 14 -1 2 9 1821.01 383.775 14 0 -1 -9 1470.73 389.733 18 -1 0 -9 180.436 178.196 18 -2 1 -9 249.786 216.120 6 -3 2 -9-96.1759 99.4533 6 -2 2 9 1168.80 314.844 14 -1 1 9 973.237 304.459 14 1 -1 -9 666.821 272.830 19 0 0 -9 565.798 237.657 18 0 0 -9 857.765 355.334 19 -1 1 -9 451.436 280.211 6 -2 2 -9 77.1799 138.628 6 -3 3 -9 172.686 116.697 6 -3 2 9 2431.43 411.070 14 -2 1 9-117.355 144.127 14 2 -1 -9 297.526 181.053 19 1 0 -9 840.916 330.538 19 0 1 -9 156.820 173.842 19 -1 2 -9 2648.50 594.461 6 -2 3 -9 207.145 214.127 6 -3 4 -9-20.2775 64.8551 6 3 -1 -9 248.883 103.676 19 2 0 -9 2756.16 574.221 19 1 1 -9 16.6191 112.614 19 0 2 -9 5305.67 869.245 6 0 2 -9 7781.63 977.432 19 -1 3 -9 5307.42 822.529 6 -2 4 -9 253.882 164.450 6 -4 1 9 888.113 215.749 14 3 0 -9 626.767 249.814 19 2 1 -9 265.168 95.2647 19 1 2 -9 572.884 281.835 19 0 3 -9 263.991 204.385 6 0 3 -9 347.986 160.781 19 -1 4 -9 10.1136 86.1753 6 -2 5 -9 281.773 139.453 7 -2 5 -9 295.778 153.159 6 3 1 -9 271.801 191.161 19 2 2 -9 443.197 277.798 19 1 3 -9 460.299 221.509 19 0 4 -9 737.302 279.785 19 -1 5 -9-251.431 171.198 6 -2 6 -9 752.011 230.532 7 -2 6 -9 660.900 205.795 6 4 1 -9-128.392 97.7656 19 3 2 -9 1671.14 453.923 19 2 3 -9 4422.81 756.860 19 1 4 -9 427.127 202.971 7 1 4 -9 989.936 341.462 19 0 5 -9 368.337 218.596 7 -1 6 -9 110.307 145.925 7 4 2 -9 727.706 231.099 19 3 3 -9-84.1533 135.641 19 2 4 -9 7133.48 933.032 19 1 5 -9 17571.5 1342.06 7 1 5 -9 19183.2 1421.83 19 0 6 -9 296.029 173.844 7 -1 7 -9 6.31321 100.287 7 4 3 -9 855.154 257.026 19 3 4 -9 1462.85 422.797 19 2 5 -9 52098.1 2400.38 19 1 6 -9 9462.29 957.135 7 1 6 -9 10951.6 950.792 19 0 7 -9 37.4205 140.501 7 4 4 -9 2159.67 395.167 19 3 5 -9 311.338 209.690 19 2 6 -9-261.533 165.817 19 1 7 -9 266.084 158.427 7 4 5 -9 103.641 63.6815 19 3 6 -9 2.07662 89.8659 19 2 7 -9 624.722 210.911 19 3 7 -9 427.979 150.743 19 0 -1 -10 8914.96 709.341 6 -1 0 -10 1995.77 335.361 6 0 0 -10 350.180 151.578 6 -1 1 -10 85.6360 90.1875 6 1 0 -10 337.330 172.807 19 0 1 -10 252.486 141.999 6 -1 2 -10 161.196 128.130 6 2 0 -10 1761.96 363.341 19 1 1 -10-19.8874 105.488 19 0 2 -10-3.70846 75.8724 6 0 2 -10 54.9771 91.9223 19 -1 3 -10-98.1900 110.137 6 2 1 -10 5303.89 685.821 19 1 2 -10 1522.14 398.224 19 0 3 -10-223.254 136.384 19 -1 4 -10 139.871 106.944 6 3 1 -10 4013.94 502.291 19 2 2 -10 7753.42 865.165 19 1 3 -10 62.9605 102.251 19 0 4 -10 172.590 138.982 7 -1 5 -10-132.147 113.000 7 3 2 -10 1005.52 270.462 19 2 3 -10 993.569 319.872 19 1 4 -10 27.3898 80.8373 19 0 5 -10 703.798 249.129 7 -1 6 -10 114.137 88.7450 7 3 3 -10-84.3095 76.7230 19 2 4 -10 22.4037 86.8538 19 1 5 -10 1635.01 318.149 7 1 5 -10 2022.10 359.275 19 0 6 -10 209.986 145.212 7 3 4 -10 44.2386 76.2955 19 2 5 -10 552.979 217.033 19 3 5 -10 142.724 120.192 19 2 6 -10 448.163 150.225 19 0 0 0 0.00 0.00 0 TITL e2879 Kam in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 5.558663 8.667318 8.764931 105.6536 98.5600 90.7838 ZERR 4.00 0.000889 0.001265 0.001211 0.0124 0.0128 0.0127 LATT 1 SFAC C H N O UNIT 44.00 40.00 4.00 4.00 TREF HKLF 4 END ; _shelx_hkl_checksum 41873 _shelx_res_file ; e2879.res created by SHELXL-2014/7 TITL shelxt_a.res in P-1 CELL 1.54184 5.558663 8.667318 8.764931 105.6536 98.56 90.7838 ZERR 2 0.000889 0.001265 0.001211 0.0124 0.0128 0.0127 LATT 1 SFAC C H N O UNIT 16 10 6 6 ACTA L.S. 10 PLAN 20 BOND $H LIST 6 MORE -1 CONF fmap 2 WGHT 0.061500 EXTI 0.011799 FVAR 20.58253 O1 4 0.635279 0.190864 0.527775 11.00000 0.07308 0.04521 = 0.07360 0.00137 0.03516 0.00194 O2 4 0.732763 0.941980 0.852498 11.00000 0.12725 0.04169 = 0.12299 -0.00145 0.05248 -0.01645 O3 4 0.893456 0.776309 0.671664 11.00000 0.07295 0.06181 = 0.09181 0.02150 0.02866 -0.00498 N1 3 0.130479 0.318300 0.827939 11.00000 0.06053 0.04895 = 0.06805 0.01024 0.02597 -0.00040 C2 1 0.160066 0.173564 0.748231 11.00000 0.06212 0.04574 = 0.06905 0.01257 0.02126 -0.00308 AFIX 43 H2 2 0.057593 0.092868 0.759250 11.00000 -1.20000 AFIX 0 N3 3 0.327671 0.128724 0.649680 11.00000 0.06739 0.03684 = 0.06462 0.00578 0.02259 0.00042 C4 1 0.488060 0.234289 0.620915 11.00000 0.05531 0.04310 = 0.05571 0.00731 0.01689 0.00353 C4A 1 0.464540 0.401196 0.709435 11.00000 0.05343 0.03985 = 0.04858 0.00821 0.01287 0.00301 C5 1 0.619728 0.522761 0.695542 11.00000 0.05494 0.04778 = 0.05416 0.01220 0.01540 0.00422 AFIX 43 H5 2 0.739879 0.499767 0.630644 11.00000 -1.20000 AFIX 0 C6 1 0.589655 0.677509 0.780666 11.00000 0.05709 0.04298 = 0.05792 0.01184 0.01111 -0.00129 C7 1 0.411991 0.716224 0.879614 11.00000 0.06743 0.03964 = 0.06002 0.00519 0.01427 0.00674 AFIX 43 H7 2 0.395648 0.822406 0.934929 11.00000 -1.20000 AFIX 0 C8 1 0.262622 0.596779 0.894357 11.00000 0.06170 0.04638 = 0.06056 0.00608 0.02107 0.00696 AFIX 43 H8 2 0.144581 0.621383 0.960725 11.00000 -1.20000 AFIX 0 C8A 1 0.286555 0.435854 0.809199 11.00000 0.05345 0.04362 = 0.05421 0.00923 0.01353 0.00270 N9 3 0.750421 0.807122 0.767773 11.00000 0.06938 0.04533 = 0.07444 0.01379 0.01330 -0.00431 H3 2 0.333925 0.037549 0.598102 11.00000 0.05746 HKLF 4 REM shelxt_a.res in P-1 REM R1 = 0.0469 for 1124 Fo > 4sig(Fo) and 0.0645 for all 1598 data REM 132 parameters refined using 0 restraints END WGHT 0.0631 0.0000 REM Highest difference peak 0.181, deepest hole -0.173, 1-sigma level 0.042 Q1 1 0.4815 0.3301 0.6836 11.00000 0.05 0.18 Q2 1 0.2809 0.4996 0.8372 11.00000 0.05 0.18 Q3 1 0.5344 0.4407 0.7173 11.00000 0.05 0.15 Q4 1 0.5397 0.6782 0.8003 11.00000 0.05 0.15 Q5 1 0.1985 0.3766 0.8225 11.00000 0.05 0.14 Q6 1 0.8080 1.0391 0.8610 11.00000 0.05 0.13 Q7 1 0.0443 0.4047 0.9450 11.00000 0.05 0.13 Q8 1 1.0016 0.8658 0.6642 11.00000 0.05 0.13 Q9 1 0.3104 0.8872 1.0361 11.00000 0.05 0.12 Q10 1 0.8910 0.6532 0.6225 11.00000 0.05 0.11 Q11 1 0.6580 0.0855 0.4751 11.00000 0.05 0.11 Q12 1 -0.0706 -0.0015 0.7994 11.00000 0.05 0.11 Q13 1 0.4797 0.4185 0.9589 11.00000 0.05 0.10 Q14 1 -0.1170 0.1113 0.8654 11.00000 0.05 0.10 Q15 1 0.0000 0.5000 1.0000 10.50000 0.05 0.10 Q16 1 0.5000 0.0000 0.5000 10.50000 0.05 0.10 Q17 1 1.1068 0.8993 0.6573 11.00000 0.05 0.10 Q18 1 0.7776 0.3845 0.5438 11.00000 0.05 0.10 Q19 1 0.6332 0.5628 0.9372 11.00000 0.05 0.10 Q20 1 0.2613 0.4041 0.5574 11.00000 0.05 0.10 ; _shelx_res_checksum 39932 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.6353(3) 0.19086(17) 0.52777(19) 0.0644(5) Uani d 1 . . O O2 0.7328(5) 0.9420(2) 0.8525(3) 0.0988(8) Uani d 1 . . O O3 0.8935(3) 0.7763(2) 0.6717(2) 0.0739(5) Uani d 1 . . N N1 0.1305(3) 0.3183(2) 0.8279(2) 0.0587(5) Uani d 1 . . C C2 0.1601(4) 0.1736(3) 0.7482(3) 0.0585(5) Uani d 1 . . H H2 0.0576 0.0929 0.7592 0.070 Uiso calc 1 . . N N3 0.3277(4) 0.1287(2) 0.6497(2) 0.0566(5) Uani d 1 . . C C4 0.4881(4) 0.2343(2) 0.6209(2) 0.0517(5) Uani d 1 . . C C4A 0.4645(4) 0.4012(2) 0.7094(2) 0.0476(5) Uani d 1 . . C C5 0.6197(4) 0.5228(2) 0.6955(3) 0.0519(5) Uani d 1 . . H H5 0.7399 0.4998 0.6306 0.062 Uiso calc 1 . . C C6 0.5897(4) 0.6775(2) 0.7807(3) 0.0529(5) Uani d 1 . . C C7 0.4120(4) 0.7162(2) 0.8796(3) 0.0569(5) Uani d 1 . . H H7 0.3956 0.8224 0.9349 0.068 Uiso calc 1 . . C C8 0.2626(4) 0.5968(2) 0.8944(3) 0.0567(5) Uani d 1 . . H H8 0.1446 0.6214 0.9607 0.068 Uiso calc 1 . . C C8A 0.2866(4) 0.4359(2) 0.8092(2) 0.0507(5) Uani d 1 . . N N9 0.7504(4) 0.8071(2) 0.7678(3) 0.0635(5) Uani d 1 . . H H3 0.334(5) 0.038(3) 0.598(3) 0.057(6) Uiso d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0731(10) 0.0452(8) 0.0736(11) 0.0019(7) 0.0352(9) 0.0014(7) O2 0.1272(18) 0.0417(9) 0.1230(17) -0.0165(10) 0.0525(15) -0.0014(9) O3 0.0730(11) 0.0618(10) 0.0918(13) -0.0050(8) 0.0287(10) 0.0215(9) N1 0.0605(10) 0.0490(9) 0.0681(11) -0.0004(7) 0.0260(9) 0.0102(8) C2 0.0621(12) 0.0457(11) 0.0690(14) -0.0031(9) 0.0213(11) 0.0126(9) N3 0.0674(11) 0.0368(8) 0.0646(11) 0.0004(7) 0.0226(9) 0.0058(8) C4 0.0553(11) 0.0431(10) 0.0557(11) 0.0035(8) 0.0169(9) 0.0073(8) C4A 0.0534(10) 0.0398(9) 0.0486(10) 0.0030(8) 0.0129(8) 0.0082(8) C5 0.0549(11) 0.0478(11) 0.0542(11) 0.0042(8) 0.0154(9) 0.0122(8) C6 0.0571(11) 0.0430(10) 0.0579(11) -0.0013(8) 0.0111(9) 0.0118(8) C7 0.0674(13) 0.0396(10) 0.0600(12) 0.0067(9) 0.0143(10) 0.0052(8) C8 0.0617(12) 0.0464(11) 0.0606(12) 0.0070(9) 0.0211(10) 0.0061(9) C8A 0.0535(11) 0.0436(10) 0.0542(11) 0.0027(8) 0.0135(9) 0.0092(8) N9 0.0694(12) 0.0453(10) 0.0744(12) -0.0043(8) 0.0133(10) 0.0138(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 N1 C8A . . 115.80(17) ? N1 C2 N3 . . 125.57(19) ? N1 C2 H2 . . 117.2 ? N3 C2 H2 . . 117.2 ? C2 N3 C4 . . 123.57(17) ? C2 N3 H3 . . 122.0(18) ? C4 N3 H3 . . 114.3(18) ? O1 C4 N3 . . 122.34(17) ? O1 C4 C4A . . 124.23(18) ? N3 C4 C4A . . 113.43(16) ? C5 C4A C8A . . 120.89(18) ? C5 C4A C4 . . 120.21(17) ? C8A C4A C4 . . 118.90(18) ? C6 C5 C4A . . 117.95(18) ? C6 C5 H5 . . 121.0 ? C4A C5 H5 . . 121.0 ? C5 C6 C7 . . 122.54(19) ? C5 C6 N9 . . 118.89(18) ? C7 C6 N9 . . 118.57(18) ? C8 C7 C6 . . 119.31(18) ? C8 C7 H7 . . 120.3 ? C6 C7 H7 . . 120.3 ? C7 C8 C8A . . 120.21(19) ? C7 C8 H8 . . 119.9 ? C8A C8 H8 . . 119.9 ? N1 C8A C4A . . 122.73(18) ? N1 C8A C8 . . 118.18(18) ? C4A C8A C8 . . 119.09(19) ? O2 N9 O3 . . 122.9(2) ? O2 N9 C6 . . 118.0(2) ? O3 N9 C6 . . 119.03(18) ? 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 C4 . 1.233(2) ? O2 N9 . 1.218(2) ? O3 N9 . 1.223(2) ? N1 C2 . 1.287(3) y N1 C8A . 1.388(3) ? C2 N3 . 1.354(3) y C2 H2 . 0.9300 ? N3 C4 . 1.366(3) y N3 H3 . 0.80(3) ? C4 C4A . 1.463(3) ? C4A C5 . 1.395(3) ? C4A C8A . 1.399(3) ? C5 C6 . 1.374(3) ? C5 H5 . 0.9300 ? C6 C7 . 1.395(3) ? C6 N9 . 1.464(3) y C7 C8 . 1.363(3) ? C7 H7 . 0.9300 ? C8 C8A . 1.412(3) ? C8 H8 . 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 N3 H3 O1 2_656 0.80(3) 2.02(3) 2.814(2) 178(4) y C8 H8 N1 2_567 0.93 2.53 3.450(3) 172 y C2 H2 O2 1_445 0.93 2.57 3.466(4) 163 y C7 H7 O2 2_677 0.93 2.56 3.437(3) 158 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 C8A N1 C2 N3 . . . . -0.1(4) ? N1 C2 N3 C4 . . . . -0.7(4) ? C2 N3 C4 O1 . . . . -178.3(2) ? C2 N3 C4 C4A . . . . 1.0(3) ? O1 C4 C4A C5 . . . . -2.2(3) ? N3 C4 C4A C5 . . . . 178.5(2) ? O1 C4 C4A C8A . . . . 178.6(2) ? N3 C4 C4A C8A . . . . -0.7(3) ? C8A C4A C5 C6 . . . . -1.0(3) ? C4 C4A C5 C6 . . . . 179.8(2) ? C4A C5 C6 C7 . . . . 0.3(3) ? C4A C5 C6 N9 . . . . -179.9(2) ? C5 C6 C7 C8 . . . . 0.5(4) ? N9 C6 C7 C8 . . . . -179.3(2) ? C6 C7 C8 C8A . . . . -0.5(4) ? C2 N1 C8A C4A . . . . 0.5(3) ? C2 N1 C8A C8 . . . . -179.8(2) ? C5 C4A C8A N1 . . . . -179.2(2) ? C4 C4A C8A N1 . . . . 0.0(3) ? C5 C4A C8A C8 . . . . 1.1(3) ? C4 C4A C8A C8 . . . . -179.8(2) ? C7 C8 C8A N1 . . . . 180.0(2) ? C7 C8 C8A C4A . . . . -0.2(3) ? C5 C6 N9 O2 . . . . -175.0(2) ? C7 C6 N9 O2 . . . . 4.9(4) ? C5 C6 N9 O3 . . . . 6.0(3) ? C7 C6 N9 O3 . . . . -174.2(2) ? _cod_database_fobs_code 2243909