#------------------------------------------------------------------------------ #$Date: 2016-04-02 23:02:54 +0300 (Sat, 02 Apr 2016) $ #$Revision: 180910 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/10/51/2105194.hkl $ #------------------------------------------------------------------------------ # # 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_2105194_Fobs loop_ _publ_author_name 'Siegler, Maxime A.' 'Parkin, Sean' 'Brock, Carolyn Pratt' _publ_section_title ; [Ni(MeCN)(H~2~O)~2~(NO~3~)~2~]·(15-crown-5)·MeCN: detailed study of a four-phase sequence that includes an intermediate modulated phase ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 389 _journal_page_last 400 _journal_volume 68 _journal_year 2012 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _cell_angle_alpha 90.000 _cell_angle_beta 105.410 _cell_angle_gamma 90.000 _cell_length_a 12.1720 _cell_length_b 12.2570 _cell_length_c 16.1900 _exptl_crystal_F_000 1096.00 _reflns_d_resolution_high 0.7702 _cod_data_source_file hw5021218K_III_2sup24.hkl _cod_data_source_block 218K_III_2 #BEGIN Tags that were not found in dictionaries: _shelx_title ' k06109 in P2(1)/c' _shelx_refln_list_code 4 _shelx_f_calc_maximum 293.83 _shelx_f_squared_multiplier 1.000 #END Tags that were not found in dictionaries loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_observed_status 1 0 0 6122.78 5801.64 85.29 o 2 0 0 25310.07 25605.00 399.40 o 3 0 0 700.14 836.23 14.56 o 4 0 0 1351.03 1121.22 20.80 o 5 0 0 40079.27 44002.15 619.90 o 6 0 0 1627.12 2055.22 39.52 o 7 0 0 8671.50 8668.13 176.82 o 8 0 0 6668.17 6587.95 164.33 o 9 0 0 437.37 488.84 33.28 o 10 0 0 417.55 357.79 29.12 o 11 0 0 961.29 900.72 49.92 o 12 0 0 1326.02 1487.33 89.45 o 13 0 0 934.85 990.17 66.57 o 14 0 0 21.80 20.80 29.12 o 15 0 0 183.43 139.37 81.13 o 1 1 0 45834.66 45913.88 1206.03 o 2 1 0 1155.70 1269.11 15.39 o 3 1 0 9410.84 8643.89 99.08 o 4 1 0 16948.61 17535.57 186.18 o 5 1 0 1244.12 1097.72 13.92 o 6 1 0 12005.39 12441.68 129.95 o 7 1 0 2485.18 2520.70 33.45 o 8 1 0 110.13 116.42 13.52 o 9 1 0 731.71 760.78 19.52 o 10 1 0 179.11 194.44 31.20 o 11 1 0 2482.97 2728.23 73.55 o 12 1 0 1088.25 1192.49 45.31 o 13 1 0 142.52 141.89 23.97 o 14 1 0 175.59 103.09 31.39 o 15 1 0 2.60 53.81 32.98 o 0 2 0 12494.28 11810.36 215.85 o 1 2 0 1055.96 1134.74 14.71 o 2 2 0 3063.30 3266.78 40.43 o 3 2 0 9425.45 8868.01 100.69 o 4 2 0 645.15 816.20 24.96 o 5 2 0 18381.41 19365.38 207.88 o 6 2 0 43.18 28.43 4.41 o 7 2 0 4561.67 4848.71 65.47 o 8 2 0 3417.72 3715.32 49.25 o 9 2 0 927.21 984.11 50.96 o 10 2 0 2481.77 2795.06 67.23 o 11 2 0 2.18 14.56 16.64 o 12 2 0 703.14 737.18 37.49 o 13 2 0 308.78 345.69 32.26 o 14 2 0 16.11 -17.89 25.46 o 15 2 0 339.98 314.81 59.41 o 1 3 0 5073.74 5320.44 62.50 o 2 3 0 5096.09 5419.92 74.89 o 3 3 0 8691.08 9052.91 107.10 o 4 3 0 17487.73 17745.85 194.69 o 5 3 0 1341.03 1022.46 14.71 o 6 3 0 962.92 976.45 14.49 o 7 3 0 860.80 937.16 17.47 o 8 3 0 1173.84 1302.30 73.85 o 9 3 0 3244.55 3486.91 52.47 o 10 3 0 557.42 506.01 28.08 o 11 3 0 1877.54 2062.92 61.03 o 12 3 0 51.11 50.28 20.99 o 13 3 0 1.25 12.97 21.48 o 14 3 0 249.69 286.98 47.33 o 0 4 0 44256.90 44636.50 934.95 o 1 4 0 2169.72 2337.26 27.49 o 2 4 0 12766.33 13006.85 150.03 o 3 4 0 8337.24 8347.07 91.85 o 4 4 0 770.47 611.05 17.68 o 5 4 0 9606.34 10259.74 118.90 o 6 4 0 848.99 814.40 14.71 o 7 4 0 3412.96 3563.93 50.73 o 8 4 0 3133.30 3305.76 50.35 o 9 4 0 76.09 57.45 13.52 o 10 4 0 2250.38 2572.90 66.91 o 11 4 0 107.92 103.13 19.97 o 12 4 0 129.09 103.55 22.99 o 13 4 0 94.26 59.85 40.56 o 14 4 0 7.87 20.04 41.60 o 1 5 0 12327.06 12143.08 135.23 o 2 5 0 10585.63 12337.16 141.80 o 3 5 0 8617.71 8677.95 98.52 o 4 5 0 6923.09 7473.97 88.22 o 5 5 0 4.93 8.32 6.24 o 6 5 0 4018.45 4124.68 54.36 o 7 5 0 42.71 47.57 7.99 o 8 5 0 24.30 14.94 7.99 o 9 5 0 1305.56 1381.30 30.39 o 10 5 0 291.77 226.96 40.56 o 11 5 0 997.12 1241.63 48.27 o 12 5 0 27.28 40.56 26.14 o 13 5 0 24.87 27.20 50.96 o 14 5 0 377.45 382.73 55.39 o 0 6 0 18558.49 19091.14 294.33 o 1 6 0 78.14 92.58 5.88 o 2 6 0 9805.24 10276.27 121.02 o 3 6 0 414.08 473.43 10.30 o 4 6 0 423.48 423.46 13.52 o 5 6 0 5204.23 5395.28 71.06 o 6 6 0 28.76 22.62 6.50 o 7 6 0 2280.40 2254.53 37.31 o 8 6 0 238.68 222.59 12.99 o 9 6 0 46.55 30.94 11.49 o 10 6 0 1437.94 1631.25 48.27 o 11 6 0 95.75 64.21 28.09 o 12 6 0 255.23 187.42 36.12 o 13 6 0 198.86 167.22 39.25 o 14 6 0 7.42 32.93 41.96 o 1 7 0 1988.33 1947.38 27.83 o 2 7 0 443.62 531.51 13.24 o 3 7 0 1097.62 1066.71 19.82 o 4 7 0 1300.47 1296.90 23.92 o 5 7 0 6.79 2.38 3.86 o 6 7 0 2681.84 2858.32 45.48 o 7 7 0 394.22 479.25 13.85 o 8 7 0 47.26 27.04 12.48 o 9 7 0 366.64 274.36 20.44 o 10 7 0 63.62 70.87 20.39 o 11 7 0 700.92 706.49 46.28 o 12 7 0 139.66 108.55 36.12 o 13 7 0 6.23 -39.52 39.52 o 0 8 0 2940.21 3239.58 66.86 o 1 8 0 443.18 347.94 20.80 o 2 8 0 34.31 35.70 13.52 o 3 8 0 998.30 949.86 21.29 o 4 8 0 71.66 79.28 7.99 o 5 8 0 4309.26 4744.97 118.57 o 6 8 0 537.03 591.84 36.40 o 7 8 0 178.65 168.11 15.39 o 8 8 0 315.02 316.76 20.44 o 9 8 0 13.50 21.56 15.98 o 10 8 0 519.96 563.29 32.26 o 11 8 0 35.93 73.21 28.08 o 12 8 0 25.85 27.86 52.00 o 13 8 0 83.65 8.32 53.04 o 1 9 0 875.52 780.93 38.48 o 2 9 0 1308.36 1317.54 45.76 o 3 9 0 82.04 84.82 9.48 o 4 9 0 172.74 140.20 10.38 o 5 9 0 230.06 277.71 17.65 o 6 9 0 524.49 568.93 25.71 o 7 9 0 995.86 1057.49 34.48 o 8 9 0 127.15 93.10 16.49 o 9 9 0 149.11 145.80 22.76 o 10 9 0 14.40 12.02 19.49 o 11 9 0 78.56 55.40 26.92 o 12 9 0 81.22 49.30 40.63 o 0 10 0 6785.41 7005.42 190.47 o 1 10 0 44.36 47.22 15.60 o 2 10 0 88.86 55.14 10.30 o 3 10 0 557.21 671.62 35.36 o 4 10 0 1.97 10.16 13.52 o 5 10 0 232.97 196.95 17.65 o 6 10 0 58.07 73.52 16.87 o 7 10 0 36.32 14.89 13.92 o 8 10 0 190.63 121.49 20.99 o 9 10 0 0.11 12.02 19.49 o 10 10 0 51.19 39.87 25.39 o 11 10 0 30.95 23.50 42.64 o 1 11 0 508.33 523.45 44.72 o 2 11 0 30.73 30.74 12.99 o 3 11 0 8.55 43.98 15.60 o 4 11 0 95.57 33.88 15.39 o 5 11 0 22.80 -8.89 15.98 o 6 11 0 293.02 262.25 24.88 o 7 11 0 146.16 132.03 21.29 o 8 11 0 1.65 -4.83 21.92 o 9 11 0 12.65 -16.64 22.06 o 10 11 0 0.08 16.74 41.60 o 11 11 0 46.30 11.08 38.16 o 0 12 0 20.32 16.87 19.82 o 1 12 0 8.78 7.28 14.71 o 2 12 0 2.86 5.06 16.49 o 3 12 0 518.01 463.90 28.98 o 4 12 0 14.58 34.20 18.34 o 5 12 0 621.79 667.24 39.86 o 6 12 0 1.00 32.85 28.08 o 7 12 0 0.53 57.83 24.23 o 8 12 0 0.56 13.61 23.92 o 9 12 0 1.46 2.08 33.83 o 10 12 0 46.49 57.32 42.72 o 1 13 0 6.60 -0.46 19.49 o 2 13 0 168.49 169.01 33.43 o 3 13 0 36.33 -5.78 19.49 o 4 13 0 238.41 186.84 58.25 o 5 13 0 2.37 3.40 24.53 o 6 13 0 32.47 49.01 29.60 o 7 13 0 5.46 6.79 25.16 o 8 13 0 0.73 -3.50 29.93 o 0 14 0 4.58 12.48 68.65 o 1 14 0 2.70 24.96 54.08 o 2 14 0 0.49 58.25 49.92 o 3 14 0 6.55 22.88 33.28 o 4 14 0 23.78 52.00 35.36 o 5 14 0 6.72 -14.56 37.44 o 6 14 0 0.27 31.20 37.44 o 7 14 0 4.08 2.08 35.36 o 1 15 0 2.12 2.08 45.76 o 2 15 0 0.10 -52.00 52.00 o 3 15 0 0.90 47.84 49.92 o 4 15 0 9.15 -20.80 58.25 o 5 15 0 0.41 -45.76 45.76 o -15 1 1 0.02 7.31 34.66 o -14 1 1 33.54 3.47 54.08 o -13 1 1 0.81 -20.59 20.59 o -12 1 1 32.74 15.10 16.87 o -11 1 1 89.14 48.03 16.87 o -10 1 1 16.93 11.33 12.99 o -9 1 1 898.05 886.14 27.83 o -8 1 1 224.55 230.50 12.48 o -7 1 1 1046.54 1104.98 34.32 o -6 1 1 5.15 10.82 3.46 o -5 1 1 744.67 746.84 11.77 o -4 1 1 53.31 46.83 2.94 o -3 1 1 14.85 22.29 3.12 o -2 1 1 4.96 6.54 2.08 o -1 1 1 10.54 11.54 1.47 o 0 1 1 22.87 24.96 1.47 o 1 1 1 2.16 6.24 1.47 o 2 1 1 101.07 97.95 4.16 o 3 1 1 183.86 156.04 4.41 o 4 1 1 608.86 631.34 10.30 o 5 1 1 101.57 93.61 4.99 o 6 1 1 1695.16 1714.35 22.76 o 7 1 1 104.39 96.19 6.50 o 8 1 1 388.93 367.29 10.96 o 9 1 1 0.88 1.04 12.48 o 10 1 1 5.02 -4.80 8.82 o 11 1 1 24.39 1.47 17.47 o 12 1 1 16.08 35.08 38.48 o 13 1 1 34.83 18.03 24.24 o 14 1 1 0.87 -24.91 28.65 o -15 2 1 26.59 30.87 34.66 o -14 2 1 0.75 -5.55 23.45 o -13 2 1 44.11 10.54 21.29 o -12 2 1 14.93 -4.32 18.45 o -11 2 1 74.47 45.76 14.71 o -10 2 1 368.49 384.87 32.24 o -9 2 1 25.32 21.15 10.40 o -8 2 1 461.43 486.97 15.39 o -7 2 1 2.23 11.59 4.99 o -6 2 1 1200.35 1027.81 15.39 o -5 2 1 57.66 65.34 3.46 o -4 2 1 209.16 206.02 4.41 o -3 2 1 204.97 192.47 4.41 o -2 2 1 8.22 23.64 4.16 o -1 2 1 549.30 454.27 6.50 o 0 2 1 214.47 189.85 4.16 o 1 2 1 858.10 798.79 10.96 o 2 2 1 244.51 264.67 8.32 o 3 2 1 159.88 119.62 4.41 o 4 2 1 300.34 336.13 6.50 o 5 2 1 41.81 32.04 8.32 o 6 2 1 186.35 144.35 6.50 o 7 2 1 635.24 610.18 18.72 o 8 2 1 7.57 3.86 4.99 o 9 2 1 28.32 28.11 5.58 o 10 2 1 3.43 2.34 10.70 o 11 2 1 1.98 -6.24 16.18 o 12 2 1 153.76 126.51 23.40 o 13 2 1 1.61 0.15 20.44 o 14 2 1 23.71 -0.13 35.21 o -15 3 1 11.82 -5.18 43.09 o -14 3 1 71.39 14.31 34.28 o -13 3 1 1.38 8.05 23.92 o -12 3 1 3.01 4.39 19.49 o -11 3 1 14.08 19.03 14.49 o -10 3 1 79.54 62.52 11.93 o -9 3 1 108.39 68.03 11.44 o -8 3 1 82.70 74.57 8.32 o -7 3 1 905.60 905.06 17.47 o -6 3 1 220.43 209.79 6.50 o -5 3 1 786.21 750.23 15.60 o -4 3 1 1200.09 1212.51 17.68 o -3 3 1 9.05 12.07 1.86 o -2 3 1 4028.15 3949.08 47.79 o -1 3 1 182.15 242.70 9.36 o 0 3 1 1715.47 1452.29 19.82 o 1 3 1 2286.87 2144.31 27.18 o 2 3 1 40.97 38.74 3.12 o 3 3 1 845.52 752.51 13.52 o 4 3 1 603.62 595.98 24.96 o 5 3 1 1.77 -5.20 7.28 o 6 3 1 85.14 84.49 6.50 o 7 3 1 42.50 40.27 6.50 o 8 3 1 83.63 65.17 9.36 o 9 3 1 5.15 -1.66 17.68 o 10 3 1 9.89 -1.70 7.22 o 11 3 1 72.52 51.73 39.52 o 12 3 1 19.52 -16.87 16.87 o 13 3 1 21.62 35.65 26.35 o 14 3 1 7.72 -33.28 33.28 o -14 4 1 11.78 21.86 33.98 o -13 4 1 131.12 166.48 67.61 o -12 4 1 0.07 4.95 20.99 o -11 4 1 36.80 22.50 24.96 o -10 4 1 13.67 1.04 10.30 o -9 4 1 109.71 107.47 13.52 o -8 4 1 12.01 16.87 6.50 o -7 4 1 739.88 723.33 30.16 o -6 4 1 1848.42 1671.95 38.48 o -5 4 1 1236.83 1231.38 39.52 o -4 4 1 1114.74 1189.71 17.47 o -3 4 1 148.75 147.72 5.88 o -2 4 1 133.55 119.84 5.20 o -1 4 1 1584.26 1315.01 20.80 o 0 4 1 1142.79 1010.97 14.71 o 1 4 1 526.53 487.99 7.99 o 2 4 1 66.35 76.05 4.41 o 3 4 1 51.39 53.07 4.41 o 4 4 1 522.32 472.79 16.64 o 5 4 1 1015.94 953.86 15.39 o 6 4 1 208.48 189.95 19.76 o 7 4 1 592.64 590.01 16.64 o 8 4 1 110.12 107.62 9.98 o 9 4 1 64.34 50.02 12.48 o 10 4 1 19.93 9.29 16.64 o 11 4 1 45.76 20.80 17.65 o 12 4 1 172.93 118.72 30.16 o 13 4 1 0.03 8.27 28.03 o 14 4 1 33.07 21.15 36.53 o -14 5 1 156.46 122.51 48.70 o -13 5 1 7.40 -32.63 32.63 o -12 5 1 181.03 124.40 29.24 o -11 5 1 49.32 48.95 21.92 o -10 5 1 585.40 596.63 24.88 o -9 5 1 516.73 480.19 17.47 o -8 5 1 45.23 42.44 6.50 o -7 5 1 651.85 613.74 13.92 o -6 5 1 965.43 961.25 17.47 o -5 5 1 198.61 184.57 9.36 o -4 5 1 830.80 824.90 14.71 o -3 5 1 25.23 22.79 5.20 o -2 5 1 3747.92 3624.83 64.49 o -1 5 1 2255.31 2240.71 27.18 o 0 5 1 925.74 991.78 13.92 o 1 5 1 3041.02 2818.93 33.74 o 2 5 1 86.27 71.32 10.40 o 3 5 1 2242.94 2088.32 28.08 o 4 5 1 1116.30 1062.09 36.40 o 5 5 1 775.64 751.00 16.18 o 6 5 1 1566.63 1637.92 26.35 o 7 5 1 149.85 117.70 9.48 o 8 5 1 609.17 588.71 18.95 o 9 5 1 113.12 139.78 12.99 o 10 5 1 114.14 134.51 15.60 o 11 5 1 277.67 292.06 25.71 o 12 5 1 1.23 -12.48 24.96 o 13 5 1 39.72 -6.54 33.84 o 14 5 1 0.09 2.16 36.90 o -14 6 1 22.10 43.13 35.48 o -13 6 1 226.58 157.50 38.88 o -12 6 1 114.83 71.79 34.32 o -11 6 1 444.11 405.51 36.82 o -10 6 1 1287.61 1248.40 51.28 o -9 6 1 440.16 415.42 19.49 o -8 6 1 546.31 527.19 15.60 o -7 6 1 111.04 91.20 7.99 o -6 6 1 318.66 292.59 7.44 o -5 6 1 1424.20 1387.35 41.60 o -4 6 1 63.55 66.33 7.35 o -3 6 1 2609.01 2692.40 31.60 o -2 6 1 662.10 690.16 12.44 o -1 6 1 1840.04 1882.85 26.00 o 0 6 1 2550.40 2412.98 40.56 o 1 6 1 459.91 488.18 13.52 o 2 6 1 5849.30 5987.02 67.61 o 3 6 1 74.97 62.68 5.88 o 4 6 1 4123.13 4249.23 58.78 o 5 6 1 135.96 116.09 7.99 o 6 6 1 178.21 188.38 9.48 o 7 6 1 1593.42 1563.39 31.96 o 8 6 1 279.13 252.30 14.98 o 9 6 1 725.13 706.75 27.18 o 10 6 1 275.12 224.82 18.95 o 11 6 1 251.60 244.58 32.32 o 12 6 1 203.86 165.01 37.46 o 13 6 1 4.13 -1.96 71.77 o -13 7 1 0.98 27.04 33.06 o -12 7 1 131.03 129.45 36.17 o -11 7 1 298.23 234.10 33.30 o -10 7 1 372.80 384.47 31.98 o -9 7 1 1612.46 1641.76 55.02 o -8 7 1 326.62 299.62 32.24 o -7 7 1 1577.39 1719.03 38.46 o -6 7 1 122.26 123.03 16.64 o -5 7 1 389.30 421.48 14.56 o -4 7 1 3102.76 3260.29 52.40 o -3 7 1 0.18 3.57 4.99 o -2 7 1 5002.18 5109.81 64.46 o -1 7 1 296.07 370.27 10.30 o 0 7 1 1326.49 1420.55 45.76 o 1 7 1 4127.26 4203.65 58.48 o 2 7 1 0.30 3.12 5.88 o 3 7 1 3753.47 3855.54 53.67 o 4 7 1 650.29 632.22 28.08 o 5 7 1 225.24 259.02 11.77 o 6 7 1 634.54 648.21 24.96 o 7 7 1 28.26 35.79 8.46 o 8 7 1 1039.07 1032.11 30.47 o 9 7 1 430.02 444.41 25.01 o 10 7 1 174.75 190.33 26.47 o 11 7 1 164.29 119.53 41.60 o 12 7 1 8.28 50.15 33.84 o 13 7 1 44.95 9.91 82.17 o -13 8 1 171.25 192.25 36.01 o -12 8 1 14.06 54.70 41.60 o -11 8 1 44.09 109.56 27.98 o -10 8 1 244.87 246.86 25.01 o -9 8 1 2.91 -11.23 14.49 o -8 8 1 436.23 561.93 59.29 o -7 8 1 9.17 4.16 13.52 o -6 8 1 999.12 1137.08 30.79 o -5 8 1 1876.87 1917.24 41.75 o -4 8 1 560.97 546.62 16.49 o -3 8 1 2290.96 2434.47 57.21 o -2 8 1 5.54 13.52 5.88 o -1 8 1 1390.66 1376.36 29.12 o 0 8 1 404.41 424.64 23.92 o 1 8 1 523.08 512.69 14.56 o 2 8 1 1811.98 1965.18 35.21 o 3 8 1 81.79 64.83 9.36 o 4 8 1 885.16 964.19 38.48 o 5 8 1 145.27 162.49 10.30 o 6 8 1 42.59 34.98 7.44 o 7 8 1 190.03 171.62 16.64 o 8 8 1 0.90 5.20 13.24 o 9 8 1 265.50 282.91 61.37 o 10 8 1 118.66 118.69 34.32 o 11 8 1 40.73 37.95 30.13 o 12 8 1 85.45 23.01 33.39 o -12 9 1 100.20 58.71 52.00 o -11 9 1 37.44 65.40 30.16 o -10 9 1 90.89 56.16 20.77 o -9 9 1 354.80 403.78 25.46 o -8 9 1 32.61 29.33 14.49 o -7 9 1 597.97 685.15 25.99 o -6 9 1 620.02 626.17 45.76 o -5 9 1 59.98 51.25 11.49 o -4 9 1 1207.04 1325.50 35.99 o -3 9 1 61.90 59.78 13.52 o -2 9 1 2381.01 2527.64 47.96 o -1 9 1 228.93 232.98 15.60 o 0 9 1 383.79 387.65 13.92 o 1 9 1 743.53 755.10 18.95 o 2 9 1 16.34 3.97 7.99 o 3 9 1 664.58 710.12 22.76 o 4 9 1 155.80 153.63 16.64 o 5 9 1 296.41 327.74 14.98 o 6 9 1 251.26 269.08 18.95 o 7 9 1 0.07 19.58 12.44 o 8 9 1 82.51 81.07 16.87 o 9 9 1 173.50 159.38 22.48 o 10 9 1 98.16 103.87 24.88 o 11 9 1 138.36 71.72 46.80 o 12 9 1 0.03 -36.97 36.97 o -12 10 1 29.30 -27.43 39.63 o -11 10 1 130.65 106.78 31.63 o 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