data_1542481 _cell_angle_alpha 72.994 _cell_angle_beta 86.500 _cell_angle_gamma 87.152 _cell_length_a 7.3066 _cell_length_b 7.9672 _cell_length_c 12.8467 _exptl_crystal_F_000 420.00 _reflns_d_resolution_high 0.7673 _cod_data_source_file wm4001Isup2.hkl _cod_data_source_block I _shelx_title ' PB2-3 NEEDLES SOTON DATA' _shelx_refln_list_code 4 _shelx_f_calc_maximum 219.68 _shelx_f_squared_multiplier 1.000 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 2 0 0 359.36 464.00 39.79 o 3 0 0 7074.64 6910.63 347.01 o 4 0 0 11549.49 12197.10 552.97 o 5 0 0 4208.20 3828.94 253.10 o 6 0 0 26.06 -11.69 19.50 o 7 0 0 536.57 463.33 62.70 o 8 0 0 4177.82 4789.27 183.62 o 9 0 0 888.40 1089.81 191.55 o -9 1 0 3.42 -28.37 72.80 o -8 1 0 485.01 478.93 65.01 o -7 1 0 431.40 439.72 57.19 o -6 1 0 212.14 204.11 35.06 o -5 1 0 138.63 155.50 28.50 o -4 1 0 348.47 341.95 25.20 o -3 1 0 1094.73 902.62 56.15 o -2 1 0 2094.41 2072.17 74.89 o -1 1 0 268.38 294.43 15.62 o 1 1 0 2944.62 2600.88 65.55 o 2 1 0 1048.99 947.04 32.93 o 3 1 0 2562.91 2338.32 124.23 o 4 1 0 68.82 28.19 47.78 o 5 1 0 1223.96 1301.87 65.90 o 6 1 0 2830.09 3167.99 99.95 o 7 1 0 1355.10 1483.90 154.87 o 8 1 0 1.75 -31.86 45.67 o 9 1 0 674.52 881.19 81.71 o -9 2 0 47.79 154.42 70.02 o -8 2 0 1431.42 1194.68 152.77 o -7 2 0 4392.06 4383.60 417.84 o -6 2 0 841.07 735.20 50.83 o -5 2 0 45.70 72.65 24.67 o -4 2 0 4417.98 4291.16 188.47 o -3 2 0 12073.79 11665.83 539.80 o -2 2 0 6192.00 5864.27 200.12 o -1 2 0 45.27 29.62 15.15 o 0 2 0 1405.02 1282.68 62.66 o 1 2 0 48261.13 55388.75 2286.29 o 2 2 0 65.84 45.61 13.93 o 3 2 0 104.31 114.47 23.28 o 4 2 0 1328.49 1376.54 68.64 o 5 2 0 2520.79 2621.40 106.77 o 6 2 0 1180.98 1155.05 56.46 o 7 2 0 220.28 291.47 112.10 o 8 2 0 32.44 50.32 50.15 o 9 2 0 764.77 770.93 113.73 o -8 3 0 700.93 720.95 63.70 o -7 3 0 159.38 213.65 49.51 o -6 3 0 2792.14 2763.91 133.66 o -5 3 0 1686.82 1578.29 85.35 o -4 3 0 3625.69 3418.59 218.66 o -3 3 0 513.92 464.24 32.52 o -2 3 0 4927.29 4400.24 217.72 o -1 3 0 10661.39 10146.10 460.26 o 0 3 0 2486.57 2243.43 89.51 o 1 3 0 203.12 210.29 24.97 o 2 3 0 5861.67 5106.60 290.74 o 3 3 0 6495.88 6553.97 341.66 o 4 3 0 4807.81 5592.89 142.84 o 5 3 0 121.05 185.22 44.76 o 6 3 0 1610.67 1690.49 90.88 o 7 3 0 4068.01 4600.75 173.82 o 8 3 0 527.44 548.64 65.26 o 9 3 0 84.92 137.36 84.36 o -8 4 0 2.79 -13.10 58.75 o -7 4 0 266.56 199.58 52.14 o -6 4 0 1011.18 884.68 75.13 o -5 4 0 661.20 613.49 63.02 o -4 4 0 293.80 288.69 29.55 o -3 4 0 515.28 492.85 49.04 o -2 4 0 798.43 807.32 36.07 o -1 4 0 1102.41 1048.63 57.88 o 0 4 0 585.52 632.36 33.90 o 1 4 0 162.06 207.84 45.06 o 2 4 0 1069.45 1060.02 79.10 o 3 4 0 128.59 116.37 33.28 o 4 4 0 994.22 1014.73 113.93 o 5 4 0 70.15 73.48 36.71 o 6 4 0 3.38 25.90 34.51 o 7 4 0 28.88 65.20 38.79 o 8 4 0 581.80 637.50 80.67 o -8 5 0 1188.75 1402.76 195.86 o -7 5 0 1501.89 1602.75 99.70 o -6 5 0 118.77 186.46 62.03 o -5 5 0 4153.45 4311.27 247.62 o -4 5 0 4378.58 4547.83 202.81 o -3 5 0 2427.86 2452.72 132.86 o -2 5 0 447.89 474.12 56.68 o -1 5 0 3282.48 3511.41 184.16 o 0 5 0 8440.61 8511.42 318.98 o 1 5 0 2139.13 2266.98 129.73 o 2 5 0 50.43 71.83 23.08 o 3 5 0 2716.43 2460.82 170.49 o 4 5 0 3290.61 3569.19 235.91 o 5 5 0 1376.63 1451.75 122.33 o 6 5 0 84.31 128.74 56.36 o 7 5 0 375.37 445.26 91.87 o 8 5 0 1459.80 1466.23 166.22 o -7 6 0 313.77 287.85 82.67 o -6 6 0 251.73 170.11 66.01 o -5 6 0 11.95 20.16 48.12 o -4 6 0 254.40 217.47 41.37 o -3 6 0 643.70 629.27 54.22 o -2 6 0 888.10 1016.05 66.96 o -1 6 0 1254.26 1175.49 90.64 o 0 6 0 343.25 410.96 41.42 o 1 6 0 1642.93 1664.83 153.83 o 2 6 0 1798.38 1630.71 76.64 o 3 6 0 817.63 822.99 67.69 o 4 6 0 104.25 81.80 32.08 o 5 6 0 1028.66 1259.46 178.16 o 6 6 0 686.82 884.80 170.96 o 7 6 0 414.69 562.87 82.07 o -6 7 0 655.05 660.53 106.16 o -5 7 0 40.45 -58.74 58.74 o -4 7 0 1313.43 1571.91 94.68 o -3 7 0 1815.98 1901.84 87.76 o -2 7 0 597.24 682.12 51.50 o -1 7 0 29.29 -5.71 36.22 o 0 7 0 311.22 269.41 49.88 o 1 7 0 1667.83 1724.31 152.58 o 2 7 0 513.94 541.51 41.09 o 3 7 0 37.37 32.38 35.10 o 4 7 0 118.89 113.68 40.87 o 5 7 0 280.17 139.70 56.45 o 6 7 0 184.97 202.44 121.66 o -5 8 0 971.10 1080.84 172.00 o -4 8 0 300.98 364.72 120.92 o -3 8 0 38.83 72.50 61.14 o -2 8 0 768.11 880.45 85.45 o -1 8 0 1912.90 2004.41 189.85 o 0 8 0 1682.05 1719.19 99.77 o 1 8 0 174.10 330.17 60.57 o 2 8 0 1012.77 1057.99 81.65 o 3 8 0 1305.37 1557.64 91.23 o 4 8 0 882.52 636.26 84.98 o 5 8 0 16.90 -38.59 77.18 o -3 9 0 1.23 69.13 61.14 o -2 9 0 177.91 134.11 105.70 o -1 9 0 127.67 200.76 76.54 o 0 9 0 53.06 22.08 52.93 o 1 9 0 136.32 126.02 101.95 o 2 9 0 29.52 142.27 75.19 o 3 9 0 81.30 120.10 203.04 o 4 9 0 121.64 148.56 148.56 o -3 -9 1 62.50 178.55 88.70 o -2 -9 1 26.27 16.83 69.10 o -1 -9 1 946.70 1068.88 120.29 o 0 -9 1 833.83 1125.40 112.50 o 1 -9 1 406.24 583.39 198.42 o 2 -9 1 45.55 85.85 87.29 o 3 -9 1 839.82 743.76 126.06 o -5 -8 1 66.70 39.57 78.81 o -4 -8 1 117.92 25.43 100.89 o -3 -8 1 211.82 160.54 92.94 o -2 -8 1 55.64 41.02 66.76 o -1 -8 1 2.78 27.23 47.57 o 0 -8 1 478.43 550.40 73.87 o 1 -8 1 509.83 493.59 64.29 o 2 -8 1 116.44 134.96 78.61 o 3 -8 1 13.67 19.88 101.25 o 4 -8 1 50.15 47.01 76.15 o 5 -8 1 425.44 336.75 113.71 o -6 -7 1 165.74 325.05 162.53 o -5 -7 1 121.53 442.45 120.99 o -4 -7 1 1357.19 1572.02 198.80 o -3 -7 1 1326.62 1371.09 81.15 o -2 -7 1 334.31 355.75 67.01 o -1 -7 1 36.70 61.98 34.17 o 0 -7 1 1995.39 2182.02 127.22 o 1 -7 1 1460.92 1552.54 106.19 o 2 -7 1 616.14 609.69 64.40 o 3 -7 1 4.96 -50.20 50.20 o 4 -7 1 824.48 965.76 98.57 o 5 -7 1 1065.52 1116.10 139.52 o 6 -7 1 136.12 85.87 102.32 o -7 -6 1 178.99 186.24 57.70 o -6 -6 1 715.55 887.30 90.37 o -5 -6 1 687.33 635.36 94.24 o -4 -6 1 152.62 204.39 41.04 o -3 -6 1 628.51 687.64 51.94 o -2 -6 1 2249.96 2103.25 78.51 o -1 -6 1 2137.44 2370.85 146.11 o 0 -6 1 1471.69 1583.92 86.01 o 1 -6 1 1596.13 1743.95 99.94 o 2 -6 1 3441.65 3598.04 102.33 o 3 -6 1 2331.46 2330.69 88.94 o 4 -6 1 293.38 433.57 101.09 o 5 -6 1 92.08 299.41 59.12 o 6 -6 1 1469.19 1348.04 97.67 o 7 -6 1 1215.13 1077.47 115.26 o -8 -5 1 5.97 81.14 58.03 o -7 -5 1 477.82 687.31 134.76 o -6 -5 1 865.97 1010.19 236.42 o -5 -5 1 235.81 178.28 36.39 o -4 -5 1 43.09 48.83 23.52 o -3 -5 1 926.95 1113.30 100.89 o -2 -5 1 555.71 490.79 37.55 o -1 -5 1 334.47 317.85 35.86 o 0 -5 1 312.20 408.51 44.03 o 1 -5 1 445.95 455.60 65.99 o 2 -5 1 358.33 399.14 55.11 o 3 -5 1 207.32 208.36 31.29 o 4 -5 1 290.25 259.29 35.85 o 5 -5 1 8.42 87.02 40.89 o 6 -5 1 14.65 44.01 48.66 o 7 -5 1 64.49 126.61 55.33 o -8 -4 1 1616.78 1580.36 125.41 o -7 -4 1 92.14 65.59 39.04 o -6 -4 1 828.76 933.14 146.42 o -5 -4 1 3054.08 3854.46 150.37 o -4 -4 1 4702.88 4369.24 373.32 o -3 -4 1 1801.68 2011.42 168.17 o -2 -4 1 2273.80 2495.81 154.56 o -1 -4 1 7300.34 6945.28 299.21 o 0 -4 1 8660.25 7984.00 385.02 o 1 -4 1 5583.25 5273.89 197.05 o 2 -4 1 4682.27 4542.65 114.13 o 3 -4 1 6440.88 6333.66 207.06 o 4 -4 1 4248.67 4138.37 143.24 o 5 -4 1 828.50 878.43 67.52 o 6 -4 1 118.63 63.32 58.51 o 7 -4 1 1511.56 1460.33 174.93 o 8 -4 1 1536.70 1425.91 259.76 o -9 -3 1 252.60 554.50 163.20 o -8 -3 1 11.18 -34.27 53.80 o -7 -3 1 784.34 843.78 63.15 o -6 -3 1 27.40 -11.49 24.50 o -5 -3 1 185.10 165.96 30.87 o -4 -3 1 245.31 344.28 34.32 o -3 -3 1 1494.24 1421.27 102.94 o -2 -3 1 879.10 789.64 33.96 o -1 -3 1 329.22 360.12 68.34 o 0 -3 1 331.88 260.74 50.73 o 1 -3 1 5323.60 4829.07 199.49 o 2 -3 1 1551.27 1452.15 93.24 o 3 -3 1 896.70 921.31 36.82 o 4 -3 1 34.38 73.72 40.15 o 5 -3 1 2647.12 2646.14 137.10 o 6 -3 1 2948.18 2858.33 149.29 o 7 -3 1 705.00 659.43 60.07 o 8 -3 1 251.94 201.01 68.19 o -9 -2 1 402.68 323.83 74.88 o -8 -2 1 1031.56 1123.21 79.58 o -7 -2 1 3677.59 3793.73 139.04 o -6 -2 1 276.54 243.93 31.98 o -5 -2 1 1195.53 1184.57 76.59 o -4 -2 1 3805.28 4040.21 177.97 o -3 -2 1 9033.85 8061.90 548.52 o -2 -2 1 2896.38 2932.09 128.20 o -1 -2 1 3214.92 3062.29 210.93 o 0 -2 1 8295.28 7629.76 285.11 o 1 -2 1 8348.11 7466.10 312.95 o 2 -2 1 4533.18 4535.39 106.95 o 3 -2 1 2180.90 2295.34 112.97 o 4 -2 1 1676.49 1499.60 45.56 o 5 -2 1 2189.74 2179.98 73.41 o 6 -2 1 643.81 689.06 60.57 o 7 -2 1 4.44 69.40 29.69 o 8 -2 1 221.76 236.12 46.86 o 9 -2 1 355.84 398.94 91.66 o -9 -1 1 459.47 586.70 117.25 o -8 -1 1 41.22 119.07 45.90 o -7 -1 1 3.23 128.02 44.42 o -6 -1 1 5923.37 5977.97 338.64 o -5 -1 1 3771.27 4490.90 152.08 o -4 -1 1 220.16 264.22 29.31 o -3 -1 1 2304.23 2106.92 178.66 o -2 -1 1 12050.89 11917.75 243.68 o -1 -1 1 10354.41 9978.99 226.59 o 0 -1 1 1157.13 1187.52 69.18 o 1 -1 1 150.66 132.00 17.24 o 2 -1 1 12822.43 12124.42 246.96 o 3 -1 1 10530.17 10276.11 280.93 o 4 -1 1 3672.10 3394.50 177.88 o 5 -1 1 802.40 842.25 47.52 o 6 -1 1 4055.87 3878.18 261.80 o 7 -1 1 4920.05 5418.89 316.90 o 8 -1 1 966.23 921.31 127.74 o 9 -1 1 407.55 530.04 87.80 o -9 0 1 53.63 129.87 70.20 o -8 0 1 13.84 3.39 65.02 o -7 0 1 294.77 231.88 34.59 o -6 0 1 2037.29 2065.81 76.18 o -5 0 1 466.54 515.05 36.20 o -4 0 1 38.87 0.00 17.42 o -3 0 1 362.54 354.13 28.12 o -2 0 1 3918.65 3740.35 196.24 o -1 0 1 9.43 124.87 31.14 o 1 0 1 17.34 114.46 37.14 o 2 0 1 253.65 252.70 30.26 o 3 0 1 1991.55 1801.22 87.67 o 4 0 1 733.14 632.40 33.42 o 5 0 1 485.31 524.22 51.97 o 6 0 1 132.05 95.30 26.82 o 7 0 1 143.81 116.62 27.86 o 8 0 1 437.12 528.12 70.47 o 9 0 1 323.51 355.49 79.45 o -9 1 1 1334.30 1458.98 114.39 o -8 1 1 2060.43 2342.19 211.53 o -7 1 1 91.26 82.88 34.23 o -6 1 1 349.38 324.56 29.10 o -5 1 1 12376.80 12266.58 637.52 o -4 1 1 8606.56 7873.96 337.75 o -3 1 1 390.45 361.49 21.78 o -2 1 1 7448.99 7343.54 299.81 o -1 1 1 11241.35 10629.38 400.76 o 1 1 1 2108.32 2019.57 58.75 o 2 1 1 175.96 218.07 30.97 o 3 1 1 10792.78 10446.85 344.00 o 4 1 1 8822.84 8763.92 429.54 o 5 1 1 1785.15 1750.21 108.72 o 6 1 1 1253.45 1262.68 56.43 o 7 1 1 864.90 749.42 77.49 o 8 1 1 1783.35 2236.55 108.03 o 9 1 1 551.99 726.80 75.55 o -9 2 1 66.39 175.35 82.01 o -8 2 1 89.36 90.30 86.34 o -7 2 1 1641.18 1504.44 65.90 o -6 2 1 329.53 338.71 74.44 o -5 2 1 34.01 79.74 22.02 o -4 2 1 1029.98 960.12 63.33 o -3 2 1 3168.13 2949.83 155.91 o -2 2 1 3105.48 3071.75 118.95 o -1 2 1 710.05 804.77 69.33 o 0 2 1 1747.40 1767.64 128.62 o 1 2 1 44162.34 47630.69 2634.18 o 2 2 1 4102.90 3751.42 145.10 o 3 2 1 394.01 320.80 30.10 o 4 2 1 1286.55 1302.71 84.84 o 5 2 1 4293.55 4250.38 134.78 o 6 2 1 2742.21 2900.56 184.58 o 7 2 1 178.03 181.71 53.27 o 8 2 1 8.24 92.71 52.12 o 9 2 1 1391.23 1399.07 108.34 o -8 3 1 1086.48 907.43 84.25 o -7 3 1 2263.85 2088.74 185.77 o -6 3 1 340.38 344.62 51.96 o -5 3 1 1175.15 1188.83 57.18 o -4 3 1 4922.02 4789.60 273.10 o -3 3 1 3589.52 3541.44 107.58 o -2 3 1 272.20 260.53 30.00 o -1 3 1 1365.67 1338.29 56.20 o 0 3 1 2287.45 2080.53 50.79 o 1 3 1 3529.90 2908.62 269.31 o 2 3 1 1559.52 1418.74 63.01 o 3 3 1 116.62 108.24 21.17 o 4 3 1 951.60 1283.27 97.04 o 5 3 1 902.13 1004.66 47.75 o 6 3 1 364.10 375.96 52.29 o 7 3 1 20.02 15.65 54.11 o 8 3 1 70.44 24.38 36.07 o 9 3 1 146.90 181.24 85.77 o -8 4 1 11.79 -26.13 104.52 o -7 4 1 402.72 435.89 70.14 o -6 4 1 4980.90 4902.39 399.33 o -5 4 1 1756.35 1712.96 68.12 o -4 4 1 715.94 788.68 72.76 o -3 4 1 1436.94 1297.11 82.78 o -2 4 1 9528.20 9828.02 258.30 o -1 4 1 7928.21 8073.25 373.34 o 0 4 1 1325.68 1340.25 45.15 o 1 4 1 49.21 123.98 18.31 o 2 4 1 27859.73 30210.45 1910.81 o 3 4 1 2933.66 2689.27 201.84 o 4 4 1 682.12 731.56 59.13 o 5 4 1 551.21 609.05 50.34 o 6 4 1 2889.31 3643.05 208.78 o 7 4 1 1957.18 2016.91 136.98 o 8 4 1 254.19 221.29 59.96 o -8 5 1 126.87 60.28 71.81 o -7 5 1 22.59 110.61 61.19 o -6 5 1 433.11 337.66 56.25 o -5 5 1 624.58 634.18 52.80 o -4 5 1 80.07 95.62 37.06 o -3 5 1 63.97 105.68 30.34 o -2 5 1 441.48 471.41 33.57 o -1 5 1 592.08 610.72 82.01 o 0 5 1 461.54 480.01 54.92 o 1 5 1 78.34 73.33 32.35 o 2 5 1 9.17 18.17 19.82 o 3 5 1 778.24 781.47 69.20 o 4 5 1 402.74 476.69 33.15 o 5 5 1 626.43 703.34 44.82 o 6 5 1 43.61 -2.69 41.07 o 7 5 1 209.48 180.51 150.91 o 8 5 1 399.42 433.39 89.48 o -7 6 1 32.21 35.20 104.85 o -6 6 1 360.86 500.89 123.72 o -5 6 1 3237.19 3515.97 303.75 o -4 6 1 1760.31 1822.85 129.83 o -3 6 1 952.66 1025.27 74.93 o -2 6 1 820.04 908.44 53.42 o -1 6 1 4838.96 4982.35 156.49 o 0 6 1 3134.69 3266.06 138.84 o 1 6 1 521.39 602.98 62.70 o 2 6 1 6.73 -5.89 34.37 o 3 6 1 5873.26 6308.06 558.81 o 4 6 1 796.13 866.67 73.44 o 5 6 1 503.62 658.14 68.90 o 6 6 1 58.40 47.99 38.36 o 7 6 1 493.54 396.49 95.45 o -6 7 1 634.30 747.76 168.44 o -5 7 1 7.34 2.53 98.89 o -4 7 1 1155.90 1237.05 77.58 o -3 7 1 722.54 858.94 88.41 o -2 7 1 1753.27 1746.53 149.15 o -1 7 1 10.75 25.95 32.99 o 0 7 1 560.18 544.12 50.04 o 1 7 1 1999.80 2006.18 205.15 o 2 7 1 900.50 902.10 50.28 o 3 7 1 459.31 426.03 67.24 o 4 7 1 523.18 533.82 43.68 o 5 7 1 823.47 738.80 66.09 o 6 7 1 884.14 1164.16 161.48 o 7 7 1 145.62 22.50 156.84 o -5 8 1 10.94 -31.24 96.78 o -4 8 1 493.08 615.81 99.62 o -3 8 1 632.54 634.88 75.05 o -2 8 1 352.42 356.15 71.76 o -1 8 1 15.06 10.34 50.37 o 0 8 1 267.70 207.36 80.98 o 1 8 1 422.83 453.57 45.95 o 2 8 1 275.93 305.51 40.17 o 3 8 1 141.00 119.07 39.41 o 4 8 1 153.42 116.96 49.26 o 5 8 1 86.13 223.80 111.90 o 6 8 1 245.76 304.66 76.25 o -3 9 1 808.63 878.59 123.46 o -2 9 1 989.17 1122.08 101.36 o -1 9 1 1091.39 1296.75 111.24 o 0 9 1 5.79 -23.08 76.95 o 1 9 1 156.47 345.13 151.23 o 2 9 1 1057.65 807.38 76.75 o 3 9 1 506.17 467.57 103.40 o 4 9 1 215.15 398.55 183.79 o 0 10 1 219.10 126.60 151.84 o 1 10 1 165.92 244.49 330.72 o -2 -9 2 136.36 52.92 149.05 o -1 -9 2 37.29 179.65 97.69 o 0 -9 2 5.15 38.15 99.34 o 1 -9 2 7.22 42.31 87.56 o 2 -9 2 53.18 -5.67 141.54 o -5 -8 2 825.00 919.62 160.47 o -4 -8 2 474.56 478.77 159.71 o -3 -8 2 9.03 -16.73 51.54 o -2 -8 2 512.48 609.54 68.91 o -1 -8 2 1952.21 2108.84 143.94 o 0 -8 2 839.20 905.80 128.73 o 1 -8 2 26.04 100.67 54.23 o 2 -8 2 723.83 866.62 187.86 o 3 -8 2 1497.52 1819.48 153.57 o 4 -8 2 828.75 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