#------------------------------------------------------------------------------ #$Date: 2017-11-18 08:27:06 +0200 (Sat, 18 Nov 2017) $ #$Revision: 203329 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/81/1548115.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_1548115 loop_ _publ_author_name 'Dakovi\'c, Marijana' 'Soldin, \ 2\s(I)' _cod_data_source_file lq5009.cif _cod_data_source_block 5 _cod_original_cell_volume 631.67(10) _cod_database_code 1548115 _shelx_shelxl_version_number 2014/7 _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_res_file ; shelxl.res created by SHELXL-2014/7 TITL exp_505 in P2(1)/n CELL 0.71073 3.8840 23.1636 7.0359 90.000 93.712 90.000 ZERR 2 0.0003 0.0021 0.0008 0.000 0.009 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O BR CD UNIT 16 16 8 4 4 2 MERG 2 OMIT -1.00 50.00 FMAP 2 PLAN 20 BOND $H HTAB HTAB C1 Br1 EQIV $1 x+1/2, -y+1/2, z-1/2 HTAB N2 O1_$1 DFIX 0.86 N2 H21 CONF ACTA TEMP 23 L.S. 10 WGHT 0.045400 0.098500 FVAR 5.76675 CD1 6 0.500000 0.000000 0.500000 10.50000 0.03027 0.02212 = 0.02961 -0.00101 0.00781 -0.00126 BR1 5 0.971666 0.042102 0.259911 11.00000 0.03339 0.03390 = 0.02948 0.00459 0.00762 -0.00015 N1 3 0.514463 0.090867 0.665340 11.00000 0.04295 0.02139 = 0.02491 -0.00566 0.00890 -0.00347 N2 3 0.593574 0.190076 0.654918 11.00000 0.05970 0.02395 = 0.03685 0.00181 0.01897 -0.00328 H21 2 0.660024 0.216676 0.582061 11.00000 -1.20000 O1 4 0.449084 0.252009 0.888318 11.00000 0.11039 0.03143 = 0.04944 -0.01983 0.03256 0.00121 C1 1 0.607197 0.137550 0.580658 11.00000 0.04301 0.02165 = 0.03283 -0.00072 0.01104 0.00423 AFIX 43 H1 2 0.688685 0.133964 0.459808 11.00000 -1.20000 AFIX 0 C2 1 0.465867 0.201424 0.831075 11.00000 0.05185 0.03515 = 0.03188 -0.00161 0.01467 0.00338 C3 1 0.367304 0.149978 0.925023 11.00000 0.04911 0.03143 = 0.03096 -0.00127 0.01712 -0.00534 AFIX 43 H3 2 0.281678 0.152358 1.045191 11.00000 -1.20000 AFIX 0 C4 1 0.396383 0.098783 0.842950 11.00000 0.05040 0.03423 = 0.02199 0.00249 0.00775 -0.00666 AFIX 43 H4 2 0.332794 0.066294 0.909989 11.00000 -1.20000 AFIX 0 HKLF 4 REM exp_505 in P2(1)/n REM R1 = 0.0445 for 944 Fo > 4sig(Fo) and 0.0550 for all 1108 data REM 82 parameters refined using 1 restraints END WGHT 0.0453 0.1126 REM Instructions for potential hydrogen bonds HTAB N2 O1_$1 HTAB C1 Br1 EQIV $2 x-1, y, z+1 HTAB C4 Br1_$2 EQIV $3 -x+1, -y, -z+1 HTAB C4 Br1_$3 REM Highest difference peak 1.667, deepest hole -0.793, 1-sigma level 0.170 Q1 1 0.2493 0.0000 0.5134 11.00000 0.05 1.67 Q2 1 0.0000 0.0000 0.5000 10.50000 0.05 1.42 Q3 1 0.7226 0.0425 0.2668 11.00000 0.05 1.36 Q4 1 1.2373 0.0406 0.2394 11.00000 0.05 1.24 Q5 1 1.4687 0.0424 0.2585 11.00000 0.05 1.13 Q6 1 0.4399 0.0823 1.0195 11.00000 0.05 0.56 Q7 1 0.3956 0.2513 0.7897 11.00000 0.05 0.44 Q8 1 0.8737 0.0464 0.3937 11.00000 0.05 0.42 Q9 1 0.9399 0.1340 0.4414 11.00000 0.05 0.41 Q10 1 0.4720 -0.0016 0.7205 11.00000 0.05 0.39 Q11 1 0.9238 0.2411 0.8661 11.00000 0.05 0.38 Q12 1 0.1951 0.0872 1.0258 11.00000 0.05 0.36 Q13 1 0.8381 0.1547 0.9112 11.00000 0.05 0.36 Q14 1 0.1650 0.0437 0.7462 11.00000 0.05 0.36 Q15 1 0.5227 0.1381 1.0919 11.00000 0.05 0.35 Q16 1 0.1414 0.1262 0.5675 11.00000 0.05 0.35 Q17 1 0.7272 0.0755 0.1093 11.00000 0.05 0.34 Q18 1 -0.0885 0.1022 0.9202 11.00000 0.05 0.34 Q19 1 0.1050 0.0734 0.6345 11.00000 0.05 0.34 Q20 1 0.8481 0.2457 0.9021 11.00000 0.05 0.33 ; _shelx_res_checksum 52093 _shelx_hkl_file ; 0 0 -2 53214.9 2242.83 1 0 0 2 52423.9 2467.75 2 0 0 -2 54925.6 2651.16 2 0 0 -3 149.555 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74311.0 4078.34 3 0 -2 -5 69614.7 4173.70 1 0 2 -6 846.129 987.395 1 0 2 -6 1218.64 833.914 3 0 -2 -6 3710.69 1513.01 1 0 2 -7 21693.0 2556.85 3 0 2 -7 24208.9 2898.47 1 0 2 -8 66856.4 4660.39 3 0 2 -8 76325.0 5527.03 1 0 -2 -9 5115.21 1460.44 3 0 3 -2 8665.53 874.825 3 0 -3 -2 11310.2 1259.78 2 0 3 2 8487.86 1000.69 1 0 3 2 9907.19 1140.81 2 0 3 3 132109. 5121.78 2 0 -3 -3 133713. 4657.65 1 0 3 -3 132733. 4390.30 3 0 3 -3 135062. 5193.02 2 0 -3 -4 8915.58 1605.26 1 0 3 4 7444.43 1454.22 2 0 3 -4 6707.50 1143.19 3 0 3 -5 127588. 5431.64 3 0 3 -5 131470. 5717.92 1 0 -3 -5 121046. 5568.05 1 0 3 -6 9764.13 1665.32 3 0 3 -6 9138.82 1808.68 1 0 3 -7 7226.99 1623.91 3 0 3 -7 5863.63 1708.22 1 0 3 -8 3983.80 1322.64 3 0 3 -8 4461.81 1872.26 1 0 -3 -9 13895.0 2403.90 3 0 3 -9 25407.4 3634.66 1 0 -4 -1 520508. 10458.5 2 0 -4 1 508306. 9523.57 3 0 4 1 510295. 10380.0 2 0 4 2 9040.95 1026.89 1 0 -4 -2 10883.3 1250.63 2 0 4 -2 9857.24 904.064 3 0 4 2 9950.66 1148.08 2 0 -4 2 11084.9 881.776 3 0 4 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426569. 9804.39 2 0 -6 -1 427730. 9779.24 2 0 6 -2 292415. 6764.06 3 0 -6 2 286007. 6653.97 3 0 6 2 287421. 7982.76 2 0 6 3 184020. 6674.42 2 0 6 -3 199206. 5551.83 3 0 6 -4 144059. 5062.14 3 0 6 4 131930. 6011.43 2 0 6 -5 164554. 5992.41 3 0 6 5 141191. 6849.25 2 0 6 -6 21730.8 2303.45 3 0 6 -7 47095.7 3592.68 3 0 6 -7 60560.1 4476.84 1 0 6 -8 9011.42 2163.15 1 0 6 -8 9211.08 1741.67 3 0 -7 0 43.8265 230.095 3 0 7 0 467.786 326.782 2 0 7 1 185916. 5317.85 2 0 -7 -1 182397. 5275.59 2 0 -7 1 187418. 4692.11 3 0 7 -1 183839. 4675.91 3 0 7 -2 3768.70 684.625 3 0 7 2 3358.52 839.098 2 0 -7 2 3554.17 551.088 3 0 7 3 168276. 6310.42 2 0 -7 3 171474. 5020.32 3 0 7 -3 173527. 5039.78 3 0 7 4 7707.57 1537.85 2 0 7 -4 7716.29 1129.10 3 0 7 5 38802.4 3444.67 2 0 7 -5 37278.6 2694.21 3 0 7 -6 21065.0 2236.58 3 0 7 6 20315.2 2713.28 2 0 7 -7 32571.1 3008.85 3 0 7 -7 29502.1 3228.39 1 0 7 -8 6116.23 1696.01 1 0 8 0 35823.4 1805.68 2 0 -8 0 37650.2 1816.01 3 0 8 1 482292. 10981.7 2 0 -8 -1 478404. 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4331.73 1013.68 3 0 15 4 6819.36 1745.56 2 0 15 -5 13753.4 1740.93 3 0 15 5 14166.4 2493.10 2 0 15 6 3299.07 1444.96 2 0 15 -6 2464.11 968.860 3 0 15 7 18368.4 2994.67 2 0 16 0 19108.0 1918.94 2 0 16 1 177241. 6737.13 2 0 16 -1 170472. 5971.79 2 0 16 -2 195919. 6508.99 3 0 16 2 201362. 7689.15 2 0 16 -2 188897. 6314.83 2 0 16 3 55920.0 4113.04 2 0 16 -3 55815.3 3227.66 3 0 16 -4 3411.83 907.330 3 0 16 4 1657.89 1030.50 2 0 16 5 38010.4 3885.67 2 0 16 -5 34203.2 2832.75 3 0 16 6 42470.4 4378.03 2 0 16 7 12085.4 2575.17 2 0 17 0 143.427 564.528 2 0 17 -1 83592.4 4068.49 2 0 17 1 85797.9 4635.98 2 0 17 2 4289.31 1340.70 2 0 17 -2 4122.16 1066.74 3 0 17 -2 4263.43 989.097 2 0 17 3 42860.4 3695.96 2 0 17 -3 45377.0 2978.25 3 0 17 4 6082.71 1662.80 2 0 17 -4 5335.73 1132.80 3 0 17 5 30494.4 3533.67 2 0 17 -5 28611.9 2590.58 3 0 17 6 4646.15 1590.41 2 0 17 7 11207.4 2495.65 2 0 18 0 8119.41 1405.38 2 0 18 -1 60749.9 3537.94 2 0 18 1 64673.6 4122.11 2 0 18 -2 50072.5 3095.18 2 0 18 2 54045.4 3911.63 2 0 18 3 87445.1 5480.02 2 0 18 -3 85465.1 4325.30 3 0 18 -4 66140.2 3840.50 3 0 18 4 63653.0 4894.18 2 0 18 -5 49031.3 3446.14 3 0 18 5 52500.9 4681.38 2 0 18 6 14277.1 2689.51 2 0 19 0 3464.62 1157.68 2 0 19 -1 28861.5 2569.05 2 0 19 1 28166.8 2857.54 2 0 19 -2 2322.06 813.910 2 0 19 2 2056.65 1093.98 2 0 19 -3 47396.1 3316.97 3 0 19 -3 46813.4 3119.45 2 0 19 3 53028.6 4345.23 2 0 19 4 1468.33 1026.56 2 0 19 -4 1047.78 610.769 3 0 19 -5 34753.6 2930.54 3 0 19 5 38373.8 4130.51 2 0 19 6 358.159 969.199 2 0 20 0 274571. 9344.53 2 0 20 -1 31891.7 2724.49 2 0 20 1 32945.4 3135.64 2 0 20 -2 1651.25 880.116 2 0 20 2 3590.04 1224.11 2 0 20 3 51798.8 4398.27 2 0 20 -3 46966.0 3208.51 2 0 20 -3 55469.1 3584.14 3 0 20 -4 45200.2 3387.20 3 0 20 4 41747.9 4187.98 2 0 20 5 27938.5 3654.19 2 0 20 6 1562.23 1282.32 2 0 21 0 7808.35 1667.71 2 0 21 1 64075.0 4409.64 2 0 21 -1 63831.1 4040.76 2 0 21 -2 8126.92 1421.38 2 0 21 2 9276.19 1936.43 2 0 21 -3 8123.15 1402.46 2 0 21 3 10344.1 2006.94 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63143.4 4066.72 3 -3 5 -2 60211.2 4042.35 3 -3 -5 -3 36290.0 3491.96 3 -3 5 -3 34381.7 3167.49 3 -3 -5 -4 10363.5 2302.17 3 -3 5 -4 6720.97 1710.18 3 -3 -5 -5 24812.0 3503.41 3 -3 5 -5 26026.2 3394.53 3 -3 -5 -6 12651.6 2815.85 3 -3 5 -6 12833.9 2641.14 3 3 -6 -7 8368.18 2310.64 1 3 6 -7 5784.28 1891.20 1 -3 6 6 20032.5 2478.46 2 3 -6 -6 20000.7 3064.84 1 3 -6 -5 17546.4 2797.23 1 -3 6 5 11783.2 1851.04 2 3 -6 -4 23039.3 2901.62 1 -3 6 4 24231.3 2466.52 2 3 -6 -3 66331.0 4291.52 1 -3 6 3 64287.8 3939.56 2 -3 6 2 26992.7 2231.41 3 3 -6 -2 26225.1 2524.67 1 -3 6 1 62464.6 3596.84 3 -3 -6 1 58119.5 2655.56 3 -3 -6 0 24487.3 1986.54 3 -3 6 0 24882.4 2335.24 3 -3 -6 -1 28361.1 2457.18 3 -3 6 -1 25743.1 2582.65 3 -3 -6 -2 16893.4 2268.91 3 -3 6 -2 18008.0 2347.58 3 -3 -6 -3 26695.0 3078.54 3 -3 6 -3 31713.0 3125.29 3 -3 -6 -4 2992.72 1396.60 3 -3 6 -4 1970.39 1217.66 3 -3 -6 -5 15395.7 2876.85 3 -3 6 -5 10985.6 2298.25 3 -3 -6 -6 412.961 1185.36 3 -3 6 -6-268.739 1156.42 3 -3 7 6 10923.8 1952.87 2 3 -7 -5 22240.0 2980.95 1 -3 7 5 20618.3 2427.48 2 3 -7 -4 88099.7 5401.23 1 -3 7 4 86806.9 4905.29 2 3 -7 -3 53082.1 3851.38 1 -3 7 3 46241.1 3374.86 2 -3 7 2 19465.4 1930.74 3 -3 7 1 56039.4 3414.51 3 -3 -7 1 54835.4 2540.07 3 -3 -7 0 48908.3 2808.16 3 -3 7 0 45263.4 3186.59 3 -3 -7 -1 42909.9 3066.26 3 -3 7 -1 45608.9 3392.91 3 -3 -7 -2 12351.1 1975.34 3 -3 7 -2 14347.3 2071.69 3 -3 -7 -3 39621.6 3787.62 3 -3 7 -3 44397.0 3730.91 3 -3 -7 -4 24702.3 3316.55 3 -3 7 -4 25585.9 2966.70 3 -3 -7 -5 18176.7 2973.35 3 -3 7 -5 16772.7 2629.68 3 -3 -7 -6 1074.05 1253.45 3 -3 7 -6-79.2741 1140.09 3 -3 8 6 12949.1 2182.65 2 -3 8 5 87547.3 5170.27 2 -3 8 4 13277.5 1939.20 2 -3 8 3 5964.30 1310.12 2 -3 8 2 19592.8 2021.70 3 -3 8 1 74167.2 4030.63 3 -3 -8 1 71621.3 2973.30 3 -3 -8 0 22075.6 1969.01 3 -3 8 0 19179.1 2218.75 3 -3 -8 -1 20734.5 2202.35 3 -3 8 -1 22343.1 2484.75 3 -3 -8 -2 10852.5 1891.93 3 -3 8 -2 11858.5 1979.46 3 -3 -8 -3 28478.6 3312.86 3 -3 8 -3 28581.5 3059.18 3 -3 -8 -4 2501.71 1358.88 3 -3 8 -4 3366.64 1519.54 3 -3 -8 -5 10181.1 2480.55 3 -3 8 -5 10558.0 2199.75 3 -3 -8 -6 182.856 1365.71 3 -3 8 -6-603.378 1321.33 3 -3 9 6 2889.55 1267.38 2 -3 9 5 23810.3 2770.96 2 -3 9 4 71271.0 4564.15 2 -3 9 3 35563.4 3074.55 2 -3 9 2 2495.88 935.843 3 -3 9 1 15494.5 2013.31 3 -3 -9 1 16421.8 1393.52 3 -3 9 0 149388. 6415.42 3 -3 -9 0 161778. 5772.20 3 -3 9 -1 12352.5 1892.06 3 -3 -9 -1 17301.1 2054.78 3 -3 -9 -2-340.076 942.099 3 -3 9 -2 953.049 1118.89 3 -3 -9 -3 9682.98 2141.32 3 -3 9 -3 14038.4 2348.05 3 -3 -9 -4 65491.3 5402.78 3 -3 9 -4 65342.6 4991.85 3 -3 -9 -5 5459.65 1871.24 3 -3 9 -5 5618.18 1644.33 3 -3 -9 -6-1154.25 1504.16 3 -3 9 -6-2848.47 1278.76 3 -3 10 7 434.505 880.430 2 -3 10 6 6087.57 1709.45 2 -3 10 5 81735.5 5223.95 2 -3 10 4 3302.08 1186.53 2 -3 10 3 2101.37 1113.14 2 -3 10 2 2023.22 970.178 3 -3 10 1 112981. 5285.73 3 -3 -10 0 5840.75 1250.00 3 -3 10 0 6891.42 1664.76 3 -3 -10 -1 6563.89 1418.15 3 -3 10 -1 8320.66 1646.80 3 -3 -10 -2 1525.89 783.059 3 -3 10 -2 1576.15 924.822 3 -3 -10 -3 32397.6 3528.13 3 -3 10 -3 33218.2 3408.63 3 -3 -10 -4 4070.65 1857.81 3 -3 10 -4 2837.27 1842.11 3 -3 -10 -5 7839.95 2272.27 3 -3 10 -5 7050.66 1927.62 3 -3 11 7 1746.83 1141.33 2 -3 11 6 466.491 805.012 2 -3 11 5 1292.86 1031.97 2 -3 11 4 64396.8 4591.21 2 -3 11 3-172.640 601.712 2 -3 11 2 135.133 723.454 3 -3 11 1 5433.98 1462.51 3 -3 11 0 199465. 7780.58 3 -3 -11 0 202343. 6923.98 3 -3 -11 -1 3021.94 1021.28 3 -3 11 -1 3141.94 1308.94 3 -3 11 -2 1835.15 983.597 3 -3 -11 -2 1649.03 1010.77 3 -3 11 -3 4349.02 1604.95 3 -3 -11 -4 82817.0 6362.34 3 -3 11 -4 96338.3 6240.00 3 -3 11 -5 167.180 1199.72 3 -3 -11 -5 1310.51 1207.72 3 -3 12 7-228.131 818.242 2 -3 12 6 37.4600 765.696 2 -3 12 5 85743.4 5562.62 2 -3 12 4 57.9207 918.504 2 -3 12 3 2728.96 1061.31 2 -3 12 2 130.954 701.551 3 -3 12 1 109045. 5412.76 3 -3 -12 0 1739.97 945.854 3 -3 12 0 2214.82 1267.41 3 -3 12 -1 7892.26 1672.45 3 -3 -12 -1 6045.61 1315.65 3 -3 12 -2 1382.24 1159.72 3 -3 12 -3 31332.1 3369.64 3 -3 12 -4 3746.49 1929.29 3 -3 12 -5 4120.71 1493.73 3 -3 13 7 287.400 1163.39 2 -3 13 6 2271.64 1121.61 2 -3 13 5-505.201 885.848 2 -3 13 4 108239. 6299.35 2 -3 13 3 9729.88 1851.71 2 -3 13 2 2203.53 1097.02 3 -3 13 1 4783.90 1588.98 3 -3 13 0 127168. 6222.51 3 -3 -13 0 137190. 5707.93 3 -3 13 -1 1402.95 1020.60 3 -3 13 -2 2452.73 1204.64 3 -3 13 -3 2931.20 1504.48 3 -3 13 -4 54817.8 4841.61 3 -3 13 -5 212.765 1263.95 3 -3 14 6 3418.32 1357.87 2 -3 14 5 44693.1 4222.94 2 -3 14 4 3897.38 1512.16 2 -3 14 3 2829.40 1286.07 2 -3 14 2-43.8059 802.285 2 -3 14 1 78274.6 4798.72 3 -3 14 0 9612.37 1846.08 3 -3 -14 0 8371.12 1535.55 3 -3 14 -1 3844.33 1391.69 3 -3 14 -2 2692.12 1351.42 3 -3 14 -3 33812.8 3549.38 3 -3 14 -4 2341.13 1500.04 3 -3 14 -5-2347.18 1511.99 3 -3 15 6 3400.37 1394.68 2 -3 15 5 9785.53 2000.26 2 -3 15 4 55365.4 4576.15 2 -3 15 3 4192.83 1351.44 2 -3 15 2 2878.11 1169.67 2 -3 15 1 13432.2 2170.84 3 -3 15 0 83394.3 5124.94 3 -3 15 -1 13569.3 2150.89 3 -3 15 -2 2432.69 1253.75 3 -3 15 -3 11524.6 2370.52 3 -3 15 -4 33787.5 3771.95 3 -3 15 -5 9938.20 2401.82 3 -3 16 5 23011.0 3161.09 2 -3 16 4 16798.2 2671.14 2 -3 16 3 16393.2 2544.49 2 -3 16 2 14149.0 2331.16 2 -3 16 1 36695.4 3422.25 3 -3 16 0 7159.22 1791.61 3 -3 16 -1 4213.06 1457.03 3 -3 16 -2 5412.91 1737.63 3 -3 16 -3 28484.1 3476.15 3 -3 16 -4 3802.27 1844.17 3 -3 17 5 7709.69 1924.69 2 -3 17 4 31430.0 3562.40 2 -3 17 3 23712.7 3014.20 2 -3 17 2 9631.52 1983.14 2 -3 17 1 32637.4 3334.83 3 -3 17 0 28461.6 3184.43 3 -3 17 -1 19280.5 2708.69 3 -3 17 -2 20694.4 2940.00 3 -3 17 -3 18660.7 2926.98 3 -3 17 -4 19006.7 3165.13 3 -3 18 5 7609.65 1984.44 2 -3 18 4 17841.8 2825.78 2 -3 18 3 16734.8 2680.15 2 -3 18 2 13507.4 2363.82 2 -3 18 1 21300.1 2730.51 3 -3 18 0 5791.12 1685.22 3 -3 18 -1 25651.9 3054.50 3 -3 18 -2 3907.16 1505.43 3 -3 18 -3 13314.9 2598.44 3 -3 18 -4 4244.11 1802.08 3 -3 19 4 8596.39 2050.74 2 -3 19 3 7665.03 1937.70 2 -3 19 2 25196.5 3252.02 2 -3 19 1 12400.5 2293.80 3 -3 19 1 11155.8 2264.84 2 -3 19 0 7822.47 1778.24 3 -3 19 -1 35750.6 3692.00 3 -3 19 -2 22818.5 3123.66 3 -3 19 -3 23057.8 3312.73 3 -3 20 3 27690.7 3535.45 2 -3 20 2 7204.33 1805.51 2 -3 20 1 2718.55 1225.82 2 -3 20 0 12970.4 2344.78 3 -3 20 -1 31282.2 3489.65 3 -3 20 -2 2260.88 1470.66 3 -3 20 -3 8611.51 2154.12 3 -3 21 3 7364.03 1972.83 2 -3 21 2 55045.9 4909.35 2 -3 21 1 6560.09 1897.38 2 -3 21 0-52.6899 867.888 3 -3 21 -1 9156.01 2185.52 3 -3 21 -2 25170.5 3363.54 3 -3 22 2 3017.33 1486.26 2 -3 22 1 5858.11 1811.00 2 -3 22 0-2589.71 1402.20 3 -3 22 -1 20630.6 3087.32 3 -3 23 0 40.3485 1014.04 2 4 0 -5 4105.65 1642.92 1 4 0 -4 54331.5 4402.60 1 4 0 -3-147.366 1032.89 1 4 0 -2-617.207 897.897 1 -4 0 1 6502.85 1386.51 3 -4 0 0 87314.7 4813.18 3 -4 0 -1-689.297 830.130 3 -4 0 -2 4604.09 1412.71 3 -4 0 -3 4751.25 1680.27 3 -4 0 -4 40661.0 4155.79 3 4 1 -5 75901.5 5717.89 1 4 -1 -5 70522.4 5435.05 1 4 -1 -4 4676.94 1597.58 1 4 1 -4 2422.76 1279.58 1 4 -1 -3-920.366 1109.09 1 4 1 -3 307.394 1002.33 1 4 -1 -2 1994.60 895.234 1 4 1 -2 1824.74 901.603 1 -4 -1 1 96159.4 4454.56 3 -4 1 1 96215.8 4681.82 3 -4 -1 0 12921.0 1993.57 3 -4 1 0 7808.17 1712.59 3 -4 -1 -1 589.794 740.969 3 -4 1 -1-559.900 929.894 3 -4 -1 -2 2298.52 1112.24 3 -4 1 -2 863.092 876.409 3 -4 -1 -3 25171.9 3083.10 3 -4 1 -3 23192.6 2902.31 3 -4 -1 -4 9385.77 2267.50 3 -4 1 -4 10492.3 2450.44 3 4 2 -5 7686.17 2058.86 1 4 -2 -5 5901.03 1897.07 1 4 2 -4 64110.7 4863.88 1 4 -2 -4 54205.9 4490.26 1 4 -2 -3 2046.22 1160.77 1 4 2 -3 3531.87 1253.35 1 4 -2 -2-204.761 739.730 1 -4 2 1 19683.3 2189.00 3 -4 -2 0 86926.8 4532.40 3 -4 2 0 82004.6 4594.82 3 -4 -2 -1 7351.63 1532.20 3 -4 2 -1 4556.24 1403.07 3 -4 -2 -2 1588.39 1009.82 3 -4 2 -2-1543.98 1177.61 3 -4 -2 -3 8591.42 2135.35 3 -4 2 -3 7692.16 1934.67 3 -4 -2 -4 29765.4 3701.37 3 -4 2 -4 30380.3 3658.11 3 4 -3 -5 48867.1 4553.36 1 4 3 -5 45514.4 4472.78 1 4 3 -4 11354.3 2341.31 1 4 -3 -4 11026.7 2225.62 1 4 -3 -3 1343.98 1204.06 1 4 -3 -2 5500.94 1334.44 1 -4 3 1 69797.1 4084.44 3 -4 -3 0 13518.7 1805.95 3 -4 3 0 9857.57 1836.16 3 -4 -3 -1 4454.49 1324.68 3 -4 3 -1 3713.86 1289.27 3 -4 -3 -2 6614.89 1599.47 3 -4 3 -2 7376.85 1750.92 3 -4 -3 -3 23886.6 3009.32 3 -4 3 -3 25732.0 3110.30 3 -4 -3 -4 8559.43 2177.04 3 -4 3 -4 8157.81 2016.70 3 4 4 -5 5194.87 1965.02 1 4 -4 -5 5904.66 1856.01 1 4 -4 -4 28352.1 3261.56 1 4 -4 -3 14983.3 2297.64 1 -4 4 2 8486.18 1421.88 3 4 -4 -2 10453.5 1730.01 1 -4 4 1 19141.6 2216.27 3 -4 -4 0 62016.9 3697.35 3 -4 4 0 65291.3 4168.28 3 -4 -4 -1 16800.2 2133.49 3 -4 4 -1 16354.5 2348.05 3 -4 -4 -2 3965.34 1319.40 3 -4 4 -2 4915.02 1389.24 3 -4 -4 -3 18032.2 2726.73 3 -4 4 -3 18724.4 2820.89 3 -4 -4 -4 16545.5 2760.43 3 -4 4 -4 21747.0 3169.45 3 4 -5 -5 19163.6 3061.79 1 4 -5 -4 18925.6 2801.82 1 -4 5 4 16382.9 2175.29 2 4 -5 -3 26448.1 2882.26 1 -4 5 2 20984.9 2115.80 3 -4 5 1 24613.8 2534.73 3 -4 -5 0 23301.8 2226.20 3 -4 5 0 28448.7 2798.71 3 -4 -5 -1 8069.21 1682.77 3 -4 5 -1 12576.8 2091.36 3 -4 -5 -2 9384.18 1868.81 3 -4 5 -2 7376.99 1822.43 3 -4 5 -3 21997.8 2953.63 3 -4 -5 -3 23115.3 3062.59 3 -4 -5 -4 3292.44 1610.79 3 -4 5 -4 2244.26 1413.05 3 4 -6 -5 5464.36 1947.84 1 -4 6 4 24159.0 2689.81 2 4 -6 -4 24219.4 3064.26 1 4 -6 -3 28061.8 2980.62 1 -4 6 3 25799.3 2767.25 2 -4 6 2 17545.2 2097.73 3 -4 6 1 20732.4 2307.65 3 -4 6 0 13983.1 2064.18 3 -4 6 -1 19940.4 2496.79 3 -4 -6 -1 21150.4 2430.51 3 -4 -6 -2 13241.7 2291.29 3 -4 6 -2 15901.5 2441.29 3 -4 -6 -3 20359.7 2889.64 3 -4 6 -3 18927.8 2859.43 3 -4 -6 -4 8521.15 2105.86 3 -4 6 -4 6106.46 1903.74 3 -4 7 4 34212.7 3248.25 2 -4 7 3 37881.2 3487.76 2 -4 7 2 28507.2 2651.89 3 -4 7 1 10579.5 1846.39 3 -4 7 0 14757.1 2176.81 3 -4 -7 -1 22773.5 2576.38 3 -4 7 -1 22776.0 2702.91 3 -4 -7 -2 10356.6 2113.30 3 -4 7 -2 7477.46 1824.40 3 -4 -7 -3 12166.5 2327.99 3 -4 7 -3 7753.03 1921.98 3 -4 -7 -4 2092.67 1202.86 3 -4 7 -4 2885.44 1372.21 3 -4 8 4 9021.97 1779.27 2 -4 8 3 9753.48 1898.91 2 -4 8 2 40293.4 3216.53 3 -4 8 1 16291.2 2152.33 3 -4 8 0 5232.69 1408.07 3 -4 -8 -1 25460.5 2717.25 3 -4 8 -1 24311.6 2842.30 3 -4 -8 -2 28245.2 3126.17 3 -4 8 -2 30274.2 3327.96 3 -4 -8 -3 8664.56 1966.71 3 -4 8 -3 10351.2 2175.59 3 -4 -8 -4 359.374 1075.21 3 -4 8 -4 1122.32 1423.42 3 -4 9 5 1343.90 917.220 2 -4 9 4 7049.81 1636.79 2 -4 9 3 43894.0 3830.20 2 -4 9 2 15116.4 2106.63 3 -4 9 1 1348.26 1032.79 3 -4 9 0 7917.41 1695.01 3 -4 -9 -1 44767.1 3558.72 3 -4 9 -1 41476.0 3725.03 3 -4 -9 -2 7329.03 1826.90 3 -4 9 -2 5657.89 1821.83 3 -4 -9 -3 3248.81 1453.89 3 -4 9 -3 153.521 1000.07 3 -4 -9 -4-377.751 1257.22 3 -4 10 5 2164.52 1127.00 2 -4 10 4 1259.90 950.012 2 -4 10 3 4759.38 1425.40 2 -4 10 2 68507.7 4450.38 3 -4 10 1 3972.21 1163.46 3 -4 10 0 2952.46 1243.77 3 -4 10 -1 13533.6 2325.81 3 -4 -10 -2 43599.7 3983.00 3 -4 10 -2 44207.9 4060.07 3 -4 -10 -3 449.760 880.539 3 -4 10 -3 1955.73 1492.22 3 -4 -10 -4-1438.60 1300.88 3 -4 11 5 1777.99 982.623 2 -4 11 4 1152.91 1043.46 2 -4 11 3 53432.5 4396.56 2 -4 11 2 4993.44 1418.72 3 -4 11 1 799.738 738.031 3 -4 11 0 2007.21 977.931 3 -4 11 -1 47937.3 4120.89 3 -4 -11 -2 7106.49 2015.31 3 -4 11 -2 8043.05 2156.86 3 -4 -11 -3 409.701 1104.23 3 -4 11 -3 1527.53 1172.71 3 -4 -11 -4-1076.98 1268.74 3 -4 12 5-291.604 554.832 2 -4 12 4 90.0541 809.276 2 -4 12 3 4470.42 1536.23 2 -4 12 2 52238.0 4016.70 3 -4 12 1 246.770 740.233 3 -4 12 0 1383.50 1105.20 3 -4 12 -1 6127.72 1794.53 3 -4 -12 -2 46395.6 4291.08 3 -4 12 -2 54155.0 4620.70 3 -4 -12 -3 1473.51 1045.81 3 -4 12 -3 2333.02 1481.49 3 -4 -12 -4 1128.17 1498.02 3 -4 13 5-215.348 658.775 2 -4 13 4 2436.86 1100.68 2 -4 13 3 45987.1 4200.76 2 -4 13 2 11665.2 2185.75 3 -4 13 1 298.288 1013.65 3 -4 13 0 1520.61 1012.84 3 -4 13 -1 44032.2 4163.51 3 -4 13 -2 7086.42 2015.86 3 -4 -13 -3-713.626 1222.64 3 -4 -13 -4 3858.93 2082.31 3 -4 14 4 559.958 1037.92 2 -4 14 3 4348.70 1526.21 2 -4 14 2 31665.9 3281.88 3 -4 14 1 2740.71 1290.33 3 -4 14 0-1.56339 930.055 3 -4 14 -1 9395.30 2138.67 3 -4 14 -2 32764.8 3795.76 3 -4 -14 -3 4061.69 1840.95 3 -4 15 3 40537.7 4108.60 2 -4 15 2 11606.1 2350.82 2 -4 15 1 1656.00 1231.78 3 -4 15 0 4180.84 1506.46 3 -4 15 -1 18430.9 2793.39 3 -4 -15 -3 3890.63 1666.05 3 -4 16 2 27925.1 3511.59 2 -4 16 1 8844.72 2096.27 3 -4 16 0 3639.61 1416.60 3 -4 16 -1 11061.7 2330.78 3 -4 17 1 8209.47 1916.21 3 -4 17 0 8180.44 2051.84 3 -4 18 1 10979.5 2198.61 3 -5 0 -2 2647.35 1515.15 3 -5 -1 -2 20769.9 2991.29 3 -5 1 -2 20194.4 2984.18 3 -5 2 -1 25002.8 3058.82 3 -5 -2 -2 3137.69 1466.78 3 -5 2 -2 1531.84 1427.59 3 -5 3 -1 1696.29 1230.90 3 -5 3 -2 15722.7 2707.62 3 -5 4 -1 15389.3 2442.94 3 -5 5 -1 7011.35 1681.12 3 -5 6 -1 5233.00 1507.18 3 -5 7 0 8495.94 1959.28 3 -5 7 -1 2872.05 1325.40 3 -5 8 0 6378.03 1808.60 3 -5 9 0 17986.1 2686.40 3 0 0 0 0.00 0.00 0 TITL exp_505 in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 0.71073 3.884019 23.163621 7.035930 90.0000 93.7115 90.0000 ZERR 1.00 0.000319 0.002067 0.000766 0.0000 0.0088 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N O Br Cd UNIT 18.00 10.00 4.00 2.00 2.00 1.00 TREF HKLF 4 END ; _shelx_hkl_checksum 89329 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Cd1 Cd 0.5000 0.0000 0.5000 0.0271(3) Uani 1 2 d S . P Br1 Br 0.97167(17) 0.04210(3) 0.25991(10) 0.0320(3) Uani 1 1 d . . . N1 N 0.5145(14) 0.0909(2) 0.6653(8) 0.0295(14) Uani 1 1 d . . . N2 N 0.5936(18) 0.1901(3) 0.6549(9) 0.0395(17) Uani 1 1 d D . . H21 H 0.66(2) 0.217(2) 0.582(10) 0.047 Uiso 1 1 d D U . O1 O 0.4491(19) 0.2520(3) 0.8883(8) 0.063(2) Uani 1 1 d . . . C1 C 0.6072(19) 0.1375(3) 0.5807(11) 0.0321(17) Uani 1 1 d . . . H1 H 0.6887 0.1340 0.4598 0.039 Uiso 1 1 calc R U . C2 C 0.466(2) 0.2014(4) 0.8311(11) 0.039(2) Uani 1 1 d . . . C3 C 0.367(2) 0.1500(3) 0.9250(11) 0.0365(19) Uani 1 1 d . . . H3 H 0.2817 0.1524 1.0452 0.044 Uiso 1 1 calc R U . C4 C 0.3964(19) 0.0988(3) 0.8429(10) 0.0353(18) Uani 1 1 d . . . H4 H 0.3328 0.0663 0.9100 0.042 Uiso 1 1 calc R U . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0303(4) 0.0221(4) 0.0296(4) -0.0010(3) 0.0078(3) -0.0013(3) Br1 0.0334(4) 0.0339(5) 0.0295(4) 0.0046(3) 0.0076(3) -0.0001(4) N1 0.043(3) 0.021(3) 0.025(3) -0.006(3) 0.009(3) -0.003(3) N2 0.060(5) 0.024(3) 0.037(4) 0.002(3) 0.019(4) -0.003(3) O1 0.110(5) 0.031(3) 0.049(4) -0.020(3) 0.033(4) 0.001(4) C1 0.043(4) 0.022(4) 0.033(4) -0.001(3) 0.011(3) 0.004(4) C2 0.052(5) 0.035(5) 0.032(5) -0.002(4) 0.015(4) 0.003(4) C3 0.049(5) 0.031(4) 0.031(4) -0.001(4) 0.017(4) -0.005(4) C4 0.050(5) 0.034(4) 0.022(4) 0.002(3) 0.008(3) -0.007(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 N1 Cd1 N1 180.0 3_656 . N1 Cd1 Br1 89.49(13) 3_656 3_656 N1 Cd1 Br1 90.51(13) . 3_656 N1 Cd1 Br1 90.51(13) 3_656 . N1 Cd1 Br1 89.49(13) . . Br1 Cd1 Br1 180.0 3_656 . N1 Cd1 Br1 91.15(14) 3_656 1_455 N1 Cd1 Br1 88.85(14) . 1_455 Br1 Cd1 Br1 90.16(2) 3_656 1_455 Br1 Cd1 Br1 89.84(2) . 1_455 N1 Cd1 Br1 88.85(14) 3_656 3_756 N1 Cd1 Br1 91.15(14) . 3_756 Br1 Cd1 Br1 89.84(2) 3_656 3_756 Br1 Cd1 Br1 90.16(2) . 3_756 Br1 Cd1 Br1 180.00(3) 1_455 3_756 Cd1 Br1 Cd1 89.84(2) . 1_655 C1 N1 C4 115.2(6) . . C1 N1 Cd1 120.4(4) . . C4 N1 Cd1 124.0(5) . . C1 N2 C2 123.4(6) . . C1 N2 H21 114(5) . . C2 N2 H21 123(5) . . N1 C1 N2 124.4(6) . . N1 C1 H1 117.8 . . N2 C1 H1 117.8 . . O1 C2 N2 119.8(7) . . O1 C2 C3 128.0(7) . . N2 C2 C3 112.2(7) . . C4 C3 C2 120.8(6) . . C4 C3 H3 119.6 . . C2 C3 H3 119.6 . . C3 C4 N1 124.0(7) . . C3 C4 H4 118.0 . . N1 C4 H4 118.0 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cd1 N1 2.404(6) 3_656 Cd1 N1 2.404(6) . Cd1 Br1 2.7498(7) 3_656 Cd1 Br1 2.7498(7) . Cd1 Br1 2.7507(8) 1_455 Cd1 Br1 2.7507(8) 3_756 Br1 Cd1 2.7508(8) 1_655 N1 C1 1.297(9) . N1 C4 1.371(9) . N2 C1 1.327(9) . N2 C2 1.390(9) . N2 H21 0.85(2) . O1 C2 1.242(10) . C1 H1 0.9300 . C2 C3 1.427(10) . C3 C4 1.327(10) . C3 H3 0.9300 . C4 H4 0.9300 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C1 H1 Br1 0.93 2.81 3.521(7) 133.8 . N2 H21 O1 0.85(2) 1.96(4) 2.750(8) 154(7) 4_665 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 C4 N1 C1 N2 0.0(12) Cd1 N1 C1 N2 173.8(6) C2 N2 C1 N1 -2.3(13) C1 N2 C2 O1 -177.3(9) C1 N2 C2 C3 2.7(12) O1 C2 C3 C4 178.9(9) N2 C2 C3 C4 -1.1(12) C2 C3 C4 N1 -1.0(14) C1 N1 C4 C3 1.6(12) Cd1 N1 C4 C3 -171.9(6)