+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2008/2 for Windows + + Copyright(C) 2008 Bruker-AXS All Rights Reserved + + 2010sl0006 started at 18:41:07 on 23-Dec-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.465 7.619 21.290 90.00 90.00 90.00 10253 Reflections read from file 2010sl0006.hkl; mean (I/sigma) = 3.55 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5121 5138 5113 5104 7686 6849 6845 10253 N (int>3sigma) = 0 2315 2260 2391 2295 3483 3156 3126 4723 Mean intensity = 0.0 14.6 14.9 15.1 14.7 14.8 15.5 15.7 15.4 Mean int/sigma = 0.0 3.6 3.5 3.7 3.5 3.6 3.6 3.6 3.6 Lattice type: P chosen Volume: 1048.61 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 6.465 7.619 21.290 90.00 90.00 90.00 Niggli form: a.a = 41.79 b.b = 58.04 c.c = 453.25 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(sym) = 0.090 [ 3114] Cell: 6.465 7.619 21.290 90.00 90.00 90.00 Volume: 1048.61 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5121 5138 5113 5104 7686 6849 6845 10253 N (int>3sigma) = 0 2315 2260 2391 2295 3483 3156 3126 4723 Mean intensity = 0.0 14.6 14.9 15.1 14.7 14.8 15.5 15.7 15.4 Mean int/sigma = 0.0 3.6 3.5 3.7 3.5 3.6 3.6 3.6 3.6 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.795 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 423 421 422 14 483 494 485 7 157 151 152 30 N I>3s 202 165 183 0 215 222 191 0 75 71 78 0 12.4 17.0 18.8 0.4 16.2 21.1 15.2 0.3 22.1 28.2 15.4 0.8 3.9 3.1 3.7 0.6 3.7 3.9 3.3 0.4 4.0 4.3 3.8 0.6 Identical indices and Friedel opposites combined before calculating R(sym) Option Space Group No. Type Axes CSD R(sym) N(eq) Syst. Abs. CFOM [A] P2(1)2(1)2(1) # 19 chiral 1 5917 0.090 3114 0.6 / 3.1 3.84 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2010sl0006.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.25 73 79 92.4 7.38 79.9 24.69 0.0375 0.0317 2.25 - 1.77 73 73 100.0 9.21 34.1 25.02 0.0628 0.0342 1.77 - 1.52 73 73 100.0 9.63 26.3 19.63 0.0816 0.0383 1.52 - 1.37 75 75 100.0 9.60 14.0 14.24 0.1193 0.0536 1.37 - 1.25 80 80 100.0 9.61 11.5 12.68 0.1418 0.0647 1.25 - 1.18 75 75 100.0 10.36 13.7 12.44 0.1360 0.0591 1.18 - 1.11 74 74 100.0 10.05 13.5 11.93 0.1489 0.0675 1.11 - 1.06 80 80 100.0 9.05 8.0 8.49 0.2102 0.0904 1.06 - 1.01 86 86 100.0 8.66 10.0 9.61 0.1843 0.0894 1.01 - 0.97 81 81 100.0 7.85 4.6 5.62 0.3060 0.1462 0.97 - 0.93 96 96 100.0 7.00 3.4 4.32 0.3639 0.2023 0.93 - 0.90 96 96 100.0 5.91 2.3 2.45 0.4787 0.3388 0.90 - 0.87 93 93 100.0 4.94 3.4 2.90 0.3690 0.3068 0.87 - 0.84 110 110 100.0 4.26 1.9 1.73 0.5796 0.5643 0.84 - 0.82 82 82 100.0 4.15 1.5 1.35 0.5923 0.7583 0.82 - 0.80 90 90 100.0 3.79 1.5 1.03 0.6513 0.9036 0.80 - 0.78 97 98 99.0 3.35 1.4 1.01 0.6468 0.9881 0.78 - 0.77 3 17 17.6 0.24 0.2 0.09 0.0084 11.9096 ------------------------------------------------------------------------------ 0.87 - 0.77 416 431 96.5 3.82 1.7 1.41 0.5762 0.7289 Inf - 0.77 1437 1458 98.6 7.03 12.2 8.58 0.1135 0.0850 Merged [A], lowest resolution = 6.46 Angstroms, 368 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2010sl0006.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C13H5F4N Formula weight = 251.18 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.591, non-H atomic volume = 14.6 and following cell contents and analysis: C 52.00 62.16 % H 20.00 2.01 % N 4.00 5.58 % F 16.00 30.25 % F(000) = 504.0 Mo-K(alpha) radiation Mu (mm-1) = 0.14 ------------------------------------------------------------------------------- File 2010sl0006a.ins set up as follows: TITL 2010sl0006a in P2(1)2(1)2(1) CELL 0.71073 6.4649 7.6187 21.2897 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0004 0.0013 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N F UNIT 52 20 4 16 TEMP 0.08 TREF HKLF 4 END 10253 Reflections written to new reflection file 2010sl0006a.hkl -------------------------------------------------------------------------------