+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2008/2 for Windows + + Copyright(C) 2008 Bruker-AXS All Rights Reserved + + 2008lsh140 started at 18:01:24 on 27-Nov-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 4.603 9.590 14.534 90.00 90.00 90.00 6289 Reflections read from file 2008lsh140.hkl; mean (I/sigma) = 6.81 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3150 3183 3129 3152 4731 4209 4188 6289 N (int>3sigma) = 0 2128 2168 2220 2220 3258 2984 2973 4424 Mean intensity = 0.0 25.4 24.9 27.6 25.6 26.0 25.8 26.2 26.3 Mean int/sigma = 0.0 6.7 6.8 7.0 7.0 6.8 6.8 6.8 6.8 Lattice type: P chosen Volume: 641.52 ------------------------------------------------------------------------------- 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: 4.603 9.590 14.534 90.00 90.00 90.00 Niggli form: a.a = 21.19 b.b = 91.97 c.c = 211.23 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) = 0.041 [ 1904] Cell: 4.603 9.590 14.534 90.00 90.00 90.00 Volume: 641.52 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 3150 3183 3129 3152 4731 4209 4188 6289 N (int>3sigma) = 0 2128 2168 2220 2220 3258 2984 2973 4424 Mean intensity = 0.0 25.4 24.9 27.6 25.6 26.0 25.8 26.2 26.3 Mean int/sigma = 0.0 6.7 6.8 7.0 7.0 6.8 6.8 6.8 6.8 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.775 [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 411 414 413 5 220 223 223 11 122 117 117 28 N I>3s 284 266 240 5 133 169 126 0 73 50 61 0 35.9 40.8 30.2 44.1 26.2 44.8 32.9 0.5 68.7 46.6 60.9 0.3 7.5 6.9 6.2 12.1 6.6 8.4 6.6 0.8 7.4 6.1 6.3 0.5 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 # 18 chiral 3 359 0.041 1904 0.8 / 6.1 2.12 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh140.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.28 46 50 92.0 5.82 161.3 31.53 0.0237 0.0285 2.28 - 1.79 46 46 100.0 8.24 89.1 38.40 0.0288 0.0222 1.79 - 1.52 46 46 100.0 8.50 33.7 32.53 0.0421 0.0259 1.52 - 1.38 46 46 100.0 8.85 23.6 28.06 0.0544 0.0276 1.38 - 1.27 50 50 100.0 8.86 18.3 23.64 0.0733 0.0345 1.27 - 1.17 52 52 100.0 9.35 33.5 26.39 0.0530 0.0299 1.17 - 1.11 50 50 100.0 8.56 25.1 23.48 0.0606 0.0365 1.11 - 1.06 48 48 100.0 8.75 11.3 15.96 0.1054 0.0482 1.06 - 1.01 57 57 100.0 8.65 21.3 18.93 0.0829 0.0441 1.01 - 0.96 59 59 100.0 8.61 9.6 14.71 0.1162 0.0579 0.96 - 0.93 47 47 100.0 8.09 8.9 11.92 0.1446 0.0712 0.93 - 0.90 55 55 100.0 6.29 5.5 9.04 0.1874 0.1020 0.90 - 0.88 46 46 100.0 6.04 6.8 9.09 0.1631 0.0950 0.88 - 0.85 67 67 100.0 5.28 6.1 6.86 0.2038 0.1147 0.85 - 0.82 70 70 100.0 4.29 4.3 5.06 0.2286 0.1611 0.82 - 0.80 57 57 100.0 3.37 3.5 3.84 0.2725 0.2535 0.80 - 0.78 60 61 98.4 3.07 4.3 3.85 0.2112 0.2164 0.78 - 0.77 5 6 83.3 1.00 2.4 1.80 0.0332 0.5462 ------------------------------------------------------------------------------ 0.86 - 0.77 243 245 99.2 3.88 4.5 4.66 0.2247 0.1826 Inf - 0.77 907 913 99.3 6.89 24.9 16.75 0.0554 0.0403 Merged [A], lowest resolution = 5.79 Angstroms, 217 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh140.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C10H13N1O2 Formula weight = 179.22 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.856, non-H atomic volume = 12.3 and following cell contents and analysis: C 40.00 67.02 % H 52.00 7.31 % N 4.00 7.82 % O 8.00 17.85 % F(000) = 384.0 Mo-K(alpha) radiation Mu (mm-1) = 0.13 ------------------------------------------------------------------------------- File p21212.ins set up as follows: TITL p21212 in P2(1)2(1)2 CELL 0.71073 9.5899 14.5337 4.6028 90.000 90.000 90.000 ZERR 4.00 0.0010 0.0014 0.0003 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, Z SYMM 0.5-X, 0.5+Y, -Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O UNIT 40 52 4 8 TEMP 0.06 TREF HKLF 4 END 6289 Reflections written to new reflection file p21212.hkl -------------------------------------------------------------------------------