++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh029 started at 23:29:28 on 12-Nov-2010 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.502 12.177 12.964 90.00 90.00 90.00 10311 Reflections read from file 2008lsh029.hkl; mean (I/sigma) = 10.56 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5139 5157 5150 5189 7723 6855 6878 10311 N (int>3sigma) = 0 3616 3547 3643 3764 5403 4978 5013 7486 Mean intensity = 0.0 10.0 9.1 9.3 9.4 9.5 9.4 9.5 9.3 Mean int/sigma = 0.0 10.3 10.3 10.5 10.6 10.3 10.7 10.7 10.6 Lattice type: P chosen Volume: 1500.00 ------------------------------------------------------------------------------- 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: 9.502 12.177 12.964 90.00 90.00 90.00 Niggli form: a.a = 90.30 b.b = 148.27 c.c = 168.06 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) = 0.024 [ 3068] Cell: 9.502 12.177 12.964 90.00 90.00 90.00 Volume: 1500.00 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 5139 5157 5150 5189 7723 6855 6878 10311 N (int>3sigma) = 0 3616 3547 3643 3764 5403 4978 5013 7486 Mean intensity = 0.0 10.0 9.1 9.3 9.4 9.5 9.4 9.5 9.3 Mean int/sigma = 0.0 10.3 10.3 10.5 10.6 10.3 10.7 10.7 10.6 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.938 [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 377 356 379 7 226 214 222 13 247 228 239 12 N I>3s 159 1 160 0 79 0 79 0 115 1 116 1 19.5 0.1 19.4 0.0 8.2 0.1 8.3 0.1 9.0 0.1 9.3 0.4 6.8 0.6 6.8 0.6 5.2 0.6 5.3 0.9 8.5 0.6 8.7 1.3 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] Pbca # 61 centro 2 2293 0.024 3068 1.3 / 5.2 2.32 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh029.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 100 109 91.7 5.80 43.7 38.19 0.0171 0.0240 2.20 - 1.70 112 112 100.0 7.27 20.6 42.67 0.0202 0.0160 1.70 - 1.45 114 114 100.0 7.90 15.2 44.10 0.0270 0.0171 1.45 - 1.30 122 122 100.0 7.73 5.5 31.27 0.0407 0.0200 1.30 - 1.20 105 105 100.0 7.70 7.8 32.79 0.0343 0.0199 1.20 - 1.10 167 167 100.0 6.95 7.9 28.53 0.0413 0.0254 1.10 - 1.00 217 217 100.0 6.14 5.9 23.34 0.0445 0.0294 1.00 - 0.95 147 147 100.0 5.39 3.5 18.16 0.0580 0.0377 0.95 - 0.90 183 183 100.0 4.61 2.4 14.01 0.0685 0.0506 0.90 - 0.85 230 232 99.1 3.83 1.8 10.42 0.0840 0.0750 0.85 - 0.80 269 276 97.5 2.75 1.5 7.43 0.1051 0.1135 0.80 - 0.77 199 207 96.1 2.11 1.1 4.77 0.1418 0.1770 ------------------------------------------------------------------------------ 0.90 - 0.77 698 715 97.6 2.91 1.5 7.66 0.0978 0.1111 Inf - 0.77 1965 1991 98.7 5.18 7.4 21.01 0.0322 0.0295 Merged [A], lowest resolution = 6.49 Angstroms, 259 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh029.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8 H8 F1 N1 O1 Formula weight = 153.15 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.356, non-H atomic volume = 17.0 and following cell contents and analysis: C 64.00 62.73 % H 64.00 5.27 % N 8.00 9.15 % O 8.00 10.45 % F 8.00 12.41 % F(000) = 640.0 Mo-K(alpha) radiation Mu (mm-1) = 0.11 ------------------------------------------------------------------------------- File Pbca.ins set up as follows: TITL Pbca in Pbca CELL 0.71073 12.1766 9.5024 12.9638 90.000 90.000 90.000 ZERR 8.00 0.0004 0.0003 0.0003 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 O F UNIT 64 64 8 8 8 TEMP file. TREF HKLF 4 END 10311 Reflections written to new reflection file Pbca.hkl -------------------------------------------------------------------------------