++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh057 started at 18:58:16 on 10-Nov-2010 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.439 10.513 15.163 90.00 90.00 90.00 13328 Reflections read from file 2008lsh057.hkl; mean (I/sigma) = 10.49 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6673 6680 6689 6648 10021 8917 8925 13328 N (int>3sigma) = 0 4543 4348 4401 4516 6646 6108 6169 9159 Mean intensity = 0.0 22.9 17.4 22.3 21.9 20.9 21.9 21.5 21.8 Mean int/sigma = 0.0 10.6 9.8 10.3 10.2 10.2 10.6 10.6 10.6 Lattice type: P chosen Volume: 1504.78 ------------------------------------------------------------------------------- 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: 9.439 10.513 15.163 90.00 90.00 90.00 Niggli form: a.a = 89.10 b.b = 110.53 c.c = 229.93 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) = 0.027 [ 4229] Cell: 9.439 10.513 15.163 90.00 90.00 90.00 Volume: 1504.78 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 6673 6680 6689 6648 10021 8917 8925 13328 N (int>3sigma) = 0 4543 4348 4401 4516 6646 6108 6169 9159 Mean intensity = 0.0 22.9 17.4 22.3 21.9 20.9 21.9 21.5 21.8 Mean int/sigma = 0.0 10.6 9.8 10.3 10.2 10.2 10.6 10.6 10.6 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.966 [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 399 390 391 16 451 457 446 9 266 259 257 15 N I>3s 169 4 169 0 189 1 188 0 99 5 100 0 31.1 0.2 31.7 0.1 20.7 0.2 20.9 0.1 18.7 0.2 19.3 0.2 8.1 0.6 8.2 0.3 6.9 0.6 7.0 0.5 6.9 0.7 7.1 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] Pbca # 61 centro 2 2293 0.027 4229 0.7 / 6.9 1.65 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh057.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 101 110 91.8 5.47 101.7 43.92 0.0212 0.0224 2.20 - 1.70 111 111 100.0 7.63 58.8 52.85 0.0238 0.0129 1.70 - 1.45 118 119 99.2 8.35 29.4 45.53 0.0319 0.0139 1.45 - 1.30 118 118 100.0 8.73 17.2 34.96 0.0346 0.0174 1.30 - 1.20 109 109 100.0 9.01 26.8 36.45 0.0306 0.0168 1.20 - 1.10 159 159 100.0 9.16 23.1 35.82 0.0370 0.0189 1.10 - 1.05 102 102 100.0 9.01 23.9 34.00 0.0394 0.0214 1.05 - 1.00 129 129 100.0 8.81 14.4 27.13 0.0491 0.0235 1.00 - 0.95 138 138 100.0 7.75 9.1 21.19 0.0620 0.0314 0.95 - 0.90 189 189 100.0 6.66 8.9 18.35 0.0718 0.0367 0.90 - 0.85 227 227 100.0 5.22 5.3 12.18 0.0961 0.0573 0.85 - 0.80 278 278 100.0 3.97 4.6 8.97 0.1074 0.0795 0.80 - 0.77 214 215 99.5 3.47 3.3 6.34 0.1537 0.1267 ------------------------------------------------------------------------------ 0.90 - 0.77 719 720 99.9 4.22 4.4 9.20 0.1099 0.0817 Inf - 0.77 1993 2004 99.5 6.65 19.7 24.81 0.0367 0.0248 Merged [A], lowest resolution = 6.37 Angstroms, 435 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh057.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H8F1N1O1 Formula weight = 153.15 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.352, non-H atomic volume = 17.1 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 10.5132 9.4393 15.1635 90.000 90.000 90.000 ZERR 8.00 0.0004 0.0003 0.0005 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 0.5 TREF HKLF 4 END 13328 Reflections written to new reflection file Pbca.hkl -------------------------------------------------------------------------------