++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh166 started at 13:02:21 on 06-Jan-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 4.782 13.417 13.979 90.00 92.53 90.00 11785 Reflections read from file 2008lsh166.hkl; mean (I/sigma) = 4.74 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5881 5885 5914 5911 8840 7875 7833 11785 N (int>3sigma) = 0 3255 3074 3111 3095 4720 4269 4201 6361 Mean intensity = 0.0 14.2 11.4 13.8 12.6 13.1 13.6 13.8 13.2 Mean int/sigma = 0.0 4.9 4.7 4.7 4.7 4.8 4.8 4.8 4.8 Lattice type: P chosen Volume: 896.06 ------------------------------------------------------------------------------- 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: 4.782 13.417 13.979 90.00 92.53 90.00 Niggli form: a.a = 22.87 b.b = 180.02 c.c = 195.42 b.c = 0.00 a.c = -2.95 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. MONOCLINIC P-lattice R(sym) = 0.057 [ 1762] Cell: 4.782 13.417 13.979 90.00 92.53 90.00 Volume: 896.06 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 5881 5885 5914 5911 8840 7875 7833 11785 N (int>3sigma) = 0 3255 3074 3111 3095 4720 4269 4201 6361 Mean intensity = 0.0 14.2 11.4 13.8 12.6 13.1 13.6 13.8 13.2 Mean int/sigma = 0.0 4.9 4.7 4.7 4.7 4.8 4.8 4.8 4.8 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.961 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 22 321 312 323 N I>3s 1 100 102 2 0.4 36.5 37.6 0.4 0.7 3.0 3.1 0.7 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)/n # 14 centro 1 19410 0.057 1762 0.7 / 3.0 4.27 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh166.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.10 115 118 97.5 6.34 74.7 23.19 0.0737 0.0434 2.10 - 1.65 110 110 100.0 7.35 30.0 25.35 0.0567 0.0304 1.65 - 1.45 112 112 100.0 7.26 16.7 21.16 0.0619 0.0348 1.45 - 1.30 123 123 100.0 7.37 13.2 18.18 0.0777 0.0518 1.30 - 1.20 113 113 100.0 7.38 13.9 15.51 0.0760 0.0445 1.20 - 1.10 183 183 100.0 7.17 9.3 14.42 0.0955 0.0510 1.10 - 1.05 113 113 100.0 7.05 8.7 12.26 0.1026 0.0571 1.05 - 1.00 123 123 100.0 7.06 7.2 11.34 0.1311 0.0632 1.00 - 0.95 151 151 100.0 6.18 4.2 7.49 0.1714 0.0971 0.95 - 0.90 220 220 100.0 5.46 5.3 6.75 0.2208 0.2416 0.90 - 0.85 251 252 99.6 4.38 2.2 4.29 0.3254 0.1948 0.85 - 0.80 292 294 99.3 3.16 1.6 2.48 0.4385 0.3816 0.80 - 0.77 244 266 91.7 2.00 1.6 1.89 0.4811 0.5219 ------------------------------------------------------------------------------ 0.90 - 0.77 787 812 96.9 3.16 1.8 2.87 0.3821 0.3468 Inf - 0.77 2150 2178 98.7 5.41 11.0 10.29 0.0914 0.0725 Merged [A], lowest resolution = 6.98 Angstroms, 367 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh166.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C9H8F3N1O1 Formula weight = 203.16 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.506, non-H atomic volume = 16.0 and following cell contents and analysis: C 36.00 53.20 % H 32.00 3.97 % N 4.00 6.90 % O 4.00 7.88 % F 12.00 28.06 % F(000) = 416.0 Mo-K(alpha) radiation Mu (mm-1) = 0.14 ------------------------------------------------------------------------------- File 2008lsh166.ins set up as follows: TITL 2008lsh166 in P2(1)/n CELL 0.71073 4.7821 13.4170 13.9793 90.000 92.527 90.000 ZERR 4.00 0.0004 0.0016 0.0015 0.000 0.007 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O F UNIT 36 32 4 4 12 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------