+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2008/2 for Windows + + Copyright(C) 2008 Bruker-AXS All Rights Reserved + + 2010sl0008 started at 20:06:51 on 23-Dec-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.392 7.477 21.635 90.00 89.97 90.00 13504 Reflections read from file 2010sl0008.hkl; mean (I/sigma) = 2.11 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6751 6761 6720 6738 10116 8982 9009 13504 N (int>3sigma) = 0 1656 1777 1791 1828 2612 2364 2396 3599 Mean intensity = 0.0 13.3 14.3 13.7 14.3 13.8 14.7 15.0 14.5 Mean int/sigma = 0.0 2.2 2.3 2.3 2.3 2.2 2.3 2.3 2.3 Lattice type: P chosen Volume: 1034.05 ------------------------------------------------------------------------------- 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: 6.392 7.477 21.635 90.00 89.97 90.00 Niggli form: a.a = 40.86 b.b = 55.90 c.c = 468.09 b.c = 0.00 a.c = 0.07 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.030 deg. ORTHORHOMBIC P-lattice R(sym) = 0.163 [ 2924] Cell: 6.392 7.477 21.635 90.00 89.97 90.00 Volume: 1034.05 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.132 [ 1826] Cell: 6.392 7.477 21.635 90.00 90.03 90.00 Volume: 1034.05 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.030 deg. MONOCLINIC P-lattice R(sym) = 0.135 [ 1991] Cell: 6.392 21.635 7.477 90.00 90.00 90.03 Volume: 1034.05 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.030 deg. MONOCLINIC P-lattice R(sym) = 0.144 [ 1837] Cell: 7.477 6.392 21.635 90.03 90.00 90.00 Volume: 1034.05 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. TRICLINIC P-lattice R(sym) = 0.000 [ 0] Cell: 6.392 7.477 21.635 90.00 90.03 90.00 Volume: 1034.05 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 Option E selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6751 6761 6720 6738 10116 9009 8982 13504 N (int>3sigma) = 0 1656 1777 1791 1828 2612 2396 2364 3599 Mean intensity = 0.0 13.3 14.3 13.7 14.3 13.8 15.0 14.7 14.5 Mean int/sigma = 0.0 2.2 2.3 2.3 2.3 2.2 2.3 2.3 2.3 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.792 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic 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] P-1 # 2 centro 1 8646 0.000 0 0.0 / 2.3 7.48 [B] P1 # 1 chiral 1 700 0.000 0 0.0 / 2.3 4.83 Option [B] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2010sl0008.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.14 218 224 97.3 4.38 82.5 14.17 0.0470 0.0516 2.14 - 1.71 225 225 100.0 4.55 32.3 12.40 0.1003 0.0686 1.71 - 1.48 230 230 100.0 4.45 21.5 8.33 0.1278 0.0889 1.48 - 1.35 228 228 100.0 4.43 7.8 5.21 0.2612 0.1620 1.35 - 1.25 222 222 100.0 4.44 8.1 4.55 0.2478 0.1772 1.25 - 1.18 238 238 100.0 4.47 9.8 4.65 0.2456 0.1669 1.18 - 1.12 227 227 100.0 3.95 8.0 3.40 0.3129 0.2263 1.12 - 1.06 266 271 98.2 3.42 5.2 2.64 0.3829 0.3405 1.06 - 1.02 243 249 97.6 3.24 5.8 2.66 0.3654 0.3505 1.02 - 0.98 255 269 94.8 2.98 2.8 1.37 0.5912 0.7005 0.98 - 0.94 281 296 94.9 2.64 2.4 1.09 0.6648 0.9569 0.94 - 0.91 259 280 92.5 2.10 1.8 0.68 0.7978 1.4985 0.91 - 0.88 307 342 89.8 1.84 1.6 0.55 0.8260 1.8715 0.88 - 0.86 220 247 89.1 1.75 1.8 0.56 0.7892 1.8432 0.86 - 0.84 218 236 92.4 1.77 1.6 0.45 0.8602 2.3236 0.84 - 0.82 233 286 81.5 1.44 0.9 0.19 1.1841 4.5084 0.82 - 0.80 243 336 72.3 1.18 1.0 0.21 1.2657 4.1861 0.80 - 0.76 233 465 50.1 0.71 0.7 0.16 1.1714 6.7955 ------------------------------------------------------------------------------ 0.86 - 0.76 1045 1455 71.8 1.22 1.1 0.27 1.0527 3.7274 Inf - 0.76 4346 4871 89.2 2.77 10.2 3.35 0.1670 0.2638 Merged [A], lowest resolution = 6.39 Angstroms, 256 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2010sl0008.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C13H8F3N1 Formula weight = 235.20 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.511, non-H atomic volume = 15.2 and following cell contents and analysis: C 52.00 66.38 % H 32.00 3.43 % N 4.00 5.96 % F 12.00 24.23 % F(000) = 480.0 Mo-K(alpha) radiation Mu (mm-1) = 0.13 ------------------------------------------------------------------------------- File 2010sl0008a.ins set up as follows: TITL 2010sl0008a in P1 CELL 0.71073 6.3923 7.4769 21.6354 90.000 90.030 90.000 ZERR 4.00 0.0012 0.0010 0.0042 0.000 0.007 0.000 LATT -1 SFAC C H N F UNIT 52 32 4 12 TEMP 0.05 TREF HKLF 4 END 13504 Reflections written to new reflection file 2010sl0008a.hkl -------------------------------------------------------------------------------