+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2008/2 for Windows + + Copyright(C) 2008 Bruker-AXS All Rights Reserved + + 2008lsh060 started at 20:42:31 on 30-Oct-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 4.767 18.498 18.632 90.00 90.00 90.00 61277 Reflections read from file 2008lsh060.hkl; mean (I/sigma) = 8.12 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 30682 30571 30597 30711 45925 40848 40858 61277 N (int>3sigma) = 0 22758 22514 22796 22929 34034 30360 30339 45634 Mean intensity = 0.0 25.6 26.2 24.9 25.9 25.6 26.0 25.9 25.6 Mean int/sigma = 0.0 8.1 8.1 8.2 8.2 8.1 8.2 8.2 8.2 Lattice type: P chosen Volume: 1642.88 ------------------------------------------------------------------------------- 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: 4.767 18.498 18.632 90.00 90.00 90.00 Niggli form: a.a = 22.72 b.b = 342.19 c.c = 347.14 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 = 0.206 deg. TETRAGONAL P-lattice R(sym) = 0.537 [ 5393] Cell: 18.498 18.632 4.767 90.00 90.00 90.00 Volume: 1642.88 Matrix: 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(sym) = 0.020 [ 5283] Cell: 4.767 18.498 18.632 90.00 90.00 90.00 Volume: 1642.88 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 30682 30571 30597 30711 45925 40848 40858 61277 N (int>3sigma) = 0 22758 22514 22796 22929 34034 30360 30339 45634 Mean intensity = 0.0 25.6 26.2 24.9 25.9 25.6 26.0 25.9 25.6 Mean int/sigma = 0.0 8.1 8.1 8.2 8.2 8.1 8.2 8.2 8.2 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.756 [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 4039 4039 4056 25 981 1009 982 110 972 968 990 92 N I>3s 2768 2676 2748 0 589 700 591 0 737 643 612 0 34.2 27.1 37.1 0.3 36.3 41.0 34.4 0.3 42.6 33.5 16.8 0.2 8.2 7.9 8.4 0.6 7.8 8.3 7.7 0.4 8.9 7.5 6.8 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(1) # 19 chiral 1 5917 0.020 5283 0.6 / 6.8 1.63 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh060.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.26 114 121 94.2 24.98 141.3 78.96 0.0305 0.0120 2.26 - 1.75 115 115 100.0 33.67 72.0 98.47 0.0312 0.0092 1.75 - 1.51 118 118 100.0 33.96 40.4 80.76 0.0376 0.0097 1.51 - 1.37 113 113 100.0 35.73 31.2 69.74 0.0438 0.0112 1.37 - 1.25 122 122 100.0 37.30 26.6 62.15 0.0536 0.0139 1.25 - 1.17 116 116 100.0 35.34 25.3 56.61 0.0565 0.0149 1.17 - 1.11 123 123 100.0 36.21 22.4 52.55 0.0637 0.0167 1.11 - 1.06 117 117 100.0 36.26 14.7 43.43 0.0789 0.0185 1.06 - 1.01 132 132 100.0 35.61 12.2 37.46 0.0901 0.0207 1.01 - 0.97 121 121 100.0 31.44 7.4 29.21 0.1180 0.0273 0.97 - 0.94 115 115 100.0 27.80 8.9 28.34 0.1148 0.0280 0.94 - 0.91 134 134 100.0 25.78 5.6 21.19 0.1567 0.0372 0.91 - 0.88 148 148 100.0 22.97 6.0 19.54 0.1651 0.0414 0.88 - 0.85 163 163 100.0 19.75 5.5 15.69 0.1851 0.0499 0.85 - 0.83 124 124 100.0 16.58 5.1 13.43 0.1854 0.0585 0.83 - 0.81 116 116 100.0 15.57 3.6 10.50 0.2654 0.0815 0.81 - 0.79 164 164 100.0 14.18 3.5 9.21 0.2618 0.0909 0.79 - 0.77 85 92 92.4 11.16 2.7 6.79 0.2951 0.1528 ------------------------------------------------------------------------------ 0.86 - 0.77 599 606 98.8 15.45 4.0 10.94 0.2263 0.0780 Inf - 0.77 2240 2254 99.4 27.19 22.9 39.48 0.0533 0.0171 Merged [A], lowest resolution = 6.56 Angstroms, 2812 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh060.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H8Cl1N1O1 Formula weight = 169.61 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.371, non-H atomic volume = 18.7 and following cell contents and analysis: C 64.00 56.65 % H 64.00 4.75 % N 8.00 8.26 % O 8.00 9.43 % Cl 8.00 20.90 % F(000) = 704.0 Mo-K(alpha) radiation Mu (mm-1) = 0.40 ------------------------------------------------------------------------------- File 2008lsh060.ins set up as follows: TITL 2008lsh060 in P2(1)2(1)2(1) CELL 0.71073 4.7667 18.4984 18.6318 90.000 90.000 90.000 ZERR 8.00 0.0001 0.0004 0.0004 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 CL UNIT 64 64 8 8 8 TEMP 0.1 TREF HKLF 4 END -------------------------------------------------------------------------------