++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh024 started at 14:18:57 on 06-Jul-2008 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.239 8.594 9.190 90.00 90.00 90.00 5685 Reflections read from file 2008lsh024.hkl; mean (I/sigma) = 15.76 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2819 2825 2836 2882 4240 3789 3794 5685 N (int>3sigma) = 0 2344 2365 2397 2458 3553 3250 3267 4907 Mean intensity = 0.0 326.8 334.1 168.8 270.5 276.4 297.3 304.2 329.6 Mean int/sigma = 0.0 15.2 15.4 14.8 16.0 15.1 15.7 15.7 15.8 Lattice type: P chosen Volume: 571.69 ------------------------------------------------------------------------------- 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: 7.239 8.594 9.190 90.00 90.00 90.00 Niggli form: a.a = 52.40 b.b = 73.85 c.c = 84.45 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) = 0.016 [ 1652] Cell: 7.239 8.594 9.190 90.00 90.00 90.00 Volume: 571.69 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 2819 2825 2836 2882 4240 3789 3794 5685 N (int>3sigma) = 0 2344 2365 2397 2458 3553 3250 3267 4907 Mean intensity = 0.0 326.8 334.1 168.8 270.5 276.4 297.3 304.2 329.6 Mean int/sigma = 0.0 15.2 15.4 14.8 16.0 15.1 15.7 15.7 15.8 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.929 [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 239 235 234 11 203 198 175 15 215 193 208 8 N I>3s 205 213 204 0 113 113 0 0 104 0 104 0 198.1 446.4 488.7 1.4 179.2 183.7 1.1 0.3 253.7 0.8 262.1 0.5 18.3 18.3 19.5 0.7 11.2 11.5 0.7 0.3 11.0 0.6 11.3 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] Pna2(1) # 33 non-cen 3 903 0.016 1652 0.7 / 11.0 4.81 [B] Pnma # 62 centro 2 894 0.016 1652 0.7 / 11.0 1.23 Option [B] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh024.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.25 41 45 91.1 6.73 1248.6 49.42 0.0181 0.0249 2.25 - 1.70 48 48 100.0 9.94 645.4 70.26 0.0186 0.0123 1.70 - 1.45 44 44 100.0 10.27 541.4 64.24 0.0210 0.0124 1.45 - 1.30 50 50 100.0 10.44 390.2 62.54 0.0220 0.0131 1.30 - 1.20 46 46 100.0 9.91 324.0 49.69 0.0279 0.0164 1.20 - 1.10 65 65 100.0 9.57 353.8 47.95 0.0209 0.0146 1.10 - 1.00 94 94 100.0 8.12 229.8 41.46 0.0281 0.0171 1.00 - 0.95 53 53 100.0 7.40 127.4 32.67 0.0418 0.0222 0.95 - 0.90 67 67 100.0 6.58 141.4 29.23 0.0402 0.0249 0.90 - 0.85 94 94 100.0 5.11 179.2 24.38 0.0373 0.0300 0.85 - 0.80 110 110 100.0 4.45 141.2 21.25 0.0412 0.0375 0.80 - 0.77 83 84 98.8 3.42 71.9 14.57 0.0604 0.0503 ------------------------------------------------------------------------------ 0.90 - 0.77 287 288 99.7 4.36 133.6 20.34 0.0420 0.0362 Inf - 0.77 795 800 99.4 7.11 301.4 37.96 0.0249 0.0206 Merged [A], lowest resolution = 6.28 Angstroms, 210 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh024.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C7H7Cl1N2O1 Formula weight = 170.60 Tentative Z (number of formula units/cell) = 3.0 giving rho = 1.487, non-H atomic volume = 17.3 and following cell contents and analysis: C 21.00 49.28 % H 21.00 4.14 % N 6.00 16.42 % O 3.00 9.38 % Cl 3.00 20.78 % F(000) = 264.0 Mo-K(alpha) radiation Mu (mm-1) = 0.44 ------------------------------------------------------------------------------- File pnma.ins set up as follows: TITL pnma in Pnma CELL 0.71073 8.5936 7.2391 9.1897 90.000 90.000 90.000 ZERR 3.00 0.0002 0.0002 0.0003 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, -Z SYMM 0.5+X, 0.5-Y, 0.5-Z SFAC C H N O CL UNIT 21 21 6 3 3 TEMP 0.12 TREF HKLF 4 END -------------------------------------------------------------------------------