++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh006 started at 17:26:35 on 17-Nov-2010 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.576 9.698 12.387 90.00 90.00 90.00 8699 Reflections read from file 2008lsh006.hkl; mean (I/sigma) = 9.24 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4367 4380 4337 4361 6542 5802 5822 8699 N (int>3sigma) = 0 2926 2143 2937 3087 4003 4011 4038 6034 Mean intensity = 0.0 25.9 2.9 26.2 26.3 18.3 25.4 25.4 25.6 Mean int/sigma = 0.0 9.3 4.2 9.4 9.5 7.6 9.3 9.4 9.3 Lattice type: P chosen Volume: 789.94 ------------------------------------------------------------------------------- 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: 6.576 9.698 12.387 90.00 90.00 90.00 Niggli form: a.a = 43.24 b.b = 94.05 c.c = 153.45 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) = 0.027 [ 2262] Cell: 6.576 9.698 12.387 90.00 90.00 90.00 Volume: 789.94 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 4367 4380 4337 4361 6542 5802 5822 8699 N (int>3sigma) = 0 2926 2143 2937 3087 4003 4011 4038 6034 Mean intensity = 0.0 25.9 2.9 26.2 26.3 18.3 25.4 25.4 25.6 Mean int/sigma = 0.0 9.3 4.2 9.4 9.5 7.6 9.3 9.4 9.3 Crystal system O and Lattice type P selected Mean |E*E-1| = 1.078 [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 391 398 401 10 303 298 299 11 197 203 200 24 N I>3s 241 203 262 0 145 145 0 0 73 0 73 0 25.3 4.1 25.7 0.0 37.9 38.5 0.1 0.2 5.4 0.1 5.3 0.1 8.9 5.0 9.6 0.3 8.7 8.9 0.4 0.5 4.1 0.5 4.0 0.3 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 0.027 2262 0.5 / 4.0 14.65 [B] Pnma # 62 centro 2 894 0.027 2262 0.5 / 4.0 4.16 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh006.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.25 56 60 93.3 7.35 88.1 39.89 0.0259 0.0181 2.25 - 1.70 61 61 100.0 9.64 69.2 50.92 0.0227 0.0120 1.70 - 1.50 56 56 100.0 9.91 48.5 45.28 0.0357 0.0172 1.50 - 1.30 76 76 100.0 10.32 26.5 40.38 0.0359 0.0144 1.30 - 1.20 63 63 100.0 10.40 27.5 35.81 0.0376 0.0179 1.20 - 1.10 84 84 100.0 10.95 30.4 37.06 0.0413 0.0185 1.10 - 1.05 58 58 100.0 9.93 19.4 24.15 0.0460 0.0227 1.05 - 1.00 67 67 100.0 10.45 15.3 21.84 0.0517 0.0282 1.00 - 0.95 76 76 100.0 9.13 16.1 20.98 0.0606 0.0305 0.95 - 0.90 101 101 100.0 7.60 10.8 16.87 0.0684 0.0397 0.90 - 0.85 126 126 100.0 6.47 10.5 13.68 0.0819 0.0464 0.85 - 0.80 158 158 100.0 4.70 7.6 8.79 0.0935 0.0700 0.80 - 0.77 114 118 96.6 3.91 7.6 7.98 0.0936 0.0798 ------------------------------------------------------------------------------ 0.90 - 0.77 398 402 99.0 5.02 8.5 10.10 0.0879 0.0633 Inf - 0.77 1096 1104 99.3 7.88 23.7 24.18 0.0401 0.0247 Merged [A], lowest resolution = 6.58 Angstroms, 358 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh006.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H8Cl1N1O1 Formula weight = 169.60 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.426, non-H atomic volume = 18.0 and following cell contents and analysis: C 32.00 56.65 % H 32.00 4.75 % N 4.00 8.26 % O 4.00 9.43 % Cl 4.00 20.90 % F(000) = 352.0 Mo-K(alpha) radiation Mu (mm-1) = 0.42 ------------------------------------------------------------------------------- File pna21.ins set up as follows: TITL pna21 in Pna2(1) CELL 0.71073 9.6978 12.3874 6.5757 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0004 0.0002 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, 0.5-Y, Z SYMM 0.5-X, 0.5+Y, 0.5+Z SFAC C H N O CL UNIT 32 32 4 4 4 TEMP 0.1 TREF HKLF 4 END 8699 Reflections written to new reflection file pna21.hkl -------------------------------------------------------------------------------