++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh050 started at 15:08:23 on 21-Jul-2008 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.666 9.254 10.596 90.00 90.00 90.00 7319 Reflections read from file 2008lsh050.hkl; mean (I/sigma) = 15.36 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3664 3632 3674 3686 5485 4869 4885 7319 N (int>3sigma) = 0 3030 2906 3010 2951 4473 4065 4086 6117 Mean intensity = 0.0 58.5 55.4 58.4 49.8 57.4 61.2 60.2 59.9 Mean int/sigma = 0.0 15.3 14.6 14.9 14.0 14.9 15.5 15.4 15.4 Lattice type: P chosen Volume: 751.65 ------------------------------------------------------------------------------- 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: 7.666 9.254 10.596 90.00 90.00 90.00 Niggli form: a.a = 58.76 b.b = 85.64 c.c = 112.27 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) = 0.020 [ 2132] Cell: 7.666 9.254 10.596 90.00 90.00 90.00 Volume: 751.65 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 3664 3632 3674 3686 5485 4869 4885 7319 N (int>3sigma) = 0 3030 2906 3010 2951 4473 4065 4086 6117 Mean intensity = 0.0 58.5 55.4 58.4 49.8 57.4 61.2 60.2 59.9 Mean int/sigma = 0.0 15.3 14.6 14.9 14.0 14.9 15.5 15.4 15.4 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.720 [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 337 340 337 8 271 265 266 12 172 177 175 21 N I>3s 141 2 139 0 219 209 202 0 78 79 1 0 46.7 0.2 46.7 0.5 65.6 67.9 49.6 0.1 49.1 47.8 0.4 0.2 9.3 0.6 9.2 0.8 14.8 15.4 13.8 0.5 10.8 10.5 0.6 0.4 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 5 903 0.020 2132 0.8 / 9.2 1.29 [B] Pnma # 62 centro 4 894 0.020 2132 0.8 / 9.2 7.41 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh050.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 55 61 90.2 6.23 188.1 66.38 0.0177 0.0146 2.20 - 1.70 59 59 100.0 8.56 151.0 81.06 0.0205 0.0092 1.70 - 1.45 61 61 100.0 8.82 85.3 69.11 0.0238 0.0107 1.45 - 1.30 60 60 100.0 9.43 60.2 61.49 0.0291 0.0126 1.30 - 1.20 59 59 100.0 9.49 59.2 55.08 0.0291 0.0139 1.20 - 1.10 78 78 100.0 9.47 77.4 53.19 0.0285 0.0159 1.10 - 1.05 57 57 100.0 9.09 33.6 38.94 0.0382 0.0206 1.05 - 1.00 61 61 100.0 9.15 46.0 38.36 0.0369 0.0198 1.00 - 0.95 80 80 100.0 8.39 28.6 30.60 0.0493 0.0252 0.95 - 0.90 93 93 100.0 7.41 24.0 24.83 0.0611 0.0351 0.90 - 0.85 112 112 100.0 5.89 17.3 19.62 0.0666 0.0395 0.85 - 0.80 147 147 100.0 4.25 12.9 12.84 0.0853 0.0614 0.80 - 0.77 99 100 99.0 3.10 12.4 10.22 0.0764 0.0799 ------------------------------------------------------------------------------ 0.90 - 0.77 358 359 99.7 4.44 14.1 14.24 0.0746 0.0575 Inf - 0.77 1021 1028 99.3 7.12 50.8 37.37 0.0301 0.0193 Merged [A], lowest resolution = 6.97 Angstroms, 267 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh050.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H9N1O2 Formula weight = 151.16 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.336, non-H atomic volume = 17.1 and following cell contents and analysis: C 32.00 63.56 % H 36.00 6.00 % N 4.00 9.27 % O 8.00 21.17 % F(000) = 320.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File pna21.ins set up as follows: TITL pna21 in Pna2(1) CELL 0.71073 10.5957 7.6655 9.2544 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0003 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 UNIT 32 36 4 8 TEMP 0.4 TREF HKLF 4 END -------------------------------------------------------------------------------