++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh045 started at 17:07:12 on 18-Jul-2008 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.066 10.342 11.738 90.00 90.00 90.00 10051 Reflections read from file 2008lsh045.hkl; mean (I/sigma) = 7.10 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5014 5025 5039 5033 7539 6707 6675 10051 N (int>3sigma) = 0 3435 3538 3461 3418 5217 4719 4704 7080 Mean intensity = 0.0 163.6 158.7 147.7 146.1 156.7 150.3 153.3 150.4 Mean int/sigma = 0.0 7.0 7.2 7.0 6.9 7.1 7.1 7.2 7.2 Lattice type: P chosen Volume: 1100.59 ------------------------------------------------------------------------------- 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: 9.066 10.342 11.738 90.00 90.00 90.00 Niggli form: a.a = 82.20 b.b = 106.96 c.c = 137.78 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) = 0.042 [ 2970] Cell: 9.066 10.342 11.738 90.00 90.00 90.00 Volume: 1100.59 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 5014 5025 5039 5033 7539 6707 6675 10051 N (int>3sigma) = 0 3435 3538 3461 3418 5217 4719 4704 7080 Mean intensity = 0.0 163.6 158.7 147.7 146.1 156.7 150.3 153.3 150.4 Mean int/sigma = 0.0 7.0 7.2 7.0 6.9 7.1 7.1 7.2 7.2 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.770 [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 350 346 342 14 331 321 340 12 266 265 269 17 N I>3s 153 152 1 3 148 3 151 1 134 162 148 0 266.8 270.0 3.3 10.9 185.7 3.3 181.2 5.6 98.5 138.6 155.7 3.0 6.0 6.1 0.7 1.5 5.5 0.7 5.4 1.2 5.2 6.8 6.1 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 1 903 0.042 2970 1.5 / 5.2 2.42 [B] Pnma # 62 centro 6 894 0.042 2970 1.5 / 5.2 6.21 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh045.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 79 85 92.9 8.15 797.9 35.11 0.0269 0.0233 2.20 - 1.70 79 79 100.0 9.91 316.7 36.24 0.0379 0.0223 1.70 - 1.45 93 93 100.0 9.78 174.4 28.28 0.0543 0.0283 1.45 - 1.30 81 81 100.0 10.04 92.1 24.58 0.0837 0.0319 1.30 - 1.20 86 86 100.0 9.78 122.1 24.39 0.0676 0.0312 1.20 - 1.10 125 125 100.0 9.38 119.8 23.68 0.0729 0.0331 1.10 - 1.00 159 159 100.0 8.30 79.3 18.71 0.0935 0.0415 1.00 - 0.95 108 108 100.0 6.96 56.3 13.44 0.1181 0.0578 0.95 - 0.90 135 135 100.0 6.07 36.2 10.53 0.1497 0.0825 0.90 - 0.85 170 171 99.4 4.82 31.1 7.58 0.1629 0.1136 0.85 - 0.80 206 209 98.6 3.56 22.3 4.64 0.2236 0.1813 0.80 - 0.77 153 162 94.4 2.32 17.0 3.04 0.2792 0.2979 ------------------------------------------------------------------------------ 0.90 - 0.77 529 542 97.6 3.59 23.6 5.12 0.1976 0.1769 Inf - 0.77 1474 1493 98.7 6.73 117.5 16.20 0.0575 0.0406 Merged [A], lowest resolution = 6.82 Angstroms, 258 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh045.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H9N1O3 Formula weight = 167.16 Tentative Z (number of formula units/cell) = 5.0 giving rho = 1.261, non-H atomic volume = 18.3 and following cell contents and analysis: C 40.00 57.48 % H 45.00 5.43 % N 5.00 8.38 % O 15.00 28.71 % F(000) = 440.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File 2008lsh045.ins set up as follows: TITL 2008lsh045 in Pna2(1) CELL 0.71073 9.0662 10.3420 11.7380 90.000 90.000 90.000 ZERR 5.00 0.0003 0.0004 0.0004 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 40 45 5 15 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------