++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh167 started at 20:49:36 on 22-Nov-2010 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.514 9.315 12.900 90.00 90.00 90.00 7477 Reflections read from file 2008lsh167.hkl; mean (I/sigma) = 6.30 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3738 3771 3723 3728 5616 5024 4983 7477 N (int>3sigma) = 0 2153 2287 2164 2158 3302 3032 2932 4456 Mean intensity = 0.0 238.8 223.1 227.8 261.5 229.9 258.9 251.6 244.4 Mean int/sigma = 0.0 6.1 6.6 6.2 6.3 6.3 6.5 6.3 6.4 Lattice type: P chosen Volume: 902.84 ------------------------------------------------------------------------------- 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: 7.514 9.315 12.900 90.00 90.00 90.00 Niggli form: a.a = 56.46 b.b = 86.76 c.c = 166.41 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) = 0.043 [ 2001] Cell: 7.514 9.315 12.900 90.00 90.00 90.00 Volume: 902.84 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 3738 3771 3723 3728 5616 5024 4983 7477 N (int>3sigma) = 0 2153 2287 2164 2158 3302 3032 2932 4456 Mean intensity = 0.0 238.8 223.1 227.8 261.5 229.9 258.9 251.6 244.4 Mean int/sigma = 0.0 6.1 6.6 6.2 6.3 6.3 6.5 6.3 6.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.906 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 7 279 294 293 N I>3s 0 81 128 133 1.5 41.0 270.0 282.6 0.3 2.2 4.6 4.9 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) # 4 chiral 1 3543 0.036 1250 0.3 / 2.2 7.40 [B] P2(1)/m # 11 centro 1 402 0.036 1250 0.3 / 2.2 5.10 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh167.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.15 99 115 86.1 4.43 1201.9 26.06 0.0463 0.0362 2.15 - 1.70 102 106 96.2 5.27 775.1 28.96 0.0433 0.0301 1.70 - 1.45 125 128 97.7 5.24 241.8 19.52 0.0523 0.0348 1.45 - 1.30 130 132 98.5 5.28 105.8 14.88 0.0895 0.0549 1.30 - 1.20 125 127 98.4 5.06 175.8 17.08 0.0677 0.0487 1.20 - 1.10 161 161 100.0 4.78 173.1 14.77 0.0703 0.0495 1.10 - 1.05 119 123 96.7 4.15 90.6 11.70 0.1035 0.0728 1.05 - 1.00 127 131 96.9 3.79 67.2 9.88 0.1360 0.0934 1.00 - 0.95 158 166 95.2 3.54 61.1 8.00 0.1494 0.1012 0.95 - 0.90 197 217 90.8 2.87 50.1 6.06 0.1859 0.1374 0.90 - 0.85 210 246 85.4 2.37 30.9 3.98 0.3197 0.2435 0.85 - 0.80 243 318 76.4 1.61 24.3 2.76 0.3545 0.3409 0.80 - 0.77 172 266 64.7 1.19 19.3 2.47 0.5040 0.4269 ------------------------------------------------------------------------------ 0.90 - 0.77 625 830 75.3 1.70 25.1 3.09 0.3550 0.3189 Inf - 0.77 1968 2236 88.0 3.34 176.0 10.90 0.0648 0.0574 Merged [A], lowest resolution = 5.85 Angstroms, 135 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh167.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C10H11N1O3 Formula weight = 193.20 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.421, non-H atomic volume = 16.1 and following cell contents and analysis: C 40.00 62.16 % H 44.00 5.74 % N 4.00 7.25 % O 12.00 24.84 % F(000) = 408.0 Mo-K(alpha) radiation Mu (mm-1) = 0.11 ------------------------------------------------------------------------------- File p-1.ins set up as follows: TITL p-1 in P2(1) CELL 0.71073 7.5138 9.3146 12.8999 90.000 90.000 90.000 ZERR 4.00 0.0005 0.0007 0.0011 0.000 0.000 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O UNIT 40 44 4 12 TEMP 0.08 TREF HKLF 4 END 7477 Reflections written to new reflection file p-1.hkl -------------------------------------------------------------------------------