++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh023 started at 11:36:52 on 19-Nov-2010 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.442 9.577 13.877 90.00 103.02 90.00 11374 Reflections read from file 2008lsh023.hkl; mean (I/sigma) = 7.13 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5667 5676 5701 5689 8522 7572 7584 11374 N (int>3sigma) = 0 3557 3681 3470 3507 5354 4819 4806 7299 Mean intensity = 0.0 126.1 126.2 123.9 131.0 125.4 137.1 131.4 137.8 Mean int/sigma = 0.0 7.0 7.3 6.9 7.0 7.1 7.2 7.1 7.2 Lattice type: P chosen Volume: 963.53 ------------------------------------------------------------------------------- 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: 7.442 9.577 13.877 90.00 103.02 90.00 Niggli form: a.a = 55.38 b.b = 91.72 c.c = 192.57 b.c = 0.00 a.c = -23.27 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. MONOCLINIC P-lattice R(sym) = 0.032 [ 1808] Cell: 7.442 9.577 13.877 90.00 103.02 90.00 Volume: 963.53 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 5667 5676 5701 5689 8522 7572 7584 11374 N (int>3sigma) = 0 3557 3681 3470 3507 5354 4819 4806 7299 Mean intensity = 0.0 126.1 126.2 123.9 131.0 125.4 137.1 131.4 137.8 Mean int/sigma = 0.0 7.0 7.3 6.9 7.0 7.1 7.2 7.1 7.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.976 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 13 410 431 431 N I>3s 0 3 167 168 4.9 2.3 192.3 192.6 1.2 0.6 5.0 5.1 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)/c # 14 centro 4 19410 0.032 1808 1.2 / 5.0 2.24 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh023.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.10 124 131 94.7 6.63 725.6 34.68 0.0283 0.0250 2.10 - 1.65 130 131 99.2 7.21 295.5 32.22 0.0375 0.0232 1.65 - 1.40 151 151 100.0 7.29 145.4 24.80 0.0505 0.0271 1.40 - 1.25 156 157 99.4 7.03 88.5 20.62 0.0681 0.0326 1.25 - 1.15 161 161 100.0 6.81 96.6 20.03 0.0696 0.0336 1.15 - 1.05 216 218 99.1 6.08 98.3 18.14 0.0644 0.0376 1.05 - 1.00 147 147 100.0 5.45 57.6 13.84 0.0845 0.0493 1.00 - 0.95 167 167 100.0 5.22 40.5 11.67 0.1064 0.0617 0.95 - 0.90 226 227 99.6 4.17 33.6 8.73 0.1254 0.0821 0.90 - 0.85 268 268 100.0 3.50 22.3 5.80 0.1624 0.1309 0.85 - 0.80 339 343 98.8 2.59 17.0 4.08 0.2030 0.1939 0.80 - 0.77 240 261 92.0 1.88 16.3 3.36 0.2275 0.2451 ------------------------------------------------------------------------------ 0.90 - 0.77 847 872 97.1 2.66 18.5 4.42 0.1867 0.1826 Inf - 0.77 2325 2362 98.4 4.82 103.0 13.89 0.0521 0.0410 Merged [A], lowest resolution = 5.86 Angstroms, 245 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh023.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H9N1O2 Formula weight = 151.16 Tentative Z (number of formula units/cell) = 5.0 giving rho = 1.303, non-H atomic volume = 17.5 and following cell contents and analysis: C 40.00 63.56 % H 45.00 6.00 % N 5.00 9.27 % O 10.00 21.17 % F(000) = 400.0 Mo-K(alpha) radiation Mu (mm-1) = 0.09 ------------------------------------------------------------------------------- File p21c.ins set up as follows: TITL p21c in P2(1)/c CELL 0.71073 13.8770 9.5769 7.4415 90.000 103.022 90.000 ZERR 5.00 0.0004 0.0004 0.0003 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 40 45 5 10 TEMP 0.02 TREF HKLF 4 END 11374 Reflections written to new reflection file p21c.hkl -------------------------------------------------------------------------------