+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2008/2 for Windows + + Copyright(C) 2008 Bruker-AXS All Rights Reserved + + 2008lsh083 started at 18:06:09 on 04-Nov-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.556 4.976 15.412 90.00 97.13 90.00 11870 Reflections read from file 2008lsh083.hkl; mean (I/sigma) = 7.13 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5935 5950 5907 5960 8896 7906 7930 11870 N (int>3sigma) = 0 3854 3583 3845 3396 5641 5100 5154 7638 Mean intensity = 0.0 28.0 25.7 28.3 24.3 27.3 28.5 27.8 27.9 Mean int/sigma = 0.0 7.3 6.8 7.2 6.5 7.1 7.2 7.3 7.2 Lattice type: P chosen Volume: 803.26 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 4.976 10.556 15.412 97.13 90.00 90.00 Niggli form: a.a = 24.76 b.b = 111.44 c.c = 237.52 b.c = -20.21 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. MONOCLINIC P-lattice R(sym) = 0.026 [ 1588] Cell: 10.556 4.976 15.412 90.00 97.13 90.00 Volume: 803.26 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 5935 5950 5907 5960 8896 7906 7930 11870 N (int>3sigma) = 0 3854 3583 3845 3396 5641 5100 5154 7638 Mean intensity = 0.0 28.0 25.7 28.3 24.3 27.3 28.5 27.8 27.9 Mean int/sigma = 0.0 7.3 6.8 7.2 6.5 7.1 7.2 7.3 7.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.986 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 10 738 745 737 N I>3s 0 316 317 1 0.4 26.9 26.6 0.3 0.7 5.0 5.0 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] P2(1)/n # 14 centro 1 19410 0.026 1588 0.7 / 5.0 2.28 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh083.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.19 105 112 93.8 6.13 126.4 37.63 0.0217 0.0197 2.19 - 1.69 105 105 100.0 7.29 62.7 36.04 0.0310 0.0195 1.69 - 1.49 104 104 100.0 7.52 39.5 30.89 0.0417 0.0219 1.49 - 1.34 107 107 100.0 7.62 24.9 25.06 0.0476 0.0277 1.34 - 1.24 108 108 100.0 7.55 25.4 22.16 0.0493 0.0282 1.24 - 1.16 118 118 100.0 7.77 27.2 20.77 0.0538 0.0302 1.16 - 1.10 107 107 100.0 7.81 24.3 20.47 0.0580 0.0339 1.10 - 1.05 107 107 100.0 7.73 20.0 17.10 0.0682 0.0419 1.05 - 1.00 127 127 100.0 7.21 15.3 15.38 0.0800 0.0433 1.00 - 0.96 129 129 100.0 6.02 14.5 11.76 0.0803 0.0540 0.96 - 0.93 110 110 100.0 5.87 10.4 11.45 0.0884 0.0630 0.93 - 0.90 124 124 100.0 5.35 7.0 8.32 0.1227 0.0830 0.90 - 0.87 142 142 100.0 4.48 7.8 7.39 0.1285 0.0964 0.87 - 0.84 143 143 100.0 3.62 6.0 5.70 0.1439 0.1207 0.84 - 0.82 132 132 100.0 3.20 6.9 5.57 0.1139 0.1216 0.82 - 0.80 141 142 99.3 3.04 5.0 3.94 0.1853 0.1737 0.80 - 0.78 146 146 100.0 2.83 5.3 4.28 0.1727 0.1793 0.78 - 0.77 2 12 16.7 0.33 0.4 0.72 1.2615 1.4032 ------------------------------------------------------------------------------ 0.87 - 0.77 614 625 98.2 3.22 5.8 5.01 0.1507 0.1437 Inf - 0.77 2057 2075 99.1 5.72 23.1 15.57 0.0482 0.0383 Merged [A], lowest resolution = 6.58 Angstroms, 369 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh083.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H8N2O3 Formula weight = 180.16 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.490, non-H atomic volume = 15.4 and following cell contents and analysis: C 32.00 53.33 % H 32.00 4.48 % N 8.00 15.55 % O 12.00 26.64 % F(000) = 376.0 Mo-K(alpha) radiation Mu (mm-1) = 0.12 ------------------------------------------------------------------------------- File 2008lsh083.ins set up as follows: TITL 2008lsh083 in P2(1)/n CELL 0.71073 10.5564 4.9758 15.4117 90.000 97.134 90.000 ZERR 4.00 0.0004 0.0002 0.0005 0.000 0.002 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 32 32 8 12 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------