++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh058 started at 18:20:11 on 22-Jul-2008 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 4.615 5.370 31.270 90.00 91.98 90.00 6482 Reflections read from file 2008lsh058.hkl; mean (I/sigma) = 8.17 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3231 3240 3205 3254 4838 4336 4307 6482 N (int>3sigma) = 0 2170 1967 2169 1940 3153 2887 2828 4274 Mean intensity = 0.0 28.7 25.0 26.1 24.7 26.6 28.3 28.3 29.0 Mean int/sigma = 0.0 8.5 7.7 8.3 7.4 8.2 8.3 8.3 8.3 Lattice type: P chosen Volume: 774.52 ------------------------------------------------------------------------------- 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: 4.615 5.370 31.270 90.00 91.98 90.00 Niggli form: a.a = 21.30 b.b = 28.83 c.c = 977.81 b.c = 0.00 a.c = -4.98 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) = 0.028 [ 1135] Cell: 4.615 5.370 31.270 90.00 91.98 90.00 Volume: 774.52 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 3231 3240 3205 3254 4838 4336 4307 6482 N (int>3sigma) = 0 2170 1967 2169 1940 3153 2887 2828 4274 Mean intensity = 0.0 28.7 25.0 26.1 24.7 26.6 28.3 28.3 29.0 Mean int/sigma = 0.0 8.5 7.7 8.3 7.4 8.2 8.3 8.3 8.3 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.959 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 12 531 472 491 N I>3s 0 209 209 0 0.1 24.7 27.8 0.2 0.6 5.9 6.6 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 0.028 1135 0.6 / 5.9 1.87 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh058.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.15 101 107 94.4 6.38 106.4 33.58 0.0341 0.0228 2.15 - 1.65 115 116 99.1 5.29 56.2 32.43 0.0321 0.0226 1.65 - 1.45 98 98 100.0 4.67 30.7 23.91 0.0344 0.0339 1.45 - 1.30 122 122 100.0 4.46 20.1 20.21 0.0453 0.0332 1.30 - 1.20 98 102 96.1 3.51 27.6 21.16 0.0394 0.0340 1.20 - 1.10 160 164 97.6 2.92 20.9 15.08 0.0425 0.0459 1.10 - 1.05 97 101 96.0 2.98 14.0 13.10 0.0519 0.0526 1.05 - 1.00 120 122 98.4 2.97 20.8 14.73 0.0441 0.0490 1.00 - 0.95 140 142 98.6 2.61 10.3 9.78 0.0725 0.0692 0.95 - 0.90 165 168 98.2 2.70 6.4 7.28 0.0990 0.0997 0.90 - 0.85 250 251 99.6 2.64 7.9 7.96 0.0994 0.0940 0.85 - 0.80 271 271 100.0 2.79 4.3 5.18 0.1585 0.1389 0.80 - 0.77 173 190 91.1 2.31 3.9 4.38 0.1980 0.1986 ------------------------------------------------------------------------------ 0.90 - 0.77 694 712 97.5 2.61 5.5 5.98 0.1337 0.1260 Inf - 0.77 1910 1954 97.7 3.32 20.4 13.70 0.0429 0.0437 Merged [A], lowest resolution = 6.25 Angstroms, 167 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh058.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H10N2O1 Formula weight = 150.18 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.288, non-H atomic volume = 17.6 and following cell contents and analysis: C 32.00 63.98 % H 40.00 6.71 % N 8.00 18.66 % O 4.00 10.65 % F(000) = 320.0 Mo-K(alpha) radiation Mu (mm-1) = 0.09 ------------------------------------------------------------------------------- File 2008lsh058.ins set up as follows: TITL 2008lsh058 in P2(1)/n CELL 0.71073 4.6154 5.3698 31.2699 90.000 91.978 90.000 ZERR 4.00 0.0002 0.0002 0.0013 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 40 8 4 TEMP 0.06 TREF HKLF 4 END -------------------------------------------------------------------------------