++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh010 started at 14:58:39 on 23-Jun-2008 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.203 11.922 17.429 90.00 90.00 90.00 10907 Reflections read from file 2008lsh010.hkl; mean (I/sigma) = 4.04 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5480 5459 5437 5456 8188 7266 7255 10907 N (int>3sigma) = 0 2585 2539 2452 2468 3788 3470 3467 5171 Mean intensity = 0.0 14.9 17.7 15.1 15.1 15.9 16.4 16.3 16.8 Mean int/sigma = 0.0 4.1 4.1 4.0 4.0 4.1 4.2 4.2 4.2 Lattice type: P chosen Volume: 1496.69 ------------------------------------------------------------------------------- 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: 7.203 11.922 17.429 90.00 90.00 90.00 Niggli form: a.a = 51.88 b.b = 142.15 c.c = 303.77 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) = 0.075 [ 4307] Cell: 7.203 11.922 17.429 90.00 90.00 90.00 Volume: 1496.69 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 5480 5459 5437 5456 8188 7266 7255 10907 N (int>3sigma) = 0 2585 2539 2452 2468 3788 3470 3467 5171 Mean intensity = 0.0 14.9 17.7 15.1 15.1 15.9 16.4 16.3 16.8 Mean int/sigma = 0.0 4.1 4.1 4.0 4.0 4.1 4.2 4.2 4.2 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.984 [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 429 426 433 5 285 279 284 12 171 180 179 17 N I>3s 133 1 134 0 72 0 72 0 52 0 52 0 14.0 0.7 13.8 0.4 18.6 0.6 18.7 1.0 26.8 0.6 25.7 0.5 3.4 0.5 3.4 0.3 2.9 0.6 2.9 0.7 3.2 0.6 3.2 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] Pbca # 61 centro 2 2293 0.075 4307 0.7 / 2.9 4.30 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh010.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 104 114 91.2 5.11 85.0 19.81 0.0279 0.0341 2.20 - 1.70 107 107 100.0 6.69 46.3 21.77 0.0423 0.0313 1.70 - 1.45 118 118 100.0 7.15 21.2 17.79 0.0682 0.0386 1.45 - 1.30 125 125 100.0 7.02 10.8 11.91 0.1091 0.0601 1.30 - 1.20 109 109 100.0 7.45 21.4 12.81 0.0769 0.0500 1.20 - 1.10 164 164 100.0 7.15 15.8 11.03 0.0949 0.0630 1.10 - 1.00 220 220 100.0 7.20 10.4 9.10 0.1371 0.0762 1.00 - 0.95 152 152 100.0 6.00 7.6 6.71 0.1683 0.1078 0.95 - 0.90 175 175 100.0 5.44 5.9 5.90 0.2061 0.1404 0.90 - 0.85 232 232 100.0 4.18 3.6 3.50 0.3411 0.2449 0.85 - 0.80 273 273 100.0 3.16 3.8 2.81 0.3587 0.2822 0.80 - 0.77 228 239 95.4 2.60 2.8 2.17 0.4212 0.4323 ------------------------------------------------------------------------------ 0.90 - 0.77 733 744 98.5 3.30 3.4 2.83 0.3639 0.3087 Inf - 0.77 2007 2028 99.0 5.38 14.7 8.62 0.0867 0.0721 Merged [A], lowest resolution = 6.66 Angstroms, 376 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh010.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H10N2O1 Formula weight = 150.18 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.333, non-H atomic volume = 17.0 and following cell contents and analysis: C 64.00 63.98 % H 80.00 6.71 % N 16.00 18.66 % O 8.00 10.65 % F(000) = 640.0 Mo-K(alpha) radiation Mu (mm-1) = 0.09 ------------------------------------------------------------------------------- File pbca.ins set up as follows: TITL pbca in Pbca CELL 0.71073 11.9225 7.2026 17.4291 90.000 90.000 90.000 ZERR 8.00 0.0007 0.0002 0.0010 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O UNIT 64 80 16 8 TEMP 0.08 TREF HKLF 4 END -------------------------------------------------------------------------------