++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh121 started at 17:17:55 on 30-Mar-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 20.803 4.716 6.709 90.00 105.89 90.00 3631 Reflections read from file 2008lsh121.hkl; mean (I/sigma) = 10.20 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1820 1820 0 1824 1820 2412 2428 3631 N (int>3sigma) = 0 1533 1533 0 1541 1533 2034 2024 3040 Mean intensity = 0.0 197.8 197.8 0.0 199.2 197.8 189.5 191.5 194.8 Mean int/sigma = 0.0 10.6 10.6 0.0 10.4 10.6 10.1 10.2 10.2 Lattice type: C chosen Volume: 633.14 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.5000 -0.5000 0.0000 Unitcell: 4.716 6.709 10.665 74.51 77.23 90.00 Niggli form: a.a = 22.24 b.b = 45.02 c.c = 113.75 b.c = 19.11 a.c = 11.12 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 C-lattice R(sym) = 0.025 [ 576] Cell: 20.803 4.716 6.709 90.00 105.89 90.00 Volume: 633.14 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC I-lattice R(sym) = 0.025 [ 576] Cell: 6.709 4.716 20.034 90.00 92.90 90.00 Volume: 633.14 Matrix: 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1824 1850 1820 0 2747 2413 2406 3631 N (int>3sigma) = 0 1541 1602 1533 0 2338 2034 2009 3040 Mean intensity = 0.0 199.2 198.6 197.8 0.0 198.5 191.5 202.8 194.8 Mean int/sigma = 0.0 10.4 10.7 10.6 0.0 10.6 10.2 10.3 10.2 Crystal system M and Lattice type I selected Mean |E*E-1| = 0.765 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -a- N 295 N I>3s 249 296.6 11.7 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] I2 # 5 chiral 1 552 0.025 576 0.0 / 10.2 1.24 [B] I2/m # 12 centro 1 310 0.025 576 0.0 / 10.2 5.40 [C] Im # 8 non-cen 1 32 0.025 576 0.0 / 10.2 4.09 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh121.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 41 42 97.6 5.48 1024.1 41.46 0.0249 0.0219 2.20 - 1.70 42 42 100.0 6.79 377.1 42.34 0.0304 0.0196 1.70 - 1.50 41 41 100.0 6.98 229.5 39.70 0.0374 0.0214 1.50 - 1.30 56 56 100.0 6.43 153.2 30.05 0.0480 0.0267 1.30 - 1.20 44 44 100.0 6.84 162.7 31.88 0.0530 0.0259 1.20 - 1.10 72 72 100.0 5.72 140.0 23.73 0.0579 0.0322 1.10 - 1.00 89 89 100.0 5.10 128.3 22.30 0.0533 0.0368 1.00 - 0.95 61 61 100.0 4.46 79.1 16.26 0.0773 0.0496 0.95 - 0.90 72 72 100.0 3.78 53.8 12.49 0.0875 0.0638 0.90 - 0.85 97 97 100.0 3.14 38.1 9.24 0.1020 0.0924 0.85 - 0.80 114 118 96.6 2.37 34.8 6.83 0.1111 0.1232 0.80 - 0.77 79 84 94.0 2.07 30.2 5.73 0.1316 0.1555 ------------------------------------------------------------------------------ 0.90 - 0.77 290 299 97.0 2.54 34.6 7.34 0.1104 0.1195 Inf - 0.77 808 818 98.8 4.44 152.5 19.68 0.0419 0.0347 Merged [A], lowest resolution = 6.45 Angstroms, 87 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh121.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H8N2O3 Formula weight = 180.16 Tentative Z (number of formula units/cell) = 2.0 giving rho = 0.945, non-H atomic volume = 24.4 and following cell contents and analysis: C 16.00 53.33 % H 16.00 4.48 % N 4.00 15.55 % O 6.00 26.64 % F(000) = 188.0 Mo-K(alpha) radiation Mu (mm-1) = 0.07 ------------------------------------------------------------------------------- File test.ins set up as follows: TITL test in I2 CELL 0.71073 6.7095 4.7163 20.0338 90.000 92.902 90.000 ZERR 2.00 0.0003 0.0003 0.0013 0.000 0.004 0.000 LATT -2 SYMM -X, Y, -Z SFAC C H N O UNIT 16 16 4 6 TEMP 0.01 TREF HKLF 4 END 3631 Reflections written to new reflection file test.hkl -------------------------------------------------------------------------------