++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh011 started at 15:20:10 on 23-Jun-2008 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.729 13.339 12.985 90.00 103.79 90.00 24487 Reflections read from file 2008lsh011.hkl; mean (I/sigma) = 9.17 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 12286 12224 12270 12243 18390 16307 16298 24487 N (int>3sigma) = 0 9142 9191 9099 9212 13716 12250 12275 18413 Mean intensity = 0.0 26.1 22.1 25.2 26.3 24.5 26.7 25.3 26.0 Mean int/sigma = 0.0 9.1 9.1 8.9 9.3 9.1 9.2 9.2 9.2 Lattice type: P chosen Volume: 1636.48 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 9.729 12.985 13.339 90.00 90.00 103.79 Niggli form: a.a = 94.64 b.b = 168.61 c.c = 177.93 b.c = 0.00 a.c = 0.00 a.b = -30.11 ------------------------------------------------------------------------------- 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) = 0.024 [ 3480] Cell: 9.729 13.339 12.985 90.00 103.79 90.00 Volume: 1636.48 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 12286 12224 12270 12243 18390 16307 16298 24487 N (int>3sigma) = 0 9142 9191 9099 9212 13716 12250 12275 18413 Mean intensity = 0.0 26.1 22.1 25.2 26.3 24.5 26.7 25.3 26.0 Mean int/sigma = 0.0 9.1 9.1 8.9 9.3 9.1 9.2 9.2 9.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.901 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 28 567 564 559 N I>3s 2 307 323 402 0.6 8.8 9.3 16.0 1.1 6.1 6.5 9.1 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) # 4 chiral 1 3543 0.024 3480 1.1 / 6.1 4.62 [B] P2(1)/m # 11 centro 1 402 0.024 3480 1.1 / 6.1 2.56 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh011.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.10 201 211 95.3 7.31 99.1 47.69 0.0254 0.0189 2.10 - 1.65 205 205 100.0 8.51 58.7 51.51 0.0300 0.0153 1.65 - 1.40 259 259 100.0 8.39 39.7 41.94 0.0349 0.0175 1.40 - 1.25 271 271 100.0 8.33 20.9 33.21 0.0467 0.0240 1.25 - 1.15 262 262 100.0 8.29 28.3 29.94 0.0435 0.0246 1.15 - 1.05 378 378 100.0 8.30 23.6 26.76 0.0493 0.0277 1.05 - 1.00 234 234 100.0 8.01 16.3 20.76 0.0645 0.0334 1.00 - 0.95 291 291 100.0 6.76 11.1 17.14 0.0870 0.0452 0.95 - 0.90 363 366 99.2 5.98 8.2 13.37 0.1076 0.0602 0.90 - 0.85 451 456 98.9 4.65 6.6 9.29 0.1403 0.0849 0.85 - 0.80 567 575 98.6 3.44 5.1 6.52 0.1758 0.1323 0.80 - 0.77 422 434 97.2 3.06 3.9 4.71 0.2124 0.1901 ------------------------------------------------------------------------------ 0.90 - 0.77 1440 1465 98.3 3.71 5.2 6.86 0.1653 0.1261 Inf - 0.77 3904 3942 99.0 6.21 20.9 21.14 0.0462 0.0331 Merged [A], lowest resolution = 6.82 Angstroms, 882 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh011.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H8N2O3 Formula weight = 180.16 Tentative Z (number of formula units/cell) = 7.0 giving rho = 1.280, non-H atomic volume = 18.0 and following cell contents and analysis: C 56.00 53.33 % H 56.00 4.48 % N 14.00 15.55 % O 21.00 26.64 % F(000) = 658.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File 2008lsh011.ins set up as follows: TITL 2008lsh011 in P2(1) CELL 0.71073 9.7285 13.3392 12.9849 90.000 103.791 90.000 ZERR 7.00 0.0005 0.0007 0.0005 0.000 0.003 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O UNIT 56 56 14 21 TEMP 0.2 TREF HKLF 4 END -------------------------------------------------------------------------------