++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2007may0020 started at 11:37:10 on 05-Oct-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 5.108 5.853 16.014 90.00 90.62 90.00 6845 Reflections read from file 2007may0020.hkl; mean (I/sigma) = 7.88 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3420 3426 3434 3406 5140 4542 4556 6845 N (int>3sigma) = 0 1915 2122 2075 2097 3056 2766 2812 4222 Mean intensity = 0.0 16.6 22.1 22.2 22.7 20.3 21.8 22.4 22.5 Mean int/sigma = 0.0 6.9 7.9 7.9 8.1 7.6 7.9 7.9 8.0 Lattice type: P chosen Volume: 478.77 ------------------------------------------------------------------------------- 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: 5.108 5.853 16.014 90.00 90.62 90.00 Niggli form: a.a = 26.09 b.b = 34.26 c.c = 256.45 b.c = 0.00 a.c = -0.89 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.624 deg. ORTHORHOMBIC P-lattice R(sym) = 0.486 [ 1426] Cell: 5.108 5.853 16.014 90.00 90.62 90.00 Volume: 478.77 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 P-lattice R(sym) = 0.032 [ 910] Cell: 5.108 5.853 16.014 90.00 90.62 90.00 Volume: 478.77 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.624 deg. MONOCLINIC P-lattice R(sym) = 0.504 [ 980] Cell: 5.108 16.014 5.853 90.00 90.00 89.38 Volume: 478.77 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.624 deg. MONOCLINIC P-lattice R(sym) = 0.570 [ 891] Cell: 5.853 5.108 16.014 89.38 90.00 90.00 Volume: 478.77 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3420 3426 3434 3406 5140 4542 4556 6845 N (int>3sigma) = 0 1915 2122 2075 2097 3056 2766 2812 4222 Mean intensity = 0.0 16.6 22.1 22.2 22.7 20.3 21.8 22.4 22.5 Mean int/sigma = 0.0 6.9 7.9 7.9 8.1 7.6 7.9 7.9 8.0 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.933 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 16 403 394 393 N I>3s 0 144 1 143 0.4 27.5 0.7 28.0 1.0 5.6 0.6 5.7 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] P2(1)/c # 14 centro 1 19410 0.032 910 1.0 / 5.6 2.10 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2007may0020.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.15 65 67 97.0 6.25 91.6 36.99 0.0425 0.0868 2.15 - 1.65 70 70 100.0 7.20 45.9 36.61 0.0422 0.1267 1.65 - 1.40 83 83 100.0 7.30 43.1 33.33 0.0377 0.1327 1.40 - 1.25 77 77 100.0 7.49 20.4 27.40 0.0539 0.0247 1.25 - 1.15 84 84 100.0 7.33 20.8 25.34 0.0727 0.0810 1.15 - 1.05 110 110 100.0 7.66 19.7 24.40 0.0552 0.0286 1.05 - 1.00 73 73 100.0 7.15 13.1 15.51 0.0739 0.0389 1.00 - 0.95 98 98 100.0 6.11 11.7 13.37 0.0952 0.0480 0.95 - 0.90 112 112 100.0 5.60 7.7 10.59 0.1194 0.1062 0.90 - 0.85 120 120 100.0 4.43 5.0 6.93 0.1557 0.1031 0.85 - 0.80 194 194 100.0 3.31 4.8 5.46 0.1695 0.1335 0.80 - 0.77 128 129 99.2 2.78 2.7 3.07 0.3163 0.2507 ------------------------------------------------------------------------------ 0.90 - 0.77 442 443 99.8 3.46 4.2 5.16 0.1827 0.1455 Inf - 0.77 1214 1217 99.8 5.62 19.0 16.94 0.0591 0.0909 Merged [A], lowest resolution = 5.85 Angstroms, 233 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2007may0020.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C5H4O3 Formula weight = 112.08 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.555, non-H atomic volume = 15.0 and following cell contents and analysis: C 20.00 53.58 % H 16.00 3.60 % O 12.00 42.83 % F(000) = 232.0 Mo-K(alpha) radiation Mu (mm-1) = 0.13 ------------------------------------------------------------------------------- File 2007may0020.ins set up as follows: TITL 2007may0020 in P2(1)/c CELL 0.71073 5.1078 5.8535 16.0142 90.000 90.624 90.000 ZERR 4.00 0.0004 0.0005 0.0014 0.000 0.005 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O UNIT 20 16 12 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------