++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 08:54:35 on 01-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 5.928 8.118 9.040 67.00 90.01 90.02 4307 Reflections read from file s92.hkl; mean (I/sigma) = 6.29 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2154 2137 2153 2157 3222 2861 2861 4307 N (int>3sigma) = 0 1270 1328 1294 1309 1946 1724 1725 2623 Mean intensity = 0.0 26.8 25.8 30.8 29.0 27.8 31.7 29.3 30.9 Mean int/sigma = 0.0 6.0 6.3 6.3 6.3 6.2 6.4 6.3 6.3 Lattice type: P chosen Volume: 400.46 ------------------------------------------------------------------------------- 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: 5.928 8.118 9.040 67.00 89.99 89.98 Niggli form: a.a = 35.14 b.b = 65.91 c.c = 81.72 b.c = 28.68 a.c = 0.01 a.b = 0.01 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.017 deg. MONOCLINIC P-lattice R(int) = 0.074 [ 3323] Cell: 8.118 5.928 9.040 89.99 113.00 90.02 Volume: 400.46 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 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 2137 2154 2153 2157 3222 2861 2861 4307 N (int>3sigma) = 0 1328 1270 1294 1309 1946 1724 1725 2623 Mean intensity = 0.0 25.8 26.8 30.8 29.0 27.8 31.7 29.3 30.9 Mean int/sigma = 0.0 6.3 6.0 6.3 6.3 6.2 6.4 6.3 6.3 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.819 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 6 215 216 215 N I>3s 0 132 130 140 0.7 49.9 38.7 42.7 0.4 6.8 6.5 6.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1) # 4 chiral 1 3543 0.074 3323 0.4 / 6.3 2.29 [B] P2(1)/m # 11 centro 1 402 0.074 3323 0.4 / 6.3 4.04 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C11 H15 O5 Formula weight = 227.23 Tentative Z (number of formula units/cell) = 1.0 giving rho = 0.942, non-H atomic volume = 25.0 and following cell contents and analysis: C 11.00 58.14 % H 15.00 6.65 % O 5.00 35.21 % F(000) = 121.0 Mo-K(alpha) radiation Mu (mm-1) = 0.07 ------------------------------------------------------------------------------- File s93.ins set up as follows: TITL s93 in P2(1) CELL 0.71073 8.1183 5.9280 9.0398 90.000 113.000 90.000 ZERR 1.00 0.0007 0.0005 0.0007 0.000 0.007 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H O UNIT 11 15 5 TREF HKLF 4 END -------------------------------------------------------------------------------