++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 16:09:34 on 13-AUG-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.973 12.764 20.721 90.00 90.00 90.00 26699 Reflections read from file s92.hkl; mean (I/sigma) = 3.31 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 13279 13318 13357 13291 19977 17816 17807 26699 N (int>3sigma) = 0 4156 4282 4152 4277 6295 5669 5683 8586 Mean intensity = 0.0 32.6 31.2 29.6 34.2 31.1 33.0 33.4 33.5 Mean int/sigma = 0.0 3.5 3.4 3.4 3.4 3.4 3.4 3.5 3.5 Lattice type: P chosen Volume: 2902.16 ------------------------------------------------------------------------------- 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: 10.973 12.764 20.721 90.00 90.00 90.00 Niggli form: a.a = 120.41 b.b = 162.91 c.c = 429.37 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(int) = 0.098 [ 23006] Cell: 10.973 12.764 20.721 90.00 90.00 90.00 Volume: 2902.16 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 13279 13318 13357 13291 19977 17816 17807 26699 N (int>3sigma) = 0 4156 4282 4152 4277 6295 5669 5683 8586 Mean intensity = 0.0 32.6 31.2 29.6 34.2 31.1 33.0 33.4 33.5 Mean int/sigma = 0.0 3.5 3.4 3.4 3.4 3.4 3.4 3.5 3.5 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.759 [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 616 611 541 8 447 426 447 10 417 408 417 15 N I>3s 173 173 0 0 125 0 125 0 202 165 169 0 74.3 75.0 1.6 0.8 53.9 1.8 53.9 1.1 61.5 31.9 62.7 1.5 3.5 3.5 0.5 0.3 3.3 0.5 3.3 0.3 5.0 4.4 4.5 0.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pna2(1) # 33 non-cen 1 903 0.098 23006 0.5 / 3.3 3.71 [B] Pnma # 62 centro 6 894 0.098 23006 0.5 / 3.3 8.04 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C15 H19 O4 F1 Formula weight = 282.30 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.292, non-H atomic volume = 18.1 and following cell contents and analysis: C 120.00 63.81 % H 152.00 6.78 % O 32.00 22.67 % F 8.00 6.73 % F(000) = 1200.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in Pna2(1) CELL 0.71073 10.9732 12.7636 20.7212 90.000 90.000 90.000 ZERR 8.00 0.0022 0.0026 0.0041 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, 0.5-Y, Z SYMM 0.5-X, 0.5+Y, 0.5+Z SFAC C H O F UNIT 120 152 32 8 TREF HKLF 4 END -------------------------------------------------------------------------------