++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 11:55:14 on 26-NOV-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 14.149 17.300 17.434 90.00 90.00 90.00 27115 Reflections read from file s92.hkl; mean (I/sigma) = 3.75 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 13563 13580 13555 13529 20349 18049 18080 27115 N (int>3sigma) = 0 4891 4825 4918 4994 7317 6667 6645 10037 Mean intensity = 0.0 11.5 11.1 12.3 12.3 11.6 12.4 12.3 12.4 Mean int/sigma = 0.0 3.7 3.7 3.8 3.9 3.8 3.9 3.9 3.9 Lattice type: P chosen Volume: 4267.62 ------------------------------------------------------------------------------- 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: 14.149 17.300 17.434 90.00 90.00 90.00 Niggli form: a.a = 200.20 b.b = 299.30 c.c = 303.94 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.221 deg. TETRAGONAL P-lattice R(int) = 0.638 [ 21985] Cell: 17.300 17.434 14.149 90.00 90.00 90.00 Volume: 4267.62 Matrix: 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(int) = 0.108 [ 21688] Cell: 14.149 17.300 17.434 90.00 90.00 90.00 Volume: 4267.62 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 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 13563 13580 13555 13529 20349 18049 18080 27115 N (int>3sigma) = 0 4891 4825 4918 4994 7317 6667 6645 10037 Mean intensity = 0.0 11.5 11.1 12.3 12.3 11.6 12.4 12.3 12.4 Mean int/sigma = 0.0 3.7 3.7 3.8 3.9 3.8 3.9 3.9 3.9 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.942 [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 630 634 632 14 506 512 506 18 516 515 509 19 N I>3s 0 162 162 0 4 143 145 0 0 146 146 0 0.6 12.6 12.6 0.2 0.5 20.0 20.2 0.6 0.5 29.6 29.9 0.5 0.5 3.0 3.1 0.4 0.5 3.6 3.6 0.5 0.5 3.6 3.7 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pbca # 61 centro 1 2293 0.108 21688 0.5 / 3.0 4.02 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C23 H24 O9 Formula weight = 444.42 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.383, non-H atomic volume = 16.7 and following cell contents and analysis: C 184.00 62.15 % H 192.00 5.44 % O 72.00 32.40 % F(000) = 1872.0 Mo-K(alpha) radiation Mu (mm-1) = 0.11 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in Pbca CELL 0.71073 14.1493 17.3003 17.4340 90.000 90.000 90.000 ZERR 8.00 0.0028 0.0035 0.0035 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H O UNIT 184 192 72 TREF HKLF 4 END -------------------------------------------------------------------------------