++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 11:43:02 on 11-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.778 20.111 13.196 90.00 96.67 90.00 6549 Reflections read from file s92.hkl; mean (I/sigma) = 8.04 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3280 3280 0 3256 3280 4374 4353 6549 N (int>3sigma) = 0 2086 2086 0 2064 2086 2770 2801 4204 Mean intensity = 0.0 41.3 41.3 0.0 44.9 41.3 46.3 47.0 46.7 Mean int/sigma = 0.0 8.0 8.0 0.0 7.9 8.0 8.1 8.1 8.1 Lattice type: C chosen Volume: 1786.56 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 Unitcell: 6.778 10.611 13.196 87.87 83.33 71.38 Niggli form: a.a = 45.94 b.b = 112.60 c.c = 174.14 b.c = 5.20 a.c = 10.39 a.b = 22.97 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC C-lattice R(int) = 0.060 [ 4481] Cell: 6.778 20.111 13.196 90.00 96.67 90.00 Volume: 1786.56 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 3280 3280 0 3256 3280 4374 4353 6549 N (int>3sigma) = 0 2086 2086 0 2064 2086 2770 2801 4204 Mean intensity = 0.0 41.3 41.3 0.0 44.9 41.3 46.3 47.0 46.7 Mean int/sigma = 0.0 8.0 8.0 0.0 7.9 8.0 8.1 8.1 8.1 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.997 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 82 N I>3s 0 0.8 0.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.060 4481 0.4 / 8.1 1.40 [B] Cc # 9 non-cen 1 566 0.060 4481 0.4 / 8.1 8.27 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C22 H20 O6 Formula weight = 380.38 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.414, non-H atomic volume = 16.0 and following cell contents and analysis: C 88.00 69.46 % H 80.00 5.30 % O 24.00 25.24 % F(000) = 800.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in C2/c CELL 0.71073 6.7778 20.1108 13.1963 90.000 96.674 90.000 ZERR 4.00 0.0003 0.0011 0.0009 0.000 0.002 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H O UNIT 88 80 24 TREF HKLF 4 END -------------------------------------------------------------------------------