++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 12:14:49 on 30-APR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 23.827 12.998 22.179 90.00 108.16 90.00 20504 Reflections read from file s92.hkl; mean (I/sigma) = 9.17 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 10232 10232 0 10249 10232 13666 13687 20504 N (int>3sigma) = 0 6513 6513 0 6477 6513 8878 8857 13402 Mean intensity = 0.0 94.5 94.5 0.0 85.2 94.5 104.5 103.4 104.2 Mean int/sigma = 0.0 9.0 9.0 0.0 8.6 9.0 9.3 9.1 9.2 Lattice type: C chosen Volume: 6526.78 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 Unitcell: 12.998 13.571 22.179 74.13 90.00 61.39 Niggli form: a.a = 168.94 b.b = 184.16 c.c = 491.93 b.c = 82.33 a.c = 0.00 a.b = 84.47 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC C-lattice R(int) = 0.058 [ 12861] Cell: 23.827 12.998 22.179 90.00 108.16 90.00 Volume: 6526.78 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 10232 10232 0 10249 10232 13666 13687 20504 N (int>3sigma) = 0 6513 6513 0 6477 6513 8878 8857 13402 Mean intensity = 0.0 94.5 94.5 0.0 85.2 94.5 104.5 103.4 104.2 Mean int/sigma = 0.0 9.0 9.0 0.0 8.6 9.0 9.3 9.1 9.2 Crystal system M and Lattice type C selected Mean |E*E-1| = 1.084 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 561 N I>3s 0 0.7 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.058 12861 0.5 / 9.2 2.52 [B] Cc # 9 non-cen 1 566 0.058 12861 0.5 / 9.2 13.44 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C48 H40 Si8 O12 Formula weight = 1033.52 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.052, non-H atomic volume = 24.0 and following cell contents and analysis: C 192.00 55.78 % H 160.00 3.90 % O 48.00 18.58 % Si 32.00 21.74 % F(000) = 2144.0 Mo-K(alpha) radiation Mu (mm-1) = 0.21 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in C2/c CELL 0.71073 23.8267 12.9976 22.1794 90.000 108.155 90.000 ZERR 4.00 0.0048 0.0026 0.0044 0.000 0.030 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H O SI UNIT 192 160 48 32 TREF HKLF 4 END -------------------------------------------------------------------------------