++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 15:17:33 on 08-APR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.482 22.666 10.037 90.00 116.14 90.00 12261 Reflections read from file s92.hkl; mean (I/sigma) = 10.06 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6109 6082 6169 6168 9180 8161 8152 12261 N (int>3sigma) = 0 4417 4447 4542 4510 6703 5942 5977 8989 Mean intensity = 0.0 78.1 79.6 79.4 85.9 79.1 79.4 83.9 83.3 Mean int/sigma = 0.0 10.0 10.1 10.0 10.2 10.0 10.0 10.2 10.1 Lattice type: P chosen Volume: 1936.51 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 9.482 10.037 22.666 90.00 90.00 116.14 Niggli form: a.a = 89.92 b.b = 100.74 c.c = 513.72 b.c = 0.00 a.c = 0.00 a.b = -41.93 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.068 [ 7812] Cell: 9.482 22.666 10.037 90.00 116.14 90.00 Volume: 1936.51 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 6109 6082 6169 6168 9180 8161 8152 12261 N (int>3sigma) = 0 4417 4447 4542 4510 6703 5942 5977 8989 Mean intensity = 0.0 78.1 79.6 79.4 85.9 79.1 79.4 83.9 83.3 Mean int/sigma = 0.0 10.0 10.1 10.0 10.2 10.0 10.0 10.2 10.1 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.980 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 12 187 173 180 N I>3s 0 78 2 78 0.5 98.9 0.8 102.7 0.5 6.2 0.5 6.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.068 7812 0.5 / 6.2 1.77 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C18H28N2O2SSi Formula weight = 364.57 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.250, non-H atomic volume = 20.2 and following cell contents and analysis: C 72.00 59.30 % H 112.00 7.74 % N 8.00 7.69 % O 8.00 8.78 % Si 4.00 7.70 % S 4.00 8.79 % F(000) = 784.0 Mo-K(alpha) radiation Mu (mm-1) = 0.24 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/c CELL 0.71073 9.4824 22.6655 10.0368 90.000 116.140 90.000 ZERR 4.00 0.0002 0.0006 0.0003 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O SI S UNIT 72 112 8 8 4 4 TREF HKLF 4 END -------------------------------------------------------------------------------