++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 10:06:58 on 03-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.728 14.895 14.669 90.00 103.20 90.00 17576 Reflections read from file s92.hkl; mean (I/sigma) = 4.07 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8813 8792 8785 8782 13195 11702 11722 17576 N (int>3sigma) = 0 3800 3784 3790 3755 5687 5069 5015 7563 Mean intensity = 0.0 10.5 11.7 11.9 11.1 11.4 10.9 10.8 11.3 Mean int/sigma = 0.0 4.1 4.2 4.2 4.2 4.2 4.2 4.2 4.2 Lattice type: P chosen Volume: 2282.06 ------------------------------------------------------------------------------- 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: 10.728 14.669 14.895 90.00 90.00 103.20 Niggli form: a.a = 115.09 b.b = 215.18 c.c = 221.86 b.c = 0.00 a.c = 0.00 a.b = -35.95 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.094 [ 12368] Cell: 10.728 14.895 14.669 90.00 103.20 90.00 Volume: 2282.06 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 8813 8792 8785 8782 13195 11702 11722 17576 N (int>3sigma) = 0 3800 3784 3790 3755 5687 5069 5015 7563 Mean intensity = 0.0 10.5 11.7 11.9 11.1 11.4 10.9 10.8 11.3 Mean int/sigma = 0.0 4.1 4.2 4.2 4.2 4.2 4.2 4.2 4.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.937 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 25 335 331 332 N I>3s 0 105 0 105 0.3 13.5 0.4 13.6 0.4 3.7 0.5 3.7 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.094 12368 0.5 / 3.7 3.21 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12 H12 N2 S1 O2 Formula weight = 248.30 Tentative Z (number of formula units/cell) = 7.0 giving rho = 1.265, non-H atomic volume = 19.2 and following cell contents and analysis: C 84.00 58.04 % H 84.00 4.87 % N 14.00 11.28 % O 14.00 12.89 % S 7.00 12.91 % F(000) = 910.0 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 10.7281 14.8951 14.6689 90.000 103.204 90.000 ZERR 7.00 0.0021 0.0030 0.0029 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O S UNIT 84 84 14 14 7 TREF HKLF 4 END -------------------------------------------------------------------------------