++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 10:03:01 on 11-AUG-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.778 15.436 15.688 90.00 102.46 90.00 24955 Reflections read from file s92.hkl; mean (I/sigma) = 2.07 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 12502 12469 12505 12474 18738 16637 16625 24955 N (int>3sigma) = 0 3179 2948 3191 3052 4659 4247 4224 6403 Mean intensity = 0.0 8.1 6.4 8.0 7.1 7.5 7.5 7.7 7.6 Mean int/sigma = 0.0 2.3 2.1 2.2 2.2 2.2 2.3 2.3 2.3 Lattice type: P chosen Volume: 2548.61 ------------------------------------------------------------------------------- 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: 10.778 15.436 15.688 90.00 102.46 90.00 Niggli form: a.a = 116.17 b.b = 238.27 c.c = 246.12 b.c = 0.00 a.c = -36.47 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.187 [ 19478] Cell: 10.778 15.436 15.688 90.00 102.46 90.00 Volume: 2548.61 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.159 [ 14947] Cell: 10.778 15.436 15.688 90.00 77.54 90.00 Volume: 2548.61 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 12502 12469 12505 12474 18738 16637 16625 24955 N (int>3sigma) = 0 3179 2948 3191 3052 4659 4247 4224 6403 Mean intensity = 0.0 8.1 6.4 8.0 7.1 7.5 7.5 7.7 7.6 Mean int/sigma = 0.0 2.3 2.1 2.2 2.2 2.2 2.3 2.3 2.3 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.875 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 13 497 500 503 N I>3s 0 126 125 1 0.9 7.2 7.2 0.8 0.6 2.1 2.1 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.187 19478 0.6 / 2.1 7.10 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C13 H14 N2 S1 O2 Formula weight = 262.32 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.367, non-H atomic volume = 17.7 and following cell contents and analysis: C 104.00 59.52 % H 112.00 5.38 % N 16.00 10.68 % O 16.00 12.20 % S 8.00 12.22 % F(000) = 1104.0 Mo-K(alpha) radiation Mu (mm-1) = 0.25 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/n CELL 0.71073 10.7781 15.4360 15.6882 90.000 102.457 90.000 ZERR 8.00 0.0022 0.0031 0.0031 0.000 0.030 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O S UNIT 104 112 16 16 8 TREF HKLF 4 END -------------------------------------------------------------------------------