++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 13:38:20 on 04-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.027 7.940 12.193 82.26 89.81 88.35 4242 Reflections read from file s92.hkl; mean (I/sigma) = 11.29 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2123 2122 2121 2114 3183 2819 2832 4242 N (int>3sigma) = 0 1690 1668 1682 1662 2520 2260 2259 3365 Mean intensity = 0.0 189.3 184.8 185.5 183.1 186.5 185.7 183.1 187.6 Mean int/sigma = 0.0 11.3 11.2 11.4 11.4 11.3 11.5 11.4 11.3 Lattice type: P chosen Volume: 577.93 ------------------------------------------------------------------------------- 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: 6.027 7.940 12.193 82.26 89.81 88.35 Niggli form: a.a = 36.32 b.b = 63.05 c.c = 148.67 b.c = 13.03 a.c = 0.25 a.b = 1.38 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.034 [ 1868] Cell: 6.027 7.940 12.193 82.26 89.81 88.35 Volume: 577.93 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 2123 2122 2121 2114 3183 2819 2832 4242 N (int>3sigma) = 0 1690 1668 1682 1662 2520 2260 2259 3365 Mean intensity = 0.0 189.3 184.8 185.5 183.1 186.5 185.7 183.1 187.6 Mean int/sigma = 0.0 11.3 11.2 11.4 11.4 11.3 11.5 11.4 11.3 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.942 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P-1 # 2 centro 1 8646 0.034 1868 0.0 / 11.3 0.96 [B] P1 # 1 chiral 1 700 0.034 1868 0.0 / 11.3 5.28 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) = 2.0 giving rho = 1.427, non-H atomic volume = 17.0 and following cell contents and analysis: C 24.00 58.04 % H 24.00 4.87 % N 4.00 11.28 % O 4.00 12.89 % S 2.00 12.91 % F(000) = 260.0 Mo-K(alpha) radiation Mu (mm-1) = 0.27 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P-1 CELL 0.71073 6.0265 7.9404 12.1931 82.265 89.808 88.351 ZERR 2.00 0.0012 0.0016 0.0024 0.030 0.030 0.030 LATT 1 SFAC C H N O S UNIT 24 24 4 4 2 TREF HKLF 4 END -------------------------------------------------------------------------------