++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 10:18:51 on 13-NOV-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 12.179 9.610 13.353 90.00 101.92 90.00 11591 Reflections read from file s92.hkl; mean (I/sigma) = 9.73 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5787 5790 5791 5809 8684 7731 7737 11591 N (int>3sigma) = 0 4038 3778 4000 3936 5908 5400 5346 8076 Mean intensity = 0.0 107.9 84.5 96.6 110.1 96.3 106.7 106.6 106.5 Mean int/sigma = 0.0 9.9 9.0 9.7 9.5 9.5 9.8 9.7 9.8 Lattice type: P chosen Volume: 1529.11 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 9.610 12.179 13.353 101.92 90.00 90.00 Niggli form: a.a = 92.35 b.b = 148.34 c.c = 178.29 b.c = -33.59 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.040 [ 7910] Cell: 12.179 9.610 13.353 90.00 101.92 90.00 Volume: 1529.11 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 5787 5790 5791 5809 8684 7731 7737 11591 N (int>3sigma) = 0 4038 3778 4000 3936 5908 5400 5346 8076 Mean intensity = 0.0 107.9 84.5 96.6 110.1 96.3 106.7 106.6 106.5 Mean int/sigma = 0.0 9.9 9.0 9.7 9.5 9.5 9.8 9.7 9.8 Crystal system M and Lattice type P selected Mean |E*E-1| = 1.002 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 7 345 345 350 N I>3s 1 145 148 3 0.9 93.3 93.3 1.2 1.3 6.4 6.5 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.040 7910 1.3 / 6.4 1.81 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C13 N5 S2 O2 H17 Formula weight = 339.44 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.474, non-H atomic volume = 17.4 and following cell contents and analysis: C 52.00 46.00 % H 68.00 5.05 % N 20.00 20.64 % O 8.00 9.43 % S 8.00 18.89 % F(000) = 712.0 Mo-K(alpha) radiation Mu (mm-1) = 0.36 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/n CELL 0.71073 12.1793 9.6098 13.3527 90.000 101.921 90.000 ZERR 4.00 0.0024 0.0019 0.0027 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 52 68 20 8 8 TREF HKLF 4 END -------------------------------------------------------------------------------