++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 15:43:18 on 31-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.512 7.940 11.213 75.67 86.60 75.93 4557 Reflections read from file s92.hkl; mean (I/sigma) = 12.77 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2274 2274 2276 2279 3412 3050 3052 4557 N (int>3sigma) = 0 1861 1854 1831 1898 2773 2490 2451 3721 Mean intensity = 0.0 204.3 208.6 203.0 214.6 205.3 209.8 195.6 212.4 Mean int/sigma = 0.0 12.8 12.7 12.8 12.9 12.8 12.9 12.6 12.8 Lattice type: P chosen Volume: 544.88 ------------------------------------------------------------------------------- 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: 6.512 7.940 11.213 75.67 86.60 75.93 Niggli form: a.a = 42.40 b.b = 63.05 c.c = 125.73 b.c = 22.04 a.c = 4.32 a.b = 12.57 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.036 [ 2414] Cell: 6.512 7.940 11.213 75.67 86.60 75.93 Volume: 544.88 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 2274 2274 2276 2279 3412 3050 3052 4557 N (int>3sigma) = 0 1861 1854 1831 1898 2773 2490 2451 3721 Mean intensity = 0.0 204.3 208.6 203.0 214.6 205.3 209.8 195.6 212.4 Mean int/sigma = 0.0 12.8 12.7 12.8 12.9 12.8 12.9 12.6 12.8 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.940 [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 0.036 2414 0.0 / 12.8 0.87 [B] P1 # 1 chiral 1 700 0.036 2414 0.0 / 12.8 5.09 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C10 S2 O2 N2 H9 Formula weight = 253.31 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.544, non-H atomic volume = 17.0 and following cell contents and analysis: C 20.00 47.41 % H 18.00 3.58 % N 4.00 11.06 % O 4.00 12.63 % S 4.00 25.31 % F(000) = 262.0 Mo-K(alpha) radiation Mu (mm-1) = 0.47 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P-1 CELL 0.71073 6.5117 7.9405 11.2128 75.668 86.605 75.932 ZERR 2.00 0.0013 0.0016 0.0022 0.030 0.030 0.030 LATT 1 SFAC C H N O S UNIT 20 18 4 4 4 TREF HKLF 4 END -------------------------------------------------------------------------------