++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 15:39:20 on 22-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 15.837 8.625 18.643 90.00 94.14 90.00 9608 Reflections read from file s92.hkl; mean (I/sigma) = 5.35 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4795 4795 0 4805 4795 6420 6396 9608 N (int>3sigma) = 0 2442 2442 0 2202 2442 3286 3226 4885 Mean intensity = 0.0 21.1 21.1 0.0 15.5 21.1 23.1 21.4 21.9 Mean int/sigma = 0.0 5.4 5.4 0.0 4.8 5.4 5.5 5.4 5.5 Lattice type: C chosen Volume: 2539.87 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 Unitcell: 8.625 9.017 18.643 86.37 90.00 61.43 Niggli form: a.a = 74.39 b.b = 81.30 c.c = 347.57 b.c = 10.66 a.c = 0.00 a.b = 37.19 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC C-lattice R(int) = 0.058 [ 6519] Cell: 15.837 8.625 18.643 90.00 94.14 90.00 Volume: 2539.87 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 4795 4795 0 4805 4795 6420 6396 9608 N (int>3sigma) = 0 2442 2442 0 2202 2442 3286 3226 4885 Mean intensity = 0.0 21.1 21.1 0.0 15.5 21.1 23.1 21.4 21.9 Mean int/sigma = 0.0 5.4 5.4 0.0 4.8 5.4 5.5 5.4 5.5 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.928 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 309 N I>3s 1 0.5 0.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.058 6519 0.4 / 5.5 2.16 [B] Cc # 9 non-cen 1 566 0.058 6519 0.4 / 5.5 5.85 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12 H13 N3 S1 O2 Formula weight = 263.31 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.377, non-H atomic volume = 17.6 and following cell contents and analysis: C 96.00 54.73 % H 104.00 4.98 % N 24.00 15.96 % O 16.00 12.15 % S 8.00 12.18 % F(000) = 1104.0 Mo-K(alpha) radiation Mu (mm-1) = 0.25 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in C2/c CELL 0.71073 15.8373 8.6247 18.6432 90.000 94.139 90.000 ZERR 8.00 0.0032 0.0017 0.0037 0.000 0.030 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O S UNIT 96 104 24 16 8 TREF HKLF 4 END -------------------------------------------------------------------------------