++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 13:44:48 on 13-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.810 10.575 24.736 90.00 90.00 90.00 11021 Reflections read from file s92.hkl; mean (I/sigma) = 6.94 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5503 5505 5518 5508 8263 7345 7333 11021 N (int>3sigma) = 0 2979 3138 3217 3143 4667 4365 4366 6558 Mean intensity = 0.0 26.0 37.5 35.9 33.7 33.1 39.8 39.4 38.7 Mean int/sigma = 0.0 6.2 6.8 6.8 6.8 6.6 7.0 7.0 7.0 Lattice type: P chosen Volume: 2304.35 ------------------------------------------------------------------------------- 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: 8.810 10.575 24.736 90.00 90.00 90.00 Niggli form: a.a = 77.61 b.b = 111.82 c.c = 611.85 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(int) = 0.047 [ 8028] Cell: 8.810 10.575 24.736 90.00 90.00 90.00 Volume: 2304.35 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 5503 5505 5518 5508 8263 7345 7333 11021 N (int>3sigma) = 0 2979 3138 3217 3143 4667 4365 4366 6558 Mean intensity = 0.0 26.0 37.5 35.9 33.7 33.1 39.8 39.4 38.7 Mean int/sigma = 0.0 6.2 6.8 6.8 6.8 6.6 7.0 7.0 7.0 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.999 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 453 439 440 4 319 321 320 9 132 128 130 18 N I>3s 1 149 150 0 1 118 119 0 0 42 42 0 0.6 34.1 34.0 0.2 0.5 40.5 40.6 0.5 0.5 21.1 20.7 0.5 0.5 4.9 4.8 0.3 0.5 4.7 4.7 0.5 0.5 5.2 5.1 0.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pbca # 61 centro 1 2293 0.047 8028 0.5 / 4.7 2.50 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) = 8.0 giving rho = 1.431, non-H atomic volume = 16.9 and following cell contents and analysis: C 96.00 58.04 % H 96.00 4.87 % N 16.00 11.28 % O 16.00 12.89 % S 8.00 12.91 % F(000) = 1040.0 Mo-K(alpha) radiation Mu (mm-1) = 0.27 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in Pbca CELL 0.71073 8.8098 10.5745 24.7356 90.000 90.000 90.000 ZERR 8.00 0.0018 0.0021 0.0049 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O S UNIT 96 96 16 16 8 TREF HKLF 4 END -------------------------------------------------------------------------------