++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 16:24:09 on 10-AUG-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.218 8.835 16.655 90.00 99.09 90.00 13164 Reflections read from file s92.hkl; mean (I/sigma) = 10.35 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6581 6585 6570 6570 9868 8791 8774 13164 N (int>3sigma) = 0 4624 4793 4817 4750 7117 6388 6369 9628 Mean intensity = 0.0 101.6 113.9 105.6 111.8 107.1 113.1 113.1 111.8 Mean int/sigma = 0.0 10.1 10.3 10.2 10.3 10.2 10.4 10.4 10.4 Lattice type: P chosen Volume: 1484.64 ------------------------------------------------------------------------------- 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: 8.835 10.218 16.655 99.09 90.00 90.00 Niggli form: a.a = 78.05 b.b = 104.42 c.c = 277.40 b.c = -26.90 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.042 [ 9553] Cell: 10.218 8.835 16.655 90.00 99.09 90.00 Volume: 1484.64 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 6581 6585 6570 6570 9868 8791 8774 13164 N (int>3sigma) = 0 4624 4793 4817 4750 7117 6388 6369 9628 Mean intensity = 0.0 101.6 113.9 105.6 111.8 107.1 113.1 113.1 111.8 Mean int/sigma = 0.0 10.1 10.3 10.2 10.3 10.2 10.4 10.4 10.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.932 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 12 467 479 474 N I>3s 0 202 6 206 0.7 141.9 0.7 139.8 0.8 6.8 0.6 6.8 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.042 9553 0.8 / 6.8 1.75 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12 H13 N2 S1 O2 Formula weight = 249.30 Tentative Z (number of formula units/cell) = 5.0 giving rho = 1.394, non-H atomic volume = 17.5 and following cell contents and analysis: C 60.00 57.81 % H 65.00 5.26 % N 10.00 11.24 % O 10.00 12.84 % S 5.00 12.86 % F(000) = 655.0 Mo-K(alpha) radiation Mu (mm-1) = 0.26 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/c CELL 0.71073 10.2184 8.8345 16.6552 90.000 99.094 90.000 ZERR 5.00 0.0020 0.0018 0.0033 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O S UNIT 60 65 10 10 5 TREF HKLF 4 END -------------------------------------------------------------------------------