++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0019 started at 14:31:12 on 12-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 5.689 8.964 13.246 90.00 97.11 90.00 8560 Reflections read from file 06skc0019.hkl; mean (I/sigma) = 6.38 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4288 4304 4276 4273 6434 5693 5695 8560 N (int>3sigma) = 0 2901 2915 2784 2849 4300 3783 3769 5700 Mean intensity = 0.0 505.7 495.7 487.7 542.5 496.4 508.8 518.8 509.8 Mean int/sigma = 0.0 6.5 6.4 6.3 6.5 6.4 6.4 6.4 6.4 Lattice type: P chosen Volume: 670.26 ------------------------------------------------------------------------------- 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: 5.689 8.964 13.246 90.00 97.11 90.00 Niggli form: a.a = 32.36 b.b = 80.35 c.c = 175.45 b.c = 0.00 a.c = -9.33 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.085 [ 6913] Cell: 5.689 8.964 13.246 90.00 97.11 90.00 Volume: 670.26 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 4288 4304 4276 4273 6434 5693 5695 8560 N (int>3sigma) = 0 2901 2915 2784 2849 4300 3783 3769 5700 Mean intensity = 0.0 505.7 495.7 487.7 542.5 496.4 508.8 518.8 509.8 Mean int/sigma = 0.0 6.5 6.4 6.3 6.5 6.4 6.4 6.4 6.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.694 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 12 296 288 286 N I>3s 0 179 175 162 21.8 694.8 695.6 643.4 0.6 6.7 6.5 6.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1) # 4 chiral 1 3543 0.085 6913 0.6 / 6.4 1.76 [B] P2(1)/m # 11 centro 1 402 0.085 6913 0.6 / 6.4 9.30 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C14H17O3N1S1 Formula weight = 279.35 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.384, non-H atomic volume = 17.6 and following cell contents and analysis: C 28.00 60.19 % H 34.00 6.13 % N 2.00 5.02 % O 6.00 17.18 % S 2.00 11.48 % F(000) = 296.0 Mo-K(alpha) radiation Mu (mm-1) = 0.24 ------------------------------------------------------------------------------- File 06skc0019p21.ins set up as follows: TITL 06skc0019p21 in P2(1) CELL 0.71073 5.6889 8.9638 13.2457 90.000 97.112 90.000 ZERR 2.00 0.0004 0.0004 0.0011 0.000 0.003 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O S UNIT 28 34 2 6 2 TEMP 0.01 TREF HKLF 4 END 8560 Reflections written to new reflection file 06skc0019p21.hkl -------------------------------------------------------------------------------