++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 12:48:48 on 21-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.146 14.656 12.532 90.00 105.64 90.00 9439 Reflections read from file s92.hkl; mean (I/sigma) = 7.10 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4706 4698 4722 4712 7063 6277 6295 9439 N (int>3sigma) = 0 2511 2619 2512 2576 3821 3495 3464 5199 Mean intensity = 0.0 43.1 47.3 46.8 44.0 45.7 47.6 45.4 45.4 Mean int/sigma = 0.0 7.1 7.2 7.0 7.1 7.1 7.2 7.2 7.2 Lattice type: P chosen Volume: 1440.79 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 8.146 12.532 14.656 90.00 90.00 105.64 Niggli form: a.a = 66.36 b.b = 157.05 c.c = 214.80 b.c = 0.00 a.c = 0.00 a.b = -27.51 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.038 [ 6039] Cell: 8.146 14.656 12.532 90.00 105.64 90.00 Volume: 1440.79 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 4706 4698 4722 4712 7063 6277 6295 9439 N (int>3sigma) = 0 2511 2619 2512 2576 3821 3495 3464 5199 Mean intensity = 0.0 43.1 47.3 46.8 44.0 45.7 47.6 45.4 45.4 Mean int/sigma = 0.0 7.1 7.2 7.0 7.1 7.1 7.2 7.2 7.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.937 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 16 209 212 211 N I>3s 0 86 0 86 0.3 100.5 0.5 99.5 0.3 6.2 0.5 6.2 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.038 6039 0.5 / 6.2 1.83 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C14 H15 O3 S1 N3 Formula weight = 305.35 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.408, non-H atomic volume = 17.2 and following cell contents and analysis: C 56.00 55.06 % H 60.00 4.95 % N 12.00 13.76 % O 12.00 15.72 % S 4.00 10.50 % F(000) = 640.0 Mo-K(alpha) radiation Mu (mm-1) = 0.24 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/c CELL 0.71073 8.1459 14.6561 12.5319 90.000 105.635 90.000 ZERR 4.00 0.0016 0.0029 0.0025 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O S UNIT 56 60 12 12 4 TREF HKLF 4 END 9439 Reflections written to new reflection file s92.hkl -------------------------------------------------------------------------------