++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 16:39:52 on 27-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.748 5.919 14.655 90.00 99.30 90.00 6346 Reflections read from file s92.hkl; mean (I/sigma) = 5.65 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3164 3176 3172 3171 4756 4223 4218 6346 N (int>3sigma) = 0 1732 1877 1877 1848 2743 2398 2502 3736 Mean intensity = 0.0 37.6 42.8 43.5 42.1 41.3 37.6 42.5 41.5 Mean int/sigma = 0.0 5.4 5.7 5.8 5.7 5.6 5.5 5.8 5.7 Lattice type: P chosen Volume: 1005.61 ------------------------------------------------------------------------------- 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: 5.919 11.748 14.655 99.30 90.00 90.00 Niggli form: a.a = 35.03 b.b = 138.02 c.c = 214.77 b.c = -27.84 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.051 [ 4075] Cell: 11.748 5.919 14.655 90.00 99.30 90.00 Volume: 1005.61 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 3164 3176 3172 3171 4756 4223 4218 6346 N (int>3sigma) = 0 1732 1877 1877 1848 2743 2398 2502 3736 Mean intensity = 0.0 37.6 42.8 43.5 42.1 41.3 37.6 42.5 41.5 Mean int/sigma = 0.0 5.4 5.7 5.8 5.7 5.6 5.5 5.8 5.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.968 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 5 379 376 379 N I>3s 0 158 0 158 0.4 79.7 0.6 79.7 0.5 4.5 0.5 4.6 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.051 4075 0.5 / 4.5 2.46 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C10 H9 N3 S1 O2 Formula weight = 235.26 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.554, non-H atomic volume = 15.7 and following cell contents and analysis: C 40.00 51.05 % H 36.00 3.86 % N 12.00 17.87 % O 8.00 13.60 % S 4.00 13.63 % F(000) = 488.0 Mo-K(alpha) radiation Mu (mm-1) = 0.31 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/c CELL 0.71073 11.7481 5.9187 14.6551 90.000 99.304 90.000 ZERR 4.00 0.0023 0.0012 0.0029 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O S UNIT 40 36 12 8 4 TREF HKLF 4 END -------------------------------------------------------------------------------