++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 09:08:31 on 30-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.970 12.766 11.500 90.00 107.27 90.00 11218 Reflections read from file s92.hkl; mean (I/sigma) = 10.09 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5621 5630 5629 5594 8440 7486 7469 11218 N (int>3sigma) = 0 4020 4147 4117 4139 6142 5476 5506 8240 Mean intensity = 0.0 113.5 117.1 116.6 116.2 115.7 114.8 112.9 117.5 Mean int/sigma = 0.0 9.9 10.3 10.2 10.3 10.1 10.2 10.1 10.2 Lattice type: P chosen Volume: 1537.79 ------------------------------------------------------------------------------- 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: 10.970 11.500 12.766 90.00 90.00 107.27 Niggli form: a.a = 120.35 b.b = 132.24 c.c = 162.96 b.c = 0.00 a.c = 0.00 a.b = -37.46 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.054 [ 7637] Cell: 10.970 12.766 11.500 90.00 107.27 90.00 Volume: 1537.79 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 5621 5630 5629 5594 8440 7486 7469 11218 N (int>3sigma) = 0 4020 4147 4117 4139 6142 5476 5506 8240 Mean intensity = 0.0 113.5 117.1 116.6 116.2 115.7 114.8 112.9 117.5 Mean int/sigma = 0.0 9.9 10.3 10.2 10.3 10.1 10.2 10.1 10.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.977 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 12 280 281 275 N I>3s 2 124 5 125 1.0 127.2 0.9 129.6 1.3 7.0 0.6 7.2 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.054 7637 1.3 / 7.0 1.57 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12 H15 N3 S1 O3 Formula weight = 281.33 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.215, non-H atomic volume = 20.2 and following cell contents and analysis: C 48.00 51.23 % H 60.00 5.37 % N 12.00 14.94 % O 12.00 17.06 % S 4.00 11.40 % F(000) = 592.0 Mo-K(alpha) radiation Mu (mm-1) = 0.22 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/c CELL 0.71073 10.9702 12.7656 11.4996 90.000 107.272 90.000 ZERR 4.00 0.0022 0.0026 0.0023 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O S UNIT 48 60 12 12 4 TREF HKLF 4 END -------------------------------------------------------------------------------