++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0022 started at 11:35:43 on 26-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.329 8.698 13.747 90.00 97.36 90.00 15465 Reflections read from file 06skc0022.hkl; mean (I/sigma) = 3.76 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7740 7697 7745 7762 11591 10337 10328 15465 N (int>3sigma) = 0 3185 3287 3044 3299 4758 4302 4374 6473 Mean intensity = 0.0 268.7 277.2 261.9 279.9 269.2 269.3 271.3 270.7 Mean int/sigma = 0.0 3.9 4.0 3.7 3.8 3.8 3.8 3.9 3.9 Lattice type: P chosen Volume: 1224.77 ------------------------------------------------------------------------------- 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: 8.698 10.329 13.747 97.36 90.00 90.00 Niggli form: a.a = 75.65 b.b = 106.69 c.c = 188.97 b.c = -18.19 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.132 [ 12461] Cell: 10.329 8.698 13.747 90.00 97.36 90.00 Volume: 1224.77 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.117 [ 9987] Cell: 8.698 10.329 13.747 82.64 90.00 90.00 Volume: 1224.77 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 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 7740 7697 7745 7762 11591 10337 10328 15465 N (int>3sigma) = 0 3185 3287 3044 3299 4758 4302 4374 6473 Mean intensity = 0.0 268.7 277.2 261.9 279.9 269.2 269.3 271.3 270.7 Mean int/sigma = 0.0 3.9 4.0 3.7 3.8 3.8 3.8 3.9 3.9 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.890 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 16 532 529 529 N I>3s 0 1 164 165 14.2 18.1 350.6 351.9 0.5 0.6 3.5 3.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 4 19410 0.132 12461 0.6 / 3.5 4.06 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12H15O4N1S1 Formula weight = 269.31 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.461, non-H atomic volume = 17.0 and following cell contents and analysis: C 48.00 53.51 % H 60.00 5.61 % N 4.00 5.20 % O 16.00 23.76 % S 4.00 11.90 % F(000) = 568.0 Mo-K(alpha) radiation Mu (mm-1) = 0.27 ------------------------------------------------------------------------------- File 06skc0022p21c.ins set up as follows: TITL 06skc0022p21c in P2(1)/c CELL 0.71073 13.7465 8.6976 10.3290 90.000 97.361 90.000 ZERR 4.00 0.0012 0.0008 0.0006 0.000 0.005 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O S UNIT 48 60 4 16 4 TEMP 0.01 TREF HKLF 4 END 15465 Reflections written to new reflection file 06skc0022p21c.hkl -------------------------------------------------------------------------------