++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0020 started at 17:27:15 on 02-NOV-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 5.694 7.104 23.756 90.00 90.00 90.00 8277 Reflections read from file 06skc0020.hkl; mean (I/sigma) = 5.03 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4139 4132 4133 4132 6202 5525 5510 8277 N (int>3sigma) = 0 2325 2364 2397 2327 3543 3153 3155 4771 Mean intensity = 0.0 113.9 118.2 113.1 104.5 115.1 113.4 113.0 114.4 Mean int/sigma = 0.0 5.1 5.1 5.1 5.0 5.1 5.1 5.1 5.1 Lattice type: P chosen Volume: 960.95 ------------------------------------------------------------------------------- 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: 5.694 7.104 23.756 90.00 90.00 90.00 Niggli form: a.a = 32.43 b.b = 50.46 c.c = 564.35 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(int) = 0.089 [ 6939] Cell: 5.694 7.104 23.756 90.00 90.00 90.00 Volume: 960.95 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 4139 4132 4133 4132 6202 5525 5510 8277 N (int>3sigma) = 0 2325 2364 2397 2327 3543 3153 3155 4771 Mean intensity = 0.0 113.9 118.2 113.1 104.5 115.1 113.4 113.0 114.4 Mean int/sigma = 0.0 5.1 5.1 5.1 5.0 5.1 5.1 5.1 5.1 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.852 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 523 518 519 6 385 387 382 9 102 99 97 40 N I>3s 274 269 255 0 1 159 160 1 37 38 1 1 113.2 81.2 126.0 3.8 3.8 185.6 188.1 10.4 266.5 275.0 4.6 7.0 4.5 4.3 4.5 1.0 0.6 4.3 4.4 1.4 4.8 5.0 0.7 0.9 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pna2(1) # 33 non-cen 4 903 0.089 6939 1.4 / 4.3 4.21 [B] Pnma # 62 centro 5 894 0.089 6939 1.4 / 4.3 4.21 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H13O3N1S1 Formula weight = 203.25 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.405, non-H atomic volume = 18.5 and following cell contents and analysis: C 32.00 47.27 % H 52.00 6.45 % N 4.00 6.89 % O 12.00 23.62 % S 4.00 15.77 % F(000) = 432.0 Mo-K(alpha) radiation Mu (mm-1) = 0.31 ------------------------------------------------------------------------------- File 06skc0020pna21.ins set up as follows: TITL 06skc0020pna21 in Pna2(1) CELL 0.71073 23.7560 7.1036 5.6944 90.000 90.000 90.000 ZERR 4.00 0.0012 0.0004 0.0002 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, 0.5-Y, Z SYMM 0.5-X, 0.5+Y, 0.5+Z SFAC C H N O S UNIT 32 52 4 12 4 TEMP 0.2 TREF HKLF 4 END 8277 Reflections written to new reflection file 06skc0020pna21.hkl -------------------------------------------------------------------------------