++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0076 started at 14:39:54 on 27-NOV-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 4.923 11.373 14.094 82.68 90.02 89.99 12224 Reflections read from file 06skc0076.hkl; mean (I/sigma) = 6.30 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6131 6115 6058 6120 9152 8166 8119 12224 N (int>3sigma) = 0 3875 3873 3210 3899 5479 5147 5091 7710 Mean intensity = 0.0 246.0 238.8 125.9 231.2 203.9 237.8 239.8 241.4 Mean int/sigma = 0.0 6.4 6.5 5.1 6.4 6.0 6.4 6.3 6.4 Lattice type: P chosen Volume: 782.63 ------------------------------------------------------------------------------- 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: 4.923 11.373 14.094 97.32 90.02 90.01 Niggli form: a.a = 24.23 b.b = 129.35 c.c = 198.64 b.c = -20.43 a.c = -0.02 a.b = -0.01 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.019 deg. MONOCLINIC P-lattice R(int) = 0.073 [ 10201] Cell: 11.373 4.923 14.094 89.98 97.32 89.99 Volume: 782.63 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 6115 6131 6058 6120 9152 8166 8119 12224 N (int>3sigma) = 0 3873 3875 3210 3899 5479 5147 5091 7710 Mean intensity = 0.0 238.8 246.0 125.9 231.2 203.9 237.8 239.8 241.4 Mean int/sigma = 0.0 6.5 6.4 5.1 6.4 6.0 6.4 6.3 6.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.925 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 13 743 774 783 N I>3s 0 1 336 335 4.1 4.9 379.1 374.9 0.5 0.6 5.6 5.6 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 4 19410 0.073 10201 0.6 / 5.6 2.21 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C11H22O4N2S1 Formula weight = 278.37 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.181, non-H atomic volume = 21.7 and following cell contents and analysis: C 22.00 47.46 % H 44.00 7.97 % N 4.00 10.07 % O 8.00 22.99 % S 2.00 11.52 % F(000) = 300.0 Mo-K(alpha) radiation Mu (mm-1) = 0.22 ------------------------------------------------------------------------------- File 06skc0076p21c.ins set up as follows: TITL 06skc0076p21c in P2(1)/c CELL 0.71073 14.0939 4.9227 11.3731 90.000 97.321 90.000 ZERR 2.00 0.0006 0.0002 0.0005 0.000 0.003 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O S UNIT 22 44 4 8 2 TEMP 0.02 TREF HKLF 4 END 12224 Reflections written to new reflection file 06skc0076p21c.hkl -------------------------------------------------------------------------------