++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 13:40:23 on 24-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 17.088 21.400 21.730 90.00 91.32 90.00 45381 Reflections read from file s92.hkl; mean (I/sigma) = 5.30 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 22701 22695 22698 22688 34047 30249 30194 45381 N (int>3sigma) = 0 9413 8867 9278 9496 13779 12659 12593 18924 Mean intensity = 0.0 32.2 18.6 30.2 32.6 27.0 31.0 30.5 31.0 Mean int/sigma = 0.0 5.4 4.7 5.3 5.5 5.2 5.4 5.4 5.4 Lattice type: P chosen Volume: 7944.08 ------------------------------------------------------------------------------- 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: 17.088 21.400 21.730 90.00 91.32 90.00 Niggli form: a.a = 292.00 b.b = 457.95 c.c = 472.19 b.c = 0.00 a.c = -8.54 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.075 [ 27233] Cell: 17.088 21.400 21.730 90.00 91.32 90.00 Volume: 7944.08 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 22701 22695 22698 22688 34047 30249 30194 45381 N (int>3sigma) = 0 9413 8867 9278 9496 13779 12659 12593 18924 Mean intensity = 0.0 32.2 18.6 30.2 32.6 27.0 31.0 30.5 31.0 Mean int/sigma = 0.0 5.4 4.7 5.3 5.5 5.2 5.4 5.4 5.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.920 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 25 721 710 709 N I>3s 0 2 236 234 0.4 1.0 36.1 36.1 0.3 0.5 4.8 4.8 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 4 19410 0.075 27233 0.5 / 4.8 2.55 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C16 H34 N1 S1 O5 Formula weight = 352.50 Tentative Z (number of formula units/cell) = 18.0 giving rho = 1.326, non-H atomic volume = 19.2 and following cell contents and analysis: C 288.00 54.51 % H 612.00 9.72 % N 18.00 3.97 % O 90.00 22.69 % S 18.00 9.09 % F(000) = 3474.0 Mo-K(alpha) radiation Mu (mm-1) = 0.21 ------------------------------------------------------------------------------- File s93.ins set up as follows: TITL s93 in P2(1)/c CELL 0.71073 21.7299 21.3998 17.0880 90.000 91.318 90.000 ZERR 18.00 0.0043 0.0043 0.0034 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O S UNIT 288 612 18 90 18 TREF HKLF 4 END -------------------------------------------------------------------------------