++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 15:30:41 on 10-JAN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 12.732 13.131 13.040 90.00 96.88 90.00 16818 Reflections read from file s92.hkl; mean (I/sigma) = 6.55 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8425 8410 8409 8428 12622 11223 11198 16818 N (int>3sigma) = 0 4236 4228 4228 4055 6346 5710 5682 8539 Mean intensity = 0.0 34.4 35.6 36.1 29.2 35.4 35.4 34.6 34.4 Mean int/sigma = 0.0 6.5 6.7 6.7 6.3 6.6 6.7 6.6 6.7 Lattice type: P chosen Volume: 2164.33 ------------------------------------------------------------------------------- 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: 12.732 13.040 13.131 90.00 90.00 96.88 Niggli form: a.a = 162.11 b.b = 170.03 c.c = 172.41 b.c = 0.00 a.c = 0.00 a.b = -19.88 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.054 [ 11656] Cell: 12.732 13.131 13.040 90.00 96.88 90.00 Volume: 2164.33 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 8425 8410 8409 8428 12622 11223 11198 16818 N (int>3sigma) = 0 4236 4228 4228 4055 6346 5710 5682 8539 Mean intensity = 0.0 34.4 35.6 36.1 29.2 35.4 35.4 34.6 34.4 Mean int/sigma = 0.0 6.5 6.7 6.7 6.3 6.6 6.7 6.6 6.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 1.008 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 21 358 351 355 N I>3s 1 125 125 0 0.5 103.8 105.8 0.6 0.8 6.0 6.2 0.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.054 11656 0.8 / 6.0 1.95 Option [A] chosen ------------------------------------------------------------------------------- ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C21H20O5S3 Formula weight = 448.55 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.377, non-H atomic volume = 18.7 and following cell contents and analysis: C 84.00 56.23 % H 80.00 4.49 % O 20.00 17.84 % S 12.00 21.44 % F(000) = 936.0 Mo-K(alpha) radiation Mu (mm-1) = 0.37 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/n CELL 0.71073 12.7323 13.1306 13.0397 90.000 96.876 90.000 ZERR 4.00 0.0025 0.0026 0.0026 0.000 0.030 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H O S UNIT 84 80 20 12 TREF HKLF 4 END -------------------------------------------------------------------------------