++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 13:20:20 on 20-APR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.823 12.944 17.369 90.00 95.67 90.00 15087 Reflections read from file s92.hkl; mean (I/sigma) = 10.22 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7557 7541 7534 7540 11316 10066 10053 15087 N (int>3sigma) = 0 6215 6291 6244 6249 9375 8379 8297 12456 Mean intensity = 0.0 89.1 88.8 88.1 89.5 88.7 89.1 88.8 88.7 Mean int/sigma = 0.0 10.2 10.3 10.2 10.2 10.2 10.3 10.3 10.2 Lattice type: P chosen Volume: 1750.25 ------------------------------------------------------------------------------- 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: 7.823 12.944 17.369 90.00 95.67 90.00 Niggli form: a.a = 61.20 b.b = 167.56 c.c = 301.67 b.c = 0.00 a.c = -13.42 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.088 [ 10895] Cell: 7.823 12.944 17.369 90.00 95.67 90.00 Volume: 1750.25 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 7557 7541 7534 7540 11316 10066 10053 15087 N (int>3sigma) = 0 6215 6291 6244 6249 9375 8379 8297 12456 Mean intensity = 0.0 89.1 88.8 88.1 89.5 88.7 89.1 88.8 88.7 Mean int/sigma = 0.0 10.2 10.3 10.2 10.2 10.2 10.3 10.3 10.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.765 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 15 410 406 406 N I>3s 0 331 315 324 0.5 146.5 155.0 160.2 0.5 10.9 10.5 11.2 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1) # 4 chiral 1 3543 0.088 10895 0.5 / 10.2 1.09 [B] P2(1)/m # 11 centro 1 402 0.088 10895 0.5 / 10.2 5.33 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C30 N2 O10 S1 Formula weight = 580.38 Tentative Z (number of formula units/cell) = 3.0 giving rho = 1.652, non-H atomic volume = 13.6 and following cell contents and analysis: C 90.00 62.08 % N 6.00 4.83 % O 30.00 27.57 % S 3.00 5.52 % F(000) = 870.0 Mo-K(alpha) radiation Mu (mm-1) = 0.21 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1) CELL 0.71073 7.8231 12.9445 17.3686 90.000 95.668 90.000 ZERR 3.00 0.0016 0.0026 0.0035 0.000 0.030 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C N O S UNIT 90 6 30 3 TREF HKLF 4 END -------------------------------------------------------------------------------