++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 15:15:15 on 17-APR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.608 15.212 15.257 67.79 84.48 73.89 22373 Reflections read from file s92.hkl; mean (I/sigma) = 3.37 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 11132 11220 11206 11159 16779 14906 14933 22373 N (int>3sigma) = 0 3886 3833 3787 3709 5753 5056 5038 7601 Mean intensity = 0.0 7.3 7.3 7.1 7.1 7.2 7.2 7.3 7.4 Mean int/sigma = 0.0 3.6 3.5 3.5 3.5 3.6 3.5 3.5 3.5 Lattice type: P chosen Volume: 1776.85 ------------------------------------------------------------------------------- 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: 8.608 15.212 15.257 67.79 84.48 73.89 Niggli form: a.a = 74.10 b.b = 231.39 c.c = 232.79 b.c = 87.75 a.c = 12.64 a.b = 36.34 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.125 [ 14645] Cell: 8.608 15.212 15.257 67.79 84.48 73.89 Volume: 1776.85 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 11132 11220 11206 11159 16779 14906 14933 22373 N (int>3sigma) = 0 3886 3833 3787 3709 5753 5056 5038 7601 Mean intensity = 0.0 7.3 7.3 7.1 7.1 7.2 7.2 7.3 7.4 Mean int/sigma = 0.0 3.6 3.5 3.5 3.5 3.6 3.5 3.5 3.5 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.925 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P-1 # 2 centro 1 8646 0.125 14645 0.0 / 3.5 3.03 [B] P1 # 1 chiral 1 700 0.125 14645 0.0 / 3.5 6.56 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C25 H30 O10 N5 S1 Formula weight = 592.60 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.108, non-H atomic volume = 21.7 and following cell contents and analysis: C 50.00 50.67 % H 60.00 5.10 % N 10.00 11.82 % O 20.00 27.00 % S 2.00 5.41 % F(000) = 622.0 Mo-K(alpha) radiation Mu (mm-1) = 0.14 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P-1 CELL 0.71073 8.6082 15.2116 15.2575 67.786 84.475 73.886 ZERR 2.00 0.0004 0.0006 0.0008 0.002 0.001 0.003 LATT 1 SFAC C H N O S UNIT 50 60 10 20 2 TREF HKLF 4 END -------------------------------------------------------------------------------