++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src0079 started at 13:27:39 on 09-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 15.800 5.176 16.979 90.00 99.72 90.00 14519 Reflections read from file 2007src0079.hkl; mean (I/sigma) = 7.23 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7282 7202 7280 7234 10882 9680 9657 14519 N (int>3sigma) = 0 4959 4644 4923 4695 7263 6669 6595 9954 Mean intensity = 0.0 130.6 108.5 135.1 128.9 124.8 140.0 139.6 139.7 Mean int/sigma = 0.0 7.3 6.9 7.3 6.8 7.1 7.3 7.3 7.3 Lattice type: P chosen Volume: 1368.70 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 5.176 15.800 16.979 99.72 90.00 90.00 Niggli form: a.a = 26.79 b.b = 249.66 c.c = 288.27 b.c = -45.31 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.053 [ 11025] Cell: 15.800 5.176 16.979 90.00 99.72 90.00 Volume: 1368.70 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 7282 7202 7280 7234 10882 9680 9657 14519 N (int>3sigma) = 0 4959 4644 4923 4695 7263 6669 6595 9954 Mean intensity = 0.0 130.6 108.5 135.1 128.9 124.8 140.0 139.6 139.7 Mean int/sigma = 0.0 7.3 6.9 7.3 6.8 7.1 7.3 7.3 7.3 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 9 873 875 842 N I>3s 0 365 370 7 1.0 157.3 157.3 2.3 0.7 5.4 5.4 0.7 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.053 11025 0.7 / 5.4 2.38 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C13H13N1O5S1 Formula weight = 295.30 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.433, non-H atomic volume = 17.1 and following cell contents and analysis: C 52.00 52.87 % H 52.00 4.44 % N 4.00 4.74 % O 20.00 27.09 % S 4.00 10.86 % F(000) = 616.0 Mo-K(alpha) radiation Mu (mm-1) = 0.25 ------------------------------------------------------------------------------- File 2007src0079.ins set up as follows: TITL 2007src0079 in P2(1)/n CELL 0.71073 15.8005 5.1763 16.9786 90.000 99.723 90.000 ZERR 4.00 0.0006 0.0001 0.0006 0.000 0.002 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O S UNIT 52 52 4 20 4 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------