++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 10:45:24 on 04-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 13.681 5.845 14.858 90.00 114.97 90.00 8071 Reflections read from file s92.hkl; mean (I/sigma) = 8.60 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4046 4037 4029 4017 6056 5382 5379 8071 N (int>3sigma) = 0 2693 2895 2882 2834 4235 3844 3798 5718 Mean intensity = 0.0 83.2 89.7 94.5 94.7 89.1 91.8 92.6 90.3 Mean int/sigma = 0.0 8.1 8.7 8.7 8.6 8.5 8.7 8.6 8.7 Lattice type: P chosen Volume: 1077.08 ------------------------------------------------------------------------------- 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: 5.845 13.681 14.858 114.97 90.00 90.00 Niggli form: a.a = 34.16 b.b = 187.16 c.c = 220.78 b.c = -85.80 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.043 [ 5443] Cell: 13.681 5.845 14.858 90.00 114.97 90.00 Volume: 1077.08 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 4046 4037 4029 4017 6056 5382 5379 8071 N (int>3sigma) = 0 2693 2895 2882 2834 4235 3844 3798 5718 Mean intensity = 0.0 83.2 89.7 94.5 94.7 89.1 91.8 92.6 90.3 Mean int/sigma = 0.0 8.1 8.7 8.7 8.6 8.5 8.7 8.6 8.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.948 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 5 541 540 541 N I>3s 0 239 7 238 1.0 161.8 0.7 161.8 0.5 6.3 0.6 6.3 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.043 5443 0.6 / 6.3 1.80 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C10 H10 N4 S1 O2 Formula weight = 250.28 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.543, non-H atomic volume = 15.8 and following cell contents and analysis: C 40.00 47.99 % H 40.00 4.03 % N 16.00 22.39 % O 8.00 12.79 % S 4.00 12.81 % F(000) = 520.0 Mo-K(alpha) radiation Mu (mm-1) = 0.30 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/c CELL 0.71073 13.6805 5.8449 14.8585 90.000 114.966 90.000 ZERR 4.00 0.0027 0.0012 0.0030 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O S UNIT 40 40 16 8 4 TREF HKLF 4 END -------------------------------------------------------------------------------