++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 16:51:49 on 13-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 18.931 9.413 14.701 90.00 115.96 90.00 7863 Reflections read from file s92.hkl; mean (I/sigma) = 5.57 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3929 3929 0 3933 3929 5245 5244 7863 N (int>3sigma) = 0 1863 1863 0 1901 1863 2635 2630 3959 Mean intensity = 0.0 14.4 14.4 0.0 14.5 14.4 18.1 17.7 17.9 Mean int/sigma = 0.0 5.2 5.2 0.0 5.2 5.2 5.7 5.7 5.7 Lattice type: C chosen Volume: 2355.35 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 -0.5000 -1.0000 Unitcell: 9.413 10.571 14.354 70.42 70.86 63.56 Niggli form: a.a = 88.60 b.b = 111.75 c.c = 206.04 b.c = 50.84 a.c = 44.30 a.b = 44.30 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC C-lattice R(int) = 0.070 [ 5194] Cell: 18.931 9.413 14.701 90.00 115.96 90.00 Volume: 2355.35 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC I-lattice R(int) = 0.070 [ 5194] Cell: 14.701 9.413 18.190 90.00 110.65 90.00 Volume: 2355.35 Matrix: 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3929 3929 0 3933 3929 5245 5244 7863 N (int>3sigma) = 0 1863 1863 0 1901 1863 2635 2630 3959 Mean intensity = 0.0 14.4 14.4 0.0 14.5 14.4 18.1 17.7 17.9 Mean int/sigma = 0.0 5.2 5.2 0.0 5.2 5.2 5.7 5.7 5.7 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.956 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 229 N I>3s 0 0.4 0.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.070 5194 0.4 / 5.7 1.93 [B] Cc # 9 non-cen 1 566 0.070 5194 0.4 / 5.7 6.91 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12 H12 S1 O2 N2 Formula weight = 248.30 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.400, non-H atomic volume = 17.3 and following cell contents and analysis: C 96.00 58.04 % H 96.00 4.87 % N 16.00 11.28 % O 16.00 12.89 % S 8.00 12.91 % F(000) = 1040.0 Mo-K(alpha) radiation Mu (mm-1) = 0.27 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in C2/c CELL 0.71073 18.9310 9.4130 14.7006 90.000 115.957 90.000 ZERR 8.00 0.0038 0.0019 0.0029 0.000 0.030 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O S UNIT 96 96 16 16 8 TREF HKLF 4 END -------------------------------------------------------------------------------