XPREP - RECIPROCAL SPACE EXPLORATION ------------------------------------- Original cell in Angstroms and degrees: 7.205 13.880 11.754 90.00 107.18 90.00 8740 reflections read from file s92.HKL Mean(I/sigma) = 7.25 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4387 4382 4371 4377 6570 5810 5823 8740 N (int>3sigma) = 0 2935 2920 2905 2922 4380 3945 3920 5889 Mean intensity = 0.0 211.7 216.7 182.4 186.0 203.7 212.3 211.0 213.1 Mean int/sigma = 0.0 7.3 7.2 7.1 7.1 7.2 7.4 7.3 7.3 Lattice type P chosen Volume: 1123.03 ------------------------------------------------------------------------------- Determination of reduced (Niggli) cell Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.205 11.754 13.880 90.00 90.00 107.18 Niggli form: a.a = 51.92 b.b = 138.15 c.c = 192.65 b.c = 0.00 a.c = 0.00 a.b = -25.01 ------------------------------------------------------------------------------- Search for higher METRIC symmetry ------------------------------------------------------------------------------- Option A: FOM = 0.669 deg. ORTHORHOMBIC C-lattice R(int) = 0.235 [ 5339] Cell: 7.205 22.460 13.880 90.00 90.00 89.33 Volume: 2246.06 Matrix: -1.0000 0.0000 0.0000 -1.0000 0.0000 -2.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------- Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.039 [ 4767] Cell: 7.205 13.880 11.754 90.00 107.18 90.00 Volume: 1123.03 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------- Option C: FOM = 0.669 deg. MONOCLINIC C-lattice R(int) = 0.225 [ 4505] Cell: 22.460 7.205 13.880 90.00 90.00 90.67 Volume: 2246.06 Matrix: -1.0000 0.0000 -2.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------- Option D: FOM = 0.669 deg. MONOCLINIC C-lattice R(int) = 0.217 [ 4583] Cell: 7.205 22.460 13.880 90.00 90.00 89.33 Volume: 2246.06 Matrix: -1.0000 0.0000 0.0000 -1.0000 0.0000 -2.0000 0.0000 -1.0000 0.0000 Option B selected ------------------------------------------------------------------------------- Space group determination Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4387 4382 4371 4377 6570 5810 5823 8740 N (int>3sigma) = 0 2935 2920 2905 2922 4380 3945 3920 5889 Mean intensity = 0.0 211.7 216.7 182.4 186.0 203.7 212.3 211.0 213.1 Mean int/sigma = 0.0 7.3 7.2 7.1 7.1 7.2 7.4 7.3 7.3 Crystal system M and Lattice type P selected Mean |E*E-1| = 1.015 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 12 210 217 213 N I>3s 0 6 97 99 3.2 2.2 509.8 519.5 0.6 0.6 6.5 6.7 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 4 19410 0.039 4767 0.6 / 6.5 1.90 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12 H12 N2 O2 S1 Formula weight = 248.30 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.469, non-H atomic volume = 16.5 and following cell contents and analysis: C 48.00 58.05 % H 48.00 4.87 % N 8.00 11.28 % O 8.00 12.89 % S 4.00 12.91 % F(000) = 520.0 Mo-K(alpha) radiation Mu (mm-1) = 0.27 ------------------------------------------------------------------------------- File s92.INS set up as follows: TITL s92 in P2(1)/c CELL 0.71073 11.754 13.880 7.205 90.00 107.18 90.00 ZERR 4.00 0.002 0.003 0.001 0.00 0.03 0.00 LATT 1 SYMM -X, .5+Y, .5-Z SFAC C H N O S UNIT 48 48 8 8 4 TREF HKLF 4 1 0.0000 0.0000 1.0000 0.0000-1.0000 0.0000 1.0000 0.0000 0.0000 END -------------------------------------------------------------------------------