XPREP - RECIPROCAL SPACE EXPLORATION ------------------------------------- Original cell in Angstroms and degrees: 5.572 14.600 18.483 90.00 90.00 90.00 14500 reflections read from file s92.HKL Mean(I/sigma) = 8.58 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7257 7233 7294 7251 10892 9682 9660 14500 N (int>3sigma) = 0 4697 4223 4600 4604 6760 6276 6240 9347 Mean intensity = 0.0 432.7 343.3 394.1 387.2 390.1 415.2 416.8 409.9 Mean int/sigma = 0.0 8.6 7.8 8.5 8.6 8.3 8.7 8.7 8.7 Lattice type P chosen Volume: 1503.70 ------------------------------------------------------------------------------- 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: 5.572 14.600 18.483 90.00 90.00 90.00 Niggli form: a.a = 31.05 b.b = 213.17 c.c = 341.60 b.c = 0.00 a.c = -0.01 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher METRIC symmetry ------------------------------------------------------------------------------- Option A: FOM = 0.005 deg. ORTHORHOMBIC P-lattice R(int) = 0.026 [ 8654] Cell: 5.572 14.600 18.483 90.00 90.00 90.00 Volume: 1503.70 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 7257 7233 7294 7251 10892 9660 9682 14500 N (int>3sigma) = 0 4697 4223 4600 4604 6760 6240 6276 9347 Mean intensity = 0.0 432.7 343.3 394.1 387.2 390.1 416.8 415.2 409.9 Mean int/sigma = 0.0 8.6 7.8 8.5 8.6 8.3 8.7 8.7 8.7 Crystal system O and Lattice type P selected Mean |E*E-1| = 1.102 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 1079 1068 1065 6 228 245 227 41 259 286 281 25 N I>3s 409 7 406 0 63 6 67 0 100 2 100 0 475.2 3.5 481.2 1.3 151.7 2.5 152.3 2.5 722.4 2.3 666.0 4.0 5.9 0.6 6.0 1.0 3.9 0.7 4.0 0.5 6.9 0.5 6.4 0.8 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pbca # 61 centro 2 2293 0.026 8654 1.0 / 3.9 4.90 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C6 H8 N2 O2 S Formula weight = 172.20 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.521, non-H atomic volume = 17.1 and following cell contents and analysis: C 48.00 41.85 % H 64.00 4.68 % N 16.00 16.27 % O 16.00 18.58 % S 8.00 18.62 % F(000) = 720.0 Mo-K(alpha) radiation Mu (mm-1) = 0.36 ------------------------------------------------------------------------------- File s92.INS set up as follows: TITL s92 in Pbca CELL 0.71073 14.600 5.572 18.483 90.00 90.00 90.00 ZERR 8.00 0.003 0.001 0.004 0.00 0.00 0.00 LATT 1 SYMM .5-X, -Y, .5+Z SYMM -X, .5+Y, .5-Z SYMM .5+X, .5-Y, -Z SFAC C H N O S UNIT 48 64 16 16 8 TREF HKLF 4 1 0.0000-1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000-1.0000 END -------------------------------------------------------------------------------