XPREP - RECIPROCAL SPACE EXPLORATION ------------------------------------- Original cell in Angstroms and degrees: 7.230 15.594 19.618 90.00 90.00 90.00 8635 reflections read from file s92.HKL Mean(I/sigma) = 3.85 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4244 4270 4232 4351 6373 5736 5713 8635 N (int>3sigma) = 0 1460 1543 1651 1602 2327 2083 2098 3122 Mean intensity = 0.0 184.2 191.0 228.4 211.7 201.2 205.5 205.5 207.8 Mean int/sigma = 0.0 3.5 3.7 4.1 3.9 3.8 3.8 3.8 3.9 Lattice type P chosen Volume: 2211.82 ------------------------------------------------------------------------------- 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: 7.230 15.594 19.618 90.00 90.00 90.00 Niggli form: a.a = 52.27 b.b = 243.17 c.c = 384.87 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher METRIC symmetry ------------------------------------------------------------------------------- Option A: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(int) = 0.038 [ 3458] Cell: 7.230 15.594 19.618 90.00 90.00 90.00 Volume: 2211.82 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 4244 4270 4232 4351 6373 5736 5713 8635 N (int>3sigma) = 0 1460 1543 1651 1602 2327 2083 2098 3122 Mean intensity = 0.0 184.2 191.0 228.4 211.7 201.2 205.5 205.5 207.8 Mean int/sigma = 0.0 3.5 3.7 4.1 3.9 3.8 3.8 3.8 3.9 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.846 [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 198 245 257 5 115 169 168 7 110 130 134 9 N I>3s 0 77 77 0 1 65 66 0 0 40 40 0 8.9 258.8 247.2 6.8 9.0 264.6 267.5 9.7 9.1 690.8 669.0 6.2 0.3 3.7 3.6 0.3 0.4 4.8 4.9 0.4 0.4 9.0 8.7 0.2 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pbca # 61 centro 1 2293 0.038 3458 0.4 / 3.6 4.56 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C 10 H 9 N 4 S 1 Cl 1 Formula weight = 252.72 Tentative Z (number of formula units/cell) = 7.0 giving rho = 1.328, non-H atomic volume = 19.7 and following cell contents and analysis: C 70.00 47.53 % H 63.00 3.59 % N 28.00 22.17 % S 7.00 12.69 % Cl 7.00 14.03 % F(000) = 910.0 Mo-K(alpha) radiation Mu (mm-1) = 0.44 ------------------------------------------------------------------------------- File s92.INS set up as follows: TITL s92 in Pbca CELL 0.71073 7.230 15.594 19.618 90.00 90.00 90.00 ZERR 7.00 0.001 0.003 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 S CL UNIT 70 63 28 7 7 TREF HKLF 4 END -------------------------------------------------------------------------------