++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0030 started at 11:43:28 on 28-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 5.687 7.908 24.117 98.32 90.02 89.96 21749 Reflections read from file 06skc0030.hkl; mean (I/sigma) = 3.69 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 10880 10879 10837 10874 16298 14502 14477 21749 N (int>3sigma) = 0 4534 4535 4757 4461 6913 6196 6119 9260 Mean intensity = 0.0 126.5 135.0 118.1 119.2 126.5 140.8 142.7 142.0 Mean int/sigma = 0.0 3.6 3.7 3.7 3.5 3.7 3.8 3.7 3.8 Lattice type: P chosen Volume: 1073.21 ------------------------------------------------------------------------------- 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: 5.687 7.908 24.117 81.68 89.98 89.96 Niggli form: a.a = 32.34 b.b = 62.54 c.c = 581.64 b.c = 27.61 a.c = 0.05 a.b = 0.03 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.038 deg. MONOCLINIC P-lattice R(int) = 0.146 [ 18998] Cell: 7.908 5.687 24.117 90.02 98.32 89.96 Volume: 1073.21 Matrix: 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.131 [ 16825] Cell: 5.687 7.908 24.117 81.68 89.98 89.96 Volume: 1073.21 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 10879 10880 10837 10874 16298 14477 14502 21749 N (int>3sigma) = 0 4535 4534 4757 4461 6913 6119 6196 9260 Mean intensity = 0.0 135.0 126.5 118.1 119.2 126.5 142.7 140.8 142.0 Mean int/sigma = 0.0 3.7 3.6 3.7 3.5 3.7 3.7 3.8 3.8 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.849 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 21 1174 1155 1145 N I>3s 7 404 391 47 126.1 143.3 144.1 12.2 2.3 3.9 3.9 0.9 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2/n # 13 centro 1 292 0.146 18998 0.9 / 2.3 8.89 [B] Pn # 7 non-cen 1 226 0.146 18998 0.9 / 2.3 8.87 [C] P2(1)/n # 14 centro 1 19410 0.146 18998 2.3 / 3.8 6.70 Option [C] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12H14O4N2S1 Formula weight = 282.31 Tentative Z (number of formula units/cell) = 2.0 giving rho = 0.874, non-H atomic volume = 28.2 and following cell contents and analysis: C 24.00 51.05 % H 28.00 5.00 % N 4.00 9.93 % O 8.00 22.67 % S 2.00 11.36 % F(000) = 296.0 Mo-K(alpha) radiation Mu (mm-1) = 0.16 ------------------------------------------------------------------------------- File 06skc0030p21n.ins set up as follows: TITL 06skc0030p21n in P2(1)/n CELL 0.71073 7.9081 5.6870 24.1173 90.000 98.322 90.000 ZERR 2.00 0.0008 0.0006 0.0024 0.000 0.007 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O S UNIT 24 28 4 8 2 TEMP 0.01 TREF HKLF 4 END 21749 Reflections written to new reflection file 06skc0030p21n.hkl -------------------------------------------------------------------------------