++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 09:20:43 on 04-AUG-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 5.517 8.765 20.695 90.00 96.25 90.00 5074 Reflections read from file s92.hkl; mean (I/sigma) = 6.75 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2523 2537 2542 2531 3801 3388 3353 5074 N (int>3sigma) = 0 1622 1544 1602 1540 2384 2151 2135 3231 Mean intensity = 0.0 48.0 44.3 34.2 47.1 42.2 46.7 46.7 47.4 Mean int/sigma = 0.0 6.9 6.5 6.6 6.5 6.7 6.7 6.8 6.8 Lattice type: P chosen Volume: 994.76 ------------------------------------------------------------------------------- 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: 5.517 8.765 20.695 90.00 96.25 90.00 Niggli form: a.a = 30.43 b.b = 76.83 c.c = 428.29 b.c = 0.00 a.c = -12.42 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.057 [ 2950] Cell: 5.517 8.765 20.695 90.00 96.25 90.00 Volume: 994.76 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 2523 2537 2542 2531 3801 3388 3353 5074 N (int>3sigma) = 0 1622 1544 1602 1540 2384 2151 2135 3231 Mean intensity = 0.0 48.0 44.3 34.2 47.1 42.2 46.7 46.7 47.4 Mean int/sigma = 0.0 6.9 6.5 6.6 6.5 6.7 6.7 6.8 6.8 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.944 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 4 218 215 217 N I>3s 0 84 84 0 1.2 40.9 41.4 0.6 0.9 4.5 4.5 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2/n # 13 centro 1 292 0.057 2950 0.5 / 4.5 2.86 [B] Pn # 7 non-cen 1 226 0.057 2950 0.5 / 4.5 7.21 [C] P2(1)/n # 14 centro 1 19410 0.057 2950 0.5 / 4.5 2.52 Option [C] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C9 S2 N2 O2 H8 Formula weight = 240.29 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.604, non-H atomic volume = 16.6 and following cell contents and analysis: C 36.00 44.98 % H 32.00 3.36 % N 8.00 11.66 % O 8.00 13.32 % S 8.00 26.68 % F(000) = 496.0 Mo-K(alpha) radiation Mu (mm-1) = 0.51 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/n CELL 0.71073 5.5166 8.7652 20.6952 90.000 96.246 90.000 ZERR 4.00 0.0011 0.0018 0.0041 0.000 0.030 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O S UNIT 36 32 8 8 8 TREF HKLF 4 END -------------------------------------------------------------------------------