++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 15:34:42 on 21-NOV-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.583 15.587 25.277 90.00 90.00 90.00 20523 Reflections read from file s92.hkl; mean (I/sigma) = 8.42 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 10280 10279 10279 10263 15419 13635 13663 20523 N (int>3sigma) = 0 7575 7571 7480 7535 11313 9910 9985 15012 Mean intensity = 0.0 72.5 72.8 70.1 74.7 71.8 75.3 75.0 74.3 Mean int/sigma = 0.0 8.5 8.5 8.4 8.6 8.4 8.4 8.5 8.5 Lattice type: P chosen Volume: 3381.63 ------------------------------------------------------------------------------- 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: 8.583 15.587 25.277 90.00 90.00 90.00 Niggli form: a.a = 73.67 b.b = 242.96 c.c = 638.92 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) = 0.090 [ 16195] Cell: 8.583 15.587 25.277 90.00 90.00 90.00 Volume: 3381.63 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 10280 10279 10279 10263 15419 13635 13663 20523 N (int>3sigma) = 0 7575 7571 7480 7535 11313 9910 9985 15012 Mean intensity = 0.0 72.5 72.8 70.1 74.7 71.8 75.3 75.0 74.3 Mean int/sigma = 0.0 8.5 8.5 8.4 8.6 8.4 8.4 8.5 8.5 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.752 [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 711 698 707 5 304 294 300 19 310 305 307 14 N I>3s 456 447 461 0 187 180 189 0 207 183 192 0 108.2 102.2 104.7 2.3 72.0 65.3 68.7 0.9 87.3 77.1 73.5 1.1 8.5 8.8 8.8 0.9 7.3 6.9 7.3 0.4 9.0 7.9 8.3 0.3 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)2(1)2(1) # 19 chiral 1 5917 0.090 16195 0.9 / 6.9 1.48 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: P6 N9 S2 O1 C23 Cl6 H34 Formula weight = 915.23 Tentative Z (number of formula units/cell) = 3.0 giving rho = 1.348, non-H atomic volume = 24.0 and following cell contents and analysis: C 69.00 30.18 % H 102.00 3.74 % N 27.00 13.78 % O 3.00 1.75 % P 18.00 20.30 % S 6.00 7.01 % Cl 18.00 23.24 % F(000) = 1401.0 Mo-K(alpha) radiation Mu (mm-1) = 0.72 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)2(1)2(1) CELL 0.71073 8.5829 15.5872 25.2769 90.000 90.000 90.000 ZERR 3.00 0.0017 0.0031 0.0051 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O P S CL UNIT 69 102 27 3 18 6 18 TREF HKLF 4 END -------------------------------------------------------------------------------