++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 10:36:41 on 23-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 13.957 14.612 20.003 90.00 98.68 90.00 34507 Reflections read from file s92.hkl; mean (I/sigma) = 8.23 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 17220 17242 17234 17273 25848 22975 22990 34507 N (int>3sigma) = 0 11733 11933 11946 11830 17806 15851 15962 23917 Mean intensity = 0.0 45.6 47.0 46.4 47.1 46.3 45.5 47.0 46.2 Mean int/sigma = 0.0 8.2 8.3 8.3 8.2 8.3 8.3 8.3 8.3 Lattice type: P chosen Volume: 4032.58 ------------------------------------------------------------------------------- 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: 13.957 14.612 20.003 90.00 98.68 90.00 Niggli form: a.a = 194.80 b.b = 213.52 c.c = 400.10 b.c = 0.00 a.c = -42.15 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.053 [ 24990] Cell: 13.957 14.612 20.003 90.00 98.68 90.00 Volume: 4032.58 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 17220 17242 17234 17273 25848 22975 22990 34507 N (int>3sigma) = 0 11733 11933 11946 11830 17806 15851 15962 23917 Mean intensity = 0.0 45.6 47.0 46.4 47.1 46.3 45.5 47.0 46.2 Mean int/sigma = 0.0 8.2 8.3 8.3 8.2 8.3 8.3 8.3 8.3 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.954 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 16 659 602 665 N I>3s 0 301 0 301 0.5 56.3 0.7 55.8 0.5 6.5 0.4 6.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.053 24990 0.5 / 6.5 1.68 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C41H34FeRuP2Cl2 Formula weight = 816.44 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.345, non-H atomic volume = 21.4 and following cell contents and analysis: C 164.00 60.31 % H 136.00 4.20 % P 8.00 7.59 % Cl 8.00 8.68 % Fe 4.00 6.84 % Ru 4.00 12.38 % F(000) = 1656.0 Mo-K(alpha) radiation Mu (mm-1) = 0.97 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/c CELL 0.71073 13.9569 14.6122 20.0025 90.000 98.683 90.000 ZERR 4.00 0.0002 0.0002 0.0004 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H P CL FE RU UNIT 164 136 8 8 4 4 TREF HKLF 4 END -------------------------------------------------------------------------------