++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04src0437r started at 11:49:55 on 07-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 19.438 11.118 30.276 89.99 91.58 90.01 50486 Reflections read from file 04src0437r.hkl; mean (I/sigma) = 11.94 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 25286 25238 25228 25252 37876 33660 33684 50486 N (int>3sigma) = 0 18093 18706 18567 18620 27683 24901 24968 37305 Mean intensity = 0.0 256.9 255.9 258.7 251.2 257.1 255.8 256.4 256.5 Mean int/sigma = 0.0 11.7 12.1 12.0 12.0 11.9 12.0 12.1 12.0 Lattice type: P chosen Volume: 6540.22 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 11.118 19.438 30.276 88.42 89.99 89.99 Niggli form: a.a = 123.61 b.b = 377.82 c.c = 916.62 b.c = 16.22 a.c = 0.04 a.b = 0.03 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.009 deg. MONOCLINIC P-lattice R(int) = 0.034 [ 34742] Cell: 19.438 11.118 30.276 89.99 91.58 90.01 Volume: 6540.22 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 25286 25238 25228 25252 37876 33660 33684 50486 N (int>3sigma) = 0 18093 18706 18567 18620 27683 24901 24968 37305 Mean intensity = 0.0 256.9 255.9 258.7 251.2 257.1 255.8 256.4 256.5 Mean int/sigma = 0.0 11.7 12.1 12.0 12.0 11.9 12.0 12.1 12.0 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.968 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 16 1446 1462 1436 N I>3s 0 612 10 612 1.5 281.4 2.2 283.2 0.6 8.5 0.6 8.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.034 34742 0.6 / 8.5 1.27 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C30H52Cl2Fe1P2Pd1 Formula weight = 707.81 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.438, non-H atomic volume = 22.7 and following cell contents and analysis: C 240.00 50.90 % H 416.00 7.41 % P 16.00 8.75 % Cl 16.00 10.02 % Fe 8.00 7.89 % Pd 8.00 15.03 % F(000) = 2944.0 Mo-K(alpha) radiation Mu (mm-1) = 1.27 ------------------------------------------------------------------------------- File 04src0437r.ins set up as follows: TITL 04src0437r in P2(1)/c CELL 0.71073 19.4376 11.1178 30.2758 90.000 91.579 90.000 ZERR 8.00 0.0015 0.0011 0.0027 0.000 0.008 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H P CL FE PD UNIT 240 416 16 16 8 8 TEMP 0.16 TREF HKLF 4 END -------------------------------------------------------------------------------