++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 10:14:37 on 05-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.082 24.850 31.120 90.00 90.00 90.00 11518 Reflections read from file s92.hkl; mean (I/sigma) = 5.49 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5682 5741 5683 5784 8553 7619 7616 11518 N (int>3sigma) = 0 2995 2963 2908 3122 4433 4066 4053 6136 Mean intensity = 0.0 21.8 19.2 21.4 21.9 20.8 20.5 20.5 21.4 Mean int/sigma = 0.0 5.6 5.4 5.4 5.7 5.5 5.6 5.6 5.6 Lattice type: P chosen Volume: 4703.15 ------------------------------------------------------------------------------- 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: 6.082 24.850 31.120 90.00 90.00 90.00 Niggli form: a.a = 36.99 b.b = 617.54 c.c = 968.45 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) = 0.071 [ 7629] Cell: 6.082 24.850 31.120 90.00 90.00 90.00 Volume: 4703.15 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 5682 5741 5683 5784 8553 7619 7616 11518 N (int>3sigma) = 0 2995 2963 2908 3122 4433 4066 4053 6136 Mean intensity = 0.0 21.8 19.2 21.4 21.9 20.8 20.5 20.5 21.4 Mean int/sigma = 0.0 5.6 5.4 5.4 5.7 5.5 5.6 5.6 5.6 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.970 [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 538 595 583 1 137 157 156 9 113 134 127 11 N I>3s 2 215 217 0 0 67 67 0 0 56 56 0 0.6 28.9 29.5 0.5 0.6 37.9 38.2 0.3 0.6 32.0 33.8 0.5 0.5 4.2 4.3 0.3 0.4 4.7 4.8 0.3 0.5 5.4 5.7 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pbca # 61 centro 1 2293 0.071 7629 0.5 / 4.2 2.71 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C30H26FeN2O3 Formula weight = 518.38 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.464, non-H atomic volume = 16.3 and following cell contents and analysis: C 240.00 69.51 % H 208.00 5.06 % N 16.00 5.41 % O 24.00 9.26 % Fe 8.00 10.77 % F(000) = 2160.0 Mo-K(alpha) radiation Mu (mm-1) = 0.68 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in Pbca CELL 0.71073 6.0816 24.8503 31.1200 90.000 90.000 90.000 ZERR 8.00 0.0004 0.0016 0.0027 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 FE UNIT 240 208 16 24 8 TREF HKLF 4 END -------------------------------------------------------------------------------