++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 13:45:26 on 18-JAN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.166 12.093 14.352 89.99 90.04 70.41 16827 Reflections read from file s92.hkl; mean (I/sigma) = 3.20 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8427 8396 8429 8407 12626 11243 11225 16827 N (int>3sigma) = 0 2670 2715 2677 2660 4031 3579 3566 5293 Mean intensity = 0.0 25.2 26.9 23.3 24.3 25.1 24.7 24.5 24.0 Mean int/sigma = 0.0 3.4 3.4 3.4 3.4 3.4 3.4 3.4 3.4 Lattice type: P chosen Volume: 1335.31 ------------------------------------------------------------------------------- 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: 8.166 12.093 14.352 90.01 90.04 109.59 Niggli form: a.a = 66.69 b.b = 146.24 c.c = 205.99 b.c = -0.02 a.c = -0.09 a.b = -33.11 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.149 deg. ORTHORHOMBIC C-lattice R(int) = 0.596 [ 15097] Cell: 8.166 22.786 14.352 89.98 89.96 89.86 Volume: 2670.62 Matrix: 1.0000 0.0000 0.0000 1.0000 -2.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.047 deg. MONOCLINIC P-lattice R(int) = 0.122 [ 13750] Cell: 8.166 14.352 12.093 89.99 109.59 89.96 Volume: 1335.31 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.145 deg. MONOCLINIC C-lattice R(int) = 0.589 [ 13740] Cell: 8.166 22.786 14.352 90.02 90.04 89.86 Volume: 2670.62 Matrix:-1.0000 0.0000 0.0000 -1.0000 2.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.149 deg. MONOCLINIC C-lattice R(int) = 0.589 [ 13611] Cell: 22.786 8.166 14.352 89.96 90.02 90.14 Volume: 2670.62 Matrix:-1.0000 2.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.109 [ 11094] Cell: 8.166 12.093 14.352 90.01 90.04 109.59 Volume: 1335.31 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8427 8429 8396 8407 12626 11237 11225 16827 N (int>3sigma) = 0 2670 2677 2715 2660 4031 3562 3566 5293 Mean intensity = 0.0 25.2 23.3 26.9 24.3 25.1 23.6 24.5 24.0 Mean int/sigma = 0.0 3.4 3.4 3.4 3.4 3.4 3.4 3.4 3.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 1.089 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 27 308 297 305 N I>3s 0 101 0 101 1.0 54.9 1.2 55.4 0.4 4.2 0.5 4.2 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.122 13750 0.5 / 3.4 4.91 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C16H6O8Fe2 Formula weight = 437.91 Tentative Z (number of formula units/cell) = 4.0 giving rho = 2.178, non-H atomic volume = 12.8 and following cell contents and analysis: C 64.00 43.88 % H 24.00 1.38 % O 32.00 29.23 % Fe 8.00 25.51 % F(000) = 872.0 Mo-K(alpha) radiation Mu (mm-1) = 2.23 ------------------------------------------------------------------------------- File 1.ins set up as follows: TITL 1 in P2(1)/c CELL 0.71073 8.1662 14.3524 12.0930 90.000 109.590 90.000 ZERR 4.00 0.0007 0.0014 0.0010 0.000 0.004 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O FE UNIT 64 24 32 8 TREF HKLF 4 END -------------------------------------------------------------------------------