++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 15:54:26 on 24-NOV-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.906 8.652 12.818 90.00 94.41 90.00 6318 Reflections read from file s92.hkl; mean (I/sigma) = 9.25 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3160 3163 3171 3157 4747 4221 4200 6318 N (int>3sigma) = 0 2196 2195 2279 2243 3335 3014 2990 4490 Mean intensity = 0.0 128.5 120.8 125.2 136.6 124.9 131.0 126.1 130.6 Mean int/sigma = 0.0 9.1 9.0 9.4 9.3 9.2 9.4 9.3 9.3 Lattice type: P chosen Volume: 763.59 ------------------------------------------------------------------------------- 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: 6.906 8.652 12.818 90.00 94.41 90.00 Niggli form: a.a = 47.69 b.b = 74.86 c.c = 164.31 b.c = 0.00 a.c = -6.81 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.038 [ 4474] Cell: 6.906 8.652 12.818 90.00 94.41 90.00 Volume: 763.59 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 3160 3163 3171 3157 4747 4221 4200 6318 N (int>3sigma) = 0 2196 2195 2279 2243 3335 3014 2990 4490 Mean intensity = 0.0 128.5 120.8 125.2 136.6 124.9 131.0 126.1 130.6 Mean int/sigma = 0.0 9.1 9.0 9.4 9.3 9.2 9.4 9.3 9.3 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.952 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 8 224 227 225 N I>3s 0 104 5 103 1.4 136.1 1.0 135.4 0.5 6.6 0.7 6.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.038 4474 0.7 / 6.5 1.73 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12H18N6O6Cl2Fe Formula weight = 469.07 Tentative Z (number of formula units/cell) = 2.0 giving rho = 2.040, non-H atomic volume = 14.1 and following cell contents and analysis: C 24.00 30.72 % H 36.00 3.87 % N 12.00 17.92 % O 12.00 20.47 % Cl 4.00 15.11 % Fe 2.00 11.91 % F(000) = 480.0 Mo-K(alpha) radiation Mu (mm-1) = 1.39 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/c CELL 0.71073 6.9056 8.6519 12.8184 90.000 94.411 90.000 ZERR 2.00 0.0014 0.0017 0.0026 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O CL FE UNIT 24 36 12 12 4 2 TREF HKLF 4 END -------------------------------------------------------------------------------