++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 09:20:08 on 01-MAR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 3.787 14.566 22.444 90.00 91.70 90.00 11653 Reflections read from file s92.hkl; mean (I/sigma) = 5.07 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5831 5848 5815 5836 8747 7775 7754 11653 N (int>3sigma) = 0 3106 3207 2941 3129 4627 4190 4217 6312 Mean intensity = 0.0 47.7 50.9 42.8 48.6 47.1 50.2 51.0 50.1 Mean int/sigma = 0.0 5.1 5.2 4.9 5.1 5.0 5.1 5.1 5.1 Lattice type: P chosen Volume: 1237.51 ------------------------------------------------------------------------------- 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: 3.787 14.566 22.444 90.00 91.70 90.00 Niggli form: a.a = 14.34 b.b = 212.16 c.c = 503.71 b.c = 0.00 a.c = -2.52 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.094 [ 8802] Cell: 3.787 14.566 22.444 90.00 91.70 90.00 Volume: 1237.51 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 5831 5848 5815 5836 8747 7775 7754 11653 N (int>3sigma) = 0 3106 3207 2941 3129 4627 4190 4217 6312 Mean intensity = 0.0 47.7 50.9 42.8 48.6 47.1 50.2 51.0 50.1 Mean int/sigma = 0.0 5.1 5.2 4.9 5.1 5.0 5.1 5.1 5.1 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.835 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 27 278 274 280 N I>3s 0 112 37 115 1.5 107.4 7.7 109.7 0.8 4.4 1.5 4.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.094 8802 1.5 / 4.4 5.24 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C18H12N2Se2Cu1Cl2 Formula weight = 548.66 Tentative Z (number of formula units/cell) = 3.0 giving rho = 2.209, non-H atomic volume = 16.5 and following cell contents and analysis: C 54.00 39.40 % H 36.00 2.20 % N 6.00 5.11 % Cl 6.00 12.92 % Cu 3.00 11.58 % Se 6.00 28.78 % F(000) = 795.0 Mo-K(alpha) radiation Mu (mm-1) = 6.06 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/c CELL 0.71073 3.7872 14.5657 22.4435 90.000 91.700 90.000 ZERR 3.00 0.0003 0.0011 0.0021 0.000 0.003 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N CL CU SE UNIT 54 36 6 6 3 6 TREF HKLF 4 END -------------------------------------------------------------------------------