++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2005src1160 started at 15:40:01 on 26-SEP-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.316 5.413 19.012 90.00 91.10 90.00 14902 Reflections read from file 2005src1160.hkl; mean (I/sigma) = 8.46 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7457 7448 7451 7438 11178 9916 9928 14902 N (int>3sigma) = 0 5337 5067 5302 4047 7853 7052 7060 10586 Mean intensity = 0.0 357.9 357.3 366.7 101.8 360.6 363.9 360.4 360.0 Mean int/sigma = 0.0 8.7 8.3 8.5 5.6 8.5 8.5 8.5 8.5 Lattice type: P chosen Volume: 1164.33 ------------------------------------------------------------------------------- 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: 5.413 11.316 19.012 91.10 90.00 90.00 Niggli form: a.a = 29.30 b.b = 128.04 c.c = 361.44 b.c = -4.12 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.052 [ 11951] Cell: 11.316 5.413 19.012 90.00 91.10 90.00 Volume: 1164.33 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 7457 7448 7451 7438 11178 9916 9928 14902 N (int>3sigma) = 0 5337 5067 5302 4047 7853 7052 7060 10586 Mean intensity = 0.0 357.9 357.3 366.7 101.8 360.6 363.9 360.4 360.0 Mean int/sigma = 0.0 8.7 8.3 8.5 5.6 8.5 8.5 8.5 8.5 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.955 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 7 842 843 835 N I>3s 0 395 395 10 4.6 441.6 441.5 4.2 0.5 7.3 7.3 0.6 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.052 11951 0.6 / 7.3 1.51 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C26H32F2Se2 Formula weight = 540.44 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.542, non-H atomic volume = 19.4 and following cell contents and analysis: C 52.00 57.78 % H 64.00 5.97 % F 4.00 7.03 % Se 4.00 29.22 % F(000) = 548.0 Mo-K(alpha) radiation Mu (mm-1) = 3.20 ------------------------------------------------------------------------------- File 2005src1160.ins set up as follows: TITL 2005src1160 in P2(1)/n CELL 0.71073 11.3155 5.4133 19.0117 90.000 91.099 90.000 ZERR 2.00 0.0004 0.0001 0.0007 0.000 0.002 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H F SE UNIT 52 64 4 4 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------