++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 11:41:45 on 19-JAN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 20.426 5.584 25.536 90.00 93.05 90.00 16416 Reflections read from file s92.hkl; mean (I/sigma) = 4.52 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8204 8204 0 8199 8204 10916 10961 16416 N (int>3sigma) = 0 3274 3274 0 3132 3274 4720 4744 7132 Mean intensity = 0.0 19.5 19.5 0.0 17.3 19.5 24.1 23.1 23.3 Mean int/sigma = 0.0 4.3 4.3 0.0 4.1 4.3 4.7 4.7 4.7 Lattice type: C chosen Volume: 2908.57 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 Unitcell: 5.584 10.588 25.536 87.06 90.00 74.71 Niggli form: a.a = 31.18 b.b = 112.10 c.c = 652.10 b.c = 13.87 a.c = 0.00 a.b = 15.59 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC C-lattice R(int) = 0.075 [ 12778] Cell: 20.426 5.584 25.536 90.00 93.05 90.00 Volume: 2908.57 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 8204 8204 0 8199 8204 10916 10961 16416 N (int>3sigma) = 0 3274 3274 0 3132 3274 4720 4744 7132 Mean intensity = 0.0 19.5 19.5 0.0 17.3 19.5 24.1 23.1 23.3 Mean int/sigma = 0.0 4.3 4.3 0.0 4.1 4.3 4.7 4.7 4.7 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.968 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 1105 N I>3s 0 0.5 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.075 12778 0.5 / 4.7 2.40 [B] Cc # 9 non-cen 1 566 0.075 12778 0.5 / 4.7 7.95 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C15H17O3F3 Formula weight = 302.29 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.381, non-H atomic volume = 17.3 and following cell contents and analysis: C 120.00 59.60 % H 136.00 5.67 % O 24.00 15.88 % F 24.00 18.86 % F(000) = 1264.0 Mo-K(alpha) radiation Mu (mm-1) = 0.12 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in C2/c CELL 0.71073 20.4261 5.5841 25.5362 90.000 93.049 90.000 ZERR 8.00 0.0041 0.0011 0.0051 0.000 0.030 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H O F UNIT 120 136 24 24 TREF HKLF 4 END -------------------------------------------------------------------------------