++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 12:54:18 on 15-APR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.637 20.362 9.229 90.00 91.00 90.00 14575 Reflections read from file s92.hkl; mean (I/sigma) = 7.09 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7277 7293 7324 7269 10947 9729 9705 14575 N (int>3sigma) = 0 4056 4169 4227 4166 6226 5497 5593 8357 Mean intensity = 0.0 59.7 59.1 58.2 58.8 59.0 58.8 61.5 59.1 Mean int/sigma = 0.0 7.0 7.1 7.2 7.2 7.1 7.1 7.3 7.2 Lattice type: P chosen Volume: 1434.97 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.637 9.229 20.362 90.00 90.00 91.00 Niggli form: a.a = 58.33 b.b = 85.17 c.c = 414.59 b.c = 0.00 a.c = 0.00 a.b = -1.23 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.074 [ 10690] Cell: 7.637 20.362 9.229 90.00 91.00 90.00 Volume: 1434.97 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 7277 7293 7324 7269 10947 9729 9705 14575 N (int>3sigma) = 0 4056 4169 4227 4166 6226 5497 5593 8357 Mean intensity = 0.0 59.7 59.1 58.2 58.8 59.0 58.8 61.5 59.1 Mean int/sigma = 0.0 7.0 7.1 7.2 7.2 7.1 7.1 7.3 7.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.975 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 38 217 219 218 N I>3s 2 18 79 81 0.5 1.1 98.2 98.8 0.7 1.0 5.0 5.1 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 4 19410 0.074 10690 1.0 / 5.0 2.47 Option [A] chosen ------------------------------------------------------------------------------- ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C16H17F3O2 Formula weight = 298.30 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.381, non-H atomic volume = 17.1 and following cell contents and analysis: C 64.00 64.42 % H 68.00 5.74 % O 8.00 10.73 % F 12.00 19.11 % F(000) = 624.0 Mo-K(alpha) radiation Mu (mm-1) = 0.12 ------------------------------------------------------------------------------- File 1.ins set up as follows: TITL 1 in P2(1)/c CELL 0.71073 9.2288 20.3616 7.6375 90.000 91.003 90.000 ZERR 4.00 0.0018 0.0041 0.0015 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O F UNIT 64 68 8 12 TREF HKLF 4 END -------------------------------------------------------------------------------