++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 15:19:09 on 12-APR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.954 9.552 10.695 97.61 110.44 104.17 5358 Reflections read from file s92.hkl; mean (I/sigma) = 6.13 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2666 2687 2723 2690 4038 3560 3583 5358 N (int>3sigma) = 0 1172 1160 1200 1197 1766 1597 1597 2394 Mean intensity = 0.0 11.3 9.2 11.8 12.0 10.8 11.8 12.2 11.5 Mean int/sigma = 0.0 6.3 6.0 6.3 6.2 6.2 6.3 6.4 6.3 Lattice type: P chosen Volume: 716.69 ------------------------------------------------------------------------------- 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: 7.954 9.552 10.695 97.61 110.44 104.17 Niggli form: a.a = 63.26 b.b = 91.25 c.c = 114.38 b.c = -13.54 a.c = -29.71 a.b = -18.60 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.049 [ 2412] Cell: 7.954 9.552 10.695 97.61 110.44 104.17 Volume: 716.69 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 2666 2687 2723 2690 4038 3560 3583 5358 N (int>3sigma) = 0 1172 1160 1200 1197 1766 1597 1597 2394 Mean intensity = 0.0 11.3 9.2 11.8 12.0 10.8 11.8 12.2 11.5 Mean int/sigma = 0.0 6.3 6.0 6.3 6.2 6.2 6.3 6.4 6.3 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.944 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P-1 # 2 centro 1 8646 0.049 2412 0.0 / 6.3 1.66 [B] P1 # 1 chiral 1 700 0.049 2412 0.0 / 6.3 6.05 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C14H14F3O2Br Formula weight = 351.16 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.627, non-H atomic volume = 17.9 and following cell contents and analysis: C 28.00 47.88 % H 28.00 4.02 % O 4.00 9.11 % F 6.00 16.23 % Br 2.00 22.76 % F(000) = 352.0 Mo-K(alpha) radiation Mu (mm-1) = 2.90 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P-1 CELL 0.71073 7.9539 9.5523 10.6949 97.614 110.439 104.170 ZERR 2.00 0.0016 0.0019 0.0021 0.030 0.030 0.030 LATT 1 SFAC C H O F BR UNIT 28 28 4 6 2 TREF HKLF 4 END -------------------------------------------------------------------------------