++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 14:40:33 on 11-NOV-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.958 23.151 23.549 79.22 82.97 75.45 60530 Reflections read from file s92.hkl; mean (I/sigma) = 5.51 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 30277 30245 30230 30161 45376 40300 40358 60530 N (int>3sigma) = 0 14087 14087 13988 14086 21081 18802 18816 28197 Mean intensity = 0.0 39.7 40.4 16.9 37.8 32.4 38.2 37.4 38.0 Mean int/sigma = 0.0 5.6 5.7 5.2 5.7 5.5 5.7 5.6 5.6 Lattice type: P chosen Volume: 6179.26 ------------------------------------------------------------------------------- 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: 11.958 23.151 23.549 79.22 82.97 75.45 Niggli form: a.a = 143.00 b.b = 535.95 c.c = 554.55 b.c = 101.93 a.c = 34.49 a.b = 69.56 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.083 [ 35018] Cell: 11.958 23.151 23.549 79.22 82.97 75.45 Volume: 6179.26 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 30277 30245 30230 30161 45376 40300 40358 60530 N (int>3sigma) = 0 14087 14087 13988 14086 21081 18802 18816 28197 Mean intensity = 0.0 39.7 40.4 16.9 37.8 32.4 38.2 37.4 38.0 Mean int/sigma = 0.0 5.6 5.7 5.2 5.7 5.5 5.7 5.6 5.6 Crystal system A and Lattice type P selected Mean |E*E-1| = 1.187 [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 0.083 35018 0.0 / 5.6 6.59 [B] P1 # 1 chiral 1 700 0.083 35018 0.0 / 5.6 22.28 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C42H56Cl4N7O4F Formula weight = 883.74 Tentative Z (number of formula units/cell) = 6.0 giving rho = 1.425, non-H atomic volume = 17.8 and following cell contents and analysis: C 252.00 57.08 % H 336.00 6.39 % N 42.00 11.10 % O 24.00 7.24 % F 6.00 2.15 % Cl 24.00 16.05 % F(000) = 2796.0 Mo-K(alpha) radiation Mu (mm-1) = 0.34 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P-1 CELL 0.71073 11.9582 23.1506 23.5489 79.225 82.965 75.447 ZERR 6.00 0.0002 0.0003 0.0004 0.001 0.001 0.001 LATT 1 SFAC C H N O F CL UNIT 252 336 42 24 6 24 TREF HKLF 4 END -------------------------------------------------------------------------------