++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 10:36:36 on 08-MAR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.338 16.197 34.010 90.00 90.00 90.00 20398 Reflections read from file s92.hkl; mean (I/sigma) = 3.17 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 10179 10177 10172 10202 15264 13583 13635 20398 N (int>3sigma) = 0 3223 3081 3070 3124 4687 4221 4203 6345 Mean intensity = 0.0 10.4 9.6 10.6 9.8 10.2 10.8 10.8 10.7 Mean int/sigma = 0.0 3.4 3.2 3.3 3.3 3.3 3.3 3.3 3.3 Lattice type: P chosen Volume: 5143.98 ------------------------------------------------------------------------------- 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: 9.338 16.197 34.010 90.00 90.00 90.00 Niggli form: a.a = 87.19 b.b = 262.35 c.c = 1156.71 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(int) = 0.163 [ 15155] Cell: 9.338 16.197 34.010 90.00 90.00 90.00 Volume: 5143.98 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.141 [ 11451] Cell: 9.338 34.010 16.197 90.00 90.00 90.00 Volume: 5143.98 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.138 [ 10958] Cell: 16.197 9.338 34.010 90.00 90.00 90.00 Volume: 5143.98 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.138 [ 10980] Cell: 9.338 16.197 34.010 90.00 90.00 90.00 Volume: 5143.98 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.092 [ 4871] Cell: 9.338 16.197 34.010 90.00 90.00 90.00 Volume: 5143.98 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 10179 10177 10172 10202 15264 13583 13635 20398 N (int>3sigma) = 0 3223 3081 3070 3124 4687 4221 4203 6345 Mean intensity = 0.0 10.4 9.6 10.6 9.8 10.2 10.8 10.8 10.7 Mean int/sigma = 0.0 3.4 3.2 3.3 3.3 3.3 3.3 3.3 3.3 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.958 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 768 697 773 7 394 374 406 13 211 190 211 20 N I>3s 225 0 225 0 87 0 87 0 52 0 52 0 14.8 0.7 14.7 0.4 10.6 0.9 10.3 0.8 15.8 0.8 15.8 0.7 3.1 0.4 3.1 0.3 2.7 0.5 2.6 0.6 3.4 0.5 3.4 0.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pbca # 61 centro 2 2293 0.163 15155 0.6 / 2.6 4.70 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C24 H30 N5 O2 P1 F6 Cl2 Formula weight = 636.40 Tentative Z (number of formula units/cell) = 7.0 giving rho = 1.438, non-H atomic volume = 18.4 and following cell contents and analysis: C 168.00 45.29 % H 210.00 4.75 % N 35.00 11.01 % O 14.00 5.03 % F 42.00 17.91 % P 7.00 4.87 % Cl 14.00 11.14 % F(000) = 2296.0 Mo-K(alpha) radiation Mu (mm-1) = 0.34 ------------------------------------------------------------------------------- File s93.ins set up as follows: TITL s93 in Pbca CELL 0.71073 16.1973 9.3378 34.0104 90.000 90.000 90.000 ZERR 7.00 0.0005 0.0002 0.0012 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O F P CL UNIT 168 210 35 14 42 7 14 TREF HKLF 4 END -------------------------------------------------------------------------------