++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 15:18:16 on 18-JAN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 12.336 13.608 12.665 90.00 95.81 90.00 16865 Reflections read from file s92.hkl; mean (I/sigma) = 5.31 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8407 8418 8477 8456 12651 11257 11224 16865 N (int>3sigma) = 0 3834 3847 3823 3838 5752 5225 5186 7833 Mean intensity = 0.0 29.9 31.6 34.1 28.9 31.9 31.9 32.3 31.8 Mean int/sigma = 0.0 5.2 5.4 5.3 5.4 5.3 5.4 5.4 5.4 Lattice type: P chosen Volume: 2115.16 ------------------------------------------------------------------------------- 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: 12.336 12.665 13.608 90.00 90.00 95.81 Niggli form: a.a = 152.18 b.b = 160.40 c.c = 185.17 b.c = 0.00 a.c = 0.00 a.b = -15.81 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.078 [ 12214] Cell: 12.336 13.608 12.665 90.00 95.81 90.00 Volume: 2115.16 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 8407 8418 8477 8456 12651 11257 11224 16865 N (int>3sigma) = 0 3834 3847 3823 3838 5752 5225 5186 7833 Mean intensity = 0.0 29.9 31.6 34.1 28.9 31.9 31.9 32.3 31.8 Mean int/sigma = 0.0 5.2 5.4 5.3 5.4 5.3 5.4 5.4 5.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.980 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 14 378 376 374 N I>3s 0 1 122 123 1.1 0.8 28.2 28.4 0.6 0.5 4.7 4.7 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 4 19410 0.078 12214 0.6 / 4.7 2.42 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C22 H28 N4 O2 Formula weight = 380.48 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.195, non-H atomic volume = 18.9 and following cell contents and analysis: C 88.00 69.44 % H 112.00 7.42 % N 16.00 14.73 % O 8.00 8.41 % F(000) = 816.0 Mo-K(alpha) radiation Mu (mm-1) = 0.08 ------------------------------------------------------------------------------- File s93.ins set up as follows: TITL s93 in P2(1)/c CELL 0.71073 12.6651 13.6078 12.3362 90.000 95.807 90.000 ZERR 4.00 0.0025 0.0027 0.0025 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 88 112 16 8 TREF HKLF 4 END -------------------------------------------------------------------------------