++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 10:01:34 on 17-JAN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.960 26.611 12.101 90.00 105.14 90.00 15287 Reflections read from file s92.hkl; mean (I/sigma) = 2.65 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7628 7648 7626 7638 11451 10201 10163 15287 N (int>3sigma) = 0 2028 2135 2229 2148 3196 2919 2925 4356 Mean intensity = 0.0 10.1 10.7 12.3 11.8 11.0 12.2 11.5 11.6 Mean int/sigma = 0.0 2.7 2.8 2.9 2.9 2.8 2.9 2.9 2.8 Lattice type: P chosen Volume: 2163.33 ------------------------------------------------------------------------------- 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: 6.960 12.101 26.611 90.00 90.00 105.14 Niggli form: a.a = 48.44 b.b = 146.44 c.c = 708.14 b.c = 0.00 a.c = 0.00 a.b = -22.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.123 [ 10850] Cell: 6.960 26.611 12.101 90.00 105.14 90.00 Volume: 2163.33 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. TRICLINIC P-lattice R(int) = 0.096 [ 7465] Cell: 6.960 12.101 26.611 90.00 90.00 105.14 Volume: 2163.33 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7628 7648 7626 7638 11451 10201 10163 15287 N (int>3sigma) = 0 2028 2135 2229 2148 3196 2919 2925 4356 Mean intensity = 0.0 10.1 10.7 12.3 11.8 11.0 12.2 11.5 11.6 Mean int/sigma = 0.0 2.7 2.8 2.9 2.9 2.8 2.9 2.9 2.8 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.892 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 22 217 219 224 N I>3s 0 50 47 3 0.6 18.2 18.0 0.6 0.4 2.7 2.6 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.123 10850 0.5 / 2.6 5.26 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 = 1.168, non-H atomic volume = 19.3 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 s92.ins set up as follows: TITL s92 in P2(1)/n CELL 0.71073 6.9597 26.6109 12.1011 90.000 105.145 90.000 ZERR 4.00 0.0014 0.0053 0.0024 0.000 0.030 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 88 112 16 8 TREF HKLF 4 END -------------------------------------------------------------------------------