++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 16:10:36 on 21-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 25.529 18.972 9.713 90.00 103.11 90.00 24093 Reflections read from file s92.hkl; mean (I/sigma) = 6.72 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 12039 12039 0 12074 12039 16059 16058 24093 N (int>3sigma) = 0 7191 7191 0 7260 7191 9825 9846 14689 Mean intensity = 0.0 45.3 45.3 0.0 44.6 45.3 46.6 47.3 45.6 Mean int/sigma = 0.0 6.7 6.7 0.0 6.6 6.7 6.8 6.8 6.8 Lattice type: C chosen Volume: 4581.75 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 0.5000 -0.5000 0.0000 Unitcell: 9.713 15.903 15.903 73.23 79.51 79.51 Niggli form: a.a = 94.34 b.b = 252.92 c.c = 252.92 b.c = 72.96 a.c = 28.12 a.b = 28.12 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC C-lattice R(int) = 0.095 [ 18749] Cell: 25.529 18.972 9.713 90.00 103.11 90.00 Volume: 4581.75 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 I-lattice R(int) = 0.095 [ 18749] Cell: 9.713 18.972 25.171 90.00 98.96 90.00 Volume: 4581.75 Matrix: 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 12039 12039 0 12074 12039 16059 16058 24093 N (int>3sigma) = 0 7191 7191 0 7260 7191 9825 9846 14689 Mean intensity = 0.0 45.3 45.3 0.0 44.6 45.3 46.6 47.3 45.6 Mean int/sigma = 0.0 6.7 6.7 0.0 6.6 6.7 6.8 6.8 6.8 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.912 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 311 N I>3s 3 0.9 0.6 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.095 18749 0.6 / 6.8 1.94 [B] Cc # 9 non-cen 1 566 0.095 18749 0.6 / 6.8 4.86 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C26 H30 N3 O2 Formula weight = 416.53 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.208, non-H atomic volume = 18.5 and following cell contents and analysis: C 208.00 74.97 % H 240.00 7.26 % N 24.00 10.09 % O 16.00 7.68 % F(000) = 1784.0 Mo-K(alpha) radiation Mu (mm-1) = 0.08 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in C2/c CELL 0.71073 25.5294 18.9718 9.7130 90.000 103.111 90.000 ZERR 8.00 0.0051 0.0038 0.0019 0.000 0.030 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O UNIT 208 240 24 16 TREF HKLF 4 END -------------------------------------------------------------------------------