++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 09:17:54 on 09-MAR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.489 9.493 27.453 91.48 88.32 73.52 17661 Reflections read from file s92.hkl; mean (I/sigma) = 4.09 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8817 8829 8870 8852 13258 11778 11780 17661 N (int>3sigma) = 0 3396 3344 3494 3374 5117 4554 4526 6806 Mean intensity = 0.0 13.8 12.4 14.0 14.0 13.4 14.0 13.7 14.2 Mean int/sigma = 0.0 4.2 4.1 4.3 4.2 4.2 4.2 4.2 4.2 Lattice type: P chosen Volume: 2368.73 ------------------------------------------------------------------------------- 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: 9.489 9.493 27.453 91.48 91.68 106.48 Niggli form: a.a = 90.04 b.b = 90.11 c.c = 753.69 b.c = -6.74 a.c = -7.63 a.b = -25.55 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.125 deg. MONOCLINIC C-lattice R(int) = 0.530 [ 11629] Cell: 11.360 15.207 27.453 89.88 92.64 89.98 Volume: 4737.46 Matrix: 1.0000 -1.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.101 [ 7676] Cell: 9.489 9.493 27.453 91.48 91.68 106.48 Volume: 2368.73 Matrix: 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8817 8829 8870 8852 13258 11756 11771 17661 N (int>3sigma) = 0 3396 3344 3494 3374 5117 4597 4513 6806 Mean intensity = 0.0 13.8 12.4 14.0 14.0 13.4 14.0 14.2 14.2 Mean int/sigma = 0.0 4.2 4.1 4.3 4.2 4.2 4.2 4.2 4.2 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.895 [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 0.101 7676 0.0 / 4.2 2.92 [B] P1 # 1 chiral 1 700 0.101 7676 0.0 / 4.2 5.03 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C30 H23 N3 O2 Formula weight = 457.51 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.283, non-H atomic volume = 16.9 and following cell contents and analysis: C 120.00 78.75 % H 92.00 5.07 % N 12.00 9.19 % O 8.00 6.99 % F(000) = 960.0 Mo-K(alpha) radiation Mu (mm-1) = 0.08 ------------------------------------------------------------------------------- File s93.ins set up as follows: TITL s93 in P-1 CELL 0.71073 9.4890 9.4925 27.4534 91.483 91.679 106.480 ZERR 4.00 0.0019 0.0019 0.0055 0.030 0.030 0.030 LATT 1 SFAC C H N O UNIT 120 92 12 8 TREF HKLF 4 END -------------------------------------------------------------------------------