++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 13:15:30 on 30-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 20.573 17.974 25.379 90.00 101.58 90.00 63765 Reflections read from file s92.hkl; mean (I/sigma) = 2.11 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 31909 31909 0 31854 31909 42517 42497 63765 N (int>3sigma) = 0 6145 6145 0 6056 6145 8727 8636 12873 Mean intensity = 0.0 5.0 5.0 0.0 4.9 5.0 5.5 5.5 5.7 Mean int/sigma = 0.0 2.2 2.2 0.0 2.2 2.2 2.3 2.3 2.3 Lattice type: C chosen Volume: 9193.68 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 Unitcell: 13.660 13.660 25.379 81.30 81.30 82.29 Niggli form: a.a = 186.58 b.b = 186.58 c.c = 644.08 b.c = 52.42 a.c = 52.42 a.b = 25.05 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC C-lattice R(int) = 0.233 [ 51276] Cell: 20.573 17.974 25.379 90.00 101.58 90.00 Volume: 9193.69 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) = 0.209 [ 42117] Cell: 13.660 13.660 25.379 81.30 81.30 82.29 Volume: 4596.84 Matrix:-0.5000 0.5000 0.0000 -0.5000 -0.5000 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 31909 31909 0 31854 31909 42517 42497 63765 N (int>3sigma) = 0 6145 6145 0 6056 6145 8727 8636 12873 Mean intensity = 0.0 5.0 5.0 0.0 4.9 5.0 5.5 5.5 5.7 Mean int/sigma = 0.0 2.2 2.2 0.0 2.2 2.2 2.3 2.3 2.3 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.942 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 1235 N I>3s 2 0.7 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.233 51276 0.5 / 2.3 5.53 [B] Cc # 9 non-cen 1 566 0.233 51276 0.5 / 2.3 9.87 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C53 H60 O6 N4 Formula weight = 849.05 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.227, non-H atomic volume = 18.2 and following cell contents and analysis: C 424.00 74.97 % H 480.00 7.12 % N 32.00 6.60 % O 48.00 11.31 % F(000) = 3632.0 Mo-K(alpha) radiation Mu (mm-1) = 0.08 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in C2/c CELL 0.71073 20.5733 17.9742 25.3788 90.000 101.582 90.000 ZERR 8.00 0.0041 0.0036 0.0051 0.000 0.030 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O UNIT 424 480 32 48 TREF HKLF 4 END -------------------------------------------------------------------------------