++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 11:56:01 on 17-APR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 13.457 10.164 20.303 90.00 104.06 90.00 21623 Reflections read from file s92.hkl; mean (I/sigma) = 3.19 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 10830 10819 10779 10861 16214 14418 14437 21623 N (int>3sigma) = 0 3990 3981 3771 4121 5871 5345 5332 7979 Mean intensity = 0.0 16.6 15.9 13.6 15.5 15.4 14.4 15.2 14.8 Mean int/sigma = 0.0 3.4 3.3 3.2 3.4 3.3 3.4 3.3 3.3 Lattice type: P chosen Volume: 2693.77 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 10.164 13.457 20.303 104.06 90.00 90.00 Niggli form: a.a = 103.30 b.b = 181.09 c.c = 412.23 b.c = -66.36 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.110 [ 15172] Cell: 13.457 10.164 20.303 90.00 104.06 90.00 Volume: 2693.77 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 10830 10819 10779 10861 16214 14418 14437 21623 N (int>3sigma) = 0 3990 3981 3771 4121 5871 5345 5332 7979 Mean intensity = 0.0 16.6 15.9 13.6 15.5 15.4 14.4 15.2 14.8 Mean int/sigma = 0.0 3.4 3.3 3.2 3.4 3.3 3.4 3.3 3.3 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.942 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 10 647 670 689 N I>3s 0 2 205 205 0.4 0.7 28.1 27.4 0.3 0.4 3.1 3.0 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 4 19410 0.110 15172 0.4 / 3.0 3.96 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C30 H19 O10 N7 Formula weight = 637.52 Tentative Z (number of formula units/cell) = 3.0 giving rho = 1.179, non-H atomic volume = 19.1 and following cell contents and analysis: C 90.00 56.52 % H 57.00 3.00 % N 21.00 15.38 % O 30.00 25.10 % F(000) = 984.0 Mo-K(alpha) radiation Mu (mm-1) = 0.09 ------------------------------------------------------------------------------- File s93.ins set up as follows: TITL s93 in P2(1)/c CELL 0.71073 20.3034 10.1636 13.4570 90.000 104.057 90.000 ZERR 3.00 0.0011 0.0005 0.0006 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 90 57 21 30 TREF HKLF 4 END -------------------------------------------------------------------------------