++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0062 started at 18:20:45 on 12-OCT-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.201 23.631 10.406 90.00 95.17 90.00 22674 Reflections read from file 06skc0062.hkl; mean (I/sigma) = 6.13 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 11314 11351 11313 11342 16989 15105 15123 22674 N (int>3sigma) = 0 5670 5849 5531 5689 8525 7807 7773 11626 Mean intensity = 0.0 64.7 91.9 86.7 88.1 81.1 101.3 102.2 100.0 Mean int/sigma = 0.0 5.8 6.3 5.9 6.0 6.0 6.3 6.3 6.3 Lattice type: P chosen Volume: 2253.33 ------------------------------------------------------------------------------- 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: 9.201 10.406 23.631 90.00 90.00 95.17 Niggli form: a.a = 84.65 b.b = 108.29 c.c = 558.43 b.c = 0.00 a.c = 0.00 a.b = -8.63 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.080 [ 19326] Cell: 9.201 23.631 10.406 90.00 95.17 90.00 Volume: 2253.33 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 11314 11351 11313 11342 16989 15105 15123 22674 N (int>3sigma) = 0 5670 5849 5531 5689 8525 7807 7773 11626 Mean intensity = 0.0 64.7 91.9 86.7 88.1 81.1 101.3 102.2 100.0 Mean int/sigma = 0.0 5.8 6.3 5.9 6.0 6.0 6.3 6.3 6.3 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.995 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 37 350 352 358 N I>3s 0 96 95 1 2.3 50.5 49.8 3.3 0.5 4.2 4.2 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.080 19326 0.5 / 4.2 2.75 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C10H12O4N1 Formula weight = 210.21 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.239, non-H atomic volume = 18.8 and following cell contents and analysis: C 80.00 57.13 % H 96.00 5.75 % N 8.00 6.66 % O 32.00 30.45 % F(000) = 888.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File 06skc0062p21n.ins set up as follows: TITL 06skc0062p21n in P2(1)/n CELL 0.71073 9.2008 23.6311 10.4061 90.000 95.173 90.000 ZERR 8.00 0.0003 0.0010 0.0004 0.000 0.003 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 80 96 8 32 TEMP 0.04 TREF HKLF 4 END 22674 Reflections written to new reflection file 06skc0062p21n.hkl -------------------------------------------------------------------------------