++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0051 started at 08:36:46 on 12-SEP-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 3.901 17.329 13.863 90.00 96.30 90.00 10034 Reflections read from file 06skc0051.hkl; mean (I/sigma) = 5.67 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5024 4997 4993 5001 7507 6701 6662 10034 N (int>3sigma) = 0 2719 2982 2995 2977 4348 3939 3923 5914 Mean intensity = 0.0 81.6 98.6 96.5 103.5 92.2 99.4 93.1 97.7 Mean int/sigma = 0.0 5.3 5.7 5.8 5.8 5.6 5.8 5.7 5.7 Lattice type: P chosen Volume: 931.61 ------------------------------------------------------------------------------- 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: 3.901 13.863 17.329 90.00 90.00 96.30 Niggli form: a.a = 15.22 b.b = 192.18 c.c = 300.30 b.c = 0.00 a.c = 0.00 a.b = -5.93 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.072 [ 7824] Cell: 3.901 17.329 13.863 90.00 96.30 90.00 Volume: 931.61 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 5024 4997 4993 5001 7507 6701 6662 10034 N (int>3sigma) = 0 2719 2982 2995 2977 4348 3939 3923 5914 Mean intensity = 0.0 81.6 98.6 96.5 103.5 92.2 99.4 93.1 97.7 Mean int/sigma = 0.0 5.3 5.7 5.8 5.8 5.6 5.8 5.7 5.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.935 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 27 210 210 208 N I>3s 0 86 0 86 3.8 151.5 1.9 153.0 1.1 5.2 0.6 5.3 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.072 7824 1.1 / 5.2 2.34 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H12O4N2 Formula weight = 200.20 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.427, non-H atomic volume = 16.6 and following cell contents and analysis: C 32.00 47.99 % H 48.00 6.04 % N 8.00 14.00 % O 16.00 31.97 % F(000) = 424.0 Mo-K(alpha) radiation Mu (mm-1) = 0.12 ------------------------------------------------------------------------------- File 06skc0051p21c.ins set up as follows: TITL 06skc0051p21c in P2(1)/c CELL 0.71073 3.9015 17.3293 13.8628 90.000 96.299 90.000 ZERR 4.00 0.0002 0.0010 0.0007 0.000 0.003 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 32 48 8 16 TEMP 0.06 TREF HKLF 4 END 10034 Reflections written to new reflection file 06skc0051p21c.hkl -------------------------------------------------------------------------------