++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0013 started at 09:59:49 on 20-MAR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.869 13.299 12.125 90.00 109.50 90.00 18518 Reflections read from file 06skc0013.hkl; mean (I/sigma) = 3.14 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 9260 9292 9274 9292 13913 12355 12359 18518 N (int>3sigma) = 0 3043 3165 3150 2982 4679 4204 4078 6196 Mean intensity = 0.0 83.6 92.6 93.4 83.0 89.9 95.7 86.8 92.5 Mean int/sigma = 0.0 3.2 3.3 3.3 3.1 3.2 3.3 3.2 3.3 Lattice type: P chosen Volume: 1348.09 ------------------------------------------------------------------------------- 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: 8.869 12.125 13.299 90.00 90.00 109.50 Niggli form: a.a = 78.66 b.b = 147.02 c.c = 176.86 b.c = 0.00 a.c = 0.00 a.b = -35.90 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.169 [ 15284] Cell: 8.869 13.299 12.125 90.00 109.50 90.00 Volume: 1348.09 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) = 0.153 [ 12484] Cell: 8.869 12.125 13.299 90.00 90.00 109.50 Volume: 1348.09 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 9260 9292 9274 9292 13913 12355 12359 18518 N (int>3sigma) = 0 3043 3165 3150 2982 4679 4204 4078 6196 Mean intensity = 0.0 83.6 92.6 93.4 83.0 89.9 95.7 86.8 92.5 Mean int/sigma = 0.0 3.2 3.3 3.3 3.1 3.2 3.3 3.2 3.3 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.870 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 25 500 493 497 N I>3s 0 122 124 2 7.6 128.0 130.1 10.6 0.6 2.9 2.9 0.7 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.169 15284 0.7 / 2.9 5.41 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12H18O4N2 Formula weight = 254.28 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.253, non-H atomic volume = 18.7 and following cell contents and analysis: C 48.00 56.68 % H 72.00 7.14 % N 8.00 11.02 % O 16.00 25.17 % F(000) = 544.0 Mo-K(alpha) radiation Mu (mm-1) = 0.09 ------------------------------------------------------------------------------- File 06skc0013.ins set up as follows: TITL 06skc0013 in P2(1)/n CELL 0.71073 8.8691 13.2988 12.1250 90.000 109.500 90.000 ZERR 4.00 0.0007 0.0017 0.0014 0.000 0.007 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 48 72 8 16 TEMP 0.01 TREF HKLF 4 END 18518 Reflections written to new reflection file 06skc0013.hkl -------------------------------------------------------------------------------