++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 05skc0002 started at 14:02:51 on 16-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 5.158 5.326 7.522 78.73 83.33 79.08 4317 Reflections read from file 05skc0002.hkl; mean (I/sigma) = 12.43 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2146 2132 2140 2140 3209 2876 2905 4317 N (int>3sigma) = 0 1887 1891 1852 1869 2815 2514 2525 3788 Mean intensity = 0.0 530.6 533.9 526.9 519.8 530.4 508.5 528.0 503.5 Mean int/sigma = 0.0 12.7 12.7 12.3 12.5 12.6 12.5 12.3 12.4 Lattice type: P chosen Volume: 198.31 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 5.158 5.326 7.522 78.73 83.33 79.08 Niggli form: a.a = 26.60 b.b = 28.37 c.c = 56.58 b.c = 7.83 a.c = 4.51 a.b = 5.21 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.037 [ 3407] Cell: 5.158 5.326 7.522 78.73 83.33 79.08 Volume: 198.31 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 2146 2132 2140 2140 3209 2876 2905 4317 N (int>3sigma) = 0 1887 1891 1852 1869 2815 2514 2525 3788 Mean intensity = 0.0 530.6 533.9 526.9 519.8 530.4 508.5 528.0 503.5 Mean int/sigma = 0.0 12.7 12.7 12.3 12.5 12.6 12.5 12.3 12.4 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.797 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P-1 # 2 centro 1 8646 0.037 3407 0.0 / 12.4 3.75 [B] P1 # 1 chiral 1 700 0.037 3407 0.0 / 12.4 1.31 Option [B] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C5O6N1H11 Formula weight = 181.15 Tentative Z (number of formula units/cell) = 1.0 giving rho = 1.517, non-H atomic volume = 16.5 and following cell contents and analysis: C 5.00 33.15 % H 11.00 6.12 % N 1.00 7.73 % O 6.00 53.00 % F(000) = 96.0 Mo-K(alpha) radiation Mu (mm-1) = 0.14 ------------------------------------------------------------------------------- File 05skc0002p1.ins set up as follows: TITL 05skc0002p1 in P1 CELL 0.71073 5.1580 5.3261 7.5218 78.735 83.330 79.077 ZERR 1.00 0.0005 0.0007 0.0006 0.008 0.010 0.011 LATT -1 SFAC C H N O UNIT 5 11 1 6 TEMP 0.02 TREF HKLF 4 END 4317 Reflections written to new reflection file 05skc0002p1.hkl -------------------------------------------------------------------------------