++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0068 started at 14:16:30 on 14-NOV-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.322 11.203 11.915 90.00 97.79 90.00 19764 Reflections read from file 06skc0068.hkl; mean (I/sigma) = 2.55 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 9922 9869 9835 9915 14813 13177 13173 19764 N (int>3sigma) = 0 2366 2619 2583 2676 3784 3555 3480 5227 Mean intensity = 0.0 18.6 25.2 24.8 25.3 22.8 22.7 28.0 26.4 Mean int/sigma = 0.0 2.5 2.7 2.7 2.7 2.7 2.8 2.7 2.7 Lattice type: P chosen Volume: 1100.72 ------------------------------------------------------------------------------- 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: 8.322 11.203 11.915 90.00 97.79 90.00 Niggli form: a.a = 69.26 b.b = 125.52 c.c = 141.98 b.c = 0.00 a.c = -13.43 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.220 [ 16823] Cell: 8.322 11.203 11.915 90.00 97.79 90.00 Volume: 1100.72 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) = 0.185 [ 14277] Cell: 8.322 11.203 11.915 90.00 82.21 90.00 Volume: 1100.72 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 9922 9869 9835 9915 14813 13173 13177 19764 N (int>3sigma) = 0 2366 2619 2583 2676 3784 3480 3555 5227 Mean intensity = 0.0 18.6 25.2 24.8 25.3 22.8 28.0 22.7 26.4 Mean int/sigma = 0.0 2.5 2.7 2.7 2.7 2.7 2.7 2.8 2.7 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.846 [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 0.185 14277 0.0 / 2.7 5.18 [B] P1 # 1 chiral 1 700 0.185 14277 0.0 / 2.7 5.04 Option [B] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C5H6O5N2 Formula weight = 174.12 Tentative Z (number of formula units/cell) = 5.0 giving rho = 1.313, non-H atomic volume = 18.3 and following cell contents and analysis: C 25.00 34.49 % H 30.00 3.47 % N 10.00 16.09 % O 25.00 45.95 % F(000) = 450.0 Mo-K(alpha) radiation Mu (mm-1) = 0.12 ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C5H6O5N2 Formula weight = 174.12 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.051, non-H atomic volume = 22.9 and following cell contents and analysis: C 20.00 34.49 % H 24.00 3.47 % N 8.00 16.09 % O 20.00 45.95 % F(000) = 360.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File 06skc0068p1.ins set up as follows: TITL 06skc0068p1 in P1 CELL 0.71073 8.3222 11.2034 11.9155 90.000 82.214 90.000 ZERR 4.00 0.0038 0.0053 0.0052 0.000 0.034 0.000 LATT -1 SFAC C H N O UNIT 20 24 8 20 TEMP 0.01 TREF HKLF 4 END 19764 Reflections written to new reflection file 06skc0068p1.hkl -------------------------------------------------------------------------------