++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 07skc0021 started at 18:46:03 on 18-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.281 7.934 9.491 67.22 76.46 67.85 6449 Reflections read from file 07skc0021.hkl; mean (I/sigma) = 8.48 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3231 3237 3222 3223 4845 4334 4297 6449 N (int>3sigma) = 0 2411 2399 2418 2426 3614 3257 3181 4835 Mean intensity = 0.0 212.4 212.2 233.6 235.0 219.4 207.5 231.3 230.7 Mean int/sigma = 0.0 8.5 8.4 8.5 8.6 8.5 8.5 8.4 8.5 Lattice type: P chosen Volume: 465.64 ------------------------------------------------------------------------------- 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: 7.281 7.934 9.491 67.22 76.46 67.85 Niggli form: a.a = 53.01 b.b = 62.94 c.c = 90.08 b.c = 29.16 a.c = 16.18 a.b = 21.78 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.046 [ 4300] Cell: 7.281 7.934 9.491 67.22 76.46 67.85 Volume: 465.64 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 3231 3237 3222 3223 4845 4334 4297 6449 N (int>3sigma) = 0 2411 2399 2418 2426 3614 3257 3181 4835 Mean intensity = 0.0 212.4 212.2 233.6 235.0 219.4 207.5 231.3 230.7 Mean int/sigma = 0.0 8.5 8.4 8.5 8.6 8.5 8.5 8.4 8.5 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.934 [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 0.046 4300 0.0 / 8.5 1.30 [B] P1 # 1 chiral 1 700 0.046 4300 0.0 / 8.5 5.25 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C9H15O5N1 Formula weight = 217.22 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.549, non-H atomic volume = 15.5 and following cell contents and analysis: C 18.00 49.76 % H 30.00 6.96 % N 2.00 6.45 % O 10.00 36.83 % F(000) = 232.0 Mo-K(alpha) radiation Mu (mm-1) = 0.13 ------------------------------------------------------------------------------- File 07skc0021p-1.ins set up as follows: TITL 07skc0021p-1 in P-1 CELL 0.71073 7.2807 7.9336 9.4911 67.216 76.457 67.849 ZERR 2.00 0.0004 0.0005 0.0006 0.002 0.003 0.004 LATT 1 SFAC C H N O UNIT 18 30 2 10 TEMP 0.04 TREF HKLF 4 END 6449 Reflections written to new reflection file 07skc0021p-1.hkl -------------------------------------------------------------------------------