++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 07skc0001 started at 15:45:25 on 27-JAN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.502 13.373 27.693 90.00 90.00 90.00 14749 Reflections read from file 07skc0001.hkl; mean (I/sigma) = 3.82 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7353 7350 7351 7365 11027 9836 9816 14749 N (int>3sigma) = 0 2883 2721 2900 2953 4252 3915 3864 5881 Mean intensity = 0.0 240.0 191.1 225.9 211.7 219.0 241.8 245.4 235.3 Mean int/sigma = 0.0 3.9 3.7 3.9 3.9 3.8 4.0 4.0 4.0 Lattice type: P chosen Volume: 3148.87 ------------------------------------------------------------------------------- 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: 8.502 13.373 27.693 90.00 90.00 90.00 Niggli form: a.a = 72.29 b.b = 178.84 c.c = 766.91 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(int) = 0.100 [ 11263] Cell: 8.502 13.373 27.693 90.00 90.00 90.00 Volume: 3148.87 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 7353 7350 7351 7365 11027 9836 9816 14749 N (int>3sigma) = 0 2883 2721 2900 2953 4252 3915 3864 5881 Mean intensity = 0.0 240.0 191.1 225.9 211.7 219.0 241.8 245.4 235.3 Mean int/sigma = 0.0 3.9 3.7 3.9 3.9 3.8 4.0 4.0 4.0 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.903 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 585 568 583 5 424 413 417 14 200 177 197 20 N I>3s 190 4 190 0 117 2 115 0 92 0 92 0 295.0 15.5 296.6 19.8 258.0 13.2 261.6 11.8 557.6 9.7 565.9 13.4 3.5 0.7 3.5 0.9 3.2 0.6 3.2 0.8 5.1 0.7 5.1 0.6 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pbca # 61 centro 2 2293 0.100 11263 0.9 / 3.2 4.44 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12H23O6N1 Formula weight = 277.31 Tentative Z (number of formula units/cell) = 9.0 giving rho = 1.316, non-H atomic volume = 18.4 and following cell contents and analysis: C 108.00 51.97 % H 207.00 8.36 % N 9.00 5.05 % O 54.00 34.62 % F(000) = 1350.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File 07skc0001pbca.ins set up as follows: TITL 07skc0001pbca in Pbca CELL 0.71073 13.3732 8.5025 27.6932 90.000 90.000 90.000 ZERR 9.00 0.0016 0.0009 0.0034 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O UNIT 108 207 9 54 TEMP 0.02 TREF HKLF 4 END 14749 Reflections written to new reflection file 07skc0001pbca.hkl -------------------------------------------------------------------------------