++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 07ch0001 started at 13:26:42 on 31-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 3.977 16.106 11.512 90.00 90.41 90.00 8296 Reflections read from file 07ch0001.hkl; mean (I/sigma) = 5.92 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4159 4153 4144 4154 6228 5540 5543 8296 N (int>3sigma) = 0 2220 2371 2337 2296 3464 3125 3133 4642 Mean intensity = 0.0 16.1 17.4 17.1 16.6 16.9 18.0 18.4 17.6 Mean int/sigma = 0.0 5.7 6.1 6.0 6.0 5.9 6.1 6.1 6.0 Lattice type: P chosen Volume: 737.27 ------------------------------------------------------------------------------- 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: 3.977 11.512 16.106 90.00 90.00 90.41 Niggli form: a.a = 15.81 b.b = 132.51 c.c = 259.41 b.c = 0.00 a.c = 0.00 a.b = -0.32 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.407 deg. ORTHORHOMBIC P-lattice R(int) = 0.455 [ 7243] Cell: 3.977 11.512 16.106 90.00 90.00 90.41 Volume: 737.27 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.057 [ 6533] Cell: 3.977 16.106 11.512 90.00 90.41 90.00 Volume: 737.27 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.407 deg. MONOCLINIC P-lattice R(int) = 0.438 [ 6357] Cell: 11.512 3.977 16.106 90.00 90.00 89.59 Volume: 737.27 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.407 deg. MONOCLINIC P-lattice R(int) = 0.448 [ 6599] Cell: 3.977 11.512 16.106 90.00 90.00 90.41 Volume: 737.27 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4159 4153 4144 4154 6228 5540 5543 8296 N (int>3sigma) = 0 2220 2371 2337 2296 3464 3125 3133 4642 Mean intensity = 0.0 16.1 17.4 17.1 16.6 16.9 18.0 18.4 17.6 Mean int/sigma = 0.0 5.7 6.1 6.0 6.0 5.9 6.1 6.1 6.0 Crystal system M and Lattice type P selected Mean |E*E-1| = 1.099 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 34 172 170 168 N I>3s 0 59 0 59 0.2 16.0 0.2 16.4 0.6 4.3 0.5 4.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.057 6533 0.6 / 4.3 4.35 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H8O4 Formula weight = 168.14 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.515, non-H atomic volume = 15.4 and following cell contents and analysis: C 32.00 57.14 % H 32.00 4.80 % O 16.00 38.06 % F(000) = 352.0 Mo-K(alpha) radiation Mu (mm-1) = 0.12 ------------------------------------------------------------------------------- File 07ch0001.ins set up as follows: TITL 07ch0001 in P2(1)/c CELL 0.71073 3.9766 16.1062 11.5115 90.000 90.407 90.000 ZERR 4.00 0.0003 0.0013 0.0009 0.000 0.005 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O UNIT 32 32 16 TEMP 0.06 TREF HKLF 4 END -------------------------------------------------------------------------------