++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04sjc0831 started at 17:11:15 on 06-OCT-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.325 16.496 20.061 89.89 89.98 89.97 21771 Reflections read from file 04sjc0831.hkl; mean (I/sigma) = 4.04 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 10903 10899 10886 10861 16344 14516 14524 21771 N (int>3sigma) = 0 4670 4273 4701 4677 6822 6286 6298 9454 Mean intensity = 0.0 83.6 63.8 83.7 82.6 77.0 83.1 83.4 83.1 Mean int/sigma = 0.0 4.1 3.7 4.2 4.2 4.0 4.2 4.2 4.2 Lattice type: P chosen Volume: 2754.94 ------------------------------------------------------------------------------- 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: 8.325 16.496 20.061 89.89 89.98 89.97 Niggli form: a.a = 69.30 b.b = 272.13 c.c = 402.44 b.c = 0.63 a.c = 0.05 a.b = 0.08 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.114 deg. ORTHORHOMBIC P-lattice R(int) = 0.094 [ 18176] Cell: 8.325 16.496 20.061 89.89 89.98 89.97 Volume: 2754.94 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.039 deg. MONOCLINIC P-lattice R(int) = 0.085 [ 15035] Cell: 16.496 8.325 20.061 89.98 90.11 90.03 Volume: 2754.94 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.111 deg. MONOCLINIC P-lattice R(int) = 0.086 [ 15542] Cell: 8.325 20.061 16.496 89.89 90.03 90.02 Volume: 2754.94 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.114 deg. MONOCLINIC P-lattice R(int) = 0.085 [ 15233] Cell: 8.325 16.496 20.061 89.89 90.02 90.03 Volume: 2754.94 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 10903 10899 10886 10861 16344 14516 14524 21771 N (int>3sigma) = 0 4670 4273 4701 4677 6822 6286 6298 9454 Mean intensity = 0.0 83.6 63.8 83.7 82.6 77.0 83.1 83.4 83.1 Mean int/sigma = 0.0 4.1 3.7 4.2 4.2 4.0 4.2 4.2 4.2 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.944 [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 941 932 935 8 386 384 384 28 318 315 319 20 N I>3s 270 3 271 1 93 18 97 2 105 2 107 1 129.4 3.4 130.7 8.9 78.7 5.1 79.1 5.2 112.4 3.9 112.5 11.6 3.6 0.6 3.7 1.1 2.9 0.8 2.9 0.9 4.2 0.6 4.2 1.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pbca # 61 centro 2 2293 0.094 18176 1.5 / 2.9 4.82 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C14H20O5 Formula weight = 268.30 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.294, non-H atomic volume = 18.1 and following cell contents and analysis: C 112.00 62.67 % H 160.00 7.51 % O 40.00 29.82 % F(000) = 1152.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File 1.ins set up as follows: TITL 1 in Pbca CELL 0.71073 16.4963 8.3249 20.0608 90.000 90.000 90.000 ZERR 8.00 0.0018 0.0030 0.0063 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 O UNIT 112 160 40 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------