++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + S92 started at 11:19:23 on 04-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.418 16.684 27.993 90.00 90.00 90.00 20380 Reflections read from file s92.hkl; mean (I/sigma) = 2.97 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 10199 10207 10216 10193 15311 13590 13574 20380 N (int>3sigma) = 0 2904 2934 2674 2947 4256 3946 3967 5910 Mean intensity = 0.0 9.2 8.3 7.3 9.0 8.3 9.3 9.3 9.2 Mean int/sigma = 0.0 3.2 3.0 2.8 3.1 3.0 3.2 3.2 3.2 Lattice type: P chosen Volume: 3464.50 ------------------------------------------------------------------------------- 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: 7.418 16.684 27.993 90.00 90.00 90.00 Niggli form: a.a = 55.03 b.b = 278.35 c.c = 783.63 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) = 0.179 [ 15881] Cell: 7.418 16.684 27.993 90.00 90.00 90.00 Volume: 3464.50 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. MONOCLINIC P-lattice R(int) = 0.152 [ 12298] Cell: 7.418 27.993 16.684 90.00 90.00 90.00 Volume: 3464.50 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.156 [ 12403] Cell: 7.418 16.684 27.993 90.00 90.00 90.00 Volume: 3464.50 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.148 [ 11958] Cell: 16.684 7.418 27.993 90.00 90.00 90.00 Volume: 3464.50 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.091 [ 5934] Cell: 7.418 16.684 27.993 90.00 90.00 90.00 Volume: 3464.50 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 10199 10207 10216 10193 15311 13590 13574 20380 N (int>3sigma) = 0 2904 2934 2674 2947 4256 3946 3967 5910 Mean intensity = 0.0 9.2 8.3 7.3 9.0 8.3 9.3 9.3 9.2 Mean int/sigma = 0.0 3.2 3.0 2.8 3.1 3.0 3.2 3.2 3.2 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.909 [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 949 951 956 6 437 444 439 15 220 222 216 41 N I>3s 0 247 247 0 0 100 100 0 0 43 43 0 0.6 16.0 15.9 0.4 0.6 5.4 5.4 0.4 0.7 16.8 17.2 0.2 0.4 3.1 3.1 0.3 0.4 2.5 2.5 0.3 0.4 2.9 3.0 0.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pbca # 61 centro 1 2293 0.179 15881 0.4 / 2.5 5.23 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C21 H16 O9 Formula weight = 412.34 Tentative Z (number of formula units/cell) = 7.0 giving rho = 1.383, non-H atomic volume = 16.5 and following cell contents and analysis: C 147.00 61.17 % H 112.00 3.91 % O 63.00 34.92 % F(000) = 1498.0 Mo-K(alpha) radiation Mu (mm-1) = 0.11 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL S92 in Pbca CELL 0.71073 7.4181 16.6837 27.9934 90.000 90.000 90.000 ZERR 7.00 0.0015 0.0033 0.0056 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 147 112 63 TREF HKLF 4 END -------------------------------------------------------------------------------