++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 10:22:28 on 26-MAR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.077 11.839 22.695 91.84 90.07 89.95 16091 Reflections read from file s92.hkl; mean (I/sigma) = 1.24 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8101 8064 7999 8022 12082 10693 10729 16091 N (int>3sigma) = 0 959 1028 1073 929 1530 1417 1433 2142 Mean intensity = 0.0 2.8 2.9 3.2 2.5 3.0 3.0 2.9 3.0 Mean int/sigma = 0.0 1.4 1.5 1.5 1.4 1.5 1.5 1.5 1.5 Lattice type: P chosen Volume: 2169.14 ------------------------------------------------------------------------------- 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: 8.077 11.839 22.695 88.16 89.93 89.95 Niggli form: a.a = 65.24 b.b = 140.16 c.c = 515.06 b.c = 8.63 a.c = 0.21 a.b = 0.08 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.081 deg. MONOCLINIC P-lattice R(int) = 0.408 [ 12262] Cell: 11.839 8.077 22.695 90.07 91.84 89.95 Volume: 2169.14 Matrix: 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.357 [ 9729] Cell: 8.077 11.839 22.695 88.16 89.93 89.95 Volume: 2169.14 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 Option A selected ------------------------------------------------------------------------------- Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8064 8101 7999 8022 12082 10729 10693 16091 N (int>3sigma) = 0 1028 959 1073 929 1530 1433 1417 2142 Mean intensity = 0.0 2.9 2.8 3.2 2.5 3.0 2.9 3.0 3.0 Mean int/sigma = 0.0 1.5 1.4 1.5 1.4 1.5 1.5 1.5 1.5 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.827 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 9 773 789 784 N I>3s 0 114 114 0 0.1 5.6 5.5 0.6 0.3 1.8 1.8 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.408 12262 0.5 / 1.5 11.51 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C23 H26 O8 Formula weight = 430.44 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.318, non-H atomic volume = 17.5 and following cell contents and analysis: C 92.00 64.17 % H 104.00 6.09 % O 32.00 29.74 % F(000) = 912.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File s93.ins set up as follows: TITL s93 in P2(1)/n CELL 0.71073 11.8390 8.0773 22.6950 90.000 91.840 90.000 ZERR 4.00 0.0024 0.0016 0.0045 0.000 0.030 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H O UNIT 92 104 32 TREF HKLF 4 END -------------------------------------------------------------------------------