++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04mbh0607 started at 14:21:13 on 28-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.388 14.227 21.744 90.01 93.87 89.99 23934 Reflections read from file 04mbh0607.hkl; mean (I/sigma) = 6.10 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 11955 11966 11929 11947 17925 15947 15923 23934 N (int>3sigma) = 0 6192 6376 6246 6338 9407 8557 8483 12719 Mean intensity = 0.0 115.9 120.9 109.7 122.3 115.5 116.6 119.7 117.8 Mean int/sigma = 0.0 6.1 6.2 5.9 6.2 6.1 6.2 6.2 6.2 Lattice type: P chosen Volume: 2280.35 ------------------------------------------------------------------------------- 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: 7.388 14.227 21.744 89.99 86.13 89.99 Niggli form: a.a = 54.59 b.b = 202.40 c.c = 472.80 b.c = 0.05 a.c = 10.84 a.b = 0.01 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.011 deg. MONOCLINIC P-lattice R(int) = 0.062 [ 18459] Cell: 7.388 14.227 21.744 90.01 93.87 89.99 Volume: 2280.35 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 11955 11966 11929 11947 17925 15947 15923 23934 N (int>3sigma) = 0 6192 6376 6246 6338 9407 8557 8483 12719 Mean intensity = 0.0 115.9 120.9 109.7 122.3 115.5 116.6 119.7 117.8 Mean int/sigma = 0.0 6.1 6.2 5.9 6.2 6.1 6.2 6.2 6.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.986 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 27 423 410 413 N I>3s 0 162 2 164 2.4 130.2 3.7 133.7 0.5 5.2 0.6 5.3 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.062 18459 0.6 / 5.2 2.19 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C4 H6 O6 Formula weight = 150.09 Tentative Z (number of formula units/cell) = 13.0 giving rho = 1.421, non-H atomic volume = 17.5 and following cell contents and analysis: C 52.00 32.01 % H 78.00 4.03 % O 78.00 63.96 % F(000) = 1014.0 Mo-K(alpha) radiation Mu (mm-1) = 0.14 ------------------------------------------------------------------------------- File 04mbh0607.ins set up as follows: TITL 04mbh0607 in P2(1)/c CELL 0.71073 7.3883 14.2268 21.7440 90.000 93.867 90.000 ZERR 13.00 0.0026 0.0048 0.0077 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O UNIT 52 78 78 TEMP 0.03 TREF HKLF 4 END -------------------------------------------------------------------------------