++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04mbh0603 started at 16:54:54 on 29-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 20.104 7.630 15.302 90.01 129.99 89.96 10029 Reflections read from file 04mbh0603.hkl; mean (I/sigma) = 6.57 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5039 5039 0 5022 5039 6690 6680 10029 N (int>3sigma) = 0 3065 3065 0 3244 3065 4434 4401 6664 Mean intensity = 0.0 156.7 156.7 0.0 191.0 156.7 205.7 197.9 203.6 Mean int/sigma = 0.0 6.1 6.1 0.0 6.5 6.1 6.6 6.6 6.6 Lattice type: C chosen Volume: 1798.21 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 Unitcell: 7.630 10.749 12.329 82.76 71.99 69.25 Niggli form: a.a = 58.21 b.b = 115.55 c.c = 152.01 b.c = 16.71 a.c = 29.08 a.b = 29.06 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.040 deg. MONOCLINIC C-lattice R(int) = 0.059 [ 7828] Cell: 20.104 7.630 15.302 90.01 129.99 89.96 Volume: 1798.21 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.040 deg. MONOCLINIC I-lattice R(int) = 0.059 [ 7828] Cell: 15.302 7.630 15.586 89.96 98.79 89.99 Volume: 1798.21 Matrix: 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5039 5039 0 5022 5039 6690 6680 10029 N (int>3sigma) = 0 3065 3065 0 3244 3065 4434 4401 6664 Mean intensity = 0.0 156.7 156.7 0.0 191.0 156.7 205.7 197.9 203.6 Mean int/sigma = 0.0 6.1 6.1 0.0 6.5 6.1 6.6 6.6 6.6 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.994 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 406 N I>3s 3 2.8 0.6 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.059 7828 0.6 / 6.6 1.74 [B] Cc # 9 non-cen 1 566 0.059 7828 0.6 / 6.6 8.50 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C5 H6 O6 N1 Formula weight = 176.11 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.301, non-H atomic volume = 18.7 and following cell contents and analysis: C 40.00 34.10 % H 48.00 3.43 % N 8.00 7.96 % O 48.00 54.51 % F(000) = 728.0 Mo-K(alpha) radiation Mu (mm-1) = 0.12 ------------------------------------------------------------------------------- File 04mbh0603.ins set up as follows: TITL 04mbh0603 in C2/c CELL 0.71073 20.1042 7.6296 15.3016 90.000 129.990 90.000 ZERR 8.00 0.0040 0.0015 0.0031 0.000 0.030 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O UNIT 40 48 8 48 TEMP 0.05 TREF HKLF 4 END -------------------------------------------------------------------------------