++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0061 started at 10:58:59 on 10-OCT-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.790 8.806 10.729 106.79 89.98 90.06 8668 Reflections read from file 06skc0061.hkl; mean (I/sigma) = 6.65 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4313 4419 4480 4217 6606 5819 5725 8668 N (int>3sigma) = 0 2658 2783 2593 2587 4017 3577 3498 5290 Mean intensity = 0.0 240.0 231.5 200.2 242.8 223.7 227.1 227.5 228.0 Mean int/sigma = 0.0 7.0 7.0 6.3 6.8 6.8 6.8 6.7 6.7 Lattice type: P chosen Volume: 704.58 ------------------------------------------------------------------------------- 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: 7.790 8.806 10.729 73.21 89.98 89.94 Niggli form: a.a = 60.68 b.b = 77.55 c.c = 115.10 b.c = 27.30 a.c = 0.03 a.b = 0.07 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.062 deg. MONOCLINIC P-lattice R(int) = 0.047 [ 7344] Cell: 8.806 7.790 10.729 90.02 106.79 89.94 Volume: 704.58 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) = 0.043 [ 6441] Cell: 7.790 8.806 10.729 73.21 89.98 89.94 Volume: 704.58 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 4419 4313 4480 4217 6606 5702 5759 8668 N (int>3sigma) = 0 2783 2658 2593 2587 4017 3481 3534 5290 Mean intensity = 0.0 231.5 240.0 200.2 242.8 223.7 219.2 222.7 228.0 Mean int/sigma = 0.0 7.0 7.0 6.3 6.8 6.8 6.7 6.7 6.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.929 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 21 604 469 453 N I>3s 0 1 136 135 2.6 2.4 222.7 230.6 0.5 0.4 4.0 4.2 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 4 19410 0.047 7344 0.5 / 4.0 2.93 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H12O5N1 Formula weight = 202.19 Tentative Z (number of formula units/cell) = 2.0 giving rho = 0.953, non-H atomic volume = 25.2 and following cell contents and analysis: C 16.00 47.52 % H 24.00 5.98 % N 2.00 6.93 % O 10.00 39.57 % F(000) = 214.0 Mo-K(alpha) radiation Mu (mm-1) = 0.08 ------------------------------------------------------------------------------- File 06skc0061p21c.ins set up as follows: TITL 06skc0061p21c in P2(1)/c CELL 0.71073 10.7285 7.7897 8.8064 90.000 106.793 90.000 ZERR 2.00 0.0004 0.0003 0.0003 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 16 24 2 10 TEMP 0.16 TREF HKLF 4 END 8668 Reflections written to new reflection file 06skc0061p21c.hkl -------------------------------------------------------------------------------