++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0034 started at 11:29:46 on 07-AUG-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.462 18.819 7.149 90.00 98.88 90.00 11615 Reflections read from file 06skc0034.hkl; mean (I/sigma) = 3.99 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5803 5800 5799 5803 8701 7731 7744 11615 N (int>3sigma) = 0 2401 2548 2515 2624 3732 3390 3398 5087 Mean intensity = 0.0 87.3 96.4 79.3 74.8 87.7 87.1 88.7 87.1 Mean int/sigma = 0.0 3.9 4.1 4.0 4.2 4.0 4.1 4.1 4.1 Lattice type: P chosen Volume: 859.03 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 6.462 7.149 18.819 90.00 90.00 98.88 Niggli form: a.a = 41.76 b.b = 51.11 c.c = 354.14 b.c = 0.00 a.c = 0.00 a.b = -7.13 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.104 [ 9555] Cell: 6.462 18.819 7.149 90.00 98.88 90.00 Volume: 859.03 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 5803 5800 5799 5803 8701 7731 7744 11615 N (int>3sigma) = 0 2401 2548 2515 2624 3732 3390 3398 5087 Mean intensity = 0.0 87.3 96.4 79.3 74.8 87.7 87.1 88.7 87.1 Mean int/sigma = 0.0 3.9 4.1 4.0 4.2 4.0 4.1 4.1 4.1 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.960 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 41 215 216 209 N I>3s 0 79 0 79 7.7 200.9 3.8 206.7 1.0 4.2 0.6 4.3 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.104 9555 1.0 / 4.1 3.00 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C6H8O4N2 Formula weight = 172.14 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.331, non-H atomic volume = 17.9 and following cell contents and analysis: C 24.00 41.86 % H 32.00 4.68 % N 8.00 16.28 % O 16.00 37.18 % F(000) = 360.0 Mo-K(alpha) radiation Mu (mm-1) = 0.11 ------------------------------------------------------------------------------- File 06skc0034p21c.ins set up as follows: TITL 06skc0034p21c in P2(1)/c CELL 0.71073 6.4624 18.8186 7.1493 90.000 98.878 90.000 ZERR 4.00 0.0004 0.0010 0.0005 0.000 0.004 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 24 32 8 16 TEMP 0.01 TREF HKLF 4 END 11615 Reflections written to new reflection file 06skc0034p21c.hkl -------------------------------------------------------------------------------