++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 07skc0014 started at 14:48:16 on 17-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.745 8.715 11.306 101.83 91.51 92.37 8728 Reflections read from file 07skc0014.hkl; mean (I/sigma) = 6.30 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4343 4369 4364 4350 6538 5811 5812 8728 N (int>3sigma) = 0 2749 2757 2750 2733 4128 3665 3592 5463 Mean intensity = 0.0 128.7 141.1 132.2 134.2 134.0 126.5 118.9 131.0 Mean int/sigma = 0.0 6.4 6.5 6.3 6.4 6.4 6.4 6.3 6.4 Lattice type: P chosen Volume: 649.55 ------------------------------------------------------------------------------- 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: 6.745 8.715 11.306 101.83 91.51 92.37 Niggli form: a.a = 45.50 b.b = 75.96 c.c = 127.82 b.c = -20.21 a.c = -2.01 a.b = -2.43 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.057 [ 5758] Cell: 6.745 8.715 11.306 101.83 91.51 92.37 Volume: 649.55 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 4343 4369 4364 4350 6538 5811 5812 8728 N (int>3sigma) = 0 2749 2757 2750 2733 4128 3665 3592 5463 Mean intensity = 0.0 128.7 141.1 132.2 134.2 134.0 126.5 118.9 131.0 Mean int/sigma = 0.0 6.4 6.5 6.3 6.4 6.4 6.4 6.3 6.4 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.977 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P-1 # 2 centro 1 8646 0.057 5758 0.0 / 6.4 1.59 [B] P1 # 1 chiral 1 700 0.057 5758 0.0 / 6.4 7.53 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C10H11O4N1 Formula weight = 209.20 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.070, non-H atomic volume = 21.7 and following cell contents and analysis: C 20.00 57.41 % H 22.00 5.30 % N 2.00 6.70 % O 8.00 30.59 % F(000) = 220.0 Mo-K(alpha) radiation Mu (mm-1) = 0.08 ------------------------------------------------------------------------------- File 07skc0014.ins set up as follows: TITL 07skc0014 in P-1 CELL 0.71073 6.7452 8.7155 11.3058 101.834 91.509 92.367 ZERR 2.00 0.0003 0.0005 0.0006 0.003 0.003 0.003 LATT 1 SFAC C H N O UNIT 20 22 2 8 TEMP 0.02 TREF HKLF 4 END 8728 Reflections written to new reflection file 07skc0014.hkl -------------------------------------------------------------------------------