++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04skc0013 started at 10:29:05 on 10-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.143 9.494 14.362 90.00 94.41 89.98 14183 Reflections read from file 04skc0013.hkl; mean (I/sigma) = 6.96 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7098 7099 7107 7090 10652 9449 9461 14183 N (int>3sigma) = 0 4213 4465 4462 4466 6570 5818 5822 8777 Mean intensity = 0.0 154.5 190.8 196.3 197.7 180.5 190.9 185.4 185.2 Mean int/sigma = 0.0 6.5 7.1 7.1 7.1 6.9 7.0 7.0 7.0 Lattice type: P chosen Volume: 1107.04 ------------------------------------------------------------------------------- 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: 8.143 9.494 14.362 90.00 85.59 89.98 Niggli form: a.a = 66.31 b.b = 90.14 c.c = 206.26 b.c = 0.01 a.c = 9.00 a.b = 0.02 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.016 deg. MONOCLINIC P-lattice R(int) = 0.055 [ 11461] Cell: 8.143 9.494 14.362 90.00 94.41 89.98 Volume: 1107.04 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 7098 7099 7107 7090 10652 9449 9461 14183 N (int>3sigma) = 0 4213 4465 4462 4466 6570 5818 5822 8777 Mean intensity = 0.0 154.5 190.8 196.3 197.7 180.5 190.9 185.4 185.2 Mean int/sigma = 0.0 6.5 7.1 7.1 7.1 6.9 7.0 7.0 7.0 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.956 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 16 491 502 495 N I>3s 1 196 0 196 2.8 304.8 2.7 302.5 0.8 5.9 0.6 5.8 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.055 11461 0.8 / 5.8 1.91 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H17O6N1 Formula weight = 223.23 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.339, non-H atomic volume = 18.5 and following cell contents and analysis: C 32.00 43.04 % H 68.00 7.68 % N 4.00 6.28 % O 24.00 43.01 % F(000) = 480.0 Mo-K(alpha) radiation Mu (mm-1) = 0.11 ------------------------------------------------------------------------------- File 04skc0013p21c.ins set up as follows: TITL 04skc0013p21c in P2(1)/c CELL 0.71073 8.1431 9.4941 14.3618 90.000 94.415 90.000 ZERR 4.00 0.0013 0.0019 0.0031 0.000 0.015 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 32 68 4 24 TEMP 0.03 TREF HKLF 4 END 14183 Reflections written to new reflection file 04skc0013p21c.hkl -------------------------------------------------------------------------------