++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0035 started at 10:14:14 on 23-AUG-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.698 8.617 10.908 74.60 89.99 89.99 16487 Reflections read from file 06skc0035.hkl; mean (I/sigma) = 5.09 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8230 8262 8190 8245 12341 10961 10994 16487 N (int>3sigma) = 0 4627 4725 4468 4678 6910 6174 6207 9273 Mean intensity = 0.0 133.7 116.2 109.1 137.4 119.7 133.5 126.8 127.7 Mean int/sigma = 0.0 5.2 5.2 4.9 5.2 5.1 5.2 5.1 5.2 Lattice type: P chosen Volume: 697.58 ------------------------------------------------------------------------------- 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: 7.698 8.617 10.908 74.60 89.99 89.99 Niggli form: a.a = 59.27 b.b = 74.25 c.c = 118.98 b.c = 24.96 a.c = 0.02 a.b = 0.01 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.014 deg. MONOCLINIC P-lattice R(int) = 0.075 [ 14735] Cell: 8.617 7.698 10.908 89.99 105.40 90.01 Volume: 697.58 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 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 8262 8230 8190 8245 12341 10977 10966 16487 N (int>3sigma) = 0 4725 4627 4468 4678 6910 6175 6200 9273 Mean intensity = 0.0 116.2 133.7 109.1 137.4 119.7 132.1 130.7 127.7 Mean int/sigma = 0.0 5.2 5.2 4.9 5.2 5.1 5.2 5.1 5.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 1.033 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 21 635 632 635 N I>3s 2 2 226 228 6.2 2.5 216.9 216.0 1.4 0.6 4.3 4.3 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 4 19410 0.075 14735 1.4 / 4.3 3.38 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H14O5N1 Formula weight = 204.20 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.944, non-H atomic volume = 12.5 and following cell contents and analysis: C 32.00 47.05 % H 56.00 6.91 % N 4.00 6.86 % O 20.00 39.18 % F(000) = 436.0 Mo-K(alpha) radiation Mu (mm-1) = 0.16 ------------------------------------------------------------------------------- File 06skc0035p21c.ins set up as follows: TITL 06skc0035p21c in P2(1)/c CELL 0.71073 10.9078 7.6984 8.6167 90.000 105.403 90.000 ZERR 4.00 0.0005 0.0002 0.0003 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 32 56 4 20 TEMP 0.08 TREF HKLF 4 END 16487 Reflections written to new reflection file 06skc0035p21c.hkl -------------------------------------------------------------------------------