++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 07skc0003 started at 12:36:31 on 05-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.816 12.754 14.190 90.00 90.00 90.00 4648 Reflections read from file 07skc0003.hkl; mean (I/sigma) = 5.96 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2292 2292 0 2308 2292 3111 3126 4648 N (int>3sigma) = 0 1282 1282 0 1240 1282 1781 1776 2685 Mean intensity = 0.0 177.0 177.0 0.0 151.7 177.0 208.1 204.3 211.2 Mean int/sigma = 0.0 5.7 5.7 0.0 5.7 5.7 6.0 6.0 6.1 Lattice type: C chosen Volume: 1233.44 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 Unitcell: 6.816 7.230 14.190 90.00 90.00 61.88 Niggli form: a.a = 46.45 b.b = 52.28 c.c = 201.35 b.c = 0.00 a.c = 0.00 a.b = 23.23 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. ORTHORHOMBIC C-lattice R(int) = 0.064 [ 3812] Cell: 6.816 12.754 14.190 90.00 90.00 90.00 Volume: 1233.44 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 2292 2292 0 2308 2292 3111 3126 4648 N (int>3sigma) = 0 1282 1282 0 1240 1282 1781 1776 2685 Mean intensity = 0.0 177.0 177.0 0.0 151.7 177.0 208.1 204.3 211.2 Mean int/sigma = 0.0 5.7 5.7 0.0 5.7 5.7 6.0 6.0 6.1 Crystal system O and Lattice type C selected Mean |E*E-1| = 1.054 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: c-- n-- -c- -n- --a --b --21 N 247 247 109 109 95 95 22 N I>3s 154 154 1 1 60 60 0 233.9 233.9 3.9 3.9 600.6 600.6 4.3 6.7 6.7 0.7 0.7 6.8 6.8 0.8 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Cmc2(1) # 36 non-cen 1 102 0.064 3812 0.8 / 6.1 12.91 [B] Cmcm # 63 centro 1 100 0.064 3812 0.8 / 6.1 3.57 [C] Ama2 # 40 non-cen 4 21 0.064 3812 0.8 / 6.1 16.49 Option [B] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C10H16O5N1 Formula weight = 230.24 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.240, non-H atomic volume = 19.3 and following cell contents and analysis: C 40.00 52.16 % H 64.00 7.00 % N 4.00 6.09 % O 20.00 34.75 % F(000) = 492.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File 07skc0003cmcm.ins set up as follows: TITL 07skc0003cmcm in Cmcm CELL 0.71073 6.8156 12.7537 14.1899 90.000 90.000 90.000 ZERR 4.00 0.0006 0.0012 0.0011 0.000 0.000 0.000 LATT 7 SYMM -X, -Y, 0.5+Z SYMM -X, Y, 0.5-Z SYMM X, -Y, -Z SFAC C H N O UNIT 40 64 4 20 TEMP 0.01 TREF HKLF 4 END 4648 Reflections written to new reflection file 07skc0003cmcm.hkl -------------------------------------------------------------------------------