++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 07skc0027 started at 12:21:38 on 09-May-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 3.954 11.497 18.702 90.00 90.00 90.00 5732 Reflections read from file 07skc0027.hkl; mean (I/sigma) = 5.28 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2856 2878 2834 2836 4284 3804 3805 5732 N (int>3sigma) = 0 1475 1420 1489 1435 2192 1960 1983 2965 Mean intensity = 0.0 183.0 148.4 165.0 195.9 165.5 193.3 190.8 190.3 Mean int/sigma = 0.0 5.4 5.0 5.4 5.4 5.3 5.4 5.4 5.4 Lattice type: P chosen Volume: 850.06 ------------------------------------------------------------------------------- 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: 3.954 11.497 18.702 90.00 90.00 90.00 Niggli form: a.a = 15.63 b.b = 132.17 c.c = 349.78 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(sym) = 0.075 [ 1980] Cell: 3.954 11.497 18.702 90.00 90.00 90.00 Volume: 850.06 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 2856 2878 2834 2836 4284 3804 3805 5732 N (int>3sigma) = 0 1475 1420 1489 1435 2192 1960 1983 2965 Mean intensity = 0.0 183.0 148.4 165.0 195.9 165.5 193.3 190.8 190.3 Mean int/sigma = 0.0 5.4 5.0 5.4 5.4 5.3 5.4 5.4 5.4 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.771 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 414 419 419 5 194 193 183 10 98 85 91 24 N I>3s 217 206 211 0 89 89 0 0 35 1 34 0 214.9 263.9 279.4 2.3 465.2 467.2 6.3 6.1 125.8 8.2 134.7 7.7 6.1 5.9 6.2 0.3 5.9 5.8 0.5 0.5 4.3 0.7 4.5 0.6 Identical indices and Friedel opposites combined before calculating R(sym) Option Space Group No. Type Axes CSD R(sym) N(eq) Syst. Abs. CFOM [A] Pna2(1) # 33 non-cen 3 903 0.075 1980 0.7 / 4.3 2.94 [B] Pnma # 62 centro 2 894 0.075 1980 0.7 / 4.3 6.71 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C7H10O4N2 Formula weight = 186.17 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.455, non-H atomic volume = 16.3 and following cell contents and analysis: C 28.00 45.16 % H 40.00 5.41 % N 8.00 15.05 % O 16.00 34.38 % F(000) = 392.0 Mo-K(alpha) radiation Mu (mm-1) = 0.12 ------------------------------------------------------------------------------- File 07skc0027pna21.ins set up as follows: TITL 07skc0027pna21 in Pna2(1) CELL 0.71073 11.4966 18.7024 3.9535 90.000 90.000 90.000 ZERR 4.00 0.0019 0.0027 0.0005 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, 0.5-Y, Z SYMM 0.5-X, 0.5+Y, 0.5+Z SFAC C H N O UNIT 28 40 8 16 TEMP 0.01 TREF HKLF 4 END 5732 Reflections written to new reflection file 07skc0027pna21.hkl -------------------------------------------------------------------------------