++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 07skc0005 started at 11:36:48 on 08-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 5.301 19.374 10.078 90.00 94.01 90.00 8927 Reflections read from file 07skc0005.hkl; mean (I/sigma) = 7.42 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4451 4451 0 4446 4451 5968 5939 8927 N (int>3sigma) = 0 2881 2881 0 2913 2881 4030 4063 6073 Mean intensity = 0.0 192.1 192.1 0.0 209.7 192.1 218.3 200.4 210.0 Mean int/sigma = 0.0 7.2 7.2 0.0 7.2 7.2 7.5 7.5 7.5 Lattice type: C chosen Volume: 1032.43 ------------------------------------------------------------------------------- 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: 5.301 10.043 10.078 88.94 85.99 74.70 Niggli form: a.a = 28.10 b.b = 100.86 c.c = 101.57 b.c = 1.87 a.c = 3.74 a.b = 14.05 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC C-lattice R(int) = 0.057 [ 7701] Cell: 5.301 19.374 10.078 90.00 94.01 90.00 Volume: 1032.43 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 4451 4451 0 4446 4451 5968 5939 8927 N (int>3sigma) = 0 2881 2881 0 2913 2881 4030 4063 6073 Mean intensity = 0.0 192.1 192.1 0.0 209.7 192.1 218.3 200.4 210.0 Mean int/sigma = 0.0 7.2 7.2 0.0 7.2 7.2 7.5 7.5 7.5 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.825 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 142 N I>3s 0 2.7 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.057 7701 0.5 / 7.5 3.48 [B] Cc # 9 non-cen 1 566 0.057 7701 0.5 / 7.5 2.40 Option [B] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H12O5N2 Formula weight = 216.20 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.391, non-H atomic volume = 17.2 and following cell contents and analysis: C 32.00 44.44 % H 48.00 5.59 % N 8.00 12.96 % O 20.00 37.00 % F(000) = 456.0 Mo-K(alpha) radiation Mu (mm-1) = 0.12 ------------------------------------------------------------------------------- File 07skc0005cc.ins set up as follows: TITL 07skc0005cc in Cc CELL 0.71073 5.3007 19.3739 10.0780 90.000 94.012 90.000 ZERR 4.00 0.0004 0.0020 0.0009 0.000 0.006 0.000 LATT -7 SYMM X, -Y, 0.5+Z SFAC C H N O UNIT 32 48 8 20 TEMP 0.09 TREF HKLF 4 END 8927 Reflections written to new reflection file 07skc0005cc.hkl -------------------------------------------------------------------------------