++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0046 started at 16:37:42 on 18-SEP-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 16.640 14.438 7.687 90.00 117.30 90.00 10980 Reflections read from file 06skc0046.hkl; mean (I/sigma) = 8.35 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5489 5489 0 5531 5489 7287 7312 10980 N (int>3sigma) = 0 3169 3169 0 3378 3169 4505 4536 6818 Mean intensity = 0.0 173.5 173.5 0.0 148.4 173.5 197.6 202.7 198.0 Mean int/sigma = 0.0 7.6 7.6 0.0 7.8 7.6 8.5 8.4 8.4 Lattice type: C chosen Volume: 1641.19 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 Unitcell: 7.687 11.015 11.015 81.89 69.73 69.73 Niggli form: a.a = 59.09 b.b = 121.34 c.c = 121.34 b.c = 17.11 a.c = 29.33 a.b = 29.33 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.214 deg. ORTHORHOMBIC I-lattice R(int) = 0.356 [ 9887] Cell: 7.687 14.438 14.787 90.00 89.79 90.00 Volume: 1641.19 Matrix: 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC C-lattice R(int) = 0.056 [ 9023] Cell: 16.640 14.438 7.687 90.00 117.30 90.00 Volume: 1641.19 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.000 deg. MONOCLINIC I-lattice R(int) = 0.056 [ 9023] Cell: 7.687 14.438 14.787 90.00 90.21 90.00 Volume: 1641.19 Matrix: 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.214 deg. MONOCLINIC C-lattice R(int) = 0.348 [ 9032] Cell: 16.357 14.787 7.687 89.79 118.03 90.10 Volume: 1641.19 Matrix: 0.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.214 deg. MONOCLINIC I-lattice R(int) = 0.348 [ 9032] Cell: 14.438 14.787 7.687 89.79 90.00 90.00 Volume: 1641.19 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option F: FOM = 0.214 deg. MONOCLINIC C-lattice R(int) = 0.352 [ 8996] Cell: 20.667 7.687 14.438 90.00 134.32 89.85 Volume: 1641.19 Matrix: 1.0000 1.0000 1.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option G: FOM = 0.214 deg. MONOCLINIC I-lattice R(int) = 0.352 [ 8996] Cell: 14.787 7.687 14.438 90.00 90.00 89.79 Volume: 1641.19 Matrix: 1.0000 0.0000 1.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5489 5489 0 5531 5489 7287 7312 10980 N (int>3sigma) = 0 3169 3169 0 3378 3169 4505 4536 6818 Mean intensity = 0.0 173.5 173.5 0.0 148.4 173.5 197.6 202.7 198.0 Mean int/sigma = 0.0 7.6 7.6 0.0 7.8 7.6 8.5 8.4 8.4 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.938 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 213 N I>3s 1 3.4 0.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.056 9023 0.4 / 8.4 1.36 [B] Cc # 9 non-cen 1 566 0.056 9023 0.4 / 8.4 5.50 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C6H8O5N2 Formula weight = 188.14 Tentative Z (number of formula units/cell) = 4.0 giving rho = 0.761, non-H atomic volume = 31.6 and following cell contents and analysis: C 24.00 38.30 % H 32.00 4.29 % N 8.00 14.89 % O 20.00 42.52 % F(000) = 392.0 Mo-K(alpha) radiation Mu (mm-1) = 0.07 ------------------------------------------------------------------------------- File 06skc0046c2c.ins set up as follows: TITL 06skc0046c2c in C2/c CELL 0.71073 16.6403 14.4382 7.6872 90.000 117.299 90.000 ZERR 4.00 0.0010 0.0005 0.0005 0.000 0.002 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O UNIT 24 32 8 20 TEMP 0.1 TREF HKLF 4 END 10980 Reflections written to new reflection file 06skc0046c2c.hkl -------------------------------------------------------------------------------