++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0028 started at 10:27:12 on 24-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.352 14.038 20.577 90.04 89.81 89.91 47818 Reflections read from file 06skc0028.hkl; mean (I/sigma) = 2.51 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 23940 23963 23923 23939 35913 31838 31835 47818 N (int>3sigma) = 0 7165 7155 6720 7684 10520 10101 10059 14968 Mean intensity = 0.0 43.4 35.9 38.8 44.7 39.4 46.6 46.5 46.7 Mean int/sigma = 0.0 2.6 2.6 2.5 2.7 2.5 2.7 2.7 2.7 Lattice type: P chosen Volume: 2123.75 ------------------------------------------------------------------------------- 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: 7.352 14.038 20.577 90.04 90.19 90.09 Niggli form: a.a = 54.05 b.b = 197.07 c.c = 423.41 b.c = -0.18 a.c = -0.50 a.b = -0.16 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.208 deg. ORTHORHOMBIC P-lattice R(int) = 0.170 [ 44972] Cell: 7.352 14.038 20.577 90.04 89.81 89.91 Volume: 2123.75 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.096 deg. MONOCLINIC P-lattice R(int) = 0.165 [ 42681] Cell: 7.352 14.038 20.577 90.04 90.19 90.09 Volume: 2123.75 Matrix: 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.191 deg. MONOCLINIC P-lattice R(int) = 0.165 [ 42749] Cell: 7.352 20.577 14.038 89.96 90.09 89.81 Volume: 2123.75 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.208 deg. MONOCLINIC P-lattice R(int) = 0.165 [ 42504] Cell: 14.038 7.352 20.577 89.81 90.04 89.91 Volume: 2123.75 Matrix: 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.154 [ 38043] Cell: 7.352 14.038 20.577 90.04 90.19 90.09 Volume: 2123.75 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 23940 23963 23923 23939 35913 31838 31835 47818 N (int>3sigma) = 0 7165 7155 6720 7684 10520 10101 10059 14968 Mean intensity = 0.0 43.4 35.9 38.8 44.7 39.4 46.6 46.5 46.7 Mean int/sigma = 0.0 2.6 2.6 2.5 2.7 2.5 2.7 2.7 2.7 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.899 [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 2041 2040 2033 21 1088 1104 1110 50 707 697 690 69 N I>3s 3 524 525 1 296 298 4 0 192 2 192 1 3.5 50.3 50.5 3.4 127.6 125.9 3.4 3.0 50.9 3.0 52.1 3.5 0.6 2.5 2.5 0.8 2.6 2.6 0.6 0.7 2.6 0.6 2.6 0.7 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pccn # 56 centro 5 196 0.170 44972 0.8 / 2.5 6.33 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C7H10O4N2 Formula weight = 186.17 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.165, non-H atomic volume = 20.4 and following cell contents and analysis: C 56.00 45.16 % H 80.00 5.41 % N 16.00 15.05 % O 32.00 34.38 % F(000) = 784.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File 06skc0028pccn.ins set up as follows: TITL 06skc0028pccn in Pccn CELL 0.71073 20.5769 7.3521 14.0383 90.000 90.000 90.000 ZERR 8.00 0.0012 0.0004 0.0008 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, 0.5-Y, Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, -Y, 0.5-Z SFAC C H N O UNIT 56 80 16 32 TEMP 0.2 TREF HKLF 4 END 47818 Reflections written to new reflection file 06skc0028pccn.hkl -------------------------------------------------------------------------------