++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0012 started at 18:49:08 on 27-MAR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.197 14.666 14.340 90.00 90.00 90.00 23268 Reflections read from file 06skc0012.hkl; mean (I/sigma) = 4.02 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 11592 11656 11632 11633 17440 15487 15523 23268 N (int>3sigma) = 0 4445 4436 4609 4619 6745 5994 5933 9121 Mean intensity = 0.0 81.9 83.5 85.2 97.0 83.5 90.6 90.9 91.8 Mean int/sigma = 0.0 4.0 4.0 4.2 4.1 4.1 4.1 4.1 4.2 Lattice type: P chosen Volume: 1724.02 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 8.197 14.340 14.666 90.00 90.00 90.00 Niggli form: a.a = 67.19 b.b = 205.65 c.c = 215.09 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(int) = 0.160 [ 21792] Cell: 8.197 14.340 14.666 90.00 90.00 90.00 Volume: 1724.02 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.156 [ 20654] Cell: 8.197 14.666 14.340 90.00 90.00 90.00 Volume: 1724.02 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 P-lattice R(int) = 0.156 [ 20565] Cell: 14.340 8.197 14.666 90.00 90.00 90.00 Volume: 1724.02 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.155 [ 20648] Cell: 8.197 14.340 14.666 90.00 90.00 90.00 Volume: 1724.02 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.147 [ 18302] Cell: 8.197 14.340 14.666 90.00 90.00 90.00 Volume: 1724.02 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 11592 11632 11656 11633 17440 15515 15487 23268 N (int>3sigma) = 0 4445 4609 4436 4619 6745 5962 5994 9121 Mean intensity = 0.0 81.9 85.2 83.5 97.0 83.5 91.0 90.6 91.8 Mean int/sigma = 0.0 4.0 4.2 4.0 4.1 4.1 4.1 4.1 4.2 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.778 [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 1031 1027 1024 22 628 633 641 42 501 510 509 49 N I>3s 461 472 451 0 272 297 293 0 200 220 208 0 128.3 110.9 153.2 5.1 103.3 202.4 191.7 9.0 249.3 332.7 136.3 3.0 5.1 5.1 5.0 0.4 5.4 5.9 6.0 0.6 5.3 6.3 5.1 0.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)2(1)2(1) # 19 chiral 1 5917 0.160 21792 0.6 / 4.2 2.81 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C5H6O3N1 Formula weight = 128.11 Tentative Z (number of formula units/cell) = 12.0 giving rho = 1.481, non-H atomic volume = 16.0 and following cell contents and analysis: C 60.00 46.87 % H 72.00 4.72 % N 12.00 10.94 % O 36.00 37.47 % F(000) = 804.0 Mo-K(alpha) radiation Mu (mm-1) = 0.12 ------------------------------------------------------------------------------- File 06skc0012p212121.ins set up as follows: TITL 06skc0012p212121 in P2(1)2(1)2(1) CELL 0.71073 8.1972 14.3404 14.6661 90.000 90.000 90.000 ZERR 12.00 0.0010 0.0020 0.0015 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O UNIT 60 72 12 36 TEMP 0.06 TREF HKLF 4 END 23268 Reflections written to new reflection file 06skc0012p212121.hkl -------------------------------------------------------------------------------