++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0018 started at 08:26:13 on 09-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 5.868 13.731 15.418 64.40 90.00 90.07 19254 Reflections read from file 06skc0018.hkl; mean (I/sigma) = 3.89 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 9614 9609 9561 9587 14392 12841 12828 19254 N (int>3sigma) = 0 4006 3756 4188 4085 5975 5337 5407 8121 Mean intensity = 0.0 89.7 69.4 85.4 84.7 81.5 85.7 86.3 87.4 Mean int/sigma = 0.0 4.0 3.6 4.1 4.0 3.9 3.9 4.0 4.0 Lattice type: P chosen Volume: 1120.18 ------------------------------------------------------------------------------- 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: 5.868 13.731 15.418 115.60 90.00 90.07 Niggli form: a.a = 34.43 b.b = 188.53 c.c = 237.72 b.c = -91.49 a.c = 0.00 a.b = -0.10 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.837 deg. ORTHORHOMBIC C-lattice R(int) = 0.577 [ 17730] Cell: 13.731 27.811 5.868 90.04 90.07 89.17 Volume: 2240.36 Matrix: 0.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.083 deg. MONOCLINIC P-lattice R(int) = 0.136 [ 16426] Cell: 13.731 5.868 15.418 90.00 115.60 89.93 Volume: 1120.18 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.834 deg. MONOCLINIC C-lattice R(int) = 0.568 [ 16588] Cell: 13.731 27.811 5.868 90.04 90.07 89.17 Volume: 2240.36 Matrix: 0.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.837 deg. MONOCLINIC C-lattice R(int) = 0.566 [ 16528] Cell: 27.811 13.731 5.868 89.93 90.04 90.83 Volume: 2240.36 Matrix: 0.0000 -1.0000 2.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.121 [ 14167] Cell: 5.868 13.731 15.418 115.60 90.00 90.07 Volume: 1120.18 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 9609 9614 9561 9587 14392 12855 12809 19254 N (int>3sigma) = 0 3756 4006 4188 4085 5975 5326 5397 8121 Mean intensity = 0.0 69.4 89.7 85.4 84.7 81.5 85.5 87.1 87.4 Mean int/sigma = 0.0 3.6 4.0 4.1 4.0 3.9 3.9 4.0 4.0 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.851 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 20 929 943 930 N I>3s 0 322 7 323 5.5 147.7 6.9 147.5 0.8 4.0 0.8 4.0 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.136 16426 0.8 / 4.0 4.49 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H15O4N1S1 Formula weight = 221.27 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.312, non-H atomic volume = 20.0 and following cell contents and analysis: C 32.00 43.42 % H 60.00 6.83 % N 4.00 6.33 % O 16.00 28.92 % S 4.00 14.49 % F(000) = 472.0 Mo-K(alpha) radiation Mu (mm-1) = 0.28 ------------------------------------------------------------------------------- File 06skc0018p21c.ins set up as follows: TITL 06skc0018p21c in P2(1)/c CELL 0.71073 13.7305 5.8676 15.4181 90.000 115.604 90.000 ZERR 4.00 0.0021 0.0006 0.0024 0.000 0.006 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O S UNIT 32 60 4 16 4 TEMP 0.01 TREF HKLF 4 END 19254 Reflections written to new reflection file 06skc0018p21c.hkl -------------------------------------------------------------------------------