++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 06skc0072 started at 14:21:01 on 22-NOV-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.641 6.292 22.249 90.00 96.15 90.00 14684 Reflections read from file 06skc0072.hkl; mean (I/sigma) = 2.24 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7343 7312 7323 7340 10989 9801 9783 14684 N (int>3sigma) = 0 1985 1915 1952 1928 2926 2671 2631 3955 Mean intensity = 0.0 136.9 135.1 130.2 142.5 134.0 136.4 136.9 134.1 Mean int/sigma = 0.0 2.4 2.3 2.4 2.4 2.4 2.4 2.4 2.4 Lattice type: P chosen Volume: 1620.15 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 6.292 11.641 22.249 96.15 90.00 90.00 Niggli form: a.a = 39.58 b.b = 135.52 c.c = 495.00 b.c = -27.74 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.251 [ 10700] Cell: 11.641 6.292 22.249 90.00 96.15 90.00 Volume: 1620.15 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.216 [ 7838] Cell: 6.292 11.641 22.249 83.85 90.00 90.00 Volume: 1620.15 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 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 7343 7312 7323 7340 10989 9801 9783 14684 N (int>3sigma) = 0 1985 1915 1952 1928 2926 2671 2631 3955 Mean intensity = 0.0 136.9 135.1 130.2 142.5 134.0 136.4 136.9 134.1 Mean int/sigma = 0.0 2.4 2.3 2.4 2.4 2.4 2.4 2.4 2.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.771 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 7 799 821 810 N I>3s 1 265 270 257 16.0 245.8 309.0 333.1 1.4 3.0 2.9 2.8 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2 # 3 chiral 1 29 0.251 10700 0.0 / 1.4 10.80 [B] P2/m # 10 centro 1 21 0.251 10700 0.0 / 1.4 15.77 [C] Pm # 6 non-cen 1 1 0.251 10700 0.0 / 1.4 57.47 [D] P2(1) # 4 chiral 1 3543 0.251 10700 1.4 / 2.4 4.84 [E] P2(1)/m # 11 centro 1 402 0.251 10700 1.4 / 2.4 8.81 Option [D] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C14H26O3N1S1 Formula weight = 288.42 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.182, non-H atomic volume = 21.3 and following cell contents and analysis: C 56.00 58.30 % H 104.00 9.09 % N 4.00 4.86 % O 12.00 16.64 % S 4.00 11.12 % F(000) = 628.0 Mo-K(alpha) radiation Mu (mm-1) = 0.20 ------------------------------------------------------------------------------- File 06skc0072p21.ins set up as follows: TITL 06skc0072p21 in P2(1) CELL 0.71073 11.6414 6.2915 22.2485 90.000 96.148 90.000 ZERR 4.00 0.0017 0.0008 0.0032 0.000 0.007 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O S UNIT 56 104 4 12 4 TEMP 0.02 TREF HKLF 4 END 14684 Reflections written to new reflection file 06skc0072p21.hkl -------------------------------------------------------------------------------