++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + s92 started at 15:40:11 on 01-Oct-2002 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 5.408 16.587 16.685 90.00 90.00 90.00 4160 Reflections read from file s92.hkl; mean (I/sigma) = 5.57 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2110 2059 2081 2088 3125 2748 2778 4160 N (int>3sigma) = 0 1255 1250 1251 1259 1878 1666 1693 2505 Mean intensity = 0.0 63.9 71.8 70.0 74.8 68.5 71.5 72.7 71.9 Mean int/sigma = 0.0 5.6 5.6 5.7 5.6 5.6 5.7 5.7 5.6 Lattice type: P chosen Volume: 1496.70 ------------------------------------------------------------------------------- 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: 5.408 16.587 16.685 90.00 90.00 90.00 Niggli form: a.a = 29.25 b.b = 275.13 c.c = 278.41 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.170 deg. TETRAGONAL P-lattice R(sym) = 0.572 [ 2109] Cell: 16.587 16.685 5.408 90.00 90.00 90.00 Volume: 1496.70 Matrix: 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(sym) = 0.193 [ 2019] Cell: 5.408 16.587 16.685 90.00 90.00 90.00 Volume: 1496.70 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(sym) = 0.060 [ 1090] Cell: 5.408 16.685 16.587 90.00 90.00 90.00 Volume: 1496.70 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.202 [ 1100] Cell: 5.408 16.587 16.685 90.00 90.00 90.00 Volume: 1496.70 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.219 [ 907] Cell: 16.587 5.408 16.685 90.00 90.00 90.00 Volume: 1496.70 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Option C selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2110 2081 2059 2088 3125 2775 2778 4160 N (int>3sigma) = 0 1255 1251 1250 1259 1878 1652 1693 2505 Mean intensity = 0.0 63.9 70.0 71.8 74.8 68.5 71.5 72.7 71.9 Mean int/sigma = 0.0 5.6 5.7 5.6 5.6 5.6 5.6 5.7 5.6 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.861 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 10 79 78 77 N I>3s 0 31 1 30 1.7 95.1 1.7 97.4 0.7 4.0 0.7 3.9 Identical indices and Friedel opposites combined before calculating R(sym) Option Space Group No. Type Axes CSD R(sym) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.060 1090 0.7 / 3.9 4.15 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 s92.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.25 145 159 91.2 2.50 330.9 16.58 0.0542 0.0546 2.25 - 1.75 156 161 96.9 1.94 144.1 13.37 0.0616 0.0696 1.75 - 1.50 176 189 93.1 1.73 74.6 10.87 0.0682 0.0789 1.50 - 1.35 147 158 93.0 1.57 52.7 9.25 0.0604 0.0870 1.35 - 1.25 177 188 94.1 1.43 45.3 7.57 0.0895 0.1087 1.25 - 1.15 210 240 87.5 1.29 59.3 8.01 0.0490 0.1022 1.15 - 1.05 266 320 83.1 1.17 34.1 6.28 0.0807 0.1351 1.05 - 1.00 193 235 82.1 1.12 29.7 5.35 0.1057 0.1491 1.00 - 0.95 224 277 80.9 1.11 22.3 4.62 0.1089 0.1800 0.95 - 0.90 243 302 80.5 1.03 15.8 3.33 0.1290 0.2631 0.90 - 0.85 345 449 76.8 0.98 16.8 2.95 0.1690 0.2877 0.85 - 0.80 366 505 72.5 0.88 12.4 2.19 0.2224 0.4086 0.80 - 0.78 138 254 54.3 0.63 10.0 1.75 0.2420 0.5451 ------------------------------------------------------------------------------ 0.90 - 0.78 849 1208 70.3 0.86 13.8 2.43 0.1943 0.3651 Inf - 0.78 2786 3437 81.1 1.21 52.8 6.24 0.0638 0.1108 Merged [A], lowest resolution = 5.88 Angstroms, 69 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 s92.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C18H19O2N1S1 Formula weight = 313.40 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.391, non-H atomic volume = 17.0 and following cell contents and analysis: C 72.00 68.98 % H 76.00 6.11 % N 4.00 4.47 % O 8.00 10.21 % S 4.00 10.23 % F(000) = 664.0 Mo-K(alpha) radiation Mu (mm-1) = 0.22 ------------------------------------------------------------------------------- File s93.ins set up as follows: TITL s93 in P2(1)/c CELL 0.71073 5.4079 16.6855 16.5870 90.000 90.000 90.000 ZERR 4.00 0.0009 0.0029 0.0026 0.000 0.000 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O S UNIT 72 76 4 8 4 TREF HKLF 4 END -------------------------------------------------------------------------------