++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + s92 started at 10:44:17 on 19-Nov-2002 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.164 10.897 24.763 90.00 93.38 90.00 12209 Reflections read from file s92.hkl; mean (I/sigma) = 9.38 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6058 6096 6116 6096 9135 8153 8119 12209 N (int>3sigma) = 0 3919 4060 4103 4144 6041 5493 5438 8228 Mean intensity = 0.0 62.8 72.8 58.5 62.0 64.7 67.8 66.0 66.3 Mean int/sigma = 0.0 9.1 9.3 9.4 9.4 9.3 9.5 9.4 9.4 Lattice type: P chosen Volume: 1660.48 ------------------------------------------------------------------------------- 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: 6.164 10.897 24.763 90.00 93.38 90.00 Niggli form: a.a = 38.00 b.b = 118.74 c.c = 613.21 b.c = 0.00 a.c = -9.01 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.043 [ 2325] Cell: 6.164 10.897 24.763 90.00 93.38 90.00 Volume: 1660.48 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 6058 6096 6116 6096 9135 8153 8119 12209 N (int>3sigma) = 0 3919 4060 4103 4144 6041 5493 5438 8228 Mean intensity = 0.0 62.8 72.8 58.5 62.0 64.7 67.8 66.0 66.3 Mean int/sigma = 0.0 9.1 9.3 9.4 9.4 9.3 9.5 9.4 9.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.985 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 8 337 281 328 N I>3s 0 170 0 170 0.9 79.9 0.8 82.0 0.7 8.4 0.5 8.7 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 0.043 2325 0.7 / 8.4 1.28 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 - 2.05 201 225 89.3 5.65 247.9 46.35 0.0591 0.0177 2.05 - 1.65 207 210 98.6 4.76 115.3 33.84 0.0635 0.0232 1.65 - 1.45 196 199 98.5 4.19 65.6 23.94 0.0693 0.0294 1.45 - 1.30 239 239 100.0 4.13 52.7 21.52 0.0682 0.0321 1.30 - 1.20 218 218 100.0 3.62 56.5 19.90 0.0780 0.0367 1.20 - 1.10 323 323 100.0 3.27 50.8 17.38 0.0700 0.0420 1.10 - 1.05 194 196 99.0 3.14 38.4 13.88 0.0808 0.0505 1.05 - 1.00 252 252 100.0 2.98 29.9 11.65 0.0915 0.0607 1.00 - 0.95 314 315 99.7 2.71 22.9 9.16 0.0993 0.0805 0.95 - 0.90 347 349 99.4 2.62 21.8 8.59 0.1048 0.0921 0.90 - 0.85 471 487 96.7 2.29 18.3 6.50 0.1341 0.1222 0.85 - 0.80 533 585 91.1 2.11 17.1 5.51 0.1512 0.1502 0.80 - 0.77 359 407 88.2 1.93 16.0 4.72 0.1546 0.1815 ------------------------------------------------------------------------------ 0.90 - 0.77 1363 1479 92.2 2.12 17.2 5.64 0.1457 0.1476 Inf - 0.77 3854 4005 96.2 3.05 47.0 14.34 0.0714 0.0493 Merged [A], lowest resolution = 6.57 Angstroms, 975 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 s92.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C20H19N1O2S1 Formula weight = 337.42 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.350, non-H atomic volume = 17.3 and following cell contents and analysis: C 80.00 71.19 % H 76.00 5.68 % N 4.00 4.15 % O 8.00 9.48 % S 4.00 9.50 % F(000) = 712.0 Mo-K(alpha) radiation Mu (mm-1) = 0.21 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/c CELL 0.71073 6.1644 10.8967 24.7631 90.000 93.383 90.000 ZERR 4.00 0.0001 0.0003 0.0007 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O S UNIT 80 76 4 8 4 TREF HKLF 4 END -------------------------------------------------------------------------------