++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 09:08:23 on 03-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.651 8.651 20.538 90.00 90.00 90.00 4779 Reflections read from file s92.hkl; mean (I/sigma) = 15.33 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2387 2389 2372 2377 3574 3181 3190 4779 N (int>3sigma) = 0 2198 2200 2198 2196 3298 2928 2941 4413 Mean intensity = 0.0 214.4 202.2 208.8 194.6 208.5 212.0 211.7 207.8 Mean int/sigma = 0.0 15.4 15.3 15.5 15.2 15.4 15.3 15.3 15.3 Lattice type: P chosen Volume: 1537.24 ------------------------------------------------------------------------------- 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: 8.651 8.651 20.538 90.00 90.00 90.00 Niggli form: a.a = 74.85 b.b = 74.85 c.c = 421.83 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TETRAGONAL P-lattice R(int) = 0.028 [ 3011] Cell: 8.651 8.651 20.538 90.00 90.00 90.00 Volume: 1537.24 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 2387 2389 2372 2377 3574 3181 3190 4779 N (int>3sigma) = 0 2198 2200 2198 2196 3298 2928 2941 4413 Mean intensity = 0.0 214.4 202.2 208.8 194.6 208.5 212.0 211.7 207.8 Mean int/sigma = 0.0 15.4 15.3 15.5 15.2 15.4 15.3 15.3 15.3 Crystal system T and Lattice type P selected Mean |E*E-1| = 0.797 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: 41/43 42 n-- -b- -c- -n- -21- --c N 9 5 68 320 320 322 8 209 N I>3s 1 0 59 309 297 300 8 192 1.0 1.1 324.3 261.3 244.0 247.9 220.9 319.1 1.4 1.1 16.3 17.8 16.6 16.7 19.3 18.3 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P4(1) # 76 chiral 1 114 0.028 3011 1.4 / 15.3 1.91 [B] P4(3) # 78 chiral 1 114 0.028 3011 1.4 / 15.3 1.91 Option [B] chosen ------------------------------------------------------------------------------- ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C15 H16 N3 S1 O2 Formula weight = 302.37 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.306, non-H atomic volume = 18.3 and following cell contents and analysis: C 60.00 59.58 % H 64.00 5.33 % N 12.00 13.90 % O 8.00 10.58 % S 4.00 10.60 % F(000) = 636.0 Mo-K(alpha) radiation Mu (mm-1) = 0.22 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P4(3) CELL 0.71073 8.6514 8.6514 20.5385 90.000 90.000 90.000 ZERR 4.00 0.0012 0.0012 0.0041 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM -Y, X, 0.75+Z SYMM Y, -X, 0.25+Z SFAC C H N O S UNIT 60 64 12 8 4 TREF HKLF 4 END -------------------------------------------------------------------------------