++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src0258 started at 22:31:48 on 27-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.501 11.501 16.783 90.00 90.00 90.00 56868 Reflections read from file 2007src0258.hkl; mean (I/sigma) = 11.68 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 28480 28480 28446 28460 42703 37934 37901 56868 N (int>3sigma) = 0 25303 25267 25402 25394 37986 33849 33827 50667 Mean intensity = 0.0 465.4 460.4 467.4 478.5 464.4 480.9 479.5 476.3 Mean int/sigma = 0.0 11.5 11.5 11.7 11.7 11.6 11.7 11.7 11.7 Lattice type: P chosen Volume: 2219.95 ------------------------------------------------------------------------------- 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: 11.501 11.501 16.783 90.00 90.00 90.00 Niggli form: a.a = 132.27 b.b = 132.27 c.c = 281.68 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) = 0.044 [ 54224] Cell: 11.501 11.501 16.783 90.00 90.00 90.00 Volume: 2219.95 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 28480 28480 28446 28460 42703 37934 37901 56868 N (int>3sigma) = 0 25303 25267 25402 25394 37986 33849 33827 50667 Mean intensity = 0.0 465.4 460.4 467.4 478.5 464.4 480.9 479.5 476.3 Mean int/sigma = 0.0 11.5 11.5 11.7 11.7 11.6 11.7 11.7 11.7 Crystal system T and Lattice type P selected Mean |E*E-1| = 0.770 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: 41/43 42 n-- -b- -c- -n- -21- --c N 81 60 858 3154 3087 3087 70 2159 N I>3s 1 1 723 2934 2801 2755 70 1991 3.0 2.8 551.8 583.7 729.3 491.2 298.8 588.8 0.6 0.6 10.7 13.3 13.3 12.3 11.9 14.2 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P4(1) # 76 chiral 1 114 0.044 54224 0.6 / 10.7 1.97 [B] P4(3) # 78 chiral 1 114 0.044 54224 0.6 / 10.7 1.97 Option [B] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C18H24N5O2P3S2 Formula weight = 499.45 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.494, non-H atomic volume = 18.5 and following cell contents and analysis: C 72.00 43.28 % H 96.00 4.84 % N 20.00 14.03 % O 8.00 6.41 % P 12.00 18.60 % S 8.00 12.84 % F(000) = 1040.0 Mo-K(alpha) radiation Mu (mm-1) = 0.48 ------------------------------------------------------------------------------- File 2007src0258.ins set up as follows: TITL 2007src0258 in P4(3) CELL 0.71073 11.5009 11.5009 16.7834 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0001 0.0001 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 P S UNIT 72 96 20 8 12 8 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------