++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src0258r started at 18:01:54 on 20-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.489 11.489 16.765 90.00 90.00 90.00 19890 Reflections read from file 2007src0258r.hkl; mean (I/sigma) = 14.02 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 9954 9952 9952 9983 14929 13269 13240 19890 N (int>3sigma) = 0 9309 9315 9326 9384 13975 12468 12435 18657 Mean intensity = 0.0 500.4 492.7 500.8 510.4 498.0 516.3 514.4 508.9 Mean int/sigma = 0.0 13.9 13.9 14.0 14.0 13.9 14.0 14.0 14.0 Lattice type: P chosen Volume: 2212.96 ------------------------------------------------------------------------------- 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: 11.489 11.489 16.765 90.00 90.00 90.00 Niggli form: a.a = 132.00 b.b = 132.00 c.c = 281.05 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) = 0.036 [ 17267] Cell: 11.489 11.489 16.765 90.00 90.00 90.00 Volume: 2212.96 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 9954 9952 9952 9983 14929 13269 13240 19890 N (int>3sigma) = 0 9309 9315 9326 9384 13975 12468 12435 18657 Mean intensity = 0.0 500.4 492.7 500.8 510.4 498.0 516.3 514.4 508.9 Mean int/sigma = 0.0 13.9 13.9 14.0 14.0 13.9 14.0 14.0 14.0 Crystal system T and Lattice type P selected Mean |E*E-1| = 0.742 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: 41/43 42 n-- -b- -c- -n- -21- --c N 42 31 324 1218 1168 1184 28 828 N I>3s 1 1 280 1170 1100 1090 28 776 11.5 13.5 498.0 645.8 816.6 541.0 302.5 588.0 1.1 1.1 13.2 15.2 15.2 14.2 14.3 15.8 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P4(1) # 76 chiral 1 114 0.036 17267 1.1 / 13.2 1.69 [B] P4(3) # 78 chiral 1 114 0.036 17267 1.1 / 13.2 1.69 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C18H24N5O2P3S2 Formula weight = 499.45 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.499, non-H atomic volume = 18.4 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 2007src0258r.ins set up as follows: TITL 2007src0258r in P4(1) CELL 0.71073 11.4892 11.4892 16.7646 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0001 0.0003 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM -Y, X, 0.25+Z SYMM Y, -X, 0.75+Z SFAC C H N O P S UNIT 72 96 20 8 12 8 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------