++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src0011 started at 15:19:47 on 30-JAN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.491 11.491 16.789 90.00 90.00 90.00 41685 Reflections read from file 2007src0011.hkl; mean (I/sigma) = 17.57 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 20851 20886 20797 20871 31267 27770 27761 41685 N (int>3sigma) = 0 19467 19524 19453 19557 29222 26062 26045 39007 Mean intensity = 0.0 654.0 657.0 675.9 682.5 662.3 687.3 684.4 682.0 Mean int/sigma = 0.0 17.3 17.4 17.6 17.7 17.4 17.6 17.6 17.6 Lattice type: P chosen Volume: 2216.95 ------------------------------------------------------------------------------- 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: 11.491 11.491 16.789 90.00 90.00 90.00 Niggli form: a.a = 132.05 b.b = 132.05 c.c = 281.87 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) = 0.032 [ 39049] Cell: 11.491 11.491 16.789 90.00 90.00 90.00 Volume: 2216.95 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 20851 20886 20797 20871 31267 27770 27761 41685 N (int>3sigma) = 0 19467 19524 19453 19557 29222 26062 26045 39007 Mean intensity = 0.0 654.0 657.0 675.9 682.5 662.3 687.3 684.4 682.0 Mean int/sigma = 0.0 17.3 17.4 17.6 17.7 17.4 17.6 17.6 17.6 Crystal system T and Lattice type P selected Mean |E*E-1| = 0.760 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: 41/43 42 n-- -b- -c- -n- -21- --c N 52 36 809 2174 2128 2144 63 1542 N I>3s 0 0 717 2068 1993 1989 63 1449 3.3 3.5 767.9 749.8 808.1 549.1 391.4 800.6 0.5 0.6 18.4 19.3 19.3 18.0 21.4 21.1 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P4(1) # 76 chiral 1 114 0.032 39049 0.6 / 17.6 1.51 [B] P4(3) # 78 chiral 1 114 0.032 39049 0.6 / 17.6 1.51 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C18H24N5O2S2P3 Formula weight = 499.45 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.496, 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 2007src0011.ins set up as follows: TITL 2007src0011 in P4(1) CELL 0.71073 11.4912 11.4912 16.7890 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0001 0.0002 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 0.4 TREF HKLF 4 END -------------------------------------------------------------------------------