++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2006src0567 started at 17:26:35 on 03-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 14.830 6.093 15.411 90.00 109.50 90.00 2151 Reflections read from file 2006src0567.hkl; mean (I/sigma) = 9.10 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1034 1034 0 1079 1034 1441 1444 2151 N (int>3sigma) = 0 673 673 0 734 673 1034 1045 1547 Mean intensity = 0.0 296.1 296.1 0.0 303.6 296.1 368.8 389.9 376.2 Mean int/sigma = 0.0 8.0 8.0 0.0 8.6 8.0 9.1 9.2 9.2 Lattice type: C chosen Volume: 1312.56 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 -0.5000 -1.0000 Unitcell: 6.093 8.016 15.016 77.47 78.30 67.67 Niggli form: a.a = 37.12 b.b = 64.26 c.c = 225.48 b.c = 26.12 a.c = 18.56 a.b = 18.56 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC C-lattice R(int) = 0.048 [ 888] Cell: 14.830 6.093 15.411 90.00 109.50 90.00 Volume: 1312.56 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 1034 1034 0 1079 1034 1441 1444 2151 N (int>3sigma) = 0 673 673 0 734 673 1034 1045 1547 Mean intensity = 0.0 296.1 296.1 0.0 303.6 296.1 368.8 389.9 376.2 Mean int/sigma = 0.0 8.0 8.0 0.0 8.6 8.0 9.1 9.2 9.2 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.786 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 105 N I>3s 2 14.9 0.8 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.048 888 0.8 / 9.2 4.52 [B] Cc # 9 non-cen 1 566 0.048 888 0.8 / 9.2 1.60 Option [B] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C4H8Cl4N3O2P3 Formula weight = 364.84 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.846, non-H atomic volume = 20.5 and following cell contents and analysis: C 16.00 13.17 % H 32.00 2.21 % N 12.00 11.52 % O 8.00 8.77 % P 12.00 25.47 % Cl 16.00 38.87 % F(000) = 728.0 Mo-K(alpha) radiation Mu (mm-1) = 1.25 ------------------------------------------------------------------------------- File 2006src0567.ins set up as follows: TITL 2006src0567 in Cc CELL 0.71073 14.8296 6.0926 15.4113 90.000 109.500 90.000 ZERR 4.00 0.0009 0.0003 0.0012 0.000 0.003 0.000 LATT -7 SYMM X, -Y, 0.5+Z SFAC C H N O P CL UNIT 16 32 12 8 12 16 TEMP 0.2 TREF HKLF 4 END -------------------------------------------------------------------------------