++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2006SRC0702 started at 22:28:46 on 13-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 15.948 12.191 16.523 90.00 99.19 90.00 42429 Reflections read from file 2006src0702.hkl; mean (I/sigma) = 9.07 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 21247 21224 21199 21200 31835 28305 28321 42429 N (int>3sigma) = 0 12940 13980 13484 13623 20202 18140 18206 27231 Mean intensity = 0.0 132.1 113.9 140.9 143.3 129.0 139.3 140.0 139.8 Mean int/sigma = 0.0 8.8 9.1 9.2 9.3 9.0 9.2 9.2 9.2 Lattice type: P chosen Volume: 3171.20 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 12.191 15.948 16.523 99.19 90.00 90.00 Niggli form: a.a = 148.61 b.b = 254.35 c.c = 273.02 b.c = -42.08 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.048 [ 34804] Cell: 15.948 12.191 16.523 90.00 99.19 90.00 Volume: 3171.20 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 21247 21224 21199 21200 31835 28305 28321 42429 N (int>3sigma) = 0 12940 13980 13484 13623 20202 18140 18206 27231 Mean intensity = 0.0 132.1 113.9 140.9 143.3 129.0 139.3 140.0 139.8 Mean int/sigma = 0.0 8.8 9.1 9.2 9.3 9.0 9.2 9.2 9.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.994 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 27 1239 1259 1250 N I>3s 2 501 0 501 1.2 122.7 1.9 121.6 0.7 7.2 0.4 7.1 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.048 34804 0.7 / 7.1 1.57 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C7H14Cl4N3O2P3 Formula weight = 406.92 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.705, non-H atomic volume = 20.9 and following cell contents and analysis: C 56.00 20.66 % H 112.00 3.47 % N 24.00 10.33 % O 16.00 7.86 % P 24.00 22.83 % Cl 32.00 34.85 % F(000) = 1648.0 Mo-K(alpha) radiation Mu (mm-1) = 1.05 ------------------------------------------------------------------------------- File 2006src0702.ins set up as follows: TITL 2006SRC0702 in P2(1)/c CELL 0.71073 15.9483 12.1905 16.5233 90.000 99.189 90.000 ZERR 8.00 0.0005 0.0003 0.0004 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O P CL UNIT 56 112 24 16 24 32 TEMP 0.2 TREF HKLF 4 END -------------------------------------------------------------------------------