++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src0194 started at 16:28:13 on 06-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.048 27.138 10.499 90.00 96.18 90.00 17520 Reflections read from file 2007src0194.hkl; mean (I/sigma) = 8.01 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8771 8750 8799 8794 13160 11655 11711 17520 N (int>3sigma) = 0 6436 6455 6449 6494 9670 8640 8617 12966 Mean intensity = 0.0 313.3 326.8 307.9 352.5 316.0 330.4 336.3 334.8 Mean int/sigma = 0.0 7.9 8.0 7.9 8.0 8.0 8.1 8.0 8.1 Lattice type: P chosen Volume: 1712.97 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 6.048 10.499 27.138 90.00 90.00 96.18 Niggli form: a.a = 36.57 b.b = 110.22 c.c = 736.45 b.c = 0.00 a.c = 0.00 a.b = -6.83 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.052 [ 13555] Cell: 6.048 27.138 10.499 90.00 96.18 90.00 Volume: 1712.97 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 8771 8750 8799 8794 13160 11655 11711 17520 N (int>3sigma) = 0 6436 6455 6449 6494 9670 8640 8617 12966 Mean intensity = 0.0 313.3 326.8 307.9 352.5 316.0 330.4 336.3 334.8 Mean int/sigma = 0.0 7.9 8.0 7.9 8.0 8.0 8.1 8.0 8.1 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.936 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 76 226 212 220 N I>3s 1 107 14 103 2.9 861.7 5.2 885.4 0.8 6.0 1.1 6.1 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.052 13555 1.1 / 6.0 2.16 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C6H4ClF8N3O2P3 Formula weight = 430.48 Tentative Z (number of formula units/cell) = 5.0 giving rho = 2.087, non-H atomic volume = 14.9 and following cell contents and analysis: C 30.00 16.74 % H 20.00 0.94 % N 15.00 9.76 % O 10.00 7.43 % F 40.00 35.31 % P 15.00 21.58 % Cl 5.00 8.23 % F(000) = 1055.0 Mo-K(alpha) radiation Mu (mm-1) = 0.73 ------------------------------------------------------------------------------- File 2007src0194.ins set up as follows: TITL 2007src0194 in P2(1)/c CELL 0.71073 6.0475 27.1376 10.4986 90.000 96.177 90.000 ZERR 5.00 0.0004 0.0015 0.0007 0.000 0.003 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O F P CL UNIT 30 20 15 10 40 15 5 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------