++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src0354 started at 17:57:48 on 15-MAR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.387 10.626 18.580 90.00 98.72 90.00 20512 Reflections read from file 2007src0354.hkl; mean (I/sigma) = 9.36 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 10244 10248 10280 10250 15386 13682 13699 20512 N (int>3sigma) = 0 6856 6900 6072 6930 9914 9214 9244 13829 Mean intensity = 0.0 216.7 219.7 134.7 233.8 190.3 227.3 224.1 223.0 Mean int/sigma = 0.0 9.5 9.4 7.8 9.4 8.9 9.4 9.4 9.4 Lattice type: P chosen Volume: 1636.59 ------------------------------------------------------------------------------- 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: 8.387 10.626 18.580 90.00 98.72 90.00 Niggli form: a.a = 70.34 b.b = 112.91 c.c = 345.21 b.c = 0.00 a.c = -23.62 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.041 [ 16569] Cell: 8.387 10.626 18.580 90.00 98.72 90.00 Volume: 1636.59 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 10244 10248 10280 10250 15386 13682 13699 20512 N (int>3sigma) = 0 6856 6900 6072 6930 9914 9214 9244 13829 Mean intensity = 0.0 216.7 219.7 134.7 233.8 190.3 227.3 224.1 223.0 Mean int/sigma = 0.0 9.5 9.4 7.8 9.4 8.9 9.4 9.4 9.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 1.000 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 15 661 659 668 N I>3s 0 1 257 256 2.7 1.6 322.4 318.1 0.7 0.5 6.6 6.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 4 19410 0.041 16569 0.7 / 6.5 1.77 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C15H15NPF9 Formula weight = 411.25 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.669, non-H atomic volume = 15.7 and following cell contents and analysis: C 60.00 43.81 % H 60.00 3.68 % N 4.00 3.41 % F 36.00 41.58 % P 4.00 7.53 % F(000) = 832.0 Mo-K(alpha) radiation Mu (mm-1) = 0.26 ------------------------------------------------------------------------------- File 1.ins set up as follows: TITL 1 in P2(1)/c CELL 0.71073 18.5797 10.6257 8.3867 90.000 98.718 90.000 ZERR 4.00 0.0005 0.0003 0.0001 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N F P UNIT 60 60 4 36 4 TEMP 0.1 TREF HKLF 4 END -------------------------------------------------------------------------------