++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src0546 started at 15:33:16 on 24-APR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.582 16.968 18.046 90.00 97.20 90.00 40743 Reflections read from file 2007src0546.hkl; mean (I/sigma) = 6.89 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 20401 20410 20409 20378 30610 27205 27175 40743 N (int>3sigma) = 0 11595 11435 11266 11569 17148 15372 15300 23017 Mean intensity = 0.0 104.3 101.4 110.7 101.6 105.5 105.9 105.3 105.0 Mean int/sigma = 0.0 7.0 6.9 6.9 7.0 6.9 7.0 7.0 7.0 Lattice type: P chosen Volume: 2911.01 ------------------------------------------------------------------------------- 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: 9.582 16.968 18.046 90.00 97.20 90.00 Niggli form: a.a = 91.82 b.b = 287.91 c.c = 325.65 b.c = 0.00 a.c = -21.67 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.056 [ 33842] Cell: 9.582 16.968 18.046 90.00 97.20 90.00 Volume: 2911.01 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 20401 20410 20409 20378 30610 27205 27175 40743 N (int>3sigma) = 0 11595 11435 11266 11569 17148 15372 15300 23017 Mean intensity = 0.0 104.3 101.4 110.7 101.6 105.5 105.9 105.3 105.0 Mean int/sigma = 0.0 7.0 6.9 6.9 7.0 6.9 7.0 7.0 7.0 Crystal system M and Lattice type P selected Mean |E*E-1| = 1.025 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 36 629 624 629 N I>3s 0 0 240 240 1.8 1.6 123.6 122.5 0.5 0.5 5.7 5.7 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 4 19410 0.056 33842 0.5 / 5.7 2.26 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C13H16NPF6 Formula weight = 331.24 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.512, non-H atomic volume = 17.3 and following cell contents and analysis: C 104.00 47.14 % H 128.00 4.87 % N 8.00 4.23 % F 48.00 34.42 % P 8.00 9.35 % F(000) = 1360.0 Mo-K(alpha) radiation Mu (mm-1) = 0.25 ------------------------------------------------------------------------------- File 1.ins set up as follows: TITL 1 in P2(1)/c CELL 0.71073 18.0459 16.9680 9.5823 90.000 97.198 90.000 ZERR 8.00 0.0005 0.0005 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 104 128 8 48 8 TEMP 0.04 TREF HKLF 4 END -------------------------------------------------------------------------------