++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2005src0670 started at 16:47:35 on 27-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.771 14.739 23.365 90.02 90.02 90.02 27400 Reflections read from file 2005src0670.hkl; mean (I/sigma) = 8.62 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 13717 13689 13740 13700 20573 18268 18265 27400 N (int>3sigma) = 0 8947 8667 7970 8789 12792 11898 11860 17826 Mean intensity = 0.0 162.2 159.0 123.9 164.5 148.3 171.9 168.9 174.3 Mean int/sigma = 0.0 8.7 8.5 7.5 8.6 8.2 8.7 8.6 8.7 Lattice type: P chosen Volume: 3709.37 ------------------------------------------------------------------------------- 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: 10.771 14.739 23.365 90.02 90.02 90.02 Niggli form: a.a = 116.02 b.b = 217.23 c.c = 545.94 b.c = -0.10 a.c = -0.07 a.b = -0.06 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.029 deg. ORTHORHOMBIC P-lattice R(int) = 0.053 [ 22660] Cell: 10.771 14.739 23.365 90.02 90.02 90.02 Volume: 3709.37 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 13717 13689 13740 13700 20573 18268 18265 27400 N (int>3sigma) = 0 8947 8667 7970 8789 12792 11898 11860 17826 Mean intensity = 0.0 162.2 159.0 123.9 164.5 148.3 171.9 168.9 174.3 Mean int/sigma = 0.0 8.7 8.5 7.5 8.6 8.2 8.7 8.6 8.7 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.892 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P-1 # 2 centro 1 8646 0.042 13323 0.0 / 8.7 1.73 [B] P1 # 1 chiral 1 700 0.042 13323 0.0 / 8.7 3.74 Option [B] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C21H12N1F6Fe1 Formula weight = 448.17 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.605, non-H atomic volume = 16.0 and following cell contents and analysis: C 168.00 56.28 % H 96.00 2.70 % N 8.00 3.13 % F 48.00 25.44 % Fe 8.00 12.46 % F(000) = 1800.0 Mo-K(alpha) radiation Mu (mm-1) = 0.88 ------------------------------------------------------------------------------- File 2005src0670.ins set up as follows: TITL 2005src0670 in P1 CELL 0.71073 10.7713 14.7387 23.3654 90.017 90.017 90.023 ZERR 8.00 0.0009 0.0012 0.0023 0.008 0.007 0.008 LATT -1 SFAC C H N F FE UNIT 168 96 8 48 8 TEMP 0.05 TREF HKLF 4 END ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C21 H16 N1 F6 Fe1 Br1 Formula weight = 532.11 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.906, non-H atomic volume = 15.5 and following cell contents and analysis: C 168.00 47.40 % H 128.00 3.03 % N 8.00 2.63 % F 48.00 21.42 % Fe 8.00 10.50 % Br 8.00 15.02 % F(000) = 2112.0 Mo-K(alpha) radiation Mu (mm-1) = 3.03 ------------------------------------------------------------------------------- File 2005src0670.ins set up as follows: TITL 2005src0670 in P1 CELL 0.71073 10.7713 14.7387 23.3654 90.017 90.017 90.023 ZERR 8.00 0.0009 0.0012 0.0023 0.008 0.007 0.008 LATT -1 SFAC C H N F FE BR UNIT 168 128 8 48 8 8 TEMP 0.05 TREF HKLF 4 END -------------------------------------------------------------------------------