++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 14:57:18 on 19-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.689 13.406 13.689 93.63 93.59 113.06 13192 Reflections read from file s92.hkl; mean (I/sigma) = 5.14 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6595 6611 6580 6606 9893 8787 8793 13192 N (int>3sigma) = 0 3553 3567 3580 3534 5350 4753 4711 7074 Mean intensity = 0.0 22.2 21.7 22.3 22.2 22.1 21.5 22.2 21.9 Mean int/sigma = 0.0 5.2 5.2 5.3 5.2 5.3 5.2 5.2 5.2 Lattice type: P chosen Volume: 1793.08 ------------------------------------------------------------------------------- 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: 10.689 13.406 13.689 93.63 93.59 113.06 Niggli form: a.a = 114.27 b.b = 179.72 c.c = 187.38 b.c = -11.61 a.c = -9.16 a.b = -56.13 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.061 [ 6543] Cell: 10.689 13.406 13.689 93.63 93.59 113.06 Volume: 1793.08 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 6595 6611 6580 6606 9893 8787 8793 13192 N (int>3sigma) = 0 3553 3567 3580 3534 5350 4753 4711 7074 Mean intensity = 0.0 22.2 21.7 22.3 22.2 22.1 21.5 22.2 21.9 Mean int/sigma = 0.0 5.2 5.2 5.3 5.2 5.3 5.2 5.2 5.2 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.972 [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 0.061 6543 0.0 / 5.2 1.93 [B] P1 # 1 chiral 1 700 0.061 6543 0.0 / 5.2 7.63 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C19 H5 B1 F10 Fe1 O2 Formula weight = 521.89 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.933, non-H atomic volume = 13.6 and following cell contents and analysis: C 76.00 43.72 % H 20.00 0.97 % B 4.00 2.07 % O 8.00 6.13 % F 40.00 36.41 % Fe 4.00 10.70 % F(000) = 1024.0 Mo-K(alpha) radiation Mu (mm-1) = 0.96 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P-1 CELL 0.71073 10.6895 13.4060 13.6885 93.628 93.588 113.060 ZERR 4.00 0.0021 0.0027 0.0027 0.030 0.030 0.030 LATT 1 SFAC C H B O F FE UNIT 76 20 4 8 40 4 TREF HKLF 4 END -------------------------------------------------------------------------------