++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2005src1061 started at 11:32:16 on 06-SEP-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.710 9.970 12.025 106.09 90.92 90.82 18318 Reflections read from file 2005src1061.hkl; mean (I/sigma) = 13.24 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 9144 9155 9163 9115 13731 12204 12190 18318 N (int>3sigma) = 0 8001 7981 7932 7872 11957 10607 10541 15906 Mean intensity = 0.0 638.0 644.3 613.0 650.2 631.8 641.1 623.2 641.7 Mean int/sigma = 0.0 13.2 13.4 13.3 13.2 13.3 13.3 13.2 13.3 Lattice type: P chosen Volume: 772.74 ------------------------------------------------------------------------------- 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: 6.710 9.970 12.025 106.09 90.92 90.82 Niggli form: a.a = 45.03 b.b = 99.41 c.c = 144.59 b.c = -33.23 a.c = -1.29 a.b = -0.96 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.035 [ 14775] Cell: 6.710 9.970 12.025 106.09 90.92 90.82 Volume: 772.74 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 9144 9155 9163 9115 13731 12204 12190 18318 N (int>3sigma) = 0 8001 7981 7932 7872 11957 10607 10541 15906 Mean intensity = 0.0 638.0 644.3 613.0 650.2 631.8 641.1 623.2 641.7 Mean int/sigma = 0.0 13.2 13.4 13.3 13.2 13.3 13.3 13.2 13.3 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.917 [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 0.035 14775 0.0 / 13.3 1.02 [B] P1 # 1 chiral 1 700 0.035 14775 0.0 / 13.3 4.18 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C28H20Br2Fe4In2O8 Formula weight = 1097.30 Tentative Z (number of formula units/cell) = 1.0 giving rho = 2.358, non-H atomic volume = 17.6 and following cell contents and analysis: C 28.00 30.65 % H 20.00 1.84 % O 8.00 11.66 % Fe 4.00 20.36 % Br 2.00 14.56 % In 2.00 20.93 % F(000) = 524.0 Mo-K(alpha) radiation Mu (mm-1) = 5.93 ------------------------------------------------------------------------------- File 2005src1061.ins set up as follows: TITL 2005src1061 in P-1 CELL 0.71073 6.7104 9.9705 12.0246 106.093 90.916 90.823 ZERR 1.00 0.0001 0.0003 0.0004 0.001 0.002 0.002 LATT 1 SFAC C H O FE BR IN UNIT 28 20 8 4 2 2 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------