++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2005src1438 started at 15:09:46 on 28-NOV-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 12.154 19.343 20.260 90.00 104.43 90.00 57642 Reflections read from file 2005src1438.hkl; mean (I/sigma) = 7.70 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 28873 28841 28848 28824 43281 38476 38408 57642 N (int>3sigma) = 0 18145 18373 18270 18454 27394 24417 24571 36665 Mean intensity = 0.0 214.6 221.4 212.6 222.6 216.2 219.3 216.3 217.9 Mean int/sigma = 0.0 7.6 7.8 7.8 7.8 7.7 7.8 7.8 7.8 Lattice type: P chosen Volume: 4612.75 ------------------------------------------------------------------------------- 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: 12.154 19.343 20.260 90.00 104.43 90.00 Niggli form: a.a = 147.73 b.b = 374.16 c.c = 410.45 b.c = 0.00 a.c = -61.38 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.053 [ 46722] Cell: 12.154 19.343 20.260 90.00 104.43 90.00 Volume: 4612.75 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 28873 28841 28848 28824 43281 38476 38408 57642 N (int>3sigma) = 0 18145 18373 18270 18454 27394 24417 24571 36665 Mean intensity = 0.0 214.6 221.4 212.6 222.6 216.2 219.3 216.3 217.9 Mean int/sigma = 0.0 7.6 7.8 7.8 7.8 7.7 7.8 7.8 7.8 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.944 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 49 993 1004 991 N I>3s 6 396 23 415 12.6 332.9 3.7 334.5 1.4 6.2 0.7 6.3 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.053 46722 1.4 / 6.2 2.07 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C62H49N1O4B1F24Fe2In1 Formula weight = 1565.35 Tentative Z (number of formula units/cell) = 3.0 giving rho = 1.691, non-H atomic volume = 16.2 and following cell contents and analysis: C 186.00 47.57 % H 147.00 3.16 % B 3.00 0.69 % N 3.00 0.90 % O 12.00 4.09 % F 72.00 29.13 % Fe 6.00 7.14 % In 3.00 7.34 % F(000) = 2346.0 Mo-K(alpha) radiation Mu (mm-1) = 0.96 ------------------------------------------------------------------------------- File 2005src1438.ins set up as follows: TITL 2005src1438 in P2(1)/c CELL 0.71073 12.1544 19.3432 20.2595 90.000 104.435 90.000 ZERR 3.00 0.0003 0.0005 0.0003 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H B N O F FE IN UNIT 186 147 3 3 12 72 6 3 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------