++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04src0339 started at 09:33:26 on 27-APR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 14.605 12.024 14.879 89.99 111.40 90.01 29686 Reflections read from file 04src0339.hkl; mean (I/sigma) = 14.48 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 14794 14860 14852 14807 22253 19851 19751 29686 N (int>3sigma) = 0 12333 12442 12261 12365 18518 16523 16414 24719 Mean intensity = 0.0 516.7 520.4 496.7 515.4 511.3 516.2 523.6 516.3 Mean int/sigma = 0.0 14.5 14.5 14.2 14.5 14.4 14.5 14.5 14.5 Lattice type: P chosen Volume: 2432.68 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 12.024 14.605 14.879 68.60 89.99 89.99 Niggli form: a.a = 144.56 b.b = 213.30 c.c = 221.39 b.c = 79.29 a.c = 0.02 a.b = 0.03 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.010 deg. MONOCLINIC P-lattice R(int) = 0.031 [ 23817] Cell: 14.605 12.024 14.879 89.99 111.40 90.01 Volume: 2432.68 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 14794 14860 14852 14807 22253 19851 19751 29686 N (int>3sigma) = 0 12333 12442 12261 12365 18518 16523 16414 24719 Mean intensity = 0.0 516.7 520.4 496.7 515.4 511.3 516.2 523.6 516.3 Mean int/sigma = 0.0 14.5 14.5 14.2 14.5 14.4 14.5 14.5 14.5 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.903 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 31 739 714 717 N I>3s 0 3 325 324 1.0 1.8 738.7 735.5 0.5 0.5 10.0 9.9 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 4 19410 0.031 23817 0.5 / 9.9 1.49 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C24H22N1O4F7Pt1 Formula weight = 716.52 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.956, non-H atomic volume = 16.4 and following cell contents and analysis: C 96.00 40.23 % H 88.00 3.09 % N 4.00 1.96 % O 16.00 8.93 % F 28.00 18.56 % Pt 4.00 27.23 % F(000) = 1384.0 Mo-K(alpha) radiation Mu (mm-1) = 5.85 ------------------------------------------------------------------------------- File s93.ins set up as follows: TITL s93 in P2(1)/c CELL 0.71073 14.8792 12.0235 14.6049 90.000 111.400 90.000 ZERR 4.00 0.0010 0.0006 0.0008 0.000 0.005 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O F PT UNIT 96 88 4 16 28 4 TEMP 0.03 TREF HKLF 4 END 29686 Reflections written to new reflection file s93.hkl -------------------------------------------------------------------------------