++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 16:58:06 on 29-JAN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.736 13.149 15.993 90.42 99.76 91.45 29685 Reflections read from file s92.hkl; mean (I/sigma) = 5.03 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 14844 14898 14848 14864 22295 19784 19761 29685 N (int>3sigma) = 0 7185 7399 7274 7292 10929 9793 9674 14555 Mean intensity = 0.0 17.5 19.4 19.0 19.0 18.6 19.1 19.1 18.9 Mean int/sigma = 0.0 5.0 5.2 5.1 5.1 5.1 5.2 5.1 5.1 Lattice type: P chosen Volume: 2017.00 ------------------------------------------------------------------------------- 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: 9.736 13.149 15.993 90.42 99.76 91.45 Niggli form: a.a = 94.80 b.b = 172.89 c.c = 255.77 b.c = -1.53 a.c = -26.40 a.b = -3.25 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.093 [ 20719] Cell: 9.736 13.149 15.993 90.42 99.76 91.45 Volume: 2017.00 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 14844 14898 14848 14864 22295 19784 19761 29685 N (int>3sigma) = 0 7185 7399 7274 7292 10929 9793 9674 14555 Mean intensity = 0.0 17.5 19.4 19.0 19.0 18.6 19.1 19.1 18.9 Mean int/sigma = 0.0 5.0 5.2 5.1 5.1 5.1 5.2 5.1 5.1 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.930 [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 0.093 20719 0.0 / 5.1 2.10 [B] P1 # 1 chiral 1 700 0.093 20719 0.0 / 5.1 5.86 Option [A] chosen ------------------------------------------------------------------------------- ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C20H18N2PSClPd Formula weight = 491.24 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.618, non-H atomic volume = 19.4 and following cell contents and analysis: C 80.00 48.90 % H 72.00 3.69 % N 8.00 5.70 % P 4.00 6.30 % S 4.00 6.53 % Cl 4.00 7.22 % Pd 4.00 21.66 % F(000) = 984.0 Mo-K(alpha) radiation Mu (mm-1) = 1.24 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P-1 CELL 0.71073 9.7364 13.1488 15.9927 90.416 99.760 91.453 ZERR 4.00 0.0019 0.0026 0.0032 0.030 0.030 0.030 LATT 1 SFAC C H N P S CL PD UNIT 80 72 8 4 4 4 4 TREF HKLF 4 END -------------------------------------------------------------------------------