++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 16:10:15 on 03-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.257 11.471 12.937 100.82 94.20 105.23 12763 Reflections read from file s92.hkl; mean (I/sigma) = 5.77 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6399 6387 6388 6388 9587 8513 8532 12763 N (int>3sigma) = 0 4134 4079 4159 4178 6186 5445 5572 8236 Mean intensity = 0.0 18.8 18.6 18.8 18.0 18.7 18.9 18.7 18.7 Mean int/sigma = 0.0 5.8 5.8 5.8 5.8 5.8 5.8 5.9 5.8 Lattice type: P chosen Volume: 872.56 ------------------------------------------------------------------------------- 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: 6.257 11.471 12.937 100.82 94.20 105.23 Niggli form: a.a = 39.15 b.b = 131.58 c.c = 167.37 b.c = -27.87 a.c = -5.93 a.b = -18.85 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.078 [ 8894] Cell: 6.257 11.471 12.937 100.82 94.20 105.23 Volume: 872.56 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 6399 6387 6388 6388 9587 8513 8532 12763 N (int>3sigma) = 0 4134 4079 4159 4178 6186 5445 5572 8236 Mean intensity = 0.0 18.8 18.6 18.8 18.0 18.7 18.9 18.7 18.7 Mean int/sigma = 0.0 5.8 5.8 5.8 5.8 5.8 5.8 5.9 5.8 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.798 [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 0.078 8894 0.0 / 5.8 4.62 [B] P1 # 1 chiral 1 700 0.078 8894 0.0 / 5.8 2.25 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C30 H26 N2 S4 Cl2 Pd1 Formula weight = 720.07 Tentative Z (number of formula units/cell) = 1.0 giving rho = 1.370, non-H atomic volume = 22.4 and following cell contents and analysis: C 30.00 50.04 % H 26.00 3.64 % N 2.00 3.89 % S 4.00 17.81 % Cl 2.00 9.85 % Pd 1.00 14.78 % F(000) = 364.0 Mo-K(alpha) radiation Mu (mm-1) = 0.94 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P-1 CELL 0.71073 6.2568 11.4708 12.9370 100.823 94.201 105.230 ZERR 1.00 0.0003 0.0005 0.0009 0.002 0.002 0.002 LATT 1 SFAC C H N S CL PD UNIT 30 26 2 4 2 1 TREF HKLF 4 END -------------------------------------------------------------------------------