++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 13:49:54 on 23-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 12.560 9.108 14.227 90.00 102.86 90.00 12469 Reflections read from file s92.hkl; mean (I/sigma) = 3.72 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6232 6191 6239 6212 9331 8316 8327 12469 N (int>3sigma) = 0 2325 2205 2360 2218 3445 3124 3116 4651 Mean intensity = 0.0 16.1 12.3 16.3 13.5 14.9 16.2 16.2 15.7 Mean int/sigma = 0.0 3.9 3.6 3.9 3.7 3.8 3.9 3.9 3.9 Lattice type: P chosen Volume: 1586.82 ------------------------------------------------------------------------------- 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: 9.108 12.560 14.227 102.86 90.00 90.00 Niggli form: a.a = 82.96 b.b = 157.75 c.c = 202.42 b.c = -39.77 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.123 [ 8695] Cell: 12.560 9.108 14.227 90.00 102.86 90.00 Volume: 1586.82 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.092 [ 5674] Cell: 9.108 12.560 14.227 77.14 90.00 90.00 Volume: 1586.82 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 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 6232 6191 6239 6212 9331 8316 8327 12469 N (int>3sigma) = 0 2325 2205 2360 2218 3445 3124 3116 4651 Mean intensity = 0.0 16.1 12.3 16.3 13.5 14.9 16.2 16.2 15.7 Mean int/sigma = 0.0 3.9 3.6 3.9 3.7 3.8 3.9 3.9 3.9 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.923 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 8 397 397 358 N I>3s 0 128 128 0 1.2 34.9 34.9 1.0 0.5 4.2 4.2 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.123 8695 0.5 / 3.9 3.17 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C16H34Cl4N10O4P6 Formula weight = 758.15 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.587, non-H atomic volume = 19.8 and following cell contents and analysis: C 32.00 25.35 % H 68.00 4.52 % N 20.00 18.48 % O 8.00 8.44 % P 12.00 24.51 % Cl 8.00 18.70 % F(000) = 780.0 Mo-K(alpha) radiation Mu (mm-1) = 0.72 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/n CELL 0.71073 12.5600 9.1084 14.2275 90.000 102.860 90.000 ZERR 2.00 0.0008 0.0008 0.0011 0.000 0.005 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O P CL UNIT 32 68 20 8 12 8 TREF HKLF 4 END -------------------------------------------------------------------------------