++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 14:14:20 on 04-APR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 14.734 11.235 19.338 90.00 111.88 90.00 17980 Reflections read from file s92.hkl; mean (I/sigma) = 17.54 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8964 8973 9011 8965 13474 11980 12023 17980 N (int>3sigma) = 0 7653 7867 7882 7836 11701 10451 10503 15711 Mean intensity = 0.0 508.0 511.4 492.7 504.4 504.0 503.6 512.5 508.8 Mean int/sigma = 0.0 17.3 17.6 17.6 17.5 17.5 17.6 17.6 17.6 Lattice type: P chosen Volume: 2970.62 ------------------------------------------------------------------------------- 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: 11.235 14.734 19.338 111.88 90.00 90.00 Niggli form: a.a = 126.23 b.b = 217.09 c.c = 373.95 b.c = -106.17 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.514 deg. ORTHORHOMBIC C-lattice R(int) = 0.556 [ 14222] Cell: 14.734 35.891 11.235 90.00 90.00 89.49 Volume: 5941.23 Matrix: 1.0000 0.0000 0.0000 1.0000 0.0000 2.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.035 [ 10989] Cell: 14.734 11.235 19.338 90.00 111.88 90.00 Volume: 2970.62 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.514 deg. MONOCLINIC C-lattice R(int) = 0.524 [ 11162] Cell: 35.891 14.734 11.235 90.00 90.00 90.51 Volume: 5941.23 Matrix:-1.0000 0.0000 -2.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.514 deg. MONOCLINIC C-lattice R(int) = 0.546 [ 11563] Cell: 14.734 35.891 11.235 90.00 90.00 89.49 Volume: 5941.23 Matrix:-1.0000 0.0000 0.0000 -1.0000 0.0000 -2.0000 0.0000 -1.0000 0.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8964 8973 9011 8965 13474 11980 12023 17980 N (int>3sigma) = 0 7653 7867 7882 7836 11701 10451 10503 15711 Mean intensity = 0.0 508.0 511.4 492.7 504.4 504.0 503.6 512.5 508.8 Mean int/sigma = 0.0 17.3 17.6 17.6 17.5 17.5 17.6 17.6 17.6 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.910 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 7 547 524 537 N I>3s 0 285 32 289 1.5 427.2 2.1 435.3 0.5 11.8 1.0 12.1 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.035 10989 1.0 / 11.8 1.26 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C29H45F3NO2PPd Formula weight = 634.03 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.418, non-H atomic volume = 20.1 and following cell contents and analysis: C 116.00 54.93 % H 180.00 7.15 % N 4.00 2.21 % O 8.00 5.05 % F 12.00 8.99 % P 4.00 4.88 % Pd 4.00 16.78 % F(000) = 1320.0 Mo-K(alpha) radiation Mu (mm-1) = 0.72 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/c CELL 0.71073 14.7341 11.2352 19.3377 90.000 111.878 90.000 ZERR 4.00 0.0002 0.0002 0.0003 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O F P PD UNIT 116 180 4 8 12 4 4 TREF HKLF 4 END -------------------------------------------------------------------------------