++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + S92 started at 09:55:54 on 02-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.536 15.036 17.367 89.99 80.22 89.97 39037 Reflections read from file s92.hkl; mean (I/sigma) = 7.06 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 19549 19377 19570 19346 29248 26006 25990 39037 N (int>3sigma) = 0 13537 13050 13577 13068 20082 18013 17881 26980 Mean intensity = 0.0 41.6 41.4 40.5 41.3 41.2 41.7 41.1 41.4 Mean int/sigma = 0.0 7.1 6.9 7.1 6.9 7.1 7.1 7.1 7.1 Lattice type: P chosen Volume: 2711.38 ------------------------------------------------------------------------------- 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: 10.536 15.036 17.367 89.99 80.22 89.97 Niggli form: a.a = 111.01 b.b = 226.08 c.c = 301.61 b.c = 0.04 a.c = 31.07 a.b = 0.08 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.030 deg. MONOCLINIC P-lattice R(int) = 0.094 [ 32666] Cell: 10.536 15.036 17.367 89.99 99.78 90.03 Volume: 2711.38 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 19549 19377 19570 19346 29248 25997 26033 39037 N (int>3sigma) = 0 13537 13050 13577 13068 20082 17829 18031 26980 Mean intensity = 0.0 41.6 41.4 40.5 41.3 41.2 41.3 41.6 41.4 Mean int/sigma = 0.0 7.1 6.9 7.1 6.9 7.1 7.1 7.1 7.1 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.954 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 19 718 726 584 N I>3s 0 360 359 1 0.5 81.0 80.1 0.7 0.4 6.0 5.9 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.094 32666 0.5 / 5.9 1.85 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C27H45INPPd Formula weight = 647.91 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.587, non-H atomic volume = 21.9 and following cell contents and analysis: C 108.00 50.05 % H 180.00 7.00 % N 4.00 2.16 % P 4.00 4.78 % Pd 4.00 16.42 % I 4.00 19.59 % F(000) = 1312.0 Mo-K(alpha) radiation Mu (mm-1) = 1.90 ------------------------------------------------------------------------------- File 1.ins set up as follows: TITL 1 in P2(1)/n CELL 0.71073 10.5363 15.0361 17.3668 90.000 99.776 90.000 ZERR 4.00 0.0002 0.0003 0.0003 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N P PD I UNIT 108 180 4 4 4 4 TREF HKLF 4 END -------------------------------------------------------------------------------