++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 15:21:08 on 17-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.592 12.189 31.323 90.00 90.00 90.00 16759 Reflections read from file s92.hkl; mean (I/sigma) = 11.67 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8334 8341 8383 8373 12529 11181 11192 16759 N (int>3sigma) = 0 5898 5703 5847 5968 8724 7931 7908 11875 Mean intensity = 0.0 212.9 215.3 211.1 211.3 213.1 213.1 212.6 210.1 Mean int/sigma = 0.0 11.8 11.4 11.7 11.8 11.6 11.7 11.7 11.7 Lattice type: P chosen Volume: 3662.15 ------------------------------------------------------------------------------- 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: 9.592 12.189 31.323 90.00 90.00 90.00 Niggli form: a.a = 92.01 b.b = 148.56 c.c = 981.11 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(int) = 0.044 [ 12169] Cell: 9.592 12.189 31.323 90.00 90.00 90.00 Volume: 3662.15 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 8334 8341 8383 8373 12529 11181 11192 16759 N (int>3sigma) = 0 5898 5703 5847 5968 8724 7931 7908 11875 Mean intensity = 0.0 212.9 215.3 211.1 211.3 213.1 213.1 212.6 210.1 Mean int/sigma = 0.0 11.8 11.4 11.7 11.8 11.6 11.7 11.7 11.7 Crystal system O and Lattice type P selected Mean |E*E-1| = 1.050 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 608 560 590 6 367 340 363 14 216 188 216 9 N I>3s 254 16 264 0 173 8 169 0 114 5 111 0 307.9 2.1 317.3 1.6 281.7 2.0 284.6 1.6 298.3 2.2 298.1 3.6 8.8 0.9 9.1 0.6 8.8 0.8 8.8 0.9 10.5 1.0 10.4 1.2 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pbca # 61 centro 2 2293 0.044 12169 1.2 / 8.8 1.99 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C17 H27 N2 Fe1 I1 Formula weight = 442.16 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.604, non-H atomic volume = 21.8 and following cell contents and analysis: C 136.00 46.18 % H 216.00 6.16 % N 16.00 6.34 % Fe 8.00 12.63 % I 8.00 28.70 % F(000) = 1776.0 Mo-K(alpha) radiation Mu (mm-1) = 2.51 ------------------------------------------------------------------------------- File s93.ins set up as follows: TITL S93 in Pbca CELL 0.71073 12.1886 9.5923 31.3227 90.000 90.000 90.000 ZERR 8.00 0.0002 0.0001 0.0005 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N FE I UNIT 136 216 16 8 8 TREF HKLF 4 END 16759 Reflections written to new reflection file s93.hkl -------------------------------------------------------------------------------