++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src0656 started at 20:06:22 on 14-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.459 16.854 19.061 90.00 90.00 90.00 61045 Reflections read from file 2007src0656.hkl; mean (I/sigma) = 6.80 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 30491 30490 30541 30521 45761 40705 40686 61045 N (int>3sigma) = 0 19964 19943 19549 20655 29728 27224 27206 40828 Mean intensity = 0.0 23.8 22.4 23.8 24.1 23.3 24.4 24.5 24.1 Mean int/sigma = 0.0 6.7 6.7 6.7 6.9 6.7 6.9 6.9 6.9 Lattice type: P chosen Volume: 3681.34 ------------------------------------------------------------------------------- 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: 11.459 16.854 19.061 90.00 90.00 90.00 Niggli form: a.a = 131.32 b.b = 284.05 c.c = 363.33 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) = 0.050 [ 56339] Cell: 11.459 16.854 19.061 90.00 90.00 90.00 Volume: 3681.34 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 30491 30490 30541 30521 45761 40705 40686 61045 N (int>3sigma) = 0 19964 19943 19549 20655 29728 27224 27206 40828 Mean intensity = 0.0 23.8 22.4 23.8 24.1 23.3 24.4 24.5 24.1 Mean int/sigma = 0.0 6.7 6.7 6.7 6.9 6.7 6.9 6.9 6.9 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.949 [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 1848 1838 1832 21 1041 1027 1034 47 897 899 914 53 N I>3s 4 700 698 0 7 401 402 0 20 362 360 0 0.3 30.7 30.8 0.2 0.3 31.2 31.0 0.2 0.4 24.9 24.5 0.2 0.6 4.5 4.5 0.6 0.6 4.9 4.8 0.6 0.8 5.3 5.2 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pbca # 61 centro 1 2293 0.050 56339 0.8 / 4.5 2.79 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C9H18Cl4N3O2P3 Formula weight = 434.97 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.570, non-H atomic volume = 21.9 and following cell contents and analysis: C 72.00 24.85 % H 144.00 4.17 % N 24.00 9.66 % O 16.00 7.36 % P 24.00 21.36 % Cl 32.00 32.60 % F(000) = 1776.0 Mo-K(alpha) radiation Mu (mm-1) = 0.91 ------------------------------------------------------------------------------- File 2007src0656.ins set up as follows: TITL 2007src0656 in Pbca CELL 0.71073 11.4593 16.8538 19.0612 90.000 90.000 90.000 ZERR 8.00 0.0002 0.0002 0.0002 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 O P CL UNIT 72 144 24 16 24 32 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------