++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2006src0699 started at 11:04:56 on 05-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.601 23.212 9.168 90.00 90.01 90.00 16235 Reflections read from file 2006src0699.hkl; mean (I/sigma) = 9.11 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8125 8102 8109 8108 12168 10821 10826 16235 N (int>3sigma) = 0 6281 6243 6384 6324 9454 8485 8487 12730 Mean intensity = 0.0 20.2 18.9 20.6 19.1 19.9 20.0 19.9 20.0 Mean int/sigma = 0.0 9.0 9.0 9.1 9.1 9.0 9.2 9.2 9.1 Lattice type: P chosen Volume: 1617.57 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 7.601 9.168 23.212 90.00 90.00 90.01 Niggli form: a.a = 57.77 b.b = 84.06 c.c = 538.82 b.c = 0.00 a.c = 0.00 a.b = -0.01 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.010 deg. ORTHORHOMBIC P-lattice R(int) = 0.048 [ 13915] Cell: 7.601 9.168 23.212 90.00 90.00 90.01 Volume: 1617.57 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8125 8109 8102 8108 12168 10821 10821 16235 N (int>3sigma) = 0 6281 6384 6243 6324 9454 8488 8485 12730 Mean intensity = 0.0 20.2 20.6 18.9 19.1 19.9 20.4 20.0 20.0 Mean int/sigma = 0.0 9.0 9.1 9.0 9.1 9.0 9.2 9.2 9.1 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.847 [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 727 731 728 11 574 566 564 11 207 202 203 45 N I>3s 557 495 556 5 4 255 257 2 104 101 7 2 21.7 7.7 22.9 1.5 0.3 35.3 35.4 0.8 44.3 45.3 0.3 0.4 9.4 7.5 9.5 2.0 0.6 6.6 6.7 1.3 7.3 7.4 0.7 1.1 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pna2(1) # 33 non-cen 4 903 0.048 13915 2.0 / 6.6 3.01 [B] Pnma # 62 centro 5 894 0.048 13915 2.0 / 6.6 3.25 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C9H10Cl4N3O2P3 Formula weight = 426.91 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.753, non-H atomic volume = 19.3 and following cell contents and analysis: C 36.00 25.32 % H 40.00 2.36 % N 12.00 9.85 % O 8.00 7.50 % P 12.00 21.76 % Cl 16.00 33.22 % F(000) = 856.0 Mo-K(alpha) radiation Mu (mm-1) = 1.03 ------------------------------------------------------------------------------- File 1.ins set up as follows: TITL 1 in Pna2(1) CELL 0.71073 23.2125 9.1684 7.6006 90.000 90.000 90.000 ZERR 4.00 0.0007 0.0002 0.0002 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, 0.5-Y, Z SYMM 0.5-X, 0.5+Y, 0.5+Z SFAC C H N O P CL UNIT 36 40 12 8 12 16 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------