++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2006src0700 started at 13:01:55 on 02-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 12.280 13.029 18.033 90.00 90.00 90.00 25767 Reflections read from file 2006src0700.hkl; mean (I/sigma) = 7.46 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 12872 12882 12834 12851 19294 17193 17176 25767 N (int>3sigma) = 0 7236 7768 7840 7849 11422 10471 10484 15664 Mean intensity = 0.0 108.7 153.5 156.5 157.8 139.6 161.4 160.9 159.0 Mean int/sigma = 0.0 6.6 7.7 7.7 7.7 7.3 7.6 7.6 7.6 Lattice type: P chosen Volume: 2885.11 ------------------------------------------------------------------------------- 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: 12.280 13.029 18.033 90.00 90.00 90.00 Niggli form: a.a = 150.79 b.b = 169.75 c.c = 325.19 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) = 0.059 [ 22041] Cell: 12.280 13.029 18.033 90.00 90.00 90.00 Volume: 2885.11 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 12872 12882 12834 12851 19294 17193 17176 25767 N (int>3sigma) = 0 7236 7768 7840 7849 11422 10471 10484 15664 Mean intensity = 0.0 108.7 153.5 156.5 157.8 139.6 161.4 160.9 159.0 Mean int/sigma = 0.0 6.6 7.7 7.7 7.7 7.3 7.6 7.6 7.6 Crystal system O and Lattice type P selected Mean |E*E-1| = 1.002 [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 748 766 740 15 612 619 607 24 460 463 453 32 N I>3s 299 3 298 0 209 1 208 1 183 4 183 0 258.3 2.6 260.9 3.2 199.9 2.5 201.6 1.5 148.5 3.3 150.5 1.6 5.8 0.5 5.8 0.5 5.4 0.5 5.5 0.5 6.0 0.7 6.1 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pbca # 61 centro 2 2293 0.059 22041 0.7 / 5.4 2.26 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C3H4BrCl4N4O4P3 Formula weight = 474.72 Tentative Z (number of formula units/cell) = 7.0 giving rho = 1.913, non-H atomic volume = 21.7 and following cell contents and analysis: C 21.00 7.59 % H 28.00 0.85 % N 28.00 11.80 % O 28.00 13.48 % P 21.00 19.57 % Cl 28.00 29.87 % Br 7.00 16.83 % F(000) = 1610.0 Mo-K(alpha) radiation Mu (mm-1) = 3.44 ------------------------------------------------------------------------------- File 1.ins set up as follows: TITL 1 in Pbca CELL 0.71073 13.0288 12.2797 18.0331 90.000 90.000 90.000 ZERR 7.00 0.0004 0.0004 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 O P CL BR UNIT 21 28 28 28 21 28 7 TEMP 0.1 TREF HKLF 4 END -------------------------------------------------------------------------------