++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 13:32:41 on 17-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.780 10.470 13.369 90.00 90.00 90.00 5397 Reflections read from file s92.hkl; mean (I/sigma) = 12.49 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2685 2700 2691 2695 4038 3608 3607 5397 N (int>3sigma) = 0 2329 2376 2339 2352 3522 3192 3195 4769 Mean intensity = 0.0 135.1 204.2 194.9 216.5 178.1 220.5 220.0 217.7 Mean int/sigma = 0.0 11.9 12.6 12.1 12.3 12.2 12.5 12.4 12.5 Lattice type: P chosen Volume: 1228.96 ------------------------------------------------------------------------------- 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: 8.780 10.470 13.369 90.00 90.00 90.00 Niggli form: a.a = 77.09 b.b = 109.63 c.c = 178.72 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) = 0.040 [ 3771] Cell: 8.780 10.470 13.369 90.00 90.00 90.00 Volume: 1228.96 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 2685 2700 2691 2695 4038 3608 3607 5397 N (int>3sigma) = 0 2329 2376 2339 2352 3522 3192 3195 4769 Mean intensity = 0.0 135.1 204.2 194.9 216.5 178.1 220.5 220.0 217.7 Mean int/sigma = 0.0 11.9 12.6 12.1 12.3 12.2 12.5 12.4 12.5 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.799 [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 211 213 208 3 169 181 180 5 92 89 81 14 N I>3s 183 172 169 0 1 90 91 0 51 51 2 0 362.1 395.8 229.3 0.7 0.9 337.3 339.3 0.5 192.5 198.9 1.0 0.8 12.6 12.3 11.6 0.8 0.6 9.0 9.0 0.3 9.8 10.1 0.6 0.6 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pna2(1) # 33 non-cen 4 903 0.040 3771 0.6 / 9.0 1.69 [B] Pnma # 62 centro 5 894 0.040 3771 0.6 / 9.0 4.14 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C3H6Cl4N3O2P3 Formula weight = 350.82 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.896, non-H atomic volume = 20.5 and following cell contents and analysis: C 12.00 10.27 % H 24.00 1.72 % N 12.00 11.98 % O 8.00 9.12 % P 12.00 26.48 % Cl 16.00 40.42 % F(000) = 696.0 Mo-K(alpha) radiation Mu (mm-1) = 1.34 ------------------------------------------------------------------------------- File 1.ins set up as follows: TITL 1 in Pna2(1) CELL 0.71073 13.3686 10.4704 8.7799 90.000 90.000 90.000 ZERR 4.00 0.0005 0.0004 0.0003 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 12 24 12 8 12 16 TREF HKLF 4 END -------------------------------------------------------------------------------