++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2005src0648 started at 15:48:18 on 17-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.975 11.539 12.427 90.01 90.01 90.02 14711 Reflections read from file 2005src0648.hkl; mean (I/sigma) = 16.46 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7369 7365 7374 7359 11054 9804 9797 14711 N (int>3sigma) = 0 6032 5724 5910 5683 8833 8015 7991 12010 Mean intensity = 0.0 401.6 288.1 379.6 302.7 356.4 384.5 388.9 395.4 Mean int/sigma = 0.0 16.6 15.1 16.1 15.5 15.9 16.4 16.5 16.5 Lattice type: P chosen Volume: 1430.35 ------------------------------------------------------------------------------- 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: 9.975 11.539 12.427 90.01 90.01 90.02 Niggli form: a.a = 99.50 b.b = 133.15 c.c = 154.43 b.c = -0.01 a.c = -0.02 a.b = -0.03 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.019 deg. ORTHORHOMBIC P-lattice R(int) = 0.027 [ 12820] Cell: 9.975 11.539 12.427 90.01 90.01 90.02 Volume: 1430.35 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 7369 7365 7374 7359 11054 9804 9797 14711 N (int>3sigma) = 0 6032 5724 5910 5683 8833 8015 7991 12010 Mean intensity = 0.0 401.6 288.1 379.6 302.7 356.4 384.5 388.9 395.4 Mean int/sigma = 0.0 16.6 15.1 16.1 15.5 15.9 16.4 16.5 16.5 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.946 [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 424 426 432 14 387 388 387 13 375 378 387 19 N I>3s 363 373 336 2 172 174 2 0 187 182 9 0 662.7 536.4 468.3 4.9 624.5 623.0 1.6 0.8 584.8 580.1 1.5 1.4 20.3 21.1 17.9 1.3 11.0 11.0 0.6 0.6 12.4 12.3 0.7 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pnnm # 58 centro 3 61 0.027 12820 1.3 / 11.0 2.63 [B] Pnn2 # 34 non-cen 3 21 0.027 12820 1.3 / 11.0 9.94 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C5H10Cl4N3O2P3 Formula weight = 378.87 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.759, non-H atomic volume = 21.0 and following cell contents and analysis: C 20.00 15.85 % H 40.00 2.66 % N 12.00 11.09 % O 8.00 8.45 % P 12.00 24.52 % Cl 16.00 37.43 % F(000) = 760.0 Mo-K(alpha) radiation Mu (mm-1) = 1.15 ------------------------------------------------------------------------------- File 1.ins set up as follows: TITL 1 in Pnnm CELL 0.71073 11.5390 12.4271 9.9748 90.000 90.000 90.000 ZERR 4.00 0.0009 0.0008 0.0005 0.000 0.000 0.000 LATT 1 SYMM -X, -Y, Z SYMM 0.5-X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, 0.5-Z SFAC C H N O P CL UNIT 20 40 12 8 12 16 TEMP 0.13 TREF HKLF 4 END -------------------------------------------------------------------------------