++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src0657 started at 17:31:53 on 15-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 10.632 12.087 15.626 90.00 101.58 90.00 25924 Reflections read from file 2007src0657.hkl; mean (I/sigma) = 10.49 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 12966 12953 12953 12943 19436 17286 17293 25924 N (int>3sigma) = 0 9657 9676 9863 9824 14598 13121 13206 19703 Mean intensity = 0.0 29.9 30.1 30.6 30.1 30.2 29.9 30.1 30.0 Mean int/sigma = 0.0 10.3 10.5 10.5 10.5 10.4 10.5 10.6 10.5 Lattice type: P chosen Volume: 1967.03 ------------------------------------------------------------------------------- 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: 10.632 12.087 15.626 90.00 101.58 90.00 Niggli form: a.a = 113.03 b.b = 146.09 c.c = 244.16 b.c = 0.00 a.c = -33.36 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.040 [ 21193] Cell: 10.632 12.087 15.626 90.00 101.58 90.00 Volume: 1967.03 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 12966 12953 12953 12943 19436 17286 17293 25924 N (int>3sigma) = 0 9657 9676 9863 9824 14598 13121 13206 19703 Mean intensity = 0.0 29.9 30.1 30.6 30.1 30.2 29.9 30.1 30.0 Mean int/sigma = 0.0 10.3 10.5 10.5 10.5 10.4 10.5 10.6 10.5 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.972 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 23 662 661 659 N I>3s 0 279 2 279 0.2 40.0 0.2 40.2 0.6 7.0 0.5 7.0 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.040 21193 0.6 / 7.0 1.53 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C11H22Cl4N3O2P3 Formula weight = 463.03 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.564, non-H atomic volume = 21.4 and following cell contents and analysis: C 44.00 28.53 % H 88.00 4.79 % N 12.00 9.08 % O 8.00 6.91 % P 12.00 20.07 % Cl 16.00 30.62 % F(000) = 952.0 Mo-K(alpha) radiation Mu (mm-1) = 0.86 ------------------------------------------------------------------------------- File 2007src0657.ins set up as follows: TITL 2007src0657 in P2(1)/c CELL 0.71073 10.6315 12.0869 15.6257 90.000 101.585 90.000 ZERR 4.00 0.0002 0.0002 0.0003 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O P CL UNIT 44 88 12 8 12 16 TEMP 0.15 TREF HKLF 4 END -------------------------------------------------------------------------------