++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src0400 started at 13:31:42 on 16-MAR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.652 11.363 16.018 90.00 102.01 90.00 21040 Reflections read from file 2007src0400.hkl; mean (I/sigma) = 15.87 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 10524 10528 10502 10538 15777 14031 14029 21040 N (int>3sigma) = 0 8601 8709 8668 8707 12989 11564 11544 17360 Mean intensity = 0.0 428.7 408.4 411.7 410.6 416.3 417.7 401.1 408.7 Mean int/sigma = 0.0 16.0 16.2 16.2 16.0 16.1 15.9 15.9 15.9 Lattice type: P chosen Volume: 1540.31 ------------------------------------------------------------------------------- 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: 8.652 11.363 16.018 90.00 102.01 90.00 Niggli form: a.a = 74.85 b.b = 129.12 c.c = 256.57 b.c = 0.00 a.c = -28.83 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.029 [ 17325] Cell: 8.652 11.363 16.018 90.00 102.01 90.00 Volume: 1540.31 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 10524 10528 10502 10538 15777 14031 14029 21040 N (int>3sigma) = 0 8601 8709 8668 8707 12989 11564 11544 17360 Mean intensity = 0.0 428.7 408.4 411.7 410.6 416.3 417.7 401.1 408.7 Mean int/sigma = 0.0 16.0 16.2 16.2 16.0 16.1 15.9 15.9 15.9 Crystal system M 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: -21- -a- -c- -n- N 20 511 501 524 N I>3s 0 241 17 240 1.6 287.6 2.0 280.5 0.8 10.0 0.8 9.8 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.029 17325 0.8 / 9.8 1.17 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12H26Cl8N8P6 Formula weight = 751.83 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.621, non-H atomic volume = 22.7 and following cell contents and analysis: C 24.00 19.17 % H 52.00 3.49 % N 16.00 14.91 % P 12.00 24.72 % Cl 16.00 37.72 % F(000) = 760.0 Mo-K(alpha) radiation Mu (mm-1) = 1.06 ------------------------------------------------------------------------------- File 2007src0400.ins set up as follows: TITL 2007src0400 in P2(1)/c CELL 0.71073 8.6518 11.3633 16.0178 90.000 102.006 90.000 ZERR 2.00 0.0001 0.0001 0.0002 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N P CL UNIT 24 52 16 12 16 TEMP 0.3 TREF HKLF 4 END -------------------------------------------------------------------------------