++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src0399 started at 13:19:28 on 19-MAR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 14.636 16.350 12.345 90.00 107.46 90.00 24343 Reflections read from file 2007src0399.hkl; mean (I/sigma) = 8.35 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 12155 12155 0 12195 12155 16183 16234 24343 N (int>3sigma) = 0 10663 10663 0 10713 10663 14342 14415 21578 Mean intensity = 0.0 412.4 412.4 0.0 429.6 412.4 432.3 437.0 433.8 Mean int/sigma = 0.0 8.3 8.3 0.0 8.3 8.3 8.4 8.4 8.4 Lattice type: C chosen Volume: 2817.97 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 -0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 Unitcell: 10.972 10.972 12.345 101.54 101.54 96.33 Niggli form: a.a = 120.38 b.b = 120.38 c.c = 152.39 b.c = -27.10 a.c = -27.10 a.b = -13.28 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC C-lattice R(int) = 0.055 [ 20997] Cell: 14.636 16.350 12.345 90.00 107.46 90.00 Volume: 2817.97 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 12155 12155 0 12195 12155 16183 16234 24343 N (int>3sigma) = 0 10663 10663 0 10713 10663 14342 14415 21578 Mean intensity = 0.0 412.4 412.4 0.0 429.6 412.4 432.3 437.0 433.8 Mean int/sigma = 0.0 8.3 8.3 0.0 8.3 8.3 8.4 8.4 8.4 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.727 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 453 N I>3s 1 2.8 0.6 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.055 20997 0.6 / 8.4 7.12 [B] Cc # 9 non-cen 1 566 0.055 20997 0.6 / 8.4 1.46 Option [B] chosen ------------------------------------------------------------------------------- ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C12H12Cl8N8OP6 Formula weight = 753.72 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.777, non-H atomic volume = 20.1 and following cell contents and analysis: C 48.00 19.12 % H 48.00 1.60 % N 32.00 14.87 % O 4.00 2.12 % P 24.00 24.65 % Cl 32.00 37.63 % F(000) = 1496.0 Mo-K(alpha) radiation Mu (mm-1) = 1.17 ------------------------------------------------------------------------------- File 2007src0399.ins set up as follows: TITL 2007src0399 in Cc CELL 0.71073 14.6358 16.3497 12.3448 90.000 107.455 90.000 ZERR 4.00 0.0002 0.0002 0.0001 0.000 0.001 0.000 LATT -7 SYMM X, -Y, 0.5+Z SFAC C H N O P CL UNIT 48 48 32 4 24 32 TEMP 0.01 TREF HKLF 4 END -------------------------------------------------------------------------------