++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2006src0966 started at 10:26:28 on 09-AUG-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.479 10.228 11.414 88.42 78.17 79.69 16631 Reflections read from file 2006src0966.hkl; mean (I/sigma) = 16.94 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8313 8334 8323 8306 12485 11092 11072 16631 N (int>3sigma) = 0 6913 6968 6937 7029 10409 9257 9235 13901 Mean intensity = 0.0 352.1 362.4 366.9 337.5 360.5 358.5 353.9 355.6 Mean int/sigma = 0.0 16.9 16.8 17.0 17.1 16.9 16.9 17.1 17.0 Lattice type: P chosen Volume: 1065.66 ------------------------------------------------------------------------------- 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: 9.479 10.228 11.414 88.42 78.17 79.69 Niggli form: a.a = 89.85 b.b = 104.62 c.c = 130.29 b.c = 3.21 a.c = 22.18 a.b = 17.35 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.025 [ 12438] Cell: 9.479 10.228 11.414 88.42 78.17 79.69 Volume: 1065.66 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 8313 8334 8323 8306 12485 11092 11072 16631 N (int>3sigma) = 0 6913 6968 6937 7029 10409 9257 9235 13901 Mean intensity = 0.0 352.1 362.4 366.9 337.5 360.5 358.5 353.9 355.6 Mean int/sigma = 0.0 16.9 16.8 17.0 17.1 16.9 16.9 17.1 17.0 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.976 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P-1 # 2 centro 1 8646 0.025 12438 0.0 / 17.0 0.61 [B] P1 # 1 chiral 1 700 0.025 12438 0.0 / 17.0 6.47 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C4H4N5Cl4P3 Formula weight = 356.83 Tentative Z (number of formula units/cell) = 3.0 giving rho = 1.668, non-H atomic volume = 22.2 and following cell contents and analysis: C 12.00 13.46 % H 12.00 1.13 % N 15.00 19.63 % P 9.00 26.04 % Cl 12.00 39.74 % F(000) = 528.0 Mo-K(alpha) radiation Mu (mm-1) = 1.15 ------------------------------------------------------------------------------- File 2006src0966p-1.ins set up as follows: TITL 2006src0966p-1 in P-1 CELL 0.71073 9.4791 10.2283 11.4144 88.423 78.172 79.694 ZERR 3.00 0.0002 0.0002 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H N P CL UNIT 12 12 15 9 12 TEMP 0.14 TREF HKLF 4 END 16631 Reflections written to new reflection file 2006src0966p-1.hkl -------------------------------------------------------------------------------