++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src1029 started at 17:29:11 on 02-AUG-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.916 9.901 20.661 90.15 99.45 89.98 26743 Reflections read from file 2007src1029.hkl; mean (I/sigma) = 1.87 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 13370 13371 13325 13315 20033 17877 17844 26743 N (int>3sigma) = 0 3322 3363 3265 3326 4975 4460 4543 6740 Mean intensity = 0.0 5.9 6.9 7.5 5.0 6.8 6.6 6.9 6.6 Mean int/sigma = 0.0 2.1 2.1 2.1 2.1 2.1 2.1 2.1 2.1 Lattice type: P chosen Volume: 1597.30 ------------------------------------------------------------------------------- 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: 7.916 9.901 20.661 89.85 80.55 89.98 Niggli form: a.a = 62.66 b.b = 98.02 c.c = 426.89 b.c = 0.55 a.c = 26.84 a.b = 0.02 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.155 deg. MONOCLINIC P-lattice R(int) = 0.228 [ 22808] Cell: 7.916 9.901 20.661 90.15 99.45 89.98 Volume: 1597.30 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.192 [ 19613] Cell: 7.916 9.901 20.661 89.85 80.55 89.98 Volume: 1597.30 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 13370 13371 13325 13315 20033 17877 17844 26743 N (int>3sigma) = 0 3322 3363 3265 3326 4975 4460 4543 6740 Mean intensity = 0.0 5.9 6.9 7.5 5.0 6.8 6.6 6.9 6.6 Mean int/sigma = 0.0 2.1 2.1 2.1 2.1 2.1 2.1 2.1 2.1 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.883 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 22 930 933 951 N I>3s 2 186 168 42 0.8 10.3 10.0 1.0 1.0 1.8 1.7 0.8 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM No acceptable space group - change tolerances or unset chiral flag or possibly change input lattice type, then recheck cell using H-option ------------------------------------------------------------------------------- Input space group symbol: P2(1)/n Number: 14 centrosymmetric CSD frequency: 19410 R(int) = 0.228 22808 reflections merged Systematic absence exceptions: -21- -a- -c- -n- N 22 930 933 951 N I>3s 2 186 168 42 0.8 10.3 10.0 1.0 1.0 1.8 1.7 0.8 ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C14H15F6N2O2P Formula weight = 388.25 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.614, non-H atomic volume = 16.0 and following cell contents and analysis: C 56.00 43.31 % H 60.00 3.89 % N 8.00 7.22 % O 8.00 8.24 % F 24.00 29.36 % P 4.00 7.98 % F(000) = 792.0 Mo-K(alpha) radiation Mu (mm-1) = 0.25 ------------------------------------------------------------------------------- File 2007src1029.ins set up as follows: TITL 2007src1029 in P2(1)/n CELL 0.71073 7.9157 9.9007 20.6614 90.000 99.445 90.000 ZERR 4.00 0.0017 0.0022 0.0044 0.000 0.012 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O F P UNIT 56 60 8 8 24 4 TEMP 0.04 TREF HKLF 4 END -------------------------------------------------------------------------------