++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src0607 started at 22:43:21 on 14-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.756 15.619 18.446 90.00 90.00 90.00 44953 Reflections read from file 2007src0607.hkl; mean (I/sigma) = 4.37 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 22449 22501 22470 22491 33710 29976 29958 44953 N (int>3sigma) = 0 9613 9656 9479 9523 14374 12756 12671 19055 Mean intensity = 0.0 93.0 99.5 100.8 97.8 97.8 101.0 99.3 99.8 Mean int/sigma = 0.0 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 Lattice type: P chosen Volume: 3387.05 ------------------------------------------------------------------------------- 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: 11.756 15.619 18.446 90.00 90.00 90.00 Niggli form: a.a = 138.20 b.b = 243.95 c.c = 340.27 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(int) = 0.092 [ 40775] Cell: 11.756 15.619 18.446 90.00 90.00 90.00 Volume: 3387.05 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 22449 22501 22470 22491 33710 29976 29958 44953 N (int>3sigma) = 0 9613 9656 9479 9523 14374 12756 12671 19055 Mean intensity = 0.0 93.0 99.5 100.8 97.8 97.8 101.0 99.3 99.8 Mean int/sigma = 0.0 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.789 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 1104 1101 1093 20 734 730 740 26 825 809 816 29 N I>3s 463 570 527 0 270 364 314 0 260 312 274 0 55.4 156.6 146.0 2.7 32.6 157.4 152.4 1.9 33.5 137.4 128.6 2.8 4.7 6.1 5.6 0.6 3.6 5.2 4.8 0.4 3.2 4.6 4.2 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)2(1)2(1) # 19 chiral 1 5917 0.092 40775 0.6 / 3.2 3.54 Option [A] chosen ------------------------------------------------------------------------------- Input space group symbol: Pbca Number: 61 centrosymmetric CSD frequency: 2293 R(int) = 0.092 40775 reflections merged Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 1104 1101 1093 20 734 730 740 26 825 809 816 29 N I>3s 463 570 527 0 270 364 314 0 260 312 274 0 55.4 156.6 146.0 2.7 32.6 157.4 152.4 1.9 33.5 137.4 128.6 2.8 4.7 6.1 5.6 0.6 3.6 5.2 4.8 0.4 3.2 4.6 4.2 0.5 ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C13H19N2OPF6 Formula weight = 364.27 Tentative Z (number of formula units/cell) = 9.0 giving rho = 1.607, non-H atomic volume = 16.4 and following cell contents and analysis: C 117.00 42.86 % H 171.00 5.26 % N 18.00 7.69 % O 9.00 4.39 % F 54.00 31.30 % P 9.00 8.50 % F(000) = 1692.0 Mo-K(alpha) radiation Mu (mm-1) = 0.25 ------------------------------------------------------------------------------- File 2007src0607.ins set up as follows: TITL 2007src0607 in Pbca CELL 0.71073 11.7560 15.6189 18.4464 90.000 90.000 90.000 ZERR 9.00 0.0004 0.0003 0.0006 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O F P UNIT 117 171 18 9 54 9 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------