++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008src0764 started at 13:30:56 on 01-Jul-2008 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.697 13.235 17.356 90.00 90.00 90.00 21554 Reflections read from file 2008src0764.hkl; mean (I/sigma) = 11.25 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 10802 10783 10789 10741 16187 14375 14343 21554 N (int>3sigma) = 0 9067 9137 9144 9035 13674 12209 12159 18317 Mean intensity = 0.0 40.2 39.9 40.4 42.4 40.2 40.8 40.8 41.3 Mean int/sigma = 0.0 11.2 11.1 11.2 11.1 11.2 11.3 11.2 11.3 Lattice type: P chosen Volume: 2227.56 ------------------------------------------------------------------------------- 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: 9.697 13.235 17.356 90.00 90.00 90.00 Niggli form: a.a = 94.04 b.b = 175.16 c.c = 301.24 b.c = 0.00 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(sym) = 0.028 [ 6595] Cell: 9.697 13.235 17.356 90.00 90.00 90.00 Volume: 2227.56 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 10802 10783 10789 10741 16187 14375 14343 21554 N (int>3sigma) = 0 9067 9137 9144 9035 13674 12209 12159 18317 Mean intensity = 0.0 40.2 39.9 40.4 42.4 40.2 40.8 40.8 41.3 Mean int/sigma = 0.0 11.2 11.1 11.2 11.1 11.2 11.3 11.2 11.3 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.751 [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 633 640 631 12 568 563 575 18 381 387 390 24 N I>3s 509 536 491 0 403 419 436 0 293 269 288 0 48.6 37.4 50.0 0.3 46.4 37.9 45.4 0.3 74.5 56.5 52.6 0.1 11.8 11.9 11.3 0.6 10.2 10.3 10.2 0.5 12.7 11.2 11.4 0.4 Identical indices and Friedel opposites combined before calculating R(sym) Option Space Group No. Type Axes CSD R(sym) N(eq) Syst. Abs. CFOM [A] P2(1)2(1)2(1) # 19 chiral 1 5917 0.028 6595 0.6 / 10.2 1.02 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008src0764.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.15 152 166 91.6 7.46 160.1 63.58 0.0200 0.0162 2.15 - 1.70 147 147 100.0 9.45 95.4 63.37 0.0243 0.0139 1.70 - 1.45 174 174 100.0 9.53 73.2 54.15 0.0289 0.0158 1.45 - 1.30 179 179 100.0 9.77 56.4 49.06 0.0327 0.0179 1.30 - 1.20 161 161 100.0 9.76 43.9 42.64 0.0367 0.0199 1.20 - 1.10 224 224 100.0 9.97 37.0 36.70 0.0439 0.0222 1.10 - 1.05 157 157 100.0 9.69 32.1 31.61 0.0501 0.0253 1.05 - 1.00 174 174 100.0 9.60 26.3 30.55 0.0643 0.0271 1.00 - 0.95 215 215 100.0 8.19 18.0 23.15 0.0748 0.0342 0.95 - 0.90 275 275 100.0 7.17 12.6 17.67 0.0988 0.0452 0.90 - 0.85 332 332 100.0 5.61 10.2 13.41 0.1146 0.0622 0.85 - 0.80 413 413 100.0 4.28 9.0 10.14 0.1178 0.0854 0.80 - 0.77 303 305 99.3 3.79 8.7 8.60 0.1378 0.1034 ------------------------------------------------------------------------------ 0.90 - 0.77 1048 1050 99.8 4.56 9.3 10.73 0.1206 0.0822 Inf - 0.77 2906 2922 99.5 7.38 35.5 28.78 0.0397 0.0255 Merged [A], lowest resolution = 6.47 Angstroms, 878 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008src0764.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C22H25N2OF6P Formula weight = 478.41 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.427, non-H atomic volume = 17.4 and following cell contents and analysis: C 88.00 55.23 % H 100.00 5.27 % N 8.00 5.86 % O 4.00 3.34 % F 24.00 23.83 % P 4.00 6.47 % F(000) = 992.0 Mo-K(alpha) radiation Mu (mm-1) = 0.19 ------------------------------------------------------------------------------- File 2008src0764.ins set up as follows: TITL 2008src0764 in P2(1)2(1)2(1) CELL 0.71073 9.6974 13.2347 17.3564 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0002 0.0002 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 88 100 8 4 24 4 TEMP 0.2 TREF HKLF 4 END -------------------------------------------------------------------------------