++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008src0405r started at 17:44:46 on 24-Apr-2008 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.427 5.665 27.460 90.00 92.25 90.00 18309 Reflections read from file 2008src0405r.hkl; mean (I/sigma) = 5.36 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 9164 9191 9175 9163 13765 12241 12204 18309 N (int>3sigma) = 0 4817 4789 4448 4717 7027 6346 6369 9519 Mean intensity = 0.0 16.9 16.6 15.8 17.8 16.4 17.8 17.9 17.5 Mean int/sigma = 0.0 5.5 5.5 5.1 5.4 5.4 5.5 5.5 5.5 Lattice type: P chosen Volume: 1776.42 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 5.665 11.427 27.460 92.25 90.00 90.00 Niggli form: a.a = 32.10 b.b = 130.59 c.c = 754.05 b.c = -12.32 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. MONOCLINIC P-lattice R(sym) = 0.049 [ 2601] Cell: 11.427 5.665 27.460 90.00 92.25 90.00 Volume: 1776.42 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 9164 9191 9175 9163 13765 12241 12204 18309 N (int>3sigma) = 0 4817 4789 4448 4717 7027 6346 6369 9519 Mean intensity = 0.0 16.9 16.6 15.8 17.8 16.4 17.8 17.9 17.5 Mean int/sigma = 0.0 5.5 5.5 5.1 5.4 5.4 5.5 5.5 5.5 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.997 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 12 1115 1101 1118 N I>3s 0 1 392 393 0.2 0.3 24.6 24.3 0.6 0.5 4.6 4.6 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)/c # 14 centro 4 19410 0.049 2601 0.6 / 4.6 2.54 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008src0405r.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 220 230 95.7 6.85 79.4 31.24 0.0302 0.0209 2.20 - 1.70 239 239 100.0 7.59 31.5 25.85 0.0438 0.0268 1.70 - 1.45 251 251 100.0 7.76 15.5 18.75 0.0641 0.0333 1.45 - 1.30 278 278 100.0 5.96 10.8 14.67 0.0930 0.0514 1.30 - 1.20 256 258 99.2 5.22 12.2 14.21 0.0842 0.0508 1.20 - 1.10 348 349 99.7 5.05 11.9 11.66 0.0947 0.0558 1.10 - 1.05 227 232 97.8 4.39 10.4 9.39 0.1097 0.0683 1.05 - 1.00 276 283 97.5 3.39 6.7 7.24 0.1337 0.1041 1.00 - 0.95 298 305 97.7 3.12 6.2 6.22 0.1336 0.1245 0.95 - 0.90 421 436 96.6 2.93 5.0 4.56 0.1887 0.1747 0.90 - 0.85 484 505 95.8 2.69 3.4 3.10 0.2806 0.2830 0.85 - 0.80 599 648 92.4 2.38 2.5 2.26 0.4133 0.4156 0.80 - 0.77 458 535 85.6 2.05 2.2 1.85 0.5022 0.5466 ------------------------------------------------------------------------------ 0.90 - 0.77 1541 1688 91.3 2.37 2.7 2.40 0.3740 0.3953 Inf - 0.77 4355 4549 95.7 4.02 11.8 9.45 0.0664 0.0743 Merged [A], lowest resolution = 6.86 Angstroms, 588 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008src0405r.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C21H19FN2O3 Formula weight = 366.38 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.370, non-H atomic volume = 16.4 and following cell contents and analysis: C 84.00 68.84 % H 76.00 5.23 % N 8.00 7.65 % O 12.00 13.10 % F 4.00 5.19 % F(000) = 768.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File 1.ins set up as follows: TITL 1 in P2(1)/c CELL 0.71073 27.4599 5.6654 11.4275 90.000 92.250 90.000 ZERR 4.00 0.0012 0.0002 0.0005 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O F UNIT 84 76 8 12 4 TEMP 0.03 TREF HKLF 4 END -------------------------------------------------------------------------------