++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh001 started at 13:38:05 on 17-Nov-2010 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.663 9.289 19.822 90.00 90.03 90.00 20015 Reflections read from file 2008lsh001.hkl; mean (I/sigma) = 5.78 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 9983 10036 10029 9997 15024 13315 13331 20015 N (int>3sigma) = 0 4467 5087 5156 5013 7355 6634 6635 10021 Mean intensity = 0.0 12.7 20.6 21.1 20.2 18.1 19.9 19.9 19.6 Mean int/sigma = 0.0 5.1 6.0 6.0 5.9 5.7 5.9 5.9 5.9 Lattice type: P chosen Volume: 1779.19 ------------------------------------------------------------------------------- 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: 9.289 9.663 19.822 90.03 90.00 90.00 Niggli form: a.a = 86.28 b.b = 93.37 c.c = 392.92 b.c = -0.11 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 = 0.032 deg. ORTHORHOMBIC P-lattice R(sym) = 0.034 [ 5327] Cell: 9.289 9.663 19.822 90.03 90.00 90.00 Volume: 1779.19 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 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 10036 9983 10029 9997 15024 13312 13351 20015 N (int>3sigma) = 0 5087 4467 5156 5013 7355 6632 6637 10021 Mean intensity = 0.0 20.6 12.7 21.1 20.2 18.1 19.6 19.9 19.6 Mean int/sigma = 0.0 6.0 5.1 6.0 5.9 5.7 5.8 5.9 5.9 Crystal system O and Lattice type P selected Mean |E*E-1| = 1.185 [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 688 679 671 15 677 697 672 13 288 284 286 34 N I>3s 285 2 287 0 235 2 235 0 78 1 79 0 52.2 0.3 53.5 0.1 22.6 0.2 22.8 0.2 3.4 0.2 3.4 0.3 7.1 0.5 7.3 0.4 5.1 0.5 5.1 0.4 2.9 0.5 2.9 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] Pbca # 61 centro 2 2293 0.034 5327 0.5 / 2.9 8.95 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh001.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 119 131 90.8 7.91 73.3 30.82 0.0287 0.0175 2.20 - 1.70 127 127 100.0 10.45 63.6 32.15 0.0295 0.0152 1.70 - 1.45 141 141 100.0 10.73 47.0 32.14 0.0349 0.0185 1.45 - 1.30 145 145 100.0 10.79 20.5 25.43 0.0474 0.0204 1.30 - 1.20 126 126 100.0 11.20 25.3 24.39 0.0461 0.0226 1.20 - 1.10 189 189 100.0 11.16 20.3 22.69 0.0550 0.0242 1.10 - 1.00 264 264 100.0 10.95 14.1 18.70 0.0684 0.0298 1.00 - 0.95 172 172 100.0 10.19 9.4 13.02 0.0918 0.0418 0.95 - 0.90 219 219 100.0 8.59 8.3 10.38 0.1146 0.0515 0.90 - 0.85 268 268 100.0 7.03 5.0 7.74 0.1552 0.0759 0.85 - 0.80 331 331 100.0 5.03 2.9 4.40 0.2377 0.1507 0.80 - 0.77 263 271 97.0 3.63 2.1 2.78 0.3208 0.2607 ------------------------------------------------------------------------------ 0.90 - 0.77 862 870 99.1 5.21 3.3 4.94 0.2000 0.1362 Inf - 0.77 2364 2384 99.2 8.40 18.4 15.67 0.0512 0.0296 Merged [A], lowest resolution = 6.78 Angstroms, 915 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh001.hkl ------------------------------------------------------------------------------- ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8 H8 N1 O1 F3 Formula weight = 191.15 Tentative Z (number of formula units/cell) = 9.0 giving rho = 1.606, non-H atomic volume = 15.2 and following cell contents and analysis: C 72.00 50.26 % H 72.00 4.22 % N 9.00 7.33 % O 9.00 8.37 % F 27.00 29.82 % F(000) = 882.0 Mo-K(alpha) radiation Mu (mm-1) = 0.15 ------------------------------------------------------------------------------- File Pbca.ins set up as follows: TITL Pbca in Pbca CELL 0.71073 9.6630 9.2888 19.8221 90.000 90.000 90.000 ZERR 9.00 0.0003 0.0002 0.0005 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 UNIT 72 72 9 9 27 TEMP file. TREF HKLF 4 END 20015 Reflections written to new reflection file Pbca.hkl -------------------------------------------------------------------------------