++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh013 started at 10:01:13 on 19-Nov-2010 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.495 9.117 24.663 90.00 90.00 90.00 15636 Reflections read from file 2008lsh013.hkl; mean (I/sigma) = 6.84 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7825 7815 7868 7831 11754 10432 10446 15636 N (int>3sigma) = 0 5245 5049 5016 5310 7655 7008 7009 10509 Mean intensity = 0.0 31.5 29.1 30.4 30.6 30.3 33.0 33.1 32.7 Mean int/sigma = 0.0 6.9 6.6 6.6 6.9 6.7 7.0 7.0 6.9 Lattice type: P chosen Volume: 1685.29 ------------------------------------------------------------------------------- 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: 7.495 9.117 24.663 90.00 90.00 90.00 Niggli form: a.a = 56.18 b.b = 83.12 c.c = 608.25 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) = 0.036 [ 5161] Cell: 7.495 9.117 24.663 90.00 90.00 90.00 Volume: 1685.29 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 7825 7815 7868 7831 11754 10432 10446 15636 N (int>3sigma) = 0 5245 5049 5016 5310 7655 7008 7009 10509 Mean intensity = 0.0 31.5 29.1 30.4 30.6 30.3 33.0 33.1 32.7 Mean int/sigma = 0.0 6.9 6.6 6.6 6.9 6.7 7.0 7.0 6.9 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.983 [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 699 712 701 12 649 666 653 10 188 194 188 45 N I>3s 318 1 317 0 235 1 236 0 57 1 56 0 39.7 0.2 39.6 0.2 24.9 0.3 24.8 0.1 16.4 0.2 16.4 0.2 5.3 0.5 5.3 0.4 4.6 0.6 4.6 0.4 3.6 0.6 3.6 0.5 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 0.036 5161 0.6 / 3.6 3.41 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh013.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 116 125 92.8 8.44 113.4 26.32 0.0381 0.0324 2.20 - 1.70 129 129 100.0 10.71 83.5 34.63 0.0366 0.0230 1.70 - 1.45 130 130 100.0 11.24 38.9 29.36 0.0490 0.0240 1.45 - 1.30 130 130 100.0 11.30 26.7 25.96 0.0725 0.0266 1.30 - 1.20 139 139 100.0 8.95 29.8 22.89 0.0668 0.0319 1.20 - 1.10 171 171 100.0 8.26 35.9 22.05 0.0700 0.0333 1.10 - 1.05 115 115 100.0 7.50 22.4 18.20 0.0729 0.0387 1.05 - 1.00 143 143 100.0 6.90 17.7 16.14 0.0796 0.0421 1.00 - 0.95 161 161 100.0 5.56 15.4 13.78 0.0675 0.0498 0.95 - 0.90 211 211 100.0 5.30 11.3 11.27 0.0795 0.0597 0.90 - 0.85 251 251 100.0 4.98 9.0 9.51 0.0971 0.0688 0.85 - 0.80 329 329 100.0 4.59 6.3 7.28 0.1226 0.0929 0.80 - 0.77 228 228 100.0 4.33 4.5 5.89 0.1706 0.1239 ------------------------------------------------------------------------------ 0.90 - 0.77 808 808 100.0 4.64 6.7 7.58 0.1202 0.0887 Inf - 0.77 2253 2262 99.6 6.91 25.8 16.33 0.0550 0.0374 Merged [A], lowest resolution = 6.40 Angstroms, 668 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh013.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H11N1O2 Formula weight = 153.18 Tentative Z (number of formula units/cell) = 9.0 giving rho = 1.358, non-H atomic volume = 17.0 and following cell contents and analysis: C 72.00 62.72 % H 99.00 7.24 % N 9.00 9.15 % O 18.00 20.89 % F(000) = 738.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File pbca.ins set up as follows: TITL pbca in Pbca CELL 0.71073 9.1172 7.4950 24.6628 90.000 90.000 90.000 ZERR 9.00 0.0002 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 UNIT 72 99 9 18 TEMP 0.1 TREF HKLF 4 END 15636 Reflections written to new reflection file pbca.hkl -------------------------------------------------------------------------------