++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh038 started at 22:19:37 on 13-Nov-2010 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 4.068 10.513 17.044 90.00 90.00 90.00 6471 Reflections read from file 2008lsh038.hkl; mean (I/sigma) = 14.87 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3238 3210 3190 3219 4819 4308 4307 6471 N (int>3sigma) = 0 2861 2783 2850 2805 4247 3878 3880 5826 Mean intensity = 0.0 655.7 545.3 625.3 568.7 608.9 654.6 645.7 641.3 Mean int/sigma = 0.0 14.8 14.3 14.6 14.4 14.6 15.0 14.9 14.9 Lattice type: P chosen Volume: 728.80 ------------------------------------------------------------------------------- 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: 4.068 10.513 17.044 90.00 90.00 90.00 Niggli form: a.a = 16.54 b.b = 110.52 c.c = 290.48 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) = 0.019 [ 2034] Cell: 4.068 10.513 17.044 90.00 90.00 90.00 Volume: 728.80 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 3238 3210 3190 3219 4819 4308 4307 6471 N (int>3sigma) = 0 2861 2783 2850 2805 4247 3878 3880 5826 Mean intensity = 0.0 655.7 545.3 625.3 568.7 608.9 654.6 645.7 641.3 Mean int/sigma = 0.0 14.8 14.3 14.6 14.4 14.6 15.0 14.9 14.9 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.753 [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 617 597 616 5 221 212 209 11 107 98 95 42 N I>3s 525 479 510 0 114 110 4 3 45 3 48 4 778.4 614.3 792.4 1.0 600.7 625.0 2.8 7.8 616.6 2.7 695.3 6.0 14.6 14.2 14.6 0.3 9.6 9.8 0.7 1.5 8.2 0.7 9.3 1.2 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] Pna2(1) # 33 non-cen 3 903 0.019 2034 1.5 / 8.2 1.47 [B] Pnma # 62 centro 2 894 0.019 2034 1.5 / 8.2 6.05 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh038.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 53 61 86.9 6.07 2484.9 53.09 0.0139 0.0151 2.20 - 1.70 63 63 100.0 8.02 1449.5 57.83 0.0191 0.0152 1.70 - 1.45 59 59 100.0 9.05 765.1 57.07 0.0231 0.0139 1.45 - 1.30 63 63 100.0 8.98 498.8 47.71 0.0303 0.0171 1.30 - 1.20 63 63 100.0 9.03 617.0 50.16 0.0286 0.0164 1.20 - 1.10 84 84 100.0 8.45 632.1 45.71 0.0265 0.0169 1.10 - 1.00 110 110 100.0 7.57 482.5 39.92 0.0326 0.0216 1.00 - 0.95 76 76 100.0 6.91 216.6 29.84 0.0491 0.0259 0.95 - 0.90 95 96 99.0 5.36 218.2 24.49 0.0505 0.0304 0.90 - 0.85 113 113 100.0 4.49 179.4 20.63 0.0619 0.0404 0.85 - 0.80 141 142 99.3 3.50 140.0 14.99 0.0586 0.0521 0.80 - 0.77 116 119 97.5 2.86 99.4 11.78 0.0769 0.0729 ------------------------------------------------------------------------------ 0.90 - 0.77 370 374 98.9 3.59 139.3 15.71 0.0633 0.0522 Inf - 0.77 1036 1049 98.8 6.17 514.8 33.42 0.0262 0.0206 Merged [A], lowest resolution = 6.62 Angstroms, 221 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh038.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H9N1O2 Formula weight = 151.16 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.378, non-H atomic volume = 16.6 and following cell contents and analysis: C 32.00 63.56 % H 36.00 6.00 % N 4.00 9.27 % O 8.00 21.17 % F(000) = 320.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File Pna21.ins set up as follows: TITL Pna21 in Pna2(1) CELL 0.71073 10.5129 17.0435 4.0675 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0004 0.0001 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, 0.5-Y, Z SYMM 0.5-X, 0.5+Y, 0.5+Z SFAC C H N O UNIT 32 36 4 8 TEMP 0.06 TREF HKLF 4 END 6471 Reflections written to new reflection file Pna21.hkl -------------------------------------------------------------------------------