++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2007may0017 started at 17:59:48 on 02-Oct-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.848 8.398 24.125 90.00 90.00 90.00 17116 Reflections read from file 2007may0017.hkl; mean (I/sigma) = 5.97 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8517 8518 8467 8528 12751 11398 11395 17116 N (int>3sigma) = 0 5011 5489 4852 4986 7676 7145 7164 10715 Mean intensity = 0.0 89.7 114.9 93.1 95.6 99.3 109.7 107.8 109.0 Mean int/sigma = 0.0 5.6 6.2 5.5 5.6 5.8 6.1 6.1 6.1 Lattice type: P chosen Volume: 1590.19 ------------------------------------------------------------------------------- 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: 7.848 8.398 24.125 90.00 90.00 90.00 Niggli form: a.a = 61.60 b.b = 70.53 c.c = 582.04 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) = 0.046 [ 3846] Cell: 7.848 8.398 24.125 90.00 90.00 90.00 Volume: 1590.19 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 8517 8518 8467 8528 12751 11398 11395 17116 N (int>3sigma) = 0 5011 5489 4852 4986 7676 7145 7164 10715 Mean intensity = 0.0 89.7 114.9 93.1 95.6 99.3 109.7 107.8 109.0 Mean int/sigma = 0.0 5.6 6.2 5.5 5.6 5.8 6.1 6.1 6.1 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.921 [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 769 764 735 18 665 692 683 16 249 253 242 32 N I>3s 342 346 36 0 255 4 257 7 188 213 189 1 66.0 66.8 2.2 1.2 100.2 1.4 97.6 6.1 73.9 127.3 126.0 3.0 5.0 5.1 0.9 0.7 4.0 0.7 3.9 2.1 7.7 9.2 8.5 0.9 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 1 903 0.046 3846 2.1 / 3.9 6.80 [B] Pnma # 62 centro 6 894 0.046 3846 2.1 / 3.9 3.62 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2007may0017.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 113 120 94.2 16.36 562.1 37.72 0.0527 0.0311 2.20 - 1.70 115 115 100.0 18.62 192.6 37.42 0.0592 0.0210 1.70 - 1.45 128 129 99.2 14.19 76.6 27.06 0.0680 0.0262 1.45 - 1.30 124 129 96.1 11.09 56.7 24.66 0.0776 0.0332 1.30 - 1.20 117 117 100.0 9.15 55.7 21.00 0.0889 0.0395 1.20 - 1.10 173 175 98.9 8.16 54.0 16.47 0.0963 0.0430 1.10 - 1.00 237 237 100.0 6.65 30.7 13.03 0.1154 0.0575 1.00 - 0.95 161 162 99.4 5.48 19.2 9.10 0.1746 0.0928 0.95 - 0.90 194 196 99.0 5.53 13.6 7.12 0.1990 0.1047 0.90 - 0.85 225 233 96.6 5.11 8.7 5.73 0.2850 0.1566 0.85 - 0.80 297 309 96.1 4.68 7.4 4.34 0.3727 0.2170 0.80 - 0.77 214 232 92.2 4.61 7.0 3.77 0.4100 0.2697 ------------------------------------------------------------------------------ 0.90 - 0.77 736 774 95.1 4.79 7.7 4.60 0.3496 0.2098 Inf - 0.77 2098 2154 97.4 7.95 65.3 14.16 0.0677 0.0420 Merged [A], lowest resolution = 6.89 Angstroms, 370 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2007may0017.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C9H10O3 Formula weight = 166.17 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.388, non-H atomic volume = 16.6 and following cell contents and analysis: C 72.00 65.05 % H 80.00 6.07 % O 24.00 28.89 % F(000) = 704.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File 2007may0017.ins set up as follows: TITL 2007may0017 in Pna2(1) CELL 0.71073 7.8484 8.3983 24.1255 90.000 90.000 90.000 ZERR 8.00 0.0006 0.0007 0.0018 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 O UNIT 72 80 24 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------