++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2009src0667 started at 12:18:57 on 22-Jul-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.329 25.403 9.010 90.00 90.02 90.00 17319 Reflections read from file 2009src0667.hkl; mean (I/sigma) = 8.31 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8709 8635 8702 8607 13023 11508 11499 17319 N (int>3sigma) = 0 6841 6770 6757 6564 10184 9095 9088 13659 Mean intensity = 0.0 148.1 150.6 136.6 112.8 145.1 147.8 145.0 143.9 Mean int/sigma = 0.0 8.4 8.3 8.3 7.9 8.3 8.3 8.3 8.3 Lattice type: P chosen Volume: 1906.25 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 8.329 9.010 25.403 90.00 90.00 90.02 Niggli form: a.a = 69.37 b.b = 81.18 c.c = 645.30 b.c = 0.00 a.c = 0.00 a.b = -0.02 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.016 deg. ORTHORHOMBIC P-lattice R(sym) = 0.046 [ 5819] Cell: 8.329 9.010 25.403 90.00 90.00 90.02 Volume: 1906.25 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 8709 8702 8635 8607 13023 11507 11508 17319 N (int>3sigma) = 0 6841 6757 6770 6564 10184 9080 9095 13659 Mean intensity = 0.0 148.1 136.6 150.6 112.8 145.1 146.6 147.8 143.9 Mean int/sigma = 0.0 8.4 8.3 8.3 7.9 8.3 8.3 8.3 8.3 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.740 [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 640 656 642 11 650 637 643 11 233 232 223 37 N I>3s 462 451 425 0 520 511 473 0 169 172 153 2 195.9 186.8 120.4 1.3 247.3 292.3 250.6 1.3 428.3 482.7 289.0 2.9 8.3 7.9 7.5 0.8 9.6 10.0 9.3 0.7 9.4 9.8 8.3 1.1 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)2(1)2(1) # 19 chiral 1 5917 0.046 5819 1.1 / 7.5 1.52 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2009src0667.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 132 140 94.3 12.04 683.9 49.30 0.0320 0.0185 2.20 - 1.70 136 136 100.0 11.08 303.6 43.33 0.0403 0.0201 1.70 - 1.45 158 158 100.0 9.28 128.1 33.91 0.0573 0.0248 1.45 - 1.30 150 150 100.0 8.79 89.1 29.11 0.0635 0.0276 1.30 - 1.20 144 144 100.0 8.35 93.0 27.56 0.0663 0.0306 1.20 - 1.10 198 198 100.0 7.29 98.5 24.92 0.0669 0.0363 1.10 - 1.05 128 128 100.0 6.79 71.8 22.24 0.0777 0.0364 1.05 - 1.00 154 154 100.0 6.39 52.6 18.03 0.0956 0.0437 1.00 - 0.95 185 185 100.0 6.01 39.5 14.71 0.1157 0.0535 0.95 - 0.90 236 236 100.0 5.59 31.8 12.78 0.1316 0.0662 0.90 - 0.85 293 294 99.7 5.21 17.0 8.17 0.1937 0.1059 0.85 - 0.80 362 362 100.0 4.87 16.6 6.98 0.2101 0.1205 0.80 - 0.77 258 260 99.2 4.29 15.0 6.03 0.2411 0.1454 ------------------------------------------------------------------------------ 0.90 - 0.77 913 916 99.7 4.81 16.3 7.09 0.2110 0.1221 Inf - 0.77 2534 2545 99.6 6.81 96.7 19.28 0.0520 0.0321 Merged [A], lowest resolution = 6.96 Angstroms, 1025 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2009src0667.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C16H22O11 Formula weight = 390.34 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.360, non-H atomic volume = 17.7 and following cell contents and analysis: C 64.00 49.23 % H 88.00 5.68 % O 44.00 45.09 % F(000) = 824.0 Mo-K(alpha) radiation Mu (mm-1) = 0.12 ------------------------------------------------------------------------------- File 2009src0667a.ins set up as follows: TITL 2009src0667a in P2(1)2(1)2(1) CELL 0.71073 8.3288 9.0098 25.4028 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0003 0.0008 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 O UNIT 64 88 44 TEMP 0.03 TREF HKLF 4 END 17319 Reflections written to new reflection file 2009src0667a.hkl -------------------------------------------------------------------------------