++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2009src0671 started at 16:37:21 on 14-Jul-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 18.949 5.602 20.793 90.00 90.36 90.00 10903 Reflections read from file 2009src0671.hkl; mean (I/sigma) = 7.37 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5449 5449 0 5451 5449 7260 7299 10903 N (int>3sigma) = 0 4021 4021 0 4114 4021 5430 5477 8114 Mean intensity = 0.0 316.0 316.0 0.0 315.5 316.0 335.5 339.8 337.1 Mean int/sigma = 0.0 7.3 7.3 0.0 7.5 7.3 7.4 7.5 7.4 Lattice type: C chosen Volume: 2207.36 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 0.0000 -0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 Unitcell: 5.602 9.880 20.793 89.66 90.00 73.53 Niggli form: a.a = 31.39 b.b = 97.61 c.c = 432.37 b.c = 1.22 a.c = 0.00 a.b = 15.69 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.355 deg. ORTHORHOMBIC C-lattice R(sym) = 0.525 [ 3266] Cell: 5.602 18.949 20.793 89.64 90.00 90.00 Volume: 2207.36 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC C-lattice R(sym) = 0.042 [ 1973] Cell: 18.949 5.602 20.793 90.00 90.36 90.00 Volume: 2207.36 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.355 deg. MONOCLINIC C-lattice R(sym) = 0.537 [ 2144] Cell: 5.602 18.949 20.793 90.36 90.00 90.00 Volume: 2207.36 Matrix: 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.355 deg. MONOCLINIC P-lattice R(sym) = 0.544 [ 2161] Cell: 5.602 20.793 9.880 90.34 106.47 90.00 Volume: 1103.68 Matrix: 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 0.5000 -0.5000 0.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5449 5449 0 5451 5449 7260 7299 10903 N (int>3sigma) = 0 4021 4021 0 4114 4021 5430 5477 8114 Mean intensity = 0.0 316.0 316.0 0.0 315.5 316.0 335.5 339.8 337.1 Mean int/sigma = 0.0 7.3 7.3 0.0 7.5 7.3 7.4 7.5 7.4 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.732 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 719 N I>3s 483 461.7 7.1 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] C2 # 5 chiral 1 552 0.042 1973 0.0 / 7.1 1.59 [B] C2/m # 12 centro 1 310 0.042 1973 0.0 / 7.1 7.31 [C] Cm # 8 non-cen 1 32 0.042 1973 0.0 / 7.1 4.44 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2009src0671.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.15 148 154 96.1 6.05 1419.4 33.12 0.0329 0.0256 2.15 - 1.65 157 157 100.0 6.76 634.8 29.57 0.0424 0.0272 1.65 - 1.40 180 180 100.0 6.76 381.0 25.05 0.0612 0.0327 1.40 - 1.25 205 206 99.5 5.18 259.7 19.71 0.0779 0.0434 1.25 - 1.15 177 177 100.0 4.92 253.9 18.27 0.0741 0.0450 1.15 - 1.05 267 268 99.6 4.29 205.8 14.75 0.0846 0.0553 1.05 - 1.00 168 171 98.2 3.81 151.6 12.54 0.0938 0.0710 1.00 - 0.95 200 201 99.5 3.33 124.0 9.47 0.1140 0.0877 0.95 - 0.90 253 253 100.0 2.80 81.9 6.72 0.1459 0.1306 0.90 - 0.85 333 339 98.2 2.72 73.6 5.99 0.1478 0.1480 0.85 - 0.80 381 384 99.2 2.49 60.2 4.65 0.1911 0.1966 0.80 - 0.77 307 323 95.0 2.17 53.8 3.85 0.2103 0.2362 ------------------------------------------------------------------------------ 0.90 - 0.77 1021 1046 97.6 2.46 62.6 4.85 0.1768 0.1882 Inf - 0.77 2776 2813 98.7 3.88 240.1 12.94 0.0598 0.0547 Merged [A], lowest resolution = 6.98 Angstroms, 203 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2009src0671.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C21H26O9S Formula weight = 454.48 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.368, non-H atomic volume = 17.8 and following cell contents and analysis: C 84.00 55.49 % H 104.00 5.77 % O 36.00 31.68 % S 4.00 7.05 % F(000) = 960.0 Mo-K(alpha) radiation Mu (mm-1) = 0.20 ------------------------------------------------------------------------------- File 2009src0671.ins set up as follows: TITL 2009src0671 in C2 CELL 0.71073 18.9488 5.6024 20.7934 90.000 90.355 90.000 ZERR 4.00 0.0006 0.0001 0.0006 0.000 0.002 0.000 LATT -7 SYMM -X, Y, -Z SFAC C H O S UNIT 84 104 36 4 TEMP 0.15 TREF HKLF 4 END -------------------------------------------------------------------------------