+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2007/1 for Windows + + Copyright(C) 2007 Bruker-AXS All Rights Reserved + + 2007src1375 started at 17:05:56 on 20-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 5.692 8.336 26.310 90.00 90.00 90.00 8764 Reflections read from file 2007src1375.hkl; mean (I/sigma) = 6.30 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4388 4391 4367 4382 6573 5830 5863 8764 N (int>3sigma) = 0 2748 2667 2611 2721 4013 3715 3747 5567 Mean intensity = 0.0 161.0 116.7 140.1 135.9 139.3 153.7 153.8 151.1 Mean int/sigma = 0.0 6.3 6.0 6.1 6.3 6.2 6.5 6.5 6.4 Lattice type: P chosen Volume: 1248.39 ------------------------------------------------------------------------------- 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: 5.692 8.336 26.310 90.00 90.00 90.00 Niggli form: a.a = 32.40 b.b = 69.49 c.c = 692.20 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) = 0.049 [ 2977] Cell: 5.692 8.336 26.310 90.00 90.00 90.00 Volume: 1248.39 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 4388 4391 4367 4382 6573 5830 5863 8764 N (int>3sigma) = 0 2748 2667 2611 2721 4013 3715 3747 5567 Mean intensity = 0.0 161.0 116.7 140.1 135.9 139.3 153.7 153.8 151.1 Mean int/sigma = 0.0 6.3 6.0 6.1 6.3 6.2 6.5 6.5 6.4 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.976 [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 471 500 509 4 425 451 404 7 95 99 88 42 N I>3s 2 187 187 0 223 225 10 0 76 69 63 4 2.4 185.7 182.6 0.7 326.8 308.8 2.9 5.6 805.3 668.4 637.6 4.1 0.7 4.3 4.3 0.6 6.1 5.9 0.9 1.2 8.0 7.2 7.7 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 2 903 0.049 2977 1.2 / 4.3 8.80 [B] Pnma # 62 centro 3 894 0.049 2977 1.2 / 4.3 3.02 Option [B] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2007src1375.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.30 87 93 93.5 8.75 823.7 22.82 0.0554 0.0372 2.30 - 1.75 89 89 100.0 7.83 294.5 24.69 0.0599 0.0336 1.75 - 1.52 88 88 100.0 6.93 241.0 20.05 0.0576 0.0343 1.52 - 1.36 92 92 100.0 6.33 124.2 18.30 0.0588 0.0407 1.36 - 1.25 97 97 100.0 6.61 161.7 19.18 0.0669 0.0369 1.25 - 1.17 87 87 100.0 6.18 121.1 15.55 0.0674 0.0371 1.17 - 1.10 108 108 100.0 5.38 154.6 16.65 0.0623 0.0415 1.10 - 1.05 90 90 100.0 5.18 63.2 12.68 0.0762 0.0527 1.05 - 1.00 109 109 100.0 5.07 48.2 13.27 0.0892 0.0586 1.00 - 0.96 93 93 100.0 4.94 66.1 13.73 0.0854 0.0527 0.96 - 0.93 88 90 97.8 4.11 48.0 9.66 0.0888 0.0660 0.93 - 0.90 116 116 100.0 4.22 48.4 10.22 0.0970 0.0682 0.90 - 0.87 115 115 100.0 4.05 38.4 8.48 0.1038 0.0813 0.87 - 0.84 115 116 99.1 3.71 36.1 8.03 0.1122 0.0915 0.84 - 0.82 98 103 95.1 3.30 19.0 5.95 0.1528 0.1353 0.82 - 0.80 113 113 100.0 3.19 30.2 6.60 0.1055 0.1120 0.80 - 0.78 121 121 100.0 2.98 27.5 5.61 0.1289 0.1231 0.78 - 0.77 6 16 37.5 0.38 23.5 3.66 0.2438 ------------------------------------------------------------------------------ 0.87 - 0.77 493 509 96.9 3.24 27.8 6.51 0.1227 0.1135 Inf - 0.77 1712 1736 98.6 5.05 127.1 13.12 0.0644 0.0451 Merged [A], lowest resolution = 6.58 Angstroms, 118 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2007src1375.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C22H12S3 Formula weight = 372.53 Tentative Z (number of formula units/cell) = 3.0 giving rho = 1.487, non-H atomic volume = 16.6 and following cell contents and analysis: C 66.00 70.93 % H 36.00 3.25 % S 9.00 25.82 % F(000) = 576.0 Mo-K(alpha) radiation Mu (mm-1) = 0.45 ------------------------------------------------------------------------------- File 2.ins set up as follows: TITL 2 in Pnma CELL 0.71073 8.3358 26.3096 5.6923 90.000 90.000 90.000 ZERR 3.00 0.0006 0.0017 0.0003 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, -Z SYMM 0.5+X, 0.5-Y, 0.5-Z SFAC C H S UNIT 66 36 9 TEMP 0.005 TREF HKLF 4 END ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C22H12S Formula weight = 308.40 Tentative Z (number of formula units/cell) = 2.0 giving rho = 0.820, non-H atomic volume = 27.1 and following cell contents and analysis: C 44.00 85.68 % H 24.00 3.92 % S 2.00 10.40 % F(000) = 320.0 Mo-K(alpha) radiation Mu (mm-1) = 0.13 -------------------------------------------------------------------------------