++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2007src0763 started at 17:16:42 on 28-Jun-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.380 12.992 15.408 90.00 90.00 90.00 11136 Reflections read from file 2007src0763.hkl; mean (I/sigma) = 9.00 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5595 5548 5585 5600 8364 7426 7440 11136 N (int>3sigma) = 0 4833 4777 4786 4750 7198 6457 6480 9680 Mean intensity = 0.0 33.4 39.1 40.0 36.9 37.5 39.9 39.8 39.6 Mean int/sigma = 0.0 8.8 9.0 9.0 8.7 8.9 9.0 9.0 9.0 Lattice type: P chosen Volume: 1877.70 ------------------------------------------------------------------------------- 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: 9.380 12.992 15.408 90.00 90.00 90.00 Niggli form: a.a = 87.98 b.b = 168.80 c.c = 237.39 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) = 0.040 [ 4989] Cell: 9.380 12.992 15.408 90.00 90.00 90.00 Volume: 1877.70 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 5595 5548 5585 5600 8364 7426 7440 11136 N (int>3sigma) = 0 4833 4777 4786 4750 7198 6457 6480 9680 Mean intensity = 0.0 33.4 39.1 40.0 36.9 37.5 39.9 39.8 39.6 Mean int/sigma = 0.0 8.8 9.0 9.0 8.7 8.9 9.0 9.0 9.0 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.831 [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 390 396 392 8 255 277 286 11 200 204 196 21 N I>3s 344 347 339 1 69 180 175 1 104 116 16 5 75.4 59.3 59.1 0.6 1.3 61.5 59.4 0.6 73.4 72.2 0.6 1.3 9.7 10.0 9.6 1.2 2.3 7.0 6.7 0.9 7.0 7.1 1.0 2.2 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 4 903 0.040 4989 2.3 / 6.7 3.28 [B] Pnma # 62 centro 5 894 0.040 4989 2.3 / 6.7 4.24 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2007src0763.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.10 143 154 92.9 5.65 133.3 29.99 0.0482 0.0277 2.10 - 1.60 159 159 100.0 6.82 70.1 31.23 0.0490 0.0268 1.60 - 1.40 147 147 100.0 6.88 46.3 28.32 0.0510 0.0299 1.40 - 1.25 170 170 100.0 6.09 45.9 26.48 0.0520 0.0331 1.25 - 1.15 159 159 100.0 5.23 43.5 23.54 0.0576 0.0400 1.15 - 1.05 234 235 99.6 4.82 28.8 20.43 0.0578 0.0422 1.05 - 1.00 147 147 100.0 4.41 18.8 17.57 0.0652 0.0468 1.00 - 0.95 190 190 100.0 3.83 16.5 14.95 0.0687 0.0524 0.95 - 0.90 223 225 99.1 3.10 12.2 12.06 0.0762 0.0663 0.90 - 0.85 280 280 100.0 2.99 11.7 10.89 0.0724 0.0721 0.85 - 0.80 361 362 99.7 2.77 10.2 8.87 0.0829 0.0872 0.80 - 0.75 437 442 98.9 2.47 8.5 7.62 0.0955 0.1058 0.75 - 0.74 96 108 88.9 1.54 7.1 6.54 0.1073 0.1392 ------------------------------------------------------------------------------ 0.85 - 0.74 894 912 98.0 2.48 9.0 8.01 0.0896 0.1002 Inf - 0.74 2746 2778 98.8 4.01 28.6 16.30 0.0546 0.0429 Merged [A], lowest resolution = 6.82 Angstroms, 220 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2007src0763.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C19H28Cl1N1O2S1 Formula weight = 369.93 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.309, non-H atomic volume = 19.6 and following cell contents and analysis: C 76.00 61.68 % H 112.00 7.63 % N 4.00 3.79 % O 8.00 8.65 % S 4.00 8.67 % Cl 4.00 9.58 % F(000) = 792.0 Mo-K(alpha) radiation Mu (mm-1) = 0.33 ------------------------------------------------------------------------------- File Test.ins set up as follows: TITL Test in Pna2(1) CELL 0.71073 15.4076 12.9924 9.3800 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0004 0.0003 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 S CL UNIT 76 112 4 8 4 4 TEMP 0.1 TREF HKLF 4 END 11136 Reflections written to new reflection file Test.hkl -------------------------------------------------------------------------------