+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2008/2 for Windows + + Copyright(C) 2008 Bruker-AXS All Rights Reserved + + 2010src0401 started at 10:16:38 on 01-Jun-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.374 24.541 21.295 90.00 97.47 90.00 27069 Reflections read from file 2010src0401.hkl; mean (I/sigma) = 3.50 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 13542 13561 13535 13559 20319 18020 18076 27069 N (int>3sigma) = 0 5179 4832 5095 4984 7553 6662 6711 10089 Mean intensity = 0.0 102.5 81.6 98.8 88.6 94.3 98.4 97.2 96.4 Mean int/sigma = 0.0 3.8 3.5 3.6 3.6 3.6 3.7 3.7 3.7 Lattice type: P chosen Volume: 3820.80 ------------------------------------------------------------------------------- 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: 7.374 21.295 24.541 90.00 90.00 97.47 Niggli form: a.a = 54.37 b.b = 453.49 c.c = 602.24 b.c = 0.00 a.c = 0.00 a.b = -20.43 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.108 [ 5406] Cell: 7.374 24.541 21.295 90.00 97.47 90.00 Volume: 3820.80 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 13542 13561 13535 13559 20319 18020 18076 27069 N (int>3sigma) = 0 5179 4832 5095 4984 7553 6662 6711 10089 Mean intensity = 0.0 102.5 81.6 98.8 88.6 94.3 98.4 97.2 96.4 Mean int/sigma = 0.0 3.8 3.5 3.6 3.6 3.6 3.7 3.7 3.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.873 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 29 380 365 345 N I>3s 0 135 133 2 9.2 362.4 377.3 7.3 0.6 4.5 4.7 0.6 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)/n # 14 centro 1 19410 0.108 5406 0.6 / 3.7 4.18 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2010src0401.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.15 430 443 97.1 7.49 330.9 21.47 0.0547 0.0310 2.15 - 1.70 444 444 100.0 5.93 176.5 16.21 0.0776 0.0468 1.70 - 1.47 458 459 99.8 4.72 115.5 11.63 0.0961 0.0677 1.47 - 1.34 444 446 99.6 4.25 70.8 8.34 0.1247 0.1017 1.34 - 1.24 428 430 99.5 3.94 63.1 7.35 0.1475 0.1179 1.24 - 1.17 449 450 99.8 3.64 47.2 5.48 0.1839 0.1585 1.17 - 1.11 447 451 99.1 3.14 44.5 4.68 0.1904 0.1908 1.11 - 1.06 434 441 98.4 2.86 39.7 3.75 0.2262 0.2305 1.06 - 1.02 452 460 98.3 2.63 35.6 3.32 0.2491 0.2769 1.02 - 0.98 498 513 97.1 2.42 28.1 2.56 0.3066 0.3653 0.98 - 0.94 561 579 96.9 2.33 28.2 2.38 0.3229 0.3932 0.94 - 0.91 510 538 94.8 2.14 24.5 1.92 0.3686 0.4778 0.91 - 0.88 553 610 90.7 2.02 23.3 1.81 0.3731 0.5355 0.88 - 0.85 609 668 91.2 1.90 19.9 1.39 0.5113 0.6758 0.85 - 0.83 443 497 89.1 1.86 20.6 1.40 0.5140 0.6719 0.83 - 0.81 498 584 85.3 1.65 14.6 0.96 0.5945 1.0049 0.81 - 0.79 540 659 81.9 1.61 15.5 0.98 0.6593 0.9609 0.79 - 0.77 336 465 72.3 1.39 13.1 0.83 0.6657 1.1789 ------------------------------------------------------------------------------ 0.86 - 0.77 2224 2647 84.0 1.67 16.6 1.10 0.5868 0.8718 Inf - 0.77 8534 9137 93.4 2.96 58.9 5.11 0.1159 0.1844 Merged [A], lowest resolution = 7.01 Angstroms, 212 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2010src0401.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C18H16N2O3SFe Formula weight = 396.24 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.378, non-H atomic volume = 19.1 and following cell contents and analysis: C 144.00 54.56 % H 128.00 4.07 % N 16.00 7.07 % O 24.00 12.11 % S 8.00 8.09 % Fe 8.00 14.09 % F(000) = 1632.0 Mo-K(alpha) radiation Mu (mm-1) = 0.92 ------------------------------------------------------------------------------- File 2010src0401.ins set up as follows: TITL 2010src0401 in P2(1)/n CELL 0.71073 7.3738 24.5405 21.2954 90.000 97.475 90.000 ZERR 8.00 0.0004 0.0019 0.0016 0.000 0.004 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O S FE UNIT 144 128 16 24 8 8 TEMP 0.02 TREF HKLF 4 END 27069 Reflections written to new reflection file 2010src0401.hkl -------------------------------------------------------------------------------