+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2008/2 for Windows + + Copyright(C) 2008 Bruker-AXS All Rights Reserved + + 2008lsh076 started at 17:17:00 on 21-Oct-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 4.797 12.498 14.679 90.00 98.34 90.00 11493 Reflections read from file 2008lsh076.hkl; mean (I/sigma) = 17.64 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5704 5706 5742 5749 8576 7696 7649 11493 N (int>3sigma) = 0 5105 5046 5149 5101 7650 6948 6840 10330 Mean intensity = 0.0 83.5 82.5 82.0 81.7 82.6 83.0 82.2 82.4 Mean int/sigma = 0.0 17.8 17.5 17.7 17.6 17.7 17.8 17.7 17.7 Lattice type: P chosen Volume: 870.71 ------------------------------------------------------------------------------- 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: 4.797 12.498 14.679 90.00 98.34 90.00 Niggli form: a.a = 23.01 b.b = 156.19 c.c = 215.47 b.c = 0.00 a.c = -10.21 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. MONOCLINIC P-lattice R(sym) = 0.014 [ 1859] Cell: 4.797 12.498 14.679 90.00 98.34 90.00 Volume: 870.71 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 5704 5706 5742 5749 8576 7696 7649 11493 N (int>3sigma) = 0 5105 5046 5149 5101 7650 6948 6840 10330 Mean intensity = 0.0 83.5 82.5 82.0 81.7 82.6 83.0 82.2 82.4 Mean int/sigma = 0.0 17.8 17.5 17.7 17.6 17.7 17.8 17.7 17.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.878 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 16 264 239 239 N I>3s 1 144 138 24 0.1 78.9 87.1 0.3 0.4 12.0 13.1 1.3 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 0.014 1859 1.3 / 12.0 1.74 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh076.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.09 106 115 92.2 5.92 187.0 64.89 0.0240 0.0151 2.09 - 1.66 107 108 99.1 7.36 171.3 74.96 0.0224 0.0109 1.66 - 1.46 106 107 99.1 6.93 135.9 67.26 0.0210 0.0114 1.46 - 1.33 108 108 100.0 7.41 107.9 61.38 0.0241 0.0118 1.33 - 1.22 106 106 100.0 7.60 120.1 66.12 0.0240 0.0123 1.22 - 1.15 117 117 100.0 7.15 74.7 49.60 0.0285 0.0158 1.15 - 1.09 119 120 99.2 7.30 78.4 48.52 0.0266 0.0155 1.09 - 1.04 112 112 100.0 7.25 57.6 41.51 0.0253 0.0179 1.04 - 0.99 134 134 100.0 6.91 64.8 38.18 0.0285 0.0198 0.99 - 0.95 138 138 100.0 5.49 53.3 31.15 0.0330 0.0249 0.95 - 0.92 116 116 100.0 5.19 42.5 28.97 0.0372 0.0280 0.92 - 0.89 135 135 100.0 4.82 42.9 26.71 0.0381 0.0282 0.89 - 0.87 109 109 100.0 4.03 43.7 24.75 0.0412 0.0323 0.87 - 0.84 154 155 99.4 3.54 31.1 18.94 0.0405 0.0386 0.84 - 0.82 120 120 100.0 3.12 24.6 15.74 0.0383 0.0451 0.82 - 0.80 135 135 100.0 2.90 32.1 16.47 0.0326 0.0485 0.80 - 0.78 166 169 98.2 2.64 27.7 15.02 0.0412 0.0530 0.78 - 0.77 4 8 50.0 0.88 16.9 13.41 0.1334 0.0693 ------------------------------------------------------------------------------ 0.87 - 0.77 636 644 98.8 3.10 29.3 17.27 0.0399 0.0451 Inf - 0.77 2092 2112 99.1 5.44 71.6 38.50 0.0265 0.0197 Merged [A], lowest resolution = 6.28 Angstroms, 435 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh076.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H8I1N1O1 Formula weight = 261.06 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.991, non-H atomic volume = 19.8 and following cell contents and analysis: C 32.00 36.81 % H 32.00 3.09 % N 4.00 5.37 % O 4.00 6.13 % I 4.00 48.61 % F(000) = 496.0 Mo-K(alpha) radiation Mu (mm-1) = 3.62 ------------------------------------------------------------------------------- File 2008lsh076.ins set up as follows: TITL 2008lsh076 in P2(1)/n CELL 0.71073 4.7969 12.4977 14.6790 90.000 98.336 90.000 ZERR 4.00 0.0001 0.0003 0.0003 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O I UNIT 32 32 4 4 4 TEMP 0.2 TREF HKLF 4 END -------------------------------------------------------------------------------