+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2008/2 for Windows + + Copyright(C) 2008 Bruker-AXS All Rights Reserved + + 2008lsh071 started at 19:16:32 on 21-Oct-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 17.540 13.763 7.772 90.00 101.88 90.00 14404 Reflections read from file 2008lsh071.hkl; mean (I/sigma) = 9.32 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7191 7191 0 7212 7191 9624 9617 14404 N (int>3sigma) = 0 4915 4915 0 4918 4915 6661 6614 9985 Mean intensity = 0.0 21.9 21.9 0.0 20.1 21.9 21.0 20.1 20.4 Mean int/sigma = 0.0 9.4 9.4 0.0 9.2 9.4 9.4 9.3 9.4 Lattice type: C chosen Volume: 1835.98 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 1.0000 -0.5000 0.5000 0.0000 -0.5000 -0.5000 0.0000 Unitcell: 7.772 11.148 11.148 76.24 80.68 80.68 Niggli form: a.a = 60.40 b.b = 124.27 c.c = 124.27 b.c = 29.56 a.c = 14.03 a.b = 14.03 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC C-lattice R(sym) = 0.021 [ 1995] Cell: 17.540 13.763 7.772 90.00 101.88 90.00 Volume: 1835.98 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 7191 7191 0 7212 7191 9624 9617 14404 N (int>3sigma) = 0 4915 4915 0 4918 4915 6661 6614 9985 Mean intensity = 0.0 21.9 21.9 0.0 20.1 21.9 21.0 20.1 20.4 Mean int/sigma = 0.0 9.4 9.4 0.0 9.2 9.4 9.4 9.3 9.4 Crystal system M and Lattice type C selected Mean |E*E-1| = 1.066 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 338 N I>3s 1 0.1 0.5 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/c # 15 centro 1 3696 0.021 1995 0.5 / 9.4 2.11 [B] Cc # 9 non-cen 1 566 0.021 1995 0.5 / 9.4 12.19 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh071.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.13 111 116 95.7 7.85 66.5 54.20 0.0268 0.0154 2.13 - 1.69 113 113 100.0 8.70 59.4 53.55 0.0251 0.0149 1.69 - 1.46 114 115 99.1 8.70 25.8 44.00 0.0315 0.0151 1.46 - 1.32 115 115 100.0 8.92 12.5 33.60 0.0455 0.0200 1.32 - 1.22 127 127 100.0 8.62 28.0 30.31 0.0327 0.0200 1.22 - 1.14 120 120 100.0 8.69 27.8 31.50 0.0358 0.0196 1.14 - 1.08 136 136 100.0 8.77 20.8 26.62 0.0417 0.0239 1.08 - 1.03 120 120 100.0 8.48 13.9 24.21 0.0531 0.0266 1.03 - 0.98 145 145 100.0 7.66 14.5 20.83 0.0518 0.0289 0.98 - 0.95 113 113 100.0 6.81 8.2 16.63 0.0645 0.0396 0.95 - 0.92 130 130 100.0 6.35 7.1 13.54 0.0835 0.0462 0.92 - 0.89 133 133 100.0 5.71 8.4 12.62 0.0796 0.0498 0.89 - 0.86 164 164 100.0 4.48 6.3 9.02 0.1098 0.0703 0.86 - 0.84 116 116 100.0 3.95 4.9 8.73 0.1097 0.0807 0.84 - 0.82 136 136 100.0 3.65 5.0 7.41 0.1042 0.0836 0.82 - 0.80 138 138 100.0 3.28 4.3 6.10 0.1117 0.1056 0.80 - 0.78 155 155 100.0 3.34 4.0 6.29 0.1167 0.1094 0.78 - 0.77 7 14 50.0 0.86 7.7 6.17 0.1288 0.1193 ------------------------------------------------------------------------------ 0.87 - 0.77 670 677 99.0 3.61 4.8 7.30 0.1103 0.0911 Inf - 0.77 2193 2206 99.4 6.53 17.5 22.25 0.0398 0.0271 Merged [A], lowest resolution = 6.88 Angstroms, 501 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh071.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C10H11N1O3 Formula weight = 193.20 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.398, non-H atomic volume = 16.4 and following cell contents and analysis: C 80.00 62.17 % H 88.00 5.74 % N 8.00 7.25 % O 24.00 24.84 % F(000) = 816.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File 2008lsh071.ins set up as follows: TITL 2008lsh071 in C2/c CELL 0.71073 17.5403 13.7630 7.7717 90.000 101.876 90.000 ZERR 8.00 0.0005 0.0003 0.0002 0.000 0.001 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O UNIT 80 88 8 24 TEMP 0.3 TREF HKLF 4 END -------------------------------------------------------------------------------