+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2008/2 for Windows + + Copyright(C) 2008 Bruker-AXS All Rights Reserved + + 2010src0792r started at 09:54:26 on 19-Aug-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 19.623 4.071 32.979 90.00 101.70 90.00 10009 Reflections read from file 2010src0792r.hkl; mean (I/sigma) = 5.30 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4981 4981 0 4978 4981 6707 6672 10009 N (int>3sigma) = 0 2370 2370 0 2600 2370 3768 3696 5554 Mean intensity = 0.0 186.5 186.5 0.0 311.0 186.5 321.0 314.7 321.8 Mean int/sigma = 0.0 4.4 4.4 0.0 5.2 4.4 5.5 5.4 5.4 Lattice type: C chosen Volume: 2579.83 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 Unitcell: 4.071 10.020 32.509 83.87 86.41 78.28 Niggli form: a.a = 16.57 b.b = 100.41 c.c = 1056.84 b.c = 34.80 a.c = 8.29 a.b = 8.29 ------------------------------------------------------------------------------- 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) = 0.051 [ 1639] Cell: 19.623 4.071 32.979 90.00 101.70 90.00 Volume: 2579.83 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 4981 4981 0 4978 4981 6707 6672 10009 N (int>3sigma) = 0 2370 2370 0 2600 2370 3768 3696 5554 Mean intensity = 0.0 186.5 186.5 0.0 311.0 186.5 321.0 314.7 321.8 Mean int/sigma = 0.0 4.4 4.4 0.0 5.2 4.4 5.5 5.4 5.4 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.852 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 905 N I>3s 4 12.0 0.7 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 0.051 1639 0.7 / 5.4 3.49 [B] Cc # 9 non-cen 1 566 0.051 1639 0.7 / 5.4 3.62 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2010src0792r.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.21 166 176 94.3 4.11 1119.5 19.16 0.0342 0.0334 2.21 - 1.74 168 169 99.4 4.44 700.7 20.04 0.0490 0.0383 1.74 - 1.51 168 170 98.8 4.23 478.6 15.80 0.0584 0.0430 1.51 - 1.35 181 184 98.4 3.91 369.1 15.11 0.0657 0.0509 1.35 - 1.25 173 174 99.4 3.79 321.6 13.42 0.0722 0.0563 1.25 - 1.17 182 182 100.0 3.40 264.8 11.25 0.0786 0.0684 1.17 - 1.10 195 196 99.5 3.32 198.2 8.95 0.0981 0.0856 1.10 - 1.05 170 174 97.7 2.95 199.0 7.97 0.1016 0.0961 1.05 - 1.00 205 212 96.7 2.79 166.3 7.15 0.1134 0.1106 1.00 - 0.97 166 171 97.1 2.67 138.4 5.68 0.1372 0.1338 0.97 - 0.94 172 175 98.3 2.61 109.1 4.91 0.1558 0.1641 0.94 - 0.91 179 186 96.2 2.54 102.9 5.01 0.1535 0.1692 0.91 - 0.88 221 224 98.7 2.42 85.4 3.96 0.1831 0.2178 0.88 - 0.85 228 232 98.3 2.31 89.9 3.86 0.1776 0.2177 0.85 - 0.82 277 285 97.2 2.28 68.4 2.97 0.2483 0.2934 0.82 - 0.80 214 224 95.5 2.08 51.7 2.18 0.3140 0.4243 0.80 - 0.78 224 243 92.2 1.95 51.8 2.14 0.3352 0.4376 0.78 - 0.77 9 22 40.9 0.45 99.0 2.33 2.6897 0.3897 ------------------------------------------------------------------------------ 0.86 - 0.77 867 920 94.2 2.10 62.0 2.65 0.2635 0.3435 Inf - 0.77 3298 3399 97.0 2.94 243.5 8.22 0.0722 0.0845 Merged [A], lowest resolution = 6.91 Angstroms, 112 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2010src0792r.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C15H10Br1N1O1 Formula weight = 300.15 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.546, non-H atomic volume = 17.9 and following cell contents and analysis: C 120.00 60.02 % H 80.00 3.36 % N 8.00 4.67 % O 8.00 5.33 % Br 8.00 26.62 % F(000) = 1200.0 Mo-K(alpha) radiation Mu (mm-1) = 3.17 ------------------------------------------------------------------------------- File 2010src0792ra.ins set up as follows: TITL 2010src0792ra in C2/c CELL 0.71073 19.6228 4.0710 32.9795 90.000 101.698 90.000 ZERR 8.00 0.0026 0.0005 0.0044 0.000 0.003 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O BR UNIT 120 80 8 8 8 TEMP 0.02 TREF HKLF 4 END 10009 Reflections written to new reflection file 2010src0792ra.hkl -------------------------------------------------------------------------------