++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh052 started at 18:31:59 on 10-Nov-2010 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 4.781 11.934 14.686 90.00 96.82 90.00 11305 Reflections read from file 2008lsh052.hkl; mean (I/sigma) = 11.60 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5649 5642 5639 5653 8465 7529 7545 11305 N (int>3sigma) = 0 4481 4289 4402 4281 6586 5885 5890 8820 Mean intensity = 0.0 45.7 44.0 45.7 44.1 45.1 44.7 45.0 44.7 Mean int/sigma = 0.0 12.1 11.5 11.7 11.5 11.8 11.8 11.6 11.7 Lattice type: P chosen Volume: 831.99 ------------------------------------------------------------------------------- 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: 4.781 11.934 14.686 90.00 96.82 90.00 Niggli form: a.a = 22.86 b.b = 142.43 c.c = 215.68 b.c = 0.00 a.c = -8.34 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) = 0.020 [ 1711] Cell: 4.781 11.934 14.686 90.00 96.82 90.00 Volume: 831.99 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 5649 5642 5639 5653 8465 7529 7545 11305 N (int>3sigma) = 0 4481 4289 4402 4281 6586 5885 5890 8820 Mean intensity = 0.0 45.7 44.0 45.7 44.1 45.1 44.7 45.0 44.7 Mean int/sigma = 0.0 12.1 11.5 11.7 11.5 11.8 11.8 11.6 11.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.941 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 20 365 355 358 N I>3s 1 165 166 1 0.5 51.0 52.4 0.3 0.7 8.2 8.4 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] P2(1)/n # 14 centro 1 19410 0.020 1711 0.7 / 8.2 1.38 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh052.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.10 104 108 96.3 6.69 135.2 50.82 0.0207 0.0159 2.10 - 1.65 106 106 100.0 7.38 89.8 59.57 0.0238 0.0131 1.65 - 1.45 102 102 100.0 7.45 68.3 46.33 0.0284 0.0149 1.45 - 1.30 122 122 100.0 7.65 54.2 46.53 0.0320 0.0159 1.30 - 1.20 102 102 100.0 7.57 56.2 40.09 0.0336 0.0181 1.20 - 1.10 172 172 100.0 7.40 42.8 31.97 0.0355 0.0231 1.10 - 1.05 104 104 100.0 7.42 25.9 23.91 0.0517 0.0276 1.05 - 1.00 110 110 100.0 7.47 28.8 25.10 0.0468 0.0290 1.00 - 0.95 149 150 99.3 6.03 27.8 21.20 0.0495 0.0340 0.95 - 0.90 198 198 100.0 5.27 23.5 17.31 0.0573 0.0409 0.90 - 0.85 232 232 100.0 4.36 17.8 13.94 0.0753 0.0522 0.85 - 0.80 273 273 100.0 3.31 14.0 10.31 0.0807 0.0711 0.80 - 0.77 220 244 90.2 2.48 11.3 7.78 0.0908 0.0963 ------------------------------------------------------------------------------ 0.90 - 0.77 725 749 96.8 3.37 14.4 10.71 0.0798 0.0696 Inf - 0.77 1994 2023 98.6 5.59 37.8 25.67 0.0360 0.0273 Merged [A], lowest resolution = 6.22 Angstroms, 395 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh052.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H8Br1N1O1 Formula weight = 214.06 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.709, non-H atomic volume = 18.9 and following cell contents and analysis: C 32.00 44.88 % H 32.00 3.77 % N 4.00 6.54 % O 4.00 7.47 % Br 4.00 37.33 % F(000) = 424.0 Mo-K(alpha) radiation Mu (mm-1) = 4.88 ------------------------------------------------------------------------------- File 2008lsh052.ins set up as follows: TITL 2008lsh052 in P2(1)/n CELL 0.71073 4.7808 11.9344 14.6859 90.000 96.820 90.000 ZERR 4.00 0.0001 0.0005 0.0005 0.000 0.002 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O BR UNIT 32 32 4 4 4 TEMP 0.04 TREF HKLF 4 END -------------------------------------------------------------------------------