++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh086 started at 15:42:27 on 05-Mar-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 4.562 9.537 14.752 90.00 90.00 90.00 12892 Reflections read from file 2008lsh086.hkl; mean (I/sigma) = 10.44 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6414 6476 6438 6447 9664 8590 8581 12892 N (int>3sigma) = 0 5868 6032 5896 5964 8898 7987 7979 11989 Mean intensity = 0.0 63.1 62.5 62.4 61.8 62.7 62.1 62.4 62.2 Mean int/sigma = 0.0 10.3 10.4 10.3 10.4 10.3 10.4 10.4 10.5 Lattice type: P chosen Volume: 641.81 ------------------------------------------------------------------------------- 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: 4.562 9.537 14.752 90.00 90.00 90.00 Niggli form: a.a = 20.81 b.b = 90.95 c.c = 217.61 b.c = 0.00 a.c = 0.00 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. ORTHORHOMBIC P-lattice R(sym) = 0.022 [ 1941] Cell: 4.562 9.537 14.752 90.00 90.00 90.00 Volume: 641.81 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 6414 6476 6438 6447 9664 8590 8581 12892 N (int>3sigma) = 0 5868 6032 5896 5964 8898 7987 7979 11989 Mean intensity = 0.0 63.1 62.5 62.4 61.8 62.7 62.1 62.4 62.2 Mean int/sigma = 0.0 10.3 10.4 10.3 10.4 10.3 10.4 10.4 10.5 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.652 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 951 960 949 8 372 364 380 30 246 244 248 49 N I>3s 738 775 729 4 281 304 285 0 197 173 186 0 93.4 95.9 91.1 2.7 43.2 91.1 85.2 0.3 68.9 54.4 66.7 0.2 10.0 10.2 10.1 5.6 8.3 10.2 9.2 0.5 8.3 7.3 7.1 0.4 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)2(1)2 # 18 chiral 3 359 0.022 1941 0.5 / 5.6 2.85 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh086.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 46 51 90.2 12.08 204.0 50.38 0.0315 0.0190 2.20 - 1.75 49 49 100.0 16.04 156.2 61.69 0.0333 0.0148 1.75 - 1.50 46 46 100.0 17.54 113.1 65.20 0.0339 0.0141 1.50 - 1.35 50 50 100.0 17.78 79.2 60.23 0.0372 0.0147 1.35 - 1.20 67 67 100.0 18.84 74.0 54.66 0.0379 0.0164 1.20 - 1.10 77 77 100.0 17.94 58.7 46.27 0.0526 0.0190 1.10 - 1.05 49 49 100.0 18.24 47.1 40.65 0.0560 0.0233 1.05 - 1.00 59 59 100.0 18.25 35.8 37.85 0.0572 0.0221 1.00 - 0.95 61 61 100.0 17.51 34.2 34.56 0.0642 0.0264 0.95 - 0.90 78 78 100.0 14.64 28.9 28.33 0.0684 0.0307 0.90 - 0.85 113 113 100.0 11.74 22.2 24.09 0.0756 0.0372 0.85 - 0.80 121 121 100.0 8.92 19.7 18.89 0.0793 0.0460 0.80 - 0.77 87 87 100.0 6.48 11.9 12.62 0.0998 0.0632 ------------------------------------------------------------------------------ 0.90 - 0.77 321 321 100.0 9.25 18.4 19.02 0.0798 0.0453 Inf - 0.77 903 908 99.4 14.20 55.8 36.79 0.0446 0.0215 Merged [A], lowest resolution = 5.83 Angstroms, 670 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh086.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C7 H7 Br1 N2 O1 Formula weight = 215.06 Tentative Z (number of formula units/cell) = 3.0 giving rho = 1.669, non-H atomic volume = 19.4 and following cell contents and analysis: C 21.00 39.09 % H 21.00 3.28 % N 6.00 13.03 % O 3.00 7.44 % Br 3.00 37.16 % F(000) = 318.0 Mo-K(alpha) radiation Mu (mm-1) = 4.75 ------------------------------------------------------------------------------- File p21212.ins set up as follows: TITL p21212 in P2(1)2(1)2 CELL 0.71073 9.5368 14.7516 4.5621 90.000 90.000 90.000 ZERR 3.00 0.0002 0.0004 0.0001 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, Z SYMM 0.5-X, 0.5+Y, -Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O BR UNIT 21 21 6 3 3 TEMP file. TREF HKLF 4 END 12892 Reflections written to new reflection file p21212.hkl -------------------------------------------------------------------------------