++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh168 started at 11:26:45 on 15-Jan-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 18.336 5.002 19.855 90.00 108.65 90.00 20190 Reflections read from file 2008lsh168.hkl; mean (I/sigma) = 3.66 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 10147 10098 10111 10098 15178 13500 13447 20190 N (int>3sigma) = 0 4962 4831 4651 4829 7222 6558 6480 9809 Mean intensity = 0.0 17.2 17.1 16.7 17.1 17.0 16.6 16.6 16.9 Mean int/sigma = 0.0 3.8 3.7 3.6 3.7 3.7 3.8 3.8 3.8 Lattice type: P chosen Volume: 1725.36 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 5.002 18.336 19.855 108.65 90.00 90.00 Niggli form: a.a = 25.02 b.b = 336.21 c.c = 394.22 b.c = -116.45 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. MONOCLINIC P-lattice R(sym) = 0.059 [ 2916] Cell: 18.336 5.002 19.855 90.00 108.65 90.00 Volume: 1725.36 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 10147 10098 10111 10098 15178 13500 13447 20190 N (int>3sigma) = 0 4962 4831 4651 4829 7222 6558 6480 9809 Mean intensity = 0.0 17.2 17.1 16.7 17.1 17.0 16.6 16.6 16.9 Mean int/sigma = 0.0 3.8 3.7 3.6 3.7 3.7 3.8 3.8 3.8 Crystal system M and Lattice type P selected Mean |E*E-1| = 1.012 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 8 1478 1437 1439 N I>3s 0 2 541 543 0.2 0.4 28.6 28.6 0.6 0.5 3.2 3.2 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)/c # 14 centro 4 19410 0.059 2916 0.6 / 3.2 3.94 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh168.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.15 231 248 93.1 4.65 86.8 14.32 0.0577 0.0551 2.15 - 1.65 248 248 100.0 5.67 48.5 15.63 0.0624 0.0463 1.65 - 1.45 236 236 100.0 5.73 28.8 14.02 0.0755 0.0492 1.45 - 1.30 250 250 100.0 5.98 22.9 12.94 0.0884 0.0522 1.30 - 1.20 252 252 100.0 6.17 16.8 11.24 0.1112 0.0591 1.20 - 1.10 363 363 100.0 6.12 11.5 9.89 0.1284 0.0668 1.10 - 1.00 458 458 100.0 6.09 8.6 8.49 0.1473 0.0790 1.00 - 0.95 352 359 98.1 5.30 5.4 6.99 0.1946 0.1108 0.95 - 0.90 405 413 98.1 4.46 4.5 5.25 0.2244 0.1391 0.90 - 0.85 480 487 98.6 3.47 3.5 3.79 0.2492 0.1947 0.85 - 0.80 620 637 97.3 2.70 2.2 2.35 0.3862 0.3485 0.80 - 0.77 463 498 93.0 2.14 1.6 1.67 0.5086 0.5077 ------------------------------------------------------------------------------ 0.90 - 0.77 1563 1622 96.4 2.76 2.4 2.59 0.3286 0.3126 Inf - 0.77 4358 4449 98.0 4.54 14.8 7.50 0.0952 0.0741 Merged [A], lowest resolution = 5.79 Angstroms, 587 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh168.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H8Br1N1O1 Formula weight = 214.06 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.648, non-H atomic volume = 19.6 and following cell contents and analysis: C 64.00 44.88 % H 64.00 3.77 % N 8.00 6.54 % O 8.00 7.47 % Br 8.00 37.33 % F(000) = 848.0 Mo-K(alpha) radiation Mu (mm-1) = 4.71 ------------------------------------------------------------------------------- File p21c.ins set up as follows: TITL p21c in P2(1)/c CELL 0.71073 19.8550 5.0020 18.3360 90.000 108.655 90.000 ZERR 8.00 0.0015 0.0005 0.0016 0.000 0.004 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O BR UNIT 64 64 8 8 8 TEMP 0.06 TREF HKLF 4 END 20190 Reflections written to new reflection file p21c.hkl -------------------------------------------------------------------------------