++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh144 started at 12:05:51 on 06-Mar-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 4.666 11.569 11.577 90.00 90.00 90.00 7284 Reflections read from file 2008lsh144.hkl; mean (I/sigma) = 11.90 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3649 3615 3632 3651 5448 4855 4854 7284 N (int>3sigma) = 0 3379 3412 3373 3354 5082 4503 4502 6764 Mean intensity = 0.0 53.9 55.1 54.2 52.4 54.4 54.0 53.5 53.3 Mean int/sigma = 0.0 11.9 12.0 11.9 11.9 12.0 11.9 11.9 11.9 Lattice type: P chosen Volume: 624.98 ------------------------------------------------------------------------------- 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: 4.666 11.569 11.577 90.00 90.00 90.00 Niggli form: a.a = 21.77 b.b = 133.84 c.c = 134.03 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 = 0.020 deg. TETRAGONAL P-lattice R(sym) = 0.445 [ 1875] Cell: 11.569 11.577 4.666 90.00 90.00 90.00 Volume: 624.98 Matrix: 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(sym) = 0.029 [ 1798] Cell: 4.666 11.569 11.577 90.00 90.00 90.00 Volume: 624.98 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 3649 3615 3632 3651 5448 4855 4854 7284 N (int>3sigma) = 0 3379 3412 3373 3354 5082 4503 4502 6764 Mean intensity = 0.0 53.9 55.1 54.2 52.4 54.4 54.0 53.5 53.3 Mean int/sigma = 0.0 11.9 12.0 11.9 11.9 12.0 11.9 11.9 11.9 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.654 [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 468 453 461 7 213 222 211 14 193 180 177 20 N I>3s 410 404 378 7 174 201 169 0 177 154 149 0 86.4 82.1 74.6 60.2 43.7 63.6 71.6 0.6 71.0 44.7 73.8 0.4 13.7 14.4 12.6 12.1 10.1 11.7 11.2 0.7 11.7 11.6 10.9 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] P2(1)2(1)2 # 18 chiral 3 359 0.029 1798 0.7 / 10.1 1.96 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh144.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.25 49 52 94.2 8.52 185.6 49.42 0.0255 0.0200 2.25 - 1.75 45 45 100.0 12.04 121.4 64.72 0.0321 0.0151 1.75 - 1.50 47 47 100.0 11.89 71.6 54.64 0.0432 0.0164 1.50 - 1.35 47 47 100.0 12.00 68.4 52.26 0.0424 0.0164 1.35 - 1.20 71 71 100.0 12.62 48.7 45.52 0.0492 0.0199 1.20 - 1.10 73 73 100.0 10.27 46.5 38.42 0.0506 0.0230 1.10 - 1.00 93 93 100.0 9.67 26.9 31.09 0.0644 0.0281 1.00 - 0.95 60 60 100.0 8.57 29.3 27.98 0.0667 0.0330 0.95 - 0.90 84 84 100.0 7.58 22.2 23.13 0.0756 0.0392 0.90 - 0.85 106 106 100.0 5.84 18.5 18.69 0.0796 0.0484 0.85 - 0.80 120 120 100.0 4.65 11.8 12.84 0.0915 0.0694 0.80 - 0.77 85 85 100.0 3.56 10.9 11.55 0.0921 0.0854 ------------------------------------------------------------------------------ 0.90 - 0.77 311 311 100.0 4.76 13.8 14.48 0.0852 0.0633 Inf - 0.77 880 883 99.7 8.25 43.7 31.15 0.0446 0.0258 Merged [A], lowest resolution = 5.79 Angstroms, 236 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh144.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8 H8 Br1 N1 O2 Formula weight = 230.06 Tentative Z (number of formula units/cell) = 3.0 giving rho = 1.834, non-H atomic volume = 17.4 and following cell contents and analysis: C 24.00 41.76 % H 24.00 3.51 % N 3.00 6.09 % O 6.00 13.91 % Br 3.00 34.73 % F(000) = 342.0 Mo-K(alpha) radiation Mu (mm-1) = 4.89 ------------------------------------------------------------------------------- File p21212.ins set up as follows: TITL p21212 in P2(1)2(1)2 CELL 0.71073 11.5691 11.5772 4.6662 90.000 90.000 90.000 ZERR 3.00 0.0004 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 24 24 3 6 3 TEMP file. TREF HKLF 4 END 7284 Reflections written to new reflection file p21212.hkl -------------------------------------------------------------------------------