++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh018 started at 14:27:03 on 05-Jul-2008 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.280 9.382 20.744 90.00 90.00 90.00 14951 Reflections read from file 2008lsh018.hkl; mean (I/sigma) = 10.30 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7442 7461 7445 7456 11174 9966 9954 14951 N (int>3sigma) = 0 5068 5052 5060 5092 7590 6993 6997 10451 Mean intensity = 0.0 375.0 313.9 381.1 370.4 356.6 375.9 375.2 370.4 Mean int/sigma = 0.0 10.1 9.9 10.4 10.2 10.1 10.4 10.4 10.4 Lattice type: P chosen Volume: 1806.10 ------------------------------------------------------------------------------- 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: 9.280 9.382 20.744 90.00 90.00 90.00 Niggli form: a.a = 86.13 b.b = 88.02 c.c = 430.30 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 = 0.312 deg. TETRAGONAL P-lattice R(sym) = 0.662 [ 4654] Cell: 9.280 9.382 20.744 90.00 90.00 90.00 Volume: 1806.10 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. ORTHORHOMBIC P-lattice R(sym) = 0.024 [ 4424] Cell: 9.280 9.382 20.744 90.00 90.00 90.00 Volume: 1806.10 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 7442 7461 7445 7456 11174 9966 9954 14951 N (int>3sigma) = 0 5068 5052 5060 5092 7590 6993 6997 10451 Mean intensity = 0.0 375.0 313.9 381.1 370.4 356.6 375.9 375.2 370.4 Mean int/sigma = 0.0 10.1 9.9 10.4 10.2 10.1 10.4 10.4 10.4 Crystal system O and Lattice type P selected Mean |E*E-1| = 1.076 [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 487 460 487 16 523 490 501 12 263 248 263 17 N I>3s 233 1 234 0 247 2 249 0 119 0 119 0 787.1 3.9 787.9 2.6 521.6 2.7 544.5 2.7 105.0 2.5 104.9 14.0 9.1 0.7 9.2 0.7 8.0 0.6 8.3 0.7 6.7 0.6 6.7 1.4 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] Pbca # 61 centro 2 2293 0.024 4424 1.4 / 6.7 2.86 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh018.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 121 133 91.0 6.73 1133.1 35.78 0.0196 0.0227 2.20 - 1.70 135 135 100.0 8.71 1020.0 44.54 0.0214 0.0170 1.70 - 1.45 138 138 100.0 9.03 566.6 42.66 0.0270 0.0172 1.45 - 1.30 141 141 100.0 9.15 464.4 38.51 0.0281 0.0170 1.30 - 1.20 134 134 100.0 9.54 410.2 36.38 0.0337 0.0189 1.20 - 1.10 194 194 100.0 8.81 360.9 33.26 0.0366 0.0208 1.10 - 1.00 271 271 100.0 7.43 198.1 23.24 0.0480 0.0270 1.00 - 0.95 160 160 100.0 6.64 161.1 19.14 0.0569 0.0309 0.95 - 0.90 238 238 100.0 5.82 161.3 16.92 0.0619 0.0379 0.90 - 0.85 263 264 99.6 4.48 101.5 11.61 0.0820 0.0557 0.85 - 0.80 338 339 99.7 3.41 76.6 8.56 0.0906 0.0795 0.80 - 0.77 239 254 94.1 2.20 64.8 5.72 0.1045 0.1209 ------------------------------------------------------------------------------ 0.90 - 0.77 840 857 98.0 3.38 81.0 8.71 0.0883 0.0796 Inf - 0.77 2372 2401 98.8 6.23 307.5 22.64 0.0335 0.0268 Merged [A], lowest resolution = 6.92 Angstroms, 403 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh018.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C9H10Br1N1O1 Formula weight = 228.09 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.678, non-H atomic volume = 18.8 and following cell contents and analysis: C 72.00 47.39 % H 80.00 4.42 % N 8.00 6.14 % O 8.00 7.01 % Br 8.00 35.03 % F(000) = 912.0 Mo-K(alpha) radiation Mu (mm-1) = 4.50 ------------------------------------------------------------------------------- File Pbca.ins set up as follows: TITL Pbca in Pbca CELL 0.71073 9.3819 9.2804 20.7436 90.000 90.000 90.000 ZERR 8.00 0.0002 0.0002 0.0005 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O BR UNIT 72 80 8 8 8 TEMP 0.1 TREF HKLF 4 END -------------------------------------------------------------------------------