++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2009lsh008 started at 18:40:11 on 02-Mar-2009 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.425 10.517 16.266 90.00 90.00 90.00 12449 Reflections read from file 2009lsh008.hkl; mean (I/sigma) = 9.07 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6217 6208 6225 6243 9325 8308 8275 12449 N (int>3sigma) = 0 3909 3799 4086 4046 5897 5473 5461 8183 Mean intensity = 0.0 14.9 13.0 14.4 15.1 14.1 14.7 14.7 15.1 Mean int/sigma = 0.0 9.1 8.6 9.3 9.0 9.0 9.1 9.1 9.1 Lattice type: P chosen Volume: 1612.39 ------------------------------------------------------------------------------- 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: 9.425 10.517 16.266 90.00 90.00 90.00 Niggli form: a.a = 88.83 b.b = 110.62 c.c = 264.57 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) = 0.034 [ 4769] Cell: 9.425 10.517 16.266 90.00 90.00 90.00 Volume: 1612.39 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 6217 6208 6225 6243 9325 8308 8275 12449 N (int>3sigma) = 0 3909 3799 4086 4046 5897 5473 5461 8183 Mean intensity = 0.0 14.9 13.0 14.4 15.1 14.1 14.7 14.7 15.1 Mean int/sigma = 0.0 9.1 8.6 9.3 9.0 9.0 9.1 9.1 9.1 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.985 [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 425 425 428 9 330 336 324 11 213 205 214 16 N I>3s 169 4 169 0 108 0 108 1 78 4 82 0 21.2 0.2 21.1 0.4 14.9 0.2 15.1 0.2 17.1 0.3 17.1 0.2 6.6 0.6 6.6 0.8 6.7 0.6 6.8 1.1 7.4 0.9 7.5 0.6 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 0.034 4769 1.1 / 6.6 1.80 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2009lsh008.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 111 120 92.5 5.83 74.3 40.27 0.0237 0.0186 2.20 - 1.70 117 117 100.0 7.19 31.8 46.38 0.0262 0.0139 1.70 - 1.45 127 127 100.0 7.58 24.3 36.80 0.0348 0.0170 1.45 - 1.30 127 127 100.0 7.69 13.2 29.75 0.0479 0.0228 1.30 - 1.20 119 119 100.0 7.87 15.0 27.32 0.0447 0.0222 1.20 - 1.10 173 173 100.0 7.72 16.5 28.38 0.0442 0.0231 1.10 - 1.00 235 235 100.0 7.64 8.7 19.62 0.0646 0.0344 1.00 - 0.95 158 159 99.4 6.48 6.9 17.03 0.0754 0.0432 0.95 - 0.90 198 198 100.0 5.78 5.7 13.03 0.0841 0.0530 0.90 - 0.85 244 247 98.8 4.33 5.1 10.43 0.1048 0.0700 0.85 - 0.80 297 302 98.3 3.35 4.1 7.73 0.1129 0.0973 0.80 - 0.77 221 222 99.5 2.90 2.8 5.63 0.1525 0.1488 ------------------------------------------------------------------------------ 0.90 - 0.77 762 771 98.8 3.53 4.0 7.99 0.1151 0.0964 Inf - 0.77 2127 2146 99.1 5.80 13.5 19.97 0.0442 0.0305 Merged [A], lowest resolution = 6.44 Angstroms, 371 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2009lsh008.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H8Cl1N1O1 Formula weight = 169.60 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.397, non-H atomic volume = 18.3 and following cell contents and analysis: C 64.00 56.65 % H 64.00 4.75 % N 8.00 8.26 % O 8.00 9.43 % Cl 8.00 20.90 % F(000) = 704.0 Mo-K(alpha) radiation Mu (mm-1) = 0.41 ------------------------------------------------------------------------------- File pbca.ins set up as follows: TITL pbca in Pbca CELL 0.71073 10.5174 9.4252 16.2656 90.000 90.000 90.000 ZERR 8.00 0.0002 0.0004 0.0006 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 CL UNIT 64 64 8 8 8 TEMP 0.08 TREF HKLF 4 END 12449 Reflections written to new reflection file pbca.hkl -------------------------------------------------------------------------------