++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh039 started at 22:34:59 on 13-Nov-2010 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 4.908 9.750 18.612 90.00 90.00 90.00 4208 Reflections read from file 2008lsh039.hkl; mean (I/sigma) = 9.04 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 2106 2116 2118 2106 3170 2799 2818 4208 N (int>3sigma) = 0 1850 1865 1895 1879 2805 2502 2510 3761 Mean intensity = 0.0 353.7 349.1 353.6 342.5 352.1 345.0 349.7 347.2 Mean int/sigma = 0.0 9.0 8.9 9.1 9.1 9.0 9.0 9.0 9.1 Lattice type: P chosen Volume: 890.58 ------------------------------------------------------------------------------- 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: 4.908 9.750 18.612 90.00 90.00 90.00 Niggli form: a.a = 24.08 b.b = 95.07 c.c = 346.39 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) = 0.042 [ 1508] Cell: 4.908 9.750 18.612 90.00 90.00 90.00 Volume: 890.58 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 2106 2116 2118 2106 3170 2799 2818 4208 N (int>3sigma) = 0 1850 1865 1895 1879 2805 2502 2510 3761 Mean intensity = 0.0 353.7 349.1 353.6 342.5 352.1 345.0 349.7 347.2 Mean int/sigma = 0.0 9.0 8.9 9.1 9.1 9.0 9.0 9.0 9.1 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 339 344 343 2 129 133 118 7 59 66 61 12 N I>3s 277 267 274 0 101 109 88 1 51 51 50 1 593.8 572.9 541.6 2.3 240.4 499.9 484.0 3.2 555.9 510.0 231.3 3.9 8.6 8.2 8.7 0.7 8.0 8.7 8.3 0.8 9.0 8.3 8.0 0.9 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 0.042 1508 0.9 / 8.0 2.22 [B] P2(1)2(1)2(1) # 19 chiral 1 5917 0.042 1508 0.9 / 8.0 1.96 Option [B] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh039.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.25 59 70 84.3 4.01 1564.8 24.44 0.0549 0.0410 2.25 - 1.70 67 70 95.7 4.96 804.4 25.86 0.0509 0.0378 1.70 - 1.45 77 80 96.3 3.88 516.1 21.39 0.0507 0.0482 1.45 - 1.30 73 74 98.6 4.32 388.2 20.93 0.0466 0.0460 1.30 - 1.20 66 67 98.5 4.09 300.7 19.85 0.0538 0.0474 1.20 - 1.10 100 100 100.0 4.22 229.6 19.39 0.0667 0.0473 1.10 - 1.05 64 67 95.5 3.87 181.9 18.17 0.0695 0.0516 1.05 - 1.00 65 67 97.0 4.54 143.7 19.89 0.0761 0.0454 1.00 - 0.95 96 98 98.0 3.66 124.9 15.96 0.0780 0.0615 0.95 - 0.90 111 112 99.1 3.56 110.9 14.23 0.0779 0.0608 0.90 - 0.85 129 138 93.5 2.84 67.4 11.49 0.0868 0.0768 0.85 - 0.80 151 170 88.8 1.88 52.5 8.03 0.0937 0.1067 0.80 - 0.77 109 138 79.0 1.60 43.9 7.07 0.1142 0.1245 ------------------------------------------------------------------------------ 0.90 - 0.77 389 446 87.2 2.09 55.0 8.91 0.0936 0.0985 Inf - 0.77 1167 1251 93.3 3.36 277.5 15.97 0.0577 0.0484 Merged [A], lowest resolution = 6.73 Angstroms, 90 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh039.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H8I1N1O1 Formula weight = 261.05 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.947, non-H atomic volume = 20.2 and following cell contents and analysis: C 32.00 36.80 % H 32.00 3.09 % N 4.00 5.37 % O 4.00 6.13 % I 4.00 48.61 % F(000) = 496.0 Mo-K(alpha) radiation Mu (mm-1) = 3.54 ------------------------------------------------------------------------------- File 2008lsh039.ins set up as follows: TITL 2008lsh039 in P2(1)2(1)2(1) CELL 0.71073 4.9076 9.7504 18.6116 90.000 90.000 90.000 ZERR 4.00 0.0005 0.0008 0.0011 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 I UNIT 32 32 4 4 4 TEMP 0.02 TREF HKLF 4 END -------------------------------------------------------------------------------