++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008lsh007 started at 18:27:28 on 18-Nov-2010 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.426 10.305 9.578 90.00 109.29 90.00 11187 Reflections read from file 2008lsh007.hkl; mean (I/sigma) = 16.01 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5603 5596 5601 5587 8400 7465 7458 11187 N (int>3sigma) = 0 4889 4911 4780 4858 7290 6549 6493 9776 Mean intensity = 0.0 73.7 75.7 73.0 74.4 74.1 74.6 75.4 74.5 Mean int/sigma = 0.0 16.0 16.1 15.7 16.0 16.0 16.1 16.0 16.0 Lattice type: P chosen Volume: 878.13 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 9.426 9.578 10.305 90.00 90.00 109.29 Niggli form: a.a = 88.85 b.b = 91.74 c.c = 106.19 b.c = 0.00 a.c = 0.00 a.b = -29.82 ------------------------------------------------------------------------------- Search for higher metric symmetry Identical indices and Friedel opposites combined before calculating R(sym) ------------------------------------------------------------------------------ Option A: FOM = 0.974 deg. ORTHORHOMBIC C-lattice R(sym) = 0.523 [ 2777] Cell: 10.998 15.499 10.305 90.00 90.00 89.03 Volume: 1756.25 Matrix: 1.0000 0.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(sym) = 0.012 [ 1824] Cell: 9.426 10.305 9.578 90.00 109.29 90.00 Volume: 878.13 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.974 deg. MONOCLINIC C-lattice R(sym) = 0.550 [ 1806] Cell: 15.499 10.998 10.305 90.00 90.00 90.97 Volume: 1756.25 Matrix: 1.0000 0.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.974 deg. MONOCLINIC C-lattice R(sym) = 0.548 [ 1833] Cell: 10.998 15.499 10.305 90.00 90.00 89.03 Volume: 1756.25 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5603 5596 5601 5587 8400 7465 7458 11187 N (int>3sigma) = 0 4889 4911 4780 4858 7290 6549 6493 9776 Mean intensity = 0.0 73.7 75.7 73.0 74.4 74.1 74.6 75.4 74.5 Mean int/sigma = 0.0 16.0 16.1 15.7 16.0 16.0 16.1 16.0 16.0 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.935 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 20 335 320 321 N I>3s 0 22 164 164 0.1 0.2 68.0 67.8 0.6 1.0 9.8 9.8 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 0.012 1824 1.0 / 9.8 1.25 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008lsh007.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.05 111 125 88.8 5.09 164.1 48.34 0.0177 0.0229 2.05 - 1.65 107 108 99.1 6.77 149.8 62.50 0.0192 0.0152 1.65 - 1.40 135 135 100.0 6.99 139.0 64.50 0.0208 0.0126 1.40 - 1.25 150 150 100.0 6.89 106.7 57.54 0.0225 0.0133 1.25 - 1.15 143 143 100.0 7.19 91.2 54.46 0.0247 0.0148 1.15 - 1.05 198 198 100.0 7.16 70.1 43.18 0.0241 0.0179 1.05 - 1.00 128 128 100.0 6.73 57.7 36.28 0.0261 0.0215 1.00 - 0.95 158 158 100.0 5.99 43.8 30.47 0.0291 0.0253 0.95 - 0.90 210 210 100.0 5.06 39.0 25.51 0.0347 0.0314 0.90 - 0.85 239 240 99.6 4.04 30.9 19.25 0.0420 0.0380 0.85 - 0.80 312 314 99.4 3.00 23.1 14.85 0.0358 0.0497 0.80 - 0.77 233 272 85.7 2.27 15.7 11.79 0.0464 0.0612 ------------------------------------------------------------------------------ 0.90 - 0.77 784 826 94.9 3.06 23.3 15.28 0.0405 0.0473 Inf - 0.77 2124 2181 97.4 5.13 64.3 34.15 0.0242 0.0220 Merged [A], lowest resolution = 6.80 Angstroms, 460 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008lsh007.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C8H8I1N1O1 Formula weight = 261.05 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.975, non-H atomic volume = 20.0 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) = 3.59 ------------------------------------------------------------------------------- File p21c.ins set up as follows: TITL p21c in P2(1)/c CELL 0.71073 9.5782 10.3047 9.4258 90.000 109.285 90.000 ZERR 4.00 0.0003 0.0003 0.0002 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O I UNIT 32 32 4 4 4 TEMP 0.16 TREF HKLF 4 END 11187 Reflections written to new reflection file p21c.hkl -------------------------------------------------------------------------------