+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2008/2 for Windows + + Copyright(C) 2008 Bruker-AXS All Rights Reserved + + 2010src0402 started at 10:54:18 on 10-May-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.365 17.328 20.989 90.00 90.00 90.00 21774 Reflections read from file 2010src0402.hkl; mean (I/sigma) = 6.68 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 10931 10909 10878 10898 16359 14526 14502 21774 N (int>3sigma) = 0 7759 7378 7667 7806 11402 10457 10444 15678 Mean intensity = 0.0 31.3 20.9 31.0 28.4 27.7 31.4 31.4 31.6 Mean int/sigma = 0.0 6.7 6.3 6.6 6.7 6.5 6.8 6.8 6.8 Lattice type: P chosen Volume: 2678.48 ------------------------------------------------------------------------------- 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: 7.365 17.328 20.989 90.00 90.00 90.00 Niggli form: a.a = 54.24 b.b = 300.26 c.c = 440.52 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 [ 8299] Cell: 7.365 17.328 20.989 90.00 90.00 90.00 Volume: 2678.48 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 10931 10909 10878 10898 16359 14526 14502 21774 N (int>3sigma) = 0 7759 7378 7667 7806 11402 10457 10444 15678 Mean intensity = 0.0 31.3 20.9 31.0 28.4 27.7 31.4 31.4 31.6 Mean int/sigma = 0.0 6.7 6.3 6.6 6.7 6.5 6.8 6.8 6.8 Crystal system O and Lattice type P selected Mean |E*E-1| = 1.011 [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 1186 1209 1189 7 374 379 367 30 308 320 306 32 N I>3s 504 4 502 0 134 1 135 0 125 2 123 0 36.1 0.2 36.0 0.3 17.2 0.2 17.5 0.2 25.2 0.2 25.4 0.2 4.4 0.6 4.4 0.7 4.1 0.6 4.2 0.6 4.6 0.6 4.5 0.5 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 8299 0.7 / 4.1 3.13 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2010src0402.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.23 177 189 93.7 6.47 69.2 21.18 0.0267 0.0358 2.23 - 1.72 181 181 100.0 8.20 75.4 28.72 0.0276 0.0262 1.72 - 1.49 178 178 100.0 8.56 67.9 31.31 0.0298 0.0247 1.49 - 1.35 183 183 100.0 8.44 46.5 27.12 0.0342 0.0259 1.35 - 1.24 192 192 100.0 8.68 31.4 24.80 0.0442 0.0295 1.24 - 1.17 177 177 100.0 8.58 24.1 20.93 0.0522 0.0342 1.17 - 1.10 207 207 100.0 8.60 26.5 19.41 0.0522 0.0370 1.10 - 1.05 178 178 100.0 8.16 26.2 17.09 0.0593 0.0420 1.05 - 1.01 183 183 100.0 7.04 23.2 15.33 0.0622 0.0451 1.01 - 0.97 207 207 100.0 6.79 17.5 13.82 0.0695 0.0487 0.97 - 0.93 231 231 100.0 6.16 18.9 12.48 0.0718 0.0554 0.93 - 0.90 223 223 100.0 5.01 17.7 10.87 0.0826 0.0622 0.90 - 0.87 233 233 100.0 4.40 15.5 9.06 0.0862 0.0748 0.87 - 0.85 179 179 100.0 3.70 11.9 8.37 0.0770 0.0813 0.85 - 0.83 181 181 100.0 3.56 10.6 7.15 0.0818 0.0955 0.83 - 0.81 230 230 100.0 3.45 9.5 7.33 0.1009 0.0966 0.81 - 0.79 239 239 100.0 3.35 9.0 6.38 0.1000 0.1059 0.79 - 0.77 133 135 98.5 3.11 7.6 5.46 0.1012 0.1171 ------------------------------------------------------------------------------ 0.87 - 0.77 1038 1040 99.8 3.50 9.8 7.01 0.0915 0.0971 Inf - 0.77 3512 3526 99.6 6.18 27.4 15.61 0.0450 0.0424 Merged [A], lowest resolution = 7.00 Angstroms, 815 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2010src0402.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C20H19Fe1N3O2 Formula weight = 389.23 Tentative Z (number of formula units/cell) = 6.0 giving rho = 1.448, non-H atomic volume = 17.2 and following cell contents and analysis: C 120.00 61.72 % H 114.00 4.92 % N 18.00 10.80 % O 12.00 8.22 % Fe 6.00 14.35 % F(000) = 1212.0 Mo-K(alpha) radiation Mu (mm-1) = 0.86 ------------------------------------------------------------------------------- File 2010src0402a.ins set up as follows: TITL 2010src0402a in Pbca CELL 0.71073 17.3279 7.3648 20.9885 90.000 90.000 90.000 ZERR 6.00 0.0002 0.0001 0.0003 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 FE UNIT 120 114 18 12 6 TEMP 0.06 TREF HKLF 4 END 21774 Reflections written to new reflection file 2010src0402a.hkl -------------------------------------------------------------------------------