++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2007src0902r started at 19:36:15 on 08-Aug-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 7.373 13.248 30.324 90.00 93.12 90.00 28108 Reflections read from file 2007src0902r.hkl; mean (I/sigma) = 4.04 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 14038 14025 14085 14067 21074 18737 18752 28108 N (int>3sigma) = 0 5809 6110 5899 6007 8909 8083 7974 12022 Mean intensity = 0.0 9.7 10.6 10.3 10.0 10.2 10.2 10.5 10.4 Mean int/sigma = 0.0 4.1 4.3 4.1 4.2 4.2 4.2 4.1 4.2 Lattice type: P chosen Volume: 2957.49 ------------------------------------------------------------------------------- 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: 7.373 13.248 30.324 90.00 93.12 90.00 Niggli form: a.a = 54.36 b.b = 175.50 c.c = 919.55 b.c = 0.00 a.c = -12.18 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. MONOCLINIC P-lattice R(sym) = 0.084 [ 4818] Cell: 7.373 13.248 30.324 90.00 93.12 90.00 Volume: 2957.49 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 14038 14025 14085 14067 21074 18737 18752 28108 N (int>3sigma) = 0 5809 6110 5899 6007 8909 8083 7974 12022 Mean intensity = 0.0 9.7 10.6 10.3 10.0 10.2 10.2 10.5 10.4 Mean int/sigma = 0.0 4.1 4.3 4.1 4.2 4.2 4.2 4.1 4.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.934 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 20 766 772 786 N I>3s 0 202 5 205 0.4 4.2 0.6 4.1 0.7 2.7 0.6 2.6 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] P2(1)/c # 14 centro 1 19410 0.084 4818 0.7 / 2.6 5.05 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2007src0902r.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.10 373 384 97.1 8.93 31.1 24.91 0.0411 0.0262 2.10 - 1.65 377 377 100.0 6.90 21.2 20.21 0.0574 0.0328 1.65 - 1.40 464 464 100.0 5.98 13.7 15.76 0.0770 0.0452 1.40 - 1.25 471 471 100.0 5.29 8.9 11.04 0.1085 0.0650 1.25 - 1.15 481 481 100.0 4.42 6.4 7.83 0.1528 0.0959 1.15 - 1.05 648 648 100.0 3.88 5.4 5.85 0.1900 0.1325 1.05 - 1.00 458 462 99.1 3.47 5.0 5.03 0.2012 0.1638 1.00 - 0.95 520 522 99.6 3.30 4.4 4.27 0.2465 0.1909 0.95 - 0.90 658 663 99.2 2.96 4.4 3.49 0.2816 0.2709 0.90 - 0.85 810 825 98.2 2.81 3.2 2.65 0.3880 0.3576 0.85 - 0.80 1007 1039 96.9 2.58 2.3 1.76 0.5914 0.5799 0.80 - 0.77 752 876 85.8 2.16 1.5 1.16 0.9951 0.9040 ------------------------------------------------------------------------------ 0.90 - 0.77 2569 2740 93.8 2.51 2.4 1.86 0.5592 0.5473 Inf - 0.77 7019 7212 97.3 3.90 7.2 6.92 0.1091 0.1354 Merged [A], lowest resolution = 6.77 Angstroms, 785 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2007src0902r.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C18H11N2Cl1Fe1 Formula weight = 346.59 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.557, non-H atomic volume = 16.8 and following cell contents and analysis: C 144.00 62.37 % H 88.00 3.20 % N 16.00 8.08 % Cl 8.00 10.23 % Fe 8.00 16.11 % F(000) = 1408.0 Mo-K(alpha) radiation Mu (mm-1) = 1.20 ------------------------------------------------------------------------------- File 2007src0902r.ins set up as follows: TITL 2007src0902r in P2(1)/c CELL 0.71073 7.3730 13.2476 30.3241 90.000 93.123 90.000 ZERR 8.00 0.0005 0.0010 0.0023 0.000 0.004 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N CL FE UNIT 144 88 16 8 8 TEMP 0.01 TREF HKLF 4 END -------------------------------------------------------------------------------