+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2009/1 for Windows + + Copyright(C) 2009 Bruker-AXS All Rights Reserved + + 2009src0359 started at 10:56:52 on 02-Apr-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 13.251 8.739 17.931 90.00 110.15 90.00 23445 Reflections read from file 2009src0359.hkl; mean (I/sigma) = 9.55 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 11747 11772 11697 11721 17608 15650 15636 23445 N (int>3sigma) = 0 9138 9331 9299 9399 13884 12435 12400 18640 Mean intensity = 0.0 57.7 57.8 55.9 57.6 57.2 58.0 57.3 57.9 Mean int/sigma = 0.0 9.4 9.5 9.6 9.7 9.5 9.6 9.6 9.6 Lattice type: P chosen Volume: 1949.37 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 8.739 13.251 17.931 110.15 90.00 90.00 Niggli form: a.a = 76.37 b.b = 175.59 c.c = 321.51 b.c = -81.83 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. MONOCLINIC P-lattice R(sym) = 0.023 [ 3362] Cell: 13.251 8.739 17.931 90.00 110.15 90.00 Volume: 1949.37 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 11747 11772 11697 11721 17608 15650 15636 23445 N (int>3sigma) = 0 9138 9331 9299 9399 13884 12435 12400 18640 Mean intensity = 0.0 57.7 57.8 55.9 57.6 57.2 58.0 57.3 57.9 Mean int/sigma = 0.0 9.4 9.5 9.6 9.7 9.5 9.6 9.6 9.6 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.860 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 14 925 937 940 N I>3s 0 426 1 425 0.2 66.6 0.3 65.5 0.5 6.7 0.6 6.6 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 0.023 3362 0.6 / 6.6 2.82 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2009src0359.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.14 243 253 96.0 6.51 132.6 34.67 0.0284 0.0235 2.14 - 1.68 247 247 100.0 7.32 112.5 40.65 0.0302 0.0186 1.68 - 1.46 247 247 100.0 7.31 83.0 38.43 0.0328 0.0195 1.46 - 1.33 240 240 100.0 7.43 74.5 34.26 0.0362 0.0208 1.33 - 1.23 253 253 100.0 7.36 53.8 30.00 0.0435 0.0251 1.23 - 1.16 242 242 100.0 7.27 54.7 28.06 0.0451 0.0276 1.16 - 1.10 243 243 100.0 6.23 48.3 23.06 0.0513 0.0337 1.10 - 1.05 261 261 100.0 5.64 54.1 21.17 0.0482 0.0367 1.05 - 1.00 296 296 100.0 5.35 39.6 18.03 0.0576 0.0425 1.00 - 0.96 297 297 100.0 4.73 40.4 15.88 0.0617 0.0487 0.96 - 0.93 259 259 100.0 4.12 35.3 13.39 0.0681 0.0549 0.93 - 0.90 283 283 100.0 3.45 27.8 11.54 0.0698 0.0648 0.90 - 0.87 342 342 100.0 3.11 26.8 9.84 0.0650 0.0753 0.87 - 0.84 361 361 100.0 3.01 24.5 9.03 0.0706 0.0786 0.84 - 0.82 298 298 100.0 2.78 23.4 8.19 0.0723 0.0898 0.82 - 0.80 295 295 100.0 2.81 20.6 7.95 0.0904 0.0947 0.80 - 0.78 364 365 99.7 2.61 18.1 6.41 0.0875 0.1101 0.78 - 0.77 4 15 26.7 0.27 39.2 5.89 0.1346 ------------------------------------------------------------------------------ 0.87 - 0.77 1457 1469 99.2 2.80 22.1 8.03 0.0768 0.0903 Inf - 0.77 4775 4797 99.5 4.89 48.1 19.32 0.0431 0.0396 Merged [A], lowest resolution = 6.62 Angstroms, 791 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2009src0359.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C18H30N2Cl2Ir1 Formula weight = 537.57 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.832, non-H atomic volume = 21.2 and following cell contents and analysis: C 72.00 40.22 % H 120.00 5.63 % N 8.00 5.21 % Cl 8.00 13.19 % Ir 4.00 35.76 % F(000) = 1052.0 Mo-K(alpha) radiation Mu (mm-1) = 7.12 ------------------------------------------------------------------------------- File 2009src0359.ins set up as follows: TITL 2009src0359 in P2(1)/c CELL 0.71073 13.2510 8.7390 17.9308 90.000 110.145 90.000 ZERR 4.00 0.0002 0.0002 0.0004 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N CL IR UNIT 72 120 8 8 4 TEMP 0.06 TREF HKLF 4 END -------------------------------------------------------------------------------