+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2008/2 for Windows + + Copyright(C) 2008 Bruker-AXS All Rights Reserved + + 2008src0880 started at 14:25:55 on 16-Sep-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 12.764 11.958 29.257 90.00 98.80 90.00 34226 Reflections read from file 2008src0880.hkl; mean (I/sigma) = 9.63 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 17129 17141 17090 17117 25680 22806 22815 34226 N (int>3sigma) = 0 12284 12723 12743 12744 18875 16999 17006 25500 Mean intensity = 0.0 33.3 35.3 34.0 33.6 34.2 34.2 33.7 34.2 Mean int/sigma = 0.0 9.3 9.7 9.6 9.6 9.5 9.7 9.7 9.7 Lattice type: P chosen Volume: 4413.19 ------------------------------------------------------------------------------- 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: 11.958 12.764 29.257 98.80 90.00 90.00 Niggli form: a.a = 143.00 b.b = 162.93 c.c = 855.95 b.c = -57.14 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) = 0.028 [ 6751] Cell: 12.764 11.958 29.257 90.00 98.80 90.00 Volume: 4413.19 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 17129 17141 17090 17117 25680 22806 22815 34226 N (int>3sigma) = 0 12284 12723 12743 12744 18875 16999 17006 25500 Mean intensity = 0.0 33.3 35.3 34.0 33.6 34.2 34.2 33.7 34.2 Mean int/sigma = 0.0 9.3 9.7 9.6 9.6 9.5 9.7 9.7 9.7 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.950 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 22 990 1009 999 N I>3s 0 434 14 438 0.3 45.1 0.3 44.7 0.7 6.7 0.7 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 0.028 6751 0.7 / 6.6 1.72 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008src0880.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.13 525 547 96.0 6.57 90.2 42.17 0.0386 0.0198 2.13 - 1.69 540 541 99.8 4.89 65.2 33.33 0.0378 0.0232 1.69 - 1.47 527 532 99.1 4.38 51.9 28.93 0.0373 0.0260 1.47 - 1.33 551 562 98.0 4.20 43.4 25.73 0.0399 0.0291 1.33 - 1.23 551 564 97.7 3.79 35.5 21.29 0.0391 0.0321 1.23 - 1.15 585 607 96.4 3.32 29.7 18.59 0.0449 0.0392 1.15 - 1.09 536 551 97.3 3.12 30.7 17.23 0.0430 0.0399 1.09 - 1.04 586 600 97.7 3.02 24.8 15.69 0.0459 0.0450 1.04 - 1.00 536 555 96.6 2.92 23.6 14.75 0.0554 0.0493 1.00 - 0.96 661 676 97.8 2.85 19.9 13.10 0.0592 0.0554 0.96 - 0.92 723 740 97.7 2.70 18.6 11.61 0.0604 0.0627 0.92 - 0.89 689 699 98.6 2.59 16.9 10.63 0.0637 0.0702 0.89 - 0.86 734 745 98.5 2.55 13.7 9.06 0.0807 0.0817 0.86 - 0.84 575 593 97.0 2.46 12.7 8.41 0.0821 0.0889 0.84 - 0.82 622 634 98.1 2.34 12.0 7.73 0.0900 0.0964 0.82 - 0.80 674 691 97.5 2.30 10.7 7.17 0.0928 0.1055 0.80 - 0.78 763 788 96.8 2.26 9.3 6.47 0.1086 0.1204 0.78 - 0.77 35 63 55.6 0.73 6.7 4.02 0.0650 0.2074 ------------------------------------------------------------------------------ 0.87 - 0.77 3167 3273 96.8 2.33 11.4 7.58 0.0911 0.0996 Inf - 0.77 10413 10688 97.4 3.20 28.0 16.24 0.0458 0.0433 Merged [A], lowest resolution = 6.82 Angstroms, 806 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008src0880.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C42H24OP2F6Cl4Au2 Formula weight = 1256.32 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.891, non-H atomic volume = 19.4 and following cell contents and analysis: C 168.00 40.15 % H 96.00 1.93 % O 4.00 1.27 % F 24.00 9.07 % P 8.00 4.93 % Cl 16.00 11.29 % Au 8.00 31.36 % F(000) = 2376.0 Mo-K(alpha) radiation Mu (mm-1) = 7.01 ------------------------------------------------------------------------------- File 2008src0880.ins set up as follows: TITL 2008src0880 in P2(1)/c CELL 0.71073 12.7644 11.9584 29.2566 90.000 98.801 90.000 ZERR 4.00 0.0002 0.0002 0.0005 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O F P CL AU UNIT 168 96 4 24 8 16 8 TEMP 0.22 TREF HKLF 4 END -------------------------------------------------------------------------------