+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 2008/2 for Windows + + Copyright(C) 2008 Bruker-AXS All Rights Reserved + + 2008src0845 started at 14:44:55 on 15-Jul-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 21.596 9.524 30.617 90.00 107.43 90.00 53794 Reflections read from file 2008src0845.hkl; mean (I/sigma) = 4.83 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 26929 26838 26925 26901 40346 35806 35864 53794 N (int>3sigma) = 0 12434 11767 12503 11882 18352 16452 16644 24756 Mean intensity = 0.0 81.0 82.4 80.4 72.2 81.3 82.2 88.2 82.5 Mean int/sigma = 0.0 5.0 4.7 5.0 4.8 4.9 5.0 5.0 5.0 Lattice type: P chosen Volume: 6008.00 ------------------------------------------------------------------------------- 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: 9.524 21.596 30.617 107.43 90.00 90.00 Niggli form: a.a = 90.71 b.b = 466.37 c.c = 937.38 b.c = -198.06 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) = 0.036 [ 10901] Cell: 21.595 9.524 30.617 90.00 107.43 90.00 Volume: 6008.00 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 26929 26838 26925 26901 40346 35806 35864 53794 N (int>3sigma) = 0 12434 11767 12503 11882 18352 16452 16644 24756 Mean intensity = 0.0 81.0 82.4 80.4 72.2 81.3 82.2 88.2 82.5 Mean int/sigma = 0.0 5.0 4.7 5.0 4.8 4.9 5.0 5.0 5.0 Crystal system M and Lattice type P selected Mean |E*E-1| = 1.246 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 15 1815 1799 1738 N I>3s 3 602 605 11 3.9 85.2 85.9 2.1 1.8 4.0 4.0 0.7 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/n # 13 centro 1 292 0.036 10901 0.7 / 1.8 17.68 [B] Pn # 7 non-cen 1 226 0.036 10901 0.7 / 1.8 36.07 [C] P2(1)/n # 14 centro 1 19410 0.036 10901 1.8 / 4.0 11.35 Option [C] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008src0845.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.14 735 766 96.0 5.28 371.3 21.90 0.0261 0.0263 2.14 - 1.69 734 736 99.7 5.20 166.8 18.69 0.0305 0.0282 1.69 - 1.47 763 763 100.0 5.10 83.7 15.25 0.0425 0.0332 1.47 - 1.33 747 748 99.9 4.64 63.9 12.29 0.0534 0.0396 1.33 - 1.23 792 793 99.9 4.46 62.2 11.92 0.0578 0.0423 1.23 - 1.15 832 833 99.9 4.21 61.7 11.33 0.0604 0.0459 1.15 - 1.09 781 783 99.7 3.89 58.3 9.95 0.0601 0.0512 1.09 - 1.04 788 793 99.4 3.75 54.7 9.11 0.0656 0.0555 1.04 - 1.00 784 787 99.6 3.54 38.9 7.70 0.0845 0.0709 1.00 - 0.96 866 869 99.7 3.40 28.2 6.12 0.1093 0.0941 0.96 - 0.93 802 805 99.6 3.32 24.0 5.83 0.1149 0.1048 0.93 - 0.90 893 897 99.6 3.22 17.3 4.44 0.1446 0.1398 0.90 - 0.87 986 993 99.3 3.03 14.6 3.79 0.1746 0.1710 0.87 - 0.85 765 767 99.7 2.87 15.2 3.92 0.1607 0.1729 0.85 - 0.83 813 820 99.1 2.83 17.1 3.95 0.1660 0.1636 0.83 - 0.81 894 899 99.4 2.81 13.3 3.25 0.1870 0.2073 0.81 - 0.79 1028 1036 99.2 2.70 11.2 2.89 0.2226 0.2436 0.79 - 0.77 521 570 91.4 2.36 11.6 2.87 0.2161 0.2546 ------------------------------------------------------------------------------ 0.87 - 0.77 4395 4467 98.4 2.76 13.8 3.39 0.1868 0.1987 Inf - 0.77 14524 14658 99.1 3.67 58.9 8.38 0.0498 0.0538 Merged [A], lowest resolution = 6.99 Angstroms, 612 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008src0845.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C23H20N2O6 Formula weight = 420.41 Tentative Z (number of formula units/cell) = 12.0 giving rho = 1.394, non-H atomic volume = 16.2 and following cell contents and analysis: C 276.00 65.71 % H 240.00 4.79 % N 24.00 6.66 % O 72.00 22.83 % F(000) = 2640.0 Mo-K(alpha) radiation Mu (mm-1) = 0.10 ------------------------------------------------------------------------------- File 2008src0845.ins set up as follows: TITL 2008src0845 in P2(1)/n CELL 0.71073 21.5955 9.5241 30.6167 90.000 107.431 90.000 ZERR 12.00 0.0007 0.0003 0.0010 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 276 240 24 72 TEMP 0.09 TREF HKLF 4 END 53794 Reflections written to new reflection file 2008src0845.hkl -------------------------------------------------------------------------------