++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008src0009 started at 11:15:46 on 14-Jan-2008 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 18.305 8.139 39.269 90.00 101.66 90.00 49698 Reflections read from file 2008src0009.hkl; mean (I/sigma) = 5.17 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 24832 24917 24885 24873 37317 33119 33110 49698 N (int>3sigma) = 0 12722 11863 12623 11885 18604 16814 16728 25354 Mean intensity = 0.0 7.5 6.8 7.5 6.8 7.3 7.5 7.5 7.5 Mean int/sigma = 0.0 5.3 5.0 5.3 5.0 5.2 5.3 5.2 5.3 Lattice type: P chosen Volume: 5729.73 ------------------------------------------------------------------------------- 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: 8.139 18.305 39.269 101.66 90.00 90.00 Niggli form: a.a = 66.24 b.b = 335.08 c.c = 1542.06 b.c = -145.31 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) = 0.055 [ 7719] Cell: 18.305 8.139 39.269 90.00 101.66 90.00 Volume: 5729.73 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 24832 24917 24885 24873 37317 33119 33110 49698 N (int>3sigma) = 0 12722 11863 12623 11885 18604 16814 16728 25354 Mean intensity = 0.0 7.5 6.8 7.5 6.8 7.3 7.5 7.5 7.5 Mean int/sigma = 0.0 5.3 5.0 5.3 5.0 5.2 5.3 5.2 5.3 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.983 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 11 2351 2339 2384 N I>3s 0 706 705 1 0.1 4.2 4.2 0.2 0.6 3.5 3.5 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] P2(1)/n # 14 centro 1 19410 0.055 7719 0.6 / 3.5 3.41 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008src0009.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.20 647 677 95.6 9.20 22.6 31.38 0.0345 0.0220 2.20 - 1.70 703 732 96.0 6.61 13.3 24.11 0.0461 0.0298 1.70 - 1.45 796 828 96.1 5.41 8.5 16.68 0.0636 0.0427 1.45 - 1.30 799 827 96.6 4.90 8.2 14.31 0.0740 0.0500 1.30 - 1.20 772 802 96.3 3.91 7.8 11.55 0.0760 0.0617 1.20 - 1.10 1059 1110 95.4 3.36 4.6 7.94 0.1037 0.0910 1.10 - 1.05 663 708 93.6 3.13 3.7 6.32 0.1307 0.1177 1.05 - 1.00 814 873 93.2 2.98 3.1 5.50 0.1580 0.1408 1.00 - 0.95 982 1061 92.6 2.74 2.9 4.75 0.1778 0.1638 0.95 - 0.90 1147 1284 89.3 2.68 2.6 4.24 0.2139 0.1965 0.90 - 0.85 1319 1645 80.2 2.41 2.3 3.65 0.2451 0.2288 0.85 - 0.80 1560 2027 77.0 2.35 1.7 2.75 0.3461 0.3333 0.80 - 0.77 1116 1695 65.8 1.97 1.3 1.97 0.4705 0.4640 ------------------------------------------------------------------------------ 0.90 - 0.77 3995 5367 74.4 2.25 1.8 2.83 0.3303 0.3148 Inf - 0.77 12377 14269 86.7 3.48 5.3 8.79 0.0771 0.0904 Merged [A], lowest resolution = 6.87 Angstroms, 1543 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008src0009.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C5H13Cl3N5OP3 Formula weight = 358.46 Tentative Z (number of formula units/cell) = 16.0 giving rho = 1.662, non-H atomic volume = 21.1 and following cell contents and analysis: C 80.00 16.75 % H 208.00 3.66 % N 80.00 19.54 % O 16.00 4.46 % P 48.00 25.92 % Cl 48.00 29.67 % F(000) = 2912.0 Mo-K(alpha) radiation Mu (mm-1) = 0.97 ------------------------------------------------------------------------------- File 2008src0009.ins set up as follows: TITL 2008src0009 in P2(1)/n CELL 0.71073 18.3051 8.1390 39.2691 90.000 101.662 90.000 ZERR 16.00 0.0005 0.0001 0.0009 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O P CL UNIT 80 208 80 16 48 48 TEMP 0.05 TREF HKLF 4 END -------------------------------------------------------------------------------