++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - Reciprocal space exploration - Version 6.12 - W95/98/NT/2000/ME + + COPYRIGHT(c) 2001 Bruker-AXS All Rights Reserved + + 2008src0232 started at 13:16:04 on 27-Mar-2008 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 6.307 17.644 9.548 90.00 96.55 90.00 12418 Reflections read from file 2008src0232.hkl; mean (I/sigma) = 15.36 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6208 6187 6209 6202 9302 8290 8293 12418 N (int>3sigma) = 0 5949 5951 5972 5939 8936 7980 7961 11951 Mean intensity = 0.0 590.1 577.3 601.1 589.2 589.5 577.1 564.9 584.3 Mean int/sigma = 0.0 15.3 15.5 15.4 15.3 15.4 15.4 15.3 15.4 Lattice type: P chosen Volume: 1055.62 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 6.307 9.548 17.644 90.00 90.00 96.55 Niggli form: a.a = 39.78 b.b = 91.17 c.c = 311.30 b.c = 0.00 a.c = 0.00 a.b = -6.87 ------------------------------------------------------------------------------- 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) = 0.018 [ 2132] Cell: 6.307 17.644 9.548 90.00 96.55 90.00 Volume: 1055.62 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 6208 6187 6209 6202 9302 8290 8293 12418 N (int>3sigma) = 0 5949 5951 5972 5939 8936 7980 7961 11951 Mean intensity = 0.0 590.1 577.3 601.1 589.2 589.5 577.1 564.9 584.3 Mean int/sigma = 0.0 15.3 15.5 15.4 15.3 15.4 15.4 15.3 15.4 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.708 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 25 255 250 255 N I>3s 0 242 235 239 2.3 863.0 834.1 732.7 0.9 16.3 15.6 16.0 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) # 4 chiral 1 3543 0.018 2132 0.9 / 15.4 0.78 [B] P2(1)/m # 11 centro 1 402 0.018 2132 0.9 / 15.4 7.70 Option [A] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 2008src0232.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) R(sigma) Inf - 2.05 136 142 95.8 6.73 1873.8 58.76 0.0212 0.0186 2.05 - 1.65 128 128 100.0 7.52 1017.1 58.41 0.0261 0.0157 1.65 - 1.40 167 167 100.0 7.55 659.6 56.15 0.0314 0.0162 1.40 - 1.25 160 160 100.0 7.42 758.2 52.01 0.0296 0.0173 1.25 - 1.15 179 179 100.0 7.25 675.5 47.01 0.0337 0.0187 1.15 - 1.05 223 223 100.0 5.99 470.1 38.40 0.0385 0.0230 1.05 - 1.00 159 159 100.0 5.53 321.5 31.19 0.0447 0.0280 1.00 - 0.95 198 198 100.0 4.81 226.2 26.35 0.0536 0.0330 0.95 - 0.90 220 220 100.0 4.08 209.7 21.42 0.0545 0.0389 0.90 - 0.85 302 302 100.0 3.47 208.3 17.78 0.0538 0.0467 0.85 - 0.80 354 355 99.7 2.95 177.6 14.33 0.0592 0.0599 0.80 - 0.77 271 283 95.8 2.11 167.4 11.19 0.0611 0.0797 ------------------------------------------------------------------------------ 0.90 - 0.77 927 940 98.6 2.86 184.6 14.54 0.0571 0.0603 Inf - 0.77 2497 2516 99.2 4.94 462.7 31.44 0.0328 0.0263 Merged [A], lowest resolution = 6.46 Angstroms, 377 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 2008src0232.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C18H24N5O4P3 Formula weight = 467.33 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.470, non-H atomic volume = 17.6 and following cell contents and analysis: C 36.00 46.26 % H 48.00 5.18 % N 10.00 14.99 % O 8.00 13.69 % P 6.00 19.88 % F(000) = 488.0 Mo-K(alpha) radiation Mu (mm-1) = 0.32 ------------------------------------------------------------------------------- File 2008src0232.ins set up as follows: TITL 2008src0232 in P2(1) CELL 0.71073 6.3073 17.6438 9.5481 90.000 96.552 90.000 ZERR 2.00 0.0001 0.0004 0.0002 0.000 0.001 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O P UNIT 36 48 10 8 6 TEMP 0.04 TREF HKLF 4 END -------------------------------------------------------------------------------