++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 2007src0256 started at 15:33:52 on 23-FEB-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.563 10.601 19.568 91.04 90.75 90.04 32022 Reflections read from file 2007src0256.hkl; mean (I/sigma) = 6.41 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 15991 16020 16061 16047 24036 21335 21377 32022 N (int>3sigma) = 0 10614 10167 10581 10495 15681 13896 14184 21232 Mean intensity = 0.0 197.4 190.1 194.4 206.3 194.0 192.7 205.5 207.4 Mean int/sigma = 0.0 6.5 6.2 6.4 6.4 6.4 6.3 6.5 6.5 Lattice type: P chosen Volume: 1983.18 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Unitcell: 9.563 10.601 19.568 91.04 90.75 90.04 Niggli form: a.a = 91.45 b.b = 112.37 c.c = 382.91 b.c = -3.76 a.c = -2.45 a.b = -0.07 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.753 deg. MONOCLINIC P-lattice R(int) = 0.081 [ 27243] Cell: 10.601 9.563 19.568 89.25 91.04 89.96 Volume: 1983.18 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.061 [ 23367] Cell: 9.563 10.601 19.568 91.04 90.75 90.04 Volume: 1983.18 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 15991 16020 16061 16047 24036 21335 21377 32022 N (int>3sigma) = 0 10614 10167 10581 10495 15681 13896 14184 21232 Mean intensity = 0.0 197.4 190.1 194.4 206.3 194.0 192.7 205.5 207.4 Mean int/sigma = 0.0 6.5 6.2 6.4 6.4 6.4 6.3 6.5 6.5 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.974 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P-1 # 2 centro 1 8646 0.061 23367 0.0 / 6.5 1.56 [B] P1 # 1 chiral 1 700 0.061 23367 0.0 / 6.5 7.33 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C18H24N5O2P3 Formula weight = 435.33 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.458, non-H atomic volume = 17.7 and following cell contents and analysis: C 72.00 49.66 % H 96.00 5.56 % N 20.00 16.09 % O 8.00 7.35 % P 12.00 21.34 % F(000) = 912.0 Mo-K(alpha) radiation Mu (mm-1) = 0.33 ------------------------------------------------------------------------------- File 2007src0256.ins set up as follows: TITL 2007src0256 in P-1 CELL 0.71073 9.5629 10.6006 19.5682 91.038 90.752 90.038 ZERR 4.00 0.0004 0.0006 0.0011 0.002 0.003 0.004 LATT 1 SFAC C H N O P UNIT 72 96 20 8 12 TEMP 0.2 TREF HKLF 4 END -------------------------------------------------------------------------------