++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 04src0794 started at 16:42:41 on 11-OCT-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 13.648 17.348 33.734 90.01 90.01 90.01 71170 Reflections read from file 04src0794.hkl; mean (I/sigma) = 5.09 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 35530 35593 35641 35555 53382 47417 47454 71170 N (int>3sigma) = 0 18891 19656 19187 19304 28867 25647 25618 38586 Mean intensity = 0.0 114.0 111.4 112.2 110.6 112.5 114.1 113.0 116.1 Mean int/sigma = 0.0 5.1 5.2 5.1 5.1 5.1 5.1 5.1 5.2 Lattice type: P chosen Volume: 7987.12 ------------------------------------------------------------------------------- TOLERANCES CHANGED Maximum deviation (deg.) in higher symmetry cell search = 1.000 Threshold (deg.) for terminating search = 0.005 R(int) maximum for terminating cell search = 0.120 R(int) maximum for space group determination = 0.300 Minimum number of data in group for syst. absence test = 5 Maximum mean I/sigma(I) for systematic absences = 2.009 Minimum I/sigma gap between absences and rest = 1.019 ------------------------------------------------------------------------------- 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: 13.648 17.348 33.734 90.01 90.01 90.01 Niggli form: a.a = 186.27 b.b = 300.96 c.c = 1137.99 b.c = -0.06 a.c = -0.09 a.b = -0.04 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.014 deg. ORTHORHOMBIC P-lattice R(int) = 0.092 [ 61143] Cell: 13.648 17.348 33.734 90.01 90.01 90.01 Volume: 7987.12 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.010 deg. MONOCLINIC P-lattice R(int) = 0.085 [ 52497] Cell: 13.648 17.348 33.734 90.01 90.01 90.01 Volume: 7987.12 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.012 deg. MONOCLINIC P-lattice R(int) = 0.085 [ 52762] Cell: 13.648 33.734 17.348 89.99 90.01 89.99 Volume: 7987.12 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.014 deg. MONOCLINIC P-lattice R(int) = 0.085 [ 52356] Cell: 17.348 13.648 33.734 89.99 90.01 89.99 Volume: 7987.12 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.071 [ 37153] Cell: 13.648 17.348 33.734 90.01 90.01 90.01 Volume: 7987.12 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 35530 35593 35641 35555 53382 47417 47454 71170 N (int>3sigma) = 0 18891 19656 19187 19304 28867 25647 25618 38586 Mean intensity = 0.0 114.0 111.4 112.2 110.6 112.5 114.1 113.0 116.1 Mean int/sigma = 0.0 5.1 5.2 5.1 5.1 5.1 5.1 5.1 5.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.815 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 18 1202 1215 1207 N I>3s 1 488 209 501 5.5 222.4 18.3 221.9 1.0 4.4 1.8 4.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.085 52497 1.8 / 4.4 6.20 Option [A] chosen ------------------------------------------------------------------------------- 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: 13.648 17.348 33.734 90.01 90.01 90.01 Niggli form: a.a = 186.27 b.b = 300.96 c.c = 1137.99 b.c = -0.06 a.c = -0.09 a.b = -0.04 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.014 deg. ORTHORHOMBIC P-lattice R(int) = 0.092 [ 61143] Cell: 13.648 17.348 33.734 90.01 90.01 90.01 Volume: 7987.12 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.010 deg. MONOCLINIC P-lattice R(int) = 0.085 [ 52497] Cell: 13.648 17.348 33.734 90.01 90.01 90.01 Volume: 7987.12 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.012 deg. MONOCLINIC P-lattice R(int) = 0.085 [ 52762] Cell: 13.648 33.734 17.348 89.99 90.01 89.99 Volume: 7987.12 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.014 deg. MONOCLINIC P-lattice R(int) = 0.085 [ 52356] Cell: 17.348 13.648 33.734 89.99 90.01 89.99 Volume: 7987.12 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.071 [ 37153] Cell: 13.648 17.348 33.734 90.01 90.01 90.01 Volume: 7987.12 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Option E selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 35530 35593 35641 35555 53382 47417 47454 71170 N (int>3sigma) = 0 18891 19656 19187 19304 28867 25647 25618 38586 Mean intensity = 0.0 114.0 111.4 112.2 110.6 112.5 114.1 113.0 116.1 Mean int/sigma = 0.0 5.1 5.2 5.1 5.1 5.1 5.1 5.1 5.2 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.815 [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 0.071 37153 0.0 / 5.2 4.29 [B] P1 # 1 chiral 1 700 0.071 37153 0.0 / 5.2 2.71 Option [B] chosen ------------------------------------------------------------------------------- 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: 13.648 17.348 33.734 90.01 90.01 90.01 Niggli form: a.a = 186.27 b.b = 300.96 c.c = 1137.99 b.c = -0.06 a.c = -0.09 a.b = -0.04 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.014 deg. ORTHORHOMBIC P-lattice R(int) = 0.092 [ 61143] Cell: 13.648 17.348 33.734 90.01 90.01 90.01 Volume: 7987.12 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.010 deg. MONOCLINIC P-lattice R(int) = 0.085 [ 52497] Cell: 13.648 17.348 33.734 90.01 90.01 90.01 Volume: 7987.12 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.012 deg. MONOCLINIC P-lattice R(int) = 0.085 [ 52762] Cell: 13.648 33.734 17.348 89.99 90.01 89.99 Volume: 7987.12 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.014 deg. MONOCLINIC P-lattice R(int) = 0.085 [ 52356] Cell: 17.348 13.648 33.734 89.99 90.01 89.99 Volume: 7987.12 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.071 [ 37153] Cell: 13.648 17.348 33.734 90.01 90.01 90.01 Volume: 7987.12 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 35530 35593 35641 35555 53382 47417 47454 71170 N (int>3sigma) = 0 18891 19656 19187 19304 28867 25647 25618 38586 Mean intensity = 0.0 114.0 111.4 112.2 110.6 112.5 114.1 113.0 116.1 Mean int/sigma = 0.0 5.1 5.2 5.1 5.1 5.1 5.1 5.1 5.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.815 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 18 1202 1215 1207 N I>3s 1 488 209 501 5.5 222.4 18.3 221.9 1.0 4.4 1.8 4.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.085 52497 1.8 / 4.4 6.20 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C11H23Cl2N4O6P3 Formula weight = 471.14 Tentative Z (number of formula units/cell) = 15.0 giving rho = 1.469, non-H atomic volume = 20.5 and following cell contents and analysis: C 165.00 28.04 % H 345.00 4.92 % N 60.00 11.89 % O 90.00 20.38 % P 45.00 19.72 % Cl 30.00 15.05 % F(000) = 3660.0 Mo-K(alpha) radiation Mu (mm-1) = 0.56 ------------------------------------------------------------------------------- File 04src0794.ins set up as follows: TITL 04src0794 in P2(1)/c CELL 0.71073 13.6480 17.3481 33.7341 90.000 90.011 90.000 ZERR 15.00 0.0031 0.0030 0.0079 0.000 0.018 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O P CL UNIT 165 345 60 90 45 30 TEMP 0.01 TREF HKLF 4 END -------------------------------------------------------------------------------