++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 10:29:15 on 29-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 15.384 8.068 24.194 90.00 105.88 90.00 23544 Reflections read from file s92.hkl; mean (I/sigma) = 4.65 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 11769 11645 11820 11738 17617 15691 15657 23544 N (int>3sigma) = 0 5259 5121 5328 5130 7854 6959 6910 10513 Mean intensity = 0.0 18.4 17.9 18.1 17.4 18.1 18.0 17.7 18.1 Mean int/sigma = 0.0 4.8 4.6 4.8 4.7 4.8 4.8 4.7 4.8 Lattice type: P chosen Volume: 2888.46 ------------------------------------------------------------------------------- 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: 8.068 15.384 24.194 105.88 90.00 90.00 Niggli form: a.a = 65.10 b.b = 236.66 c.c = 585.33 b.c = -101.82 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.083 [ 16623] Cell: 15.384 8.068 24.194 90.00 105.88 90.00 Volume: 2888.46 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 11769 11645 11820 11738 17617 15691 15657 23544 N (int>3sigma) = 0 5259 5121 5328 5130 7854 6959 6910 10513 Mean intensity = 0.0 18.4 17.9 18.1 17.4 18.1 18.0 17.7 18.1 Mean int/sigma = 0.0 4.8 4.6 4.8 4.7 4.8 4.8 4.7 4.8 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.984 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 7 816 820 734 N I>3s 0 288 288 0 0.5 25.1 24.9 0.7 0.5 4.4 4.4 0.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.083 16623 0.5 / 4.4 2.55 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C24H30F6N3O7P3 Formula weight = 679.42 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.562, non-H atomic volume = 16.8 and following cell contents and analysis: C 96.00 42.42 % H 120.00 4.45 % N 12.00 6.19 % O 28.00 16.48 % F 24.00 16.78 % P 12.00 13.67 % F(000) = 1400.0 Mo-K(alpha) radiation Mu (mm-1) = 0.29 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/n CELL 0.71073 15.3839 8.0685 24.1935 90.000 105.877 90.000 ZERR 4.00 0.0004 0.0002 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 F P UNIT 96 120 12 28 24 12 TREF HKLF 4 END -------------------------------------------------------------------------------