++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 16:52:23 on 17-JUN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.829 10.331 21.632 90.00 100.20 90.00 19305 Reflections read from file s92.hkl; mean (I/sigma) = 8.77 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 9630 9587 9549 9590 14383 12852 12859 19305 N (int>3sigma) = 0 6109 5762 6033 5980 8952 8167 8161 12338 Mean intensity = 0.0 59.3 51.3 60.3 57.5 57.0 58.8 58.8 59.6 Mean int/sigma = 0.0 8.9 8.2 8.8 8.6 8.6 8.8 8.8 8.9 Lattice type: P chosen Volume: 2601.84 ------------------------------------------------------------------------------- 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: 10.331 11.829 21.632 100.20 90.00 90.00 Niggli form: a.a = 106.73 b.b = 139.93 c.c = 467.93 b.c = -45.33 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.038 [ 13174] Cell: 11.829 10.331 21.632 90.00 100.20 90.00 Volume: 2601.84 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 9630 9587 9549 9590 14383 12852 12859 19305 N (int>3sigma) = 0 6109 5762 6033 5980 8952 8167 8161 12338 Mean intensity = 0.0 59.3 51.3 60.3 57.5 57.0 58.8 58.8 59.6 Mean int/sigma = 0.0 8.9 8.2 8.8 8.6 8.6 8.8 8.8 8.9 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.958 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 11 515 522 461 N I>3s 0 228 230 2 0.4 67.5 66.6 0.6 0.3 7.2 7.1 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.038 13174 0.5 / 7.1 1.52 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C22H32N3O7P3 Formula weight = 543.42 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.387, non-H atomic volume = 18.6 and following cell contents and analysis: C 88.00 48.62 % H 128.00 5.94 % N 12.00 7.73 % O 28.00 20.61 % P 12.00 17.10 % F(000) = 1144.0 Mo-K(alpha) radiation Mu (mm-1) = 0.28 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/n CELL 0.71073 11.8293 10.3312 21.6318 90.000 100.203 90.000 ZERR 4.00 0.0002 0.0002 0.0005 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O P UNIT 88 128 12 28 12 TREF HKLF 4 END -------------------------------------------------------------------------------