++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 18:52:04 on 12-MAR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 16.438 7.824 18.128 90.00 109.97 90.00 13796 Reflections read from file s92.hkl; mean (I/sigma) = 2.76 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6890 6903 6889 6906 10341 9185 9178 13796 N (int>3sigma) = 0 1921 2115 2050 2069 3043 2724 2782 4125 Mean intensity = 0.0 7.3 7.9 8.1 8.2 7.8 8.0 7.9 7.9 Mean int/sigma = 0.0 2.7 3.0 2.9 2.9 2.9 2.9 3.0 2.9 Lattice type: P chosen Volume: 2191.21 ------------------------------------------------------------------------------- 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: 7.824 16.438 18.128 109.97 90.00 90.00 Niggli form: a.a = 61.21 b.b = 270.20 c.c = 328.64 b.c = -101.78 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.157 [ 9193] Cell: 16.438 7.824 18.128 90.00 109.97 90.00 Volume: 2191.21 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.120 [ 5938] Cell: 7.824 16.438 18.128 70.03 90.00 90.00 Volume: 2191.21 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 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 6890 6903 6889 6906 10341 9185 9178 13796 N (int>3sigma) = 0 1921 2115 2050 2069 3043 2724 2782 4125 Mean intensity = 0.0 7.3 7.9 8.1 8.2 7.8 8.0 7.9 7.9 Mean int/sigma = 0.0 2.7 3.0 2.9 2.9 2.9 2.9 3.0 2.9 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.926 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 9 576 572 566 N I>3s 0 147 0 147 0.4 14.3 0.5 14.5 0.4 3.0 0.5 3.0 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.157 9193 0.5 / 2.9 4.19 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C50 H50 N4 P1 O6 Formula weight = 833.91 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.264, non-H atomic volume = 18.0 and following cell contents and analysis: C 100.00 72.01 % H 100.00 6.04 % N 8.00 6.72 % O 12.00 11.51 % P 2.00 3.71 % F(000) = 882.0 Mo-K(alpha) radiation Mu (mm-1) = 0.12 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/c CELL 0.71073 16.4377 7.8238 18.1284 90.000 109.971 90.000 ZERR 2.00 0.0033 0.0016 0.0036 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O P UNIT 100 100 8 12 2 TREF HKLF 4 END -------------------------------------------------------------------------------