++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 10:45:57 on 03-JUL-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.686 18.643 15.560 90.00 104.50 90.00 22831 Reflections read from file s92.hkl; mean (I/sigma) = 2.94 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 11375 11445 11394 11395 17107 15230 15248 22831 N (int>3sigma) = 0 3779 3635 3718 3599 5566 4953 5017 7493 Mean intensity = 0.0 9.9 9.3 9.3 9.4 9.5 9.6 9.4 9.5 Mean int/sigma = 0.0 3.1 3.0 3.1 3.0 3.1 3.1 3.1 3.1 Lattice type: P chosen Volume: 2720.27 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 9.686 15.560 18.643 90.00 90.00 104.50 Niggli form: a.a = 93.82 b.b = 242.12 c.c = 347.56 b.c = 0.00 a.c = 0.00 a.b = -37.74 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.202 [ 16715] Cell: 9.686 18.643 15.560 90.00 104.50 90.00 Volume: 2720.27 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) = 0.175 [ 12148] Cell: 9.686 15.560 18.643 90.00 90.00 104.50 Volume: 2720.27 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 11375 11445 11394 11395 17107 15230 15248 22831 N (int>3sigma) = 0 3779 3635 3718 3599 5566 4953 5017 7493 Mean intensity = 0.0 9.9 9.3 9.3 9.4 9.5 9.6 9.4 9.5 Mean int/sigma = 0.0 3.1 3.0 3.1 3.0 3.1 3.1 3.1 3.1 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.927 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 22 413 412 417 N I>3s 0 110 111 3 0.9 12.8 12.9 0.7 0.7 2.9 2.9 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/n # 14 centro 1 19410 0.202 16715 0.7 / 2.9 4.27 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C42 H40 N4 P1 O6 S1 Formula weight = 759.81 Tentative Z (number of formula units/cell) = 3.0 giving rho = 1.391, non-H atomic volume = 16.8 and following cell contents and analysis: C 126.00 66.39 % H 120.00 5.31 % N 12.00 7.38 % O 18.00 12.63 % P 3.00 4.08 % S 3.00 4.22 % F(000) = 1197.0 Mo-K(alpha) radiation Mu (mm-1) = 0.19 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/n CELL 0.71073 9.6860 18.6429 15.5603 90.000 104.503 90.000 ZERR 3.00 0.0019 0.0037 0.0031 0.000 0.030 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O P S UNIT 126 120 12 18 3 3 TREF HKLF 4 END -------------------------------------------------------------------------------