++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 13:57:50 on 08-DEC-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.898 19.847 32.285 89.97 90.01 90.02 44265 Reflections read from file s92.hkl; mean (I/sigma) = 1.48 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 22110 22119 22049 22128 33139 29490 29546 44265 N (int>3sigma) = 0 3134 2959 2881 3234 4487 4158 4158 6338 Mean intensity = 0.0 3.8 3.7 3.1 3.9 3.6 3.8 3.8 3.7 Mean int/sigma = 0.0 1.8 1.7 1.7 1.8 1.7 1.8 1.8 1.8 Lattice type: P chosen Volume: 7624.18 ------------------------------------------------------------------------------- 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: 11.898 19.847 32.285 89.97 89.99 89.98 Niggli form: a.a = 141.57 b.b = 393.92 c.c = 1042.35 b.c = 0.28 a.c = 0.08 a.b = 0.08 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.031 deg. ORTHORHOMBIC P-lattice R(int) = 0.440 [ 37153] Cell: 11.898 19.847 32.285 89.97 90.01 90.02 Volume: 7624.18 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.022 deg. MONOCLINIC P-lattice R(int) = 0.397 [ 31839] Cell: 19.847 11.898 32.285 89.99 90.03 90.02 Volume: 7624.18 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.028 deg. MONOCLINIC P-lattice R(int) = 0.399 [ 32154] Cell: 11.898 32.285 19.847 89.97 90.02 90.01 Volume: 7624.18 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.031 deg. MONOCLINIC P-lattice R(int) = 0.403 [ 32151] Cell: 11.898 19.847 32.285 89.97 90.01 90.02 Volume: 7624.18 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.325 [ 23600] Cell: 11.898 19.847 32.285 89.97 89.99 89.98 Volume: 7624.18 Matrix: 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 Option A selected ------------------------------------------------------------------------------- Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 22110 22119 22049 22128 33139 29490 29546 44265 N (int>3sigma) = 0 3134 2959 2881 3234 4487 4158 4158 6338 Mean intensity = 0.0 3.8 3.7 3.1 3.9 3.6 3.8 3.8 3.7 Mean int/sigma = 0.0 1.8 1.7 1.7 1.8 1.7 1.8 1.8 1.8 Crystal system O and Lattice type P selected Mean |E*E-1| = 0.804 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: b-- c-- n-- 21-- -c- -a- -n- -21- --a --b --n --21 N 1464 1515 1509 14 872 862 842 26 482 532 524 36 N I>3s 3 270 267 0 139 138 1 0 0 104 104 0 0.8 13.5 13.6 0.6 4.0 4.0 0.9 0.9 0.6 5.0 5.1 0.7 0.5 2.2 2.2 0.4 2.0 2.0 0.5 0.7 0.5 2.6 2.6 0.4 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] Pbcn # 60 centro 5 571 0.440 37153 0.7 / 1.8 10.67 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C45 H45 O8 N4 Formula weight = 769.85 Tentative Z (number of formula units/cell) = 8.0 giving rho = 1.341, non-H atomic volume = 16.7 and following cell contents and analysis: C 360.00 70.20 % H 360.00 5.89 % N 32.00 7.28 % O 64.00 16.63 % F(000) = 3256.0 Mo-K(alpha) radiation Mu (mm-1) = 0.09 ------------------------------------------------------------------------------- File s93.ins set up as follows: TITL s93 in Pbcn CELL 0.71073 32.2854 11.8982 19.8475 90.000 90.000 90.000 ZERR 8.00 0.0024 0.0006 0.0011 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, 0.5-Y, 0.5+Z SYMM -X, Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O UNIT 360 360 32 64 TREF HKLF 4 END -------------------------------------------------------------------------------