++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 10:49:14 on 29-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 24.800 16.681 24.906 90.00 107.16 90.00 97906 Reflections read from file s92.hkl; mean (I/sigma) = 4.01 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 48933 48874 48919 48956 73363 65306 65295 97906 N (int>3sigma) = 0 17506 18077 17979 18105 26781 23793 23930 35997 Mean intensity = 0.0 16.5 17.7 19.0 18.4 17.7 18.3 18.8 18.4 Mean int/sigma = 0.0 4.0 4.1 4.2 4.2 4.1 4.1 4.2 4.2 Lattice type: P chosen Volume: 9844.19 ------------------------------------------------------------------------------- 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: 16.681 24.800 24.906 107.16 90.00 90.00 Niggli form: a.a = 278.24 b.b = 615.03 c.c = 620.29 b.c = -182.24 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.256 deg. ORTHORHOMBIC C-lattice R(int) = 0.660 [ 87470] Cell: 29.510 39.998 16.681 90.00 90.00 89.74 Volume: 19688.38 Matrix: 1.0000 0.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.161 [ 77858] Cell: 24.800 16.681 24.906 90.00 107.16 90.00 Volume: 9844.19 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.256 deg. MONOCLINIC C-lattice R(int) = 0.641 [ 78115] Cell: 39.998 29.510 16.681 90.00 90.00 90.26 Volume: 19688.38 Matrix: 1.0000 0.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.256 deg. MONOCLINIC C-lattice R(int) = 0.647 [ 78218] Cell: 29.510 39.998 16.681 90.00 90.00 89.74 Volume: 19688.38 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.147 [ 60932] Cell: 16.681 24.800 24.906 72.84 90.00 90.00 Volume: 9844.19 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 Option B selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 48933 48874 48919 48956 73363 65306 65295 97906 N (int>3sigma) = 0 17506 18077 17979 18105 26781 23793 23930 35997 Mean intensity = 0.0 16.5 17.7 19.0 18.4 17.7 18.3 18.8 18.4 Mean int/sigma = 0.0 4.0 4.1 4.2 4.2 4.1 4.1 4.2 4.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.942 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 29 2163 2155 2136 N I>3s 22 655 3 652 133.3 33.1 0.7 33.5 12.6 4.6 0.5 4.6 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2/c # 13 centro 1 292 0.161 77858 0.5 / 4.2 3.11 [B] Pc # 7 non-cen 1 226 0.161 77858 0.5 / 4.2 7.37 Option [A] chosen ------------------------------------------------------------------------------- Input space group symbol: P2(1)/c Number: 14 centrosymmetric CSD frequency: 19410 R(int) = 0.161 77858 reflections merged Systematic absence exceptions: -21- -a- -c- -n- N 29 2163 2155 2136 N I>3s 22 655 3 652 133.3 33.1 0.7 33.5 12.6 4.6 0.5 4.6 ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C54 H60 O6 N2 Formula weight = 833.04 Tentative Z (number of formula units/cell) = 9.0 giving rho = 1.265, non-H atomic volume = 17.6 and following cell contents and analysis: C 486.00 77.85 % H 540.00 7.26 % N 18.00 3.36 % O 54.00 11.52 % F(000) = 4014.0 Mo-K(alpha) radiation Mu (mm-1) = 0.08 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P2(1)/c CELL 0.71073 24.7998 16.6806 24.9057 90.000 107.161 90.000 ZERR 9.00 0.0050 0.0033 0.0050 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 486 540 18 54 TREF HKLF 4 END -------------------------------------------------------------------------------