++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 11:49:22 on 03-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 9.540 13.248 28.592 89.93 81.27 89.74 62283 Reflections read from file s92.hkl; mean (I/sigma) = 7.09 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 31162 31166 31020 31137 46674 41495 41522 62283 N (int>3sigma) = 0 20049 20222 20077 20281 30174 26929 27037 40633 Mean intensity = 0.0 34.0 35.5 34.9 35.0 34.8 35.3 34.9 35.0 Mean int/sigma = 0.0 7.0 7.1 7.1 7.1 7.1 7.1 7.1 7.1 Lattice type: P chosen Volume: 3571.60 ------------------------------------------------------------------------------- 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: 9.540 13.248 28.592 89.93 81.27 89.74 Niggli form: a.a = 91.01 b.b = 175.50 c.c = 817.48 b.c = 0.49 a.c = 41.39 a.b = 0.58 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.912 deg. ORTHORHOMBIC C-lattice R(int) = 0.539 [ 57650] Cell: 9.540 56.527 13.248 90.03 89.74 89.13 Volume: 7143.20 Matrix: 1.0000 0.0000 0.0000 1.0000 0.0000 -2.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.265 deg. MONOCLINIC P-lattice R(int) = 0.075 [ 53711] Cell: 9.540 13.248 28.592 90.07 98.73 89.74 Volume: 3571.60 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.874 deg. MONOCLINIC C-lattice R(int) = 0.533 [ 53918] Cell: 9.540 56.527 13.248 89.97 90.26 89.13 Volume: 7143.20 Matrix:-1.0000 0.0000 0.0000 -1.0000 0.0000 2.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option D: FOM = 0.912 deg. MONOCLINIC C-lattice R(int) = 0.531 [ 53520] Cell: 56.527 9.540 13.248 90.26 90.03 90.87 Volume: 7143.20 Matrix: 1.0000 0.0000 -2.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option E: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.062 [ 45935] Cell: 9.540 13.248 28.592 89.93 81.27 89.74 Volume: 3571.60 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 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 31162 31166 31020 31137 46674 41522 41495 62283 N (int>3sigma) = 0 20049 20222 20077 20281 30174 27037 26929 40633 Mean intensity = 0.0 34.0 35.5 34.9 35.0 34.8 34.9 35.3 35.0 Mean int/sigma = 0.0 7.0 7.1 7.1 7.1 7.1 7.1 7.1 7.1 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.892 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 48 1488 1465 1469 N I>3s 0 720 197 721 0.5 44.6 1.5 45.3 0.5 6.0 1.5 6.2 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 1 19410 0.075 53711 1.5 / 6.0 2.82 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C42H45O2Sb Formula weight = 703.53 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.308, non-H atomic volume = 19.8 and following cell contents and analysis: C 168.00 71.70 % H 180.00 6.45 % O 8.00 4.55 % Sb 4.00 17.31 % F(000) = 1456.0 Mo-K(alpha) radiation Mu (mm-1) = 0.81 ------------------------------------------------------------------------------- File 1.ins set up as follows: TITL 1 in P2(1)/c CELL 0.71073 9.5400 13.2477 28.5916 90.000 98.729 90.000 ZERR 4.00 0.0019 0.0026 0.0057 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O SB UNIT 168 180 8 4 TREF HKLF 4 END -------------------------------------------------------------------------------