++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 11:30:54 on 23-JAN-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 13.341 11.709 14.291 90.00 115.86 90.00 10044 Reflections read from file s92.hkl; mean (I/sigma) = 6.12 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 5023 5026 5023 5009 7536 6701 6720 10044 N (int>3sigma) = 0 2555 2564 2523 2577 3821 3467 3431 5109 Mean intensity = 0.0 59.2 59.5 58.3 59.5 59.0 63.6 63.7 62.3 Mean int/sigma = 0.0 6.3 6.2 6.1 6.2 6.2 6.3 6.3 6.2 Lattice type: P chosen Volume: 2008.91 ------------------------------------------------------------------------------- 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: 11.709 13.341 14.291 115.86 90.00 90.00 Niggli form: a.a = 137.10 b.b = 177.98 c.c = 204.23 b.c = -83.15 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.086 [ 6072] Cell: 13.341 11.709 14.291 90.00 115.86 90.00 Volume: 2008.91 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 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 5023 5026 5023 5009 7536 6701 6720 10044 N (int>3sigma) = 0 2555 2564 2523 2577 3821 3467 3431 5109 Mean intensity = 0.0 59.2 59.5 58.3 59.5 59.0 63.6 63.7 62.3 Mean int/sigma = 0.0 6.3 6.2 6.1 6.2 6.2 6.3 6.3 6.2 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.933 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 6 273 285 282 N I>3s 0 3 99 96 0.3 2.2 69.1 70.0 0.3 0.6 4.8 4.8 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2(1)/c # 14 centro 4 19410 0.086 6072 0.6 / 4.8 2.47 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C18H28N2O2SSi Formula weight = 364.57 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.205, non-H atomic volume = 20.9 and following cell contents and analysis: C 72.00 59.30 % H 112.00 7.74 % N 8.00 7.69 % O 8.00 8.78 % Si 4.00 7.70 % S 4.00 8.79 % F(000) = 784.0 Mo-K(alpha) radiation Mu (mm-1) = 0.23 ------------------------------------------------------------------------------- File 1.ins set up as follows: TITL 1 in P2(1)/c CELL 0.71073 14.2910 11.7090 13.3411 90.000 115.857 90.000 ZERR 4.00 0.0029 0.0023 0.0027 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O SI S UNIT 72 112 8 8 4 4 TREF HKLF 4 END -------------------------------------------------------------------------------