++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 13:54:08 on 04-DEC-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 8.803 9.681 10.862 83.99 71.84 78.35 12927 Reflections read from file s92.hkl; mean (I/sigma) = 9.60 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 6470 6467 6473 6458 9705 8609 8633 12927 N (int>3sigma) = 0 4654 4688 4660 4665 7001 6247 6228 9372 Mean intensity = 0.0 142.4 142.0 145.0 133.7 143.1 137.1 137.7 139.6 Mean int/sigma = 0.0 9.6 9.7 9.6 9.7 9.6 9.7 9.6 9.6 Lattice type: P chosen Volume: 860.60 ------------------------------------------------------------------------------- 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: 8.803 9.681 10.862 83.99 71.84 78.35 Niggli form: a.a = 77.49 b.b = 93.72 c.c = 117.99 b.c = 11.01 a.c = 29.80 a.b = 17.21 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.057 [ 9067] Cell: 8.803 9.681 10.862 83.99 71.84 78.35 Volume: 860.60 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 6470 6467 6473 6458 9705 8609 8633 12927 N (int>3sigma) = 0 4654 4688 4660 4665 7001 6247 6228 9372 Mean intensity = 0.0 142.4 142.0 145.0 133.7 143.1 137.1 137.7 139.6 Mean int/sigma = 0.0 9.6 9.7 9.6 9.7 9.6 9.7 9.6 9.6 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.940 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absences not required for triclinic Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P-1 # 2 centro 1 8646 0.057 9067 0.0 / 9.6 1.13 [B] P1 # 1 chiral 1 700 0.057 9067 0.0 / 9.6 5.35 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C21 O6 H29 S1 N3 Formula weight = 451.53 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.742, non-H atomic volume = 13.9 and following cell contents and analysis: C 42.00 55.86 % H 58.00 6.47 % N 6.00 9.31 % O 12.00 21.26 % S 2.00 7.10 % F(000) = 480.0 Mo-K(alpha) radiation Mu (mm-1) = 0.24 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P-1 CELL 0.71073 8.8031 9.6811 10.8622 83.989 71.839 78.348 ZERR 2.00 0.0018 0.0019 0.0022 0.030 0.030 0.030 LATT 1 SFAC C H N O S UNIT 42 58 6 12 2 TREF HKLF 4 END -------------------------------------------------------------------------------