++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 10:40:29 on 15-APR-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.657 12.171 12.486 86.56 85.94 77.23 18254 Reflections read from file s92.hkl; mean (I/sigma) = 6.62 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 9194 9109 9145 9160 13724 12115 12187 18254 N (int>3sigma) = 0 5366 5299 5393 5333 8029 7040 7067 10701 Mean intensity = 0.0 71.7 68.6 70.8 71.4 70.4 70.4 69.3 70.2 Mean int/sigma = 0.0 6.7 6.7 6.8 6.8 6.7 6.7 6.7 6.7 Lattice type: P chosen Volume: 1721.68 ------------------------------------------------------------------------------- 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: 11.657 12.171 12.486 86.56 85.94 77.23 Niggli form: a.a = 135.89 b.b = 148.14 c.c = 155.91 b.c = 9.12 a.c = 10.30 a.b = 31.37 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.070 [ 11932] Cell: 11.657 12.171 12.486 86.56 85.94 77.23 Volume: 1721.68 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 9194 9109 9145 9160 13724 12115 12187 18254 N (int>3sigma) = 0 5366 5299 5393 5333 8029 7040 7067 10701 Mean intensity = 0.0 71.7 68.6 70.8 71.4 70.4 70.4 69.3 70.2 Mean int/sigma = 0.0 6.7 6.7 6.8 6.8 6.7 6.7 6.7 6.7 Crystal system A and Lattice type P selected Mean |E*E-1| = 0.929 [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 0.070 11932 0.0 / 6.7 1.65 [B] P1 # 1 chiral 1 700 0.070 11932 0.0 / 6.7 5.34 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C33H25INO2Sb Formula weight = 716.19 Tentative Z (number of formula units/cell) = 2.0 giving rho = 1.382, non-H atomic volume = 22.7 and following cell contents and analysis: C 66.00 55.34 % H 50.00 3.52 % N 2.00 1.96 % O 4.00 4.47 % Sb 2.00 17.00 % I 2.00 17.72 % F(000) = 700.0 Mo-K(alpha) radiation Mu (mm-1) = 1.72 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in P-1 CELL 0.71073 11.6573 12.1713 12.4865 86.561 85.943 77.228 ZERR 2.00 0.0013 0.0012 0.0015 0.004 0.005 0.009 LATT 1 SFAC C H N O SB I UNIT 66 50 2 4 2 2 TREF HKLF 4 END -------------------------------------------------------------------------------