XPREP - RECIPROCAL SPACE EXPLORATION ------------------------------------- Original cell in Angstroms and degrees: 10.082 20.406 18.756 90.00 103.87 90.00 14500 reflections read from file S92.HKL Mean(I/sigma) = 6.86 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7256 7231 7285 7263 10886 9661 9672 14500 N (int>3sigma) = 0 4620 4611 4613 4648 6922 6236 6187 9281 Mean intensity = 0.0 701.5 706.8 700.6 693.2 703.0 714.9 702.2 704.7 Mean int/sigma = 0.0 6.9 6.9 6.9 6.9 6.9 7.0 6.9 6.9 Lattice type P chosen Volume: 3746.45 ------------------------------------------------------------------------------- Determination of reduced (Niggli) cell Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 10.082 18.756 20.406 90.00 90.00 103.87 Niggli form: a.a = 101.65 b.b = 351.80 c.c = 416.42 b.c = 0.00 a.c = 0.00 a.b = -45.34 ------------------------------------------------------------------------------- Search for higher METRIC symmetry ------------------------------------------------------------------------------- Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.071 [ 8519] Cell: 10.082 20.406 18.756 90.00 103.87 90.00 Volume: 3746.45 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------- Option B: FOM = 0.000 deg. TRICLINIC P-lattice R(int) = 0.064 [ 7124] Cell: 10.082 18.756 20.406 90.00 90.00 103.87 Volume: 3746.45 Matrix: -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Option A selected ------------------------------------------------------------------------------- Space group determination Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 7256 7231 7285 7263 10886 9661 9672 14500 N (int>3sigma) = 0 4620 4611 4613 4648 6922 6236 6187 9281 Mean intensity = 0.0 701.5 706.8 700.6 693.2 703.0 714.9 702.2 704.7 Mean int/sigma = 0.0 6.9 6.9 6.9 6.9 6.9 7.0 6.9 6.9 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.940 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 0 303 291 272 N I>3s 0 111 4 111 0.01087.3 28.61204.9 0.0 6.2 0.5 6.8 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2/c # 13 centro 1 292 0.071 8519 0.5 / 6.2 2.18 [B] Pc # 7 non-cen 1 226 0.071 8519 0.5 / 6.2 6.38 [C] P2(1)/c # 14 centro 1 19410 0.071 8519 0.5 / 6.2 1.84 Option [C] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C46H37O6Sb Formula weight = 807.54 Tentative Z (number of formula units/cell) = 4.0 giving rho = 1.432, non-H atomic volume = 17.7 and following cell contents and analysis: C 184.00 68.42 % H 148.00 4.62 % O 24.00 11.89 % Sb 4.00 15.08 % F(000) = 1648.0 Mo-K(alpha) radiation Mu (mm-1) = 0.79 ------------------------------------------------------------------------------- File S92.INS set up as follows: TITL S92 in P2(1)/c CELL 0.71073 10.082 20.406 18.756 90.00 103.87 90.00 ZERR 4.00 0.002 0.004 0.004 0.00 0.03 0.00 LATT 1 SYMM -X, .5+Y, .5-Z SFAC C H O SB UNIT 184 148 24 4 TREF HKLF 4 END -------------------------------------------------------------------------------