++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + 97src139 started at 15:40:18 on 13-SEP-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 11.817 5.983 31.689 90.00 97.34 90.00 8492 Reflections read from file 97src139.hkl; mean (I/sigma) = 9.83 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4258 4158 4210 3948 6313 5662 5679 8492 N (int>3sigma) = 0 2906 2715 2891 2493 4256 3866 3899 5815 Mean intensity = 0.0 57.6 58.8 57.6 42.8 58.0 57.9 57.7 57.2 Mean int/sigma = 0.0 9.8 9.7 9.9 8.3 9.8 9.9 9.9 9.8 Lattice type: P chosen Volume: 2222.09 ------------------------------------------------------------------------------- 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: 5.983 11.817 31.689 97.34 90.00 90.00 Niggli form: a.a = 35.80 b.b = 139.64 c.c = 1004.19 b.c = -47.84 a.c = 0.00 a.b = 0.00 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC P-lattice R(int) = 0.138 [ 4974] Cell: 11.817 5.983 31.689 90.00 97.34 90.00 Volume: 2222.09 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) = 0.138 [ 2745] Cell: 5.983 11.817 31.689 82.66 90.00 90.00 Volume: 2222.09 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 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 4258 4158 4210 3948 6313 5662 5679 8492 N (int>3sigma) = 0 2906 2715 2891 2493 4256 3866 3899 5815 Mean intensity = 0.0 57.6 58.8 57.6 42.8 58.0 57.9 57.7 57.2 Mean int/sigma = 0.0 9.8 9.7 9.9 8.3 9.8 9.9 9.9 9.8 Crystal system M and Lattice type P selected Mean |E*E-1| = 0.904 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -21- -a- -c- -n- N 5 322 325 213 N I>3s 2 167 170 3 7.2 78.8 78.4 1.6 3.5 11.2 11.1 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] P2/n # 13 centro 1 292 0.138 4974 0.5 / 3.5 4.02 [B] Pn # 7 non-cen 1 226 0.138 4974 0.5 / 3.5 6.55 [C] P2(1)/n # 14 centro 1 19410 0.138 4974 3.5 / 9.8 1.70 Option [C] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C14H8Hg1N2S4 Formula weight = 533.05 Tentative Z (number of formula units/cell) = 5.0 giving rho = 1.992, non-H atomic volume = 21.2 and following cell contents and analysis: C 70.00 31.54 % H 40.00 1.51 % N 10.00 5.26 % S 20.00 24.06 % Hg 5.00 37.63 % F(000) = 1250.0 Mo-K(alpha) radiation Mu (mm-1) = 9.12 ------------------------------------------------------------------------------- File 97src139.ins set up as follows: TITL 97src139 in P2(1)/n CELL 0.71073 11.8170 5.9830 31.6890 90.000 97.340 90.000 ZERR 5.00 0.0024 0.0012 0.0063 0.000 0.030 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N S HG UNIT 70 40 10 20 5 TREF HKLF 4 END 8492 Reflections written to new reflection file 97src139.hkl -------------------------------------------------------------------------------