Experimental. Elemental analysis: calculated for C7H3NO4Pb: (Mr=372.29) C, 22.56; H, 0.81; N, 3.76%. Found:C,22.47; H, 0.89; N, 3.85%. IR data (cm-1): 3429(s), 1602(s), 1579(s), 1551(s), 1459(w), 1385(s), 1276(w), 1236(w), 1105(m), 871(m), 825(m), 779(m), 711(s), 700(m), 660(m), 603(w), 534(w), 443(w). |
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Refinement. Refinement on F2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. |