b) From 2. A solution of 223 mg (0.216 mmol) of 2 in 10 mL of toluene was saturated with CO. The red microcrystalline 3, which precipitated after 8 h, was filtered and vacuum-dried.(c) From Pd(PCy,),. The absorption of CO by a solution containing 434 mg (0.652 mmol) of Pd (PCy,), in 20 mL of toluene was measured with a gas-volumetric apparatus; 0.645 mmol of CO was absorbed. From the solution a red microcrystalline solid precipitated, which was shown to be identical with a sample prepared by method a.X-ray Crystallography. Crystal data and details of measurements for 1 and 2 are reported in Table I. Diffraction intensities were collected at room temperature by the w/28 scan method of an Enraf-Nonius CAD-4 diffractometer with Mo K a radiation (A = 0.71069 A) and reduced to F, values.The structures were solved by Patterson and direct methods and refined by full-matrix least-squares calculations. For all computations the SHELX76 and SHELX86I3*l4 packages of crystallographic programs were used with the analytical scattering factors, corrected for real and imaginary parts of anomalous dispersions, taken from ref 14b. Thermal vibrations were treated anisotropically.In both compounds the H atoms bound to Pd(I1) were found in a final difference map by using a reduced reflection sphere ((sin 8)/A = 0.3) and kept at their observed distances [ 1.57 (2) and 1.46 (2) A, respectively] from Pd. Also, the phenol and pentafluorophenol 0-bound H atoms were directly located and kept at their found positions of 1.18 and 0.89 A, respectively, from 043. All the remaining H atoms were added in calculated positions (C-H = 1.08 A) and refined riding on the corresponding C atoms. Common temperature factors were refined for chemically equivalent H atoms, while the H(hydride) and H(bridging) atoms were treated independently.Final difference Fourier maps showed residual peaks lower than 1 e A-' in both compounds. Final atomic coordinates for 1 and 2 are listed in Tables I1 and 111, while relevant bond distances and angles are reported in Table IV. Absorption correction was made by applying the Walker and Stuartls method after a complete structural model was obtained and all atoms were refined isotropically for 1. For 2 an empirical absorption correction was applied by measuring scans at intervals of IOo around the diffraction vectors of eight selected reflections near x = 90' (transmission range Registry No. 1, 112469-70-2: 2, 119455-96-8; 3 ( n = 3), 95246-51-8; 7 l-lOO%). Pd(PCy,),, 33309-88-5; PhOH, 108-95-2; C,F,OH, 771-61-9: CH,OH, 67-56-1; i-PrOH, 67-63-0. Supplementary Material Available: Hydrogen atom coordinates (Tables S-I and S-II), anisotropic thermal parameters (Tables S-I11 and S-IV), bond distances and angles (Tables S-V and S-VI), and crystal data and intensity collection parameters (Table S-IX) (74 pages); observed and calculated structural factors (Tables S-VI1 and S-VIII) (78 pages). Ordering information is given on any current masthead page. (15) Walker, N.: Stuart, D. Acta Crystallogr., Sect. A 1983, 158. Acid dissociati...
