X-ray powder diffraction data for RuCI 2 (TRIPHOS)(DMSO) dichioro [bis(2-diphenylphosphinoethyl) phenylphosphine] [dimethylsulfoxide] ruthenium (II) Gerzon Delgado, A. Valentina Rivera, Trino Suarez, and Bernardo Fontal Departamento de Quimica, Facultad de Ciencias, Universidad de Los Andes Merida, Merida 5101, Venezuela (Received 12 August 1994; accepted for publication 15 November 1994) X-ray powder diffraction data for Dichioro [bis(2-diphenylphosphinoethyl) phenylphosphine] [dimethylsulfoxide] Ruthenium (II) is reported. The powder pattern was obtained using CuKa radiation. The lattice parameters determinated by least-squares refinement for the monoclinic space group P2 x lc are: a = 21.073(3) A, b= 11.970(2) A, c= 16.889(3) A, and /3= 107.72(1)°, with M 20 = 10.67 and F 30 = 15.4 (0.0145, 134), and are in good agreement with those obtained from the single crystal structure determination. Observed and calculated X-ray powder diffraction data are given for the titled compound. I. INTRODUCTION The ruthenium complex RuCl 2 (TRIPHOS)(DMSO) pre- sents interesting catalytic activity. It catalyzes the homoge- neous hydrogenation and isomerization of olefins, hydroge- nation of alkines, aldehydes, ketones, and nitriles, under moderate reaction conditions in different organic solvents (Suarez and Fontal, 1988). The X-ray structure determination, was carried out using single-crystal difractometry by Delgado et al. (1994). The structure consists of discrete molecules of the complex and solvent held together by normal van der Waals forces. Single-crystal data obtained for RuCl 2 (TRIPHOS)(DMSO) reveals that the complex crystallizes in the monoclinic space group P2 x lc [C\ h ,N°\A], with a = 2\. 070(5) A, fc= 11.968(3) A, c= 16.892(4) A, (3= 107.7(2)°, V=4057.2 A 3 , Z = 4, D m =\A5 gr/cm 3 , /? = 4.88% (/? w = 4.82%) for 4184 unique reflections with />3o-(/). This paper details how the powder data of this compound were obtain and indexed. II. EXPERIMENTAL DATA The synthesis of the complex was carried out by reacting RuCl 2 (DMSO) 4 with a equimolar quantity of TRIPHOS [PhP(CH 2 CH 2 PPh 2 ) 2 ] (see Figure 1) in dry toluene. A small quantity of the yellow beige precipitate obtained was ground mechanically in an agate mortar. The resulting fine powder was mounted using the side-loading technique of McMurdie et al. (1986), but with no diluent added, and placed into a Rigaku D/Max-IIIB Diffractometer. The X-ray source was operated at 30 KV and 15 mA, and the instrumental conditions were as follows: \= 1.54059 A graphite scintillation 0.3 mm 0.01° 17min 0.02° 2616 2° to 60° ^uivu| radiation, monochromator: detector: receiving slits: step size: scan speed: step/sample: scan mode: range of 26: The position of the peaks was established using the a { component. The a 2 component was stripped mathematically using the difractometer software. III. RESULTS Table I shows the powder diffraction data for RuCl 2 (TRIPHOS)(DMSO). The observed 26 values of 48 reflections from the powder pattern were used as input to the least-squares unit cell parameter refinement and indexing program NBS*AIDS (Mighell et al, 1981) modified for a PC computer by Garvey (1992) in the PDFEAPC program. The lattice parameters obtained are as follows: a = 21.073(3)A, b= 11.970(2)A, c=16.889(3)A, and /?= 107.72(1)°; with figures of merit: M 20 =10.7 (de Wolf, 1968) F 30 = 15.4(0.0145,134) (Smith and Snyder, 1979) and are in agreement with the single-crystal unit cell param- eters. In general, the observed and calculated patterns are very similar (Table I) with a maximum 26 difference, A(20), of 0.045°, and good agreement in intensities. P-CH 2 CH 2 -P-CH 2 CH 2 -P Figure 1. TRIPHOS [bis(2-diphenylphosphinoethyl) phenylphosphine]. 178 Powder Diffraction 10 (3), September 1995 0885-7156/95/10(3)/178/2/$6.00 > 1995 JCPDS-ICDD 178