Crystal structure of bis(phenylethynyl)tetrakis(dimethylphenylphos- phine)ruthenium(II), C 48 H 54 P 4 Ru Frederick P. Malan, Eric Singleton and Reinout Meijboom * Research Centre for Synthesis and Catalysis, Department of Chemistry, University of Johannesburg, P. O Box 524, Auckland Park, 2006, Johannesburg, South Africa Received January 23, 2014, accepted May 15, 2014, available online May 28, 2014, CCDC no. 1267/4112 Abstract C 48 H 54 P 4 Ru, triclinic, P1 (no. 2), a = 12.029(5) Å, b = 13.439(5) Å, c = 14.582(7) Å, a = 79.962(17)°, b = 80.974(18)°, g = 71.343(13)°, V = 2186.2 Å 3 , Z = 2, R gt (F) = 0.0416, wR ref (F 2 ) = 0.1067, T = 223 K. Source of material All reagents were obtained from Sigma-Aldrich and used without fur ther pu ri fi ca tion. The pre cur sor com plex, [RuH(PMe 2 Ph) 5 ](PF 6 ), was synthesised according to literature procedures [3]. The latter complex (293 mg, 0.3 mmol) was re- acted with 2.1 molar equivalents of phenylacetylene in boiling MeOH in air. A clear light yellow solution was obtained from which yellow prisms crystallized overnight (144 mg, 54%). Experimental details The aromatic H atoms were placed in geometrically idealized po- sitions (C–H = 0.97 Å) and constrained to ride on their parent at- oms, with U iso (H) = 1.2U eq (C) for all H atoms. The highest calculated residual electron density is 0.56 e×Å –3 at 1.54 Å from C104, which bears no physical meaning. Discussion Ongoing research in s-alkynyl-metal complexes is stimulated by their expanded use in nonlinear optics, luminescence, and liquid crystalline materials brought about by their rigid linear structures, intrinsic stability and unique p-electron configurations [4, 5]. As seen in the figure, the Ru atom exhibits an slightly disordered oc- tahedral geometry with P1–Ru1–P3 = 92.094(2)°, P1–Ru1–P4 = 91.702(2)°, P2–Ru1–P3 = 91.753(2)°, and P1–Ru1–C9 = 90.763(2)°. The two acetylide moieties are coordinated trans to each other (C1–Ru1–C9 = 177.072(3)°), with the four remaining PMe 2 Ph occupying the same plane. An average Ru–C and Ru–P bond length of 2.07 Å and 2.38 Å, respectively are comparable to the similar complex trans-[Ru(C 8 H 5 ) 2 (PMe 3 ) 4 ] reported by Field et al. [6]. Z. Kristallogr. NCS 229 (2014) xxx-xxx / DOI 10.1515/ncrs-2014-0109 1 © 2014 by Walter de Gruyter Berlin/Boston Crystal: colourless prisms, size 0.2´0.2´0.2 mm Wavelength: Mo K a radiation (0.71075 Å) m: 5.37 cm -1 Diffractometer, scan mode: Rigaku XtaLAB mini, w 2q max : 55.02° N(hkl) measured , N(hkl) unique : 12594, 9760 Criterion for I obs , N(hkl) gt : I obs > 2 s(I obs ), 8187 N(param) refined : 486 Programs: SHELX [1], OLEX2 [2] Table 1. Data collection and handling. _____________ * Correspondence author (e-mail: rmeijboom@uj.ac.za) H(20A) 2i 0.9123 0.0791 0.5671 0.088 H(20B) 2i 1.0518 0.0384 0.5612 0.088 H(20C) 2i 0.9870 0.1546 0.5156 0.088 H(104) 2i 0.5769 0.1990 0.8425 0.067 H(7) 2i 0.5175 -0.1529 0.8213 0.080 H(30A) 2i 1.0203 0.1564 0.8807 0.083 H(30B) 2i 0.9686 0.2076 0.9743 0.083 H(30C) 2i 0.9950 0.2796 0.8804 0.083 H(20D) 2i 1.0009 0.0307 0.8172 0.078 H(20E) 2i 1.0666 -0.0295 0.7306 0.078 H(20F) 2i 0.9279 -0.0028 0.7531 0.078 H(208) 2i 1.0742 0.3090 0.7145 0.062 H(4) 2i 0.7193 -0.0188 0.5564 0.063 H(6) 2i 0.5637 -0.2362 0.6877 0.081 H(308) 2i 0.7689 0.0488 0.8580 0.058 H(205) 2i 1.4034 0.0383 0.6230 0.069 H(204) 2i 1.2166 0.0229 0.6262 0.060 H(306) 2i 0.7101 -0.0926 1.1197 0.084 H(8) 2i 0.5705 -0.0022 0.8227 0.061 H(206) 2i 1.4275 0.1852 0.6687 0.079 H(307) 2i 0.7290 -0.0922 0.9593 0.073 H(30D) 2i 0.7538 0.4189 0.9097 0.095 H(30E) 2i 0.7713 0.3408 1.0047 0.095 H(30F) 2i 0.6569 0.3625 0.9541 0.095 H(404) 2i 0.6715 0.2368 0.5407 0.081 H(5) 2i 0.6621 -0.1672 0.5552 0.080 Table 2. Atomic coordinates and displacement parameters (in Å 2 ). Atom Site x y z U iso Unauthenticated | 152.106.99.20 Download Date | 7/8/14 10:36 AM