摘要:
J. CHEM. SOC. DALTON TRANS. 1995 1251Synthesis of Complexes [Au( PPh,)L]' (L = Primary,Secondary or Tertiary Amine). Crystal Structure of[Au( PPh,j( NMe,)][CIO,].CH,Cl,tJose Vicente,*ea Maria-Teresa Chicote,*s8 Rita Guerreroa and Peter G. Jones * s i ba Grupo de Quimica Organometalica, Departamento de Quimica Jnorganica, Facultad de Quimica,Universidad de Murcia, Aptdo. 4021, E-30071 Murcia, Spain38023 Braunschweig, Germanylnstitut fur Anorganische und AnaJytische Chernie, Technische Universitat Braunsch weig, Postfach 3329,The 1 :1 reaction of [Au(acac)(PPh,)] (Hacac = acetylacetone) with ammonium salts [HLIX(X = CF,SO,, L = 2-nitroaniline, 4-methoxyaniline, NHPh, or NHEt,; X = CIO,, L = NMe,) in diethyl ethergave complexes [Au( PPh,)L]X and acetylacetone. The crystal structure of [Au( PPh,) (NMe,)] [CIO,] wasdetermined; orthorhombic, space group P2,2,2,.a = 9.498(2), b = t0.322(2), c = 26.1 54(4) A, wR(F2)0.091. The gold atom is linearly co-ordinated to both ligands [Au-P 2.231 (2), Au-N 2.1 08(7) A, P-Au-N179.3(2)"] and no intermolecular Au Au contacts exist.Gold(1) complexes with neutral N-donor ligands are much lesscommon than those with P-donor ligands because of the softacid nature of the metal centre. For instance, [AuX(ER,)] and[Au(ER,),]+ complexes with E = P are known for a widerange of X and R groups,' whereas, as far as we are aware, onlyone complex of each type with E = N has been reported,namely the rather unstable [AuCl@ip)] (pip = piperidine) and[Au(pip),] + . Therefore, mixed complexes [Au(PR,)(NR',)] +might be expected to be of intermediate stability. However, onlya few such complexes have been described with full experimentalor spectroscopic details., Only one of them [Au(PPh,)-(qncd)]BFq (qncd = quinuclidine) 3d has been characterizedby X-ray diffraction methods.These complexes are prepared(usually in low yields) by the reaction of [AuX(PR,)] with thecorresponding amine, where X is C104-, BF,- or NO3-. Wereport in this paper a method to prepare some related mixed-ligand complexes and the crystal structure of one of them.Results and DiscussionBy reacting [Au(acac)(PPh,)] (Hacac = acetylacetone) withammonium salts WHRR',]X (1 : l), the cationic complexes[Au(PPh,)(NRR',)]X (X = ClO,, R = R' = Me 1; X =NO2-2, R' = H 4; R = C6H40Me-4, R' = H 5) can be isolated[equation (l)].Except for 4, all complexes were obtained inCF3SO3, R = H, R' = Et 2; R = H, R' = Ph 3; R = C6H4-[Au(acac)(PPh,)] + [NHRR',]X --+Hacac + [Au(PPh,)(NRR',)]X (1)high yield (78-95%).The result of these reactions depends on the nature of thesolvent. Thus, acetone could only be used in the case of thesynthesis of the tertiary amine complex 1, while a mixture ofcomplexes is obtained for primary and secondary amines. We~~~~~~~~~~~~~~t Gold(r) Complexes with N-Donor Ligands. Part 1.Supplementary data available: Full details have been deposited at theFachinformationszentrum Karlsruhe, Gesellschaft fur Wissenschaft-lichtechnische Information mbH, D-76344 Eggenstein-Leopoldshafen,Germany. Any request for this material should quote a full literaturecitation and the reference number CSD 401358.assume that complexes 2-5, behaving as ammonium salts,react rapidly in acetone with [Au(acac)(PPh,)] to give gold(])complexes with bridging amido or imido ligands [equations(2X4)I.[Au(acac)(PPh,)] + [Au(PPh,)(NHR',)]X - Hacac + [(AuPP~,)~(~-NR'~)]X (2)[Au( acac)( PPh ,)I + [Au( PPh,)( NH R)] X --+Hacac + [(AuPPh,),(p-NHR)]X (3)[Au(acac)( PPh,)] + [( AuPPh,), (p-NHR)]X - Hacac + [(AuPPh,),(l,-NR)]X (4)Examples of these aurioammonium salts, i.e.one diaurio-ammonium salt [(AuPP~,),(~-NHC~H,NO~-~)]BF+,~ andseveral triaurioammonium salts [( AuPPh ,) , (p,-NR)] BF,(R = alkyl or aryl) have been de~cribed.~.' The tendency ofgold(1) to establish weak intramolecular Au Au bondinginteractions (aurophilicity) in these di- or tri-nuclear com-plexes is probably the reason why they are much more stablethan complexes 1-5, which slowly decompose in the solid stateand in solution. This is also likely to be the reason for theformation of the very stable [(AuPPh3),(p4-N)]BF4 ' and thehypervalent [(AUPP~,)~(~~-N)]BF~ * complexes. Althoughthis stabilizing aurophilicity can also lead to intermolecularAu Au interactions,6 these were not observed in the onlypreviously reported crystal structure of a monoaurioammoniumsalt [A~(PPh,)(qncd)lBF,,~~ or in complex 1 (see below).The success of reactions leading to complexes 2-4 relied onthe use of diethyl ether because of the solubility of theammonium trifluoromethanesulfonates and [Au(acac)(PPh,)]and the insolubility of the resulting complexes in this solvent.Probably, the rapid precipitation of complexes 2-4 allows thecorresponding reactions to be performed without specialprecautions against atmospheric moisture and preventsreactions (2H4).In those reported methods where reactionconditions were indicated,3bd a dinitrogen atmosphere wasused. Careful precautions to eliminate all traces of moisturefrom the reactants proved to be vital for the generation of[A~(PPh,)(qncd)lBF,.~~ In the presence of water, the reactionbetween quinuclidine and [Au(PPh,)]BF, gives quinuclidiniumand [(AuPPh,),O] 1252 J. CHEM. SOC. DALTON TRANS. 1995p> AuPPh3 - ( i )RI RC(O)CH$Pb ci)02R = R' = CN or C02MeS-Au-S -2CSH4NSH-2 (v)_ [cN N9]Scheme 1 (i) +[Au(acac)(PPh,)] - Hacac; (ii) +2[Au(acac)(PPh,)] - 2 Hacac; (iii) +3[Au(acac)L] (L = PPh,) - 3Hacac; (iu) + 4 [Au(acac)L] (L = PMe,Ph) - 4 Hacac; ( u ) +[Au(acac),]- - 2 HacacThis is a new example of the utility of acetylacetonatogold(1)complexes as starting materials for the synthesis of gold(1)complexes (see Scheme l).' We have previously used[Au(acac)(PPh,)] to prepare mono-, di-, tri- and tetra-nucleargold(r) complexes.More recently Laguna and co-workershave also found interesting synthetic applications for[Au(acac)(PPh,)].All complexes behave in solution as 1 : 1 electrolytes." TheIR spectra of complexes 2,4 and 5 show v(NH) in the region3214-3092 cm-'.For complex 3, v(NH) could not be assignedbecause only very weak bands in this region were observed.Structure of Complex 1.-The structure of complex 1 (see Fig.1 and Table 1) consists of the cation [Au(PPh,)(NMe,)]+, aperchlorate anion and a dichloromethane molecule. In thecation the gold atom is linearly co-ordinated [P-Au-N179.3(2)"]. The Au-N and Au-P bond distances [2.108(7) and2.231(2) A, respectively] are similar to those in the complex[Au(PPh,)(qncd)]BF, 3d [2.11(1) and 2.240(4) A, respectively].The cationic nature of 1 and the large PPh, groups are probablyresponsible for the absence of Au Au contacts.ExperimentalThe IR, C, H and N analyses, conductance measurements andmelting point determinations were carried out as describedel~ewhere.~ The NMR spectra were recorded in CDCl, on aVarian Unity 300 spectrometer and conductivity measure-ments were carried out in acetone.Chemical shifts are referredto SiMe, ('H and 13C) or external H3PO4 (,'P). Thefollowing reagents were commercially available: CF,SO,H,NH,(C6H,0Me-4) (Merck), LXHMe,]Cl (Fluka), NHEt,,NH,(C6H4N0,-2) (Aldrich), NHPh, (Probus). The compound[Au(acac)(PPh,)] was prepared following a literature method.Syntheses.-~HMe,][ClO, 1. To a solution of [NHMe,]Cl(1 g, 10.46 mmol) in acetone (20 cm3) was added NaC104-H,0(1.47 g, 10.46 mmol) and the suspension stirred for 30 min.It was then filtered through Celite, the resulting solutionconcentrated (2 cm3) and diethyl ether (20 cm3) added toprecipitate ~HMe,][C10,] (1.33 g, 92%) as a white solidwhich was washed with diethyl ether (2 x 5 cm3) and air dried.M.p.234 "C (Found: C, 22.65; H, 6.50; N, 8.55. Calc. forC3HloC1NO4: C, 22.60; H, 6.30; N, 8.80%). A M = 146 Q-' cm2mol-' (1.35 x lo-, mol dm-,). NMR: 'H, 6 3.12 (s, 9 H, Me),4.16 (br, 1 H, NH). IR: v(NH) 3 128 cm-' .[NH,Et,][CF,SO,]. To a solution of NHEt, (98%, 1 cm3,9.47 mmol) in diethyl ether (20 cm3) H03SCF, (Merck, 0.83t,Fig. 1 The structure of complex 1Table 1 Selected bond lengths (A) and angles (") for compound 1Au-N 2.108(7) Au-P 2.23 l(2)P-C( 2 1 ) 1.804( 10) P-C( 1 1) 1.804(9)P-C(3 1 ) 1.807(9) N-C( 2) 1.472( 12)N-C( 3) 1.482(11) N-C( 1 ) 1.487( 10)C(21 jP-C(31) 104.5(4) C(lI)-P-C(31) 105.7(4)c(31bP-A~ 112.5(3) C(2)-N-C(3) 108.6(7)N-Au-P 179.3(2) C(21)-P-C( 11) 107.9(4)C(21)-P-Au 113.0(3) C(l l)-P-Au 112.6(3)C(2)-N-C( 1) 109.1(8) C(3)-N-C(1) 109.5(8)c ( 2 b N - A ~ 109.3(6) c ( 3 b N - A ~ 110.2(6)C(1)-N-AU 110.1(5)cm3, 9.47 mmol) was added dropwise.A white solid precipitatedimmediately which was washed with diethyl ether (2 x 5 cm3),filtered off and air dried (381 mg, 18%). M.p. 121 "C (Found:C, 27.35; H, 5.75; N, 6.45; S, 14.60. Calc. for C,H,,F,NO,S:C, 26.90; H, 5.40; N, 6.25; S, 14.35%). AM = 85 0-' cm2 mol-'(7.2 x lo4 mol dm-3). NMR: ' H, 6 1.35 (t, 6 H, Me), 3.23 (m,4 H, CH,), 7.69 (m br, 2 H, NH). IR: v(NH) 3156,3054 cm-'.~H,Ph,][CF,SO,]. Similarly, [NH,Ph,][CF,SO,] (350mg, 18%) was obtained from NHPh, (1 g, 5.9 1 mmol) in diethylether (10 cm3) and CF,SO,H (0.8 cm3, 9.1 mmol).M.p. 135 "C(Found: C, 49.50; H, 3.90; N, 4.55; S, 9.50. Calc. for106 Q-' cm2 mol-' (5.0 x 104mol drn-,). 'H NMR: 6 7.39-7.87(m, Ph). IR: v(NH) 3 184 cm-'.[NH,(C6H4NO2-2)][CF,SO3]. Similarly, [NH,(C6H4-N02-2)][CF3S03] (650 mg, 63%) was obtained from a solutionof NH,(C,H,NO,-2) (98%, 500 mg, 3.55 mmol) in diethyl ether(20 cm3) and HO,SCF, (0.5 cm3, 5.7 mmol). M.p. 148 "C(Found: C, 29.70; H, 2.50; N, 10.00; S , 10.75. Calc. forC7H7F3N205S: C, 29.15; H, 2.45; N, 9.70; S, 11 .lo%). A, = 94Q-' cm2 mol-' (6.9 x mol dm-,). NMR: 'H, 6 7.96(m, 2 H), 8.06 (m, 1 H), 8.43 (m, 1 H). The 'H NMR spectrumshows the presence of a small amount of 2-nitroaniline inequilibrium with the ammoniun salt. IR: v(NH) 31 19 cm-'.~H,(C6H40Me-4)][CF3s03]. Similarly, [NH,(C,H,-OMe-4)][CF3S0,] (820 mg, 92%) was obtained from asolution of NH,(C6H,0Me-4) (400 mg, 3.25 mmol) in diethylether (15 cm3) and CF,SO,H (0.3 cm3, 3.25 mmol).M.p.232 "C (Found: C, 35.35; H, 3.80; N, 5.20; S, 11.65. Calc. for115 W' cm2 mol-' (7.32 x mol dm-,). 'H NMR: 6 3.87 (s,3 H, OMe), 7.1 1, 7.16, 7.47, 7.52 (AA'BB' system). IR: v(NH)3073 cm-'.[Au(PPh,)(NMe,)][ClO,] 1. To a suspension of [Au-Ci,H,,F,NO,S: C, 48.90; H, 3.80; N, 4.40; S, 10.05%). AM =C,H1oF,NO,S: C, 35.15; H, 3.70; N, 5.15; S, 11.75%). AM J. CHEM. SOC. DALTON TRANS. 1995 1253Table 2 Atomic coordinates ( x lo4) for compound 1X3 598.1(4)3 367(2)3 836(8)3 771(12)5 209( 10)2 712(10)2 398( 10)1 223(10)432( 10)807( 12)2 004(11)2 779( 12)5 033( 10)6 255(10)7 512(11)7 599( 1 1)6 392( 1 1)5 120(10)2 428(9)2 767(10)2 114(10)1 096(9)743(9)1 394(10)9 038(2)9 301(10)8 38 l(9)8 171(9)10 339(9)2 971(15)3 249(4)4 535(5)Y2 878.9(3)4 766(2)1089(7)8(7)I 060( 10)923( 10)4 619(9)3 836(9)3 718(11)4 364(12)5 147(11)5 285(10)5 526( 10)4 772( 10)5 382( 1 1)6 686( 10)7 409( 10)6 856( 10)5 956(8)6 051(10)6 959( 10)7 758(10)7 660(8)6 766(8)1041(2)1 170(8)2 179(8)854(9)908( 14)-755(4)1 742(4)- 66( 8)Z4 273.69( 12)3 866.7(8)4 652(3)4 277(4)4 913(4)5 040(4)3 276(3)3 267(3)2 832(4)2 397(4)2 395(4)2 837(4)3 725(3)3 697(3)3 586(4)3 488(4)3 507(3)3 631(3)4 242(4)4 761(3)5 064(3)4 868(3)4 352(3)4 036(3)3 994.0(8)4 530(3)3 801(3)3 917(3)2 885(5)2 826(2)2 994(2)3 735(3)(acac)(PPh,)] (500 mg, 0.89 mmol) in degassed acetone (10cm3), [NHMe,][ClO,] (143 mg, 0.89 mmol) was added and thereaction mixture stirred under a nitrogen atmosphere in an ice-water bath for 1.5 h.The resulting solution was concentrated (2cm3) and diethyl ether (20 cm3) added to precipitate 1 (523 mg,95%) as a white solid which was recrystallized twice fromdichloromethane-diethyl ether. M.p. 178 "C (decomp.) (Found:C, 40.70; H, 4.20; Au, 31.55; N, 2.20. Calc. for C,,H,,Au-cm2 mol-' (3.24 x 10" mol drn-,). NMR: 'H, 6 2.97 (s, 9 H,Me), 7.4-6.1 (m, 15 H, Ph); 31P, 6 30.42 (s); 13C, 6 134.5 (d, ,JPc13), 133.1 (s), 130.0 (d, ,JPc 12), 127.1 (d, 'Jpc 64 Hz), 52.76, Me).[Au(PPh,)(NHEt,)][CF,SO,] 2.To a suspension of[Au(acac)(PPh,)] (179.5 mg, 0.32 mmol) in diethyl ether (15cm3) was added [NH,Et,][CF,SO,] (71.7 mg, 0.32 mmol).Immediate reaction was observed with formation of an oilwhich converted into a powder upon stirring in diethyl etherfor 1 h. It was filtered off, washed with diethyl ether (10 cm3)and recrystallized from acetoneaiethyl ether to give 2 (191 mg,87%). M.p. 124 "C (Found: C, 40.00; H, 3.70; Au, 29.00;N, 1.95; S, 4.60. Calc. for C,,H,,AuF,NO,PS: C, 40.55; H,3.85; Au, 29.0; N, 2.05; S, 4.70%). AM = 101 SZ-' cm2 mol-'(2.96 x lo-, mol drn-,). NMR: 'H, 6 1.48 (t, 6 H, Me, ,JHH = 7Hz), 3.2 (m, 4 H, CH,), 7.4-7.6 (m, 15 H, Ph); 31P, 6 30.89 (s).IR: v(NH) 3 149 cm-' .[Au(PPh,)(NHPh,)][CF,SO,] 3.To a suspension of[Au(acac)(PPh,)] (60 mg, 0.1 1 mmol) in diethyl ether (10 cm3),[NH,Ph,][CF,SO,] (40 mg, 0.11 mmol) was added. Theresulting solution gave, on stirring, a suspension which wasfiltered after 1 h. The cream solid was washed with diethyl ether(5 cm3) and recrystallized from dichloromethaneediethyl etherto give 3 (67 mg, 78%) as a white solid. M.p. 137 "C (decomp.)(Found: C, 47.60; H, 3.35; Au, 26.10; N, 1.80; S, 4.45. Calc. forS, 4.10%). AM = 110 SZ-' cm2 mol-' (9.25 x lo-' mol drn-,).ClNOdP: C, 40.80; H, 4.00; Au, 3 1.90; N, 2.25%). AM = 90 0-lC,,H~~AUF,NO,PS: C, 47.90; H, 3.35; Au, 25.35; N, 1.80;NMR: 'H, 6 7.0-7.8 (m, 25 H, Ph), 8.84 (s br, 1 H, NH); "P,6 28.89 (s).[Au(PPh3){NH2(C,H4N02-2))][CF3S03] 4.To a solutionof CNH,(C6H,N0,-2)][CF,S0,] (81.6 mg, 0.28 mmol) indiethyl ether (15 cm3) was added [Au(acac)(PPh,)] (158 mg,0.28 mmol). The resulting suspension was stirred for 3 h andfiltered to give 4 (68 mg, 32%) which was washed with diethylether (10 cm3) and air dried. M.p. 150 "C (decomp.) (Found:C, 40.45; H, 2.60; Au, 25.70; N, 3.35; S, 4.35. Calc. forC,,H2,AuF3N2OSPS: C, 40.25; H, 2.85; Au, 26.40; N, 3.75;S, 4.30%). AM = 99 SZ-' cm2 mol-' (2.84 x lo4 mol drn-,).NMR: 'H, 6 7.02 ('t', 1 H, NH2C6H4N02-2), 7.4-7.7 (m, 15 H,PPh, + 2 H, NH,C,H,NO2-2), 8.17 ('d', 1 H, NHzC6H4-NO,-2); ,'P, 6 28.99 (s). IR: v(NH) 3214 cm-'.[Au(PPh,){NH,(C6H,0Me-4))][CF,S03] 5. To a sus-pension of [Au(acac)(PPh,)] (174 mg, 0.31 mmol) in diethylether (20 cm3) was added CNH3(C6H4OMe-4)][CF,S0,](105 mg, 0.31 mmol).Immediate reaction was observed withformation of an oily solid which converted into a powder uponstirring in diethyl ether for 1 h. It was filtered off, washed withdiethyl ether (5 cm3) and air dried to give 5 (1 89 mg, 83%). M.p.131 "C (decomp.) (Found: C, 42.25; H, 3.05; Au, 27.50; N, 1.85;S, 4.40. Calc. for C,,H,,AUF,N~~PS: C, 42.70; H, 3.30; Au,26.95; N, 1.85; S, 4.40%). AM = 52 i2-l cm2 mol-' (4.65 x 10"mol dm-,). NMR: 'H, 6 3.71 (s, 3 H, Me), 6.73,6.76, 7.24, 7.27(AA'BB', 4 H), 7.4-7.6 (m, 15 H, PPh,); ,'P, 6 31.07 (s). IR:v(NH) 3173,3092 cm-'.Crystal Structure Determination of Compound 1 .-Crystaldata. C2,H,,AuC1,NO,P, orthorhombic, space group P212,2,,a = 9.498(2), b = 10.322(2), c = 26.154(4) A, U = 2564.1 A,Z = 4, D, = 1.820 Mg m-,, F(OO0) = 1368, h(M0-Ka) =0.710 73 A, p = 6.1 mm-', T = - 130 "C.A colourless prismca. 0.5 x 0.2 x 0.15 mm was mounted on a glass fibre ininert oil and transferred to the cold-gas stream of thediffractometer (Stoe STADI-4 with Siemens LT-2 lowtemperature attachment). A total of 61 14 reflections werecollected to 28 55", of which 5288 were independent (Rint 0.0359)after an absorption correction based on y scans (transmissionsof 0.56-0.99). Cell constants were refined from k o values of 74reflections in the range 20 20-23".Structure solution and refinement. The structure was solved bythe heavy-atom method and refined on F2 (ref.13). Hydrogenatoms were included using a riding model or as rigid methylgroups. The absolute structure was determined by the xparameter - 0.022( 1 1). l4 The final wR(F2) was 0.09 1 for allreflections, with a conventional R(F) of 0.043, for 292parameters and 192 restraints; S = 1.05, max. A/o 0.002, Max.Ap 0.75 e A-3. Selected bond lengths and angles are given inTable 1 and final atomic coordinates in Table 2.Additional material available from the Cambridge Crystallo-graphic Data Centre comprises H-atom coordinates, thermalparameters and remaining bond lengths and angles.AcknowledgementsWe thank Direccibn General de Investigacion Cientifica yTkcnica (PB92-0982-C) and the Fonds der ChemischenIndustrie for financial support.References1 R.J. Puddephatt, in Comprehensive Coordination Chemistry, eds.G. Wilkinmn, R. D. Gillard and J. A. McCleverty, Pergamon,Oxford, 1987, vol. 5, p. 861 and refs. therein.2 J. J. Guy, P. G. Jones, M. J. Mays and G. M. Sheldrick, J. Chem. Soc.,Dalton Trans., 1977, 8.3 (a) E. G. Perevalova, K. I. Grandberg, V. P. Dyadchenko andT. V. 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Vicente,M. T. Chicote, P. Gonzalez-Herrero and P. G. Jones, J. Chem.Soc., Dalton Trans., 1994, 3183; J. Vicente, M. T. Chicote,P. Gonzalez-Herrero, P. G. Jones and B. Ahrens, Angew. Chem.,int. Ed. Engl., 1994,33, 1852.10 M. C. Gimeno, A. Laguna, M. Laguna, F. Sanmartin andP. G. Jones, Organometallics, 1993, 12, 3984; 1994, 13, 1538;E. J. Fernandez, M. C. Gimeno, P. G. Jones, A. Laguna, M. Lagunaand J. M. Lopez de Luzuriaga, Angew. Chem., Znt. Ed. Engl., 1994,33, 87 and refs. therein.1 1 W. J. Geary, Coord. Chem. Rev., 1981,7,81.12 D. Gibson, B. F. G. Johnson and J. Lewis, J. Chem. SOC. A, 1970,13 G. M. Sheldrick, SHELXL 93, Program for refining crystal14 H. D. Flack, Acta Crystallogr., Sect. A, 1983,39, 876.367.structures, J. Appl. Crystallogr., in the press.Received 4th October 1994; Paper 4/06055
ISSN:1477-9226
DOI:10.1039/DT9950001251
出版商:RSC
年代:1995
数据来源: RSC