Lewis-Base Adducts of Group 11 Metal(I) Compounds. XXV. Synthesis and Structural Properties of Tris(Triphenylphosphine)Copper(I) Perchlorate and Nitrate

The syntheses and room-temperature single-crystal X-ray structural characterization of 1 : 3 adducts formed between silver(I) (pseudo-) halides, AgX, and triphenylstibine, SbPh3, are described for X = Cl, I, SCN, NCS, CN, NO3 (1)-(6). The chloride, as its methanol solvate (1a), is isomorphous with the arsine analogue: triclinic, P-1, a 13·373(4), b 14·48(6), c 14·702(3) Å, α 83·49(3), β 87·76(2), γ 76·45(3)°; Z = 2, conventional R on F being 0·046 for No 5514 independent ‘observed’ reflections (I > 3σ(I )). A new form (1b) of the chloride has also been authenticated: monoclinic, P 21/c, a 12·832(2), b 54·24(1), c 18·519(8) Å, β 129·68(3)°; Z = 8 (R 0·065 for No 5672). No bromide has been obtained; the iodide (2) is described as monoclinic, P 21/n, a 19·611(4), b 14·473(6), c 17·74(1) Å, β 98·28(3)°; Z = 4 (R 0·036 for No 6769). The thiocyanate crystallizes from acetonitrile or pyridine as an S-bonded form (3) isomorphous with the arsine analogue: monoclinic, P 21/n, a 19·143(7), b 14·288(5), c 18·694(6) Å, β 98·81(2)°; Z = 4 (R 0·037 for No 4482). From 2-methylpyridine, remarkably, a solvate is obtained in which the thiocyanate is N-bonded (4): triclinic, P-1, a 27·261(5), b 14·767(3), c 13·319(1) Å, α 91·53(1), β 101·58(1), γ 92·29(2)°; Z = 4 (R 0·045 for No 6900). The cyanide is also monoclinic, P 21/n, a 19·442(7), b 14·267(3), c 17·741(6) Å, β 97·63(3)°, z = 4; R 0·057 for No 2487. The unsolvated 1 : 3 nitrate complex (6a) is monoclinic, P 21/n, a 19·602(5), b 14·455(1), c 17·727(2) Å, β 97·19(2)°, Z = 4; R was 0·034 for No 6522. The complex is isomorphous with the arsenic and phosphorus analogues, being mononuclear [(Ph3Sb)3Ag(O2NO)]. The ethanol solvate (6b) is triclinic, P-1, a 13·352(5), b 14·548(9), c 14·701(4) Å, α 81·64(4), β 84·45(3), γ 75·32(4)°, Z = 2; R was 0·058 for No 4702. Ag-Sb range between 2·6980(8) and 2·843(3) Å in the precise determinations; Ag-X are 2·481(4) and 2·52(1) Å (the two chlorides), 2·757(1) (I), 2·533(3) (SCN), 2·21(1) (NCS), 2· 09(3) (CN), 2·377(7) Å (unidentate ONO2)

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“…109 · 44(5) 108 · 82(5) 110 · 37(4) 111 · 85(5) 108 · 83(5) 108 · 70(4) Ag-Sb-C (11) 119 · 8(4) 124 · 5(5) 120 · 0(4) 117 · 7(4)…”

Section: Discussionunclassified

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LXVIII Synthesis and Structural Systematics of Some 1 : 3 Adducts of Silver(I) Compounds with Triphenylstibine, [(Ph3Sb)3AgX], X = Cl, I, SCN, NCS, CN, ONO2

Effendy¹,

Kildea²,

White³

1997

Aust. J. Chem.

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“…The title compound, (I), is an example of a methanol solvate of a previously published ethanol solvate complex (Dyason et al, 1986). Both complexes crystallize in the P2 1 /n space group with similar cell lengths and angles.…”

Section: S1 Commentmentioning

confidence: 98%

“…The title compound is structurally related to the ethanol solvate derivative (Dyason et al, 1986). For related diketonato complexes, see: Hill & Steyl (2008); Steyl & Roodt (2006); Steyl (2007); Steyl & Hill (2009).…”

Section: Related Literaturementioning

confidence: 99%

Nitratotris(triphenylphosphine)copper(I) methanol solvate

Steyl

2009

Acta Cryst E

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“…While markedly different, the P-Cu-P bond angles for for I (Table 1) fall within this range with an average of 116 (2)°. The dissimilarity observed for the O-Cu-P bond angles (Table 1) .EtOH (Dyason et al, 1986), [Cu(PPh 3 ) 3 (NO 3 )].MeOH (Steyl, 2009) and I were observed to be 2.329 (9) Å, 2.326 (10) Å and 2.300 (13) Å respectively.…”

Section: Methodsmentioning

confidence: 99%

“…For related complexes, see: Hanna et al (2005); Steyl (2009); Saravanabharathi et al (2002); Dyason et al (1986); Matthew et al (1971).…”

Section: Related Literaturementioning

confidence: 99%

(Nitrato-κO)tris[tris(4-fluorophenyl)phosphane-κP]copper(I)

Hill

Roodt

2012

Acta Cryst E

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Key indicators: single-crystal X-ray study; T = 100 K; mean (C-C) = 0.003 Å; R factor = 0.035; wR factor = 0.085; data-to-parameter ratio = 18.4.In the title complex, [Cu(NO 3 )(C 18 H 12 F 3 P) 3 ], the ligating atoms define a distorted tetrahedon with the three tris(4-fluorophenyl)phosphane ligands in the basal positions and the nitrate ligand in the axial position. The intramolecularinteraction [centroid-centroid distance = 3.6113 (11) Å ] between two of the 4-fluorophenyl groups is complemented by both C-HÁ Á ÁF and C-HÁ Á ÁO interactions with distances in the range 2.51-2.60 Å , resulting in a tight head-to-tail packing. Related literature

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Lewis-Base Adducts of Group 11 Metal(I) Compounds. XXV. Synthesis and Structural Properties of Tris(Triphenylphosphine)Copper(I) Perchlorate and Nitrate

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Lewis-Base Adducts of Group 11 Metal(I) Compounds. LXVIII Synthesis and Structural Systematics of Some 1 : 3 Adducts of Silver(I) Compounds with Triphenylstibine, [(Ph3Sb)3AgX], X = Cl, I, SCN, NCS, CN, ONO2

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LXVIII Synthesis and Structural Systematics of Some 1 : 3 Adducts of Silver(I) Compounds with Triphenylstibine, [(Ph3Sb)3AgX], X = Cl, I, SCN, NCS, CN, ONO2

Nitratotris(triphenylphosphine)copper(I) methanol solvate

(Nitrato-κO)tris[tris(4-fluorophenyl)phosphane-κP]copper(I)

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