Structure of chlorotris(triphenylphosphine)copper(I)–tetrahydrofuran (1/3)

Folting, Kirsten; Huffman, John C.; Mahoney, Wayne S.; Stryker, Jeffrey M.; Caulton, Kenneth G.

doi:10.1107/s0108270187091352

Cited by 16 publications

(12 citation statements)

References 2 publications

Supporting

Mentioning

Contrasting

Unclassified

Order By: Relevance

“…51 These examples were often obtained inadvertently, with the P−O−P fragments resulting from the evolution of R2POH and/or R2(O=)P−PR2 molecules due to isomerisation of P=O bonding in the presence of M 2+ ions (Cu, Co…). [52][53][54] Recently 67 The averages for the P-Cu-P and P-Cu-X angles, respectively 100.6(12) and 117 2 76 the Cu−P bond length is also similar to those measured in 5 and 5'.…”

Section: Formation Of Iron Complexes 3 and 3'supporting

confidence: 63%

Complexes of the tripodal phosphine ligands PhSi(XPPh₂)₃(X = CH₂, O): synthesis, structure and catalytic activity in the hydroboration of CO₂

et al. 2016

View full text Add to dashboard Cite

The coordination chemistry of Fe(2+), Co(2+) and Cu(+) ions was explored with the triphosphine and triphosphinite ligands PhSi{CH2PPh2}3 (1) and PhSi{OPPh2}3 (2), so as to evaluate the impact of the electronic properties of the tripodal phosphorus ligands on the structure and reactivity of the corresponding complexes. The synthesis and characterization of the complexes [Fe(κ(3)-PhSi{CH2PPh2}3)(MeCN)3][OTf]2 (3) (OTf = O3SCF3), [Fe(κ(3)-PhSi{OPPh2}3)(MeCN)3][OTf]2 (3'), [Co(κ(2)-PhSi{CH2PPh2}3)Cl2] (4), [Co(κ(3)-PhSi{OPPh2}3)Cl2] (4'), [Cu(κ(3)-PhSi{CH2PPh2}3)Br] (5) and [Cu(κ(3)-PhSi{OPPh2}3)I] (5') were carried out. The crystal structures of 3, 3', 4, 4', and of the solvates 5·3THF and 5'·THF are reported. Complexes 3-5' were shown to promote the catalytic hydroboration of CO2 with (9-BBN)2 (9-BBN = 9-borabicyclo[3.3.1]nonane). While the iron and cobalt complexes of the triphosphine 1 are more active than the analogous complexes with 2, the opposite trend is observed with the copper catalysts. Overall, the copper catalysts 5 and 5' are both more reactive and more selective than the Fe and Co catalysts, enabling the formation of the acetal H2C(OBBN)2 with a high molar ratio of H2C(OBBN)2 : CH3OBBN up to 92 : 8.

show abstract

Section: Formation Of Iron Complexes 3 and 3'supporting

confidence: 63%

Complexes of the tripodal phosphine ligands PhSi(XPPh₂)₃(X = CH₂, O): synthesis, structure and catalytic activity in the hydroboration of CO₂

et al. 2016

View full text Add to dashboard Cite

show abstract

“…119 · 0(4) 115 · 8(4) C(11)-Sb-C (21) 98 · 1(5) 99 · 8(5) 99 · 7(5) 98 · 3(5) 99 · 9(5) 100 · 3(5) C(11)-Sb-C(31) 100 · 2(5) 101 · 5(4) 99 · 8(5) 101 · 4(5) 102 · 0(5) 96 · 6(5) C(21)-Sb-C(31) 100 · 1(5) 98 · 5(5) 99 · 3(5) 100 · 4(5) 98 · 7(5) 100 · 2(5) Sb-C(11)-C (12) 117 · 8(9) 120(1) 119(1) 118(1) 120(1) 118 · 2(9) Sb-C(11)-C (16) 125(1) 121(1) 124(1) 122(1) 122(1) 124(1) Sb-C(21)-C (16) 119 · 6(9) 120(1) 118 · 2(9) 117 · 2(9) 118(1) 120(1) Sb-C(21)-C (26) 122 · 6(9) 124 · 8 these: those distances and angles, associated with the E 3 MX molecular core, giving some feel for consistent perturbations which may be particularly associated with one particular lattice type vis-a-vis the others, and the overall ranges for any given parameter; inclusion of other parameters, notably ring torsion angles within the ligand, also suggest themselves as useful in an aggregate comparison, but space does not permit such a more comprehensive delineation. The following general comments may be made in respect of the more common types.…”

Section: Discussionmentioning

confidence: 99%

“…Molecular volumes range from 1136 to 1263Å 3 , c. 10% change, the extrema corresponding to pseudo-halogen anionic ligands, these Distances/Å Sb-C(11) 2 · 122(5) 2 · 121(6) 2 · 120(5) Sb-C (21) 2 · 128(6) 2 · 129(6) 2 · 136(5) Sb-C(31) 2 · 121(5) 2 · 107(5) 2 · 103 (5) Angles/degrees Ag-Sb-C(11) 113 · 9(1) 116 · 1(1) 120 · 0(2) Ag-Sb-C (21) 118 · 9(2) 124 · 4(2) 121 · 9(1) Ag-Sb-C(31) 123 · 1(1) 111 · 0(2) 109 · 1(2) C(11)-Sb-C (21) 99 · 7(2) 99 · 8(2) 102 · 5(2) C(11)-Sb-C(31) 100 · 9(2) 103 · 2(2) 101 · 2(2) C(21)-Sb-C(31) 96 · 2(2) 99 · 0(2) 98 · 3(2) Sb-C(11)-C (12) 118 · 7(4) 118 · 4(4) 117 · 0(4) Sb-C(11)-C (16) 122 · 5(4) 123 · 2(4) 123 · 4(4) Sb-C(21)-C (22) 118 · 4(5) 119 · 4(4) 118 · 9(4) Sb-C(21)-C (26) 121 · 9(5) 121 · 8(5) 122 · 1(4) Sb-C(31)-C (22) 119 · 2(4) 117 · 9(4) 117 · 1(4) Sb-C(31)-C(36) 122 · 8(4) 124 · 7(4) 124 · 4(5)…”

Section: Type A(ii) Monoclinic P2 1 /N Z = 4 Moleculesunclassified

“…Torsion angles/degrees (carbon atoms denoted by number only) Ag-Sb-11- 12 23 · 3(5) 34 · 4(5) 3 · 8(5) Ag-Sb- [21][22] 39 · 0(7) 38 · 1(5) 54 · 6(5) Ag-Sb-31-32 41 · 4(5) 24 · 0(6) 59 · 2(5) being CN, SCN. Varieties of E/M/X embrace E = P, As, Sb, for M = Ag only, the anionic X assortment being diverse.…”

Section: Type A(ii) Monoclinic P2 1 /N Z = 4 Moleculesmentioning

confidence: 99%

See 1 more Smart Citation

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.

View full text Add to dashboard Cite

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)

show abstract

“…The remaining two, both as tetrahydrofuran solvates, crystallize as two polymorphs, viz. a noncentrosymmetric form in P6 3 (Folting et al, 1987) and a centrosymmetric form in P2 1 /c (Carlson et al, 1996;Kraü ter & Neumü ller, 1996). This report presents the second known polymorph of the (pure) title compound.…”

Section: Commentmentioning

confidence: 99%

A centrosymmetric polymorph of chloridotris(triphenylphosphine-κP)copper(I) at 150 K

et al. 2008

View full text Add to dashboard Cite

This study characterizes a new polymorph of the title compound, [CuCl(C18H15P)3], and analyses the influence of the extensive network of weak hydrogen-bonding interactions in the generation of this different crystal structure. The compound crystallizes in the centrosymmetric space group C2/c with two crystallographically independent molecules per asymmetric unit, in contrast with the previously determined polymorph which crystallizes in the noncentrosymmetric space group P3 with three crystallographically independent molecules in the asymmetric unit, each with crystallographically imposed C3 symmetry [Gill, Mayerle, Welcker, Lewis, Ucko, Barton, Stowens & Lippard (1976). Inorg. Chem. 15, 1155-1168]. The geometries of the two molecules of the title compound are very similar, with each having an approximately tetrahedral coordination around the central Cu atom and approximate C(s) molecular symmetry. The molecules pack in chains parallel to the crystallographic b axis, connected by C-H...Cl and C-H...pi(phenyl) hydrogen bonds.

show abstract

Structure of chlorotris(triphenylphosphine)copper(I)–tetrahydrofuran (1/3)

Cited by 16 publications

References 2 publications

Complexes of the tripodal phosphine ligands PhSi(XPPh₂)₃(X = CH₂, O): synthesis, structure and catalytic activity in the hydroboration of CO₂

Complexes of the tripodal phosphine ligands PhSi(XPPh₂)₃(X = CH₂, O): synthesis, structure and catalytic activity in the hydroboration of CO₂

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

A centrosymmetric polymorph of chloridotris(triphenylphosphine-κP)copper(I) at 150 K

Contact Info

Product

Resources

About

Structure of chlorotris(triphenylphosphine)copper(I)–tetrahydrofuran (1/3)

Cited by 16 publications

References 2 publications

Complexes of the tripodal phosphine ligands PhSi(XPPh2)3(X = CH2, O): synthesis, structure and catalytic activity in the hydroboration of CO2

Complexes of the tripodal phosphine ligands PhSi(XPPh2)3(X = CH2, O): synthesis, structure and catalytic activity in the hydroboration of CO2

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

A centrosymmetric polymorph of chloridotris(triphenylphosphine-κP)copper(I) at 150 K

Contact Info

Product

Resources

About

Complexes of the tripodal phosphine ligands PhSi(XPPh₂)₃(X = CH₂, O): synthesis, structure and catalytic activity in the hydroboration of CO₂

Complexes of the tripodal phosphine ligands PhSi(XPPh₂)₃(X = CH₂, O): synthesis, structure and catalytic activity in the hydroboration of CO₂