Synthesis and Characterization of New Square Planar Iridium Complexes [trans-Ir(CO)L2X] (L = PCy3, X = OH or OCH3; L = P(p-tolyl)3, X = OCH2C6H5 or O(p-C6H4CH3)): Crystal and Molecular Structures of trans-Ir(CO)(OH)(PCy3)2, trans-Ir(CO)(OCH2C6H5)(P(p-tolyl)3)2, and trans-Ir(CO)(O-p-C6H4CH3)(P(p-tolyl)3)2

Cynthia A. Miller; Thomas S. Janik; Charles H. Lake; Laurence M. Toomey; Melvyn Rowen Churchill; Jim D. Atwood

doi:10.1021/om00024a059

Synthesis and Characterization of New Square Planar Iridium Complexes [trans-Ir(CO)L₂X] (L = PCy₃, X = OH or OCH₃; L = P(p-tolyl)₃, X = OCH₂C₆H₅ or O(p-C₆H₄CH₃)): Crystal and Molecular Structures of trans-Ir(CO)(OH)(PCy₃)₂, trans-Ir(CO)(OCH₂C₆H₅)(P(p-tolyl)₃)₂, and trans-Ir(CO)(O-p-C₆H₄CH₃)(P(p-tolyl)₃)₂

Cynthia A. Miller
, Thomas S. Janik
, Charles H. Lake
, Laurence M. Toomey
, Melvyn Rowen Churchill
, Jim D. Atwood

Chemistry

University at Buffalo

SUNY Buffalo

Research output: Contribution to journal › Article › peer-review

23 Scopus citations

Abstract

Three new Ir(I) complexes have been prepared, characterized and studied by X-ray crystallography. No evidence is found for pi-donation from an alkoxy (Ir(CO)(OCH₂C₆H₅)(P(p-tolyl)₃)₂) or an aryloxy (Ir(CO)(O-p-C₆H₄CH₃(P(p-toly)₃)₂) to iridium. The phenylmethoxy complex IR(CO)(OCH₂C₆H₅)(P(p-tolyl)₃)₂ crystallizes in the triclinic space group P1 with a = 10.5187(16), b = 12.8320(15), c = 17.4940(19)Å, α = 71.447(8), β = 84.907(11), ³ = 72.407- (11) °, V = 2133.8(5)Å3 and Z = 2. The structure was solved and refined to R = 2.48% for 4567 reflections with F₀ > 6σ(F₀). Interatomic distances of note are Ir-P = 2.306(2) and 2.334(2), Ir-CO = 1.806(6) and Ir-O = 2.022(4)Å. The p-cresolate derivative crystallizes as the p-cresol adduct Ir(CO)(OC₆H₄CH₃)(P(p-tolyl)₃)₂·CH₃C₆H₄OH in the monoclinic space group P2₁/c with a = 21.1172(28), b = 12.0167(15), c = 22.5658(31)Å, β = 117.180(10)°, V = 5094.0- (12) Å3 and Z = 4. The structure was refined to R = 4.26% for 3296 reflections with F₀ > 6σ(F₀). Interatomic distances include Ir-P = 2.322(4) and 2.330(4), Ir-CO = 1.781(13) and Ir-O = 2.067(7)Å. The hydroxy derivative Ir(CO)(OH)(PCy₃)₂ crystallizes in the triclinic space group P1 with a = 9.916(3), b = 10.305(4), c = 10.825(4)Å, α = 114.16(3), β = 109.55(3), γ = 90.14(3)°, V = 938.6(5)Å3 and Z = 1. This structure is disordered with a scrambled image of the carbonyl and hydroxide ligands. Distances of note are Ir-P = 2.331(1), Ir-CO = 1.887- (13) and Ir-OH = 1.978(12)Å; the Ir-CO and Ir-OH distances may suffer from systematic errors due to disorder.

Original language	English
Pages (from-to)	5080-5087
Number of pages	8
Journal	Organometallics
Volume	13
Issue number	12
DOIs	https://doi.org/10.1021/om00024a059
State	Published - Dec 1 1994

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Miller, C. A., Janik, T. S., Lake, C. H., Toomey, L. M., Churchill, M. R., & Atwood, J. D. (1994). Synthesis and Characterization of New Square Planar Iridium Complexes [trans-Ir(CO)L₂X] (L = PCy₃, X = OH or OCH₃; L = P(p-tolyl)₃, X = OCH₂C₆H₅ or O(p-C₆H₄CH₃)): Crystal and Molecular Structures of trans-Ir(CO)(OH)(PCy₃)₂, trans-Ir(CO)(OCH₂C₆H₅)(P(p-tolyl)₃)₂, and trans-Ir(CO)(O-p-C₆H₄CH₃)(P(p-tolyl)₃)₂. Organometallics, 13(12), 5080-5087. https://doi.org/10.1021/om00024a059

Miller, Cynthia A. ; Janik, Thomas S. ; Lake, Charles H. et al. / Synthesis and Characterization of New Square Planar Iridium Complexes [trans-Ir(CO)L₂X] (L = PCy₃, X = OH or OCH₃; L = P(p-tolyl)₃, X = OCH₂C₆H₅ or O(p-C₆H₄CH₃)) : Crystal and Molecular Structures of trans-Ir(CO)(OH)(PCy₃)₂, trans-Ir(CO)(OCH₂C₆H₅)(P(p-tolyl)₃)₂, and trans-Ir(CO)(O-p-C₆H₄CH₃)(P(p-tolyl)₃)₂. In: Organometallics. 1994 ; Vol. 13, No. 12. pp. 5080-5087.

@article{47b07a721fa64c8383ecd98faab8ea97,

title = "Synthesis and Characterization of New Square Planar Iridium Complexes [trans-Ir(CO)L2X] (L = PCy3, X = OH or OCH3; L = P(p-tolyl)3, X = OCH2C6H5 or O(p-C6H4CH3)): Crystal and Molecular Structures of trans-Ir(CO)(OH)(PCy3)2, trans-Ir(CO)(OCH2C6H5)(P(p-tolyl)3)2, and trans-Ir(CO)(O-p-C6H4CH3)(P(p-tolyl)3)2",

abstract = "Three new Ir(I) complexes have been prepared, characterized and studied by X-ray crystallography. No evidence is found for pi-donation from an alkoxy (Ir(CO)(OCH2C6H5)(P(p-tolyl)3)2) or an aryloxy (Ir(CO)(O-p-C6H4CH3(P(p-toly)3)2) to iridium. The phenylmethoxy complex IR(CO)(OCH2C6H5)(P(p-tolyl)3)2 crystallizes in the triclinic space group P1 with a = 10.5187(16), b = 12.8320(15), c = 17.4940(19){\AA}, α = 71.447(8), β = 84.907(11), ³ = 72.407- (11) °, V = 2133.8(5){\AA}3 and Z = 2. The structure was solved and refined to R = 2.48\% for 4567 reflections with F0 > 6σ(F0). Interatomic distances of note are Ir-P = 2.306(2) and 2.334(2), Ir-CO = 1.806(6) and Ir-O = 2.022(4){\AA}. The p-cresolate derivative crystallizes as the p-cresol adduct Ir(CO)(OC6H4CH3)(P(p-tolyl)3)2·CH3C6H4OH in the monoclinic space group P21/c with a = 21.1172(28), b = 12.0167(15), c = 22.5658(31){\AA}, β = 117.180(10)°, V = 5094.0- (12) {\AA}3 and Z = 4. The structure was refined to R = 4.26\% for 3296 reflections with F0 > 6σ(F0). Interatomic distances include Ir-P = 2.322(4) and 2.330(4), Ir-CO = 1.781(13) and Ir-O = 2.067(7){\AA}. The hydroxy derivative Ir(CO)(OH)(PCy3)2 crystallizes in the triclinic space group P1 with a = 9.916(3), b = 10.305(4), c = 10.825(4){\AA}, α = 114.16(3), β = 109.55(3), γ = 90.14(3)°, V = 938.6(5){\AA}3 and Z = 1. This structure is disordered with a scrambled image of the carbonyl and hydroxide ligands. Distances of note are Ir-P = 2.331(1), Ir-CO = 1.887- (13) and Ir-OH = 1.978(12){\AA}; the Ir-CO and Ir-OH distances may suffer from systematic errors due to disorder.",

author = "Miller, \{Cynthia A.\} and Janik, \{Thomas S.\} and Lake, \{Charles H.\} and Toomey, \{Laurence M.\} and Churchill, \{Melvyn Rowen\} and Atwood, \{Jim D.\}",

year = "1994",

month = dec,

day = "1",

doi = "10.1021/om00024a059",

language = "English",

volume = "13",

pages = "5080--5087",

journal = "Organometallics",

issn = "0276-7333",

publisher = "American Chemical Society",

number = "12",

}

Miller, CA, Janik, TS, Lake, CH, Toomey, LM, Churchill, MR & Atwood, JD 1994, 'Synthesis and Characterization of New Square Planar Iridium Complexes [trans-Ir(CO)L₂X] (L = PCy₃, X = OH or OCH₃; L = P(p-tolyl)₃, X = OCH₂C₆H₅ or O(p-C₆H₄CH₃)): Crystal and Molecular Structures of trans-Ir(CO)(OH)(PCy₃)₂, trans-Ir(CO)(OCH₂C₆H₅)(P(p-tolyl)₃)₂, and trans-Ir(CO)(O-p-C₆H₄CH₃)(P(p-tolyl)₃)₂', Organometallics, vol. 13, no. 12, pp. 5080-5087. https://doi.org/10.1021/om00024a059

Synthesis and Characterization of New Square Planar Iridium Complexes [trans-Ir(CO)L₂X] (L = PCy₃, X = OH or OCH₃; L = P(p-tolyl)₃, X = OCH₂C₆H₅ or O(p-C₆H₄CH₃)): Crystal and Molecular Structures of trans-Ir(CO)(OH)(PCy₃)₂, trans-Ir(CO)(OCH₂C₆H₅)(P(p-tolyl)₃)₂, and trans-Ir(CO)(O-p-C₆H₄CH₃)(P(p-tolyl)₃)₂. / Miller, Cynthia A.; Janik, Thomas S.; Lake, Charles H. et al.
In: Organometallics, Vol. 13, No. 12, 01.12.1994, p. 5080-5087.

Research output: Contribution to journal › Article › peer-review

TY - JOUR

T1 - Synthesis and Characterization of New Square Planar Iridium Complexes [trans-Ir(CO)L2X] (L = PCy3, X = OH or OCH3; L = P(p-tolyl)3, X = OCH2C6H5 or O(p-C6H4CH3))

T2 - Crystal and Molecular Structures of trans-Ir(CO)(OH)(PCy3)2, trans-Ir(CO)(OCH2C6H5)(P(p-tolyl)3)2, and trans-Ir(CO)(O-p-C6H4CH3)(P(p-tolyl)3)2

AU - Miller, Cynthia A.

AU - Janik, Thomas S.

AU - Lake, Charles H.

AU - Toomey, Laurence M.

AU - Churchill, Melvyn Rowen

AU - Atwood, Jim D.

PY - 1994/12/1

Y1 - 1994/12/1

N2 - Three new Ir(I) complexes have been prepared, characterized and studied by X-ray crystallography. No evidence is found for pi-donation from an alkoxy (Ir(CO)(OCH2C6H5)(P(p-tolyl)3)2) or an aryloxy (Ir(CO)(O-p-C6H4CH3(P(p-toly)3)2) to iridium. The phenylmethoxy complex IR(CO)(OCH2C6H5)(P(p-tolyl)3)2 crystallizes in the triclinic space group P1 with a = 10.5187(16), b = 12.8320(15), c = 17.4940(19)Å, α = 71.447(8), β = 84.907(11), ³ = 72.407- (11) °, V = 2133.8(5)Å3 and Z = 2. The structure was solved and refined to R = 2.48% for 4567 reflections with F0 > 6σ(F0). Interatomic distances of note are Ir-P = 2.306(2) and 2.334(2), Ir-CO = 1.806(6) and Ir-O = 2.022(4)Å. The p-cresolate derivative crystallizes as the p-cresol adduct Ir(CO)(OC6H4CH3)(P(p-tolyl)3)2·CH3C6H4OH in the monoclinic space group P21/c with a = 21.1172(28), b = 12.0167(15), c = 22.5658(31)Å, β = 117.180(10)°, V = 5094.0- (12) Å3 and Z = 4. The structure was refined to R = 4.26% for 3296 reflections with F0 > 6σ(F0). Interatomic distances include Ir-P = 2.322(4) and 2.330(4), Ir-CO = 1.781(13) and Ir-O = 2.067(7)Å. The hydroxy derivative Ir(CO)(OH)(PCy3)2 crystallizes in the triclinic space group P1 with a = 9.916(3), b = 10.305(4), c = 10.825(4)Å, α = 114.16(3), β = 109.55(3), γ = 90.14(3)°, V = 938.6(5)Å3 and Z = 1. This structure is disordered with a scrambled image of the carbonyl and hydroxide ligands. Distances of note are Ir-P = 2.331(1), Ir-CO = 1.887- (13) and Ir-OH = 1.978(12)Å; the Ir-CO and Ir-OH distances may suffer from systematic errors due to disorder.

AB - Three new Ir(I) complexes have been prepared, characterized and studied by X-ray crystallography. No evidence is found for pi-donation from an alkoxy (Ir(CO)(OCH2C6H5)(P(p-tolyl)3)2) or an aryloxy (Ir(CO)(O-p-C6H4CH3(P(p-toly)3)2) to iridium. The phenylmethoxy complex IR(CO)(OCH2C6H5)(P(p-tolyl)3)2 crystallizes in the triclinic space group P1 with a = 10.5187(16), b = 12.8320(15), c = 17.4940(19)Å, α = 71.447(8), β = 84.907(11), ³ = 72.407- (11) °, V = 2133.8(5)Å3 and Z = 2. The structure was solved and refined to R = 2.48% for 4567 reflections with F0 > 6σ(F0). Interatomic distances of note are Ir-P = 2.306(2) and 2.334(2), Ir-CO = 1.806(6) and Ir-O = 2.022(4)Å. The p-cresolate derivative crystallizes as the p-cresol adduct Ir(CO)(OC6H4CH3)(P(p-tolyl)3)2·CH3C6H4OH in the monoclinic space group P21/c with a = 21.1172(28), b = 12.0167(15), c = 22.5658(31)Å, β = 117.180(10)°, V = 5094.0- (12) Å3 and Z = 4. The structure was refined to R = 4.26% for 3296 reflections with F0 > 6σ(F0). Interatomic distances include Ir-P = 2.322(4) and 2.330(4), Ir-CO = 1.781(13) and Ir-O = 2.067(7)Å. The hydroxy derivative Ir(CO)(OH)(PCy3)2 crystallizes in the triclinic space group P1 with a = 9.916(3), b = 10.305(4), c = 10.825(4)Å, α = 114.16(3), β = 109.55(3), γ = 90.14(3)°, V = 938.6(5)Å3 and Z = 1. This structure is disordered with a scrambled image of the carbonyl and hydroxide ligands. Distances of note are Ir-P = 2.331(1), Ir-CO = 1.887- (13) and Ir-OH = 1.978(12)Å; the Ir-CO and Ir-OH distances may suffer from systematic errors due to disorder.

UR - https://www.scopus.com/pages/publications/0000066078

U2 - 10.1021/om00024a059

DO - 10.1021/om00024a059

M3 - Article

SN - 0276-7333

VL - 13

SP - 5080

EP - 5087

JO - Organometallics

JF - Organometallics

IS - 12

ER -

Miller CA, Janik TS, Lake CH, Toomey LM, Churchill MR, Atwood JD. Synthesis and Characterization of New Square Planar Iridium Complexes [trans-Ir(CO)L₂X] (L = PCy₃, X = OH or OCH₃; L = P(p-tolyl)₃, X = OCH₂C₆H₅ or O(p-C₆H₄CH₃)): Crystal and Molecular Structures of trans-Ir(CO)(OH)(PCy₃)₂, trans-Ir(CO)(OCH₂C₆H₅)(P(p-tolyl)₃)₂, and trans-Ir(CO)(O-p-C₆H₄CH₃)(P(p-tolyl)₃)₂. Organometallics. 1994 Dec 1;13(12):5080-5087. doi: 10.1021/om00024a059

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