Trimethylamine-N-oxide induced disproportionation of Re2(CO)10: Synthesis and X-ray crystal structure of [fac-Re(CO)3(ONMe3)3] [ReO4]

Sean D. Christie; Michael D. Clerk; Michael J. Zaworotko

doi:10.1007/BF01228770

Trimethylamine-N-oxide induced disproportionation of Re₂(CO)₁₀: Synthesis and X-ray crystal structure of [fac-Re(CO)₃(ONMe₃)₃] [ReO₄]

Sean D. Christie
, Michael D. Clerk
, Michael J. Zaworotko

Saint Mary's University Halifax

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

Abstract

An attempted synthesis of [Re(CO₃) (μ-OH)]₄, 1, by reacting Re₂(CO)₁₀ with an excess of NMe₃O in THF resulted instead in isolation of a disproportionation product, [fac-Re(CO)₃(ONMe₃)₃][ReO₄], 2. The structure of 2 was determined via X-ray crystallography: tri-clinic, P1^-, a=9.499(5), b=9.841(2), c=13.448(2)Å, α=109.92(2), β=106.89(3), γ=93.15(4)°, D_calc=2.22 g^-3 and Z=2. Least-squares refinement based on 1606 observed (I>3σ(I)) reflections gave final values of R=0.040 and R_w=0.047. The cation is a distorted octahedron that exhibits several structural manifestations of steric crowding among the bulky NMe₃O ligands.

Original language	English
Pages (from-to)	591-594
Number of pages	4
Journal	Journal of Crystal and Molecular Structure
Volume	23
Issue number	7
DOIs	https://doi.org/10.1007/BF01228770
Publication status	Published - Jul 1993
Externally published	Yes

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@article{82a7100d11954a2295b6343bd4e36e54,

title = "Trimethylamine-N-oxide induced disproportionation of Re2(CO)10: Synthesis and X-ray crystal structure of [fac-Re(CO)3(ONMe3)3] [ReO4]",

abstract = "An attempted synthesis of [Re(CO3) (μ-OH)]4, 1, by reacting Re2(CO)10 with an excess of NMe3O in THF resulted instead in isolation of a disproportionation product, [fac-Re(CO)3(ONMe3)3][ReO4], 2. The structure of 2 was determined via X-ray crystallography: tri-clinic, P1-, a=9.499(5), b=9.841(2), c=13.448(2){\AA}, α=109.92(2), β=106.89(3), γ=93.15(4)°, Dcalc=2.22 g-3 and Z=2. Least-squares refinement based on 1606 observed (I>3σ(I)) reflections gave final values of R=0.040 and Rw=0.047. The cation is a distorted octahedron that exhibits several structural manifestations of steric crowding among the bulky NMe3O ligands.",

author = "Christie, \{Sean D.\} and Clerk, \{Michael D.\} and Zaworotko, \{Michael J.\}",

year = "1993",

month = jul,

doi = "10.1007/BF01228770",

language = "English",

volume = "23",

pages = "591--594",

journal = "Journal of Crystal and Molecular Structure",

issn = "0277-8068",

number = "7",

}

TY - JOUR

T1 - Trimethylamine-N-oxide induced disproportionation of Re2(CO)10

T2 - Synthesis and X-ray crystal structure of [fac-Re(CO)3(ONMe3)3] [ReO4]

AU - Christie, Sean D.

AU - Clerk, Michael D.

AU - Zaworotko, Michael J.

PY - 1993/7

Y1 - 1993/7

N2 - An attempted synthesis of [Re(CO3) (μ-OH)]4, 1, by reacting Re2(CO)10 with an excess of NMe3O in THF resulted instead in isolation of a disproportionation product, [fac-Re(CO)3(ONMe3)3][ReO4], 2. The structure of 2 was determined via X-ray crystallography: tri-clinic, P1-, a=9.499(5), b=9.841(2), c=13.448(2)Å, α=109.92(2), β=106.89(3), γ=93.15(4)°, Dcalc=2.22 g-3 and Z=2. Least-squares refinement based on 1606 observed (I>3σ(I)) reflections gave final values of R=0.040 and Rw=0.047. The cation is a distorted octahedron that exhibits several structural manifestations of steric crowding among the bulky NMe3O ligands.

AB - An attempted synthesis of [Re(CO3) (μ-OH)]4, 1, by reacting Re2(CO)10 with an excess of NMe3O in THF resulted instead in isolation of a disproportionation product, [fac-Re(CO)3(ONMe3)3][ReO4], 2. The structure of 2 was determined via X-ray crystallography: tri-clinic, P1-, a=9.499(5), b=9.841(2), c=13.448(2)Å, α=109.92(2), β=106.89(3), γ=93.15(4)°, Dcalc=2.22 g-3 and Z=2. Least-squares refinement based on 1606 observed (I>3σ(I)) reflections gave final values of R=0.040 and Rw=0.047. The cation is a distorted octahedron that exhibits several structural manifestations of steric crowding among the bulky NMe3O ligands.

UR - https://www.scopus.com/pages/publications/0010840926

U2 - 10.1007/BF01228770

DO - 10.1007/BF01228770

M3 - Article

AN - SCOPUS:0010840926

SN - 0277-8068

VL - 23

SP - 591

EP - 594

JO - Journal of Crystal and Molecular Structure

JF - Journal of Crystal and Molecular Structure

IS - 7

ER -

Trimethylamine-N-oxide induced disproportionation of Re₂(CO)₁₀: Synthesis and X-ray crystal structure of [fac-Re(CO)₃(ONMe₃)₃] [ReO₄]

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