Synthesis and characterization by diffraction and 31P- and 77Se-NMR spectroscopy of [Mo3(μ3-Se)(μ2-Se2) 3(N(SePPh2)2)3]Br and [Mo3(μ3-Se)(μ2-Se2) 3(Se2P(OCH2CH3)2) 3]Br

Virginie Béreau; James A. Ibers

doi:10.1016/S1387-1609(00)00124-9

Synthesis and characterization by diffraction and ³¹P- and ⁷⁷Se-NMR spectroscopy of [Mo₃(μ₃-Se)(μ₂-Se₂) ₃(N(SePPh₂)₂)₃]Br and [Mo₃(μ₃-Se)(μ₂-Se₂) ₃(Se₂P(OCH₂CH₃)₂) ₃]Br

Virginie Béreau, James A. Ibers

Chemistry

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

20 Scopus citations

Abstract

The new Mo/Se clusters [Mo₃(μ₃-Se)(μ₂-Se₂) ₃(N(SePPh₂)₂)₃]Br (1) and [Mo₃(μ₃-Se)(μ₂-Se₂) ₃(Se₂P(OCH₂CH₃)₂) ₃]Br (2) have been synthesized by the selective substitution of the bromo ligands in the starting material [PPh₄]₂[Mo₃(μ₃-Se)(μ ₂-Se₂)₃Br₆] with the selenoorgano bidentate ligands [N(SePPh₂)₂]^- and [Se₂P(OEt)₂]^-. The complexes have been characterized in solution by ³¹P- and ⁷⁷Se-NMR spectroscopy and in the solid state by single crystal X-ray diffraction; the same cation structures are present both in solution and in the solid state. Crystallographic data for 1: [Mo₃(μ₃-Se)(μ₂-Se₂) ₃(N(SePPh₂)₂)₃]Br·3 CH₂Cl₂, C₇₂H₆₀BrMo₃N₃P₆Se ₁₃·3 CH₂Cl₂, trigonal, space group R₃, a=21.299 (10) Å, c=38.433 (27) Å, V=15 100 (15) Å³, T=-120°C, Z=6; crystallographic data for 2: Mo₃(μ₃-Se)(μ₂-Se₂) ₃(Se₂P(OCH₂CH₃)₂) ₃]Br, C₁₂H₃₀BrMo₃P₃O₃Se ₁₃, monoclinic, space group P2₁/n, a=13.404 (2) Å, b=22.732 (4) Å, c=13.932 (3) Å, β=113.134 (3)°, V=3 903.7(12) Å³, T=-120°C, Z=4.

Original language	English (US)
Pages (from-to)	123-129
Number of pages	7
Journal	Comptes Rendus de l'Academie des Sciences - Series IIc: Chemistry
Volume	3
Issue number	2
DOIs	https://doi.org/10.1016/S1387-1609(00)00124-9
State	Published - Apr 1 2000

Keywords

Amine
Cluster de molybdène
Phosphate
Phosphine
RMN de Se
Sélénium

ASJC Scopus subject areas

General Chemistry

Access to Document

10.1016/S1387-1609(00)00124-9

Cite this

@article{665a360c71634270aa78a43f22f919c5,

title = "Synthesis and characterization by diffraction and 31P- and 77Se-NMR spectroscopy of [Mo3(μ3-Se)(μ2-Se2) 3(N(SePPh2)2)3]Br and [Mo3(μ3-Se)(μ2-Se2) 3(Se2P(OCH2CH3)2) 3]Br",

abstract = "The new Mo/Se clusters [Mo3(μ3-Se)(μ2-Se2) 3(N(SePPh2)2)3]Br (1) and [Mo3(μ3-Se)(μ2-Se2) 3(Se2P(OCH2CH3)2) 3]Br (2) have been synthesized by the selective substitution of the bromo ligands in the starting material [PPh4]2[Mo3(μ3-Se)(μ 2-Se2)3Br6] with the selenoorgano bidentate ligands [N(SePPh2)2]- and [Se2P(OEt)2]-. The complexes have been characterized in solution by 31P- and 77Se-NMR spectroscopy and in the solid state by single crystal X-ray diffraction; the same cation structures are present both in solution and in the solid state. Crystallographic data for 1: [Mo3(μ3-Se)(μ2-Se2) 3(N(SePPh2)2)3]Br·3 CH2Cl2, C72H60BrMo3N3P6Se 13·3 CH2Cl2, trigonal, space group R3, a=21.299 (10) {\AA}, c=38.433 (27) {\AA}, V=15 100 (15) {\AA}3, T=-120°C, Z=6; crystallographic data for 2: Mo3(μ3-Se)(μ2-Se2) 3(Se2P(OCH2CH3)2) 3]Br, C12H30BrMo3P3O3Se 13, monoclinic, space group P21/n, a=13.404 (2) {\AA}, b=22.732 (4) {\AA}, c=13.932 (3) {\AA}, β=113.134 (3)°, V=3 903.7(12) {\AA}3, T=-120°C, Z=4.",

keywords = "Amine, Cluster de molybd{\`e}ne, Phosphate, Phosphine, RMN de Se, S{\'e}l{\'e}nium",

author = "Virginie B{\'e}reau and Ibers, {James A.}",

note = "Funding Information: This work was kindly supported by the U.S. National Science Foundation, Grant No. CHE-9819385.",

year = "2000",

month = apr,

day = "1",

doi = "10.1016/S1387-1609(00)00124-9",

language = "English (US)",

volume = "3",

pages = "123--129",

journal = "Comptes Rendus de l'Academie des Sciences - Series IIc: Chemistry",

issn = "1387-1609",

publisher = "Elsevier BV",

number = "2",

}

Synthesis and characterization by diffraction and ³¹P- and ⁷⁷Se-NMR spectroscopy of [Mo₃(μ₃-Se)(μ₂-Se₂) ₃(N(SePPh₂)₂)₃]Br and [Mo₃(μ₃-Se)(μ₂-Se₂) ₃(Se₂P(OCH₂CH₃)₂) ₃]Br. / Béreau, Virginie; Ibers, James A.
In: Comptes Rendus de l'Academie des Sciences - Series IIc: Chemistry, Vol. 3, No. 2, 01.04.2000, p. 123-129.

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

TY - JOUR

T1 - Synthesis and characterization by diffraction and 31P- and 77Se-NMR spectroscopy of [Mo3(μ3-Se)(μ2-Se2) 3(N(SePPh2)2)3]Br and [Mo3(μ3-Se)(μ2-Se2) 3(Se2P(OCH2CH3)2) 3]Br

AU - Béreau, Virginie

AU - Ibers, James A.

N1 - Funding Information: This work was kindly supported by the U.S. National Science Foundation, Grant No. CHE-9819385.

PY - 2000/4/1

Y1 - 2000/4/1

N2 - The new Mo/Se clusters [Mo3(μ3-Se)(μ2-Se2) 3(N(SePPh2)2)3]Br (1) and [Mo3(μ3-Se)(μ2-Se2) 3(Se2P(OCH2CH3)2) 3]Br (2) have been synthesized by the selective substitution of the bromo ligands in the starting material [PPh4]2[Mo3(μ3-Se)(μ 2-Se2)3Br6] with the selenoorgano bidentate ligands [N(SePPh2)2]- and [Se2P(OEt)2]-. The complexes have been characterized in solution by 31P- and 77Se-NMR spectroscopy and in the solid state by single crystal X-ray diffraction; the same cation structures are present both in solution and in the solid state. Crystallographic data for 1: [Mo3(μ3-Se)(μ2-Se2) 3(N(SePPh2)2)3]Br·3 CH2Cl2, C72H60BrMo3N3P6Se 13·3 CH2Cl2, trigonal, space group R3, a=21.299 (10) Å, c=38.433 (27) Å, V=15 100 (15) Å3, T=-120°C, Z=6; crystallographic data for 2: Mo3(μ3-Se)(μ2-Se2) 3(Se2P(OCH2CH3)2) 3]Br, C12H30BrMo3P3O3Se 13, monoclinic, space group P21/n, a=13.404 (2) Å, b=22.732 (4) Å, c=13.932 (3) Å, β=113.134 (3)°, V=3 903.7(12) Å3, T=-120°C, Z=4.

AB - The new Mo/Se clusters [Mo3(μ3-Se)(μ2-Se2) 3(N(SePPh2)2)3]Br (1) and [Mo3(μ3-Se)(μ2-Se2) 3(Se2P(OCH2CH3)2) 3]Br (2) have been synthesized by the selective substitution of the bromo ligands in the starting material [PPh4]2[Mo3(μ3-Se)(μ 2-Se2)3Br6] with the selenoorgano bidentate ligands [N(SePPh2)2]- and [Se2P(OEt)2]-. The complexes have been characterized in solution by 31P- and 77Se-NMR spectroscopy and in the solid state by single crystal X-ray diffraction; the same cation structures are present both in solution and in the solid state. Crystallographic data for 1: [Mo3(μ3-Se)(μ2-Se2) 3(N(SePPh2)2)3]Br·3 CH2Cl2, C72H60BrMo3N3P6Se 13·3 CH2Cl2, trigonal, space group R3, a=21.299 (10) Å, c=38.433 (27) Å, V=15 100 (15) Å3, T=-120°C, Z=6; crystallographic data for 2: Mo3(μ3-Se)(μ2-Se2) 3(Se2P(OCH2CH3)2) 3]Br, C12H30BrMo3P3O3Se 13, monoclinic, space group P21/n, a=13.404 (2) Å, b=22.732 (4) Å, c=13.932 (3) Å, β=113.134 (3)°, V=3 903.7(12) Å3, T=-120°C, Z=4.

KW - Amine

KW - Cluster de molybdène

KW - Phosphate

KW - Phosphine

KW - RMN de Se

KW - Sélénium

UR - http://www.scopus.com/inward/record.url?scp=0008346721&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=0008346721&partnerID=8YFLogxK

U2 - 10.1016/S1387-1609(00)00124-9

DO - 10.1016/S1387-1609(00)00124-9

M3 - Article

AN - SCOPUS:0008346721

SN - 1387-1609

VL - 3

SP - 123

EP - 129

JO - Comptes Rendus de l'Academie des Sciences - Series IIc: Chemistry

JF - Comptes Rendus de l'Academie des Sciences - Series IIc: Chemistry

IS - 2

ER -

Synthesis and characterization by diffraction and ³¹P- and ⁷⁷Se-NMR spectroscopy of [Mo₃(μ₃-Se)(μ₂-Se₂) ₃(N(SePPh₂)₂)₃]Br and [Mo₃(μ₃-Se)(μ₂-Se₂) ₃(Se₂P(OCH₂CH₃)₂) ₃]Br

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CCDC 136236: Experimental Crystal Structure Determination

CCDC 136235: Experimental Crystal Structure Determination

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Synthesis and characterization by diffraction and 31P- and 77Se-NMR spectroscopy of [Mo3(μ3-Se)(μ2-Se2) 3(N(SePPh2)2)3]Br and [Mo3(μ3-Se)(μ2-Se2) 3(Se2P(OCH2CH3)2) 3]Br

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CCDC 136236: Experimental Crystal Structure Determination

CCDC 136235: Experimental Crystal Structure Determination

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Synthesis and characterization by diffraction and ³¹P- and ⁷⁷Se-NMR spectroscopy of [Mo₃(μ₃-Se)(μ₂-Se₂) ₃(N(SePPh₂)₂)₃]Br and [Mo₃(μ₃-Se)(μ₂-Se₂) ₃(Se₂P(OCH₂CH₃)₂) ₃]Br