Synthesis and characterization of the silver maleonitrilediselenolates and silver maleonitriledithiolates [K([2.2.2]-cryptand)]4[Ag4 (Se2C2(CN)2)4], [Na([2.2.2]-cryptand)]4[Ag4 (S2C2(CN)2)4]·0.33MeCN

C. C. McLauchlan; J. A. Ibers

doi:10.1021/ic000868q

Synthesis and characterization of the silver maleonitrilediselenolates and silver maleonitriledithiolates [K([2.2.2]-cryptand)]₄[Ag₄ (Se₂C₂(CN)₂)₄], [Na([2.2.2]-cryptand)]₄[Ag₄ (S₂C₂(CN)₂)₄]·0.33MeCN

C. C. McLauchlan, J. A. Ibers^*

^*Corresponding author for this work

Chemistry

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

21 Scopus citations

Abstract

Reaction of AgBF₄, KNH₂, K₂Se, Se, and [2.2.2]-cryptand in acetonitrile yields [K([2.2.2]-cryptand)]₄[Ag₄ (Se₂C₂(CN)₂)₄] (1). In the unit cell of 1 there are four [K([2.2.2]-cryptand)]⁺ units and a tetrahedral Ag₄ anionic core coordinated in μ₁-Se, μ₂-Se fashion by each of four mns ligands (mns = maleonitrilediselenolate, [Se₂C₂(CN)₂]^2-). Reaction of AgNO₃, Na₂(mnt) (mnt = maleonitriledithiolate, [S₂C₂(CN)₂]^2-), and [2.2.2]-cryptand in acetonitrile yields [Na([2.2.2]-cryptand)]₄[Ag₄ (mnt)₄]·0.33MeCN (2). The Ag₄ anion of 2 is analogous to that in 1. Reaction of AgNO₃, Na₂(mnt), and [NBu₄]Br in acetonitrile yields [NBu₄]₄[Ag₄(mnt)₄] (3). The anion of 3 also comprises an Ag₄ core coordinated by four mnt ligands, but the Ag₄ core is diamond-shaped rather than tetrahedral. Reaction of [K([2.2.2]-cryptand)]₃[Ag(mns)(Se₆)] with KNH₂ and [2.2.2]-cryptand in acetonitrile yields [K([2.2.2]-cryptand)]₃[Ag(mns)₂]·2MeCN (4). The anion of 4 comprises an Ag center coordinated by two mns ligands in a tetrahedral arrangement. Reaction of AgNO₃, 2 equiv of Na₂(mnt), and [2.2.2]-cryptand in acetonitrile yields [Na([2.2.2]-cryptand)]₃[Ag(mnt)₂] (5). The anion of 5 is analogous to that of 4. Electronic absorption and infrared spectra of each complex show behavior characteristic of metal-maleonitriledichalcogenates. Crystal data (153 K): 1, P2/n, Z = 2, a = 18.362(2) Å, b = 16.500(1) Å, c = 19.673(2) Å, β = 94.67(1)°, V = 5941(1) Å³; 2, P4̄, Z = 4, a = 27.039(4) Å, c = 15.358(3) Å, V = 11229(3) Å³; 3, P2₁/c, Z = 6, a = 15.689(3) Å, b = 51.924(11) Å, c = 17.393(4) Å, β = 93.51(1)°, V = 14142(5) Å³; 4, P2₁/c, Z = 4, a = 13.997(1) Å, b = 21.866(2) Å, c = 28.281(2) Å, β = 97.72(1)°, V = 8578(1) Å³; 5, P2/n, Z = 2, a = 11.547(2) Å, b = 11.766(2) Å, c = 27.774(6) Å, β = 91.85(3)°, V = 3772(1) Å³.

Original language	English (US)
Pages (from-to)	1809-1815
Number of pages	7
Journal	Inorganic chemistry
Volume	40
Issue number	8
DOIs	https://doi.org/10.1021/ic000868q
State	Published - Apr 9 2001

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry

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@article{523e0b003a8c44a2b53e788cacfb0f16,

title = "Synthesis and characterization of the silver maleonitrilediselenolates and silver maleonitriledithiolates [K([2.2.2]-cryptand)]4[Ag4 (Se2C2(CN)2)4], [Na([2.2.2]-cryptand)]4[Ag4 (S2C2(CN)2)4]·0.33MeCN",

abstract = "Reaction of AgBF4, KNH2, K2Se, Se, and [2.2.2]-cryptand in acetonitrile yields [K([2.2.2]-cryptand)]4[Ag4 (Se2C2(CN)2)4] (1). In the unit cell of 1 there are four [K([2.2.2]-cryptand)]+ units and a tetrahedral Ag4 anionic core coordinated in μ1-Se, μ2-Se fashion by each of four mns ligands (mns = maleonitrilediselenolate, [Se2C2(CN)2]2-). Reaction of AgNO3, Na2(mnt) (mnt = maleonitriledithiolate, [S2C2(CN)2]2-), and [2.2.2]-cryptand in acetonitrile yields [Na([2.2.2]-cryptand)]4[Ag4 (mnt)4]·0.33MeCN (2). The Ag4 anion of 2 is analogous to that in 1. Reaction of AgNO3, Na2(mnt), and [NBu4]Br in acetonitrile yields [NBu4]4[Ag4(mnt)4] (3). The anion of 3 also comprises an Ag4 core coordinated by four mnt ligands, but the Ag4 core is diamond-shaped rather than tetrahedral. Reaction of [K([2.2.2]-cryptand)]3[Ag(mns)(Se6)] with KNH2 and [2.2.2]-cryptand in acetonitrile yields [K([2.2.2]-cryptand)]3[Ag(mns)2]·2MeCN (4). The anion of 4 comprises an Ag center coordinated by two mns ligands in a tetrahedral arrangement. Reaction of AgNO3, 2 equiv of Na2(mnt), and [2.2.2]-cryptand in acetonitrile yields [Na([2.2.2]-cryptand)]3[Ag(mnt)2] (5). The anion of 5 is analogous to that of 4. Electronic absorption and infrared spectra of each complex show behavior characteristic of metal-maleonitriledichalcogenates. Crystal data (153 K): 1, P2/n, Z = 2, a = 18.362(2) {\AA}, b = 16.500(1) {\AA}, c = 19.673(2) {\AA}, β = 94.67(1)°, V = 5941(1) {\AA}3; 2, P{\=4}, Z = 4, a = 27.039(4) {\AA}, c = 15.358(3) {\AA}, V = 11229(3) {\AA}3; 3, P21/c, Z = 6, a = 15.689(3) {\AA}, b = 51.924(11) {\AA}, c = 17.393(4) {\AA}, β = 93.51(1)°, V = 14142(5) {\AA}3; 4, P21/c, Z = 4, a = 13.997(1) {\AA}, b = 21.866(2) {\AA}, c = 28.281(2) {\AA}, β = 97.72(1)°, V = 8578(1) {\AA}3; 5, P2/n, Z = 2, a = 11.547(2) {\AA}, b = 11.766(2) {\AA}, c = 27.774(6) {\AA}, β = 91.85(3)°, V = 3772(1) {\AA}3.",

author = "McLauchlan, {C. C.} and Ibers, {J. A.}",

year = "2001",

month = apr,

day = "9",

doi = "10.1021/ic000868q",

language = "English (US)",

volume = "40",

pages = "1809--1815",

journal = "Inorganic Chemistry",

issn = "0020-1669",

publisher = "American Chemical Society",

number = "8",

}

Synthesis and characterization of the silver maleonitrilediselenolates and silver maleonitriledithiolates [K([2.2.2]-cryptand)]₄[Ag₄ (Se₂C₂(CN)₂)₄], [Na([2.2.2]-cryptand)]₄[Ag₄ (S₂C₂(CN)₂)₄]·0.33MeCN. / McLauchlan, C. C.; Ibers, J. A.

In: Inorganic chemistry, Vol. 40, No. 8, 09.04.2001, p. 1809-1815.

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

TY - JOUR

T1 - Synthesis and characterization of the silver maleonitrilediselenolates and silver maleonitriledithiolates [K([2.2.2]-cryptand)]4[Ag4 (Se2C2(CN)2)4], [Na([2.2.2]-cryptand)]4[Ag4 (S2C2(CN)2)4]·0.33MeCN

AU - McLauchlan, C. C.

AU - Ibers, J. A.

PY - 2001/4/9

Y1 - 2001/4/9

N2 - Reaction of AgBF4, KNH2, K2Se, Se, and [2.2.2]-cryptand in acetonitrile yields [K([2.2.2]-cryptand)]4[Ag4 (Se2C2(CN)2)4] (1). In the unit cell of 1 there are four [K([2.2.2]-cryptand)]+ units and a tetrahedral Ag4 anionic core coordinated in μ1-Se, μ2-Se fashion by each of four mns ligands (mns = maleonitrilediselenolate, [Se2C2(CN)2]2-). Reaction of AgNO3, Na2(mnt) (mnt = maleonitriledithiolate, [S2C2(CN)2]2-), and [2.2.2]-cryptand in acetonitrile yields [Na([2.2.2]-cryptand)]4[Ag4 (mnt)4]·0.33MeCN (2). The Ag4 anion of 2 is analogous to that in 1. Reaction of AgNO3, Na2(mnt), and [NBu4]Br in acetonitrile yields [NBu4]4[Ag4(mnt)4] (3). The anion of 3 also comprises an Ag4 core coordinated by four mnt ligands, but the Ag4 core is diamond-shaped rather than tetrahedral. Reaction of [K([2.2.2]-cryptand)]3[Ag(mns)(Se6)] with KNH2 and [2.2.2]-cryptand in acetonitrile yields [K([2.2.2]-cryptand)]3[Ag(mns)2]·2MeCN (4). The anion of 4 comprises an Ag center coordinated by two mns ligands in a tetrahedral arrangement. Reaction of AgNO3, 2 equiv of Na2(mnt), and [2.2.2]-cryptand in acetonitrile yields [Na([2.2.2]-cryptand)]3[Ag(mnt)2] (5). The anion of 5 is analogous to that of 4. Electronic absorption and infrared spectra of each complex show behavior characteristic of metal-maleonitriledichalcogenates. Crystal data (153 K): 1, P2/n, Z = 2, a = 18.362(2) Å, b = 16.500(1) Å, c = 19.673(2) Å, β = 94.67(1)°, V = 5941(1) Å3; 2, P4̄, Z = 4, a = 27.039(4) Å, c = 15.358(3) Å, V = 11229(3) Å3; 3, P21/c, Z = 6, a = 15.689(3) Å, b = 51.924(11) Å, c = 17.393(4) Å, β = 93.51(1)°, V = 14142(5) Å3; 4, P21/c, Z = 4, a = 13.997(1) Å, b = 21.866(2) Å, c = 28.281(2) Å, β = 97.72(1)°, V = 8578(1) Å3; 5, P2/n, Z = 2, a = 11.547(2) Å, b = 11.766(2) Å, c = 27.774(6) Å, β = 91.85(3)°, V = 3772(1) Å3.

AB - Reaction of AgBF4, KNH2, K2Se, Se, and [2.2.2]-cryptand in acetonitrile yields [K([2.2.2]-cryptand)]4[Ag4 (Se2C2(CN)2)4] (1). In the unit cell of 1 there are four [K([2.2.2]-cryptand)]+ units and a tetrahedral Ag4 anionic core coordinated in μ1-Se, μ2-Se fashion by each of four mns ligands (mns = maleonitrilediselenolate, [Se2C2(CN)2]2-). Reaction of AgNO3, Na2(mnt) (mnt = maleonitriledithiolate, [S2C2(CN)2]2-), and [2.2.2]-cryptand in acetonitrile yields [Na([2.2.2]-cryptand)]4[Ag4 (mnt)4]·0.33MeCN (2). The Ag4 anion of 2 is analogous to that in 1. Reaction of AgNO3, Na2(mnt), and [NBu4]Br in acetonitrile yields [NBu4]4[Ag4(mnt)4] (3). The anion of 3 also comprises an Ag4 core coordinated by four mnt ligands, but the Ag4 core is diamond-shaped rather than tetrahedral. Reaction of [K([2.2.2]-cryptand)]3[Ag(mns)(Se6)] with KNH2 and [2.2.2]-cryptand in acetonitrile yields [K([2.2.2]-cryptand)]3[Ag(mns)2]·2MeCN (4). The anion of 4 comprises an Ag center coordinated by two mns ligands in a tetrahedral arrangement. Reaction of AgNO3, 2 equiv of Na2(mnt), and [2.2.2]-cryptand in acetonitrile yields [Na([2.2.2]-cryptand)]3[Ag(mnt)2] (5). The anion of 5 is analogous to that of 4. Electronic absorption and infrared spectra of each complex show behavior characteristic of metal-maleonitriledichalcogenates. Crystal data (153 K): 1, P2/n, Z = 2, a = 18.362(2) Å, b = 16.500(1) Å, c = 19.673(2) Å, β = 94.67(1)°, V = 5941(1) Å3; 2, P4̄, Z = 4, a = 27.039(4) Å, c = 15.358(3) Å, V = 11229(3) Å3; 3, P21/c, Z = 6, a = 15.689(3) Å, b = 51.924(11) Å, c = 17.393(4) Å, β = 93.51(1)°, V = 14142(5) Å3; 4, P21/c, Z = 4, a = 13.997(1) Å, b = 21.866(2) Å, c = 28.281(2) Å, β = 97.72(1)°, V = 8578(1) Å3; 5, P2/n, Z = 2, a = 11.547(2) Å, b = 11.766(2) Å, c = 27.774(6) Å, β = 91.85(3)°, V = 3772(1) Å3.

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