Synthesis and structural characterization of magnesium based coordination networks in different solvents

Debasis Banerjee; Jeffrey Finkelstein; A. Smirnov; Paul M. Forster; Lauren A. Borkowski; Simon J. Teat; John B. Parise

doi:10.1021/cg200327y

Synthesis and structural characterization of magnesium based coordination networks in different solvents

Debasis Banerjee
, Jeffrey Finkelstein
, A. Smirnov
, Paul M. Forster
, Lauren A. Borkowski
, Simon J. Teat
, John B. Parise

Geosciences

Stony Brook University

Stony Brook University
University of Nevada, Las Vegas
Lawrence Berkeley National Laboratory

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

108 Scopus citations

Abstract

Three magnesium based metal-organic frameworks, Mg₃(3,5-PDC) ₃(DMF)₃•DMF [1], Mg(3,5-PDC)(H₂O) •(H₂O) [3], and Mg₄(3,5-PDC)₄(DMF) ₂(H₂O)₂•2DMF•4.5H₂O [4], and a 2-D coordination polymer, [Mg(3,5-PDC)(H₂O)₂] [2] [PDC = pyridinedicarboxylate], were synthesized using a combination of DMF, methanol, ethanol, and water. Compound 1 [space group P2₁/n, a = 12.3475(5) Å, b = 11.1929(5) Å, c = 28.6734(12) Å, β = 98.8160(10)°, V = 3916.0(3) Å³] consists of a combination of isolated and corner-sharing magnesium octahedra connected by the organic linkers to form a 3-D network with a 12.2 Å × 4.6 Å 1-D channel. The channel contains coordinated and free DMF molecules. In compound 2 [space group C2/c, a = 9.964(5) Å, b = 12.0694(6) Å, c = 7.2763(4) Å, β = 106.4970(6)°, V = 836.70(6) Å³], PDC connects isolated seven coordinated magnesium polyhedra into a layered structure. Compound 3 [space group P6₁22, a = 11.479(1) Å, c = 14.735(3) Å, V = 1681.7(4) Å³] (previously reported) contains isolated magnesium octahedra connected by the organic linker with each other forming a 3D network. Compound 4 [space group P2₁/c, a = 13.7442(14) Å, b = 14.2887(15) Å, c = 14.1178(14) Å, β = 104.912(2)°, V = 2679.2(5) Å³] also exhibits a 3D network based on isolated magnesium octahedra with square cavities containing both disordered DMF and water molecules. The structural topologies originate due to the variable coordination ability of solvent molecules with the metal center. Water molecules coordinate with the magnesium metal centers preferably over other polar solvents (DMF, methanol, ethanol) used to synthesize the coordination networks. Despite testing multiple desolvation routes, we were unable to measure BET surface areas greater than 51.9 m²/g for compound 1.

Original language	English
Pages (from-to)	2572-2579
Number of pages	8
Journal	Crystal Growth and Design
Volume	11
Issue number	6
DOIs	https://doi.org/10.1021/cg200327y
State	Published - Jun 1 2011

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10.1021/cg200327y

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@article{7a3cfe9da0ba45d88b7a907b14225b2a,

title = "Synthesis and structural characterization of magnesium based coordination networks in different solvents",

abstract = "Three magnesium based metal-organic frameworks, Mg3(3,5-PDC) 3(DMF)3•DMF [1], Mg(3,5-PDC)(H2O) •(H2O) [3], and Mg4(3,5-PDC)4(DMF) 2(H2O)2•2DMF•4.5H2O [4], and a 2-D coordination polymer, [Mg(3,5-PDC)(H2O)2] [2] [PDC = pyridinedicarboxylate], were synthesized using a combination of DMF, methanol, ethanol, and water. Compound 1 [space group P21/n, a = 12.3475(5) {\AA}, b = 11.1929(5) {\AA}, c = 28.6734(12) {\AA}, β = 98.8160(10)°, V = 3916.0(3) {\AA}3] consists of a combination of isolated and corner-sharing magnesium octahedra connected by the organic linkers to form a 3-D network with a 12.2 {\AA} × 4.6 {\AA} 1-D channel. The channel contains coordinated and free DMF molecules. In compound 2 [space group C2/c, a = 9.964(5) {\AA}, b = 12.0694(6) {\AA}, c = 7.2763(4) {\AA}, β = 106.4970(6)°, V = 836.70(6) {\AA}3], PDC connects isolated seven coordinated magnesium polyhedra into a layered structure. Compound 3 [space group P6122, a = 11.479(1) {\AA}, c = 14.735(3) {\AA}, V = 1681.7(4) {\AA}3] (previously reported) contains isolated magnesium octahedra connected by the organic linker with each other forming a 3D network. Compound 4 [space group P21/c, a = 13.7442(14) {\AA}, b = 14.2887(15) {\AA}, c = 14.1178(14) {\AA}, β = 104.912(2)°, V = 2679.2(5) {\AA}3] also exhibits a 3D network based on isolated magnesium octahedra with square cavities containing both disordered DMF and water molecules. The structural topologies originate due to the variable coordination ability of solvent molecules with the metal center. Water molecules coordinate with the magnesium metal centers preferably over other polar solvents (DMF, methanol, ethanol) used to synthesize the coordination networks. Despite testing multiple desolvation routes, we were unable to measure BET surface areas greater than 51.9 m2/g for compound 1.",

author = "Debasis Banerjee and Jeffrey Finkelstein and A. Smirnov and Forster, \{Paul M.\} and Borkowski, \{Lauren A.\} and Teat, \{Simon J.\} and Parise, \{John B.\}",

year = "2011",

month = jun,

day = "1",

doi = "10.1021/cg200327y",

language = "English",

volume = "11",

pages = "2572--2579",

journal = "Crystal Growth and Design",

issn = "1528-7483",

publisher = "American Chemical Society",

number = "6",

}

TY - JOUR

T1 - Synthesis and structural characterization of magnesium based coordination networks in different solvents

AU - Banerjee, Debasis

AU - Finkelstein, Jeffrey

AU - Smirnov, A.

AU - Forster, Paul M.

AU - Borkowski, Lauren A.

AU - Teat, Simon J.

AU - Parise, John B.

PY - 2011/6/1

Y1 - 2011/6/1

N2 - Three magnesium based metal-organic frameworks, Mg3(3,5-PDC) 3(DMF)3•DMF [1], Mg(3,5-PDC)(H2O) •(H2O) [3], and Mg4(3,5-PDC)4(DMF) 2(H2O)2•2DMF•4.5H2O [4], and a 2-D coordination polymer, [Mg(3,5-PDC)(H2O)2] [2] [PDC = pyridinedicarboxylate], were synthesized using a combination of DMF, methanol, ethanol, and water. Compound 1 [space group P21/n, a = 12.3475(5) Å, b = 11.1929(5) Å, c = 28.6734(12) Å, β = 98.8160(10)°, V = 3916.0(3) Å3] consists of a combination of isolated and corner-sharing magnesium octahedra connected by the organic linkers to form a 3-D network with a 12.2 Å × 4.6 Å 1-D channel. The channel contains coordinated and free DMF molecules. In compound 2 [space group C2/c, a = 9.964(5) Å, b = 12.0694(6) Å, c = 7.2763(4) Å, β = 106.4970(6)°, V = 836.70(6) Å3], PDC connects isolated seven coordinated magnesium polyhedra into a layered structure. Compound 3 [space group P6122, a = 11.479(1) Å, c = 14.735(3) Å, V = 1681.7(4) Å3] (previously reported) contains isolated magnesium octahedra connected by the organic linker with each other forming a 3D network. Compound 4 [space group P21/c, a = 13.7442(14) Å, b = 14.2887(15) Å, c = 14.1178(14) Å, β = 104.912(2)°, V = 2679.2(5) Å3] also exhibits a 3D network based on isolated magnesium octahedra with square cavities containing both disordered DMF and water molecules. The structural topologies originate due to the variable coordination ability of solvent molecules with the metal center. Water molecules coordinate with the magnesium metal centers preferably over other polar solvents (DMF, methanol, ethanol) used to synthesize the coordination networks. Despite testing multiple desolvation routes, we were unable to measure BET surface areas greater than 51.9 m2/g for compound 1.

AB - Three magnesium based metal-organic frameworks, Mg3(3,5-PDC) 3(DMF)3•DMF [1], Mg(3,5-PDC)(H2O) •(H2O) [3], and Mg4(3,5-PDC)4(DMF) 2(H2O)2•2DMF•4.5H2O [4], and a 2-D coordination polymer, [Mg(3,5-PDC)(H2O)2] [2] [PDC = pyridinedicarboxylate], were synthesized using a combination of DMF, methanol, ethanol, and water. Compound 1 [space group P21/n, a = 12.3475(5) Å, b = 11.1929(5) Å, c = 28.6734(12) Å, β = 98.8160(10)°, V = 3916.0(3) Å3] consists of a combination of isolated and corner-sharing magnesium octahedra connected by the organic linkers to form a 3-D network with a 12.2 Å × 4.6 Å 1-D channel. The channel contains coordinated and free DMF molecules. In compound 2 [space group C2/c, a = 9.964(5) Å, b = 12.0694(6) Å, c = 7.2763(4) Å, β = 106.4970(6)°, V = 836.70(6) Å3], PDC connects isolated seven coordinated magnesium polyhedra into a layered structure. Compound 3 [space group P6122, a = 11.479(1) Å, c = 14.735(3) Å, V = 1681.7(4) Å3] (previously reported) contains isolated magnesium octahedra connected by the organic linker with each other forming a 3D network. Compound 4 [space group P21/c, a = 13.7442(14) Å, b = 14.2887(15) Å, c = 14.1178(14) Å, β = 104.912(2)°, V = 2679.2(5) Å3] also exhibits a 3D network based on isolated magnesium octahedra with square cavities containing both disordered DMF and water molecules. The structural topologies originate due to the variable coordination ability of solvent molecules with the metal center. Water molecules coordinate with the magnesium metal centers preferably over other polar solvents (DMF, methanol, ethanol) used to synthesize the coordination networks. Despite testing multiple desolvation routes, we were unable to measure BET surface areas greater than 51.9 m2/g for compound 1.

UR - https://www.scopus.com/pages/publications/79958019531

U2 - 10.1021/cg200327y

DO - 10.1021/cg200327y

M3 - Article

SN - 1528-7483

VL - 11

SP - 2572

EP - 2579

JO - Crystal Growth and Design

JF - Crystal Growth and Design

IS - 6

ER -

Synthesis and structural characterization of magnesium based coordination networks in different solvents

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