Synthesis and Characterization of a New Series of Zinc Phosphites

C. Yolanda Ortiz-avila; Philip J. Squattrito; Minghuey Shieh; Abraham Clearfield

doi:10.1021/ic00312a021

Synthesis and Characterization of a New Series of Zinc Phosphites

C. Yolanda Ortiz-avila, Philip J. Squattrito, Minghuey Shieh, Abraham Clearfield^*

^*Corresponding author for this work

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

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Abstract

Several new zinc phosphites have been synthesized in aqueous solution by reactions of Zn²⁺ with H₃P0₃ and either Na⁺, K⁺, or Ba²⁺. The structures were determined by single-crystal X-ray diffraction techniques. Zn(H₂PO₃)₂⋅3H₂O; R₃ a = 21.128 (2) Å, c = 7.769 (6) Å, V = 3003 (2) Å³, Z = 18, R(F) = 0.073 for 494 observations (I > 3σ(I)), 82 variables. Zn₂(HPO₃)₂-(H₂O)₄⋅H₂O: PĪ, a = 7.670 (2) Å, b = 9.454 (1) Å, c = 7.554 (1) Å, α = 90.83 (1)°, β = 92.90 (1)°, y = 88.54 (2)°, V= 546.9 (2) Å³, Z = 2, R(F) = 0.022 for 1430 observations ( I > 3σ(I)) 175 variables. Zn₃Na₂(HPO₃)₄: Pnma, a= 8.331 (2) Å, b = 12.243 (2) Å, c = 12.669 (1) Å, V = 1292.2 (6) Å³, Z = 4, R(F) = 0.038 for 704 observations (I > 3σ(I)), 103 variables. Zn₃K₂(HPO₃)₄: P2₁/c,a = 12.373 (2) Å, b = 13.635 (2) Å, c = 8.571 (2) Å, β = 90.24 (1)°, V= 1445.9 (4) Å³, Z = 4, R(F) = 0.037 for 1525 observations ( I > 3σ(I)), 206 variables. Zn₃Ba(HPO₃)₄(H₂O)₆: C2/c, a = 22.707 (2) Å, b = 5.302 (3) Å, c = 15.029 (1) Å, β = 105.28 (1)°, V= 1745 (1) Å³, Z = 4, R(F) = 0.054 for 1530 observations (I> 3σ(I))_t141 variables. Each of the five structures is a new type with the Zn atoms in either octahedral or tetrahedral coordination bridged by phosphite groups to produce a framework of zinc and phosphorus-centered oxygen polyhedra. Several of the frameworks have open channels lined with phosphite H atoms or coordinated water molecules. In some cases, these polyhedra are bridged by alkali-metal or alkaline-earth-metal ions to produce different frameworks. The exact nature of each structure is highly dependent on the identity of the second metal as each adopts a different coordination environment. The coordination numbers of the Na⁺, K⁺, and Ba²⁺ ions are 6, 7, and 12, respectively. The role of the alkali and alkaline-earth metals in the structures is discussed, and the phosphite structures are compared with similar known phosphates.

Original language	English
Pages (from-to)	2608-2615
Number of pages	8
Journal	Inorganic Chemistry
Volume	28
Issue number	13
DOIs	https://doi.org/10.1021/ic00312a021
Publication status	Published - 1989 Jun 1
Externally published	Yes

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry

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10.1021/ic00312a021

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@article{fd405f8ec0c24b65886682d9cf7487c6,

title = "Synthesis and Characterization of a New Series of Zinc Phosphites",

abstract = "Several new zinc phosphites have been synthesized in aqueous solution by reactions of Zn2+ with H3P03 and either Na+, K+, or Ba2+. The structures were determined by single-crystal X-ray diffraction techniques. Zn(H2PO3)2⋅3H2O; R3 a = 21.128 (2) {\AA}, c = 7.769 (6) {\AA}, V = 3003 (2) {\AA}3, Z = 18, R(F) = 0.073 for 494 observations (I > 3σ(I)), 82 variables. Zn2(HPO3)2-(H2O)4⋅H2O: PĪ, a = 7.670 (2) {\AA}, b = 9.454 (1) {\AA}, c = 7.554 (1) {\AA}, α = 90.83 (1)°, β = 92.90 (1)°, y = 88.54 (2)°, V= 546.9 (2) {\AA}3, Z = 2, R(F) = 0.022 for 1430 observations ( I > 3σ(I)) 175 variables. Zn3Na2(HPO3)4: Pnma, a= 8.331 (2) {\AA}, b = 12.243 (2) {\AA}, c = 12.669 (1) {\AA}, V = 1292.2 (6) {\AA}3, Z = 4, R(F) = 0.038 for 704 observations (I > 3σ(I)), 103 variables. Zn3K2(HPO3)4: P21/c,a = 12.373 (2) {\AA}, b = 13.635 (2) {\AA}, c = 8.571 (2) {\AA}, β = 90.24 (1)°, V= 1445.9 (4) {\AA}3, Z = 4, R(F) = 0.037 for 1525 observations ( I > 3σ(I)), 206 variables. Zn3Ba(HPO3)4(H2O)6: C2/c, a = 22.707 (2) {\AA}, b = 5.302 (3) {\AA}, c = 15.029 (1) {\AA}, β = 105.28 (1)°, V= 1745 (1) {\AA}3, Z = 4, R(F) = 0.054 for 1530 observations (I> 3σ(I))t141 variables. Each of the five structures is a new type with the Zn atoms in either octahedral or tetrahedral coordination bridged by phosphite groups to produce a framework of zinc and phosphorus-centered oxygen polyhedra. Several of the frameworks have open channels lined with phosphite H atoms or coordinated water molecules. In some cases, these polyhedra are bridged by alkali-metal or alkaline-earth-metal ions to produce different frameworks. The exact nature of each structure is highly dependent on the identity of the second metal as each adopts a different coordination environment. The coordination numbers of the Na+, K+, and Ba2+ ions are 6, 7, and 12, respectively. The role of the alkali and alkaline-earth metals in the structures is discussed, and the phosphite structures are compared with similar known phosphates.",

author = "Ortiz-avila, {C. Yolanda} and Squattrito, {Philip J.} and Minghuey Shieh and Abraham Clearfield",

year = "1989",

month = jun,

day = "1",

doi = "10.1021/ic00312a021",

language = "English",

volume = "28",

pages = "2608--2615",

journal = "Inorganic Chemistry",

issn = "0020-1669",

publisher = "American Chemical Society",

number = "13",

}

TY - JOUR

T1 - Synthesis and Characterization of a New Series of Zinc Phosphites

AU - Ortiz-avila, C. Yolanda

AU - Squattrito, Philip J.

AU - Shieh, Minghuey

AU - Clearfield, Abraham

PY - 1989/6/1

Y1 - 1989/6/1

N2 - Several new zinc phosphites have been synthesized in aqueous solution by reactions of Zn2+ with H3P03 and either Na+, K+, or Ba2+. The structures were determined by single-crystal X-ray diffraction techniques. Zn(H2PO3)2⋅3H2O; R3 a = 21.128 (2) Å, c = 7.769 (6) Å, V = 3003 (2) Å3, Z = 18, R(F) = 0.073 for 494 observations (I > 3σ(I)), 82 variables. Zn2(HPO3)2-(H2O)4⋅H2O: PĪ, a = 7.670 (2) Å, b = 9.454 (1) Å, c = 7.554 (1) Å, α = 90.83 (1)°, β = 92.90 (1)°, y = 88.54 (2)°, V= 546.9 (2) Å3, Z = 2, R(F) = 0.022 for 1430 observations ( I > 3σ(I)) 175 variables. Zn3Na2(HPO3)4: Pnma, a= 8.331 (2) Å, b = 12.243 (2) Å, c = 12.669 (1) Å, V = 1292.2 (6) Å3, Z = 4, R(F) = 0.038 for 704 observations (I > 3σ(I)), 103 variables. Zn3K2(HPO3)4: P21/c,a = 12.373 (2) Å, b = 13.635 (2) Å, c = 8.571 (2) Å, β = 90.24 (1)°, V= 1445.9 (4) Å3, Z = 4, R(F) = 0.037 for 1525 observations ( I > 3σ(I)), 206 variables. Zn3Ba(HPO3)4(H2O)6: C2/c, a = 22.707 (2) Å, b = 5.302 (3) Å, c = 15.029 (1) Å, β = 105.28 (1)°, V= 1745 (1) Å3, Z = 4, R(F) = 0.054 for 1530 observations (I> 3σ(I))t141 variables. Each of the five structures is a new type with the Zn atoms in either octahedral or tetrahedral coordination bridged by phosphite groups to produce a framework of zinc and phosphorus-centered oxygen polyhedra. Several of the frameworks have open channels lined with phosphite H atoms or coordinated water molecules. In some cases, these polyhedra are bridged by alkali-metal or alkaline-earth-metal ions to produce different frameworks. The exact nature of each structure is highly dependent on the identity of the second metal as each adopts a different coordination environment. The coordination numbers of the Na+, K+, and Ba2+ ions are 6, 7, and 12, respectively. The role of the alkali and alkaline-earth metals in the structures is discussed, and the phosphite structures are compared with similar known phosphates.

AB - Several new zinc phosphites have been synthesized in aqueous solution by reactions of Zn2+ with H3P03 and either Na+, K+, or Ba2+. The structures were determined by single-crystal X-ray diffraction techniques. Zn(H2PO3)2⋅3H2O; R3 a = 21.128 (2) Å, c = 7.769 (6) Å, V = 3003 (2) Å3, Z = 18, R(F) = 0.073 for 494 observations (I > 3σ(I)), 82 variables. Zn2(HPO3)2-(H2O)4⋅H2O: PĪ, a = 7.670 (2) Å, b = 9.454 (1) Å, c = 7.554 (1) Å, α = 90.83 (1)°, β = 92.90 (1)°, y = 88.54 (2)°, V= 546.9 (2) Å3, Z = 2, R(F) = 0.022 for 1430 observations ( I > 3σ(I)) 175 variables. Zn3Na2(HPO3)4: Pnma, a= 8.331 (2) Å, b = 12.243 (2) Å, c = 12.669 (1) Å, V = 1292.2 (6) Å3, Z = 4, R(F) = 0.038 for 704 observations (I > 3σ(I)), 103 variables. Zn3K2(HPO3)4: P21/c,a = 12.373 (2) Å, b = 13.635 (2) Å, c = 8.571 (2) Å, β = 90.24 (1)°, V= 1445.9 (4) Å3, Z = 4, R(F) = 0.037 for 1525 observations ( I > 3σ(I)), 206 variables. Zn3Ba(HPO3)4(H2O)6: C2/c, a = 22.707 (2) Å, b = 5.302 (3) Å, c = 15.029 (1) Å, β = 105.28 (1)°, V= 1745 (1) Å3, Z = 4, R(F) = 0.054 for 1530 observations (I> 3σ(I))t141 variables. Each of the five structures is a new type with the Zn atoms in either octahedral or tetrahedral coordination bridged by phosphite groups to produce a framework of zinc and phosphorus-centered oxygen polyhedra. Several of the frameworks have open channels lined with phosphite H atoms or coordinated water molecules. In some cases, these polyhedra are bridged by alkali-metal or alkaline-earth-metal ions to produce different frameworks. The exact nature of each structure is highly dependent on the identity of the second metal as each adopts a different coordination environment. The coordination numbers of the Na+, K+, and Ba2+ ions are 6, 7, and 12, respectively. The role of the alkali and alkaline-earth metals in the structures is discussed, and the phosphite structures are compared with similar known phosphates.

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Synthesis and Characterization of a New Series of Zinc Phosphites

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