Hydrothermal synthesis, structural, Raman, and luminescence studies of Am[M(CN)2]3·3H2O and Nd[M(CN)2]3·3H2O (M=Ag, Au): Bimetallic coordination polymers containing both trans-plutonium and transition metal elements

The polymeric compounds consisting of the man-made element, americium, and gold and silver dicyanides were prepared under mild hydrothermal conditions at 120 °C. It was found that the americium ion and the transition metal ions are interconnected through cyanide bridging in the compounds. Given the similarities in the radii of americium and neodymium, crystals of the latter were also characterized for comparison purposes. The four compounds are isostructural and crystallize in the hexagonal space group, P6₃/mcm, with only slight differences in their unit cell parameters. Crystallographic data (MoKα, λ=0.71073 Å): Am[Ag(CN)₂]₃·3H₂O (1), a=6.7205(10) Å, c=18.577(3) Å, V=726.64(19), Z=2; Am[Au(CN)₂]₃·3H₂O (2),a=6.666(2) Å, c=18.342(3) Å, V=705.9(4), Z=2; Nd[Ag(CN)₂]₃·3H₂O (3), a=6.7042(4) Å, c=18.6199(14) Å, V=724.77(8), Z=2; and Nd[Au(CN)₂]₃·3H₂O (4), a=6.6573(13) Å, c=18.431(4) Å, V=707.2(2), Z=2. The coordination around the Am and/or Nd consists of six N-bound CN⁻ groups resulting in a trigonal prismatic arrangement. Three capping oxygen atoms of coordinated water molecules complete the tricapped trigonal prismatic coordination environment, providing a total coordination number of nine for the f-elements. Raman spectroscopy, which compliments the structural analyses, reveals that the four compounds display strong signals in the ν_CN stretching region. When compared with KAg(CN)₂ or KAu(CN)₂, the ν_CN stretching frequencies for these compounds blue-shift due to bridging of the dicyanometallate ions with the f-element ions. There is subsequent reduction in electron density at the cyanide center. Compared with the silver systems, the ν_CN frequency appears at higher energy in the gold dicyanide complexes. This shift is consistent with the structural data where the carbon-nitrogen bond distance is found to be shorter in the gold dicyanides.     

Hydrothermal syntheses and crystal structures of two CuI coordination polymers: [CuI(TATP)(CN)] n and [CuI(bpy)(SCN)] n (TATP = 1,4,8,9-tetranitrogen-trisphene, bpy = 2,2′-bipyridine)

Two new Cu^I coordination polymers, [Cu^I(TATP) (CN)] _n (1) and [Cu^I(bpy)(SCN)] _n (2) (TATP = 1,4,8,9-tetranitrogen-trisphene, bpy = 2,2′-bipyiridine), have been synthesized under hydrothermal conditions and structurally characterized by elemental analysis, IR, and X-ray crystallography. In 1 and 2, the metal centers are linked by bridging CN⁻/SCN⁻ to form one-dimensional chains in the crystals and are stabilized by interchain π–π stacking interaction.     

Three-dimensional five-connected coordination polymer [M2(C3H2O4)2(H2O)2(μ2-hmt)]n with 46 topologies (M=Zn, Cu; hmt=hexamethylenetetramine)

Two novel three-dimensional five-connected coordination polymers [M₂(C₃H₂O₄)₂(H₂O)₂(μ₂-hmt)]_n with 4⁴6⁶ topologies (M=Zn, Cu; hmt=hexamethylenetetramine) were synthesized and characterized by elemental analysis, crystal structure, IR, thermal gravimetric analyses. Both [Zn₂(C₃H₂O₄)₂(H₂O)₂(μ₂-hmt)]_n and [Cu₂(C₃H₂O₄)₂(H₂O)₂(μ₂-hmt)]_n all crystallize in the orthorhombic system, space group Imm2, and with Z=2. Metal ions have all octahedral geometry coordinated by four oxygen atoms from three malonates, one oxygen atom from a water molecule and one nitrogen atom of hmt ligand. Each malonate binds a metal ion with its two oxygen atoms in a chelating mode and connects to adjacent two metal ions with another two oxygen atoms to form an infinite wavy layer. The layers are bridged by μ₂-hmt molecules to form a three-dimensional framework with channels. The magnetic susceptibility data show there is a weak antiferromagnetic exchange interaction in the complex [Cu₂(C₃H₂O₄)₂(H₂O)₂(μ₂-hmt)]_n.     

新型笼状同多钒酸盐[Ni(1,10′-phen)3]2·[V2ⅣV8ⅤO26]的水热合成和晶体结构

尽管多金属氧酸盐(POMs)的研究已有180多年的历史, 但大量的POMs结构在最近几十年才被陆续解析出来[1～4].     

Hydrothermal synthesis and characterization of a new three-dimensional hybrid zinc phosphate [Zn2(HPO4)2(4,4′-bipy)]·3H2O with neutral porous framework

Employing 4,4′-bipyridine as a bridged ligand, a new three-dimensional (3-D) hybrid zinc phosphate [Zn₂(HPO₄)₂(4,4′-bipy)]·3H₂O has been prepared under hydrothermal conditions and characterized by single crystal X-ray diffraction. This compound crystallizes in the monoclinic space group C2/c, with cell parameters, , , , β=90.21(3)°, and Z=4. The connectivity of the ZnO₃N and HPO₄ tetrahedra results in a 2-D neutral layer that with interesting 4,8² net along the bc plane. Furthermore, the 4,4′-bipyridine molecule links the 4,8² net into a 3-D structure. The water molecules sit in the middle of the channels and interact with the framework via hydrogen bonds. The compound exhibits intense photoluminescence at room temperature.     

一种新型的一维杂化磷酸锌化合物(2,2′-bipy)2·Zn2(PO4H)(PO4H2)2的合成与结构表征

作为磷酸盐基空旷骨架(Open-framework)化合物的一个重要组成部分, 磷酸锌基空旷骨架化合物经过近10年的发展已经成为内涵丰富的一个族系[1～6]. 实验证明有机胺基团可以作为配体, 起到电荷平衡阳离子与磷酸锌构成骨架作用[1～6]. 我们认为, 有机胺和骨架上的部分锌原子键合方式与多金属氧酸盐中的配体-次级金属结构模型存在相似性. 因此, 将多金属氧酸盐的配体-次级金属模型向过渡金属磷酸盐领域进行"嫁接", 不仅存在着实验参考依据[3,4], 而且将会推动磷酸盐配位化学的发展. 与多面体构成的钼酸盐和钒酸盐相比较, 这种"嫁接"意味着以磷氧四面体为结构单元的过渡金属磷酸盐可能存在着新颖的拓扑结构. 我们选用2,2′-联吡啶作为螯合配体, 制备新颖的具有杂化磷酸锌骨架的化合物, 并通过刚性配体的空间效应在一定程度上限制磷酸锌聚合体的外延连接. 本文报道一种一维链状杂化磷酸盐(2,2′-bipy)2Zn2(PO4H)(PO4H2)2(以下简称FJ-10, FJ: Fujian Institute of Research on the Structure of Matter)的水热合成及单晶结构表征. 在磷酸锌体系中, FJ-10具有新颖的骨架拓扑结构和堆垛方式. 我们将对此类化合物的合成、结构与性质进行系列报道.     

氢键构筑的新颖微孔配位聚合物[Co2(Hisor)2·(4,4′-bpy)2(H2O)2]·4,4′-bpy的合成与结构

A novel microporous coordination polymer [Co2(Hisor)2(4,4′-bpy)2(H2O)2]·4,4′-bpy was synthesized by hydrothermal reaction and characterized by single crystal X-ray diffraction, elemental analysis and IR spectrum. The crystal belongs to the monoclinic system and space group is P2/n with a=1.040 6(3) nm, b=1.138 8(4) nm, c=1.854 7(6) nm, β=102.991(6)°, V= 2.141 6(12) nm3, Z=2, Dc=1.443 Mg/m3, Mr=930.62, μ=0.842 mm-1, F(000)=952, GOF= 1.072, R=0.065 4, wR=0.146 8[I>2σ(I)]. There are two crystallographically independent Co(Ⅱ) ions in the title complex. The Hisor2- and 4,4′-bpy link the metal ions into 2D grids with dimension of 0.522 3 nm×1.138 8 nm. There are O—H…O and N—H…O hydrogen bonds in the complex resulting in the formation of 3D network with 1D channels, in which are free 4,4′-bpy molecules.     

Hydrothermal synthesis and crystal structure of a novel three-dimensional mixed-valence iron coordination polymer [Fe2FeO2(IN)2(ox)] (IN=isonicotinate, OX=oxalate)

A novel three-dimensional (3D) mixed-valence iron coordination polymer [Fe₂^IIIFe^IIO₂(IN)₂(ox)] (IN=isonicotinate, OX=oxalate) (1) has been hydrothermally synthesized by using two different anionic ligands and characterized by elemental analysis, IR spectrum, electron spin resonance (ESR), X-ray photoelectron spectrum (XPS), thermogravimetric analysis (TGA) and single crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic, space group P2(1)/c with a=5.8774(7) Å, b=18.528(2) Å, c=7.7117(9) Å, V=817.69(17) Å³, Z=2, and R₁=0.0321 (wR₂=0.0777). The Fe(II) and Fe(III) centers in 1 both exhibit a distorted octahedral coordination geometry and are bridged by the IN and oxalate groups into a covalently bonded 3D metal–organic network. TGA showed that the 3D network possesses a good stability up to 291 °C.     

(2,2′-bipy)[In2(OH)2(H2O)](SO4)2: The first indium sulfate with a layer structure

The first indium sulfate coordination complex, (2,2′-bipy)[In₂(OH)₂(H₂O)](SO₄)₂ (2,2′-bipy=2,2′-bipyridyl) was hydrothermally synthesized and characterized by single-crystal X-ray diffraction (XRD), the powder XRD, elemental analysis, inductively coupled plasma (ICP) analysis, thermogravimetric analysis (TGA), IR spectroscopy and fluorescent spectroscopy. It is noteworthy that this compound exhibits a novel two-dimensional layer structure, which is built up from two distinct motifs, a butlerite-type chain and a single 4-ring (S4R) unit. The adjacent layers are stably packed together and extended into three-dimensional supramolecular arrays via π-π stacking interactions of the 2,2′-bipy ligands. Additionally, this compound shows strong fluorescent property at room temperature, which may be assigned to ligand-centered π*-π transitions.     

Synthesis and crystal structure of gallosilicate- and aluminogermanate tetrahydroborate sodalites Na8[GaSiO4]6(BH4)2 and Na8[AlGeO4]6(BH4)2

Tetrahydroborate enclathrated sodalites with gallosilicate and aluminogermanate host framework were synthesized under mild hydrothermal conditions and characterized by X-ray powder diffraction and IR spectroscopy. Crystal structures were refined in the space group P-43n from X-ray powder data using the Rietveld method. Na₈[GaSiO₄]₆(BH₄)₂: a=895.90(1) pm, V=0.71909(3)×10⁻⁶ nm³, R_P=0.074, R_B=0.022, Na₈[AlGeO₄]₆(BH₄)₂: a=905.89(2) pm, V=0.74340(6)×10⁻⁶ nm³, R_P=0.082, R_B=0.026. The tetrahedral framework T-atoms are completely ordered in each case and the boron atoms are located at the centre of the sodalite cages. The hydrogen atoms of the enclathrated anions were refined on x, x, x positions, restraining them to boron-hydrogen distances of 116.8 pm as found in NaBD₄.The IR-absorption spectra of the novel phases show the typical bands of the tetrahedral group as found in the spectrum of pure sodium boron hydride.The new sodalites are discussed as interesting -containing model compounds which could release pure hydrogen.     

Synthesis and characterization of two new open-framework zinc phosphites [M(C6N4H18)][Zn3(HPO3)4] (M=Ni, Co) with multi-directional intersecting 12-membered ring channels

Two new open-framework zinc phosphites, [M(C₆N₄H₁₈)][Zn₃(HPO₃)₄] (M=Ni, Co), have been prepared under hydrothermal conditions. Single-crystal X-ray diffraction analysis shows that [Ni(C₆N₄H₁₈)][Zn₃(HPO₃)₄] (1) and [Co(C₆N₄H₁₈)][Zn₃(HPO₃)₄] (2) are isostructural and both crystallize in the monoclinic space group C2/c with , , , β=109.83(3)°, Z=4, R₁=0.0408 (I>2σ(I)), and wR₂=0.1104 (all data) for 1, and , , , β=109.328(2)°, Z=4, R₁=0.0380 (I>2σ(I)), and wR₂=0.1093 (all data) for 2. The structures of 1 and 2 are built up from strictly alternating ZnO₄ tetrahedra and HPO₃ pseudo-pyramids linked through oxygen vertices to form the three-dimensional (3-D) open-frameworks with multi-directional intersecting 12-membered ring (12-MR) channels. The M(TETA) (M=Ni, Co) complexes self-assembled under hydrothermal system connect with the inorganic host via M-O-P linkages and interact with inorganic framework through weak H-bonds. The two compounds show intense photoluminescence upon photoexcitation at 235 nm.     

[Ni(C6N2H14)2][Zn4(H2O)(HPO3)5]: A new open-framework zinc phosphite with intersecting 8-, 12- and 16-ring channels

A new three-dimensional (3-D) zinc phosphite with Zn/P ratio of 4/5, [Ni(C₆N₂H₁₄)₂][Zn₄(H₂O)(HPO₃)₅] (1), has been prepared by using self-assembled nickel complexes as the structure-directing agents. Its structure is built up from strict alternation of ZnO₄ tetrahedra and HPO₃ pseudo-pyramids, resulting in an open framework with multi-directional intersecting 8-, 12- and 16-ring channels. The unique nickel complexes Ni(DACH)₂ (DACH=1,2-diaminocyclohexane) only involving the cis-DACH acting as ligands are self-assembled under hydrothermal conditions, and act as the structure-directing agents (SDAs) to direct the formation of compound 1. Nickel complexes reside in the channels in a manner that the hydrophobic ends of the cis-DACH molecules exclusively protrude into the 16-ring pores and the amino groups closely interact with the charged inorganic framework through weak H-bonds. The interesting arrangements of nickel complexes imply a feasible approach to the design and synthesis of extra-large pore materials.     

The first rubidium rare-earth(III) thiophosphates: Rb3M3[PS4]4 (M=Pr, Er)

The two non-isotypical rubidium rare-earth(III) thiophosphates Rb₃M₃[PS₄]₄ of praseodymium and erbium can easily be obtained by the stoichiometric reaction of the respective rare-earth metal, red phosphorus and sulfur with an excess of rubidium bromide (RbBr) as flux and rubidium source at 950°C for 14 days in evacuated silica tubes. The pale green platelet-shaped single crystals of Rb₃Pr₃[PS₄]₄ as well as the pink rods of Rb₃Er₃[PS₄]₄ are moisture sensitive. Rb₃Pr₃[PS₄]₄ crystallizes triclinically in the space group (, , , α=84.329(4)°, β=88.008(4)°, γ=80.704(4)°; Z=2), Rb₃Er₃[PS₄]₄ monoclinically in the space group P2₁/n (, , , β=95.601(6)°; Z=4). In both structures, there are three crystallographically different rare-earth cations present. (M1)³⁺ is eightfold coordinated in the shape of a square antiprism, (M2)³⁺ and (M3)³⁺ are both surrounded by eight sulfur atoms as bicapped trigonal prisms each with a coordination number of eight as well as for the praseodymium, but better described as CN=7+1 in the case of the erbium compound. These [MS₈]¹³⁻ polyhedra form a layer according to by sharing edges with the isolated [PS₄]³⁻ tetrahedra (d(P-S)=200-209 pm, ?(S-P-S)=102-116°). These layers are stacked with a repetition period of three in the case of the praseodymium compound, but of only two for the erbium analog. The rubidium cation (Rb1)⁺ is located in cavities of these layers and tenfold coordinated in the shape of a tetracapped trigonal antiprism. The also tenfold but more irregularly coordinated rubidium cations (Rb2)⁺ and (Rb3)⁺ reside between the layers.     

Hydrothermal syntheses and crystal structures of bimetallic cluster complexes [{Cd(phen)2}2V4O12]·5H2O and [Ni(phen)3]2[V4O12]·17.5H2O

The hydrothermal reactions of vanadium oxide starting materials with divalent transition metal cations in the presence of nitrogen donor chelating ligands yield the bimetallic cluster complexes with the formulae [{Cd(phen₂)₂V₄O₁₂]·5H₂O (1) and [Ni(phen)₃]₂[V₄O₁₂]·17.5H₂O (2). Crystal data: C₄₈H₅₂Cd₂N₈O₂₂V₄ (1), triclinic. a=10.3366(10), b=11.320(3), c=13.268(3) Å, =103.888(17)°, β=92.256(15)°, γ=107.444(14)°, Z=1; C₇₂H₁₃₁N₁₂Ni₂O_29.5V₄ (2), triclinic. a=12.305(3), b=13.172(6), c=15.133(4), =79.05(3)°, β=76.09(2)°, γ=74.66(3)°, Z=1. Data were collected on a Siemens P4 four-circle diffractometer at 293 K in the range 1.59° <θ<26.02° and 2.01°<θ<25.01° using the ω-scan technique, respectively. The structure of 1 consists of a [V₄O₁₂]⁴⁻ cluster covalently attached to two {Cd(phen)₂}²⁺ fragments, in which the [V₄O₁₂]⁴⁻ cluster adopts a chair-like configuration. In the structure of 2, the [V₄O₁₂]⁴⁻ cluster is isolated. And the complex formed a layer structure via hydrogen bonds between the [V₄O₁₂]⁴⁻ unit and crystallization water molecules.     

Two new hydrogen bond-supported supramolecular compounds assembly from arsenic vanadates and [M(H2O)6] cations (MCo, Ni)

Two new supramolecular compounds based on arsenic vanadates formulated as [H₂As₆V₁₅O₄₂(H₂O)][Co(H₂O)₆]₂·2H₂O (1) and [H₂As₆V₁₅O₄₂(H₂O)][Ni(H₂O)₆]₂·2H₂O (2) have been prepared by reacting V₂O₅, H₂C₂O₄·2H₂O, As₂O₃,·H₂SO₄, CoCl₂·6H₂O (NiSO₄·6H₂O) and enMe (enMe=1,2-diaminopropane) under mild hydrothermal conditions and characterized by elemental analyses, IR, ESR, XPS and single crystal X-ray diffraction analyses. Crystal structure analyses reveal that compounds 1 and 2 are isostructural and exhibit novel 2-D supramolecular layer structures constructed from arsenic-vanadium clusters and two different types of secondary building units (SBUs), respectively, the different SBUs are formed by joint of two adjacent [Co(H₂O)₆]²⁺ cations in compounds 1 and [Ni(H₂O)₆]²⁺ cations in 2, respectively.     

[Zn(H2PO4)4] clusters and ∞[Zn2(HPO4)3(H2PO4)2] layers in two new zinc phosphates templated by [H2(4-amino-2.2.6.6-tetramethylpiperidine)] cations

Two zinc phosphates (ZnPO), [H₂(N₂C₉H₂₀)]·[Zn(H₂PO₄)₄] (I) and [H₂(N₂C₉H₂₀)]₂·[Zn₂(HPO₄)₃(H₂PO₄)₂]·H₂O (II), are synthesized under hydrothermal conditions using 4-amino-2.2.6.6-tetramethylpiperidine as organic template. I crystallizes in space group with , , , α=92.57(1)°, β=89.76(1)°, γ=102.16(2)°, and Z=2. Its structure, refined to R=0.029 and R_w=0.076 for 4279 independent reflections, consists of [Zn(H₂PO₄)₄]²⁻ clusters held together through strong hydrogen bonds to form pseudo-layers between which the doubly protonated amine molecules are inserted. II is monoclinic, C2, with , , , β=103.72(5)°, and Z=4 (R=0.079, R_w=0.268, 2477 independent reflections). The structure of II consists of _∞[Zn₂(HPO₄)₃(H₂PO₄)₂]⁴⁻ inorganic (2D) layers built up from vertex-sharing [ZnO₄] and [(H₂/H)PO₄] tetrahedra. Organic cations and water molecules ensure the connection between these layers via hydrogen bonds. It is shown that numerous (1D), (2D), e.g., [H₂(N₂C₉H₂₀)]₂·[Zn₂(HPO₄)₃(H₂PO₄)₂]·H₂O, and (3D) (ZnPO) result from the condensation of the [Zn(H₂PO₄)₄]²⁻ clusters.     

Ligand-controlled assembly of Cd(II) coordination polymers based on mixed ligands of naphthalene-dicarboxylate and dipyrido[3,2-d:2′,3′-f]quinoxaline: From 0D+1D cocrystal, 2D rectangular network (4,4), to 3D PtS-type architecture

Three novel Cd(II) coordination polymers, namely, [Cd(Dpq)(1,8-NDC)(H₂O)₂][Cd(Dpq)(1,8-NDC)]·2H₂O (1), [Cd(Dpq)(1,4-NDC)(H₂O)] (2), and [Cd(Dpq)(2,6-NDC)] (3) have been obtained from hydrothermal reactions of cadmium(II) nitrate with the mixed ligands dipyrido [3,2-d:2′,3′-f]quinoxaline (Dpq) and three structurally related naphthalene-dicarboxylate ligands [1,8-naphthalene-dicarboxylic acid (1,8-H₂NDC), 1,4-naphthalene-dicarboxylic acid (1,4-H₂NDC), and 2,6-naphthalene-dicarboxylic acid (2,6-H₂NDC)]. Single-crystal X-ray diffraction analysis reveals that the three polymers exhibit novel structures due to different naphthalene-dicarboxylic acid. Compound 1 is a novel cocrystal of left- and right-handed helical chains and binuclear complexes and ultimately packed into a 3D supramolecular structure through hydrogen bonds and π-π stacking interactions. Compound 2 shows a 2D rectangular network (4,4) bridged by 1,4-NDC with two kinds of coordination modes and ultimately packed into a 3D supramolecular structure through inter-layer π-π stacking interactions. Compound 3 is a new 3D coordination polymer with distorted PtS-type network. In addition, the title compounds exhibit blue/green emission in solid state at room temperature.     

A second crystal form of [Ni(2,2′-bipyridine)(H2O)3(NO3)](NO3) featuring a different molecular orientation

The molecular structure of a second form of [Ni(2,2′-bipyridine)(H₂O)₃(NO₃)](NO₃) is reported. The previous report is for a blue monoclinic polymorph. The second form is orthorhombic and crystallises as green blocks with unit cell parameters a = 9.1201(12) Å, b = 14.444(2) Å, c = 21.805(4) Å, V = 2872.4(8) Å³, Z = 8. The complex was characterised by elemental analysis, infrared spectroscopy, UV-Vis spectroscopy, and thermogravimetry. The bipyridine acts as a bidentate ligand to Ni²⁺ and the octahedral coordination is completed by three water molecules and one monodentate nitrate ion. A second nitrate forms hydrogen bonds to the bound water molecules. The difference between the two forms in terms of the molecular geometry is described in relation to other similar compounds. The key difference between the two forms is the orientation of the two nitrate anions, and hence the hydrogen bonding present.     

Syntheses, structure and magnetic properties of pillared layered diphosphonates: M2(O3PC6H4PO3)(H2O)2 (M=Co, Ni)

This paper describes the hydrothermal syntheses of two isostructural metal bisphosphonates: M₂(O₃PC₆H₄PO₃)(H₂O)₂ [M=Co^II (1), Ni^II (2)]. Single-crystal structure determination of compound 1 revealed a pillared layered structure in which the phenyl groups connect the inorganic layers of cobalt phosphonate. Crystal data for 1: orthorhombic, space group Pnnm, a=19.306(5), b=4.8293(12), c=5.6390(14) Å, V=525.7(2) Å³, Z=2. Magnetic susceptibility data indicate that antiferromagnetic interactions are mediated in both cases.     

Syntheses and crystal structures of two new hydrated borates, Zn8[(BO3)3O2(OH)3] and Pb[B5O8(OH)]·1.5H2O

Two new hydrated borates, Zn₈[(BO₃)₃O₂(OH)₃] and Pb[B₅O₈(OH)]·1.5H₂O, have been prepared by hydrothermal reactions at 170 °C. Single-crystal X-ray structural analyses showed that Zn₈[(BO₃)₃O₂(OH)₃] crystallizes in a non-centrosymmetric space group R32 with a=8.006(2) Å, c=17.751(2) Å, Z=3 and Pb[B₅O₈(OH)]·1.5H₂O in a triclinic space group P1¯ with a=6.656(2) Å, b=6.714(2) Å, c=10.701(2) Å, α=99.07(2)°, β=93.67(2)°, γ=118.87(1)°, Z=2. Zn₈[(BO₃)₃O₂(OH)₃] represents a new structure type in which Zn-centered tetrahedra are connected via common vertices leading to helical ribbons _∞¹[Zn₈O₁₅(OH)₃]¹⁷⁻ that pack side by side and are further condensed through sharing oxygen atoms to form a three-dimensional _∞³[Zn₈O₁₁(OH)₃]⁹⁻ framework. The boron atoms are incorporated into the channels in the framework to complete the final structure. Pb[B₅O₈(OH)]·1.5H₂O is a layered compound containing double ring [B₅O₈(OH)]²⁻ building units that share exocyclic oxygen atoms to form a two-dimensional layer. Symmetry-center-related layers are stacked along the c-axis and held together by interlayer Pb²⁺ ions and water molecules via electrostatic and hydrogen bonding interactions. The IR spectra further confirmed the existence of both triangular BO₃ and OH groups in Zn₈[(BO₃)₃O₂(OH)₃], and BO₃, BO₄, OH groups as well as guest water molecules in Pb[B₅O₈(OH)]·1.5H₂O.