Preparation and Structure of Melemium Melem Perchlorate HC6N7(NH2)3ClO4·C6N7(NH2)3

A new perchlorate salt of melem (2,6,10‐triamino‐s‐heptazine, C₆N₇(NH₂)₃) was obtained from an aqueous solution of HClO₄ at lower concentration than the ones reported for the synthesis of melemium perchlorate monohydrate (HC₆N₇(NH₂)₃)ClO₄·H₂O. The new salt was identified as melemium melem perchlorate (HC₆N₇(NH₂)₃)ClO₄·C₆N₇(NH₂)₃ representing a melem adduct of water free melemium perchlorate. The crystal structure was solved by single‐crystal X‐ray methods ( , no. 2, Z = 2, a = 892.1(2), b = 992.7(2), c = 1201.5(2) pm, α = 112.30(3), β = 96.96(3), γ = 95.38(3)°, V = 965.8(4)·10⁶ pm³, 4340 data, 387 parameters, R1 = 0.039). Melemium melem perchlorate crystallizes in a layer‐like structure containing both protonated HC₆N₇(NH₂)₃ and non protonated C₆N₇(NH₂)₃ moieties in the coplanar layers as well as perchlorate ions between them, all of which being interconnected by hydrogen bonds. Vibrational spectroscopic investigations (FTIR and Raman) of the salt were conducted.     

Formation and Characterization of Melam,Melam Hydrate,and a Melam–Melem Adduct

Until recently, melam, [C₃N₃(NH₂)₂]₂NH, has been regarded as a short‐lived intermediate in the condensation process of melamine that is only detectable under special reaction conditions owing to its high reactivity. A new synthetic approach has allowed a closer look at the formation and condensation behavior of melam by using elevated ammonia pressure in autoclaves. Whereas the thermal treatment of dicyandiamide at 450 °C and 0.2 MPa ammonia yielded melam in large amounts, prolonged treatment under these conditions (9 days) led to the formation of a melam–melem adduct, thus enabling the first insight into the condensation process of melam into melem. The hydrothermal treatment of melam at 300 °C (24 h) yields melam hydrate, [C₃N₃(NH₂)₂]₂NH ? 2 H₂O (space group P2₁/c; a=676.84(2), b=1220.28(4), c=1394.24(4) pm; β=98.372(2)°; V=1139.28(6)×10⁶ pm³; Z=4), which crystallizes as a layered structure that is composed of almost‐planar melam molecules, thereby forming ellipsoidal rosette‐like motifs. The resulting voids are filled with four water molecules, thus forming a dense network of hydrogen bonds.     

[{Na(7‐Nitro‐5‐sulfonate‐naphthalene‐1,4‐dicarboxy‐acid (H2O)2}·H2O]n: A Water‐Soluble 2D Layer Polymeric Complex with Microporous Molecular Channels

The X‐ray crystallographic studies are reported for a water‐soluble sodium complex of organic acid, {[Na(NSNDC)(H₂O)₂]·H₂O}_n, (NSNDC = 7‐Nitro‐5‐sulfonate‐napthalene‐1,4‐dicarboxy‐acid). It contains layers of vertically oriented NNSDC‐anions sandwiching cations and water molecules. The rows of anions are linked in a direction by sodium ions and along b by hydrogen bonding, which have microporous channels (9.410 × 3.210Ų) along the crystallographic b‐axis. Considering the Na coordination environments, π‐π stacking interaction between aryl ring and hydrogen bonds, the title compound represents a stably 2D infinitely extended structure.     

N-(4-甲基苯甲酰氨基) N’-[5-(2-三氟甲基苯基)-2-呋喃甲酰硫脲的合成、晶体结构测定与生物活性测定

本文首次合成标题化合物N-(4-甲基苯甲酰氨基)-N’-[5-(2-三氟甲基苯基)-2-呋喃甲酰硫脲。化合物(C21H16F3N3O3S, Mr = 447.43)单晶经测定为单斜晶体,空间群为P -1。在晶体中,存在一些分子内和分子间的相互作用,分子间还有C—H···π 的相互作用,这可能导致晶体更稳定的原因。目标产物的结构经IR, H NMR和元素分析测定确证。初步生物活性测试表明,部分化合物对棉花枯萎病、黄瓜灰霉病、苹果轮纹病和棉花炭疽病有较好的选择性杀菌活性;部分目标化合物有较好的除草活性。     

Melamine–Melem Adduct Phases: Investigating the Thermal Condensation of Melamine

By studying the thermal condensation of melamine, we have identified three solid molecular adducts consisting of melamine C₃N₃(NH₂)₃ and melem C₆N₇(NH₂)₃ in differing molar ratios. We solved the crystal structure of 2 C₃N₃(NH₂)₃?C₆N₇(NH₂)₃ ( 1 ; C2/c; a=21.526(4), b=12.595(3), c=6.8483(14) Å; β=94.80(3)°; Z=4; V=1850.2(7) ų), C₃N₃(NH₂)₃?C₆N₇(NH₂)₃ ( 2 ; Pcca; a=7.3280(2), b=7.4842(2), c=24.9167(8) Å; Z=4; V=1366.54(7) ų), and C₃N₃(NH₂)₃?3 C₆N₇(NH₂)₃ ( 3 ; C2/c; a=14.370(3), b=25.809(5), c=8.1560(16) Å; β=94.62(3)°; Z=4; V=3015.0(10) ų) by using single‐crystal XRD. All syntheses were carried out in sealed glass ampoules starting from melamine. By variation of the reaction conditions in terms of temperature, pressure, and the presence of ammonia‐binding metals (europium) we gained a detailed insight into the occurrence of the three adduct phases during the thermal condensation process of melamine leading to melem. A rational bulk synthesis allowed us to realize adduct phases as well as phase separation into melamine and melem under equilibrium conditions. A solid‐state NMR spectroscopic investigation of adduct 1 was conducted.     

Zur Kenntnis der Kristallstruktur von Melem C6N7(NH2)3

On the Crystal Structure of Melem C₆N₇(NH₂)₃ Single crystals of melem ( 1 ) were grown from both DMSO‐solutions and the gas phase. The structure of melem ( 1 ) was solved by single‐crystal X‐ray diffraction (P2₁/c, Z = 4, a = 741.66(15), b = 862.28(17), c = 1335.9(3) pm, β = 99.91(3)° R1 = 0.037 for 1098 reflections). The structure determination by X‐ray powder diffraction, which has been previously conducted, is in agreement with our data. The increased quality of the structural information allows for a more detailed understanding of the hydrogen bonding network.     

Formation of a hydrogen-bonded heptazine framework by self-assembly of melem into a hexagonal channel structure

Self-assembly of melem C(6)N(7)(NH(2))(3) in hot aqueous solution leads to the formation of hydrogen-bonded, hexagonal rosettes of melem units surrounding infinite channels with a diameter of 8.9 ?. The channels are filled with strongly disordered water molecules, which are bound to the melem network through hydrogen bonds. Single-crystals of melem hydrate C(6)N(7)(NH(2))(3)?xH(2)O (x≈2.3) were obtained by hydrothermal treatment of melem at 200 °C and the crystal structure (R ?3c, a=2879.0(4), c=664.01(13) pm, V=4766.4(13)×10(6) pm(3), Z=18) was elucidated by single-crystal X-ray diffraction. With respect to the structural similarity to the well-known adduct between melamine and cyanuric acid, the composition of the obtained product was further analyzed by solid-state NMR spectroscopy. Hydrolysis of melem to cyameluric acid during syntheses at elevated temperatures could thus be ruled out. DTA/TG studies revealed that, during heating of melem hydrate, water molecules can be removed from the channels of the structure to a large extent. The solvent-free framework is stable up to 430 °C without transforming into the denser structure of anhydrous melem. Dehydrated melem hydrate was further characterized by solid-state NMR spectroscopy, powder X-ray diffraction, and sorption measurements to investigate structural changes induced by the removal of water from the channels. During dehydration, the hexagonal, layered arrangement of melem units is maintained whereas the formation of additional hydrogen bonds between melem entities requires the stacking mode of hexagonal layers to be altered. It is assumed that layers are shifted perpendicular to the direction of the channels, thereby making them inaccessible for guest molecules.     

Synthesis,Crystal Structure,Hydrogen Bonding,and Thermal Behavior of a Three‐Dimensional CuII‐benzene‐1,2,4,5‐tetracarboxylate Templated by 1,9‐Diaminononane

Triclinic single crystals of Cu₄(H₃N–(CH₂)₉–NH₃)(OH)₂[C₆H₂(COO)₄]₂ · 5H₂O were prepared in aqueous solution at 80 °C in the presence of 1,9‐diaminononane. Space group P$\bar{1}$ (no. 2) with a = 1057.5(2), b = 1166.0(2), c = 1576.7(2) pm, α = 106.080(10)°, β = 90.73(2)° and γ = 94.050(10)°. The four crystallographic independent Cu²⁺ ions are surrounded by five oxygen atoms each with Cu–O distances between 191.4(3) and 231.7(4) pm. The connection between the Cu²⁺ coordination polyhedra and the [C₆H₂(COO)₄]^4– anions yields three‐dimensional framework with negative excess charge and wide centrosymmetric channel‐like voids. These voids extend parallel to [001] with the diagonal of the nearly rectangular cross‐section of approximately 900 pm. The channels of the framework accommodate [H₃N–(CH₂)₉–NH₃]²⁺ cations and water molecules, which are not connected to Cu²⁺. The nonane‐1,9‐diammonium cations adopt a partial gauche conformation. Thermoanalytical measurements in air show a loss of water of crystallization starting at 90 °C and finishing at approx. 170 °C. The dehydrated compound is stable up to 260 °C followed by an exothermic decomposition yielding copper oxide.     

Synthesis and Crystal Structure of Two CuII‐benzene‐1,2,4,5‐tetracarboxylates with Three‐Dimensional Open Frameworks

Two new three‐dimensional frameworks with zeolite‐like channels were prepared in the presence of 1,6‐diaminohexane. Cu_1.5(H₃N–(CH₂)₆–NH₃)_0.5[C₆H₂(COO)₄] · 5H₂O ( 1 ) crystallizes in the triclinic space group P$\bar{1}$ with a = 772.56(7), b = 1110.36(7), c = 1111.98(8) pm, α = 98.720(7)°, β = 108.246(9)°, and γ = 95.559(7)°. Cu₂(H₃N–(CH₂)₆–NH₃)_0.5(OH)[C₆H₂(COO)₄] · 3H₂O ( 2 ) crystallizes in the monoclinic space group P2/c with a = 1159.34(11), b = 1059.44(7), c = 1582.2(2) pm, and β = 106.130(11)°. The Cu²⁺ coordination polyhedra are connected by [C₆H₂(COO)₄]^4– anions to yield three‐dimensional frameworks with wide centrosymmetric channel‐like voids. Complex 1 reveals voids extending along [100] with diagonals of 900 pm and 300 pm, whereas in complex 2 the diagonal of the nearly rectangular crossection of the channels extending parallel to [001] is 900 pm. The negative excess charges of the frameworks are compensated by [H₃N–(CH₂)₆–NH₃]²⁺ cations, which occupy the voids along with water molecules. The [H₃N–(CH₂)₆–NH₃]²⁺ cations are not connected to Cu²⁺ and have served as templates.     

2,5,8‐Trihydrazino‐s‐heptazine: A Precursor for Heptazine‐based Iminophosphoranes

The title compound  C₆N₇(NHNH₂)₃ ( 1 ) was obtained from melem C₆N₇(NH₂)₃ or melon [C₆N₇(NH₂)NH]_n and hydrazine by an autoclave synthesis. Upon treatment with a 10 % HCl solution it is transformed into the trihydrochloride  [C₆N₇(NHNH₃)₃]Cl₃ ( 2 ). Compounds 1 and 2 were analysed with ¹³C NMR, ¹⁵N NMR, FTIR and Raman spectroscopy. Furthermore, the single‐crystal X‐ray structure of the pentahydrate of 2 is reported (P\bar{1} , a = 674.96(3), b = 1214.17(6), c = 1272.15(6) pm, α = 66.288(2)°, β = 75.153(2)°, γ = 80.420(2)°, V = 920.30(8)·10⁶ pm³, Z = 2, T = 90(2) K). The thermal decomposition of 1 and 2 was investigated with TG/DTA. Reaction of 1 with NaNO₂/HCl yields triazido‐s‐heptazine, C₆N₇(N₃)₃ ( 3 ). Tris(tri‐n‐butylphosphinimino)‐s‐heptazine ( 4 ) was synthesised from 3 and characterised by means of ¹³C, ³¹P, ¹H NMR, FTIR and MALDI‐TOF spectroscopy. Similar to s‐heptazine derivative 3 , compounds 1 and 4 are precursors for graphitic carbon nitrides, which have attracted considerable attention recently, and to various potential applications, such as flame retardants and (photo) catalysis.     

Ionothermal Synthesis and Structural Characterization of a Novel Open Framework Zinc Diphosphonate with Carboxylate‐like Linker

A novel crystalline zinc diphosphonate, (CH₃NH₃ )₄Zn₂ (xbp)₂•H₂O , denoted as compound 1 , was ionothermally synthesized from tetraethyl‐p ‐xylylenebisphosphonate (Texbp) and Zn(OAc )₂ in a protic eutectic mixture with urea/methylamine hydrochloride. Its structure was determined by single‐crystal X‐ray diffraction data and had a special three‐dimensional open framework with rhombic channels. Compound 1 belongs to the monoclinic system (space group C2 /c ), with lattice parameters a =22.6876(19) Å, b =8.73 76(7) Å, c =8.1673(9) Å, β =108.146(2)°, V =1538.5(2) ų, Z =2. Its structure is totally different from the typical organic pillared structure, only two oxygens of the phosphonate group are coordinated with zinc atoms, and the third oxygen exists in the terminal form, which is similar to the popular dicarboxylate linkers in MOFs . The organic cations [CH₃NH₃ ]⁺ of the eutectic mixture played a structure‐directing role for constructing this framework and were confined in the pore channels to balance the negative charges resulting from the zinc phosphonate inorganic chains.     

Hydrogen‐bonded two‐ and three‐dimensional polymeric structures in the ammonium salts of 3,5‐dinitrobenzoic acid, 4‐nitrobenzoic acid and 2,4‐dichlorobenzoic acid

The structures of ammonium 3,5‐dinitrobenzoate, NH₄⁺·C₇H₃N₂O₆⁻, (I), ammonium 4‐nitrobenzoate dihydrate, NH₄⁺·C₇H₄NO₄⁻·2H₂O, (II), and ammonium 2,4‐dichlorobenzoate hemihydrate, NH₄⁺·C₇H₃Cl₂O₂⁻·0.5H₂O, (III), have been determined and their hydrogen‐bonded structures are described. All three salts form hydrogen‐bonded polymeric structures, viz. three‐dimensional in (I) and two‐dimensional in (II) and (III). With (I), a primary cation–anion cyclic association is formed [graph set R₄³(10)] through N—H...O hydrogen bonds, involving a carboxylate group with both O atoms contributing to the hydrogen bonds (denoted O,O′‐carboxylate) on one side and a carboxylate group with one O atom involved in two hydrogen bonds (denoted O‐carboxylate) on the other. Structure extension involves N—H...O hydrogen bonds to both carboxylate and nitro O‐atom acceptors. With structure (II), the primary inter‐species interactions and structure extension into layers lying parallel to (001) are through conjoined cyclic hydrogen‐bonding motifs, viz.R₄³(10) (one cation, an O,O′‐carboxylate group and two water molecules) and centrosymmetric R₄²(8) (two cations and two water molecules). The structure of (III) also has conjoined R₄³(10) and centrosymmetric R₄²(8) motifs in the layered structure but these differ in that the first motif involves one cation, an O,O′‐carboxylate group, an O‐carboxylate group and one water molecule, and the second motif involves two cations and two O‐carboxylate groups. The layers lie parallel to (100). The structures of salt hydrates (II) and (III), displaying two‐dimensional layered arrays through conjoined hydrogen‐bonded nets, provide further illustration of a previously indicated trend among ammonium salts of carboxylic acids, but the anhydrous three‐dimensional structure of (I) is inconsistent with that trend.     

Crystalline Structure of Mangiferin,a C‐Glycosyl‐Substituted 9H‐Xanthen‐9‐one Isolated from the Stem Bark of Mangifera indica

The crystalline structure of mangiferin (=2‐β‐D ‐glucopyranosyl‐1,3,6,7‐tetrahydroxy‐9H‐xanthen‐9‐one; 1 ), a biologically active xanthenone C‐glycoside, isolated from the stem bark of Mangifera indica (Anacardiaceae), was unambiguously determined by single‐crystal X‐ray diffraction (XRD). The crystal structure is summarized as follows: triclinic, P1, a=7.6575(5), b=11.2094(8), c=11.8749(8) Å, α=79.967(5), β=87.988(4), γ=72.164(4)°, V=955.3(1) ų, and Z=2. The structure also shows two molecules in the asymmetric unit cell and five crystallization H₂O molecules. The packing is stabilized by several intermolecular H‐bonds involving either the two symmetry‐independent mangiferin molecules 1a and 1b , or the H₂O ones.     

Preparation,Structure, and Second‐order Nonlinear Optical Properties of a Borate‐Carboxylic Acid Compound: NH4B[d‐(+)‐C4H4O5]2·H2O

The organic‐inorganic hybrid nonlinear optical (NLO) material NH₄B(d‐ (+)‐C₄H₄O₅)₂ · H₂O (NBC) was synthesized in a borate‐carboxylic acid system. Its structure was determined by single crystal X‐ray diffraction. It crystallizes in the orthorhombic system, space group Pna2₁ (No. 33), with cell parameters a = 11.484(6) Å, b = 5.354(3) Å, c = 21.079(12) Å, V = 1296.0(12), Z = 4. It exhibits a three‐dimensional pseudo tunnel structure consisting of fundamental building block [B(d‐ (+)‐C₄H₄O₅)₂]^– anions. The small cavities are occupied by the H₂O molecules and NH₄⁺ cations, which stabilize the whole structure by O–H ··· O and N–H ··· O hydrogen bonds. The powder X‐ray diffraction (PXRD) of the crystal was also recorded. Elemental analyses, FT‐IR and FT‐Raman spectra analyses, thermal analysis, and diffuse‐reflectance spectra for the compound are also presented, as are band structures and density of states calculation. Nonlinear optical measurements indicate that the material has second harmonic generation (SHG) properties and is phase‐matchable.     

Hydrogen bonding in polyamino‐polyalcohols: a monohydrated cocrystal of 1,3‐diamino‐5‐azaniumyl‐1,3,5‐trideoxy‐cis‐inositol iodide and 1,3,5‐triamino‐1,3,5‐trideoxy‐cis‐inositol

In the title monohydrated cocrystal, namely 1,3‐diamino‐5‐azaniumyl‐1,3,5‐trideoxy‐cis‐inositol iodide–1,3,5‐triamino‐1,3,5‐trideoxy‐cis‐inositol–water (1/1/1), C₆H₁₆N₃O₃⁺·I⁻·C₆H₁₅N₃O₃·H₂O, the neutral 1,3,5‐triamino‐1,3,5‐trideoxy‐cis‐inositol (taci) molecule and the monoprotonated 1,3‐diamino‐5‐azaniumyl‐1,3,5‐trideoxy‐cis‐inositol cation (Htaci⁺) both adopt a chair conformation, with the three O atoms in axial and the three N atoms in equatorial positions. The cation, but not the neutral taci unit, exhibits intramolecular O—H...O hydrogen bonding. The entire structure is stabilized by a complex three‐dimensional network of intermolecular hydrogen bonds. The neutral taci entities and the Htaci⁺ cations are each aligned into chains along [001]. In these chains, two O—H...N interactions generate a ten‐membered ring as the predominant structural motif. The rings consist of vicinal 2‐amino‐1‐hydroxyethylene units of neighbouring molecules, which are paired via centres of inversion. The chains are interconnected into undulating layers parallel to the ac plane, and the layers are further held together by O—H...N hydrogen bonds and additional interactions with the iodide counter‐anions and solvent water molecules.     

硫酰杯[4]芳烃与铜(II)双核配合物的合成与晶体结构

The X-ray crystallographic structure was reported for a dinuclear copper（Ⅱ） complex with a tetraanionic ligand of p-tert-butylsulfonylcalix[4]arene [Cu2L（CH3OH）6]·4CH3OH （H4L=p-tert-butylsuffonylcalix[4]arene）. The complex belongs to triclinic system, P1^-- space group, with a = 1.2303（3） nm, b = 1.2377（3） nm, c = 1.3110（3） nm, a =66.862（4）°, β= 67.206（4）°, γ=61.711（3）°, Z= 1, V= 1.5659（7） nm^3, Dc= 1.371 g/cm^3, F（000） = 682,μ（Mo Kα） = 0.883 mm^-1, R1 =0.0325, wR2=0.0870. In this complex, the calix[4]arene acts as a bis-tridentate chelating ligand with the 1,2-alternate conformation.     

K3[C3N3(COO)3]·2H2O – Crystal Structure of a New Alkali Derivative of the Multidentate Ligand Triazine Tricarboxylate

Potassium‐1,3,5‐triazine‐2,4,6‐tricarboxylate dihydrate K₃[C₃N₃(COO)₃] · 2H₂O was obtained by saponification of the respective ethyl ester in aqueous solution under mild conditions and subsequent crystallization at 4 °C. The crystal structure of the molecular salt was elucidated by single‐crystal X‐ray diffraction [P , a = 696.63(14), b = 1748.5(3), c = 1756.0(3) pm, α = 119.73(3), β = 91.96(3), γ = 93.84(3)°, V = 1847.6(6) · 10⁶ pm³, Z = 6, T = 200 K]. Perpendicular to [100] the triazine tricarboxylate and potassium ions are arranged in layers alternating with layers of crystal water molecules. Two thirds of the triazine tricarboxylate units form hexagonal channels being filled with the remaining triazine tricarboxylate molecules. K₃[C₃N₃(COO)₃] · 2H₂O was additionally investigated by means of FTIR spectroscopy, TG and DTA measurements.     

Adsorption behaviour of a CdII–triazole MOF for butan‐2‐one in a single‐crystal‐to‐single‐crystal (SCSC) fashion: the role of hydrogen bonding and C—H…π interactions

The adsorption behaviour of the Cd^II–MOF {[Cd(L)₂(ClO₄)₂]·H₂O ( 1 ), where L is 4‐amino‐3,5‐bis[3‐(pyridin‐4‐yl)phenyl]‐1,2,4‐triazole, for butan‐2‐one was investigated in a single‐crystal‐to‐single‐crystal (SCSC) fashion. A new host–guest system that encapsulated butan‐2‐one molecules, namely poly[[bis{μ₃‐4‐amino‐3,5‐bis[3‐(pyridin‐4‐yl)phenyl]‐1,2,4‐triazole}cadmium(II)] bis(perchlorate) butanone sesquisolvate], {[Cd(C₂₄H₁₈N₆)₂](ClO₄)₂·1.5C₄H₈O}_n, denoted C₄H₈O@Cd‐MOF ( 2 ), was obtained via an SCSC transformation. MOF 2 crystallizes in the tetragonal space group P4₃2₁2. The specific binding sites for butan‐2‐one in the host were determined by single‐crystal X‐ray diffraction studies. N—H…O and C—H…O hydrogen‐bonding interactions and C—H…π interactions between the framework, ClO₄^? anions and guest molecules co‐operatively bind 1.5 butan‐2‐one molecules within the channels. The adsorption behaviour was further evidenced by ¹H NMR, IR, TGA and powder X‐ray diffraction experiments, which are consistent with the single‐crystal X‐ray analysis. A ¹H NMR experiment demonstrates that the supramolecular interactions between the framework, ClO₄^? anions and guest molecules in MOF 2 lead to a high butan‐2‐one uptake in the channel.     

Chloro‐N′,N′‐dimethylformamidinium‐(dimethylcyanamid)trichloroberyllat, [Me2NC(Cl)NH2]+[BeCl3(NCNMe2)]−

Chloro‐N′,N′‐dimethylformamidinium‐(dimethylcyanamide)trichloroberyllate, [Me₂NC(Cl)NH₂]⁺[BeCl₃(NCNMe₂)]^? Chloro‐N′,N′‐dimethylformamidinium‐(dimethylcyanamide)trichloroberyllate, [Me₂NC(Cl)NH₂]⁺[BeCl₃(NCNMe₂)]^? was prepared from BeCl₂ with two equivalents of dimethylcyanamide in CH₂Cl₂ suspension. The compound was characterized by X‐ray crystallography and by IR spectroscopy. Space group , Z = 2, lattice dimensions at 193 K: a = 620.7(1), b = 744.9(2), c = 1520.3(3) pm, α = 96.87(2)°, β = 100.41(2)°, γ = 100.17(2)°, R₁ = 0.0443. Cations and anions form N–H…Cl hydrogen bridges along [010].     

具有三维交叉孔道的新型亚磷酸锌的合成与结构

本文报道了一种新型三维亚磷酸锌[HO(CH₂)₂NH₃]₂•[Zn₃(HPO₃)₄]的合成和晶体结构。在它的结构中，ZnO₄和HPO₃严格按照顶点连接的方式交替相连。骨架结构存在两个沿着不同方向无限延伸的由ZnO₄和HPO₃组成的四元环链，在[0 1 0]、[0 4 15]和[0 -4 15]三个方向形成了三个交叉8元环孔道，有机胺阳离子起着平衡电荷和稳定骨架的结构。它的晶体数据为：[HO(CH₂)₂NH₃]₂•[Zn₃(HPO₃)₄],M=640.21, 正交晶系, Fdd2空间群, a=2.8528, b=0.8426, c=1.6159nm, Z=8, V=3.884nm³, R₁=0.0219, wR₂=0.0544。