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1.
A novel mixed alkali metal hydrated borate NaCs[B10O14(OH)4] was synthesized under hydrothermal conditions. Its structure was determined by single-crystal X-ray diffraction and further characterized by FT-IR spectroscopy, TG-DTA, powder X-ray diffraction, and chemical analysis. NaCs[B10O14(OH)4] crystallizes in monoclinic space group P2/c with a = 7.6588(3) Å, b = 9.0074(3) Å, c = 11.8708(6) Å, and β = 115.682(3)°. The crystal structure of NaCs[B10O14(OH)4] consists of Na–O, Cs–O polyhedral, and [B10O14(OH)4]2? polyborate anions. [B10O14(OH)4]2? units are connected together through common oxygen atoms forming a 1D helical chain-like structure, which are further connected by O–H···O hydrogen bonds forming a 3D supramolecular structure. Through a designed thermochemical cycle, the standard molar enthalpy of formation of this borate was determined to be ?7888.6 ± 8.1 kJ mol?1 by using a heat conduction microcalorimeter.  相似文献   

2.
Two new pentaborates [M(dap)3][B5O6(OH)4]2·H2O (M = Co (1) and Ni (2); dap = 1,2-diaminopropane) have been hydrothermally synthesized. Both structures were determined by single crystal X-ray diffraction and further characterized by elemental analysis, FT-IR, thermogravimetric analysis and photoluminescence spectroscopy. Two compounds are isostructural and consist of isolated pentaborate [B5O6(OH)4]? anions and [M(dap)3]2+ complex cations. The anionic [B5O6(OH)4]? groups are linked by extensive hydrogen bonds to form a 3-D supramolecular framework with large channels, in which the transition-metal complex templates are located. The luminescent properties of 1 and 2 were studied, and blue luminescence occurs with an emission maximum at 405 and 408 nm upon excitation at 332 and 328 nm respectively. Crystal data: 1, monoclinic, space group P21/c (No. 14), a = 9.7159(5) Å, b = 29.3372(19) Å, c = 11.5121(6) Å, β = 103.286(5)°, V = 3193.6(3) Å3, Z = 4; 2, monoclinic, space group P21/c, a = 9.7264(4) Å, b = 29.3810(16) Å, c = 11.5185(6) Å, β = 103.249(4)°, V = 3204.0(3) Å3, Z = 4.  相似文献   

3.
Synthetic methods are reported for the preparation of compounds containing the trinuclear triangular cluster [W3S4Br3(depe)3[+. These involve reactions between WBr5 and NaB(C2 H5)3H or NaBH4 as reducing agent in THF, and subsequent addition of methanolic solutions of NaHS and depe ligand. Both compounds, [W3S3Br3(depe)3]PF6·0.5C7H8,1, and [W3S4Br3(depe)3]Br·2CH3OH,2, are characterized by x-ray single crystal studies. Compounds1 and2 crystallize in space group \(P\bar 1\) . For1,a=10.427 (3) Å,b=15.415(4) Å,c=18.140(5) Å, α=79.36(2)°, β=73.59(2)°, γ=81.54(2)°, andV=2734.8(2) Å3;R=0.050 and for 2a=10.491(3) Å,b=15.074(3) Å,c=18.246 Å, α=95.76(2)°, β=105.82(2)°, γ=98.18(2)°, andV=2718.4(3) Å3;R=0.081. The two cations in1 and2 possess C3 symmetry. The W-W distances are in the range 2.783?2.891 Å (for1) and 2.778?2.785 Å (for2) and the average W-Br distances in1 and2 are 2.616[2] Å and 2.594[4] Å, respectively. Each metal atom in the [W3S4Br3(depe)3]+ ions is attached to one capping sulfur atom, two bridging sulfur atoms, one bromine atom, and one chelating depe ligand. One P atom in depe ligand istrans to μ3-S and the otherP atom istrans to a μ2-S atom. UV-Vis and NMR spectra for these compounds are also reported.  相似文献   

4.
Tetraamminecobalt hydrogen hexamolybdoferrate [Co(NH3)4] · H[FeMo6O18(OH)6] · 6H2O (I) and tetraamminecobalt hydrogen hexamolybdogallate(III) [Co(NH3)4] · H[GaMo6O18(OH)6] · 6H2O (II) were synthesized and studied by mass spectrometry, thermogravimetry, IR spectroscopy, and X-ray diffraction. Crystals of I and II are monoclinic; a = 16.21 Å, b = 5.43 Å, c = 12.32 Å, β = 119.63°, V = 1092.11 Å3, ρcalcd = 2.21 g/cm3, and Z = 1 for I; a = 16.24 Å, b = 5.59 Å, c = 12.29 Å, β = 119.79°, V = 1064.05 Å3, ρcalcd = 2.15 g/cm3, and Z = 1 for II. Compounds I and II were used as catalysts for soft oxidation of natural gas.  相似文献   

5.
Hydrogen hexamolybdogallate and hexamolybdoaluminate with the hexamminecadmium cation [Cd(NH3)6] · H[GaMo6O18(OH)6] · 6H2O (I) and [Cd(NH3)6] · H[AlMo6O18(OH)6] · 6H2O (II) were synthesized and studied by mass spectrometry, thermogravimetric analysis, powder X-ray diffraction, and IR spectroscopy. The crystals are monoclinic; I: a = 10.82 Å, b = 3.69 Å, c = 11.99 Å, β = 91.06°, V= 469.72 Å3, ρcalcd = 2.34 g/cm3, Z = 2; II: a = 10.81 Å, b = 3.67 Å, c =11.98 Å, β = 91.08°, V = 469.78 Å3, ρcalcd = 2.38 g/cm3, Z = 2.  相似文献   

6.
Two new borate clusters, [NH3(CH2)3NH3]2[B14O20(OH)6] (1) and [NH3(CH2)6NH3]2[B14O20(OH)6] (2), have been made under solvothermal conditions and characterized by single-crystal X-ray structural analysis. Also their IR and UV–Vis spectroscopy, thermogravimetric analysis, and elemental analysis have been investigated, respectively. Crystal data for 1: triclinic, P-1, a = 8.8049(4) Å, b = 9.1585(5) Å, c = 10.1912(5) Å, α = 74.925(4)°, β = 80.987(4)°, γ = 67.495(5)°, Z = 1. Crystal data for 2: triclinic, P-1, a = 9.2010(4) Å, b = 9.8663(4) Å, c = 11.4191(4) Å, α = 107.014(4)°, β = 92.514(3)°, γ = 107.265(4)°, Z = 1. The structures consist of isolated 8-membered boron ring made of the [B7O10(OH)3]2?cluster subunits. UV–Vis spectral investigation indicates that they are wide-band-gap semiconductors. Fluorescence spectroscopy indicates that they are potential blue light materials.  相似文献   

7.
Two strontium borates Sr2[B6O9(OH)4] (1) and Sr2B5O9(OH)·H2O (2), with acentric structures have been synthesized under hydro/solvothermal conditions. Compound 1 is reported for the first time in the strontium borates system, and it crystallizes in the monoclinic space group P21 with unit cell parameters a = 6.8445(5) Å, b = 8.7033(6) Å, c = 8.4632(6) Å, β = 100.581(6)°, V = 495.58(6) Å3 and Z = 2. Its structure consists of unusual borate layers of 3, 11-membered rings, which are interconnected via Sr–O ionic bonds and hydrogen bonds to generate a 3D supramolecular network. Compound 2 is a known strontium borate, crystallizing in the monoclinic space group C 2 with a = 10.161 (13) Å, b = 7.965(4) Å, c = 6.393(11) Å, β = 128.0(2)°, V = 407.7(14) Å3 and Z = 2. Second-harmonic generation measurements on the powder samples reveal that 1 and 2 exhibits good SHG efficiency about 1.5 and 2 times that of KDP (KH2PO4) powder respectively.  相似文献   

8.
利用水热法合成了两种过渡金属配合物为模板剂的含水硼酸盐晶体Co(en)3[B4O5(OH)4]Cl·3H2O(1) 和 [Ni(en)3][B5O6(OH)4]2·2H2O (2),并通过元素分析、X射线单晶衍射、红外光谱及热重分析对其进行了表征。化合物1晶体结构的主要特点是在所有组成Co(en)33+, [B4O5(OH)4]2–, Cl– 和 H2O之间通过O–H…O、O–H…Cl、N–H…Cl和N–H…O四种氢键连接形成网状超分子结构。化合物2晶体结构的特点是[B5O6(OH)4]–阴离子通过O–H…O氢键连接形成沿a方向有较大通道的三维超分子骨架,模板剂[Ni(en)3]2+阳离子和结晶水分子填充在通道中。  相似文献   

9.
A new mixed-metal polyborate, Na5Li[B12O18(OH)6]·2H2O (1), has been synthesized using solvothermal method and characterized by IR spectroscopy, thermogravimetric analysis, UV–Vis spectroscopy, powder and single-crystal X-ray diffraction, respectively. It crystallizes in the trigonal space group R-3c (No. 167) with unit cell parameters of a = b = 9.6767(6) Å, c = 36.358(5) Å, and Z = 6. Its structure features unprecedented 3D framework constructed from novel honeycomb-shaped inorganic Na-O sheets with unique 12-MR sodium rings and supramolecular polyborate 2D layers of lithium-centered [B12O18(OH)6]6-. UV–Vis spectral characterization indicates that compound 1 is a wide-band-gap semiconductor.  相似文献   

10.
Polycrystalline thorium(IV) phosphate-triphosphate, Th2(PO4)(P3O10) (1), was obtained by (NH4)2Th(PO4)2·H2O (2) heating from room temperature to 1,273 K. 1 crystallizes in the orthorhombic space group Pn21 a (a = 11.6846(2) Å, b = 7.1746(1) Å, c = 12.9320(3) Å, Z = 4). Combining powder synchrotron X-ray diffraction data and DFT geometry optimization, a structural model is proposed for 1. The structure is built on ThO8 polyhedral chains along the b-axis. PO4 3? and P3O10 5? groups coexist in the structure and the latter group forms non-linear chains. Cohesion of the structure is made by the linkage of ThO8 chains by PO4 and P3O10 groups. Thermal transformation from 2 to 1 was monitored by thermogravimetric analysis (activation energy as a function of the extent of conversion was obtained from Kissinger–Akahira–Sunose (KAS) isoconversional method) and powder X-ray thermo-diffraction. For 2, the dehydration process takes place in two steps, with the apparition of a layered intermediate phase, (NH4)2Th(PO4)2·nH2O (0 < n < 1, d = 6.42 Å), previously to the formation of (NH4)2Th(PO4)2 (d = 6.31 Å). The condensation process produces an amorphous material that crystallizes to α-ThP2O7 (3) when the temperature increases. At 1,273 K, 3 slowly transforms to 1.  相似文献   

11.
Tetramminenickel hydrogen hexamolybdoaluminate and hexamolybdogallate(III) of compositions [Ni(NH3)4] · H[AlMo6O18(OH)6] · 10H2O (I) and [Ni(NH3)4] · H[GaMo6O18(OH)6] · 10H2O (II) were synthesized and characterized by mass spectrometry, thermogravimetry, X-ray powder diffraction, and IR spectroscopy. Their crystals are triclinic. For compound I, a= 17.30 Å, b= 14.69 Å, c= 10.45 Å, α = 129.07, β = 65.91°, γ = 138.01°, V = 1338.7l Å3, ρcalcd = 2.75g/cm3, Z = 2; for compound II, a = 17.38 Å, b= 14.75 Å, c= 10.51 Å, α = 131.38°, β= 65.96°, γ = 138.09, V = 1338.15 Å3, ρcalcd = 2.68 g/cm3, Z = 2.  相似文献   

12.
[Co(NH3)6] · H2[NiMo6O18(OH)6] · 6H2O (I) and [Co(NH3)6] · H2[ZnMo6O18(OH)6] · 6H2O (II) have been synthesized and studied by mass spectroscopy, thermogravimetry, and X-ray powder diffraction. The crystals of compounds I and II are monoclinic, Z = 1; for compound I: a = 16.10 Å, b = 5.58 Å, c = 12.22 Å, β = 117.86°, V = 1045.14 Å3, and ρcalcd = 2.26 g/cm3; for compound II: a = 16.12 Å, b = 5.52 Å, c = 12.12 Å, β = 117.90°, V = 1043.21 Å3, and ρcalcd = 2.21 g/cm3.  相似文献   

13.
A new Keggin polyoxometalate-based polymer, formulated as (Hppy)2Cu2(ppy)4[SiMo12O40] (1) ppy = 4-(5-phenylpyridin-2-yl)pyridine, had been synthesized under hydrothermal conditions. Complex 1 exhibits a one-dimensional polyoxometalate-based chain constructed from Keggin anions of [SiMo12O40]4? weakly connected by dinuclear [Cu(ppy)2] groups. This complex crystallizes in the triclinic space group P-1, a = 12.621(3) Å, b = 13.168(3) Å, c = 17.467(4) Å, α = 86.09(3)°, β = 85.35(3)°, γ = 64.10(3)°, = 2601.1(9) Å3, Z = 1. The elemental analyses, FT-IR, TG-DTA for this compound were also determined.  相似文献   

14.
Hydrothermal reactions of trilacunary precursor A-α-AsW9O34 9? polyoxoanions and nickel ions in the presence of ethylenediamine (en = ethylenediamine) led to two new hexa-Ni-substituted Keggin-type tungstoarsenates [Ni6(μ 3-OH)3(en)3(H2O)6(B-α-AsW9O34)]·6H2O (1) and [Ni6(μ 3-OH)3(en)3(H2O)6(B-α-AsW9O34)]·10H2O (2), which have been characterized by elemental analyses, IR spectra, powder X-ray diffraction, thermogravimetric analyses and single-crystal X-ray diffraction. Crystal data for 1: hexagonal, R3c, a = b = 20.4379(5) Å, c = 21.5062(6) Å, β = 120º, V = 7779.8 (3) Å3 and Z = 6; for 2: momoclinic, P21/c, a = 13.4200(3) Å, b = 19.1428(5) Å, c = 22.8845(9) Å, β = 112.403(3)º, V = 5435.2(3) Å3 and Z = 4. Structural analyses reveal that the [Ni6(μ 3-OH)3(B-α-AsW9O34)] clusters in 1 and 2 are covalently functionalized by neutral en ligands, in which two similar {Ni6(μ 3-OH)3(en)3(H2O)6}9+ cores have been observed by our lab. Notably, 1 and 2 represent the highest number of substituted transition metal ions in all known lacunary Keggin-type polyoxotungstoarsenate monomers.  相似文献   

15.
The solid-state structures of two non-metal pentaborates [Me3NCH2CH2OH][B5O6(OH)4] (1) and [4-MepyH, 4-Mepy][B5O6(OH)4] (2) have been determined by single-crystal X-ray diffraction methods. Structures 1 and 2 both contain supramolecular pentaborate frameworks held together by extensive H-bond interactions. The framework of 1 exists essentially as planes of pentaborate anions linked via three pairwise ‘planar’ β → α interactions, with a fourth β → β interaction crosslinking the planes. The framework of 2 is very similar except that one of the three pairwise linkages within the plane is replaced by pairwise ‘step-like’ bifurcated H-bonds to both α sites of a neighboring anion. The cations in 1 and the cations and neutral 4-Mepy ligands in 2 are present in the framework cavities and channels, with additional H-bond interactions existing between cations and anions.  相似文献   

16.
The cage-like cyclobutyltellurium(IV)-containing tungstoarsenate(III) dimers [(C4H8Te-OH)2(C4H8Te)6{As2W17O61(H2O)}2]14? (1) and [{(C4H8Te)2W2O5(H2O)2As2W19O67(H2O)}2]16? (2) were synthesized in moderately acidic aqueous medium by reaction of C4H8TeI2 with the lacunary tungstoarsenates(III) [B-α-AsW9O33]9? and [As2W19O67(H2O)]14?, respectively. Polyanion 1 was isolated as a mixed cesium-guanidinium salt Cs8.5(C(NH2)3)5.5[(C4H8TeOH)2(C4H8Te)6{As2W17O61(H2O)}2]·60H2O (1a), whereas 2 crystallized as a mixed cesium-potassium salt Cs9K7[{(C4H8Te)2W2O5(H2O)2As2W19O67(H2O)}2]·90H2O (2a). Single crystal X-ray analysis demonstrated that 1a and 2a crystallized in the triclinic space group \( P \bar{1} \), with a = 12.7738(8) Å, b = 18.7490(14) Å, c = 21.9831(14) Å, α = 111.155(4)o, β = 93.312(3)o, γ = 99.530(4) and Z = 1 for 1a and a = 19.309(6) Å, b = 24.674(8) Å, c = 26.071(8) Å, α = 63.218(17)°, β = 89.26(16)°, γ = 79.948(17)° and Z = 2 for 2a. The polyanion salts 1a and 2a were characterized by solid state NMR (1H, 13C, 125Te), FT-IR, TGA-DSC, and elemental analysis.  相似文献   

17.
Hexaamminecadmium hydrogen hexamolybdocobaltate(III) and hydrogen hexamolybdochromate(III) of compositions [Cd(NH3)6] · H[CoMo6O18(OH)6] · 6H2O (I) and [Cd(NH3)6] · H[CrMo6O18(OH)6] · 6H2O (II), respectively, were synthesized and studied by mass spectroscopy, thermo-gravimetry, X-ray powder diffraction, and IR spectroscopy. Crystals of I and II are monoclinic. For I: a = 10.79 Å, b = 3.70 Å, c = 11.95 Å, β = 91.05°, V = 470.12 Å3, ρcalc = 2.37 g/cm3, Z = 2; and for II: a = 10.80 Å, b = 3.68 Å, c = 11.97 Å, β = 91.07°, V = 468.98 Å3, ρcalc = 2.36 g/cm3, Z = 2.  相似文献   

18.
Two new coordination polymers, [Pb(IDPT)2(NO3)2] (I) and [Mn(IDPT)(SO4)(H2O)2] (II) (IDPT = imidazo[4,5-f][1,10]phenanthroline), were synthesized by hydrothermal method and characterized by elemental analysis and single-crystal X-ray diffraction technique. The results reveal that the complex I belongs to monoclinic crystal system, space group C2/c and complex II belongs to monoclinic crystal system, P21/c space group. The cell parameters are: a = 19.1970(13), b = 7.3875(5), c = 17.3825(12) Å, β = 100.47(10)°, V = 2424.0(3) Å3, Z = 4, F(000) = 1488 for I; a = 10.9135(6), b = 7.0230(4), c = 19.7034(10) Å, β = 99.32(10)°, V = 1490.25(14) Å3, Z = 4, F(000) = 828 for II. In the structure of complex I, the metal center Pb(II) is six-coordinated, displays an octahedral geometry. Each molecule is further connected with neighboring one via π-π interactions into 1D chain. In complex II, Mn(II) is six-coordinated to form a distorted octahedral geometry. Compound II displays 1D supramolecular chain formed through hydrogen bonds. Additionally, the fluorescent properties for the complexes were investigated. Complexes I and II exhibit strong photoluminescence with emission maximum at 583 and 529 nm at room temperature.  相似文献   

19.
Complexes RbL (I) and [Li2(C2H5OH)L2] (II) (L = C23H15O3) have been synthesized and their crystal structures have been studied. Both compounds have monoclinic crystals with space group P21/c and Z = 4; I: a = 11.632(2) Å, b = 15.154(3) Å, c = 11.457(2) Å, β = 104.34(3)°; II: a = 12.982(3)Å, b = 12.083(2) Å, c = 25.317(5) Å β = 100.11(3)°. In the structure of I, dimeric groups [Rb2O6] with a shared edge are linked by the ligands to give infinite layers perpendicular to the x axis and cavities that form oblong channels. In the structure of II, Li2O7 dimers are formed by vertex sharing. The coordination of one of the lithium atoms (Li(1)) is completed to tetrahedral by the oxygen atom of the ethanol molecule. The structure of II, like that of I, is layered.  相似文献   

20.
Ping Li  Zhihong Liu 《中国化学》2012,30(4):847-853
A new hydrated lithium borate, Li4[B8O13(OH)2]·3H2O, has been hydrothermally synthesized and characterized by single crystal X‐ray diffraction, FT‐IR spectroscopy, simultaneous TGA‐DTA and chemical analysis. It crystallizes in the triclinic, space group , a=8.4578(5) Å, b=8.7877(5) Å, c=10.8058(7) Å, α=87.740(3)°, β=71.819(3)°, γ=61.569(3)°, Z=2, V=665.26(7) Å3, Dc=2.043 g/cm3. Its crystal structure features polyborate anionic layers with the larger odd 13‐membered boron rings constructed by [B8O13(OH)2]4? FBBs. Through designing the thermochemical cycle, the standard molar enthalpy of formation of this borate was determined to be ?(7953.8±6.6) kJ·mol?1 by using a heat conduction microcalorimeter.  相似文献   

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