首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献,搜索用时 31 毫秒
1.
Two novel borates [(CH3)3NH][B5O6(OH)4] (I) and Na2[H2TMED][B7O9(OH)5]2 (II) have been synthesized under solvothermal conditions, and characterized by elemental analyses, FT-IR spectroscopy, and single crystal X-ray diffraction. Crystal data for I: monoclinic, P21/c, a = 9.3693(11) Å, b = 14.0375(17) Å, c = 10.0495(9) Å, β = 91.815(9)°, Z = 4. Crystal data for II: monoclinic, P21/c, a = 11.6329(2) Å, b = 11.9246(3) Å, c = 10.2528(2) Å, β = 100.178(2)°, Z = 4. Their crystal structures both have 3D supramolecular framework with large channels constructed by O–H···O hydrogen-bonding among the polyanions of [B5O6(OH)4]? or [B7O9(OH)5]2? clusters. The templating organic amines cations in I and II are both located in the channels of 3D supramolecular frameworks, respectively, and interact with the polyborate frameworks both electrostatically and via hydrogen bonds of N–H···O. Na2[H2TMED][B7O9(OH)5]2 is the first example of heptaborate co-templated by alkali metal and organic base, which is also rare in borates. The photoluminescence property of the synthetic sample of Na2[H2TMED][B7O9(OH)5]2 in the solid state at room temperature was also investigated by fluorescence spectrophotometer.  相似文献   

2.
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   

3.
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   

4.
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   

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.
New hydrated potassium hexaborate K2[B6O9(OH)2] has been synthesized under mild solvothermal conditions. The structure was determined by single-crystal X-ray diffraction and further characterized by FT-IR, Rarnan spectra and DTA-TG. It crystallizes in the monoclinic system with space group P21/n, a=0.9036(2) nm, b=0.66052(18) nm, c=1.5997(4) nm, β=91.862(4)°, V=0.9543(4) nm^3 and Z=4. Its crystal structure consists of K-O polyhedra and 1-D stepped polyborate chains constructed by new [B6O9(OH)2]2- fundamental building blocks. 1-D polyborate chains contain 3,8-membered boron rings. Adjacent chains are further linked via H-bonding interactions into 2-D layers. The K^+ cations reside not only between the layers but also in the 8-membered boron rings of the chains, compensating the negative charges of the borate chains and holding the layers together into the 3-D structure through bonding with oxygen atoms of the chains.  相似文献   

7.
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   

8.
Four Fe(II/III) supramolecules, {[Fe(Hpdc)2(H2O)2]·2H2O} (1), [Fe(HImbc)2(H2O)2] (2), [Fe(phen)2(CN)2]·CH3CH2OH·2H2O (3), K[Fe(tp)2]·SO4 (4) (H2pdc = 2,5-Pyridinedicarboxylic acid, H2Imbc = 4,5-Imidazoledicarboxylic acid, phen = 1,10-phenanthroline, tp = poly(pyrazolyl)borate), were synthesized by hydrothermal and room temperature stirring methods. They were characterized by single crystal X-ray diffraction, surface photovoltage spectroscopy (SPS), field-induced surface photovoltage spectroscopy (FISPS), electron paramagnetic resonance (EPR), UV–Vis absorption spectra (UV–Vis), infrared spectra (IR) and element analysis. The structural analyses indicate that complex (1) is a supramolecule with 2D structure connected by hydrogen bonds. Complex (2) is a supramolecule with hydrogen-bonded 3D structure. Complexes (3) and (4) are both 1D supramolecules connected by hydrogen bonds. The electronic state of central metal Fe(II) ions in complexes (1) and (2) is d6 with FeN2O4 coordination mode, lying in weaker distorted octahedral field. The electronic state of Fe(II) ion in complex (3) is d6 with Fe(CN)2N4 mode in the strong distorted octahedral field. The electronic state of Fe(III) ion in complex (4) is d5 with FeN6 mode, lying in the strong octahedral field. The micro-environment of Fe(II/III) ions in the four complexes is further investigated by EPR. The SPS of four complexes all exhibit photovoltage responses in the range of 300–700 nm. This indicates that they all possess certain photoelectric conversion capability. The effects of component, structure, type of ligands of the complexes, valence state and coordination micro-environment of the central metal ions on the SPS were discussed. Furthermore, the SPS and UV–Vis absorption spectra were interrelated.  相似文献   

9.
《Solid State Sciences》2012,14(10):1512-1519
The asymmetrically substituted heterocyclic alkyne 5-(pyridin-3-ylethynyl) picolinate (P3PA) was synthesized via a one-pot Sonogashira coupling. After purification, P3PA was reacted with Pb(NO3)2 into the two-dimensional coordination polymer Pb(P3PA)2(H2O)2 (1) under hydrothermal conditions. Coordination polymer 1 crystallizes into the monoclinic space group I2/a, with a = 15.5775(10) Å, b = 5.9949(4) Å, c = 24.8380(16) Å, and β = 90.7500(10)°. In addition, the luminescent fluorene-based ligands, fluorene-9-carboxylate (FCA) and fluorenone-2,7-dicarboxylate (FDCA), were incorporated into hybrid materials via coordination to the lead (II) cation. Coordination polymer Pb(FCA)2 (2) crystallizes in the monoclinic space group P21/c (a = 8.0518(9) Å, b = 25.338(3) Å, c = 10.5842(12) Å, β = 94.913(2)°), and forms a 1-D polymeric chain. Coordination polymer Pb3(FDCA)3(H2O)3 (3) crystallizes in the triclinic space group P1 (a = 6.6990(5) Å, b = 10.1529(7) Å, c = 13.6935(9) Å, α = 81.884(2)°, β = 87.260(2)°, γ = 84.399(2)°), and forms pillared 3-D layers. These three compounds have been identified via single crystal X-ray diffraction and characterized via powder X-ray diffraction, UV–Vis spectroscopy, and fluorescence spectroscopy.  相似文献   

10.
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   

11.
Two new heteropolyoxovanadoborates (H2dap)2H6{(VO)12O6[B3O6(OH)]6(H2O)}·13H2O (1, dap = 1,2-diaminopropane) and {[Zn(dien)]2[Zn(dien)(H2O)]4(VO)12O6[B3O6(OH)]6(H2O)}2·15H2O (2, dien = diethylenetriamine) have been hydrothermally synthesized and structurally characterized. Both 1 and 2 contain {(VO)12O6[B3O6(OH)]6(H2O)} cluster (denoted on V12B18), which is constructed by a puckered B18O36(OH)6 ring sandwiched between two triangles of six alternating cis and trans edge-sharing vanadium atoms, and a central water molecule. 1 consists of discrete [V12B18]10− cluster anions with H2dap2+ as counterions, while 2 consists of discrete neutral {[Zn(dien)]2[Zn(dien)(H2O)]4[V12B18]} clusters, which are built from two types of zinc(II) complex fragments connecting with V12B18 cluster through two Zn-(μ 3-O)-B bonds. Interestingly, 2 is the only example of the V12B18 cluster decorated by two types of zinc(II) complex fragments.  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.
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   

14.
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   

15.
Two new rare earth containing orthoborate crystals ASr4La3(BO3)6 (A = Li, Na) have been obtained by spontaneous nucleation from high-temperature melts of A2O–SrO–La2O3–B2O3–AF. X-ray diffraction analyses show that they both crystallize in the rhombohedral space group R-3 with cell parameters of a = 12.309(7) Å, c = 9.316(7) Å and a = 12.4049(13) Å, c = 9.348(2) Å for the Li and Na compounds respectively. Similar to the large A′6MM′(BO3)6 family, these compounds are all related to the structure of Sr3Y(BO3)3 with La and Sr statistically occupy the Sr site, and the alkaline elements and remaining Sr enter the ordered Y1 and Y2 sites, which can be approximately represented as (La2.91Sr3.09)(La0.09Sr0.91)Li[B6O18] and (La2.85Sr3.15)(La0.15Sr0.85)Na[B6O18]. The characteristic of the structure is that the La/Sr and isolated BO3 groups form a network with tunnels along the c-axis where the alkaline A and Sr ions alternatively reside. The optical transmission spectrum shows that the ultraviolet absorption edge of NaSr4La3(BO3)6 crystal is about 193 nm and Raman spectra reveal that both crystals possess sharp peaks at 930 cm−1.  相似文献   

16.
A nonmetal pentaborate [C6H13N2][B5O6(OH)4] (1) has been synthesized by 1,4-diazabicyclo[2.2.2] octane (DABCO) and boric acid, and characterized by single-crystal X-ray diffraction, FTIR, elemental analysis, and thermogravimetric analysis. Compound 1 crystallizes in the monoclinic system with space group Cc (no. 9), a=10.205(2) Å, b=14.143(3) Å, c=11.003(2) Å, β=113.97(3)°, V=1451.1(5) Å3, Z=4. The anionic units, [B5O6(OH)4], are interlinked via hydrogen bonding to form a three-dimensional (3D) supramolecular network containing large channels, in which the protonated [C6H13N2]+ cations are located. Second-harmonic generation (SHG) measurements on the powder samples reveal that 1 exhibits SHG efficiency approximately 0.9 times that of potassium dihydrogen phosphate (KDP).  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.
Hydro­thermally prepared Ba3V2(HPO4)6 contains a three‐dimensional network of VIIIO6 octahedra [dav(V—O) = 2.014 (2) Å] and HPO4 [dav(P—O) = 1.537 (3) Å] tetrahedra, sharing vertices. 12‐coordinate Ba2+ cations [dav(Ba—O) = 2.944 (4) Å] complete the structure.  相似文献   

19.
Synthesis and X-ray study of the polyanion [AsIII 4Mo6W14O72(H2O)2]12 isomorphous of [AsIII 4W20O72(H2O)2]12. The addition of an excess of MoO42– to a solution of [AsIII2W8O30(OH)]7– led at pH=4 to a new polyanion [AsIII 4Mo6W14O72(H2O)2]12– isostructural of [AsIII 4W20O72(H2O)2]12–. The structure of this compound was determined by X-ray diffraction: a=11.183(4) Å, b=13.432(3) Å, c=19.626(5) Å, α=77.87(2), β=73.57(3), γ=67.44(3)°, V=2 594(1) Å3, P1̄. Reliability factors are R=7.89 and Rw=9.97. The starting compound underwent an isomerisation β→α and one tungsten was formally substituted by one molybdenum atom; two other molybdenum atoms were incorporated. The polyanion is formed of two units αB–AsIIIMo2W7O33 connected by a double chain AsIIIOMo2O2(H2O). Arsenic and molybdenum are both bound to two octahedrons WO6 of one unit AsIIIOMoO2W7O33, both molybdenum atoms of which are contiguous. © 2000 Académie des sciences / Éditions scientifiques et médicales Elsevier SASpolymolybdotungstate / arsenomolybdotungstate / crystal structure / (hexamolybdenumtetradecatungsten)ate / synthesis of a new mixed polytungstate  相似文献   

20.
《Solid State Sciences》2007,9(11):1012-1019
Two novel inorganic–organic hybrid compounds composed of Keggin tungstocobaltate framework and cobalt(II)–N coordination complexes, K[Co(phen)2(H2O)]2[HCoW12O40]·2H2O (1) (phen = 1,10-phenanthroline) and [Co(2,2′-bipy)3]1.5{[Co(2,2′-bipy)2(H2O)][HCoW12O40]·0.5H2O (2) (bipy = bipyridine), have been synthesized under hydrothermal conditions by directly using Keggin POMs as starting materials, which were characterized by elemental analyses, IR, TG analyses and X-ray single crystal diffraction. Crystal data for compound 1: C48H41Co3KN8O44W12, triclinic, space group P-1, a = 10.918(5) Å, b = 13.401(5) Å, c = 13.693(5) Å, α = 69.291(5)°, β = 71.568(5)°, γ = 78.421(5)°, V = 1768.9(12) Å3, Z = 1; for compound 2: C130H104Co7N26O83W24, orthorhombic, space group, C2/c, a = 46.839(9) Å, b = 14.347(3) Å, c = 26.147(5) Å, α = β = γ = 90°, V = 17,570(6) Å3, Z = 4. Compound 1 exhibits a pseudo-1D chainlike structure, in which potassium ions act as linkages of Keggin unit doubly grafted by [Co(phen)2(H2O)] complex. Compound 2 represents a [Co(2,2′-bipy)2(H2O)]2+ mono-grafted Keggin tungstocobaltate derivative with 1.5[Co(2,2′-bipy)3]2+ countercations. The cyclic voltammetric behavior of 1-CPE is similar to the parent 3-CPE, but the cyclic voltammetric behavior of CoII shows a little difference. Variable-temperature magnetic susceptibility measurement of compound 1 demonstrates the presence of antiferromagnetic interactions.  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号