碳酸镉@二氧化硅菱形体核壳结构以及二氧化硅菱形体空心结构微粒的制备

利用Stöber种子生长法, 第一次在尺寸为2 μm左右的碳酸镉菱形微粒表面直接包覆二氧化硅层, 得到碳酸镉@二氧化硅核壳结构的胶体粒子. 作为核壳结构的壳层部分, 二氧化硅层的厚度可以通过加入体系中的正硅酸乙酯的量来控制. 作为核层的碳酸镉胶体部分可以被盐酸刻蚀掉, 进而得到具有菱形体空心结构的二氧化硅微粒.     

Infrared spectroscopic and density functional theory studies on the reactions of cadmium atoms with carbon monoxide in solid argon

Reactions of laser-ablated cadmium atoms with carbon monoxide molecules in solid argon have been investigated using matrix isolation infrared spectroscopy. On the basis of isotopic substitution, the absorption at 1858.2 cm(-1) is assigned to the C-O stretching of the CdCO molecule, which is formed during the sample deposition. Cadmium di- and tricarbonyls, Cd(CO)n (n = 2, 3), have not been observed under the same experimental conditions. Density functional theory calculations have been performed on the cadmium carbonyls Cd(CO)n (n = 1-3), which lend strong support to the experimental assignments of the infrared spectra. It is predicted that the CdCO molecule is a linear triplet molecule and its formation involves Cd 5s --> 5p promotion. This promotion increases the Cd-CO bonding by decreasing the sigma repulsion and increasing the Cd 5p orbital --> CO pi back-donation. The absence of cadmium di- and tricarbonyls, Cd(CO)n (n = 2, 3), has also been discussed in some detail.     

碳酸镉饱和溶液作标准用便携式AAS测定镉的研究

以CdCO3固体溶于煮沸冷却的去离子水中配制成饱和溶液,将该饱和溶液稀释成标准溶液系列用于便携式钨丝电热原子吸收光谱仪野外实时与在线分析环境水样中痕微量镉。经测定在25℃该饱和溶液中镉的浓度为272μg.L-1,与理论计算值279μg.L-1有很好的吻合。实验优化了相关的仪器条件和实验条件,在最优的条件下该方法的线性相关系数为0.9948,检出限为0.08μg.L-1。通过检测分析环境中的水样验证了该方法是可行的。     

Solvothermal Syntheses and Crystal Structures of Two New Nonmetal Borates:C_4H_(10)N_2·B_6O_8(OH)_2 and (NH_3CH_2CH_2NH_3)B_5O_8(OH)

Two new borate compounds,C4H10N2·B6O8(OH)2 1 and (NH3CH2CH2NH3)B5O8-(OH) 2,have been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction,IR,elemental analysis and thermal analysis. Compound 1 crystallizes in the monoclinic system,space group P21/c,with a=8.3318(17),b=6.2118(12),c=12.479(3) ,β=108.96(3)o,V=610.8(2) 3,Mr=313.02,Z=2,Dc=1.702 g/cm3,μ=0.150 mm-1,F(000)=320,R =0.0387 and wR =0.0924. Its layered structure is linked by infinite covalently coordinated neutral sheets with 3,20-membered window system,which are built up from alternative B6O8(OH)2 subunits donated by two piperzazine nitrogen donors. 2 crystallizes in monoclinic,space group Cc,with a=6.7207(13),b=11.481(2),c=12.564(3) ,β=95.25(3)o,V=965.4(3) 3,Mr=261.18,Z=4,Dc=1.797 g/cm3,μ= 0.164 mm-1,F(000)=536,R=0.0396 and wR=0.0752. Its oxoborate structure is generated from the sheets of 3,9-membered boron rings bonded diamine molecules through electrostatic and H-bonding interactions to form a two-dimensional layered network.     

镧(Ⅲ)系锑硒化合物[Ln(en)_4]SbSe_4·0.5en(Ln=Dy,Ho)的溶剂热合成与晶体结构(英文)

本文研究了Ln2O3/Sb/Se/en溶剂热反应体系,合成了2个镧(Ⅲ)系锑硒化合物[Ln(en)4]SbSe4·0.5en[Ln=Dy(1),Ho(2)],用元素分析和红外光谱对化合物进行了表征,并用X-射线单晶衍射测定了化合物的单晶结构,两者都属于单斜晶系,P21/n空间群。结构对比研究发现,在en溶剂中,SbSe43-离子可以与半径较大的La3+和Nd3+离子配位,而不与半径较小的Dy3+和Ho3+离子配位,可见镧系收缩效应对SbSe43-离子与镧系金属离子Ln3+的配位有重要影响。     

单一手性烯烃铜(Ⅰ)配位聚合物

The solvothermal reaction of CuCl with R-(-)-1-allyl-3-methylpiperazine at 70 ℃ gives one-dimensional chain Cu-coordination polymer through olefin moiety binding to Cu atoms formulated as [Cu(C₈H₁₆N₂)Cl]. It is interesting to note that through Cu₂Cl₂ dimer unit 1 results in a supramolecular 3-dimensional coordination polymer. Powdered sample measurement of 1 reveals that 1 is second-harmonic generation (SHG) active compound. Crystal parameters for 1, space group P2₁2₁2₁, a=0.763 1(9) nm, b=0.891 0(10) nm, c=1.494 6(17) nm, α=90°, β=90°, γ=90°, V=1.016(2) nm³, Z=2, M=478.44, D_c=1.564 Mg·m^-3. CCDC: 650193.     

一维链状氧族化合物［Mn(en)3］CdSnTe4的制备及其半导体性质的研究

The solvothermal technique was used for the synthesis of ［Mn(en)₃］CdSnTe₄ (Ⅰ). The crystal structure has been determined by single crystal X-ray diffraction techniques. The crystal belongs to the triclinic, space group P1(No.1     

含非交换氘的四唑-锌配合物

The solvothermal reaction (D₂O) of 2,6-dideuterium-4-cyanopyridine with ZnCl₂ in the presence of NaN₃ offers a novel complex Zn(OD)(C₆H₂D₂N₄) (1) in which Zn has a distorted tetrahedron composed of two N atoms from one tetrazoyl group and pyridyl group and two O atoms from two deuteratohydroxy OD groups. Crystal data for 1: Pbcn, a=1.456 8(5) nm, b=0.659 2(2) nm, c=1.645 3(5) nm, α=90°, β=90°, γ=90°, V=1.580 0(9) nm³, Z=8, M=231.54, D_c=2.236 Mg·m^-3, μ=3.070 mm^-1, R₁=0.043 4, wR₂=0.120 6, S=1.029. CCDC: 660629.     

Solvothermal Synthesis and Structure Studies of a Mixed-valence Oxochloromolybdenum Complex

Emerald green crystals of a new mixed-valence oxochloromolybdenum complex,Mo(OH)2(2,2′-bipy)Cl2.[MoO(2,2′-bipy)Cl3]2, were obtained in an attempt to synthesize the Mo-S cluster compounds under solvothermal conditions. The title compound was characterized by EPR and X-ray single-crystal diffraction techniques. Crystallographic data: orthorhombic, space group Fdd2, a = 12.684(1), b = 21.518(2), c = 29.096(3)A, Mr = 1103.97, V= 7941(1)A^3, Z= 8, Dc =1.843 g/cm^3,μ= 1.514 mm^-1, F(000) = 4304, R = 0.0654 and wR = 0.1544 for 1944 observed reflections with 1 ≥/ 2σ(I). The compound consists of two different neutral molecules, Mo^IV-(OH)2(2,2′-bipy)Cl2 and MoVO(2,2′-bipy)Cl3. Both Mo^IV and Mo^V ions are in a distorted octahedral environment. The Mo(1)^IV atom is surrounded by two Cl^- ions and two O atoms from OH^- and two N atoms from a 2,2′-bipy ligand. The Mo(2) atom is surrounded by three Cl^- ions, one O^2- anion and two N atoms from another 2,2“-bipy ligand. The bipyridine occupies two cis-equatorial sites, while the Cl^- ions are located at the axial and equatorial positions.     

Solvothermal Synthesis and Crystal Structure of [H2N（CH2）2NH3]{Co[H2N（CH2）2NH2]3}[SbSe4]

1 INTRODUCTION The chalcogenidometallates with open frame- works have attracted considerable interest as pos- sible zeolite-like materials, of which highly interes- ting properties could be expected. Over the last de- cades a large number of thioanti…     

Synthesis and Crystal Structure of a Coordination Polymer {[Co(phth)(phen)(H2O)]·(C2H5OH)}n

The coordination polymer {[Co(phth)(phen)(H2O)]·(C2H5OH)}n (phth = phthalate, phen = 1,10-phenanthroline) with formula C22H20CoN2O6 (Mr = 467.33) was synthesized by the solvothermal method under low temperature, and its crystal structure was determined by singlecrystal X-ray diffraction. The complex belongs to monoclinic system, space group P21/n with a =12.7352(16), b = 8.8125(11), c = 18.677(2) (A), β = 102.633(2)°, V = 2045.3(4) (A)3, Z = 4, Dc =1.518 g/cm3,μ = 0.882 mm-1, F(000) = 964, S = 1.053, the final R = 0.0401 and wR = 0.0984 for 3135 observed reflections (I ＞ 2σ(I)). Single-crystal X-ray analysis revealed that the Co(Ⅱ) ion is six-coordinated. The cobalt complex forms a one-dimensional chain structure via phthalate bridging ligand. In the cobalt complex, a 3D network structure is formed by π-π stacking interaction of 1,10-phenanthroline as well as intermolecular hydrogen bonding interactions.     

New Dimeric Selenidoarsenate(Ⅲ): Solvothermal Synthesis and Crystal Structure of [Co(en)3]2As2Se5

A new selenidoarsenate [Co(en)3]2As2Se5 1 (en = ethylenediamine) was synthesized by a reaction of AsCl3, COCl2·6H2O and Se in en under mild solvothermal conditions, and the structure was determined by single-crystal X-ray diffraction. 1 crystallizes in the orthorhombic system, space group Pbca with a = 15.5092(12), b = 11.5756(9), c = 17.8138(14) (A), V= 3198.1(4)(A)3, Mr = 1023.12, Z = 4, Dc = 2.125 g/cm3,μ = 8.807 mm-1, F(000) = 1976, S = 1.171, the final R =0.0591 and wR = 0.1067 for 3170 observed reflections with I ＞ 2σ(Ⅰ). 1 consists of isolated dimeric[As2Se5]4- anion constructed by two comer-sharing AsSe3 trigonal pyramids and transition metal [Co(en)3]2+ cations. The optical absorption property and thermal stability of 1 are reported.     

New Dimeric Selenidoarsenate(III):Solvothermal Synthesis and Crystal Structure of [Co(en)_3]_2As_2Se_5

1 INTRODUCTION The mild solvothermal synthesis with the presence of a structure-directing agent is proved to be a versa- tile route for the preparation of chalcogenidometa- lates of the heavier group (14 and 15) elements[1～3]. Templated by the transition metal complex cations, a large number of chalcogenidoantimonates containing transition metal complex ions have been synthesized by solvothermal method, such as Mn2(en)2Sb2S5[4], [Co(en)3]CoSb4S8[5], [M(en)3]Sb2S4 (M = Co, Ni)[6], [N…     

Solvothermal Synthesis and Crystal Structure of a Layered Thioantimonate(Ⅲ) [C_4H_9NH_3]_2Sb_4S_7

An inorganic-organic hybrid thioantimonate(Ⅲ) [CH3(CH2)3NH3]2Sb4S7 1 with layered structure was synthesized by solvothermal method. 1 crystallizes in the triclinic system,space group P1 with a=7.0124(11),b=11.919(2),c=14.879(3),α=108.791(3),β=102.441(3),γ=92.846(2)o,V=1140.1(3)3,Mr=859.71,Z=2,Dc=2.504 g/cm3,μ =5.324 mm-1,F(000)=804,S=1.013,the final R=0.0297 and wR=0.0618 for 3534 observed reflections with I > 2σ(I). 1 consists of [C4H9NH3]+ cations and two-dimensional [Sb4S7]n2n- anion which is composed of three SbS3 trigonal pyramids and one SbS4 unit joined by sharing common corners. The anionic layers are stacked perpendicularly to the c axis of the unit cell forming two-dimensional channels between the layers. The [C4H9NH3]+ cations interdigitate in a bilayer and reside in the 2D channels leading to a sandwich-like arrangement of the anion and cations.     

Synthesis,Crystal Structure and Photoluminescence of a One-dimensional Zinc(Ⅱ)Coordination Polymer with Substituted Terpyridine

<正>The title compound,[Zn(4-pytpy)(NO_3)_2](4-pytpy=4'-(4-pyridyl)-2,2':6',2"- terpyridine)1,has been synthesized by the solvothermal reaction of Zn(NO_3)_2·6H_2O with 4-pytpy in CH_3OH solution.It crystallizes in the triclinic system,space group P_1~-with a=8.358(6),b= 11.121(8),c=11.374(8)(?),α=74.226(11),β=74.532(11),γ=83.085(12)°,M_r=499.74,V= 979.3(12)(?)~3,Z=2,D_c=1.695 g/cm~3,F(000)=508,μ=1.309 mm~(-1),the final R=0.0547 and wR= 0.1588.X-ray crystal structure analysis revealed that the Zn~Ⅱis hexa-coordinated by two oxygen atoms from two nitrate groups and four nitrogen atoms,three of which are from the tridentate domain of one 4-pytpy and the other from the monodentate domain of another 4-pytpy.4-pytpy as a bridging ligand connects Zn~Ⅱinto a one-dimensional coordination polymer.     

Structural Evidence of Anion's Effect on the Ion Packing of [Ni2(teta)3]4+ in the View of H-bonding Interaction

Two dinuclear nickel(II) complexes [Ni2(teta)3]Cl4·2H2O 1 and [Ni2(teta)3](NO3)4 2 (teta = triethylenetetramine) were synthesized by a solvothermal method and structurally characterized. Complex 1: orthorhombic, Pbca, a = 13.791(3), b = 13.078(3), c = 18.323(4) , V = 3304.8(12) 3, Z = 4, Mr = 733.98, Dc = 1.475 g/cm3, μ = 1.500 mm-1, F(000) = 1560, R = 0.0585 (I > 2σ(I)) and wR = 0.1243. Complex 2: orthorhombic, P212121, a = 7.8279(14), b = 14.209(3), c = 31.163(6) , V = 3466.2(11) 3, Z = 4, Mr = 804.19, Dc = 1.541 g/cm3, μ = 1.164 mm-1, F(000) = 1704, R = 0.0401 and wR = 0.0840 for 5950 observed reflections (I > 2σ(I)). Two Ni2+ ions are connected by one linear bridging teta ligand, forming a dinuclear [Ni2(teta)3]4+ cation. Each Ni2+ ion in 1 and 2 takes a distorted octahedral geometry with six coordinated N atoms from two teta ligands. The effect of different anions on the arrangement of [Ni2(teta)3]4+ cations has been discussed in view of H-bonding interactions. Thermal stability of 1 and 2 was also investigated.     

碱金属硒化物MHgSbSe~3(M=K,Rb, Cs)的晶体结构及其半导体性 质的研究

用有机溶剂热生长技术(SolvothermalTechnique)制备碱金属硒化物MHgSbSe~3(M=K,Rb,Cs),用单晶X射线衍射技术对其进行晶体结构分析,热分析结果表明,在常温(<200℃)下均为稳定的化合物。光学性质测试表明它们是半导体材料,KHgSbSe~3,RbHgSbSe~3,CsHgSbSe~3的禁带宽度依次为1.85eV,1.75eV,1.65eV。     

过渡金属配合物为模板合成两个新的硫代锡酸盐(英)

利用溶剂热方法在温和的条件下合成了二个新的硫代锡酸盐[Mn(en)₃]₂Sn₂S₆·2H₂O(en=H₂NC₂H₄NH₂) (1)和[Mn(dien)₂]₂Sn₂S₆ (dien=H₂NC₂H₄NHC₂H₄NH₂) (2)，通过X-射线衍射分析表征其晶体结构。化合物1的晶体学参数：C₁₂H₄₈Mn₂N₁₂S₆Sn₂·2H₂O，M_r=936.28，单斜晶系，P2₁/c，a=1.012 9(3)，b=1.574 6(4)，c=1.152 4(3) nm，β=102.36(1)°，V=1.795 5(8) nm³，Z=2，D_c=1.732 g·cm^-3，μ(MoKα)=2.442 mm^-1，F(000)=940，R=0.063 3，wR=0.081 4；化合物2的晶体学参数：C₁₆H₅₂Mn₂N₁₂S₆Sn₂，M_r=952.32，单斜晶系，P2₁/c，a=1.248 12(3)，b=0.937 60(4), c=1.776 17 (7) nm，β=121.752(2)°，V=1.767 5(1) nm³，Z=2，D_c=1.789 g·cm^-3，μ(MoKα)=2.479 mm^-1，F(000)=956，R=0.057 9，wR=0.137 4。在两个化合物中存在的[Sn₂S₆]^4-阴离子均由共边的两个SnS₄四面体构成。在1中，锰离子螯合3个乙二胺做为阳离子模板，而在2中锰离子螯合2个二乙烯三胺做为阳离子模板。金属配合物作为模板对阴离子[Sn₂S₆]^4-在晶体结构中的排列产生重要的影响。     

金属碲化物[Ga(en)~3]In~3Te~7晶体结构和性质的研究

以有机溶剂热生长技术(solvothermaltechnique),即在180℃乙二胺(en)溶液中,以GaCl~3,InCl~3,Rb~2Te和Te在密闭容器中反应7d,制备出新的硫族化合物[Ga(en)~3]In~3Te~7。其阴离子基团为Zintlanion:~∞^2[In~3Te~7]^3^-,阳离子基团为Ga与乙二胺(en)的配合物:[Ga(en)~3]^3^+。以单晶X射线衍射技术解得该晶体结构属单钭晶系,空间群为P2~1/c,(no.14),{Ga(en)~3]In~3Te~7的晶胞数据：a=1.0460(2)nm,b=1.6981(3)nm,c=1.4994(6)nm,α=90°,β=95.46(2)°,γ=90°,V=2.651(1)nm^3,Z=4。热分析结果表明,该化合物的热分解分三步进行。光学性质测试表明它们是半导体材料,禁带宽度为1.65eV。     

Solvothermal Synthesis,Crystal Structure and Electrochemical Property of Complex [Co(p-MBA)_2(2,2′-bipy)(H_2O)]·(H_2O)

One novel complex [Co(p-MBA)2(2,2′-bipy)(H2O)]·(H2O) has been synthesized by the reaction of p-methylbenzoic acid with 2,2′-bipyridine in the solvent mixture of water and methanol. It crystallizes in triclinic,space group P1 with a=0.70479(14),b=1.1211(2),c=1.6718(3) nm,α=103.806(3),β=90.795(3),γ=104.207(3)o,V=1.2399(4) nm3,Mr=512.41,Dc=1.373 g/cm3,Z=2,F(000)=532,μ=0.733 mm-1,R= 0.0432 and wR=0.0957. The crystal structural analysis shows that the cobalt atom is coordinated with three oxygen atoms from two p-methylbenzoic acids and one water molecule and two nitrogen atoms from one 2,2′-bipyridine,forming a distorted square-pyramidal coordination geometry. The cyclic voltammetry behavior of the complex is also reported.