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1.
Single crystals of the compounds (C3N6 H7)4(CN3H6)2[UO2(CrO4)4] · 4H2O (I) and (H3O)6[UO2(CrO4)4] (II) are synthesized, and their structures are investigated using X-ray diffraction. Compound I crystallizes in the triclinic system with the unit cell parameters a = 6.3951(8) ?, b = 10.8187(16) ?, c = 16.9709(18) ?, α = 93.674(4)°, β = 97.127(4)°, γ = 92.020(4)°, space group, P Z = 1, V = 1161.6(3) ?3, and R = 0.0470. Crystals of compound II belong to the monoclinic system with the unit cell parameters a = 14.3158(4) ?, b = 11.7477(3) ?, c = 13.1351(4) ?, β= 105.836(1)°, space group C2/c, Z = 4, V = 2125.2(1) ?3, and R = 0.0213. The uranium-containing structural units of crystals I and II are mononuclear anionic complexes of the composition [UO2(CrO4)4]6− with an island structure, which belong to the crystal-chemical group Am 14 (A = UO2+2, M 1 = CrO2−4) of the uranyl complexes. The [UO2(CrO4)4]6− anionic complexes are joined into a three-dimensional framework through the electrostatic interactions with outer-sphere cations and a system of hydrogen bonds. Original Russian Text ? L.B. Serezhkina, E.V. Peresypkina, A.V. Virovets, A.G. Verevkin, D.V. Pushkin, 2009, published in Kristallografiya, 2009, Vol. 54, No. 2, pp. 284–290.  相似文献   

2.
Single crystals of the compound K8[(UO2)2(C2O4)2(SeO4)4] · 2H2O (I) are synthesized, and their structure is investigated using X-ray diffraction. Compound I crystallizes in the monoclinic system with the unit cell parameters a = 14.9290(4) ?, b = 7.2800(2) ?, c = 15.3165(4) ?, β = 109.188(1)°, V = 1572.17(7) ?3, space group P21/n, Z = 2, and R = 0.0297. The uranium-containing structural units of crystals I are dimers of the composition [(UO 2)2(C2O4)2(SeO4)4]8−, which belong to the crystal-chemical group AB 01 B 2 M 1 (A = UO22+, B 01 = C2O42−, B 2 = SeO42−, M 1 = SeO42−) of the uranyl complexes. The [(UO2)2(C2O4)2(SeO4)4]8− dimers are joined into a three-dimensional framework through electrostatic interactions with the outer-sphere potassium cations. Original Russian Text ? L.B. Serezhkina, E.V. Peresypkina, A.V. Virovets, A.G. Verevkin, D.V. Pushkin, 2009, published in Kristallografiya, 2009, Vol. 54, No. 1, pp. 68–71.  相似文献   

3.
以五氧化二钒干凝胶、碳酸锰、磷酸二氢铵、碳酸锂、乙炔黑为原料,采用固相法在相对较低的温度条件下合成了x Li Mn PO4·y Li3V2(PO4)3锂离子电池复合正极材料。采用X射线衍射(XRD)、扫描电镜(SEM)对其晶体结构和表面形貌进行表征。结果表明,750℃下烧结15 h合成的3Li Mn PO4·Li3V2(PO4)3为结晶良好的两相结构,颗粒粒径较小且分布比较均匀,其在室温、0.2 C倍率下首次充放电容量分别为144.8 m Ah/g和139.8 m Ah/g,循环50次后容量为130.5 m Ah/g。  相似文献   

4.
Single crystals of the compound {NH2(C2H5)2}2[(UO2)2C2O4(CH3COO)4] · 2H2O (I) are synthesized, and their structure is investigated using X-ray diffraction. Compound I crystallizes in the monoclinic system with the unit cell parameters a = 9.210(2) ?, b = 14.321(3) ?, c = 12.659(3) ?, β = 105.465(13)°, V = 1609.2(6) ?3, space group P21/c, Z = 2, and R = 0.0198. The structural units of crystals I are binuclear groups of the composition [(UO2)2C2O4(CH3COO)4]2− with an island structure, which belong to the crystal-chemical group A 2 K 02 B 401 (A = UO22+, K 02 = C2O42−, B 01 = CH3COO) of the uranyl complexes, diethylammonium cations, and water molecules. The uranium-containing groups are joined into a three-dimensional framework through electrostatic interactions with diethylammonium cations and a system of hydrogen bonds, which are formed with the participation of the atoms involved in the composition of the water molecules, oxalate ions, acetate ions, and diethylammonium cations. Original Russian Text ? L.B. Serezhkina, A.V. Vologzhanina, N.A. Neklyudova, V.N. Serezhkin, 2009, published in Kristallografiya, 2009, Vol. 54, No. 1, pp. 65–67.  相似文献   

5.
Single crystals of the compound K2[(UO2)4(O)2(OH)2(C2O4)(CH3COO)2(H2O)2]·2H2O (I) are synthesized, and their structure is investigated using X-ray diffraction. Crystals of compound I belong to the triclinic system with the unit cell parameters a = 7.6777(6) ?, b = 7.9149(7) ?, c = 10.8729(9) ?, α = 72.379(2)°, β = 86.430(3)°, γ = 87.635(2)°, V = 628.33(9) ?3, space group P , Z = 1, and R 1 = 0.0323. The main structural units of the crystals are [(UO2)4(O)2(OH)2(C2O4)(CH3COO)2(H2O)2]2− chains, which belong to the crystal-chemical group A 4 M 23 M 22 K 02 B 201 M 21 (A = UO22+, M 3 = O2−, M 2 = OH, K 02 = C2O42−, B 01 = CH3COO, M 1 = H2O) of the uranyl complexes. The chains are formed by linking the centrosymmetric tetramers of the composition (UO2)4(O)2(OH)2(CH3COO)2(H2O)2 via tetradentate bridging oxalate ions. The uranium-containing groups are joined into a three-dimensional framework through the electrostatic interaction with potassium cations and a system of hydrogen bonds, which are formed with the participation of atoms involved in the composition of the water molecules, hydroxide ions, and uranyl ions. Original Russian Text ? L.B. Serezhkina, A.V. Vologzhanina, N.A. Neklyudova, V.N. Serezhkin, 2009, published in Kristallografiya, 2009, Vol. 54, No. 3, pp. 483–487.  相似文献   

6.

Abstract  

The synthesis and crystal structure of the dinuclear manganese (II) compound [Mn2(bpy)4(2-ClC6H4COO)2](ClO4)2·2EtOH is described. The complex crystallizes in the monoclinic system, space group P21/n with a = 12.2067(18), b = 17.335(3), c = 13.706(3) ? and β = 92.606(8)°. In this structure, two manganese ions are bridged by two 2-chlorobenzoate ligands in a synanti mode. The hexa-coordination of each manganese is completed by two 2,2′-bipyridine ligands. Two perchlorate anions and two molecules of ethanol complete the packing. In order to check the magnetic properties previously reported from a powder sample, new magnetic studies have been carried out from a crystal sample, obtaining J = −1.79 cm−1 and g = 2.00 (H = −JS 1 ·S 2 ).  相似文献   

7.

Abstract  

In the present study we report the synthesis, crystal structure, spectroscopic and thermal analysis of mixed alkali A1−x (NH4) x (H2C2O4)(HC2O4)(H2O)2 with A = K, Rb. Single crystal refinements showed that the two compounds Rb0.86(NH4)0.14(H2C2O4)(HC2O4)(H2O)2 and K0.53(NH4)0.47(H2C2O4)(HC2O4)(H2O)2 adopt P − 1 space group. The nine fold coordination cationic sites are randomly occupied by Rb+/NH4 + and K+/NH4 + respectively for rubidium and potassium compounds. The structure consists of a three-dimensional network formed by the succession along (c) axis of corrugated sheets formed by alkali polyhedra layers in the packing of four-membered rings [A4(HC2O4)2(H2C2O4)2] linked and bridged by oxalate groups that behave as bi and tetradentate ligand under three different coordination modes. The stability of the crystal lattice is ensured by interesting hydrogen bonding contacts: N–H···O and O–H···O. The thermal behavior under air reveals two anomalies at 368 and 402 K attributed respectively to a structural phase transition probably due to the reorientation of ammonium tetrahedral and to the release of crystalline water. IR spectroscopy further confirms that this material loses crystallization water gradually in the temperature range 400–460 K.  相似文献   

8.
Abstract  Treatment of Mn2(CO)10 with 2-thiazoline-2-thiol in the presence of Me3NO at room temperature afforded the dimanganese complexes [Mn2(CO)7(μ-NS2C3H4)2] (1) and [Mn2(CO)6(μ-NS2C3H4)2] (2) in 51 and 34% yields, respectively. Compound 1 was quantitatively converted into 2 when reacted with one equiv of Me3NO. Reaction of 1 with triphenylphosphine at room temperature furnished the mononuclear complex [Mn(CO)3(PPh3)(κ 2-NS2C3H4)] (3) in 66% yield. All three new complexes have been characterized by elemental analyzes and spectroscopic data together with single crystal X-ray diffraction studies for 1 and 3. Compound 1 crystallizes in the orthorhombic space group Pbca with a = 12.4147(2), b = 16.2416(3), c = 19.0841(4) ?, β = 90°, Z = 8 and V = 3848.01(12) ?3 and 3 crystallizes in the monoclinic space group P 21/n with a = 10.41730(10), b = 14.7710(2), c = 14.9209(2) ?, β = 91.1760(10)°, Z = 4 and V = 2295.45(5) ?3. Graphical Abstract  Two new dimanganese complexes [Mn2(CO)7(μ-NS2C3H4)2] (1) and [Mn2(CO)6(μ-NS2C3H4)2] (2) were formed when [Mn2(CO)10] was treated with 2-thiazoline-2-thiol in the presence of Me3NO. Compound 2 reacts with PPh3 to give the monomeric complex [Mn(CO)3(PPh3 )(κ 2-NS2C3H4)]. The structures of 1 and 3 were established by crystallography. Shishir Ghosh, Faruque Ahmed, Rafique Al-Mamun, Daniel T. Haworth, Sergey V. Lindeman, Tasneem A. Siddiquee, Dennis W. Bennett, Shariff E. Kabir Investigations of 2-thiazoline-2-thiol as a ligand: Synthesis and X-ray structures of [Mn2(CO)7(μ-NS2C3H4)2] and [Mn(CO)3 (PPh3)(κ 2-NS2C3H4)].   相似文献   

9.
刘丽英  陈炼  张海燕  翟玉春 《人工晶体学报》2012,41(6):1686-1690,1695
分别以柠檬酸、葡萄糖和蔗糖为碳源,采用球磨与碳热还原结合法制备了锂离子电池正极材料Li3V2(PO4)3/C。采用TG-DTA分析确定了合成过程的反应机理。通过XRD、SEM及恒电流充放电等测试研究了碳源对产物物理及电化学特性的影响。结果表明,碳源的选择对产物形貌和电化学性能影响较大。不同碳源制备的材料都具有单一相的Li3V2(PO4)3晶体结构,以柠檬酸为碳源制备的磷酸钒锂综合电化学性能较好,0.1 C和1 C条件下,首次放电容量分别为151.0 mAh·g-1和131.6 mAh.g-1,50次循环后容量保持率为95.0%和96.6%。  相似文献   

10.
[NH3(CH2)3NH3]2[Ni(HP2O7)2(H2O)2] 4H2O (NiDAP) is a new diphosphate of transition metallic and organic cations obtained from a mixture of H4P2O7, 2NiCO3 Ni(OH)2 4H2O and NH2(CH2)3NH2 in a 1:1/6:1 molar ratio. This mixed organo-mineral compound crystallizes in the triclinic system, P¯, with the unit cell dimensions: a = 7.3678(3)~Å, b = 7.8018(5)Å, c = 11.1958(7)Å, = 76.914(4), = 81.052(4), = 85.46(1), V = 618.57(6)Å3 and Z = 1. The crystal structure of NiDAP consists of a complex anion, [Ni(HP2O7)2(H2O)2]4– and a diammoniumpropane cation. The complex anion is built up from two neutral water molecules (OW1) and two diphosphosphoric anions coordinated to Ni(II) in a bidentate chelating manner. (OW1) molecules link anionic complexes, [Ni(HP2O7)2(H2O)2]4– to create a thick bidimensional layers parallel to the (a, b) plane. These layers are interconnected in three dimensions through hydrogen bonds established between organic cations, the remaining water molecules OW2, OW3, and some external oxygen atoms of the anionic complex arrays. NiDAP was also characterized by IR spectroscopy, TG-DTA, and DSC analyses.  相似文献   

11.

Abstract  

Using 1,4,8,11-tetraazacyclotetradecane (cyclam) as a template, two new layered zincophosphites, Zn(HPO3)2·0.5(C10H28N4) (1) and Zn2(HPO3)3·0.5(C10H28N4) (2), were synthesized and characterized by single crystal X-ray diffraction. The two new compounds crystallize in the triclinic system with the space group P − 1 and the cell parameters: a = 8.3130 ?, b = 8.7289 ?, c = 9.0055 ?, α = 106.90(1), β = 95.56(1), γ = 105.30(1), V = 592.31 ?3, Z = 2 for 1 and a = 9.0406 ?, b = 9.4234 ?, c = 9.4519 ?, α = 91.19(1), β = 100.73(1), γ = 106.85(1), V = 754.82 ?3, Z = 2 for 2. Both structures are described in terms of phosphometallic slabs hosting the cyclam cation.  相似文献   

12.
采用溶胶-凝胶法制备Eu3+掺杂的Zn Al2O4/Si O2(ZAS)块状透明微晶玻璃发光材料。利用X射线衍射(XRD),透射电子显微镜(TEM)和荧光光谱(PL)等测试手段,系统研究了不同Eu3+掺杂浓度对ZAS发光性能的影响以及不同热处理温度对ZAS∶Eu3+发光性能的影响。结果表明,ZAS∶Eu3+在611 nm处具有强烈的红光发射峰,发射强度随着Eu3+掺杂浓度的增加,出现浓度淬灭效应,当掺杂量为20mol%时,发光强度最大;随着热处理温度的升高,存在高温淬灭效应,当热处理温度为900℃时,材料发光强度最优。CIE色度图分析表明,ZAS∶0.20Eu3+是一种潜在、优良的红光显示微晶玻璃材料。  相似文献   

13.
The molecular and crystal structures of two p-alkoxybenzylidene)-p′-toluidines C2H5O-C6H4-CH=N-C6H4-CH3 (1) and C4H9O-C6H4-CH=N-C6H4-CH3 (2) are determined by X-ray diffraction. Crystals 1 and 2 contain four and two crystallographically independent molecules, respectively. In 1, the geometry of the independent molecules is almost identical. In 2, the independent molecules differ in the conformation of the alkyl chain, which is disordered in one of them. An analysis of the crystal packing of 2 reveals the alternation of spacious layers formed by loosely packed aliphatic fragments of molecules and layers of closely packed aromatic fragments, which ensures the formation of the mesogenic phase in the course of melting of crystals 2. In crystal 1, loose aliphatic layers are absent. Original Russian Text ? L.G. Kuz’mina, N.S. Kucherepa, M.N. Rodnikova, 2008, published in Kristallografiya, 2008, Vol. 53, No. 6, pp. 1072–1078.  相似文献   

14.
Three Sr2+ compounds with the Edta 4− and H2 Edta 2− ligands—Sr2(Edta) · 5H2O (I), Sr2(H2 Edta)(HCO3)2 · 4H2O (II), and Sr2(H2 Edta)Cl2 · 5H2O (III)—are synthesized, and their crystal structures are studied. In I, the Sr(1) atom is coordinated by the hexadentate Edta 4− ligand following the 2N + 4O pattern and by two O atoms of the neighboring ligands, which affords the formation of zigzag chains. The Sr(2) atom forms bonds with O atoms of five water molecules and attaches itself to a chain via bonds with three O atoms of the Edta 4− ligands. The Sr(1)-O and Sr(2)-O bond lengths fall in the ranges 2.520(2)–2.656(3) and 2.527(3)–2.683(2) ?, respectively. The Sr(1)-N bonds are 2.702(3) and 2.743(3) ? long. In II and III, the H2 Edta 2− anions have a centrosymmetric structure with the trans configuration of the planar ethylenediamine fragment. The N atoms are blocked by acid protons. In II, the environment of the Sr atom is formed by six O atoms of three H2 Edta ligands, two O atoms of water molecules, and an O atom of the bicarbonate ion, which is disordered over two positions. In III, the environment of the Sr atom includes six O atoms of four H2 Edta 2− ligands and three O atoms of water molecules. The coordination number of the Sr atoms is equal to 8 + 1. In II and III, the main bonds fall in the ranges 2.534(3)–2.732(2) and 2.482(2)–2.746(3) ?, whereas the ninth bond is elongated to 2.937(3) and 3.055(3) ?, respectively. In II, all the structural elements are linked into wavy layers. The O-H…O interactions contribute to the stabilization of the layer and link neighboring layers. In III, hydrated Sr2+ cations and H2 Edta anions form a three-dimensional [Sr2(H2 Edta)(H2O)3] n 2n+ framework. The Cl anions are fixed in channels of the framework by hydrogen bonds with four water molecules. In II and III, the N-H groups form four-center N-H…O3 hydrogen bonds, which include one intermolecular and two intramolecular components. PACS numbers: 61.66.Hq Original Russian Text ? I.N. Polyakova, A.L. Poznyak, V.S. Sergienko, 2009, published in Kristallografiya, 2009, Vol. 54, No. 2, pp. 262–267.  相似文献   

15.
The K2Co(SO4)2 · 6H2O-K2Ni(SO4)2 · 6H2O system has been studied, and a series of K2Ni(SO4)2 · 6H2O/K2Co(SO4)2 · 6H2O bicrystals have been grown. The processes of defect formation at the substrate/layer interface K2Co(SO4)2 · 6H2O/K2Ni(SO4)2 · 6H2O are studied by probe microanalysis, X-ray topography, and optical microscopy. It is found that inclusions and threading dislocations are formed at the interface, due to which elastic stresses relax in the crystal. Nickel is nonuniformly distributed in the layer; its concentration decreases with an increase in the layer thickness, which is indicative of substrate dissolution in the initial stage of interaction. A way for the elastic mismatch stresses to relax in heterostructures of brittle crystals obtained from solutions at low temperatures is proposed which implies the formation of inclusions at the substrate/layer interface. Original Russian Text ? M.S. Grigor’eva, A.é. Voloshin, E.B. Rudneva, V.L. Manomenova, S.N. Khakhanov, V.Ya. Shklover, 2009, published in Kristallografiya, 2009, Vol. 54, No. 4, pp. 679–687.  相似文献   

16.
Abstract  The mononuclear complex [Na(C7H6O4)(H2O)3](C7H5O4) · 2H2O has been synthesized and characterized by IR, single crystal X-ray and thermal analysis. The compound crystallizes in the monoclinic space group P21 with a = 3.623(2) ?, b = 15.872(6) ?, c = 15.650(5) ?, β = 93.13(4)°, V = 896.6(7) ?3 and Z = 2. The central sodium ion is six coordinated with distorted octahedral geometry by two oxygen atoms from two bridging 3,5-dihydroxybenzoate ligands and four ones from different water molecules. The notable feature of the title complex is the formation of a three-dimensional network, through the combination of coordination bonds, hydrogen bonds and π···π interactions. There are one-dimensional channels in the structure, filled in by water molecules. The compound dehydrates in the temperature range of 70–125 °C and then is stable up to 230 °C. Index Abstract  The mononuclear complex [Na(C7H6O4)(H2O)3](C7H5O4) · 2H2O has been synthesized and characterized by IR, single crystal X-ray and thermal analysis.   相似文献   

17.
18.
本文采用固相合成方法制备了Bi4(GexSi1-x)3O12(BGSO)固溶体(x=0~0.4),研究了它的固溶特性和析晶行为。实验结果表明,不同组成混合料在900℃左右固相反应能生成BGSO纯相;XRD分析显示,在x=0~0.4区间内,Bi4Si3O12和Bi4Ge3O12可以完全互溶,其晶格常数随x的增加呈线性增长。采用坩埚下降法生长了x=0.15组成的BGSO混晶,获得了透明晶体,并测试了晶体的光学性能。  相似文献   

19.
MnBi2Te4是首次被发现的一种本征磁性拓扑绝缘体,具有重要的研究意义。本文通过在MnBi2Te4晶体中进行稀土元素掺杂,合成了Er掺杂MnBi2Te4晶体,Er原子进入晶格并取代Mn位。在晶体制备过程中,考虑到目前晶体制备工艺周期较长,生成物存在Bi2Te3助熔剂等杂质的问题,对晶体制备工艺进行了优化探索。XRD测试结果表明,利用改进工艺制备的Er掺杂MnBi2Te4晶体结晶性能良好,不含杂质相。磁电输运测量结果显示,少量Er掺杂MnBi2Te4晶体的磁性增强,掺杂样品在25.2 K发生反铁磁相变。使用原子力显微镜对Er掺杂MnBi2Te4晶体层间距进行了研究,发现层间距为单层MnBi2Te4的整数倍。通过拉曼测试研究了Er掺杂MnBi...  相似文献   

20.
Compounds K2[UO2(C3H2O4)2] · H2O (I) and Rb2[UO2(C3H2O4)2] · H2O (II) are synthesized and their crystal structures are determined by X-ray diffraction. The compounds crystallize in the monoclinic crystal system; for I, a = 7.1700(2) ?, b =12.3061(3) ?, c = 14.3080(4) ?, β = 95.831(2)°, space group P21/n, Z = 4, and R = 0.0275; for II, a = 7.1197(2) ?, b = 12.6433(4) ?, c = 14.6729(6) ?, β = 96.353(2)°, space group P21/n, Z = 4, and R = 0.0328. It is found that I and II are isostructural. The main structural units of the crystals are the [UO2(C3H2O4)2]2− chains, which belong to the AT 11 B 01 (A = UO22+, T 11, and B 01 = C3H2O42−) crystal chemical group of uranyl complexes. The chains and alkali metal ions R (R = K or Rb) are connected by electrostatic interactions and hydrogen bonds. Some specific structural features of [UO2(C3H2O4)2]2− complex groups are discussed.  相似文献   

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