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1.
The crystal structure of [Ni(C5H2N2O4)(2, 2?-bipy)(H2O)2]·2H2O 1 has been determined by X-ray diffraction. Crystal data: triclinic system, space group P ī with a = 7.9424(3), b = 9.9417(3), c = 12.1867(3) (A。), α = 84.771(1), β = 77.375(2), γ = 68.993(2)°, C15H18N4O8Ni, Mr = 440.7, V = 876.16(5) (A。)3, Z = 2, Dc = 1.672 g/cm3, F(000) = 456, ((MoK() = 1.162 mm-1, the final R = 0.0464 and wR = 0.1055 for 3026 observed reflections with I > 2((I). In the title compound, the nickel ion is coordinated by a nitrogen atom and an oxygen atom from the orotate ligand, two nitrogen atoms from 2, 2'-bipy and two oxygen atoms from the coordinated water molecules in a distorted octahedral geometry. The presence of intermolecular hydrogen bonding and (-( stacking interaction of aromatic rings from 2, 2'-bipy results in a 3D structure.  相似文献   

2.
Xiaoyan You  Lixia Zhu  Jia Sun 《中国化学》2010,28(11):2174-2178
A novel organically templated copper pentaborate, [Cu(C3N2H4)4][Cu(CH3COO)2(C3N2H4)2(H2O)2]‐ [B5O6(OH)4]2, was synthesized by hydrothermal reaction and characterized by elemental analysis, single‐crystal X‐ray diffraction, FT‐IR spectroscopy, Raman spectroscopy and TGA. The crystal structure of this compound consists of two copper‐centered polyhedra and two discrete [B5O6(OH)4]? pentaborate anions, which are linked together through intensive hydrogen bonding interactions, forming a 3D framework with large channels along c axis. The discrete pentaborate anions form infinite layers by hydrogen bonds. Moreover, the two crystallographically different octahedral coppers are connected by common oxygen atom to form an infinite chain.  相似文献   

3.
The templated borate, [C9H14N] · [B5O6(OH)4], was synthesized under hydrothermal conditions. Single crystal X‐ray diffraction techonology reveals that it crystallizes in the triclinic system, space group P$\bar{1}$ (No. 2). The material was also characterized by element analysis, Fourier transform infrared spectroscopy (FTIR), powder X‐ray diffraction (PXRD), thermogravimetric and differential thermal analysis (TG‐DTA), and luminescence spectroscopy. The compound consisted of isolated pentaborate [B5O6(OH)4] and N‐butylpyridinium cations [C9H14N]+. The [B5O6(OH)4] anions are connected together by hydrogen bonds to form a three‐dimensional framework, in which [C9H14N]+ cations are located in. [C9H14N] · [B5O6(OH)4] exhibits tunable luminescence emission at 415–458 nm by means of heating treatment from 100 to 300 °C.  相似文献   

4.
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   

5.
The reaction of UO2(ClO4nH2O with 15-crown-5 and 18-crown-6 in acetonitrile yielded the title complexes. [UO2(OH2)5] [ClO4]2·3(15-crown-5)·CH3CN crystallizes in the triclinic space groupPT with (at–150°C)a=8.288(6),b=12.874(7),c=24.678(7) Å, =82.62(4), =76.06(5), =81.06(5)°, andD calc=1.67 g cm–3 forZ=2 formula units. Least-squares refinement using 6248 independent observed reflections [F o5(F o)] led toR=0.111. [UO2(OH2)5] [ClO4]2·2(18-crown-6)·2CH3CN·H2O is orthorhombicP212121 with (at–150 °C)a=12.280(2),b=17.311(7),c=22.056(3) Å,D calc=1.68 g cm–3,Z=4, andR=0.032 (3777 observed reflections). In each complex the crown ether molecules are hydrogen bonded to the water molecules of the pentagonal bipyramidal [UO2(OH2)5]2+ ions, each crown ether having exclusive use of two hydrogen atoms from one water molecule and one hydrogen from another water molecule. In the 15-crown-5 complex the remaining hydrogen bonding interaction is between one of the water molecules and one of the perchlorate anions. The solvent molecule has a close contact between the methyl group and a perchlorate anion suggesting a weak interaction. There are a total of three U-OH...OClO3 hydrogen bonds to the two perchlorate anions in [UO2(OH2)5] [ClO4]2·(18-crown-6)·2CH3CN ·H2O. The remaining coordinated water hydrogen bond is to the uncoordinated 2H2O molecule, which in turn is hydrogen bonded to a perchlorate oxygen atom and an acetonitrile nitrogen atom. One solvent methyl group interacts with an anion, the other with one of the 18-crown-6 molecules. Unlike the 15-crown-5 structure, the hydrogen bonding in this complex results in a polymeric network with formula units joined by hydrogen bonds from one of the solvent molecules and the uncoordinated water molecule. Supplementary data relating to this article are deposited with the British Library as Supplementary Publication No. SUP 82051 (37 pages).For Part 10, see reference [1].  相似文献   

6.
Colourless triclinic single crystals of Na4(NH4)2[TeMo6O24] · 16H2O were grown in aqueous solution (space group P1 , a = 1 075.3(1), b = 1 074.2(1), c = 1 089.8(1) pm, = 96.259(9), β = 118.556(7), γ = 113.355(8)°, Z = 1, 295 K, 311 parameters, 3 689 reflections, Rg = 0.0197). There are two crystallographically independent Na+ cations. Na(1) is coordinated octahedrally by four water molecules and two oxygen atoms of the centrosymmetric [TeMo6O24]6? anion. Na(2) is bound to five water molecules in a considerably distorted trigonally bipyramidal fashion. These bipyramids are linked with NH4+ by hydrogen bonds to yield centrosymmetric cluster cations consisting of two NH4+ and two Na(H2O)5+ each. Hydrogen bonds envolving all except one (O(10)) of the oxygen atoms of the [TeMo6O24]6? anion as almost equivalent proton acceptors regardless of their bonding mode to Te and Mo, respectively, establish further connections to NH4+ and the water of crystallization.  相似文献   

7.
1 INTRODUCTION Orotic acid (H3dtpc), an important pyrimidine derivative as the effective precursor in the biosynthesis of pyrimidine base of nucleic acids in living organisms, plays a unique role in bioinorganic and pharmaceutical. Aside from the biological interest, orotic acid is also interesting in coordination chemistry. Its ketonic and enolic tautomers along with asymmetric geometry make it to be a very good versatile polydentate ligand[1~5]. The incorporation of metals into supram…  相似文献   

8.
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   

9.
Li6[TeMo6O24] · 18 H2O is triclinic (space group P1 , a = 1 041.7(1), b = 1 058.6(1), c = 1 070.8(1) pm, α = 61.08(1), β = 60.44(1), γ = 73.95(1)°). Single crystal X-ray structure analysis (Z = 1, 295 K, 317 parameters, 3 973 reflections, Rg = 0.0250) revealed an infinite branched chain of edge-sharing Li coordination polyhedra to be the prominent structural feature. One of the four crystallographically independent Li+ is coordinated octahedrally. The coordination polyhedra of the remaining Li+ are distorted trigonal bipyramids. Only three unique oxygen atoms (O(9), O(10), O(12)) of the centrosymmetric [TeMo6O24]6? anion are bound to Li+. The further positions in the coordination spheres of the Li+ are occupied by water molecules. Intermolecular hydrogen bonds involve mainly oxygen atoms of the [TeMo6O24]6? anion as nearly equivalent proton acceptors without regard to their different bonding modes to Te and Mo, respectively. Li6[TeMo6O24] · Te(OH)6 · 18 H2O crystallizes monoclinically in space group P21/n with Z = 4, a = 994.1(3), b = 2 344.8(10), c = 1 764.9(4) pm, and β = 91.36(4)°. Single crystal structure analysis with least squares refinement of 627 parameters (5 900 reflections, 295 K) converged to Rg = 0.0324. There are six unique Li+ cations. The coordination polyhedra of Li(1), Li(2), Li(3), and Li(4) are linked by common edges to yield an eight membered centrosymmetric strand. The coordination polyhedra of the remaining two Li+ sites (Li(5), Li(6)) are connected to a dimeric unit via a common corner. All oxygen atoms of the Te(OH)6 molecule are involved in the coordination of Li+. However, only three oxygen atoms (O(13), O(18), O(23)) of the [TeMo6O24]6? anion which lacks crystallographic symmetry are involved in the coordination of Li+. The oxygen atoms of the anion act as proton acceptors in hydrogen bonds of predominantly medium strength. Te(OH)6 molecules and [TeMo6O24]6? anions connected by strong hydrogen bonds form an infinite chain.  相似文献   

10.
A novel tetramethylammonium aluminosilicate hydrate with the approximate composition [NMe4]6[AlxSi8?xO18?x(OH)2+x] · 44H2O (x = 3–4) has been identified by powder X-ray diffraction as a component in a polyphasic solid mixture which crystallized at room temperature from an aqueous NMe4OH? Al2O3? SiO2 solution. Large crystals of the novel hydrate phase could be mechanically selected from that mixture. The crystal structure has been determined from 1 196 unique MoKα diffraction data measured at 180 K: Tetragonal crystal system, cell constants a = 16.181(4) and c = 17.450(4) Å, space group P4/mnc with Z = 2 formula units per unit cell, R = 0.072. The host-guest compound is of polyhedral clathrate type with a mixed three-dimensional, (mainly) four-connected network composed of oligomeric aluminosilicate anions [AlxSi8?xO18?x(OH)2+x]6? and H2O molecules linked via hydrogen bonds O? H …? O. The aluminosilicate anions possess a cube-shaped (double four-ring) structure. Orientationally disordered cationic guest species NMe4+ are enclosed in the large [4668] and [4151067] polyhedral voids of the host framework; the small [46] cages (i.e. the double four-ring anions) and [4356] cages are empty. The hydrate is a further member in a recently discovered series of clathrates with mixed tetrahedral networks, which provides a structure-chemical link between zeolite- and clathrate hydrate-type host-guest compounds.  相似文献   

11.
利用水热法合成了五硼酸三乙胺[HN(C2H5)3][B5O6(OH)4], 并利用单晶X射线衍射技术解析了其结构, 同时利用傅立叶红外分析、元素分析及热分析技术加以佐证. 该化合物属于单斜晶系, 其空间群为P21/c, 相应的晶胞参数为a=1.0036(2) nm, b=1.1353(2) nm, c=1.4843(3) nm和β=106.54(3)°. 它由孤立的五硼酸阴离子[B5O6(OH)4]-和三乙胺阳离子[HN(C2H5)3]+构成. 五硼酸阴离子[B5O6(OH)4]-通过氢键构成三维网状结构, [HN(C2H5)3]+位于其中的孔道中.  相似文献   

12.
13.
The reaction of Ru3(CO)12 with tetramethyltrifluoromethylcyclopentadiene at various ratios of the reagents was studied. Refluxing of Ru3(CO)12 with a sixfold excess of tetramethyltrifluoromethylcyclopentadiene in octane in an inert atmosphere gave a complex, which is, according to X-ray diffraction data, a dimer,trans-[Ru(η5-C5Me4CF3)(CO)2]2. The reaction under the same conditions but starting from Ru3(CO)12 and C5Me4CF3H in 2∶1 molar ratio gave a hexaruthenium cluster [Ru63-H)(η24-CO)2(μ-CO)(Co)125-C5Me4CF2)], which was characterized by IR as well as1H,13C, and19F NMR spectroscopy. According to X-ray diffraction data, an Ru4 tetrahedron, in which two edges are bound by additional “briding” Ru atoms, constitutes the frame of this compound. This complex has one (η5-C5Me4CF3) ligand, as well as one (μ3-H) and two (η24-CO) groups. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 3, pp. 507–512, March, 1998.  相似文献   

14.
利用三苯基氯化锡和对苯二甲酸二钠、哌嗪荒酸二钠在甲醇中反应 ,合成了双核有机锡 (Ⅳ )配合物 [Ph3 Sn (CH3 OH)O2 CC6H4 CO2 (CH3 OH)SnPh3 ]·2CH3 OH (1)和 [Ph3 SnS2 CN(CH2 CH2 ) 2 NCS2 SnPh3 ]·2CH3 OH (2 ) .通过元素分析、红外光谱和核磁共振氢谱对其结构进行了表征 .用X射线单晶衍射测定了这两个化合物的晶体结构 .化合物 1为单斜晶系 ,空间群P2 1/n ,a =1.5 199(5 )nm ,b =0 .90 0 0 (3)nm ,c =1.82 0 6 (6 )nm ,β =113.970 (5 )° ,Z =2 ,V =2 .2 75 5(13)nm3 ,Dc=1.413g/cm3 ,μ =1.146mm-1,F(0 0 0 ) =980 ,R1=0 .0 35 3,wR2 =0 .0 6 0 6 .化合物 2为单斜晶系 ,空间群P2 1/c,a =1.5 0 6 6 (5 )nm ,b =1.0 875 (4 )nm ,c =1.35 42 (5 )nm ,β =91.6 14(5 )°,Z =2 ,V =2 .2 178(14)nm3 ,Dc=1.498g/cm3 ,μ =1.35 1mm-1,F(0 0 0 ) =10 0 8,R1=0 .0 40 1,wR2 =0 .1148.在 1和 2的晶体中 ,锡原子呈五配位畸变三角双锥构型 .配合物 1由未配位的甲醇分子通过氢键作用形成二维网状结构  相似文献   

15.
The crystal structures of diphenyl (cycloheptylamido)phosphate, C19H24NO3P or (C6H5O)2P(O)(NHC7H13), ( I ), and diphenyl (dibenzylamido)phosphate, C26H24NO3P or (C6H5O)2P(O)[N(CH2C6H5)2], ( II ), are reported. The NHC7H13 group in ( I ) provides two significant hydrogen‐donor sites in N—H…O and C—H…O hydrogen bonds, needed for a one‐dimensional hydrogen‐bond pattern along [100] in the crystal, while ( II ), with a (C6H5CH2)2N moiety, lacks these hydrogen bonds, but its three‐dimensional supramolecular structure is mediated by C—H…π interactions. The conformational behaviour of the phenyl rings in ( I ), ( II ) and analogous structures from the Cambridge Structural Database (CSD) were studied in terms of flexibility, volume of the other group attached to phosphorus and packing forces. From this study, synclinal (±sc), anticlinal (±ac) and antiperiplanar (±ap) conformations were found to occur. In the structure of ( II ), there is an intramolecular Cortho—H…O interaction that imposes a +sc conformation for the phenyl ring involved. For the structures from the CSD, the +sc and ±ap conformations appear to be mainly imposed by similar Cortho—H…O intramolecular interactions. The large contribution of the C…H/H…C contacts (32.3%) in the two‐dimensional fingerprint plots of ( II ) is a result of the C—H…π interactions. The differential scanning calorimetry (DSC) analyses exhibit peak temperatures (Tm) at 109 and 81 °C for ( I ) and ( II ), respectively, which agree with the strengths of the intermolecular contacts and the melting points.  相似文献   

16.
Alkaline Molybdotellurates: Preparation and Crystal Structures of Rb6[TeMo6O24] · 10H2O and Rb6[TeMo6O24] · Te(OH)6 · 6H2O Single crystals of Rb6[TeMo6O24] · 10 H2O and Rb6[TeMo6O24] · Te(OH)6 · 6 H2O, respectively, were grown from aqueous solution. Rb6[TeMo6O24] · 10 H2O possesses the space group P1 . The lattice dimensions are a = 963.40(13), b = 972.56(12), c = 1 056.18(13) pm, α = 97.556(10), β = 113.445(9), γ = 102.075(10)°; Z = 1, 2 860 reflections, 215 parameters refined, Rg = 0.0257. The centrosymmetrical [TeMo6O24]6? anions are stacked parallel to [010]. Rb(2) is coordinated with one exception by water molecules only. Folded chains consisting of [TeMo6O24]6? anions and Rb(2) coordination polyhedra which are linked to pairs represent the prominent structural feature. Rb6[TeMo6O24] · Te(OH)6 · 6 H2O crystallizes monoclinically in the space group C2/c with a = 1 886.4(3), b = 1 000.9(1), c = 2 126.5(3) pm, and β = 115.90(1)°; Z = 4, 3 206 reflections, 240 parameters refined, Rg = 0.0333. It is isostructural in high extent with (NH4)6[TeMo6O24] · Te(OH)6 · 7 H2O. Hydrogen bonds between Te(OH)6 molecules and [TeMo6O24]6? anions establish infinite strands. The [TeMo6O24]6? anions gather around Te(OH)6 providing channel-like voids extending parallel to [001].  相似文献   

17.
The crystal structures of three new diaqua-tetrafluoro-manganate(III) compounds with different organic N-cations have been determined: 2-picoH[MnF4(H2O)2] 1 (2-pico = 2-methyl-pyridine), space group P21/c, a = 9.439, b = 13.662, c = 7.641 Å, β = 91.31°; R = 0.059; TMEDAH2[MnF4(H2O)2]2 2 (TMEDA = N,N,N′,N′-tetramethyl ethane diamine), space group P21/c, a = 5.421, b = 15.970, c = 9.677 Å, β = 96.37°, R = 0.031, and TMBDAH2[MnF4(H2O)2]2 3 (TMBDA = N,N,N′,N′-tetramethyl-1,4-butane-diamine), space group P21/n, a = 12.631, b = 5.577, c = 12.976 Å, β = 98.10°, R = 0.040. All three compounds show 2 D H-bonding networks of [MnF4(H2O)2] anions separated by the organic cations. However, the topology of the anionic H-bonding nets is different for each compound. The anions are strongly elongated by the Jahn-Teller effect and are arranged in a ferrodistortive way in compounds 1 and 2 , whereas in compound 3 the arrangement is described as in a herringbone-like antiferrodistortive variant.  相似文献   

18.
nBu2Sn[O2CCH2CH(4-ClC6H4)Ge(OCH2CH2)3N]2.H2O(Mr=1053.66) is an air-stable compound which crystallizes in the monoclinic space group C2/c with a=21.182(5), b=12.174(3), c=17.108(4) , β=99.59(2)°, V=4350(3) 3, Z=4, F(000)=2104, μ=2.104 mm-1. The refinement of structure with I≥3σ(I) for 1819 reflections converged at R=0.045. The coordination geometry around the Sn atom is best described as an askew-pentagonal bipyramid, in which four carboxylate oxygen atoms( Sn(1)-O(5), Sn(1)-O(5a)=2.099 and Sn(1)-O(4), Sn(1)-O(4a)=2.158 ) and an oxygen atom from an aqua ligand comprise the pentagonal plane, with two butyl groups occupying axial positions.  相似文献   

19.
合成了一个新配合物[Mn(napn)(CH3OH)2]ClO4 (C26H26 Cl N2O8Mn,Mr = 584.88,H2napn = 双a-萘酚醛缩乙二胺),并测定了其晶体结构。晶体属于三斜晶系,空间群P ,a = 7.813(1),b = 13.025(2),c = 14.089(2) ? = 64.89(3), = 83.98(3), = 78.11(3)海琕 = 1270.16 ?,Z = 2, Dc = 1.529 g/cm3, F(000) = 604, R = 0.0837, wR = 0.1636。锰(Ⅲ)离子的配位构型为拉长的八面体。Schiff碱配体napn2-中的N2O2在赤道平面与锰(Ⅲ)形成四配位,2个CH3OH中的O原子分别在赤道平面两侧轴向位置与锰(Ⅲ)配位。由于Jahn-Teller效应,轴向上的MnO平均键长为2.52 拧A硗猓О写嬖诜肿幽诤头肿蛹淝饧?  相似文献   

20.
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