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1.
The heteropolytungstate (NH4)20[Na2(H2O)2Ni(H2O)5{Ni(H2O)}2As4W40O140] · 61H2O is obtained by the reaction of Na27[NaAs4W40O140] · 60H2O with NiCl2 · 6H2O and NH4Cl in pH≈4.0. The structure and chemical composition are determined by X-ray diffraction analysis and element analysis. The crystal data and main structure refinement are: a = 1.33135(18) nm, b = 1.9722(3) nm, c = 3.6430(5) nm, α = 78.010(2)°, β = 82.145(2)δ, γ = 74.385(2)°, V = 8.978(2) nm3, triclinic crystal system, space group: P1, Z = 2, R1 = 0.0512, and wR2 = 0.0684(I >2σ). The four S2 sites of the big cyclic ligand [As4W40O140]28- are occupied by two Na+ and two Ni2+ respectively, and each site supplies four Od coordinating to metal ion. The coordination number of Ni2+ is six, and that of two Na+ is five and six respectively. The third Ni2+ locates outside the cyclic [As4W40O140]28- and connects with one Od, and its coordination number is six. 相似文献
2.
The heteropolytungstate Na9[{Na(H2O)2}3{Cu(H2O)}3(BiW9O33) 42H2O is obtained by the reaction of Na2WO4·2H2O, Bi(NO3)3 · 5H2O with CuCl2 · 2H2O at pH≠6. The structure and chemical composition are determined by X‐ray diffraction analysis and elemental analysis. The crystal data and main structure refinement are: a = 1.410(3) nm, b=2.338(5) nm, c=3.173(6) nm, β=98.06(4)°. V= 10.354(35) nm3. monoclinic crystal system, space group: C2/c, Z = 4, R1= 0.0471. wR2 = 0.0642 I>2σ(I)]. R1= 0.1371, wR2 = 0.0868 (all data). [(Na(H2O)2}3{Cu(H2O)}3W9O33)2]9– has D34 symmetry. IR, UV‐vis spectra, TG curve and magnetic property of the complex were also discussed. The compound exhibits an antiferromagnetic coupling with J= ‐8.08 cm?1 and g =2.21. 相似文献
3.
Reactions of 1,10‐phenanthroline monohydrate, Na2C4H4O4 · 6 H2O and MnSO4 · H2O in CH3OH/H2O yielded a mixture of [Mn2(H2O)4(phen)2(C4H4O4)2] · 2 H2O ( 1 ) and [Mn(phen)2(H2O)2][Mn(phen)2(C4H4O4)](C4H4O4) · 7 H2O ( 2 ). The crystal structure of 1 (P1 (no. 2), a = 8.257(1) Å, b = 8.395(1) Å, c = 12.879(2) Å, α = 95.33(1)°, β = 104.56(1)°, γ = 106.76(1)°, V = 814.1(2) Å3, Z = 1) consists of the dinuclear [Mn2(H2O)4(phen)2(C4H4O4)2] molecules and hydrogen bonded H2O molecules. The centrosymmetric dinuclear molecules, in which the Mn atoms are octahedrally coordinated by two N atoms of one phen ligand and four O atoms from two H2O molecules and two bis‐monodentate succinato ligands, are assembled via π‐π stacking interactions into 2 D supramolecular layers parallel to (101) (d(Mn–O) = 2.123–2.265 Å, d(Mn–N) = 2.307 Å). The crystal structure of 2 (P1 (no. 2), a = 14.289(2) Å, b = 15.182(2) Å, c = 15.913(2) Å, α = 67.108(7)°, β = 87.27(1)°, γ = 68.216(8)°, V = 2934.2(7) Å3, Z = 2) is composed of the [Mn(phen)2(H2O)2]2+ cations, [Mn(phen)2(C4H4O4)] complex molecules, (C4H4O4)2– anions, and H2O molecules. The (C4H4O4)2– anions and H2O molecules form 3 D hydrogen bonded network and the cations and complex molecules in the tunnels along [001] and [011], respectively, are assembled via the π‐π stacking interactions into 1 D supramolecular chains. The Mn atoms are octahedrally coordinated by four N atoms of two bidentate chelating phen ligands and two water O atoms or two carboxyl O atoms (d(Mn–O) = 2.088–2.129 Å, d(Mn–N) = 2.277–2.355 Å). Interestingly, the succinato ligands in the complex molecules assume gauche conformation bidentately to chelate the Mn atoms into seven‐membered rings. 相似文献
4.
Reactions of a freshly prepared Zn(OH)2‐2x(CO3)x · yH2O precipitate, phenanthroline with azelaic and sebacic acid in CH3OH/H2O afforded [Zn(phen)(C9H15O4)2] ( 1 ) and [Zn2(phen)2(H2O)2(C10H16O4)2] · 3H2O ( 2 ), respectively. They were structurally characterized by X‐ray diffraction methods. Compound 1 consists of complex molecules [Zn(phen)(C9H15O4)2] in which the Zn atoms are tetrahedrally coordinated by two N atoms of one phen ligand and two O atoms of different monodentate hydrogen azelaato groups. Intermolecular C(alkyl)‐H···π interactions and the intermolecular C(aryl)‐H···O and O‐H···O hydrogen bonds are responsible for the supramolecular assembly of the [Zn(phen)(C9H15O4)2] complexes. Compound 2 is built up from crystal H2O molecules and the centrosymmetric binuclear [Zn2(phen)2(H2O)2(C10H16O4)2] complex, in which two [Zn(phen)(H2O)]2+ moieties are bridged by two sebacato ligands. Through the intermolecular C(alkyl)‐H···O hydrogen bonds and π‐π stacking interactions, the binuclear complex molecules are assembled into layers, between which the lattice H2O molecules are sandwiched. Crystal data: ( 1 ) C2/c (no. 15), a = 13.887(2), b = 9.790(2), c = 22.887(3)Å, β = 107.05(1)°, U = 2974.8(8)Å3, Z = 4; ( 2 ) P1¯ (no. 2), a = 8.414(1), b = 10.679(1), c = 14.076(2)Å, α = 106.52(1)°, β = 91.56(1)°, γ = 99.09(1)°, U = 1193.9(2)Å3, Z = 1. 相似文献
5.
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
6.
The Lanthanum Dodecahydro‐closo‐Dodecaborate Hydrate [La(H2O)9]2[B12H12]3·15 H2O and its Oxonium‐Chloride Derivative [La(H2O)9](H3O)Cl2[B12H12]·H2O By neutralization of an aqueous solution of the free acid (H3O)2[B12H12] with basic La2O3 and after isothermic evaporation colourless, face‐rich single crystals of a water‐rich lanthanum(III) dodecahydro‐closo‐dodecaborate hydrate [La(H2O)9]2[B12H12]3·15 H2O are isolated. The compound crystallizes in the trigonal system with the centrosymmetric space group (a = 1189.95(2), c = 7313.27(9) pm, c/a = 6.146; Z = 6; measuring temperature: 100 K). The crystal structure of [La(H2O)9]2[B12H12]3·15 H2O can be characterized by two of each other independent, one into another posed motives of lattice components. The [B12H12]2− anions (d(B–B) = 177–179 pm; d(B–H) = 105–116 pm) are arranged according to the samarium structure, while the La3+ cations are arranged according to the copper structure. The lanthanum cations are coordinated in first sphere by nine oxygen atoms from water molecules in form of a threecapped trigonal prism (d(La–O) = 251–262 pm). A coordinative influence of the [B12H12]2− anions on La3+ has not been determined. Since “zeolitic” water of hydratation is also present, obviously the classical H–Oδ–···+δH–O‐hydrogen bonds play a significant role in the stabilization of the crystal structure. During the conversion of an aqueous solution of (H3O)2[B12H12] with lanthanum trichloride an anion‐mixed salt with the composition [La(H2O)9](H3O)Cl2[B12H12]·H2O is obtained. The compound crystallizes in the hexagonal system with the non‐centrosymmetric space group (a = 808.84(3), c = 2064.51(8) pm, c/a = 2.552; Z = 2; measuring temperature: 293 K). The crystal structure can be characterized as a layer‐like structure, in which [B12H12]2− anions and H3O+ cations alternate with layers of [La(H2O)9]3+ cations (d(La–O) = 252–260 pm) and Cl− anions along [001]. The [B12H12]2− (d(B–B) = 176–179 pm; d(B–H) = 104–113 pm) and Cl− anions exhibit no coordinative influence on La3+. Hydrogen bonds are formed between the H3O+ cations and [B12H12]2− anions, also between the water molecules of [La(H2O)9]3+ and Cl− anions, which contribute to the stabilization of the crystal structure. 相似文献
7.
The synthesis and the structural characterization of the title compound H2Na3[W3O(CCH3)-(O2CCH3)6(H2O)3][H2W12O40]·13.5H2O are described. It is known that the mixed oxo-ethylidynecapped tritungsten cluster can be obtained by Zn dust reduction of Na2WO4·2H2O in acetic anhydride. The title compound has been characterized by X-ray diffraction, UV/VIS and 1H NMR spectra. The tungsten atoms in the cluster cation and anion are in the oxidation states of W(IV) and W(VI) respectively. The crystal is rhombohedral with the space group R32, a = 17.058 (3)Å, c = 49.665 (9)Å, γ=120°, V=12516(9)Å3, Z=6, final R = 0.037 for 2071 reflections with I ≥3σ (I). Both the cluster cation and anion have a C3 symmetry. The important interatomic distances in angstroms for the cluster cation are: W—W, 2.730(2); W—μ3?O, 2.00; W—O (carboxy1), 2.12; W—Ot 2.18 (2). 相似文献
8.
Three new alkali metal transition metal sulfate‐oxalates, RbFe(SO4)(C2O4)0.5 · H2O and CsM(SO4)(C2O4)0.5 · H2O (M = Mn, Fe) were prepared through hydrothermal reactions and characterized by single‐crystal X‐ray diffraction, solid state UV/Vis/NIR diffuse reflectance spectroscopy, infrared spectra, thermogravimetric analysis, and powder X‐ray diffraction. The title compounds all crystallize in the monoclinic space group P21/c (no. 14) with lattice parameters: a = 7.9193(5), b = 9.4907(6), c = 8.8090(6) Å, β = 95.180(2)°, Z = 4 for RbFe(SO4)(C2O4)0.5 · H2O; a = 8.0654(11), b = 9.6103(13), c = 9.2189(13) Å, β = 94.564(4)°, Z = 4 for CsMn(SO4)(C2O4)0.5 · H2O; and a = 7.9377(3), b = 9.5757(4), c = 9.1474(4) Å, β = 96.1040(10)°, Z = 4 for CsFe(SO4)(C2O4)0.5 · H2O. All compounds exhibit three‐dimensional frameworks composed of [MO6] octahedra, [SO4]2– tetrahedra, and [C2O4]2– anions. The alkali cations are located in one‐dimensional tunnels. 相似文献
9.
IntroductionMolecularpolymerwithonedimensionalormultidimen sionalstructureassemblingthroughhydrogenbondsisanim portantresearchcontentinthesupramolecularchemistryandcrystalenginnering .1,2 Withthedevelopmentofnewtypefunctionalmaterialssuchasmolecularmagnetic ,selectedcatalysis ,reversiblecatalysis ,reversiblehost guestmolecular(ion)exchangeetc.,3themoleculardesignandsynthesishavealreadyattractedconsiderableattentioninsupramolecu larsystem .Thesupramolecularcomplexesandorganiccom poundscontainin… 相似文献
10.
Hydrothermal investigations in the system MgO/B2O3/P2O5(/H2O) yielded two new magnesium borophosphates, Mg2(H2O)[BP3O9(OH)4] and Mg(H2O)2[B2P2O8(OH)2]·H2O. The crystal structures were solved by means of single crystal X‐ray diffraction. While the acentric crystal structure of Mg2(H2O)[BP3O9(OH)4] (orthorhombic, P212121 (No. 19), a = 709.44(5) pm, b = 859.70(4) pm, c = 1635.1(1) pm, V = 997.3(3) × 106 pm3, Z = 4) contains 1D infinite chains of magnesium coordination octahedra interconnected by a borophosphate tetramer, Mg(H2O)2[B2P2O8(OH)2]·H2O (monoclinic, P21/c (No. 14), a = 776.04(5) pm, b = 1464.26(9) pm, c = 824.10(4) pm, β = 90.25(1)°, V = 936.44(9) × 106 pm3,Z = 4) represents the first layered borophosphate with 63 net topology. The structures are discussed and classified in terms of structural systematics. 相似文献
11.
Reaction of CuCl2 · 2H2O, phenanthroline, maleic acid and NaOH in CH3OH/H2O (1:1 v/v) at pH = 7.0 yielded blue {[Cu(phen)]2(C4H2O4)2} · 4.5H2O, which crystallizes in the monoclinic space group C2/c (no. 15) with cell dimensions: a = 18.127(2)Å, b = 12.482(2)Å, c = 14.602(2)Å, β = 103.43(1)°, U = 3213.5(8)Å3, Z = 4. The crystal structure consists of the centrosymmetric dinuclear {[Cu(phen)]2(C4H2O4)2} complex molecules and hydrogen bonded H2O molecules. The Cu atoms are each square‐pyramidally coordinated by two N atoms of one phen ligand and three carboxyl O atoms of two maleato ligands with one carboxyl O atom at the apical position (d(Cu‐N) = 2.008, 2.012Å, equatorial d(Cu‐O) = 1.933, 1.969Å, axial d(Cu‐O) = 2.306Å). Two square‐pyramids are condensed via two apical carboxyl O atoms with a relatively larger Cu···Cu separation of 3.346(1)Å. The dinuclear complex molecules are assembled via the intermolecular π—π stacking interactions into 1D ribbons. Crossover of the resulting ribbons via interribbon π—π stacking interactions forms a 3D network with the tunnels occupied by H2O molecules. The title complex behaves paramagnetically between 5—300 K, following the Curie‐Weiss law χm(T—θ) = 0.435 cm3 · mol—1 · K with θ = 1.59 K. 相似文献
12.
Annika Arndt Damir Posavec Stefan Schwarzer Mathias S. Wickleder Prof. Dr. 《无机化学与普通化学杂志》2008,634(3):431-435
The reaction of the nitrates M(NO3)3·6H2O (M = La, Pr) and (H3O)2PtCl6 led to yellow single crystals of [M(NO3)2(H2O)6]2[PtCl6]·2H2O (M = La, Pr) (monoclinic, P21/c, Z = 2, La/Pr: a = 697.4(3)/695.5(1), b = 1654.5(1)/1652.5(2), c = 1317.7(6)/1318.5(3) pm, β = 93.97°(7)/93.93°(2), Rall = 0.0169/0.0659) while the reaction of M(NO3)3·5H2O (M = Gd, Dy) and (H3O)2PtCl6 yielded yellow single crystals of [M(NO3)(H2O)7][PtCl6]·4H2O (monoclinic, P21/n, Z = 4, Gd/Dy: a = 838.72(3)/838.40(2), b = 2131.98(6)/2139.50(7), c = 1142.63(3)/1143.10(3) pm, β = 95.670(4)/95.698(3), Rall = 0.0475/0.0337). The crystal structures consist of octahedral [PtCl6]2? anions and complex [M(NO3)2(H2O)6]2+ and [M(NO3)(H2O)7]2+ cations, respectively. The thermal decomposition of both types of compounds leads via various steps to elemental platinum and the oxide chlorides MOCl (M = La, Pr, Gd, Dy). 相似文献
13.
Blue needle—shaped crystals of [Cu(bpy)(H2O)2(C4H4O4)]· 2H2O were obtained by slow evaporation of a methanolic aqueous solution containing a fresh Cu(C4H4O4)· 2H2O precipitate, 4, 4′—bipyridine, and ammonia. Within the complex, the six—coordinated Cu atoms are linked by bis—monodentate gauche succinate anions into chains propagating helically around the [001] axis. The chains are interconnected by 4, 4′—bipyridine ligands into a 3D framework with the crystal H2O molecules located in the channels along the [100], [010] and [110] directions. The Cu2+ ions are in distorted octahedral coordination of two nitrogen and four oxygen atoms (equatorial bonds: Cu—N 1.986(5), 2.015(5)Å; Cu—O 1.950(6), 1.954(6)Å; axial bonds Cu—O: 2.524(9), 2.539(8)Å). Furthermore, the thermal and magnetic behavior of the compound will be discussed. Crystal data: hexagonal, P61 (no. 169), a = 11.066(2)Å, c = 24.965(5)Å, V = 2647.5(8)Å3, Z = 6, R = 0.0528 and wR2 = 0.1103 for 1426 observed reflections (Fo2 > 2σ(Fo2)) out of 2170 unique reflections. 相似文献
14.
《Journal of Coordination Chemistry》2012,65(1):83-92
Abstract The heterometallic polymeric cluster Na2[AlW3O4 (O2CEt)8]2 (1) has been prepared by reaction of W(CO)6 and NaWO4·2H2O with AlCl3 at 120°C in propionic anhydride and characterized by X-ray crystallography, with the following crystal data: triclinic, space group P1, a = 12.205(5), b = 13.032(4), c = 13.925(3) Å, α = 90.21(3)°, β = 109.53(5)°, γ = 117.26(6)°, V = 1822.8(1)Å3, Z = 1, R = 0.038 and Rw = 0.101. The structure consists of two triangular [W3O4(O2CEt)8]4? cluster unit, which act as polydenate ligands to link Al3+ and Na+ ions forming a one–dimensional chain structure. IR spectra show characteristic [W3O4]4+ bands at 746–815 cm?1. Thermal analysis reveals that the complex is air stable up to 250°C. Cluster 1 decomposes in hot aqueous 2 M HCl solution to produce discrete [W3O4]4+ units. 相似文献
15.
A new cyano‐bridged binuclear 4f‐3d complex Sm(DMSO)4‐(H2O)3Cr(CN)6 was synthesized and characterized by single crystal structure analysis. It crystallizes in monoclinic, space group P21 with a=0.9367(2) nm, b = 1.3917(3) nm, c = 1.1212(2) run, β = 99.88(3)° and Z = 2. In this binuclear complex, Sm atom is eight coordinated and linked to the Cr atom by a cyano bridge. The molecules packs to form 3D structure due to the hydrogen bonds among them. [K3(18‐C‐6)3(H2O)4]Cr(CN)6·3H2O (18‐C‐6 represents 18‐crown‐6‐ether) that was synthesized as a byproduct in the preparation of a Gd—Cr complex is also structurally characterized. Crystal data: triclinic, space group P‐l with a = 1.0496(7) nm, b= 1.1567(14) nm, c = 1.3530(13) nm, a = 94.15(9)°, β = 96.04(8)°, γ = 95.25(9)° and Z = l. [K3(18‐C‐6)3(H2O)4]‐Cr(CN)6·3H2O consists of ionic [K3(18‐C‐6)3(H2O)4]3+ and [Cr(CN)6]3‐ pairs, of which the [K3(18‐C‐6)3(H2O)4]3+ ion is a trinuclear duster connected by water, and K atoms are eight coordinated by eight oxygen atoms of one 18‐C‐6 and two water molecules. 相似文献
16.
The reaction of CuBr2, N(CH2CH2COOH)3, and Nd(NO3)3·6H2O in water adjusted pH = 5‐6 with H2SO4 at constant 55 °C afforded a novel three‐dimensional coordination complex [Cu12(SO4)12(3H2O)]·H2O, ( 1 ), which was characterized by IR, elemental analysis, and X‐ray diffraction. The crystal structure data of 1 as follows: Cubic, , a = b = c = 24.018(2) Å, V = 13855 (3) Å3, Z = 968, Dc = 1.905 g/cm3, F(000) = 7712, R1 = 0.0352, wR2 = 0.0866 (I > 2σ(I)), R1 = 0.0449, wR2 = 0.0927 (for all data) and S = 1.075. The analysis of crystal structure indicates that the structure of 1 is similar to that of silicate zeolite (Na12[Al12Si12O48]·27H2O). 相似文献
17.
《Journal of Coordination Chemistry》2012,65(11):1003-1012
A new composite complex of [La(NMP)4(H2O)4][HSiMo12O40]·2NMP·H2O (NMP = N-methyl-2- pyrrolidone) was synthesized and characterized by IR, UV, ESR, TG-DTA and single crystal structural analysis. The water and organic ligands (NMP) coordinate directly with La(III) to form a dodecahedral complex and the SiMo12O4? 40 anion is the counter ion. IR and X-ray analysis show that there is strong interaction between the polyoxometalate and organic donors. The complex is strongly photosensitive under irradiation with sunlight, resulting in a charge-transfer complex by oxidation of the N-methyl-2-pyrrolidone and reduction of the polyoxometalate. Low temperature ESR spectra indicate thermal electron delocalization among the Mo atoms in the title compound. 相似文献
18.
Cubic [Ta6Br12(H2O)6][CuBr2X2]·10H2O and triclinic [Ta6Br12(H2O)6]X2·trans‐[Ta6Br12(OH)4(H2O)2]·18H2O (X = Cl, Br, NO3) cocrystallize in aqueous solutions of [Ta6Br12]2+ in the presence of Cu2+ ions. The crystal structures of [Ta6Br12(H2O)6]Cl2·trans‐[Ta6Br12(OH)4(H2O)2]·18H2O ( 1 ) and [Ta6Br12(H2O)6]Br2·trans‐[Ta6Br12(OH)4(H2O)2]·18H2O ( 3 )have been solved in the triclinic space group P&1macr; (No. 2). Crystal data: 1 , a = 9.3264(2) Å, b = 9.8272(2) Å, c = 19.0158(4) Å, α = 80.931(1)?, β = 81.772(2)?, γ = 80.691(1)?; 3 , a = 9.3399(2) Å, b = 9.8796(2) Å, c = 19.0494(4) Å; α = 81.037(1)?, β = 81.808(1)?, γ = 80.736(1)?. 1 and 3 consist of two octahedral differently charged cluster entities, [Ta6Br12]2+ in the [Ta6Br12(H2O)6]2+ cation and [Ta6Br12]4+ in trans‐[Ta6Br12(OH)4(H2O)2]. Average bond distances in the [Ta6Br12(H2O)6]2+ cations: 1 , Ta‐Ta, 2.9243 Å; Ta‐Bri , 2.607 Å; Ta‐O, 2.23 Å; 3 , Ta‐Ta, 2.9162 Å; Ta‐Bri , 2.603 Å; Ta‐O, 2.24 Å. Average bond distances in trans‐[Ta6‐Br12(OH)4(H2O)2]: 1 , Ta‐Ta, 3.0133 Å; Ta‐Bri, 2.586 Å; Ta‐O(OH), 2.14 Å; Ta‐O(H2O), 2.258(9) Å; 3 , Ta‐Ta, 3.0113 Å; Ta‐Bri, 2.580 Å; Ta‐O(OH), 2.11 Å; Ta‐O(H2O), 2.23(1) Å. The crystal packing results in short O···O contacts along the c axes. Under the same experimental conditions, [Ta6Cl12]2+ oxidized to [Ta6Cl12]4+ , whereas [Nb6X12]2+ clusters were not affected by the Cu2+ ion. 相似文献
19.
Single crystals of fluoride hydrates Mn3F8 · 12 H2O and AgMnF4 · 4 H2O have been prepared and characterized by X-ray methods. Mn3F8 · 12 H2O crystallizes in the space group P1 (a = 623.0(3), b = 896.7(4), c = 931.8(4) pm, α = 110.07(2)°, β = 103.18(2)°, γ = 107.54(2)°, Z = 1); AgMnF4 · 4 H2O crystallizes in the space group P21/m (a = 700.9(2), b = 726.1(1), c = 749.4(3) pm, β = 107.17(3)°, Z = 2). Both structures contain Jahn-Teller-distorted [Mn(H2O)2F4]? anions as well as crystal water molecules and exhibit a complex hydrogen bond network between anions and cations, i. e. [Mn(H2O)6]2+ for the first and a polymeric [Ag(H2O)2]? cation for the second compound. 相似文献