Synthesis and Crystal Structure of [Zn(HPDB)_2(H_2O)_2]n·2nDMSO·2nH_2O (H_2-PDB = Pyridine-3,4-dicarboxylic Acid)

1 INTRODUCTION Metal-organic coordination polymers are currently of considerable interest and importance because they can be used as new functional materials applicable in adsorption, luminescent and NLO materials fields[1, 2]. Due to the manifold N- and O-donors of pyridine- (bi)carboxylic ligands, metal pyridine-(bi)carboxyla- tes can construct versatile structural motifs, which finally aggregate to generate various supramolecular architectures with interesting properties[3, 4]. The d…     

Hydrothermal Synthesis and Crystal Structure of a New Zero-dimensional Complex: [Zn(H2BPTC)(phen)2]n·3nH2O

A new metal-organic coordination complex [Zn(H2BPTC)(phen)2]n·3nH2O (BPTC =3,3',4,4'-benzophenone tetracarboxylate, phen = 1,10-phenanthroline) 1 has been obtained from hydrothermal reaction and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. In compound 1, the zinc cation is hexa-coordinated with two carboxylate oxygen atoms from one H2BPTC ligand and four nitrogen atoms from two different phen ligands, showing a slightly distorted octahedral geometry. Crystal data: C41H30N4O12Zn, Mr = 836.06, monoclinic,P21/c, a = 14.2714(9), b = 16.9386(10), c = 15.0151(9) (A),β = 101.3420(10)°, V= 3558.8(4) (A)3, Dc= 1.560 g/cm3,μ(MoKα) = 0.766 mm-1, F(000) = 1720, Z = 4, R = 0.0439 and wR = 0.1157 for 4123observed reflections with I ＞ 2σ(I).     

Synthesis and Crystal Structure of a Three-dimensional Manganese(Ⅱ)Complex (tataH)2[Mn(pydc)2]·4H2O(tata= 2,4,6-Triamino-1,3,4,-triazine,pydcH2= Pyridine-2,6-dicarboxylic Acid)

A manganese(Ⅱ) complex (tataH)2[Mn(pydc)2]·4H2O (C20H28MnN14O12, Mr = 711.50, tata = 2,4,6-triamino-1,3,5-triazine, pydcH2 = pyridine-2,6-dicarboxylic acid) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1, with a = 9.9847(3), b = 10.9813(3), c = 15.2616(5) (A), α =101.5310(10), β = 90.2610(10), γ = 116.4600(10)°, V = 1459.44(8) A3, Z = 2, Dc = 1.619 g/cm3, μ = 0.539 mm-1, F(000) = 734, the final R = 0.0292 and wR = 0.0745. In the crystal the MnⅡ atom is six-coordinated by four carbonyl oxygen atoms and two pyridine nitrogen atoms from two tridentate H-bonded tetramer. The molecules are packed in a three-dimensional framework structure by the combination of O-H…O,N-H…O and N-H…N hydrogen bonds between (tataH) ,[Mn(pydc)2]2- and crystal water.     

Synthesis, Crystal Structure and Luminescent Property of [Zn(C12H9O3)2(C10H8N2)]n·nH2O

Under hydrothermal condition, the reaction of 2-naphthoxyacetic acid with ZnCl2 and 4,4'-bipyridine (4,4'-bipy)has afforded a new Zn(Ⅱ) compound,[Zn(C12H9O3)2(C10H8N2)]n·nH2O1, which was structurally characterized by single-crystal X-ray diffraction analysis. The crystal is of monoclinic, space group P21/c with a = 7.7335(2), b = 19.3834(4), c = 20.1707(4) (A), β =104.9830(10)°, V = 2920.82(11) A3, C34H28ZnN2O7, Mr = 641.95, Z = 4, Dc = 1.460 g/cm3, μ = 0.895 mm-1, F(000) = 1328, R = 0.0406 and wR = 0.0876 for 4417 observed reflections (Ⅰ>2σ(Ⅰ)). Complex 1 consists of one-dimensional zigzag chains deriving from Zn(C12H9O3)2 units linked by 4,4'-bipy ligands, and lattice water molecules decorate between the chains. Non-covalent interactions, such as hydrogen-bonding and aromatic π-π interactions, lead to the formation of a 3D network structure. The thermogravimetric analysis (TGA) and luminescent property for 1 have also been studied in this paper.     

Synthesis and Crystal Structure of [{Cd(hmbdc)(H2O)3}·2H2O]n

A novel coordination polymer [{Cd(hmbdc)(H2O)3}·2H2O]n (hmbdc=5-hydroxy- isophthalic acid) has been synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c, with a=9.599(3), b=18.699(5), c=7.557(2) (A), β= 108.198(4)°, V=1288.6(6) (A)3, Z=4, Mr=382.60, Dc=1.972 g/cm3, F(000)=760, μ=1.740, the final R=0.0555 and wR=0.0995 for 1732 observed reflections with Ⅰ ＞ 2σ(Ⅰ). The structural analysis shows that the intermolecular hydrogen bonds and π-π interactions result in a three-dimensional supramolecular framework.     

Synthesis and Crystal Structure of [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O

A novel complex [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O (Fc = (η5-C5H5)Fe(η5-C5H4), 2,2′-bipy = 2,2′-bipyridine) has been synthesized and characterized by elemental analysis, IR and X-ray diffraction. It crystallizes in monoclinic system, space group P21/c with a = 6.8187(4), b = 21.7155(13), c = 19.7411(12) (A), α = 90, β = 97.7420(10), γ = 90°, C64H58Fe4Zn2N4O11, Mr = 1413.28, V = 2896.4(3) (A)3, Dc = 1.620 g/cm3, Z = 2, F(000) = 1444, μ(MoKα) = 1.857 mm-1, R = 0.0523 and wR = 0.0982 for 3219 observed reflections (I ＞ 2σ(I)). Structural analysis shows that the zinc atom is coordinated with three oxygen atoms from two ferrocenemonocarboxylates and one water molecule together with two nitrogen atoms from 2,2′-bipyridine, giving a distorted square-pyramidal coordination geometry. The complex molecules are linked to form an infinite one-dimensional chain by both intermolecular hydrogen bonds and π-π stacking interactions of the bipyridine rings.     

Synthesis and Crystal Structure of [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O

A novel complex [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O (Fc = (η5-C5H5)Fe(η5-C5H4), 2,2′-bipy = 2,2′-bipyridine) has been synthesized and characterized by elemental analysis, IR and X-ray diffraction. It crystallizes in monoclinic system, space group P21/c with a = 6.8187(4), b = 21.7155(13), c = 19.7411(12) (A), α = 90, β = 97.7420(10), γ = 90°, C64H58Fe4Zn2N4O11, Mr = 1413.28, V = 2896.4(3) (A)3, Dc = 1.620 g/cm3, Z = 2, F(000) = 1444, μ(MoKα) = 1.857 mm-1, R = 0.0523 and wR = 0.0982 for 3219 observed reflections (I ＞ 2σ(I)). Structural analysis shows that the zinc atom is coordinated with three oxygen atoms from two ferrocenemonocarboxylates and one water molecule together with two nitrogen atoms from 2,2′-bipyridine, giving a distorted square-pyramidal coordination geometry. The complex molecules are linked to form an infinite one-dimensional chain by both intermolecular hydrogen bonds and π-π stacking interactions of the bipyridine rings.     

Synthesis, Crystal Structure and Luminescence Property of [Co(hmz)2(H2O)4]·2H2O

A new mononuclear Co(Ⅱ) complex, [Co(hmz)2(H2O)4]·2H2O, has been synthesized by the reaction of Co(CH3COO)2·4H2O with 1-(4-hydroxyphenyl)-5-mercaptotetrazole (Hhmz). It crystallizes in the monoclinic system, space group P21/n with a = 13.502(5), b = 6.718(3), c = 13.972(6) (A), β = 117.532(4)°, V = 1123.9(8) (A)3, Z = 2, M r = 553.45, F(000) = 570, Dc = 1.635 g/cm3, μ = 1.008 mm-1, the final R = 0.0272 and wR = 0.0684 for 2194 observed reflections (Ⅰ＞ 2σ(Ⅰ)). The Co(Ⅱ) is six-coordinated by two nitrogen atoms from two hmz-1 ligands and four water molecules, forming an octahedral geometry. The intermolecular hydrogen bonding and offset-panel π-π stacking interactions between the adjacent molecules extend the compound into a three- dimensional supramolecular framework. The title compound emits strong blue fluorescent light (λem(max) = 427 nm) at room temperature and is red-shifted compared with free ligand Hhmz (λem(max) = 342 nm).     

Synthesis and Crystal Structure of a Novel Zinc Complex[Zn(OH2)(HDPA)2]·3H2O

A new complex [Zn(OH2)(HDPA)2]·3H2O 1 (H2DPA = 2,6-pyridine-dicarboxylic acid) has been prepared at room temperature from the reaction of zinc(II) chloride and 2,6-pyri- dine-dicarboxylic acid in mixed solvent of H2O and EtOH with pyridine, and characterized by X-ray analysis and thermal analysis, exhibiting that the coordination geometry of Zn(II) ion is an octa- hedron. Crystal data: ZnC14H16N2O12, Mr = 469.66, monoclinic, P21/n, a = 7.0067(3), b = 23.8215 (12), c = 10.7404(3)(A), β = 99.823(2)°,V = 1766.40(13)(A)3, Z = 4, Dc = 1.766 g/cm3, F(000) = 960, μ = 1.463 mm-1, R1 = 0.0462 and wR2 = 0.0884 (I > 2σ(I)).     

Synthesis and Crystal Structure of K3[HO{VO(O2)2}2]·H2O

The title compound K3[HO{VO(O2)2}2]·H2O has been synthesized and its crystal structure was determined by X-ray diffraction method. The crystal is of monoclinic, space group P21/c with a = 6.7078(3), b = 9.9539(6), c = 15.8182(9)A, β = 93.702(3)0, V = 1053.96(10)A3, Mr = 414.20, Dc = 2.610 g/cm3, Z = 4, λ(MoKα) = 0.71073A, F(000) = 808, μ = 3.014 mm-1, the final R = 0.0173 and wR = 0.0466 for 2178 observed reflections with I > 2σ(I). X-ray diffraction reveals that the coordination polyhedra of V atoms are not chemically equivalent: the V(1) and V(2) polyhedra can be described as pentagonal pyramid and pentagonal bipyramid, respectively.     

Synthesis,Crystal Structure and Luminescent Property of [Zn（C12H9O3）2（C10H8N2）]n·nH2O

Under hydrothermal condition, the reaction of 2-naphthoxyacetic acid with ZnCl2 and 4,4′-bipyridine （4,4′-bipy） has afforded a new Zn（Ⅱ） compound, [Zn（C12H9O3）2（C10H8N2）]n·nH2O1, which was structurally characterized by single-crystal X-ray diffraction analysis. The crystal is of monoclinic, space group P21/c with a = 7.7335（2）, b = 19.3834（4）, c = 20.1707（4） A, β = 104.9830（10）°, V = 2920.82（11） A^3, C34H28ZnN2O7, Mr = 641.95, Z = 4, Dc = 1.460 g/cm^3,μ = 0.895 mm^-1, F（000） = 1328, R = 0.0406 and wR = 0.0876 for 4417 observed reflections （I〉 2σ（I）） Complex 1 consists of one-dimensional zigzag chains deriving from Zn（C12H9O3）2 units linked by 4,4′-bipy ligands, and lattice water molecules decorate between the chains. Non-covalent interactions, such as hydrogen-bonding and aromatic π-π interactions, lead to the formation of a 3D network structure. The thermogravimetric analysis （TGA） and luminescent property for 1 have also been studied in this paper.     

Synthesis and Crystal Structure of [H-amp]4[Mo8O26(DMF)2]·2H2O (amp = 2-Amino-6-methyl-pyridine)

The reaction of MoO2(acac)2 with 2-amino-6-methyl-pyridine (amp) in the mixed solvent of DMF (N,N-dimethylformamide) and water affords the title complex [H-amp]4- [Mo8O26(DMF)2]·2H2O which was characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction analysis with the following crystallographic data: C30H54Mo8N10O30, Mr = 1802.35, monoclinic, P21/n, a = 8.631(1), b = 24.260(3), c = 13.351(2)A,β= 104.688(3)°, V = 2704.2(7) A3, Z = 2, Dc = 2.213 g/cm3, μ =1.890 mm－1 and F(000) = 1760. The final R = 0.0281 and Wr = 0.0620 for 4935 observed reflections with I > 2σ(I). X-ray structure analysis has confirmed the existence of γ-[Mo8O26]4－ anion in the molecule. Eight MoO6 distorted octahedra share edges with short terminal Mo-O bonds from 1.691(3) to 1.749(2)A, medium bonds from 1.868(2) to 1.965(2) A And long bonds from 2.059(2) to 2.450(2) A. In the terminal site there exist two DMF ligands bound to the Mo atom through O atoms with the Mo-ODMF bond length of 2.166(3) A, affording a bond strength of 0.433. A three-dimensional network structure was formed through hydrogen bonds.     

Synthesis and Crystal Structure of K6.5H4.5[CeK2(SiW11O39)2]·26H2O

The title compound, K_6.5H_4.5[CeK₂(SiW₁₁O₃₉)₂]·26H₂O was prepared and its structure characterized by IR and single crystal X-ray structural analysis. It belongs to triclinic, space group P1 with a = 12.719(3) Å, b = 16.658(4) Å, c = 23.075(6) Å, α = 94.41(2)°, β = 98.90(2)°, γ = 92.40(2)°; V = 4809(2) Å^?3, Z = 2, Dc = 4.344 g cm^?3, μ = 27.170 mm^?1, F (000) = 5519. The results show that the cerium and two potassium atoms link the two anionic units SiW₁₁O^8? ₃₉ through O-Ce-O and O-K-O bridges and construct the double 1 : 11 series heteropolytungstate. Furthermore, cerium is coordinated to eight oxygen atoms (four O_c and four O_b) from two tetradentate SiW₁₁O^8? ₃₉ ligands forming a square anti-prism. The coordination numbers for K1 and K2 are 8 and 7, respectively.     

Synthesis, Crystal Structure and Magnetic Properties of Novel Three-dimensional Frameworks [Mn(PDC)H2O]n

A novel coordination polymer, [Mn(PDC)H2O]n (1) (H2PDC＝pyridine-2,3-dicarboxylic acid), has been hydrothermally synthesized and characterized by elemental analysis, IR and single crystal X-ray diffraction. X-ray single crystal structural analyses revealed that two-dimensional frameworks were formed, and further assembled into a three-dimensional supramolecular structure bridged by PDC ligands. Moreover, the magnetic study of complex 1 shows weak antiferromagnetic interaction between the neighboring Mn(II) centers within the chains and even weak ferromagnetic interactions between the Mn(II) centers in different chains.     

Synthesis and Crystal Structure of Complex [Pb(qina)2(DMSO)]·H2O

A novel complex [Pb(qina)2(DMSO)]·H2O was synthesized, of which qina- is the quinaldic acid radical and DMSO the dimethyl sulfoxide. Elemental analysis, IR spectra, and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure. This complex belongs to monoclinic system, space group P121/n1, with a = 7.1553(17), b = 17.543(2), c = 17.306(2)(A),β = 91.671(4)°, C22H20N2O6PbS, Mr = 647.65, Z = 4, V= 2171.5(6)(A)3, Dc= 1.981g/cm3,μ = 7.908 mm-1, F(000) = 1248, -9≤h≤6, -23≤k≤ 19, -22≤l≤22, R= 0.0221 and wR =0.0488. Weak coordinate bond is formed between oxygen atom in DMSO and Pb(Ⅱ ). There are also weak interactions, such as π-π interaction, hydrogen bonds and so on, among the complex molecules.     

Synthesis, Crystal Structure, and Photoluminescent and Semiconductive Properties of [La(C6NO2H5)3-(H2O)2]2n·(nH5O2)(nHgCl5)(2nHgCl4)·(2nH2O)

A new heterometallic 4f-5d inorganic-organic metal-isonicotinic acid complex [La(C6NO2H5)3(H2O)2]2n·(nH5O2)(nHgCl5)(2nHgCl4)·(2nH2O) 1 has been synthesized via hydro-thermal reaction and structurally characterized. Complex 1 crystallizes in the space group C2/c of monoclinic system with four formula units in a cell: α= 24.140(7), b = 20.884(7), c = 15.462(2) (A), β = 127.46(1)°,V = 6187(3) (A)3, C36H47Cl13Hg3La2N6O20, Mr = 2224.24, Dc = 2.388 g/cm3, Z = 4, T = 293(2) K, μ(MoKα) = 9.401 mm-1, F(000) = 4160 and R/wR = 0.0376/0.0636 for 4130 observed reflections (I > 2σ(I)) and 5617 unique reflections. Complex 1 is characteristic of a one-dimensional polycationic chain-like structure. Photoluminescent investigation reveals that the title complex displays interesting emissions in violet and orange regions. The luminescence spectra show stronger orange emission than violet emission. Optical absorption spectra of 1 reveal the presence of a wide optical bandgap of 3.41 eV.     

Synthesis and Crystal Structure of [La（BTC）（H2O）6]n

1 INTRODUCTION desired topologies owing to their rich coordination modes[8~12] and we have been exploring the chemi- The assembly of metal-organic infinite frame- stry of coordination polymers constructed by tran- works via coordination of metal ions with multifunc- sition metals and benzoic multicarboxylic acids[13~16]. tional organic ligands is a field of increasing inte- In addition, lanthanide ions have high affinity for rest[1~4]. A rational designed and predictable coor- hard donor a…     

Synthesis,Crystal Structure,and Properties of [Dy(p-ABA)3Phen · H2O] · 1.5H2O1

(1.10-Phenanthroline)-tris(4-amidobenzoate)dysprosium, [Dy(p-ABA)₃Phen · H₂O] · 1.5H₂O (where p-ABA = p-amidobenzoate and Phen = 1.10-phenanthroline) has been synthesized. The complex was characterized by elemental analysis, UV, IR spectroscopy, and molar conductance. The crystal structure was determined by X-ray crystallography. The coordination number of the mononuclear complex is nine. The crystals are triclinic, space group P1 with a = 10.4484(13) Å, b = 12.2015(15) Å, c = 14.0170(17) Å; α = 92.800(2)°, β = 102.7220(10)°, γ = 108.880(2)°. Z = 2, d _c = 1.617 mg m^?3, F(000) = 786. R1 = 0.0327, and wR2 = 0.0911.     

Synthesis and Crystal Structure of a Three-dimensional Manganese(II) Complex (tataH)_2[Mn(pydc)_2]·4H_2O (tata = 2,4,6-Triamino-1,3,5-triazine, pydcH_2 = Pyridine-2,6-dicarboxylic Acid)

A manganese(II) complex (tataH)2[Mn(pydc)2]·4H2O (C20H28MnN14O12, Mr = 711.50, tata = 2,4,6-triamino-1,3,5-triazine, pydcH2 = pyridine-2,6-dicarboxylic acid) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1, with a = 9.9847(3), b = 10.9813(3), c = 15.2616(5) , α = 101.5310(10), β = 90.2610(10), γ = 116.4600(10)°, V = 1459.44(8) 3, Z = 2, Dc = 1.619 g/cm3, μ = 0.539 mm–1, F(000) = 734, the final R = 0.0292 and wR = 0.0745. In the crystal the MnII atom is six-coordinated by four carbonyl oxygen atoms and two pyridine nitrogen atoms from two tridentate pydc ligands to furnish a distorted octahedral geometry. The complex shows the A…D…D’…A’ H-bonded tetramer. The molecules are packed in a three-dimensional framework structure by the combination of O–H…O, N–H…O and N–H…N hydrogen bonds between (tataH)+, [Mn(pydc)2]2– and crystal water.     

Synthesis,Crystal Structure and Spectral Properties of [Ce(NO3)5(H2O)2]·2(Hphen)·(H2O)

A novel complex [Ce(NO3)5(H2O)2]·2(Hphen)·(H2O) (phen =1,10-phenanthroline) with formula C24H24CeN9O18 and Mr = 866.64 has been synthesized and structurally characterized by X-ray diffraction. It crystallizes in triclinic, space group Pī with a = 7.5534(2), b = 8.083(2), c = 25.8377(6) A, α = 86.847(1), β = 89.937(1), γ = 86.981(1)o, V = 1572.94(6) A3, Dc = 1.830 g/cm3, F(000) = 866, β = 1.545 cm-1 and Z = 2. The final refinement gave R = 0.0486 and wR = 0.1278 for 4852 observed reflections with I > 2σ(I). It consists of discrete [Ce(NO3)5(H2O)2]2- anion, two Hphen+ cations and a lattice water molecule. In the compound, all of the five nitrates are bidentate, and the coordination of Ce(III) is 12. The photo-luminescence of this compound was also investigated.