Syntheses and Crystal Structures of Two New One-dimensional Double Hydrogen-bonding-chain Complexes [Ni(bipy)_2Cl]·ClO_4 and [Zn(bipy)_2Cl]·BF_4

Two new transition metal complexes, [Ni(bipy)2Cl]·ClO4 (bipy = 2,2'-bipyridine) 1 and [Zn(bipy)2Cl]·BF4 2, have been synthesized and characterized by single-crystal X-ray diffraction analysis. Both 1 and 2 crystallize in monoclinic space group P21/n with Z = 4. For 1, a = 10.776(1), b = 12.067(1), c = 16.146(2) , β = 93.021(2)o, V = 2031.9(4) 3, Mr = 505.98, Dc = 1.654 g/cm3, μ = 1.255 mm–1, F(000) = 1032, the final R = 0.0406 and wR = 0.1002 for 3983 observed reflections with I > 2σ(I). For 2, a = 10.758(4), b = 12.058(4), c = 16.135(5) , β = 104.57(1)o, V = 2025.7(12) 3, Mr = 500.00, Dc = 1.639 g/cm3, μ = 1.396 mm–1, F(000) = 1008, the final R = 0.0470 and wR = 0.1237 for 3759 observed reflections with I > 2σ(I). The crystal structures of 1 and 2 are isostructural with very similar supramolecular structures. A one-dimen-sional zigzag double hydrogen-bonding-chain is generated by the intermolecular M-bipy ···anion···bipy- M hydrogen bonding interactions between the chelating ligands of bipy and anion.     

Synthesis and Characterization of Chiral Mercury（II） and Cadmium（II） Complexes with 3,3＇-Bipyridine-5,5＇,6,6＇-tetramethyl-2,2＇-dimethoxy-1,1＇-biphenyl

Two homochiral mercury (1) and cadmium (2) complexes derived from chiral twisted biphenyl pyridine ligand (3,3'-bipyridine-5,5',6,6'-tetramethyl-2,2'-dimethoxy-1,1'-biphenyl) have been synthesized and characterized by IR, microanalysis, TGA, UV-Vis, powder and single-crystal X-ray crystallography. Both 1 and 2 crystallize in orthorhombic space group P21212 with Z = 2. For 1, a = 14.2038(16), b = 14.3630(17), c = 7.0257(8), V = 1433.3(3)3, Mr = 878.91, Dc = 2.037 g/cm3, μ = 7.549 mm-1, F(000) = 824, the final GOF = 1.017, R = 0.0296 and wR = 0.0645 for 2925 observed reflections with I > 2σ(I). For 2, a = 14.212(3), b = 14.392(3), c = 7.0498(14), V = 1442.0(5)3, Mr = 790.72, Dc = 1.821 g/cm3, μ = 2.924 mm-1, F(000) = 760, the final GOF = 1.075, R = 0.0340 and wR = 0.0834 for 3144 observed reflections with I > 2σ(I). The crystal structures of 1 and 2 are isostructural and each adopts a two-dimensional supramolecular network which contains the C-H···π interactions.     

Synthesis and Characterization of Two Chiral Cadmium Coordination Compounds Constructed from (1S,1′S)-1,1′-(4-amino-4H-1,2,4-triazole-3,5-diyl)diethanol

Two chiral cadmium coordination compounds,(S)-[Cd(deoatrz)2 Cl2](1)and(S)[Cd(deoatrz)2 (NO3)2](2)(deoatrz=(1S,1 S)-1,1-(4-amino-4H-1,2,4-triazole-3,5-diyl)diethanol),are reported.Both 1 and 2 are mononuclear,crystallizing in tetragonal P41212 chiral space group with Z=2.For1,a=11.520(3),b=11.520(3),c=15.175(1),V=2013.6(1)3,Mr=527.7,Dc =1.741 g/cm 3,μ=1.386mm-1,F(000)=1064,the final GOF=1.05,R=0.0147 and wR=0.0433 for1932 observed reflections with I>2σ(I).For 2,a=12.201(3),b=12.201(3),c=15.027(4),V=2237.1(1)3,Mr=580.8,Dc=1.725 g/cm 3,μ=1.047mm-1,F(000)=1176,the final GOF=1.00,R=0.0201 and wR=0.0415 for 2408 observed reflections with I>2σ(I).Compounds 1 and 2 are connected into three-dimensional supramolecular networks through hydrogen bonding interactions.     

Addition Reaction of Bis（diphenylphosphinyl） Butadiyne with Methylcyclopentadiene

Bis(diphenylphosphinyl)butadiyne reacted with methylcyclopentadiene at room tem- perature and four isomeric products were obtained. Crystal structures of isomers 1 and 3 have been determined. Crystal data for compound 1 C40H36O2P2·2CHCl3: monoclinic, space group C12/c1 with a = 17.983(2), b = 11.8723(12), c = 20.081(2) , β = 111.218(3)°, V = 3996.5(8) 3, Z = 4, Mr = 849.36, Dc = 1.412 g/cm3, F(000) = 1752, μ = 0.546 mm-1, the final R = 0.0351 and wR = 0.0951 for 3965 observed reflections (I > 2σ(I)); and those for compound 3 C40H36O2P2·H2O: triclinic, space group P1 with a = 10.4144(15), b = 13.0558(18), c = 13.742(2) , α = 70.453(8), β = 75.382(8), γ = 72.312(8)°, V = 1653.7(4) 3, Z = 2, Mr = 628.64, Dc = 1.262 g/cm3, F(000) = 664, μ = 0.169 mm-1, the final R = 0.0593 and wR = 0.1296 for 4891 observed reflections (I > 2σ(I)). The structures of the other two isomers are identified via IR, 1H NMR and MS spectra.     

Syntheses and Crystal Structures of Two New Macrocyclic Compounds

Two new macrocyclic compounds, [Cu2(L)2](ClO4)4·2CH3OH (1) and [Cu(L)](ClO4)2·2H2O (2) (L = 1,3,10,12,15,18-hexaazatetracyclodocosane) were synthesized by condensation reactions involving amines and formaldehyde in the presence of copper anion. Compound 1 crystallizes in triclinic, space group Pí with a = 10.442(2), b = 14.197(3), c = 17.388(4), α = 91.218(4), β = 90.69(3), γ = 93.756(4)o, V = 2520.4(9)3, Z = 2, F(000) = 1260, Dc = 1.589 Mg/m3, Mr = 1205.92, μ = 1.137 mm-1, λ = 0.71073, the final R = 0.0668 and wR = 0.1573 for 9703 observed reflections with I > 2σ(I). Compound 2 crystallizes in monoclinic, space group C2/c with a = 16.911(2), b = 11.4172(15), c = 27.059(4), β = 107.787(2)o, V = 4974.7(12)3, Z = 8, F(000) = 2504, Dc = 1.610 Mg/m3, Mr = 602.92, μ = 1.155 mm-1, λ = 0.71073 , the final R = 0.0419 and wR = 0.1131 for 4374 observed reflections with I > 2σ(I).     

Synthesis and Characterization of Nickel(II) and Copper(II) Complexes with Schiff Base (1R,2R)-(-)-Diaminocyclohexane-N,N'-bis(3-tert-butyl-5-(4'-benzoic acid)-salicylidene)

Two homochiral metallosalen complexes, Ni(salen) (salen = (1R,2R)-(-)-diaminocyclohexane-N,N'-bis(3-tert-butyl-5-(4'-benzoic acid)-salicylidene) 1 and Cu(salen) 2, have been synthesized and characterized by IR, microanalysis, TGA, powder and single-crystal X-ray crystallography. Both 1 and 2 crystallize in orthorhombic space group P21212 with Z = 4. For 1, a = 12.082(2), b = 15.447(3), c = 18.784(4) , V = 3505.7(12) 3, Mr = 731.50, Dc = 1.386 g/cm3, μ = 0.606 mm–1, F(000) = 1544, the final GOOF = 1.043, R = 0.0496 and wR = 0.1248 for 4791 observed reflections with I > 2σ(I). For 2, a = 12.181(2), b = 15.501(3), c = 18.877(4) , V = 3564.3(12) 3, Mr = 736.33, Dc = 1.372 g/cm3, μ = 0.665 mm–1, F(000) = 1548, the final GOOF = 1.062, R = 0.0575 and wR = 0.1508 for 4562 observed reflections with I > 2σ(I). The crystal structures of 1 and 2 are isostructural with very similar supramolecular structures. An infinite two-dimensional network is generated by hydrogen bonding interactions and intermolecular π···π interactions.     

Syntheses, Crystal Structures and Magnetism of Two New Coordination Polymers [Ni（bix）2Cl2]n and [Co（bix）Cl2]n

The self-assembly reactions of MIICl2 (M = Ni, Co) with the flexible bix ligand [bix = 1,4-bis(imidazole-1-ylmethyl)benzene] yielded a 2D network [NiII(bix)2Cl2]n 1 and a 1D chain [CoII(bix)Cl2]n 2. Their crystal structures have been determined by X-ray single-crystal diffraction analysis. Complex 1 characters a two-dimensional grid-type structure and crystallizes in monoclinic, space group P21/c with a = 7.7231(7), b = 12.7787(9), c = 13.9374(13) , β = 105.419(4)o, C28H28Cl2N8Ni, Mr = 606.19, Ζ = 2, V = 1326.0(2) 3, Dc = 1.518 g/cm3, μ = 0.969 mm-1, F(000) = 628, R = 0.0429 and wR = 0.0783 for 2503 observed reflections (I > 2σ(I)). Compound 2 is a one-dimensional chain and crystallizes in orthorhombic, space group Pbca with a = 11.3696(6), b = 10.2128(6), c = 14.4943(9) , C14H14Cl2CoN4, Mr = 368.12, Z = 4, V = 1683.01(17) 3, Dc = 1.453 g/cm3, μ = 1.334 mm-1, F(000) = 748, R = 0.0317 and wR = 0.0800 for 1778 observed reflections (I > 2σ(I)). Magnetic properties of the title complexes were also investigated.     

Synthesis, Structure and Luminescent Properties of Polymeric Copper(Ⅰ) Halide Complexes Bearing Phosphine and N-donor Bridging Ligands

Three polymeric copper(Ⅰ) halide complexes bearing phosphine and N-donor bridging ligands, [(PPh3)2Cu2(μ-Br)2(μ-4,4'-bipy)]∞ 1 (bipy=bipyridine), [(PPh3)2Cu2(μ-Br)2(μ-bpe)]∞ 2 (bpe=trans-1,2-bis(4-pyridyl)ethene) and [(PPh3)2Cu2(μ-Cl)2(μ-bpe)]∞ 3, were synthesized by the multilayer diffusion method, and the structures were refined by single-crystal X-ray diffraction. Complex 1 crystallizes in triclinic, space group P-1 with a=9.122(3), b=9.322(3), c=13.201(4) (A),α=106.440(4), β=105.965(5), γ=94.167(5)°, V=1021.3(6) (A), Mr=967.62, Z=1,Dc=1.573 g/cm3, F(000)=486,μ=3.111 mm-1, the final R=0.0383 and wR=0.0960 for 2792observed reflections (I ＞ 2σ(Ⅰ)). Complex 2 crystallizes in triclinic, space group P-1 with a=9.420(3), b=10.209(4), c=12.407(4)(A), α=104.136(6), β=108.132(5), γ=95.338(6)°, V=1081.0(7)(A), Mr=496.83, Z=2, Dc=1.526 g/cm3, F(000)=500,μ=2.941 mm-1, the final R=0.0445 and wR=0.1117 for 3251 observed reflections (I＞ 2σ(Ⅰ)). Complex 3 crystallizes in triclinic,space group P-1 with a=8.32(1), b=11.53(2), c=13.94(3)(A), α=109.57(3), β=93.85(3), γ=97.28(3)°, V=1242(4)(A)3, Mr=1074.59, Z=1, Dc=1.436 g/cm3, F(000)=548,μ=1.279 mm-1,the final R=0.0786 and wR=0.1586 for 2266 observed reflections (I ＞ 2σ(Ⅰ)). The complexes exhibit intensive solid-state photoluminescence tentatively assigned to an admixture of triplet intraligand (IL) and metal-to-ligand charge-transfer (MLCT) excited state.     

Synthesis and Crystal Structure of 3-Methyl-10-(4-nitrophenyl)-7,8,10,10a-tetrahydropyrano[4,3-b]chromene-1,9(4aH,6H)-dione

The title compound (C19H15NO6) was synthesized via a three-component reaction and characterized by means of IR and 1H NMR. Its crystal and molecular structures were determined by X-ray diffractometry. It belongs to the monoclinic system, space group P21/c with a = 11.670(3), b = 12.076(3), c = 11.613(3), β = 99.490(4)°, V = 1614.2(7)3, Mr = 353.32, Z = 4, Dc = 1.454 g/cm3, λ = 0.71073, μ = 0.110 mm-1, F(000) = 736, the final R = 0.0503 and wR = 0.1311. A total of 8454 reflections were collected, of which 3497 were independent (Rint = 0.0333) and 2102 were observed with I > 2σ(I).     

Synthesis and Crystal Structure of 2-Amino-4- chloro-5-（4-methylbenzyl）-6-methylpyrimidine

The title compound 2-amino-4-chloro-5-(4-methylbenzyl)-6-methylpyrimidine (C26H28Cl2N6, Mr = 495.44) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/c with a = 14.892(7), b = 6.129(3), c = 14.889(7) , β = 109.795(8)°, V = 1278.7(10) 3, Z = 2, F(000) = 520, Dc = 1.287 g/cm3, μ = 0.280 mm-1, the final R = 0.0577 and wR = 0.1589 for 1357 observed reflections with I > 2σ(I). A total of 6091 reflections were collected, of which 2257 were independent (Rint = 0.033). The X-ray analysis reveals that the chlorine atom and methyl of the title compound are disordered.     

Two New Coordination Polymers Containing Metal-carboxylate Helix

Two novel compounds, {[Cd(nbdc)(bpp)(H2O)]·H2O}n 1 and {[Cd(nbdc)(dpds)-(H2O)]·H2O}n 2(H2nbdc = 4-nitro-1,2-benzenedicarboxylic acid, bpp = 1,3-bis(4-pyridyl)propane and dpds = 4,4ˊ-dipyridyldisulfide), were solvothermally synthesized and characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis(TGA), fluorescent analysis and single-crystal X-ray diffraction. Complex 1 is of monoclinic system, space group P21/c with a = 14.4370(17), b = 8.4090(10), c = 19.168(2) , β = 104.5050(10)°, V = 2252.8(5) 3, Dc = 1.639 g/cm3, Mr = 555.81, Z = 4, F(000) = 1120, μ = 1.022 mm-1, the final R = 0.0269 and wR = 0.0599 for 16656 observed reflections with I 2σ(I). 2 is isostructural to 1 with a = 14.4175(11), b = 8.4737(7), c = 18.0120(14) , β = 106.7220(10)°, V = 2107.5(3)3, Dc = 1.821 g/cm3, Mr = 577.85, Z = 4, F(000) = 1152, μ = 1.287 mm-1, the final R = 0.0280 and wR = 0.0705 for 15136 observed reflections with I 2σ(I). Both complexes present intimately related structures featuring infinite Cd-carboxylate helix of [CdⅡ(nbdc)(H2O)]n connected by bpp(or dpds) molecule to produce the 2D layer frameworks.     

Synthesis and Structure of a Zinc(Ⅱ)Complex:[Zn(Pybta)·Cl2]n

The title compound, [Zn(Pybta)Cl2]n (Pybta = 1-(2-pyridylmethyl)benzontriazole), has a zigzag chain structure. It crystallizes in the monoclinic system, space group P21/c with a = 9.0103(11), b = 17.0276(18), c = 9.2288(11) A, β = 101.309(6)°, Mr= 346.51, V= 1388.4(3) (A)3, Z= 4, Dc= 1.658 g/cm3, F(000) = 696, μ = 2.143 mm-1, the final R = 0.0492 and wR = 0.1236 for 2545 observed reflections with Ⅰ 2σ(Ⅰ). The Zn atom is four-coordinated by two N and two Cl atoms, forming a slightly distorted tetrahedral geometry. Each zigzag chain links its adjacent symmetry-related equivalents via multiple π-π interactions, which are not frequently observed in the previously reported architectures.     

Syntheses, Crystal Structures and Characterization of Layered and Layer-pillared Zinc Arsonates

Two zinc arsonate coordination polymers, Zn(4-apa)·H2O (1, 4-apaH2 = 4-amino- phenylarsonatic acid) and Zn(4-apa) (2), have been hydrothermally synthesized and characterized by elemental analysis, IR and single-crystal and powder X-ray diffraction. Crystal data for 1: monoclinic, space group C2/c with a = 23.056(5), b = 5.4224(11), c = 15.027(3) , β = 121.22(3)°, V = 1606.6(6) ?3, Dc = 2.468 g·cm-3, F(000) = 1168, μ = 7.122 mm-1, Z = 8, the final R = 0.0309 and wR = 0.0752 for 1763 observed reflections with I > 2σ(I). For 2: monoclinic, space group P21/c with a = 8.7852(18), b = 9.2744(19), c = 9.752(2) , β = 103.45(3)°, V = 772.7(3)3, Dc = 2.410 g·cm-3, F(000) = 544, μ = 7.387 mm-1, Z = 4, the final R = 0.0321 and wR = 0.0741 for 1696 observed reflections with I > 2σ(I). The structure of 1 shows a two-dimensional (4,4)-network composed of an inorganic ladder chain bridged by the phenyl-linkers of 4-apa ligands. Compound 2 exhibits a 3D layer-pillared framework with crb net, in which inorganic (4-82)-networks are joined by the phenyl-linkers.     

Syntheses and Crystal Structures of Two New Ag(Ⅰ) Complexes with Betaine Derivative: Structure Changes via Metal-to-ligand Ratio

Two new Ag(I) complexes {Ag2(L)(NO3)(H2O)}n(1) and {Ag(L)}n·nH2O(2) have been synthesized via the reaction of silver nitrate and betaine derivative 1-carboxymethylpyridinium-3-carboxylate(L) by only changing the metal-to-ligand ratio. The results of X-ray crystallographic analysis indicate that complexes 1 and 2 both crystallize in the monoclinic space group P21/c with a = 5.0809(14), b = 17.390(5), c = 13.399(4), β = 91.677(5)o, V = 1183.4(6)3, Z = 4, Mr = 475.90, Dc = 2.671 g/cm3, F(000) = 912, μ = 3.352 mm-1, S = 1.259, the final R = 0.0320 and wR = 0.0831 for 2036 observed reflections with I 2σ(I) for 1 and a = 12.180(2), b = 5.0283(10), c = 14.396(3), β = 94.87(3)o, V = 878.5(3)3, Z = 4, Mr = 306.02, Dc = 2.314 g/cm3, F(000) = 600, μ = 2.294 mm-1, S = 1.053, the final R = 0.0283 and wR = 0.0684 for 2011 observed reflections with I 2σ(I) for 2. Complexes 1 and 2 both feature a unique 2D structure. For 1, the 2D undulated network consists of 1D infinite helical chains running parallel to the b axis, while for 2, the 2D network is made up of 1D tubes along the b axis. Moreover, the Ag…Ag interactions in complexes 1 and 2 are also discussed.     

Synthesis, Structure and Luminescent Properties of Polymeric Copper（Ⅰ） Halide Complexes Bearing Phosphine and N-donor Bridging Ligands

Three polymeric copper(I) halide complexes bearing phosphine and N-donor bridging ligands,[(PPh3)2Cu2(μ-Br)2(μ-4,4′-bipy)]∞ 1 (bipy=bipyridine),[(PPh3)2Cu2(μ-Br)2(μ-bpe)]∞ 2 (bpe=trans-1,2-bis(4-pyridyl)ethene) and [(PPh3)2Cu2(μ-Cl)2(μ-bpe)]∞ 3,were synthe-sized by the multilayer diffusion method,and the structures were refined by single-crystal X-ray diffraction. Complex 1 crystallizes in triclinic,space group P1 with a=9.122(3),b=9.322(3),c=13.201(4),α=106.440(4),β=105.965(5),γ=94.167(5)°,V=1021.3(6) 3,Mr=967.62,Z=1,Dc=1.573 g/cm3,F(000)=486,μ=3.111 mm-1,the final R=0.0383 and wR=0.0960 for 2792 observed reflections (I > 2σ(I)). Complex 2 crystallizes in triclinic,space group P1 with a=9.420(3),b=10.209(4),c=12.407(4),α=104.136(6),β=108.132(5),γ=95.338(6)°,V=1081.0(7) 3,Mr=496.83,Z=2,Dc=1.526 g/cm3,F(000)=500,μ=2.941 mm-1,the final R= 0.0445 and wR=0.1117 for 3251 observed reflections (I > 2σ(I)). Complex 3 crystallizes in triclinic,space group P1 with a=8.32(1),b=11.53(2),c=13.94(3),α=109.57(3),β=93.85(3),γ= 97.28(3)°,V=1242(4) 3,Mr=1074.59,Z=1,Dc=1.436 g/cm3,F(000)=548,μ=1.279 mm-1,the final R=0.0786 and wR=0.1586 for 2266 observed reflections (I > 2σ(I)). The complexes exhibit intensive solid-state photoluminescence tentatively assigned to an admixture of triplet intraligand (IL) and metal-to-ligand charge-transfer (MLCT) excited state.     

Syntheses,Structures, and Photoluminescent Properties of Two 2D Coordination Polymers Based on 1,3-Di(2,4-dicarboxyphenyl) Benzene and 1,3-Di(4-pyridyl)propane

Two new 2D coordination polymers, [Zn(HL)(Hbpp)]n(1) and [Cd(HL)(Hbpp)(H2O)]n(2)(H4L = 1,3-di(2,4-dicarboxyphenyl) benzene, bpp = 1,3-di(4-pyridyl)propane), have been hydrothermally synthesized and characterized by single-crystal X-ray diffraction analysis, elemental analysis, TGA and IR spectroscopy. Complex 1 crystallizes in monoclinic, space group P21/n, with a = 13.1031(6), b = 14.7315(7), c = 15.0041(7) A, β = 91.202(1)°, V = 2895.6(2) A3, Dc = 1.532g/cm3, Mr = 667.97, F(000) = 1376.0, μ = 0.909 mm–1, Z = 4, the final R = 0.0481 and wR = 0.1304 for 7027 observed reflections with I 2σ(I). Complex 2 also belongs to the monoclinic space group P21/n, with a = 13.6326(4), b = 14.6432(4), c = 14.9395(5) A, β = 93.132(1)o, V = 2977.84(16) A3,Dc = 1.613 g/cm3, Mr = 1445.98, F(000) = 733.0, μ = 0.794 mm–1, Z = 2, the final R = 0.0283 and w R = 0.0784 for 7230 observed reflections with I 2σ(I). Both complexes 1 and 2 form 2D net structures, which are further linked to form 3D supramolecular net structures via intermolecular hydrogen bonds and aromatic π-π stacking interactions.     

Syntheses, Crystal Structures and Properties of Two Supramolecules Assembled from Weak Interactions

Two complexes, [Cu2(Htdb)4(H2O)2] (1) and [Cd(bipy)2(Hmcmbc)2] (2) (H2tdb = 2,2-thiodibenzoic acid, H2mcmbc = m-(carboxyl-methyloxy)-benzenecarboxylic acid, bipy = 4,4'-bipyridine), have been prepared, and were characterized by elemental analysis, FT-IR and single-crystal X-ray diffraction. Structures indicate that complex 1 is a single molecule, and 2 is a one-dimensional chain. Their two-and three-dimensional frameworks are constructed through hydrogen bonding, π…π or C–H…π stacking, and such other weak interactions. The cyclic voltametric behavior of complex 1 and luminescence property of complex 2 were investigated. 1 belongs to the triclinic system, space group P with a = 7.8607(6), b = 11.7619(9), c = 15.3481(12) , α = 109.3670(10), β = 92.4420(10), γ = 92.0450(10)°, V = 1335.65(18) 3, Mr = 1256.26, Dc = 1.5619(2) g/cm3, F(000) = 642, μ = 1.029 mm–1, Z = 1, the final R = 0.0289 and wR = 0.0763 for 5199 observed reflections with I > 2σ(I). Complex 2 crystallizes in triclinic, space group P with a = 9.6378(10), b = 9.7508(10), c = 19.055(2) , α = 88.7020(10), β = 80.5260(10), γ = 69.2000(10)o, V = 1649.9(3) 3, Mr = 815.07, Dc = 1.641 g/cm3, μ = 0.732 mm-1, F(000) = 828, Z = 2, the final R = 0.0511 and wR = 0.1149 for 4729 observed reflections (I > 2σ(I)).     

Synthesis and Crystal Structure of a New Mixed-ligand Cluster[Mo3O4(C2O4)2bipy-(H2O3)]·EtOH·2H2O(bipy=2,2'-Bipyridine)

The novel mixed-ligand neutral compound [Mo3O4(C2O4)2·bipy(H2O)3]·EtOH·2H2O (bipy = 2,2'-bipyridine) has been prepared by the reaction of oxalic acid elution of Mo(Ⅳ) and bipy, and characterized by single-crystal X-ray diffraction analysis and IR. The crystal is of triclinic, space groups P1 with a = 9.5520(2), b = 10.3730(1), c = 13.5722(2) (A), α = 74.940(12), β = 80.772(14), γ = 69.898(11)°, V = 1215.73(11) (A)3, Z = 2, C16H24Mo3N2O18, Mr = 820.19, Dc = 2.241 g/cm3, μ = 1.616 mm-1, F(000) = 808, T= 293(2) K, the final R = 0.0424 and wR = 0.0939 for 4119 observed reflections with Ⅰ> 2σ(Ⅰ). The trinuclear unit is coordinated by mixed ligands of oxalate and bipy. The intermolecular hydrogen bonding interactions among adjacent [Mo3O4(C2O4)2·bipy(H2O)3] extend the compound into a therr-dimensional supramolecular framework. The uncoordinated water molecules and ethal molecules act as space-fillers and consolidate the whole architecture through hydrogen bonding interactions.     

Two Co(Ⅱ) Coordination Polymers Based on 3,5-Di(4H-1,2,4-triazole-4-yl)benzoic Acid Ligand: Syntheses,Structures and Magnetic Property

Two Co(Ⅱ) coordination polymers, namely [Co(L)Cl]_n(1) and [Co(L)(CH_3 COO)]_n(2), {HL = 3,5-di(4 H-1,2,4-triazole-4-yl)benzoic acid}, were synthesized under hydrothermal conditions. Compound 1 crystallizes in orthorhombic system, space group Pmma with a = 7.032(5), b = 11.555(8), c = 8.185(5) ?, V = 665.1(7) ?~3, Z = 2, Dc = 1.746 g/cm3~, F(000) = 350, Mr = 349.61, μ = 1.504 mm~(-1), the final R = 0.0568 and w R = 0.1739 for 2312 observed reflections with I 2σ(I). Compound 2 crystallizes in orthorhombic system, space group Pmma with a = 7.7505(17), b = 11.391(3), c = 8.0298(18) ?, V = 708.9(3) ?~3, Z = 2, Dc = 1.748 g/cm~3, F(000) = 378, Mr = 373.20, μ = 1.245 mm-1, the final R = 0.0350 and w R = 0.0873 for 5239 observed reflections with I 2σ(I). Single-crystal X-ray analyses revealed that complexes 1 and 2 exhibit similar 2 D layer structures with uncoordinated carboxyl as dangling arms. The neighboring layers are further connected by these arms, leading to interest 2 D → 3 D polythreading frameworks. Moreover, the magnetic susceptibility study indicates compound 1 exhibits antiferromagnetic behavior.     

A Zinc TTR Complex with a Novel 2-D Structure （TTR = 3-Amino-1H-1,2,4-triazole）

The solvothermal reaction of 3-amino-1H-1,2,4-triazole (ttr) with Zn(ClO4)2·6H2O and NaCl in a 1:1:1 molar ratio gave a new complex [Zn(ttr)Cl]n with a 3-connected (4.82) 2-D struc- ture. The layers stack in the -ABAB- way along the c axis with abundant hydrogen bonding interac- tions to form the crystal structure. The complex [Zn(ttr)Cl]n crystallizes in the orthorhombic space group Pbca with a = 9.369(1), b = 10.049(1), c = 11.905(1) , V = 1120.9(3) 3, Z = 8.00, C2N4H3ZnCl, Mr = 183.90, Dc = 2.180 g/cm3, μ = 4.740 mm-1, F(000) = 720, S = 1.059 and T = 293(2) K. The final R = 0.0662 and wR = 0.2457 for 956 observed reflections with I > 2σ(I), and R = 0.0689 and wR = 0.2504 for all data.