Distinct Hydrogen-bonded M^Ⅱ（H2O）8 Clusters as Second Building Units for 1-D, 2-D and 3-D Supramolecular Architectures （M = Cobalt and Nickel）

Two mononuclear metal-organic complexes, [Co（Hmpdc）2（H2O）4]·4H2O 1 and [Ni（Hfmpdc）2（H2O）4]·6H2O 2, were prepared from 2,6-dimethylpyridine-3,5-dicarboxylic acid （Hzmpdc） and 4-furyl-2,6-dimethylpyridine-3,5-dicarboxylic acid （H2fmpdc） with M（NO3）2 salts, respectively, and characterized by single-crystal X-ray diffraction, elemental analyses, IR spectroscopy, and photoluminescent measurement. Complex 1 crystallizes in triclinic, space group P1 with a = 7.634（5）, b = 8.695（5）, c = 10.757（6）A, α = 69.647（7）, β = 69.957（8）, γ = 83.733（7）°, V = 628.9（7）A^3, Dc = 1. 561 g/cm^3,μ（MoKa） = 0.763 mm^-1, F（000） = 309, Z = 1, the final R = 0.0553 and wR = 0.1469 for 1909 observed reflections （Ⅰ 〉 2σ（Ⅰ））. Complex 2 crystallizes in monoclinic, space group P21/n with a = 9.5934（16）, b = 12.422（2）, c = 14.826（3） A, β = 105.201（2）°, V = 1705.0（5）A3, Dc = 1. 479 g/cm^3,μ（MoKa） = 0.655 mm^-1, F（000） = 796, Z = 2, the final R= 0.0351 and wR = 0.0889 for 2387 obsevved reflections （Ⅰ 〉 2σ（Ⅰ））. In the crystal structures of 1 and 2, diverse supramolecular motifs from 1-D chains/ladders to 3-D networks are constructed from corresponding distinct [M^Ⅱ（H2O）8] ion clusters as the second building units, respectively. The solid state compounds of 1 and 2 show similar photoluminescent spectra with emission maximum at ca.     

Syntheses and Characterizations of Luminescent Complexes [(BINAP)Pt(C≡CC6H4R-p)2] (R = H, 1; CH3, 2) (BINAP = 2,2''-Bis(diphenylphosphino)-1,1''-binaphthyl)

[(BINAP)Pt(C≡CC6H4R-p)2] (R = H, 1; CH3, 2) (BINAP = 2,2'-bis(diphenylphos- phino)-1,1'-binaphthyl) were synthesized and characterized by X-ray crystallography. Complex 1 crystallizes in triclinic, space group P with a = 11.699(3), b = 12.512(3), c = 15.611(4)(A), α = 93.277(3),β= 97.626(2), γ = 97.375(14)o, V = 2239.9(9)(A)3, Mr = 1014.92, Z = 2, Dc = 1.505 g/cm3, F(000) = 1010, μ(MoKα) = 3.244 mm-1, the final R = 0.0338 and wR = 0.0905 for 7738 observed reflections (I > 2σ(I)). Complex 2 crystallizes in monoclinic, space group P21/n with a = 18.03690 (10), b = 13.06060(10), c = 21.6913(3)(A), β= 96.5430(10)o, V = 5076.60(9)(A)3, Mr = 1132.94, Z = 4, Dc = 1.482 g/cm3, F(000) = 2272, μ(MoKα) = 2.973 mm-1, the final R = 0.0481 and wR = 0.0893 for 8916 observed reflections (I > 2σ(I)). Both complexes emit intensively photoluminescence in both solid state and fluid solution due to MLCT (Pt→-C≡CC6H4R-p) emissive state.     

Hydrothermal Synthesis and Crystal Structure of a Cadmium（Ⅱ） Polymer with a Two-dimensional Network Structure： [ Cd（pzdc）（2,2＇-bipy） ]n·nH2O

A metal-organic coordination compound formulated as [Cd（pzdc）（2,2＇-bipy）]n·nH2O 1 （Hzpzdc = pyrazine-2,3-dicarboxylic acid, 2,2＇-bipy = 2,2＇-bipyridine） has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, TG fluorescence spectrum and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P2 1/c with a = 10.8081（13）, b = 14.4328（17）, c = 10.2530（12） A, β = 98.504（2）°, V= 1581.8（3） ]A3, C16H14CdN4O5, Mr= 454.71, Dc = 1.909 g/cm^3, μ（MoKa） = 1.420 mm^-1, F（000） = 904, Z = 4, the final R = 0.0230 and wR = 0.0554 for 2901 observed reflections （I 〉 2σ（I））. It exhibits an interesting two-dimensional network structure and shows yellow photoluminescent property at room temperature.     

From Chain to Layer Structure: ZnⅡ Coordination Polymers Derived from Diphenic Acid

Three ZnⅡ coordination polymers, [Zn(py)(H2O)(dpa)]n 1, [Zn2(4,4'-bipy)2(dpa)2]n 2 and [Zn(bpe)(H2O)2(Hdpa)2]n 3 (py = pyridine, H2dpa = diphenic acid, 4,4'-bipy = 4,4'-bipyridine,bpe = 1,2-bis(4-pyridyl)ethane), were synthesized and characterized by X-ray single-crystal structure determination. 1 crystallizes in monoclinic, space group C2/c with a = 23.014(3), b = 8.7184(13), c = 18.091(3) (A), β = 95.964(3)°, V = 3610.2(9) (A)3, Z = 8, C19H15NO5Zn, Mr = 402.69,Dc= 1.482 g/cm3, F(000) = 1648, μ(MoKα) = 1.389 mm-1, the final R = 0.0431 and wR = 0.1120 for 4239 observed reflections with I ＞ 2σ(Ⅰ). 2 crystallizes in orthorhombic, space group Fddd with a = 23.1613(5), b = 24.0324(6), c = 29.4785(1) (A), V= 16408.4(5) (A)3, Z = 32, C24H16N2O4Zn, Mr = 461.76, Dc= 1.495 g/cm3, F(000) = 7552, μ(MoKα) = 1.232 mm-1, the final R = 0.0542 and wR = 0.1724 for 3632 observed reflections with I ＞ 2σ(Ⅰ). 3 crystallizes in orthorhombic, space group C2/c with a = 19.142(4), b = 13.862(3), c = 15.625(3) (A), β = 122.404(3)°, V = 3500.3(11) (A)3, Z = 8,C20H17NO5Zn0.50, Mr = 384.03, Dc= 1.457 g/cm3, F(000) = 1592,μ(MoKα) = 0.766 mm-1, the final R = 0.0400 and wR = 0.1210 for 4024 observed reflections with I ＞ 2σ(Ⅰ).     

Syntheses and Crystal Structures of Two 3D Zinc(II) Compounds Involving Coordination and Hydrogen Bonds

1 INTRODUCTION Self-assembly through coordination and hydrogen bonds has been proved to be a powerful tool for con- structing functional organic crystalline materials[1~4]. Except for the important role of H-bonds in the sta- bilization of structures, hydrogen bonding groups namely hydroxyl, amide groups in adjacent coor- dination polymeric chains or discrete lamellas can form hydrogen bonds, which allow for the assembly of well-formed crystalline solid[5, 6]. Our recent inte- rest is foc…     

Synthesis and Crystal Structure of a New Zn(II) Nitronyl Nitroxide Complex [Zn(NIT4Py)(PDA)(H2O)3]

1 INTRODUCTION Nitronyl nitroxides, independently or in combina- tion with metal ions, have been one of the most wi- dely studied systems in molecular magnetism for understanding radical-radical or metal-radical inte- ractions as well as for synthesizing organic ferroma- gnets and metal-radical magnetic materials[1～4]. Up to now, lots of metal-radical complexes have been reported[5～8]. On the other hand, cooperative inter- molecular interactions, such as coordination bonds, hydrogen bon…     

Hydrothermal Synthesis, Crystal Structure and Photoluminescent Property of a Metal-organic Coordination Polymer with Supramolecular Structure： [Cd2（dpphen）2（BDC）0.5Cl3]n

A novel metal-organic coordination polymer [Cd2(dpphen)2(BDC)0.5Cl3]n (dpphen = 4,7-diphenyl-1,10-phenanthroline, BDC = terephthalate) 1 has been obtained by using hydrothermal synthesis and characterized by elemental analysis, IR, fluorescence spectrum and single-crystal X-ray diffraction. The complex crystallizes in triclinic, space group P1 with a = 9.981(5), b = 10.436(5), c = 21.104(10) , α = 94.640(7), β = 103.160(7), γ = 92.958(8)o, V = 2127.8(17) 3, C52H34Cd2Cl3N4O2, Mr = 1077.98, Dc = 1.682 g/cm3, μ(MoKα) = 1.237 mm-1, F(000) = 1074, Z = 2, the final R = 0.0314 and wR = 0.0757 for 7358 observed reflections (I > 2σ(I)). Furthermore, compound 1 shows blue photoluminescent property at room temperature.     

Syntheses and Crystal Structures of Methyl 2-（4,5-Dibromo- 1-methylpyrrole-2-carbonylamino）-3-phenyl propanoate and 4,5-Dibromo-1-methyl-2-trichloroacetylpyrrole

1 INTRODUCTION Pyrrole and its derivatives have attracted much attention due to their chemical properties as well as biological activities[1]. They have been widely used as the materials to produce pharmaceutical, essences, biochemicals, etc. It has been found that a great deal of pyrrole derivatives present bioactivities, such as antitumor and antiviral activities[2~5]. Thus, due to the interest in exploring the syntheses of potential bioactive materials which contain pyrrole ring andna…     

A 3-D Supramolecular Network with 1-D Cation Metal.organic Coordination Polymers and Diverse Motifs from Hydrogenbonded [M（H2O）4]-Carboxylates

One-pot solvothermal reaction of Iransition metal Znn salt with 4,4-bipyddyl （bpy） and 1,4-benzenediacrylic add （H2L） in the presence of Et3N generates a three-dimensional （3-D） supramolecular network with 1-D cation metal-organic coordination polymer, [Zn（H20）a（bpy）]-L 1, and structurally characterized by single-crystal X-ray diffraction, elemental analyses, IR spectroscopy, and photoluminescent property. The complex crystallizes in triclinic, space group P1 with a = 7.1291（2）, b = 7.3784（3）, c = 10.5042（3）A, α = 95.049（2）, β = 102.162（2）, 7 = 97.027（3）0, V= 532.38（3）A3, C22H24N2O8Zn, Mr = 509.82, De= 1.590 g/cm3, p（MoKa）= 1.207 ram-l, F（000） = 264, Z = 1,the finalR=O.0438and wR=O.lOll for 1589 observed reflections （I 〉 2σ（I））. In the crystal structure, the second building unit composed of [Zn（H2O）4].L constructs two distinct 2-D supramolecular sheets and a neutral 3-D architecture. The title compound 1 shows strong photoluminescence with emission maximum at 2 = 455 nm upon λex.max = 355 nm.     

Synthesis,Crystal Structure and Anticancer Property of （Z）-N-（4-Bromo-5-ethoxy-3,5-dimethyl-furan-2（5H）-ylidene）-4-methylbenzenesulfonamide

The novel title compound(Z)-N-(4-bromo-5-ethoxy-3,5-dimethylfuran-2(5H)-yli-dene)-4-methylbenzenesulfonamide 1(C15H18BrNO4S) has been unexpectedly synthesized by the aminohalogenation reaction of ethyl 2-methylpenta-2,3-dienoate with TsNBr2,and characterized by mp,IR,1H NMR,EIMS,ESIHRMS and single-crystal X-ray diffraction.It crystallizes in mono-clinic,space group P21/c with a = 11.714(5),b = 14.106(5),c = 10.402(4) ,β = 97.298(8)°,V = 1704.9(12) 3,Mr = 388.27,Z = 4,Dc = 1.513 g/cm3,μ(MoKα) = 2.549 mm-1,F(000) = 792,the final R = 0.033 and wR = 0.062 for 3098 observed reflections(Ⅰ 2σ(Ⅰ)).     

Syntheses and Structure Determination of Two Copper Compounds with 4,4--Sulfonyldibenzoilate Ligands

The two title compounds [Cu(sdba)(py)2(H2O)]n·2n(py) 1 and [Cu(sdba)(phen)(H2O)]n 2(H2sdba = 4,4'-sulfonyldibenzoic acid,py = pyridine,phen = 1,10-phenanthroline) have been synthesized and characterized by single-crystal structure determination,IR and TG analyses.Compound 1 crystallizes in orthorhombic,space group Pbcm with a = 5.9833(12),b = 22.333(5),c = 24.571(5),V = 3283.3(12) 3,Z = 4,C34H30N4O7SCu,Mr = 702.22,Dc = 1.388 g/cm3,F(000) = 1396,μ(MoKα) = 0.780 mm-1,the final R = 0.0599 and wR = 0.1767 for 3416 observed reflections with I > 2σ(I).Compound 2 crystallizes in monoclinic,space group C2/c with a = 22.9549(4),b = 12.2443(3),c = 17.8687(4) ,β = 110.873(1)°,V = 4692.69(18) 3,Z = 8,C26H18N2O7SCu,Mr = 566.02,Dc = 1.602 g/cm3,F(000) = 2312,μ(MoKα) = 1.078 mm-1,the final R = 0.0697 and wR = 0.1330 for 3452 observed reflections with I > 2σ(I).In both structures,the CuII metal centers adopt five-coordination in slightly distorted tetragonal pyramidal geometries,while the second N-donor ligands bond or chelate to CuII ions as the terminal moiety.The weak interactions extend the two structures into high-dimensional supramolecular coordination-polymers.     

Syntheses and Crystal Structures of(H_3O)(C_3H_5N_2)[Mn(OH)_6Mo_6O_(18)]·3.5H_2O and (H_3O)_3[Co(OH)_6Mo_6O_(18)]·7H_2O

1 INTRODUCTION Polyoxometalates, a rich and remarkable classof inorganic cluster system[1], exhibit diverse appli-cation possibilities due to their topological and elec-tronic properties, ranging from their well-known roleas reagents in analytical, b…     

Two Isostructural 2-D Metal(Ⅱ)-organic Coordination Polymers from 4,4'-Bipyridyl and (E)-2,6-Dimethyl-4-styrylpyridine-3,5-dicarboxylic Acid

(E)-2,6-Dimethyl-4-styrylpyridine-3,5-dicarboxylic acid (H2mspda) is firstly employed in coordination chemistry.Two isostructural two-dimensional (2-D) 4-connected metal-organic coordination polymers with a general formula of {M2[(mspda)2(bpy)(H2O)2]}n (M=Zn(1) and Co(2)) are assembled from H2mspda,4,4'-bipyridyl (bpy),zinc and cobalt ions under hydrothermal conditions,and characterized by single-crystal X-ray diffraction analyses.Complex 1 crystallizes in monoclinic,space group P21/n with a=14.551(4),b=10.941(3),c=14.945(4),β=98.817(4)o,V=2351.3(1)3,Dc=1.511 g/cm3,μ(MoKα)=1.090 mm-1,F(000)=1104,Z=4,the final R=0.0335 and wR=0.0485 for 3296 observed reflections (I 2σ(I)).In compound 1,mspda2-spacers are only arrayed in a head-to-tail fashion which corresponds to a 2-D coordination polymer.Solid-state H2mspda and complex 1 have expected photoluminescence (λem=475～496 nm) at room temperature.     

Synthesis and Crystal Structure of Poly{diaqua[N-(2-hydroxybenzyl)-D,L- aspartate]cadmium(II)}

1 INTRODUCTION Coordination-driven supramolecular assembly hasattracted great interest in constructing beautiful mo-tifs and developing new materials[1～5]. It is crucial toselect or synthesize suitable bridging organic li-gands[6～10]. The reduced Schiff base N-(2-hydro-xybenzyl)-D,L-amino acid is an excellent ligand forself-assembly with metal ions, not only due to itsprolific coordination sites but also its strong abilityto afford hydrogen bonding from secondary aminegroup and carbox…     

pH-Dependent Assembly of Hybrid Materials Based on Molybdates and Copper/imidazole Complexes

Three novel inorganic-organic hybrid materials, [Cu（imi）2（H2O）（MoO4）]n 1, [Cuz（imi）3（MoO4）E]n.nH2O 2 and [Cu3（imi）2（OH）2（MoO4）2]n 3 （imi = imidazole）, were synthesized and characterized by X-ray single-crystal structure determination. 1 crystallizes in orthorhombic, space group Pca21 with a = 13.382（4）, b = 8.527（2）, c = 9.622（3）A, V = 1098.0（5） A^3 Z = 4, C6H10CuMoN4O5, Mr = 377.66, Dc = 2.285 g/cm^3, F（000） = 740,μ（MoKa） = 3.095 mm^-1, the final R = 0.0256 and wR = 0.0722 for 1896 observed reflections with I 〉 2σ（I）. 2 crystallizes in monoclinic, space group P2t/c with a= 11.170（2）, b = 7.8244（15）, c = 22.631（4）A, β = 115.790（7）°, V = 1780.9（6）A^3 Z = 4, C9H14Cu2Mo2N6O9, Mr = 669.24, Dc= 2.496 g/cm^3, F（000）=1295,μ（MoKa） = 3.792 mm^-1, the final R = 0.0225 and wR = 0.0615 for 3838 observed reflections with I 〉 2σ（I）. 3 crystallizes in monoclinic, space group P21/c with a = 5.5599（19）, b = 23.771（8）, c = 7.3044（18）A , β = 129.356（16）°, V = 746.5（4）A^3, Z = 2, C6H10Cu3Mo2N4O10, Mr = 680.71, Dc = 3.029 g/cm^3, F（000） = 650,μ（MoKa） = 5.900 mm^-1, the final R = 0.0215 and wR = 0.0524 for 1620 observed reflections with I 〉 2σ（I）.     

Synthesis and Crystal Structure of CoCl（ieaa）（C10H7—ieai）（C10H7NH2）

1 INTRODUCTION A number of isonitroso-b-diketones and isonitroso-b-ketoesters such as isonitrosoacetyl- acetone(Hiaa), isonitrosobenzoylacetone(Hiba) and isonitrosoethylacetoacetate (Hieaa) have been employed as reagents in spectrophotometric determination of iron, palladium and ruthenium[1]. Transition metal complexes of such ligands[2] are potential models for metal binding sites in ferroverdin[3]. They were found as dyes and light-absorbing agents for the acceleration of the sol…     

A Cadmium(II) Coordination Polymer:Crystal Structure and Fluorescent Property of [CdCl2(4,4''-bipyridine)]∞

The reaction of L-histidine,CdCl2(2.5H2O and 4,4'-bipyridine in methane/water gave rise to a two-dimensional coordination polymer [CdCl2(4,4'-bipyridine)]( which has been characterized by single-crystal X-ray diffraction.The polymer crystallizes in the orthorhombic sys-tem,space group Cmmm with a = 12.083(7),b = 11.771(7),c = 3.781(2)(A),V = 537.8(6)(A)3,Z = 2,C10H8N2CdCl2,Mr = 339.48,Dc = 2.097 g/cm3,F(000) = 328 and μ(MoKα) = 2.490 mm-1.The final R = 0.0658 and wR = 0.1398 for 257 observed reflections with I≥2σ(I).     

Syntheses,Crystal Structures and Properties of Three New Complexes [Ni（C9N2O2H7）2（CH3OH）2],[Zn（C9N2O2H7）2（H2O）2] and [Cd（C9N2O2H7）2（CH3OH）2]

Three novel metal-organic complexes with formulas [Ni(C9N2O2H7)2(CH3OH)2](1),[Zn(C9N2O2H7)2(H2O)2](2) and [Cd(C9N2O2H7)2(CH3OH)2](3) were synthesized by the reactions of Ni,Zn and Cd salts with ethyl 2-benzimidazolylacetate under hydrothermal conditions or layering technique,and characterized by single-crystal X-ray diffraction analysis,IR spec-troscopy,solid-state luminescent properties and thermogravimetric(TG) analysis.The crystal data for these three complexes are as follows:for 1,monoclinic,space group P21/c,a = 9.384(3),b = 9.634(3),c = 11.292(3) ,β = 95.787(5)°,V = 1015.7(5) 3,Z = 2,F(000) = 492,Dc = 1.547 Kg/m3,μ = 1.002 mm-1,the final R = 0.0451 and wR = 0.0900 for 1833 observed reflections with Ⅰ 2σ(Ⅰ);for 2,orthorhombic,space group Pbca,a = 10.031(4),b = 10.379(4),c = 17.525(7),V = 1824.6(12) 3,Z = 4,F(000) = 928,Dc = 1.645 Kg/m3,μ = 1.392 mm-1,the final R = 0.0452 and wR = 0.0996 for 1661 observed reflections with Ⅰ 2σ(Ⅰ);for 3,monoclinic,space group P21/c,a = 9.9114(13),b =10.4852(15),c = 10.4120(14) ,β = 108.453(5)°,V = 1026.4(2) 3,Z = 2,F(000) = 532,Dc = 1.705 Kg/m3,μ = 1.110 mm-1,the final R = 0.0322 and wR = 0.0805 for 1822 observed reflections with Ⅰ 2σ(Ⅰ).In the three complexes,the ethyl 2-benzimidazolylacetate shows the same chelating mode,and the adjacent units are interlinked into a two-dimensional layer through hydrogen-bonds(O-H···O,N-H···O).     

Synthesis and Crystal Structure of a Lanthanum(III) Complex with Chelidamic Acid

A new lanthanum complex, (H3O)2[La(C7H3NO5)2(H2O)2]2·3(H2O) or (H3O)2[La(HChel)2(H2O)2]2·3(H2O) 1 (H3Chel = 4-hydroxypyridine-2,6-dicarboxylic(chelidamic) acid), has been prepared by the hydrothermal reaction, and its crystal structure was determined based on single-crystal diffraction data. Compound 1 crystallizes in triclinic, space group P with a = 9.6939(19), b = 10.176(2), c = 11.502(2) (A), α = 111.52(3), β = 93.74(3), γ = 103.33(3)°, V = 1013.0(3) (A)3, Dc = 1.912 g/cm3, Z = 1, Mr = 1166.40, μ = 2.188 mm-1, λ(MoKα) = 0.71073 (A) and F(000) = 574. The final R = 0.0342 and wR = 0.0737 for 4080 observed reflections with I > 2σ(I), and R = 0.0429 and wR = 0.0772 for all data. Compound 1 contains two lanthanum ions, four chelidamic acid ligands, four coordinated water molecules, two hydroniums, and three discrete water molecules. The LaIII atom is ten-coordinated by four oxygen and two nitrogen atoms from two tridentate chelating chelidamic acid ligands, two carboxylic oxygen atoms from an adjacent chelidamic acid ligand and two coordinated water molecules, leading to a distorted dodecahedral geometry. A three-dimensional network is formed by H-bonds.     

Syntheses and Crystal Structures of Two Gd（Ⅲ） Hydrogen Supramolecules Based on p-Sulfonatothiacalix[4]arene

Two novel polymeric complexes, [Gd（HsTCAS）（H2O）7]·4H2O 1 and [Gd（HsTCAS） （CH3COCH3）（H2O）6]·6H2O 2 （H4TCAS = p-sulfonatothiacalix[4]arene）, have been synthesized and characterized by single-crystal X-ray diffraction analyses. Complex 1 crystallizes in monoclinic, space group C2/m with a = 20.2308（12）, b = 19.0894（10）, c = 12.2448（7）A, β = 101.847（3）°, V = 4628.1（5）A^3, C24H43GdO27S8, Mr = 1169.25, Z = 4, Dc = 1.690 g/cm^3, F（000） = 2380,μ = 1.879 mm^-1, the final R = 0.0404 and wR = 0.1038 for 5127 observed reflections with I 〉 2σ（I）. Complex 2 is pseudo-isostructural with complex 1.