Syntheses and Crystal Structures of Two New Iron-sulfur Carbonyl Complexes: [Fe2(SC6H4Cl)2(CO)6]·0.5(Et2O) and [Fe3(SC6H4NH2)6(CO)6]·2(MeOH)

Two new iron-sulfur carbonyl complexes, [Fe2(SC6H4Cl)2(CO)6]·0.5(Et2O) 1 and [Fe3(SC6H4NH2)6(CO)6]·2(MeOH) 2, have been prepared and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. Crystal data for 1: monoclinic, C2/c, a = 18.4439(8), b = 11.0999(5), c = 25.1830(10)(A), β = 97.0370(10)o, V = 5116.8(4)(A)3, Z = 8, C20H13Cl2Fe2O6.50S2, Mr = 604.02, Dc = 1.568 g/cm3, μ = 1.540 mm-1, F(000) = 2424, the final R = 0.0545 and wR = 0.1454 for 3443 observed reflections with I > 2σ(I); 2: monoclinic, P21/n, a = 12.350, b = 26.3050(11), c = 16.057(A),β = 97.891(3)°, V = 5166.9(2)(A)3, Z = 4, C44H44Fe3N6O8S6, Mr = 1144.76, Dc = 1.472 g/cm3, μ = 1.128 mm-1, F(000) = 2352, the final R = 0.0442 and wR = 0.1197 for 7978 observed reflections with I > 2σ(I). Complex 1 contains one iron dimer, in which two tricarbonyliron(I) fragments are bridged together by two 4-chlorophenylthiolate ligands, whereas complex 2 contains a linear tri-iron cluster, in which two terminal tricarbonyliron(II) fragments and the central Fe(II) atom are linked together by six 4-aminophenylthiolate bridging ligands.     

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 Ternary Mixed Ligand Complex [Cu（ampym）（bapa）Cl]（ClO4） （ampym = 2-Aminopyrimidine, bapa = Bi（3-aminopropyl）amine）

1 INTRODUCTION The pyrimidine substructure plays a vital role in physiological system. It occurs not only in organisms such as nucleic acids, vitamins and coenzymes[1~3], but also frequently presents in commercially availa- ble drugs such as antibiotics, antiatherosclerotic and antihypertensive agent[4, 5]. Studying the interaction of pyrimidine derivatives and metal ions is important as a means of understanding the role of pyrimidine ring in biological systems. This paper describes the …     

Syntheses and Crystal Structures of Zinc(II) and Nickel(II) Complexes Involving Reduced Nitroxide Radicals

1 INTRODUCTION The synthesis of new molecular magnetic mate- rials that combine transition metal ions and pure organic radicals as ligating sites has attracted much more attention in the last few years[1~4]. Nitronyl ni- troxide radicals, independently or in combination with metal ions, have been one of the most studied systems in molecular magnetism for understanding the radical-radical or metal-radical interactions as well as for synthesizing organic ferromagnets and metal-radical magne…     

Synthesis and Crystal Structure of a New Glycinato Copper Compound

1 INTRODUCTION Amino acids (AA) are some of the most important biological ligands, and metal ions are known to par- ticipate in a variety of biological reactions, therefore, research on the coordination behavior of metal-ami- no acid complexes is one of the most essential ele- ments of chemical biology[1, 2]. For over three deca- des their structures have been of considerable inte- rest and importance in coordination chemistry[2, 3]. Studies of these relatively simple complexes may en- ha…     

Syntheses and Crystal Structures of Two Isomeric Au Complexes

<正>Two new isomeric Au complexes,Au(PPh_3)(bmt),have been synthesized via the reaction of Au(PPh_3)Cl with 2-benzimidazolethiol(Hbmt)in dichloromethane(CH_2Cl_2)solution. Their crystal structures were determined by elemental analysis and single-crystal X-ray diffraction studies.Complex 1 crystallizes in the monoclinic system,space group C2/c with a=19.589(2),b= 21.1368(15),c=23.424(2)(?),β=108.346(4)°,V=9206.1(14)(?)~3,M_r=1216.85,D_c=1.756 g/cm~3,μ=6.566 mm~(-1),F(000)=4704,Z=8,the final R=0.0563 and wR=0.1028 for 8125 reflections with I2σ(I).Complex 2 crystallizes in the monoclinic system,space group P2_l/n with a= 9.627(3),b=21.384(8),c=22.308(8)(?),P=92.068(6)°,V=4590(3)(?)~3,M_r=1216.85,D_c=1.761 g/cm~3,μ=6.585 mm~(-1),F(000)=2352,Z=4,the final R=0.0500 and wR=0.0883 for 10477 reflections with I2σ(I).X-ray diffraction studies reveal that complexes 1 and 2 both feature a 1D chain along the a axis.     

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.     

Synthesis and Crystal Structure of a New Mononuclear Copper( Ⅱ ) Complex: [Cu(BMI)_4(SO_4)]·DMF·2H_2O

A new copper(II) complex, [Cu(BMI)4(SO4)]·DMF·2H2O (BMI = benzimida- zole), has been synthesized by the treatment of CuCN with 2-mercaptobenzimidazole in the presence of 1,10-phenanthroline, and characterized by single-crystal X-ray diffraction. It crystalli- zes in monoclinic, space group P21/n with a = 17.6260(4), b = 11.1252(3), c = 18.6573(4)(A),β = 107.9010(10)°, V = 3481.45(14)(A)3, Z = 4, C31H35CuN9O7S, Mr = 741.28, F(000) = 1540, Dc = 1.414 g/cm3, μ = 0.746 mm-1, the final R = 0.0649 and wR = 0.1609 for 4382 observed reflections with I > 2σ(I). The Cu(II) atom is coordinated by five unidentate ligands (one sulfate and four benzimidazole ligands) generated in situ, displaying a slightly distorted square pyramid geometry.     

Syntheses and Crystal Structures of Molybdenum-Sulfur Clusters Mo_3S_4 (dtp)_3(o-CH_3OC_6H_4COO)(Py) and Mo_3S_4 (dtp)_3(p-HOC_6H_4COO)(DMF)·EtOH

1 INTRODUCTION Recent years have seen a drastic increase of compounds containing the Mo3S4 core. A major synthetic route to these compounds is by the reaction of the aqua ion [Mo3S4(H2O)9]4+ with different kinds of ligands replacing some or all of the water molecules. In this way, Mo3S4(dtp)4(H2O), which was synthesized by the spontaneous- assembly method in 1986[1] and its structural characterization and chemical reactivity have been well recognized [2], can be rationally synthesize…     

Syntheses and Crystal Structures of Ternary Complexes of Zinc(Ⅱ) and Cadmium(Ⅱ) with 3-Aminobenzoic Acid and 1,10-Phenanthroline

Two new ternary complexes [Zn(3-aba)2(phen)](2.58H2O 1 and {[Cd(3-aba)- (phen)2]·(NO3)·(1.5H2O)}n 2 (3-aba = 3-aminobenzoic acid anion, phen = 1,10-phenanthroline) were synthesized and characterized by elemental analysis, IR, UV spectrum and X-ray diffraction. Complex 1 crystallizes in the rhombohedral system, space group R with a = 3.5733(3), b = 3.5733(3), c = 1.1231(2) nm, V = 12.419(3) nm3, C26H25.17N4O6.58Zn, Mr = 564.37, Z = 18, F(000) = 5253, μ = 0.937 mm-1, Dc = 1.358 g/cm3, R = 0.0668 and wR = 0.1690 for 2424 observed reflections (I > 2σ(I)). Complex 2 belongs to the tetragonal system, space group P4/ncc with a = 2.88451(10), b = 2.88451(10), c = 1.55571(11) nm, V = 12.9441(11) nm3, C31H25CdN6O6.50, Mr = 697.97, Z = 16, F(000) = 5648, μ = 0.727 mm-1, Dc = 1.433 g/cm3, R = 0.0607 and wR = 0.1742 for 3468 observed reflections (I > 2σ(I)). Complex 1 displays a mononuclear structure. The carboxylate group of 3-aminobenzoic acid anion coordinates to Zn(Ⅱ) in a chelating bidentate mode, and the nitrogen atom of the ligand does not involve in coordination. Complex 2 exhibits a one-dimensional chain structure with 3-aminobenzoic acid anion coordinating to Cd(Ⅱ) in a μ2-bridging mode through its nitrogen atom and one of its oxygen atoms.     

Cadmium(II)-1,4-phenylenediacetate Complex with Green Luminescence

1 INTRODUCTION The design and construction of coordination fra- meworks are of great interest due to their intriguing structural motifs and potential applications as func- tional materials[1～4]. Many interesting fra-meworks with different dimensionalities have been obtained through self-assembly of selected metal centers and tailored ligands[5, 6]. Among them, dicarboxylate ligands, such as terephthalate[7, 8], isophthalate[9～12] and succinate[13, 14], are often used as bridges to bond m…     

Blue Luminescent Zinc(II)-and Cadmium(II)-1,4-phenylenediacetate Complexes

1 INTRODUCTION The crystal engineering and design of solid-state coordination polymers have become a very attrac- tive field in recent years[1～4]. Many interesting fra- meworks with intriguing potential applications have been obtained through the self-assembly of selected metal centers and carboxylate ligands[5, 6]. Compared with aromatic carboxylate ligands such as terephtha- lic acid[7, 8], benzene tricarboxylic acid[9, 10], benzene tetracarboxylic acid[11, 12] and so on, those ligands …     

Syntheses and(Crystal Structures of Two New One-dimensional Double Hydrogen-bonding-chain Complexes [Ni(bipy)2Cl]·ClO4 and [Zn(bipy)2Cl]·BF4

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)(A), β= 93.021(2)o, V = 2031.9(4)(A)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) (A), β = 104.57(1)o, V = 2025.7(12) (A)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, Crystal Structure and Thermal Property of a Manganese(II) 4-Carboxyphenoxyacetate Complex

1 INTRODUCTION Organic aromatic carboxylic acids which com-monly possess multiple coordination modes are ex-cellent candidates for constructing supramolecularmetal complexes[1～6]. 4-Carboxyphenoxyacetic acid(4-CPOAH2), widely used in biological activitystudies, is a multidentate flexible ligand that not onlyhas versatile binding possibilities but also can formregular hydrogen bonds as both hydrogen-bond donorand acceptor. However, there have been few reportson the coordination chemistr…     

Synthesis and Crystal Structure of 2-Ethoxy-spiro[2H-1, 4,2-benzoxazaphosphorine-3（4H）, 1＇-Cycloheptane] 2-Oxide

1 INTRODUCTION α-Aminophosphonates are an important class of compounds since they are considered as structural analogues of the corresponding α-amino acids. Their utilities as enzyme inhibitors, antibiotics, pharma- cological agents and many other applications are well documented[1~5]. Moreover, cyclic α-amino- phosphonates, one important kind of α-aminopho- sphonates, have attracted chemists’ interests for a long time[6~11]. In order to search for potent and selec- tive herbicides a…     

Synthesis and Crystal Structure of a Copper(II) Compound Constructed by N-(4,6- Dimethoxylpyrimidin)-N'-(ethoxycarbonyl)thiourea

A copper(Ⅱ) complex Cu(L)2(NO3)2 constructed by the L (L = N-(4,6-dime- thoxylpyrimidin)-N'-(ethoxycarbonyl)thiourea) ligand crystallizes in monoclinic, space group C2/c with a = 16.2416(16), b = 9.1385(7), c = 22.0008(18) (A),β = 108.077(2)°, V ＝ 3104.3(5)(A)3, Dc = 1.627 g/cm3, Z = 4, C20H28CuN10O14S2, Mr = 760.18, μ(MoKα) = 0.920 mm-1, F(000) = 1564, R = 0.0471 and wR = 0.1284 for 2239 observed reflections (I > 2σ(I)). X-ray diffraction shows the existence of weak complementary intramolecular N-H…O (DA) hydrogen bonds which further strengthen the coordination from the two L ligands with the Cu(II) ion, intermolecular C-H…O hydrogen bonds and weak π…π stacking interactions, leading to the formation of a multi-dimen- sional supramolecular network.     

Syntheses and Crystal Structures of [Ni(L)2(NCS)2] and [Co(L)2(NCS)2] (L = Azobis(2-pyridine)

1 INTRODUCTION The synthesis of new organic-inorganic hybrid compounds is a relatively new research area that has developed rapidly in the last several years[1]. Bische- late ligand[2, 3], such as azobis(2-pyridine), is a novel tetradentate ligand expect…     

Hydrothermal Synthesis and Structure of [Mn(C8H5NO4)·H2O]n·2nH2O

A novel 5-aminoisophthalate compound, [Mn(C8H5NO4)(H2O]n(2nH2O 1, has been synthesized by the hydrothermal assembly of 5-aminoisophthalic acid with manganese acetate. Ele- mental analysis, X-ray crystal structure analyses, IR spectra, FT-Raman and ESR were carried out for the structural determination and characterization of the title compound. Compound 1 crystallizes in triclinic, space group Pī with a = 7.7562(2), b = 8.6121(3), c = 8.7107(2)(A), α = 85.411(2), β = 76.030(2), γ = 66.510(2)o, V = 517.76(3)(A)3, MnC8H11NO7, Mr = 288.12, Z = 2, Dc = 1.848 g/cm3, μ = 1.300 mm-1, F(000) = 294, R = 0.0381 and wR = 0.1043 for 1652 observed reflections (I > 2σ(I)).     

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.     

Blue Luminescent Zinc(Ⅱ)- and Cadmium(Ⅱ)-1,4-phenylenediacetate Complexes

Two mixed-ligand polymeric complexes formulated as {[Zn(pda)(bpy)]·0.5H2O}n (pdathermally synthesized. Single-crystal X-ray diffraction analyses reveal that the structures of complexes 1 and 2 possess similar one-dimensional zigzag chains. Crystal data for compound 1: monoclinic, space group P21/c, a = 15.965(2), b = 8.305(1), c = 14.856(2) (A),β= 1 1 1.048(2)°, Mr = 422.73, V= 1838.2(4) A3, Z= 4, Dc = 1.528 g/cm3, μ = 1.368 mm-1, F(000) = 868, the final R = 0.0783 and wR= 0.1469 (w=1/[σ2(Fo2) + (0.035 1p)2+ 8.0014P], where P = (Fo2+ 2Fc2)/3) based on 2025 observed reflections with I ＞ 2σ(I); and those for compound 2: monoclinic, space group C2/c, a = 29.921 (7), b= 8.5400(17), c = 15.320(3) (A),β= 99.59(3)°, Mr = 487.75, V = 3859.9(14) A3, Z = 8, Dc = 1.668g/cm3, μ = 1.169 mm-1, F(000) = 1936, the final R = 0.0723 and wR = 0.1612 (w = 1/[σ32(Fo2 ) +(0.0681p)2+ 55.9577P], where P = (Fo2+ 2Fc2)/3) based on 2130 observed reflections with I ＞ 2σ(I).Fluorescent analyses show that both complexes exhibit intense blue luminescence (λmax = 485 nm for 1and 475 nm for 2) upon excitation at 330 nm.