Synthesis and Crystal Structure of [Mn（DPMT）2Cl2（H2O）2]

The title compound [Mn(DPMT)2Cl2(H2O)2] (DPMT = 1-[[2-(2,4-dichlorophenyl)- 1,3-dioxolan-2-yl]methyl]-1H-1,2,4-triazole) was synthesized by the reaction of MnCl2·4H2O and DPMT in ethanol solution and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a = 23.913(4), b = 7.8883(13), c = 8.6291(14) , β = 95.816(3)o, V = 1619.4(5) 3, Z = 2, C24H26Cl6MnN6O6, Mr = 762.15, Dc = 1.563 g/cm3, μ = 0.950 mm-1, S = 1.045, F(000) = 774, R = 0.0462 and wR = 0.0981. The molecular structure is a centrosymmetric conformation, and two ligands are symmetrically located on both sides of the Mn atom. The manganese atom is surrounded by two nitrogen atoms from ligands, two chlorine atoms and two oxygen atoms from water molecules to form a slightly distorted octahedral geometry.     

Hydrothermal Synthesis, Crystal Structure and Electrochemical Properties of Complex Mn2（phen）2（p-CBA）4（H2O）

One novel complex Mn2(phen)2(p-CBA)4(H2O) has been hydrothermally syn- thesized from p-chlorobenzoic acid (p-CBA), 1,10-phenanthroline (phen) and anhydrous man- ganese(Ⅱ) sulfate and then characterized. Crystal data for this complex: monoclinic, space group C2/c, with a = 2.3416(3), b = 1.5604(2), c =1.5605(2) nm, β = 121.048(2)o, V = 4.8849(12) nm3, Dc = 1.510 g/cm3, Mr = 555.26, Z = 8, μ = 0.798 mm-1, F(000) = 2256, GOOF = 1.032, the final R = 0.0393 and wR = 0.0816. The crystal structure shows that two neighboring manganese(Ⅱ ) ions are linked together by two bridge-chelating p-chlorobenzoic groups and one bridging water molecule, forming a cage structure with the Mn–Mn bond distance of 0.3512 nm. Each manganese(Ⅱ ) ion is coordinated by two nitrogen atoms of one 1,10-phenanthroline molecule and four oxygen atoms from three p-chlorobenzoic acid anions and one water molecule, giving a distorted octahedral coordination geometry. The cyclic voltammetric behavior of the complex was also investigated.     

Synthesis, Crystal Structure and Electrochemical Properties of [Ni(phen)3]·(m-nitrobenzoic acid)2·(H2O)

A new nickel(Ⅱ) coordination complex [Ni(phen)3]·(m-nitrobenzoic acid)2·(H2O) was synthesized by self-assembly of m-nitrobenzoic acid, 1,10-phenanthroline and nickelous perchlorate. It crystallizes in the monoclinic system, space group C2/c, with a = 2.4596(6), b = 1.2124(3), c = 1.9824(5) nm, β = 97.088(5)°, V = 5.866(3) nm3, Dc = 1.474 g/cm3, Z = 4, Mr = 1301.82, μ(MoKα) = 0.417 mm-1 F(000) = 2688, R = 0.0493 and wR = 0.1025. Structural determination indicates that the nickel(Ⅱ) ion is coordinated with six nitrogen atoms from three phens, giving a distorted octahedral coordination geometry. The cyclic voltametric analysis shows that the electron transfer in the electrode reaction is irreversible.     

Synthesis and Crystal Structure of Mn（phen）（PhCOO）2（H2O）

1 INTRODUCTION During the last decade the manganese che- mistry has aroused great interest due to its diverse redox functions of enzymes in photosystem Ⅱ and its specially structural, magnetic and spectroscopic properties[1, 2]. A lot of manganese complexes involving carboxylate ligands have been reported, and their properties been fully explored[3, 4]. The coordination environment of the manganese site in biosystem often consists of oxygen and nitrogen atoms from the carboxylate groups…     

Synthesis, Crystal Structure and Electrochemical Properties of a One-dimensional Chain Coordination Polymer [Mn（phen）（2,4,6-TMBA）2（H2O）]n

A one-dimensional chain-like coordination polymer [Mn(phen)(2,4,6-TMBA)2(H2O)]n has been synthesized from 2,4,6-trimethylbenzoic acid, 1,10-phenanthroline and anhydrous manga- nese(Ⅱ ) sulfate and then characterized. Crystal data for this complex: tetragonal, space group I41, a = 2.05643(16), b = 2.05643(16), c = 1.3939(2) nm, V = 5.8946(11) nm3, Mr = 579.54, Z = 8, Dc = 1.306 g/cm3, μ(MoKα) = 0.490 mm-1, F(000) = 2424, S = 0.985, the final R = 0.0411 and wR = 0.0950. The Flack factor is -0.01(2). The crystal structure shows that two neighboring man- ganese(Ⅱ ) ions are linked together by one bridge-chelating 2,4,6-trimethylbenzoic group, forming a one-dimensional chain structure. The manganese(Ⅱ ) ion is coordinated with two nitrogen atoms of one 1,10-phenanthroline, three oxygen atoms from three 2,4,6-trimethylbenzoic acids and one water oxygen atom, giving a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex was also investigated.     

Synthesis and Crystal Structure of 4-（4-Bromophenyl）- 3,4-dihydro-6-methyl quinolin-2（1H）-one

The title compound (C16H14BrNO) has been synthesized by the reaction of p-tolylamine, Meldrum’s acid and 4-bromo-benzaldehyde, and its structure was characterized by IR, 1H NMR and X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P21/n with a = 7.6850(11), b = 8.3004(11), c = 21.301(3) , β = 95.110(2)°, V = 1353.4(3) 3, Mr = 316.19, Z = 4, Dc = 1.552 g/cm3, μ(MoKα) = 3.028 mm-1, F(000) = 640, the final R = 0.0345 and wR = 0.0768. X-ray analysis reveals that the atoms of C(1), C(2), C(3), C(4), C(5) and N(1) form a six-membered ring of boat conformation.     

配合物[Mn(2,2''-bipy)(H2O)4]·(m-phth)的水热合成和晶体结构

A mononuclear manganese complex [Mn(2,2'-bipy)(H2O)4]·(m-phth) (2,2'-bipy=2,2'-bipyridine, m-phth=isophthalate) has been synthesized by hydrothermal methods. The crystal structure was determined by singlecrystal X-ray diffraction. The crystal is of orthorhombic, space group Pnna with a=0.766 8(8) nm, b =2.050 2(2)0.027 0, R=0.028 0 and wR=0.075 5. In the crystal the manganese atom is six-coordinated by two nitrogen atoms from 2,2'-bipyradine and four oxygen atoms from water molecules, completing an octahedral coordination geometry. The isophthalate molecules are included in the lattice and connected to Mn(2,2'-bipy)(H2O)4 by hydrogen bonding interactions to form a three-dimensional supramolecular structure. CCDC:286965.     

Synthesis and Crystal Structure of an Inclusion Compound Mn(SCN)2(H2O)4(2C6H12N4

A mononuclear manganese complex Mn(SCN)2(H2O)4(2C6H12N4 (C14H32O4N10MnS2, C6H12N4 = hexamethylenetetramine) has been synthesized. The molecular and crystal structures were determined by single-crystal X-ray diffraction. The crystal is of tetragonal, space group P42/mnm with a = 9.5591(7), b = 9.5591(7), c = 13.8253(15) (A), V = 1263.31(19) (A)3, Z = 2, Mr = 523.56, Dc = 1.376 g/cm3, μ = 0.727 mm-1, F(000) = 550, Rint = 0.0302, T = 293(2) K, R = 0.0380 and wR = 0.1184 for 549 observed reflections with I > 2σ(I). In the crystal the manganese atom is six-coordinated by two nitrogen atoms from isothiocyanato anion and four oxygen atoms from water molecules, completing an octahedral geometry. Hexamethylenetetramine molecules are included in the lattice and connected to Mn(SCN)2(H2O)4 by hydrogen bonding and S...S interac- tions to form a three-dimensional supramolecular architecture.     

Synthesis, Crystal Structure and Electrochemical Properties of One-dimensional Chain Coordination Polymer [Co(Ⅱ)(C6H5CH=CHCOOH)2(4,4''-bipy)(H2O)5]n

A one-dimensional chain coordination polymer [Co(Ⅱ)(C6H5CH=CHCOOH)2(4,4'-bipy)(H2O)5]n has been synthesized with cinnamylic acid, 4,4'-bipy and cobaltous chloride as raw materials. Crystal data for this complex: monoclinic, space group P21/c, a - 1.1481(3), b =1.1230(2), c = 1.1759(3) nm, β = 97.054(4)°, V = 1.5046(6) nm3, Mr= 617.50, Dc = 1.363 g/cm3, Z= 2, μ(MoKα) = 0.627 mm-1, F(000) = 646, S = 1.062, R 0.0443 and wR = 0.1178. The crystal structure shows that two neighboring cobalt(Ⅱ) ions are linked together by one 4,4'-bipy, and the whole complex molecule adopts a one-dimensional chain structure. Each cobalt(Ⅱ) ion is coordinated with two nitrogen atoms from two 4,4'-bipy molecules and four oxygen atoms from four water molecules, giving a distorted octahedral coordination geometry. The electrochemical properties were analyzed by combining with the crystal structure.     

Hydrothermal Synthesis, Crystal Structure and Electrochemical Properties of Complex Zn（phen）（m-CBA）2（H2O）

A novel complex Zn(phen)(m-CBA)2(H2O) with m-chlorobenzoic acid (m-CBA), 1,10-phenanthroline (phen) and zinc chloride has been hydrothermally synthesized and characterized. Crystal data for this complex: triclinic, space group P1, a = 0.8361(5), b = 1.2455(7), c = 1.3107(7) nm, α = 115.637(8), β = 91.014(9), γ = 104.857(8)o, V = 1.1763(11) nm3, Dc = 1.623 g/cm3, Z = 2, F(000) = 584, GOOF = 1.078, the final R = 0.0453 and wR = 0.1192. Structure analysis shows that the zinc ion coordinates with two nitrogen atoms of one 1,10-phenanthroline molecule, three oxygen atoms from two m-chlorobenzoic acid molecules and one water molecule, giving a distorted square-pyramidal coordination geometry. The cyclic voltametric behavior of the complex was also investigated.     

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)).     

配合物[Mn(phendione)(PDC)(H2O)2]·2H2O的合成与晶体结构

The title compound [Mn(phendione)(PDC)(H₂O)₂]·2H₂O (H₂PDC=pyridine-2，6-dicarboxylic acid) has been prepared in aqueous solution and characterized by single X-ray diffraction structure determination， elemental analysis， IR spectroscopy， and thermal analyses. The compound crystallizes in Monoclinic system， space group C2/c， a=1.017 51(11) nm， b=1.483 25(11) nm， c=1.461 21(13) nm， β=109.86(10)°， V=2.074 1(3) nm³， Z=4， F(000)=1 028， μ=0.701 mm^-1， D_c=1.609 g·cm^-3， R₁=0.028 9， wR₂=0.078 8 [I>2σ(I)]. Crystal structure reveals that complex consists of one-dimensional chain framework bridged by hydrogen bonds that formed by uncoordinated water and oxygen atom of carboxyl group in PDC^2-. Furthermore， the complexes form a three-dimensional super-molecular structure through hydrogen bonds. CCDC: 648570.     

配合物[Mn(C13H8N2OBr)2(C5H5N)2]·3C5H5N的结构与磁性研究

The complex [Mn(C₁₃H₈N₂OBr)₂(C₅H₅N)₂]·3C₅H₅N has been synthesized and characterized by X-Ray diffraction, IR and variable temperature (～10 to ～278K) magnetic susceptibility. X-Ray diffraction result for the single crystal shows that the crystal belongs to monoclinic, space group P2₁/c, a=1.0969(3)nm, b=2.0903(5)nm, c=2.0481(6)nm, β=97.366(6), V=4.657(2)nm³, Z=4, D_c=1.47g·cm^-3。     

三元混配配合物[Ni(PMBP-sal)(py)]的合成、表征与晶体结构

合成了混配配合物[Ni(PMBP-sal)(py)]，(PMBP：1-苯基-3-甲基-4-苯亚甲基吡唑啉酮-5，sal：水杨酰肼，py：吡啶)，并用元素分析，IR光谱，紫外可见吸收光谱，循环伏安和单晶X-射线衍射进行表征。结构分析表明N-(1-苯基-3-甲基-4-苯亚甲基吡唑啉酮-5)-水杨酰肼和吡啶与Ni(Ⅱ)配位形成略微畸变的平面正方形化合物。     

Synthesis and Crystal Structure of 2-p-Methyloxyphenyl- 3a-（2-phenyl-1,2,3-triazole-4-yl）-3,4-dihydro-1,2,4- oxa-diazolo[4,5-d][1,5] Benzothiazepine

The title compound2-p-methyloxyphenyl-3a-(2-phenyl-1,2,3-triazole-4-yl)-3,4- dihydro-1,2,4-oxa-diazolo[4,5-d][1,5] benzothiazepine (C31H25N5O2S, Mr = 531.63) has been syn- thesized and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P1 with a = 10.888(2), b = 15.115(3), c = 16.702(3), α = 99.90(3), β = 95.21(3), γ = 100.41(3)o, V = 2642.1(9) nm3, Dc = 1.336 g/cm3, Z = 4, F(000) = 1112, μ = 0.162 mm-1 ,λ(MoKα) = 0.071073 nm, R = 0.0357 and wR = 0.1126 for 10620 observed reflections with I > 2σ(I). X-ray analysis reveals that the molecular backbone consists of a tricyclic system with the central seven- membered ring in a twisted boat-like conformation.     

Synthesis and Crystal Structure of [NdCl5(THF)]2-[HO-4,6-di-tBu-C6H2-2-CH2{CH(iPrNCHCHN)}]2+·THF

The title complex 1·THF has been synthesized by the reaction of [HO-4,6-di-tBu-C6H2-2-CH2{CH(iprNCHCHN)}]Cl with NdCl3 in a 2:1 molar ratio in THF, and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/c with a =9.6501(14), b = 16.393(2), c = 36.745(6) (A), β = 97.444(4)°, V = 5763.7(15)(A)3, Mr= 1124.69, Z =4, Dc= 1.296 g/cm3, μ(MoKa) = 1.175 mm-1, F(000) = 2348, the final R = 0.0729 and wR =0.1762 for 8735 observed reflections with I ＞ 2σ(1). Complex 1 consists of an anion [NdCl5(THF)]2- and two cations [HO-4,6-di-tBu-C6H2-2-CH2{CH(iprNCHCHN)}]2 to form a layer structure by the interconnection of anions and cations via hydrogen bonding. The central metal Nd in the anionic unit is coordinated by five Cl atoms and one oxygen atom from solvated THF molecule assuming a distorted octahedral geometry.     

Solvothermal Synthesis, Crystal Structure and Electrochemical Property of Complex [Co(p-MBA)2(2,2''-bipy)(H2O)]·(H2O)

One novel complex [Co(p-MBA)2(2,2'-bipy)(H2O)]·(H2O) has been synthesized by the reaction of p-methylbenzoic acid with 2,2'-bipyridine in the solvent mixture of water and methanol. It crystallizes in triclinic, space group P-1 with a=0.70479(14), b=1.1211(2), c=1.6718(3) nm, α=103.806(3), β=90.795(3), γ=104.207(3)°, V=1.2399(4) nm3, Mr=512.41, Dc=1.373 g/cm3, Z=2, F(000)=532, μ=0.733 mm-1, R=0.0432 and wR=0.0957. The crystal structural analysis shows that the cobalt atom is coordinated with three oxygen atoms from two p-methylbenzoic acids and one water molecule and two nitrogen atoms from one 2,2'-bipyridine,forming a distorted square-pyramidal coordination geometry. The cyclic voltammetry behavior of the complex is also reported.     

Synthesis and Crystal Structure of the Polyoxometalatebased Complex [Mn（DMSO）5H2O]2SiMo12O40

1 INTRODUCTION The design and assembly of organic-inorganic solid-state materials with active physical properties, such as materials with electrical, magnetic and opti- cal properties, has become a focus of a great deal of interest in recent years[1, 2].…     

Synthesis and Crystal Structure of a Model for the Active Sites of Fe-only Hydrogenases： [Fe2（SCH2）2N（3-PhCF3）（CO）6]2

A model compound for the active sites of Fe-only hydrogenases,[Fe2(SCH2)2N(3-PhCF3)(CO)6]2,has been synthesized and structurally characterized by single-crystal X-ray diffraction.It crystallizes in tetragonal,space group P43,with a = 12.6324(3),b = 12.6324(3),c=24.0453(12) (A),V = 3837.1(2) (A)3,Z = 4,Fe4S4N2C30O12F6H16,Mr= 1062.09,Dc= 1.839 g/cm3,μ(MoKa) = 1.791 mm-1,F(000) = 2112,T= 293(2) K,Flack = 0.034(9),R= 0.0282 and wR =0.0685 for 8148 observed reflections with I ＞ 2σ(I).In the title compound,each Fe1 atom is coordinated by three terminal carbonyl C atoms (Fe-C:1.783(3)～ 1.816(3)(A)),two bridging S atoms (Fe-S:2.2609(7)～2.2757(8)(A)) and another Fe atom (Fe-Fe 2.5011(5) (A)),adopting a distorted octahedral geometry with trans angles ranging from 152.45( 11 ) to 157.77(10)°.     

4-羧基苯氧乙酸锰配位聚合物[Mn(p-CPOA)(H_2O)_3]_n的合成与晶体结构

0引言由于羧酸化合物具有丰富的配位结构类型,而且羧酸桥联多核配合物广泛存在于生物体内金属蛋白和金属酶的活性部位,使其在配位化学中占有重要地位[1]。尤其是近年来,研究发现羧酸配位聚合物具有潜在的光学、磁学、吸附分离、信息储存以及催化等性能,使得由苯二甲酸,均苯三甲