Synthesis and Crystal Structure of a New Copper(II) Complex with 4-Cyanobenzoic Acid

A new Cu（Ⅱ） complex [Cu（4-cba）（1,10-phen）（H2O）2]（NO3） （4-Hcba = 4-cyanobenzoic acid） has been synthesized by solvothermal reaction in an ethanol/water mixed solution at 100 ℃ and structurally characterized by single-crystal X-ray diffraction. Crystallographic data： C20H16CuN4O7, Mr= 487.91, triclinic, space group PI, a = 7.8420（2）, b = 9.1070（2）, c = 15.1140（6） A, a = 76.889（9）, β = 81.332（11）, γ = 74.844（ 11）°, V = 1009.89（5） A^3, Z = 2, Dc = 1.605 g/cm^3, F（000） = 498, μ = 1.134 mm^-1, the final R = 0.0379 and wR = 0.0865 for 2977 observed reflections with 1 〉 2σ（Ⅰ）. The Cu（Ⅱ） atom is coordinated by two terminal water molecules, one chelating 1,10-phen molecule and one monodentate 4-cba ligand to form a slightly distorted square pyramid. The title complex molecules are connected through hydrogen bonds and π-π stacking interactions to generate a 2D layered network. The thermogravimetric analysis of the title complex has also been discussed.

Synthesis and Crystal Structure of a Copper(II) Complex with 2,4-Dihydroxybenzylidene Benzoylhydrazone Ligand

A new copper（Ⅱ） complex with formula CuL（py）, where L^2- is the dianion of 2,4-dihydroxybenzylidene benzoylhydrazone, has been synthesized and characterized by IR spectra and single-crystal X-ray diffraction method. The crystal belongs to monoclinic, space group P2 1/c with a=0.9630（4）, b=1.4808（6）, c=1.2320（5） nm, β=104.969（6）°, V=1.6973（Ⅱ） nm^3, Z=4, Dc=1.553 g/cm^3,μ（MoKa）=1.311 mm^-1, F（000）=812, R=0.0694 and wR=0.1727 for 1511 observed reflections （I〉2σ（I））. The crystal structure analysis indicates that the copper（Ⅱ） ion lies in a distorted square-planar environment composed of two oxygen atoms, one nitrogen atom from the tridentate acylhydrazone Schiff base ligand L^2- and one nitrogen atom from the pyridine ligand. Two adjacent molecules are connected via weak Cu…O bonding interactions to form dimers, which are further linked to generate a two-dimensional layer structure via interdimeric hydrogen bonds.

Synthesis and Crystal Structure of a Binuclear Gadolinium（Ⅲ） Complex Bridged by Cucurbit[6]uril

A new cucurbit[6]uril bridsed binuclear complex {[Gd（H2O）6]2[Q6（H2O）]}C16·4H2O, where Q6 represents cucurbit[6]uril, has been synthesized and characterized by X-ray diffraction. The crystal structure shows that the complex has an extended cucurbit[6]uril-bridged structure consisting of two gadolinium（Ⅲ） ions, in which each gadolinium（Ⅲ） ion is coordinated with two neighboring carbonylic oxygen atoms of Q6 and six oxygen atoms of water molecules that leans toward one side of the portal. One disordered guest water molecule resides in the Q6 molecule cavity and occupies two different positions. Hydrogen bonds assemble the complcx to threedimensional supramolecular structure.

Synthesis, Crystal Structure and Properties of a Copper Complex with the Bicycle[2.2.1]-2-heptene-5,6-dicarboxylic Acid

A new copper complex 2{Cu（C10H8N2）[C8H11O2（COO）]（H2O）3}·（H2O）5 with bicycle[2.2.1]hept-2-en-5,6-dicarboxylic acid（H2L） [C7H8（COOH）2], basic copper carbonate and 2,2＇-bipyridine has been synthesized in the mixed solvents of methanol and water. It crystallizes in the triclinic system, space group P1, with a = 7.4626（5）, b = 11.9779（8）, c = 12.9841（8）A, α = 109.7040（10）, β = 98.7550（10）, γ = 90.6240（10）°, V = 1077.50（12）A3, Dc = 1.538 g/cm^3, Z = 1, F（000） = 520, GOOF = 1.065, R = 0.0360 and wR = 0.0950. The copper ion is coordinated with four oxygen atoms from one H2 L molecule and three water molecules together with two nitrogen atoms from the 2,2＇-bipyridine molecule, forming a distorted octahedral coordination geometry. The thermal stability and electrochemical properties were also studied.

Synthesis and Crystal Structure of the Copper Complex {[Cu(CH_3COO)_2(bbtz)](H_2O)_2}_n

The new copper complex { [Cu（CH3COO）2（bbtz）]（H2O）2 }, 1 （bbtz = 1,4-bis（ 1,2,4- triazol-1-ylmethyl）benzene） was synthesized and the structure was determined by single-crystal X-ray diffraction. Crystal data： C16H22CuN6O6, monoclinic, space group P21/n, a = 12.589（5）, b = 6.455（2）, c = 12.677（5） A, β= 98.748（9）°, V= 1018.2（7） A^3, Mr = 457.95, Z = 2, Dc= 1.494 g/cm^3, F（000） = 474, μ = 1.118 mm^-1, R = 0.0463 and wR = 0.0939 for 1971 observed reflections with I 〉 2σ（I）. The crystal structure of 1 is a one-dimensional chain via the bridging flexible ligand bbtz.

Synthesis and Crystal Structures of the α and β Forms of Bis(salicylaldoxime)copper(Ⅱ) Complexes

Modified α and β bis(salicylaldoxime)copper(Ⅱ) have been obtained by recrystallization from ethyl acetate(CCDC Nos. 212157 & 212158). The X-ray analysis reveals that the two modificated forms have the same structure with different geometric parameters. The α form crystallizes in the P2(1)/c space group and the β form in the P1 space group. Both the crystal structures consist of centrosymmetric monomeric molecules of Cu(OC_6H_4CNOH)_2. The IR spectra are in agreement with the structural data.

Synthesis, Crystal Structure and Characterization of Energetic Monovalent Copper Azide Complex: [Cu_2(dmpz)(N_3)_2]_n

A novel cuprous azide complex with the formula of [Cu2（dmpz）（N3）2]n（1, dmpz： 2,6-dimethylpyrazine） has been synthesized through hydrothermal synthesis with the reducibility of H3PO3 and structurally characterized by single-crystal X-ray diffraction method. Single-crystal X-ray diffraction analysis reveals the title complex represents a three-dimensional network structure featuring 2D [Cu N3]n plane units bridged by bridging dmpz ligands to form a 3D network. Research results reveal that 1 has lower impact sensitivity and friction sensitivity, which may be expected to become insensitive energetic material and have potential applications. Crystal data： monoclinic, space group C2/c, a = 17.8599（15）, b = 8.2889（5）, c = 14.8076（14） A, β = 113.2580（10）o, V = 2014.0（3） A3, Z = 8, S = 1.025, the final R = 0.0303, w R = 0.0825 for 1460 observed reflections with I 2σ（I） and R = 0.0386, wR = 0.0870 for all reflections. In addition, elemental analysis, IR, and sensitivity characterization are presented.

Syntheses and Crystal Structures of Mono-and Binuclear Copper(Ⅱ) Mixed-ligand Complexes Involving Schiff Base

The mononuclear copper（Ⅱ） complex [Cu（L）（2-AP）] 1 and binuclear copper（Ⅱ） complex [Cu（L）（py）]2 2 （L = C10H11O5NS, taurine o-vanillin, py = prydine, 2-AP = 2-aminopyridine） with mixed ligand have been synthesized and characterized by X-ray diffraction method. Crystal data for 1： orthorhombic, space group Pbca with a = 11.921（4）, b = 15.816（6）, c = 17.076（6） A, V= 3219.7（19） A^3, C15H17CuN3O5S, Z = 8, Mr = 414.92, De = 1.712 g/cm^3,μ（MoKα） = 1.520 mm^-1, F（000） = 1704, the final R = 0.0300 and wR = 0.0705 for 2840 observed reflections with I 〉 2σ（I）; and crystal data for 2： monoclinic, space group P21/c with a = 7.929（3）, b = 17.038（5）, c = 11.734（4） A, β = 98.162（6）°, V = 1569.1（9） A^3, C15H16CuN2O5S, Z = 4, Mr = 399.90, Dc = 1.693 g/cm^3, F（000） = 820,μ（MoKα） = 1.554 mm^-1, the final R = 0.0351 and wR = 0.0848 for 2767 observed reflections （I 〉 2σ（I））. The molecular structure of complex 1 consists of one tetra-coordinated Cu（Ⅱ） atom generating a slightly distorted square plane, and a one-dimensional chain structure is formed by intermolecular hydrogen bonds. Complex 2 consists of a diphenolic hydroxyl O-bridged binuclear copper（Ⅱ） structure. The crystal structures of complexes 1 and 2 reveal that the coordinate copper centers are bound to both nitrogen and oxygen atom donors. The usual N,O-trans arrangement of ligands is observed in both cases.

Synthesis and Crystal Structure of Binuclear Copper (Ⅱ) Complex Containing (Dimethylaminomethyl)ferrocene

A binuclear complex including ferrocenyl, Cu2{Fe(C5H5)[C5H4CH2N(CH3)2]}2 (CH3COO)4, was synthesized and characterized by X-ray diffraction. The title complex crystallizes in triclinic, space group P with a = 8.2779(8), b = 9.4830(8), c = 12.262(1) ? = 81.079(5), b = 80.620(4), g = 78.960(4), V = 924.4(1) 3, Z = 1, C34H46Cu2Fe2N2O8, Mr = 849.51, Dc = 1.526 g/cm3, l(MoK) = 0.71073 ? ?= 1.954 mm-1, F(000) = 438, R = 0.0297 and wR = 0.0901. Both cyclopentadienyl rings in each dmaf (dmaf = (dimethylaminomethyl)ferrocene, Fe(C5H5)- [C5H4CH2N(CH3)2]) have an eclipsed conformation. The binuclear molecule has a crystallographic centrosymmetry; four acetates and two Cu atoms form a cage structure with the distance between two neighboring Cu atoms of 2.655(1) .

Synthesis and Crystal Structure of a Novel Hexanuclear Copper-indium Thiolate Complex [(InCl)_2(OMe)(μ-OMe)_2(μ_3-OMe)(μ-SPr^n)_2(CuPPh_3)]_2

A novel hexanuclear copper-indium thiolate complex, [（InCl）2（OMe）（μ-OMe）2（μ- OMe）（μ-SPrn）2（CuPPh3）]2 1, was synthesized from the reaction of NaSPrn, InCl3 and [Cu（Me- CN）a][PF6] in the presence of Ph3P and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P211n with a = 11.3533（8）, b = 15.4939（11）, c = 20.5189（14） A, β = 98.577（2）°, V = 3569.0（4） A3, Z = 2, C56H82Cl4Cu2In4O8P2S4, Mr = 1801.56, Dc = 1.676 g/cm3,μ（MoKa） = 2.213 mm^-1, F（000） = 1796, S = 0.985, the final R = 0.0559 and wR = 0.1099 for 8878 observed reflections with I 〉 2σ（I） and 367 variables. Complex 1 consists of two CuPPh3 fragments which symmetrically side-attach to the tetranuclear core of [InaCl4（OMe）2（μ-OMe）a（μ- OMe）2（μ-SPrn）4] by coordinating with sulfur atoms of propane-thio moieties. The average In-Ot （terminal）, In-μ-O and In-μ3-O bond distances are 2.305（4）, 2.144（4） and 2.294（4） A, respectively.

Synthesis and Crystal Structure of a Copper(II) Complex with Benzilic Acid and 1,10-Phenanthroline

A new complex [Cu（phen）3][（C6H4）2C（OH）COO]2·6H2O was prepared by selfassembly of benzilic acid, 1,10-phenanthroline （phen）, and copper perchlorate. It crystallizes in triclinic, space group P1-, with a = 1.14661（17）, b = 1.6455（2）, c = 1.6457（2） nm, α= 74.779（2）, β = 74.904（3）, γ = 84.424（3）°, V = 2.8914（7） nm^3, Dc = 1.340 g/cm^3, Z = 2, F（000） = 1218, GOOF = 1.018, the final R = 0.0643 and wR= 0.1633. The crystal structure shows that the copper ion is coordinated with six nitrogen atoms from six 1,10-phenanthroline molecules, forming a distorted octahedral coordination geometry.

Synthesis and Crystal Structure of 1-D Chain Copper(Ⅱ) Complex: [Cu(L)Cl_2]_n (L=2,5-Di-2-pyridyl-1,3,4-oxodiazole)

The title complex, [Cu(L)Cl2]n (L = 2,5-di-2-pyridyl-1,3,4-oxodiazole) 1, has been obtained from the reaction of 3,6-di-2-pyridyl-1,2,4,5-tetrazine (bptz) and CuCl2?H2O in a mixture solvent of CH3CN and CH2Cl2 (L is generated from the metal-assisted hydrolysis reaction of bptz) and structurally characterized. It crystallizes in space group C2/c of monoclinic system with cell parameters: a = 9.812(2), b = 12.679(3), c = 11.111(2) ? b = 103.92(3)? V = 1341.6(5) 3, Z = 4, Dc = 1.776 g/cm3, Mr = 358.66, F(000) = 716, ?= 2.024 mm1 and S = 1.004. The final R = 0.0346 and wR = 0.0938 for 1011 observed reflections with I > 2(I). The Cu(Ⅱ) ion is six-coordinated by four N atoms of two L ligands and two Cl ions in a distorted octahedral geometry. The ligand L acts as a bis-bidentate ligand to bridge the Cu(Ⅱ) ions, resulting in an infinite chain structure.

Synthesis, Magnetic Property and Crystal Structure of a Ytterbium-Copper Mixed Metal Complex:Yb_2Cu_3L_6·6H_2O (L=O(CH_2COO)_2)

Reaction of hydrated ytterbium nitrate and copper nitrate with diglycolic acid at pH= 7 produced a new Yb-Cu mixed metal complex, Yb2Cu3L6. 6H2O(L= O(CH2COO)2). Complex Yb2Cu3O36C2H36 (Mr= 1437. 23) crystallized in hexagonalP6/mcc (No. 192) with cell parameters of a= 14. 344 (3), c= 15. 470(7) A,V= 2757(2) A 3; Z= 2; F(000) = 1390; Dcalc.= 1- 731 g/cm3 μ(MoKa) =45. 8 cm-1. The final agreernent factors are R= 0. 077 and Rw = 0.089 for 867 observed reflections with I>3δ(I). It has been characterized by elemental analysis, IR spectrum, magnetic measurement and X-ray crystallography. In the complex, the Yb3+ ion is 9-coordinated tothree ether oxygen and six carboxylate oxygen atoms from three ligands, the copper ionis coordinated to four oxygen atoms from four carboxylate groups of four ligands andtwo water molecules. The Yb3+ ions and the Cu2+ ions are connected by the carboxylate groups of the ligands, thus resulting in the formation of the complicated networkstructure.

Synthesis and Crystal Structure of a Novel Copper (II) Complex with Acetylenedicarboxylate and 2, 2′-Bipyridine

The title compound [Cu （ADC） （2, 2＇-bipy）]n （ADC = C2 （COO）2^2.） was prepared and characterized by elemental analysis, IR spectroscopy, X-ray analysis, respectively. The analysis of the crystal structure reveals that the copper atom is five-coordinated with two nitrogen atoms of 2, 2＇-bipy and three oxygen atoms of different acetylenedicarboxylate dianions. ADC as bridging ligands link the Cu （Ⅱ） ions, forming coordination polymer structure.

Hydrothermal Synthesis and Crystal Structure of Binuclear Copper(Ⅱ) Complex Bridged by 1,2,4,5- Benzenetetracarboxylato Trivalent Anion

The title complex [(phen) 2Cu(Htcb)Cu(phen) 2]H 3tcb(tcb=1,2,4,5-benzenetetracarboxylato tetravalent anion; phen=1,10-phenanthroline) was synthesized by the hydrothermal synthesis method. The crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in the triclinic system with space group P1, a=1.04174(8) nm, b=1.07119(8) nm, c=1.26360(10) nm, α=98.169(2)°, β=99.679(10)°, γ=93.658(10)°, V=1.37031(18) nm3, Z=1. The two copper(Ⅱ) cations are bridged by Htcb in the monodentate fashion, and have the same five-coordinated environment completed by the four N atoms from the two phen molecules and one O atom from the carboxylic group of Htcb respectively, which can be best described as distorted trigonal-bipyramid geometry. Moreover, the three dimensional network is formed by H-bonding interactions [O…O distance from 0.2506(10) nm to 0.3176(11) nm] and π-π stacking interactions between the phen rings of adjacent binuclear entities with a face-to-face separation of ca. 0.354 nm.

Synthesis and Crystal Structure of Copper(II) Complex with N-Acetoxyl-picolinamide

Using Cu(II) as the template, a complex {[Cu2L2(H2O)2]·4H2O}n (L = N-acetoxyl- picolinamide) has been successfully synthesized and characterized by single-crystal X-ray diffrac- tion. The crystal is of monoclinic, space group C2/c, with a = 24.144(5), b = 7.1622(14), c = 17.283(4) ?, C16H24Cu2N4O12, Mr = 591.47, β = 131.73(3)o, V = 2230.3(8) ?3, Z = 4, Dc = 1.761 g/cm3, F(000) = 1208, μ = 1.978 mm?1, R = 0.0400 and wR = 0.1099. The copper (II) ion is five- coordinated with a distorted square pyramidal geometry. The complex can be viewed as a one- dimensional chain structure by carboxylic bridges among copper atoms. In the complex there exist hydrogen bonding interactions to stabilize the structure.

X-ray Crystal Structure of a Mononuclear Copper (Ⅱ) Complex with Unusual Monodentate O-coordination of Carboxylate Group of Isonicotinate

Reaction of Cu(ClO4)2'6H2O with tripodal ligand tri s (2-benzi nd dazol yl methyl ) aInine(ntb) and sodium isonicotinate (Iso) yielded a mononuclear complex lCu(ntb)(lso)]ClO4.3.5H2O. Thestructure has been established by X-ray crystallography The Cu (Ⅱ) atom is in a distorted trigonalbipyranddal environment with three benzimindazole N atoms of ntb defining the equatorial plane, oneandne N atom of ntb, and one O atom of the carboxylate group of isonicotinate occupying the axialpositions.

Syntheses and Crystal Structures of Two Copper(II) Complexes Derived from Bidentate Schiff Bases

Two new Cu（Ⅱ） complexes have been synthesized with two different bidentate N2O2 donor Schiffbase ligands HL1 （2-（（E）-（4-chlorophenylimino）methyl）-6-bromo-4-chlorophenol） and HL2 （2-（（E）-（2-chlorophenylimino）methyl）-6-bromo-4-chlorophenol）, respectively. Both complexes 1 and 2 have been characterized by elemental analysis and single-crystal X-ray diffraction studies. Structural studies reveal that in both complexes the metal centers are four-coordinated with N202 donor set of Schiff base ligands. Complex 1 belongs to the tetragonal system, space group P4（3）2（1）2 with a = 10.2379（2）, b = 10.2379（2）, c = 24.9623（90） A, V = 2616.41（12） A^3, Z = 4, Dc = 1.908 g/cm^3,μ（MoKa） = 4.3327 mm^-1, F（000） = 1468, S = 0.999, the final R = 0.0345 and wR = 0.0835 for 3506 unique reflections （Rint= 0.0428） with 3249 observed ones （I 〉 2σ（I））. Complex 2 is of monoclinic system, space group P21/c with a = 11.064（3）, b = 9.437（2）, c = 13.277（4） A, fl = 108.997（3）°, V = 1310.8（6） A^3, Z = 2, Dc= 1.904 g/cm^3,μ（MoKa） = 4.319 mm^-1, F（000） = 734, S = 0.997, the final R = 0.0282 and wR = 0.0619 for 3491 unique reflections （Rint = 0.0428） with 2777 observed ones （I 〉 20（I））. The units of the complex are linked via weak interactions, such as C-H…Br hydrogen bonds together with Cl…C1 and Cu…Cl interactions, leading to the formation of one-dimensional chain and two-dimensional network and stabilizing the crystal structure.

Synthesis and Crystal Structure of a Copper(II) Complex with α-Hydroxylated Acid, [Cu(C_(14)H_8O_3)(C_5H_(13)NO)(H_2O)].0.5H_2O

The complex monoaqua[(9-hydroxy-fluorene-9-carboxylato)(N,N-Dimethylisopro- panolamine)]copper(II) semihydrate, Cu(C14H8O3)(C5H13NO)(H2O)]0.5H2O (Mr = 417.93), crystallizes in triclinic system, space group P with a = 9.846(2), b =12.419(3), c =16.781(3)? =75.55(3), b = 75.00(3), g = 84.58(3), V =1918.5(7)?, Z = 4, F(000) =872, Dc=1.45g/cm3 and m= 1.17mm-1. The final R and wR are 0.0481 and 0.1427 for 7099 observed reflections, respectively. The coordination polyhedron around the copper atom is a distorted square pyramid, the basal plane consisting of one carboxyl oxygen atom and one -hydroxylated oxygen atom from a 9-hydroxy-fluorene-9-carboxylato ligand, one nitrogen atom and one oxygen atom from the N,N-dimethylisopropanolamine ligand; while the axial coordination site is occupied by a water oxygen atom with a Cu-O bond length of 2.428(3)?

Synthesis and Crystal Structure of Bis(barbiturato)triwater Complex of Copper(Ⅱ)

The crystal structure of the bis(barbiturato)triwater copper(Ⅱ) complex formulated as Cu(barb)2(HO2)3 (barb = barbiturato) has been determined by single-crystal X-ray diffraction. The analysis was carried out by direct and Fourier methods and the structure was refined by full-matrix least-square computations. The title compound crystallizes in orthorhombic, space group Fdd2 with a = 11.691(1), b = 30.200(4), c = 7.1901(9) , V = 2538.7(5) 3, Z = 8, C8H12CuN4O9, Mr = 371.76, Dc = 1.945 g/cm3, m(MoKa) = 1.781 mm-1, F(000) = 1512, the final R = 0.0347 and wR = 0.0766 for 827 observed reflections (I > 2s(I)). The copper atom is square- pyramidally bonded to the exocyclic oxygen atoms of the barbital anions (CuO, 1.976(3)) and the water molecules (CuO, 1.926(4) and 2.164(7) ?. The molecules are held together to form an extensive three-dimensional network via OH贩稯 and NH贩稯 hydrogen-bonded contacts.