Crystal Structure of Di[bis(diphenylphosphino)propane]Copper(Ⅰ) Perchlorate Complex

1INTRODUCT1oNIthasbeenwellknownthatthereactionofcopper(E)saltswithditertiaryphosphinesorarsinesisoftenaconvenientroutetocopper(I)analogues.8-dimethylarsinoquinolinee,3-methylthiopropyldimethylarsineand(o-diphenylarsi-nophenyl)diphenylphosphinesulphideallonlyyieldcopper(I)complexesofthiskindofligandsfromreactioninvolvingcopper(I)salts.Insimilarmanner,copper(I)nitratecomplexesofstoichiometryCu(dppm)(NO,),Cu2(dppe)3(NO,)2,Cu-(dppe),(NO,),andCu(dppe)(NO,)havebeenprepared.ltappearsthatthe…     

Synthesis,Crystal Structure and Magnetochemistry of a Novel Trinuclear Iron Complex [Fe 3 O(ClC 6 H 4 CO 2 ) 6 (H 2 O) 2.5 (C 2 H 5 OH) 0.5 ]ClO 4 ·0.5H 2 O

A novel trinuclear iron complex was synthesized in ethanol solution, [Fe 3 O(ClC 6 H 4 CO 2 ) 6 (H 2 O) 2.5 (C 2 H 5 OH) 0.5 ]ClO 4 ·0.5H 2 O. The title complex crystallizes in the tetragonal system, space group $P_{4_1}$     

Crystal Structure and Interaction with DNA of [Ni(phen)(mal)(H2O)2]·3H2O

A new complex [Ni(phen)(mal)(H2O)2]·3H2O (phen = 1,10-phenanthroline,mal2-= malonic acid) has been synthesized by the reaction of nickel nitrate,phen and malonic acid.EA,IR spectra and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure of the title complex.Crystal data:monoclinic system,space group P2/c,a =8.937(3),b = 12.163(5),c = 9.725(3)(A),β = 119.36°,C15H19N2O9Ni,Mr= 430.03,Z = 2,F(000) =446,V = 921.3 (A)3,Dc = 1.550 g/cm3,μ = 1.104 mm-1,-10≤h≤ 10,-12≤k≤ 14,-11 ≤l≤7,R =0.0261 and wR = 0.0609 for 4376 (Rint = 0.0203) independent reflections and 1631 observed ones (I＞ 2σ(I)).Ni(Ⅱ) exhibits an octahedral coordination geometry,with hydrogen bonds and π-π interactions stabilizing the whole structure.UV spectrum of the complex interacting with protamine DNA indicates that the title compound interacts with DNA via insertion mode with bonding constant Kb of 1.11 × 104.     

Synthesis and Crystal Structure of a Cyano-bridged Bimetallic Complex [La(betaine)2(H2O)6Fe(CN)6]·2H2O

The title complex [La(betaine)2(H2O)6Fe(CN)6](2H2O (betaine = (CH3)3NCH2CO2) has been synthesized and characterized by X-ray single-crystal structure analysis. The crystal crystallizes in monoclinic, space group P21/n with a = 15.793(5), b = 8.927(3), c = 22.257(7) (A), β = 110.147(5)°, C16H38FeLaN8O12, Mr = 729.31, Z = 4, V = 2946.0(15) (A)3, Dc = 1.640 g/m3, μ(MoKα) = 1.988 mm-1, F(000) =1476, R = 0.0388 and wR = 0.0827 for 4237 observed reflections (I > 2σ(I)). The La3+ ion is nine-coordinated by one cyano nitrogen atom and eight oxygen atoms of two betaine and six water molecules. Each complex molecule is connected to form a 3D network structure by some O-H…O and O-H…N hydrogen bonds.     

Synthesis and Crystal Structure of a Two-dimensional Framework Supramolecular Complex [Mn(phen)(DPZDA)(H2O)]·2H2O

A novel two-dimensional supramolecular complex [Mn(phen)(DPZDA)(H2O)]·2H2Ohas been synthesized by the reaction of Mn(CH3COO)2, 1,10-phenanthroline (phen) and H2DPZDA (3,5-dimethyl-pyrazine-2,6-dicarboxylic acid). Elemental analysis, IR spectra and X-ray singlecrystal diffraction were carried out to determine the composition and crystal structure of the title complex. Crystal data: triclinic system, space group P-1, a = 7.7474(13), b = 9.3381(15), c =15.146(3)(A), α = 93.872(3), β = 102.451(11), γ = 105.261(11)°, C20H20MnN4O7, Mr = 483.34, Z = 2,F(000) = 498, V = 1023.2(3)(A)3, Dc = 1.569 g/cm3, μ = 0.697 mm-1, -9≤h≤9, -11 ≤k≤ 10, -18≤l≤12, R = 0.0365 and wR = 0.0901 for 3585 independent reflections (Rint = 0.0165) and 2923observed reflections (I ＞ 2σ(I)). Structural analysis indicates that Mn(Ⅱ) adopts a distorted octahedral geometry. The 2-D framework supramolecular structure of the title complex is constructed from hydrogen bonds and π…πinteractions.     

Synthesis and Crystal Structure of the Binuclear Complex: [Cu2(phen)2(ip)(Hip)2]·4H2O

A binuclear complex [Cu2(phen)2(ip)(Hip)2]·4H2O has been synthesized by the reaction of Cu(CH3COO)2·H2O, phen(1,10-phenanthroline) and isophthalic acid (H2ip) under hydrothermal condition. Elemental analysis, IR spectra and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure. Crystal data for this complex: monoclinic, space group C2/c, a = 19.214(3), b = 10.6973(14), c = 22.567(3) (A), β = 105.081(2)°,C24H19N2O8Cu, Mr= 526.95, Z = 8, F(000) = 2160, V= 4478.6(10)(A)3, Dc = 1.563 g/cm3, μ = 1.030mm-1, -24≤h≤16, -13 ≤k≤ 13, -28≤l≤28, R = 0.0369 and wR = 0.0819 for 4615 (Rint = 1.0357)independent reflections and 3290 observed ones (I＞ 2σ(Ⅰ)). Structural analysis shows that coordination geometry of Cu(Ⅱ) is a planar square, and the title complex exhibits a 2-D framework supramolecular structure by hydrogen bonds and π-π stacking interactions.     

Synthesis and Crystal Structure of a [Cu(HTren)Cl2]ClO4·H2O Complex (Tren = Tris(2-aminoethyl)amine)

The title complex [Cu(HTren)Cl2]ClO4·H2O (Tren = tris(2-aminoethyl)amine) was crystal (CuC6H21Cl3N4O5) is of triclinic, space group P-1, with a = 8.2689(2), b = 8.4503(3), c=11.6801(4)(A), a = 96.9350(10), β= 108.2440(10), γ = 90.7550(10)°, V= 768.32(4)(A)3, Z= 2, Mr=399.16, Dc= 1.725 g/cm3,μ= 1.962 mm-1, F(000) = 410, T= 293(2) K, the final R = 0.0479 and wR = 0.1339 for 2659 observed reflections with I ＞ 2σ(I). X-ray single-crystal structure analysis reveals that the copper(Ⅱ) atom adopts a slightly distorted square-pyramidal geometry. The distances between Cu and N atoms (N(1), N(2), N(3)) range from 1.975(4) to 2.116(3)(A). The bond lengths of Cu-Cl(1) and Cu-Cl(2) are 2.309(10) and 2.591(10) (A), respectively. The whole crystal presents a three-dimensional network structure by hydrogen bonds.     

Synthesis and Crystal Structure of a New Iron Complex with Cyclic Water Hexamers [Fe(CDTA)(H_2O)]·[Fe(1,10-phen)_3]·10H_2O·2OH

The title complex [Fe(CDTA)(H2O)]·[Fe(1,10-phen)3]·10H2O·2OH (CDTA = transcyclohexane-1,2-diamine-N,N,N,N′-tetraacetate) has been prepared and characterized by single-crystal X-ray diffraction analysis. The crystal adopts space group P with a = 12.793(4), b = 14.104(5), c = 17.880(5), V = 2792.2(1)3, Dc = 1.459 g/cm3, C50H66Fe2N8O21, Mr = 1226.81, F(000) = 1284, μ = 0.604 mm-1, Z = 2, R = 0.1055 and wR = 0.2581 for 8675 observed reflections (I > 2σ(I)). X-ray crystallography analysis exhibits that the title compound consists of two crystallographically independent molecules [Fe(CDTA)(H2O)] and [Fe(1,10-phen)3], and they are connected through O-H···O hydrogen bonds and π···π stacking interactions forming a 3D supramolecular structure. Interestingly, there is a cyclic water hexamer with chair conformation in this complex.     

Disordered Crystal Structure of Bis[(2.2.2-Cryptand)Sodium] Bis[Aqua(Isothiocyanato)(μ-Isothiocyanato)Sodium] 2[Na(2.2.2-Crypt)]+ · [Na2(NCS)2(μ-NCS)2(H2O)2]2–

Crystals of bis[(2.2.2-cryptand)sodium] bis[aqua(isothiocyanato)(-isothiocyanato)sodium]: 2[Na(C₁₈H₃₆N₂O₆)]⁺ · [Na₂(NCS)₂(-NCS)₂(H₂O)₂]^2– (I) were synthesized and studied by X-ray diffraction analysis. The disordered structure of I (a = 12.715 Å, b = 10.458 Å, c = 21.767 Å, = 102.56°, space group P2₁/n) was solved by the direct method and refined by the full-matrix least-squares method in anisotropic approximation to R = 0.058 from 3896 independent reflections (CAD4 automated diffractometer, MoK ). The crystal consists of two complex ions [I¹]⁺ and [I²]^2– (molar ratio 2 : 1). The Na⁺ cation of the host–guest cation I¹ is coordinated by all eight heteroatoms (6O + 2N) of the cryptand ligand. The coordination polyhedron of this Na⁺ cation is a distorted cube. The atoms of two groups (CH₂–CH₂ and CH₂–O–CH₂–CH₂) in the cryptand ligand are disordered over two positions. The independent cation Na⁺ of the centrosymmetric binuclear complex anion I² is coordinated by one bifurcated O atom of the disordered water molecule and by three N atoms of the SCN^– ligands (including two bridging ligands). The coordination polyhedron of this Na⁺ caiotn is a distorted tetrahedron. The complex ions in the crystal structure of I are united by hydrogen bonds.     

Synthesis and Crystal Structure of Complex [Pb(qina)2(DMSO)]·H2O

A novel complex [Pb(qina)2(DMSO)]·H2O was synthesized, of which qina- is the quinaldic acid radical and DMSO the dimethyl sulfoxide. Elemental analysis, IR spectra, and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure. This complex belongs to monoclinic system, space group P121/n1, with a = 7.1553(17), b = 17.543(2), c = 17.306(2)(A),β = 91.671(4)°, C22H20N2O6PbS, Mr = 647.65, Z = 4, V= 2171.5(6)(A)3, Dc= 1.981g/cm3,μ = 7.908 mm-1, F(000) = 1248, -9≤h≤6, -23≤k≤ 19, -22≤l≤22, R= 0.0221 and wR =0.0488. Weak coordinate bond is formed between oxygen atom in DMSO and Pb(Ⅱ ). There are also weak interactions, such as π-π interaction, hydrogen bonds and so on, among the complex molecules.     

Crystal Structure and Magnetic Properties of A One-Dimensional Polymer [Mn(im2-py)(tp)(H2O)2]·1.25H2O

A new manganese(II) complex [Mn(im2-py)(tp)(H₂O)₂]·1.25H₂O (im2-py=2-(2'-pyridyl)-4,4,5,5-tetramethylimidazoline-1-oxyl and tp=terephthalato dianion) has been synthesized and characterized structurally and magnetically. The crystal structure consists of neutral chains of manganese(II) ions linked by the terephthalate ligand. Variable temperature magnetic susceptibility data exhibit a weak antiferromagnetic coupling between the manganese(II) ion and the imino nitroxide radical.     

Crystal structure and Raman spectra of [Fe(H2O)6]3+(ClO 4 ? )3·3H2O

Single crystal X-ray diffraction is used to study the structure of colorless crystals isolated from the saturated aqueous solution of trivalent iron perchlorate (TIP) in 67.5% perchloric acid. It is found that the compound crystallizes in the trigonal crystal symmetry; parameters of the hexagonal unit cell: a = b = 16.079(2) ?, c = 11.369(2) ?, ?? = ?? = 90°, ?? = 120°, space group R{ie907-1}(S ₆), Z = 6, ??_calc = 2.021 g/cm³. The structural form of the crystal hydrate is [Fe(H₂O)₆]³⁺(ClO ₄ ^? )₃·3H₂O. The structure contains two independent complex iron cations. Each of them is in the special position {ie907-2}, but retains the regular octahedral structure: average bond lengths are r(Fe-O) = 1.997(1) ?, {ie907-3}O-Fe-O bond angles differ from 90° by only 0.93°. Independent [Fe(H₂O)₆]³⁺ cations form short H-bonds (O??O 2.64 ?) with three crystallization water molecules and somewhat longer H-bonds (O??O 2.73 ?) with three ClO ₄ ^? anions. The ClO ₄ ^? anion is disordered over two positions with occupancies of 0.62(2) and 0.37(2). Both positions correspond to the general position. The outer-sphere crystallization water molecule is characterized by the tetrahedral direction of H-bonds, which it forms with two anions and two independent [Fe(H₂O)₆]³⁺ cations. All water molecules are in the general position. The Raman spectroscopic study of polycrystalline samples reveals weak bands belonging to the internal vibrations of two types of water molecules. The least broad bands are assigned to the transitions of crystallization water molecules whose symmetry is insignificantly lowered by two anion-molecular Hbonds. Anomalously broad bands are assigned to the transitions of a coordinated water molecule whose symmetry is more lowered by intermolecular and anion-molecular H-bonds.     

Synthesis and Crystal Structure of a Mixed Cu-Cd Bimetallic Complex {[CuCd(pba)(H2O)3]·2H2O}n

A one-dimensional bimetallic compound {[CuCd(pba)(H2O)3]·2H2O}n in which pba was propylenebis (oxamic acid), was prepared. Crystal structure of the title compound was determined. It belongs to orthorhombic system, molecular formula CuCdC7H16N2O11, Mr=480.17, space group Pnma(#62), a=12.953(2), b=21.626(6), c=5.253(3)(A), V=1471(2)(A)3 and Dx=2.17g/cm3 for Z=4. The structure was solved by direct methods with final R=0.052 and Rw=0.063 for 1055 observed reflections with I>3σ(I). Two nitrogen atoms and two oxygen atoms from the oxamide and a water molecule coordinated to the CuII ion forming a square pyramidal geometry. Four oxygen atoms from the oxamide and two water molecules coordinated to the CdII ion forming an elongated octahedral geometry.     

Crystal Structure of Dimer Complex of 〔K (dndb)(H_2O)(NCS)〕_2

1INtrODUCTIONThecrownethercomPOundsandtheirderivativeshavecontinuouslyattractedconsiderableattentioneversincetheywerefirstreportedin1967illbecauseoftheirexcellentcapacitytoattachmetalatomstoformcomplexes.Nowadaystheyareappliedextensivelyinchemistry,biology,medicine,agriculture,metallurgyandmanyotherfields.Manypapersonsynthesesofnewcrownethers,theirstructuredeterminationandcharactersareoftenpublished.Inthestudiesthenitrifiedreactionofcrownetherisknownasasignificantwaybywhichfunctionalgroup…     

Crystal Structure of the Bis(Picrato-O,O")Tetraaquacalcium Complex with 18-Crown-6, [Ca(Pic)2(H2O)4] · 18C6

The crystal structure of the bis(picrato-O,O")tetraaquacalcium complex with 18-crown-6, [Ca(Pic)₂(H₂O)₄] · 18C6 (I), was studied using X-ray diffraction analysis: space group C2/c, a= 20.446 Å, b= 14.985 Å, c= 16.163 Å, = 135. 41°, Z= 4. The structure of Iwas solved by the direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R= 0.047 over all 3044 measured independent reflections (CAD4 automated diffractometer, MoK radiation). In the crystal, Iis not a guest–host complex but exists as individual [Ca(Pic)₂(H₂O)₄] and 18C6 molecules joined by intermolecular hydrogen bonds and van der Waals interactions. The Ca²⁺cation (CN 8) is located on a twofold crystallographic axis, its coordination polyhedron being a distorted square antiprism. The centrosymmetrical 18C6 molecule has a crown conformation with approximate D _3d symmetry and has six neighboring water molecules (three on each side of its mean plane), which form eight hydrogen bonds involving all six O atoms of 18C6.     

Hydrothermal Synthesis and Crystal Structure of a New Zero-dimensional Complex: [Zn(H2BPTC)(phen)2]n·3nH2O

A new metal-organic coordination complex [Zn(H2BPTC)(phen)2]n·3nH2O (BPTC =3,3',4,4'-benzophenone tetracarboxylate, phen = 1,10-phenanthroline) 1 has been obtained from hydrothermal reaction and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. In compound 1, the zinc cation is hexa-coordinated with two carboxylate oxygen atoms from one H2BPTC ligand and four nitrogen atoms from two different phen ligands, showing a slightly distorted octahedral geometry. Crystal data: C41H30N4O12Zn, Mr = 836.06, monoclinic,P21/c, a = 14.2714(9), b = 16.9386(10), c = 15.0151(9) (A),β = 101.3420(10)°, V= 3558.8(4) (A)3, Dc= 1.560 g/cm3,μ(MoKα) = 0.766 mm-1, F(000) = 1720, Z = 4, R = 0.0439 and wR = 0.1157 for 4123observed reflections with I ＞ 2σ(I).     

Synthesis, Crystal Structure and Luminescence Property of [Co(hmz)2(H2O)4]·2H2O

A new mononuclear Co(Ⅱ) complex, [Co(hmz)2(H2O)4]·2H2O, has been synthesized by the reaction of Co(CH3COO)2·4H2O with 1-(4-hydroxyphenyl)-5-mercaptotetrazole (Hhmz). It crystallizes in the monoclinic system, space group P21/n with a = 13.502(5), b = 6.718(3), c = 13.972(6) (A), β = 117.532(4)°, V = 1123.9(8) (A)3, Z = 2, M r = 553.45, F(000) = 570, Dc = 1.635 g/cm3, μ = 1.008 mm-1, the final R = 0.0272 and wR = 0.0684 for 2194 observed reflections (Ⅰ＞ 2σ(Ⅰ)). The Co(Ⅱ) is six-coordinated by two nitrogen atoms from two hmz-1 ligands and four water molecules, forming an octahedral geometry. The intermolecular hydrogen bonding and offset-panel π-π stacking interactions between the adjacent molecules extend the compound into a three- dimensional supramolecular framework. The title compound emits strong blue fluorescent light (λem(max) = 427 nm) at room temperature and is red-shifted compared with free ligand Hhmz (λem(max) = 342 nm).     

Synthesis and Structure of anti-Configuration Complex [Cu(tssb)2]·2[(H3O)Cl]·4H2O

The title complex [Cu(tssb)2]·2[(H3O)Cl]·4H2O (C18H34Cl2CuN2O14S2) (tssb = taurine salicylaldehyde Schiff base) has been synthesized by the reaction of taurine salicylaldehyde Schiff base (tssb) and copper acetate in water-ethanol. Its single-crystal structure was determined by X-ray diffraction method. The crystal structure belongs to triclinic, space group P with a = 0.7407(1), b = 1.3329(3), c = 1.5736(3)nm, α = 103.800(4), β = 95.030(4), γ = 104.416(4)°, Mr = 701.06, V = 1.4433(5) nm3, Z = 2, Dc = 1.613 g/cm3, μ = 1.153 mm-1 and F(000) = 726. The compound is an infinitely expanding three-dimensional network connected with hydrogen bonds. The Cu(Ⅱ) atom is coordinated by two nitrogen and two oxygen atoms to form a distorted planar coordination compound which adopts anti-configuration because two sulfonic acid groups are positioned diagonally on a plane.     

Synthesis, Crystal Structure and Electrochemical Properties of the Complex Cd(α-FRA)2(Phen)(H2O)

A new cadmium complex Cd(α-FRA)2(Phen)(H2O) was synthesized by self- assembly reaction of α-furoic acid, phenanthroline (phen), and Cd(NO3)2(4H2O. It crystallizes in monoclinic, space group P21/c, with a = 0.6799(2), b = 1.7780(6), c = 1.6866(6) nm, β = 94.912(6)o, V = 2.0315(12) nm3, Dc = 1.742 g/cm3, Z = 4, Mr = 532.77, μ(MoKα) = 1.124 mm-1, F(000) = 1064, R = 0.0411, wR = 0.0790. The structural analysis shows that the cadmium ion is coordinated with two nitrogen atoms from one phen molecule and four oxygen atoms respectively from two α-furoic acids and one water molecule, giving a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex was also discussed, which shows that the electrode process is irreversible in the electrode reactor.     

Synthesis and Crystal Structure of a Palladium(Ⅱ)Coordination Polymer [Na2Pd(2,6-pydc)2(H2O)6]n

A novel coordination polymer [Na2Pd(2,6-pydc)2(H2O)6]n (2,6-H2pyde = 2,6-pyri-dinedicarboxylie acid) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinie system, space group P21/c,with a = 11.962(2), b = 6.5552(13), c = 12.673(3) A, β = 91.72(3)°, V= 993.3(3) A3,Z = 2, Mr=590.68, Dc = 1.975 g/cm3,μ=1.059 mm-1, F(000) = 592, the final R = 0.0211 and wR = 0.0454. In the crystal the Pd(Ⅱ) ion adopts a distorted four-coordinated square-planar geometry and bonds to two bidentate 2,6-pyridinedicarboxylate molecules through caronyl oxygen and pyridine nitrogen atoms. The title complex exhibits a novel three-dimensional network structure.