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1.
A new centrosymmetric mononuclear copper(II) complex [Cu(L)2](ClO4)2 (I) and a new centrosymmetric mononuclear nickel(II) complex [Ni(L)2(MeOH)2](ClO4)2 (II), where L is the zwitterionic ligand 2-bromo-4-chloro-6-[(2-methylammonioethylimino)methyl]phenolate, have been prepared from the Schiff base 2-bromo-4-chloro-6-[(2-methylaminoethylimino)methyl]phenol with copper perchlorate and nickel perchlorate, respectively. The complexes were characterized by elemental analysis, infrared spectra, and single-cyrstal X-ray diffraction (CIF files CCDC nos. 1408054 (I) and 1407973 (II)). Complex I crystallizes in the monoclinic space group P21/c with unit cell dimensions a = 7.7736(4), b = 21.608(1), c = 8.5194(4) Å, β = 93.907(2)°, V = 1427.7(1) Å3, Z = 2, R 1 = 0.0546, and wR 2 = 0.1531. Complex II crystallizes in the monoclinic space group P21/c with unit cell dimensions a = 21.324(3), b = 16.821(2), c = 9.425(1) Å, β = 90.114(2)°, V = 3380.5(7) Å3, Z = 4, R 1 = 0.0693, and wR 2 = 0.1627. The Cu atom in I is in square planar coordination, and the Ni atom in II is in octahedral coordination.  相似文献   

2.
The solution reactions of CuCl2 with 2,2′:6′,2″-terpyridine (Terpy) and dicarboxylic acid (glutaric acid or suberic acid) afforded two 1D coordination polymers [Cu(Terpy)(C5H6O4)] n (I) and [Cu(Terpy)(C8H12O4)] · 3H2O (II) and their structures were characterized by IR, TG-DTA, and single-crystal X-ray diffraction. Crystallographic data for I: C20H16CuN3O4, M r = 425.90, monoclinic, space group C2/c, a = 10.335(2), b = 21.193(4), c = 8.580(2) Å, β = 111.99(3)°, V = 1742.5(6) Å3, Z = 4, ρ c = 1.623 g/cm3, F(000) = 872, R = 0.0304 and wR = 0.0915; and those for II: C23H29CuN3O7, M r = 523.03, triclinic, space group P \(\bar 1\), a = 8.362(2), b = 10.605(2), c = 14.617(3) Å, α = 73.26(3)°, β = 86.23(3)°, γ = 69.45(3)°, V = 1161.3(4) Å3, Z = 2, ρ c = 1.496 g/cm3, F(000) = 546, R = 0.0636 and wR = 0.1106. X-ray diffracion studies reveal that both complexes I and II feature 1D chain. The 1D polymer chains are connected by π-π-stacking interactions to generate 2D supramolecular layers.  相似文献   

3.
A new complex salt [4,7,13,16,21,24-hexaoxa-1,10-diazoniabicyclo[8.8.8]hexacosane bis[dichloro(thiocyanato)copper(II)], [H2(Crypt-222)][CuCl2(SCN)]2, is synthesized and studied by X-ray diffraction analysis. The crystals are monoclinic (space group C2/c, a = 14.603 Å, b = 8.330 Å, c = 25.091 Å, β = 100.76°, Z = 4). The structure is solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.047 for 2943 independent reflections (CAD-4 automated diffractometer, λMoK α radiation). The Cu2+ cations and Cl? and SCN? anions form infinite polymeric chains of spiro-conjugated alternating centrosymmetric four-membered CuCl2Cu cycles and eight-membered Cu(SCN)2Cu cycles through coordination bonds. The coordination polyhedron of the Cu2+ cation is a distorted trigonal bipyramid. The [H2(Crypt-222)]2+ dication contains trifurcate N+-(…O)3 bonds on axis 2.  相似文献   

4.
A novel Cu(II) complex Cu2(Endc)2(Bipy)2 has been synthesized by the reaction of Cu(NO3)2 · 3H2O, Endc (endo-norbornene-cis-5,6-dicarboxylic acid), and Bipy (2,2-bipyridine) at room temperature. 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: triclinic, P \(\bar 1\) with a = 9.0373(10), b = 10.1637(11), c = 10.5574(12) Å, α = 65.78(1)°, β = 72.32(2)°, β = 73.23(2)°, Z = 1, V = 827.46(16) Å3, ρ c = 2.160 g/cm3, F(000) = 410.0, R = 0.0483 and wR = 0.0958 independent reflections for 4468 observed ones (I > 2 σ(I)).The Cu2+ ion is coordinated by two nitrogen atoms from the Bipy molecule and three oxygen atoms from two Endc, giving a distorted squarepyramidal coordination geometry. Two neighboring Cu2+ ions are bridged by a pair of bimonodentate carboxyl groups of different Endc acids, giving a centrosymmetrical binuclear structure which a Cu…Cu distance of 3.2946 Å. The photoluminescence properties of the complex were studied at room temperature. The complex displays an obvious photoluminescent emission upon excitation at 390 nm in the solid state.  相似文献   

5.
A new mixed-ligand one-dimensional copper(II) coordination polymer [Cu(en)(sal)Cl] n where en = ethylenediamine(C2H8N2) and Hsal = 2-hydroxybenzoic acid (salicylic acid; C7H6O3) is synthesized and characterized by FTIR spectroscopy and single crystal X-ray diffraction. The structure contains Cu2+ ions in two different distorted octahedral coordination environments: an axially extended CuN4Cl2 moiety arising from a pair of bidentate en ligands and a CuO4Cl2 moiety arising from a pair of asymmetrically coordinated sal anions. The chloride ions bridge the copper ions into a zigzag chain propagating in [001]. The structure is consolidated by N–H???O and N–H???Cl hydrogen bonds which generate a layered network. Crystal data: C9H13ClCuN2O3, M r = 296.20, monoclinic, P21/c, a = 13.9179(10) Å, b = 10.4900(8) Å, c = 8.5181(6) Å, β = 105.518(4)°, V = 1198.30(15) Å3, Z = 4, R(F) = 0.026, w R(F 2) = 0.068.  相似文献   

6.
X-ray structural analysis has been performed for two complex compounds: Cu(en)2(o-HB)2H2O (I) (a = 16.873(4) Å, b = 8.713(2) Å, c = 14.803(3) Å, β = 91.15(2)°, V = 2175.8(8) Å3, C2/c, Z = 4, R(F) = 0.0263, 1516 reflections with I > 3σ (I)) and [Cu(en)2(OH2)2]2+(o-AB?)2 (II) (a = 7.488(5) Å, b = 22.122(8) Å, c = 7.856(5) Å, β = 118.77(2)°, V = 1140.7(11) Å3, P21/n, Z = 2, R(F) = 0.0432, 1684 reflections with I > 3σ(I)) synthesized under identical conditions (en is ethylenediamine, o-HB is o-hydroxybenzoate, and o-AB is o-aminobenzoate). Although the compounds were assumed to have similar structures and the Cu-Lig bond lengths and the cis and trans angles are acceptable for an octahedral structure, the geometric parameters of o-HB suggest that the copper atom has a plane square environment.  相似文献   

7.
A new copper(II) complex [Cu(5-NO2-2-CH3CONHC6H3COO)2(H2O)3] · 2H2O was synthesized by the reaction of sodium 5-nitro-5-acetamidobenzoate with CuSO4 · 5H2O (2: 1), and its structure was determined by X-ray diffraction. Crystals are monoclinic: a = 11.7146(7) Å, b = 16.8463(10) Å, c = 13.2408(9) Å, β = 113.896(5)°, Z = 4, ρcalc = 1.668 g/cm3, space group P21/c, R = 0.0338. In the monomer complex, the copper atom has an elongated square-pyramidal coordination (4 + 1); the coordination sphere is formed by two oxygen atoms of the carboxylate groups of two monodentate organic ligands and the three oxygen atoms O(w) of the water molecules (the O(3w) atom is in the axial position). In the structure, the complex molecules are linked by hydrogen bonds involving two uncoordinated water molecules.  相似文献   

8.
Copper(II) chelates with β-diimine derivatives of acetylacetone that have a general formula of Cu(R1C(NR2)CHC(NR2)R1)2, where R1, R2 are alkyl substituents, are synthesized. The complexes were identified using elemental analysis, melting point measurements, and high-temperature mass spectrometry data. Knudsen technique is employed to determine the vapor pressure temperature dependence, and standard thermodynamic parameters of sublimation ΔH T 0 and ΔS T 0 are derived. A single crystal X-ray diffraction study is carried out for copper(II) complexes of Cu(CH3-C(NCH3)-CH-C(NCH3)-CH3)2 (a = 10.363(1) Å, b = 11.978(1) Å, c = 12.653(1) Å, V = 1570.6(3) Å3, space group Pnc2, Z = 4, d calc = 1.328 g/cm3, R = 0.027), Cu(CH3-C(NC2H5)-CH-C(NC2H5)-CH3)2 (a = 11.782(4) Å, b = 13.951(8) Å, c = 25.591(8) Å, V = 4206(3) Å3, space group C2221, Z = 8, d calc = 1.169 g/cm3, R = 0.10), and also 2-(methylamino)-4-(methylimino)-pentene-2 CH3-(C=(NCH3))-CH=(C-(NHCH3))-CH3 (a = 12.129(2) Å, b = 12.034(2) Å, c = 5.692(1) Å, β = 107.05(3)°, V = 794.3(3) Å3, space group Cc, Z = 4, d calc = 1.055 g/cm3, R = 0.06). Van der Waals lattice energy E cryst is calculated for the cooper(II) complexes by the atom-atom potential technique. The calculated values are compared to experimental sublimation enthalpies Δ H T 0 .  相似文献   

9.
Two Mn(II) coordination polymers, {[Mn3 (Pfca)6(Phen)2] · 2DMF} n (I) and [Mn(Pfca)2(Phen)(H2O)] n (II) (HPfca = 4-fluorocinnamic acid, Phen = 1,10-phenanthroline), were synthesized and characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis, and singlecrystal X-ray diffraction (CIF files CCDC nos. 967513 (I), 1542972 (II)). Complex I crystallizes in the triclinic crystal system, space group Pī with a = 11.0821(11), b = 12.2632(12), c = 15.0288(15) Å, α = 87.3760(10)°, β = 88.4610(10)°, γ = 81.2220(10)°, V = 2016.0(3) Å3, ρc = 1.369 g/cm3, M r = 1662.25, Z = 1, F(000) = 853, μ = 0.543 mm–1, the final R = 0.0592 and wR = 0.1681 for 15498 observed reflections with I > 2σ(I). Complex II is of monoclinic system, space group P21/c with a = 18.0539(19), b = 8.5806(9), c = 18.758(2) Å, β = 116.5700(10)°, V = 2599.0(5) Å3, ρc = 1.491 g/cm3, M r = 583.44, Z = 4, F(000) = 1196, μ = 0.567 mm–1, the final R = 0.0337 and wR = 0.0853 for 18139 observed reflections with I > 2σ(I). Complex I features linear Mn(II)-trinuclear units, which form 1D chain structure through F···F weak interactions, and complex II is 1D polymeric Mn(II)-chains. Antiferromagnetic coupling interactions exist within Mn(II)- carboxylate trinuclear in I (J =–0.40 cm–1) and Mn(II)-carboxylate chain in II (J =–0.45 cm–1).  相似文献   

10.
A novel coordination polymer [Co5(OH)2(dnbpdc)4(H2O)6]·16H2O (1) (dnbpdc = 6,6′-dinitro-4,4′-biphenyldicarboxylic acid) is obtained from a hydrothermal reaction. The structure of complex 1 is characterized by elemental analysis, IR spectroscopy, and single crystal X-ray diffraction analysis. The title compound (C56H70Co5N8O56, M r = 2045.85) crystallizes in the triclinic space group P-1 with a = 11.9349(2) Å, b = 12.1895(2) Å, c = 15.420(2) Å, α = 109.390(7)°, β = 94.786(1)°, γ = 108.027(9)°, V = 1968.4(4) Å3, Z = 1, D c = 1.726 g/cm3, F(000) = 1045, μ(MoK α) = 1.154 mm–1, T = 133(2) K, the final R = 0.0316 and wR = 0.0692 for 7032 observed reflections with I > 2σ(I). The coordination polymer is built of a pentanuclear Co(II) cluster, four dnbpdc ligands, two hydroxyl groups, six coordination water and sixteen crystal water molecules. Ligand oxygen atoms exhibit three types of coordination modes (monodentate, syn-syn bridging bidentate and bridging tridentate). Moreover, the infinite three-dimensional supramolecular network is generated by coordination and hydrogen bonds. The thermal stability of complex 1 is evaluated by differential scanning calorimetry and thermogravimetric analysis.  相似文献   

11.
The syntheses and crystal structures of the layered coordination polymers M(C8H8NO2)2 [M = Mn (1), Co (2), Ni (3) and Zn (4)] are described. These isostructural compounds contain centrosymmetric trans-MN2O4 octahedra as parts of infinite sheets; the ligand bonds to three adjacent metal ions in μ3-N,O,O′ mode from both its carboxylate O atoms and its amine N atom. In each case, weak intra-sheet N–H?O and C–H?O hydrogen bonds may help to consolidate the structure. Crystal data: 1, C16H16MnN2O4, M r = 355.25, monoclinic, P21/c (No. 14), a = 10.6534(2) Å, b = 4.3990(1) Å, c = 15.5733(5) Å, β = 95.1827(10)°, V = 726.85(3) Å3, Z = 2, R(F) = 0.026, wR(F 2) = 0.067. 2, C16H16CoN2O4, M r = 359.24, monoclinic, P21/c (No. 14), a = 10.6131(10) Å, b = 4.3374(4) Å, c = 15.3556(17) Å, β = 95.473(4)°, V = 703.65(12) Å3, Z = 2, R(F) = 0.041, wR(F 2) = 0.091. 3, C16H16N2NiO4, M r = 359.02, monoclinic, P21/c (No. 14), a = 10.6374(4) Å, b = 4.2964(2) Å, c = 15.2827(8) Å, β = 95.9744(14)°, V = 694.66(6) Å3, Z = 2, R(F) = 0.028, wR(F 2) = 0.070. 4, C16H16N2O4Zn, M r = 365.68, monoclinic, P21/c (No. 14), a = 10.6385(5) Å, b = 4.2967(3) Å, c = 15.2844(8) Å, β = 95.941(3)°, V = 694.89(7) Å3, Z = 2, R(F) = 0.038, wR(F 2) = 0.107.  相似文献   

12.
The crystal structures of cobalt(II) Schiff base complex (CoIIL2 · H2O) and Schiff base ligand 3,5-dichlorosalicylidene-2-chlorophenylmethylamine (HL) have been determined by single-crystal X-ray analysis. The geometry around cobalt in CoIIL2 · H2O is distorted tetrahedral. CoIIL2 · H2O crystallizes in the monoclinic system, in space group C2/c, with crystallographic parameters: a = 12.9143(16) Å, b = 8.8326(16) Å, c = 25.115(3) Å, β = 92.791(10)°, V = 2861.4(7) Å3, Z = 4, F(000) = 1420, and the final R indices (I > 2σ(I)) are R 1 = 0.0440, wR 2 = 0.1272. HL crystallizes in the monoclinic system, in space group P21/c, with crystallographic parameters: a = 11.9764(15), b = 8.2331(10), c = 14.2211(17) Å, β = 98.723(6)°, V = 1386.0(3) Å3, Z = 4, F(000) = 640, and the final R indices (I > 2σ(I)) are R 1 = 0.0397, wR 2 = 0.1018.  相似文献   

13.
The single crystal X-ray diffraction (XRD) method was used to determine the structure of the [Cu(mi-tfac)2] (mi-tfac = MeC(O)CHC(NMe)CF3) complex at the temperature of 150 K. The crystallographic data are as follows: space group Pnna, a = 11.8798(16) Å, b = 12.0315(16) Å, c = 10.6259(14) Å, V = 1518.8(4) Å3, Z = 4, R = 0.0288. The structure is molecular, the coordination environment of copper in the molecule adopts a distorted tetrahedral geometry. The Cu–O and Cu–N distances are 1.9182(13) Å and 1.9610(16) Å respectively, the OCuN chelate angle is 94.18(5)°. The thermal properties of the compounds [Cu(mi-tfac)2] and [Cu(RC(O)CHC(NMe)R)2] (R = Me, t Bu) in the condensed phase have been studied by the methods of thermogravimetry and differential scanning calorimetry. The thermodynamic characteristics of the melting processes have been determined.  相似文献   

14.
A new 1D chiral metal-organic coordination polymer [Cu(Cphe)2] · 3H2O (I) (HCphe = L-3-Cyanophenylalanine) has been synthesized in an aqueous solution and characterized by elemental analysis, thermogravimetric analysis (TGA), X-ray powder diffraction (XRPD), infrared spectroscopy (IR) and single crystal X-ray diffraction. The X-ray diffraction analysis reveals that I crystallizes in the monoclinic space group P21. The adjacent copper(II) atoms are linked by Cphe ligands to form a 1D zigzag chain, which is further connected via strong hydrogen bonds to form a 3D supramolecular framework. The unit cell parameters for I are: a = 12.0201(8), b = 6.1495(4), c = 14.8576(10) Å, β = 94.1720(10)°, V = 1095.00(13) Å3, and Z = 2.  相似文献   

15.
A new manganeses(II) complex MnLCl2 · CH3OH (L = N,N′-bis(furaldehyde)diethylenetriamine) was synthesized and characterized by X-ray crystallographic analysis. The crystals are orthorhombic, space group Pnma with cell parameters a = 20.998(6), b = 13.314(5), c = 6.785(8) Å, Z = 4, R 1 = 0.0609, and wR2 = 0.2116. The coordination geometry around Mn(II) atom is a trigonal-bipyramidic containing one tridenate ligand L and two Cl? ions.  相似文献   

16.
Two new dioxomolybdenum(VI) complexes, [MoO2L1(MeOH)] (I) and [MoO2L2] (II), where L1 and L2 are the anionic forms of N'-(2-hydroxy-3,5-di-tert-butylbenzylidene)-4-methoxybenzohydrazide and 2-amino-N'-(2-hydroxy-3,5-di-tert-butylbenzylidene)benzohydrazide, respectively, have been synthesized and characterized by elemental analysis, FT-IR spectra, and single crystal X-ray determination (CF files CCDC nos. 1448089 (I), 1487063 (II)). The crystal of I is monoclinic: space group P21/n, a = 7.353(1), b = 24.758(3), c = 13.891(2) Å, β = 101.013(2)°, V = 2482.3(6) Å3, Z = 4, R 1 = 0.0848, wR 2 = 0.2050. The crystal of II is monoclinic: space group P21/c, a = 6.752(1), b = 16.947(1), c = 19.510(1) Å, β = 96.891(2)°, V = 2216.5(4) Å3, Z = 4, R 1 = 0.0670, wR 2 = 0.1638. The Mo atom in complex I is in octahedral coordination, with three donor atoms of the hydrazone ligand, two oxo groups, and one methanol O atom. The Mo atom in complex II is in square pyramidal coordination, with three donor atoms of the hydrazone ligand, and two oxo groups. The complexes have interesting catalytic properties for sulfoxidation reactions.  相似文献   

17.
Two copper (imidazole) complexes, namely, [Cu(im)6]Cl2 · 4H2O (1), and [Cu(im)6]Cl2 · 2H2O (2) (im-imidazole) have been synthesized by hydrothermal method. Single-crystal X-ray analysis revealed that the complex 1 belongs to triclinic system, space group P \(\bar 1\) with a = 8.8097(18) Å, b = 9.0812(18) Å, c = 10.586(2) Å; α = 75.08(3)°, β = 83.14(2)°, γ = 61.84(3)°; R 1 = 0.0562, wR 2 = 0.1607. In compound 1, [Cu(im)6]2+ cation and counter anions Cl? alternatively array in an ABAB fashion via N-H...Cl hydrogen bonding. Compound 2 falls into monoclinic system, space group P21/n with a = 8.073(2) Å, b = 13.239(2) Å, c = 15.0810(10) Å; β = 97.940(10)°; R 1 = 0.0434, wR 2 = 0.1243. The equatorial ligands are involved into a complex hydrogen bond network that involves the chloride anions and uncoordinated water molecules. We report there synthesis, crystal structure, thermal stability, IR spectrum and fluorescent property.  相似文献   

18.
The crystal structures of catechol (o-dihydroxybenzene) and its 2:1 complex with dimethylsulfoxide are determined at T = 150 K. Crystal data: C14H18O5S, M = 298.37, triclinic, space group P \(\bar 1\), unit cell parameters: a = 7.7285(13) Å, b = 9.9924(17) Å, c = 10.3188(18) Å, α = 89.963(4)°, β = 89.968(4)°, γ = 69.076(5)°, V = 744.3(2)Å3, Z = 2, D x = 1.331 g/cm3, R1 = 0.048; C6H6O2, M = 110.11, monoclinic, space group P21/n, a = 9.8206(6)Å, b = 5.5903(3)Å, c = 10.4439(6)Å, β = 114.952(2)°; V = 519.85(5) Å3, Z = 4, D x = 1.407 g/cm3, R1 = 0.0289. In the 2:1 complex the molecules are joined in a supramolecular ensemble by D-H...A hydrogen bonds (D = O, C; A = O, π); in catechol they are bonded only by O-H...O. The state diagram of the catechol-dimethylsulfoxide system is examined by DTA.  相似文献   

19.
A new Schiff base ligand C19H13NO5(H2L) was synthesized using 2-aminoterephthalic acid and 2-hydroxy-1-naphthaldehyde. A complex of this ligand [Cu(C19H11NO5)(C2H6O)] n was synthesized and characterized by IR, UV, fluorescence spectroscopy and X-ray diffraction single-crystal analysis. The crystal crystallizes in the monoclinic system, space group Pbca with a = 8.7745(18), b = 18.613(4), c = 24.644(5) Å, V = 4024.9(14) Å3, Z = 8, F(000) = 1816, S = 1.009, ρ calcd = 1.462 g cm?3, μ = 1.122 mm?1, the final R = 0.0477 and wR = 0.1594 for 4609 observed reflections (I > 2σ(I)). The Cu(II) is five-coordinated by one N atom and two O atoms from the Schiff base ligand and two carboxylate O atoms from another two ligands to form a distorted square-pyramidal geometry. Each ligand serves as a bridging ligand to link Cu2+ ions, leading to a two-dimensional coordination polymer. The fluorescence properties of the ligand and complex were also studied. The ligand shows strong fluorescence, and the fluorescence intensity is weakened after the Cu(II) complex formed.  相似文献   

20.
The crystal structure of europium cinnamate of the composition [Eu(Cin)3] n (Cin is cinnamic acid anion C9H7O 2 ? ) was determined by X-ray crystallography (a = 22.626(1) Å, c = 7.7330(7) Å, space group R3/c, Z = 3, ρcalc = 1.448 g/cm3). The coordination polyhedron of Eu atoms is a distorted trigonal prism with three centered square faces. The structure is built of infinite polymeric chains [Eu(Cin)3] n running along the c axis and linked by van der Waals and π stacking interactions. Luminescent characteristics of the compound were determined.  相似文献   

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