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1.
Solvothermal reactions of MnCl_2·4H_2O with(pyridin-2-yl)methyl 4-(2-(4-((pyridin-2-yl)methoxy)phenyl)diazenyl)benzoate(L1) via an in situ ligand transformation reaction produced a new coordination polymer, {[Mn_(2.5)Cl_3L_2(H_2O)]·H_2O}_n(1, where HL = 4-(2-(4-((pyridin-2-yl)methoxy)phenyl)diazenyl)benzoic acid). The L1 ligand was decomposed in situ to L~- which was coordinated with Mn(Ⅱ) to form compound 1 in the solvothermal synthesis process. Complex 1 was characterized by IR spectroscopy, powder X-ray diffraction and single-crystal X-ray diffraction.Compound 1 possesses a 2D network. In addition, stability and photoluminescent property of 1 were also investigated.  相似文献   

2.
IR and NMR spectra of novel bionics insecticide—C_5NS_4O_6H_(12)Na·H_2O have been studied. The molecular and crystal structures of the compound also have been determined. The compound crystallizes in the monoclinic space group C_(2h)~5, - P2_1/n with α= 8.0972. (9) , b =16.262(4), c = 10.370(3), β= 94.26(2)° and z = 4.The result shows that N atom in this compound captures a proton to form HN~ group, Na~ is in statistical disorder. Therefore, the structural formula of tho compound is (CH_3)_2HN~ —CH(CH_2S_2O_3~-)_2·1/2 (Na~ )_2·H_2O.  相似文献   

3.
The reaction of Cd(NO_3)_2·4H_2O with 4,4?-dipyridylacetylene(4,4?-DPA) and 2-nitroterephthalic acid(2-NO_2-H_2BDC) in DMF/H_2O mixed solvent has afforded a compound {[Cd(2-NO_2-BDC)(4,4?-DPA)]·(DMF)}_n(1). Compound 1 has been characterized by single-crystal X-ray diffraction, powder X-ray diffraction, thermogravimetry analysis, and IR spectrum. Compound 1 crystallizes in the monoclinic system, space group P21/n, with a = 12.1488(3), b = 14.6689(3), c = 13.1615(3) ?, β = 111.809(3)o, V = 2177.63(9) ?~3, Z = 4, C_(23)H_(18)N_4O_7 Cd, M_r = 574.81, D_c = 1.753 g/cm~3, μ = 8.523 mm~(-1), F(000) = 1152, the final R = 0.0411 and wR = 0.1064 for 3589 observed reflections with I 2s(I). In compound 1, the Cd(Ⅱ) ions are linked by the carboxylate groups of 2-NO_2-BDC ligands to give a two-dimensional layered structure based on the centrosymmetric dinuclear Cd_2(COO)_2 units, which are further connected by the 4,4?-DPA ligands to produce a three-dimensional framework with pcu topology. Careful examination revealed that compound 1 is a 2-fold interpenetrating framework. Furthermore, the gas adsorption properties of 1 for N_2 and CO_2 have also been investigated.  相似文献   

4.
A new cobalt-sodium coordination polymer [CoNa(C_9H_9N_3O_2S)_2·H_2O]_2·C_2H_3N·H_2O(1) has been synthesized with cobalt chloride,2-(2-hydroxy-3-methoxybenzylidene)hydrazinecarbothio amide(L) and sodium hydroxide.It crystallizes in the triclinic space group P1,with a = 9.972(4),b = 10.923(4),c = 13.489(5) ?,α = 108.005(10),β = 92.728(10),γ = 93.16(1)o,V = 1392.0(9) ?~3,Mr = 1151.95,Dc = 1.374 g/cm~3,Z = 2,F(000) = 592,the final GOOF = 1.126,R = 0.1091 and wR = 0.2412.Each unit molecule consists of two cobalt ions and two sodium ions bridged by four 2-(2-hydroxy-3-methoxybenzylidene)hydrazinecarbothio amide anions.The coordination environment of Co ion is CoO_2N_2S_2,giving a distorted octahedral geometry and the Na(1) ion is NaO_4N,giving a distorted square pyramidal geometry.The results show that 1 shows one strong intense fluorescence emission wavelength of 429 nm with an excitation wavelength of 376 nm,and the electron transfer of 1 is irreversible in electrode reactions.  相似文献   

5.
Two 1-methyl-1H-benzo[d]imidazole derivatives, C_(18)H_(14)CuN_4O_4·C_4H_8O_2(1) and C_9H_9N_3O(2), have been synthesized and characterized by NMR, MS, FT-IR, elementary analysis and X-ray single-crystal diffraction. Compound 1 crystallizes in monoclinic, space group P2_1/n with a = 9.6888(3), b = 7.3772(2), c = 14.3277(4) ?, β = 95.819(3)°, V = 1018.81(5) ?~3, M_r = 501.98, Z = 2, D_c = 1.636 g/cm~3, F(000) = 518, μ = 1.123 mm~(-1), MoKα radiation(λ = 0.71073 ?), the final R = 0.0325 and wR = 0.0859 for 1821 observed reflections with I 2σ(I). Compound 2 crystallizes in monoclinic, space group C2/c with a = 14.2908(14), b = 14.4268(13), c = 8.4802(6) ?, β = 108.513(9)o, V = 1657.9(3) ?~3, M_r = 175.19, Z = 8, D_c = 1.404 g/cm~3, F(000) = 736, μ = 0.097 mm~(-1), Mo Kα radiation(λ = 0.71073 ?), the final R = 0.0563 and wR = 0.1531 for 1231 observed reflections with I 2σ(I). Intermolecular(N-H···N, N-H···O) and intramolecular(N-H···N, C-H···O) hydrogen bonds, as well as C-H···π and π-π stacking interactions, help to stabilize the crystal structure of compound 2.  相似文献   

6.
《结构化学》2020,39(4):673-681
Two dibenzyltin compounds, {[C_6H_5 O(O)C=N–N=C(Ph)COO](m-Cl–C_6H_4CH_2)_2-Sn(CH_3OH)}_2(1) and {[p-Me–C_6H_4O(O)C=N–N=C(Ph)COO](m-Cl–C_6H_4CH_2)_2 Sn(CH_3OH)}_2(2), have been synthesized by microwave "one pot" reaction with benzoylhydrazine(or p-methyl benzhydrazine), phenylglyoxylic acid and di-m-chlorobenzyltin dichloride. Compound 2 contains two crystals 2 a and 2 b. The compounds have been characterized with IR, elemental analysis, ~1 H, ~(13)C and ~(119)Sn NMR spectra, H RMS. Three crystals are all binuclear molecules with a Sn_2O_2 four-membered ring plane, and each Sn atom center is seven-coordinated with [SnO_4C_2 N] to form a distorted pentagonal bipyramidal configuration. In vitro antitumor activities of all compounds and carboplatin were evaluated by MTT against three human cancer cells such as NCI-H460(lung cancer cells), HepG_2(liver cancer cells) and MCF7(breast cancer cells), and compound 2 exhibited better antitumor activity.  相似文献   

7.
The title compound, 2-(3-silatranylpropylamino)-4-dichlorophenyl-5,5-dimethyl-1,3,2-dioxaphosphorinane-2-oxide(2(C_(20)H_(33)N_2O_6Psi)·C_2H_6O·CH_4O, Mr = 991.20), has been synthesized by the nucleophilic substitution reaction of 2-chloro-4-phenyl-5,5-dimethyl-1,3,2-dioxaphosphorinane-2-oxide with γ-aminopropylsilatrane, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 10.3783(15), b = 11.2402(17), c = 12.1675(18) ?, a = 70.653(4), b = 82.908(4), g = 85.690(4)°, V = 1328.1(3) ?3, Z = 1, Dc = 1.239 g/cm~3, μ = 0.19 mm~(-1), F(000) = 532, the final R = 0.0640 and wR = 0.2090 for 3615 observed reflections with I 2s(I). The cyclic dioxaphosphorinane ring in the molecule adopts a thermodynamically stable cis conformation, while the silatrane fragment forms a cage-like structure in which there exists an intramolecular Si?N donor-acceptor bond. In the crystal structure, centrosymmetrically related molecules are linked by pairs of N–H···O hydrogen bonds into dimers, generating rings with graph-set motif R22(8). Furthermore, a couple of O(7)–H(10)···O(3) hydrogen bonds were formed by O atom of P=O and H atom from hydroxyl in the solvent ethanol. Thermal property of the compound was also studied by means of thermogravimetry(TGA). The thermal analysis and preliminary fireproofing test show that the title compound has good flame retardance.  相似文献   

8.
A new cobalt(II) compound, {(Me2NH2)4[Co(SIP)2]·2(DMF)·3(H2O)}n(1, H3 SIP =5-sulfoisophthalic acid), has been synthesized under solvothermal condition and structurally characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in the tetragonal system,space group P 4 21 m, with a = 14.3080(7), b = 14.3080(7), c = 12.1837(9) ?, V = 2494.2(3) ?~3, Z =2, C_(330)H_(58)N_6O_(19)S_2Co, Mr = 929.87, Dc = 1.238 g/cm, μ = 0.496 mm~(-1), F(000) = 982, flack parameter of 0.007(9), the final R = 0.0767 and wR = 0.2110 for 2391 observed reflections with I 2σ(I). The tetrahedral Co(II) ions are linked by carboxylate groups of the 5-sulfoisophthalate ligands to form an anionic two-dimensional(2D) layer displaying a(4,4) square network, which was charge-balanced by the [Me_2NH_2] + cations occupying the spaces between the 2D layers. Magnetic properties of 1 have been investigated in detail using direct-current and alternating-current susceptibility measurements.  相似文献   

9.
A benzothiazole-based compound 1, C_(28)H_(24)N_4O_2S, has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P2_1/c with a = 9.6309(14), b = 15.230(2), c = 17.197(3) ?, β = 105.222(2)°, V = 2433.9(6) ?~3, Z = 4, F(000) = 1008, D_c = 1.311 Mg/m~3, M_r = 480.57, μ = 0.166 mm~(-1), the final R = 0.0509 and wR = 0.1481 for 6643 observed reflections with I 2σ(I). The crystal structure of compound 1 is stabilized by C–H···O, N–H···N, N–H···O, O–H···N and C–H···N hydrogen bonds. The spectroscopic studies of the title compound toward various metal ions were also investigated in 25%(V/V) ethanol aqueous solution, and the result showed that it can selectively recognize Cu~(2+) with fluorescence quenching.  相似文献   

10.
Six first row transition metal complexes with 1,6-bis(2′-pyridyl)-2,5-dithiahexane(Py_2S_2), namely, MnPy_2S_2Cl_2(1), FePy_2S_2Cl_2(2), Co Py_2S_2Cl(3), CoPy_2S_2(SCN)_2(4), NiPy_2S_2(SCN)_2(5) and NiPy_2S_2(N_3)_2(6), have been synthesized. A mixture of MCl_2·x H_2O(M = Mn, Co) in MeOH(FeCl_2·4H_2O in MeCN) and the stoichiometric amount of Py_2S_2 was stirred for 4 h at room temperature, then these aiming products 1, 2 and 3 could be obtained by purification. A mixture of MPy_2S_2Cl_2(M = Co, Ni) in MeOH and two equivalents of KSCN or NaN_3 was stirred for 4 h at room temperature. After that, complexes 4, 5 and 6 could be got by purifying. For 1, 2, 3, 4 and 5, the metal centers are hexa-coordinated in a similar distorted octahedral geometry and the crystal structures have the same space group Pbcn. The crystal structure of compound 6 belongs to monoclinic with space group P21/c. The coordinated atoms around M(Ⅱ) are two pyridyl N atoms(N(1) and N(2)), two thioether S atoms(S(1) and S(2)) and two chloride ions(Cl(1) and Cl(2)) in compounds 1, 2, and 3, but in 4, 5, and 6, two chloride ions(Cl(1) and Cl(2)) are replaced by another two N atoms from N_3~– or NCS~–.  相似文献   

11.
《结构化学》2020,39(5):942-948
A novel heterometallic complex constructed by imidazole ligand, CoZn(C_3N_2H_3)_4(1), has been synthesized under hydrothermal conditions. Compound 1 was characterized by IR spectra, thermal analysis, powder X-ray diffraction and single-crystal X-ray diffraction. Single-crystal X-ray diffraction studies reveals that compound 1 is in the tetragonal system, space group I4_1cd with a = 23.4371(5), b = 23.4371(5), c = 12.4430(7) ?, V = 6834.9(4) ?~3, Z = 16, C_(12)H_(12)CoN_8Zn, M_r = 392.60, D_c = 1.526 g/cm~3, F(000) = 3152, μ = 2.381 mm~(–1), R = 0.0323 and w R = 0.0789. The CoZn(C_3N_2H_3)_4 is one-dimensional heterometallic molecular chains, which are further extended into a 3D open framework. Moreover, the solid-state fluorescence property of the complex has also been investigated at room temperature.  相似文献   

12.
The title complex N,O-bis{2-[[(2-benzhydryl-4,6-dimethylphenyl)imino]-methyl]-phenol}-nickel(II)(C_(56)H_(48)N_2NiO_2) has been synthesized by the reaction of 2-[[(2-benzhydryl-4,6-dimethylphenyl)mino]-methyl]-phenol with Ni(CH_3COO)_2·4 H_2O, and characterized by elemental analysis and IR spectrum. The spatial structure of the complex has been confirmed by single-crystal X-ray diffraction analysis. The compound belongs to the monoclinic system, space group C2/c with a = 39.035(8), b = 13.276(3), c = 17.679(4) ?, β = 98.06(3)°, V = 9071(3) ?~3, C_(56)H_(48)N_2NiO_2, M_r = 839.67, Z = 8, D_c = 1.230 Mg/m~3, μ = 0.472 mm~(-1), F(000) = 3536, T = 293(2) K, the final R = 0.0675 and w R = 0.1345(I 2s(I)). The compound showed excellent catalytic activity up to 1.268 × 10~7 g of PNB(mol of Ni)~(-1)h~(-1) for the addition polymerization of norbornene by using methylaluminoxane(MAO) as a cocatalyst.  相似文献   

13.
The title compound BNPT-DTO (C_(15)H_6N_4O_9S_4, Mr=514.51) has been synthesized and Its crystal structure determined. It is crystallized in orthorhombic system, space group P2_12_12_1, a=10.078(1), b=19.352(1),  相似文献   

14.
丁丹丹  张秀梅  刘结平 《结构化学》2014,33(7):1037-1042
One compound with N-(4-pyridylmethyl)imidazole liand, [Co(pyim)2(N3)2]n 1(pyim = N-(4-pyridylmethyl)imidazole), was synthesized and structurally characterized. Compound 1 crystallizes in triclinic, space group P21/c with a = 8.090(3), b = 16.109(3), c = 8.590(3), B= 117.800(12)o, V = 990.3(5) A3, Z = 2, Mr = 461.37, Dc = 1.547 g/cm3, F(000) = 474, μ = 0.901 mm-1, the final R = 0.0381 and wR = 0.0950 for 1581 observed reflections with I 2A(I). In this compound, the unique Co(Ⅱ) resides at a crystallographic inversion center and exhibits an octahedral coordination geometry. The adjacent Co(Ⅱ) ions are connected by the pyim ligands to form a 2D layer structure. The layers are stacked in an ABAB mode and reinforced by the weak interlayer C–H···N hydrogen bonds and π-π stacking to give a 3D architecture. The thermal property and electrochemical property of compound 1 have also been studied.  相似文献   

15.
The crystal structure of two isomorphic cluster compounds with formula (C_5H_7S_2)-[Mo_3(μ_3-O)(μ-X)_3(μ-OAc)_3Cl_3] (X=Cl for compound (Ⅰ) and compound (Ⅱ)) has been investigated by X-ray diffraction method. The parameters of two crystals are: a=10.423(1),b=17.095(4), c=14.062(7), β=97.54(4)(°); Dc=2.20gcm~(-3), D_o=2.17g cm~(-3) for compound (Ⅰ). and a=10.511(3), b=11.213(2), c=14.053(3), β=96.12(2)(°); D_c=2.52g cm~(-3), D_o=2.53gcm~(-3) for compound (Ⅱ). The space groups are P2_1/C. Z=4. The 2621 and 2548 independent reflections with I>3σ(I) were collected on a CAD-4 four-circle diffractometer by means of MoKα radiation. The crystal structures were solved by heavy atom method and refined by full-matrix least-squares technique to a final discrepancy factors of R=0.061 and 0.051 respectively. The results of investigation show that the molecule consists of the cation (C_5H_7S_2)+ and the trinuclear Mo cluster anion, the configuration of which is similar to that of (Et_4N)_2[Mo_3(μ_3-O)(μ  相似文献   

16.
One two-dimensional coordination polymer with a formula of {[Cd(L)(imidazole)(H_2O)](H_2O)}n(1) was obtained by the synthetic reactions in aqueous solution using a newly synthesized H_2L(H_2L = methyl-3-hydroxy-5-carboxy-2-thiophenecarboxylate) ligand.Compound1 crystallizes in monoclinic system,space group C2/c with a = 18.3176(11),b = 8.5366(9),c =8.4152(5) ?,β = 101.789(6)o,V = 2797.1(3) ?~3,D_c = 1.979 g/cm~3,C_(10)H_(12)N_2O_7SCd,Mr = 416.68 F(000) = 1648,μ = 1.745 mm~(-1),F(000) = 1648,the final R = 0.0323 and wR = 0.0604 for 2604 observed reflections with I 2s(I).Structure analyses reveal that the compound is constructed by dinuclear Cd(Ⅱ) clusters bridged by two hydroxyl oxygens of L~(2-)anions,which features a two-dimensional network with 4-connected sql topology.Furthermore,the compound exhibits high thermal stability and intense fluorescent emission,and could be explored for potentia luminescent materials.  相似文献   

17.
A dinuclear dysprosium(III) compound,[Dy_2(μ_2-OH)_2(QLC)_4(1,10-phen)_2]·4H_2O(1)(QLC-= 2-quinolinecarboxylate and 1,10-phen = 1,10-phenanthroline),was synthesized and structurally and magnetically characterized.Compound 1 crystallizes in triclinic system,space group P1 with a = 10.9439(3),b = 11.2823(3),c = 12.2323(4) ?,α = 107.446(3),β = 91.700(3),γ = 91.511(2)°,V = 1439.25(8) ?~3,Z = 1,C_(64)H_(50)N_8O_(14)Dy_2,Mr = 1480.12,Dc = 1.708 g/cm3,μ = 2.653 mm-1 and F(000) = 734.The final R = 0.0366 and w R = 0.0736 for 5816 observed reflections with I 2σ(I).Compound 1 contains the mononuclear [Dy(QLC)_2(1,10-phen)] subunit formed from one 1,10-phen and two QLC-ligands chelating Dy(III) ion.Two mononuclear [Dy(QLC)_2(1,10-phen)] subunits are bridged by a pair of μ_2-OH groups to give a centrosymmetric dinuclear [Dy_2(μ2-OH)_2(QLC)4(1,10-phen)_2] with each Dy(III) ion being eight-coordinated.Detailed susceptibility measurements revealed that compound 1 does not show slow magnetic relaxation under zero direct-current field but exhibits field-induced slow magnetic relaxation under 2 kOe applied field.  相似文献   

18.
A new compound, [Ni(Hdctrz)(H_2O)_4](1, H_3dctrz = 1-H-1,2,4-triazole-3,5-dicarboxylic acid), has been successfully synthesized via slow evaporation. The structure of 1 was characterized by FT-IR, elemental analysis and single-crystal X-ray diffraction. Compound 1 crystallizes in monoclinic, space group P21/c with a = 6.871(1), b = 11.468(1), c = 12.178(1) ?, b = 101.291(1)o, V = 941.01(16) ?~3, Z = 4, C_4H_9N_3O_8Ni, M_r = 285.85, D_c = 2.018 g·cm~(–3), m = 2.10 mm~(–1), F(000) = 584, GOOF = 1.025, the final R = 0.0515 and wR = 0.2125 for 1404 observed reflections(I 2s(I)). The crystal structure is assembled by a slightly distorted {NiNO_5} octahedral geometry and hydrogen bonds viz. N–H···O, O–H···O, C–O···π and π···π weak interactions. A rare π···π interaction from triazolate and carboxylate is affirmed through the molecular orbitals(MO) of three adjacent Ni CN molecules. The 3D Hirshfeld surface analysis was employed to gain additional insight into the interactions responsible for the packing of compound 1. Quantitative examination of 2D fingerprint plots revealed, amongst others, the dominating participation of O···H, N···H and π···π interactions in the molecular packing.  相似文献   

19.
{[Cu_3(cis-DAM)_4(OH)_2]·12H_2O}_n 1 and [Ag_3(trans-DAM)_2(NO_3)]_n 2 with a flexible ligand N,N?-diacetic acid imidazolium(HDAM) were synthesized and characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in the orthorhombic I222 space group with a = 12.033(2),b = 12.498(3),c = 14.963(3) ?,V = 2250.4(8) ?~3,Z = 8,C_7H_(13.5)N_2O_(7.5)Cu_(0.75),M_r = 293.35,D_c = 1.732 g·cm~(-3),F(000) = 1210,GOF = 1.087,the final R(I 2σ(I)) = 0.0521 and w R(all data) = 0.1386. Compound 2 crystallizes in the monoclinic C2/c space group with a = 21.601(4),b = 8.321(2),c = 13.589(3) ?,β = 126.95(3)°,V = 1951.9(7) ?~3,Z = 8,C_7H_7N_(2.5)O_(5.5)Ag_(1.5),M_r = 375.96,D_c = 2.559 g·cm~(-3),F(000) = 1448,GOF = 1.017,R(I 2σ(I)) = 0.0222 and w R(all data) = 0.0633. Compound 1 displays a novel 2D layer,consisting of a couple of left-helical chains with a pitch of 12.498(3) ? formed by μ_3-cis-DAM~– ligands and Cu(1) ions,which are stabilized by hydrogen bonding interactions to give a 3D supramolecular framework. As for 2,Ag(1) ions are doubly bridged by trans-DAM~– and NO_3~– to form [Ag(1)_2O_4] chains,which are further connected by Ag(2) and trans-DAM~– to build a 3D framework. Additionally,thermogravimetric analyses,FT-IR spectroscopy,UV-visible spectroscopy,and the fluorescent properties were discussed.  相似文献   

20.
We synthesized one novel Schiff-base ligand by modifying the aromatic aldehyde: H_2L~1(H_2L~1 = N,N?-bis(2-oxy-acetate-3-methoxyl)benzylpropylene(1,3-propane)diamine). [Ni(C_(23)H_(24)N_2O_8)]·6H_2O](1) was prepared by the reaction between H_2L~1 and NiCl_2·6H_2O in C_2H_5 OH. Compound 1 was structurally characterized by elemental analysis, IR, H NMR and single-crystal X-ray diffraction. 1 crystallizes in monoclinic system, space group P21/n with a = 1.3952(4), b = 1.3746(9), c = 1.6121(0) nm, β = 112.66(3)°, V = 2.8533(4) nm~3, Z = 4, M_r = 623.25 and D_c = 1.451 g·cm~(-3). The Ni(Ⅱ) atom is hexa-coordinated to furnish a slightly distorted octahedral geometry. Lattice water molecules are found in 1, and the H-bonding intersections formed novel water clusters. The IR, antibacterial activity and luminescence of 1 are studied.  相似文献   

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