Synthesis, Structure, Luminescence and Theoretical Investigations on a New Tin Complex with (2,3-f)-pyrazino(1,10)phenanthroline-2,3-dicarboxylic Acid

A new tin complex Sn(CH3 HPPDA)Cl4 (1) was prepared from SnCl4·5H2O with (2,3-f)-pyrazino(1,10)phenanthroline-2,3-dicarboxylic acid (H2PPDA) by solvothermal reaction in methanol, and characterized by single-crystal X-ray diffraction analysis, optical absorption spectrum and photoluminescence. Compound 1 crystallizes in a monoclinic centrosymmetric space group of P21/c with a = 12.418(2), b = 11.9467(12), c = 15.845(3), β= 107.948(7)°, V = 2236.2(6)3 , Z = 4, Mr = 594.78, Dc = 1.767 g/cm3 , μ= 1.651 mm-1 , F(000) = 1160, S = 1.023 and T = 293(2) K. The final R = 0.0847 and wR = 0.2431 for 3144 observed reflections with Ⅰ > 2σ(Ⅰ). The discrete mononuclear Sn(CH 3 HPPDA)Cl 4 complex is connected into a supramolecular network of 1 by intramolecular and intermolecular C-H···Cl and intermolecular C-H···O hydrogen bonding interactions. Compound 1 displays fluorescence with a lifetime value of about 7.58 ns in the visible region under visible-light excitation, and the origin of the luminescent emission is primarily assigned to the combination of intraligand charge-transfer of CH3 HPPDA and Cl--to-CH 3 HPPDA charge-transfer mechanism which is probed by the density of states (DOS) calculations.     

Synthesis, Crystal Structure, Luminescence Property and DFT Calculations of a New Coordination Compound Containing 8-Aminoquinoline Ligand

A new luminescent compound, Zn(8-aminoql)2(SCN)2 (1, 8-aminoql = 8-amino quinoline), has been synthesized and its structure was characterized by IR, elemental analysis and X-ray single-crystal diffraction. Compound 1 belongs to the orthorhombic system, space group Pbca with a = 8.503(2), b = 14.427(4), c = 31.922(8), V = 3916.0(18)3 , Z = 8, C20H16N6S2Zn, Mr = 469.88, D c = 1.594 Mg/m3 , μ = 1.488 mm-1 , F(000) = 1920, T = 296(2) K, the final R = 0.0293 and wR = 0.0645 for all 2763 observed reflections (Ⅰ > 2σ(Ⅰ)). Compound 1 displays a 3D supramolecular architecture formed by N H···S hydrogen bonds and π···π aromatic packing interactions. Photoluminescence studies reveal that it displays obvious fluorescent emission band (λ ex = 320 nm) at 533 nm in the solid state at room temperature. The emission bands possess a broad asymmetric feature, which can be assigned to ligand-to-ligand charge transfer transitions based on DFT calculations.     

Synthesis,Crystal Structure and Band Structure of Tb3Co4Sn（13）

A new intermetallic compound,Tb3Co4Sn13,has been synthesized by solid-state reaction of the corresponding pure elements in a welded tantalum tube at high temperature.Its crystal structure was established by single-crystal X-ray diffraction.Tb3Co4Sn13 crystallizes in cubic,space group Pm3n(No.223) with a = 9.5072(2) ,V = 859.33(3) 3,Z = 2,Mr = 2255.45,Dc = 8.717 g/cm3,μ = 34.369 mm-1,F(000) = 1906,and the final R = 0.0140 and wR = 0.0312 for 199 observed reflections with I > 2σ(I).The structure of Tb3Co4Sn13 belongs to the Yb3Rh4Sn13 type.It is isostructural with RE3Co4Sn13(RE = La,Ce),featuring a 3D [Co4Sn12] framework based on [CoSn6] trigonal prisms.The [CoSn6] trigonal prisms are interconnected via corner-sharing and Sn-Sn bonds to form a 3D [Co4Sn12] framework.The other Sn and Tb atoms are located in the spacers of the 3D framework.Band structure calculations indicate that Tb3Co4Sn13 is metallic.     

Synthesis and Crystal Structure of 2-O-(2-hydroxyethyl)-D-glucose

The title compound, 2-O-(2-hydroxyethyl)-D-glucose (C8H16O7 , Mr = 224.21), has been synthesized and its structure was characterized by using NMR spectrum and X-ray single-crystal diffraction. This molecule crystallizes in the monoclinic system, space group P21 , with a = 8.399(17), b = 6.620(14), c = 9.81(2), β = 115.110(17)°, V = 493.7(18)3 , Z = 2, Dc = 1.508 mg/m3 , μ = 0.13 mm-1 , F(000) = 240, the final R = 0.0464 and wR = 0.115 for 1521 observed reflections (Ⅰ > 2σ(Ⅰ)). X-ray crystal structure analysis revealed that the conformation of the pyranosyl ring existed in a slightly distorted 4C1 chair conformation (Cremer-Pople puckering parameters of Q = 0.573(4) , θ = 6.7(3)° and Ф = -5.2(2) °). The molecule exists as a monomer in the solid state, whose conformation is stabilized via multiple inter- and intramolecular hydrogen bonds.     

Synthesis and Structure of Ethyl 3-acetamido-4-aryl-6-methyl-2-oxo-3,4-dihydropyran-5-carboxylates

Two ethyl 3-acetamido-4-aryl-6-methyl-2-oxo-3,4-dihydropyran-5-carboxylates(3) were synthesized with high diastereoselectivities and characterized by IR,NMR and MS.The configuration of 3a was confirmed by single-crystal X-ray diffraction,ethyl 3-acetamido-4-(4-nitrophenyl)-6-methyl-2-oxo-3,4-dihydropyran-5-carboxylate(3a),C17H18N2O7.The crystal is of orthorhombic,space group Pbca with a = 11.7781(16),b = 9.5979(10),c = 32.115(3),V = 3630.4(7)3,Z = 8,Mr = 362.33,Dc = 1.326 Mg/m3,λ = 0.71073,μ(MoKα) = 0.104 mm-1,F(000) = 1520,the final R = 0.0646 and wR = 0.1464 for 1788 observed reflections with I > 2σ(I).The N-H and oxygen atom are involved in intermolecular hydrogen bonds which link the molecules into a one-dimensional chain and stabilize the structure.     

Crystal Structure, Photoluminescent, and Theoretical Studies of 3-Acetyl-8-methoxy-coumarin

The structure of 3-acetyl-8-methoxy-coumarin (AMC) was verified by single-crystal X-ray crystallography. It crystallizes in monoclinic, space group C2/c with a=15.073(3), b=13.068(3), c=11.549(2), β=119.92(3)o, V=1971.7(7)3 , Z=8, F(000)=912, D c=1.470 Mg/m3 , Mr=218.20, μ=0.111 mm-1 , the final R=0.0340 and wR=0.0968 for 1446 observed reflections with I > 2σ(I). The UV-vis absorption and fluorescence of AMC were discussed. The compound exhibits strong blue emission under ultraviolet light excitation. The molecular structure of AMC was optimized using density functional theory (DFT) at the B3LYP/6-31G(d) level, showing that the optimized geometer parameters are in good agreement with the experiment data. In addition, the HOMO and LUMO levels of AMC were deduced.     

Synthesis and Crystal Structure of (E)-Ethyl (9-bromo-5-oxo-4-phenyl-1,10b-dihydro-5H-pyrano [3,4-c] chromen-2-ylidene) Acetate

The crystal structure of the title compound (C22H17BrO5 , Mr = 441.27) has been determined by single-crystal X-ray diffraction. The crystal is of orthorhombic system, space group Pna21 with a = 11.76(1), b = 14.58(1), c = 11.52(1), V = 1973.93 , Z = 4, Dc = 1.485 g/cm3 , F(000) = 896, μ(MoKα) = 2.113 mm-1 , the final R = 0.0394 and wR = 0.0809 for 3918 observed reflections (Ⅰ > 2 (Ⅰ)). The single-crystal X-ray diffraction data indicate that the C=C bond is in an E-configuration. The intramolecular C(10)-H(10B)···O(4) and intermolecular C(17)-H(17)···O(4) hydrogen bonds contribute to the stability of the structure.     

Crystal Structure of Derivative of H_4′-NOBIN and the Applications in Hetero-Diels-Alder Reaction

Novel Schiff bases of H4′-NOBIN 5a and 5b were synthesized by condensation of 3 with aldehydes. Compound 5b was structurally characterized by single-crystal X-ray diffraction. The asymmetric hetero-Diels-Alder reactions were carried out with high yields and good enan-tioselectivities in the presence of Ti-(S)-5a complex as catalyst. Crystallographic data for 5b: C27H22BrNO, Mr = 456.37, triclinic, space group P1 with a = 9.1618(2), b = 10.3836(2), c = 12.7718(2), α = 105.4860(10),β = 94.6360(10), γ = 108.4610(10)o, V = 1092.32(4)3, Z = 2, Dc = 1.388 g/cm3, μ = 1.900 mm-1, F(000) = 468, R = 0.0476 and wR = 0.1248 for 3092 observed reflections (Ⅰ > 2σ(Ⅰ)).     

Synthesis, Crystal Structure and Antibacterial Activity of Two Hydrazones Derived from 2-Fluorobenzhydrazide

Two new Schiff base benzoyl hydrazone compounds, C14H10FN3O3 (Ⅰ) and C14H10F2N2O (Ⅱ), have been synthesized and characterized by elemental analysis, IR, UV and X-ray single-crystal diffraction. Both compounds crystallize in monoclinic, space group P21/c with a = 7.0514(14), b = 25.928(5), c = 7.7099(15), β = 111.823(2)°, V = 1308.6(4)3, Z = 4, C14H10FN3O3, Mr = 287.25, Dc = 1.458 g/cm3, μ(MoKα) = 0.115 mm-1, F(000) = 592, the final R = 0.0841 and wR = 0.2489 for 1901 observed reflections (I > 2σ(I)) for I; a = 11.232(3), b =12.735(4), c = 8.612(2) , β = 90.869(3)°, V = 1231.7(6)3, Z = 4, C14H10F2N2O, Mr = 260.24, Dc = 1.403 g/cm3, μ(MoKα) = 0.111 mm-1, F(000) = 536, the final R = 0.0453 and wR = 0.1085 for 1317 observed reflections (I > 2σ(I)) for Ⅱ. The antibacterial activities of both compounds against two bacteria were first studied and one compound showed considerable antibacterial activity against K. Pneumonia and S. aureus.     

Syntheses and Crystal Structures of Two New Macrocyclic Compounds

Two new macrocyclic compounds, [Cu2(L)2](ClO4)4·2CH3OH (1) and [Cu(L)](ClO4)2·2H2O (2) (L = 1,3,10,12,15,18-hexaazatetracyclodocosane) were synthesized by condensation reactions involving amines and formaldehyde in the presence of copper anion. Compound 1 crystallizes in triclinic, space group Pí with a = 10.442(2), b = 14.197(3), c = 17.388(4), α = 91.218(4), β = 90.69(3), γ = 93.756(4)o, V = 2520.4(9)3, Z = 2, F(000) = 1260, Dc = 1.589 Mg/m3, Mr = 1205.92, μ = 1.137 mm-1, λ = 0.71073, the final R = 0.0668 and wR = 0.1573 for 9703 observed reflections with I > 2σ(I). Compound 2 crystallizes in monoclinic, space group C2/c with a = 16.911(2), b = 11.4172(15), c = 27.059(4), β = 107.787(2)o, V = 4974.7(12)3, Z = 8, F(000) = 2504, Dc = 1.610 Mg/m3, Mr = 602.92, μ = 1.155 mm-1, λ = 0.71073 , the final R = 0.0419 and wR = 0.1131 for 4374 observed reflections with I > 2σ(I).     

Synthesis and Crystal Structure of (E)-2-(1-(2-Hydroxy-4-methoxyphenyl)ethylideneamino)-3-(4-hydroxyphenyl)methyl Propionate

(E)-2-(1-(2-Hydroxy-4-methoxyphenyl)ethylideneamino)-3-(4-hydroxyphenyl)methyl propionate (C22H27O6N, Mr = 401.45) has been synthesized by a condensation reaction of paeonol with tyrosin methyl ester hydrochloride, and its structure was determined by IR, NMR, HR MS and X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P21/c, with a = 11.91291(15), b = 9.49947(12), c = 19.8727(3) , β = 106.1104(15)°, V = 2160.60(5)3, Z = 4, Dc = 1.234 g/cm3, μ = 0.739 mm-1, F(000) = 856, R = 0.0466 and wR = 0.1461 for 3859 observed reflections with (Ⅰ> 2σ(Ⅰ)). In the crystal structure, the title compound is constructed by a centrosymmetric dimmer unit composed of a pair of π-π stacking enantiomers, and such units are linked by intermolecular O(5)-H(5)…O(1) and intramolecular N(1)-H(1)…O(1) hydrogen bonds.     

Synthesis, Crystal Structure and Luminescent Properties of the Indium(Ⅲ) Complex Based on 2,6-Bis(1-phenylbenzimidazol-2-yl)pyridine

The complex [In(bpbp)Cl3]·H2O, where bpbp is 2,6-bis(1-phenylbenzimidazol- 2-yl)-pyridine (bpbp), was synthesized and characterized by X-ray single-crystal structure analysis. For the complex: C31H21Cl3InN5·H2O, Mr = 702.71, monoclinic, space group, P21/n, a = 9.3918(10), b = 21.024(2), c = 14.5323(15), β = 96.938(2)°, V = 2848.4(5)3, Z = 4, Dc = 1.639 g/cm3, λ = 0.71073, μ(MoKα) = 1.147 mm-1, F(000) = 1408, S = 1.00, R = 0.0430 and wR = 0.1438 for 4620 observed reflections with Ⅰ > 2σ(Ⅰ). It is a neutral complex. The In(Ⅲ) ion adopts a distorted trigonal bipyramidal geometry coordinated by three nitrogen atoms of the ligand and three chlorine atoms. The complex emits blue luminescence with emission peaks at 430 nm in the solid state.     

Hydrothermal Synthesis and Crystal Structure of a New Three-dimensional Heterometallic Coordination Polymer

A new 3d-4f heterometallic polymer {[Sm2Cu(PDC)2(SO4)2(H2O)6]·2H2O}n 1 has been synthesized by Sm2O3, Cu(SO4)2·5H2O and pyridine-3,5-dicarboxylic acid under hydrothermal conditions. The compound crystallizes in triclinic system, space group P1, with a = 6.352(7), b = 10.040(10), c = 10.315(11) , α = 94.958(14), β = 95.556(7), γ = 99.747(14)°, V = 641.7(12)3, Z = 1, Mr = 1030.63, Dc = 2.651 Mg/m3, μ = 5.615 mm-1, F(000) = 491, the final R = 0.0491 and wR = 0.1345 for 2098 observed reflections with I > 2σ(I). The compound is a three-dimensional network structure in which infinite lanthanide-carboxylate chains are linked by [Cu(SO4)2]2- metalloligands to form a mixed-metal coordination network.     

Synthesis and Crystal Structure of Novel Mixed-metal Alkoxide Clusters of Ytterbium and Sodium: Yb4O4（OiPr）16Na12

The mixed-metal cluster Yb4O4(OiPr)16Na12 has been synthesized and structurally determined by IR, elemental analysis, and single-crystal X-ray diffraction. The crystal belongs to the cubic system, space group P23 with a = b = c = 13.9788(3), V = 2731.55(10)3 , Z = 1, Dc = 1.202 g/cm 3 , Mr = 1977.42, = 3.480 mm-1 , F(000) = 972, the final R = 0.0288 and wR = 0.1511 for 1677 observed reflections with Ⅰ > 2σ(Ⅰ). X-ray analysis reveals that Yb4O4 (OiPr)16Na12 is centrosym-metric and the structure contains four ytterbium metals and twelve sodium metals, and each ytterbium atom is coordinated by six oxygen atoms. In addition, an ancillary computational analysis of the optimized molecular unit was provided. The large energy gap (3.31 eV) between HOMO and LUMO indicates that the structure framework is particularly stable.     

Synthesis, Crystal Structure and Biological Activity of a New 1,2,4-Triazole Derivative

A new 1,2,4-triazole containing cyclopropane moiety was synthesized and characte- rized by 1H NMR, MS and elemental analyses. The crystal structure of the title compound (C13H14FN3S, Mr = 263.33) has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 12.614(3), b = 7.0202(14), c = 15.556(3), β = 110.92(3)°, V = 1286.7(4)3 , Z = 4, F(000) = 552, Dc = 1.359 g/cm 3 , μ = 0.25 mm-1 , the final R = 0.0336 and wR = 0.0898 for 2568 observed reflections with Ⅰ > 2σ(Ⅰ). A total of 10093 reflections were collected, of which 3045 were independent (Rint = 0.0268). The herbicidal activity of the title compound was determined, and this compound displays excellent herbicidal activity against Brassica campestris.     

Synthesis and Crystal Structure of a Two-dimensional Cadmium Complex Based on Terephthalate and 1-Methyl-2,2'-bibenzimidazole

The title complex, Cd(MeHbibzim)(1,4-bdc)n (1, MeHbibzim = 1-methyl-2,2'- bibenzimidazole, 1,4-bdc = terephthalate), was synthesized with hydrothermal reactions. The compound crystallizes in monoclinic, space group C2/c with a = 9.822(4), b = 18.510(7), c = 22.372(9), β = 98.359(6)°, C23H16CdN4O4 , Mr = 524.81, V = 4024(3)3 , Z = 8, Dc = 1.733 g/cm3 , μ(MoKα) = 1.126 mm-1 , F(000) = 2096, the final R = 0.0597 and wR = 0.1374 for 3906 observed reflections (Ⅰ > 2σ(Ⅰ)). X-ray diffraction analysis reveals that the Cd atom is coordinated by two nitrogen atoms from the chelating MeHbibzim and three carboxyl oxygen atoms from three terephthalate ligands, thus forming a distorted square pyramidal coordination sphere, CdN2O3. Every two Cd atoms are linked together via two carboxyl groups into a dinuclear unit with Cd···Cd separation of 3.806(4). The dinuclear building units are linked by terephthalate ligands into two-dimensional layers, which are further aggregated into a 3D framework via hydrogen bonding interactions.     

Synthesis and Crystal Structure of [K（2,2,2-crypt）]_3Sb_（11）

The title complex [K(2,2,2-crypt)]3Sb11 has been prepared by the reaction of K3Cd2Sb with Cu-C≡CH in ethylenediamine in the presence of 2,2,2-crypt, and characterized by low temperature X-ray structure analysis. The crystal is of orthorhombic system, space group C2221 with a = 15.475(3), b = 22.807(5), c = 24.834(6), V = 8765(3)3, Dc = 1.960 g/cm3, C54H108K3N6O18Sb11, Mr = 2586.01, F(000) = 4944, μ = 3.531 mm-1, Z = 4, R = 0.0442 and wR = 0.1053 for 10265 observed reflections (I > 2σ(I)). The "naked" Sb113- anion is stable due to the completely sequestered alkali metal cations through ion-ion interactions.     

Synthesis and Crystal Structure of Tetrakis（1- vinylimidazole-kN^3）diisothiocyanatomanganese（II）

The title compound I （C22H24MnN10S2, Mr = 547.57） has been synthesized and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the monoclinic system, space group P2 1/c with a = 8.6010（17）, b = 9.0180（18）, c = 17.773（4）A, β = 101.79（3）°, V = 1349.5（5）A^3, Z = 2, Dc = 1.348 g/cm^3,/1 = 0.674 mm^-1, F（000） = 566, the final R = 0.0488 and wR = 0.1289. In the structure, each Mn atom is coordinated by four Vim （Vim = 1-vinylimidazole） ligands and a pair of monodentate isothioeyanic groups, affording a compressed oetahedral MnN6 core.     

Synthesis and Crystal Structure of a Ruthenium（Ⅱ） Compound of Dinitrogen

The title compound [Ru（bph）（PPh3）2（N2）]·（PF6）·1.5CH2Cl2 （bph = N-（benzoyl）- N＇-（picolinylidene）-hydrazine） has been prepared and characterized by X-ray diffraction analysis. It crystallizes in the monoclinic system, space group P21/n with a = 13.5201（6）, b = 15.5078（6）, c = 25.0656（13） A, β= 100.257（3）°, C50.50H43Cl3F6N5OP3Ru, Mr= 1150.23, V= 5171.4（4） A3, Z = 4, F（000） = 2332, Dc = 1.477 g/cm^3 and ,μ（MoKa） = 0.615 mm^-1. The structure was refined to R = 0.0524 and wR = 0.1398 for 8060 observed reflections （I 〉 2σ（I））. The Ru-N2 and N-N bond distances are 1.919（4） and 1.133（5）A, respectively.     

Synthesis and Crystal Structure of （E）-N,N＇- dicyclohexyl- 1-（3-（3,4-dihydroxyphenyl）acryloyl）urea

The title compound, (E)-N,N′-dicyclohexyl-1-(3-(3,4-dihydroxyphenyl)acryloyl)- urea (DDA), has been synthesized and characterized by FT-IR and 1H-NMR spectroscopy, ESI- MS, and X-ray single-crystal diffraction. Its crystallizes in monoclinic, space group C2/c with a = 20.483(12), b = 11.153(6), c = 21.134(12) , β = 117.098(7), V = 4298(4) 3, Z = 8, F(000) = 1664, Dc = 1.195 Mg/m3, Mr = 386.48, μ= 0.082 mm-1, the final R = 0.0474 and wR = 0.1370 for 4853 observed reflections with I > 2σ(I).