Crystal Data For Compound Research Articles

Synthesis of Tetrahydrocarbazole-Tethered Triazoles as Compounds Targeting Telomerase in Human Breast Cancer Cells

Telomere shortening and the induction of senescence and/or cell death may result from inhibition of telomerase activity in cancer cells. Herein, the properties of carbazole–triazole compounds targeting telomerase in human breast cancer cells are explored. All derivatives were evaluated for loss of viability in MCF-7 breast cancer cells, with compound 5g identified as the most potent within the examined series. Green synthesis was employed using water, a reusable nano-Fe2O3-catalyzed reaction, and an electrochemical method for the synthesis of tetrahydrocarbazole and triazoles. The crystal data of compound 4 is also reported. Furthermore, in silico analysis predicted that compound 5g may target human telomerase. Molecular docking analysis of compound 5g towards hTERT predicted a binding affinity of −6.74 kcal/mol. In flow cytometry assays, compound 5g promoted apoptosis and cell cycle arrest in the G2-M phase. Finally, compound 5g inhibited the enzymatic activity of telomerase in human breast cancer cells. In conclusion, a green synthesized series of carbazole–triazoles that target telomerase in cancer cells is reported.

Identification, structural revision and biological evaluation of the phyllocladane-type diterpenoids from Callicarpa longifolia var. floccosa

Phyllocladane-type diterpenoids represent a rare group of tetracyclic diterpenes. Two diterpenoids (1 and 2) were extracted from Callicarpa longifolia var. floccosa, along with the Chemically synthesized derivatized compound 3. The crystal data for compound 1 were first reported in this study, and compound 2 was identified as a novel phyllocladane-type diterpenoid. In addition, calliterpenone monoacetate was previously erroneously reported as compound 2. We corrected the structure of calliterpenone monoacetate to 2a by X-ray diffraction, NMR calculations, and chemical synthesis, as well as the TDDFT-ECD method. At the same time, the antitumor activity of compounds 1 and 2 was studied.

Flux synthesis and characterization of two barium hydroxyborosilicates with triple and single tetrahedral layers: Ba2[Si3B3O12(OH)] and Ba[Si2BO6(OH)

Two new barium hydroxyborosilicates, Ba2[Si3B3O12(OH)] (1) and Ba[Si2BO6(OH)] (2), have been synthesized by a flux method at 480 ​°C and characterized by single-crystal X-ray diffraction and infrared spectroscopy. Both compounds have 2D layer structures. Compound 1 contains planar slabs of borosilicate formed of tetrahedral building units which can be described as condensation of three 3-connected 2D single layers with a 63 network topology. The Ba2+ cations are located in both the interlayer and intralayer regions. The structure is unusual with respect to the triple tetrahedral layers. Compound 2 consists of very contorted (3,4)-connected single layers with the rare (42.62)(4.62)2 topology. The single layer is composed of both tertiary and quaternary tetrahedra. The synthesis method is new. A mixture of Ba(OH)2·8H2O, H3BO3 and SiO2 was sealed in a gold ampoule, heated at high temperature in a pressure vessel, and the flux is a small amount of concentrated aqueous hydroxide solution. Crystal data for compound 1: monoclinic, P21/n, a ​= ​4.7112(2) Å, b ​= ​29.9482(14) Å, c ​= ​7.3773(4) Å, β ​= ​92.593(2)°, V ​= ​1039.81(9) Å3, Z ​= ​4, and R1 ​= ​0.0246; compound 2: monoclinic, P21/c, a ​= ​7.4206(2) Å, b ​= ​8.9405(2) Å, c ​= ​8.5677(2) Å, β ​= ​90.208(1)°, V ​= ​568.41(2) Å3, Z ​= ​4, and R1 ​= ​0.0467.

Researches on the construction of supramolecular helical chains in crystallized β-alaninium sulfate/ perchlorate compounds

A new compound, (H2L)2SO4 (1) (HL = β-alanine), was synthesized and studied based on X-ray single crystal diffraction analysis. β-alanine molecular displays two kinds of molecule torsion geometries (I and II) in compound 1, which construct supramolecular Z-shaped chains and supramolecular helical chains respectively. Based on our understanding of the helical packing mechanism of β-alanine in compound 1, we predicted and found supramolecular helical chains in another compound H2LClO4 (2) for the first time, although the crystal data of compound 2 has been reported previously. The way of simple β-alanine self-organizing into supramolecular helical chains was discussed in detail by comparing the structure of the compound 1 and compound 2, which may be important for understanding the way of simple molecules self-organizing into supramolecular helical structure and offers a good case for achiral ligands to construct supramolecular helical chains.

An efficient route for the synthesis of some monoazo disperse dyes derived from nicotinic acid derivatives

Ethyl 2-amino-3-cyano-4-phenylnicotinates ( 8 ), could be readily synthesized via reacting ethyl propiolate with benzylidenemalononitrile in the presence of L-proline as a catalyst and subsequent rearrangement of the so formed 2-aminopyran ( 7 ), with acetic acid in the presence of ammonium acetate. A series of 2-amino and 2-hydroxyarylazonicotinates monoazo disperse dyes ( 12a - c ), were prepared in a good yields via condensation of arylhydrazonals ( 11a - c ), with active methylene nitriles. The compound 9 was also characterized by single crystal X-ray diffraction studies. Crystal data for compound 9 , C 15 H 18 O 6 ( M = 294.29): hexagonal, space group P6 5 (no. 170), a = 11.3311(5) Å, c = 19.5375(10) Å, V = 2172.42(18) Å 3 , Z = 6, T = 296(2) K, μ(MoKα) = 0.879 mm -1 , Dcalc = 1.350 g/mm 3 , 4546 reflections measured (9.02 ≤ 2Θ ≤ 132.96), 2271 unique ( R int = 0.0921) which were used in all calculations. The final R 1 was 0.0686 (>2σ(I)) and wR 2 was 0.1691 (all data).

A 2-D coordination polymer with Cu4 IS4-core as joints

A coordination polymer based on copper(I) and a heterocyclic thione ligand, HPPT4 (HPPT4 = 4-pyridin-4-yl-pyrimidine-2-thiol) has been prepared. The compound C21H19Cu2N7OS2 (1) has a 2-D polymeric structure with -core as joints linked by μ-thiolate bridges. Crystal data for compound 1: Monoclinic, space group C2/c, a = 22.346(14) Å, b = 15.649(10) Å, c = 13.588(9) Å, β = 97.183(12)°, V = 4714(5) Å3, and Z = 8. Compound 1 displays multiple emissions with maximum wavelength at 391 and 469 nm under photoexcitation at 340 nm.

Synthesis and Electrochemical Properties of a New 1D Organic–Inorganic Hybrid Compound Based on Keggin-Type Heteropolyanions and Isopolyanions Decorated by Transition Metal Fragments

A new chain-like organic–inorganic hybrid compound composed of the heteropolyanions and isopolyanions, [{CuII(2,2′-bpy)}6(MoVMoVI5O22)] [PMoVI12O40] · H2O 1 (bpy = 2,2′-bipyridine) has been hydrothermally synthesized and characterized by elemental analysis, IR spectroscopy, TG analysis, XPS spectrum and single-crystal X-ray diffraction. Crystal data for compound 1: monoclinic, space group P2(1)/c, a = 13.9382(14) A, b = 20.0300(19) A, c = 17.1757(17) A, β = 94.054(2)°, V = 4783.2(8) A3, Z = 2. The Keggin-heteropolyanion [PMo12O40]3− and the Cu-supporting isopolyanion [{Cu(2,2′-bpy)}6(Mo6O22)]3+ building units are bridged through the O–Cu–O bridges into 1D infinite chain. Note that, the [{Cu(2,2′-bpy)}6(Mo6O22)]3+ unit, which contains a rarely reported isopolyanion [Mo6O22]9− decorated by six [Cu(2,2′-bpy)] fragments. Furthermore, the electrochemical behavior of a 1-modified carbon paste electrode (1-CPE) and its electrocatalytic reduction of nitrite were investigated.

A New Sandwich Polyoxometalate Constructed from a Zn 6 12+ Hexagon Cluster Sandwiched by Two B-α-[BiW9O33]9−

A new sandwich polyoxometalate Na4Zn2[Zn2(H2O)10(ZnCl)6(B-α- BiW9O33)2] · 40.5H2O (1) has been obtained in aqueous solution and characterized by IR, UV, element analysis, TG and single-crystal X-ray analysis. Polyoxoanion 1 is composed of a Zn 6 12+ hexagon sandwiched by two [BiW9O33]9− units, which is firstly observed in tungstobismutate. The crystal data for compound 1: Triclinic, space group P–1, a = 15.426(3) A, b = 15.467(3) A, c = 15.526(3) A, α = 74.24(3)°, β = 64.37(3)°, γ = 60.73(3)°, V = 2905.3(1) A3, Z = 1.

Assembly of hexad-track Ag–N coordination polymeric chain-modified Keggin polyoxometalates

Two new organic–inorganic hybrid compounds based on the Keggin POMs modified by hexad-track Ag–N coordination polymeric chains, {[Ag(bipy)] 3[HXW 12O 40]}[bipy] (X = Si 1, Ge 2) (bipy = 4,4′-bipyridine), have been hydrothermally synthesized and structurally characterized. Crystal data for compound 1: C 40H 33Ag 3N 8O 40SiW 12, triclinic, space group P-1, a = 11.369, b = 12.087, c = 13.110, α = 112.88, β = 94.43, γ = 99.49, V = 1617.2; for compound 2: C 40H 33Ag 3N 8O 40SiW 12, triclinic, space group P-1, a = 11.383, b = 12.119, c = 13.136, α = 112.95, β = 94.35, γ = 99.51, V = 1626.0. They represent important examples of the POM family which are modified by Ag complexes. By changing POMs, compound 3 (H 2bipy) 2[SiMo 12O 40] has been obtained, which exhibits a supramolecular structure. Their structural differences reveal that the abilities of oxidation of POMs play a major role in their modification of POMs by the transition metal Ag.

Synthesis and Characterization of a Novel 3D Organic–Inorganic Hybrid Framwork Templated by Keggin Anions

A novel 3D compound, {K3H2[Cu(Gly)2]3BW12O40}·10H2O 1 (Gly = glycine), has been synthesized and characterized by elemental analyses, IR, TG analyses, cyclic voltammetry, and single-crystal X-ray diffraction. Compound 1 contains square-grid layers constructed by potassium cations and copper-glycine coordination complexes, the [BW12O40]4− anions as templates are accommodated in the square grids by connecting with the K atoms. The K atoms link [BW12O40]4− anions from different layers together to yield a 3D novel structure. The crystal data for compounds 1: monoclinic, space group p2(1)/n, a = 18.832(4) A, b = 16.488(3) A, c = 20.570(4) A, β = 106.21(3)°, V = 6133(2) A3, Z = 4.

An interesting fourfold interpenetrating network constructed by polyoxometalates and metal–organic coordination complexes: [formula omitted

A novel fourfold interpenetrating 3D network compound, [ Cu I 5 ( bpy ) 5 ( H 2 O ) 2 ] [ [ Cu II ( H 2 O ) 3 ] 2 Cu II [ P 4 Mo V 6 O 25 ( OH ) 6 ] 2 ] · H 3 O + · 2 H 2 O 1 (bpy = 4,4′-bipyridine), has been synthesized and characterized by elemental analyses, IR, TG analyses, and single-crystal X-ray diffraction. Compound 1 is built up of Cu[P 4Mo 6O 25(OH) 6] 2 clusters covalently linked by Cu-bpy coordination polymer chains to yield unusual two-dimensional layers, which are further connected together by metal coppers to produce an interesting fourfold interpenetrating 3D network structure. The crystal data for compounds 1: Triclinic, space group P 1 ¯ , a = 12.714(3) Å, b = 14.882(3) Å, c = 15.369(3) Å, α = 72.74(3)°, β = 72.12(3)°, γ = 65.62(3)°, V = 2471.9(9) Å 3, Z = 1.

Two new hydrogen bond-supported supramolecular compounds assembly from polyoxovanadate and organoamines

Two novel organic–inorganic hybrid compounds based on organoamines and polyoxovanadates formulated as (H 2dien) 4[H 10V 18O 42(PO 4)](PO 4)·2H 2O ( 1) (dien=diethylenetriamine) and (Him) 8[HV 18O 42(PO 4)] ( 2) (im=imidazole) have been prepared under hydrothermal conditions by using different starting materials, and characterized by elemental analyses, IR, ESR, XPS, TGA and single-crystal X-ray diffraction analyses. Crystal data for compound 1: C 16H 74N 12O 52V 18P 2, Monoclinic, space group C2 /c, a=23.9593(4) Å, b=13.0098(2) Å, c=20.1703(4) Å, β=105.566(3)°, V=6056.6(19) Å 3, Z=4; for compound 2, C 24H 41N 16O 46V 18P, Tetragonal, space group I4 /mmm, a=13.5154(8) Å, b=13.5154(8) Å, c=19.1136 Å, β=90°, V=3491.4(3) Å 3, Z=2. Compound 1 consists of protonated diens together with polyoxovanadates [H 10V 18O 42(PO 4)] 5−. Compound 2 is composed of protonated ims and polyoxovanadates [HV 18O 42(PO 4)] 8−. There are hydrogen-bonding interactions between polyoxovanadates and different organoamines in 1 and 2. Polyoxovanadates are linked through H 2dien into a three-dimensional network via hydrogen bonds in 1, while polyoxovanadates are linked by Him into a two-dimensional layer network via hydrogen bonds in 2. The crystal packing patterns of the two compounds reveal various supramolecular frameworks.

A new grid network based on diphosphopentamolybdate cluster supported transition metal complexes

A new grid architecture built from diphosphopentamolybdate supported copper-imidazole, [{CuII(im)4}2{H2Mo5P2O23}] · 3H2O · (im) (1) (im = imidazole), is reported. The structure of 1 features a 2-D grid network built by the interconnection of bisupporting diphosphopentamolybdate clusters, [{CuII(im)4}2{H2Mo5P2O23}]; free water molecules and imidazole ligands fill the void of the crystal lattice. Crystal data for compound 1: Orthorhombic, space group Pnma, a = 14.598(3) Å, b = 21.059(4) Å, c = 16.609(3) Å, α = β = γ = 90°; V = 5106.1 Å3; Z = 4.

Two New Three-Dimensional Networks Constructed on Polyoxovanadates

To investigate the role of polyoxovanadates in network connectivity, two new organic–inorganic hybrid vanadates with three-dimensional entangled coordination frameworks, namely [Cu2(biim)3V4O12] 1 and [Co2(biim)3V4O12]·4H2O 2 have been synthesized and characterized by infrared (IR), thermogravimetric analysis (TGA), and single-crystal X-ray diffraction. Crystal data for compound 1: triclinic, P-1, a 9.504(2), b 10.650(2), c 11.993(2) Å; α 72.13(3), β 76.02(3), γ 65.40(3)°; V 1041.4(4) Å3, Z 2, R(final) 0.0492. Crystal data for compound 2: triclinic, P-1, a 9.037(3), b 10.577(2), c 11.9470(2) Å; α 87.80(3), β 81.71(3), γ 85.29(3)°; V 1125.8(4) Å3, Z 1, R(final) 0.0774. Compound 1 is a three-dimensional inclined hetero-catenated framework designed from two two-dimensional sub-layers, [Cu(biim)V4O12] and [Cu(biim)2]. Compound 2 is a rare case of a self-catenated ‘ilc’ network that displays an unusual 424·5·63 topology with the binuclear {Co2O4N6} units as eight-connected nodes.

Organically templated uranium(iv) fluorooxalates with layer structures: (H4TREN)[U2F6(C2O4)3]·4H2O (TREN = tris(2-aminoethyl)amine) and (H4APPIP)[U2F6(C2O4)3]·4H2O (APPIP = 1,4-bis(3-amino-propyl)piperazine)

Two organically-templated layered uranium(IV) fluorooxalates, (H(4)TREN)[U(2)F(6)(C(2)O(4))(3)].4H(2)O (1) (TREN = tris(2-aminoethyl)amine) and (H(4)APPIP)[U(2)F(6)(C(2)O(4))(3)].4H(2)O (2) (APPIP = 1,4-bis(3-aminopropyl)piperazine), have been synthesized by hydrothermal methods and structurally characterized by single-crystal X-ray diffraction, thermogravimetric analysis, and magnetic susceptibility. Both structures consist of anionic [U(2)F(6)(C(2)O(4))(3)](4-) layers separated by organic ammonium cations and lattice water molecules. The UF(3)O(6) polyhedra are connected by oxalate ligands in different ways within the layers. They are the first examples of organically-templated uranium fluorooxalates. Crystal data for compound 1 follow: monoclinic, P2(1)/c (No. 14), a = 19.1563(5) A, b = 8.9531(2) A, c = 16.6221(4) A, beta = 114.633(1) degrees, and Z = 4. Crystal data for compound are the same as those for 1 except a = 10.3309(8) A, b = 15.564(1) A, c = 17.537(1) A, and beta = 95.430(4) degrees.

Two unprecedented inorganic–organic boxlike and chainlike hybrids based on arsenic–vanadium clusters linked by nickel complexes

Two novel organic–inorganic hybrid arsenic-vanadates, [{Ni(en) 2} 4(4,4′-bipy) 4{Ni(H 2O) 2}] 2[As 8V 14O 42(NO 3)] 4·16H 2O 1 and [Ni(en) 2(H 2O) 2] 2[{Ni(en) 2(H 2O)} 2As 8V 14O 42(NO 3)][{Ni(en) 2}As 8V 14O 42(NO 3)]·6H 2O 2 are reported in this study. Crystal data for compound 1: Tetragonal, I4/ m, a=27.507(4) Å, b=27.507(4) Å, c=22.101(4) Å; V=16722(5) Å 3, Z=2, R(final)=0.0508. Crystal data for compound 2: Triclinic, P–1, a=11.530(2) Å, b=14.883(3) Å, c=21.330(4) Å, α=76.94(3)°, β=76.58(3)°, γ=69.54(3)°, V=3293.4(1) Å 3, Z=1, R(final)=0.0559. The boxlike structure of compound 1 is designed from [{Ni(en) 2} 4(4,4′-bipy) 4{Ni(H 2O) 2}] sheets pillared by [ α-As 8V 14O 42] clusters, which represents the first mixed-organic ligand-decorated tetrameric As–V–O cluster. Compound 2 is constructed from the rarely [ β-As 8V 14O 42] clusters and Ni coordination complex fragments. The electrochemical property and magnetic property of compound 1 have been studied.

Synthesis and structure of the first organic–inorganic hybrid tin (II) chlorosulfate: [C 6N 2H 14][SnCl 2SO 4

The first organic–inorganic hybrid tin (II) chlorosulfate [C 6N 2H 14][SnCl 2SO 4] ( I) has been synthesized hydrothermally in the presence of organic amine 1,4-diazobicyclo[2,2,2]octane (DABCO) and characterized by single-crystal X-ray diffraction, IR, ICP and elemental analysis and thermogravimetric analysis and its structure solved by single-crystal X-ray diffraction. The structure of I consists of [SnCl 2SO 4] 2− anions and diprotonated DABCO cations resulting in the formation of a 2D supramolecular network based on hydrogen bonds which contact between diprotonated DABCO cations and [SnCl 2SO 4] 2− anions. Crystal data for compound I, orthorhombic space group C222 1, a = 9.354(6) Å, b = 9.6880(7) Å, c = 13.2888(9) Å, V = 1204.32(14) Å 3, Z = 4, M = 399.84(1), D calc = 2.205 g cm −3, Mo Kα, R 1 = 0.0254, wR 2 = 0.0616, GOF = 1.092.

Hydrothermal synthesis and characterization of two new bicapped Keggin heteropoly tungstovanadated derivatives

Two new heteropoly tungstovanadate derivatives, [Fe(phen) 3] 2[W 10.5V 4.5O 42]·3H 2O (1) and [Fe(phen) 3] 2[W 10V 5O 42].6H 2O (2) (phen=1,10′-phenanthroline), have been synthesized under hydrothermal conditions by using different starting materials, and characterized by elemental analysis, IR, ESR, XPS, TGA and single-crystal X-ray diffraction analysis. Crystal data for compound 1: C 72H 54Fe 2N 12O 45V 4.5W 10.5, monoclinic, space group C2/c, a = 30.244 ( 9 ) Å , b = 13.586 ( 3 ) Å , c = 24.707 Å , β = 99.882 (8)°, V = 10002 (5) Å 3, Z = 4 ; for compound 2, C 72H 60Fe 2N 12O 48V 5W 10, monoclinic, space group C2/c, a = 30.246 (6) Å, b = 13.909 ( 3 ) Å , c = 25.329 (5) Å, β = 100.34 (3)°, V = 10483 (4) Å 3, Z = 4 . The crystal structure analysis reveals that both polyoxoanions are decorated with the [Fe(phen) 3] 2+ cations , and that they have analogous structure to each other with slightly different packing modes of the polyoxoanions, [Fe(phen) 3] 2+ cations and water molecules. They are further linked to form two-dimensional (2D) supramolecular networks through extensive hydrogen bonding.

Hydrothermal synthesis and structural characterization of two unprecedented coordination polymers: {Co 3[O 2C(CH 2) 4CO 2] 3[1,10′-phen] 2} n and {Co 2[O 2C(CH 2) 3CO 2] 2[1,10′-phen] 2} n

Two new cobalt (II) containing coordination polymers {Co 3[O 2C(CH 2) 4CO 2] 3[1,10′-phen] 2} n ( 1) and {Co 2[O 2C(CH 2) 3CO 2] 2[1,10′-phen] 2} n ( 2) have been synthesized under the hydrothermal condition and characterized by elemental analyses, IR, TG analyses and the single crystal X-ray diffractions. Crystal data for compound 1: C 42H 42Co 3N 4O 12, triclinic P-1, a=9.0014(18) Å, b=9.0573(18) Å, c=13.327(3) Å, α=97.93(3), β=100.06(3), γ=104.85(3), Z=1. Crystal data for compound 2: C 34H 32Co 2N 4O 8, monoclinic P2(1)/ c, a=10.537(2) Å, b=20.780(4) Å, c=13.471(3) Å, β=100.63(3), Z=4. Compound 1 exhibits a novel two-dimensional layer framework, in which the trinuclear Co clusters are linked by adipate anions. Compound 2 represents a one-dimensional chain. Furthermore, the magnetic behavior of compound 2 is studied.

Hydrothermal synthesis and structure of an unprecedented layered Cd-citrate complex containing helical chains

An exploration of the cadmium-citrate system under hydrothermal conditions, has led to the isolation of a novel framework [Cd 3(H 2O) 2(C 6H 5O 7) 2] n 1. This compound features a novel 2D undulated sheet containing infinite double-stranded helical chains, which is unique among metal-citrate system identified so far. Crystal data for compound 1: Monoclinic, Space group P2 1 / c, a=6.0974(12) Å, b=15.271(3) Å, c=9.781(2) Å, β=102.74(3)°, V=888.3(3) Å 3, Z=2. Other characterizations by elemental analysis, IR and TG are also described.