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C32H48CoMo2N16O7, triclinic, P1‾ $P\overline{1}$ (no. 2), a = 10.425(2) Å, b = 10.517(2) Å, c = 11.187(2) Å, α = 94.671(7)°, β = 112.270(6)°, γ = 104.108(7)°, V = 1080.0(3) Å3, Z = 1, Rgt (F) = 0.0407, wRref (F 2) = 0.1015, T = 273 K.

C24H36N6O28V10, monoclinic, P21/c (no. 14), a = 10.4869(6) Å, b = 11.5123(7) Å, c = 17.4627(9) Å, β = 108.459(3)°, V = 1999.8(2) Å3, Z = 2, Rgt (F) = 0.0209, wRref (F 2) = 0.0582, T = 296 K.

C19H20N4O6Zn, monoclinic, P21/n (no. 14), a = 11.7411(7) Å, b = 13.7831(9) Å, c = 13.5425(10) Å, β = 97.564(2)∘ $97.564{(2)}^{\circ }$ , V = 2172.5(3) Å3, Z = 4, R gt(F) = 0.0645, wR ref(F 2) = 0.1643, T = 298 K.

C32H48CoMo2N16O7, triclinic, P 1 ‾ (no. 2), a = 10.425(2) Å, b = 10.517(2) Å, c = 11.187(2) Å, α = 94.671(7)°, β = 112.270(6)°, γ = 104.108(7)°, V = 1080.0(3) Å3, Z = 1, Rgt(F) = 0.0407, wRref(F2) = 0.1015, T = 273 K. [ABSTRACT FROM AUTHOR]

C24H36N6O28V10, monoclinic, P21/c (no. 14), a = 10.4869(6) Å, b = 11.5123(7) Å, c = 17.4627(9) Å, β = 108.459(3)°, V = 1999.8(2) Å3, Z = 2, Rgt(F) = 0.0209, wRref(F2) = 0.0582, T = 296 K. [ABSTRACT FROM AUTHOR]

C20H16Li5NO13, orthorhombic, Pnma (no. 62), a = 9.9218(8) Å, b = 14.6941(11) Å, c = 13.5697(10) Å, V = 1978.4(3) Å3, Z = 4, Rgt(F) = 0.0439, wRref(F2) = 0.0960, T = 173(2) K.

Two thiacalix[4]arene-protected silver(I) alkynyl nanoclusters, [Na2(H2O)2][Ag9(TC4A)(tBuC≡C)4(CH3OH)2(SbF6)0.5(OH)2.5]·3.5H2O·CH3OH (1, abbreviated as Ag9) and [Ag9(TC4A)(tBuC≡C)4(CF3COO)]2·4CH3OH (2, abbreviated as Ag18), were synthesized by the reaction of [tBuC≡CAg]n, p-tert-butylthiacalix[4]arene (H4TC4A), NaBH4, and AgSbF6 or CF3COOAg in the mixed solvent of methanol-trichloromethane-toluene under solvothermal conditions, respectively. Driven by SbF6− and CF3COO− with different coordination properties, the structural unit [Ag9(TC4A)(tBuC≡C)4]+ in both the compounds migrated in different modes, accompanied by distinct Ag⋯Ag distances. Ag9 and Ag18 exhibit similar UV-Vis absorption and diffuse reflection spectra along with contrary tendency between photocurrent responses and solid-state fluorescence. The solution stability of Ag9 and Ag18 was demonstrated by 1H NMR and MALDI-TOF mass spectrometry. The fluorescence responses of Ag9 and Ag18 towards different organic molecules were also investigated, which indicated that the polarity of solvent has a certain effect on the emission intensities of Ag9 and Ag18. This study provides a positive guide for the controlled synthesis and further study of the structure–activity relationship of thiacalix[4]arene-protected silver alkynyl nanoclusters. [ABSTRACT FROM AUTHOR]

C9H4Na2O6, monoclinic, C2/c (no. 15), a = 14.6828(15) Å, b = 9.8602(10) Å, c = 6.5024(7) Å, β = 101.360(4)°, V = 922.94(17) Å3, Z = 4, Rgt(F) = 0.0337, wRref(F2) = 0.0775, T = 173(2) K.

Structural transformation is important for the study of silver cluster compounds, in which controlled synthesis of their shapes and sizes via anion template‐driven is one key scientific question. In this work, the CO32− anion templates were captured by the [tBuC≡CAg]n system under the stimulation induced by carboxylate ligand CF3COO−/PhCOO−, and two silver alkynyl clusters [(CO32−)@Ag21(tBuC≡C)16(CF3COO)3(H2O)]⋅DMF⋅2CH2Cl2 (1) and [(CO32−)2@Ag24(tBuC≡C)16(PhCOO)4]⋅CH3OH⋅4DMF (2) have been successfully isolated and charactered. With the increase of the number of CO32− templates from single to double, the outer silver atoms from twenty‐one to twenty‐four, accompanied by the growth of the cluster skeleton from 9.8 Å ×6.9 Å of the (CO32−)@Ag21 unit to 10.5 Å ×7.3 Å of the (CO32−)2@Ag24 unit. In addition, the syntheses, structures, photocurrent responses, cyclic voltammetry characteristics, luminescence, and photodegradation of compounds 1 and 2 have been studied. [ABSTRACT FROM AUTHOR]

C19H20N4O6Zn, monoclinic, P21/n (no. 14), a = 11.7411(7) Å, b = 13.7831(9) Å, c = 13.5425(10) Å, β = 97.564 (2) ∘ , V = 2172.5(3) Å3, Z = 4, Rgt(F) = 0.0645, wRref(F2) = 0.1643, T = 298 K. [ABSTRACT FROM AUTHOR]

Compound [Ag44(W10O32)(StBu)24(CF3COO)8](CF3COO)6 ⋅ 6H2O (1) was synthesized through a one‐pot method. This is the first case of isolating a new silver thiolate cluster containing a [W10O32]6− template which transforms from WO42− polyoxoanion through a self‐assembly process. The anionic nature of the reduced [W10O32]6− template and the effective silver‐oxygen interaction contribute to the formation of the Ag44 nanowheel in 1. The luminescence, photocatalytic activity and electrochemistry properties of 1 were studied. [ABSTRACT FROM AUTHOR]

Three trinuclear silver nanoclusters, [Ag3(dppm)3(tBuC≡C)](CF3SO3)2 (1), [Ag3(dppm)3(CO3)(CH3OH)](CF3SO3)·H2O (2) and [Ag3(dppm)3(Cl)2](CF3SO3)·3DMF (3) (dppm = 1,2-bis-(diphenylphosphino)methane) were obtained and characterized by a series of techniques including single-crystal X-ray diffraction (SCXRD), Fourier transform infrared spectrometry (FT-IR), powder X-ray diffraction (PXRD) and thermogravimetric analysis (TGA). In the three compounds, their main body skeletons are made up of similar Ag3 cores shaped in a silver triangle. All the three compounds consist of three silver atoms, three dppm bis-(phosphine) ligands, which are further stabilized by CF3SO3− anions. While the other auxiliary ligands, tBuC≡C−, CO32− and Cl− are separately attached to similar Ag3 cores, making them structurally different. Moreover, the luminescence properties, photocurrent responses and electrochemical properties of compounds 1–3 have been investigated. The results indicate that different structures have a very important influence on their properties. The structure–activity relationship of silver cluster materials provides positive guidance for further design and synthesis of functional silver cluster materials. [ABSTRACT FROM AUTHOR]

C20H16Li5NO13, orthorhombic, Pnma (no. 62), a = 9.9218(8) Å, b = 14.6941(11) Å, c = 13.5697(10) Å, V = 1978.4(3) Å3, Z = 4, Rgt(F) = 0.0439, wRref(F2) = 0.0960, T = 173(2) K. [ABSTRACT FROM AUTHOR]

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C32H48CoMo2N16O7, triclinic, P 1 ‾ (no. 2), a = 10.425(2) Å, b = 10.517(2) Å, c = 11.187(2) Å, α = 94.671(7)°, β = 112.270(6)°, γ = 104.108(7)°, V = 1080.0(3) Å3, Z = 1, Rgt(F) = 0.0407, wRref(F2) = 0.1015, T = 273 K. [ABSTRACT FROM AUTHOR]

C24H36N6O28V10, monoclinic, P21/c (no. 14), a = 10.4869(6) Å, b = 11.5123(7) Å, c = 17.4627(9) Å, β = 108.459(3)°, V = 1999.8(2) Å3, Z = 2, Rgt(F) = 0.0209, wRref(F2) = 0.0582, T = 296 K. [ABSTRACT FROM AUTHOR]

C20H16Li5NO13, orthorhombic, Pnma (no. 62), a = 9.9218(8) Å, b = 14.6941(11) Å, c = 13.5697(10) Å, V = 1978.4(3) Å3, Z = 4, Rgt(F) = 0.0439, wRref(F2) = 0.0960, T = 173(2) K. [ABSTRACT FROM AUTHOR]

C9H4Na2O6, monoclinic, C2/c (no. 15), a = 14.6828(15) Å, b = 9.8602(10) Å, c = 6.5024(7) Å, β = 101.360(4)°, V = 922.94(17) Å3, Z = 4, Rgt(F) = 0.0337, wRref(F2) = 0.0775, T = 173(2) K. [ABSTRACT FROM AUTHOR]

Abstract: Two novel metal–organic coordination complexes [Cu(HBTC)(BPO)]·H2O (1) and [Co3(BTC)2(BPO)3(H2O)2]·5.25H2O (2), have been synthesized from hydrothermal reaction of metal chloride with the mixed ligands 1,3,5-benzenetricarboxylate (H3BTC) and bent dipyridyl based ligand 2,5-bis(3-pyridyl)-1,3,4-oxadiazole (BPO), and structurally characterized by elemental analyses, IR, TG and single-crystal X-ray diffraction analysis. The results reveal that each dinuclear CuII unit is bridged by two kinds of different ligands (H3BTC and BPO) to form one-dimensional (1-D) chain structure in complex 1. The adjacent chains for 1 are further linked by π–π stacking interactions and hydrogen bonding interactions to form a three-dimensional (3-D) supramolecular framework. Complex 2 possesses a 3-D network composed of three different cobalt(II) centers [carboxylate-bridged dinuclear cobalt units and mononuclear cobalt ion] and bridging ligands BTC and BPO, which presents the first example of 3-D coordination polymer constructed from the BPO ligands simultaneously showing three different coordination modes. Moreover, the electrochemical behaviors of the two complexes bulk-modified carbon paste electrodes (1-CPE and 2-CPE) have been reported. [Copyright &y& Elsevier]

Abstract: Three novel metal–organic frameworks [M(1,3-BDC)(Dpdq)(H2O) m ]· nH2O, (M=CoII (1), CdII (2) or ZnII (3); m =0, 1; n =0, 1, 2, respectively) have been obtained from hydrothermal reactions of three different metal(II) nitrates with the same mixed ligands [isophthalic acid (1,3-BDC) and 2,3-di-2-pyridylquinoxaline (Dpdq)], and structurally characterized by elemental analyses, IR spectroscopy, and single-crystal X-ray diffraction analyses. Single-crystal X-ray analyses show that each pair of metal ions are bridged by various coordination modes of 1,3-BDC ligands to form left- and right-handed helical chains in 1, linear chains in 2, and double chains in 3, respectively. N-containing flexible ligand Dpdq takes a chelating coordination mode acting as terminal ligand. In the compound 1, adjacent left- and right-handed helical chains are packed through hydrogen bonds to form a two-dimensional (2-D) structure. In the compounds 2 and 3, adjacent chains are further linked by hydrogen bonds and/or π–π stacking interactions to form a three-dimensional (3-D) distorted hexagon meshes supramolecular framework for 2 and a ZnS-related three-dimensional (3-D) topology for 3, respectively. The different structures of compounds 1–3 illustrate that the influence of the metal ions in the self-assembly of polymeric coordination architectures. In addition, compounds 2 and 3 exhibit blue emission in the solid state at room temperature. [Copyright &y& Elsevier]

Two thiacalix[4]arene-protected silver(I) alkynyl nanoclusters, [Na 2 (H 2 O) 2 ][Ag 9 (TC4A)( t BuCC) 4 (CH 3 OH) 2 (SbF 6 ) 0.5 (OH) 2.5 ]·3.5H 2 O·CH 3 OH (1, abbreviated as Ag9) and [Ag 9 (TC4A)( t BuCC) 4 (CF 3 COO)] 2 ·4CH 3 OH (2, abbreviated as Ag18), were synthesized by the reaction of [ t BuCCAg] n , p-tert -butylthiacalix[4]arene (H 4 TC4A), NaBH 4 , and AgSbF 6 or CF 3 COOAg in the mixed solvent of methanol-trichloromethane-toluene under solvothermal conditions, respectively. Driven by SbF 6 - and CF 3 COO - with different coordination properties, the structural unit [Ag 9 (TC4A)( t BuCC) 4 ] + in both the compounds migrated in different modes, accompanied by distinct Ag⋯Ag distances. Ag9 and Ag18 exhibit similar UV-Vis absorption and diffuse reflection spectra along with contrary tendency between photocurrent responses and solid-state fluorescence. The solution stability of Ag9 and Ag18 was demonstrated by 1 H NMR and MALDI-TOF mass spectrometry. The fluorescence responses of Ag9 and Ag18 towards different organic molecules were also investigated, which indicated that the polarity of solvent has a certain effect on the emission intensities of Ag9 and Ag18. This study provides a positive guide for the controlled synthesis and further study of the structure-activity relationship of thiacalix[4]arene-protected silver alkynyl nanoclusters.

Structural transformation is important for the study of silver cluster compounds, in which controlled synthesis of their shapes and sizes via anion template-driven is one key scientific question. In this work, the CO 3 2- anion templates were captured by the [ t BuC≡CAg] n system under the stimulation induced by carboxylate ligand CF 3 COO - /PhCOO - , and two silver alkynyl clusters [(CO 3 2- )@Ag 21 ( t BuC≡C) 16 (CF 3 COO) 3 (H 2 O)]⋅DMF⋅2CH 2 Cl 2 (1) and [(CO 3 2- ) 2 @Ag 24 ( t BuC≡C) 16 (PhCOO) 4 ]⋅CH 3 OH⋅4DMF (2) have been successfully isolated and charactered. With the increase of the number of CO 3 2- templates from single to double, the outer silver atoms from twenty-one to twenty-four, accompanied by the growth of the cluster skeleton from 9.8 Å ×6.9 Å of the (CO 3 2- )@Ag 21 unit to 10.5 Å ×7.3 Å of the (CO 3 2- ) 2 @Ag 24 unit. In addition, the syntheses, structures, photocurrent responses, cyclic voltammetry characteristics, luminescence, and photodegradation of compounds 1 and 2 have been studied., (© 2023 Wiley-VCH GmbH.)