A novel and efficient method for functionalizing organosulfones has been established, utilizing a visible-light-driven intermolecular radical cascade cyclization of -allyl--ketosulfones. This process employs -Ir(ppy) as the photoredox catalyst and -carbonyl alkyl bromide as the oxidizing agent. Via this approach, the substrates experience intermolecular addition of -carbonyl alkyl radicals to the alkene bonds, initiating a sequence of C-C bond formations that culminate in the production of organosulfone derivatives.
View Article and Find Full Text PDFThe visible-light-promoted difunctionalization of alkenyl ketones has been developed for easy access of various tetralones, cyclopropane, or alkenyl migration compounds. With -[Ir(ppy)] as the photocatalyst, alkenyl ketones captured the α-carbonyl alkyl radical and evolved through intramolecular cyclization and the elimination of a proton to give the difunctionalized products. This strategy is characterized by good yields, mild reaction conditions, and outstanding functional group tolerance.
View Article and Find Full Text PDFThe active sites of [FeFe]-hydrogenase promoted by Fe/E (E = S, Se) clusters have attracted considerable interest due to their significance in understanding the interconversion of hydrogen with protons and electrons. As an extension of the study on Fe/Se clusters related to H-cluster model compounds of [FeFe]-hydrogenase, a series of tertiary phosphine substituted Fe/Se carbonyls were successfully prepared. The treatment of Fe(μ-SePh)(CO) (A) and excess PR resulted in the ferrous bis(selenolate) carbonyls Fe(SePh)(CO)(PR) (PR = PPhMe, 1; PMe, 2) in moderate yields.
View Article and Find Full Text PDFThe wide prevalence of organic and inorganic pollutants in water from various industries is responsible for serious environmental problems and endangers human beings. Therefore, the search for effective methods to detect these pollutants has gained great importance. In this work, a new luminescent MOF, {[Zn(L)(bpe)]·DMF} (1) [HL = 4,4'-((naphthalene-1,4-dicarbonyl)bis(azanediyl))dibenzoic acid, bpe = 1,2-bis(4-pyridyl)ethene], was solvothermally synthesized and structurally characterized.
View Article and Find Full Text PDFSix novel organotin phosphonate complexes, [(MeSn)(HL)]1, [(MeSn)(HL)]2, [(MeSn)L(HO)]3, [(PhSn)(HL)]4, [(PhSn)L]5 and [(PhSn)L]6, derived from phosphonic acid ligands [NaHL = 1-CHOPO(OH)Na, HL = 1-CHPO(OH), HL = 2-CHPO(OH)], have been synthesized and characterized by elemental analysis, FT-IR, NMR (H, C, P and Sn) spectroscopy and X-ray crystallography. The structural analysis reveals that complexes 1 and 5 display 1D infinite zig-zag chain structures, and complex 2 shows 1D right-handed helical chain structure, while complex 3 displays 1D left-handed helical chain structure. Complexes 4 and 6 are 24-membered macrocyclic rings interconnected by P, O and Sn atoms.
View Article and Find Full Text PDFA novel macrocyclic zirconocene(iv) aromatic selenite [(CpZr)L]·2(CpZr(μ-O)Cl) (complex 1) (Cp = cyclopentadienyl anion; L = 4-fluorobenzeneseleninic acid) was prepared by the reaction of bis(cyclopentadienyl)zirconium dichloride with 4-fluorobenzeneseleninic acid and characterized by elemental analysis, infrared spectroscopy, H, C NMR spectroscopy, ESI-MS, XRD and X-ray diffraction. The structure analysis shows that complex 1 is a centrosymmetric 32-membered macrocycle containing an eight-nuclear zirconocene. In this complex, the 4-fluorobenzeneseleninic acid ligands adopt bidentate mode in coordinating to zirconium, which play a bridging role in the formation of a macrocycle.
View Article and Find Full Text PDFWith the 2-thienylselenoacetic acid ligand, four new organotin complexes, [Me3Sn(O2CCH2SeC4H3S-o)]n (), [(Ph3Sn)6(O2CCH2SeC4H3S-o)6] (), [(Me2Sn)4(μ3-O)2(O2CCH2SeC4H3S-o)4] (), and [(PhSn)6(μ3-O)6(O2CCH2SeC4H3S-o)6] (), have been synthesized and characterized by X-ray crystallography, elemental analysis, FT-IR and NMR ((1)H, (13)C, and (119)Sn) spectroscopy. The structure analysis indicates that complex adopts a 1D infinite zig-zag chain structure, while complex shows a centrosymmetric hexanuclear 24-membered macrocycle. In contrast, complex and complex display ladder and drum structures, respectively.
View Article and Find Full Text PDFA new arenetelluronic triorganotin ester, namely (Me3Sn)4[o-Me-PhTe(μ-O)(OH)O2)]2 (1) has been prepared by the reaction of o-tolyltelluronic acid and Me3SnCl in the presence of potassium hydroxide. The complex was fully characterized by elemental analysis, FT-IR, NMR ((1)H, (13)C, (119)Sn) spectroscopy and X-ray crystallography. Structure analysis revealed that the complex crystallized as Sn4Te2 units and a 1D linear chain was formed by intermolecular C-HO interactions.
View Article and Find Full Text PDFActa Crystallogr Sect E Struct Rep Online
December 2011
In the title polymeric coordination compound, [Sn(CH(3))(3)(C(6)H(5)O(2)S)](n), which contains two formula units in the asymmetric unit, the Sn(IV) atom has a distorted trigonal-bipyramidal geometry, with two O atoms of the ligands in axial positions and three methyl groups in equatorial positions. Adjacent Sn(IV) atoms are bridged by the ligands, thereby forming a chain propagating in [010].
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December 2011
In the polymeric title coordination compound, [Sn(C(6)H(5))(3)(C(7)H(7)O(2)Se)](n), the Sn(IV) atom has a distorted trigonal-bipyramidal geometry, with two O atoms from two symmetry-related bridging seleninate ligands in axial positions and three phenyl groups in the equatorial plane. In the crystal, the complex exhibits a zigzag chain structure running parallel to the c axis. An intra-chain C-H⋯O hydrogen bond is observed.
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December 2011
In the title polymeric coordination compound, [Sn(CH(3))(2)(C(2)H(2)ClO(2))Cl](n), the Sn atom has a distorted trigonal-bipyramidal geometry, with two O atoms of the ligands in axial positions and two methyl groups and one Cl atom in equatorial positions. Adjacent Sn atoms are bridged by the two O atoms of the carboxylate ligand, forming a chain structure along the a-axis direction.
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January 2011
In the title polymeric coordination compound, [Sn(CH(3))(3)(C(6)H(5)O(2)Se)](n), the Sn(IV) atom has a distorted trigonal-bipyramidal geometry, with two O atoms of two symmetry-related bridging phenyl-seleninate anions in axial positions and three methyl groups in equatorial positions. In the crystal, the complex exhibits a chain structure parallel to the b axis.
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November 2010
In the title polymeric coordination compound, [Sn(CH(3))(3)(C(10)H(11)O(2))](n), the Sn atom has a distorted trigonal-bipyramidal coordination geometry, with two O atoms of two symmetry-related carboxyl-ate ligands in axial positions and three methyl groups in equatorial positions. In the crystal structure, carboxyl-ate bridges link the metal atoms, forming zigzag chains parallel to the b axis.
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August 2010
The asymmetric unit of the title complex, [Sn(CH(3))(2)(C(6)H(7)N(2)S)(2)], contains two independent mol-ecules with similar configurations. In each, the Sn(IV) cation is coordinated by two methyl and two 4,6-dimethyl-pyrimidine-2-thiol-ate anions in a distorted SnS(2)C(2) tetra-hedral geometry. In the two mol-ecules, the S-Sn-S bond angles are 87.
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January 2010
In the title compound, [Sn(2)(C(6)H(5))(6)(C(4)H(8)O(2)S(2))], the geometry around the Sn atoms is distorted tetra-hedral. The hydr-oxy groups are involved in O-H⋯O hydrogen bonding, which connects mol-ecules into centrosymmetric dimers.
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February 2009
In the title compound, C(20)H(24)N(2)O(4), the mol-ecule lies on a centre of symmetry and is approximately planar (r.m.s.
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February 2009
The title complex, [Sn(CH(3))(2)(C(8)H(10)O(4))](n), was synthesized from cis-cyclo-hexane-1,2-dicarboxylic acid and dimethyl-tin dichloride. The complex has a bridging bis-bidentate carboxyl-ate group resulting in a zig-zag chain structure parallel to [001]. The Sn atom is six-coordinated and displays a distorted octa-hedral geometry.
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December 2009
The title compound, [Sn(CH(3))(3)(C(7)H(9)O(2))](n), forms an extended zigzag chain structure propagating parallel to [010]. The Sn atom is in a slightly distorted trigonal-bipyramidal coordination environment with two carboxyl-ate O atoms in the axial and the three methyl groups in equatorial sites. The cyclo-hexene ring has a distorted half-boat conformation.
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December 2009
In the title polymeric coordination compound, [Sn(CH(3))(3)(C(20)H(12)O(4)P)](n), the Sn atom exhibits a distorted trigonal-bipyramidal coordination geometry with the phosphate O atoms of the 1,1'-binaphthyl-2,2'-diyl phospho-nate ligands in axial positions and equatorial sites occupied by the three methyl groups. Adjacent Sn atoms are bridged by coordination to the two O atoms of each 1,1'-binaphthyl-2,2'-diyl phospho-nate ligand, forming a one-dimensional chain structure parallel to the b axis.
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December 2009
The crystal structure of the title compound, [Na(C(3)H(3)N(2)S(3))(H(2)O)(2)](n), features polymeric chains made up of O⋯O edge-shared NaSN(H(2)O)(4) units running along the b axis. The Na(+) ion and all non-H atoms of the thia-diazole ligand lie on a mirror plane.
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August 2009
In the title compound, [Sn(CH(3))(2)(C(3)H(3)N(2)S(3))(2)], the Sn(IV) atom is coordinated within a C(2)N(2)S(2) donor set that defines a skew-trapezoidal bipyramidal geometry in which the methyl groups lie over the weakly coordinated N atoms. Two independent mol-ecules comprise the asymmetric unit, each of which lies on a mirror plane that passes through the C(2)Sn unit.
View Article and Find Full Text PDFThe reaction of 1-(4-carboxyphenyl)-5-mercapto-1 H-tetrazole with trimethyltin chloride in the presence of sodium ethoxide in benzene affords a novel 2D organotin network structure complex 1, which is an unusual organotin network containing a hexanuclear 60-membered organotin macrocycle. The complex has been characterized by elemental analysis, IR, and (1)H, (13)C, and (119)Sn NMR spectroscopy. Furthermore, we have also characterized the complex by X-ray crystallography.
View Article and Find Full Text PDFFour novel organotin complexes of two types--[R2Sn(o-SC6H4CO2)]6 (R = Me, 1 x H2O; nBu, 2) and {[R2Sn(m-CO2C6H4S)R2Sn(m-SC6H4CO2)SnR2]O}2 (R = Me, 3; nBu, 4)--have been prepared by treatment of o- or m-mercaptobenzoic acid and the corresponding R2SnCl2 (R = Me, nBu) with sodium ethoxide in ethanol (95%). All the complexes were characterized by elemental analysis, FT-IR and NMR (1H, (3C, 119Sn) spectroscopy, TGA, and X-ray crystallography diffraction analysis. The molecular structure analyses reveal that both 1 and 2 are hexanuclear macrocycles with hydrophobic "pseudo-cage" structures, while 3 and 4 are hexanuclear macrocycles with double-cavity structures.
View Article and Find Full Text PDFA series of diorganotin(IV) compounds of the type [R(2)Sn(pca)Cl](3)(R = CH(3); (n)Bu; C(6)H(5); C(6)H(5)CH(2); Hpca = 2-pyrazinecarboxylic acid), R(2)Sn(pca)(2)(mH(2)O)xnH(2)O (m= 1: R = CH(3), n= 2, R =(n)Bu, n= 0; m= 0, n= 0: R =(n)Bu, C(6)H(5), C(6)H(5)CH(2)) and (Et(3)NH)(+)[R(2)Sn(pca)(2)Cl](-)xmH(2)O (m= 0: R = CH(3), (n)Bu, C(6)H(5)CH(2); m= 1: R = C(6)H(5)) have been obtained by reactions of 2-pyrazinecarboxylic acid with diorganotin(iv) dichloride in the presence of sodium ethoxide or triethylamine. All compounds were characterized by elemental, IR and NMR spectra analyses. Except for compounds, and, the others were also characterized by X-ray crystallography diffraction analyses, which revealed that compounds and were trinuclear macrocyclic structures with six-coordinate tin(IV) atoms, compounds and were monomeric structures with seven-coordinate tin(IV) atoms, compounds and were polymeric chain structures with seven-coordinate tin(IV) atoms and compounds and were stannate with seven-coordinate tin(IV) atoms.
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