14 research outputs found

    Syntheses and Structures of Mononuclear, Dinuclear and Polynuclear Silver(I) Complexes of 2‑Pyrazole-Substituted 1,10-Phenanthroline Ligands

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    A series of mononuclear, dinuclear and polynuclear silver­(I) complexes (<b>1</b>–<b>6</b>) bearing 2-pyrazole-substituted 1,10-phenanthroline derivatives (<b>L</b><sup><b>1</b></sup>, <sup><b>F</b></sup><b>L</b><sup><b>1</b></sup>, <b>L</b><sup><b>2</b></sup>) have been synthesized and characterized by <sup>1</sup>H and <sup>13</sup>C NMR, IR spectroscopy, elemental analysis, and single crystal X-ray diffraction. Reaction of <b>L</b><sup><b>1</b></sup> (<b>L</b><sup>1</sup> = 2-(3,5-dimethylpyrazol-1-yl)-1,10-phenanthroline) with AgClO<sub>4</sub> or AgBF<sub>4</sub> afforded two dinuclear silver­(I) complexes [Ag<sub>2</sub>(<b>L</b><sup><b>1</b></sup>)<sub>2</sub>(CH<sub>3</sub>CN)<sub>2</sub>]­(ClO<sub>4</sub>)<sub>2</sub> (<b>1</b>) and [Ag<sub>2</sub>(<b>L</b><sup><b>1</b></sup>)<sub>2</sub>(CH<sub>3</sub>CN)<sub>2</sub>]­(BF<sub>4</sub>)<sub>2</sub> (<b>2</b>), in which two [Ag<b>L</b><sup><b>1</b></sup>(CH<sub>3</sub>CN)]<sup>+</sup> units are linked by Ag···Ag interaction (Ag···Ag separation: 3.208(2) and 3.248(1) Å, respectively). A one-dimensional polymer {[Ag<b>L</b><sup><b>1</b></sup>]­(BF<sub>4</sub>)}<sub>∞</sub> (<b>3</b>) consisting of an infinite ···Ag···Ag···Ag··· chain (Ag···Ag separation: 3.059(1) Å), as well as a dinuclear complex [Ag<sub>2</sub>(ClO<sub>4</sub>)<sub>2</sub>(<b>L</b><sup><b>1</b></sup>)<sub>2</sub>] (<b>4</b>) in which the perchlorate anions instead of solvents are involved in the metal coordination, have also been obtained. The mononuclear complex [Ag­(<sup><b>F</b></sup><b>L</b><sup><b>1</b></sup>)<sub>2</sub>]­(BF<sub>4</sub>) (<b>5</b>) was synthesized from <sup><b>F</b></sup><b>L</b><sup><b>1</b></sup> (<sup><b>F</b></sup><b>L</b><sup><b>1</b></sup> = 2-(3,5-bis­(trifluoromethyl)­pyrazol-1-yl)-1,10-phenanthroline) and AgBF<sub>4</sub>, while the dinuclear [Ag<sub>2</sub>(BF<sub>4</sub>)<sub>2</sub>(<b>L</b><sup><b>2</b></sup>)<sub>2</sub>] (<b>6</b>) was isolated from <b>L</b><sup><b>2</b></sup> (<b>L</b><sup><b>2</b></sup> = 2-[<i>N</i>-(3-methyl-5-phenylpyrazole)]-1,10-phenanthroline). The photoluminescence properties of the ligands and complexes <b>1</b>–<b>6</b> have been studied both in the solid state and in solution

    Syntheses and Structures of Mononuclear, Dinuclear and Polynuclear Silver(I) Complexes of 2‑Pyrazole-Substituted 1,10-Phenanthroline Ligands

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    A series of mononuclear, dinuclear and polynuclear silver­(I) complexes (1–6) bearing 2-pyrazole-substituted 1,10-phenanthroline derivatives (L1, FL1, L2) have been synthesized and characterized by 1H and 13C NMR, IR spectroscopy, elemental analysis, and single crystal X-ray diffraction. Reaction of L1 (L1 = 2-(3,5-dimethylpyrazol-1-yl)-1,10-phenanthroline) with AgClO4 or AgBF4 afforded two dinuclear silver­(I) complexes [Ag2(L1)2(CH3CN)2]­(ClO4)2 (1) and [Ag2(L1)2(CH3CN)2]­(BF4)2 (2), in which two [AgL1(CH3CN)]+ units are linked by Ag···Ag interaction (Ag···Ag separation: 3.208(2) and 3.248(1) Å, respectively). A one-dimensional polymer {[AgL1]­(BF4)}∞ (3) consisting of an infinite ···Ag···Ag···Ag··· chain (Ag···Ag separation: 3.059(1) Å), as well as a dinuclear complex [Ag2(ClO4)2(L1)2] (4) in which the perchlorate anions instead of solvents are involved in the metal coordination, have also been obtained. The mononuclear complex [Ag­(FL1)2]­(BF4) (5) was synthesized from FL1 (FL1 = 2-(3,5-bis­(trifluoromethyl)­pyrazol-1-yl)-1,10-phenanthroline) and AgBF4, while the dinuclear [Ag2(BF4)2(L2)2] (6) was isolated from L2 (L2 = 2-[N-(3-methyl-5-phenylpyrazole)]-1,10-phenanthroline). The photoluminescence properties of the ligands and complexes 1–6 have been studied both in the solid state and in solution

    Homometallic Silver(I) Complexes of a Heterotopic NHC-Bridged Bis-Bipyridine Ligand

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    By varying the metal to ligand ratio, stepwise formation of a series of homonuclear silver­(I) complexes of a carbene-bridged bis-bipyridine ligand (L) was achieved. In the mononuclear 1:2 complex [AgL2]Br (1) only the carbene carbon is involved in the metal coordination, while both of the 2,2′-bipyridine (bpy) arms are free. When the amount of silver­(I) ion was increased, isomorphous 2:2 dinuclear complexes with different counteranions, [Ag2L2]­X2 (X = Br– (2a), PF6– (2b), BPh4– (2c)), were synthesized from the ligand LX, in which the carbene carbon and one of the bpy units participate in the coordination with silver­(I) ions. Further addition of AgI salt afforded the one-dimensional coordination polymer {[Ag3L2]­(PF6)3·4CH3CN}n (3), wherein the hanging bipyridine units also coordinate with AgI and thus all the coordination sites of the ligand are employed. The results reveal the preference of AgI ion for the carbene carbon donor rather than the bpy units. The synthesis, structures, and interconversion of the complexes and the counteranion effects on the structures are reported, and the luminescent properties of the ligand LX and the silver complexes have also been studied

    Homometallic Silver(I) Complexes of a Heterotopic NHC-Bridged Bis-Bipyridine Ligand

    No full text
    By varying the metal to ligand ratio, stepwise formation of a series of homonuclear silver­(I) complexes of a carbene-bridged bis-bipyridine ligand (L) was achieved. In the mononuclear 1:2 complex [AgL<sub>2</sub>]Br (<b>1</b>) only the carbene carbon is involved in the metal coordination, while both of the 2,2′-bipyridine (bpy) arms are free. When the amount of silver­(I) ion was increased, isomorphous 2:2 dinuclear complexes with different counteranions, [Ag<sub>2</sub>L<sub>2</sub>]­X<sub>2</sub> (X = Br<sup>–</sup> (<b>2a</b>), PF<sub>6</sub><sup>–</sup> (<b>2b</b>), BPh<sub>4</sub><sup>–</sup> (<b>2c</b>)), were synthesized from the ligand LX, in which the carbene carbon and one of the bpy units participate in the coordination with silver­(I) ions. Further addition of Ag<sup>I</sup> salt afforded the one-dimensional coordination polymer {[Ag<sub>3</sub>L<sub>2</sub>]­(PF<sub>6</sub>)<sub>3</sub>·4CH<sub>3</sub>CN}<sub><i>n</i></sub> (<b>3</b>), wherein the hanging bipyridine units also coordinate with Ag<sup>I</sup> and thus all the coordination sites of the ligand are employed. The results reveal the preference of Ag<sup>I</sup> ion for the carbene carbon donor rather than the bpy units. The synthesis, structures, and interconversion of the complexes and the counteranion effects on the structures are reported, and the luminescent properties of the ligand LX and the silver complexes have also been studied

    Tris Chelating Phosphate Complexes of Bis(thio)urea Ligands

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    Two bisurea (L1, L2) and one bisthiourea (L3) ligands were synthesized and their anion coordination behavior was studied. These ligands can readily form the tris chelates [PO4(L)3]3– (1, 5, and 6) with phosphate ion (PO43–) in the solid state, in which the anion is coordinated by six urea groups through 12 hydrogen bonds. Solution binding studies by 1H NMR and UV–vis spectroscopy revealed different binding properties of the ligands toward phosphate ion. While the bis­(p-nitrophenyl)-substituted bisurea L1 retains the 3:1 (host to guest) binding ratio in solution, the diethyl derivative L2 only forms 1:1 complex with phosphate ion. The more acidic thiourea L3 undergoes deprotonation/decomposition in the presence of phosphate ion. Moreover, the sulfate complex (2) of L1 and bicarbonate (3) and carbonate (4) complexes of L2 have also been obtained, which show lower coordination numbers both in the solid state and in solution

    Synthesis and Structure of a Zinc−Zinc-Bonded Compound with a Monoanionic α-Diimine Ligand, [LZn−ZnL] (L = [(2,6-<sup><i>i</i></sup>Pr<sub>2</sub>C<sub>6</sub>H<sub>3</sub>)NC(Me)]<sub>2</sub><sup>−</sup>)

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    A zinc−zinc-bonded compound with a monoanionic α-diimine ligand, [LZn−ZnL] (L = [(2,6-iPr2C6H3)NC(Me)]2−) (3), has been synthesized by the reaction of ZnCl2 and [Na2L]. The Zn−Zn bond distance (2.3403(18) Å) is shorter than that in the analogues with the dianionic ligand

    Synthesis and Structure of a Zinc−Zinc-Bonded Compound with a Monoanionic α-Diimine Ligand, [LZn−ZnL] (L = [(2,6-<sup><i>i</i></sup>Pr<sub>2</sub>C<sub>6</sub>H<sub>3</sub>)NC(Me)]<sub>2</sub><sup>−</sup>)

    No full text
    A zinc−zinc-bonded compound with a monoanionic α-diimine ligand, [LZn−ZnL] (L = [(2,6-iPr2C6H3)NC(Me)]2−) (3), has been synthesized by the reaction of ZnCl2 and [Na2L]. The Zn−Zn bond distance (2.3403(18) Å) is shorter than that in the analogues with the dianionic ligand

    Tris Chelating Phosphate Complexes of Bis(thio)urea Ligands

    No full text
    Two bisurea (L1, L2) and one bisthiourea (L3) ligands were synthesized and their anion coordination behavior was studied. These ligands can readily form the tris chelates [PO4(L)3]3– (1, 5, and 6) with phosphate ion (PO43–) in the solid state, in which the anion is coordinated by six urea groups through 12 hydrogen bonds. Solution binding studies by 1H NMR and UV–vis spectroscopy revealed different binding properties of the ligands toward phosphate ion. While the bis­(p-nitrophenyl)-substituted bisurea L1 retains the 3:1 (host to guest) binding ratio in solution, the diethyl derivative L2 only forms 1:1 complex with phosphate ion. The more acidic thiourea L3 undergoes deprotonation/decomposition in the presence of phosphate ion. Moreover, the sulfate complex (2) of L1 and bicarbonate (3) and carbonate (4) complexes of L2 have also been obtained, which show lower coordination numbers both in the solid state and in solution
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