Relatively Air‐Stable M(II) saccharinates, M = V, or Cr

Cotton, F. Albert; Libby, Eduardo; Murillo, Carlos A.; Valle, G.; Derringer, Daniel R.; Walton, Richard A.

doi:10.1002/9780470132586.ch59

Cited by 39 publications

(8 citation statements)

References 3 publications

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“…Although ApyH has possible sites for coordination to the metal ions, it remained outside the coordination sphere as a counter ion. Previous studies showed that all the aqua complexes of sac with first-row divalent transition metal ions consist of neutral [M(sac) 2 (H 2 O) 4 ] AE 2H 2 O complexes, containing only two coordinated sac ligands in the trans positions within the coordination sphere [6][7][8][9][10][11][12][13]. Furthermore, mixed-ligand sac complexes of transition metals prepared by us or other groups also contain one or two sac ligands, depending on steric hindrance of the co-ligands [17][18][19][20][21][22][23][24][25][26][27][28][29], and the presence of three sac ligands in the primary coordination sphere is unusual.…”

Section: Synthesismentioning

confidence: 99%

“…Although no metal complex of molecular saccharin is known, the corresponding deprotonated saccharinate anion [sac ¼ (C 7 H 4 NO 3 S) ) ] behaves as a versatile polyfunctional ligand and forms a number of complexes with different metal ions rather easily, due to the presence of the negatively charged imino nitrogen atom and the carbonyl and sulfonyl oxygen atoms. The first copper(II)-saccharinato complex, reported by Ahmed et al [6] in 1981, received considerable interest and gradually syntheses and X-ray structures of a series of tetraaquabis (saccharinato) metal(II) complexes with formula [M(sac) 2 (H 2 O) 4 ] AE 2H 2 O, where M II ¼ V [7,8], Cr [8,9], Mn [10], Fe [10][11][12], Co [10][11][12], Ni [10][11][12], Cu [6,11,12], Zn [9,10,12,13] and Cd [10,13], were reported. The structural analysis of these bis(saccharinato) complexes showed that all of them are isostructural, crystalizing in the monoclinic space group P2 1 /c, and all the metal(II) ions have octahedral geometry with four aqua ligands and two sac anions in trans positions.…”

Section: Introductionmentioning

confidence: 99%

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The first tris(saccharinato) complexes. Syntheses, spectral, thermal and structural characterization of ApyH[Cu(N?sac)2(O?sac)(H2O)2] and ApyH[Zn(N?sac)3- (H2O)] (ApyH=2?aminopyridinium and sac=saccharinate)

Yılmaz

Kazak

2005

Transition Met Chem

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The reaction of the Schiff base salicylideneaminopyridine with [M(sac) 2 (H 2 O) 4 ] AE 2H 2 O, where M is copper(II) or zinc(II), and sac is the saccharinate anion, results in the formation of the new tris(saccharinato) complexes ApyH[Cu(N-sac) 2 (O-sac)(H 2 O) 2 ] (1) and ApyH[Zn(N-sac) 3 (H 2 O)](2), which have been characterized by elemental analyses, magnetic measurements, FT-IR spectroscopy, thermal analysis and X-ray diffraction. The Schiff base did not coordinate to the metal ions, but decomposed during the reaction, forming a 2-aminopyridinium cation ApyH, which remained outside the coordination sphere as a counter ion. (1) and (2) are the first examples of mononuclear tris(saccharinato) complexes of copper(II) and zinc(II). Both complexes are isomorphous with the triclinic space group P-1, (1) consisting of an ApyH cation and a [Cu(sac) 3 (H 2 O) 2 ] ) anion in which the copper(II) ion has trigonal bipyramidal surroundings. The sac ligands in (1) exhibit unusual and non-equivalent coordination, behaving as ambidentate ligands. One of them coordinates to the metals through the carbonyl oxygen atom, while the other two sac ligands are bonded to the metals via the imino nitrogen atom. The zinc(II) ion in (2) is tetrahedrally coordinated by three N-donor sac ligands and an aqua ligand. The crystal structures of (1) and (2) are stabilized by intermolecular hydrogen bonds and aromatic p-p stacking interactions.

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Section: Synthesismentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

The first tris(saccharinato) complexes. Syntheses, spectral, thermal and structural characterization of ApyH[Cu(N?sac)2(O?sac)(H2O)2] and ApyH[Zn(N?sac)3- (H2O)] (ApyH=2?aminopyridinium and sac=saccharinate)

Yılmaz

Kazak

2005

Transition Met Chem

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“…Because of potential pathological effects, research has expanded to include mono-(imidazole, pyridine) or polycyclic N-donor ligand (2,2 0 -bipyridine, 1,10-phenanthroline) adducts. Several reports about mixed ligand complexes containing saccharinate and these N-donor ligands of various first-row transition metals such as V(II) [17,18], Cr(II) [19], Mn(II) [20][21][22], Fe(II) [23,24], Co(II) [20,25,26], Ni(II) [26][27][28], and Cu(II) [29][30][31][32][33][34][35][36] [29], and [Zn(sac)(bipy) 2 (H 2 O)]sac [40] were determined by single crystal X-ray. Zinc(II)-saccharinate can form a coordination polymer in the presence of a bridging ligand such as pyrazine, as it has been found in [Zn(sac) 2 (m-pyz)(H 2 O)] n [41].…”

Section: Introductionmentioning

confidence: 99%

Saccharin complexes of zinc(II) with phenanthroline and 2,9-dimethyl-1,10-phenanthroline: synthesis and characterization

Raad

Boghaei

Khavasi

2009

Journal of Coordination Chemistry

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The saccharinato complexes [Zn(phen) 2 (sac)(H 2 O)]sac (1) and [Zn(sac)(dmp)(H 2 O)](sac) (2), where phen ¼ 1,10-phenanthroline, dmp ¼ 2,9-dimethyl-1,10-phenanthroline, and sac ¼ saccharinato ion/ligand, were synthesized by the reaction of [Zn(sac) 2 (H 2 O) 4 ] Á 2H 2 O with ligands and have been characterized by elemental analysis, IR, and 1 H NMR spectroscopies. Conductivity of complexes was measured in DMSO. Compound 1 is characterized by single crystal X-ray diffraction and compared with some isomorphous zinc-saccharinate complexes reported previously. Complex 1 crystallizes in the triclinic system, space group P" 1, with Z ¼ 2, and consists of alternating slightly distorted octahedral [Zn(phen) 2 (sac)(H 2 O)] þ and noncoordinated saccharinate. The zinc bound aqua is hydrogen bonded to an oxygen of carbonyl in the saccharinate ligand and the SO 2 group in the saccharinate counter-ion from an adjacent molecule. Intermolecular and intramolecular hydrogen bonds and C-H Á Á Á O and C-H Á Á Á N short contacts lead to a 3-D network.

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“…Although no metal complexes of neutral, molecular saccharin are known, the corresponding deprotonated saccharinate anion [sac: (C 7 H 4 NO 3 S) − ] behaves as a versatile, polyfunctional, ligand due to the presence of the negatively charged imino nitrogen atom and the carbonyl and sulfonyl oxygen atoms and forms a number of complexes with different metal ions rather easily. The most common coordination mode of sac is ligation through the negatively charged nitrogen atom, typically observed in the aquabis(saccharinato) complexes of transition metals [1][2][3][4][5][6].…”

Section: Introductionmentioning

confidence: 99%

A Chiral Coordination Polymer of Silver(I) with Saccharinate and Pyridine: Synthesis, Spectral, Thermal, and Structural Characterization of [Ag(sac)(py)]n

2005

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The first silver(I) complex of saccharinate (sac) with pyridine (py), [Ag(sac)(py)] n has been synthesized and characterized by elemental analysis, IR spectroscopy and single crystal X-ray diffractometry. The complex crystallizes in chiral, trigonal space group P3 1 21 (No. 152) with unit cell parameters of a = 11.2605 (2)Å, c = 17.3300(4)Å, V = 1903.02(6)Å 3 and Z = 6. [Ag(sac)(py)] n contains monomeric [Ag(sac)(py)] units linked into infinite helices by way of Ag· · ·Ag interactions [d(Ag· · ·Ag) = 2.909(2) and 2.985(1)Å]. The distorted square-planar environment of Ag is completed by an N-bonded sac [Ag N = 2.084(2)Å] and a py molecule [Ag N = 2.116(2)Å].The N sac Ag N py angle is 173.85(10) • . The one-dimensional chains are crosslinked by C H· · ·O interactions involving the carbonyl and sulfonyl O atoms of sac and aromatic-ring hydrogen atoms of both sac and py. The thermal stability of the title complex was investigated using thermogravimetry and differential thermal analysis in a static atmosphere of air. The first decomposition stage between 90 and 160 • C corresponds to removal of the py molecule in a single stage, while the degradation of the sac moiety occurs at two stages in the temperature range 370-515 • C, giving an end product of metallic Ag.

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Relatively Air‐Stable M(II) saccharinates, M = V, or Cr

Cited by 39 publications

References 3 publications

The first tris(saccharinato) complexes. Syntheses, spectral, thermal and structural characterization of ApyH[Cu(N?sac)2(O?sac)(H2O)2] and ApyH[Zn(N?sac)3- (H2O)] (ApyH=2?aminopyridinium and sac=saccharinate)

The first tris(saccharinato) complexes. Syntheses, spectral, thermal and structural characterization of ApyH[Cu(N?sac)2(O?sac)(H2O)2] and ApyH[Zn(N?sac)3- (H2O)] (ApyH=2?aminopyridinium and sac=saccharinate)

Saccharin complexes of zinc(II) with phenanthroline and 2,9-dimethyl-1,10-phenanthroline: synthesis and characterization

A Chiral Coordination Polymer of Silver(I) with Saccharinate and Pyridine: Synthesis, Spectral, Thermal, and Structural Characterization of [Ag(sac)(py)]n

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