X-Ray crystallographic investigation of organic ligands of the complexone type.

Shkol'nikova, L. M.; Polyanchuk, G. V.; Zavodnik, V. E.; Rudomino, M. V.; Pisareva, S. A.; Dyatlova, N. M.; Zhadanov, B. V.; Polyakova, I. A.

doi:10.1007/bf00749555

Cited by 5 publications

(6 citation statements)

References 7 publications

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“…These chains are connected to each other in the b -axis direction by the organic chain of the ligand. This connectivity results in formation of layers (Figure ), which are similar to the layers defined by the chlorinated ligand: ethylenediaminediisopropylphosphonic acid dichloride 2 Representation of cadmium octahedra dimers sharing an edge through chloride ion bridging.…”

Section: Resultsmentioning

confidence: 95%

“…The range of PO stretching vibrations in the IR spectrum of H 4 L, prepared by us, supports the betaine structure. The spectrum exhibits three strong bands at 1156, 1029, and 939 cm -1 , assigned to ν as (PO 2 ), ν s (PO 2 ), and ν(P−OH), respectively, indicating clearly the presence of PO 3 H groups. ,, Furthermore, all the PO bands are low-frequency shifted due to the strong intra- and intermolecular hydrogen bonds with lattice water molecules and NH 2 + groups . The NH 2 + groups are expected to give two bands between 3000 and 2700 cm -1 , which are usually broad, unresolved, and extended to 2273 cm -1 .…”

Section: Resultsmentioning

confidence: 99%

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A Novel Cadmium Aminophosphonate: X-ray Powder Diffraction Structure, Solid-State IR and NMR Spectroscopic Determination of the Fine Structure of the Organic Moieties

et al. 2004

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A new divalent cadmium phosphonate, Cd2Cl2(H2O)4(H2L), has been synthesized from the ethylenediamine-N,N'-bis(methylenephosphonic acid) (H4L). The obtained microcrystalline compound has been characterized by solid-state IR spectra and 13C, 31P, and 113Cd CP MAS NMR. The static 13P NMR spectra have been also recorded to give the delta11, delta22, and delta33 chemical shift parameters for both compounds. The spectral data, collected for Cd2Cl2(H2O)4(H2L), are in an agreement with its X-ray powder diffraction structure solved with the cell dimensions a = 16.6105(10), b = 7.1572(4), and c = 6.8171(4) A and beta = 98.327(4) degrees. The octahedral coordination sphere of the cadmium atoms consists of two phosphonate oxygen atoms, two water oxygen atoms, and the two chlorine atoms. Cadmium atoms are bridged by the chlorine atoms forming four-membered rings. The phosphorus atoms exhibit a tetrahedral coordination with two oxygen atoms bonded to the cadmium atoms with P-O distances of 1.503(10) and 1.504(10) A. The third oxygen atom, showing a longer P-O distance (1.546(9) A), is not bonded to the metal center, nor is it bonded to a proton. The combined IR and NMR proton-phosphorus cross-polarization kinetic data together with the X-ray data confirm that the cadmium phosphonate has the zwitterionic structure (NH2(+)CH2P(O2Cd2)O-) similar to the initial aminophosphonic acid H4L.

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Section: Resultsmentioning

confidence: 95%

Section: Resultsmentioning

confidence: 99%

A Novel Cadmium Aminophosphonate: X-ray Powder Diffraction Structure, Solid-State IR and NMR Spectroscopic Determination of the Fine Structure of the Organic Moieties

et al. 2004

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“…Phosphonic acids containing one or two amine groups usually exist as Zwitter ions, as does H 4 PMIDA . Under acidic conditions, such acids do not act as chelating ligands; only the phosphonic group is coordinated to the metal ions, and carboxylic groups and nitrogen are only involved in hydrogen bonding.…”

Section: Discussionmentioning

confidence: 99%

Metal Carboxylate-Phosphonate Hybrid Layered Compounds: Synthesis and Single Crystal Structures of Novel Divalent Metal Complexes with N-(Phosphonomethyl)iminodiacetic Acid

2002

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Two novel divalent metal complexes with N-(phosphonomethyl)iminodiacetic acid, H(2)O(3)PCH(2)N(CH(2)CO(2)H)(2) (H(4)PMIDA), [Co(2)(PMIDA)(H(2)O)(5)] x H(2)O, 1, and [Zn(2)(PMIDA)(CH(3)CO(2)H)] x 2H(2)O, 2, have been synthesized and structurally characterized. The structure of complex 1 features two different kinds of Co(II) layers, namely, a cobalt phosphonate layer along the <100> plane and a cobalt carboxylate layer along the <300> plane. The Co(II) atoms in the phosphonate layer are octahedrally coordinated by 4 aqua ligands and 2 oxygen atoms from two phosphonic acid groups. Two Co(II) octahedra are bridged by a pair of phosphonic groups into a dimeric unit, and such dimers are interconnected into a layer through hydrogen bonding between aqua ligands. The Co(II) atoms in the carboxylate layer are octahedrally coordinated by a chelating PMIDA ligand, one aqua ligand, and one phosphonic oxygen atom from the neighboring PMIDA ligand. These Co(II) octahedra are interlinked by bridging carboxylic groups into a one-dimensional chain along the c-axis; such chains are held together by hydrogen bonds formed between carboxylic oxygen atoms and lattice water molecules, in such a way as to form a layer along the <300> direction. Two such layers are interconnected into a double layer via hydrogen bonding. These double layers are further interconnected with the Co(II) phosphonate layers through phosphonate tetrahedra along the a direction, resulting in the formation of a complicated three-dimensional network. The crystal structure of 2 contains a metal phosphonate and metal carboxylate hybrid layer along the <202> plane. One of the two zinc atoms in the asymmetric unit is tetrahedrally coordinated by four oxygen atoms from two phosphonic acid groups and two carboxylic groups; the other zinc atom is 5-coordinated by three oxygen atoms and a nitrogen atom from a chelating PMIDA ligand and one oxygen atom from the acetic acid. The above two types of zinc metal ions are interconnected by bridging carboxylic and phosphonic groups, resulting in the formation of a layered structure.

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“…23 The P-N-C(13) bond angle (122.3(1)Њ) is more obtuse than the P-C-C angle found in Ph 2 PCH 2 CO 2 Et (113.24Њ) 24 and Ph 2 PCH 2 CO 2 H (110.188Њ). 25…”

Section: Crystal Structures Of 1 and 12bmentioning

confidence: 99%

Coordination properties of novel hemilabile acetamide-derived P,O phosphine ligands. Crystal structures of Ph2PNHC(O)Me and [PdMe{PPh2NHC(O)Me}{PPh2NHC(O)Me}][O3SCF3] †

Braunstein

Frison

Morise

et al. 2000

J. Chem. Soc., Dalton Trans.

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Cationic methyl Pd() complexes are described in which the new heterofunctional phosphine ligands Ph 2 PNHC(O)Me 1 or Ph 2 PN(Me)C(O)Me 3 behave as rigid and/or hemilabile P,O chelates. The chelating ability of 3 is higher than that of 1 and both are compared to that of other P,O ligands, such as the keto-and amido-phosphines Ph 2 PCH 2 C(O)Ph and Ph 2 PCH 2 C(O)NPh 2 , respectively. The crystal structure of 1 reveals the presence in the solid-state of an intermolecular hydrogen-bonded network N-H ؒ ؒ ؒ O and that of12b establishes the presence of both a chelating and a monodentate ligand 1 in the same complex. Carbonylation of the cationic methyl complexes 8a, 17, 18a and 20a afforded the corresponding acetyl complexes in which this ligand occupies a position cis to phosphorus, irrespective of that of the alkyl ligand in the precursor complex.

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X-Ray crystallographic investigation of organic ligands of the complexone type.

Cited by 5 publications

References 7 publications

A Novel Cadmium Aminophosphonate: X-ray Powder Diffraction Structure, Solid-State IR and NMR Spectroscopic Determination of the Fine Structure of the Organic Moieties

A Novel Cadmium Aminophosphonate: X-ray Powder Diffraction Structure, Solid-State IR and NMR Spectroscopic Determination of the Fine Structure of the Organic Moieties

Metal Carboxylate-Phosphonate Hybrid Layered Compounds: Synthesis and Single Crystal Structures of Novel Divalent Metal Complexes with N-(Phosphonomethyl)iminodiacetic Acid

Coordination properties of novel hemilabile acetamide-derived P,O phosphine ligands. Crystal structures of Ph2PNHC(O)Me and [PdMe{PPh2NHC(O)Me}{PPh2NHC(O)Me}][O3SCF3] †

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