Structure du trihydrogéno hydroxy-1 ethanedi(phosphonate)-1,1 de rubidium dihydrate

Charpin, P.; Lance, M.; Nierlich, M.; Vigner, D.; Lee, M.-R.; Silvestre, J.-P.; Dao, Nguyen Quy

doi:10.1107/s0108270188001283

Cited by 11 publications

(15 citation statements)

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“…Both phases were characterised by single crystal structure determination with the phase I structure isomorphous with that of the K complex 1b, whereas the phase II structure is isomorphous with that of 3b. The calculated PXRD pattern for 2b (phase I) matched that obtained for the bulk isolated product, suggesting that the latter is pure phase I, and this was confirmed by the solid state 31 The reactions of alendronic acid with the group 1 metal hydroxide salts, MOH were also performed with a 1:2 acid to metal ratio to yield complexes of the form M 2 (LH 3 ).n(H 2 O) (M = Na 6, K 7, Rb 8, Cs 9). The final pH of the solutions prior to precipitation of the products was between 9-10 consistent with the presence of LH 3 2-.…”

Section: Resultssupporting

confidence: 78%

“…A complex series of absorption bands between 1250-750 cm -1 was also observed in all the spectra, and these are in the typical region for P-O stretching vibrations. 22 The current M(LH 4 ), M(LH 4 )(LH 5 ) and M 2 (LH 3 ) complexes were also analysed by solid state 31 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 13 K + cations, and the metal-ligand connectivity is shown in Figure S5 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 14 long...…”

Section: Resultsmentioning

confidence: 99%

“…However, analysis of the M–O bond distances shows two additional longer interactions in the 3.4–3.6 Å range for each complex, as indicated in Figure S5.2. Comparable data for group 1 metal phosphonate complexes that possess similar lamella topographies, [M(HO 3 P-R-PO 3 H 2 )] R = CH 2 CH 2 , C 6 H 4 C 6 H 4 , [Rb(HEDP)]·2(H 2 O) (HEDP = MeC(OH)(PO 3 H) 2 ) show metal–oxygen bond distances typically <3.1 Å for M = K, <3.3 Å for M = Rb and <3.5 Å for M = Cs. These suggest that significantly longer M–O distances are beyond the limit to be considered as primary coordination bonds and are more akin to weaker interactions such as metal-π-arene (K···C ca.…”

Section: Description Of Crystal Structuresmentioning

confidence: 99%

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Coordination Polymers of Increasing Complexity Derived from Alkali Metal Cations and (4-Amino-1-hydroxybutylidine)-1,1-bisphosphonic Acid (Alendronic Acid): The Competitive Influences of Coordination and Supramolecular Interactions

Deacon

Forsyth

Greenhill

et al. 2015

Crystal Growth & Design

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Reactions of (4-amino-1-hydroxybutylidine)-1,1-bisphosphonic acid (alendronic acid = LH 5 ) with one equivalent of the group 1 metal bases KOH, KHCO 3 , Rb 2 CO 3 , RbOH or Cs 2 CO 3 in aqueous solution at pH 4-5 gave the corresponding complexes [M(LH 4 )(H 2 O) n ].m(H 2 O), M = K (1), Rb (2) or Cs (3). Crystallisation of the products under varying conditions yielded differing hydrates and/or polymorphic phases. Rapid crystallisation of the potassium complex 1 from water/EtOH or water/DMSO gave 2[K(LH 4 )].3(H 2 O) (1a) whereas slow crystallisation from water or water/DMSO gave [K 2 (LH 4 ) 2 (H 2 O) 2 ].2H 2 O (1b phase I). For the rubidium complex 2, rapid crystallisation from water/EtOH gave the analogous [Rb 2 (LH 4 ) 2 (H 2 O) 2 ].2H 2 O (2b phase I) whereas slow crystallisation from water/DMSO also gave 2b, but as a mixture of phase I and the structural polymorph [Rb(LH 4 )(H 2 O)].H 2 O (2b phase II). In contrast, only [Cs(LH 4 )(H 2 O)].H 2 O (3b phase II) was obtained for the caesium complex 3 under all crystallisation conditions. A second complex type [M(LH 4 )(LH 5 )].2H 2 O (M = Rb 4, Cs 5), incorporating an additional coordinated alendronic acid molecule was also observed for the larger metals Rb and Cs as a minor product in some syntheses and isolated by fractional crystallisation for 4, but as the sole product from Cs(O 2 CH) and LH 5 for 5. The crystal structures of the complexes [M(LH 4 )(H 2 O) n ].m(H 2 O) 1a, 2b (phase II) and 3b (phase II) comprise edge-shared or corner-shared polyhedral chains that are linked by bridging bisphosphonate ligands into 2-D sheets. The 4-ammoniobutylidene chains protrude above and below the coordination layers and interact with neighbouring layers through hydrogen bonding of the terminal ammonium group forming distinctive supramolecular 3-D arrays. The phase I structure of 1b and 2b comprises ribbons of parallel M 4 (LH 4 ) 4 (H 2 O) 4 subunits arranged in a more close packed 3-D supramolecular network. For [M(LH 4 )(LH 5 )].2H 2 O (M = Rb 4, Cs 5), isolated M + cations, bridged by bisphosphonate ligands, are arranged into 2-D sheets, with the pendant 4-ammoniumbutylidene chains resulting in a 3-D lamellar network similar to those of 1a and 2b/3b (phase II). All of the [M(LH 4 )(H 2 O) n ].m(H 2 O) and [M(LH 4 )(LH 5 )].2H 2 O structures display strong PO-H…O(phosphonate) and N-H…O(phosphonate/water) hydrogen bond motifs which significantly impact upon the observed structures. Reactions of LH 5 with two equivalents of the group 1 metal bases MOH (M = Na, K, Rb, Cs) at pH 9-10 gave the di-metallated complexes [M 2 (LH 3 )(H 2 O) n ].(H 2 O) m (M = Na 6, K 7, Rb 8, Cs 9). Crystallisation of 6 from water/MeOH gave [Na 2 (LH 3 )(H 2 O) 4 ].H 2 O (6a) as a single phase. For 7, crystallisation from water/MeOH gave K 2 (LH 3 ).3(H 2 O) (7a) as the bulk product, whereas crystals of [K 2 (LH 3 )(H 2 O) 6 ] (7b) were grown from water/DMSO solutions. On standing, the crystals of 7b were converted into the bulk product 7a. The structures of 6a and 7b are chain rather than ...

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Section: Resultssupporting

confidence: 78%

Section: Resultsmentioning

confidence: 99%

Section: Description Of Crystal Structuresmentioning

confidence: 99%

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Coordination Polymers of Increasing Complexity Derived from Alkali Metal Cations and (4-Amino-1-hydroxybutylidine)-1,1-bisphosphonic Acid (Alendronic Acid): The Competitive Influences of Coordination and Supramolecular Interactions

Deacon

Forsyth

Greenhill

et al. 2015

Crystal Growth & Design

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“…À0.14285 (15) 0.33417 (9) 0.03903 (8) 1.77 (4) O36 0.80666 (14) À0.03021 (8) 0.42657 (8) 1.75 (4) O37 0.57666 (14) 0.17496 (9) 0.21222 (7) 1.65 (4) O38 0.44310 (16) 0.21072 (9) 0.43131 (8) 2.13 (4) O39 0.39704 (21) 0.34144 (9) 0.00070 (9) 3.14 (5) O40…”

Section: Article In Pressunclassified

Chemistry of organophosphonate scale growth inhibitors: two-dimensional, layered polymeric networks in the structure of tetrasodium 2-hydroxyethyl-amino-bis(methylenephosphonate)

Demadis¹,

Baran²

2004

Journal of Solid State Chemistry

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“…Ca-O(PO 3) bond lengths are 2.352(4) and 2.420(3) Å, whereas the Ca-O(H) bond is much longer, at 2.608(3) Å In a similar Rb-HEDP complex Rb-O(PO 3 ) bond lengths are 2.949(3) Å and 2.952(3) Å whereas the Rb-O(H) bond is much longer, at 3.078(3) Å. 29 Nardelli et al described the crystal structure of calcium dichloro-methylene diphosphonate. 25 Phosphonate groups are monodeprotonated, and there is extensive hydrogen bonding.…”

Section: Crystal and Molecular Structure Of A Ca-amp Complex A Bettementioning

confidence: 99%

Rational Development of New Cooling Water Chemical Treatment Programs for Scale and Microbial Control

Demadis

Yang

Young

et al.

Advances in Crystal Growth Inhibition Technologies

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Structure du trihydrogéno hydroxy-1 ethanedi(phosphonate)-1,1 de rubidium dihydrate

Cited by 11 publications

References 0 publications

Coordination Polymers of Increasing Complexity Derived from Alkali Metal Cations and (4-Amino-1-hydroxybutylidine)-1,1-bisphosphonic Acid (Alendronic Acid): The Competitive Influences of Coordination and Supramolecular Interactions

Coordination Polymers of Increasing Complexity Derived from Alkali Metal Cations and (4-Amino-1-hydroxybutylidine)-1,1-bisphosphonic Acid (Alendronic Acid): The Competitive Influences of Coordination and Supramolecular Interactions

Chemistry of organophosphonate scale growth inhibitors: two-dimensional, layered polymeric networks in the structure of tetrasodium 2-hydroxyethyl-amino-bis(methylenephosphonate)

Rational Development of New Cooling Water Chemical Treatment Programs for Scale and Microbial Control

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