A gadolinium cryptate with two coordinated water molecules

AbstractIrinotecan inhibits cell proliferation and thus is used for the primary treatment of colorectal cancer. Metabolism of irinotecan involves incorporation of β-glucuronic acid to facilitate excretion. During transit of the glucuronidated product through the gastrointestinal tract, an induced upregulation of gut microbial β-glucuronidase (GUS) activity may cause severe diarrhea and thus force many patients to stop treatment. We herein report the development of uronic isofagomine (UIFG) derivatives that act as general, potent inhibitors of bacterial GUSs, especially those of Escherichia coli and Clostridium perfringens. The best inhibitor, C6-nonyl UIFG, is 23,300-fold more selective for E. coli GUS than for human GUS (Ki = 0.0045 and 105 μM, respectively). Structural evidence indicated that the loss of coordinated water molecules, with the consequent increase in entropy, contributes to the high affinity and selectivity for bacterial GUSs. The inhibitors also effectively reduced irinotecan-induced diarrhea in mice without damaging intestinal epithelial cells.

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Crystal structure of poly[diaquabis(μ5-benzene-1,3-dicarboxylato)(N,N-dimethylformamide)cadmium(II)disodium(I)]

Acta Crystallographica Section E Crystallographic Communications ◽

10.1107/s2056989017013871 ◽

2017 ◽

Vol 73 (11) ◽

pp. 1599-1602 ◽

Cited By ~ 1

Author(s):

Matimon Sangsawang ◽

Kittipong Chainok ◽

Nanthawat Wannarit

Keyword(s):

Crystal Structure ◽

Coordination Polymer ◽

Hydrogen Bonds ◽

Three Dimensional ◽

Water Molecules ◽

Asymmetric Unit ◽

Carboxylate Groups ◽

Benzene Rings ◽

Coordinated Water ◽

Coordinate Geometry

The title compound, [CdNa2(C8H4O4)2(C3H7NO)(H2O)2]nor [CdNa2(1,3-bdc)2(DMF)(H2O)2]n, is a new CdII–NaIheterobimetallic coordination polymer. The asymmetric unit consists of one CdIIatom, two NaIatoms, two 1,3-bdc ligands, two coordinated water molecules and one coordinated DMF molecule. The CdIIatom exhibits a seven-coordinate geometry, while the NaIatoms can be considered to be pentacoordinate. The metal ions and their symmetry-related equivalents are connectedviachelating–bridging carboxylate groups of the 1,3-bdc ligands to generate a three-dimensional framework. In the crystal, there are classical O—H...O hydrogen bonds involving the coordinated water molecules and the 1,3-bdc carboxylate groups and π–π stacking between the benzene rings of the 1,3-bdc ligands present within the frameworks.

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Crystal structure ofcatena-poly[[[tetraaquairon(II)]-trans-μ-1,2-bis(pyridin-4-yl)ethene-κ2N:N′] bis(p-toluenesulfonate) methanol disolvate]

Acta Crystallographica Section E Crystallographic Communications ◽

10.1107/s2056989017017054 ◽

2017 ◽

Vol 73 (12) ◽

pp. 1977-1980

Author(s):

Volodymyr M. Hiiuk ◽

Diana D. Barakhty ◽

Sergiu Shova ◽

Ruslan A. Polunin ◽

Il'ya A. Gural'skiy

Keyword(s):

Crystal Structure ◽

Hydrogen Bonds ◽

Three Dimensional ◽

Distorted Octahedral Geometry ◽

Water Molecules ◽

Supramolecular Network ◽

Polymeric Complex ◽

Distorted Octahedral ◽

Polymeric Chains ◽

Coordinated Water

In the title polymeric complex, {[Fe(C12H10N2)2(H2O)4](CH3C6H4SO3)2·2CH3OH}n, the FeIIcation, located on an inversion centre, is coordinated by four water molecules in the equatorial positions and two 1,2-bis(pyridin-4-yl)ethene molecules in the axial positions. This results in a distorted octahedral geometry for the [N2O4] coordination polyhedron. The 1,2-bis(pyridin-4-yl)ethene molecules bridge the FeIIcations, forming polymeric chains running along thea-axis direction. Stabilization of the crystal structure is provided by O—H...O hydrogen bonds; these are formed by coordinated water molecules as donors towards the O atoms of the methanol molecules and tosylate anions as acceptors of protons, leading to the formation of a three-dimensional supramolecular network. Weak C—H...O hydrogen bonds are also observed in the crystal.

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Crystal structure of a nickel compound comprising two nickel(II) complexes with different ligand environments: [Ni(tren)(H2O)2][Ni(H2O)6](SO4)2

Acta Crystallographica Section E Crystallographic Communications ◽

10.1107/s2056989020001358 ◽

2020 ◽

Vol 76 (3) ◽

pp. 314-317

Author(s):

Karilys González Nieves ◽

Dalice M. Piñero Cruz

Keyword(s):

Crystal Structure ◽

Title Compound ◽

Molar Ratio ◽

Water Molecules ◽

Nickel Compound ◽

Counter Anion ◽

Cationic Complex ◽

Coordinated Water ◽

Co Precipitation ◽

Metal Ligand

The title compound, diaqua[tris(2-aminoethyl)amine]nickel(II) hexaaquanickel(II) bis(sulfate), [Ni(C6H18N4)(H2O)2][Ni(H2O)6](SO4)2 or [Ni(tren)(H2O)2][Ni(H2O)6](SO4)2, consists of two octahedral nickel complexes within the same unit cell. These metal complexes are formed from the reaction of [Ni(H2O)6](SO4) and the ligand tris(2-aminoethyl)amine (tren). The crystals of the title compound are purple, different from those of the starting complex [Ni(H2O)6](SO4), which are turquoise. The reaction was performed both in a 1:1 and 1:2 metal–ligand molar ratio, always yielding the co-precipitation of the two types of crystals. The asymmetric unit of the title compound, which crystallizes in the space group Pnma, consists of two half NiII complexes and a sulfate counter-anion. The mononuclear cationic complex [Ni(tren)(H2O)2]2+ comprises an Ni ion, the tren ligand and two water molecules, while the mononuclear complex [Ni(H2O)6]2+ consists of another Ni ion surrounded by six coordinated water molecules. The [Ni(tren)(H2O)2] and [Ni(H2O)6] subunits are connected to the SO4 2− counter-anions through hydrogen bonding, thus consolidating the crystal structure.

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Synthesis, Single Crystal Structural Investigation, Hirshfeld Surface Analysis, Thermoanalysis and Spectroscopic Study of Two New Cu(II) and Co(II) Transition-Metal Complexes

Crystals ◽

10.3390/cryst11080986 ◽

2021 ◽

Vol 11 (8) ◽

pp. 986

Author(s):

Rim Boubakri ◽

Mirosław Szybowicz ◽

Mariola Sadej ◽

Sarra Soudani ◽

Frédéric Lefebvre ◽

...

Keyword(s):

Hydrogen Bonds ◽

Single Crystal ◽

Organic Ligand ◽

Free Water ◽

Pyrimidine Ring ◽

Water Molecules ◽

Absorption Bands ◽

Infrared And Raman Spectroscopy ◽

Homo And Lumo ◽

Coordinated Water

Two new complexes, [Cu(dimpyr)2(H2O)2](NO3)2.2H2O (1) and (Hamdimpy)2[CoCl4].H2O (2), with the monodentate ligand 2-amino-6-methylpyrimidin-4-(1H)-one (dimpyr) and the countercation 4-amino-2,6-dimetylpyrimidium (Hamdimpy), respectively, were prepared and characterized by single crystal X-ray diffraction, elemental analysis and IR spectroscopy. In (1), the Cu(II) cation is tetracoordinated, in a square plan fashion, by two nitrogen atoms from the pyrimidine ring of the organic ligand and two oxygen atoms of two coordinated water molecules. In the atomic arrangement, the CuO2N2 square planes are interconnected via the formation of O-H…O hydrogen bonds involving both coordinated and free water molecules and NO3− nitrate anions to form inorganic layers parallel to the (a, b) plane at z = (2n + 1)/4. In (2), the central atom Co(II) is four-coordinated in a distorted tetrahedral fashion by four Cl− ions. The [CoCl4]2− tetrahedra are arranged parallel to the plane (110) at x = (2n + 1)/2 and the organic cations are grafted between them by establishing with them hydrogen bonds of CH…Cl and NH…Cl types. The vibrational absorption bands were identified by infrared and Raman spectroscopy. Intermolecular interactions were investigated via Hirshfeld surfaces and electronic properties such as HOMO and LUMO energies were derived. The two compounds were characterized by thermal analysis to determine their thermal behavior with respect to temperature.

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Crystal structure of poly[[di-μ3-acetato-tetraaquabis(μ2-cyclohexane-1,4-dicarboxylato)dilanthanum(III)] dihydrate]

Acta Crystallographica Section E Crystallographic Communications ◽

10.1107/s2056989017016103 ◽

2017 ◽

Vol 73 (12) ◽

pp. 1926-1930

Author(s):

R. Drisya ◽

U. S. Soumya Mol ◽

P. R. Satheesh Chandran ◽

M. Sithambaresan ◽

M. R. Sudarsankumar

Keyword(s):

Crystal Structure ◽

Coordination Mode ◽

Three Dimensional ◽

Raw Material ◽

Water Molecules ◽

Supramolecular Network ◽

Formula Unit ◽

Remarkable Feature ◽

Two Component ◽

Coordinated Water

The title compound, {[La2(CH3COO)2(C8H10O4)2(H2O)4]·2H2O}nor [La2(ac)2(e,a-cis-1,4-chdc)2(H2O)4]·2H2O, whereacis acetate and 1,4-chdc is cyclohexane-1,4-dicarboxylate anion, is a binuclear lanthanum(III) complex. Each metal atom is decacoordinated by four O atoms from two distinct 1,4-chdc2−ligands, four O atoms from three acetate groups and two O atoms from coordinated water molecules to form a distorted bicapped square-antiprismatic geometry. Two non-coordinated water molecules are also present in the formula unit. The most remarkable feature of this compound is that it possesses a onlycisconformation for cyclohexane-1,4-dicarboxylic acid, although the raw material consists of a mixture ofcisandtransisomers. The μ3-η2:η2coordination mode of the bridging acetate group and the flexible dicarboxylate fragments of 1,4-chdc2−results in the formation of infinite two-dimensional lanthanide–carboxylate layers within the crystal structure. The directionality of strong intermolecular O—H...O and weak C—H...O interactions provides robustness to the layers, which leads to the construction of a three-dimensional supramolecular network. The crystal studied was refined as a two-component twin.

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Synthesis, crystal structure, and quantum mechanical studies regarding a new metal–organic complex based on Cd (II)

10.21203/rs.3.rs-735356/v1 ◽

2021 ◽

Author(s):

zohreh razmara ◽

Fereshteh Shiri ◽

Pouya Karimi ◽

Marek Necas

Keyword(s):

Three Dimensional ◽

Pentagonal Bipyramid ◽

Quantum Mechanical ◽

Water Molecules ◽

Organic Complex ◽

Polymeric Networks ◽

Metal Organic Complex ◽

Metal Organic ◽

Coordinated Water ◽

Mechanical Studies

Abstract A novel metal-organic complex formulated as [Cd (phen)(dipic) (H2O)2]. 3 H2O (phen = 1, 10-phenanthroline; dipic2−= pyridine-2,6-dicarboxylate) has been hydrothermally synthesized at 150°C for 48h. The structure of Cd complex was characterized by elemental analysis, Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), differential thermal analysis (DTA), and single-crystal X-ray diffraction (SC-XRD). The crystal system of Cd complex is monoclinic with space group C 2/c. The pentagonal bipyramid (seven coordinate) around Cd2+ center filled by two terminal water ligands, one 1,10-phenanthroline, and one pyridine-2,6-dicarboxylate anion. Extensive O–H···O hydrogen bonding interactions involving all coordinated water molecules, dipicolinate oxygens, and crystallization water molecules further stabilize the complex units by linking them to form three-dimensional polymeric networks. Indeed, quantum mechanical studies were performed to understand effective factors on stability of the Cd(II) complex.

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Double Palindrome Water Chain in Cu(II) Theophylline Complex. Synthesis, Characterization, Biological Activity of Cu(II), Zn(II) Complexes with Theophylline

Crystals ◽

10.3390/cryst10020097 ◽

2020 ◽

Vol 10 (2) ◽

pp. 97 ◽

Cited By ~ 1

Author(s):

Michał Gacki ◽

Karolina Kafarska ◽

Anna Pietrzak ◽

Izabela Korona-Głowniak ◽

Wojciech M. Wolf

Keyword(s):

Crystal Packing ◽

Radical Scavenging ◽

Absorption Spectrometry ◽

Water Molecules ◽

X Ray Diffraction ◽

Flame Atomic Absorption ◽

Hirshfeld Surfaces ◽

Water Chain ◽

Radical Scavenging Ability ◽

Coordinated Water

Two metal complexes of theophylline were synthesized. Namely, 1 with the formula [Cu(theop)2(H2O)3]·2H2O and 2, [Zn(theop)2]∙H2O (where: theop = theophylline ion). Their properties were thoroughly investigated by the elemental analysis (EA), flame atomic absorption spectrometry (FAAS), Fourier-transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA) that were augmented by antimicrobial and antioxidant analyses. Their radical scavenging ability (RSA) is notably higher than that of a pure theophylline itself. Similarly to theophylline complexes already studied by us 3, [Mn(theop)2(H2O)4] 4, [Co(theop)2(H2O)4] and 5, [Ni(theop)2(H2O)4] title compounds are inactive against Gram-negative bacteria, but they show moderate or mild activity against Gram-positive rods. The low temperature, single crystal X-ray diffraction technique determines the crystal structure of 1. Its supramolecular crystal topology is affected by the unique, double palindrome water chain that formed by two conserved and a sole coordinated water molecules. Crystal packing arrangements were characterized by fingerprint plots that were derived from the Hirshfeld surfaces (HS), as calculated for all structures in the series 1, 3, 4, 5.

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A one-dimensional heterometallic coordination polymer with a three-dimensional supramolecular framework: poly[μ2-aqua-diaqua(2,2′-bipyridyl)(μ5-2-sulfonatobutanedioato)copper(II)sodium(I)]

Acta Crystallographica Section C Crystal Structure Communications ◽

10.1107/s0108270112030909 ◽

2012 ◽

Vol 68 (8) ◽

pp. m209-m212 ◽

Cited By ~ 1

Author(s):

Jiang-Hong Fu ◽

Yu-Ling Wang ◽

Ying Chen ◽

Chang-Hui Hu ◽

Li Tang

Keyword(s):

Title Compound ◽

Three Dimensional ◽

Distorted Octahedral Geometry ◽

Water Molecules ◽

Stacking Interactions ◽

Supramolecular Framework ◽

One Dimensional ◽

Distorted Octahedral ◽

Coordinated Water ◽

Thermal Stability Of

The title compound, [CuNa(C4H3O7S)(C10H8N2)(H2O)3]n, consists of one CuIIcation, one NaIcation, one 2-sulfonatobutanedioate trianion (SSC3−), one 2,2′-bipyridyl (bpy) ligand and three coordinated water molecules as the building unit. The coordination of the CuIIcation is composed of two pyridyl N atoms, one water O atom and two carboxylate O atoms in a distorted square-pyramidal coordination geometry with an axial elongation. The NaIcation is six-coordinated by three water molecules and three carboxylate O atoms from three SSC3−ligands in a distorted octahedral geometry. Two SSC3−ligands link two CuIIcations to form a Cu2(SSC)2(bpy)2macrocyclic unit lying across an inversion centre, which is further linked by NaIcationsviaNa—O bonds to give a one-dimensional chain. Interchain hydrogen bonds link these chains to form a two-dimensional layer, which is further extended into a three-dimensional supramolecular framework through π–π stacking interactions. The thermal stability of the title compound has also been investigated.

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Diaquabis{4-[(pyridin-2-yl)methylideneamino]benzenesulfonato-κ2 N,N′}nickel(II) tetrahydrate

Acta Crystallographica Section E Structure Reports Online ◽

10.1107/s1600536812022179 ◽

2012 ◽

Vol 68 (6) ◽

pp. m809-m810 ◽

Cited By ~ 1

Author(s):

Chao-Zhu Li ◽

Xue-Ren Huang

Keyword(s):

Hydrogen Bonding ◽

Three Dimensional ◽

Title Complex ◽

Water Molecules ◽

Framework Structure ◽

Distorted Octahedral Environment ◽

Hydrogen Bonding Interactions ◽

Octahedral Environment ◽

Distorted Octahedral ◽

Coordinated Water

In the title complex, [Ni(C12H9N2O3S)2(H2O)2]·4H2O, the NiII ion is coordinated by four N atoms from two bidentate chelating 4-[(pyridin-2-yl)methylideneamino]benzenesulfonate ligands and two O atoms from cis-related water molecules in a slightly distorted octahedral environment [Ni—N = 2.071 (3)–2.121 (3) Å and Ni—O = 2.071 (2) and 2.073 (3) Å]. In the crystal, the coordinated water molecules and the four water molecules of solvation are involved in intermolecular O—H...O hydrogen-bonding interactions with water and sulfonate O-atom acceptors, giving a three-dimensional framework structure.

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