A new three dimensional proton transfer compound including citric acid and 2,4,6-triamine-1,3,5-triazine: synthesis, characterization and X-ray crystal structure

Two isostructural diarsenates, SrZnAs2O7(strontium zinc diarsenate), (I), and BaCuAs2O7[barium copper(II) diarsenate], (II), have been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction. The three-dimensional open-framework crystal structure consists of corner-sharingM2O5(M2 = Zn or Cu) square pyramids and diarsenate (As2O7) groups. Each As2O7group shares its five corners with five differentM2O5square pyramids. The resulting framework delimits two types of tunnels aligned parallel to the [010] and [100] directions where the large divalent nine-coordinatedM1 (M1 = Sr or Ba) cations are located. The geometrical characteristics of theM1O9,M2O5and As2O7groups of known isostructural diarsenates, adopting the general formulaM1IIM2IIAs2O7(M1II= Sr, Ba, Pb;M2II= Mg, Co, Cu, Zn) and crystallizing in the space groupP21/n, are presented and discussed.

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The Crystal Structure of KIO3.HIO3

Canadian Journal of Chemistry ◽

10.1139/v71-072 ◽

1971 ◽

Vol 49 (3) ◽

pp. 468-476 ◽

Cited By ~ 12

Author(s):

Lilian Y. Y. Chan ◽

F. W. B. Einstein

Keyword(s):

Crystal Structure ◽

Three Dimensional ◽

Monoclinic Space Group ◽

X Ray ◽

R Factor ◽

Octahedral Environment ◽

Distorted Octahedral ◽

Potassium Hydrogen ◽

A Cell ◽

Least Squares Techniques

The crystal structure of potassium hydrogen di-iodate (bi-iodate) KIO3.HIO3 was determined from three dimensional X-ray data collected by counter methods. The structure was refined by full-matrix least-squares techniques to a conventional R factor of 5.0 % for the 1392 observed reflexions. The salt crystallizes in the monoclinic space group P21/c with eight formula units in a cell of dimension a = 7.028(1) Å, b = 8.203(1) Å, c = 21.841(3) Å, β = 98.03(1)°.The iodate units are all basically pyramidal; weak interionic I—O contacts complete a very distorted octahedral environment around three iodine atoms. There is a capped octahedral (7-coordinate) environment around the remaining iodine atom. The I—O bonds are in the range 1.75–1.82 Å and the I—OH bonds are 1.91 and 1.95 Å, variations in length can be correlated with differences in the degree of involvement in (a) hydrogen bonding and (b) interaction with adjacent iodine atoms.

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The crystal structure of gatehouseite

Mineralogical Magazine ◽

10.1180/minmag.2011.075.6.2823 ◽

2011 ◽

Vol 75 (6) ◽

pp. 2823-2832

Author(s):

P. Elliott ◽

A. Pring

Keyword(s):

Crystal Structure ◽

Hydrogen Bonding ◽

Three Dimensional ◽

Direct Methods ◽

Chemical Analyses ◽

X Ray Diffraction ◽

X Ray ◽

Manganese Phosphate ◽

Phosphate Mineral ◽

Unit Formula

AbstractThe crystal structure of the manganese phosphate mineral gatehouseite, ideally Mn52+(PO4)2(OH)4, space group P212121, a = 17.9733(18), b = 5.6916(11), c = 9.130(4) Å, V= 933.9(4) Å3, Z = 4, has been solved by direct methods and refined from single-crystal X-ray diffraction data (T = 293 K) to an R index of 3.76%. Gatehouseite is isostructural with arsenoclasite and with synthetic Mn52+(PO4)2(OH)4. The structure contains five octahedrally coordinated Mn sites, occupied by Mn plus very minor Mg with observed <Mn—O> distances from 2.163 to 2.239 Å. Two tetrahedrally coordinated P sites, occupied by P, Si and As, have <P—O> distances of 1.559 and 1.558 Å. The structure comprises two types of building unit. A strip of edge-sharing Mn(O,OH)6 octahedra, alternately one and two octahedra wide, extends along [010]. Chains of edge- and corner-shared Mn(O,OH)6 octahedra coupled by PO4 tetrahedra extend along [010]. By sharing octahedron and tetrahedron corners, these two units form a dense three-dimensional framework, which is further strengthened by weak hydrogen bonding. Chemical analyses by electron microprobe gave a unit formula of (Mn4.99Mg0.02)Σ5.01(P1.76Si0.07(As0.07)Σ2.03O8(OH)3.97.

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Piperazinium Bis(hydrogen-3,5-pyrazoledicarboxylate) Proton Transfer Compound and Its Zinc(II) Complex: Synthesis, Characterization and Crystal Structure

Journal of Chemical Crystallography ◽

10.1007/s10870-018-0741-3 ◽

2018 ◽

Vol 49 (2) ◽

pp. 98-105 ◽

Cited By ~ 1

Author(s):

Mahboubeh A. Sharif ◽

Gholam Reza Najafi

Keyword(s):

Crystal Structure ◽

Proton Transfer ◽

Proton Transfer Compound

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X-Ray Single Crystal Structural Analysis of Magnetically Oriented Microcrystals

Acta Crystallographica Section A Foundations and Advances ◽

10.1107/s2053273314088615 ◽

2014 ◽

Vol 70 (a1) ◽

pp. C1138-C1138

Author(s):

Chiaki Tsuboi ◽

Kazuki Aburaya ◽

Shingo Higuchi ◽

Fumiko Kimura ◽

Masataka Maeyama ◽

...

Keyword(s):

Molecular Structure ◽

Crystal Structure ◽

Single Crystal ◽

Three Dimensional ◽

Diffraction Measurement ◽

X Ray Diffraction ◽

Data Set ◽

Uv Curable ◽

X Ray

We have developed magnetically oriented microcrystal array (MOMA) technique that enables single crystal X-ray diffraction analyses from microcrystalline powder. In this method, microcrystals suspended in a UV-curable monomer matrix are there-dimensionally aligned by special rotating magnetic field, followed by consolidation of the matrix by photopolymerization. From thus achieved MOMAs, we have been succeeded in crystal structure analysis for some substances [1, 2]. Though MOMA method is an effective technique, it has some problems as follows: in a MOMA, the alignment is deteriorated during the consolidation process. In addition, the sample microcrystals cannot be recovered from a MOMA. To overcome these problems, we performed an in-situ X-ray diffraction measurement using a three-dimensional magnetically oriented microcrystal suspension (3D MOMS) of L-alanine. An experimental setting of the in-situ X-ray measurement of MOMS is schematically shown in the figure. L-alanine microcrystal suspension was poured into a glass capillary and placed on the rotating unit equipped with a pair of neodymium magnets. Rotating X-ray chopper with 10°-slits was placed between the collimator and the suspension. By using this chopper, it was possible to expose the X-ray only when the rotating MOMS makes a specific direction with respect to the impinging X-ray. This has the same effect as the omega oscillation in conventional single crystal measurement. A total of 22 XRD images of 10° increments from 0° to 220° were obtained. The data set was processed by using conventional software to obtain three-dimensional molecular structure of L-alanine. The structure is in good agreement with that reported for the single crystal. R1 and wR2 were 6.53 and 17.4 %, respectively. RMSD value between the determined molecular structure and the reported one was 0.0045 Å. From this result, we conclude that this method can be effective and practical to be used widely for crystal structure analyses.

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Crystal structure and hydrogen bonding in the water-stabilized proton-transfer salt brucinium 4-aminophenylarsonate tetrahydrate

Acta Crystallographica Section E Crystallographic Communications ◽

10.1107/s2056989016006691 ◽

2016 ◽

Vol 72 (5) ◽

pp. 751-755 ◽

Cited By ~ 1

Author(s):

Graham Smith ◽

Urs D. Wermuth

Keyword(s):

Crystal Structure ◽

Hydrogen Bond ◽

Hydrogen Bonding ◽

Hydrogen Bonds ◽

Proton Transfer ◽

Network Structure ◽

Three Dimensional ◽

Water Molecules ◽

Arsanilic Acid ◽

Dimensional Network

In the structure of the brucinium salt of 4-aminophenylarsonic acid (p-arsanilic acid), systematically 2,3-dimethoxy-10-oxostrychnidinium 4-aminophenylarsonate tetrahydrate, (C23H27N2O4)[As(C6H7N)O2(OH)]·4H2O, the brucinium cations form the characteristic undulating and overlapping head-to-tail layered brucine substructures packed along [010]. The arsanilate anions and the water molecules of solvation are accommodated between the layers and are linked to them through a primary cation N—H...O(anion) hydrogen bond, as well as through water O—H...O hydrogen bonds to brucinium and arsanilate ions as well as bridging water O-atom acceptors, giving an overall three-dimensional network structure.

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An Unexpected Trinuclear Cobalt(II) Complex Based on a Half-Salamo-Like Ligand: Synthesis, Crystal Structure, Hirshfeld Surface Analysis, Antimicrobial and Fluorescent Properties

Crystals ◽

10.3390/cryst9080408 ◽

2019 ◽

Vol 9 (8) ◽

pp. 408 ◽

Cited By ~ 1

Author(s):

Ruo-Yan Li ◽

Xiao-Xin An ◽

Juan-Li Wu ◽

You-Peng Zhang ◽

Wen-Kui Dong

Keyword(s):

Crystal Structure ◽

Surface Analysis ◽

Three Dimensional ◽

Antimicrobial Activities ◽

Hirshfeld Surface ◽

Hirshfeld Surface Analysis ◽

Fluorescent Properties ◽

X Ray ◽

X Ray Crystallography ◽

Elemental Analyses

An unexpected trinuclear Co(II) complex, [Co3(L2)2(μ-OAc)2(CH3OH)2]·2CH3OH (H2L2 = 4,4′-dibromo-2,2′-[ethylenedioxybis(nitrilomethylidyne)]diphenol) constructed from a half-Salamo-based ligand (HL1 = 2-[O-(1-ethyloxyamide)]oxime-4-bromophenol) and Co(OAc)2·4H2O, has been synthesized and characterized by elemental analyses, infrared spectra (IR), UV-Vis spectra, X-ray crystallography and Hirshfeld surface analysis. The Co(II) complex contains three Co(II) atoms, two completely deprotonated (L2)2− units, two bridged acetate molecules, two coordinated methanol molecules and two crystalline methanol molecules, and finally, a three-dimensional supramolecular structure with infinite extension was formed. Interestingly, during the formation of the Co(II) complex, the ligand changed from half-Salamo-like to a symmetrical single Salamo-like ligand due to the bonding interactions of the molecules. In addition, the antimicrobial activities of HL1 and its Co(II) complex were also investigated.

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