scholarly journals Crystal engineering: co-crystals of cinnamic acid derivatives with a pyridyl derivative co-crystallizer

Author(s):  
Daniel A. Lorenzo ◽  
Sebastian J. K. Forrest ◽  
Hazel A. Sparkes

A number of hydrogen-bonded co-crystals, consisting of a cinnamic acid derivative and a pyridyl co-crystallizer, have been synthesized and their properties investigated by X-ray diffraction. Samples were prepared by recrystallization or solvent drop grinding oftrans-cinnamic acid (1), 4-methylcinnamic acid (2), 4-methoxy cinnamic acid (3) or 3,4-methoxy cinnamic acid (4), with 4,4-dipyridyl (A),iso-nicotinamide (B) or nicotinamide (C). The X-ray single-crystal structures of seven novel co-crystals, obtained through recrystallization, are examined and the hydrogen-bonding interactions discussed. Consistent hydrogen-bonding motifs were observed for samples prepared when using 4,4-dipyridyl (A) oriso-nicotinamide (B) as the co-crystallizing agent. Powder X-ray diffraction analysis of the samples prepared by solvent drop grinding suggests the formation of ten co-crystals.

2015 ◽  
Vol 1105 ◽  
pp. 335-338
Author(s):  
Qiong Wu ◽  
Jing Lu ◽  
Xiao Lin Ji ◽  
Tao Yu Zou ◽  
Zhen Fang Qiao ◽  
...  

Modifying polyoxometalates with organic and/or metal-organic moieties is a widely adopted method for broading the range of properties. In this work a new polyoxometalate constructed from Anderson-type polyoxoanions and L-arginine (Arg =L-arginine) molecules Na [CrMo6(OH)6O18]}(H2Arg)2·8H2O(1) has been synthesized via conventional method and characterized by routine techniques. Single-crystal X-Ray diffraction analysis shows that compound 1 is constructed by chiralL-arginine grafted Anderson-type clusters, sodium cation and water molecules which are further stabilized by hydrogen bonding interactions constitute 3D supramolecular networks. In addition, both antitumor behavior and photocatalytic activities of compound 1 were investigated.


2013 ◽  
Vol 834-836 ◽  
pp. 515-518
Author(s):  
Hai Xing Liu ◽  
Qing Liu ◽  
Ting Ting Huang ◽  
Yang Xu ◽  
Lin Tong Wang ◽  
...  

A novel praseodymium complex C5H13O11Pr has been synthesized from hydrothermal reaction and the crystal structure has been determined by means of single-crystal X-ray diffraction. The Pr1 atom is nine coordinated by nine O atoms. The crystal packing is stabilized by O-H...O hydrogen bonding interactions.


2017 ◽  
Vol 73 (4) ◽  
pp. 305-313 ◽  
Author(s):  
Yun-Deng Wu ◽  
Xiao-Lei Zhang ◽  
Xiao-Hong Liu ◽  
Jian Xu ◽  
Mei Zhang ◽  
...  

Apremilast (AP) {systematic name: (S)-2-[1-(3-ethoxy-4-methoxyphenyl)-2-(methylsulfonyl)ethyl]-4-acetamidoisoindoline-1,3-dione} is an inhibitor of phosphodieasterase-4 (PDE4) and is indicated for the treatment of adult patients with active psoriatic arthritis. The ability of AP to form solvates has been investigated and three solvatomorphs of AP, namely, the AP ethyl acetate hemisolvate, C22H24N2O7S·0.5C4H8O2, the AP toluene hemisolvate, C22H24N2O7S·0.5C7H8, and the AP dichloromethane monosolvate, C22H24N2O7S·CH2Cl2, were obtained. The three AP solvatomorphs were characterized by X-ray powder diffraction, thermogravimetric analysis and differential scanning calorimetry. Single-crystal X-ray diffraction was used to analyze the structures, crystal symmetry, packing modes, stoichiometry and hydrogen-bonding interactions of the solvatomorphs. In addition, dissolution analyses were performed to study the dissolution rates of different AP solvatomorph tablets in vitro and to make comparisons with commercial apremilast tablets (produced by Celgene); all three solvatomorphs showed similar dissolution rates and similar values of the similarity factor f2 in a comparison of their dissolution profiles.


2012 ◽  
Vol 554-556 ◽  
pp. 792-795
Author(s):  
Hai Xing Liu ◽  
Jing Wang ◽  
Fang Fang Jian ◽  
Hui Juan Yue ◽  
Guang Zeng ◽  
...  

A new Eu complex [Eu (C3O9H6)] ·2(H2O) has been synthesized from a hydrothermal reaction and the crystal structure has been determined by means of single-crystal X-ray diffraction. The Eu atom is coordinated by eight O atoms. The molecular is antisymmetric structure by the C3-C3 axis. It is striking that the structure of the complex exhibits extensive O-H…O hydrogen-bonding interactions.


2018 ◽  
Vol 74 (8) ◽  
pp. 889-893
Author(s):  
Qian-Kun Zhou ◽  
Lin Wang ◽  
Dong Liu

As a class of multifunctional materials, crystalline supramolecular complexes have attracted much attention because of their unique architectures, intriguing topologies and potential applications. In this article, a new supramolecular compound, namely catena-poly[4,4′-(buta-1,3-diene-1,4-diyl)dipyridin-1-ium [(μ4-benzene-1,2,4,5-tetracarboxylato-κ6 O 1,O 1′:O 2:O 4,O 4′:O 5)cadmium(II)]], {(C14H14N2)[Cd(C10H2O8)]} n or {(1,4-H2bpbd)[Cd(1,2,4,5-btc)]} n , has been prepared by the self-assembly of Cd(NO3)2·4H2O, benzene-1,2,4,5-tetracarboxylic acid (1,2,4,5-H4btc) and 1,4-bis(pyridin-4-yl)buta-1,3-diene (1,4-bpbd) under hydrothermal conditions. The title compound has been structurally characterized by IR spectroscopy, elemental analysis, powder X-ray diffraction and single-crystal X-ray diffraction analysis. Each CdII centre is coordinated by six O atoms from four different (1,2,4,5-btc)4− tetraanions. Each CdII cation, located on a site of twofold symmetry, binds to four carboxylate groups belonging to four separate (1,2,4,5-btc)4− ligands. Each (1,2,4,5-btc)4− anion, situated on a position of \overline{1} symmetry, binds to four crystallographically equivalent CdII centres. Neighbouring CdII cations interconnect bridging (1,2,4,5-btc)4− anions to form a three-dimensional {[Cd(1,2,4,5-btc)]2−} n anionic coordination network with infinite tubular channels. The channels are visible in both the [1\overline{1}0] and the [001] direction. Such a coordination network can be simplified as a (4,4)-connected framework with the point symbol (4284)(4284). To balance the negative charge of the metal–carboxylate coordination network, the cavities of the network are occupied by protonated (1,4-H2bpbd)2+ cations that are located on sites of twofold symmetry. In the crystal, there are strong hydrogen-bonding interactions between the anionic coordination network and the (1,4-H2bpbd)2+ cations. Considering the hydrogen-bonding interactions, the structure can be further regarded as a three-dimensional (4,6)-connected supramolecular architecture with the point symbol (4264)(42687·84). The thermal stability and photoluminescence properties of the title compound have been investigated.


2013 ◽  
Vol 785-786 ◽  
pp. 424-427
Author(s):  
Hai Xing Liu ◽  
Qing Hua Zhang ◽  
Zhang Xue Yu ◽  
Quan Hua Fan ◽  
Ting Ting Huang ◽  
...  

The Y complex C4H10O10Y has been synthesized from a hydrothermal reaction and the crystal structure has been determined by means of single-crystal X-ray diffraction. The Y atom is coordinated by nine O atoms. The molecular structure stabilized by the O-H…O hydrogen-bonding interactions.


2014 ◽  
Vol 1004-1005 ◽  
pp. 542-545
Author(s):  
Ya Bing Liu ◽  
Li Guang Xiao

A new bi-capped Keggin heteropoly molybdovanadated derivative, [Co (en)3]2[SiMo8V6O42]∙6H2O (1) (en = ethylendiamine) has been hydrothermally synthesized and structurally characterized by the elemental analysis, IR, XPS and single crystal X-ray diffraction. The crystal structure analysis reveals that compound 1 consists of [Co (en)3]2+transition metal coordination fragment and the [SiMo8V6O42]4-building blocks, which are linked together via hydrogen-bonding interactions to form a new 3-D supramolecular networks.


2014 ◽  
Vol 70 (10) ◽  
pp. 949-952 ◽  
Author(s):  
Silvia C. Capelli ◽  
Hans-Beat Bürgi ◽  
Sax A. Mason ◽  
Dylan Jayatilaka

Neutron diffraction data have been collected at 12, 50, 150 and 295 K for the dipeptide glycyl-L-alanine, C5H10N2O3, in order to obtain accurate positional and anisotropic displacement parameters for the H atoms. The values of these parameters serve as a benchmark for assessing the equivalent parameters obtained from a so-called Hirshfeld-atom refinement of X-ray diffraction data described elsewhere [Capelliet al.(2014).IUCrJ,1, 361–379]. The flexibility of the glycyl-L-alanine molecule in the solid and the hydrogen-bonding interactions as a function of temperature are also considered.


2021 ◽  
Vol 252 ◽  
pp. 02069
Author(s):  
Xiaoyan Ren ◽  
Haixing Liu ◽  
Yanfang Huo

A novel complex Ni(C12H12N2)3●(C7H5O3)2●(H3BO3) has been synthesized from a hydrothermal reaction and the crystal structure has been determined by means of single-crystal X-ray diffraction. Triclinic, P-1. a= 12.5380(13) Å, b = 13.0100(15) Å, c = 15.1490(18) Å, α= 102.760(3)°, β= 94.480(2)°, γ= 94.540(2)°. V=2390.9(5) Å3. Z=2. R1 =0.0661, wR2 = 0.2128, T=293(2) K. The Ni atom is coordinated by six N atoms from three 4,4′-dimethyl-2,2′-dipyridyl molecular. The molecular structure stabilized by the O-H…O hydrogen-bonding interactions.


2018 ◽  
Vol 74 (8) ◽  
pp. 1117-1120
Author(s):  
Talal F. Al-Azemi ◽  
Mickey Vinodh ◽  
Abdirahman A. Mohamod ◽  
Fatemeh H. Alipour

Co-crystallization of a monofunctionalized hydroxy pillar[5]arene with 1-octanamine resulted in the formation of an inclusion complex where the alkyl chain is threaded in the macrocycle cavity, namely 1,2,3,4-(1,4-dimethoxy)-5-(1-hydroxy-4-methoxy)-pillar[5]arene–1-octanamine–water (1/1/1), C44H48O10·C8H19N·H2O. The guest compound is stabilized inside the cavity by hydrogen-bonding and C—H...π interactions. The water molecule in the asymmetric unit mediates the formation of a supramolecular dimer by hydrogen-bonding interactions. These functionalized-pillararene hosts expand the possibility of exploring more supramolecular interactions with various guest species.


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