Crystal structures of the pyrazinamide–p-aminobenzoic acid (1/1) cocrystal and the transamidation reaction product 4-(pyrazine-2-carboxamido)benzoic acid in the molten state

2015 ◽  
Vol 71 (11) ◽  
pp. 1010-1016 ◽  
Author(s):  
Shridhar H. Thorat ◽  
Sanjay Kumar Sahu ◽  
Rajesh G. Gonnade
Keyword(s):  
Benzoic Acid ◽  
Linear Chain ◽  
Acid Amide ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Two Dimensional ◽  
Molten State ◽  
Aminobenzoic Acid ◽  
Characterization Methods ◽  
Space Group

The synthesis of pharmaceutical cocrystals is a strategy to enhance the performance of active pharmaceutical ingredients (APIs) without affecting their therapeutic efficiency. The 1:1 pharmaceutical cocrystal of the antituberculosis drug pyrazinamide (PZA) and the cocrystal formerp-aminobenzoic acid (p-ABA), C7H7NO2·C5H5N3O, (1), was synthesized successfully and characterized by relevant solid-state characterization methods. The cocrystal crystallizes in the monoclinic space groupP21/ncontaining one molecule of each component. Both molecules associateviaintermolecular O—H...O and N—H...O hydrogen bonds [O...O = 2.6102 (15) Å and O—H...O = 168.3 (19)°; N...O = 2.9259 (18) Å and N—H...O = 167.7 (16)°] to generate a dimeric acid–amide synthon. Neighbouring dimers are linked centrosymmetrically through N—H...O interactions [N...O = 3.1201 (18) Å and N—H...O = 136.9 (14)°] to form a tetrameric assembly supplemented by C—H...N interactions [C...N = 3.5277 (19) Å and C—H...N = 147°]. Linking of these tetrameric assemblies through N—H...O [N...O = 3.3026 (19) Å and N—H...O = 143.1 (17)°], N—H...N [N...N = 3.221 (2) Å and N—H...N = 177.9 (17)°] and C—H...O [C...O = 3.5354 (18) Å and C—H...O = 152°] interactions creates the two-dimensional packing. Recrystallization of the cocrystals from the molten state revealed the formation of 4-(pyrazine-2-carboxamido)benzoic acid, C12H9N3O3, (2), through a transamidation reaction between PZA andp-ABA. Carboxamide (2) crystallizes in the triclinic space groupP-1 with one molecule in the asymmetric unit. Molecules of (2) form a centrosymmetric dimeric homosynthon through an acid–acid O—H...O hydrogen bond [O...O = 2.666 (3) Å and O—H...O = 178 (4)°]. Neighbouring assemblies are connected centrosymmetricallyviaa C—H...N interaction [C...N = 3.365 (3) Å and C—H...N = 142°] engaging the pyrazine groups to generate a linear chain. Adjacent chains are connected looselyviaC—H...O interactions [C...O = 3.212 (3) Å and C—H...O = 149°] to generate a two-dimensional sheet structure. Closely associated two-dimensional sheets in both compounds are stackedviaaromatic π-stacking interactions engaging the pyrazine and benzene rings to create a three-dimensional multi-stack structure.

Crystal structure of 2-(2,6-Dichlorophenylcarbamoyl)benzoic acid

1982 ◽  
Vol 35 (9) ◽  
pp. 1933 ◽  
Author(s):  
CHL Kennard ◽  
G Smith ◽  
GF Katekar
Keyword(s):  
Crystal Structure ◽  
Benzoic Acid ◽  
Dihedral Angle ◽  
Acid Amide ◽  
Three Dimensional ◽  
Direct Methods ◽  
Acid Group ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
A Cell

The crystal structure of 2-(2,6-dichlorophenylcarbamoyl)benzoic acid has been determined by direct methods from three-dimensional X-ray diffraction data and refined to R 0.076 for 971 'observed' reflections. Crystals are monoclinic, space group P21/c with Z4 in a cell of dimensions a 12.150(6), b l3.629(6), c 8.368(4) �, β lO3.75(4)�. The molecules form centrosymmetric hydrogen-bonded cyclic dimers [O. . .O, 2.64(1) �] with the carboxylic acid group lying in the approximate plane of the attached benzene ring (dihedral angle 7.63�). This is in turn almost parallel to the 2,6-dichlorophenyl substituent group on the acid amide (dihedral angle 4.14�). The amide group is synclinally related to the ring systems in a similar way to that found in other phthalamic acids.

scholarly journals Synthesis, structure and magnetocaloric properties of a new two-dimensional gadolinium(III) coordination polymer based on azobenzene-2,2′,3,3′-tetracarboxylic acid

2021 ◽  
Vol 77 (10) ◽  
pp. 591-598
Author(s):  
Wen-Wen Wei ◽  
Li-Ping Lu ◽  
Si-Si Feng ◽  
Miao-Li Zhu ◽  
Ulli Englert
Keyword(s):  
Coordination Polymer ◽  
Linear Chain ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Two Dimensional ◽  
Tetracarboxylic Acid ◽  
Symmetry Direction ◽  
Carboxylate Groups ◽  
Dimensional Network ◽  
Short Hydrogen Bond

A new Gd3+ coordination polymer (CP), namely, poly[diaqua[μ4-1′-carboxy-3,3′-(diazene-1,2-diyl)dibenzene-1,2,2′-tricarboxylato]gadolinium(III)], [Gd(C16H7N2O8)(H2O)2] n , (I), has been synthesized hydrothermally from Gd(NO3)3·6H2O and azobenzene-2,2′,3,3′-tetracarboxylic acid (H4abtc). The target solid has been characterized by single-crystal and powder X-ray diffraction, elemental analysis, IR spectroscopy and susceptibility measurements. CP (I) crystallizes in the monoclinic space group C2/c. The structure features a 4-connected topology in which Gd3+ ions are connected by carboxylate groups into a linear chain along the monoclinic symmetry direction. Adjacent one-dimensional aggregates are bridged by Habtc3− ligands to form a two-dimensional CP in the (10-1) plane. A very short hydrogen bond [O...O = 2.4393 (4) Å] links neighbouring layers into a three-dimensional network. A magnetic study revealed antiferromagnetic Gd...Gd coupling within the chain direction. CP (I) displays a significant magnetocaloric effect (MCE), with a maximum −ΔS m of 27.26 J kg−1 K−1 for ΔH = 7 T at 3.0 K. As the MCE in (I) exceeds that of the commercial magnetic refrigerant GGG (Gd3Ga5O12, −ΔS m = 24 J kg−1 K−1, ΔH = 30 kG), CP (I) can be regarded as a potential cryogenic material for low-temperature magnetic refrigeration.

Two- and three-dimensional coordination polymers based on zinc(II) and furan-2,5-dicarboxylic acid: structure variation due to metal-to-linker ratio

2018 ◽  
Vol 74 (12) ◽  
pp. 1719-1724 ◽  
Author(s):  
Yimin Mao ◽  
Peter Y. Zavalij
Keyword(s):  
Dicarboxylic Acid ◽  
Coordination Polymers ◽  
Three Dimensional ◽  
Molar Ratio ◽  
Monoclinic Space Group ◽  
Structure Variation ◽  
Space Group ◽  
Hydrogen Bonding Pattern ◽  
Solvent Molecules ◽  
A Chain

Two ZnII-based coordination polymers (CPs) were synthesized by the hydrothermal method, using Zn(NO3)2·6H2O and furan-2,5-dicarboxylic acid (FDCA) in dimethylformamide (DMF) solvent, at 95 °C. Poly[tetrakis(dimethylazanium) [tetrakis(μ2-furan-2,5-dicarboxylato-κ2 O 2:O 5)dizinc(II)]], {(C2H8N)4[Zn2(C6H2O5)4]} n or {[DMA]4[ZnII 2(FDC)4]} n (DMA = dimethylazanium and FDC = furan-2,5-dicarboxylate), (1), was obtained with a 1:1 molar ratio of ZnII and FDCA. It crystallized in the monoclinic space group C2/c. Coordinated by ZnII ions, FDC2− ligands form 21 double-stranded helices propagating along the b axis. The helices are interconnected and extend laterally in the a direction, forming a two-dimensional (2D) sheet-like network. The 2D sheets are stacked along the c direction without interconnections. DMA cations are cocrystallized in (1) and are hydrogen bonded with carboxylate O atoms of the FDC2− ligands. The hydrogen-bonding pattern consists of R 2 2(4) and R 2 2(10) motifs alternating in a chain. Poly[bis(dimethylazanium) [bis(μ4-furan-2,5-dicarboxylato-κO 2:κO 2′:κO 5:κO 5)bis(μ3-furan-2,5-dicarboxylato-κO 2:κO 2′:κO 5)dizinc(II)] dimethylformamide 3.08-solvate], {(C2H8N)2[Zn2(C6H2O5)4]·3.08C3H7NO} n or {[DMA]2[ZnII 3(FDC)4]·3.08DMF} n , (2), was obtained with a 1:2 molar ratio of ZnII and FDCA. It crystallized in the monoclinic space group P21/c, forming a three-dimensional network. The pores are filled with DMA cations and DMF solvent molecules.

Dislocation lines in the swallowtail diffraction catastrophe

2006 ◽  
Vol 463 (2078) ◽  
pp. 343-355 ◽  
Author(s):  
J.F Nye
Keyword(s):  
Three Dimensional ◽  
Optical Vortices ◽  
Monoclinic Space Group ◽  
Tail Region ◽  
Amplitude Wave ◽  
Space Group ◽  
Wave Interference ◽  
Diffraction Integral ◽  
Dimensional Distribution ◽  
Front Region

The three-dimensional distribution of amplitude and phase represented by the swallowtail catastrophe diffraction integral is based on a network of null lines for amplitude (wave dislocations or optical vortices), where the phase is singular. In the tail region there is four-wave interference, which results in an approximately repeating pattern of amplitude based on the monoclinic space group C 2/ m and also an approximately repeating pattern of wave dislocations based on the black–white monoclinic space group C 2/ m ′. Helical dislocations spring from the plane of symmetry and gradually straighten out to be parallel to the two riblines of the caustic; eventually they become the straight dislocations of the Pearcey pattern for the cusp catastrophe. In the front region, where there are zero or two points of stationary phase, each dark Airy fringe surface associated with the fold surface condenses into a single dislocation in the plane of symmetry.

Crystallography of quasi-crystals

1986 ◽  
Vol 42 (4) ◽  
pp. 261-271 ◽  
Author(s):  
T. Janssen
Keyword(s):  
Three Dimensional ◽  
Three Dimensions ◽  
Crystal Phase ◽  
Two Dimensional ◽  
Space Group ◽  
Quasi Crystals ◽  
Special Case

The symmetry of quasi-crystals, a class of materials that has recently aroused interest, is discussed. It is shown that a quasi-crystal is a special case of an incommensurate crystal phase and that it can be described by a space group in more than three dimensions. A number of relevant three-dimensional quasi-crystals is discussed, in particular dihedral and icosahedral structures. The symmetry considerations are also applied to the two-dimensional Penrose patterns.

Crystal and Molecular Structure of Difluorochlorine(III)-hexafluoroarsenate(V), ClF2AsF6

1971 ◽  
Vol 49 (15) ◽  
pp. 2539-2543 ◽  
Author(s):  
H. Lynton ◽  
J. Passmore
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Chlorine Atom ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Arsenic Atom ◽  
Space Group

Crystals of difluorochlorine(III)hexafluoroarsenate(V), ClF2AsF6, are monoclinic, space group A2/a, a = 10.676(9), b = 7.673(7), c = 8.064(7) Å, β = 113.40(5)°. The structure was refined by three dimensional least squares methods to R = 0.045 for 185 independent observed reflections. The chlorine atom has two nearest fluorine neighbors at 1.541(14) Å, with a F—Cl—F angle of 103.17(0.70)°, and two longer fluorine bonds at 2.339(14) Å. All five atoms lie in a plane. The arsenic atom is octahedrally coordinated to six fluorine atoms and is connected to two ClF2+ groups via trans fluorine bridges.

Dinuclear cobalt and nickel complexes of a mercaptoacetic acid substituted 1,2,4-triazole ligand: syntheses, structures and urease inhibitory studies

2019 ◽  
Vol 75 (12) ◽  
pp. 1658-1665 ◽  
Author(s):  
Zi-Yi Fang ◽  
Li Zhang ◽  
Jian-Ping Ma ◽  
Long Zhao ◽  
Shi-Ling Wang ◽  
...  
Keyword(s):  
Three Dimensional ◽  
Mercaptoacetic Acid ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
Hydrogen Bond Interactions ◽  
Triazole Ligand ◽  
Coordination Ability ◽  
Urease Inhibitory ◽  
Cobalt And Nickel

Because of its versatile coordination modes and strong coordination ability, the mercaptoacetic acid substituted 1,2,4-triazole 2-{[5-(pyridin-2-yl)-4H-1,2,4-triazol-3-yl]sulfanyl}acetic acid (H2L) was synthesized and characterized. Treatment of H2L with cobalt and nickel acetate afforded the dinuclear complexes {μ-3-[(carboxylatomethyl)sulfanyl]-5-(pyridin-2-yl)-4H-1,2,4-triazol-4-ido-κ2 N 1,N 5:N 2,O}bis[aqua(methanol-κO)cobalt(II)] methanol disolvate, [Co2(C9H6N4O2S)2(CH3OH)2(H2O)2]·2CH3OH (1), and {μ-3-[(carboxylatomethyl)sulfanyl]-5-(pyridin-2-yl)-4H-1,2,4-triazol-4-ido-κ2 N 1,N 5:N 2,O}bis[diaquanickel(II)] methanol disolvate dihydrate, [Ni2(C9H6N4O2S)2(H2O)4]·2CH3OH·2H2O (2), respectively. Complex 1 crystallized in the monoclinic space group P21/c, while 2 crystallized in the tetragonal space group I41/a. Single-crystal X-ray diffraction studies revealed that H2L is doubly deprotonated and acts as a tetradentate bridging ligand in complexes 1 and 2. For both of the obtained complexes, extensive hydrogen-bond interactions contribute to the formation of their three-dimensional supermolecular structures. Hirshfeld surface analysis was used to illustrate the intermolecular interactions. Additionally, the urease inhibitory activities of 1, 2 and H2L were investigated against jack bean urease, where the two complexes revealed strong urease inhibition activities.

Die Kristallstruktur von Zinkformiat-Dihydrat

1977 ◽  
Vol 145 (5-6) ◽  
Author(s):  
N. Burger ◽  
H. Fuess
Keyword(s):  
Hydrogen Bonding ◽  
Three Dimensional ◽  
Dimensional Structure ◽  
Water Molecules ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Three Dimensional Structure ◽  
Oxygen Atoms

AbstractZinc formate cristallizes isomorphous to the formates of Mg, Sr, Cd, Mn and Ni in the monoclinic space groupThe structure has been refined including an isotropic extinction correction toThe octahedra of the two nonequivalent zinc atoms are slightly distorted. Zn(l) in (000) is surrounded by six oxygen atoms of the formate groups [distances Zn(l)–O = 2.071 Å–2.145 Å]; the octahedron of Zn(2) in (½½0) consists of the oxygen atoms of the two formate groups and two water molecules [distances Zn(2)–O = 2.053 Å–2.165 Å].The three-dimensional structure is stabilized by hydrogen bonding between formate groups and water molecules.

Self-assembling of three rare structurally various homomultinuclear CuII complexes derived from a bis(salamo)-based multioxime ligand

2021 ◽  
Vol 77 (5) ◽  
pp. 848-860
Author(s):  
Peng Li ◽  
Ting Zhang ◽  
Li-Li Li ◽  
Wen-Kui Dong
Keyword(s):  
Complex Structure ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray Crystallography ◽  
Self Assembling ◽  
Elemental Analyses ◽  
New Type ◽  
Spiral Structures ◽  
Solvent Molecules

A family of rare structurally different homometal multinuclear CuII bis(salamo)-based complexes, [Cu4(L)2(MeOH)2](ClO4)2·2MeOH (1), [Cu4(L)2(EtOH)2](NO3)2·2EtOH (2) and [Cu2(HL)(EtOH)Br2]·CHCl3 (3), has been successfully synthesized by the reactions of cupric salts with a bis(salamo)-based multidentate chelate ligand (H3 L). The salamo-based ligand [R-CH=N—O—(CH2) n —O—N=CH—R] is a new type of salen-based analog. Complexes (1) and (2) are isostructural structures, and crystallize in monoclinic space group P21/n with centrosymmetric spiral structures, where the main structures contain two fully deprotonated ligand (L)3− units, a charged tetranuclear CuII folding center and two coordinated solvent molecules. Complex (3) crystallizes in monoclinic space group Cc and consists of two CuII cations, one incompletely deprotonated ligand (HL)2− unit and one coordinated ethanol molecule, and forms a novel homo-binuclear CuII complex structure due to Br− counter anions. Complexes (1)–(3) have zero-dimensional cluster-based structures and are further assembled into three-dimensional frameworks via intermolecular interactions. Because of the different solvents and counter anions which have a significant influence on the structures of complexes (1)–(3), the interactions were quantitatively evaluated by Hirshfeld surfaces analyses. Complexes (1)–(3) have been characterized by elemental analyses, IR spectra, UV–vis spectra and X-ray crystallography analyses. In addition, fluorescence properties are evaluated and DFT calculations are performed.

A new heteroleptic oxalate-based compound: poly[[2-(aminomethyl)pyridine]di-μ6-oxalato-chromium(III)potassium(I)]

2013 ◽  
Vol 70 (1) ◽  
pp. 12-15 ◽  
Author(s):  
Patrice Kenfack Tsobnang ◽  
Emmanuel Wenger ◽  
Siméon Ponou ◽  
Slimane Dahaoui ◽  
John Lambi Ngolui ◽  
...  
Keyword(s):  
Aqueous Solution ◽  
Hydrogen Bonding ◽  
Title Compound ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Pyridine Ligands ◽  
Partial Overlap

The title compound, [KCr(C2O2)2(C6H8N2)]n, was obtained from aqueous solution and analyzed with single-crystal X-ray diffraction at 100 K. It crystallizes in the monoclinic space groupC2/cand displays a three-dimensional polymeric architecture built up by bimetallic oxalate-bridged CrIII–K helical chains linked through centrosymmetric K2O2units to yield a sheet-like alternatingP/Marrangement which looks like that of the previously described two-dimensional [NaCr(ox)2(pyim)(H2O)]·2H2O [pyim is 2-(pyridin-2-yl)imidazole; Leiet al.(2006).Inorg. Chem. Commun.9, 486–488]. The CrIIIions in each helix have the same chirality. The infinite neutral sheets are eclipsed with respect to each other and are held together by a hydrogen-bonding network involving 2-(aminomethyl)pyridine H atoms and oxalate O atoms. Each sheet gives rise to channels of Cr4K4octanuclear rings and each resultant hole is occupied by a pair of 2-(aminomethyl)pyridine ligands with partial overlap. The shortest Cr...Cr distance [5.593 (4) Å] is shorter than usually observed in the K–MIII–oxalate family.

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