Monoclinic Crystal Class Research Articles

Structure elucidation, DFT and IRI computational investigations of a novel 4-(3-(4-chlorophenyl)-1-phenyl-1H-pyrazol-4-yl)2,6-dimethyl-1,4-dihydropyridine-3,5-dicarbonitrile

A novel symmetric dihydropyridine possessing cyano group at C11 and C14 has been synthesized using a modified Hantzsch method. The compound (▪) was characterized spectroscopically by Mass, IR and 1H NMR methods and finally confirmed by X-ray diffraction study. The compound crystallizes in a monoclinic crystal class with P21/c space group. In the title molecule, the dihydropyridine ring is puckered and displayed an envelope conformation of the type E1. The solid state of the title compound is governed by an intermolecular C–H…N, C–H…Cl and C–H…π interactions in the building of a crystal. It is investigated by three dimensional Hirshfeld surfaces mapped on different properties, also the relevant fingerprint graphs are obtained to recognize the percentage contribution from various inter atomic contacts. The topology of three dimensional interaction energy frameworks were constructed using the energy density wave function of DFT/B3LYP/6-311++G(d,p) and the energy corresponding to intermolecular interactions were assessed. The density functional theory analysis has been carried out and hence an energy gap and global index parameters are evaluated, also the geometric parameters are computed by optimizing the molecular structure of the title compound. The natural bonding orbitals (NBO) analysis is carried out to know the intermolecular charge transfer in the molecule. Reduced density gradients (RDG) and interaction region indicators (IRI) analysis reveals the chemical bonding and weak interactions regions. The molecular docking has been performed on 1B38, 2OHM, 3VNT and 4URO receptors shows good binding affinities and their results reveal that it serves as potential anti-cancer agent.

Synthesis, XRD, characterization and antibacterial activity of novel α,β unsaturated carbonyl compound: (Z)-2-((3-(4-chlorophenyl)-1-phenyl-1H-pyrazol-4-yl)methylene)-3,4-dihydronaphthalen-1(2H)-one (C26H19ClN2O)

A novel organic α,β unsaturated carbonyl compound (Z)-2-((3-(4-chlorophenyl)-1-phenyl-1H-pyrazol-4-yl)methylene)-3,4-dihydronaphthalen-1(2H)-one (K) was Synthesized through Ultrasound Irradiation by the help of green solvent and grown a high quality single crystal by slow evaporation method. Structural confirmation was carried out by most acceptable spectroscopic techniques i.e. MS, IR, NMR, CMR, DSC, Crystal Structure of K was determined by single crystal X-ray Diffraction. The single crystal of K was developed in 0.40 × 0.35 × 0.30 mm dimension in EtOH:Acetone (1:2) solvent system. K crystallizes in the monoclinic crystal class in the asymmetrical space group with Z = 4. Potency of compound was assayed against four bacterial microorganisms.

Crystal structures and Hirshfeld surface analysis of (cat)2[FeIII(η3-dipic)(NCS)3] and (cat)[FeIII(η3-dipic)(H2O)(NCS)2] (dipic = dipicolinate)

Crystal and molecular structures of black (cat)2[FeIII(η3-dipic)(NCS)3] (cat = C9H7NH; C10H9NH); (HNC10H8NH)[FeIII(dipic)(NCS)3], and (C6H7NH)[FeIII(η3-dipic)(H2O)(NCS)2] (dipic pyridine-2,6-dicarboxylate (−2); C9H7NH = quinolinium; C10H9NH = 3-methylisoquinolinium; HNC10H8NH = 4,4-bipyridinium; C6H7NH = 2-picolinium) were determinated. These complexes crystallized in monoclinic crystal class. Each Fe(III) atom is six coordinated. The octahedron is build up unsymmetrically, one half side is creates by terdentate dipic–1O,2N,3O ligand and the other half by three monodentate (NCS)3 or (NCS)2(H2O) donor ligands. The terdentate dipic–1O,2N,3O ligand forms a pair of five-membered metallocyclic rings with the common central 2N atom of pyridine (1OC22NC23O) with the mean value of O–Fe–N bite angles of 75.5°. The mean value of trans1O–Fe–3O bond angles is 150.8° in complexes with an inner coordination spheres FeO2N4 and FeO3N3. The mean value of sum of all three ((Fe–1O) + (Fe–2N) + (Fe–3O)) bond distances is 6.217 Å (FeO2N4) and 6.183 Å (FeO3N3). The opposite side in FeO2N4 is created by three monodentate NCS groups with the sum of Fe–N(x3) bond distances of 6.050 Å and in the FeO3N3 two NCS groups with water create opposite side with the sum of (Fe–N(x2) + Fe–O) bond distances of 6.183 Å. One polymorph of complex (C10H9NH)2[FeIII(dipic)(NCS)3] contains two crystallographically independent molecules differ mostly by degree of distortion in Fe–L bond distances and L–Fe–L bond angles and are examples of distortion isomerism. The data of the complexes are compare and discuses with the data of familiar iron(III) complexes. The intermolecular interactions of all compounds are studied by Hirshfeld surface analysis.

Synthesis, Characterization, Crystal and Molecular Structure Analysis of 1-(2-Chlorophenyl)-3-methyl-4-(p-tolylthio)-1H-pyrazol-5-ol

The synthesis of a novel tolylthiopyrazol bearing methyl group has been achieved by transition metal free N-chlorosuccinimide mediated direct sulfenylation of 1-aryl pyrazolones at room temperature. The product obtained was characterized by spectroscopic techniques and finally confirmed by X-ray diffraction studies. The compound 1-(2-chlorophenyl)-3-methyl-4-(p-tolylthio)-1H-pyrazol-5-ol (m.f. C17H15N2OSCl) crystallizes in monoclinic crystal class in space group P21/c with cell parameters a = 9.6479(5) Å, b = 15.1233(8) Å, c = 11.4852(6) Å, β = 108.374(2)°, V=1590.4(2) Å3 and Z = 4. The final residual factor R1 = 0.0499.

Synthesis, Characterization, Crystal, and Molecular Structure Analysis of 3,4-dihydro-6-(2-hydroxyphenyl)-5-nitro-4-phenylpyrimidin-2(1H)-one

A novel nitro and 2-hydroxyphenyl functionalized pyrimidinone at C5 and C6, respectively, has been synthesized using 1-(2-hydroxyphenyl)-2-nitroethanone, benzaldehyde, urea, and etidronic acid as a catalyst is described. The synthesized compound characterized by spectroscopic techniques and finally confirmed by X-ray diffraction studies. The molecule crystallizes in the monoclinic crystal class in the space group P21/c with cell parameters a = 11.1070(10)Å, b = 8.8210(4)Å, c = 15.1110(13)Å, β = 106.193(2)°, and Z = 4. The pyrimidine ring adopts flattened boat conformation.

Synthesis, Characterization, Crystal and Molecular Structure Analysis of 2,6-Dimethyl-3-Acetyl-5-Carbomethoxy-4-Phenyl-1,4-Dihydropyridine

The synthesis of a novel unsymmetrical dihydropyridine, bearing carboxy methyl and carbomethoxy groups at C(3) and C(5), respectively, has been achieved by applying the modified Hantzsch-type condensation, which involves the Michael addition of Knoevenagel adduct with an enamine. The product obtained was characterized by spectroscopic techniques and finally confirmed by X-ray diffraction studies. The title compound C17H19NO3 crystallizes in Monoclinic crystal class in space group P21/c with cell parameters a = 9.9130(12) Å, b = 7.3320(5) Å, c = 22.018(3) Å, β = 109.637(3)°, V = 1507.2(3) Å3 and Z = 4. The final residual factor R 1 = 0.0642. The structure exhibits both intra and inter-molecular hydrogen bonding of the type C–H···O and N–H···O. The pyridine ring gives boat conformation. The crystal and molecular structure of 2,6-dimethyl-3-acetyl-5-carbomethoxy-4-phenyl-1,4-dihydropyridine has been determined by X-ray diffraction methods.

Structural Conformation of a Novel Piperidine-4-One Derivative: 1-Acryloyl-3-Methyl-2,6-Dip-Tolylpiperidine-4-One

The novel 3-methyl-2,6-dip-toylpiperidine-4-one was acylated by 3-chloropropanoychloride and subjected for dehydrohalogenation. The synthesized compound was characterized by spectroscopic techniques and finally confirmed by X-ray diffraction studies. The molecule crystallizes in the monoclinic crystal class in the space group C(2)/c with cell parameters a = 18.538(2) angstrom, b = 9.9050(1) angstrom, c = 22.954(2) angstrom, beta = 94.486(8)degrees and Z = 8. The piperidine ring adopts a twist boat conformation.

Synthesis and Crystal Structure of 4-(1,3-Diphenyl-1H-pyrazol-5-yl)pyridine

The title compound, C20H15N3, was synthesized and the structure was investigated by X-ray crystallography. The compound crystallizes in the monoclinic crystal class in the space group P21/c with cell parameters a = 10.5700(6)Å, b = 12.2810(13)Å, c = 12.1750(13)Å, β = 94.429(7)° and Z = 4.

Crystal and Molecular Structure Studies of a Novel 1-Benzhydryl-piperazine Derivative: 1-Benzhydryl-4-(4-chloro-2-fluoro-benzene-sulfonyl)-piperazine

The title compound 1-benzhydryl-4-(4-chloro-2-fluoro-benzenesulfonyl)-piperazine was synthesized, and structure of the product obtained was confirmed by the X-ray diffraction study. The compound C23H22ClFN2O2S crystallizes in the monoclinic crystal class in the space group P21/c with cell parameters a = 9.6180(7) Å , b = 12.9670(10) Å , c = 19.4020(12) Å , β = 114.716(3)°, and Z = 4. The structure has been solved by direct methods and refined to R 1 = 0.0440 for 3877 observed reflections with I > 2σ(I). The structure reveals that the piperazine ring is in a chair conformation. The geometry around the S atom is distorted tetrahedral.

Structural Conformation of a Novel 1-Benzhydrylpiperazine Derivative: 1-Benzhydryl-4-(toluene-4-sulfonyl)-piperazine

The title compound 1-benzhydryl-4-(toluene-4-sulfonyl)-piperazine was synthesized and the structure was investigated by X-ray crystallography. The title compound, C24H26N2O2S crystallizes in the monoclinic crystal class in the space group P21/c with cell parameters a = 13.5800(10) A, b = 8.9630(7) A, c = 18.9040(10) A, β = 106.851(3)°, Z = 4 and V = 2202.1(3) A3. The structure has been solved by direct methods and refined to R 1 = 0.0468 for 3174 observed reflections I > 2σ(I). The structure reveals that the piperazine ring is in a chair conformation. The geometry around the S atom is a distorted tetrahedron. The title compound 1-benzhydryl-4-(toluene-4-sulfonyl)-piperazine was synthesized and the structure was investigated by X-ray crystallography. The title compound, C24H26N2O2S crystallizes in the monoclinic crystal class in the space group P21/c with cell parameters a = 13.5800(10) A, b = 8.9630(7) A, c = 18.9040(10) A, β = 106.851(3)°, Z = 4 and V = 2202.1(3) A3. The structure has been solved by direct methods and refined to R 1 = 0.0468 for 3174 observed reflections I > 2σ(I). The structure reveals that the piperazine ring is in a chair conformation. The geometry around the S atom is a distorted tetrahedron.

Synthesis and Crystal Structure of [1-(Toluene-4-Sulfonyl)-Piperidin-4-yl]-Methanol

The title compound, [1-(toluene-4-sulfonyl)-piperidin-4-yl]-methanol was synthesized by the condensation of diphenyl(piperidin-4-yl)methanol with p-toluenesulfonyl chloride in methylene dichloromethane as solvent and triethylamine as the base. The product obtained was characterized by spectroscopic techniques and the structure was investigated by X-ray crystallography. The compound crystallizes in the monoclinic crystal class in the space group P21/c with cell parameters a = 10.2490(13) A˚, b = 11.4710(9) A˚, c = 20.997(3) A˚, β = 116.344(3)°, V = 2212.2(5) A˚3 for Z = 4. The structure reveals that the piperidine ring is in a chair conformation. The geometry around the S atom is comparable with the classic tetrahedral value. The structure exhibits both inter and intramolecular hydrogen bonds of the type O–H · · · O and C–H · · · O.

Synthesis and Crystal Structure of 1-(2-Nitro-benzenesulfonyl)-piperidin-4-yl-diphenyl-methanol

The title compound 1-(2-nitro-benzenesulfonyl)-piperidin-4-yl-diphenyl-methanol was synthesized by the condensation of [piperidin-4-yl]-diphenyl-methanol with 2-nitro benzene sulfonylchloride in methylene dichloride as solvent and triethylamine as the base. The product obtained was characterized by spectroscopic techniques and the structure was investigated by X-ray crystallography. The compound crystallizes in the monoclinic crystal class in the space group Pc with cell parameters a = 9.2360(4) Å, b = 10.7750(8) Å, c = 13.4110(8) Å, β = 124.162(4)°, V = 1104.35(12)Å3 for Z = 2. The structure reveals that the piperidine ring is in a chair conformation. There is a large discrepancy around the bond angles of the piperidine N atom. The geometry around the S atom is distorted tetrahedron.

Crystal and Molecular Structure Analysis of 7-Chloro-5-cyclopropyl-9-methyl-10-(2-nitro-4-trifluromethyl-Phenyl)-5,10-dihydro-4,5,6,10-tetraaza-dibenzo [a, d]cyclohepten-11-one

The compound 7-chloro-5-cyclopropyl-9-methyl-10-(2-nitro-4-trifluromethyl-phenyl)- 5,10-dihydro-4,5,6,10-tetraaza-dibenzo[a,d]cyclohepten-11-one, C22H15N5O3F3Cl, crystallizes in the monoclinic crystal class under the space group P21/c with cell parameters a = 16.595(7) Å, b = 8.775(7) Å, c = 14.973(1) Å, β = 97.465(4), V = 2161.9(3) Å3, Z = 4. The structure was solved by direct methods using SHELXS-97, and refined using SHELXL-97. The final residual factor is R1 = 0.0604 for 4116 reflections and 342 parameters. The molecular structure exhibits intramolecular hydrogen bond of the type C–H · · · O.

Synthesis and Structural Conformation Studies of a Potent Unsymmetrical 1,4-Dihydropyridine

2,6-Dimethyl-5-(phenylcarbamoyl)-4-(3-nitrophenyl)-1,4-dihydropyridine-2-carboxylate was synthesized in two steps and was characterized spectroscopically and confirmed by X-ray diffraction studies. The molecule crystallizes in the monoclinic crystal class in the spacegroup P21/c with cell parameters a = 10.5960(6) A, b = 10.2450(7) A, c = 19.5790(11) A, β = 107.448(3)° and Z = 4. The 1,4-dihydropyridine ring in the structure adopts a flattened boat conformation. 2,6-Dimethyl-5-(phenylcarbamoyl)-4-(3-nitrophenyl)-1,4-dihydropyridine-2-carboxylate was synthesized in two steps and was characterized spectroscopically and confirmed by X-ray diffraction studies. The molecule crystallizes in the monoclinic crystal class in the spacegroup P21/c with cell parameters a = 10.5960(6) A, b = 10.2450(7) A, c = 19.5790(11) A, β = 107.448(3)° and Z = 4. The 1,4-dihydropyridine ring in the structure adopts a flattened boat conformation.

Synthesis and Crystal Structure of 1-Benzhydryl-4-Methane-Sulfonyl-Piperazine

The title compound, 1-benzhydryl-4-methanesulfonyl-piperazine, was synthesized by the nucleophilic substitution of 1-benzhydryl-piperazine with methyl sulfonyl chloride. The product obtained was characterized by spectroscopic techniques, and the structure was investigated by X-ray crystallography. The compound crystallizes in the monoclinic crystal class in the space group P21/c with cell parameters a = 9.5820(4) A○, b = 16.8150(12) A○, c = 13.5280(8) A○, β = 127.270(5)°, and V = 1734.5(2)A○ 3 for Z = 4. The structure reveals that the piperazine ring is in a chair conformation. There is a large discrepancy around the bond angles of the piperazine N atoms. The geometry around the S atom is distorted tetrahedral.

Synthesis and Crystal Structure of 1-Benzenesulfonyl-4-benzhydryl-piperazine

1-Benzenesulfonyl-4-benzhydryl-piperazine was synthesized from 1-benzhydryl piperazine with benzenesulfonyl chloride. The title compound, C23H24N2O2S, was synthesized and the structure was investigated by X-ray crystallography. The compound crystallizes in the monoclinic crystal class in the space group P21/c with cell parameters a = 13.2390(10) Å, b = 9.1960(7) Å, c = 18.5810(16) Å, β = 110.873(3)°, and Z = 4. The piperazine ring in the structure is in a chair conformation. The geometry around the S atom is distorted tetrahedral. The structure exhibits an intermolecular hydrogen bond of the type C‒H · O.

Synthesis and Crystal Structure of 1-Tosyl-1H-[1,2,4]-triazole

The title compound was synthesized and the structure was investigated by X-ray crystallography. The compound crystallizes in the monoclinic crystal class in the space group P21/c with cell parameters a = 7.541(4)A, b = 17.958(8)A, c = 8.091(4)A, β = 111.16(4)° and Z = 4. The geometry around the S atom is distorted tetrahedral. The structure exhibits intermolecular hydrogen bonds of the type C-H…O.

Synthesis and Crystal Structure of 1-(4-fluorophenyl)-3-(3,4,5-trimethoxyphenyl)-2-propen-1-one

The title compound C18 H17FO4 was synthesized and recrystallized from an organic solution. The crystal structure of 1-(4-fluorophenyl)-3-(3,4,5-trimethoxyphenyl)-2-propen-1-one was determined by X-ray diffraction analysis. The title compound crystallizes in the monoclinic crystal class in the space group P21/c with cell parameters a = 7.6930(6) Å, b = 15.2320(11)Å, c = 14.1280(12) Å, β = 106.596(3)°, Z = 4, and V = 1586.6(2) Å3. The unsaturated keto group is not strictly planar and is in a s-cis conformation.

Synthesis and Crystal Structure of 3,4,5-Trimethoxybenzaldehyde oxime monohydrate

The title compd., C10H13NO5 was synthesized and the structure was investigated by X-ray methods. The compd. crystallizes in monoclinic crystal class in the space group P21/c with cell parameters a = 8.2660(4)A…, b = 18.5580(19)A…, c = 7.3470(8)A…, I² = 90.352(6)°, V = 1127.01(18) and Z = 4. The structure exhibits intermol. hydrogen bonds of the type O-H···O. [on SciFinder(R)]

Crystal Structure of 3-para tolyl-6-(4'-methyl-biphenyl-2-yl)-[1,2,4]triazolo[3,4-b][1,3,4]thiadiazole

The title compound, C23H18N4S, was synthesized and the structure was investigated by X-ray crystallography. The compound crystallizes in the monoclinic crystal class in the space group P21/c with cell parameters a = 16.378(2)Å, b = 5.9050(4)Å, c = 25.026(3)Å, β = 127.981(3)°, Z = 4 and V = 1907.7(4)Å3. The condensed 1,2,4-triazolo thiadiazole ring is planar. The bond lengths indicate electron deloclization in the triazole ring system.