Pub Date : 2024-02-08DOI: 10.1107/s2056989024001233
S. Ö. Yıldırım, M. Akkurt, Ezgi Pehlivanlar, Gökalp Çetin, R. Şimşek, R. Butcher, Ajaya Bhattarai
The crystal structures and Hirshfeld surface analyses of three similar compounds are reported. Methyl 4-[4-(difluoromethoxy)phenyl]-2,7,7-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, (C21H23F2NO4), (I), crystallizes in the monoclinic space group C2/c with Z = 8, while isopropyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, (C23H27F2NO4), (II) and tert-butyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, (C24H29F2NO4), (III) crystallize in the orthorhombic space group Pbca with Z = 8. In the crystal structure of (I), molecules are linked by N—H...O and C—H...O interactions, forming a tri-periodic network, while molecules of (II) and (III) are linked by N—H...O, C—H...F and C—H...π interactions, forming layers parallel to (002). The cohesion of the molecular packing is ensured by van der Waals forces between these layers. In (I), the atoms of the 4-difluoromethoxyphenyl group are disordered over two sets of sites in a 0.647 (3): 0.353 (3) ratio. In (III), the atoms of the dimethyl group attached to the cyclohexane ring, and the two carbon atoms of the cyclohexane ring are disordered over two sets of sites in a 0.646 (3):0.354 (3) ratio.
{"title":"Syntheses, characterizations, crystal structures and Hirshfeld surface analyses of methyl 4-[4-(difluoromethoxy)phenyl]-2,7,7-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, isopropyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate and t","authors":"S. Ö. Yıldırım, M. Akkurt, Ezgi Pehlivanlar, Gökalp Çetin, R. Şimşek, R. Butcher, Ajaya Bhattarai","doi":"10.1107/s2056989024001233","DOIUrl":"https://doi.org/10.1107/s2056989024001233","url":null,"abstract":"The crystal structures and Hirshfeld surface analyses of three similar compounds are reported. Methyl 4-[4-(difluoromethoxy)phenyl]-2,7,7-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, (C21H23F2NO4), (I), crystallizes in the monoclinic space group C2/c with Z = 8, while isopropyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, (C23H27F2NO4), (II) and tert-butyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, (C24H29F2NO4), (III) crystallize in the orthorhombic space group Pbca with Z = 8. In the crystal structure of (I), molecules are linked by N—H...O and C—H...O interactions, forming a tri-periodic network, while molecules of (II) and (III) are linked by N—H...O, C—H...F and C—H...π interactions, forming layers parallel to (002). The cohesion of the molecular packing is ensured by van der Waals forces between these layers. In (I), the atoms of the 4-difluoromethoxyphenyl group are disordered over two sets of sites in a 0.647 (3): 0.353 (3) ratio. In (III), the atoms of the dimethyl group attached to the cyclohexane ring, and the two carbon atoms of the cyclohexane ring are disordered over two sets of sites in a 0.646 (3):0.354 (3) ratio.","PeriodicalId":504738,"journal":{"name":"Acta Crystallographica Section E Crystallographic Communications","volume":" 20","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139793344","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-02-08DOI: 10.1107/s2056989024000963
B. Chidambaranathan, S. Sivaraj, P. Vijayamathubalan, S. Abraham Rajasekar, S. Selvakumar
The title compound, [CdBr2(C6H14N2O)], was synthesized upon complexation of 4-(2-aminoethyl)morpholine and cadmium(II) bromide tetrahydrate at 303 K. It crystallizes as a centrosymmetric dimer, with one cadmium atom, two bromine atoms and one N,N′-bidentate 4-(2-aminoethyl)morpholine ligand in the asymmetric unit. The metal atom is six-coordinated and has a distorted octahedral geometry. In the crystal, O...Cd interactions link the dimers into a polymeric double chain and intermolecular C—H...O hydrogen bonds form R 2 2(6) ring motifs. Further C—H...Br and N—H...Br hydrogen bonds link the components into a three-dimensional network. As the N—H...Br hydrogen bonds are shorter than the C—H...Br interactions, they have a larger effect on the packing. A Hirshfeld surface analysis reveals that the largest contributions to the packing are from H...H (46.1%) and Br...H/H...Br (38.9%) interactions with smaller contributions from the O...H/H...O (4.7%), Br...Cd/Cd...Br (4.4%), O...Cd/Cd...O (3.5%), Br...Br (1.1%), Cd...H/H...Cd (0.9%), Br...O/O...Br (0.3%) and O...N/N...O (0.1%) contacts.
{"title":"[4-(2-Aminoethyl)morpholine-κ2\u0000 N,N′]dibromidocadmium(II): synthesis, crystal structure and Hirshfeld surface analysis","authors":"B. Chidambaranathan, S. Sivaraj, P. Vijayamathubalan, S. Abraham Rajasekar, S. Selvakumar","doi":"10.1107/s2056989024000963","DOIUrl":"https://doi.org/10.1107/s2056989024000963","url":null,"abstract":"The title compound, [CdBr2(C6H14N2O)], was synthesized upon complexation of 4-(2-aminoethyl)morpholine and cadmium(II) bromide tetrahydrate at 303 K. It crystallizes as a centrosymmetric dimer, with one cadmium atom, two bromine atoms and one N,N′-bidentate 4-(2-aminoethyl)morpholine ligand in the asymmetric unit. The metal atom is six-coordinated and has a distorted octahedral geometry. In the crystal, O...Cd interactions link the dimers into a polymeric double chain and intermolecular C—H...O hydrogen bonds form R\u0000 2\u0000 2(6) ring motifs. Further C—H...Br and N—H...Br hydrogen bonds link the components into a three-dimensional network. As the N—H...Br hydrogen bonds are shorter than the C—H...Br interactions, they have a larger effect on the packing. A Hirshfeld surface analysis reveals that the largest contributions to the packing are from H...H (46.1%) and Br...H/H...Br (38.9%) interactions with smaller contributions from the O...H/H...O (4.7%), Br...Cd/Cd...Br (4.4%), O...Cd/Cd...O (3.5%), Br...Br (1.1%), Cd...H/H...Cd (0.9%), Br...O/O...Br (0.3%) and O...N/N...O (0.1%) contacts.","PeriodicalId":504738,"journal":{"name":"Acta Crystallographica Section E Crystallographic Communications","volume":"6 4","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139851781","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-02-06DOI: 10.1107/s2056989024001051
Ashley M. Hastings, Ashley Williams, Robert G. Surbella III, A. Hixon, Ana Arteaga
Lanthanide-containing materials are of interest in the field of crystal engineering because of their unique properties and distinct structure types. In this context, a new samarium–sodium heterometallic coordination polymer, poly[tetrakis(μ2-2-formyl-6-methoxyphenolato)samarium(III)sodium(I)], {[SmNa(C8H7O3)4]·solvent} n (Sm-1), was synthesized and crystallized via slow evaporation from a mixture of ethanol and acetonitrile. The compound features alternating SmIII and NaI ions, which are linked by ortho-vanillin (o-vanillin) ligands to form a mono-periodic chain-like coordination polymer. The chains propagate along the [001] direction. Residual electron density of disordered solvent molecules in the void space could not be reasonably modeled, thus the SQUEEZE function was applied. The structural, vibrational, and optical properties are reported.
含镧系元素的材料因其独特的性质和不同的结构类型而在晶体工程领域备受关注。在此背景下，我们合成了一种新型钐钠杂金属配位聚合物--聚[四(μ2-2-甲酰基-6-甲氧基苯酚)钐(III)钠(I)]，{[SmNa(C8H7O3)4]-溶剂} n (Sm-1)，并通过乙醇和乙腈混合物的缓慢蒸发结晶。该化合物以交替出现的 SmIII 离子和 NaI 离子为特征，它们通过正香兰素（邻香兰素）配体连接形成单周期链状配位聚合物。链沿着 [001] 方向传播。空隙中无序溶剂分子的残留电子密度无法合理建模，因此采用了 SQUEEZE 函数。报告了其结构、振动和光学特性。
{"title":"Structural characterization of a new samarium–sodium heterometallic coordination polymer","authors":"Ashley M. Hastings, Ashley Williams, Robert G. Surbella III, A. Hixon, Ana Arteaga","doi":"10.1107/s2056989024001051","DOIUrl":"https://doi.org/10.1107/s2056989024001051","url":null,"abstract":"Lanthanide-containing materials are of interest in the field of crystal engineering because of their unique properties and distinct structure types. In this context, a new samarium–sodium heterometallic coordination polymer, poly[tetrakis(μ2-2-formyl-6-methoxyphenolato)samarium(III)sodium(I)], {[SmNa(C8H7O3)4]·solvent}\u0000 n\u0000 (Sm-1), was synthesized and crystallized via slow evaporation from a mixture of ethanol and acetonitrile. The compound features alternating SmIII and NaI ions, which are linked by ortho-vanillin (o-vanillin) ligands to form a mono-periodic chain-like coordination polymer. The chains propagate along the [001] direction. Residual electron density of disordered solvent molecules in the void space could not be reasonably modeled, thus the SQUEEZE function was applied. The structural, vibrational, and optical properties are reported.","PeriodicalId":504738,"journal":{"name":"Acta Crystallographica Section E Crystallographic Communications","volume":"104 3","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139801421","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-02-06DOI: 10.1107/s2056989024000938
A. Temesgen, A. Sapronov, A. S. Kubasov, Alexander S. Novikov, Tuan Anh Le, A. Tskhovrebov
The reaction between 2-pyridylselenenyl chloride and isobutyronitrile results in the formation of the corresponding cationic pyridinium-fused 1,2,4-selenodiazole, namely, 3-(propan-2-yl)-1,2,4-[1,2,4]selenadiazolo[4,5-a]pyridin-4-ylium chloride, C9H11N2Se+·Cl−, in high yield (89%). The structure of the compound, established by means of single-crystal X-ray analysis at 100 K, has monoclinic (P21/c) symmetry and revealed the presence of bifurcated chalcogen-hydrogen bonding Se...Cl−...H—Cl, and these non-covalent contacts were analysed by DFT calculations followed by a topological analysis of the electron-density distribution (wB97XD/6-311++G** level of theory).
2-pyridylselenyl chloride 与异丁腈反应生成了相应的阳离子吡啶融合 1,2,4-selenodiazole 即 3-(propan-2-yl)-1,2,4-[1,2,4]硒二唑并[4,5-a]吡啶-4-鎓氯化物 C9H11N2Se+-Cl-，收率高达 89%。通过在 100 K 温度下进行单晶 X 射线分析，确定了该化合物的结构具有单斜（P21/c）对称性，并揭示了 Se...Cl-...H-Cl 的二叉查耳根氢键的存在，这些非共价接触通过 DFT 计算进行了分析，随后对电子密度分布进行了拓扑分析（wB97XD/6-311++G** 理论水平）。
{"title":"Synthesis and crystal structure of the adduct between 2-pyridylselenyl chloride and isobutyronitrile","authors":"A. Temesgen, A. Sapronov, A. S. Kubasov, Alexander S. Novikov, Tuan Anh Le, A. Tskhovrebov","doi":"10.1107/s2056989024000938","DOIUrl":"https://doi.org/10.1107/s2056989024000938","url":null,"abstract":"The reaction between 2-pyridylselenenyl chloride and isobutyronitrile results in the formation of the corresponding cationic pyridinium-fused 1,2,4-selenodiazole, namely, 3-(propan-2-yl)-1,2,4-[1,2,4]selenadiazolo[4,5-a]pyridin-4-ylium chloride, C9H11N2Se+·Cl−, in high yield (89%). The structure of the compound, established by means of single-crystal X-ray analysis at 100 K, has monoclinic (P21/c) symmetry and revealed the presence of bifurcated chalcogen-hydrogen bonding Se...Cl−...H—Cl, and these non-covalent contacts were analysed by DFT calculations followed by a topological analysis of the electron-density distribution (wB97XD/6-311++G** level of theory).","PeriodicalId":504738,"journal":{"name":"Acta Crystallographica Section E Crystallographic Communications","volume":"8 2","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139800516","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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