Pub Date : 2024-03-01DOI: 10.1107/S2414314624001913
Esther H. Park , Sarah M. Ortiz , Todd K. Liang , Bradley W. Smucker , S. Bernès (Editor)
In the structure of the title compound, the Ru—N distances of the DMAP ligands are influenced by the trans chloride or dimethylsulfoxide-κS ligands.
The structure of the title compound, [RuCl2(C7H10N2)2(C2H6OS)2], has monoclinic (P21/n) symmetry. The Ru—N distances of the coordination compound are influenced by the trans chloride or dimethylsulfoxide-κS ligands. The molecular structure exhibits disorder for two of the terminal methyl groups of a dimethyl sulfoxide ligand.
{"title":"cis,cis,cis-Dichloridobis(N 4,N 4-dimethylpyridin-4-amine-κN 1)bis(dimethyl sulfoxide-κS)ruthenium(II)","authors":"Esther H. Park , Sarah M. Ortiz , Todd K. Liang , Bradley W. Smucker , S. Bernès (Editor)","doi":"10.1107/S2414314624001913","DOIUrl":"10.1107/S2414314624001913","url":null,"abstract":"<div><p>In the structure of the title compound, the Ru—N distances of the DMAP ligands are influenced by the <em>trans</em> chloride or dimethylsulfoxide-κ<em>S</em> ligands.</p></div><div><p>The structure of the title compound, [RuCl<sub>2</sub>(C<sub>7</sub>H<sub>10</sub>N<sub>2</sub>)<sub>2</sub>(C<sub>2</sub>H<sub>6</sub>OS)<sub>2</sub>], has monoclinic (<em>P</em>2<sub>1</sub>/<em>n</em>) symmetry. The Ru—N distances of the coordination compound are influenced by the <em>trans</em> chloride or dimethylsulfoxide-κ<em>S</em> ligands. The molecular structure exhibits disorder for two of the terminal methyl groups of a dimethyl sulfoxide ligand. <span><figure><span><img><ol><li><span>Download : <span>Download high-res image (270KB)</span></span></li><li><span>Download : <span>Download full-size image</span></span></li></ol></span></figure></span> </p></div>","PeriodicalId":94324,"journal":{"name":"IUCrData","volume":"9 3","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140077896","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
The title compound was synthesized using Mn(CO)5Br. The manganese atom is situated on a crystallographic inversion center. The supramolecular architecture is characterized by several intermolecular C—H⋯N, N—H⋯Br and C—H⋯π interactions.
The title compound, trans-dibromidotetrakis(5-methyl-1H-pyrazole-κN2)manganese(II), [MnBr2(C4H6N2)4] or [Mn(3-MePzH)4Br2] (1) crystallizes in the triclinic P space group with the cell parameters a = 7.6288 (3), b = 8.7530 (4), c = 9.3794 (4) Å and α = 90.707 (4), β = 106.138 (4), γ = 114.285 (5)°, V = 542.62 (5) Å3, T = 120 K. The asymmetric unit contains only half the molecule with the manganese atom is situated on a crystallographic inversion center. The 3-MePzH ligands are present in an AABB type manner with two methyl groups pointing up and the other two down. The supramolecular architecture is characterized by several intermolecular C—H⋯N, N—H⋯Br, and C—H⋯π interactions. Earlier, a polymorphic structure of [Mn(3-MePzH)4Br2] (2) with a similar geometry and also an AABB arrangement for the pyrazole ligands was described [Reedijk et al. (1971#). Inorg. Chem. 10, 2594–2599; a = 8.802 (6), b = 9.695 (5), c = 7.613 (8) Å and α = 105.12 (4), β = 114.98 (4), γ = 92.90 (3)°, V = 558.826 (5) Å3, T = 295 K]. A varying supramolecular pattern was reported, with the structure of 1 featuring a herringbone type pattern while that of structure 2 shows a pillared network type of arrangement along the a axis. A nickel complex [Ni(3-MePzH)4Br2] isomorphic to 1 and the analogous chloro derivatives of FeII, CoII and CuII are also known.
{"title":"trans-Dibromidotetrakis(5-methyl-1H-pyrazole-κN 2)manganese(II)","authors":"Manikumar Athan , Soundararajan Krishnan , Nagarajan Loganathan , M. Zeller (Editor)","doi":"10.1107/S2414314624002372","DOIUrl":"10.1107/S2414314624002372","url":null,"abstract":"<div><p>The title compound was synthesized using Mn(CO)<sub>5</sub>Br. The manganese atom is situated on a crystallographic inversion center. The supramolecular architecture is characterized by several intermolecular C—H⋯N, N—H⋯Br and C—H⋯π interactions.</p></div><div><p>The title compound, <em>trans</em>-dibromidotetrakis(5-methyl-1<em>H</em>-pyrazole-κ<em>N</em> <sup>2</sup>)manganese(II), [MnBr<sub>2</sub>(C<sub>4</sub>H<sub>6</sub>N<sub>2</sub>)<sub>4</sub>] or [Mn(3-MePzH)<sub>4</sub>Br<sub>2</sub>] (<strong>1</strong>) crystallizes in the triclinic <em>P</em> <figure><img></figure> space group with the cell parameters <em>a</em> = 7.6288 (3), <em>b</em> = 8.7530 (4), <em>c</em> = 9.3794 (4) Å and α = 90.707 (4), β = 106.138 (4), γ = 114.285 (5)°, <em>V</em> = 542.62 (5) Å<sup>3</sup>, <em>T</em> = 120 K. The asymmetric unit contains only half the molecule with the manganese atom is situated on a crystallographic inversion center. The 3-MePzH ligands are present in an <em>AABB</em> type manner with two methyl groups pointing up and the other two down. The supramolecular architecture is characterized by several intermolecular C—H⋯N, N—H⋯Br, and C—H⋯π interactions. Earlier, a polymorphic structure of [Mn(3-MePzH)<sub>4</sub>Br<sub>2</sub>] (<strong>2</strong>) with a similar geometry and also an <em>AABB</em> arrangement for the pyrazole ligands was described [Reedijk <em>et al.</em> (1971<span>#</span>). <em>Inorg. Chem</em>. <strong>10</strong>, 2594–2599; <em>a</em> = 8.802 (6), <em>b</em> = 9.695 (5), <em>c</em> = 7.613 (8) Å and α = 105.12 (4), β = 114.98 (4), γ = 92.90 (3)°, <em>V</em> = 558.826 (5) Å<sup>3</sup>, <em>T</em> = 295 K]. A varying supramolecular pattern was reported, with the structure of <strong>1</strong> featuring a herringbone type pattern while that of structure <strong>2</strong> shows a pillared network type of arrangement along the <em>a</em> axis. A nickel complex [Ni(3-MePzH)<sub>4</sub>Br<sub>2</sub>] isomorphic to <strong>1</strong> and the analogous chloro derivatives of Fe<sup>II</sup>, Co<sup>II</sup> and Cu<sup>II</sup> are also known. <span><figure><span><img><ol><li><span>Download : <span>Download high-res image (274KB)</span></span></li><li><span>Download : <span>Download full-size image</span></span></li></ol></span></figure></span> </p></div>","PeriodicalId":94324,"journal":{"name":"IUCrData","volume":"9 3","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140230317","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-03-01DOI: 10.1107/S2414314624001755
Benjamin Knies , Ingo Hartenbach , M. Weil (Editor)
The crystal structure of defect-scheelite type Nd2/3[WO4] consists of [WO4]2− tetrahedra and trigonal [NdO8]13– dodecahedra.
Neodymium(III) ortho-oxidotungstate(VI) was synthesized as a side-product in an unsuccessful synthesis attempt at fluoride derivatives of neodymium tungstate in fused silica ampoules, using neodymium(III) oxide, neodymium(III) fluoride and tungsten trioxide. Violet, platelet-shaped single crystals of the title compound emerged of the bulk, which crystallize in the defect scheelite type with a trigonal dodecahedral coordination of oxide anions around the Nd3+ cations and the hexavalent tungsten cations situated in the centers of oxide tetrahedra.
{"title":"Crystal structure of defect scheelite-type Nd2/3[WO4]","authors":"Benjamin Knies , Ingo Hartenbach , M. Weil (Editor)","doi":"10.1107/S2414314624001755","DOIUrl":"10.1107/S2414314624001755","url":null,"abstract":"<div><p>The crystal structure of defect-scheelite type Nd<sub>2/3</sub>[WO<sub>4</sub>] consists of [WO<sub>4</sub>]<sup>2−</sup> tetrahedra and trigonal [NdO<sub>8</sub>]<sup>13–</sup> dodecahedra.</p></div><div><p>Neodymium(III) <em>ortho</em>-oxidotungstate(VI) was synthesized as a side-product in an unsuccessful synthesis attempt at fluoride derivatives of neodymium tungstate in fused silica ampoules, using neodymium(III) oxide, neodymium(III) fluoride and tungsten trioxide. Violet, platelet-shaped single crystals of the title compound emerged of the bulk, which crystallize in the defect scheelite type with a trigonal dodecahedral coordination of oxide anions around the Nd<sup>3+</sup> cations and the hexavalent tungsten cations situated in the centers of oxide tetrahedra. <span><figure><span><img><ol><li><span>Download : <span>Download high-res image (168KB)</span></span></li><li><span>Download : <span>Download full-size image</span></span></li></ol></span></figure></span> </p></div>","PeriodicalId":94324,"journal":{"name":"IUCrData","volume":"9 3","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140262806","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-03-01DOI: 10.1107/S2414314624002359
Mohd Abdul Fatah Abdul Manan , David B. Cordes , Aidan P. McKay , W. T. A. Harrison (Editor)
The crystal structure of a new fluorinated dithiocarbazate imine containing the isatin moiety, 4-fluorobenzyl (Z)-2-(2-oxoindolin-3-ylidene)hydrazine-1-carbodithioate, is described.
The title compound, C16H12FN3OS, a fluorinated dithiocarbazate imine derivative, was synthesized by the one-pot, multi-component condensation reaction of hydrazine hydrate, carbon disulfide, 4-fluorobenzyl chloride and isatin. The compound demonstrates near-planarity across much of the molecule in the solid state and a Z configuration for the azomethine C=N bond. The Z form is further stabilized by the presence of an intramolecular N—H⋯O hydrogen bond. In the extended structure, molecules are linked into dimers by N—H⋯O hydrogen bonds and further connected into chains along either [2 0] or [100] by weak C—H⋯S and C—H⋯F hydrogen bonds, which further link into corrugated sheets and in combination form the overall three-dimensional network.
{"title":"4-Fluorobenzyl (Z)-2-(2-oxoindolin-3-ylidene)hydrazine-1-carbodithioate","authors":"Mohd Abdul Fatah Abdul Manan , David B. Cordes , Aidan P. McKay , W. T. A. Harrison (Editor)","doi":"10.1107/S2414314624002359","DOIUrl":"10.1107/S2414314624002359","url":null,"abstract":"<div><p>The crystal structure of a new fluorinated dithiocarbazate imine containing the isatin moiety, 4-fluorobenzyl (<em>Z</em>)-2-(2-oxoindolin-3-ylidene)hydrazine-1-carbodithioate, is described.</p></div><div><p>The title compound, C<sub>16</sub>H<sub>12</sub>FN<sub>3</sub>OS, a fluorinated dithiocarbazate imine derivative, was synthesized by the one-pot, multi-component condensation reaction of hydrazine hydrate, carbon disulfide, 4-fluorobenzyl chloride and isatin. The compound demonstrates near-planarity across much of the molecule in the solid state and a <em>Z</em> configuration for the azomethine C=N bond. The <em>Z</em> form is further stabilized by the presence of an intramolecular N—H⋯O hydrogen bond. In the extended structure, molecules are linked into dimers by N—H⋯O hydrogen bonds and further connected into chains along either [2 <figure><img></figure> 0] or [100] by weak C—H⋯S and C—H⋯F hydrogen bonds, which further link into corrugated sheets and in combination form the overall three-dimensional network. <span><figure><span><img><ol><li><span>Download : <span>Download high-res image (225KB)</span></span></li><li><span>Download : <span>Download full-size image</span></span></li></ol></span></figure></span> </p></div>","PeriodicalId":94324,"journal":{"name":"IUCrData","volume":"9 3","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140228684","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-03-01DOI: 10.1107/S2414314624001986
Liping Kang , Sihui Long , W. T. A. Harrison (Editor)
The molecules of the title compound pair up to form carboxylic acid–carboxylic acid homodimers in the crystal structure.
The title compound, C13H10BrNO2, was obtained by the reaction of 2,5-dibromobenzoic acid and aniline. The molecule is twisted with a dihedral angle between the aromatic rings of 45.74 (11)° and an intramolecular N—H⋯O hydrogen bond is seen. In the crystal, pairwise O—H⋯O hydrogen bonds generate carboxylic acid inversion dimers.
{"title":"5-Bromo-2-(phenylamino)benzoic acid","authors":"Liping Kang , Sihui Long , W. T. A. Harrison (Editor)","doi":"10.1107/S2414314624001986","DOIUrl":"10.1107/S2414314624001986","url":null,"abstract":"<div><p>The molecules of the title compound pair up to form carboxylic acid–carboxylic acid homodimers in the crystal structure.</p></div><div><p>The title compound, C<sub>13</sub>H<sub>10</sub>BrNO<sub>2</sub>, was obtained by the reaction of 2,5-dibromobenzoic acid and aniline. The molecule is twisted with a dihedral angle between the aromatic rings of 45.74 (11)° and an intramolecular N—H⋯O hydrogen bond is seen. In the crystal, pairwise O—H⋯O hydrogen bonds generate carboxylic acid inversion dimers. <span><figure><span><img><ol><li><span>Download : <span>Download high-res image (220KB)</span></span></li><li><span>Download : <span>Download full-size image</span></span></li></ol></span></figure></span> </p></div>","PeriodicalId":94324,"journal":{"name":"IUCrData","volume":"9 3","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140078524","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-03-01DOI: 10.1107/S2414314624002347
Claudia Oliva-Colunga , Jessica J. Sánchez García , Marcos Flores-Alamo , Elena I. Klimova , E. R. T. Tiekink (Editor)
The structure of 2-ferrocenyl-2-[(2-ferrocenylethenyl)(morpholin-4-yl)methyl]-1,3-dithiolane, is described. In the crystal, cyclopentadienyl-C—H⋯O(morpholinyl) interactions feature within helical chains parallel to the c-axis direction. The chains are connected by methylene- and cyclopentadienyl-C—H⋯O(cyclopentadienyl) interactions.
The molecular structure of 2-ferrocenyl-2-[(2-ferrocenylethenyl)(morpholin-4-yl)methyl]-1,3-dithiolane, [Fe2(C5H5)2(C19H21NOS2)] or C29H31Fe2NOS2, has the ferrocenyl fragments in a trans disposition with respect to the vinyl group. One of the methylene groups is disordered over two sites with occupancies of 0.782 (13):0.218 (13). In the crystal, cyclopentadienyl-C—H⋯O(morpholinyl) interactions feature within helical chains parallel to the c-axis direction. The chains are connected by methylene- and cyclopentadienyl-C—H⋯O(cyclopentadienyl) interactions.
2-ferrocenyl-2-[(2-ferrocenylethenyl)(morpholin-4-yl)methyl]-1,3-dithiolane, [Fe2(C5H5)2(C19H21NOS2)] 或 C29H31Fe2NOS2 的分子结构中,二茂铁基片段与乙烯基呈反式排列。其中一个亚甲基杂乱地分布在两个位点上,占据率分别为 0.782 (13):0.218 (13)。在晶体中,环戊二烯基-C-H...O(吗啉基)相互作用在平行于 c 轴方向的螺旋链上。这些链通过亚甲基和环戊二烯基-C-H...O(环戊二烯基)相互作用连接起来。
{"title":"2-Ferrocenyl-2-[(2-ferrocenylethenyl)(morpholin-4-yl)methyl]-1,3-dithiolane","authors":"Claudia Oliva-Colunga , Jessica J. Sánchez García , Marcos Flores-Alamo , Elena I. Klimova , E. R. T. Tiekink (Editor)","doi":"10.1107/S2414314624002347","DOIUrl":"10.1107/S2414314624002347","url":null,"abstract":"<div><p>The structure of 2-ferrocenyl-2-[(2-ferrocenylethenyl)(morpholin-4-yl)methyl]-1,3-dithiolane, is described. In the crystal, cyclopentadienyl-C—H⋯O(morpholinyl) interactions feature within helical chains parallel to the <em>c</em>-axis direction. The chains are connected by methylene- and cyclopentadienyl-C—H⋯O(cyclopentadienyl) interactions.</p></div><div><p>The molecular structure of 2-ferrocenyl-2-[(2-ferrocenylethenyl)(morpholin-4-yl)methyl]-1,3-dithiolane, [Fe<sub>2</sub>(C<sub>5</sub>H<sub>5</sub>)<sub>2</sub>(C<sub>19</sub>H<sub>21</sub>NOS<sub>2</sub>)] or C<sub>29</sub>H<sub>31</sub>Fe<sub>2</sub>NOS<sub>2</sub>, has the ferrocenyl fragments in a <em>trans</em> disposition with respect to the vinyl group. One of the methylene groups is disordered over two sites with occupancies of 0.782 (13):0.218 (13). In the crystal, cyclopentadienyl-C—H⋯O(morpholinyl) interactions feature within helical chains parallel to the <em>c</em>-axis direction. The chains are connected by methylene- and cyclopentadienyl-C—H⋯O(cyclopentadienyl) interactions. <span><figure><span><img><ol><li><span>Download : <span>Download high-res image (323KB)</span></span></li><li><span>Download : <span>Download full-size image</span></span></li></ol></span></figure></span> </p></div>","PeriodicalId":94324,"journal":{"name":"IUCrData","volume":"9 3","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140223256","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
The bis-chelated mononuclear nickel(II) complex shows inversion symmetry, with the dithiocarbazato ligand in the usual trans configuration and the central metal cation in a square-planar coordination environment.
The central NiII atom in the title complex, [Ni(C13H25N2S2)2], is located on an inversion center and adopts a roughly square-planar coordination environment defined by two chelating N,S donor sets of two symmetry-related ligands in a trans configuration. The Ni—N and Ni—S bond lenghts are 1.9193 (14) and 2.1788 (5) Å, respectively, with a chelating N—Ni—S bond angle of 86.05 (4)°. These data are compared with those measured for similar dithiocarbazato ligands that bear n-octyl or n-hexyl alkyl chains. Slight differences are observed with respect to the phenylethylidene derivative where the ligands are bound cis relative to one another.
{"title":"Bis[S-octyl 3-(2-methylpropylidene)dithiocarbazato-κ2 N 3,S]nickel(II)","authors":"Sultana Shakila Khan , Md. Belayet Hossain Howlader , Md. Chanmiya Sheikh , Ryuta Miyatake , Ennio Zangrando , M. Weil (Editor)","doi":"10.1107/S241431462400186X","DOIUrl":"10.1107/S241431462400186X","url":null,"abstract":"<div><p>The bis-chelated mononuclear nickel(II) complex shows inversion symmetry, with the dithiocarbazato ligand in the usual <em>trans</em> configuration and the central metal cation in a square-planar coordination environment.</p></div><div><p>The central Ni<sup>II</sup> atom in the title complex, [Ni(C<sub>13</sub>H<sub>25</sub>N<sub>2</sub>S<sub>2</sub>)<sub>2</sub>], is located on an inversion center and adopts a roughly square-planar coordination environment defined by two chelating <em>N</em>,<em>S</em> donor sets of two symmetry-related ligands in a <em>trans</em> configuration. The Ni—N and Ni—S bond lenghts are 1.9193 (14) and 2.1788 (5) Å, respectively, with a chelating N—Ni—S bond angle of 86.05 (4)°. These data are compared with those measured for similar dithiocarbazato ligands that bear <em>n</em>-octyl or <em>n</em>-hexyl alkyl chains. Slight differences are observed with respect to the phenylethylidene derivative where the ligands are bound <em>cis</em> relative to one another. <span><figure><span><img><ol><li><span>Download : <span>Download high-res image (207KB)</span></span></li><li><span>Download : <span>Download full-size image</span></span></li></ol></span></figure></span> </p></div>","PeriodicalId":94324,"journal":{"name":"IUCrData","volume":"9 3","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140077844","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}