IUCrDataPub Date : 2022-07-29eCollection Date: 2022-07-01DOI: 10.1107/S2414314622006216
Mohcine Missioui, Walid Guerrab, Abdulsalam Alsubari, Joel T Mague, Youssef Ramli
{"title":"2-Azido-<i>N</i>-(4-methyl-phen-yl)acetamide.","authors":"Mohcine Missioui, Walid Guerrab, Abdulsalam Alsubari, Joel T Mague, Youssef Ramli","doi":"10.1107/S2414314622006216","DOIUrl":"10.1107/S2414314622006216","url":null,"abstract":"<p><p>The asymmetric unit of the title compound, C<sub>9</sub>H<sub>10</sub>N<sub>4</sub>O, comprises three independent mol-ecules, two pairs of which differ significantly in the rotational orientation of the azido group and one pair having very similar conformations; the N-N-C-C torsion angles are -173.9 (2), -102.7 (2) and -173.6 (2)°. In the crystal, each independent mol-ecule forms N-H⋯O hydrogen bonds with its glide-plane-related counterparts, forming zigzag chains extending along the <i>c</i>-axis direction.</p>","PeriodicalId":14692,"journal":{"name":"IUCrData","volume":"7 Pt 7","pages":"x220621"},"PeriodicalIF":0.0,"publicationDate":"2022-07-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9635410/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"40669610","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}
IUCrDataPub Date : 2022-07-19eCollection Date: 2022-07-01DOI: 10.1107/S2414314622007295
Silvana Moris, Antonio Galdámez
{"title":"Rerefinement of the crystal structure of SnTe<sub>0.73(2)</sub>Se<sub>0.27(2)</sub> from single-crystal X-ray diffraction data.","authors":"Silvana Moris, Antonio Galdámez","doi":"10.1107/S2414314622007295","DOIUrl":"10.1107/S2414314622007295","url":null,"abstract":"<p><p>Compounds of the solid solution series SnTe<sub>1-<i>x</i></sub> Se <sub><i>x</i></sub> , derived from pristine SnSe and SnTe, are considered as thermoelectric lead-free materials. The crystal structure re-refinement of NaCl-type SnTe<sub>0.73 (2)</sub>Se<sub>0.27 (2)</sub> is based on single-crystal X-ray diffraction data and results in higher precision of the bond length [Sn-(Te,Se) = 3.0798 (3) Å] compared to a previous report on basis of powder X-ray data [Krebs & Langner (1964 ▸). <i>Z. Anorg. Allg. Chem.</i> <b>334</b>, 37-49].</p>","PeriodicalId":14692,"journal":{"name":"IUCrData","volume":"7 Pt 7","pages":"x220729"},"PeriodicalIF":0.0,"publicationDate":"2022-07-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9635412/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"40471238","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}
IUCrDataPub Date : 2022-07-14eCollection Date: 2022-07-01DOI: 10.1107/S2414314622006939
Nadeem Abad, Mohcine Missioui, Abdulsalam Alsubari, Joel T Mague, El Mokhtar Essassi, Youssef Ramli
{"title":"Crystal structure of ethyl 2-{4-[(2-oxo-3-phenyl-1,2-di-hydro-quinoxalin-1-yl)meth-yl]-1<i>H</i>-1,2,3-triazol-1-yl}acetate.","authors":"Nadeem Abad, Mohcine Missioui, Abdulsalam Alsubari, Joel T Mague, El Mokhtar Essassi, Youssef Ramli","doi":"10.1107/S2414314622006939","DOIUrl":"10.1107/S2414314622006939","url":null,"abstract":"<p><p>The quinoxaline portion of the title mol-ecule, C<sub>21</sub>H<sub>19</sub>N<sub>5</sub>O<sub>3</sub>, is not quite planar as indicated by a dihedral angle of 3.38 (7)° between the constituent rings. The mol-ecule is 'U-shaped', which is consolidated by an intra-molecular anti-parallel carbonyl electrostatic inter-action with C··O distances of 2.8905 (16) and 3.0221 (15) Å, in the crystal forms corrugated layers through C-H⋯O and C-H⋯N hydrogen bonds and C-H⋯π(ring) and π-stacking inter-actions.</p>","PeriodicalId":14692,"journal":{"name":"IUCrData","volume":"7 Pt 7","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2022-07-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9635411/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"40669609","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}
IUCrDataPub Date : 2022-07-12eCollection Date: 2022-07-01DOI: 10.1107/S2414314622006940
Yawei Zhou, Changzeng Fan, Bin Wen, Lifeng Zhang
{"title":"Natural djurleite with refined composition Cu<sub>61.39</sub>S<sub>32</sub> revealing disorder of some Cu sites.","authors":"Yawei Zhou, Changzeng Fan, Bin Wen, Lifeng Zhang","doi":"10.1107/S2414314622006940","DOIUrl":"10.1107/S2414314622006940","url":null,"abstract":"<p><p>A djurleite crystal was discovered from a natural sample originally labelled as chalcocite. The djurleite crystal under investigation has a refined composition of Cu<sub>61.39</sub>S<sub>32</sub>, thus revealing a Cu deficiency compared to the originally reported Cu<sub>62</sub>S<sub>32</sub> phase [Evans (1979). <i>Z. Kristallogr.</i> <b>150</b>, 299-320], where all atomic sites are reported to be fully occupied. In addition, the current refinement revealed a splitting of eight of the Cu sites into pairs.</p>","PeriodicalId":14692,"journal":{"name":"IUCrData","volume":"7 Pt 7","pages":"x220694"},"PeriodicalIF":0.0,"publicationDate":"2022-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9635409/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"40471236","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}
IUCrDataPub Date : 2022-07-08eCollection Date: 2022-07-01DOI: 10.1107/S241431462200685X
Joshua Rushlow, Andrei V Astashkin, Daniel R Albert, Edward Rajaseelan
{"title":"[(1,2,5,6-η)-Cyclo-octa-1,5-diene](4-isopropyl-1-methyl-1,2,4-triazol-5-yl-idene)(tri-cyclo-hexyl-phosphane-κ<i>P</i>)iridium(I) tetra-fluorido-borate di-chloro-methane monosolvate.","authors":"Joshua Rushlow, Andrei V Astashkin, Daniel R Albert, Edward Rajaseelan","doi":"10.1107/S241431462200685X","DOIUrl":"10.1107/S241431462200685X","url":null,"abstract":"<p><p>The title compound, [Ir(C<sub>8</sub>H<sub>12</sub>)(C<sub>6</sub>H<sub>11</sub>N<sub>3</sub>)(C<sub>18</sub>H<sub>33</sub>P)]BF<sub>4</sub>·CH<sub>2</sub>Cl<sub>2</sub>, a triazole-based N-heterocyclic carbene iridium(I) cationic complex with a tetra-fluorido-borate counter-anion, crystallizes with one di-chloro-methane solvent mol-ecule per formula unit. The Ir<sup>I</sup> atom of the cationic complex has a distorted square-planar coordination environment, defined by a bidentate cyclo-octa-1,5-diene (COD) ligand, an N-heterocyclic carbene, and a tri-cyclo-hexyl-phosphane ligand. The complex crystallizes in a <i>C</i>-centered monoclinic unit cell and has an unusually high number of eight formula units.</p>","PeriodicalId":14692,"journal":{"name":"IUCrData","volume":"7 Pt 7","pages":"x220685"},"PeriodicalIF":0.0,"publicationDate":"2022-07-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9635413/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"40471234","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}
IUCrDataPub Date : 2022-06-24eCollection Date: 2022-06-01DOI: 10.1107/S2414314622006228
Donna Franklin, Aundrea Lee, Frank R Fronczek, Thomas Junk
{"title":"[1,4]Ditellurino[2,3-<i>b</i>:5,6-<i>b</i>']di-pyrazine.","authors":"Donna Franklin, Aundrea Lee, Frank R Fronczek, Thomas Junk","doi":"10.1107/S2414314622006228","DOIUrl":"10.1107/S2414314622006228","url":null,"abstract":"<p><p>[1,4]Ditellurino[2,3-<i>b</i>:5,6-<i>b</i>']di-pyrazine represents the first reported [1,4]chalcogena[2,3-<i>b</i>:5,6-<i>b</i>']di-pyrazine containing a heavy chalcogens The asymmetric unit consists of three mol-ecules. In contrast to its sulfur analog, which is planar [Lynch <i>et al.</i> (1994 ▸) <i>Cryst. Struct. Commun.</i> <b>50</b>,1470-1472], C<sub>8</sub>H<sub>4</sub>N<sub>4</sub>Te<sub>2</sub> is folded along the Te⋯Te axis to accommodate the larger chalcogenide atoms. The dihedral angle between the two Te<sub>2</sub>C<sub>2</sub> rings of the central ring is 57.9° (mean of three). C-Te bond lengths range from 2.1105 (16) Å to 2.1381 (17) Å, in good agreement with those predicted by their covalent radii. All Te atoms are involved in inter-molecular Te⋯N contacts, with distances in the range 2.894 (2) to 2.963 (2) Å. These result in a spiral supra-molecular assembly, forming helical columns.</p>","PeriodicalId":14692,"journal":{"name":"IUCrData","volume":"7 Pt 6","pages":"x220622"},"PeriodicalIF":0.0,"publicationDate":"2022-06-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9462040/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"40669518","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}
IUCrDataPub Date : 2022-06-24eCollection Date: 2022-06-01DOI: 10.1107/S2414314622006277
Aarón Pérez-Benítez, Jorge Luis Ariza-Ramírez, Monserrat Fortis-Valera, Rosa Elena Arroyo-Carmona, María Isabel Martínez de la Luz, Diego Ramírez-Contreras, Sylvain Bernès
{"title":"Bis{[amino-(iminium-yl)meth-yl]urea} tetra-kis-{2-[(di-methyl-amino)(iminium-yl)meth-yl]guanidine} di-μ<sub>6</sub>-oxido-tetra-μ<sub>3</sub>-oxido-tetra-deca-μ<sub>2</sub>-oxido-octa-oxidodeca-vanadium(V) tetra-hydrate.","authors":"Aarón Pérez-Benítez, Jorge Luis Ariza-Ramírez, Monserrat Fortis-Valera, Rosa Elena Arroyo-Carmona, María Isabel Martínez de la Luz, Diego Ramírez-Contreras, Sylvain Bernès","doi":"10.1107/S2414314622006277","DOIUrl":"10.1107/S2414314622006277","url":null,"abstract":"<p><p>The title compound, (C<sub>4</sub>H<sub>12</sub>N<sub>5</sub>)<sub>4</sub>(C<sub>2</sub>H<sub>7</sub>N<sub>4</sub>O)<sub>2</sub>[V<sub>10</sub>O<sub>28</sub>]·4H<sub>2</sub>O, is a by-product obtained by reacting ammonium metavanadate(V), metformin hydro-chloride and acetic acid in the presence of sodium hypochlorite, at pH = 5. The crystal structure comprises a deca-vanadate(V) anion (V<sub>10</sub>O<sub>28</sub>)<sup>6-</sup> lying on an inversion centre in space group <i>P</i> , while cations and solvent water mol-ecules are placed in general positions, surrounding the anion, and forming numerous N-H⋯O and O-H⋯O hydrogen bonds. Metforminium (C<sub>4</sub>H<sub>12</sub>N<sub>5</sub>)<sup>+</sup> and guanylurea (C<sub>2</sub>H<sub>7</sub>N<sub>4</sub>O)<sup>+</sup> cations display the expected shape. Inter-estingly, in physiology the latter cation is known to be the main metabolite of the former one. The reported structure thus supports the role of sodium hypochlorite as an oxidizing reagent being able to degrade metformin hydro-chloride to form guanylurea.</p>","PeriodicalId":14692,"journal":{"name":"IUCrData","volume":"7 Pt 6","pages":"x220627"},"PeriodicalIF":0.0,"publicationDate":"2022-06-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9462036/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"40669524","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}
IUCrDataPub Date : 2022-06-16eCollection Date: 2022-06-01DOI: 10.1107/S2414314622006186
Florian Schröder, Martin Köckerling
{"title":"Tetra-aqua-dodekakis-μ<sub>2</sub>-chlorido-di-iodido-<i>octa-hedro</i>-hexa-niobium(12 <i>Nb</i>-<i>Nb</i>) tetra-hydro-furan octa-solvate.","authors":"Florian Schröder, Martin Köckerling","doi":"10.1107/S2414314622006186","DOIUrl":"10.1107/S2414314622006186","url":null,"abstract":"<p><p>The title compound, [Nb<sub>6</sub>Cl<sub>12</sub>I<sub>2</sub>(H<sub>2</sub>O)<sub>4</sub>]·8THF (THF is tetra-hydro-furan, C<sub>4</sub>H<sub>8</sub>O), comprises an uncharged niobium cluster unit surrounded by THF solvent mol-ecules. The edges of the {Nb<sub>6</sub>} octa-hedron are <i>μ</i> <sub>2</sub>-coordinated by twelve chlorido ligands. Four in-plane (equatorial plane) aqua ligands and two iodido ligands coordinating above and below the plane are bound at the corners of the {Nb<sub>6</sub>} atomic octa-hedron. O-H⋯O hydrogen bonds are formed between the aqua ligands and the THF solvent mol-ecules; one THF molecule is disordered over two positions with the major component having a site occupancy of 0.64 (2).</p>","PeriodicalId":14692,"journal":{"name":"IUCrData","volume":"7 Pt 6","pages":"x220618"},"PeriodicalIF":0.0,"publicationDate":"2022-06-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9462034/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"40669519","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}
IUCrDataPub Date : 2022-06-10eCollection Date: 2022-06-01DOI: 10.1107/S2414314622005983
Walid Guerrab, Abderrazzak El Moutaouakil Ala Allah, Abdulsalam Alsubari, Joel T Mague, Youssef Ramli
{"title":"3-Isobutyl-5,5-di-phenyl-imidazolidine-2,4-dione.","authors":"Walid Guerrab, Abderrazzak El Moutaouakil Ala Allah, Abdulsalam Alsubari, Joel T Mague, Youssef Ramli","doi":"10.1107/S2414314622005983","DOIUrl":"10.1107/S2414314622005983","url":null,"abstract":"<p><p>The imidazolidine ring in the title mol-ecule, C<sub>19</sub>H<sub>20</sub>N<sub>2</sub>O<sub>2</sub>, is slightly 'ruffled'. In the crystal, a layer structure is generated by N-H⋯O and C-H⋯O hydrogen bonds plus C-H⋯π(ring) inter-actions.</p>","PeriodicalId":14692,"journal":{"name":"IUCrData","volume":"7 Pt 6","pages":"x220598"},"PeriodicalIF":0.0,"publicationDate":"2022-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9462038/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"40669523","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}
IUCrDataPub Date : 2022-06-10eCollection Date: 2022-06-01DOI: 10.1107/S2414314622006071
Peter W R Corfield
{"title":"<i>trans</i>-Carbonyl-chlorido-bis-(tri-ethyl-phosphane-κ<i>P</i>)platinum(II) tetra-fluorido-borate.","authors":"Peter W R Corfield","doi":"10.1107/S2414314622006071","DOIUrl":"10.1107/S2414314622006071","url":null,"abstract":"<p><p>The chemical formulation of the title compound was established as <i>trans</i>-[PtCl{P(C<sub>2</sub>H<sub>5</sub>)<sub>3</sub>(CO)}BF<sub>4</sub> by single-crystal X-ray analysis, in contrast to the five-coordinate tetra-fluoro-ethyl-ene complex that had been anti-cipated. The compound had been prepared by reaction of <i>trans</i>-PtHCl(P(C<sub>2</sub>H<sub>5</sub>)<sub>3</sub>)<sub>2</sub> with C<sub>2</sub>F<sub>4</sub> in the absence of air, and the presence of the carbonyl group was not suspected. The square-planar cations and BF<sub>4</sub> <sup>-</sup> anions are linked by C-H⋯F and C-H⋯O inter-actions into thick wavy (010) sheets. The present crystal-structure refinement is based on the original intensity data recorded in 1967.</p>","PeriodicalId":14692,"journal":{"name":"IUCrData","volume":"7 Pt 6","pages":"x220607"},"PeriodicalIF":0.0,"publicationDate":"2022-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9462037/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"40669521","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}