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2-Azido-N-(4-methyl-phen-yl)acetamide. 2-叠氮-N-(4-甲基苯基)乙酰胺。
Pub Date : 2022-07-29 eCollection Date: 2022-07-01 DOI: 10.1107/S2414314622006216
Mohcine Missioui, Walid Guerrab, Abdulsalam Alsubari, Joel T Mague, Youssef Ramli

The asymmetric unit of the title compound, C9H10N4O, 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 c-axis direction.

标题化合物 C9H10N4O 的不对称单元由三个独立的分子单元组成,其中两对分子单元在叠氮基团的旋转方向上存在显著差异,而一对分子单元则具有非常相似的构象;N-N-C-C 扭转角分别为 -173.9 (2)、-102.7 (2) 和 -173.6 (2)°。在晶体中,每个独立的分子单元与其滑行面相关的对应物形成 N-H⋯O 氢键,形成沿 c 轴方向延伸的人字形链。
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引用次数: 0
Rerefinement of the crystal structure of SnTe0.73(2)Se0.27(2) from single-crystal X-ray diffraction data. 根据单晶 X 射线衍射数据重新确定 SnTe0.73(2)Se0.27(2)的晶体结构。
Pub Date : 2022-07-19 eCollection Date: 2022-07-01 DOI: 10.1107/S2414314622007295
Silvana Moris, Antonio Galdámez

Compounds of the solid solution series SnTe1-x Se x , derived from pristine SnSe and SnTe, are considered as thermoelectric lead-free materials. The crystal structure re-refinement of NaCl-type SnTe0.73 (2)Se0.27 (2) 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 ▸). Z. Anorg. Allg. Chem. 334, 37-49].

固溶体系列 SnTe1-x Se x 化合物,源自原始 SnSe 和 SnTe,被认为是热电无铅材料。根据单晶 X 射线衍射数据,对 NaCl 型 SnTe0.73 (2)Se0.27 (2) 的晶体结构进行了再细化,与之前基于粉末 X 射线数据的报告[Krebs & Langner (1964 ▸)。 Z. Anorg. Allg. Chem. 334, 37-49]相比,其键长[Sn-(Te,Se)=3.0798 (3) Å]的精度更高。
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引用次数: 0
Crystal structure of ethyl 2-{4-[(2-oxo-3-phenyl-1,2-di-hydro-quinoxalin-1-yl)meth-yl]-1H-1,2,3-triazol-1-yl}acetate. 2-{4-[(2-oxo-3-phenyl-1,2-di-hydro-quinoxalin-1-yl)meth-yl]-1H-1,2,3-triazol-1-yl} 乙酸乙酯的晶体结构。
Pub Date : 2022-07-14 eCollection Date: 2022-07-01 DOI: 10.1107/S2414314622006939
Nadeem Abad, Mohcine Missioui, Abdulsalam Alsubari, Joel T Mague, El Mokhtar Essassi, Youssef Ramli

The quinoxaline portion of the title mol-ecule, C21H19N5O3, 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.

标题分子单元 C21H19N5O3 中的喹喔啉部分并不完全是平面的,组成环之间的二面角为 3.38 (7)°。该分子单元呈 "U "形,通过分子内反平行的羰基静电相互作用(C--O 间距分别为 2.8905 (16) Å 和 3.0221 (15) Å),在晶体中通过 C-H⋯O 和 C-H⋯N 氢键以及 C-H⋯π (环) 和 π-stacking 相互作用形成波纹层。
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引用次数: 0
Natural djurleite with refined composition Cu61.39S32 revealing disorder of some Cu sites. 天然榴辉石的精制成分 Cu61.39S32 揭示了某些铜位点的无序性。
Pub Date : 2022-07-12 eCollection Date: 2022-07-01 DOI: 10.1107/S2414314622006940
Yawei Zhou, Changzeng Fan, Bin Wen, Lifeng Zhang

A djurleite crystal was discovered from a natural sample originally labelled as chalcocite. The djurleite crystal under investigation has a refined composition of Cu61.39S32, thus revealing a Cu deficiency compared to the originally reported Cu62S32 phase [Evans (1979). Z. Kristallogr. 150, 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.

从一个最初被标记为白云母的天然样本中发现了一个榴辉石晶体。与最初报道的 Cu62S32 相相比[Evans (1979). Z. Kristallogr. 150, 299-320],正在研究的榴辉石晶体的细化成分为 Cu61.39S32,从而显示了铜的缺乏,据报道,Cu62S32 相中的所有原子位点都被完全占据。此外,目前的细化结果显示有八个铜位点分裂成对。
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引用次数: 0
[(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-κP)iridium(I) tetra-fluorido-borate di-chloro-methane monosolvate. [(1,2,5,6-η)-环辛烷-1,5-二烯](4-异丙基-1-甲基-1,2,4-三唑-5-基-亚烯)(三环己基磷烷-κP)铱(I)四氟硼酸二氯甲烷单溶液。
Pub Date : 2022-07-08 eCollection Date: 2022-07-01 DOI: 10.1107/S241431462200685X
Joshua Rushlow, Andrei V Astashkin, Daniel R Albert, Edward Rajaseelan

The title compound, [Ir(C8H12)(C6H11N3)(C18H33P)]BF4·CH2Cl2, 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 IrI 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 C-centered monoclinic unit cell and has an unusually high number of eight formula units.

标题化合物[Ir(C8H12)(C6H11N3)(C18H33P)]BF4-CH2Cl2 是一种基于三唑的 N-杂环碳化铱(I)阳离子络合物,带有一个四氟硼酸对位离子,每个式单元结晶出一个二氯甲烷溶剂分子。阳离子络合物中的 IrI 原子具有扭曲的方形平面配位环境,该环境由双齿环辛烷-1,5-二烯(COD)配体、N-杂环碳烯和三环己基膦烷配体确定。该复合物结晶于一个以 C 为中心的单斜晶胞中,并具有非常多的 8 个配方单元。
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引用次数: 0
[1,4]Ditellurino[2,3-b:5,6-b']di-pyrazine. [1,4]Ditellurino[2,3-b:5,6-b']di-pyrazine.
Pub Date : 2022-06-24 eCollection Date: 2022-06-01 DOI: 10.1107/S2414314622006228
Donna Franklin, Aundrea Lee, Frank R Fronczek, Thomas Junk

[1,4]Ditellurino[2,3-b:5,6-b']di-pyrazine represents the first reported [1,4]chalcogena[2,3-b:5,6-b']di-pyrazine containing a heavy chalcogens The asymmetric unit consists of three mol-ecules. In contrast to its sulfur analog, which is planar [Lynch et al. (1994 ▸) Cryst. Struct. Commun. 50,1470-1472], C8H4N4Te2 is folded along the Te⋯Te axis to accommodate the larger chalcogenide atoms. The dihedral angle between the two Te2C2 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.

[1,4]Ditellurino[2,3-b:5,6-b']di-pyrazine 是首次报道的含有重金 属的 [1,4]chalcogena[2,3-b:5,6-b']di-pyrazine 不对称单元由三个分子组成。C8H4N4Te2 的硫类似物是平面的[Lynch 等人 (1994 ▸) Cryst. Struct.中心环的两个 Te2C2 环之间的二面角为 57.9°(三个的平均值)。C-Te 键长度从 2.1105 (16) Å 到 2.1381 (17) Å 不等,与它们的共价半径预测值十分吻合。所有 Te 原子都参与了分子间 Te⋯N 接触,其距离范围为 2.894 (2) Å 至 2.963 (2) Å。这些接触形成了螺旋状的超分子组装,形成螺旋柱。
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引用次数: 0
Bis{[amino-(iminium-yl)meth-yl]urea} tetra-kis-{2-[(di-methyl-amino)(iminium-yl)meth-yl]guanidine} di-μ6-oxido-tetra-μ3-oxido-tetra-deca-μ2-oxido-octa-oxidodeca-vanadium(V) tetra-hydrate. 双{[氨基-(亚氨基基)甲基]脲}四-{2-[(二甲基氨基)(亚氨基)甲基]胍}二-μ6-氧化-四-μ3-氧化-四-D-μ2-氧化-八-氧化-钒(V)四水合物。
Pub Date : 2022-06-24 eCollection Date: 2022-06-01 DOI: 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

The title compound, (C4H12N5)4(C2H7N4O)2[V10O28]·4H2O, 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 (V10O28)6- lying on an inversion centre in space group P , 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 (C4H12N5)+ and guanylurea (C2H7N4O)+ 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.

标题化合物(C4H12N5)4(C2H7N4O)2[V10O28]-4H2O 是一种副产品,由偏钒酸铵(V)、氢氯二甲双胍和醋酸在 pH = 5 的次氯酸钠存在下反应生成。晶体结构包括一个位于 P 空间群反转中心的十-钒酸盐(V)阴离子(V10O28)6-,而阳离子和溶剂水分子则位于阴离子周围的一般位置,并形成许多 N-H⋯O 和 O-H⋯O 氢键。二甲双胍 (C4H12N5)+ 和鸟苷酸 (C2H7N4O)+ 阳离子显示出预期的形状。在生理学中,后一种阳离子是前一种阳离子的主要代谢产物。因此,所报告的结构支持次氯酸钠作为氧化试剂,能够降解二甲双胍氢氯化物,生成鸟苷酸。
{"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}
引用次数: 0
Tetra-aqua-dodekakis-μ2-chlorido-di-iodido-octa-hedro-hexa-niobium(12 Nb-Nb) tetra-hydro-furan octa-solvate. Tetra-aqua-dodekakis-μ2-chlorido-di-iodido-octa-hedro-hexa-niobium(12 Nb-Nb) tetra-hydro-furan octa-solvate。
Pub Date : 2022-06-16 eCollection Date: 2022-06-01 DOI: 10.1107/S2414314622006186
Florian Schröder, Martin Köckerling

The title compound, [Nb6Cl12I2(H2O)4]·8THF (THF is tetra-hydro-furan, C4H8O), comprises an uncharged niobium cluster unit surrounded by THF solvent mol-ecules. The edges of the {Nb6} octa-hedron are μ 2-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 {Nb6} 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).

标题化合物[Nb6Cl12I2(H2O)4]-8THF(THF 指四氢呋喃,C4H8O)由一个不带电的铌簇单元组成,周围环绕着 THF 溶剂分子。{Nb6}八面体的边缘由十二个氯配体配位。在{Nb6}原子八面体的四角结合了四个平面内(赤道面)水配位体和两个在平面上下配位的碘配位体。水配体和四氢呋喃溶剂分子之间形成 O-H⋯O 氢键;一个四氢呋喃分子在两个位置上无序排列,主要成分的位点占有率为 0.64 (2)。
{"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}
引用次数: 0
3-Isobutyl-5,5-di-phenyl-imidazolidine-2,4-dione. 3-异丁基-5,5-二苯基-咪唑烷-2,4-二酮。
Pub Date : 2022-06-10 eCollection Date: 2022-06-01 DOI: 10.1107/S2414314622005983
Walid Guerrab, Abderrazzak El Moutaouakil Ala Allah, Abdulsalam Alsubari, Joel T Mague, Youssef Ramli

The imidazolidine ring in the title mol-ecule, C19H20N2O2, 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.

标题分子 C19H20N2O2 中的咪唑烷环略有 "皱褶"。在晶体中,N-H⋯O 和 C-H⋯O 氢键加上 C-H⋯π(环)相互作用产生了层状结构。
{"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}
引用次数: 0
trans-Carbonyl-chlorido-bis-(tri-ethyl-phosphane-κP)platinum(II) tetra-fluorido-borate. 反式-羰基-氯基-双-(三乙基膦-κP)四氟硼酸铂(II)。
Pub Date : 2022-06-10 eCollection Date: 2022-06-01 DOI: 10.1107/S2414314622006071
Peter W R Corfield

The chemical formulation of the title compound was established as trans-[PtCl{P(C2H5)3(CO)}BF4 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 trans-PtHCl(P(C2H5)3)2 with C2F4 in the absence of air, and the presence of the carbonyl group was not suspected. The square-planar cations and BF4 - 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.

通过单晶 X 射线分析,确定了标题化合物的化学式为反式-[PtCl{P(C2H5)3(CO)}BF4,这与已反萃的五配位四氟乙烯络合物不同。该化合物是通过反式铂氢(P(C2H5)3)2 与 C2F4 在无空气条件下反应制备的,没有怀疑羰基的存在。方形平面阳离子和 BF4 - 阴离子通过 C-H⋯F 和 C-H⋯O 相互作用连接成厚的波浪状 (010) 薄片。目前的晶体结构改进是基于 1967 年记录的原始强度数据。
{"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}
引用次数: 0
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