X-ray Structure Analysis Online最新文献

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Crystal Structure of a Lantern-type Dirhodium(II) Complex with Axial Pyridine Molecules cis-[Rh2(4-Me-pf )2(O2CCMe3)2(py)2], 4-Me-pf− = N,N′-Di-p-tolylformamidinate Anion Lantern型铱(II)与吡啶轴分子顺式-[Rh2(4-Me-pf)配合物的晶体结构 )2(O2CCMe3)2(py)2],4-Me-pf−=N,N′-二对甲苯磺酰亚胺阴离子
IF 0.2
X-ray Structure Analysis Online Pub Date : 2021-11-10 DOI: 10.2116/xraystruct.37.69
M. Handa, Makoto Kano, Natsumi Yano, M. Mikuriya, Y. Kataoka
{"title":"Crystal Structure of a Lantern-type Dirhodium(II) Complex with Axial Pyridine Molecules cis-[Rh2(4-Me-pf )2(O2CCMe3)2(py)2], 4-Me-pf− = N,N′-Di-p-tolylformamidinate Anion","authors":"M. Handa, Makoto Kano, Natsumi Yano, M. Mikuriya, Y. Kataoka","doi":"10.2116/xraystruct.37.69","DOIUrl":"https://doi.org/10.2116/xraystruct.37.69","url":null,"abstract":"The complexes [M2(O2CR)4] (m = 0 – 2), in which two transition metal ions are bridged with four μ-carboxylato bidentate ligands, are called lantern-type (or paddlewheel type) diuclear complexes from the view point of their molecular structures.1 The axial sites of the dinuclear complexes are coordinated by linkage ligands, such as pyrazine, to produce the assembled polymer complexes. The polymer complexes have been attracting many chemists concerning their interesting properties. For instance, nitrogen gas occulusion properties have been found for polymer complexes [Cu2(O2CPh)4(pyz)]n and [Rh2(O2CPh)4(pyz)]n. N,N′-Diarylformamidinato ions (R-pf–) also work as bidentate ligands for metal ions to give lantern-type dinuclear complexes. We have reported on the polymer complexes [Rh2(4-Me-pf )4(1,4-dib)]n (4-Me-pf– = N,N′-di-p-tolylformamidinate anion; 1,4-dib = 1,4-diisocyanobenzene) and cis-[Rh2(4-Me-pf )2(O2CR)2(L)]n (R = CF3 and CMe3; L = pyz and 4,4′-bipyridine (4,4′-bpy)).4,5 We also reported on the bis-adduct complexes 4-phenylpyridine (4-phpy) cis-[Rh2(4-Me-pf )2(O2CR)4(4-phpy)2] (R = CF3 and CMe3) and cis-[Rh2(4-Me-pf )2(O2CCMe3)2(4-phpy)2]BF4. A pyridine adduct complex, cis-[Rh2(4-Me-pf )2(O2CCF3)4(py)2], has been synthesized, but not reported concerning its crystal structure.6 In this report, we here report on the synthesis and crystal structure of cis-[Rh2(4-Me-pf )2(O2CCMe3)4(py)2] (1). The chemical structure of the title compound 1 is depicted in Fig. 1. The starting material, cis-[Rh2(4-Me-pf )2(O2CCMe3)2], was prepared according to a method described in the literature.7 To a solution of cis-[Rh2(4-Me-pf )2(O2CCMe3)2] (96.0 mg (0.11 mmol) in chloroform (5.0 mL) and methanol (15.0 mL) was added pyridine (1.0 mL), and the mixture was stirred for 3 h at room temperature. To the resultant solution was added water (1.0 mL), and the reaction mixture was evaporatd to ca. 3 mL. The evapotated solution was left at room temperature until red microcrystals were deposited. The deposited microcrytals were collected by suction, washed with a small portion of water, and dried over P2O5 in a vaccum desicater for 3 h. The yield was 76.3 mg (68.2% base on cis-[Rh2(4-Mepf )2(O2CCMe3)2]). Anal. Found: C, 59.12; H, 5.34; N, 8.26. Calcd for C50H58N6O4Rh2: C, 59.29; H, 5.77; N, 8.30%. IR (KBr, cm–1): 2983 w, 2917 w, 2859 w (CH), 1622 s, 1592 s (Ar), 1504 s, 1480 m, 1412 s, 1333 m (COO), 1222 s (Ar). X-ray quality crystals of 1 were obtained by recrystallization from dichlroromethane solution with several drops of pyridine. X-ray crystallographic data (Table 1) were collected for a single crystal of 1 at 150 K on a RIGAKU HyPix6000 CCD system equipped with a Mo rotating-anode X-ray generator (λ = 2021 © The Japan Society for Analytical Chemistry","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-11-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47188912","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}
引用次数: 0
Crystal Structure and Hirshfeld Surface Analysis of 1-(4-Chlorophenyl)-5-{4-[(2-methylphenyl)methoxy]phenyl}-1H-Pyrazole 1-(4-氯苯基)-5-{4-[(2-甲基苯基)甲氧基]苯基}- 1h -吡唑的晶体结构和Hirshfeld表面分析
IF 0.2
X-ray Structure Analysis Online Pub Date : 2021-11-10 DOI: 10.2116/xraystruct.37.77
A. Aydın, M. Akkurt, Sümeyye Turanlı, E. Banoglu, N. Ozcelik
{"title":"Crystal Structure and Hirshfeld Surface Analysis of 1-(4-Chlorophenyl)-5-{4-[(2-methylphenyl)methoxy]phenyl}-1H-Pyrazole","authors":"A. Aydın, M. Akkurt, Sümeyye Turanlı, E. Banoglu, N. Ozcelik","doi":"10.2116/xraystruct.37.77","DOIUrl":"https://doi.org/10.2116/xraystruct.37.77","url":null,"abstract":"The aim of the study is to explore the crystal structure and performe Hirshfeld surface analysis of 1-(4-chlorophenyl)-5-{4-[(2-methylphenyl)methoxy]phenyl}-1 H -pyrazole. In the title compound, C 23 H 19 ClN 2 O, the 4-chlorophenyl, 2-methylphenyl and benzene rings are oriented with dihedral angles of 71.22(10), 31.82(9) and 59.76(9) ° , respectively, with respect to the pyrazole ring. Pairs of molecules are linked by intermolecular C–H···O hydrogen contacts with R 2 2 (8) ring motifs forming sheets lying parallel to (100). Furthermore C–H··· π interactions also contribute to stabilizing the molecular packing. A Hirshfeld surface analysis has been used to confirm and quantify the supramolecular interactions which indicate that the most important contributions for the crystal packing are from H···H (42.5%) and H···C/C···H (35%) and H···Cl/Cl···H (12%) interactions.","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-11-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47281863","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}
引用次数: 1
Dinuclear Praseodymium(III) Complex with N,N′-Bis(2-hydroxy-3,5-dimethylbenzyl)-N,N′-dimethyl-1,2-ethanediamine 双核镨(III)配合物N,N ' -双(2-羟基-3,5-二甲基苄基)-N,N ' -二甲基-1,2-乙二胺
IF 0.2
X-ray Structure Analysis Online Pub Date : 2021-11-10 DOI: 10.2116/xraystruct.37.73
M. Mikuriya, Chika Kawai, Kana Nagai, Akiko Morita, Asuka Kanemori, D. Yoshioka, M. Tsuboi
{"title":"Dinuclear Praseodymium(III) Complex with N,N′-Bis(2-hydroxy-3,5-dimethylbenzyl)-N,N′-dimethyl-1,2-ethanediamine","authors":"M. Mikuriya, Chika Kawai, Kana Nagai, Akiko Morita, Asuka Kanemori, D. Yoshioka, M. Tsuboi","doi":"10.2116/xraystruct.37.73","DOIUrl":"https://doi.org/10.2116/xraystruct.37.73","url":null,"abstract":"N,N′-Bis(2-hydroxy-3,5-dimethylbenzyl)-N,N′-dimethyl-1,2ethanediamine (H2hdde) is a tetradentate N2O2 ligand similar to the famous tetradentate Schiff-base, N,N′-ethylenebis(salicylideneimine), H2salen, but with two saturated C–N bonds, being different from the H2salen ligand.1 So far, mononuclear vanadium,2 manganese,3 iron,4 and molybdenum5 complexes, dinuclear vanadium,2 dinuclear iron,6 trinuclear manganese,3,7 tetranuclear manganese,3 tetranuclear zinc,8 tetranuclear cadmium,8 tetranuclear nickel,9 hexanuclear nickel,9 and heptanuclear nickel10 complexes were reported concerning the H2hdde ligand. In our laboratory, we have aimed to extend the coordination chemistry of this ligand to the rare-earth elements. In this study, we successfully synthesized a praseodymium complex with hdde2– and determined the crystal structure in order to elucidate the dinuclear molecule (Fig. 1). The ligand H2hdde was synthesized by a method described in the literature.11 The complex was prepared by a reaction of H2hdde and praseodymium(III) salt. To a methanol solution (5 cm3) of H2hdde (53.9 mg, 0.15 mmol) was added 35.9 mg (0.1 mmol) of praseodymium(III) acetate dihydrate, and then six drops of triethylamine were added into the reaction mixture to obtain a pale-green precipitate. The precipitate was collected and dried under a vacuum. Yield, 51.2 mg (84.6%). Anal. Found: C, 49.21; H, 6.35; N, 4.25%. Calcd for C50H78N4O12Pr2[Pr2(hdde)2(CH3COO)2(CH3OH)2]·2H2O: C, 49.67; H, 6.50; N, 4.63%. IR (KBr, cm–1): 3320 ν(OH), 2980 νas(CH3), 2916 νas(CH2), 2854 νs(CH3), 2808 νs(CH2), 1556 νas(COO), 1476 δ(CH3), 1425 νs(COO). X-ray quality crystals were grown by recrystallization from methanol–dichloromethane. X-ray diffraction data were collected on a Bruker CCD X-ray diffractometer (SMART APEX) using graphite-monochromated Mo-Kα radiation. Crystal data and details concerning the data collection are given in Table 1. The structure was solved by an intrinsic phasing method and refined by full-matrix least-squares methods. The hydrogen atoms were inserted at their calculated positions, and fixed there, except for the hydrogen atom attached to the O5 atom of the coordinated methanol molecule, which was located from a D-Fourier map. All of the calculations were carried out on a Windows 7 Core i5 computer utilizing the SHELXT-201412 and SHELXL-2014.13 Crystallographic data have been deposited with Cambridge Crystallographic Data Centre (Deposit number CCDC-2091175). Copies of the data can be obtained free of charge via http://www.ccdc.cam.ac.uk/conts/ retrieving.html (or from the Cambridge Crystallographic Data Centre, 12, Union Road, Cambridge, CB2 1EZ, UK; Fax, +44 1223 336033; e-mail, deposit@ccdc.cam.ac.uk). A single-crystal X-ray structure analysis revealed that the molecule is a centrosymmetric dinuclear praseodymium complex. The asymmetric unit consists of one half of a [Pr2(hdde)2(CH3COO)2(CH3OH)2] complex and one dichloromethane molecule. The molecular structure, drawn","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-11-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43762778","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}
引用次数: 0
Frontmatter
IF 0.2
X-ray Structure Analysis Online Pub Date : 2021-11-08 DOI: 10.1515/9783110610833-fm
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引用次数: 0
9 Qualitative and quantitative evaluation of powder patterns 粉末图案的定性和定量评价
IF 0.2
X-ray Structure Analysis Online Pub Date : 2021-11-08 DOI: 10.1515/9783110610833-009
{"title":"9 Qualitative and quantitative evaluation of powder patterns","authors":"","doi":"10.1515/9783110610833-009","DOIUrl":"https://doi.org/10.1515/9783110610833-009","url":null,"abstract":"","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-11-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"72371781","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}
引用次数: 0
8 Powder diffraction methods 8粉末衍射法
IF 0.2
X-ray Structure Analysis Online Pub Date : 2021-11-08 DOI: 10.1515/9783110610833-008
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引用次数: 0
Index 指数
IF 0.2
X-ray Structure Analysis Online Pub Date : 2021-11-08 DOI: 10.1515/9783110610833-012
{"title":"Index","authors":"","doi":"10.1515/9783110610833-012","DOIUrl":"https://doi.org/10.1515/9783110610833-012","url":null,"abstract":"","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-11-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77339425","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}
引用次数: 0
3 Waves 3波
IF 0.2
X-ray Structure Analysis Online Pub Date : 2021-11-08 DOI: 10.1515/9783110610833-003
{"title":"3 Waves","authors":"","doi":"10.1515/9783110610833-003","DOIUrl":"https://doi.org/10.1515/9783110610833-003","url":null,"abstract":"","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-11-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76576416","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}
引用次数: 0
7 Single crystal methods 7单晶法
IF 0.2
X-ray Structure Analysis Online Pub Date : 2021-11-08 DOI: 10.1515/9783110610833-007
{"title":"7 Single crystal methods","authors":"","doi":"10.1515/9783110610833-007","DOIUrl":"https://doi.org/10.1515/9783110610833-007","url":null,"abstract":"","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-11-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"72964134","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}
引用次数: 0
6 X-ray physics 6 x射线物理学
IF 0.2
X-ray Structure Analysis Online Pub Date : 2021-11-08 DOI: 10.1515/9783110610833-006
{"title":"6 X-ray physics","authors":"","doi":"10.1515/9783110610833-006","DOIUrl":"https://doi.org/10.1515/9783110610833-006","url":null,"abstract":"","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-11-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86738419","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}
引用次数: 0
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