X-ray Structure Analysis Online最新文献

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Dinuclear Manganese(III) Complex with a Schiff-base Having a Di-μ-acetato-μ-alkoxido-bridged Core 双核锰(III)与具有二-μ-乙酰基-μ-烷氧基桥联核的席夫碱配合物
IF 0.2
X-ray Structure Analysis Online Pub Date : 2020-03-10 DOI: 10.2116/xraystruct.36.7
M. Mikuriya, Yoshiki Koyama, D. Yoshioka, R. Mitsuhashi
{"title":"Dinuclear Manganese(III) Complex with a Schiff-base Having a Di-μ-acetato-μ-alkoxido-bridged Core","authors":"M. Mikuriya, Yoshiki Koyama, D. Yoshioka, R. Mitsuhashi","doi":"10.2116/xraystruct.36.7","DOIUrl":"https://doi.org/10.2116/xraystruct.36.7","url":null,"abstract":"The chemistry of mononuclear, dinuclear, and tetranuclear manganese complexes with organic ligands is interesting, having relevance to some active centers in biological systems, such as superoxide dismutase, catalase, and the oxygen-evolving complex (OEC) of photosystem II (PSII) in green plants.1 So far, mononuclear, dinuclear, tetranuclear, and polynuclear manganese complexes with dinucleating Schiff-base ligands having a bridging alkoxido-oxygen, 1,3-bis(salicylideneamino)2-propanol (H3sap) and its substituent derivatives, have appeared in the literature.2–8 In this study, we isolated a new dinuclear manganese complex with 1,3-bis(3-methoxysalicylideneamino)2-propanol (H3msap) and determined the crystal structure, which shows a dinuclear core with one alkoxido-oxygen and two-μ-acetato bridges, as shown in Fig. 1. This paper describes the synthesis, crystal structure and electronic spectra of [Mn2(msap)(μ-CH3COO)2(CH3COO)(CH3OH)] (1). The ligand H3msap was synthesized by a method described in the literature.7 The complex was prepared by a 1:2 reaction of H3msap and manganese(II) salt. To an acetonitrile solution (2 cm3) of H3msap (18.0 mg, 0.05 mmol) was added an absolute methanol solution (1 cm3) of 24.9 mg (0.1 mmol) of manganese(II) acetate tetrahydrate, and then three drops of 2020 © The Japan Society for Analytical Chemistry","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2020-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44121944","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: 3
Preparation and Crystal Structure of Sodium Tetraperoxidochromate(V) 四氧化铬酸钠(V)的制备及其晶体结构
IF 0.2
X-ray Structure Analysis Online Pub Date : 2020-02-10 DOI: 10.2116/xraystruct.36.3
M. Mikuriya, Shuichi Hiroshima, Yoshiki Koyama, Keisuke Terada, D. Yoshioka, R. Mitsuhashi
{"title":"Preparation and Crystal Structure of Sodium Tetraperoxidochromate(V)","authors":"M. Mikuriya, Shuichi Hiroshima, Yoshiki Koyama, Keisuke Terada, D. Yoshioka, R. Mitsuhashi","doi":"10.2116/xraystruct.36.3","DOIUrl":"https://doi.org/10.2116/xraystruct.36.3","url":null,"abstract":"","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2020-02-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46343879","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 of S8 Molecule from Thiourea 硫脲S8分子的晶体结构
IF 0.2
X-ray Structure Analysis Online Pub Date : 2020-01-10 DOI: 10.2116/xraystruct.36.1
M. Mikuriya, K. Taniguchi, Yoshiki Koyama, Hiroaki Watanabe, D. Yoshioka, R. Mitsuhashi, E. Asato
{"title":"Crystal Structure of S8 Molecule from Thiourea","authors":"M. Mikuriya, K. Taniguchi, Yoshiki Koyama, Hiroaki Watanabe, D. Yoshioka, R. Mitsuhashi, E. Asato","doi":"10.2116/xraystruct.36.1","DOIUrl":"https://doi.org/10.2116/xraystruct.36.1","url":null,"abstract":"Thiourea is an interesting ligand for metal complexes, which have attracted much attention of many researchers as potential applications from optical devices to cancer-treatment reagents.1 Such thiourea-based metal complexes have also been employed as precursors in preparing metal sulfide materials.2 For example, bismuth sulfide obtained from thiourea complexes is known to be as an important semiconductor.3 The formation of thiourea complexes of bismuth is used for the qualitative analysis of bismuth in undergraduate inorganic-chemistry courses.4 In the course of our study on bismuth complexes with thiourea, we isolated crystals of the S8 molecule instead of the bismuth complex, and determined the crystal structure (Fig. 1). Thiourea (229 mg, 3.0 mmol) and bismuth nitrate pentahydrate (242 mg, 0.5 mmol) were dissolved in N,N-dimethylformamide (8 cm3). The solution was left at room temperature for several days. The resulting pale-yellow crystals were filtered off. Yield, 17.2 mg (17.9%). A preliminary examination was made, and 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 integrated and scaled data were empirically corrected with TWINABS.5 The structure was solved as a 2-component twin with the only non-overlapping reflections of component 1 and refined using the hklf 5 routine with all reflections of component 1 (including the overlapping ones). Crystallographic data have been deposited with Cambridge Crystallographic Data Centre (Deposit number CCDC-1947735). Copies of the data can be obtained free of charge via http://www.ccdc.cam.ac.uk/conts/ 2020 © The Japan Society for Analytical Chemistry","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2020-01-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.2116/xraystruct.36.1","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41379115","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: 5
Crystal Structure of Dinaphtho[2,1,1′,2′]furan Picrate 二萘并[2,1′,2′]呋喃Picrate的晶体结构
IF 0.2
X-ray Structure Analysis Online Pub Date : 2019-12-10 DOI: 10.2116/xraystruct.35.69
Risa Honda, A. Tanaka, K. Hirabayashi, K. Akiyama, Toshio Shimizu, K. Sugiura
{"title":"Crystal Structure of Dinaphtho[2,1,1′,2′]furan Picrate","authors":"Risa Honda, A. Tanaka, K. Hirabayashi, K. Akiyama, Toshio Shimizu, K. Sugiura","doi":"10.2116/xraystruct.35.69","DOIUrl":"https://doi.org/10.2116/xraystruct.35.69","url":null,"abstract":"Dinaphtho[2,1,1′,2′]furan (DNF, 1) is well characterized as a heteroatom helicene,1 i.e., an analogue of [5]helicene replacing one double bond with isoelectronic ether oxygen.2 Owing to the expanded π-system of DNF, DNF as an advanced material has been applied in various devices, such as field-effect transistors3 and light-emitting devices.4 One of the unique applications of DNF is as a precursor of Buchiwild-type monodentate optically active phosphine (MOP) ligands.5 Furthermore, Tsubaki synthesized the highly conjugated fan-shaped oligonaphthofurans using the DNF unit.6 In the beginning of the last century from the 1900s to the 1930s, the structure of DNF was confused with that of binapthyl 3.1,7 At that time, the two compounds were distinguished solely based on the formation of picrate, i.e., DNF 1 produces a red charge transfer complex with picric acid 2 (vide infra) and 3 is not formed. Because of the many applications of DNF currently, especially in electronic devices mentioned above, the structure of a DNF-based charge-transfer complex should be determined. In this study, we synthesized the DNF picrate and characterized it by spectroscopic studies. Bulk samples for spectroscopic and differential scanning calorimetry (DSC) studies were harvested from a hot EtOH solution (20 mL) of 1 (20 mg) and 2 (57 mg, Wako Pure Chemical Industries, Ltd.) to obtain red picrate. A single crystal suitable for X-ray diffraction analysis was obtained from a diluted EtOH solution evaporated slowly to give red plates. The following results were obtained: melting points (MPs): 161.4°C 2019 © The Japan Society for Analytical Chemistry","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-12-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48679441","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
Crystal Structure of a Mononuclear Iron(II) Complex, Tris(1,10-phenanthroline-κ2N,N′)iron(II) Bis(hexafluoridophosphate) 单核铁(II)配合物,三(1,10-菲咯啉-κ2N,N′)铁(Ⅱ)双(六氟磷酸盐)的晶体结构
IF 0.2
X-ray Structure Analysis Online Pub Date : 2019-11-10 DOI: 10.2116/xraystruct.35.67
Ryusei Hoshikawa, R. Mitsuhashi, M. Mikuriya, H. Sakiyama
{"title":"Crystal Structure of a Mononuclear Iron(II) Complex, Tris(1,10-phenanthroline-κ2N,N′)iron(II) Bis(hexafluoridophosphate)","authors":"Ryusei Hoshikawa, R. Mitsuhashi, M. Mikuriya, H. Sakiyama","doi":"10.2116/xraystruct.35.67","DOIUrl":"https://doi.org/10.2116/xraystruct.35.67","url":null,"abstract":"included in Table 1. The structure was solved by intrinsic phasing methods and expanded using Fourier techniques. The non-hydrogen atoms were refined anisotropically, and hydrogen atoms were refined using the riding model. The final cycle of a full-matrix least-squares refinement on F 2 was allowed to satisfactory converge with mononuclear iron(II) complex, [Fe(phen) ][PF was synthesized, and characterized by a single-crystal X-ray method. The compound crystallized in the monoclinic space group C 2/ c and Z = 8 with cell parameters a = 36.529(4)Å, b = 15.8597(16)Å, c = 11.7747(12)Å, β = 100.528(2) ° , V = 6706.7(12)Å 3 . The R 1 [ I > 2 σ ( I )] and wR 2 (all data) values were 0.0631 and 0.1787, respectively, for all 8068 independent reflections. Despite the symmetrical tris(1,10-phenanthroline) environment, the symmetry around the iron(II)","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-11-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48134926","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
Cocrystal Structure of the Redox-active Phenylenediamine and Quinonediimine Derivatives 氧化还原活性苯二胺和醌二亚胺衍生物的共晶结构
IF 0.2
X-ray Structure Analysis Online Pub Date : 2019-11-10 DOI: 10.2116/xraystruct.35.63
S. Ohmura, T. Hirao, N. Miyoshi, T. Moriuchi
{"title":"Cocrystal Structure of the Redox-active Phenylenediamine and Quinonediimine Derivatives","authors":"S. Ohmura, T. Hirao, N. Miyoshi, T. Moriuchi","doi":"10.2116/xraystruct.35.63","DOIUrl":"https://doi.org/10.2116/xraystruct.35.63","url":null,"abstract":"The cocrystal structure of diethyl 2,5-bis{[4-(ethoxycarbonyl)phenyl]amino}terephthalate (PDA) and diethyl (3E,6E)-3,6-bis{[4-(ethoxycarbonyl)phenyl]amino}cyclohexa-1,4-diene-1,4-dicarboxylate (QDI) was determined by X-ray crystallography. The compound crystallizes in a triclinic system and was characterized thus: P-1, a = 8.6778(3)A, b =13.0702(4)A, c = 13.5152(4)A, α = 79.1570(15)°, β = 71.8459(15)°, γ = 72.5962(16)°, Z = 1, V = 1382.28(7)A3. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.078 and 0.190, respectively, for all 4179 independent reflections. In the crystal, a polymeric alternating arrangement of PDA and QDI exists through a network of π-π interactions, wherein both components adopt an anti-conformation of the π-conjugated backbones.","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-11-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.2116/xraystruct.35.63","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46950719","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
Crystal Structure of μ-Phenoxo-μ-benzoate-bridged Dinuclear Fe(II) Complex with a Dinucleating Ligand Having a Sterically Bulky Imidazolyl Group μ-苯氧基-μ-苯甲酸偶联双核咪唑基配合物的晶体结构
IF 0.2
X-ray Structure Analysis Online Pub Date : 2019-10-18 DOI: 10.2116/XRAYSTRUCT.35.11
Y. Yasuda, H. Furutachi, Yosuke Hayashi, Kaname Ishizaki, S. Fujinami, Shigehisa Akine, Masatatsu Suzuki, S. Nagatomo, T. Kitagawa
{"title":"Crystal Structure of μ-Phenoxo-μ-benzoate-bridged Dinuclear Fe(II) Complex with a Dinucleating Ligand Having a Sterically Bulky Imidazolyl Group","authors":"Y. Yasuda, H. Furutachi, Yosuke Hayashi, Kaname Ishizaki, S. Fujinami, Shigehisa Akine, Masatatsu Suzuki, S. Nagatomo, T. Kitagawa","doi":"10.2116/XRAYSTRUCT.35.11","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.35.11","url":null,"abstract":"The end-off type compartmental ligands, having a phenolic and alcoholic oxygen as an endogenous bridge, have been used for modeling bimetallic active sites of metalloprotains,1–4 such as hemerythrin (Hr)5 and methane monooxygenase (MMO).6 We have demonstrated that the thermal stability of (μ-peroxo) diiron(III) complexes and the oxygenation-deoxygenation reversibility are highly dependent on the nature of the end-off type compartmental ligands.4,7–11 Previously, we reported the crystal structure of a (μ-peroxo)diiron(III) complex, [Fe2(Phbimp)(PhCO2)(O2)], with a dinucleating ligand (Ph-bimp) bearing a sterically bulky imidazolyl group,8 which was obtained in a reversible reaction of the corresponding diiron(II) precursor complex, [Fe2(Ph-bimp)(PhCO2)](BF4)2·3H2O, with dioxygen in acetonitrile at ambient temperature. In this paper, we report details of the crystal structure of the diiron(II) precursor complex [Fe2(Ph-bimp)(PhCO2)(CH3CN)](BF4)2·2CH3CN·3CH3CH2OH (1) (Fig. 1). A single crystal of [Fe2(Ph-bimp)(PhCO2)(CH3CN)](BF4)2· 2CH3CN·3CH3CH2OH (1) suitable for X-ray crystallography was obtained by recrystallization of [Fe2(Ph-bimp)(PhCO2)](BF4)2·3H2O from a mixture of acetonitrile/ethanol at ambient temperature under N2. It was picked up on a hand-made cold copper plate mounted inside a liquid N2 Dewar vessel and mounted on a glass rod at –80°C. X-ray diffraction measurements were made on a Rigaku CCD Mercury diffractometer with graphite monochromated Mo Kα radiation at 108 K. The structure was solved by a direct method (SIR 92)12 and expanded using a Fourier technique. The structure was refined by a fullmatrix least-squares method by using SHELXL 201413 (Yadokari-XG).14 All non-hydrogen atoms were refined with anisotropic displacement parameters (ADP) and all hydrogen atoms were included using a riding model. The occupancy factors were also refined for the two BF4 anions, one acetonitrile molecule, and three ethanol molecules, which were disordered over two or three orientations. Distance/ADP restraints were applied to the disordered atoms in the anions and solvents. The crystal data is summarized in Table 1. The molecular structure of complex cation [Fe2(Ph-bimp)(PhCO2)(CH3CN)] of 1 is shown in Fig. 2. Selected bond distances (Å) and angles (°) are given in Table 2. The diiron(II) center is doubly bridged by phenoxide oxygen of Ph-bimp and benzoate oxygens, as found for closely related diiron(II) complexes: [Fe2(Ph-tidp)(PhCO2)] (2) (Ph-tidp = N,N,N′,N′tetrakis(1-methyl-4,5-diphenyl-2-imidazolyl)methyl-1,3-diamino2-propanolate),9 [Fe2(L)(PhCO2)] (3) (LPh4 = N,N,N′,N′tetrakis(1-methyl-2-phenyl-4-imidazolyl)methyl-1,3-diamino2-propanolate),10 and [Fe2(N-Et-HPTB)(PhCO2)] (4) (N-EtHPTB = N,N,N′,N′-tetrakis(1-ethyl-2-benzimidazolyl)methyl1,3-diamino-2-propanolate).15 The two iron atoms in 1 have different coordination geometries. The five-coordinate iron 2019 © The Japan Society for Analytical Chemistry","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-10-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.2116/XRAYSTRUCT.35.11","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42953418","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
Crystal Structure of 6,7-Dihydro-5a,7a,13,14-tetraaza-pentaphene-5,8-dione 6,7-二氢-5a,7a,13,14-四氮杂-五苯-5,8-二酮的晶体结构
IF 0.2
X-ray Structure Analysis Online Pub Date : 2019-10-10 DOI: 10.2116/xraystruct.35.57
Jean Guillon, Maria de Fatima Pereira-Rosenfeld, Noël Pinaud, Thierry Besson, V. Thiéry, Laurent Picot, Mathieu Marchivie
{"title":"Crystal Structure of 6,7-Dihydro-5a,7a,13,14-tetraaza-pentaphene-5,8-dione","authors":"Jean Guillon, Maria de Fatima Pereira-Rosenfeld, Noël Pinaud, Thierry Besson, V. Thiéry, Laurent Picot, Mathieu Marchivie","doi":"10.2116/xraystruct.35.57","DOIUrl":"https://doi.org/10.2116/xraystruct.35.57","url":null,"abstract":"The X-ray crystal structure of 6,7-dihydro-5a,7a,13,14-tetraaza-pentaphene-5,8-dione, a potential antiproliferative agent on A2058 melanoma cells, was established. It crystallizes in the monoclinic space group P21/c with cell parameters a = 24.879(3)A, b = 6.868(2)A, c = 26.068(4A, α = 90, β = 110.49(2), γ = 90, V = 4172.4(15)A3 and Z = 12. The crystal structure was refined to final values of R1 = 0.1353 and wR2 = 0.1936. An X-ray crystal structure analysis revealed that each molecule features intermolecular CArom.–H···O hydrogen bonds to form trimers.","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.2116/xraystruct.35.57","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43416051","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: 3595
Crystal Structure of a Dinuclear Co Complex with Doubly Bridged Fluorides: Di-μ-fluoride Bis{(2-pyridylmethyl)bis(2-quinolylmethyl)amine} Dicobalt(II) Bis(tetrafluoroborate), [Co2(μ-F)2(pbqa)2](BF4)2 双核双桥氟化物钴配合物的晶体结构:二-μ-氟双{(2-吡啶甲基)双(2-喹啉甲基)胺}二钴(II)双(四氟硼酸盐),[Co2(μ-F)2(pbqa)2](BF4)2
IF 0.2
X-ray Structure Analysis Online Pub Date : 2019-10-10 DOI: 10.2116/xraystruct.35.61
Takuto Mibu, Y. Suenaga, T. Okubo, M. Maekawa, T. Kuroda–Sowa
{"title":"Crystal Structure of a Dinuclear Co Complex with Doubly Bridged Fluorides: Di-μ-fluoride Bis{(2-pyridylmethyl)bis(2-quinolylmethyl)amine} Dicobalt(II) Bis(tetrafluoroborate), [Co2(μ-F)2(pbqa)2](BF4)2","authors":"Takuto Mibu, Y. Suenaga, T. Okubo, M. Maekawa, T. Kuroda–Sowa","doi":"10.2116/xraystruct.35.61","DOIUrl":"https://doi.org/10.2116/xraystruct.35.61","url":null,"abstract":"Dioxo-, dihydroxoand difluoro-bridged dinuclear metal complexes are well known. Their research concerning the complexes plays an important role in understanding the properties of metal–metal interaction such as energy, electron transfer, valence intermolecular charge-transfer, magnetic coupling. Also, these complexes have been interesting regarding organic synthesis catalysis and photosynthesis catalysis.1 The study of a fluorine crosslinked dinuclear cobalt complex has been reported by Cho et al.2 The fluorine source has an origin from hydrolysis of the tetrafluoroborate ions. The difluoride bridged dinuclear cobalt complex described in this manuscript has tetrafluoroborate ions too. However, the cobalt–cobalt distance is closed due to strong π–π interactions between two quinoline rings of ancillary ligands. In 2014, we reported on the crystal structure of [Co2(μ-F)2(Me3tpa)2](BF4)2 (Me3tpa = tris(6methyl-2-pyridylmethyl)amine), which involves μ-fluoro bridged between two cobalt(II) ions; the distance of Co···Co was 3.158 Å.3 We expected a greater steric hindrance and electronic effect of the ancillary ligand than Mentpa (n = 1, 2, 3), and chose pbqa (pbqa = (2-pyridylmethyl)bis(2-quinolylmethyl) amine)4,5 containing quinoline groups. In this paper we describe the synthesis and crystal structure of a μ-fluoro di-cobalt(II) complex using a simpler ancillary ligand, and have also compared it with [Co2(μ-F)2(Me3tpa)2](BF4)2. (Fig. 1). Crystals suitable for the single-crystal X-ray structure analysis were obtained as follows. A solution of Co(BF4)2·6H2O in dry methanol was added to a methanol solution of (2-pyridylmethyl)bis(2-quinolylmethyl)amine (pbqa). The resulting solution was stirred for 30 min. The methanol solution was transferred to some glass tubes, and diethyl ether was added to the solution slowly. After this sealed glass tube was left standing at ambient temperature, over a period of 9 days, brown microcrystals of [Co2(μ-F)2(pbqa)2](BF4)2 separated from the solution. Characterization was on the basis of ESI-MS, a satisfactory elemental analysis and single crystal crystallographic data. X-ray diffraction data for one of these crystals were collected at 100 K on a Rigaku XtaLAB P200 using multi-layer mirror monochromated Mo-Kα radiation. Crystal data and details concerning the data collection are given in Table 1. The structure was solved by direct methods, and refined by fullmatrix least-squares methods. Hydrogen atoms were refined using the riding model with C–H = 0.95 or 0.98 Å and with Uiso(H) = 1.2Ueq(C). The final crystals of a full matrix leastsquares refinement on F2 was based on 7897 observed reflections and 447 variable parameters, and converged (largest parameters shift was 0.00 times its esd) with unweighted and weighted agreement factors of R1 = 0.0403 (I > 2σ(I)) and wR2 = 0.1018 (all data). The standard deviation of an observation of unit weights was used. The maximum and minimum peaks on the final difference Fourier map co","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.2116/xraystruct.35.61","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46291071","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 of Hexakis(quinoline-2-thiolatosilver(I)) 六烷基喹啉-2-硫代银(I)的晶体结构
IF 0.2
X-ray Structure Analysis Online Pub Date : 2019-09-10 DOI: 10.2116/xraystruct.35.51
Y. Ozawa, A. Masunaga, M. Kubo, N. Yasuda, K. Toriumi
{"title":"Crystal Structure of Hexakis(quinoline-2-thiolatosilver(I))","authors":"Y. Ozawa, A. Masunaga, M. Kubo, N. Yasuda, K. Toriumi","doi":"10.2116/xraystruct.35.51","DOIUrl":"https://doi.org/10.2116/xraystruct.35.51","url":null,"abstract":"with ten-micron dimensions were obtained. Single-crystal X-ray diffraction measurements were performed at the SPring-8 BL40XU undulator beamline, and the diffraction intensities were collected by a RIGAKU Saturn-724 CCD detector at 150 K. Crystal data and detailed experimental conditions for diffraction measurements are given in Table 1. The structure The structure of a hexanuclear silver(I) complex with six quinoline-2-thiolato (2-qnt – ) ligands [Ag 6 (C 9 H 6 NS) 6 ] ( 1 ) has been synthesized and characterized. Complex 1 crystallized in a triclinic space group P -1 (No. 2) with a = 8.064(6), b = 13.480(3), c = 13.573(5)Å, α = 113.528(15) ° , β = 104.24(3) ° , γ = 100.46(3) ° , V = 1244.5(11)Å 3 , Z = 1, T = 150 K. The R 1 [ I > 2 σ ( I )] and wR 2(all data) values are 0.032 and 0.089, respectively, for all 4437 independent reflections. The complex has a paddle-wheel-like structure with a trigonally distorted Ag 6 octahedral metal core.","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-09-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41255002","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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