X-ray Structure Analysis Online最新文献

{"title":"Crystal Structure of 6-Aza-3,9-dithiaundecane Hydrochloride","authors":"Mari Toyama, K. Chayama","doi":"10.2116/xraystruct.35.55","DOIUrl":"https://doi.org/10.2116/xraystruct.35.55","url":null,"abstract":"was also observed in a series of acyclic polythioethers. 5 The title compound consists of two parts: a protonated N -H-ATU cation, ( N -H 2 -ATU) + , and a Cl – anion. Two hydrogen atoms on the N1 atom connect with the counter anion, Cl – , The crystal structure of the title compound, 6-aza-3,9-dithiaundecane hydrochloride ( N -H-ATU·HCl), was determined by X-ray crystallography. The hydrogen-bonding networks in the crystal extend along with the b and c axes to form a 2D-triple-sheet, in which the Cl – ions put between two ( N -H 2 -ATU) + sheets. The compound was crystallized in an orthorhombic system as: Pccn , a = 25.0091(4), b = 5.39364(10), c = 9.37759(19)Å, Z = 4, V = 1264.94(4)Å 3 . The R 1 and wR 2 values were 0.0341 and 0.0880, respectively, for 1162 reflections.","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":"44554342","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}

{"title":"Crystal Structure of 7-(Dimethylamino)-3-phenylcoumarin","authors":"K. Kubo, Taisuke Matsumoto, H. Takechi","doi":"10.2116/XRAYSTRUCT.35.47","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.35.47","url":null,"abstract":"","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-08-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.2116/XRAYSTRUCT.35.47","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41648176","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}

{"title":"Crystal Structure of Catena-((μ8-benzene-1,2,4,5-tetracarboxylato)-triaqua-calcium(II)-copper(II))","authors":"Gaoxiang Meng, Qiang Li, Yongming Yang","doi":"10.2116/XRAYSTRUCT.35.49","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.35.49","url":null,"abstract":"The construction of some metal-organic framework (MOF) based on alkaline earth metals and aromatic carboxylic acid has been emerging as a research field for more than thirty years.1 The lack of d-orbital electrons in alkaline elements may result in even more coordination geometries in the construction of a MOF material.1 However, by introducing both one transition and alkaline earth metals simultaneously into a MOF structure has been only reported recently.2 The unsaturated coordination and weak coordinated solvent molecules around metal centers can provide some new type of potentially valuable MOF materials.3–6 Based on this design strategy, we have now prepared one Cu(II)-Ca(II) combined coordination complex (I) under the hydrothermal condition (Fig. 1). In (I), these two types of metals are bridged by benzene-1,2,4,5-tetracarboxylic acid (H4BTA). Although no crystallographic void was detected in (I), it can adsorb N2 gas to a certain extent. Herein, we will report the crystal structure of (I). In this research, compound (I) was prepared by dissovling Cu(NO3)2·2(H2O) (0.2 mmol, 48.0 mg), CaCl2 (0.2 mmol, 23 mg) and H4BTA acid (0.2 mmol, 51.0 mg) in 10 mL of water. The mixture was stirred for 10 min at ambient temperature and then heated in a 20-mL capacity Teflon-lined reaction vessel at 160°C for 3 days. After slowly cooling to room temperature at a rate of 5°C h–1, the final plate-blue crystals (51.2 mg), suitable for X-ray structure analysis, could be obtained. The crystal and structure refinement data are summarized in Table 1. 2019 © The Japan Society for Analytical Chemistry","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-08-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.2116/XRAYSTRUCT.35.49","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43572911","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}

{"title":"Crystal Structure of [N-(9-Anthracenylmethyl)-1,3-propanediamine](2,2′-bipyridine)platinum(II) Chloride","authors":"T. Kiwada, H. Takayama, Hiromu Katakasu, A. Odani","doi":"10.2116/XRAYSTRUCT.35.39","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.35.39","url":null,"abstract":"The crystal structure of [ N -(9-anthracenylmethyl)-1,3-propanediamine](2,2 ′ -bipyridine)platinum(II) chloride was determined by X-ray crystallography. The title complex crystallized in the monoclinic space group P 21/ c and Z = 4 with cell parameters a = 11.2466(7)Å, b = 17.3553(10)Å, c = 13.7027(9)Å, β = 100.501(2) ° , V = 2629.8(3)Å 3 . [ I > 2 σ ( I )] and wR 2 (all data) values are 0.0271 and 0.0619, respectively, for all 5995 independent reflections. The intramolecular π-π stacking interaction was observed between the anthracene and the bipyridine. In the crystal packing structure, the intermolecular π-π stacking interaction was observed. 2019)","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.2116/XRAYSTRUCT.35.39","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44655489","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}

{"title":"Crystal Structure of a Co(III) Complex with 2-Aminoethanethiol and Triethylenetetramine","authors":"Chika Kurogi, T. Yonemura","doi":"10.2116/XRAYSTRUCT.35.43","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.35.43","url":null,"abstract":"The structure of β (Nprim)-[Co(aet)(trien)]Cl 2 [aet: 2-aminoethanethiolate, trien: triethylenetetramine] was synthesized and characterized by single-crystal X-ray analysis. The compound crystallizes in a triclinic space group P 1 with a = 8.279(3), b = 10.673(5), c = 10.696(4)Å, α = 64.70(3), β = 95.76(3), γ = 91.17(4) ° , V = 849.9(6)Å 3 , D calcd = 1.552 g/cm 3 , Z = 2. The R 1 [ I > 2 σ ( I )] and wR 2 (all data) values are 0.0385 and 0.1145, respectively, for all 3913 independent reflections. Central cobalt(III) atoms have an approximate octahedral geometry and are coordinated by five nitrogen atoms and one sulfur atom. The obtained compound from the major eluate is in the β (Nprim) form in which the sulfur atom is present in the trans position to a primary nitrogen atom of the triethylenetetramine (trien).","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43232785","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}

{"title":"Crystal Structure of (2,2′-Bipyridine)(N-(1-naphthyl)methyl-1,3-propanediamine)platinum(II) Chloride","authors":"T. Kiwada, Aika Hirasaki, A. Odani","doi":"10.2116/XRAYSTRUCT.35.35","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.35.35","url":null,"abstract":"The crystal structure of (2,2 ′ -bipyridine)( N -(1-naphthyl)methyl-1,3-propanediamine)platinum(II) chloride was determined by X-ray crystallography. The title complex crystallized in the monoclinic space group C 2/ c and Z = 8 with cell parameters a = 23.3026(14)Å, b = 17.4118(12)Å, c = 12.3816(7)Å, β = 109.032(8) ° , V = 4749.1(6)Å 3 . The R 1 [ I > 2 σ ( I )] and wR 2 (all data) values are 0.0242 and 0.0490, respectively, for all 5435 independent reflections. In the crystal structure, disorder was observed for the N -(1-naphthyl)methyl-1,3-propanediamine moiety. Hydrogen-bond network was formed between the (2,2 ′ -bipyridine)( N -(1-naphthyl)methyl-1,3-propanediamine)platinum(II) cations and chloride anions.","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48317773","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}

{"title":"Synthesis and Crystal Structure of Bis[2-(1,4,5,6-tetrahydropyrimidin-2-yl)phenolato]zinc(II)","authors":"R. Mitsuhashi, M. Mikuriya","doi":"10.2116/XRAYSTRUCT.35.37","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.35.37","url":null,"abstract":"Magnetic dilution of coordination compounds, in which paramagnetic atoms in a crystal are partially substituted by diamagnetic atoms, is a useful technique to investigate the magnetic interactions in detail.1 To achieve magnetic dilution, it is necessarily to employ a diamagnetic metal ion with the same oxidation state and similar size to that of the original paramagnetic ion. Furthermore, the diamagnetic analogue of the desired complex has to be isomorphic. Since mononuclear cobalt(II) complexes can be a single-ion magnet,2,3 the preparation of a zinc(II) analogue is important. On the other hand, we recently reported that the bis[2-(1,4,5,6-tetrahydropyrimidin-2-yl)phenolato]cobalt(II) complex exhibits magnetic slow relaxation, even in the absence of an external magnetic field.3 It is suggested that the origin of the slow relaxation is to be intermolecular magnetic interactions induced by hydrogenbonding interactions. To investigate the effect of intermolecular interactions, we focused on the synthesis, crystal structure and hydrogen-bonded supramolecular structure of the zinc(II) analogue, bis[2-(1,4,5,6-tetrahydropyrimidin-2-yl)phenolato]zinc(II) (Fig. 1). The unsymmetrical bidentate ligand precursor, 2-(1,4,5,6tetrahydropyrimidin-2-yl)phenol (H2thp), was synthesized by a reported procedure.4 Although previously reported [Co(Hthp)2] was synthesized from the Co(BF4)2·6H2O, preparation of [Zn(Hthp)2] from the BF4 salt resulted in the formation of colorless microcrystals. Alternatively, colorless single crystals of [Zn(Hthp)2] were obtained by a reaction of ZnCl2, H2thp and KOtBu in a 1:2:2 ratio in ethanol. Yield: 34.1 mg (40%). Crystal data are included in Table 1. X-ray crystallographic 2019 © The Japan Society for Analytical Chemistry","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44810659","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}

{"title":"Crystal Structure of a Mononuclear Iron(III) Complex, Hexakis(dimethylsulfoxide-κO)iron(III) Tris(hexafluoridophosphate)","authors":"Kaoru Shomura, R. Mitsuhashi, M. Mikuriya, Y. Kataoka, M. Handa, H. Sakiyama","doi":"10.2116/XRAYSTRUCT.35.31","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.35.31","url":null,"abstract":"X-ray method. The compound crystallized in the trigonal space group R 3 and Z = 3 with cell parameters a = 11.598(8)Å, c = 25.367(18)Å, V = 2955(4)Å 3 . The R 1 [ I > 2 σ ( I )] and wR 2 (all data) values were 0.0509 and 0.1565, respectively, for all 1630 independent reflections. The symmetry of the complex cation was found to belong to the S 6 point group, possessing a trigonally compressed octahedral coordination geometry with an O 6 donor set.","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42326360","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}

{"title":"Synthesis and Crystal Structure of 1,3-Bis(5-chloro-3-methoxysalicylideneamino)-2-propanol Trihydrate","authors":"M. Mikuriya, Yoshiki Koyama, R. Mitsuhashi","doi":"10.2116/XRAYSTRUCT.35.33","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.35.33","url":null,"abstract":"X-ray quality crystals were grown by slow the data collected on a Bruker CCD X-ray diffractometer (SMART APEX) using graphite-monochromated Mo- K α radiation. Crystal data and data Table The structure was solved by an intrinsic phasing method and refined The title compound, 1,3-bis(5-chloro-3-methoxysalicylideneamino)-2-propanol trihydrate, was synthesized and the crystal structure was determined by the single-crystal X-ray diffraction method at 90 K. It crystallizes in the monoclinic space group P 2/ c with a = 18.098(3)Å, b = 4.3275(8)Å, c = 14.572(3)Å, β = 104.283(3) ° , V = 1106.0(3)Å 3 , D x = 1.445 g/cm 3 ,","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43745348","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}

{"title":"Synthesis and Crystal Structure of the Bis(μ-hydroxo)diiron(II) Complex with Tridentate Ligands Having a Sterically Bulky Imidazolyl Group","authors":"Reiko Yaguchi, H. Furutachi, Sanae Shirotsuki, Xi Zhang, T. Ishikawa, Shigehisa Akine, T. Tosha, S. Fujinami, Masatatsu Suzuki, T. Kitagawa","doi":"10.2116/XRAYSTRUCT.35.27","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.35.27","url":null,"abstract":"The Fe2/O2-mediated arene hydroxylation is of current interest for understanding the reaction mechanism of a dioxygen activating non-heme dinuclear iron enzyme, such as toluene monooxygenase (TMO).1–3 Previously, we reported on intramolecular aromatic ligand hydroxylation via the decay of (μ-peroxo)diiron(III) complexes with the dinucleating ligands having a phenyl group as a reaction probe.4–6 In this study, we synthesized the bis(μ-hydroxo)diiron(II) complex [Fe2(OH)2(L)2](ClO4)2 (1) with a tridentate ligand (L) having 2-phenylimidazolyl groups in order to examine the Fe2/O2-mediated arene hydroxylation (Fig. 1). In this paper, we report on the crystal structure of 1 together with the reactivity toward dioxygen. The tridentate ligand L·H2O was synthesized according to a literature method.7 The diiron(II) complex with L was prepared under a N2 atmosphere. A mixture of Fe(CF3SO3)2·2CH3CN (0.436 g, 1.0 mmol) and L·H2O (0.456 g, 1.0 mmol) in dryTHF/CH2Cl2 (1:1, 20 mL) was added a THF solution (3 mL) containing H2O (18 μL, 1.0 mmol) and triethylamine (138 μL, 1.0 mmol) to give a yellow-green solution. Diethyl ether (20 mL) was added to the resulting yellow-green solution to give a yellow-green powder, which was filtered and washed with diethyl ether. Yield: 0.32 g, 47%. Anal. Found: C, 52.51; H, 4.43; N, 10.18%. Calcd for [Fe2(OH)2(L)2](CF3SO3)2·2H2O, C60H64F6Fe2N10O10S2: C, 52.41; H, 4.69; N, 10.19%. Single crystals of [Fe2(OH)2(L)2](ClO4)2 (1) suitable for X-ray crystallography were obtained by slow diffusion of diethyl ether onto a dry-CH2Cl2/MeCN (1:1) solution of a yellow-green powder containing (n-Bu)4NClO4. X-ray diffraction measurements were made on a Rigaku CCD Mercury diffractometer with graphite-monochromated Mo Kα radiation at 123 K. The structure was solved by a direct method (SHELXS 97)9 and expanded using a Fourier technique. The structure was refined by a full-matrix least-squares method by using a SHELXL 201410 (Yadokari-XG).11 All non-hydrogen atoms were refined with anisotropic displacement parameters. The μ-hydroxo hydrogen atoms were refined using distance restraints with Uiso constrained to 1.2-times the Ueq of the parent oxygen atoms. Other hydrogen atoms were included using a riding model. The crystal data are summarized in Table 1. X-ray crystallography of 1 reveals that the asymmetric unit contains a half of the complex cation [Fe2(OH)2(L)2] and a perchlorate anion. The molecular structure of the complex cation [Fe2(OH)2(L)2] of 1 is shown in Fig. 2. Selected bond distances (Å) and angles (°) are given in Table 2. The complex cation [Fe2(OH)2(L)2] of 1 has a centrosymmetric bis(μhydroxo)diiron(II) diamond core, as found for a closely related five-coordinated bis(μ-hydroxo)diiron(II) complex [Fe2(OH)22019 © The Japan Society for Analytical Chemistry","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.2116/XRAYSTRUCT.35.27","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44921865","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}