X-ray Structure Analysis Online最新文献

{"title":"Crystal Structure of cis-Bis(2,2′-bipyridyl)bis(trifluoromethanesulfonato)cobalt(II)","authors":"Mari Toyama, Yuichi Yamamoto","doi":"10.2116/XRAYSTRUCT.35.21","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.35.21","url":null,"abstract":"Cobalt(II) complexes with polypyridyl ligands were used as photo-catalysts for hydrogen generation from water,1 sensitizers in dye-sensitized solar cells,2 or building blocks for magnetic supramoleculars,3 because of their redox and magnetic properties. When synthesizing a new functional cobalt(II) complex with polypyridyl ligands, such as cis-[Co(L)2(N-N)2] or cis-[Co(L-L)(N-N)2] (L = monodentate ligand, L-L = bidentate ligand, N-N = 2,2′-bipyridine (bpy) or 1,10-phenanthroline (phen) etc.), cis-[Co(solvent)2(N-N)2] or cis-[CoII(OTf )2(N-N)2] (OTf– = trifluoromethanesulfonato or CF3SO3) have been utilized as a precursor.3 This is a popular synthetic method for not only cobalt(II) complexes, but also many transition metal complexes. However, there are only four reports concerning the crystal structure of cis-[MII(OTf )2(bpy)2] (M = Mn, Ni, Cu, or Zn),3 because OTf– ligands might be too labile to be isolated from a reaction solution as single crystals. Smith and co-workers prepared cis-[MII(OTf )2(bpy)2] (M = Mn or Co) complexes from the reaction of cis-[MCl2(bpy)2] with Ag(OTf ) in acetonitrile.3 The cis-[MnII(OTf )2(bpy)2] complex was characterized by elemental analysis, IR spectra, and X-ray crystal structure, whereas the Co(II) complex was reported based on only IR spectroscopic data. Fortunately, we were able to determine the crystal structure of cis-[CoII(OTf )2(bpy)2] (Fig. 1). Here we report on it, and compare the lattice parameters of our Co2+ complex with those of other transition metal complexes, cis-[MII(OTf )2(bpy)2]. We obtained yellow crystals of cis-[CoII(OTf )2(bpy)2], which were suitable for X-ray crystallography, from the reaction mixture of [Co(CO)3(bpy)2](OTf )4 and di-2-pyridylamine (Hdpa) in EtOH–H2O containing a small amount of HOTf(aq). We expected that [Co(bpy)2(Hdpa)] would be obtained from the reaction, but the anticipated complex was not yielded. The 1H NMR spectrum of the product showed that [Co(bpy)3] and a CoIII-Hdpa complex, probably [Co(Hdpa)3] or trans[Co(OH2)2(Hdpa)2], existed in the NMR sample. We tried to crystalize the CoIII-Hdpa complex by the vapor diffusion of diethyl ether into an EtOH–MeOH (1:1) solution of the mixed product. However, this plan went wrong. From the solution, two kinds of yellow crystals, which had different shapes, for [Co(bpy)3](OTf )3 and cis-[CoII(OTf )2(bpy)2], and a yellowbrown oily product, which would be the CoIII-Hdpa complex, were obtained. The Co2+ complex, cis-[CoII(OTf )2(bpy)2], might be produced from a reduction reaction of the Co3+ complex, [Co(CO3)(bpy)2], by EtOH in the reaction solution. We thought that it would be important for coordination chemists, because it is the first report concerning the crystal structure of cis-[CoII(OTf )2(bpy)2]. In 2013, Kurahashi and Fujii reported on a very unique cobalt complex with a salen ligand (Fig. S1, Supporting Information) and an OTf– ligand, [Co(salen)(OTf )], which was characterized by X-ray crystallography, cyclic voltammetry,","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-04-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47501849","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 Bis(2-methoxy-6-((Z)-(p-tolylimino)methyl)phenoxy)palladium","authors":"K. Kassim, Muhammad Ashraf Mohd Kahar, B. Yamin, Mohd Abdul Fatah Abdul Manan, M. Yusof","doi":"10.2116/XRAYSTRUCT.35.25","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.35.25","url":null,"abstract":"Schiff-base complexes are being continuously studied concerning catalyst,1–3 biomedical4,5 and material applications for their structural fundamental and theoretical understanding. Pd(II) Schiff-base complexes have remarkable properties, such as high selectivity and activity by manipulating the ligand environment.6 The complex C30H28N2O4Pd was synthesized according to previous studies7 with slight modification. A 0.2mmol (Z)-2-methoxy-6-((p-tolylimino)methyl)phenol was added to a stirred solution of 0.1 mmol of palladium(II) acetate in 5 mL of ethanol. The solution was refluxed for 6 h, and cooled to the room temperature. The precipitate was filtered off and air-dried. The product was recrystallized in ethanol:chloroform (1:1) through a slow evaporation method to produce an orange crystal. Yield, 62.0%; m.p. 558 – 561 K. Anal. Calc. for C30H28N2O4Pd: C, 61.8; H, 4.4; N, 10.3%; Found: C, 61.6; H, 4.5; N, 10.7%. The IR spectrum was obtained as a KBr disc on a Perkin Elmer Spectrum One FTIR Spectrometer from 450 – 4000 cm–1. The peaks at 1596, 1327, 1258, 1542, 580 and 449 cm–1 were assigned to ν(C=N), ν(C–N), ν(C–O), ν(C=C aromatic), ν(Pd–O) and ν(Pd–N), respectively. The infrared data obtained are nearly similar based on a previous study reported.8 The NMR spectrum was obtained as a CDCl3 solution on Jeol 400 MHz spectrometer. The 1H NMR chemical shifts, δ, observed are (ppm): 2.42 (s, 3H, CH3), 3.36 (s, 3H, OCH3), 6.39 – 7.29 (m, 7H, aromatic, JHH = 1 – 3 and 6 – 9 Hz), 7.66 (s, 1H, HC=N). The coupling constant indicates the presence of meta and ortho aromatic protons. The crystal and structure-refinement data are summarized in Table 1 and selected bond distances and angles in Table 2. H atoms were positioned geometrically and allowed to ride on the parent C atom, with C–H = 0.95 – 0.98 Å, and with Uiso(H) = 1.2 (1.5 for methyl groups) times Ueq(C). Figure 1 represents the chemical diagram whereas Fig. 2 shows the ORTEP structure of the title compound. In this centrosymmetric complex, the two ligands are symmetrically related to each other and have the same bond angles and distances. The ligand was coordinated to the metal center through ONNO atoms, forming a square-planar complex, yielding two six-membered rings surrounding the metal center. 2019 © The Japan Society for Analytical Chemistry","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-04-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47679024","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 Bis(μ-hydroxo)diiron(III) Complex with Tripodal Ligands Having a Terminal Carboxylate Group","authors":"Xi Zhang, H. Furutachi, Yuya Ohyama, S. Fujinami, Shigehisa Akine, Masatatsu Suzuki","doi":"10.2116/XRAYSTRUCT.35.17","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.35.17","url":null,"abstract":"Hydroxoor oxo-bridged non-heme diiron centers with terminal carboxylates are structural motifs found in metalloproteins, such as soluble methane monooxygenase (sMMO) and ribonucleotide reductase (RNR).1–4 Synthetic diiron model complexes with Fe2(OH)2, Fe2(O)(OH), and Fe2(O)2 cores are of particular importance for obtaining fundamental insights into the structural and spectroscopic properties of the active centers in the metalloproteins mentioned above.2–4 Previously, we reported that the crystal structure of a (μ-oxo)(μ-hydroxo)diiron(III) complex, [Fe2(6Me2-BPP)2(O)(OH)] (2),5 with a tetradentate tripodal ligand (6Me2-BPP) having a terminal carboxylate, which was derived from deprotonation of its conjugate acid, [Fe2(6Me2-BPP)2(OH)2]. In this paper, we report on the crystal structure of the bis(μ-hydroxo)diiron(III) complex [Fe2(6Me2BPP)2(OH)2](NO3)1.9553·Br0.0447·8H2O (1) (Fig. 1). A single crystal of [Fe2(6Me2-BPP)2(OH)2](NO3)1.9553·Br0.0447· 8H2O (1) suitable for X-ray crystallography was obtained by the recrystallization of [Fe2(6Me2-BPP)2(OH)2](NO3)2·4.5H2O from water. 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 123 K. The structure was solved by a direct method (SHELXS 97)6 and expanded using a Fourier technique. The structure was refined by a full-matrix least-squares method by using the SHELXL 20147 (YadokariXG).8 The asymmetric unit contains two very similar molecules that could be nearly related by each other with a translation symmetry in the [0 1 1] direction. This could be interpreted as a structure with a half unit-cell volume. However, the counter anions (NO3, Br –) and crystallizing water molecules are located at different positions that could not be related by a translational symmetry. Also, the diffractions with k + l = odd showed significant intensities (around 1/3 of those with k + l = even). Therefore, we concluded that the structure should have two independent molecules in the asymmetric unit. All nonhydrogen atoms were refined with anisotropic displacement parameters. The hydrogen atoms in the μ-hydroxo groups and water molecules were restrained to ensure reasonable distances (0.84 Å) by applying the default values for O–H DFIX restraints. 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 two halves of complex cations, [Fe2(6Me2-BPP)2(OH)2] (molecules A and B), 1.9553 nitrate ions, 0.0447 bromide ion, and eight water molecules. The partial content of the bromide ion appears to be due to the preparation route of the 6Me2BPPH ligand, which was obtained from the reaction of bis(6methyl-2-pyridylmethyl)amine with 3-bromopropionic acid in the presence of triethylamine.5 ORTEP drawing of the complex cati","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-04-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46200627","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-(2-imidazolinyl)phenolato]zinc(II)","authors":"R. Mitsuhashi, M. Mikuriya","doi":"10.2116/xraystruct.35.15","DOIUrl":"https://doi.org/10.2116/xraystruct.35.15","url":null,"abstract":"Cobalt(II) complexes have been extensively investigated in the last two decades owing to potential application to singlemolecule magnets.1 To precisely understand the static and dynamic magnetic properties, the synthesis and crystallization of an analogous complex with a diamagnetic transition metal ion is important. Recently, we have reported on the crystal structure and single-ion magnet (SIM) behavior of the bis[2-(2imidazolinyl)phenolato]cobalt(II) complex.2 This complex is a rare example of 3d SIM, which shows slow magnetic relaxation under zero field. The origin of the zero-field SIM behavior was suggested to be intermolecular magnetic interactions arising from the hydrogen-bonded chain structure of the complex. To investigate the effect of intermolecular interactions on the static and dynamic magnetic property, the crystallization of an isomorphous complex with a diamagnetic ion is necessary. In this study, we report on the synthesis, crystal structure and hydrogen-bonded interactions of a zinc(II) analogue, bis[2-(2imidazolinyl)phenolato]zinc(II) (Fig. 1). The ligand precursor, 2-(2-imidazolinyl)phenol (H2imn), was synthesized by a previously reported procedure.3 A zinc(II) complex analogous to the title compound was reported by He, although this compound includes a methanol molecule as a solvent of crystallization.4 To obtain a zinc(II) complex isomorphous to [Co(Himn)2], we employed the same synthetic procedure, except for the reaction condition.2 Colorless crystals of [Zn(Himn)2] were immediately formed upon mixing a 10-mL methanol solution of KOtBu (45.4 mg) and H2imn (65.7 mg) and a 10-mL methanol solution of ZnCl2 (27.9 mg) in air, while the cobalt(II) analogue was synthesized under an Ar atmosphere. Yield: 63.3 mg (80%). The crystal data are included in Table 1. X-ray crystallographic data were collected on a Bruker smart APEX CCD diffractometer at 90 K. The integrated and scaled data were empirically corrected with SADABS.5 The initial structure was solved by an intrinsic phasing method with SHELXT-2014,6 and refined using the full-matrix least-squares method on F2 utilizing SHELXL-2014.7 The non-hydrogen atoms were refined 2019 © The Japan Society for Analytical Chemistry","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47532268","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 Bis(μ-hydroxo)diiron(II) Complex with a Dinucleating Ligand Having a Butyl Linker","authors":"Mio Sekino, H. Furutachi, Kyosuke Tasaki, T. Ishikawa, S. Fujinami, Shigehisa Akine, Y. Sakata, Masatatsu Suzuki, Takashi Nomura, T. Ogura, T. Kitagawa","doi":"10.2116/XRAYSTRUCT.35.5","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.35.5","url":null,"abstract":"","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-02-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.2116/XRAYSTRUCT.35.5","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47381515","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-(4-Methylimidazolin-2-yl)phenol: an Another Polymorph","authors":"R. Mitsuhashi, M. Mikuriya","doi":"10.2116/XRAYSTRUCT.35.9","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.35.9","url":null,"abstract":"The self-assembly of coordination compounds by hydrogenbonding interactions is a promising strategy to construct a supramolecular structure to enable versatile functionalities. We have been focusing on tris-chelate and bis-chelate cobalt complexes with a 2-(2-imidazolinyl)phenolate ligand to control the coordination geometry1 and tune the static and dynamic magnetic properties of a complex.2,3 We previously reported on the synthesis and crystal structure of a methyl substituted analogue of the ligand precursor, (R)-2-(4-methylimidazolin-2yl)phenol, to investigate the effect of a chiral group on the resulting hydrogen-bonded network.4 This compound crystallized from an enantiomerically pure solution to afford the chiral space group P21. In this study, we focused on the crystallization of a racemic mixture of 2-(4-methylimidazolin-2yl)phenol, and report a new chiral polymorph (Fig. 1). The title compound was synthesized using a method modified from that reported in the literature.5 A mixture of methyl salicylate (7.68 g) and a racemic mixture of 1,2-diaminopropane (11.40 g) were heated at 160°C overnight. The unreacted 1,2-diaminopropane was evaporated under atmospheric pressure. After cooling, the title compound was obtained as a pale-yellow residue. The residue was recrystallized from ethanol. The crystal data are included in Table 1. The X-ray crystallographic data was collected on a Bruker smart APEX CCD diffractmeter at –183°C. The integrated and scaled data were empirically corrected with SADABS.6 The initial structure was solved by an intrinsic phasing method with SHELXT-2014,7 and refined using a full-matrix least-squares method on F2 utilizing SHELXL-2014.8 The non-hydrogen atoms were refined anisotropically, and hydrogen atoms were refined using the riding model, except for the N–H atoms. The N–H atoms were located by a difference Fourier map and refined isotropically. The Flack parameter could not be determined reliably because of low Friedel pair coverage. Crystallographic data have been deposited with Cambridge Crystallographic Data 2019 © The Japan Society for Analytical Chemistry","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-02-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.2116/XRAYSTRUCT.35.9","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46951307","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 Tertiarybutyl Ammonium Bis[(naphthalene-2,3-diolato)borate] Dimethyl Sulfoxide Solvate","authors":"M. Tombul","doi":"10.2116/xraystruct.35.3","DOIUrl":"https://doi.org/10.2116/xraystruct.35.3","url":null,"abstract":"Ammonium The structure of tertiarybutyl ammonium bis[naphthalene-2,3-diolato)borate] dimethyl sulfoxide solvate was determined by X-Ray crystallography. The compound crystallized in a triclinic system, and was characterized to be in the space group P -1, with cell parameters a = 9.6282(9)Å, b = 11.0221(9)Å, c = 13.0273(12)Å, α = 91.050(4) 0 , β = 109.419(4) 0 , γ = 94.574(2) 0 , Z = 2, and V = 1298.2(2)Å 3 . The crystal packing is governed by intermolecular and intramolecular N–H···O hydrogen bonds. The B atom takes a distorted tetrahedral geometry with four O atoms of naphthalene-2,3-diolato ligands.","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-01-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.2116/xraystruct.35.3","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43469408","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 Gramicidin S Hydrochloride at 1.1 Å Resolution","authors":"A. Asano, M. Doi","doi":"10.2116/XRAYSTRUCT.35.1","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.35.1","url":null,"abstract":"","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2019-01-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48719134","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":"Molecular Planarity and Crystal Structures of N-Salicylideneaminopyrazine Derivatives","authors":"Haruki Sugiyama","doi":"10.2116/XRAYSTRUCT.34.57","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.34.57","url":null,"abstract":"Schiff bases (also called azomethines) are considered to be important organic compounds containing acyclic and cyclic imine C=N bonds, which have various applications in photoluminescence materials,1 optical materials and devices,2 organic light-emitting diodes,3 oxidation hair dyes4 and color print materials.5 N-Salicylideneaniline (SA), which is one of the Schiff bases, and its structural analogues are known to show photochromism in the crystalline state upon UV light irradiation.6 Interestingly, SA crystals including non-planar molecules with dihedral angle between two aromatic rings greater than 30° are photochromic, and those including planar molecules with a dihedral angle of less than 20° are non-photochromic.7,8 N-Salicylidene aminopyrazine (SAPz) is one of the SA derivatives that include a pyrazine (Pz) (Fig. 1). SAPz derivative molecules would prefer a planar conformation by taking one of two possible Pz orientations, which avoids the intramolecular H to H steric repulsion between Pz C–H and imine C–H. On the other hand, SA derivatives have always suffered from such steric repulsions, so the conformation may not be necessarily planar. In order to demonstrate that SAPz crystals have planar molecules, but no photochromic property, we synthesized two SAPz derivatives of 2SAPZ (1) and 3,5-Br-2SAPZ (2), and analyzed their crystal structures and photochromic properties. The synthesis schemes of compounds 1 and 2 are as follows: A mixture of salicylaldehyde derivative (10 mmol) and 2-aminopyrazine (10 mmol) was heated at 393 K for 2 h without a plug. The resulting melt was cooled, and then red crude title compounds were precipitated. Single crystals were obtained by recrystallizations from chloroform and methanol, respectively. Single crystals X-ray diffraction data were collected at 293 K on a R-AXIS RAPID imaging plate area detector (RIGAKU) using graphite-monochromated Mo-Kα radiation from a rotating anode source. Scaling and absorption corrections were performed using ABSCOR.9 Crystal data and refinement details of 1 and 2 are given in Table 1. The initial structures were determined by using a dual space method with SHELXT-2014/4, and refined by full-matrix least-squares on Fo with SHELXL-2018/1.10,11 All hydrogen atoms were found in the difference Fourier map; however, they were placed by geometrical calculations and treated using a riding model with Uiso(H) = 1.2 × Ueq(C) or 1.5 × Ueq(O). ORTEP drawings are shown in Fig. 2. The hydrogen-bond lengths and angles in the crystal of 1 and 2 are summarized in Tables S1 and S2 (Supporting Information), respectively. Solid-state diffuse reflectance spectra were measured at 298 K with a JASCO V-560 spectrometer. Analytical samples were prepared as a mixture of the 2SAPz crystals (10 mg) and barium sulfate powder (100 mg). UV irradiation was performed with a high-power UV-LED irradiator (Keyence Corporation) at a wavelength of 365 nm. The measured spectra are shown in Fig. S1 (Supporting Informati","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2018-12-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.2116/XRAYSTRUCT.34.57","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46803810","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 Supramolecular Complex Built up from Molybdenum(II) Trifluoroacetate and Copper(II) Schiff-Base Components, [{CuLt-Bu}2{Mo2(O2CCF3)4}3(H2O)2]n, H2Lt-Bu = 2,3-bis((5-tert-butyl-2-hydroxybenzylidene)amino)-2,3-butenedinitrile","authors":"M. Handa, H. Kamada, D. Yoshioka, I. Hiromitsu, K. Kasuga, M. Mikuriya","doi":"10.2116/XRAYSTRUCT.34.59","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.34.59","url":null,"abstract":"There has been much interest for the use of tetracarboxylato dimetal complexes with a lantern-like structure as building blocks in combination with bridging ligands to construct two or three-dimensional architectures, because they show remarkable properties, such as gas-occlusion and ferrior ferromagnetism.1–3 Here, we report on a new assembled complex, [{CuL}2 {Mo2(O2CCF3)4}3(H2O)2] (1), H2L = 2,3-bis((5-tert-butyl-2hydroxybenzylidene)amino)-2,3-butenedinitrile. The copper(II) complex with a Schiff-base ligand ([CuLt-Bu]) is paramagnetic, based on the d9 configuration, although the lantern-type dinuclear molybdenum(II) complex is diamagnetic based on the σ2π4δ2 configuration of the Mo–Mo quadruple bond core. The phenoxido oxygen of [CuLt-Bu] was shown to participate in the axial interaction with the molybdenum(II) dinuclear core to assemble the component complex units, giving the supramolecular chain structure (Fig. 1).","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2018-12-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42543171","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}