Pub Date : 2022-02-10DOI: 10.2116/xraystruct.38.33
M. Mikuriya, Yoshiki Koyama, Chinatsu Kamioka, R. Mitsuhashi, M. Tsuboi
{"title":"Mixed-valent Manganese Complex with a Schiff-base Having a Di-μ4-oxido-di-μ3-oxido-di-μ3-carboxylato-hexa-μ-carboxylato-bridged MnII2MnIII6 Core","authors":"M. Mikuriya, Yoshiki Koyama, Chinatsu Kamioka, R. Mitsuhashi, M. Tsuboi","doi":"10.2116/xraystruct.38.33","DOIUrl":"https://doi.org/10.2116/xraystruct.38.33","url":null,"abstract":"","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":" ","pages":""},"PeriodicalIF":0.2,"publicationDate":"2022-02-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45061744","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}
Single-molecule magnets (SMMs) are intensively discussed as high-density storage, quantum computing, or spintronic technology.1–3 We have reported the weak SMM ability of a tetranuclear Co complex, [Co4(L1-H)4Cl2(CH3OH)2], but found that the stability of the complex depends on the coordinating solvent molecules.4 To improve the stability, we are working on the synthesis of new Co complexes in which the coordination solvents are replaced with various monodentate ligands. While an attempt was made to prepare a tetranuclear Co complex coordinated with dmpa, we obtained single crystals of [Co(L1-H)(HL1-H)dmpa]·CH3CN (1). Here, we report on the synthesis and the crystal structure of 1 (Fig. 1). The ligand H2L1-H was obtained by a literature method.5 An acetonitrile solution (10 mL) containing bis(acetylacetonato) diaquacobalt(II) (0.182 g, 0.5 mmol), H2L1-H (0.113 g, 0.5 mmol), and triethylamine (0.055 g, 0.5 mmol) was stirred at ca. 80°C for 30 min. To the obtained solution was added 4-dimethylaminopyridine (0.122 g, 1.0 mmol) with stirring. The orange precipitate was filtered off, and the filtrate was allowed to stand at room temperature. Reddish brown crystals suitable for X-ray analysis were obtained after 3 days. Yield, 0.009 g (3.0%). Measurements were made on a Rigaku VariMax Saturn CCD 724+ diffractometer with graphite-monochromated Mo-Kα radiation at 113 K. An empirical analytical absorption correction was applied. The structure was solved by direct methods (SIR92) and expanded using Fourier techniques. The nonhydrogen atoms were refined anisotropically. The alcoholic hydrogen atom, H3A, was found from Fourier peaks. The other hydrogen atoms were located at the calculated positions and refined using the riding model. The final cycle of a full-matrix least-squares refinement on F2 using SHELXL-2016 was based on observed reflections and variable parameters and converged with unweighted and weighted agreement factors of R1 (0.0483) and wR2 (0.1226).6 Details of the X-ray structure determination are listed in Table 1. An ORTEP drawing of the title complex 1 is shown in Fig. 2, and selected bond lengths and angles are provided in Table 2. The crystal structure of 1 consists of a Co atom, dianionic (L1-H)2–, monoanionic (HL1-H)–, and neutral dmpa ligands. The first ligand, (L1-H)2–, is coordinated to Co1 as a tridentate ligand with mer-manner. This coordination mode is similar to that of Co(III) units in the previously reported [Co4(L1-H)4Cl2(CH3OH)2]. The second ligand, (HL1-H)–, is bound to Co(III) as a bidentate chelate by phenoxo oxygen and imino nitrogen atoms. Only the tridentate coordination mode of (HL1-H)–, such as [Co(HL1-H)2]NO3, has been reported so far. This is the first example of the structurally analyzed bidentate coordination mode of H2L1-H. The remaining coordination site is occupied by the dmpa. The coordination geometry around the central Co atom is an octahedral with mer-N3O3 coordination environment. The bond distances between
{"title":"Synthesis and Crystal Structure of a Mononuclear Cobalt(III) Complex with 2-[(2-Hydroxymethylphenyl)iminomethyl]phenol and Dimethylaminopyridine","authors":"N. Sato, Ko Yoneda, Y. Yamada, Masayuki Koikawa","doi":"10.2116/xraystruct.38.1","DOIUrl":"https://doi.org/10.2116/xraystruct.38.1","url":null,"abstract":"Single-molecule magnets (SMMs) are intensively discussed as high-density storage, quantum computing, or spintronic technology.1–3 We have reported the weak SMM ability of a tetranuclear Co complex, [Co4(L1-H)4Cl2(CH3OH)2], but found that the stability of the complex depends on the coordinating solvent molecules.4 To improve the stability, we are working on the synthesis of new Co complexes in which the coordination solvents are replaced with various monodentate ligands. While an attempt was made to prepare a tetranuclear Co complex coordinated with dmpa, we obtained single crystals of [Co(L1-H)(HL1-H)dmpa]·CH3CN (1). Here, we report on the synthesis and the crystal structure of 1 (Fig. 1). The ligand H2L1-H was obtained by a literature method.5 An acetonitrile solution (10 mL) containing bis(acetylacetonato) diaquacobalt(II) (0.182 g, 0.5 mmol), H2L1-H (0.113 g, 0.5 mmol), and triethylamine (0.055 g, 0.5 mmol) was stirred at ca. 80°C for 30 min. To the obtained solution was added 4-dimethylaminopyridine (0.122 g, 1.0 mmol) with stirring. The orange precipitate was filtered off, and the filtrate was allowed to stand at room temperature. Reddish brown crystals suitable for X-ray analysis were obtained after 3 days. Yield, 0.009 g (3.0%). Measurements were made on a Rigaku VariMax Saturn CCD 724+ diffractometer with graphite-monochromated Mo-Kα radiation at 113 K. An empirical analytical absorption correction was applied. The structure was solved by direct methods (SIR92) and expanded using Fourier techniques. The nonhydrogen atoms were refined anisotropically. The alcoholic hydrogen atom, H3A, was found from Fourier peaks. The other hydrogen atoms were located at the calculated positions and refined using the riding model. The final cycle of a full-matrix least-squares refinement on F2 using SHELXL-2016 was based on observed reflections and variable parameters and converged with unweighted and weighted agreement factors of R1 (0.0483) and wR2 (0.1226).6 Details of the X-ray structure determination are listed in Table 1. An ORTEP drawing of the title complex 1 is shown in Fig. 2, and selected bond lengths and angles are provided in Table 2. The crystal structure of 1 consists of a Co atom, dianionic (L1-H)2–, monoanionic (HL1-H)–, and neutral dmpa ligands. The first ligand, (L1-H)2–, is coordinated to Co1 as a tridentate ligand with mer-manner. This coordination mode is similar to that of Co(III) units in the previously reported [Co4(L1-H)4Cl2(CH3OH)2]. The second ligand, (HL1-H)–, is bound to Co(III) as a bidentate chelate by phenoxo oxygen and imino nitrogen atoms. Only the tridentate coordination mode of (HL1-H)–, such as [Co(HL1-H)2]NO3, has been reported so far. This is the first example of the structurally analyzed bidentate coordination mode of H2L1-H. The remaining coordination site is occupied by the dmpa. The coordination geometry around the central Co atom is an octahedral with mer-N3O3 coordination environment. The bond distances between","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":" ","pages":""},"PeriodicalIF":0.2,"publicationDate":"2022-01-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44174323","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}
M. Mikuriya, Nagisa Tsuchimoto, Yoshiki Koyama, R. Mitsuhashi, M. Tsuboi
Schiff-base molecules, 1,3-bis(salicylideneamino)-2-propanol (H3salpr), and their substituted derivatives, are potential pentadentate ligands with two phenolato-oxygen, two iminonitrogen, and one central alcoholate-oxygen donor atoms by deprotonation with coordination to metal atoms. It is known that these Schiff-base ligands form a mononuclear copper(II) complex as a tetradentate O, N, N, O-chelate,1 and dinuclear copper(II),2 nickel(II),3 manganese(III),4 and cobalt(III)5 complexes as tridentate O, N, O-chelates. Previously, we reported on the crystal structures of a monosubstituted Schiffbase ligand, 1,3-bis(5-nitrosalicylideneamino)-2-propanol (H3nsalpr) and a disubstituted Schiff-base ligand, 1,3-bis(5chloro-3-methoxysalicylideneamino)-2-propanol (H3cmsalpr). The former has one nitro group at the salicylideneamino ring, whereas the latter has one chloro group and one methoxy group at the salicylideneamino ring. In this study, we prepared 1,3-bis(3,5-dibromosalicylideneamino)-2-propanol (H3dbsalpr), which has two bromo groups at the salicylideneamino ring (Fig. 1), and determined the crystal structure of H3dbsalpr, which has not been elucidated so far. 1,3-Diamino-2-propanol (0.646 g, 7 mmol) and 3,5-dibromosalicylaldehyde (4.00 g, 14 mmol) were dissolved in methanol (50 cm3)–acetonitrile (10 cm3). The solution was refluxed for 3 h, and then left at room temperature. The resulting yellow precipitate was filtered off, washed with methanol, and dried under a vacuum. Yield, 3.98 g (91%). IR (KBr, cm–1): 3235 (ν(OH)), 3055 (ν(CH(phenyl)), 2925 (νasCH2), 2889 (νsCH2), 1632 (νC=N). X-ray quality crystals were grown by recrystallization from acetonitrile. 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 with SHELXT-2014, and refined by full-matrix least-squares methods with SHELXL-2018. The hydrogen atoms were inserted at their calculated positions, and fixed there with restraints. The hydrogen atoms at the imino groups were also inserted at the calculated positions because it was difficult to locate the hydrogen atoms from the D-Fourier maps including the phenolate oxygen areas. For thermal anisotropic displacement parameters (ADPs) of most of the carbon atoms, enhanced rigid bond restraints were applied. Crystallographic data have been deposited with Cambridge Crystallographic Data Centre (Deposit number CCDC2091176). 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). In the crystal, the asymmetric unit consists of three independent 1,3-bis(3,5-dibromosalicylideneamino)-2-propanol, H3dbsalpr molecules, like in the case for 1,3-bis(salicy
{"title":"Crystal Structure of 1,3-Bis(3,5-dibromosalicylideneamino)-2-propanol","authors":"M. Mikuriya, Nagisa Tsuchimoto, Yoshiki Koyama, R. Mitsuhashi, M. Tsuboi","doi":"10.2116/xraystruct.38.3","DOIUrl":"https://doi.org/10.2116/xraystruct.38.3","url":null,"abstract":"Schiff-base molecules, 1,3-bis(salicylideneamino)-2-propanol (H3salpr), and their substituted derivatives, are potential pentadentate ligands with two phenolato-oxygen, two iminonitrogen, and one central alcoholate-oxygen donor atoms by deprotonation with coordination to metal atoms. It is known that these Schiff-base ligands form a mononuclear copper(II) complex as a tetradentate O, N, N, O-chelate,1 and dinuclear copper(II),2 nickel(II),3 manganese(III),4 and cobalt(III)5 complexes as tridentate O, N, O-chelates. Previously, we reported on the crystal structures of a monosubstituted Schiffbase ligand, 1,3-bis(5-nitrosalicylideneamino)-2-propanol (H3nsalpr) and a disubstituted Schiff-base ligand, 1,3-bis(5chloro-3-methoxysalicylideneamino)-2-propanol (H3cmsalpr). The former has one nitro group at the salicylideneamino ring, whereas the latter has one chloro group and one methoxy group at the salicylideneamino ring. In this study, we prepared 1,3-bis(3,5-dibromosalicylideneamino)-2-propanol (H3dbsalpr), which has two bromo groups at the salicylideneamino ring (Fig. 1), and determined the crystal structure of H3dbsalpr, which has not been elucidated so far. 1,3-Diamino-2-propanol (0.646 g, 7 mmol) and 3,5-dibromosalicylaldehyde (4.00 g, 14 mmol) were dissolved in methanol (50 cm3)–acetonitrile (10 cm3). The solution was refluxed for 3 h, and then left at room temperature. The resulting yellow precipitate was filtered off, washed with methanol, and dried under a vacuum. Yield, 3.98 g (91%). IR (KBr, cm–1): 3235 (ν(OH)), 3055 (ν(CH(phenyl)), 2925 (νasCH2), 2889 (νsCH2), 1632 (νC=N). X-ray quality crystals were grown by recrystallization from acetonitrile. 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 with SHELXT-2014, and refined by full-matrix least-squares methods with SHELXL-2018. The hydrogen atoms were inserted at their calculated positions, and fixed there with restraints. The hydrogen atoms at the imino groups were also inserted at the calculated positions because it was difficult to locate the hydrogen atoms from the D-Fourier maps including the phenolate oxygen areas. For thermal anisotropic displacement parameters (ADPs) of most of the carbon atoms, enhanced rigid bond restraints were applied. Crystallographic data have been deposited with Cambridge Crystallographic Data Centre (Deposit number CCDC2091176). 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). In the crystal, the asymmetric unit consists of three independent 1,3-bis(3,5-dibromosalicylideneamino)-2-propanol, H3dbsalpr molecules, like in the case for 1,3-bis(salicy","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":" ","pages":""},"PeriodicalIF":0.2,"publicationDate":"2022-01-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45839714","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}
James T. P. Matshwele, Sebusi Odisitse, Ofentse Mazimba, F. Nareetsile, Lebogang G Julius, Dalitso Keitumetse
placed at geometrically calculated positions and included in the least-squares calculations using the riding-atom model. Their U iso values were fixed at 1.2 U eq of The structure of pyridin-4-ylmethyl 4-nitrobenzoate was determined by the single-crystal X-ray diffraction method. The compound crystallized in a monoclinic system, P 2 1 / n , and the unit cell parameters are, a = 9.981(2), b = 12.347(3), c = 10.161(3)Å, β = 101.450(9), Z = 4, V = 1227.3(5)Å 3 . The crystal structure was solved by intrinsic phasing and refined to final values of R 1 = 0.0451 and wR 2 = 0.1393.
{"title":"Crystal Structure of Pyridin-4-ylmethyl 4-Nitrobenzoate, C13H10N2O4","authors":"James T. P. Matshwele, Sebusi Odisitse, Ofentse Mazimba, F. Nareetsile, Lebogang G Julius, Dalitso Keitumetse","doi":"10.2116/xraystruct.38.7","DOIUrl":"https://doi.org/10.2116/xraystruct.38.7","url":null,"abstract":"placed at geometrically calculated positions and included in the least-squares calculations using the riding-atom model. Their U iso values were fixed at 1.2 U eq of The structure of pyridin-4-ylmethyl 4-nitrobenzoate was determined by the single-crystal X-ray diffraction method. The compound crystallized in a monoclinic system, P 2 1 / n , and the unit cell parameters are, a = 9.981(2), b = 12.347(3), c = 10.161(3)Å, β = 101.450(9), Z = 4, V = 1227.3(5)Å 3 . The crystal structure was solved by intrinsic phasing and refined to final values of R 1 = 0.0451 and wR 2 = 0.1393.","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":" ","pages":""},"PeriodicalIF":0.2,"publicationDate":"2022-01-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46762942","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}
Pub Date : 2021-12-10DOI: 10.2116/xraystruct.37.85
Yuka Mineyama, Ko Yoneda, Y. Yamada, Masayuki Koikawa
correction was applied. The structure was solved by direct methods (SIR92) and expanded using Fourier techniques. The non-2021 The title compound, [Ni(HL1–NO 2 ) 2 ]·CH 3 CN, [H 2 L1–NO 2 = 2-[2-(hydroxymethylphenyl)iminomethyl]-4-nitrophenol], was synthesized and characterized by single-crystal X-ray analysis. The compound crystallizes in the triclinic space group P 1 with cell parameters a = 10.556(2)Å, b = 11.779(3)Å, c = 12.247(3)Å, α = 86.412(10) ° , β = 71.135(8) ° , γ = 73.009(8) ° , V = 1377.2(5)Å 3 , D calcd = 1.549 g/cm 3 , Z = 2. The R 1 [ I > 2 σ ( I )] and wR 2 (all data) values are 0.0362 and 0.1024, respectively, for all 5989 independent reflections. The tridentate ligands coordinate to the nickel atom as a mer -manner.
进行了校正。用直接法(SIR92)求解该结构，并用傅里叶技术展开。合成了非2021标题化合物[Ni(h1 - no 2) 2]·ch3 CN， [h2 L1-NO 2 = 2-[2-(羟甲基苯基)亚甲基]-4-硝基苯酚]，并用单晶x射线分析对其进行了表征。晶胞参数为a = 10.556(2)Å， b = 11.779(3)Å， c = 12.247(3)Å， α = 86.412(10)°，β = 71.135(8)°，γ = 73.009(8)°，V = 1377.2(5)Å 3, D calcd = 1.549 g/cm 3, Z = 2。5989个独立反射的R 1 [I > 2 σ (I)]和wR 2(所有数据)值分别为0.0362和0.1024。三叉戟配体与镍原子以聚合物的方式配位。
{"title":"Synthesis and Crystal Structure of Bis{2-[(2-hydroxymethylphenyl)iminomethyl]-4-nitrophenolato}nickel(II) Monoacetonitrile","authors":"Yuka Mineyama, Ko Yoneda, Y. Yamada, Masayuki Koikawa","doi":"10.2116/xraystruct.37.85","DOIUrl":"https://doi.org/10.2116/xraystruct.37.85","url":null,"abstract":"correction was applied. The structure was solved by direct methods (SIR92) and expanded using Fourier techniques. The non-2021 The title compound, [Ni(HL1–NO 2 ) 2 ]·CH 3 CN, [H 2 L1–NO 2 = 2-[2-(hydroxymethylphenyl)iminomethyl]-4-nitrophenol], was synthesized and characterized by single-crystal X-ray analysis. The compound crystallizes in the triclinic space group P 1 with cell parameters a = 10.556(2)Å, b = 11.779(3)Å, c = 12.247(3)Å, α = 86.412(10) ° , β = 71.135(8) ° , γ = 73.009(8) ° , V = 1377.2(5)Å 3 , D calcd = 1.549 g/cm 3 , Z = 2. The R 1 [ I > 2 σ ( I )] and wR 2 (all data) values are 0.0362 and 0.1024, respectively, for all 5989 independent reflections. The tridentate ligands coordinate to the nickel atom as a mer -manner.","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":" ","pages":""},"PeriodicalIF":0.2,"publicationDate":"2021-12-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42340974","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}
Pub Date : 2021-12-10DOI: 10.2116/xraystruct.37.81
M. Mikuriya, Hitomi Yamada, K. Morita, Ai Shibutani, Eiichi Nagayama, Shinya Minato, D. Yoshioka, M. Tsuboi
in A μ -phenolato- μ -chlorido-bridged dinuclear manganese(II) complex with 2,6-bis( N -(4-imidazolylethyl)iminomethyl)-4-methylphenol (Hbimmp), [Mn 2 (bimmp)( μ -Cl)Cl 2 ], was isolated. The crystal structure was determined by a single-crystal X-ray diffraction method at 293 K. The complex crystallizes in the orthorhombic space group F dd2 with a = 40.557(4), b = 9.2353(9), c = 12.5138(2)Å, V = 4687.1(8)Å 3 , D calcd = 1.603 g/cm 3 , Z = 8. The R 1 [ I > 2 σ ( I )] and wR 2 (all data) values are 0.0309 and 0.0826, respectively, for all 2683 independent reflections. The two manganese(II) atoms are bridged by a phenolato-oxygen of bimmp – and a μ -chlorido atom, where each manganese(II) atom is further coordinated by imino- and imidazolyl-nitrogen atoms of bimmp – and chlorido atoms to form a square-pyramidal geometry. (Received
从A μ -酚- μ -氯-桥接双核锰(II)与2,6-双(N -(4-咪唑乙基)亚甲基)-4-甲基苯酚(Hbimmp)配合物中分离得到[Mn 2 (bimmp)(μ -Cl)Cl 2]。在293 K下用单晶x射线衍射法测定了晶体结构。配合物在正交空间群F dd2中结晶，a = 40.557(4)， b = 9.2353(9)， c = 12.5138(2)Å， V = 4687.1(8)Å 3, D calcd = 1.603 g/cm 3, Z = 8。所有2683个独立反射的R 1 [I > 2 σ (I)]和wR 2(所有数据)值分别为0.0309和0.0826。两个锰(II)原子由一个苯基氧原子和一个μ -氯原子桥接，其中每个锰(II)原子进一步由苯基氧原子和氯原子的亚氮原子和咪唑氮原子配位，形成方形金字塔几何结构。(收到
{"title":"μ-Phenolato-μ-chlorido-bridged Dinuclear Manganese(II) Complex with a Dinucleating Schiff-base Ligand Having Imidazolyl Groups","authors":"M. Mikuriya, Hitomi Yamada, K. Morita, Ai Shibutani, Eiichi Nagayama, Shinya Minato, D. Yoshioka, M. Tsuboi","doi":"10.2116/xraystruct.37.81","DOIUrl":"https://doi.org/10.2116/xraystruct.37.81","url":null,"abstract":"in A μ -phenolato- μ -chlorido-bridged dinuclear manganese(II) complex with 2,6-bis( N -(4-imidazolylethyl)iminomethyl)-4-methylphenol (Hbimmp), [Mn 2 (bimmp)( μ -Cl)Cl 2 ], was isolated. The crystal structure was determined by a single-crystal X-ray diffraction method at 293 K. The complex crystallizes in the orthorhombic space group F dd2 with a = 40.557(4), b = 9.2353(9), c = 12.5138(2)Å, V = 4687.1(8)Å 3 , D calcd = 1.603 g/cm 3 , Z = 8. The R 1 [ I > 2 σ ( I )] and wR 2 (all data) values are 0.0309 and 0.0826, respectively, for all 2683 independent reflections. The two manganese(II) atoms are bridged by a phenolato-oxygen of bimmp – and a μ -chlorido atom, where each manganese(II) atom is further coordinated by imino- and imidazolyl-nitrogen atoms of bimmp – and chlorido atoms to form a square-pyramidal geometry. (Received","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":" ","pages":""},"PeriodicalIF":0.2,"publicationDate":"2021-12-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45499315","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}
Pub Date : 2021-12-10DOI: 10.2116/xraystruct.37.87
Yoshimi Ichimaru, Koichi Kato, Wanchun Jin, K. Sugiura, Emiko Kinoshita-Kikuta, E. Kinoshita, H. Kurosaki, T. Koike
The crystal structure of bis{1,3-bis[bis(pyridin-2-ylmethyl)amino]propan-2-olato-dizinc(II)}orthophosphate tris(perchlorate) octahydrate, [(Phos-tag) 2 -PO 43– ][ClO 4– ] 3 ·8H 2 O was determined by the single-crystal X-ray diffraction method at 93.15 K. The titled complex crystallized in the monoclinic space group C 2/c and Z = 4 with a = 16.8423(2), b = 21.3554(2), c = 19.9942(2)Å, β = 106.8690(10) ° , and V = 6881.95(13)Å 3 . The R 1 [ I > 2 σ ( I )] and wR 2 (all data) values were 0.0447 and 0.1142, respectively, for all 6253 independent reflections. In the crystal structure, each zinc(II) ion is coordinated with two pyridyl amines, a tertiary amine, an alkoxide oxygen, and a phosphate oxygen to form a trigonal bipyramidal geometry. The orthophosphate trianion connects two dinuclear zinc(II) complex (Phos-tag) in a μ 4 η 4 bridge mode.
用单晶x射线衍射法在93.15 K下测定了双{1,3-双[双(吡啶-2-甲基)氨基]丙-2-奥拉托-二锌(II)}正磷酸盐三(高氯酸盐)八水合物[(Phos-tag) 2- po 43 -][ClO 4 -] 3·8H 2o的晶体结构。在单斜空间群C 2/ C和Z = 4中结晶，a = 16.8423(2)， b = 21.3554(2)， C = 19.9942(2)Å， β = 106.8690(10)°，V = 6881.95(13)Å 3。6253个独立反射的R 1 [I > 2 σ (I)]和wR 2(所有数据)值分别为0.0447和0.1142。在晶体结构中，每个锌(II)离子与两个吡啶胺、一个叔胺、一个醇氧和一个磷酸氧配位，形成三角双锥体几何结构。正磷酸盐三阴离子以μ 4 η 4桥模式连接两个双核锌(II)配合物(Phos-tag)。
{"title":"Crystal Structure of Bis{1,3-bis[bis(pyridin-2-ylmethyl)amino]propan-2-olato-dizinc(II)}orthophosphate Tris(perchlorate) Octahydrate, [(Phos-tag)2-PO43−][ClO4−]3·8H2O","authors":"Yoshimi Ichimaru, Koichi Kato, Wanchun Jin, K. Sugiura, Emiko Kinoshita-Kikuta, E. Kinoshita, H. Kurosaki, T. Koike","doi":"10.2116/xraystruct.37.87","DOIUrl":"https://doi.org/10.2116/xraystruct.37.87","url":null,"abstract":"The crystal structure of bis{1,3-bis[bis(pyridin-2-ylmethyl)amino]propan-2-olato-dizinc(II)}orthophosphate tris(perchlorate) octahydrate, [(Phos-tag) 2 -PO 43– ][ClO 4– ] 3 ·8H 2 O was determined by the single-crystal X-ray diffraction method at 93.15 K. The titled complex crystallized in the monoclinic space group C 2/c and Z = 4 with a = 16.8423(2), b = 21.3554(2), c = 19.9942(2)Å, β = 106.8690(10) ° , and V = 6881.95(13)Å 3 . The R 1 [ I > 2 σ ( I )] and wR 2 (all data) values were 0.0447 and 0.1142, respectively, for all 6253 independent reflections. In the crystal structure, each zinc(II) ion is coordinated with two pyridyl amines, a tertiary amine, an alkoxide oxygen, and a phosphate oxygen to form a trigonal bipyramidal geometry. The orthophosphate trianion connects two dinuclear zinc(II) complex (Phos-tag) in a μ 4 η 4 bridge mode.","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":"1 1","pages":""},"PeriodicalIF":0.2,"publicationDate":"2021-12-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41530564","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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