Pub Date : 2019-11-10DOI: 10.2116/xraystruct.35.67
Ryusei Hoshikawa, R. Mitsuhashi, M. Mikuriya, H. Sakiyama
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)
{"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}
Pub Date : 2019-11-10DOI: 10.2116/xraystruct.35.63
S. Ohmura, T. Hirao, N. Miyoshi, T. Moriuchi
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.
{"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}
Pub Date : 2019-10-10DOI: 10.2116/xraystruct.35.57
Jean Guillon, Maria de Fatima Pereira-Rosenfeld, Noël Pinaud, Thierry Besson, V. Thiéry, Laurent Picot, Mathieu Marchivie
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.
建立了具有抗A2058黑色素瘤细胞增殖潜力的6,7-二氢-5a,7a,13,14-四氮杂-五苯-5,8-二酮的x射线晶体结构。晶胞参数为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, Z = 12。晶体结构细化至最终值R1 = 0.1353, wR2 = 0.1936。x射线晶体结构分析显示，每个分子都具有分子间的CArom。-H···O氢键形成三聚体。
{"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}
Pub Date : 2019-10-10DOI: 10.2116/xraystruct.35.61
Takuto Mibu, Y. Suenaga, T. Okubo, M. Maekawa, T. Kuroda–Sowa
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
{"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}
Pub Date : 2019-09-10DOI: 10.2116/xraystruct.35.51
Y. Ozawa, A. Masunaga, M. Kubo, N. Yasuda, K. Toriumi
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.
{"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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