Pub Date : 2021-03-10DOI: 10.2116/XRAYSTRUCT.37.13
Naho Shinde, Ryunosuke Handa, H. Furutachi, Y. Sakata, Shigehisa Akine, S. Fujinami, Masatatsu Suzuki
The bimetallic active centers of metalloproteins exhibit versatile roles; model studies using simple dinuclear metal complexes are important in order to gain insight into the biological functions of such bimetallic cores.1–5 The end-off type dinucleating ligands, having a phenolic and alcoholic oxygen as an endogenous bridge, have been used for modeling carboxylate-bridged bimetallic active sites of metalloproteins.1–5 Previously, we reported on the synthesis and characterization of a peroxo complex, [Co2(tpdb)(O2)(CH3CO2)], and a mixed-valence complex, [FeFe(tpdb)(C6H5CO2)2], having an unsymmetric dinucleating ligand with pyridyl groups (tpdb) as models for hemerythrin and purple acid phosphatase. In this paper, we report on the crystal structure of a dicobalt(II, III) mixed-valence complex, [CoII Co(tpdb)(CH3CO2)(CH3O)](ClO4)2·0.75CH3OH· 0.25CH3CN (1) (Fig. 1), which was obtained by an oxidative degradation of [Co2(tpdb)(CH3CO2)] in methanol/acetonitrile at ambient temperature under air. A mixture of Co(ClO4)2·6H2O (0.366 g, 1.0 mmol) and Htpdb (0.235 g, 0.5 mmol) in methanol/acetonitrile (3:1, 12 mL) was added to a methanol solution (5 mL) containing CH3CO2Na·3H2O (0.07 g, 0.5 mmol) and triethylamine (69 μL, 0.5 mmol) to give a dark-brown solution. Oxygen gas was bubbled for 5 min into the solution. The resulting dark-brown solution was allowed to stand for several weeks at ambient temperature under air to give single crystals of [CoCo(tpdb)(CH3CO2)(CH3O)](ClO4)2· 0.75CH3OH· 0.25CH3CN (1) suitable for X-ray crystallography. Yield: 0.28 g, 63 % (Anal. Found: C, 41.20; H, 4.37; N, 9.28%. Calcd for [CoCo(tpdb)(CH3CO2)(CH3O)](ClO4)2·1.5H2O, C31H40Cl2Co2N6O13.5: C, 41.30; H, 4.47; N, 9.32%.). It was picked up from the solution by a loop on a hand-made cold copper plate mounted inside a liquid N2 Dewar vessel at –80°C; the loop was mounted on the diffractometer. X-ray diffraction measurements were made on a Bruker D8 VENTURE diffractometer (Cu Kα radiation) at 90 K. The structure was solved by a direct method (SHELXT)8 and expanded using a Fourier technique. The structure was refined by a full-matrix least-squares method by using SHELXL 20149 (Yadokari-XG).10 All non-hydrogen atoms were refined with anisotropic displacement parameters. The hydrogen atoms were included using a riding model. For the disordered anion and solvent molecules, occupancy factors were refined using distance/ADP restraints. The crystal data are summarized in Table 1. The X-ray crystallography of 1 reveals that the asymmetric unit contains a complex cation [CoCo(tpdb)(CH3CO2) (CH3O)], two ClO4, and 0.75 methanol and 0.25 acetonitrile molecule (Fig. S1). An ORTEP drawing of the complex cation, [CoCo(tpdb)(CH3CO2)(CH3O)] of 1, is shown in Fig. 2. Selected bond distances (Å) and angle (°) are given in Table 2. The complex cation of 1 has distinct cobalt centers that are triply bridged by alkoxo oxygens of tpdp and methoxo, and acetate group as found for closely related dicobalt(I
{"title":"Synthesis and Crystal Structure of (μ-Acetato)bis(μ-Alkoxo)dicobalt(II, III) Complex with an Unsymmetric Dinucleating Ligand","authors":"Naho Shinde, Ryunosuke Handa, H. Furutachi, Y. Sakata, Shigehisa Akine, S. Fujinami, Masatatsu Suzuki","doi":"10.2116/XRAYSTRUCT.37.13","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.37.13","url":null,"abstract":"The bimetallic active centers of metalloproteins exhibit versatile roles; model studies using simple dinuclear metal complexes are important in order to gain insight into the biological functions of such bimetallic cores.1–5 The end-off type dinucleating ligands, having a phenolic and alcoholic oxygen as an endogenous bridge, have been used for modeling carboxylate-bridged bimetallic active sites of metalloproteins.1–5 Previously, we reported on the synthesis and characterization of a peroxo complex, [Co2(tpdb)(O2)(CH3CO2)], and a mixed-valence complex, [FeFe(tpdb)(C6H5CO2)2], having an unsymmetric dinucleating ligand with pyridyl groups (tpdb) as models for hemerythrin and purple acid phosphatase. In this paper, we report on the crystal structure of a dicobalt(II, III) mixed-valence complex, [CoII Co(tpdb)(CH3CO2)(CH3O)](ClO4)2·0.75CH3OH· 0.25CH3CN (1) (Fig. 1), which was obtained by an oxidative degradation of [Co2(tpdb)(CH3CO2)] in methanol/acetonitrile at ambient temperature under air. A mixture of Co(ClO4)2·6H2O (0.366 g, 1.0 mmol) and Htpdb (0.235 g, 0.5 mmol) in methanol/acetonitrile (3:1, 12 mL) was added to a methanol solution (5 mL) containing CH3CO2Na·3H2O (0.07 g, 0.5 mmol) and triethylamine (69 μL, 0.5 mmol) to give a dark-brown solution. Oxygen gas was bubbled for 5 min into the solution. The resulting dark-brown solution was allowed to stand for several weeks at ambient temperature under air to give single crystals of [CoCo(tpdb)(CH3CO2)(CH3O)](ClO4)2· 0.75CH3OH· 0.25CH3CN (1) suitable for X-ray crystallography. Yield: 0.28 g, 63 % (Anal. Found: C, 41.20; H, 4.37; N, 9.28%. Calcd for [CoCo(tpdb)(CH3CO2)(CH3O)](ClO4)2·1.5H2O, C31H40Cl2Co2N6O13.5: C, 41.30; H, 4.47; N, 9.32%.). It was picked up from the solution by a loop on a hand-made cold copper plate mounted inside a liquid N2 Dewar vessel at –80°C; the loop was mounted on the diffractometer. X-ray diffraction measurements were made on a Bruker D8 VENTURE diffractometer (Cu Kα radiation) at 90 K. The structure was solved by a direct method (SHELXT)8 and expanded using a Fourier technique. The structure was refined by a full-matrix least-squares method by using SHELXL 20149 (Yadokari-XG).10 All non-hydrogen atoms were refined with anisotropic displacement parameters. The hydrogen atoms were included using a riding model. For the disordered anion and solvent molecules, occupancy factors were refined using distance/ADP restraints. The crystal data are summarized in Table 1. The X-ray crystallography of 1 reveals that the asymmetric unit contains a complex cation [CoCo(tpdb)(CH3CO2) (CH3O)], two ClO4, and 0.75 methanol and 0.25 acetonitrile molecule (Fig. S1). An ORTEP drawing of the complex cation, [CoCo(tpdb)(CH3CO2)(CH3O)] of 1, is shown in Fig. 2. Selected bond distances (Å) and angle (°) are given in Table 2. The complex cation of 1 has distinct cobalt centers that are triply bridged by alkoxo oxygens of tpdp and methoxo, and acetate group as found for closely related dicobalt(I","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44155383","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, Sayuri Ono, Yoshiki Koyama, R. Mitsuhashi, M. Tsuboi
C7, N1, O2, O3, and O7 atoms to form a dinuclear manganese molecule A dinuclear manganese(III) complex with 2-(5-nitro-2-hydroxyphenyl)-1,3-bis(2-(5-nitro-2-hydroxybenzylideneamino)-ethyl)imidazolidine (H 3 L NO2 ) was synthesized. The crystal structure was determined by the single-crystal X-ray diffraction method at 90 K. The complex crystallized as [(C 2 H 5 ) 3 NH][Mn 2 ( μ -L NO2 )( μ -O)Br 2 ]·2THF in the orthorhombic space group Pnma with a = 14.890(2), b = 20.903(3), c = 14.7765(19)Å, V = 4599.3(11)Å 3 , D calcd = 1.621 g/cm 3 , Z = 4. The R 1 [ I > 2 σ ( I )] and wR 2 (all data) values are 0.0539 and 0.1260, respectively, for all 5416 independent reflections. The two manganese(III) atoms are bridged by a phenolato-oxygen atom of L NO23– and a μ -oxido-oxygen atom, where each manganese(III) atom is further coordinated by phenolato-oxygen, imino- and imidazolidine-nitrogen atoms of L NO2
合成了双核锰(III)与2-(5-硝基-2-羟基苯基)-1,3-二(2-(5-硝基-2-羟基苄基氨基)-乙基)咪唑烷(h3l NO2)配合物。在90k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Pnma中结晶为[(c2h 5) 3nh][Mn 2 (μ -L NO2)(μ -O)Br 2]·2THF, a = 14.890(2)， b = 20.903(3)， C = 14.7765(19)Å， V = 4599.3(11)Å 3, D calcd = 1.621 g/cm 3, Z = 4。所有5416个独立反射的R 1 [I > 2 σ (I)]和wR 2(所有数据)值分别为0.0539和0.1260。两个锰(III)原子由L NO23 -的酚氧原子和μ -氧化氧原子桥接，其中每个锰(III)原子进一步由L NO2的酚氧原子、亚胺原子和咪唑烷氮原子配位
{"title":"Crystal Structure of μ-Oxido-μ-phenolato-bridged Dinuclear Manganese(III) Complex of Schiff-base Ligand with Bromido Coordination","authors":"M. Mikuriya, Sayuri Ono, Yoshiki Koyama, R. Mitsuhashi, M. Tsuboi","doi":"10.2116/XRAYSTRUCT.37.9","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.37.9","url":null,"abstract":"C7, N1, O2, O3, and O7 atoms to form a dinuclear manganese molecule A dinuclear manganese(III) complex with 2-(5-nitro-2-hydroxyphenyl)-1,3-bis(2-(5-nitro-2-hydroxybenzylideneamino)-ethyl)imidazolidine (H 3 L NO2 ) was synthesized. The crystal structure was determined by the single-crystal X-ray diffraction method at 90 K. The complex crystallized as [(C 2 H 5 ) 3 NH][Mn 2 ( μ -L NO2 )( μ -O)Br 2 ]·2THF in the orthorhombic space group Pnma with a = 14.890(2), b = 20.903(3), c = 14.7765(19)Å, V = 4599.3(11)Å 3 , D calcd = 1.621 g/cm 3 , Z = 4. The R 1 [ I > 2 σ ( I )] and wR 2 (all data) values are 0.0539 and 0.1260, respectively, for all 5416 independent reflections. The two manganese(III) atoms are bridged by a phenolato-oxygen atom of L NO23– and a μ -oxido-oxygen atom, where each manganese(III) atom is further coordinated by phenolato-oxygen, imino- and imidazolidine-nitrogen atoms of L NO2","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-02-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42667355","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, Sayuri Ono, Yoshiki Koyama, R. Mitsuhashi, M. Tsuboi
A μ -phenolato- μ -oxido-bridged dinuclear manganese(III) complex with 2-(5-nitro-2-hydroxyphenyl)-1,3-bis(2-(5-nitro-2-hydroxybenzylideneamino)ethyl)imidazolidine (H 3 L NO2 ) was synthesized. The crystal structure was determined by the single-crystal X-ray diffraction method at 90 K. The complex crystallized as [(C 2 H 5 ) 3 NH][Mn 2 ( μ -L NO2 )( μ -O)Cl 2 ]·2THF in the orthorhombic space group Pnma with a = 15.052(3), b = 20.449(4), c = 14.700(3)Å, V = 4524.5(16)Å 3 , D calcd = 1.518 g/cm 3 , Z = 4. The R 1 [ I > 2 σ ( I )] and wR 2 (all data) values are 0.0713 and 0.1700, respectively, for all 5336 independent reflections. The two manganese(III) atoms are bridged by a phenolato-oxygen atom of L NO23– and a μ -oxido-oxygen atom, where each manganese(III) atom is further coordinated by phenolato-oxygen, imino- and imidazolidine-nitrogen atoms of L NO23– in a meridional fashion and a chlorido ligand to form a distorted octahedral geometry.
合成了一种μ -苯酚- μ -氧化桥接的2-(5-硝基-2-羟基苯基)-1,3-双(2-(5-硝基-2-羟基苄基氨基)乙基)咪唑烷(h3l NO2)双核锰配合物。在90k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Pnma中结晶为[(c2h5) 3nh][Mn 2(μ -L NO2)(μ -O)Cl 2]·2THF, a = 15.052(3)， b = 20.449(4)， C = 14.700(3)Å， V = 4524.5(16)Å 3, D calcd = 1.518 g/cm 3, Z = 4。所有5336个独立反射的R 1 [I > 2 σ (I)]和wR 2(所有数据)值分别为0.0713和0.1700。两个锰(III)原子由L NO23 -的酚氧原子和μ -氧化氧原子桥接，其中每个锰(III)原子进一步由L NO23 -的酚氧、亚胺和咪唑氮原子以子午方式和氯配体配位，形成扭曲的八面体几何形状。
{"title":"Crystal Structure of a μ-Phenolato-μ-oxido-bridged Dinuclear Manganese(III) Complex with Dinucleating Schiff-base Ligand Having Three Phenolate Groups","authors":"M. Mikuriya, Sayuri Ono, Yoshiki Koyama, R. Mitsuhashi, M. Tsuboi","doi":"10.2116/XRAYSTRUCT.37.3","DOIUrl":"https://doi.org/10.2116/XRAYSTRUCT.37.3","url":null,"abstract":"A μ -phenolato- μ -oxido-bridged dinuclear manganese(III) complex with 2-(5-nitro-2-hydroxyphenyl)-1,3-bis(2-(5-nitro-2-hydroxybenzylideneamino)ethyl)imidazolidine (H 3 L NO2 ) was synthesized. The crystal structure was determined by the single-crystal X-ray diffraction method at 90 K. The complex crystallized as [(C 2 H 5 ) 3 NH][Mn 2 ( μ -L NO2 )( μ -O)Cl 2 ]·2THF in the orthorhombic space group Pnma with a = 15.052(3), b = 20.449(4), c = 14.700(3)Å, V = 4524.5(16)Å 3 , D calcd = 1.518 g/cm 3 , Z = 4. The R 1 [ I > 2 σ ( I )] and wR 2 (all data) values are 0.0713 and 0.1700, respectively, for all 5336 independent reflections. The two manganese(III) atoms are bridged by a phenolato-oxygen atom of L NO23– and a μ -oxido-oxygen atom, where each manganese(III) atom is further coordinated by phenolato-oxygen, imino- and imidazolidine-nitrogen atoms of L NO23– in a meridional fashion and a chlorido ligand to form a distorted octahedral geometry.","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2021-01-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48866486","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 : 2020-12-10DOI: 10.2116/xraystruct.36.49
U. Osman, Sharmili Silvarajoo, I. Bhat, M. Razali, Mohd Zul Helmi Rozaini, T. B. Ravoof
The present compound, namely ( Z )-4-[4-fluorophenyl]thiosemicarbazide, crystallized in a monoclinic space group, P 2 1 / c , with cell parameters a = 12.1056(8)Å, b = 5.5177(4)Å, c = 12.5617(8)Å, β = 90.063(2) ° , V = 839.06(10)Å 3 , and Z = 4. The structure was solved and the data was refined to reach R and wR indices of 0.0946 and 0.1377, respectively. In the crystal, each molecule was linked to the next molecule by two N–H···S intermolecular hydrogen bonds.
该化合物(Z)-4-[4-氟苯基]硫代氨基脲在单斜空间群p21 / c中结晶，晶胞参数为a = 12.1056(8)Å， b = 5.5177(4)Å， c = 12.5617(8)Å， β = 90.063(2)°，V = 839.06(10)Å 3, Z = 4。对结构进行求解，对数据进行细化，得到R和wR指数分别为0.0946和0.1377。在晶体中，每个分子通过两个N-H···S分子间氢键连接到下一个分子。
{"title":"Crystal Structure of (Z)-4-[4-Fluorophenyl]thiosemicarbazide4","authors":"U. Osman, Sharmili Silvarajoo, I. Bhat, M. Razali, Mohd Zul Helmi Rozaini, T. B. Ravoof","doi":"10.2116/xraystruct.36.49","DOIUrl":"https://doi.org/10.2116/xraystruct.36.49","url":null,"abstract":"The present compound, namely ( Z )-4-[4-fluorophenyl]thiosemicarbazide, crystallized in a monoclinic space group, P 2 1 / c , with cell parameters a = 12.1056(8)Å, b = 5.5177(4)Å, c = 12.5617(8)Å, β = 90.063(2) ° , V = 839.06(10)Å 3 , and Z = 4. The structure was solved and the data was refined to reach R and wR indices of 0.0946 and 0.1377, respectively. In the crystal, each molecule was linked to the next molecule by two N–H···S intermolecular hydrogen bonds.","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2020-12-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44213278","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 : 2020-11-10DOI: 10.2116/xraystruct.36.45
Marco Blangetti, D. O’Shea
A racemic mixture of planar chiral 4-iodo-5-methoxy[2.2]metacylophane ( 2 ) was synthesized by the low-temperature directed ortho aryl metalation of 5-methoxy[2.2]metacyclophane ( 1 ) and subsequent in situ reaction with iodine. The crystal structure was determined by the single-crystal X-ray diffraction method at 100 K. The compound crystallized in an orthorhombic system and was characterized as: Pca 2 1 , a = 13.5690(2), b = 14.2212(2), c = 7.5004(1)Å, Z = 4, V = 1447.33(4)Å 3 . The crystal structure was solved by direct methods and refined by full-matrix least-squares
采用5-甲氧基[2.2]元环烷(1)的低温定向邻芳基金属化反应，与碘原位反应，合成了平面手性4-碘-5-甲氧基[2.2]元环烷(2)的外消旋混合物。在100 K下用单晶x射线衍射法测定了晶体结构。该化合物在正交晶系中结晶，表征为:Pca 21, a = 13.5690(2)， b = 14.2212(2)， c = 7.5004(1)Å， Z = 4, V = 1447.33(4)Å 3。晶体结构采用直接法求解，并用全矩阵最小二乘法进行细化
{"title":"Crystal Structure of rac-4-Iodo-5-methoxy[2.2]metacylophane; A Rare Example of a Halogenated Metacyclophane with Planar Chirality","authors":"Marco Blangetti, D. O’Shea","doi":"10.2116/xraystruct.36.45","DOIUrl":"https://doi.org/10.2116/xraystruct.36.45","url":null,"abstract":"A racemic mixture of planar chiral 4-iodo-5-methoxy[2.2]metacylophane ( 2 ) was synthesized by the low-temperature directed ortho aryl metalation of 5-methoxy[2.2]metacyclophane ( 1 ) and subsequent in situ reaction with iodine. The crystal structure was determined by the single-crystal X-ray diffraction method at 100 K. The compound crystallized in an orthorhombic system and was characterized as: Pca 2 1 , a = 13.5690(2), b = 14.2212(2), c = 7.5004(1)Å, Z = 4, V = 1447.33(4)Å 3 . The crystal structure was solved by direct methods and refined by full-matrix least-squares","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2020-11-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46173223","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 : 2020-11-10DOI: 10.2116/xraystruct.36.47
N. Nakamura, Yoshimi Ichimaru, Koichi Kato, M. Sano, H. Kurosaki, K. Hayashi, S. Miyairi
HyPix3000 diffractometer using graphite monochromated Cu- K α radiation K. crystal and experimental data Table The initial structure was solved by an intrinsic phasing method with SHELXT-2015. 8 All non-hydrogen atoms were refined using a full-matrix least-squares method on an F 2 utilizing SHELXL-2015. 9 All calculations were performed using Olex2 crystallographic software. 10 The residual electron density peaks, which may be from an EtOH molecule, were observed in the void area. The oxygen atoms in the EtOH molecules were disordered into four positions (O A–D ) with occupation factors of 0.333 (O A and O C ) The structure of 5-methoxyindirubin 3 ′ -oxime was determined by a single-crystal X-ray diffraction method at 93.15 K. The compound was crystallized in a monoclinic system, and was characterized as thus: P 2 1 / c , a = 16.0352(4)Å, b = 5.55140(10)Å, c = 17.2061(4)Å, β = 100.324(3) ° , Z = 4, and V = 1506.85(6)Å 3 . The crystal structure was solved by direct methods and refined by full-matrix least-squares on an F 2 to final values of R 1 = 0.0524 ( I > 2 σ ( I )) and wR 2 = 0.1411 (all data). 5-Methoxyindirubin
hyix3000衍射仪采用石墨单铬化Cu- K α辐射K晶体和实验数据表。8使用SHELXL-2015在f2上使用全矩阵最小二乘法对所有非氢原子进行细化。所有计算均使用Olex2晶体学软件进行。在空穴区观察到残留的电子密度峰，可能来自乙氧氢分子。在93.15 K下，用单晶x射线衍射法测定了5-甲氧基靛玉红3′-肟的结构。该化合物在单斜晶系中结晶，表征为:P 21 / c, a = 16.0352(4)Å， b = 5.55140(10)Å， c = 17.2061(4)Å， β = 100.324(3)°，Z = 4, V = 1506.85(6)Å 3。用直接法求解晶体结构，并用全矩阵最小二乘在f2上细化到最终值r1 = 0.0524 (I bbb_2 σ (I))， wr2 = 0.1411(所有数据)。5-Methoxyindirubin
{"title":"Crystal Structure of 5-Methoxyindirubin 3′-Oxime","authors":"N. Nakamura, Yoshimi Ichimaru, Koichi Kato, M. Sano, H. Kurosaki, K. Hayashi, S. Miyairi","doi":"10.2116/xraystruct.36.47","DOIUrl":"https://doi.org/10.2116/xraystruct.36.47","url":null,"abstract":"HyPix3000 diffractometer using graphite monochromated Cu- K α radiation K. crystal and experimental data Table The initial structure was solved by an intrinsic phasing method with SHELXT-2015. 8 All non-hydrogen atoms were refined using a full-matrix least-squares method on an F 2 utilizing SHELXL-2015. 9 All calculations were performed using Olex2 crystallographic software. 10 The residual electron density peaks, which may be from an EtOH molecule, were observed in the void area. The oxygen atoms in the EtOH molecules were disordered into four positions (O A–D ) with occupation factors of 0.333 (O A and O C ) The structure of 5-methoxyindirubin 3 ′ -oxime was determined by a single-crystal X-ray diffraction method at 93.15 K. The compound was crystallized in a monoclinic system, and was characterized as thus: P 2 1 / c , a = 16.0352(4)Å, b = 5.55140(10)Å, c = 17.2061(4)Å, β = 100.324(3) ° , Z = 4, and V = 1506.85(6)Å 3 . The crystal structure was solved by direct methods and refined by full-matrix least-squares on an F 2 to final values of R 1 = 0.0524 ( I > 2 σ ( I )) and wR 2 = 0.1411 (all data). 5-Methoxyindirubin","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":null,"pages":null},"PeriodicalIF":0.2,"publicationDate":"2020-11-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43201938","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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