X-ray Structure Analysis Online
Online ISSN : 1883-3578
ISSN-L : 1883-3578
Current issue
Showing 1-23 articles out of 23 articles from the selected issue
Part 1
Part 2
Part 3
Part 4
Part 5
  • Takayoshi FUJII, Megumi KURIBAYASHI, Kanji KUBO
    2021 Volume 37 Pages 21-23
    Published: May 10, 2021
    Released: May 10, 2021
    JOURNAL FREE ACCESS
    Supplementary material

    The structure of 1,3-diphenyl-2,3-dihydro-1H-benzo[d][1,3]dithiole-1,3-dinium bis(tetrafluoroborate) acetonitrile solvate (1) was determined by X-ray crystallography. It crystallizes in the space group P1 (#2) with cell parameters a = 8.3368(2)Å, b = 8.9193(2)Å, c = 16.7407(4)Å, α = 79.659(2)°, β = 77.822(2)°, γ = 78.551(2)°, Z = 2, and 1180.22(5)Å3. The R1(I > 2σ(I)) and wR2 (all data) values are 0.0770 and 0.2579, respectively. The structure of 1 consists of [C19H16S2]2+ and 2BF4 ion pair with CH3CN. Intermolecular C–H···F, C–H···N interactions, S···F, C···F contacts were observed in the crystal lattice.

    Download PDF (592K)
  • Ryoji MITSUHASHI
    2021 Volume 37 Pages 25-26
    Published: May 10, 2021
    Released: May 10, 2021
    JOURNAL FREE ACCESS
    Supplementary material

    The crystal structure of a pseudo-tetrahedral zinc(II) complex with a 2-(2-imidazolinyl)-6-methoxy phenolate ligand was determined by X-ray crystallography. The title compound was synthesized by a reaction of ZnCl2 and 2-(2-imidazolinyl)-6-methoxyphenolate in methanol. The compound crystallizes in the monoclinic space group P21/c and Z= 4 with cell parameters a = 14.6485(5)Å, b = 19.2428(6)Å, c = 7.5851(3)Å, β = 104.253(4)°, V = 2072.26(13)Å3. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0304 and 0.0833, respectively, for all 4597 independent reflections. The title compound was found to take the bis-bidentate coordination mode. Intermolecular hydrogen-bonds were formed between the complexes to form a dimeric structure. Furthermore, hydrogen-bonds were formed between the dimer and a methanal molecule of crystallization to construct one-dimensional chain networks.

    Download PDF (1146K)
Part 6
Part 7
Part 8
  • Emmanuel MARFO-OWUSU, Amber L. THOMPSON
    2021 Volume 37 Pages 39-40
    Published: August 10, 2021
    Released: August 10, 2021
    JOURNAL FREE ACCESS
    Supplementary material

    A tetrapentylammonium chloride complex with rac-1,1′-bi-2-naphthol entraps solvent (acetonitrile) molecules during crystallization. It crystallizes in monoclinic space group P21/n, with unit-cell parameters of; a = 13.5728(2)Å, b = 21.5734(3)Å, c = 14.1231(2)Å, β = 109.2852(7)°, V = 3903.35(10)Å3, and Z = 4. Conformational adjustments occur in the binaphthol molecule, and the alkyl chains of tetrapentylammonium chloride due to size of the counter anion, and the solvent in the hydrogen-bonded binaphthol cavity. The structure is stabilized by, Coulombic interaction, strong and weak H-bonds.

    Download PDF (106K)
  • Masahiro MIKURIYA, Sayuri ONO, Yoshiki KOYAMA, Ryoji MITSUHASHI, Motoh ...
    2021 Volume 37 Pages 41-43
    Published: August 10, 2021
    Released: August 10, 2021
    JOURNAL FREE ACCESS
    Supplementary material

    A hexanuclear MnII2MnIII4 complex with 2-(5-nitro-2-hydroxyphenyl)-1,3-bis(2-(5-nitro-2-hydroxybenzylideneamino)ethyl)imidazolidine (H3LNO2) and its hydrolyzed ligand, 1,10-bis(5-nitrosalicylideneamino)-4,7-azadecane (H2LNO2′), was isolated. The crystal structure was determined by the single-crystal X-ray diffraction method at 90 K. The complex crystallized as [{Mn33-O)(μ-CH3COO)2(μ-LNO2)}2(LNO2′)]·2.5THF·CH3OH in the monoclinic space group C2/c with a = 21.253(3), b = 16.630(2), c = 29.508(4)Å, β = 93.147(2)°, V = 10413(2)Å3, Dcalcd = 1.551 g/cm3, Z = 4. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0836 and 0.2500, respectively, for all 11924 independent reflections. The complex is a hexanuclear manganese molecule which has a crystallographic inversion center at the midpoint of the ethylenediamine backbone of LNO22− ligand. In the asymmetric unit, three manganese atoms (Mn1, Mn2, and Mn3) are arranged in a μ3-oxido-centered triangle, and the Mn1 and Mn2 atoms are further bridged by a phenolato-oxygen atom of LNO23−, and both of the Mn1 and Mn3 atoms and the Mn2 and Mn3 atoms are further bridged by an acetato ligand in a syn-syn mode. The charge balance and a bond valence sum calculation supported the mixed-valent MnII2MnIII4 state with the MnII state for the Mn1 atom and the MnIII state for the Mn2 and Mn3 atoms, respectively.

    Download PDF (1822K)
  • Mustafa TOMBUL, Elmas TÜRKMENOGLU, Onur SAHIN
    2021 Volume 37 Pages 45-47
    Published: August 10, 2021
    Released: August 10, 2021
    JOURNAL FREE ACCESS
    Supplementary material

    The structure of the reaction product of boric acid, chloral hydrate, and potassium carbonate in H2O, potassium bis(carbonato)borate hydrate K[B(CO2-μ-O-CO2)2]·2H2O, was determined by X-ray crystallography. The compound crystallized in the orthorhombic system, and was characterized to be in the space group Aba2, with cell parameters of a = 11.0579(10)Å, b = 11.1695(10)Å, c = 9.0504(9)Å, Z = 4, and V = 1117.83(18)Å3. In the crystal structure, intermolecular O–H···O hydrogen bonds link the molecules into a supramolecular structure, in which they may be effective in stabilizing the structure. The B atom espouses a distorted tetrahedral geometry with four O atoms of carbonate ligands.

    Download PDF (895K)
Part 9
  • Masahiro MIKURIYA, Chihiro YAMAKAWA, Kensuke TANABE, Raigo NUKITA, Dai ...
    2021 Volume 37 Pages 49-51
    Published: September 10, 2021
    Released: September 10, 2021
    JOURNAL FREE ACCESS
    Supplementary material

    A dinuclear copper(II) carboxylate with 2,3,6-trimethoxybenzoic acid (H236-tmbz), tetrakis(μ-2,3,6-trimethoxybenzoato-κOO′)bis[(methanol)copper(II)], [Cu2(236-tmbz)4(CH3OH)2], was prepared, and the crystal structure was determined by a single-crystal X-ray structure analysis at 90 K. It crystallizes in the triclinic space group P1 with a = 7.4282(11)Å, b = 12.2389(18)Å, c = 13.3158(19)Å, α = 115.128(2)°, β = 95.396(3)°, γ = 91.086(2)°, V = 1088.8(3)Å3, Dx = 1.580 g/cm3, and Z = 1. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0513 and 0.1207, respectively, for all 4894 independent reflections. The two copper atoms are bridged by four 2,3,6-trimethoxybenzoato ligands in a syn-syn mode to form a dinuclear cluster (Cu···Cu 2.6071(8)Å) with the apical methanol molecules. The benzoate phenyl rings are largely rotated to the bridging OCO moieties with a rotation angle (ϕrot) of 74.9(2) and 44.6(3)°.

    Download PDF (1801K)
  • Mari TOYAMA, Noriharu NAGAO
    2021 Volume 37 Pages 53-55
    Published: September 10, 2021
    Released: September 10, 2021
    JOURNAL FREE ACCESS
    Supplementary material

    The crystal structure of a 2-(pyridin-2-ylamino)pyridinium trifluoromethanesulfonate, H2dpa(OTf ) (OTf = CF3SO3), which consisted of a protonated 2-(pyridin-2-ylamino)pyridine (Hdpa) cation and a trifluoromethanesulfonate anion, was elucidated at 173 K by the single-crystal X-ray diffraction method. The compound crystallized in the monoclinic space group P21/m with a = 7.6770(4), b = 9.6170(5), c = 9.2748(5)Å, β = 106.201(6)°, Z = 2, V = 657.56(6)Å3. The R1 and wR2 values were 0.0461 and 0.1223, respectively, for 1887 reflections.

    Download PDF (236K)
  • Kirara SUGIURA, Yoshimi ICHIMARU, Koichi KATO, Masanori IMAI, Hiromasa ...
    2021 Volume 37 Pages 57-58
    Published: September 10, 2021
    Released: September 10, 2021
    JOURNAL FREE ACCESS
    Supplementary material

    The structure of 2-(1-benzoylazetidin-3-yl)thio-1,3-thiazoline was determined by the single-crystal X-ray diffraction method at 93.15 K. It crystallizes in the orthorhombic space group P212121 with a = 6.10680(10), b = 12.9876(3), c = 16.2388(3), V = 1287.94(4), and Z = 4. The R1 [I > 2σ(I)] and wR2 (all data) values were 0.0356 and 0.0938, respectively, for all 2343 independent reflections. In the crystal structure, the title compound might form CH···π interactions intermolecularly.

    Download PDF (197K)
Part 10
  • Vahobjon SABIROV, Mannon JUMAEV, Djumanali IRKABAEV, Jamshid ASHUROV
    2021 Volume 37 Pages 59-60
    Published: October 10, 2021
    Released: October 10, 2021
    JOURNAL FREE ACCESS
    Supplementary material

    The crystal structures of two chalcanthites, (Cu0.90Fe0.10)SO4·5H2O (I) and (Cu0.80Fe0.20)SO4·5H2O (II), were determined by single-crystal X-ray diffraction at room temperature. The crystallographic data are (I), triclinic P1, Z = 2, a = 5.9642(3), b = 6.1186(3), c = 10.7128(5)Å, α = 77.340(4), β = 82.384(4), γ = 72.633(4)°, V = 363.13(3)Å3, R = 0.036; (II), triclinic P1, Z = 2, a = 5.9611(6), b = 6.1270(6), c = 10.7101(9)Å, α = 77.200(8), β = 82.314(8), γ = 72.484(9)°, V = 362.82(6)Å3, R = 0.0701. Both of the crystal structures are isostructural with chalcanthite, CuSO4·5H2O, and composed of the square-planar [Cu(H2O)4]2+ ion at the M1 site and the [(Cu,Fe)(H2O)4]2+ ion at the M2 site, and the SO4 tetrahedra which acts as a μ2-bridge between these sites and one water molecule crystallization. However, unlike chalcanthite, in both crystals aqua ligands at the M2 site are disordered over two positions, and in the second crystal the O atoms of sulfate group are disordered over two positions. The O atoms of the disordered aqua ligands surrounding the Cu2 atom are with occupation factors 0.42(4)/0.58(4) and 0.47(2)/0.53(2) for structure (I), and, 0.50(7)/0.50(7) and 0.7(1)/0.3(1) for structure (II).

    Download PDF (156K)
  • Shusaku WADA, Daisuke YOSHIOKA, Motohiro TSUBOI, Masahiro MIKURIYA
    2021 Volume 37 Pages 61-63
    Published: October 10, 2021
    Released: October 10, 2021
    JOURNAL FREE ACCESS
    Supplementary material

    Dinuclear zinc(II) complex with 1,4,8,11-tetrakis(salicylideneaminoethyl)-1,4,8,11-tetraazacyclotetradecane (H4tsaec), [Zn2(tsaec)]·2CHCl3, was synthesized. The crystal structure was determined by the single-crystal X-ray diffraction method at 293 K. The complex crystallizes in the monoclinic space group P21/c with a = 9.496(3), b = 11.568(3), c = 23.338(7)Å, β = 96.270(4)°, V = 2548.3(12)Å3, Dcalcd = 1.505 g/cm3, Z = 2. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0407 and 0.1034, respectively, for all 6119 independent reflections. The two zinc(II) atoms are bound to the tsaec ligand outside the central teraazacyclotetradecane ring with an intramolecular Zn···Zn distance of 9.426(2)Å, where each zinc(II) atom is coordinated by two Schiff-base pendant arms with two phenolato-oxygen and two imino-nitrogen atoms to form a distorted tetrahedral geometry.

    Download PDF (1376K)
  • Jean GUILLON, Noël PINAUD, Solène SAVRIMOUTOU, Mathieu MARCHIVIE, Stép ...
    2021 Volume 37 Pages 65-67
    Published: October 10, 2021
    Released: October 10, 2021
    JOURNAL FREE ACCESS
    Supplementary material

    The X-ray crystal structure of the antimalarial 1-(3-ferrocenyl-2-methylpyrrolo[1,2-a]quinoxalin-4-yl)piperazin-4-ium chloride has been established. It crystallizes in the tetragonal space group P-421c with cell parameters a = 24.6705(19)Å, b = 24.6705(19)Å, c = 7.4533(6)Å, α = 90°, β = 90°, γ = 90° V = 4536.3(8)Å3 and Z = 8. The crystal structure was refined to final values of R1 = 0.0354 and wR2 = 0.0837. An X-ray crystal structure analysis revealed that each molecule features intermolecular N–H···Cl hydrogen bonds interactions between the ammonium group and the chloride anion to form tetramers.

    Download PDF (341K)
feedback
Top