X-ray Structure Analysis Online
Online ISSN : 1883-3578
ISSN-L : 1883-3578
Volume 36
Displaying 1-17 of 17 articles from this issue
Part 1
  • Masahiro MIKURIYA, Kazuki TANIGUCHI, Yoshiki KOYAMA, Hiroaki WATANABE, ...
    2020 Volume 36 Pages 1-2
    Published: January 10, 2020
    Released on J-STAGE: January 10, 2020
    JOURNAL FREE ACCESS
    Supplementary material

    Sulfur S8 was isolated from a reaction solution of thiourea and bismuth nitrate in N,N-dimethylformamide. The crystal structure was determined by the single-crystal X-ray diffraction method at 90 K. It crystallizes in the orthorhombic space group Fddd with a = 10.3310(8)Å, b = 12.6786(10)Å, c = 24.3519(19)Å, V = 3189.7(4)Å3, Dx = 2.136 g/cm3, and Z = 6. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0220 and 0.0570, respectively, for all 1864 independent reflections. The S8 molecule has a crown-shaped ring structure with the α-form.

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Part 2
  • Masahiro MIKURIYA, Shuichi HIROSHIMA, Yoshiki KOYAMA, Keisuke TERADA, ...
    2020 Volume 36 Pages 3-5
    Published: February 10, 2020
    Released on J-STAGE: February 10, 2020
    JOURNAL FREE ACCESS
    Supplementary material

    Sodium tetraperoxidochromate(V), Na3Cr(O2)4·14H2O, was prepared and the crystal structure was determined by the single-crystal X-ray diffraction method at 90 K. It crystallizes in the triclinic space group P1 with a = 7.5349(6)Å, b = 8.6378(7)Å, c = 8.9921(7)Å, α = 64.087(1), β = 81.565(1), γ = 69.348(1)°, V = 492.56(7)Å3, Dx = 1.690 g/cm3, and Z = 1. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0277 and 0.0722, respectively, for all 2310 independent reflections. The chromium ion is coordinated by four peroxido ligands in a distorted dodecahedral geometry, whereas each sodium ion is coordinated by six water molecules to form an octahedral Na(H2O)6 unit, which is connected by two bridging water molecules to form zigzag [cis-{Na(H2O)2(μ-H2O)4}-trans-{Na(H2O)2(μ-H2O)4}]n chain molecules in the crystal.

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Part 3
  • Masahiro MIKURIYA, Yoshiki KOYAMA, Daisuke YOSHIOKA, Ryoji MITSUHASHI
    2020 Volume 36 Pages 7-9
    Published: March 10, 2020
    Released on J-STAGE: March 10, 2020
    JOURNAL FREE ACCESS
    Supplementary material

    The di-μ-acetato-μ-alkoxido-bridged dinuclear manganese(III) complex with 1,3-bis(3-methoxysalicylideneamino)-2-propanol (H3msap), [Mn2(msap)(μ-CH3COO)2(CH3COO)(CH3OH)], was synthesized. The crystal structure was determined by the single-crystal X-ray diffraction method at 90 K. The complex crystallizes in the monoclinic space group P21/n with a = 10.4020(8), b = 22.6864(17), c = 12.1807(10)Å, β = 92.0340(10)°, V = 2872.6(4)Å3, Dcalcd = 1.559 g/cm3, Z = 4. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0495 and 0.1218, respectively, for all 6587 independent reflections. The two manganese(III) ions are bridged by alkoxido-oxygen of msap2− and two μ-acetato with a hydrogen bonding between monodentate acetato and methanol molecules.

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Part 4
  • Sami AYARI, Kazunori HIRABAYASHI, Toshio SHIMIZU, Bassem JAMOUSSI, Meh ...
    2020 Volume 36 Pages 11-13
    Published: April 10, 2020
    Released on J-STAGE: April 10, 2020
    JOURNAL FREE ACCESS
    Supplementary material

    Phthalonitrile-3-yl (PN3) substituted indole derivative 1 was structurally characterized. The compound was crystallized in a monoclinic system and characterized as follows: P21/c, a = 23.232(5), b = 7.4413(14), c = 15.361(4)Å, β = 106.818(5)°, Z = 8, V = 2542.0(10)Å3. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F2 to the final values of R1 = 0.0660 and wR2 = 0.1610. 1 has two crystallographically independent molecules in the asymmetric unit. The dihedral angle between indole and PN3 is 42.17(8)°. Theoretical studies revealed that the rotational barrier of PN3 is 8.82 kcal mol−1. 1H NMR spectroscopy demonstrated an interesting long-range spin–spin coupling between benzylic H of the methyl group and the adjacent aromatic H through four bonds with a coupling constant of 1.3 Hz (in acetone-d6). The double-bond character of the bond connecting these protons is responsible for this phenomenon.

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Part 5
Part 6
  • Masahiro MIKURIYA, Nanami WATANABE, Yoshiki KOYAMA, Daisuke YOSHIOKA, ...
    2020 Volume 36 Pages 17-19
    Published: June 10, 2020
    Released on J-STAGE: June 10, 2020
    JOURNAL FREE ACCESS
    Supplementary material

    The crystal structure of manganese(II) hexafluorosilicate hexahydrate, [Mn(H2O)6]SiF6, was determined by the single-crystal X-ray diffraction method at 90 K. The complex crystallizes in the monoclinic space group P21/c with a = 6.473(3), b = 9.639(5), c = 8.579(4)Å, β = 100.009(7)°, V = 527.2(4)Å3, Dcalcd = 1.922 g/cm3, Z = 2. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0330 and 0.0734, respectively, for all 1278 independent reflections. The manganese(II) ion is located at the crystallographic inversion center with six water molecules, each of which is disordered into two positions, forming a distorted octahedral geometry. The hexafluorosilicate ion is also located at the crystallographic inversion center with six disordered fluoride atoms. The temperature dependence of the magnetic susceptibility obeys the Curie–Weiss law with C = 4.476(2)cm3 mol−1, θ = –0.39(6)K, showing almost no magnetic interaction between the metal centers.

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Part 7
Part 8
Part 9
  • Ryoji MITSUHASHI, Masahiro MIKURIYA
    2020 Volume 36 Pages 33-34
    Published: September 10, 2020
    Released on J-STAGE: September 10, 2020
    JOURNAL FREE ACCESS
    Supplementary material

    The crystal structure of the Ru(III) complex with 2-(2-imidazolinyl)phenolate was determined by X-ray crystallography. The title compound was synthesized by a reaction of RuCl3·nH2O and 2-(2-imidazolinyl)phenolate in ethanol. The compound crystallized in the monoclinic space group P21/c and Z = 4 with cell parameters a = 10.2053(18)Å, b = 33.277(6)Å, c = 8.8733(15)Å, β = 113.904(3)°, V = 2754.9(8)Å3. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0711 and 0.1487, respectively, for all 6316 independent reflections. The title compound was found to take a meridional configuration. In the crystal, a centrosymmetric dimer structure was formed by intermolecular hydrogen-bonds between the coordinating phenolate-O atom (O2) of a ligand and a noncoordinating N–H bond (N5–H5A) in the symmetry equivalent ligand.

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  • Md Awlad HOSSAIN, Kazunori HIRABAYASHI, Tohru NISHINAGA, Toshio SHIMIZ ...
    2020 Volume 36 Pages 35-37
    Published: September 10, 2020
    Released on J-STAGE: September 10, 2020
    JOURNAL FREE ACCESS
    Supplementary material

    The molecular structure of sterically crowded 1,4,5,8-tetrabromonaphthalene 1 was refined. The compound crystallized in a monoclinic system and was characterized as follows: P21/c, a = 9.470(3), b = 15.530(4), c = 7.340(2)Å, β = 92.147(9)°, Z = 4, V = 1078.7(5)Å3. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F2 to final values of R1 = 0.0332 and wR2 = 0.0572. Because of the steric repulsion between the peri-bromines, 1 takes a twisted structure having a D2 point group, i.e., a chiral structure. Symmetry operation of this space group generates the corresponding enantiomer in the crystal. In marked contrast to the noticeably short intramolecular Br–Br contact of 3.209 Å (average), there is no short Br–Br contact intermolecularly.

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Part 10
  • Makoto HANDA, Hideaki ISHIDA, Daisuke YOSHIOKA, Fumiaki KUGITA, Ichiro ...
    2020 Volume 36 Pages 39-41
    Published: October 10, 2020
    Released on J-STAGE: October 10, 2020
    JOURNAL FREE ACCESS
    Supplementary material

    The title compound of a lantern-type ruthenium(II,III) dinuclear complex, [Ru2(O2CCMe3)4(NCS)(DMF)], was isolated and the crystal structure was determined by the single-crystal X-ray diffraction method at 293 K. It crystallizes in the monoclinc space group P21/n with a = 11.549(6)Å, b = 9.849(5)Å, c = 14.250(8)Å, β = 91.898(7)°, V = 1619.9(15)Å3, Dx = 1.513 g/cm3, and Z = 2. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0389 and 0.0916, respectively, for all 3860 independent reflections. The axial sites of the dinuclear core are occupied by NCS and DMF ligands with distances of Ru–Nax (NCS) = 2.29(3)Å and Ru–Oax (DMF) = 2.201(19)Å, respectively. The Ru–Ru distance is 2.2713(10)Å, of which the value is in the range of those for the other lantern-type diruthenium(II,III) tetracarboxylate complexes.

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  • Yoshimi ICHIMARU, Masanori IMAI, Haruto FUJIOKA, Yuhzo HIEDA, Tohru KO ...
    2020 Volume 36 Pages 43-44
    Published: October 10, 2020
    Released on J-STAGE: October 10, 2020
    JOURNAL FREE ACCESS
    Supplementary material

    The crystal structure of [3-(1,4,7,10-tetraazacyclododecan-1-yl)propan-1-amine = L]zinc(II) bis(perchlorate), [ZnIIL](ClO4)2, was determined by the single-crystal X-ray diffraction method at 93.15 K. The titled complex crystallized in the orthorhombic space group P212121 and Z = 4 with a = 9.09970(10), b = 14.0995(2), c = 14.9908(2)Å, and V = 1923.34(4)Å3. The R1 [I > 2σ(I)] and wR2 (all data) values were 0.0214 and 0.0538, respectively, for all 3079 independent reflections. In the crystal structure, the zinc center is coordinated with the three secondary amines and one tertiary amine of the macrocycle and with the primary amine from the N-propylamino pendant arm, forming a distorted square pyramidal geometry.

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Part 11
  • Marco BLANGETTI, Donal F. O’SHEA
    2020 Volume 36 Pages 45-46
    Published: November 10, 2020
    Released on J-STAGE: November 10, 2020
    JOURNAL FREE ACCESS
    Supplementary material

    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: Pca21, a = 13.5690(2), b = 14.2212(2), c = 7.5004(1)Å, Z = 4, V = 1447.33(4)Å3. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F2 to final values of R1 = 0.0281 and wR2 = 0.0733 for all 3021 independent reflections.

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  • Niina NAKAMURA, Yoshimi ICHIMARU, Koichi KATO, Makoto SANO, Hiromasa K ...
    2020 Volume 36 Pages 47-48
    Published: November 10, 2020
    Released on J-STAGE: November 10, 2020
    JOURNAL FREE ACCESS
    Supplementary material

    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: P21/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)Å3. The crystal structure was solved by direct methods and refined by full-matrix least-squares on an F2 to final values of R1 = 0.0524 (I > 2σ(I)) and wR2 = 0.1411 (all data). 5-Methoxyindirubin 3′-oxime forms three hydrogen bonds intramolecularly and intermolecularly without intervening solvent molecules.

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Part 12
  • Uwaisulqarni M. OSMAN, Sharmili SILVARAJOO, Irshad Ul Haq BHAT, Mohd H ...
    2020 Volume 36 Pages 49-50
    Published: December 10, 2020
    Released on J-STAGE: December 10, 2020
    JOURNAL FREE ACCESS
    Supplementary material

    The present compound, namely (Z)-4-[4-fluorophenyl]thiosemicarbazide, crystallized in a monoclinic space group, P21/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)Å3, 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.

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