X-ray Structure Analysis Online
Online ISSN : 1883-3578
ISSN-L : 1883-3578
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Part 1
  • Akiko ASANO, Mitsunobu DOI
    2019 Volume 35 Pages 1-2
    Published: January 10, 2019
    Released: January 10, 2019
    JOURNALS FREE ACCESS

    Gramicidin S hydrochloride [cyclic(–Val–Orn–Leu–d-Phe–Pro–)2·2HCl] was crystallized in the space group P21212 with cell parameters a = 34.988(1)Å, b = 23.381(1)Å, c = 18.8662(5)Å, V = 15433(1)Å3 and Z = 8. The diffraction data were collected at 1.1 Å resolution. The structure refinements converged at R = 0.165. Two independent peptide molecules were found, which formed antiparallel-sheets having intramolecular hydrogen bonds between Val and Leu residues. The peptides turned at the d-Phe–Pro moieties, and the conformations were defined as type II’ β-turn. Adjacent molecules formed an angle of 49° and were arranged side-by-side to form a β-sheet along the c-axis.

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  • Mustafa TOMBUL
    2019 Volume 35 Pages 3-4
    Published: January 10, 2019
    Released: January 10, 2019
    JOURNALS FREE ACCESS

    The structure of tertiarybutyl ammonium bis[naphthalene-2,3-diolato)borate] dimethyl sulfoxide solvate was determined by X-Ray crystallography. The compound crystallized in a triclinic system, and was characterized to be in the space group P-1, with cell parameters a = 9.6282(9)Å, b = 11.0221(9)Å, c = 13.0273(12)Å, α = 91.050(4)0, β = 109.419(4)0, γ = 94.574(2)0, Z = 2, and V = 1298.2(2)Å3. The crystal packing is governed by intermolecular and intramolecular N–H···O hydrogen bonds. The B atom takes a distorted tetrahedral geometry with four O atoms of naphthalene-2,3-diolato ligands.

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Part 2
  • Mio SEKINO, Hideki FURUTACHI, Kyosuke TASAKI, Takanao ISHIKAWA, Shuhei ...
    2019 Volume 35 Pages 5-7
    Published: February 10, 2019
    Released: February 10, 2019
    JOURNALS FREE ACCESS

    The structure of the dinuclear Fe(II) complex [Fe2(OH)2(LBu)]2+ (1) was determined by X-ray crystallography, where LBu is N,N,N′,N′-tetrakis(6-methyl-2-pyridylmethyl)-1,4-diaminobutane. The compound crystallizes in a monoclinic space group, P21/a, with a = 21.678(3), b = 16.3791(16), c = 22.447(3)Å, β = 111.522(2)°, Z = 4, V = 7414.5(14)Å3. The R1 [I > 2σ(I)] and wR2 (all data) values were 0.0474 and 0.1274, respectively, for all 16779 independent reflections. The complex has a bis(μ-hydroxo)diiron core structure.

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  • Ryoji MITSUHASHI, Masahiro MIKURIYA
    2019 Volume 35 Pages 9-10
    Published: February 10, 2019
    Released: February 10, 2019
    JOURNALS FREE ACCESS

    The crystal structure of 2-(4-methylimidazolin-2-yl)phenol was determined by X-ray crystallography. Single crystals were obtained from a racemic mixture of the title compound by the slow evaporation of an ethanol solution. The compound crystallizes in the orthorhombic chiral space group Pna21 and Z = 4 with cell parameters a = 12.595(4)Å, b = 6.2362(18)Å, c = 11.529(3)Å, V = 905.6(5)Å3. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0460 and 0.0997, respectively, for all 1953 independent reflections. In the crystal, the compound exists as zwitterionic form. An intermolecular hydrogen-bond was formed between the phenolate-O atom and N–H atom, which resulted in the formation of a 1D chain structure.

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Part 3
  • Yuichi YASUDA, Hideki FURUTACHI, Yosuke HAYASHI, Kana ISHIZAKI, Shuhei ...
    2019 Volume 35 Pages 11-13
    Published: March 10, 2019
    Released: March 10, 2019
    JOURNALS FREE ACCESS

    The structure of the dinuclear Fe(II) complex [Fe2(Ph-bimp)(PhCO2)(CH3CN)](BF4)2·2CH3CN·3CH3CH2OH (1) was determined by X-ray crystallography, where Ph-bimp is 2,6-bis[bis{2-(1-methyl-4,5-diphenylimidazolyl)methyl}aminomethyl]-4-methylpenolate. The compound crystallizes in a monoclinic space group Cc with a = 15.5690(10), b = 23.8260(8), c = 24.821(1)Å, β = 95.3460(3)°, Z = 4, V = 9167.2(10)Å3. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0336 and 0.0850, respectively, for all 16812 independent reflections. The complex has a μ-phenoxo-μ-benzoate-bridged diiron(II) core structure.

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  • Ryoji MITSUHASHI, Masahiro MIKURIYA
    2019 Volume 35 Pages 15-16
    Published: March 10, 2019
    Released: March 10, 2019
    JOURNALS FREE ACCESS

    The crystal structure of the Zn(II) complex with 2-(2-imidazolinyl)phenolate was determined by X-ray crystallography. The title compound was synthesized by reacting ZnCl2 and 2-(2-imidazolinyl)phenolate in methanol. The compound crystallized in the monoclinic space group P21/n and Z = 4 with cell parameters a = 12.0318(15)Å, b = 7.6706(10)Å, c = 18.617(2)Å, β = 105.089(2)°, V = 1658.9(14)Å3. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0454 and 0.1096, respectively, for all 4047 independent reflections. The title compound was found to take a pseudo-tetrahedral coordination geometry in the bis-bidentate fashion. In the crystal, a 1D chain structure was formed by intermolecular hydrogen-bonds between the coordinating phenolate–O atom and a noncoordinating N–H bond.

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Part 4
Part 5
Part 6
  • Tatsuto KIWADA, Aika HIRASAKI, Akira ODANI
    2019 Volume 35 Pages 35-36
    Published: June 10, 2019
    Released: June 10, 2019
    JOURNALS FREE ACCESS

    The crystal structure of (2,2′-bipyridine)(N-(1-naphthyl)methyl-1,3-propanediamine)platinum(II) chloride was determined by X-ray crystallography. The title complex crystallized in the monoclinic space group C2/c and Z = 8 with cell parameters a = 23.3026(14)Å, b = 17.4118(12)Å, c = 12.3816(7)Å, β = 109.032(8)°, V = 4749.1(6)Å3. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0242 and 0.0490, respectively, for all 5435 independent reflections. In the crystal structure, disorder was observed for the N-(1-naphthyl)methyl-1,3-propanediamine moiety. Hydrogen-bond network was formed between the (2,2′-bipyridine)(N-(1-naphthyl)methyl-1,3-propanediamine)platinum(II) cations and chloride anions.

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  • Ryoji MITSUHASHI, Masahiro MIKURIYA
    2019 Volume 35 Pages 37-38
    Published: June 10, 2019
    Released: June 10, 2019
    JOURNALS FREE ACCESS

    The crystal structure of tetracoordinated a zinc(II) complex with two 2-(1,4,5,6-tetrahydropyrimidin-2-yl)phenolate ligands was determined by X-ray crystallography. The title compound was synthesized by a reaction of ZnCl2 and 2-(1,4,5,6-tetrahydropyrimidin-2-yl)phenolate in ethanol. The compound crystallizes in the monoclinic space group C2/c and Z = 4 with cell parameters a = 13.7667(14)Å, b = 11.4666(11)Å, c = 12.2213(12)Å, β = 116.242(2)°, V = 1730.4(3)Å3. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0401 and 0.1064, respectively, for all 2104 independent reflections. The crystal structure was solved as a two-component twin. The title compound was found to take a pseudo-tetrahedral geometry with the bis-bidentate coordination mode. The non-coordinating N–H bond in the ligands formed intermolecular hydrogen-bonds to construct one-dimensional chain structures.

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Part 7
  • Tatsuto KIWADA, Hiroshi TAKAYAMA, Hiromu KATAKASU, Akira ODANI
    2019 Volume 35 Pages 39-41
    Published: July 10, 2019
    Released: July 10, 2019
    JOURNALS FREE ACCESS

    The crystal structure of [N-(9-anthracenylmethyl)-1,3-propanediamine](2,2′-bipyridine)platinum(II) chloride was determined by X-ray crystallography. The title complex crystallized in the monoclinic space group P21/c and Z = 4 with cell parameters a = 11.2466(7)Å, b = 17.3553(10)Å, c = 13.7027(9)Å, β = 100.501(2)°, V = 2629.8(3)Å3. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0271 and 0.0619, respectively, for all 5995 independent reflections. The intramolecular π-π stacking interaction was observed between the anthracene and the bipyridine. In the crystal packing structure, the intermolecular π-π stacking interaction was observed.

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  • Chika KUROGI, Toshiaki YONEMURA
    2019 Volume 35 Pages 43-45
    Published: July 10, 2019
    Released: July 10, 2019
    JOURNALS FREE ACCESS

    The structure of β(Nprim)-[Co(aet)(trien)]Cl2 [aet: 2-aminoethanethiolate, trien: triethylenetetramine] was synthesized and characterized by single-crystal X-ray analysis. The compound crystallizes in a triclinic space group P1 with a = 8.279(3), b = 10.673(5), c = 10.696(4)Å, α = 64.70(3), β = 95.76(3), γ = 91.17(4)°, V = 849.9(6)Å3, Dcalcd = 1.552 g/cm3, Z = 2. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0385 and 0.1145, respectively, for all 3913 independent reflections. Central cobalt(III) atoms have an approximate octahedral geometry and are coordinated by five nitrogen atoms and one sulfur atom. The obtained compound from the major eluate is in the β(Nprim) form in which the sulfur atom is present in the trans position to a primary nitrogen atom of the triethylenetetramine (trien).

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Part 8
  • Kanji KUBO, Taisuke MATSUMOTO, Haruko TAKECHI
    2019 Volume 35 Pages 47-48
    Published: August 10, 2019
    Released: August 10, 2019
    JOURNALS FREE ACCESS

    The structure of 7-(dimethylamino)-3-phenylcoumarin (1) was determined by X-ray crystallography. It crystallizes in the space group P21/a (#14) with cell parameters a = 15.290(3)Å, b = 6.5298(14)Å, c = 27.551(6)Å, β = 105.054(13)°, Z = 8, and V = 2656.2(9)Å3. The R1 (I > 2σ(I)) and wR2 (all data) values are 0.0591 and 0.1864, respectively. The structure of 1 contains two crystallographically independent molecules (1A and 1B). The coumarin rings make angles of 35.2(1)° for 1A and 33.4(1)° for 1B with phenyl groups. Intermolecular C–H···O, C–H···π, and π···π interactions were observed in the crystal lattice.

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  • Gaoxiang MENG, Qiang LI, Yongming YANG
    2019 Volume 35 Pages 49-50
    Published: August 10, 2019
    Released: August 10, 2019
    JOURNALS FREE ACCESS

    The structure of catena-((μ8-benzene-1,2,4,5-tetracarboxylato)-triaqua-calcium(II)-copper(II)) (I) was determine by X-ray crystallography. There is half of one benzene-1,2,4,5-tetracar-boxylate tetra-anion (BTA4−), each half Cu(II) and Ca(II) dications, and one and a half coordinated water molecules in its asymmetric unit. The compound crystallizes in the monoclinic C2/c space group and was characterized as follows: a = 14.1365(13)Å, b = 13.2077(12)Å, c = 8.8865(8)Å, b = 126.365(3)°, V = 1336.1(2)Å3, Z = 4, T = 150(2)K. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F2 to final values of R1 = 0.0779 and wR2 = 0.1666.

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Part 9
  • Yoshiki OZAWA, Azusa MASUNAGA, Masahiro KUBO, Nobuhiro YASUDA, Koshiro ...
    2019 Volume 35 Pages 51-53
    Published: September 10, 2019
    Released: September 10, 2019
    JOURNALS FREE ACCESS

    The structure of a hexanuclear silver(I) complex with six quinoline-2-thiolato (2-qnt) ligands [Ag6(C9H6NS)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)Å3, Z = 1, T = 150 K. The R1 [I > 2σ(I)] and wR2(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 Ag6 octahedral metal core.

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  • Mari TOYAMA, Kenji CHAYAMA
    2019 Volume 35 Pages 55-56
    Published: September 10, 2019
    Released: September 10, 2019
    JOURNALS FREE ACCESS

    The crystal structure of the title compound, 6-aza-3,9-dithiaundecane hydrochloride (N-H-ATU·HCl), was determined by X-ray crystallography. The hydrogen-bonding networks in the crystal extend along with the b and c axes to form a 2D-triple-sheet, in which the Cl ions put between two (N-H2-ATU)+ sheets. The compound was crystallized in an orthorhombic system as: Pccn, a = 25.0091(4), b = 5.39364(10), c = 9.37759(19)Å, Z = 4, V = 1264.94(4)Å3. The R1 and wR2 values were 0.0341 and 0.0880, respectively, for 1162 reflections.

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