The Crystal Structure of [2,6-Bis(1-methyl-4-methylthio-5-thia-2,3-diazahexa-1,3-dienyl)-pyridine]dithiocyanatonickel(II), a Complex of a Potentially Pentadentate N3S2 Ligand, and a Comparison with Complexes of an N3O2 Ligand

1979 ◽  
Vol 32 (6) ◽  
pp. 1199 ◽  
Author(s):  
W Choong ◽  
NC Stephenson ◽  
MA Ali ◽  
MA Malik ◽  
DJ Phillips
Keyword(s):  
Crystal Structure ◽  
Data Structure ◽  
Pyridine Ring ◽  
Structure Refinement ◽  
Three Dimensional ◽  
Octahedral Structure ◽  
Potential Donor ◽  
X Ray ◽  
Distorted Octahedral ◽  
R Value

The crystal structure of Ni(dapsm)(NCS)2 [dapsm is 2,6-bis(1-methyl-4-methylthio-5-thia-2,3-diazahexa-1,3-dienyl)pyridinel has been determined from three-dimensional single-crystal diffractometer X-ray data. Structure refinement was carried out by least-squares methods to a final R value of 0.059. The ligand dapsm is a potential N3S2 pentadentate, but it coordinates as a tetradentate, giving a planar N3S donor grouping. Rotation occurs about an N-N bond in dapsm, moving a potential donor sulfur atom away from the nickel(II) ion. The pyridine ring of the ligand, and the N3S donor grouping, are approximately coplanar. Two thiocyanate groups are coordinated to the nickel, giving a distorted octahedral structure. The structure and electronic spectrum of Ni(dapsm)- (NCS)2 are compared with those for seven-coordinate complexes with the related N3O2 ligand, 2,6-diacetylpyridine bissemicarbazone.

The Crystal Structure of KIO3.HIO3

1971 ◽  
Vol 49 (3) ◽  
pp. 468-476 ◽  
Author(s):  
Lilian Y. Y. Chan ◽  
F. W. B. Einstein
Keyword(s):  
Crystal Structure ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
X Ray ◽  
R Factor ◽  
Octahedral Environment ◽  
Distorted Octahedral ◽  
Potassium Hydrogen ◽  
A Cell ◽  
Least Squares Techniques

The crystal structure of potassium hydrogen di-iodate (bi-iodate) KIO3.HIO3 was determined from three dimensional X-ray data collected by counter methods. The structure was refined by full-matrix least-squares techniques to a conventional R factor of 5.0 % for the 1392 observed reflexions. The salt crystallizes in the monoclinic space group P21/c with eight formula units in a cell of dimension a = 7.028(1) Å, b = 8.203(1) Å, c = 21.841(3) Å, β = 98.03(1)°.The iodate units are all basically pyramidal; weak interionic I—O contacts complete a very distorted octahedral environment around three iodine atoms. There is a capped octahedral (7-coordinate) environment around the remaining iodine atom. The I—O bonds are in the range 1.75–1.82 Å and the I—OH bonds are 1.91 and 1.95 Å, variations in length can be correlated with differences in the degree of involvement in (a) hydrogen bonding and (b) interaction with adjacent iodine atoms.

The crystal structure of Bis[2-(pyridin-2-ylamino)-4-(pyridin-2-yl)thiazole]iron(II) Bis(tetrafluoroborate) trihydrate

1984 ◽  
Vol 37 (2) ◽  
pp. 443 ◽  
Author(s):  
AT Baker ◽  
HA Goodwin ◽  
AD Rae
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Complex Cation ◽  
Monoclinic Space Group ◽  
Octahedral Structure ◽  
Space Group ◽  
X Ray ◽  
Disordered Structure ◽  
Distorted Octahedral ◽  
A Cell

The crystal structure of an iron(II) complex of 2-(pyridin-2-ylamino)-4-(pyridin-2-yl)tliazoe (paptH) has been determined by single-crystal X-ray diffractometry. [Fe(paptH)2] [BF4]2.3H2O is monoclinic, space group P21/c, with Z = 4 in a cell of dimensions a 8.968(6), b 9.038(4), c 41.15(2)�, β 94.81(2)�. The disordered structure was refined to a residual R 0.0826 for 2549 observed reflections. The ligands and anions are orientationally disordered, and the waters of crystallization are positionally disordered. Comprehensive constrained refinement, with 220 parameters for 139 atom positions, produced reliable geometry. The complex cation has a distorted octahedral structure of meridional configuration with both paptH ligands functioning as tridentates.

Synthesis, crystal structure and characterization of a three-dimensional CdII coordination polymer constructed from 2,5-bis(1H-1,2,4-triazol-1-yl)terephthalate

2018 ◽  
Vol 74 (2) ◽  
pp. 166-170 ◽  
Author(s):  
Li Meng ◽  
Miao-Li Zhu ◽  
Li-Ping Lu
Keyword(s):  
Crystal Structure ◽  
Coordination Polymer ◽  
Three Dimensional ◽  
X Ray ◽  
Distorted Octahedral ◽  
Ft Ir ◽  
A Chain ◽  
Coordinated Water ◽  
Dimensional Crystal

Bifunctional organic ligands are very popular for the design of coordination polymers because they allow the formation of a great diversity of structures. In the title coordination polymer, the new bifunctional inversion-symmetric ligand 2,5-bis(1H-1,2,4-triazol-1-yl)terephthalic acid (abbreviated as H2bttpa) links CdII cations, giving rise to the three-dimensional CdII coordination polymer catena-poly[diaqua[μ4-2,5-bis(1H-1,2,4-triazol-1-yl)terephthalato-κ4 O 1:O 4:N 4:N 4′]cadmium(II)], [Cd(C12H6N6O4)(H2O)2] n or [Cd(bttpa)(H2O)2] n . The asymmetric unit consists of half a CdII cation, half a bttpa2− ligand and one coordinated water molecule. The CdII cation is located on a twofold axis and is hexacoordinated in a distorted octahedral environment of four O and two N atoms. Four different bttpa2− ligands contribute to this coordination, with two carboxylate O atoms in trans positions and two triazole N atoms in cis positions. Two aqua ligands in cis positions complete the coordination sphere. The fully deprotonated bttpa2− ligand sits about a crystallographic centre of inversion and links two CdII cations to form a chain in a μ2-terephthalato-κ2 O 1:O 4 bridge. This chain extends in the other two directions via the triazole heterocycles, producing a three-dimensional framework. O—H...O hydrogen bonds and weak C—H...N interactions stabilize the three-dimensional crystal structure. The FT–IR spectrum, X-ray powder pattern, thermogravimetric behaviour and solid-state photoluminescence of the title polymer have been investigated. The photoluminescence is enhanced and red-shifted with respect to the uncoordinated ligand.

scholarly journals Crystal structure of bis[(oxalato-κ2O1,O2)(1,4,8,11-tetraazacyclotetradecane-κ4N)chromium(III)] dichromate octahydrate from synchrotron X-ray data

2017 ◽  
Vol 73 (3) ◽  
pp. 403-406 ◽  
Author(s):  
Dohyun Moon ◽  
Jong-Ha Choi
Keyword(s):  
Crystal Structure ◽  
Three Dimensional ◽  
Distorted Octahedral Geometry ◽  
Water Molecules ◽  
Asymmetric Unit ◽  
Intermolecular Hydrogen Bonds ◽  
X Ray ◽  
Dimensional Network ◽  
Oxalate Ligand ◽  
Distorted Octahedral

The asymmetric unit of the title compound, [Cr(C2O4)(C10H24N4)]2[Cr2O7]·8H2O (C10H24N4= 1,4,8,11-tetraazacyclotetradecane, cyclam; C2O4= oxalate, ox) contains one [Cr(ox)(cyclam)]+cation, one half of a dichromate anion that lies about an inversion centre so that the bridging O atom is equally disordered over two positions, and four water molecules. The terminal O atoms of the dichromate anion are also disordered over two positions with a refined occupancy ratio 0.586 (6):0.414 (6). The CrIIIion is coordinated by the four N atoms of the cyclam ligand and one bidentate oxalato ligand in acisarrangement, resulting in a distorted octahedral geometry. The Cr—N(cyclam) bond lengths are in the range 2.069 (2)–2.086 (2) Å, while the average Cr—O(ox) bond length is 1.936 Å. The macrocyclic cyclam moiety adopts thecis-V conformation. The dichromate anion has a staggered conformation. The crystal structure is stabilized by intermolecular hydrogen bonds involving the cyclam N—H groups and water O—H groups as donors, and the O atoms of oxalate ligand, water molecules and the Cr2O72−anion as acceptors, giving rise to a three-dimensional network.

Nitridomolybdenum Complexes of Tris(3,5-dimethylpyrazol-1-yl)Hydroborate and the X-Ray Crystal-Structure of {HB(3,5-Me2C3N2H)3)MoN(N3)2

1990 ◽  
Vol 43 (8) ◽  
pp. 1347 ◽  
Author(s):  
CG Young ◽  
F Janos ◽  
MA Bruck ◽  
PA Wexler ◽  
JH Enemark
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Least Squares ◽  
Elemental Analysis ◽  
Bond Distance ◽  
Octahedral Complex ◽  
Fourier Methods ◽  
X Ray ◽  
Distorted Octahedral ◽  
R Value

The reaction of (NEt4)2[MoNCl5] and K{HB(Me2pz)3}[HB(Me2pz)3- = tris (3,5- dimethylpyrazol-1-yl) hydroborate anion] produces both purple, diamagnetic {HB(Me2pz)3}MoNCl2 (1) and yellow, paramagnetic Net4 [{HB(Me2pz)3}MoNCl2] (2) (e.s.r.: {g} 1.961, {a}(95Mo) 57×10-4 cm-1), which have been separately isolated under different conditions. In contrast, the reaction of [ MoN (N3)4]- with Na{HB(Me2pz)3} results in the exclusive formation of red {HB(Me2pz)3} MoN (N3)2 (3). Crystals of (3) are monoclinic and belong to space group P21/n with a 16.440(2), b 8.787(2), c 16.754(2) Ǻ,β 112.47(1)°, V 2236.4 Ǻ3, and Z 4. The structure was solved by Patterson and Fourier methods, followed by least-squares refinement, using 3208 reflections, to a conventional R value of 0.032 ( Rw 0.047). In the distorted octahedral complex the molybdenum(VI) atom is coordinated by a facial HB(Me2pz)3- ligand , a terminal nitrido ligand with a Mo-N bond distance of 1.646(4)Ǻ, and two azide ligands. All complexes have been characterized by elemental analysis, infrared, 1H n.m.r. or e.s.r. spectroscopy, and mass spectrometry. Improved syntheses for the starting materials (NEt4)2 [MoNCl5] and (NEt4)2 [MoNCl4] are also reported.

Structural Studies of Technetium Complexes. X. The Crystal-Structure of Tetraphenylarsonium Hexakis(Isothiocyanato)Technetate(IV)-Dichloromethane (1/1)

1987 ◽  
Vol 40 (1) ◽  
pp. 27 ◽  
Author(s):  
GA Williams ◽  
J Bonnyman ◽  
J Baldas
Keyword(s):  
Crystal Structure ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
Octahedral Structure ◽  
Crystal Lattices ◽  
Full Matrix ◽  
X Ray ◽  
C And N ◽  
R Value ◽  
A Site

The crystal structure of [AsPh4]2 [ Tc (NCS)6].CH2Cl2 has been determined by single-crystal X-ray diffraction methods at 23 � 1�C . Crystals are tetragonal, space group I4/m, with a 11.523(5), c 22.43(2) �, and Z 2. Diffraction data from two different crystals were analysed and in both cases disorder was present in the crystal lattices. Full-matrix least-squares refinement gave a final R value of 0.073 for 1188m independent reflections. The [TC(NCS)6]2- anion has an octahedral structure with the technetium(1V) atom situated on a site of 4/m symmetry. The Tc -N bond lengths are 2.00(1) and 2.01(1) Ǻ with N- Tc -N angles of exactly 90�. Two of the Tc -NCS groups are constrained by the crystal symmetry to be perfectly linear, while for the remaining four Tc -NCS groupings the Tc -N-C and N-C-S angles are 175.9(9)� and 175.3(10)� respectively.

X-Ray Structure of a Nickel(II) Complex of the Tetra-N-methylated Macrocycle Dibenzocyclam with a Folded Ligand Configuration

1984 ◽  
Vol 39 (7) ◽  
pp. 903-906 ◽  
Author(s):  
Horst Elias ◽  
Rüdiger Grewe ◽  
Dirk-Detlev Klaehn ◽  
Helmut Paulus
Keyword(s):  
Three Dimensional ◽  
Bidentate Ligand ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Nitrate Ion ◽  
Light Blue ◽  
X Ray ◽  
Mild Conditions ◽  
Distorted Octahedral ◽  
R Value

Under mild conditions nickel(II) nitrate reacts with the macrocyclic N4 ligand TMBC ( = 1,4 ,8,11-tetramethyl-1,4,8,11-tetraazadibenzo[b,i]cyclotetradecane) to form the light blue-green complex Ni (TMBC) (NO3)2. A three-dimensional X-ray diffraction study shows that the complex crystallizes in the monoclinic space group P21/c with a = 896.1(3) pm, b = 2059.9(7) pm , c = 1298.6(6) pm, β = 91.37(1)° and Z = 4. The nickel is six-coordinate. The distorted octahedral N4O2 arrangement of donor atoms around the nickel is formed by the tetradentate N4 macrocycle TMBC in an unexpected folded form and by a nitrate ion as a bidentate ligand occupying two depositions. The structure could be refined to the final R-value of 0.045 only by assuming disorder for the second, noncoordinated nitrate ion.

scholarly journals Crystal structure of bis[cis-(1,4,8,11-tetraazacyclotetradecane-κ4N)bis(thiocyanato-κN)chromium(III)] dichromate monohydrate from synchrotron X-ray diffraction data

2017 ◽  
Vol 73 (1) ◽  
pp. 72-75 ◽  
Author(s):  
Dohyun Moon ◽  
Masahiro Takase ◽  
Takashiro Akitsu ◽  
Jong-Ha Choi
Keyword(s):  
Crystal Structure ◽  
Three Dimensional ◽  
Complex Salt ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Intermolecular Hydrogen Bonds ◽  
Rotation Symmetry ◽  
X Ray ◽  
Dimensional Network ◽  
Distorted Octahedral

The structure of the complex salt,cis-[Cr(NCS)2(cyclam)]2[Cr2O7]·H2O (cyclam = 1,4,8,11-tetraazacyclotetradecane, C10H24N4), has been determined from synchrotron data. The asymmetric unit comprises of one [Cr(NCS)2(cyclam)]+cation, one half of a Cr2O72−anion (completed by inversion symmetry) and one half of a water molecule (completed by twofold rotation symmetry). The CrIIIion is coordinated by the four cyclam N atoms and by two N atoms ofcis-arranged thiocyanate anions, displaying a distorted octahedral coordination sphere. The Cr—N(cyclam) bond lengths are in the range 2.080 (2) to 2.097 (2) Å while the average Cr—N(NCS) bond length is 1.985 (4) Å. The macrocyclic cyclam moiety adopts thecis-V conformation. The bridging O atom of the dichromate anion is disordered around an inversion centre, leading to a bending of the Cr—O—Cr bridging angle [157.7 (3)°]; the anion has a staggered conformation. The crystal structure is stabilized by intermolecular hydrogen bonds involving the cyclam N—H groups and water O—H groups as donor groups, and the O atoms of the Cr2O72−anion and water molecules as acceptor groups, giving rise to a three-dimensional network.

scholarly journals Bis(N,N′-bis(2-hydroxyethyl)ethylenediamine)nickel(II) saccharinate: synthesis, characterization and crystal structure

2015 ◽  
Vol 34 (1) ◽  
pp. 101
Author(s):  
Alparslan Karadogan ◽  
Ahmet Karadag ◽  
Veysel T. Yilmaz
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Complex Cation ◽  
Three Dimensional ◽  
Title Complex ◽  
X Ray Diffraction ◽  
X Ray ◽  
Distorted Octahedral

A new nickel(II) saccharinate (sac) complex containing <em>N</em>,<em>N</em>′-bis(2-hydroxyethyl)ethylenediamine (bishydeten), [Ni(bishydeten)<sub>2</sub>](sac)<sub>2</sub>, has been synthesized and characterized by elemental analysis, FTIR and single crystal X-ray diffraction. The title complex consists of a [Ni(bishydeten)<sub>2</sub>]<sup>2+</sup> cation and two sac anions. In the complex cation, the nickel(II) ion is coordinated by two neutral bishydeten ligands, leading to a distorted octahedral NiN<sub>4</sub>O<sub>2</sub> coordination, while both sac anions remain outside the coordination sphere. In the crystal, the complex cations and sac anions are connected by an extensive network of N–H∙∙∙N, N–H∙∙∙O, O–H∙∙∙O and C–H∙∙∙O hydrogen bonds into a three-dimensional supramolecular lattice.

X-ray crystal structure of N'-[(1E)-1-(2,4-dihydroxyphenyl)-ethylidene]pyridine-4-carbohydrazide

2019 ◽  
Vol 6 (1) ◽  
Author(s):  
Venkatesan Jayaprakash ◽  
Ajay Kumar Timiri ◽  
Viswanathan Vijayan ◽  
Barij Nayan Sinha ◽  
Velmurugan Devadasan
Keyword(s):  
Crystal Structure ◽  
Dengue Virus ◽  
Three Dimensional ◽  
Crystallographic Structure ◽  
Slow Evaporation ◽  
Schiff’S Base ◽  
X Ray ◽  
R Value ◽  
Isonicotinyl Hydrazide ◽  
Ns3 Protease

Schiff’s base of isonicotinyl hydrazide with 2’,4’-dihydroxy acetophenone (INH-RA) has been designed and synthesized as a part of library enumeration targeting the NS2B-NS3 protease of Dengue virus. Slow evaporation from methanol results in the formation of monoclinic crystals C2/c space group with eight molecules in the unit cell (a=20.0165(3) Å, b=7.7594(10) Å, c=19.4809(3) Å, α=90 °, β=111.368(1) °, γ=90 ° and Z=8).Three dimensional X-ray crystallographic structure of the compound has been determined and refined using SHELXS-97 and SHELXL-2014, respectively to a final R-value of 4.64%

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