scholarly journals A New Supramolecular Assembly Obtained by Reaction Between Thiosaccharin and Hexamethylenediamine

2007 ◽  
Vol 62 (12) ◽  
pp. 1530-1534
Author(s):  
Enrique J. Baran ◽  
Oscar E. Piro ◽  
Juan Zinczuk
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Ionic Crystal ◽  
Functional Group ◽  
Three Dimensional ◽  
Supramolecular Assembly ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Anions And Cations

The crystal structure of hexamethylenediammonium bis(thiosaccharinate) dihydrate, [H3N-(CH2)6-NH3](tsac)2 · 2H2O (tsac=C7H4NO2S2, the anion of thiosaccharin), was determined by single-crystal X-ray diffraction. It crystallizes in the monoclinic space group P21/a with Z = 4. The thiosaccharinate moiety is planar and shows small but significant modifications in the bonding of the thioamide functional group as compared with the protonated neutral molecule. The ionic crystal is further stabilized by an extensive H-bonding network, which links the anions and cations into an infinite three-dimensional supramolecular assembly. The FTIR spectrum of the compound is briefly discussed in comparison with those of the neutral constituent molecules.

scholarly journals Two New Supramolecular Assemblies Obtained by Reaction Between Saccharin and Long-chain Diamines

2009 ◽  
Vol 64 (9) ◽  
pp. 1041-1045
Author(s):  
Eduardo E Castellano ◽  
Oscar E. Piro ◽  
Beatriz S. Parajón-Costa ◽  
Enrique J. Baran
Keyword(s):  
Three Dimensional ◽  
Supramolecular Assembly ◽  
Monoclinic Space Group ◽  
Ionic Crystals ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Anions And Cations ◽  
Bonding Characteristics

The crystal structures of heptamethylenediammonium bis(saccharinate) monohydrate, [H3N - (CH2)7 -NH3](sac)2・H2O (1) and octamethylenediammonium bis(saccharinate) hemihydrate, [H3N- (CH2)8-NH3](sac)2・0.5H2O (2), were determined by single-crystal X-ray diffraction methods. Compound 1 crystallizes in the triclinic space group P1̄ with 2 molecules per unit cell, and 2 in the monoclinic space group P21/a with Z = 4. The saccharinate moiety is planar in both compounds presenting bonding characteristics comparable to those found in other saccharinate salts. The ionic crystals are further stabilized by an extensive H-bonding network, which links the anions and cations into an infinite three-dimensional supramolecular assembly. The FTIR spectra of the adducts are briefly discussed in comparison with those of the constituent molecules.

scholarly journals An investigation of polyhedral deformation in two mixed-metal diarsenates: SrZnAs2O7and BaCuAs2O7

2015 ◽  
Vol 71 (4) ◽  
pp. 330-337 ◽  
Author(s):  
Sabina Kovač ◽  
Ljiljana Karanović ◽  
Tamara Đorđević
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
General Formula ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Hydrothermal Conditions ◽  
X Ray ◽  
Open Framework ◽  
Geometrical Characteristics ◽  
Barium Copper

Two isostructural diarsenates, SrZnAs2O7(strontium zinc diarsenate), (I), and BaCuAs2O7[barium copper(II) diarsenate], (II), have been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction. The three-dimensional open-framework crystal structure consists of corner-sharingM2O5(M2 = Zn or Cu) square pyramids and diarsenate (As2O7) groups. Each As2O7group shares its five corners with five differentM2O5square pyramids. The resulting framework delimits two types of tunnels aligned parallel to the [010] and [100] directions where the large divalent nine-coordinatedM1 (M1 = Sr or Ba) cations are located. The geometrical characteristics of theM1O9,M2O5and As2O7groups of known isostructural diarsenates, adopting the general formulaM1IIM2IIAs2O7(M1II= Sr, Ba, Pb;M2II= Mg, Co, Cu, Zn) and crystallizing in the space groupP21/n, are presented and discussed.

The first proof of protonated anion tetrahedra in the tsumcorite-type compounds

2004 ◽  
Vol 68 (5) ◽  
pp. 757-767 ◽  
Author(s):  
T. Mihajlović ◽  
H. Effenberger
Keyword(s):  
Crystal Structure ◽  
Hydrothermal Synthesis ◽  
Single Crystal ◽  
Diffraction Data ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Synthetic Compounds ◽  
X Ray

AbstractHydrothermal synthesis produced the new compound SrCo2(AsO4)(AsO3OH)(OH)(H2O). The compound belongs to the tsumcorite group (natural and synthetic compounds with the general formula M(1)M(2)2(XO4)2(H2O,OH)2; M(1)1+,2+,3+ = Na, K, Rb, Ag, NH4, Ca, Pb, Bi, Tl; M(2)2+,3+ = Al, Mn3+, Fe3+, Co, Ni, Cu, Zn; and X5+,6+ = P, As, V, S, Se, Mo). It represents (1) the first Sr member, (2) the until now unknown [7]-coordination for the M(1) position, (3) the first proof of (partially) protonated arsenate groups in this group of compounds, and (4) a new structure variant.The crystal structure of the title compound was determined using single-crystal X-ray diffraction data. The compound is monoclinic, space group P21/a, with a = 9.139(2), b = 12.829(3), c = 7.522(2) Å, β = 114.33(3)°, V = 803.6(3) Å3, Z = 4 [wR2 = 0.065 for 3530 unique reflections]. The hydrogen atoms were located experimentally.

scholarly journals X-Ray Single Crystal Structural Analysis of Magnetically Oriented Microcrystals

2014 ◽  
Vol 70 (a1) ◽  
pp. C1138-C1138
Author(s):  
Chiaki Tsuboi ◽  
Kazuki Aburaya ◽  
Shingo Higuchi ◽  
Fumiko Kimura ◽  
Masataka Maeyama ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Three Dimensional ◽  
Diffraction Measurement ◽  
X Ray Diffraction ◽  
Data Set ◽  
Uv Curable ◽  
X Ray

We have developed magnetically oriented microcrystal array (MOMA) technique that enables single crystal X-ray diffraction analyses from microcrystalline powder. In this method, microcrystals suspended in a UV-curable monomer matrix are there-dimensionally aligned by special rotating magnetic field, followed by consolidation of the matrix by photopolymerization. From thus achieved MOMAs, we have been succeeded in crystal structure analysis for some substances [1, 2]. Though MOMA method is an effective technique, it has some problems as follows: in a MOMA, the alignment is deteriorated during the consolidation process. In addition, the sample microcrystals cannot be recovered from a MOMA. To overcome these problems, we performed an in-situ X-ray diffraction measurement using a three-dimensional magnetically oriented microcrystal suspension (3D MOMS) of L-alanine. An experimental setting of the in-situ X-ray measurement of MOMS is schematically shown in the figure. L-alanine microcrystal suspension was poured into a glass capillary and placed on the rotating unit equipped with a pair of neodymium magnets. Rotating X-ray chopper with 10°-slits was placed between the collimator and the suspension. By using this chopper, it was possible to expose the X-ray only when the rotating MOMS makes a specific direction with respect to the impinging X-ray. This has the same effect as the omega oscillation in conventional single crystal measurement. A total of 22 XRD images of 10° increments from 0° to 220° were obtained. The data set was processed by using conventional software to obtain three-dimensional molecular structure of L-alanine. The structure is in good agreement with that reported for the single crystal. R1 and wR2 were 6.53 and 17.4 %, respectively. RMSD value between the determined molecular structure and the reported one was 0.0045 Å. From this result, we conclude that this method can be effective and practical to be used widely for crystal structure analyses.

Crystal Structure and Vibrational Behaviour of Aqua Di(saccharinato)di(nicotinamide)copper(II)

2002 ◽  
Vol 57 (1) ◽  
pp. 43-46 ◽  
Author(s):  
Beatriz S. Parajón-Costaa ◽  
Enrique J. Baran ◽  
Oscar E. Piro ◽  
Eduardo E Castellano
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Ir Spectrum ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The crystal structure of [Cu(sac)2(nic)2(H2O)] (sac = saccharinate anion; nic = nicotinamide) has been determined by single-crystal X-ray diffraction. It crystallizes in the monoclinic space group C2/c with Z = 4 and the Cu(II) ion presents a CuN4O square pyramidal coordination. Some comparisons with related structures are made and the most important features of its IR spectrum were also discussed.

scholarly journals Serendipitous formation and characterization of K2[Pd(NO3)4]·2HNO3

2019 ◽  
Vol 74 (4) ◽  
pp. 381-387
Author(s):  
Michael Zoller ◽  
Jörn Bruns ◽  
Gunter Heymann ◽  
Klaus Wurst ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Monoclinic Space Group ◽  
Solvothermal Process ◽  
X Ray Diffraction ◽  
Glass Ampoule ◽  
Space Group ◽  
X Ray ◽  
Complex Anions

AbstractA potassium tetranitratopalladate(II) with the composition K2[Pd(NO3)4] · 2HNO3 was synthesized by a simple solvothermal process in a glass ampoule. The new compound crystallizes in the monoclinic space group P21/c (no. 14) with the lattice parameters a = 1017.15(4), b = 892.94(3), c = 880.55(3) Å, and β = 98.13(1)° (Z = 2). The crystal structure of K2[Pd(NO3)4] · 2HNO3 reveals isolated complex [Pd(NO3)4]2− anions, which are surrounded by eight potassium cations and four HNO3 molecules. The complex anions and the cations are associated in layers which are separated by HNO3 molecules. K2[Pd(NO3)4] · 2HNO3 can thus be regarded as a HNO3 intercalation variant of β-K2[Pd(NO3)4]. The characterization is based on single-crystal X-ray and powder X-ray diffraction.

A New Supramolecular Synthon Using N-Methylaniline. The Crystal Structure of the 1 : 1 Adduct of N-Methylaniline with 5-Nitrofuran-2-carboxylic Acid

1998 ◽  
Vol 51 (9) ◽  
pp. 867 ◽  
Author(s):  
Daniel E. Lynch ◽  
Lisa C. Thomas ◽  
Graham Smith ◽  
Karl A. Byriel ◽  
Colin H. L. Kennard
Keyword(s):  
Crystal Structure ◽  
Carboxylic Acid ◽  
Proton Transfer ◽  
Single Crystal ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Supramolecular Synthon ◽  
X Ray ◽  
C 23 ◽  
A Cell

The crystal structure of the 1 : 1 adduct of N-methylaniline with 5-nitrofuran-2-carboxylic acid has been determined by single-crystal X-ray diffraction. Crystals are monoclinic, space group P21/c with Z 4 in a cell of dimensions a 8·467(5), b 6·106(2), c 23·95(1) Å, β 94·48(3)°. The molecules associate in a tetrameric, proton-transfer formation which has potential as a new supramolecular synthon.

scholarly journals The reaction of 3,5-diphenyl-1,2-dithiolium-4-olate with aniline: the crystal structure of 1-phenylimino-2-phenylamino-3-phenylindene

1987 ◽  
Vol 65 (12) ◽  
pp. 2830-2833 ◽  
Author(s):  
David M. McKinnon ◽  
Peter D. Clark ◽  
Robert O. Martin ◽  
Louis T. J. Delbaere ◽  
J. Wilson Quail
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

3,5-Diphenyl-1,2-dithiolium-4-olate (1) reacts with aniline to form 1-phenylimino-2-phenylamino-3-phenylindene (3a). Under suitable conditions, 6-phenylbenzo[b]indeno[1,2-e]-1,2-thiazine is also formed. These structures are confirmed by alternative syntheses. The molecular structure of 3a has been determined by single crystal X-ray diffraction. Compound 3a crystallizes in the monoclinic space group C2/c with unit cell dimensions a = 20.777(3) Å, b = 6.130(3) Å, c = 31.327(3) Å, 3 = 99.59(1)°, and Z = 8. The structure was solved by direct methods and refined by least squares to a final R = 0.055. The molecular structure of 3a shows the three phenyl containing substituents to have the planes of their ring systems tilted between 40° and 60° from the plane of the indene system due to steric repulsions.

Crystal structure of zerumbone [(E,E,E)-2,6,9,9-Tetramethylcycloundeca-2,6,10-trien-1-one]

1981 ◽  
Vol 34 (10) ◽  
pp. 2243 ◽  
Author(s):  
SR Hall ◽  
S Nimgirawath ◽  
CL Raston ◽  
A Sittatrakul ◽  
S Thadaniti ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Membered Ring ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Zingiber Zerumbet ◽  
Space Group ◽  
X Ray ◽  
Considerable Distortion

The crystal structure of zerumbone, C15H22O, extracted from the rhizomes of Zingiber zerumbet Smith, has been determined by single-crystal X-ray diffraction at 295(1) K and refined by least squares to a residual of 0.051 for 925 'observed' reflections. Crystals are monoclinic, space group P21/c, a 9.036(3), b 9.712(5), c 15.643(6) �, β 97.19(3)�, Z = 4. Although the molecule has no chiral centre, the presence of the three trans double bonds confers considerable distortion and rigidity on the eleven-membered ring and renders the whole molecule chiral and potentially resolvable.

Hylbrownite, Na3MgP3O10·12H2O, a new triphosphate mineral from the Dome Rock Mine, South Australia: description and crystal structure

2013 ◽  
Vol 77 (3) ◽  
pp. 385-398 ◽  
Author(s):  
P. Elliott ◽  
J. Brugger ◽  
T. Caradoc-Davies ◽  
A. Pring
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
South Australia ◽  
New Mineral ◽  
Monoclinic Space Group ◽  
Thick Sheet ◽  
X Ray Diffraction ◽  
X Ray ◽  
New Mineral Species ◽  
Mohs Hardness

AbstractHylbrownite, ideally Na3MgP3O10·12H2O, the second known triphosphate mineral, is a new mineral species from the Dome Rock mine, Boolcoomatta Reserve, Olary Province, South Australia, Australia. The mineral forms aggregates and sprays of crystals up to 0.5 mm across with individual crystals up to 0.12 mm in length and 0.02 mm in width. Crystals are thin prismatic to acicular in habit and are elongate along [001]. Forms observed are {010}, {100}, {001}, {210} and {201}. Crystals are colourless to white, possess a white streak, are transparent, brittle, have a vitreous lustre and are nonfluorescent. The measured density is 1.81(4) g cm−3; Mohs' hardness was not determined. Cleavage is good parallel to {001} and to {100} and the fracture is uneven. Hylbrownite crystals are nonpleochroic, biaxial (−), with α = 1.390(4), β = 1.421(4), γ = 1.446(4) and 2Vcalc. = 82.2°. Hylbrownite is monoclinic, space group P21/n, with a = 14.722(3), b = 9.240(2), c = 15.052(3) Å, β = 90.01(3)°, V = 2047.5(7) Å3, (single-crystal data) and Z = 4. The strongest lines in the powder X-ray diffraction pattern are [d (Å)(I)(hkl)]: 10.530(60)(10,101), 7.357(80)(200), 6.951(100)(11, 111), 4.754(35)(10, 103), 3.934(40)(022), 3.510(45)(30, 303), 3.336(35)(41, 411). Chemical analysis by electron microprobe gave Na2O 16.08, MgO 7.08, CaO 0.43, P2O5 37.60, H2Ocalc 38.45, total 99.64 wt.%. The empirical formula, calculated on the basis of 22 oxygen atoms is Na2.93Mg0.99Ca0.04P2.99O9.97·12.03H2O. The crystal structure was solved from single-crystal X-ray diffraction data using synchrotron radiation (T = 123 K) and refined to R1 = 4.50% on the basis of 2417 observed reflections with F0 > 4 σ(F0). [Mg(H2O)3P3O10] clusters link in the b direction to Naφ6 octahedra, by face and corner sharing. Edge sharing Naφ6 Octahedra and Naφ7 polyhedra form Na2O9 groups which link via corners to form chains along the b direction. Chains link to [Mg(H2O)3P3O10] clusters via corner-sharing in the c direction and form a thick sheet parallel to (100). Sheets are linked in the a direction via hydrogen bonds.

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