Synthesis and Structural Characterization of N-Methyl-DL-glutamic Acid

2000 ◽  
Vol 53 (3) ◽  
pp. 237 ◽  
Author(s):  
Andrew B. Hughes ◽  
Maureen F. Mackay ◽  
Luigi Aurelio
Keyword(s):  
Three Dimensional ◽  
Amino Nitrogen ◽  
Measured Data ◽  
X Ray ◽  
X Ray Crystallography ◽  
Zwitterionic Form ◽  
Dimensional Network ◽  
Orthorhombic Crystals ◽  
Solid State Conformation

The solid-state conformation of racemic N-methylglutamic acid has been defined by single-crystal X-ray crystallography. Orthorhombic crystals belong to the space group Pbca with a 15.219(2), b 10.583(1), c 9.595(1) Å and Z 8. The structure was refined to a final R value of 0.049 for the 1285 measured data. In the crystal the molecules adopt a zwitterionic form with protonation having occurred at the amino nitrogen atom. The a-carboxyl is unprotonated with the d-carboxy group retaining a proton. The i.r. spectrum shows absorptions which also are indicative of the amino acid being in the zwitterionic form. Intermolecular H-bonds involving the carboxylate proton and the two protons on the N-atom link the molecules into a three-dimensional network in the crystal.

Formation and Structural Characterization of [RuCl2(CO)2(SPh2)2], [RuCl2(CO)3(OH2)], and [Ru(OH2)6][RuCl3(CO)3]2 · 2H2O

2003 ◽  
Vol 58 (10) ◽  
pp. 959-964 ◽  
Author(s):  
Marjaana Taimisto ◽  
Raija Oilunkaniemi ◽  
Risto S. Laitinen ◽  
Markku Ahlgrén
Keyword(s):  
Hydrogen Bonding ◽  
Hydrogen Bonds ◽  
Room Temperature ◽  
Three Dimensional ◽  
Temperature Reaction ◽  
X Ray ◽  
X Ray Crystallography ◽  
Dimensional Network ◽  
Moderate Yield

While the room temperature reaction of [RuCl2(CO)3]2 and Ph2S in tetrahydrofuran in air affords [RuCl2(CO)2(SPh2)2] (1) in moderate yield, that in dichloromethane results in the formation of a mixture of [RuCl2(CO)3(H2O)] (2) and [Ru(H2O)6][RuCl3(CO)3]2·2H2O (3). Very small amounts of 1 are produced only upon prolonged reflux of the reagents. All compounds were characterized by X-ray crystallography. 1 crystallizes as discrete octahedral cis(CO), cis(Cl), trans(Ph2S) complexes, which are joined into stacks by weak H···Cl hydrogen bonds. 2 is also composed of discrete octahedral complexes. Four hydrogen bonds involving aqua and chlorido ligands link two complexes into a dimer. The structure of 3 consists of octahedral hexaaquaruthenium cations and two tricarbonyltrichloridoruthenate anions. The water of crystallization is involved in hydrogen bonding between the cations and anions resulting in the formation of a continuous three-dimensional network.

Synthesis and Structural Characterization of the Mixed Ligand Complex [Cu(Hml)2(Phen)] · 2 H2O (H2ml = 2-Methyllactic Acid)

2003 ◽  
Vol 58 (1) ◽  
pp. 151-154 ◽  
Author(s):  
Rosa Carballo ◽  
Berta Covelo ◽  
Ezequiel M. Vázquez-Lópeza ◽  
Alfonso Castiñeiras ◽  
Juan Niclós
Keyword(s):  
Magnetic Measurements ◽  
Mixed Ligand Complex ◽  
Three Dimensional ◽  
Mixed Ligand ◽  
Water Molecules ◽  
Ligand Complex ◽  
X Ray ◽  
Dimensional Network ◽  
Distorted Octahedral

Abstract A new mixed-ligand complex of copper(II) with 1,10-phenanthroline and 2-methyllactate was prepared. [Cu(HmL)2(phen)] ·2H2O (where HmL = monodeprotonated 2-methyllactic acid) was characterized by elemental analysis, IR, electronic and EPR spectroscopy, magnetic measurements at room temperature, thermogravimetric analysis and X-ray diffractometry. The copper atom is in a tetragonally distorted octahedral environment and the 2-methyllactato ligand is bidentately chelating. The presence of lattice water molecules mediates the formation of a three-dimensional network.

scholarly journals Preparation and Characterization of 2-Phenoxyethyl(thiophen-2-yl)tellane (C4H3S)TeCH2CH2OC6H5

2006 ◽  
Vol 61 (1) ◽  
pp. 61-64
Author(s):  
Ludmila Vigo ◽  
Raija Oilunkaniemi ◽  
Risto S. Laitinen
Keyword(s):  
Three Dimensional ◽  
Monoclinic Crystal ◽  
X Ray ◽  
Compound C ◽  
Dimensional Network ◽  
Cell Dimensions ◽  
Weak Hydrogen Bonds ◽  
Intermolecular Contacts ◽  
Unit Cell Dimensions

The synthesis and structure of (C4H3S)TeCH2CH2OC6H5 (1) (C4H3S = thiophen-2-yl) are reported and compared to those of the analogous selenium compound (C4H3S)SeCH2CH2OC6H5 previously synthesized by our group. The compound was characterized by 1H, 13C{1H}-, and 125Te- NMR spectroscopy as well as by X-ray single crystal crystallography. 1 crystallizes in the monoclinic crystal system, space group P21, with Z = 2, and unit cell dimensions a = 10.618(2) Å , b = 5.357(1) Å , c = 10.684(2) Å , β = 96.57(3)°. The lattice is composed of discrete molecules that are joined together by weak hydrogen bonds into a three-dimensional network. The thiophen-2-yl ring is disordered and shows two alternative orientations with the site occupation factors of 0.70(1) and 0.30(1). All bond parameters are quite normal. The comparison of the lattices in 1 and in its selenium anologue shows that while the closest intermolecular contacts are similar, the packing of the molecules is different.

New Inclusion Compounds of Selenourea with Tetraethyl- and Tetra-n-propylammonium Halides

1997 ◽  
Vol 53 (2) ◽  
pp. 262-271 ◽  
Author(s):  
Q. Li ◽  
T. C. W. Mak
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Three Dimensional ◽  
Crystal Data ◽  
Tetraethylammonium Chloride ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Dimensional Network ◽  
Single Column

Air-sensitive selenourea inclusion complexes tetraethylammonium chloride–selenourea (1/2), (C2H5)4N+.C1−.2[(NH2)2CSe] (1), tetra-n-propyl-ammonium chloride–selenourea (1/3), (n-C3H7)4N+.C1−.3[(NH2)2CSe] (2), tetra-n-propylammonium bromide–selenourea (1/3), (n-C3H7)4N+.Br−.3[(NH2)2CSe] (3), and tetra-n-propylammonium iodide–selenourea (1/1), (n-C3H7)4N+.I−.(NH2)2CSe (4), have been prepared and characterized by X-ray crystallography. Crystal data, Mo Kα radiation: (1), space group P21/n, Z = 4, a = 8.768 (5), b = 11.036 (6), c = 19.79 (1) Å, β = 96.92 (1)°, R F = 0.055 for 1468 observed data; (2), space group Cc, Z = 4, a = 18.091 (4), b = 13.719 (3), c = 11.539 (2) Å, β = 111.93 (3)°, R F = 0.051 for 1187 observed data; (3), space group Cc, Z = 4, a = 18.309  (4), b = 13.807 (3), c = 11.577 (2) Å, β = 112.45 (3)°, R F = 0.049 for 1592 observed data; (4), space group P21/n, Z = 4, a = 8.976 (1), b = 14.455 (2), c = 15.377 (3) Å, β = 94.16(1)°, R F = 0.062 for 1984 observed data. In the crystal structure of (1) the parallel alternate arrangement of selenourea–chloride ribbons and selenourea chains generates a puckered layer and the cations are sandwiched between them. In the isomorphous complexes (2) and (3) wide selenourea–halide double ribbons are crosslinked by bridging selenourea molecules via N—H...Se and N—H...X hydrogen bonds [average N...Se = 3.521 (8) and 3.527 (7), N...Cl = 3.354 (8) and N...Br = 3.500 (7) Å in (2) and (3), respectively] to form a channel-like three-dimensional network and the cations are accommodated in a single column within each channel. In the crystal structure of (4) the selenourea molecules are joined in the shoulder-to-shoulder fashion via N—H...Se hydrogen bonds [N...Se = 3.529 (7) and 3.534 (7) Å] to generate a ribbon and each selenourea molecule also forms a pair of chelating N—H...I hydrogen bonds [N...I = 3.567 (7) and 3.652 (7) Å] to an adjacent iodide ion.

Synthesis and structural characterization of two coordination polymers constructed by bis(4-(1H-imidazol-1-yl)phenyl)methanone and 5-(tert-butyl)isophthalate ligands

2019 ◽  
Vol 74 (3) ◽  
pp. 261-265 ◽  
Author(s):  
Gao-Feng Wang ◽  
Shu-Wen Sun ◽  
Wei-Bing Wang ◽  
Hong Sun ◽  
Shao-Fei Song
Keyword(s):  
Single Crystal ◽  
Coordination Polymers ◽  
Weak Interactions ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dimensional Network ◽  
Elemental Analyses ◽  
Solvothermal Methods

AbstractTwo coordination polymers, {[Co(bipmo)(tbip)]·3H2O}n (1) and {[Cd(bipmo)(tbip)]·3H2O}n (2) (bipmo=bis(4-(1H-imidazol-1-yl)phenyl)methanone, H2tbip=5-tert-butylisophthalic acid), were synthesized by solvothermal methods and structurally characterized by elemental analyses, infrared spectroscopy, and single-crystal X-ray diffraction. The results from single-crystal X-ray diffraction data indicate that the solid state structures of 1 and 2 consist of metal-aromatic carboxylate layers, which are pillared by weak interactions to generate a three-dimensional network. The topological structures of 1 and 2 are uninodal nets based on 3-connected nodes with the Schläfli symbol of {63}.

Chiral Helices in a 3D Network of Zn2(en)V2O7 (en = Ethylenediamine)

2008 ◽  
Vol 55-57 ◽  
pp. 669-672 ◽  
Author(s):  
S. Krachodnok ◽  
K.J. Haller ◽  
I.D. Williams
Keyword(s):  
Thermal Stability ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Tg Analysis ◽  
X Ray ◽  
X Ray Crystallography ◽  
Organic Hybrid ◽  
Dimensional Network ◽  
3D Network ◽  
Thermal Stability Of

An inorganic-organic hybrid vanadate complex, Zn2(en)V2O7 (en = ethylenediamine) has been hydrothermally synthesized and characterized by single-crystal X-ray crystallography, TG analysis, IR spectroscopy, and elemental analysis. The title compound crystallizes in the monoclinic space group P21 with a = 7.0885(7), b = 8.6040(9), c = 8.1869(8) Å, b = 112.224(2)° and V = 462.22(8) Å3, T = 298±2 K and R1[I>2s(I)] = 0.0291 for 2170 observed reflections. The structure consists of undulating sheets constructed from helical chains that share Zn coordination centers with repeating units propagated into a helix by the two-fold screw axes at 0, y, ½ and pillared with alternating VO4 tetrahedra to generate a 3D chiral network. Neighboring helices are interconnected by µ2-O bridges to form the three-dimensional network. The strength of the network is reinforced by hydrogen bonding. TG analysis shows thermal stability of the network up to 283 °C.

scholarly journals Synthesis and Physico-Chemical Characterization of a New Non-Centrosymmetric Organic Cation Iodate

2011 ◽  
Vol 7 (2) ◽  
pp. 1315-1323 ◽  
Author(s):  
A.C. Dhiab ◽  
W. Smirani Sta ◽  
M. Rzaigui
Keyword(s):  
Organic Cation ◽  
Three Dimensional ◽  
Chemical Characterization ◽  
Halogen Bonds ◽  
Monoclinic System ◽  
X Ray ◽  
Dimensional Network ◽  
Physico Chemical ◽  
Graph Set

The synthesis, crystal structure and physico-chemical characterization are presented for the piperazinium bis iodate dihydrate. An X-ray investigation has shown that this compound crystallizes in a non-centrosymmetric monoclinic system, space group Pc with the lattice parameters: a = 8.969 (2) Å, b = 6.027 (3)  Å, c = 11.958 (2)  Å; V = 612.7 (3)  Å3 and Z = 2. The structure was solved from 3546 independent reflexions with R1 = 0.053 and wR2 = 0.130. I…O halogen bonds [R22(4) graph-set motif] range between 2.770 (4) and 3.108 (1) Å and connect neighboring IO-3 anions with each other so as to create a bi-dimensional layer parallel to the (b,c) plane. These layers are interconnected via N−H…O and C−H…O, to the piperazinium dication to generate a three-dimensional network.

scholarly journals Crystalline and Molecular Structure of Hexaaqua-1,3-diammoniumpropane Cobalt(II) Nitrate, Co(H2O)6[C3H12N2] (NO3)4

2010 ◽  
Vol 7 (3) ◽  
pp. 887-893
Author(s):  
M. L. Mrad ◽  
C. Ben Nasr ◽  
M. Rzaigui
Keyword(s):  
Direct Method ◽  
Three Dimensional ◽  
Chemical Preparation ◽  
Orthorhombic System ◽  
X Ray ◽  
R Factor ◽  
Dimensional Network ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

Chemical preparation and x-ray characterization of a new compound hexaaqua-1,3-diammoniumpropane cobalt(II) nitrate, Co(H2O)6[C3H12N2] (NO3)4are reported. This mixed organo-mineral compound crystallizes in the orthorhombic system with Cmcm space group. The unit cell dimensions are: a = 10.795(7), b = 11.969(4), c = 14.685(5) Å, Z = 4 and V = 1897.5(12) Å3. The structure was solved using the direct method and refined to reliability R-factor of 0.036 using 2554 independent reflections. In this atomic arrangement the different species built a three-dimensional network.

scholarly journals Synthesis, X-Ray Structure, and Characterization of a Complex Containing the Hexakis(urea)cobalt(II) Cation and Lattice Urea Molecules

2007 ◽  
Vol 2007 ◽  
pp. 1-7 ◽  
Author(s):  
Labrini Drakopoulou ◽  
Constantina Papatriantafyllopoulou ◽  
Aris Terzis ◽  
Spyros P. Perlepes ◽  
Evy Manessi-Zoupa ◽  
...  
Keyword(s):  
Room Temperature ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Two Dimensional ◽  
X Ray ◽  
Lattice Constants ◽  
Dimensional Network ◽  
Different Types ◽  
Hydrogen Bonded

The 12: 1 reaction of urea (U) with CoI2in EtOH yielded the “clathrate-coordination” compound[CoU6]I2·4U (1). The complex crystallizes in the monoclinic space group P21/c. The lattice constants area= 9.844(4),b= 7.268(3),c= 24.12(1) Å, andβ=98.12(1)∘. The crystal structure determination demonstrates the existence of octahedral[CoU6]2+cations,I-counterions, and two different types (twoU1and twoU2) of hydrogen-bonded, lattice urea molecules. The[CoU6]2+cations and theU1lattice molecules form two-dimensional hydrogen-bonded layers which are parallel to theabplane. TheI-anions are placed above and below each layer, and are hydrogen bonded both toU1molecules and[CoU6]2+cations. EachU2molecule is connected to a[CoU6]2+cation through anN–H⋯Ohydrogen bond resulting in a three-dimensional network. Room temperature magnetic susceptibility and spectroscopic (solid-state UV/Vis, IR, Raman) data of1are discussed in terms of the nature of bonding and the known structure.

scholarly journals Crystal structure of 1,4,8,11-tetramethyl-1,4,8,11-tetraazoniacyclotetradecane bis[chloridochromate(VI)] dichloride from synchrotron X-ray data

2020 ◽  
Vol 76 (4) ◽  
pp. 523-526
Author(s):  
Dohyun Moon ◽  
Jong-Ha Choi
Keyword(s):  
Crystal Structure ◽  
Organic Cation ◽  
Three Dimensional ◽  
Chloride Anion ◽  
Inversion Center ◽  
X Ray ◽  
X Ray Crystallography ◽  
Compound C ◽  
Dimensional Network ◽  
Cl Atom

The crystal structure of title compound, (C14H36N4)[CrO3Cl]2Cl2, has been determined by synchrotron radiation X-ray crystallography at 220 K. The macrocyclic cation lies across a crystallographic inversion center and hence the asymmetric unit contains one half of the organic cation, one chlorochromate anion and one chloride anion. Both the Cl− anion and chlorochromate Cl atom are involved in hydrogen bonding. In the crystal, hydrogen bonds involving the 1,4,8,11-tetramethyl-1,4,8,11-tetraazoniacyclotetradecane (TMC) N—H groups and C—H groups as donor groups and three O atoms of the chlorochromate and the chloride anion as acceptor groups link the components, giving rise to a three-dimensional network.

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