scholarly journals Crystal structures of two nickel(II) macrocyclic salts: (5,7,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)nickel(II) bis(perchlorate) monohydrate and (5,7,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)nickel(II) dibromide trihydrate

2019 ◽  
Vol 75 (3) ◽  
pp. 332-337
Author(s):  
Peter W. R. Corfield ◽  
Virgil L. Goedken
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
The Other ◽  
Water Molecules ◽  
Asymmetric Unit ◽  
The Mean ◽  
The Many ◽  
Hydrogen Bonded

The crystal structure of the Ni-14 macrocycle salt, (5,7,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)nickel(II) bis(perchlorate) hemihydrate, [Ni(C16H36N4)]2(ClO4)4·H2O, contains two different diasteriomeric macrocyclic cations in the asymmetric unit, one with two NH protons on each side of the cation (Ia), and the other with all four NH protons on the same side (Ib). The crystal structure of the bromide trihydrate salt of the same Ni-14 macrocyclic cation, namely (5,7,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)nickel(II) dibromide trihydrate, [Ni(C16H36N4)]Br2·3H2O (II), contains only the same diastereomer as Ib, with the four N—H bonds on the same side. The geometry around the Ni atom differs slightly between the two diastereomeric cations, as the mean Ni—N distance in Ia is 1.952 (2) Å, while that for Ib and II is 1.928 (2) Å. The hexamethyl substitution in all three macrocyclic cations has the two dimethyl-substituted C atoms cis to one another, different from the trans 5,5,7,12,12,14-hexamethyl Ni-14 cations found in all but one of the many published crystal structures of hexamethyl Ni-14 macrocycles. In each of the two crystal structures, the anions, water molecules, and N—H protons of the macrocyclic cations form extensive hydrogen-bonded zigzag chains propagating along [001] in I and [010] in II.

Structural Studies on N-(2,4,6-Trimethylphenyl)-methyl/ chloro-acetamides, 2,4,6-(CH3)3C6H2NH-CO-CH3–yXy (X = CH3 or Cl and y = 0, 1, 2)

2006 ◽  
Vol 61 (10-11) ◽  
pp. 588-594 ◽  
Author(s):  
Basavalinganadoddy Thimme Gowda ◽  
Jozef Kožíšek ◽  
Hartmut Fuess
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Structural Data ◽  
The Other ◽  
Side Chain ◽  
Structural Studies ◽  
Asymmetric Unit ◽  
Lattice Constants ◽  
Peptide Linkage ◽  
The Mean

TMPAThe effect of substitutions in the ring and in the side chain on the crystal structure of N- (2,4,6-trimethylphenyl)-methyl/chloro-acetamides of the configuration 2,4,6-(CH3)3C6H2NH-COCH3− yXy (X = CH3 or Cl and y = 0,1, 2) has been studied by determining the crystal structures of N-(2,4,6-trimethylphenyl)-acetamide, 2,4,6-(CH3)3C6H2NH-CO-CH3 (); N-(2,4,6- trimethylphenyl)-2-methylacetamide, 2,4,6-(CH3)3C6H2NH-CO-CH2-CH3 (TMPMA); N-(2,4,6- trimethylphenyl)-2,2-dimethylacetamide, 2,4,6-(CH3)3C6H2NH-CO-CH(CH3)2 (TMPDMA) and N-(2,4,6-trimethylphenyl)-2,2-dichloroacetamide, 2,4,6-(CH3)3C6H2NH-CO-CHCl2 (TMPDCA). The crystallographic system, space group, formula units and lattice constants in Å are: TMPA: monoclinic, Pn, Z = 2, a = 8.142(3), b = 8.469(3), c = 8.223(3), β = 113.61(2)◦; TMPMA: monoclinic, P21/n, Z = 8, a = 9.103(1), b = 15.812(2), c = 16.4787(19), α = 89.974(10)◦, β = 96.951(10)◦, γ =89.967(10)◦; TMPDMA: monoclinic, P21/c, Z = 4, a =4.757(1), b= 24.644(4), c =10.785(2), β = 99.647(17)◦; TMPDCA: triclinic, P¯1, Z = 2, a = 4.652(1), b = 11.006(1), c = 12.369(1), α = 82.521(7)◦, β = 83.09(1)◦, γ = 79.84(1)◦. The results are analyzed along with the structural data of N-phenylacetamide, C6H5NH-CO-CH3; N-(2,4,6-trimethylphenyl)-2-chloroacetamide, 2,4,6-(CH3)3C6H2NH-CO-CH2Cl; N-(2,4,6-trichlorophenyl)-acetamide, 2,4,6-Cl3C6H2NH-COCH3; N-(2,4,6-trichlorophenyl)-2-chloroacetamide, 2,4,6-Cl3C6H2NH-CO-CH2Cl; N-(2,4,6-trichlorophenyl)- 2,2-dichloroacetamide, 2,4,6-Cl3C6H2NH-CO-CHCl2 and N-(2,4,6-trichlorophenyl)- 2,2,2-trichloroacetamide, 2,4,6-Cl3C6H2NH-CO-CCl3. TMPA, TMPMA and TMPDCA have one molecule each in their asymmetric units, while TMPDMA has two molecules in its asymmetric unit. Changes in the mean ring distances are smaller on substitution as the effect has to be transmitted through the peptide linkage. The comparison of the other bond parameters reveal that there are significant changes in them on substitution.

scholarly journals Synthesis and crystal structure of a disubstituted nickel(II) bis[(dimethylaminophenylimino)ethyl]pyridine chloride complex

2017 ◽  
Vol 73 (8) ◽  
pp. 1167-1171 ◽  
Author(s):  
Morgan Matthews ◽  
Madison Sendzik ◽  
Adrienne Bruggeman ◽  
Claire Kearns ◽  
Allen G. Oliver ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Pyridine Ring ◽  
Phenyl Group ◽  
Chloride Complex ◽  
The Other ◽  
Water Molecules ◽  
Asymmetric Unit ◽  
Synthesis And Crystal Structure ◽  
Solvent Molecules ◽  
Hydrogen Bonded

The solvated title compound, bis[2,6-bis(1-{[4-(dimethylamino)phenyl]imino-κN}ethyl)pyridine-κN]nickel(II) dichloride–dichloromethane–water (1/2/2), [Ni(C25H29N5)2]Cl2·2CH2Cl2·2H2O, represents a nickel(II) bis(pyridine diimine) complex with electron-donating dimethylaminophenyl substituents. The complex crystallizes as a water/dichloromethane solvate with Z′ = 2, thus the asymmetric unit consists of two NiII complex cations, four chloride anions, four adventitious water and four dichloromethane solvent molecules. Around each octahedrally coordinated NiII cation, one pendant phenyl group on each of the two ligands has an intramolecular π–π interaction with the pyridine ring of the other chelating ligand. In the crystal, pairs of water molecules are hydrogen bonded to pairs of chlorine atoms. The dichloromethane solvent molecules are likewise hydrogen bonded to the chloride anions.

scholarly journals Diosgenin hemihydrate

2012 ◽  
Vol 68 (8) ◽  
pp. o2357-o2357 ◽  
Author(s):  
María-Guadalupe Hernández Linares ◽  
Sylvain Bernès ◽  
Marcos Flores-Alamo ◽  
Gabriel Guerrero-Luna ◽  
Anselmo A. Martínez-Gallegos
Keyword(s):  
Crystal Structure ◽  
Water Molecule ◽  
Dimethyl Sulfoxide ◽  
Starting Material ◽  
Water Molecules ◽  
Asymmetric Unit ◽  
Acta Cryst ◽  
X Ray ◽  
Hydroxy Groups ◽  
Hydrogen Bonded

Diosgenin [or (22R,25R)-spirost-5-en-3β-ol] is the starting material of the Marker degradation, a cheap semi-synthesis of progesterone, which has been designated as an International Historic Chemical Landmark. Thus far, a single X-ray structure for diosgenin is known, namely its dimethyl sulfoxide solvate [Zhanget al.(2005).Acta Cryst.E61, o2324–o2325]. We have now determined the structure of the hemihydrate, C27H42O3·0.5H2O. The asymmetric unit contains two diosgenin molecules, with quite similar conformations, and one water molecule. Hydroxy groups in steroids and water molecules form O—H...O hydrogen-bondedR54(10) ring motifs. Fused edge-sharingR(10) rings form a backbone oriented along [100], which aggregates the diosgenin molecules in the crystal structure.

scholarly journals Crystal structures of (Z)-5-[2-(benzo[b]thiophen-2-yl)-1-(3,5-dimethoxyphenyl)ethenyl]-1H-tetrazole and (Z)-5-[2-(benzo[b]thiophen-3-yl)-1-(3,4,5-trimethoxyphenyl)ethenyl]-1H-tetrazole

2016 ◽  
Vol 72 (5) ◽  
pp. 652-655 ◽  
Author(s):  
Narsimha Reddy Penthala ◽  
Jaishankar K. B. Yadlapalli ◽  
Sean Parkin ◽  
Peter A. Crooks
Keyword(s):  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Related Compound ◽  
Condensation Reaction ◽  
Dihedral Angles ◽  
Asymmetric Unit ◽  
The Mean ◽  
Hydrogen Bonded

(Z)-5-[2-(Benzo[b]thiophen-2-yl)-1-(3,5-dimethoxyphenyl)ethenyl]-1H-tetrazole methanol monosolvate, C19H16N4O2S·CH3OH, (I), was prepared by the reaction of (Z)-3-(benzo[b]thiophen-2-yl)-2-(3,5-dimethoxyphenyl)acrylonitrile with tributyltin azideviaa [3 + 2]cycloaddition azide condensation reaction. The structurally related compound (Z)-5-[2-(benzo[b]thiophen-3-yl)-1-(3,4,5-trimethoxyphenyl)ethenyl]-1H-tetrazole, C20H18N4O3S, (II), was prepared by the reaction of (Z)-3-(benzo[b]thiophen-3-yl)-2-(3,4,5-trimethoxyphenyl)acrylonitrile with tributyltin azide. Crystals of (I) have two molecules in the asymmetric unit (Z′ = 2), whereas crystals of (II) haveZ′ = 1. The benzothiophene rings in (I) and (II) are almost planar, with r.m.s deviations from the mean plane of 0.0084 and 0.0037 Å in (I) and 0.0084 Å in (II). The tetrazole rings of (I) and (II) make dihedral angles with the mean planes of the benzothiophene rings of 88.81 (13) and 88.92 (13)° in (I), and 60.94 (6)° in (II). The dimethoxyphenyl and trimethoxyphenyl rings make dihedral angles with the benzothiophene rings of 23.91 (8) and 24.99 (8)° in (I) and 84.47 (3)° in (II). In both structures, molecules are linked into hydrogen-bonded chains. In (I), these chains involve both tetrazole and methanol, and are parallel to thebaxis. In (II), molecules are linked into chains parallel to theaaxis by N—H...N hydrogen bonds between adjacent tetrazole rings.

scholarly journals Crystal structure of poly[diaqua(μ2-benzene-1,4-dicarboxylato-κ2O1:O4)(μ2-benzene-1,4-dicarboxylato-κ4O1,O1′:O4,O4′)bis(μ2-3,3′,5,5′-tetramethyl-4,4′-bipyrazole-κ2N:N′)dinickel(II)]

2015 ◽  
Vol 71 (6) ◽  
pp. m127-m128
Author(s):  
Chao Wu ◽  
Peng Cao
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Water Molecule ◽  
Crystal Packing ◽  
Three Dimensional ◽  
The Other ◽  
Water Molecules ◽  
Inversion Symmetry ◽  
Asymmetric Unit ◽  
Dimensional Network

The asymmetric unit of the polymeric title compound, [Ni(C8H4O4)(C10H14N4)(H2O)]n, contains one Ni2+cation, one coordinating water molecule, one 3,3′,5,5′-tetramethyl-4,4′-bipyrazole ligand and half each of two benzene-1,4-dicarboxylate anions, the other halves being generated by inversion symmetry. The Ni2+cation exhibits an octahedral N2O4coordination sphere defined by the O atoms of the water molecule and two different anions and the N atoms of two symmetry-relatedN-heterocycles. TheN-heterocycles and both anions bridge adjacent Ni2+cations into a three-dimensional network structure, with one of the anions in a bis-bidentate and the other in a bis-monodentate bridging mode. N—H...O and O—H...O hydrogen bonds between the N-heterocycles and water molecules as donor groups and the carboxylate O atoms as acceptor groups consolidate the crystal packing.

Dibutyltin derivatives of 2,6-pyridinedicarboxylic acids. Crystal structures of bis(diisopropylammonium) tris(2,6-pyridinedicarboxylato)bis(dibutylstannate) trihydrate and bis(diisopropylammonium) bis[aquadibutylstannyl(2,6-pyridinedicarboxylato-4-olate)]

1998 ◽  
Vol 213 (7-8) ◽  
Author(s):  
Seik Weng Ng
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Three Dimensional ◽  
Water Molecules ◽  
Derivatives Of ◽  
Pyridinedicarboxylic Acids ◽  
Hydrogen Bonded

AbstractDibutytlin oxide condenses with diisopropylammonium hydrogen 2,6-pyridinedicarboxylate to form bis(diisopropylammonium) tris(2,6-pyridinedicarboxylato)bis(dibutylstannate) trihydrate, whose crystal structure consists of a three-dimensional hydrogen-bonded framework of ammonium cations, stannate anions and water molecules. In the dianion, the carboxyl –CO

scholarly journals (E)-2-[4-(Diethylamino)styryl]-1-methylquinolin-1-ium 4-chlorobenzenesulfonate monohydrate

2014 ◽  
Vol 70 (4) ◽  
pp. o395-o396
Author(s):  
Suchada Chantrapromma ◽  
Narissara Kaewmanee ◽  
Nawong Boonnak ◽  
Ching Kheng Quah ◽  
Hoong-Kun Fun
Keyword(s):  
Hydrogen Bonds ◽  
Benzene Ring ◽  
Ring System ◽  
The Other ◽  
Water Molecules ◽  
Sulfonate Group ◽  
Asymmetric Unit ◽  
Solvent Water ◽  
Hydrated Salt ◽  
The Mean

The asymmetric unit of the title hydrated salt, C22H25N2+·C6H4ClO3S−·H2O, comprises two 2-[4-(diethylamino)styryl]-1-methylquinolin-1-ium cations, two 4-chlorobenzenesulfonate anions and two solvent water molecules. One ethyl group of both cations displays disorder over two positions in a 0.659 (2):0.341 (2) ratio in one molecule and in a 0.501 (2):0.499 (2) ratio in the other. The sulfonate group of one anion is also disordered over two positions in a 0.893 (7):0.107 (7) ratio. The dihedral angle between the mean plane of the quinolinium ring system and that of benzene ring is 10.57 (18)° in one cation and 14.4 (2)° in the other. In the crystal, cations, anions and water molecules are linked into chains along the [010] direction by O—H...Osulfonatehydrogen bonds, together with weak C—H...Osulfonateand C—H...Cl interactions. The cations are stacked by π–π interactions, with centroid–centroid distances in the range 3.675 (2)–4.162 (3) Å.

Temperature dependence of crystal structure of NaK0.72(NH4)0.28(+)-C4H4O6.4H2O in the paraelectric phase

1996 ◽  
Vol 52 (6) ◽  
pp. 976-981 ◽  
Author(s):  
E. Suzuki ◽  
H. Kabasawa ◽  
T. Honma ◽  
R. Nozaki ◽  
Y. Shiozaki
Keyword(s):  
Crystal Structure ◽  
Structural Change ◽  
Temperature Dependence ◽  
Crystal Structures ◽  
Paraelectric Phase ◽  
The Other ◽  
Carboxylate Anion ◽  
Water Molecules ◽  
Crystal Data ◽  
X Ray

The crystal structures of the ferroelectric NaK0.72 (NH4)0.28(+)-C4H4O6.4H2O (RS0.72ARS0.28) have been studied in the paraelectric phase [Mr = 276.32, orthorhombic, P21212,° Z = 4, F(000) = 575.04, λ(Mo Kα1) = 0.70926 Å]; T = 213 (1), 253 (1) and 293 (1) K. The crystal data are as follows: (I) at T = 213 (1) K: R = 0.0424, wR = 0.0399, number of reflections = 3414, a = 11.899 (2), b = 14.273 (2), c = 6.211 (1) Å, V = 1054.9 (2) Å3, Dx = 1.740 g cm−3; (II) at T = 253 (1) K: R = 0.0498, wR = 0.0442, number of reflections = 3284, a = 11.929 (1), b = 14.297 (1), c = 6.221 (1) Å, V = 1061.0 (2) Å3, Dx = 1.730 g cm−3; (III) at T = 293 (1) K: R = 0.0473, wR = 0.0392, number of reflections = 3179, a = 11.955 (1), b = 14.317 (1), c = 6.231 (1) Å, V = 1066.5 (1) Å3, Dx = 1.721 g cm−3. X-ray investigations reveal details of structural change with temperature in the paraelectric phase. The carboxylate anion O(3)—C(4)—O(4) in the tartrate molecule is displaced along the a axis as the temperature decreases; moreover, the O(8) atom is displaced in the opposite direction against the shift of the carboxylate anion. The temperature dependence of the thermal motions of O(8) shows different behavior from the other O atoms of the water molecules. The amplitude of the thermal motion of O(8) does not tend to zero at T = 0 K, while the other O atoms of the water molecules tend to zero.

scholarly journals Crystal structure of 4-(trimethylgermyl)benzoic acid

2015 ◽  
Vol 71 (6) ◽  
pp. 687-689
Author(s):  
Lena Knauer ◽  
Eva R. Barth ◽  
Christopher Golz ◽  
Carsten Strohmann
Keyword(s):  
Crystal Structure ◽  
Benzoic Acid ◽  
Aromatic Ring ◽  
Title Compound ◽  
Asymmetric Unit ◽  
Ring Plane ◽  
Acta Cryst ◽  
The Mean ◽  
Hydrogen Bonded

The title compound, [Ge(CH3)3(C7H5O2)], was obtained as a by-product in the synthesis of the corresponding aldehyde. Two slightly different molecules are present in the asymmetric unit. In both molecules, the geometry of the aromatic ring plane is distorted by varying intensities. Additionally, the Ge atoms deviate from the mean aromatic ring planes. Whereas the distance of the Ge atom to the ring plane is only 0.101 (4) Å in the first molecule, this distance is increased to 0.210 (4) Å in the second. In the crystal structure, centrosymmetric O—H...O hydrogen-bonded dimers are formed. The title compound is isostructural with the Si analogue [Haberechtet al.(2004).Acta Cryst.E60, o329–0330].

scholarly journals Crystal structure of [NaZn(BTC)(H2O)4]·1.5H2O (BTC = benzene-1,3,5-tricarboxylate): a heterometallic coordination compound

2015 ◽  
Vol 71 (7) ◽  
pp. m143-m144 ◽  
Author(s):  
Min Ni ◽  
Quanle Li ◽  
Hao Chen ◽  
Shengqing Li
Keyword(s):  
Crystal Structure ◽  
Ionic Liquid ◽  
Coordination Polymer ◽  
Hydrogen Bonds ◽  
Tricarboxylic Acid ◽  
The Other ◽  
Water Molecules ◽  
Asymmetric Unit ◽  
Solvent Water ◽  
Bridging Ligand

The title coordination polymer, poly[[μ-aqua-triaqua(μ3-benzene-1,3,5-tricarboxylato)sodiumzinc] sesquihydrate], {[NaZn(C9H3O6)(H2O)4]·1.5H2O}n, was obtained in ionic liquid microemulsion at room temperture by the reaction of benzene-1,3,5-tricarboxylic acid (H3BTC) with Zn(NO3)2·6H2O in the presence of NaOH. The asymmetric unit comprises two Na+ions (each located on an inversion centre), one Zn2+ion, one BTC ligand, four coordinating water molecules and two solvent water molecules, one of which is disordered about an inversion centre and shows half-occupation. The Zn2+cation is five-coordinated by two carboxylate O atoms from two different BTC ligands and three coordinating H2O molecules; the Zn—O bond lengths are in the range 1.975 (2)–2.058 (3) Å. The Na+cations are six-coordinated but have different arrangements of the ligands: one is bound to two carboxylate O atoms of two BTC ligands and four O atoms from four coordinating H2O molecules while the other is bound by four carboxylate O atoms from four BTC linkers and two O atoms of coordinating H2O molecules. The completely deprotonated BTC ligand acts as a bridging ligand binding the Zn2+atom and Na+ions, forming a layered structure extending parallel to (100). An intricate network of O—H...O hydrogen bonds is present within and between the layers.

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