Three new 2,6-dimethylanilinium salts of 2-naphthalenesulfonate, 2-chloro-4-nitrobenzoate, and hydrogen dibenzoyl-L-tartarate were acquired by mixing the respective components at room temperature (RT). All isolated as the single-crystals by the slow solvent volatilization technique. The characterization was conducted through the single crystal X-ray diffraction, IR and elemental analysis (EA), their melting points were also gauged. The synthons in the salts were illucidated. Significant non-covalent interactions were calculated by means of the Hirshfeld surface analysis for understanding the noncovalent interactions which stabilized the crystal packings. Compound 1 adopts the monoclinic, space group P21/c, with a = 13.5040(14) Å, b = 5.8541(6) Å, c = 22.450(2) Å, β = 106.021(3)°, V = 1705.8(3) Å3, Z = 4. Compound 2 belongs to the triclinic, space group Pī, with a = 7.1123(7) Å, b = 8.3750(8) Å, c = 13.6298(11) Å, α = 95.6350(10)°, β = 99.354(2)°, γ = 97.6250(10)°, V = 788.01(13) Å3, Z = 2. Compound 3 crystallizes in the monoclinic, space group P 21, with a = 7.8923(8) Å, b = 24.818(3) Å, c = 13.2206(16) Å, β = 104.727(3)°, V = 2504.5(5) Å3, Z = 4. For 3 only one carboxyl was ionized to get the hydrogen carboxylate salt, different from 1–2. All supramolecular architectures of 1–3 involve the N–H···O hydrogen bonds. The other noncovalent interactions (CH3-CH/CH-CH, CH3-O/CH-O, CH3···Cl, CH3-π, O-π and O-C) in the crystal packings were also ascertained. These weak interactions combined, the salts displayed 2D-3D framework structures.
The crystal structures of 3 salts assembled by dma, 2-naphthalenesulfonic acid, 2-chloro-4-nitrobenzoic acid, and dibenzoyl-L-tartaric acid are chiefly stabilized through the traditional Hbonds in combination with the CH3-CH/CH-CH, CH3-O/CH-O, CH3-S, CH3···Cl, CH3-π, O-π and O-C contacts, building the ultimate 2D-3D appearances.
Reported here is a new series of guest-free and guest-filled frameworks with charge-assisted hydrogen bonds between anionic metal complexes and cationic organic moieties. The latter are the tri-protonated 2,4,6-Tris(4-pyridyl)-1,3,5-triazinium (H34tpt)3+ or 2,4,6-Tris(3-pyridyl)-1,3,5-triazine (H33tpt)3+ trications while the metal complex is the trianionic [Fe(ox)3]3−. The aryl derivatives 4-methoxyphenol (mp), 1,5-dihydroxynaphthalene (dhn), 2-naphthol, and methyl-4-aminobenzoate (mab) were used as guests the framework. In addition to van der Waals interactions with the host framework, these aromatic guest molecules exhibit also donor–acceptor interactions with the aromatic trigonal-planar triazinium-based linkers. The general formula of the guest-filled frameworks is [tpt][Fe(ox)3]·m[guest]·n[solvent] with m reaching 3 in some of the compounds. The fact that guest-filled frameworks can be prepared with both (H34tpt)3+ and (H33tpt)3+ demonstrates the flexibility of these soft frameworks where the nitrogen position in the pyridyl groups does not affect their capability to include guests.
Flexible empty and guest filled hydrogen bonded frameworks of tricationic triazinium linkers and trianinonic [Fe(ox)3]3− nodeswere reported. The donor-acceptor and van der Waals interaction between the triangular triazinium linkers and guest molecules was confirmed by single crystal structure and spectroscopic methods.
The chiral Boranil dye (LB(O)-Br) exhibits polymorphism forming two distinctly different structures in the solid state. Polymorph I crystallises in the space group I41/a and exhibits C-H‧‧‧O and C-H‧‧‧Br interactions to produce a columnar structure with 3D connectivity. Polymorph II crystallises in P21/c and, in addition to C-H‧‧‧O contacts, forms Br‧‧‧O halogen bonds and edge-to-face π-interactions to give a 2D layered structure. Given the propensity of these compounds to fluoresce in the crystalline state, polymorphism of these structures is an important factor to consider when designing dyes of this kind for solid-state applications.
An overlay highlights the areas of the title molecule and its analogue that vary most in terms of conformation.
The current investigation presents two new crystal structures of organotin complexes, R2SnCl2 (1) and [R2Sn(µ-S)]2 (2), where R is 2-acetamido-5-methyl phenyl. This research aims to integrate O → Sn intramolecular coordination via an unexplored functionalization on organotin center. The complexes are crystallized in a triclinic system, specifically within the P-1 space group. The asymmetric unit of complex 2 is comprised of two identical R2SnS units. The Sn center in both complexes displays a distorted octahedral geometry. The observed elongation of the Sn–O bond upon complexation indicates weaker intramolecular coordination in 2 (2.59 Å) compared to 1 (2.22 Å). Complex 2 exhibits various intermolecular interactions including N–H···O and N–H···S in their supramolecular assembly. Hirshfeld surface is generated for complex 2 to study the reactive surfaces of the complex. 2D fingerprint plots revealed the major contributions in crystal packing of 2 are C···C (0.2%), C···H/H···C (20.2%), O···H/H···O (10.6%), S···H/H···S (6.1%), and N···H/H···N (3.2%).
Crystal Structures of Two Diorganotin Complexes Are presented, Including a New Diorganotin Sulfide [R2Sn(µ-S)]2 Exploiting O→Sn Intramolecular Coordination Arising from 2-acetamido-5-methylphenyl group. Hirshfeld Surface Analysis Reveals Key Supramolecular interactions, Providing Deeper Insight into Intramolecular Coordination in Organotin Systems
Two new optical spiro materials, C17 H16 F3 N O4 (F1) and C14 H12 F3 N O4 (F2), have been synthesized. Their structures were determined by X-ray diffraction and characterized using FT-IR, UV–vis, and (1H and 13C) NMR spectroscopies. The crystal structure determinations show compound F1, belongs to the triclinic system, space group P (overline{1 }), with a = 6.1216(14) Å, b = 9.536(3) Å, c = 13.957(4) Å, α = 80.044(7)° Å, β = 86.260(8)°, γ = 81.694(7)°, Mr = 355.31, V = 793.4(3) Å3, Z = 2, F(000) = 368. Compound J2, is monoclinic system, space group P21/c with a = 14.932(3) Å, b = 5.355(9) Å, c = 17.732(4) Å, β = 92.21(4)°, Mr = 315.25, V = 1417(2) Å3, Z = 4, F(000) = 648. The both compounds form three-dimensional network structures via C–H···O and N–H···O intra- and intermolecular hydrogen bonds. The observed bond lengths, bond angles, vibrational frequencies, and UV–vis absorption peaks were in agreement with the data obtained from DFT calculations. Hirshfeld surface analyses of F1 and F2 highlighted that F···H/H···F and H···H intermolecular interactions were significant contributors. The TG/DTA demonstrated that both compounds possessed strong thermal stability. The energy gaps (ΔEHOMO-LUMO) for F1 and F2 were calculated to be 4.369 eV and 4.316 eV, respectively. Potential electrophilic and nucleophilic sites were identified through MEP analysis. Additionally, NBO and Mulliken analyses were also studied.
Two new nonlinear optical spiro materials containing CF3 group have been obtained, C17 H16 F3 N O4 (F1) and C14 H12 F3 N O4 (F2) and their structures were determined by FT-IR, UV–vis, TG analysis, (1H and 13C) NMR spectroscopies, and single crystal crystallography. The vibrational spectra, UV–vis spectra of F1 and F2 were compared to the predicted values using the level of B3LYP/6-31G(d,p). The HOMO–LUMO energies, NBO, MEP, NLO, Milliken charge distribution, TG/DTA and fluorescence behavior were also studied.
The structure of a 2-pyrenolato–coordinated gallium porphyrin complex incorporating an additional hydrogen-bonded 2-pyrenol molecule has been determined [monoclinic, a = 18.60720(10) Å, b = 15.74080(10) Å, c = 28.3753(2) Å, β = 106.9530(10)°, space group P2₁/c]. The additional 2-pyrenol molecule forms a hydrogen bond with the oxygen atom of the coordinated 2-pyrenol. The gallium ion (Ga3⁺) is five-coordinate, adopting a square-pyramidal geometry with four nitrogen atoms from the porphyrin ligand and one oxygen atom from the 2-pyrenolato ligand. The Ga–O bond distance is 1.8799(15) Å, which deviates from previously reported values for gallium porphyrins bearing oxygen-containing axial ligands. The introduction of 2-pyrenol imparts properties characteristic of pyrene, namely CH–π and π–π interactions.
This paper describes a crystallographic study of a gallium porphyrin complex coordinated with 2-pyrenolato and incorporating an additional hydrogen-bonded 2-pyrenol molecule.
The reaction of the labile tri-osmium carbonyl cluster, [Os₃(CO)₁₀(NCMe)₂] 1, with 2-ethymercaptobenzothiazole 2 produced a novel hydridobridged triosmium complex, Os₃(CO)₁₀(μ-H){μN,C-NC(SC₂H₅)SC₆H₃} 3 in moderate yield. The complex was formed via the regioselective C–H bond activation at the ortho-position of the ligand. The crystal structure of 3 demonstrated an N,C-bridging NC(SC2H5)SC6H3 group coordinated to the two osmium atoms from the axial sites. The presence of the bridging hydride was confirmed by a distinctive resonance in the 1H NMR spectroscopy at −13.12 ppm, X-ray crystallography, and computational study. Compound 3 crystallized in the monoclinic crystal system, space group P2₁/n, a = 17.642(11) Å, b = 7.720(4) Å, c = 18.102(11) Å, β = 100.773(6)°, Z = 4. The molecular geometry of 3 was very close to its DFT optimized geometry, demonstrating the N,C-bridged motif's stability.
A new tri-osmium cluster, Os3(CO)10(µ-H){µN,C-NC(SC2H5)SC6H3} 3, was synthesized from the reaction of the labile tri-osmium cluster, [Os3(CO)10(NCMe)2] 1 and 2-ethylmercaptobenzothiazole 2, which was structurally characterized.
The guest encapsulation behavior and solid-state supramolecular assembly of four bromoethoxy-substituted pillar[5]arenes were investigated. These macrocycles selectively encapsulate 1,4-dibromobutane from equimolar mixtures of four α,ω-dibromoalkanes, forming 1:1 crystalline inclusion complexes. Single-crystal X-ray diffraction revealed that encapsulation is stabilized by C–H···π and C–H···O interactions within the macrocyclic cavity. The number and position of bromoethoxy groups significantly influence the supramolecular packing. While mono- and di-bromoethoxy-functionalized pillar[5]arenes exhibit only C–H···π and C–H···O interactions, the tetra- and hexa-bromoethoxy derivatives additionally display C–H···Br contacts, with the guest contributing to the assembly. Notably, the hexabromoethoxy-functionalized pillar[5]arene also exhibits Br···Br contacts, resulting in a distinct packing arrangement compared to the other systems.
The structures of [Fe(CO)3(η4-6-exo-(OH)cyclohepta-2,4-dien-1-one] [monoclinic, a = 6.6080(2), b = 11.9177(3), c = 13.1157(4), β = 102.590(3) space group P21/c] and [Fe(CO)3(η4-6-exo-(OD)cyclohepta-2,4-dien-1-one] [monoclinic, a = 6.5999(3), b = 11.8947(4), c = 13.1040(5), β = 102.497(4) space group P21/c] have been determined. There is moderate intermolecular hydrogen bonding observed between the alcohol and the ketone. The iron centers adopt a slightly distorted square pyramidal geometry.
Addition of H2O or D2O to [Fe(CO)3(η5-cyclohepta-2,4-dien-5-yl-1-one)][BF4] results in a product that is formally attack at the coordinated ring in a position exo- to the iron atom forming the corresponding [Fe(CO)3(η4-6-exo-(OH/OD)cyclohepta-2,4-dien-1-one] compounds, which were structurally characterized
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