Crystal structure determination of an Fe^II azo aldehyde complex [Fe(C₁₄H₁₁N₂O₃)₂(H₂O)₂] by MicroED

The title compound, di­aquabis­{2-formyl-6-meth­oxy-4-[(E)-2-phenyl­diazen-1-yl]phenolato-κ²O¹,O²}iron(II), [Fe(C₁₄H₁₁N₂O₃)₂(H₂O)₂], comprises two bidentate ligands derived from 2-meth­oxy-4-(phenyl­diazen­yl)-6-formyl­phenol and two coordinated water mol­ecules. The crystal structure was determined at 79 K using the MicroED method (λ = 0.02508 Å).

Flux-growth method for the targeted synthesis of the salt-inclusion copper(II) phosphate Rb₉Na₂Cu₆(P₂O₇)₄Cl₇

The title com­pound, Rb₉Na₂Cu₆(P₂O₇)₄Cl₇, is another member of the series of salt-templated phosphates and arsenates, A₂M₃(X₂O₇)₂·(salt) [where A = K, Rb, Cs; M = Mn, Cu; X = P, As] commonly known as CU-2 materials. The structure exhibits rarely seen corner-sharing Na₄Cl₈ units.

Crystal structures of (S)-3-{1-[(4-chloro­phen­yl)sulfon­yl]piperidin-2-yl}pyridine, (S)-3-[1-(4-methyl­phen­yl)piperidin-2-yl]pyridine, (S)-3-{1-[(4-meth­oxy­phen­yl)sulfon­yl]piperidin-2-yl}pyridine and (S)-3-{1-[(3,4-di­methyl­phen­yl)sulfon­yl]piperidin-2-yl}pyridine

The crystal structures of (S)-3-{1-[(4-chloro­phen­yl)sulfon­yl]piperidin-2-yl}pyridine, (S)-3-[1-(4-methyl­phen­yl)piperidin-2-yl]pyridine, (S)-3-{1-[(4-meth­oxy­phen­yl)sulfon­yl]piperidin-2-yl}pyridine and (S)-3-{1-[(3,4-di­methyl­phen­yl)sulfon­yl]piperidin-2-yl}pyridine are compared. The similarities in the spatial structures of the mol­ecules are explained, particularly the mutual arrangement of the pyridine and piperidine rings, as well as the positioning of the aryl­sulfonyl group relative to the piperidine ring.

Crystal structure and Hirshfeld surface analysis of hydro­nium 3,5-di­carb­oxy­benzene­sulfonate trihydrate

The title com­pound crystallizes in the triclinic space group P. The structure, containing one oxonium ion and a hy­dro­gen-bonded water cluster with eight mol­ecules, forms an R₈⁶(16) ring motif through inter­molecular hy­dro­gen bonding.

Insights into [(2-phen­oxy­phen­yl)lithium(THF)(TMEDA)] and di­phenyl ether: structural influence of metalation on the aromatic system

The title compound, (2-phen­oxy­phenyl-κC¹)(tetra­hydro­furan-κO)(N,N,N′,N′-tetra­methyl­ethylenedi­amine-κ²N,N′)lithium, [Li(C₁₂H₉O)(C₆H₁₆N₂)(C₄H₈O)] or [(2-phen­oxy­phen­yl)lithium(THF)(TMEDA)] is a monomeric lithium complex in which tetra­hydro­furan (THF) and N,N,N′,N′-tetra­methyl­ethylenedi­amine (TMEDA) play essential roles in stabilizing the lithium ion and promoting a monomeric aggregate. For comparison, diphenyl ether was also redetermined at 100 K.

Synthesis and crystal structure analysis of (3aRS,6RS,7aRS)-N-(4-bromo­phen­yl)-1,6,7,7a-tetra­hydro-3a,6-ep­oxy­iso­indole-2(3H)-carboseleno­amide

There are two crystallographically independent mol­ecules in the asymmetric unit of the title compound in which the cyclo­hexene and pyrrole rings are in boat and envelope conformations, respectively. In the crystal, C—H⋯O and N—H⋯Se hydrogen bonds link the mol­ecules into [100] chains. C—H⋯π(ring) inter­actions help to consolidate the packing.

Synthesis and structure of (RS)-6-hy­droxy-6-(2-oxoprop­yl)-1,10-phenanthrolin-5(6H)-one

The title compound was synthesized by reacting phendione with acetone in ethanol under microwave irradiation. An intra­molecular C=O⋯π inter­action supports the mol­ecular conformation. In the crystal, inversion dimers linked by pairwise, bifurcated O—H⋯(N,N) hydrogen bonds are seen and the dimers are further linked by weak C—H⋯N and C—H⋯O hydrogen bonds and aromatic π–π stacking inter­actions.

Synthesis and crystal structure of di-μ-chlorido-bis­[bis­(2,6-di­methyl­pyrazine)­copper(I)] and di-μ-bromido-bis­[bis­(2,6-di­methyl­pyrazine)copper(I)]

The crystal structures of [(CuCl)₂(C₆H₈N₂)₄] (1) and [(CuBr)₂(C₆H₈N₂)₄] (2) are isotypic and consists of dinuclear complexes, in which each copper cation is tetra­hedrally coordinated by two μ-1,1 bridging halide anions and two terminally coordinated 2,6-di­methyl­pyrazine ligands.

The crystal structure of (3Z)-4-[(3-hy­droxy­phen­yl)amino]­pent-3-en-2-one: helices and π-stacking inter­actions of hy­dro­gen-bridged rings

The title com­pound displays a strong intra­molecular N—H⋯O inter­action resulting in a six-membered hy­dro­gen-bridged ring. An inter­molecular O—H⋯O hy­dro­gen bond leads to a helix formation. The Hirshfeld surface analysis of inter­molecular inter­actions is pre­sent­ed.

Crystal structure of 4-bromo-3-[(5-bromo­thio­phen-2-yl)methyl­idene]-2-(di­cyano­methyl­idene)-5,6-di­fluoro-2,3-di­hydro­inden-1-one

In the crystal, the nearly planar title mol­ecules are held together by a Br⋯O halogen bond and a C—H⋯N inter­action.

Crystal structure and Hirshfeld surface analysis of 1-(di­methyl­amino­meth­yl)-2-(pyrrolidin-1-ylmeth­yl)ferrocene complexes with zinc(II) bromide and cadmium(II) bromide

The title transition-metal complexes rac-1 and rac-2 exhibit some differences in terms of the bond lengths as well as the bond angles. Furthermore, not only the space groups, P2₁/n for rac-1 and P2₁2₁2₁ for rac-2, but also the crystal packings differ from each other, which can be seen in different configurations of the pyrrolidine substituents.

Crystal structure and Hirshfeld surface analysis of saflufenacil

The crystal structure of saflufenacil is reported for the first time, revealing an almost perpendicular arrangement of the pyrimidine and benzene rings and a two-dimensional hydrogen-bonded network that is qu­anti­tatively characterized by Hirshfeld surface and energy framework analyses.

Crystal structures of two hydrous sodium potassium molybdates: Na₃K(MoO₄)₂(H₂O)₉ and NaK(MoO₄)(H₂O)

The crystal structures of two hydrous mixed alkali orthomolybdates [Na₃K(MoO₄)₂(H₂O)₉ and NaK(MoO₄)(H₂O)] are presented, including a discussion of structural similarities with related phases.

Diadochic single crystal of an erbium–neodymium nitrate complex

Tetra­aqua­trinitratoerbium/neodymium(0.359/0.641) dihydrate exhibits structural features, including a network of water mol­ecules and extensive hydrogen bonding between layers, that are isomorphous with other light lanthanide crystal structures.

A new hexa­gonal polymorph of magnesium perchlorate hexa­hydrate obtained from an acetamide medium

A new magnesium perchlorate hexa­hydrate phase, Mg(ClO₄)₂·6H₂O, was obtained from the mixed solvents of water and acetamide. The structure crystallizes in the hexa­gonal space group P63mc and is isostructural with previously reported M(ClO₄)₂·6H₂O (M = Zn, Ni, Fe) phases. The Mg site is half occupied, indicating positional disorder of the metal cation. Prolonged crystallization leads to the formation of larger crystals consistent with an expanded unit cell, suggesting the formation of a disorder-related superstructure.

Crystal structure and computational study of 1-hy­droxy-3,6,7-trimeth­oxy-2,8-bis­(3-methyl­but-2-en-1-yl)-9H-xanthen-9-one (fuscaxanthone C)

The title compound consists of a xanthone fused ring system with hy­droxy, meth­oxy and 3-methyl­butenyl substituents. In the crystal, the mol­ecules are linked by C—H⋯O, C—H⋯π and C—O⋯π inter­actions.

Crystal structure of sunvozertinib, C₂₉H₃₅ClFN₇O₃, from synchrotron X-ray powder data and DFT optimization

The crystal structure of sunvozertinib has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques.

Crystal structure of binimetinib (Form A), C₁₇H₁₅BrF₂N₄O₃, from synchrotron X-ray powder diffraction data and density functional theory

The crystal structure of binimetinib (Form A) has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques

Midodrine hydro­chloride Form A, C₁₂H₁₉N₂O₄⁺·Cl⁻

The crystal structure of midodrine hydro­chloride Form A has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques.

Avutometinib

The crystal structure of avutometinib has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques.

Synthesis, crystal structure and Hirshfeld analysis of the bis­{(E)-2-[1-(benzo[d][1,3]dioxol-5-yl)ethyl­idene]-N-ethyl­hydrazine-1-carbo­thio­amide-κS}di­chlorido­mercury(II) complex

The synthesis, crystal structure and Hirshfeld analysis of the Hg^II complex with two mol­ecules of (E)-2-[1-(benzo[d][1,3]dioxol-5-yl)ethyl­idene]-N-ethyl­hydrazine-1-carbo­thio­amide, acting as κS-donors, and two chlorido ligands are reported. For the first time, the structural N—H⋯Cl intra­molecular inter­actions for TSC–mercury(II) complexes are addressed as a chelate-like coordination environment with S(6) graph-set motifs.

Crystal structure and Hirshfeld surface analyses, inter­action energy calculations and energy frameworks of (Z)-4-benzyl-2-(4-methyl­benzyl­idene)-2H-[1,4]benzo­thia­zin-3(4H)-one

The thia­zine ring exhibits a screw-boat conformation and is significantly folded along the S⋯N axis. In the crystal, mol­ecules pack in wave-like layers parallel to the bc plane aided by C—H⋯π(ring) inter­actions.

Synthesis and structure of (Z)-2-(eth­oxy­methyl­idene)-8-methyl-2,3,4,9-tetra­hydro-1H-carbazol-1-one

In the extended structure of the title compound, N—H⋯O hydrogen bonds connect the mol­ecules into [100] chains and weak C—H⋯O inter­actions and pairwise C—H⋯π inter­actions consolidate the packing.

Synthesis and structure of 1-{(E)-[(6-meth­oxy­pyridin-2-yl)methyl­idene]amino}-3-phenyl­thio­urea

In the title com­pound, the mol­ecular conformation is supported by two intra­molecular N—H⋯N hy­dro­gen bonds. In the extended structure, N—H⋯O hy­dro­gen bonds link the mol­ecules into [011] chains.

Synthesis and crystal structure of a mixed-metal 3D coordination polymer poly[[bis­(μ₅-anthra­quinone-1,8-di­sulfonato-κ⁵O:O′:O′′:O′′′:O′′′′)di-μ₂-aqua-κ⁴O:O-tetra­aqua­copper(II)disodium] dihydrate]

A Na^I–Cu^II mixed-metal three-dimensional coordination polymer based on anthra­quinone-1,8-di­sulfonate has been synthesized and characterized by single-crystal X-ray diffraction, infrared spectroscopy and thermogravimetric analysis. The complex exhibits a three-dimensional pillar-layered coordination framework with rich hydrogen-bonding motifs in the solid state.

Dibasic 3,3′-di­nitro-4,4′-bi­pyrazole-1,1′-diides of K, Rb and Cs reveal metal-selective ring–π over ring–N coordination

A series of late alkali metal salts introduce electron-depleted nitro­pyrazolate anions as common N-ligands for K⁺ and Rb⁺, but π-ligands for softer Lewis acid Cs⁺.

Crystal structure of a tetra­nuclear copper(II) complex with 1,10-phenanthroline and 3-nitro­phthalate ligands

A tetra­nuclear copper(II) complex assembled from 1,10-phenanthroline and 3-nitro­phthalate ligands features carboxyl­ate-bridged metal centres and supra­molecular stabilization via hydrogen bonding and aromatic π–π stacking inter­actions.

Crystal structure and Hirshfeld surface analysis of 1-(furan-2-yl)-2-(thio­phene-2-carbon­yl)-3-(thio­phen-2-yl)-2,3,3a,8a-tetra­hydro­cyclo­penta­[a]inden-8(1H)-one

In the crystal, pairs of mol­ecules are connected by C—H⋯O hydrogen inter­actions, generating R²₂(10) ring motifs. Pairs of mol­ecules are further linked by C—H⋯O inter­actions, forming ribbons propagating along the a-axis direction. C—H⋯π inter­actions between these ribbons create layers parallel to the (001) plane. van der Waals inter­actions between the layers maintain the cohesion of the crystal structure.

Synthesis and structure of 2-amino-4-methyl­pyridin-1-ium hippurate dihydrate

In the title salt, the crystal structure features N—H⋯O and O—H⋯O hydrogen-bonding inter­actions, which link the components into infinite chains and generate an extended supra­molecular network.

Levosimendan Form I, C₁₄H₁₂N₆O

The crystal structure of levosimendan Form I has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques.

[Tpy₂Co][Co(CO)₄]: a mixed-valent cobalt(III)/cobalt(−I) com­plex based on phenyl­tris­(pyridin-2-yl)borate (Tpy⁻)

The reaction of hy­dro­gen phenyl­tris­(pyridin-2-yl)borate (TpyH), tri­ethyl­amine, and Co(CO)₄I gives a mixed-valent salt [Tpy₂Co][Co(CO)₄], consisting of a homoleptic cobalt(III) com­plex and a cobalt(–I) counter-ion. [Tpy₂Co][Co(CO)₄] represents the first mixed-valent tris­(pyridin-2-yl)borate com­plex.

Solid-state structure and supra­molecular packing of 1,2-bis­(2-phenyl-1H-benzo[d]imidazol-1-yl)diazene

The title compound crystallizes in the monoclinic space group P2₁/c. The primary inter­molecular inter­actions are π–π stacking with the mol­ecules organized in one-dimensional π-stacks along the a-axis direction and two-dimensional ribbons parallel to the bc plane.

Synthesis, crystal structure determination, Hirshfeld surface and crystal void analyses, inter­action energy calculations and energy frameworks of (3aRS,4RS,9aRS)-2-benzyl-3-oxo-2,3,3a,4,9,9a-hexa­hydro-1H-benzo[f]iso­indole-4-carb­oxy­lic acid

The asymmetric unit of the title compound consists of a benzyl moiety bonded to the nitro­gen atom of a 1H-benzo[f]iso­indole-4-carb­oxy­lic acid group. In the crystal, O—H⋯O and C—H⋯O hydrogen bonds link the mol­ecules into infinite double-chains along the a-axis direction. π–π stacking inter­actions and C—H⋯π(ring) inter­actions help to consolidate the packing.

Crystal structure of nicotinamide ethyl­ene glycol hemisolvate

The asymmetric unit of the title solvate consists of one nicotinamide mol­ecule and half of an ethyl­ene glycol mol­ecule, which is completed by crystallographic inversion symmetry. The dihedral angle between the acetamide group and the pyridine ring is 21.9 (8)°. In the crystal, the components are linked by N—H⋯O and O—H⋯N hydrogen bonds into (102) sheets and weak offset π–π stacking is also observed.

Crystal structure and Hirshfeld surface analysis of 5-bromo-1,3,4-thia­diazol-2-amine

In the crystal of the title compound, N—H⋯N hydrogen bonds connect mol­ecules together, forming ribbons connected along the c-axis direction. The actual packing between these ribbons is a result of Br—Br repulsion (steric and/or electrostatic) and they form a zipper-like pattern that obstructs each other's path.

Crystal structure and Hirshfeld surface analysis of 3-acetyl-11-keto-β-boswellic acid

The title compound crystallizes in the ortho­rhom­bic space group P2₁2₁2 and exhibits a rigid penta­cyclic framework with eleven stereogenic centres. The cyclo­hexane rings adopt near-ideal chair conformations with minimal steric strain. The crystal packing is governed by O—H⋯O hydrogen bonds, forming zigzag chains along the [100] direction and extending into a three-dimensional network and is further consolidated by van der Waals inter­actions.

Synthesis and crystal structure of catena-poly[[[aqua­(2,3-di­methyl­pyrazine-κN)cadmium(II)]-di-μ-bromido] 2,3-di­methyl­pyrazine monosolvate hemihydrate]

In the crystal structure of CdBr₂(2,3-di­methyl­pyrazine)(H₂O)-2,3-di­methyl­pyrazine-solvate hemihydrate, the cadmium cations are linked by pairs of μ-1,1 bridging bromide anions into chains that are linked by inter­molecular hydrogen bonding to the water and the 2,3-di­methyl­pyrazine solvate mol­ecules.

Preparation of a chloride salt of covalently modified isoniazid

A novel covalently modified isoniazid salt {4-[N′-(propan-2-yl­idene)hydrazinecarbon­yl]pyridin-1-ium chloride}, C₉H₁₂N₃O⁺·Cl⁻, was synthesized using a slow diffusion layering technique under ambient conditions. The crystal structure features prominent N—H⋯Cl hydrogen bonds, indicating strong inter­molecular inter­actions between the chloride ion and the modified isoniazid framework.

Crystal structure of (3R,5aS,6R,9R,12R,12aR)-3,6,9-tri­methyl­deca­hydro-12H-3,12-ep­oxy[1,2]dioxepino[4,3-i]isochromen-10-yl 5-((3aS,4S,6aR)-2-oxohexa­hydro-1H-thieno[3,4-d]imidazol-4-yl)penta­noate

In the title biotin-conjugated di­hydro­artemisinin (DHA) derivative, the mol­ecule retains the essential endoperoxide bridge and links the C-10 position of DHA to the penta­noate chain of biotin via an ester bond. This structure determination provides a valuable blueprint for the rational design of hybrid anti­malarial and anti­cancer therapies based on DHA–biotin conjugates.

Mol­ecular and crystal structure of catena-poly[1-benzyl-[1,2,4]triazolo[1,5-c]quinazolin-1-ium-2,5-bis­(thiol­ate) [[aqua­sodium]-di-μ-aqua]]

The crystal structure of the title compound shows a layered arrangement stacked along [100] where layers of ¹_∞[Na(H₂O)_1/1(H₂O)_4/2] chains are sandwiched by layers of mol­ecular anions.