0000000001299668

AUTHOR

Andris Actiņš

showing 79 related works from this author

Polymorphism and solvates of flecainide base

2013

Flecainide base is pharmaceutically active substance used for production of flecainide acetate which is known in market as Tambacor, Almarytm, Apocard, Ecrinal or Flecaine. It is determined that flecainide base forms four polymorphic forms abbreviated as Ib, IIb, IIIb and IVb. Flecainide base form Ib is thermodynamically stable form at laboratory temperature while form IIIb is stable at higher temperatures. Flecainide form Ib absorbs water in its structure between layers and forms non-stoichiometric hydrate. Flecainide base binds with organic solvents and form monosolvates. Flecainide base form Ib crystallizes in orthorhombic crystals with lattice parameters a = 27.88 Å, b = 13.78 Å, c = 9.…

Voltage-Gated Sodium Channel BlockersFlecainideChemistryWaterPharmaceutical ScienceGeneral MedicineFlecainide Acetatelaw.inventionCrystallographyX-Ray DiffractionPolymorphism (materials science)lawX-ray crystallographymedicineThermodynamicsMoleculeOrthorhombic crystal systemCrystallizationCrystallizationHydrateAnti-Arrhythmia AgentsFlecainidemedicine.drugPharmaceutical Development and Technology
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The effect of excipients on the stability and phase transition rate of xylazine hydrochloride and zopiclone

2015

The compatibility of thermodynamically unstable polymorph of two active pharmaceutical compounds (xylazine hydrochloride form X and zopiclone form C) with different excipients was investigated. The effects of the excipient and its amount in the sample on the thermal properties and possible chemical interactions were studied. The most commonly used excipients in the pharmaceutical industry - calcium carbonate, lactose hydrate, cellulose, magnesium stearate hydrate and calcium stearate hydrate were selected for this study. The dependence of the phase transition rate from an unstable to a more stable polymorph on the excipients and their amounts in the initial sample was analysed at 80°C, and …

XylazinePhase transitionDrug IndustryClinical BiochemistryPharmaceutical ScienceExcipientCalcium stearatePhase TransitionPiperazinesAnalytical ChemistryExcipientschemistry.chemical_compoundReaction rate constantDrug StabilityDrug DiscoverymedicineMagnesium stearateCelluloseSpectroscopyChromatographyTemperatureKineticsCalcium carbonatechemistryThermodynamicsHydrateAzabicyclo CompoundsNuclear chemistrymedicine.drugJournal of Pharmaceutical and Biomedical Analysis
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Enrichment and activation of smectite-poor clay

2011

A new method of smectite clay enrichment has been developed. The method is based on dispersing clay in a phosphate solution and sequential coagulation. The product of enrichment is characterized with X-ray powder diffraction, wavelength dispersive X-ray fluorescence spectrometry, differential thermal analysis and thermogravimetry. Sorption of methylene blue and hexadecylpyridinium bromide on raw and purified clays was studied.

inorganic chemicalsChemistryInorganic chemistryFluorescence spectrometrySorptionPhosphatecomplex mixturesThermogravimetrychemistry.chemical_compoundDifferential thermal analysisClay mineralsPowder diffractionMethylene blueNuclear chemistryIOP Conference Series: Materials Science and Engineering
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Solvates of Dasatinib: Diversity and Isostructurality

2015

A series of dasatinib crystalline forms were obtained, and a hierarchical cluster analysis of their powder X-ray diffraction patterns was performed. The resulting dendrogram implies 3 structural groups. The crystal structures of several solvates representing 2 of these groups were determined. The crystal structure analysis confirms the isostructurality of solvates within structural group I and suggests a correlation between solvent molecule size and trends in crystal structures within this group. In addition, the formation relationships in 2-solvent media between different dasatinib solvate groups were determined. The formation preference of solvates was found to follow the ranking group I …

Models MolecularStereochemistryGroup iiDasatinibPharmaceutical ScienceAntineoplastic Agents02 engineering and technologyCrystal structure010402 general chemistry01 natural scienceslaw.inventionX-Ray DiffractionlawGroup (periodic table)medicineCluster AnalysisCrystallizationChemistrySolvation021001 nanoscience & nanotechnology0104 chemical sciencesDasatinibCrystallographyX-ray crystallographyCrystallization0210 nano-technologyPowder DiffractionPowder diffractionmedicine.drugJournal of Pharmaceutical Sciences
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On the Formation of Droperidol Solvates: Characterization of Structure and Properties

2014

A solvate screening and characterization of the obtained solvates was performed to rationalize and understand the solvate formation of active pharamaceutical ingredient droperidol. The solvate screening revealed that droperidol can form 11 different solvates. The analysis of the crystal structures and molecular properties revealed that droperidol solvate formation is mainly driven by the inability of droperidol molecules to pack efficiently. The obtained droperidol solvates were characterized by X-ray diffraction and thermal analysis. It was found that droperidol forms seven nonstoichiometric isostructural solvates, and the crystal structures were determined for five of these solvates. To b…

ChemistryStereochemistryGeneral ChemistryCrystal structureCondensed Matter PhysicsSolventCrystallographyLattice constantmedicineMoleculeGeneral Materials ScienceIsostructuralHydrateThermal analysisDroperidolmedicine.drugCrystal Growth & Design
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Optimization of sample preparation conditions for detecting trace amounts of β-tegafur in α- and β-tegafur mixture.

2012

We report a semiquantitative method for determining trace amounts (<1%) of thermodynamically stable forms in polymorphic mixtures, focusing on sample preparation ef- fects on solid phase transitions. Tegafur (5-fluoro-1-(oxolan-2-yl)-1,2,3,4-tetrahydropyrimidine- 2,4-dione) was used as a model material in this study. The amounts of the thermodynamically stable $ tegafur were increased to levels detectable by powder X-ray diffractometry by grind- ing the samples in a ball mill in the presence of water. The limit of detection for this method was as low as 0.0005% of $ tegafur in " and $ tegafur mixtures. The amount of $ tegafur after sample preparation was found to be proportional to the init…

Detection limitLangmuirAntimetabolites AntineoplasticTrace AmountsChemistryAnalytical chemistryPharmaceutical ScienceTegafurPhase TransitionPolymorphism (materials science)IsomerismX-Ray DiffractionLimit of DetectionmedicineThermodynamicsSample preparationBall millMass fractionPowder Diffractionmedicine.drugTegafurJournal of pharmaceutical sciences
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Organic solvent desorption from two tegafur polymorphs.

2013

Desorption behavior of 8 different solvents from α and β tegafur (5-fluoro-1-(tetrahydro-2-furyl)uracil) has been studied in this work. Solvent desorption from samples stored at 95% and 50% relative solvent vapor pressure was studied in isothermal conditions at 30 °C. The results of this study demonstrated that: solvent desorption rate did not differ significantly for both phases; solvent desorption in all cases occurred faster from samples with the largest particle size; and solvent desorption in most cases occurred in two steps. Structure differences and their surface properties were not of great importance on the solvent desorption rates because the main factor affecting desorption rate …

Antimetabolites AntineoplasticVapor PressureChemistry PharmaceuticalInorganic chemistryEthyl acetatePharmaceutical ScienceElectron donorSolventchemistry.chemical_compoundAdsorptionchemistryDesorptionSolventsAdsorptionSolvent effectsAcetonitrileCrystallizationTetrahydrofuranTegafurInternational journal of pharmaceutics
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The influence of pH on the stability of antazoline: kinetic analysis

2015

Degradation of the drug antazoline was studied in aqueous solutions by means of pH-rate profiling (pH 0–7.4). The novel approach of Runge–Kutta numerical integration in combination with multi-parameter optimisation was applied to UV-Vis spectral data to determine a valid kinetic model and kinetic parameters of the degradation process. The overall degradation mechanism was found to be dependent on the environmental pH. In the pH range of 3.0–7.4, the formation of the antazoline hydrolysis product (N-(2-aminoethyl)-2-(N-benzylanilino)acetamide) through three different pathways (acidic, non-catalysed, and semi-alkaline hydrolysis) was observed. In highly acidic media (pH 0–2), the degradation …

Aqueous solutionChemistryGeneral Chemical EngineeringKinetic analysisInorganic chemistryAnalytical chemistryGeneral ChemistryKinetic energyHigh-performance liquid chromatographychemistry.chemical_compoundHydrolysisAntazolinemedicineSpectral dataAcetamidemedicine.drugRSC Advances
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Comparison and Rationalization of Droperidol Isostructural Solvate Stability: An Experimental and Computational Study

2014

In order to find a tool for comparison of solvate stability and to rationalize their relative stability, droperidol nonstoichiometric isostructural solvates were characterized experimentally and computationally. For the experimental evaluation of stability, three comparison tools were considered: thermal stability characterized by the desolvation rate, desolvation activation energy, and solvent sorption–desorption isotherms. It was found that the desolvation process was limited by diffusion, and the same activation energy values were obtained for all of the characterized solvates, while the solvent content in the sorption isotherm was determined by the steric factors. Therefore, the only cr…

Steric effectsChemistryDiffusionThermodynamicsGeneral ChemistryActivation energyCondensed Matter PhysicsStability (probability)SolventCrystallographyGeneral Materials ScienceDesolvationThermal stabilityIsostructuralCrystal Growth &amp; Design
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On the Rationalization of Formation of Solvates: Experimental and Computational Study of Solid Forms of Several Nitrobenzoic Acid Derivatives

2020

Analysis of crystal structures, molecular properties, interaction strength in solution and computationally generated non-solvated form solid form landscapes of five chloronitrobenzoic acid isomers ...

010405 organic chemistryRationalization (psychology)Interaction strengthGeneral ChemistryCrystal structure010402 general chemistryCondensed Matter Physics01 natural sciences0104 chemical scienceschemistry.chemical_compoundchemistryComputational chemistryNitrobenzoic acidGeneral Materials ScienceCrystal Growth &amp; Design
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Why Do Chemically Similar Pharmaceutical Molecules Crystallize in Different Structures: A Case of Droperidol and Benperidol

2016

A detailed study of molecular conformation and intermolecular interactions in the experimental crystal structures and general trends observed in the Cambridge Structural Database as well as theoretical calculations were performed to identify the reason for the formation of different crystal structures of two chemically very similar pharmaceutical molecules benperidol and droperidol. The most important difference between both molecules was the weak intermolecular interactions formed by the central ring which therefore was responsible for the formation of different crystal structures. Cross-seeding experiments were performed to check the possibility for the formation of mutually isostructural…

ChemistryIntermolecular force02 engineering and technologyGeneral ChemistryCrystal structure010402 general chemistry021001 nanoscience & nanotechnologyCondensed Matter PhysicsRing (chemistry)01 natural sciencesMolecular conformation0104 chemical sciencesBenperidolCrystallographymedicineMoleculeGeneral Materials ScienceIsostructural0210 nano-technologyDroperidolmedicine.drugCrystal Growth &amp; Design
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Organic solvent vapor effects on phase transition of α and β tegafur upon grinding with solvent additives.

2012

Abstract Solvent effects on α tegafur (5-fluoro-1-(tetrahydro-2-furyl)uracil) phase transition to β tegafur during grinding with solvent additive, as well as phase transition in samples exposed to 95% relative solvent vapor pressure has been studied in this research. Samples containing 0.5% and 0.1% of β tegafur in α and β tegafur mixture, as well as samples of pure α tegafur were ground with different solvent additives, and conversion degrees depending on the solvent were determined using PXRD method. Samples with α and β tegafur weight fraction of 1:1 were exposed to 95% relative solvent vapor pressure, and phase transition rates were determined. Solubility of α tegafur, solvent sorption …

Vapor PressureChemistryDrug CompoundingInorganic chemistryPharmaceutical ScienceSorptionTegafurPhase TransitionSolventPolymorphism (materials science)IsomerismSolubilityX-Ray DiffractionDesorptionAlcoholsmedicineSolventsThermodynamicsAdsorptionSolubilitySolvent effectsVolatilizationMass fractionmedicine.drugTegafurInternational journal of pharmaceutics
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Investigation of the phase transitions occurring during and after the dehydration of xylazine hydrochloride monohydrate.

2014

This paper reports an investigation of a complex solid state phase transition where two inter-converting polymorphs (X and A) of the pharmaceutical molecule xylazine hydrochloride formed and transformed during and after the dehydration of its monohydrate (H). The crystal structures of all three forms were compared. During the investigation of this solid state phase transition it was determined that the dehydration of H produced either a pure X form, or a mixture of the X and A forms. The phase composition depended on the sample preparation procedure and the experimental conditions. It was found that grinding of the hydrate enhanced the formation of polymorph X as a product of dehydration, w…

Models MolecularXylazinePhase transitionPharmaceutical ScienceCrystal structureCrystallography X-RayPhase TransitionDrug StabilitymedicineMoleculeTechnology PharmaceuticalSample preparationRelative humidityDehydrationDesiccationParticle SizeMicroscopyChemistryTemperatureWaterHumiditymedicine.diseaseGrindingCrystallographyKineticsHydrateCrystallizationPowder DiffractionInternational journal of pharmaceutics
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Dehydration of mildronate dihydrate: a study of structural transformations and kinetics

2014

The dehydration of mildronate dihydrate (3-(1,1,1-trimethylhydrazin-1-ium-2-yl)propionate dihydrate) was investigated by powder X-ray diffraction, thermal analysis, hot-stage microscopy, water sorption–desorption studies and dehydration kinetic studies. It was determined that mildronate dihydrate dehydrated in a single step, directly transforming into the anhydrous form. In order to understand the reasons for a one step dehydration mechanism, crystal structures of dihydrate, monohydrate and anhydrous forms were compared, proving the similarity of the dihydrate and anhydrous forms. In order to understand the reasons for molecule reorganization during dehydration, the energy of the anhydrous …

Phase boundaryChemistryInorganic chemistryKineticsGeneral ChemistryCrystal structureCondensed Matter Physicsmedicine.diseaseRate-determining stepPhase (matter)medicineAnhydrousPhysical chemistryGeneral Materials ScienceDehydrationThermal analysisCrystEngComm
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Powder X-Ray Diffraction Investigation of Xylazine Hydrochloride Solid Phase Transformation Kinetics

2013

The kinetics of the solid-state phase transformation of xylazine hydrochloride form X to A has been investigated using powder X-ray diffraction and differential thermal analysis. Three different kinetic models have been used to describe transition kinetics: the Avrami–Erofeev equation, the Cardew equation, and the methodology for simulation of solid-state phase transition kinetics by the combination of nucleation and nuclei growth processes. The latter has been recently developed and has been tested in this paper for the case of a real solid-state transition. The relative humidity, mechanical pressure, temperature, and sample-preparation effect on phase-transition kinetics have been investi…

DiffractionChemistryOrganic ChemistryKineticsNucleationThermodynamicsBiochemistryInorganic ChemistryReaction rate constantPhase (matter)Differential thermal analysisX-ray crystallographyPhysical chemistryRelative humidityPhysical and Theoretical ChemistryInternational Journal of Chemical Kinetics
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Structure and Stability of Racemic and Enantiopure Pimobendan Monohydrates: On the Phenomenon of Unusually High Stability

2017

Study of structures and physicochemical properties of racemic (rac-H) and enantiopure (enant-H) hydrates of the active pharmaceutical ingredient pimobendan revealed that both hydrates have highly similar crystal structures and exhibit unusually high stability. Both structures contain identical two-dimensional layers and very similar conformations. The most significant difference is the stacking of these layers. The high stability of both hydrates appeared as extremely low solubility over a wide temperature range as well as an exceptionally high dehydration temperature and melting point. Study of the dehydration process showed that both hydrates have different activation energies of dehydrat…

Hydrogen bondChemistryStacking02 engineering and technologyGeneral ChemistryCrystal structureAtmospheric temperature range010402 general chemistry021001 nanoscience & nanotechnologyCondensed Matter Physics01 natural sciences0104 chemical sciencesCrystallographyEnantiopure drugMelting pointOrganic chemistryGeneral Materials ScienceSolubility0210 nano-technologyDispersion (chemistry)Crystal Growth &amp; Design
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Single Enantiomer’s Urge to Crystallize in Centrosymmetric Space Groups: Solid Solutions of Phenylpiracetam

2017

A detailed thermochemical and structural study of the phenylpiracetam enantiomer system was performed by characterizing the solid solutions, rationalizing the structural driving force for their formation, as well as identifying a common structural origin responsible for the formation of solid solutions of enantiomers. Enantiomerically pure phenylpiracetam forms two enantiotropically related polymorphs (enant–A and enant–B). The transition point (70(7) °C) was determined based on isobaric heat capacity measurements. Structural studies revealed that enant–A and enant–B crystallize in space groups P1 (Z′ = 4) and P212121 (Z′ = 2), respectively. However, pseudoinversion centers were present res…

010405 organic chemistryChemistrySpace groupGeneral Chemistry010402 general chemistryCondensed Matter PhysicsCentrosymmetry01 natural sciencesMiscibilityHeat capacity0104 chemical sciencesCrystallographyTransition pointIsobaric processGeneral Materials ScienceEnantiomerSolid solutionCrystal Growth &amp; Design
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Polymorphs and Hydrates of Sequifenadine Hydrochloride: Crystallographic Explanation of Observed Phase Transitions and Thermodynamic Stability

2017

In this study, detailed analysis of crystal structures was used to rationalize the observed stability and phase transformations of sequifenadine hydrochloride polymorphs and hydrates, as well as to understand the observed structural diversity. The performed polymorph and hydrate screening revealed the existence of six polymorphs and four hydrates. Crystal structures of these phases were determined either from single crystal or from powder diffraction data. The different possibilities for packing of sequifenadine cations were found to be the main reason for the observed structural diversity of polymorphs. The hydrate structures were found to be structurally similar and related to those of pa…

Phase transitionChemistryHydrochloride02 engineering and technologyGeneral ChemistryCrystal structure010402 general chemistry021001 nanoscience & nanotechnologyCondensed Matter Physics01 natural sciences0104 chemical sciencesCrystallographychemistry.chemical_compoundPhase (matter)General Materials ScienceChemical stability0210 nano-technologyHydrateSingle crystalPowder diffractionCrystal Growth &amp; Design
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Three anhydrous forms and a dihydrate form of quifenadine hydrochloride: a structural study of the thermodynamic stability and dehydration mechanism

2015

Crystal structures of dihydrate (DH) and three anhydrous forms (A, B and C) of quifenadine (1-azabicyclo[2.2.2]oct-8-yl-diphenyl-methanol) hydrochloride are presented, and crystal structure information is used to explain and rationalize the relative stability of polymorphs and observed phase transformations. The dehydration mechanism of the hydrate is provided by interpreting the results obtained in studies of crystal structures, dehydration kinetics and thermal analysis. Structural analysis is used to explain the observed relative stability of the anhydrous phases and the hydrate. The crystal structures have been determined either from single crystal (form DH) or from powder diffraction da…

CrystallographyChemistryPhase (matter)AnhydrousGeneral Materials ScienceChemical stabilityGeneral ChemistryCrystal structureCondensed Matter PhysicsThermal analysisHydrateSingle crystalPowder diffractionCrystEngComm
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Flecainide acetate acetic acid solvates.

2011

Flecainide acetate forms acetic acid solvates with 0.5 and 2 acetic acid molecules. Powder X-ray diffraction, differential thermal analysis/thermogravimetric, infrared, and potentiometric titration were used to determine the composition of solvates. Flecainide acetate hemisolvate with acetic acid decomposes to form a new crystalline form of flecainide acetate. This form is less stable than the already known polymorphic form at all temperatures, and it is formed due to kinetic reasons. Both flecainide acetate nonsolvated and flecainide acetate hemisolvate forms crystallize in monoclinic crystals, but flecainide triacetate forms triclinic crystals. Solvate formation was not observed when flec…

FlecainideSpectrophotometry InfraredChemistryFormic acidPotentiometric titrationPharmaceutical ScienceFlecainide AcetateMedicinal chemistryAcetic acidchemistry.chemical_compoundPropanoic acidPolymorphism (materials science)SolubilityX-Ray DiffractionThermogravimetrymedicinePotentiometrySolventsOrganic chemistryCrystallizationFlecainideAnti-Arrhythmia Agentsmedicine.drugMonoclinic crystal systemAcetic AcidJournal of pharmaceutical sciences
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Hydration and dehydration kinetics of xylazine hydrochloride

2009

From the experiments where mixture of xylazine hydrochloride hydrate H and anhydrous X were held at constant conditions, the stable form of xylazine hydrochloride can be found out. To determine equilibrium relative humidity, the unstable form of xylazine hydrochloride was inserted in thermostated humidity chamber and its weight was recorded by weighing the sample outside the chamber. The kinetic model and the rate constant for each condition were determined. The rate constants give information regarding the speed of the process at every experimentally used relative humidity. Thus using the data in coordinates k – p for each temperature it is possible to determine the water vapor pressure of…

XylazineStereochemistryChemistry PharmaceuticalVapour pressure of waterEnthalpyAnalytical chemistryPharmaceutical ScienceXylazineReaction rate constantDrug StabilitymedicineRelative humidityDesiccationChemistryTemperaturefood and beveragesHumidityHumidityGeneral MedicinehumanitiesKineticsAnhydrousThermodynamicsCrystallizationHydrateAdrenergic alpha-Agonistsmedicine.drugPharmaceutical Development and Technology
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Gone to smelt iron in Courland: technology transfer in the development of an early modern industry

2019

SUMMARY: In the Duchy of Courland and Semigallia, corresponding to the southern and western parts of present-day Latvia, an iron industry based on blast-furnace technology, mainly using local bog iron ore, existed in the 17th and 18th centuries. Transfer of knowledge and skill through the recruitment of specialists from other countries of Europe was crucial to the development of this industry; technology was also re-exported to Russia and elsewhere. Recent archaeological and archaeometallurgical investigations supplement the written evidence, highlighting the specific local conditions that influenced the development of ferrous metalworking here in the early modern period. This article will …

ArcheologyHistoryGeographygeography.geographical_feature_categorybiologyTechnology transferEconomic historyIron industrySmeltbiology.organism_classificationDuchyBogPost-Medieval Archaeology
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Organic solvents vapor pressure and relative humidity effects on the phase transition rate of α and β forms of tegafur.

2011

The objective of this work was to investigate the relative humidity (RH) and solvent vapor pressure effects on the phase transition dynamics between tegafur polymorphic forms that do not form hydrates and solvates. The commercially available α and β modifications of 5-fluoro-1-(tetrahydro-2-furyl)-uracil, known as the antitumor agent tegafur, were used as model materials for this study. While investigating the phase transitions of α and β tegafur under various partial pressures of methanol, n-propanol, n-butanol, and water vapor, it was determined that the phase transition rate increased in the presence of solvent vapors, even though no solvates were formed. By increasing the relative air h…

Phase transitionAntimetabolites AntineoplasticChromatographyCapillary condensationVapor PressureChemistryVapor pressureMethanolAnalytical chemistryPharmaceutical ScienceWaterHumidityGeneral MedicinePartial pressure1-PropanolPhase TransitionReaction rate constant1-ButanolPhase (matter)Relative humidityCrystallizationWater vaporTegafurPharmaceutical development and technology
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Speciation of Substituted Benzoic Acids in Solution: Evaluation of Spectroscopic and Computational Methods for the Identification of Associates and T…

2021

Materials scienceComputational chemistrylawGenetic algorithmGeneral Materials ScienceIdentification (biology)General ChemistryCrystallizationCondensed Matter Physicslaw.inventionCrystal Growth &amp; Design
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Structural Characterization and Rationalization of Formation, Stability, and Transformations of Benperidol Solvates

2015

Experimental and theoretical characterization and studies of phase transitions and stability of the solvates obtained in solvate screening of the pharmaceutical compound benperidol were performed to rationalize and understand the solvate formation, stability, and phase transitions occurring during their desolvation. The solvate screening revealed that benperidol can form 11 solvates, including two sets of isostructural solvates. The analysis of the solvate crystal structures and molecular properties indicated that benperidol solvate formation is mainly driven by the complications during packing of benperidol molecules in an energetically efficient way in the absence of solvent molecules, as…

Phase transitionHydrogen bondChemistryGeneral ChemistryCrystal structureCondensed Matter PhysicsCharacterization (materials science)SolventBenperidolCrystallographymedicineMoleculeGeneral Materials ScienceIsostructuralmedicine.drugCrystal Growth &amp; Design
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Effect of Experimental and Sample Factors on Dehydration Kinetics of Mildronate Dihydrate: Mechanism of Dehydration and Determination of Kinetic Para…

2014

The dehydration kinetics of mildronate dihydrate [3-(1,1,1-trimethylhydrazin-1-ium-2-yl)propionate dihydrate] was analyzed in isothermal and nonisothermal modes. The particle size, sample preparation and storage, sample weight, nitrogen flow rate, relative humidity, and sample history were varied in order to evaluate the effect of these factors and to more accurately interpret the data obtained from such analysis. It was determined that comparable kinetic parameters can be obtained in both isothermal and nonisothermal mode. However, dehydration activation energy values obtained in nonisothermal mode showed variation with conversion degree because of different rate-limiting step energy at hi…

ChemistrySAMPLE historyKineticsWaterPharmaceutical ScienceThermodynamicsCardiovascular AgentsActivation energyKinetic energymedicine.diseaseIsothermal processKineticsmedicineSample preparationParticle sizeDehydrationParticle SizeMethylhydrazinesJournal of Pharmaceutical Sciences
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Formation and Transformations of Organic Salt Hydrates: Four Encenicline Hydrochloride Monohydrates and Respective Isostructural Desolvates

2018

Encenicline hydrochloride (Enc-HCl) crystallizes in four different monohydrate phases, but at the same time crystallization in a nonsolvated phase is not observed, indicating that water plays a crucial role in guiding the crystallization process and ensuring structure stability. All monohydrate phases show exceptionally high stability, and the main structural motif stays intact even after dehydration, leading to isostructural (for I and II) or isomorphic (for III) desolvates. Three monohydrate phases with determined crystal structure information consists of Enc-HCl-water hexamers that are stacked into similar slabs, that are further packed identically in monohydrates I, II, and III. The fea…

chemistry.chemical_classification010405 organic chemistryHydrochlorideIntermolecular forceSalt (chemistry)General ChemistryCrystal structureRandom hexamer010402 general chemistryCondensed Matter Physics01 natural sciences0104 chemical scienceslaw.inventionchemistry.chemical_compoundCrystallographychemistrylawPhase (matter)General Materials ScienceIsostructuralCrystallizationCrystal Growth &amp; Design
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The relative stability of xylazine hydrochloride polymorphous forms

2009

All four known xylazine hydrochloride polymorphous forms were obtained and their relative stabilities were compared directly at three different temperatures. At higher temperatures, it is possible to determine the relative stability of all forms directly by measuring the changes in the composition of the mixtures of two polymorphous forms using powder x-ray diffraction methods. At lower temperatures, a solvent was added to the mixture and the changes in composition were determined. Polymorph transition temperatures were determined directly. To predict the transition temperature which was not found using the direct method, the polymorph melting data and determined transition temperatures wer…

XylazineVapor PressureVapor pressureStereochemistryChemistryTransition temperatureVapour pressure of waterTemperatureAnalytical chemistryWaterPharmaceutical ScienceGeneral Medicinelaw.inventionSolventDrug StabilityX-Ray DiffractionPolymorphism (materials science)lawX-ray crystallographySolventsAnhydrousTransition TemperatureCrystallizationCrystallizationAdrenergic alpha-AgonistsPharmaceutical Development and Technology
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The Preparation and Characterization of New Antazoline Salts with Dicarboxylic Acids

2015

New antazoline salts with organic acids (fumaric acid, oxalic acid, and maleic acid) were prepared. The effect of the crystallization solvent and mechanochemical treatment on the crystalline forms of these salts was studied. Two polymorphs of antazoline hydrogen maleate were identified and their relative stability was determined. The molecular structures of antazoline hydrogen oxalate and antazoline hydrogen maleate showed differences in antazoline cation conformation. In crystal structures of all salts both imidazoline nitrogens of antazoline cation are involved in hydrogen bond formation with carboxyl groups of the acid.

Fumaric acidMaleic acidHydrogen bondOxalic acidGeneral ChemistryCondensed Matter PhysicsOxalateSolventchemistry.chemical_compoundchemistryPolymorphism (materials science)Polymer chemistryAntazolinemedicineOrganic chemistryGeneral Materials Sciencemedicine.drugMolecular Crystals and Liquid Crystals
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Multi-technique approach for qualitative and quantitative characterization of furazidin degradation kinetics under alkaline conditions

2016

Degradation of drug furazidin was studied under different conditions of environmental pH (11-13) and temperature (30-60°C). The novel approach of hybrid hard- and soft-multivariate curve resolution-alternating least squares (HS-MCR-ALS) method was applied to UV-vis spectral data to determine a valid kinetic model and kinetic parameters of the degradation process. The system was found to be comprised of three main species and best characterized by two consecutive first-order reactions. Furazidin degradation rate was found to be highly dependent on the applied environmental conditions, showing more prominent differences between both degradation steps towards higher pH and temperature. Complim…

Clinical BiochemistryAnalytical chemistryPharmaceutical ScienceHydantoin02 engineering and technologyDerivativeKinetic energy01 natural sciencesLeast squaresMass SpectrometrySpectral lineAnalytical ChemistryHydrolysischemistry.chemical_compoundUltraviolet visible spectroscopyDrug DiscoverySpectroscopyFuraginHydrolysis010401 analytical chemistryTemperatureHydrogen-Ion Concentration021001 nanoscience & nanotechnology0104 chemical sciencesKineticschemistryDegradation (geology)Spectrophotometry Ultraviolet0210 nano-technologyJournal of Pharmaceutical and Biomedical Analysis
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Understanding complex phase transition mechanism by crystal structure analysis

2014

Xylazine hydrochloride (2-(2,6-xylidino)-5,6-dihydro-4H-1,3-thiazine hydrochloride) is an adrenergic α-agonist used as a sedative, analgesic, and muscle relaxant in veterinary medicine. It has four polymorphous forms (A, Z, M and X), monohydrate (H), hemihydrate and solvates with dichloromethane and 2-propanol. It has been reported that the polymorph X is thermodynamically the least stable of these polymorphs, while the A is the most stable form at temperatures above 500C. The X forms only in H dehydration process, and at elevated temperature X transforms to polymorph A [1]. The crystal structures of the polymorphs A and X as well as hydrate H have been reported. Crystal structure of A and …

Inorganic ChemistryPhase transitionMaterials scienceStructural BiologyChemical physicsGeneral Materials ScienceCrystal structurePhysical and Theoretical ChemistryCondensed Matter PhysicsBiochemistryMechanism (sociology)Acta Crystallographica Section A Foundations and Advances
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Determination of trace amounts of β tegafur in commercial α tegafur by powder X-ray diffractometric analysis.

2011

Abstract Objectives The main objective of this work was to develop a suitable analytical technique for determining trace amounts of the thermodynamically stable solid form in bulk samples of metastable form, to a sensitivity of 0.005%–1.0%. Tegafur (5-fluoro-1-(tetrahydro-2-furyl)-uracil) α and β crystalline forms were used as a model for this problem. Methods The trace content of the thermodynamically stable β polymorphic form in tegafur samples was increased by promoting phase transition from the bulk of thermodynamically metastable α form to β form, and achieving sufficient β form content for a quantitative powder X-ray diffractometry (PXRD) analysis. The phase transition was stimulated …

PharmacologyPhase transitionMaterials scienceTrace AmountsAnalytical chemistryPharmaceutical ScienceCrystallography X-RaySolventCrystallographyX-Ray DiffractionPhase (matter)ThermodynamicsSample preparationLeast-Squares AnalysisPowdersCrystallizationMass fractionSeed crystalPowder diffractionTegafurThe Journal of pharmacy and pharmacology
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Solvent-mediated phase transformation between two tegafur polymorphs in several solvents

2014

This paper describes a study of the solvent-mediated polymorphic transformation (SMPT) of the metastable α tegafur to the thermodynamically stable β tegafur in several solvents. Phase transformation in acetone, ethanol, i-propanol, toluene, and water at 22 °C was described using the solid-state kinetic model P2; the rate constants for this process were in the range from 0.028 min−1 to 0.0056 min−1. In all of the employed solvents, an induction time was observed. Kinetic, solubility and scanning electron microscopy data indicated that nucleation kinetics corresponded to a second-order power function and according to the kinetic model, the nuclei growth rate was constant in the examined SMPT.…

Phase transitionSupersaturationChromatographyChemistryNucleationGeneral ChemistryCondensed Matter PhysicsTolueneSolventchemistry.chemical_compoundReaction rate constantPhase (matter)Physical chemistryGeneral Materials ScienceSolubilityCrystEngComm
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Polymorphism of R-Encenicline Hydrochloride: Access to the Highest Number of Structurally Characterized Polymorphs Using Desolvation of Various Solva…

2019

In a study of the solid form landscape of R-encenicline hydrochloride (Enc-HCl), it was found that this compound is dodecamorphic and presents the first published example of polymorphism with a rec...

chemistry.chemical_compoundchemistryPolymorphism (materials science)010405 organic chemistryHydrochlorideStereochemistryGeneral Materials ScienceDesolvationGeneral Chemistry010402 general chemistryCondensed Matter Physics01 natural sciences0104 chemical sciencesCrystal Growth &amp; Design
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A Maze of Solid Solutions of Pimobendan Enantiomers: An Extraordinary Case of Polymorph and Solvate Diversity

2017

Over 10 polymorphs and solvatomorphs of the chiral pharmaceutically active ingredient pimobendan were found to lack enantioselectivity in the solid state, accordingly, forming solid solutions of enantiomers, which is reported to be a rare phenomenon. Solid form screening was performed on different enantiomeric composition samples to analyze obtained phases with powder X-ray diffraction and thermogravimetric differential scanning calorimetry. For nonsolvated forms, a melt phase diagram has been constructed convincingly showing the existence of stable and metastable solid solutions near the pure enantiomer and around the racemic composition regions. A crystal structure study combined with sol…

Thermogravimetric analysisMaterials science02 engineering and technologyGeneral ChemistryCrystal structure010402 general chemistry021001 nanoscience & nanotechnologyCondensed Matter Physics01 natural sciences0104 chemical sciencesCrystallographyDifferential scanning calorimetryPimobendanMetastabilitymedicineGeneral Materials ScienceEnantiomer0210 nano-technologyPhase diagramSolid solutionmedicine.drug
researchProduct

CCDC 910846: Experimental Crystal Structure Determination

2016

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Space GroupCrystallography1-((3-(5-nitro-2-furyl)prop-2-en-1-ylidene)amino)imidazolidine-24-dione tetrahydrofuran solvate monohydrateCrystal SystemCrystal StructureCell ParametersExperimental 3D Coordinates
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CCDC 1046558: Experimental Crystal Structure Determination

2015

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Space GroupCrystallographyCrystal System1-(1-[4-(4-Fluorophenyl)-4-oxobutyl]piperidin-4-yl)-13-dihydro-2H-benzimidazol-2-one hemihydrateCrystal StructureCell ParametersExperimental 3D Coordinates
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CCDC 1046551: Experimental Crystal Structure Determination

2015

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Space GroupCrystallographyCrystal SystemCrystal StructureCell Parameters1-(1-(4-(4-fluorophenyl)-4-oxobutyl)piperidin-4-yl)-13-dihydro-2H-benzimidazol-2-one ethyl acetate solvateExperimental 3D Coordinates
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CCDC 1051734: Experimental Crystal Structure Determination

2015

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3-(hydroxy(diphenyl)methyl)-1-azoniabicyclo[2.2.2]octane chlorideSpace GroupCrystallographyCrystal SystemCrystal StructureCell ParametersExperimental 3D Coordinates
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CCDC 1895188: Experimental Crystal Structure Determination

2020

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N-[(3R)-1-azabicyclo[2.2.2]oct-3-yl]-7-chloro-1-benzothiophene-2-carboxamide hydrochlorideSpace GroupCrystallographyCrystal SystemCrystal StructureCell ParametersExperimental 3D Coordinates
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CCDC 1895194: Experimental Crystal Structure Determination

2020

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N-[(3R)-1-azabicyclo[2.2.2]oct-3-yl]-7-chloro-1-benzothiophene-2-carboxamide hydrochlorideSpace GroupCrystallographyCrystal SystemCrystal StructureCell ParametersExperimental 3D Coordinates
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CCDC 1916269: Experimental Crystal Structure Determination

2020

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Space GroupCrystallographyCrystal SystemN-[(3R)-1-azabicyclo[2.2.2]oct-3-yl]-7-chloro-1-benzothiophene-2-carboxamide hydrochloride acetonitrile solvateCrystal StructureCell ParametersExperimental 3D Coordinates
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CCDC 1046554: Experimental Crystal Structure Determination

2015

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Space GroupCrystallographyCrystal SystemCrystal StructureCell Parameters1-(1-(4-(4-fluorophenyl)-4-oxobutyl)piperidin-4-yl)-13-dihydro-2H-benzimidazol-2-one acetonitrile solvateExperimental 3D Coordinates
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CCDC 1046552: Experimental Crystal Structure Determination

2015

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Space GroupCrystallographyCrystal SystemCrystal StructureCell Parameters1-(1-(4-(4-fluorophenyl)-4-oxobutyl)piperidin-4-yl)-13-dihydro-2H-benzimidazol-2-one ethanol solvateExperimental 3D Coordinates
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CCDC 1420813: Experimental Crystal Structure Determination

2018

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Space GroupCrystallographyN-(2-chloro-6-methylphenyl)-2-((6-(4-(2-hydroxyethyl)piperazin-1-yl)-2-methylpyrimidin-4-yl)amino)-13-thiazole-5-carboxamide dimethyl sulfoxide solvateCrystal SystemCrystal StructureCell ParametersExperimental 3D Coordinates
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CCDC 1895196: Experimental Crystal Structure Determination

2020

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Space GroupCrystallography3-[(7-chloro-1-benzothiophene-2-carbonyl)amino]-1-azabicyclo[2.2.2]octan-1-ium chlorideCrystal SystemCrystal StructureCell ParametersExperimental 3D Coordinates
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CCDC 1916266: Experimental Crystal Structure Determination

2020

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Space GroupCrystallographyCrystal SystemCrystal StructureCell Parameters3-[(7-chloro-1-benzothiophene-2-carbonyl)amino]-1-azabicyclo[2.2.2]octan-1-ium chloride monohydrateExperimental 3D Coordinates
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CCDC 1440783: Experimental Crystal Structure Determination

2016

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Space GroupCrystallographyCrystal SystemCrystal StructureCell Parameters1-(1-(4-(4-fluorophenyl)-4-oxobutyl)-1236-tetrahydropyridin-4-yl)-13-dihydro-2H-benzimidazol-2-one ethanol solvateExperimental 3D Coordinates
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CCDC 1046557: Experimental Crystal Structure Determination

2015

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Space GroupCrystallographyCrystal SystemCrystal StructureCell Parameters1-(1-(4-(4-fluorophenyl)-4-oxobutyl)piperidin-4-yl)-13-dihydro-2H-benzimidazol-2-one dihydrateExperimental 3D Coordinates
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CCDC 1916267: Experimental Crystal Structure Determination

2020

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Space GroupCrystallographyCrystal SystemCrystal StructureCell Parameters3-[(7-chloro-1-benzothiophene-2-carbonyl)amino]-1-azabicyclo[2.2.2]octan-1-ium chloride acetonitrile solvateExperimental 3D Coordinates
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CCDC 1895193: Experimental Crystal Structure Determination

2020

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N-[(3R)-1-azabicyclo[2.2.2]oct-3-yl]-7-chloro-1-benzothiophene-2-carboxamide hydrochlorideSpace GroupCrystallographyCrystal SystemCrystal StructureCell ParametersExperimental 3D Coordinates
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CCDC 1453864: Experimental Crystal Structure Determination

2017

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Space GroupCrystallography6-(2-(4-methoxyphenyl)-1H-benzimidazol-5-yl)-5-methyl-45-dihydropyridazin-3(2H)-one monohydrateCrystal SystemCrystal StructureCell ParametersExperimental 3D Coordinates
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CCDC 1420812: Experimental Crystal Structure Determination

2018

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Space GroupCrystallographyCrystal SystemCrystal StructureCell ParametersN-(2-chloro-6-methylphenyl)-2-((6-(4-(2-hydroxyethyl)piperazin-1-yl)-2-methylpyrimidin-4-yl)amino)-13-thiazole-5-carboxamide propan-2-ol solvateExperimental 3D Coordinates
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CCDC 1420811: Experimental Crystal Structure Determination

2018

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N-(2-chloro-6-methylphenyl)-2-({6-[4-(2-hydroxyethyl)piperazin-1-yl]-2-methylpyrimidin-4-yl}amino)-13-thiazole-5-carboxamide isopropyl acetate solvateSpace GroupCrystallographyCrystal SystemCrystal StructureCell ParametersExperimental 3D Coordinates
researchProduct

CCDC 1420810: Experimental Crystal Structure Determination

2018

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Space GroupCrystallographyCrystal SystemCrystal StructureCell ParametersN-(2-chloro-6-methylphenyl)-2-((6-(4-(2-hydroxyethyl)piperazin-1-yl)-2-methylpyrimidin-4-yl)amino)-13-thiazole-5-carboxamide 14-dioxane solvateExperimental 3D Coordinates
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CCDC 1895198: Experimental Crystal Structure Determination

2020

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3-[(7-chloro-1-benzothiophene-2-carbonyl)amino]-1-azabicyclo[2.2.2]octan-1-ium chloride 2-methylpropan-1-ol solvateSpace GroupCrystallographyCrystal SystemCrystal StructureCell ParametersExperimental 3D Coordinates
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CCDC 1046553: Experimental Crystal Structure Determination

2015

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Space GroupCrystallographyCrystal SystemCrystal StructureCell Parameters1-(1-(4-(4-fluorophenyl)-4-oxobutyl)piperidin-4-yl)-13-dihydro-2H-benzimidazol-2-one benzyl alcohol solvateExperimental 3D Coordinates
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CCDC 1895189: Experimental Crystal Structure Determination

2020

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Space GroupCrystallography3-[(7-chloro-1-benzothiophene-2-carbonyl)amino]-1-azabicyclo[2.2.2]octan-1-ium chloride formic acid solvateCrystal SystemCrystal StructureCell ParametersExperimental 3D Coordinates
researchProduct

CCDC 1051733: Experimental Crystal Structure Determination

2015

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3-(hydroxy(diphenyl)methyl)-1-azoniabicyclo[2.2.2]octane chlorideSpace GroupCrystallographyCrystal SystemCrystal StructureCell ParametersExperimental 3D Coordinates
researchProduct

CCDC 1895195: Experimental Crystal Structure Determination

2020

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3-[(7-chloro-1-benzothiophene-2-carbonyl)amino]-1-azabicyclo[2.2.2]octan-1-ium chloride acetic acid solvateSpace GroupCrystallographyCrystal SystemCrystal StructureCell ParametersExperimental 3D Coordinates
researchProduct

CCDC 1895199: Experimental Crystal Structure Determination

2020

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N-[(3R)-1-azabicyclo[2.2.2]oct-3-yl]-7-chloro-1-benzothiophene-2-carboxamide hydrochlorideSpace GroupCrystallographyCrystal SystemCrystal StructureCell ParametersExperimental 3D Coordinates
researchProduct

CCDC 1046550: Experimental Crystal Structure Determination

2015

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Space GroupCrystallographyCrystal SystemCrystal StructureCell Parameters1-(1-[4-(4-Fluorophenyl)-4-oxobutyl]piperidin-4-yl)-13-dihydro-2H-benzimidazol-2-one methanol solvateExperimental 3D Coordinates
researchProduct

CCDC 1051731: Experimental Crystal Structure Determination

2015

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3-(hydroxy(diphenyl)methyl)-1-azoniabicyclo[2.2.2]octane chloride dihydrateSpace GroupCrystallographyCrystal SystemCrystal StructureCell ParametersExperimental 3D Coordinates
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CCDC 1453863: Experimental Crystal Structure Determination

2017

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Space GroupCrystallographyCrystal SystemCrystal Structure(RS)-6-[2-(4-methoxyphenyl)-1H-benzimidazol-5-yl]-5-methyl-45-dihydropyridazin-3(2H)-one monohydrateCell ParametersExperimental 3D Coordinates
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CCDC 1895190: Experimental Crystal Structure Determination

2020

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Space GroupCrystallographyCrystal SystemCrystal StructureCell Parameters3-[(7-chloro-1-benzothiophene-2-carbonyl)amino]-1-azabicyclo[2.2.2]octan-1-ium chloride ethanol solvateExperimental 3D Coordinates
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CCDC 1420814: Experimental Crystal Structure Determination

2018

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Space GroupCrystallographyCrystal SystemCrystal StructureCell ParametersN-(2-chloro-6-methylphenyl)-2-({6-[4-(2-hydroxyethyl)piperazin-1-yl]-2-methylpyrimidin-4-yl}amino)-13-thiazole-5-carboxamide butyl acetate solvateExperimental 3D Coordinates
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CCDC 1046555: Experimental Crystal Structure Determination

2015

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1-(1-(4-(4-fluorophenyl)-4-oxobutyl)piperidin-4-yl)-13-dihydro-2H-benzimidazol-2-oneSpace GroupCrystallographyCrystal SystemCrystal StructureCell ParametersExperimental 3D Coordinates
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CCDC 1895192: Experimental Crystal Structure Determination

2020

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Space GroupCrystallographyCrystal SystemCrystal StructureCell Parameters3-[(7-chloro-1-benzothiophene-2-carbonyl)amino]-1-azabicyclo[2.2.2]octan-1-ium chloride acetonitrile solvateExperimental 3D Coordinates
researchProduct

CCDC 1046556: Experimental Crystal Structure Determination

2015

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Space GroupCrystallographyCrystal SystemCrystal StructureCell Parameters1-(1-[4-(4-fluorophenyl)-4-oxobutyl]piperidin-4-yl)-13-dihydro-2H-benzimidazol-2-oneExperimental 3D Coordinates
researchProduct

CCDC 1420809: Experimental Crystal Structure Determination

2018

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N-(2-chloro-6-methylphenyl)-2-({6-[4-(2-hydroxyethyl)piperazin-1-yl]-2-methylpyrimidin-4-yl}amino)-13-thiazole-5-carboxamide butan-1-ol solvateSpace GroupCrystallographyCrystal SystemCrystal StructureCell ParametersExperimental 3D Coordinates
researchProduct

CCDC 910834: Experimental Crystal Structure Determination

2016

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Space GroupCrystallographyCrystal SystemCrystal StructureCell Parameters1-((3-(5-nitro-2-furyl)prop-2-en-1-ylidene)amino)imidazolidine-24-dione NN-dimethylformamide solvate monohydrateExperimental 3D Coordinates
researchProduct

CCDC 1420807: Experimental Crystal Structure Determination

2018

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Space GroupCrystallographyCrystal SystemCrystal StructureN-(2-chloro-6-methylphenyl)-2-((6-(4-(2-hydroxyethyl)piperazin-1-yl)-2-methylpyrimidin-4-yl)amino)-13-thiazole-5-carboxamide acetone solvateCell ParametersExperimental 3D Coordinates
researchProduct

CCDC 1916268: Experimental Crystal Structure Determination

2020

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Space GroupCrystallographyCrystal SystemCrystal StructureCell Parameters3-[(7-chloro-1-benzothiophene-2-carbonyl)amino]-1-azabicyclo[2.2.2]octan-1-ium chloride acetonitrile solvateExperimental 3D Coordinates
researchProduct

CCDC 1420808: Experimental Crystal Structure Determination

2018

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Space GroupCrystallographyCrystal SystemCrystal StructureN-(2-chloro-6-methylphenyl)-2-((6-(4-(2-hydroxyethyl)piperazin-1-yl)-2-methylpyrimidin-4-yl)amino)-13-thiazole-5-carboxamide ethanol solvateCell ParametersExperimental 3D Coordinates
researchProduct

CCDC 1051732: Experimental Crystal Structure Determination

2015

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3-(hydroxy(diphenyl)methyl)-1-azoniabicyclo[2.2.2]octane chlorideSpace GroupCrystallographyCrystal SystemCrystal StructureCell ParametersExperimental 3D Coordinates
researchProduct

CCDC 1895191: Experimental Crystal Structure Determination

2020

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Space GroupCrystallographyCrystal SystemCrystal StructureCell Parameters3-[(7-chloro-1-benzothiophene-2-carbonyl)amino]-1-azabicyclo[2.2.2]octan-1-ium chloride benzyl alchohol solvateExperimental 3D Coordinates
researchProduct

CCDC 1895197: Experimental Crystal Structure Determination

2020

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N-[(3R)-1-azabicyclo[2.2.2]oct-3-yl]-7-chloro-1-benzothiophene-2-carboxamide hydrochlorideSpace GroupCrystallographyCrystal SystemCrystal StructureCell ParametersExperimental 3D Coordinates
researchProduct

CCDC 1587797: Experimental Crystal Structure Determination

2017

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Space GroupCrystallographyCrystal SystemCrystal Structure3-(222-trimethyldiazan-2-ium-1-yl)propanoate monohydrateCell ParametersExperimental 3D Coordinates
researchProduct

CCDC 1587798: Experimental Crystal Structure Determination

2017

Related Article: Agris Bērziņš, Andris Actiņš|2014|CrystEngComm|16|3926|doi:10.1039/c3ce42077a

Space GroupCrystallography3-(222-trimethyldiazan-2-ium-1-yl)propanoateCrystal SystemCrystal StructureCell ParametersExperimental 3D Coordinates
researchProduct