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Auteur : Grafiati
Publié le 7 septembre 2023

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1

Tanaka, Koichi, Naoki Daikawa et Shigeru Ohba. « Novel Bisurea Host Compounds ». Journal of Chemical Research 2002, no 11 (novembre 2002) : 579–81. http://dx.doi.org/10.3184/030823402103170853.

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New host molecules, 4,4′-bis(dimethylamino-urea)diphenylmethane (1) and its derivatives (2 and 3), are reported. These hosts are shown to give inclusion complex crystals with a wide variety of organic guest molecules with high selectivity. The crystal structure of 1:2 inclusion complex of 1 with THF has been determined from X-ray crystal structure analysis. The cyclic N–H...O intermolecular hydrogen bonds between host molecules were found to form columns for accommodation of the guest molecules.
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2

Postnikov, Valery A., Nataliya I. Sorokina, Artem A. Kulishov, Maria S. Lyasnikova, Vadim V. Grebenev, Alexey E. Voloshin, Oleg V. Borshchev et al. « Highly luminescent crystals of a novel linear π-conjugated thiophene–phenylene co-oligomer with a benzothiadiazole fragment ». Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials 75, no 6 (14 novembre 2019) : 1076–85. http://dx.doi.org/10.1107/s2052520619012484.

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The synthesis, growth from solutions and structure of crystals of a new linear thiophene–phenylene co-oligomer with a central benzothiadiazole fragment with a conjugated core, (TMS-2T-Ph)2-BTD, are presented. Single-crystal samples in the form of needles with a length of up to 7 mm were grown and their crystal structure was determined at 85 K and 293 K using single-crystal X-ray diffraction. The conformational differences between the crystal structures are insignificant. The parameters of melting and liquid crystalline phase transitions of (TMS-2T-Ph)2-BTD were established using differential scanning calorimetry and the thermal stability of the crystals was investigated using thermogravimetric analysis. The optical absorption and photoluminescence spectra of the solutions and crystals of (TMS-2T-Ph)2-BTD were obtained, and the kinetics of their photodegradation under the action of UV radiation were studied.
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3

Bolla, Geetha, et Ashwini Nangia. « Novel pharmaceutical salts of albendazole ». CrystEngComm 20, no 41 (2018) : 6394–405. http://dx.doi.org/10.1039/c8ce01311j.

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Novel pharmaceutical salts of albendazole drugs are crystallized with sulfonic acids and carboxylic acids. The disorder of the thiopropyl chain in the parent crystal structure is resolved in the salt crystal structures.
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4

Chong, Kenneth CW, Brian O. Patrick et John R. Scheffer. « The crystal structure of a simple enol formed in a single-crystal-to-single-crystal enolene rearrangement ». Canadian Journal of Chemistry 82, no 2 (1 février 2004) : 301–5. http://dx.doi.org/10.1139/v03-207.

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When crystals of 9-tricyclo[4.4.1.0]undecalyl-4-(carbomethoxy)phenyl ketone (1) were allowed to stand in the dark for extended periods of time at room temperature, the compound underwent a thermal reaction — the enolene rearrangement — to afford enol 2. The crystals remained transparent and appeared unchanged in shape as the reaction proceeded. X-ray diffraction data were collected on single crystals containing 17%, 25%, 66%, and 100% of the enol. The crystal structure of a simple enol was obtained via this novel single-crystal-to-single-crystal enolene rearrangement.Key words: single crystal, thermal, rearrangement, enol, enolene.
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5

Prasad, J. Shashidhara, M. A. Sridhar et V. Surendranath. « Crystal structure of a novel dimesogen ». Liquid Crystals 26, no 11 (janvier 1999) : 1707–12. http://dx.doi.org/10.1080/02678292.1999.11509454.

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Shashidhara Prasad, M. A. Sridhar,, J. « Crystal structure of a novel dimesogen ». Liquid Crystals 26, no 11 (1 novembre 1999) : 1707–12. http://dx.doi.org/10.1080/026782999203715.

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7

Radaelli, Paolo G., et James D. Jorgensen. « Neutron Diffraction from Novel Materials ». MRS Bulletin 24, no 12 (décembre 1999) : 24–28. http://dx.doi.org/10.1557/s0883769400053689.

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The discovery and development of new materials is the foundation of the science and technology “food chains.” Examples of new materials with novel properties that have stimulated new scientific questions and/or led to new technologies include liquid crystals, advanced batteries, structural ceramics, dielectrics, ferroelectrics, catalysts, high-temperature superconductors, har dmagnets, and magnetoresistive devices. Establishing the crystal structure of a newly discovered Compound is a mandatory first step, but the most important contribution of diffraction techniques is to provide an understanding of the relationships among chemical composition, crystal structure, and physical behavior. In this way, diffraction experiments provide critical Information for testing theories that explain novel behavior and guide the optimization of new materials to meet the demands of emerging technologies.The first samples of newly discovered materials are often polycrystalline. With state-of-the-art neutron powder diffraction data and Rietveld refinement techniques, for structures of modest complexity, the precision for atom positions rivals that obtained by single-crystal diffraction. Rietveld refinement is a method of obtaining accurate values for atom positions and other structural parameters from powder diffraction data by least-squares fitting of a calculated model to the full diffraction pattern. As evidence of thi s success, the Inorganic Crystal Structure Database contains 6044 entries from neutron powder diffraction, 7096 from laboratory x-ray powder diffraction, an d 228 from Synchrotron x-ray powder diffraction. Other reasons for the rapidly growing impact of neutron diffraction include the favorable neutron-scattering cross sections for light elements, the sensitivity to magnetic moments, and the ability to penetrate special sample environments for in situ studies. These strengths are widely accepted and have been exploited for many years. Previous reviews have focused on these topics.
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8

Shlyk, Larysa, et Rainer Niewa. « Crystal Structure and Magnetic Properties of the Novel Hollandite Ba1.3Co1.3Ti6.7O16 ». Zeitschrift für Naturforschung B 66, no 11 (1 novembre 2011) : 1097–100. http://dx.doi.org/10.1515/znb-2011-1103.

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Single crystals of the new barium hollandite Ba1.3Co1.3Ti6.7O16 were obtained from a BaCl2 flux (I2/m, Z = 1, a = 9.9470(4), b = 2.9714(2), c = 10.2260(5) Å , β = 90.906(2)◦). In the crystal structure piles of Ba atoms are situated within a framework of edge- and vertex-sharing octahedra (Co,Ti)O6. The composition was deduced from microprobe analyses, structure refinements and charge balance arguments in agreement with the observed magnetic properties. The temperature dependence of the magnetic susceptibility χ(T) of Ba1.3Co1.3Ti6.7O16 single crystals reveals paramagnetism down to 2 K. The value of the Co magnetic moment deduced from the Curie-Weiss law agrees well with the theoretical value of the high-spin state spin-only moment of μeff = 3.87 μB for Co2+ (S = 3/2)
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9

Carmely, S., T. Gebreyesus, Y. Kashman, BW Skelton, AH White et T. Yosief. « Dysidamide, a Novel Metabolite From a Red Sea Sponge Dysidea herbacea ». Australian Journal of Chemistry 43, no 11 (1990) : 1881. http://dx.doi.org/10.1071/ch9901881.

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A hexachloro metabolite, dysidamide (2) has been isolated from a Red Sea sponge Dysidea herbacea. The structure of (2) has been established from spectroscopic and chemical evidence, and confirmed by an X-ray crystal structure determination. Crystals of (2) are orthorhombic P212121, a 20.509(13), b 18.411(11), c 11.356(9)Ǻ, Z 8. The structure was refined by least-squares methods to a residual of 0.049 for 2277 'observed' reflections. Two different conformations of the molecule are present in the crystal.
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10

Alarfaj, Abeer Abdulaziz, et Hanan Ahmed Hosni Mahmoud. « Feature Fusion Deep Learning Model for Defects Prediction in Crystal Structures ». Crystals 12, no 9 (19 septembre 2022) : 1324. http://dx.doi.org/10.3390/cryst12091324.

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Detection of defective crystal structures can help in refute such defective structures to decrease industrial defects. In our research, we are concerned with Silicon nitride crystals. There are four types of crystal structure classes, namely no-defect structures, pristine crystal structures, defective random displacement crystal structures, and defective 25% vacancies crystal structures. This paper proposes a deep learning model to detect the four types of crystal structures with high accuracy and precision. The proposed model consists of both classification and regression models with a new loss function definition. After training both models, the features extracted are fused and utilized as an input to a perceptron classifier to identify the four types of crystal structures. A novel dense neural network (DNN) is proposed with a multitasking tactic. The developed multitask tactic is validated using a dataset of 16,000 crystal structures, with 30% highly defective crystals. Crystal structure images are captured under cobalt blue light. The multitask DNN model achieves an accuracy and precision of 97% and 96% respectively. Also, the average area under the curve (AUC) is 0.96 on average, which outperforms existing detection methods for crystal structures. The experiments depict the computational time comparison of a single training epoch of our model versus state-of-the-art models. the training computational time is performed using crystal structures diffraction image database of twelve image batches. It can be realized that the prediction computational time of our multitasking model is the least time of 21 s.
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11

Vasilyeva, A. A., T. Yu Glazunova, D. S. Tereshchenko et E. Kh Lermontova. « A novel сalcium trifluoroacetate structure ». Fine Chemical Technologies 16, no 4 (29 septembre 2021) : 352–62. http://dx.doi.org/10.32362/2410-6593-2021-16-4-352-362.

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Objectives. The study was devoted to considering the features of the synthesis and crystal structure of calcium trifluoroacetate Ca2(CF3COO)4·8CF3COOH and investigating the products of its thermal behavior.Methods. The compositions of the proposed structural form were characterized by various physicochemical methods (X-ray diffraction, IR spectroscopy), and the products of thermal decomposition were determined under dynamic vacuum conditions.Results. The reaction between calcium carbonate and 99% trifluoroacetic acid yielded a new structural type of calcium trifluoroacetate Ca2(CF3COO)4·8CF3COOH (I) in the form of colorless prismatic crystals unstable air. X-ray diffraction results confirmed the composition I: space group P21, with unit cell parameters: a = 10.0193(5) Å, b = 15.2612(7) Å, c = 16.3342(8) Å, β = 106.106(2)°, V = 2399.6(2) Å3, Z = 2. The structure is molecular, constructed from Ca2(CF3COO)4·8CF3COOH dimers. The end molecules of the trifluoroacetic acid were involved in the formation of intramolecular hydrogen bonds with oxygen atoms of the bidentate bridging anions CF3COO−. There were strongly pronouncedsymmetric and asymmetric absorption bands of COO and CF3-groups in the IR spectrum of the resulting compound in the range of 1200–1800 cm−1. The definite peak of the oscillation of the OH-group at 3683 cm−1 corresponds to the trifluoroacetic acid molecules present in the structure. The broadpeak of the valence oscillations in the range of 3300–3500 cm−1 is caused by the presence of intramolecular hydrogen bonds. Decomposition began at 250°C and 10−2 mm Hg with calcium fluoride CaF2 as the final decomposition product.Conclusions. We obtained a previously undescribed calcium–trifluoroacetic acid complex whose composition can be represented by Ca2(CF3COO)4·8CF3COOH. The crystal island structure is a dimeric molecule where the calcium atoms are bound into dimers by four trifluoroacetate groups. The complex was deposited in the Cambridge Structural Data Bank with a deposit number CCDC 2081186. Although the compound has a molecular structure, thermal decomposition leads to the formation of calcium fluoride characterized by a small particle size, which may further determine its applications.
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12

Zhang, Fajun, Georg Zocher, Andrea Sauter, Thilo Stehle et Frank Schreiber. « Novel approach to controlled protein crystallization through ligandation of yttrium cations ». Journal of Applied Crystallography 44, no 4 (8 juin 2011) : 755–62. http://dx.doi.org/10.1107/s0021889811017997.

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Crystal structure determination of macromolecules is often hampered by the lack of crystals suitable for diffraction experiments. This article describes a protocol to crystallize the acidic protein bovine β-lactoglobulin in the presence of yttrium to yield high-quality crystals that belong to a new space group. The yttrium ions not only are used to engineer the crystallization, but are an integral part of the crystal lattice and can therefore be used to solve the phase problem using anomalous dispersion methods. Protein crystallization conditions were first optimized using an experimental phase diagram in the protein and salt concentration plane. Crystal growth strongly depends on the position in the phase diagram, and the best crystals grow near the phase transition boundaries. The structure analysis demonstrates the specific binding of yttrium ions to surface-exposed glutamate and aspartate side chains contributed by different molecules in the crystal lattice. By bridging molecules in this manner, contacts between molecules are formed that enable the formation of a stable crystal lattice. The potential application of this strategy to the crystallization of other acidic proteins is discussed on the basis of the universal features of the phase behavior of these proteins and the interactions induced by multivalent ions.
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13

Yakubovich, O. V., et O. V. Dimitrova. « Novel Polyoxovanadate K2ZnV5O14 : Crystal Structure and Peculiarities of Crystal Chemistry ». Crystallography Reports 63, no 5 (septembre 2018) : 738–44. http://dx.doi.org/10.1134/s1063774518050322.

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14

Wierzbicka-Wieczorek, Maria, et Gerald Giester. « Novel silicates with apatite crystal structure type ». Acta Crystallographica Section A Foundations of Crystallography 69, a1 (25 août 2013) : s458. http://dx.doi.org/10.1107/s0108767313096025.

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Wierzbicka-Wieczorek, Maria, et Gerald Giester. « Novel silicates with apatite crystal structure type ». Acta Crystallographica Section A Foundations of Crystallography 69, a1 (25 août 2013) : s133. http://dx.doi.org/10.1107/s0108767313098887.

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16

Tratsiak, Katsiaryna, Tatyana Prudnikova, Ivana Drienovska, Lukas Chrast, Jiri Damborsky, Pavlina Rezacova, Michal Kuty, Radka Chaloupkova et Ivana Kuta Smatanova. « Crystal structure of the novel haloalkane dehalogenases ». Acta Crystallographica Section A Foundations and Advances 70, a1 (5 août 2014) : C1678. http://dx.doi.org/10.1107/s2053273314083211.

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Haloalkane dehalogenases (EC 3.8.1.5; HLDs) are microbial enzymes with catalytic activity for the hydrolytic conversion of xenobiotic and highly toxic halogenated aliphatic compounds to the corresponding alcohols. Biodegradation, biosensing, biocatalysis and cellular imaging are potentially practical applications for the HLDs. Two newly isolated and purified psychrophilic haloalkane dehalogenases, exhibiting interesting catalytic properties, DpcA from Psychrobacter cryohalolentis K5 and DmxA from Marinobacter sp. ELB17, were used for the crystallization experiments and structure determination. Diffracted crystals of DpcA(left) and DmxA(right) (see figure, the scale bar -100μm) were refined up to the 1.05 Å and 1.45 Å resolutions, respectively. Diffraction data for DpcA were collected on beamline 14.2 at the BESSY II electron-storage ring (Helmholtz-Zentrum Berlin (HZB), Germany) and equipped with a Rayonics MX-225 CCD detector at the wavelengths of 0.978 Å, and for DmxA were collected using Pilatus 6M-F detector at the wavelengths of 0.972 Å on the beamline ID29, at the European Synchrotron Radiation Facility (ESRF) in Grenoble (France). Crystals of DpcA belonged to P21 space group with unit-cell parameters: a = 41.3, b = 79.4, c = 43.5 A °, α = β = 90.0, γ = 95.0 and contained 1 molecule in the asymmetric unit. Crystals of DmxA belonged to P212121 space group, with unit-cell parameters: a = 43.371, b = 78.343, c = 150.51; α = γ = β = 90.0 and contained 2 molecules in the asymmetric unit. The structures were solved by molecular replacement with MOLREP from the CCP4 software suite. The coordinates of Xanthobacter autotrophicus (PDB code: 1B6G; 40% sequence identities for 121 residues and 53% sequence similarity was used as search model for DpcA structure and for DmxA from Rhodococcus rhodochrous (PDB entry 4E46; 48% sequence identity for 142 residues and 63% sequence similarity). Belonging to the superfamily of α/β - hydrolases, according to the catalytic pentad, HLDs are subdivided onto the three subfamilies. DpcA belongs to the HLD - I: Asp- His - Asp + Trp - Trp and DmxA to the HLD – II: Asp - His - Glu + Asn - Trp. We thank M. Weiss and S. Pühringer (BESSY). This work is supported by the Grant Agency of the Czech Republic (P207/12/0775).Also by the Ministry of Education of the Czech Republic (CZ.1.05/2.1.00/01.0024 and CZ.1.05/2.1.00/01.0001). The support of the Academy of Sciences of the Czech Republic is acknowledged as well.
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TURSINA, A. I., A. V. GRIBANOV, N. G. BUKHAN’KO, P. ROGL et Y. D. SEROPEGIN. « Crystal structure of the novel compound Ce3Pt4Al6 ». Chemistry of Metals and Alloys 1, no 1 (2008) : 62–66. http://dx.doi.org/10.30970/cma1.0027.

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Day, Graeme. « Insight from energy surfaces : structure prediction by lattice energy exploration ». Acta Crystallographica Section A Foundations and Advances 70, a1 (5 août 2014) : C28. http://dx.doi.org/10.1107/s2053273314099719.

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A long-standing challenge for the application of computational chemistry in the field of crystallography is the prediction of crystal packing, given no more than the chemical bonding of the molecules being crystallised. Recent years have seen significant progress towards reliable crystal structure prediction methods, even for traditionally challenging systems involving flexible molecules and multi-component solids [1]. These methods are based on global searches of the lattice energy surface: a search is performed to locate all possible packing arrangements, and these structures are ranked by their calculated energy [2]. One aim of this lecture is to provide an overview of advances in methods for crystal structure prediction, focussing on molecular organic crystals, and highlighting strategies that are being explored to extend the reach of these methods to more complex systems. A second aim is to discuss the range applications of crystal structure prediction calculations, which have traditionally included solid form screening, particularly of pharmaceutically active molecules, and structure determination. As energy models become more reliable at correctly ranking the stability order of putative structures, and the timescale required for structure searching decreases, crystal structure prediction has the potential for the discovery of novel molecular materials with targeted properties. Prospects for computer-guided discovery of materials will be discussed.
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19

Filatov, Stanislav K., Yaroslav P. Biryukov, Rimma S. Bubnova et Andrey P. Shablinskii. « The novel borate Lu5Ba6B9O27 with a new structure type : synthesis, disordered crystal structure and negative linear thermal expansion ». Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials 75, no 4 (20 juillet 2019) : 697–703. http://dx.doi.org/10.1107/s2052520619007443.

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Single crystals of Lu5Ba6B9O27 were obtained by cooling from a melt and polycrystals of the borate were prepared using a multi-step solid-state synthesis. The crystal structure was determined from single-crystal X-ray diffraction data. The borate crystallizes in a new structure type in the monoclinic crystal system in space group C2/c, with cell parameters a = 13.0927 (3), b = 9.9970 (2) and c = 20.4884 (4) Å, β = 106.827 (1)°, V = 2566.86 (9) Å3 and Z = 4. It is described as a framework composed of rings consisting of vertex-sharing [BO3] triangles and [LuO6] octahedra. The Ba atoms are in the cavities of the framework. The structure is disordered: one of the B atoms is surrounded by six O atoms with partial occupancies of 0.5. The thermal properties of Lu5Ba6B9O27 were investigated by thermal analysis and high-temperature X-ray powder diffraction. Its thermal expansion is highly anisotropic. The negative expansion (contraction) is along the b axis, i.e. parallel to the planes of the largest number of [BO3] triangles. The coefficient of negative linear expansion ranges from −1.42 (at 20°C) to −5.57 × 10–6 °C–1 (at 1000°C). Thermal deformation of the ac plane is described in terms of the theory of shear deformation of monoclinic crystals. The Lu5Ba6B9O27 sample melts at 1170°C.
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Kleppa, Kurt O., Norbert A. Harringer et Hubert Preßlinger. « Ca10V5.2Fe0.8O24, a Novel Oxometalate with Discrete Complex Anions ». Zeitschrift für Naturforschung B 58, no 11 (1 novembre 2003) : 1112–16. http://dx.doi.org/10.1515/znb-2003-1113.

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Abstract Lustrous needle shaped prismatic single crystals of the new compound Ca10V5.2Fe0.8O24 were obtained out of a sample with nominal composition Ca2Fe1.6V0.4O5 prepared at 1400 °C. The crystals are opaque and stable to humid air. Ca10V5.2Fe0.8O24 crystallizes with a new structure type, space group Pnma with a = 6.803(3), b = 16.015(8), c = 10.418(7)Å , Z = 2, R = 0.041. The crystal structure is characterized by two mononuclear tetrahedral species, MO4, which differ significantly from each other with respect to their M-O bond lengths. One with an average bond distance of 1.709(8)Å represents an orthovanadate ion. The other with a significantly larger value d(M-O) = 1.744(6) Å corresponds to a mixed occupation of its centre according to [V0.8Fe0.2O4]3.5−. In the crystal structure the complex anions are arranged in separate sheets parallel to the (010) plane. They are separated from each other by three crystallographically independent Ca2+ ions which are each coordinated by 7 oxygen atoms in distorted pentagonal bipyramidal and trigonal prismatic configurations, respectively.
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Averkiev, Boris B., Iryna Davydenko, Xu Wang, Stephen Barlow et Seth R. Marder. « Crystal structure of 5,6-bis(9H-carbazol-9-yl)benzo[c][1,2,5]thiadiazole : distortion from a hypothetical higher-symmetry structure ». Acta Crystallographica Section C Structural Chemistry 73, no 4 (7 mars 2017) : 319–24. http://dx.doi.org/10.1107/s2053229617003035.

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Nucleophilic substitution of F atoms in 5,6-difluorobenzo[c][1,2,5]thiadiazole (DFBT) for carbazole could be potentially interesting as a novel way of synthesizing building blocks for new conjugated materials for applications in organic chemistry. The crystal structures of 5,6-bis(9H-carbazol-9-yl)benzo[c][1,2,5]thiadiazole (DCBT), C30H18N4S, and its hydrate, C30H18N4S·0.125H2O, were investigated using single-crystal X-ray analysis. The hydrate contains two symmetry-independent DCBT molecules. The dihedral angles between the plane of the central benzothiadiazole fragment and that of the carbazole units vary between 50.8 and 69.9°, indicating conformational flexibility of the DCBT molecule in the crystals, which is consistent with quantum chemical calculations. The analysis of the crystal packing of DCBT revealed that the experimental triclinic structure could be described as a distortion from a hypothetical higher-symmetry monoclinic structure. The quantum chemical calculations of two possible monoclinic structures, which are related to the experimental structure by a shifting of molecular layers, showed that the proposed structures are higher in energy by 5.4 and 10.1 kcal mol−1. This energy increase is caused by less dense crystal packings of the symmetric structures, which results in a decrease of the number of intermolecular interactions.
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Porada, Jan H., Jörg-M. Neudörfl et Dirk Blunk. « Planar and distorted indigo as the core motif in novel chromophoric liquid crystals ». New Journal of Chemistry 39, no 11 (2015) : 8291–301. http://dx.doi.org/10.1039/c5nj01594d.

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Shevelkov, A. V., E. V. Dikarev et B. A. Popovkin. « A Novel Metallic Halide, Hg2As3Br : Synthesis and Crystal Structure, and Crystal Structure of Cd2As3Br ». Journal of Solid State Chemistry 113, no 1 (novembre 1994) : 116–19. http://dx.doi.org/10.1006/jssc.1994.1348.

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KIRUBAVATHI, K., K. SELVARAJU et S. KUMARARAMAN. « STUDIES ON GROWTH AND CHARACTERIZATION OF BIS THIOUREA LEAD CHLORIDE : A NOVEL NONLINEAR OPTICAL CRYSTAL ». Journal of Nonlinear Optical Physics & ; Materials 18, no 01 (mars 2009) : 153–59. http://dx.doi.org/10.1142/s0218863509004531.

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Single crystals of the metal-organic nonlinear optical material bis thiourea lead chloride were grown from solution growth technique for the first time. The grown crystals were characterized by single crystal X-ray diffraction analysis to confirm the crystal structure. The presence of various functional groups and the coordination of metal ions to thiourea were confirmed by Fourier transform infrared analysis. UV-Vis. spectrum was recorded to study the optical transparency of the grown crystals. The second order nonlinear optical property of the grown crystal was examined by Kurtz powder technique and mechanical behavior was studied by Vickers micro hardness test.
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Tamboli, Majid Ismail, Yohei Utusmi, Takayuki Furuishi, Kaori Fukuzawa et Etsuo Yonemochi. « Crystal Structure of Novel Terephthalate Salt of Antiarrhythmic Drug Disopyramide ». Crystals 11, no 4 (31 mars 2021) : 368. http://dx.doi.org/10.3390/cryst11040368.

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1:1 salt of Disopyramide (DPA) with Terephthalic acid (TA) was obtained by the slow solvent evaporation and the slurry crystallization methods. X-ray single crystal diffraction of DPA:TA confirmed the formation of salt by the transfer of an acidic proton from one of the carboxylic acidic groups of TA to the tertiary amino group of the chain moiety (N3-nitrogen atom) of the DPA molecules. DPA:TA salt crystals crystalize in the triclinic system with space group P-1. The asymmetric unit, comprising one protonated DPA and one TA anion, are linked by a strong charge assisted N+–H∙∙∙O¯ hydrogen bond and a C–H∙∙∙O¯ hydrogen bond. Moreover, structural characterization of DPA:TA salt was carried out using Fourier transform infrared spectroscopy, differential scanning calorimeter, thermogravimetric analysis, and powder X-ray diffraction techniques
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Kimura, Fumiko, Wataru Oshima, Hiroko Matsumoto, Hidehiro Uekusa, Kazuaki Aburaya, Masataka Maeyama et Tsunehisa Kimura. « Magnetically Oriented Powder Crystal to Indexing and Structure Determination ». Acta Crystallographica Section A Foundations and Advances 70, a1 (5 août 2014) : C1560. http://dx.doi.org/10.1107/s2053273314084393.

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In pharmaceutical sciences, the crystal structure is of primary importance because it influences drug efficacy. Due to difficulties of growing a large single crystal suitable for the single crystal X-ray diffraction analysis, powder diffraction method is widely used. In powder method, two-dimensional diffraction information is projected onto one dimension, which impairs the accuracy of the resulting crystal structure. To overcome this problem, we recently proposed a novel method of fabricating a magnetically oriented microcrystal array (MOMA), a composite in which microcrystals are aligned three-dimensionally in a polymer matrix. The X-ray diffraction of the MOMA is equivalent to that of the corresponding large single crystal, enabling the determination of the crystal lattice parameters and crystal structure of the embedded microcrytals.[1-3] Because we make use of the diamagnetic anisotropy of crystal, those crystals that exhibit small magnetic anisotropy do not take sufficient three-dimensional alignment. However, even for these crystals that only align uniaxially, the determination of the crystal lattice parameters can be easily made compared with the determination by powder diffraction pattern. Once these parameters are determined, crystal structure can be determined by X-ray powder diffraction method. In this paper, we demonstrate possibility of the MOMA method to assist the structure analysis through X-ray powder and single crystal diffraction methods. We applied the MOMA method to various microcrystalline powders including L-alanine, 1,3,5-triphenyl benzene, and cellobiose. The obtained MOMAs exhibited well-resolved diffraction spots, and we succeeded in determination of the crystal lattice parameters and crystal structure analysis.
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Li, Xianbo, et Qin Zhang. « Effect of Molecular Structure of Organic Acids on the Crystal Habit of α-CaSO4·0.5H2O from Phosphogypsum ». Crystals 10, no 1 (6 janvier 2020) : 24. http://dx.doi.org/10.3390/cryst10010024.

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The organic acid crystal modifiers play an important role in the control of the crystal habit of α-hemihydrate gypsum (α-CaSO4·0.5H2O) from phosphogypsum, but the molecular structure characteristics of crystal modifiers have not been clarified, which makes it difficult to judge whether an organic acid has the ability to regulate the crystal habit of α-CaSO4·0.5H2O directly. In this work, the effect of organic acids with different molecular structures on the crystal habit of α-CaSO4·0.5H2O and its adsorption differences onto the α-CaSO4·0.5H2O surface were explored. The results show that the molecular structure characteristics of crystal modifiers contain two or more carboxylic groups (COOH) that are separated by two methylene or methine groups. Furthermore, organic acids with the regulation ability can adsorb on the surface of α-CaSO4·0.5H2O and change its growth habit. With the increase in the crystal modifier concentration, the α-CaSO4·0.5H2O crystals are shortened in length and enlarged in width, resulting in the decrease in aspect ratio and the increase in compressive strength. Conversely, when the adsorption of ineffective organic acids on the surface of α-CaSO4·0.5H2O was not detected, the α-CaSO4·0.5H2O crystals remained long hexagonal prisms. These results have guiding significance for the screening of novel organic acid crystal modifiers.
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Li, Fangzhi, Chunfeng Hu, Jiemin Wang, Bin Liu, Jingyang Wang et Yanchun Zhou. « Crystal Structure and Electronic Structure of a Novel Hf3AlN Ceramic ». Journal of the American Ceramic Society 92, no 2 (février 2009) : 476–80. http://dx.doi.org/10.1111/j.1551-2916.2008.02880.x.

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Valle, Mario, et Artem R. Oganov. « Crystal fingerprint space – a novel paradigm for studying crystal-structure sets ». Acta Crystallographica Section A Foundations of Crystallography 66, no 5 (12 août 2010) : 507–17. http://dx.doi.org/10.1107/s0108767310026395.

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Anandha babu, G., P. Ramasamy, K. Ravikumar et B. Sridhar. « Crystal structure and characterization of a novel organic crystal : 4-Dimethylaminobenzophenone ». Materials Research Bulletin 44, no 6 (juin 2009) : 1265–69. http://dx.doi.org/10.1016/j.materresbull.2009.01.007.

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Wojtaś, M., A. Ga¸gor, O. Czupiński, W. Medycki et R. Jakubas. « Crystal structure and characterization of the novel hydrogen bonded polar crystal ». Journal of Solid State Chemistry 187 (mars 2012) : 35–44. http://dx.doi.org/10.1016/j.jssc.2011.12.020.

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Reiss, Céleste A., Jan B. van Mechelen, Kees Goubitz et René Peschar. « Reassessment of paracetamol orthorhombic Form III and determination of a novel low-temperature monoclinic Form III-m from powder diffraction data ». Acta Crystallographica Section C Structural Chemistry 74, no 3 (28 février 2018) : 392–99. http://dx.doi.org/10.1107/s2053229618002619.

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Paracetamol [N-(4-hydroxyphenyl)acetamide, C8H9NO2] has several polymorphs, just like many other drugs. The most stable polymorphs, denoted Forms I and II, can be obtained easily and their crystal structures are known. Crystals of the orthorhombic, less stable, room-temperature Form III are difficult to grow; they need a special recipe to crystallize and suffer from severe preferred orientation. A crystal structure model of Form III has been proposed and solved from a combination of structure prediction and powder X-ray diffraction (PXRD) [Perrinet al.(2009).Chem. Commun.22, 3181–3183]. The finalRwpvalue of 0.138 and the corresponding considerable residual trace were reasons to check its validity. A new structure determination of Form III using new high-resolution PXRD data led to a finalRwpvalue of 0.042 and an improvement of the earlier proposed model. In addition, a reversible phase transition was found at 170–220 K between the orthorhombic Form III and a novel monoclinic Form III-m. The crystal structure of Form III-m has been determined and refined from PXRD data to a finalRwpvalue of 0.059.
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Inam, Muhammad, Jiajia Wu, Jie Shen, Chi Phan, Guping Tang et Xiurong Hu. « Preparation and Characterization of Novel Pharmaceutical Co-Crystals : Ticagrelor with Nicotinamide ». Crystals 8, no 9 (21 août 2018) : 336. http://dx.doi.org/10.3390/cryst8090336.

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Two new co-crystals, Ticagrelor with Nicotinamide, have been prepared with improved solubility. Because Ticalegor has a poor solubility and dissolution rate, a novel co-crystallization method with structurally homogenous crystalline material, an active pharmaceutical ingredient (API), and co-former indefinite stoichiometric amount has been made to improve Ticagrelor’s solubility. The co-crystal of Ticagrelor (TICA) with Nicotinamide (NCA) was prepared in ratio (1:1) and confirmed by FTIR, DSC, and XRD characterization. Furthermore, the single crystal structure of TICA-NCA hydrate was analyzed. The solubility of co-crystals was investigated in pH 2 acidic medium, which was a significant improvement as compared to the solubility of a free drug. The in vitro dissolution rate of co-crystal was larger than that of the commercial product.
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Liu, Ying, et Haixing Liu. « Study on novel structure of Mn complex, C24H18CrMnN4O5 ». E3S Web of Conferences 252 (2021) : 02071. http://dx.doi.org/10.1051/e3sconf/202125202071.

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The novel Mn complex C24H18CrMnN4O5 was investigated by hydrothermal and its crystal structure was characterized using X-ray diffraction technology. The Mn atom is six coordinated by four N atom from two 1, 10-phenanthroline and two O atoms from CrO4-. The hydrogen bonding O-H...O had central effect for crystal stability.
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Zhang, Tianyao, Zhaohui Zhang et Mark A. Arnold. « Crystal Structure-Free Method for Dielectric and Polarizability Characterization of Crystalline Materials at Terahertz Frequencies ». Applied Spectroscopy 75, no 6 (8 mars 2021) : 647–53. http://dx.doi.org/10.1177/0003702821991594.

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Terahertz (THz) time-domain spectroscopy provides a direct and nondestructive method for measuring the dielectric properties of materials directly from the phase delay of coherent electromagnetic radiation propagating through the sample. In cases when crystals are embedded within an inert polymeric pellet, the Landau, Lifshitz, and Looyenga (LLL) effective medium model can be used to extract the intrinsic dielectric constant of the crystalline sample. Subsequently, polarizability can be obtained from the Clausius–Mossotti (CM) relationship. Knowledge of the crystal structure density is required for an analytical solution to the LLL and CM relationships. A novel crystal structure-free graphical method is presented as a way to estimate both dielectric constants and polarizability values for the situation when the crystal structure density is unknown, and the crystals are embedded within a pellet composed of a non-porous polymer. The utility of this crystal structure-free method is demonstrated by analyzing THz time-domain spectra collected for a set of amino acids (L-alanine, L-threonine, and L-glutamine) embedded within pellets composed of polytetrafluoroethylene. Crystal structures are known for each amino acid, thereby enabling a direct comparison of results using the analytical solution and the proposed crystal structure-free graphical method. For each amino acid, the intrinsic dielectric constant is extracted through the LLL effective medium model without using information of their crystal structure densities. THz polarizabilities are then calculated with the CM relationship by using the determined intrinsic dielectric constant for each amino acid coupled with its crystal density as determined graphically. Comparison between the analytical and graphical solutions reveal relative differences between dielectric constants of 3.7, 5.1, and 13.6% for threonine, alanine, and glutamine, respectively, and relative differences between polarizability of 0.6, 0.9, and 5.4%, respectively. These values were determined over the 10–20 cm−1 THz frequency range. The proposed method requires no prior knowledge of crystal structure information.
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Shruthi, C., V. Ravindrachary, K. Byrappa, B. Guruswamy, Janet Goveas, Karthik Kumara et N. K. Lokanath. « Synthesis, Optical and Thermal Properties of 1-(4-Methoxyphenyl)-2-((5-(1-(Naphthalene-1-Yloxy)Ethyl)-[1,3,4]-Oxadiazol-2-Yl)Sulfanyl)Ethanoe - A Novel Heterocyclic Compound ». Materials Science Forum 962 (juillet 2019) : 10–16. http://dx.doi.org/10.4028/www.scientific.net/msf.962.10.

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A novel heterocyclic compound, 1-(4-methoxy phenyl)-2-((5-(1-(naphthalen-1-yloxy) ethyl) -[1,3,4]-oxadiazol-2-yl) sulfanyl) ethanone was synthesized using standard method and chemical structure of the synthesized compound was identified using FTIR spectrum. Needle shaped single crystals have been grown using solution growth technique. The grown crystals were characterized using single crystal XRD, UV-visible and Thermal analysis. The crystal structure study shows that the compound crystallizes in Monoclinic crystal system with a space group of P21/a and cell parameters are determined. UV-Visible study shows that the crystal is transparent in the entire visible region. The thermal stability of the material was determined by TG and DTA analysis.
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37

Bezzu, C. Grazia, Madeleine Helliwell, Benson M. Kariuki et Neil B. McKeown. « Synthesis and crystal structure of a novel phthalocyanine-calixarene conjugate ». Journal of Porphyrins and Phthalocyanines 15, no 07n08 (juillet 2011) : 686–90. http://dx.doi.org/10.1142/s1088424611003628.

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We report the synthesis and crystal structure of a novel phthalocyanine-calixarene conjugate (Pc-Calix) derived from a calixarene-based phthalonitrile (Pn-Calix). Crystal structures confirm the retention of the full cone configuration of the calixarene unit, which is thus suitable for the binding of appropriate chemical species. This new conjugate may find application as a molecular sensor in which the calixarene acts as the binding site and the perturbations of the optical properties of the phthalocyanine reports the presence of the binding species.
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38

Schreyer, Martin, Liangfeng Guo, Satyanarayana Thirunahari, Feng Gao et Marc Garland. « Simultaneous determination of several crystal structures from powder mixtures : the combination of powder X-ray diffraction, band-target entropy minimization and Rietveld methods ». Journal of Applied Crystallography 47, no 2 (19 mars 2014) : 659–67. http://dx.doi.org/10.1107/s1600576714003379.

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Crystal structure determination is the key to a detailed understanding of crystalline materials and their properties. This requires either single crystals or high-quality single-phase powder X-ray diffraction data. The present contribution demonstrates a novel method to reconstruct single-phase powder diffraction data from diffraction patterns of mixtures of several components and subsequently to determine the individual crystal structures. The new method does not require recourse to any database of known materials but relies purely on numerical separation of the mixture data into individual component diffractograms. The resulting diffractograms can subsequently be treated like single-phase powder diffraction data,i.e.indexing, structure solution and Rietveld refinement. This development opens up a host of new opportunities in materials science and related areas. For example, crystal structures can now be determined at much earlier stages when only impure samples or polymorphic mixtures are available.
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Ruseikina, Anna V., Maxim V. Grigoriev, Leonid A. Solovyov, Vladimir A. Chernyshev, Aleksandr S. Aleksandrovsky, Alexander S. Krylov, Svetlana N. Krylova et al. « A Challenge toward Novel Quaternary Sulfides SrLnCuS3 (Ln = La, Nd, Tm) : Unraveling Synthetic Pathways, Structures and Properties ». International Journal of Molecular Sciences 23, no 20 (18 octobre 2022) : 12438. http://dx.doi.org/10.3390/ijms232012438.

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We report on the novel heterometallic quaternary sulfides SrLnCuS3 (Ln = La, Nd, Tm), obtained as both single crystals and powdered samples. The structures of both the single crystal and powdered samples of SrLaCuS3 and SrNdCuS3 belong to the orthorhombic space group Pnma but are of different structural types, while both samples of SrTmCuS3 crystallize in the orthorhombic space group Cmcm with the structural type KZrCuS3. Three-dimensional crystal structures of SrLaCuS3 and SrNdCuS3 are formed from the (Sr/Ln)S7 capped trigonal prisms and CuS4 tetrahedra. In SrLaCuS3, alternating 2D layers are stacked, while the main backbone of the structure of SrNdCuS3 is a polymeric 3D framework [(Sr/Ln)S7]n, strengthened by 1D polymeric chains (CuS4)n with 1D channels, filled by the other Sr2+/Ln3+ cations, which, in turn, form 1D dimeric ribbons. A 3D crystal structure of SrTmCuS3 is constructed from the SrS6 trigonal prisms, TmS6 octahedra and CuS4 tetrahedra. The latter two polyhedra are packed together into 2D layers, which are separated by 1D chains (SrS6)n and 1D free channels. In both crystal structures of SrLaCuS3 obtained in this work, the crystallographic positions of strontium and lanthanum were partially mixed, while only in the structure of SrNdCuS3, solved from the powder X-ray diffraction data, were the crystallographic positions of strontium and neodymium partially mixed. Band gaps of SrLnCuS3 (Ln = La, Nd, Tm) were found to be 1.86, 1.94 and 2.57 eV, respectively. Both SrNdCuS3 and SrTmCuS3 were found to be paramagnetic at 20–300 K, with the experimental magnetic characteristics being in good agreement with the corresponding calculated parameters.
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40

Fuller, DJ, DL Kepert, BW Skelton et AH White. « Structure, Stereochemistry and Novel 'Hydrogen Bonding' in Two Bipyridinium Salts of the B10H102- Anion ». Australian Journal of Chemistry 40, no 12 (1987) : 2097. http://dx.doi.org/10.1071/ch9872097.

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Crystal structure determinations of (LH)2(B10H10), (1), and (LH2)(B10H10), (2), L = 2,2'- bipyridine , have been carried out by single-crystal X-ray diffraction methods at 295 K, being refined by full-matrix least squares to residuals of 0.041, 0.047 for 1758, 1771 'observed' independent reflections respectively. Crystals of (1) are monoclinic, P21/n, a 12.040(7), b 17.71(1), c 11.142(4) �, β 101.78(4)�, Z 4. Crystals of (2) are monoclinic, P21/c, a 9.937(4), b 10.837(3), c 14.856(5) �, β 109 2l(3)�, Z 4. The colour of the compounds is accounted for by charge-transfer interactions of a novel type, namely between the positively charged cationic acid hydrogen atoms and the negatively charged non-apical hydrogen atoms of the anion. In yellow (1), these distances are 2.26(5) �, while in red (2), they are much shorter, being 1.89(4), 1.97(3) �.
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41

Hou, Xiaomeng, Linfei Xu, Xuesong Tang, Yang Song et Yinjuan Bai. « Synthesis and Crystal Structure of Novel Benzimidazole Cyclophanes ». Chinese Journal of Organic Chemistry 33, no 3 (2013) : 643. http://dx.doi.org/10.6023/cjoc201209043.

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42

Shcherbakova, Ye V., G. V. Ivanova, V. S. Gaviko et A. M. Gabay. « Crystal structure of novel ferromagnetic LaFe13−xGaxC compounds ». Journal of Magnetism and Magnetic Materials 267, no 1 (novembre 2003) : 26–34. http://dx.doi.org/10.1016/s0304-8853(03)00300-7.

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43

Kim, Sungho, Roger Bishop, Donald C. Craig, Ian G. Dance et Marcia L. Scudder. « Formation and crystal structure of a novel azabishomotwistane ». Journal of Organic Chemistry 55, no 1 (janvier 1990) : 355–58. http://dx.doi.org/10.1021/jo00288a064.

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Lisnyak, V. V., N. V. Stus, N. S. Slobodyanik, N. M. Belyavina et V. Ya Markiv. « Crystal structure of a novel cubic pyrophosphate WP2O7 ». Journal of Alloys and Compounds 309, no 1-2 (septembre 2000) : 83–87. http://dx.doi.org/10.1016/s0925-8388(00)00922-1.

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45

Stępień-Damm, J., Z. Bukowski, V. I. Zaremba, A. P. Pikul et D. Kaczorowski. « Crystal structure of a novel cerium indide Ce6Pt11In14 ». Journal of Alloys and Compounds 379, no 1-2 (octobre 2004) : 204–8. http://dx.doi.org/10.1016/j.jallcom.2004.03.070.

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Zou Jun, Huang Tao-Hua, Wang Jun, Zhang Lian-Han, Zhou Sheng-Ming et Xu Jun. « The structure analysis of novel Ti : LiAlO2 crystal ». Acta Physica Sinica 55, no 7 (2006) : 3536. http://dx.doi.org/10.7498/aps.55.3536.

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Schnering, H. G. von, R. Kröner, W. Carrillo-Cabrera, K. Peters et R. Nesper. « Crystal structure of the novel chiral clathrate, Ba6In4Ge21 ». Zeitschrift für Kristallographie - New Crystal Structures 213, no 1-4 (avril 1998) : 705–6. http://dx.doi.org/10.1524/ncrs.1998.213.14.705.

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Morozova, Yu, A. Gribanov, E. Murashova, S. Dunaev, A. Grytsiv, P. Rogl, G. Giester et D. Kaczorowski. « Novel ternary compound Ce4Pt9Al13 : Crystal structure, physical properties ». Journal of Alloys and Compounds 767 (octobre 2018) : 496–503. http://dx.doi.org/10.1016/j.jallcom.2018.07.146.

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Grytsiv, A., P. Rogl, E. Bauer, H. Michor, E. Royanian et G. Giester. « Novel silicide BaPt5Si12 : Crystal structure and physical properties ». Intermetallics 18, no 1 (janvier 2010) : 173–78. http://dx.doi.org/10.1016/j.intermet.2009.07.009.

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Fedorchuk, A. O., G. Lakshminarayana, Y. O. Tokaychuk et O. V. Parasyuk. « The crystal structure of novel silver sulphogermanate Ag10Ge3S11 ». Journal of Alloys and Compounds 576 (novembre 2013) : 134–39. http://dx.doi.org/10.1016/j.jallcom.2013.04.110.

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