Disclosing the Rich Crystal Chemistry of Lesinurad by ab Initio Laboratory X-ray Powder Diffraction Methods

Terruzzi Stephanie; Bellomi Sonja; Marras Giovanni; Barreca Giuseppe; Ventimiglia Giampiero; Cervellino Antonio; Masciocchi Norberto

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Disclosing the Rich Crystal Chemistry of Lesinurad by ab Initio Laboratory X-ray Powder Diffraction Methods

机译：通过AB Initio实验室X射线粉末衍射方法揭示Lesinurad的丰富晶体化学

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Lesinurad, a uric acid reabsorption inhibitor that received Food and Drug Administration approval in 2015, is known to crystallize in three unsolvated crystal forms and in a few solvated phases. The structures of the former have been determined by state-of-the-art powder diffraction methods, highlighting significant conformational as well as supramolecular differences, resulting in hydrogen bonded centrosymmetric dimers (Form 1) or helical chains (Form 2). In the complex crystal packing in Form 3, additional one-dimensional (1D) ribbons held together by unexpected C=O center dot center dot center dot Br interactions of the halogen-bond type are found. Thermal analyses and variable-temperature powder diffraction measurements (including high temperature synchrotron X-ray diffraction experiments) provided evidence for the reversible formation of a new phase, Form 2hT, obtained upon heating above 100 degrees C powders of Form 2. Structure solution and refinement of the high-temperature phase made it possible to attribute the structural change to a 60 degrees rotation of the cyclopropyl residue, leaving unaffected the conformation of the (longer) polar branch and the supramolecular 1D helical chain arrangement found in the RT phase.

机译：Lesinurad是在2015年接受食品和药物管理批准的尿酸重吸收抑制剂，已知以三种未经许的晶体形式和少量溶剂化相结晶。前者的结构已经通过最先进的粉末衍射方法确定，突出显示显着的构象以及超分子差异，导致氢键键合的亚里索二聚体（形式1）或螺旋链（形式2）。在形式3中的复杂晶体包装中，发现通过意外的C = O中心点中心点中心点BRα相互作用的附加一维（1D）丝带。热分析和可变温度粉末衍射测量（包括高温同步旋转X射线衍射实验）提供了在2℃的21℃以上加热后获得的新阶段的可逆形成2HT的证据。结构溶液和细化在高温阶段使得结构变化将结构变化归因于环丙基残基的60℃，留下不受影响的（更长）极性分支的构象和在RT相中发现的超分子1D螺旋链装置。

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《Crystal growth & design》 |2018年第11期|共10页
作者
Terruzzi Stephanie; Bellomi Sonja; Marras Giovanni; Barreca Giuseppe; Ventimiglia Giampiero; Cervellino Antonio; Masciocchi Norberto;
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作者单位

Univ Insubria Dipartimento Sci &

Alta Tecnol Via Valleggio 11 I-22100 Como Italy;

Chemessentia Srl Via Bovio 6 I-28100 Novara Italy;

Chemessentia Srl Via Bovio 6 I-28100 Novara Italy;

Chemessentia Srl Via Bovio 6 I-28100 Novara Italy;

Chemessentia Srl Via Bovio 6 I-28100 Novara Italy;

Paul Scherrer Inst Swiss Light Source CH-5232 Villigen Switzerland;

Univ Insubria Dipartimento Sci &

Alta Tecnol Via Valleggio 11 I-22100 Como Italy;

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正文语种 eng
中图分类晶体学;
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1. Disclosing the Rich Crystal Chemistry of Lesinurad by ab Initio Laboratory X-ray Powder Diffraction Methods [J] . Terruzzi Stephanie, Bellomi Sonja, Marras Giovanni, Crystal growth & design . 2018,第11期

机译：通过AB Initio实验室X射线粉末衍射方法揭示Lesinurad的丰富晶体化学
2. Ab Initio Structure Determination Of The Low-temperature Phaseof Succinonitrile From Laboratory X-ray Powder Diffraction Data-coping With Potential Poor Powder Quality Using Dft Ab Initio Methods [J] . P. S. Whitfield, Y. Le Page, A. Abouimrane, Powder diffraction . 2008,第4期

机译：从实验室X射线粉末衍射数据复制（使用Dft从头算法得出潜在的粉末质量较差）确定琥珀腈低温相的从头算结构
3. POLYMORPHISM IN COORDINATION CHEMISTRY - SELECTIVE SYNTHESES AND AB INITIO X-RAY POWDER DIFFRACTION CHARACTERIZATION OF TWO NEW CRYSTALLINE PHASES OF SOLID [PD(DMPZ)(2)(HDMPZ)(2)](2) (HDMPZ=3,5-DIMETHYLPYRAZOLE) [J] . Masciocchi N., Lamonica G., Moret M., Inorganic Chemistry: A Research Journal that Includes Bioinorganic, Catalytic, Organometallic, Solid-State, and Synthetic Chemistry and Reaction Dynamics . 1997,第3期

机译：固体[PD（DMPZ）（2）（HDMPZ）（2）]（2）的两个新结晶相的配位化学选择性合成和从头算X射线粉末衍射表征（HDMPZ = 3,5-二甲基）
4. Ab Initio Structure Determination of Quasicrystals via Single Crystal X-Ray Diffraction [C] . Hiroyuki Takakura, Akiji Yamamoto, Marc de Boissieu, Materials Research Society . 2004

机译：AB Initio结构通过单晶X射线衍射测定拟rγrate
5. A novel method for the determination of single crystal elastic constants using powder X-ray diffraction. [D] . Hou, Weimin. 2002

机译：一种使用粉末X射线衍射测定单晶弹性常数的新方法。
6. Crystal structure of dicesium hydrogen citrate from laboratory single-crystal and powder X-ray diffraction data and DFT comparison [O] . Alagappa Rammohan, Amy A. Sarjeant, James A. Kaduk 2017

机译：实验室单晶和粉末X射线衍射数据与DFT比较的柠檬酸氢二铯的晶体结构
7. Ab initio structure determination of the low-temperature phase of succinonitrile from laboratory X-ray powder diffraction data - coping with potential poor powder quality using DFT ab initio methods [O] . Whitfield, Pamela, Le Page, Yvon, Abouimrane, A., 2008

机译：从实验室X射线粉末衍射数据确定琥珀腈低温相的从头算结构-使用DFT从头算方法应对潜在的不良粉末质量
8. SUBSTRUCTURE CHARACTERISTICS OF FINE-GRAINED AND ALLOYS DISCLOSED BY X-RAY MICROSCOPY AND DIFFRACTION ANALYSIS Description and Application of Diffraction Method Description of X-Ray Double-Crystal Diffractometer Combining X-ray Microscopy and Diffraction [R] . Sigmund Weissmann, K. A. Turner 1958

机译：X射线显微镜衍射分析细晶粒和合金的子结构特征及衍射分析描述X射线双晶衍射仪结合X射线显微镜和衍射的描述和应用

Disclosing the Rich Crystal Chemistry of Lesinurad by ab Initio Laboratory X-ray Powder Diffraction Methods

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