Journal of Chemical Crystallography最新文献

{"title":"Hydrolysis of 2,4,6-tris(2-pyrimidyl)-1,3,5-triazine with Pd(II) and Pt(II) Complexes","authors":"Leonardo E. Cruz-Estrada,&nbsp;Simón Hernández-Ortega,&nbsp;Jesús Valdés-Martínez","doi":"10.1007/s10870-022-00948-y","DOIUrl":"10.1007/s10870-022-00948-y","url":null,"abstract":"<div><p>In this paper, we report the crystal and molecular structure of two compounds obtained from the reactions between the ligand 2,4,6-tris(2-pyrimidyl)-1,3,5-triazine (TpymT) with Pd(II) and Pt(II) [M(Cl₂(CH₃CN)₂] complexes. The ligand hydrolyses into the anion N-[(pyrimidine)carbonyl]pyrimidine-2-carboxamidato (bpcam⁻), giving compounds with the formula [Pd(bpcam)Cl]·H₂O, <b>1</b>, and [Pt(bpcam)Cl]·DMSO, <b>2</b>. Compounds <b>1</b> and <b>2</b> crystallize in the monoclinic crystal system with C2/c and P2₁/n space groups. The compounds are square planar, with the bpcam⁻ acting as a tridentate-κ³N anionic ligand and the Cl⁻ anion in the fourth position. In both complexes, the molecules stack in columns presenting interactions between the aromatic rings, reinforced in <b>2</b> by Pt···Pt interactions. The complexes interact with the solvent molecules through H-bonds building a 3D structure. We analyzed the systems through geometric parameters and Hirshfeld surface studies. The energy frameworks indicate that the main interactions between molecules in the crystal are dispersion forces.</p><h3>Graphical Abstract</h3><p>The paper presents the X-ray structures of [M(bpcam)Cl]·where bdcam- is the anion N-[(pyrimidine)carbonyl]pyrimidine-2-carboxamidato and M = Pd(II) and Pt(II), as well as Hirshfeld Surface and Energy Framework studies.</p>\u0000 <figure><div><div><div><picture><source><img></source></picture></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 1","pages":"127 - 137"},"PeriodicalIF":0.8,"publicationDate":"2022-06-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4759885","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Synthesis and Crystal Studies of Novel 11,12-Dihydro-Taxoids Derived from 1-Deoxybaccatin VI","authors":"Ye-Sha Cui,&nbsp;Ping Tang,&nbsp;Yong-Mei Cui,&nbsp;Ling-Yun Yue,&nbsp;Hai-Xia Lin","doi":"10.1007/s10870-022-00947-z","DOIUrl":"10.1007/s10870-022-00947-z","url":null,"abstract":"<div><p>Two novel taxoids were synthesized from 1-deoxybacctin VI (<b>1</b>) and their crystal structures were determined by X-ray crystallographic techniques. The influence of the 11,12-olefin of the tetracyclic moiety on molecular conformations were investigated. Comparison to other baccatin analogs, a larger effect on the conformation of the diterpenoid core is observed when the 11,12-olefin is reducted. Conformational analysis show that the reduction of the 11,12-olefin has a decisive influence on the conformation of the A and B ring. Compounds <b>3</b> and <b>5</b> crystallize in orthorhombic system, space group <i>P2</i>_<i>1</i><i>2</i>_<i>1</i><i>2</i>_<i>1</i>. In the structure of compound <b>3</b>, the six-membered A ring exhibits the 1,3-diplanar boat conformation, the eight-membered B ring adopts a boat–chair conformation, and the six-membered C ring exhibits a slightly distorted half-chair conformation. However, in 11,12-dihydro-taxoids <b>5</b>, the six-membered A ring exhibits a chair conformation and the conformation of the eightmembered B ring has a large distortion.</p><h3>Graphical Abstract</h3><p>The synthesis of novel 11,12-dihydro-taxoids from 1-deoxybacctin VI are presented, in which the crystal structure of the compound <b>5</b> was characterized.</p>\u0000 <figure><div><div><div><picture><source><img></source></picture></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 1","pages":"117 - 126"},"PeriodicalIF":0.8,"publicationDate":"2022-06-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-022-00947-z.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4465021","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A Diamidocarbene-Supported Aminoborylene: Characterization and Discussion of the Elusive Crystal Structure","authors":"Anthony D. Ledet,&nbsp;Eric W. Reinheimer,&nbsp; Todd W. Hudnall","doi":"10.1007/s10870-022-00950-4","DOIUrl":"10.1007/s10870-022-00950-4","url":null,"abstract":"<div><p>Five years after we published the synthesis of the first diamidocarbene (DAC)-supported amino borylene <b>4</b>, we now report the elusive single crystal X-ray structure. The X-ray structure of <b>4</b> was found to corroborate our previous computational studies which indicated that the borylene adopted a heterocumulenic geometry with a near linear C_(carbene) = B = N unit (175.88(18)^◦) as well as short C = B and B = N distances of 1.416(3) and 1.344(3) Å, respectively. Additionally, we further provide a qualitative and quantitative discourse on said structure with respect to the precursor compounds used to prepare <b>4</b> as well as to the known cyclic (alkyl) amino carbene (CAAC) analog <b>2.</b></p></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 1","pages":"112 - 116"},"PeriodicalIF":0.8,"publicationDate":"2022-06-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4348682","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"2D Honeycomb Coordination Polymers from 2,2′-Dithiobis(pyridine N-oxide) and Bismuth(III) Halides","authors":"Rüdiger W. Seidel,&nbsp;Iris M. Oppel","doi":"10.1007/s10870-022-00949-x","DOIUrl":"10.1007/s10870-022-00949-x","url":null,"abstract":"<div><p>Two bismuth(III) coordination polymers, namely [Bi₂<i>X</i>₆(<i>µ</i>-dtpo)₃]_n [<i>X</i> = Cl (<b>1)</b>, Br (<b>2</b>); dtpo = 2,2′-dithiobis(pyridine <i>N</i>-oxide)], were prepared using a crystal engineering strategy and structurally characterized by X-ray crystallography. In the isostructural compounds <b>1</b> and <b>2</b> (trigonal system, space group <i>P</i>-3<i>c</i>1), <i>fac</i>-configured Bi<i>X</i>₃ units as nodes are joined by the <i>C</i>₂-symmetrical dtpo bridging ligand as spacers to generate 2D honeycomb layers with (6,3) topology. The 2D sheets stack along the [001] direction, resulting in virtually hexagonal channels parallel to this direction, which are occupied by disordered methanol and water molecules. The potential solvent area per unit cell volume is 42.2% for <b>1</b> and 44.0% for <b>2</b>.</p><h3>Graphical Abstract</h3><p>Two isostructural 2D honeycomb bismuth(III) coordination, synthesized from 2,2′-dithiobis(pyridine <i>N</i>-oxide) and bismuth(III) halides are described.</p>\u0000 <figure><div><div><div><picture><source><img></source></picture></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 1","pages":"105 - 111"},"PeriodicalIF":0.8,"publicationDate":"2022-06-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-022-00949-x.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4261776","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Case of Charge-Assisted Hydrogen Bonding in the Crystal Structure of Sodium Laurate, Lauric Acid","authors":"Ibrahima Goudiaby,&nbsp;Benoît Guillot,&nbsp;Emmanuel Wenger,&nbsp;Sarra Soudani,&nbsp;Cherif ben Nasr,&nbsp;Magatte Camara,&nbsp;Abdoulaye Gassama,&nbsp;Christian Jelsch","doi":"10.1007/s10870-022-00946-0","DOIUrl":"10.1007/s10870-022-00946-0","url":null,"abstract":"<div><p>Crystals of Sodium Laurate, Lauric Acid (NaLLA) were obtained and the structure was determined by single-crystal X-ray diffraction. The new crystal form is monoclinic of space group P2₁/c. The asymmetric unit contains two independent laurate molecules whose carboxylic/carboxylate groups are linked by a low barrier O-H…O hydrogen bond. Two lauric/laurate molecules are in a head-to-head configuration and the elongated hydrophobic chains are parallel to the long <i>b</i> axis. The carboxylic hydrogen atom was found to be disordered, bound on each of the two carboxylate groups in an unsymmetrical way. The non-symmetrical character of the hydrogen bond is related to the presence of two independent fatty acid molecules in the asymmetric unit and is in accordance with the different lengths of the four C-O bonds present in the molecular structure. The crystal structure was analyzed in terms of interactions on the Hirshfeld surface. The packing is stabilized by hydrogen bonds and O…Na ionic interactions in the hydrophilic layer and by C-H…H-C contacts in the hydrophobic layers which are the most enriched major contacts.</p></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 1","pages":"93 - 104"},"PeriodicalIF":0.8,"publicationDate":"2022-05-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4759508","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Synthesis, Crystal Structure, Hirshfeld Surface Analysis and Interaction Energy and Energy Framework Studies of Novel Hydrazone Derivative Containing Barbituric Acid Moiety","authors":"Sultan Kıncal,&nbsp;Cansu Topkaya,&nbsp;Tolga Göktürk,&nbsp;Tuncer Hökelek,&nbsp;Ramazan Güp","doi":"10.1007/s10870-022-00945-1","DOIUrl":"10.1007/s10870-022-00945-1","url":null,"abstract":"<div><p>New hydrazone derivate, (1Z,2E)-2-(2-(1-(1,3-dimethyl-2,4,6-trioxotetrahydropyrimidin-5(2H)-ylidene)ethyl)hydrazineylidene)-2-(p-tolyl)acetaldehyde oxime (H₂L) was synthesized by 5-acetyl-1,3-dimethyl-barbituric acid and p-methyl isonitrosophenylhydrazine. Its molecular and crystal structures were determined by single crystal X-ray analysis. It belongs to triclinic system <i>P</i>-1 space group with <i>a</i> = 7.1722 (3) Å, <i>b</i> = 10.5362 (4) Å, <i>c</i> = 11.7675 (5) Å, α = 98.844 (4)°, <i>β</i> = 98.882 (4)°, γ = 104.330 (4)°, <i>Z</i> = 2 and <i>V</i> = 833.95 (6) ų. In the molecular structure, the intramolecular N–H···O and N–H···N hydrogen bonds enclose S(6) ring motifs. In the crystal structure, the intermolecular C–H···O and O–H···O hydrogen bonds link the molecules into centrosymmetric dimers, enclosing R₂²(10) and R₄⁴(10) ring motifs, in which they may be effective in stabilization of the structure. The Hirshfeld surface analysis of crystal structure indicates that the most important contributions for crystal packing are from H…H (48.5%), H…O/O…H (23.7%) and H…C/C…H (9.7%) interactions. Hydrogen bonding and van der Waals interactions are the dominant interactions in crystal packing. Computational chemistry indicates that in the crystal, O–H···O and C–H···O hydrogen bond energies are 95.9 and 87.5 kJ mol⁻¹. The evaluation of the electrostatic, dispersion and total energy frameworks indicates that stabilization is dominated via the nearly equal strengths of the electrostatic and dispersion energy contributions.</p><h3>Graphical Abstract</h3>\u0000 <figure><div><div><div><picture><source><img></source></picture></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 1","pages":"81 - 92"},"PeriodicalIF":0.8,"publicationDate":"2022-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-022-00945-1.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4584858","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Synthesis and Crystal Structure of a New Hexavanadate Hybrid with Alkynyl Ligands","authors":"Xingyue Wang,&nbsp;Chunhui Ma,&nbsp;Chenqi Zhao,&nbsp;Yanchao Zhao,&nbsp;Taozhu Zhan,&nbsp;Lihong Chen,&nbsp;Zicheng Xiao,&nbsp;Pingfan Wu","doi":"10.1007/s10870-022-00943-3","DOIUrl":"10.1007/s10870-022-00943-3","url":null,"abstract":"<div><p>A new hexavanadate hybrid with alkynyl ligands (DIEA)₂[V₆O₁₃{(OCH₂)₃CNHCOC₆H₄C≡CH}₂] was synthesized and its molecular structure has been determined by single-crystal X-ray diffraction. The compound crystallize in the orthorhombic system, space group <i>Pccn</i> with the cell parameters <i>a</i> = 15.951(2) Å, <i>b</i> = 33.240 Å, <i>c</i> = 10.5960(14) Å, <i>α</i> = <i>β</i> = <i>γ</i> = 90°, <i>V</i> = 5618.2(13) Å ³. The electrostatic potential was also calculated to show the electron distribution in the polyoxoanion.</p><h3>Graphical Abstract</h3><p>\u0000A new hexavanadate hybrid with alkynyl ligands (DIEA)₂ [V₆O₁₃{(OCH₂)₃CNHCOC₆H₄C≡CH}₂] was synthesized by post-functionalization. Each of the structures looks like a flabellum and both ends are straight and rigid on account of the conjugated effect in the organic ligands.</p><figure><div><div><div><picture><source><img></source></picture></div></div></div></figure></div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 1","pages":"75 - 80"},"PeriodicalIF":0.8,"publicationDate":"2022-04-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"5102236","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Design and Synthesis of Pentadentate N3O2-Type Donor Schiff Bases and their Interactive Behavior with UO2(VI) Ion: An Instance of Strange Behavior of Pyridine in a Uranyl (UO22+) Complex","authors":"Renu Kumari,&nbsp; Jyoti,&nbsp;Jai Deo Singh,&nbsp;Ray J. Butcher,&nbsp;Christopher Richardson","doi":"10.1007/s10870-022-00944-2","DOIUrl":"10.1007/s10870-022-00944-2","url":null,"abstract":"<div><p>Mononuclear uranyl(VI) Schiff base complexes of formula [UO₂(L₁)]·py (<b>1·py</b>) {[UO₂(L²)]}₂·MeCN·H₂O (<b>2·MeCN·H</b>_<b>2</b><b>O</b>) have been prepared and characterized by both IR and ¹H NMR spectroscopy and X-ray crystallography. The complex species <b>1·py</b> crystallizes as orange needle-like crystals in the <i>orthorhombic</i> space group, <i>Pbca</i>, with 8 molecules per unit cell. Interestingly, the pyridine molecule does not participate in coordination to the metal center and was found as a solvent molecule embedded in the crystal structure with weaker interactions to the metal complex. The crystals of the complex species, <b>2·MeCN·H</b>_<b>2</b><b>O</b>, crystallized in a <i>monoclinic</i> form, space group, <i>P</i>2₁, with 2 molecules in the asymmetric unit. The two molecules [(UO₂)(L₂)(CH₃CN or H₂O)] in the asymmetric unit of <b>2·MeCN·H</b>_<b>2</b><b>O</b> exhibit a competitive (CH₃CN/H₂O) scenario without any direct coordination to the uranyl ion.</p><h3>Graphical Abstract</h3><p>Uranyl(VI) Schiff base complexes of general formula [UO₂(L₁)]·py (<b>1·py</b>) and {[UO₂(L²)]}₂·MeCN·H₂O (<b>2·MeCN·H</b>_<b>2</b><b>O</b>) have been prepared and characterized by spectroscopic analysis and X-ray crystallography.</p>\u0000 <figure><div><div><div><picture><source><img></source></picture></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 1","pages":"66 - 74"},"PeriodicalIF":0.8,"publicationDate":"2022-04-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"5032744","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Syntheses and Structures of Diphenyl-Tellurium Oxide Copper(II)/Manganese(III) Complexes [CuII(Ph2TeO)4]Cl2·14H2O and [MnIIICl(Ph2TeO)4]Cl2·4H2O","authors":"Qian-Ya Xu,&nbsp;Yu-Jie Cui,&nbsp;Feng Hu,&nbsp;Ai-Quan Jia,&nbsp;Qian-Feng Zhang","doi":"10.1007/s10870-022-00942-4","DOIUrl":"10.1007/s10870-022-00942-4","url":null,"abstract":"<div><p>Treatment of diphenyl tellurium oxide (Ph₂TeO) with CuCl₂·2H₂O in a 4:1 molar ratio afforded the copper(II) complex [Cu^II(Ph₂TeO)₄]Cl₂·14H₂O (<b>1</b>), in which the copper(II) center is four-coordinated by four oxygen atoms from four Ph₂TeO units. Reaction of MnCl₂·4H₂O, (^<i>n</i>Bu₄N)[MnO₄] and Ph₂TeO at a molar ratio of 4:1:16 gave the manganese(III) complex [Mn^IIICl(Ph₂TeO)₄]Cl₂·4H₂O (<b>2</b>), in which the manganese(III) center is five-coordinated by one chlorine atom and four oxygen atoms from four Ph₂TeO moieties. Complex <b>1</b> crystallizes in the triclinic space group <i>P</i>ī, with <i>a</i> = 8.9904(18), <i>b</i> = 13.068(3), <i>c</i> = 13.573(3) Å, <i>α</i> = 100.42(3)°, <i>β</i> = 109.17(3)°, <i>γ</i> = 99.56(3)°, and <i>Z</i> = 1. The unit cell of <b>2</b> has a monoclinic <i>P</i>2₁<i>/c</i> symmetry with the cell parameters <i>a</i> = 20.179(5), <i>b</i> = 13.917(3), <i>c</i> = 19.210(4) Å, <i>β</i>  =  94.840(7)°, and <i>Z</i> = 4.</p><h3>Graphical Abstract</h3><p>Two new transition metal complexes with diphenyl tellurium oxide as ligands have been synthesized and studied.</p>\u0000 <figure><div><div><div><picture><source><img></source></picture></div></div></div></figure>\u0000 </div>","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 1","pages":"1 - 7"},"PeriodicalIF":0.8,"publicationDate":"2022-04-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4919151","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Syntheses and Structures of [Fe(TPA)X2](ClO4) and [{Fe(TPA)Y}2O](ClO4)2 Where TPA = Tris-(2-pyridylmethyl)amine, X = N3, or Br, and Y = N3, Br, NCO, or NCS","authors":"Jia Xue,&nbsp;Yelda Hangun-Balkir,&nbsp;Matthew Mullaney,&nbsp;Shamila Nadir,&nbsp;Justin Cody Lewis,&nbsp;Christine Henry-Smith,&nbsp;Naleen B. Jayaratna,&nbsp;C. A. U. Kawshalya Kumarihami,&nbsp;Richard E. Norman","doi":"10.1007/s10870-022-00941-5","DOIUrl":"10.1007/s10870-022-00941-5","url":null,"abstract":"&lt;div&gt;&lt;p&gt;[Fe(TPA)(N&lt;sub&gt;3&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;](ClO&lt;sub&gt;4&lt;/sub&gt;) and [Fe(TPA)Br&lt;sub&gt;2&lt;/sub&gt;](ClO&lt;sub&gt;4&lt;/sub&gt;), where TPA is tris-(2-pyridylmethyl)amine, crystallize in the monoclinic space group P2&lt;sub&gt;1&lt;/sub&gt;/c with a = 8.7029(5) Å, b = 19.168(1) Å, c = 13.5728(7) Å, β = 101.472(3)°, and a = 8.944(3) Å, b = 16.578(6) Å, c = 15.108(6) Å, β = 103.18(2)°, respectively. The structures were determined at 150 K from 3397 reflections (1426 observed) with R = 0.063 (R&lt;sub&gt;w&lt;/sub&gt; = 0.097), and at 115 K from 5617 reflections (2261 observed) with R = 0.057 (R&lt;sub&gt;w&lt;/sub&gt; = 0.065), respectively. In both cases, the iron is pseudo-octahedral with the two halide/pseudohalide ions &lt;i&gt;cis&lt;/i&gt;. The Fe–X bond &lt;i&gt;trans&lt;/i&gt; to the tertiary amine is shorter. The structures of [{Fe(TPA)X}&lt;sub&gt;2&lt;/sub&gt;O](ClO&lt;sub&gt;4&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt; where X = N&lt;sub&gt;3&lt;/sub&gt;, Br, &lt;i&gt;N&lt;/i&gt;CO, and two polymorphic forms of &lt;i&gt;N&lt;/i&gt;CS, are also reported. The azide derivative [CH&lt;sub&gt;3&lt;/sub&gt;CN solvate, monoclinic P2&lt;sub&gt;1&lt;/sub&gt;/n, a = 11.8038(11) Å, b = 22.547(2) Å, c = 17.344(2) Å, β = 106.972(4)°, determined at 100 K from 8972 reflections (4404 observed) with R = 0.087 (R&lt;sub&gt;w&lt;/sub&gt; = 0.145)] has two distinct Fe environments—the tertiary amine is &lt;i&gt;cis&lt;/i&gt; to the oxido bridge at one site and is &lt;i&gt;trans&lt;/i&gt; to the oxido bridge at the other site; the &lt;i&gt;trans&lt;/i&gt; Fe–N&lt;sub&gt;3°&lt;/sub&gt; distance is longer. Both the Br and &lt;i&gt;N&lt;/i&gt;CO derivatives are monoclinic, C2/c [with a = 16.1480(17), b = 17.2036(13), c = 16.8521(12), β = 111.204(10), data collected at 293 K, 3753 reflections (2404 observed), R = 0.069 (R&lt;sub&gt;w&lt;/sub&gt; = 0.151), and a = 15.7470(9), b = 18.2270(11), c = 16.8950(8), β = 110.666(3), data collected at 90 K, 5392 reflections (3028 observed), R = 0.064 (R&lt;sub&gt;w&lt;/sub&gt; = 0.091), respectively]. Both polymorphs of the &lt;i&gt;N&lt;/i&gt;CS derivative are monoclinic—one is P2&lt;sub&gt;1&lt;/sub&gt;/c and the other P2&lt;sub&gt;1&lt;/sub&gt;/n [a = 11.075(2), b = 15.436(2), c = 12.351(2), β = 95.528(7), data collected at 90 K, 5378 reflections (4345 observed), R = 0.068 (R&lt;sub&gt;w&lt;/sub&gt; = 0.198), and a = 12.396(2), b = 15.428(3), c = 44.505(8), β = 95.211(7), data collected at 110 K, 16,527 reflections (6540 observed), R = 0.069 (R&lt;sub&gt;w&lt;/sub&gt; = 0.105), respectively]. For the Br, &lt;i&gt;N&lt;/i&gt;CO and &lt;i&gt;N&lt;/i&gt;CS dimers, each iron of the [{Fe(TPA)X}&lt;sub&gt;2&lt;/sub&gt;O]&lt;sup&gt;2+&lt;/sup&gt; unit is pseudo-octahedral with the halide/pseudohalide and oxide ions &lt;i&gt;cis&lt;/i&gt;. The oxide bridge is linear, and the two halides/pseudohalides are &lt;i&gt;anti&lt;/i&gt;. The ranking of &lt;i&gt;trans&lt;/i&gt; influence of the ligands is O&lt;sup&gt;2−&lt;/sup&gt; ≫ Br&lt;sup&gt;−&lt;/sup&gt; &gt; Cl&lt;sup&gt;−&lt;/sup&gt; &gt; N&lt;sub&gt;3&lt;/sub&gt;&lt;sup&gt;−&lt;/sup&gt; &gt; &lt;i&gt;N&lt;/i&gt;CO&lt;sup&gt;−&lt;/sup&gt; ≥ &lt;i&gt;N&lt;/i&gt;CS&lt;sup&gt;−&lt;/sup&gt; &gt; pyridyl &gt; tertiary amine and the ranking of &lt;i&gt;cis&lt;/i&gt; influence of the ligands is O&lt;sup&gt;2−&lt;/sup&gt; ≫ N&lt;sub&gt;3&lt;/sub&gt;&lt;sup&gt;−&lt;/sup&gt; &gt; &lt;i&gt;N&lt;/i&gt;CO&lt;sup&gt;−&lt;/sup&gt; &gt; Cl&lt;sup&gt;−&lt;/sup&gt; ≥ Br&lt;sup&gt;−&lt;/sup&gt; &gt; &lt;i&gt;N&lt;/i&gt;CS&lt;sup&gt;−&lt;/sup&gt;.&lt;/p&gt;&lt;h3&gt;Graphical Abstract&lt;/h3&gt;&lt;p&gt;The X-ray structures of two monomeric [Fe(TPA)(X)&lt;sub&gt;2&lt;/s","PeriodicalId":615,"journal":{"name":"Journal of Chemical Crystallography","volume":"53 1","pages":"50 - 65"},"PeriodicalIF":0.8,"publicationDate":"2022-04-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10870-022-00941-5.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"4887659","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}