We report the comparative synthetic methodologies and characterization of a tetradentate Schiff base ligand 1,2-(diimino-4&#x2032;-antipyrinyl)-1,2-diphenylethane (DE). The target synthesis of oxovanadium(IV) and dioxouranium(VI) complexes (vanadyl and uranyl) with the (DE) ligand was also attempted to envisage the effect of metal ion steric factor on complexation process through solution phase thermodynamic and kinetic studies. The thermodynamic stabilities of synthesized vanadyl and uranyl (DE) complexes are discussed in light of their solution phase thermodynamic stability constants obtained by electroanalytical method. A comparative kinetic profile of vanadyl and uranyl complexation with DE is also reported. The complexation reaction proceeds with an overall 2nd order kinetics with both metal ions. Temperature dependent studies of rate constants present an activation energy barrier of ca. 40.913 and 48.661&#x2009;KJ&#x2009;mol&#x2212;1, for vanadyl and uranyl complexation, respectively, highlighting the metal ion steric and ligand preorganization effects. The synthesized Schiff base ligand and its vanadyl and uranyl complexes were screened for biocidal potential as antibacterial, antifungal, and anthelmintic agents with the results compared to corresponding reference drugs.

Shabnum Bashir

Syed Raashid Maqsood

Ghulam Mustafa Peerzada

Badruddin Khan

Masood Ahmad Rizvi

Complexation of Oxovanadium(IV) and Dioxouranium(VI) with Synthesized 1,2-(Diimino-4&#x2032;-antipyrinyl)-1,2-diphenylethane Schiff Base: A Thermodynamic, Kinetic, and Bioactivity Investigation

Rutile pigments <svg xmlns:xlink="http://www.w3.org/1999/xlink" xmlns="http://www.w3.org/2000/svg" style="vertical-align:-3.542pt" id="M1" height="13.2403pt" version="1.1" viewBox="-0.0498162 -9.6983 106.633 13.2403" width="106.633pt"><g transform="matrix(.0135,0,0,-0.0135,0,0)"><path id="g190-85" d="M592 498C586 556 582 629 581 675H560C545 656 537 650 510 650H115C87 650 74 652 60 675H40C38 620 33 555 28 495H57C69 539 77 568 89 585C102 607 122 616 205 616H267V123C267 44 259 34 168 28V0H454V28C360 34 352 44 352 123V616H422C498 616 514 608 531 584C542 568 552 543 562 495L592 498Z"/></g><g transform="matrix(.0135,0,0,-0.0135,8.142,0)"><path id="g190-106" d="M135 536C164 536 186 560 186 587C186 617 164 639 136 639C109 639 85 617 85 587C85 560 109 536 135 536ZM252 0V26C188 32 181 38 181 106V451C138 433 90 420 39 412V388C99 379 102 374 102 312V106C102 38 95 32 32 26V0H252Z"/></g><g transform="matrix(.0095,0,0,-0.0095,11.818,3.264)"><path id="g50-50" d="M389 0V32C297 38 291 46 291 118V635C234 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89C47 89 24 61 24 40C24 8 49 -12 75 -12C125 -12 175 31 271 175L312 64C330 15 357 -12 382 -12C421 -12 475 35 515 98L496 121C466 88 439 62 420 62C402 62 384 92 363 147L325 247C349 280 374 309 397 333C422 361 446 381 462 381C471 381 481 374 488 366C493 360 499 357 505 357C521 357 545 380 545 403Z"/></g><g transform="matrix(.0135,0,0,-0.0135,32.82,0)"><path id="g190-68" d="M614 175C564 76 510 21 408 21C256 21 146 149 146 336C146 488 235 629 402 629C510 629 570 586 597 480L626 488C620 541 614 582 606 638C578 643 510 665 429 665C206 665 44 527 44 316C44 157 153 -15 402 -15C474 -15 558 5 586 11C604 45 629 119 643 165L614 175Z"/></g><g transform="matrix(.0135,0,0,-0.0135,41.83,0)"><path id="g190-115" d="M181 342V451C133 431 89 419 40 411V388C98 381 102 377 102 311V104C102 38 95 32 33 26V0H263V26C186 32 181 38 181 104V287C203 343 235 372 261 372C277 372 289 366 304 352C310 346 318 345 330 350C349 359 362 379 362 399C362 422 338 449 304 449C256 449 213 393 183 342H181Z"/></g><g 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635C179 635 131 609 100 575L42 494L67 471C94 510 138 565 205 565C277 565 321 517 321 435C321 348 258 270 195 195C146 137 88 81 33 26V0H411C423 44 433 88 446 135L414 144Z"/></g><g transform="matrix(.0095,0,0,-0.0095,74.495,3.264)"><use xlink:href="#g50-121"/></g><g transform="matrix(.0135,0,0,-0.0135,80.427,0)"><path id="g190-80" d="M381 665C170 665 44 498 44 318C44 125 188 -15 369 -15C552 -15 703 117 703 333C703 534 550 665 381 665ZM359 629C491 629 601 517 601 306C601 114 502 21 390 21C249 21 146 158 146 346S248 629 359 629Z"/></g><g transform="matrix(.0095,0,0,-0.0095,90.585,3.264)"><use xlink:href="#g50-51"/></g><g transform="matrix(.0095,0,0,-0.0095,95.204,3.264)"><path id="g54-37" d="M556 297V350H337V548H275V350H56V297H275V85H337V297H556ZM556 -23V30H56V-23H556Z"/></g><g transform="matrix(.0095,0,0,-0.0095,100.998,3.264)"><path id="g50-226" d="M501 517C491 587 426 710 310 710C240 710 175 662 175 601C175 561 201 517 250 452C219 438 187 423 157 404C88 360 24 280 24 178C24 71 90 -12 195 -12C250 -12 297 6 334 32C412 87 452 170 452 249C452 335 408 396 333 481C259 565 229 601 229 621C229 642 245 652 275 652C359 652 427 583 490 499L501 517ZM364 233C364 142 323 33 222 33C173 33 119 81 119 178C119 265 156 335 193 374C213 395 242 413 272 425C308 384 364 319 364 233Z"/></g></svg> (where <svg xmlns:xlink="http://www.w3.org/1999/xlink" xmlns="http://www.w3.org/2000/svg" style="vertical-align:-0.2130003pt" id="M2" height="8.91176pt" version="1.1" viewBox="-0.0498162 -8.69876 29.7816 8.91176" width="29.7816pt"><g transform="matrix(.0135,0,0,-0.0135,0,0)"><path id="g113-121" d="M536 404C536 423 520 448 491 448C445 448 398 404 308 283L286 338C255 416 242 448 217 448C182 448 138 402 92 341L111 321C149 368 169 378 178 378C188 378 198 363 214 320L254 212C185 117 138 65 107 65C98 65 85 69 82 75C79 82 73 86 65 86C44 86 23 60 23 39C23 7 44 -12 71 -12C119 -12 168 33 265 177L306 61C321 17 347 -12 373 -12C413 -12 465 33 507 96L491 119C459 84 432 60 413 60C395 60 378 92 358 148L321 250C341 279 369 310 389 332C417 363 439 382 456 382C466 382 475 376 481 368C486 361 492 358 496 358C513 358 536 381 536 404Z"/></g><g transform="matrix(.0135,0,0,-0.0135,11.359,0)"><path id="g117-34" d="M535 323V373H52V323H535ZM535 138V188H52V138H535Z"/></g><g transform="matrix(.0135,0,0,-0.0135,23.096,0)"><path id="g113-49" d="M241 635C89 635 35 457 35 312C35 153 89 -12 240 -12C390 -12 443 166 443 312C443 466 390 635 241 635ZM238 602C329 602 354 454 354 312C354 172 330 22 240 22C152 22 124 173 124 313S148 602 238 602Z"/></g></svg>, 0.05, 0.10, 0.20, 0.30 and 0.50) prepared by solid-state reaction are investigated. Chromium is chromophore (coloring ion) and niobium is counterion (charge-compensating element for electroneutrality). The effect of composition (x), calcination temperature (850, 900, 950, 1000, 1050, 1100 and 1150°C), and starting titanium compounds (anatase TiO2, hydrated anatase paste, TiOSO4<svg xmlns:xlink="http://www.w3.org/1999/xlink" xmlns="http://www.w3.org/2000/svg" style="vertical-align:-0.04981995pt" id="M3" height="4.3561pt" version="1.1" viewBox="-0.0498162 -4.30628 3.20019 4.3561" width="3.20019pt"><g transform="matrix(.0135,0,0,-0.0135,0,0)"><path id="g113-46" d="M170 255C170 288 146 313 114 313S58 288 58 255C58 221 82 198 114 198S170 221 170 255Z"/></g></svg>2H2O, and hydrated Na2Ti4O9 paste) on their color properties into organic matrix and particle size distribution was observed. According to the highest chroma C and visual color evaluation, yellow and orange pigments were selected as in color the most interesting. They have concentration <svg xmlns:xlink="http://www.w3.org/1999/xlink" xmlns="http://www.w3.org/2000/svg" style="vertical-align:-0.2130003pt" id="M4" height="8.91176pt" version="1.1" viewBox="-0.0498162 -8.69876 45.9372 8.91176" width="45.9372pt"><g transform="matrix(.0135,0,0,-0.0135,0,0)"><use xlink:href="#g113-121"/></g><g transform="matrix(.0135,0,0,-0.0135,11.359,0)"><use xlink:href="#g117-34"/></g><g transform="matrix(.0135,0,0,-0.0135,23.096,0)"><use xlink:href="#g113-49"/></g><g transform="matrix(.0135,0,0,-0.0135,29.6,0)"><path id="g113-47" d="M113 -12C146 -12 170 11 170 46C170 78 146 103 114 103S58 78 58 46C58 11 82 -12 113 -12Z"/></g><g transform="matrix(.0135,0,0,-0.0135,32.689,0)"><use xlink:href="#g113-49"/></g><g transform="matrix(.0135,0,0,-0.0135,39.192,0)"><path id="g113-54" d="M153 550H386L412 615L406 623H120L82 318C104 327 142 338 184 338C294 338 347 275 347 187C347 112 305 39 221 39C160 39 119 71 97 89C88 97 80 96 71 90C59 80 50 67 49 57C48 45 52 36 66 23C80 9 123 -12 169 -12C221 -11 288 15 342 59C403 109 431 165 431 225C431 308 366 395 238 395C212 395 165 379 127 364L153 550Z"/></g></svg> or 0.10 and are prepared from anatase TiO2 and TiOSO4<svg xmlns:xlink="http://www.w3.org/1999/xlink" xmlns="http://www.w3.org/2000/svg" style="vertical-align:-0.04981995pt" id="M5" height="4.3561pt" version="1.1" viewBox="-0.0498162 -4.30628 3.20019 4.3561" width="3.20019pt"><g transform="matrix(.0135,0,0,-0.0135,0,0)"><use xlink:href="#g113-46"/></g></svg>2H2O at temperature <svg xmlns:xlink="http://www.w3.org/1999/xlink" xmlns="http://www.w3.org/2000/svg" style="vertical-align:-1.16493pt" id="M6" height="9.26535pt" version="1.1" viewBox="-0.0498162 -8.10042 8.08224 9.26535" width="8.08224pt"><g transform="matrix(.0135,0,0,-0.0135,0,0)"><path id="g117-94" d="M531 285V335L57 550V494L473 310L57 127V71L531 285ZM531 -40V10H57V-40H531Z"/></g></svg>1050°C.

Jan Ve&#x10d;e&#x159;a

Iveta &#x160;edov&#xe1;

Petr Mikul&#xe1;&#x161;ek

Petra &#x160;ulcov&#xe1;

Synthesis and Characterization of Rutile Pigments with Cr and Nb

High quality and transparent single crystals of undoped rutile TiO2, Al-doped rutile (Al&#x2009;:&#x2009;TiO2), and Zr-doped rutile (Zr&#x2009;:&#x2009;TiO2) have been grown successfully by tilting-mirror-type floating zone (TMFZ) using travelling solvent floating (TSFZ) technique. The effect of doping on the electronic and optical properties of rutile has been studied experimentally as well as by simulation calculations. The effect of doping on the quality of crystals was also investigated by observing optical micrograph and measuring etch pits density that reveals the presence of defects. Undoped rutile crystals were dark blue and comprised many low-angle grain boundaries. Al+3 and Zr+4 ions pin down the migration of dislocations during the cooling and create oxygen vacancies. Doping of the impurities would improve the electronic and optical properties of rutile. The elastic properties might be changed for doping of the impurities in the rutile crystals.

Md. Abdur Razzaque Sarker

Optical Properties of Al- and Zr-Doped Rutile Single Crystals Grown by Tilting-Mirror-Type Floating Zone Method and Study of Structure-Property Relationships by First Principle Calculations

Copper(II) complexes of 2-(methylthiomethyl)anilines (1a&#x2013;1f) have been obtained and characterized by elemental analyses, IR, electronic spectra, conductivity, and X-ray crystallography. The complexes (2a&#x2013;2f) have the structural formula [CuCl2L] with the bidentate ligand coordinating through sulfur and nitrogen. The single crystal X-ray diffraction data reveal that the copper complex (2f) has a tetragonally distorted octahedral structure with long Cu&#x2013;Cl equatorial bonds. Magnetic susceptibility measurements indicate the availability of one unpaired electron in the complexes and the conductivity measurements in DMF show their behaviour as nonelectrolytes. The solid reflectance spectra and the electronic spectra of the complexes in DMSO were determined. The ligands and their copper complexes were screened for in vitro antimicrobial activity against S. aureus, B. subtilis, E. coli, and C. albicans. The methoxysubstituted complex (2c) showed more promising antibacterial activity against S. aureus and B. subtilis than other compounds at the concentration tested.

Temitope E. Olalekan

Denzil R. Beukes

Bernardus Van Brecht

Gareth M. Watkins

Copper(II) Complexes of 2-(Methylthiomethyl)anilines: Spectral and Structural Properties and In Vitro Antimicrobial Activity

Mixed-ligand palladium(II) chloride complexes bearing the nucleobases, adenine (Ad), cytosine (Cyt), and guanine (Gua), have been synthesized and characterized by UV-vis spectrophotometric methods, magnetic susceptibility, molar conductivity, elemental analysis, FTIR, and 1H-NMR. The complexes were found to have the composition cis-[PdCl2(Gua)(Cyt)], cis-[PdCl2(Ad)(Cyt)], and cis-[PdCl2(Ad)(Gua)]. A four-coordinated square-planar geometry is proposed for these Pd(II) complexes based on magnetic evidence and electronic spectra. The complexes as well as the free nucleobase ligands were tested for their in vitro cytotoxicity on human promyelocytic leukemia (HL60) and human histiocytic leukemia (U937) cell lines. cis-[PdCl2(Ad)(Gua)] showed IC50 values of 11.29&#x2009;&#xb1;&#x2009;2.91 and 8.31&#x2009;&#xb1;&#x2009;1.44&#x2009;&#x3BC;M against HL60 and U937, respectively, which was higher than that of the positive control (curcumin) against U937. The complexes also showed significant antioxidant activity when tested against 2,2-diphenyl-1-picrylhydrazylradical (DPPH).

Samuel Tetteh

David K. Dodoo

Regina Appiah-Opong

Isaac Tuffour

Spectroscopic Characterization, In Vitro Cytotoxicity, and Antioxidant Activity of Mixed Ligand Palladium(II) Chloride Complexes Bearing Nucleobases

New symmetrical binucleating ligands N,N-bis[2-hydroxy-5-methyl-3-(4-methyl-piperazinomethyl)benzyl]-alkylamines L1 and L2 and their copper(II) complexes [Cu2L(X)2]&#x000B7;2H2O, where X = CH3COO&#x2212;, C6H5COO&#x2212;, Cl&#x2212;, and <svg style="vertical-align:-3.276pt;width:42.375px;" id="M1" height="16.3125" version="1.1" viewBox="0 0 42.375 16.3125" width="42.375" xmlns:xlink="http://www.w3.org/1999/xlink" xmlns="http://www.w3.org/2000/svg">
	
		
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			<g transform="matrix(.012,-0,0,-.012,28.362,16.25)"><path id="x34" d="M456 178h-96v-72q0 -51 12.5 -62.5t72.5 -16.5v-27h-256v27q65 5 78 17t13 62v72h-260v28q182 271 300 426h40v-407h96v-47zM280 225v295h-2q-107 -148 -196 -295h198z" /></g><g transform="matrix(.012,-0,0,-.012,34.7,4)"><path id="x2212" d="M535 230h-483v50h483v-50z" /></g>

		
	
</svg>, were prepared and characterised. All the complexes undergo quasi-reversible reduction at negative potential (E = &#x2212;0.48 to &#x2212;1.02&#x2009;V). The acetate and benzoate complexes undergo a two-step single electron transfer at &#x2013;0.48 to &#x2013;0.60&#x2009;V and &#x2212;0.9 to &#x2212;1.02&#x2009;V. The chloro and perchlorate complexes undergo a single step two-electron transfer at &#x2212;0.55 to &#x2212;0.75&#x2009;V. Variable temperature magnetic studies show the presence of weak exchange interaction for acetate (&#x2212;2&#x2009;J around 25 to 40&#x2009;cm&#x2212;1) and benzoate (&#x2212;2&#x2009;J around 45 to 55&#x2009;cm&#x2212;1) bridged complexes and no exchange interaction is found for chloro and perchlorate complexes. ESR spectra of chloro and perchlorate complexes are like mononuclear copper(II) complexes with hyperfine splitting (A = 165 &#xb1; 5, <svg style="vertical-align:-5.59785pt;width:15.3125px;" id="M2" height="14.7125" version="1.1" viewBox="0 0 15.3125 14.7125" width="15.3125" xmlns:xlink="http://www.w3.org/1999/xlink" xmlns="http://www.w3.org/2000/svg">
	
		
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			<g transform="matrix(.012,-0,0,-.012,9.738,12.712)"><path id="x2016" d="M162 -163h-60v866h60v-866zM309 -163h-60v866h60v-866z" /></g>

		
	
</svg> = 2.17&#x2013;2.23, and <svg style="vertical-align:-4.0404pt;width:18.4px;" id="M3" height="12.775" version="1.1" viewBox="0 0 18.4 12.775" width="18.4" xmlns:xlink="http://www.w3.org/1999/xlink" xmlns="http://www.w3.org/2000/svg">
	
		
			<g transform="matrix(.017,-0,0,-.017,.062,7.675)"><use xlink:href="#x1D454"/></g>

			<g transform="matrix(.012,-0,0,-.012,9.738,12.713)"><path id="x27C2" d="M619 0h-566v50h254v498h58v-498h254v-50z" /></g>

		
	
</svg> = 2.05&#x2013;2.10). The ESR spectra of acetate and benzoate complexes are like binuclear copper(II) complexes with broad signal (<svg style="vertical-align:-3.56265pt;width:9.8000002px;" id="M4" height="12.175" version="1.1" viewBox="0 0 9.8000002 12.175" width="9.8000002" xmlns:xlink="http://www.w3.org/1999/xlink" xmlns="http://www.w3.org/2000/svg">
	
		
			<g transform="matrix(.017,-0,0,-.017,.062,7.675)"><use xlink:href="#x1D454"/></g>

		
	
</svg> = 2.2).

K. Jothivenkatachalam

S. Chandra Mohan

Synthesis and Characterisation of New Symmetrical Binucleating Ligands and Their Binuclear Copper(II) Complexes

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Journal of Inorganic Chemistry