Startseite Naturwissenschaften Crystal structure of fac-(acetylacetonato-κ2O,O′)tricarbonyl(tri(p-tolyl)phosphine-κP)rhenium(I), C29H28O5PRe
Artikel Open Access

Crystal structure of fac-(acetylacetonato-κ2O,O′)tricarbonyl(tri(p-tolyl)phosphine-κP)rhenium(I), C29H28O5PRe

  • Amanda-Lee Manicum EMAIL logo , Marietjie Schutte-Smith und Hendrik G. Visser
Veröffentlicht/Copyright: 13. September 2017

Abstract

C29H28O5PRe, triclinic, P1̄ (no. 2), a = 12.733(7) Å, b = 18.668(11) Å, c = 24.779(15) Å, α = 101.442(20)°, β = 100.844(18)°, γ = 104.240(19)°, V = 5419(9) Å3, Z = 8, Rgt(F) = 0.0307, wRref(F2) = 0.0772, T = 100 K.

CCDC no.:: 1569066

One representative complex is shown (Z′ = 4) n = A, B, C, D and n′ = 1–4 for the four respective molecules. Tables 1 and 2 contain details of the measurement method and a list of the atoms including atomic coordinates and displacement parameters.

Table 1

Data collection and handling.

Crystal:Colourless cuboid
Size:0.44 × 0.34 × 0.24 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:45.8 cm−1
Diffractometer, scan mode:Bruker APEX-II, φ and ω
2θmax, completeness:56.6°, >99%
N(hkl)measured, N(hkl)unique, Rint:108469, 26855, 0.068
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 22905
N(param)refined:1298
Programs:Bruker programs [1], SHELX [2], SIR97 [3], DIAMOND [4], ORTEP [5]
Table 2

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).

AtomxyzUiso*/Ueq
C1A0.8610(3)0.4638(2)0.06053(15)0.0215(7)
C1B0.1405(3)0.1967(2)0.21517(15)0.0236(8)
C1C0.7777(3)−0.09041(19)0.24114(14)0.0175(7)
C1D1.3331(3)−0.3686(2)0.40066(15)0.0211(7)
C2A0.6893(3)0.36545(19)0.08047(14)0.0196(7)
C2B0.2517(3)0.1190(2)0.27255(15)0.0216(7)
C2C0.8896(3)−0.1711(2)0.29682(14)0.0211(7)
C2D1.1544(3)−0.4750(2)0.39997(15)0.0228(7)
C3A0.6554(3)0.4456(2)0.00131(15)0.0268(8)
C3B0.0652(3)0.0409(2)0.18988(15)0.0248(8)
C3C0.9625(3)−0.0141(2)0.32562(16)0.0265(8)
C3D1.3439(3)−0.4620(2)0.47095(16)0.0277(8)
C4A0.4951(3)0.1825(2)−0.11948(15)0.0239(8)
H4A10.46160.168−0.08930.036*
H4A20.51690.1397−0.13920.036*
H4A30.44060.1954−0.14660.036*
C4B0.3412(3)−0.0594(2)0.11076(16)0.0304(9)
H4B10.3706−0.06450.14880.046*
H4B20.4034−0.04270.09370.046*
H4B30.2909−0.10880.0870.046*
C4C0.8849(3)−0.0739(2)0.50317(15)0.0294(8)
H4C10.9265−0.11140.49730.044*
H4C20.8208−0.09490.51770.044*
H4C30.9341−0.02680.53070.044*
C4D1.1549(3)−0.4244(3)0.61471(18)0.0382(10)
H4D11.0942−0.46920.59090.057*
H4D21.1235−0.38840.6360.057*
H4D31.2058−0.44050.64140.057*
C5A0.5970(3)0.2509(2)−0.09391(14)0.0201(7)
C5B0.2779(3)−0.00123(19)0.11499(15)0.0212(7)
C5C0.8442(3)−0.0566(2)0.44757(15)0.0233(7)
C5D1.2181(3)−0.3860(2)0.57760(16)0.0265(8)
C6A0.6577(3)0.2819(2)−0.12914(15)0.0251(8)
H6A0.63210.2581−0.16870.03*
C6B0.2288(3)0.0162(2)0.06637(15)0.0252(8)
H6B0.2358−0.01120.03120.03*
C6C0.7827(3)−0.0041(2)0.44570(14)0.0251(8)
H6C0.76930.01890.48050.03*
C6D1.3086(3)−0.3203(2)0.60350(15)0.0292(9)
H6D1.3247−0.30240.64370.035*
C7A0.7527(3)0.3448(2)−0.11150(15)0.0238(8)
C7B0.1699(3)0.0702(2)0.06393(15)0.0226(7)
C7C0.7394(3)0.01749(19)0.39798(15)0.0213(7)
C7D1.3768(3)−0.2789(2)0.57595(15)0.0230(7)
C8A0.8099(3)0.3691(2)−0.15599(15)0.0345(9)
H8A10.8750.414−0.13770.052*
H8A20.75730.382−0.18410.052*
H8A30.83430.3272−0.1750.052*
C8B0.1227(3)0.0833(2)0.00765(15)0.0310(9)
H8B10.08460.12270.01360.047*
H8B20.06930.0356−0.01710.047*
H8B30.18360.1001−0.01030.047*
C8C0.6729(3)0.0743(2)0.40238(16)0.0305(9)
H8C10.6490.08310.36490.046*
H8C20.71960.12270.42920.046*
H8C30.60690.05390.41590.046*
C8D1.4706(3)−0.2093(2)0.61028(16)0.0298(8)
H8D11.5109−0.18660.58490.045*
H8D21.5221−0.22390.63770.045*
H8D31.44−0.1720.63070.045*
C11A0.9796(3)0.34911(19)0.10138(14)0.0184(7)
C11B0.4316(3)0.30111(19)0.24776(14)0.0200(7)
C11C0.6094(3)−0.28057(19)0.26070(14)0.0182(7)
C11D1.0342(3)−0.35206(19)0.36933(14)0.0187(7)
C12A1.0891(3)0.3813(2)0.10062(16)0.0268(8)
H12A1.11020.3750.06560.032*
C12B0.5157(3)0.3609(2)0.24207(16)0.0284(8)
H12B0.5440.35470.20910.034*
C12C0.5417(3)−0.3467(2)0.26843(15)0.0251(8)
H12C0.5171−0.34510.30240.03*
C12D0.9190(3)−0.36788(19)0.36152(14)0.0206(7)
H12D0.8889−0.35550.39320.025*
C13A1.1686(3)0.4230(2)0.15099(16)0.0310(9)
H13A1.24360.44480.14970.037*
C13B0.5586(3)0.4291(2)0.28400(16)0.0286(8)
H13B0.61560.46930.27920.034*
C13C0.5098(3)−0.4150(2)0.22671(16)0.0275(8)
H13C0.464−0.45960.23290.033*
C13D0.8478(3)−0.4015(2)0.30800(15)0.0255(8)
H13D0.7693−0.41170.30350.031*
C14A1.1414(3)0.4334(2)0.20260(15)0.0269(8)
C14B0.5196(3)0.4400(2)0.33298(15)0.0259(8)
C14C0.5428(3)−0.4200(2)0.17632(15)0.0242(8)
C14D0.8887(3)−0.4207(2)0.26055(15)0.0248(8)
C15A1.0309(3)0.4013(2)0.20307(16)0.0288(8)
H15A1.010.40760.23810.035*
C15B0.4352(3)0.3804(2)0.33813(15)0.0261(8)
H15B0.40650.38660.37090.031*
C15C0.6112(3)−0.3530(2)0.16883(15)0.0258(8)
H15C0.6355−0.35460.13480.031*
C15D1.0049(3)−0.4030(2)0.26833(15)0.0270(8)
H15D1.0351−0.41440.23650.032*
C16A0.9516(3)0.3607(2)0.15361(15)0.0245(8)
H16A0.87630.34020.15490.029*
C16B0.3920(3)0.3118(2)0.29634(15)0.0240(8)
H16B0.33470.27180.3010.029*
C16C0.6434(3)−0.2851(2)0.21032(14)0.0218(7)
H16C0.6899−0.24060.20440.026*
C16D1.0752(3)−0.3697(2)0.32123(15)0.0246(8)
H16D1.1537−0.35820.32550.03*
C17A1.2290(3)0.4776(3)0.25685(17)0.0427(11)
H17A1.19440.47940.2890.064*
H17B1.26190.52970.25440.064*
H17C1.28770.45230.26240.064*
C17B0.5686(4)0.5141(2)0.37821(17)0.0384(10)
H17D0.53170.51210.40940.058*
H17E0.55740.55630.36210.058*
H17F0.64890.52230.39270.058*
C17C0.5085(3)−0.4945(2)0.13160(17)0.0352(9)
H17G0.5391−0.48660.09910.053*
H17H0.4266−0.51350.11910.053*
H17I0.5373−0.5320.14750.053*
C17D0.8114(3)−0.4596(3)0.20221(16)0.0390(10)
H17J0.8558−0.46810.17460.059*
H17K0.7656−0.42710.19130.059*
H17L0.7626−0.50880.20290.059*
C21A0.8087(3)0.20825(18)0.05539(13)0.0177(7)
C21B0.5125(3)0.17775(19)0.20704(14)0.0185(7)
C21C0.5145(3)−0.16280(19)0.29751(13)0.0167(7)
C21D1.1984(3)−0.21424(19)0.43085(14)0.0191(7)
C22A0.8785(3)0.1720(2)0.08264(14)0.0228(7)
H22A0.95730.19460.09340.027*
C22B0.6087(3)0.2137(2)0.19256(15)0.0241(8)
H22B0.60720.2520.17250.029*
C22C0.4135(3)−0.2079(2)0.30319(15)0.0221(7)
H22C0.4127−0.25150.31760.026*
C22D1.3141(3)−0.1799(2)0.44813(14)0.0205(7)
H22D1.3615−0.20630.46440.025*
C23A0.8321(3)0.1028(2)0.09390(15)0.0282(8)
H23A0.88020.07830.11220.034*
C23B0.7067(3)0.1943(2)0.20693(16)0.0266(8)
H23B0.77120.21940.19640.032*
C23C0.3148(3)−0.1897(2)0.28808(14)0.0226(7)
H23C0.2476−0.22070.29280.027*
C23D1.3601(3)−0.1078(2)0.44170(15)0.0247(8)
H23D1.4389−0.08540.45390.03*
C24A0.7168(3)0.0682(2)0.07908(15)0.0261(8)
C24B0.7122(3)0.1387(2)0.23663(15)0.0232(7)
C24C0.3122(3)−0.1269(2)0.26605(14)0.0219(7)
C24D1.2938(3)−0.0676(2)0.41784(15)0.0240(8)
C25A0.6485(3)0.1056(2)0.05262(15)0.0238(8)
H25A0.56970.08330.04250.029*
C25B0.6158(3)0.1026(2)0.25096(15)0.0236(8)
H25B0.61750.06430.2710.028*
C25C0.4115(3)−0.0827(2)0.25981(14)0.0218(7)
H25C0.4112−0.03990.24460.026*
C25D1.1787(3)−0.1022(2)0.40055(15)0.0267(8)
H25D1.1315−0.0760.38390.032*
C26A0.6929(3)0.1743(2)0.04071(14)0.0213(7)
H26A0.64450.19850.02250.026*
C26B0.5172(3)0.12169(19)0.23653(14)0.0199(7)
H26B0.45250.09640.24680.024*
C26C0.5121(3)−0.0996(2)0.27539(14)0.0205(7)
H26C0.5792−0.06810.2710.025*
C26D1.1312(3)−0.1744(2)0.40712(15)0.0247(8)
H26D1.0524−0.19660.39530.03*
C27A0.6670(4)−0.0067(2)0.09175(19)0.0398(10)
H27A0.7272−0.02440.11030.06*
H27B0.6238−0.04470.05620.06*
H27C0.61770.00040.1170.06*
C27B0.8192(3)0.1181(2)0.25245(17)0.0336(9)
H27D0.87740.14910.23880.05*
H27E0.80650.06380.2350.05*
H27F0.84320.12810.29390.05*
C27C0.2042(3)−0.1082(2)0.24890(17)0.0325(9)
H27G0.1433−0.14550.25640.049*
H27H0.188−0.11040.20830.049*
H27I0.2111−0.05680.27080.049*
C27D1.3449(3)0.0108(2)0.41083(18)0.0358(10)
H27J1.28560.03030.39360.054*
H27K1.39650.00770.38630.054*
H27L1.3860.04540.44810.054*
C31A0.9373(3)0.26878(19)−0.01782(14)0.0183(7)
C31B0.3794(3)0.23526(19)0.12813(14)0.0188(7)
C31C0.6471(3)−0.21734(19)0.37949(13)0.0167(7)
C31D1.0556(3)−0.2951(2)0.49070(14)0.0199(7)
C32A0.9962(3)0.3251(2)−0.03973(15)0.0221(7)
H32A1.00110.3771−0.0250.027*
C32B0.3264(3)0.2901(2)0.11822(15)0.0247(8)
H32B0.29530.31290.14660.03*
C32C0.7144(3)−0.2628(2)0.39317(14)0.0229(8)
H32C0.7578−0.27760.36810.028*
C32D0.9880(3)−0.3586(2)0.50176(15)0.0240(8)
H32D0.9767−0.40820.47850.029*
C33A1.0476(3)0.3056(2)−0.08286(15)0.0256(8)
H33A1.08830.3445−0.0970.031*
C33B0.3185(3)0.3117(2)0.06750(15)0.0261(8)
H33B0.28280.34970.06190.031*
C33C0.7193(3)−0.2869(2)0.44278(15)0.0250(8)
H33C0.7652−0.31840.45110.03*
C33D0.9370(3)−0.3501(2)0.54645(16)0.0298(9)
H33D0.8893−0.3940.55260.036*
C34A1.0403(3)0.2292(2)−0.10578(15)0.0236(8)
C34B0.3616(3)0.2788(2)0.02480(15)0.0219(7)
C34C0.6575(3)−0.2653(2)0.48048(14)0.0211(7)
C34D0.9544(3)−0.2788(3)0.58233(16)0.0335(10)
C35A0.9801(3)0.1736(2)−0.08430(15)0.0234(7)
H35A0.9730.1214−0.09980.028*
C35B0.4101(3)0.2219(2)0.03401(15)0.0246(8)
H35B0.43810.19740.0050.03*
C35C0.5952(3)−0.2163(2)0.46820(14)0.0221(7)
H35C0.5557−0.19870.49440.026*
C35D1.0192(3)−0.2157(3)0.57058(16)0.0336(9)
H35D1.03−0.16620.5940.04*
C36A0.9301(3)0.19315(19)−0.04068(14)0.0198(7)
H36A0.89040.1542−0.02630.024*
C36B0.4185(3)0.2000(2)0.08456(14)0.0212(7)
H36B0.45140.16050.08950.025*
C36C0.5896(3)−0.1927(2)0.41858(14)0.0198(7)
H36C0.5463−0.15940.41110.024*
C36D1.0694(3)−0.2230(2)0.52489(15)0.0274(8)
H36D1.1129−0.17870.51730.033*
C37A1.0964(3)0.2081(2)−0.15229(16)0.0343(9)
H37A1.13460.2545−0.16180.052*
H37B1.04010.1737−0.1860.052*
H37C1.15110.1824−0.13930.052*
C37B0.3565(3)0.3052(2)−0.02864(16)0.0317(9)
H37D0.31930.3455−0.02690.048*
H37E0.31420.2621−0.06140.048*
H37F0.43260.3254−0.03260.048*
C37C0.6571(3)−0.2946(2)0.53295(16)0.0331(9)
H37G0.7054−0.32810.53460.05*
H37H0.5806−0.32340.53150.05*
H37I0.6852−0.25130.56680.05*
C37D0.9076(4)−0.2705(3)0.63470(17)0.0485(13)
H37J0.8639−0.3210.63620.073*
H37K0.8593−0.2370.63270.073*
H37L0.9694−0.24830.6690.073*
O1A0.9307(2)0.51703(14)0.08670(11)0.0319(6)
O1B0.0997(2)0.24427(17)0.22686(12)0.0380(7)
O1C0.74866(19)−0.08874(14)0.19430(10)0.0232(5)
O1D1.3778(2)−0.35750(15)0.36545(10)0.0276(6)
O2A0.6562(2)0.35904(14)0.12002(10)0.0274(6)
O2B0.2779(2)0.12048(16)0.32028(11)0.0310(6)
O2C0.9300(2)−0.21903(15)0.28540(11)0.0296(6)
O2D1.0945(2)−0.52600(15)0.36482(11)0.0323(6)
O3A0.6113(3)0.49184(19)−0.00153(13)0.0492(9)
O3B−0.0171(2)−0.00089(16)0.18877(12)0.0359(7)
O3C1.0441(2)0.03077(16)0.32850(13)0.0388(7)
O3D1.3856(2)−0.51004(18)0.47353(13)0.0425(8)
O4A0.61673(18)0.27630(13)−0.03988(9)0.0191(5)
O4B0.27709(19)0.02853(14)0.16623(10)0.0209(5)
O4C0.87074(19)−0.09210(14)0.40541(10)0.0228(5)
O4D1.1838(2)−0.41809(15)0.52454(10)0.0242(6)
O5A0.79732(19)0.38462(14)−0.06084(10)0.0207(5)
O5B0.1534(2)0.11241(14)0.10691(10)0.0229(5)
O5C0.74901(19)−0.00613(14)0.34744(10)0.0217(5)
O5D1.37022(18)−0.29578(14)0.52267(10)0.0211(5)
P1A0.86810(7)0.29695(5)0.03730(4)0.01593(17)
P2B0.38580(7)0.20841(5)0.19499(4)0.01696(17)
P3C0.64372(7)−0.18889(5)0.31314(4)0.01565(17)
P4D1.13523(7)−0.30956(5)0.43782(4)0.01733(17)
Re1A0.742490(10)0.375516(7)0.014352(5)0.01548(4)
Re2B0.205511(11)0.116401(8)0.194413(6)0.01708(4)
Re3C0.822697(10)−0.092164(8)0.318269(5)0.01607(4)
Re4D1.258990(11)−0.391199(8)0.458099(6)0.01742(4)

Source of materials

The starting complex fac-[Re(CO)3(H2O)(acac)] was prepared according to a published procedure [1]. fac-[Re(Acac)(CO)3(H2O)] (39 mg; 0.1 mmol) was dissolved in methanol (3 mL) and P(p-tolyl)3 (31 mg; 0.1 mmol) dissolved in 3 mL methanol was added. The solution was stirred for 8 hours at room temperature and then left to crystallize. Yield = 49 mg, 72%. IR (KBr, cm−1): νCO = 2020, 1887.

Experimental details

In the structure all the H atoms were positioned geometrically and refined discemible using a riding model, with C—Hmethine = 0.98 Å; C—Hmethyl = 0.96 Å; C—Haromatic = 0.93 Å. The H atom isotropic displacement parameters were fixed; Uiso(H) = 1.2Ueq(C) for aromatic and methine and Uiso(H) = 1.5Ueq(C) for methyl protons, allowing them to ride on the parent atom.

Comment

In recent years, rhenium has become one of the most studied transition metals due to the development of the fac-[Re(CO)3(H2O)3]+ cation, which bears the possibility of developing radiopharmaceuticals. The coordinated β-diketone type ligand, acetylacetone (Acac), is one of the most frequently used ligands to coordinate to the fac-[Re(CO)3]+ synthon, because the possibility exists to link biomolecules to its backbone. The main reason for the use of a phosphine ligand is because they form robust bonds with organometallic fragments. This study is part of a investigation where the electronic and steric properties of the mono- and bidentate ligands are altered and coordinated to various transition metals to explore their chelating behaviour and reactivity [6], [7], [8], [9], [10], [11], [12], [13].

The title complex, fac-[Re(Acac)(CO)3(P(p-tolyl)3)] crystallizes with eight formula units in the unit cell (Z = 8) and the asymmetric unit contains four independent Re(I) complexes (A, B, C and D). The structure displays a typical octahedral geometry with the rhenium centre surrounded by three facial carbonyl ligands, a β-diketonato ligand and a monodentate tri(p-tolyl)phosphine ligand [14], [15], [16], [17], [18], [19], [20]. All four crystallographically independent complexes display distortion in its octahedral geometry, which is evident from the P1A-Re1A-C3A (174.45(12)°), P2B-Re2B-C3B (176.71(10)°), P3C-Re3C-C3C (177.44(11)°) and P4D-Re4D-C3D (175.15(12)°) bond angles. Intra- and intermolecular C—H⋯O interactions contribute to the supramolecular aggregation.

Acknowledgement

Financial assistance from the University of the Free State is gratefully acknowledged. We also express our gratitude towards NTeMBI, PETLabs Pharmaceuticals, SASOL and the South African National Research Foundation (SA-NRF/THRIP) and Prof A. Roodt. This work is based on the research supported in part by the National Research Foundations of South-Africa and the Thuthuka programme (Grant specific unique reference numbers (UID) 84913 and 94142).

References

Bruker. SADABS and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA, (2004).Suche in Google Scholar

Sheldrick, G. M.: A short history of SHELX. Acta Crystallogr. A64 (2008) 112–122.10.1107/S0108767307043930Suche in Google Scholar PubMed

Altomare, A.; Burla, M. C.; Camalli, M.; Cascarano, G. L.; Giacovazzo, C.; Guagliardi, A.; Moliterni, A. G. G.; Polidori, G.; Spagna, R.: SIR97: a new tool for crystal structure determination and refinement. J. Appl. Crystallogr. 32 (1999) 115–119.10.1107/S0021889898007717Suche in Google Scholar

Brandenburg, K.; Putz, H.: DIAMOND. Visual crystal structure information system. Version 3.2i. Crystal Impact, Bonn, Germany, (2012).Suche in Google Scholar

Farrugia, L. J.: WinGX and ORTEP for Windows: an update. J. Appl. Crystallogr. 45 (2012) 849–854.10.1107/S0021889812029111Suche in Google Scholar

Manicum, A.; Schutte-Smith, M.; Kemp, G.; Visser, H. G.: Illustration of the electronic influence of coordinated β-diketone type ligands: A kinetic and structural study. Polyhedron 85 (2015) 190–195.10.1016/j.poly.2014.08.005Suche in Google Scholar

Manicum, A.; Schutte-Smith, M.; Visser, H. G.; Pretorius, C.; Roodt, A.: Crystal structure of fac-tricarbonyl(hexafluoroacetylacetonato-κ2O,O′)-(nitrato-κO)rhenium(I), C16H21O8N2F6Re, Z. Kristallogr. -NCS 231 (2016) 263–266.10.1515/ncrs-2015-0115Suche in Google Scholar

Visser, H. G.; Roodt, A.; Volmink, A.; Kemp, G.: fac-Tricarbonyl-(pyridine-κN)(1,1,1-trifluoroacetylacetone-κ2O,O′)-rhenium(I). Acta Crystallogr. E67 (2011) m1631–m1631.10.1107/S160053681104476XSuche in Google Scholar PubMed PubMed Central

Schutte, M.; Roodt, A.; Visser, H. G.: Coordinated aqua vs methanol substitution kinetics in fac-Re(I) tricarbonyl tropolonato complexes. Inorg. Chem. 51 (2012) 11996–12006.10.1021/ic301891uSuche in Google Scholar PubMed

Schutte, M.; Kemp, G.; Visser, H. G.; Roodt, A.: Tuning the reactivity in classic low-spin d6 rhenium(I) tricarbonyl radiopharmaceutical synthon by selective bidentate ligand variation (L,L′-Bid; L,L′ = N,N′, N,O and O,O′ donor atom sets) in fac-[Re(CO)3(L,L′-Bid)(MeOH)]n complexes. Inorg. Chem. 50 (2011) 12486–12498.10.1021/ic2013792Suche in Google Scholar PubMed

Brink, A.; Visser, H. G.; Roodt, A.: Novel imino rhenium(I) tricarbonyl complexes of salicylidene-derived ligands: Synthesis, X-ray crystallographic studies, spectroscopic characterization and DFT calculations. Polyhedron 52 (2013) 416–423.10.1016/j.poly.2012.08.059Suche in Google Scholar

Riondato, M.; Camporese, D.; Martín, D.; Suades, J.; Alvarez-Larena, A.; Mazzi, U.: Synthesis and characterisation of [Re(CO)3(SS)(P)] complexes: a [2 + 1] concept for 99mTc- and 188Re-radiopharmaceutical applications. Eur. J. Inorg. Chem. 44 (2005) 4048–4055.10.1002/ejic.200500247Suche in Google Scholar

Marmion, M. E.; Woulfe, S. R.; Neumann, W. L.; Nosco, D. L.; Deutsch, E.: Complexes of technetium-99g and -99m with substituted acac2en and trialkyl phosphines (where acac2en = N,N′-ethylenebis[acetylacetone iminato]). Nucl. Med. Biol. 26 (1999) 755–770.10.1016/S0969-8051(99)00040-2Suche in Google Scholar

Manicum, A.; Visser, H. G.; Engelbrecht, I.; Roodt, A.: Crystal structure of fac-(acetylacetonato-κ2O,O′) tricarbonyl(cyclohexyldiphenylphosphine-κP) rhenium(I), C26H28O5PRe, Z. Kristallogr. -NCS 230 (2015) 150–152.10.1515/ncrs-2014-9013Suche in Google Scholar

Brink, A.; Visser, H. G.; Roodt, A.: Tetraethylammonium (acetylacetonenato)bromidotricarbonylrhenate(I). Acta Crystallogr. E67 (2011) m34–m35.10.1107/S1600536810050105Suche in Google Scholar PubMed PubMed Central

Benny, P. D.; Fugate, G. A.; Barden, A. O.; Morley, J. E.; Silva-Lopez, E.; Twamley, B.: Metal-assisted in situ formation of a tridentate acetylacetone ligand for complexation of fac-Re(CO)3+ for radiopharmaceutical applications. Inorg. Chem. Comm. 47 (2008) 2240–2242.10.1021/ic701996eSuche in Google Scholar PubMed

Sagnou, M.; Tsoukalas, C.; Triantis, C.; Raptopoulou, C. P.; Terzis, A.; Pirmettis, I.; Pelecanou, M.; Papadopoulos, M.: A new tricarbonyl fac-[M(acac)(isc)(CO)3] complex (M = Re, 99mTc) with acetylacetonate (acac) and isocyanide (isc) in a 2 + 1 combination. Inorg. Chim. Acta 363 (2010) 1649–1653.10.1016/j.ica.2010.01.004Suche in Google Scholar

Triantis, C.; Tsotakos, T.; Tsoukalas, C.; Sagnou, M.; Raptopoulou, C.; Terzis, A.; Psycharis, V.; Pelecanou, M.; Pirmettis, I.; Papadopoulos, M.: Synthesis and characterization of fac-[M(CO)3(P)(OO)] and cis-trans-[M(CO)2(P)(OO)] complexes (M = Re, 99mTc) with acetylacetone and curcumin as OO donor bidentate ligands. Inorg. Chem. 52 (2013) 12995–13003.10.1021/ic401503bSuche in Google Scholar PubMed

Papagiannopoulou, D.; Triantis, C.; Vassileiadis, V.; Raptopoulou, C. P.; Psycharis, V.; Terzis, A.; Pirmettis, I.; Papadopoulous, M. S.: Synthesis, structural characterisation and radiochemistry of di- and tricarbonyl Re(I) and 99mTc(I) complexes with 8-hydroxy quinolone or 8-mercaptoquinoline and triphenylphosphine. Polyhedron 68 (2014) 46–52.10.1016/j.poly.2013.09.039Suche in Google Scholar

Vassileiadis, V.; Triantis, C.; Raptopoulou, C. P.; Psycharis, V.; Pirmettis, I.; Papadopoulous, M. S.; Papagiannopoulou, D.: Synthesis, structural characterisation and radiochemistry of ‘2 + 1’ fac-[99mTc/Re(CO)3(L)(2-mercaptopyridine)] complexes, where L is phosphine or isocyanide. Polyhedron 81 (2014) 511–516.10.1016/j.poly.2014.07.008Suche in Google Scholar

Received: 2017-4-6
Accepted: 2017-8-15
Published Online: 2017-9-13
Published in Print: 2017-11-27

©2017 Amanda-Lee Manicum et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 License.

Artikel in diesem Heft

  1. Cover and Frontmatter
  2. Crystal structure of potassium 1-methyl-1H-1,2,3,4-tetrazole-5-thiolate, C2H3N4SK
  3. Crystal structure of bis(3-(3-ethylureido)-N,N-dimethylpropan-1-aminium) bis (μ3-2-(hydroxymethyl)-2-(oxidomethyl)propane-1,3-bis(olato))-(μ6-oxo)-hexakis(μ2-oxo)-hexaoxo-hexavanadium(V) – dichloromethane (1/1), C27H60Cl2N6O23V6
  4. Crystal structure of bis(μ3-methanolato-κ3O:O:O)-bis(μ2-methanolato-κ2O:O)-dimethanol-bis{6,6′-(1,3-dihydroxyl-2-acetylpropane-1,3-diyl)bis(2-chloro-4-bromophenolato)}tetramanganese(III) C40H40Br4Cl4Mn4O16
  5. Synthesis and crystal structure of tetrakis(μ2-methanolato)-dimethanol-bis(μ2-2-acetyl-1,3-bis(3,5-dibromo-2-oxidophenyl)propane-1,3-bis(olato)-κ5O1,O2,O3:O3,O4,O5)tetramanganese(III), C40H40Br8Mn4O16
  6. Synthesis and crystal structure tetrakis(μ2-methanolato)-dimethanol-bis(μ2-2-acetyl-1,3-bis(3,5-dichloro-2-oxidophenyl)propane-1,3-bis(olato)-κ5O1,O2,O3:O3,O4,O5), tetramanganese(III), C40H40Cl8Mn4O16
  7. Crystal structure of bis{5-methoxy-2-((E)-((4-((E)-1-(methoxyimino)ethyl)phenyl)imino)methyl)phenolato-κ2N,O)}copper(II), C34H34CuN4O6
  8. Crystal structure of (E)-1-(2-hydroxy-3-{[2-hydroxybenzylidene]amino}phenyl)ethan-1-one, C15H13NO3
  9. Crystal structure of bis(μ2-acetato-κ2O:O′)-bis{μ2-4-chloro-2-(8-(4-(diethylamino)-2-oxidophenyl)-3,6-dioxa-2,7-diazaocta-1,7-dien-1-yl)phenolato-κ6O:O,N,N′,O′′:O′′}tricobalt(II), C44H49Cl2Co3N6O12
  10. Crystal structure of bis{μ2-2,4-dichloro-6-(8-(4-(diethylamino)-2-oxidophenyl)-3,6-dioxa-2,7-diazaocta-1,7-dien-1-yl)phenolato-κ5O:O,N,N′,O′}dicobalt(II) acetone solvate, C43H48Br4Co2N6O9
  11. Synthesis and crystal structure of bis(μ2-acetato-κ2O:O′)-bis{μ2-4-chloro-2-(8-(4-(diethylamino)-2-oxidophenyl)-3,6-dioxa-2,7-diazaocta-1,7-dien-1-yl)phenolato-κ6O:O,N,N′,O′:O′}trizinc(II), C44H49Cl2N6O12Zn3
  12. Crystal structure of bis{5-(N,N′-diethylamine)-5′-methoxy -2,2′-[ethylenediyldioxybis(nitrilomethylidyne)]diphenolato}-bis(μ2-acetato-κ2O:O′)trizinc(II), C46H56Zn3N6O14
  13. Crystal structure of tris(cyano-(hydrogen tris(3,5-dimethylpyrazolyl)borate))-iron(III) 4-methoxypyridinium monohydrate, C24H32BN10O2Fe
  14. Synthesis and crystal structure of bis{1-(((4-(1-(hydroxyimino)ethyl)phenyl)imino)methyl)naphthalen-2-olato-κ2O,N}copper(II), C38H30CuN4O4
  15. Crystal structure of (E)-1-(4-{[(E)-2-Hydroxy-1-naphthalenylmethylene] amino}phenyl)ethanone oxime, C19H16N2O2
  16. The pseudosymmetric crystal structure of 2-(2-naphthalenyl)-3-nitro-2H-1-benzopyran, C38H26N2O6
  17. Crystal structure of 2-benzoyl-3-(4-methoxyphenyl)cyclopropane-1,1-dicarbonitrile, C19H14N2O2
  18. N′-(5-ethoxycarbonyl-3,4-dimethyl-pyrrol-2-yl-methylidene)-4-hydroxybenzohydrazide monohydrate, C17H21N3O5
  19. The crystal structure of carbonyl-[4-(2,4-dichlorophenylamino)pent-3-en-2-onato-κ2N,O]-(triphenylphosphine-κP)rhodium(I), RhC30H25Cl2NO2P
  20. Crystal structure of (E)-5-(diethylamino)-2-(((1,1,2-trihydroxyethyl)iminio)methyl)phenolate, C15H24N2O4
  21. Crystal structure of poly[(μ2-1,4-bis((2-ethyl-1H-benzo[d]imidazol-1-yl)methyl)benzene-κ2N:N′)(μ2-isophthalato-κ4O,O′:O′′,O′′′)cadmium(II)], C34H30N4O4Cd
  22. Crystal structure of 5,6-Dihydro-9,10-dimethoxybenzo[g]-1,3-benzodioxolo[5,6-a]chinolizinium 3-(4-hydroxyphenyl)-4-oxo-4H-chromen-7-olate - methanol - water (1/1/1), C36H33NO10
  23. A single crystal study on 2-(methylcarbamoyl)benzoic acid, C9H9NO3
  24. Crystal structure of the salt 1,1′-(ethane-1,2-diyl)bis(1,4-diazabicyclo[2.2.2]octan-1-ium) diperchlorate, C14H28N4(ClO4)2
  25. Crystal structure of 2,5-bis((E)-2-(trifluoromethyl)benzylidene)cyclopentan-1-one, C21H14F6O
  26. Crystal structure of catena-poly[(μ2-benzene-1,4-dicarboxylato-κ2O:O′)-(1-ethyl-6-fluoro-7-(4-methylpiperazin-1-ium-1-yl)-4-oxo-1,4-dihydroquinoline-3-carboxylato-κ2O,O′)zinc(II)] 1.25 hydrate, C25H26.5N3O8.25FZn
  27. Crystal structure of 1-methyl-1,4-diazabicyclo[2.2.2]octan-1-ium poly[aqua-bis(μ2-perchlorato-κ3O,O′:O′′)sodium], C7H17Cl2N2NaO9
  28. Crystal structure of trimethyammonium 2,6-dicarboxyisonicotinate monohydrate, C11H16N2O7
  29. Crystal structure of dodecaguanidinium bis(tetrapropylammonium) heptacarbonate, C43H128N38O21
  30. Crystal structure of poly[tetraaqua-bis(μ6-benzene-1,2,4,5-tetracarboxylato)nickel(II)diyttrium(III)]dihydrate, C20H16NiO22Y2
  31. Halogen bonds and π–π interactions in the crystal structure of 1,3,5-trifluoro-2,4,6-triiodobenzene–N,N-dimethylformamide (1/1), C9H7F3I3NO
  32. Crystal structure of guanidinium tetraethylammonium carbonate dihydrate, C10H30N4O5
  33. The crystal structure of oxonium chlorido-ethylenediaminetetraactetotin(IV) hydrate, C10H17ClN2O10Sn
  34. Crystal structure of 8-((E)-((4-((E)-1-((benzyloxy)imino)ethyl)phenyl)imino)methyl)-7-hydroxy-4-methyl-2H-chromen-2-one, C26H22N2O4
  35. Crystal structure of bis{5-(diethylamino)-2-(((2-oxo-2H-chromen-6-yl)imino)methyl)phenolato-κ2O,N}copper(II), C40H38CuN4O6
  36. Crystal structure of fac-(acetylacetonato-κ2O,O′)tricarbonyl(tri(p-tolyl)phosphine-κP)rhenium(I), C29H28O5PRe
  37. Crystal structure of fac-(acetylacetonato-κ2O,O′)tricarbonyl(benzyldiphenylphosphine-κP)rhenium(I), C27H24O5PRe
  38. Crystal structure of triethylammonium bis{3-(((3-oxidonaphthalen-1-yl)methylene)amino)-2-oxo-2H-chromen-4-olato-κ3O,N,O′}manganese(III), C46H38MnN3O8
  39. Crystal structure of bis(N,N,N-ethyldimethylethanaminium) bis(heptaselenido-κ2Se1,Se7)palladate(II), C12H32N2PdSe14
  40. Crystal structure of bis(4-(1H-pyrazol-5-yl)pyridine-κ2N:N′)-bis(2-(2-((2,6-difluorophenyl)amino)phenyl)acetate-κO)cadmium(II), C44H34N8CdCl4O4
  41. Crystal structure of 4,4′-(1,4-phenylene)bis(pyridin-1-ium) catena-poly[diaqua-bis(μ2-3′,5′-dicarboxy-[1,1′-biphenyl]-2,5-dicarboxylato-κ2O:O′] dihydrate, C48H42O22N2Ca
  42. The crystal structure of (S)-2-benzylsuccinic acid, C11H12O4
  43. Crystal structure of poly[aqua-(μ3-4-(pyridin-4-yl)isophthalato-κ4O,O′:O′′:O′′′)-(μ2-5-carboxy-2-(pyridin-4-yl)benzoato-κ2O:O′)yttrium(III)], C26H17N2O9Y
  44. Crystal structure of ethyl 1-(3,4-dimethylphenyl)-5-methyl-1H-1,2,3-triazole-4-carboxylate, C14H17N3O2
  45. Crystal structure of tetrakis(methanol-κO)-bis{μ2-3-((4-methoxy-2-oxidobenzylidene)amino)-2-oxo-2H-chromen-4-olate-κ4O,N;O′:O′}dizinc(II), C38H38Zn2N2O14
  46. Crystal structure of bromido(4,4′-dimethoxy-2,2′-bipyridine-κ2N,N′)(isopropyl(diphenyl)phosphane-κP)copper(I), C27H29BrCuN2O2P
  47. Crystal structure of bis(4,4,5,5-tetramethyl-1,3,2-dioxaborolane)-9,9-dioctylfluorene, C41H64B2O4
  48. Crystal structure of 11-oxo-2,3,6,7-tetrahydro-1H,5H,11H-pyrano[2,3-f]pyrido[3,2,1-ij]quinoline-10-carbaldehyde - a julolidine derivative, C16H15NO3
  49. Crystal structure of 1,3-dimethyl-5,5-dibenzylbarbituric acid, C20H20N2O3
  50. Crystal structure of bis(N,N,N-trimethylethanaminium) poly[bis(μ2-heptaselenido-κ2Se1,Se7)palladate(II)], C10H28N2PdSe14
  51. Crystal structure of 1-{4-[(5-Chloro-2-hydroxy-benzylidene)amino]phenyl} ethanone O-ethyl-oxime, C17H17ClN2O2
  52. The crystal structure of methyl N-(4-bromophenyl)carbamate, C8H8BrNO2
  53. Synthesis and crystal structure of 1-{4-[(2-hydroxy-benzylidene)amino]phenyl}ethanone oxime, C15H14N2O2
  54. Crystal structure of 1,1′-butanebis(3-methyl-1H-imidazol-3-ium)bis(hexafluorophosphate), C12H20F12N4P2
  55. (E)-N-benzylidene-3-(benzylthio)-5-p-tolyl-4H-1,2,4-triazol-4-amine, C23H20N4S
  56. Crystal structure of ethyl 5-methyl-1-(pyridin-3-yl)-1H-1,2,3-triazole-4-carboxylate, C11H12N4O2
  57. Crystal structure of 5,5-difluoro-10-(4-fluorophenyl)-1,3,7,9-tetramethyl-5H-4l4,5l4-dipyrrolo[1,2-c:2′,1′-f][1,3,2]diazaborinine - a Z′ = 3 structure, C19H18B2F3N2
  58. The crystal structure of the Matrine derivative: 12-(1H-indol-1-yl)dodecahydro-1H,5H,10H-dipyrido[2,1-f:3′,2′,1′-ij][1,6]naphthyridin-10-one hydrate, C23H29N3O
  59. The crystal structure of tris(μ2-1,3-bis(4,4,4-trifluoro-3-oxido-1-(oxo)but-2-en-1-yl)phenyl-κ4O,O′:O′′,O′′′)-bis(1,2-dimethoxyethane-κ2O,O′)dilutetium(III), C50H38F18Lu2O16
  60. The crystal structure of (Z)-2-(3-(2-(4-chlorobenzoyl)hydrazono)-2-oxoindolin-1-yl) acetic acid, C17H12ClN3O4
  61. Synthesis and crystal structure of trans-tetraqua-bis(2-(((7-hydroxy-3-(4-hydroxy-3-sulfonatophenyl)-4-oxo-4H-chromen-8-yl)methyl)ammonio)acetato-κO)cobalt(II) hexahydrate, C36H48CoN2O28S2
  62. The crystal structure of N,N-dimethyl-2,6-di-p-tolylpyrimidin-4-amine, C20H21N3
  63. The crystal structure (E)-4-methyl-N′-(2-nitrobenzylidene)benzenesulfonohydrazide, C14H13N3O4S
  64. Crystal structure of catena-poly[(μ2-1,3-bis(benzimidazol-1-yl)propane κ2N:N′)-(μ2-5-methoxyisophthalato-κ2O:O′)zinc(II)] hydrate, C26H24ZnN4O6
  65. The crystal structure of (E)-N′-(quinolin-2-ylmethylene)furan-2-carbohydrazide monohydrate, C15H13N3O3
  66. Crystal structure of 2,8-diphenyl-3,7,9-trioxa-1-azaspiro[4.5]dec-1-ene, C18H17N1O3
  67. Crystal structure of diethyl 2-(4-chlorophenyl)-1,3-dioxane-5,5-dicarboxylate, C16H19ClO6
  68. Crystal structure of 1-(carboxymethyl)-1H-benzo[d][1,2,3]triazole 3-oxide, C8H7N3O3
  69. Crystal structure of (acetylacetonato-κ2O,O′)-(2-amino-6-chlorobenzoato-κO)-oxido(1,10-phenanthroline-κ2N,N′)vanadium(IV) – trichloromethane (1/1)
  70. Crystal structure of (1E,4E)-1,5-bis(4-chlorophenyl)penta-1,4-dien-3-one, C17H12Cl2O
  71. The crystal structure of trans-dibromido-bis(pyridine-κN)platinum(II), C10H10Br2N2Pt
Heruntergeladen am 25.1.2026 von https://www.degruyterbrill.com/document/doi/10.1515/ncrs-2017-0095/html
Button zum nach oben scrollen