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1.
Rodica Olar Michaela Badea E. Cristurean C. Parnau D. Marinescu 《Journal of Thermal Analysis and Calorimetry》2006,84(1):53-58
The complexes of the type M(HDMBG)2(CH3COO)2·nH2O ((1)
M:Mn, n=1.5; (2)
M:Ni, n=0; (3)
M:Cu, n=2; (4)
M:Zn, n=2; DMBG: N,N-dimethylbiguanide)
present in vitro antimicrobial activity. The thermal analysis has evidenced
the thermal intervals of stability and also the thermodynamics effects that
accompany them. The different nature of the ligands generates a different
thermal behaviour for the complexes. The thermal transformations are complex
processes according to TG and DTG curves including dehydration, oxidative
condensation of –C=N– units as well as thermolysis processes.
The final products of decomposition are the most stable metal oxides. 相似文献
2.
I. G. Fomina G. G. Aleksandrov Zh. V. Dobrokhotova O. Yu. Proshenkina M. A. Kiskin Yu. A. Velikodnyi V. N. Ikorskii V. M. Novotortsev I. L. Eremenko 《Russian Chemical Bulletin》2006,55(11):1909-1919
A coordination polymer of the general formula [Co(OOCCMe3)2]n (2) was prepared by mild thermolysis of the coordination polymer of variable composition [(HOOCCMe3)xCo(OH)n(OOCCMe3)2−n
]m, the dinuclear cobalt complex Co2(μ-H2O)(OOCCMe3)4(HOOCCMe3)4, the tetranuclear cobalt cluster Co4(μ3-OH)2(OOCCMe3)6(HOEt)6, and the hexanuclear cluster [Co6(μ4-O)2(μn-OOCCMe3)10(C4H8O)3(H2O)]·1.5(C4H8O) (7) in organic solvents. In the crystal, the polymer has a chain structure. Unlike thermolysis of cobalt pivalates, thermolysis
of the dinuclear complex Ni2(μ-H2O)(OOCCMe3)4(HOOCCMe3)4 gave rise to the hexanuclear complex Ni6(μ2-OOCCMe3)6(μ3-OOCCMe3)6 (3). The magnetic properties of compound 2 are substantially different from those of 3. Compound 2 undergoes the magnetic phase transition into the ordered state at T
c = 3.4 K (H = 1 Oe), whereas compound 3 exhibits antiferromagnetic properties. Solid-state decomposition of polymeric cobalt carboxylate 2 (below 350 °C) afforded the octanuclear cluster Co8(μ4-O)2(μ2-OOCCMe3)6(μ3-OOCCMe3)6 (9) as the major product, which sublimes without decomposition. Decomposition of 3 gave nickel oxide as the final product. Pivalates 2 and 3 reacted with 2,3-lutidine in acetonitrile at 80 °C to form the isostructural dinuclear complexes (2,3-Me2C5H3N)2M2(μ-OOCCMe3)4 (M = Co or Ni). The structures of compounds 3 and 7 were established by X-ray diffraction. The structure of polymer 2 was determined by powder X-ray diffraction analysis.
Dedicated to Academician O. M. Nefedov on the occasion of his 75th birthday.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 11, pp. 1841–1850, November, 2006. 相似文献
3.
Triethylamine reacts with aqueous zinc acetate and the product of its thermolysis in the presence of benzoic acid to yield
the complexes [Zn7(μ4-O)(μ-OOCMe)10][η-OC(Me)OHNEt3]2 (1) and [Zn2(μOOCPh)4][η-OC(Me)OHNEt3]2 (2), respectively. The reactions of 1 and 2 with 3,5-dimethylpyrazole at room temperature in benzene yield pyrazolate-bridged binuclear complexes Zn2(μdmpz)2(Hdmpz)2(OOCR)2 (R = Me (3), Ph (4)). The structures of complexes 1–4 have been determined by X-ray crystallography. 相似文献
4.
Zuzana Vasková Zdenka Padělková Milan Mazur Dušan Valigura Jan Moncol 《Transition Metal Chemistry》2011,36(8):883-889
The synthesis, spectral characterization and crystal structures of two nitrobenzoatocopper(II) complexes, namely [Cu(2-O2Nbz)2(pca)2(H2O)2] (1) and [Cu(3,5-(O2N)2bz)2(pca)2(H2O)2] (2) (where 2-O2Nbz = 2-nitrobenzoate, 3,5-(O2N)2bz = 3,5-dinitrobenzoate, pca = pyrazinecarboxamide), are reported. Complexes 1 and 2 consist of centrosymmetric molecules with the Cu(II) atom monodentately coordinated by a pair of anionic 2-nitrobenzoato
(1) or 3,5-dinitrobenzoato (2) ligands and a pair of pyrazinecarboxamide ligands, forming a nearly tetragonal basal plane, and by a pair of water ligands
that complete the tetragonal–bipyramidal coordination polyhedron. The molecules of both complexes are linked by N–H⋯O and
O–H⋯O hydrogen bonds and lie in planes, which have different orientations depending on the space group. Similar experiments
with 3-nitrobenzoic acid resulted in the isolation of the hydrolysis product [Cu(pyzCOO)2]
n
(3) (pyzCOO = pyrazinecarboxylate). The known crystal structure of complex 3 has been re-determined at low temperature with significantly higher precision. The crystal packing and C–H⋯O/C–H⋯N hydrogen
bonds are discussed. 相似文献
5.
The complexes K2[PtCln] (n = 4 or 6) react with pyrazoles 3,5-MeRpzH (R = H or Me) in 0.1 M HCl at 20–25 °C to form the isomerically pure cis-[PtCln(3,5-MeRpzH)2] complexes (n = 2 or 4) (1a,b and 3a,b), whereas a decrease in the acidity of the medium leads to a substantial decrease in selectivity of the reaction. Thermal
isomerization of complexes 1a,b and 3a,b both in solution (MeNO2) and in the solid state affords the trans-[PtCln(3,5-MeRpzH)2] complexes (n = 2 or 4) (2a,b and 4a, b). Platinum(II) complexes 1a,b and 2a,b were also prepared by selective reduction of genetically related PtIV compounds (3a,b and 4a,b) with the phosphorus ylide Ph3P=CHCO2Me in chloroform. Platinum(IV) complexes (3a,b and 4a,b) were synthesized by oxidation of the corresponding PtII complexes (1a,b and 2a,b) with molecular chlorine. X-ray diffraction study demonstrated that coordination of 3(5)-MepzH to PtIV in complex 4a stabilizes the sterically least hindered tautomer in the solid state.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2, pp. 242—249, February, 2006. 相似文献
6.
Mihaela Badea Rodica Olar Dana Marinescu E. Segal A. Rotaru 《Journal of Thermal Analysis and Calorimetry》2007,88(2):317-321
A series of new complexes with mixed ligands
of the type M(4,4’-dipy)(C3H3O2)2(H2O)y ((1) M=Mn, y=2; (2) M=Ni, y=2; 4,4’-dipy: 4,4’-dipyridyl and C3H3O2 is acrylate anion) and respectively M2(4,4’-dipy)(C3H3O2)4(H2O)y
((3) M=Cu, y=0; (4) M=Zn, y=1). The
modification evidenced in IR spectra was correlated with the presence of acrylate
ion as unidentate in the case of complex (1)
and as bidentate for others complexes. The electronic reflectance spectra
showed the d–d
transition for complex (1) and (2) characteristic for the octahedral surrounding while
the spectrum for complex (3) have the characteristic
pattern for square-pyramidal stereochemistry. The thermal behaviour steps
were investigated. The thermal transformations are complex processes according
to TG and DTG curves including dehydration, acrylate ion oxidative degradation
and thermolysis process of aromatic amine. The final products of decomposition
are the most stable metal oxides. 相似文献
7.
Two bis(bipyridine) polymeric metal nitrate complexes
with 4,4’-bipyridine of simple formula like [M(bipy)2](NO3)2⋅xH2O (where M=Co, Ni and Cu; x=4, 2 and 0, respectively) have been prepared and
characterized. Their thermal decomposition has been undertaken using simultaneous
TG-DTG-DTA and DSC in nitrogen atmosphere and non-isothermal TG in air atmosphere.
Isothermal TG has been performed at decomposition temperature range of the
complexes to evaluate the kinetics of decomposition by applying model-fitting
as well as isoconversional method. Possible mechanistic pathways have also
been proposed for the thermolysis. Ignition delay measurements have been carried
out to investigate the response of these complexes under the condition of
rapid heating. 相似文献
8.
New divalent transition metal 3,5-pyrazoledicarboxylate
hydrates of empirical formula Mpz(COO)2(H2O)2,
where M=Mn, Co, Ni, Cu, Zn and Cd (pz(COO)2=3,5-pyrazoledicarboxylate),
metal hydrazine complexes of the type Mpz(COO)2N2H4
where M=Co, Zn or Cd and Mpz(COO)2nN2H4·H2O,
where n=1 for M=Ni
and n=0.5 for M=Cu
have been prepared and characterized by physico-chemical methods. Electronic
spectroscopic data suggest that Co and Ni complexes adopt an octahedral geometry.
The IR spectra confirm the presence of unidentate carboxylate anion (Δν=νasy(COO–)–νsym(COO–)>215
cm–1) in all the complexes and bidentate
bridging hydrazine (νN–N=985–950 cm–1)
in the metal hydrazine complexes. Both metal carboxylate and metal hydrazine
carboxylate complexes undergo endothermic dehydration and/or dehydrazination
followed by exothermic decomposition of organic moiety to give the respective
metal oxides as the end products except manganese pyrazoledicarboxylate hydrate,
which leaves manganese carbonate. X-ray powder diffraction patterns reveal
that the metal carboxylate hydrates are isomorphous as are those of metal
hydrazine complexes of cobalt, zinc and cadmium. 相似文献
9.
Juribašić M Bellotto L Traldi P Tušek-Božić L 《Journal of the American Society for Mass Spectrometry》2011,22(10):1815-1825
The mass spectrometric behavior of palladium(II) halide complexes of three types of quinolinylaminophosphonates, diethyl and
dibutyl esters of [α-anilino-(quinolin-2-yl)methyl]phosphonic (L1, L2), [α-anilino-(quinolin-3-yl)methyl]phosphonic (L3, L4), and [α-(quinolin-3-ylamino)-N-benzyl]phosphonic acid (L5, L6), was investigated under positive ion electrospray ionization conditions. Each type of ligand forms complexes with different
metal–ligand interactions. Mononuclear dihalide adducts cis-[Pd(L1/L2)X2] (1–4) and trans-[Pd(L3/L4)2X2] (5–8) as well as dinuclear tetrahalide complexes [Pd2(L5/L6)3X4] (9–12) (X = Cl, Br) are formed by metal bonding either through the quinoline or both the quinoline and amino nitrogen atoms. The
sodiated molecule [M + Na]+ is observed in the mass spectra of all the complexes, and its abundance as well as the fragmentation pathway depend on the
type of the complex. In the cis complexes (1–4) the initial decomposition goes under two fragmentation routes: those in which the sodium molecular adduct sequentially loses
halides HX/NaX and those in which this loss is in the competition with the loss of dialkyl phosphite. The predominant pathways
for decomposition of trans dihalide (5–8) and tetrahalide (9–12) complexes include three competitive reactions; the loss of halides, dialkyl phosphites and the intact phosphonate ligand
molecule and its fragments formed by ester dissociation or complete loss of the phosphonate ester moiety. A series of acetonitrile
adducts and cluster ions derived from dimolecular clusters [2M + Na]+ were also detected. The most important fragmentation patterns are rationalized and supported by the MS
n
studies. 相似文献
10.
A. L. Emelina Zh. V. Dobrokhotova A. A. Sinelshchikova Yu. A. Velikodnyi I. G. Fomina P. S. Koroteev V. M. Novotortsev I. L. Eremenko 《Russian Journal of Inorganic Chemistry》2010,55(11):1754-1761
Kinetic analysis of the thermolysis of samarium pivalate [Sm2(μ2-OOCCMe3)4(OOCCMe3)2(HOOCCMe3)6] · HOOCCMe3 (1) was carried out (the input data were differential scanning calorimetry (DSC) and thermogravimetry data), and a mathematic
model of the process was developed that allowed us to optimize (by calculation) the conditions for formation of {Sm(OOCCMe3)3}
n
(2) samarium tris-pivalate via thermal decomposition of complex 1. The results of the thermal study of samarium and gadolinium tris-pivalates in the temperature range of −50…+50°C are reported.
Specific anomalies were found in the DSC curves and heat capacity versus temperature curves in the temperature range of 0–50°C. 相似文献
11.
New Polydentate Trimethylsilyl Chalcogenide Reagents for the Assembly of Polyferrocenyl Architectures
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Mahmood Azizpoor Fard Bahareh Khalili Najafabadi Mahdi Hesari Prof. Dr. Mark S. Workentin Prof. Dr. John F. Corrigan 《Chemistry (Weinheim an der Bergstrasse, Germany)》2014,20(23):7037-7047
A series of polychalcogenotrimethylsilane complexes Ar(CH2ESiMe3)n, (Ar=aryl; E=S, Se; n=2, 3, and 4) can be prepared from the corresponding polyorganobromide and M[ESiMe3] (M=Na, Li). These represent the first examples of the incorporation of such a large number of reactive ?ESiMe3 moieties onto an organic molecular framework. They are shown to be convenient reagents for the preparation of the polyferrocenylseleno‐ and thioesters from ferrocenoyl chloride. The synthesis, structures, and spectroscopic properties of the new silyl chalcogen complexes 1,4‐(Me3SiECH2)2(C6Me4) (E=S, 1 ; E=Se, 2 ), 1,3,5‐(Me3SiECH2)3(C6Me3) (E=S, 3 ; E=Se, 4 ) and 1,2,4,5‐(Me3SiECH2)4(C6H2) (E=S, 5 ; E=Se, 6 ) and the polyferrocenyl chalcogenoesters [1,4‐{FcC(O)ECH2}2(C6Me4)] (E=S, 7 ; E=Se, 8 ), [1,3,5‐{FcC(O)ECH2}3(C6Me3)] (E=S, 9 ; E=Se, 10 ) and [1,2,4,5‐{FcC(O)ECH2}4(C6H2)] (E=S, 11 illustrated; E=Se, 12 ) are reported. The new polysilylated reagents and polyferrocenyl chalcogenoesters have been characterized by multinuclear NMR spectroscopy (1H, 13C, 77Se), electrospray ionization mass spectrometry and, for complexes 1 , 2 , 3 , 4 , 7 , 8 , and 11 , single‐crystal X‐ray diffraction. The cyclic voltammograms of complexes 7 – 11 are presented. 相似文献
12.
Limin Han Guangbin Zhang Ning Zhu Ruijun Xie Quanling Suo Meihua Luo Linhong Weng 《Journal of Cluster Science》2010,21(4):789-801
Two novel bimetallic complexes, [Cr(CO)3(η
6-C6H5)–C≡C–C6H4–Fc] (Fc = C5H5FeC5H4] (1) and [Cr(CO)3(η
6-C6H5)–C ≡ C–Fc–C(CH3)2–Fc] (3), were synthesized by the Sonogashira coupling reaction. By using of (1) and (3) as ligands to react with Co2(CO)8, two others novel polymetallic complexes, [Cr(CO)3(η
6-C6H5){Co2(CO)6-η
2-μ
2-C≡C–}–C6H4–Fc] (2) and [Cr(CO)3(η
6-C6H5){Co2(CO)6-η
2-μ
2-C≡C–}Fc–C(CH3)2–Fc] (4) were obtained. Four carbonyl complexes were characterized by elemental analysis, FT-IR, NMR and MS. The molecular structures
of complexes (1), (2) and (4) were determined by single crystal X-ray diffraction. The interactions among the ferrocenyl,
Cr(CO)3 and Co2(CO)6-η
2-μ
2-C≡C– units were investigated by cyclic voltammetry. 相似文献
13.
K. Ramalingam R. Thiruneelakandan G. Bocelli L. Righi 《Transition Metal Chemistry》2012,37(3):265-270
The complexes trans-[Ni(4-MP)2(NCS)2]·MeCN (1) and trans-[Ni(3-MP)2(NCS)2] (2) (4-MP = tri(4-methylphenyl)phosphine, 3-MP = tri(3-methylphenyl)phosphine) were prepared and characterized by IR, UV–visible,
NMR spectra, CV, TGA and single crystal X-ray crystallography. Both the complexes have planar geometry and are diamagnetic.
The Ni–P distances in both complexes are relatively short as a result of strong back donation from nickel to phosphorus. The
phenyl rings in the 3-MP analogue (2) show increased pitching with reference to the plane formed by the ipso carbons due to increased steric effects. For complex
(2), the N–Ni–N and P–Ni–P angles are significantly lower than the almost linear N–Ni–N and N–Ni–P angles observed for both
complex (1) and trans-[Ni(PPh3)2(NCS)2]. This observation indicates that the 3-methylphosphine ligand forces complex (2) to distort towards a tetrahedral geometry. IR spectra of both complexes show strong bands around 2,090 cm−1 due to N-coordinated thiocyanate, while the electronic spectra contain d–d transitions around 452 nm. Cyclic voltammograms
show that the irreversible one-electron reduction potentials increase in the following order: trans- [Ni(PPh3)2(NCS)2] < trans- [Ni(3-MP)2(NCS)2] < trans-[Ni(4-MP)2(NCS)2], revealing the electron releasing effect of the methyl groups. The planar complexes exhibit interallogony in coordinating
solvents. 相似文献
14.
M. A. Il’in E. V. Kabin V. A. Emel’yanov I. A. Baidina V. A. Vorob’yov 《Journal of Structural Chemistry》2009,50(2):328-334
Methods for the synthesis of trans-diammino complexes [RuNO(NH3)2(NO2)2(OH)] (I) and [RuNO(NH3)2(H2O)(NO3)2](NO3)·H2O (II) are suggested. The compounds were studied by IR spectroscopy and X-ray phase and X-ray structural analyses. Crystal data:
space group P-1; a = 6.2328(2) ?, b = 11.0488(3) ?, c = 11.0981(4) ?, α = 71.942(1)°, β = 83.291(1)°, γ = 86.877(1)° (I); space group P21; a = 6.6290(2) ?, b = 13.4389(5) ?, c = 7.0180(2) ?, β 114.281(1)° (II). Complex II readily lost some part of crystal water on storage in open air.
Original Russian Text Copyright ? 2009 by M. A. Il’in, E. V. Kabin, V. A. Emel’yanov, I. A. Baidina, and V. A. Vorob’yov
__________
Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 2, pp. 341–348, March–April, 2009. 相似文献
15.
I. G. Fomina Zh. V. Dobrokhotova M. A. Kiskin G. G. Aleksandrov O. Yu. Proshenkina A. L. Emelina V. N. Ikorskii V. M. Novotortsev I. L. Eremenko 《Russian Chemical Bulletin》2007,56(9):1712-1721
The solid-state thermal decomposition of the tetrabridged dinuclear MnII, FeII, CoII, NiII, and CuII pivalate complexes with apical α-substituted pyridine ligands containing different substituents (2,3-dimethylpyridine or
quinoline) was studied by differential scanning calorimetry and thermogravimetry. The decomposition of the CoII complexes is accompanied by the aggregation to form the volatile octanuclear complex Co8(μ4-O)2(μn-OOCCMe3)12, where n = 2 or 3, whereas the thermolysis of the MnII, FeII, NiII, and CuII complexes is accompanied by the degradation of the starting compounds, the phase composition of the decomposition products
being substantially dependent on the nature of metal and the apical organic ligand.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 1650–1659, September, 2007. 相似文献
16.
S. A. Martynova K. V. Yusenko I. V. Korolkov S. A. Gromilov 《Russian Journal of Coordination Chemistry》2007,33(7):530-534
The double complex salts [Ru(NH3)5Cl][PtCl6] (I) and [Ru(NH3)5Cl]2[PtCl6]Cl2 (II) were synthesized and studied by X-ray diffraction. They were found to be isostructural to the previously synthesized [Rh(NH3)5Cl][OsCl6] and [Ir(NH3)5Cl]2[PtCl6]Cl2. The thermolysis of the complexes in the atmosphere of hydrogen and helium was studied by the powder X-ray diffraction analysis.
The product of the salt I thermolysis is a single-phase solid solution Ru0.5Pt0.5 (a = 3.857(3) ?), the thermolysis of salt II results in a double-phase metallic powder.
Original Russian Text ? S.A. Martynova, K.V. Yusenko, I.V. Korol’kov, S.A. Gromilov, 2007, published in Koordinatsionnaya
Khimiya, 2007, Vol. 33, No. 7, pp. 541–545. 相似文献
17.
Brajagopal Samanta Joy Chakraborty C. R. Choudhury S. K. Dey D. K. Dey S. R. Batten P. Jensen Glenn P. A. Yap Samiran Mitra 《Structural chemistry》2007,18(1):33-41
We have reported herein the synthesis of three new Cu(II) complexes of tri- and tetradentate Schiff base ligands containing
N3 or N4 donor set along with terminal NNN− or SCN− ligands: [L1Cu(NCS)]ClO4 (1), [L2Cu(NCS)2] (2) and [L3Cu(NNN)]ClO4 (3) [L1 = NC5H4C(CH3)=N(CH2)3N=C(CH3)C5H4N, L2= Me2N–(CH2)3–N=C(CH3)C5H4N and L3 = NC5H4CH=N–(CH2)4–N=CHC5H4N]. The complexes have been systematically characterised by elemental, spectroscopic and electrochemical techniques. Antimicrobial
activities of the Schiff base ligands and their metal complexes have been studied using the disc diffusion method on the strains
of Candida tropicalis and Bacillus megaterium. Structures of all the complexes have been unequivocally established from single crystal X-ray diffraction analyses that
show the monomeric units containing a five-coordinated copper center in highly distorted square pyramidal geometry with thiocyanate
or azide anion coordinated as terminal ligand. The complexes 1 and 3 crystallise in monoclinic (P21/c) and 2 in triclinic (P-1) space group, respectively. 相似文献
18.
Germán Gascón Marisol C. Ortega José D. Suárez Alvaro J. Pardey Clementina Longo 《Reaction Kinetics and Catalysis Letters》2008,94(1):85-89
Rhodium(I) complexes, cis-[Rh(CO)2(amine)2](PF6) (amine = 4-picoline, 3-picoline, 2-picoline, pyridine, 3,5-lutidine or 2,6-lutidine) dissolved in an aqueous solution of
tetrabutylammonium hydrogensulfate (N(C4H9)4HSO4), catalyze the water-gas shift reaction (WGSR). The role of the coordinated amine on the catalytic activity was examined. 相似文献
19.
This paper reports the investigation of the thermal
stability of a series of new complexes with azo and azomethinic chromophores
of the type [Er(HL)2(H2O)2](HO);
((B) H2L: o,o’-dihydroxy-azobenzene (A);
(D) H2L: N-(2-hydroxy-1-naphthalidene)aminophenol
(C); (F)
H2L: N-(2-hydroxy-1-naphthalidene)anthranilic acid
(E)). The complexes thermal behaviour steps
were investigated and comparatively presented with those of corresponding
ligand. The thermal transformations are complex processes according to TG
and DTG curves including phenol elimination, oxidative condensation and thermolysis
processes. The final product of complexes decomposition is Er2O3. 相似文献
20.
The ortho-metalated complex [Pd(x){κ
2
(C,N)-[C6H4CH2NRR′ (Y)}] (2a–4a and 2b–3b) was prepared by refluxing in benzene equimolecular amounts of Pd(OAc)2 and secondary benzylamine [a, EtNHCH2Ph; b, t-BuNHCH2Ph followed by addition of excess NaCl. The reaction of the complexes [Pd(x){κ
2
(C,N)-[C6H4CH2NRR′ (Y)}] (2a–4a and 2b–3b) with a stoichiometric amount of Ph3P=C(H)COC6H4-4-Z (Z = Br, Ph) (ZBPPY) (1:1 molar ratio), in THF at low temperature, gives the cationic derivatives [Pd(OC(Z-4-C6H4C=CHPPh3){κ
2
(C,N)-[C6H4CH2NRR′(Y)}] (5a–9a, 4b–6b, and 4b′–6b′), in which the ylide ligand is O-coordinated to the Pd(II) center and trans to the ortho-metalated C(6)H(4) group, in an “end-on
carbonyl”. Ortho-metallation, ylide O-coordination, and C-coordination in complexes (5a–9a, 4b–6b, and 4b′–6b′) were characterized by elemental analysis as well as various spectroscopic techniques. 相似文献