• Title/Summary/Keyword: 1,2-$(P^iPr_2)_2-1,2-C_2B_{10}H_{10}$

Search Result 10, Processing Time 0.031 seconds

Two New closo- or nido-Carborane Diphosphine Complexes: Synthesis, Characterization and Crystal Structures

  • Kong, Lingqian;Zhang, Daopeng;Su, Fangfang;Li, Dacheng;Dou, Jianmin
    • Bulletin of the Korean Chemical Society
    • /
    • v.32 no.7
    • /
    • pp.2249-2252
    • /
    • 2011
  • Two new carborane complexes containing closo- or nido-carborane diphosphine ligands with the formula: complex $[Hg(7,8-(PPh_2)_2-7,8-C_2B_9H_{10})_2]$ $CH_2Cl_2$ (1) and $[Ag_2({\mu}-Cl)_2(1,2-(P^iPr_2)_2-1,2-C_2B_{10}H_{10})_2]$ (2) have been synthesized and characterized by elemental analysis, 1H and 13C NMR spectroscopy and X-ray structure determination. The X-ray structure analyses revealed that the carborane diphosphine ligand was degraded from closo-1,2-$(PPh_2)_2-1,2-C_2B_{10}H_{10}$ to nido-[$7,8-(PPh_2)_2-7,8-C_2B_9H_{10}]^-$ in complex 1, while the closo nature of the starting ligand $1,2-(P^iPr_2)_2-1,2-C_2B_{10}H_{10}$ was retained in complex 2. In either of the two complexes, the carborane diphosphine ligand was coordinated bidentately to the Hg(II) or Ag(I) center through its two phosphorus atoms, therefore forming a five-member cheating ring between the carborane ligand and the metal center. The coordination geometry of the metal atom is distorted tetrahedron formed by $P_4$ unit in complex 1 and $P_2Cl_2$ unit in complex 2, respectively.

Structure of $[cis-ReCl_4(py)(N-C_6H_3-2,6-i-Pr_2)\cdot(NH_2-C_6H_3-2,6-i-Pr_2)]$ (py=pyridine) ($[cis-ReCl_4(py)(N-C_6H_3-2,6-i-Pr_2)\cdot(NH_2-C_6H_3-2,6-i-Pr_2)]$ 착물의 구조(py=pyridine))

  • 최남선;이순원
    • Korean Journal of Crystallography
    • /
    • v.10 no.2
    • /
    • pp.105-109
    • /
    • 1999
  • Ar 기류 하에서 Re(N-C6H3-2,6-i-Pr2)2Cl3(py) (1)과 propionaldehyde (C2H5CHO)가 반응하여 생성된 혼합물에서, [cis-ReCl4(py)(N-C6H3-2,6-i-Pr2)·(NH2-C6H3-2,6-i-Pr2)] (2)가 분리되었다. 이 화합물의 구조가 X-ray 회절법으로 규명되었다. 착물 2의 결정학 자료: 단사정계 공간군 P21/n, a=11.555(1) Å, b=27.066(3) Å, c=11.881(1) Å, β=117.991(8)°, Z=4, R(wR2)=0.0332(0.0851.

  • PDF

Formation of Mo(NAr)(PMe₃)₂Cl₃and Mo₂(PMe₃)₄Cl₄from Reduction of Mo(NAr)₂Cl₂(DME) with Mg in the Presence of PMe₃[Ar=2,6-diisopropylphenyl]

  • 정건수;박병규;Lee, Soon W.
    • Bulletin of the Korean Chemical Society
    • /
    • v.18 no.2
    • /
    • pp.213-217
    • /
    • 1997
  • Magnesium reduction of Mo(N-C6H3-2,6-i-Pr2)2Cl2(DME) in the presence of trimethylphosphine led to a mixture of Mo(N-C6H3-2,6-i-Pr2)(PMe3)2Cl3, 1, and Mo2(PMe3)4Cl4, 2. In solution 1 is slowly air-oxidized to Mo(N-2,6-i-Pr2-C6H3)(OPMe3)(PMe3)Cl3, 3. 1 is chemically inert to carbon nucleophiles (ZnMe2, ZnEt2, AlMe3, AlEt3, LiCp, NaCp, TlCp, NaCp*, MeMgBr, EtMgBr), oxygen nucleophiles (LiOEt, LiO-i-Pr, LiOPh, LiOSPh), and hydrides (LiBEt3H, LiBEt3D). Crystal data for 1: orthorhombic space group P212121, a=11.312(3) Å, b=11.908(3) Å, c=19.381(6) Å, Z=4, R(wR2)=0.0463 (0.1067). Crystal data for 2: monoclinic space group Cc, a=18.384(3) Å, b=9.181(2) Å, c=19.118(3) Å, b=124.98(1)°, Z=4, R(wR2)=0.0228 (0.0568). Crystal data for 3: orthorhombic space group P212121, a=11.464(1) Å, b=14.081(2) Å, c=16.614(3) Å, Z=4, R(wR2)=0.0394 (0.0923).

C-H…H-Fe Dihydrogen Bonding: Synthesis and Structure of $trans-[FeH(NCS(i-Pr)-S)(dppe)_2]I$ $(dppe=Ph_2PCH_2Ch_2PPh_2)$ (C-H…H-Fe Dihydrogen 결합: $trans-[FeH(NCS(i-Pr)-S)(dppe)_2]I$ 착물의 합성 및 구조)

  • 이지화;이순원
    • Korean Journal of Crystallography
    • /
    • v.11 no.1
    • /
    • pp.10-15
    • /
    • 2000
  • Compound trans-[FeH(NCS(i-Pr)-S)(dppe)₂](1) reacted with isopropyl iodide (i-PrI) to give an Fe(II)-organic isothiocyanide complex, trans-[FeH(NCS(i-Pr)-S)(dppe)₂]I (2). Compound 2 was structurally characterized, in which the hydride ligand appears to be involved in the "dihydrogen" bonding, M-H…H-C. Crystallographic data for 2: monoclinic space group P2₁/n, a=13.490(2)Å, b=17.269(3)Å, c=21.384(3)Å, β=90.682(7)°, Z=4, R(wR₂)=0.0348(0.0894).

  • PDF

Preparation, Structure, and Property of Re(Nar)$(PR_3)_2Cl_3$, $(PR_3 = PMe_3, PEt_3, P(Ome)_3;Ar = C_6H_5, 2,6-i-Pr_2-C_6H_3)$

  • 박병규;최남선;이순우
    • Bulletin of the Korean Chemical Society
    • /
    • v.20 no.3
    • /
    • pp.314-320
    • /
    • 1999
  • Several bisphosphine- and bisphosphite-substituted Re-imido complexes have been prepared from Re(NPh)(PPh3)2Cl3, 1, and Re(N-C6H3-i-Pr2)2Cl3(py), 4. Compound 1 reacted with trimethyl phosphate (P(OMe)3) to give a mixture of two isomers,mer,trans-Re(NPh)(P(OMe)3)2Cl3, 2, and fac,cis-Re(NPh)(P(OMe)3)2Cl3, 2a. In this reaction, the mer,trans-isomer is a major product. Complex 1 also reacted with triethylphosphine (PEt3) to exclusively give mertrans-Re(NPh)(PEt3)2Cl3, 3. Compound 4 reacted with trimethylphosphine (PMe3) to give mer,trans-Re(N-C6H3-i-Pr2)(PMe3)2Cl3, 5, which was converted to mer-Re(N-C6H3-i-Pr2)(PMe)(OPMe3)Cl3, 6, on exposure to air. Crystallographic data for 2: monoclinic space group P21/n, a = 8.870(2) Å, b = 14.393(3) Å, c = 17.114(4) Å, β = 101.43(2)°, Z = 4, R(wR2) = 0.0521(0.1293). Crystallographic data for 5: orthorhombic space group P212121, a = 11.307(l) Å, b = 11.802(l) Å, c = 19.193(2) Å, Z = 4, R(wR2) = 0.0250(0.0593). Crystallographic data for 6: orthorhombic space group P212121, a = 14.036(4) Å, b = 16.486(5) Å, c = 11.397(3) Å, Z = 4, R(wR2) = 0.0261(0.0630).

Preparation and Structure of Re$({\equiv}NC_6H_5)(PPh_3)(PR_3)Cl_3,\;PR_3=PMe_3,\;P(OMe)_3$

  • Kim, Young-woong;Jung, June-ho;Park, Hee-sook;Lee, Soon W.
    • Bulletin of the Korean Chemical Society
    • /
    • v.15 no.10
    • /
    • pp.891-896
    • /
    • 1994
  • Reactions of mer, trans-$Re({\equiv}NC_6H_5)(PPh_3)_2Cl_3$, I, with $PMe_3$ and $P(OMe)_34 at room temperature, led to mer, trans-$Re({\equiv}NC_6H_5)(PPh_3)(PMe_3)Cl_3$, II, and fac-$Re({\equiv}NC_6H_5)(PPh_3)(P(OMe)_3)Cl_34, III, respectively. The crystal structures of II and III were determined through X-ray diffraction. Ⅱ crystallizes in the orthorhombic system, space group $Pna2_1$ with cell parameters a=19.379(4) ${\AA}$, b=11.867(2) ${\AA}$, c = 12.676(3) ${\AA}$, and Z = 4. Least-squares refinement of the structure led to a $R(wR_2)$ factor of 0.0251 (0.0621) for 2203 unique reflections of $I>2{\sigma}(I)$ and for 306 variables. III crystallizes in the monoclinic system, space group $P2_1/n$ with cell parameters a=11.399(3) ${\AA}$, b=14.718(4) ${\AA}$, c=17.558(5) ${\AA}$, ${\beta}=97.79(2){\circ}$, and Z=4. Least-squares refinement of the structure led to a $R(wR_2)$ factor of 0.0571 (0.1384) for 3739 unique reflections of $I>2{\sigma}(I)$ and for 344 variables. Structural studies showed that the relative orientations of the two phosphines in both complexes are different, probably due to the differences in the coordinating abilities between $PMe_3$ and $P(OMe)_3$ to the 5-coordinate fluxional intermediate.

Synthesis and Characterization of (THF)3 Li(NC)CU(C6H3-2,6-Mes2)and Br(THF)2 Mg(C6H3-2,6-Trip2) (Mes = C6H2-2,4,6-Me3; Trip = C6H2-2,4,6-i-Pr3): The Structures of a Monomeric Lower-Order Lithi

  • Hwang, Cheong-Soo;Power, Philip P.
    • Bulletin of the Korean Chemical Society
    • /
    • v.24 no.5
    • /
    • pp.605-609
    • /
    • 2003
  • The lower-order lithium organocyanocuprate compound, (THF)₃Li(NC)Cu($C_6$H₃-2,6-Mes₂) (1), and the bulky terphenyl Grignard reagent, Br(THF)₂Mg($C_6$H₃-2,6-Trip₂) (2), have been synthesized and structurally characterized both in the solid state by single crystal x-ray crystallography and in solution by multi-nuclear NMR and IR spectroscopy. The compound (1) was isolated as a monomeric contact ion-pair in which the C (organic ipso)-Cu-CN-Li atoms are coordinated linearly. The lithium has a tetrahedral geometry as a result of solvation by three THF molecules. The compound (1) is the first example of fully characterized monomeric lower order lithium organocyanocuprate. The bulky Grignard reagent (2) was also isolated as a monomer in which the magnesium, solvated by two THF molecules, has a distorted tetrahedral geometry. The crystals of (1) possess triclinic symmetry with the space group $P{\={1}}$, Z = 2, with a = 12.456(3) Å, b = 12.508(3) Å, c = 13.904(3) Å, α = 99.81°, β = 103.72(3)°, and γ = 119.44(3)°. The crystals (2) have a monoclinic symmetry of space group $P2_{1/C}$, Z = 4, with a = 13.071(3) Å, b = 14.967(3) Å, c = 22.070(4) Å, and β = 98.95(3)°.

Effect of Certain Herb Extracts on Renal Function and $Na^+-K^+$-ATPase in Rabbit Kidney (수종 생약제가 신기능 및 신장 $Na^+-K^+$ ATPase에 미치는 영향)

  • Kim I.S.;Yeom Y.H.;Lee S.B.;Cho B.H.;Cho K.C.
    • The Korean Journal of Pharmacology
    • /
    • v.16 no.1 s.26
    • /
    • pp.51-56
    • /
    • 1980
  • Phytolaccae Radix (PR), Brunella Herba (BH), Akebiae Lignum (AL) and Atractylis Rhizoma (AR) are some of the diuretic agents used in Chinese medicine and folk remedy. Water or methanol extracts of them (100mg/kg) were intravenously injected to rabbits in order to re-evaluate the effects on renal function. PR water extract elicited moderate diuresis while water extracts of BH, AL and methanol extract of AR had antidiuretic effects. Influence of PR on renal hemodynamics and $Na^+-K^+$-ATPase activity in rabbit kidney were observed in vivo and in vitro. The results were as follows: 1) Clearances of inulin and p-aminohippuric acid increased significantly after 15 minutes following the administration of PR water extract, but Na+ reabsorption rate was not changed. 2) The increase of $Na^+-K^+$-ATPase activity in renal cortex, outer and inner medulla was observed at 15 minutes after PR water fraction was given intravenously, and the change was most prominent in cortical area. 3) More than 50% of decrease in $Na^+-K^+$-ATPase activity in renal tissues was observed with PR water fraction $(10^{-2}g/ml)$ in vitro experiments. However, the inhibition of $Na^+-K^+$-ATPase activity was reversed with lower concentrations $(10^{-4}g/ml,\;10^{-6}g/ml)$ of PR water fraction in outer and inner medullary zone. These results suggest the diuretic effect of PR is due to improved renal hemodynamics, and contradictory reults concerning $Na^+-K^+$-ATPase activity require further investigation.

  • PDF

The Dyeing Properties of Woody Fiber Regenerated from Waste MDF by Reactive Dyes (반응성염료에 의한 폐MDF 재생 목질섬유의 염색특성)

  • Ju, Seon-Gyeong;Roh, JeongKwan
    • Journal of the Korean Wood Science and Technology
    • /
    • v.47 no.2
    • /
    • pp.163-177
    • /
    • 2019
  • This study aims to review the relations between the dyeing conditions (i.e., dye concentration, addition amounts of salt and alkali, and dyeing temperature) and dyeing properties and color fastness to light for identifying the optimal dyeing conditions when dyed regenerated woody fibers were obtained through the defibration of waste medium density fiberboard (MDF) using reactive Red H-E3B (Bis-monochlorotriazine (MCT)/MCT type) and reactive Red RB133% (Bis-MCT/Vinyl sulphone type). The dyeing yield (K/S) obtained using two types of reactive dyes increased as the dye concentration increased by 1-10% (on the weight of fiber (OWF)). In addition, the K/S of H-E3B was higher than that of RB133% irrespective of the dye concentration. The color difference of H-E3B after ultraviolet (UV) radiation was lower than that of RB133%, denoting good resistance to discoloration by UV. As the amount of sodium sulfate increased, the color difference and K/S also increased, and the adequate salt content was determined to be 50-70 g/L. Further, the color difference and K/S significantly increased only the addition of 2 g/L of sodium carbonate; however, almost no difference was observed when more than 2 g/L of sodium carbonate was added. The addition amount of sodium carbonate was adequate 5-10 g/L to dyeing the fiber and the pH at this addition level was 10. The dyeing yield of H-E3B increased when the dyeing temperature increased; however, it subsequently decreased after the dyeing temperature became $80^{\circ}C$. The dyeing yield of RB133% was almost the same up to $60-70^{\circ}C$ but declined subsequently. Thus, the adequate temperatures were $80^{\circ}C$ and $60^{\circ}C$ for H-E3B and RB133%, respectively. If the waste MDF woody fiber was dyed under the aforementioned optimal conditions, dyed regenerated woody fiber can be obtained having the following colors: 1.5 to 2.0R with the H-E3B dye and 9.6 to 10.0 PR with RB133%.

The Recovery, In Vitro Maturation and Fertilization of Nili-Ravi Buffalo Follicular Oocytes

  • Samad, H.A.;Khan, I.Q.;Rehman, N.U.;Ahmad, N.
    • Asian-Australasian Journal of Animal Sciences
    • /
    • v.11 no.5
    • /
    • pp.491-497
    • /
    • 1998
  • Four types of serum supplements viz. estrus cow serum (ECS), estrus buffalo serum (EBS), pro-estrus buffalo serum (PrBS) and post-estrus buffalo serum (PtBS), added to TCM-199, were evaluated for in vitro maturation and fertilization of buffalo follicular oocytes. The oocytes were recovered from buffalo ovaries after slaughter, using either aspiration or scoring (multiple incisions) method. The recovered oocytes were categorized as A, B and C based on their cumulus investment and ooplasm homogeneity and cultured in four media. The in vitro matured oocytes were inseminated with $1{\times}10^6$ spermatozoa washed in 2.9% sodium citrate solution. The scoring method yielded greater number of morphologically good oocytes than the aspiration method (3.85 vs 1.76 per ovary, p < 0.01). The maturation rates of three categories of oocytes did not differ from one another. The maturation rates of 80.00, 82.08, 78.77 and 66.23%, while the fertilization rates of 54.54, 55.38, 52.80 and 36.76% were recorded for media containing ECS, EBS, PrBS, and PtBS, respectively. The medium containing PtBS gave lower maturation, as well as fertilization, rates than the other three media (p < 0.05). Thus, the scoring method was better than the aspiration method for the recovery of follicular oocytes. The oocytes categorized A, B and C had similar maturation capabilities. The TCM-199 containing buffalo/cow serum collected at pro-estrus or estrus appeared better for in vitro maturation and fertilization of buffalo follicular oocytes than that containing serum collected at post estrus.