• 제목/요약/키워드: x-ray crystallography

검색결과 316건 처리시간 0.021초

Paddle-wheel유형의 2차 쌓음 단위 $Zn_2(CO_2R)_4$에 기초한 2차원 아연 배위 고분자: [Zn(ATP)(DMF)] $(ATP=2-aminoterephthalate,\;H_2N-C_6H_3-1,4-(COO)_2;\;DMF\;=\;N,\;N-dimethylformamide)$ (Two-dimensional Zinc Coordination Polymer Based Paddle-Wheel Type Secondary Building Units of $Zn_2(CO_2R)_4$: [Zn(ATP)(DMF)] $(ATP=2-aminoterephthalate,\;H_2N-C_6H_3-1,4-(COO)_2;\;DMF\;=\;N,\;N-dimethylformamide)$)

  • 민동원;이희근;이순원
    • 한국결정학회지
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    • 제15권2호
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    • pp.78-82
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    • 2004
  • 벤젠 존재 하에서, DMF와 에탄올의 혼합 용매에서 zinc(II) nitrate $(Zn(NO_3)_2\;{\cdot}\;6H_2O)$$ATP(2-aminoterephthalate,\;H_2N-C_6H_3-1,4-(COO)_2)$의 용매열 반응으로 2차원 배위 고분자 [Zn(ATP) (DMF)] (1)이 얻어졌다 X-ray구조 결정 결과, 2개의 아연 금속과 4개의 ATP 리간드가 paddle-wheel유형의 2차 쌓음 단위들을 형성하고, 이것들은 ATP 리간드에 의해서 연결되어 2차원 4각 망을 이룬다는 것이 밝혀졌다. 아연 금속을 기준으로 각 4각형의 크기는 약$11.1\times11.1\;{\AA}$효이다. 고분자 1을 양질의 결정 상태로 얻기 위해서는 벤젠이 요구되었다.

수소 결합에 의한 삼차원의 Copper(II) 거대고리 착물과 2,5-Pyridinedicarboxylate와의 자기조립 (Self-Assembly of Three-Dimensional Copper(II) Macrocyclic Complex with 2,5-Pyridinedicarboxylate Linked by Hydrogen Bond)

  • 최기영;류해일;김용선
    • 대한화학회지
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    • 제47권2호
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    • pp.104-108
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    • 2003
  • $[Cu(L)]Cl_2{\cdot}2H_2O(L=3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,0^{1.18},0^{7.12}]docosane)$과 2,5-pyridinedicarboxylate(pdc)의 반응으로부터 $[Cu(L)(H_2O)](pdc){\cdot}6H_2O(1)$가 합성되었다. 화합물 1의 구조가 X-ray 회절법 및 분광학적 방법으로 규명되었다. 중심 copper 원자는 거대고리 리간드로부터 4개의 이차 아민과 축방향 위치의 물분자로 결합된 약간 일그러진 사각뿔 구조를 갖는다. 또한 분자간 수소결합은 삼차원의 분자구조를 형성한다.

cis,fac-Dibromooxotris(2,6- dimethylphenyl isocyanide)molybdenum (IV), cis,fac-$[Mo(O)Br_2(CN-C_6H_3-2,6-Me_2)_3]$의 분리 및 구조 (Isolation and Structure of cis,fac -Dibromooxotris(2,6-dimethylphenyl isocyanide)molybdenum(IV), cis,fac-$[Mo(O)Br_2(CN-C_6H_3-2,6-Me_2)_3]$)

  • 이범준;한원석;이순원
    • 한국결정학회지
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    • 제13권2호
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    • pp.82-85
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    • 2002
  • cis,cis,trans-[MoBr/sub 2/(CO)/sub 2/(PPh/sub 3/)/sub 2/]와 2,6-dimethylphenyl isocyanide의 반응으로부터 화합물cis,fac-[Mo(O)Br/sub 2/,(CN-C/sub 6/H/sub 3/,-2,6-Me/sub 2/)sub 3/] (1)이 분리되었다. 화합물 1의 구조가 분광학적 방법(/sup 1/H-NMR, /sup 13/C{/sup 1/H}-NMR, IR) 및 X-ray 회절법으로 규명되었다. 화합물 1의 결정학 자료: 삼사정계 공 간군 P(equation omitted), a=9.172(2) (equation omitted), b = 11.550(3) (equation omitted), c = 15.106(3) (equation omitted), α = 100.44(2)°, β= 107.12(2)°, γ= 107.83(1)°, Z = 2, R(wR/sub 2/) = 0.0529(0.1344).

은(I)화합물:비스(디프로필디싸이오포스페이토)비스(1,10-펜안트로린)이온(I);Ag2[Phen]2[S2P(OPr)2]2 (Dimeric Silver(I) Complex: Bis(dipropyldithiophosphato) bis(1,10-phenanthroline) Disilver(I); Dimeric Silver(I) Complex: Bis(dipropyldithiophosphato) bis(1,10-phenanthroline) Disilver(I);Ag2[Phen]2[S2P(OPr)2]2)

  • Fang Fang Jian;Hai Lian Xiao;Huan Xiang Wang;Kui Jiao
    • 대한화학회지
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    • 제47권1호
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    • pp.26-30
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    • 2003
  • 이핵 화합물, $Ag_2$[Phen]_2[S_2P(OPr)_2]_2$(Phen=1,10-phenanthroline; Pr=propyl)은 비스(디프로필디싸이오포스페이토) 은(|)화합물과 1,10 펜안트로린 리간드 반응에 의하여 합성되었고, 그 화합물 구조는 X-ray에 의하여 규명되었다. 두 디프로필디싸이오포스페이토 리간드는 두 개의 은 원자를 연결하여 팔각형 $Ag_2S_4P_2$ 고리를 형성하였고, 1,10-펜안트로린 리간드는 은 이온과 결합하여 사면체구조를 이루었다. Ag-S 결합거리는 2.471(1)와 2.567(1) ${\AA}$이었고, Ag-N 결합 거리는 2.3666(3)와 2.471(3) ${\AA}$이었다.

Crystal and Molecular Structure of Methyl 12-(3-bromophenyl)-9-[(4-methylbenzene)sulfonyl]-22-oxo-13,21-dioxa-9-azapentacyclo[12.8.0.02,11.03,8.015,20]docosa-1(14),3,5,7,15(20),16,18-heptaene-11-carboxylate

  • Kothandan, Gugan;Ganapathy, Jagadeesan;Damodharan, Kannan;Sanmargam, Aravindhan
    • 통합자연과학논문집
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    • 제7권2호
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    • pp.92-102
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    • 2014
  • The crystal structure of the title compounds with both coumarin and sulfonamide moieties were examined. These two groups have very special for their pharmaceutical and medicinal properties have been determined from single crystal X-ray diffraction data. In the title compound crystallizes in the monoclinic space group C2/c with unit cell dimension a = 28.633(3) ${\AA}$, b= 9.3215(7) ${\AA}$ and c= 24.590(2) ${\AA}$ [alpha & gamma=$90^{\circ}$ beta= $115.976(3)^{\circ}$]. In the structure The S1 atom shows a distorted tetrahedral geometry, with O1-S1-O2 [119.74 $(2)^{\circ}$] and N1-S1-C5 [$105.57(1)^{\circ}$] angles deviating from ideal tetrahedral values are attributed to the Thrope-Ingold effect. The sum of bond angles around N1 ($316.2(1)^{\circ}$) indicates that N1 is in sp2 hybridization. The Pyridine ring adopts boat conformation and pyran rings adopt a sofa conformation. The carboxylate group of atoms were disordered over two positions with site occupancy factors 0.598 (9):0.402 (9). Crystal structure and packing is stabilized by $C-H{\ldots}O$ intra and inter molecular hydrogen bond interactions.

New Azobenzene Crown p-tert-Butylcalix[4]arenes as Switchable Receptors for $Na^+ and K^+$ ions: Synthesis and Isomerization Studies

  • Bongkot Pipoosananakaton;Mongkol Sukwattanasinitt;Nongnuj Jaiboon;Narongsak Chaichit;Thawatchai Tuntulani
    • Bulletin of the Korean Chemical Society
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    • 제21권9호
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    • pp.867-874
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    • 2000
  • Two new azobenzene crown ether calix[4]arenes, 10 and 11, were synthesized by two pathways. In the first pathway,two ethoxy nitrobenzene groups were attached to t-butylcalix[4]arenes in a 1,3 position. Subsequent reduction ofthe nitrobenzene group s by metallic zinc in an alkaline solution afforded 10 and 11 in8% and 12%,respectively. In the second pathway,an azobenzene containing two glycolic units was prepared prior connect-ing to t-butylcalix[4]arenes. The yields from the second approach (5%, 8% for 10 and 11, respectively) were lower than those from the former approach. Single crystals of 10 suitable for X-ray crystallography was ob-tained by recrystallization in methanol.Both the X-ray structure and the 1H-NMR spectrum of 10 indicated that the stereoisomer of the azobenzene moiety was trans and the calixarene platform was in cone conformation. 1H NMR spectroscopy suggested that 10 underwent an observable cis-trans isomerization in CDCl3 under room light and upon UV irradiation with cis:trans ratios of 33:67 and 36:64,respectively. Compound 6 which was the precursor of 11showed fluxional behavior and was found to have mixed conformations ofcone and partial cone with a ratio of 47:53 at -30 $^{\circ}C.$ 1H NMR spectrum of 11 suggested that 11 was initially isolated as cis azobenzene with calix[4]arene in cone conformation and underwent conformational interconversion through calix[4]arene annulas in a similar fashion to 6 upon exposing to light. The complexation studies of 10 with picrate salts of Na+ and K+ using 1H NMR spectroscopysuggested that Na+ preferred to bind the cis form of 10 while K+ preferred to bind the trans form. The stereoisomer of the azobenzene unit in 11 changed partially from cis to trans upon complexing with K+.

Synthesis and Reaction Chemistry of Some Ferrocene-Containing Chelate Ligands with Dirhodium Acetate: X-ray Crystal Structure of $(\eta^1-(S,R)-CPFA)_2Rh_2(OAc)_4$

  • Kim, Eun-Jin;Kim, Tae-Jeong
    • Bulletin of the Korean Chemical Society
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    • 제15권11호
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    • pp.990-996
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    • 1994
  • New ferrocene-based chelate amines, $Fe[C_5H_4CH(Me)NMe_2]_2\;(3), \;Fe[C_5H-3(CH(Me)NMe_2)(PPh_2)-1,2]_2\;(4),\;(C_5H_5)Fe(C_5H_3(CH_2NMe_2)(CH(CN)NMe_2-1,2)\;(6),\;and\;(C_5H_5)Fe(C_5H_3(CH_2NMe_2)(CH(Me)NMe_2-1,2)$ (7) have been prepared. The reaction and the coordination chemistry of 4 and other related compounds (S,R)-(1-N,N-dimethylaminoethyl)-2-dicyclohexylphosphino)ferrocene (CPFA) and 1,1'-bis-(diphenylphosphino)ferrocene (BPPF) with $Rh_2(OAc)_4(MeOH)_2$ were investigated. The reaction of the chiral ligand (S,R)-CPFA forms a complex of the type (${\eta}^1$-(S,R)-CPFA-P)$_2Rh_2(OAc)_4$ (8) in which the ligand is coordinated to both rhodium centers in a monodentate fashion through phosphorus. In contrast, the bisphosphine analogues such as BPPF and 4 afford chelate complexes of the type (${\eta}^2-PP)Rh_2(OAc)_4$ (9 & 10) where both ligands act as a chelate bidentate to a single rhodium atom. All these complexes were characterized by microanalytical and spectroscopic techniques. In one case, the structure of 8 was determined by X-ray crystallography. Crystals are monoclinic, space group C2 (No. 5), with a=26.389 (3), b=12.942 (1), c=11.825 (1) A, ${\beta}$=111.22(1)$^{\circ}$, V=3964.7 (8) $A^3$, Z=4, and $D_{calc}$=1.58 g $cm^{-3}$. Two Rh(II) centers are bridged by four $AcO^-$ groups in the ${\eta}^1$ : ${\eta}^1$ mode across a Rh-Rh single bond, and octahedral coordination at Rh(1) and Rh(1') is completed by axially coordinating (S,R)-CPFA and a briding $AcO^-$, respectively.

Synthesis, Characterization, and Catalytic Properties of Gp 6 Metal Complexes of 1-N,N-dimethylaminomethyl-$1^{\prime}$,2-bis(diphenylphosphino)ferrocene (FcNPP). X-ray Crystal Structure of W$(CO)_4({\eta}^2-FcNPP(O)-P,N)$

  • Kim, Tae-Jeong;Kim, Yong-Hoon;Kim, Eun-Jin;Oh, Sang-Ho;Kim, Hong-Seok;Jeong, Jong-Hwa
    • Bulletin of the Korean Chemical Society
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    • 제15권5호
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    • pp.379-386
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    • 1994
  • Reactions of 1',2-bis(diphenylphosphino)-l-(N,N-dimethylaminomethyl)ferrocene (FcNPP) with $M(CO)_6$ (M=Cr, Mo, W) in the presence of TMNO (Trimethylamine oxide) in a stoichiometric ratio of 1 : 1.5 : 3.5 produced a series of Gp 6 metal carbonyl derivatives with a variety of coordination modes: M(CO)$_4({\eta}^2$-FcNPP-P,P) (M=Cr, Mo, W), $M(CO)_5({\eta}^1-FcNPP-P) (M=Mo, W)\;,\; M_2(CO)_9({\eta}^1\;,\;{\eta}^2-FcNPP-P,P,N) (M=Cr, Mo)\;,\;M_2(CO)_{10}({\eta}^1\;,\;{\eta}^1-FcNPP-P,P) (M=Cr, Mo, W)\;, and\;W(CO)_4({\eta}^2-FcNPP(O)-P,N)$. All these complexes were characterized by microanalytical and spectroscopic techniques. In one case, the structure of W(CO)$_4({\eta}^2$-FcNPP(O)-P,N) was determined by X-ray crystallography. Crystals are monocinic, space group P$2_{1/C}$, with a=10.147(2), b=19.902(3), c=19.821(4) ${\AA},\;{\beta}=96.88(2)^{\circ},\;V=3974(l){\AA}^3$, Z=4, and $D_{calc}=1.64 g cm^{-3}$. The geometry around the central tungsten metal is a distorted octahedron, with the nitrogen and phosphorus atoms being cis to each other. Some of these complexes exhibited catalytic activities in the allylic oxidation and epoxidation of cholesterly acetate. Other oxidation products were also formed with the different chemical yields and product distribution depending upon the ligand and the central metal.

Ethylenediammonium Chromate의 합성 및 결정구조 연구 (Synthesis and Structure of Ethylenediammonium Chromate)

  • 남궁해;박상수
    • 한국결정학회지
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    • 제17권1호
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    • pp.10-13
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    • 2006
  • Ethylenediammonium chromate, $C_2H_{10}N_2{\cdot}CrO_4$ 결정구조는 a=6.667(2), b=8.845(2), c=11.827(2) ${\AA}$, 사방정계(Orthorhombic), 공간군 $P2_12_12_1$, 공간군 번호 19이며, Z=4, V=697.4(3) ${\AA}{^3},\;Dc=1.696gcm^{-3},\;{\mu}=1.594mm^{-1}$이었다. 구조분석은 중금속법으로 풀었으며, 최소 자승법으로 정밀화하였고, 최종 신뢰도 값들은 1204개의 회절반점에 대하여 $R_1=0.0254,\;R_w=0.070,\;R_{all}=0.0255$, S=1.133이었다. 두가지 이온들의 자료들은 기존 유사물질들의 자료에 상응하였으며, Ethylenediammonium 이온은 trans 구조로써 주위의 음이온과 사이에 많은 수소결합으로 연결되어 있다.

[Ni($L^2$)($H_2O$)]Cl$\cdot$$H_2O$ ($L^2$: 3,14-dimethyl-2,6,13,17-tetraazatricyclo [14,4,$0^{1.18}$,$0^{7.12}$docosane-N-acetic acid) 착물의 합성 및 결정구조 (Preparationan dCrystal Structure of [Ni($L^2$)($H_2O$)]Cl$\cdot$$H_2O$ ($L^2$: 3,14-dimethyl-2,6,13,17-tetraazatricyclo [14,4,$0^{1.18}$,$0^{7.12}$]docosane-N-acetic acid))

  • Park, Ki-Yonng;Park, Young-Soo;Kim, Jin-Gyu;Suh, Il-Hwan;Kim, Chang-Suk
    • 한국결정학회지
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    • 제10권1호
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    • pp.33-38
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    • 1999
  • The complex [Ni(L2)(H2O)]Cl·H2O (1) (L2=3,14-dimethyl-2,6,13,17-tetraazartricyclo [14,4,01.18,07.12]docosane-N-acetic acid) has been synthesized and characterized by X-ray crystallography. 1 crystallizes in the triclinic system, space group P, with a=11.274(1), b=13.851(1), c=17.159(6) , α=90.24(2), β=101.10(2), γ=92.11(1)o V=2682.5(11) 3, Z=4, R1=0.042 and wR2=0.111 for 9432 observed reflections with [I>2σ(I)]. The central nicke(II) ion is six-coordinated octahedral geometry with bonds to the four amine nitrogen atoms the carboxylic oxygen atom of the macrocyclic ligand and to the water molecule occupying a position trans to the pendant arm.

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