Crystal Structures of Two New Monoprotonated Products of 1,4,7-trimethyl- 1,4,7-triazacyclononane: (Me3 [9] aneN3H ) (SO3CF3) and (Me3 [9] aneN3H) I

Two new monoprotonated products of macrocyclic polyamine 1,4,7-trimethyl- 1,4,7-triazacyclononane (Me3 [9]aneN3), (Me3 [9]aneN3H) (SO3CF3) 1 (C10H22N3O3SF3, Mr=321.36) and (Me3[9]aneN3H)I 2 (C9H22N3I, Mr=299.20) were obtained by the reactions of Me3[9]aneN3 and yttrium triflate or ytterbium diiodide as the unexpected products. The crystal structures of compounds 1 and 2 have been determined. Crystal 1is orthorhombic, space group P212121(#19), a =12. 609(3), b=13. 531(1), c=9.225(3) A, V=1573.9(7) A3, Z=4, Dc=1. 356g/cm3, μ=2.47cm- 1, F (000) = 680 and R= 0. 052, Rw= 0. 052 for 807 unique reflections with I＞ 2σ(I). Crystal 2 belongs to the orthorhombic system with space group P212121 (# 19), a=11.417(2), b=13.099(3), c=8.762(2) A, V=1310.5(4) A3, Z=4, Dc=1. 516 g/cm3, μ= 24.14 cm-1, F(000)=600 and R=0. 035, Rw=0. 042 for 1427 u-nique reflections with I＞3σ(I). The two structures contain the same cyclic framework in which the acid proton is bonded to an amine nitrogen. This proton exhibits strong intramolecular hydrogen bonds with the other two nitrogen atoms. The methyl groups are directed away from the ring cavity. The bond distance between acid proton and an amine nitrogen in compound 2 is extremely short. The bond angles for 1 and 2 also exhibit obvous diversity inside of triazacyclononae.     

CRYSTAL STRUCTURE OF p—PROPIONYLCALIX [4]ARENE

<正> The title compound was synthesized by Friedel-Crafts reaction of tetrahydroxycalix [4] arene and propionyl choride, and its crystal structure was determined by X-ray diffraction technique. C10O8H40,Mr = 648. 75, triclinic, space group P1 with cell parameters, a = 9. 930(5), b = 11. 838(3), c=14. 522(7) A,α= 94. 92(3),β=102. 96(4),γ= 98. 32(3)°, V = 1635A3, Z = 2, Dc = 1. 399g/ cm3, μ(CuKa) = 3. 27cm-1, F (000) = 344. The final R = 0. 075, Rw = 0.092 for 5716 independent reflections with I>3σ(I). The crystal structure analysis shows that the molecule exists in fine cone conformation.     

Synthesis and Crystal Structure of 8-(2,3-Dimethoxyphenyl)-10,11,12,13-tetrahydro-9H-benzo [f] cyclohepta [c] quinoline

The title compound 8-(2,3-dimethoxyphenyl)-10,11,12,13-tetrahydro-9H-benzo[f]-cyclohepta[c]quinoline(C26H25NO2,Mr=383.47) was synthesized and characterized by IR,1H NMR,13C NMR and elemental analysis.The crystal belongs to triclinic,space group P1 with a= 8.1490(16),b=9.2550(19),c=14.373(3) ,α=86.96(3),β=89.66(3),γ=70.32(3)°,Z=2,V=1019.2(4) 3,Dc=1.250 g·cm-3,μ(MoKα)=0.078 mm-1,F(000)=408,the final R=0.0555 and wR=0.1240 for 2228 observed reflections(Ⅰ > 2σ(Ⅰ)).X-ray analysis reveals that the seven-numbered ring is slightly similar to a six-numbered ring,forming the chair-like conformation.The four rings(Ⅰ,Ⅱ,Ⅲ and Ⅳ) in the benzo[f]cyclohepta[c]quinoline moiety form a screw structure.     

Synthesis and Crystal Structure of [Cu (C_8H_4O_2F_3S) (2, 2' -bipy) ]

1INTRODUCTIONCoppercomplexesarewidelyusedascatalystsinthedecompositionofdisubsti-tutedperoxides"'-Theelectronicstructureandbondingatthecatalystscanbeprof-itablypursuedbystudyingmodelcomplexes.Generally,theCu(I)complexesareob-tainedbyreactionofCu(l)saltswithligands.Wereporthereamethodofpreparingcopper(I)complexbythereactionofCupowderwith2-thenoyltrifluoroacetone,2,2'-bipyinmethanol.2EXPERIMENTALReactionwascarriedoutundernitrogenatmosphere.2,2-bipy(1mmol)wasaddedtoamixtureof2-thenoyl…     

Synthesis and Structural Characterization of [Mn（sapn）（H2O）2]Br

1 INTRODUCTION Many of the recent advances in the coordination chemistry of manganese have been driven by the involvement of the manganese in several biological redox-active systems[1,2], of which the most important is the oxygen-evolving complex (EOC) of photosystem II (PS II) in green plants [3]. Since the preparations and structural characterizations of the complexes containing N,O-donor ligands have been studied extensively as simple active-site models for the photosystem II[4,5]…     

Crystal and Molecular Structure of 2-(2, 6-Dinitro-4-Trifluoromethyl) phenylthio-5, 7-Dimethyl-1,2,4-Triazolo [1, 5-a] Pyrimidine

1INTRoDUCTIONItwasreportedthattheheterocycliccompoundscontainingl,2,4-triazolo[1,5-ajpyrimldinyldisplayedpotentialbioIogicalactivities['2i.Howeverltheherbicidalac-tivityofthethio-etherderivativesof1,2,4xtriazolo[1,5-ajpyrimidinewasrarelyre-ported"'.Inourpreviouspaper"',wedesignedandsynthesizedaseriesof2-arylthio-l,2,4-triazolo{l,5-ajpyrimidines,someofwhichdisplayedgoodherbicidalactivity.Inordertostudythestructure-activityrelationshipofthesecompounds,thestructureofthetitlecompound(1)wasan…     

Synthesis and Crystal Structure of H2Mo8O26[(n-Bu)4N]2[(CH3)2COHCH2COCH3]2

The title compound 4-methyl-4-hydroxy-2-pentone is obtained by the condensed reaction of acetone, and co-crystallized with octamolybdate anion and tetrabutyl-ammonium cation. The crystal structure belongs to triclinic system, space group P1, Mo8C44H98O30N2 Mr= 1902.77, a=11. 512(6), b=12. 790(3), c=13. 395(4)A, α=65. 22(2), β=78. 26(4), γ=71. 12(3), V=1689(1) A3, Z=1, Dx=1. 869g/cm3, F(000)=950, μ=14.79 cm-1, final R=0. 053 and Rw=0. 067. Theorbital hybridization of C (53) and C (55) are sp3 and sp2 separately in (CH3)2COHCH2COCH3 and the catalysis of β-octamolybdate anion might be present for the condensed reaction of acetone.     

Crystal Structure of 1 －Acetyl －2－［O－methylphenyl） phenyl－ thiophosphonyl］ Hydrazine

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅＯｆ１－Ａｃｅｔｙｌ－２－［Ｏ－ｍｅｔｈｙｌｐｈｅｎｙｌ）ｐｈｅｎｙｌ－ｔｈｉｏｐｈｏｓｐｈｏｎｙｌ］Ｈｙｄｒａｚｉｎｅ￥ＺｈａｎｇＬｉ－Ｊｕａｎ；ＬｉｕＸｉａｏ－Ｌａｎ；ＭｉａｏＦａｎｇ－Ｍｉｎｇ（Ｉｎｓｔｉｔｕｔｅ...     

CRYSTAL STRUCTURAL FEATURE OF [HMTTeF·I][HMTTeF·I_2]

<正> The title complex, [HMTTeF·I][HMTTeF·I2] , HMTTeF = hexam-ethylenetetratellurafulvalene C5H8Te2CHCHTe2C5H8, was synthesized by the electrochemical method and was determined from single crystal X-ray diffraction. Mr = 857 ,monoclin-ic,space group C2/m,a= 16. 529(4) ,b= 19. 381 (4),c= 12. 616(2) A ,= 102. 32 (1)°,V= 3948(1)A3,Z=4,DC = 2. 88gcm-3,F(000) = 2972,μ(MoKa) = 842cm-1,R= 0. 049. Both ionic bond and covalent bond with mixed valence co-exist in this compound.     

Synthesis and Structure of a Dimolybdenum Carbonyl Compound with Thiolato-Bridges [Et4N] 2 [Mo2 (CO) 8 (SC6H4-Cl -p) 2]

Reaction of Mo (CO)6 with p-Cl-C6H4SNa and Et4NCl · H2O in CH3CN afforded a dinuclear molybdenum (0) compound [Et4N]2 [Mo2 (CO)8 (SC6H4-Cl-p)2] (1). The crystal structure was determined by X-ray diffraction. The crystallographic data: C36H48Cl2Mo2N2O8S2, Mr= 963.71, monoclinie, P21/c, a=9. 269(4),b=13.750(3), c=17.466(6) A ;β=104.84(3)°; V=2151.8(3) A3; Z=2; Dc=1.49 g/cm3; F(000)=984; μ=8.3 cm-1; MoKα radiation (λ=0. 71073A ); Final R = 0. 055 and Rw=0. 065 for 3287 reflections with I＞3. 0σ(I). The X-ray structure analysis revealed that the Mo2S2 core is planar. The geometry around each Mo atom is a distance is 4. 014(2) A , and this obviously indicates the absence of Mo-Mo bond.     

Synthesis and Structure of Dinuclear Molybdenum Carbonyl Thiolate Compound [Et4N ] 2 [Mo2 (CO) 8 (SC6H4-OCH3-p) 2]

Reaction of Mo(CO)6 with p-H3CO-C6H4SNa and Et4NCl · H2O in CH3CN afforded a dinuclear molybdenum(0) compound [Et4N]2[Mo2 (CO)8 (SC6H4-OCH3-p)2] (1). The crystal structure was determined by X-ray diffraction. The crystallographic data: C38H54Mo2N2O10S2, Mr = 954.87, triclinic, P-1, a = 11.348 (7), b =11.616(5), c=10.065(7) A, a=113.86(4), β=111.39(5), γ=91.92(5)°, V=1104.0(1) A3, Z=1, Dc=1.44 g/cm3, F(000)=492, μ=7.0cm-1, Final R=0. 046 and Rw=0. 049 for 2657 reflections with I＞3. Oσ(I). The X-ray structure analysis revealed that the Mo2S2 core of 1 is planar. The geometry around each Mo atom is a distorted octahedron, the two octahedrons form an edge-sharing bioctahedron. The bond. In addition, the 95Mo NMR chemical shift of 1 is discussed.     

Synthesis and Structural Characterization of a Hetcrobimctallic Molybdenum-Copper-Sulfur Compound [Et_4N]_2 CMoCu_3S_4 (S_2CNEt_2)_3]

<正> The title compound crystallizes in orthogonal space group P212121with α= 12. 848 (5), b =13. 227 (3), c = 29. 519(8) A ,Z = 4 , V= 5016. 5 A3 and Dc = 1. 483g/cm3. 4940 independent reflcctiions were collected on a CAD4 diffractometer with MoKa radiation in the range of 1°<0<25°,of which 3559 reflections having intensities I >3σ(I) were used for structure determination. The structure was solved by direct methods and refined by the least-squares method to final discrepancy factors R=0. 071 and Rw - 0. 075. The anion of the title compound can be described as a slightly distorted MoS42-tetrahedron coordinated by three [CuS2CNEt2] units ,with the four metal atoms lying approximately in a plane.     

Crystal Structure of 1, 1-Dichloro-la, 3-diphenyl-1, la, 2, 3-tetrahydro-azirino [2, 1-d ] [1, 5]benzothiazepine (C_(22),H_(17)Cl_2NS )

1INTR0DUCTI0NBenzoheteroazepinecompoundsareimportantpharmaceuticalagents"-".Inre-centyears,ithasbeenfoundthatbenzoheter0azepinetricyclicderivatives,especiallythosefusedwithotherfiveorsix-memberedheterocycle,area1soofpotentialphar-maceuticalinterestst4-6j.Hence,muchattentionhasbeenpaidtothesynthesesofthem,suchasl,3-oxazino[3,2-djt1,5jbenzothia/diazepin-l-onet"'J,1,2,4-tria-zolo[4,3-dj[1,5jbenzothia/diazepine"',1,2,4-oxadiazolo[4,5-dj[l,5jbenzothia/diazepine',',andsoon.Meanwhiletheirstructur…     

Synthesis and Crystal Structure of Dinuclear Copper Cluster Compound ［Cu（dtp）PPh_3］_2

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＤｉｎｕｃｌｅａｒＣｏｐｐｅｒＣｌｕｓｔｅｒＣｏｍｐｏｕｎｄ［Ｃｕ（ｄｔｐ）ＰＰｈ_３］_２ＣｈｅｎＱｉｕ－Ｈｕａ；ＬｕＳｈａｏ－Ｆａｎｇ；ＨｕａｎｇＸｉａｏ－Ｙｉｎｇ（ＳｔａｔｅｋｅｙＬａｂ...     

Synthesis and Crystal Structure of 2-Ethoxycarbonylmethyl-8-chloro-3a,4-dihydro-3a-methyl-chromeno[4,3-c]pyrazol-3（2H）-one

The crystal structure of the title compound 2-ethoxycarbonylmethyl-8-chloro-3a,4-dihydro-3a-methyl-chromeno[4,3-c]pyrazol-3(2H)-one(C15H15ClN2O4,Mr = 322.74) has been prepared and determined by single-crystal X-ray diffraction.The crystal is of orthorhombic,space group Pccn with a = 16.7246(10),b = 19.6626(12),c = 9.3013(6) ,V = 3058.7(3) 3,Z = 8,Dc = 1.402 g/cm3,μ = 0.269 mm-1,F(000) = 1344,the final R = 0.0506 and wR = 0.1464 for 2568 reflections with I 2σ(I).In addition,disordered C(14) and C(15) atoms exist in the crystal structure.     

Synthesis and Structure of Dinuclear Molybdenum Carbonyl Thiolate Compound[Et4N]2[Mo2(CO)8(SC6H4-CH3-p)2]

1　ＩＮＴＲＯＤＵＣＴＩＯＮＳｉｎｃｅｔｈｉｏｌａｔｅｌｉｇａｎｄｗａｓｉｎｔｒｏｄｕｃｅｄｉｎｔｏｍｏｌｙｂｄｅｎｕｍｃａｒｂｏｎｙｌｃｏｍｐｏｕｎｄｉｎ1 984 [1],ｔｈｅｉｎｖｅｓｔｉｇａｔｉｏｎｏｎｌｏｗ ｖａｌｅｎｃｅＭｏ -ＳＲｃｏｍｐｏｕｎｄｓｈａｓｒｅｃｅｉｖｅｄａｔｔｅｎｔｉｏｎｆｏｒｔｈｉｓｋｉｎｄｏｆｌｏｗ ｖａｌｅｎｃｅｃｏｍｐｏｕｎｄｓｐｏｓｓｅｓｓｃｅｒｔａｉｎａｄｖａｎｔａｇｅｏｎｃｏｍｐｏｕｎｄｓｙｎ ｔｈｅｓｉｓ,ｍｏｌｅｃｕｌｅｓｔｒｕｃｔｕｒｅａｎｄｐｈｙｓｉｃａｌａ…     

Crystal Structure of 3－hydroxyl－1，5－diazacycloheptane Dihydrobromide C_5H_（12）N_2O·2HBr

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ３－ｈｙｄｒｏｘｙｌ－１，５－ｄｉａｚａｃｙｃｌｏｈｅｐｔａｎｅＤｉｈｙｄｒｏｂｒｏｍｉｄｅＣ_５Ｈ_（１２）Ｎ_２Ｏ·２ＨＢｒＬＩＵＹｏｎｇ；ＸＵＥＧｕｏ－Ｐｉｎｇ；ＷＵＣｈｅｎｇ－Ｔａｉ（Ｄｅｐａｒｔｍｅｎｔｏｆ?..     

CRYSTAL STRUCTURE OF HETEROPOLY TUNGSTOANTIMONATE (NH4)_12[Cu3(H_2O)_3Sb_2W_18O_56]·9H_2O

<正> (NH4)12[Cu3(H2O)3Sb2W18O66].9H2O,Mr = 5232.06, orthorhombic, space group Pmcn, a=15.423(4), b = 19.307(6), c = 30.275(6) A,V= 9015.0 A3, Z=4,Dc=3.866 g/cm3,u= 247.569 cm-1,R = 0.064 for 2652 observed reflections [I> 3σ(I)]. X-ray analysis shows that the heteropoly anion of the title compound consists of two α-β-SbW9O33 subunits, which are derived from the a-Keggin structure by loss of one W3O13 group constituted by three edge-sharing WO6 octahedra, merged together through the connection with three CuO4(H2O) units with the O atoms shared with the W atoms.     

Synthesis and Crystal Structure of Gd3（BSiO6）（SiO4）

1INTRODUCTIONRareearthborosilicateshaverarelybeenreportedinthepastdecade.LnBMO5(M=Ge,Si)(l,z,31exhibitsthestillwellitestructureonlyforlargerlanthanide,initsstructure,twoBO'tetrahedraandoneSiO'tetrahedronareconnectedbycorner-sharedeachothertoformsix-memberringthatconstructinfinitehelicalchainsparal-lelto3lscrewaxis-Serhanetal(43synthesizedNd,BM2O,,(M=Si Ge)whosestructurecontainstri-coordinatedboronatoms.Recently,wehavesynthesizedSm3BSi2O1,andEu,BSi,O,,t"6),herewerffportthesynthes…     

OXIDATION DECARBONYLATION OF NH_4[Mo(CO)_5I]: SYNTHE-SES AND CRYSTAL STRUCTURES OF CMo(S_2CNC_4H_8)_4]I_3 · C_7H_8 and Mo_2S_2O_2(S_2CNC4H_8)_2

<正> Both of the title complexes were produced by oxidative decarbony-lation of NH4 CMO (CO)5I]. The complexes CMo(S2CNC4H8)4]I3 ?C7H8(1) and Mo2S2O2 (S2CNC4H8)2(2) both crystallize in triclinic, space group P1 with cell dimensions for (1) : a=13. 554(4), b=13. 620(4), c= 13. 058 (4) A , α=95. 58 (3), β=105. 38(2), γ=115. 49(2)°,V = 2035(1) A3, Z=2, Dc=1. 89 g. cm-3, final R=0. 054 and Rw = 0. 062 for 2926 observed reflections; and for (2): a = 8.730(2), b=16.592(6), c = 6. 688(2)A, α=97. 67(3), β=98. 10(2), γ=80. 26(2)% V = 939. 2(5) A3, Z = 2, Dc = 2. 05 g. cm-3, final R = 0. 038 and Rw = 0. 046 for 2248 observed reflections. The Mo(V) atom is bonded to eight S atoms in distorted dodecahedron for (1). The Mo atoms in compound (2) are bridged by two S atoms and each Mo atom is coordinated by two S atoms from S2CNC4H8 and one O atom to form distorted tetragonal pyramid.