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1.
Chiral Dimethylgallium Amino Alkoxides Me3Ga reacts with (S)-1-methyl-2-pyrrolidinyl-methanol, (+);(–)-2-piperidyl-methanol, and (S)-α,α,-diphenyl-2-pyrrolidinyl-methanol in molar ratio 1 : 1 with formation of the corresponding dimethylgallium aminoalkoxides 1 – 3 . As a consequence of the Ga–N-interaction new centres of chirality containing asymmetric surrounded N-atoms are formed. Compounds 1 – 3 were characterized by their 1H, 13C nmr and mass spectra. The crystal structures of 1 – 3 were determined by single crystal structure analysis. 1 and 2 are dimeric in solid state, 3 is forming monomeric molecules. 1 and 3 crystallize in the monoclinic space group P21 with Z = 2, a = 7.245(4), b = 11.887(3), c = 11.807(6) Å, β = 93.48(3)° for 1 and Z = 4, a = 11.0871(7); b = 6.539(4), c = 12.6919(8) Å, β = 107.04(1)° for 3 . 2 and 2 a crystallize in the monoclinic space groups C2/m and C2/c with Z = 2, a = 15.891(3), b = 9.526(2), c = 7.345(1) Å, β = 111.89(3)° for 2 and Z = 4, a = 19.374(4), b = 8.430(2), c = 19.961(4) Å, β = 100.09(3)° for 2 a .  相似文献   

2.
Abstract

It has been shown that host compound 1,1,6,6-tetraphenylhexa-2,4-diyne-1,6-diol is able to include polar guests and now we report on its ability to form clathrate compounds with apolar guests. The structures of this host with cyclohexane (1) and the ortho (2), meta (3) and para (4) xylenes have been determined and are discussed. Crystal data: (1) 2C30H22O2C6H12, M r = 913.20 g mol?1, mono-clinic, C2/c, a = 22.851(6), b = 14.010(2), c = 17.076(6) Å, β = 108.71(3)°, V = 5178(2) Å3, Z = 4, D c = 1.17g cm?3, N = 3326, R = 0.092. (2) 2C30H22O21 ½C8H10, M r = 1976.5 g mol?1, triclinic, P 1, a = 13.185(3), b = 15.466(3), c = 16.573(2) Å, α = 96.39(13)°, β = 106.96(15)°, γ = 114.94(18)°, V = 2822(2) Å3, Z = 2, D c = 1.16 g cm?3, N = 6152, R = 0.075. (3) 2C30H22O21 ½C8H10, M r = 1976.5 g mol?1, triclinic, P 1, a = 13.267(5), b = 15.453(3), c = 16.654(5) Å, α = 97.12(2)°, β = 107.09(3)°, γ = 114.68(3)°, V = 2843(2) Å3, Z = 2, D c = 1.15 g cm?3, N = 6505, R = 0.083. (4) 2C30H22O21 ½C8H10, M r = 1976.5 g mol?1, triclinic, P 1, α = 13.070(2), b = 15.348(3), c = 16.776(3) Å, α = 67.88<2)°, β = 74.27(1)°, γ = 65.29(1)°, V = 2817(1) Å3, Z = 2, D c = 1.15 g cm?3, N = 6711, R = 0.050. Thermal analysis studies were also performed in order to examine their stability and the strength with which the guest species are held in the crystal lattice.  相似文献   

3.
Twelve ternary alloys in the Ca‐Cu‐Sn system were synthesized as a test on the existing phases. They were prepared from the elements sealed under argon in Ta crucibles, melted in an induction furnace and annealed at 700 °C or 600 °C. Four ordered compounds were found: CaCuSn (YbAuSn type), Imm2, a = 4.597(1) Å, b = 22.027(2) Å, c = 7.939(1) Å, Z = 12, wR2 = 0.080, 1683 F2 values; Ca3Cu8Sn4 (Nd3Co8Sn4 type), P63mc, a = 9.125(1) Å, c = 7.728(1) Å, Z = 2, wR2 = 0.087, 704 F2 values; CaCu2Sn2 (new structure type), C2/m, a = 10.943(3) Å, b = 4.222(1) Å, c = 4.834(1) Å, β = 107.94(1)°, Z = 2, wR2 = 0.051, 343 F2 values; CaCu9Sn4 (LaFe9Si4 type), I4/mcm, a = 8.630(1) Å, c = 12.402(1) Å, Z = 4, wR2 = 0.047, 566 F2 values. In all phases the shortest Cu‐Sn distances are in the range 2.59‐2.66Å, while the shortest Cu‐Cu distances are practically the same, 2.53‐2.54Å, except CaCuSn where no Cu‐Cu contacts occur.  相似文献   

4.
Five new complex compounds of the formula Ln(phen)2(NO3)3 were prepared. The X‐ray structural analyses indicate that they crystallize isostructurally in the monoclinic space group C2/c (no. 15) with cell dimensions for example for Pr(phen)2(NO3)3: a = 11.194(1) Å, b = 18.095(2) Å, c = 13.101(2) Å, β = 100.52(1)°, V = 2609.1(6) Å3, Z = 4. The crystal structures consist of [Ln(phen)2(NO3)3] complex molecules. The rare earth atoms are coordinated by four N atoms of two phen ligands and six O atoms of three nitrato groups to complete a distorted bicapped dodecahedron. The [Ln(phen)2(NO3)3] complex molecules are assembled via π‐π stacking interactions between the neighboring phen ligands to form 1D columnar chains, which are then arranged in the crystal structures according to pseudo 1D close‐packed patterns.  相似文献   

5.
Rare Earth Halides Ln4X5Z. Part 1: C and/or C2 in Ln4X5Z The compounds Ln4X5Cn (Ln = La, Ce, Pr; X = Br, I and 1.0 < n < 2.0) are prepared by the reaction of LnX3, Ln metal and graphite in sealed Ta‐ampoules at temperatures 850 °C < T < 1050 °C. They crystallize in the monoclinic space group C2/m. La4I5C1.5: a = 19.849(4) Å, b = 4.1410(8) Å, c = 8.956(2) Å, β = 103.86(3)°, La4I5C2.0: a = 19.907(4) Å, b = 4.1482(8) Å, c = 8.963(2) Å, β = 104.36(3)°, Ce4Br5C1.0: a = 18.306(5) Å, b = 3.9735(6) Å, c = 8.378(2) Å, β=104.91(2)°, Ce4Br5C1.5: a = 18.996(2) Å, b = 3.9310(3) Å, c = 8.282(7) Å, β = 106.74(1)°, Pr4Br5C1.3: a = 18.467(2) Å, b = 3.911(1) Å, c = 8.258(7) Å, β = 105.25(1)° and Pr4Br5C1.5: a = 19.044(2) Å, b = 3.9368(1) Å, c = 8.254(7) Å, β = 106.48(1)°. In the crystal structure the lanthanide metals are connected to Ln6‐octahedra centered by carbon atoms or C2‐groups. The Ln6‐octahedra are condensed via opposite edges to chains and surrounded by X atoms which interconnect the chains. A part n of isolated C‐atoms is substituted by 1‐n C2‐groups. The C‐C distances range between 1.26 and 1.40Å. In the ionic formulation (Ln3+)4(X?)5(C4?)n(C2m?)1?n·e? with 0 < n < 1 and m = 2, 4, 6 (C22?, C24? C26?), there are 1 < e? < 5 electrons centered in metal‐metal bonds.  相似文献   

6.
Reactions of a solution of AgNO3 in aqueous methanol with solutions of 1,4-diallylpiperazine (acidified with HNO3 to pH = 4) and 1-allyloxybenzotriazole in ethanol gave the crystalline silver(I) π-complexes [Ag2(C4H8N2(C3H5)2(H+)2)(H2O)2(NO3)2](NO3)2 (I) and [Ag(C6H4N3(OC3H5)(NO3))] (II). Their crystal structures were determined by X-ray diffraction. Crystals of complexes I and II are monoclinic, space group P21/c; for I: a = 7.053(3)Å, b = 9.389(3)Å, c = 15.488(4)Å, β = 91.60°, V = 1025.3(6)Å3, Z = 4; for II: a = 10.650(4)Å, b = 15.062(5)Å, c = 7.412(4)Å, β = 104.20(3)°, V = 1152.6(8)Å3, Z = 4. In both structures, the organic components act as bidentate ligands forming with AgNO3 34- and 14-membered topological rings, respectively. In complex I, the nearly tetrahedral environment of the Ag(I) atom is made up of the olefinic C=C bond, the O atoms of the nitrate anions, and the water molecule. 1-Allyloxybenzotriazole in structure II causes the deformation of the coordination polyhedron of Ag into a trigonal pyramid via inclusion of the ligand N atom in its coordination sphere. The topological units of the complexes form infinite polymer layers linked by anionic NO 3 ? bridges. In structure I, these layers are united through a system of hydrogen bonds into a three-dimensional framework.  相似文献   

7.
Two new cobalt complexes were successfully synthesized from the reaction of binaphthyl Schiff base 2 with Co(OAc)2 in the presence of sodium methoxide at 80 °C for 24 h and Co(acac)3 in toluene under reflux. Their unique crystal structures are unambiguously disclosed by X‐ray analysis. Complex 3 is triclinic, space group P1 , unit cell dimensions a = 10.742(2) Å, b = 11.153(2) Å, c = 12.715 Å, α = 79.865(3) °, β = 76.053 °, γ = 72.532(4) °, volume 1401.3(5) Å3, Z = 2. Complex 4 is triclinic, space group P1 , unit cell dimensions a = 10.801(2) Å, b = 12.554(3) Å, c = 15.219(3) Å, α = 105.672(4) °, β = 103.048 °, γ = 104.594(4) °, volume 1824.8(7) Å3, Z = 2, calculated density 1.428 Mg m−3. Copyright © 2003 John Wiley & Sons, Ltd.  相似文献   

8.
Two zinc complexes of enoxacin were synthesized and their crystal structures were determined. Compound 1, [Zn(H-Eno) · Cl2] · 3H2O (H-Eno = Enoxacin), crystallizes in the triclinic system, space group P 1, with lattice parameters a = 8.7731(12), b = 9.4976(14), and c = 13.2033(19) Å, α = 86.319(7)°, β = 71.912(7)°, and γ = 80.604(7)°, V = 1031.6(3) Å3, Z = 2, D Calcd = 1.631 Mg m?3; compound 2, [Zn(H-Eno) · (H2O)2] · 2NO3, also crystallizes in the triclinic system, space group P 1, with lattice parameters a = 8.751(2), b = 9.014(2), and c = 12.594(3) Å, α = 92.277(14)°, β = 109.867(12)°, and γ = 111.469(12)°, V = 854.1(3) Å3, Z = 1, D Calcd = 1.684 Mg m?3.  相似文献   

9.
Two complexes with enoxacin and ciprofloxacin were synthesized and the crystal structures are reported. Compound 1, [Cu(H-Eno) · Cl2] · 3H2O (H-Eno = Enoxacin), crystallizes in the triclinic system, space group P 1, with lattice parameters a = 8.7731(12) Å, b = 9.4976(14) Å, c = 13.2033(19) Å, α = 86.319(7)°, β = 71.912(7)°, γ = 80.604(7)°, V = 1031.6(3) Å3, Z = 2, D c = 1.625 mgm?3. 2, [Mn(Cip)2] · 2H2O (Cip = mono-anion of ciprofloxacin), crystallizes in the monoclinic, space group P2(1)/c, with lattice parameters a = 5.85690(10), b = 21.9490(6), c = 13.4443(3) Å, β = 100.9700(10)°, V = 1696.72(7) Å3, Z = 2, D c = 1.459 mgm?3.  相似文献   

10.
The complexes of 2,11‐dithia‐4,5,6,7,8,9‐hexahydro[3.3]paracyclophane (dthhpcp) with Cu(I), i.e. [Cu2I2(dthhpcp)2]·2H2O 1 , or with Ag(I), i.e. [Ag(dthhpcp)(NO3)]thf 2 and [Ag(dthpcp)(CF3COO)] 3 , were prepared for structural study by single‐crystal X‐ray diffraction analysis. For these three complexes, dthhpcp serves as a bridging group in the polymeric structure through bridging sulfur atoms via metal, while the bonding of anion with the second metal atom forms the multi‐diminished structures. Complex 1 is a novel two‐dimensional coordination polymer composed of Cu6 motifs, in which Cu2I2 formed a square planar unit to link the dthhpcp molecule. The two oxygen atoms of the nitrate anion as a bridge for two Ag atoms in complex 2 provides a three‐dimensional channel framework of silver(I) with a tetrahydrofuran molecule as a guest inside the open cavities. In contrast, the analogous reaction with silver triflouroacetate gave a complex 3 , which is composed of infinite linear chains of‐Ag‐dthhpcp‐Ag‐dthhpcp‐ along the a axis. Unit cell data: complex 1 , orthorhombic system, space group P2(1)2(1)2(1), a = 19.2982(11) Å b = 16.5661(10) Å, c = 25.3006(15) Å, β = 90°, Z = 8; complex 2 , orthorhombic system, space group Pna2(1), a = 8.8595(6) Å, b = 12.6901(9) Å, c = 19.8449(14) Å, β = 90°, Z = 4; complex 3 , monoclinic system, space group P2(1)/n, a = 8.845(3) Å, b = 20.841(6) Å, c = 11.061(3) Å, β = 107.832(6)°, Z = 4.  相似文献   

11.
Three adipato bridged mixed ligand catena complexes {[M(phen)(H2O)]‐(C6H8O4)2/2} with M = NiII ( 1 ), CuII ( 2 ), ZnII ( 3 ) were synthesized. Structure determination based on X‐ray diffraction shows that they crystallize isostructurally in the monoclinic space group C2/c (no. 15) with cell dimensions of: 1 a = 22.451(4)Å, b = 9.041(1)Å, c = 17.440(2)Å, β = 103.41(1)°, U = 3443.4(9)Å3, Z = 8; 2 a = 22.479(2)Å, b = 9.067(1)Å, c = 17.494(3)Å, β = 103.67(1)°, U = 3464.6(8)Å3, Z = 8; 3 a = 22.635(3)Å, b = 9.052(1)Å, c = 17.571(3)Å, β = 103.24(1)°, U = 3504.5(9)Å3, Z = 8. The crystal structure consists of 1D {[M(phen)(H2O)]‐(C6H8O4)2/2} zigzag chains, in which the metal atoms are all octahedrally coordinated by two N atoms of one phen ligands and four O atoms of one H2O molecule and two adipato ligands. The zigzag chains are held together by interchain π‐π stacking interactions and interchain hydrogen bonds.  相似文献   

12.
Three polymorphs of barium dihydrogen‐hypodiphosphate(IV)‐dihydrate, BaH2P2O6 · 2H2O ( A , B and C ), were obtained and structurally characterized by single‐crystal X‐ray diffraction. A crystallizes in the monoclinic space group P21/n (no. 14) with a = 7.459(1) Å, b = 8.066(1) Å, c = 12.460(2) Å, β = 91.27(1) ° and Z = 4. B crystallizes in the monoclinic space group C2/c (no. 15) with a = 11.049(8) Å, b = 6.486(3) Å, c = 10.956(6) Å, β = 106.89(5) ° and Z = 4. C crystallizes in the orthorhombic space group C2221 (no. 20) with a = 9.193(3) Å, b = 6.199(2) Å, c = 12.888(4) Å and Z = 4. Discrete [H2P2O6]2– units, barium cations and water molecules, held together by intermolecular hydrogen bonds of the type O–H ··· O, build up the structures of the three polymorphs. The phase purity of A and C was verified by powder diffraction measurements.  相似文献   

13.
Novel complex salts [Au(en)2]Cl(ReO4)2 (I) and [Au(en)2](ReO4)3 (II), en = ethylenediamine, are obtained. Their crystal structures are determined by single crystal X-ray diffraction. Complex I crystallizes in the triclinic crystal system: a = 6.2172(7) Å, b = 7.1644(8) Å, c = 8.8829(8) Å, α = 96.605(4)°, β = 110.000(4)°, γ = 97.802(4)°, P-1 space group, Z = 1, d x = 3.905 g/cm3; complex II crystallizes in the monoclinic crystal system: a = 15.244(2) Å, b = 7.6809(8) Å, c = 9.3476(12) Å, β = 127.004(3)°, C2 space group, Z = 4, d x = 4.057 g/cm3.  相似文献   

14.
Compounds [Rh(NH3)5(NO2)](NO3)2·H2O (I) with a = 7.6230(3) Å, b = 7.6230(3) Å, c = 10.3584(4) Å, space group I-42m, Z = 2, d calc = 2.026 g/cm3, V = 601.93(4) Å3, Rh-NH3 eq = 2.074 Å, Rh-NH3 ax (NO2) = 2.048 Å; [Rh(NH3)5(NO2)][Pd(NO2)4] (II) with a = 8.095(3) Å, b = 22.422(8) Å, c = 7.887(3) Å, β = 98.559(17)°, space group Cc, Z = 4, d calc = 2.461 g/cm3, V = 1415.6(9) Å3, Rh-NH3 eq = 2.069 Å, Rh-NH3 ax = 2.090 Å, Rh-NO2 = 2.002 Å; K2[Rh(NH3)(NO2)5]·H2O (III) with a = 7.5177(5) Å, b = 20.9856(15) Å, c = 7.7017(5) Å, space group Cmc21, Z = 4, d calc = 2.439 g/cm3, V = 1215.05(14) Å3, Rh-NH3 ax (NO2) = 2.094 Å, Rh-NO2 eq = 2.030 Å are synthesized and studied using single crystal X-ray diffraction.  相似文献   

15.
We correct the crystal structure of MnF3, of which the space group was reported as monoclinic C2/c (no. 15) with a = 8.9202, b = 5.0472, c = 13.4748 Å, β = 92.64°, V = 606.02 ų, Z = 12, mS48, T not given, likely 298 K. In the structure model proposed here, we use a unit cell of one third of the former volume. The ruby red crystals of MnF3 were synthesized by a high-pressure/high-temperature method, where MnF4 was used as a starting material. As determined on a single crystal, MnF3 crystallizes in the monoclinic space group I2/a (no. 15) with a = 5.4964(11), b = 5.0084(10), c = 7.2411(14) Å, β = 93.00(3)°, V = 199.06(7) Å3, Z = 4, mS16, T = 183(2) K. The crystal structure of MnF3 is related by a direct group-subgroup transition to the VF3 structure-type. We performed quantum chemical calculations on the crystal structure to allow the assignment of bands of the obtained vibrational spectra.  相似文献   

16.
The complexes with the formulae [Mn(L1)2] · 0.5H2O (I) and [Mn(L2)2] (II), where L1 and L2 are the dianionic form of 2,4-dichloro-6-[(2-hydroxyethylimino)methyl]phenol and 2-{[1-(3-ethoxy-2-hydroxyphenyl)methylidene]amino}-2-methylpropane-1,3-diol, respectively, were obtained and characterized by elemental analysis and IR spectroscopy. The crystal structures of complexes I and II were determined using X-ray diffraction. The crystal of I is orthorhombic space group Fdd2: a = 24.170(2), b = 32.021(3), c = 11.352(2) Å, V = 8785.9(19) Å3, Z = 8. The crystal of II is monoclinic space group C2/c: a = 13.931(4), b = 18.381(5), c = 12.444(5) Å, β = 121.980(3)°, V = 2702.9(15) Å3, Z = 4. The Mn atom in each of the complexes is in an octahedral coordination.  相似文献   

17.
Two new mononuclear cobalt(III) complexes, [Co(MP)2(N3)] (I) and [Co(BP)2]NO3 · 2H2O (II), where MP is 2-methoxy-6-[(2-morpholin-4-ylethylimino)methyl]phenolate and BP is 4-bromo-2-[(2-methylaminoethylimino)methyl]phenolate, were prepared and structurally characterized by physicochemical methods and single crystal X-ray diffraction. Both complexes crystallize in the monoclinic space group P21/c. For I: a = 10.3526(18), b = 25.371(4), c = 11.3585(19) Å, β = 101.529(8)°, V = 2923.1(8) Å3, Z = 4; for II: a = 9.801(2), b = 27.183(3), c = 10.846(2) Å, β = 114.269(2)°, V = 2634.2(8) Å3, Z = 4. An X-ray structural analysis indicates that in both complexes the Co atoms adopt octahedral coordination. The hindrance effects of the Schiff bases can influence the coordination of the secondary ligands such as azide.  相似文献   

18.
Two 4-phenylbenzophenones (I) and (II) are synthesized via Friedel-Crafts reactions. There are four crystallographically independent molecules with different conformations in the crystal structure of [1,1′-biphenyl]-4-yl(2-chlorophenyl)methanone (I). Crystals are orthorhombic, Pca21, C19H13ClO, a = 13.699(3) Å, b = 8.9385(17) Å, c = 46.836(9) Å; V = 5735(2) Å3, Z = 16, d x = 1.356 g/cm3. Torsion angles between the biphenyl rings are between 28.5° and 30.8°. Several C-H…O and C-H…Cl hydrogen bonds and weak π-π stacking contacts consolidate the crystal. Crystals of [1,1′-biphenyl]-4-yl(3-methoxyphenyl)methanone (II) are orthorhombic, Pbca, C20H16O2, a = 7.8179(15) Å, b = 16.003(3) Å, c = 23.345(5) Å; V = 2920.7(10) Å3, Z = 8, d x = 1.311 g/cm3. The torsion angle between the biphenyl rings is 28.1° and C-H…O hydrogen bonds are observed in compound (II).  相似文献   

19.
Single crystals of two new modifications of [P(C6H5)4]2[Cu2I4] were obtained by reaction of granulated copper with iodine and [P(C6H5)4]I in dry acetone under nitrogen atmosphere. They crystallise monoclinically, space group P21/n (No. 14), a = 11.550(6), b = 7.236(2), c = 27.232(13) Å, β = 98.13(3)°, V = 2253(2) Å3, and Z = 2 ([P(C6H5)4]2[Cu2I4]-C), and space group Cc (No. 9), a = 17.133(5), b = 15.941(5), c = 18.762 (6) Å, β = 114.02(1)°, V = 4681(3) Å3, and Z = 4 ([P(C6H5)4]2[Cu2I4]-D), respectively. In these compounds the [CuI2]? anions form dimers di-μ-iodo-diiodocuprate(I), which are either planar ( C ) or folded ( D ).  相似文献   

20.
Self-assembly between silver carboxylates with 2-aminopyridine derivatives give two silver(I) complexes, [[Ag(5MP)2(CNB)] · NH3 (I) and [Ag(3MP)2(HMB)] (II), where 5MP, CNB, 3MP, and HMB represent 2-amin-5-methylpyridine, 5-chloro-2-nitrobenzoate, 2-amino-3-methylpyridine, and 2-hydroxy-3-methoxybenzoate, respectively. The crystal structures of the complexes were investigated. The Ag atom in each complex is coordinated by two pyridine N atoms and weakly coordinated by a carboxylic O atom. The crystal of I is triclinic: space group P $ \bar 1 $ , a = 7.562(2), b = 11.708(3), c = 12.933(3) Å, α = 103.378(4)°, β = 93.910(4)°, γ = 99.001(4)°, V = 1093.7(5) Å3, Z = 2. The crystal of II is monoclinic: space group C2/c, a = 25.727(5), b = 10.274(2), c = 19.872(4) Å, β = 126.62(3)°, V = 4215.7(15) Å3, Z = 4.  相似文献   

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