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1.
Structures, conformations, and crystallization behavior of compounds cis--[Co(trien)(NO2)2]·ClO4 (I), cis--[Co(trien)(NO2)2]Br·2H2O (II), and cis--[Co(trien)(NO2)2]·ClO3 (III) are reported. Compound (I) crystallized in space group Pbca, with a = 12.3323(9), b = 13.0265(9) and c = 18.1597(13) Å; compound (II) crystallized in space group Pca21, with a = 8.1844(7), b = 14.7011(14) and c = 12.4875(12) Å, while compound (III) also crystallized in space group Pca21, with a = 12.4897(8), b = 8.8499(6) and c = 12.6500(8) Å. In all three cases, the Co(III) ions were six-coordinated with nitrogens from trien and two nitrates. Inter- and intramolecular hydrogen bonding interactions are discussed to explain the conglomerate versus racemate crystallization behavior adopted by these three compounds, with comparison of their known analogue compounds of cis-/-[Co(trien)(NO2)2]X, where X = halide and NO 3. For the cis--[Co(trien)(NO2)2]+ cation, the conformation of the cation itself determines the intramolecular hydrogen bonding pattern, and the interaction of counteranions can be ignored, while in cis--[Co(trien)(NO2)2]·ClO4, the perchlorate interrupts the intramolecular hydrogen bonding pattern observed in the halide analog.  相似文献   

2.
Two cadmium halide complexes with 1,2-bis[2-(diphenylphosphinylmethyl)phenoxy]ethane (L 1) and 1,3-bis[2-(diphenylphosphinylmethyl)phenoxy]propane (L), namely, CdBr2 ? L 1 (I) and CdI2 ? L(II), have been synthesized. An analysis of their vibrational spectra is carried out. The structures of I and II are determined by X-ray diffraction. Crystals I are monoclinic, a = 31.562(6) Å, b = 13.548(3) Å, c = 18.733(4) Å, β = 91.28(3)°, space group C2/c, Z = 8, and R = 0.051 for 3776 reflections. Crystals II are triclinic, a = 11.803(2) Å, b = 12.554(3) Å, c = 14.686(3) Å, α = 90.30(3)°, β = 90.29(3)°, γ = 106.08(3)°, space group $P\bar 1$ , Z = 2, and R = 0.043 for 4916 reflections. Compounds I and II exhibit a polymeric chain structure. The potentially tetradentate ligands L 1 and L are coordinated to the metal atoms only through two phosphoryl oxygen atoms and fulfill the bidentate bridging function. The environment of the Cd atom is completed to the tetrahedral coordination by two Br atoms in complex I and two I atoms in complex II. The mean distances are as follows: Cd-Br, 2.526(2) Å; Cd-I, 2.695 Å; and Cd-O, 2.243(8) Å in I and 2.210(4) Å in II. The L 1 and L ligands in complexes I and II adopt an S-shaped conformation.  相似文献   

3.
The crystal and molecular structure of [ZnCl2(N4-trzCH2COPh)2] (trz = 1,2,4-triazole) has been determined by X-ray crystallography. It crystallizes in the monoclinic system, space group C2/c, with lattice parameters a = 26.7892(4) Å, b = 4.9392(2) Å, c = 20.7872(1) Å, = 127.517 (1), and z = 4. The complex has C 2 symmetry. The coordination geometry of each Zn atom is distorted tetrahedral formed by two Cl atoms and two tertiary N atoms of the -(1,2,4-triazole-1-yl)-acetophenone ligands. The two equivalent Zn–Cl and Zn–N bonds form bond angles around the Zn(II) atom in the range 101.4(1)–120.8(1). C–H O intermolecular interactions link the molecules in infinite chains in the [101] direction.  相似文献   

4.
Crystallography Reports - N-(Phenyl)-2-benzoylethylamine (I), N-(4-chlorophenyl)-2-benzoylethylamine (II), and N-(2-chlorophenyl)-2-benzoylethylamine hydrazone (III) were synthesized in the...  相似文献   

5.
The structure of [NO2Py]2[Ni(mnt)2], as determined by x-ray single crystal analysis, consists of two 1-(4-nitrobenzyl)pyridinium cations and one [Ni(mnt)2]2– anion. The crystallographic data for the complex:monoclinic P21/n, a = 9.913(2) Å, b = 11.968(2) Å, c = 14.566(3) Å, = 100.36(3)°, V = 1699.9(6) Å3, Z = 2. The [Ni(mnt)2]2– anion has a crystallographically imposed center of symmetry and exhibits a relatively planar structure. The cation, [NO2Py]+, adopts a conformation where both the aromatic rings are twisted to the C11-C10-N3 reference plane. The anions (A) and the cations (C) consist of alternating layers (i.e., of type ···C1A1C2A2C1A1C2···) along the c axis of the crystallographic unit cell.  相似文献   

6.
Reaction of 2-pyridylbis(diphenylphosphino)methane (NPP) with [Cu(NCMe)4]BF4 and with [Ni(H2O)6]Cl2 forms [Cu(NPP)(THF)]2(BF4)2 (after recrystallization in the presence of THF) (1) and NiCl2(NPP) (2) respectively Attempts to recrystallize2 led ultimately to the ligand cleavage product [Ni(Ph2PCH2C5H4N)2][NiCl4]·0.85CH2Cl2 (3). Complex1 crystallizes in the monoclinic space groupP21/n witha=13.148(2),b=19.221(2),c=13.458(2) Å3, β=108.61(1)o,V=3222.6(8) ÅZ=2. The structure was refined onF 2 toR1=0.11,wR2=0.14 (R1=0.044 forI≥2σ(I)) for 5661 observed reflections. Complex3 crystallizes in the triclinic space groupP1 witha=12.795(2),b=17.535(1),c=10.203(1) Å, α=107.564(6), β=114.260(8), γ=78.435(8)o,V=1982.1(8) Å3;Z=2. The structure was refined onF toR1=0.044,R w=0.059 for 3534 observed reflections. Dinuclear complex1 has crystallographically imposed centrosymmetry with the NPP ligands arranged in a head-to-tail fashion. The Cu...Cu separation of 3.372(1) Å is too long to support significant metal-metal interaction. Complex3 results from the cleavage of a {PPh2} unit from the NPP ligand and contains an approximately square nickel atom surrounded by two Ph2PCH2C5H4N ligands coordinated in a head-to-head fashion.  相似文献   

7.
The title compound, C30H24N2O4, 3,3′-[1,2-ethanediyl-bis(oxy-2,1-phenylene)]bis[1-(2-pyridyl)-2-propen-1-one] was synthesized and characterized by elemental analysis, FT-IR spectra, 1H NMR, and X-ray single-crystal diffraction. In the molecule, the pyridine plane and the adjacent phenyl plane are almost coplanar with the dihedral angle of 3.07°, while the dihedral angle between the mean planes of the two asymmetric units is 67.56°. The crystal packing is stabilized by weak intermolecular C-H...N and C-H...O hydrogen bonds, C-H...π and π...π stacking interactions.  相似文献   

8.
The complex [Ni(H2O)3(phen)(C4H2O4)] H2O (1), which was obtained by reaction of phenanthroline, Ni(NO3)2 6H2O, and maleic acid in CH3OH/H2O at pH = 7.05, crystallized in the monoclinic space group P21 (no. 4) with cell dimensions: a = 9.350(1) Å, b = 7.631(1) Å, c = 12.821(1) Å, = 106.25(1), and D calc = 1.607 g/cm3 for Z = 2. The Ni atoms are each octahe drally coordinated by one chelating phen ligand, three H2O molecules and one monodentate maleato ligand to form [Ni(H2O)3(phen)(C4H2O4)] complex molecules with d(Ni–O) = 2.038–2.090 Å, d(Ni–N) = 2.066, 2.089 Å. The formed complex molecules are, via the intermolecular hydrogen bonds, assembled into columnar 1D chains. Interdigitation of the chelating phen ligands of the neighboring chains leads to 2D layers and the crystal H2O molecules are hydrogen bonded to the oxygen atoms of the maleate not coordinated to the Ni atom. However, reaction of NiCO3, phen, and maleic acid in CH3OH/H2O at pH = 6.33 afforded [Ni(H2O)2(phen)(C4H2O4)] 2H2O (2), which crystallized in the triclinic space group (no. 2) with cell dimensions: a = 7.971(1) Å, b = 8.237(1) Å, c = 13.304(1) Å, = 81.005(6)°, = 87.877(8)°, = 78.322(8)°, and D calc = 1.671 g/cm3 for Z = 2. The Ni atoms are each octahedrally coordinated by two N atoms of one phen ligand and four O atoms of two H2O molecules and two bis–monodentate maleato ligands with d(Ni–O) = 2.041–2.120 Å and d(Ni–N) = 2.095 Å. The Ni atoms are bridged by the maleato ligands to generate 1D 1 [Ni(H2O)2(phen)(C4H2O4)2/2] chains along [100]. The supramolecular assemblies of the 1D chains via – stacking inter- actions result in thick 2D layers parallel to (001), between which the noncoordinating H2O molecules are sandwiched. The paramagnetic [Ni(H2O)2(phen)(C4H2O4)2/2] 2H2O (2) obeys the Curie–Weiss law m(T-) = 1.139cm3 mol–1 K with the Weiss constant = –0.95 K.  相似文献   

9.
[HB(3,4,5-Me3pz)3]2Zn (1) and [H2B(3,4,5-Me3pz)2]Zn(-3,4,5-Me3pz)2Zn[H2B(3,4,5-Me3pz)2] (2) are present in equal amounts in a crystal in the triclinic space group, P-1 with a = 11.5924(11) Å, b = 12.7799(12) Å, c = 15.7317(14) Å = 107.905(2)° = 96.796(2)°, = 105.786(2)°, and Z = 1. The structure of 1 is a trigonally distorted octahedron and is very similar to the structure of [HB(3,5-Me2pz)3]2Zn showing that the introduction of the third methyl group on the pyrazolyl ring does not impact on structure. [H2B(pz)2]2Zn (3) is orthorhombic, Pca2(1) with a = 10.1473(3) Å, b = 11.1117(2) Å, c = 14.1831(5) Å, = = = 90° and Z = 4. The zinc(II) centers in both 2 and 3 are similar and have pseudotetrahedral structures.  相似文献   

10.

Abstract  

Ozagrel, (E)-3-[4-(1H-imidiazol-1-ylmethyl)phenyl]-2-propenic acid, crystallizes with fumaric acid in absolute ethanol to give the dihydrous fumarate salt, [(C13H13N2O2)2]2+ [C4H2O4]2−·2H2O, which crystallizes in the monoclinic space group P2(1)/n with a = 4.7981(19), b = 11.101(6), c = 26.930(11) Å, β = 90.567(16)°, V = 1434.3(11) Å3, Z = 4, C15H16N2O5, M r  = 304.30, D c  = 1.409 g/cm3. In the crystal structure, fumaric acid transfers two protons to imidazole ring N atoms of ozagrel. And the resulting carboxylate anions are simultaneously hydrogen-boned to carboxylic group and imidazole ring of ozagrel to give rise to a 2D layer structure. Hydrogen-bonding interactions between water and fumarate dianion result in a 3D structure.  相似文献   

11.

Abstract  

The title compound, C23H23FN3O2 has been synthesized and the structure was investigated by X-ray diffraction studies. The compound crystallizes in the triclinic crystal class in the space group P[`1]P\overline{1} with cell parameters a = 9.345(2) ?, b = 10.940(3) ?, c = 11.986(4) ?, α = 72.349(6)°, β = 68.106(18)°, γ = 66.867(5)°, Z = 2 and V = 1027.8(5) ?3. The hydantoin ring adopts a planar conformation and is affected by the π conjugation. The pyrrolidine and piperidine rings in the bicyclo octane moiety adopt envelope and chair conformations respectively. The structure exhibits both inter and intramolecular hydrogen bonds of the type N–H···O, C–H···O and C–H···N. One of the oxygen atoms attached to the hydantoin ring simultaneously accepts two hydrogen bonds to form a three centered hydrogen bonding pattern.  相似文献   

12.
A new microporous coordination polymer, [Co(saccharinate)2(L1)(H2O)2] n solvate, has been prepared from the reaction of the N,N bidentate ligand 1,4-bis(3-pyridyl)-2,3-diaza-1,3-butadiene (L1) with [Co(saccharinate)2·4H2O]·2H2O in a methylene chloride/ethanol solvent mixture. The compound crystallizes in the triclinic system, space group P-1, with lattice parameters a = 7.6893(5) Å, b = 11.0169(7) Å, c = 11.2369(7) Å, = 66.2610(10)°, = 74.4160(10)°, = 74.6740(10)°. The structure consists of one-dimensional chains composed of octahedrally coordinated Co(II) centers linked by L1. The packing of these chains, along with intrachain and interchain hydrogen bonds, generates a 3-D framework with infinite channels that are occupied by disordered guest molecules. The compound was further characterized by IR spectroscopy and DTA/TGA.  相似文献   

13.
Compounds (CN3H6)2[UO2(OH)2(NCS)]NO3 (I) and β-Cs3[UO2(NCS)5] (II) are synthesized and studied by IR spectroscopy and single-crystal X-ray diffraction. I and II crystallize in the orthorhombic system. For I, a = 12.2015(13) Å, b = 7.3295(8) Å, c = 16.310(2) Å, space group Pnma, Z = 4, and R = 0.0327; for II, a = 21.7891(6) Å, b = 13.5120(3) Å, c = 6.8522(2) Å, space group Pnma, Z = 4, and R = 0.0268. In structure I, complex groups form infinite chains [UO2(OH)2(NCS)] n n? belonging to the AM 2 2 M 1 crystal chemical group of uranyl complexes (A = UO 2 2+ , M 2 = OH?, and M 1 = NCS?). The main structural elements of crystals II are mononuclear [UO2(NCS)5]3? groups belonging to the AM 5 1 group of uranyl complexes (A = UO 2 2+ and M 1 = NCS?). In I and II, uranium-containing complexes are connected with outer-sphere cations by electrostatic interactions, and in I a system of hydrogen bonds also contributes to their binding. Specific features of the packing of complex [UO2(NCS)5]3? groups in the structures of two modifications of Cs3[UO2(NCS)5] are discussed.  相似文献   

14.
The structure of the title compound [Cu2Cl2(C13H12NO2)2]·1/2 H2O has been determined from single crystal X-ray diffraction data by direct methods. Full-matrix least-squares refinement of the structural parameters led to conventionalR factor of 0.037 for 4367 intensities above 3(I). The compound forms a dinuclear complex with distorted tetragonal-pyramidal geometry at each copper center. The unsymmetrical dimers are formed by weak axial coordination to one copper center by chloride ligands which are in the base plane of the adjacent copper atom. The apical Cu1-C12 and Cu2-C11 distances are 2.788(1) and 3.130(1) Å, respectively. The Cu1-Cu2 separation is 3.4995(3) Å in the dimers. A disorder of one five-membered chelate ring has been observed. Two alternative positionsa andb of the C26 atom were found and refined with constrained bond lengths. The geometry of the ligand and hydrogen bonds is discussed.  相似文献   

15.
The crystal structure of the title compound has been determined from three-dimensional, single crystal X-ray diffraction data. [Cu2Cl2(C13H12NO2)2]·2H2O crystallizes in the orthorhombic space group P212121 with lattice constants,a=11.866(2),b=13.555(3),c=17.380(3) Å. Final full-matrix least-squares refinement of 3735 unique reflections yieldedR=0.054. The structure consists of dimeric C26H24Cl2Cu2N2O4 molecules and water molecules connected with the dimeric molecules by a hydrogen bond system. Both of the copper(II) centers are five-coordinated by twotrans oxygen atoms and one nitrogen atom from one ligand molecule and two chloride ions. The geometry at each copper(II) center is best described as distorted tetragonal pyramidal. The apical Cu1–Cl2 and Cu2–C11 distances are 2.747(2) and 2.938(3)Å, respectively. The Cu...Cu separation is 3.496(1)Å. The comparison with previously reported crystal structure of [Cu2Cl2 (C13H12NO2)2]·1/2H2O is given.  相似文献   

16.
17.
The dimeric complex [Mn2(-pyS)2(CO)6] (1) reacted with 2 M equivalents of both PPh3 and PHPh2 to give the respective monomeric phosphine complexes [Mn(pyS)(L)(CO)3][L = PPh3 (2) and PHPh2 (3)]; with 4 M equivalents of dppm, it yielded the complex [Mn(pyS)(1-dppm)2(CO)2](4). An X-ray structure determination of 4 shows that it crystallizes in the monoclinic space group P21/n with a = 11.027(3), b = 24.984(7), c = 18.379(5) Å, = 99.870(8)°, V = 4988(2) Å3, and Z = 4. The complex has an octahedral geometry with the chelating pyS ligand and two CO groups occupying the equatorial sites and the two monodentate dppm ligands lying in the trans positions.  相似文献   

18.
The crystalline products [Me2Al–N(CH2CH2)2–C–(OCH2)2]2 (I) and [Me2Ga–N(Si(H)Me2)2]2 (II) were prepared from reactions of trimethylaluminum and trimethylgallium with 1,4-dioxa-8-azaspiro[4.5]-decane and 1,1,3,3-tetramethyldisilazane, respectively, in toluene. The organoaluminum dimer crystallizes in the monoclinic space groupP21/c with unit cell parametersa=8.970(2) ,b=9.683(2) ,c=12.833(3) , =103.18(2)°,V=1085.3(3) 3, andD calcd=1.22 g cm–3 forZ=2. Least-squares refinement based on 935 observed reflectionsI>3(I) in the range 3.5°<2<45.0° led to a finalR factor of 0.033 (R w =0.041). The dimeric organosilazagallium crystallizes in the triclinic space group with unit cell parametersa=7.636(2) ,b=9.168(2) ,c=9.466(3), =72.81(2)°, =87.94(2)°, =69.90(2)°,V=593.0(3) 3, andD calcd=1.30 g cm–3 forZ=1. Least-squares refinement based on 1661 observed reflectionsI>3(I) in the range 3.5°<2<48.0° led to a finalR factor of 0.055 (R w =0.070). Both compoundsI andII reside about a crystallographic center of symmetry and contain a planar M2N2 (M=Al forI, Ga forII) four-membered ring withI having an Al...Al contact of 2.801 .  相似文献   

19.
A new decavanadate with mixed cations, [Mn(H2O)6]2[N(CH3)4]2[V10O28]·2H2O (1), was crystallized from a hydrothermal reaction between MnCO3 and V2O5 in the presence of N(CH3)4Br at 100°C. The structure of 1, as determined by x-ray single crystal analysis, consists of cations and anions of hexa-aqua manganese [Mn(H2O)6]2+, tetramethyl ammonium [N(CH3)4]+ and decavanadate [V10O28]6–. The extended H-bonding between the [Mn(H2O)6]2+ and [V10O28]6– ions gives rise to a pseudo- two-dimensional network in the crystal lattice x-ray crystallographic data for 1: monoclinic P21/n, a = 9.1499(5), b = 12.8725(7), c = 18.625(1) Å, = 92.252(1)°, V = 2192.0(2) Å3, MZ = 2, and D calcd = 2.22 g cm–3.  相似文献   

20.
The crystal structure of the title compound was determined by X-ray crystallography. The compound crystallizes in the monoclinic crystal system witha=8.152(4),b=17.994(7),c=8.634(9) Å, =108.92(5)°, space group P21/c (N:14),V=1198.02 Å3,Z=4. The mercuryl(II) atom forms two strong, almost colinear bonds (bond angle 176.1(4)°) with a carbon of the phenyl ring (Hg–C=1.99(1) Å) and one of the acetate oxygen atoms (Hg–O(1)=2.005(7) Å). These primary bonds are supplemented by secondary intramolecular interactions with the pyridine nitrogen (Hg...N=2.727(9) Å) and the other acetate oxygen (Hg...O(2)=2.925(8) Å), although the latter is very weak and the acetate anion therefore practically monodentate. Weak additional intermolecular Hg–C and Hg–O(1)interactions contribute to the lattice structure.  相似文献   

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